# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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. 
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#######################################################################

data_14131B
_database_code_depnum_ccdc_archive 'CCDC 1039148'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        '[Et4N][W(CO)3(PhBP3)]'
_chemical_name_common            14131b
_chemical_melting_point          573-577
_chemical_formula_moiety         'C48 H41 B O3 P3 W, C8 H20 N'
_chemical_formula_sum            'C56 H61 B N O3 P3 W'
_chemical_formula_weight         1083.62

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'
N N 0.0061 0.0033 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -z-1/2'

_cell_length_a                   21.808(3)
_cell_length_b                   20.261(3)
_cell_length_c                   22.172(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9797(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2798
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      27.46
_exptl_crystal_description       Plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_F_000             4416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.502
_shelx_estimated_absorpt_T_min   0.475
_shelx_estimated_absorpt_T_max   0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5427
_exptl_absorpt_correction_T_max  0.7924
_exptl_absorpt_process_details   'SADABS 2014/1 (Sheldrick, 2014)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            106009
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.651
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11217
_reflns_number_gt                8645
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0276P)²+18.9537P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11217
_refine_ls_number_parameters     590
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0305
_refine_ls_wR_factor_ref         0.0738
_refine_ls_wR_factor_gt          0.0665
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.002
_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
W1 W 0.20846(2) 0.34730(2) 0.13806(2) 0.01545(4) Uani 1 1 d . . . . .
P1 P 0.19711(4) 0.22310(4) 0.13149(4) 0.01758(17) Uani 1 1 d . . . . .
P2 P 0.25390(4) 0.33125(4) 0.03345(4) 0.01733(17) Uani 1 1 d . . . . .
P3 P 0.31746(4) 0.32244(4) 0.17257(4) 0.01722(17) Uani 1 1 d . . . . .
C1 C 0.12657(17) 0.36790(18) 0.10701(16) 0.0251(8) Uani 1 1 d . . . . .
O1 O 0.07853(12) 0.38544(15) 0.09010(12) 0.0373(7) Uani 1 1 d . . . . .
C2 C 0.17169(16) 0.35155(17) 0.21935(15) 0.0220(7) Uani 1 1 d . . . . .
O2 O 0.14704(13) 0.35718(14) 0.26558(11) 0.0358(7) Uani 1 1 d . . . . .
C3 C 0.21576(16) 0.44359(18) 0.14549(15) 0.0229(7) Uani 1 1 d . . . . .
O3 O 0.21537(13) 0.50092(12) 0.15239(13) 0.0347(6) Uani 1 1 d . . . . .
B1 B 0.32251(17) 0.21637(19) 0.08296(17) 0.0182(7) Uani 1 1 d . . . . .
C4 C 0.25450(15) 0.18035(16) 0.08607(15) 0.0192(7) Uani 1 1 d . . . . .
H4A H 0.2599 0.1353 0.1025 0.023 Uiso 1 1 calc R U . . .
H4B H 0.2385 0.1759 0.0445 0.023 Uiso 1 1 calc R U . . .
C5 C 0.19976(15) 0.17440(17) 0.20182(15) 0.0205(7) Uani 1 1 d . . . . .
C6 C 0.18422(17) 0.10745(18) 0.19997(17) 0.0290(8) Uani 1 1 d . . . . .
H6A H 0.1685 0.0890 0.1637 0.035 Uiso 1 1 calc R U . . .
C7 C 0.19146(18) 0.06789(18) 0.24999(19) 0.0341(9) Uani 1 1 d . . . . .
H7A H 0.1804 0.0226 0.2480 0.041 Uiso 1 1 calc R U . . .
C8 C 0.21476(18) 0.09373(19) 0.30312(19) 0.0345(9) Uani 1 1 d . . . . .
H8A H 0.2205 0.0662 0.3373 0.041 Uiso 1 1 calc R U . . .
C9 C 0.22948(19) 0.1595(2) 0.30590(18) 0.0342(9) Uani 1 1 d . . . . .
H9A H 0.2454 0.1776 0.3422 0.041 Uiso 1 1 calc R U . . .
C10 C 0.22116(17) 0.19992(18) 0.25565(16) 0.0268(8) Uani 1 1 d . . . . .
H10A H 0.2303 0.2457 0.2585 0.032 Uiso 1 1 calc R U . . .
C11 C 0.12152(16) 0.19707(17) 0.10319(17) 0.0251(8) Uani 1 1 d . . . . .
C12 C 0.11267(19) 0.1636(2) 0.04984(18) 0.0360(10) Uani 1 1 d . . . . .
H12A H 0.1470 0.1519 0.0257 0.043 Uiso 1 1 calc R U . . .
C13 C 0.0535(2) 0.1466(2) 0.0308(2) 0.0488(12) Uani 1 1 d . . . . .
H13A H 0.0477 0.1242 -0.0065 0.059 Uiso 1 1 calc R U . . .
C14 C 0.0036(2) 0.1625(2) 0.0660(2) 0.0507(13) Uani 1 1 d . . . . .
H14A H -0.0366 0.1509 0.0533 0.061 Uiso 1 1 calc R U . . .
C15 C 0.0122(2) 0.1950(3) 0.1195(3) 0.0570(14) Uani 1 1 d . . . . .
H15A H -0.0222 0.2051 0.1442 0.068 Uiso 1 1 calc R U . . .
C16 C 0.07006(18) 0.2133(2) 0.1379(2) 0.0442(11) Uani 1 1 d . . . . .
H16A H 0.0751 0.2371 0.1744 0.053 Uiso 1 1 calc R U . . .
C17 C 0.32242(15) 0.28058(16) 0.03514(15) 0.0187(7) Uani 1 1 d . . . . .
H17A H 0.3296 0.2634 -0.0061 0.022 Uiso 1 1 calc R U . . .
H17B H 0.3576 0.3093 0.0454 0.022 Uiso 1 1 calc R U . . .
C18 C 0.20474(15) 0.29109(17) -0.02371(14) 0.0200(7) Uani 1 1 d . . . . .
C19 C 0.22399(16) 0.23773(17) -0.05890(15) 0.0239(8) Uani 1 1 d . . . . .
H19A H 0.2638 0.2199 -0.0529 0.029 Uiso 1 1 calc R U . . .
C20 C 0.18583(18) 0.21033(18) -0.10253(16) 0.0283(8) Uani 1 1 d . . . . .
H20A H 0.1999 0.1745 -0.1264 0.034 Uiso 1 1 calc R U . . .
C21 C 0.12769(17) 0.23509(19) -0.11116(16) 0.0301(9) Uani 1 1 d . . . . .
H21A H 0.1016 0.2164 -0.1409 0.036 Uiso 1 1 calc R U . . .
C22 C 0.10774(17) 0.2870(2) -0.07640(17) 0.0337(9) Uani 1 1 d . . . . .
H22A H 0.0675 0.3039 -0.0820 0.040 Uiso 1 1 calc R U . . .
C23 C 0.14566(16) 0.31495(19) -0.03334(16) 0.0278(8) Uani 1 1 d . . . . .
H23A H 0.1311 0.3510 -0.0100 0.033 Uiso 1 1 calc R U . . .
C24 C 0.27705(15) 0.40591(17) -0.00878(15) 0.0204(7) Uani 1 1 d . . . . .
C25 C 0.32739(17) 0.40480(19) -0.04722(17) 0.0301(9) Uani 1 1 d . . . . .
H25A H 0.3485 0.3644 -0.0540 0.036 Uiso 1 1 calc R U . . .
C26 C 0.34732(19) 0.4619(2) -0.07587(19) 0.0381(10) Uani 1 1 d . . . . .
H26A H 0.3822 0.4606 -0.1016 0.046 Uiso 1 1 calc R U . . .
C27 C 0.3164(2) 0.5205(2) -0.06693(18) 0.0368(10) Uani 1 1 d . . . . .
H27A H 0.3299 0.5596 -0.0865 0.044 Uiso 1 1 calc R U . . .
C28 C 0.2661(2) 0.52211(19) -0.02964(17) 0.0349(9) Uani 1 1 d . . . . .
H28A H 0.2445 0.5623 -0.0237 0.042 Uiso 1 1 calc R U . . .
C29 C 0.24669(18) 0.46521(17) -0.00065(16) 0.0272(8) Uani 1 1 d . . . . .
H29A H 0.2120 0.4669 0.0252 0.033 Uiso 1 1 calc R U . . .
C30 C 0.34452(15) 0.24049(16) 0.15165(15) 0.0198(7) Uani 1 1 d . . . . .
H30A H 0.3899 0.2400 0.1535 0.024 Uiso 1 1 calc R U . . .
H30B H 0.3292 0.2082 0.1816 0.024 Uiso 1 1 calc R U . . .
C31 C 0.37962(16) 0.37660(17) 0.14449(15) 0.0217(7) Uani 1 1 d . . . . .
C32 C 0.44125(17) 0.35869(19) 0.14741(18) 0.0304(9) Uani 1 1 d . . . . .
H32A H 0.4522 0.3178 0.1655 0.036 Uiso 1 1 calc R U . . .
C33 C 0.48700(18) 0.3993(2) 0.1245(2) 0.0367(10) Uani 1 1 d . . . . .
H33A H 0.5287 0.3858 0.1269 0.044 Uiso 1 1 calc R U . . .
C34 C 0.47236(18) 0.4590(2) 0.09836(18) 0.0345(9) Uani 1 1 d . . . . .
H34A H 0.5037 0.4865 0.0823 0.041 Uiso 1 1 calc R U . . .
C35 C 0.41200(18) 0.4783(2) 0.09571(18) 0.0344(9) Uani 1 1 d . . . . .
H35A H 0.4016 0.5196 0.0783 0.041 Uiso 1 1 calc R U . . .
C36 C 0.36608(17) 0.43759(17) 0.11842(17) 0.0269(8) Uani 1 1 d . . . . .
H36A H 0.3246 0.4516 0.1161 0.032 Uiso 1 1 calc R U . . .
C37 C 0.33062(15) 0.33233(16) 0.25411(15) 0.0197(7) Uani 1 1 d . . . . .
C38 C 0.36222(18) 0.28756(19) 0.28982(16) 0.0315(9) Uani 1 1 d . . . . .
H38A H 0.3786 0.2487 0.2721 0.038 Uiso 1 1 calc R U . . .
C39 C 0.37021(19) 0.2989(2) 0.35132(17) 0.0372(10) Uani 1 1 d . . . . .
H39A H 0.3909 0.2669 0.3752 0.045 Uiso 1 1 calc R U . . .
C40 C 0.34865(17) 0.35575(19) 0.37815(16) 0.0289(8) Uani 1 1 d . . . . .
H40A H 0.3560 0.3644 0.4196 0.035 Uiso 1 1 calc R U . . .
C41 C 0.31599(17) 0.39989(18) 0.34304(16) 0.0275(8) Uani 1 1 d . . . . .
H41A H 0.2998 0.4388 0.3609 0.033 Uiso 1 1 calc R U . . .
C42 C 0.30662(16) 0.38815(16) 0.28224(15) 0.0218(7) Uani 1 1 d . . . . .
H42A H 0.2833 0.4188 0.2592 0.026 Uiso 1 1 calc R U . . .
C43 C 0.37389(15) 0.16507(15) 0.05579(14) 0.0176(7) Uani 1 1 d . . . . .
C44 C 0.36582(16) 0.09691(16) 0.05029(15) 0.0218(7) Uani 1 1 d . . . . .
H44A H 0.3300 0.0774 0.0670 0.026 Uiso 1 1 calc R U . . .
C45 C 0.40817(16) 0.05669(17) 0.02132(16) 0.0243(8) Uani 1 1 d . . . . .
H45A H 0.4010 0.0105 0.0188 0.029 Uiso 1 1 calc R U . . .
C46 C 0.46070(16) 0.08337(17) -0.00392(15) 0.0232(7) Uani 1 1 d . . . . .
H46A H 0.4889 0.0561 -0.0250 0.028 Uiso 1 1 calc R U . . .
C47 C 0.47155(16) 0.15014(18) 0.00200(16) 0.0247(7) Uani 1 1 d . . . . .
H47A H 0.5079 0.1690 -0.0141 0.030 Uiso 1 1 calc R U . . .
C48 C 0.42910(16) 0.18960(17) 0.03157(17) 0.0257(8) Uani 1 1 d . . . . .
H48A H 0.4377 0.2353 0.0357 0.031 Uiso 1 1 calc R U . . .
N1 N 0.49368(15) 0.03596(19) 0.20267(15) 0.0407(9) Uani 1 1 d . . . . .
C49 C 0.50720(19) 0.0397(2) 0.13538(18) 0.0419(11) Uani 1 1 d . . . . .
H49A H 0.4890 0.0007 0.1155 0.050 Uiso 1 1 calc R U . . .
H49B H 0.4868 0.0794 0.1187 0.050 Uiso 1 1 calc R U . . .
C50 C 0.5746(2) 0.0427(2) 0.1195(2) 0.0454(11) Uani 1 1 d . . . . .
H50A H 0.5792 0.0475 0.0757 0.068 Uiso 1 1 calc R U . . .
H50B H 0.5948 0.0020 0.1327 0.068 Uiso 1 1 calc R U . . .
H50C H 0.5935 0.0806 0.1398 0.068 Uiso 1 1 calc R U . . .
C51 C 0.5174(2) 0.0966(2) 0.2350(2) 0.0468(12) Uani 1 1 d . . . . .
H51A H 0.5625 0.0977 0.2309 0.056 Uiso 1 1 calc R U . . .
H51B H 0.5079 0.0920 0.2785 0.056 Uiso 1 1 calc R U . . .
C52 C 0.4918(3) 0.1622(3) 0.2132(2) 0.0631(16) Uani 1 1 d . . . . .
H52A H 0.5123 0.1984 0.2345 0.095 Uiso 1 1 calc R U . . .
H52B H 0.4476 0.1639 0.2212 0.095 Uiso 1 1 calc R U . . .
H52C H 0.4990 0.1665 0.1697 0.095 Uiso 1 1 calc R U . . .
C53 C 0.5251(2) -0.0229(2) 0.2312(2) 0.0468(11) Uani 1 1 d . . . . .
H53A H 0.5699 -0.0174 0.2264 0.056 Uiso 1 1 calc R U . . .
H53B H 0.5162 -0.0224 0.2750 0.056 Uiso 1 1 calc R U . . .
C54 C 0.5074(2) -0.0898(2) 0.2065(2) 0.0559(13) Uani 1 1 d . . . . .
H54A H 0.5338 -0.1237 0.2244 0.084 Uiso 1 1 calc R U . . .
H54B H 0.5126 -0.0900 0.1626 0.084 Uiso 1 1 calc R U . . .
H54C H 0.4645 -0.0991 0.2165 0.084 Uiso 1 1 calc R U . . .
C55 C 0.4238(2) 0.0300(3) 0.2067(2) 0.0535(13) Uani 1 1 d . . . . .
H55A H 0.4051 0.0675 0.1847 0.064 Uiso 1 1 calc R U . . .
H55B H 0.4110 -0.0111 0.1860 0.064 Uiso 1 1 calc R U . . .
C56 C 0.3987(3) 0.0291(3) 0.2702(2) 0.0733(17) Uani 1 1 d . . . . .
H56A H 0.3539 0.0252 0.2688 0.110 Uiso 1 1 calc R U . . .
H56B H 0.4100 0.0701 0.2908 0.110 Uiso 1 1 calc R U . . .
H56C H 0.4159 -0.0086 0.2921 0.110 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C1 1.959(4) . ?
W1 C3 1.964(4) . ?
W1 C2 1.975(3) . ?
W1 P1 2.5326(9) . ?
W1 P2 2.5430(9) . ?
W1 P3 2.5473(9) . ?
P1 C4 1.825(3) . ?
P1 C11 1.841(4) . ?
P1 C5 1.846(3) . ?
P2 C17 1.813(3) . ?
P2 C18 1.849(3) . ?
P2 C24 1.849(3) . ?
P3 C30 1.822(3) . ?
P3 C37 1.841(3) . ?
P3 C31 1.852(4) . ?
C1 O1 1.168(4) . ?
C2 O2 1.163(4) . ?
C3 O3 1.171(4) . ?
B1 C43 1.643(5) . ?
B1 C4 1.655(5) . ?
B1 C30 1.670(5) . ?
B1 C17 1.678(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.382(5) . ?
C5 C6 1.399(5) . ?
C6 C7 1.377(5) . ?
C6 H6A 0.9500 . ?
C7 C8 1.386(6) . ?
C7 H7A 0.9500 . ?
C8 C9 1.373(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.394(5) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C12 1.377(5) . ?
C11 C16 1.400(5) . ?
C12 C13 1.402(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.377(7) . ?
C13 H13A 0.9500 . ?
C14 C15 1.370(7) . ?
C14 H14A 0.9500 . ?
C15 C16 1.377(6) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C23 1.393(5) . ?
C18 C19 1.398(5) . ?
C19 C20 1.392(5) . ?
C19 H19A 0.9500 . ?
C20 C21 1.377(5) . ?
C20 H20A 0.9500 . ?
C21 C22 1.375(5) . ?
C21 H21A 0.9500 . ?
C22 C23 1.384(5) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 C29 1.384(5) . ?
C24 C25 1.390(5) . ?
C25 C26 1.390(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.378(6) . ?
C26 H26A 0.9500 . ?
C27 C28 1.375(6) . ?
C27 H27A 0.9500 . ?
C28 C29 1.386(5) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.393(5) . ?
C31 C36 1.396(5) . ?
C32 C33 1.389(5) . ?
C32 H32A 0.9500 . ?
C33 C34 1.379(6) . ?
C33 H33A 0.9500 . ?
C34 C35 1.374(5) . ?
C34 H34A 0.9500 . ?
C35 C36 1.391(5) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 C38 1.387(5) . ?
C37 C42 1.394(5) . ?
C38 C39 1.394(5) . ?
C38 H38A 0.9500 . ?
C39 C40 1.379(5) . ?
C39 H39A 0.9500 . ?
C40 C41 1.383(5) . ?
C40 H40A 0.9500 . ?
C41 C42 1.384(5) . ?
C41 H41A 0.9500 . ?
C42 H42A 0.9500 . ?
C43 C44 1.397(4) . ?
C43 C48 1.409(5) . ?
C44 C45 1.389(5) . ?
C44 H44A 0.9500 . ?
C45 C46 1.385(5) . ?
C45 H45A 0.9500 . ?
C46 C47 1.380(5) . ?
C46 H46A 0.9500 . ?
C47 C48 1.388(5) . ?
C47 H47A 0.9500 . ?
C48 H48A 0.9500 . ?
N1 C51 1.513(6) . ?
N1 C53 1.514(5) . ?
N1 C49 1.523(5) . ?
N1 C55 1.532(5) . ?
C49 C50 1.513(6) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.520(6) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.512(6) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.511(6) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?

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
C1 W1 C3 83.78(14) . . ?
C1 W1 C2 86.63(14) . . ?
C3 W1 C2 85.01(14) . . ?
C1 W1 P1 95.88(11) . . ?
C3 W1 P1 178.21(10) . . ?
C2 W1 P1 93.22(10) . . ?
C1 W1 P2 93.55(10) . . ?
C3 W1 P2 99.90(10) . . ?
C2 W1 P2 175.08(10) . . ?
P1 W1 P2 81.87(3) . . ?
C1 W1 P3 176.71(11) . . ?
C3 W1 P3 95.48(10) . . ?
C2 W1 P3 96.51(10) . . ?
P1 W1 P3 84.96(3) . . ?
P2 W1 P3 83.40(3) . . ?
C4 P1 C11 106.85(16) . . ?
C4 P1 C5 101.00(15) . . ?
C11 P1 C5 99.38(16) . . ?
C4 P1 W1 115.86(11) . . ?
C11 P1 W1 113.06(11) . . ?
C5 P1 W1 118.65(12) . . ?
C17 P2 C18 104.05(15) . . ?
C17 P2 C24 104.39(15) . . ?
C18 P2 C24 99.86(15) . . ?
C17 P2 W1 112.00(11) . . ?
C18 P2 W1 117.11(11) . . ?
C24 P2 W1 117.62(11) . . ?
C30 P3 C37 107.37(15) . . ?
C30 P3 C31 102.55(16) . . ?
C37 P3 C31 98.71(15) . . ?
C30 P3 W1 113.95(11) . . ?
C37 P3 W1 114.76(11) . . ?
C31 P3 W1 117.71(11) . . ?
O1 C1 W1 174.4(3) . . ?
O2 C2 W1 175.2(3) . . ?
O3 C3 W1 174.3(3) . . ?
C43 B1 C4 110.3(3) . . ?
C43 B1 C30 108.9(3) . . ?
C4 B1 C30 110.4(3) . . ?
C43 B1 C17 105.0(3) . . ?
C4 B1 C17 111.5(3) . . ?
C30 B1 C17 110.5(3) . . ?
B1 C4 P1 115.4(2) . . ?
B1 C4 H4A 108.4 . . ?
P1 C4 H4A 108.4 . . ?
B1 C4 H4B 108.4 . . ?
P1 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
C10 C5 C6 118.0(3) . . ?
C10 C5 P1 122.7(3) . . ?
C6 C5 P1 119.1(3) . . ?
C7 C6 C5 120.9(4) . . ?
C7 C6 H6A 119.6 . . ?
C5 C6 H6A 119.6 . . ?
C6 C7 C8 120.4(4) . . ?
C6 C7 H7A 119.8 . . ?
C8 C7 H7A 119.8 . . ?
C9 C8 C7 119.4(4) . . ?
C9 C8 H8A 120.3 . . ?
C7 C8 H8A 120.3 . . ?
C8 C9 C10 120.2(4) . . ?
C8 C9 H9A 119.9 . . ?
C10 C9 H9A 119.9 . . ?
C5 C10 C9 121.0(3) . . ?
C5 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C12 C11 C16 118.4(4) . . ?
C12 C11 P1 124.0(3) . . ?
C16 C11 P1 117.6(3) . . ?
C11 C12 C13 120.6(4) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13A 120.0 . . ?
C12 C13 H13A 120.0 . . ?
C15 C14 C13 119.6(4) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
C14 C15 C16 120.8(5) . . ?
C14 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C15 C16 C11 120.6(4) . . ?
C15 C16 H16A 119.7 . . ?
C11 C16 H16A 119.7 . . ?
B1 C17 P2 116.9(2) . . ?
B1 C17 H17A 108.1 . . ?
P2 C17 H17A 108.1 . . ?
B1 C17 H17B 108.1 . . ?
P2 C17 H17B 108.1 . . ?
H17A C17 H17B 107.3 . . ?
C23 C18 C19 117.4(3) . . ?
C23 C18 P2 119.3(3) . . ?
C19 C18 P2 123.3(3) . . ?
C20 C19 C18 121.1(3) . . ?
C20 C19 H19A 119.4 . . ?
C18 C19 H19A 119.4 . . ?
C21 C20 C19 120.1(3) . . ?
C21 C20 H20A 119.9 . . ?
C19 C20 H20A 119.9 . . ?
C22 C21 C20 119.5(3) . . ?
C22 C21 H21A 120.3 . . ?
C20 C21 H21A 120.3 . . ?
C21 C22 C23 120.7(4) . . ?
C21 C22 H22A 119.6 . . ?
C23 C22 H22A 119.6 . . ?
C22 C23 C18 121.1(3) . . ?
C22 C23 H23A 119.5 . . ?
C18 C23 H23A 119.5 . . ?
C29 C24 C25 118.2(3) . . ?
C29 C24 P2 120.9(3) . . ?
C25 C24 P2 120.9(3) . . ?
C26 C25 C24 120.9(4) . . ?
C26 C25 H25A 119.5 . . ?
C24 C25 H25A 119.5 . . ?
C27 C26 C25 119.9(4) . . ?
C27 C26 H26A 120.1 . . ?
C25 C26 H26A 120.1 . . ?
C28 C27 C26 119.9(4) . . ?
C28 C27 H27A 120.1 . . ?
C26 C27 H27A 120.1 . . ?
C27 C28 C29 120.1(4) . . ?
C27 C28 H28A 119.9 . . ?
C29 C28 H28A 119.9 . . ?
C24 C29 C28 121.1(4) . . ?
C24 C29 H29A 119.5 . . ?
C28 C29 H29A 119.5 . . ?
B1 C30 P3 113.9(2) . . ?
B1 C30 H30A 108.8 . . ?
P3 C30 H30A 108.8 . . ?
B1 C30 H30B 108.8 . . ?
P3 C30 H30B 108.8 . . ?
H30A C30 H30B 107.7 . . ?
C32 C31 C36 117.0(3) . . ?
C32 C31 P3 122.4(3) . . ?
C36 C31 P3 120.6(3) . . ?
C33 C32 C31 121.4(4) . . ?
C33 C32 H32A 119.3 . . ?
C31 C32 H32A 119.3 . . ?
C34 C33 C32 120.4(4) . . ?
C34 C33 H33A 119.8 . . ?
C32 C33 H33A 119.8 . . ?
C35 C34 C33 119.3(4) . . ?
C35 C34 H34A 120.3 . . ?
C33 C34 H34A 120.3 . . ?
C34 C35 C36 120.3(4) . . ?
C34 C35 H35A 119.8 . . ?
C36 C35 H35A 119.8 . . ?
C35 C36 C31 121.5(4) . . ?
C35 C36 H36A 119.3 . . ?
C31 C36 H36A 119.3 . . ?
C38 C37 C42 117.5(3) . . ?
C38 C37 P3 124.5(3) . . ?
C42 C37 P3 118.0(3) . . ?
C37 C38 C39 120.9(3) . . ?
C37 C38 H38A 119.6 . . ?
C39 C38 H38A 119.6 . . ?
C40 C39 C38 121.1(4) . . ?
C40 C39 H39A 119.4 . . ?
C38 C39 H39A 119.4 . . ?
C39 C40 C41 118.2(3) . . ?
C39 C40 H40A 120.9 . . ?
C41 C40 H40A 120.9 . . ?
C40 C41 C42 120.9(3) . . ?
C40 C41 H41A 119.6 . . ?
C42 C41 H41A 119.6 . . ?
C41 C42 C37 121.3(3) . . ?
C41 C42 H42A 119.3 . . ?
C37 C42 H42A 119.3 . . ?
C44 C43 C48 115.0(3) . . ?
C44 C43 B1 124.8(3) . . ?
C48 C43 B1 120.0(3) . . ?
C45 C44 C43 122.4(3) . . ?
C45 C44 H44A 118.8 . . ?
C43 C44 H44A 118.8 . . ?
C46 C45 C44 120.5(3) . . ?
C46 C45 H45A 119.7 . . ?
C44 C45 H45A 119.7 . . ?
C47 C46 C45 119.1(3) . . ?
C47 C46 H46A 120.5 . . ?
C45 C46 H46A 120.5 . . ?
C46 C47 C48 119.7(3) . . ?
C46 C47 H47A 120.1 . . ?
C48 C47 H47A 120.1 . . ?
C47 C48 C43 123.1(3) . . ?
C47 C48 H48A 118.4 . . ?
C43 C48 H48A 118.4 . . ?
C51 N1 C53 106.7(3) . . ?
C51 N1 C49 110.9(4) . . ?
C53 N1 C49 111.2(3) . . ?
C51 N1 C55 112.1(3) . . ?
C53 N1 C55 111.3(4) . . ?
C49 N1 C55 104.7(3) . . ?
C50 C49 N1 114.7(3) . . ?
C50 C49 H49A 108.6 . . ?
N1 C49 H49A 108.6 . . ?
C50 C49 H49B 108.6 . . ?
N1 C49 H49B 108.6 . . ?
H49A C49 H49B 107.6 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N1 C51 C52 115.7(4) . . ?
N1 C51 H51A 108.4 . . ?
C52 C51 H51A 108.4 . . ?
N1 C51 H51B 108.4 . . ?
C52 C51 H51B 108.4 . . ?
H51A C51 H51B 107.4 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 N1 116.1(4) . . ?
C54 C53 H53A 108.3 . . ?
N1 C53 H53A 108.3 . . ?
C54 C53 H53B 108.3 . . ?
N1 C53 H53B 108.3 . . ?
H53A C53 H53B 107.4 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C55 N1 114.5(4) . . ?
C56 C55 H55A 108.6 . . ?
N1 C55 H55A 108.6 . . ?
C56 C55 H55B 108.6 . . ?
N1 C55 H55B 108.6 . . ?
H55A C55 H55B 107.6 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

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
C43 B1 C4 P1 165.8(2) . . . . ?
C30 B1 C4 P1 45.4(3) . . . . ?
C17 B1 C4 P1 -77.8(3) . . . . ?
C11 P1 C4 B1 156.1(2) . . . . ?
C5 P1 C4 B1 -100.5(3) . . . . ?
W1 P1 C4 B1 29.1(3) . . . . ?
C4 P1 C5 C10 112.8(3) . . . . ?
C11 P1 C5 C10 -137.9(3) . . . . ?
W1 P1 C5 C10 -15.0(3) . . . . ?
C4 P1 C5 C6 -62.0(3) . . . . ?
C11 P1 C5 C6 47.4(3) . . . . ?
W1 P1 C5 C6 170.2(2) . . . . ?
C10 C5 C6 C7 -1.5(5) . . . . ?
P1 C5 C6 C7 173.4(3) . . . . ?
C5 C6 C7 C8 -0.4(6) . . . . ?
C6 C7 C8 C9 1.3(6) . . . . ?
C7 C8 C9 C10 -0.1(6) . . . . ?
C6 C5 C10 C9 2.7(5) . . . . ?
P1 C5 C10 C9 -172.1(3) . . . . ?
C8 C9 C10 C5 -1.9(6) . . . . ?
C4 P1 C11 C12 -12.7(4) . . . . ?
C5 P1 C11 C12 -117.3(3) . . . . ?
W1 P1 C11 C12 115.9(3) . . . . ?
C4 P1 C11 C16 168.2(3) . . . . ?
C5 P1 C11 C16 63.6(3) . . . . ?
W1 P1 C11 C16 -63.2(3) . . . . ?
C16 C11 C12 C13 0.3(6) . . . . ?
P1 C11 C12 C13 -178.7(3) . . . . ?
C11 C12 C13 C14 -1.1(7) . . . . ?
C12 C13 C14 C15 0.2(7) . . . . ?
C13 C14 C15 C16 1.3(8) . . . . ?
C14 C15 C16 C11 -2.1(8) . . . . ?
C12 C11 C16 C15 1.2(7) . . . . ?
P1 C11 C16 C15 -179.6(4) . . . . ?
C43 B1 C17 P2 157.4(2) . . . . ?
C4 B1 C17 P2 37.9(3) . . . . ?
C30 B1 C17 P2 -85.3(3) . . . . ?
C18 P2 C17 B1 -88.9(3) . . . . ?
C24 P2 C17 B1 166.9(2) . . . . ?
W1 P2 C17 B1 38.6(3) . . . . ?
C17 P2 C18 C23 175.3(3) . . . . ?
C24 P2 C18 C23 -77.1(3) . . . . ?
W1 P2 C18 C23 51.1(3) . . . . ?
C17 P2 C18 C19 -5.5(3) . . . . ?
C24 P2 C18 C19 102.2(3) . . . . ?
W1 P2 C18 C19 -129.7(3) . . . . ?
C23 C18 C19 C20 1.0(5) . . . . ?
P2 C18 C19 C20 -178.2(3) . . . . ?
C18 C19 C20 C21 -0.9(5) . . . . ?
C19 C20 C21 C22 0.0(6) . . . . ?
C20 C21 C22 C23 0.6(6) . . . . ?
C21 C22 C23 C18 -0.4(6) . . . . ?
C19 C18 C23 C22 -0.4(5) . . . . ?
P2 C18 C23 C22 178.9(3) . . . . ?
C17 P2 C24 C29 -155.4(3) . . . . ?
C18 P2 C24 C29 97.2(3) . . . . ?
W1 P2 C24 C29 -30.6(3) . . . . ?
C17 P2 C24 C25 21.3(3) . . . . ?
C18 P2 C24 C25 -86.1(3) . . . . ?
W1 P2 C24 C25 146.1(3) . . . . ?
C29 C24 C25 C26 1.1(6) . . . . ?
P2 C24 C25 C26 -175.7(3) . . . . ?
C24 C25 C26 C27 -0.9(6) . . . . ?
C25 C26 C27 C28 0.1(7) . . . . ?
C26 C27 C28 C29 0.6(6) . . . . ?
C25 C24 C29 C28 -0.4(5) . . . . ?
P2 C24 C29 C28 176.3(3) . . . . ?
C27 C28 C29 C24 -0.4(6) . . . . ?
C43 B1 C30 P3 151.4(2) . . . . ?
C4 B1 C30 P3 -87.3(3) . . . . ?
C17 B1 C30 P3 36.6(3) . . . . ?
C37 P3 C30 B1 167.3(2) . . . . ?
C31 P3 C30 B1 -89.3(3) . . . . ?
W1 P3 C30 B1 39.0(3) . . . . ?
C30 P3 C31 C32 -37.4(3) . . . . ?
C37 P3 C31 C32 72.7(3) . . . . ?
W1 P3 C31 C32 -163.4(3) . . . . ?
C30 P3 C31 C36 141.7(3) . . . . ?
C37 P3 C31 C36 -108.2(3) . . . . ?
W1 P3 C31 C36 15.8(3) . . . . ?
C36 C31 C32 C33 -1.0(5) . . . . ?
P3 C31 C32 C33 178.1(3) . . . . ?
C31 C32 C33 C34 0.3(6) . . . . ?
C32 C33 C34 C35 0.7(6) . . . . ?
C33 C34 C35 C36 -0.9(6) . . . . ?
C34 C35 C36 C31 0.2(6) . . . . ?
C32 C31 C36 C35 0.8(5) . . . . ?
P3 C31 C36 C35 -178.4(3) . . . . ?
C30 P3 C37 C38 7.0(4) . . . . ?
C31 P3 C37 C38 -99.2(3) . . . . ?
W1 P3 C37 C38 134.8(3) . . . . ?
C30 P3 C37 C42 -172.2(3) . . . . ?
C31 P3 C37 C42 81.7(3) . . . . ?
W1 P3 C37 C42 -44.4(3) . . . . ?
C42 C37 C38 C39 -0.9(6) . . . . ?
P3 C37 C38 C39 179.9(3) . . . . ?
C37 C38 C39 C40 -2.0(6) . . . . ?
C38 C39 C40 C41 3.3(6) . . . . ?
C39 C40 C41 C42 -1.7(6) . . . . ?
C40 C41 C42 C37 -1.2(6) . . . . ?
C38 C37 C42 C41 2.5(5) . . . . ?
P3 C37 C42 C41 -178.3(3) . . . . ?
C4 B1 C43 C44 -14.9(4) . . . . ?
C30 B1 C43 C44 106.5(4) . . . . ?
C17 B1 C43 C44 -135.2(3) . . . . ?
C4 B1 C43 C48 160.1(3) . . . . ?
C30 B1 C43 C48 -78.5(4) . . . . ?
C17 B1 C43 C48 39.8(4) . . . . ?
C48 C43 C44 C45 -2.0(5) . . . . ?
B1 C43 C44 C45 173.2(3) . . . . ?
C43 C44 C45 C46 -0.4(5) . . . . ?
C44 C45 C46 C47 2.4(5) . . . . ?
C45 C46 C47 C48 -1.7(5) . . . . ?
C46 C47 C48 C43 -0.9(6) . . . . ?
C44 C43 C48 C47 2.7(5) . . . . ?
B1 C43 C48 C47 -172.8(3) . . . . ?
C51 N1 C49 C50 61.6(5) . . . . ?
C53 N1 C49 C50 -56.9(5) . . . . ?
C55 N1 C49 C50 -177.2(4) . . . . ?
C53 N1 C51 C52 179.7(4) . . . . ?
C49 N1 C51 C52 58.5(5) . . . . ?
C55 N1 C51 C52 -58.1(5) . . . . ?
C51 N1 C53 C54 179.0(4) . . . . ?
C49 N1 C53 C54 -60.0(5) . . . . ?
C55 N1 C53 C54 56.3(5) . . . . ?
C51 N1 C55 C56 -56.5(6) . . . . ?
C53 N1 C55 C56 62.9(6) . . . . ?
C49 N1 C55 C56 -176.9(5) . . . . ?

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_site_symmetry_A
C23 H23A O1 0.95 2.59 3.417(4) 145.2 .
C54 H54B O1 0.98 2.60 3.230(5) 121.8 6_655

_refine_diff_density_max         2.196
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.105
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_14132a
_database_code_depnum_ccdc_archive 'CCDC 1039149'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        '[Et4N][Mo(CO)3(PhBP3)]'
_chemical_name_common            14132a
_chemical_melting_point          546-547
_chemical_formula_moiety         'C48 H41 B Mo O3 P3, C8 H20 N'
_chemical_formula_sum            'C56 H61 B Mo N O3 P3'
_chemical_formula_weight         995.71

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'
N N 0.0061 0.0033 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -z-1/2'

_cell_length_a                   21.795(2)
_cell_length_b                   20.281(2)
_cell_length_c                   22.166(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9798.3(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2930
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      27.41

_exptl_crystal_description       Needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_F_000             4160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.411
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7618
_exptl_absorpt_correction_T_max  0.9084
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'

_exptl_special_details           'Prof. P. Fischer'

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            109647
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.651
_diffrn_reflns_theta_max         27.451
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11192
_reflns_number_gt                8879
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/3 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0279P)²+9.9603P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11192
_refine_ls_number_parameters     590
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0326
_refine_ls_wR_factor_ref         0.0790
_refine_ls_wR_factor_gt          0.0711
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_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
Mo1 Mo 0.20777(2) 0.34668(2) 0.13868(2) 0.01346(5) Uani 1 1 d . . . . .
P1 P 0.19708(2) 0.22230(2) 0.13140(2) 0.01554(11) Uani 1 1 d . . . . .
P2 P 0.25360(2) 0.33098(2) 0.03362(2) 0.01479(10) Uani 1 1 d . . . . .
P3 P 0.31747(2) 0.32191(3) 0.17326(2) 0.01518(11) Uani 1 1 d . . . . .
C1 C 0.12586(10) 0.36745(11) 0.10817(9) 0.0211(4) Uani 1 1 d . . . . .
O1 O 0.07785(7) 0.38585(9) 0.09222(7) 0.0351(4) Uani 1 1 d . . . . .
C2 C 0.17041(9) 0.35119(10) 0.21941(9) 0.0194(4) Uani 1 1 d . . . . .
O2 O 0.14504(8) 0.35759(9) 0.26528(7) 0.0338(4) Uani 1 1 d . . . . .
C3 C 0.21390(9) 0.44294(10) 0.14651(9) 0.0195(4) Uani 1 1 d . . . . .
O3 O 0.21188(8) 0.49979(8) 0.15394(7) 0.0308(4) Uani 1 1 d . . . . .
B1 B 0.32274(10) 0.21680(11) 0.08300(10) 0.0156(4) Uani 1 1 d . . . . .
C4 C 0.25500(9) 0.18043(10) 0.08580(9) 0.0173(4) Uani 1 1 d . . . . .
H4A H 0.2606 0.1353 0.1019 0.021 Uiso 1 1 calc R U . . .
H4B H 0.2391 0.1762 0.0441 0.021 Uiso 1 1 calc R U . . .
C5 C 0.20014(9) 0.17320(10) 0.20147(9) 0.0186(4) Uani 1 1 d . . . . .
C6 C 0.18571(10) 0.10606(11) 0.19926(11) 0.0257(5) Uani 1 1 d . . . . .
H6A H 0.1704 0.0875 0.1629 0.031 Uiso 1 1 calc R U . . .
C7 C 0.19349(11) 0.06649(11) 0.24946(12) 0.0317(5) Uani 1 1 d . . . . .
H7A H 0.1832 0.0210 0.2474 0.038 Uiso 1 1 calc R U . . .
C8 C 0.21606(11) 0.09252(12) 0.30260(11) 0.0318(6) Uani 1 1 d . . . . .
H8A H 0.2222 0.0649 0.3367 0.038 Uiso 1 1 calc R U . . .
C9 C 0.22969(11) 0.15882(12) 0.30588(10) 0.0298(5) Uani 1 1 d . . . . .
H9A H 0.2449 0.1771 0.3424 0.036 Uiso 1 1 calc R U . . .
C10 C 0.22108(10) 0.19907(11) 0.25553(10) 0.0242(5) Uani 1 1 d . . . . .
H10A H 0.2297 0.2449 0.2584 0.029 Uiso 1 1 calc R U . . .
C11 C 0.12211(9) 0.19543(10) 0.10283(10) 0.0212(4) Uani 1 1 d . . . . .
C12 C 0.11344(11) 0.16192(12) 0.04900(11) 0.0319(5) Uani 1 1 d . . . . .
H12A H 0.1479 0.1508 0.0248 0.038 Uiso 1 1 calc R U . . .
C13 C 0.05474(12) 0.14437(14) 0.02991(13) 0.0418(7) Uani 1 1 d . . . . .
H13A H 0.0495 0.1217 -0.0073 0.050 Uiso 1 1 calc R U . . .
C14 C 0.00452(12) 0.15953(14) 0.06431(14) 0.0464(7) Uani 1 1 d . . . . .
H14A H -0.0354 0.1475 0.0511 0.056 Uiso 1 1 calc R U . . .
C15 C 0.01218(12) 0.19230(16) 0.11833(15) 0.0505(8) Uani 1 1 d . . . . .
H15A H -0.0224 0.2020 0.1429 0.061 Uiso 1 1 calc R U . . .
C16 C 0.07040(11) 0.21105(14) 0.13675(13) 0.0384(6) Uani 1 1 d . . . . .
H16A H 0.0751 0.2351 0.1733 0.046 Uiso 1 1 calc R U . . .
C17 C 0.32248(9) 0.28084(9) 0.03562(9) 0.0156(4) Uani 1 1 d . . . . .
H17A H 0.3300 0.2639 -0.0056 0.019 Uiso 1 1 calc R U . . .
H17B H 0.3574 0.3098 0.0462 0.019 Uiso 1 1 calc R U . . .
C18 C 0.20450(9) 0.29057(10) -0.02362(9) 0.0172(4) Uani 1 1 d . . . . .
C19 C 0.22463(10) 0.23818(10) -0.05942(9) 0.0204(4) Uani 1 1 d . . . . .
H19A H 0.2650 0.2214 -0.0541 0.024 Uiso 1 1 calc R U . . .
C20 C 0.18649(10) 0.21016(11) -0.10283(9) 0.0233(5) Uani 1 1 d . . . . .
H20A H 0.2010 0.1746 -0.1269 0.028 Uiso 1 1 calc R U . . .
C21 C 0.12774(10) 0.23386(11) -0.11099(10) 0.0265(5) Uani 1 1 d . . . . .
H21A H 0.1018 0.2149 -0.1407 0.032 Uiso 1 1 calc R U . . .
C22 C 0.10693(11) 0.28534(12) -0.07557(10) 0.0300(5) Uani 1 1 d . . . . .
H22A H 0.0664 0.3015 -0.0807 0.036 Uiso 1 1 calc R U . . .
C23 C 0.14508(10) 0.31348(11) -0.03249(10) 0.0247(5) Uani 1 1 d . . . . .
H23A H 0.1303 0.3490 -0.0087 0.030 Uiso 1 1 calc R U . . .
C24 C 0.27684(9) 0.40549(10) -0.00854(9) 0.0173(4) Uani 1 1 d . . . . .
C25 C 0.32681(10) 0.40458(11) -0.04733(10) 0.0258(5) Uani 1 1 d . . . . .
H25A H 0.3478 0.3643 -0.0546 0.031 Uiso 1 1 calc R U . . .
C26 C 0.34655(11) 0.46193(12) -0.07561(11) 0.0326(6) Uani 1 1 d . . . . .
H26A H 0.3814 0.4608 -0.1014 0.039 Uiso 1 1 calc R U . . .
C27 C 0.31581(12) 0.52060(12) -0.06642(11) 0.0321(5) Uani 1 1 d . . . . .
H27A H 0.3294 0.5598 -0.0856 0.039 Uiso 1 1 calc R U . . .
C28 C 0.26524(12) 0.52182(11) -0.02916(10) 0.0304(5) Uani 1 1 d . . . . .
H28A H 0.2436 0.5619 -0.0231 0.037 Uiso 1 1 calc R U . . .
C29 C 0.24573(11) 0.46467(11) -0.00034(9) 0.0240(5) Uani 1 1 d . . . . .
H29A H 0.2108 0.4661 0.0252 0.029 Uiso 1 1 calc R U . . .
C30 C 0.34490(9) 0.24010(10) 0.15200(9) 0.0162(4) Uani 1 1 d . . . . .
H30A H 0.3903 0.2397 0.1538 0.019 Uiso 1 1 calc R U . . .
H30B H 0.3296 0.2076 0.1817 0.019 Uiso 1 1 calc R U . . .
C31 C 0.37938(9) 0.37686(10) 0.14524(9) 0.0185(4) Uani 1 1 d . . . . .
C32 C 0.44094(10) 0.35916(11) 0.14837(10) 0.0260(5) Uani 1 1 d . . . . .
H32A H 0.4519 0.3184 0.1665 0.031 Uiso 1 1 calc R U . . .
C33 C 0.48675(11) 0.39977(12) 0.12551(12) 0.0326(6) Uani 1 1 d . . . . .
H33A H 0.5285 0.3867 0.1281 0.039 Uiso 1 1 calc R U . . .
C34 C 0.47142(11) 0.45932(12) 0.09891(11) 0.0306(5) Uani 1 1 d . . . . .
H34A H 0.5025 0.4869 0.0826 0.037 Uiso 1 1 calc R U . . .
C35 C 0.41085(11) 0.47830(12) 0.09622(11) 0.0296(5) Uani 1 1 d . . . . .
H35A H 0.4001 0.5194 0.0786 0.035 Uiso 1 1 calc R U . . .
C36 C 0.36532(10) 0.43732(11) 0.11920(10) 0.0246(5) Uani 1 1 d . . . . .
H36A H 0.3237 0.4510 0.1171 0.030 Uiso 1 1 calc R U . . .
C37 C 0.33057(9) 0.33156(10) 0.25490(9) 0.0171(4) Uani 1 1 d . . . . .
C38 C 0.36294(11) 0.28685(12) 0.29029(10) 0.0287(5) Uani 1 1 d . . . . .
H38A H 0.3793 0.2480 0.2725 0.034 Uiso 1 1 calc R U . . .
C39 C 0.37165(12) 0.29858(13) 0.35168(10) 0.0336(6) Uani 1 1 d . . . . .
H39A H 0.3932 0.2672 0.3754 0.040 Uiso 1 1 calc R U . . .
C40 C 0.34935(10) 0.35523(11) 0.37830(10) 0.0265(5) Uani 1 1 d . . . . .
H40A H 0.3568 0.3639 0.4198 0.032 Uiso 1 1 calc R U . . .
C41 C 0.31599(10) 0.39928(11) 0.34366(10) 0.0234(5) Uani 1 1 d . . . . .
H41A H 0.2997 0.4380 0.3616 0.028 Uiso 1 1 calc R U . . .
C42 C 0.30624(9) 0.38707(10) 0.28286(9) 0.0196(4) Uani 1 1 d . . . . .
H42A H 0.2825 0.4172 0.2599 0.023 Uiso 1 1 calc R U . . .
C43 C 0.37430(9) 0.16582(10) 0.05545(9) 0.0160(4) Uani 1 1 d . . . . .
C44 C 0.36643(9) 0.09743(10) 0.05082(9) 0.0178(4) Uani 1 1 d . . . . .
H44A H 0.3310 0.0779 0.0683 0.021 Uiso 1 1 calc R U . . .
C45 C 0.40873(9) 0.05698(10) 0.02155(9) 0.0203(4) Uani 1 1 d . . . . .
H45A H 0.4017 0.0108 0.0193 0.024 Uiso 1 1 calc R U . . .
C46 C 0.46078(9) 0.08355(10) -0.00423(9) 0.0201(4) Uani 1 1 d . . . . .
H46A H 0.4890 0.0562 -0.0252 0.024 Uiso 1 1 calc R U . . .
C47 C 0.47140(9) 0.15073(10) 0.00091(9) 0.0210(4) Uani 1 1 d . . . . .
H47A H 0.5074 0.1696 -0.0160 0.025 Uiso 1 1 calc R U . . .
C48 C 0.42927(9) 0.19027(10) 0.03082(10) 0.0211(4) Uani 1 1 d . . . . .
H48A H 0.4379 0.2360 0.0348 0.025 Uiso 1 1 calc R U . . .
N1 N 0.49644(9) 0.03958(12) 0.20211(9) 0.0360(5) Uani 1 1 d . . . . .
C49 C 0.50967(12) 0.04262(14) 0.13479(10) 0.0357(6) Uani 1 1 d . . . . .
H49A H 0.4907 0.0037 0.1153 0.043 Uiso 1 1 calc R U . . .
H49B H 0.4895 0.0823 0.1180 0.043 Uiso 1 1 calc R U . . .
C50 C 0.57655(12) 0.04451(14) 0.11805(12) 0.0374(6) Uani 1 1 d . . . . .
H50A H 0.5806 0.0501 0.0743 0.056 Uiso 1 1 calc R U . . .
H50B H 0.5962 0.0031 0.1302 0.056 Uiso 1 1 calc R U . . .
H50C H 0.5965 0.0815 0.1387 0.056 Uiso 1 1 calc R U . . .
C51 C 0.52121(13) 0.10017(14) 0.23402(12) 0.0420(7) Uani 1 1 d . . . . .
H51A H 0.5134 0.0955 0.2778 0.050 Uiso 1 1 calc R U . . .
H51B H 0.5662 0.1018 0.2282 0.050 Uiso 1 1 calc R U . . .
C52 C 0.49406(15) 0.16482(15) 0.21301(13) 0.0535(8) Uani 1 1 d . . . . .
H52A H 0.5137 0.2013 0.2346 0.080 Uiso 1 1 calc R U . . .
H52B H 0.4499 0.1652 0.2212 0.080 Uiso 1 1 calc R U . . .
H52C H 0.5010 0.1699 0.1696 0.080 Uiso 1 1 calc R U . . .
C53 C 0.52825(13) -0.01909(14) 0.23073(11) 0.0396(6) Uani 1 1 d . . . . .
H53A H 0.5731 -0.0136 0.2255 0.048 Uiso 1 1 calc R U . . .
H53B H 0.5197 -0.0185 0.2746 0.048 Uiso 1 1 calc R U . . .
C54 C 0.51020(14) -0.08592(15) 0.20627(13) 0.0484(7) Uani 1 1 d . . . . .
H54A H 0.5369 -0.1198 0.2237 0.073 Uiso 1 1 calc R U . . .
H54B H 0.5145 -0.0860 0.1623 0.073 Uiso 1 1 calc R U . . .
H54C H 0.4675 -0.0953 0.2170 0.073 Uiso 1 1 calc R U . . .
C55 C 0.42701(12) 0.03325(18) 0.20704(12) 0.0501(8) Uani 1 1 d . . . . .
H55A H 0.4080 0.0705 0.1851 0.060 Uiso 1 1 calc R U . . .
H55B H 0.4143 -0.0079 0.1866 0.060 Uiso 1 1 calc R U . . .
C56 C 0.40208(15) 0.0324(2) 0.27093(14) 0.0657(10) Uani 1 1 d . . . . .
H56A H 0.3574 0.0268 0.2698 0.099 Uiso 1 1 calc R U . . .
H56B H 0.4121 0.0741 0.2910 0.099 Uiso 1 1 calc R U . . .
H56C H 0.4206 -0.0043 0.2933 0.099 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C1 1.955(2) . ?
Mo1 C3 1.965(2) . ?
Mo1 C2 1.968(2) . ?
Mo1 P1 2.5385(6) . ?
Mo1 P2 2.5539(6) . ?
Mo1 P3 2.5607(6) . ?
P1 C4 1.827(2) . ?
P1 C11 1.835(2) . ?
P1 C5 1.846(2) . ?
P2 C17 1.814(2) . ?
P2 C24 1.848(2) . ?
P2 C18 1.851(2) . ?
P3 C30 1.826(2) . ?
P3 C37 1.842(2) . ?
P3 C31 1.857(2) . ?
C1 O1 1.166(3) . ?
C2 O2 1.165(2) . ?
C3 O3 1.165(3) . ?
B1 C43 1.645(3) . ?
B1 C4 1.652(3) . ?
B1 C17 1.670(3) . ?
B1 C30 1.672(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.386(3) . ?
C5 C6 1.398(3) . ?
C6 C7 1.382(3) . ?
C6 H6A 0.9500 . ?
C7 C8 1.381(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.379(3) . ?
C8 H8A 0.9500 . ?
C9 C10 1.395(3) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C12 1.386(3) . ?
C11 C16 1.391(3) . ?
C12 C13 1.394(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.369(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.380(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.386(4) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C23 1.390(3) . ?
C18 C19 1.397(3) . ?
C19 C20 1.393(3) . ?
C19 H19A 0.9500 . ?
C20 C21 1.380(3) . ?
C20 H20A 0.9500 . ?
C21 C22 1.383(3) . ?
C21 H21A 0.9500 . ?
C22 C23 1.389(3) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 C25 1.388(3) . ?
C24 C29 1.390(3) . ?
C25 C26 1.390(3) . ?
C25 H25A 0.9500 . ?
C26 C27 1.381(3) . ?
C26 H26A 0.9500 . ?
C27 C28 1.378(3) . ?
C27 H27A 0.9500 . ?
C28 C29 1.390(3) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C36 1.390(3) . ?
C31 C32 1.391(3) . ?
C32 C33 1.390(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.385(3) . ?
C33 H33A 0.9500 . ?
C34 C35 1.376(3) . ?
C34 H34A 0.9500 . ?
C35 C36 1.391(3) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 C42 1.390(3) . ?
C37 C38 1.391(3) . ?
C38 C39 1.394(3) . ?
C38 H38A 0.9500 . ?
C39 C40 1.380(3) . ?
C39 H39A 0.9500 . ?
C40 C41 1.384(3) . ?
C40 H40A 0.9500 . ?
C41 C42 1.387(3) . ?
C41 H41A 0.9500 . ?
C42 H42A 0.9500 . ?
C43 C44 1.401(3) . ?
C43 C48 1.407(3) . ?
C44 C45 1.394(3) . ?
C44 H44A 0.9500 . ?
C45 C46 1.380(3) . ?
C45 H45A 0.9500 . ?
C46 C47 1.387(3) . ?
C46 H46A 0.9500 . ?
C47 C48 1.388(3) . ?
C47 H47A 0.9500 . ?
C48 H48A 0.9500 . ?
N1 C53 1.516(3) . ?
N1 C51 1.517(3) . ?
N1 C49 1.521(3) . ?
N1 C55 1.523(3) . ?
C49 C50 1.505(3) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.512(4) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.512(4) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.517(4) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?

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
C1 Mo1 C3 83.02(9) . . ?
C1 Mo1 C2 85.80(8) . . ?
C3 Mo1 C2 84.35(8) . . ?
C1 Mo1 P1 96.22(6) . . ?
C3 Mo1 P1 178.03(6) . . ?
C2 Mo1 P1 93.79(6) . . ?
C1 Mo1 P2 93.93(6) . . ?
C3 Mo1 P2 100.24(6) . . ?
C2 Mo1 P2 175.33(6) . . ?
P1 Mo1 P2 81.607(17) . . ?
C1 Mo1 P3 176.88(6) . . ?
C3 Mo1 P3 96.02(6) . . ?
C2 Mo1 P3 97.08(6) . . ?
P1 Mo1 P3 84.825(17) . . ?
P2 Mo1 P3 83.299(18) . . ?
C4 P1 C11 106.64(10) . . ?
C4 P1 C5 100.94(9) . . ?
C11 P1 C5 99.34(9) . . ?
C4 P1 Mo1 115.71(7) . . ?
C11 P1 Mo1 113.50(7) . . ?
C5 P1 Mo1 118.64(7) . . ?
C17 P2 C24 104.12(9) . . ?
C17 P2 C18 104.30(9) . . ?
C24 P2 C18 100.02(9) . . ?
C17 P2 Mo1 111.79(6) . . ?
C24 P2 Mo1 117.80(7) . . ?
C18 P2 Mo1 117.01(7) . . ?
C30 P3 C37 107.42(9) . . ?
C30 P3 C31 102.78(9) . . ?
C37 P3 C31 98.76(9) . . ?
C30 P3 Mo1 114.00(7) . . ?
C37 P3 Mo1 114.70(7) . . ?
C31 P3 Mo1 117.43(7) . . ?
O1 C1 Mo1 173.47(19) . . ?
O2 C2 Mo1 174.48(18) . . ?
O3 C3 Mo1 173.21(19) . . ?
C43 B1 C4 110.13(16) . . ?
C43 B1 C17 104.93(15) . . ?
C4 B1 C17 111.59(16) . . ?
C43 B1 C30 108.65(16) . . ?
C4 B1 C30 110.49(16) . . ?
C17 B1 C30 110.87(16) . . ?
B1 C4 P1 115.53(13) . . ?
B1 C4 H4A 108.4 . . ?
P1 C4 H4A 108.4 . . ?
B1 C4 H4B 108.4 . . ?
P1 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
C10 C5 C6 118.2(2) . . ?
C10 C5 P1 122.36(16) . . ?
C6 C5 P1 119.19(16) . . ?
C7 C6 C5 120.6(2) . . ?
C7 C6 H6A 119.7 . . ?
C5 C6 H6A 119.7 . . ?
C8 C7 C6 120.6(2) . . ?
C8 C7 H7A 119.7 . . ?
C6 C7 H7A 119.7 . . ?
C9 C8 C7 119.6(2) . . ?
C9 C8 H8A 120.2 . . ?
C7 C8 H8A 120.2 . . ?
C8 C9 C10 119.9(2) . . ?
C8 C9 H9A 120.0 . . ?
C10 C9 H9A 120.0 . . ?
C5 C10 C9 121.0(2) . . ?
C5 C10 H10A 119.5 . . ?
C9 C10 H10A 119.5 . . ?
C12 C11 C16 117.8(2) . . ?
C12 C11 P1 124.33(17) . . ?
C16 C11 P1 117.85(18) . . ?
C11 C12 C13 120.8(2) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C14 C13 C12 120.5(3) . . ?
C14 C13 H13A 119.8 . . ?
C12 C13 H13A 119.8 . . ?
C13 C14 C15 119.7(2) . . ?
C13 C14 H14A 120.2 . . ?
C15 C14 H14A 120.2 . . ?
C14 C15 C16 119.9(3) . . ?
C14 C15 H15A 120.1 . . ?
C16 C15 H15A 120.1 . . ?
C15 C16 C11 121.3(3) . . ?
C15 C16 H16A 119.3 . . ?
C11 C16 H16A 119.3 . . ?
B1 C17 P2 117.01(13) . . ?
B1 C17 H17A 108.0 . . ?
P2 C17 H17A 108.0 . . ?
B1 C17 H17B 108.0 . . ?
P2 C17 H17B 108.0 . . ?
H17A C17 H17B 107.3 . . ?
C23 C18 C19 117.82(19) . . ?
C23 C18 P2 119.18(15) . . ?
C19 C18 P2 123.00(16) . . ?
C20 C19 C18 121.0(2) . . ?
C20 C19 H19A 119.5 . . ?
C18 C19 H19A 119.5 . . ?
C21 C20 C19 120.1(2) . . ?
C21 C20 H20A 119.9 . . ?
C19 C20 H20A 119.9 . . ?
C20 C21 C22 119.5(2) . . ?
C20 C21 H21A 120.2 . . ?
C22 C21 H21A 120.2 . . ?
C21 C22 C23 120.3(2) . . ?
C21 C22 H22A 119.9 . . ?
C23 C22 H22A 119.9 . . ?
C22 C23 C18 121.2(2) . . ?
C22 C23 H23A 119.4 . . ?
C18 C23 H23A 119.4 . . ?
C25 C24 C29 118.38(19) . . ?
C25 C24 P2 121.17(16) . . ?
C29 C24 P2 120.41(16) . . ?
C24 C25 C26 120.8(2) . . ?
C24 C25 H25A 119.6 . . ?
C26 C25 H25A 119.6 . . ?
C27 C26 C25 120.3(2) . . ?
C27 C26 H26A 119.9 . . ?
C25 C26 H26A 119.9 . . ?
C28 C27 C26 119.5(2) . . ?
C28 C27 H27A 120.3 . . ?
C26 C27 H27A 120.3 . . ?
C27 C28 C29 120.3(2) . . ?
C27 C28 H28A 119.8 . . ?
C29 C28 H28A 119.8 . . ?
C28 C29 C24 120.7(2) . . ?
C28 C29 H29A 119.6 . . ?
C24 C29 H29A 119.6 . . ?
B1 C30 P3 113.48(13) . . ?
B1 C30 H30A 108.9 . . ?
P3 C30 H30A 108.9 . . ?
B1 C30 H30B 108.9 . . ?
P3 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C36 C31 C32 117.5(2) . . ?
C36 C31 P3 120.55(16) . . ?
C32 C31 P3 121.97(16) . . ?
C33 C32 C31 121.5(2) . . ?
C33 C32 H32A 119.3 . . ?
C31 C32 H32A 119.3 . . ?
C34 C33 C32 119.9(2) . . ?
C34 C33 H33A 120.0 . . ?
C32 C33 H33A 120.0 . . ?
C35 C34 C33 119.6(2) . . ?
C35 C34 H34A 120.2 . . ?
C33 C34 H34A 120.2 . . ?
C34 C35 C36 120.1(2) . . ?
C34 C35 H35A 120.0 . . ?
C36 C35 H35A 120.0 . . ?
C31 C36 C35 121.5(2) . . ?
C31 C36 H36A 119.3 . . ?
C35 C36 H36A 119.3 . . ?
C42 C37 C38 118.04(19) . . ?
C42 C37 P3 117.70(15) . . ?
C38 C37 P3 124.27(16) . . ?
C37 C38 C39 120.5(2) . . ?
C37 C38 H38A 119.7 . . ?
C39 C38 H38A 119.7 . . ?
C40 C39 C38 120.8(2) . . ?
C40 C39 H39A 119.6 . . ?
C38 C39 H39A 119.6 . . ?
C39 C40 C41 119.0(2) . . ?
C39 C40 H40A 120.5 . . ?
C41 C40 H40A 120.5 . . ?
C40 C41 C42 120.3(2) . . ?
C40 C41 H41A 119.9 . . ?
C42 C41 H41A 119.9 . . ?
C41 C42 C37 121.3(2) . . ?
C41 C42 H42A 119.4 . . ?
C37 C42 H42A 119.4 . . ?
C44 C43 C48 115.13(18) . . ?
C44 C43 B1 124.45(17) . . ?
C48 C43 B1 120.30(17) . . ?
C45 C44 C43 122.38(19) . . ?
C45 C44 H44A 118.8 . . ?
C43 C44 H44A 118.8 . . ?
C46 C45 C44 120.44(19) . . ?
C46 C45 H45A 119.8 . . ?
C44 C45 H45A 119.8 . . ?
C45 C46 C47 119.13(19) . . ?
C45 C46 H46A 120.4 . . ?
C47 C46 H46A 120.4 . . ?
C46 C47 C48 119.78(19) . . ?
C46 C47 H47A 120.1 . . ?
C48 C47 H47A 120.1 . . ?
C47 C48 C43 123.04(19) . . ?
C47 C48 H48A 118.5 . . ?
C43 C48 H48A 118.5 . . ?
C53 N1 C51 106.13(18) . . ?
C53 N1 C49 110.82(19) . . ?
C51 N1 C49 110.9(2) . . ?
C53 N1 C55 111.0(2) . . ?
C51 N1 C55 112.9(2) . . ?
C49 N1 C55 105.20(18) . . ?
C50 C49 N1 115.3(2) . . ?
C50 C49 H49A 108.5 . . ?
N1 C49 H49A 108.5 . . ?
C50 C49 H49B 108.5 . . ?
N1 C49 H49B 108.5 . . ?
H49A C49 H49B 107.5 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C52 C51 N1 114.8(2) . . ?
C52 C51 H51A 108.6 . . ?
N1 C51 H51A 108.6 . . ?
C52 C51 H51B 108.6 . . ?
N1 C51 H51B 108.6 . . ?
H51A C51 H51B 107.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 N1 115.8(2) . . ?
C54 C53 H53A 108.3 . . ?
N1 C53 H53A 108.3 . . ?
C54 C53 H53B 108.3 . . ?
N1 C53 H53B 108.3 . . ?
H53A C53 H53B 107.4 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C55 N1 115.1(2) . . ?
C56 C55 H55A 108.5 . . ?
N1 C55 H55A 108.5 . . ?
C56 C55 H55B 108.5 . . ?
N1 C55 H55B 108.5 . . ?
H55A C55 H55B 107.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

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
C43 B1 C4 P1 165.89(13) . . . . ?
C17 B1 C4 P1 -77.99(18) . . . . ?
C30 B1 C4 P1 45.9(2) . . . . ?
C11 P1 C4 B1 156.38(14) . . . . ?
C5 P1 C4 B1 -100.31(15) . . . . ?
Mo1 P1 C4 B1 29.10(16) . . . . ?
C4 P1 C5 C10 113.10(18) . . . . ?
C11 P1 C5 C10 -137.79(18) . . . . ?
Mo1 P1 C5 C10 -14.4(2) . . . . ?
C4 P1 C5 C6 -61.48(18) . . . . ?
C11 P1 C5 C6 47.63(18) . . . . ?
Mo1 P1 C5 C6 171.01(14) . . . . ?
C10 C5 C6 C7 -1.4(3) . . . . ?
P1 C5 C6 C7 173.43(17) . . . . ?
C5 C6 C7 C8 -0.4(4) . . . . ?
C6 C7 C8 C9 1.4(4) . . . . ?
C7 C8 C9 C10 -0.5(4) . . . . ?
C6 C5 C10 C9 2.3(3) . . . . ?
P1 C5 C10 C9 -172.35(17) . . . . ?
C8 C9 C10 C5 -1.4(3) . . . . ?
C4 P1 C11 C12 -12.8(2) . . . . ?
C5 P1 C11 C12 -117.3(2) . . . . ?
Mo1 P1 C11 C12 115.80(19) . . . . ?
C4 P1 C11 C16 168.78(18) . . . . ?
C5 P1 C11 C16 64.3(2) . . . . ?
Mo1 P1 C11 C16 -62.6(2) . . . . ?
C16 C11 C12 C13 -0.3(4) . . . . ?
P1 C11 C12 C13 -178.72(19) . . . . ?
C11 C12 C13 C14 -0.5(4) . . . . ?
C12 C13 C14 C15 -0.1(4) . . . . ?
C13 C14 C15 C16 1.5(4) . . . . ?
C14 C15 C16 C11 -2.4(4) . . . . ?
C12 C11 C16 C15 1.7(4) . . . . ?
P1 C11 C16 C15 -179.8(2) . . . . ?
C43 B1 C17 P2 156.92(13) . . . . ?
C4 B1 C17 P2 37.7(2) . . . . ?
C30 B1 C17 P2 -85.96(18) . . . . ?
C24 P2 C17 B1 167.14(14) . . . . ?
C18 P2 C17 B1 -88.43(15) . . . . ?
Mo1 P2 C17 B1 38.92(15) . . . . ?
C17 P2 C18 C23 174.19(17) . . . . ?
C24 P2 C18 C23 -78.30(18) . . . . ?
Mo1 P2 C18 C23 50.14(18) . . . . ?
C17 P2 C18 C19 -6.75(19) . . . . ?
C24 P2 C18 C19 100.75(18) . . . . ?
Mo1 P2 C18 C19 -130.81(15) . . . . ?
C23 C18 C19 C20 0.4(3) . . . . ?
P2 C18 C19 C20 -178.65(16) . . . . ?
C18 C19 C20 C21 -0.2(3) . . . . ?
C19 C20 C21 C22 -0.3(3) . . . . ?
C20 C21 C22 C23 0.7(4) . . . . ?
C21 C22 C23 C18 -0.4(4) . . . . ?
C19 C18 C23 C22 -0.1(3) . . . . ?
P2 C18 C23 C22 179.01(18) . . . . ?
C17 P2 C24 C25 22.2(2) . . . . ?
C18 P2 C24 C25 -85.44(19) . . . . ?
Mo1 P2 C24 C25 146.64(16) . . . . ?
C17 P2 C24 C29 -155.46(17) . . . . ?
C18 P2 C24 C29 96.89(18) . . . . ?
Mo1 P2 C24 C29 -31.03(19) . . . . ?
C29 C24 C25 C26 2.2(3) . . . . ?
P2 C24 C25 C26 -175.49(18) . . . . ?
C24 C25 C26 C27 -1.3(4) . . . . ?
C25 C26 C27 C28 -0.3(4) . . . . ?
C26 C27 C28 C29 0.9(4) . . . . ?
C27 C28 C29 C24 0.1(4) . . . . ?
C25 C24 C29 C28 -1.6(3) . . . . ?
P2 C24 C29 C28 176.13(17) . . . . ?
C43 B1 C30 P3 151.48(14) . . . . ?
C4 B1 C30 P3 -87.60(17) . . . . ?
C17 B1 C30 P3 36.7(2) . . . . ?
C37 P3 C30 B1 167.35(13) . . . . ?
C31 P3 C30 B1 -89.07(15) . . . . ?
Mo1 P3 C30 B1 39.10(15) . . . . ?
C30 P3 C31 C36 141.22(17) . . . . ?
C37 P3 C31 C36 -108.57(18) . . . . ?
Mo1 P3 C31 C36 15.23(19) . . . . ?
C30 P3 C31 C32 -37.67(19) . . . . ?
C37 P3 C31 C32 72.54(19) . . . . ?
Mo1 P3 C31 C32 -163.67(15) . . . . ?
C36 C31 C32 C33 -1.0(3) . . . . ?
P3 C31 C32 C33 177.92(18) . . . . ?
C31 C32 C33 C34 0.0(4) . . . . ?
C32 C33 C34 C35 1.0(4) . . . . ?
C33 C34 C35 C36 -1.1(4) . . . . ?
C32 C31 C36 C35 1.0(3) . . . . ?
P3 C31 C36 C35 -177.96(17) . . . . ?
C34 C35 C36 C31 0.0(4) . . . . ?
C30 P3 C37 C42 -172.14(16) . . . . ?
C31 P3 C37 C42 81.43(17) . . . . ?
Mo1 P3 C37 C42 -44.29(18) . . . . ?
C30 P3 C37 C38 7.6(2) . . . . ?
C31 P3 C37 C38 -98.8(2) . . . . ?
Mo1 P3 C37 C38 135.44(18) . . . . ?
C42 C37 C38 C39 -1.4(3) . . . . ?
P3 C37 C38 C39 178.86(19) . . . . ?
C37 C38 C39 C40 -1.2(4) . . . . ?
C38 C39 C40 C41 2.5(4) . . . . ?
C39 C40 C41 C42 -1.2(3) . . . . ?
C40 C41 C42 C37 -1.4(3) . . . . ?
C38 C37 C42 C41 2.7(3) . . . . ?
P3 C37 C42 C41 -177.53(16) . . . . ?
C4 B1 C43 C44 -16.2(3) . . . . ?
C17 B1 C43 C44 -136.45(19) . . . . ?
C30 B1 C43 C44 104.9(2) . . . . ?
C4 B1 C43 C48 159.56(18) . . . . ?
C17 B1 C43 C48 39.3(2) . . . . ?
C30 B1 C43 C48 -79.3(2) . . . . ?
C48 C43 C44 C45 -2.7(3) . . . . ?
B1 C43 C44 C45 173.25(18) . . . . ?
C43 C44 C45 C46 0.1(3) . . . . ?
C44 C45 C46 C47 1.9(3) . . . . ?
C45 C46 C47 C48 -1.1(3) . . . . ?
C46 C47 C48 C43 -1.7(3) . . . . ?
C44 C43 C48 C47 3.6(3) . . . . ?
B1 C43 C48 C47 -172.59(19) . . . . ?
C53 N1 C49 C50 -56.1(3) . . . . ?
C51 N1 C49 C50 61.5(3) . . . . ?
C55 N1 C49 C50 -176.1(2) . . . . ?
C53 N1 C51 C52 -178.7(2) . . . . ?
C49 N1 C51 C52 60.9(3) . . . . ?
C55 N1 C51 C52 -56.9(3) . . . . ?
C51 N1 C53 C54 179.5(2) . . . . ?
C49 N1 C53 C54 -60.0(3) . . . . ?
C55 N1 C53 C54 56.5(3) . . . . ?
C53 N1 C55 C56 62.7(3) . . . . ?
C51 N1 C55 C56 -56.3(4) . . . . ?
C49 N1 C55 C56 -177.4(3) . . . . ?

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_site_symmetry_A
C23 H23A O1 0.95 2.62 3.456(3) 147.0 .
C54 H54B O1 0.98 2.61 3.225(3) 121.3 6_655

_refine_diff_density_max         0.449
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.068
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH3CN/Et2O'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_14143zzz
_database_code_depnum_ccdc_archive 'CCDC 1039150'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        '[Et4N][W(CO)3{6-(PhBP3)Mo(CO)3}]'
_chemical_name_common            14143zzz
_chemical_melting_point          493-494
_chemical_formula_moiety         'C51 H45 B Mo N O6 P3 W, C8 H16 N, C4 H8 O'
_chemical_formula_sum            'C63 H69 B Mo N O7 P3 W'
_chemical_formula_weight         1335.70

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'
N N 0.0061 0.0033 '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'
B B 0.0013 0.0007 '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'
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                   12.2758(11)
_cell_length_b                   33.375(3)
_cell_length_c                   14.5010(13)
_cell_angle_alpha                90
_cell_angle_beta                 92.090(1)
_cell_angle_gamma                90
_cell_volume                     5937.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2760
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      27.39

_exptl_crystal_description       Plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_F_000             2704
_exptl_transmission_factor_min   0.4056
_exptl_transmission_factor_max   0.4915
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.281
_shelx_estimated_absorpt_T_min   0.462
_shelx_estimated_absorpt_T_max   0.741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4056
_exptl_absorpt_correction_T_max  0.4915
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'

_exptl_special_details           'Prof. P. Fischer'

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56403
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.532
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13612
_reflns_number_gt                10948
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.500 360 88 ' '
2 0.106 0.002 0.968 16 1 ' '
3 0.501 1.000 1.000 359 88 ' '
4 0.400 0.503 0.532 15 1 ' '
5 0.607 0.497 0.466 13 1 ' '
6 0.893 -0.003 0.034 13 1 ' '
_platon_squeeze_details          
;

 PLATON/SQUEEZE applied to treat appareent THF/DEE compositional disorder
 PLATON/SQUEEZE RESULTS Summary and Remarks :N = NOTE, W = WARNING, E = ERROR
 ============================================================================

 N: No S.U.'s (esd) on observed/calculated parameters.
 ---------------------------------------------------------------------------
 N: Number of moved primary input atoms: ................................ 104
 N: Total Potential Solvent Accessible Void Vol ..............   781.6 Ang^3
 N: Electron Count / Cell = 179 - To be included in D(calc), F000 & Mol.Wght.

 ============================================================================

 empirical formula assumes 100% THF
 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0398P)²+1.3094P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13612
_refine_ls_number_parameters     653
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0837
_refine_ls_wR_factor_gt          0.0799
_refine_ls_goodness_of_fit_ref   1.080
_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
Mo1 Mo 0.34162(2) 0.67853(2) 0.02295(2) 0.01677(6) Uani 1 1 d . . . . .
C1 C 0.4939(3) 0.69446(10) 0.0481(2) 0.0274(7) Uani 1 1 d . . . . .
O1 O 0.58119(18) 0.70775(8) 0.05996(19) 0.0408(7) Uani 1 1 d . . . . .
C2 C 0.3686(2) 0.69455(9) -0.1039(2) 0.0245(7) Uani 1 1 d . . . . .
O2 O 0.3902(2) 0.70531(8) -0.17725(18) 0.0399(6) Uani 1 1 d . . . . .
C3 C 0.3110(2) 0.73520(10) 0.0479(2) 0.0253(7) Uani 1 1 d . . . . .
O3 O 0.29882(19) 0.76942(7) 0.05813(19) 0.0382(6) Uani 1 1 d . . . . .
C4 C 0.3000(2) 0.57002(9) 0.0589(2) 0.0197(6) Uani 1 1 d . . . . .
H4A H 0.2882 0.5449 0.0236 0.024 Uiso 1 1 calc R U . . .
H4B H 0.3454 0.5634 0.1147 0.024 Uiso 1 1 calc R U . . .
C5 C 0.5202(2) 0.59014(10) -0.0001(2) 0.0218(7) Uani 1 1 d . . . . .
C6 C 0.5950(3) 0.61361(10) -0.0469(3) 0.0290(8) Uani 1 1 d . . . . .
H6A H 0.5694 0.6351 -0.0848 0.035 Uiso 1 1 calc R U . . .
C7 C 0.7056(3) 0.60583(11) -0.0387(3) 0.0379(9) Uani 1 1 d . . . . .
H7A H 0.7554 0.6216 -0.0718 0.045 Uiso 1 1 calc R U . . .
C8 C 0.7436(3) 0.57506(11) 0.0179(3) 0.0385(9) Uani 1 1 d . . . . .
H8A H 0.8197 0.5704 0.0259 0.046 Uiso 1 1 calc R U . . .
C9 C 0.6708(3) 0.55132(11) 0.0625(3) 0.0371(9) Uani 1 1 d . . . . .
H9A H 0.6967 0.5297 0.0997 0.045 Uiso 1 1 calc R U . . .
C10 C 0.5591(3) 0.55874(10) 0.0534(3) 0.0320(8) Uani 1 1 d . . . . .
H10A H 0.5094 0.5421 0.0844 0.038 Uiso 1 1 calc R U . . .
C11 C 0.3438(2) 0.58589(9) -0.1294(2) 0.0202(6) Uani 1 1 d . . . . .
C12 C 0.2742(2) 0.60643(10) -0.1908(2) 0.0235(7) Uani 1 1 d . . . . .
H12A H 0.2490 0.6324 -0.1749 0.028 Uiso 1 1 calc R U . . .
C13 C 0.2407(3) 0.58957(10) -0.2751(2) 0.0274(7) Uani 1 1 d . . . . .
H13A H 0.1913 0.6036 -0.3154 0.033 Uiso 1 1 calc R U . . .
C14 C 0.2798(3) 0.55213(10) -0.3001(2) 0.0316(8) Uani 1 1 d . . . . .
H14A H 0.2570 0.5404 -0.3573 0.038 Uiso 1 1 calc R U . . .
C15 C 0.3516(3) 0.53225(11) -0.2412(3) 0.0375(9) Uani 1 1 d . . . . .
H15A H 0.3798 0.5070 -0.2586 0.045 Uiso 1 1 calc R U . . .
C16 C 0.3832(3) 0.54864(10) -0.1573(2) 0.0307(8) Uani 1 1 d . . . . .
H16A H 0.4326 0.5344 -0.1175 0.037 Uiso 1 1 calc R U . . .
P1 P 0.37612(6) 0.60503(2) -0.01217(6) 0.01904(17) Uani 1 1 d . . . . .
C17 C 0.1936(2) 0.61668(9) 0.1828(2) 0.0200(6) Uani 1 1 d . . . . .
H17A H 0.1993 0.5999 0.2391 0.024 Uiso 1 1 calc R U . . .
H17B H 0.1264 0.6329 0.1864 0.024 Uiso 1 1 calc R U . . .
C18 C 0.4225(3) 0.62135(10) 0.2404(2) 0.0297(8) Uani 1 1 d . . . . .
C19 C 0.5286(3) 0.62959(15) 0.2204(3) 0.0511(12) Uani 1 1 d . . . . .
H19A H 0.5434 0.6503 0.1776 0.061 Uiso 1 1 calc R U . . .
C20 C 0.6155(4) 0.60812(19) 0.2616(3) 0.0686(16) Uani 1 1 d . . . . .
H20A H 0.6883 0.6147 0.2476 0.082 Uiso 1 1 calc R U . . .
C21 C 0.5960(4) 0.57813(15) 0.3210(4) 0.0651(16) Uani 1 1 d . . . . .
H21A H 0.6549 0.5633 0.3482 0.078 Uiso 1 1 calc R U . . .
C22 C 0.4903(5) 0.56907(13) 0.3422(4) 0.0738(18) Uani 1 1 d . . . . .
H22A H 0.4763 0.5480 0.3841 0.089 Uiso 1 1 calc R U . . .
C23 C 0.4037(3) 0.59088(12) 0.3021(3) 0.0551(13) Uani 1 1 d . . . . .
H23A H 0.3310 0.5847 0.3175 0.066 Uiso 1 1 calc R U . . .
C24 C 0.2846(2) 0.68726(10) 0.2746(2) 0.0229(7) Uani 1 1 d . . . . .
C25 C 0.3438(3) 0.72277(10) 0.2769(2) 0.0294(8) Uani 1 1 d . . . . .
H25A H 0.3983 0.7269 0.2330 0.035 Uiso 1 1 calc R U . . .
C26 C 0.3251(3) 0.75208(11) 0.3414(3) 0.0354(9) Uani 1 1 d . . . . .
H26A H 0.3684 0.7757 0.3427 0.043 Uiso 1 1 calc R U . . .
C27 C 0.2450(3) 0.74755(11) 0.4034(3) 0.0352(9) Uani 1 1 d . . . . .
H27A H 0.2301 0.7682 0.4461 0.042 Uiso 1 1 calc R U . . .
P2 P 0.30975(6) 0.65047(2) 0.18337(6) 0.02000(17) Uani 1 1 d . . . . .
C28 C 0.1853(3) 0.71169(12) 0.4029(3) 0.0416(10) Uani 1 1 d . . . . .
H28A H 0.1303 0.7078 0.4464 0.050 Uiso 1 1 calc R U . . .
C29 C 0.2058(3) 0.68237(11) 0.3399(2) 0.0351(9) Uani 1 1 d . . . . .
H29A H 0.1652 0.6581 0.3409 0.042 Uiso 1 1 calc R U . . .
C30 C 0.1093(2) 0.60878(9) 0.0049(2) 0.0200(6) Uani 1 1 d . . . . .
H30A H 0.0304 0.6061 0.0158 0.024 Uiso 1 1 calc R U . . .
H30B H 0.1241 0.5946 -0.0533 0.024 Uiso 1 1 calc R U . . .
C31 C 0.0388(2) 0.68588(9) 0.0625(2) 0.0199(6) Uani 1 1 d . . . . .
C32 C 0.0693(2) 0.71209(9) 0.1336(2) 0.0241(7) Uani 1 1 d . . . . .
H32A H 0.1438 0.7191 0.1435 0.029 Uiso 1 1 calc R U . . .
C33 C -0.0090(3) 0.72795(10) 0.1900(2) 0.0297(8) Uani 1 1 d . . . . .
H33A H 0.0127 0.7452 0.2396 0.036 Uiso 1 1 calc R U . . .
C34 C -0.1183(3) 0.71891(11) 0.1749(3) 0.0358(9) Uani 1 1 d . . . . .
H34A H -0.1716 0.7301 0.2133 0.043 Uiso 1 1 calc R U . . .
C35 C -0.1492(3) 0.69353(11) 0.1034(3) 0.0359(9) Uani 1 1 d . . . . .
H35A H -0.2240 0.6873 0.0925 0.043 Uiso 1 1 calc R U . . .
C36 C -0.0719(3) 0.67722(10) 0.0478(2) 0.0294(8) Uani 1 1 d . . . . .
H36A H -0.0942 0.6598 -0.0012 0.035 Uiso 1 1 calc R U . . .
C37 C 0.0895(2) 0.67658(9) -0.1250(2) 0.0197(6) Uani 1 1 d . . . . .
C38 C 0.1236(2) 0.71344(9) -0.1599(2) 0.0249(7) Uani 1 1 d . . . . .
H38A H 0.1683 0.7305 -0.1221 0.030 Uiso 1 1 calc R U . . .
C39 C 0.0932(3) 0.72534(10) -0.2485(2) 0.0301(8) Uani 1 1 d . . . . .
H39A H 0.1174 0.7504 -0.2710 0.036 Uiso 1 1 calc R U . . .
C40 C 0.0284(3) 0.70119(11) -0.3043(2) 0.0322(8) Uani 1 1 d . . . . .
H40A H 0.0092 0.7092 -0.3656 0.039 Uiso 1 1 calc R U . . .
C41 C -0.0087(3) 0.66510(11) -0.2702(2) 0.0315(8) Uani 1 1 d . . . . .
H41A H -0.0552 0.6486 -0.3078 0.038 Uiso 1 1 calc R U . . .
C42 C 0.0221(3) 0.65281(10) -0.1809(2) 0.0257(7) Uani 1 1 d . . . . .
H42A H -0.0035 0.6279 -0.1582 0.031 Uiso 1 1 calc R U . . .
P3 P 0.14164(6) 0.66190(2) -0.00893(6) 0.01743(16) Uani 1 1 d . . . . .
B1 B 0.1802(3) 0.58658(10) 0.0919(2) 0.0181(7) Uani 1 1 d . . . . .
C43 C 0.1041(2) 0.54850(9) 0.1217(2) 0.0201(6) Uani 1 1 d . . . . .
C44 C 0.0244(2) 0.55263(10) 0.1893(2) 0.0266(7) Uani 1 1 d . . . . .
H44A H 0.0187 0.5776 0.2201 0.032 Uiso 1 1 calc R U . . .
C45 C -0.0477(3) 0.52112(11) 0.2136(3) 0.0314(8) Uani 1 1 d . . . . .
H45A H -0.1008 0.5255 0.2585 0.038 Uiso 1 1 calc R U . . .
C46 C -0.0398(3) 0.48393(11) 0.1710(2) 0.0285(8) Uani 1 1 d . . . . .
H46A H -0.0865 0.4626 0.1876 0.034 Uiso 1 1 calc R U . . .
C47 C 0.0379(3) 0.47807(10) 0.1033(2) 0.0274(7) Uani 1 1 d . . . . .
H47A H 0.0426 0.4530 0.0728 0.033 Uiso 1 1 calc R U . . .
C48 C 0.1086(3) 0.50958(9) 0.0809(2) 0.0239(7) Uani 1 1 d . . . . .
H48A H 0.1619 0.5047 0.0365 0.029 Uiso 1 1 calc R U . . .
W1 W 0.13468(2) 0.49802(2) 0.23810(2) 0.02454(5) Uani 1 1 d . . . . .
C49 C 0.1451(3) 0.44548(12) 0.2960(3) 0.0413(10) Uani 1 1 d . . . . .
O4 O 0.1526(3) 0.41407(9) 0.3298(2) 0.0662(10) Uani 1 1 d . . . . .
C50 C 0.2919(3) 0.49346(11) 0.2197(3) 0.0352(9) Uani 1 1 d . . . . .
O5 O 0.3838(2) 0.49086(9) 0.2065(2) 0.0522(8) Uani 1 1 d . . . . .
C51 C 0.1748(3) 0.52060(13) 0.3582(3) 0.0441(10) Uani 1 1 d . . . . .
O6 O 0.2016(3) 0.53414(12) 0.4298(2) 0.0794(11) Uani 1 1 d . . . . .
N1 N 0.4658(2) 0.35342(9) 0.4089(2) 0.0343(7) Uani 1 1 d . . . . .
C52 C 0.5853(3) 0.36336(14) 0.4281(3) 0.0572(12) Uani 1 1 d . . . . .
H52A H 0.6041 0.3866 0.3894 0.069 Uiso 1 1 calc R U . . .
H52B H 0.5944 0.3718 0.4933 0.069 Uiso 1 1 calc R U . . .
C53 C 0.6654(4) 0.33073(15) 0.4112(4) 0.0702(15) Uani 1 1 d . . . . .
H53A H 0.7377 0.3389 0.4351 0.105 Uiso 1 1 calc R U . . .
H53B H 0.6681 0.3256 0.3448 0.105 Uiso 1 1 calc R U . . .
H53C H 0.6429 0.3063 0.4427 0.105 Uiso 1 1 calc R U . . .
C54 C 0.4504(4) 0.34387(17) 0.3053(3) 0.0639(14) Uani 1 1 d . . . . .
H54A H 0.4795 0.3666 0.2699 0.077 Uiso 1 1 calc R U . . .
H54B H 0.4950 0.3200 0.2916 0.077 Uiso 1 1 calc R U . . .
C55 C 0.3367(4) 0.33612(18) 0.2712(3) 0.0716(16) Uani 1 1 d . . . . .
H55A H 0.3374 0.3249 0.2088 0.107 Uiso 1 1 calc R U . . .
H55B H 0.2956 0.3613 0.2699 0.107 Uiso 1 1 calc R U . . .
H55C H 0.3020 0.3171 0.3124 0.107 Uiso 1 1 calc R U . . .
C56 C 0.3957(4) 0.38708(14) 0.4340(3) 0.0598(13) Uani 1 1 d . . . . .
H56A H 0.4020 0.3903 0.5018 0.072 Uiso 1 1 calc R U . . .
H56B H 0.3193 0.3793 0.4185 0.072 Uiso 1 1 calc R U . . .
C57 C 0.4147(4) 0.42705(15) 0.3920(5) 0.0859(19) Uani 1 1 d . . . . .
H57A H 0.3603 0.4461 0.4132 0.129 Uiso 1 1 calc R U . . .
H57B H 0.4085 0.4249 0.3246 0.129 Uiso 1 1 calc R U . . .
H57C H 0.4879 0.4365 0.4104 0.129 Uiso 1 1 calc R U . . .
C58 C 0.4347(4) 0.31567(14) 0.4603(3) 0.0581(12) Uani 1 1 d . . . . .
H58A H 0.3555 0.3112 0.4498 0.070 Uiso 1 1 calc R U . . .
H58B H 0.4730 0.2927 0.4329 0.070 Uiso 1 1 calc R U . . .
C59 C 0.4587(5) 0.31561(16) 0.5597(3) 0.0711(15) Uani 1 1 d . . . . .
H59A H 0.4189 0.2937 0.5884 0.107 Uiso 1 1 calc R U . . .
H59B H 0.4362 0.3412 0.5860 0.107 Uiso 1 1 calc R U . . .
H59C H 0.5372 0.3119 0.5715 0.107 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C2 1.955(4) . ?
Mo1 C3 1.965(3) . ?
Mo1 C1 1.965(3) . ?
Mo1 P3 2.5429(8) . ?
Mo1 P1 2.5441(8) . ?
Mo1 P2 2.5511(9) . ?
C1 O1 1.166(4) . ?
C2 O2 1.163(4) . ?
C3 O3 1.162(4) . ?
C4 B1 1.658(4) . ?
C4 P1 1.836(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.379(5) . ?
C5 C6 1.401(4) . ?
C5 P1 1.839(3) . ?
C6 C7 1.384(5) . ?
C6 H6A 0.9500 . ?
C7 C8 1.385(5) . ?
C7 H7A 0.9500 . ?
C8 C9 1.373(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.395(4) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C12 1.392(4) . ?
C11 C16 1.398(4) . ?
C11 P1 1.846(3) . ?
C12 C13 1.395(5) . ?
C12 H12A 0.9500 . ?
C13 C14 1.391(5) . ?
C13 H13A 0.9500 . ?
C14 C15 1.376(5) . ?
C14 H14A 0.9500 . ?
C15 C16 1.377(5) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 B1 1.660(5) . ?
C17 P2 1.818(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.372(5) . ?
C18 C23 1.379(5) . ?
C18 P2 1.861(3) . ?
C19 C20 1.401(6) . ?
C19 H19A 0.9500 . ?
C20 C21 1.348(7) . ?
C20 H20A 0.9500 . ?
C21 C22 1.378(7) . ?
C21 H21A 0.9500 . ?
C22 C23 1.398(6) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 C29 1.388(5) . ?
C24 C25 1.390(4) . ?
C24 P2 1.840(3) . ?
C25 C26 1.379(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.365(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.403(5) . ?
C27 H27A 0.9500 . ?
C28 C29 1.368(5) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 B1 1.679(4) . ?
C30 P3 1.830(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.393(4) . ?
C31 C36 1.397(4) . ?
C31 P3 1.845(3) . ?
C32 C33 1.390(4) . ?
C32 H32A 0.9500 . ?
C33 C34 1.386(5) . ?
C33 H33A 0.9500 . ?
C34 C35 1.381(5) . ?
C34 H34A 0.9500 . ?
C35 C36 1.380(5) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 C42 1.386(4) . ?
C37 C38 1.400(4) . ?
C37 P3 1.846(3) . ?
C38 C39 1.383(5) . ?
C38 H38A 0.9500 . ?
C39 C40 1.376(5) . ?
C39 H39A 0.9500 . ?
C40 C41 1.385(5) . ?
C40 H40A 0.9500 . ?
C41 C42 1.398(5) . ?
C41 H41A 0.9500 . ?
C42 H42A 0.9500 . ?
B1 C43 1.644(4) . ?
C43 C44 1.417(4) . ?
C43 C48 1.429(4) . ?
C43 W1 2.405(3) . ?
C44 C45 1.426(4) . ?
C44 W1 2.363(3) . ?
C44 H44A 0.9500 . ?
C45 C46 1.391(5) . ?
C45 W1 2.382(3) . ?
C45 H45A 0.9500 . ?
C46 C47 1.407(5) . ?
C46 W1 2.367(3) . ?
C46 H46A 0.9500 . ?
C47 C48 1.409(4) . ?
C47 W1 2.347(3) . ?
C47 H47A 0.9500 . ?
C48 W1 2.322(3) . ?
C48 H48A 0.9500 . ?
W1 C51 1.945(4) . ?
W1 C49 1.946(4) . ?
W1 C50 1.964(4) . ?
C49 O4 1.159(4) . ?
C50 O5 1.155(5) . ?
C51 O6 1.169(5) . ?
N1 C56 1.469(5) . ?
N1 C52 1.519(5) . ?
N1 C58 1.520(5) . ?
N1 C54 1.541(5) . ?
C52 C53 1.493(6) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.487(6) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 C57 1.489(6) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C59 1.461(6) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?

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 Mo1 C3 87.15(14) . . ?
C2 Mo1 C1 84.70(14) . . ?
C3 Mo1 C1 83.85(13) . . ?
C2 Mo1 P3 94.83(9) . . ?
C3 Mo1 P3 93.06(9) . . ?
C1 Mo1 P3 176.89(10) . . ?
C2 Mo1 P1 92.31(9) . . ?
C3 Mo1 P1 178.32(9) . . ?
C1 Mo1 P1 97.69(10) . . ?
P3 Mo1 P1 85.40(3) . . ?
C2 Mo1 P2 174.29(9) . . ?
C3 Mo1 P2 98.55(10) . . ?
C1 Mo1 P2 96.14(11) . . ?
P3 Mo1 P2 84.63(3) . . ?
P1 Mo1 P2 81.99(3) . . ?
O1 C1 Mo1 173.1(3) . . ?
O2 C2 Mo1 175.9(3) . . ?
O3 C3 Mo1 174.9(3) . . ?
B1 C4 P1 115.1(2) . . ?
B1 C4 H4A 108.5 . . ?
P1 C4 H4A 108.5 . . ?
B1 C4 H4B 108.5 . . ?
P1 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
C10 C5 C6 118.6(3) . . ?
C10 C5 P1 124.8(2) . . ?
C6 C5 P1 116.6(2) . . ?
C7 C6 C5 120.8(3) . . ?
C7 C6 H6A 119.6 . . ?
C5 C6 H6A 119.6 . . ?
C6 C7 C8 119.9(3) . . ?
C6 C7 H7A 120.1 . . ?
C8 C7 H7A 120.1 . . ?
C9 C8 C7 119.7(3) . . ?
C9 C8 H8A 120.1 . . ?
C7 C8 H8A 120.1 . . ?
C8 C9 C10 120.5(3) . . ?
C8 C9 H9A 119.7 . . ?
C10 C9 H9A 119.7 . . ?
C5 C10 C9 120.4(3) . . ?
C5 C10 H10A 119.8 . . ?
C9 C10 H10A 119.8 . . ?
C12 C11 C16 117.7(3) . . ?
C12 C11 P1 121.6(2) . . ?
C16 C11 P1 120.6(2) . . ?
C11 C12 C13 121.1(3) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C14 C13 C12 119.8(3) . . ?
C14 C13 H13A 120.1 . . ?
C12 C13 H13A 120.1 . . ?
C15 C14 C13 119.4(3) . . ?
C15 C14 H14A 120.3 . . ?
C13 C14 H14A 120.3 . . ?
C14 C15 C16 120.7(3) . . ?
C14 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C15 C16 C11 121.3(3) . . ?
C15 C16 H16A 119.4 . . ?
C11 C16 H16A 119.4 . . ?
C4 P1 C5 106.39(14) . . ?
C4 P1 C11 101.56(14) . . ?
C5 P1 C11 99.62(14) . . ?
C4 P1 Mo1 114.18(10) . . ?
C5 P1 Mo1 114.08(10) . . ?
C11 P1 Mo1 119.10(10) . . ?
B1 C17 P2 115.7(2) . . ?
B1 C17 H17A 108.3 . . ?
P2 C17 H17A 108.3 . . ?
B1 C17 H17B 108.3 . . ?
P2 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C19 C18 C23 117.9(3) . . ?
C19 C18 P2 119.8(3) . . ?
C23 C18 P2 122.2(3) . . ?
C18 C19 C20 121.4(5) . . ?
C18 C19 H19A 119.3 . . ?
C20 C19 H19A 119.3 . . ?
C21 C20 C19 120.2(5) . . ?
C21 C20 H20A 119.9 . . ?
C19 C20 H20A 119.9 . . ?
C20 C21 C22 119.7(4) . . ?
C20 C21 H21A 120.1 . . ?
C22 C21 H21A 120.1 . . ?
C21 C22 C23 120.1(5) . . ?
C21 C22 H22A 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C18 C23 C22 120.7(4) . . ?
C18 C23 H23A 119.7 . . ?
C22 C23 H23A 119.7 . . ?
C29 C24 C25 117.5(3) . . ?
C29 C24 P2 123.5(3) . . ?
C25 C24 P2 119.0(2) . . ?
C26 C25 C24 121.4(3) . . ?
C26 C25 H25A 119.3 . . ?
C24 C25 H25A 119.3 . . ?
C27 C26 C25 120.7(3) . . ?
C27 C26 H26A 119.6 . . ?
C25 C26 H26A 119.6 . . ?
C26 C27 C28 118.6(3) . . ?
C26 C27 H27A 120.7 . . ?
C28 C27 H27A 120.7 . . ?
C17 P2 C24 105.39(14) . . ?
C17 P2 C18 104.42(15) . . ?
C24 P2 C18 99.83(15) . . ?
C17 P2 Mo1 111.70(11) . . ?
C24 P2 Mo1 116.50(11) . . ?
C18 P2 Mo1 117.42(12) . . ?
C29 C28 C27 120.3(3) . . ?
C29 C28 H28A 119.8 . . ?
C27 C28 H28A 119.8 . . ?
C28 C29 C24 121.4(3) . . ?
C28 C29 H29A 119.3 . . ?
C24 C29 H29A 119.3 . . ?
B1 C30 P3 113.6(2) . . ?
B1 C30 H30A 108.8 . . ?
P3 C30 H30A 108.8 . . ?
B1 C30 H30B 108.8 . . ?
P3 C30 H30B 108.8 . . ?
H30A C30 H30B 107.7 . . ?
C32 C31 C36 118.5(3) . . ?
C32 C31 P3 121.1(2) . . ?
C36 C31 P3 120.4(2) . . ?
C33 C32 C31 120.1(3) . . ?
C33 C32 H32A 119.9 . . ?
C31 C32 H32A 119.9 . . ?
C34 C33 C32 120.7(3) . . ?
C34 C33 H33A 119.7 . . ?
C32 C33 H33A 119.7 . . ?
C35 C34 C33 119.3(3) . . ?
C35 C34 H34A 120.3 . . ?
C33 C34 H34A 120.3 . . ?
C36 C35 C34 120.4(3) . . ?
C36 C35 H35A 119.8 . . ?
C34 C35 H35A 119.8 . . ?
C35 C36 C31 121.0(3) . . ?
C35 C36 H36A 119.5 . . ?
C31 C36 H36A 119.5 . . ?
C42 C37 C38 118.2(3) . . ?
C42 C37 P3 124.1(2) . . ?
C38 C37 P3 117.6(2) . . ?
C39 C38 C37 120.9(3) . . ?
C39 C38 H38A 119.6 . . ?
C37 C38 H38A 119.6 . . ?
C40 C39 C38 120.6(3) . . ?
C40 C39 H39A 119.7 . . ?
C38 C39 H39A 119.7 . . ?
C39 C40 C41 119.3(3) . . ?
C39 C40 H40A 120.3 . . ?
C41 C40 H40A 120.3 . . ?
C40 C41 C42 120.3(3) . . ?
C40 C41 H41A 119.8 . . ?
C42 C41 H41A 119.8 . . ?
C37 C42 C41 120.6(3) . . ?
C37 C42 H42A 119.7 . . ?
C41 C42 H42A 119.7 . . ?
C30 P3 C31 101.72(14) . . ?
C30 P3 C37 106.70(14) . . ?
C31 P3 C37 100.07(14) . . ?
C30 P3 Mo1 113.82(10) . . ?
C31 P3 Mo1 118.65(10) . . ?
C37 P3 Mo1 114.12(10) . . ?
C43 B1 C4 109.7(2) . . ?
C43 B1 C17 107.5(3) . . ?
C4 B1 C17 111.6(2) . . ?
C43 B1 C30 104.7(2) . . ?
C4 B1 C30 111.8(3) . . ?
C17 B1 C30 111.3(2) . . ?
C44 C43 C48 114.4(3) . . ?
C44 C43 B1 121.3(3) . . ?
C48 C43 B1 124.3(3) . . ?
C44 C43 W1 71.11(18) . . ?
C48 C43 W1 69.27(18) . . ?
B1 C43 W1 130.55(19) . . ?
C43 C44 C45 123.3(3) . . ?
C43 C44 W1 74.34(18) . . ?
C45 C44 W1 73.22(19) . . ?
C43 C44 H44A 118.4 . . ?
C45 C44 H44A 118.4 . . ?
W1 C44 H44A 126.0 . . ?
C46 C45 C44 119.7(3) . . ?
C46 C45 W1 72.37(19) . . ?
C44 C45 W1 71.79(18) . . ?
C46 C45 H45A 120.2 . . ?
C44 C45 H45A 120.2 . . ?
W1 C45 H45A 127.7 . . ?
C45 C46 C47 119.6(3) . . ?
C45 C46 W1 73.56(19) . . ?
C47 C46 W1 71.86(19) . . ?
C45 C46 H46A 120.2 . . ?
C47 C46 H46A 120.2 . . ?
W1 C46 H46A 126.2 . . ?
C46 C47 C48 119.7(3) . . ?
C46 C47 W1 73.42(19) . . ?
C48 C47 W1 71.49(19) . . ?
C46 C47 H47A 120.1 . . ?
C48 C47 H47A 120.1 . . ?
W1 C47 H47A 126.9 . . ?
C47 C48 C43 123.4(3) . . ?
C47 C48 W1 73.39(19) . . ?
C43 C48 W1 75.59(18) . . ?
C47 C48 H48A 118.3 . . ?
C43 C48 H48A 118.3 . . ?
W1 C48 H48A 124.3 . . ?
C51 W1 C49 87.27(18) . . ?
C51 W1 C50 86.17(17) . . ?
C49 W1 C50 86.51(16) . . ?
C51 W1 C48 146.72(15) . . ?
C49 W1 C48 125.28(15) . . ?
C50 W1 C48 88.91(14) . . ?
C51 W1 C47 163.76(15) . . ?
C49 W1 C47 97.30(14) . . ?
C50 W1 C47 109.60(15) . . ?
C48 W1 C47 35.12(11) . . ?
C51 W1 C44 95.33(16) . . ?
C49 W1 C44 148.43(14) . . ?
C50 W1 C44 125.04(13) . . ?
C48 W1 C44 61.38(12) . . ?
C47 W1 C44 72.69(12) . . ?
C51 W1 C46 129.88(15) . . ?
C49 W1 C46 92.45(14) . . ?
C50 W1 C46 143.88(15) . . ?
C48 W1 C46 62.55(11) . . ?
C47 W1 C46 34.72(11) . . ?
C44 W1 C46 61.99(12) . . ?
C51 W1 C45 102.39(15) . . ?
C49 W1 C45 113.76(14) . . ?
C50 W1 C45 158.08(14) . . ?
C48 W1 C45 72.79(12) . . ?
C47 W1 C45 61.49(12) . . ?
C44 W1 C45 34.99(11) . . ?
C46 W1 C45 34.07(12) . . ?
C51 W1 C43 112.65(15) . . ?
C49 W1 C43 160.07(14) . . ?
C50 W1 C43 95.06(13) . . ?
C48 W1 C43 35.14(11) . . ?
C47 W1 C43 63.43(10) . . ?
C44 W1 C43 34.56(11) . . ?
C46 W1 C43 74.62(11) . . ?
C45 W1 C43 63.02(11) . . ?
O4 C49 W1 179.0(4) . . ?
O5 C50 W1 178.2(4) . . ?
O6 C51 W1 178.3(4) . . ?
C56 N1 C52 111.0(3) . . ?
C56 N1 C58 110.6(3) . . ?
C52 N1 C58 110.5(3) . . ?
C56 N1 C54 110.3(3) . . ?
C52 N1 C54 107.9(3) . . ?
C58 N1 C54 106.4(3) . . ?
C53 C52 N1 116.6(4) . . ?
C53 C52 H52A 108.1 . . ?
N1 C52 H52A 108.1 . . ?
C53 C52 H52B 108.1 . . ?
N1 C52 H52B 108.1 . . ?
H52A C52 H52B 107.3 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C55 C54 N1 116.1(4) . . ?
C55 C54 H54A 108.3 . . ?
N1 C54 H54A 108.3 . . ?
C55 C54 H54B 108.3 . . ?
N1 C54 H54B 108.3 . . ?
H54A C54 H54B 107.4 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N1 C56 C57 118.8(4) . . ?
N1 C56 H56A 107.6 . . ?
C57 C56 H56A 107.6 . . ?
N1 C56 H56B 107.6 . . ?
C57 C56 H56B 107.6 . . ?
H56A C56 H56B 107.0 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C59 C58 N1 116.1(4) . . ?
C59 C58 H58A 108.3 . . ?
N1 C58 H58A 108.3 . . ?
C59 C58 H58B 108.3 . . ?
N1 C58 H58B 108.3 . . ?
H58A C58 H58B 107.4 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?

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
C10 C5 C6 C7 -0.8(5) . . . . ?
P1 C5 C6 C7 177.1(3) . . . . ?
C5 C6 C7 C8 -1.4(6) . . . . ?
C6 C7 C8 C9 2.8(6) . . . . ?
C7 C8 C9 C10 -2.0(6) . . . . ?
C6 C5 C10 C9 1.6(5) . . . . ?
P1 C5 C10 C9 -176.1(3) . . . . ?
C8 C9 C10 C5 -0.2(6) . . . . ?
C16 C11 C12 C13 3.0(5) . . . . ?
P1 C11 C12 C13 -172.7(2) . . . . ?
C11 C12 C13 C14 -1.9(5) . . . . ?
C12 C13 C14 C15 -0.3(5) . . . . ?
C13 C14 C15 C16 1.4(6) . . . . ?
C14 C15 C16 C11 -0.3(6) . . . . ?
C12 C11 C16 C15 -1.9(5) . . . . ?
P1 C11 C16 C15 173.9(3) . . . . ?
B1 C4 P1 C5 157.6(2) . . . . ?
B1 C4 P1 C11 -98.6(2) . . . . ?
B1 C4 P1 Mo1 30.8(2) . . . . ?
C10 C5 P1 C4 -0.5(3) . . . . ?
C6 C5 P1 C4 -178.3(3) . . . . ?
C10 C5 P1 C11 -105.7(3) . . . . ?
C6 C5 P1 C11 76.5(3) . . . . ?
C10 C5 P1 Mo1 126.3(3) . . . . ?
C6 C5 P1 Mo1 -51.5(3) . . . . ?
C12 C11 P1 C4 107.7(3) . . . . ?
C16 C11 P1 C4 -67.9(3) . . . . ?
C12 C11 P1 C5 -143.2(3) . . . . ?
C16 C11 P1 C5 41.2(3) . . . . ?
C12 C11 P1 Mo1 -18.6(3) . . . . ?
C16 C11 P1 Mo1 165.8(2) . . . . ?
C23 C18 C19 C20 -0.6(6) . . . . ?
P2 C18 C19 C20 -179.6(3) . . . . ?
C18 C19 C20 C21 1.3(7) . . . . ?
C19 C20 C21 C22 -1.0(7) . . . . ?
C20 C21 C22 C23 0.1(7) . . . . ?
C19 C18 C23 C22 -0.4(6) . . . . ?
P2 C18 C23 C22 178.7(3) . . . . ?
C21 C22 C23 C18 0.7(7) . . . . ?
C29 C24 C25 C26 0.0(5) . . . . ?
P2 C24 C25 C26 177.3(3) . . . . ?
C24 C25 C26 C27 -2.1(6) . . . . ?
C25 C26 C27 C28 2.7(6) . . . . ?
B1 C17 P2 C24 166.7(2) . . . . ?
B1 C17 P2 C18 -88.6(2) . . . . ?
B1 C17 P2 Mo1 39.3(2) . . . . ?
C29 C24 P2 C17 13.3(3) . . . . ?
C25 C24 P2 C17 -163.8(3) . . . . ?
C29 C24 P2 C18 -94.7(3) . . . . ?
C25 C24 P2 C18 88.2(3) . . . . ?
C29 C24 P2 Mo1 137.8(3) . . . . ?
C25 C24 P2 Mo1 -39.3(3) . . . . ?
C19 C18 P2 C17 153.2(3) . . . . ?
C23 C18 P2 C17 -25.9(4) . . . . ?
C19 C18 P2 C24 -98.0(3) . . . . ?
C23 C18 P2 C24 83.0(3) . . . . ?
C19 C18 P2 Mo1 28.9(4) . . . . ?
C23 C18 P2 Mo1 -150.2(3) . . . . ?
C26 C27 C28 C29 -1.4(6) . . . . ?
C27 C28 C29 C24 -0.7(6) . . . . ?
C25 C24 C29 C28 1.4(5) . . . . ?
P2 C24 C29 C28 -175.8(3) . . . . ?
C36 C31 C32 C33 2.2(5) . . . . ?
P3 C31 C32 C33 -176.1(3) . . . . ?
C31 C32 C33 C34 -1.9(5) . . . . ?
C32 C33 C34 C35 0.7(5) . . . . ?
C33 C34 C35 C36 0.2(6) . . . . ?
C34 C35 C36 C31 0.1(6) . . . . ?
C32 C31 C36 C35 -1.3(5) . . . . ?
P3 C31 C36 C35 177.0(3) . . . . ?
C42 C37 C38 C39 -1.7(5) . . . . ?
P3 C37 C38 C39 176.1(2) . . . . ?
C37 C38 C39 C40 0.2(5) . . . . ?
C38 C39 C40 C41 1.6(5) . . . . ?
C39 C40 C41 C42 -1.8(5) . . . . ?
C38 C37 C42 C41 1.4(5) . . . . ?
P3 C37 C42 C41 -176.1(2) . . . . ?
C40 C41 C42 C37 0.3(5) . . . . ?
B1 C30 P3 C31 -92.2(2) . . . . ?
B1 C30 P3 C37 163.4(2) . . . . ?
B1 C30 P3 Mo1 36.6(2) . . . . ?
C32 C31 P3 C30 124.6(3) . . . . ?
C36 C31 P3 C30 -53.6(3) . . . . ?
C32 C31 P3 C37 -125.8(3) . . . . ?
C36 C31 P3 C37 55.9(3) . . . . ?
C32 C31 P3 Mo1 -1.1(3) . . . . ?
C36 C31 P3 Mo1 -179.3(2) . . . . ?
C42 C37 P3 C30 10.5(3) . . . . ?
C38 C37 P3 C30 -167.0(2) . . . . ?
C42 C37 P3 C31 -95.1(3) . . . . ?
C38 C37 P3 C31 87.4(3) . . . . ?
C42 C37 P3 Mo1 137.1(2) . . . . ?
C38 C37 P3 Mo1 -40.4(3) . . . . ?
P1 C4 B1 C43 160.2(2) . . . . ?
P1 C4 B1 C17 -80.9(3) . . . . ?
P1 C4 B1 C30 44.5(3) . . . . ?
P2 C17 B1 C43 158.8(2) . . . . ?
P2 C17 B1 C4 38.5(3) . . . . ?
P2 C17 B1 C30 -87.1(3) . . . . ?
P3 C30 B1 C43 155.1(2) . . . . ?
P3 C30 B1 C4 -86.2(3) . . . . ?
P3 C30 B1 C17 39.2(3) . . . . ?
C4 B1 C43 C44 150.4(3) . . . . ?
C17 B1 C43 C44 28.9(4) . . . . ?
C30 B1 C43 C44 -89.5(3) . . . . ?
C4 B1 C43 C48 -32.0(4) . . . . ?
C17 B1 C43 C48 -153.4(3) . . . . ?
C30 B1 C43 C48 88.1(3) . . . . ?
C4 B1 C43 W1 59.1(3) . . . . ?
C17 B1 C43 W1 -62.3(3) . . . . ?
C30 B1 C43 W1 179.2(2) . . . . ?
C48 C43 C44 C45 -1.6(5) . . . . ?
B1 C43 C44 C45 176.3(3) . . . . ?
W1 C43 C44 C45 -57.1(3) . . . . ?
C48 C43 C44 W1 55.5(2) . . . . ?
B1 C43 C44 W1 -126.6(3) . . . . ?
C43 C44 C45 C46 1.3(5) . . . . ?
W1 C44 C45 C46 -56.3(3) . . . . ?
C43 C44 C45 W1 57.6(3) . . . . ?
C44 C45 C46 C47 -1.2(5) . . . . ?
W1 C45 C46 C47 -57.3(3) . . . . ?
C44 C45 C46 W1 56.1(3) . . . . ?
C45 C46 C47 C48 1.6(5) . . . . ?
W1 C46 C47 C48 -56.5(3) . . . . ?
C45 C46 C47 W1 58.1(3) . . . . ?
C46 C47 C48 C43 -2.0(5) . . . . ?
W1 C47 C48 C43 -59.5(3) . . . . ?
C46 C47 C48 W1 57.5(3) . . . . ?
C44 C43 C48 C47 2.0(5) . . . . ?
B1 C43 C48 C47 -175.8(3) . . . . ?
W1 C43 C48 C47 58.5(3) . . . . ?
C44 C43 C48 W1 -56.5(2) . . . . ?
B1 C43 C48 W1 125.7(3) . . . . ?
C56 N1 C52 C53 176.3(4) . . . . ?
C58 N1 C52 C53 53.2(5) . . . . ?
C54 N1 C52 C53 -62.8(5) . . . . ?
C56 N1 C54 C55 -54.4(6) . . . . ?
C52 N1 C54 C55 -175.8(4) . . . . ?
C58 N1 C54 C55 65.6(5) . . . . ?
C52 N1 C56 C57 55.9(5) . . . . ?
C58 N1 C56 C57 178.9(4) . . . . ?
C54 N1 C56 C57 -63.6(5) . . . . ?
C56 N1 C58 C59 -69.2(5) . . . . ?
C52 N1 C58 C59 54.1(5) . . . . ?
C54 N1 C58 C59 171.0(4) . . . . ?

_refine_diff_density_max         1.470
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.098

_shelxl_version_number           2014-3


# start Validation Reply Form
_vrf_ABSMU01_14143zzz            
;
PROBLEM: The ratio of given/expected absorption coefficient lies
RESPONSE: ... Disordered solvent treated with PLATON/SQUEEZE with
THF atoms included in the formula
;
_vrf_DIFMN02_14143zzz            
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*2.00
RESPONSE: ... Tungsten is present
;
_vrf_DIFMX01_14143zzz            
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*2.00
RESPONSE: ... Tungsten is present
;
_vrf_CHEMW03_14143zzz            
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: ... Disordered solvent treated with PLATON/SQUEEZE with
THF atoms included in the formula
;
_vrf_PLAT047_14143zzz            
;
PROBLEM: SumFormula Not Given ...........................     Please Do ! 
RESPONSE: ...
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Et2O'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_14145b
_database_code_depnum_ccdc_archive 'CCDC 1039151'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        '[Et4N][W(CO)3{6-(PhBP3)W(CO)3}]'
_chemical_name_common            14145a
_chemical_melting_point          553
_chemical_formula_moiety         'C51 H41 B O6 P3 W2, C8 H20 N'
_chemical_formula_sum            'C59 H61 B N O6 P3 W2'
_chemical_formula_weight         1351.50

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'
N N 0.0061 0.0033 '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           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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, y+1/2, -z'

_cell_length_a                   12.0742(11)
_cell_length_b                   13.3231(12)
_cell_length_c                   17.7935(16)
_cell_angle_alpha                90
_cell_angle_beta                 108.1280(10)
_cell_angle_gamma                90
_cell_volume                     2720.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2900
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      27.74

_exptl_crystal_description       Plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_F_000             1336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    4.365
_shelx_estimated_absorpt_T_min   0.476
_shelx_estimated_absorpt_T_max   0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5530
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'

_exptl_special_details           'Prof. P. Fischer'


_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX-II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31902
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.775
_diffrn_reflns_theta_max         27.801
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12578
_reflns_number_gt                11336
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_max     0.964
_reflns_Friedel_fraction_full    0.997

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0306P)²+0.8723P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 4973 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(5)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         12578
_refine_ls_number_parameters     653
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0685
_refine_ls_wR_factor_gt          0.0657
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_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
W1 W 0.32265(2) 0.38750(2) 0.67156(2) 0.01751(7) Uani 1 1 d . . . . .
C1 C 0.2221(7) 0.4120(5) 0.5630(5) 0.0233(19) Uani 1 1 d . . . . .
O1 O 0.1640(5) 0.4213(5) 0.4969(3) 0.0347(16) Uani 1 1 d . . . . .
C2 C 0.3481(7) 0.2556(7) 0.6299(5) 0.0288(19) Uani 1 1 d . . . . .
O2 O 0.3661(6) 0.1819(5) 0.6002(4) 0.0480(18) Uani 1 1 d . . . . .
C3 C 0.4519(7) 0.4327(6) 0.6354(5) 0.0262(18) Uani 1 1 d . . . . .
O3 O 0.5242(5) 0.4581(5) 0.6076(4) 0.0381(15) Uani 1 1 d . . . . .
C4 C 0.1666(6) 0.3731(6) 0.8214(4) 0.0196(16) Uani 1 1 d . . . . .
H4A H 0.0882 0.3879 0.8253 0.024 Uiso 1 1 calc R U . . .
H4B H 0.1969 0.3138 0.8551 0.024 Uiso 1 1 calc R U . . .
P1 P 0.15099(17) 0.33988(16) 0.71892(12) 0.0193(4) Uani 1 1 d . . . . .
C5 C 0.1116(7) 0.2061(6) 0.7123(5) 0.0269(18) Uani 1 1 d . . . . .
C6 C 0.1054(8) 0.1520(7) 0.6433(6) 0.036(2) Uani 1 1 d . . . . .
H6A H 0.1148 0.1863 0.5989 0.044 Uiso 1 1 calc R U . . .
C7 C 0.0858(11) 0.0503(8) 0.6392(7) 0.058(3) Uani 1 1 d . . . . .
H7A H 0.0823 0.0147 0.5922 0.070 Uiso 1 1 calc R U . . .
C8 C 0.0709(11) -0.0008(8) 0.7035(7) 0.060(3) Uani 1 1 d . . . . .
H8A H 0.0607 -0.0715 0.7015 0.072 Uiso 1 1 calc R U . . .
C9 C 0.0711(10) 0.0514(8) 0.7696(6) 0.049(3) Uani 1 1 d . . . . .
H9A H 0.0562 0.0170 0.8123 0.059 Uiso 1 1 calc R U . . .
C10 C 0.0926(8) 0.1529(7) 0.7754(5) 0.035(2) Uani 1 1 d . . . . .
H10A H 0.0946 0.1875 0.8225 0.041 Uiso 1 1 calc R U . . .
C11 C 0.0090(6) 0.3976(6) 0.6647(4) 0.0232(16) Uani 1 1 d . . . . .
C12 C 0.0018(7) 0.4819(6) 0.6177(5) 0.0245(17) Uani 1 1 d . . . . .
H12A H 0.0705 0.5091 0.6105 0.029 Uiso 1 1 calc R U . . .
C13 C -0.1052(7) 0.5270(7) 0.5810(5) 0.032(2) Uani 1 1 d . . . . .
H13A H -0.1092 0.5851 0.5493 0.038 Uiso 1 1 calc R U . . .
C14 C -0.2062(7) 0.4874(8) 0.5905(5) 0.038(2) Uani 1 1 d . . . . .
H14A H -0.2794 0.5183 0.5655 0.046 Uiso 1 1 calc R U . . .
C15 C -0.1997(7) 0.4026(9) 0.6367(5) 0.042(2) Uani 1 1 d . . . . .
H15A H -0.2689 0.3743 0.6424 0.050 Uiso 1 1 calc R U . . .
C16 C -0.0930(7) 0.3588(7) 0.6744(5) 0.034(2) Uani 1 1 d . . . . .
H16A H -0.0891 0.3019 0.7074 0.041 Uiso 1 1 calc R U . . .
P2 P 0.30179(16) 0.56200(15) 0.72419(12) 0.0175(4) Uani 1 1 d . . . . .
C17 C 0.2218(6) 0.5645(6) 0.7953(4) 0.0187(15) Uani 1 1 d . . . . .
H17A H 0.2398 0.6280 0.8257 0.022 Uiso 1 1 calc R U . . .
H17B H 0.1373 0.5641 0.7664 0.022 Uiso 1 1 calc R U . . .
C18 C 0.2279(6) 0.6519(6) 0.6462(4) 0.0212(16) Uani 1 1 d . . . . .
C19 C 0.2569(8) 0.6524(7) 0.5769(5) 0.0323(19) Uani 1 1 d . . . . .
H19A H 0.3170 0.6095 0.5717 0.039 Uiso 1 1 calc R U . . .
C20 C 0.1987(9) 0.7150(7) 0.5149(5) 0.043(3) Uani 1 1 d . . . . .
H20A H 0.2192 0.7144 0.4675 0.052 Uiso 1 1 calc R U . . .
C21 C 0.1123(10) 0.7773(7) 0.5212(6) 0.045(3) Uani 1 1 d . . . . .
H21A H 0.0730 0.8200 0.4784 0.054 Uiso 1 1 calc R U . . .
C22 C 0.0824(8) 0.7782(6) 0.5892(5) 0.033(2) Uani 1 1 d . . . . .
H22A H 0.0215 0.8208 0.5933 0.039 Uiso 1 1 calc R U . . .
C23 C 0.1410(7) 0.7168(6) 0.6527(5) 0.031(2) Uani 1 1 d . . . . .
H23A H 0.1215 0.7193 0.7004 0.037 Uiso 1 1 calc R U . . .
C24 C 0.4339(6) 0.6349(5) 0.7764(4) 0.0195(16) Uani 1 1 d . . . . .
C25 C 0.4247(7) 0.7269(6) 0.8113(5) 0.0253(18) Uani 1 1 d . . . . .
H25A H 0.3501 0.7553 0.8046 0.030 Uiso 1 1 calc R U . . .
C26 C 0.5239(7) 0.7771(6) 0.8558(5) 0.0286(19) Uani 1 1 d . . . . .
H26A H 0.5162 0.8395 0.8795 0.034 Uiso 1 1 calc R U . . .
C27 C 0.6325(7) 0.7388(6) 0.8662(5) 0.0290(19) Uani 1 1 d . . . . .
H27A H 0.6995 0.7734 0.8980 0.035 Uiso 1 1 calc R U . . .
C28 C 0.6443(6) 0.6492(6) 0.8303(5) 0.0265(18) Uani 1 1 d . . . . .
H28A H 0.7195 0.6224 0.8365 0.032 Uiso 1 1 calc R U . . .
C29 C 0.5458(6) 0.5985(6) 0.7850(4) 0.0239(16) Uani 1 1 d . . . . .
H29A H 0.5545 0.5379 0.7593 0.029 Uiso 1 1 calc R U . . .
C30 C 0.3932(6) 0.4360(5) 0.8839(4) 0.0176(15) Uani 1 1 d . . . . .
H30A H 0.4148 0.4045 0.9369 0.021 Uiso 1 1 calc R U . . .
H30B H 0.4407 0.4975 0.8883 0.021 Uiso 1 1 calc R U . . .
P3 P 0.43066(16) 0.34947(14) 0.81587(12) 0.0184(4) Uani 1 1 d . . . . .
C31 C 0.5902(6) 0.3497(6) 0.8421(5) 0.0250(17) Uani 1 1 d . . . . .
C32 C 0.6406(8) 0.3010(7) 0.7911(6) 0.040(2) Uani 1 1 d . . . . .
H32A H 0.5915 0.2708 0.7441 0.048 Uiso 1 1 calc R U . . .
C33 C 0.7598(8) 0.2959(9) 0.8076(6) 0.048(3) Uani 1 1 d . . . . .
H33A H 0.7932 0.2586 0.7745 0.058 Uiso 1 1 calc R U . . .
C34 C 0.8303(8) 0.3465(9) 0.8737(8) 0.057(3) Uani 1 1 d . . . . .
H34A H 0.9123 0.3466 0.8836 0.069 Uiso 1 1 calc R U . . .
C35 C 0.7852(8) 0.3962(8) 0.9250(7) 0.052(3) Uani 1 1 d . . . . .
H35A H 0.8349 0.4290 0.9704 0.062 Uiso 1 1 calc R U . . .
C36 C 0.6624(7) 0.3976(7) 0.9086(5) 0.037(2) Uani 1 1 d . . . . .
H36A H 0.6294 0.4316 0.9435 0.044 Uiso 1 1 calc R U . . .
C37 C 0.4093(7) 0.2226(6) 0.8511(5) 0.0218(17) Uani 1 1 d . . . . .
C38 C 0.4053(9) 0.1397(6) 0.8028(6) 0.038(2) Uani 1 1 d . . . . .
H38A H 0.4124 0.1495 0.7516 0.045 Uiso 1 1 calc R U . . .
C39 C 0.3915(9) 0.0444(6) 0.8272(6) 0.040(2) Uani 1 1 d . . . . .
H39A H 0.3910 -0.0108 0.7932 0.049 Uiso 1 1 calc R U . . .
C40 C 0.3783(8) 0.0273(7) 0.9005(6) 0.037(2) Uani 1 1 d . . . . .
H40A H 0.3656 -0.0387 0.9165 0.044 Uiso 1 1 calc R U . . .
C41 C 0.3839(8) 0.1078(7) 0.9497(5) 0.036(2) Uani 1 1 d . . . . .
H41A H 0.3771 0.0974 1.0010 0.043 Uiso 1 1 calc R U . . .
C42 C 0.3993(8) 0.2039(6) 0.9253(5) 0.032(2) Uani 1 1 d . . . . .
H42A H 0.4030 0.2586 0.9603 0.038 Uiso 1 1 calc R U . . .
B1 B 0.2521(7) 0.4692(6) 0.8580(5) 0.0163(16) Uani 1 1 d . . . . .
C43 C 0.2326(6) 0.5035(5) 0.9413(4) 0.0189(15) Uani 1 1 d . . . . .
C44 C 0.1634(7) 0.4488(6) 0.9789(5) 0.0233(17) Uani 1 1 d . . . . .
H44A H 0.1263 0.3890 0.9544 0.028 Uiso 1 1 calc R U . . .
C45 C 0.1471(7) 0.4787(6) 1.0506(5) 0.0276(18) Uani 1 1 d . . . . .
H45A H 0.1014 0.4390 1.0741 0.033 Uiso 1 1 calc R U . . .
C46 C 0.1997(7) 0.5690(6) 1.0874(5) 0.0278(18) Uani 1 1 d . . . . .
H46A H 0.1863 0.5922 1.1343 0.033 Uiso 1 1 calc R U . . .
C47 C 0.2718(6) 0.6234(7) 1.0537(4) 0.0269(17) Uani 1 1 d . . . . .
H47A H 0.3118 0.6813 1.0798 0.032 Uiso 1 1 calc R U . . .
C48 C 0.2851(7) 0.5922(6) 0.9810(4) 0.0238(17) Uani 1 1 d . . . . .
H48A H 0.3309 0.6322 0.9578 0.029 Uiso 1 1 calc R U . . .
W2 W 0.08364(3) 0.61241(2) 0.95909(2) 0.02197(8) Uani 1 1 d . . . . .
C49 C 0.0786(9) 0.7468(7) 0.9137(6) 0.040(2) Uani 1 1 d . . . . .
O4 O 0.0765(8) 0.8253(5) 0.8861(5) 0.065(2) Uani 1 1 d . . . . .
C50 C -0.0302(8) 0.5812(7) 0.8569(5) 0.031(2) Uani 1 1 d . . . . .
O5 O -0.0963(6) 0.5650(5) 0.7939(4) 0.0432(17) Uani 1 1 d . . . . .
C51 C -0.0450(7) 0.6556(7) 0.9960(5) 0.033(2) Uani 1 1 d . . . . .
O6 O -0.1191(6) 0.6833(6) 1.0204(4) 0.057(2) Uani 1 1 d . . . . .
N1 N 0.3823(8) 0.3743(8) 0.3672(5) 0.055(2) Uani 1 1 d . . . . .
C52 C 0.4856(9) 0.3769(11) 0.3351(6) 0.064(3) Uani 1 1 d . . . . .
H52A H 0.5011 0.3073 0.3215 0.077 Uiso 1 1 calc R U . . .
H52B H 0.4623 0.4160 0.2854 0.077 Uiso 1 1 calc R U . . .
C53 C 0.5959(10) 0.4192(9) 0.3872(8) 0.069(4) Uani 1 1 d . . . . .
H53A H 0.6555 0.4159 0.3604 0.103 Uiso 1 1 calc R U . . .
H53B H 0.6217 0.3806 0.4364 0.103 Uiso 1 1 calc R U . . .
H53C H 0.5837 0.4894 0.3992 0.103 Uiso 1 1 calc R U . . .
C54 C 0.4089(12) 0.3083(8) 0.4407(7) 0.062(4) Uani 1 1 d . . . . .
H54A H 0.4765 0.3368 0.4822 0.074 Uiso 1 1 calc R U . . .
H54B H 0.3412 0.3093 0.4608 0.074 Uiso 1 1 calc R U . . .
C55 C 0.4354(15) 0.2018(10) 0.4254(12) 0.117(7) Uani 1 1 d . . . . .
H55A H 0.4423 0.1612 0.4726 0.176 Uiso 1 1 calc R U . . .
H55B H 0.5089 0.1992 0.4129 0.176 Uiso 1 1 calc R U . . .
H55C H 0.3723 0.1752 0.3807 0.176 Uiso 1 1 calc R U . . .
C56 C 0.3520(12) 0.4743(9) 0.3913(8) 0.064(3) Uani 1 1 d . . . . .
H56A H 0.4174 0.4970 0.4372 0.077 Uiso 1 1 calc R U . . .
H56B H 0.2831 0.4664 0.4097 0.077 Uiso 1 1 calc R U . . .
C57 C 0.3260(16) 0.5564(12) 0.3304(10) 0.106(6) Uani 1 1 d . . . . .
H57A H 0.2952 0.6150 0.3506 0.158 Uiso 1 1 calc R U . . .
H57B H 0.2681 0.5326 0.2818 0.158 Uiso 1 1 calc R U . . .
H57C H 0.3977 0.5750 0.3190 0.158 Uiso 1 1 calc R U . . .
C58 C 0.2803(11) 0.3339(13) 0.2991(8) 0.092(5) Uani 1 1 d . . . . .
H58A H 0.3053 0.2717 0.2786 0.110 Uiso 1 1 calc R U . . .
H58B H 0.2601 0.3838 0.2557 0.110 Uiso 1 1 calc R U . . .
C59 C 0.1706(12) 0.3111(16) 0.3232(11) 0.131(9) Uani 1 1 d . . . . .
H59A H 0.1070 0.2903 0.2765 0.197 Uiso 1 1 calc R U . . .
H59B H 0.1474 0.3715 0.3459 0.197 Uiso 1 1 calc R U . . .
H59C H 0.1878 0.2570 0.3625 0.197 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C3 1.960(8) . ?
W1 C1 1.963(9) . ?
W1 C2 1.969(9) . ?
W1 P3 2.543(2) . ?
W1 P2 2.548(2) . ?
W1 P1 2.5486(19) . ?
C1 O1 1.174(10) . ?
C2 O2 1.166(10) . ?
C3 O3 1.178(9) . ?
C4 B1 1.646(10) . ?
C4 P1 1.829(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
P1 C5 1.840(8) . ?
P1 C11 1.853(8) . ?
C5 C6 1.404(12) . ?
C5 C10 1.406(12) . ?
C6 C7 1.374(13) . ?
C6 H6A 0.9500 . ?
C7 C8 1.391(15) . ?
C7 H7A 0.9500 . ?
C8 C9 1.366(14) . ?
C8 H8A 0.9500 . ?
C9 C10 1.376(12) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C12 1.387(12) . ?
C11 C16 1.395(11) . ?
C12 C13 1.390(11) . ?
C12 H12A 0.9500 . ?
C13 C14 1.386(12) . ?
C13 H13A 0.9500 . ?
C14 C15 1.385(14) . ?
C14 H14A 0.9500 . ?
C15 C16 1.383(12) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
P2 C17 1.816(7) . ?
P2 C18 1.840(7) . ?
P2 C24 1.851(7) . ?
C17 B1 1.654(11) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.382(11) . ?
C18 C23 1.392(11) . ?
C19 C20 1.387(12) . ?
C19 H19A 0.9500 . ?
C20 C21 1.365(14) . ?
C20 H20A 0.9500 . ?
C21 C22 1.366(13) . ?
C21 H21A 0.9500 . ?
C22 C23 1.396(12) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 C25 1.394(11) . ?
C24 C29 1.398(10) . ?
C25 C26 1.384(11) . ?
C25 H25A 0.9500 . ?
C26 C27 1.365(12) . ?
C26 H26A 0.9500 . ?
C27 C28 1.382(12) . ?
C27 H27A 0.9500 . ?
C28 C29 1.386(10) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 B1 1.679(10) . ?
C30 P3 1.827(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
P3 C31 1.835(8) . ?
P3 C37 1.848(8) . ?
C31 C36 1.388(12) . ?
C31 C32 1.400(12) . ?
C32 C33 1.379(13) . ?
C32 H32A 0.9500 . ?
C33 C34 1.393(16) . ?
C33 H33A 0.9500 . ?
C34 C35 1.370(16) . ?
C34 H34A 0.9500 . ?
C35 C36 1.420(12) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 C42 1.385(11) . ?
C37 C38 1.392(11) . ?
C38 C39 1.369(12) . ?
C38 H38A 0.9500 . ?
C39 C40 1.382(13) . ?
C39 H39A 0.9500 . ?
C40 C41 1.373(13) . ?
C40 H40A 0.9500 . ?
C41 C42 1.385(12) . ?
C41 H41A 0.9500 . ?
C42 H42A 0.9500 . ?
B1 C43 1.638(11) . ?
C43 C48 1.421(10) . ?
C43 C44 1.424(10) . ?
C43 W2 2.407(7) . ?
C44 C45 1.407(11) . ?
C44 W2 2.365(8) . ?
C44 H44A 0.9500 . ?
C45 C46 1.422(12) . ?
C45 W2 2.374(8) . ?
C45 H45A 0.9500 . ?
C46 C47 1.403(11) . ?
C46 W2 2.350(8) . ?
C46 H46A 0.9500 . ?
C47 C48 1.414(10) . ?
C47 W2 2.374(7) . ?
C47 H47A 0.9500 . ?
C48 W2 2.356(8) . ?
C48 H48A 0.9500 . ?
W2 C51 1.952(8) . ?
W2 C50 1.953(9) . ?
W2 C49 1.956(10) . ?
C49 O4 1.152(11) . ?
C50 O5 1.177(10) . ?
C51 O6 1.169(10) . ?
N1 C56 1.480(15) . ?
N1 C54 1.523(14) . ?
N1 C52 1.526(12) . ?
N1 C58 1.532(14) . ?
C52 C53 1.477(15) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.498(16) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 C57 1.502(17) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C59 1.544(18) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?

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
C3 W1 C1 86.4(3) . . ?
C3 W1 C2 85.2(3) . . ?
C1 W1 C2 84.2(3) . . ?
C3 W1 P3 100.5(3) . . ?
C1 W1 P3 173.1(2) . . ?
C2 W1 P3 96.4(3) . . ?
C3 W1 P2 91.2(2) . . ?
C1 W1 P2 96.2(2) . . ?
C2 W1 P2 176.3(3) . . ?
P3 W1 P2 83.63(6) . . ?
C3 W1 P1 176.5(2) . . ?
C1 W1 P1 92.8(2) . . ?
C2 W1 P1 98.1(3) . . ?
P3 W1 P1 80.26(6) . . ?
P2 W1 P1 85.53(6) . . ?
O1 C1 W1 176.1(7) . . ?
O2 C2 W1 174.1(8) . . ?
O3 C3 W1 174.7(7) . . ?
B1 C4 P1 116.1(5) . . ?
B1 C4 H4A 108.3 . . ?
P1 C4 H4A 108.3 . . ?
B1 C4 H4B 108.3 . . ?
P1 C4 H4B 108.3 . . ?
H4A C4 H4B 107.4 . . ?
C4 P1 C5 104.1(4) . . ?
C4 P1 C11 102.2(3) . . ?
C5 P1 C11 100.9(4) . . ?
C4 P1 W1 115.3(2) . . ?
C5 P1 W1 116.1(3) . . ?
C11 P1 W1 116.1(3) . . ?
C6 C5 C10 117.6(8) . . ?
C6 C5 P1 119.7(6) . . ?
C10 C5 P1 122.7(6) . . ?
C7 C6 C5 120.9(10) . . ?
C7 C6 H6A 119.5 . . ?
C5 C6 H6A 119.5 . . ?
C6 C7 C8 120.2(10) . . ?
C6 C7 H7A 119.9 . . ?
C8 C7 H7A 119.9 . . ?
C9 C8 C7 119.6(10) . . ?
C9 C8 H8A 120.2 . . ?
C7 C8 H8A 120.2 . . ?
C8 C9 C10 120.9(10) . . ?
C8 C9 H9A 119.5 . . ?
C10 C9 H9A 119.5 . . ?
C9 C10 C5 120.7(9) . . ?
C9 C10 H10A 119.7 . . ?
C5 C10 H10A 119.7 . . ?
C12 C11 C16 118.8(7) . . ?
C12 C11 P1 121.6(6) . . ?
C16 C11 P1 119.4(6) . . ?
C11 C12 C13 120.6(8) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C14 C13 C12 120.2(9) . . ?
C14 C13 H13A 119.9 . . ?
C12 C13 H13A 119.9 . . ?
C13 C14 C15 119.5(8) . . ?
C13 C14 H14A 120.2 . . ?
C15 C14 H14A 120.2 . . ?
C16 C15 C14 120.3(8) . . ?
C16 C15 H15A 119.9 . . ?
C14 C15 H15A 119.9 . . ?
C15 C16 C11 120.6(9) . . ?
C15 C16 H16A 119.7 . . ?
C11 C16 H16A 119.7 . . ?
C17 P2 C18 106.0(3) . . ?
C17 P2 C24 101.7(3) . . ?
C18 P2 C24 100.2(3) . . ?
C17 P2 W1 114.1(2) . . ?
C18 P2 W1 113.4(3) . . ?
C24 P2 W1 119.7(2) . . ?
B1 C17 P2 113.7(5) . . ?
B1 C17 H17A 108.8 . . ?
P2 C17 H17A 108.8 . . ?
B1 C17 H17B 108.8 . . ?
P2 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C19 C18 C23 118.5(7) . . ?
C19 C18 P2 118.5(6) . . ?
C23 C18 P2 122.9(6) . . ?
C18 C19 C20 120.4(8) . . ?
C18 C19 H19A 119.8 . . ?
C20 C19 H19A 119.8 . . ?
C21 C20 C19 120.8(9) . . ?
C21 C20 H20A 119.6 . . ?
C19 C20 H20A 119.6 . . ?
C20 C21 C22 119.7(9) . . ?
C20 C21 H21A 120.1 . . ?
C22 C21 H21A 120.1 . . ?
C21 C22 C23 120.4(8) . . ?
C21 C22 H22A 119.8 . . ?
C23 C22 H22A 119.8 . . ?
C18 C23 C22 120.1(8) . . ?
C18 C23 H23A 119.9 . . ?
C22 C23 H23A 119.9 . . ?
C25 C24 C29 117.6(7) . . ?
C25 C24 P2 120.6(6) . . ?
C29 C24 P2 121.7(6) . . ?
C26 C25 C24 120.3(8) . . ?
C26 C25 H25A 119.8 . . ?
C24 C25 H25A 119.8 . . ?
C27 C26 C25 121.3(8) . . ?
C27 C26 H26A 119.3 . . ?
C25 C26 H26A 119.3 . . ?
C26 C27 C28 119.5(8) . . ?
C26 C27 H27A 120.2 . . ?
C28 C27 H27A 120.2 . . ?
C27 C28 C29 119.8(7) . . ?
C27 C28 H28A 120.1 . . ?
C29 C28 H28A 120.1 . . ?
C28 C29 C24 121.3(7) . . ?
C28 C29 H29A 119.3 . . ?
C24 C29 H29A 119.3 . . ?
B1 C30 P3 115.1(5) . . ?
B1 C30 H30A 108.5 . . ?
P3 C30 H30A 108.5 . . ?
B1 C30 H30B 108.5 . . ?
P3 C30 H30B 108.5 . . ?
H30A C30 H30B 107.5 . . ?
C30 P3 C31 106.7(4) . . ?
C30 P3 C37 105.2(4) . . ?
C31 P3 C37 99.3(3) . . ?
C30 P3 W1 112.8(2) . . ?
C31 P3 W1 115.1(3) . . ?
C37 P3 W1 116.3(3) . . ?
C36 C31 C32 118.8(8) . . ?
C36 C31 P3 123.3(6) . . ?
C32 C31 P3 117.9(7) . . ?
C33 C32 C31 121.4(10) . . ?
C33 C32 H32A 119.3 . . ?
C31 C32 H32A 119.3 . . ?
C32 C33 C34 118.6(10) . . ?
C32 C33 H33A 120.7 . . ?
C34 C33 H33A 120.7 . . ?
C35 C34 C33 122.1(9) . . ?
C35 C34 H34A 119.0 . . ?
C33 C34 H34A 119.0 . . ?
C34 C35 C36 118.5(10) . . ?
C34 C35 H35A 120.8 . . ?
C36 C35 H35A 120.8 . . ?
C31 C36 C35 120.5(9) . . ?
C31 C36 H36A 119.8 . . ?
C35 C36 H36A 119.8 . . ?
C42 C37 C38 116.7(8) . . ?
C42 C37 P3 123.4(6) . . ?
C38 C37 P3 119.9(6) . . ?
C39 C38 C37 121.7(8) . . ?
C39 C38 H38A 119.2 . . ?
C37 C38 H38A 119.2 . . ?
C38 C39 C40 120.9(8) . . ?
C38 C39 H39A 119.5 . . ?
C40 C39 H39A 119.5 . . ?
C41 C40 C39 118.5(8) . . ?
C41 C40 H40A 120.8 . . ?
C39 C40 H40A 120.8 . . ?
C40 C41 C42 120.4(8) . . ?
C40 C41 H41A 119.8 . . ?
C42 C41 H41A 119.8 . . ?
C37 C42 C41 121.8(8) . . ?
C37 C42 H42A 119.1 . . ?
C41 C42 H42A 119.1 . . ?
C43 B1 C4 109.0(6) . . ?
C43 B1 C17 109.4(6) . . ?
C4 B1 C17 110.6(6) . . ?
C43 B1 C30 104.1(6) . . ?
C4 B1 C30 111.2(6) . . ?
C17 B1 C30 112.4(6) . . ?
C48 C43 C44 115.4(7) . . ?
C48 C43 B1 121.0(6) . . ?
C44 C43 B1 123.6(6) . . ?
C48 C43 W2 70.7(4) . . ?
C44 C43 W2 71.0(4) . . ?
B1 C43 W2 127.7(5) . . ?
C45 C44 C43 123.3(7) . . ?
C45 C44 W2 73.1(5) . . ?
C43 C44 W2 74.3(4) . . ?
C45 C44 H44A 118.3 . . ?
C43 C44 H44A 118.3 . . ?
W2 C44 H44A 126.3 . . ?
C44 C45 C46 119.2(7) . . ?
C44 C45 W2 72.4(5) . . ?
C46 C45 W2 71.5(5) . . ?
C44 C45 H45A 120.4 . . ?
C46 C45 H45A 120.4 . . ?
W2 C45 H45A 127.8 . . ?
C47 C46 C45 119.2(7) . . ?
C47 C46 W2 73.7(5) . . ?
C45 C46 W2 73.4(5) . . ?
C47 C46 H46A 120.4 . . ?
C45 C46 H46A 120.4 . . ?
W2 C46 H46A 124.0 . . ?
C46 C47 C48 120.1(7) . . ?
C46 C47 W2 71.8(5) . . ?
C48 C47 W2 71.9(4) . . ?
C46 C47 H47A 120.0 . . ?
C48 C47 H47A 120.0 . . ?
W2 C47 H47A 128.6 . . ?
C47 C48 C43 122.6(7) . . ?
C47 C48 W2 73.3(4) . . ?
C43 C48 W2 74.6(4) . . ?
C47 C48 H48A 118.7 . . ?
C43 C48 H48A 118.7 . . ?
W2 C48 H48A 125.1 . . ?
C51 W2 C50 88.4(3) . . ?
C51 W2 C49 86.7(4) . . ?
C50 W2 C49 83.6(4) . . ?
C51 W2 C46 92.4(3) . . ?
C50 W2 C46 152.5(3) . . ?
C49 W2 C46 124.0(4) . . ?
C51 W2 C48 150.1(3) . . ?
C50 W2 C48 121.4(3) . . ?
C49 W2 C48 94.1(4) . . ?
C46 W2 C48 62.5(3) . . ?
C51 W2 C44 123.5(3) . . ?
C50 W2 C44 94.5(3) . . ?
C49 W2 C44 149.8(3) . . ?
C46 W2 C44 62.3(3) . . ?
C48 W2 C44 61.2(3) . . ?
C51 W2 C45 96.4(3) . . ?
C50 W2 C45 117.5(3) . . ?
C49 W2 C45 158.7(4) . . ?
C46 W2 C45 35.0(3) . . ?
C48 W2 C45 72.8(3) . . ?
C44 W2 C45 34.5(3) . . ?
C51 W2 C47 115.4(3) . . ?
C50 W2 C47 156.1(3) . . ?
C49 W2 C47 97.8(4) . . ?
C46 W2 C47 34.5(3) . . ?
C48 W2 C47 34.8(3) . . ?
C44 W2 C47 72.3(3) . . ?
C45 W2 C47 61.7(3) . . ?
C51 W2 C43 158.0(3) . . ?
C50 W2 C43 95.0(3) . . ?
C49 W2 C43 115.2(3) . . ?
C46 W2 C43 74.6(3) . . ?
C48 W2 C43 34.7(2) . . ?
C44 W2 C43 34.7(2) . . ?
C45 W2 C43 62.8(3) . . ?
C47 W2 C43 62.7(3) . . ?
O4 C49 W2 178.8(10) . . ?
O5 C50 W2 177.2(8) . . ?
O6 C51 W2 177.5(8) . . ?
C56 N1 C54 106.1(8) . . ?
C56 N1 C52 113.1(10) . . ?
C54 N1 C52 110.8(9) . . ?
C56 N1 C58 109.6(10) . . ?
C54 N1 C58 112.3(10) . . ?
C52 N1 C58 105.1(8) . . ?
C53 C52 N1 117.2(9) . . ?
C53 C52 H52A 108.0 . . ?
N1 C52 H52A 108.0 . . ?
C53 C52 H52B 108.0 . . ?
N1 C52 H52B 108.0 . . ?
H52A C52 H52B 107.2 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C55 C54 N1 113.0(11) . . ?
C55 C54 H54A 109.0 . . ?
N1 C54 H54A 109.0 . . ?
C55 C54 H54B 109.0 . . ?
N1 C54 H54B 109.0 . . ?
H54A C54 H54B 107.8 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
N1 C56 C57 117.5(11) . . ?
N1 C56 H56A 107.9 . . ?
C57 C56 H56A 107.9 . . ?
N1 C56 H56B 107.9 . . ?
C57 C56 H56B 107.9 . . ?
H56A C56 H56B 107.2 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
N1 C58 C59 113.4(10) . . ?
N1 C58 H58A 108.9 . . ?
C59 C58 H58A 108.9 . . ?
N1 C58 H58B 108.9 . . ?
C59 C58 H58B 108.9 . . ?
H58A C58 H58B 107.7 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?

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
B1 C4 P1 C5 155.1(6) . . . . ?
B1 C4 P1 C11 -100.2(6) . . . . ?
B1 C4 P1 W1 26.7(6) . . . . ?
C4 P1 C5 C6 -172.9(7) . . . . ?
C11 P1 C5 C6 81.5(8) . . . . ?
W1 P1 C5 C6 -45.0(8) . . . . ?
C4 P1 C5 C10 3.9(8) . . . . ?
C11 P1 C5 C10 -101.7(8) . . . . ?
W1 P1 C5 C10 131.8(7) . . . . ?
C10 C5 C6 C7 -2.4(15) . . . . ?
P1 C5 C6 C7 174.5(9) . . . . ?
C5 C6 C7 C8 0.5(18) . . . . ?
C6 C7 C8 C9 3(2) . . . . ?
C7 C8 C9 C10 -3.9(19) . . . . ?
C8 C9 C10 C5 1.8(17) . . . . ?
C6 C5 C10 C9 1.3(14) . . . . ?
P1 C5 C10 C9 -175.6(8) . . . . ?
C4 P1 C11 C12 108.3(6) . . . . ?
C5 P1 C11 C12 -144.5(6) . . . . ?
W1 P1 C11 C12 -18.0(7) . . . . ?
C4 P1 C11 C16 -68.1(7) . . . . ?
C5 P1 C11 C16 39.1(7) . . . . ?
W1 P1 C11 C16 165.5(5) . . . . ?
C16 C11 C12 C13 0.0(12) . . . . ?
P1 C11 C12 C13 -176.5(6) . . . . ?
C11 C12 C13 C14 -0.5(12) . . . . ?
C12 C13 C14 C15 -0.2(13) . . . . ?
C13 C14 C15 C16 1.4(14) . . . . ?
C14 C15 C16 C11 -2.0(14) . . . . ?
C12 C11 C16 C15 1.3(12) . . . . ?
P1 C11 C16 C15 177.9(7) . . . . ?
C18 P2 C17 B1 165.2(5) . . . . ?
C24 P2 C17 B1 -90.5(6) . . . . ?
W1 P2 C17 B1 39.7(6) . . . . ?
C17 P2 C18 C19 -168.4(7) . . . . ?
C24 P2 C18 C19 86.3(7) . . . . ?
W1 P2 C18 C19 -42.5(7) . . . . ?
C17 P2 C18 C23 9.1(8) . . . . ?
C24 P2 C18 C23 -96.3(7) . . . . ?
W1 P2 C18 C23 135.0(6) . . . . ?
C23 C18 C19 C20 -1.2(13) . . . . ?
P2 C18 C19 C20 176.4(7) . . . . ?
C18 C19 C20 C21 0.2(15) . . . . ?
C19 C20 C21 C22 -0.1(16) . . . . ?
C20 C21 C22 C23 1.0(15) . . . . ?
C19 C18 C23 C22 2.1(13) . . . . ?
P2 C18 C23 C22 -175.4(6) . . . . ?
C21 C22 C23 C18 -2.0(14) . . . . ?
C17 P2 C24 C25 -48.1(7) . . . . ?
C18 P2 C24 C25 60.8(7) . . . . ?
W1 P2 C24 C25 -174.7(5) . . . . ?
C17 P2 C24 C29 129.5(6) . . . . ?
C18 P2 C24 C29 -121.7(6) . . . . ?
W1 P2 C24 C29 2.8(7) . . . . ?
C29 C24 C25 C26 -2.9(11) . . . . ?
P2 C24 C25 C26 174.7(6) . . . . ?
C24 C25 C26 C27 0.4(12) . . . . ?
C25 C26 C27 C28 1.6(13) . . . . ?
C26 C27 C28 C29 -1.0(12) . . . . ?
C27 C28 C29 C24 -1.6(12) . . . . ?
C25 C24 C29 C28 3.6(11) . . . . ?
P2 C24 C29 C28 -174.1(6) . . . . ?
B1 C30 P3 C31 166.1(5) . . . . ?
B1 C30 P3 C37 -89.1(6) . . . . ?
B1 C30 P3 W1 38.7(6) . . . . ?
C30 P3 C31 C36 7.9(8) . . . . ?
C37 P3 C31 C36 -101.2(7) . . . . ?
W1 P3 C31 C36 133.9(6) . . . . ?
C30 P3 C31 C32 -170.5(6) . . . . ?
C37 P3 C31 C32 80.5(7) . . . . ?
W1 P3 C31 C32 -44.4(7) . . . . ?
C36 C31 C32 C33 3.0(13) . . . . ?
P3 C31 C32 C33 -178.5(7) . . . . ?
C31 C32 C33 C34 -4.5(14) . . . . ?
C32 C33 C34 C35 3.7(15) . . . . ?
C33 C34 C35 C36 -1.4(16) . . . . ?
C32 C31 C36 C35 -0.7(12) . . . . ?
P3 C31 C36 C35 -179.0(7) . . . . ?
C34 C35 C36 C31 -0.1(14) . . . . ?
C30 P3 C37 C42 -15.7(8) . . . . ?
C31 P3 C37 C42 94.5(8) . . . . ?
W1 P3 C37 C42 -141.4(7) . . . . ?
C30 P3 C37 C38 165.8(7) . . . . ?
C31 P3 C37 C38 -84.0(8) . . . . ?
W1 P3 C37 C38 40.1(8) . . . . ?
C42 C37 C38 C39 0.4(14) . . . . ?
P3 C37 C38 C39 179.0(8) . . . . ?
C37 C38 C39 C40 1.5(16) . . . . ?
C38 C39 C40 C41 -2.5(16) . . . . ?
C39 C40 C41 C42 1.7(14) . . . . ?
C38 C37 C42 C41 -1.2(13) . . . . ?
P3 C37 C42 C41 -179.7(7) . . . . ?
C40 C41 C42 C37 0.1(14) . . . . ?
P1 C4 B1 C43 167.3(5) . . . . ?
P1 C4 B1 C17 47.1(7) . . . . ?
P1 C4 B1 C30 -78.4(7) . . . . ?
P2 C17 B1 C43 151.7(5) . . . . ?
P2 C17 B1 C4 -88.2(6) . . . . ?
P2 C17 B1 C30 36.6(8) . . . . ?
P3 C30 B1 C43 156.8(5) . . . . ?
P3 C30 B1 C4 39.6(7) . . . . ?
P3 C30 B1 C17 -84.9(7) . . . . ?
C4 B1 C43 C48 -172.4(7) . . . . ?
C17 B1 C43 C48 -51.5(9) . . . . ?
C30 B1 C43 C48 68.8(8) . . . . ?
C4 B1 C43 C44 7.4(10) . . . . ?
C17 B1 C43 C44 128.4(7) . . . . ?
C30 B1 C43 C44 -111.4(7) . . . . ?
C4 B1 C43 W2 -83.8(7) . . . . ?
C17 B1 C43 W2 37.2(8) . . . . ?
C30 B1 C43 W2 157.5(5) . . . . ?
C48 C43 C44 C45 -0.2(11) . . . . ?
B1 C43 C44 C45 180.0(7) . . . . ?
W2 C43 C44 C45 -56.8(7) . . . . ?
C48 C43 C44 W2 56.6(6) . . . . ?
B1 C43 C44 W2 -123.2(7) . . . . ?
C43 C44 C45 C46 1.3(12) . . . . ?
W2 C44 C45 C46 -56.1(7) . . . . ?
C43 C44 C45 W2 57.4(7) . . . . ?
C44 C45 C46 C47 -3.4(12) . . . . ?
W2 C45 C46 C47 -59.8(7) . . . . ?
C44 C45 C46 W2 56.5(7) . . . . ?
C45 C46 C47 C48 4.4(12) . . . . ?
W2 C46 C47 C48 -55.3(7) . . . . ?
C45 C46 C47 W2 59.7(7) . . . . ?
C46 C47 C48 C43 -3.4(12) . . . . ?
W2 C47 C48 C43 -58.6(7) . . . . ?
C46 C47 C48 W2 55.3(7) . . . . ?
C44 C43 C48 C47 1.2(11) . . . . ?
B1 C43 C48 C47 -178.9(7) . . . . ?
W2 C43 C48 C47 58.0(7) . . . . ?
C44 C43 C48 W2 -56.8(6) . . . . ?
B1 C43 C48 W2 123.0(6) . . . . ?
C56 N1 C52 C53 56.7(15) . . . . ?
C54 N1 C52 C53 -62.2(15) . . . . ?
C58 N1 C52 C53 176.3(13) . . . . ?
C56 N1 C54 C55 176.9(12) . . . . ?
C52 N1 C54 C55 -60.0(15) . . . . ?
C58 N1 C54 C55 57.2(14) . . . . ?
C54 N1 C56 C57 177.7(13) . . . . ?
C52 N1 C56 C57 56.0(16) . . . . ?
C58 N1 C56 C57 -60.9(16) . . . . ?
C56 N1 C58 C59 -66.4(17) . . . . ?
C54 N1 C58 C59 51.3(17) . . . . ?
C52 N1 C58 C59 171.8(15) . . . . ?

_refine_diff_density_max         1.157
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.116

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/E2O'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_14158a
_database_code_depnum_ccdc_archive 'CCDC 1039152'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        '[Et4N][Cr(CO)3(PhBP3)]'
_chemical_name_common            14158a
_chemical_melting_point          513-514
_chemical_formula_moiety         'C48 H41 B Cr O3 P3, C8 H20 N'
_chemical_formula_sum            'C56 H61 B Cr N O3 P3'
_chemical_formula_weight         951.77

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'
N N 0.0061 0.0033 '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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -z-1/2'

_cell_length_a                   21.680(2)
_cell_length_b                   20.2863(19)
_cell_length_c                   21.999(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9675.2(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2983
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      27.34

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             4016
_exptl_transmission_factor_min   0.7495
_exptl_transmission_factor_max   0.9148
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.382
_shelx_estimated_absorpt_T_min   0.934
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7495
_exptl_absorpt_correction_T_max  0.9148
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'

_exptl_special_details           
;
 'Prof. P. Fischer'
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38218
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.851
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             10804
_reflns_number_gt                7137
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          'Prof. P. Fischer'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0365P)²+5.0957P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10804
_refine_ls_number_parameters     590
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0475
_refine_ls_wR_factor_ref         0.1117
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_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
Cr1 Cr 0.21237(2) 0.34144(2) 0.13527(2) 0.01522(10) Uani 1 1 d . . . . .
P1 P 0.19993(3) 0.22411(3) 0.13017(3) 0.01636(15) Uani 1 1 d . . . . .
P2 P 0.25369(3) 0.32875(3) 0.03405(3) 0.01560(14) Uani 1 1 d . . . . .
P3 P 0.31652(3) 0.32144(3) 0.16932(3) 0.01624(15) Uani 1 1 d . . . . .
C1 C 0.13554(13) 0.36146(13) 0.10728(11) 0.0212(6) Uani 1 1 d . . . . .
O1 O 0.08688(9) 0.38217(10) 0.09437(9) 0.0336(5) Uani 1 1 d . . . . .
C2 C 0.17697(13) 0.34468(12) 0.21087(12) 0.0205(6) Uani 1 1 d . . . . .
O2 O 0.15013(9) 0.35166(9) 0.25653(8) 0.0312(5) Uani 1 1 d . . . . .
C3 C 0.21747(12) 0.43092(13) 0.14337(11) 0.0205(6) Uani 1 1 d . . . . .
O3 O 0.21319(9) 0.48786(9) 0.15220(8) 0.0313(5) Uani 1 1 d . . . . .
B1 B 0.32456(14) 0.21542(14) 0.08096(12) 0.0166(6) Uani 1 1 d . . . . .
C4 C 0.25617(11) 0.17941(12) 0.08417(11) 0.0178(5) Uani 1 1 d . . . . .
H4A H 0.2613 0.1345 0.1011 0.021 Uiso 1 1 calc R U . . .
H4B H 0.2398 0.1748 0.0424 0.021 Uiso 1 1 calc R U . . .
C5 C 0.20258(12) 0.17492(12) 0.20100(11) 0.0191(6) Uani 1 1 d . . . . .
C6 C 0.18688(13) 0.10808(13) 0.19858(12) 0.0250(6) Uani 1 1 d . . . . .
H6A H 0.1712 0.0899 0.1619 0.030 Uiso 1 1 calc R U . . .
C7 C 0.19394(14) 0.06813(14) 0.24903(14) 0.0308(7) Uani 1 1 d . . . . .
H7A H 0.1826 0.0230 0.2469 0.037 Uiso 1 1 calc R U . . .
C8 C 0.21742(14) 0.09349(14) 0.30244(13) 0.0312(7) Uani 1 1 d . . . . .
H8A H 0.2233 0.0656 0.3367 0.037 Uiso 1 1 calc R U . . .
C9 C 0.23224(13) 0.15888(14) 0.30592(12) 0.0284(7) Uani 1 1 d . . . . .
H9A H 0.2481 0.1765 0.3428 0.034 Uiso 1 1 calc R U . . .
C10 C 0.22418(12) 0.19985(13) 0.25570(11) 0.0215(6) Uani 1 1 d . . . . .
H10A H 0.2336 0.2454 0.2590 0.026 Uiso 1 1 calc R U . . .
C11 C 0.12327(12) 0.19891(12) 0.10323(12) 0.0207(6) Uani 1 1 d . . . . .
C12 C 0.11277(14) 0.16471(14) 0.04985(13) 0.0305(7) Uani 1 1 d . . . . .
H12A H 0.1466 0.1524 0.0249 0.037 Uiso 1 1 calc R U . . .
C13 C 0.05291(16) 0.14810(16) 0.03232(15) 0.0423(8) Uani 1 1 d . . . . .
H13A H 0.0464 0.1250 -0.0047 0.051 Uiso 1 1 calc R U . . .
C14 C 0.00362(15) 0.16474(17) 0.06782(16) 0.0465(9) Uani 1 1 d . . . . .
H14A H -0.0370 0.1529 0.0560 0.056 Uiso 1 1 calc R U . . .
C15 C 0.01350(15) 0.19891(17) 0.12095(17) 0.0467(9) Uani 1 1 d . . . . .
H15A H -0.0205 0.2105 0.1460 0.056 Uiso 1 1 calc R U . . .
C16 C 0.07255(14) 0.21645(15) 0.13815(15) 0.0367(7) Uani 1 1 d . . . . .
H16A H 0.0785 0.2409 0.1745 0.044 Uiso 1 1 calc R U . . .
C17 C 0.32358(12) 0.27967(12) 0.03310(11) 0.0172(5) Uani 1 1 d . . . . .
H17A H 0.3300 0.2630 -0.0087 0.021 Uiso 1 1 calc R U . . .
H17B H 0.3588 0.3088 0.0430 0.021 Uiso 1 1 calc R U . . .
C18 C 0.20394(12) 0.28967(12) -0.02411(11) 0.0184(6) Uani 1 1 d . . . . .
C19 C 0.22346(13) 0.23697(12) -0.06026(11) 0.0216(6) Uani 1 1 d . . . . .
H19A H 0.2636 0.2191 -0.0545 0.026 Uiso 1 1 calc R U . . .
C20 C 0.18496(13) 0.21034(13) -0.10450(12) 0.0250(6) Uani 1 1 d . . . . .
H20A H 0.1992 0.1749 -0.1290 0.030 Uiso 1 1 calc R U . . .
C21 C 0.12672(13) 0.23465(14) -0.11312(12) 0.0263(6) Uani 1 1 d . . . . .
H21A H 0.1005 0.2162 -0.1433 0.032 Uiso 1 1 calc R U . . .
C22 C 0.10647(14) 0.28635(14) -0.07734(12) 0.0300(7) Uani 1 1 d . . . . .
H22A H 0.0660 0.3033 -0.0828 0.036 Uiso 1 1 calc R U . . .
C23 C 0.14478(13) 0.31363(14) -0.03357(12) 0.0251(6) Uani 1 1 d . . . . .
H23A H 0.1302 0.3494 -0.0096 0.030 Uiso 1 1 calc R U . . .
C24 C 0.27511(12) 0.40442(12) -0.00758(11) 0.0192(6) Uani 1 1 d . . . . .
C25 C 0.32666(13) 0.40565(13) -0.04520(12) 0.0265(6) Uani 1 1 d . . . . .
H25A H 0.3492 0.3662 -0.0522 0.032 Uiso 1 1 calc R U . . .
C26 C 0.34555(14) 0.46375(14) -0.07263(13) 0.0321(7) Uani 1 1 d . . . . .
H26A H 0.3815 0.4640 -0.0974 0.038 Uiso 1 1 calc R U . . .
C27 C 0.31264(14) 0.52112(14) -0.06429(13) 0.0318(7) Uani 1 1 d . . . . .
H27A H 0.3258 0.5609 -0.0831 0.038 Uiso 1 1 calc R U . . .
C28 C 0.26046(14) 0.52050(13) -0.02851(12) 0.0301(7) Uani 1 1 d . . . . .
H28A H 0.2372 0.5597 -0.0231 0.036 Uiso 1 1 calc R U . . .
C29 C 0.24196(13) 0.46264(13) -0.00049(11) 0.0248(6) Uani 1 1 d . . . . .
H29A H 0.2059 0.4627 0.0241 0.030 Uiso 1 1 calc R U . . .
C30 C 0.34599(12) 0.24002(12) 0.15001(11) 0.0171(5) Uani 1 1 d . . . . .
H30A H 0.3916 0.2407 0.1522 0.021 Uiso 1 1 calc R U . . .
H30B H 0.3310 0.2078 0.1804 0.021 Uiso 1 1 calc R U . . .
C31 C 0.37888(12) 0.37710(12) 0.14147(11) 0.0189(6) Uani 1 1 d . . . . .
C32 C 0.44094(13) 0.35908(14) 0.14452(13) 0.0285(7) Uani 1 1 d . . . . .
H32A H 0.4520 0.3181 0.1623 0.034 Uiso 1 1 calc R U . . .
C33 C 0.48669(14) 0.40024(15) 0.12196(14) 0.0341(7) Uani 1 1 d . . . . .
H33A H 0.5287 0.3870 0.1241 0.041 Uiso 1 1 calc R U . . .
C34 C 0.47147(14) 0.46040(14) 0.09642(13) 0.0312(7) Uani 1 1 d . . . . .
H34A H 0.5027 0.4883 0.0805 0.037 Uiso 1 1 calc R U . . .
C35 C 0.41119(14) 0.47928(14) 0.09434(13) 0.0305(7) Uani 1 1 d . . . . .
H35A H 0.4006 0.5209 0.0775 0.037 Uiso 1 1 calc R U . . .
C36 C 0.36492(13) 0.43822(13) 0.11672(12) 0.0259(6) Uani 1 1 d . . . . .
H36A H 0.3232 0.4523 0.1150 0.031 Uiso 1 1 calc R U . . .
C37 C 0.32932(12) 0.33297(12) 0.25157(11) 0.0181(5) Uani 1 1 d . . . . .
C38 C 0.36150(13) 0.28901(14) 0.28813(12) 0.0282(7) Uani 1 1 d . . . . .
H38A H 0.3778 0.2498 0.2708 0.034 Uiso 1 1 calc R U . . .
C39 C 0.37016(14) 0.30161(15) 0.34974(12) 0.0332(7) Uani 1 1 d . . . . .
H39A H 0.3920 0.2709 0.3742 0.040 Uiso 1 1 calc R U . . .
C40 C 0.34713(13) 0.35843(14) 0.37533(12) 0.0260(6) Uani 1 1 d . . . . .
H40A H 0.3539 0.3675 0.4172 0.031 Uiso 1 1 calc R U . . .
C41 C 0.31419(13) 0.40222(13) 0.33997(12) 0.0245(6) Uani 1 1 d . . . . .
H41A H 0.2979 0.4413 0.3575 0.029 Uiso 1 1 calc R U . . .
C42 C 0.30494(12) 0.38893(12) 0.27869(11) 0.0198(6) Uani 1 1 d . . . . .
H42A H 0.2814 0.4188 0.2548 0.024 Uiso 1 1 calc R U . . .
C43 C 0.37623(12) 0.16444(12) 0.05332(11) 0.0166(5) Uani 1 1 d . . . . .
C44 C 0.36917(12) 0.09613(12) 0.05000(11) 0.0186(6) Uani 1 1 d . . . . .
H44A H 0.3340 0.0766 0.0684 0.022 Uiso 1 1 calc R U . . .
C45 C 0.41163(13) 0.05567(13) 0.02085(11) 0.0224(6) Uani 1 1 d . . . . .
H45A H 0.4050 0.0094 0.0195 0.027 Uiso 1 1 calc R U . . .
C46 C 0.46335(12) 0.08228(13) -0.00606(11) 0.0223(6) Uani 1 1 d . . . . .
H46A H 0.4918 0.0548 -0.0269 0.027 Uiso 1 1 calc R U . . .
C47 C 0.47331(12) 0.14940(13) -0.00228(12) 0.0229(6) Uani 1 1 d . . . . .
H47A H 0.5091 0.1683 -0.0201 0.027 Uiso 1 1 calc R U . . .
C48 C 0.43089(12) 0.18909(13) 0.02763(11) 0.0213(6) Uani 1 1 d . . . . .
H48A H 0.4392 0.2349 0.0309 0.026 Uiso 1 1 calc R U . . .
N1 N 0.49415(12) 0.03724(14) 0.20379(11) 0.0388(7) Uani 1 1 d . . . . .
C49 C 0.50874(15) 0.04093(18) 0.13668(13) 0.0411(8) Uani 1 1 d . . . . .
H49A H 0.4904 0.0020 0.1165 0.049 Uiso 1 1 calc R U . . .
H49B H 0.4884 0.0806 0.1197 0.049 Uiso 1 1 calc R U . . .
C50 C 0.57638(15) 0.04370(17) 0.12073(14) 0.0420(8) Uani 1 1 d . . . . .
H50A H 0.5810 0.0490 0.0767 0.063 Uiso 1 1 calc R U . . .
H50B H 0.5965 0.0027 0.1336 0.063 Uiso 1 1 calc R U . . .
H50C H 0.5956 0.0812 0.1415 0.063 Uiso 1 1 calc R U . . .
C51 C 0.51865(17) 0.09723(17) 0.23674(14) 0.0460(9) Uani 1 1 d . . . . .
H51A H 0.5641 0.0981 0.2324 0.055 Uiso 1 1 calc R U . . .
H51B H 0.5092 0.0926 0.2806 0.055 Uiso 1 1 calc R U . . .
C52 C 0.49291(19) 0.16271(18) 0.21460(15) 0.0597(11) Uani 1 1 d . . . . .
H52A H 0.5135 0.1989 0.2360 0.090 Uiso 1 1 calc R U . . .
H52B H 0.4485 0.1644 0.2227 0.090 Uiso 1 1 calc R U . . .
H52C H 0.5001 0.1670 0.1708 0.090 Uiso 1 1 calc R U . . .
C53 C 0.52533(16) -0.02208(16) 0.23266(14) 0.0431(9) Uani 1 1 d . . . . .
H53A H 0.5705 -0.0172 0.2276 0.052 Uiso 1 1 calc R U . . .
H53B H 0.5166 -0.0214 0.2768 0.052 Uiso 1 1 calc R U . . .
C54 C 0.50660(18) -0.08863(18) 0.20789(16) 0.0535(10) Uani 1 1 d . . . . .
H54A H 0.5318 -0.1231 0.2269 0.080 Uiso 1 1 calc R U . . .
H54B H 0.5129 -0.0894 0.1638 0.080 Uiso 1 1 calc R U . . .
H54C H 0.4630 -0.0966 0.2169 0.080 Uiso 1 1 calc R U . . .
C55 C 0.42431(15) 0.0312(2) 0.20730(15) 0.0563(11) Uani 1 1 d . . . . .
H55A H 0.4058 0.0690 0.1855 0.068 Uiso 1 1 calc R U . . .
H55B H 0.4117 -0.0094 0.1857 0.068 Uiso 1 1 calc R U . . .
C56 C 0.39805(19) 0.0291(2) 0.27104(16) 0.0733(13) Uani 1 1 d . . . . .
H56A H 0.3532 0.0232 0.2690 0.110 Uiso 1 1 calc R U . . .
H56B H 0.4075 0.0706 0.2920 0.110 Uiso 1 1 calc R U . . .
H56C H 0.4165 -0.0077 0.2934 0.110 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1 C1 1.821(3) . ?
Cr1 C3 1.827(3) . ?
Cr1 C2 1.833(3) . ?
Cr1 P1 2.3981(8) . ?
Cr1 P3 2.4134(8) . ?
Cr1 P2 2.4139(8) . ?
P1 C4 1.826(2) . ?
P1 C11 1.837(3) . ?
P1 C5 1.851(3) . ?
P2 C17 1.813(2) . ?
P2 C24 1.847(3) . ?
P2 C18 1.852(3) . ?
P3 C30 1.821(2) . ?
P3 C37 1.845(2) . ?
P3 C31 1.865(3) . ?
C1 O1 1.171(3) . ?
C2 O2 1.169(3) . ?
C3 O3 1.175(3) . ?
B1 C43 1.641(4) . ?
B1 C4 1.654(4) . ?
B1 C30 1.665(4) . ?
B1 C17 1.676(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.387(3) . ?
C5 C6 1.399(4) . ?
C6 C7 1.383(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.380(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.367(4) . ?
C8 H8A 0.9500 . ?
C9 C10 1.393(3) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C12 1.383(4) . ?
C11 C16 1.388(4) . ?
C12 C13 1.395(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.366(5) . ?
C13 H13A 0.9500 . ?
C14 C15 1.376(5) . ?
C14 H14A 0.9500 . ?
C15 C16 1.382(4) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C23 1.387(4) . ?
C18 C19 1.398(3) . ?
C19 C20 1.391(4) . ?
C19 H19A 0.9500 . ?
C20 C21 1.369(4) . ?
C20 H20A 0.9500 . ?
C21 C22 1.383(4) . ?
C21 H21A 0.9500 . ?
C22 C23 1.387(4) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 C25 1.391(4) . ?
C24 C29 1.391(3) . ?
C25 C26 1.386(4) . ?
C25 H25A 0.9500 . ?
C26 C27 1.377(4) . ?
C26 H26A 0.9500 . ?
C27 C28 1.378(4) . ?
C27 H27A 0.9500 . ?
C28 C29 1.385(4) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C36 1.388(4) . ?
C31 C32 1.396(4) . ?
C32 C33 1.388(4) . ?
C32 H32A 0.9500 . ?
C33 C34 1.384(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.363(4) . ?
C34 H34A 0.9500 . ?
C35 C36 1.394(4) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 C42 1.387(3) . ?
C37 C38 1.389(3) . ?
C38 C39 1.392(4) . ?
C38 H38A 0.9500 . ?
C39 C40 1.376(4) . ?
C39 H39A 0.9500 . ?
C40 C41 1.380(4) . ?
C40 H40A 0.9500 . ?
C41 C42 1.389(3) . ?
C41 H41A 0.9500 . ?
C42 H42A 0.9500 . ?
C43 C44 1.396(3) . ?
C43 C48 1.405(3) . ?
C44 C45 1.390(3) . ?
C44 H44A 0.9500 . ?
C45 C46 1.378(4) . ?
C45 H45A 0.9500 . ?
C46 C47 1.381(3) . ?
C46 H46A 0.9500 . ?
C47 C48 1.388(3) . ?
C47 H47A 0.9500 . ?
C48 H48A 0.9500 . ?
N1 C49 1.512(4) . ?
N1 C51 1.513(4) . ?
N1 C53 1.519(4) . ?
N1 C55 1.521(4) . ?
C49 C50 1.509(4) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.521(4) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.511(4) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.514(4) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?

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
C1 Cr1 C3 82.35(12) . . ?
C1 Cr1 C2 85.18(11) . . ?
C3 Cr1 C2 84.33(11) . . ?
C1 Cr1 P1 95.90(9) . . ?
C3 Cr1 P1 175.84(8) . . ?
C2 Cr1 P1 91.77(8) . . ?
C1 Cr1 P3 176.28(9) . . ?
C3 Cr1 P3 94.59(8) . . ?
C2 Cr1 P3 96.66(9) . . ?
P1 Cr1 P3 87.30(3) . . ?
C1 Cr1 P2 92.94(8) . . ?
C3 Cr1 P2 99.99(8) . . ?
C2 Cr1 P2 175.04(9) . . ?
P1 Cr1 P2 83.84(2) . . ?
P3 Cr1 P2 85.48(3) . . ?
C4 P1 C11 106.69(12) . . ?
C4 P1 C5 100.26(11) . . ?
C11 P1 C5 98.61(12) . . ?
C4 P1 Cr1 116.35(8) . . ?
C11 P1 Cr1 113.14(8) . . ?
C5 P1 Cr1 119.49(8) . . ?
C17 P2 C24 103.91(12) . . ?
C17 P2 C18 104.11(11) . . ?
C24 P2 C18 99.19(11) . . ?
C17 P2 Cr1 112.29(8) . . ?
C24 P2 Cr1 117.52(8) . . ?
C18 P2 Cr1 117.83(8) . . ?
C30 P3 C37 106.91(11) . . ?
C30 P3 C31 102.60(12) . . ?
C37 P3 C31 97.84(11) . . ?
C30 P3 Cr1 114.10(8) . . ?
C37 P3 Cr1 115.07(9) . . ?
C31 P3 Cr1 118.33(9) . . ?
O1 C1 Cr1 170.4(2) . . ?
O2 C2 Cr1 172.8(2) . . ?
O3 C3 Cr1 171.1(2) . . ?
C43 B1 C4 110.4(2) . . ?
C43 B1 C30 109.7(2) . . ?
C4 B1 C30 110.1(2) . . ?
C43 B1 C17 105.4(2) . . ?
C4 B1 C17 111.0(2) . . ?
C30 B1 C17 110.1(2) . . ?
B1 C4 P1 113.76(17) . . ?
B1 C4 H4A 108.8 . . ?
P1 C4 H4A 108.8 . . ?
B1 C4 H4B 108.8 . . ?
P1 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C10 C5 C6 117.9(2) . . ?
C10 C5 P1 122.98(19) . . ?
C6 C5 P1 118.9(2) . . ?
C7 C6 C5 120.7(3) . . ?
C7 C6 H6A 119.6 . . ?
C5 C6 H6A 119.6 . . ?
C8 C7 C6 120.4(3) . . ?
C8 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C9 C8 C7 119.8(3) . . ?
C9 C8 H8A 120.1 . . ?
C7 C8 H8A 120.1 . . ?
C8 C9 C10 120.3(3) . . ?
C8 C9 H9A 119.8 . . ?
C10 C9 H9A 119.8 . . ?
C5 C10 C9 120.9(2) . . ?
C5 C10 H10A 119.6 . . ?
C9 C10 H10A 119.6 . . ?
C12 C11 C16 117.9(3) . . ?
C12 C11 P1 124.2(2) . . ?
C16 C11 P1 117.8(2) . . ?
C11 C12 C13 120.6(3) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C14 C13 C12 120.7(3) . . ?
C14 C13 H13A 119.7 . . ?
C12 C13 H13A 119.7 . . ?
C13 C14 C15 119.2(3) . . ?
C13 C14 H14A 120.4 . . ?
C15 C14 H14A 120.4 . . ?
C14 C15 C16 120.4(3) . . ?
C14 C15 H15A 119.8 . . ?
C16 C15 H15A 119.8 . . ?
C15 C16 C11 121.1(3) . . ?
C15 C16 H16A 119.4 . . ?
C11 C16 H16A 119.4 . . ?
B1 C17 P2 115.50(17) . . ?
B1 C17 H17A 108.4 . . ?
P2 C17 H17A 108.4 . . ?
B1 C17 H17B 108.4 . . ?
P2 C17 H17B 108.4 . . ?
H17A C17 H17B 107.5 . . ?
C23 C18 C19 117.5(2) . . ?
C23 C18 P2 119.48(19) . . ?
C19 C18 P2 123.0(2) . . ?
C20 C19 C18 120.9(3) . . ?
C20 C19 H19A 119.6 . . ?
C18 C19 H19A 119.6 . . ?
C21 C20 C19 120.7(3) . . ?
C21 C20 H20A 119.7 . . ?
C19 C20 H20A 119.7 . . ?
C20 C21 C22 119.2(3) . . ?
C20 C21 H21A 120.4 . . ?
C22 C21 H21A 120.4 . . ?
C21 C22 C23 120.5(3) . . ?
C21 C22 H22A 119.7 . . ?
C23 C22 H22A 119.7 . . ?
C22 C23 C18 121.2(3) . . ?
C22 C23 H23A 119.4 . . ?
C18 C23 H23A 119.4 . . ?
C25 C24 C29 117.8(2) . . ?
C25 C24 P2 120.80(19) . . ?
C29 C24 P2 121.3(2) . . ?
C26 C25 C24 120.8(3) . . ?
C26 C25 H25A 119.6 . . ?
C24 C25 H25A 119.6 . . ?
C27 C26 C25 120.5(3) . . ?
C27 C26 H26A 119.7 . . ?
C25 C26 H26A 119.7 . . ?
C26 C27 C28 119.6(3) . . ?
C26 C27 H27A 120.2 . . ?
C28 C27 H27A 120.2 . . ?
C27 C28 C29 120.0(3) . . ?
C27 C28 H28A 120.0 . . ?
C29 C28 H28A 120.0 . . ?
C28 C29 C24 121.3(3) . . ?
C28 C29 H29A 119.3 . . ?
C24 C29 H29A 119.3 . . ?
B1 C30 P3 112.75(17) . . ?
B1 C30 H30A 109.0 . . ?
P3 C30 H30A 109.0 . . ?
B1 C30 H30B 109.0 . . ?
P3 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
C36 C31 C32 117.6(2) . . ?
C36 C31 P3 120.8(2) . . ?
C32 C31 P3 121.6(2) . . ?
C33 C32 C31 120.9(3) . . ?
C33 C32 H32A 119.5 . . ?
C31 C32 H32A 119.5 . . ?
C34 C33 C32 120.3(3) . . ?
C34 C33 H33A 119.8 . . ?
C32 C33 H33A 119.8 . . ?
C35 C34 C33 119.4(3) . . ?
C35 C34 H34A 120.3 . . ?
C33 C34 H34A 120.3 . . ?
C34 C35 C36 120.7(3) . . ?
C34 C35 H35A 119.7 . . ?
C36 C35 H35A 119.7 . . ?
C31 C36 C35 121.0(3) . . ?
C31 C36 H36A 119.5 . . ?
C35 C36 H36A 119.5 . . ?
C42 C37 C38 117.9(2) . . ?
C42 C37 P3 117.91(19) . . ?
C38 C37 P3 124.19(19) . . ?
C37 C38 C39 120.9(3) . . ?
C37 C38 H38A 119.5 . . ?
C39 C38 H38A 119.5 . . ?
C40 C39 C38 120.2(3) . . ?
C40 C39 H39A 119.9 . . ?
C38 C39 H39A 119.9 . . ?
C39 C40 C41 119.7(2) . . ?
C39 C40 H40A 120.1 . . ?
C41 C40 H40A 120.1 . . ?
C40 C41 C42 119.8(3) . . ?
C40 C41 H41A 120.1 . . ?
C42 C41 H41A 120.1 . . ?
C37 C42 C41 121.4(2) . . ?
C37 C42 H42A 119.3 . . ?
C41 C42 H42A 119.3 . . ?
C44 C43 C48 115.1(2) . . ?
C44 C43 B1 124.8(2) . . ?
C48 C43 B1 120.0(2) . . ?
C45 C44 C43 122.5(2) . . ?
C45 C44 H44A 118.7 . . ?
C43 C44 H44A 118.7 . . ?
C46 C45 C44 120.4(2) . . ?
C46 C45 H45A 119.8 . . ?
C44 C45 H45A 119.8 . . ?
C45 C46 C47 119.2(2) . . ?
C45 C46 H46A 120.4 . . ?
C47 C46 H46A 120.4 . . ?
C46 C47 C48 119.8(3) . . ?
C46 C47 H47A 120.1 . . ?
C48 C47 H47A 120.1 . . ?
C47 C48 C43 122.9(2) . . ?
C47 C48 H48A 118.6 . . ?
C43 C48 H48A 118.6 . . ?
C49 N1 C51 110.8(3) . . ?
C49 N1 C53 110.8(2) . . ?
C51 N1 C53 106.3(2) . . ?
C49 N1 C55 105.2(2) . . ?
C51 N1 C55 112.9(3) . . ?
C53 N1 C55 111.0(3) . . ?
C50 C49 N1 115.6(3) . . ?
C50 C49 H49A 108.4 . . ?
N1 C49 H49A 108.4 . . ?
C50 C49 H49B 108.4 . . ?
N1 C49 H49B 108.4 . . ?
H49A C49 H49B 107.4 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N1 C51 C52 114.9(3) . . ?
N1 C51 H51A 108.6 . . ?
C52 C51 H51A 108.6 . . ?
N1 C51 H51B 108.6 . . ?
C52 C51 H51B 108.6 . . ?
H51A C51 H51B 107.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 N1 115.9(3) . . ?
C54 C53 H53A 108.3 . . ?
N1 C53 H53A 108.3 . . ?
C54 C53 H53B 108.3 . . ?
N1 C53 H53B 108.3 . . ?
H53A C53 H53B 107.4 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C55 N1 115.1(3) . . ?
C56 C55 H55A 108.5 . . ?
N1 C55 H55A 108.5 . . ?
C56 C55 H55B 108.5 . . ?
N1 C55 H55B 108.5 . . ?
H55A C55 H55B 107.5 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?

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
C43 B1 C4 P1 166.35(16) . . . . ?
C30 B1 C4 P1 45.1(2) . . . . ?
C17 B1 C4 P1 -77.1(2) . . . . ?
C11 P1 C4 B1 156.53(17) . . . . ?
C5 P1 C4 B1 -101.17(19) . . . . ?
Cr1 P1 C4 B1 29.2(2) . . . . ?
C4 P1 C5 C10 114.3(2) . . . . ?
C11 P1 C5 C10 -136.9(2) . . . . ?
Cr1 P1 C5 C10 -14.1(3) . . . . ?
C4 P1 C5 C6 -60.4(2) . . . . ?
C11 P1 C5 C6 48.5(2) . . . . ?
Cr1 P1 C5 C6 171.28(17) . . . . ?
C10 C5 C6 C7 -1.2(4) . . . . ?
P1 C5 C6 C7 173.7(2) . . . . ?
C5 C6 C7 C8 -0.9(4) . . . . ?
C6 C7 C8 C9 1.7(4) . . . . ?
C7 C8 C9 C10 -0.5(4) . . . . ?
C6 C5 C10 C9 2.5(4) . . . . ?
P1 C5 C10 C9 -172.2(2) . . . . ?
C8 C9 C10 C5 -1.7(4) . . . . ?
C4 P1 C11 C12 -13.0(3) . . . . ?
C5 P1 C11 C12 -116.5(2) . . . . ?
Cr1 P1 C11 C12 116.2(2) . . . . ?
C4 P1 C11 C16 168.2(2) . . . . ?
C5 P1 C11 C16 64.7(2) . . . . ?
Cr1 P1 C11 C16 -62.6(2) . . . . ?
C16 C11 C12 C13 -0.5(4) . . . . ?
P1 C11 C12 C13 -179.3(2) . . . . ?
C11 C12 C13 C14 -0.6(5) . . . . ?
C12 C13 C14 C15 0.8(5) . . . . ?
C13 C14 C15 C16 0.2(5) . . . . ?
C14 C15 C16 C11 -1.4(5) . . . . ?
C12 C11 C16 C15 1.6(4) . . . . ?
P1 C11 C16 C15 -179.6(2) . . . . ?
C43 B1 C17 P2 157.88(17) . . . . ?
C4 B1 C17 P2 38.3(2) . . . . ?
C30 B1 C17 P2 -83.9(2) . . . . ?
C24 P2 C17 B1 166.35(17) . . . . ?
C18 P2 C17 B1 -90.24(19) . . . . ?
Cr1 P2 C17 B1 38.32(19) . . . . ?
C17 P2 C18 C23 177.3(2) . . . . ?
C24 P2 C18 C23 -75.7(2) . . . . ?
Cr1 P2 C18 C23 52.2(2) . . . . ?
C17 P2 C18 C19 -3.7(2) . . . . ?
C24 P2 C18 C19 103.3(2) . . . . ?
Cr1 P2 C18 C19 -128.78(19) . . . . ?
C23 C18 C19 C20 0.8(4) . . . . ?
P2 C18 C19 C20 -178.30(19) . . . . ?
C18 C19 C20 C21 -0.8(4) . . . . ?
C19 C20 C21 C22 0.2(4) . . . . ?
C20 C21 C22 C23 0.5(4) . . . . ?
C21 C22 C23 C18 -0.5(4) . . . . ?
C19 C18 C23 C22 -0.1(4) . . . . ?
P2 C18 C23 C22 179.0(2) . . . . ?
C17 P2 C24 C25 18.3(2) . . . . ?
C18 P2 C24 C25 -88.8(2) . . . . ?
Cr1 P2 C24 C25 143.03(19) . . . . ?
C17 P2 C24 C29 -159.0(2) . . . . ?
C18 P2 C24 C29 93.9(2) . . . . ?
Cr1 P2 C24 C29 -34.3(2) . . . . ?
C29 C24 C25 C26 2.5(4) . . . . ?
P2 C24 C25 C26 -174.8(2) . . . . ?
C24 C25 C26 C27 -1.6(4) . . . . ?
C25 C26 C27 C28 -0.2(5) . . . . ?
C26 C27 C28 C29 1.0(4) . . . . ?
C27 C28 C29 C24 0.0(4) . . . . ?
C25 C24 C29 C28 -1.8(4) . . . . ?
P2 C24 C29 C28 175.6(2) . . . . ?
C43 B1 C30 P3 152.05(17) . . . . ?
C4 B1 C30 P3 -86.2(2) . . . . ?
C17 B1 C30 P3 36.5(3) . . . . ?
C37 P3 C30 B1 167.67(18) . . . . ?
C31 P3 C30 B1 -89.97(19) . . . . ?
Cr1 P3 C30 B1 39.3(2) . . . . ?
C30 P3 C31 C36 144.6(2) . . . . ?
C37 P3 C31 C36 -106.0(2) . . . . ?
Cr1 P3 C31 C36 18.1(2) . . . . ?
C30 P3 C31 C32 -35.2(2) . . . . ?
C37 P3 C31 C32 74.1(2) . . . . ?
Cr1 P3 C31 C32 -161.79(19) . . . . ?
C36 C31 C32 C33 -1.8(4) . . . . ?
P3 C31 C32 C33 178.1(2) . . . . ?
C31 C32 C33 C34 0.6(4) . . . . ?
C32 C33 C34 C35 0.9(4) . . . . ?
C33 C34 C35 C36 -1.0(4) . . . . ?
C32 C31 C36 C35 1.6(4) . . . . ?
P3 C31 C36 C35 -178.3(2) . . . . ?
C34 C35 C36 C31 -0.2(4) . . . . ?
C30 P3 C37 C42 -173.5(2) . . . . ?
C31 P3 C37 C42 80.7(2) . . . . ?
Cr1 P3 C37 C42 -45.7(2) . . . . ?
C30 P3 C37 C38 6.1(3) . . . . ?
C31 P3 C37 C38 -99.7(3) . . . . ?
Cr1 P3 C37 C38 133.9(2) . . . . ?
C42 C37 C38 C39 -1.4(4) . . . . ?
P3 C37 C38 C39 178.9(2) . . . . ?
C37 C38 C39 C40 -0.5(5) . . . . ?
C38 C39 C40 C41 1.5(5) . . . . ?
C39 C40 C41 C42 -0.5(4) . . . . ?
C38 C37 C42 C41 2.4(4) . . . . ?
P3 C37 C42 C41 -178.0(2) . . . . ?
C40 C41 C42 C37 -1.4(4) . . . . ?
C4 B1 C43 C44 -17.7(3) . . . . ?
C30 B1 C43 C44 103.8(3) . . . . ?
C17 B1 C43 C44 -137.7(2) . . . . ?
C4 B1 C43 C48 158.6(2) . . . . ?
C30 B1 C43 C48 -79.9(3) . . . . ?
C17 B1 C43 C48 38.6(3) . . . . ?
C48 C43 C44 C45 -2.9(4) . . . . ?
B1 C43 C44 C45 173.6(2) . . . . ?
C43 C44 C45 C46 0.3(4) . . . . ?
C44 C45 C46 C47 1.7(4) . . . . ?
C45 C46 C47 C48 -0.9(4) . . . . ?
C46 C47 C48 C43 -2.0(4) . . . . ?
C44 C43 C48 C47 3.8(4) . . . . ?
B1 C43 C48 C47 -172.9(2) . . . . ?
C51 N1 C49 C50 60.7(4) . . . . ?
C53 N1 C49 C50 -57.0(4) . . . . ?
C55 N1 C49 C50 -177.0(3) . . . . ?
C49 N1 C51 C52 59.7(4) . . . . ?
C53 N1 C51 C52 -179.9(3) . . . . ?
C55 N1 C51 C52 -58.0(4) . . . . ?
C49 N1 C53 C54 -61.1(4) . . . . ?
C51 N1 C53 C54 178.5(3) . . . . ?
C55 N1 C53 C54 55.3(4) . . . . ?
C49 N1 C55 C56 -177.9(3) . . . . ?
C51 N1 C55 C56 -57.0(4) . . . . ?
C53 N1 C55 C56 62.3(4) . . . . ?

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_site_symmetry_A
C23 H23A O1 0.95 2.56 3.381(3) 144.6 .
C54 H54B O1 0.98 2.71 3.270(4) 116.7 6_655

_refine_diff_density_max         0.387
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.074

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH3CN/THF'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_14160a
_database_code_depnum_ccdc_archive 'CCDC 1039153'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        Mn(CO)3(PhBP3)
_chemical_name_common            14160a
_chemical_melting_point          537-538
_chemical_formula_moiety         'C48 H41 B Mn O3 P3, 2(C4 H8 O)'
_chemical_formula_sum            'C56 H57 B Mn O5 P3'
_chemical_formula_weight         968.67

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'
Mn Mn 0.3368 0.7283 '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/c'
_space_group_name_Hall           '-P 2ybc'

_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   21.363(3)
_cell_length_b                   9.8951(15)
_cell_length_c                   24.197(4)
_cell_angle_alpha                90
_cell_angle_beta                 110.360(2)
_cell_angle_gamma                90
_cell_volume                     4795.6(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2716
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.38
_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   0.6669
_exptl_transmission_factor_max   0.7456
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.425
_shelx_estimated_absorpt_T_min   0.865
_shelx_estimated_absorpt_T_max   0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6669
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABs 2012/1 (Sheldrick, 2014)'

_exptl_special_details           'Prof. P. Fischer'

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44288
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.728
_diffrn_reflns_theta_max         27.416
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10875
_reflns_number_gt                8485
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2012)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²+3.1683P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10875
_refine_ls_number_parameters     599
_refine_ls_number_restraints     118
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1044
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.003
_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
Mn1 Mn 0.81184(2) 0.33744(3) 0.08944(2) 0.01561(8) Uani 1 1 d . . . . .
C1 C 0.89991(10) 0.3361(2) 0.13358(9) 0.0212(4) Uani 1 1 d . . . . .
O1 O 0.95594(7) 0.34523(16) 0.16011(7) 0.0323(4) Uani 1 1 d . . . . .
C2 C 0.83336(10) 0.3389(2) 0.02371(9) 0.0198(4) Uani 1 1 d . . . . .
O2 O 0.84978(8) 0.34535(16) -0.01668(7) 0.0277(3) Uani 1 1 d . . . . .
C3 C 0.81477(10) 0.5203(2) 0.08960(9) 0.0217(4) Uani 1 1 d . . . . .
O3 O 0.81851(8) 0.63539(15) 0.08727(7) 0.0325(4) Uani 1 1 d . . . . .
P1 P 0.79823(2) 0.09829(5) 0.08316(2) 0.01567(11) Uani 1 1 d . . . . .
P2 P 0.78420(2) 0.33146(5) 0.17601(2) 0.01586(11) Uani 1 1 d . . . . .
P3 P 0.69800(2) 0.34693(5) 0.03183(2) 0.01560(11) Uani 1 1 d . . . . .
C4 C 0.74411(9) 0.04218(19) 0.12184(8) 0.0167(4) Uani 1 1 d . . . . .
H4A H 0.7276 -0.0497 0.1080 0.020 Uiso 1 1 calc R U . . .
H4B H 0.7704 0.0364 0.1645 0.020 Uiso 1 1 calc R U . . .
C5 C 0.76376(10) 0.0172(2) 0.00990(9) 0.0188(4) Uani 1 1 d . . . . .
C6 C 0.79442(11) 0.0371(2) -0.03194(9) 0.0247(5) Uani 1 1 d . . . . .
H6A H 0.8327 0.0935 -0.0226 0.030 Uiso 1 1 calc R U . . .
C7 C 0.76983(12) -0.0244(2) -0.08689(10) 0.0317(5) Uani 1 1 d . . . . .
H7A H 0.7909 -0.0090 -0.1150 0.038 Uiso 1 1 calc R U . . .
C8 C 0.71457(13) -0.1083(2) -0.10065(10) 0.0357(6) Uani 1 1 d . . . . .
H8A H 0.6973 -0.1493 -0.1385 0.043 Uiso 1 1 calc R U . . .
C9 C 0.68462(12) -0.1324(2) -0.05937(10) 0.0321(5) Uani 1 1 d . . . . .
H9A H 0.6475 -0.1917 -0.0684 0.039 Uiso 1 1 calc R U . . .
C10 C 0.70886(10) -0.0697(2) -0.00469(9) 0.0239(4) Uani 1 1 d . . . . .
H10A H 0.6877 -0.0862 0.0233 0.029 Uiso 1 1 calc R U . . .
C11 C 0.87814(9) 0.00856(19) 0.11146(8) 0.0180(4) Uani 1 1 d . . . . .
C12 C 0.93234(10) 0.0546(2) 0.09672(9) 0.0214(4) Uani 1 1 d . . . . .
H12A H 0.9267 0.1290 0.0706 0.026 Uiso 1 1 calc R U . . .
C13 C 0.99410(10) -0.0075(2) 0.11993(10) 0.0251(5) Uani 1 1 d . . . . .
H13A H 1.0306 0.0244 0.1097 0.030 Uiso 1 1 calc R U . . .
C14 C 1.00286(11) -0.1156(2) 0.15790(10) 0.0268(5) Uani 1 1 d . . . . .
H14A H 1.0455 -0.1570 0.1742 0.032 Uiso 1 1 calc R U . . .
C15 C 0.94967(11) -0.1635(2) 0.17216(10) 0.0249(5) Uani 1 1 d . . . . .
H15A H 0.9556 -0.2386 0.1980 0.030 Uiso 1 1 calc R U . . .
C16 C 0.88728(10) -0.1020(2) 0.14875(9) 0.0205(4) Uani 1 1 d . . . . .
H16A H 0.8508 -0.1359 0.1584 0.025 Uiso 1 1 calc R U . . .
C17 C 0.69989(9) 0.27109(19) 0.16094(8) 0.0176(4) Uani 1 1 d . . . . .
H17A H 0.6954 0.2403 0.1983 0.021 Uiso 1 1 calc R U . . .
H17B H 0.6685 0.3471 0.1458 0.021 Uiso 1 1 calc R U . . .
C18 C 0.83417(10) 0.2267(2) 0.23921(8) 0.0192(4) Uani 1 1 d . . . . .
C19 C 0.81576(11) 0.2226(2) 0.28927(9) 0.0254(5) Uani 1 1 d . . . . .
H19A H 0.7792 0.2756 0.2905 0.031 Uiso 1 1 calc R U . . .
C20 C 0.85010(12) 0.1424(2) 0.33713(10) 0.0309(5) Uani 1 1 d . . . . .
H20A H 0.8370 0.1408 0.3708 0.037 Uiso 1 1 calc R U . . .
C21 C 0.90361(11) 0.0643(2) 0.33599(10) 0.0303(5) Uani 1 1 d . . . . .
H21A H 0.9268 0.0084 0.3686 0.036 Uiso 1 1 calc R U . . .
C22 C 0.92276(11) 0.0687(2) 0.28720(9) 0.0268(5) Uani 1 1 d . . . . .
H22A H 0.9596 0.0160 0.2863 0.032 Uiso 1 1 calc R U . . .
C23 C 0.88845(10) 0.1499(2) 0.23930(9) 0.0216(4) Uani 1 1 d . . . . .
H23A H 0.9024 0.1527 0.2061 0.026 Uiso 1 1 calc R U . . .
C24 C 0.79315(10) 0.49355(19) 0.21555(8) 0.0188(4) Uani 1 1 d . . . . .
C25 C 0.85466(11) 0.5595(2) 0.23394(9) 0.0241(4) Uani 1 1 d . . . . .
H25A H 0.8913 0.5204 0.2261 0.029 Uiso 1 1 calc R U . . .
C26 C 0.86275(12) 0.6823(2) 0.26372(10) 0.0291(5) Uani 1 1 d . . . . .
H26A H 0.9051 0.7256 0.2768 0.035 Uiso 1 1 calc R U . . .
C27 C 0.80959(12) 0.7409(2) 0.27416(10) 0.0307(5) Uani 1 1 d . . . . .
H27A H 0.8148 0.8262 0.2933 0.037 Uiso 1 1 calc R U . . .
C28 C 0.74863(12) 0.6758(2) 0.25685(10) 0.0298(5) Uani 1 1 d . . . . .
H28A H 0.7121 0.7163 0.2644 0.036 Uiso 1 1 calc R U . . .
C29 C 0.74036(11) 0.5511(2) 0.22835(9) 0.0237(4) Uani 1 1 d . . . . .
H29A H 0.6987 0.5055 0.2177 0.028 Uiso 1 1 calc R U . . .
C30 C 0.64854(9) 0.20864(19) 0.04482(9) 0.0175(4) Uani 1 1 d . . . . .
H30A H 0.6026 0.2415 0.0374 0.021 Uiso 1 1 calc R U . . .
H30B H 0.6459 0.1358 0.0161 0.021 Uiso 1 1 calc R U . . .
C31 C 0.64935(10) 0.49778(19) 0.03594(9) 0.0198(4) Uani 1 1 d . . . . .
C32 C 0.66890(11) 0.5898(2) 0.08200(9) 0.0234(4) Uani 1 1 d . . . . .
H32A H 0.7105 0.5781 0.1130 0.028 Uiso 1 1 calc R U . . .
C33 C 0.62866(12) 0.6986(2) 0.08348(11) 0.0309(5) Uani 1 1 d . . . . .
H33A H 0.6423 0.7596 0.1158 0.037 Uiso 1 1 calc R U . . .
C34 C 0.56886(13) 0.7187(2) 0.03815(11) 0.0364(6) Uani 1 1 d . . . . .
H34A H 0.5417 0.7943 0.0388 0.044 Uiso 1 1 calc R U . . .
C35 C 0.54864(12) 0.6285(3) -0.00811(11) 0.0369(6) Uani 1 1 d . . . . .
H35A H 0.5074 0.6419 -0.0394 0.044 Uiso 1 1 calc R U . . .
C36 C 0.58804(11) 0.5187(2) -0.00925(10) 0.0288(5) Uani 1 1 d . . . . .
H36A H 0.5733 0.4565 -0.0411 0.035 Uiso 1 1 calc R U . . .
C37 C 0.68604(9) 0.3541(2) -0.04688(8) 0.0184(4) Uani 1 1 d . . . . .
C38 C 0.70394(11) 0.4732(2) -0.06875(9) 0.0246(5) Uani 1 1 d . . . . .
H38A H 0.7198 0.5481 -0.0431 0.030 Uiso 1 1 calc R U . . .
C39 C 0.69899(11) 0.4837(2) -0.12695(10) 0.0314(5) Uani 1 1 d . . . . .
H39A H 0.7114 0.5652 -0.1412 0.038 Uiso 1 1 calc R U . . .
C40 C 0.67581(12) 0.3746(3) -0.16479(10) 0.0324(5) Uani 1 1 d . . . . .
H40A H 0.6722 0.3815 -0.2049 0.039 Uiso 1 1 calc R U . . .
C41 C 0.65811(11) 0.2567(2) -0.14393(9) 0.0291(5) Uani 1 1 d . . . . .
H41A H 0.6427 0.1819 -0.1697 0.035 Uiso 1 1 calc R U . . .
C42 C 0.66272(10) 0.2462(2) -0.08530(9) 0.0227(4) Uani 1 1 d . . . . .
H42A H 0.6498 0.1647 -0.0714 0.027 Uiso 1 1 calc R U . . .
B1 B 0.67831(11) 0.1444(2) 0.11221(10) 0.0161(4) Uani 1 1 d . . . . .
C43 C 0.62012(10) 0.05969(19) 0.12686(9) 0.0181(4) Uani 1 1 d . . . . .
C44 C 0.63572(10) -0.0095(2) 0.18061(9) 0.0214(4) Uani 1 1 d . . . . .
H44A H 0.6809 -0.0113 0.2065 0.026 Uiso 1 1 calc R U . . .
C45 C 0.58806(12) -0.0751(2) 0.19751(10) 0.0288(5) Uani 1 1 d . . . . .
H45A H 0.6009 -0.1203 0.2344 0.035 Uiso 1 1 calc R U . . .
C46 C 0.52179(12) -0.0752(2) 0.16082(11) 0.0323(5) Uani 1 1 d . . . . .
H46A H 0.4889 -0.1198 0.1723 0.039 Uiso 1 1 calc R U . . .
C47 C 0.50440(11) -0.0093(2) 0.10738(11) 0.0311(5) Uani 1 1 d . . . . .
H47A H 0.4591 -0.0083 0.0818 0.037 Uiso 1 1 calc R U . . .
C48 C 0.55290(10) 0.0557(2) 0.09072(10) 0.0237(4) Uani 1 1 d . . . . .
H48A H 0.5398 0.0989 0.0534 0.028 Uiso 1 1 calc R U . . .
O4 O 0.59238(8) 0.42257(15) 0.23380(8) 0.0411(4) Uani 1 1 d D U . . .
C49 C 0.54753(12) 0.3206(2) 0.20298(15) 0.0586(9) Uani 1 1 d D U . . .
H49A H 0.5428 0.2519 0.2310 0.070 Uiso 1 1 calc R U . A 1
H49B H 0.5647 0.2754 0.1747 0.070 Uiso 1 1 calc R U . A 1
C50 C 0.48158(11) 0.3838(3) 0.17094(12) 0.0491(7) Uani 0.773(7) 1 d D U P B 1
H50A H 0.4515 0.3788 0.1941 0.059 Uiso 0.773(7) 1 calc R U P B 1
H50B H 0.4596 0.3410 0.1320 0.059 Uiso 0.773(7) 1 calc R U P B 1
C51 C 0.50205(17) 0.5301(3) 0.16466(16) 0.0557(13) Uani 0.773(7) 1 d D U P B 1
H51A H 0.5157 0.5409 0.1298 0.067 Uiso 0.773(7) 1 calc R U P B 1
H51B H 0.4654 0.5940 0.1617 0.067 Uiso 0.773(7) 1 calc R U P B 1
C52 C 0.55996(12) 0.5498(2) 0.22079(12) 0.0491(7) Uani 0.773(7) 1 d D U P B 1
H52A H 0.5907 0.6195 0.2156 0.059 Uiso 0.773(7) 1 calc R U P B 1
H52B H 0.5443 0.5784 0.2530 0.059 Uiso 0.773(7) 1 calc R U P B 1
C50' C 0.48158(11) 0.3838(3) 0.17094(12) 0.0491(7) Uani 0.227(7) 1 d D U P B 2
H50C H 0.4452 0.3329 0.1780 0.059 Uiso 0.227(7) 1 calc R U P B 2
H50D H 0.4729 0.3862 0.1280 0.059 Uiso 0.227(7) 1 calc R U P B 2
C51' C 0.48670(16) 0.5260(5) 0.1958(5) 0.0557(13) Uani 0.227(7) 1 d D U P B 2
H51C H 0.4646 0.5923 0.1644 0.067 Uiso 0.227(7) 1 calc R U P B 2
H51D H 0.4664 0.5315 0.2268 0.067 Uiso 0.227(7) 1 calc R U P B 2
C52' C 0.55996(12) 0.5498(2) 0.22079(12) 0.0491(7) Uani 0.227(7) 1 d D U P B 2
H52C H 0.5749 0.5993 0.1920 0.059 Uiso 0.227(7) 1 calc R U P B 2
H52D H 0.5711 0.6049 0.2571 0.059 Uiso 0.227(7) 1 calc R U P B 2
O5 O 0.97878(9) 0.7120(2) -0.04318(8) 0.0540(5) Uani 1 1 d D . . . .
C53 C 0.91378(12) 0.7687(3) -0.05686(13) 0.0575(8) Uani 1 1 d D . . . .
H53A H 0.8881 0.7612 -0.0996 0.069 Uiso 1 1 calc R U . . .
H53B H 0.9167 0.8651 -0.0454 0.069 Uiso 1 1 calc R U . . .
C54 C 0.88148(11) 0.6876(3) -0.02192(13) 0.0569(9) Uani 1 1 d D . . . .
H54A H 0.8592 0.6065 -0.0440 0.068 Uiso 1 1 calc R U . . .
H54B H 0.8483 0.7423 -0.0116 0.068 Uiso 1 1 calc R U . . .
C55 C 0.94008(11) 0.6487(3) 0.03305(10) 0.0386(6) Uani 1 1 d D . . . .
H55A H 0.9392 0.7006 0.0677 0.046 Uiso 1 1 calc R U . . .
H55B H 0.9391 0.5510 0.0415 0.046 Uiso 1 1 calc R U . . .
C56 C 1.00066(11) 0.6836(3) 0.01831(10) 0.0438(6) Uani 1 1 d D . . . .
H56A H 1.0234 0.7634 0.0412 0.053 Uiso 1 1 calc R U . . .
H56B H 1.0324 0.6069 0.0279 0.053 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 C2 1.803(2) . ?
Mn1 C3 1.811(2) . ?
Mn1 C1 1.812(2) . ?
Mn1 P3 2.3467(6) . ?
Mn1 P2 2.3667(7) . ?
Mn1 P1 2.3826(7) . ?
C1 O1 1.148(2) . ?
C2 O2 1.150(2) . ?
C3 O3 1.144(2) . ?
P1 C4 1.809(2) . ?
P1 C11 1.833(2) . ?
P1 C5 1.849(2) . ?
P2 C17 1.8103(19) . ?
P2 C24 1.843(2) . ?
P2 C18 1.849(2) . ?
P3 C30 1.8217(19) . ?
P3 C37 1.833(2) . ?
P3 C31 1.841(2) . ?
C4 B1 1.681(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.397(3) . ?
C5 C6 1.398(3) . ?
C6 C7 1.389(3) . ?
C6 H6A 0.9500 . ?
C7 C8 1.386(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.381(4) . ?
C8 H8A 0.9500 . ?
C9 C10 1.388(3) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C16 1.388(3) . ?
C11 C12 1.401(3) . ?
C12 C13 1.385(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.379(3) . ?
C13 H13A 0.9500 . ?
C14 C15 1.382(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.394(3) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 B1 1.672(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C23 1.386(3) . ?
C18 C19 1.398(3) . ?
C19 C20 1.385(3) . ?
C19 H19A 0.9500 . ?
C20 C21 1.388(3) . ?
C20 H20A 0.9500 . ?
C21 C22 1.378(3) . ?
C21 H21A 0.9500 . ?
C22 C23 1.391(3) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 C29 1.391(3) . ?
C24 C25 1.394(3) . ?
C25 C26 1.392(3) . ?
C25 H25A 0.9500 . ?
C26 C27 1.375(3) . ?
C26 H26A 0.9500 . ?
C27 C28 1.381(3) . ?
C27 H27A 0.9500 . ?
C28 C29 1.394(3) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 B1 1.657(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.386(3) . ?
C31 C36 1.399(3) . ?
C32 C33 1.386(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.378(3) . ?
C33 H33A 0.9500 . ?
C34 C35 1.378(4) . ?
C34 H34A 0.9500 . ?
C35 C36 1.381(3) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 C42 1.390(3) . ?
C37 C38 1.399(3) . ?
C38 C39 1.379(3) . ?
C38 H38A 0.9500 . ?
C39 C40 1.390(3) . ?
C39 H39A 0.9500 . ?
C40 C41 1.376(3) . ?
C40 H40A 0.9500 . ?
C41 C42 1.391(3) . ?
C41 H41A 0.9500 . ?
C42 H42A 0.9500 . ?
B1 C43 1.637(3) . ?
C43 C48 1.398(3) . ?
C43 C44 1.403(3) . ?
C44 C45 1.384(3) . ?
C44 H44A 0.9500 . ?
C45 C46 1.385(3) . ?
C45 H45A 0.9500 . ?
C46 C47 1.379(3) . ?
C46 H46A 0.9500 . ?
C47 C48 1.393(3) . ?
C47 H47A 0.9500 . ?
C48 H48A 0.9500 . ?
O4 C49 1.412(2) . ?
O4 C52 1.419(2) . ?
C49 C50 1.489(2) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.535(3) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.498(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C51' H51C 0.9900 . ?
C51' H51D 0.9900 . ?
O5 C53 1.425(2) . ?
O5 C56 1.424(2) . ?
C53 C54 1.497(2) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.525(3) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.498(2) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?

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 Mn1 C3 88.55(9) . . ?
C2 Mn1 C1 89.36(9) . . ?
C3 Mn1 C1 88.75(9) . . ?
C2 Mn1 P3 90.31(6) . . ?
C3 Mn1 P3 89.39(7) . . ?
C1 Mn1 P3 178.11(7) . . ?
C2 Mn1 P2 178.98(7) . . ?
C3 Mn1 P2 92.42(7) . . ?
C1 Mn1 P2 90.33(7) . . ?
P3 Mn1 P2 90.04(2) . . ?
C2 Mn1 P1 90.84(6) . . ?
C3 Mn1 P1 174.96(7) . . ?
C1 Mn1 P1 96.25(7) . . ?
P3 Mn1 P1 85.618(19) . . ?
P2 Mn1 P1 88.229(19) . . ?
O1 C1 Mn1 174.72(19) . . ?
O2 C2 Mn1 176.07(18) . . ?
O3 C3 Mn1 175.88(19) . . ?
C4 P1 C11 109.74(9) . . ?
C4 P1 C5 104.47(9) . . ?
C11 P1 C5 99.01(9) . . ?
C4 P1 Mn1 110.95(6) . . ?
C11 P1 Mn1 112.35(6) . . ?
C5 P1 Mn1 119.40(7) . . ?
C17 P2 C24 107.94(9) . . ?
C17 P2 C18 103.26(9) . . ?
C24 P2 C18 97.64(9) . . ?
C17 P2 Mn1 111.54(7) . . ?
C24 P2 Mn1 115.14(7) . . ?
C18 P2 Mn1 119.74(7) . . ?
C30 P3 C37 109.20(9) . . ?
C30 P3 C31 103.15(9) . . ?
C37 P3 C31 98.47(9) . . ?
C30 P3 Mn1 114.26(6) . . ?
C37 P3 Mn1 111.09(6) . . ?
C31 P3 Mn1 119.22(7) . . ?
B1 C4 P1 113.44(13) . . ?
B1 C4 H4A 108.9 . . ?
P1 C4 H4A 108.9 . . ?
B1 C4 H4B 108.9 . . ?
P1 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?
C10 C5 C6 117.85(18) . . ?
C10 C5 P1 121.90(16) . . ?
C6 C5 P1 120.18(15) . . ?
C7 C6 C5 121.0(2) . . ?
C7 C6 H6A 119.5 . . ?
C5 C6 H6A 119.5 . . ?
C8 C7 C6 120.0(2) . . ?
C8 C7 H7A 120.0 . . ?
C6 C7 H7A 120.0 . . ?
C9 C8 C7 120.0(2) . . ?
C9 C8 H8A 120.0 . . ?
C7 C8 H8A 120.0 . . ?
C8 C9 C10 120.0(2) . . ?
C8 C9 H9A 120.0 . . ?
C10 C9 H9A 120.0 . . ?
C9 C10 C5 121.2(2) . . ?
C9 C10 H10A 119.4 . . ?
C5 C10 H10A 119.4 . . ?
C16 C11 C12 118.68(18) . . ?
C16 C11 P1 121.80(15) . . ?
C12 C11 P1 119.49(15) . . ?
C13 C12 C11 120.50(19) . . ?
C13 C12 H12A 119.8 . . ?
C11 C12 H12A 119.8 . . ?
C14 C13 C12 120.2(2) . . ?
C14 C13 H13A 119.9 . . ?
C12 C13 H13A 119.9 . . ?
C13 C14 C15 120.0(2) . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C14 C15 C16 120.1(2) . . ?
C14 C15 H15A 119.9 . . ?
C16 C15 H15A 119.9 . . ?
C11 C16 C15 120.47(19) . . ?
C11 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
B1 C17 P2 113.60(13) . . ?
B1 C17 H17A 108.8 . . ?
P2 C17 H17A 108.8 . . ?
B1 C17 H17B 108.8 . . ?
P2 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C23 C18 C19 118.06(19) . . ?
C23 C18 P2 123.44(16) . . ?
C19 C18 P2 118.50(16) . . ?
C20 C19 C18 120.9(2) . . ?
C20 C19 H19A 119.5 . . ?
C18 C19 H19A 119.5 . . ?
C19 C20 C21 120.2(2) . . ?
C19 C20 H20A 119.9 . . ?
C21 C20 H20A 119.9 . . ?
C22 C21 C20 119.4(2) . . ?
C22 C21 H21A 120.3 . . ?
C20 C21 H21A 120.3 . . ?
C21 C22 C23 120.3(2) . . ?
C21 C22 H22A 119.8 . . ?
C23 C22 H22A 119.8 . . ?
C18 C23 C22 121.1(2) . . ?
C18 C23 H23A 119.5 . . ?
C22 C23 H23A 119.5 . . ?
C29 C24 C25 118.96(18) . . ?
C29 C24 P2 121.74(15) . . ?
C25 C24 P2 119.29(16) . . ?
C26 C25 C24 120.5(2) . . ?
C26 C25 H25A 119.8 . . ?
C24 C25 H25A 119.8 . . ?
C27 C26 C25 120.1(2) . . ?
C27 C26 H26A 119.9 . . ?
C25 C26 H26A 119.9 . . ?
C26 C27 C28 120.0(2) . . ?
C26 C27 H27A 120.0 . . ?
C28 C27 H27A 120.0 . . ?
C27 C28 C29 120.4(2) . . ?
C27 C28 H28A 119.8 . . ?
C29 C28 H28A 119.8 . . ?
C24 C29 C28 120.0(2) . . ?
C24 C29 H29A 120.0 . . ?
C28 C29 H29A 120.0 . . ?
B1 C30 P3 114.26(13) . . ?
B1 C30 H30A 108.7 . . ?
P3 C30 H30A 108.7 . . ?
B1 C30 H30B 108.7 . . ?
P3 C30 H30B 108.7 . . ?
H30A C30 H30B 107.6 . . ?
C32 C31 C36 118.01(19) . . ?
C32 C31 P3 123.93(16) . . ?
C36 C31 P3 118.04(15) . . ?
C31 C32 C33 121.0(2) . . ?
C31 C32 H32A 119.5 . . ?
C33 C32 H32A 119.5 . . ?
C34 C33 C32 120.2(2) . . ?
C34 C33 H33A 119.9 . . ?
C32 C33 H33A 119.9 . . ?
C33 C34 C35 119.7(2) . . ?
C33 C34 H34A 120.2 . . ?
C35 C34 H34A 120.2 . . ?
C34 C35 C36 120.3(2) . . ?
C34 C35 H35A 119.8 . . ?
C36 C35 H35A 119.8 . . ?
C35 C36 C31 120.8(2) . . ?
C35 C36 H36A 119.6 . . ?
C31 C36 H36A 119.6 . . ?
C42 C37 C38 118.42(19) . . ?
C42 C37 P3 123.60(16) . . ?
C38 C37 P3 117.93(15) . . ?
C39 C38 C37 121.0(2) . . ?
C39 C38 H38A 119.5 . . ?
C37 C38 H38A 119.5 . . ?
C38 C39 C40 119.9(2) . . ?
C38 C39 H39A 120.1 . . ?
C40 C39 H39A 120.1 . . ?
C41 C40 C39 119.8(2) . . ?
C41 C40 H40A 120.1 . . ?
C39 C40 H40A 120.1 . . ?
C40 C41 C42 120.4(2) . . ?
C40 C41 H41A 119.8 . . ?
C42 C41 H41A 119.8 . . ?
C37 C42 C41 120.5(2) . . ?
C37 C42 H42A 119.8 . . ?
C41 C42 H42A 119.8 . . ?
C43 B1 C30 110.44(16) . . ?
C43 B1 C17 105.96(15) . . ?
C30 B1 C17 108.87(15) . . ?
C43 B1 C4 108.87(15) . . ?
C30 B1 C4 112.53(16) . . ?
C17 B1 C4 109.95(15) . . ?
C48 C43 C44 115.27(18) . . ?
C48 C43 B1 124.83(18) . . ?
C44 C43 B1 119.80(17) . . ?
C45 C44 C43 122.7(2) . . ?
C45 C44 H44A 118.6 . . ?
C43 C44 H44A 118.6 . . ?
C44 C45 C46 120.3(2) . . ?
C44 C45 H45A 119.9 . . ?
C46 C45 H45A 119.9 . . ?
C47 C46 C45 118.9(2) . . ?
C47 C46 H46A 120.6 . . ?
C45 C46 H46A 120.6 . . ?
C46 C47 C48 120.3(2) . . ?
C46 C47 H47A 119.8 . . ?
C48 C47 H47A 119.8 . . ?
C47 C48 C43 122.5(2) . . ?
C47 C48 H48A 118.7 . . ?
C43 C48 H48A 118.7 . . ?
C49 O4 C52 109.13(17) . . ?
O4 C49 C50 108.70(16) . . ?
O4 C49 H49A 110.0 . . ?
C50 C49 H49A 110.0 . . ?
O4 C49 H49B 110.0 . . ?
C50 C49 H49B 110.0 . . ?
H49A C49 H49B 108.3 . . ?
C49 C50 C51 101.35(17) . . ?
C49 C50 H50A 111.5 . . ?
C51 C50 H50A 111.5 . . ?
C49 C50 H50B 111.5 . . ?
C51 C50 H50B 111.5 . . ?
H50A C50 H50B 109.3 . . ?
C52 C51 C50 101.96(16) . . ?
C52 C51 H51A 111.4 . . ?
C50 C51 H51A 111.4 . . ?
C52 C51 H51B 111.4 . . ?
C50 C51 H51B 111.4 . . ?
H51A C51 H51B 109.2 . . ?
O4 C52 C51 105.70(18) . . ?
O4 C52 H52A 110.6 . . ?
C51 C52 H52A 110.6 . . ?
O4 C52 H52B 110.6 . . ?
C51 C52 H52B 110.6 . . ?
H52A C52 H52B 108.7 . . ?
H51C C51' H51D 109.1 . . ?
C53 O5 C56 105.04(18) . . ?
O5 C53 C54 105.16(18) . . ?
O5 C53 H53A 110.7 . . ?
C54 C53 H53A 110.7 . . ?
O5 C53 H53B 110.7 . . ?
C54 C53 H53B 110.7 . . ?
H53A C53 H53B 108.8 . . ?
C53 C54 C55 103.19(16) . . ?
C53 C54 H54A 111.1 . . ?
C55 C54 H54A 111.1 . . ?
C53 C54 H54B 111.1 . . ?
C55 C54 H54B 111.1 . . ?
H54A C54 H54B 109.1 . . ?
C56 C55 C54 104.44(15) . . ?
C56 C55 H55A 110.9 . . ?
C54 C55 H55A 110.9 . . ?
C56 C55 H55B 110.9 . . ?
C54 C55 H55B 110.9 . . ?
H55A C55 H55B 108.9 . . ?
O5 C56 C55 107.32(16) . . ?
O5 C56 H56A 110.3 . . ?
C55 C56 H56A 110.3 . . ?
O5 C56 H56B 110.3 . . ?
C55 C56 H56B 110.3 . . ?
H56A C56 H56B 108.5 . . ?

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
C11 P1 C4 B1 165.06(13) . . . . ?
C5 P1 C4 B1 -89.61(14) . . . . ?
Mn1 P1 C4 B1 40.31(14) . . . . ?
C4 P1 C5 C10 -1.92(19) . . . . ?
C11 P1 C5 C10 111.29(17) . . . . ?
Mn1 P1 C5 C10 -126.62(15) . . . . ?
C4 P1 C5 C6 -178.98(16) . . . . ?
C11 P1 C5 C6 -65.77(17) . . . . ?
Mn1 P1 C5 C6 56.32(18) . . . . ?
C10 C5 C6 C7 1.9(3) . . . . ?
P1 C5 C6 C7 179.10(16) . . . . ?
C5 C6 C7 C8 -0.8(3) . . . . ?
C6 C7 C8 C9 -1.0(3) . . . . ?
C7 C8 C9 C10 1.7(3) . . . . ?
C8 C9 C10 C5 -0.5(3) . . . . ?
C6 C5 C10 C9 -1.3(3) . . . . ?
P1 C5 C10 C9 -178.38(16) . . . . ?
C4 P1 C11 C16 10.92(19) . . . . ?
C5 P1 C11 C16 -98.08(17) . . . . ?
Mn1 P1 C11 C16 134.86(15) . . . . ?
C4 P1 C11 C12 -167.11(16) . . . . ?
C5 P1 C11 C12 83.89(17) . . . . ?
Mn1 P1 C11 C12 -43.17(18) . . . . ?
C16 C11 C12 C13 -1.3(3) . . . . ?
P1 C11 C12 C13 176.81(16) . . . . ?
C11 C12 C13 C14 0.0(3) . . . . ?
C12 C13 C14 C15 1.0(3) . . . . ?
C13 C14 C15 C16 -0.7(3) . . . . ?
C12 C11 C16 C15 1.6(3) . . . . ?
P1 C11 C16 C15 -176.44(16) . . . . ?
C14 C15 C16 C11 -0.6(3) . . . . ?
C24 P2 C17 B1 166.72(13) . . . . ?
C18 P2 C17 B1 -90.58(15) . . . . ?
Mn1 P2 C17 B1 39.28(15) . . . . ?
C17 P2 C18 C23 125.04(17) . . . . ?
C24 P2 C18 C23 -124.42(17) . . . . ?
Mn1 P2 C18 C23 0.36(19) . . . . ?
C17 P2 C18 C19 -53.87(17) . . . . ?
C24 P2 C18 C19 56.67(17) . . . . ?
Mn1 P2 C18 C19 -178.55(13) . . . . ?
C23 C18 C19 C20 -1.1(3) . . . . ?
P2 C18 C19 C20 177.91(17) . . . . ?
C18 C19 C20 C21 -0.1(3) . . . . ?
C19 C20 C21 C22 0.8(3) . . . . ?
C20 C21 C22 C23 -0.5(3) . . . . ?
C19 C18 C23 C22 1.4(3) . . . . ?
P2 C18 C23 C22 -177.50(15) . . . . ?
C21 C22 C23 C18 -0.7(3) . . . . ?
C17 P2 C24 C29 -1.0(2) . . . . ?
C18 P2 C24 C29 -107.62(18) . . . . ?
Mn1 P2 C24 C29 124.36(16) . . . . ?
C17 P2 C24 C25 178.08(16) . . . . ?
C18 P2 C24 C25 71.43(18) . . . . ?
Mn1 P2 C24 C25 -56.59(18) . . . . ?
C29 C24 C25 C26 -1.1(3) . . . . ?
P2 C24 C25 C26 179.78(16) . . . . ?
C24 C25 C26 C27 -1.3(3) . . . . ?
C25 C26 C27 C28 2.2(3) . . . . ?
C26 C27 C28 C29 -0.5(3) . . . . ?
C25 C24 C29 C28 2.8(3) . . . . ?
P2 C24 C29 C28 -178.15(16) . . . . ?
C27 C28 C29 C24 -2.0(3) . . . . ?
C37 P3 C30 B1 153.34(14) . . . . ?
C31 P3 C30 B1 -102.68(15) . . . . ?
Mn1 P3 C30 B1 28.25(16) . . . . ?
C30 P3 C31 C32 108.65(18) . . . . ?
C37 P3 C31 C32 -139.25(18) . . . . ?
Mn1 P3 C31 C32 -19.2(2) . . . . ?
C30 P3 C31 C36 -69.38(19) . . . . ?
C37 P3 C31 C36 42.72(19) . . . . ?
Mn1 P3 C31 C36 162.73(15) . . . . ?
C36 C31 C32 C33 0.5(3) . . . . ?
P3 C31 C32 C33 -177.51(17) . . . . ?
C31 C32 C33 C34 -1.5(3) . . . . ?
C32 C33 C34 C35 1.3(4) . . . . ?
C33 C34 C35 C36 -0.1(4) . . . . ?
C34 C35 C36 C31 -0.8(4) . . . . ?
C32 C31 C36 C35 0.6(3) . . . . ?
P3 C31 C36 C35 178.75(19) . . . . ?
C30 P3 C37 C42 -20.2(2) . . . . ?
C31 P3 C37 C42 -127.37(18) . . . . ?
Mn1 P3 C37 C42 106.73(17) . . . . ?
C30 P3 C37 C38 162.45(16) . . . . ?
C31 P3 C37 C38 55.27(17) . . . . ?
Mn1 P3 C37 C38 -70.63(16) . . . . ?
C42 C37 C38 C39 -0.3(3) . . . . ?
P3 C37 C38 C39 177.18(17) . . . . ?
C37 C38 C39 C40 0.1(3) . . . . ?
C38 C39 C40 C41 -0.2(3) . . . . ?
C39 C40 C41 C42 0.6(3) . . . . ?
C38 C37 C42 C41 0.7(3) . . . . ?
P3 C37 C42 C41 -176.67(16) . . . . ?
C40 C41 C42 C37 -0.8(3) . . . . ?
P3 C30 B1 C43 161.08(13) . . . . ?
P3 C30 B1 C17 45.13(19) . . . . ?
P3 C30 B1 C4 -77.04(18) . . . . ?
P2 C17 B1 C43 154.09(13) . . . . ?
P2 C17 B1 C30 -87.12(17) . . . . ?
P2 C17 B1 C4 36.60(19) . . . . ?
P1 C4 B1 C43 158.99(13) . . . . ?
P1 C4 B1 C30 36.21(19) . . . . ?
P1 C4 B1 C17 -85.34(17) . . . . ?
C30 B1 C43 C48 -7.2(3) . . . . ?
C17 B1 C43 C48 110.5(2) . . . . ?
C4 B1 C43 C48 -131.27(19) . . . . ?
C30 B1 C43 C44 176.52(17) . . . . ?
C17 B1 C43 C44 -65.7(2) . . . . ?
C4 B1 C43 C44 52.5(2) . . . . ?
C48 C43 C44 C45 -1.2(3) . . . . ?
B1 C43 C44 C45 175.41(18) . . . . ?
C43 C44 C45 C46 0.3(3) . . . . ?
C44 C45 C46 C47 0.2(3) . . . . ?
C45 C46 C47 C48 0.2(3) . . . . ?
C46 C47 C48 C43 -1.1(3) . . . . ?
C44 C43 C48 C47 1.6(3) . . . . ?
B1 C43 C48 C47 -174.81(19) . . . . ?
C52 O4 C49 C50 -3.2(4) . . . . ?
O4 C49 C50 C51 23.9(3) . . . . ?
C49 C50 C51 C52 -34.4(3) . . . . ?
C49 O4 C52 C51 -19.9(3) . . . . ?
C50 C51 C52 O4 33.9(3) . . . . ?
C56 O5 C53 C54 -39.8(3) . . . . ?
O5 C53 C54 C55 31.7(3) . . . . ?
C53 C54 C55 C56 -12.3(3) . . . . ?
C53 O5 C56 C55 31.7(3) . . . . ?
C54 C55 C56 O5 -11.2(3) . . . . ?

_refine_diff_density_max         0.503
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.061

_shelxl_version_number           2014-3


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/pentane'
####################################################################### 
# 
# 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_14161a
_database_code_depnum_ccdc_archive 'CCDC 1039154'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        '[Et4N][Cr(CO)3{6-(PhBP3)Cr(CO)3}]'
_chemical_name_common            14161a
_chemical_melting_point          567-569
_chemical_formula_moiety         '2(C51 H41 B Cr2 O6 P3), 2(C8 H20 N), C4 H10 O'
_chemical_formula_sum            'C122 H132 B2 Cr4 N2 O13 P6'
_chemical_formula_weight         2249.73

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'
N N 0.0061 0.0033 '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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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, y+1/2, -z'

_cell_length_a                   13.9914(17)
_cell_length_b                   22.205(3)
_cell_length_c                   18.059(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.070(1)
_cell_angle_gamma                90
_cell_volume                     5609.6(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2868
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      27.42

_exptl_crystal_description       Plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_F_000             2356
_exptl_transmission_factor_min   0.5017
_exptl_transmission_factor_max   0.5629
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.526
_shelx_estimated_absorpt_T_min   0.798
_shelx_estimated_absorpt_T_max   0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5017
_exptl_absorpt_correction_T_max  0.5629
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'

_exptl_special_details           'Prof. P. Fischer'

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            65363
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.454
_diffrn_reflns_theta_max         27.449
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             25293
_reflns_number_gt                23525
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_max     0.978
_reflns_Friedel_fraction_full    0.997

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0469P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 10688 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(4)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         25293
_refine_ls_number_parameters     1352
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0781
_refine_ls_wR_factor_gt          0.0759
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.002
_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
Cr1A Cr 0.35861(3) 0.44988(2) 0.95205(2) 0.01284(9) Uani 1 1 d . . . . .
Cr2A Cr 0.38319(4) 0.66353(2) 0.66472(3) 0.02070(11) Uani 1 1 d . . . . .
P1A P 0.31590(5) 0.41568(3) 0.82975(4) 0.01280(14) Uani 1 1 d . . . . .
P2A P 0.28827(5) 0.54495(3) 0.91742(4) 0.01471(14) Uani 1 1 d . . . . .
P3A P 0.50040(5) 0.49046(3) 0.89815(4) 0.01328(14) Uani 1 1 d . . . . .
O1A O 0.19284(16) 0.38966(11) 1.02412(13) 0.0290(5) Uani 1 1 d . . . . .
O2A O 0.46148(18) 0.33841(11) 1.00026(12) 0.0321(6) Uani 1 1 d . . . . .
O3A O 0.40930(16) 0.48666(11) 1.10719(12) 0.0276(5) Uani 1 1 d . . . . .
O4A O 0.23758(18) 0.72219(12) 0.76038(15) 0.0396(6) Uani 1 1 d . . . . .
O5A O 0.41167(19) 0.78740(11) 0.60341(14) 0.0359(6) Uani 1 1 d . . . . .
O6A O 0.53251(18) 0.68805(11) 0.78067(14) 0.0345(6) Uani 1 1 d . . . . .
C1A C 0.2538(2) 0.41486(14) 0.99291(16) 0.0188(6) Uani 1 1 d . . . . .
C2A C 0.4221(2) 0.38101(14) 0.97746(16) 0.0191(6) Uani 1 1 d . . . . .
C3A C 0.3908(2) 0.47542(13) 1.04518(16) 0.0190(6) Uani 1 1 d . . . . .
C4A C 0.37284(19) 0.45711(13) 0.75571(14) 0.0147(5) Uani 1 1 d . . . . .
H4AA H 0.4375 0.4404 0.7480 0.018 Uiso 1 1 calc R U . . .
H4AB H 0.3353 0.4515 0.7092 0.018 Uiso 1 1 calc R U . . .
C5A C 0.3380(2) 0.33549(13) 0.81082(15) 0.0163(6) Uani 1 1 d . . . . .
C6A C 0.3086(3) 0.29317(15) 0.86223(18) 0.0277(7) Uani 1 1 d . . . . .
H6AA H 0.2778 0.3061 0.9059 0.033 Uiso 1 1 calc R U . . .
C7A C 0.3237(3) 0.23248(16) 0.8506(2) 0.0388(9) Uani 1 1 d . . . . .
H7AA H 0.3016 0.2041 0.8857 0.047 Uiso 1 1 calc R U . . .
C8A C 0.3703(3) 0.21274(16) 0.7890(2) 0.0340(8) Uani 1 1 d . . . . .
H8AA H 0.3815 0.1709 0.7820 0.041 Uiso 1 1 calc R U . . .
C9A C 0.4008(2) 0.25388(15) 0.7370(2) 0.0279(7) Uani 1 1 d . . . . .
H9AA H 0.4330 0.2406 0.6942 0.033 Uiso 1 1 calc R U . . .
C10A C 0.3839(2) 0.31494(13) 0.74825(17) 0.0212(6) Uani 1 1 d . . . . .
H10A H 0.4041 0.3432 0.7123 0.025 Uiso 1 1 calc R U . . .
C11A C 0.18955(19) 0.41809(13) 0.79943(16) 0.0165(5) Uani 1 1 d . . . . .
C12A C 0.1157(2) 0.43468(15) 0.84585(17) 0.0229(7) Uani 1 1 d . . . . .
H12A H 0.1292 0.4428 0.8966 0.027 Uiso 1 1 calc R U . . .
C13A C 0.0225(2) 0.43949(19) 0.81867(19) 0.0361(9) Uani 1 1 d . . . . .
H13A H -0.0273 0.4509 0.8509 0.043 Uiso 1 1 calc R U . . .
C14A C 0.0018(2) 0.4277(2) 0.7447(2) 0.0414(10) Uani 1 1 d . . . . .
H14A H -0.0618 0.4316 0.7260 0.050 Uiso 1 1 calc R U . . .
C15A C 0.0738(2) 0.4102(2) 0.6983(2) 0.0393(9) Uani 1 1 d . . . . .
H15A H 0.0598 0.4020 0.6476 0.047 Uiso 1 1 calc R U . . .
C16A C 0.1667(2) 0.40451(16) 0.72571(17) 0.0259(7) Uani 1 1 d . . . . .
H16A H 0.2156 0.3912 0.6938 0.031 Uiso 1 1 calc R U . . .
C17A C 0.2870(2) 0.55674(13) 0.81800(15) 0.0163(6) Uani 1 1 d . . . . .
H17A H 0.2292 0.5373 0.7966 0.020 Uiso 1 1 calc R U . . .
H17B H 0.2816 0.6005 0.8083 0.020 Uiso 1 1 calc R U . . .
C18A C 0.1642(2) 0.55984(14) 0.94529(16) 0.0203(6) Uani 1 1 d . . . . .
C19A C 0.1323(2) 0.53877(16) 1.01282(19) 0.0295(7) Uani 1 1 d . . . . .
H19A H 0.1754 0.5180 1.0451 0.035 Uiso 1 1 calc R U . . .
C20A C 0.0378(3) 0.5476(2) 1.0341(2) 0.0433(10) Uani 1 1 d . . . . .
H20A H 0.0170 0.5329 1.0805 0.052 Uiso 1 1 calc R U . . .
C21A C -0.0252(3) 0.5777(2) 0.9876(2) 0.0430(10) Uani 1 1 d . . . . .
H21A H -0.0898 0.5831 1.0013 0.052 Uiso 1 1 calc R U . . .
C22A C 0.0063(3) 0.60000(19) 0.9207(2) 0.0391(9) Uani 1 1 d . . . . .
H22A H -0.0368 0.6211 0.8888 0.047 Uiso 1 1 calc R U . . .
C23A C 0.0999(2) 0.59183(16) 0.90004(18) 0.0288(7) Uani 1 1 d . . . . .
H23A H 0.1209 0.6081 0.8545 0.035 Uiso 1 1 calc R U . . .
C24A C 0.3449(2) 0.61344(13) 0.95750(16) 0.0192(6) Uani 1 1 d . . . . .
C25A C 0.3621(3) 0.61527(15) 1.03391(18) 0.0286(7) Uani 1 1 d . . . . .
H25A H 0.3443 0.5819 1.0635 0.034 Uiso 1 1 calc R U . . .
C26A C 0.4045(3) 0.66482(17) 1.06711(19) 0.0355(8) Uani 1 1 d . . . . .
H26A H 0.4159 0.6650 1.1191 0.043 Uiso 1 1 calc R U . . .
C27A C 0.4303(3) 0.71367(16) 1.0258(2) 0.0349(8) Uani 1 1 d . . . . .
H27A H 0.4599 0.7475 1.0489 0.042 Uiso 1 1 calc R U . . .
C28A C 0.4129(3) 0.71339(16) 0.9505(2) 0.0324(8) Uani 1 1 d . . . . .
H28A H 0.4302 0.7473 0.9216 0.039 Uiso 1 1 calc R U . . .
C29A C 0.3697(2) 0.66330(14) 0.91617(18) 0.0245(6) Uani 1 1 d . . . . .
H29A H 0.3575 0.6637 0.8643 0.029 Uiso 1 1 calc R U . . .
C30A C 0.48134(19) 0.54354(12) 0.82197(15) 0.0153(5) Uani 1 1 d . . . . .
H30A H 0.4791 0.5849 0.8423 0.018 Uiso 1 1 calc R U . . .
H30B H 0.5363 0.5413 0.7884 0.018 Uiso 1 1 calc R U . . .
C31A C 0.5823(2) 0.52798(13) 0.96404(16) 0.0175(6) Uani 1 1 d . . . . .
C32A C 0.6173(2) 0.49428(15) 1.02364(17) 0.0241(6) Uani 1 1 d . . . . .
H32A H 0.5949 0.4543 1.0304 0.029 Uiso 1 1 calc R U . . .
C33A C 0.6841(2) 0.51764(17) 1.07334(18) 0.0297(8) Uani 1 1 d . . . . .
H33A H 0.7081 0.4936 1.1131 0.036 Uiso 1 1 calc R U . . .
C34A C 0.7157(2) 0.57635(19) 1.0647(2) 0.0352(8) Uani 1 1 d . . . . .
H34A H 0.7602 0.5932 1.0992 0.042 Uiso 1 1 calc R U . . .
C35A C 0.6823(3) 0.60979(18) 1.0061(2) 0.0381(9) Uani 1 1 d . . . . .
H35A H 0.7048 0.6498 0.9996 0.046 Uiso 1 1 calc R U . . .
C36A C 0.6156(2) 0.58607(16) 0.95570(19) 0.0289(7) Uani 1 1 d . . . . .
H36A H 0.5931 0.6100 0.9154 0.035 Uiso 1 1 calc R U . . .
C37A C 0.58850(19) 0.43697(13) 0.85917(15) 0.0157(5) Uani 1 1 d . . . . .
C38A C 0.5692(2) 0.37660(14) 0.84865(16) 0.0197(6) Uani 1 1 d . . . . .
H38A H 0.5090 0.3610 0.8628 0.024 Uiso 1 1 calc R U . . .
C39A C 0.6368(2) 0.33777(14) 0.81741(18) 0.0247(7) Uani 1 1 d . . . . .
H39A H 0.6219 0.2964 0.8100 0.030 Uiso 1 1 calc R U . . .
C40A C 0.7249(2) 0.36006(16) 0.79759(19) 0.0284(7) Uani 1 1 d . . . . .
H40A H 0.7711 0.3342 0.7764 0.034 Uiso 1 1 calc R U . . .
C41A C 0.7451(2) 0.42000(17) 0.80879(19) 0.0293(7) Uani 1 1 d . . . . .
H41A H 0.8058 0.4352 0.7955 0.035 Uiso 1 1 calc R U . . .
C42A C 0.6783(2) 0.45876(15) 0.83921(17) 0.0227(6) Uani 1 1 d . . . . .
H42A H 0.6936 0.5000 0.8464 0.027 Uiso 1 1 calc R U . . .
C43A C 0.3833(2) 0.56457(13) 0.69279(15) 0.0167(6) Uani 1 1 d . . . . .
C44A C 0.2972(2) 0.57943(13) 0.65514(16) 0.0192(6) Uani 1 1 d . . . . .
H44A H 0.2386 0.5689 0.6776 0.023 Uiso 1 1 calc R U . . .
C45A C 0.2932(2) 0.60900(14) 0.58609(17) 0.0234(6) Uani 1 1 d . . . . .
H45A H 0.2332 0.6175 0.5630 0.028 Uiso 1 1 calc R U . . .
C46A C 0.3773(3) 0.62569(14) 0.55190(17) 0.0261(7) Uani 1 1 d . . . . .
H46A H 0.3752 0.6476 0.5068 0.031 Uiso 1 1 calc R U . . .
C47A C 0.4653(2) 0.60980(15) 0.58468(18) 0.0263(7) Uani 1 1 d . . . . .
H47A H 0.5231 0.6188 0.5603 0.032 Uiso 1 1 calc R U . . .
C48A C 0.4677(2) 0.58041(14) 0.65404(17) 0.0220(6) Uani 1 1 d . . . . .
H48A H 0.5281 0.5708 0.6758 0.026 Uiso 1 1 calc R U . . .
C49A C 0.2921(2) 0.69913(15) 0.72231(18) 0.0259(7) Uani 1 1 d . . . . .
C50A C 0.4013(2) 0.73902(15) 0.62536(18) 0.0269(7) Uani 1 1 d . . . . .
C51A C 0.4741(2) 0.67978(14) 0.73570(18) 0.0247(7) Uani 1 1 d . . . . .
B1A B 0.3821(2) 0.53068(14) 0.77381(17) 0.0138(6) Uani 1 1 d . . . . .
Cr1B Cr 0.85856(3) 0.45595(2) 0.35324(2) 0.01336(9) Uani 1 1 d . . . . .
Cr2B Cr 0.89468(3) 0.64549(2) 0.68174(3) 0.01805(10) Uani 1 1 d . . . . .
P1B P 0.82857(5) 0.43958(3) 0.48304(4) 0.01357(14) Uani 1 1 d . . . . .
P2B P 0.79801(5) 0.55566(3) 0.37297(4) 0.01396(14) Uani 1 1 d . . . . .
P3B P 1.01007(5) 0.49518(3) 0.39195(4) 0.01561(14) Uani 1 1 d . . . . .
O1B O 0.67444(16) 0.39749(11) 0.30633(14) 0.0315(5) Uani 1 1 d . . . . .
O2B O 0.94182(18) 0.33625(10) 0.31415(13) 0.0310(5) Uani 1 1 d . . . . .
O3B O 0.87551(18) 0.47066(12) 0.18913(12) 0.0327(6) Uani 1 1 d . . . . .
O4B O 0.8436(2) 0.54570(15) 0.7843(2) 0.0638(10) Uani 1 1 d . . . . .
O5B O 0.8647(2) 0.72693(15) 0.81066(16) 0.0529(8) Uani 1 1 d . . . . .
O6B O 0.68915(18) 0.65358(17) 0.63712(17) 0.0598(9) Uani 1 1 d . . . . .
C1B C 0.7432(2) 0.42236(14) 0.32734(16) 0.0193(6) Uani 1 1 d . . . . .
C2B C 0.9109(2) 0.38188(14) 0.33391(16) 0.0202(6) Uani 1 1 d . . . . .
C3B C 0.8718(2) 0.46835(14) 0.25425(17) 0.0202(6) Uani 1 1 d . . . . .
C4B C 0.89863(19) 0.48925(13) 0.54439(15) 0.0153(5) Uani 1 1 d . . . . .
H4BA H 0.8672 0.4918 0.5929 0.018 Uiso 1 1 calc R U . . .
H4BB H 0.9630 0.4717 0.5527 0.018 Uiso 1 1 calc R U . . .
C5B C 0.8495(2) 0.36150(13) 0.51355(16) 0.0170(6) Uani 1 1 d . . . . .
C6B C 0.8163(2) 0.31449(14) 0.46844(18) 0.0243(7) Uani 1 1 d . . . . .
H6BA H 0.7815 0.3234 0.4241 0.029 Uiso 1 1 calc R U . . .
C7B C 0.8336(3) 0.25523(15) 0.4877(2) 0.0340(8) Uani 1 1 d . . . . .
H7BA H 0.8111 0.2237 0.4563 0.041 Uiso 1 1 calc R U . . .
C8B C 0.8831(3) 0.24148(16) 0.5519(2) 0.0374(9) Uani 1 1 d . . . . .
H8BA H 0.8961 0.2007 0.5643 0.045 Uiso 1 1 calc R U . . .
C9B C 0.9140(2) 0.28738(17) 0.5986(2) 0.0353(8) Uani 1 1 d . . . . .
H9BA H 0.9472 0.2782 0.6435 0.042 Uiso 1 1 calc R U . . .
C10B C 0.8962(2) 0.34671(15) 0.57927(19) 0.0269(7) Uani 1 1 d . . . . .
H10B H 0.9166 0.3780 0.6118 0.032 Uiso 1 1 calc R U . . .
C11B C 0.70735(19) 0.44628(12) 0.52192(15) 0.0163(5) Uani 1 1 d . . . . .
C12B C 0.6268(2) 0.45853(14) 0.47870(16) 0.0198(6) Uani 1 1 d . . . . .
H12B H 0.6329 0.4645 0.4269 0.024 Uiso 1 1 calc R U . . .
C13B C 0.5373(2) 0.46221(15) 0.51015(17) 0.0240(6) Uani 1 1 d . . . . .
H13B H 0.4831 0.4717 0.4799 0.029 Uiso 1 1 calc R U . . .
C14B C 0.5263(2) 0.45217(15) 0.58496(17) 0.0246(6) Uani 1 1 d . . . . .
H14B H 0.4646 0.4537 0.6059 0.029 Uiso 1 1 calc R U . . .
C15B C 0.6057(2) 0.43986(15) 0.62922(17) 0.0248(7) Uani 1 1 d . . . . .
H15B H 0.5990 0.4334 0.6809 0.030 Uiso 1 1 calc R U . . .
C16B C 0.6954(2) 0.43696(14) 0.59754(17) 0.0220(6) Uani 1 1 d . . . . .
H16B H 0.7498 0.4284 0.6281 0.026 Uiso 1 1 calc R U . . .
C17B C 0.8084(2) 0.58046(13) 0.46961(15) 0.0151(5) Uani 1 1 d . . . . .
H17C H 0.8047 0.6250 0.4714 0.018 Uiso 1 1 calc R U . . .
H17D H 0.7540 0.5641 0.4976 0.018 Uiso 1 1 calc R U . . .
C18B C 0.6731(2) 0.56674(13) 0.34287(16) 0.0162(6) Uani 1 1 d . . . . .
C19B C 0.6454(2) 0.54641(13) 0.27212(16) 0.0192(6) Uani 1 1 d . . . . .
H19B H 0.6911 0.5270 0.2420 0.023 Uiso 1 1 calc R U . . .
C20B C 0.5530(2) 0.55407(14) 0.24530(18) 0.0250(7) Uani 1 1 d . . . . .
H20B H 0.5357 0.5400 0.1972 0.030 Uiso 1 1 calc R U . . .
C21B C 0.4860(2) 0.58220(15) 0.2886(2) 0.0279(7) Uani 1 1 d . . . . .
H21B H 0.4224 0.5874 0.2703 0.033 Uiso 1 1 calc R U . . .
C22B C 0.5114(2) 0.60281(16) 0.35852(19) 0.0293(7) Uani 1 1 d . . . . .
H22B H 0.4653 0.6222 0.3882 0.035 Uiso 1 1 calc R U . . .
C23B C 0.6048(2) 0.59511(14) 0.38562(17) 0.0218(6) Uani 1 1 d . . . . .
H23B H 0.6218 0.6094 0.4337 0.026 Uiso 1 1 calc R U . . .
C24B C 0.8486(2) 0.62060(14) 0.32154(16) 0.0192(6) Uani 1 1 d . . . . .
C25B C 0.9108(2) 0.61241(16) 0.26422(19) 0.0275(7) Uani 1 1 d . . . . .
H25B H 0.9304 0.5728 0.2515 0.033 Uiso 1 1 calc R U . . .
C26B C 0.9456(3) 0.66189(18) 0.2244(2) 0.0387(9) Uani 1 1 d . . . . .
H26B H 0.9887 0.6558 0.1850 0.046 Uiso 1 1 calc R U . . .
C27B C 0.9172(3) 0.71935(17) 0.2427(2) 0.0380(9) Uani 1 1 d . . . . .
H27B H 0.9405 0.7529 0.2159 0.046 Uiso 1 1 calc R U . . .
C28B C 0.8552(3) 0.72798(17) 0.2997(2) 0.0353(8) Uani 1 1 d . . . . .
H28B H 0.8363 0.7676 0.3127 0.042 Uiso 1 1 calc R U . . .
C29B C 0.8201(2) 0.67898(15) 0.33843(19) 0.0274(7) Uani 1 1 d . . . . .
H29B H 0.7760 0.6854 0.3770 0.033 Uiso 1 1 calc R U . . .
C30B C 1.0010(2) 0.56151(13) 0.45056(15) 0.0169(6) Uani 1 1 d . . . . .
H30C H 1.0614 0.5663 0.4793 0.020 Uiso 1 1 calc R U . . .
H30D H 0.9929 0.5975 0.4187 0.020 Uiso 1 1 calc R U . . .
C31B C 1.0917(2) 0.51622(15) 0.31748(16) 0.0213(6) Uani 1 1 d . . . . .
C32B C 1.1041(2) 0.47588(15) 0.25912(16) 0.0230(6) Uani 1 1 d . . . . .
H32B H 1.0706 0.4387 0.2586 0.028 Uiso 1 1 calc R U . . .
C33B C 1.1652(2) 0.48994(17) 0.20190(18) 0.0320(8) Uani 1 1 d . . . . .
H33B H 1.1728 0.4626 0.1620 0.038 Uiso 1 1 calc R U . . .
C34B C 1.2148(2) 0.54358(19) 0.20310(19) 0.0362(9) Uani 1 1 d . . . . .
H34B H 1.2576 0.5528 0.1644 0.043 Uiso 1 1 calc R U . . .
C35B C 1.2027(3) 0.58379(19) 0.2599(2) 0.0377(9) Uani 1 1 d . . . . .
H35B H 1.2364 0.6210 0.2599 0.045 Uiso 1 1 calc R U . . .
C36B C 1.1418(2) 0.57043(17) 0.31719(19) 0.0305(8) Uani 1 1 d . . . . .
H36B H 1.1341 0.5984 0.3565 0.037 Uiso 1 1 calc R U . . .
C37B C 1.0957(2) 0.44776(15) 0.44606(15) 0.0212(6) Uani 1 1 d . . . . .
C38B C 1.0767(2) 0.38825(15) 0.46338(17) 0.0237(7) Uani 1 1 d . . . . .
H38B H 1.0192 0.3701 0.4457 0.028 Uiso 1 1 calc R U . . .
C39B C 1.1411(3) 0.35468(18) 0.50665(18) 0.0329(8) Uani 1 1 d . . . . .
H39B H 1.1270 0.3141 0.5189 0.039 Uiso 1 1 calc R U . . .
C40B C 1.2257(3) 0.3807(2) 0.53170(19) 0.0383(10) Uani 1 1 d . . . . .
H40B H 1.2696 0.3579 0.5612 0.046 Uiso 1 1 calc R U . . .
C41B C 1.2461(2) 0.4388(2) 0.5140(2) 0.0387(9) Uani 1 1 d . . . . .
H41B H 1.3045 0.4563 0.5309 0.046 Uiso 1 1 calc R U . . .
C42B C 1.1825(2) 0.47280(17) 0.47163(19) 0.0300(8) Uani 1 1 d . . . . .
H42B H 1.1977 0.5133 0.4597 0.036 Uiso 1 1 calc R U . . .
C43B C 0.9466(2) 0.60534(13) 0.57350(16) 0.0174(6) Uani 1 1 d . . . . .
C44B C 1.0046(2) 0.58659(14) 0.63359(16) 0.0208(6) Uani 1 1 d . . . . .
H44B H 1.0134 0.5447 0.6417 0.025 Uiso 1 1 calc R U . . .
C45B C 1.0505(2) 0.62789(16) 0.68266(18) 0.0256(7) Uani 1 1 d . . . . .
H45B H 1.0912 0.6135 0.7215 0.031 Uiso 1 1 calc R U . . .
C46B C 1.0357(2) 0.68966(16) 0.67363(18) 0.0270(7) Uani 1 1 d . . . . .
H46B H 1.0651 0.7175 0.7069 0.032 Uiso 1 1 calc R U . . .
C47B C 0.9775(2) 0.71035(15) 0.61522(18) 0.0264(7) Uani 1 1 d . . . . .
H47B H 0.9675 0.7523 0.6084 0.032 Uiso 1 1 calc R U . . .
C48B C 0.9340(2) 0.66887(14) 0.56694(17) 0.0215(6) Uani 1 1 d . . . . .
H48B H 0.8941 0.6838 0.5279 0.026 Uiso 1 1 calc R U . . .
C49B C 0.8637(3) 0.58347(17) 0.7436(2) 0.0359(8) Uani 1 1 d . . . . .
C50B C 0.8744(2) 0.69559(17) 0.75974(19) 0.0302(7) Uani 1 1 d . . . . .
C51B C 0.7686(2) 0.65064(18) 0.65372(19) 0.0342(8) Uani 1 1 d . . . . .
B1B B 0.9098(2) 0.55819(14) 0.50954(17) 0.0151(6) Uani 1 1 d . . . . .
N1C N -0.0826(2) 0.29271(16) 1.0157(2) 0.0472(9) Uani 1 1 d . . . . .
C1C C 0.0094(3) 0.2983(2) 0.9736(2) 0.0474(11) Uani 1 1 d . . . . .
H1CA H -0.0066 0.3013 0.9201 0.057 Uiso 1 1 calc R U . . .
H1CB H 0.0412 0.3364 0.9885 0.057 Uiso 1 1 calc R U . . .
C2C C 0.0794(3) 0.2472(2) 0.9851(3) 0.0579(13) Uani 1 1 d . . . . .
H2CA H 0.1361 0.2543 0.9552 0.087 Uiso 1 1 calc R U . . .
H2CB H 0.0492 0.2093 0.9699 0.087 Uiso 1 1 calc R U . . .
H2CC H 0.0983 0.2450 1.0375 0.087 Uiso 1 1 calc R U . . .
C3C C -0.1352(3) 0.2347(2) 0.9947(3) 0.0592(14) Uani 1 1 d . . . . .
H3CA H -0.0950 0.2001 1.0101 0.071 Uiso 1 1 calc R U . . .
H3CB H -0.1949 0.2327 1.0232 0.071 Uiso 1 1 calc R U . . .
C4C C -0.1603(4) 0.2279(3) 0.9141(4) 0.0756(17) Uani 1 1 d . . . . .
H4CA H -0.1923 0.1892 0.9059 0.113 Uiso 1 1 calc R U . . .
H4CB H -0.1019 0.2295 0.8850 0.113 Uiso 1 1 calc R U . . .
H4CC H -0.2032 0.2607 0.8986 0.113 Uiso 1 1 calc R U . . .
C5C C -0.0613(4) 0.2887(2) 1.0976(3) 0.0599(13) Uani 1 1 d . . . . .
H5CA H -0.0247 0.2513 1.1075 0.072 Uiso 1 1 calc R U . . .
H5CB H -0.1225 0.2855 1.1240 0.072 Uiso 1 1 calc R U . . .
C6C C -0.0050(5) 0.3419(3) 1.1296(3) 0.0748(17) Uani 1 1 d . . . . .
H6CA H 0.0068 0.3355 1.1827 0.112 Uiso 1 1 calc R U . . .
H6CB H -0.0419 0.3791 1.1223 0.112 Uiso 1 1 calc R U . . .
H6CC H 0.0561 0.3454 1.1044 0.112 Uiso 1 1 calc R U . . .
C7C C -0.1419(4) 0.3472(2) 0.9933(4) 0.0696(15) Uani 1 1 d . . . . .
H7CA H -0.1047 0.3841 1.0045 0.083 Uiso 1 1 calc R U . . .
H7CB H -0.1541 0.3459 0.9392 0.083 Uiso 1 1 calc R U . . .
C8C C -0.2363(5) 0.3508(3) 1.0322(6) 0.135(4) Uani 1 1 d . . . . .
H8CA H -0.2669 0.3896 1.0210 0.202 Uiso 1 1 calc R U . . .
H8CB H -0.2255 0.3473 1.0857 0.202 Uiso 1 1 calc R U . . .
H8CC H -0.2780 0.3180 1.0150 0.202 Uiso 1 1 calc R U . . .
N1D N 0.38341(19) 0.35173(12) 0.24386(14) 0.0228(5) Uani 1 1 d . . . . .
C1D C 0.4876(2) 0.33655(15) 0.23196(18) 0.0252(7) Uani 1 1 d . . . . .
H1DA H 0.4918 0.2939 0.2163 0.030 Uiso 1 1 calc R U . . .
H1DB H 0.5224 0.3403 0.2800 0.030 Uiso 1 1 calc R U . . .
C2D C 0.5383(2) 0.37510(17) 0.17528(19) 0.0307(7) Uani 1 1 d . . . . .
H2DA H 0.6039 0.3606 0.1697 0.046 Uiso 1 1 calc R U . . .
H2DB H 0.5396 0.4171 0.1921 0.046 Uiso 1 1 calc R U . . .
H2DC H 0.5040 0.3725 0.1275 0.046 Uiso 1 1 calc R U . . .
C3D C 0.3258(2) 0.34736(16) 0.17115(18) 0.0284(7) Uani 1 1 d . . . . .
H3DA H 0.2579 0.3559 0.1815 0.034 Uiso 1 1 calc R U . . .
H3DB H 0.3485 0.3791 0.1372 0.034 Uiso 1 1 calc R U . . .
C4D C 0.3316(3) 0.28726(16) 0.13202(19) 0.0305(7) Uani 1 1 d . . . . .
H4DA H 0.2953 0.2892 0.0852 0.046 Uiso 1 1 calc R U . . .
H4DB H 0.3047 0.2558 0.1635 0.046 Uiso 1 1 calc R U . . .
H4DC H 0.3986 0.2778 0.1221 0.046 Uiso 1 1 calc R U . . .
C5D C 0.3725(2) 0.41613(15) 0.27060(18) 0.0282(7) Uani 1 1 d . . . . .
H5DA H 0.3978 0.4436 0.2325 0.034 Uiso 1 1 calc R U . . .
H5DB H 0.3036 0.4250 0.2756 0.034 Uiso 1 1 calc R U . . .
C6D C 0.4228(3) 0.42932(17) 0.34349(19) 0.0321(8) Uani 1 1 d . . . . .
H6DA H 0.4074 0.4704 0.3593 0.048 Uiso 1 1 calc R U . . .
H6DB H 0.4920 0.4256 0.3375 0.048 Uiso 1 1 calc R U . . .
H6DC H 0.4016 0.4006 0.3810 0.048 Uiso 1 1 calc R U . . .
C7D C 0.3459(2) 0.30734(15) 0.30015(19) 0.0284(7) Uani 1 1 d . . . . .
H7DA H 0.3468 0.2666 0.2780 0.034 Uiso 1 1 calc R U . . .
H7DB H 0.3902 0.3070 0.3435 0.034 Uiso 1 1 calc R U . . .
C8D C 0.2461(3) 0.31988(18) 0.3270(2) 0.0375(9) Uani 1 1 d . . . . .
H8DA H 0.2256 0.2868 0.3590 0.056 Uiso 1 1 calc R U . . .
H8DB H 0.2020 0.3233 0.2844 0.056 Uiso 1 1 calc R U . . .
H8DC H 0.2460 0.3577 0.3551 0.056 Uiso 1 1 calc R U . . .
O1E O 0.4586(2) 0.74429(11) 0.42125(15) 0.0433(7) Uani 1 1 d . . . . .
C1E C 0.3273(3) 0.7257(2) 0.3412(3) 0.0532(12) Uani 1 1 d . . . . .
H1EA H 0.2738 0.7443 0.3138 0.080 Uiso 1 1 calc R U . . .
H1EB H 0.3027 0.6959 0.3760 0.080 Uiso 1 1 calc R U . . .
H1EC H 0.3700 0.7059 0.3063 0.080 Uiso 1 1 calc R U . . .
C2E C 0.3804(3) 0.77227(19) 0.3822(3) 0.0528(12) Uani 1 1 d . . . . .
H2EA H 0.4047 0.8030 0.3475 0.063 Uiso 1 1 calc R U . . .
H2EB H 0.3378 0.7925 0.4177 0.063 Uiso 1 1 calc R U . . .
C3E C 0.5236(4) 0.78625(19) 0.4536(2) 0.0566(13) Uani 1 1 d . . . . .
H3EA H 0.4893 0.8132 0.4877 0.068 Uiso 1 1 calc R U . . .
H3EB H 0.5524 0.8112 0.4145 0.068 Uiso 1 1 calc R U . . .
C4E C 0.5999(4) 0.7529(2) 0.4950(3) 0.0585(13) Uani 1 1 d . . . . .
H4EA H 0.6447 0.7817 0.5177 0.088 Uiso 1 1 calc R U . . .
H4EB H 0.6341 0.7268 0.4608 0.088 Uiso 1 1 calc R U . . .
H4EC H 0.5710 0.7284 0.5337 0.088 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr1A C2A 1.823(3) . ?
Cr1A C3A 1.824(3) . ?
Cr1A C1A 1.828(3) . ?
Cr1A P1A 2.4004(8) . ?
Cr1A P3A 2.4016(8) . ?
Cr1A P2A 2.4068(9) . ?
Cr2A C51A 1.825(3) . ?
Cr2A C49A 1.839(3) . ?
Cr2A C50A 1.840(3) . ?
Cr2A C48A 2.203(3) . ?
Cr2A C46A 2.204(3) . ?
Cr2A C47A 2.212(3) . ?
Cr2A C44A 2.227(3) . ?
Cr2A C45A 2.236(3) . ?
Cr2A C43A 2.255(3) . ?
P1A C4A 1.819(3) . ?
P1A C5A 1.840(3) . ?
P1A C11A 1.842(3) . ?
P2A C17A 1.814(3) . ?
P2A C18A 1.847(3) . ?
P2A C24A 1.856(3) . ?
P3A C30A 1.827(3) . ?
P3A C31A 1.836(3) . ?
P3A C37A 1.860(3) . ?
O1A C1A 1.173(4) . ?
O2A C2A 1.166(4) . ?
O3A C3A 1.172(4) . ?
O4A C49A 1.156(4) . ?
O5A C50A 1.155(4) . ?
O6A C51A 1.156(4) . ?
C4A B1A 1.671(4) . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C5A C10A 1.387(4) . ?
C5A C6A 1.389(4) . ?
C6A C7A 1.381(5) . ?
C6A H6AA 0.9500 . ?
C7A C8A 1.372(5) . ?
C7A H7AA 0.9500 . ?
C8A C9A 1.383(5) . ?
C8A H8AA 0.9500 . ?
C9A C10A 1.392(4) . ?
C9A H9AA 0.9500 . ?
C10A H10A 0.9500 . ?
C11A C12A 1.393(4) . ?
C11A C16A 1.396(4) . ?
C12A C13A 1.388(4) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.387(5) . ?
C13A H13A 0.9500 . ?
C14A C15A 1.377(5) . ?
C14A H14A 0.9500 . ?
C15A C16A 1.389(5) . ?
C15A H15A 0.9500 . ?
C16A H16A 0.9500 . ?
C17A B1A 1.668(4) . ?
C17A H17A 0.9900 . ?
C17A H17B 0.9900 . ?
C18A C19A 1.388(4) . ?
C18A C23A 1.398(4) . ?
C19A C20A 1.398(5) . ?
C19A H19A 0.9500 . ?
C20A C21A 1.379(6) . ?
C20A H20A 0.9500 . ?
C21A C22A 1.385(6) . ?
C21A H21A 0.9500 . ?
C22A C23A 1.380(5) . ?
C22A H22A 0.9500 . ?
C23A H23A 0.9500 . ?
C24A C29A 1.383(4) . ?
C24A C25A 1.397(4) . ?
C25A C26A 1.382(5) . ?
C25A H25A 0.9500 . ?
C26A C27A 1.368(5) . ?
C26A H26A 0.9500 . ?
C27A C28A 1.378(5) . ?
C27A H27A 0.9500 . ?
C28A C29A 1.404(5) . ?
C28A H28A 0.9500 . ?
C29A H29A 0.9500 . ?
C30A B1A 1.649(4) . ?
C30A H30A 0.9900 . ?
C30A H30B 0.9900 . ?
C31A C36A 1.381(4) . ?
C31A C32A 1.393(4) . ?
C32A C33A 1.384(4) . ?
C32A H32A 0.9500 . ?
C33A C34A 1.386(6) . ?
C33A H33A 0.9500 . ?
C34A C35A 1.368(6) . ?
C34A H34A 0.9500 . ?
C35A C36A 1.394(5) . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
C37A C38A 1.380(4) . ?
C37A C42A 1.400(4) . ?
C38A C39A 1.405(4) . ?
C38A H38A 0.9500 . ?
C39A C40A 1.382(5) . ?
C39A H39A 0.9500 . ?
C40A C41A 1.375(5) . ?
C40A H40A 0.9500 . ?
C41A C42A 1.391(4) . ?
C41A H41A 0.9500 . ?
C42A H42A 0.9500 . ?
C43A C44A 1.412(4) . ?
C43A C48A 1.428(4) . ?
C43A B1A 1.646(4) . ?
C44A C45A 1.410(4) . ?
C44A H44A 0.9500 . ?
C45A C46A 1.389(5) . ?
C45A H45A 0.9500 . ?
C46A C47A 1.400(5) . ?
C46A H46A 0.9500 . ?
C47A C48A 1.412(4) . ?
C47A H47A 0.9500 . ?
C48A H48A 0.9500 . ?
Cr1B C3B 1.822(3) . ?
Cr1B C1B 1.830(3) . ?
Cr1B C2B 1.837(3) . ?
Cr1B P3B 2.3845(8) . ?
Cr1B P2B 2.3997(9) . ?
Cr1B P1B 2.4166(9) . ?
Cr2B C50B 1.821(3) . ?
Cr2B C51B 1.830(4) . ?
Cr2B C49B 1.830(4) . ?
Cr2B C44B 2.209(3) . ?
Cr2B C46B 2.211(3) . ?
Cr2B C45B 2.215(3) . ?
Cr2B C47B 2.216(3) . ?
Cr2B C48B 2.217(3) . ?
Cr2B C43B 2.280(3) . ?
P1B C4B 1.834(3) . ?
P1B C5B 1.841(3) . ?
P1B C11B 1.854(3) . ?
P2B C17B 1.833(3) . ?
P2B C18B 1.837(3) . ?
P2B C24B 1.862(3) . ?
P3B C30B 1.820(3) . ?
P3B C31B 1.841(3) . ?
P3B C37B 1.858(3) . ?
O1B C1B 1.167(4) . ?
O2B C2B 1.160(4) . ?
O3B C3B 1.179(4) . ?
O4B C49B 1.153(5) . ?
O5B C50B 1.163(4) . ?
O6B C51B 1.148(4) . ?
C4B B1B 1.664(4) . ?
C4B H4BA 0.9900 . ?
C4B H4BB 0.9900 . ?
C5B C10B 1.384(4) . ?
C5B C6B 1.398(4) . ?
C6B C7B 1.381(5) . ?
C6B H6BA 0.9500 . ?
C7B C8B 1.373(6) . ?
C7B H7BA 0.9500 . ?
C8B C9B 1.387(6) . ?
C8B H8BA 0.9500 . ?
C9B C10B 1.384(5) . ?
C9B H9BA 0.9500 . ?
C10B H10B 0.9500 . ?
C11B C12B 1.386(4) . ?
C11B C16B 1.394(4) . ?
C12B C13B 1.386(4) . ?
C12B H12B 0.9500 . ?
C13B C14B 1.381(4) . ?
C13B H13B 0.9500 . ?
C14B C15B 1.384(4) . ?
C14B H14B 0.9500 . ?
C15B C16B 1.390(4) . ?
C15B H15B 0.9500 . ?
C16B H16B 0.9500 . ?
C17B B1B 1.655(4) . ?
C17B H17C 0.9900 . ?
C17B H17D 0.9900 . ?
C18B C23B 1.391(4) . ?
C18B C19B 1.403(4) . ?
C19B C20B 1.382(4) . ?
C19B H19B 0.9500 . ?
C20B C21B 1.381(5) . ?
C20B H20B 0.9500 . ?
C21B C22B 1.383(5) . ?
C21B H21B 0.9500 . ?
C22B C23B 1.397(4) . ?
C22B H22B 0.9500 . ?
C23B H23B 0.9500 . ?
C24B C25B 1.377(5) . ?
C24B C29B 1.392(5) . ?
C25B C26B 1.405(5) . ?
C25B H25B 0.9500 . ?
C26B C27B 1.378(6) . ?
C26B H26B 0.9500 . ?
C27B C28B 1.371(6) . ?
C27B H27B 0.9500 . ?
C28B C29B 1.389(5) . ?
C28B H28B 0.9500 . ?
C29B H29B 0.9500 . ?
C30B B1B 1.679(4) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C31B C36B 1.393(5) . ?
C31B C32B 1.396(4) . ?
C32B C33B 1.389(5) . ?
C32B H32B 0.9500 . ?
C33B C34B 1.379(6) . ?
C33B H33B 0.9500 . ?
C34B C35B 1.373(5) . ?
C34B H34B 0.9500 . ?
C35B C36B 1.385(5) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
C37B C38B 1.385(5) . ?
C37B C42B 1.407(4) . ?
C38B C39B 1.398(4) . ?
C38B H38B 0.9500 . ?
C39B C40B 1.385(6) . ?
C39B H39B 0.9500 . ?
C40B C41B 1.362(6) . ?
C40B H40B 0.9500 . ?
C41B C42B 1.385(5) . ?
C41B H41B 0.9500 . ?
C42B H42B 0.9500 . ?
C43B C44B 1.406(4) . ?
C43B C48B 1.426(4) . ?
C43B B1B 1.635(4) . ?
C44B C45B 1.421(4) . ?
C44B H44B 0.9500 . ?
C45B C46B 1.396(5) . ?
C45B H45B 0.9500 . ?
C46B C47B 1.399(5) . ?
C46B H46B 0.9500 . ?
C47B C48B 1.400(4) . ?
C47B H47B 0.9500 . ?
C48B H48B 0.9500 . ?
N1C C5C 1.507(6) . ?
N1C C1C 1.512(5) . ?
N1C C7C 1.517(6) . ?
N1C C3C 1.527(6) . ?
C1C C2C 1.511(7) . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C2C H2CA 0.9800 . ?
C2C H2CB 0.9800 . ?
C2C H2CC 0.9800 . ?
C3C C4C 1.499(8) . ?
C3C H3CA 0.9900 . ?
C3C H3CB 0.9900 . ?
C4C H4CA 0.9800 . ?
C4C H4CB 0.9800 . ?
C4C H4CC 0.9800 . ?
C5C C6C 1.528(8) . ?
C5C H5CA 0.9900 . ?
C5C H5CB 0.9900 . ?
C6C H6CA 0.9800 . ?
C6C H6CB 0.9800 . ?
C6C H6CC 0.9800 . ?
C7C C8C 1.509(9) . ?
C7C H7CA 0.9900 . ?
C7C H7CB 0.9900 . ?
C8C H8CA 0.9800 . ?
C8C H8CB 0.9800 . ?
C8C H8CC 0.9800 . ?
N1D C1D 1.516(4) . ?
N1D C7D 1.517(4) . ?
N1D C5D 1.518(4) . ?
N1D C3D 1.531(4) . ?
C1D C2D 1.520(5) . ?
C1D H1DA 0.9900 . ?
C1D H1DB 0.9900 . ?
C2D H2DA 0.9800 . ?
C2D H2DB 0.9800 . ?
C2D H2DC 0.9800 . ?
C3D C4D 1.513(5) . ?
C3D H3DA 0.9900 . ?
C3D H3DB 0.9900 . ?
C4D H4DA 0.9800 . ?
C4D H4DB 0.9800 . ?
C4D H4DC 0.9800 . ?
C5D C6D 1.510(5) . ?
C5D H5DA 0.9900 . ?
C5D H5DB 0.9900 . ?
C6D H6DA 0.9800 . ?
C6D H6DB 0.9800 . ?
C6D H6DC 0.9800 . ?
C7D C8D 1.513(5) . ?
C7D H7DA 0.9900 . ?
C7D H7DB 0.9900 . ?
C8D H8DA 0.9800 . ?
C8D H8DB 0.9800 . ?
C8D H8DC 0.9800 . ?
O1E C3E 1.420(5) . ?
O1E C2E 1.433(5) . ?
C1E C2E 1.466(7) . ?
C1E H1EA 0.9800 . ?
C1E H1EB 0.9800 . ?
C1E H1EC 0.9800 . ?
C2E H2EA 0.9900 . ?
C2E H2EB 0.9900 . ?
C3E C4E 1.488(7) . ?
C3E H3EA 0.9900 . ?
C3E H3EB 0.9900 . ?
C4E H4EA 0.9800 . ?
C4E H4EB 0.9800 . ?
C4E H4EC 0.9800 . ?

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
C2A Cr1A C3A 85.28(13) . . ?
C2A Cr1A C1A 86.13(14) . . ?
C3A Cr1A C1A 86.93(13) . . ?
C2A Cr1A P1A 94.48(9) . . ?
C3A Cr1A P1A 179.65(10) . . ?
C1A Cr1A P1A 92.81(9) . . ?
C2A Cr1A P3A 90.83(10) . . ?
C3A Cr1A P3A 93.74(10) . . ?
C1A Cr1A P3A 176.82(10) . . ?
P1A Cr1A P3A 86.51(3) . . ?
C2A Cr1A P2A 174.97(10) . . ?
C3A Cr1A P2A 93.42(10) . . ?
C1A Cr1A P2A 98.67(10) . . ?
P1A Cr1A P2A 86.84(3) . . ?
P3A Cr1A P2A 84.40(3) . . ?
C51A Cr2A C49A 89.96(15) . . ?
C51A Cr2A C50A 89.53(14) . . ?
C49A Cr2A C50A 85.93(15) . . ?
C51A Cr2A C48A 81.88(13) . . ?
C49A Cr2A C48A 142.08(13) . . ?
C50A Cr2A C48A 130.63(13) . . ?
C51A Cr2A C46A 137.56(14) . . ?
C49A Cr2A C46A 132.27(14) . . ?
C50A Cr2A C46A 89.61(13) . . ?
C48A Cr2A C46A 67.07(12) . . ?
C51A Cr2A C47A 101.65(14) . . ?
C49A Cr2A C47A 167.23(14) . . ?
C50A Cr2A C47A 99.31(14) . . ?
C48A Cr2A C47A 37.31(11) . . ?
C46A Cr2A C47A 36.97(13) . . ?
C51A Cr2A C44A 126.09(12) . . ?
C49A Cr2A C44A 91.44(13) . . ?
C50A Cr2A C44A 144.32(13) . . ?
C48A Cr2A C44A 65.22(11) . . ?
C46A Cr2A C44A 66.28(12) . . ?
C47A Cr2A C44A 77.49(12) . . ?
C51A Cr2A C45A 158.41(13) . . ?
C49A Cr2A C45A 101.77(13) . . ?
C50A Cr2A C45A 109.15(13) . . ?
C48A Cr2A C45A 77.73(12) . . ?
C46A Cr2A C45A 36.46(12) . . ?
C47A Cr2A C45A 65.54(12) . . ?
C44A Cr2A C45A 36.83(11) . . ?
C51A Cr2A C43A 92.13(12) . . ?
C49A Cr2A C43A 106.82(13) . . ?
C50A Cr2A C43A 167.13(13) . . ?
C48A Cr2A C43A 37.35(11) . . ?
C46A Cr2A C43A 80.57(11) . . ?
C47A Cr2A C43A 67.86(11) . . ?
C44A Cr2A C43A 36.72(10) . . ?
C45A Cr2A C43A 67.25(11) . . ?
C4A P1A C5A 105.97(13) . . ?
C4A P1A C11A 101.42(13) . . ?
C5A P1A C11A 97.87(13) . . ?
C4A P1A Cr1A 114.29(9) . . ?
C5A P1A Cr1A 115.92(9) . . ?
C11A P1A Cr1A 119.04(9) . . ?
C17A P2A C18A 104.61(13) . . ?
C17A P2A C24A 105.30(14) . . ?
C18A P2A C24A 98.26(13) . . ?
C17A P2A Cr1A 112.34(10) . . ?
C18A P2A Cr1A 117.92(10) . . ?
C24A P2A Cr1A 116.62(10) . . ?
C30A P3A C31A 106.01(13) . . ?
C30A P3A C37A 102.44(13) . . ?
C31A P3A C37A 97.20(13) . . ?
C30A P3A Cr1A 115.92(9) . . ?
C31A P3A Cr1A 114.68(10) . . ?
C37A P3A Cr1A 118.17(10) . . ?
O1A C1A Cr1A 173.2(3) . . ?
O2A C2A Cr1A 173.9(3) . . ?
O3A C3A Cr1A 173.9(3) . . ?
B1A C4A P1A 112.60(18) . . ?
B1A C4A H4AA 109.1 . . ?
P1A C4A H4AA 109.1 . . ?
B1A C4A H4AB 109.1 . . ?
P1A C4A H4AB 109.1 . . ?
H4AA C4A H4AB 107.8 . . ?
C10A C5A C6A 118.0(3) . . ?
C10A C5A P1A 123.5(2) . . ?
C6A C5A P1A 118.5(2) . . ?
C7A C6A C5A 120.7(3) . . ?
C7A C6A H6AA 119.7 . . ?
C5A C6A H6AA 119.7 . . ?
C8A C7A C6A 120.8(3) . . ?
C8A C7A H7AA 119.6 . . ?
C6A C7A H7AA 119.6 . . ?
C7A C8A C9A 119.8(3) . . ?
C7A C8A H8AA 120.1 . . ?
C9A C8A H8AA 120.1 . . ?
C8A C9A C10A 119.3(3) . . ?
C8A C9A H9AA 120.4 . . ?
C10A C9A H9AA 120.4 . . ?
C5A C10A C9A 121.4(3) . . ?
C5A C10A H10A 119.3 . . ?
C9A C10A H10A 119.3 . . ?
C12A C11A C16A 118.2(3) . . ?
C12A C11A P1A 123.2(2) . . ?
C16A C11A P1A 118.6(2) . . ?
C13A C12A C11A 120.7(3) . . ?
C13A C12A H12A 119.7 . . ?
C11A C12A H12A 119.7 . . ?
C14A C13A C12A 120.2(3) . . ?
C14A C13A H13A 119.9 . . ?
C12A C13A H13A 119.9 . . ?
C15A C14A C13A 119.8(3) . . ?
C15A C14A H14A 120.1 . . ?
C13A C14A H14A 120.1 . . ?
C14A C15A C16A 120.0(3) . . ?
C14A C15A H15A 120.0 . . ?
C16A C15A H15A 120.0 . . ?
C15A C16A C11A 121.0(3) . . ?
C15A C16A H16A 119.5 . . ?
C11A C16A H16A 119.5 . . ?
B1A C17A P2A 115.49(19) . . ?
B1A C17A H17A 108.4 . . ?
P2A C17A H17A 108.4 . . ?
B1A C17A H17B 108.4 . . ?
P2A C17A H17B 108.4 . . ?
H17A C17A H17B 107.5 . . ?
C19A C18A C23A 118.1(3) . . ?
C19A C18A P2A 119.9(2) . . ?
C23A C18A P2A 122.0(2) . . ?
C18A C19A C20A 121.0(3) . . ?
C18A C19A H19A 119.5 . . ?
C20A C19A H19A 119.5 . . ?
C21A C20A C19A 119.8(4) . . ?
C21A C20A H20A 120.1 . . ?
C19A C20A H20A 120.1 . . ?
C20A C21A C22A 119.7(3) . . ?
C20A C21A H21A 120.2 . . ?
C22A C21A H21A 120.2 . . ?
C23A C22A C21A 120.5(4) . . ?
C23A C22A H22A 119.8 . . ?
C21A C22A H22A 119.8 . . ?
C22A C23A C18A 120.8(3) . . ?
C22A C23A H23A 119.6 . . ?
C18A C23A H23A 119.6 . . ?
C29A C24A C25A 118.0(3) . . ?
C29A C24A P2A 123.7(2) . . ?
C25A C24A P2A 118.3(2) . . ?
C26A C25A C24A 121.1(3) . . ?
C26A C25A H25A 119.5 . . ?
C24A C25A H25A 119.5 . . ?
C27A C26A C25A 120.7(3) . . ?
C27A C26A H26A 119.7 . . ?
C25A C26A H26A 119.7 . . ?
C26A C27A C28A 119.4(3) . . ?
C26A C27A H27A 120.3 . . ?
C28A C27A H27A 120.3 . . ?
C27A C28A C29A 120.4(3) . . ?
C27A C28A H28A 119.8 . . ?
C29A C28A H28A 119.8 . . ?
C24A C29A C28A 120.4(3) . . ?
C24A C29A H29A 119.8 . . ?
C28A C29A H29A 119.8 . . ?
B1A C30A P3A 113.26(18) . . ?
B1A C30A H30A 108.9 . . ?
P3A C30A H30A 108.9 . . ?
B1A C30A H30B 108.9 . . ?
P3A C30A H30B 108.9 . . ?
H30A C30A H30B 107.7 . . ?
C36A C31A C32A 118.1(3) . . ?
C36A C31A P3A 124.1(2) . . ?
C32A C31A P3A 117.6(2) . . ?
C33A C32A C31A 121.6(3) . . ?
C33A C32A H32A 119.2 . . ?
C31A C32A H32A 119.2 . . ?
C32A C33A C34A 119.4(3) . . ?
C32A C33A H33A 120.3 . . ?
C34A C33A H33A 120.3 . . ?
C35A C34A C33A 119.5(3) . . ?
C35A C34A H34A 120.2 . . ?
C33A C34A H34A 120.2 . . ?
C34A C35A C36A 121.0(4) . . ?
C34A C35A H35A 119.5 . . ?
C36A C35A H35A 119.5 . . ?
C31A C36A C35A 120.3(3) . . ?
C31A C36A H36A 119.8 . . ?
C35A C36A H36A 119.8 . . ?
C38A C37A C42A 118.3(3) . . ?
C38A C37A P3A 122.9(2) . . ?
C42A C37A P3A 118.8(2) . . ?
C37A C38A C39A 121.3(3) . . ?
C37A C38A H38A 119.3 . . ?
C39A C38A H38A 119.3 . . ?
C40A C39A C38A 119.6(3) . . ?
C40A C39A H39A 120.2 . . ?
C38A C39A H39A 120.2 . . ?
C41A C40A C39A 119.4(3) . . ?
C41A C40A H40A 120.3 . . ?
C39A C40A H40A 120.3 . . ?
C40A C41A C42A 121.3(3) . . ?
C40A C41A H41A 119.3 . . ?
C42A C41A H41A 119.3 . . ?
C41A C42A C37A 120.0(3) . . ?
C41A C42A H42A 120.0 . . ?
C37A C42A H42A 120.0 . . ?
C44A C43A C48A 114.4(3) . . ?
C44A C43A B1A 120.8(2) . . ?
C48A C43A B1A 124.8(3) . . ?
C44A C43A Cr2A 70.55(16) . . ?
C48A C43A Cr2A 69.34(17) . . ?
B1A C43A Cr2A 130.20(19) . . ?
C45A C44A C43A 123.6(3) . . ?
C45A C44A Cr2A 71.95(17) . . ?
C43A C44A Cr2A 72.74(17) . . ?
C45A C44A H44A 118.2 . . ?
C43A C44A H44A 118.2 . . ?
Cr2A C44A H44A 130.0 . . ?
C46A C45A C44A 119.9(3) . . ?
C46A C45A Cr2A 70.51(18) . . ?
C44A C45A Cr2A 71.22(17) . . ?
C46A C45A H45A 120.1 . . ?
C44A C45A H45A 120.1 . . ?
Cr2A C45A H45A 130.8 . . ?
C45A C46A C47A 119.3(3) . . ?
C45A C46A Cr2A 73.02(18) . . ?
C47A C46A Cr2A 71.82(18) . . ?
C45A C46A H46A 120.3 . . ?
C47A C46A H46A 120.3 . . ?
Cr2A C46A H46A 126.7 . . ?
C46A C47A C48A 119.9(3) . . ?
C46A C47A Cr2A 71.20(19) . . ?
C48A C47A Cr2A 70.99(18) . . ?
C46A C47A H47A 120.1 . . ?
C48A C47A H47A 120.1 . . ?
Cr2A C47A H47A 130.3 . . ?
C47A C48A C43A 122.8(3) . . ?
C47A C48A Cr2A 71.70(19) . . ?
C43A C48A Cr2A 73.31(17) . . ?
C47A C48A H48A 118.6 . . ?
C43A C48A H48A 118.6 . . ?
Cr2A C48A H48A 128.9 . . ?
O4A C49A Cr2A 177.4(3) . . ?
O5A C50A Cr2A 177.2(3) . . ?
O6A C51A Cr2A 177.7(3) . . ?
C43A B1A C30A 111.5(2) . . ?
C43A B1A C17A 106.7(2) . . ?
C30A B1A C17A 111.0(2) . . ?
C43A B1A C4A 106.0(2) . . ?
C30A B1A C4A 109.5(2) . . ?
C17A B1A C4A 111.9(2) . . ?
C3B Cr1B C1B 85.19(13) . . ?
C3B Cr1B C2B 84.30(13) . . ?
C1B Cr1B C2B 86.53(13) . . ?
C3B Cr1B P3B 97.26(10) . . ?
C1B Cr1B P3B 176.74(10) . . ?
C2B Cr1B P3B 91.56(10) . . ?
C3B Cr1B P2B 92.80(10) . . ?
C1B Cr1B P2B 95.85(10) . . ?
C2B Cr1B P2B 176.10(10) . . ?
P3B Cr1B P2B 86.20(3) . . ?
C3B Cr1B P1B 175.84(9) . . ?
C1B Cr1B P1B 91.05(9) . . ?
C2B Cr1B P1B 97.29(9) . . ?
P3B Cr1B P1B 86.56(3) . . ?
P2B Cr1B P1B 85.78(3) . . ?
C50B Cr2B C51B 90.73(15) . . ?
C50B Cr2B C49B 86.89(17) . . ?
C51B Cr2B C49B 88.74(17) . . ?
C50B Cr2B C44B 141.76(13) . . ?
C51B Cr2B C44B 127.05(14) . . ?
C49B Cr2B C44B 88.22(14) . . ?
C50B Cr2B C46B 86.11(14) . . ?
C51B Cr2B C46B 144.21(16) . . ?
C49B Cr2B C46B 126.57(15) . . ?
C44B Cr2B C46B 66.92(12) . . ?
C50B Cr2B C45B 105.61(14) . . ?
C51B Cr2B C45B 163.14(13) . . ?
C49B Cr2B C45B 96.13(15) . . ?
C44B Cr2B C45B 37.47(11) . . ?
C46B Cr2B C45B 36.77(13) . . ?
C50B Cr2B C47B 96.47(15) . . ?
C51B Cr2B C47B 108.69(15) . . ?
C49B Cr2B C47B 162.15(15) . . ?
C44B Cr2B C47B 78.27(12) . . ?
C46B Cr2B C47B 36.84(13) . . ?
C45B Cr2B C47B 66.06(13) . . ?
C50B Cr2B C48B 128.70(14) . . ?
C51B Cr2B C48B 88.93(14) . . ?
C49B Cr2B C48B 144.36(15) . . ?
C44B Cr2B C48B 65.41(12) . . ?
C46B Cr2B C48B 66.23(12) . . ?
C45B Cr2B C48B 77.71(12) . . ?
C47B Cr2B C48B 36.81(11) . . ?
C50B Cr2B C43B 163.49(14) . . ?
C51B Cr2B C43B 96.20(13) . . ?
C49B Cr2B C43B 108.17(15) . . ?
C44B Cr2B C43B 36.47(11) . . ?
C46B Cr2B C43B 79.50(11) . . ?
C45B Cr2B C43B 66.94(11) . . ?
C47B Cr2B C43B 67.12(11) . . ?
C48B Cr2B C43B 36.96(11) . . ?
C4B P1B C5B 107.78(13) . . ?
C4B P1B C11B 101.85(12) . . ?
C5B P1B C11B 95.95(13) . . ?
C4B P1B Cr1B 113.27(9) . . ?
C5B P1B Cr1B 113.73(10) . . ?
C11B P1B Cr1B 122.15(9) . . ?
C17B P2B C18B 107.44(13) . . ?
C17B P2B C24B 102.61(13) . . ?
C18B P2B C24B 96.70(13) . . ?
C17B P2B Cr1B 113.36(9) . . ?
C18B P2B Cr1B 114.59(9) . . ?
C24B P2B Cr1B 120.13(10) . . ?
C30B P3B C31B 105.71(14) . . ?
C30B P3B C37B 101.78(13) . . ?
C31B P3B C37B 97.20(13) . . ?
C30B P3B Cr1B 113.25(9) . . ?
C31B P3B Cr1B 116.04(10) . . ?
C37B P3B Cr1B 120.51(11) . . ?
O1B C1B Cr1B 173.6(3) . . ?
O2B C2B Cr1B 173.0(3) . . ?
O3B C3B Cr1B 172.9(3) . . ?
B1B C4B P1B 112.18(18) . . ?
B1B C4B H4BA 109.2 . . ?
P1B C4B H4BA 109.2 . . ?
B1B C4B H4BB 109.2 . . ?
P1B C4B H4BB 109.2 . . ?
H4BA C4B H4BB 107.9 . . ?
C10B C5B C6B 118.0(3) . . ?
C10B C5B P1B 123.4(2) . . ?
C6B C5B P1B 118.7(2) . . ?
C7B C6B C5B 120.6(3) . . ?
C7B C6B H6BA 119.7 . . ?
C5B C6B H6BA 119.7 . . ?
C8B C7B C6B 120.5(3) . . ?
C8B C7B H7BA 119.7 . . ?
C6B C7B H7BA 119.7 . . ?
C7B C8B C9B 119.8(3) . . ?
C7B C8B H8BA 120.1 . . ?
C9B C8B H8BA 120.1 . . ?
C10B C9B C8B 119.6(3) . . ?
C10B C9B H9BA 120.2 . . ?
C8B C9B H9BA 120.2 . . ?
C5B C10B C9B 121.4(3) . . ?
C5B C10B H10B 119.3 . . ?
C9B C10B H10B 119.3 . . ?
C12B C11B C16B 118.0(3) . . ?
C12B C11B P1B 122.9(2) . . ?
C16B C11B P1B 119.1(2) . . ?
C11B C12B C13B 120.8(3) . . ?
C11B C12B H12B 119.6 . . ?
C13B C12B H12B 119.6 . . ?
C14B C13B C12B 120.6(3) . . ?
C14B C13B H13B 119.7 . . ?
C12B C13B H13B 119.7 . . ?
C13B C14B C15B 119.6(3) . . ?
C13B C14B H14B 120.2 . . ?
C15B C14B H14B 120.2 . . ?
C14B C15B C16B 119.5(3) . . ?
C14B C15B H15B 120.2 . . ?
C16B C15B H15B 120.2 . . ?
C15B C16B C11B 121.4(3) . . ?
C15B C16B H16B 119.3 . . ?
C11B C16B H16B 119.3 . . ?
B1B C17B P2B 112.17(19) . . ?
B1B C17B H17C 109.2 . . ?
P2B C17B H17C 109.2 . . ?
B1B C17B H17D 109.2 . . ?
P2B C17B H17D 109.2 . . ?
H17C C17B H17D 107.9 . . ?
C23B C18B C19B 118.1(3) . . ?
C23B C18B P2B 123.8(2) . . ?
C19B C18B P2B 118.1(2) . . ?
C20B C19B C18B 121.3(3) . . ?
C20B C19B H19B 119.3 . . ?
C18B C19B H19B 119.3 . . ?
C21B C20B C19B 119.8(3) . . ?
C21B C20B H20B 120.1 . . ?
C19B C20B H20B 120.1 . . ?
C20B C21B C22B 120.1(3) . . ?
C20B C21B H21B 120.0 . . ?
C22B C21B H21B 120.0 . . ?
C21B C22B C23B 120.1(3) . . ?
C21B C22B H22B 119.9 . . ?
C23B C22B H22B 119.9 . . ?
C18B C23B C22B 120.6(3) . . ?
C18B C23B H23B 119.7 . . ?
C22B C23B H23B 119.7 . . ?
C25B C24B C29B 118.4(3) . . ?
C25B C24B P2B 121.6(2) . . ?
C29B C24B P2B 119.9(2) . . ?
C24B C25B C26B 120.8(3) . . ?
C24B C25B H25B 119.6 . . ?
C26B C25B H25B 119.6 . . ?
C27B C26B C25B 119.8(3) . . ?
C27B C26B H26B 120.1 . . ?
C25B C26B H26B 120.1 . . ?
C28B C27B C26B 119.9(3) . . ?
C28B C27B H27B 120.0 . . ?
C26B C27B H27B 120.0 . . ?
C27B C28B C29B 120.2(4) . . ?
C27B C28B H28B 119.9 . . ?
C29B C28B H28B 119.9 . . ?
C28B C29B C24B 120.9(3) . . ?
C28B C29B H29B 119.5 . . ?
C24B C29B H29B 119.5 . . ?
B1B C30B P3B 113.32(19) . . ?
B1B C30B H30C 108.9 . . ?
P3B C30B H30C 108.9 . . ?
B1B C30B H30D 108.9 . . ?
P3B C30B H30D 108.9 . . ?
H30C C30B H30D 107.7 . . ?
C36B C31B C32B 118.8(3) . . ?
C36B C31B P3B 122.8(2) . . ?
C32B C31B P3B 118.4(2) . . ?
C33B C32B C31B 120.3(3) . . ?
C33B C32B H32B 119.9 . . ?
C31B C32B H32B 119.9 . . ?
C34B C33B C32B 119.9(3) . . ?
C34B C33B H33B 120.0 . . ?
C32B C33B H33B 120.0 . . ?
C35B C34B C33B 120.3(3) . . ?
C35B C34B H34B 119.8 . . ?
C33B C34B H34B 119.8 . . ?
C34B C35B C36B 120.3(4) . . ?
C34B C35B H35B 119.8 . . ?
C36B C35B H35B 119.8 . . ?
C35B C36B C31B 120.3(3) . . ?
C35B C36B H36B 119.8 . . ?
C31B C36B H36B 119.8 . . ?
C38B C37B C42B 118.1(3) . . ?
C38B C37B P3B 122.3(2) . . ?
C42B C37B P3B 119.5(3) . . ?
C37B C38B C39B 120.7(3) . . ?
C37B C38B H38B 119.6 . . ?
C39B C38B H38B 119.6 . . ?
C40B C39B C38B 119.9(4) . . ?
C40B C39B H39B 120.0 . . ?
C38B C39B H39B 120.0 . . ?
C41B C40B C39B 120.0(3) . . ?
C41B C40B H40B 120.0 . . ?
C39B C40B H40B 120.0 . . ?
C40B C41B C42B 120.8(3) . . ?
C40B C41B H41B 119.6 . . ?
C42B C41B H41B 119.6 . . ?
C41B C42B C37B 120.5(4) . . ?
C41B C42B H42B 119.7 . . ?
C37B C42B H42B 119.7 . . ?
C44B C43B C48B 115.2(3) . . ?
C44B C43B B1B 121.7(3) . . ?
C48B C43B B1B 122.5(3) . . ?
C44B C43B Cr2B 69.04(16) . . ?
C48B C43B Cr2B 69.12(17) . . ?
B1B C43B Cr2B 139.05(19) . . ?
C43B C44B C45B 122.6(3) . . ?
C43B C44B Cr2B 74.49(17) . . ?
C45B C44B Cr2B 71.49(17) . . ?
C43B C44B H44B 118.7 . . ?
C45B C44B H44B 118.7 . . ?
Cr2B C44B H44B 127.5 . . ?
C46B C45B C44B 119.8(3) . . ?
C46B C45B Cr2B 71.47(18) . . ?
C44B C45B Cr2B 71.04(17) . . ?
C46B C45B H45B 120.1 . . ?
C44B C45B H45B 120.1 . . ?
Cr2B C45B H45B 129.8 . . ?
C45B C46B C47B 119.6(3) . . ?
C45B C46B Cr2B 71.76(18) . . ?
C47B C46B Cr2B 71.77(18) . . ?
C45B C46B H46B 120.2 . . ?
C47B C46B H46B 120.2 . . ?
Cr2B C46B H46B 128.5 . . ?
C46B C47B C48B 119.6(3) . . ?
C46B C47B Cr2B 71.39(19) . . ?
C48B C47B Cr2B 71.61(18) . . ?
C46B C47B H47B 120.2 . . ?
C48B C47B H47B 120.2 . . ?
Cr2B C47B H47B 129.1 . . ?
C47B C48B C43B 123.2(3) . . ?
C47B C48B Cr2B 71.58(18) . . ?
C43B C48B Cr2B 73.92(17) . . ?
C47B C48B H48B 118.4 . . ?
C43B C48B H48B 118.4 . . ?
Cr2B C48B H48B 128.6 . . ?
O4B C49B Cr2B 177.8(4) . . ?
O5B C50B Cr2B 177.5(3) . . ?
O6B C51B Cr2B 179.0(4) . . ?
C43B B1B C17B 111.9(2) . . ?
C43B B1B C4B 110.6(2) . . ?
C17B B1B C4B 110.8(2) . . ?
C43B B1B C30B 100.8(2) . . ?
C17B B1B C30B 111.5(2) . . ?
C4B B1B C30B 111.0(2) . . ?
C5C N1C C1C 110.1(3) . . ?
C5C N1C C7C 113.9(4) . . ?
C1C N1C C7C 105.5(3) . . ?
C5C N1C C3C 106.2(4) . . ?
C1C N1C C3C 110.9(4) . . ?
C7C N1C C3C 110.4(3) . . ?
C2C C1C N1C 115.2(3) . . ?
C2C C1C H1CA 108.5 . . ?
N1C C1C H1CA 108.5 . . ?
C2C C1C H1CB 108.5 . . ?
N1C C1C H1CB 108.5 . . ?
H1CA C1C H1CB 107.5 . . ?
C1C C2C H2CA 109.5 . . ?
C1C C2C H2CB 109.5 . . ?
H2CA C2C H2CB 109.5 . . ?
C1C C2C H2CC 109.5 . . ?
H2CA C2C H2CC 109.5 . . ?
H2CB C2C H2CC 109.5 . . ?
C4C C3C N1C 115.4(4) . . ?
C4C C3C H3CA 108.4 . . ?
N1C C3C H3CA 108.4 . . ?
C4C C3C H3CB 108.4 . . ?
N1C C3C H3CB 108.4 . . ?
H3CA C3C H3CB 107.5 . . ?
C3C C4C H4CA 109.5 . . ?
C3C C4C H4CB 109.5 . . ?
H4CA C4C H4CB 109.5 . . ?
C3C C4C H4CC 109.5 . . ?
H4CA C4C H4CC 109.5 . . ?
H4CB C4C H4CC 109.5 . . ?
N1C C5C C6C 114.7(4) . . ?
N1C C5C H5CA 108.6 . . ?
C6C C5C H5CA 108.6 . . ?
N1C C5C H5CB 108.6 . . ?
C6C C5C H5CB 108.6 . . ?
H5CA C5C H5CB 107.6 . . ?
C5C C6C H6CA 109.5 . . ?
C5C C6C H6CB 109.5 . . ?
H6CA C6C H6CB 109.5 . . ?
C5C C6C H6CC 109.5 . . ?
H6CA C6C H6CC 109.5 . . ?
H6CB C6C H6CC 109.5 . . ?
C8C C7C N1C 113.5(5) . . ?
C8C C7C H7CA 108.9 . . ?
N1C C7C H7CA 108.9 . . ?
C8C C7C H7CB 108.9 . . ?
N1C C7C H7CB 108.9 . . ?
H7CA C7C H7CB 107.7 . . ?
C7C C8C H8CA 109.5 . . ?
C7C C8C H8CB 109.5 . . ?
H8CA C8C H8CB 109.5 . . ?
C7C C8C H8CC 109.5 . . ?
H8CA C8C H8CC 109.5 . . ?
H8CB C8C H8CC 109.5 . . ?
C1D N1D C7D 107.2(2) . . ?
C1D N1D C5D 110.9(2) . . ?
C7D N1D C5D 111.2(2) . . ?
C1D N1D C3D 110.9(2) . . ?
C7D N1D C3D 110.5(2) . . ?
C5D N1D C3D 106.2(2) . . ?
N1D C1D C2D 115.6(3) . . ?
N1D C1D H1DA 108.4 . . ?
C2D C1D H1DA 108.4 . . ?
N1D C1D H1DB 108.4 . . ?
C2D C1D H1DB 108.4 . . ?
H1DA C1D H1DB 107.4 . . ?
C1D C2D H2DA 109.5 . . ?
C1D C2D H2DB 109.5 . . ?
H2DA C2D H2DB 109.5 . . ?
C1D C2D H2DC 109.5 . . ?
H2DA C2D H2DC 109.5 . . ?
H2DB C2D H2DC 109.5 . . ?
C4D C3D N1D 115.1(3) . . ?
C4D C3D H3DA 108.5 . . ?
N1D C3D H3DA 108.5 . . ?
C4D C3D H3DB 108.5 . . ?
N1D C3D H3DB 108.5 . . ?
H3DA C3D H3DB 107.5 . . ?
C3D C4D H4DA 109.5 . . ?
C3D C4D H4DB 109.5 . . ?
H4DA C4D H4DB 109.5 . . ?
C3D C4D H4DC 109.5 . . ?
H4DA C4D H4DC 109.5 . . ?
H4DB C4D H4DC 109.5 . . ?
C6D C5D N1D 114.4(3) . . ?
C6D C5D H5DA 108.7 . . ?
N1D C5D H5DA 108.7 . . ?
C6D C5D H5DB 108.7 . . ?
N1D C5D H5DB 108.7 . . ?
H5DA C5D H5DB 107.6 . . ?
C5D C6D H6DA 109.5 . . ?
C5D C6D H6DB 109.5 . . ?
H6DA C6D H6DB 109.5 . . ?
C5D C6D H6DC 109.5 . . ?
H6DA C6D H6DC 109.5 . . ?
H6DB C6D H6DC 109.5 . . ?
C8D C7D N1D 115.4(3) . . ?
C8D C7D H7DA 108.4 . . ?
N1D C7D H7DA 108.4 . . ?
C8D C7D H7DB 108.4 . . ?
N1D C7D H7DB 108.4 . . ?
H7DA C7D H7DB 107.5 . . ?
C7D C8D H8DA 109.5 . . ?
C7D C8D H8DB 109.5 . . ?
H8DA C8D H8DB 109.5 . . ?
C7D C8D H8DC 109.5 . . ?
H8DA C8D H8DC 109.5 . . ?
H8DB C8D H8DC 109.5 . . ?
C3E O1E C2E 113.3(3) . . ?
C2E C1E H1EA 109.5 . . ?
C2E C1E H1EB 109.5 . . ?
H1EA C1E H1EB 109.5 . . ?
C2E C1E H1EC 109.5 . . ?
H1EA C1E H1EC 109.5 . . ?
H1EB C1E H1EC 109.5 . . ?
O1E C2E C1E 108.5(3) . . ?
O1E C2E H2EA 110.0 . . ?
C1E C2E H2EA 110.0 . . ?
O1E C2E H2EB 110.0 . . ?
C1E C2E H2EB 110.0 . . ?
H2EA C2E H2EB 108.4 . . ?
O1E C3E C4E 109.1(4) . . ?
O1E C3E H3EA 109.9 . . ?
C4E C3E H3EA 109.9 . . ?
O1E C3E H3EB 109.9 . . ?
C4E C3E H3EB 109.9 . . ?
H3EA C3E H3EB 108.3 . . ?
C3E C4E H4EA 109.5 . . ?
C3E C4E H4EB 109.5 . . ?
H4EA C4E H4EB 109.5 . . ?
C3E C4E H4EC 109.5 . . ?
H4EA C4E H4EC 109.5 . . ?
H4EB C4E H4EC 109.5 . . ?

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
C5A P1A C4A B1A -166.73(18) . . . . ?
C11A P1A C4A B1A 91.5(2) . . . . ?
Cr1A P1A C4A B1A -37.8(2) . . . . ?
C4A P1A C5A C10A -4.0(3) . . . . ?
C11A P1A C5A C10A 100.3(3) . . . . ?
Cr1A P1A C5A C10A -132.0(2) . . . . ?
C4A P1A C5A C6A 175.1(2) . . . . ?
C11A P1A C5A C6A -80.6(3) . . . . ?
Cr1A P1A C5A C6A 47.1(3) . . . . ?
C10A C5A C6A C7A -0.8(5) . . . . ?
P1A C5A C6A C7A -179.9(3) . . . . ?
C5A C6A C7A C8A 1.7(6) . . . . ?
C6A C7A C8A C9A -1.3(6) . . . . ?
C7A C8A C9A C10A 0.1(5) . . . . ?
C6A C5A C10A C9A -0.5(5) . . . . ?
P1A C5A C10A C9A 178.6(2) . . . . ?
C8A C9A C10A C5A 0.8(5) . . . . ?
C4A P1A C11A C12A -131.2(3) . . . . ?
C5A P1A C11A C12A 120.6(3) . . . . ?
Cr1A P1A C11A C12A -4.9(3) . . . . ?
C4A P1A C11A C16A 46.6(3) . . . . ?
C5A P1A C11A C16A -61.5(3) . . . . ?
Cr1A P1A C11A C16A 173.0(2) . . . . ?
C16A C11A C12A C13A -2.1(5) . . . . ?
P1A C11A C12A C13A 175.8(3) . . . . ?
C11A C12A C13A C14A 0.1(6) . . . . ?
C12A C13A C14A C15A 1.0(7) . . . . ?
C13A C14A C15A C16A -0.1(7) . . . . ?
C14A C15A C16A C11A -2.0(6) . . . . ?
C12A C11A C16A C15A 3.1(5) . . . . ?
P1A C11A C16A C15A -174.9(3) . . . . ?
C18A P2A C17A B1A -165.7(2) . . . . ?
C24A P2A C17A B1A 91.2(2) . . . . ?
Cr1A P2A C17A B1A -36.7(2) . . . . ?
C17A P2A C18A C19A 161.5(3) . . . . ?
C24A P2A C18A C19A -90.3(3) . . . . ?
Cr1A P2A C18A C19A 35.8(3) . . . . ?
C17A P2A C18A C23A -18.2(3) . . . . ?
C24A P2A C18A C23A 90.1(3) . . . . ?
Cr1A P2A C18A C23A -143.8(2) . . . . ?
C23A C18A C19A C20A 1.9(5) . . . . ?
P2A C18A C19A C20A -177.8(3) . . . . ?
C18A C19A C20A C21A 0.0(6) . . . . ?
C19A C20A C21A C22A -1.3(7) . . . . ?
C20A C21A C22A C23A 0.6(6) . . . . ?
C21A C22A C23A C18A 1.4(6) . . . . ?
C19A C18A C23A C22A -2.6(5) . . . . ?
P2A C18A C23A C22A 177.1(3) . . . . ?
C17A P2A C24A C29A 5.7(3) . . . . ?
C18A P2A C24A C29A -102.0(3) . . . . ?
Cr1A P2A C24A C29A 131.0(2) . . . . ?
C17A P2A C24A C25A -175.4(2) . . . . ?
C18A P2A C24A C25A 76.9(3) . . . . ?
Cr1A P2A C24A C25A -50.1(3) . . . . ?
C29A C24A C25A C26A -1.4(5) . . . . ?
P2A C24A C25A C26A 179.6(3) . . . . ?
C24A C25A C26A C27A 0.4(6) . . . . ?
C25A C26A C27A C28A 0.5(6) . . . . ?
C26A C27A C28A C29A -0.4(6) . . . . ?
C25A C24A C29A C28A 1.4(5) . . . . ?
P2A C24A C29A C28A -179.7(2) . . . . ?
C27A C28A C29A C24A -0.6(5) . . . . ?
C31A P3A C30A B1A -158.24(19) . . . . ?
C37A P3A C30A B1A 100.4(2) . . . . ?
Cr1A P3A C30A B1A -29.7(2) . . . . ?
C30A P3A C31A C36A 3.0(3) . . . . ?
C37A P3A C31A C36A 108.2(3) . . . . ?
Cr1A P3A C31A C36A -126.2(3) . . . . ?
C30A P3A C31A C32A -172.8(2) . . . . ?
C37A P3A C31A C32A -67.6(2) . . . . ?
Cr1A P3A C31A C32A 58.0(2) . . . . ?
C36A C31A C32A C33A -0.3(5) . . . . ?
P3A C31A C32A C33A 175.8(2) . . . . ?
C31A C32A C33A C34A 1.3(5) . . . . ?
C32A C33A C34A C35A -1.7(5) . . . . ?
C33A C34A C35A C36A 1.2(6) . . . . ?
C32A C31A C36A C35A -0.2(5) . . . . ?
P3A C31A C36A C35A -176.0(3) . . . . ?
C34A C35A C36A C31A -0.2(6) . . . . ?
C30A P3A C37A C38A -117.6(2) . . . . ?
C31A P3A C37A C38A 134.1(3) . . . . ?
Cr1A P3A C37A C38A 11.1(3) . . . . ?
C30A P3A C37A C42A 62.0(2) . . . . ?
C31A P3A C37A C42A -46.2(2) . . . . ?
Cr1A P3A C37A C42A -169.21(19) . . . . ?
C42A C37A C38A C39A -1.2(4) . . . . ?
P3A C37A C38A C39A 178.5(2) . . . . ?
C37A C38A C39A C40A 0.8(5) . . . . ?
C38A C39A C40A C41A 0.0(5) . . . . ?
C39A C40A C41A C42A -0.4(5) . . . . ?
C40A C41A C42A C37A 0.1(5) . . . . ?
C38A C37A C42A C41A 0.8(4) . . . . ?
P3A C37A C42A C41A -178.9(2) . . . . ?
C48A C43A C44A C45A -1.8(4) . . . . ?
B1A C43A C44A C45A 179.3(3) . . . . ?
Cr2A C43A C44A C45A 53.4(3) . . . . ?
C48A C43A C44A Cr2A -55.2(2) . . . . ?
B1A C43A C44A Cr2A 125.9(2) . . . . ?
C43A C44A C45A C46A -0.7(5) . . . . ?
Cr2A C44A C45A C46A 53.0(3) . . . . ?
C43A C44A C45A Cr2A -53.7(3) . . . . ?
C44A C45A C46A C47A 3.6(5) . . . . ?
Cr2A C45A C46A C47A 56.9(3) . . . . ?
C44A C45A C46A Cr2A -53.4(3) . . . . ?
C45A C46A C47A C48A -3.9(5) . . . . ?
Cr2A C46A C47A C48A 53.7(3) . . . . ?
C45A C46A C47A Cr2A -57.5(3) . . . . ?
C46A C47A C48A C43A 1.3(5) . . . . ?
Cr2A C47A C48A C43A 55.1(3) . . . . ?
C46A C47A C48A Cr2A -53.8(3) . . . . ?
C44A C43A C48A C47A 1.5(4) . . . . ?
B1A C43A C48A C47A -179.7(3) . . . . ?
Cr2A C43A C48A C47A -54.3(3) . . . . ?
C44A C43A C48A Cr2A 55.8(2) . . . . ?
B1A C43A C48A Cr2A -125.3(3) . . . . ?
C44A C43A B1A C30A -155.7(3) . . . . ?
C48A C43A B1A C30A 25.5(4) . . . . ?
Cr2A C43A B1A C30A -65.9(3) . . . . ?
C44A C43A B1A C17A -34.3(3) . . . . ?
C48A C43A B1A C17A 147.0(3) . . . . ?
Cr2A C43A B1A C17A 55.5(3) . . . . ?
C44A C43A B1A C4A 85.2(3) . . . . ?
C48A C43A B1A C4A -93.6(3) . . . . ?
Cr2A C43A B1A C4A 174.97(19) . . . . ?
P3A C30A B1A C43A -162.62(19) . . . . ?
P3A C30A B1A C17A 78.5(2) . . . . ?
P3A C30A B1A C4A -45.6(3) . . . . ?
P2A C17A B1A C43A -161.95(19) . . . . ?
P2A C17A B1A C30A -40.2(3) . . . . ?
P2A C17A B1A C4A 82.5(3) . . . . ?
P1A C4A B1A C43A -153.01(18) . . . . ?
P1A C4A B1A C30A 86.5(2) . . . . ?
P1A C4A B1A C17A -37.0(3) . . . . ?
C5B P1B C4B B1B 164.35(19) . . . . ?
C11B P1B C4B B1B -95.4(2) . . . . ?
Cr1B P1B C4B B1B 37.6(2) . . . . ?
C4B P1B C5B C10B 10.5(3) . . . . ?
C11B P1B C5B C10B -94.0(3) . . . . ?
Cr1B P1B C5B C10B 136.9(2) . . . . ?
C4B P1B C5B C6B -169.8(2) . . . . ?
C11B P1B C5B C6B 85.7(2) . . . . ?
Cr1B P1B C5B C6B -43.4(3) . . . . ?
C10B C5B C6B C7B -2.8(5) . . . . ?
P1B C5B C6B C7B 177.5(3) . . . . ?
C5B C6B C7B C8B 0.5(5) . . . . ?
C6B C7B C8B C9B 1.5(6) . . . . ?
C7B C8B C9B C10B -1.2(5) . . . . ?
C6B C5B C10B C9B 3.1(5) . . . . ?
P1B C5B C10B C9B -177.2(3) . . . . ?
C8B C9B C10B C5B -1.1(5) . . . . ?
C4B P1B C11B C12B 130.2(3) . . . . ?
C5B P1B C11B C12B -120.2(3) . . . . ?
Cr1B P1B C11B C12B 2.7(3) . . . . ?
C4B P1B C11B C16B -51.7(3) . . . . ?
C5B P1B C11B C16B 57.9(3) . . . . ?
Cr1B P1B C11B C16B -179.2(2) . . . . ?
C16B C11B C12B C13B 0.9(4) . . . . ?
P1B C11B C12B C13B 179.0(2) . . . . ?
C11B C12B C13B C14B -1.7(5) . . . . ?
C12B C13B C14B C15B 1.7(5) . . . . ?
C13B C14B C15B C16B -0.9(5) . . . . ?
C14B C15B C16B C11B 0.1(5) . . . . ?
C12B C11B C16B C15B -0.1(5) . . . . ?
P1B C11B C16B C15B -178.3(2) . . . . ?
C18B P2B C17B B1B 166.43(19) . . . . ?
C24B P2B C17B B1B -92.3(2) . . . . ?
Cr1B P2B C17B B1B 38.8(2) . . . . ?
C17B P2B C18B C23B 6.3(3) . . . . ?
C24B P2B C18B C23B -99.2(3) . . . . ?
Cr1B P2B C18B C23B 133.2(2) . . . . ?
C17B P2B C18B C19B -175.0(2) . . . . ?
C24B P2B C18B C19B 79.5(2) . . . . ?
Cr1B P2B C18B C19B -48.0(2) . . . . ?
C23B C18B C19B C20B -0.1(4) . . . . ?
P2B C18B C19B C20B -179.0(2) . . . . ?
C18B C19B C20B C21B -0.1(5) . . . . ?
C19B C20B C21B C22B 0.2(5) . . . . ?
C20B C21B C22B C23B -0.2(5) . . . . ?
C19B C18B C23B C22B 0.1(4) . . . . ?
P2B C18B C23B C22B 178.9(3) . . . . ?
C21B C22B C23B C18B 0.0(5) . . . . ?
C17B P2B C24B C25B 136.3(3) . . . . ?
C18B P2B C24B C25B -114.1(3) . . . . ?
Cr1B P2B C24B C25B 9.4(3) . . . . ?
C17B P2B C24B C29B -46.7(3) . . . . ?
C18B P2B C24B C29B 62.9(3) . . . . ?
Cr1B P2B C24B C29B -173.6(2) . . . . ?
C29B C24B C25B C26B 0.8(5) . . . . ?
P2B C24B C25B C26B 177.8(3) . . . . ?
C24B C25B C26B C27B -0.1(5) . . . . ?
C25B C26B C27B C28B 0.1(6) . . . . ?
C26B C27B C28B C29B -0.8(6) . . . . ?
C27B C28B C29B C24B 1.5(5) . . . . ?
C25B C24B C29B C28B -1.5(5) . . . . ?
P2B C24B C29B C28B -178.6(3) . . . . ?
C31B P3B C30B B1B 165.73(19) . . . . ?
C37B P3B C30B B1B -93.2(2) . . . . ?
Cr1B P3B C30B B1B 37.6(2) . . . . ?
C30B P3B C31B C36B 7.2(3) . . . . ?
C37B P3B C31B C36B -97.2(3) . . . . ?
Cr1B P3B C31B C36B 133.7(2) . . . . ?
C30B P3B C31B C32B -173.1(2) . . . . ?
C37B P3B C31B C32B 82.5(3) . . . . ?
Cr1B P3B C31B C32B -46.7(3) . . . . ?
C36B C31B C32B C33B -0.2(5) . . . . ?
P3B C31B C32B C33B -179.9(2) . . . . ?
C31B C32B C33B C34B 0.8(5) . . . . ?
C32B C33B C34B C35B -1.3(5) . . . . ?
C33B C34B C35B C36B 1.1(6) . . . . ?
C34B C35B C36B C31B -0.4(6) . . . . ?
C32B C31B C36B C35B -0.1(5) . . . . ?
P3B C31B C36B C35B 179.6(3) . . . . ?
C30B P3B C37B C38B 128.6(2) . . . . ?
C31B P3B C37B C38B -123.6(3) . . . . ?
Cr1B P3B C37B C38B 2.4(3) . . . . ?
C30B P3B C37B C42B -50.5(3) . . . . ?
C31B P3B C37B C42B 57.3(3) . . . . ?
Cr1B P3B C37B C42B -176.7(2) . . . . ?
C42B C37B C38B C39B 1.6(4) . . . . ?
P3B C37B C38B C39B -177.5(2) . . . . ?
C37B C38B C39B C40B -1.0(5) . . . . ?
C38B C39B C40B C41B -0.2(5) . . . . ?
C39B C40B C41B C42B 0.6(5) . . . . ?
C40B C41B C42B C37B 0.0(5) . . . . ?
C38B C37B C42B C41B -1.1(5) . . . . ?
P3B C37B C42B C41B 178.0(3) . . . . ?
C48B C43B C44B C45B -2.4(4) . . . . ?
B1B C43B C44B C45B 169.1(3) . . . . ?
Cr2B C43B C44B C45B -55.4(3) . . . . ?
C48B C43B C44B Cr2B 53.0(2) . . . . ?
B1B C43B C44B Cr2B -135.6(3) . . . . ?
C43B C44B C45B C46B 2.5(5) . . . . ?
Cr2B C44B C45B C46B -54.3(3) . . . . ?
C43B C44B C45B Cr2B 56.7(3) . . . . ?
C44B C45B C46B C47B -1.5(5) . . . . ?
Cr2B C45B C46B C47B -55.5(3) . . . . ?
C44B C45B C46B Cr2B 54.1(3) . . . . ?
C45B C46B C47B C48B 0.6(5) . . . . ?
Cr2B C46B C47B C48B -54.9(3) . . . . ?
C45B C46B C47B Cr2B 55.5(3) . . . . ?
C46B C47B C48B C43B -0.6(5) . . . . ?
Cr2B C47B C48B C43B -55.5(3) . . . . ?
C46B C47B C48B Cr2B 54.8(3) . . . . ?
C44B C43B C48B C47B 1.5(4) . . . . ?
B1B C43B C48B C47B -169.9(3) . . . . ?
Cr2B C43B C48B C47B 54.4(3) . . . . ?
C44B C43B C48B Cr2B -53.0(2) . . . . ?
B1B C43B C48B Cr2B 135.7(3) . . . . ?
C44B C43B B1B C17B 153.5(3) . . . . ?
C48B C43B B1B C17B -35.7(4) . . . . ?
Cr2B C43B B1B C17B 59.5(4) . . . . ?
C44B C43B B1B C4B 29.5(4) . . . . ?
C48B C43B B1B C4B -159.6(3) . . . . ?
Cr2B C43B B1B C4B -64.5(4) . . . . ?
C44B C43B B1B C30B -87.9(3) . . . . ?
C48B C43B B1B C30B 82.9(3) . . . . ?
Cr2B C43B B1B C30B 178.1(2) . . . . ?
P2B C17B B1B C43B 149.8(2) . . . . ?
P2B C17B B1B C4B -86.3(2) . . . . ?
P2B C17B B1B C30B 37.8(3) . . . . ?
P1B C4B B1B C43B 164.83(18) . . . . ?
P1B C4B B1B C17B 40.2(3) . . . . ?
P1B C4B B1B C30B -84.1(2) . . . . ?
P3B C30B B1B C43B 157.05(19) . . . . ?
P3B C30B B1B C17B -84.1(3) . . . . ?
P3B C30B B1B C4B 39.8(3) . . . . ?
C5C N1C C1C C2C 58.8(5) . . . . ?
C7C N1C C1C C2C -177.9(4) . . . . ?
C3C N1C C1C C2C -58.5(5) . . . . ?
C5C N1C C3C C4C -177.7(4) . . . . ?
C1C N1C C3C C4C -58.1(5) . . . . ?
C7C N1C C3C C4C 58.4(6) . . . . ?
C1C N1C C5C C6C 57.8(5) . . . . ?
C7C N1C C5C C6C -60.4(5) . . . . ?
C3C N1C C5C C6C 177.9(4) . . . . ?
C5C N1C C7C C8C -57.1(7) . . . . ?
C1C N1C C7C C8C -177.9(6) . . . . ?
C3C N1C C7C C8C 62.3(7) . . . . ?
C7D N1D C1D C2D 178.3(3) . . . . ?
C5D N1D C1D C2D -60.1(3) . . . . ?
C3D N1D C1D C2D 57.6(4) . . . . ?
C1D N1D C3D C4D 55.9(4) . . . . ?
C7D N1D C3D C4D -62.9(4) . . . . ?
C5D N1D C3D C4D 176.5(3) . . . . ?
C1D N1D C5D C6D -60.9(3) . . . . ?
C7D N1D C5D C6D 58.3(4) . . . . ?
C3D N1D C5D C6D 178.6(3) . . . . ?
C1D N1D C7D C8D 172.5(3) . . . . ?
C5D N1D C7D C8D 51.1(4) . . . . ?
C3D N1D C7D C8D -66.5(4) . . . . ?
C3E O1E C2E C1E 170.7(3) . . . . ?
C2E O1E C3E C4E 177.9(3) . . . . ?

_refine_diff_density_max         0.577
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.051

_shelxl_version_number           2014-3


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Et2O'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_14167aaa
_database_code_depnum_ccdc_archive 'CCDC 1039155'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        '[Et4N][Cr(CO)3{6-(PhBP3)Mo(CO)3}]'
_chemical_name_common            14167aaa
_chemical_melting_point          562-563
_chemical_formula_moiety         'C51 H651 B Cr Mo O6 P3, C8 H20 N, C4 H8 O'
_chemical_formula_sum            'C63 H69 B Cr Mo N O7 P3'
_chemical_formula_weight         1203.85

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'
N N 0.0061 0.0033 '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'
B B 0.0013 0.0007 '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'
Cr Cr 0.3209 0.6236 '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                   12.2709(17)
_cell_length_b                   33.329(5)
_cell_length_c                   14.548(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.4969(18)
_cell_angle_gamma                90
_cell_volume                     5944.2(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2977
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      27.68

_exptl_crystal_description       Needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_F_000             2504
_exptl_transmission_factor_min   0.4430
_exptl_transmission_factor_max   0.4915
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.527
_shelx_estimated_absorpt_T_min   0.797
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4430
_exptl_absorpt_correction_T_max  0.4915
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'

_exptl_special_details           'Prof. P. Fischer'

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            69510
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.528
_diffrn_reflns_theta_max         27.737
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13814
_reflns_number_gt                10110
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0700P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13814
_refine_ls_number_parameters     653
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1291
_refine_ls_wR_factor_gt          0.1200
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.002
_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
Mo1 Mo 0.34547(2) 0.67872(2) 0.02248(2) 0.02206(8) Uani 1 1 d . . . . .
C1 C 0.4979(2) 0.69516(9) 0.0473(2) 0.0302(7) Uani 1 1 d . . . . .
O1 O 0.58504(17) 0.70864(7) 0.05853(17) 0.0437(6) Uani 1 1 d . . . . .
C2 C 0.3728(2) 0.69458(9) -0.1039(2) 0.0288(6) Uani 1 1 d . . . . .
O2 O 0.39419(19) 0.70469(7) -0.17742(16) 0.0435(6) Uani 1 1 d . . . . .
C3 C 0.3135(2) 0.73521(9) 0.0469(2) 0.0288(6) Uani 1 1 d . . . . .
O3 O 0.29961(18) 0.76951(6) 0.05814(17) 0.0426(6) Uani 1 1 d . . . . .
C4 C 0.3046(2) 0.56999(8) 0.0585(2) 0.0239(6) Uani 1 1 d . . . . .
H4A H 0.2926 0.5450 0.0227 0.029 Uiso 1 1 calc R U . . .
H4B H 0.3502 0.5631 0.1141 0.029 Uiso 1 1 calc R U . . .
C5 C 0.5253(2) 0.59045(8) 0.0023(2) 0.0268(6) Uani 1 1 d . . . . .
C6 C 0.6001(2) 0.61364(10) -0.0439(2) 0.0353(7) Uani 1 1 d . . . . .
H6A H 0.5747 0.6352 -0.0819 0.042 Uiso 1 1 calc R U . . .
C7 C 0.7108(2) 0.60585(10) -0.0352(3) 0.0419(8) Uani 1 1 d . . . . .
H7A H 0.7606 0.6214 -0.0685 0.050 Uiso 1 1 calc R U . . .
C8 C 0.7486(3) 0.57538(11) 0.0220(3) 0.0438(9) Uani 1 1 d . . . . .
H8A H 0.8247 0.5706 0.0298 0.053 Uiso 1 1 calc R U . . .
C9 C 0.6763(3) 0.55197(11) 0.0675(3) 0.0469(9) Uani 1 1 d . . . . .
H9A H 0.7026 0.5310 0.1067 0.056 Uiso 1 1 calc R U . . .
C10 C 0.5643(2) 0.55890(10) 0.0565(2) 0.0383(8) Uani 1 1 d . . . . .
H10A H 0.5145 0.5419 0.0862 0.046 Uiso 1 1 calc R U . . .
C11 C 0.3496(2) 0.58555(8) -0.12806(19) 0.0262(6) Uani 1 1 d . . . . .
C12 C 0.2790(2) 0.60546(9) -0.1896(2) 0.0294(6) Uani 1 1 d . . . . .
H12A H 0.2531 0.6314 -0.1743 0.035 Uiso 1 1 calc R U . . .
C13 C 0.2453(3) 0.58823(10) -0.2735(2) 0.0348(7) Uani 1 1 d . . . . .
H13A H 0.1949 0.6019 -0.3137 0.042 Uiso 1 1 calc R U . . .
C14 C 0.2853(3) 0.55122(10) -0.2979(2) 0.0412(8) Uani 1 1 d . . . . .
H14A H 0.2627 0.5393 -0.3550 0.049 Uiso 1 1 calc R U . . .
C15 C 0.3583(3) 0.53169(10) -0.2391(2) 0.0483(9) Uani 1 1 d . . . . .
H15A H 0.3867 0.5063 -0.2560 0.058 Uiso 1 1 calc R U . . .
C16 C 0.3910(3) 0.54865(10) -0.1551(2) 0.0407(8) Uani 1 1 d . . . . .
H16A H 0.4422 0.5349 -0.1156 0.049 Uiso 1 1 calc R U . . .
P1 P 0.38083(6) 0.60506(2) -0.01107(5) 0.02299(16) Uani 1 1 d . . . . .
C17 C 0.2000(2) 0.61646(8) 0.18274(19) 0.0246(6) Uani 1 1 d . . . . .
H17A H 0.2074 0.5996 0.2387 0.030 Uiso 1 1 calc R U . . .
H17B H 0.1327 0.6325 0.1873 0.030 Uiso 1 1 calc R U . . .
C18 C 0.4305(2) 0.62217(9) 0.2385(2) 0.0316(7) Uani 1 1 d . . . . .
C19 C 0.5360(3) 0.63319(14) 0.2227(3) 0.0559(11) Uani 1 1 d . . . . .
H19A H 0.5496 0.6556 0.1844 0.067 Uiso 1 1 calc R U . . .
C20 C 0.6236(3) 0.61153(17) 0.2627(3) 0.0696(14) Uani 1 1 d . . . . .
H20A H 0.6960 0.6193 0.2505 0.084 Uiso 1 1 calc R U . . .
C21 C 0.6072(4) 0.57996(13) 0.3182(3) 0.0626(13) Uani 1 1 d . . . . .
H21A H 0.6674 0.5657 0.3453 0.075 Uiso 1 1 calc R U . . .
C22 C 0.5044(4) 0.56892(12) 0.3349(3) 0.0690(14) Uani 1 1 d . . . . .
H22A H 0.4922 0.5467 0.3740 0.083 Uiso 1 1 calc R U . . .
C23 C 0.4149(3) 0.58991(10) 0.2951(3) 0.0552(11) Uani 1 1 d . . . . .
H23A H 0.3428 0.5817 0.3074 0.066 Uiso 1 1 calc R U . . .
C24 C 0.2908(2) 0.68747(9) 0.2743(2) 0.0266(6) Uani 1 1 d . . . . .
C25 C 0.3472(2) 0.72342(9) 0.2746(2) 0.0334(7) Uani 1 1 d . . . . .
H25A H 0.3993 0.7283 0.2295 0.040 Uiso 1 1 calc R U . . .
C26 C 0.3281(3) 0.75248(10) 0.3403(2) 0.0397(8) Uani 1 1 d . . . . .
H26A H 0.3698 0.7765 0.3415 0.048 Uiso 1 1 calc R U . . .
C27 C 0.2501(3) 0.74695(11) 0.4034(2) 0.0422(8) Uani 1 1 d . . . . .
H27A H 0.2356 0.7673 0.4468 0.051 Uiso 1 1 calc R U . . .
P2 P 0.31562(6) 0.65065(2) 0.18246(5) 0.02413(16) Uani 1 1 d . . . . .
C28 C 0.1924(3) 0.71118(11) 0.4030(2) 0.0478(9) Uani 1 1 d . . . . .
H28A H 0.1376 0.7071 0.4462 0.057 Uiso 1 1 calc R U . . .
C29 C 0.2139(3) 0.68134(10) 0.3402(2) 0.0393(8) Uani 1 1 d . . . . .
H29A H 0.1758 0.6565 0.3421 0.047 Uiso 1 1 calc R U . . .
C30 C 0.1135(2) 0.60845(8) 0.0052(2) 0.0238(6) Uani 1 1 d . . . . .
H30A H 0.0348 0.6057 0.0161 0.029 Uiso 1 1 calc R U . . .
H30B H 0.1278 0.5942 -0.0528 0.029 Uiso 1 1 calc R U . . .
C31 C 0.0433(2) 0.68616(8) 0.0617(2) 0.0251(6) Uani 1 1 d . . . . .
C32 C 0.0734(2) 0.71187(8) 0.1332(2) 0.0280(6) Uani 1 1 d . . . . .
H32A H 0.1482 0.7184 0.1443 0.034 Uiso 1 1 calc R U . . .
C33 C -0.0041(3) 0.72812(10) 0.1890(2) 0.0356(7) Uani 1 1 d . . . . .
H33A H 0.0179 0.7455 0.2382 0.043 Uiso 1 1 calc R U . . .
C34 C -0.1133(3) 0.71915(10) 0.1732(2) 0.0391(8) Uani 1 1 d . . . . .
H34A H -0.1664 0.7305 0.2110 0.047 Uiso 1 1 calc R U . . .
C35 C -0.1447(2) 0.69360(11) 0.1023(2) 0.0409(8) Uani 1 1 d . . . . .
H35A H -0.2196 0.6871 0.0917 0.049 Uiso 1 1 calc R U . . .
C36 C -0.0672(2) 0.67736(10) 0.0462(2) 0.0347(7) Uani 1 1 d . . . . .
H36A H -0.0896 0.6601 -0.0030 0.042 Uiso 1 1 calc R U . . .
C37 C 0.0917(2) 0.67606(8) -0.1249(2) 0.0248(6) Uani 1 1 d . . . . .
C38 C 0.1262(2) 0.71280(8) -0.1609(2) 0.0287(6) Uani 1 1 d . . . . .
H38A H 0.1714 0.7301 -0.1239 0.034 Uiso 1 1 calc R U . . .
C39 C 0.0951(2) 0.72418(10) -0.2501(2) 0.0349(7) Uani 1 1 d . . . . .
H39A H 0.1190 0.7491 -0.2735 0.042 Uiso 1 1 calc R U . . .
C40 C 0.0303(3) 0.69965(10) -0.3044(2) 0.0378(8) Uani 1 1 d . . . . .
H40A H 0.0103 0.7074 -0.3657 0.045 Uiso 1 1 calc R U . . .
C41 C -0.0061(3) 0.66370(10) -0.2704(2) 0.0364(7) Uani 1 1 d . . . . .
H41A H -0.0521 0.6470 -0.3080 0.044 Uiso 1 1 calc R U . . .
C42 C 0.0244(2) 0.65171(9) -0.1807(2) 0.0300(6) Uani 1 1 d . . . . .
H42A H -0.0008 0.6269 -0.1578 0.036 Uiso 1 1 calc R U . . .
P3 P 0.14548(5) 0.66179(2) -0.00918(5) 0.02155(15) Uani 1 1 d . . . . .
B1 B 0.1848(2) 0.58633(9) 0.0916(2) 0.0230(6) Uani 1 1 d . . . . .
C43 C 0.1086(2) 0.54837(8) 0.12143(19) 0.0243(6) Uani 1 1 d . . . . .
C44 C 0.0298(2) 0.55274(9) 0.1883(2) 0.0339(7) Uani 1 1 d . . . . .
H44A H 0.0245 0.5778 0.2188 0.041 Uiso 1 1 calc R U . . .
C45 C -0.0419(3) 0.52148(10) 0.2121(2) 0.0404(8) Uani 1 1 d . . . . .
H45A H -0.0949 0.5261 0.2565 0.048 Uiso 1 1 calc R U . . .
C46 C -0.0352(2) 0.48441(9) 0.1712(2) 0.0357(7) Uani 1 1 d . . . . .
H46A H -0.0818 0.4632 0.1883 0.043 Uiso 1 1 calc R U . . .
C47 C 0.0417(3) 0.47838(9) 0.1037(2) 0.0339(7) Uani 1 1 d . . . . .
H47A H 0.0462 0.4532 0.0736 0.041 Uiso 1 1 calc R U . . .
C48 C 0.1117(2) 0.50969(9) 0.0808(2) 0.0305(7) Uani 1 1 d . . . . .
H48A H 0.1639 0.5048 0.0358 0.037 Uiso 1 1 calc R U . . .
Cr1 Cr 0.13033(4) 0.49939(2) 0.22967(4) 0.03317(13) Uani 1 1 d . . . . .
C49 C 0.1369(3) 0.45069(12) 0.2850(3) 0.0539(10) Uani 1 1 d . . . . .
O4 O 0.1445(3) 0.41917(9) 0.3202(3) 0.0880(11) Uani 1 1 d . . . . .
C50 C 0.2766(3) 0.49390(11) 0.2129(3) 0.0472(9) Uani 1 1 d . . . . .
O5 O 0.3698(2) 0.48994(9) 0.2038(2) 0.0686(8) Uani 1 1 d . . . . .
C51 C 0.1678(4) 0.52245(13) 0.3402(3) 0.0594(11) Uani 1 1 d . . . . .
O6 O 0.1955(3) 0.53660(12) 0.4109(2) 0.1007(13) Uani 1 1 d . . . . .
N1 N 0.4615(2) 0.35479(8) 0.40737(19) 0.0396(7) Uani 1 1 d . . . . .
C52 C 0.5819(3) 0.36451(14) 0.4261(3) 0.0666(12) Uani 1 1 d . . . . .
H52A H 0.6003 0.3880 0.3881 0.080 Uiso 1 1 calc R U . . .
H52B H 0.5920 0.3727 0.4914 0.080 Uiso 1 1 calc R U . . .
C53 C 0.6613(4) 0.33222(14) 0.4086(4) 0.0749(14) Uani 1 1 d . . . . .
H53A H 0.7350 0.3414 0.4266 0.112 Uiso 1 1 calc R U . . .
H53B H 0.6578 0.3255 0.3429 0.112 Uiso 1 1 calc R U . . .
H53C H 0.6436 0.3084 0.4445 0.112 Uiso 1 1 calc R U . . .
C54 C 0.4457(4) 0.34547(17) 0.3044(3) 0.0803(15) Uani 1 1 d . . . . .
H54A H 0.4749 0.3682 0.2693 0.096 Uiso 1 1 calc R U . . .
H54B H 0.4899 0.3215 0.2905 0.096 Uiso 1 1 calc R U . . .
C55 C 0.3304(4) 0.33793(19) 0.2703(3) 0.0881(17) Uani 1 1 d . . . . .
H55A H 0.3300 0.3282 0.2067 0.132 Uiso 1 1 calc R U . . .
H55B H 0.2886 0.3629 0.2726 0.132 Uiso 1 1 calc R U . . .
H55C H 0.2972 0.3177 0.3092 0.132 Uiso 1 1 calc R U . . .
C56 C 0.3926(4) 0.38886(14) 0.4333(4) 0.0762(14) Uani 1 1 d . . . . .
H56A H 0.3158 0.3812 0.4192 0.091 Uiso 1 1 calc R U . . .
H56B H 0.4010 0.3920 0.5010 0.091 Uiso 1 1 calc R U . . .
C57 C 0.4094(5) 0.42811(15) 0.3928(5) 0.107(2) Uani 1 1 d . . . . .
H57A H 0.3529 0.4466 0.4125 0.160 Uiso 1 1 calc R U . . .
H57B H 0.4051 0.4258 0.3255 0.160 Uiso 1 1 calc R U . . .
H57C H 0.4814 0.4383 0.4129 0.160 Uiso 1 1 calc R U . . .
C58 C 0.4316(4) 0.31697(15) 0.4586(3) 0.0761(14) Uani 1 1 d . . . . .
H58A H 0.3518 0.3132 0.4497 0.091 Uiso 1 1 calc R U . . .
H58B H 0.4669 0.2941 0.4282 0.091 Uiso 1 1 calc R U . . .
C59 C 0.4578(4) 0.31398(15) 0.5545(3) 0.0817(15) Uani 1 1 d . . . . .
H59A H 0.4217 0.2904 0.5794 0.123 Uiso 1 1 calc R U . . .
H59B H 0.4327 0.3382 0.5856 0.123 Uiso 1 1 calc R U . . .
H59C H 0.5369 0.3114 0.5646 0.123 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C2 1.955(3) . ?
Mo1 C3 1.959(3) . ?
Mo1 C1 1.967(3) . ?
Mo1 P3 2.5406(8) . ?
Mo1 P1 2.5441(8) . ?
Mo1 P2 2.5496(9) . ?
C1 O1 1.165(3) . ?
C2 O2 1.163(4) . ?
C3 O3 1.168(3) . ?
C4 B1 1.659(4) . ?
C4 P1 1.829(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.387(4) . ?
C5 C6 1.395(4) . ?
C5 P1 1.840(3) . ?
C6 C7 1.383(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.380(5) . ?
C7 H7A 0.9500 . ?
C8 C9 1.374(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.396(4) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C12 1.387(4) . ?
C11 C16 1.394(4) . ?
C11 P1 1.846(3) . ?
C12 C13 1.395(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.380(5) . ?
C13 H13A 0.9500 . ?
C14 C15 1.376(5) . ?
C14 H14A 0.9500 . ?
C15 C16 1.389(5) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 B1 1.667(4) . ?
C17 P2 1.820(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C23 1.372(5) . ?
C18 C19 1.375(5) . ?
C18 P2 1.858(3) . ?
C19 C20 1.400(5) . ?
C19 H19A 0.9500 . ?
C20 C21 1.347(6) . ?
C20 H20A 0.9500 . ?
C21 C22 1.346(6) . ?
C21 H21A 0.9500 . ?
C22 C23 1.406(5) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 C25 1.384(4) . ?
C24 C29 1.389(4) . ?
C24 P2 1.849(3) . ?
C25 C26 1.388(4) . ?
C25 H25A 0.9500 . ?
C26 C27 1.367(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.387(5) . ?
C27 H27A 0.9500 . ?
C28 C29 1.384(5) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 B1 1.671(4) . ?
C30 P3 1.834(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.386(4) . ?
C31 C36 1.395(4) . ?
C31 P3 1.846(3) . ?
C32 C33 1.386(4) . ?
C32 H32A 0.9500 . ?
C33 C34 1.382(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.380(5) . ?
C34 H34A 0.9500 . ?
C35 C36 1.389(4) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 C42 1.393(4) . ?
C37 C38 1.404(4) . ?
C37 P3 1.844(3) . ?
C38 C39 1.389(4) . ?
C38 H38A 0.9500 . ?
C39 C40 1.368(5) . ?
C39 H39A 0.9500 . ?
C40 C41 1.378(5) . ?
C40 H40A 0.9500 . ?
C41 C42 1.400(4) . ?
C41 H41A 0.9500 . ?
C42 H42A 0.9500 . ?
B1 C43 1.643(4) . ?
C43 C44 1.409(4) . ?
C43 C48 1.419(4) . ?
C43 Cr1 2.276(3) . ?
C44 C45 1.416(4) . ?
C44 Cr1 2.232(3) . ?
C44 H44A 0.9500 . ?
C45 C46 1.375(5) . ?
C45 Cr1 2.242(3) . ?
C45 H45A 0.9500 . ?
C46 C47 1.406(4) . ?
C46 Cr1 2.224(3) . ?
C46 H46A 0.9500 . ?
C47 C48 1.400(4) . ?
C47 Cr1 2.204(3) . ?
C47 H47A 0.9500 . ?
C48 Cr1 2.195(3) . ?
C48 H48A 0.9500 . ?
Cr1 C49 1.812(4) . ?
Cr1 C51 1.823(4) . ?
Cr1 C50 1.830(4) . ?
C49 O4 1.171(4) . ?
C50 O5 1.165(4) . ?
C51 O6 1.168(5) . ?
N1 C56 1.475(5) . ?
N1 C58 1.518(5) . ?
N1 C52 1.525(5) . ?
N1 C54 1.534(5) . ?
C52 C53 1.482(6) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C55 1.500(6) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 C57 1.454(7) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C59 1.421(6) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?

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 Mo1 C3 87.41(12) . . ?
C2 Mo1 C1 84.07(12) . . ?
C3 Mo1 C1 83.98(12) . . ?
C2 Mo1 P3 95.35(9) . . ?
C3 Mo1 P3 92.69(8) . . ?
C1 Mo1 P3 176.65(9) . . ?
C2 Mo1 P1 92.46(9) . . ?
C3 Mo1 P1 178.21(8) . . ?
C1 Mo1 P1 97.77(9) . . ?
P3 Mo1 P1 85.54(2) . . ?
C2 Mo1 P2 174.01(9) . . ?
C3 Mo1 P2 98.57(9) . . ?
C1 Mo1 P2 96.21(9) . . ?
P3 Mo1 P2 84.72(2) . . ?
P1 Mo1 P2 81.57(3) . . ?
O1 C1 Mo1 173.2(3) . . ?
O2 C2 Mo1 176.5(3) . . ?
O3 C3 Mo1 175.9(3) . . ?
B1 C4 P1 115.57(18) . . ?
B1 C4 H4A 108.4 . . ?
P1 C4 H4A 108.4 . . ?
B1 C4 H4B 108.4 . . ?
P1 C4 H4B 108.4 . . ?
H4A C4 H4B 107.4 . . ?
C10 C5 C6 118.4(3) . . ?
C10 C5 P1 124.6(2) . . ?
C6 C5 P1 117.0(2) . . ?
C7 C6 C5 121.1(3) . . ?
C7 C6 H6A 119.4 . . ?
C5 C6 H6A 119.4 . . ?
C8 C7 C6 119.7(3) . . ?
C8 C7 H7A 120.1 . . ?
C6 C7 H7A 120.1 . . ?
C9 C8 C7 120.1(3) . . ?
C9 C8 H8A 119.9 . . ?
C7 C8 H8A 119.9 . . ?
C8 C9 C10 120.3(3) . . ?
C8 C9 H9A 119.9 . . ?
C10 C9 H9A 119.9 . . ?
C5 C10 C9 120.3(3) . . ?
C5 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C12 C11 C16 117.7(3) . . ?
C12 C11 P1 121.7(2) . . ?
C16 C11 P1 120.5(2) . . ?
C11 C12 C13 121.4(3) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C14 C13 C12 119.9(3) . . ?
C14 C13 H13A 120.1 . . ?
C12 C13 H13A 120.1 . . ?
C15 C14 C13 119.5(3) . . ?
C15 C14 H14A 120.3 . . ?
C13 C14 H14A 120.3 . . ?
C14 C15 C16 120.7(3) . . ?
C14 C15 H15A 119.7 . . ?
C16 C15 H15A 119.7 . . ?
C15 C16 C11 120.8(3) . . ?
C15 C16 H16A 119.6 . . ?
C11 C16 H16A 119.6 . . ?
C4 P1 C5 106.60(13) . . ?
C4 P1 C11 101.20(13) . . ?
C5 P1 C11 99.48(13) . . ?
C4 P1 Mo1 114.51(9) . . ?
C5 P1 Mo1 113.99(9) . . ?
C11 P1 Mo1 119.09(9) . . ?
B1 C17 P2 115.83(19) . . ?
B1 C17 H17A 108.3 . . ?
P2 C17 H17A 108.3 . . ?
B1 C17 H17B 108.3 . . ?
P2 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C23 C18 C19 117.8(3) . . ?
C23 C18 P2 122.7(3) . . ?
C19 C18 P2 119.5(3) . . ?
C18 C19 C20 120.2(4) . . ?
C18 C19 H19A 119.9 . . ?
C20 C19 H19A 119.9 . . ?
C21 C20 C19 121.4(4) . . ?
C21 C20 H20A 119.3 . . ?
C19 C20 H20A 119.3 . . ?
C22 C21 C20 119.1(4) . . ?
C22 C21 H21A 120.4 . . ?
C20 C21 H21A 120.4 . . ?
C21 C22 C23 120.8(4) . . ?
C21 C22 H22A 119.6 . . ?
C23 C22 H22A 119.6 . . ?
C18 C23 C22 120.6(4) . . ?
C18 C23 H23A 119.7 . . ?
C22 C23 H23A 119.7 . . ?
C25 C24 C29 118.7(3) . . ?
C25 C24 P2 118.6(2) . . ?
C29 C24 P2 122.6(2) . . ?
C24 C25 C26 120.5(3) . . ?
C24 C25 H25A 119.8 . . ?
C26 C25 H25A 119.8 . . ?
C27 C26 C25 120.8(3) . . ?
C27 C26 H26A 119.6 . . ?
C25 C26 H26A 119.6 . . ?
C26 C27 C28 119.1(3) . . ?
C26 C27 H27A 120.5 . . ?
C28 C27 H27A 120.5 . . ?
C17 P2 C24 105.12(13) . . ?
C17 P2 C18 104.81(14) . . ?
C24 P2 C18 99.65(13) . . ?
C17 P2 Mo1 112.02(10) . . ?
C24 P2 Mo1 116.79(10) . . ?
C18 P2 Mo1 116.86(10) . . ?
C29 C28 C27 120.6(3) . . ?
C29 C28 H28A 119.7 . . ?
C27 C28 H28A 119.7 . . ?
C28 C29 C24 120.3(3) . . ?
C28 C29 H29A 119.8 . . ?
C24 C29 H29A 119.8 . . ?
B1 C30 P3 113.93(18) . . ?
B1 C30 H30A 108.8 . . ?
P3 C30 H30A 108.8 . . ?
B1 C30 H30B 108.8 . . ?
P3 C30 H30B 108.8 . . ?
H30A C30 H30B 107.7 . . ?
C32 C31 C36 118.4(3) . . ?
C32 C31 P3 121.8(2) . . ?
C36 C31 P3 119.8(2) . . ?
C31 C32 C33 120.9(3) . . ?
C31 C32 H32A 119.5 . . ?
C33 C32 H32A 119.5 . . ?
C34 C33 C32 120.2(3) . . ?
C34 C33 H33A 119.9 . . ?
C32 C33 H33A 119.9 . . ?
C35 C34 C33 119.7(3) . . ?
C35 C34 H34A 120.2 . . ?
C33 C34 H34A 120.2 . . ?
C34 C35 C36 120.2(3) . . ?
C34 C35 H35A 119.9 . . ?
C36 C35 H35A 119.9 . . ?
C35 C36 C31 120.6(3) . . ?
C35 C36 H36A 119.7 . . ?
C31 C36 H36A 119.7 . . ?
C42 C37 C38 118.1(3) . . ?
C42 C37 P3 124.1(2) . . ?
C38 C37 P3 117.6(2) . . ?
C39 C38 C37 120.7(3) . . ?
C39 C38 H38A 119.6 . . ?
C37 C38 H38A 119.6 . . ?
C40 C39 C38 120.4(3) . . ?
C40 C39 H39A 119.8 . . ?
C38 C39 H39A 119.8 . . ?
C39 C40 C41 120.1(3) . . ?
C39 C40 H40A 120.0 . . ?
C41 C40 H40A 120.0 . . ?
C40 C41 C42 120.4(3) . . ?
C40 C41 H41A 119.8 . . ?
C42 C41 H41A 119.8 . . ?
C37 C42 C41 120.3(3) . . ?
C37 C42 H42A 119.9 . . ?
C41 C42 H42A 119.9 . . ?
C30 P3 C37 106.51(13) . . ?
C30 P3 C31 102.07(13) . . ?
C37 P3 C31 99.89(12) . . ?
C30 P3 Mo1 113.85(9) . . ?
C37 P3 Mo1 114.37(9) . . ?
C31 P3 Mo1 118.38(9) . . ?
C43 B1 C4 110.2(2) . . ?
C43 B1 C17 107.4(2) . . ?
C4 B1 C17 111.0(2) . . ?
C43 B1 C30 104.7(2) . . ?
C4 B1 C30 111.6(2) . . ?
C17 B1 C30 111.7(2) . . ?
C44 C43 C48 114.4(3) . . ?
C44 C43 B1 121.2(2) . . ?
C48 C43 B1 124.3(2) . . ?
C44 C43 Cr1 70.11(17) . . ?
C48 C43 Cr1 68.41(16) . . ?
B1 C43 Cr1 133.22(18) . . ?
C43 C44 C45 123.0(3) . . ?
C43 C44 Cr1 73.48(17) . . ?
C45 C44 Cr1 71.91(19) . . ?
C43 C44 H44A 118.5 . . ?
C45 C44 H44A 118.5 . . ?
Cr1 C44 H44A 128.6 . . ?
C46 C45 C44 120.4(3) . . ?
C46 C45 Cr1 71.37(19) . . ?
C44 C45 Cr1 71.18(18) . . ?
C46 C45 H45A 119.8 . . ?
C44 C45 H45A 119.8 . . ?
Cr1 C45 H45A 130.2 . . ?
C45 C46 C47 119.0(3) . . ?
C45 C46 Cr1 72.77(19) . . ?
C47 C46 Cr1 70.74(18) . . ?
C45 C46 H46A 120.5 . . ?
C47 C46 H46A 120.5 . . ?
Cr1 C46 H46A 128.1 . . ?
C48 C47 C46 119.7(3) . . ?
C48 C47 Cr1 71.05(17) . . ?
C46 C47 Cr1 72.25(18) . . ?
C48 C47 H47A 120.1 . . ?
C46 C47 H47A 120.1 . . ?
Cr1 C47 H47A 128.8 . . ?
C47 C48 C43 123.4(3) . . ?
C47 C48 Cr1 71.82(18) . . ?
C43 C48 Cr1 74.63(17) . . ?
C47 C48 H48A 118.3 . . ?
C43 C48 H48A 118.3 . . ?
Cr1 C48 H48A 127.5 . . ?
C49 Cr1 C51 88.92(19) . . ?
C49 Cr1 C50 86.85(17) . . ?
C51 Cr1 C50 87.04(19) . . ?
C49 Cr1 C48 125.41(16) . . ?
C51 Cr1 C48 144.65(15) . . ?
C50 Cr1 C48 86.84(14) . . ?
C49 Cr1 C47 95.50(15) . . ?
C51 Cr1 C47 164.53(17) . . ?
C50 Cr1 C47 107.96(15) . . ?
C48 Cr1 C47 37.13(11) . . ?
C49 Cr1 C46 89.49(15) . . ?
C51 Cr1 C46 128.55(17) . . ?
C50 Cr1 C46 144.16(15) . . ?
C48 Cr1 C46 66.63(11) . . ?
C47 Cr1 C46 37.01(11) . . ?
C49 Cr1 C44 147.86(15) . . ?
C51 Cr1 C44 90.98(17) . . ?
C50 Cr1 C44 125.24(14) . . ?
C48 Cr1 C44 64.94(12) . . ?
C47 Cr1 C44 77.40(12) . . ?
C46 Cr1 C44 65.85(11) . . ?
C49 Cr1 C45 111.60(15) . . ?
C51 Cr1 C45 99.36(17) . . ?
C50 Cr1 C45 160.41(14) . . ?
C48 Cr1 C45 77.21(12) . . ?
C47 Cr1 C45 65.23(13) . . ?
C46 Cr1 C45 35.87(12) . . ?
C44 Cr1 C45 36.91(11) . . ?
C49 Cr1 C43 162.11(15) . . ?
C51 Cr1 C43 108.97(15) . . ?
C50 Cr1 C43 93.74(13) . . ?
C48 Cr1 C43 36.96(10) . . ?
C47 Cr1 C43 67.28(11) . . ?
C46 Cr1 C43 79.57(11) . . ?
C44 Cr1 C43 36.41(10) . . ?
C45 Cr1 C43 66.68(11) . . ?
O4 C49 Cr1 177.9(4) . . ?
O5 C50 Cr1 178.6(4) . . ?
O6 C51 Cr1 177.6(5) . . ?
C56 N1 C58 111.1(3) . . ?
C56 N1 C52 110.6(3) . . ?
C58 N1 C52 110.0(3) . . ?
C56 N1 C54 110.9(3) . . ?
C58 N1 C54 106.8(3) . . ?
C52 N1 C54 107.3(3) . . ?
C53 C52 N1 117.0(4) . . ?
C53 C52 H52A 108.0 . . ?
N1 C52 H52A 108.0 . . ?
C53 C52 H52B 108.0 . . ?
N1 C52 H52B 108.0 . . ?
H52A C52 H52B 107.3 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C55 C54 N1 115.7(4) . . ?
C55 C54 H54A 108.3 . . ?
N1 C54 H54A 108.3 . . ?
C55 C54 H54B 108.3 . . ?
N1 C54 H54B 108.3 . . ?
H54A C54 H54B 107.4 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C57 C56 N1 119.7(5) . . ?
C57 C56 H56A 107.4 . . ?
N1 C56 H56A 107.4 . . ?
C57 C56 H56B 107.4 . . ?
N1 C56 H56B 107.4 . . ?
H56A C56 H56B 106.9 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C59 C58 N1 119.4(4) . . ?
C59 C58 H58A 107.5 . . ?
N1 C58 H58A 107.5 . . ?
C59 C58 H58B 107.5 . . ?
N1 C58 H58B 107.5 . . ?
H58A C58 H58B 107.0 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?

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
C10 C5 C6 C7 -0.8(5) . . . . ?
P1 C5 C6 C7 177.6(3) . . . . ?
C5 C6 C7 C8 -1.9(5) . . . . ?
C6 C7 C8 C9 2.3(5) . . . . ?
C7 C8 C9 C10 -0.2(6) . . . . ?
C6 C5 C10 C9 3.0(5) . . . . ?
P1 C5 C10 C9 -175.3(3) . . . . ?
C8 C9 C10 C5 -2.5(5) . . . . ?
C16 C11 C12 C13 3.7(4) . . . . ?
P1 C11 C12 C13 -172.1(2) . . . . ?
C11 C12 C13 C14 -2.3(4) . . . . ?
C12 C13 C14 C15 0.0(5) . . . . ?
C13 C14 C15 C16 0.7(5) . . . . ?
C14 C15 C16 C11 0.9(6) . . . . ?
C12 C11 C16 C15 -3.0(5) . . . . ?
P1 C11 C16 C15 172.8(3) . . . . ?
B1 C4 P1 C5 156.8(2) . . . . ?
B1 C4 P1 C11 -99.6(2) . . . . ?
B1 C4 P1 Mo1 29.8(2) . . . . ?
C10 C5 P1 C4 -0.7(3) . . . . ?
C6 C5 P1 C4 -179.0(2) . . . . ?
C10 C5 P1 C11 -105.4(3) . . . . ?
C6 C5 P1 C11 76.3(3) . . . . ?
C10 C5 P1 Mo1 126.7(3) . . . . ?
C6 C5 P1 Mo1 -51.6(3) . . . . ?
C12 C11 P1 C4 106.8(2) . . . . ?
C16 C11 P1 C4 -68.9(3) . . . . ?
C12 C11 P1 C5 -144.1(2) . . . . ?
C16 C11 P1 C5 40.3(3) . . . . ?
C12 C11 P1 Mo1 -19.7(3) . . . . ?
C16 C11 P1 Mo1 164.7(2) . . . . ?
C23 C18 C19 C20 0.7(6) . . . . ?
P2 C18 C19 C20 -178.6(3) . . . . ?
C18 C19 C20 C21 -0.9(7) . . . . ?
C19 C20 C21 C22 0.5(7) . . . . ?
C20 C21 C22 C23 0.0(7) . . . . ?
C19 C18 C23 C22 -0.2(6) . . . . ?
P2 C18 C23 C22 179.0(3) . . . . ?
C21 C22 C23 C18 -0.1(7) . . . . ?
C29 C24 C25 C26 0.9(5) . . . . ?
P2 C24 C25 C26 177.7(2) . . . . ?
C24 C25 C26 C27 -2.9(5) . . . . ?
C25 C26 C27 C28 2.2(5) . . . . ?
B1 C17 P2 C24 166.3(2) . . . . ?
B1 C17 P2 C18 -89.1(2) . . . . ?
B1 C17 P2 Mo1 38.5(2) . . . . ?
C25 C24 P2 C17 -162.3(2) . . . . ?
C29 C24 P2 C17 14.4(3) . . . . ?
C25 C24 P2 C18 89.4(3) . . . . ?
C29 C24 P2 C18 -93.9(3) . . . . ?
C25 C24 P2 Mo1 -37.4(3) . . . . ?
C29 C24 P2 Mo1 139.3(2) . . . . ?
C23 C18 P2 C17 -21.0(3) . . . . ?
C19 C18 P2 C17 158.2(3) . . . . ?
C23 C18 P2 C24 87.6(3) . . . . ?
C19 C18 P2 C24 -93.2(3) . . . . ?
C23 C18 P2 Mo1 -145.7(3) . . . . ?
C19 C18 P2 Mo1 33.6(3) . . . . ?
C26 C27 C28 C29 0.5(6) . . . . ?
C27 C28 C29 C24 -2.5(6) . . . . ?
C25 C24 C29 C28 1.8(5) . . . . ?
P2 C24 C29 C28 -174.9(3) . . . . ?
C36 C31 C32 C33 0.8(4) . . . . ?
P3 C31 C32 C33 -176.3(2) . . . . ?
C31 C32 C33 C34 -0.7(5) . . . . ?
C32 C33 C34 C35 0.7(5) . . . . ?
C33 C34 C35 C36 -0.8(5) . . . . ?
C34 C35 C36 C31 0.9(5) . . . . ?
C32 C31 C36 C35 -0.9(5) . . . . ?
P3 C31 C36 C35 176.3(3) . . . . ?
C42 C37 C38 C39 -0.8(4) . . . . ?
P3 C37 C38 C39 175.5(2) . . . . ?
C37 C38 C39 C40 -0.1(4) . . . . ?
C38 C39 C40 C41 1.1(5) . . . . ?
C39 C40 C41 C42 -1.1(5) . . . . ?
C38 C37 C42 C41 0.8(4) . . . . ?
P3 C37 C42 C41 -175.2(2) . . . . ?
C40 C41 C42 C37 0.1(5) . . . . ?
B1 C30 P3 C37 163.45(19) . . . . ?
B1 C30 P3 C31 -92.3(2) . . . . ?
B1 C30 P3 Mo1 36.5(2) . . . . ?
C42 C37 P3 C30 9.8(3) . . . . ?
C38 C37 P3 C30 -166.3(2) . . . . ?
C42 C37 P3 C31 -96.0(3) . . . . ?
C38 C37 P3 C31 87.9(2) . . . . ?
C42 C37 P3 Mo1 136.5(2) . . . . ?
C38 C37 P3 Mo1 -39.6(2) . . . . ?
C32 C31 P3 C30 123.2(2) . . . . ?
C36 C31 P3 C30 -53.9(3) . . . . ?
C32 C31 P3 C37 -127.4(2) . . . . ?
C36 C31 P3 C37 55.5(3) . . . . ?
C32 C31 P3 Mo1 -2.7(3) . . . . ?
C36 C31 P3 Mo1 -179.7(2) . . . . ?
P1 C4 B1 C43 160.85(19) . . . . ?
P1 C4 B1 C17 -80.3(3) . . . . ?
P1 C4 B1 C30 45.0(3) . . . . ?
P2 C17 B1 C43 159.64(18) . . . . ?
P2 C17 B1 C4 39.1(3) . . . . ?
P2 C17 B1 C30 -86.1(2) . . . . ?
P3 C30 B1 C43 154.90(19) . . . . ?
P3 C30 B1 C4 -85.9(2) . . . . ?
P3 C30 B1 C17 39.0(3) . . . . ?
C4 B1 C43 C44 150.6(3) . . . . ?
C17 B1 C43 C44 29.6(3) . . . . ?
C30 B1 C43 C44 -89.3(3) . . . . ?
C4 B1 C43 C48 -32.5(4) . . . . ?
C17 B1 C43 C48 -153.5(3) . . . . ?
C30 B1 C43 C48 87.6(3) . . . . ?
C4 B1 C43 Cr1 59.2(3) . . . . ?
C17 B1 C43 Cr1 -61.8(3) . . . . ?
C30 B1 C43 Cr1 179.4(2) . . . . ?
C48 C43 C44 C45 -1.0(5) . . . . ?
B1 C43 C44 C45 176.1(3) . . . . ?
Cr1 C43 C44 C45 -54.6(3) . . . . ?
C48 C43 C44 Cr1 53.6(2) . . . . ?
B1 C43 C44 Cr1 -129.2(2) . . . . ?
C43 C44 C45 C46 1.6(5) . . . . ?
Cr1 C44 C45 C46 -53.8(3) . . . . ?
C43 C44 C45 Cr1 55.3(3) . . . . ?
C44 C45 C46 C47 -1.8(5) . . . . ?
Cr1 C45 C46 C47 -55.4(3) . . . . ?
C44 C45 C46 Cr1 53.7(3) . . . . ?
C45 C46 C47 C48 1.6(5) . . . . ?
Cr1 C46 C47 C48 -54.9(3) . . . . ?
C45 C46 C47 Cr1 56.4(3) . . . . ?
C46 C47 C48 C43 -1.1(5) . . . . ?
Cr1 C47 C48 C43 -56.6(3) . . . . ?
C46 C47 C48 Cr1 55.4(3) . . . . ?
C44 C43 C48 C47 0.8(4) . . . . ?
B1 C43 C48 C47 -176.2(3) . . . . ?
Cr1 C43 C48 C47 55.3(3) . . . . ?
C44 C43 C48 Cr1 -54.5(2) . . . . ?
B1 C43 C48 Cr1 128.4(3) . . . . ?
C56 N1 C52 C53 176.6(4) . . . . ?
C58 N1 C52 C53 53.5(5) . . . . ?
C54 N1 C52 C53 -62.3(5) . . . . ?
C56 N1 C54 C55 -54.9(6) . . . . ?
C58 N1 C54 C55 66.3(6) . . . . ?
C52 N1 C54 C55 -175.8(4) . . . . ?
C58 N1 C56 C57 179.1(4) . . . . ?
C52 N1 C56 C57 56.7(6) . . . . ?
C54 N1 C56 C57 -62.3(6) . . . . ?
C56 N1 C58 C59 -70.8(6) . . . . ?
C52 N1 C58 C59 52.0(6) . . . . ?
C54 N1 C58 C59 168.1(5) . . . . ?

_refine_diff_density_max         1.068
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.082

_shelxl_version_number           2014-3

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.030 0.000 0.000 403 93 ' '
2 0.010 0.500 0.500 403 93 ' '
_platon_squeeze_details          
;

 PLATON/SQUEEZE applied to treat apparent THF/DEE compositional disorder
 PLATON/SQUEEZE RESULTS Summary and Remarks :N = NOTE, W = WARNING, E = ERROR
 ============================================================================

 N: No S.U.'s (esd) on observed/calculated parameters.
 ---------------------------------------------------------------------------
 N: Number of moved primary input atoms: ................................ 104
 N: Total Potential Solvent Accessible Void Vol ..............   811.5 Ang^3
 N: Electron Count / Cell = 186 - To be included in D(calc), F000 & Mol.Wght.

 ============================================================================

 empirical formula assumes 100% THF
 
;
# start Validation Reply Form

_vrf_DENSX01_14167aaa            
;
PROBLEM: The ratio of the calculated to measured crystal density
RESPONSE: ... PLATON/SQUEEZE treatment of disordered THF.
;
_vrf_CHEMW03_14167aaa            
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: ... PLATON/SQUEEZE treatment of disordered THF.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Et2O'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_14169d
_database_code_depnum_ccdc_archive 'CCDC 1039156'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        '[Et4N][W(CO)3{6-(PhBP3)W(CO)3}]'
_chemical_name_common            14169d
_chemical_melting_point          553
_chemical_formula_moiety         '2(C51 H41 B Cr O6 P3 W), 2(C8 H20 N)'
_chemical_formula_sum            'C118 H122 B2 Cr2 N2 O12 P6 W2'
_chemical_formula_weight         2439.31

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'
N N 0.0061 0.0033 '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'
Cr Cr 0.3209 0.6236 '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           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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, y+1/2, -z'

_cell_length_a                   14.1281(19)
_cell_length_b                   23.778(3)
_cell_length_c                   17.324(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.660(2)
_cell_angle_gamma                90
_cell_volume                     5819.4(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2967
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.35

_exptl_crystal_description       Plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_F_000             2472
_exptl_transmission_factor_min   0.2777
_exptl_transmission_factor_max   0.3334
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    2.292
_shelx_estimated_absorpt_T_min   0.501
_shelx_estimated_absorpt_T_max   0.598
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2777
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2012)'

_exptl_special_details           'Prof. P. Fischer'

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            67782
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.454
_diffrn_reflns_theta_max         27.413
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             26263
_reflns_number_gt                24123
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_max     0.987
_reflns_Friedel_fraction_full    0.999

_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0470P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 10829 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         26263
_refine_ls_number_parameters     1305
_refine_ls_number_restraints     1359
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.0853
_refine_ls_wR_factor_gt          0.0834
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.002
_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
W1A W 0.60405(2) 0.25963(2) 0.78320(2) 0.02714(6) Uani 1 1 d . U . . .
Cr1A Cr 0.66342(6) 0.08676(4) 1.12712(5) 0.02174(19) Uani 1 1 d . U . . .
P1A P 0.75047(11) 0.16611(7) 1.08302(9) 0.0258(3) Uani 1 1 d . U . . .
P2A P 0.70164(11) 0.04288(7) 1.00498(9) 0.0246(3) Uani 1 1 d . U . . .
P3A P 0.52957(11) 0.12587(7) 1.05757(9) 0.0246(3) Uani 1 1 d . U . . .
O1A O 0.8286(4) 0.0400(2) 1.2154(3) 0.0494(13) Uani 1 1 d . U . . .
O2A O 0.5627(4) -0.0085(3) 1.2025(3) 0.0537(15) Uani 1 1 d . U . . .
O3A O 0.6237(4) 0.1381(3) 1.2807(3) 0.0508(14) Uani 1 1 d . U . . .
O4A O 0.6618(5) 0.3485(3) 0.9070(4) 0.0661(17) Uani 1 1 d . U . . .
O5A O 0.5597(5) 0.3568(3) 0.6694(4) 0.0657(18) Uani 1 1 d . U . . .
O6A O 0.3986(4) 0.2664(3) 0.8411(5) 0.090(3) Uani 1 1 d . U . . .
C1A C 0.7683(5) 0.0584(3) 1.1776(4) 0.0313(13) Uani 1 1 d . U . . .
C2A C 0.5993(5) 0.0278(3) 1.1677(4) 0.0340(14) Uani 1 1 d . U . . .
C3A C 0.6364(5) 0.1209(3) 1.2184(4) 0.0328(14) Uani 1 1 d . U . . .
C4A C 0.7571(4) 0.1720(3) 0.9776(3) 0.0277(12) Uani 1 1 d . U . . .
H4AA H 0.7698 0.2116 0.9638 0.033 Uiso 1 1 calc R U . . .
H4AB H 0.8109 0.1491 0.9594 0.033 Uiso 1 1 calc R U . . .
C5A C 0.7176(5) 0.2384(3) 1.1100(4) 0.0364(14) Uani 1 1 d . U . . .
C6A C 0.6413(5) 0.2500(3) 1.1543(4) 0.0468(17) Uani 1 1 d . U . . .
H6AA H 0.6042 0.2200 1.1737 0.056 Uiso 1 1 calc R U . . .
C7A C 0.6166(7) 0.3045(4) 1.1715(6) 0.062(2) Uani 1 1 d . U . . .
H7AA H 0.5618 0.3120 1.2010 0.075 Uiso 1 1 calc R U . . .
C8A C 0.6717(7) 0.3478(4) 1.1459(6) 0.066(2) Uani 1 1 d . U . . .
H8AA H 0.6556 0.3855 1.1583 0.080 Uiso 1 1 calc R U . . .
C9A C 0.7505(7) 0.3368(4) 1.1020(6) 0.061(2) Uani 1 1 d . U . . .
H9AA H 0.7882 0.3670 1.0838 0.073 Uiso 1 1 calc R U . . .
C10A C 0.7745(6) 0.2826(3) 1.0846(5) 0.0465(17) Uani 1 1 d . U . . .
H10A H 0.8296 0.2750 1.0555 0.056 Uiso 1 1 calc R U . . .
C11A C 0.8731(5) 0.1654(3) 1.1197(3) 0.0300(13) Uani 1 1 d . U . . .
C12A C 0.8919(5) 0.1837(3) 1.1942(4) 0.0413(16) Uani 1 1 d . U . . .
H12A H 0.8423 0.1997 1.2236 0.050 Uiso 1 1 calc R U . . .
C13A C 0.9823(5) 0.1790(3) 1.2269(5) 0.0470(18) Uani 1 1 d . U . . .
H13A H 0.9930 0.1909 1.2786 0.056 Uiso 1 1 calc R U . . .
C14A C 1.0552(5) 0.1578(3) 1.1855(5) 0.0474(17) Uani 1 1 d . U . . .
H14A H 1.1169 0.1556 1.2076 0.057 Uiso 1 1 calc R U . . .
C15A C 1.0389(6) 0.1395(3) 1.1116(5) 0.0478(18) Uani 1 1 d . U . . .
H15A H 1.0899 0.1253 1.0822 0.057 Uiso 1 1 calc R U . . .
C16A C 0.9473(5) 0.1416(3) 1.0786(4) 0.0364(15) Uani 1 1 d . U . . .
H16A H 0.9361 0.1269 1.0283 0.044 Uiso 1 1 calc R U . . .
C17A C 0.6558(4) 0.0814(3) 0.9217(3) 0.0262(12) Uani 1 1 d . U . . .
H17A H 0.6931 0.0710 0.8758 0.031 Uiso 1 1 calc R U . . .
H17B H 0.5894 0.0698 0.9119 0.031 Uiso 1 1 calc R U . . .
C18A C 0.8274(4) 0.0307(3) 0.9799(4) 0.0291(13) Uani 1 1 d . U . . .
C19A C 0.8836(5) -0.0024(3) 1.0314(4) 0.0433(17) Uani 1 1 d . U . . .
H19A H 0.8583 -0.0151 1.0788 0.052 Uiso 1 1 calc R U . . .
C20A C 0.9749(6) -0.0158(4) 1.0118(5) 0.056(2) Uani 1 1 d . U . . .
H20A H 1.0119 -0.0385 1.0457 0.067 Uiso 1 1 calc R U . . .
C21A C 1.0138(5) 0.0030(4) 0.9441(5) 0.056(2) Uani 1 1 d . U . . .
H21A H 1.0779 -0.0053 0.9326 0.068 Uiso 1 1 calc R U . . .
C22A C 0.9596(6) 0.0341(3) 0.8931(5) 0.0495(19) Uani 1 1 d . U . . .
H22A H 0.9852 0.0465 0.8456 0.059 Uiso 1 1 calc R U . . .
C23A C 0.8668(5) 0.0468(3) 0.9121(4) 0.0380(15) Uani 1 1 d . U . . .
H23A H 0.8293 0.0676 0.8763 0.046 Uiso 1 1 calc R U . . .
C24A C 0.6599(4) -0.0299(3) 0.9920(4) 0.0325(14) Uani 1 1 d . U . . .
C25A C 0.6649(6) -0.0668(3) 1.0537(5) 0.0471(18) Uani 1 1 d . U . . .
H25A H 0.6949 -0.0555 1.1005 0.057 Uiso 1 1 calc R U . . .
C26A C 0.6266(7) -0.1198(4) 1.0476(7) 0.069(2) Uani 1 1 d . U . . .
H26A H 0.6319 -0.1452 1.0897 0.083 Uiso 1 1 calc R U . . .
C27A C 0.5806(7) -0.1362(4) 0.9808(7) 0.071(3) Uani 1 1 d . U . . .
H27A H 0.5509 -0.1720 0.9783 0.086 Uiso 1 1 calc R U . . .
C28A C 0.5775(6) -0.1012(3) 0.9178(7) 0.063(2) Uani 1 1 d . U . . .
H28A H 0.5493 -0.1133 0.8706 0.075 Uiso 1 1 calc R U . . .
C29A C 0.6166(5) -0.0474(3) 0.9244(5) 0.0444(17) Uani 1 1 d . U . . .
H29A H 0.6133 -0.0224 0.8817 0.053 Uiso 1 1 calc R U . . .
C30A C 0.5632(4) 0.1717(3) 0.9774(3) 0.0266(12) Uani 1 1 d . U . . .
H30A H 0.5102 0.1732 0.9397 0.032 Uiso 1 1 calc R U . . .
H30B H 0.5735 0.2102 0.9975 0.032 Uiso 1 1 calc R U . . .
C31A C 0.4404(4) 0.0779(3) 1.0132(3) 0.0266(12) Uani 1 1 d . U . . .
C32A C 0.4437(4) 0.0198(3) 1.0246(4) 0.0298(13) Uani 1 1 d . U . . .
H32A H 0.4934 0.0040 1.0550 0.036 Uiso 1 1 calc R U . . .
C33A C 0.3751(5) -0.0154(3) 0.9920(4) 0.0345(14) Uani 1 1 d . U . . .
H33A H 0.3784 -0.0548 1.0002 0.041 Uiso 1 1 calc R U . . .
C34A C 0.3027(5) 0.0069(3) 0.9480(4) 0.0355(14) Uani 1 1 d . U . . .
H34A H 0.2560 -0.0170 0.9257 0.043 Uiso 1 1 calc R U . . .
C35A C 0.2984(5) 0.0654(3) 0.9364(4) 0.0363(15) Uani 1 1 d . U . . .
H35A H 0.2487 0.0810 0.9059 0.044 Uiso 1 1 calc R U . . .
C36A C 0.3656(5) 0.1001(3) 0.9689(4) 0.0331(14) Uani 1 1 d . U . . .
H36A H 0.3614 0.1396 0.9613 0.040 Uiso 1 1 calc R U . . .
C37A C 0.4445(4) 0.1654(3) 1.1148(4) 0.0283(12) Uani 1 1 d . U . . .
C38A C 0.4115(5) 0.1406(3) 1.1835(4) 0.0387(15) Uani 1 1 d . U . . .
H38A H 0.4367 0.1054 1.1996 0.046 Uiso 1 1 calc R U . . .
C39A C 0.3432(6) 0.1664(4) 1.2282(5) 0.0519(19) Uani 1 1 d . U . . .
H39A H 0.3207 0.1490 1.2739 0.062 Uiso 1 1 calc R U . . .
C40A C 0.3081(6) 0.2190(4) 1.2040(5) 0.056(2) Uani 1 1 d . U . . .
H40A H 0.2636 0.2383 1.2351 0.067 Uiso 1 1 calc R U . . .
C41A C 0.3370(6) 0.2429(4) 1.1366(6) 0.065(2) Uani 1 1 d . U . . .
H41A H 0.3110 0.2779 1.1203 0.078 Uiso 1 1 calc R U . . .
C42A C 0.4054(6) 0.2158(3) 1.0910(5) 0.052(2) Uani 1 1 d . U . . .
H42A H 0.4247 0.2324 1.0438 0.062 Uiso 1 1 calc R U . . .
C43A C 0.6612(4) 0.1745(3) 0.8432(3) 0.0277(12) Uani 1 1 d . U . . .
C44A C 0.7390(5) 0.2050(3) 0.8117(4) 0.0316(13) Uani 1 1 d . U . . .
H44A H 0.7898 0.2153 0.8452 0.038 Uiso 1 1 calc R U . . .
C45A C 0.7438(5) 0.2207(3) 0.7329(4) 0.0371(15) Uani 1 1 d . U . . .
H45A H 0.7973 0.2402 0.7137 0.044 Uiso 1 1 calc R U . . .
C46A C 0.6664(5) 0.2066(3) 0.6831(4) 0.0384(15) Uani 1 1 d . U . . .
H46A H 0.6677 0.2176 0.6304 0.046 Uiso 1 1 calc R U . . .
C47A C 0.5883(5) 0.1766(3) 0.7108(4) 0.0337(14) Uani 1 1 d . U . . .
H47A H 0.5381 0.1658 0.6771 0.040 Uiso 1 1 calc R U . . .
C48A C 0.5860(4) 0.1626(3) 0.7913(3) 0.0271(12) Uani 1 1 d . U . . .
H48A H 0.5312 0.1445 0.8107 0.033 Uiso 1 1 calc R U . . .
C49A C 0.6400(5) 0.3152(3) 0.8615(4) 0.0404(16) Uani 1 1 d . U . . .
C50A C 0.5771(5) 0.3205(3) 0.7127(4) 0.0410(17) Uani 1 1 d . U . . .
C51A C 0.4751(4) 0.2656(3) 0.8191(5) 0.0477(18) Uani 1 1 d . U . . .
B1A B 0.6594(5) 0.1511(3) 0.9325(4) 0.0257(13) Uani 1 1 d . U . . .
W1B W 0.07028(2) 0.27141(2) 0.83569(2) 0.03320(7) Uani 1 1 d . U . . .
Cr1B Cr 0.15143(7) 0.07628(4) 0.51985(5) 0.0251(2) Uani 1 1 d . U . . .
P1B P 0.00947(10) 0.11415(6) 0.57543(9) 0.0237(3) Uani 1 1 d . U . . .
P2B P 0.21741(11) 0.16656(7) 0.55577(9) 0.0275(3) Uani 1 1 d . U . . .
P3B P 0.19401(11) 0.04401(7) 0.64612(9) 0.0260(3) Uani 1 1 d . U . . .
O1B O 0.1175(4) 0.1092(2) 0.3555(3) 0.0476(13) Uani 1 1 d . U . . .
O2B O 0.3234(4) 0.0209(4) 0.4562(4) 0.081(2) Uani 1 1 d . U . . .
O3B O 0.0613(4) -0.0311(2) 0.4684(3) 0.0553(15) Uani 1 1 d . U . . .
O4B O 0.1935(5) 0.3764(3) 0.7966(4) 0.074(2) Uani 1 1 d . U . . .
O5B O -0.0716(5) 0.3490(3) 0.9206(4) 0.0705(19) Uani 1 1 d . U . . .
O6B O -0.0515(4) 0.2976(2) 0.6903(3) 0.0487(13) Uani 1 1 d . U . . .
C1B C 0.1267(5) 0.0995(3) 0.4206(4) 0.0344(14) Uani 1 1 d . U . . .
C2B C 0.2578(5) 0.0438(4) 0.4837(4) 0.0452(18) Uani 1 1 d . U . . .
C3B C 0.0942(5) 0.0107(3) 0.4923(4) 0.0374(15) Uani 1 1 d . U . . .
C4B C 0.0286(4) 0.1627(3) 0.6555(3) 0.0259(12) Uani 1 1 d . U . . .
H4BA H 0.0292 0.2016 0.6351 0.031 Uiso 1 1 calc R U . . .
H4BB H -0.0253 0.1596 0.6912 0.031 Uiso 1 1 calc R U . . .
C5B C -0.0805(4) 0.0666(3) 0.6178(4) 0.0273(12) Uani 1 1 d . U . . .
C6B C -0.0656(5) 0.0083(3) 0.6238(4) 0.0365(15) Uani 1 1 d . U . . .
H6BA H -0.0097 -0.0081 0.6036 0.044 Uiso 1 1 calc R U . . .
C7B C -0.1339(5) -0.0258(3) 0.6598(5) 0.0448(17) Uani 1 1 d . U . . .
H7BA H -0.1234 -0.0651 0.6650 0.054 Uiso 1 1 calc R U . . .
C8B C -0.2156(5) -0.0022(3) 0.6874(5) 0.0477(18) Uani 1 1 d . U . . .
H8BA H -0.2623 -0.0251 0.7107 0.057 Uiso 1 1 calc R U . . .
C9B C -0.2294(5) 0.0557(3) 0.6809(5) 0.0429(17) Uani 1 1 d . U . . .
H9BA H -0.2852 0.0721 0.7012 0.051 Uiso 1 1 calc R U . . .
C10B C -0.1633(5) 0.0899(3) 0.6455(4) 0.0367(15) Uani 1 1 d . U . . .
H10B H -0.1747 0.1291 0.6402 0.044 Uiso 1 1 calc R U . . .
C11B C -0.0698(4) 0.15131(19) 0.5075(3) 0.0290(12) Uani 1 1 d D U . . .
C12B C -0.0950(4) 0.1239(3) 0.4399(3) 0.0372(14) Uani 1 1 d D U . . .
H12B H -0.0676 0.0885 0.4279 0.045 Uiso 1 1 calc R U . . .
C13B C -0.1612(4) 0.1485(3) 0.3891(4) 0.0484(17) Uani 1 1 d D U . . .
H13B H -0.1795 0.1304 0.3424 0.058 Uiso 1 1 calc R U . . .
C14B C -0.1970(4) 0.1978(3) 0.4087(4) 0.063(2) Uani 1 1 d D U . . .
H14B H -0.2418 0.2142 0.3741 0.075 Uiso 1 1 calc R U . . .
C15B C -0.1763(4) 0.2264(3) 0.4722(4) 0.0499(17) Uani 1 1 d D U . . .
H15B H -0.2050 0.2617 0.4823 0.060 Uiso 1 1 calc R U . . .
C16B C -0.1102(4) 0.2028(2) 0.5241(4) 0.0397(15) Uani 1 1 d D U . . .
H16B H -0.0935 0.2221 0.5703 0.048 Uiso 1 1 calc R U . . .
C17B C 0.2213(4) 0.1776(3) 0.6597(3) 0.0249(12) Uani 1 1 d . U . . .
H17C H 0.2792 0.1598 0.6811 0.030 Uiso 1 1 calc R U . . .
H17D H 0.2254 0.2185 0.6702 0.030 Uiso 1 1 calc R U . . .
C18B C 0.1582(5) 0.2309(3) 0.5177(4) 0.0367(14) Uani 1 1 d . U . . .
C19B C 0.1469(7) 0.2349(4) 0.4362(5) 0.059(2) Uani 1 1 d . U . . .
H19B H 0.1691 0.2058 0.4036 0.070 Uiso 1 1 calc R U . . .
C20B C 0.1037(8) 0.2814(4) 0.4055(6) 0.076(3) Uani 1 1 d . U . . .
H20B H 0.0980 0.2846 0.3510 0.091 Uiso 1 1 calc R U . . .
C21B C 0.0676(7) 0.3245(4) 0.4518(6) 0.067(2) Uani 1 1 d . U . . .
H21B H 0.0353 0.3558 0.4299 0.081 Uiso 1 1 calc R U . . .
C22B C 0.0805(5) 0.3198(3) 0.5291(5) 0.0517(19) Uani 1 1 d . U . . .
H22B H 0.0590 0.3493 0.5615 0.062 Uiso 1 1 calc R U . . .
C23B C 0.1239(4) 0.2736(3) 0.5628(4) 0.0416(15) Uani 1 1 d . U . . .
H23B H 0.1300 0.2714 0.6174 0.050 Uiso 1 1 calc R U . . .
C24B C 0.3375(4) 0.1825(3) 0.5230(4) 0.0345(14) Uani 1 1 d . U . . .
C25B C 0.3698(6) 0.1606(4) 0.4525(4) 0.055(2) Uani 1 1 d . U . . .
H25B H 0.3293 0.1369 0.4229 0.065 Uiso 1 1 calc R U . . .
C26B C 0.4596(6) 0.1728(5) 0.4255(5) 0.066(3) Uani 1 1 d . U . . .
H26B H 0.4811 0.1568 0.3786 0.079 Uiso 1 1 calc R U . . .
C27B C 0.5182(5) 0.2092(4) 0.4683(5) 0.057(2) Uani 1 1 d . U . . .
H27B H 0.5804 0.2178 0.4519 0.069 Uiso 1 1 calc R U . . .
C28B C 0.4825(6) 0.2317(4) 0.5341(5) 0.057(2) Uani 1 1 d . U . . .
H28B H 0.5206 0.2583 0.5612 0.068 Uiso 1 1 calc R U . . .
C29B C 0.3972(5) 0.2191(3) 0.5639(4) 0.0387(15) Uani 1 1 d . U . . .
H29B H 0.3781 0.2349 0.6117 0.046 Uiso 1 1 calc R U . . .
C30B C 0.1387(4) 0.0832(2) 0.7240(3) 0.0240(11) Uani 1 1 d . U . . .
H30C H 0.0752 0.0672 0.7336 0.029 Uiso 1 1 calc R U . . .
H30D H 0.1771 0.0785 0.7717 0.029 Uiso 1 1 calc R U . . .
C31B C 0.3206(4) 0.0417(3) 0.6771(3) 0.0288(13) Uani 1 1 d . U . . .
C32B C 0.3421(4) 0.0192(3) 0.7494(4) 0.0347(14) Uani 1 1 d . U . . .
H32B H 0.2925 0.0073 0.7822 0.042 Uiso 1 1 calc R U . . .
C33B C 0.4353(5) 0.0140(3) 0.7738(4) 0.0394(16) Uani 1 1 d . U . . .
H33B H 0.4495 -0.0008 0.8235 0.047 Uiso 1 1 calc R U . . .
C34B C 0.5069(5) 0.0301(3) 0.7265(4) 0.0369(15) Uani 1 1 d . U . . .
H34B H 0.5709 0.0257 0.7429 0.044 Uiso 1 1 calc R U . . .
C35B C 0.4866(5) 0.0528(3) 0.6555(4) 0.0347(14) Uani 1 1 d . U . . .
H35B H 0.5369 0.0644 0.6232 0.042 Uiso 1 1 calc R U . . .
C36B C 0.3955(5) 0.0588(3) 0.6304(4) 0.0330(14) Uani 1 1 d . U . . .
H36B H 0.3827 0.0748 0.5811 0.040 Uiso 1 1 calc R U . . .
C37B C 0.1698(5) -0.0308(3) 0.6648(4) 0.0374(15) Uani 1 1 d . U . . .
C38B C 0.2084(9) -0.0694(4) 0.6147(6) 0.077(3) Uani 1 1 d . U . . .
H38B H 0.2439 -0.0569 0.5718 0.092 Uiso 1 1 calc R U . . .
C39B C 0.1954(12) -0.1271(5) 0.6271(8) 0.102(4) Uani 1 1 d . U . . .
H39B H 0.2247 -0.1535 0.5938 0.123 Uiso 1 1 calc R U . . .
C40B C 0.1438(10) -0.1447(5) 0.6835(8) 0.097(4) Uani 1 1 d . U . . .
H40B H 0.1322 -0.1838 0.6891 0.117 Uiso 1 1 calc R U . . .
C41B C 0.1051(9) -0.1069(4) 0.7361(8) 0.087(3) Uani 1 1 d . U . . .
H41B H 0.0697 -0.1205 0.7785 0.105 Uiso 1 1 calc R U . . .
C42B C 0.1186(6) -0.0500(3) 0.7263(6) 0.055(2) Uani 1 1 d . U . . .
H42B H 0.0925 -0.0240 0.7620 0.066 Uiso 1 1 calc R U . . .
C43B C 0.1207(4) 0.1804(3) 0.7905(3) 0.0265(12) Uani 1 1 d . U . . .
C44B C 0.1972(5) 0.2075(3) 0.8274(4) 0.0311(13) Uani 1 1 d . U . . .
H44B H 0.2536 0.2132 0.7991 0.037 Uiso 1 1 calc R U . . .
C45B C 0.1942(5) 0.2270(3) 0.9049(4) 0.0378(15) Uani 1 1 d . U . . .
H45B H 0.2483 0.2442 0.9277 0.045 Uiso 1 1 calc R U . . .
C46B C 0.1111(5) 0.2207(3) 0.9476(4) 0.0410(16) Uani 1 1 d . U . . .
H46B H 0.1081 0.2339 0.9993 0.049 Uiso 1 1 calc R U . . .
C47B C 0.0312(6) 0.1943(3) 0.9121(4) 0.0417(16) Uani 1 1 d . U . . .
H47B H -0.0254 0.1895 0.9405 0.050 Uiso 1 1 calc R U . . .
C48B C 0.0354(5) 0.1750(3) 0.8354(4) 0.0340(14) Uani 1 1 d . U . . .
H48B H -0.0190 0.1582 0.8125 0.041 Uiso 1 1 calc R U . . .
C49B C 0.1469(6) 0.3380(3) 0.8129(5) 0.0478(19) Uani 1 1 d . U . . .
C50B C -0.0176(6) 0.3206(3) 0.8885(4) 0.0467(18) Uani 1 1 d . U . . .
C51B C -0.0041(5) 0.2878(3) 0.7439(4) 0.0369(15) Uani 1 1 d . U . . .
B1B B 0.1278(5) 0.1518(3) 0.7047(4) 0.0232(13) Uani 1 1 d . U . . .
N1C N 0.3274(5) 0.4649(3) 0.5782(4) 0.0491(15) Uani 1 1 d . U . . .
C1C C 0.3886(7) 0.4509(5) 0.5114(6) 0.078(3) Uani 1 1 d . U . . .
H1CA H 0.3732 0.4764 0.4680 0.094 Uiso 1 1 calc R U . . .
H1CB H 0.3749 0.4119 0.4944 0.094 Uiso 1 1 calc R U . . .
C2C C 0.4951(7) 0.4560(5) 0.5318(7) 0.080(3) Uani 1 1 d . U . . .
H2CA H 0.5327 0.4449 0.4871 0.120 Uiso 1 1 calc R U . . .
H2CB H 0.5103 0.4314 0.5756 0.120 Uiso 1 1 calc R U . . .
H2CC H 0.5098 0.4951 0.5455 0.120 Uiso 1 1 calc R U . . .
C3C C 0.3464(8) 0.4259(4) 0.6495(6) 0.067(2) Uani 1 1 d . U . . .
H3CA H 0.4126 0.4313 0.6674 0.080 Uiso 1 1 calc R U . . .
H3CB H 0.3043 0.4374 0.6920 0.080 Uiso 1 1 calc R U . . .
C4C C 0.3309(8) 0.3652(4) 0.6329(8) 0.085(3) Uani 1 1 d . U . . .
H4CA H 0.3348 0.3438 0.6811 0.128 Uiso 1 1 calc R U . . .
H4CB H 0.3796 0.3519 0.5974 0.128 Uiso 1 1 calc R U . . .
H4CC H 0.2682 0.3601 0.6092 0.128 Uiso 1 1 calc R U . . .
C5C C 0.2257(7) 0.4575(5) 0.5517(6) 0.069(3) Uani 1 1 d . U . . .
H5CA H 0.2127 0.4843 0.5092 0.083 Uiso 1 1 calc R U . . .
H5CB H 0.2183 0.4191 0.5305 0.083 Uiso 1 1 calc R U . . .
C6C C 0.1539(6) 0.4659(5) 0.6122(6) 0.071(3) Uani 1 1 d . U . . .
H6CA H 0.0924 0.4738 0.5879 0.106 Uiso 1 1 calc R U . . .
H6CB H 0.1726 0.4977 0.6451 0.106 Uiso 1 1 calc R U . . .
H6CC H 0.1493 0.4318 0.6438 0.106 Uiso 1 1 calc R U . . .
C7C C 0.3413(9) 0.5235(4) 0.6078(6) 0.074(3) Uani 1 1 d . U . . .
H7CA H 0.4018 0.5255 0.6371 0.089 Uiso 1 1 calc R U . . .
H7CB H 0.2896 0.5328 0.6437 0.089 Uiso 1 1 calc R U . . .
C8C C 0.3427(9) 0.5683(5) 0.5403(7) 0.085(3) Uani 1 1 d . U . . .
H8CA H 0.3446 0.6063 0.5623 0.127 Uiso 1 1 calc R U . . .
H8CB H 0.2856 0.5641 0.5082 0.127 Uiso 1 1 calc R U . . .
H8CC H 0.3988 0.5623 0.5086 0.127 Uiso 1 1 calc R U . . .
N1D N 0.8080(4) 0.4624(3) 0.7548(3) 0.0393(13) Uani 1 1 d . U . . .
C1D C 0.9123(6) 0.4791(4) 0.7324(5) 0.0480(18) Uani 1 1 d . U . . .
H1DA H 0.9172 0.4786 0.6755 0.058 Uiso 1 1 calc R U . . .
H1DB H 0.9244 0.5181 0.7499 0.058 Uiso 1 1 calc R U . . .
C2D C 0.9863(6) 0.4426(4) 0.7648(5) 0.056(2) Uani 1 1 d . U . . .
H2DA H 1.0482 0.4604 0.7581 0.084 Uiso 1 1 calc R U . . .
H2DB H 0.9852 0.4063 0.7381 0.084 Uiso 1 1 calc R U . . .
H2DC H 0.9749 0.4368 0.8199 0.084 Uiso 1 1 calc R U . . .
C3D C 0.7970(7) 0.4644(4) 0.8403(4) 0.053(2) Uani 1 1 d . U . . .
H3DA H 0.8429 0.4381 0.8645 0.063 Uiso 1 1 calc R U . . .
H3DB H 0.7326 0.4514 0.8535 0.063 Uiso 1 1 calc R U . . .
C4D C 0.8126(8) 0.5234(4) 0.8741(5) 0.070(3) Uani 1 1 d . U . . .
H4DA H 0.7832 0.5257 0.9250 0.105 Uiso 1 1 calc R U . . .
H4DB H 0.7838 0.5515 0.8397 0.105 Uiso 1 1 calc R U . . .
H4DC H 0.8806 0.5307 0.8792 0.105 Uiso 1 1 calc R U . . .
C5D C 0.7461(6) 0.5026(4) 0.7146(5) 0.0518(19) Uani 1 1 d . U . . .
H5DA H 0.7569 0.4994 0.6584 0.062 Uiso 1 1 calc R U . . .
H5DB H 0.7645 0.5411 0.7304 0.062 Uiso 1 1 calc R U . . .
C6D C 0.6407(6) 0.4950(4) 0.7293(6) 0.065(2) Uani 1 1 d . U . . .
H6DA H 0.6068 0.5294 0.7145 0.098 Uiso 1 1 calc R U . . .
H6DB H 0.6309 0.4874 0.7842 0.098 Uiso 1 1 calc R U . . .
H6DC H 0.6167 0.4633 0.6986 0.098 Uiso 1 1 calc R U . . .
C7D C 0.7888(6) 0.4021(3) 0.7301(5) 0.0484(18) Uani 1 1 d . U . . .
H7DA H 0.8360 0.3774 0.7557 0.058 Uiso 1 1 calc R U . . .
H7DB H 0.7256 0.3910 0.7488 0.058 Uiso 1 1 calc R U . . .
C8D C 0.7921(6) 0.3918(3) 0.6446(4) 0.0486(19) Uani 1 1 d . U . . .
H8DA H 0.7800 0.3519 0.6341 0.073 Uiso 1 1 calc R U . . .
H8DB H 0.8547 0.4020 0.6253 0.073 Uiso 1 1 calc R U . . .
H8DC H 0.7437 0.4147 0.6186 0.073 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1A C50A 1.928(7) . ?
W1A C51A 1.936(6) . ?
W1A C49A 1.957(8) . ?
W1A C48A 2.325(6) . ?
W1A C46A 2.326(7) . ?
W1A C47A 2.348(7) . ?
W1A C44A 2.354(6) . ?
W1A C45A 2.357(7) . ?
W1A C43A 2.411(6) . ?
Cr1A C2A 1.815(7) . ?
Cr1A C3A 1.822(7) . ?
Cr1A C1A 1.841(7) . ?
Cr1A P1A 2.3827(18) . ?
Cr1A P3A 2.4166(17) . ?
Cr1A P2A 2.4257(19) . ?
P1A C4A 1.834(6) . ?
P1A C11A 1.839(6) . ?
P1A C5A 1.842(7) . ?
P2A C17A 1.822(6) . ?
P2A C24A 1.841(6) . ?
P2A C18A 1.856(6) . ?
P3A C37A 1.827(6) . ?
P3A C30A 1.832(6) . ?
P3A C31A 1.859(6) . ?
O1A C1A 1.155(8) . ?
O2A C2A 1.177(8) . ?
O3A C3A 1.169(8) . ?
O4A C49A 1.156(9) . ?
O5A C50A 1.168(9) . ?
O6A C51A 1.151(8) . ?
C4A B1A 1.654(9) . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C5A C6A 1.359(10) . ?
C5A C10A 1.398(10) . ?
C6A C7A 1.375(11) . ?
C6A H6AA 0.9500 . ?
C7A C8A 1.368(13) . ?
C7A H7AA 0.9500 . ?
C8A C9A 1.381(14) . ?
C8A H8AA 0.9500 . ?
C9A C10A 1.368(11) . ?
C9A H9AA 0.9500 . ?
C10A H10A 0.9500 . ?
C11A C12A 1.384(9) . ?
C11A C16A 1.394(10) . ?
C12A C13A 1.396(10) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.359(11) . ?
C13A H13A 0.9500 . ?
C14A C15A 1.369(11) . ?
C14A H14A 0.9500 . ?
C15A C16A 1.410(10) . ?
C15A H15A 0.9500 . ?
C16A H16A 0.9500 . ?
C17A B1A 1.668(9) . ?
C17A H17A 0.9900 . ?
C17A H17B 0.9900 . ?
C18A C23A 1.361(9) . ?
C18A C19A 1.425(9) . ?
C19A C20A 1.374(11) . ?
C19A H19A 0.9500 . ?
C20A C21A 1.376(12) . ?
C20A H20A 0.9500 . ?
C21A C22A 1.378(12) . ?
C21A H21A 0.9500 . ?
C22A C23A 1.389(10) . ?
C22A H22A 0.9500 . ?
C23A H23A 0.9500 . ?
C24A C29A 1.379(10) . ?
C24A C25A 1.384(10) . ?
C25A C26A 1.373(12) . ?
C25A H25A 0.9500 . ?
C26A C27A 1.377(15) . ?
C26A H26A 0.9500 . ?
C27A C28A 1.373(15) . ?
C27A H27A 0.9500 . ?
C28A C29A 1.398(11) . ?
C28A H28A 0.9500 . ?
C29A H29A 0.9500 . ?
C30A B1A 1.647(9) . ?
C30A H30A 0.9900 . ?
C30A H30B 0.9900 . ?
C31A C32A 1.397(9) . ?
C31A C36A 1.401(8) . ?
C32A C33A 1.395(9) . ?
C32A H32A 0.9500 . ?
C33A C34A 1.374(10) . ?
C33A H33A 0.9500 . ?
C34A C35A 1.408(10) . ?
C34A H34A 0.9500 . ?
C35A C36A 1.374(9) . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
C37A C42A 1.382(10) . ?
C37A C38A 1.412(9) . ?
C38A C39A 1.387(10) . ?
C38A H38A 0.9500 . ?
C39A C40A 1.409(13) . ?
C39A H39A 0.9500 . ?
C40A C41A 1.365(13) . ?
C40A H40A 0.9500 . ?
C41A C42A 1.410(11) . ?
C41A H41A 0.9500 . ?
C42A H42A 0.9500 . ?
C43A C48A 1.413(8) . ?
C43A C44A 1.430(9) . ?
C43A B1A 1.645(9) . ?
C44A C45A 1.418(9) . ?
C44A H44A 0.9500 . ?
C45A C46A 1.425(10) . ?
C45A H45A 0.9500 . ?
C46A C47A 1.403(10) . ?
C46A H46A 0.9500 . ?
C47A C48A 1.434(9) . ?
C47A H47A 0.9500 . ?
C48A H48A 0.9500 . ?
W1B C51B 1.935(8) . ?
W1B C50B 1.943(8) . ?
W1B C49B 1.961(8) . ?
W1B C47B 2.333(7) . ?
W1B C48B 2.344(7) . ?
W1B C46B 2.349(7) . ?
W1B C44B 2.355(7) . ?
W1B C45B 2.360(7) . ?
W1B C43B 2.412(6) . ?
Cr1B C2B 1.809(7) . ?
Cr1B C3B 1.818(8) . ?
Cr1B C1B 1.836(7) . ?
Cr1B P3B 2.3886(18) . ?
Cr1B P1B 2.4094(18) . ?
Cr1B P2B 2.419(2) . ?
P1B C4B 1.822(6) . ?
P1B C11B 1.841(6) . ?
P1B C5B 1.858(6) . ?
P2B C17B 1.820(6) . ?
P2B C24B 1.835(6) . ?
P2B C18B 1.862(7) . ?
P3B C30B 1.823(6) . ?
P3B C37B 1.842(7) . ?
P3B C31B 1.862(6) . ?
O1B C1B 1.157(8) . ?
O2B C2B 1.180(8) . ?
O3B C3B 1.171(9) . ?
O4B C49B 1.162(9) . ?
O5B C50B 1.165(9) . ?
O6B C51B 1.163(8) . ?
C4B B1B 1.652(9) . ?
C4B H4BA 0.9900 . ?
C4B H4BB 0.9900 . ?
C5B C10B 1.384(9) . ?
C5B C6B 1.406(9) . ?
C6B C7B 1.412(10) . ?
C6B H6BA 0.9500 . ?
C7B C8B 1.374(11) . ?
C7B H7BA 0.9500 . ?
C8B C9B 1.395(11) . ?
C8B H8BA 0.9500 . ?
C9B C10B 1.387(10) . ?
C9B H9BA 0.9500 . ?
C10B H10B 0.9500 . ?
C11B C12B 1.382(6) . ?
C11B C16B 1.383(6) . ?
C12B C13B 1.405(7) . ?
C12B H12B 0.9500 . ?
C13B C14B 1.323(7) . ?
C13B H13B 0.9500 . ?
C14B C15B 1.323(7) . ?
C14B H14B 0.9500 . ?
C15B C16B 1.406(7) . ?
C15B H15B 0.9500 . ?
C16B H16B 0.9500 . ?
C17B B1B 1.659(9) . ?
C17B H17C 0.9900 . ?
C17B H17D 0.9900 . ?
C18B C23B 1.372(10) . ?
C18B C19B 1.421(10) . ?
C19B C20B 1.367(12) . ?
C19B H19B 0.9500 . ?
C20B C21B 1.402(15) . ?
C20B H20B 0.9500 . ?
C21B C22B 1.355(13) . ?
C21B H21B 0.9500 . ?
C22B C23B 1.384(10) . ?
C22B H22B 0.9500 . ?
C23B H23B 0.9500 . ?
C24B C29B 1.401(10) . ?
C24B C25B 1.408(10) . ?
C25B C26B 1.389(11) . ?
C25B H25B 0.9500 . ?
C26B C27B 1.403(13) . ?
C26B H26B 0.9500 . ?
C27B C28B 1.361(12) . ?
C27B H27B 0.9500 . ?
C28B C29B 1.350(10) . ?
C28B H28B 0.9500 . ?
C29B H29B 0.9500 . ?
C30B B1B 1.671(9) . ?
C30B H30C 0.9900 . ?
C30B H30D 0.9900 . ?
C31B C32B 1.392(9) . ?
C31B C36B 1.401(9) . ?
C32B C33B 1.384(9) . ?
C32B H32B 0.9500 . ?
C33B C34B 1.363(10) . ?
C33B H33B 0.9500 . ?
C34B C35B 1.371(10) . ?
C34B H34B 0.9500 . ?
C35B C36B 1.361(9) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
C37B C42B 1.373(11) . ?
C37B C38B 1.380(11) . ?
C38B C39B 1.400(15) . ?
C38B H38B 0.9500 . ?
C39B C40B 1.295(18) . ?
C39B H39B 0.9500 . ?
C40B C41B 1.396(17) . ?
C40B H40B 0.9500 . ?
C41B C42B 1.379(13) . ?
C41B H41B 0.9500 . ?
C42B H42B 0.9500 . ?
C43B C44B 1.406(9) . ?
C43B C48B 1.447(9) . ?
C43B B1B 1.640(9) . ?
C44B C45B 1.421(9) . ?
C44B H44B 0.9500 . ?
C45B C46B 1.403(10) . ?
C45B H45B 0.9500 . ?
C46B C47B 1.425(11) . ?
C46B H46B 0.9500 . ?
C47B C48B 1.407(9) . ?
C47B H47B 0.9500 . ?
C48B H48B 0.9500 . ?
N1C C7C 1.496(12) . ?
N1C C1C 1.491(12) . ?
N1C C5C 1.513(11) . ?
N1C C3C 1.566(11) . ?
C1C C2C 1.547(14) . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C2C H2CA 0.9800 . ?
C2C H2CB 0.9800 . ?
C2C H2CC 0.9800 . ?
C3C C4C 1.487(14) . ?
C3C H3CA 0.9900 . ?
C3C H3CB 0.9900 . ?
C4C H4CA 0.9800 . ?
C4C H4CB 0.9800 . ?
C4C H4CC 0.9800 . ?
C5C C6C 1.481(13) . ?
C5C H5CA 0.9900 . ?
C5C H5CB 0.9900 . ?
C6C H6CA 0.9800 . ?
C6C H6CB 0.9800 . ?
C6C H6CC 0.9800 . ?
C7C C8C 1.582(14) . ?
C7C H7CA 0.9900 . ?
C7C H7CB 0.9900 . ?
C8C H8CA 0.9800 . ?
C8C H8CB 0.9800 . ?
C8C H8CC 0.9800 . ?
N1D C5D 1.467(10) . ?
N1D C3D 1.491(10) . ?
N1D C7D 1.521(9) . ?
N1D C1D 1.579(9) . ?
C1D C2D 1.464(12) . ?
C1D H1DA 0.9900 . ?
C1D H1DB 0.9900 . ?
C2D H2DA 0.9800 . ?
C2D H2DB 0.9800 . ?
C2D H2DC 0.9800 . ?
C3D C4D 1.534(12) . ?
C3D H3DA 0.9900 . ?
C3D H3DB 0.9900 . ?
C4D H4DA 0.9800 . ?
C4D H4DB 0.9800 . ?
C4D H4DC 0.9800 . ?
C5D C6D 1.524(12) . ?
C5D H5DA 0.9900 . ?
C5D H5DB 0.9900 . ?
C6D H6DA 0.9800 . ?
C6D H6DB 0.9800 . ?
C6D H6DC 0.9800 . ?
C7D C8D 1.503(11) . ?
C7D H7DA 0.9900 . ?
C7D H7DB 0.9900 . ?
C8D H8DA 0.9800 . ?
C8D H8DB 0.9800 . ?
C8D H8DC 0.9800 . ?

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
C50A W1A C51A 88.2(3) . . ?
C50A W1A C49A 88.9(3) . . ?
C51A W1A C49A 88.0(3) . . ?
C50A W1A C48A 139.6(3) . . ?
C51A W1A C48A 87.1(3) . . ?
C49A W1A C48A 131.0(3) . . ?
C50A W1A C46A 90.5(3) . . ?
C51A W1A C46A 130.1(3) . . ?
C49A W1A C46A 141.8(3) . . ?
C48A W1A C46A 63.2(2) . . ?
C50A W1A C47A 106.0(3) . . ?
C51A W1A C47A 98.6(3) . . ?
C49A W1A C47A 163.8(3) . . ?
C48A W1A C47A 35.7(2) . . ?
C46A W1A C47A 34.9(2) . . ?
C50A W1A C44A 134.4(3) . . ?
C51A W1A C44A 137.3(3) . . ?
C49A W1A C44A 91.4(3) . . ?
C48A W1A C44A 61.9(2) . . ?
C46A W1A C44A 62.9(2) . . ?
C47A W1A C44A 73.7(2) . . ?
C50A W1A C45A 102.7(3) . . ?
C51A W1A C45A 160.5(3) . . ?
C49A W1A C45A 108.0(3) . . ?
C48A W1A C45A 74.1(2) . . ?
C46A W1A C45A 35.4(2) . . ?
C47A W1A C45A 63.0(3) . . ?
C44A W1A C45A 35.0(2) . . ?
C50A W1A C43A 165.0(3) . . ?
C51A W1A C43A 103.5(3) . . ?
C49A W1A C43A 100.7(3) . . ?
C48A W1A C43A 34.7(2) . . ?
C46A W1A C43A 74.8(2) . . ?
C47A W1A C43A 63.5(2) . . ?
C44A W1A C43A 34.9(2) . . ?
C45A W1A C43A 63.4(2) . . ?
C2A Cr1A C3A 84.2(3) . . ?
C2A Cr1A C1A 86.3(3) . . ?
C3A Cr1A C1A 85.7(3) . . ?
C2A Cr1A P1A 175.9(2) . . ?
C3A Cr1A P1A 92.3(2) . . ?
C1A Cr1A P1A 91.5(2) . . ?
C2A Cr1A P3A 95.7(2) . . ?
C3A Cr1A P3A 95.2(2) . . ?
C1A Cr1A P3A 177.8(2) . . ?
P1A Cr1A P3A 86.52(6) . . ?
C2A Cr1A P2A 97.0(2) . . ?
C3A Cr1A P2A 178.8(2) . . ?
C1A Cr1A P2A 94.1(2) . . ?
P1A Cr1A P2A 86.56(6) . . ?
P3A Cr1A P2A 84.92(6) . . ?
C4A P1A C11A 106.6(3) . . ?
C4A P1A C5A 101.4(3) . . ?
C11A P1A C5A 99.2(3) . . ?
C4A P1A Cr1A 114.3(2) . . ?
C11A P1A Cr1A 111.7(2) . . ?
C5A P1A Cr1A 121.6(2) . . ?
C17A P2A C24A 105.4(3) . . ?
C17A P2A C18A 103.0(3) . . ?
C24A P2A C18A 97.5(3) . . ?
C17A P2A Cr1A 113.2(2) . . ?
C24A P2A Cr1A 115.9(2) . . ?
C18A P2A Cr1A 119.6(2) . . ?
C37A P3A C30A 106.5(3) . . ?
C37A P3A C31A 95.3(3) . . ?
C30A P3A C31A 103.4(3) . . ?
C37A P3A Cr1A 116.3(2) . . ?
C30A P3A Cr1A 113.5(2) . . ?
C31A P3A Cr1A 119.5(2) . . ?
O1A C1A Cr1A 173.4(6) . . ?
O2A C2A Cr1A 171.7(6) . . ?
O3A C3A Cr1A 172.9(6) . . ?
B1A C4A P1A 113.3(4) . . ?
B1A C4A H4AA 108.9 . . ?
P1A C4A H4AA 108.9 . . ?
B1A C4A H4AB 108.9 . . ?
P1A C4A H4AB 108.9 . . ?
H4AA C4A H4AB 107.7 . . ?
C6A C5A C10A 119.2(7) . . ?
C6A C5A P1A 122.5(6) . . ?
C10A C5A P1A 118.3(5) . . ?
C5A C6A C7A 121.3(8) . . ?
C5A C6A H6AA 119.3 . . ?
C7A C6A H6AA 119.3 . . ?
C8A C7A C6A 119.5(9) . . ?
C8A C7A H7AA 120.3 . . ?
C6A C7A H7AA 120.3 . . ?
C7A C8A C9A 120.1(8) . . ?
C7A C8A H8AA 120.0 . . ?
C9A C8A H8AA 120.0 . . ?
C10A C9A C8A 120.2(9) . . ?
C10A C9A H9AA 119.9 . . ?
C8A C9A H9AA 119.9 . . ?
C9A C10A C5A 119.6(8) . . ?
C9A C10A H10A 120.2 . . ?
C5A C10A H10A 120.2 . . ?
C12A C11A C16A 117.9(6) . . ?
C12A C11A P1A 119.3(5) . . ?
C16A C11A P1A 122.5(5) . . ?
C11A C12A C13A 121.2(7) . . ?
C11A C12A H12A 119.4 . . ?
C13A C12A H12A 119.4 . . ?
C14A C13A C12A 120.7(7) . . ?
C14A C13A H13A 119.6 . . ?
C12A C13A H13A 119.6 . . ?
C13A C14A C15A 119.4(7) . . ?
C13A C14A H14A 120.3 . . ?
C15A C14A H14A 120.3 . . ?
C14A C15A C16A 120.8(8) . . ?
C14A C15A H15A 119.6 . . ?
C16A C15A H15A 119.6 . . ?
C11A C16A C15A 119.9(7) . . ?
C11A C16A H16A 120.0 . . ?
C15A C16A H16A 120.0 . . ?
B1A C17A P2A 113.6(4) . . ?
B1A C17A H17A 108.8 . . ?
P2A C17A H17A 108.8 . . ?
B1A C17A H17B 108.8 . . ?
P2A C17A H17B 108.8 . . ?
H17A C17A H17B 107.7 . . ?
C23A C18A C19A 117.7(6) . . ?
C23A C18A P2A 124.1(5) . . ?
C19A C18A P2A 117.9(5) . . ?
C20A C19A C18A 119.5(7) . . ?
C20A C19A H19A 120.3 . . ?
C18A C19A H19A 120.3 . . ?
C19A C20A C21A 121.3(8) . . ?
C19A C20A H20A 119.3 . . ?
C21A C20A H20A 119.3 . . ?
C20A C21A C22A 119.8(7) . . ?
C20A C21A H21A 120.1 . . ?
C22A C21A H21A 120.1 . . ?
C21A C22A C23A 118.9(7) . . ?
C21A C22A H22A 120.5 . . ?
C23A C22A H22A 120.5 . . ?
C18A C23A C22A 122.7(7) . . ?
C18A C23A H23A 118.7 . . ?
C22A C23A H23A 118.7 . . ?
C29A C24A C25A 118.8(7) . . ?
C29A C24A P2A 121.7(5) . . ?
C25A C24A P2A 119.3(6) . . ?
C26A C25A C24A 120.4(9) . . ?
C26A C25A H25A 119.8 . . ?
C24A C25A H25A 119.8 . . ?
C25A C26A C27A 120.4(9) . . ?
C25A C26A H26A 119.8 . . ?
C27A C26A H26A 119.8 . . ?
C28A C27A C26A 120.4(8) . . ?
C28A C27A H27A 119.8 . . ?
C26A C27A H27A 119.8 . . ?
C27A C28A C29A 118.8(9) . . ?
C27A C28A H28A 120.6 . . ?
C29A C28A H28A 120.6 . . ?
C24A C29A C28A 121.1(8) . . ?
C24A C29A H29A 119.4 . . ?
C28A C29A H29A 119.4 . . ?
B1A C30A P3A 113.8(4) . . ?
B1A C30A H30A 108.8 . . ?
P3A C30A H30A 108.8 . . ?
B1A C30A H30B 108.8 . . ?
P3A C30A H30B 108.8 . . ?
H30A C30A H30B 107.7 . . ?
C32A C31A C36A 118.3(6) . . ?
C32A C31A P3A 121.8(5) . . ?
C36A C31A P3A 119.9(5) . . ?
C33A C32A C31A 120.9(6) . . ?
C33A C32A H32A 119.6 . . ?
C31A C32A H32A 119.6 . . ?
C34A C33A C32A 120.2(7) . . ?
C34A C33A H33A 119.9 . . ?
C32A C33A H33A 119.9 . . ?
C33A C34A C35A 119.4(6) . . ?
C33A C34A H34A 120.3 . . ?
C35A C34A H34A 120.3 . . ?
C36A C35A C34A 120.5(6) . . ?
C36A C35A H35A 119.8 . . ?
C34A C35A H35A 119.8 . . ?
C35A C36A C31A 120.8(6) . . ?
C35A C36A H36A 119.6 . . ?
C31A C36A H36A 119.6 . . ?
C42A C37A C38A 118.6(6) . . ?
C42A C37A P3A 123.2(5) . . ?
C38A C37A P3A 118.0(5) . . ?
C39A C38A C37A 121.7(7) . . ?
C39A C38A H38A 119.1 . . ?
C37A C38A H38A 119.1 . . ?
C38A C39A C40A 118.0(8) . . ?
C38A C39A H39A 121.0 . . ?
C40A C39A H39A 121.0 . . ?
C41A C40A C39A 121.2(7) . . ?
C41A C40A H40A 119.4 . . ?
C39A C40A H40A 119.4 . . ?
C40A C41A C42A 120.1(8) . . ?
C40A C41A H41A 119.9 . . ?
C42A C41A H41A 119.9 . . ?
C37A C42A C41A 120.2(7) . . ?
C37A C42A H42A 119.9 . . ?
C41A C42A H42A 119.9 . . ?
C48A C43A C44A 115.7(5) . . ?
C48A C43A B1A 120.7(5) . . ?
C44A C43A B1A 123.5(5) . . ?
C48A C43A W1A 69.4(3) . . ?
C44A C43A W1A 70.4(3) . . ?
B1A C43A W1A 132.9(4) . . ?
C45A C44A C43A 123.2(6) . . ?
C45A C44A W1A 72.6(4) . . ?
C43A C44A W1A 74.7(4) . . ?
C45A C44A H44A 118.4 . . ?
C43A C44A H44A 118.4 . . ?
W1A C44A H44A 126.3 . . ?
C44A C45A C46A 118.4(6) . . ?
C44A C45A W1A 72.4(4) . . ?
C46A C45A W1A 71.1(4) . . ?
C44A C45A H45A 120.8 . . ?
C46A C45A H45A 120.8 . . ?
W1A C45A H45A 127.7 . . ?
C47A C46A C45A 120.9(6) . . ?
C47A C46A W1A 73.4(4) . . ?
C45A C46A W1A 73.5(4) . . ?
C47A C46A H46A 119.6 . . ?
C45A C46A H46A 119.6 . . ?
W1A C46A H46A 125.3 . . ?
C46A C47A C48A 118.5(6) . . ?
C46A C47A W1A 71.7(4) . . ?
C48A C47A W1A 71.3(4) . . ?
C46A C47A H47A 120.7 . . ?
C48A C47A H47A 120.7 . . ?
W1A C47A H47A 128.5 . . ?
C43A C48A C47A 123.2(6) . . ?
C43A C48A W1A 76.0(4) . . ?
C47A C48A W1A 73.0(4) . . ?
C43A C48A H48A 118.4 . . ?
C47A C48A H48A 118.4 . . ?
W1A C48A H48A 124.2 . . ?
O4A C49A W1A 179.0(7) . . ?
O5A C50A W1A 178.9(7) . . ?
O6A C51A W1A 176.8(8) . . ?
C43A B1A C30A 111.4(5) . . ?
C43A B1A C4A 108.7(5) . . ?
C30A B1A C4A 112.1(5) . . ?
C43A B1A C17A 103.4(5) . . ?
C30A B1A C17A 108.9(5) . . ?
C4A B1A C17A 112.1(5) . . ?
C51B W1B C50B 85.5(3) . . ?
C51B W1B C49B 88.1(3) . . ?
C50B W1B C49B 88.0(4) . . ?
C51B W1B C47B 119.7(3) . . ?
C50B W1B C47B 92.9(3) . . ?
C49B W1B C47B 152.2(3) . . ?
C51B W1B C48B 94.8(3) . . ?
C50B W1B C48B 117.0(3) . . ?
C49B W1B C48B 154.9(3) . . ?
C47B W1B C48B 35.0(2) . . ?
C51B W1B C46B 155.1(3) . . ?
C50B W1B C46B 94.2(3) . . ?
C49B W1B C46B 116.7(3) . . ?
C47B W1B C46B 35.5(3) . . ?
C48B W1B C46B 63.2(2) . . ?
C51B W1B C44B 119.1(2) . . ?
C50B W1B C44B 155.3(3) . . ?
C49B W1B C44B 94.9(3) . . ?
C47B W1B C44B 73.3(2) . . ?
C48B W1B C44B 61.9(2) . . ?
C46B W1B C44B 62.6(2) . . ?
C51B W1B C45B 154.2(3) . . ?
C50B W1B C45B 120.3(3) . . ?
C49B W1B C45B 93.2(3) . . ?
C47B W1B C45B 62.5(3) . . ?
C48B W1B C45B 73.6(2) . . ?
C46B W1B C45B 34.7(2) . . ?
C44B W1B C45B 35.1(2) . . ?
C51B W1B C43B 94.2(2) . . ?
C50B W1B C43B 152.4(3) . . ?
C49B W1B C43B 119.6(3) . . ?
C47B W1B C43B 63.3(2) . . ?
C48B W1B C43B 35.4(2) . . ?
C46B W1B C43B 74.7(2) . . ?
C44B W1B C43B 34.3(2) . . ?
C45B W1B C43B 62.8(2) . . ?
C2B Cr1B C3B 84.9(3) . . ?
C2B Cr1B C1B 87.4(3) . . ?
C3B Cr1B C1B 86.1(3) . . ?
C2B Cr1B P3B 88.8(2) . . ?
C3B Cr1B P3B 94.1(2) . . ?
C1B Cr1B P3B 176.1(2) . . ?
C2B Cr1B P1B 175.7(3) . . ?
C3B Cr1B P1B 93.2(2) . . ?
C1B Cr1B P1B 96.4(2) . . ?
P3B Cr1B P1B 87.48(6) . . ?
C2B Cr1B P2B 98.6(3) . . ?
C3B Cr1B P2B 176.2(2) . . ?
C1B Cr1B P2B 92.5(2) . . ?
P3B Cr1B P2B 87.55(6) . . ?
P1B Cr1B P2B 83.43(6) . . ?
C4B P1B C11B 105.5(2) . . ?
C4B P1B C5B 100.4(3) . . ?
C11B P1B C5B 97.5(2) . . ?
C4B P1B Cr1B 115.09(19) . . ?
C11B P1B Cr1B 115.25(16) . . ?
C5B P1B Cr1B 120.5(2) . . ?
C17B P2B C24B 105.0(3) . . ?
C17B P2B C18B 103.9(3) . . ?
C24B P2B C18B 97.7(3) . . ?
C17B P2B Cr1B 113.0(2) . . ?
C24B P2B Cr1B 117.3(2) . . ?
C18B P2B Cr1B 117.9(2) . . ?
C30B P3B C37B 106.4(3) . . ?
C30B P3B C31B 102.7(3) . . ?
C37B P3B C31B 95.7(3) . . ?
C30B P3B Cr1B 114.1(2) . . ?
C37B P3B Cr1B 115.2(2) . . ?
C31B P3B Cr1B 120.3(2) . . ?
O1B C1B Cr1B 172.3(6) . . ?
O2B C2B Cr1B 175.5(7) . . ?
O3B C3B Cr1B 174.1(6) . . ?
B1B C4B P1B 114.2(4) . . ?
B1B C4B H4BA 108.7 . . ?
P1B C4B H4BA 108.7 . . ?
B1B C4B H4BB 108.7 . . ?
P1B C4B H4BB 108.7 . . ?
H4BA C4B H4BB 107.6 . . ?
C10B C5B C6B 119.7(6) . . ?
C10B C5B P1B 118.5(5) . . ?
C6B C5B P1B 121.8(5) . . ?
C5B C6B C7B 119.8(6) . . ?
C5B C6B H6BA 120.1 . . ?
C7B C6B H6BA 120.1 . . ?
C8B C7B C6B 119.9(7) . . ?
C8B C7B H7BA 120.0 . . ?
C6B C7B H7BA 120.0 . . ?
C7B C8B C9B 119.6(7) . . ?
C7B C8B H8BA 120.2 . . ?
C9B C8B H8BA 120.2 . . ?
C10B C9B C8B 121.3(7) . . ?
C10B C9B H9BA 119.3 . . ?
C8B C9B H9BA 119.3 . . ?
C5B C10B C9B 119.6(6) . . ?
C5B C10B H10B 120.2 . . ?
C9B C10B H10B 120.2 . . ?
C12B C11B C16B 119.4(6) . . ?
C12B C11B P1B 117.6(4) . . ?
C16B C11B P1B 122.8(4) . . ?
C11B C12B C13B 119.9(6) . . ?
C11B C12B H12B 120.1 . . ?
C13B C12B H12B 120.1 . . ?
C14B C13B C12B 117.5(6) . . ?
C14B C13B H13B 121.3 . . ?
C12B C13B H13B 121.3 . . ?
C15B C14B C13B 126.0(8) . . ?
C15B C14B H14B 117.0 . . ?
C13B C14B H14B 117.0 . . ?
C14B C15B C16B 117.7(6) . . ?
C14B C15B H15B 121.1 . . ?
C16B C15B H15B 121.1 . . ?
C11B C16B C15B 119.6(6) . . ?
C11B C16B H16B 120.2 . . ?
C15B C16B H16B 120.2 . . ?
B1B C17B P2B 113.3(4) . . ?
B1B C17B H17C 108.9 . . ?
P2B C17B H17C 108.9 . . ?
B1B C17B H17D 108.9 . . ?
P2B C17B H17D 108.9 . . ?
H17C C17B H17D 107.7 . . ?
C23B C18B C19B 118.7(7) . . ?
C23B C18B P2B 124.4(5) . . ?
C19B C18B P2B 116.9(6) . . ?
C20B C19B C18B 119.0(9) . . ?
C20B C19B H19B 120.5 . . ?
C18B C19B H19B 120.5 . . ?
C19B C20B C21B 122.2(9) . . ?
C19B C20B H20B 118.9 . . ?
C21B C20B H20B 118.9 . . ?
C22B C21B C20B 117.3(8) . . ?
C22B C21B H21B 121.3 . . ?
C20B C21B H21B 121.3 . . ?
C21B C22B C23B 122.5(9) . . ?
C21B C22B H22B 118.7 . . ?
C23B C22B H22B 118.7 . . ?
C18B C23B C22B 120.2(7) . . ?
C18B C23B H23B 119.9 . . ?
C22B C23B H23B 119.9 . . ?
C29B C24B C25B 118.0(6) . . ?
C29B C24B P2B 121.7(5) . . ?
C25B C24B P2B 120.2(6) . . ?
C26B C25B C24B 121.5(8) . . ?
C26B C25B H25B 119.2 . . ?
C24B C25B H25B 119.2 . . ?
C25B C26B C27B 119.1(8) . . ?
C25B C26B H26B 120.5 . . ?
C27B C26B H26B 120.5 . . ?
C28B C27B C26B 117.6(7) . . ?
C28B C27B H27B 121.2 . . ?
C26B C27B H27B 121.2 . . ?
C29B C28B C27B 125.0(9) . . ?
C29B C28B H28B 117.5 . . ?
C27B C28B H28B 117.5 . . ?
C28B C29B C24B 118.7(7) . . ?
C28B C29B H29B 120.7 . . ?
C24B C29B H29B 120.7 . . ?
B1B C30B P3B 113.0(4) . . ?
B1B C30B H30C 109.0 . . ?
P3B C30B H30C 109.0 . . ?
B1B C30B H30D 109.0 . . ?
P3B C30B H30D 109.0 . . ?
H30C C30B H30D 107.8 . . ?
C32B C31B C36B 118.2(6) . . ?
C32B C31B P3B 118.0(5) . . ?
C36B C31B P3B 123.7(5) . . ?
C33B C32B C31B 120.4(6) . . ?
C33B C32B H32B 119.8 . . ?
C31B C32B H32B 119.8 . . ?
C34B C33B C32B 120.1(7) . . ?
C34B C33B H33B 119.9 . . ?
C32B C33B H33B 119.9 . . ?
C33B C34B C35B 120.0(6) . . ?
C33B C34B H34B 120.0 . . ?
C35B C34B H34B 120.0 . . ?
C36B C35B C34B 121.0(6) . . ?
C36B C35B H35B 119.5 . . ?
C34B C35B H35B 119.5 . . ?
C35B C36B C31B 120.2(6) . . ?
C35B C36B H36B 119.9 . . ?
C31B C36B H36B 119.9 . . ?
C42B C37B C38B 118.9(8) . . ?
C42B C37B P3B 123.9(6) . . ?
C38B C37B P3B 117.2(7) . . ?
C37B C38B C39B 120.1(11) . . ?
C37B C38B H38B 119.9 . . ?
C39B C38B H38B 119.9 . . ?
C40B C39B C38B 120.5(13) . . ?
C40B C39B H39B 119.8 . . ?
C38B C39B H39B 119.8 . . ?
C39B C40B C41B 120.9(12) . . ?
C39B C40B H40B 119.5 . . ?
C41B C40B H40B 119.5 . . ?
C42B C41B C40B 119.7(12) . . ?
C42B C41B H41B 120.2 . . ?
C40B C41B H41B 120.2 . . ?
C37B C42B C41B 119.7(10) . . ?
C37B C42B H42B 120.1 . . ?
C41B C42B H42B 120.1 . . ?
C44B C43B C48B 115.9(5) . . ?
C44B C43B B1B 123.2(5) . . ?
C48B C43B B1B 120.7(5) . . ?
C44B C43B W1B 70.7(4) . . ?
C48B C43B W1B 69.7(3) . . ?
B1B C43B W1B 133.5(4) . . ?
C43B C44B C45B 123.2(6) . . ?
C43B C44B W1B 75.1(4) . . ?
C45B C44B W1B 72.6(4) . . ?
C43B C44B H44B 118.4 . . ?
C45B C44B H44B 118.4 . . ?
W1B C44B H44B 125.8 . . ?
C46B C45B C44B 119.9(6) . . ?
C46B C45B W1B 72.2(4) . . ?
C44B C45B W1B 72.3(4) . . ?
C46B C45B H45B 120.1 . . ?
C44B C45B H45B 120.1 . . ?
W1B C45B H45B 127.4 . . ?
C45B C46B C47B 118.9(6) . . ?
C45B C46B W1B 73.1(4) . . ?
C47B C46B W1B 71.7(4) . . ?
C45B C46B H46B 120.6 . . ?
C47B C46B H46B 120.6 . . ?
W1B C46B H46B 126.5 . . ?
C48B C47B C46B 120.5(6) . . ?
C48B C47B W1B 72.9(4) . . ?
C46B C47B W1B 72.9(4) . . ?
C48B C47B H47B 119.7 . . ?
C46B C47B H47B 119.7 . . ?
W1B C47B H47B 126.4 . . ?
C47B C48B C43B 121.6(6) . . ?
C47B C48B W1B 72.1(4) . . ?
C43B C48B W1B 74.9(4) . . ?
C47B C48B H48B 119.2 . . ?
C43B C48B H48B 119.2 . . ?
W1B C48B H48B 125.6 . . ?
O4B C49B W1B 177.1(8) . . ?
O5B C50B W1B 178.3(7) . . ?
O6B C51B W1B 177.7(6) . . ?
C43B B1B C4B 110.0(5) . . ?
C43B B1B C17B 109.2(5) . . ?
C4B B1B C17B 112.0(5) . . ?
C43B B1B C30B 103.3(5) . . ?
C4B B1B C30B 109.4(5) . . ?
C17B B1B C30B 112.6(5) . . ?
C7C N1C C1C 113.6(8) . . ?
C7C N1C C5C 109.5(8) . . ?
C1C N1C C5C 107.2(7) . . ?
C7C N1C C3C 105.1(7) . . ?
C1C N1C C3C 112.5(8) . . ?
C5C N1C C3C 108.9(7) . . ?
N1C C1C C2C 112.1(9) . . ?
N1C C1C H1CA 109.2 . . ?
C2C C1C H1CA 109.2 . . ?
N1C C1C H1CB 109.2 . . ?
C2C C1C H1CB 109.2 . . ?
H1CA C1C H1CB 107.9 . . ?
C1C C2C H2CA 109.5 . . ?
C1C C2C H2CB 109.5 . . ?
H2CA C2C H2CB 109.5 . . ?
C1C C2C H2CC 109.5 . . ?
H2CA C2C H2CC 109.5 . . ?
H2CB C2C H2CC 109.5 . . ?
C4C C3C N1C 113.5(9) . . ?
C4C C3C H3CA 108.9 . . ?
N1C C3C H3CA 108.9 . . ?
C4C C3C H3CB 108.9 . . ?
N1C C3C H3CB 108.9 . . ?
H3CA C3C H3CB 107.7 . . ?
C3C C4C H4CA 109.5 . . ?
C3C C4C H4CB 109.5 . . ?
H4CA C4C H4CB 109.5 . . ?
C3C C4C H4CC 109.5 . . ?
H4CA C4C H4CC 109.5 . . ?
H4CB C4C H4CC 109.5 . . ?
C6C C5C N1C 115.1(8) . . ?
C6C C5C H5CA 108.5 . . ?
N1C C5C H5CA 108.5 . . ?
C6C C5C H5CB 108.5 . . ?
N1C C5C H5CB 108.5 . . ?
H5CA C5C H5CB 107.5 . . ?
C5C C6C H6CA 109.5 . . ?
C5C C6C H6CB 109.5 . . ?
H6CA C6C H6CB 109.5 . . ?
C5C C6C H6CC 109.5 . . ?
H6CA C6C H6CC 109.5 . . ?
H6CB C6C H6CC 109.5 . . ?
N1C C7C C8C 112.1(8) . . ?
N1C C7C H7CA 109.2 . . ?
C8C C7C H7CA 109.2 . . ?
N1C C7C H7CB 109.2 . . ?
C8C C7C H7CB 109.2 . . ?
H7CA C7C H7CB 107.9 . . ?
C7C C8C H8CA 109.5 . . ?
C7C C8C H8CB 109.5 . . ?
H8CA C8C H8CB 109.5 . . ?
C7C C8C H8CC 109.5 . . ?
H8CA C8C H8CC 109.5 . . ?
H8CB C8C H8CC 109.5 . . ?
C5D N1D C3D 112.5(7) . . ?
C5D N1D C7D 112.2(6) . . ?
C3D N1D C7D 106.8(6) . . ?
C5D N1D C1D 105.8(6) . . ?
C3D N1D C1D 110.1(6) . . ?
C7D N1D C1D 109.3(6) . . ?
C2D C1D N1D 115.0(7) . . ?
C2D C1D H1DA 108.5 . . ?
N1D C1D H1DA 108.5 . . ?
C2D C1D H1DB 108.5 . . ?
N1D C1D H1DB 108.5 . . ?
H1DA C1D H1DB 107.5 . . ?
C1D C2D H2DA 109.5 . . ?
C1D C2D H2DB 109.5 . . ?
H2DA C2D H2DB 109.5 . . ?
C1D C2D H2DC 109.5 . . ?
H2DA C2D H2DC 109.5 . . ?
H2DB C2D H2DC 109.5 . . ?
N1D C3D C4D 113.1(7) . . ?
N1D C3D H3DA 109.0 . . ?
C4D C3D H3DA 109.0 . . ?
N1D C3D H3DB 109.0 . . ?
C4D C3D H3DB 109.0 . . ?
H3DA C3D H3DB 107.8 . . ?
C3D C4D H4DA 109.5 . . ?
C3D C4D H4DB 109.5 . . ?
H4DA C4D H4DB 109.5 . . ?
C3D C4D H4DC 109.5 . . ?
H4DA C4D H4DC 109.5 . . ?
H4DB C4D H4DC 109.5 . . ?
N1D C5D C6D 114.9(7) . . ?
N1D C5D H5DA 108.5 . . ?
C6D C5D H5DA 108.5 . . ?
N1D C5D H5DB 108.5 . . ?
C6D C5D H5DB 108.5 . . ?
H5DA C5D H5DB 107.5 . . ?
C5D C6D H6DA 109.5 . . ?
C5D C6D H6DB 109.5 . . ?
H6DA C6D H6DB 109.5 . . ?
C5D C6D H6DC 109.5 . . ?
H6DA C6D H6DC 109.5 . . ?
H6DB C6D H6DC 109.5 . . ?
C8D C7D N1D 115.1(7) . . ?
C8D C7D H7DA 108.5 . . ?
N1D C7D H7DA 108.5 . . ?
C8D C7D H7DB 108.5 . . ?
N1D C7D H7DB 108.5 . . ?
H7DA C7D H7DB 107.5 . . ?
C7D C8D H8DA 109.5 . . ?
C7D C8D H8DB 109.5 . . ?
H8DA C8D H8DB 109.5 . . ?
C7D C8D H8DC 109.5 . . ?
H8DA C8D H8DC 109.5 . . ?
H8DB C8D H8DC 109.5 . . ?

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
C11A P1A C4A B1A 159.6(4) . . . . ?
C5A P1A C4A B1A -97.0(5) . . . . ?
Cr1A P1A C4A B1A 35.7(5) . . . . ?
C4A P1A C5A C6A 126.3(6) . . . . ?
C11A P1A C5A C6A -124.5(6) . . . . ?
Cr1A P1A C5A C6A -1.8(7) . . . . ?
C4A P1A C5A C10A -54.6(6) . . . . ?
C11A P1A C5A C10A 54.6(6) . . . . ?
Cr1A P1A C5A C10A 177.3(5) . . . . ?
C10A C5A C6A C7A 3.0(12) . . . . ?
P1A C5A C6A C7A -177.9(7) . . . . ?
C5A C6A C7A C8A -2.2(14) . . . . ?
C6A C7A C8A C9A 1.0(15) . . . . ?
C7A C8A C9A C10A -0.7(15) . . . . ?
C8A C9A C10A C5A 1.5(13) . . . . ?
C6A C5A C10A C9A -2.6(11) . . . . ?
P1A C5A C10A C9A 178.2(6) . . . . ?
C4A P1A C11A C12A 154.2(6) . . . . ?
C5A P1A C11A C12A 49.3(6) . . . . ?
Cr1A P1A C11A C12A -80.3(6) . . . . ?
C4A P1A C11A C16A -32.7(6) . . . . ?
C5A P1A C11A C16A -137.7(6) . . . . ?
Cr1A P1A C11A C16A 92.8(5) . . . . ?
C16A C11A C12A C13A 0.6(11) . . . . ?
P1A C11A C12A C13A 174.0(6) . . . . ?
C11A C12A C13A C14A 1.8(12) . . . . ?
C12A C13A C14A C15A -1.6(12) . . . . ?
C13A C14A C15A C16A -1.1(12) . . . . ?
C12A C11A C16A C15A -3.3(10) . . . . ?
P1A C11A C16A C15A -176.4(5) . . . . ?
C14A C15A C16A C11A 3.6(11) . . . . ?
C24A P2A C17A B1A 164.2(4) . . . . ?
C18A P2A C17A B1A -94.1(5) . . . . ?
Cr1A P2A C17A B1A 36.6(5) . . . . ?
C17A P2A C18A C23A -2.3(7) . . . . ?
C24A P2A C18A C23A 105.5(6) . . . . ?
Cr1A P2A C18A C23A -128.9(5) . . . . ?
C17A P2A C18A C19A -175.8(5) . . . . ?
C24A P2A C18A C19A -68.0(6) . . . . ?
Cr1A P2A C18A C19A 57.6(6) . . . . ?
C23A C18A C19A C20A 1.3(11) . . . . ?
P2A C18A C19A C20A 175.2(6) . . . . ?
C18A C19A C20A C21A 1.3(14) . . . . ?
C19A C20A C21A C22A -2.7(15) . . . . ?
C20A C21A C22A C23A 1.5(14) . . . . ?
C19A C18A C23A C22A -2.4(11) . . . . ?
P2A C18A C23A C22A -176.0(6) . . . . ?
C21A C22A C23A C18A 1.1(13) . . . . ?
C17A P2A C24A C29A 8.9(6) . . . . ?
C18A P2A C24A C29A -96.9(6) . . . . ?
Cr1A P2A C24A C29A 134.9(5) . . . . ?
C17A P2A C24A C25A -165.7(5) . . . . ?
C18A P2A C24A C25A 88.5(6) . . . . ?
Cr1A P2A C24A C25A -39.7(6) . . . . ?
C29A C24A C25A C26A -0.5(11) . . . . ?
P2A C24A C25A C26A 174.2(6) . . . . ?
C24A C25A C26A C27A -1.7(13) . . . . ?
C25A C26A C27A C28A 4.0(14) . . . . ?
C26A C27A C28A C29A -4.0(14) . . . . ?
C25A C24A C29A C28A 0.5(11) . . . . ?
P2A C24A C29A C28A -174.1(6) . . . . ?
C27A C28A C29A C24A 1.7(12) . . . . ?
C37A P3A C30A B1A 164.6(4) . . . . ?
C31A P3A C30A B1A -95.7(5) . . . . ?
Cr1A P3A C30A B1A 35.3(5) . . . . ?
C37A P3A C31A C32A -118.5(5) . . . . ?
C30A P3A C31A C32A 133.1(5) . . . . ?
Cr1A P3A C31A C32A 5.8(6) . . . . ?
C37A P3A C31A C36A 59.4(5) . . . . ?
C30A P3A C31A C36A -49.0(6) . . . . ?
Cr1A P3A C31A C36A -176.2(4) . . . . ?
C36A C31A C32A C33A 0.8(9) . . . . ?
P3A C31A C32A C33A 178.8(5) . . . . ?
C31A C32A C33A C34A -0.1(10) . . . . ?
C32A C33A C34A C35A -0.1(10) . . . . ?
C33A C34A C35A C36A -0.3(10) . . . . ?
C34A C35A C36A C31A 0.9(10) . . . . ?
C32A C31A C36A C35A -1.2(10) . . . . ?
P3A C31A C36A C35A -179.2(5) . . . . ?
C30A P3A C37A C42A 9.3(7) . . . . ?
C31A P3A C37A C42A -96.4(7) . . . . ?
Cr1A P3A C37A C42A 136.9(6) . . . . ?
C30A P3A C37A C38A -176.1(5) . . . . ?
C31A P3A C37A C38A 78.3(6) . . . . ?
Cr1A P3A C37A C38A -48.5(6) . . . . ?
C42A C37A C38A C39A -1.7(11) . . . . ?
P3A C37A C38A C39A -176.6(6) . . . . ?
C37A C38A C39A C40A -1.1(11) . . . . ?
C38A C39A C40A C41A 3.1(13) . . . . ?
C39A C40A C41A C42A -2.1(14) . . . . ?
C38A C37A C42A C41A 2.7(12) . . . . ?
P3A C37A C42A C41A 177.3(7) . . . . ?
C40A C41A C42A C37A -0.8(14) . . . . ?
C48A C43A C44A C45A -2.6(9) . . . . ?
B1A C43A C44A C45A 174.2(6) . . . . ?
W1A C43A C44A C45A -56.7(6) . . . . ?
C48A C43A C44A W1A 54.1(5) . . . . ?
B1A C43A C44A W1A -129.2(6) . . . . ?
C43A C44A C45A C46A 1.6(10) . . . . ?
W1A C44A C45A C46A -56.1(6) . . . . ?
C43A C44A C45A W1A 57.7(6) . . . . ?
C44A C45A C46A C47A -1.6(10) . . . . ?
W1A C45A C46A C47A -58.3(6) . . . . ?
C44A C45A C46A W1A 56.7(6) . . . . ?
C45A C46A C47A C48A 2.8(10) . . . . ?
W1A C46A C47A C48A -55.6(5) . . . . ?
C45A C46A C47A W1A 58.4(6) . . . . ?
C44A C43A C48A C47A 3.9(9) . . . . ?
B1A C43A C48A C47A -173.0(6) . . . . ?
W1A C43A C48A C47A 58.5(6) . . . . ?
C44A C43A C48A W1A -54.6(5) . . . . ?
B1A C43A C48A W1A 128.5(5) . . . . ?
C46A C47A C48A C43A -4.1(10) . . . . ?
W1A C47A C48A C43A -59.9(6) . . . . ?
C46A C47A C48A W1A 55.8(6) . . . . ?
C48A C43A B1A C30A -56.2(8) . . . . ?
C44A C43A B1A C30A 127.2(6) . . . . ?
W1A C43A B1A C30A 33.4(8) . . . . ?
C48A C43A B1A C4A 179.8(5) . . . . ?
C44A C43A B1A C4A 3.2(8) . . . . ?
W1A C43A B1A C4A -90.6(6) . . . . ?
C48A C43A B1A C17A 60.6(7) . . . . ?
C44A C43A B1A C17A -116.0(6) . . . . ?
W1A C43A B1A C17A 150.2(5) . . . . ?
P3A C30A B1A C43A 155.3(4) . . . . ?
P3A C30A B1A C4A -82.6(6) . . . . ?
P3A C30A B1A C17A 42.0(6) . . . . ?
P1A C4A B1A C43A 164.1(4) . . . . ?
P1A C4A B1A C30A 40.5(6) . . . . ?
P1A C4A B1A C17A -82.3(6) . . . . ?
P2A C17A B1A C43A 155.8(4) . . . . ?
P2A C17A B1A C30A -85.6(5) . . . . ?
P2A C17A B1A C4A 39.0(6) . . . . ?
C11B P1B C4B B1B -155.8(4) . . . . ?
C5B P1B C4B B1B 103.3(4) . . . . ?
Cr1B P1B C4B B1B -27.6(5) . . . . ?
C4B P1B C5B C10B 55.9(6) . . . . ?
C11B P1B C5B C10B -51.5(6) . . . . ?
Cr1B P1B C5B C10B -176.7(4) . . . . ?
C4B P1B C5B C6B -122.7(6) . . . . ?
C11B P1B C5B C6B 130.0(5) . . . . ?
Cr1B P1B C5B C6B 4.7(6) . . . . ?
C10B C5B C6B C7B -1.7(10) . . . . ?
P1B C5B C6B C7B 176.9(5) . . . . ?
C5B C6B C7B C8B 1.4(11) . . . . ?
C6B C7B C8B C9B -1.4(12) . . . . ?
C7B C8B C9B C10B 1.6(13) . . . . ?
C6B C5B C10B C9B 1.9(10) . . . . ?
P1B C5B C10B C9B -176.7(6) . . . . ?
C8B C9B C10B C5B -1.9(12) . . . . ?
C4B P1B C11B C12B 179.1(3) . . . . ?
C5B P1B C11B C12B -77.9(3) . . . . ?
Cr1B P1B C11B C12B 51.0(3) . . . . ?
C4B P1B C11B C16B -6.2(4) . . . . ?
C5B P1B C11B C16B 96.8(3) . . . . ?
Cr1B P1B C11B C16B -134.3(2) . . . . ?
C16B C11B C12B C13B 0.01(10) . . . . ?
P1B C11B C12B C13B 174.9(4) . . . . ?
C11B C12B C13B C14B -0.03(10) . . . . ?
C12B C13B C14B C15B 0.07(10) . . . . ?
C13B C14B C15B C16B -0.08(10) . . . . ?
C12B C11B C16B C15B -0.01(10) . . . . ?
P1B C11B C16B C15B -174.6(4) . . . . ?
C14B C15B C16B C11B 0.04(10) . . . . ?
C24B P2B C17B B1B -166.7(4) . . . . ?
C18B P2B C17B B1B 91.3(5) . . . . ?
Cr1B P2B C17B B1B -37.7(5) . . . . ?
C17B P2B C18B C23B -2.6(6) . . . . ?
C24B P2B C18B C23B -110.2(6) . . . . ?
Cr1B P2B C18B C23B 123.3(5) . . . . ?
C17B P2B C18B C19B 178.6(6) . . . . ?
C24B P2B C18B C19B 71.0(6) . . . . ?
Cr1B P2B C18B C19B -55.6(7) . . . . ?
C23B C18B C19B C20B 1.0(12) . . . . ?
P2B C18B C19B C20B 179.9(7) . . . . ?
C18B C19B C20B C21B -2.0(15) . . . . ?
C19B C20B C21B C22B 2.8(15) . . . . ?
C20B C21B C22B C23B -2.7(13) . . . . ?
C19B C18B C23B C22B -0.9(10) . . . . ?
P2B C18B C23B C22B -179.7(5) . . . . ?
C21B C22B C23B C18B 1.8(11) . . . . ?
C17B P2B C24B C29B -26.0(6) . . . . ?
C18B P2B C24B C29B 80.7(6) . . . . ?
Cr1B P2B C24B C29B -152.4(5) . . . . ?
C17B P2B C24B C25B 158.1(6) . . . . ?
C18B P2B C24B C25B -95.2(7) . . . . ?
Cr1B P2B C24B C25B 31.7(7) . . . . ?
C29B C24B C25B C26B 2.6(13) . . . . ?
P2B C24B C25B C26B 178.7(8) . . . . ?
C24B C25B C26B C27B -2.0(15) . . . . ?
C25B C26B C27B C28B -1.3(15) . . . . ?
C26B C27B C28B C29B 4.2(14) . . . . ?
C27B C28B C29B C24B -3.5(13) . . . . ?
C25B C24B C29B C28B 0.0(11) . . . . ?
P2B C24B C29B C28B -176.0(6) . . . . ?
C37B P3B C30B B1B -164.5(4) . . . . ?
C31B P3B C30B B1B 95.6(4) . . . . ?
Cr1B P3B C30B B1B -36.3(5) . . . . ?
C30B P3B C31B C32B 56.0(6) . . . . ?
C37B P3B C31B C32B -52.3(6) . . . . ?
Cr1B P3B C31B C32B -176.0(4) . . . . ?
C30B P3B C31B C36B -127.1(6) . . . . ?
C37B P3B C31B C36B 124.7(6) . . . . ?
Cr1B P3B C31B C36B 1.0(7) . . . . ?
C36B C31B C32B C33B -0.1(10) . . . . ?
P3B C31B C32B C33B 177.0(6) . . . . ?
C31B C32B C33B C34B -1.1(11) . . . . ?
C32B C33B C34B C35B 1.6(12) . . . . ?
C33B C34B C35B C36B -0.9(11) . . . . ?
C34B C35B C36B C31B -0.3(10) . . . . ?
C32B C31B C36B C35B 0.8(10) . . . . ?
P3B C31B C36B C35B -176.1(5) . . . . ?
C30B P3B C37B C42B 0.6(7) . . . . ?
C31B P3B C37B C42B 105.7(7) . . . . ?
Cr1B P3B C37B C42B -126.8(6) . . . . ?
C30B P3B C37B C38B -177.4(7) . . . . ?
C31B P3B C37B C38B -72.3(7) . . . . ?
Cr1B P3B C37B C38B 55.2(7) . . . . ?
C42B C37B C38B C39B -0.2(15) . . . . ?
P3B C37B C38B C39B 177.9(10) . . . . ?
C37B C38B C39B C40B 3(2) . . . . ?
C38B C39B C40B C41B -4(2) . . . . ?
C39B C40B C41B C42B 3(2) . . . . ?
C38B C37B C42B C41B -1.2(13) . . . . ?
P3B C37B C42B C41B -179.2(8) . . . . ?
C40B C41B C42B C37B 0.1(16) . . . . ?
C48B C43B C44B C45B 2.4(10) . . . . ?
B1B C43B C44B C45B -173.0(6) . . . . ?
W1B C43B C44B C45B 57.1(6) . . . . ?
C48B C43B C44B W1B -54.6(5) . . . . ?
B1B C43B C44B W1B 129.9(6) . . . . ?
C43B C44B C45B C46B -1.7(11) . . . . ?
W1B C44B C45B C46B 56.4(6) . . . . ?
C43B C44B C45B W1B -58.2(6) . . . . ?
C44B C45B C46B C47B 0.6(11) . . . . ?
W1B C45B C46B C47B 57.1(6) . . . . ?
C44B C45B C46B W1B -56.5(6) . . . . ?
C45B C46B C47B C48B -0.4(11) . . . . ?
W1B C46B C47B C48B 57.4(7) . . . . ?
C45B C46B C47B W1B -57.8(6) . . . . ?
C46B C47B C48B C43B 1.2(11) . . . . ?
W1B C47B C48B C43B 58.6(6) . . . . ?
C46B C47B C48B W1B -57.4(7) . . . . ?
C44B C43B C48B C47B -2.2(10) . . . . ?
B1B C43B C48B C47B 173.4(6) . . . . ?
W1B C43B C48B C47B -57.3(6) . . . . ?
C44B C43B C48B W1B 55.1(5) . . . . ?
B1B C43B C48B W1B -129.3(5) . . . . ?
C44B C43B B1B C4B -141.7(6) . . . . ?
C48B C43B B1B C4B 43.0(8) . . . . ?
W1B C43B B1B C4B -47.4(7) . . . . ?
C44B C43B B1B C17B -18.4(8) . . . . ?
C48B C43B B1B C17B 166.3(6) . . . . ?
W1B C43B B1B C17B 75.9(6) . . . . ?
C44B C43B B1B C30B 101.5(7) . . . . ?
C48B C43B B1B C30B -73.7(7) . . . . ?
W1B C43B B1B C30B -164.2(4) . . . . ?
P1B C4B B1B C43B -159.5(4) . . . . ?
P1B C4B B1B C17B 78.8(6) . . . . ?
P1B C4B B1B C30B -46.7(6) . . . . ?
P2B C17B B1B C43B -162.2(4) . . . . ?
P2B C17B B1B C4B -40.1(6) . . . . ?
P2B C17B B1B C30B 83.7(5) . . . . ?
P3B C30B B1B C43B -157.0(4) . . . . ?
P3B C30B B1B C4B 85.9(5) . . . . ?
P3B C30B B1B C17B -39.3(6) . . . . ?
C7C N1C C1C C2C 59.8(12) . . . . ?
C5C N1C C1C C2C -179.1(9) . . . . ?
C3C N1C C1C C2C -59.4(11) . . . . ?
C7C N1C C3C C4C 176.9(9) . . . . ?
C1C N1C C3C C4C -59.0(11) . . . . ?
C5C N1C C3C C4C 59.6(11) . . . . ?
C7C N1C C5C C6C -60.4(11) . . . . ?
C1C N1C C5C C6C 176.0(10) . . . . ?
C3C N1C C5C C6C 54.0(11) . . . . ?
C1C N1C C7C C8C 46.4(12) . . . . ?
C5C N1C C7C C8C -73.3(11) . . . . ?
C3C N1C C7C C8C 169.9(9) . . . . ?
C5D N1D C1D C2D -178.1(7) . . . . ?
C3D N1D C1D C2D 60.1(9) . . . . ?
C7D N1D C1D C2D -57.0(8) . . . . ?
C5D N1D C3D C4D -55.4(10) . . . . ?
C7D N1D C3D C4D -179.0(8) . . . . ?
C1D N1D C3D C4D 62.4(9) . . . . ?
C3D N1D C5D C6D -58.6(9) . . . . ?
C7D N1D C5D C6D 61.9(9) . . . . ?
C1D N1D C5D C6D -178.9(7) . . . . ?
C5D N1D C7D C8D 53.5(9) . . . . ?
C3D N1D C7D C8D 177.3(7) . . . . ?
C1D N1D C7D C8D -63.5(8) . . . . ?

_refine_diff_density_max         1.830
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.091

_shelxl_version_number           2014-3

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.314 0.347 0.264 289 98 ' '
2 -0.314 0.847 0.735 289 98 ' '
_platon_squeeze_details          
;
 The refined structure exhibited two putative THF molecules that had 
 excessively large Uij terms or refined partial occupancies. Both appeared
 overlayed with difference Fourier peaks from other unknown solvents. The
 crystallization included both THF and DEE. No DEE could be identified. 
 Analysis of both void space and refined electrons suggest the possibility
 of additional solvent that is invisible. The empirical formula includes only
 the anions and cations.
 =============================================================================
  
 N: No S.U.'s (esd) on observed/calculated parameters.
 -----------------------------------------------------------------------------
 N: Number of Isotropic Non-H Atoms ....................................    2
 N: Number of moved primary input atoms: ...............................  104
 N: Number of modified (= # ) ATOM labels ..............................   51
 W: Number of unusual anisotropic displacement parameters ..............    1
 N: Total Potential Solvent Accessible Void Vol ...............   580.9 Ang^3
 N: Electron Count / Cell = 196 - To be included in D(calc), F000 & Mol.Wght.
 
 =============================================================================

;

# start Validation Reply Form
_vrf_PLAT733_14169c              
;
PROBLEM: Torsion Calc     -0.1(9), Rep   -0.03(10) ......       9.00 su-Rat
RESPONSE: ... C11B-C12B-C13B-C14B is part of a phenyl ring.
;
_vrf_PLAT330_14169c              
;
PROBLEM: Large Average Phenyl  C-C Dist.  C43A   -C48A          1.42 Ang.  
RESPONSE: ... Phenyl ring pi-bonded to W(CO)3
;
_vrf_PLAT934_14169c              
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          2 Check 
RESPONSE: ... Two much, much worse were excluded. You must draw the line
somewhere. VGY
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Et2O'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_14175b
_database_code_depnum_ccdc_archive 'CCDC 1039157'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        W(CO)3{6-(PhBP3)Mn(CO)3}
_chemical_name_common            14175b
_chemical_melting_point          ?
_chemical_formula_moiety         'C51 H41 B Mn O6 P3 W'
_chemical_formula_sum            'C51 H41 B Mn O6 P3 W'
_chemical_formula_weight         1092.35

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'
B B 0.0013 0.0007 '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'
Mn Mn 0.3368 0.7283 '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/c'
_space_group_name_Hall           '-P 2ybc'

_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.9471(11)
_cell_length_b                   25.023(2)
_cell_length_c                   17.8217(15)
_cell_angle_alpha                90
_cell_angle_beta                 110.161(1)
_cell_angle_gamma                90
_cell_volume                     5419.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2982
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.45

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_F_000             2176
_exptl_transmission_factor_min   0.4006
_exptl_transmission_factor_max   0.4915
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    2.484
_shelx_estimated_absorpt_T_min   0.401
_shelx_estimated_absorpt_T_max   0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4006
_exptl_absorpt_correction_T_max  0.4915
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'

_exptl_special_details           'Prof. P. Fischer'

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.000 632 179 ' '
2 0.500 0.500 0.500 632 179 ' '
_platon_squeeze_details          
;

Summary and Remarks : N = NOTE, W = WARNING, E = ERROR
 =============================================================================

 N: DISORDERED structure ATOMS with Pop. .LT. 1.0 are not moved or as a group.
 -----------------------------------------------------------------------------
 N: Number of moved primary input atoms: ...............................  115
 W: Number of unusual anisotropic displacement parameters ................   1
 N: Total Potential Solvent Accessible Void Vol ................  1270.3 Ang^3
 N: Electron Count / Cell =  358 - To be included in D(calc), F000 & Mol.Wght.

 =============================================================================

 The specimens were grown in DEE/THF/pentane. There are
 channels of disordered solvent of unknown composition.
 The 1270.3 Ang^3 volume could contain 12-14 total molecules of
 these 5-non-hydrogen atom solvents. The refined electron count
 corresponds to about 9 of these solvent molecules.
;


_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62668
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.464
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12411
_reflns_number_gt                10953
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0105P)²+17.8669P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12411
_refine_ls_number_parameters     611
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0803
_refine_ls_wR_factor_gt          0.0788
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.140
_refine_ls_shift/su_max          0.002
_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
W1 W 0.49609(2) 0.29387(2) 0.82814(2) 0.03181(5) Uani 1 1 d . . . . .
Mn1 Mn -0.01990(5) 0.39582(2) 0.82329(3) 0.02441(12) Uani 1 1 d . . . . .
P1 P 0.16091(9) 0.40235(4) 0.91673(5) 0.0283(2) Uani 1 1 d D . . . .
P2 P 0.03882(7) 0.31172(3) 0.79238(5) 0.02108(17) Uani 1 1 d . . . . .
P3 P 0.04292(8) 0.43487(4) 0.72639(5) 0.02383(19) Uani 1 1 d . . . . .
O1 O -0.1264(3) 0.34928(11) 0.93035(17) 0.0415(7) Uani 1 1 d . . . . .
O2 O -0.0933(4) 0.49692(13) 0.8730(2) 0.0849(15) Uani 1 1 d . . . . .
O3 O -0.2485(2) 0.39669(11) 0.71037(17) 0.0364(6) Uani 1 1 d . . . . .
O4 O 0.4944(3) 0.30152(16) 1.00253(18) 0.0567(9) Uani 1 1 d . . . . .
O5 O 0.7313(3) 0.24486(15) 0.8965(2) 0.0539(9) Uani 1 1 d . . . . .
O6 O 0.4068(3) 0.17874(14) 0.83122(19) 0.0554(9) Uani 1 1 d . . . . .
C1 C -0.0779(4) 0.36532(14) 0.8918(2) 0.0324(9) Uani 1 1 d . . . . .
C2 C -0.0595(4) 0.45952(16) 0.8535(2) 0.0458(12) Uani 1 1 d . . . . .
C3 C -0.1578(3) 0.39437(14) 0.7507(2) 0.0271(8) Uani 1 1 d . . . . .
C4 C 0.2635(3) 0.37020(14) 0.8844(2) 0.0283(8) Uani 1 1 d . . . . .
H4A H 0.3337 0.3898 0.9078 0.034 Uiso 1 1 calc R U . . .
H4B H 0.2754 0.3335 0.9066 0.034 Uiso 1 1 calc R U . . .
C5 C 0.2117(4) 0.47018(15) 0.9521(4) 0.0247(14) Uani 0.639(5) 1 d D . P A 1
C6 C 0.1597(4) 0.51739(18) 0.9201(3) 0.0236(12) Uani 0.639(5) 1 d D . P A 1
H6A H 0.0904 0.5163 0.8782 0.028 Uiso 0.639(5) 1 calc R U P A 1
C7 C 0.2077(5) 0.56641(17) 0.9485(4) 0.0315(14) Uani 0.639(5) 1 d D . P A 1
H7A H 0.1706 0.5986 0.9265 0.038 Uiso 0.639(5) 1 calc R U P A 1
C8 C 0.3090(5) 0.56847(19) 1.0087(4) 0.041(2) Uani 0.639(5) 1 d D . P A 1
H8A H 0.3419 0.6020 1.0281 0.049 Uiso 0.639(5) 1 calc R U P A 1
C9 C 0.3620(6) 0.5215(2) 1.0404(5) 0.060(3) Uani 0.639(5) 1 d D . P A 1
H9A H 0.4319 0.5226 1.0816 0.072 Uiso 0.639(5) 1 calc R U P A 1
C10 C 0.3133(5) 0.47263(19) 1.0122(4) 0.0438(19) Uani 0.639(5) 1 d D . P A 1
H10A H 0.3503 0.4405 1.0345 0.053 Uiso 0.639(5) 1 calc R U P A 1
C5' C 0.2337(8) 0.4677(3) 0.9414(8) 0.0247(14) Uani 0.361(5) 1 d D . P A 2
C6' C 0.1898(8) 0.5018(3) 0.9839(7) 0.038(3) Uani 0.361(5) 1 d D . P A 2
H6B H 0.1284 0.4902 0.9973 0.045 Uiso 0.361(5) 1 calc R U P A 2
C7' C 0.2333(10) 0.5523(4) 1.0076(8) 0.047(4) Uani 0.361(5) 1 d D . P A 2
H7B H 0.2013 0.5748 1.0365 0.057 Uiso 0.361(5) 1 calc R U P A 2
C8' C 0.3227(10) 0.5699(3) 0.9892(9) 0.041(2) Uani 0.361(5) 1 d D . P A 2
H8B H 0.3514 0.6048 1.0040 0.049 Uiso 0.361(5) 1 calc R U P A 2
C9' C 0.3698(7) 0.5360(3) 0.9490(6) 0.036(3) Uani 0.361(5) 1 d D . P A 2
H9B H 0.4327 0.5472 0.9373 0.043 Uiso 0.361(5) 1 calc R U P A 2
C10' C 0.3254(7) 0.4857(3) 0.9256(5) 0.028(2) Uani 0.361(5) 1 d D . P A 2
H10B H 0.3588 0.4629 0.8980 0.033 Uiso 0.361(5) 1 calc R U P A 2
C11 C 0.1748(4) 0.37451(14) 1.0149(2) 0.0321(9) Uani 1 1 d . . . . .
C12 C 0.1014(4) 0.39119(15) 1.0518(2) 0.0340(9) Uani 1 1 d . . . . .
H12A H 0.0436 0.4151 1.0247 0.041 Uiso 1 1 calc R U . . .
C13 C 0.1120(4) 0.37323(17) 1.1275(2) 0.0394(10) Uani 1 1 d . . . . .
H13A H 0.0614 0.3848 1.1521 0.047 Uiso 1 1 calc R U . . .
C14 C 0.1955(4) 0.33861(17) 1.1674(2) 0.0449(11) Uani 1 1 d . . . . .
H14A H 0.2027 0.3263 1.2194 0.054 Uiso 1 1 calc R U . . .
C15 C 0.2678(5) 0.32208(17) 1.1319(2) 0.0492(12) Uani 1 1 d . . . . .
H15A H 0.3254 0.2982 1.1595 0.059 Uiso 1 1 calc R U . . .
C16 C 0.2588(4) 0.33971(16) 1.0554(2) 0.0409(10) Uani 1 1 d . . . . .
H16A H 0.3099 0.3279 1.0314 0.049 Uiso 1 1 calc R U . . .
C17 C 0.1427(3) 0.31859(14) 0.7463(2) 0.0231(7) Uani 1 1 d . . . . .
H17A H 0.1817 0.2841 0.7505 0.028 Uiso 1 1 calc R U . . .
H17B H 0.1059 0.3265 0.6887 0.028 Uiso 1 1 calc R U . . .
C18 C 0.0979(3) 0.26431(14) 0.8755(2) 0.0259(7) Uani 1 1 d . . . . .
C19 C 0.0378(3) 0.24969(14) 0.9239(2) 0.0293(8) Uani 1 1 d . . . . .
H19A H -0.0326 0.2651 0.9144 0.035 Uiso 1 1 calc R U . . .
C20 C 0.0786(4) 0.21315(15) 0.9853(2) 0.0340(9) Uani 1 1 d . . . . .
H20A H 0.0366 0.2039 1.0178 0.041 Uiso 1 1 calc R U . . .
C21 C 0.1804(4) 0.19009(16) 0.9992(2) 0.0393(10) Uani 1 1 d . . . . .
H21A H 0.2087 0.1652 1.0415 0.047 Uiso 1 1 calc R U . . .
C22 C 0.2407(3) 0.20329(16) 0.9516(2) 0.0357(9) Uani 1 1 d . . . . .
H22A H 0.3103 0.1870 0.9608 0.043 Uiso 1 1 calc R U . . .
C23 C 0.2003(3) 0.24033(15) 0.8902(2) 0.0293(8) Uani 1 1 d . . . . .
H23A H 0.2429 0.2494 0.8580 0.035 Uiso 1 1 calc R U . . .
C24 C -0.0704(3) 0.26992(13) 0.7254(2) 0.0223(7) Uani 1 1 d . . . . .
C25 C -0.1705(3) 0.26415(14) 0.7381(2) 0.0277(8) Uani 1 1 d . . . . .
H25A H -0.1811 0.2816 0.7822 0.033 Uiso 1 1 calc R U . . .
C26 C -0.2545(3) 0.23340(16) 0.6872(3) 0.0362(9) Uani 1 1 d . . . . .
H26A H -0.3219 0.2296 0.6968 0.043 Uiso 1 1 calc R U . . .
C27 C -0.2400(3) 0.20843(16) 0.6227(3) 0.0367(9) Uani 1 1 d . . . . .
H27A H -0.2980 0.1879 0.5872 0.044 Uiso 1 1 calc R U . . .
C28 C -0.1423(3) 0.21320(15) 0.6098(2) 0.0336(9) Uani 1 1 d . . . . .
H28A H -0.1329 0.1958 0.5652 0.040 Uiso 1 1 calc R U . . .
C29 C -0.0566(3) 0.24324(14) 0.6610(2) 0.0280(8) Uani 1 1 d . . . . .
H29A H 0.0115 0.2456 0.6520 0.034 Uiso 1 1 calc R U . . .
C30 C 0.1879(3) 0.42534(15) 0.7454(2) 0.0312(8) Uani 1 1 d . . . . .
H30A H 0.2019 0.4286 0.6944 0.037 Uiso 1 1 calc R U . . .
H30B H 0.2295 0.4541 0.7814 0.037 Uiso 1 1 calc R U . . .
C31 C -0.0207(3) 0.41303(13) 0.6219(2) 0.0240(7) Uani 1 1 d . . . . .
C32 C -0.1027(3) 0.37474(14) 0.5965(2) 0.0260(7) Uani 1 1 d . . . . .
H32A H -0.1277 0.3576 0.6346 0.031 Uiso 1 1 calc R U . . .
C33 C -0.1492(3) 0.36088(16) 0.5160(2) 0.0321(8) Uani 1 1 d . . . . .
H33A H -0.2057 0.3347 0.4996 0.039 Uiso 1 1 calc R U . . .
C34 C -0.1127(3) 0.38544(16) 0.4603(2) 0.0314(8) Uani 1 1 d . . . . .
H34A H -0.1439 0.3760 0.4054 0.038 Uiso 1 1 calc R U . . .
C35 C -0.0306(3) 0.42372(15) 0.4844(2) 0.0295(8) Uani 1 1 d . . . . .
H35A H -0.0051 0.4404 0.4461 0.035 Uiso 1 1 calc R U . . .
C36 C 0.0142(3) 0.43763(14) 0.5638(2) 0.0271(7) Uani 1 1 d . . . . .
H36A H 0.0696 0.4643 0.5797 0.032 Uiso 1 1 calc R U . . .
C37 C 0.0134(3) 0.50675(14) 0.7130(2) 0.0266(8) Uani 1 1 d . . . . .
C38 C -0.0959(3) 0.52344(16) 0.6792(2) 0.0358(9) Uani 1 1 d . . . . .
H38A H -0.1529 0.4975 0.6630 0.043 Uiso 1 1 calc R U . . .
C39 C -0.1223(4) 0.57702(16) 0.6690(2) 0.0363(9) Uani 1 1 d . . . . .
H39A H -0.1970 0.5877 0.6452 0.044 Uiso 1 1 calc R U . . .
C40 C -0.0407(4) 0.61504(15) 0.6932(2) 0.0362(9) Uani 1 1 d . . . . .
H40A H -0.0591 0.6519 0.6869 0.043 Uiso 1 1 calc R U . . .
C41 C 0.0670(4) 0.59959(16) 0.7263(3) 0.0413(10) Uani 1 1 d . . . . .
H41A H 0.1231 0.6259 0.7426 0.050 Uiso 1 1 calc R U . . .
C42 C 0.0952(4) 0.54539(15) 0.7364(2) 0.0334(9) Uani 1 1 d . . . . .
H42A H 0.1702 0.5351 0.7592 0.040 Uiso 1 1 calc R U . . .
C43 C 0.3469(3) 0.35440(15) 0.7670(2) 0.0297(8) Uani 1 1 d . . . . .
C44 C 0.4461(3) 0.38368(17) 0.8046(2) 0.0378(9) Uani 1 1 d . . . . .
H44A H 0.4480 0.4088 0.8449 0.045 Uiso 1 1 calc R U . . .
C45 C 0.5409(3) 0.37689(19) 0.7844(3) 0.0431(11) Uani 1 1 d . . . . .
H45A H 0.6040 0.3983 0.8092 0.052 Uiso 1 1 calc R U . . .
C46 C 0.5423(4) 0.33804(18) 0.7270(3) 0.0421(10) Uani 1 1 d . . . . .
H46A H 0.6073 0.3322 0.7148 0.051 Uiso 1 1 calc R U . . .
C47 C 0.4473(3) 0.30824(18) 0.6884(2) 0.0371(9) Uani 1 1 d . . . . .
H47A H 0.4463 0.2831 0.6482 0.044 Uiso 1 1 calc R U . . .
C48 C 0.3522(3) 0.31607(16) 0.7099(2) 0.0317(8) Uani 1 1 d . . . . .
H48A H 0.2893 0.2946 0.6848 0.038 Uiso 1 1 calc R U . . .
C49 C 0.4965(3) 0.29836(19) 0.9374(2) 0.0411(10) Uani 1 1 d . . . . .
C50 C 0.6437(4) 0.26312(19) 0.8723(3) 0.0420(10) Uani 1 1 d . . . . .
C51 C 0.4416(4) 0.22134(18) 0.8294(2) 0.0409(10) Uani 1 1 d . . . . .
B1 B 0.2346(3) 0.36628(17) 0.7866(2) 0.0269(8) 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
W1 C49 1.949(4) . ?
W1 C51 1.950(4) . ?
W1 C50 1.957(5) . ?
W1 C44 2.336(4) . ?
W1 C48 2.348(4) . ?
W1 C45 2.360(4) . ?
W1 C46 2.361(4) . ?
W1 C47 2.377(4) . ?
W1 C43 2.401(4) . ?
Mn1 C1 1.809(4) . ?
Mn1 C3 1.809(4) . ?
Mn1 C2 1.812(4) . ?
Mn1 P3 2.3595(10) . ?
Mn1 P1 2.3648(12) . ?
Mn1 P2 2.3662(10) . ?
P1 C4 1.809(4) . ?
P1 C11 1.834(4) . ?
P1 C5 1.851(4) . ?
P1 C5' 1.862(4) . ?
P2 C17 1.809(3) . ?
P2 C24 1.831(3) . ?
P2 C18 1.845(4) . ?
P3 C30 1.805(4) . ?
P3 C37 1.837(4) . ?
P3 C31 1.841(3) . ?
O1 C1 1.150(5) . ?
O2 C2 1.137(5) . ?
O3 C3 1.147(5) . ?
O4 C49 1.173(5) . ?
O5 C50 1.158(5) . ?
O6 C51 1.162(5) . ?
C4 B1 1.655(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.381(4) . ?
C5 C10 1.382(4) . ?
C6 C7 1.389(5) . ?
C6 H6A 0.9500 . ?
C7 C8 1.380(5) . ?
C7 H7A 0.9500 . ?
C8 C9 1.379(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.388(5) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C5' C6' 1.386(4) . ?
C5' C10' 1.386(4) . ?
C6' C7' 1.389(5) . ?
C6' H6B 0.9500 . ?
C7' C8' 1.379(5) . ?
C7' H7B 0.9500 . ?
C8' C9' 1.380(5) . ?
C8' H8B 0.9500 . ?
C9' C10' 1.388(5) . ?
C9' H9B 0.9500 . ?
C10' H10B 0.9500 . ?
C11 C16 1.386(6) . ?
C11 C12 1.393(6) . ?
C12 C13 1.384(5) . ?
C12 H12A 0.9500 . ?
C13 C14 1.377(6) . ?
C13 H13A 0.9500 . ?
C14 C15 1.364(7) . ?
C14 H14A 0.9500 . ?
C15 C16 1.399(5) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 B1 1.664(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.395(5) . ?
C18 C23 1.395(5) . ?
C19 C20 1.384(5) . ?
C19 H19A 0.9500 . ?
C20 C21 1.381(6) . ?
C20 H20A 0.9500 . ?
C21 C22 1.376(6) . ?
C21 H21A 0.9500 . ?
C22 C23 1.392(5) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 C29 1.393(5) . ?
C24 C25 1.397(5) . ?
C25 C26 1.384(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.376(6) . ?
C26 H26A 0.9500 . ?
C27 C28 1.367(6) . ?
C27 H27A 0.9500 . ?
C28 C29 1.389(5) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 B1 1.668(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.385(5) . ?
C31 C36 1.405(5) . ?
C32 C33 1.395(5) . ?
C32 H32A 0.9500 . ?
C33 C34 1.382(5) . ?
C33 H33A 0.9500 . ?
C34 C35 1.385(5) . ?
C34 H34A 0.9500 . ?
C35 C36 1.377(5) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 C42 1.387(5) . ?
C37 C38 1.398(6) . ?
C38 C39 1.380(6) . ?
C38 H38A 0.9500 . ?
C39 C40 1.376(6) . ?
C39 H39A 0.9500 . ?
C40 C41 1.369(6) . ?
C40 H40A 0.9500 . ?
C41 C42 1.400(6) . ?
C41 H41A 0.9500 . ?
C42 H42A 0.9500 . ?
C43 C48 1.417(6) . ?
C43 C44 1.429(5) . ?
C43 B1 1.635(6) . ?
C44 C45 1.402(6) . ?
C44 H44A 0.9500 . ?
C45 C46 1.416(7) . ?
C45 H45A 0.9500 . ?
C46 C47 1.400(6) . ?
C46 H46A 0.9500 . ?
C47 C48 1.424(6) . ?
C47 H47A 0.9500 . ?
C48 H48A 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
C49 W1 C51 85.31(18) . . ?
C49 W1 C50 87.40(18) . . ?
C51 W1 C50 86.36(19) . . ?
C49 W1 C44 91.70(18) . . ?
C51 W1 C44 144.93(17) . . ?
C50 W1 C44 128.48(17) . . ?
C49 W1 C48 127.68(16) . . ?
C51 W1 C48 93.01(15) . . ?
C50 W1 C48 144.79(16) . . ?
C44 W1 C48 61.71(14) . . ?
C49 W1 C45 111.28(18) . . ?
C51 W1 C45 162.56(16) . . ?
C50 W1 C45 99.31(17) . . ?
C44 W1 C45 34.74(15) . . ?
C48 W1 C45 72.82(14) . . ?
C49 W1 C46 145.28(18) . . ?
C51 W1 C46 129.25(17) . . ?
C50 W1 C46 91.25(17) . . ?
C44 W1 C46 62.59(16) . . ?
C48 W1 C46 62.32(14) . . ?
C45 W1 C46 34.91(16) . . ?
C49 W1 C47 161.23(17) . . ?
C51 W1 C47 100.76(15) . . ?
C50 W1 C47 110.56(16) . . ?
C44 W1 C47 73.07(15) . . ?
C48 W1 C47 35.08(13) . . ?
C45 W1 C47 61.80(15) . . ?
C46 W1 C47 34.36(14) . . ?
C49 W1 C43 98.15(16) . . ?
C51 W1 C43 110.77(16) . . ?
C50 W1 C43 162.28(15) . . ?
C44 W1 C43 35.09(12) . . ?
C48 W1 C43 34.71(13) . . ?
C45 W1 C43 62.98(14) . . ?
C46 W1 C43 74.58(14) . . ?
C47 W1 C43 63.08(14) . . ?
C1 Mn1 C3 86.37(17) . . ?
C1 Mn1 C2 86.81(19) . . ?
C3 Mn1 C2 85.39(19) . . ?
C1 Mn1 P3 175.73(13) . . ?
C3 Mn1 P3 89.39(11) . . ?
C2 Mn1 P3 93.31(15) . . ?
C1 Mn1 P1 95.43(13) . . ?
C3 Mn1 P1 177.11(11) . . ?
C2 Mn1 P1 92.44(16) . . ?
P3 Mn1 P1 88.83(4) . . ?
C1 Mn1 P2 91.34(12) . . ?
C3 Mn1 P2 97.64(11) . . ?
C2 Mn1 P2 176.35(14) . . ?
P3 Mn1 P2 88.76(4) . . ?
P1 Mn1 P2 84.60(4) . . ?
C4 P1 C11 107.08(18) . . ?
C4 P1 C5 107.6(2) . . ?
C11 P1 C5 96.7(2) . . ?
C4 P1 C5' 95.6(3) . . ?
C11 P1 C5' 103.5(4) . . ?
C4 P1 Mn1 113.74(12) . . ?
C11 P1 Mn1 113.15(14) . . ?
C5 P1 Mn1 116.90(14) . . ?
C5' P1 Mn1 121.6(4) . . ?
C17 P2 C24 106.63(16) . . ?
C17 P2 C18 104.96(17) . . ?
C24 P2 C18 99.73(15) . . ?
C17 P2 Mn1 111.71(12) . . ?
C24 P2 Mn1 114.95(12) . . ?
C18 P2 Mn1 117.55(12) . . ?
C30 P3 C37 108.05(17) . . ?
C30 P3 C31 102.98(17) . . ?
C37 P3 C31 99.13(15) . . ?
C30 P3 Mn1 113.98(12) . . ?
C37 P3 Mn1 113.08(12) . . ?
C31 P3 Mn1 118.08(12) . . ?
O1 C1 Mn1 171.6(4) . . ?
O2 C2 Mn1 173.1(5) . . ?
O3 C3 Mn1 172.7(3) . . ?
B1 C4 P1 115.9(3) . . ?
B1 C4 H4A 108.3 . . ?
P1 C4 H4A 108.3 . . ?
B1 C4 H4B 108.3 . . ?
P1 C4 H4B 108.3 . . ?
H4A C4 H4B 107.4 . . ?
C6 C5 C10 118.7(4) . . ?
C6 C5 P1 125.3(3) . . ?
C10 C5 P1 115.9(3) . . ?
C5 C6 C7 120.8(4) . . ?
C5 C6 H6A 119.6 . . ?
C7 C6 H6A 119.6 . . ?
C8 C7 C6 120.1(4) . . ?
C8 C7 H7A 119.9 . . ?
C6 C7 H7A 119.9 . . ?
C9 C8 C7 119.5(5) . . ?
C9 C8 H8A 120.3 . . ?
C7 C8 H8A 120.3 . . ?
C8 C9 C10 120.2(4) . . ?
C8 C9 H9A 119.9 . . ?
C10 C9 H9A 119.9 . . ?
C5 C10 C9 120.8(4) . . ?
C5 C10 H10A 119.6 . . ?
C9 C10 H10A 119.6 . . ?
C6' C5' C10' 116.9(5) . . ?
C6' C5' P1 113.6(5) . . ?
C10' C5' P1 129.5(5) . . ?
C5' C6' C7' 121.7(4) . . ?
C5' C6' H6B 119.1 . . ?
C7' C6' H6B 119.1 . . ?
C8' C7' C6' 120.3(5) . . ?
C8' C7' H7B 119.9 . . ?
C6' C7' H7B 119.9 . . ?
C7' C8' C9' 119.0(5) . . ?
C7' C8' H8B 120.5 . . ?
C9' C8' H8B 120.5 . . ?
C8' C9' C10' 120.1(5) . . ?
C8' C9' H9B 120.0 . . ?
C10' C9' H9B 120.0 . . ?
C5' C10' C9' 121.9(4) . . ?
C5' C10' H10B 119.0 . . ?
C9' C10' H10B 119.0 . . ?
C16 C11 C12 118.9(3) . . ?
C16 C11 P1 122.4(3) . . ?
C12 C11 P1 118.6(3) . . ?
C13 C12 C11 120.6(4) . . ?
C13 C12 H12A 119.7 . . ?
C11 C12 H12A 119.7 . . ?
C14 C13 C12 120.3(4) . . ?
C14 C13 H13A 119.9 . . ?
C12 C13 H13A 119.9 . . ?
C15 C14 C13 119.6(4) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
C14 C15 C16 121.2(4) . . ?
C14 C15 H15A 119.4 . . ?
C16 C15 H15A 119.4 . . ?
C11 C16 C15 119.5(4) . . ?
C11 C16 H16A 120.3 . . ?
C15 C16 H16A 120.3 . . ?
B1 C17 P2 113.9(2) . . ?
B1 C17 H17A 108.8 . . ?
P2 C17 H17A 108.8 . . ?
B1 C17 H17B 108.8 . . ?
P2 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C19 C18 C23 117.9(3) . . ?
C19 C18 P2 119.9(3) . . ?
C23 C18 P2 122.1(3) . . ?
C20 C19 C18 121.4(4) . . ?
C20 C19 H19A 119.3 . . ?
C18 C19 H19A 119.3 . . ?
C21 C20 C19 119.9(4) . . ?
C21 C20 H20A 120.1 . . ?
C19 C20 H20A 120.1 . . ?
C22 C21 C20 119.9(4) . . ?
C22 C21 H21A 120.0 . . ?
C20 C21 H21A 120.0 . . ?
C21 C22 C23 120.4(4) . . ?
C21 C22 H22A 119.8 . . ?
C23 C22 H22A 119.8 . . ?
C22 C23 C18 120.6(4) . . ?
C22 C23 H23A 119.7 . . ?
C18 C23 H23A 119.7 . . ?
C29 C24 C25 118.3(3) . . ?
C29 C24 P2 121.4(3) . . ?
C25 C24 P2 120.3(3) . . ?
C26 C25 C24 121.0(3) . . ?
C26 C25 H25A 119.5 . . ?
C24 C25 H25A 119.5 . . ?
C27 C26 C25 119.8(4) . . ?
C27 C26 H26A 120.1 . . ?
C25 C26 H26A 120.1 . . ?
C28 C27 C26 120.1(4) . . ?
C28 C27 H27A 120.0 . . ?
C26 C27 H27A 120.0 . . ?
C27 C28 C29 120.9(4) . . ?
C27 C28 H28A 119.6 . . ?
C29 C28 H28A 119.6 . . ?
C28 C29 C24 120.0(4) . . ?
C28 C29 H29A 120.0 . . ?
C24 C29 H29A 120.0 . . ?
B1 C30 P3 113.3(2) . . ?
B1 C30 H30A 108.9 . . ?
P3 C30 H30A 108.9 . . ?
B1 C30 H30B 108.9 . . ?
P3 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
C32 C31 C36 117.8(3) . . ?
C32 C31 P3 124.1(3) . . ?
C36 C31 P3 118.0(3) . . ?
C31 C32 C33 121.2(3) . . ?
C31 C32 H32A 119.4 . . ?
C33 C32 H32A 119.4 . . ?
C34 C33 C32 119.7(4) . . ?
C34 C33 H33A 120.2 . . ?
C32 C33 H33A 120.2 . . ?
C33 C34 C35 120.0(3) . . ?
C33 C34 H34A 120.0 . . ?
C35 C34 H34A 120.0 . . ?
C36 C35 C34 120.0(3) . . ?
C36 C35 H35A 120.0 . . ?
C34 C35 H35A 120.0 . . ?
C35 C36 C31 121.2(3) . . ?
C35 C36 H36A 119.4 . . ?
C31 C36 H36A 119.4 . . ?
C42 C37 C38 118.4(4) . . ?
C42 C37 P3 122.7(3) . . ?
C38 C37 P3 118.9(3) . . ?
C39 C38 C37 121.0(4) . . ?
C39 C38 H38A 119.5 . . ?
C37 C38 H38A 119.5 . . ?
C40 C39 C38 120.1(4) . . ?
C40 C39 H39A 119.9 . . ?
C38 C39 H39A 119.9 . . ?
C41 C40 C39 119.8(4) . . ?
C41 C40 H40A 120.1 . . ?
C39 C40 H40A 120.1 . . ?
C40 C41 C42 120.7(4) . . ?
C40 C41 H41A 119.6 . . ?
C42 C41 H41A 119.6 . . ?
C37 C42 C41 119.9(4) . . ?
C37 C42 H42A 120.1 . . ?
C41 C42 H42A 120.1 . . ?
C48 C43 C44 115.1(4) . . ?
C48 C43 B1 122.9(3) . . ?
C44 C43 B1 121.9(4) . . ?
C48 C43 W1 70.6(2) . . ?
C44 C43 W1 70.0(2) . . ?
B1 C43 W1 130.8(2) . . ?
C45 C44 C43 122.9(4) . . ?
C45 C44 W1 73.6(3) . . ?
C43 C44 W1 74.9(2) . . ?
C45 C44 H44A 118.6 . . ?
C43 C44 H44A 118.6 . . ?
W1 C44 H44A 124.6 . . ?
C44 C45 C46 119.9(4) . . ?
C44 C45 W1 71.7(2) . . ?
C46 C45 W1 72.6(2) . . ?
C44 C45 H45A 120.0 . . ?
C46 C45 H45A 120.0 . . ?
W1 C45 H45A 127.8 . . ?
C47 C46 C45 119.5(4) . . ?
C47 C46 W1 73.5(2) . . ?
C45 C46 W1 72.5(2) . . ?
C47 C46 H46A 120.2 . . ?
C45 C46 H46A 120.2 . . ?
W1 C46 H46A 125.5 . . ?
C46 C47 C48 119.3(4) . . ?
C46 C47 W1 72.2(2) . . ?
C48 C47 W1 71.4(2) . . ?
C46 C47 H47A 120.4 . . ?
C48 C47 H47A 120.4 . . ?
W1 C47 H47A 128.2 . . ?
C43 C48 C47 123.2(4) . . ?
C43 C48 W1 74.7(2) . . ?
C47 C48 W1 73.6(2) . . ?
C43 C48 H48A 118.4 . . ?
C47 C48 H48A 118.4 . . ?
W1 C48 H48A 125.1 . . ?
O4 C49 W1 178.5(4) . . ?
O5 C50 W1 178.2(4) . . ?
O6 C51 W1 177.9(4) . . ?
C43 B1 C4 109.9(3) . . ?
C43 B1 C17 109.5(3) . . ?
C4 B1 C17 111.5(3) . . ?
C43 B1 C30 106.3(3) . . ?
C4 B1 C30 109.1(3) . . ?
C17 B1 C30 110.4(3) . . ?

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
C11 P1 C4 B1 153.0(3) . . . . ?
C5 P1 C4 B1 -103.9(3) . . . . ?
C5' P1 C4 B1 -101.0(5) . . . . ?
Mn1 P1 C4 B1 27.3(3) . . . . ?
C4 P1 C5 C6 119.3(6) . . . . ?
C11 P1 C5 C6 -130.3(6) . . . . ?
C5' P1 C5 C6 106(3) . . . . ?
Mn1 P1 C5 C6 -10.1(7) . . . . ?
C4 P1 C5 C10 -56.5(6) . . . . ?
C11 P1 C5 C10 53.8(6) . . . . ?
C5' P1 C5 C10 -70(2) . . . . ?
Mn1 P1 C5 C10 174.1(5) . . . . ?
C10 C5 C6 C7 -1.0(10) . . . . ?
P1 C5 C6 C7 -176.7(5) . . . . ?
C5 C6 C7 C8 0.8(10) . . . . ?
C6 C7 C8 C9 -0.1(12) . . . . ?
C7 C8 C9 C10 -0.4(14) . . . . ?
C6 C5 C10 C9 0.5(12) . . . . ?
P1 C5 C10 C9 176.6(7) . . . . ?
C8 C9 C10 C5 0.2(14) . . . . ?
C4 P1 C5' C6' -168.2(10) . . . . ?
C11 P1 C5' C6' -59.1(11) . . . . ?
C5 P1 C5' C6' -1.4(18) . . . . ?
Mn1 P1 C5' C6' 69.4(11) . . . . ?
C4 P1 C5' C10' 9.6(13) . . . . ?
C11 P1 C5' C10' 118.7(12) . . . . ?
C5 P1 C5' C10' 176(4) . . . . ?
Mn1 P1 C5' C10' -112.9(12) . . . . ?
C10' C5' C6' C7' 2(2) . . . . ?
P1 C5' C6' C7' -180.0(11) . . . . ?
C5' C6' C7' C8' 0(2) . . . . ?
C6' C7' C8' C9' -2(2) . . . . ?
C7' C8' C9' C10' 2(2) . . . . ?
C6' C5' C10' C9' -1.9(18) . . . . ?
P1 C5' C10' C9' -179.6(10) . . . . ?
C8' C9' C10' C5' 0.0(18) . . . . ?
C4 P1 C11 C16 6.1(4) . . . . ?
C5 P1 C11 C16 -104.7(4) . . . . ?
C5' P1 C11 C16 -94.3(5) . . . . ?
Mn1 P1 C11 C16 132.2(3) . . . . ?
C4 P1 C11 C12 -177.4(3) . . . . ?
C5 P1 C11 C12 71.8(4) . . . . ?
C5' P1 C11 C12 82.3(4) . . . . ?
Mn1 P1 C11 C12 -51.2(3) . . . . ?
C16 C11 C12 C13 -0.2(6) . . . . ?
P1 C11 C12 C13 -176.9(3) . . . . ?
C11 C12 C13 C14 0.1(6) . . . . ?
C12 C13 C14 C15 0.0(7) . . . . ?
C13 C14 C15 C16 0.1(7) . . . . ?
C12 C11 C16 C15 0.2(6) . . . . ?
P1 C11 C16 C15 176.8(3) . . . . ?
C14 C15 C16 C11 -0.1(7) . . . . ?
C24 P2 C17 B1 166.6(2) . . . . ?
C18 P2 C17 B1 -88.2(3) . . . . ?
Mn1 P2 C17 B1 40.2(3) . . . . ?
C17 P2 C18 C19 -179.6(3) . . . . ?
C24 P2 C18 C19 -69.3(3) . . . . ?
Mn1 P2 C18 C19 55.6(3) . . . . ?
C17 P2 C18 C23 -2.3(3) . . . . ?
C24 P2 C18 C23 108.0(3) . . . . ?
Mn1 P2 C18 C23 -127.1(3) . . . . ?
C23 C18 C19 C20 0.9(5) . . . . ?
P2 C18 C19 C20 178.3(3) . . . . ?
C18 C19 C20 C21 -0.5(6) . . . . ?
C19 C20 C21 C22 -0.4(6) . . . . ?
C20 C21 C22 C23 0.9(6) . . . . ?
C21 C22 C23 C18 -0.5(6) . . . . ?
C19 C18 C23 C22 -0.4(5) . . . . ?
P2 C18 C23 C22 -177.7(3) . . . . ?
C17 P2 C24 C29 10.0(3) . . . . ?
C18 P2 C24 C29 -98.9(3) . . . . ?
Mn1 P2 C24 C29 134.4(3) . . . . ?
C17 P2 C24 C25 -169.8(3) . . . . ?
C18 P2 C24 C25 81.2(3) . . . . ?
Mn1 P2 C24 C25 -45.5(3) . . . . ?
C29 C24 C25 C26 -0.9(5) . . . . ?
P2 C24 C25 C26 178.9(3) . . . . ?
C24 C25 C26 C27 -0.6(6) . . . . ?
C25 C26 C27 C28 1.2(6) . . . . ?
C26 C27 C28 C29 -0.2(6) . . . . ?
C27 C28 C29 C24 -1.4(6) . . . . ?
C25 C24 C29 C28 1.9(5) . . . . ?
P2 C24 C29 C28 -177.9(3) . . . . ?
C37 P3 C30 B1 161.8(3) . . . . ?
C31 P3 C30 B1 -93.9(3) . . . . ?
Mn1 P3 C30 B1 35.2(3) . . . . ?
C30 P3 C31 C32 126.0(3) . . . . ?
C37 P3 C31 C32 -122.9(3) . . . . ?
Mn1 P3 C31 C32 -0.5(4) . . . . ?
C30 P3 C31 C36 -55.6(3) . . . . ?
C37 P3 C31 C36 55.5(3) . . . . ?
Mn1 P3 C31 C36 177.9(2) . . . . ?
C36 C31 C32 C33 0.1(5) . . . . ?
P3 C31 C32 C33 178.5(3) . . . . ?
C31 C32 C33 C34 0.4(6) . . . . ?
C32 C33 C34 C35 -0.2(6) . . . . ?
C33 C34 C35 C36 -0.5(6) . . . . ?
C34 C35 C36 C31 1.0(6) . . . . ?
C32 C31 C36 C35 -0.8(5) . . . . ?
P3 C31 C36 C35 -179.3(3) . . . . ?
C30 P3 C37 C42 -16.2(3) . . . . ?
C31 P3 C37 C42 -123.1(3) . . . . ?
Mn1 P3 C37 C42 110.9(3) . . . . ?
C30 P3 C37 C38 165.0(3) . . . . ?
C31 P3 C37 C38 58.1(3) . . . . ?
Mn1 P3 C37 C38 -67.9(3) . . . . ?
C42 C37 C38 C39 0.2(6) . . . . ?
P3 C37 C38 C39 179.0(3) . . . . ?
C37 C38 C39 C40 -0.9(6) . . . . ?
C38 C39 C40 C41 1.0(6) . . . . ?
C39 C40 C41 C42 -0.4(6) . . . . ?
C38 C37 C42 C41 0.4(5) . . . . ?
P3 C37 C42 C41 -178.4(3) . . . . ?
C40 C41 C42 C37 -0.3(6) . . . . ?
C48 C43 C44 C45 2.6(6) . . . . ?
B1 C43 C44 C45 -175.2(4) . . . . ?
W1 C43 C44 C45 58.5(4) . . . . ?
C48 C43 C44 W1 -55.9(3) . . . . ?
B1 C43 C44 W1 126.3(3) . . . . ?
C43 C44 C45 C46 -2.8(7) . . . . ?
W1 C44 C45 C46 56.3(4) . . . . ?
C43 C44 C45 W1 -59.1(4) . . . . ?
C44 C45 C46 C47 2.7(6) . . . . ?
W1 C45 C46 C47 58.6(4) . . . . ?
C44 C45 C46 W1 -55.9(4) . . . . ?
C45 C46 C47 C48 -2.5(6) . . . . ?
W1 C46 C47 C48 55.6(3) . . . . ?
C45 C46 C47 W1 -58.1(4) . . . . ?
C44 C43 C48 C47 -2.4(5) . . . . ?
B1 C43 C48 C47 175.3(3) . . . . ?
W1 C43 C48 C47 -58.0(3) . . . . ?
C44 C43 C48 W1 55.6(3) . . . . ?
B1 C43 C48 W1 -126.7(3) . . . . ?
C46 C47 C48 C43 2.5(6) . . . . ?
W1 C47 C48 C43 58.5(3) . . . . ?
C46 C47 C48 W1 -56.0(3) . . . . ?
C48 C43 B1 C4 135.4(3) . . . . ?
C44 C43 B1 C4 -47.0(5) . . . . ?
W1 C43 B1 C4 43.3(4) . . . . ?
C48 C43 B1 C17 12.6(5) . . . . ?
C44 C43 B1 C17 -169.8(3) . . . . ?
W1 C43 B1 C17 -79.5(4) . . . . ?
C48 C43 B1 C30 -106.6(4) . . . . ?
C44 C43 B1 C30 71.0(4) . . . . ?
W1 C43 B1 C30 161.3(3) . . . . ?
P1 C4 B1 C43 162.1(2) . . . . ?
P1 C4 B1 C17 -76.3(4) . . . . ?
P1 C4 B1 C30 45.9(4) . . . . ?
P2 C17 B1 C43 158.0(2) . . . . ?
P2 C17 B1 C4 36.1(4) . . . . ?
P2 C17 B1 C30 -85.3(3) . . . . ?
P3 C30 B1 C43 157.9(3) . . . . ?
P3 C30 B1 C4 -83.6(3) . . . . ?
P3 C30 B1 C17 39.2(4) . . . . ?

_refine_diff_density_max         1.937
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.093

_shelxl_version_number           2014-3

# start Validation Reply Form
_vrf_PLAT410_14175b              
;
PROBLEM: Short Intra H...H Contact  H4A    ..  H10B    ..       1.88 Ang.  
RESPONSE: ... H10B is a minor disordered position of the phenyl ring.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Et2O/pentane'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_14176c
_database_code_depnum_ccdc_archive 'CCDC 1039158'
_audit_update_record             
;
2014-12-15 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        Cr(CO)3{6-(PhBP3)Mn(CO)3}
_chemical_name_common            14176c
_chemical_melting_point          552-553
_chemical_formula_moiety         'C51 H41 B Cr Mn O6 P3, C4 H10 O'
_chemical_formula_sum            'C55 H51 B Cr Mn O7 P3'
_chemical_formula_weight         1034.61

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'
B B 0.0013 0.0007 '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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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                   13.0955(15)
_cell_length_b                   16.4800(19)
_cell_length_c                   22.950(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.913(2)
_cell_angle_gamma                90
_cell_volume                     4946.6(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    751
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      14.10
_exptl_crystal_description       Plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_F_000             2144
_exptl_transmission_factor_min   0.6473
_exptl_transmission_factor_max   0.7456
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.625
_shelx_estimated_absorpt_T_min   0.766
_shelx_estimated_absorpt_T_max   0.896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6473
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'

_exptl_special_details           'Prof. P. Fischer'

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56126
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.522
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11225
_reflns_number_gt                8976
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0505P)²+1.4169P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11225
_refine_ls_number_parameters     594
_refine_ls_number_restraints     801
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.1040
_refine_ls_wR_factor_gt          0.0987
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.002
_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
Mn1 Mn 0.25071(2) 0.62755(2) 0.06473(2) 0.02285(8) Uani 1 1 d . U . . .
Cr1 Cr 0.25796(2) 1.00712(2) -0.07236(2) 0.02928(9) Uani 1 1 d . U . . .
P1 P 0.15845(4) 0.68111(3) -0.01685(2) 0.02326(11) Uani 1 1 d . U . . .
P2 P 0.18883(4) 0.73497(3) 0.12256(2) 0.02365(11) Uani 1 1 d D U . . .
P3 P 0.38420(4) 0.71657(3) 0.04018(2) 0.02449(11) Uani 1 1 d D U . . .
O1 O 0.09194(12) 0.50783(9) 0.09103(7) 0.0412(4) Uani 1 1 d . U . . .
O2 O 0.35587(12) 0.54759(10) 0.16594(7) 0.0448(4) Uani 1 1 d . U . . .
O3 O 0.33009(12) 0.48848(9) -0.00023(7) 0.0393(4) Uani 1 1 d . U . . .
O4 O 0.24563(14) 0.87072(10) -0.15834(7) 0.0498(4) Uani 1 1 d . U . . .
O5 O 0.2258(2) 1.10545(14) -0.18009(9) 0.0939(9) Uani 1 1 d . U . . .
O6 O 0.48075(15) 1.00611(17) -0.09216(14) 0.1022(9) Uani 1 1 d . U . . .
C1 C 0.14857(14) 0.55818(12) 0.08088(9) 0.0291(4) Uani 1 1 d . U . . .
C2 C 0.31924(15) 0.58389(12) 0.12748(9) 0.0304(4) Uani 1 1 d . U . . .
C3 C 0.30016(14) 0.54528(12) 0.02224(9) 0.0283(4) Uani 1 1 d . U . . .
C4 C 0.19392(14) 0.78475(11) -0.03231(8) 0.0258(4) Uani 1 1 d . U . . .
H4A H 0.2519 0.7839 -0.0584 0.031 Uiso 1 1 calc R U . . .
H4B H 0.1356 0.8114 -0.0538 0.031 Uiso 1 1 calc R U . . .
C5 C 0.17294(15) 0.62438(12) -0.08472(8) 0.0279(4) Uani 1 1 d . U . . .
C6 C 0.13407(14) 0.54576(12) -0.08893(8) 0.0271(4) Uani 1 1 d . U . . .
H6A H 0.1060 0.5214 -0.0558 0.032 Uiso 1 1 calc R U . . .
C7 C 0.13578(15) 0.50273(12) -0.14065(9) 0.0305(4) Uani 1 1 d . U . . .
H7A H 0.1079 0.4496 -0.1431 0.037 Uiso 1 1 calc R U . . .
C8 C 0.17792(18) 0.53693(13) -0.18859(9) 0.0385(5) Uani 1 1 d . U . . .
H8A H 0.1780 0.5079 -0.2244 0.046 Uiso 1 1 calc R U . . .
C9 C 0.2201(2) 0.61367(15) -0.18439(11) 0.0565(7) Uani 1 1 d . U . . .
H9A H 0.2514 0.6366 -0.2170 0.068 Uiso 1 1 calc R U . . .
C10 C 0.2173(2) 0.65769(14) -0.13263(10) 0.0512(7) Uani 1 1 d . U . . .
H10A H 0.2458 0.7107 -0.1303 0.061 Uiso 1 1 calc R U . . .
C11 C 0.01726(14) 0.68355(11) -0.01786(8) 0.0245(4) Uani 1 1 d . U . . .
C12 C -0.03870(14) 0.66427(11) 0.03014(8) 0.0267(4) Uani 1 1 d . U . . .
H12A H -0.0037 0.6504 0.0660 0.032 Uiso 1 1 calc R U . . .
C13 C -0.14545(15) 0.66496(12) 0.02642(9) 0.0310(4) Uani 1 1 d . U . . .
H13A H -0.1825 0.6518 0.0597 0.037 Uiso 1 1 calc R U . . .
C14 C -0.19734(15) 0.68475(12) -0.02568(10) 0.0338(5) Uani 1 1 d . U . . .
H14A H -0.2700 0.6846 -0.0285 0.041 Uiso 1 1 calc R U . . .
C15 C -0.14270(16) 0.70466(13) -0.07349(9) 0.0358(5) Uani 1 1 d . U . . .
H15A H -0.1780 0.7189 -0.1092 0.043 Uiso 1 1 calc R U . . .
C16 C -0.03660(16) 0.70407(12) -0.06982(9) 0.0314(4) Uani 1 1 d . U . . .
H16A H -0.0001 0.7178 -0.1032 0.038 Uiso 1 1 calc R U . . .
C17 C 0.14759(15) 0.82187(11) 0.07856(8) 0.0273(4) Uani 1 1 d . U . . .
H17A H 0.0781 0.8115 0.0611 0.033 Uiso 1 1 calc R U . . .
H17B H 0.1441 0.8703 0.1039 0.033 Uiso 1 1 calc R U . . .
C18 C 0.08438(14) 0.70537(12) 0.16853(8) 0.0269(4) Uani 1 1 d . U . . .
C19 C 0.09714(16) 0.63749(13) 0.20448(9) 0.0343(5) Uani 1 1 d . U . . .
H19A H 0.1571 0.6054 0.2027 0.041 Uiso 1 1 calc R U . . .
C20 C 0.02290(18) 0.61639(15) 0.24291(9) 0.0414(5) Uani 1 1 d . U . . .
H20A H 0.0322 0.5700 0.2671 0.050 Uiso 1 1 calc R U . . .
C21 C -0.06381(18) 0.66255(15) 0.24588(10) 0.0427(5) Uani 1 1 d . U . . .
H21A H -0.1146 0.6479 0.2721 0.051 Uiso 1 1 calc R U . . .
C22 C -0.07755(17) 0.73018(15) 0.21089(10) 0.0414(5) Uani 1 1 d . U . . .
H22A H -0.1376 0.7621 0.2132 0.050 Uiso 1 1 calc R U . . .
C23 C -0.00377(15) 0.75184(13) 0.17216(9) 0.0328(4) Uani 1 1 d . U . . .
H23A H -0.0136 0.7984 0.1482 0.039 Uiso 1 1 calc R U . . .
C24 C 0.27155(14) 0.78115(11) 0.18155(9) 0.0297(4) Uani 0.807(3) 1 d D U P A 1
C25 C 0.3665(2) 0.75011(16) 0.20141(11) 0.0379(6) Uani 0.807(3) 1 d D U P A 1
H25A H 0.3916 0.7021 0.1842 0.045 Uiso 0.807(3) 1 calc R U P A 1
C26 C 0.4251(2) 0.78800(19) 0.24587(12) 0.0484(8) Uani 0.807(3) 1 d D U P A 1
H26A H 0.4902 0.7666 0.2579 0.058 Uiso 0.807(3) 1 calc R U P A 1
C27 C 0.38914(17) 0.85594(14) 0.27227(10) 0.0497(6) Uani 0.807(3) 1 d D U P A 1
H27A H 0.4303 0.8826 0.3017 0.060 Uiso 0.807(3) 1 calc R U P A 1
C28 C 0.2936(2) 0.88574(18) 0.25640(13) 0.0488(8) Uani 0.807(3) 1 d D U P A 1
H28A H 0.2677 0.9316 0.2760 0.059 Uiso 0.807(3) 1 calc R U P A 1
C29 C 0.2350(2) 0.84862(16) 0.21161(11) 0.0413(7) Uani 0.807(3) 1 d D U P A 1
H29A H 0.1689 0.8694 0.2012 0.050 Uiso 0.807(3) 1 calc R U P A 1
C24' C 0.27155(14) 0.78115(11) 0.18155(9) 0.0297(4) Uani 0.193(3) 1 d D U P A 2
C25' C 0.3306(7) 0.7351(2) 0.2216(3) 0.0379(6) Uani 0.193(3) 1 d D U P A 2
H25B H 0.3315 0.6777 0.2182 0.045 Uiso 0.193(3) 1 calc R U P A 2
C26' C 0.3882(8) 0.7728(2) 0.2666(4) 0.0484(8) Uani 0.193(3) 1 d D U P A 2
H26B H 0.4275 0.7406 0.2937 0.058 Uiso 0.193(3) 1 calc R U P A 2
C27' C 0.38914(17) 0.85594(14) 0.27227(10) 0.0497(6) Uani 0.193(3) 1 d D U P A
2
H27B H 0.4215 0.8811 0.3056 0.060 Uiso 0.193(3) 1 calc R U P A 2
C28' C 0.3421(8) 0.9018(2) 0.2285(3) 0.0488(8) Uani 0.193(3) 1 d D U P A 2
H28B H 0.3504 0.9590 0.2288 0.059 Uiso 0.193(3) 1 calc R U P A 2
C29' C 0.2823(7) 0.8655(2) 0.1838(3) 0.0413(7) Uani 0.193(3) 1 d D U P A 2
H29B H 0.2488 0.8983 0.1546 0.050 Uiso 0.193(3) 1 calc R U P A 2
C30 C 0.34811(15) 0.82208(11) 0.04827(9) 0.0298(4) Uani 1 1 d . U . . .
H30A H 0.3578 0.8377 0.0898 0.036 Uiso 1 1 calc R U . . .
H30B H 0.3939 0.8564 0.0257 0.036 Uiso 1 1 calc R U . . .
C31 C 0.50063(14) 0.69648(12) 0.08536(8) 0.0288(4) Uani 1 1 d . U . . .
C32 C 0.53841(16) 0.61741(14) 0.08911(10) 0.0393(5) Uani 1 1 d . U . . .
H32A H 0.5054 0.5761 0.0662 0.047 Uiso 1 1 calc R U . . .
C33 C 0.62194(16) 0.59747(15) 0.12488(11) 0.0405(5) Uani 1 1 d . U . . .
H33A H 0.6465 0.5432 0.1261 0.049 Uiso 1 1 calc R U . . .
C34 C 0.6693(2) 0.65527(16) 0.15843(12) 0.0543(7) Uani 1 1 d . U . . .
H34A H 0.7241 0.6410 0.1852 0.065 Uiso 1 1 calc R U . . .
C35 C 0.6377(3) 0.73451(18) 0.15365(16) 0.0843(12) Uani 1 1 d . U . . .
H35A H 0.6738 0.7756 0.1752 0.101 Uiso 1 1 calc R U . . .
C36 C 0.5528(2) 0.75510(15) 0.11738(13) 0.0615(8) Uani 1 1 d . U . . .
H36A H 0.5309 0.8100 0.1148 0.074 Uiso 1 1 calc R U . . .
C37 C 0.43926(14) 0.71073(10) -0.03227(8) 0.0272(4) Uani 0.766(4) 1 d D U P B 1
C38 C 0.4715(2) 0.63684(15) -0.05385(12) 0.0378(7) Uani 0.766(4) 1 d D U P B 1
H38A H 0.4603 0.5885 -0.0325 0.045 Uiso 0.766(4) 1 calc R U P B 1
C39 C 0.5200(3) 0.63269(16) -0.10636(13) 0.0449(8) Uani 0.766(4) 1 d D U P B 1
H39A H 0.5395 0.5814 -0.1211 0.054 Uiso 0.766(4) 1 calc R U P B 1
C40 C 0.54016(17) 0.70228(12) -0.13722(10) 0.0428(5) Uani 0.766(4) 1 d D U P B
1
H40A H 0.5741 0.6994 -0.1728 0.051 Uiso 0.766(4) 1 calc R U P B 1
C41 C 0.5101(3) 0.77611(17) -0.11540(12) 0.0454(8) Uani 0.766(4) 1 d D U P B 1
H41A H 0.5232 0.8244 -0.1363 0.054 Uiso 0.766(4) 1 calc R U P B 1
C42 C 0.4608(2) 0.78087(15) -0.06316(11) 0.0360(7) Uani 0.766(4) 1 d D U P B 1
H42A H 0.4417 0.8323 -0.0485 0.043 Uiso 0.766(4) 1 calc R U P B 1
C37' C 0.43926(14) 0.71073(10) -0.03227(8) 0.0272(4) Uani 0.234(4) 1 d D U P B
2
C38' C 0.4224(6) 0.6465(4) -0.0711(3) 0.0378(7) Uani 0.234(4) 1 d D U P B 2
H38B H 0.3744 0.6056 -0.0625 0.045 Uiso 0.234(4) 1 calc R U P B 2
C39' C 0.4746(7) 0.6412(4) -0.1224(3) 0.0449(8) Uani 0.234(4) 1 d D U P B 2
H39B H 0.4649 0.5954 -0.1472 0.054 Uiso 0.234(4) 1 calc R U P B 2
C40' C 0.54016(17) 0.70228(12) -0.13722(10) 0.0428(5) Uani 0.234(4) 1 d D U P B
2
H40B H 0.5736 0.6999 -0.1730 0.051 Uiso 0.234(4) 1 calc R U P B 2
C41' C 0.5569(7) 0.7668(4) -0.0999(3) 0.0454(8) Uani 0.234(4) 1 d D U P B 2
H41B H 0.6040 0.8081 -0.1093 0.054 Uiso 0.234(4) 1 calc R U P B 2
C42' C 0.5052(6) 0.7720(4) -0.0485(3) 0.0360(7) Uani 0.234(4) 1 d D U P B 2
H42B H 0.5152 0.8181 -0.0241 0.043 Uiso 0.234(4) 1 calc R U P B 2
C43 C 0.21322(16) 0.93624(12) 0.00773(8) 0.0295(4) Uani 1 1 d . U . . .
C44 C 0.12469(15) 0.96410(12) -0.02520(9) 0.0304(4) Uani 1 1 d . U . . .
H44A H 0.0743 0.9255 -0.0376 0.036 Uiso 1 1 calc R U . . .
C45 C 0.10851(17) 1.04588(13) -0.04018(10) 0.0374(5) Uani 1 1 d . U . . .
H45A H 0.0480 1.0618 -0.0617 0.045 Uiso 1 1 calc R U . . .
C46 C 0.1830(2) 1.10429(13) -0.02292(10) 0.0428(5) Uani 1 1 d . U . . .
H46A H 0.1733 1.1598 -0.0330 0.051 Uiso 1 1 calc R U . . .
C47 C 0.2708(2) 1.07980(14) 0.00893(11) 0.0488(6) Uani 1 1 d . U . . .
H47A H 0.3212 1.1187 0.0208 0.059 Uiso 1 1 calc R U . . .
C48 C 0.2852(2) 0.99640(12) 0.02378(10) 0.0394(5) Uani 1 1 d . U . . .
H48A H 0.3459 0.9809 0.0454 0.047 Uiso 1 1 calc R U . . .
C49 C 0.24929(16) 0.92150(13) -0.12317(9) 0.0346(5) Uani 1 1 d . U . . .
C50 C 0.2396(2) 1.06854(15) -0.13740(11) 0.0512(6) Uani 1 1 d . U . . .
C51 C 0.3952(2) 1.00652(18) -0.08286(14) 0.0597(7) Uani 1 1 d . U . . .
B1 B 0.22690(17) 0.84034(13) 0.02562(10) 0.0269(4) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 C2 1.807(2) . ?
Mn1 C3 1.809(2) . ?
Mn1 C1 1.812(2) . ?
Mn1 P1 2.3482(6) . ?
Mn1 P3 2.3717(6) . ?
Mn1 P2 2.3794(6) . ?
Cr1 C50 1.809(2) . ?
Cr1 C51 1.826(3) . ?
Cr1 C49 1.830(2) . ?
Cr1 C47 2.216(2) . ?
Cr1 C44 2.216(2) . ?
Cr1 C46 2.220(2) . ?
Cr1 C45 2.220(2) . ?
Cr1 C48 2.224(2) . ?
Cr1 C43 2.2795(19) . ?
P1 C4 1.8098(19) . ?
P1 C5 1.8349(19) . ?
P1 C11 1.8483(19) . ?
P2 C17 1.8185(19) . ?
P2 C18 1.8355(19) . ?
P2 C24 1.854(2) . ?
P3 C30 1.8140(19) . ?
P3 C31 1.830(2) . ?
P3 C37 1.8484(19) . ?
O1 C1 1.145(2) . ?
O2 C2 1.151(2) . ?
O3 C3 1.147(2) . ?
O4 C49 1.162(3) . ?
O5 C50 1.159(3) . ?
O6 C51 1.150(3) . ?
C4 B1 1.654(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.383(3) . ?
C5 C6 1.394(3) . ?
C6 C7 1.384(3) . ?
C6 H6A 0.9500 . ?
C7 C8 1.376(3) . ?
C7 H7A 0.9500 . ?
C8 C9 1.382(3) . ?
C8 H8A 0.9500 . ?
C9 C10 1.394(3) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C12 1.390(3) . ?
C11 C16 1.396(3) . ?
C12 C13 1.396(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.384(3) . ?
C13 H13A 0.9500 . ?
C14 C15 1.380(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.388(3) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 B1 1.666(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C23 1.391(3) . ?
C18 C19 1.395(3) . ?
C19 C20 1.390(3) . ?
C19 H19A 0.9500 . ?
C20 C21 1.371(3) . ?
C20 H20A 0.9500 . ?
C21 C22 1.380(3) . ?
C21 H21A 0.9500 . ?
C22 C23 1.392(3) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C24 C25 1.399(2) . ?
C24 C29 1.405(2) . ?
C25 C26 1.393(3) . ?
C25 H25A 0.9500 . ?
C26 C27 1.368(3) . ?
C26 H26A 0.9500 . ?
C27 C28 1.375(3) . ?
C27 H27A 0.9500 . ?
C28 C29 1.393(3) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C25' C26' 1.393(3) . ?
C25' H25B 0.9500 . ?
C26' H26B 0.9500 . ?
C28' C29' 1.393(3) . ?
C28' H28B 0.9500 . ?
C29' H29B 0.9500 . ?
C30 B1 1.672(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C36 1.374(3) . ?
C31 C32 1.395(3) . ?
C32 C33 1.374(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.355(3) . ?
C33 H33A 0.9500 . ?
C34 C35 1.372(4) . ?
C34 H34A 0.9500 . ?
C35 C36 1.397(4) . ?
C35 H35A 0.9500 . ?
C36 H36A 0.9500 . ?
C37 C38 1.388(2) . ?
C37 C42 1.392(2) . ?
C38 C39 1.392(3) . ?
C38 H38A 0.9500 . ?
C39 C40 1.380(3) . ?
C39 H39A 0.9500 . ?
C40 C41 1.381(3) . ?
C40 H40A 0.9500 . ?
C41 C42 1.393(3) . ?
C41 H41A 0.9500 . ?
C42 H42A 0.9500 . ?
C38' C39' 1.393(3) . ?
C38' H38B 0.9500 . ?
C39' H39B 0.9500 . ?
C41' C42' 1.392(3) . ?
C41' H41B 0.9500 . ?
C42' H42B 0.9500 . ?
C43 C48 1.404(3) . ?
C43 C44 1.427(3) . ?
C43 B1 1.640(3) . ?
C44 C45 1.404(3) . ?
C44 H44A 0.9500 . ?
C45 C46 1.413(3) . ?
C45 H45A 0.9500 . ?
C46 C47 1.390(3) . ?
C46 H46A 0.9500 . ?
C47 C48 1.426(3) . ?
C47 H47A 0.9500 . ?
C48 H48A 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 Mn1 C3 87.38(9) . . ?
C2 Mn1 C1 85.85(9) . . ?
C3 Mn1 C1 85.73(9) . . ?
C2 Mn1 P1 178.36(7) . . ?
C3 Mn1 P1 92.05(6) . . ?
C1 Mn1 P1 92.58(6) . . ?
C2 Mn1 P3 95.36(6) . . ?
C3 Mn1 P3 92.71(6) . . ?
C1 Mn1 P3 177.98(7) . . ?
P1 Mn1 P3 86.20(2) . . ?
C2 Mn1 P2 91.21(7) . . ?
C3 Mn1 P2 178.53(7) . . ?
C1 Mn1 P2 94.56(6) . . ?
P1 Mn1 P2 89.37(2) . . ?
P3 Mn1 P2 87.04(2) . . ?
C50 Cr1 C51 89.11(13) . . ?
C50 Cr1 C49 84.51(11) . . ?
C51 Cr1 C49 86.64(12) . . ?
C50 Cr1 C47 113.16(10) . . ?
C51 Cr1 C47 94.64(12) . . ?
C49 Cr1 C47 162.28(9) . . ?
C50 Cr1 C44 120.46(11) . . ?
C51 Cr1 C44 150.19(11) . . ?
C49 Cr1 C44 92.27(8) . . ?
C47 Cr1 C44 77.86(9) . . ?
C50 Cr1 C46 88.54(10) . . ?
C51 Cr1 C46 122.34(12) . . ?
C49 Cr1 C46 150.12(10) . . ?
C47 Cr1 C46 36.52(9) . . ?
C44 Cr1 C46 66.53(8) . . ?
C50 Cr1 C45 91.79(10) . . ?
C51 Cr1 C45 159.35(12) . . ?
C49 Cr1 C45 113.98(9) . . ?
C47 Cr1 C45 66.10(10) . . ?
C44 Cr1 C45 36.90(7) . . ?
C46 Cr1 C45 37.12(9) . . ?
C50 Cr1 C48 150.54(10) . . ?
C51 Cr1 C48 91.20(12) . . ?
C49 Cr1 C48 124.92(9) . . ?
C47 Cr1 C48 37.47(8) . . ?
C44 Cr1 C48 65.21(9) . . ?
C46 Cr1 C48 66.61(8) . . ?
C45 Cr1 C48 78.03(9) . . ?
C50 Cr1 C43 157.39(11) . . ?
C51 Cr1 C43 113.50(11) . . ?
C49 Cr1 C43 96.23(8) . . ?
C47 Cr1 C43 67.03(8) . . ?
C44 Cr1 C43 36.99(7) . . ?
C46 Cr1 C43 79.57(8) . . ?
C45 Cr1 C43 67.18(7) . . ?
C48 Cr1 C43 36.31(8) . . ?
C4 P1 C5 106.00(9) . . ?
C4 P1 C11 104.10(9) . . ?
C5 P1 C11 98.45(9) . . ?
C4 P1 Mn1 112.60(7) . . ?
C5 P1 Mn1 114.46(6) . . ?
C11 P1 Mn1 119.47(6) . . ?
C17 P2 C18 108.63(9) . . ?
C17 P2 C24 103.19(9) . . ?
C18 P2 C24 96.55(8) . . ?
C17 P2 Mn1 112.09(6) . . ?
C18 P2 Mn1 114.07(7) . . ?
C24 P2 Mn1 120.66(6) . . ?
C30 P3 C31 109.23(10) . . ?
C30 P3 C37 104.92(8) . . ?
C31 P3 C37 98.53(8) . . ?
C30 P3 Mn1 111.69(6) . . ?
C31 P3 Mn1 110.89(6) . . ?
C37 P3 Mn1 120.49(6) . . ?
O1 C1 Mn1 172.53(17) . . ?
O2 C2 Mn1 171.52(19) . . ?
O3 C3 Mn1 173.50(18) . . ?
B1 C4 P1 115.10(13) . . ?
B1 C4 H4A 108.5 . . ?
P1 C4 H4A 108.5 . . ?
B1 C4 H4B 108.5 . . ?
P1 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
C10 C5 C6 118.72(19) . . ?
C10 C5 P1 122.58(16) . . ?
C6 C5 P1 118.64(14) . . ?
C7 C6 C5 120.93(18) . . ?
C7 C6 H6A 119.5 . . ?
C5 C6 H6A 119.5 . . ?
C8 C7 C6 120.04(19) . . ?
C8 C7 H7A 120.0 . . ?
C6 C7 H7A 120.0 . . ?
C7 C8 C9 119.6(2) . . ?
C7 C8 H8A 120.2 . . ?
C9 C8 H8A 120.2 . . ?
C8 C9 C10 120.5(2) . . ?
C8 C9 H9A 119.7 . . ?
C10 C9 H9A 119.7 . . ?
C5 C10 C9 120.1(2) . . ?
C5 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C12 C11 C16 117.93(18) . . ?
C12 C11 P1 123.52(14) . . ?
C16 C11 P1 118.54(14) . . ?
C11 C12 C13 121.06(18) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C14 C13 C12 120.06(19) . . ?
C14 C13 H13A 120.0 . . ?
C12 C13 H13A 120.0 . . ?
C15 C14 C13 119.44(19) . . ?
C15 C14 H14A 120.3 . . ?
C13 C14 H14A 120.3 . . ?
C14 C15 C16 120.54(19) . . ?
C14 C15 H15A 119.7 . . ?
C16 C15 H15A 119.7 . . ?
C15 C16 C11 120.96(19) . . ?
C15 C16 H16A 119.5 . . ?
C11 C16 H16A 119.5 . . ?
B1 C17 P2 111.73(13) . . ?
B1 C17 H17A 109.3 . . ?
P2 C17 H17A 109.3 . . ?
B1 C17 H17B 109.3 . . ?
P2 C17 H17B 109.3 . . ?
H17A C17 H17B 107.9 . . ?
C23 C18 C19 118.74(18) . . ?
C23 C18 P2 122.21(15) . . ?
C19 C18 P2 118.86(15) . . ?
C20 C19 C18 120.6(2) . . ?
C20 C19 H19A 119.7 . . ?
C18 C19 H19A 119.7 . . ?
C21 C20 C19 120.0(2) . . ?
C21 C20 H20A 120.0 . . ?
C19 C20 H20A 120.0 . . ?
C20 C21 C22 120.2(2) . . ?
C20 C21 H21A 119.9 . . ?
C22 C21 H21A 119.9 . . ?
C21 C22 C23 120.3(2) . . ?
C21 C22 H22A 119.9 . . ?
C23 C22 H22A 119.9 . . ?
C18 C23 C22 120.1(2) . . ?
C18 C23 H23A 119.9 . . ?
C22 C23 H23A 119.9 . . ?
C25 C24 C29 116.6(2) . . ?
C25 C24 P2 124.36(15) . . ?
C29 C24 P2 118.85(14) . . ?
C26 C25 C24 121.5(2) . . ?
C26 C25 H25A 119.3 . . ?
C24 C25 H25A 119.3 . . ?
C27 C26 C25 120.2(2) . . ?
C27 C26 H26A 119.9 . . ?
C25 C26 H26A 119.9 . . ?
C26 C27 C28 120.2(2) . . ?
C26 C27 H27A 119.9 . . ?
C28 C27 H27A 119.9 . . ?
C27 C28 C29 119.9(2) . . ?
C27 C28 H28A 120.1 . . ?
C29 C28 H28A 120.1 . . ?
C28 C29 C24 121.4(2) . . ?
C28 C29 H29A 119.3 . . ?
C24 C29 H29A 119.3 . . ?
C26' C25' H25B 119.8 . . ?
C25' C26' H26B 119.4 . . ?
C29' C28' H28B 119.5 . . ?
C28' C29' H29B 119.8 . . ?
B1 C30 P3 112.88(13) . . ?
B1 C30 H30A 109.0 . . ?
P3 C30 H30A 109.0 . . ?
B1 C30 H30B 109.0 . . ?
P3 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
C36 C31 C32 117.3(2) . . ?
C36 C31 P3 123.57(17) . . ?
C32 C31 P3 119.12(16) . . ?
C33 C32 C31 122.0(2) . . ?
C33 C32 H32A 119.0 . . ?
C31 C32 H32A 119.0 . . ?
C34 C33 C32 119.9(2) . . ?
C34 C33 H33A 120.0 . . ?
C32 C33 H33A 120.0 . . ?
C33 C34 C35 119.7(2) . . ?
C33 C34 H34A 120.1 . . ?
C35 C34 H34A 120.1 . . ?
C34 C35 C36 120.4(3) . . ?
C34 C35 H35A 119.8 . . ?
C36 C35 H35A 119.8 . . ?
C31 C36 C35 120.5(2) . . ?
C31 C36 H36A 119.8 . . ?
C35 C36 H36A 119.8 . . ?
C38 C37 C42 118.3(2) . . ?
C38 C37 P3 120.40(14) . . ?
C42 C37 P3 120.88(14) . . ?
C37 C38 C39 120.8(2) . . ?
C37 C38 H38A 119.6 . . ?
C39 C38 H38A 119.6 . . ?
C40 C39 C38 120.7(2) . . ?
C40 C39 H39A 119.6 . . ?
C38 C39 H39A 119.6 . . ?
C39 C40 C41 118.7(2) . . ?
C39 C40 H40A 120.6 . . ?
C41 C40 H40A 120.6 . . ?
C40 C41 C42 121.0(2) . . ?
C40 C41 H41A 119.5 . . ?
C42 C41 H41A 119.5 . . ?
C37 C42 C41 120.4(2) . . ?
C37 C42 H42A 119.8 . . ?
C41 C42 H42A 119.8 . . ?
C39' C38' H38B 119.3 . . ?
C38' C39' H39B 119.9 . . ?
C42' C41' H41B 119.8 . . ?
C41' C42' H42B 119.4 . . ?
C48 C43 C44 115.36(18) . . ?
C48 C43 B1 123.45(19) . . ?
C44 C43 B1 121.19(18) . . ?
C48 C43 Cr1 69.70(12) . . ?
C44 C43 Cr1 69.10(11) . . ?
B1 C43 Cr1 131.78(13) . . ?
C45 C44 C43 123.1(2) . . ?
C45 C44 Cr1 71.71(12) . . ?
C43 C44 Cr1 73.91(11) . . ?
C45 C44 H44A 118.4 . . ?
C43 C44 H44A 118.4 . . ?
Cr1 C44 H44A 128.4 . . ?
C44 C45 C46 119.4(2) . . ?
C44 C45 Cr1 71.39(11) . . ?
C46 C45 Cr1 71.42(13) . . ?
C44 C45 H45A 120.3 . . ?
C46 C45 H45A 120.3 . . ?
Cr1 C45 H45A 129.2 . . ?
C47 C46 C45 119.4(2) . . ?
C47 C46 Cr1 71.60(14) . . ?
C45 C46 Cr1 71.47(12) . . ?
C47 C46 H46A 120.3 . . ?
C45 C46 H46A 120.3 . . ?
Cr1 C46 H46A 128.9 . . ?
C46 C47 C48 120.1(2) . . ?
C46 C47 Cr1 71.88(14) . . ?
C48 C47 Cr1 71.57(13) . . ?
C46 C47 H47A 120.0 . . ?
C48 C47 H47A 120.0 . . ?
Cr1 C47 H47A 128.9 . . ?
C43 C48 C47 122.6(2) . . ?
C43 C48 Cr1 73.99(12) . . ?
C47 C48 Cr1 70.96(13) . . ?
C43 C48 H48A 118.7 . . ?
C47 C48 H48A 118.7 . . ?
Cr1 C48 H48A 128.8 . . ?
O4 C49 Cr1 175.40(18) . . ?
O5 C50 Cr1 177.4(3) . . ?
O6 C51 Cr1 176.9(3) . . ?
C43 B1 C4 108.17(16) . . ?
C43 B1 C17 107.12(15) . . ?
C4 B1 C17 109.76(16) . . ?
C43 B1 C30 109.93(16) . . ?
C4 B1 C30 110.80(15) . . ?
C17 B1 C30 110.95(16) . . ?

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
C5 P1 C4 B1 -159.21(13) . . . . ?
C11 P1 C4 B1 97.51(14) . . . . ?
Mn1 P1 C4 B1 -33.33(15) . . . . ?
C4 P1 C5 C10 8.4(2) . . . . ?
C11 P1 C5 C10 115.8(2) . . . . ?
Mn1 P1 C5 C10 -116.4(2) . . . . ?
C4 P1 C5 C6 -169.00(15) . . . . ?
C11 P1 C5 C6 -61.61(17) . . . . ?
Mn1 P1 C5 C6 66.27(17) . . . . ?
C10 C5 C6 C7 -2.6(3) . . . . ?
P1 C5 C6 C7 174.87(15) . . . . ?
C5 C6 C7 C8 1.2(3) . . . . ?
C6 C7 C8 C9 1.2(3) . . . . ?
C7 C8 C9 C10 -2.2(4) . . . . ?
C6 C5 C10 C9 1.7(4) . . . . ?
P1 C5 C10 C9 -175.7(2) . . . . ?
C8 C9 C10 C5 0.7(5) . . . . ?
C4 P1 C11 C12 -118.62(16) . . . . ?
C5 P1 C11 C12 132.43(16) . . . . ?
Mn1 P1 C11 C12 8.04(18) . . . . ?
C4 P1 C11 C16 62.84(17) . . . . ?
C5 P1 C11 C16 -46.11(17) . . . . ?
Mn1 P1 C11 C16 -170.50(13) . . . . ?
C16 C11 C12 C13 0.4(3) . . . . ?
P1 C11 C12 C13 -178.19(15) . . . . ?
C11 C12 C13 C14 0.2(3) . . . . ?
C12 C13 C14 C15 -0.8(3) . . . . ?
C13 C14 C15 C16 0.7(3) . . . . ?
C14 C15 C16 C11 -0.1(3) . . . . ?
C12 C11 C16 C15 -0.4(3) . . . . ?
P1 C11 C16 C15 178.20(16) . . . . ?
C18 P2 C17 B1 -167.65(13) . . . . ?
C24 P2 C17 B1 90.66(14) . . . . ?
Mn1 P2 C17 B1 -40.68(15) . . . . ?
C17 P2 C18 C23 -7.76(19) . . . . ?
C24 P2 C18 C23 98.57(17) . . . . ?
Mn1 P2 C18 C23 -133.59(15) . . . . ?
C17 P2 C18 C19 177.35(16) . . . . ?
C24 P2 C18 C19 -76.32(17) . . . . ?
Mn1 P2 C18 C19 51.52(17) . . . . ?
C23 C18 C19 C20 0.4(3) . . . . ?
P2 C18 C19 C20 175.48(17) . . . . ?
C18 C19 C20 C21 -0.2(3) . . . . ?
C19 C20 C21 C22 -0.2(4) . . . . ?
C20 C21 C22 C23 0.3(3) . . . . ?
C19 C18 C23 C22 -0.3(3) . . . . ?
P2 C18 C23 C22 -175.21(16) . . . . ?
C21 C22 C23 C18 0.0(3) . . . . ?
C17 P2 C24 C25 -135.6(2) . . . . ?
C18 P2 C24 C25 113.5(2) . . . . ?
Mn1 P2 C24 C25 -9.5(2) . . . . ?
C17 P2 C24 C29 49.0(2) . . . . ?
C18 P2 C24 C29 -61.9(2) . . . . ?
Mn1 P2 C24 C29 175.00(17) . . . . ?
C29 C24 C25 C26 -4.7(4) . . . . ?
P2 C24 C25 C26 179.8(2) . . . . ?
C24 C25 C26 C27 1.7(4) . . . . ?
C25 C26 C27 C28 2.1(5) . . . . ?
C26 C27 C28 C29 -2.7(5) . . . . ?
C27 C28 C29 C24 -0.5(5) . . . . ?
C25 C24 C29 C28 4.1(4) . . . . ?
P2 C24 C29 C28 179.9(2) . . . . ?
C31 P3 C30 B1 -162.80(13) . . . . ?
C37 P3 C30 B1 92.40(14) . . . . ?
Mn1 P3 C30 B1 -39.76(15) . . . . ?
C30 P3 C31 C36 -3.0(2) . . . . ?
C37 P3 C31 C36 106.2(2) . . . . ?
Mn1 P3 C31 C36 -126.5(2) . . . . ?
C30 P3 C31 C32 175.51(16) . . . . ?
C37 P3 C31 C32 -75.35(17) . . . . ?
Mn1 P3 C31 C32 51.99(18) . . . . ?
C36 C31 C32 C33 2.4(3) . . . . ?
P3 C31 C32 C33 -176.13(18) . . . . ?
C31 C32 C33 C34 0.9(4) . . . . ?
C32 C33 C34 C35 -4.3(4) . . . . ?
C33 C34 C35 C36 4.3(6) . . . . ?
C32 C31 C36 C35 -2.4(4) . . . . ?
P3 C31 C36 C35 176.1(3) . . . . ?
C34 C35 C36 C31 -1.0(6) . . . . ?
C30 P3 C37 C38 -177.4(2) . . . . ?
C31 P3 C37 C38 70.0(2) . . . . ?
Mn1 P3 C37 C38 -50.4(2) . . . . ?
C30 P3 C37 C42 10.5(2) . . . . ?
C31 P3 C37 C42 -102.1(2) . . . . ?
Mn1 P3 C37 C42 137.4(2) . . . . ?
C42 C37 C38 C39 -2.8(4) . . . . ?
P3 C37 C38 C39 -175.2(2) . . . . ?
C37 C38 C39 C40 2.1(5) . . . . ?
C38 C39 C40 C41 -0.8(5) . . . . ?
C39 C40 C41 C42 0.3(5) . . . . ?
C38 C37 C42 C41 2.3(4) . . . . ?
P3 C37 C42 C41 174.6(2) . . . . ?
C40 C41 C42 C37 -1.1(5) . . . . ?
C48 C43 C44 C45 -1.0(3) . . . . ?
B1 C43 C44 C45 178.29(18) . . . . ?
Cr1 C43 C44 C45 -54.66(17) . . . . ?
C48 C43 C44 Cr1 53.71(17) . . . . ?
B1 C43 C44 Cr1 -127.05(17) . . . . ?
C43 C44 C45 C46 0.8(3) . . . . ?
Cr1 C44 C45 C46 -54.81(18) . . . . ?
C43 C44 C45 Cr1 55.64(17) . . . . ?
C44 C45 C46 C47 -0.4(3) . . . . ?
Cr1 C45 C46 C47 -55.2(2) . . . . ?
C44 C45 C46 Cr1 54.80(17) . . . . ?
C45 C46 C47 C48 0.2(4) . . . . ?
Cr1 C46 C47 C48 -55.0(2) . . . . ?
C45 C46 C47 Cr1 55.1(2) . . . . ?
C44 C43 C48 C47 0.7(3) . . . . ?
B1 C43 C48 C47 -178.5(2) . . . . ?
Cr1 C43 C48 C47 54.1(2) . . . . ?
C44 C43 C48 Cr1 -53.40(16) . . . . ?
B1 C43 C48 Cr1 127.37(18) . . . . ?
C46 C47 C48 C43 -0.3(4) . . . . ?
Cr1 C47 C48 C43 -55.5(2) . . . . ?
C46 C47 C48 Cr1 55.1(2) . . . . ?
C48 C43 B1 C4 -136.4(2) . . . . ?
C44 C43 B1 C4 44.4(2) . . . . ?
Cr1 C43 B1 C4 -44.6(2) . . . . ?
C48 C43 B1 C17 105.3(2) . . . . ?
C44 C43 B1 C17 -73.9(2) . . . . ?
Cr1 C43 B1 C17 -162.82(14) . . . . ?
C48 C43 B1 C30 -15.3(3) . . . . ?
C44 C43 B1 C30 165.49(17) . . . . ?
Cr1 C43 B1 C30 76.5(2) . . . . ?
P1 C4 B1 C43 -158.43(13) . . . . ?
P1 C4 B1 C17 -41.87(19) . . . . ?
P1 C4 B1 C30 81.01(17) . . . . ?
P2 C17 B1 C43 -156.53(14) . . . . ?
P2 C17 B1 C4 86.26(17) . . . . ?
P2 C17 B1 C30 -36.5(2) . . . . ?
P3 C30 B1 C43 -155.98(13) . . . . ?
P3 C30 B1 C4 -36.47(19) . . . . ?
P3 C30 B1 C17 85.72(17) . . . . ?

_refine_diff_density_max         0.473
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.056

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.093 0.056 0.188 167 42 ' '
2 -0.093 -0.056 0.812 167 42 ' '
3 0.062 0.583 0.700 10 0 ' '
4 0.407 0.556 0.312 167 42 ' '
5 0.593 0.444 0.688 167 42 ' '
6 0.438 0.083 0.800 10 0 ' '
7 0.562 0.917 0.200 10 0 ' '
8 0.938 0.417 0.300 10 0 ' '
_platon_squeeze_details          
;
 
Summary and Remarks : N = NOTE, W = WARNING, E = ERROR
 =============================================================================
 
 N: No S.U.'s (esd) on observed/calculated parameters.
 -----------------------------------------------------------------------------
 N: Number of Isotropic Non-H Atoms ....................................    1
 N: Number of moved primary input atoms: ...............................  104
 N: Total Potential Solvent Accessible Void Vol ...............   712.9 Ang^3
 N: Electron Count / Cell  169 - To be included in D(calc), F000 & Mol.Wght.
 
 =============================================================================
 
 The solvent, either DEE and/or pentane, was located but refined very poorly 
 with huge Uijs. PLATON/SQUEEZE applied prior to disorder modeling of two
 phenyl groups. The void volume and refined electons support this model.

;

# start Validation Reply Form
_vrf_CHEMW03_14176c              
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: ... PLATON/SQUEEZE applied to treat a disordered DEE and/or pentane
The formula was left with 100% DEE however this could be an admixture.
;
_vrf_PLAT410_14176c              
;
PROBLEM: Short Intra H...H Contact  H17B   ..  H29B    ..       1.81 Ang.  
RESPONSE: ... C29 is part of a disordered phenyl group.
;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Et2O/pentane'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
