 
data_kek_70b
 
_audit_creation_method            'SHELXL-2017/1'
_shelx_SHELXL_version_number      '2017/1'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C24 H32 N7 O3 P'
_chemical_formula_sum
 'C24 H32 N7 O3 P' 
_chemical_formula_weight          497.54

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'
 'N'  'N'   0.0311   0.0180
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0492   0.0322
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/n'
_space_group_name_Hall            '-P 2yn'
 
_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+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    15.7906(2)
_cell_length_b                    15.1059(2)
_cell_length_c                    21.9456(3)
_cell_angle_alpha                 90
_cell_angle_beta                  106.4610(10)
_cell_angle_gamma                 90
_cell_volume                      5020.15(12)
_cell_formula_units_Z             8
_cell_measurement_temperature     160.0(1)
_cell_measurement_reflns_used     33557  
_cell_measurement_theta_min       3.5970 
_cell_measurement_theta_max       76.8560
 
_exptl_crystal_description        'block'     
_exptl_crystal_colour             'colourless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.317          
_exptl_crystal_F_000              2112
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.05
_exptl_crystal_size_min           0.04
_exptl_absorpt_coefficient_mu     1.304
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.86688
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_process_details    
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       160.0(1)
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\a
_diffrn_source                    'micro-focus sealed X-ray tube'  
_diffrn_measurement_device_type   'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method        'ω scans'                       
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             50182
_diffrn_reflns_av_unetI/netI      0.0200
_diffrn_reflns_av_R_equivalents   0.0311
_diffrn_reflns_limit_h_min        -19
_diffrn_reflns_limit_h_max        19
_diffrn_reflns_limit_k_min        -19
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        27
_diffrn_reflns_theta_min          3.602
_diffrn_reflns_theta_max          77.157
_diffrn_reflns_theta_full         67.684
_diffrn_measured_fraction_theta_max   0.949
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.949
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.949
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              10318
_reflns_number_gt                 9670
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_cell_refinement        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction         'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_structure_solution     'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1377P)²+13.5366P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          10318
_refine_ls_number_parameters      638
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0830
_refine_ls_R_factor_gt            0.0801
_refine_ls_wR_factor_ref          0.2723
_refine_ls_wR_factor_gt           0.2696
_refine_ls_goodness_of_fit_ref    1.177
_refine_ls_restrained_S_all       1.177
_refine_ls_shift/su_max           0.005
_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
P21 P 0.84958(6) 0.61700(6) 0.57290(4) 0.0220(2) Uani 1 1 d . . . . .
P56 P 0.70866(6) 0.11631(6) 0.57745(5) 0.0232(2) Uani 1 1 d . . . . .
O25 O 0.91134(18) 0.69895(18) 0.58938(13) 0.0266(6) Uani 1 1 d . . . . .
O22 O 0.83109(19) 0.59166(19) 0.63731(13) 0.0297(6) Uani 1 1 d . . . . .
O63 O 0.64734(18) 0.04679(18) 0.54593(14) 0.0296(6) Uani 1 1 d . . . . .
O60 O 0.7772(2) 0.0904(2) 0.64201(14) 0.0316(6) Uani 1 1 d . . . . .
O57 O 0.65997(19) 0.19772(19) 0.59483(14) 0.0309(6) Uani 1 1 d . . . . .
O28 O 0.88569(18) 0.54640(18) 0.54217(14) 0.0285(6) Uani 1 1 d . . . . .
N7 N 0.6314(2) 0.8489(2) 0.45592(15) 0.0211(6) Uani 1 1 d . . . . .
N42 N 0.8389(2) 0.3444(2) 0.45981(15) 0.0228(6) Uani 1 1 d . . . . .
N2 N 0.6850(2) 0.5924(2) 0.49739(14) 0.0210(6) Uani 1 1 d . . . . .
N37 N 0.8146(2) 0.0895(2) 0.50307(15) 0.0215(6) Uani 1 1 d . . . . .
N9 N 0.5777(2) 0.6978(2) 0.43946(14) 0.0209(6) Uani 1 1 d . . . . .
N45 N 0.9012(2) 0.0420(2) 0.43943(15) 0.0219(6) Uani 1 1 d . . . . .
N44 N 0.8788(2) 0.1935(2) 0.44543(15) 0.0222(6) Uani 1 1 d . . . . .
N10 N 0.5477(2) 0.5467(2) 0.43561(15) 0.0212(6) Uani 1 1 d . . . . .
N13 N 0.4288(2) 0.4852(2) 0.38038(18) 0.0312(8) Uani 1 1 d . . . . .
N40 N 0.7490(2) 0.3221(2) 0.52252(16) 0.0244(7) Uani 1 1 d . . . . .
N5 N 0.7679(2) 0.8233(2) 0.52129(16) 0.0247(7) Uani 1 1 d . . . . .
N14 N 0.4676(2) 0.5616(2) 0.39325(18) 0.0309(8) Uani 1 1 d . . . . .
N49 N 0.9411(3) 0.0567(2) 0.39309(18) 0.0333(8) Uani 1 1 d . . . . .
N48 N 0.9663(3) -0.0203(2) 0.37801(19) 0.0353(8) Uani 1 1 d . . . . .
C38 C 0.7736(2) 0.1545(2) 0.52656(17) 0.0204(7) Uani 1 1 d . . . . .
C4 C 0.7236(2) 0.7435(2) 0.50529(17) 0.0211(7) Uani 1 1 d . . . . .
C12 C 0.4825(2) 0.4200(2) 0.41393(18) 0.0221(7) Uani 1 1 d . . . . .
C8 C 0.6380(2) 0.7593(2) 0.46412(17) 0.0202(7) Uani 1 1 d . . . . .
C39 C 0.7819(2) 0.2413(2) 0.50893(17) 0.0208(7) Uani 1 1 d . . . . .
C36 C 0.8624(2) 0.1135(2) 0.46455(17) 0.0203(7) Uani 1 1 d . . . . .
C11 C 0.5582(2) 0.4590(2) 0.44954(18) 0.0219(7) Uani 1 1 d . . . . .
H11 H 0.606551 0.431576 0.477389 0.026 Uiso 1 1 calc R U . . .
C47 C 0.9436(2) -0.0850(3) 0.41442(18) 0.0235(7) Uani 1 1 d . . . . .
C3 C 0.7446(2) 0.6566(2) 0.52152(17) 0.0208(7) Uani 1 1 d . . . . .
C43 C 0.8373(2) 0.2554(2) 0.46908(17) 0.0214(7) Uani 1 1 d . . . . .
C46 C 0.9021(2) -0.0452(2) 0.45384(18) 0.0222(7) Uani 1 1 d . . . . .
H46 H 0.879387 -0.072111 0.483985 0.027 Uiso 1 1 calc R U . . .
C1 C 0.6075(2) 0.6175(2) 0.45904(17) 0.0206(7) Uani 1 1 d . . . . .
C50 C 0.9640(2) -0.1787(2) 0.40708(18) 0.0231(7) Uani 1 1 d . . . . .
C15 C 0.4564(2) 0.3261(2) 0.40801(18) 0.0229(7) Uani 1 1 d . . . . .
C6 C 0.7104(3) 0.8826(2) 0.49141(19) 0.0246(8) Uani 1 1 d . . . . .
H6 H 0.722448 0.942930 0.494150 0.030 Uiso 1 1 calc R U . . .
C29 C 0.5559(3) 0.9011(3) 0.41800(19) 0.0264(8) Uani 1 1 d . . . . .
H29A H 0.560497 0.961094 0.434459 0.032 Uiso 1 1 calc R U . . .
H29B H 0.501659 0.875735 0.422717 0.032 Uiso 1 1 calc R U . . .
C20 C 0.5098(3) 0.2618(3) 0.44520(19) 0.0276(8) Uani 1 1 d . . . . .
H20 H 0.562288 0.278017 0.474829 0.033 Uiso 1 1 calc R U . . .
C41 C 0.7852(3) 0.3802(3) 0.49283(19) 0.0255(8) Uani 1 1 d . . . . .
H41 H 0.775100 0.440727 0.494120 0.031 Uiso 1 1 calc R U . . .
C64 C 0.8917(3) 0.3916(3) 0.4247(2) 0.0291(8) Uani 1 1 d . . . . .
H64A H 0.941118 0.354700 0.422694 0.035 Uiso 1 1 calc R U . . .
H64B H 0.915292 0.445327 0.447392 0.035 Uiso 1 1 calc R U . . .
C51 C 1.0141(3) -0.2034(3) 0.3669(2) 0.0303(8) Uani 1 1 d . . . . .
H51 H 1.034522 -0.160336 0.344247 0.036 Uiso 1 1 calc R U . . .
C30 C 0.5508(3) 0.9042(3) 0.3481(2) 0.0351(9) Uani 1 1 d . . . . .
H30A H 0.503088 0.943614 0.326872 0.042 Uiso 1 1 calc R U . . .
H30B H 0.535932 0.845536 0.330358 0.042 Uiso 1 1 calc R U . . .
C26 C 0.9165(3) 0.7636(3) 0.6396(2) 0.0329(9) Uani 1 1 d . . . . .
H26A H 0.863091 0.761165 0.653065 0.039 Uiso 1 1 calc R U . . .
H26B H 0.921749 0.822676 0.623806 0.039 Uiso 1 1 calc R U . . .
C19 C 0.4848(3) 0.1735(3) 0.4382(2) 0.0326(9) Uani 1 1 d . . . . .
H19 H 0.520946 0.130824 0.463253 0.039 Uiso 1 1 calc R U . . .
C54 C 0.9546(3) -0.3327(3) 0.4338(2) 0.0340(9) Uani 1 1 d . . . . .
H54 H 0.934775 -0.376209 0.456425 0.041 Uiso 1 1 calc R U . . .
C18 C 0.4070(3) 0.1480(3) 0.3945(2) 0.0353(9) Uani 1 1 d . . . . .
H18 H 0.391088 0.088589 0.389744 0.042 Uiso 1 1 calc R U . . .
C53 C 1.0037(3) -0.3563(3) 0.3934(2) 0.0349(9) Uani 1 1 d . . . . .
H53 H 1.016483 -0.415506 0.388568 0.042 Uiso 1 1 calc R U . . .
C16 C 0.3770(3) 0.3003(3) 0.3638(2) 0.0312(9) Uani 1 1 d . . . . .
H16 H 0.340568 0.342521 0.338494 0.037 Uiso 1 1 calc R U . . .
C55 C 0.9344(3) -0.2444(3) 0.4409(2) 0.0302(8) Uani 1 1 d . . . . .
H55 H 0.901196 -0.229017 0.468126 0.036 Uiso 1 1 calc R U . . .
C23 C 0.8000(3) 0.5039(3) 0.6484(2) 0.0316(9) Uani 1 1 d . . . . .
H23A H 0.816011 0.460886 0.620788 0.038 Uiso 1 1 calc R U . . .
H23B H 0.736214 0.504034 0.639594 0.038 Uiso 1 1 calc R U . . .
C52 C 1.0338(3) -0.2916(3) 0.3602(2) 0.0355(9) Uani 1 1 d . . . . .
H52 H 1.067400 -0.307344 0.333321 0.043 Uiso 1 1 calc R U . . .
C65 C 0.8379(3) 0.4153(3) 0.3577(2) 0.0347(9) Uani 1 1 d . . . . .
H65A H 0.810570 0.362036 0.336202 0.042 Uiso 1 1 calc R U . . .
H65B H 0.877328 0.438143 0.334587 0.042 Uiso 1 1 calc R U . . .
C17 C 0.3531(3) 0.2118(3) 0.3579(2) 0.0370(10) Uani 1 1 d . . . . .
H17 H 0.300225 0.195052 0.328898 0.044 Uiso 1 1 calc R U . . .
C61 C 0.8267(3) 0.0072(3) 0.6487(2) 0.0363(10) Uani 1 1 d . . . . .
H61A H 0.865474 0.007649 0.621377 0.044 Uiso 1 1 calc R U . . .
H61B H 0.786436 -0.042397 0.636652 0.044 Uiso 1 1 calc R U . . .
C58 C 0.6956(3) 0.2645(3) 0.6432(2) 0.0372(10) Uani 1 1 d . . . . .
H58A H 0.687973 0.322897 0.623941 0.045 Uiso 1 1 calc R U . . .
H58B H 0.758330 0.254528 0.661890 0.045 Uiso 1 1 calc R U . . .
C66 C 0.7665(3) 0.4836(3) 0.3557(2) 0.0369(10) Uani 1 1 d . . . . .
H66A H 0.724163 0.458692 0.375481 0.044 Uiso 1 1 calc R U . . .
H66B H 0.793193 0.534791 0.380483 0.044 Uiso 1 1 calc R U . . .
C34 C 0.6437(3) 1.1941(4) 0.3423(2) 0.0428(11) Uani 1 1 d . . . . .
H34A H 0.646239 1.199289 0.386880 0.051 Uiso 1 1 calc R U . . .
H34B H 0.703669 1.198223 0.339269 0.051 Uiso 1 1 calc R U . . .
C59 C 0.6493(4) 0.2599(4) 0.6931(2) 0.0455(12) Uani 1 1 d . . . . .
H59A H 0.586916 0.266345 0.674024 0.068 Uiso 1 1 calc R U . . .
H59B H 0.670015 0.306571 0.723341 0.068 Uiso 1 1 calc R U . . .
H59C H 0.660956 0.203719 0.714306 0.068 Uiso 1 1 calc R U . . .
C33 C 0.6067(3) 1.1029(3) 0.3185(2) 0.0378(10) Uani 1 1 d . . . . .
H33A H 0.548138 1.096698 0.323952 0.045 Uiso 1 1 calc R U . . .
H33B H 0.601442 1.098066 0.273515 0.045 Uiso 1 1 calc R U . . .
C32 C 0.6653(3) 1.0292(4) 0.3539(2) 0.0418(11) Uani 1 1 d . . . . .
H32A H 0.670056 1.035143 0.398793 0.050 Uiso 1 1 calc R U . . .
H32B H 0.723942 1.037350 0.349031 0.050 Uiso 1 1 calc R U . . .
C69 C 0.6851(3) 0.6724(4) 0.3198(2) 0.0431(11) Uani 1 1 d . . . . .
H69A H 0.636247 0.711909 0.318536 0.052 Uiso 1 1 calc R U . . .
H69B H 0.715358 0.660718 0.364078 0.052 Uiso 1 1 calc R U . . .
C27 C 0.9941(4) 0.7439(4) 0.6941(2) 0.0494(13) Uani 1 1 d . . . . .
H27A H 1.046279 0.742561 0.679972 0.074 Uiso 1 1 calc R U . . .
H27B H 0.986196 0.687493 0.711849 0.074 Uiso 1 1 calc R U . . .
H27C H 1.000026 0.789048 0.725862 0.074 Uiso 1 1 calc R U . . .
C67 C 0.7177(4) 0.5138(4) 0.2890(2) 0.0444(11) Uani 1 1 d . . . . .
H67A H 0.689342 0.463004 0.264590 0.053 Uiso 1 1 calc R U . . .
H67B H 0.760158 0.537138 0.268731 0.053 Uiso 1 1 calc R U . . .
C31 C 0.6349(4) 0.9347(4) 0.3333(2) 0.0436(11) Uani 1 1 d . . . . .
H31A H 0.625837 0.930071 0.287796 0.052 Uiso 1 1 calc R U . . .
H31B H 0.682200 0.894310 0.353674 0.052 Uiso 1 1 calc R U . . .
C70 C 0.7484(4) 0.7190(4) 0.2901(3) 0.0556(14) Uani 1 1 d . . . . .
H70A H 0.722728 0.722406 0.244926 0.083 Uiso 1 1 calc R U . . .
H70B H 0.802759 0.686444 0.299196 0.083 Uiso 1 1 calc R U . . .
H70C H 0.759785 0.777627 0.307292 0.083 Uiso 1 1 calc R U . . .
C68 C 0.6478(4) 0.5846(4) 0.2876(2) 0.0473(12) Uani 1 1 d . . . . .
H68A H 0.605954 0.561329 0.308395 0.057 Uiso 1 1 calc R U . . .
H68B H 0.615817 0.596583 0.243670 0.057 Uiso 1 1 calc R U . . .
C35 C 0.5910(4) 1.2704(4) 0.3067(3) 0.0521(13) Uani 1 1 d . . . . .
H35A H 0.595772 1.271267 0.264021 0.078 Uiso 1 1 calc R U . . .
H35B H 0.613555 1.324895 0.327560 0.078 Uiso 1 1 calc R U . . .
H35C H 0.530212 1.263744 0.305694 0.078 Uiso 1 1 calc R U . . .
C24 C 0.8421(5) 0.4806(4) 0.7162(3) 0.0570(15) Uani 1 1 d . . . . .
H24A H 0.904961 0.477126 0.723830 0.086 Uiso 1 1 calc R U . . .
H24B H 0.820105 0.424416 0.725448 0.086 Uiso 1 1 calc R U . . .
H24C H 0.828424 0.525222 0.743119 0.086 Uiso 1 1 calc R U . . .
C62 C 0.8795(4) -0.0009(4) 0.7166(3) 0.0539(14) Uani 1 1 d . . . . .
H62A H 0.912133 -0.055394 0.722579 0.081 Uiso 1 1 calc R U . . .
H62B H 0.840566 -0.000523 0.743166 0.081 Uiso 1 1 calc R U . . .
H62C H 0.919821 0.047967 0.727735 0.081 Uiso 1 1 calc R U . . .
 
 
_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
P21 O28 1.461(3) . ?
P21 O25 1.554(3) . ?
P21 O22 1.570(3) . ?
P21 C3 1.821(4) . ?
P56 O63 1.463(3) . ?
P56 O57 1.554(3) . ?
P56 O60 1.569(3) . ?
P56 C38 1.811(4) . ?
O25 C26 1.457(5) . ?
O22 C23 1.458(5) . ?
O60 C61 1.465(5) . ?
O57 C58 1.457(5) . ?
N7 C8 1.366(5) . ?
N7 C6 1.367(5) . ?
N7 C29 1.475(5) . ?
N42 C43 1.362(5) . ?
N42 C41 1.373(5) . ?
N42 C64 1.470(5) . ?
N2 C1 1.328(5) . ?
N2 C3 1.350(5) . ?
N37 C36 1.333(5) . ?
N37 C38 1.356(5) . ?
N9 C1 1.328(5) . ?
N9 C8 1.330(5) . ?
N45 C46 1.354(5) . ?
N45 N49 1.358(5) . ?
N45 C36 1.427(4) . ?
N44 C43 1.328(5) . ?
N44 C36 1.330(5) . ?
N10 C11 1.359(5) . ?
N10 N14 1.360(4) . ?
N10 C1 1.423(5) . ?
N13 N14 1.300(5) . ?
N13 C12 1.370(5) . ?
N40 C41 1.316(5) . ?
N40 C39 1.391(5) . ?
N5 C6 1.311(5) . ?
N5 C4 1.387(5) . ?
N49 N48 1.302(5) . ?
N48 C47 1.373(5) . ?
C38 C39 1.383(5) . ?
C4 C3 1.377(5) . ?
C4 C8 1.417(5) . ?
C12 C11 1.363(5) . ?
C12 C15 1.472(5) . ?
C39 C43 1.418(5) . ?
C11 H11 0.9300 . ?
C47 C46 1.364(5) . ?
C47 C50 1.470(5) . ?
C46 H46 0.9300 . ?
C50 C51 1.393(6) . ?
C50 C55 1.395(6) . ?
C15 C20 1.389(6) . ?
C15 C16 1.406(5) . ?
C6 H6 0.9300 . ?
C29 C30 1.513(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C20 C19 1.388(6) . ?
C20 H20 0.9300 . ?
C41 H41 0.9300 . ?
C64 C65 1.518(6) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C51 C52 1.385(6) . ?
C51 H51 0.9300 . ?
C30 C31 1.525(7) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C26 C27 1.479(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C19 C18 1.382(7) . ?
C19 H19 0.9300 . ?
C54 C53 1.379(7) . ?
C54 C55 1.391(6) . ?
C54 H54 0.9300 . ?
C18 C17 1.382(7) . ?
C18 H18 0.9300 . ?
C53 C52 1.381(7) . ?
C53 H53 0.9300 . ?
C16 C17 1.385(6) . ?
C16 H16 0.9300 . ?
C55 H55 0.9300 . ?
C23 C24 1.490(7) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C52 H52 0.9300 . ?
C65 C66 1.521(6) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C17 H17 0.9300 . ?
C61 C62 1.493(7) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C58 C59 1.482(6) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C66 C67 1.517(6) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C34 C35 1.505(8) . ?
C34 C33 1.529(7) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C33 C32 1.514(7) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C32 C31 1.533(8) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C69 C70 1.512(8) . ?
C69 C68 1.539(8) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C67 C68 1.531(7) . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 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
O28 P21 O25 112.80(16) . . ?
O28 P21 O22 115.73(17) . . ?
O25 P21 O22 104.44(16) . . ?
O28 P21 C3 111.08(17) . . ?
O25 P21 C3 106.48(16) . . ?
O22 P21 C3 105.59(16) . . ?
O63 P56 O57 112.15(16) . . ?
O63 P56 O60 116.28(17) . . ?
O57 P56 O60 103.78(17) . . ?
O63 P56 C38 110.59(17) . . ?
O57 P56 C38 107.75(17) . . ?
O60 P56 C38 105.69(16) . . ?
C26 O25 P21 127.3(3) . . ?
C23 O22 P21 122.0(3) . . ?
C61 O60 P56 121.0(3) . . ?
C58 O57 P56 127.6(3) . . ?
C8 N7 C6 105.7(3) . . ?
C8 N7 C29 128.5(3) . . ?
C6 N7 C29 125.8(3) . . ?
C43 N42 C41 105.6(3) . . ?
C43 N42 C64 126.4(3) . . ?
C41 N42 C64 127.8(3) . . ?
C1 N2 C3 117.3(3) . . ?
C36 N37 C38 117.5(3) . . ?
C1 N9 C8 111.0(3) . . ?
C46 N45 N49 110.9(3) . . ?
C46 N45 C36 128.6(3) . . ?
N49 N45 C36 120.4(3) . . ?
C43 N44 C36 110.8(3) . . ?
C11 N10 N14 110.2(3) . . ?
C11 N10 C1 128.7(3) . . ?
N14 N10 C1 121.1(3) . . ?
N14 N13 C12 109.8(3) . . ?
C41 N40 C39 103.8(3) . . ?
C6 N5 C4 103.8(3) . . ?
N13 N14 N10 107.0(3) . . ?
N48 N49 N45 106.5(3) . . ?
N49 N48 C47 109.8(3) . . ?
N37 C38 C39 119.1(3) . . ?
N37 C38 P56 114.7(3) . . ?
C39 C38 P56 126.1(3) . . ?
C3 C4 N5 134.1(3) . . ?
C3 C4 C8 116.2(3) . . ?
N5 C4 C8 109.7(3) . . ?
C11 C12 N13 107.8(3) . . ?
C11 C12 C15 130.2(4) . . ?
N13 C12 C15 122.0(3) . . ?
N9 C8 N7 128.3(3) . . ?
N9 C8 C4 125.8(3) . . ?
N7 C8 C4 105.9(3) . . ?
C38 C39 N40 134.5(3) . . ?
C38 C39 C43 116.0(3) . . ?
N40 C39 C43 109.5(3) . . ?
N44 C36 N37 130.0(3) . . ?
N44 C36 N45 115.0(3) . . ?
N37 C36 N45 114.9(3) . . ?
N10 C11 C12 105.2(3) . . ?
N10 C11 H11 127.4 . . ?
C12 C11 H11 127.4 . . ?
C46 C47 N48 107.9(3) . . ?
C46 C47 C50 130.8(4) . . ?
N48 C47 C50 121.4(3) . . ?
N2 C3 C4 119.6(3) . . ?
N2 C3 P21 114.7(3) . . ?
C4 C3 P21 125.7(3) . . ?
N44 C43 N42 127.2(3) . . ?
N44 C43 C39 126.5(3) . . ?
N42 C43 C39 106.3(3) . . ?
N45 C46 C47 104.8(3) . . ?
N45 C46 H46 127.6 . . ?
C47 C46 H46 127.6 . . ?
N9 C1 N2 130.1(3) . . ?
N9 C1 N10 115.5(3) . . ?
N2 C1 N10 114.4(3) . . ?
C51 C50 C55 118.8(4) . . ?
C51 C50 C47 120.6(4) . . ?
C55 C50 C47 120.6(4) . . ?
C20 C15 C16 119.0(4) . . ?
C20 C15 C12 120.9(3) . . ?
C16 C15 C12 120.1(4) . . ?
N5 C6 N7 115.0(3) . . ?
N5 C6 H6 122.5 . . ?
N7 C6 H6 122.5 . . ?
N7 C29 C30 112.9(3) . . ?
N7 C29 H29A 109.0 . . ?
C30 C29 H29A 109.0 . . ?
N7 C29 H29B 109.0 . . ?
C30 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
C19 C20 C15 120.1(4) . . ?
C19 C20 H20 120.0 . . ?
C15 C20 H20 120.0 . . ?
N40 C41 N42 114.7(3) . . ?
N40 C41 H41 122.6 . . ?
N42 C41 H41 122.6 . . ?
N42 C64 C65 112.2(3) . . ?
N42 C64 H64A 109.2 . . ?
C65 C64 H64A 109.2 . . ?
N42 C64 H64B 109.2 . . ?
C65 C64 H64B 109.2 . . ?
H64A C64 H64B 107.9 . . ?
C52 C51 C50 120.6(4) . . ?
C52 C51 H51 119.7 . . ?
C50 C51 H51 119.7 . . ?
C29 C30 C31 115.2(4) . . ?
C29 C30 H30A 108.5 . . ?
C31 C30 H30A 108.5 . . ?
C29 C30 H30B 108.5 . . ?
C31 C30 H30B 108.5 . . ?
H30A C30 H30B 107.5 . . ?
O25 C26 C27 109.5(4) . . ?
O25 C26 H26A 109.8 . . ?
C27 C26 H26A 109.8 . . ?
O25 C26 H26B 109.8 . . ?
C27 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
C18 C19 C20 120.9(4) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C53 C54 C55 120.5(4) . . ?
C53 C54 H54 119.7 . . ?
C55 C54 H54 119.7 . . ?
C19 C18 C17 119.3(4) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C54 C53 C52 119.8(4) . . ?
C54 C53 H53 120.1 . . ?
C52 C53 H53 120.1 . . ?
C17 C16 C15 119.9(4) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C54 C55 C50 120.1(4) . . ?
C54 C55 H55 120.0 . . ?
C50 C55 H55 120.0 . . ?
O22 C23 C24 107.8(4) . . ?
O22 C23 H23A 110.1 . . ?
C24 C23 H23A 110.1 . . ?
O22 C23 H23B 110.1 . . ?
C24 C23 H23B 110.1 . . ?
H23A C23 H23B 108.5 . . ?
C53 C52 C51 120.3(4) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C64 C65 C66 113.2(4) . . ?
C64 C65 H65A 108.9 . . ?
C66 C65 H65A 108.9 . . ?
C64 C65 H65B 108.9 . . ?
C66 C65 H65B 108.9 . . ?
H65A C65 H65B 107.7 . . ?
C18 C17 C16 120.8(4) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
O60 C61 C62 107.5(4) . . ?
O60 C61 H61A 110.2 . . ?
C62 C61 H61A 110.2 . . ?
O60 C61 H61B 110.2 . . ?
C62 C61 H61B 110.2 . . ?
H61A C61 H61B 108.5 . . ?
O57 C58 C59 109.6(4) . . ?
O57 C58 H58A 109.8 . . ?
C59 C58 H58A 109.8 . . ?
O57 C58 H58B 109.8 . . ?
C59 C58 H58B 109.8 . . ?
H58A C58 H58B 108.2 . . ?
C67 C66 C65 113.6(4) . . ?
C67 C66 H66A 108.8 . . ?
C65 C66 H66A 108.8 . . ?
C67 C66 H66B 108.8 . . ?
C65 C66 H66B 108.8 . . ?
H66A C66 H66B 107.7 . . ?
C35 C34 C33 114.2(4) . . ?
C35 C34 H34A 108.7 . . ?
C33 C34 H34A 108.7 . . ?
C35 C34 H34B 108.7 . . ?
C33 C34 H34B 108.7 . . ?
H34A C34 H34B 107.6 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C32 C33 C34 111.6(4) . . ?
C32 C33 H33A 109.3 . . ?
C34 C33 H33A 109.3 . . ?
C32 C33 H33B 109.3 . . ?
C34 C33 H33B 109.3 . . ?
H33A C33 H33B 108.0 . . ?
C33 C32 C31 116.0(4) . . ?
C33 C32 H32A 108.3 . . ?
C31 C32 H32A 108.3 . . ?
C33 C32 H32B 108.3 . . ?
C31 C32 H32B 108.3 . . ?
H32A C32 H32B 107.4 . . ?
C70 C69 C68 114.6(4) . . ?
C70 C69 H69A 108.6 . . ?
C68 C69 H69A 108.6 . . ?
C70 C69 H69B 108.6 . . ?
C68 C69 H69B 108.6 . . ?
H69A C69 H69B 107.6 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C66 C67 C68 113.3(4) . . ?
C66 C67 H67A 108.9 . . ?
C68 C67 H67A 108.9 . . ?
C66 C67 H67B 108.9 . . ?
C68 C67 H67B 108.9 . . ?
H67A C67 H67B 107.7 . . ?
C30 C31 C32 115.9(4) . . ?
C30 C31 H31A 108.3 . . ?
C32 C31 H31A 108.3 . . ?
C30 C31 H31B 108.3 . . ?
C32 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C67 C68 C69 114.4(4) . . ?
C67 C68 H68A 108.7 . . ?
C69 C68 H68A 108.7 . . ?
C67 C68 H68B 108.7 . . ?
C69 C68 H68B 108.7 . . ?
H68A C68 H68B 107.6 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
 
_refine_diff_density_max    1.318
_refine_diff_density_min   -0.472
_refine_diff_density_rms    0.110



# start Validation Reply Form
_vrf_PLAT930_kek_70b
;
PROBLEM: Type_2 Test for Missed Twinning from FCF data
RESPONSE: TWIN instruction with recommended twin Law ( 0 0 1)[ 2 0 5] 
(Est.d BASF =  0.22) was included in the refinement process but gave a 
limited improvement of the structure. The refined value of BASF was 0.0378.   
;
# end Validation Reply Form