data_a150923b _audit_creation_date 2019-05-21 _audit_creation_method ; Olex2 1.2-beta (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C76 H78 N10, 4(F6 P), 4(C2 H3 N)' _chemical_formula_sum 'C84 H90 F24 N14 P4' _chemical_formula_weight 1875.57 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8507(5) _cell_length_b 12.4012(6) _cell_length_c 14.9512(5) _cell_angle_alpha 92.401(3) _cell_angle_beta 94.311(3) _cell_angle_gamma 107.344(4) _cell_volume 2086.65(15) _cell_formula_units_Z 1 _cell_measurement_reflns_used 5167 _cell_measurement_temperature 172.96(10) _cell_measurement_theta_max 73.5960 _cell_measurement_theta_min 4.5200 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.797 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.89133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 968 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_unetI/netI 0.0559 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 14087 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.061 _diffrn_reflns_theta_max 67.061 _diffrn_reflns_theta_min 3.743 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 172.96(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2740 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -43.00 30.00 1.0000 9.5650 omega____ theta____ kappa____ phi______ frames - -38.5000 38.0000 -90.0000 73 #__ type_ start__ end____ width___ exp.time_ 2 omega -88.00 -10.00 1.0000 9.5650 omega____ theta____ kappa____ phi______ frames - -38.5000 125.0000 -90.0000 78 #__ type_ start__ end____ width___ exp.time_ 3 omega -110.00 -18.00 1.0000 9.5650 omega____ theta____ kappa____ phi______ frames - -38.5000 -38.0000 120.0000 92 #__ type_ start__ end____ width___ exp.time_ 4 omega -109.00 -18.00 1.0000 9.5650 omega____ theta____ kappa____ phi______ frames - -38.5000 -38.0000 30.0000 91 #__ type_ start__ end____ width___ exp.time_ 5 omega 55.00 82.00 1.0000 9.5650 omega____ theta____ kappa____ phi______ frames - 43.1514 -125.0000 -180.0000 27 #__ type_ start__ end____ width___ exp.time_ 6 omega 47.00 89.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -45.0000 -180.0000 42 #__ type_ start__ end____ width___ exp.time_ 7 omega 50.00 104.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -94.0000 -150.0000 54 #__ type_ start__ end____ width___ exp.time_ 8 omega 97.00 122.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -125.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 9 omega 63.00 90.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -45.0000 -90.0000 27 #__ type_ start__ end____ width___ exp.time_ 10 omega 39.00 68.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -30.0000 0.0000 29 #__ type_ start__ end____ width___ exp.time_ 11 omega 47.00 75.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -45.0000 30.0000 28 #__ type_ start__ end____ width___ exp.time_ 12 omega 53.00 90.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -30.0000 60.0000 37 #__ type_ start__ end____ width___ exp.time_ 13 omega 55.00 112.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -77.0000 90.0000 57 #__ type_ start__ end____ width___ exp.time_ 14 omega 45.00 72.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -30.0000 150.0000 27 #__ type_ start__ end____ width___ exp.time_ 15 omega 36.00 81.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -30.0000 120.0000 45 #__ type_ start__ end____ width___ exp.time_ 16 omega 89.00 178.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 30.0000 60.0000 89 #__ type_ start__ end____ width___ exp.time_ 17 omega 113.00 176.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 45.0000 150.0000 63 #__ type_ start__ end____ width___ exp.time_ 18 omega 95.00 143.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 125.0000 -120.0000 48 #__ type_ start__ end____ width___ exp.time_ 19 omega 33.00 85.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -30.0000 -120.0000 52 #__ type_ start__ end____ width___ exp.time_ 20 omega 26.00 107.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -94.0000 -60.0000 81 #__ type_ start__ end____ width___ exp.time_ 21 omega 35.00 106.00 1.0000 38.2600 omega____ theta____ kappa____ phi______ frames - 106.0351 -94.0000 30.0000 71 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.1229101000 _diffrn_orient_matrix_UB_12 0.0897550000 _diffrn_orient_matrix_UB_13 0.0063094000 _diffrn_orient_matrix_UB_21 0.0281395000 _diffrn_orient_matrix_UB_22 -0.0340356000 _diffrn_orient_matrix_UB_23 0.0950849000 _diffrn_orient_matrix_UB_31 0.0529821000 _diffrn_orient_matrix_UB_32 -0.0883224000 _diffrn_orient_matrix_UB_33 -0.0405638000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4683 _reflns_number_total 7439 _reflns_odcompleteness_completeness 99.85 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.907 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.075 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 579 _refine_ls_number_reflns 7439 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1117 _refine_ls_R_factor_gt 0.0754 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1224P)^2^+0.8740P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1986 _refine_ls_wR_factor_ref 0.2238 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances P1-F4' = P1-F4 = P1-F2 = P1-F3 = P1-F2' = P1-F2 = P1-F1' = P1-F1 1.56 with sigma of 0.01 P1-F1' 1.56 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints Uanis(F1') \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F4') \\sim Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(F1') \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002 Uanis(F2) = Uanis(F3) Uanis(F4) = Uanis(F4') Uanis(F1) = Uanis(F1') Uanis(F2) = Uanis(F2') Uanis(F3') = Uanis(F3) 4. Others Sof(F1')=Sof(F2')=Sof(F3')=Sof(F4')=1-FVAR(1) Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1) 5.a Ternary CH refined with riding coordinates: N3(H3) 5.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C29(H29A,H29B), C31(H31A,H31B) 5.c Aromatic/amide H refined with riding coordinates: C3(H3A), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C18(H18), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C35(H35), C36(H36), C37(H37), C38(H38) 5.d Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C30(H30A,H30B,H30C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.7608(3) 0.1296(3) 0.9419(2) 0.0372(7) Uani 1 1 d . . . . . N2 N 0.6005(3) 0.1150(3) 0.8368(2) 0.0345(7) Uani 1 1 d . . . . . N3 N 0.5297(3) 0.3486(3) 0.70594(19) 0.0333(7) Uani 1 1 d . . . . . H3 H 0.5778 0.4283 0.7101 0.040 Uiso 1 1 calc R . . . . N4 N 0.4744(3) 0.5608(3) 0.7565(2) 0.0381(8) Uani 1 1 d . . . . . N5 N 0.6375(3) 0.7105(3) 0.7290(2) 0.0439(8) Uani 1 1 d . . . . . C1 C 0.9761(4) 0.1485(4) 0.9419(4) 0.0553(12) Uani 1 1 d . . . . . H1A H 0.9739 0.1526 0.8778 0.083 Uiso 1 1 calc GR . . . . H1B H 0.9601 0.0710 0.9563 0.083 Uiso 1 1 calc GR . . . . H1C H 1.0532 0.1918 0.9690 0.083 Uiso 1 1 calc GR . . . . C2 C 0.8827(4) 0.1963(4) 0.9776(3) 0.0513(11) Uani 1 1 d . . . . . H2A H 0.8891 0.1971 1.0427 0.062 Uiso 1 1 calc R . . . . H2B H 0.8978 0.2739 0.9612 0.062 Uiso 1 1 calc R . . . . C3 C 0.7058(3) 0.1687(3) 0.8776(3) 0.0351(8) Uani 1 1 d . . . . . H3A H 0.7444 0.2401 0.8593 0.042 Uiso 1 1 calc R . . . . C4 C 0.5394(4) 0.0025(3) 0.8591(3) 0.0355(8) Uani 1 1 d . . . . . C5 C 0.5960(4) -0.0411(3) 0.9293(3) 0.0375(9) Uani 1 1 d . . . . . C6 C 0.7065(4) 0.0215(3) 0.9739(3) 0.0378(9) Uani 1 1 d . . . . . C7 C 0.7588(4) -0.0216(4) 1.0432(3) 0.0469(10) Uani 1 1 d . . . . . H7 H 0.8305 0.0218 1.0735 0.056 Uiso 1 1 calc R . . . . C8 C 0.7036(5) -0.1311(4) 1.0678(3) 0.0531(12) Uani 1 1 d . . . . . H8 H 0.7397 -0.1608 1.1139 0.064 Uiso 1 1 calc R . . . . C9 C 0.5978(5) -0.1944(4) 1.0252(3) 0.0539(12) Uani 1 1 d . . . . . H9 H 0.5630 -0.2672 1.0425 0.065 Uiso 1 1 calc R . . . . C10 C 0.5392(4) -0.1522(3) 0.9550(3) 0.0446(10) Uani 1 1 d . . . . . C11 C 0.4289(4) -0.2135(3) 0.9096(3) 0.0501(11) Uani 1 1 d . . . . . H11 H 0.3902 -0.2858 0.9262 0.060 Uiso 1 1 calc R . . . . C12 C 0.3781(4) -0.1694(4) 0.8425(3) 0.0488(11) Uani 1 1 d . . . . . H12 H 0.3053 -0.2123 0.8135 0.059 Uiso 1 1 calc R . . . . C13 C 0.4326(4) -0.0591(3) 0.8149(3) 0.0417(9) Uani 1 1 d . . . . . H13 H 0.3970 -0.0297 0.7684 0.050 Uiso 1 1 calc R . . . . C14 C 0.5417(4) 0.1678(3) 0.7654(2) 0.0334(8) Uani 1 1 d . . . . . H14A H 0.4583 0.1516 0.7748 0.040 Uiso 1 1 calc R . . . . H14B H 0.5465 0.1332 0.7070 0.040 Uiso 1 1 calc R . . . . C15 C 0.5976(4) 0.2958(3) 0.7653(2) 0.0351(8) Uani 1 1 d . . . . . H15A H 0.6039 0.3291 0.8261 0.042 Uiso 1 1 calc R . . . . H15B H 0.6772 0.3115 0.7467 0.042 Uiso 1 1 calc R . . . . C16 C 0.4181(4) 0.3517(3) 0.7370(3) 0.0391(9) Uani 1 1 d . . . . . H16A H 0.3835 0.2832 0.7668 0.047 Uiso 1 1 calc R . . . . H16B H 0.3638 0.3537 0.6857 0.047 Uiso 1 1 calc R . . . . C17 C 0.4330(4) 0.4538(4) 0.8015(3) 0.0410(9) Uani 1 1 d . . . . . H17A H 0.3576 0.4488 0.8251 0.049 Uiso 1 1 calc R . . . . H17B H 0.4898 0.4538 0.8517 0.049 Uiso 1 1 calc R . . . . C18 C 0.5885(4) 0.6151(3) 0.7655(3) 0.0412(9) Uani 1 1 d . . . . . H18 H 0.6380 0.5839 0.8000 0.049 Uiso 1 1 calc R . . . . C19 C 0.5660(4) 0.7630(4) 0.6767(3) 0.0446(10) Uani 1 1 d . . . . . C20 C 0.4438(4) 0.7036(4) 0.6616(2) 0.0400(9) Uani 1 1 d . . . . . C21 C 0.3945(4) 0.5985(3) 0.6996(3) 0.0392(9) Uani 1 1 d . . . . . C22 C 0.2762(4) 0.5406(4) 0.6832(3) 0.0449(10) Uani 1 1 d . . . . . H22 H 0.2444 0.4728 0.7094 0.054 Uiso 1 1 calc R . . . . C23 C 0.2035(5) 0.5842(5) 0.6268(3) 0.0536(11) Uani 1 1 d . . . . . H23 H 0.1241 0.5426 0.6133 0.064 Uiso 1 1 calc R . . . . C24 C 0.2464(5) 0.6865(5) 0.5909(3) 0.0551(12) Uani 1 1 d . . . . . H24 H 0.1957 0.7154 0.5556 0.066 Uiso 1 1 calc R . . . . C25 C 0.3673(5) 0.7480(4) 0.6076(3) 0.0493(11) Uani 1 1 d . . . . . C26 C 0.4162(6) 0.8555(4) 0.5738(3) 0.0593(13) Uani 1 1 d . . . . . H26 H 0.3675 0.8882 0.5399 0.071 Uiso 1 1 calc R . . . . C27 C 0.5338(6) 0.9110(5) 0.5907(3) 0.0652(14) Uani 1 1 d . . . . . H27 H 0.5643 0.9811 0.5674 0.078 Uiso 1 1 calc R . . . . C28 C 0.6118(5) 0.8661(4) 0.6424(3) 0.0558(12) Uani 1 1 d . . . . . H28 H 0.6922 0.9056 0.6529 0.067 Uiso 1 1 calc R . . . . C29 C 0.7674(4) 0.7623(4) 0.7460(3) 0.0487(10) Uani 1 1 d . . . . . H29A H 0.7985 0.7945 0.6916 0.058 Uiso 1 1 calc R . . . . H29B H 0.8035 0.7036 0.7603 0.058 Uiso 1 1 calc R . . . . C30 C 0.8026(5) 0.8540(4) 0.8221(3) 0.0565(12) Uani 1 1 d . . . . . H30A H 0.7711 0.9144 0.8069 0.085 Uiso 1 1 calc GR . . . . H30B H 0.8876 0.8826 0.8316 0.085 Uiso 1 1 calc GR . . . . H30C H 0.7714 0.8229 0.8761 0.085 Uiso 1 1 calc GR . . . . C31 C 0.5232(4) 0.3135(3) 0.6094(2) 0.0355(8) Uani 1 1 d . . . . . H31A H 0.4559 0.2463 0.5945 0.043 Uiso 1 1 calc R . . . . H31B H 0.5947 0.2952 0.5969 0.043 Uiso 1 1 calc R . . . . C32 C 0.5098(3) 0.4089(3) 0.5521(2) 0.0337(8) Uani 1 1 d . . . . . C33 C 0.3994(3) 0.4060(3) 0.5089(2) 0.0337(8) Uani 1 1 d . . . . . C34 C 0.6105(3) 0.5012(3) 0.5433(2) 0.0333(8) Uani 1 1 d . . . . . C35 C 0.7258(4) 0.5062(4) 0.5840(3) 0.0412(9) Uani 1 1 d . . . . . H35 H 0.7336 0.4485 0.6195 0.049 Uiso 1 1 calc R . . . . C36 C 0.8233(4) 0.5929(4) 0.5720(3) 0.0463(10) Uani 1 1 d . . . . . H36 H 0.8972 0.5927 0.5978 0.056 Uiso 1 1 calc R . . . . C37 C 0.8146(4) 0.6836(4) 0.5210(3) 0.0470(10) Uani 1 1 d . . . . . H37 H 0.8824 0.7424 0.5130 0.056 Uiso 1 1 calc R . . . . C38 C 0.7076(4) 0.6850(4) 0.4837(3) 0.0417(9) Uani 1 1 d . . . . . H38 H 0.7030 0.7469 0.4522 0.050 Uiso 1 1 calc R . . . . P1 P 0.77556(10) 0.52739(9) 0.99598(7) 0.0431(3) Uani 1 1 d D . . . . F5 F 0.6342(2) 0.4786(3) 0.9831(2) 0.0688(8) Uani 1 1 d . . . . . F6 F 0.9156(2) 0.5735(2) 1.0088(2) 0.0662(8) Uani 1 1 d . . . . . F1 F 0.7806(4) 0.5928(4) 0.9088(3) 0.0782(12) Uani 0.770(3) 1 d D U P A 1 F2 F 0.7846(4) 0.4180(3) 0.9430(3) 0.0663(7) Uani 0.770(3) 1 d D . P A 1 F3 F 0.7708(4) 0.4648(3) 1.0879(2) 0.0663(7) Uani 0.770(3) 1 d D . P A 1 F4 F 0.7643(4) 0.6344(3) 1.0533(4) 0.0856(15) Uani 0.770(3) 1 d D U P A 1 F1' F 0.7630(14) 0.5149(15) 0.8882(5) 0.0782(12) Uani 0.230(3) 1 d D U P A 2 F2' F 0.7883(13) 0.4042(8) 0.9871(10) 0.0663(7) Uani 0.230(3) 1 d D . P A 2 F3' F 0.7891(12) 0.5638(13) 1.0892(9) 0.0663(7) Uani 0.230(3) 1 d . . P A 2 F4' F 0.7608(13) 0.6444(8) 0.9673(12) 0.0856(15) Uani 0.230(3) 1 d D U P A 2 P2 P 0.89539(13) 0.20644(12) 0.65762(9) 0.0581(4) Uani 1 1 d . . . . . F7 F 0.7599(3) 0.1917(4) 0.6302(3) 0.1078(14) Uani 1 1 d . . . . . F8 F 0.9279(5) 0.3230(4) 0.6110(3) 0.1211(16) Uani 1 1 d . . . . . F9 F 1.0294(4) 0.2248(5) 0.6833(3) 0.1165(16) Uani 1 1 d . . . . . F10 F 0.8613(5) 0.0930(4) 0.7057(3) 0.1272(18) Uani 1 1 d . . . . . F11 F 0.8910(3) 0.2722(3) 0.7502(2) 0.0871(10) Uani 1 1 d . . . . . F12 F 0.9008(4) 0.1449(5) 0.5653(3) 0.1149(16) Uani 1 1 d . . . . . N7 N 0.7230(6) -0.0687(5) 0.3448(5) 0.111(2) Uani 1 1 d . . . . . C41 C 0.8191(5) -0.0163(4) 0.3543(4) 0.0657(14) Uani 1 1 d . . . . . C42 C 0.9394(6) 0.0518(6) 0.3666(5) 0.0859(19) Uani 1 1 d . . . . . H42A H 0.9562 0.1014 0.3185 0.129 Uiso 1 1 calc GR . . . . H42B H 0.9901 0.0041 0.3668 0.129 Uiso 1 1 calc GR . . . . H42C H 0.9535 0.0960 0.4229 0.129 Uiso 1 1 calc GR . . . . N6 N 1.0525(5) 0.7459(5) 0.7874(4) 0.0783(14) Uani 1 1 d . . . . . C39 C 1.0252(5) 0.6491(6) 0.7917(3) 0.0617(13) Uani 1 1 d . . . . . C40 C 0.9918(6) 0.5282(5) 0.7959(4) 0.0724(15) Uani 1 1 d . . . . . H40A H 0.9166 0.4943 0.7617 0.109 Uiso 1 1 calc GR . . . . H40B H 0.9855 0.5095 0.8574 0.109 Uiso 1 1 calc GR . . . . H40C H 1.0509 0.4999 0.7714 0.109 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0466(19) 0.0284(16) 0.0367(17) 0.0065(13) 0.0012(14) 0.0118(14) N2 0.0407(18) 0.0279(15) 0.0341(16) 0.0081(13) 0.0025(13) 0.0087(14) N3 0.0447(18) 0.0322(15) 0.0274(14) 0.0125(12) 0.0094(13) 0.0153(14) N4 0.050(2) 0.0373(17) 0.0336(16) 0.0051(14) 0.0063(14) 0.0213(16) N5 0.054(2) 0.0389(18) 0.0408(18) 0.0015(15) 0.0085(16) 0.0158(16) C1 0.047(3) 0.047(3) 0.068(3) 0.012(2) -0.007(2) 0.009(2) C2 0.058(3) 0.035(2) 0.054(3) 0.0056(19) -0.014(2) 0.007(2) C3 0.040(2) 0.0277(18) 0.0369(19) 0.0058(15) 0.0038(16) 0.0080(16) C4 0.043(2) 0.0254(18) 0.039(2) 0.0034(15) 0.0128(16) 0.0093(16) C5 0.050(2) 0.0307(19) 0.0367(19) 0.0093(16) 0.0177(17) 0.0156(17) C6 0.052(2) 0.0302(19) 0.0339(19) 0.0069(16) 0.0105(17) 0.0148(17) C7 0.059(3) 0.048(2) 0.039(2) 0.0105(19) 0.0084(19) 0.022(2) C8 0.076(3) 0.052(3) 0.045(2) 0.024(2) 0.019(2) 0.034(3) C9 0.077(3) 0.041(2) 0.055(3) 0.026(2) 0.032(2) 0.026(2) C10 0.060(3) 0.030(2) 0.050(2) 0.0095(18) 0.026(2) 0.0187(19) C11 0.063(3) 0.028(2) 0.060(3) 0.0095(19) 0.027(2) 0.010(2) C12 0.045(2) 0.034(2) 0.064(3) -0.003(2) 0.017(2) 0.0034(18) C13 0.045(2) 0.034(2) 0.046(2) 0.0017(17) 0.0113(18) 0.0110(18) C14 0.045(2) 0.0284(18) 0.0268(17) 0.0097(14) 0.0008(15) 0.0102(16) C15 0.042(2) 0.0326(19) 0.0322(18) 0.0100(15) 0.0043(15) 0.0115(16) C16 0.045(2) 0.040(2) 0.0328(19) 0.0125(16) 0.0051(16) 0.0120(18) C17 0.051(2) 0.047(2) 0.0297(19) 0.0121(17) 0.0098(17) 0.0207(19) C18 0.055(3) 0.040(2) 0.035(2) 0.0007(17) 0.0054(18) 0.024(2) C19 0.065(3) 0.039(2) 0.033(2) 0.0021(17) 0.0072(18) 0.019(2) C20 0.058(3) 0.042(2) 0.0284(18) 0.0041(16) 0.0097(17) 0.027(2) C21 0.053(2) 0.042(2) 0.0304(18) 0.0037(16) 0.0078(17) 0.0257(19) C22 0.052(3) 0.052(2) 0.039(2) 0.0052(19) 0.0111(18) 0.026(2) C23 0.054(3) 0.072(3) 0.043(2) 0.005(2) 0.005(2) 0.032(2) C24 0.067(3) 0.076(3) 0.038(2) 0.011(2) 0.005(2) 0.043(3) C25 0.077(3) 0.054(3) 0.0284(19) 0.0063(18) 0.0076(19) 0.036(2) C26 0.096(4) 0.056(3) 0.037(2) 0.017(2) 0.007(2) 0.039(3) C27 0.104(5) 0.049(3) 0.045(3) 0.018(2) 0.011(3) 0.023(3) C28 0.077(3) 0.047(3) 0.044(2) 0.012(2) 0.012(2) 0.017(2) C29 0.052(3) 0.049(2) 0.046(2) 0.001(2) 0.0107(19) 0.014(2) C30 0.065(3) 0.052(3) 0.049(3) -0.003(2) 0.004(2) 0.014(2) C31 0.046(2) 0.0357(19) 0.0275(17) 0.0069(15) 0.0045(15) 0.0148(17) C32 0.041(2) 0.040(2) 0.0230(16) 0.0073(15) 0.0041(15) 0.0144(17) C33 0.043(2) 0.038(2) 0.0213(16) 0.0046(15) 0.0069(15) 0.0132(16) C34 0.039(2) 0.043(2) 0.0214(16) 0.0034(15) 0.0061(14) 0.0168(17) C35 0.046(2) 0.050(2) 0.0301(19) 0.0066(17) 0.0030(16) 0.0182(19) C36 0.037(2) 0.065(3) 0.037(2) 0.005(2) 0.0007(17) 0.016(2) C37 0.041(2) 0.053(3) 0.038(2) 0.0031(19) 0.0053(17) 0.0012(19) C38 0.050(2) 0.042(2) 0.0299(18) 0.0048(16) 0.0044(17) 0.0085(18) P1 0.0444(6) 0.0374(5) 0.0476(6) 0.0045(4) 0.0053(5) 0.0121(4) F5 0.0481(16) 0.086(2) 0.0696(18) 0.0166(16) 0.0031(13) 0.0150(15) F6 0.0495(16) 0.0548(16) 0.087(2) -0.0028(15) 0.0055(14) 0.0056(13) F1 0.0773(16) 0.0826(17) 0.0769(16) 0.0206(13) 0.0071(12) 0.0252(13) F2 0.0676(16) 0.0674(16) 0.0587(16) 0.0016(14) 0.0052(14) 0.0131(13) F3 0.0676(16) 0.0674(16) 0.0587(16) 0.0016(14) 0.0052(14) 0.0131(13) F4 0.083(3) 0.0414(19) 0.134(4) -0.013(2) 0.050(3) 0.0130(18) F1' 0.0773(16) 0.0826(17) 0.0769(16) 0.0206(13) 0.0071(12) 0.0252(13) F2' 0.0676(16) 0.0674(16) 0.0587(16) 0.0016(14) 0.0052(14) 0.0131(13) F3' 0.0676(16) 0.0674(16) 0.0587(16) 0.0016(14) 0.0052(14) 0.0131(13) F4' 0.083(3) 0.0414(19) 0.134(4) -0.013(2) 0.050(3) 0.0130(18) P2 0.0656(8) 0.0679(8) 0.0499(7) 0.0094(6) 0.0135(6) 0.0311(7) F7 0.074(2) 0.153(4) 0.104(3) -0.006(3) 0.003(2) 0.049(3) F8 0.171(5) 0.098(3) 0.087(3) 0.038(2) 0.009(3) 0.026(3) F9 0.075(3) 0.164(5) 0.117(3) -0.005(3) 0.003(2) 0.049(3) F10 0.181(5) 0.071(2) 0.104(3) 0.034(2) -0.006(3) 0.002(3) F11 0.097(3) 0.091(3) 0.071(2) -0.0035(19) 0.0213(18) 0.022(2) F12 0.139(4) 0.144(4) 0.077(2) -0.022(3) 0.018(2) 0.067(3) N7 0.081(4) 0.068(3) 0.164(7) 0.020(4) -0.032(4) 0.003(3) C41 0.068(4) 0.046(3) 0.077(4) 0.009(2) -0.012(3) 0.012(3) C42 0.071(4) 0.075(4) 0.103(5) 0.008(4) 0.011(3) 0.007(3) N6 0.069(3) 0.088(4) 0.075(3) -0.003(3) -0.001(2) 0.022(3) C39 0.055(3) 0.081(4) 0.046(3) -0.003(3) -0.002(2) 0.019(3) C40 0.079(4) 0.084(4) 0.059(3) 0.013(3) 0.015(3) 0.028(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.480(6) . ? N1 C3 1.310(5) . ? N1 C6 1.424(5) . ? N2 C3 1.315(5) . ? N2 C4 1.433(5) . ? N2 C14 1.507(5) . ? N3 H3 0.9800 . ? N3 C15 1.456(5) . ? N3 C16 1.445(5) . ? N3 C31 1.479(5) . ? N4 C17 1.480(5) . ? N4 C18 1.312(6) . ? N4 C21 1.420(5) . ? N5 C18 1.315(6) . ? N5 C19 1.423(6) . ? N5 C29 1.479(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C1 C2 1.521(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9300 . ? C4 C5 1.416(6) . ? C4 C13 1.369(6) . ? C5 C6 1.408(6) . ? C5 C10 1.424(6) . ? C6 C7 1.374(6) . ? C7 H7 0.9300 . ? C7 C8 1.398(7) . ? C8 H8 0.9300 . ? C8 C9 1.359(7) . ? C9 H9 0.9300 . ? C9 C10 1.419(7) . ? C10 C11 1.406(7) . ? C11 H11 0.9300 . ? C11 C12 1.350(7) . ? C12 H12 0.9300 . ? C12 C13 1.421(6) . ? C13 H13 0.9300 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.527(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C17 1.518(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18 0.9300 . ? C19 C20 1.411(6) . ? C19 C28 1.369(6) . ? C20 C21 1.422(6) . ? C20 C25 1.415(6) . ? C21 C22 1.369(6) . ? C22 H22 0.9300 . ? C22 C23 1.397(6) . ? C23 H23 0.9300 . ? C23 C24 1.368(7) . ? C24 H24 0.9300 . ? C24 C25 1.405(7) . ? C25 C26 1.418(7) . ? C26 H26 0.9300 . ? C26 C27 1.357(8) . ? C27 H27 0.9300 . ? C27 C28 1.413(7) . ? C28 H28 0.9300 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 C30 1.517(6) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C32 1.528(5) . ? C32 C33 1.405(5) . ? C32 C34 1.404(6) . ? C33 C34 1.446(5) 2_666 ? C33 C38 1.439(6) 2_666 ? C34 C33 1.446(5) 2_666 ? C34 C35 1.437(6) . ? C35 H35 0.9300 . ? C35 C36 1.353(6) . ? C36 H36 0.9300 . ? C36 C37 1.409(7) . ? C37 H37 0.9300 . ? C37 C38 1.351(6) . ? C38 C33 1.439(6) 2_666 ? C38 H38 0.9300 . ? P1 F5 1.595(3) . ? P1 F6 1.579(3) . ? P1 F1 1.559(4) . ? P1 F2 1.577(4) . ? P1 F3 1.603(4) . ? P1 F4 1.594(4) . ? P1 F1' 1.604(7) . ? P1 F2' 1.580(9) . ? P1 F3' 1.429(13) . ? P1 F4' 1.585(9) . ? P2 F7 1.581(4) . ? P2 F8 1.587(5) . ? P2 F9 1.552(4) . ? P2 F10 1.565(4) . ? P2 F11 1.589(4) . ? P2 F12 1.564(4) . ? N7 C41 1.125(8) . ? C41 C42 1.418(8) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? N6 C39 1.152(8) . ? C39 C40 1.438(9) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 N1 C2 119.3(3) . . ? C3 N1 C6 120.5(3) . . ? C6 N1 C2 120.2(3) . . ? C3 N2 C4 119.9(3) . . ? C3 N2 C14 121.8(3) . . ? C4 N2 C14 118.3(3) . . ? C15 N3 H3 103.7 . . ? C15 N3 C31 114.7(3) . . ? C16 N3 H3 103.7 . . ? C16 N3 C15 114.5(3) . . ? C16 N3 C31 114.4(3) . . ? C31 N3 H3 103.7 . . ? C18 N4 C17 117.9(3) . . ? C18 N4 C21 121.1(4) . . ? C21 N4 C17 120.8(3) . . ? C18 N5 C19 120.3(4) . . ? C18 N5 C29 118.1(4) . . ? C19 N5 C29 121.6(4) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? N1 C2 C1 112.2(4) . . ? N1 C2 H2A 109.2 . . ? N1 C2 H2B 109.2 . . ? C1 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N1 C3 N2 125.2(3) . . ? N1 C3 H3A 117.4 . . ? N2 C3 H3A 117.4 . . ? C5 C4 N2 116.0(3) . . ? C13 C4 N2 122.0(4) . . ? C13 C4 C5 122.0(4) . . ? C4 C5 C10 118.6(4) . . ? C6 C5 C4 122.1(3) . . ? C6 C5 C10 119.3(4) . . ? C5 C6 N1 116.2(3) . . ? C7 C6 N1 122.7(4) . . ? C7 C6 C5 121.2(4) . . ? C6 C7 H7 120.2 . . ? C6 C7 C8 119.6(5) . . ? C8 C7 H7 120.2 . . ? C7 C8 H8 119.6 . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H8 119.6 . . ? C8 C9 H9 119.2 . . ? C8 C9 C10 121.5(4) . . ? C10 C9 H9 119.2 . . ? C9 C10 C5 117.7(4) . . ? C11 C10 C5 118.5(4) . . ? C11 C10 C9 123.8(4) . . ? C10 C11 H11 119.4 . . ? C12 C11 C10 121.2(4) . . ? C12 C11 H11 119.4 . . ? C11 C12 H12 119.1 . . ? C11 C12 C13 121.8(4) . . ? C13 C12 H12 119.1 . . ? C4 C13 C12 117.9(4) . . ? C4 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? N2 C14 H14A 109.0 . . ? N2 C14 H14B 109.0 . . ? N2 C14 C15 113.1(3) . . ? H14A C14 H14B 107.8 . . ? C15 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? N3 C15 C14 112.8(3) . . ? N3 C15 H15A 109.0 . . ? N3 C15 H15B 109.0 . . ? C14 C15 H15A 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? N3 C16 H16A 109.2 . . ? N3 C16 H16B 109.2 . . ? N3 C16 C17 112.1(3) . . ? H16A C16 H16B 107.9 . . ? C17 C16 H16A 109.2 . . ? C17 C16 H16B 109.2 . . ? N4 C17 C16 111.3(3) . . ? N4 C17 H17A 109.4 . . ? N4 C17 H17B 109.4 . . ? C16 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N4 C18 N5 124.3(4) . . ? N4 C18 H18 117.8 . . ? N5 C18 H18 117.8 . . ? C20 C19 N5 116.7(4) . . ? C28 C19 N5 122.5(4) . . ? C28 C19 C20 120.9(4) . . ? C19 C20 C21 121.4(4) . . ? C19 C20 C25 120.2(4) . . ? C25 C20 C21 118.4(4) . . ? N4 C21 C20 115.8(4) . . ? C22 C21 N4 123.3(4) . . ? C22 C21 C20 120.9(4) . . ? C21 C22 H22 120.2 . . ? C21 C22 C23 119.6(4) . . ? C23 C22 H22 120.2 . . ? C22 C23 H23 119.3 . . ? C24 C23 C22 121.5(5) . . ? C24 C23 H23 119.3 . . ? C23 C24 H24 120.1 . . ? C23 C24 C25 119.8(4) . . ? C25 C24 H24 120.1 . . ? C20 C25 C26 117.9(5) . . ? C24 C25 C20 119.8(4) . . ? C24 C25 C26 122.3(4) . . ? C25 C26 H26 119.9 . . ? C27 C26 C25 120.1(5) . . ? C27 C26 H26 119.9 . . ? C26 C27 H27 118.8 . . ? C26 C27 C28 122.5(5) . . ? C28 C27 H27 118.8 . . ? C19 C28 C27 118.3(5) . . ? C19 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? N5 C29 H29A 109.0 . . ? N5 C29 H29B 109.0 . . ? N5 C29 C30 113.0(4) . . ? H29A C29 H29B 107.8 . . ? C30 C29 H29A 109.0 . . ? C30 C29 H29B 109.0 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 H31A 109.7 . . ? N3 C31 H31B 109.7 . . ? N3 C31 C32 110.0(3) . . ? H31A C31 H31B 108.2 . . ? C32 C31 H31A 109.7 . . ? C32 C31 H31B 109.7 . . ? C33 C32 C31 121.3(3) . . ? C34 C32 C31 118.8(3) . . ? C34 C32 C33 119.9(3) . . ? C32 C33 C34 119.8(4) . 2_666 ? C32 C33 C38 122.8(4) . 2_666 ? C38 C33 C34 117.3(3) 2_666 2_666 ? C32 C34 C33 120.3(3) . 2_666 ? C32 C34 C35 121.8(4) . . ? C35 C34 C33 117.9(4) . 2_666 ? C34 C35 H35 119.3 . . ? C36 C35 C34 121.5(4) . . ? C36 C35 H35 119.3 . . ? C35 C36 H36 119.5 . . ? C35 C36 C37 120.9(4) . . ? C37 C36 H36 119.5 . . ? C36 C37 H37 120.0 . . ? C38 C37 C36 120.0(4) . . ? C38 C37 H37 120.0 . . ? C33 C38 H38 118.9 2_666 . ? C37 C38 C33 122.3(4) . 2_666 ? C37 C38 H38 118.9 . . ? F5 P1 F3 87.68(19) . . ? F5 P1 F1' 83.2(6) . . ? F6 P1 F5 179.01(18) . . ? F6 P1 F3 91.8(2) . . ? F6 P1 F4 91.5(2) . . ? F6 P1 F1' 96.8(6) . . ? F6 P1 F2' 87.5(6) . . ? F6 P1 F4' 94.0(6) . . ? F1 P1 F5 92.6(2) . . ? F1 P1 F6 87.9(2) . . ? F1 P1 F2 92.3(3) . . ? F1 P1 F3 177.7(3) . . ? F1 P1 F4 90.3(3) . . ? F2 P1 F5 89.9(2) . . ? F2 P1 F6 89.3(2) . . ? F2 P1 F3 90.0(2) . . ? F2 P1 F4 177.3(3) . . ? F4 P1 F5 89.3(2) . . ? F4 P1 F3 87.4(3) . . ? F2' P1 F5 91.6(6) . . ? F2' P1 F1' 83.7(8) . . ? F2' P1 F4' 159.6(8) . . ? F3' P1 F5 98.5(6) . . ? F3' P1 F6 81.7(6) . . ? F3' P1 F1' 167.5(9) . . ? F3' P1 F2' 108.6(9) . . ? F3' P1 F4' 91.7(9) . . ? F4' P1 F5 86.9(6) . . ? F4' P1 F1' 75.9(8) . . ? F7 P2 F8 88.6(3) . . ? F7 P2 F11 91.2(2) . . ? F8 P2 F11 89.5(2) . . ? F9 P2 F7 178.1(3) . . ? F9 P2 F8 89.6(3) . . ? F9 P2 F10 91.2(3) . . ? F9 P2 F11 88.6(2) . . ? F9 P2 F12 91.4(3) . . ? F10 P2 F7 90.6(3) . . ? F10 P2 F8 178.3(3) . . ? F10 P2 F11 88.9(2) . . ? F12 P2 F7 88.8(2) . . ? F12 P2 F8 88.9(3) . . ? F12 P2 F10 92.6(3) . . ? F12 P2 F11 178.4(3) . . ? N7 C41 C42 178.9(7) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N6 C39 C40 179.3(7) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C6 C7 C8 -176.4(4) . . . . ? N2 C4 C5 C6 -0.9(5) . . . . ? N2 C4 C5 C10 179.6(3) . . . . ? N2 C4 C13 C12 -179.3(4) . . . . ? N2 C14 C15 N3 -171.2(3) . . . . ? N3 C16 C17 N4 64.5(4) . . . . ? N3 C31 C32 C33 -102.1(4) . . . . ? N3 C31 C32 C34 77.7(4) . . . . ? N4 C21 C22 C23 179.6(4) . . . . ? N5 C19 C20 C21 2.3(5) . . . . ? N5 C19 C20 C25 -177.7(3) . . . . ? N5 C19 C28 C27 179.5(4) . . . . ? C2 N1 C3 N2 176.0(4) . . . . ? C2 N1 C6 C5 -173.3(4) . . . . ? C2 N1 C6 C7 5.5(6) . . . . ? C3 N1 C2 C1 -103.0(4) . . . . ? C3 N1 C6 C5 3.5(5) . . . . ? C3 N1 C6 C7 -177.8(4) . . . . ? C3 N2 C4 C5 3.6(5) . . . . ? C3 N2 C4 C13 -176.3(4) . . . . ? C3 N2 C14 C15 -16.4(5) . . . . ? C4 N2 C3 N1 -2.9(6) . . . . ? C4 N2 C14 C15 164.5(3) . . . . ? C4 C5 C6 N1 -2.5(5) . . . . ? C4 C5 C6 C7 178.7(4) . . . . ? C4 C5 C10 C9 179.7(4) . . . . ? C4 C5 C10 C11 -0.4(5) . . . . ? C5 C4 C13 C12 0.8(6) . . . . ? C5 C6 C7 C8 2.4(6) . . . . ? C5 C10 C11 C12 0.9(6) . . . . ? C6 N1 C2 C1 73.8(5) . . . . ? C6 N1 C3 N2 -0.8(6) . . . . ? C6 C5 C10 C9 0.1(5) . . . . ? C6 C5 C10 C11 -179.9(4) . . . . ? C6 C7 C8 C9 -1.3(7) . . . . ? C7 C8 C9 C10 -0.4(7) . . . . ? C8 C9 C10 C5 1.0(6) . . . . ? C8 C9 C10 C11 -179.0(4) . . . . ? C9 C10 C11 C12 -179.2(4) . . . . ? C10 C5 C6 N1 177.0(3) . . . . ? C10 C5 C6 C7 -1.8(6) . . . . ? C10 C11 C12 C13 -0.5(7) . . . . ? C11 C12 C13 C4 -0.3(6) . . . . ? C13 C4 C5 C6 179.1(4) . . . . ? C13 C4 C5 C10 -0.5(6) . . . . ? C14 N2 C3 N1 177.9(3) . . . . ? C14 N2 C4 C5 -177.2(3) . . . . ? C14 N2 C4 C13 2.9(5) . . . . ? C15 N3 C16 C17 85.3(4) . . . . ? C15 N3 C31 C32 -151.2(3) . . . . ? C16 N3 C15 C14 70.9(4) . . . . ? C16 N3 C31 C32 73.4(4) . . . . ? C17 N4 C18 N5 179.8(4) . . . . ? C17 N4 C21 C20 178.7(3) . . . . ? C17 N4 C21 C22 0.4(5) . . . . ? C18 N4 C17 C16 -97.1(4) . . . . ? C18 N4 C21 C20 -6.3(5) . . . . ? C18 N4 C21 C22 175.4(4) . . . . ? C18 N5 C19 C20 -4.4(5) . . . . ? C18 N5 C19 C28 175.6(4) . . . . ? C18 N5 C29 C30 -96.9(5) . . . . ? C19 N5 C18 N4 1.0(6) . . . . ? C19 N5 C29 C30 81.5(5) . . . . ? C19 C20 C21 N4 2.8(5) . . . . ? C19 C20 C21 C22 -178.8(4) . . . . ? C19 C20 C25 C24 178.3(4) . . . . ? C19 C20 C25 C26 -3.2(6) . . . . ? C20 C19 C28 C27 -0.6(7) . . . . ? C20 C21 C22 C23 1.3(6) . . . . ? C20 C25 C26 C27 2.3(7) . . . . ? C21 N4 C17 C16 78.1(4) . . . . ? C21 N4 C18 N5 4.6(6) . . . . ? C21 C20 C25 C24 -1.7(6) . . . . ? C21 C20 C25 C26 176.8(4) . . . . ? C21 C22 C23 C24 -3.4(7) . . . . ? C22 C23 C24 C25 2.8(7) . . . . ? C23 C24 C25 C20 -0.2(6) . . . . ? C23 C24 C25 C26 -178.6(4) . . . . ? C24 C25 C26 C27 -179.2(5) . . . . ? C25 C20 C21 N4 -177.2(3) . . . . ? C25 C20 C21 C22 1.2(6) . . . . ? C25 C26 C27 C28 -0.6(8) . . . . ? C26 C27 C28 C19 -0.3(7) . . . . ? C28 C19 C20 C21 -177.6(4) . . . . ? C28 C19 C20 C25 2.4(6) . . . . ? C29 N5 C18 N4 179.4(4) . . . . ? C29 N5 C19 C20 177.3(3) . . . . ? C29 N5 C19 C28 -2.8(6) . . . . ? C31 N3 C15 C14 -64.4(4) . . . . ? C31 N3 C16 C17 -139.3(3) . . . . ? C31 C32 C33 C34 178.7(3) . . . 2_666 ? C31 C32 C33 C38 0.7(5) . . . 2_666 ? C31 C32 C34 C33 -178.7(3) . . . 2_666 ? C31 C32 C34 C35 2.1(5) . . . . ? C32 C34 C35 C36 177.1(4) . . . . ? C33 C32 C34 C33 1.0(6) . . . 2_666 ? C33 C32 C34 C35 -178.1(3) . . . . ? C33 C34 C35 C36 -2.1(6) 2_666 . . . ? C34 C32 C33 C34 -1.0(6) . . . 2_666 ? C34 C32 C33 C38 -179.0(3) . . . 2_666 ? C34 C35 C36 C37 1.9(6) . . . . ? C35 C36 C37 C38 0.4(6) . . . . ? C36 C37 C38 C33 -2.5(6) . . . 2_666 ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 -2 51.78 1.23 0 0 -3 1686.31 8.64 0 0 -3 1695.81 8.11 0 0 -4 106.3 2.64 0 0 -4 104.49 2.44 0 0 -5 264.72 4.21 0 0 -5 283.18 4.66 0 0 -6 3.34 0.93 0 0 -6 2.74 0.98 0 0 -7 10.65 1.26 0 0 -7 9.76 1.32 0 0 -8 -0.26 1.43 0 0 -8 0.36 0.87 0 0 -8 0.12 1.06 0 0 -9 3.02 1.26 0 0 -9 3.26 1.74 0 0 -10 0.92 1.66 0 0 -11 1.04 1.78 0 0 -11 0.9 0.86 0 0 -11 0.68 0.87 0 0 -12 31.38 1.82 0 0 -12 29.89 1.74 0 0 -12 29.54 3.52 0 0 -13 1.62 1.05 0 0 -13 0.91 0.98 0 0 -14 1.48 1 0 0 -14 0.9 1.09 0 0 -15 1.26 0.98 0 0 -15 1.1 0.97 0 0 -16 0.74 0.8 0 0 -16 1.04 0.89 0 0 -17 2.53 0.7 0 0 -17 1.26 0.66 0 0 -18 -0.12 0.48 0 1 -18 6.08 0.65 0 1 -17 0.47 0.68 0 1 -16 2.12 0.93 0 1 -16 2.32 0.91 0 1 -15 0.45 0.94 0 1 -15 0.71 0.96 0 1 -14 1.19 1.02 0 1 -14 0.85 1.06 0 1 -13 11.53 1.35 0 1 -13 12.01 1.38 0 1 -12 2.89 1.08 0 1 -12 2.92 2.11 0 1 -12 2.56 1.07 0 1 -11 15.16 1.41 0 1 -11 14.47 2.67 0 1 -11 15.19 1.34 0 1 -10 167.58 6.74 0 1 -9 320.34 6.99 0 1 -9 269.66 6.1 0 1 -8 123.86 3.9 0 1 -8 135.26 4.37 0 1 -7 84.34 3.16 0 1 -7 83.72 3.33 0 1 -6 2.61 1.03 0 1 -5 115.65 3.87 0 1 -5 110.4 3.16 0 1 -4 2092.06 14.16 0 1 -3 24.49 1.68 0 1 -2 29.63 1.46 0 1 -1 65.86 1.5 0 -1 0 346.65 2.87 0 1 0 345.82 2.86 0 -1 -1 68.18 1.43 0 -1 -1 69.83 1.43 0 -1 -1 70.44 1.25 0 -1 -2 255.46 3.06 0 -1 -2 263.87 3.49 0 -1 -2 254.36 3.04 0 -1 -2 259.95 2.67 0 -1 -3 35.91 1.44 0 -1 -3 37.51 1.28 0 -1 -3 35.77 1.67 0 -1 -4 103.47 3.11 0 -1 -4 103.84 2.62 0 -1 -4 102.6 2.33 0 -1 -5 2.22 0.91 0 -1 -5 -0.05 1.18 0 -1 -5 0.3 0.75 0 -1 -6 32.44 1.93 0 -1 -6 31.78 2.37 0 -1 -6 34.28 1.75 0 -1 -7 1.8 1.33 0 -1 -7 1.29 0.98 0 -1 -7 1.53 0.88 0 -1 -8 29.14 1.84 0 -1 -8 32.16 2.22 0 -1 -8 27.52 2.59 0 -1 -9 0.61 1.59 0 -1 -10 104.01 2.7 0 -1 -10 99.53 2.62 0 -1 -10 98.6 5.28 0 -1 -11 20.04 2.87 0 -1 -11 22.27 1.54 0 -1 -11 21.69 1.49 0 -1 -12 9.32 1.2 0 -1 -12 9.4 1.34 0 -1 -12 10.99 2.49 0 -1 -13 34.29 1.97 0 -1 -13 32.08 1.8 0 -1 -14 0.07 0.88 0 -1 -14 -0.25 1.08 0 -1 -15 4.67 1.2 0 -1 -15 3.85 0.97 0 -1 -16 5.44 1.04 0 -1 -16 5.53 0.92 0 -1 -17 -0.47 0.6 0 -1 -17 0.15 0.54 0 -1 -17 -0.2 0.71 0 -1 -18 2.3 0.46 0 2 -18 4.72 0.61 0 2 -17 0.89 0.74 0 2 -16 10.05 1.22 0 2 -15 2.17 1.06 0 2 -15 2.35 0.94 0 2 -14 9.12 1.24 0 2 -14 8.96 1.35 0 2 -13 12.86 1.44 0 2 -13 11.52 1.32 0 2 -12 0.34 1.02 0 2 -12 0.17 0.92 0 2 -12 0.44 1.79 0 2 -11 63.64 2.29 0 2 -11 67.74 2.38 0 2 -11 62.43 4.66 0 2 -10 0.83 0.82 0 2 -9 18.61 2.18 0 2 -9 15.76 1.93 0 2 -8 2.98 1.24 0 2 -8 4.1 1.52 0 2 -7 72.39 3.37 0 2 -6 68.8 3.66 0 2 -5 61.8 3.29 0 2 -4 91.83 3.52 0 2 -3 0.61 1.31 0 2 -2 815.24 7.39 0 2 -1 142.11 2.78 0 2 0 2.01 0.73 0 -2 -1 1530.33 8.74 0 -2 -2 537.16 5.36 0 -2 -2 551.37 5.82 0 -2 -2 544.7 5.69 0 -2 -3 4.01 0.83 0 -2 -3 3.84 1.03 0 -2 -3 3.56 1.02 0 -2 -3 4.11 1.19 0 -2 -4 181.46 4.27 0 -2 -4 184.6 3.32 0 -2 -4 173.9 3.75 0 -2 -5 78.08 2.4 0 -2 -5 74.55 2.71 0 -2 -5 78.71 3.24 0 -2 -6 21.64 1.75 0 -2 -6 23.18 1.51 0 -2 -6 20.93 2.06 0 -2 -7 43.33 2.91 0 -2 -7 46.7 2.07 0 -2 -7 46.83 2.53 0 -2 -8 60.44 3.66 0 -2 -8 70.19 3.21 0 -2 -9 10.94 2.19 0 -2 -10 109.55 5.56 0 -2 -10 111.97 2.82 0 -2 -11 8.65 1.1 0 -2 -11 7.13 1.12 0 -2 -11 7.66 1.18 0 -2 -11 7.25 2.11 0 -2 -12 3.04 1.15 0 -2 -12 2.79 0.94 0 -2 -12 1.85 1.73 0 -2 -13 2.31 0.92 0 -2 -13 2.71 1.2 0 -2 -14 17.24 1.33 0 -2 -14 17.96 1.68 0 -2 -15 0.66 1.06 0 -2 -15 0.62 0.74 0 -2 -16 2.49 0.97 0 -2 -16 2.4 0.73 0 -2 -17 0.05 0.67 0 -2 -17 0.41 0.52 0 3 -18 -0.12 0.49 0 3 -18 1.37 0.55 0 3 -17 0.44 0.74 0 3 -16 17.47 1.4 0 3 -15 -0.11 1.06 0 3 -14 0.24 1.07 0 3 -13 3.9 1.22 0 3 -13 4.08 1.03 0 3 -12 10.3 1.25 0 3 -12 11.05 1.42 0 3 -12 9.4 2.62 0 3 -11 32.78 1.84 0 3 -11 29.14 1.64 0 3 -10 18.2 1.45 0 3 -10 17.28 1.3 0 3 -10 16.28 2.16 0 3 -9 127.85 5.21 0 3 -8 1.19 1.25 0 3 -7 211.77 6.84 0 3 -6 8.99 2.1 0 3 -5 183.28 5.52 0 3 -4 6.58 1.72 0 3 -3 29.87 2.29 0 3 -2 522.69 6.89 0 3 -1 233.86 4.3 0 3 0 530.27 6.27 0 -3 -1 781.22 7.85 0 -3 -2 2.72 1.14 0 -3 -3 6.55 1.22 0 -3 -3 7.75 1.43 0 -3 -3 7.73 1.23 0 -3 -4 98.76 3.19 0 -3 -4 96.19 3.43 0 -3 -4 94.39 3.29 0 -3 -5 0.69 1.17 0 -3 -5 0.43 1.08 0 -3 -6 130.26 4.61 0 -3 -6 141.24 4.37 0 -3 -7 5.29 1.45 0 -3 -7 4.56 1.59 0 -3 -8 85.37 3.8 0 -3 -8 66.35 3.91 0 -3 -9 107.68 5.22 0 -3 -10 4.98 1.84 0 -3 -10 4.35 0.92 0 -3 -10 4.37 1 0 -3 -11 5.65 1.1 0 -3 -11 5.76 1.93 0 -3 -11 5.77 1.17 0 -3 -12 16.36 1.48 0 -3 -12 16.8 1.57 0 -3 -13 4.13 1.21 0 -3 -14 10.43 1.43 0 -3 -14 7.8 0.93 0 -3 -15 -0.2 0.68 0 -3 -15 0.26 1.02 0 -3 -16 0.38 0.86 0 -3 -16 0.41 0.57 0 -3 -17 10.61 0.94 0 4 -18 2.96 0.52 0 4 -18 1.91 0.45 0 4 -17 7.32 0.91 0 4 -16 1.01 0.88 0 4 -15 42.47 2.05 0 4 -14 62.69 2.54 0 4 -13 0.25 1.05 0 4 -12 40.39 2.08 0 4 -11 0.32 0.97 0 4 -10 28.42 1.64 0 4 -10 27.14 1.5 0 4 -10 29.37 3.01 0 4 -10 29.32 3.2 0 4 -9 174.97 6.54 0 4 -8 35.51 3.64 0 4 -7 113.75 5.44 0 4 -6 154.56 5.81 0 4 -5 26.54 2.77 0 4 -4 2.86 1.67 0 4 -3 255.08 5.86 0 4 -2 8.13 1.58 0 4 -1 6.76 1.41 0 4 0 0.91 1.19 0 4 1 49.29 2.5 0 -4 -2 10.84 1.62 0 -4 -3 0.67 1.01 0 -4 -3 0.7 1 0 -4 -4 12.95 1.73 0 -4 -4 13.78 1.66 0 -4 -5 25.5 2.23 0 -4 -6 3.19 1.35 0 -4 -7 33.03 2.85 0 -4 -8 152.29 5.96 0 -4 -9 45.76 3.69 0 -4 -9 47.79 1.81 0 -4 -9 47.19 1.92 0 -4 -10 0.78 1.49 0 -4 -10 0.43 0.81 0 -4 -10 -0.1 0.91 0 -4 -11 5.59 1.04 0 -4 -11 4.17 1.86 0 -4 -11 5.29 1.13 0 -4 -12 -0.75 1.12 0 -4 -12 -0.04 0.94 0 -4 -12 0.77 0.9 0 -4 -12 -0.68 0.79 0 -4 -13 3.5 0.77 0 -4 -13 4.4 1.21 0 -4 -14 2.82 0.7 0 -4 -14 4.45 1.12 0 -4 -15 5.68 1.11 0 -4 -16 7.23 0.96 0 -4 -17 0.82 0.6 0 -5 17 6.06 0.81 0 5 -17 3.33 0.64 0 5 -16 2.36 0.83 0 5 -15 37.22 1.86 0 5 -14 0.65 1.04 0 5 -13 3.61 1.18 0 5 -12 33.33 1.95 0 5 -11 3.19 1.03 0 5 -10 92.83 5.37 0 5 -10 90.93 2.73 0 5 -9 0.01 1.58 0 5 -9 0.44 2.34 0 5 -9 0.46 0.77 0 5 -8 1.29 2.21 0 5 -7 206.89 7.66 0 5 -6 5.4 2.29 0 5 -5 0.57 1.78 0 5 -4 9.48 2.17 0 5 -3 92.92 4.13 0 5 -2 32.15 2.54 0 5 -1 601.23 8.99 0 5 0 0.05 1.21 0 5 1 4.5 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1.74 0.94 -12 1 -7 -0.01 0.77 -12 1 -8 1.22 0.63 12 0 -11 -0.36 0.46 12 0 -10 0.45 0.56 12 0 -9 1.15 0.69 12 0 -8 1.13 0.78 12 0 -7 -0.73 0.67 12 0 -7 0.01 0.82 12 0 -6 3.73 0.94 12 0 -6 3.32 0.72 12 0 -5 0.84 0.89 12 0 -5 1.22 0.75 12 0 -4 0.1 0.92 12 0 -4 0.92 0.81 12 0 -3 0.44 0.9 12 0 -3 0.77 0.9 12 0 -2 -0.32 0.98 12 0 -2 0.53 0.92 12 0 -1 4.2 1.07 12 0 0 4.84 1.12 12 0 1 0.24 1.01 12 0 2 0.58 0.98 12 0 3 1.62 0.95 12 0 4 -1.16 0.69 -12 0 -4 0.1 1.03 -12 0 -5 0.86 0.95 -12 0 -6 0.57 0.8 -12 0 -7 0 0.66 -12 0 -8 1.7 0.54 12 1 -10 1.48 0.5 12 1 -9 0.21 0.55 12 1 -8 1.88 0.67 12 1 -7 1.61 0.62 12 1 -7 3.65 0.79 12 1 -6 -0.46 0.77 12 1 -6 0.04 0.6 12 1 -5 -0.58 0.82 12 1 -5 -0.45 0.73 12 1 -4 -0.14 0.81 12 1 -4 0.33 0.78 12 1 -3 5.07 0.96 12 1 -3 5.49 1.03 12 1 -2 0.94 0.92 12 1 -1 0.74 0.94 12 1 0 -0.37 0.95 12 1 1 3.14 0.99 12 1 2 3.75 0.98 12 1 3 4.15 0.93 12 1 4 -1.12 0.6 -12 -1 -4 -0.15 0.85 -12 -1 -5 0.57 0.8 -12 -1 -6 1.49 0.7 -12 -1 -7 3.02 0.6 12 2 -9 0.54 0.46 12 2 -8 2.8 0.6 12 2 -7 17.14 0.95 12 2 -6 1.95 0.67 12 2 -6 2.51 0.65 12 2 -5 -0.54 0.67 12 2 -5 -0.3 0.68 12 2 -4 0.36 0.68 12 2 -4 0.32 0.72 12 2 -3 0.86 0.81 12 2 -2 0.37 0.82 12 2 -1 1.83 0.9 12 2 0 1.09 0.85 12 2 1 1.21 0.83 12 2 2 1.65 0.78 12 2 3 0.64 0.68 -12 -2 -3 0.45 0.79 -12 -2 -4 0.27 0.74 -12 -2 -5 1.67 0.68 12 3 -6 0.41 0.51 12 3 -5 2.61 0.68 12 3 -4 1.75 0.7 12 3 -3 -0.4 0.72 12 3 -2 3.41 0.82 12 3 -1 0.25 0.72 12 3 0 1.3 0.78 12 3 1 5.84 0.84 12 3 2 0.89 0.64 -12 -3 -2 0.82 0.72 -12 -3 -3 0.18 0.61 -12 -3 -4 3.46 0.6 12 4 -5 3.04 0.55 12 4 -4 2.76 0.6 12 4 -3 3.18 0.65 12 4 -2 5.08 0.71 12 4 -1 0.45 0.59 12 4 0 7.48 0.74 12 4 1 0.1 0.5 -12 -4 -1 0.36 0.53 13 -11 -2 1.46 0.5 13 -11 -1 -0.25 0.49 13 -11 0 -0.06 0.49 13 -10 -4 -0.8 0.54 13 -10 -3 2 0.62 13 -10 -2 1.35 0.64 13 -10 -1 1.63 0.69 13 -10 0 3.44 0.68 13 -10 1 1.69 0.59 13 -10 2 -0.68 0.54 13 -9 -5 2.24 0.59 13 -9 -4 1.77 0.67 13 -9 -3 0.75 0.7 13 -9 -2 1.83 0.77 13 -9 -1 0.69 0.73 13 -9 0 -0.06 0.71 13 -9 1 1.76 0.74 13 -9 2 1.75 0.66 13 -9 3 2.46 0.59 13 -8 -7 10.42 0.85 13 -8 -6 13.64 0.78 13 -8 -5 2.75 0.7 13 -8 -4 2.24 0.75 13 -8 -3 0.53 0.78 13 -8 -2 8.36 1.03 13 -8 -1 -0.14 0.88 13 -8 0 7.1 0.99 13 -8 1 -0.84 0.79 13 -8 2 -0.28 0.69 13 -8 3 2.74 0.68 13 -8 4 1.16 0.52 13 -7 -8 4.1 0.7 13 -7 -7 3.57 0.8 13 -7 -6 -0.14 0.6 13 -7 -6 4.69 0.88 13 -7 -5 -0.13 0.73 13 -7 -5 4.74 0.97 13 -7 -4 2 0.84 13 -7 -3 -1.59 1 13 -7 -1 4.91 1.03 13 -7 0 -0.55 0.96 13 -7 1 7.52 1 13 -7 2 -0.66 0.78 13 -7 3 -0.28 0.67 13 -7 4 -0.02 0.55 13 -7 5 6.53 0.62 13 -6 -8 2.34 0.65 13 -6 -7 -0.06 0.51 13 -6 -7 2.7 0.75 13 -6 -6 0.33 0.67 13 -6 -6 4.24 0.87 13 -6 -5 2.69 0.81 13 -6 -5 7.49 0.98 13 -6 -4 6.3 0.97 13 -6 -3 3.95 0.98 13 -6 -2 7.89 1.12 13 -6 -1 5.52 1.09 13 -6 0 22.43 1.43 13 -6 1 13.48 1.2 13 -6 2 -1.6 0.87 13 -6 3 -1.39 0.77 13 -6 3 0.61 0.55 13 -6 4 -0.36 0.61 13 -6 4 0.44 0.56 13 -6 5 1.7 0.59 13 -6 6 0.14 0.5 13 -5 -8 2.68 0.65 13 -5 -7 -0.89 0.59 13 -5 -7 2.29 0.73 13 -5 -6 0.04 0.66 13 -5 -6 3.11 0.8 13 -5 -5 2.92 0.82 13 -5 -5 4.48 0.9 13 -5 -4 1.87 0.89 13 -5 -3 0.35 0.92 13 -5 -2 3.57 1.01 13 -5 -1 2.87 1.04 13 -5 0 0.93 0.91 13 -5 1 4.83 0.99 13 -5 2 4.26 0.88 -13 5 -2 2.81 0.75 13 -5 3 3.16 0.76 -13 5 -3 1.61 0.69 13 -5 4 -1.75 0.7 13 -5 4 -0.13 0.6 -13 5 -4 -0.12 0.59 13 -5 5 0.22 0.61 -13 5 -5 0.14 0.54 13 -5 6 0.69 0.56 -13 5 -6 0.98 0.5 13 -5 7 0.35 0.47 13 -4 -8 1.32 0.55 13 -4 -7 0.31 0.56 13 -4 -7 0.51 0.59 13 -4 -6 1.99 0.71 13 -4 -6 0.59 0.69 13 -4 -5 1.06 0.77 13 -4 -5 -0.19 0.72 13 -4 -4 0.02 0.83 13 -4 -3 0.48 0.91 13 -4 -2 1.16 0.96 13 -4 -1 2.1 0.98 13 -4 0 -0.14 0.9 13 -4 1 0.09 0.83 -13 4 -1 -0.05 0.76 13 -4 2 0.81 0.78 -13 4 -2 0.63 0.77 13 -4 3 1.53 0.71 -13 4 -3 0.64 0.74 13 -4 4 2.72 0.64 -13 4 -4 1.74 0.74 -13 4 -5 1.09 0.66 13 -4 6 0.86 0.59 -13 4 -6 0.85 0.57 13 -4 7 0.53 0.49 13 -3 -9 -0.17 0.49 13 -3 -8 -0.52 0.6 13 -3 -7 1.72 0.58 13 -3 -7 0.5 0.65 13 -3 -6 0.56 0.66 13 -3 -6 -0.08 0.73 13 -3 -5 0.3 0.76 13 -3 -5 0.11 0.75 13 -3 -4 2.58 0.87 13 -3 -3 -0.46 0.91 13 -3 -2 -0.61 0.95 13 -3 -1 2.23 0.97 13 -3 0 -0.88 0.95 13 -3 1 3.87 0.91 13 -3 2 -0.3 0.73 -13 3 -2 -0.04 0.82 13 -3 3 2.68 0.74 -13 3 -3 2.75 0.91 13 -3 4 2.41 0.61 -13 3 -4 1.72 0.81 -13 3 -5 0.49 0.7 -13 3 -6 -0.25 0.59 13 -3 7 0.17 0.46 -13 3 -7 0.22 0.47 13 -2 -9 -0.15 0.5 13 -2 -8 1.32 0.62 13 -2 -7 0.9 0.54 13 -2 -7 0.06 0.62 13 -2 -6 0.13 0.63 13 -2 -6 0.03 0.69 13 -2 -5 -0.39 0.74 13 -2 -5 -0.46 0.82 13 -2 -4 -1.02 0.89 13 -2 -4 -0.14 0.82 13 -2 -3 -0.48 0.91 13 -2 -2 3.14 0.97 13 -2 -1 2.33 0.94 13 -2 0 2.06 0.9 13 -2 1 4.1 0.89 13 -2 2 0.43 0.7 -13 2 -2 0.23 0.86 13 -2 3 1.43 0.65 -13 2 -3 1.23 0.89 13 -2 4 8.65 0.72 -13 2 -4 7.66 0.99 -13 2 -5 0.1 0.7 -13 2 -6 3.79 0.69 13 -2 7 4.04 0.56 13 -1 -9 4 0.55 13 -1 -8 -0.12 0.58 13 -1 -7 -0.4 0.49 13 -1 -7 -0.12 0.65 13 -1 -6 -0.33 0.61 13 -1 -6 -0.19 0.72 13 -1 -5 -0.99 0.73 13 -1 -5 -0.29 0.73 13 -1 -4 -0.29 0.8 13 -1 -4 1.2 0.66 13 -1 -3 -0.13 0.87 13 -1 -3 1.42 0.75 13 -1 -2 -0.25 0.89 13 -1 -2 1.06 0.77 13 -1 -1 -1.08 0.92 13 -1 -1 0.39 0.8 13 -1 0 2.06 0.86 13 -1 1 -0.25 0.77 13 -1 2 3.6 0.75 -13 1 -2 3.6 0.99 13 -1 3 3.98 0.67 -13 1 -3 3.73 0.94 -13 1 -4 2.22 0.79 -13 1 -5 0.24 0.66 -13 1 -6 2.58 0.6 13 0 -8 0.19 0.5 13 0 -7 2.77 0.65 13 0 -6 -0.13 0.55 13 0 -6 0.42 0.63 13 0 -5 -1.14 0.68 13 0 -5 -0.23 0.64 13 0 -5 0.1 0.51 13 0 -4 -0.64 0.74 13 0 -4 -0.24 0.6 13 0 -3 3.36 0.78 13 0 -2 1.84 0.77 13 0 -1 19 1.24 13 0 0 2.66 0.84 13 0 1 -0.14 0.7 13 0 2 6.47 0.76 -13 0 -2 6.4 1.03 13 0 3 0.17 0.5 -13 0 -3 0.83 0.77 -13 0 -4 3.81 0.77 -13 0 -5 0.99 0.58 13 1 -6 -0.28 0.47 13 1 -5 0.06 0.55 13 1 -5 0.8 0.5 13 1 -4 0.58 0.58 13 1 -3 0.79 0.65 13 1 -2 3.26 0.77 13 1 -1 2.43 0.72 13 1 0 -0.18 0.66 13 1 1 2.04 0.64 13 1 2 3.24 0.57 -13 -1 -2 4.18 0.84 -13 -1 -3 0.6 0.64 -13 -1 -4 4.6 0.66 13 2 -5 -0.69 0.47 13 2 -4 1.14 0.51 13 2 -3 1.69 0.59 13 2 -2 4.3 0.67 13 2 -1 1.39 0.62 13 2 0 3.76 0.68 13 2 1 1.58 0.5 -13 -2 -1 2.47 0.66 -13 -2 -2 6.48 0.71 14 -9 -2 1.99 0.51 14 -9 -1 2.25 0.53 14 -9 0 1.92 0.5 14 -8 -4 2.39 0.52 14 -8 -3 6.03 0.66 14 -8 -2 0.23 0.58 14 -8 -1 1.3 0.6 14 -8 0 1.22 0.58 14 -8 1 5.14 0.62 14 -7 -4 -0.38 0.56 14 -7 -3 5.98 0.76 14 -7 -2 1.99 0.69 14 -7 -1 -0.41 0.66 14 -7 0 -0.2 0.64 14 -7 1 0.06 0.59 14 -7 2 0.76 0.51 14 -6 -5 -1.04 0.55 14 -6 -4 -1 0.65 14 -6 -3 -1.98 0.75 14 -6 -2 1.33 0.69 14 -6 -1 -0.29 0.76 14 -6 0 5.43 0.8 14 -6 1 -1.49 0.69 14 -6 2 -0.69 0.57 14 -5 -4 -1.59 0.68 14 -5 -3 3.01 0.71 14 -5 -2 3.02 0.74 14 -5 -1 3.29 0.75 14 -5 0 1.7 0.72 14 -5 1 -1.37 0.67 14 -5 2 -1.2 0.61 14 -4 -5 1.74 0.56 14 -4 -4 1.22 0.64 14 -4 -3 1.29 0.7 14 -4 -2 1.44 0.7 14 -4 -1 1.03 0.71 14 -4 0 0.69 0.66 -14 4 0 -0.06 0.53 14 -4 1 0.67 0.62 -14 4 -1 0.19 0.53 14 -4 2 1.02 0.53 -14 4 -2 0.06 0.49 14 -3 -5 1.21 0.54 14 -3 -4 0.78 0.6 14 -3 -3 0.22 0.62 14 -3 -2 0.03 0.65 14 -3 -1 0.44 0.65 -14 3 1 -0.53 0.61 14 -3 0 0.25 0.61 -14 3 0 0.74 0.6 14 -3 1 2.59 0.64 -14 3 -1 1.25 0.61 14 -3 2 2.07 0.54 -14 3 -2 1.27 0.58 -14 3 -3 1.18 0.52 14 -2 -5 0.49 0.49 14 -2 -4 2.67 0.62 14 -2 -3 0.88 0.61 14 -2 -2 -0.12 0.64 14 -2 -1 -0.29 0.63 14 -2 0 0.35 0.6 -14 2 0 0.1 0.6 14 -2 1 0.75 0.55 -14 2 -1 0.75 0.62 14 -2 2 0.8 0.47 -14 2 -2 0.12 0.56 -14 2 -3 1.26 0.52 14 -1 -4 0.07 0.48 14 -1 -3 0.26 0.54 14 -1 -2 0.51 0.57 14 -1 -1 9.47 0.78 14 -1 0 1.32 0.56 -14 1 0 1.15 0.65 14 -1 1 0.3 0.46 -14 1 -1 0.57 0.58 -14 1 -2 0.63 0.54 14 0 -3 0.14 0.45 14 0 -2 -0.12 0.47 14 0 -1 2.19 0.52 -14 0 1 1.86 0.6 -14 0 0 0.9 0.55 _iucr_refine_instructions_details ; a150923b.res created by SHELXL-2014/7 TITL a150923b_a.res in P-1 REM Old TITL A150923B in P-1 #2 REM SHELXT solution in P-1 REM R1 0.246, Rweak 0.025, Alpha 0.062, Orientation as input REM Formula found by SHELXT: C54 N7 Cl2 CELL 1.54184 11.850652 12.401176 14.951227 92.4013 94.3109 107.3439 ZERR 1 0.000477 0.000556 0.000542 0.0033 0.0031 0.0038 LATT 1 SFAC C H F N P UNIT 84 90 24 14 4 DFIX 1.56 0.01 P1 F4' P1 F4 P1 F2 P1 F3 P1 F2' P1 F2 P1 F1' P1 F1 DFIX 1.56 0.01 P1 F1' ISOR 0.01 0.02 F1' F1 F4' F4 ISOR 0.005 0.002 F1' F1 EADP F2 F3 EADP F4 F4' EADP F1 F1' EADP F2 F2' EADP F3' F3 L.S. 20 PLAN 20 BOND $H LIST 4 MORE -1 CONF fmap 2 acta SHEL 999 0.837 REM REM REM WGHT 0.122400 0.874000 FVAR 0.25433 0.77017 N1 4 0.760810 0.129572 0.941851 11.00000 0.04659 0.02844 = 0.03672 0.00653 0.00122 0.01181 N2 4 0.600520 0.114963 0.836785 11.00000 0.04071 0.02795 = 0.03413 0.00810 0.00245 0.00872 N3 4 0.529718 0.348568 0.705942 11.00000 0.04471 0.03219 = 0.02738 0.01254 0.00938 0.01534 AFIX 13 H3 2 0.577770 0.428336 0.710061 11.00000 -1.20000 AFIX 0 N4 4 0.474448 0.560788 0.756486 11.00000 0.04950 0.03732 = 0.03364 0.00514 0.00625 0.02132 N5 4 0.637483 0.710532 0.729015 11.00000 0.05390 0.03886 = 0.04076 0.00154 0.00850 0.01584 C1 1 0.976094 0.148517 0.941904 11.00000 0.04673 0.04720 = 0.06754 0.01232 -0.00734 0.00919 AFIX 137 H1A 2 0.973916 0.152604 0.877847 11.00000 -1.50000 H1B 2 0.960074 0.070990 0.956329 11.00000 -1.50000 H1C 2 1.053229 0.191790 0.969028 11.00000 -1.50000 AFIX 0 C2 1 0.882724 0.196306 0.977559 11.00000 0.05755 0.03506 = 0.05382 0.00564 -0.01400 0.00700 AFIX 23 H2A 2 0.889106 0.197083 1.042659 11.00000 -1.20000 H2B 2 0.897805 0.273860 0.961161 11.00000 -1.20000 AFIX 0 C3 1 0.705839 0.168679 0.877566 11.00000 0.03971 0.02773 = 0.03689 0.00578 0.00375 0.00798 AFIX 43 H3A 2 0.744361 0.240090 0.859331 11.00000 -1.20000 AFIX 0 C4 1 0.539367 0.002502 0.859070 11.00000 0.04277 0.02544 = 0.03906 0.00335 0.01283 0.00929 C5 1 0.596010 -0.041103 0.929348 11.00000 0.05012 0.03073 = 0.03672 0.00927 0.01765 0.01561 C6 1 0.706547 0.021456 0.973936 11.00000 0.05216 0.03022 = 0.03391 0.00687 0.01053 0.01482 C7 1 0.758811 -0.021589 1.043191 11.00000 0.05923 0.04837 = 0.03852 0.01048 0.00836 0.02234 AFIX 43 H7 2 0.830460 0.021793 1.073480 11.00000 -1.20000 AFIX 0 C8 1 0.703572 -0.131052 1.067836 11.00000 0.07556 0.05220 = 0.04512 0.02423 0.01865 0.03384 AFIX 43 H8 2 0.739651 -0.160808 1.113926 11.00000 -1.20000 AFIX 0 C9 1 0.597774 -0.194432 1.025203 11.00000 0.07700 0.04105 = 0.05528 0.02632 0.03240 0.02602 AFIX 43 H9 2 0.562957 -0.267205 1.042472 11.00000 -1.20000 AFIX 0 C10 1 0.539180 -0.152190 0.954961 11.00000 0.06031 0.03047 = 0.05027 0.00953 0.02627 0.01875 C11 1 0.428855 -0.213526 0.909624 11.00000 0.06292 0.02822 = 0.06037 0.00953 0.02723 0.00967 AFIX 43 H11 2 0.390228 -0.285780 0.926194 11.00000 -1.20000 AFIX 0 C12 1 0.378058 -0.169363 0.842492 11.00000 0.04455 0.03371 = 0.06388 -0.00328 0.01704 0.00339 AFIX 43 H12 2 0.305346 -0.212285 0.813487 11.00000 -1.20000 AFIX 0 C13 1 0.432644 -0.059095 0.814933 11.00000 0.04548 0.03374 = 0.04622 0.00170 0.01130 0.01104 AFIX 43 H13 2 0.397014 -0.029670 0.768377 11.00000 -1.20000 AFIX 0 C14 1 0.541679 0.167751 0.765444 11.00000 0.04473 0.02842 = 0.02678 0.00968 0.00076 0.01024 AFIX 23 H14A 2 0.458325 0.151640 0.774834 11.00000 -1.20000 H14B 2 0.546548 0.133232 0.707007 11.00000 -1.20000 AFIX 0 C15 1 0.597569 0.295751 0.765343 11.00000 0.04169 0.03256 = 0.03223 0.00999 0.00432 0.01154 AFIX 23 H15A 2 0.603889 0.329139 0.826059 11.00000 -1.20000 H15B 2 0.677222 0.311491 0.746717 11.00000 -1.20000 AFIX 0 C16 1 0.418091 0.351720 0.736991 11.00000 0.04522 0.03975 = 0.03275 0.01248 0.00512 0.01197 AFIX 23 H16A 2 0.383465 0.283193 0.766824 11.00000 -1.20000 H16B 2 0.363755 0.353720 0.685667 11.00000 -1.20000 AFIX 0 C17 1 0.432954 0.453837 0.801524 11.00000 0.05131 0.04749 = 0.02967 0.01207 0.00981 0.02067 AFIX 23 H17A 2 0.357632 0.448834 0.825095 11.00000 -1.20000 H17B 2 0.489832 0.453783 0.851675 11.00000 -1.20000 AFIX 0 C18 1 0.588491 0.615067 0.765497 11.00000 0.05473 0.03989 = 0.03526 0.00066 0.00537 0.02369 AFIX 43 H18 2 0.637978 0.583949 0.799986 11.00000 -1.20000 AFIX 0 C19 1 0.565981 0.763036 0.676741 11.00000 0.06458 0.03948 = 0.03274 0.00210 0.00724 0.01946 C20 1 0.443837 0.703591 0.661578 11.00000 0.05820 0.04205 = 0.02844 0.00413 0.00974 0.02690 C21 1 0.394451 0.598526 0.699627 11.00000 0.05292 0.04239 = 0.03038 0.00371 0.00782 0.02569 C22 1 0.276175 0.540640 0.683161 11.00000 0.05215 0.05157 = 0.03896 0.00517 0.01105 0.02570 AFIX 43 H22 2 0.244420 0.472754 0.709374 11.00000 -1.20000 AFIX 0 C23 1 0.203488 0.584153 0.626755 11.00000 0.05417 0.07221 = 0.04316 0.00465 0.00480 0.03206 AFIX 43 H23 2 0.124118 0.542571 0.613260 11.00000 -1.20000 AFIX 0 C24 1 0.246381 0.686533 0.590911 11.00000 0.06672 0.07578 = 0.03759 0.01056 0.00509 0.04324 AFIX 43 H24 2 0.195662 0.715424 0.555600 11.00000 -1.20000 AFIX 0 C25 1 0.367281 0.747957 0.607573 11.00000 0.07663 0.05450 = 0.02841 0.00629 0.00763 0.03649 C26 1 0.416181 0.855542 0.573764 11.00000 0.09613 0.05638 = 0.03726 0.01668 0.00692 0.03920 AFIX 43 H26 2 0.367526 0.888178 0.539908 11.00000 -1.20000 AFIX 0 C27 1 0.533826 0.910962 0.590714 11.00000 0.10407 0.04903 = 0.04463 0.01843 0.01087 0.02339 AFIX 43 H27 2 0.564264 0.981092 0.567429 11.00000 -1.20000 AFIX 0 C28 1 0.611805 0.866101 0.642418 11.00000 0.07700 0.04699 = 0.04391 0.01187 0.01245 0.01672 AFIX 43 H28 2 0.692203 0.905564 0.652872 11.00000 -1.20000 AFIX 0 C29 1 0.767450 0.762251 0.746010 11.00000 0.05161 0.04888 = 0.04563 0.00116 0.01065 0.01395 AFIX 23 H29A 2 0.798456 0.794467 0.691606 11.00000 -1.20000 H29B 2 0.803456 0.703619 0.760332 11.00000 -1.20000 AFIX 0 C30 1 0.802631 0.853968 0.822123 11.00000 0.06526 0.05210 = 0.04900 -0.00261 0.00401 0.01410 AFIX 137 H30A 2 0.771135 0.914420 0.806881 11.00000 -1.50000 H30B 2 0.887616 0.882619 0.831598 11.00000 -1.50000 H30C 2 0.771411 0.822924 0.876069 11.00000 -1.50000 AFIX 0 C31 1 0.523163 0.313503 0.609446 11.00000 0.04552 0.03567 = 0.02754 0.00692 0.00449 0.01479 AFIX 23 H31A 2 0.455907 0.246338 0.594468 11.00000 -1.20000 H31B 2 0.594688 0.295153 0.596880 11.00000 -1.20000 AFIX 0 C32 1 0.509815 0.408931 0.552123 11.00000 0.04061 0.03955 = 0.02304 0.00726 0.00406 0.01442 C33 1 0.399391 0.405979 0.508936 11.00000 0.04267 0.03843 = 0.02135 0.00456 0.00690 0.01322 C34 1 0.610480 0.501162 0.543254 11.00000 0.03917 0.04285 = 0.02145 0.00343 0.00608 0.01677 C35 1 0.725832 0.506181 0.584037 11.00000 0.04621 0.05007 = 0.03009 0.00663 0.00304 0.01820 AFIX 43 H35 2 0.733641 0.448508 0.619490 11.00000 -1.20000 AFIX 0 C36 1 0.823337 0.592916 0.572023 11.00000 0.03720 0.06463 = 0.03694 0.00488 0.00070 0.01576 AFIX 43 H36 2 0.897169 0.592702 0.597803 11.00000 -1.20000 AFIX 0 C37 1 0.814599 0.683587 0.520992 11.00000 0.04150 0.05269 = 0.03837 0.00310 0.00525 0.00116 AFIX 43 H37 2 0.882427 0.742421 0.512983 11.00000 -1.20000 AFIX 0 C38 1 0.707627 0.684985 0.483714 11.00000 0.05015 0.04173 = 0.02990 0.00479 0.00439 0.00851 AFIX 43 H38 2 0.702992 0.746856 0.452224 11.00000 -1.20000 AFIX 0 P1 5 0.775561 0.527390 0.995983 11.00000 0.04444 0.03741 = 0.04755 0.00450 0.00533 0.01212 F5 3 0.634248 0.478631 0.983115 11.00000 0.04805 0.08584 = 0.06959 0.01657 0.00311 0.01503 F6 3 0.915552 0.573491 1.008795 11.00000 0.04948 0.05482 = 0.08679 -0.00278 0.00545 0.00561 PART 1 F1 3 0.780646 0.592829 0.908823 21.00000 0.07729 0.08257 = 0.07693 0.02065 0.00708 0.02523 F2 3 0.784629 0.418037 0.943013 21.00000 0.06758 0.06742 = 0.05872 0.00162 0.00519 0.01315 F3 3 0.770758 0.464789 1.087870 21.00000 0.06758 0.06742 = 0.05872 0.00162 0.00519 0.01315 F4 3 0.764331 0.634423 1.053327 21.00000 0.08264 0.04144 = 0.13375 -0.01250 0.05015 0.01296 PART 0 PART 2 F1' 3 0.763019 0.514950 0.888174 -21.00000 0.07729 0.08257 = 0.07693 0.02065 0.00708 0.02523 F2' 3 0.788257 0.404248 0.987080 -21.00000 0.06758 0.06742 = 0.05872 0.00162 0.00519 0.01315 F3' 3 0.789065 0.563754 1.089174 -21.00000 0.06758 0.06742 = 0.05872 0.00162 0.00519 0.01315 F4' 3 0.760772 0.644416 0.967342 -21.00000 0.08264 0.04144 = 0.13375 -0.01250 0.05015 0.01296 PART 0 P2 5 0.895393 0.206442 0.657624 11.00000 0.06556 0.06787 = 0.04992 0.00940 0.01352 0.03109 F7 3 0.759869 0.191666 0.630230 11.00000 0.07390 0.15287 = 0.10417 -0.00581 0.00326 0.04904 F8 3 0.927860 0.323050 0.611038 11.00000 0.17078 0.09794 = 0.08709 0.03778 0.00872 0.02598 F9 3 1.029448 0.224806 0.683324 11.00000 0.07483 0.16364 = 0.11742 -0.00504 0.00294 0.04917 F10 3 0.861313 0.092968 0.705655 11.00000 0.18116 0.07143 = 0.10441 0.03382 -0.00627 0.00163 F11 3 0.890963 0.272157 0.750183 11.00000 0.09671 0.09085 = 0.07096 -0.00354 0.02127 0.02202 F12 3 0.900776 0.144896 0.565280 11.00000 0.13861 0.14385 = 0.07655 -0.02233 0.01777 0.06671 N7 4 0.723033 -0.068696 0.344818 11.00000 0.08082 0.06820 = 0.16436 0.02036 -0.03244 0.00310 C41 1 0.819060 -0.016256 0.354322 11.00000 0.06786 0.04558 = 0.07744 0.00891 -0.01211 0.01155 C42 1 0.939441 0.051798 0.366633 11.00000 0.07067 0.07497 = 0.10316 0.00762 0.01070 0.00746 AFIX 137 H42A 2 0.956214 0.101407 0.318500 11.00000 -1.50000 H42B 2 0.990077 0.004094 0.366823 11.00000 -1.50000 H42C 2 0.953525 0.095963 0.422912 11.00000 -1.50000 AFIX 0 N6 4 1.052481 0.745853 0.787433 11.00000 0.06854 0.08841 = 0.07467 -0.00269 -0.00148 0.02193 C39 1 1.025239 0.649099 0.791670 11.00000 0.05519 0.08131 = 0.04557 -0.00268 -0.00195 0.01854 C40 1 0.991772 0.528159 0.795882 11.00000 0.07862 0.08429 = 0.05873 0.01349 0.01519 0.02795 AFIX 137 H40A 2 0.916576 0.494347 0.761723 11.00000 -1.50000 H40B 2 0.985527 0.509489 0.857353 11.00000 -1.50000 H40C 2 1.050868 0.499899 0.771383 11.00000 -1.50000 AFIX 0 HKLF 4 REM a150923b_a.res in P-1 REM R1 = 0.0754 for 4683 Fo > 4sig(Fo) and 0.1117 for all 7439 data REM 579 parameters refined using 33 restraints END WGHT 0.1224 0.8832 REM Highest difference peak 0.907, deepest hole -0.636, 1-sigma level 0.075 Q1 1 0.7843 0.4242 1.0471 11.00000 0.05 0.91 Q2 1 0.7764 0.4552 0.9003 11.00000 0.05 0.77 Q3 1 0.7630 0.5377 0.8731 11.00000 0.05 0.71 Q4 1 0.8093 0.6417 0.9345 11.00000 0.05 0.63 Q5 1 0.7742 0.4973 1.1050 11.00000 0.05 0.55 Q6 1 0.8455 0.0579 0.5931 11.00000 0.05 0.50 Q7 1 0.8399 0.2800 0.6296 11.00000 0.05 0.46 Q8 1 0.9637 0.1425 0.7086 11.00000 0.05 0.45 Q9 1 0.7886 0.1415 0.6793 11.00000 0.05 0.41 Q10 1 0.8244 0.6199 1.0716 11.00000 0.05 0.38 Q11 1 0.9643 0.2364 0.7134 11.00000 0.05 0.38 Q12 1 0.7059 0.4896 0.9494 11.00000 0.05 0.36 Q13 1 0.4950 0.1369 0.7403 11.00000 0.05 0.35 Q14 1 1.0021 0.3063 0.6522 11.00000 0.05 0.35 Q15 1 0.9595 0.1787 0.6382 11.00000 0.05 0.35 Q16 1 0.9218 0.2464 0.5782 11.00000 0.05 0.34 Q17 1 0.4564 0.3865 0.5047 11.00000 0.05 0.34 Q18 1 0.8517 0.5085 0.9793 11.00000 0.05 0.34 Q19 1 0.9990 0.1403 0.6110 11.00000 0.05 0.34 Q20 1 0.8015 0.1399 0.5911 11.00000 0.05 0.32 REM The information below was added by Olex2. REM REM R1 = 0.0754 for 4683 Fo > 4sig(Fo) and 0.1117 for all 15004 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.91, deepest hole -0.64 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1117 REM R1_gt = 0.0754 REM wR_ref = 0.2238 REM GOOF = 1.048 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 15004 REM Reflections_gt = 4683 REM Parameters = n/a REM Hole = -0.64 REM Peak = 0.91 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received'