 
data_4ca
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C31 H33 Cl N2 O5'
_chemical_formula_sum
 'C31 H33 Cl N2 O5' 
_chemical_formula_weight          549.04

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 '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'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            4
_space_group_name_H-M_alt         'P 21'
_space_group_name_Hall            'P 2yb'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z'
 
_cell_length_a                    8.9878(10)
_cell_length_b                    14.6983(18)
_cell_length_c                    10.8669(13)
_cell_angle_alpha                 90
_cell_angle_beta                  90.983(3)
_cell_angle_gamma                 90
_cell_volume                      1435.4(3)
_cell_formula_units_Z             2
_cell_measurement_temperature     123(2)
_cell_measurement_reflns_used     5450
_cell_measurement_theta_min       3.2
_cell_measurement_theta_max       27.5
 
_exptl_crystal_description        'Prism'
_exptl_crystal_colour             'Colorless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.270          
_exptl_crystal_F_000              580
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.300
_exptl_crystal_size_mid           0.200
_exptl_crystal_size_min           0.100
_exptl_absorpt_coefficient_mu     0.175
_shelx_estimated_absorpt_T_min    0.949
_shelx_estimated_absorpt_T_max    0.983
_exptl_absorpt_correction_type    'Multi-scans'
_exptl_absorpt_correction_T_min   0.886
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       123(2)
_diffrn_radiation_wavelength      0.71075
_diffrn_radiation_type            MoK\a
_diffrn_source                    'Rotating Anode'
_diffrn_measurement_device_type   'Rigaku Pilatus 200K'
_diffrn_measurement_method        'profile data from ω-scans'
_diffrn_detector_area_resol_mean  5.8140
_diffrn_reflns_number             9914
_diffrn_reflns_av_unetI/netI      0.0143
_diffrn_reflns_av_R_equivalents   0.0128
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          3.230
_diffrn_reflns_theta_max          25.499
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.983
_diffrn_measured_fraction_theta_full  0.984
_diffrn_reflns_Laue_measured_fraction_max    0.983
_diffrn_reflns_Laue_measured_fraction_full   0.984
_diffrn_reflns_point_group_measured_fraction_max   0.911
_diffrn_reflns_point_group_measured_fraction_full  0.913
_reflns_number_total              4860
_reflns_number_gt                 4785
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.780
_reflns_Friedel_fraction_max      0.833
_reflns_Friedel_fraction_full     0.836
 
_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.
;
 
_computing_data_collection        'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_cell_refinement        'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_data_reduction         'CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)'
_computing_structure_solution     'SIR-97'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   'YADOKARI-XG'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0415P)²+0.1309P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.075(4)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Flack x determined using 2078 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.003(11)
_chemical_absolute_configuration  ad
_refine_ls_number_reflns          4860
_refine_ls_number_parameters      363
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0244
_refine_ls_R_factor_gt            0.0241
_refine_ls_wR_factor_ref          0.0628
_refine_ls_wR_factor_gt           0.0626
_refine_ls_goodness_of_fit_ref    1.080
_refine_ls_restrained_S_all       1.080
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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
O1 O 0.88138(12) 0.25957(9) 0.67684(11) 0.0232(3) Uani 1 1 d . . . . .
O3 O 0.81127(13) 0.13281(8) 0.50928(11) 0.0214(3) Uani 1 1 d . . . . .
N1 N 0.64245(14) 0.20782(10) 0.62171(12) 0.0185(3) Uani 1 1 d . . . . .
N2 N 0.66325(17) 0.27792(10) 1.03250(13) 0.0199(3) Uani 1 1 d . . . . .
H2 H 0.573(3) 0.2721(16) 1.046(2) 0.030(6) Uiso 1 1 d . . . . .
C1 C 0.75011(17) 0.25398(11) 0.69489(14) 0.0179(3) Uani 1 1 d . . . . .
C2 C 0.67024(17) 0.29648(11) 0.80587(14) 0.0179(3) Uani 1 1 d . . . . .
C3 C 0.50914(17) 0.27617(11) 0.77575(15) 0.0177(3) Uani 1 1 d . . . . .
C4 C 0.38189(18) 0.30389(12) 0.83588(16) 0.0218(3) Uani 1 1 d . . . . .
H4 H 0.3893 0.3388 0.9093 0.026 Uiso 1 1 calc R U . . .
C5 C 0.24323(19) 0.27974(12) 0.78709(17) 0.0244(4) Uani 1 1 d . . . . .
H5 H 0.1554 0.2969 0.8285 0.029 Uiso 1 1 calc R U . . .
C6 C 0.23278(18) 0.23069(12) 0.67830(18) 0.0244(4) Uani 1 1 d . . . . .
H6 H 0.1373 0.2157 0.6453 0.029 Uiso 1 1 calc R U . . .
C7 C 0.35914(18) 0.20293(13) 0.61650(16) 0.0225(3) Uani 1 1 d . . . . .
H7 H 0.3516 0.1696 0.5417 0.027 Uiso 1 1 calc R U . . .
C8 C 0.49662(18) 0.22559(11) 0.66785(15) 0.0179(3) Uani 1 1 d . . . . .
C9 C 0.66792(18) 0.14415(12) 0.52700(15) 0.0206(3) Uani 1 1 d . . . . .
C10 C 0.8632(2) 0.06416(13) 0.41797(16) 0.0243(4) Uani 1 1 d . . . . .
C11 C 1.0306(2) 0.07502(14) 0.42946(17) 0.0294(4) Uani 1 1 d . . . . .
H11 H 1.0584 0.1369 0.4054 0.044 Uiso 1 1 calc R U . . .
H11A H 1.0792 0.0311 0.3755 0.044 Uiso 1 1 calc R U . . .
H11B H 1.0624 0.0641 0.5149 0.044 Uiso 1 1 calc R U . . .
C12 C 0.8136(3) -0.02984(14) 0.4577(2) 0.0359(5) Uani 1 1 d . . . . .
H12 H 0.8407 -0.0393 0.5445 0.054 Uiso 1 1 calc R U . . .
H12A H 0.8627 -0.0759 0.4073 0.054 Uiso 1 1 calc R U . . .
H12B H 0.7055 -0.0351 0.4468 0.054 Uiso 1 1 calc R U . . .
C13 C 0.8089(2) 0.08910(16) 0.28864(17) 0.0339(5) Uani 1 1 d . . . . .
H13 H 0.7002 0.0842 0.2839 0.051 Uiso 1 1 calc R U . . .
H13A H 0.8530 0.0475 0.2290 0.051 Uiso 1 1 calc R U . . .
H13B H 0.8387 0.1517 0.2699 0.051 Uiso 1 1 calc R U . . .
C14 C 0.70426(18) 0.39861(12) 0.81545(15) 0.0185(3) Uani 1 1 d . . . . .
C15 C 0.8280(2) 0.43142(13) 0.88154(16) 0.0222(4) Uani 1 1 d . . . . .
H15 H 0.8963 0.3895 0.9177 0.027 Uiso 1 1 calc R U . . .
C16 C 0.8525(2) 0.52396(13) 0.89507(16) 0.0258(4) Uani 1 1 d . . . . .
H16 H 0.9355 0.5453 0.9420 0.031 Uiso 1 1 calc R U . . .
C17 C 0.7558(2) 0.58471(13) 0.83997(16) 0.0257(4) Uani 1 1 d . . . . .
C18 C 0.6366(2) 0.55515(13) 0.76865(17) 0.0260(4) Uani 1 1 d . . . . .
H18 H 0.5730 0.5975 0.7279 0.031 Uiso 1 1 calc R U . . .
C19 C 0.61155(19) 0.46217(12) 0.75773(16) 0.0220(4) Uani 1 1 d . . . . .
H19 H 0.5291 0.4414 0.7096 0.026 Uiso 1 1 calc R U . . .
C20 C 0.73006(17) 0.24225(11) 0.92238(14) 0.0176(3) Uani 1 1 d . . . . .
H20 H 0.8393 0.2547 0.9296 0.021 Uiso 1 1 calc R U . . .
C21 C 0.71215(18) 0.13950(12) 0.90977(14) 0.0197(3) Uani 1 1 d . . . . .
C22 C 0.8294(2) 0.08807(13) 0.86448(16) 0.0273(4) Uani 1 1 d . . . . .
H22 H 0.9191 0.1173 0.8416 0.033 Uiso 1 1 calc R U . . .
C23 C 0.8157(3) -0.00603(14) 0.85256(19) 0.0354(5) Uani 1 1 d . . . . .
H23 H 0.8958 -0.0407 0.8211 0.043 Uiso 1 1 calc R U . . .
C24 C 0.6859(3) -0.04884(13) 0.88639(19) 0.0347(5) Uani 1 1 d . . . . .
H24 H 0.6760 -0.1128 0.8770 0.042 Uiso 1 1 calc R U . . .
C25 C 0.5706(2) 0.00152(14) 0.93396(18) 0.0314(4) Uani 1 1 d . . . . .
H25 H 0.4823 -0.0281 0.9593 0.038 Uiso 1 1 calc R U . . .
C26 C 0.5831(2) 0.09520(13) 0.94490(16) 0.0252(4) Uani 1 1 d . . . . .
H26 H 0.5028 0.1294 0.9767 0.030 Uiso 1 1 calc R U . . .
C27 C 0.74661(19) 0.31366(12) 1.12652(15) 0.0206(3) Uani 1 1 d . . . . .
C28 C 0.7124(3) 0.39695(14) 1.31853(17) 0.0337(5) Uani 1 1 d . . . . .
C29 C 0.5772(3) 0.4063(2) 1.3986(2) 0.0553(7) Uani 1 1 d . . . . .
H29 H 0.4949 0.4327 1.3502 0.083 Uiso 1 1 calc R U . . .
H29A H 0.6010 0.4461 1.4686 0.083 Uiso 1 1 calc R U . . .
H29B H 0.5480 0.3462 1.4289 0.083 Uiso 1 1 calc R U . . .
C30 C 0.7567(3) 0.48790(14) 1.2629(2) 0.0461(6) Uani 1 1 d . . . . .
H30 H 0.8368 0.4784 1.2042 0.069 Uiso 1 1 calc R U . . .
H30A H 0.7913 0.5289 1.3285 0.069 Uiso 1 1 calc R U . . .
H30B H 0.6705 0.5149 1.2202 0.069 Uiso 1 1 calc R U . . .
C31 C 0.8406(3) 0.35246(15) 1.38910(17) 0.0359(5) Uani 1 1 d . . . . .
H31 H 0.8139 0.2897 1.4098 0.054 Uiso 1 1 calc R U . . .
H31A H 0.8612 0.3867 1.4649 0.054 Uiso 1 1 calc R U . . .
H31B H 0.9295 0.3523 1.3381 0.054 Uiso 1 1 calc R U . . .
Cl1 Cl 0.78660(6) 0.70123(3) 0.85798(5) 0.04328(16) Uani 1 1 d . . . . .
O2 O 0.56658(14) 0.10727(10) 0.47316(12) 0.0323(3) Uani 1 1 d . . . . .
O4 O 0.87999(14) 0.32356(9) 1.12503(11) 0.0276(3) Uani 1 1 d . . . . .
O5 O 0.65611(14) 0.33654(9) 1.21875(11) 0.0269(3) Uani 1 1 d . . . . .
 
 
_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
O1 C1 1.202(2) . ?
O3 C9 1.317(2) . ?
O3 C10 1.495(2) . ?
N1 C9 1.413(2) . ?
N1 C1 1.415(2) . ?
N1 C8 1.435(2) . ?
N2 C27 1.362(2) . ?
N2 C20 1.446(2) . ?
N2 H2 0.83(2) . ?
C1 C2 1.546(2) . ?
C2 C3 1.509(2) . ?
C2 C14 1.535(2) . ?
C2 C20 1.582(2) . ?
C3 C4 1.388(2) . ?
C3 C8 1.391(2) . ?
C4 C5 1.392(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.390(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.388(2) . ?
C7 H7 0.9500 . ?
C9 O2 1.203(2) . ?
C10 C11 1.516(3) . ?
C10 C12 1.516(3) . ?
C10 C13 1.524(3) . ?
C11 H11 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 H13 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 C19 1.394(2) . ?
C14 C15 1.399(2) . ?
C15 C16 1.385(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.382(3) . ?
C17 Cl1 1.7453(19) . ?
C18 C19 1.390(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.525(2) . ?
C20 H20 1.0000 . ?
C21 C26 1.389(3) . ?
C21 C22 1.394(3) . ?
C22 C23 1.394(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.382(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 O4 1.208(2) . ?
C27 O5 1.344(2) . ?
C28 O5 1.484(2) . ?
C28 C29 1.513(3) . ?
C28 C31 1.521(3) . ?
C28 C30 1.523(3) . ?
C29 H29 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C30 H30 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C31 H31 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
 
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
C9 O3 C10 119.97(13) . . ?
C9 N1 C1 127.53(13) . . ?
C9 N1 C8 122.38(13) . . ?
C1 N1 C8 109.64(13) . . ?
C27 N2 C20 121.98(14) . . ?
C27 N2 H2 115.8(16) . . ?
C20 N2 H2 121.8(16) . . ?
O1 C1 N1 127.20(15) . . ?
O1 C1 C2 124.74(14) . . ?
N1 C1 C2 108.06(13) . . ?
C3 C2 C14 113.42(13) . . ?
C3 C2 C1 101.98(13) . . ?
C14 C2 C1 110.70(13) . . ?
C3 C2 C20 112.67(13) . . ?
C14 C2 C20 111.95(13) . . ?
C1 C2 C20 105.35(12) . . ?
C4 C3 C8 119.88(15) . . ?
C4 C3 C2 129.44(15) . . ?
C8 C3 C2 110.61(14) . . ?
C3 C4 C5 119.04(16) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 120.30(16) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 121.36(16) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C6 117.67(16) . . ?
C8 C7 H7 121.2 . . ?
C6 C7 H7 121.2 . . ?
C7 C8 C3 121.72(15) . . ?
C7 C8 N1 128.90(15) . . ?
C3 C8 N1 109.30(14) . . ?
O2 C9 O3 127.34(16) . . ?
O2 C9 N1 121.46(15) . . ?
O3 C9 N1 111.20(13) . . ?
O3 C10 C11 101.23(13) . . ?
O3 C10 C12 109.25(15) . . ?
C11 C10 C12 111.62(16) . . ?
O3 C10 C13 110.55(15) . . ?
C11 C10 C13 110.60(16) . . ?
C12 C10 C13 112.99(17) . . ?
C10 C11 H11 109.5 . . ?
C10 C11 H11A 109.5 . . ?
H11 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C12 H12 109.5 . . ?
C10 C12 H12A 109.5 . . ?
H12 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C13 H13 109.5 . . ?
C10 C13 H13A 109.5 . . ?
H13 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C19 C14 C15 117.63(16) . . ?
C19 C14 C2 120.54(14) . . ?
C15 C14 C2 121.84(15) . . ?
C16 C15 C14 121.10(17) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C17 C16 C15 119.53(16) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 121.19(17) . . ?
C16 C17 Cl1 119.37(14) . . ?
C18 C17 Cl1 119.43(15) . . ?
C17 C18 C19 118.68(17) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C18 C19 C14 121.74(16) . . ?
C18 C19 H19 119.1 . . ?
C14 C19 H19 119.1 . . ?
N2 C20 C21 112.87(13) . . ?
N2 C20 C2 109.83(13) . . ?
C21 C20 C2 113.15(13) . . ?
N2 C20 H20 106.9 . . ?
C21 C20 H20 106.9 . . ?
C2 C20 H20 106.9 . . ?
C26 C21 C22 118.86(17) . . ?
C26 C21 C20 121.80(15) . . ?
C22 C21 C20 119.31(16) . . ?
C21 C22 C23 120.31(19) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C24 C23 C22 120.05(19) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 119.90(18) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 120.23(19) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C21 120.61(18) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
O4 C27 O5 126.38(15) . . ?
O4 C27 N2 124.73(16) . . ?
O5 C27 N2 108.88(14) . . ?
O5 C28 C29 101.97(18) . . ?
O5 C28 C31 110.93(16) . . ?
C29 C28 C31 111.00(18) . . ?
O5 C28 C30 108.87(15) . . ?
C29 C28 C30 111.5(2) . . ?
C31 C28 C30 112.1(2) . . ?
C28 C29 H29 109.5 . . ?
C28 C29 H29A 109.5 . . ?
H29 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C30 H30 109.5 . . ?
C28 C30 H30A 109.5 . . ?
H30 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C31 H31 109.5 . . ?
C28 C31 H31A 109.5 . . ?
H31 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C27 O5 C28 119.43(15) . . ?
 
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
C9 N1 C1 O1 13.7(3) . . . . ?
C8 N1 C1 O1 -173.95(16) . . . . ?
C9 N1 C1 C2 -165.67(15) . . . . ?
C8 N1 C1 C2 6.70(17) . . . . ?
O1 C1 C2 C3 174.94(16) . . . . ?
N1 C1 C2 C3 -5.68(16) . . . . ?
O1 C1 C2 C14 54.0(2) . . . . ?
N1 C1 C2 C14 -126.65(14) . . . . ?
O1 C1 C2 C20 -67.2(2) . . . . ?
N1 C1 C2 C20 112.15(14) . . . . ?
C14 C2 C3 C4 -55.0(2) . . . . ?
C1 C2 C3 C4 -174.04(17) . . . . ?
C20 C2 C3 C4 73.5(2) . . . . ?
C14 C2 C3 C8 121.82(15) . . . . ?
C1 C2 C3 C8 2.77(17) . . . . ?
C20 C2 C3 C8 -109.69(15) . . . . ?
C8 C3 C4 C5 0.5(2) . . . . ?
C2 C3 C4 C5 177.03(16) . . . . ?
C3 C4 C5 C6 -1.6(3) . . . . ?
C4 C5 C6 C7 1.2(3) . . . . ?
C5 C6 C7 C8 0.4(3) . . . . ?
C6 C7 C8 C3 -1.5(3) . . . . ?
C6 C7 C8 N1 -178.04(16) . . . . ?
C4 C3 C8 C7 1.1(2) . . . . ?
C2 C3 C8 C7 -176.03(15) . . . . ?
C4 C3 C8 N1 178.25(15) . . . . ?
C2 C3 C8 N1 1.10(18) . . . . ?
C9 N1 C8 C7 -15.3(3) . . . . ?
C1 N1 C8 C7 171.87(17) . . . . ?
C9 N1 C8 C3 167.85(14) . . . . ?
C1 N1 C8 C3 -4.99(18) . . . . ?
C10 O3 C9 O2 -3.4(3) . . . . ?
C10 O3 C9 N1 176.45(13) . . . . ?
C1 N1 C9 O2 177.90(17) . . . . ?
C8 N1 C9 O2 6.4(3) . . . . ?
C1 N1 C9 O3 -2.0(2) . . . . ?
C8 N1 C9 O3 -173.47(14) . . . . ?
C9 O3 C10 C11 -179.86(15) . . . . ?
C9 O3 C10 C12 -62.0(2) . . . . ?
C9 O3 C10 C13 62.9(2) . . . . ?
C3 C2 C14 C19 -22.3(2) . . . . ?
C1 C2 C14 C19 91.58(17) . . . . ?
C20 C2 C14 C19 -151.20(15) . . . . ?
C3 C2 C14 C15 157.69(15) . . . . ?
C1 C2 C14 C15 -88.39(18) . . . . ?
C20 C2 C14 C15 28.8(2) . . . . ?
C19 C14 C15 C16 3.7(3) . . . . ?
C2 C14 C15 C16 -176.34(16) . . . . ?
C14 C15 C16 C17 -1.7(3) . . . . ?
C15 C16 C17 C18 -1.7(3) . . . . ?
C15 C16 C17 Cl1 179.65(14) . . . . ?
C16 C17 C18 C19 2.9(3) . . . . ?
Cl1 C17 C18 C19 -178.45(14) . . . . ?
C17 C18 C19 C14 -0.7(3) . . . . ?
C15 C14 C19 C18 -2.5(2) . . . . ?
C2 C14 C19 C18 177.57(16) . . . . ?
C27 N2 C20 C21 112.54(17) . . . . ?
C27 N2 C20 C2 -120.19(16) . . . . ?
C3 C2 C20 N2 -70.48(16) . . . . ?
C14 C2 C20 N2 58.78(17) . . . . ?
C1 C2 C20 N2 179.16(13) . . . . ?
C3 C2 C20 C21 56.65(18) . . . . ?
C14 C2 C20 C21 -174.10(13) . . . . ?
C1 C2 C20 C21 -53.72(17) . . . . ?
N2 C20 C21 C26 37.3(2) . . . . ?
C2 C20 C21 C26 -88.17(18) . . . . ?
N2 C20 C21 C22 -141.15(15) . . . . ?
C2 C20 C21 C22 93.35(17) . . . . ?
C26 C21 C22 C23 1.3(3) . . . . ?
C20 C21 C22 C23 179.78(16) . . . . ?
C21 C22 C23 C24 -0.4(3) . . . . ?
C22 C23 C24 C25 -1.1(3) . . . . ?
C23 C24 C25 C26 1.7(3) . . . . ?
C24 C25 C26 C21 -0.8(3) . . . . ?
C22 C21 C26 C25 -0.6(2) . . . . ?
C20 C21 C26 C25 -179.13(16) . . . . ?
C20 N2 C27 O4 4.1(3) . . . . ?
C20 N2 C27 O5 -176.59(14) . . . . ?
O4 C27 O5 C28 14.2(3) . . . . ?
N2 C27 O5 C28 -165.11(14) . . . . ?
C29 C28 O5 C27 178.81(17) . . . . ?
C31 C28 O5 C27 -62.9(2) . . . . ?
C30 C28 O5 C27 60.9(2) . . . . ?
 
_refine_diff_density_max    0.237
_refine_diff_density_min   -0.295
_refine_diff_density_rms    0.091



