#------------------------------------------------------------------------------
#$Date: 2025-03-04 22:01:45 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298236 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/73/7717338.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7717338
loop_
_publ_author_name
'Fener, Benjamin E.'
'Schüler, Philipp'
'Liebing, Phil'
'Görls, Helmar'
'Westerhausen, Matthias'
_publ_section_title
;
 Syntheses and structures of dimesitylphosphinite complexes of alkali
 metals and their catalytic activity in hydrophosphorylation reactions.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              181
_journal_page_last               197
_journal_paper_doi               10.1039/d4dt02721c
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         'C76 H124 K2 O6 P2'
_chemical_formula_sum            'C76 H124 K2 O6 P2'
_chemical_formula_weight         1273.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-10-18 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                97.812(4)
_cell_angle_beta                 110.737(4)
_cell_angle_gamma                96.310(4)
_cell_formula_units_Z            1
_cell_length_a                   11.8363(18)
_cell_length_b                   12.7037(18)
_cell_length_c                   14.054(2)
_cell_measurement_reflns_used    8990
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.425
_cell_measurement_theta_min      2.267
_cell_volume                     1929.3(5)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Diamond 4 (Brandenburg, 1997)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker APEX II'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20923
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.867
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.9282
_exptl_absorpt_correction_T_min  0.7734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0813 before and 0.0454 after correction.
The Ratio of minimum to maximum transmission is 0.8332.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         9360
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0639
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0002P)²+3.7553P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6347
_reflns_number_total             9360
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02721c2.cif
_cod_data_source_block           bn00600
_cod_depositor_comments
'Adding full bibliography for 7717331--7717346.cif.'
_cod_database_code               7717338
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.945
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C36-C37A \\sim C36-C37B
 with sigma of 0.02
 C38-C37A \\sim C38-C37B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C35 \\sim C36 \\sim C37A \\sim C37B \\sim C38: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(C37B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H36C)=Sof(H36D)=Sof(C37B)=Sof(H37C)=Sof(H37D)=Sof(H38C)=Sof(H38D)=1-FVAR(1)
 Sof(H36A)=Sof(H36B)=Sof(C37A)=Sof(H37A)=Sof(H37B)=Sof(H38A)=Sof(H38B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C22(H22), C25(H25), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C36(H36C,H36D), C37A(H37A,H37B), C37B(H37C,H37D),
 C38(H38A,H38B), C38(H38C,H38D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C18(H18), C20(H20)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C)
;
_olex2_date_sample_data_collection 2023-11-13
_olex2_date_sample_submission    2023-11-10
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
K1 K 0.36263(5) 0.06225(5) 0.49734(5) 0.03045(14) Uani 1 1 d . . . . .
P1 P 0.69428(6) 0.14119(5) 0.69429(5) 0.02115(14) Uani 1 1 d . . . . .
O1 O 0.59048(16) 0.11631(14) 0.58527(13) 0.0254(4) Uani 1 1 d . . . . .
O2 O 0.2440(2) 0.18751(19) 0.37588(19) 0.0602(8) Uani 1 1 d . . . . .
O3 O 0.1914(2) 0.0714(2) 0.58211(17) 0.0474(6) Uani 1 1 d . . . . .
C1 C 0.8040(2) 0.26602(19) 0.70792(18) 0.0195(5) Uani 1 1 d . . . . .
C2 C 0.8087(2) 0.3175(2) 0.62582(18) 0.0215(5) Uani 1 1 d . . . . .
C3 C 0.9055(2) 0.4003(2) 0.64417(19) 0.0240(5) Uani 1 1 d . . . . .
H3 H 0.907784 0.433681 0.588187 0.029 Uiso 1 1 calc R U . . .
C4 C 0.9988(2) 0.43614(19) 0.74032(19) 0.0216(5) Uani 1 1 d . . . . .
C5 C 0.9937(2) 0.3853(2) 0.82023(19) 0.0229(5) Uani 1 1 d . . . . .
H5 H 1.056082 0.408947 0.887141 0.028 Uiso 1 1 calc R U . . .
C6 C 0.9002(2) 0.30071(19) 0.80584(18) 0.0203(5) Uani 1 1 d . . . . .
C7 C 0.7148(2) 0.2858(2) 0.51496(19) 0.0263(5) Uani 1 1 d . . . . .
H7 H 0.645483 0.233205 0.515065 0.032 Uiso 1 1 calc R U . . .
C8 C 0.6619(3) 0.3822(2) 0.4727(2) 0.0370(7) Uani 1 1 d . . . . .
H8A H 0.599773 0.357361 0.402674 0.055 Uiso 1 1 calc R U . . .
H8B H 0.727822 0.434479 0.470359 0.055 Uiso 1 1 calc R U . . .
H8C H 0.624282 0.416529 0.517928 0.055 Uiso 1 1 calc R U . . .
C9 C 0.7714(3) 0.2296(3) 0.4444(2) 0.0387(7) Uani 1 1 d . . . . .
H9A H 0.841685 0.278669 0.445036 0.058 Uiso 1 1 calc R U . . .
H9B H 0.710159 0.209144 0.373641 0.058 Uiso 1 1 calc R U . . .
H9C H 0.798750 0.164838 0.469309 0.058 Uiso 1 1 calc R U . . .
C10 C 1.1049(2) 0.5237(2) 0.7558(2) 0.0269(6) Uani 1 1 d . . . . .
H10 H 1.156744 0.541287 0.831477 0.032 Uiso 1 1 calc R U . . .
C11 C 1.0632(3) 0.6270(2) 0.7236(2) 0.0382(7) Uani 1 1 d . . . . .
H11A H 1.015690 0.613137 0.648865 0.057 Uiso 1 1 calc R U . . .
H11B H 1.135103 0.682680 0.740348 0.057 Uiso 1 1 calc R U . . .
H11C H 1.012073 0.651628 0.760853 0.057 Uiso 1 1 calc R U . . .
C12 C 1.1842(3) 0.4830(3) 0.6988(2) 0.0379(7) Uani 1 1 d . . . . .
H12A H 1.214393 0.419190 0.723845 0.057 Uiso 1 1 calc R U . . .
H12B H 1.253972 0.539623 0.711591 0.057 Uiso 1 1 calc R U . . .
H12C H 1.135414 0.463982 0.624331 0.057 Uiso 1 1 calc R U . . .
C13 C 0.9084(2) 0.2471(2) 0.89753(19) 0.0237(5) Uani 1 1 d . . . . .
H13 H 0.835768 0.187970 0.873427 0.028 Uiso 1 1 calc R U . . .
C14 C 0.8995(3) 0.3236(2) 0.9867(2) 0.0387(7) Uani 1 1 d . . . . .
H14A H 0.969007 0.383375 1.012331 0.058 Uiso 1 1 calc R U . . .
H14B H 0.901253 0.284771 1.042691 0.058 Uiso 1 1 calc R U . . .
H14C H 0.822711 0.352114 0.962506 0.058 Uiso 1 1 calc R U . . .
C15 C 1.0225(3) 0.1941(3) 0.9315(2) 0.0358(7) Uani 1 1 d . . . . .
H15A H 1.023419 0.144292 0.872187 0.054 Uiso 1 1 calc R U . . .
H15B H 1.021141 0.154214 0.986213 0.054 Uiso 1 1 calc R U . . .
H15C H 1.096011 0.249779 0.957941 0.054 Uiso 1 1 calc R U . . .
C16 C 0.6165(2) 0.18986(19) 0.78337(19) 0.0199(5) Uani 1 1 d . . . . .
C17 C 0.5623(2) 0.28320(19) 0.77830(18) 0.0199(5) Uani 1 1 d . . . . .
C18 C 0.5058(2) 0.31467(19) 0.84713(19) 0.0222(5) Uani 1 1 d . . . . .
H18 H 0.471901 0.379116 0.843557 0.027 Uiso 1 1 calc R U . . .
C19 C 0.4977(2) 0.2544(2) 0.92062(19) 0.0223(5) Uani 1 1 d . . . . .
C20 C 0.5474(2) 0.1605(2) 0.92294(19) 0.0241(5) Uani 1 1 d . . . . .
H20 H 0.541136 0.117137 0.971457 0.029 Uiso 1 1 calc R U . . .
C21 C 0.6061(2) 0.1273(2) 0.85694(19) 0.0224(5) Uani 1 1 d . . . . .
C22 C 0.5613(2) 0.35298(19) 0.69797(19) 0.0230(5) Uani 1 1 d . . . . .
H22 H 0.596327 0.315785 0.650156 0.028 Uiso 1 1 calc R U . . .
C23 C 0.6421(3) 0.4635(2) 0.7490(2) 0.0325(6) Uani 1 1 d . . . . .
H23A H 0.610918 0.501145 0.797668 0.049 Uiso 1 1 calc R U . . .
H23B H 0.640665 0.506198 0.695654 0.049 Uiso 1 1 calc R U . . .
H23C H 0.726491 0.454013 0.786496 0.049 Uiso 1 1 calc R U . . .
C24 C 0.4311(3) 0.3661(2) 0.6330(2) 0.0339(6) Uani 1 1 d . . . . .
H24A H 0.379141 0.294954 0.604791 0.051 Uiso 1 1 calc R U . . .
H24B H 0.432776 0.402035 0.575907 0.051 Uiso 1 1 calc R U . . .
H24C H 0.398086 0.409717 0.676546 0.051 Uiso 1 1 calc R U . . .
C25 C 0.4407(2) 0.2868(2) 0.9992(2) 0.0255(5) Uani 1 1 d . . . . .
H25 H 0.392802 0.219779 1.005195 0.031 Uiso 1 1 calc R U . . .
C26 C 0.5416(3) 0.3314(2) 1.1058(2) 0.0346(6) Uani 1 1 d . . . . .
H26A H 0.595725 0.278325 1.125110 0.052 Uiso 1 1 calc R U . . .
H26B H 0.504284 0.346000 1.157314 0.052 Uiso 1 1 calc R U . . .
H26C H 0.589211 0.398336 1.103252 0.052 Uiso 1 1 calc R U . . .
C27 C 0.3530(3) 0.3663(2) 0.9700(2) 0.0322(6) Uani 1 1 d . . . . .
H27A H 0.398690 0.435687 0.970488 0.048 Uiso 1 1 calc R U . . .
H27B H 0.312989 0.376191 1.020072 0.048 Uiso 1 1 calc R U . . .
H27C H 0.290755 0.338314 0.900565 0.048 Uiso 1 1 calc R U . . .
C28 C 0.6535(2) 0.0206(2) 0.8644(2) 0.0281(6) Uani 1 1 d . . . . .
H28 H 0.711595 0.018203 0.827286 0.034 Uiso 1 1 calc R U . . .
C29 C 0.7230(3) 0.0078(2) 0.9754(2) 0.0392(7) Uani 1 1 d . . . . .
H29A H 0.787917 0.070506 1.011077 0.059 Uiso 1 1 calc R U . . .
H29B H 0.759621 -0.057748 0.974590 0.059 Uiso 1 1 calc R U . . .
H29C H 0.666297 0.002310 1.011776 0.059 Uiso 1 1 calc R U . . .
C30 C 0.5473(3) -0.0728(2) 0.8083(3) 0.0413(7) Uani 1 1 d . . . . .
H30A H 0.486474 -0.070405 0.840727 0.062 Uiso 1 1 calc R U . . .
H30B H 0.578077 -0.141227 0.812680 0.062 Uiso 1 1 calc R U . . .
H30C H 0.509059 -0.066827 0.735387 0.062 Uiso 1 1 calc R U . . .
C31 C 0.2666(4) 0.2794(3) 0.3338(3) 0.0585(10) Uani 1 1 d . . . . .
H31A H 0.355549 0.299510 0.349967 0.070 Uiso 1 1 calc R U . . .
H31B H 0.237735 0.341321 0.363371 0.070 Uiso 1 1 calc R U . . .
C32 C 0.1979(3) 0.2498(3) 0.2184(3) 0.0483(8) Uani 1 1 d . . . . .
H32A H 0.254012 0.233759 0.182341 0.058 Uiso 1 1 calc R U . . .
H32B H 0.155835 0.308909 0.191632 0.058 Uiso 1 1 calc R U . . .
C33 C 0.1051(3) 0.1494(3) 0.2038(2) 0.0444(8) Uani 1 1 d . . . . .
H33A H 0.020532 0.159763 0.164727 0.053 Uiso 1 1 calc R U . . .
H33B H 0.122926 0.085411 0.166524 0.053 Uiso 1 1 calc R U . . .
C34 C 0.1215(3) 0.1372(3) 0.3127(3) 0.0524(9) Uani 1 1 d . . . . .
H34A H 0.062240 0.172680 0.334999 0.063 Uiso 1 1 calc R U . . .
H34B H 0.108762 0.059973 0.317303 0.063 Uiso 1 1 calc R U . . .
C35 C 0.1006(3) 0.1392(3) 0.5715(3) 0.0496(8) Uani 1 1 d . U . . .
H35A H 0.026140 0.108104 0.509389 0.060 Uiso 1 1 calc R U . . .
H35B H 0.132417 0.211752 0.564040 0.060 Uiso 1 1 calc R U . . .
C36 C 0.0714(4) 0.1465(3) 0.6660(3) 0.0628(10) Uani 1 1 d D U . . .
H36A H -0.014201 0.111625 0.648591 0.075 Uiso 0.610(18) 1 calc R U P A 1
H36B H 0.081124 0.222947 0.698183 0.075 Uiso 0.610(18) 1 calc R U P A 1
H36C H 0.045699 0.215956 0.682749 0.075 Uiso 0.390(18) 1 calc R U P A 2
H36D H 0.007474 0.086126 0.660206 0.075 Uiso 0.390(18) 1 calc R U P A 2
C37A C 0.1622(7) 0.0878(10) 0.7419(5) 0.0515(18) Uani 0.610(18) 1 d D U P A 1
H37A H 0.207179 0.135313 0.810236 0.062 Uiso 0.610(18) 1 calc R U P A 1
H37B H 0.118955 0.021185 0.751487 0.062 Uiso 0.610(18) 1 calc R U P A 1
C37B C 0.1883(11) 0.1389(15) 0.7393(9) 0.056(3) Uani 0.390(18) 1 d D U P A 2
H37C H 0.178766 0.112351 0.799541 0.067 Uiso 0.390(18) 1 calc R U P A 2
H37D H 0.241158 0.210793 0.764325 0.067 Uiso 0.390(18) 1 calc R U P A 2
C38 C 0.2452(4) 0.0630(3) 0.6878(3) 0.0577(10) Uani 1 1 d D U . . .
H38A H 0.323876 0.113758 0.721348 0.069 Uiso 0.610(18) 1 calc R U P A 1
H38B H 0.262485 -0.011035 0.692784 0.069 Uiso 0.610(18) 1 calc R U P A 1
H38C H 0.335401 0.084789 0.714666 0.069 Uiso 0.390(18) 1 calc R U P A 2
H38D H 0.225340 -0.011538 0.697695 0.069 Uiso 0.390(18) 1 calc R U P A 2
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'
K K 0.2009 0.2494 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
K1 K1 P1 51.339(19) 2_656 . ?
P1 K1 K1 65.76(2) 2_656 2_656 ?
P1 K1 P1 117.10(2) 2_656 . ?
O1 K1 K1 43.96(4) . 2_656 ?
O1 K1 K1 41.75(4) 2_656 2_656 ?
O1 K1 P1 108.03(5) . 2_656 ?
O1 K1 P1 14.56(4) . . ?
O1 K1 P1 27.53(4) 2_656 2_656 ?
O1 K1 P1 91.77(4) 2_656 . ?
O1 K1 O1 85.70(6) . 2_656 ?
O1 K1 O2 117.35(7) . . ?
O1 K1 O2 119.33(8) 2_656 . ?
O1 K1 O3 124.29(7) 2_656 . ?
O1 K1 O3 128.22(7) . . ?
O2 K1 K1 130.37(7) . 2_656 ?
O2 K1 P1 124.87(5) . . ?
O2 K1 P1 94.06(6) . 2_656 ?
O2 K1 O3 85.91(8) . . ?
O3 K1 K1 143.63(6) . 2_656 ?
O3 K1 P1 116.07(5) . 2_656 ?
O3 K1 P1 114.19(5) . . ?
K1 P1 K1 62.90(2) 2_656 . ?
O1 P1 K1 51.07(7) . 2_656 ?
O1 P1 K1 23.95(7) . . ?
O1 P1 C1 110.17(10) . . ?
O1 P1 C16 103.97(10) . . ?
C1 P1 K1 125.88(8) . . ?
C1 P1 K1 119.80(8) . 2_656 ?
C1 P1 C16 101.48(10) . . ?
C16 P1 K1 82.56(7) . . ?
C16 P1 K1 136.44(8) . 2_656 ?
K1 O1 K1 94.30(6) . 2_656 ?
P1 O1 K1 141.49(11) . . ?
P1 O1 K1 101.40(9) . 2_656 ?
C31 O2 K1 140.5(2) . . ?
C31 O2 C34 105.4(2) . . ?
C34 O2 K1 112.12(18) . . ?
C35 O3 K1 130.7(2) . . ?
C38 O3 K1 108.71(19) . . ?
C38 O3 C35 108.6(3) . . ?
C2 C1 P1 125.50(18) . . ?
C6 C1 P1 115.95(17) . . ?
C6 C1 C2 117.9(2) . . ?
C1 C2 C7 123.9(2) . . ?
C3 C2 C1 119.5(2) . . ?
C3 C2 C7 116.5(2) . . ?
C2 C3 H3 118.5 . . ?
C4 C3 C2 123.0(2) . . ?
C4 C3 H3 118.5 . . ?
C3 C4 C5 117.2(2) . . ?
C3 C4 C10 121.2(2) . . ?
C5 C4 C10 121.6(2) . . ?
C4 C5 H5 118.9 . . ?
C4 C5 C6 122.2(2) . . ?
C6 C5 H5 118.9 . . ?
C1 C6 C13 122.3(2) . . ?
C5 C6 C1 120.2(2) . . ?
C5 C6 C13 117.5(2) . . ?
C2 C7 H7 107.8 . . ?
C2 C7 C8 112.6(2) . . ?
C8 C7 H7 107.8 . . ?
C9 C7 C2 110.2(2) . . ?
C9 C7 H7 107.8 . . ?
C9 C7 C8 110.4(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10 107.6 . . ?
C4 C10 C11 112.7(2) . . ?
C4 C10 C12 110.5(2) . . ?
C11 C10 H10 107.6 . . ?
C11 C10 C12 110.7(2) . . ?
C12 C10 H10 107.6 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C6 C13 H13 106.9 . . ?
C6 C13 C14 112.3(2) . . ?
C6 C13 C15 111.3(2) . . ?
C14 C13 H13 106.9 . . ?
C14 C13 C15 112.2(2) . . ?
C15 C13 H13 106.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 P1 123.63(18) . . ?
C17 C16 C21 117.5(2) . . ?
C21 C16 P1 118.83(18) . . ?
C16 C17 C22 122.0(2) . . ?
C18 C17 C16 120.6(2) . . ?
C18 C17 C22 117.5(2) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 C17 121.9(2) . . ?
C19 C18 H18 119.1 . . ?
C18 C19 C25 123.9(2) . . ?
C20 C19 C18 117.3(2) . . ?
C20 C19 C25 118.7(2) . . ?
C19 C20 H20 118.7 . . ?
C19 C20 C21 122.5(2) . . ?
C21 C20 H20 118.7 . . ?
C16 C21 C28 122.1(2) . . ?
C20 C21 C16 120.1(2) . . ?
C20 C21 C28 117.7(2) . . ?
C17 C22 H22 107.8 . . ?
C17 C22 C23 111.2(2) . . ?
C17 C22 C24 111.7(2) . . ?
C23 C22 H22 107.8 . . ?
C24 C22 H22 107.8 . . ?
C24 C22 C23 110.4(2) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C19 C25 H25 107.3 . . ?
C19 C25 C26 109.9(2) . . ?
C26 C25 H25 107.3 . . ?
C27 C25 C19 114.7(2) . . ?
C27 C25 H25 107.3 . . ?
C27 C25 C26 110.1(2) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C21 C28 H28 107.5 . . ?
C21 C28 C29 113.5(2) . . ?
C21 C28 C30 109.6(2) . . ?
C29 C28 H28 107.5 . . ?
C30 C28 H28 107.5 . . ?
C30 C28 C29 110.9(2) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O2 C31 H31A 110.3 . . ?
O2 C31 H31B 110.3 . . ?
O2 C31 C32 107.1(3) . . ?
H31A C31 H31B 108.6 . . ?
C32 C31 H31A 110.3 . . ?
C32 C31 H31B 110.3 . . ?
C31 C32 H32A 110.9 . . ?
C31 C32 H32B 110.9 . . ?
C31 C32 C33 104.2(3) . . ?
H32A C32 H32B 108.9 . . ?
C33 C32 H32A 110.9 . . ?
C33 C32 H32B 110.9 . . ?
C32 C33 H33A 111.0 . . ?
C32 C33 H33B 111.0 . . ?
H33A C33 H33B 109.0 . . ?
C34 C33 C32 103.8(3) . . ?
C34 C33 H33A 111.0 . . ?
C34 C33 H33B 111.0 . . ?
O2 C34 C33 106.0(3) . . ?
O2 C34 H34A 110.5 . . ?
O2 C34 H34B 110.5 . . ?
C33 C34 H34A 110.5 . . ?
C33 C34 H34B 110.5 . . ?
H34A C34 H34B 108.7 . . ?
O3 C35 H35A 110.2 . . ?
O3 C35 H35B 110.2 . . ?
O3 C35 C36 107.3(3) . . ?
H35A C35 H35B 108.5 . . ?
C36 C35 H35A 110.2 . . ?
C36 C35 H35B 110.2 . . ?
C35 C36 H36A 110.3 . . ?
C35 C36 H36B 110.3 . . ?
C35 C36 H36C 111.9 . . ?
C35 C36 H36D 111.9 . . ?
C35 C36 C37A 107.2(4) . . ?
H36A C36 H36B 108.5 . . ?
H36C C36 H36D 109.6 . . ?
C37A C36 H36A 110.3 . . ?
C37A C36 H36B 110.3 . . ?
C37B C36 C35 99.4(6) . . ?
C37B C36 H36C 111.9 . . ?
C37B C36 H36D 111.9 . . ?
C36 C37A H37A 111.3 . . ?
C36 C37A H37B 111.3 . . ?
H37A C37A H37B 109.2 . . ?
C38 C37A C36 102.2(4) . . ?
C38 C37A H37A 111.3 . . ?
C38 C37A H37B 111.3 . . ?
C36 C37B H37C 110.0 . . ?
C36 C37B H37D 110.0 . . ?
C36 C37B C38 108.4(7) . . ?
H37C C37B H37D 108.4 . . ?
C38 C37B H37C 110.0 . . ?
C38 C37B H37D 110.0 . . ?
O3 C38 C37A 110.4(4) . . ?
O3 C38 C37B 103.0(6) . . ?
O3 C38 H38A 109.6 . . ?
O3 C38 H38B 109.6 . . ?
O3 C38 H38C 111.2 . . ?
O3 C38 H38D 111.2 . . ?
C37A C38 H38A 109.6 . . ?
C37A C38 H38B 109.6 . . ?
C37B C38 H38C 111.2 . . ?
C37B C38 H38D 111.2 . . ?
H38A C38 H38B 108.1 . . ?
H38C C38 H38D 109.1 . . ?
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
K1 P1 3.2904(10) 2_656 ?
K1 P1 3.8422(10) . ?
K1 O1 2.5048(18) . ?
K1 O1 2.6112(19) 2_656 ?
K1 O2 2.637(2) . ?
K1 O3 2.695(2) . ?
P1 O1 1.5515(18) . ?
P1 C1 1.878(2) . ?
P1 C16 1.878(3) . ?
O2 C31 1.419(4) . ?
O2 C34 1.424(4) . ?
O3 C35 1.430(4) . ?
O3 C38 1.418(4) . ?
C1 C2 1.416(3) . ?
C1 C6 1.414(3) . ?
C2 C3 1.392(3) . ?
C2 C7 1.526(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.385(3) . ?
C4 C5 1.385(3) . ?
C4 C10 1.515(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(3) . ?
C6 C13 1.516(3) . ?
C7 H7 1.0000 . ?
C7 C8 1.532(4) . ?
C7 C9 1.525(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.521(4) . ?
C10 C12 1.522(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13 1.0000 . ?
C13 C14 1.520(4) . ?
C13 C15 1.529(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.407(3) . ?
C16 C21 1.417(3) . ?
C17 C18 1.398(3) . ?
C17 C22 1.525(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.390(3) . ?
C19 C20 1.386(3) . ?
C19 C25 1.520(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.392(4) . ?
C21 C28 1.525(3) . ?
C22 H22 1.0000 . ?
C22 C23 1.532(4) . ?
C22 C24 1.529(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25 1.0000 . ?
C25 C26 1.531(4) . ?
C25 C27 1.519(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28 1.0000 . ?
C28 C29 1.526(4) . ?
C28 C30 1.525(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.505(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.528(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.505(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.480(5) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 H36C 0.9900 . ?
C36 H36D 0.9900 . ?
C36 C37A 1.559(8) . ?
C36 C37B 1.425(10) . ?
C37A H37A 0.9900 . ?
C37A H37B 0.9900 . ?
C37A C38 1.475(7) . ?
C37B H37C 0.9900 . ?
C37B H37D 0.9900 . ?
C37B C38 1.485(10) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 H38C 0.9900 . ?
C38 H38D 0.9900 . ?
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
K1 P1 O1 K1 112.09(17) 2_656 . . . ?
K1 P1 O1 K1 -112.09(17) . . . 2_656 ?
K1 P1 C1 C2 -33.3(2) . . . . ?
K1 P1 C1 C2 43.2(2) 2_656 . . . ?
K1 P1 C1 C6 -127.00(16) 2_656 . . . ?
K1 P1 C1 C6 156.50(14) . . . . ?
K1 P1 C16 C17 -73.22(19) . . . . ?
K1 P1 C16 C17 -109.71(19) 2_656 . . . ?
K1 P1 C16 C21 67.2(2) 2_656 . . . ?
K1 P1 C16 C21 103.69(18) . . . . ?
K1 O2 C31 C32 127.3(3) . . . . ?
K1 O2 C34 C33 -129.9(2) . . . . ?
K1 O3 C35 C36 -154.6(2) . . . . ?
K1 O3 C38 C37A 169.5(6) . . . . ?
K1 O3 C38 C37B 141.9(8) . . . . ?
P1 C1 C2 C3 -170.81(19) . . . . ?
P1 C1 C2 C7 7.2(4) . . . . ?
P1 C1 C6 C5 172.97(18) . . . . ?
P1 C1 C6 C13 -5.5(3) . . . . ?
P1 C16 C17 C18 179.92(18) . . . . ?
P1 C16 C17 C22 0.6(3) . . . . ?
P1 C16 C21 C20 -179.06(18) . . . . ?
P1 C16 C21 C28 -1.4(3) . . . . ?
O1 P1 C1 C2 -12.7(2) . . . . ?
O1 P1 C1 C6 177.13(17) . . . . ?
O1 P1 C16 C17 -62.4(2) . . . . ?
O1 P1 C16 C21 114.51(19) . . . . ?
O2 C31 C32 C33 17.2(4) . . . . ?
O3 C35 C36 C37A 6.1(6) . . . . ?
O3 C35 C36 C37B 32.3(9) . . . . ?
C1 P1 O1 K1 112.58(10) . . . 2_656 ?
C1 P1 O1 K1 -135.33(15) . . . . ?
C1 P1 C16 C17 52.0(2) . . . . ?
C1 P1 C16 C21 -131.10(19) . . . . ?
C1 C2 C3 C4 -0.5(4) . . . . ?
C1 C2 C7 C8 128.1(3) . . . . ?
C1 C2 C7 C9 -108.1(3) . . . . ?
C1 C6 C13 C14 -117.3(3) . . . . ?
C1 C6 C13 C15 115.9(3) . . . . ?
C2 C1 C6 C5 2.0(3) . . . . ?
C2 C1 C6 C13 -176.5(2) . . . . ?
C2 C3 C4 C5 0.6(4) . . . . ?
C2 C3 C4 C10 177.7(2) . . . . ?
C3 C2 C7 C8 -53.8(3) . . . . ?
C3 C2 C7 C9 70.0(3) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C3 C4 C10 C11 56.7(3) . . . . ?
C3 C4 C10 C12 -67.8(3) . . . . ?
C4 C5 C6 C1 -2.0(4) . . . . ?
C4 C5 C6 C13 176.5(2) . . . . ?
C5 C4 C10 C11 -126.3(3) . . . . ?
C5 C4 C10 C12 109.3(3) . . . . ?
C5 C6 C13 C14 64.3(3) . . . . ?
C5 C6 C13 C15 -62.6(3) . . . . ?
C6 C1 C2 C3 -0.8(3) . . . . ?
C6 C1 C2 C7 177.3(2) . . . . ?
C7 C2 C3 C4 -178.7(2) . . . . ?
C10 C4 C5 C6 -176.5(2) . . . . ?
C16 P1 O1 K1 -139.38(9) . . . 2_656 ?
C16 P1 O1 K1 -27.29(18) . . . . ?
C16 P1 C1 C2 -122.4(2) . . . . ?
C16 P1 C1 C6 67.4(2) . . . . ?
C16 C17 C18 C19 -1.8(4) . . . . ?
C16 C17 C22 C23 -112.3(3) . . . . ?
C16 C17 C22 C24 123.9(2) . . . . ?
C16 C21 C28 C29 136.1(3) . . . . ?
C16 C21 C28 C30 -99.3(3) . . . . ?
C17 C16 C21 C20 -2.0(3) . . . . ?
C17 C16 C21 C28 175.7(2) . . . . ?
C17 C18 C19 C20 -0.4(4) . . . . ?
C17 C18 C19 C25 178.1(2) . . . . ?
C18 C17 C22 C23 68.3(3) . . . . ?
C18 C17 C22 C24 -55.5(3) . . . . ?
C18 C19 C20 C21 1.5(4) . . . . ?
C18 C19 C25 C26 -103.6(3) . . . . ?
C18 C19 C25 C27 21.1(3) . . . . ?
C19 C20 C21 C16 -0.3(4) . . . . ?
C19 C20 C21 C28 -178.0(2) . . . . ?
C20 C19 C25 C26 74.8(3) . . . . ?
C20 C19 C25 C27 -160.5(2) . . . . ?
C20 C21 C28 C29 -46.1(3) . . . . ?
C20 C21 C28 C30 78.4(3) . . . . ?
C21 C16 C17 C18 3.0(3) . . . . ?
C21 C16 C17 C22 -176.4(2) . . . . ?
C22 C17 C18 C19 177.5(2) . . . . ?
C25 C19 C20 C21 -177.1(2) . . . . ?
C31 O2 C34 C33 37.5(4) . . . . ?
C31 C32 C33 C34 5.1(4) . . . . ?
C32 C33 C34 O2 -25.7(4) . . . . ?
C34 O2 C31 C32 -34.2(4) . . . . ?
C35 O3 C38 C37A 22.2(7) . . . . ?
C35 O3 C38 C37B -5.3(9) . . . . ?
C35 C36 C37A C38 6.4(8) . . . . ?
C35 C36 C37B C38 -36.2(14) . . . . ?
C36 C37A C38 O3 -17.1(9) . . . . ?
C36 C37B C38 O3 27.2(14) . . . . ?
C38 O3 C35 C36 -17.1(4) . . . . ?
