#------------------------------------------------------------------------------
#$Date: 2019-11-26 09:13:46 +0200 (Tue, 26 Nov 2019) $
#$Revision: 243143 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/33/4133322.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_4133322
loop_
_publ_author_name
'Zhai, Feng'
'Bukhryakov, Konstantin V.'
'Schrock, Richard R.'
'Hoveyda, Amir H.'
'Tsay, Charlene'
'Müller, Peter'
_publ_section_title
;
 Syntheses of Molybdenum Oxo Benzylidene Complexes.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13609
_journal_page_last               13613
_journal_paper_doi               10.1021/jacs.8b09616
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C51.5 H70 F24 Mo2 O11'
_chemical_formula_weight         1512.95
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/2
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0065(4)
_cell_length_b                   17.0065(4)
_cell_length_c                   21.4575(6)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.23
_cell_measurement_theta_min      2.24
_cell_volume                     6206.0(3)
_computing_cell_refinement       'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_data_collection       'APEX3 v2017.3.0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT 8.38A (Bruker-AXS, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/2 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Photon2 CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            394249
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.967
_diffrn_reflns_theta_min         1.528
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Herbst-Irmer et al., 2015)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             3068
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.35(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         13651
_refine_ls_number_restraints     615
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0396
_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)+(0.0194P)²+6.5987P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0869
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                12714
_reflns_number_total             13651
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b09616_si_002.cif
_cod_data_source_block           P18075
_cod_original_formula_sum        'C51.50 H70 F24 Mo2 O11'
_cod_database_code               4133322
_shelx_shelxl_version_number     2017/2
_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   0.866
_shelx_estimated_absorpt_t_max   0.937
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
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 0.49253(2) 0.09294(2) 0.31560(2) 0.01761(4) Uani 1 1 d . . . . .
C11 C 0.49121(18) 0.13999(16) 0.24281(12) 0.0203(5) Uani 1 1 d . . . . .
C12 C 0.49021(16) 0.17812(15) 0.18232(13) 0.0203(4) Uani 1 1 d . . . . .
C13 C 0.41870(18) 0.1923(2) 0.15171(15) 0.0250(6) Uani 1 1 d . . . . .
H13 H 0.371029 0.174127 0.169765 0.030 Uiso 1 1 calc R U . . .
C14 C 0.4167(2) 0.2323(2) 0.09550(16) 0.0294(7) Uani 1 1 d . . . . .
H14 H 0.367824 0.241867 0.075388 0.035 Uiso 1 1 calc R U . . .
C15 C 0.4864(2) 0.25857(18) 0.06857(13) 0.0248(6) Uani 1 1 d . . . . .
C16 C 0.5581(2) 0.2433(2) 0.09712(15) 0.0252(6) Uani 1 1 d . . . . .
H16 H 0.605811 0.260021 0.078237 0.030 Uiso 1 1 calc R U . . .
C17 C 0.55939(19) 0.20329(19) 0.15364(15) 0.0240(6) Uani 1 1 d . . . . .
H17 H 0.608436 0.192867 0.173153 0.029 Uiso 1 1 calc R U . . .
O1 O 0.47804(16) 0.29914(17) 0.01420(11) 0.0340(6) Uani 1 1 d . . . . .
C18 C 0.5477(3) 0.3268(3) -0.01565(19) 0.0453(10) Uani 1 1 d . . . . .
H18A H 0.576217 0.361870 0.012669 0.068 Uiso 1 1 calc R U . . .
H18B H 0.533504 0.355570 -0.053599 0.068 Uiso 1 1 calc R U . . .
H18C H 0.581192 0.281979 -0.026543 0.068 Uiso 1 1 calc R U . . .
O2 O 0.40360(13) 0.13768(12) 0.35941(10) 0.0212(4) Uani 1 1 d . . . . .
C21 C 0.34111(18) 0.18908(19) 0.35137(15) 0.0236(5) Uani 1 1 d . . . . .
C22 C 0.3592(2) 0.2595(2) 0.30970(19) 0.0324(7) Uani 1 1 d . . . . .
H22A H 0.400016 0.291895 0.329226 0.049 Uiso 1 1 calc R U . . .
H22B H 0.311437 0.290954 0.304062 0.049 Uiso 1 1 calc R U . . .
H22C H 0.377786 0.240939 0.269051 0.049 Uiso 1 1 calc R U . . .
C23 C 0.3208(2) 0.2204(2) 0.41705(19) 0.0347(8) Uani 1 1 d . . . . .
F1 F 0.26338(16) 0.27454(17) 0.41585(12) 0.0466(6) Uani 1 1 d . . . . .
F2 F 0.38327(16) 0.25357(17) 0.44285(13) 0.0472(6) Uani 1 1 d . . . . .
F3 F 0.29688(18) 0.16321(18) 0.45572(12) 0.0505(7) Uani 1 1 d . . . . .
C24 C 0.2723(2) 0.1421(2) 0.3242(2) 0.0348(8) Uani 1 1 d . . . . .
F4 F 0.25712(15) 0.07634(17) 0.35583(14) 0.0496(7) Uani 1 1 d . . . . .
F5 F 0.28819(15) 0.12102(17) 0.26565(12) 0.0441(6) Uani 1 1 d . . . . .
F6 F 0.20509(13) 0.18359(17) 0.32169(15) 0.0507(7) Uani 1 1 d . . . . .
O3 O 0.56980(12) 0.15170(13) 0.36292(10) 0.0208(4) Uani 1 1 d . . . . .
C31 C 0.62150(19) 0.2140(2) 0.35738(16) 0.0262(6) Uani 1 1 d . . . . .
C32 C 0.5907(2) 0.28238(19) 0.3181(2) 0.0354(7) Uani 1 1 d . . . . .
H32A H 0.575484 0.262998 0.276840 0.053 Uiso 1 1 calc R U . . .
H32B H 0.632076 0.322131 0.313638 0.053 Uiso 1 1 calc R U . . .
H32C H 0.544950 0.305830 0.338681 0.053 Uiso 1 1 calc R U . . .
C33 C 0.6984(2) 0.1821(3) 0.32951(17) 0.0360(8) Uani 1 1 d . . . . .
F7 F 0.68648(14) 0.15962(17) 0.27056(11) 0.0413(6) Uani 1 1 d . . . . .
F8 F 0.72667(15) 0.11994(19) 0.35977(13) 0.0515(7) Uani 1 1 d . . . . .
F9 F 0.75514(15) 0.2370(2) 0.32823(13) 0.0611(9) Uani 1 1 d . . . . .
C34 C 0.6363(2) 0.2435(2) 0.42465(19) 0.0351(8) Uani 1 1 d . . . . .
F10 F 0.66717(17) 0.18879(16) 0.46171(11) 0.0434(6) Uani 1 1 d . . . . .
F11 F 0.6848(2) 0.30573(17) 0.42659(13) 0.0579(8) Uani 1 1 d . . . . .
F12 F 0.56876(17) 0.26571(16) 0.45038(13) 0.0469(6) Uani 1 1 d . . . . .
O4 O 0.500000 0.000000 0.40475(12) 0.0218(5) Uani 1 2 d S TU P . .
C41 C 0.5630(11) 0.0089(11) 0.4459(11) 0.020(2) Uani 0.5 1 d . U P A -1
H41A H 0.565795 0.063117 0.462582 0.024 Uiso 0.5 1 calc R U P A -1
H41B H 0.613633 -0.004509 0.425782 0.024 Uiso 0.5 1 calc R U P A -1
C42 C 0.5416(4) -0.0509(4) 0.4974(3) 0.0274(13) Uani 0.5 1 d . U P A -1
H42A H 0.557598 -0.104746 0.485402 0.033 Uiso 0.5 1 calc R U P A -1
H42B H 0.567300 -0.036990 0.537335 0.033 Uiso 0.5 1 calc R U P A -1
C43 C 0.4520(4) -0.0447(4) 0.5029(3) 0.0255(12) Uani 0.5 1 d . U P A -1
H43A H 0.427524 -0.097487 0.502104 0.031 Uiso 0.5 1 calc R U P A -1
H43B H 0.436889 -0.017847 0.542020 0.031 Uiso 0.5 1 calc R U P A -1
C44 C 0.4267(12) 0.0035(11) 0.4463(10) 0.020(2) Uani 0.5 1 d . U P A -1
H44A H 0.413851 0.058268 0.458051 0.024 Uiso 0.5 1 calc R U P A -1
H44B H 0.380640 -0.020467 0.425324 0.024 Uiso 0.5 1 calc R U P A -1
O5 O 0.42544(12) -0.00609(14) 0.29573(9) 0.0205(4) Uani 1 1 d D . . . .
H5 H 0.401(2) -0.010(3) 0.2629(13) 0.025 Uiso 1 1 d D U . . .
O1S O 0.3603(3) -0.0210(4) 0.1785(3) 0.0337(12) Uani 0.505(7) 1 d D U P B 1
C1S C 0.2788(4) -0.0311(5) 0.1672(4) 0.0378(17) Uani 0.505(7) 1 d D U P B 1
H1S1 H 0.247746 -0.018394 0.204951 0.045 Uiso 0.505(7) 1 calc R U P B 1
H1S2 H 0.267167 -0.085914 0.154601 0.045 Uiso 0.505(7) 1 calc R U P B 1
C2S C 0.2605(6) 0.0253(8) 0.1153(5) 0.048(2) Uani 0.505(7) 1 d D U P B 1
H2S1 H 0.251421 0.079107 0.131322 0.058 Uiso 0.505(7) 1 calc R U P B 1
H2S2 H 0.213828 0.008125 0.091233 0.058 Uiso 0.505(7) 1 calc R U P B 1
C3S C 0.3354(5) 0.0211(6) 0.0757(3) 0.046(2) Uani 0.505(7) 1 d D U P B 1
H3S1 H 0.328809 -0.015689 0.040375 0.055 Uiso 0.505(7) 1 calc R U P B 1
H3S2 H 0.349654 0.073633 0.059302 0.055 Uiso 0.505(7) 1 calc R U P B 1
C4S C 0.3971(4) -0.0084(5) 0.1207(3) 0.0305(14) Uani 0.505(7) 1 d D U P B 1
H4S1 H 0.420232 -0.058119 0.105174 0.037 Uiso 0.505(7) 1 calc R U P B 1
H4S2 H 0.439704 0.030820 0.125125 0.037 Uiso 0.505(7) 1 calc R U P B 1
O1T O 0.3286(4) -0.0222(5) 0.1958(3) 0.0432(16) Uani 0.495(7) 1 d D U P B 2
C1T C 0.2454(5) -0.0297(6) 0.1970(4) 0.052(2) Uani 0.495(7) 1 d D U P B 2
H1T1 H 0.224204 -0.008305 0.236475 0.062 Uiso 0.495(7) 1 calc R U P B 2
H1T2 H 0.230236 -0.085804 0.193920 0.062 Uiso 0.495(7) 1 calc R U P B 2
C2T C 0.2134(7) 0.0150(10) 0.1429(6) 0.081(4) Uani 0.495(7) 1 d D U P B 2
H2T1 H 0.196041 0.068216 0.155737 0.097 Uiso 0.495(7) 1 calc R U P B 2
H2T2 H 0.168459 -0.013009 0.123750 0.097 Uiso 0.495(7) 1 calc R U P B 2
C3T C 0.2826(6) 0.0196(10) 0.0982(4) 0.056(3) Uani 0.495(7) 1 d D U P B 2
H3T1 H 0.273493 -0.013970 0.061168 0.067 Uiso 0.495(7) 1 calc R U P B 2
H3T2 H 0.291412 0.074372 0.084217 0.067 Uiso 0.495(7) 1 calc R U P B 2
C4T C 0.3523(4) -0.0101(5) 0.1357(3) 0.0319(15) Uani 0.495(7) 1 d D U P B 2
H4T1 H 0.371983 -0.059919 0.117616 0.038 Uiso 0.495(7) 1 calc R U P B 2
H4T2 H 0.395350 0.028989 0.134594 0.038 Uiso 0.495(7) 1 calc R U P B 2
C5S C 0.5555(10) 0.5902(7) 0.1969(6) 0.071(4) Uani 0.5 1 d D U P C -1
H5S1 H 0.538510 0.569283 0.237325 0.107 Uiso 0.5 1 calc R U P C -1
H5S2 H 0.546034 0.646983 0.195677 0.107 Uiso 0.5 1 calc R U P C -1
H5S3 H 0.611668 0.579791 0.191161 0.107 Uiso 0.5 1 calc R U P C -1
C6S C 0.5096(8) 0.5508(7) 0.1456(5) 0.047(2) Uani 0.5 1 d D U P C -1
H6S1 H 0.526137 0.573163 0.105099 0.057 Uiso 0.5 1 calc R U P C -1
H6S2 H 0.453018 0.562694 0.151223 0.057 Uiso 0.5 1 calc R U P C -1
C7S C 0.5205(8) 0.4626(7) 0.1439(5) 0.054(3) Uani 0.5 1 d D U P C -1
H7S1 H 0.576900 0.450667 0.137625 0.065 Uiso 0.5 1 calc R U P C -1
H7S2 H 0.491225 0.441019 0.107845 0.065 Uiso 0.5 1 calc R U P C -1
C8S C 0.4924(7) 0.4219(6) 0.2029(5) 0.061(3) Uani 0.5 1 d D U P C -1
H8S1 H 0.498401 0.364384 0.197808 0.074 Uiso 0.5 1 calc R U P C -1
H8S2 H 0.526064 0.438501 0.238153 0.074 Uiso 0.5 1 calc R U P C -1
C9S C 0.4077(8) 0.4403(10) 0.2182(9) 0.102(5) Uani 0.5 1 d D U P C -1
H9S1 H 0.404689 0.491092 0.239616 0.153 Uiso 0.5 1 calc R U P C -1
H9S2 H 0.386406 0.399064 0.245308 0.153 Uiso 0.5 1 calc R U P C -1
H9S3 H 0.376913 0.442592 0.179615 0.153 Uiso 0.5 1 calc R U P C -1
C10S C 0.447(3) 0.536(4) 0.597(2) 0.082(9) Uani 0.140(8) 1 d D U P D -1
H10A H 0.453794 0.518267 0.640505 0.122 Uiso 0.140(8) 1 calc R U P D -1
H10B H 0.436945 0.592233 0.596375 0.122 Uiso 0.140(8) 1 calc R U P D -1
H10C H 0.403408 0.507385 0.578109 0.122 Uiso 0.140(8) 1 calc R U P D -1
C11S C 0.522(2) 0.518(4) 0.5614(15) 0.083(7) Uani 0.140(8) 1 d D U P D -1
H11A H 0.566377 0.546216 0.581393 0.100 Uiso 0.140(8) 1 calc R U P D -1
H11B H 0.532835 0.461355 0.563123 0.100 Uiso 0.140(8) 1 calc R U P D -1
C12S C 0.516(3) 0.544(2) 0.4942(15) 0.085(7) Uani 0.140(8) 1 d D U P D -1
H12A H 0.465932 0.572120 0.487800 0.102 Uiso 0.140(8) 1 calc R U P D -1
H12B H 0.559550 0.580718 0.484829 0.102 Uiso 0.140(8) 1 calc R U P D -1
C13S C 0.520(4) 0.475(2) 0.4495(16) 0.086(7) Uani 0.140(8) 1 d D U P D -1
H13A H 0.470267 0.445563 0.451831 0.103 Uiso 0.140(8) 1 calc R U P D -1
H13B H 0.563146 0.439804 0.462628 0.103 Uiso 0.140(8) 1 calc R U P D -1
C14S C 0.534(4) 0.500(4) 0.3830(15) 0.088(10) Uani 0.140(8) 1 d D U P D -1
H14A H 0.536080 0.453646 0.356211 0.133 Uiso 0.140(8) 1 calc R U P D -1
H14B H 0.491029 0.534589 0.369325 0.133 Uiso 0.140(8) 1 calc R U P D -1
H14C H 0.583959 0.528826 0.380128 0.133 Uiso 0.140(8) 1 calc R U P D -1
C10T C 0.475(4) 0.520(6) 0.619(2) 0.080(9) Uani 0.110(8) 1 d D U P D -2
H10D H 0.487894 0.492943 0.657758 0.121 Uiso 0.110(8) 1 calc R U P D -2
H10E H 0.496194 0.573062 0.619198 0.121 Uiso 0.110(8) 1 calc R U P D -2
H10F H 0.417661 0.521694 0.613660 0.121 Uiso 0.110(8) 1 calc R U P D -2
C11T C 0.510(4) 0.475(4) 0.565(2) 0.084(7) Uani 0.110(8) 1 d D U P D -2
H11C H 0.568059 0.471604 0.570292 0.101 Uiso 0.110(8) 1 calc R U P D -2
H11D H 0.489507 0.420225 0.564753 0.101 Uiso 0.110(8) 1 calc R U P D -2
C12T C 0.492(4) 0.513(3) 0.503(2) 0.084(7) Uani 0.110(8) 1 d D U P D -2
H12C H 0.541673 0.533765 0.484637 0.101 Uiso 0.110(8) 1 calc R U P D -2
H12D H 0.455909 0.557161 0.509196 0.101 Uiso 0.110(8) 1 calc R U P D -2
C13T C 0.456(3) 0.455(4) 0.457(2) 0.087(7) Uani 0.110(8) 1 d D U P D -2
H13C H 0.468647 0.400798 0.470613 0.105 Uiso 0.110(8) 1 calc R U P D -2
H13D H 0.398205 0.461199 0.457987 0.105 Uiso 0.110(8) 1 calc R U P D -2
C14T C 0.486(6) 0.468(5) 0.392(2) 0.086(9) Uani 0.110(8) 1 d D U P D -2
H14D H 0.460909 0.429576 0.363708 0.129 Uiso 0.110(8) 1 calc R U P D -2
H14E H 0.472468 0.521184 0.378095 0.129 Uiso 0.110(8) 1 calc R U P D -2
H14F H 0.542874 0.460813 0.390715 0.129 Uiso 0.110(8) 1 calc R U P D -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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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
C11 Mo1 O2 104.06(12) . .
C11 Mo1 O3 103.88(12) . .
O2 Mo1 O3 94.16(9) . .
C11 Mo1 O5 98.64(11) . 2_655
O2 Mo1 O5 154.70(9) . 2_655
O3 Mo1 O5 91.08(9) . 2_655
C11 Mo1 O5 100.36(11) . .
O2 Mo1 O5 89.38(9) . .
O3 Mo1 O5 153.82(9) . .
O5 Mo1 O5 75.54(9) 2_655 .
C11 Mo1 O4 167.37(10) . .
O2 Mo1 O4 85.19(7) . .
O3 Mo1 O4 83.68(7) . .
O5 Mo1 O4 70.80(6) 2_655 .
O5 Mo1 O4 70.76(6) . .
C11 Mo1 Mo1 117.09(9) . 2_655
O2 Mo1 Mo1 117.01(7) . 2_655
O3 Mo1 Mo1 117.36(7) . 2_655
O5 Mo1 Mo1 40.27(6) 2_655 2_655
O5 Mo1 Mo1 40.21(6) . 2_655
O4 Mo1 Mo1 50.34(4) . 2_655
C12 C11 Mo1 179.4(2) . .
C17 C12 C13 118.2(3) . .
C17 C12 C11 121.5(3) . .
C13 C12 C11 120.4(3) . .
C14 C13 C12 120.9(3) . .
C14 C13 H13 119.6 . .
C12 C13 H13 119.6 . .
C13 C14 C15 119.8(3) . .
C13 C14 H14 120.1 . .
C15 C14 H14 120.1 . .
O1 C15 C16 124.3(3) . .
O1 C15 C14 115.4(3) . .
C16 C15 C14 120.3(3) . .
C15 C16 C17 119.3(3) . .
C15 C16 H16 120.4 . .
C17 C16 H16 120.4 . .
C16 C17 C12 121.5(3) . .
C16 C17 H17 119.3 . .
C12 C17 H17 119.3 . .
C15 O1 C18 117.7(3) . .
O1 C18 H18A 109.5 . .
O1 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
O1 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C21 O2 Mo1 141.8(2) . .
O2 C21 C22 114.4(3) . .
O2 C21 C24 107.7(3) . .
C22 C21 C24 109.9(3) . .
O2 C21 C23 106.0(3) . .
C22 C21 C23 108.0(3) . .
C24 C21 C23 110.9(3) . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
F2 C23 F1 107.5(3) . .
F2 C23 F3 107.1(3) . .
F1 C23 F3 106.7(3) . .
F2 C23 C21 110.4(3) . .
F1 C23 C21 112.4(3) . .
F3 C23 C21 112.4(3) . .
F4 C24 F5 107.0(4) . .
F4 C24 F6 107.2(3) . .
F5 C24 F6 105.9(3) . .
F4 C24 C21 113.1(3) . .
F5 C24 C21 110.1(3) . .
F6 C24 C21 113.0(3) . .
C31 O3 Mo1 141.4(2) . .
O3 C31 C32 114.4(3) . .
O3 C31 C33 107.7(3) . .
C32 C31 C33 110.2(3) . .
O3 C31 C34 105.7(3) . .
C32 C31 C34 108.9(3) . .
C33 C31 C34 109.8(3) . .
C31 C32 H32A 109.5 . .
C31 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C31 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
F8 C33 F7 106.8(4) . .
F8 C33 F9 107.6(3) . .
F7 C33 F9 106.8(3) . .
F8 C33 C31 113.5(3) . .
F7 C33 C31 109.9(3) . .
F9 C33 C31 111.9(4) . .
F12 C34 F10 106.9(3) . .
F12 C34 F11 107.0(4) . .
F10 C34 F11 106.9(3) . .
F12 C34 C31 109.8(3) . .
F10 C34 C31 113.3(3) . .
F11 C34 C31 112.6(3) . .
C41 O4 C44 104.6(4) . .
C41 O4 Mo1 121.1(7) . 2_655
C44 O4 Mo1 120.9(9) . 2_655
C41 O4 Mo1 117.2(9) . .
C44 O4 Mo1 112.4(7) . .
Mo1 O4 Mo1 79.31(8) 2_655 .
O4 C41 C42 101.5(14) . .
O4 C41 H41A 111.5 . .
C42 C41 H41A 111.5 . .
O4 C41 H41B 111.5 . .
C42 C41 H41B 111.5 . .
H41A C41 H41B 109.3 . .
C43 C42 C41 104.1(8) . .
C43 C42 H42A 110.9 . .
C41 C42 H42A 110.9 . .
C43 C42 H42B 110.9 . .
C41 C42 H42B 110.9 . .
H42A C42 H42B 109.0 . .
C44 C43 C42 104.9(9) . .
C44 C43 H43A 110.8 . .
C42 C43 H43A 110.8 . .
C44 C43 H43B 110.8 . .
C42 C43 H43B 110.8 . .
H43A C43 H43B 108.8 . .
C43 C44 O4 102.2(10) . .
C43 C44 H44A 111.3 . .
O4 C44 H44A 111.3 . .
C43 C44 H44B 111.3 . .
O4 C44 H44B 111.3 . .
H44A C44 H44B 109.2 . .
Mo1 O5 Mo1 99.53(8) 2_655 .
Mo1 O5 H5 117(3) 2_655 .
Mo1 O5 H5 122(3) . .
C4S O1S C1S 107.7(6) . .
O1S C1S C2S 104.5(6) . .
O1S C1S H1S1 110.8 . .
C2S C1S H1S1 110.8 . .
O1S C1S H1S2 110.8 . .
C2S C1S H1S2 110.8 . .
H1S1 C1S H1S2 108.9 . .
C1S C2S C3S 102.0(6) . .
C1S C2S H2S1 111.4 . .
C3S C2S H2S1 111.4 . .
C1S C2S H2S2 111.4 . .
C3S C2S H2S2 111.4 . .
H2S1 C2S H2S2 109.2 . .
C4S C3S C2S 103.8(6) . .
C4S C3S H3S1 111.0 . .
C2S C3S H3S1 111.0 . .
C4S C3S H3S2 111.0 . .
C2S C3S H3S2 111.0 . .
H3S1 C3S H3S2 109.0 . .
O1S C4S C3S 107.8(5) . .
O1S C4S H4S1 110.1 . .
C3S C4S H4S1 110.1 . .
O1S C4S H4S2 110.1 . .
C3S C4S H4S2 110.1 . .
H4S1 C4S H4S2 108.5 . .
C4T O1T C1T 108.9(6) . .
O1T C1T C2T 107.6(8) . .
O1T C1T H1T1 110.2 . .
C2T C1T H1T1 110.2 . .
O1T C1T H1T2 110.2 . .
C2T C1T H1T2 110.2 . .
H1T1 C1T H1T2 108.5 . .
C1T C2T C3T 103.6(7) . .
C1T C2T H2T1 111.0 . .
C3T C2T H2T1 111.0 . .
C1T C2T H2T2 111.0 . .
C3T C2T H2T2 111.0 . .
H2T1 C2T H2T2 109.0 . .
C4T C3T C2T 104.6(6) . .
C4T C3T H3T1 110.8 . .
C2T C3T H3T1 110.8 . .
C4T C3T H3T2 110.8 . .
C2T C3T H3T2 110.8 . .
H3T1 C3T H3T2 108.9 . .
O1T C4T C3T 108.7(6) . .
O1T C4T H4T1 109.9 . .
C3T C4T H4T1 109.9 . .
O1T C4T H4T2 109.9 . .
C3T C4T H4T2 109.9 . .
H4T1 C4T H4T2 108.3 . .
C6S C5S H5S1 109.5 . .
C6S C5S H5S2 109.5 . .
H5S1 C5S H5S2 109.5 . .
C6S C5S H5S3 109.5 . .
H5S1 C5S H5S3 109.5 . .
H5S2 C5S H5S3 109.5 . .
C5S C6S C7S 113.3(9) . .
C5S C6S H6S1 108.9 . .
C7S C6S H6S1 108.9 . .
C5S C6S H6S2 108.9 . .
C7S C6S H6S2 108.9 . .
H6S1 C6S H6S2 107.7 . .
C6S C7S C8S 113.1(9) . .
C6S C7S H7S1 109.0 . .
C8S C7S H7S1 109.0 . .
C6S C7S H7S2 109.0 . .
C8S C7S H7S2 109.0 . .
H7S1 C7S H7S2 107.8 . .
C9S C8S C7S 112.8(10) . .
C9S C8S H8S1 109.0 . .
C7S C8S H8S1 109.0 . .
C9S C8S H8S2 109.0 . .
C7S C8S H8S2 109.0 . .
H8S1 C8S H8S2 107.8 . .
C8S C9S H9S1 109.5 . .
C8S C9S H9S2 109.5 . .
H9S1 C9S H9S2 109.5 . .
C8S C9S H9S3 109.5 . .
H9S1 C9S H9S3 109.5 . .
H9S2 C9S H9S3 109.5 . .
C11S C10S H10A 109.5 . .
C11S C10S H10B 109.5 . .
H10A C10S H10B 109.5 . .
C11S C10S H10C 109.5 . .
H10A C10S H10C 109.5 . .
H10B C10S H10C 109.5 . .
C12S C11S C10S 112.2(17) . .
C12S C11S H11A 109.2 . .
C10S C11S H11A 109.2 . .
C12S C11S H11B 109.2 . .
C10S C11S H11B 109.2 . .
H11A C11S H11B 107.9 . .
C13S C12S C11S 112.6(18) . .
C13S C12S H12A 109.1 . .
C11S C12S H12A 109.1 . .
C13S C12S H12B 109.1 . .
C11S C12S H12B 109.1 . .
H12A C12S H12B 107.8 . .
C12S C13S C14S 113.1(18) . .
C12S C13S H13A 109.0 . .
C14S C13S H13A 109.0 . .
C12S C13S H13B 109.0 . .
C14S C13S H13B 109.0 . .
H13A C13S H13B 107.8 . .
C13S C14S H14A 109.5 . .
C13S C14S H14B 109.5 . .
H14A C14S H14B 109.5 . .
C13S C14S H14C 109.5 . .
H14A C14S H14C 109.5 . .
H14B C14S H14C 109.5 . .
C11T C10T H10D 109.5 . .
C11T C10T H10E 109.5 . .
H10D C10T H10E 109.5 . .
C11T C10T H10F 109.5 . .
H10D C10T H10F 109.5 . .
H10E C10T H10F 109.5 . .
C12T C11T C10T 112.1(18) . .
C12T C11T H11C 109.2 . .
C10T C11T H11C 109.2 . .
C12T C11T H11D 109.2 . .
C10T C11T H11D 109.2 . .
H11C C11T H11D 107.9 . .
C11T C12T C13T 111.9(18) . .
C11T C12T H12C 109.2 . .
C13T C12T H12C 109.2 . .
C11T C12T H12D 109.2 . .
C13T C12T H12D 109.2 . .
H12C C12T H12D 107.9 . .
C14T C13T C12T 111.8(18) . .
C14T C13T H13C 109.3 . .
C12T C13T H13C 109.3 . .
C14T C13T H13D 109.3 . .
C12T C13T H13D 109.3 . .
H13C C13T H13D 107.9 . .
C13T C14T H14D 109.5 . .
C13T C14T H14E 109.5 . .
H14D C14T H14E 109.5 . .
C13T C14T H14F 109.5 . .
H14D C14T H14F 109.5 . .
H14E C14T H14F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 C11 1.755(3) .
Mo1 O2 1.937(2) .
Mo1 O3 1.938(2) .
Mo1 O5 2.076(2) 2_655
Mo1 O5 2.078(2) .
Mo1 O4 2.485(2) .
Mo1 Mo1 3.1714(5) 2_655
C11 C12 1.451(4) .
C12 C17 1.395(4) .
C12 C13 1.403(4) .
C13 C14 1.386(5) .
C13 H13 0.9500 .
C14 C15 1.392(5) .
C14 H14 0.9500 .
C15 O1 1.363(4) .
C15 C16 1.390(5) .
C16 C17 1.391(4) .
C16 H16 0.9500 .
C17 H17 0.9500 .
O1 C18 1.426(5) .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
O2 C21 1.387(4) .
C21 C22 1.526(5) .
C21 C24 1.532(5) .
C21 C23 1.546(5) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 F2 1.323(5) .
C23 F1 1.342(4) .
C23 F3 1.342(5) .
C24 F4 1.333(5) .
C24 F5 1.335(5) .
C24 F6 1.345(4) .
O3 C31 1.382(4) .
C31 C32 1.528(5) .
C31 C33 1.537(5) .
C31 C34 1.548(5) .
C32 H32A 0.9800 .
C32 H32B 0.9800 .
C32 H32C 0.9800 .
C33 F8 1.331(5) .
C33 F7 1.337(4) .
C33 F9 1.343(5) .
C34 F12 1.330(5) .
C34 F10 1.331(5) .
C34 F11 1.343(4) .
O4 C41 1.40(2) .
O4 C44 1.53(2) .
C41 C42 1.55(2) .
C41 H41A 0.9900 .
C41 H41B 0.9900 .
C42 C43 1.531(9) .
C42 H42A 0.9900 .
C42 H42B 0.9900 .
C43 C44 1.53(2) .
C43 H43A 0.9900 .
C43 H43B 0.9900 .
C44 H44A 0.9900 .
C44 H44B 0.9900 .
O5 H5 0.82(2) .
O1S C4S 1.404(7) .
O1S C1S 1.419(7) .
C1S C2S 1.504(9) .
C1S H1S1 0.9900 .
C1S H1S2 0.9900 .
C2S C3S 1.533(12) .
C2S H2S1 0.9900 .
C2S H2S2 0.9900 .
C3S C4S 1.511(8) .
C3S H3S1 0.9900 .
C3S H3S2 0.9900 .
C4S H4S1 0.9900 .
C4S H4S2 0.9900 .
O1T C4T 1.366(7) .
O1T C1T 1.422(8) .
C1T C2T 1.491(10) .
C1T H1T1 0.9900 .
C1T H1T2 0.9900 .
C2T C3T 1.522(13) .
C2T H2T1 0.9900 .
C2T H2T2 0.9900 .
C3T C4T 1.519(9) .
C3T H3T1 0.9900 .
C3T H3T2 0.9900 .
C4T H4T1 0.9900 .
C4T H4T2 0.9900 .
C5S C6S 1.506(10) .
C5S H5S1 0.9800 .
C5S H5S2 0.9800 .
C5S H5S3 0.9800 .
C6S C7S 1.513(8) .
C6S H6S1 0.9900 .
C6S H6S2 0.9900 .
C7S C8S 1.519(10) .
C7S H7S1 0.9900 .
C7S H7S2 0.9900 .
C8S C9S 1.511(10) .
C8S H8S1 0.9900 .
C8S H8S2 0.9900 .
C9S H9S1 0.9800 .
C9S H9S2 0.9800 .
C9S H9S3 0.9800 .
C10S C11S 1.509(12) .
C10S H10A 0.9800 .
C10S H10B 0.9800 .
C10S H10C 0.9800 .
C11S C12S 1.508(12) .
C11S H11A 0.9900 .
C11S H11B 0.9900 .
C12S C13S 1.508(12) .
C12S H12A 0.9900 .
C12S H12B 0.9900 .
C13S C14S 1.508(12) .
C13S H13A 0.9900 .
C13S H13B 0.9900 .
C14S H14A 0.9800 .
C14S H14B 0.9800 .
C14S H14C 0.9800 .
C10T C11T 1.511(12) .
C10T H10D 0.9800 .
C10T H10E 0.9800 .
C10T H10F 0.9800 .
C11T C12T 1.511(12) .
C11T H11C 0.9900 .
C11T H11D 0.9900 .
C12T C13T 1.512(12) .
C12T H12C 0.9900 .
C12T H12D 0.9900 .
C13T C14T 1.511(12) .
C13T H13C 0.9900 .
C13T H13D 0.9900 .
C14T H14D 0.9800 .
C14T H14E 0.9800 .
C14T H14F 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O5 H5 O1S^a 0.82(2) 1.94(2) 2.760(6) 170(4) yes
O5 H5 O1T^b 0.82(2) 1.90(2) 2.718(6) 171(4) yes
