# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Mo
_database_code_depnum_ccdc_archive 'CCDC 1407344'
_audit_update_record             
;
2015-12-13 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     '[(H)2Mo(dppe)2(O2CH)][BPh4]'
_chemical_formula_moiety         'C53 H51 Mo O2 P4, C24 H20 B'
_chemical_formula_sum            'C77 H71 B Mo O2 P4'
_chemical_formula_weight         1258.96

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'
B B 0.0013 0.0007 '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'
Mo Mo -1.6832 0.6857 '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                   17.4817(5)
_cell_length_b                   20.7047(5)
_cell_length_c                   17.5343(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.3380(10)
_cell_angle_gamma                90
_cell_volume                     6335.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    100347
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       blade
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_F_000             2624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.356
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7990
_exptl_absorpt_correction_T_max  0.9929
_exptl_absorpt_process_details   '(SADABS 2007/2; Sheldrick, 2007)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_reflns_number            50365
_diffrn_reflns_av_unetI/netI     0.0945
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.048
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             11116
_reflns_number_gt                7278
_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       'COLLECT (Hooft, 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1993)'
_computing_publication_material  
;
SHELXL-2014/7 (Sheldrick, 2015), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen et al., 2004)
;
_refine_special_details          
;
The two Mo---H distances were restrained to the same value, which was itself
freely refined.

One ring of the BPh₄⁻ anion was disordered over two positions. Refinement
was carried out with the geometry and thermal parameters of the two positions
restrained to the same values. The C--C distances in these groups were
restrained to 1.39(2)Å.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+47.1810P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11116
_refine_ls_number_parameters     790
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.0886
_refine_ls_wR_factor_ref         0.1764
_refine_ls_wR_factor_gt          0.1560
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.004
_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
C1 C 0.3056(4) 0.7979(4) 0.1548(4) 0.0352(17) Uani 1 1 d . . . . .
H1 H 0.3085 0.7964 0.2091 0.042 Uiso 1 1 calc R U . . .
C101 C 0.4730(4) 0.8752(3) 0.0114(4) 0.0353(17) Uani 1 1 d . . . . .
H10A H 0.5102 0.9066 -0.0077 0.042 Uiso 1 1 calc R U . . .
H10B H 0.4707 0.8815 0.0672 0.042 Uiso 1 1 calc R U . . .
C102 C 0.4993(4) 0.8061(4) -0.0051(4) 0.0407(18) Uani 1 1 d . . . . .
H10C H 0.5492 0.7978 0.0227 0.049 Uiso 1 1 calc R U . . .
H10D H 0.5063 0.8012 -0.0604 0.049 Uiso 1 1 calc R U . . .
C103 C 0.3586(4) 0.9723(3) -0.0028(4) 0.0319(16) Uani 1 1 d . . . . .
C104 C 0.3387(4) 1.0216(4) -0.0540(5) 0.044(2) Uani 1 1 d . . . . .
H104 H 0.3353 1.0134 -0.1074 0.053 Uiso 1 1 calc R U . . .
C105 C 0.3238(5) 1.0830(4) -0.0265(5) 0.048(2) Uani 1 1 d . . . . .
H105 H 0.3103 1.1169 -0.0613 0.057 Uiso 1 1 calc R U . . .
C106 C 0.3286(4) 1.0952(4) 0.0513(5) 0.047(2) Uani 1 1 d . . . . .
H106 H 0.3191 1.1373 0.0699 0.056 Uiso 1 1 calc R U . . .
C107 C 0.3471(4) 1.0461(4) 0.1010(5) 0.0428(19) Uani 1 1 d . . . . .
H107 H 0.3498 1.0541 0.1544 0.051 Uiso 1 1 calc R U . . .
C108 C 0.3620(4) 0.9847(3) 0.0742(5) 0.0383(18) Uani 1 1 d . . . . .
H108 H 0.3746 0.9509 0.1094 0.046 Uiso 1 1 calc R U . . .
C109 C 0.3964(4) 0.8999(3) -0.1370(4) 0.0329(16) Uani 1 1 d . . . . .
C110 C 0.4619(5) 0.9316(4) -0.1565(5) 0.060(2) Uani 1 1 d . . . . .
H110 H 0.4965 0.9483 -0.1176 0.072 Uiso 1 1 calc R U . . .
C111 C 0.4774(5) 0.9391(5) -0.2326(6) 0.072(3) Uani 1 1 d . . . . .
H111 H 0.5232 0.9602 -0.2454 0.086 Uiso 1 1 calc R U . . .
C112 C 0.4270(5) 0.9164(4) -0.2902(5) 0.053(2) Uani 1 1 d . . . . .
H112 H 0.4382 0.9217 -0.3423 0.064 Uiso 1 1 calc R U . . .
C113 C 0.3610(5) 0.8864(4) -0.2718(4) 0.0440(19) Uani 1 1 d . . . . .
H113 H 0.3247 0.8728 -0.3109 0.053 Uiso 1 1 calc R U . . .
C114 C 0.3474(4) 0.8760(3) -0.1962(4) 0.0365(17) Uani 1 1 d . . . . .
H114 H 0.3035 0.8519 -0.1840 0.044 Uiso 1 1 calc R U . . .
C115 C 0.4573(4) 0.7266(4) 0.1235(4) 0.0379(18) Uani 1 1 d . . . . .
C116 C 0.5052(5) 0.7663(4) 0.1693(5) 0.050(2) Uani 1 1 d . . . . .
H116 H 0.5280 0.8032 0.1477 0.061 Uiso 1 1 calc R U . . .
C117 C 0.5197(5) 0.7523(4) 0.2464(5) 0.061(3) Uani 1 1 d . . . . .
H117 H 0.5506 0.7806 0.2777 0.073 Uiso 1 1 calc R U . . .
C118 C 0.4898(5) 0.6978(5) 0.2776(5) 0.056(2) Uani 1 1 d . . . . .
H118 H 0.5017 0.6878 0.3298 0.067 Uiso 1 1 calc R U . . .
C119 C 0.4431(5) 0.6579(4) 0.2342(4) 0.050(2) Uani 1 1 d . . . . .
H119 H 0.4220 0.6203 0.2560 0.060 Uiso 1 1 calc R U . . .
C120 C 0.4265(5) 0.6727(4) 0.1577(4) 0.047(2) Uani 1 1 d . . . . .
H120 H 0.3932 0.6452 0.1278 0.057 Uiso 1 1 calc R U . . .
C121 C 0.4555(4) 0.6743(3) -0.0297(4) 0.0334(17) Uani 1 1 d . . . . .
C122 C 0.5060(4) 0.6289(4) 0.0010(4) 0.0399(18) Uani 1 1 d . . . . .
H122 H 0.5283 0.6344 0.0513 0.048 Uiso 1 1 calc R U . . .
C123 C 0.5241(5) 0.5754(4) -0.0416(5) 0.049(2) Uani 1 1 d . . . . .
H123 H 0.5589 0.5441 -0.0204 0.059 Uiso 1 1 calc R U . . .
C124 C 0.4920(5) 0.5671(4) -0.1147(5) 0.048(2) Uani 1 1 d . . . . .
H124 H 0.5043 0.5300 -0.1433 0.057 Uiso 1 1 calc R U . . .
C125 C 0.4425(5) 0.6123(4) -0.1461(5) 0.053(2) Uani 1 1 d . . . . .
H125 H 0.4204 0.6069 -0.1965 0.063 Uiso 1 1 calc R U . . .
C126 C 0.4252(5) 0.6662(4) -0.1029(4) 0.050(2) Uani 1 1 d . . . . .
H126 H 0.3917 0.6982 -0.1248 0.060 Uiso 1 1 calc R U . . .
C201 C 0.1034(4) 0.7900(3) 0.0187(4) 0.0334(16) Uani 1 1 d . . . . .
H20A H 0.1077 0.7652 0.0671 0.040 Uiso 1 1 calc R U . . .
H20B H 0.0513 0.8088 0.0130 0.040 Uiso 1 1 calc R U . . .
C202 C 0.1172(4) 0.7452(3) -0.0493(4) 0.0345(17) Uani 1 1 d . . . . .
H20C H 0.1079 0.7695 -0.0976 0.041 Uiso 1 1 calc R U . . .
H20D H 0.0806 0.7087 -0.0495 0.041 Uiso 1 1 calc R U . . .
C203 C 0.1618(3) 0.8989(3) 0.1095(4) 0.0279(16) Uani 1 1 d . . . . .
C204 C 0.1782(4) 0.9645(3) 0.1104(4) 0.0314(16) Uani 1 1 d . . . . .
H204 H 0.1935 0.9855 0.0655 0.038 Uiso 1 1 calc R U . . .
C205 C 0.1720(4) 0.9996(4) 0.1784(5) 0.044(2) Uani 1 1 d . . . . .
H205 H 0.1832 1.0445 0.1799 0.053 Uiso 1 1 calc R U . . .
C206 C 0.1499(5) 0.9690(5) 0.2422(5) 0.055(2) Uani 1 1 d . . . . .
H206 H 0.1449 0.9931 0.2877 0.067 Uiso 1 1 calc R U . . .
C207 C 0.1346(5) 0.9043(5) 0.2422(5) 0.055(2) Uani 1 1 d . . . . .
H207 H 0.1199 0.8838 0.2875 0.067 Uiso 1 1 calc R U . . .
C208 C 0.1408(4) 0.8683(4) 0.1757(4) 0.0409(19) Uani 1 1 d . . . . .
H208 H 0.1308 0.8232 0.1756 0.049 Uiso 1 1 calc R U . . .
C209 C 0.1312(4) 0.9083(3) -0.0521(4) 0.0258(15) Uani 1 1 d . . . . .
C210 C 0.0557(4) 0.9270(4) -0.0471(4) 0.0411(19) Uani 1 1 d . . . . .
H210 H 0.0284 0.9139 -0.0045 0.049 Uiso 1 1 calc R U . . .
C211 C 0.0195(5) 0.9646(4) -0.1039(5) 0.048(2) Uani 1 1 d . . . . .
H211 H -0.0323 0.9772 -0.0999 0.057 Uiso 1 1 calc R U . . .
C212 C 0.0582(5) 0.9834(4) -0.1652(4) 0.044(2) Uani 1 1 d . . . . .
H212 H 0.0322 1.0072 -0.2051 0.053 Uiso 1 1 calc R U . . .
C213 C 0.1340(4) 0.9686(3) -0.1702(4) 0.0383(18) Uani 1 1 d . . . . .
H213 H 0.1615 0.9844 -0.2115 0.046 Uiso 1 1 calc R U . . .
C214 C 0.1705(4) 0.9298(3) -0.1137(4) 0.0322(16) Uani 1 1 d . . . . .
H214 H 0.2227 0.9181 -0.1176 0.039 Uiso 1 1 calc R U . . .
C215 C 0.2117(5) 0.6457(3) 0.0214(4) 0.0416(19) Uani 1 1 d . . . . .
C216 C 0.2751(5) 0.6058(3) 0.0292(4) 0.046(2) Uani 1 1 d . . . . .
H216 H 0.3189 0.6149 0.0014 0.056 Uiso 1 1 calc R U . . .
C217 C 0.2753(5) 0.5516(4) 0.0781(5) 0.052(2) Uani 1 1 d . . . . .
H217 H 0.3184 0.5236 0.0826 0.062 Uiso 1 1 calc R U . . .
C218 C 0.2125(6) 0.5401(5) 0.1188(5) 0.068(3) Uani 1 1 d . . . . .
H218 H 0.2136 0.5051 0.1538 0.082 Uiso 1 1 calc R U . . .
C219 C 0.1484(7) 0.5772(5) 0.1108(6) 0.075(3) Uani 1 1 d . . . . .
H219 H 0.1044 0.5664 0.1375 0.090 Uiso 1 1 calc R U . . .
C220 C 0.1474(6) 0.6313(4) 0.0632(5) 0.065(3) Uani 1 1 d . . . . .
H220 H 0.1035 0.6583 0.0590 0.078 Uiso 1 1 calc R U . . .
C221 C 0.2232(4) 0.6749(3) -0.1367(4) 0.0285(15) Uani 1 1 d . . . . .
C222 C 0.2050(4) 0.6098(3) -0.1476(4) 0.0369(17) Uani 1 1 d . . . . .
H222 H 0.1851 0.5859 -0.1069 0.044 Uiso 1 1 calc R U . . .
C223 C 0.2153(5) 0.5795(4) -0.2162(4) 0.048(2) Uani 1 1 d . . . . .
H223 H 0.2025 0.5351 -0.2227 0.057 Uiso 1 1 calc R U . . .
C224 C 0.2443(5) 0.6138(4) -0.2754(4) 0.046(2) Uani 1 1 d . . . . .
H224 H 0.2536 0.5924 -0.3219 0.056 Uiso 1 1 calc R U . . .
C225 C 0.2600(5) 0.6792(4) -0.2678(4) 0.045(2) Uani 1 1 d . . . . .
H225 H 0.2778 0.7034 -0.3093 0.054 Uiso 1 1 calc R U . . .
C226 C 0.2492(4) 0.7087(3) -0.1977(4) 0.0388(18) Uani 1 1 d . . . . .
H226 H 0.2602 0.7534 -0.1918 0.047 Uiso 1 1 calc R U . . .
C301 C 0.7467(5) 0.7393(3) 0.9009(4) 0.0410(19) Uani 1 1 d . . . . .
C302 C 0.6673(5) 0.7295(4) 0.8939(5) 0.045(2) Uani 1 1 d . . . . .
H302 H 0.6444 0.7036 0.9310 0.054 Uiso 1 1 calc R U . . .
C303 C 0.6206(5) 0.7557(4) 0.8355(5) 0.055(2) Uani 1 1 d . . . . .
H303 H 0.5673 0.7465 0.8328 0.066 Uiso 1 1 calc R U . . .
C304 C 0.6506(5) 0.7952(4) 0.7810(5) 0.055(2) Uani 1 1 d . . . . .
H304 H 0.6185 0.8139 0.7415 0.066 Uiso 1 1 calc R U . . .
C305 C 0.7301(5) 0.8067(4) 0.7858(5) 0.052(2) Uani 1 1 d . . . . .
H305 H 0.7525 0.8331 0.7488 0.063 Uiso 1 1 calc R U . . .
C306 C 0.7751(5) 0.7795(4) 0.8442(5) 0.046(2) Uani 1 1 d . . . . .
H306 H 0.8285 0.7884 0.8465 0.055 Uiso 1 1 calc R U . . .
C307 C 0.7557(4) 0.6627(3) 1.0243(5) 0.0413(19) Uani 1 1 d . . . . .
C308 C 0.7125(4) 0.6937(4) 1.0785(4) 0.0413(18) Uani 1 1 d . . . . .
H308 H 0.7123 0.7395 1.0802 0.050 Uiso 1 1 calc R U . . .
C309 C 0.6698(4) 0.6595(5) 1.1301(5) 0.051(2) Uani 1 1 d . . . . .
H309 H 0.6414 0.6821 1.1662 0.062 Uiso 1 1 calc R U . . .
C310 C 0.6690(5) 0.5931(5) 1.1284(5) 0.052(2) Uani 1 1 d . . . . .
H310 H 0.6398 0.5698 1.1631 0.063 Uiso 1 1 calc R U . . .
C311 C 0.7096(5) 0.5613(4) 1.0775(5) 0.055(2) Uani 1 1 d . . . . .
H311 H 0.7088 0.5154 1.0762 0.066 Uiso 1 1 calc R U . . .
C312 C 0.7530(4) 0.5953(4) 1.0266(5) 0.044(2) Uani 1 1 d . . . . .
H312 H 0.7819 0.5716 0.9919 0.053 Uiso 1 1 calc R U . . .
C313 C 0.8533(4) 0.7588(3) 1.0202(5) 0.0387(19) Uani 1 1 d . . . . .
C314 C 0.8522(4) 0.8247(3) 1.0099(5) 0.0396(18) Uani 1 1 d . . . . .
H314 H 0.8234 0.8415 0.9668 0.048 Uiso 1 1 calc R U . . .
C315 C 0.8909(4) 0.8683(3) 1.0588(4) 0.0386(18) Uani 1 1 d . . . . .
H315 H 0.8871 0.9134 1.0490 0.046 Uiso 1 1 calc R U . . .
C316 C 0.9341(4) 0.8467(4) 1.1202(5) 0.045(2) Uani 1 1 d . . . . .
H316 H 0.9611 0.8760 1.1536 0.054 Uiso 1 1 calc R U . . .
C317 C 0.9379(5) 0.7801(4) 1.1335(5) 0.050(2) Uani 1 1 d . . . . .
H317 H 0.9681 0.7637 1.1759 0.060 Uiso 1 1 calc R U . . .
C318 C 0.8977(4) 0.7384(4) 1.0847(5) 0.045(2) Uani 1 1 d . . . . .
H318 H 0.9003 0.6934 1.0955 0.054 Uiso 1 1 calc R U . . .
C319 C 0.8628(5) 0.6594(4) 0.9184(5) 0.056(2) Uani 0.77(4) 1 d D U P A 1
C320 C 0.8425(10) 0.6339(7) 0.8457(7) 0.071(4) Uani 0.77(4) 1 d D U P A 1
H320 H 0.7925 0.6424 0.8238 0.086 Uiso 0.77(4) 1 calc R U P A 1
C321 C 0.8925(14) 0.5967(9) 0.8038(9) 0.083(5) Uani 0.77(4) 1 d D U P A 1
H321 H 0.8769 0.5800 0.7548 0.100 Uiso 0.77(4) 1 calc R U P A 1
C322 C 0.9662(11) 0.5850(10) 0.8367(14) 0.100(6) Uani 0.77(4) 1 d D U P A 1
H322 H 1.0035 0.5655 0.8068 0.120 Uiso 0.77(4) 1 calc R U P A 1
C323 C 0.9856(7) 0.6012(11) 0.9111(17) 0.129(9) Uani 0.77(4) 1 d D U P A 1
H323 H 1.0321 0.5867 0.9362 0.154 Uiso 0.77(4) 1 calc R U P A 1
C324 C 0.9335(7) 0.6405(10) 0.9492(13) 0.110(8) Uani 0.77(4) 1 d D U P A 1
H324 H 0.9484 0.6547 0.9994 0.132 Uiso 0.77(4) 1 calc R U P A 1
C325 C 0.8628(5) 0.6594(4) 0.9184(5) 0.056(2) Uani 0.23(4) 1 d D . P A 2
C326 C 0.824(2) 0.624(3) 0.860(2) 0.071(4) Uani 0.23(4) 1 d D . P A 2
H326 H 0.7698 0.6236 0.8578 0.086 Uiso 0.23(4) 1 calc R U P A 2
C327 C 0.860(3) 0.588(3) 0.805(3) 0.083(5) Uani 0.23(4) 1 d D . P A 2
H327 H 0.8317 0.5677 0.7634 0.100 Uiso 0.23(4) 1 calc R U P A 2
C328 C 0.941(3) 0.582(4) 0.812(5) 0.100(6) Uani 0.23(4) 1 d D . P A 2
H328 H 0.9668 0.5498 0.7851 0.120 Uiso 0.23(4) 1 calc R U P A 2
C329 C 0.979(2) 0.625(4) 0.860(5) 0.129(9) Uani 0.23(4) 1 d D . P A 2
H329 H 1.0325 0.6324 0.8548 0.154 Uiso 0.23(4) 1 calc R U P A 2
C330 C 0.9410(9) 0.658(4) 0.916(4) 0.110(8) Uani 0.23(4) 1 d D . P A 2
H330 H 0.9707 0.6809 0.9543 0.132 Uiso 0.23(4) 1 calc R U P A 2
B31 B 0.8045(5) 0.7054(4) 0.9652(5) 0.039(2) Uani 1 1 d . . . . .
O1 O 0.3395(3) 0.8425(2) 0.1198(3) 0.0340(11) Uani 1 1 d . . . . .
O2 O 0.2685(3) 0.7562(2) 0.1169(2) 0.0323(11) Uani 1 1 d . . . . .
P11 P 0.37791(10) 0.88946(9) -0.03589(10) 0.0290(4) Uani 1 1 d . . . . .
P12 P 0.42777(11) 0.74623(9) 0.02492(11) 0.0325(4) Uani 1 1 d . . . . .
P21 P 0.17492(10) 0.85419(8) 0.02073(10) 0.0268(4) Uani 1 1 d . . . . .
P22 P 0.21540(10) 0.71381(8) -0.04374(10) 0.0284(4) Uani 1 1 d . . . . .
Mo1 Mo 0.30021(3) 0.79992(3) 0.00781(3) 0.02546(16) Uani 1 1 d D . . . .
H2 H 0.336(3) 0.788(3) -0.052(3) 0.040(19) Uiso 1 1 d D . . . .
H3 H 0.271(4) 0.813(3) -0.059(3) 0.037(19) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.249(8) . ?
C1 O1 1.276(8) . ?
C1 Mo1 2.575(7) . ?
C1 H1 0.9500 . ?
C101 C102 1.537(10) . ?
C101 P11 1.837(7) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?
C102 P12 1.858(7) . ?
C102 H10C 0.9900 . ?
C102 H10D 0.9900 . ?
C103 C108 1.371(10) . ?
C103 C104 1.391(10) . ?
C103 P11 1.848(7) . ?
C104 C105 1.390(10) . ?
C104 H104 0.9500 . ?
C105 C106 1.384(11) . ?
C105 H105 0.9500 . ?
C106 C107 1.366(11) . ?
C106 H106 0.9500 . ?
C107 C108 1.385(10) . ?
C107 H107 0.9500 . ?
C108 H108 0.9500 . ?
C109 C110 1.380(10) . ?
C109 C114 1.397(10) . ?
C109 P11 1.833(7) . ?
C110 C111 1.386(12) . ?
C110 H110 0.9500 . ?
C111 C112 1.384(12) . ?
C111 H111 0.9500 . ?
C112 C113 1.366(11) . ?
C112 H112 0.9500 . ?
C113 C114 1.377(10) . ?
C113 H113 0.9500 . ?
C114 H114 0.9500 . ?
C115 C120 1.391(10) . ?
C115 C116 1.393(10) . ?
C115 P12 1.820(7) . ?
C116 C117 1.393(11) . ?
C116 H116 0.9500 . ?
C117 C118 1.370(12) . ?
C117 H117 0.9500 . ?
C118 C119 1.362(11) . ?
C118 H118 0.9500 . ?
C119 C120 1.391(10) . ?
C119 H119 0.9500 . ?
C120 H120 0.9500 . ?
C121 C126 1.371(10) . ?
C121 C122 1.377(10) . ?
C121 P12 1.850(7) . ?
C122 C123 1.384(10) . ?
C122 H122 0.9500 . ?
C123 C124 1.379(11) . ?
C123 H123 0.9500 . ?
C124 C125 1.367(11) . ?
C124 H124 0.9500 . ?
C125 C126 1.392(11) . ?
C125 H125 0.9500 . ?
C126 H126 0.9500 . ?
C201 C202 1.541(9) . ?
C201 P21 1.823(7) . ?
C201 H20A 0.9900 . ?
C201 H20B 0.9900 . ?
C202 P22 1.833(7) . ?
C202 H20C 0.9900 . ?
C202 H20D 0.9900 . ?
C203 C204 1.388(9) . ?
C203 C208 1.391(9) . ?
C203 P21 1.838(6) . ?
C204 C205 1.406(10) . ?
C204 H204 0.9500 . ?
C205 C206 1.360(11) . ?
C205 H205 0.9500 . ?
C206 C207 1.365(12) . ?
C206 H206 0.9500 . ?
C207 C208 1.392(11) . ?
C207 H207 0.9500 . ?
C208 H208 0.9500 . ?
C209 C210 1.382(9) . ?
C209 C214 1.387(9) . ?
C209 P21 1.832(7) . ?
C210 C211 1.387(10) . ?
C210 H210 0.9500 . ?
C211 C212 1.360(11) . ?
C211 H211 0.9500 . ?
C212 C213 1.367(10) . ?
C212 H212 0.9500 . ?
C213 C214 1.399(10) . ?
C213 H213 0.9500 . ?
C214 H214 0.9500 . ?
C215 C216 1.383(11) . ?
C215 C220 1.409(11) . ?
C215 P22 1.818(7) . ?
C216 C217 1.412(11) . ?
C216 H216 0.9500 . ?
C217 C218 1.366(12) . ?
C217 H217 0.9500 . ?
C218 C219 1.359(13) . ?
C218 H218 0.9500 . ?
C219 C220 1.396(12) . ?
C219 H219 0.9500 . ?
C220 H220 0.9500 . ?
C221 C226 1.377(9) . ?
C221 C222 1.396(9) . ?
C221 P22 1.831(7) . ?
C222 C223 1.378(10) . ?
C222 H222 0.9500 . ?
C223 C224 1.379(11) . ?
C223 H223 0.9500 . ?
C224 C225 1.387(11) . ?
C224 H224 0.9500 . ?
C225 C226 1.395(10) . ?
C225 H225 0.9500 . ?
C226 H226 0.9500 . ?
C301 C302 1.403(11) . ?
C301 C306 1.408(10) . ?
C301 B31 1.628(12) . ?
C302 C303 1.382(11) . ?
C302 H302 0.9500 . ?
C303 C304 1.384(11) . ?
C303 H303 0.9500 . ?
C304 C305 1.407(12) . ?
C304 H304 0.9500 . ?
C305 C306 1.376(11) . ?
C305 H305 0.9500 . ?
C306 H306 0.9500 . ?
C307 C312 1.397(10) . ?
C307 C308 1.403(10) . ?
C307 B31 1.639(11) . ?
C308 C309 1.398(11) . ?
C308 H308 0.9500 . ?
C309 C310 1.375(12) . ?
C309 H309 0.9500 . ?
C310 C311 1.345(12) . ?
C310 H310 0.9500 . ?
C311 C312 1.395(11) . ?
C311 H311 0.9500 . ?
C312 H312 0.9500 . ?
C313 C314 1.376(10) . ?
C313 C318 1.400(11) . ?
C313 B31 1.668(11) . ?
C314 C315 1.393(10) . ?
C314 H314 0.9500 . ?
C315 C316 1.355(11) . ?
C315 H315 0.9500 . ?
C316 C317 1.399(11) . ?
C316 H316 0.9500 . ?
C317 C318 1.379(11) . ?
C317 H317 0.9500 . ?
C318 H318 0.9500 . ?
C319 C324 1.377(12) . ?
C319 C320 1.405(11) . ?
C319 B31 1.649(11) . ?
C320 C321 1.406(11) . ?
C320 H320 0.9500 . ?
C321 C322 1.402(13) . ?
C321 H321 0.9500 . ?
C322 C323 1.371(14) . ?
C322 H322 0.9500 . ?
C323 C324 1.415(12) . ?
C323 H323 0.9500 . ?
C324 H324 0.9500 . ?
C325 C330 1.370(14) . ?
C325 C326 1.405(14) . ?
C325 B31 1.649(11) . ?
C326 C327 1.403(14) . ?
C326 H326 0.9500 . ?
C327 C328 1.402(15) . ?
C327 H327 0.9500 . ?
C328 C329 1.377(16) . ?
C328 H328 0.9500 . ?
C329 C330 1.403(15) . ?
C329 H329 0.9500 . ?
C330 H330 0.9500 . ?
O1 Mo1 2.225(5) . ?
O2 Mo1 2.217(4) . ?
P11 Mo1 2.4475(19) . ?
P12 Mo1 2.4940(19) . ?
P21 Mo1 2.4839(18) . ?
P22 Mo1 2.4571(18) . ?
Mo1 H2 1.27(4) . ?
Mo1 H3 1.27(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
O2 C1 O1 119.1(6) . . ?
O2 C1 Mo1 59.4(4) . . ?
O1 C1 Mo1 59.8(3) . . ?
O2 C1 H1 120.4 . . ?
O1 C1 H1 120.4 . . ?
Mo1 C1 H1 178.6 . . ?
C102 C101 P11 109.7(5) . . ?
C102 C101 H10A 109.7 . . ?
P11 C101 H10A 109.7 . . ?
C102 C101 H10B 109.7 . . ?
P11 C101 H10B 109.7 . . ?
H10A C101 H10B 108.2 . . ?
C101 C102 P12 110.8(5) . . ?
C101 C102 H10C 109.5 . . ?
P12 C102 H10C 109.5 . . ?
C101 C102 H10D 109.5 . . ?
P12 C102 H10D 109.5 . . ?
H10C C102 H10D 108.1 . . ?
C108 C103 C104 119.5(7) . . ?
C108 C103 P11 119.0(6) . . ?
C104 C103 P11 121.5(6) . . ?
C105 C104 C103 119.5(7) . . ?
C105 C104 H104 120.2 . . ?
C103 C104 H104 120.2 . . ?
C106 C105 C104 120.4(8) . . ?
C106 C105 H105 119.8 . . ?
C104 C105 H105 119.8 . . ?
C107 C106 C105 119.5(7) . . ?
C107 C106 H106 120.3 . . ?
C105 C106 H106 120.3 . . ?
C106 C107 C108 120.6(8) . . ?
C106 C107 H107 119.7 . . ?
C108 C107 H107 119.7 . . ?
C103 C108 C107 120.5(7) . . ?
C103 C108 H108 119.7 . . ?
C107 C108 H108 119.7 . . ?
C110 C109 C114 117.7(7) . . ?
C110 C109 P11 119.4(6) . . ?
C114 C109 P11 122.8(5) . . ?
C109 C110 C111 120.2(8) . . ?
C109 C110 H110 119.9 . . ?
C111 C110 H110 119.9 . . ?
C112 C111 C110 120.9(8) . . ?
C112 C111 H111 119.5 . . ?
C110 C111 H111 119.5 . . ?
C113 C112 C111 119.5(8) . . ?
C113 C112 H112 120.3 . . ?
C111 C112 H112 120.3 . . ?
C112 C113 C114 119.7(7) . . ?
C112 C113 H113 120.2 . . ?
C114 C113 H113 120.2 . . ?
C113 C114 C109 121.8(7) . . ?
C113 C114 H114 119.1 . . ?
C109 C114 H114 119.1 . . ?
C120 C115 C116 117.3(7) . . ?
C120 C115 P12 119.5(6) . . ?
C116 C115 P12 122.9(6) . . ?
C117 C116 C115 120.4(8) . . ?
C117 C116 H116 119.8 . . ?
C115 C116 H116 119.8 . . ?
C118 C117 C116 120.5(8) . . ?
C118 C117 H117 119.8 . . ?
C116 C117 H117 119.8 . . ?
C119 C118 C117 120.5(8) . . ?
C119 C118 H118 119.8 . . ?
C117 C118 H118 119.8 . . ?
C118 C119 C120 119.3(8) . . ?
C118 C119 H119 120.4 . . ?
C120 C119 H119 120.4 . . ?
C115 C120 C119 122.0(8) . . ?
C115 C120 H120 119.0 . . ?
C119 C120 H120 119.0 . . ?
C126 C121 C122 119.0(7) . . ?
C126 C121 P12 119.0(5) . . ?
C122 C121 P12 121.9(5) . . ?
C121 C122 C123 119.9(7) . . ?
C121 C122 H122 120.1 . . ?
C123 C122 H122 120.1 . . ?
C124 C123 C122 120.5(8) . . ?
C124 C123 H123 119.8 . . ?
C122 C123 H123 119.8 . . ?
C125 C124 C123 120.2(8) . . ?
C125 C124 H124 119.9 . . ?
C123 C124 H124 119.9 . . ?
C124 C125 C126 118.7(8) . . ?
C124 C125 H125 120.6 . . ?
C126 C125 H125 120.6 . . ?
C121 C126 C125 121.6(7) . . ?
C121 C126 H126 119.2 . . ?
C125 C126 H126 119.2 . . ?
C202 C201 P21 108.4(4) . . ?
C202 C201 H20A 110.0 . . ?
P21 C201 H20A 110.0 . . ?
C202 C201 H20B 110.0 . . ?
P21 C201 H20B 110.0 . . ?
H20A C201 H20B 108.4 . . ?
C201 C202 P22 111.2(5) . . ?
C201 C202 H20C 109.4 . . ?
P22 C202 H20C 109.4 . . ?
C201 C202 H20D 109.4 . . ?
P22 C202 H20D 109.4 . . ?
H20C C202 H20D 108.0 . . ?
C204 C203 C208 120.1(6) . . ?
C204 C203 P21 117.8(5) . . ?
C208 C203 P21 122.0(6) . . ?
C203 C204 C205 119.2(7) . . ?
C203 C204 H204 120.4 . . ?
C205 C204 H204 120.4 . . ?
C206 C205 C204 119.8(8) . . ?
C206 C205 H205 120.1 . . ?
C204 C205 H205 120.1 . . ?
C205 C206 C207 121.5(8) . . ?
C205 C206 H206 119.3 . . ?
C207 C206 H206 119.3 . . ?
C206 C207 C208 120.0(8) . . ?
C206 C207 H207 120.0 . . ?
C208 C207 H207 120.0 . . ?
C203 C208 C207 119.4(8) . . ?
C203 C208 H208 120.3 . . ?
C207 C208 H208 120.3 . . ?
C210 C209 C214 118.5(6) . . ?
C210 C209 P21 119.2(5) . . ?
C214 C209 P21 122.3(5) . . ?
C209 C210 C211 120.6(7) . . ?
C209 C210 H210 119.7 . . ?
C211 C210 H210 119.7 . . ?
C212 C211 C210 120.0(7) . . ?
C212 C211 H211 120.0 . . ?
C210 C211 H211 120.0 . . ?
C211 C212 C213 121.0(7) . . ?
C211 C212 H212 119.5 . . ?
C213 C212 H212 119.5 . . ?
C212 C213 C214 119.1(7) . . ?
C212 C213 H213 120.5 . . ?
C214 C213 H213 120.5 . . ?
C209 C214 C213 120.7(7) . . ?
C209 C214 H214 119.7 . . ?
C213 C214 H214 119.7 . . ?
C216 C215 C220 118.8(7) . . ?
C216 C215 P22 117.9(6) . . ?
C220 C215 P22 123.4(6) . . ?
C215 C216 C217 120.5(8) . . ?
C215 C216 H216 119.7 . . ?
C217 C216 H216 119.7 . . ?
C218 C217 C216 118.9(8) . . ?
C218 C217 H217 120.6 . . ?
C216 C217 H217 120.6 . . ?
C219 C218 C217 122.0(8) . . ?
C219 C218 H218 119.0 . . ?
C217 C218 H218 119.0 . . ?
C218 C219 C220 119.8(9) . . ?
C218 C219 H219 120.1 . . ?
C220 C219 H219 120.1 . . ?
C219 C220 C215 119.9(9) . . ?
C219 C220 H220 120.1 . . ?
C215 C220 H220 120.1 . . ?
C226 C221 C222 117.9(6) . . ?
C226 C221 P22 120.8(5) . . ?
C222 C221 P22 121.2(5) . . ?
C223 C222 C221 121.2(7) . . ?
C223 C222 H222 119.4 . . ?
C221 C222 H222 119.4 . . ?
C222 C223 C224 119.7(7) . . ?
C222 C223 H223 120.2 . . ?
C224 C223 H223 120.2 . . ?
C223 C224 C225 120.7(7) . . ?
C223 C224 H224 119.6 . . ?
C225 C224 H224 119.6 . . ?
C224 C225 C226 118.4(7) . . ?
C224 C225 H225 120.8 . . ?
C226 C225 H225 120.8 . . ?
C221 C226 C225 122.0(7) . . ?
C221 C226 H226 119.0 . . ?
C225 C226 H226 119.0 . . ?
C302 C301 C306 114.2(8) . . ?
C302 C301 B31 124.7(7) . . ?
C306 C301 B31 121.0(7) . . ?
C303 C302 C301 123.2(8) . . ?
C303 C302 H302 118.4 . . ?
C301 C302 H302 118.4 . . ?
C302 C303 C304 120.8(8) . . ?
C302 C303 H303 119.6 . . ?
C304 C303 H303 119.6 . . ?
C303 C304 C305 118.2(8) . . ?
C303 C304 H304 120.9 . . ?
C305 C304 H304 120.9 . . ?
C306 C305 C304 119.6(8) . . ?
C306 C305 H305 120.2 . . ?
C304 C305 H305 120.2 . . ?
C305 C306 C301 123.9(8) . . ?
C305 C306 H306 118.0 . . ?
C301 C306 H306 118.0 . . ?
C312 C307 C308 114.7(7) . . ?
C312 C307 B31 125.2(7) . . ?
C308 C307 B31 120.1(6) . . ?
C309 C308 C307 122.4(8) . . ?
C309 C308 H308 118.8 . . ?
C307 C308 H308 118.8 . . ?
C310 C309 C308 119.7(8) . . ?
C310 C309 H309 120.1 . . ?
C308 C309 H309 120.1 . . ?
C311 C310 C309 120.0(8) . . ?
C311 C310 H310 120.0 . . ?
C309 C310 H310 120.0 . . ?
C310 C311 C312 120.3(8) . . ?
C310 C311 H311 119.9 . . ?
C312 C311 H311 119.9 . . ?
C311 C312 C307 122.9(8) . . ?
C311 C312 H312 118.6 . . ?
C307 C312 H312 118.6 . . ?
C314 C313 C318 114.0(7) . . ?
C314 C313 B31 125.4(7) . . ?
C318 C313 B31 120.5(6) . . ?
C313 C314 C315 124.0(8) . . ?
C313 C314 H314 118.0 . . ?
C315 C314 H314 118.0 . . ?
C316 C315 C314 120.2(7) . . ?
C316 C315 H315 119.9 . . ?
C314 C315 H315 119.9 . . ?
C315 C316 C317 118.5(8) . . ?
C315 C316 H316 120.8 . . ?
C317 C316 H316 120.8 . . ?
C318 C317 C316 119.8(8) . . ?
C318 C317 H317 120.1 . . ?
C316 C317 H317 120.1 . . ?
C317 C318 C313 123.4(7) . . ?
C317 C318 H318 118.3 . . ?
C313 C318 H318 118.3 . . ?
C324 C319 C320 115.0(10) . . ?
C324 C319 B31 122.4(9) . . ?
C320 C319 B31 122.5(9) . . ?
C319 C320 C321 123.3(13) . . ?
C319 C320 H320 118.4 . . ?
C321 C320 H320 118.4 . . ?
C322 C321 C320 117.6(12) . . ?
C322 C321 H321 121.2 . . ?
C320 C321 H321 121.2 . . ?
C323 C322 C321 121.3(12) . . ?
C323 C322 H322 119.3 . . ?
C321 C322 H322 119.3 . . ?
C322 C323 C324 117.3(14) . . ?
C322 C323 H323 121.3 . . ?
C324 C323 H323 121.3 . . ?
C319 C324 C323 124.5(13) . . ?
C319 C324 H324 117.8 . . ?
C323 C324 H324 117.8 . . ?
C330 C325 C326 114(2) . . ?
C330 C325 B31 132.3(18) . . ?
C326 C325 B31 112.6(18) . . ?
C327 C326 C325 125(2) . . ?
C327 C326 H326 117.7 . . ?
C325 C326 H326 117.7 . . ?
C328 C327 C326 118(2) . . ?
C328 C327 H327 121.0 . . ?
C326 C327 H327 121.0 . . ?
C329 C328 C327 117(3) . . ?
C329 C328 H328 121.4 . . ?
C327 C328 H328 121.4 . . ?
C328 C329 C330 120(3) . . ?
C328 C329 H329 119.9 . . ?
C330 C329 H329 119.9 . . ?
C325 C330 C329 123(2) . . ?
C325 C330 H330 118.3 . . ?
C329 C330 H330 118.3 . . ?
C301 B31 C307 110.2(6) . . ?
C301 B31 C325 106.3(7) . . ?
C307 B31 C325 111.3(6) . . ?
C301 B31 C319 106.3(7) . . ?
C307 B31 C319 111.3(6) . . ?
C301 B31 C313 112.9(6) . . ?
C307 B31 C313 105.1(6) . . ?
C325 B31 C313 111.2(6) . . ?
C319 B31 C313 111.2(6) . . ?
C1 O1 Mo1 90.5(4) . . ?
C1 O2 Mo1 91.6(4) . . ?
C109 P11 C101 104.4(3) . . ?
C109 P11 C103 103.9(3) . . ?
C101 P11 C103 100.6(3) . . ?
C109 P11 Mo1 121.6(2) . . ?
C101 P11 Mo1 104.0(2) . . ?
C103 P11 Mo1 119.3(2) . . ?
C115 P12 C121 104.1(3) . . ?
C115 P12 C102 105.0(3) . . ?
C121 P12 C102 100.9(3) . . ?
C115 P12 Mo1 114.6(2) . . ?
C121 P12 Mo1 123.8(2) . . ?
C102 P12 Mo1 106.3(2) . . ?
C201 P21 C209 100.0(3) . . ?
C201 P21 C203 105.3(3) . . ?
C209 P21 C203 102.4(3) . . ?
C201 P21 Mo1 106.0(2) . . ?
C209 P21 Mo1 123.2(2) . . ?
C203 P21 Mo1 117.4(2) . . ?
C215 P22 C221 103.0(3) . . ?
C215 P22 C202 103.9(4) . . ?
C221 P22 C202 103.1(3) . . ?
C215 P22 Mo1 112.0(3) . . ?
C221 P22 Mo1 124.9(2) . . ?
C202 P22 Mo1 107.8(2) . . ?
O2 Mo1 O1 58.70(17) . . ?
O2 Mo1 P11 138.70(13) . . ?
O1 Mo1 P11 80.05(13) . . ?
O2 Mo1 P22 81.07(13) . . ?
O1 Mo1 P22 139.58(13) . . ?
P11 Mo1 P22 140.21(6) . . ?
O2 Mo1 P21 80.77(12) . . ?
O1 Mo1 P21 88.22(12) . . ?
P11 Mo1 P21 101.21(6) . . ?
P22 Mo1 P21 81.10(6) . . ?
O2 Mo1 P12 88.92(13) . . ?
O1 Mo1 P12 80.93(13) . . ?
P11 Mo1 P12 82.34(6) . . ?
P22 Mo1 P12 103.71(6) . . ?
P21 Mo1 P12 167.87(7) . . ?
O2 Mo1 C1 29.0(2) . . ?
O1 Mo1 C1 29.7(2) . . ?
P11 Mo1 C1 109.71(18) . . ?
P22 Mo1 C1 110.03(18) . . ?
P21 Mo1 C1 84.09(15) . . ?
P12 Mo1 C1 83.80(15) . . ?
O2 Mo1 H2 142(3) . . ?
O1 Mo1 H2 131(3) . . ?
P11 Mo1 H2 65(3) . . ?
P22 Mo1 H2 83(3) . . ?
P21 Mo1 H2 130(3) . . ?
P12 Mo1 H2 62(3) . . ?
C1 Mo1 H2 146(3) . . ?
O2 Mo1 H3 140(3) . . ?
O1 Mo1 H3 144(3) . . ?
P11 Mo1 H3 76(3) . . ?
P22 Mo1 H3 67(3) . . ?
P21 Mo1 H3 71(3) . . ?
P12 Mo1 H3 121(3) . . ?
C1 Mo1 H3 155(3) . . ?
H2 Mo1 H3 59(4) . . ?

_refine_diff_density_max         1.000
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.115

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_W
_database_code_depnum_ccdc_archive 'CCDC 1407345'
_audit_update_record             
;
2015-12-13 deposited with the CCDC.
2015-12-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     '[W(O2CH)(dppe)2(H)2][BPh4]'
_chemical_formula_moiety         'C53 H51 O2 P4 W, C24 H20 B'
_chemical_formula_sum            'C77 H71 B O2 P4 W'
_chemical_formula_weight         1346.87

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'
B B 0.0013 0.0007 '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'
W W -0.8490 6.8722 '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                   17.4968(6)
_cell_length_b                   20.7324(8)
_cell_length_c                   17.5670(7)
_cell_angle_alpha                90
_cell_angle_beta                 93.337(2)
_cell_angle_gamma                90
_cell_volume                     6361.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    105058
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       needle
_exptl_crystal_colour            'dark pink'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_F_000             2752
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.964
_shelx_estimated_absorpt_T_min   0.719
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6581
_exptl_absorpt_correction_T_max  0.9618
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick,2007)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_reflns_number            44369
_diffrn_reflns_av_unetI/netI     0.1237
_diffrn_reflns_av_R_equivalents  0.1130
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.168
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             11159
_reflns_number_gt                6935
_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       'COLLECT (Hooft, 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1993)'
_computing_publication_material  
;
SHELXL-2014/7 (Sheldrick, 2015), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen et al., 2004)
;
_refine_special_details          
;
The two W---H distances were restrained to 1.26(2)Å whilst the H...H
vector was restrained to 1.24Å.

One ring of the dppe ligand was disordered over two positions. Refinement
was carried out with the geometry and thermal parameters of the two positions
restrained to the same values.

One ring of the BPh₄⁻ anion was disordered over two positions. Refinement
was carried out with the geometry and thermal parameters of the two positions
constrained to the same values. The carbon atoms in this disordered part were
restrained to approximately isotropic values.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+136.3989P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11159
_refine_ls_number_parameters     792
_refine_ls_number_restraints     147
_refine_ls_R_factor_all          0.1746
_refine_ls_R_factor_gt           0.0979
_refine_ls_wR_factor_ref         0.1992
_refine_ls_wR_factor_gt          0.1743
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.007
_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
H1 H 0.224(5) 0.324(4) 0.558(3) 0.030 Uiso 1 1 d D U . . .
H2 H 0.162(4) 0.295(5) 0.553(3) 0.030 Uiso 1 1 d D U . . .
C1 C 0.3981(8) 0.2900(7) 0.4813(7) 0.042(3) Uani 1 1 d . . . . .
H1A H 0.3942 0.2658 0.4327 0.050 Uiso 1 1 calc R U . . .
H1B H 0.4500 0.3090 0.4880 0.050 Uiso 1 1 calc R U . . .
C2 C 0.3828(7) 0.2442(6) 0.5496(8) 0.039(3) Uani 1 1 d . . . . .
H2A H 0.3925 0.2679 0.5981 0.046 Uiso 1 1 calc R U . . .
H2B H 0.4187 0.2073 0.5495 0.046 Uiso 1 1 calc R U . . .
C3 C 0.2770(7) 0.1752(6) 0.6358(7) 0.035(3) Uani 1 1 d D . . . .
C4 C 0.2522(8) 0.2096(6) 0.6984(7) 0.049(4) Uani 1 1 d D . . . .
H4 H 0.2429 0.2545 0.6936 0.058 Uiso 1 1 calc R U . . .
C5 C 0.2413(9) 0.1798(7) 0.7662(7) 0.059(4) Uani 1 1 d D . . . .
H5 H 0.2227 0.2038 0.8072 0.071 Uiso 1 1 calc R U . . .
C6 C 0.2571(10) 0.1148(7) 0.7754(8) 0.063(5) Uani 1 1 d D . . . .
H6 H 0.2494 0.0941 0.8226 0.076 Uiso 1 1 calc R U . . .
C7 C 0.2837(11) 0.0806(8) 0.7161(9) 0.076(5) Uani 1 1 d D . . . .
H7 H 0.2959 0.0362 0.7228 0.091 Uiso 1 1 calc R U . . .
C8 C 0.2932(8) 0.1092(6) 0.6467(7) 0.049(4) Uani 1 1 d D . . . .
H8 H 0.3109 0.0843 0.6059 0.059 Uiso 1 1 calc R U . . .
C9 C 0.2868(9) 0.1455(7) 0.4784(8) 0.050(4) Uani 1 1 d . . . . .
C10 C 0.2228(11) 0.1058(8) 0.4703(10) 0.074(6) Uani 1 1 d . . . . .
H10 H 0.1790 0.1143 0.4982 0.088 Uiso 1 1 calc R U . . .
C11 C 0.2238(13) 0.0530(9) 0.4204(12) 0.085(6) Uani 1 1 d . . . . .
H11 H 0.1806 0.0252 0.4154 0.102 Uiso 1 1 calc R U . . .
C12 C 0.2847(15) 0.0412(10) 0.3796(10) 0.088(7) Uani 1 1 d . . . . .
H12 H 0.2828 0.0067 0.3440 0.106 Uiso 1 1 calc R U . . .
C13 C 0.3498(16) 0.0781(10) 0.3885(14) 0.113(9) Uani 1 1 d . . . . .
H13 H 0.3942 0.0666 0.3631 0.136 Uiso 1 1 calc R U . . .
C14 C 0.3501(14) 0.1326(8) 0.4349(11) 0.090(7) Uani 1 1 d . . . . .
H14 H 0.3929 0.1610 0.4372 0.108 Uiso 1 1 calc R U . . .
C15 C 0.3691(6) 0.4074(6) 0.5540(8) 0.034(3) Uani 1 1 d . . . . .
C16 C 0.3314(8) 0.4297(6) 0.6145(9) 0.044(4) Uani 1 1 d . . . . .
H16 H 0.2792 0.4183 0.6185 0.052 Uiso 1 1 calc R U . . .
C17 C 0.3666(8) 0.4681(7) 0.6700(9) 0.053(4) Uani 1 1 d . . . . .
H17 H 0.3384 0.4827 0.7114 0.064 Uiso 1 1 calc R U . . .
C18 C 0.4406(9) 0.4854(7) 0.6664(9) 0.057(4) Uani 1 1 d . . . . .
H18 H 0.4656 0.5106 0.7057 0.068 Uiso 1 1 calc R U . . .
C19 C 0.4788(9) 0.4657(8) 0.6046(10) 0.063(5) Uani 1 1 d . . . . .
H19 H 0.5304 0.4789 0.6003 0.076 Uiso 1 1 calc R U . . .
C20 C 0.4441(8) 0.4271(8) 0.5483(9) 0.057(4) Uani 1 1 d . . . . .
H20 H 0.4717 0.4143 0.5059 0.068 Uiso 1 1 calc R U . . .
C21 C 0.3391(7) 0.3981(7) 0.3934(8) 0.041(3) Uani 1 1 d . . . . .
C22 C 0.3210(7) 0.4635(7) 0.3922(8) 0.047(4) Uani 1 1 d . . . . .
H22 H 0.3047 0.4839 0.4368 0.056 Uiso 1 1 calc R U . . .
C23 C 0.3271(8) 0.5000(8) 0.3235(9) 0.054(4) Uani 1 1 d . . . . .
H23 H 0.3151 0.5447 0.3216 0.064 Uiso 1 1 calc R U . . .
C24 C 0.3508(10) 0.4679(10) 0.2606(10) 0.074(6) Uani 1 1 d . . . . .
H24 H 0.3562 0.4916 0.2149 0.088 Uiso 1 1 calc R U . . .
C25 C 0.3669(10) 0.4044(10) 0.2608(11) 0.080(6) Uani 1 1 d . . . . .
H25 H 0.3828 0.3842 0.2158 0.096 Uiso 1 1 calc R U . . .
C26 C 0.3603(8) 0.3688(8) 0.3260(8) 0.056(4) Uani 1 1 d . . . . .
H26 H 0.3702 0.3238 0.3253 0.067 Uiso 1 1 calc R U . . .
C27 C 0.0275(7) 0.3767(7) 0.4921(9) 0.049(4) Uani 1 1 d . . . . .
H27A H -0.0088 0.4078 0.5127 0.059 Uiso 1 1 calc R U . . .
H27B H 0.0279 0.3834 0.4363 0.059 Uiso 1 1 calc R U . . .
C28 C 0.0017(6) 0.3077(7) 0.5085(9) 0.051(4) Uani 1 1 d . . . . .
H28A H -0.0487 0.2996 0.4817 0.061 Uiso 1 1 calc R U . . .
H28B H -0.0040 0.3026 0.5639 0.061 Uiso 1 1 calc R U . . .
C29 C 0.0453(5) 0.1770(4) 0.5329(5) 0.045(4) Uani 1 1 d G . . . .
C30 C 0.0767(5) 0.1691(5) 0.6068(5) 0.071(5) Uani 1 1 d G . . . .
H30 H 0.1102 0.2009 0.6289 0.086 Uiso 1 1 calc R U . . .
C31 C 0.0592(6) 0.1145(5) 0.6484(4) 0.069(5) Uani 1 1 d G . . . .
H31 H 0.0806 0.1091 0.6989 0.082 Uiso 1 1 calc R U . . .
C32 C 0.0102(6) 0.0680(4) 0.6161(6) 0.054(4) Uani 1 1 d G . . . .
H32 H -0.0018 0.0307 0.6445 0.065 Uiso 1 1 calc R U . . .
C33 C -0.0213(6) 0.0760(4) 0.5422(6) 0.066(5) Uani 1 1 d G . . . .
H33 H -0.0547 0.0441 0.5200 0.079 Uiso 1 1 calc R U . . .
C34 C -0.0037(6) 0.1305(5) 0.5006(5) 0.062(5) Uani 1 1 d G . . . .
H34 H -0.0252 0.1360 0.4501 0.074 Uiso 1 1 calc R U . . .
C35 C 0.0427(8) 0.2288(8) 0.3766(9) 0.053(4) Uani 1 1 d . . . . .
C36 C 0.0752(9) 0.1743(10) 0.3440(9) 0.070(5) Uani 1 1 d . . . . .
H36 H 0.1092 0.1475 0.3740 0.084 Uiso 1 1 calc R U . . .
C37 C 0.0579(9) 0.1595(8) 0.2688(8) 0.059(4) Uani 1 1 d . . . . .
H37 H 0.0796 0.1224 0.2470 0.071 Uiso 1 1 calc R U . . .
C38 C 0.0096(10) 0.1980(11) 0.2252(9) 0.077(5) Uani 1 1 d . . . . .
H38 H -0.0038 0.1865 0.1738 0.093 Uiso 1 1 calc R U . . .
C39 C -0.0202(11) 0.2539(10) 0.2555(11) 0.080(6) Uani 1 1 d . . . . .
H39 H -0.0501 0.2824 0.2236 0.096 Uiso 1 1 calc R U . . .
C40 C -0.0063(10) 0.2683(10) 0.3332(10) 0.080(6) Uani 1 1 d . . . . .
H40 H -0.0299 0.3044 0.3554 0.096 Uiso 1 1 calc R U . . .
C41 C 0.1417(7) 0.4742(6) 0.5005(8) 0.039(3) Uani 1 1 d . . . . .
C42 C 0.1343(8) 0.4854(7) 0.4250(8) 0.048(4) Uani 1 1 d . . . . .
H42 H 0.1179 0.4514 0.3916 0.057 Uiso 1 1 calc R U . . .
C43 C 0.1501(8) 0.5449(8) 0.3949(10) 0.058(4) Uani 1 1 d . . . . .
H43 H 0.1456 0.5515 0.3413 0.069 Uiso 1 1 calc R U . . .
C44 C 0.1722(8) 0.5943(8) 0.4426(10) 0.056(4) Uani 1 1 d . . . . .
H44 H 0.1829 0.6358 0.4230 0.067 Uiso 1 1 calc R U . . .
C45 C 0.1787(9) 0.5823(8) 0.5217(11) 0.066(5) Uani 1 1 d . . . . .
H45 H 0.1935 0.6161 0.5560 0.079 Uiso 1 1 calc R U . . .
C46 C 0.1634(9) 0.5208(8) 0.5501(10) 0.063(5) Uani 1 1 d . . . . .
H46 H 0.1682 0.5122 0.6033 0.076 Uiso 1 1 calc R U . . .
C47A C 0.1055(8) 0.4016(7) 0.6365(9) 0.060(4) Uani 0.16(4) 1 d D . P A 1
C48A C 0.130(5) 0.356(3) 0.691(3) 0.037(5) Uani 0.16(4) 1 d D . P A 1
H48A H 0.1466 0.3144 0.6753 0.044 Uiso 0.16(4) 1 calc R U P A 1
C49A C 0.131(8) 0.369(5) 0.768(2) 0.052(6) Uani 0.16(4) 1 d D . P A 1
H49A H 0.1623 0.3449 0.8032 0.062 Uiso 0.16(4) 1 calc R U P A 1
C50A C 0.084(14) 0.418(9) 0.792(3) 0.075(8) Uani 0.16(4) 1 d D . P A 1
H50A H 0.0727 0.4219 0.8438 0.090 Uiso 0.16(4) 1 calc R U P A 1
C51A C 0.055(9) 0.462(7) 0.739(4) 0.123(15) Uani 0.16(4) 1 d D . P A 1
H51A H 0.0236 0.4956 0.7551 0.148 Uiso 0.16(4) 1 calc R U P A 1
C52A C 0.071(7) 0.458(3) 0.663(4) 0.067(7) Uani 0.16(4) 1 d D . P A 1
H52A H 0.0589 0.4930 0.6294 0.081 Uiso 0.16(4) 1 calc R U P A 1
C47B C 0.1055(8) 0.4016(7) 0.6365(9) 0.060(4) Uani 0.84(4) 1 d D . P A 2
C48B C 0.1539(9) 0.3772(10) 0.6972(8) 0.037(5) Uani 0.84(4) 1 d D . P A 2
H48B H 0.1966 0.3514 0.6857 0.044 Uiso 0.84(4) 1 calc R U P A 2
C49B C 0.1410(13) 0.3895(10) 0.7714(9) 0.052(6) Uani 0.84(4) 1 d D . P A 2
H49B H 0.1789 0.3795 0.8106 0.062 Uiso 0.84(4) 1 calc R U P A 2
C50B C 0.072(2) 0.417(2) 0.7894(10) 0.075(8) Uani 0.84(4) 1 d D . P A 2
H50B H 0.0583 0.4203 0.8409 0.090 Uiso 0.84(4) 1 calc R U P A 2
C51B C 0.0233(16) 0.4388(19) 0.7312(12) 0.123(15) Uani 0.84(4) 1 d D . P A 2
H51B H -0.0226 0.4597 0.7439 0.148 Uiso 0.84(4) 1 calc R U P A 2
C52B C 0.0371(12) 0.4323(13) 0.6553(11) 0.067(7) Uani 0.84(4) 1 d D . P A 2
H52B H 0.0017 0.4481 0.6166 0.081 Uiso 0.84(4) 1 calc R U P A 2
C53 C 0.1944(7) 0.2989(8) 0.3467(8) 0.045(3) Uani 1 1 d . . . . .
H53 H 0.1910 0.2972 0.2925 0.054 Uiso 1 1 calc R U . . .
O1 O 0.2305(5) 0.2581(5) 0.3861(5) 0.044(2) Uani 1 1 d . . . . .
O2 O 0.1617(5) 0.3439(5) 0.3839(6) 0.049(2) Uani 1 1 d . . . . .
P1 P 0.32462(18) 0.35402(16) 0.4812(2) 0.0342(8) Uani 1 1 d . . . . .
P2 P 0.28414(19) 0.21375(15) 0.54420(19) 0.0346(8) Uani 1 1 d . . . . .
P3 P 0.1228(2) 0.39035(19) 0.5358(2) 0.0431(9) Uani 1 1 d . . . . .
P4 P 0.0732(2) 0.2478(2) 0.4762(2) 0.0481(10) Uani 1 1 d . . . . .
W1 W 0.19964(3) 0.30086(3) 0.49514(3) 0.03265(16) Uani 1 1 d D . . . .
C54 C 0.1480(8) 0.2417(7) -0.0160(9) 0.046(4) Uani 1 1 d . . . . .
C55 C 0.1042(9) 0.2625(8) -0.0794(10) 0.061(5) Uani 1 1 d . . . . .
H55 H 0.1026 0.3075 -0.0896 0.073 Uiso 1 1 calc R U . . .
C56 C 0.0621(9) 0.2217(9) -0.1294(10) 0.065(5) Uani 1 1 d . . . . .
H56 H 0.0309 0.2387 -0.1707 0.079 Uiso 1 1 calc R U . . .
C57 C 0.0673(9) 0.1562(9) -0.1169(10) 0.064(5) Uani 1 1 d . . . . .
H57 H 0.0412 0.1274 -0.1515 0.077 Uiso 1 1 calc R U . . .
C58 C 0.1078(8) 0.1332(8) -0.0583(10) 0.055(4) Uani 1 1 d . . . . .
H58 H 0.1111 0.0879 -0.0506 0.066 Uiso 1 1 calc R U . . .
C59 C 0.1467(8) 0.1758(7) -0.0061(9) 0.053(4) Uani 1 1 d . . . . .
H59 H 0.1733 0.1580 0.0377 0.063 Uiso 1 1 calc R U . . .
C60 C 0.2557(10) 0.2608(7) 0.1014(8) 0.053(4) Uani 1 1 d . . . . .
C61 C 0.2250(10) 0.2218(7) 0.1585(9) 0.061(4) Uani 1 1 d . . . . .
H61 H 0.1714 0.2142 0.1570 0.074 Uiso 1 1 calc R U . . .
C62 C 0.2715(10) 0.1942(8) 0.2168(9) 0.065(5) Uani 1 1 d . . . . .
H62 H 0.2495 0.1670 0.2531 0.078 Uiso 1 1 calc R U . . .
C63 C 0.3511(11) 0.2065(9) 0.2223(10) 0.074(5) Uani 1 1 d . . . . .
H63 H 0.3833 0.1880 0.2618 0.088 Uiso 1 1 calc R U . . .
C64 C 0.3797(11) 0.2454(9) 0.1692(10) 0.075(5) Uani 1 1 d . . . . .
H64 H 0.4329 0.2549 0.1727 0.090 Uiso 1 1 calc R U . . .
C65 C 0.3349(10) 0.2716(9) 0.1106(10) 0.070(5) Uani 1 1 d . . . . .
H65 H 0.3584 0.2982 0.0746 0.084 Uiso 1 1 calc R U . . .
C66 C 0.2464(8) 0.3373(7) -0.0218(9) 0.057(4) Uani 1 1 d D . . . .
C67 C 0.2911(8) 0.3062(8) -0.0749(8) 0.057(4) Uani 1 1 d D . . . .
H67 H 0.2933 0.2604 -0.0752 0.068 Uiso 1 1 calc R U . . .
C68 C 0.3331(9) 0.3411(8) -0.1281(9) 0.064(5) Uani 1 1 d D . . . .
H68 H 0.3616 0.3189 -0.1643 0.077 Uiso 1 1 calc R U . . .
C69 C 0.3321(9) 0.4086(8) -0.1268(10) 0.068(5) Uani 1 1 d D . . . .
H69 H 0.3587 0.4329 -0.1627 0.081 Uiso 1 1 calc R U . . .
C70 C 0.2921(9) 0.4388(8) -0.0727(11) 0.073(5) Uani 1 1 d D . . . .
H70 H 0.2944 0.4845 -0.0691 0.087 Uiso 1 1 calc R U . . .
C71 C 0.2485(9) 0.4051(8) -0.0230(10) 0.071(5) Uani 1 1 d D . . . .
H71 H 0.2190 0.4285 0.0114 0.085 Uiso 1 1 calc R U . . .
C72A C 0.1383(9) 0.3410(7) 0.0857(10) 0.068(5) Uani 0.58(3) 1 d D U P B 1
C73A C 0.1578(18) 0.369(3) 0.158(2) 0.092(12) Uani 0.58(3) 1 d D U P B 1
H73A H 0.2085 0.3644 0.1793 0.111 Uiso 0.58(3) 1 calc R U P B 1
C74A C 0.104(2) 0.405(2) 0.1985(17) 0.079(10) Uani 0.58(3) 1 d D U P B 1
H74A H 0.1162 0.4199 0.2491 0.095 Uiso 0.58(3) 1 calc R U P B 1
C75A C 0.0317(18) 0.419(2) 0.163(2) 0.082(11) Uani 0.58(3) 1 d D U P B 1
H75A H -0.0070 0.4388 0.1903 0.098 Uiso 0.58(3) 1 calc R U P B 1
C76A C 0.0177(14) 0.4038(17) 0.087(2) 0.103(13) Uani 0.58(3) 1 d D U P B 1
H76A H -0.0262 0.4206 0.0598 0.123 Uiso 0.58(3) 1 calc R U P B 1
C77A C 0.0679(14) 0.3634(16) 0.0509(19) 0.101(13) Uani 0.58(3) 1 d D U P B 1
H77A H 0.0543 0.3503 0.0001 0.121 Uiso 0.58(3) 1 calc R U P B 1
C72B C 0.1383(9) 0.3410(7) 0.0857(10) 0.068(5) Uani 0.42(3) 1 d D U P B 2
C73B C 0.1782(19) 0.374(5) 0.147(4) 0.092(12) Uani 0.42(3) 1 d D U P B 2
H73B H 0.2325 0.3719 0.1508 0.111 Uiso 0.42(3) 1 calc R U P B 2
C74B C 0.139(2) 0.409(3) 0.203(3) 0.079(10) Uani 0.42(3) 1 d D U P B 2
H74B H 0.1673 0.4305 0.2434 0.095 Uiso 0.42(3) 1 calc R U P B 2
C75B C 0.059(2) 0.410(3) 0.197(3) 0.082(11) Uani 0.42(3) 1 d D U P B 2
H75B H 0.0316 0.4347 0.2327 0.098 Uiso 0.42(3) 1 calc R U P B 2
C76B C 0.0203(18) 0.377(3) 0.141(3) 0.103(13) Uani 0.42(3) 1 d D U P B 2
H76B H -0.0341 0.3778 0.1368 0.123 Uiso 0.42(3) 1 calc R U P B 2
C77B C 0.0584(13) 0.340(3) 0.088(3) 0.101(13) Uani 0.42(3) 1 d D U P B 2
H77B H 0.0293 0.3142 0.0531 0.121 Uiso 0.42(3) 1 calc R U P B 2
B1 B 0.1969(10) 0.2951(8) 0.0372(11) 0.054(5) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.565(16) . ?
C1 P1 1.848(14) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 P2 1.835(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.400(15) . ?
C3 C8 1.407(15) . ?
C3 P2 1.808(12) . ?
C4 C5 1.364(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.364(19) . ?
C6 H6 0.9500 . ?
C7 C8 1.374(17) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.39(2) . ?
C9 C14 1.41(2) . ?
C9 P2 1.830(15) . ?
C10 C11 1.40(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.34(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.37(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.39(2) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.364(19) . ?
C15 C20 1.384(17) . ?
C15 P1 1.831(13) . ?
C16 C17 1.377(19) . ?
C16 H16 0.9500 . ?
C17 C18 1.35(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.37(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.38(2) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.392(19) . ?
C21 C26 1.40(2) . ?
C21 P1 1.823(14) . ?
C22 C23 1.433(19) . ?
C22 H22 0.9500 . ?
C23 C24 1.38(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.35(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.37(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.531(18) . ?
C27 P3 1.817(13) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 P4 1.874(15) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.3900 . ?
C29 C34 1.3900 . ?
C29 P4 1.855(8) . ?
C30 C31 1.3900 . ?
C30 H30 0.9500 . ?
C31 C32 1.3900 . ?
C31 H31 0.9500 . ?
C32 C33 1.3900 . ?
C32 H32 0.9500 . ?
C33 C34 1.3900 . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C40 1.38(2) . ?
C35 C36 1.40(2) . ?
C35 P4 1.842(15) . ?
C36 C37 1.37(2) . ?
C36 H36 0.9500 . ?
C37 C38 1.36(2) . ?
C37 H37 0.9500 . ?
C38 C39 1.39(2) . ?
C38 H38 0.9500 . ?
C39 C40 1.40(2) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 C46 1.34(2) . ?
C41 C42 1.346(18) . ?
C41 P3 1.882(13) . ?
C42 C43 1.38(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.37(2) . ?
C43 H43 0.9500 . ?
C44 C45 1.41(2) . ?
C44 H44 0.9500 . ?
C45 C46 1.40(2) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47A C48A 1.41(2) . ?
C47A C52A 1.41(2) . ?
C47A P3 1.827(16) . ?
C48A C49A 1.36(2) . ?
C48A H48A 0.9500 . ?
C49A C50A 1.39(2) . ?
C49A H49A 0.9500 . ?
C50A C51A 1.37(2) . ?
C50A H50A 0.9500 . ?
C51A C52A 1.38(2) . ?
C51A H51A 0.9500 . ?
C52A H52A 0.9500 . ?
C47B C52B 1.412(17) . ?
C47B C48B 1.415(16) . ?
C47B P3 1.827(16) . ?
C48B C49B 1.361(17) . ?
C48B H48B 0.9500 . ?
C49B C50B 1.39(2) . ?
C49B H49B 0.9500 . ?
C50B C51B 1.37(2) . ?
C50B H50B 0.9500 . ?
C51B C52B 1.376(19) . ?
C51B H51B 0.9500 . ?
C52B H52B 0.9500 . ?
C53 O1 1.244(16) . ?
C53 O2 1.292(16) . ?
C53 W1 2.605(14) . ?
C53 H53 0.9500 . ?
O1 W1 2.206(9) . ?
O2 W1 2.215(9) . ?
P1 W1 2.474(3) . ?
P2 W1 2.458(3) . ?
P3 W1 2.423(4) . ?
P4 W1 2.476(4) . ?
W1 H1 1.255(15) . ?
W1 H2 1.250(15) . ?
C54 C59 1.379(19) . ?
C54 C55 1.38(2) . ?
C54 B1 1.65(2) . ?
C55 C56 1.40(2) . ?
C55 H55 0.9500 . ?
C56 C57 1.38(2) . ?
C56 H56 0.9500 . ?
C57 C58 1.30(2) . ?
C57 H57 0.9500 . ?
C58 C59 1.42(2) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?
C60 C65 1.40(2) . ?
C60 C61 1.42(2) . ?
C60 B1 1.64(2) . ?
C61 C62 1.39(2) . ?
C61 H61 0.9500 . ?
C62 C63 1.41(2) . ?
C62 H62 0.9500 . ?
C63 C64 1.35(2) . ?
C63 H63 0.9500 . ?
C64 C65 1.37(2) . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
C66 C71 1.408(18) . ?
C66 C67 1.408(17) . ?
C66 B1 1.64(2) . ?
C67 C68 1.420(18) . ?
C67 H67 0.9500 . ?
C68 C69 1.40(2) . ?
C68 H68 0.9500 . ?
C69 C70 1.36(2) . ?
C69 H69 0.9500 . ?
C70 C71 1.382(19) . ?
C70 H70 0.9500 . ?
C71 H71 0.9500 . ?
C72A C73A 1.42(2) . ?
C72A C77A 1.42(2) . ?
C72A B1 1.67(2) . ?
C73A C74A 1.43(2) . ?
C73A H73A 0.9500 . ?
C74A C75A 1.40(2) . ?
C74A H74A 0.9500 . ?
C75A C76A 1.37(2) . ?
C75A H75A 0.9500 . ?
C76A C77A 1.39(2) . ?
C76A H76A 0.9500 . ?
C77A H77A 0.9500 . ?
C72B C77B 1.40(2) . ?
C72B C73B 1.42(2) . ?
C72B B1 1.67(2) . ?
C73B C74B 1.43(2) . ?
C73B H73B 0.9500 . ?
C74B C75B 1.41(2) . ?
C74B H74B 0.9500 . ?
C75B C76B 1.36(3) . ?
C75B H75B 0.9500 . ?
C76B C77B 1.39(2) . ?
C76B H76B 0.9500 . ?
C77B H77B 0.9500 . ?

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
C2 C1 P1 106.6(8) . . ?
C2 C1 H1A 110.4 . . ?
P1 C1 H1A 110.4 . . ?
C2 C1 H1B 110.4 . . ?
P1 C1 H1B 110.4 . . ?
H1A C1 H1B 108.6 . . ?
C1 C2 P2 111.9(9) . . ?
C1 C2 H2A 109.2 . . ?
P2 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
P2 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 C8 117.2(11) . . ?
C4 C3 P2 120.9(9) . . ?
C8 C3 P2 121.8(9) . . ?
C5 C4 C3 121.3(12) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 120.4(13) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 119.4(13) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 121.2(14) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 H7 119.4 . . ?
C7 C8 C3 120.4(13) . . ?
C7 C8 H8 119.8 . . ?
C3 C8 H8 119.8 . . ?
C10 C9 C14 119.2(16) . . ?
C10 C9 P2 118.2(13) . . ?
C14 C9 P2 122.7(13) . . ?
C9 C10 C11 119(2) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C12 C11 C10 121(2) . . ?
C12 C11 H11 119.5 . . ?
C10 C11 H11 119.5 . . ?
C11 C12 C13 121(2) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C12 C13 C14 120(2) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C13 C14 C9 120(2) . . ?
C13 C14 H14 120.2 . . ?
C9 C14 H14 120.2 . . ?
C16 C15 C20 117.4(13) . . ?
C16 C15 P1 123.0(9) . . ?
C20 C15 P1 119.6(12) . . ?
C15 C16 C17 122.1(13) . . ?
C15 C16 H16 119.0 . . ?
C17 C16 H16 119.0 . . ?
C18 C17 C16 120.8(15) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 118.2(14) . . ?
C17 C18 H18 120.9 . . ?
C19 C18 H18 120.9 . . ?
C18 C19 C20 121.7(14) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C15 C20 C19 119.8(15) . . ?
C15 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C22 C21 C26 118.7(13) . . ?
C22 C21 P1 117.3(11) . . ?
C26 C21 P1 123.8(11) . . ?
C21 C22 C23 120.0(15) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 117.5(16) . . ?
C24 C23 H23 121.2 . . ?
C22 C23 H23 121.2 . . ?
C25 C24 C23 122.9(17) . . ?
C25 C24 H24 118.5 . . ?
C23 C24 H24 118.5 . . ?
C24 C25 C26 120(2) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 120.9(17) . . ?
C25 C26 H26 119.6 . . ?
C21 C26 H26 119.6 . . ?
C28 C27 P3 109.8(9) . . ?
C28 C27 H27A 109.7 . . ?
P3 C27 H27A 109.7 . . ?
C28 C27 H27B 109.7 . . ?
P3 C27 H27B 109.7 . . ?
H27A C27 H27B 108.2 . . ?
C27 C28 P4 110.6(9) . . ?
C27 C28 H28A 109.5 . . ?
P4 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
P4 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
C30 C29 C34 120.0 . . ?
C30 C29 P4 119.6(5) . . ?
C34 C29 P4 120.3(5) . . ?
C29 C30 C31 120.0 . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C32 C31 C30 120.0 . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C33 C32 C31 120.0 . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C34 C33 C32 120.0 . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C34 C29 120.0 . . ?
C33 C34 H34 120.0 . . ?
C29 C34 H34 120.0 . . ?
C40 C35 C36 120.5(16) . . ?
C40 C35 P4 122.2(14) . . ?
C36 C35 P4 117.3(12) . . ?
C37 C36 C35 119.9(16) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C38 C37 C36 120.3(17) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C37 C38 C39 120.4(16) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C38 C39 C40 120.2(17) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C35 C40 C39 118.4(19) . . ?
C35 C40 H40 120.8 . . ?
C39 C40 H40 120.8 . . ?
C46 C41 C42 121.6(14) . . ?
C46 C41 P3 120.0(11) . . ?
C42 C41 P3 118.3(11) . . ?
C41 C42 C43 121.5(15) . . ?
C41 C42 H42 119.3 . . ?
C43 C42 H42 119.3 . . ?
C44 C43 C42 119.6(16) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C45 118.4(14) . . ?
C43 C44 H44 120.8 . . ?
C45 C44 H44 120.8 . . ?
C46 C45 C44 120.3(16) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C41 C46 C45 118.6(16) . . ?
C41 C46 H46 120.7 . . ?
C45 C46 H46 120.7 . . ?
C48A C47A C52A 117(2) . . ?
C48A C47A P3 121(3) . . ?
C52A C47A P3 122(3) . . ?
C49A C48A C47A 121(3) . . ?
C49A C48A H48A 119.3 . . ?
C47A C48A H48A 119.3 . . ?
C48A C49A C50A 118(3) . . ?
C48A C49A H49A 120.8 . . ?
C50A C49A H49A 120.8 . . ?
C51A C50A C49A 119(3) . . ?
C51A C50A H50A 120.8 . . ?
C49A C50A H50A 120.7 . . ?
C50A C51A C52A 122(3) . . ?
C50A C51A H51A 118.8 . . ?
C52A C51A H51A 118.8 . . ?
C51A C52A C47A 119(3) . . ?
C51A C52A H52A 120.7 . . ?
C47A C52A H52A 120.7 . . ?
C52B C47B C48B 117.6(14) . . ?
C52B C47B P3 118.3(12) . . ?
C48B C47B P3 124.0(11) . . ?
C49B C48B C47B 122.0(14) . . ?
C49B C48B H48B 119.0 . . ?
C47B C48B H48B 119.0 . . ?
C48B C49B C50B 119.3(15) . . ?
C48B C49B H49B 120.3 . . ?
C50B C49B H49B 120.3 . . ?
C51B C50B C49B 118.4(16) . . ?
C51B C50B H50B 120.8 . . ?
C49B C50B H50B 120.8 . . ?
C50B C51B C52B 123.8(17) . . ?
C50B C51B H51B 118.1 . . ?
C52B C51B H51B 118.1 . . ?
C51B C52B C47B 118.0(16) . . ?
C51B C52B H52B 121.0 . . ?
C47B C52B H52B 121.0 . . ?
O1 C53 O2 115.8(13) . . ?
O1 C53 W1 57.7(7) . . ?
O2 C53 W1 58.2(7) . . ?
O1 C53 H53 122.1 . . ?
O2 C53 H53 122.1 . . ?
W1 C53 H53 178.0 . . ?
C53 O1 W1 93.9(9) . . ?
C53 O2 W1 92.1(8) . . ?
C21 P1 C15 102.4(6) . . ?
C21 P1 C1 103.3(6) . . ?
C15 P1 C1 99.5(6) . . ?
C21 P1 W1 118.3(4) . . ?
C15 P1 W1 122.8(4) . . ?
C1 P1 W1 107.4(5) . . ?
C3 P2 C9 103.1(6) . . ?
C3 P2 C2 102.7(6) . . ?
C9 P2 C2 103.9(7) . . ?
C3 P2 W1 124.5(4) . . ?
C9 P2 W1 112.6(5) . . ?
C2 P2 W1 108.1(4) . . ?
C27 P3 C47B 103.3(7) . . ?
C27 P3 C47A 103.3(7) . . ?
C27 P3 C41 100.4(6) . . ?
C47B P3 C41 104.1(7) . . ?
C47A P3 C41 104.1(7) . . ?
C27 P3 W1 105.5(5) . . ?
C47B P3 W1 120.6(5) . . ?
C47A P3 W1 120.6(5) . . ?
C41 P3 W1 120.0(4) . . ?
C35 P4 C29 105.7(6) . . ?
C35 P4 C28 105.6(7) . . ?
C29 P4 C28 99.3(6) . . ?
C35 P4 W1 115.5(5) . . ?
C29 P4 W1 122.7(3) . . ?
C28 P4 W1 105.8(4) . . ?
O1 W1 O2 58.1(4) . . ?
O1 W1 P3 137.0(3) . . ?
O2 W1 P3 79.0(3) . . ?
O1 W1 P2 80.6(3) . . ?
O2 W1 P2 138.5(3) . . ?
P3 W1 P2 142.37(12) . . ?
O1 W1 P1 80.2(2) . . ?
O2 W1 P1 87.4(2) . . ?
P3 W1 P1 101.36(12) . . ?
P2 W1 P1 81.08(11) . . ?
O1 W1 P4 88.1(2) . . ?
O2 W1 P4 80.9(2) . . ?
P3 W1 P4 82.70(13) . . ?
P2 W1 P4 103.62(12) . . ?
P1 W1 P4 166.60(13) . . ?
O1 W1 C53 28.4(4) . . ?
O2 W1 C53 29.7(4) . . ?
P3 W1 C53 108.6(4) . . ?
P2 W1 C53 109.0(4) . . ?
P1 W1 C53 83.5(3) . . ?
P4 W1 C53 83.1(3) . . ?
O1 W1 H1 146(4) . . ?
O2 W1 H1 134(5) . . ?
P3 W1 H1 68(5) . . ?
P2 W1 H1 78(5) . . ?
P1 W1 H1 70(4) . . ?
P4 W1 H1 123(4) . . ?
C53 W1 H1 152(4) . . ?
O1 W1 H2 146(4) . . ?
O2 W1 H2 128(4) . . ?
P3 W1 H2 61(5) . . ?
P2 W1 H2 88(5) . . ?
P1 W1 H2 129(4) . . ?
P4 W1 H2 64(4) . . ?
C53 W1 H2 146(4) . . ?
H1 W1 H2 59.1(10) . . ?
C59 C54 C55 113.4(15) . . ?
C59 C54 B1 127.1(15) . . ?
C55 C54 B1 119.4(13) . . ?
C54 C55 C56 124.4(15) . . ?
C54 C55 H55 117.8 . . ?
C56 C55 H55 117.8 . . ?
C57 C56 C55 118.0(17) . . ?
C57 C56 H56 121.0 . . ?
C55 C56 H56 121.0 . . ?
C58 C57 C56 120.8(19) . . ?
C58 C57 H57 119.6 . . ?
C56 C57 H57 119.6 . . ?
C57 C58 C59 120.1(16) . . ?
C57 C58 H58 119.9 . . ?
C59 C58 H58 119.9 . . ?
C54 C59 C58 123.1(16) . . ?
C54 C59 H59 118.5 . . ?
C58 C59 H59 118.5 . . ?
C65 C60 C61 114.9(16) . . ?
C65 C60 B1 125.8(14) . . ?
C61 C60 B1 118.9(15) . . ?
C62 C61 C60 121.7(17) . . ?
C62 C61 H61 119.2 . . ?
C60 C61 H61 119.2 . . ?
C61 C62 C63 120.5(16) . . ?
C61 C62 H62 119.8 . . ?
C63 C62 H62 119.8 . . ?
C64 C63 C62 117.7(18) . . ?
C64 C63 H63 121.2 . . ?
C62 C63 H63 121.2 . . ?
C63 C64 C65 122.4(18) . . ?
C63 C64 H64 118.8 . . ?
C65 C64 H64 118.8 . . ?
C64 C65 C60 122.8(17) . . ?
C64 C65 H65 118.6 . . ?
C60 C65 H65 118.6 . . ?
C71 C66 C67 115.5(13) . . ?
C71 C66 B1 123.9(13) . . ?
C67 C66 B1 120.6(13) . . ?
C66 C67 C68 122.1(14) . . ?
C66 C67 H67 118.9 . . ?
C68 C67 H67 118.9 . . ?
C69 C68 C67 119.4(14) . . ?
C69 C68 H68 120.3 . . ?
C67 C68 H68 120.3 . . ?
C70 C69 C68 118.5(14) . . ?
C70 C69 H69 120.7 . . ?
C68 C69 H69 120.7 . . ?
C69 C70 C71 122.3(16) . . ?
C69 C70 H70 118.9 . . ?
C71 C70 H70 118.9 . . ?
C70 C71 C66 122.0(15) . . ?
C70 C71 H71 119.0 . . ?
C66 C71 H71 119.0 . . ?
C73A C72A C77A 113.9(19) . . ?
C73A C72A B1 124.7(17) . . ?
C77A C72A B1 120.6(17) . . ?
C72A C73A C74A 122(2) . . ?
C72A C73A H73A 118.9 . . ?
C74A C73A H73A 118.9 . . ?
C75A C74A C73A 119(2) . . ?
C75A C74A H74A 120.6 . . ?
C73A C74A H74A 120.6 . . ?
C76A C75A C74A 120(2) . . ?
C76A C75A H75A 120.2 . . ?
C74A C75A H75A 120.2 . . ?
C75A C76A C77A 120(2) . . ?
C75A C76A H76A 120.0 . . ?
C77A C76A H76A 120.0 . . ?
C76A C77A C72A 123(2) . . ?
C76A C77A H77A 118.3 . . ?
C72A C77A H77A 118.3 . . ?
C77B C72B C73B 115(2) . . ?
C77B C72B B1 130.9(18) . . ?
C73B C72B B1 111.7(19) . . ?
C72B C73B C74B 122(2) . . ?
C72B C73B H73B 118.9 . . ?
C74B C73B H73B 118.9 . . ?
C75B C74B C73B 118(2) . . ?
C75B C74B H74B 120.8 . . ?
C73B C74B H74B 120.8 . . ?
C76B C75B C74B 119(2) . . ?
C76B C75B H75B 120.3 . . ?
C74B C75B H75B 120.3 . . ?
C75B C76B C77B 122(2) . . ?
C75B C76B H76B 119.2 . . ?
C77B C76B H76B 119.2 . . ?
C76B C77B C72B 122(2) . . ?
C76B C77B H77B 118.8 . . ?
C72B C77B H77B 118.8 . . ?
C66 B1 C60 109.3(13) . . ?
C66 B1 C54 106.0(13) . . ?
C60 B1 C54 112.4(12) . . ?
C66 B1 C72B 112.4(13) . . ?
C60 B1 C72B 106.0(13) . . ?
C54 B1 C72B 110.9(13) . . ?
C66 B1 C72A 112.4(13) . . ?
C60 B1 C72A 106.0(13) . . ?
C54 B1 C72A 110.9(13) . . ?

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
P1 C1 C2 P2 54.8(11) . . . . ?
C8 C3 C4 C5 -3(2) . . . . ?
P2 C3 C4 C5 175.1(12) . . . . ?
C3 C4 C5 C6 2(2) . . . . ?
C4 C5 C6 C7 0(3) . . . . ?
C5 C6 C7 C8 -2(3) . . . . ?
C6 C7 C8 C3 1(3) . . . . ?
C4 C3 C8 C7 1(2) . . . . ?
P2 C3 C8 C7 -176.8(13) . . . . ?
C14 C9 C10 C11 2(2) . . . . ?
P2 C9 C10 C11 -179.7(12) . . . . ?
C9 C10 C11 C12 -1(3) . . . . ?
C10 C11 C12 C13 4(3) . . . . ?
C11 C12 C13 C14 -6(3) . . . . ?
C12 C13 C14 C9 7(3) . . . . ?
C10 C9 C14 C13 -4(3) . . . . ?
P2 C9 C14 C13 177.1(16) . . . . ?
C20 C15 C16 C17 -3(2) . . . . ?
P1 C15 C16 C17 177.9(11) . . . . ?
C15 C16 C17 C18 0(2) . . . . ?
C16 C17 C18 C19 2(2) . . . . ?
C17 C18 C19 C20 -2(2) . . . . ?
C16 C15 C20 C19 3(2) . . . . ?
P1 C15 C20 C19 -177.8(11) . . . . ?
C18 C19 C20 C15 0(2) . . . . ?
C26 C21 C22 C23 -2.3(19) . . . . ?
P1 C21 C22 C23 -176.6(9) . . . . ?
C21 C22 C23 C24 0(2) . . . . ?
C22 C23 C24 C25 1(2) . . . . ?
C23 C24 C25 C26 0(3) . . . . ?
C24 C25 C26 C21 -2(2) . . . . ?
C22 C21 C26 C25 3(2) . . . . ?
P1 C21 C26 C25 177.1(12) . . . . ?
P3 C27 C28 P4 -55.4(13) . . . . ?
C34 C29 C30 C31 0.0 . . . . ?
P4 C29 C30 C31 -176.8(8) . . . . ?
C29 C30 C31 C32 0.0 . . . . ?
C30 C31 C32 C33 0.0 . . . . ?
C31 C32 C33 C34 0.0 . . . . ?
C32 C33 C34 C29 0.0 . . . . ?
C30 C29 C34 C33 0.0 . . . . ?
P4 C29 C34 C33 176.7(8) . . . . ?
C40 C35 C36 C37 -1(2) . . . . ?
P4 C35 C36 C37 -176.6(13) . . . . ?
C35 C36 C37 C38 1(3) . . . . ?
C36 C37 C38 C39 3(3) . . . . ?
C37 C38 C39 C40 -6(3) . . . . ?
C36 C35 C40 C39 -2(2) . . . . ?
P4 C35 C40 C39 173.4(13) . . . . ?
C38 C39 C40 C35 5(3) . . . . ?
C46 C41 C42 C43 1(2) . . . . ?
P3 C41 C42 C43 -177.5(11) . . . . ?
C41 C42 C43 C44 -1(2) . . . . ?
C42 C43 C44 C45 0(2) . . . . ?
C43 C44 C45 C46 1(2) . . . . ?
C42 C41 C46 C45 0(2) . . . . ?
P3 C41 C46 C45 178.6(12) . . . . ?
C44 C45 C46 C41 -1(2) . . . . ?
C52A C47A C48A C49A -9(11) . . . . ?
P3 C47A C48A C49A 167(8) . . . . ?
C47A C48A C49A C50A 21(16) . . . . ?
C48A C49A C50A C51A -17(26) . . . . ?
C49A C50A C51A C52A 0(31) . . . . ?
C50A C51A C52A C47A 12(24) . . . . ?
C48A C47A C52A C51A -7(13) . . . . ?
P3 C47A C52A C51A 176(9) . . . . ?
C52B C47B C48B C49B -8(3) . . . . ?
P3 C47B C48B C49B 176.6(13) . . . . ?
C47B C48B C49B C50B 12(3) . . . . ?
C48B C49B C50B C51B -9(5) . . . . ?
C49B C50B C51B C52B 4(6) . . . . ?
C50B C51B C52B C47B 0(5) . . . . ?
C48B C47B C52B C51B 2(3) . . . . ?
P3 C47B C52B C51B 178(2) . . . . ?
O2 C53 O1 W1 2.4(11) . . . . ?
O1 C53 O2 W1 -2.4(11) . . . . ?
C22 C21 P1 C15 -47.2(11) . . . . ?
C26 C21 P1 C15 138.8(12) . . . . ?
C22 C21 P1 C1 -150.3(10) . . . . ?
C26 C21 P1 C1 35.8(13) . . . . ?
C22 C21 P1 W1 91.2(10) . . . . ?
C26 C21 P1 W1 -82.7(12) . . . . ?
C16 C15 P1 C21 125.0(12) . . . . ?
C20 C15 P1 C21 -54.4(12) . . . . ?
C16 C15 P1 C1 -128.9(11) . . . . ?
C20 C15 P1 C1 51.6(12) . . . . ?
C16 C15 P1 W1 -11.0(13) . . . . ?
C20 C15 P1 W1 169.6(9) . . . . ?
C2 C1 P1 C21 -172.7(9) . . . . ?
C2 C1 P1 C15 82.0(10) . . . . ?
C2 C1 P1 W1 -46.9(9) . . . . ?
C4 C3 P2 C9 -162.0(11) . . . . ?
C8 C3 P2 C9 15.7(13) . . . . ?
C4 C3 P2 C2 90.3(12) . . . . ?
C8 C3 P2 C2 -92.0(12) . . . . ?
C4 C3 P2 W1 -32.4(13) . . . . ?
C8 C3 P2 W1 145.3(10) . . . . ?
C10 C9 P2 C3 64.1(12) . . . . ?
C14 C9 P2 C3 -117.2(14) . . . . ?
C10 C9 P2 C2 171.0(11) . . . . ?
C14 C9 P2 C2 -10.4(15) . . . . ?
C10 C9 P2 W1 -72.4(12) . . . . ?
C14 C9 P2 W1 106.3(14) . . . . ?
C1 C2 P2 C3 -170.3(9) . . . . ?
C1 C2 P2 C9 82.6(10) . . . . ?
C1 C2 P2 W1 -37.2(10) . . . . ?
C28 C27 P3 C47B -76.8(12) . . . . ?
C28 C27 P3 C47A -76.8(12) . . . . ?
C28 C27 P3 C41 175.9(11) . . . . ?
C28 C27 P3 W1 50.6(11) . . . . ?
C52B C47B P3 C27 -34.1(18) . . . . ?
C48B C47B P3 C27 141.1(15) . . . . ?
C52B C47B P3 C41 70.3(18) . . . . ?
C48B C47B P3 C41 -114.5(16) . . . . ?
C52B C47B P3 W1 -151.4(16) . . . . ?
C48B C47B P3 W1 23.8(17) . . . . ?
C48A C47A P3 C27 111(5) . . . . ?
C52A C47A P3 C27 -72(6) . . . . ?
C48A C47A P3 C41 -144(5) . . . . ?
C52A C47A P3 C41 32(6) . . . . ?
C48A C47A P3 W1 -6(5) . . . . ?
C52A C47A P3 W1 170(6) . . . . ?
C46 C41 P3 C27 127.2(13) . . . . ?
C42 C41 P3 C27 -54.0(12) . . . . ?
C46 C41 P3 C47B 20.6(14) . . . . ?
C42 C41 P3 C47B -160.7(11) . . . . ?
C46 C41 P3 C47A 20.6(14) . . . . ?
C42 C41 P3 C47A -160.7(11) . . . . ?
C46 C41 P3 W1 -118.0(12) . . . . ?
C42 C41 P3 W1 60.7(12) . . . . ?
C40 C35 P4 C29 123.3(13) . . . . ?
C36 C35 P4 C29 -60.8(13) . . . . ?
C40 C35 P4 C28 18.7(15) . . . . ?
C36 C35 P4 C28 -165.4(12) . . . . ?
C40 C35 P4 W1 -97.7(13) . . . . ?
C36 C35 P4 W1 78.2(12) . . . . ?
C30 C29 P4 C35 164.1(7) . . . . ?
C34 C29 P4 C35 -12.7(8) . . . . ?
C30 C29 P4 C28 -86.7(7) . . . . ?
C34 C29 P4 C28 96.5(7) . . . . ?
C30 C29 P4 W1 28.8(7) . . . . ?
C34 C29 P4 W1 -147.9(5) . . . . ?
C27 C28 P4 C35 -89.9(11) . . . . ?
C27 C28 P4 C29 160.8(10) . . . . ?
C27 C28 P4 W1 32.9(11) . . . . ?
C59 C54 C55 C56 0(2) . . . . ?
B1 C54 C55 C56 178.3(14) . . . . ?
C54 C55 C56 C57 -3(2) . . . . ?
C55 C56 C57 C58 3(3) . . . . ?
C56 C57 C58 C59 0(2) . . . . ?
C55 C54 C59 C58 3(2) . . . . ?
B1 C54 C59 C58 -174.7(13) . . . . ?
C57 C58 C59 C54 -4(2) . . . . ?
C65 C60 C61 C62 -3(2) . . . . ?
B1 C60 C61 C62 -176.6(13) . . . . ?
C60 C61 C62 C63 2(2) . . . . ?
C61 C62 C63 C64 0(2) . . . . ?
C62 C63 C64 C65 -1(3) . . . . ?
C63 C64 C65 C60 1(3) . . . . ?
C61 C60 C65 C64 1(2) . . . . ?
B1 C60 C65 C64 174.6(16) . . . . ?
C71 C66 C67 C68 -2(2) . . . . ?
B1 C66 C67 C68 178.3(15) . . . . ?
C66 C67 C68 C69 2(2) . . . . ?
C67 C68 C69 C70 2(3) . . . . ?
C68 C69 C70 C71 -5(3) . . . . ?
C69 C70 C71 C66 4(3) . . . . ?
C67 C66 C71 C70 -1(3) . . . . ?
B1 C66 C71 C70 178.8(16) . . . . ?
C77A C72A C73A C74A 14(8) . . . . ?
B1 C72A C73A C74A -176(4) . . . . ?
C72A C73A C74A C75A -7(9) . . . . ?
C73A C74A C75A C76A -7(7) . . . . ?
C74A C75A C76A C77A 13(6) . . . . ?
C75A C76A C77A C72A -6(5) . . . . ?
C73A C72A C77A C76A -7(5) . . . . ?
B1 C72A C77A C76A -178(3) . . . . ?
C77B C72B C73B C74B -6(12) . . . . ?
B1 C72B C73B C74B -171(8) . . . . ?
C72B C73B C74B C75B 1(15) . . . . ?
C73B C74B C75B C76B 2(13) . . . . ?
C74B C75B C76B C77B 0(11) . . . . ?
C75B C76B C77B C72B -6(10) . . . . ?
C73B C72B C77B C76B 9(9) . . . . ?
B1 C72B C77B C76B 171(4) . . . . ?
C71 C66 B1 C60 -108.1(17) . . . . ?
C67 C66 B1 C60 71.3(18) . . . . ?
C71 C66 B1 C54 130.6(16) . . . . ?
C67 C66 B1 C54 -50.1(19) . . . . ?
C71 C66 B1 C72B 9(2) . . . . ?
C67 C66 B1 C72B -171.4(14) . . . . ?
C71 C66 B1 C72A 9(2) . . . . ?
C67 C66 B1 C72A -171.4(14) . . . . ?
C65 C60 B1 C66 7(2) . . . . ?
C61 C60 B1 C66 179.9(12) . . . . ?
C65 C60 B1 C54 124.4(16) . . . . ?
C61 C60 B1 C54 -62.7(17) . . . . ?
C65 C60 B1 C72B -114.3(16) . . . . ?
C61 C60 B1 C72B 58.6(16) . . . . ?
C65 C60 B1 C72A -114.3(16) . . . . ?
C61 C60 B1 C72A 58.6(16) . . . . ?
C59 C54 B1 C66 126.4(16) . . . . ?
C55 C54 B1 C66 -51.5(17) . . . . ?
C59 C54 B1 C60 7(2) . . . . ?
C55 C54 B1 C60 -170.9(13) . . . . ?
C59 C54 B1 C72B -111.4(17) . . . . ?
C55 C54 B1 C72B 70.7(18) . . . . ?
C59 C54 B1 C72A -111.4(17) . . . . ?
C55 C54 B1 C72A 70.7(18) . . . . ?
C77B C72B B1 C66 119(4) . . . . ?
C73B C72B B1 C66 -79(6) . . . . ?
C77B C72B B1 C60 -121(4) . . . . ?
C73B C72B B1 C60 41(6) . . . . ?
C77B C72B B1 C54 1(5) . . . . ?
C73B C72B B1 C54 163(6) . . . . ?
C73A C72A B1 C66 -91(4) . . . . ?
C77A C72A B1 C66 78(3) . . . . ?
C73A C72A B1 C60 28(4) . . . . ?
C77A C72A B1 C60 -163(2) . . . . ?
C73A C72A B1 C54 150(4) . . . . ?
C77A C72A B1 C54 -40(3) . . . . ?

_refine_diff_density_max         2.497
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.191

