#------------------------------------------------------------------------------
#$Date: 2025-07-06 18:29:52 +0300 (Sun, 06 Jul 2025) $
#$Revision: 300767 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/86/7718692.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_7718692
loop_
_publ_author_name
'Wang, Xinchao'
'Liao, Qian'
_publ_section_title
;
 Synthesis of planar macrocyclic tetradentate phosphine-Mo complexes.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8769
_journal_page_last               8772
_journal_paper_doi               10.1039/d5dt00984g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C23 H43 Mo O3 P4, F6 P'
_chemical_formula_sum            'C23 H43 F6 Mo O3 P5'
_chemical_formula_weight         732.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2025-03-24 deposited with the CCDC.	2025-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.8221(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4237(7)
_cell_length_b                   9.6183(4)
_cell_length_c                   16.5169(6)
_cell_measurement_reflns_used    9646
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      63.39
_cell_measurement_theta_min      4.13
_cell_volume                     2937.66(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26021
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         63.438
_diffrn_reflns_theta_min         2.445
_exptl_absorpt_coefficient_mu    4.532
_exptl_absorpt_correction_T_max  0.7523
_exptl_absorpt_correction_T_min  0.5326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_recrystallization_method 'Vapour deposition'
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.48(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6980
_refine_ls_number_restraints     434
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0419
_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)+(0.0260P)²+12.7117P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                6939
_reflns_number_total             6980
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt00984g2.cif
_cod_data_source_block           '[(PPCprPPOxt)Mo(O)(OMe)][PF6]'
_cod_depositor_comments
'Adding full bibliography for 7718689--7718693.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7718692
_shelx_shelxl_version_number     2014/7
_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_min   0.338
_shelx_estimated_absorpt_t_max   0.782
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -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
Mo1 Mo 0.75151(2) 0.3751(2) 0.75553(3) 0.02475(12) Uani 1 1 d . . . . .
P2 P 0.82815(7) 0.2076(3) 0.85205(8) 0.0254(3) Uani 1 1 d . . . . .
P3 P 0.64262(8) 0.3461(3) 0.79614(8) 0.0255(4) Uani 1 1 d D . . . .
P4 P 0.67221(8) 0.5304(3) 0.65283(8) 0.0252(3) Uani 1 1 d D . . . .
P5 P 1.0000 0.8343(2) 1.0000 0.0332(5) Uani 1 2 d DS TU P . .
F1 F 0.9181(3) 0.7846(6) 0.9722(4) 0.076(3) Uani 0.5 1 d D U P A -1
F2 F 1.0811(3) 0.8841(7) 1.0210(6) 0.062(2) Uani 0.5 1 d D U P A -1
F3 F 0.9753(4) 0.9877(5) 1.0084(5) 0.087(3) Uani 0.5 1 d D U P A -1
F5 F 0.9927(4) 0.8619(7) 0.9024(3) 0.059(3) Uani 0.5 1 d D U P A -1
F4 F 1.0244(4) 0.6796(5) 0.9900(4) 0.074(3) Uani 0.5 1 d D U P A -1
F6 F 1.0064(4) 0.8050(7) 1.0958(3) 0.058(3) Uani 0.5 1 d D U P A -1
P6 P 0.5000 0.8912(3) 0.5000 0.0307(4) Uani 1 2 d DS TU P . .
F7 F 0.4945(8) 1.0521(6) 0.5163(6) 0.068(4) Uani 0.5 1 d D U P B -1
F8 F 0.5047(8) 0.7305(6) 0.4823(7) 0.075(3) Uani 0.5 1 d D U P B -1
F9 F 0.5851(3) 0.9032(16) 0.5238(8) 0.051(3) Uani 0.5 1 d D U P B -1
F10 F 0.4145(3) 0.8789(15) 0.4755(5) 0.049(3) Uani 0.5 1 d D U P B -1
F11 F 0.4928(5) 0.9203(13) 0.4032(4) 0.051(3) Uani 0.5 1 d D U P B -1
F12 F 0.5064(5) 0.8595(9) 0.5959(3) 0.070(3) Uani 0.5 1 d D U P B -1
P1 P 0.85792(7) 0.3906(3) 0.70659(8) 0.0258(3) Uani 1 1 d . . . . .
C7 C 0.7870(3) 0.1292(7) 0.9278(4) 0.0333(13) Uani 1 1 d . . . . .
H7A H 0.8113 0.0390 0.9465 0.040 Uiso 1 1 calc R U . . .
H7B H 0.7982 0.1900 0.9786 0.040 Uiso 1 1 calc R U . . .
C8 C 0.7047(4) 0.1030(7) 0.8977(4) 0.0376(13) Uani 1 1 d D U . . .
C9 C 0.6533(4) 0.2278(9) 0.8869(4) 0.0348(14) Uani 1 1 d . . . . .
H9A H 0.6697 0.2841 0.9395 0.042 Uiso 1 1 calc R U . . .
H9B H 0.6048 0.1913 0.8833 0.042 Uiso 1 1 calc R U . . .
C10 C 0.6824(8) 0.0034(13) 0.9594(7) 0.050(3) Uani 0.628(13) 1 d D U P C 1
H10A H 0.7238 -0.0290 1.0074 0.060 Uiso 0.628(13) 1 calc R U P C 1
H10B H 0.6436 0.0411 0.9804 0.060 Uiso 0.628(13) 1 calc R U P C 1
C11 C 0.681(3) -0.015(3) 0.8339(13) 0.054(4) Uani 0.628(13) 1 d D U P C 1
H11A H 0.6405 0.0111 0.7827 0.065 Uiso 0.628(13) 1 calc R U P C 1
H11B H 0.7208 -0.0576 0.8175 0.065 Uiso 0.628(13) 1 calc R U P C 1
O2 O 0.6574(7) -0.0982(12) 0.8932(6) 0.077(3) Uani 0.628(13) 1 d D U P C 1
C21 C 0.8267(8) 0.7728(12) 0.5939(9) 0.049(2) Uani 0.628(13) 1 d D U P C 1
H21A H 0.8757 0.7726 0.5871 0.058 Uiso 0.628(13) 1 calc R U P C 1
H21B H 0.7926 0.8402 0.5573 0.058 Uiso 0.628(13) 1 calc R U P C 1
C22 C 0.821(2) 0.7454(18) 0.6815(8) 0.047(3) Uani 0.628(13) 1 d D U P C 1
H22A H 0.7830 0.7961 0.6984 0.056 Uiso 0.628(13) 1 calc R U P C 1
H22B H 0.8661 0.7284 0.7282 0.056 Uiso 0.628(13) 1 calc R U P C 1
C10' C 0.8140(16) 0.7497(19) 0.5571(10) 0.062(5) Uani 0.372(13) 1 d D U P C 2
H10C H 0.8553 0.7268 0.5363 0.075 Uiso 0.372(13) 1 calc R U P C 2
H10D H 0.7717 0.7799 0.5097 0.075 Uiso 0.372(13) 1 calc R U P C 2
C11' C 0.825(4) 0.737(3) 0.6858(13) 0.062(5) Uani 0.372(13) 1 d D U P C 2
H11C H 0.7902 0.7602 0.7161 0.074 Uiso 0.372(13) 1 calc R U P C 2
H11D H 0.8723 0.7085 0.7264 0.074 Uiso 0.372(13) 1 calc R U P C 2
O2' O 0.8324(13) 0.8437(14) 0.6278(12) 0.080(5) Uani 0.372(13) 1 d D U P C 2
C21' C 0.6835(13) -0.0380(16) 0.9245(14) 0.046(3) Uani 0.372(13) 1 d D U P C 2
H21C H 0.7228 -0.0999 0.9576 0.055 Uiso 0.372(13) 1 calc R U P C 2
H21D H 0.6382 -0.0438 0.9400 0.055 Uiso 0.372(13) 1 calc R U P C 2
C22' C 0.677(4) -0.012(4) 0.8323(18) 0.042(3) Uani 0.372(13) 1 d D U P C 2
H22C H 0.6281 -0.0023 0.7916 0.050 Uiso 0.372(13) 1 calc R U P C 2
H22D H 0.7127 -0.0585 0.8091 0.050 Uiso 0.372(13) 1 calc R U P C 2
C1 C 0.8798(4) 0.2196(8) 0.6718(4) 0.0387(14) Uani 1 1 d . . . . .
H1A H 0.8375 0.1866 0.6254 0.046 Uiso 1 1 calc R U . . .
H1B H 0.9202 0.2314 0.6476 0.046 Uiso 1 1 calc R U . . .
C3 C 0.8523(4) 0.0669(7) 0.7926(4) 0.0371(13) Uani 1 1 d . . . . .
H3A H 0.8769 -0.0064 0.8333 0.044 Uiso 1 1 calc R U . . .
H3B H 0.8072 0.0262 0.7544 0.044 Uiso 1 1 calc R U . . .
C2 C 0.9008(4) 0.1064(8) 0.7395(6) 0.0482(18) Uani 1 1 d . . . . .
H2A H 0.9091 0.0206 0.7107 0.058 Uiso 1 1 calc R U . . .
H2B H 0.9481 0.1334 0.7798 0.058 Uiso 1 1 calc R U . . .
C6 C 0.9139(4) 0.2848(10) 0.9152(4) 0.0430(16) Uani 1 1 d . . . . .
H6A H 0.9093 0.3087 0.9716 0.052 Uiso 1 1 calc R U . . .
H6B H 0.9515 0.2121 0.9245 0.052 Uiso 1 1 calc R U . . .
C4 C 0.9398(4) 0.4389(10) 0.7936(5) 0.0442(16) Uani 1 1 d . . . . .
H4A H 0.9811 0.3887 0.7840 0.053 Uiso 1 1 calc R U . . .
H4B H 0.9483 0.5394 0.7878 0.053 Uiso 1 1 calc R U . . .
C5 C 0.9419(5) 0.4140(8) 0.8812(5) 0.059(2) Uani 1 1 d . . . . .
H5A H 0.9165 0.4939 0.8971 0.071 Uiso 1 1 calc R U . . .
H5B H 0.9933 0.4230 0.9155 0.071 Uiso 1 1 calc R U . . .
C12 C 0.5652(3) 0.2847(10) 0.7087(4) 0.0418(16) Uani 1 1 d . . . . .
H12A H 0.5778 0.1932 0.6897 0.050 Uiso 1 1 calc R U . . .
H12B H 0.5240 0.2701 0.7311 0.050 Uiso 1 1 calc R U . . .
C13 C 0.5399(3) 0.3818(11) 0.6298(4) 0.0463(14) Uani 1 1 d . . . . .
H13A H 0.5029 0.3296 0.5856 0.056 Uiso 1 1 calc R U . . .
H13B H 0.5145 0.4608 0.6465 0.056 Uiso 1 1 calc R U . . .
C14 C 0.5902(3) 0.4429(9) 0.5870(4) 0.0399(15) Uani 1 1 d . . . . .
H14A H 0.5625 0.5108 0.5443 0.048 Uiso 1 1 calc R U . . .
H14B H 0.6054 0.3674 0.5555 0.048 Uiso 1 1 calc R U . . .
C20 C 0.8476(4) 0.5091(8) 0.6161(4) 0.0353(14) Uani 1 1 d . . . . .
H20A H 0.8959 0.5452 0.6185 0.042 Uiso 1 1 calc R U . . .
H20B H 0.8291 0.4552 0.5627 0.042 Uiso 1 1 calc R U . . .
C18 C 0.7142(4) 0.6099(8) 0.5770(4) 0.0347(14) Uani 1 1 d . . . . .
H18A H 0.7046 0.5490 0.5265 0.042 Uiso 1 1 calc R U . . .
H18B H 0.6903 0.7002 0.5579 0.042 Uiso 1 1 calc R U . . .
C19 C 0.7963(4) 0.6344(7) 0.6125(4) 0.0405(14) Uani 1 1 d D U . . .
C23 C 0.6903(4) 0.1152(8) 0.6225(5) 0.0484(17) Uani 1 1 d . . . . .
H23A H 0.6464 0.1452 0.5786 0.073 Uiso 1 1 calc R U . . .
H23B H 0.6785 0.0394 0.6557 0.073 Uiso 1 1 calc R U . . .
H23C H 0.7259 0.0825 0.5956 0.073 Uiso 1 1 calc R U . . .
O1 O 0.7814(2) 0.5113(5) 0.8295(2) 0.0277(8) Uani 1 1 d . . . . .
C15 C 0.6197(5) 0.5203(10) 0.8302(6) 0.0285(14) Uani 0.656(11) 1 d D U P D 1
H15A H 0.5805 0.5080 0.8563 0.034 Uiso 0.656(11) 1 calc R U P D 1
H15B H 0.6626 0.5556 0.8751 0.034 Uiso 0.656(11) 1 calc R U P D 1
C16 C 0.5957(4) 0.6328(11) 0.7604(5) 0.0288(13) Uani 0.656(11) 1 d D U P D 1
H16A H 0.5831 0.7171 0.7873 0.035 Uiso 0.656(11) 1 calc R U P D 1
H16B H 0.5505 0.5997 0.7183 0.035 Uiso 0.656(11) 1 calc R U P D 1
C17 C 0.6480(5) 0.6777(10) 0.7106(6) 0.0283(13) Uani 0.656(11) 1 d D U P D 1
H17A H 0.6925 0.7169 0.7508 0.034 Uiso 0.656(11) 1 calc R U P D 1
H17B H 0.6248 0.7515 0.6695 0.034 Uiso 0.656(11) 1 calc R U P D 1
C15' C 0.5992(9) 0.5016(14) 0.8245(13) 0.0290(15) Uani 0.344(11) 1 d D U P D 2
H15C H 0.5467 0.4992 0.7943 0.035 Uiso 0.344(11) 1 calc R U P D 2
H15D H 0.6060 0.5014 0.8864 0.035 Uiso 0.344(11) 1 calc R U P D 2
C16' C 0.6323(9) 0.6363(16) 0.8003(9) 0.0289(13) Uani 0.344(11) 1 d D U P D 2
H16C H 0.6842 0.6386 0.8333 0.035 Uiso 0.344(11) 1 calc R U P D 2
H16D H 0.6090 0.7167 0.8187 0.035 Uiso 0.344(11) 1 calc R U P D 2
C17' C 0.6257(10) 0.6568(18) 0.7049(10) 0.0291(15) Uani 0.344(11) 1 d D U P D 2
H17C H 0.6442 0.7508 0.6986 0.035 Uiso 0.344(11) 1 calc R U P D 2
H17D H 0.5736 0.6561 0.6724 0.035 Uiso 0.344(11) 1 calc R U P D 2
O3 O 0.7189(2) 0.2254(5) 0.6756(2) 0.0285(9) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0583 0.0400 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2543 0.3332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.2130 2.1496 '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
O1 Mo1 O3 179.5(2) . . ?
O1 Mo1 P3 91.36(14) . . ?
O3 Mo1 P3 88.36(13) . . ?
O1 Mo1 P4 91.77(14) . . ?
O3 Mo1 P4 88.62(13) . . ?
P3 Mo1 P4 80.97(5) . . ?
O1 Mo1 P2 91.87(14) . . ?
O3 Mo1 P2 87.74(14) . . ?
P3 Mo1 P2 98.83(5) . . ?
P4 Mo1 P2 176.36(7) . . ?
O1 Mo1 P1 92.96(14) . . ?
O3 Mo1 P1 87.32(13) . . ?
P3 Mo1 P1 175.67(7) . . ?
P4 Mo1 P1 98.73(6) . . ?
P2 Mo1 P1 81.20(6) . . ?
C3 P2 C6 105.7(4) . . ?
C3 P2 C7 107.5(3) . . ?
C6 P2 C7 106.7(3) . . ?
C3 P2 Mo1 110.3(2) . . ?
C6 P2 Mo1 111.9(3) . . ?
C7 P2 Mo1 114.3(2) . . ?
C12 P3 C9 107.6(3) . . ?
C12 P3 C15' 97.6(7) . . ?
C9 P3 C15' 103.9(6) . . ?
C12 P3 C15 108.2(4) . . ?
C9 P3 C15 106.7(4) . . ?
C12 P3 Mo1 113.2(2) . . ?
C9 P3 Mo1 114.0(2) . . ?
C15' P3 Mo1 118.8(5) . . ?
C15 P3 Mo1 106.8(3) . . ?
C14 P4 C17 110.2(4) . . ?
C14 P4 C18 105.7(3) . . ?
C17 P4 C18 105.4(4) . . ?
C14 P4 C17' 96.7(6) . . ?
C18 P4 C17' 114.5(6) . . ?
C14 P4 Mo1 112.5(3) . . ?
C17 P4 Mo1 108.6(3) . . ?
C18 P4 Mo1 114.2(2) . . ?
C17' P4 Mo1 111.8(6) . . ?
F3 P5 F6 90.70(17) . . ?
F3 P5 F2 90.41(17) . . ?
F6 P5 F2 93.8(5) . . ?
F3 P5 F4 179.1(2) . . ?
F6 P5 F4 90.13(16) . . ?
F2 P5 F4 89.85(16) . . ?
F3 P5 F1 90.12(16) . . ?
F6 P5 F1 90.0(2) . . ?
F2 P5 F1 176.1(4) . . ?
F4 P5 F1 89.57(17) . . ?
F3 P5 F5 89.86(16) . . ?
F6 P5 F5 179.1(3) . . ?
F2 P5 F5 86.9(5) . . ?
F4 P5 F5 89.31(17) . . ?
F1 P5 F5 89.2(2) . . ?
F12 P6 F7 90.4(3) . . ?
F12 P6 F8 90.3(3) . . ?
F7 P6 F8 179.2(5) . . ?
F12 P6 F9 90.5(7) . . ?
F7 P6 F9 90.3(3) . . ?
F8 P6 F9 90.1(3) . . ?
F12 P6 F11 178.9(6) . . ?
F7 P6 F11 90.5(6) . . ?
F8 P6 F11 88.8(6) . . ?
F9 P6 F11 90.1(6) . . ?
F12 P6 F10 89.8(4) . . ?
F7 P6 F10 89.8(3) . . ?
F8 P6 F10 89.7(3) . . ?
F9 P6 F10 179.7(7) . . ?
F11 P6 F10 89.6(4) . . ?
C1 P1 C20 106.2(3) . . ?
C1 P1 C4 104.0(4) . . ?
C20 P1 C4 109.3(4) . . ?
C1 P1 Mo1 110.5(2) . . ?
C20 P1 Mo1 114.4(2) . . ?
C4 P1 Mo1 111.8(2) . . ?
C8 C7 P2 118.0(4) . . ?
C8 C7 H7A 107.8 . . ?
P2 C7 H7A 107.8 . . ?
C8 C7 H7B 107.8 . . ?
P2 C7 H7B 107.8 . . ?
H7A C7 H7B 107.1 . . ?
C21' C8 C22' 59.4(10) . . ?
C21' C8 C9 120.4(11) . . ?
C11 C8 C9 117(2) . . ?
C22' C8 C9 114(3) . . ?
C21' C8 C7 113.4(11) . . ?
C11 C8 C7 114(2) . . ?
C22' C8 C7 117(3) . . ?
C9 C8 C7 118.8(5) . . ?
C11 C8 C10 84.6(10) . . ?
C9 C8 C10 104.9(7) . . ?
C7 C8 C10 111.0(7) . . ?
C8 C9 P3 118.9(4) . . ?
C8 C9 H9A 107.6 . . ?
P3 C9 H9A 107.6 . . ?
C8 C9 H9B 107.6 . . ?
P3 C9 H9B 107.6 . . ?
H9A C9 H9B 107.0 . . ?
O2 C10 C8 90.9(7) . . ?
O2 C10 H10A 113.5 . . ?
C8 C10 H10A 113.5 . . ?
O2 C10 H10B 113.5 . . ?
C8 C10 H10B 113.5 . . ?
H10A C10 H10B 110.8 . . ?
O2 C11 C8 92.1(8) . . ?
O2 C11 H11A 113.3 . . ?
C8 C11 H11A 113.3 . . ?
O2 C11 H11B 113.3 . . ?
C8 C11 H11B 113.3 . . ?
H11A C11 H11B 110.6 . . ?
C10 O2 C11 92.2(7) . . ?
C22 C21 C19 60.4(6) . . ?
C22 C21 H21A 117.7 . . ?
C19 C21 H21A 117.7 . . ?
C22 C21 H21B 117.7 . . ?
C19 C21 H21B 117.7 . . ?
H21A C21 H21B 114.8 . . ?
C21 C22 C19 60.3(6) . . ?
C21 C22 H22A 117.7 . . ?
C19 C22 H22A 117.7 . . ?
C21 C22 H22B 117.7 . . ?
C19 C22 H22B 117.7 . . ?
H22A C22 H22B 114.9 . . ?
O2' C10' C19 90.9(8) . . ?
O2' C10' H10C 113.5 . . ?
C19 C10' H10C 113.5 . . ?
O2' C10' H10D 113.5 . . ?
C19 C10' H10D 113.5 . . ?
H10C C10' H10D 110.8 . . ?
O2' C11' C19 91.2(9) . . ?
O2' C11' H11C 113.4 . . ?
C19 C11' H11C 113.4 . . ?
O2' C11' H11D 113.4 . . ?
C19 C11' H11D 113.4 . . ?
H11C C11' H11D 110.7 . . ?
C10' O2' C11' 92.4(8) . . ?
C22' C21' C8 60.4(6) . . ?
C22' C21' H21C 117.7 . . ?
C8 C21' H21C 117.7 . . ?
C22' C21' H21D 117.7 . . ?
C8 C21' H21D 117.7 . . ?
H21C C21' H21D 114.8 . . ?
C21' C22' C8 60.2(7) . . ?
C21' C22' H22C 117.8 . . ?
C8 C22' H22C 117.8 . . ?
C21' C22' H22D 117.8 . . ?
C8 C22' H22D 117.8 . . ?
H22C C22' H22D 114.9 . . ?
C2 C1 P1 116.5(5) . . ?
C2 C1 H1A 108.2 . . ?
P1 C1 H1A 108.2 . . ?
C2 C1 H1B 108.2 . . ?
P1 C1 H1B 108.2 . . ?
H1A C1 H1B 107.3 . . ?
C2 C3 P2 115.8(5) . . ?
C2 C3 H3A 108.3 . . ?
P2 C3 H3A 108.3 . . ?
C2 C3 H3B 108.3 . . ?
P2 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?
C3 C2 C1 121.9(6) . . ?
C3 C2 H2A 106.8 . . ?
C1 C2 H2A 106.8 . . ?
C3 C2 H2B 106.8 . . ?
C1 C2 H2B 106.8 . . ?
H2A C2 H2B 106.7 . . ?
C5 C6 P2 119.0(5) . . ?
C5 C6 H6A 107.6 . . ?
P2 C6 H6A 107.6 . . ?
C5 C6 H6B 107.6 . . ?
P2 C6 H6B 107.6 . . ?
H6A C6 H6B 107.0 . . ?
C5 C4 P1 119.2(5) . . ?
C5 C4 H4A 107.5 . . ?
P1 C4 H4A 107.5 . . ?
C5 C4 H4B 107.5 . . ?
P1 C4 H4B 107.5 . . ?
H4A C4 H4B 107.0 . . ?
C4 C5 C6 126.4(6) . . ?
C4 C5 H5A 105.7 . . ?
C6 C5 H5A 105.7 . . ?
C4 C5 H5B 105.7 . . ?
C6 C5 H5B 105.7 . . ?
H5A C5 H5B 106.2 . . ?
C13 C12 P3 116.0(5) . . ?
C13 C12 H12A 108.3 . . ?
P3 C12 H12A 108.3 . . ?
C13 C12 H12B 108.3 . . ?
P3 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
C14 C13 C12 123.3(5) . . ?
C14 C13 H13A 106.5 . . ?
C12 C13 H13A 106.5 . . ?
C14 C13 H13B 106.5 . . ?
C12 C13 H13B 106.5 . . ?
H13A C13 H13B 106.5 . . ?
C13 C14 P4 118.4(4) . . ?
C13 C14 H14A 107.7 . . ?
P4 C14 H14A 107.7 . . ?
C13 C14 H14B 107.7 . . ?
P4 C14 H14B 107.7 . . ?
H14A C14 H14B 107.1 . . ?
C19 C20 P1 114.9(4) . . ?
C19 C20 H20A 108.6 . . ?
P1 C20 H20A 108.6 . . ?
C19 C20 H20B 108.6 . . ?
P1 C20 H20B 108.6 . . ?
H20A C20 H20B 107.5 . . ?
C19 C18 P4 115.1(4) . . ?
C19 C18 H18A 108.5 . . ?
P4 C18 H18A 108.5 . . ?
C19 C18 H18B 108.5 . . ?
P4 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
C21 C19 C22 59.3(8) . . ?
C21 C19 C18 118.5(8) . . ?
C22 C19 C18 116.2(16) . . ?
C11' C19 C18 119(3) . . ?
C11' C19 C10' 84.8(11) . . ?
C18 C19 C10' 106.1(12) . . ?
C21 C19 C20 113.7(8) . . ?
C22 C19 C20 117.6(15) . . ?
C11' C19 C20 113(3) . . ?
C18 C19 C20 118.3(5) . . ?
C10' C19 C20 108.9(12) . . ?
O3 C23 H23A 109.5 . . ?
O3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C16 C15 P3 116.7(6) . . ?
C16 C15 H15A 108.1 . . ?
P3 C15 H15A 108.1 . . ?
C16 C15 H15B 108.1 . . ?
P3 C15 H15B 108.1 . . ?
H15A C15 H15B 107.3 . . ?
C15 C16 C17 119.5(7) . . ?
C15 C16 H16A 107.4 . . ?
C17 C16 H16A 107.4 . . ?
C15 C16 H16B 107.4 . . ?
C17 C16 H16B 107.4 . . ?
H16A C16 H16B 107.0 . . ?
C16 C17 P4 111.8(7) . . ?
C16 C17 H17A 109.3 . . ?
P4 C17 H17A 109.3 . . ?
C16 C17 H17B 109.3 . . ?
P4 C17 H17B 109.3 . . ?
H17A C17 H17B 107.9 . . ?
C16' C15' P3 110.7(10) . . ?
C16' C15' H15C 109.5 . . ?
P3 C15' H15C 109.5 . . ?
C16' C15' H15D 109.5 . . ?
P3 C15' H15D 109.5 . . ?
H15C C15' H15D 108.1 . . ?
C15' C16' C17' 117.1(13) . . ?
C15' C16' H16C 108.0 . . ?
C17' C16' H16C 108.0 . . ?
C15' C16' H16D 108.0 . . ?
C17' C16' H16D 108.0 . . ?
H16C C16' H16D 107.3 . . ?
C16' C17' P4 118.8(11) . . ?
C16' C17' H17C 107.6 . . ?
P4 C17' H17C 107.6 . . ?
C16' C17' H17D 107.6 . . ?
P4 C17' H17D 107.6 . . ?
H17C C17' H17D 107.1 . . ?
C23 O3 Mo1 174.2(5) . . ?
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
Mo1 O1 1.764(4) . ?
Mo1 O3 1.925(4) . ?
Mo1 P3 2.4227(15) . ?
Mo1 P4 2.4251(15) . ?
Mo1 P2 2.4293(15) . ?
Mo1 P1 2.4433(13) . ?
P2 C3 1.815(7) . ?
P2 C6 1.830(7) . ?
P2 C7 1.840(7) . ?
P3 C12 1.835(7) . ?
P3 C9 1.843(7) . ?
P3 C15' 1.846(12) . ?
P3 C15 1.863(8) . ?
P4 C14 1.834(7) . ?
P4 C17 1.848(8) . ?
P4 C18 1.855(7) . ?
P4 C17' 1.873(11) . ?
P5 F3 1.571(5) . ?
P5 F6 1.574(5) . ?
P5 F2 1.581(5) . ?
P5 F4 1.586(5) . ?
P5 F1 1.589(5) . ?
P5 F5 1.596(5) . ?
P6 F12 1.579(5) . ?
P6 F7 1.580(5) . ?
P6 F8 1.581(5) . ?
P6 F9 1.581(5) . ?
P6 F11 1.586(5) . ?
P6 F10 1.589(5) . ?
P1 C1 1.835(7) . ?
P1 C20 1.841(7) . ?
P1 C4 1.846(7) . ?
C7 C8 1.544(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C21' 1.522(10) . ?
C8 C11 1.523(9) . ?
C8 C22' 1.526(11) . ?
C8 C9 1.537(10) . ?
C8 C10 1.554(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 O2 1.436(13) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 O2 1.439(17) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C21 C22 1.509(19) . ?
C21 C19 1.525(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C19 1.528(9) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C10' O2' 1.433(15) . ?
C10' C19 1.541(10) . ?
C10' H10C 0.9900 . ?
C10' H10D 0.9900 . ?
C11' O2' 1.436(17) . ?
C11' C19 1.531(11) . ?
C11' H11C 0.9900 . ?
C11' H11D 0.9900 . ?
C21' C22' 1.51(2) . ?
C21' H21C 0.9900 . ?
C21' H21D 0.9900 . ?
C22' H22C 0.9900 . ?
C22' H22D 0.9900 . ?
C1 C2 1.524(11) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C3 C2 1.518(11) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C6 C5 1.530(11) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C4 C5 1.456(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C12 C13 1.556(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.491(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C20 C19 1.554(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C18 C19 1.540(10) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C23 O3 1.379(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C15 C16 1.545(13) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.552(12) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C15' C16' 1.552(16) . ?
C15' H15C 0.9900 . ?
C15' H15D 0.9900 . ?
C16' C17' 1.554(16) . ?
C16' H16C 0.9900 . ?
C16' H16D 0.9900 . ?
C17' H17C 0.9900 . ?
C17' H17D 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
C3 P2 C7 C8 -88.4(5) . . . . ?
C6 P2 C7 C8 158.6(5) . . . . ?
Mo1 P2 C7 C8 34.4(6) . . . . ?
P2 C7 C8 C21' 136.6(10) . . . . ?
P2 C7 C8 C11 71.6(13) . . . . ?
P2 C7 C8 C22' 70.4(17) . . . . ?
P2 C7 C8 C9 -73.2(7) . . . . ?
P2 C7 C8 C10 165.2(6) . . . . ?
C21' C8 C9 P3 -139.0(11) . . . . ?
C11 C8 C9 P3 -70.9(12) . . . . ?
C22' C8 C9 P3 -71.4(16) . . . . ?
C7 C8 C9 P3 73.0(7) . . . . ?
C10 C8 C9 P3 -162.4(6) . . . . ?
C12 P3 C9 C8 92.7(6) . . . . ?
C15' P3 C9 C8 -164.4(8) . . . . ?
C15 P3 C9 C8 -151.3(6) . . . . ?
Mo1 P3 C9 C8 -33.6(6) . . . . ?
C11 C8 C10 O2 -3(2) . . . . ?
C9 C8 C10 O2 113.3(9) . . . . ?
C7 C8 C10 O2 -117.2(9) . . . . ?
C9 C8 C11 O2 -101(2) . . . . ?
C7 C8 C11 O2 114(2) . . . . ?
C10 C8 C11 O2 3(2) . . . . ?
C8 C10 O2 C11 3(2) . . . . ?
C8 C11 O2 C10 -3(3) . . . . ?
C19 C10' O2' C11' 7(4) . . . . ?
C19 C11' O2' C10' -7(4) . . . . ?
C9 C8 C21' C22' 102(4) . . . . ?
C7 C8 C21' C22' -108(3) . . . . ?
C9 C8 C22' C21' -112.2(19) . . . . ?
C7 C8 C22' C21' 102.6(18) . . . . ?
C20 P1 C1 C2 172.3(5) . . . . ?
C4 P1 C1 C2 57.1(6) . . . . ?
Mo1 P1 C1 C2 -63.1(6) . . . . ?
C6 P2 C3 C2 -54.3(6) . . . . ?
C7 P2 C3 C2 -167.9(5) . . . . ?
Mo1 P2 C3 C2 66.8(6) . . . . ?
P2 C3 C2 C1 -56.6(9) . . . . ?
P1 C1 C2 C3 54.9(9) . . . . ?
C3 P2 C6 C5 96.6(7) . . . . ?
C7 P2 C6 C5 -149.3(6) . . . . ?
Mo1 P2 C6 C5 -23.5(7) . . . . ?
C1 P1 C4 C5 -97.3(7) . . . . ?
C20 P1 C4 C5 149.7(7) . . . . ?
Mo1 P1 C4 C5 22.0(8) . . . . ?
P1 C4 C5 C6 41.4(12) . . . . ?
P2 C6 C5 C4 -41.0(12) . . . . ?
C9 P3 C12 C13 171.7(5) . . . . ?
C15' P3 C12 C13 64.5(8) . . . . ?
C15 P3 C12 C13 56.8(7) . . . . ?
Mo1 P3 C12 C13 -61.4(6) . . . . ?
P3 C12 C13 C14 49.0(10) . . . . ?
C12 C13 C14 P4 -49.6(11) . . . . ?
C17 P4 C14 C13 -59.9(8) . . . . ?
C18 P4 C14 C13 -173.3(6) . . . . ?
C17' P4 C14 C13 -55.4(9) . . . . ?
Mo1 P4 C14 C13 61.5(7) . . . . ?
C1 P1 C20 C19 152.7(5) . . . . ?
C4 P1 C20 C19 -95.7(6) . . . . ?
Mo1 P1 C20 C19 30.5(6) . . . . ?
C14 P4 C18 C19 -155.1(5) . . . . ?
C17 P4 C18 C19 88.1(6) . . . . ?
C17' P4 C18 C19 99.7(8) . . . . ?
Mo1 P4 C18 C19 -31.0(6) . . . . ?
C22 C21 C19 C18 105.1(18) . . . . ?
C22 C21 C19 C20 -109.2(18) . . . . ?
C21 C22 C19 C18 -109.0(12) . . . . ?
C21 C22 C19 C20 102.5(11) . . . . ?
O2' C11' C19 C18 -99(3) . . . . ?
O2' C11' C19 C10' 6(4) . . . . ?
O2' C11' C19 C20 115(3) . . . . ?
P4 C18 C19 C21 -135.8(8) . . . . ?
P4 C18 C19 C22 -68.3(9) . . . . ?
P4 C18 C19 C11' -64.3(13) . . . . ?
P4 C18 C19 C10' -157.4(9) . . . . ?
P4 C18 C19 C20 80.1(7) . . . . ?
O2' C10' C19 C11' -6(4) . . . . ?
O2' C10' C19 C18 112.8(16) . . . . ?
O2' C10' C19 C20 -118.9(15) . . . . ?
P1 C20 C19 C21 134.5(7) . . . . ?
P1 C20 C19 C22 68.1(11) . . . . ?
P1 C20 C19 C11' 66.7(18) . . . . ?
P1 C20 C19 C18 -79.7(7) . . . . ?
P1 C20 C19 C10' 159.1(9) . . . . ?
C12 P3 C15 C16 -54.7(8) . . . . ?
C9 P3 C15 C16 -170.2(6) . . . . ?
Mo1 P3 C15 C16 67.5(7) . . . . ?
P3 C15 C16 C17 -60.1(11) . . . . ?
C15 C16 C17 P4 60.1(10) . . . . ?
C14 P4 C17 C16 52.3(7) . . . . ?
C18 P4 C17 C16 165.9(6) . . . . ?
Mo1 P4 C17 C16 -71.3(7) . . . . ?
C12 P3 C15' C16' -110.4(12) . . . . ?
C9 P3 C15' C16' 139.3(11) . . . . ?
Mo1 P3 C15' C16' 11.4(15) . . . . ?
P3 C15' C16' C17' 60.2(17) . . . . ?
C15' C16' C17' P4 -63.6(18) . . . . ?
C14 P4 C17' C16' 108.3(13) . . . . ?
C18 P4 C17' C16' -141.1(11) . . . . ?
Mo1 P4 C17' C16' -9.2(15) . . . . ?
