# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1578538'
_audit_update_record             
;
2017-10-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H31 P3'
_chemical_formula_sum            'C33 H31 P3'
_chemical_formula_weight         520.49

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   9.845(2)
_cell_length_b                   11.647(2)
_cell_length_c                   13.057(3)
_cell_angle_alpha                96.65(3)
_cell_angle_beta                 106.37(3)
_cell_angle_gamma                101.39(3)
_cell_volume                     1384.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    9744
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      28.56

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_F_000             548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.774
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.235
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_process_details   'TWINABS; Bruker, 2015'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11922
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.086
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11922
_reflns_number_gt                10991
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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, SADABS and XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component perfect twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0348P)²+1.0339P] 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         11922
_refine_ls_number_parameters     328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.0975
_refine_ls_wR_factor_gt          0.0931
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_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
P1 P 0.18490(5) 0.22814(4) 0.27319(4) 0.01356(10) Uani 1 1 d . . . . .
P2 P 0.16052(5) 0.15618(5) 0.41153(4) 0.01833(11) Uani 1 1 d . . . . .
P3 P -0.06050(5) 0.16830(4) 0.36696(4) 0.01379(10) Uani 1 1 d . . . . .
C1 C 0.03288(19) 0.28606(16) 0.22397(14) 0.0145(3) Uani 1 1 d . . . . .
C2 C -0.0802(2) 0.26046(16) 0.27126(14) 0.0148(3) Uani 1 1 d . . . . .
C3 C -0.1964(2) 0.30376(16) 0.21359(15) 0.0164(4) Uani 1 1 d . . . . .
H3 H -0.286961 0.298608 0.227437 0.020 Uiso 1 1 calc R U . . .
C4 C -0.1558(2) 0.35601(16) 0.13186(14) 0.0146(4) Uani 1 1 d . . . . .
C5 C -0.01429(19) 0.34488(16) 0.13807(14) 0.0149(3) Uani 1 1 d . . . . .
H5 H 0.039674 0.372419 0.092091 0.018 Uiso 1 1 calc R U . . .
C41 C -0.2491(2) 0.41556(17) 0.05237(15) 0.0173(4) Uani 1 1 d . . . . .
C42 C -0.2060(3) 0.55045(19) 0.09089(19) 0.0300(5) Uani 1 1 d . . . . .
H42A H -0.220414 0.569025 0.161643 0.045 Uiso 1 1 calc R U . . .
H42B H -0.266698 0.587781 0.038180 0.045 Uiso 1 1 calc R U . . .
H42C H -0.103108 0.581065 0.097563 0.045 Uiso 1 1 calc R U . . .
C43 C -0.4101(2) 0.3691(2) 0.04123(19) 0.0286(5) Uani 1 1 d . . . . .
H43A H -0.436462 0.281944 0.022865 0.043 Uiso 1 1 calc R U . . .
H43B H -0.470340 0.401393 -0.016361 0.043 Uiso 1 1 calc R U . . .
H43C H -0.426690 0.394310 0.110034 0.043 Uiso 1 1 calc R U . . .
C44 C -0.2299(2) 0.3875(2) -0.05920(16) 0.0251(4) Uani 1 1 d . . . . .
H44A H -0.127199 0.416904 -0.053715 0.038 Uiso 1 1 calc R U . . .
H44B H -0.290388 0.426509 -0.110363 0.038 Uiso 1 1 calc R U . . .
H44C H -0.259635 0.301183 -0.085082 0.038 Uiso 1 1 calc R U . . .
C111 C 0.3525(2) 0.34187(17) 0.31578(15) 0.0162(4) Uani 1 1 d . . . . .
C112 C 0.4854(2) 0.3127(2) 0.35402(18) 0.0271(5) Uani 1 1 d . . . . .
H112 H 0.489265 0.231634 0.351528 0.033 Uiso 1 1 calc R U . . .
C113 C 0.6125(2) 0.4021(2) 0.3958(2) 0.0340(5) Uani 1 1 d . . . . .
H113 H 0.703544 0.382298 0.422578 0.041 Uiso 1 1 calc R U . . .
C114 C 0.6073(2) 0.5198(2) 0.39871(19) 0.0318(5) Uani 1 1 d . . . . .
H114 H 0.694774 0.580934 0.427158 0.038 Uiso 1 1 calc R U . . .
C115 C 0.4763(2) 0.5489(2) 0.36068(19) 0.0310(5) Uani 1 1 d . . . . .
H115 H 0.473096 0.630051 0.362553 0.037 Uiso 1 1 calc R U . . .
C116 C 0.3484(2) 0.46014(18) 0.31947(17) 0.0238(4) Uani 1 1 d . . . . .
H116 H 0.257587 0.480640 0.293691 0.029 Uiso 1 1 calc R U . . .
C121 C 0.2025(2) 0.12081(17) 0.16835(15) 0.0172(4) Uani 1 1 d . . . . .
C122 C 0.1309(2) 0.00250(18) 0.15411(17) 0.0228(4) Uani 1 1 d . . . . .
H122 H 0.080499 -0.022949 0.202832 0.027 Uiso 1 1 calc R U . . .
C123 C 0.1330(2) -0.07884(19) 0.06854(18) 0.0268(5) Uani 1 1 d . . . . .
H123 H 0.082805 -0.159877 0.058453 0.032 Uiso 1 1 calc R U . . .
C124 C 0.2070(2) -0.0435(2) -0.00202(18) 0.0305(5) Uani 1 1 d . . . . .
H124 H 0.209081 -0.099913 -0.059869 0.037 Uiso 1 1 calc R U . . .
C125 C 0.2775(3) 0.0737(2) 0.0118(2) 0.0355(6) Uani 1 1 d . . . . .
H125 H 0.327949 0.098619 -0.037037 0.043 Uiso 1 1 calc R U . . .
C126 C 0.2758(2) 0.1565(2) 0.09699(18) 0.0275(5) Uani 1 1 d . . . . .
H126 H 0.325139 0.237625 0.106147 0.033 Uiso 1 1 calc R U . . .
C211 C -0.0990(2) 0.22836(17) 0.48714(14) 0.0162(4) Uani 1 1 d . . . . .
C212 C -0.1910(2) 0.16074(19) 0.53237(17) 0.0242(4) Uani 1 1 d . . . . .
H212 H -0.241301 0.081142 0.498119 0.029 Uiso 1 1 calc R U . . .
C213 C -0.2091(3) 0.2102(2) 0.62840(19) 0.0330(5) Uani 1 1 d . . . . .
H213 H -0.271591 0.163959 0.659956 0.040 Uiso 1 1 calc R U . . .
C214 C -0.1376(3) 0.3250(2) 0.67774(17) 0.0316(5) Uani 1 1 d . . . . .
H214 H -0.150011 0.357641 0.743682 0.038 Uiso 1 1 calc R U . . .
C215 C -0.0473(2) 0.3939(2) 0.63223(17) 0.0280(5) Uani 1 1 d . . . . .
H215 H 0.000833 0.474048 0.666024 0.034 Uiso 1 1 calc R U . . .
C216 C -0.0276(2) 0.34544(18) 0.53730(16) 0.0211(4) Uani 1 1 d . . . . .
H216 H 0.035037 0.392226 0.506141 0.025 Uiso 1 1 calc R U . . .
C221 C -0.1937(2) 0.02732(17) 0.31431(15) 0.0188(4) Uani 1 1 d . . . . .
C222 C -0.1524(2) -0.07835(19) 0.32536(17) 0.0253(4) Uani 1 1 d . . . . .
H222 H -0.053006 -0.077380 0.358991 0.030 Uiso 1 1 calc R U . . .
C223 C -0.2560(3) -0.1858(2) 0.28735(19) 0.0359(6) Uani 1 1 d . . . . .
H223 H -0.227628 -0.258451 0.295313 0.043 Uiso 1 1 calc R U . . .
C224 C -0.3993(3) -0.1876(2) 0.23834(19) 0.0392(6) Uani 1 1 d . . . . .
H224 H -0.469814 -0.261569 0.212729 0.047 Uiso 1 1 calc R U . . .
C225 C -0.4416(3) -0.0833(2) 0.2260(2) 0.0374(6) Uani 1 1 d . . . . .
H225 H -0.541097 -0.085193 0.191511 0.045 Uiso 1 1 calc R U . . .
C226 C -0.3393(2) 0.0246(2) 0.26373(19) 0.0288(5) Uani 1 1 d . . . . .
H226 H -0.368474 0.096876 0.255119 0.035 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
P1 C1 1.7507(19) . ?
P1 C111 1.799(2) . ?
P1 C121 1.8136(19) . ?
P1 P2 2.1303(9) . ?
P2 P3 2.1260(9) . ?
P3 C2 1.7342(19) . ?
P3 C221 1.808(2) . ?
P3 C211 1.8116(19) . ?
C1 C5 1.398(3) . ?
C1 C2 1.417(2) . ?
C2 C3 1.401(3) . ?
C3 C4 1.401(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.405(2) . ?
C4 C41 1.511(3) . ?
C5 H5 0.9500 . ?
C41 C44 1.528(3) . ?
C41 C42 1.528(3) . ?
C41 C43 1.530(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C111 C116 1.382(3) . ?
C111 C112 1.387(3) . ?
C112 C113 1.384(3) . ?
C112 H112 0.9500 . ?
C113 C114 1.379(4) . ?
C113 H113 0.9500 . ?
C114 C115 1.369(3) . ?
C114 H114 0.9500 . ?
C115 C116 1.385(3) . ?
C115 H115 0.9500 . ?
C116 H116 0.9500 . ?
C121 C126 1.383(3) . ?
C121 C122 1.383(3) . ?
C122 C123 1.386(3) . ?
C122 H122 0.9500 . ?
C123 C124 1.377(3) . ?
C123 H123 0.9500 . ?
C124 C125 1.369(3) . ?
C124 H124 0.9500 . ?
C125 C126 1.391(3) . ?
C125 H125 0.9500 . ?
C126 H126 0.9500 . ?
C211 C212 1.384(3) . ?
C211 C216 1.392(3) . ?
C212 C213 1.391(3) . ?
C212 H212 0.9500 . ?
C213 C214 1.368(4) . ?
C213 H213 0.9500 . ?
C214 C215 1.383(3) . ?
C214 H214 0.9500 . ?
C215 C216 1.382(3) . ?
C215 H215 0.9500 . ?
C216 H216 0.9500 . ?
C221 C222 1.381(3) . ?
C221 C226 1.391(3) . ?
C222 C223 1.385(3) . ?
C222 H222 0.9500 . ?
C223 C224 1.369(4) . ?
C223 H223 0.9500 . ?
C224 C225 1.372(4) . ?
C224 H224 0.9500 . ?
C225 C226 1.383(3) . ?
C225 H225 0.9500 . ?
C226 H226 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
C1 P1 C111 111.87(9) . . ?
C1 P1 C121 111.17(9) . . ?
C111 P1 C121 105.46(9) . . ?
C1 P1 P2 106.64(7) . . ?
C111 P1 P2 108.11(7) . . ?
C121 P1 P2 113.64(7) . . ?
P3 P2 P1 89.76(4) . . ?
C2 P3 C221 110.26(9) . . ?
C2 P3 C211 111.89(9) . . ?
C221 P3 C211 104.34(9) . . ?
C2 P3 P2 106.73(7) . . ?
C221 P3 P2 114.87(7) . . ?
C211 P3 P2 108.84(7) . . ?
C5 C1 C2 108.11(16) . . ?
C5 C1 P1 134.80(14) . . ?
C2 C1 P1 116.74(14) . . ?
C3 C2 C1 107.69(16) . . ?
C3 C2 P3 134.03(15) . . ?
C1 C2 P3 117.37(14) . . ?
C2 C3 C4 107.98(16) . . ?
C2 C3 H3 126.0 . . ?
C4 C3 H3 126.0 . . ?
C3 C4 C5 108.44(16) . . ?
C3 C4 C41 125.09(17) . . ?
C5 C4 C41 126.46(16) . . ?
C1 C5 C4 107.77(16) . . ?
C1 C5 H5 126.1 . . ?
C4 C5 H5 126.1 . . ?
C4 C41 C44 109.82(15) . . ?
C4 C41 C42 110.47(16) . . ?
C44 C41 C42 109.13(18) . . ?
C4 C41 C43 110.16(16) . . ?
C44 C41 C43 108.28(17) . . ?
C42 C41 C43 108.93(17) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C116 C111 C112 119.56(18) . . ?
C116 C111 P1 119.75(15) . . ?
C112 C111 P1 120.44(16) . . ?
C113 C112 C111 119.8(2) . . ?
C113 C112 H112 120.1 . . ?
C111 C112 H112 120.1 . . ?
C114 C113 C112 120.2(2) . . ?
C114 C113 H113 119.9 . . ?
C112 C113 H113 119.9 . . ?
C115 C114 C113 120.1(2) . . ?
C115 C114 H114 119.9 . . ?
C113 C114 H114 119.9 . . ?
C114 C115 C116 120.2(2) . . ?
C114 C115 H115 119.9 . . ?
C116 C115 H115 119.9 . . ?
C111 C116 C115 120.1(2) . . ?
C111 C116 H116 119.9 . . ?
C115 C116 H116 119.9 . . ?
C126 C121 C122 119.45(18) . . ?
C126 C121 P1 121.22(15) . . ?
C122 C121 P1 119.11(15) . . ?
C121 C122 C123 119.8(2) . . ?
C121 C122 H122 120.1 . . ?
C123 C122 H122 120.1 . . ?
C124 C123 C122 120.7(2) . . ?
C124 C123 H123 119.6 . . ?
C122 C123 H123 119.6 . . ?
C125 C124 C123 119.5(2) . . ?
C125 C124 H124 120.2 . . ?
C123 C124 H124 120.2 . . ?
C124 C125 C126 120.5(2) . . ?
C124 C125 H125 119.8 . . ?
C126 C125 H125 119.8 . . ?
C121 C126 C125 120.1(2) . . ?
C121 C126 H126 120.0 . . ?
C125 C126 H126 120.0 . . ?
C212 C211 C216 119.69(18) . . ?
C212 C211 P3 122.41(15) . . ?
C216 C211 P3 117.84(15) . . ?
C211 C212 C213 119.5(2) . . ?
C211 C212 H212 120.3 . . ?
C213 C212 H212 120.3 . . ?
C214 C213 C212 120.5(2) . . ?
C214 C213 H213 119.7 . . ?
C212 C213 H213 119.7 . . ?
C213 C214 C215 120.4(2) . . ?
C213 C214 H214 119.8 . . ?
C215 C214 H214 119.8 . . ?
C216 C215 C214 119.6(2) . . ?
C216 C215 H215 120.2 . . ?
C214 C215 H215 120.2 . . ?
C215 C216 C211 120.3(2) . . ?
C215 C216 H216 119.9 . . ?
C211 C216 H216 119.9 . . ?
C222 C221 C226 119.5(2) . . ?
C222 C221 P3 120.39(16) . . ?
C226 C221 P3 120.13(16) . . ?
C221 C222 C223 119.9(2) . . ?
C221 C222 H222 120.0 . . ?
C223 C222 H222 120.0 . . ?
C224 C223 C222 120.2(2) . . ?
C224 C223 H223 119.9 . . ?
C222 C223 H223 119.9 . . ?
C223 C224 C225 120.5(2) . . ?
C223 C224 H224 119.8 . . ?
C225 C224 H224 119.8 . . ?
C224 C225 C226 119.9(2) . . ?
C224 C225 H225 120.0 . . ?
C226 C225 H225 120.0 . . ?
C225 C226 C221 120.0(2) . . ?
C225 C226 H226 120.0 . . ?
C221 C226 H226 120.0 . . ?

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
C111 P1 C1 C5 61.2(2) . . . . ?
C121 P1 C1 C5 -56.4(2) . . . . ?
P2 P1 C1 C5 179.20(17) . . . . ?
C111 P1 C1 C2 -126.64(14) . . . . ?
C121 P1 C1 C2 115.74(15) . . . . ?
P2 P1 C1 C2 -8.63(15) . . . . ?
C5 C1 C2 C3 0.1(2) . . . . ?
P1 C1 C2 C3 -174.04(13) . . . . ?
C5 C1 C2 P3 170.73(13) . . . . ?
P1 C1 C2 P3 -3.4(2) . . . . ?
C221 P3 C2 C3 55.9(2) . . . . ?
C211 P3 C2 C3 -59.7(2) . . . . ?
P2 P3 C2 C3 -178.67(17) . . . . ?
C221 P3 C2 C1 -111.57(15) . . . . ?
C211 P3 C2 C1 132.78(14) . . . . ?
P2 P3 C2 C1 13.81(16) . . . . ?
C1 C2 C3 C4 -0.3(2) . . . . ?
P3 C2 C3 C4 -168.63(15) . . . . ?
C2 C3 C4 C5 0.3(2) . . . . ?
C2 C3 C4 C41 -178.85(17) . . . . ?
C2 C1 C5 C4 0.1(2) . . . . ?
P1 C1 C5 C4 172.69(15) . . . . ?
C3 C4 C5 C1 -0.2(2) . . . . ?
C41 C4 C5 C1 178.91(17) . . . . ?
C3 C4 C41 C44 -142.11(19) . . . . ?
C5 C4 C41 C44 38.9(3) . . . . ?
C3 C4 C41 C42 97.5(2) . . . . ?
C5 C4 C41 C42 -81.5(2) . . . . ?
C3 C4 C41 C43 -22.9(3) . . . . ?
C5 C4 C41 C43 158.09(19) . . . . ?
C1 P1 C111 C116 7.79(19) . . . . ?
C121 P1 C111 C116 128.78(17) . . . . ?
P2 P1 C111 C116 -109.34(16) . . . . ?
C1 P1 C111 C112 -177.93(16) . . . . ?
C121 P1 C111 C112 -56.94(18) . . . . ?
P2 P1 C111 C112 64.94(17) . . . . ?
C116 C111 C112 C113 0.2(3) . . . . ?
P1 C111 C112 C113 -174.07(18) . . . . ?
C111 C112 C113 C114 -0.5(4) . . . . ?
C112 C113 C114 C115 0.3(4) . . . . ?
C113 C114 C115 C116 0.2(4) . . . . ?
C112 C111 C116 C115 0.3(3) . . . . ?
P1 C111 C116 C115 174.61(17) . . . . ?
C114 C115 C116 C111 -0.5(3) . . . . ?
C1 P1 C121 C126 86.45(19) . . . . ?
C111 P1 C121 C126 -35.0(2) . . . . ?
P2 P1 C121 C126 -153.23(16) . . . . ?
C1 P1 C121 C122 -88.20(18) . . . . ?
C111 P1 C121 C122 150.36(16) . . . . ?
P2 P1 C121 C122 32.12(18) . . . . ?
C126 C121 C122 C123 -0.2(3) . . . . ?
P1 C121 C122 C123 174.52(16) . . . . ?
C121 C122 C123 C124 0.7(3) . . . . ?
C122 C123 C124 C125 -0.9(4) . . . . ?
C123 C124 C125 C126 0.6(4) . . . . ?
C122 C121 C126 C125 -0.1(3) . . . . ?
P1 C121 C126 C125 -174.72(19) . . . . ?
C124 C125 C126 C121 -0.1(4) . . . . ?
C2 P3 C211 C212 131.29(17) . . . . ?
C221 P3 C211 C212 12.09(19) . . . . ?
P2 P3 C211 C212 -111.00(16) . . . . ?
C2 P3 C211 C216 -51.55(18) . . . . ?
C221 P3 C211 C216 -170.76(15) . . . . ?
P2 P3 C211 C216 66.16(16) . . . . ?
C216 C211 C212 C213 -0.9(3) . . . . ?
P3 C211 C212 C213 176.18(17) . . . . ?
C211 C212 C213 C214 0.4(3) . . . . ?
C212 C213 C214 C215 0.6(4) . . . . ?
C213 C214 C215 C216 -1.1(3) . . . . ?
C214 C215 C216 C211 0.6(3) . . . . ?
C212 C211 C216 C215 0.4(3) . . . . ?
P3 C211 C216 C215 -176.79(16) . . . . ?
C2 P3 C221 C222 133.70(17) . . . . ?
C211 P3 C221 C222 -106.00(17) . . . . ?
P2 P3 C221 C222 13.07(19) . . . . ?
C2 P3 C221 C226 -47.29(19) . . . . ?
C211 P3 C221 C226 73.01(18) . . . . ?
P2 P3 C221 C226 -167.91(15) . . . . ?
C226 C221 C222 C223 -0.8(3) . . . . ?
P3 C221 C222 C223 178.24(17) . . . . ?
C221 C222 C223 C224 0.3(4) . . . . ?
C222 C223 C224 C225 0.2(4) . . . . ?
C223 C224 C225 C226 -0.4(4) . . . . ?
C224 C225 C226 C221 -0.1(4) . . . . ?
C222 C221 C226 C225 0.7(3) . . . . ?
P3 C221 C226 C225 -178.36(18) . . . . ?

_refine_diff_density_max         0.365
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.054

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1578542'
_audit_update_record             
;
2017-10-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H31 Mo2 O8 P3, C4 H10 O'
_chemical_formula_sum            'C45 H41 Mo2 O9 P3'
_chemical_formula_weight         1010.57

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

_cell_length_a                   12.0912(4)
_cell_length_b                   20.0536(6)
_cell_length_c                   37.1612(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9010.6(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    9737
_cell_measurement_theta_min      2.95
_cell_measurement_theta_max      26.30

_exptl_crystal_description       Plate
_exptl_crystal_colour            gold
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_F_000             4096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.024
_exptl_absorpt_coefficient_mu    0.716
_shelx_estimated_absorpt_T_min   0.868
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_process_details   'SADABS; Bruker, 2015'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            88417
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.858
_diffrn_reflns_theta_max         26.395
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9148
_reflns_number_gt                7595
_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-2016/6 (Sheldrick, 2016)'
_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)+(0.0284P)²+11.9585P] 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         9148
_refine_ls_number_parameters     547
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0725
_refine_ls_wR_factor_gt          0.0687
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.062
_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
P1 P 0.36287(5) 0.36282(3) 0.40890(2) 0.01983(13) Uani 1 1 d . . . . .
P2 P 0.51137(5) 0.29092(3) 0.35210(2) 0.01991(13) Uani 1 1 d . . . . .
P3 P 0.45441(5) 0.39246(3) 0.36092(2) 0.02188(14) Uani 1 1 d . . . . .
C1 C 0.42660(19) 0.28682(12) 0.42119(6) 0.0194(5) Uani 1 1 d . . . . .
C2 C 0.49021(19) 0.25217(12) 0.39426(6) 0.0184(5) Uani 1 1 d . . . . .
C3 C 0.51849(19) 0.18838(12) 0.40844(6) 0.0204(5) Uani 1 1 d . . . . .
H3 H 0.561832 0.155500 0.396619 0.024 Uiso 1 1 calc R U . . .
C4 C 0.47082(19) 0.18226(12) 0.44333(6) 0.0202(5) Uani 1 1 d . . . . .
C5 C 0.41611(19) 0.24311(12) 0.45138(6) 0.0206(5) Uani 1 1 d . . . . .
H5 H 0.378720 0.253108 0.473204 0.025 Uiso 1 1 calc R U . . .
C11 C 0.2156(2) 0.34748(13) 0.40551(6) 0.0236(5) Uani 1 1 d . . . . .
C12 C 0.1746(2) 0.28301(14) 0.40435(8) 0.0331(6) Uani 1 1 d . . . . .
H12 H 0.223788 0.246093 0.404841 0.040 Uiso 1 1 calc R U . . .
C13 C 0.0607(2) 0.27257(17) 0.40248(8) 0.0434(8) Uani 1 1 d . . . . .
H13 H 0.032299 0.228426 0.401735 0.052 Uiso 1 1 calc R U . . .
C14 C -0.0109(2) 0.32619(18) 0.40169(8) 0.0441(8) Uani 1 1 d . . . . .
H14 H -0.088439 0.318854 0.400262 0.053 Uiso 1 1 calc R U . . .
C15 C 0.0298(2) 0.39021(18) 0.40299(8) 0.0415(7) Uani 1 1 d . . . . .
H15 H -0.019832 0.426924 0.402371 0.050 Uiso 1 1 calc R U . . .
C16 C 0.1426(2) 0.40150(15) 0.40518(7) 0.0323(6) Uani 1 1 d . . . . .
H16 H 0.170252 0.445780 0.406448 0.039 Uiso 1 1 calc R U . . .
C21 C 0.3755(2) 0.42931(13) 0.44124(6) 0.0236(5) Uani 1 1 d . . . . .
C22 C 0.4191(2) 0.49096(13) 0.43156(7) 0.0298(6) Uani 1 1 d . . . . .
H22 H 0.448171 0.497398 0.408061 0.036 Uiso 1 1 calc R U . . .
C23 C 0.4203(2) 0.54288(14) 0.45604(8) 0.0354(7) Uani 1 1 d . . . . .
H23 H 0.449161 0.585112 0.449267 0.042 Uiso 1 1 calc R U . . .
C24 C 0.3794(2) 0.53328(15) 0.49038(8) 0.0353(7) Uani 1 1 d . . . . .
H24 H 0.380531 0.568859 0.507257 0.042 Uiso 1 1 calc R U . . .
C25 C 0.3370(2) 0.47231(16) 0.50015(7) 0.0360(7) Uani 1 1 d . . . . .
H25 H 0.309658 0.466004 0.523870 0.043 Uiso 1 1 calc R U . . .
C26 C 0.3337(2) 0.41969(15) 0.47575(7) 0.0319(6) Uani 1 1 d . . . . .
H26 H 0.303357 0.377844 0.482552 0.038 Uiso 1 1 calc R U . . .
C31 C 0.4425(2) 0.24197(13) 0.31808(7) 0.0308(6) Uani 1 1 d . . . . .
C32 C 0.4902(3) 0.23237(15) 0.28428(8) 0.0479(8) Uani 1 1 d . . . . .
H32 H 0.560232 0.251489 0.278966 0.057 Uiso 1 1 calc R U . . .
C33 C 0.4357(4) 0.19511(18) 0.25859(10) 0.0712(13) Uani 1 1 d . . . . .
H33 H 0.468995 0.188016 0.235753 0.085 Uiso 1 1 calc R U . . .
C34 C 0.3338(5) 0.16825(19) 0.26583(11) 0.0819(16) Uani 1 1 d . . . . .
H34 H 0.296002 0.143666 0.247772 0.098 Uiso 1 1 calc R U . . .
C35 C 0.2864(4) 0.1767(2) 0.29886(12) 0.0753(13) Uani 1 1 d . . . . .
H35 H 0.216512 0.157182 0.303881 0.090 Uiso 1 1 calc R U . . .
C36 C 0.3408(3) 0.21401(17) 0.32535(9) 0.0519(9) Uani 1 1 d . . . . .
H36 H 0.307598 0.220056 0.348295 0.062 Uiso 1 1 calc R U . . .
C41 C 0.6545(2) 0.29350(13) 0.33863(6) 0.0260(5) Uani 1 1 d . . . . .
C42 C 0.7022(3) 0.35139(15) 0.32647(9) 0.0428(8) Uani 1 1 d . . . . .
H42 H 0.660353 0.391445 0.325621 0.051 Uiso 1 1 calc R U . . .
C43 C 0.8119(3) 0.35115(18) 0.31540(10) 0.0594(10) Uani 1 1 d . . . . .
H43 H 0.844644 0.390914 0.306472 0.071 Uiso 1 1 calc R U . . .
C44 C 0.8730(3) 0.2940(2) 0.31732(9) 0.0545(9) Uani 1 1 d . . . . .
H44 H 0.948398 0.294359 0.310132 0.065 Uiso 1 1 calc R U . . .
C45 C 0.8260(3) 0.23615(19) 0.32954(9) 0.0552(10) Uani 1 1 d . . . . .
H45 H 0.868848 0.196482 0.330653 0.066 Uiso 1 1 calc R U . . .
C46 C 0.7166(3) 0.23522(16) 0.34026(8) 0.0444(8) Uani 1 1 d . . . . .
H46 H 0.683991 0.195040 0.348690 0.053 Uiso 1 1 calc R U . . .
C51 C 0.4690(2) 0.11846(12) 0.46563(6) 0.0239(5) Uani 1 1 d . . . . .
C52 C 0.3829(3) 0.07298(17) 0.44873(9) 0.0537(10) Uani 1 1 d . . . . .
H52A H 0.403480 0.063627 0.423728 0.081 Uiso 1 1 calc R U . . .
H52B H 0.310515 0.094898 0.449317 0.081 Uiso 1 1 calc R U . . .
H52C H 0.379320 0.031080 0.462254 0.081 Uiso 1 1 calc R U . . .
C53 C 0.4358(4) 0.13334(17) 0.50418(8) 0.0644(12) Uani 1 1 d . . . . .
H53A H 0.432535 0.091631 0.517879 0.097 Uiso 1 1 calc R U . . .
H53B H 0.363009 0.154811 0.504448 0.097 Uiso 1 1 calc R U . . .
H53C H 0.490487 0.163194 0.515111 0.097 Uiso 1 1 calc R U . . .
C54 C 0.5803(3) 0.08440(17) 0.46473(11) 0.0613(11) Uani 1 1 d . . . . .
H54A H 0.598833 0.072726 0.439847 0.092 Uiso 1 1 calc R U . . .
H54B H 0.577492 0.043788 0.479376 0.092 Uiso 1 1 calc R U . . .
H54C H 0.636699 0.114560 0.474389 0.092 Uiso 1 1 calc R U . . .
Mo1 Mo 0.34394(2) 0.44534(2) 0.30883(2) 0.02889(7) Uani 1 1 d . . . . .
C61 C 0.2579(3) 0.48309(16) 0.26810(8) 0.0424(7) Uani 1 1 d . . . . .
C62 C 0.4521(3) 0.52282(15) 0.30642(7) 0.0398(7) Uani 1 1 d . . . . .
C63 C 0.2594(3) 0.50599(18) 0.34309(8) 0.0522(9) Uani 1 1 d . . . . .
C64 C 0.2268(3) 0.37035(18) 0.31086(8) 0.0465(8) Uani 1 1 d . . . . .
C65 C 0.4430(2) 0.39888(14) 0.27191(7) 0.0325(6) Uani 1 1 d . . . . .
O61 O 0.2059(2) 0.50196(13) 0.24428(6) 0.0621(7) Uani 1 1 d . . . . .
O62 O 0.5080(2) 0.56863(12) 0.30463(7) 0.0648(7) Uani 1 1 d . . . . .
O63 O 0.2179(3) 0.54542(14) 0.36082(7) 0.0837(10) Uani 1 1 d . . . . .
O64 O 0.1595(2) 0.33090(15) 0.31110(8) 0.0728(8) Uani 1 1 d . . . . .
O65 O 0.5013(2) 0.37908(11) 0.25033(6) 0.0514(6) Uani 1 1 d . . . . .
Mo2 Mo 0.60610(2) 0.27187(2) 0.44392(2) 0.01867(6) Uani 1 1 d . . . . .
C71 C 0.6831(2) 0.35427(14) 0.43157(7) 0.0288(6) Uani 1 1 d . . . . .
C72 C 0.7503(2) 0.22934(14) 0.44607(8) 0.0351(6) Uani 1 1 d . . . . .
C73 C 0.6316(2) 0.29196(13) 0.49431(7) 0.0305(6) Uani 1 1 d . . . . .
O71 O 0.72826(18) 0.40362(10) 0.42407(6) 0.0464(5) Uani 1 1 d . . . . .
O72 O 0.83509(18) 0.20217(12) 0.44798(8) 0.0653(8) Uani 1 1 d . . . . .
O73 O 0.6459(2) 0.30220(11) 0.52472(5) 0.0506(6) Uani 1 1 d . . . . .
O81 O 0.6449(3) 0.07248(14) 0.35580(8) 0.0806(9) Uani 1 1 d D . . . .
C81 C 0.7302(5) 0.0349(3) 0.35881(18) 0.114(2) Uani 1 1 d D . . . .
H81A H 0.764344 0.029471 0.334780 0.137 Uiso 1 1 calc R U . . .
H81B H 0.706131 -0.009685 0.367107 0.137 Uiso 1 1 calc R U . . .
C82 C 0.8142(4) 0.0607(3) 0.38392(13) 0.0894(16) Uani 1 1 d . . . . .
H82A H 0.831031 0.107207 0.377961 0.134 Uiso 1 1 calc R U . . .
H82B H 0.881692 0.033847 0.381917 0.134 Uiso 1 1 calc R U . . .
H82C H 0.785934 0.058153 0.408596 0.134 Uiso 1 1 calc R U . . .
C831 C 0.5427(7) 0.0502(5) 0.3372(2) 0.105(3) Uiso 0.676(11) 1 d D U P A 1
H83A H 0.524146 0.004725 0.345691 0.126 Uiso 0.676(11) 1 calc R U P A 1
H83B H 0.481244 0.080018 0.344362 0.126 Uiso 0.676(11) 1 calc R U P A 1
C841 C 0.5493(8) 0.0493(5) 0.30054(19) 0.091(3) Uani 0.676(11) 1 d D U P A 1
H84A H 0.565951 0.094303 0.291748 0.136 Uiso 0.676(11) 1 calc R U P A 1
H84B H 0.478620 0.034383 0.290483 0.136 Uiso 0.676(11) 1 calc R U P A 1
H84C H 0.608153 0.018705 0.293065 0.136 Uiso 0.676(11) 1 calc R U P A 1
C832 C 0.5762(15) 0.0732(7) 0.3225(5) 0.128(6) Uiso 0.324(11) 1 d D U P A 2
H83C H 0.510851 0.101842 0.326666 0.153 Uiso 0.324(11) 1 calc R U P A 2
H83D H 0.619920 0.093507 0.302814 0.153 Uiso 0.324(11) 1 calc R U P A 2
C842 C 0.5410(17) 0.0121(8) 0.3116(5) 0.134(7) Uani 0.324(11) 1 d D U P A 2
H84D H 0.594877 -0.021764 0.318975 0.202 Uiso 0.324(11) 1 calc R U P A 2
H84E H 0.533377 0.011663 0.285378 0.202 Uiso 0.324(11) 1 calc R U P A 2
H84F H 0.469225 0.002338 0.322708 0.202 Uiso 0.324(11) 1 calc R U P A 2


_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
P1 C1 1.768(2) . ?
P1 C21 1.802(3) . ?
P1 C11 1.812(2) . ?
P1 P3 2.1813(8) . ?
P2 C2 1.768(2) . ?
P2 C41 1.803(3) . ?
P2 C31 1.804(3) . ?
P2 P3 2.1743(9) . ?
P3 Mo1 2.5799(7) . ?
C1 C5 1.429(3) . ?
C1 C2 1.441(3) . ?
C1 Mo2 2.348(2) . ?
C2 C3 1.425(3) . ?
C2 Mo2 2.351(2) . ?
C3 C4 1.424(3) . ?
C3 Mo2 2.380(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.420(3) . ?
C4 C51 1.525(3) . ?
C4 Mo2 2.430(2) . ?
C5 Mo2 2.385(2) . ?
C5 H5 0.9500 . ?
C11 C12 1.385(4) . ?
C11 C16 1.397(4) . ?
C12 C13 1.395(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.391(4) . ?
C21 C26 1.392(3) . ?
C22 C23 1.383(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.374(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.392(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C36 1.378(4) . ?
C31 C32 1.396(4) . ?
C32 C33 1.380(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.371(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.365(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.401(5) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.373(4) . ?
C41 C46 1.390(4) . ?
C42 C43 1.389(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.365(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.369(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.382(4) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C54 1.510(4) . ?
C51 C53 1.517(4) . ?
C51 C52 1.519(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
Mo1 C61 1.987(3) . ?
Mo1 C62 2.033(3) . ?
Mo1 C63 2.036(3) . ?
Mo1 C65 2.046(3) . ?
Mo1 C64 2.067(4) . ?
C61 O61 1.150(4) . ?
C62 O62 1.142(4) . ?
C63 O63 1.145(4) . ?
C64 O64 1.135(4) . ?
C65 O65 1.139(3) . ?
Mo2 C73 1.940(3) . ?
Mo2 C72 1.943(3) . ?
Mo2 C71 1.951(3) . ?
C71 O71 1.164(3) . ?
C72 O72 1.163(4) . ?
C73 O73 1.162(3) . ?
O81 C81 1.282(6) . ?
O81 C831 1.484(8) . ?
O81 C832 1.491(10) . ?
C81 C82 1.474(7) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C831 C841 1.366(9) . ?
C831 H83A 0.9900 . ?
C831 H83B 0.9900 . ?
C841 H84A 0.9800 . ?
C841 H84B 0.9800 . ?
C841 H84C 0.9800 . ?
C832 C842 1.358(11) . ?
C832 H83C 0.9900 . ?
C832 H83D 0.9900 . ?
C842 H84D 0.9800 . ?
C842 H84E 0.9800 . ?
C842 H84F 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 P1 C21 115.40(11) . . ?
C1 P1 C11 107.46(12) . . ?
C21 P1 C11 104.80(11) . . ?
C1 P1 P3 102.99(8) . . ?
C21 P1 P3 107.50(9) . . ?
C11 P1 P3 119.22(8) . . ?
C2 P2 C41 113.43(11) . . ?
C2 P2 C31 108.36(12) . . ?
C41 P2 C31 105.34(13) . . ?
C2 P2 P3 103.43(8) . . ?
C41 P2 P3 108.61(9) . . ?
C31 P2 P3 117.96(9) . . ?
P2 P3 P1 91.65(3) . . ?
P2 P3 Mo1 115.84(3) . . ?
P1 P3 Mo1 117.56(3) . . ?
C5 C1 C2 107.3(2) . . ?
C5 C1 P1 133.85(19) . . ?
C2 C1 P1 117.97(17) . . ?
C5 C1 Mo2 73.82(13) . . ?
C2 C1 Mo2 72.24(13) . . ?
P1 C1 Mo2 127.30(12) . . ?
C3 C2 C1 107.70(19) . . ?
C3 C2 P2 133.45(18) . . ?
C1 C2 P2 118.75(17) . . ?
C3 C2 Mo2 73.58(13) . . ?
C1 C2 Mo2 72.04(13) . . ?
P2 C2 Mo2 122.39(12) . . ?
C4 C3 C2 108.5(2) . . ?
C4 C3 Mo2 74.72(13) . . ?
C2 C3 Mo2 71.36(13) . . ?
C4 C3 H3 125.8 . . ?
C2 C3 H3 125.8 . . ?
Mo2 C3 H3 119.9 . . ?
C5 C4 C3 107.8(2) . . ?
C5 C4 C51 126.9(2) . . ?
C3 C4 C51 125.0(2) . . ?
C5 C4 Mo2 71.11(13) . . ?
C3 C4 Mo2 70.85(13) . . ?
C51 C4 Mo2 128.72(16) . . ?
C4 C5 C1 108.7(2) . . ?
C4 C5 Mo2 74.60(13) . . ?
C1 C5 Mo2 71.03(13) . . ?
C4 C5 H5 125.7 . . ?
C1 C5 H5 125.7 . . ?
Mo2 C5 H5 120.4 . . ?
C12 C11 C16 119.8(2) . . ?
C12 C11 P1 120.8(2) . . ?
C16 C11 P1 119.3(2) . . ?
C11 C12 C13 119.7(3) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C13 120.1(3) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.5(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 119.7(3) . . ?
C15 C16 H16 120.1 . . ?
C11 C16 H16 120.1 . . ?
C22 C21 C26 119.9(2) . . ?
C22 C21 P1 121.14(19) . . ?
C26 C21 P1 118.8(2) . . ?
C23 C22 C21 120.2(2) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 119.9(3) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C25 C24 C23 120.1(3) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 120.9(3) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C21 119.0(3) . . ?
C25 C26 H26 120.5 . . ?
C21 C26 H26 120.5 . . ?
C36 C31 C32 119.3(3) . . ?
C36 C31 P2 119.7(2) . . ?
C32 C31 P2 121.0(2) . . ?
C33 C32 C31 120.0(4) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C34 C33 C32 120.4(4) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C35 C34 C33 120.3(3) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 120.1(4) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C31 C36 C35 119.9(4) . . ?
C31 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C42 C41 C46 119.9(3) . . ?
C42 C41 P2 121.3(2) . . ?
C46 C41 P2 118.8(2) . . ?
C41 C42 C43 119.7(3) . . ?
C41 C42 H42 120.1 . . ?
C43 C42 H42 120.1 . . ?
C44 C43 C42 120.3(3) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 120.3(3) . . ?
C43 C44 H44 119.9 . . ?
C45 C44 H44 119.9 . . ?
C44 C45 C46 120.3(3) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C45 C46 C41 119.5(3) . . ?
C45 C46 H46 120.2 . . ?
C41 C46 H46 120.2 . . ?
C54 C51 C53 110.2(3) . . ?
C54 C51 C52 109.2(3) . . ?
C53 C51 C52 109.1(3) . . ?
C54 C51 C4 110.8(2) . . ?
C53 C51 C4 110.6(2) . . ?
C52 C51 C4 106.8(2) . . ?
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 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C61 Mo1 C62 90.71(13) . . ?
C61 Mo1 C63 89.20(12) . . ?
C62 Mo1 C63 83.91(14) . . ?
C61 Mo1 C65 88.24(11) . . ?
C62 Mo1 C65 86.66(12) . . ?
C63 Mo1 C65 170.20(13) . . ?
C61 Mo1 C64 86.92(13) . . ?
C62 Mo1 C64 176.80(12) . . ?
C63 Mo1 C64 93.90(15) . . ?
C65 Mo1 C64 95.41(13) . . ?
C61 Mo1 P3 178.13(10) . . ?
C62 Mo1 P3 90.80(8) . . ?
C63 Mo1 P3 92.07(9) . . ?
C65 Mo1 P3 90.73(7) . . ?
C64 Mo1 P3 91.61(8) . . ?
O61 C61 Mo1 176.7(3) . . ?
O62 C62 Mo1 176.1(3) . . ?
O63 C63 Mo1 172.9(3) . . ?
O64 C64 Mo1 177.0(3) . . ?
O65 C65 Mo1 173.3(2) . . ?
C73 Mo2 C72 84.76(12) . . ?
C73 Mo2 C71 88.58(11) . . ?
C72 Mo2 C71 87.33(11) . . ?
C73 Mo2 C1 117.89(10) . . ?
C72 Mo2 C1 154.21(10) . . ?
C71 Mo2 C1 104.36(10) . . ?
C73 Mo2 C2 152.56(10) . . ?
C72 Mo2 C2 119.57(10) . . ?
C71 Mo2 C2 104.00(9) . . ?
C1 Mo2 C2 35.71(8) . . ?
C73 Mo2 C3 138.74(10) . . ?
C72 Mo2 C3 96.52(10) . . ?
C71 Mo2 C3 132.66(9) . . ?
C1 Mo2 C3 58.61(8) . . ?
C2 Mo2 C3 35.06(8) . . ?
C73 Mo2 C5 95.24(10) . . ?
C72 Mo2 C5 138.91(10) . . ?
C71 Mo2 C5 133.76(10) . . ?
C1 Mo2 C5 35.14(8) . . ?
C2 Mo2 C5 58.42(8) . . ?
C3 Mo2 C5 57.69(8) . . ?
C73 Mo2 C4 105.63(10) . . ?
C72 Mo2 C4 106.25(10) . . ?
C71 Mo2 C4 160.93(9) . . ?
C1 Mo2 C4 57.93(8) . . ?
C2 Mo2 C4 57.82(8) . . ?
C3 Mo2 C4 34.43(8) . . ?
C5 Mo2 C4 34.29(8) . . ?
O71 C71 Mo2 179.5(3) . . ?
O72 C72 Mo2 177.8(3) . . ?
O73 C73 Mo2 178.1(2) . . ?
C81 O81 C831 122.2(5) . . ?
C81 O81 C832 121.7(8) . . ?
O81 C81 C82 113.8(4) . . ?
O81 C81 H81A 108.8 . . ?
C82 C81 H81A 108.8 . . ?
O81 C81 H81B 108.8 . . ?
C82 C81 H81B 108.8 . . ?
H81A C81 H81B 107.7 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C841 C831 O81 114.8(7) . . ?
C841 C831 H83A 108.6 . . ?
O81 C831 H83A 108.6 . . ?
C841 C831 H83B 108.6 . . ?
O81 C831 H83B 108.6 . . ?
H83A C831 H83B 107.6 . . ?
C831 C841 H84A 109.5 . . ?
C831 C841 H84B 109.5 . . ?
H84A C841 H84B 109.5 . . ?
C831 C841 H84C 109.5 . . ?
H84A C841 H84C 109.5 . . ?
H84B C841 H84C 109.5 . . ?
C842 C832 O81 114.4(10) . . ?
C842 C832 H83C 108.7 . . ?
O81 C832 H83C 108.7 . . ?
C842 C832 H83D 108.7 . . ?
O81 C832 H83D 108.7 . . ?
H83C C832 H83D 107.6 . . ?
C832 C842 H84D 109.5 . . ?
C832 C842 H84E 109.5 . . ?
H84D C842 H84E 109.5 . . ?
C832 C842 H84F 109.5 . . ?
H84D C842 H84F 109.5 . . ?
H84E C842 H84F 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
C21 P1 C1 C5 56.5(3) . . . . ?
C11 P1 C1 C5 -59.9(3) . . . . ?
P3 P1 C1 C5 173.4(2) . . . . ?
C21 P1 C1 C2 -136.01(18) . . . . ?
C11 P1 C1 C2 107.52(19) . . . . ?
P3 P1 C1 C2 -19.2(2) . . . . ?
C21 P1 C1 Mo2 -47.70(18) . . . . ?
C11 P1 C1 Mo2 -164.18(13) . . . . ?
P3 P1 C1 Mo2 69.11(14) . . . . ?
C5 C1 C2 C3 -0.6(3) . . . . ?
P1 C1 C2 C3 -171.15(16) . . . . ?
Mo2 C1 C2 C3 65.46(16) . . . . ?
C5 C1 C2 P2 176.26(17) . . . . ?
P1 C1 C2 P2 5.7(3) . . . . ?
Mo2 C1 C2 P2 -117.68(16) . . . . ?
C5 C1 C2 Mo2 -66.06(16) . . . . ?
P1 C1 C2 Mo2 123.39(16) . . . . ?
C41 P2 C2 C3 -55.7(3) . . . . ?
C31 P2 C2 C3 60.9(3) . . . . ?
P3 P2 C2 C3 -173.1(2) . . . . ?
C41 P2 C2 C1 128.45(19) . . . . ?
C31 P2 C2 C1 -115.0(2) . . . . ?
P3 P2 C2 C1 11.0(2) . . . . ?
C41 P2 C2 Mo2 42.37(17) . . . . ?
C31 P2 C2 Mo2 158.96(13) . . . . ?
P3 P2 C2 Mo2 -75.09(13) . . . . ?
C1 C2 C3 C4 1.6(3) . . . . ?
P2 C2 C3 C4 -174.60(19) . . . . ?
Mo2 C2 C3 C4 66.04(16) . . . . ?
C1 C2 C3 Mo2 -64.44(16) . . . . ?
P2 C2 C3 Mo2 119.4(2) . . . . ?
C2 C3 C4 C5 -2.0(3) . . . . ?
Mo2 C3 C4 C5 61.86(16) . . . . ?
C2 C3 C4 C51 171.7(2) . . . . ?
Mo2 C3 C4 C51 -124.4(2) . . . . ?
C2 C3 C4 Mo2 -63.85(16) . . . . ?
C3 C4 C5 C1 1.6(3) . . . . ?
C51 C4 C5 C1 -172.0(2) . . . . ?
Mo2 C4 C5 C1 63.32(16) . . . . ?
C3 C4 C5 Mo2 -61.69(16) . . . . ?
C51 C4 C5 Mo2 124.7(2) . . . . ?
C2 C1 C5 C4 -0.6(3) . . . . ?
P1 C1 C5 C4 167.8(2) . . . . ?
Mo2 C1 C5 C4 -65.63(16) . . . . ?
C2 C1 C5 Mo2 64.99(16) . . . . ?
P1 C1 C5 Mo2 -126.6(2) . . . . ?
C1 P1 C11 C12 -14.1(2) . . . . ?
C21 P1 C11 C12 -137.4(2) . . . . ?
P3 P1 C11 C12 102.4(2) . . . . ?
C1 P1 C11 C16 163.88(19) . . . . ?
C21 P1 C11 C16 40.6(2) . . . . ?
P3 P1 C11 C16 -79.6(2) . . . . ?
C16 C11 C12 C13 0.7(4) . . . . ?
P1 C11 C12 C13 178.7(2) . . . . ?
C11 C12 C13 C14 0.1(4) . . . . ?
C12 C13 C14 C15 -0.4(5) . . . . ?
C13 C14 C15 C16 -0.2(4) . . . . ?
C14 C15 C16 C11 1.0(4) . . . . ?
C12 C11 C16 C15 -1.3(4) . . . . ?
P1 C11 C16 C15 -179.3(2) . . . . ?
C1 P1 C21 C22 125.2(2) . . . . ?
C11 P1 C21 C22 -116.8(2) . . . . ?
P3 P1 C21 C22 11.0(2) . . . . ?
C1 P1 C21 C26 -59.2(2) . . . . ?
C11 P1 C21 C26 58.8(2) . . . . ?
P3 P1 C21 C26 -173.43(19) . . . . ?
C26 C21 C22 C23 -0.5(4) . . . . ?
P1 C21 C22 C23 175.1(2) . . . . ?
C21 C22 C23 C24 0.9(4) . . . . ?
C22 C23 C24 C25 -0.4(4) . . . . ?
C23 C24 C25 C26 -0.5(4) . . . . ?
C24 C25 C26 C21 0.9(4) . . . . ?
C22 C21 C26 C25 -0.4(4) . . . . ?
P1 C21 C26 C25 -176.0(2) . . . . ?
C2 P2 C31 C36 39.3(3) . . . . ?
C41 P2 C31 C36 161.0(2) . . . . ?
P3 P2 C31 C36 -77.7(3) . . . . ?
C2 P2 C31 C32 -141.3(2) . . . . ?
C41 P2 C31 C32 -19.6(3) . . . . ?
P3 P2 C31 C32 101.8(2) . . . . ?
C36 C31 C32 C33 -0.1(5) . . . . ?
P2 C31 C32 C33 -179.6(3) . . . . ?
C31 C32 C33 C34 1.1(5) . . . . ?
C32 C33 C34 C35 -1.7(6) . . . . ?
C33 C34 C35 C36 1.3(6) . . . . ?
C32 C31 C36 C35 -0.3(5) . . . . ?
P2 C31 C36 C35 179.2(3) . . . . ?
C34 C35 C36 C31 -0.3(6) . . . . ?
C2 P2 C41 C42 -131.4(2) . . . . ?
C31 P2 C41 C42 110.3(2) . . . . ?
P3 P2 C41 C42 -17.0(3) . . . . ?
C2 P2 C41 C46 49.5(3) . . . . ?
C31 P2 C41 C46 -68.8(2) . . . . ?
P3 P2 C41 C46 163.9(2) . . . . ?
C46 C41 C42 C43 0.8(5) . . . . ?
P2 C41 C42 C43 -178.3(3) . . . . ?
C41 C42 C43 C44 -1.4(5) . . . . ?
C42 C43 C44 C45 1.2(6) . . . . ?
C43 C44 C45 C46 -0.4(6) . . . . ?
C44 C45 C46 C41 -0.1(5) . . . . ?
C42 C41 C46 C45 -0.1(5) . . . . ?
P2 C41 C46 C45 179.1(3) . . . . ?
C5 C4 C51 C54 -142.8(3) . . . . ?
C3 C4 C51 C54 44.6(4) . . . . ?
Mo2 C4 C51 C54 -48.1(3) . . . . ?
C5 C4 C51 C53 -20.3(4) . . . . ?
C3 C4 C51 C53 167.1(3) . . . . ?
Mo2 C4 C51 C53 74.4(3) . . . . ?
C5 C4 C51 C52 98.3(3) . . . . ?
C3 C4 C51 C52 -74.2(3) . . . . ?
Mo2 C4 C51 C52 -167.0(2) . . . . ?
C831 O81 C81 C82 -168.7(6) . . . . ?
C832 O81 C81 C82 153.2(10) . . . . ?
C81 O81 C831 C841 -75.6(10) . . . . ?
C81 O81 C832 C842 53(2) . . . . ?

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
C3 H3 O81 0.95 2.47 3.401(4) 167.9 .
C46 H46 O81 0.95 2.52 3.426(4) 160.2 .

_refine_diff_density_max         0.909
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.067

####################################################################### 
# 
# 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_p-1
_database_code_depnum_ccdc_archive 'CCDC 1578544'
_audit_update_record             
;
2017-10-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H31 Mn2 O8 P3, 0.5(C4 H10 O)'
_chemical_formula_sum            'C43 H36 Mn2 O8.50 P3'
_chemical_formula_weight         891.51

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'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   11.1044(6)
_cell_length_b                   11.8694(7)
_cell_length_c                   16.9388(10)
_cell_angle_alpha                105.480(2)
_cell_angle_beta                 93.283(2)
_cell_angle_gamma                99.354(2)
_cell_volume                     2111.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    9859
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      32.38

_exptl_crystal_description       Block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             914
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.189
_exptl_absorpt_coefficient_mu    0.764
_shelx_estimated_absorpt_T_min   0.697
_shelx_estimated_absorpt_T_max   0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_process_details   'SADABS; Bruker, 2016'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            129291
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.799
_diffrn_reflns_theta_max         32.647
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             15412
_reflns_number_gt                11085
_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-2017/1 (Sheldrick, 2017)'
_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)+(0.0428P)²+2.3856P] 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         15412
_refine_ls_number_parameters     537
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1232
_refine_ls_wR_factor_gt          0.0997
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_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
O71_1 O 0.5571(17) 0.9977(13) -0.0126(8) 0.106(3) Uani 0.5 1 d D U P A -1
C71_1 C 0.7574(15) 1.1010(9) -0.0015(6) 0.132(4) Uani 0.5 1 d D U P A -1
H71A_1 H 0.785567 1.025294 -0.007770 0.197 Uiso 0.5 1 calc R U P A -1
H71B_1 H 0.820346 1.166111 0.032721 0.197 Uiso 0.5 1 calc R U P A -1
H71C_1 H 0.742517 1.113562 -0.055793 0.197 Uiso 0.5 1 calc R U P A -1
C72_1 C 0.642(2) 1.0980(14) 0.0385(7) 0.121(4) Uani 0.5 1 d D U P A -1
H72A_1 H 0.656599 1.089112 0.094583 0.146 Uiso 0.5 1 calc R U P A -1
H72B_1 H 0.610187 1.172248 0.042713 0.146 Uiso 0.5 1 calc R U P A -1
C73_1 C 0.446(3) 0.988(3) 0.0258(16) 0.143(8) Uani 0.5 1 d D U P A -1
H73A_1 H 0.415918 1.064069 0.039229 0.172 Uiso 0.5 1 calc R U P A -1
H73B_1 H 0.458336 0.963993 0.077042 0.172 Uiso 0.5 1 calc R U P A -1
C74_1 C 0.358(2) 0.893(2) -0.0372(15) 0.179(9) Uani 0.5 1 d D U P A -1
H74A_1 H 0.347474 0.918491 -0.087410 0.268 Uiso 0.5 1 calc R U P A -1
H74B_1 H 0.278282 0.880721 -0.015515 0.268 Uiso 0.5 1 calc R U P A -1
H74C_1 H 0.389850 0.819068 -0.050003 0.268 Uiso 0.5 1 calc R U P A -1
P1 P 0.53089(4) 0.68797(4) 0.32788(3) 0.01782(9) Uani 1 1 d . . . . .
P2 P 0.68710(4) 0.51780(4) 0.22325(3) 0.01677(9) Uani 1 1 d . . . . .
P3 P 0.70975(4) 0.71539(4) 0.27553(3) 0.01727(9) Uani 1 1 d . . . . .
C1 C 0.45821(16) 0.55067(16) 0.26376(11) 0.0201(3) Uani 1 1 d . . . . .
C2 C 0.33568(17) 0.49065(17) 0.25077(12) 0.0237(4) Uani 1 1 d . . . . .
H2 H 0.268197 0.521996 0.274118 0.028 Uiso 1 1 calc R U . . .
C3 C 0.33004(16) 0.37642(16) 0.19738(11) 0.0201(3) Uani 1 1 d . . . . .
C4 C 0.44910(16) 0.36517(16) 0.17650(11) 0.0209(3) Uani 1 1 d . . . . .
H4 H 0.471498 0.296911 0.140997 0.025 Uiso 1 1 calc R U . . .
C5 C 0.52922(15) 0.47203(16) 0.21707(11) 0.0189(3) Uani 1 1 d . . . . .
C11 C 0.44234(17) 0.79902(17) 0.32059(12) 0.0228(3) Uani 1 1 d . . . . .
C12 C 0.3801(2) 0.7881(2) 0.24429(15) 0.0328(4) Uani 1 1 d . . . . .
H12 H 0.384710 0.723175 0.198210 0.039 Uiso 1 1 calc R U . . .
C13 C 0.3114(2) 0.8729(3) 0.23618(19) 0.0463(6) Uani 1 1 d . . . . .
H13 H 0.268710 0.866315 0.184445 0.056 Uiso 1 1 calc R U . . .
C14 C 0.3052(3) 0.9673(3) 0.3040(2) 0.0516(7) Uani 1 1 d . . . . .
H14 H 0.257314 1.024786 0.298530 0.062 Uiso 1 1 calc R U . . .
C15 C 0.3672(3) 0.9786(2) 0.37886(19) 0.0482(7) Uani 1 1 d . . . . .
H15 H 0.363180 1.044391 0.424502 0.058 Uiso 1 1 calc R U . . .
C16 C 0.4361(2) 0.8942(2) 0.38824(15) 0.0350(5) Uani 1 1 d . . . . .
H16 H 0.478426 0.901405 0.440216 0.042 Uiso 1 1 calc R U . . .
C21 C 0.54744(19) 0.68724(17) 0.43470(11) 0.0251(4) Uani 1 1 d . . . . .
C22 C 0.6606(2) 0.6968(2) 0.47783(13) 0.0352(5) Uani 1 1 d . . . . .
H22 H 0.734067 0.711005 0.453090 0.042 Uiso 1 1 calc R U . . .
C23 C 0.6655(3) 0.6852(3) 0.55795(16) 0.0517(7) Uani 1 1 d . . . . .
H23 H 0.742807 0.692787 0.587903 0.062 Uiso 1 1 calc R U . . .
C24 C 0.5593(3) 0.6629(3) 0.59375(15) 0.0496(7) Uani 1 1 d . . . . .
H24 H 0.563227 0.653952 0.647864 0.060 Uiso 1 1 calc R U . . .
C25 C 0.4482(3) 0.6537(4) 0.55126(19) 0.0627(9) Uani 1 1 d . . . . .
H25 H 0.374945 0.638609 0.576089 0.075 Uiso 1 1 calc R U . . .
C26 C 0.4414(3) 0.6664(3) 0.47165(17) 0.0530(8) Uani 1 1 d . . . . .
H26 H 0.363737 0.660680 0.442762 0.064 Uiso 1 1 calc R U . . .
C31 C 0.73758(16) 0.47737(16) 0.12212(11) 0.0195(3) Uani 1 1 d . . . . .
C32 C 0.66424(17) 0.48891(17) 0.05590(11) 0.0235(3) Uani 1 1 d . . . . .
H32 H 0.588826 0.516025 0.064469 0.028 Uiso 1 1 calc R U . . .
C33 C 0.7024(2) 0.4604(2) -0.02268(12) 0.0305(4) Uani 1 1 d . . . . .
H33 H 0.653746 0.469369 -0.067799 0.037 Uiso 1 1 calc R U . . .
C34 C 0.8113(2) 0.4190(2) -0.03509(13) 0.0356(5) Uani 1 1 d . . . . .
H34 H 0.836925 0.399085 -0.088848 0.043 Uiso 1 1 calc R U . . .
C35 C 0.8831(2) 0.4066(2) 0.03043(14) 0.0364(5) Uani 1 1 d . . . . .
H35 H 0.957317 0.377461 0.021296 0.044 Uiso 1 1 calc R U . . .
C36 C 0.84730(18) 0.4366(2) 0.10969(13) 0.0285(4) Uani 1 1 d . . . . .
H36 H 0.897373 0.429237 0.154762 0.034 Uiso 1 1 calc R U . . .
C41 C 0.77240(17) 0.45002(17) 0.28633(11) 0.0218(3) Uani 1 1 d . . . . .
C42 C 0.8664(3) 0.5157(2) 0.34594(17) 0.0484(7) Uani 1 1 d . . . . .
H42 H 0.884857 0.599758 0.356844 0.058 Uiso 1 1 calc R U . . .
C43 C 0.9342(3) 0.4592(3) 0.39015(19) 0.0570(8) Uani 1 1 d . . . . .
H43 H 1.001582 0.504182 0.428877 0.068 Uiso 1 1 calc R U . . .
C44 C 0.9033(3) 0.3381(2) 0.37759(18) 0.0489(7) Uani 1 1 d . . . . .
H44 H 0.944582 0.300362 0.410971 0.059 Uiso 1 1 calc R U . . .
C45 C 0.8141(3) 0.2731(2) 0.31765(18) 0.0434(6) Uani 1 1 d . . . . .
H45 H 0.795974 0.189099 0.307208 0.052 Uiso 1 1 calc R U . . .
C46 C 0.7486(2) 0.3276(2) 0.27114(16) 0.0384(5) Uani 1 1 d . . . . .
H46 H 0.687038 0.280535 0.228624 0.046 Uiso 1 1 calc R U . . .
C51 C 0.21629(17) 0.28075(18) 0.16661(13) 0.0261(4) Uani 1 1 d . . . . .
C52 C 0.2328(3) 0.1708(2) 0.19296(18) 0.0444(6) Uani 1 1 d . . . . .
H52A H 0.304089 0.141074 0.169674 0.067 Uiso 1 1 calc R U . . .
H52B H 0.159131 0.109162 0.172976 0.067 Uiso 1 1 calc R U . . .
H52C H 0.245635 0.191497 0.253207 0.067 Uiso 1 1 calc R U . . .
C53 C 0.1041(2) 0.3237(3) 0.2034(3) 0.0835(15) Uani 1 1 d . . . . .
H53A H 0.117053 0.343132 0.263575 0.125 Uiso 1 1 calc R U . . .
H53B H 0.031521 0.260794 0.182908 0.125 Uiso 1 1 calc R U . . .
H53C H 0.091476 0.394663 0.187285 0.125 Uiso 1 1 calc R U . . .
C54 C 0.1949(3) 0.2464(3) 0.07327(18) 0.0643(10) Uani 1 1 d . . . . .
H54A H 0.182990 0.316275 0.055431 0.097 Uiso 1 1 calc R U . . .
H54B H 0.121598 0.184091 0.054274 0.097 Uiso 1 1 calc R U . . .
H54C H 0.266189 0.216814 0.049841 0.097 Uiso 1 1 calc R U . . .
Mn1 Mn 0.73917(3) 0.83289(2) 0.18957(2) 0.01999(6) Uani 1 1 d . . . . .
Mn2 Mn 0.87989(3) 0.84903(3) 0.33819(2) 0.02215(7) Uani 1 1 d . . . . .
C61 C 0.8293(2) 0.9562(2) 0.16225(14) 0.0324(4) Uani 1 1 d . . . . .
O61 O 0.8872(2) 1.03226(18) 0.14417(14) 0.0560(5) Uani 1 1 d . . . . .
C62 C 0.6497(2) 0.94424(18) 0.24251(13) 0.0285(4) Uani 1 1 d . . . . .
O62 O 0.60026(17) 1.02074(15) 0.26858(13) 0.0451(4) Uani 1 1 d . . . . .
C63 C 0.62041(19) 0.77642(19) 0.10400(13) 0.0281(4) Uani 1 1 d . . . . .
O63 O 0.54470(16) 0.74150(17) 0.05015(11) 0.0435(4) Uani 1 1 d . . . . .
C64 C 0.84782(18) 0.74724(18) 0.13397(11) 0.0241(4) Uani 1 1 d . . . . .
O64 O 0.92030(15) 0.70482(16) 0.09720(10) 0.0362(4) Uani 1 1 d . . . . .
C65 C 0.97532(19) 0.9818(2) 0.32562(14) 0.0314(4) Uani 1 1 d . . . . .
O65 O 1.03465(17) 1.06754(16) 0.32027(13) 0.0469(4) Uani 1 1 d . . . . .
C66 C 0.9836(2) 0.7548(2) 0.28389(13) 0.0315(4) Uani 1 1 d . . . . .
O66 O 1.05129(18) 0.69677(19) 0.25523(13) 0.0515(5) Uani 1 1 d . . . . .
C67 C 0.9491(2) 0.8357(2) 0.43279(14) 0.0354(5) Uani 1 1 d . . . . .
O67 O 0.9955(2) 0.8261(2) 0.49248(12) 0.0590(6) Uani 1 1 d . . . . .
C68 C 0.7840(2) 0.94642(19) 0.39824(13) 0.0306(4) Uani 1 1 d . . . . .
O68 O 0.72950(18) 1.00897(18) 0.43827(12) 0.0518(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O71_1 C73_1 1.431(15) . ?
O71_1 C72_1 1.431(16) . ?
C71_1 C72_1 1.48(2) . ?
C71_1 H71A_1 0.9800 . ?
C71_1 H71B_1 0.9800 . ?
C71_1 H71C_1 0.9800 . ?
C72_1 H72A_1 0.9900 . ?
C72_1 H72B_1 0.9900 . ?
C73_1 C74_1 1.50(2) . ?
C73_1 H73A_1 0.9900 . ?
C73_1 H73B_1 0.9900 . ?
C74_1 H74A_1 0.9800 . ?
C74_1 H74B_1 0.9800 . ?
C74_1 H74C_1 0.9800 . ?
P1 C1 1.7361(18) . ?
P1 C11 1.7926(19) . ?
P1 C21 1.8107(19) . ?
P1 P3 2.2322(6) . ?
P2 C5 1.7375(17) . ?
P2 C31 1.7992(17) . ?
P2 C41 1.8102(19) . ?
P2 P3 2.2410(6) . ?
P3 Mn2 2.2604(5) . ?
P3 Mn1 2.2720(5) . ?
C1 C2 1.405(2) . ?
C1 C5 1.427(2) . ?
C2 C3 1.404(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.406(2) . ?
C3 C51 1.516(3) . ?
C4 C5 1.404(2) . ?
C4 H4 0.9500 . ?
C11 C16 1.392(3) . ?
C11 C12 1.394(3) . ?
C12 C13 1.387(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.389(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.370(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.391(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.383(3) . ?
C21 C22 1.389(3) . ?
C22 C23 1.399(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.377(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.365(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.395(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C36 1.389(3) . ?
C31 C32 1.398(3) . ?
C32 C33 1.392(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.384(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.383(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.392(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.382(3) . ?
C41 C46 1.384(3) . ?
C42 C43 1.395(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.378(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.351(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.388(3) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C54 1.518(3) . ?
C51 C52 1.521(3) . ?
C51 C53 1.525(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
Mn1 C63 1.807(2) . ?
Mn1 C61 1.815(2) . ?
Mn1 C64 1.842(2) . ?
Mn1 C62 1.853(2) . ?
Mn1 Mn2 2.8302(4) . ?
Mn2 C67 1.794(2) . ?
Mn2 C65 1.821(2) . ?
Mn2 C68 1.844(2) . ?
Mn2 C66 1.847(2) . ?
C61 O61 1.142(3) . ?
C62 O62 1.139(3) . ?
C63 O63 1.144(3) . ?
C64 O64 1.145(2) . ?
C65 O65 1.147(3) . ?
C66 O66 1.143(3) . ?
C67 O67 1.150(3) . ?
C68 O68 1.141(3) . ?

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
C73_1 O71_1 C72_1 108.2(12) . . ?
C72_1 C71_1 H71A_1 109.5 . . ?
C72_1 C71_1 H71B_1 109.5 . . ?
H71A_1 C71_1 H71B_1 109.5 . . ?
C72_1 C71_1 H71C_1 109.5 . . ?
H71A_1 C71_1 H71C_1 109.5 . . ?
H71B_1 C71_1 H71C_1 109.5 . . ?
O71_1 C72_1 C71_1 106.2(10) . . ?
O71_1 C72_1 H72A_1 110.5 . . ?
C71_1 C72_1 H72A_1 110.5 . . ?
O71_1 C72_1 H72B_1 110.5 . . ?
C71_1 C72_1 H72B_1 110.5 . . ?
H72A_1 C72_1 H72B_1 108.7 . . ?
O71_1 C73_1 C74_1 104.2(16) . . ?
O71_1 C73_1 H73A_1 110.9 . . ?
C74_1 C73_1 H73A_1 110.9 . . ?
O71_1 C73_1 H73B_1 110.9 . . ?
C74_1 C73_1 H73B_1 110.9 . . ?
H73A_1 C73_1 H73B_1 108.9 . . ?
C73_1 C74_1 H74A_1 109.5 . . ?
C73_1 C74_1 H74B_1 109.5 . . ?
H74A_1 C74_1 H74B_1 109.5 . . ?
C73_1 C74_1 H74C_1 109.5 . . ?
H74A_1 C74_1 H74C_1 109.5 . . ?
H74B_1 C74_1 H74C_1 109.5 . . ?
C1 P1 C11 109.65(9) . . ?
C1 P1 C21 111.89(9) . . ?
C11 P1 C21 107.75(9) . . ?
C1 P1 P3 102.07(6) . . ?
C11 P1 P3 112.04(6) . . ?
C21 P1 P3 113.39(7) . . ?
C5 P2 C31 109.83(8) . . ?
C5 P2 C41 113.13(9) . . ?
C31 P2 C41 106.75(9) . . ?
C5 P2 P3 102.35(6) . . ?
C31 P2 P3 112.05(6) . . ?
C41 P2 P3 112.81(6) . . ?
P1 P3 P2 88.88(2) . . ?
P1 P3 Mn2 126.12(2) . . ?
P2 P3 Mn2 129.18(2) . . ?
P1 P3 Mn1 120.38(2) . . ?
P2 P3 Mn1 118.99(2) . . ?
Mn2 P3 Mn1 77.283(18) . . ?
C2 C1 C5 107.59(16) . . ?
C2 C1 P1 132.48(14) . . ?
C5 C1 P1 119.73(13) . . ?
C3 C2 C1 108.33(16) . . ?
C3 C2 H2 125.8 . . ?
C1 C2 H2 125.8 . . ?
C2 C3 C4 108.15(16) . . ?
C2 C3 C51 126.63(16) . . ?
C4 C3 C51 125.22(17) . . ?
C5 C4 C3 108.34(16) . . ?
C5 C4 H4 125.8 . . ?
C3 C4 H4 125.8 . . ?
C4 C5 C1 107.59(15) . . ?
C4 C5 P2 133.26(14) . . ?
C1 C5 P2 119.07(13) . . ?
C16 C11 C12 120.5(2) . . ?
C16 C11 P1 121.64(16) . . ?
C12 C11 P1 117.88(15) . . ?
C13 C12 C11 119.5(2) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 119.7(3) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C15 C14 C13 120.8(2) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C15 C16 C11 119.2(2) . . ?
C15 C16 H16 120.4 . . ?
C11 C16 H16 120.4 . . ?
C26 C21 C22 119.4(2) . . ?
C26 C21 P1 117.61(18) . . ?
C22 C21 P1 122.72(15) . . ?
C21 C22 C23 119.5(2) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 120.5(3) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C25 C24 C23 119.8(2) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 120.5(3) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C21 C26 C25 120.1(3) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C36 C31 C32 120.38(17) . . ?
C36 C31 P2 121.16(15) . . ?
C32 C31 P2 118.46(13) . . ?
C33 C32 C31 119.56(18) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 120.0(2) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C35 C34 C33 120.28(19) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C34 C35 C36 120.5(2) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C31 C36 C35 119.3(2) . . ?
C31 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
C42 C41 C46 118.5(2) . . ?
C42 C41 P2 122.17(16) . . ?
C46 C41 P2 119.20(16) . . ?
C41 C42 C43 120.3(2) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 H42 119.8 . . ?
C44 C43 C42 119.9(3) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C45 C44 C43 119.8(2) . . ?
C45 C44 H44 120.1 . . ?
C43 C44 H44 120.1 . . ?
C44 C45 C46 120.8(2) . . ?
C44 C45 H45 119.6 . . ?
C46 C45 H45 119.6 . . ?
C41 C46 C45 120.4(2) . . ?
C41 C46 H46 119.8 . . ?
C45 C46 H46 119.8 . . ?
C3 C51 C54 110.40(18) . . ?
C3 C51 C52 109.65(17) . . ?
C54 C51 C52 108.6(2) . . ?
C3 C51 C53 110.58(19) . . ?
C54 C51 C53 109.7(3) . . ?
C52 C51 C53 107.9(2) . . ?
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 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C63 Mn1 C61 101.89(10) . . ?
C63 Mn1 C64 92.82(9) . . ?
C61 Mn1 C64 83.78(10) . . ?
C63 Mn1 C62 90.74(10) . . ?
C61 Mn1 C62 85.20(10) . . ?
C64 Mn1 C62 168.90(9) . . ?
C63 Mn1 P3 108.11(7) . . ?
C61 Mn1 P3 149.95(8) . . ?
C64 Mn1 P3 92.77(6) . . ?
C62 Mn1 P3 96.11(6) . . ?
C63 Mn1 Mn2 159.26(7) . . ?
C61 Mn1 Mn2 98.80(8) . . ?
C64 Mn1 Mn2 88.00(6) . . ?
C62 Mn1 Mn2 92.38(7) . . ?
P3 Mn1 Mn2 51.174(14) . . ?
C67 Mn2 C65 102.69(11) . . ?
C67 Mn2 C68 88.98(11) . . ?
C65 Mn2 C68 88.07(10) . . ?
C67 Mn2 C66 87.73(11) . . ?
C65 Mn2 C66 90.95(10) . . ?
C68 Mn2 C66 176.27(10) . . ?
C67 Mn2 P3 117.91(8) . . ?
C65 Mn2 P3 139.33(8) . . ?
C68 Mn2 P3 90.24(7) . . ?
C66 Mn2 P3 92.85(7) . . ?
C67 Mn2 Mn1 169.45(8) . . ?
C65 Mn2 Mn1 87.85(7) . . ?
C68 Mn2 Mn1 91.01(7) . . ?
C66 Mn2 Mn1 92.55(7) . . ?
P3 Mn2 Mn1 51.543(14) . . ?
O61 C61 Mn1 178.7(2) . . ?
O62 C62 Mn1 171.37(19) . . ?
O63 C63 Mn1 179.4(2) . . ?
O64 C64 Mn1 172.67(18) . . ?
O65 C65 Mn2 177.7(2) . . ?
O66 C66 Mn2 175.5(2) . . ?
O67 C67 Mn2 178.4(3) . . ?
O68 C68 Mn2 176.6(2) . . ?

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
C73_1 O71_1 C72_1 C71_1 177.2(12) . . . . ?
C72_1 O71_1 C73_1 C74_1 172(3) . . . . ?
C11 P1 C1 C2 -46.3(2) . . . . ?
C21 P1 C1 C2 73.2(2) . . . . ?
P3 P1 C1 C2 -165.28(18) . . . . ?
C11 P1 C1 C5 139.54(15) . . . . ?
C21 P1 C1 C5 -100.97(16) . . . . ?
P3 P1 C1 C5 20.60(16) . . . . ?
C5 C1 C2 C3 0.3(2) . . . . ?
P1 C1 C2 C3 -174.32(15) . . . . ?
C1 C2 C3 C4 -0.4(2) . . . . ?
C1 C2 C3 C51 179.84(18) . . . . ?
C2 C3 C4 C5 0.3(2) . . . . ?
C51 C3 C4 C5 -179.94(17) . . . . ?
C3 C4 C5 C1 -0.1(2) . . . . ?
C3 C4 C5 P2 176.60(15) . . . . ?
C2 C1 C5 C4 -0.2(2) . . . . ?
P1 C1 C5 C4 175.29(13) . . . . ?
C2 C1 C5 P2 -177.38(14) . . . . ?
P1 C1 C5 P2 -1.9(2) . . . . ?
C31 P2 C5 C4 46.7(2) . . . . ?
C41 P2 C5 C4 -72.5(2) . . . . ?
P3 P2 C5 C4 165.84(18) . . . . ?
C31 P2 C5 C1 -136.98(15) . . . . ?
C41 P2 C5 C1 103.87(16) . . . . ?
P3 P2 C5 C1 -17.80(16) . . . . ?
C1 P1 C11 C16 145.62(17) . . . . ?
C21 P1 C11 C16 23.6(2) . . . . ?
P3 P1 C11 C16 -101.79(17) . . . . ?
C1 P1 C11 C12 -35.02(18) . . . . ?
C21 P1 C11 C12 -157.03(16) . . . . ?
P3 P1 C11 C12 77.57(16) . . . . ?
C16 C11 C12 C13 -0.2(3) . . . . ?
P1 C11 C12 C13 -179.54(18) . . . . ?
C11 C12 C13 C14 -0.1(4) . . . . ?
C12 C13 C14 C15 0.7(4) . . . . ?
C13 C14 C15 C16 -1.0(4) . . . . ?
C14 C15 C16 C11 0.7(4) . . . . ?
C12 C11 C16 C15 -0.1(3) . . . . ?
P1 C11 C16 C15 179.21(19) . . . . ?
C1 P1 C21 C26 -62.9(2) . . . . ?
C11 P1 C21 C26 57.8(2) . . . . ?
P3 P1 C21 C26 -177.7(2) . . . . ?
C1 P1 C21 C22 111.67(19) . . . . ?
C11 P1 C21 C22 -127.72(19) . . . . ?
P3 P1 C21 C22 -3.1(2) . . . . ?
C26 C21 C22 C23 0.0(4) . . . . ?
P1 C21 C22 C23 -174.5(2) . . . . ?
C21 C22 C23 C24 0.9(4) . . . . ?
C22 C23 C24 C25 -1.0(5) . . . . ?
C23 C24 C25 C26 0.2(5) . . . . ?
C22 C21 C26 C25 -0.7(5) . . . . ?
P1 C21 C26 C25 174.0(3) . . . . ?
C24 C25 C26 C21 0.6(6) . . . . ?
C5 P2 C31 C36 -141.27(16) . . . . ?
C41 P2 C31 C36 -18.28(19) . . . . ?
P3 P2 C31 C36 105.69(16) . . . . ?
C5 P2 C31 C32 39.32(17) . . . . ?
C41 P2 C31 C32 162.31(15) . . . . ?
P3 P2 C31 C32 -73.72(15) . . . . ?
C36 C31 C32 C33 -0.7(3) . . . . ?
P2 C31 C32 C33 178.76(15) . . . . ?
C31 C32 C33 C34 1.1(3) . . . . ?
C32 C33 C34 C35 -0.5(3) . . . . ?
C33 C34 C35 C36 -0.6(4) . . . . ?
C32 C31 C36 C35 -0.4(3) . . . . ?
P2 C31 C36 C35 -179.79(17) . . . . ?
C34 C35 C36 C31 1.0(4) . . . . ?
C5 P2 C41 C42 -132.6(2) . . . . ?
C31 P2 C41 C42 106.5(2) . . . . ?
P3 P2 C41 C42 -17.0(2) . . . . ?
C5 P2 C41 C46 51.6(2) . . . . ?
C31 P2 C41 C46 -69.3(2) . . . . ?
P3 P2 C41 C46 167.23(17) . . . . ?
C46 C41 C42 C43 -0.8(4) . . . . ?
P2 C41 C42 C43 -176.5(3) . . . . ?
C41 C42 C43 C44 -3.5(5) . . . . ?
C42 C43 C44 C45 5.5(5) . . . . ?
C43 C44 C45 C46 -3.3(5) . . . . ?
C42 C41 C46 C45 3.0(4) . . . . ?
P2 C41 C46 C45 178.9(2) . . . . ?
C44 C45 C46 C41 -1.0(4) . . . . ?
C2 C3 C51 C54 120.3(3) . . . . ?
C4 C3 C51 C54 -59.5(3) . . . . ?
C2 C3 C51 C52 -120.1(2) . . . . ?
C4 C3 C51 C52 60.1(3) . . . . ?
C2 C3 C51 C53 -1.3(3) . . . . ?
C4 C3 C51 C53 179.0(3) . . . . ?

_refine_diff_density_max         1.197
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.084

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1578545'
_audit_update_record             
;
2017-10-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H31 Fe O4 P3'
_chemical_formula_sum            'C37 H31 Fe O4 P3'
_chemical_formula_weight         688.38

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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                   16.0868(6)
_cell_length_b                   12.0933(4)
_cell_length_c                   18.1738(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.7590(10)
_cell_angle_gamma                90
_cell_volume                     3484.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    9840
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      28.85

_exptl_crystal_description       Plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_F_000             1424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.283
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.042
_exptl_absorpt_coefficient_mu    0.608
_shelx_estimated_absorpt_T_min   0.847
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_process_details   'SADABS; Bruker, 2016'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            118875
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.795
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10530
_reflns_number_gt                7357
_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-2017/1 (Sheldrick, 2017)'
_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)+(0.0352P)²+2.1151P] 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         10530
_refine_ls_number_parameters     409
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0440
_refine_ls_wR_factor_ref         0.0939
_refine_ls_wR_factor_gt          0.0822
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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
P1 P 0.35743(3) 0.70127(4) 0.57478(2) 0.01624(9) Uani 1 1 d . . . . .
P2 P 0.17476(3) 0.65679(4) 0.49324(2) 0.01663(9) Uani 1 1 d . . . . .
P3 P 0.28015(3) 0.75768(4) 0.47003(2) 0.01781(9) Uani 1 1 d . . . . .
C1 C 0.30576(10) 0.58180(14) 0.59678(9) 0.0177(3) Uani 1 1 d . . . . .
C2 C 0.32580(11) 0.49540(15) 0.64825(9) 0.0212(3) Uani 1 1 d . . . . .
H2 H 0.375807 0.489961 0.684326 0.025 Uiso 1 1 calc R U . . .
C3 C 0.25956(11) 0.41827(14) 0.63751(9) 0.0204(3) Uani 1 1 d . . . . .
C4 C 0.19768(11) 0.45602(14) 0.57882(10) 0.0202(3) Uani 1 1 d . . . . .
H4 H 0.146213 0.419619 0.559705 0.024 Uiso 1 1 calc R U . . .
C5 C 0.22532(10) 0.55692(14) 0.55347(9) 0.0175(3) Uani 1 1 d . . . . .
C11 C 0.37505(10) 0.79559(15) 0.65248(9) 0.0206(3) Uani 1 1 d . . . . .
C12 C 0.34426(13) 0.76912(18) 0.71734(10) 0.0305(4) Uani 1 1 d . . . . .
H12 H 0.311934 0.703863 0.719695 0.037 Uiso 1 1 calc R U . . .
C13 C 0.36130(16) 0.8391(2) 0.77856(12) 0.0444(6) Uani 1 1 d . . . . .
H13 H 0.341384 0.820977 0.823381 0.053 Uiso 1 1 calc R U . . .
C14 C 0.40675(16) 0.9344(2) 0.77473(13) 0.0466(6) Uani 1 1 d . . . . .
H14 H 0.417998 0.981753 0.816939 0.056 Uiso 1 1 calc R U . . .
C15 C 0.43631(14) 0.96195(18) 0.70999(12) 0.0374(5) Uani 1 1 d . . . . .
H15 H 0.467175 1.028449 0.707576 0.045 Uiso 1 1 calc R U . . .
C16 C 0.42082(12) 0.89239(16) 0.64867(11) 0.0271(4) Uani 1 1 d . . . . .
H16 H 0.441357 0.910710 0.604183 0.032 Uiso 1 1 calc R U . . .
C21 C 0.46136(10) 0.67681(14) 0.55242(9) 0.0198(3) Uani 1 1 d . . . . .
C22 C 0.46957(12) 0.64667(19) 0.48024(11) 0.0351(5) Uani 1 1 d . . . . .
H22 H 0.420743 0.640864 0.442855 0.042 Uiso 1 1 calc R U . . .
C23 C 0.54815(13) 0.6250(2) 0.46229(13) 0.0417(5) Uani 1 1 d . . . . .
H23 H 0.552992 0.605589 0.412548 0.050 Uiso 1 1 calc R U . . .
C24 C 0.61936(12) 0.63147(17) 0.51603(12) 0.0329(4) Uani 1 1 d . . . . .
H24 H 0.673284 0.616475 0.503624 0.039 Uiso 1 1 calc R U . . .
C25 C 0.61178(12) 0.65979(18) 0.58782(12) 0.0330(4) Uani 1 1 d . . . . .
H25 H 0.660759 0.663668 0.625168 0.040 Uiso 1 1 calc R U . . .
C26 C 0.53321(11) 0.68283(16) 0.60640(10) 0.0261(4) Uani 1 1 d . . . . .
H26 H 0.528800 0.702720 0.656162 0.031 Uiso 1 1 calc R U . . .
C31 C 0.09611(10) 0.72917(14) 0.53439(10) 0.0213(3) Uani 1 1 d . . . . .
C32 C 0.09760(13) 0.71741(17) 0.61084(11) 0.0307(4) Uani 1 1 d . . . . .
H32 H 0.137005 0.668647 0.639061 0.037 Uiso 1 1 calc R U . . .
C33 C 0.04157(15) 0.7769(2) 0.64591(14) 0.0434(5) Uani 1 1 d . . . . .
H33 H 0.042754 0.768978 0.698090 0.052 Uiso 1 1 calc R U . . .
C34 C -0.01562(14) 0.84715(19) 0.60490(15) 0.0454(6) Uani 1 1 d . . . . .
H34 H -0.054047 0.887461 0.628960 0.055 Uiso 1 1 calc R U . . .
C35 C -0.01769(13) 0.85965(17) 0.52913(15) 0.0405(5) Uani 1 1 d . . . . .
H35 H -0.057620 0.908168 0.501308 0.049 Uiso 1 1 calc R U . . .
C36 C 0.03852(11) 0.80142(16) 0.49340(12) 0.0292(4) Uani 1 1 d . . . . .
H36 H 0.037659 0.810829 0.441377 0.035 Uiso 1 1 calc R U . . .
C41 C 0.12446(11) 0.59585(15) 0.40624(10) 0.0214(3) Uani 1 1 d . . . . .
C42 C 0.17484(14) 0.5617(2) 0.35603(13) 0.0464(6) Uani 1 1 d . . . . .
H42 H 0.233848 0.575170 0.366395 0.056 Uiso 1 1 calc R U . . .
C43 C 0.13995(18) 0.5079(3) 0.29059(14) 0.0599(8) Uani 1 1 d . . . . .
H43 H 0.174831 0.485478 0.256013 0.072 Uiso 1 1 calc R U . . .
C44 C 0.05471(16) 0.4871(2) 0.27602(13) 0.0479(6) Uani 1 1 d . . . . .
H44 H 0.030489 0.450644 0.231186 0.057 Uiso 1 1 calc R U . . .
C45 C 0.00487(14) 0.5190(2) 0.32609(13) 0.0436(6) Uani 1 1 d . . . . .
H45 H -0.053888 0.503690 0.316044 0.052 Uiso 1 1 calc R U . . .
C46 C 0.03898(12) 0.57343(17) 0.39135(12) 0.0333(5) Uani 1 1 d . . . . .
H46 H 0.003733 0.595278 0.425753 0.040 Uiso 1 1 calc R U . . .
C51 C 0.25497(13) 0.31289(15) 0.68223(10) 0.0278(4) Uani 1 1 d . . . . .
C52 C 0.33435(18) 0.2444(2) 0.68505(17) 0.0619(8) Uani 1 1 d . . . . .
H52A H 0.341846 0.225547 0.634144 0.093 Uiso 1 1 calc R U . . .
H52B H 0.329416 0.176451 0.713330 0.093 Uiso 1 1 calc R U . . .
H52C H 0.383120 0.287064 0.709489 0.093 Uiso 1 1 calc R U . . .
C53 C 0.2423(2) 0.3433(2) 0.76083(13) 0.0557(7) Uani 1 1 d . . . . .
H53A H 0.291369 0.384752 0.785859 0.084 Uiso 1 1 calc R U . . .
H53B H 0.235691 0.275744 0.789056 0.084 Uiso 1 1 calc R U . . .
H53C H 0.191537 0.389022 0.758172 0.084 Uiso 1 1 calc R U . . .
C54 C 0.17875(18) 0.2421(2) 0.64666(15) 0.0541(7) Uani 1 1 d . . . . .
H54A H 0.126489 0.283337 0.647657 0.081 Uiso 1 1 calc R U . . .
H54B H 0.177818 0.173242 0.674904 0.081 Uiso 1 1 calc R U . . .
H54C H 0.183559 0.224933 0.594859 0.081 Uiso 1 1 calc R U . . .
Fe Fe 0.25542(2) 0.94371(2) 0.45961(2) 0.02327(7) Uani 1 1 d . . . . .
C61 C 0.23981(13) 1.08951(17) 0.45147(11) 0.0322(4) Uani 1 1 d . . . . .
O61 O 0.22898(11) 1.18250(12) 0.44686(10) 0.0474(4) Uani 1 1 d . . . . .
C62 C 0.22511(12) 0.94940(15) 0.55069(11) 0.0283(4) Uani 1 1 d . . . . .
O62 O 0.20471(10) 0.95614(12) 0.60771(9) 0.0405(4) Uani 1 1 d . . . . .
C63 C 0.18057(13) 0.91346(17) 0.37787(12) 0.0342(5) Uani 1 1 d . . . . .
O63 O 0.13305(12) 0.89535(15) 0.32476(10) 0.0578(5) Uani 1 1 d . . . . .
C64 C 0.36138(14) 0.95618(19) 0.44144(13) 0.0405(5) Uani 1 1 d . . . . .
O64 O 0.42747(11) 0.96594(18) 0.42761(14) 0.0743(6) 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
P1 C1 1.7467(17) . ?
P1 C11 1.7999(17) . ?
P1 C21 1.8107(17) . ?
P1 P3 2.1982(6) . ?
P2 C5 1.7368(16) . ?
P2 C31 1.8019(17) . ?
P2 C41 1.8067(18) . ?
P2 P3 2.1871(6) . ?
P3 Fe 2.2869(5) . ?
C1 C2 1.403(2) . ?
C1 C5 1.428(2) . ?
C2 C3 1.405(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.406(2) . ?
C3 C51 1.520(2) . ?
C4 C5 1.403(2) . ?
C4 H4 0.9500 . ?
C11 C16 1.391(3) . ?
C11 C12 1.391(2) . ?
C12 C13 1.388(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.372(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.385(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.385(2) . ?
C21 C22 1.389(2) . ?
C22 C23 1.383(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.376(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.374(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.391(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.393(3) . ?
C31 C36 1.394(2) . ?
C32 C33 1.389(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.375(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.380(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.391(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.382(3) . ?
C41 C46 1.383(2) . ?
C42 C43 1.388(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.375(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.366(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.386(3) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C52 1.515(3) . ?
C51 C53 1.522(3) . ?
C51 C54 1.544(3) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
Fe C61 1.784(2) . ?
Fe C63 1.784(2) . ?
Fe C64 1.797(2) . ?
Fe C62 1.804(2) . ?
C61 O61 1.139(3) . ?
C62 O62 1.142(2) . ?
C63 O63 1.146(2) . ?
C64 O64 1.139(3) . ?

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 P1 C11 111.24(8) . . ?
C1 P1 C21 114.18(8) . . ?
C11 P1 C21 104.54(8) . . ?
C1 P1 P3 103.52(6) . . ?
C11 P1 P3 118.26(6) . . ?
C21 P1 P3 105.34(6) . . ?
C5 P2 C31 111.29(8) . . ?
C5 P2 C41 111.12(8) . . ?
C31 P2 C41 108.63(8) . . ?
C5 P2 P3 102.35(6) . . ?
C31 P2 P3 115.53(6) . . ?
C41 P2 P3 107.79(6) . . ?
P2 P3 P1 90.17(2) . . ?
P2 P3 Fe 115.79(2) . . ?
P1 P3 Fe 116.22(2) . . ?
C2 C1 C5 107.16(15) . . ?
C2 C1 P1 134.76(13) . . ?
C5 C1 P1 118.03(12) . . ?
C1 C2 C3 108.58(15) . . ?
C1 C2 H2 125.7 . . ?
C3 C2 H2 125.7 . . ?
C2 C3 C4 108.22(15) . . ?
C2 C3 C51 125.94(16) . . ?
C4 C3 C51 125.84(16) . . ?
C5 C4 C3 107.97(15) . . ?
C5 C4 H4 126.0 . . ?
C3 C4 H4 126.0 . . ?
C4 C5 C1 108.07(14) . . ?
C4 C5 P2 132.15(13) . . ?
C1 C5 P2 118.99(13) . . ?
C16 C11 C12 120.23(17) . . ?
C16 C11 P1 120.57(14) . . ?
C12 C11 P1 119.19(14) . . ?
C13 C12 C11 119.3(2) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C14 C13 C12 120.4(2) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 120.6(2) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C16 119.8(2) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C11 119.72(19) . . ?
C15 C16 H16 120.1 . . ?
C11 C16 H16 120.1 . . ?
C26 C21 C22 118.76(16) . . ?
C26 C21 P1 121.58(13) . . ?
C22 C21 P1 119.60(13) . . ?
C23 C22 C21 120.62(18) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 C22 120.41(19) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 119.40(18) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 120.74(18) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C21 C26 C25 120.06(17) . . ?
C21 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C32 C31 C36 119.65(17) . . ?
C32 C31 P2 118.02(14) . . ?
C36 C31 P2 122.18(15) . . ?
C33 C32 C31 120.1(2) . . ?
C33 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C34 C33 C32 119.8(2) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 120.6(2) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C34 C35 C36 120.2(2) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C36 C31 119.6(2) . . ?
C35 C36 H36 120.2 . . ?
C31 C36 H36 120.2 . . ?
C42 C41 C46 119.15(18) . . ?
C42 C41 P2 118.29(14) . . ?
C46 C41 P2 122.30(15) . . ?
C41 C42 C43 120.6(2) . . ?
C41 C42 H42 119.7 . . ?
C43 C42 H42 119.7 . . ?
C44 C43 C42 119.7(2) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C45 C44 C43 119.9(2) . . ?
C45 C44 H44 120.0 . . ?
C43 C44 H44 120.0 . . ?
C44 C45 C46 120.8(2) . . ?
C44 C45 H45 119.6 . . ?
C46 C45 H45 119.6 . . ?
C41 C46 C45 119.8(2) . . ?
C41 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C52 C51 C3 111.04(17) . . ?
C52 C51 C53 110.3(2) . . ?
C3 C51 C53 109.00(16) . . ?
C52 C51 C54 108.4(2) . . ?
C3 C51 C54 110.35(16) . . ?
C53 C51 C54 107.7(2) . . ?
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 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C61 Fe C63 93.89(9) . . ?
C61 Fe C64 91.51(10) . . ?
C63 Fe C64 113.05(11) . . ?
C61 Fe C62 88.98(9) . . ?
C63 Fe C62 121.49(10) . . ?
C64 Fe C62 125.29(10) . . ?
C61 Fe P3 178.08(7) . . ?
C63 Fe P3 87.17(7) . . ?
C64 Fe P3 86.60(7) . . ?
C62 Fe P3 91.83(6) . . ?
O61 C61 Fe 179.0(2) . . ?
O62 C62 Fe 177.83(18) . . ?
O63 C63 Fe 178.9(2) . . ?
O64 C64 Fe 177.6(2) . . ?

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 C1 C2 -63.61(19) . . . . ?
C21 P1 C1 C2 54.4(2) . . . . ?
P3 P1 C1 C2 168.36(17) . . . . ?
C11 P1 C1 C5 119.34(13) . . . . ?
C21 P1 C1 C5 -122.64(13) . . . . ?
P3 P1 C1 C5 -8.68(14) . . . . ?
C5 C1 C2 C3 -0.03(19) . . . . ?
P1 C1 C2 C3 -177.30(14) . . . . ?
C1 C2 C3 C4 0.24(19) . . . . ?
C1 C2 C3 C51 -179.05(16) . . . . ?
C2 C3 C4 C5 -0.36(19) . . . . ?
C51 C3 C4 C5 178.93(16) . . . . ?
C3 C4 C5 C1 0.34(19) . . . . ?
C3 C4 C5 P2 -169.12(14) . . . . ?
C2 C1 C5 C4 -0.19(19) . . . . ?
P1 C1 C5 C4 177.61(12) . . . . ?
C2 C1 C5 P2 170.89(12) . . . . ?
P1 C1 C5 P2 -11.31(19) . . . . ?
C31 P2 C5 C4 69.54(19) . . . . ?
C41 P2 C5 C4 -51.66(19) . . . . ?
P3 P2 C5 C4 -166.49(16) . . . . ?
C31 P2 C5 C1 -98.99(14) . . . . ?
C41 P2 C5 C1 139.81(13) . . . . ?
P3 P2 C5 C1 24.98(14) . . . . ?
C1 P1 C11 C16 175.26(14) . . . . ?
C21 P1 C11 C16 51.57(16) . . . . ?
P3 P1 C11 C16 -65.15(16) . . . . ?
C1 P1 C11 C12 -3.01(17) . . . . ?
C21 P1 C11 C12 -126.71(15) . . . . ?
P3 P1 C11 C12 116.57(14) . . . . ?
C16 C11 C12 C13 -1.4(3) . . . . ?
P1 C11 C12 C13 176.90(17) . . . . ?
C11 C12 C13 C14 1.1(3) . . . . ?
C12 C13 C14 C15 -0.1(4) . . . . ?
C13 C14 C15 C16 -0.7(4) . . . . ?
C14 C15 C16 C11 0.5(3) . . . . ?
C12 C11 C16 C15 0.6(3) . . . . ?
P1 C11 C16 C15 -177.67(15) . . . . ?
C1 P1 C21 C26 -92.88(16) . . . . ?
C11 P1 C21 C26 28.90(17) . . . . ?
P3 P1 C21 C26 154.24(14) . . . . ?
C1 P1 C21 C22 84.34(18) . . . . ?
C11 P1 C21 C22 -153.87(16) . . . . ?
P3 P1 C21 C22 -28.54(17) . . . . ?
C26 C21 C22 C23 -1.2(3) . . . . ?
P1 C21 C22 C23 -178.47(19) . . . . ?
C21 C22 C23 C24 1.0(4) . . . . ?
C22 C23 C24 C25 -0.1(4) . . . . ?
C23 C24 C25 C26 -0.6(3) . . . . ?
C22 C21 C26 C25 0.5(3) . . . . ?
P1 C21 C26 C25 177.76(16) . . . . ?
C24 C25 C26 C21 0.3(3) . . . . ?
C5 P2 C31 C32 14.25(17) . . . . ?
C41 P2 C31 C32 136.89(15) . . . . ?
P3 P2 C31 C32 -101.89(14) . . . . ?
C5 P2 C31 C36 -170.25(15) . . . . ?
C41 P2 C31 C36 -47.61(17) . . . . ?
P3 P2 C31 C36 73.61(16) . . . . ?
C36 C31 C32 C33 0.4(3) . . . . ?
P2 C31 C32 C33 176.05(17) . . . . ?
C31 C32 C33 C34 0.2(3) . . . . ?
C32 C33 C34 C35 -0.3(4) . . . . ?
C33 C34 C35 C36 -0.3(4) . . . . ?
C34 C35 C36 C31 0.9(3) . . . . ?
C32 C31 C36 C35 -1.0(3) . . . . ?
P2 C31 C36 C35 -176.42(15) . . . . ?
C5 P2 C41 C42 -73.97(19) . . . . ?
C31 P2 C41 C42 163.28(17) . . . . ?
P3 P2 C41 C42 37.43(19) . . . . ?
C5 P2 C41 C46 100.12(17) . . . . ?
C31 P2 C41 C46 -22.63(18) . . . . ?
P3 P2 C41 C46 -148.49(15) . . . . ?
C46 C41 C42 C43 1.5(4) . . . . ?
P2 C41 C42 C43 175.8(2) . . . . ?
C41 C42 C43 C44 -0.8(4) . . . . ?
C42 C43 C44 C45 -0.3(4) . . . . ?
C43 C44 C45 C46 0.8(4) . . . . ?
C42 C41 C46 C45 -1.1(3) . . . . ?
P2 C41 C46 C45 -175.11(17) . . . . ?
C44 C45 C46 C41 0.0(3) . . . . ?
C2 C3 C51 C52 -51.8(3) . . . . ?
C4 C3 C51 C52 129.1(2) . . . . ?
C2 C3 C51 C53 69.9(2) . . . . ?
C4 C3 C51 C53 -109.2(2) . . . . ?
C2 C3 C51 C54 -172.03(19) . . . . ?
C4 C3 C51 C54 8.8(3) . . . . ?

_refine_diff_density_max         0.568
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.067

####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1578546'
_audit_update_record             
;
2017-10-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H31 Co2 O6 P3'
_chemical_formula_sum            'C39 H31 Co2 O6 P3'
_chemical_formula_weight         806.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   10.6793(4)
_cell_length_b                   11.8419(5)
_cell_length_c                   14.9909(7)
_cell_angle_alpha                87.867(3)
_cell_angle_beta                 84.483(3)
_cell_angle_gamma                78.487(3)
_cell_volume                     1848.73(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    8670
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      65.26

_exptl_crystal_description       Plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_F_000             824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    8.632
_shelx_estimated_absorpt_T_min   0.378
_shelx_estimated_absorpt_T_max   0.846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_process_details   'SADABS; Bruker, 2016'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.24
_diffrn_reflns_number            51126
_diffrn_reflns_av_unetI/netI     0.0891
_diffrn_reflns_av_R_equivalents  0.1489
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.962
_diffrn_reflns_theta_max         65.381
_diffrn_reflns_theta_full        65.381
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measured_fraction_theta_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 0.965
_reflns_number_total             6131
_reflns_number_gt                4166
_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-2017/1 (Sheldrick, 2017)'
_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)+5.8070P] 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         6131
_refine_ls_number_parameters     454
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.1235
_refine_ls_wR_factor_gt          0.1102
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_restrained_S_all      1.172
_refine_ls_shift/su_max          0.000
_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
P1 P 0.41015(14) 0.72959(11) 0.69816(9) 0.0213(3) Uani 1 1 d . . . . .
P2 P 0.15664(14) 0.64980(11) 0.77956(9) 0.0209(3) Uani 1 1 d . . . . .
P3 P 0.20612(14) 0.81378(11) 0.72568(9) 0.0211(3) Uani 1 1 d . . . . .
C1 C 0.4222(5) 0.6016(4) 0.7604(3) 0.0212(13) Uani 1 1 d . . . . .
C2 C 0.5240(5) 0.5161(4) 0.7847(4) 0.0238(13) Uani 1 1 d . . . . .
H2 H 0.612426 0.517302 0.770970 0.029 Uiso 1 1 calc R U . . .
C3 C 0.4748(6) 0.4281(4) 0.8328(3) 0.0240(13) Uani 1 1 d . . . . .
C4 C 0.3412(6) 0.4583(4) 0.8380(4) 0.0252(14) Uani 1 1 d . . . . .
H4 H 0.283575 0.413743 0.866524 0.030 Uiso 1 1 calc R U . . .
C5 C 0.3056(5) 0.5653(4) 0.7941(3) 0.0207(13) Uani 1 1 d . . . . .
C11 C 0.5103(5) 0.8210(4) 0.7332(4) 0.0240(13) Uani 1 1 d . . . . .
C12 C 0.5795(6) 0.7907(5) 0.8068(4) 0.0314(15) Uani 1 1 d . . . . .
H12 H 0.574924 0.720583 0.838720 0.038 Uiso 1 1 calc R U . . .
C13 C 0.6554(6) 0.8624(5) 0.8338(4) 0.0396(17) Uani 1 1 d . . . . .
H13 H 0.703038 0.841887 0.884299 0.048 Uiso 1 1 calc R U . . .
C14 C 0.6616(7) 0.9638(5) 0.7872(5) 0.0434(17) Uani 1 1 d . . . . .
H14 H 0.715777 1.011846 0.805160 0.052 Uiso 1 1 calc R U . . .
C15 C 0.5910(6) 0.9970(5) 0.7153(4) 0.0399(17) Uani 1 1 d . . . . .
H15 H 0.595623 1.067737 0.684260 0.048 Uiso 1 1 calc R U . . .
C16 C 0.5131(6) 0.9263(5) 0.6885(4) 0.0291(14) Uani 1 1 d . . . . .
H16 H 0.461989 0.949288 0.639979 0.035 Uiso 1 1 calc R U . . .
C21 C 0.4497(5) 0.7064(4) 0.5797(3) 0.0229(13) Uani 1 1 d . . . . .
C22 C 0.3758(7) 0.6480(5) 0.5345(4) 0.0409(17) Uani 1 1 d . . . . .
H22 H 0.302637 0.624903 0.565136 0.049 Uiso 1 1 calc R U . . .
C23 C 0.4080(7) 0.6233(6) 0.4450(4) 0.053(2) Uani 1 1 d . . . . .
H23 H 0.356614 0.583338 0.414603 0.063 Uiso 1 1 calc R U . . .
C24 C 0.5132(7) 0.6556(6) 0.3993(4) 0.0432(18) Uani 1 1 d . . . . .
H24 H 0.534608 0.638062 0.337749 0.052 Uiso 1 1 calc R U . . .
C25 C 0.5866(6) 0.7133(5) 0.4432(4) 0.0395(17) Uani 1 1 d . . . . .
H25 H 0.659558 0.735870 0.411933 0.047 Uiso 1 1 calc R U . . .
C26 C 0.5557(6) 0.7391(5) 0.5331(4) 0.0286(14) Uani 1 1 d . . . . .
H26 H 0.607389 0.779546 0.562934 0.034 Uiso 1 1 calc R U . . .
C31 C 0.0596(5) 0.6691(4) 0.8848(3) 0.0211(13) Uani 1 1 d . . . . .
C32 C 0.0999(6) 0.7215(5) 0.9539(4) 0.0335(15) Uani 1 1 d . . . . .
H32 H 0.177056 0.750433 0.944646 0.040 Uiso 1 1 calc R U . . .
C33 C 0.0297(7) 0.7329(5) 1.0372(4) 0.0372(17) Uani 1 1 d . . . . .
H33 H 0.059217 0.768763 1.084572 0.045 Uiso 1 1 calc R U . . .
C34 C -0.0812(7) 0.6926(6) 1.0506(4) 0.0443(18) Uani 1 1 d . . . . .
H34 H -0.129925 0.700980 1.107272 0.053 Uiso 1 1 calc R U . . .
C35 C -0.1229(7) 0.6398(7) 0.9824(4) 0.057(2) Uani 1 1 d . . . . .
H35 H -0.200395 0.611553 0.992205 0.069 Uiso 1 1 calc R U . . .
C36 C -0.0529(6) 0.6273(6) 0.8993(4) 0.0401(17) Uani 1 1 d . . . . .
H36 H -0.082034 0.590206 0.852504 0.048 Uiso 1 1 calc R U . . .
C41 C 0.0663(5) 0.5879(4) 0.7065(3) 0.0223(13) Uani 1 1 d . . . . .
C42 C 0.1097(6) 0.4767(5) 0.6763(4) 0.0352(16) Uani 1 1 d . . . . .
H42 H 0.191210 0.435181 0.690565 0.042 Uiso 1 1 calc R U . . .
C43 C 0.0357(7) 0.4249(6) 0.6253(5) 0.051(2) Uani 1 1 d . . . . .
H43 H 0.066146 0.348242 0.605300 0.061 Uiso 1 1 calc R U . . .
C44 C -0.0810(8) 0.4848(6) 0.6041(5) 0.055(2) Uani 1 1 d . . . . .
H44 H -0.131355 0.449969 0.568554 0.067 Uiso 1 1 calc R U . . .
C45 C -0.1262(7) 0.5949(6) 0.6337(5) 0.0501(19) Uani 1 1 d . . . . .
H45 H -0.207897 0.635413 0.619004 0.060 Uiso 1 1 calc R U . . .
C46 C -0.0539(6) 0.6474(5) 0.6847(4) 0.0345(15) Uani 1 1 d . . . . .
H46 H -0.085824 0.723723 0.704954 0.041 Uiso 1 1 calc R U . . .
C51 C 0.5513(6) 0.3218(5) 0.8772(4) 0.0315(15) Uani 1 1 d . . . . .
C52 C 0.6788(6) 0.2800(5) 0.8238(5) 0.0477(19) Uani 1 1 d . . . . .
H52A H 0.664027 0.263361 0.762582 0.072 Uiso 1 1 calc R U . . .
H52B H 0.724320 0.209776 0.852180 0.072 Uiso 1 1 calc R U . . .
H52C H 0.730590 0.339786 0.822159 0.072 Uiso 1 1 calc R U . . .
C53 C 0.5720(8) 0.3503(6) 0.9722(4) 0.067(3) Uani 1 1 d . . . . .
H53A H 0.626224 0.408234 0.970069 0.100 Uiso 1 1 calc R U . . .
H53B H 0.614194 0.280312 1.002708 0.100 Uiso 1 1 calc R U . . .
H53C H 0.488975 0.380651 1.005093 0.100 Uiso 1 1 calc R U . . .
C54 C 0.4752(7) 0.2237(5) 0.8826(5) 0.0491(19) Uani 1 1 d . . . . .
H54A H 0.395624 0.246392 0.921481 0.074 Uiso 1 1 calc R U . . .
H54B H 0.527040 0.153898 0.907241 0.074 Uiso 1 1 calc R U . . .
H54C H 0.454645 0.208488 0.822412 0.074 Uiso 1 1 calc R U . . .
Co1 Co 0.10951(9) 0.92864(7) 0.63026(6) 0.0259(3) Uani 1 1 d . . . . .
Co2 Co 0.15423(9) 0.97267(7) 0.79624(6) 0.0247(2) Uani 1 1 d . . . . .
C61 C 0.0661(7) 0.8360(5) 0.5563(4) 0.0448(18) Uani 1 1 d . . . . .
O61 O 0.0390(6) 0.7756(4) 0.5059(3) 0.0712(17) Uani 1 1 d . . . . .
C62 C -0.0384(7) 1.0253(5) 0.6540(4) 0.0384(16) Uani 1 1 d . . . . .
O62 O -0.1339(5) 1.0894(4) 0.6661(3) 0.0637(15) Uani 1 1 d . . . . .
C63 C 0.2200(6) 0.9973(5) 0.5605(4) 0.0348(16) Uani 1 1 d . . . . .
O63 O 0.2845(5) 1.0416(4) 0.5118(3) 0.0618(15) Uani 1 1 d . . . . .
C64 C 0.2622(6) 0.9615(5) 0.8790(4) 0.0344(16) Uani 1 1 d . . . . .
O64 O 0.3308(5) 0.9560(4) 0.9344(3) 0.0536(13) Uani 1 1 d . . . . .
C65 C 0.0023(6) 0.9812(5) 0.8594(4) 0.0316(15) Uani 1 1 d . . . . .
O65 O -0.0930(5) 0.9909(4) 0.9047(3) 0.0504(13) Uani 1 1 d . . . . .
C66 C 0.1833(6) 1.1036(5) 0.7489(4) 0.0347(16) Uani 1 1 d . . . . .
O66 O 0.2050(5) 1.1906(4) 0.7208(3) 0.0593(15) 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
P1 C1 1.739(5) . ?
P1 C11 1.790(6) . ?
P1 C21 1.803(5) . ?
P1 P3 2.214(2) . ?
P2 C5 1.731(5) . ?
P2 C41 1.792(6) . ?
P2 C31 1.798(5) . ?
P2 P3 2.2166(19) . ?
P3 Co1 2.1306(16) . ?
P3 Co2 2.1413(16) . ?
C1 C2 1.396(7) . ?
C1 C5 1.438(8) . ?
C2 C3 1.404(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(8) . ?
C3 C51 1.526(7) . ?
C4 C5 1.405(7) . ?
C4 H4 0.9500 . ?
C11 C12 1.384(8) . ?
C11 C16 1.399(7) . ?
C12 C13 1.380(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.376(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.376(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(8) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.385(8) . ?
C21 C26 1.386(8) . ?
C22 C23 1.379(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.371(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.364(9) . ?
C24 H24 0.9500 . ?
C25 C26 1.387(8) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.373(8) . ?
C31 C36 1.383(8) . ?
C32 C33 1.390(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.358(9) . ?
C33 H33 0.9500 . ?
C34 C35 1.371(9) . ?
C34 H34 0.9500 . ?
C35 C36 1.387(8) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.384(7) . ?
C41 C46 1.398(8) . ?
C42 C43 1.389(8) . ?
C42 H42 0.9500 . ?
C43 C44 1.366(9) . ?
C43 H43 0.9500 . ?
C44 C45 1.371(9) . ?
C44 H44 0.9500 . ?
C45 C46 1.381(9) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C52 1.513(8) . ?
C51 C53 1.523(8) . ?
C51 C54 1.540(8) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
Co1 C61 1.744(7) . ?
Co1 C62 1.770(7) . ?
Co1 C63 1.797(7) . ?
Co1 Co2 2.6675(13) . ?
Co2 C66 1.753(6) . ?
Co2 C64 1.758(7) . ?
Co2 C65 1.785(7) . ?
C61 O61 1.154(7) . ?
C62 O62 1.147(7) . ?
C63 O63 1.140(7) . ?
C64 O64 1.151(7) . ?
C65 O65 1.156(7) . ?
C66 O66 1.156(6) . ?

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 P1 C11 112.6(3) . . ?
C1 P1 C21 112.8(2) . . ?
C11 P1 C21 107.8(3) . . ?
C1 P1 P3 103.54(19) . . ?
C11 P1 P3 109.50(18) . . ?
C21 P1 P3 110.60(19) . . ?
C5 P2 C41 113.4(3) . . ?
C5 P2 C31 110.5(2) . . ?
C41 P2 C31 105.8(3) . . ?
C5 P2 P3 102.57(19) . . ?
C41 P2 P3 112.77(18) . . ?
C31 P2 P3 111.92(18) . . ?
Co1 P3 Co2 77.28(6) . . ?
Co1 P3 P1 121.20(8) . . ?
Co2 P3 P1 120.64(8) . . ?
Co1 P3 P2 127.24(9) . . ?
Co2 P3 P2 123.31(8) . . ?
P1 P3 P2 91.14(7) . . ?
C2 C1 C5 107.1(5) . . ?
C2 C1 P1 134.6(4) . . ?
C5 C1 P1 118.2(4) . . ?
C1 C2 C3 109.1(5) . . ?
C1 C2 H2 125.4 . . ?
C3 C2 H2 125.4 . . ?
C4 C3 C2 107.7(5) . . ?
C4 C3 C51 125.2(5) . . ?
C2 C3 C51 127.0(5) . . ?
C3 C4 C5 109.0(5) . . ?
C3 C4 H4 125.5 . . ?
C5 C4 H4 125.5 . . ?
C4 C5 C1 107.0(5) . . ?
C4 C5 P2 131.5(4) . . ?
C1 C5 P2 121.5(4) . . ?
C12 C11 C16 120.0(5) . . ?
C12 C11 P1 120.4(4) . . ?
C16 C11 P1 119.5(4) . . ?
C13 C12 C11 119.9(6) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C14 C13 C12 119.7(6) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C15 C14 C13 121.3(6) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C15 C16 119.4(6) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C15 C16 C11 119.6(6) . . ?
C15 C16 H16 120.2 . . ?
C11 C16 H16 120.2 . . ?
C22 C21 C26 118.6(5) . . ?
C22 C21 P1 118.8(4) . . ?
C26 C21 P1 122.5(4) . . ?
C23 C22 C21 120.1(6) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 121.1(6) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C25 C24 C23 119.3(6) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C24 C25 C26 120.6(6) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C21 C26 C25 120.4(6) . . ?
C21 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C32 C31 C36 118.8(5) . . ?
C32 C31 P2 119.8(4) . . ?
C36 C31 P2 121.3(4) . . ?
C31 C32 C33 121.1(6) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C34 C33 C32 119.7(6) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 120.0(6) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C34 C35 C36 120.6(6) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
C31 C36 C35 119.8(6) . . ?
C31 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C42 C41 C46 118.6(5) . . ?
C42 C41 P2 120.5(4) . . ?
C46 C41 P2 120.7(4) . . ?
C41 C42 C43 120.9(6) . . ?
C41 C42 H42 119.5 . . ?
C43 C42 H42 119.5 . . ?
C44 C43 C42 119.6(6) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C45 120.5(7) . . ?
C43 C44 H44 119.8 . . ?
C45 C44 H44 119.8 . . ?
C44 C45 C46 120.6(7) . . ?
C44 C45 H45 119.7 . . ?
C46 C45 H45 119.7 . . ?
C45 C46 C41 119.8(6) . . ?
C45 C46 H46 120.1 . . ?
C41 C46 H46 120.1 . . ?
C52 C51 C53 110.4(6) . . ?
C52 C51 C3 111.0(5) . . ?
C53 C51 C3 109.4(5) . . ?
C52 C51 C54 108.1(5) . . ?
C53 C51 C54 108.2(6) . . ?
C3 C51 C54 109.6(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 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C61 Co1 C62 101.0(3) . . ?
C61 Co1 C63 102.6(3) . . ?
C62 Co1 C63 110.7(3) . . ?
C61 Co1 P3 103.2(2) . . ?
C62 Co1 P3 124.8(2) . . ?
C63 Co1 P3 111.2(2) . . ?
C61 Co1 Co2 149.1(2) . . ?
C62 Co1 Co2 84.8(2) . . ?
C63 Co1 Co2 103.56(19) . . ?
P3 Co1 Co2 51.54(5) . . ?
C66 Co2 C64 96.4(3) . . ?
C66 Co2 C65 115.0(3) . . ?
C64 Co2 C65 103.5(3) . . ?
C66 Co2 P3 122.6(2) . . ?
C64 Co2 P3 105.49(19) . . ?
C65 Co2 P3 110.29(19) . . ?
C66 Co2 Co1 84.4(2) . . ?
C64 Co2 Co1 149.1(2) . . ?
C65 Co2 Co1 104.1(2) . . ?
P3 Co2 Co1 51.18(5) . . ?
O61 C61 Co1 178.5(6) . . ?
O62 C62 Co1 177.4(6) . . ?
O63 C63 Co1 175.3(6) . . ?
O64 C64 Co2 178.4(6) . . ?
O65 C65 Co2 175.3(6) . . ?
O66 C66 Co2 177.1(6) . . ?

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 C1 C2 -50.7(6) . . . . ?
C21 P1 C1 C2 71.6(6) . . . . ?
P3 P1 C1 C2 -168.9(5) . . . . ?
C11 P1 C1 C5 132.8(4) . . . . ?
C21 P1 C1 C5 -104.9(4) . . . . ?
P3 P1 C1 C5 14.6(4) . . . . ?
C5 C1 C2 C3 -0.3(6) . . . . ?
P1 C1 C2 C3 -177.0(4) . . . . ?
C1 C2 C3 C4 0.5(6) . . . . ?
C1 C2 C3 C51 -175.9(5) . . . . ?
C2 C3 C4 C5 -0.5(6) . . . . ?
C51 C3 C4 C5 175.9(5) . . . . ?
C3 C4 C5 C1 0.3(6) . . . . ?
C3 C4 C5 P2 -178.3(4) . . . . ?
C2 C1 C5 C4 0.0(6) . . . . ?
P1 C1 C5 C4 177.4(4) . . . . ?
C2 C1 C5 P2 178.8(4) . . . . ?
P1 C1 C5 P2 -3.8(6) . . . . ?
C41 P2 C5 C4 -68.8(6) . . . . ?
C31 P2 C5 C4 49.8(6) . . . . ?
P3 P2 C5 C4 169.3(5) . . . . ?
C41 P2 C5 C1 112.8(4) . . . . ?
C31 P2 C5 C1 -128.6(4) . . . . ?
P3 P2 C5 C1 -9.1(5) . . . . ?
C1 P1 C11 C12 -4.4(5) . . . . ?
C21 P1 C11 C12 -129.4(5) . . . . ?
P3 P1 C11 C12 110.2(4) . . . . ?
C1 P1 C11 C16 178.8(4) . . . . ?
C21 P1 C11 C16 53.7(5) . . . . ?
P3 P1 C11 C16 -66.6(5) . . . . ?
C16 C11 C12 C13 -2.5(9) . . . . ?
P1 C11 C12 C13 -179.3(5) . . . . ?
C11 C12 C13 C14 0.0(9) . . . . ?
C12 C13 C14 C15 1.7(10) . . . . ?
C13 C14 C15 C16 -0.7(10) . . . . ?
C14 C15 C16 C11 -1.8(9) . . . . ?
C12 C11 C16 C15 3.5(8) . . . . ?
P1 C11 C16 C15 -179.7(4) . . . . ?
C1 P1 C21 C22 61.8(5) . . . . ?
C11 P1 C21 C22 -173.3(5) . . . . ?
P3 P1 C21 C22 -53.6(5) . . . . ?
C1 P1 C21 C26 -114.6(5) . . . . ?
C11 P1 C21 C26 10.4(5) . . . . ?
P3 P1 C21 C26 130.0(4) . . . . ?
C26 C21 C22 C23 0.1(9) . . . . ?
P1 C21 C22 C23 -176.4(5) . . . . ?
C21 C22 C23 C24 0.1(11) . . . . ?
C22 C23 C24 C25 -0.1(11) . . . . ?
C23 C24 C25 C26 0.0(10) . . . . ?
C22 C21 C26 C25 -0.3(9) . . . . ?
P1 C21 C26 C25 176.1(5) . . . . ?
C24 C25 C26 C21 0.2(9) . . . . ?
C5 P2 C31 C32 60.5(5) . . . . ?
C41 P2 C31 C32 -176.3(4) . . . . ?
P3 P2 C31 C32 -53.1(5) . . . . ?
C5 P2 C31 C36 -116.4(5) . . . . ?
C41 P2 C31 C36 6.7(5) . . . . ?
P3 P2 C31 C36 129.9(5) . . . . ?
C36 C31 C32 C33 -0.1(9) . . . . ?
P2 C31 C32 C33 -177.1(4) . . . . ?
C31 C32 C33 C34 -0.6(9) . . . . ?
C32 C33 C34 C35 0.7(10) . . . . ?
C33 C34 C35 C36 -0.2(12) . . . . ?
C32 C31 C36 C35 0.5(9) . . . . ?
P2 C31 C36 C35 177.5(5) . . . . ?
C34 C35 C36 C31 -0.4(11) . . . . ?
C5 P2 C41 C42 7.7(6) . . . . ?
C31 P2 C41 C42 -113.6(5) . . . . ?
P3 P2 C41 C42 123.8(4) . . . . ?
C5 P2 C41 C46 -177.4(4) . . . . ?
C31 P2 C41 C46 61.3(5) . . . . ?
P3 P2 C41 C46 -61.3(5) . . . . ?
C46 C41 C42 C43 0.0(9) . . . . ?
P2 C41 C42 C43 175.0(5) . . . . ?
C41 C42 C43 C44 0.5(11) . . . . ?
C42 C43 C44 C45 -0.8(12) . . . . ?
C43 C44 C45 C46 0.6(12) . . . . ?
C44 C45 C46 C41 -0.1(10) . . . . ?
C42 C41 C46 C45 -0.3(9) . . . . ?
P2 C41 C46 C45 -175.3(5) . . . . ?
C4 C3 C51 C52 150.3(6) . . . . ?
C2 C3 C51 C52 -34.0(8) . . . . ?
C4 C3 C51 C53 -87.6(7) . . . . ?
C2 C3 C51 C53 88.1(7) . . . . ?
C4 C3 C51 C54 30.9(7) . . . . ?
C2 C3 C51 C54 -153.4(6) . . . . ?

_refine_diff_density_max         0.546
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.087

####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1578540'
_audit_update_record             
;
2017-10-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H31 Cr O5 P3'
_chemical_formula_sum            'C38 H31 Cr O5 P3'
_chemical_formula_weight         712.54

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'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   11.2512(8)
_cell_length_b                   11.7421(7)
_cell_length_c                   15.0867(10)
_cell_angle_alpha                91.279(3)
_cell_angle_beta                 101.068(3)
_cell_angle_gamma                114.470(2)
_cell_volume                     1768.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    9150
_cell_measurement_theta_min      3.30
_cell_measurement_theta_max      27.54

_exptl_crystal_description       Block
_exptl_crystal_colour            gold
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_F_000             736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.298
_exptl_absorpt_coefficient_mu    0.501
_shelx_estimated_absorpt_T_min   0.814
_shelx_estimated_absorpt_T_max   0.865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_process_details   'SADABS; Bruker, 2015'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            78418
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.055
_diffrn_reflns_theta_max         27.569
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8157
_reflns_number_gt                6809
_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-2016/6 (Sheldrick, 2016)'
_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)+(0.0340P)²+1.1169P] 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         8157
_refine_ls_number_parameters     427
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0786
_refine_ls_wR_factor_gt          0.0727
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.000
_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
P1 P 0.37347(4) 0.43866(3) 0.21969(2) 0.01495(8) Uani 1 1 d . . . . .
P2 P 0.30261(4) 0.65873(3) 0.26538(2) 0.01533(8) Uani 1 1 d . . . . .
P3 P 0.19865(4) 0.47784(3) 0.18220(2) 0.01694(8) Uani 1 1 d . . . . .
C1 C 0.50344(14) 0.58599(13) 0.26325(9) 0.0162(3) Uani 1 1 d . . . . .
C2 C 0.47023(14) 0.68768(13) 0.28065(9) 0.0164(3) Uani 1 1 d . . . . .
C3 C 0.59070(14) 0.79596(13) 0.31219(10) 0.0187(3) Uani 1 1 d . . . . .
H3 H 0.598626 0.877514 0.329524 0.022 Uiso 1 1 calc R U . . .
C4 C 0.69727(14) 0.76253(13) 0.31359(9) 0.0169(3) Uani 1 1 d . . . . .
C5 C 0.64313(14) 0.63275(13) 0.28407(10) 0.0184(3) Uani 1 1 d . . . . .
H5 H 0.692892 0.585262 0.279162 0.022 Uiso 1 1 calc R U . . .
C11 C 0.39544(15) 0.37535(13) 0.11651(10) 0.0213(3) Uani 1 1 d . . . . .
C12 C 0.32917(18) 0.38678(16) 0.03189(11) 0.0297(4) Uani 1 1 d . . . . .
H12 H 0.266672 0.422458 0.027930 0.036 Uiso 1 1 calc R U . . .
C13 C 0.3538(2) 0.34636(19) -0.04685(13) 0.0427(5) Uani 1 1 d . . . . .
H13 H 0.307841 0.354179 -0.104500 0.051 Uiso 1 1 calc R U . . .
C14 C 0.4441(2) 0.29523(19) -0.04185(15) 0.0479(6) Uani 1 1 d . . . . .
H14 H 0.460394 0.267540 -0.096021 0.057 Uiso 1 1 calc R U . . .
C15 C 0.5114(2) 0.28381(19) 0.04167(16) 0.0464(5) Uani 1 1 d . . . . .
H15 H 0.574499 0.248929 0.044746 0.056 Uiso 1 1 calc R U . . .
C16 C 0.48734(19) 0.32326(16) 0.12163(13) 0.0330(4) Uani 1 1 d . . . . .
H16 H 0.533177 0.314692 0.179077 0.040 Uiso 1 1 calc R U . . .
C21 C 0.36746(14) 0.32492(13) 0.29937(10) 0.0189(3) Uani 1 1 d . . . . .
C22 C 0.42049(17) 0.36677(16) 0.39162(11) 0.0286(4) Uani 1 1 d . . . . .
H22 H 0.462341 0.454393 0.411767 0.034 Uiso 1 1 calc R U . . .
C23 C 0.4121(2) 0.28035(18) 0.45385(12) 0.0374(4) Uani 1 1 d . . . . .
H23 H 0.446611 0.308696 0.516866 0.045 Uiso 1 1 calc R U . . .
C24 C 0.3536(2) 0.15308(18) 0.42453(13) 0.0379(4) Uani 1 1 d . . . . .
H24 H 0.349385 0.094232 0.467384 0.046 Uiso 1 1 calc R U . . .
C25 C 0.30104(19) 0.11088(16) 0.33318(13) 0.0338(4) Uani 1 1 d . . . . .
H25 H 0.260630 0.023180 0.313416 0.041 Uiso 1 1 calc R U . . .
C26 C 0.30723(16) 0.19627(14) 0.27040(11) 0.0250(3) Uani 1 1 d . . . . .
H26 H 0.270447 0.167166 0.207641 0.030 Uiso 1 1 calc R U . . .
C31 C 0.26760(15) 0.77268(13) 0.19929(10) 0.0187(3) Uani 1 1 d . . . . .
C32 C 0.13951(17) 0.76799(17) 0.17915(11) 0.0276(3) Uani 1 1 d . . . . .
H32 H 0.070663 0.708846 0.204128 0.033 Uiso 1 1 calc R U . . .
C33 C 0.11261(19) 0.84996(18) 0.12246(12) 0.0334(4) Uani 1 1 d . . . . .
H33 H 0.024857 0.845906 0.108108 0.040 Uiso 1 1 calc R U . . .
C34 C 0.21233(19) 0.93716(16) 0.08688(11) 0.0305(4) Uani 1 1 d . . . . .
H34 H 0.193276 0.993074 0.048250 0.037 Uiso 1 1 calc R U . . .
C35 C 0.33954(19) 0.94318(16) 0.10735(13) 0.0339(4) Uani 1 1 d . . . . .
H35 H 0.408329 1.003886 0.083214 0.041 Uiso 1 1 calc R U . . .
C36 C 0.36795(17) 0.86072(15) 0.16326(12) 0.0269(3) Uani 1 1 d . . . . .
H36 H 0.455679 0.864648 0.176738 0.032 Uiso 1 1 calc R U . . .
C41 C 0.26123(15) 0.67202(15) 0.37422(10) 0.0217(3) Uani 1 1 d . . . . .
C42 C 0.2345(2) 0.57123(18) 0.42523(12) 0.0393(4) Uani 1 1 d . . . . .
H42 H 0.228658 0.493671 0.400151 0.047 Uiso 1 1 calc R U . . .
C43 C 0.2161(2) 0.5829(2) 0.51269(14) 0.0519(6) Uani 1 1 d . . . . .
H43 H 0.196898 0.513289 0.547262 0.062 Uiso 1 1 calc R U . . .
C44 C 0.2259(3) 0.6957(2) 0.54917(14) 0.0533(6) Uani 1 1 d . . . . .
H44 H 0.211920 0.703585 0.608693 0.064 Uiso 1 1 calc R U . . .
C45 C 0.2558(3) 0.7964(3) 0.49993(15) 0.0647(8) Uani 1 1 d . . . . .
H45 H 0.264738 0.874700 0.526115 0.078 Uiso 1 1 calc R U . . .
C46 C 0.2731(3) 0.7854(2) 0.41201(13) 0.0464(6) Uani 1 1 d . . . . .
H46 H 0.293142 0.855552 0.378013 0.056 Uiso 1 1 calc R U . . .
C51 C 0.84428(15) 0.85325(14) 0.33663(11) 0.0226(3) Uani 1 1 d . . . . .
C52 C 0.8879(2) 0.8977(3) 0.24928(14) 0.0588(7) Uani 1 1 d . . . . .
H52A H 0.882047 0.826258 0.210936 0.088 Uiso 1 1 calc R U . . .
H52B H 0.980496 0.962455 0.264049 0.088 Uiso 1 1 calc R U . . .
H52C H 0.829238 0.932942 0.216627 0.088 Uiso 1 1 calc R U . . .
C53 C 0.9293(2) 0.79190(19) 0.38625(19) 0.0534(6) Uani 1 1 d . . . . .
H53A H 0.896782 0.759783 0.440507 0.080 Uiso 1 1 calc R U . . .
H53B H 1.022790 0.854293 0.404294 0.080 Uiso 1 1 calc R U . . .
H53C H 0.923014 0.722101 0.345917 0.080 Uiso 1 1 calc R U . . .
C54 C 0.86771(19) 0.96944(18) 0.39759(16) 0.0442(5) Uani 1 1 d . . . . .
H54A H 0.818263 1.013584 0.365397 0.066 Uiso 1 1 calc R U . . .
H54B H 0.963546 1.025786 0.413180 0.066 Uiso 1 1 calc R U . . .
H54C H 0.836362 0.943557 0.453326 0.066 Uiso 1 1 calc R U . . .
Cr Cr -0.02036(2) 0.31863(2) 0.19390(2) 0.02095(7) Uani 1 1 d . . . . .
C61 C -0.19096(18) 0.19609(18) 0.19078(14) 0.0386(4) Uani 1 1 d . . . . .
O61 O -0.29715(15) 0.12133(16) 0.18860(14) 0.0665(5) Uani 1 1 d . . . . .
C62 C -0.08840(17) 0.36312(16) 0.08119(12) 0.0307(4) Uani 1 1 d . . . . .
O62 O -0.13559(16) 0.38808(16) 0.01545(10) 0.0538(4) Uani 1 1 d . . . . .
C63 C -0.06357(18) 0.43573(17) 0.25238(13) 0.0335(4) Uani 1 1 d . . . . .
O63 O -0.09708(17) 0.50258(15) 0.28499(12) 0.0568(4) Uani 1 1 d . . . . .
C64 C 0.04638(17) 0.27807(15) 0.30854(12) 0.0287(4) Uani 1 1 d . . . . .
O64 O 0.08332(15) 0.25371(13) 0.37809(9) 0.0455(4) Uani 1 1 d . . . . .
C65 C 0.01586(16) 0.19745(15) 0.13209(11) 0.0269(3) Uani 1 1 d . . . . .
O65 O 0.03359(14) 0.12237(13) 0.09469(9) 0.0417(3) 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
P1 C1 1.7457(14) . ?
P1 C21 1.8059(14) . ?
P1 C11 1.8126(15) . ?
P1 P3 2.1759(5) . ?
P2 C2 1.7389(14) . ?
P2 C41 1.8109(15) . ?
P2 C31 1.8125(15) . ?
P2 P3 2.1711(5) . ?
P3 Cr 2.4420(5) . ?
C1 C5 1.399(2) . ?
C1 C2 1.4240(19) . ?
C2 C3 1.4064(19) . ?
C3 C4 1.405(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.410(2) . ?
C4 C51 1.515(2) . ?
C5 H5 0.9500 . ?
C11 C12 1.389(2) . ?
C11 C16 1.395(2) . ?
C12 C13 1.387(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.370(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.380(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.396(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C26 1.393(2) . ?
C21 C22 1.394(2) . ?
C22 C23 1.385(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.381(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.385(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C36 1.390(2) . ?
C31 C32 1.392(2) . ?
C32 C33 1.389(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.378(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.376(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.393(2) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C46 1.380(2) . ?
C41 C42 1.385(2) . ?
C42 C43 1.386(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.376(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.368(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.388(3) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C53 1.521(2) . ?
C51 C52 1.522(2) . ?
C51 C54 1.526(2) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
Cr C61 1.8523(19) . ?
Cr C63 1.8893(19) . ?
Cr C64 1.9017(18) . ?
Cr C62 1.9030(18) . ?
Cr C65 1.9046(17) . ?
C61 O61 1.146(2) . ?
C62 O62 1.136(2) . ?
C63 O63 1.140(2) . ?
C64 O64 1.140(2) . ?
C65 O65 1.141(2) . ?

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 P1 C21 110.77(7) . . ?
C1 P1 C11 112.23(7) . . ?
C21 P1 C11 105.65(7) . . ?
C1 P1 P3 103.69(5) . . ?
C21 P1 P3 117.58(5) . . ?
C11 P1 P3 107.03(5) . . ?
C2 P2 C41 110.25(7) . . ?
C2 P2 C31 110.97(7) . . ?
C41 P2 C31 107.23(7) . . ?
C2 P2 P3 103.27(5) . . ?
C41 P2 P3 117.95(5) . . ?
C31 P2 P3 107.10(5) . . ?
P2 P3 P1 91.081(19) . . ?
P2 P3 Cr 123.94(2) . . ?
P1 P3 Cr 119.382(19) . . ?
C5 C1 C2 107.82(12) . . ?
C5 C1 P1 133.75(11) . . ?
C2 C1 P1 118.39(11) . . ?
C3 C2 C1 107.69(12) . . ?
C3 C2 P2 133.13(11) . . ?
C1 C2 P2 119.12(11) . . ?
C4 C3 C2 108.10(12) . . ?
C4 C3 H3 125.9 . . ?
C2 C3 H3 125.9 . . ?
C3 C4 C5 108.18(12) . . ?
C3 C4 C51 125.26(13) . . ?
C5 C4 C51 126.43(13) . . ?
C1 C5 C4 108.19(12) . . ?
C1 C5 H5 125.9 . . ?
C4 C5 H5 125.9 . . ?
C12 C11 C16 119.42(15) . . ?
C12 C11 P1 120.59(12) . . ?
C16 C11 P1 119.81(13) . . ?
C13 C12 C11 120.31(18) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 120.3(2) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.18(17) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C16 120.33(19) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C11 C16 C15 119.46(18) . . ?
C11 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C26 C21 C22 119.66(14) . . ?
C26 C21 P1 121.08(12) . . ?
C22 C21 P1 119.23(11) . . ?
C23 C22 C21 119.85(15) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C24 C23 C22 120.15(17) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.33(16) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C24 C25 C26 120.07(16) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 119.92(15) . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
C36 C31 C32 119.54(14) . . ?
C36 C31 P2 119.42(11) . . ?
C32 C31 P2 120.90(12) . . ?
C33 C32 C31 119.85(16) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C34 C33 C32 120.46(16) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C35 C34 C33 119.96(15) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C34 C35 C36 120.35(16) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C31 C36 C35 119.83(15) . . ?
C31 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C46 C41 C42 119.45(15) . . ?
C46 C41 P2 121.02(13) . . ?
C42 C41 P2 118.97(13) . . ?
C41 C42 C43 120.37(18) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 H42 119.8 . . ?
C44 C43 C42 119.70(19) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C45 C44 C43 120.13(18) . . ?
C45 C44 H44 119.9 . . ?
C43 C44 H44 119.9 . . ?
C44 C45 C46 120.6(2) . . ?
C44 C45 H45 119.7 . . ?
C46 C45 H45 119.7 . . ?
C41 C46 C45 119.73(18) . . ?
C41 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C4 C51 C53 111.18(14) . . ?
C4 C51 C52 108.95(13) . . ?
C53 C51 C52 110.53(19) . . ?
C4 C51 C54 110.66(13) . . ?
C53 C51 C54 108.03(16) . . ?
C52 C51 C54 107.43(17) . . ?
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 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C61 Cr C63 88.90(8) . . ?
C61 Cr C64 91.13(8) . . ?
C63 Cr C64 90.43(8) . . ?
C61 Cr C62 88.87(8) . . ?
C63 Cr C62 87.70(8) . . ?
C64 Cr C62 178.13(8) . . ?
C61 Cr C65 89.20(8) . . ?
C63 Cr C65 177.65(8) . . ?
C64 Cr C65 90.98(7) . . ?
C62 Cr C65 90.88(7) . . ?
C61 Cr P3 174.53(7) . . ?
C63 Cr P3 93.42(5) . . ?
C64 Cr P3 93.80(5) . . ?
C62 Cr P3 86.28(5) . . ?
C65 Cr P3 88.35(5) . . ?
O61 C61 Cr 179.16(19) . . ?
O62 C62 Cr 176.13(17) . . ?
O63 C63 Cr 176.06(18) . . ?
O64 C64 Cr 178.05(16) . . ?
O65 C65 Cr 177.93(15) . . ?

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
C21 P1 C1 C5 66.58(16) . . . . ?
C11 P1 C1 C5 -51.24(17) . . . . ?
P3 P1 C1 C5 -166.40(14) . . . . ?
C21 P1 C1 C2 -116.03(12) . . . . ?
C11 P1 C1 C2 126.15(12) . . . . ?
P3 P1 C1 C2 10.99(12) . . . . ?
C5 C1 C2 C3 -0.07(16) . . . . ?
P1 C1 C2 C3 -178.10(10) . . . . ?
C5 C1 C2 P2 -177.60(10) . . . . ?
P1 C1 C2 P2 4.38(16) . . . . ?
C41 P2 C2 C3 -67.19(16) . . . . ?
C31 P2 C2 C3 51.46(16) . . . . ?
P3 P2 C2 C3 165.91(14) . . . . ?
C41 P2 C2 C1 109.57(12) . . . . ?
C31 P2 C2 C1 -131.77(11) . . . . ?
P3 P2 C2 C1 -17.32(12) . . . . ?
C1 C2 C3 C4 0.54(16) . . . . ?
P2 C2 C3 C4 177.58(12) . . . . ?
C2 C3 C4 C5 -0.81(16) . . . . ?
C2 C3 C4 C51 175.27(13) . . . . ?
C2 C1 C5 C4 -0.42(16) . . . . ?
P1 C1 C5 C4 177.17(12) . . . . ?
C3 C4 C5 C1 0.76(16) . . . . ?
C51 C4 C5 C1 -175.25(13) . . . . ?
C1 P1 C11 C12 -98.25(14) . . . . ?
C21 P1 C11 C12 140.93(13) . . . . ?
P3 P1 C11 C12 14.87(14) . . . . ?
C1 P1 C11 C16 76.82(14) . . . . ?
C21 P1 C11 C16 -44.00(14) . . . . ?
P3 P1 C11 C16 -170.06(12) . . . . ?
C16 C11 C12 C13 0.2(2) . . . . ?
P1 C11 C12 C13 175.31(13) . . . . ?
C11 C12 C13 C14 -0.2(3) . . . . ?
C12 C13 C14 C15 -0.1(3) . . . . ?
C13 C14 C15 C16 0.5(3) . . . . ?
C12 C11 C16 C15 0.2(3) . . . . ?
P1 C11 C16 C15 -174.96(14) . . . . ?
C14 C15 C16 C11 -0.5(3) . . . . ?
C1 P1 C21 C26 -157.43(13) . . . . ?
C11 P1 C21 C26 -35.66(15) . . . . ?
P3 P1 C21 C26 83.64(13) . . . . ?
C1 P1 C21 C22 24.52(15) . . . . ?
C11 P1 C21 C22 146.29(13) . . . . ?
P3 P1 C21 C22 -94.41(13) . . . . ?
C26 C21 C22 C23 -0.5(3) . . . . ?
P1 C21 C22 C23 177.57(14) . . . . ?
C21 C22 C23 C24 1.2(3) . . . . ?
C22 C23 C24 C25 -1.1(3) . . . . ?
C23 C24 C25 C26 0.2(3) . . . . ?
C24 C25 C26 C21 0.5(3) . . . . ?
C22 C21 C26 C25 -0.4(2) . . . . ?
P1 C21 C26 C25 -178.40(13) . . . . ?
C2 P2 C31 C36 4.64(15) . . . . ?
C41 P2 C31 C36 125.11(13) . . . . ?
P3 P2 C31 C36 -107.39(12) . . . . ?
C2 P2 C31 C32 -179.61(12) . . . . ?
C41 P2 C31 C32 -59.14(14) . . . . ?
P3 P2 C31 C32 68.35(13) . . . . ?
C36 C31 C32 C33 0.8(2) . . . . ?
P2 C31 C32 C33 -174.92(13) . . . . ?
C31 C32 C33 C34 -0.8(3) . . . . ?
C32 C33 C34 C35 0.1(3) . . . . ?
C33 C34 C35 C36 0.6(3) . . . . ?
C32 C31 C36 C35 -0.1(2) . . . . ?
P2 C31 C36 C35 175.71(13) . . . . ?
C34 C35 C36 C31 -0.6(3) . . . . ?
C2 P2 C41 C46 90.52(17) . . . . ?
C31 P2 C41 C46 -30.40(17) . . . . ?
P3 P2 C41 C46 -151.27(15) . . . . ?
C2 P2 C41 C42 -80.90(15) . . . . ?
C31 P2 C41 C42 158.18(14) . . . . ?
P3 P2 C41 C42 37.32(16) . . . . ?
C46 C41 C42 C43 1.8(3) . . . . ?
P2 C41 C42 C43 173.31(17) . . . . ?
C41 C42 C43 C44 -0.6(4) . . . . ?
C42 C43 C44 C45 -1.1(4) . . . . ?
C43 C44 C45 C46 1.7(4) . . . . ?
C42 C41 C46 C45 -1.2(3) . . . . ?
P2 C41 C46 C45 -172.6(2) . . . . ?
C44 C45 C46 C41 -0.5(4) . . . . ?
C3 C4 C51 C53 145.69(17) . . . . ?
C5 C4 C51 C53 -38.9(2) . . . . ?
C3 C4 C51 C52 -92.3(2) . . . . ?
C5 C4 C51 C52 83.1(2) . . . . ?
C3 C4 C51 C54 25.6(2) . . . . ?
C5 C4 C51 C54 -159.01(16) . . . . ?

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
C42 H42 O64 0.95 2.58 3.386(2) 142.8 .

_refine_diff_density_max         0.345
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_shelx_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 1578543'
_audit_update_record             
;
2017-10-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H31 Mo O5 P3'
_chemical_formula_sum            'C38 H31 Mo O5 P3'
_chemical_formula_weight         756.48

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'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   11.3621(5)
_cell_length_b                   11.7938(6)
_cell_length_c                   15.1337(8)
_cell_angle_alpha                91.699(2)
_cell_angle_beta                 100.767(2)
_cell_angle_gamma                114.322(2)
_cell_volume                     1802.51(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    9641
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      30.52

_exptl_crystal_description       Plate
_exptl_crystal_colour            gold
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_F_000             772
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.284
_exptl_crystal_size_min          0.076
_exptl_absorpt_coefficient_mu    0.538
_shelx_estimated_absorpt_T_min   0.828
_shelx_estimated_absorpt_T_max   0.960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_process_details   'SADABS; Bruker, 2016'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            106804
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.760
_diffrn_reflns_theta_max         30.577
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11029
_reflns_number_gt                9654
_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-2017/1 (Sheldrick, 2017)'
_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)+(0.0333P)²+0.9940P] 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         11029
_refine_ls_number_parameters     427
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0711
_refine_ls_wR_factor_gt          0.0669
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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
P1 P 0.31003(3) 0.66201(3) 0.26543(2) 0.01629(6) Uani 1 1 d . . . . .
P2 P 0.37948(3) 0.44206(3) 0.22034(2) 0.01613(6) Uani 1 1 d . . . . .
P3 P 0.20779(3) 0.48180(3) 0.18334(2) 0.01832(6) Uani 1 1 d . . . . .
C1 C 0.47573(12) 0.69067(11) 0.28098(8) 0.0171(2) Uani 1 1 d . . . . .
C2 C 0.59505(12) 0.79819(11) 0.31190(9) 0.0198(2) Uani 1 1 d . . . . .
H2 H 0.603162 0.879706 0.328922 0.024 Uiso 1 1 calc R U . . .
C3 C 0.70047(12) 0.76416(11) 0.31325(8) 0.0181(2) Uani 1 1 d . . . . .
C4 C 0.64671(12) 0.63462(11) 0.28435(9) 0.0197(2) Uani 1 1 d . . . . .
H4 H 0.695692 0.586874 0.279638 0.024 Uiso 1 1 calc R U . . .
C5 C 0.50820(12) 0.58857(11) 0.26376(8) 0.0174(2) Uani 1 1 d . . . . .
C11 C 0.26692(13) 0.67547(13) 0.37338(9) 0.0233(2) Uani 1 1 d . . . . .
C12 C 0.2386(2) 0.57450(16) 0.42361(11) 0.0403(4) Uani 1 1 d . . . . .
H12 H 0.233584 0.497347 0.398638 0.048 Uiso 1 1 calc R U . . .
C13 C 0.2176(2) 0.5862(2) 0.51056(13) 0.0551(6) Uani 1 1 d . . . . .
H13 H 0.197082 0.516832 0.544652 0.066 Uiso 1 1 calc R U . . .
C14 C 0.2269(3) 0.6989(2) 0.54688(13) 0.0576(6) Uani 1 1 d . . . . .
H14 H 0.211328 0.706767 0.605799 0.069 Uiso 1 1 calc R U . . .
C15 C 0.2584(3) 0.7997(2) 0.49828(14) 0.0677(8) Uani 1 1 d . . . . .
H15 H 0.266794 0.877615 0.524403 0.081 Uiso 1 1 calc R U . . .
C16 C 0.2782(2) 0.78871(19) 0.41122(12) 0.0478(5) Uani 1 1 d . . . . .
H16 H 0.299370 0.858696 0.377752 0.057 Uiso 1 1 calc R U . . .
C21 C 0.27459(13) 0.77471(11) 0.19991(8) 0.0194(2) Uani 1 1 d . . . . .
C22 C 0.37310(14) 0.86303(13) 0.16398(10) 0.0276(3) Uani 1 1 d . . . . .
H22 H 0.460206 0.867759 0.177074 0.033 Uiso 1 1 calc R U . . .
C23 C 0.34382(17) 0.94464(15) 0.10871(12) 0.0348(3) Uani 1 1 d . . . . .
H23 H 0.411376 1.005584 0.084728 0.042 Uiso 1 1 calc R U . . .
C24 C 0.21704(17) 0.93723(14) 0.08870(10) 0.0323(3) Uani 1 1 d . . . . .
H24 H 0.197196 0.992229 0.050335 0.039 Uiso 1 1 calc R U . . .
C25 C 0.11911(17) 0.84987(16) 0.12445(11) 0.0341(3) Uani 1 1 d . . . . .
H25 H 0.031993 0.845078 0.110709 0.041 Uiso 1 1 calc R U . . .
C26 C 0.14731(15) 0.76899(15) 0.18037(10) 0.0290(3) Uani 1 1 d . . . . .
H26 H 0.079784 0.709693 0.205340 0.035 Uiso 1 1 calc R U . . .
C31 C 0.37143(13) 0.32855(11) 0.29954(9) 0.0201(2) Uani 1 1 d . . . . .
C32 C 0.42336(16) 0.36979(13) 0.39157(10) 0.0309(3) Uani 1 1 d . . . . .
H32 H 0.465789 0.456965 0.412035 0.037 Uiso 1 1 calc R U . . .
C33 C 0.41297(19) 0.28319(16) 0.45335(11) 0.0403(4) Uani 1 1 d . . . . .
H33 H 0.447191 0.311187 0.516207 0.048 Uiso 1 1 calc R U . . .
C34 C 0.35295(18) 0.15642(16) 0.42356(12) 0.0397(4) Uani 1 1 d . . . . .
H34 H 0.347161 0.097536 0.465936 0.048 Uiso 1 1 calc R U . . .
C35 C 0.30123(17) 0.11488(14) 0.33219(12) 0.0353(3) Uani 1 1 d . . . . .
H35 H 0.259844 0.027598 0.312078 0.042 Uiso 1 1 calc R U . . .
C36 C 0.30968(14) 0.20040(12) 0.26989(10) 0.0257(3) Uani 1 1 d . . . . .
H36 H 0.273536 0.171781 0.207256 0.031 Uiso 1 1 calc R U . . .
C41 C 0.40111(14) 0.37722(12) 0.11760(9) 0.0235(3) Uani 1 1 d . . . . .
C42 C 0.33408(17) 0.38659(15) 0.03316(10) 0.0342(3) Uani 1 1 d . . . . .
H42 H 0.271988 0.421908 0.029164 0.041 Uiso 1 1 calc R U . . .
C43 C 0.3582(2) 0.34415(18) -0.04539(12) 0.0500(5) Uani 1 1 d . . . . .
H43 H 0.311775 0.350093 -0.102875 0.060 Uiso 1 1 calc R U . . .
C44 C 0.4479(3) 0.29407(18) -0.04056(15) 0.0573(6) Uani 1 1 d . . . . .
H44 H 0.463854 0.265693 -0.094571 0.069 Uiso 1 1 calc R U . . .
C45 C 0.5156(2) 0.28456(18) 0.04297(16) 0.0541(6) Uani 1 1 d . . . . .
H45 H 0.578008 0.249772 0.045974 0.065 Uiso 1 1 calc R U . . .
C46 C 0.49263(18) 0.32587(15) 0.12295(13) 0.0373(4) Uani 1 1 d . . . . .
H46 H 0.538850 0.319014 0.180212 0.045 Uiso 1 1 calc R U . . .
C51 C 0.84568(13) 0.85431(12) 0.33554(9) 0.0238(2) Uani 1 1 d . . . . .
C52 C 0.88718(19) 0.9015(2) 0.24832(14) 0.0594(6) Uani 1 1 d . . . . .
H52A H 0.884367 0.832214 0.209250 0.089 Uiso 1 1 calc R U . . .
H52B H 0.977382 0.968329 0.263091 0.089 Uiso 1 1 calc R U . . .
H52C H 0.826423 0.934095 0.216667 0.089 Uiso 1 1 calc R U . . .
C53 C 0.86880(18) 0.96909(17) 0.39851(16) 0.0495(5) Uani 1 1 d . . . . .
H53A H 0.820841 1.014285 0.367447 0.074 Uiso 1 1 calc R U . . .
H53B H 0.963644 1.024523 0.414902 0.074 Uiso 1 1 calc R U . . .
H53C H 0.836701 0.941894 0.453467 0.074 Uiso 1 1 calc R U . . .
C54 C 0.93037(18) 0.79343(18) 0.38225(18) 0.0571(6) Uani 1 1 d . . . . .
H54A H 0.898656 0.759541 0.435968 0.086 Uiso 1 1 calc R U . . .
H54B H 1.022536 0.855929 0.400537 0.086 Uiso 1 1 calc R U . . .
H54C H 0.924796 0.725348 0.340536 0.086 Uiso 1 1 calc R U . . .
Mo Mo -0.02072(2) 0.31577(2) 0.19555(2) 0.02226(4) Uani 1 1 d . . . . .
C61 C -0.20161(17) 0.18568(17) 0.19221(14) 0.0426(4) Uani 1 1 d . . . . .
O61 O -0.30637(14) 0.11158(16) 0.19010(15) 0.0749(6) Uani 1 1 d . . . . .
C62 C -0.06820(18) 0.43977(16) 0.25957(13) 0.0377(4) Uani 1 1 d . . . . .
O62 O -0.10202(19) 0.50508(16) 0.29305(14) 0.0697(5) Uani 1 1 d . . . . .
C63 C 0.05138(16) 0.27296(14) 0.31818(11) 0.0323(3) Uani 1 1 d . . . . .
O63 O 0.09028(15) 0.25210(13) 0.38771(9) 0.0527(4) Uani 1 1 d . . . . .
C64 C 0.01566(15) 0.18464(14) 0.12752(11) 0.0300(3) Uani 1 1 d . . . . .
O64 O 0.03183(14) 0.10970(13) 0.08920(9) 0.0468(3) Uani 1 1 d . . . . .
C65 C -0.09344(16) 0.36504(15) 0.07595(11) 0.0337(3) Uani 1 1 d . . . . .
O65 O -0.13908(17) 0.39204(17) 0.01171(11) 0.0623(4) 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
P1 C1 1.7378(12) . ?
P1 C11 1.8115(13) . ?
P1 C21 1.8115(12) . ?
P1 P3 2.1635(4) . ?
P2 C5 1.7460(12) . ?
P2 C31 1.8090(13) . ?
P2 C41 1.8139(13) . ?
P2 P3 2.1677(4) . ?
P3 Mo 2.5734(4) . ?
C1 C2 1.4059(16) . ?
C1 C5 1.4273(16) . ?
C2 C3 1.4084(17) . ?
C2 H2 0.9500 . ?
C3 C4 1.4107(17) . ?
C3 C51 1.5140(17) . ?
C4 C5 1.4041(17) . ?
C4 H4 0.9500 . ?
C11 C16 1.384(2) . ?
C11 C12 1.389(2) . ?
C12 C13 1.393(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.372(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(2) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.3907(19) . ?
C21 C26 1.3937(19) . ?
C22 C23 1.394(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.381(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.388(2) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C32 1.3931(19) . ?
C31 C36 1.3951(17) . ?
C32 C33 1.389(2) . ?
C32 H32 0.9500 . ?
C33 C34 1.382(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.384(2) . ?
C34 H34 0.9500 . ?
C35 C36 1.3877(19) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.393(2) . ?
C41 C46 1.395(2) . ?
C42 C43 1.392(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.365(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.385(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.399(2) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C51 C54 1.512(2) . ?
C51 C52 1.528(2) . ?
C51 C53 1.532(2) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
Mo C61 1.9849(17) . ?
Mo C62 2.0321(17) . ?
Mo C65 2.0482(16) . ?
Mo C63 2.0491(16) . ?
Mo C64 2.0528(16) . ?
C61 O61 1.144(2) . ?
C62 O62 1.136(2) . ?
C63 O63 1.138(2) . ?
C64 O64 1.138(2) . ?
C65 O65 1.132(2) . ?

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 P1 C11 110.64(6) . . ?
C1 P1 C21 111.42(6) . . ?
C11 P1 C21 106.73(6) . . ?
C1 P1 P3 103.42(4) . . ?
C11 P1 P3 117.36(5) . . ?
C21 P1 P3 107.28(4) . . ?
C5 P2 C31 111.15(6) . . ?
C5 P2 C41 112.43(6) . . ?
C31 P2 C41 105.40(6) . . ?
C5 P2 P3 103.65(4) . . ?
C31 P2 P3 117.16(4) . . ?
C41 P2 P3 107.17(5) . . ?
P1 P3 P2 91.344(17) . . ?
P1 P3 Mo 124.026(16) . . ?
P2 P3 Mo 119.327(16) . . ?
C2 C1 C5 107.66(10) . . ?
C2 C1 P1 133.49(9) . . ?
C5 C1 P1 118.81(9) . . ?
C1 C2 C3 108.18(10) . . ?
C1 C2 H2 125.9 . . ?
C3 C2 H2 125.9 . . ?
C2 C3 C4 108.22(11) . . ?
C2 C3 C51 125.10(11) . . ?
C4 C3 C51 126.53(11) . . ?
C5 C4 C3 108.09(11) . . ?
C5 C4 H4 126.0 . . ?
C3 C4 H4 126.0 . . ?
C4 C5 C1 107.84(10) . . ?
C4 C5 P2 133.67(9) . . ?
C1 C5 P2 118.44(9) . . ?
C16 C11 C12 119.64(14) . . ?
C16 C11 P1 121.03(12) . . ?
C12 C11 P1 118.82(11) . . ?
C11 C12 C13 120.10(17) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 119.67(18) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C15 C14 C13 120.27(17) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 120.52(19) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C11 C16 C15 119.76(17) . . ?
C11 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C22 C21 C26 119.47(12) . . ?
C22 C21 P1 119.79(10) . . ?
C26 C21 P1 120.62(10) . . ?
C21 C22 C23 119.90(14) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C24 C23 C22 120.26(15) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 119.98(13) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 120.33(14) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 120.05(14) . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
C32 C31 C36 119.78(12) . . ?
C32 C31 P2 119.41(10) . . ?
C36 C31 P2 120.77(10) . . ?
C33 C32 C31 119.87(14) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
C34 C33 C32 120.12(15) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 120.26(14) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C34 C35 C36 120.17(14) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C35 C36 C31 119.79(13) . . ?
C35 C36 H36 120.1 . . ?
C31 C36 H36 120.1 . . ?
C42 C41 C46 119.73(14) . . ?
C42 C41 P2 120.39(11) . . ?
C46 C41 P2 119.72(12) . . ?
C43 C42 C41 119.92(18) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C44 C43 C42 120.6(2) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C43 C44 C45 120.09(16) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 C46 120.44(19) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C41 C46 C45 119.22(19) . . ?
C41 C46 H46 120.4 . . ?
C45 C46 H46 120.4 . . ?
C54 C51 C3 111.41(12) . . ?
C54 C51 C52 110.91(18) . . ?
C3 C51 C52 109.00(12) . . ?
C54 C51 C53 108.07(15) . . ?
C3 C51 C53 110.31(12) . . ?
C52 C51 C53 107.05(16) . . ?
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 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C61 Mo C62 88.21(8) . . ?
C61 Mo C65 88.82(7) . . ?
C62 Mo C65 87.28(7) . . ?
C61 Mo C63 91.53(7) . . ?
C62 Mo C63 90.21(7) . . ?
C65 Mo C63 177.45(6) . . ?
C61 Mo C64 88.78(7) . . ?
C62 Mo C64 176.64(7) . . ?
C65 Mo C64 91.18(6) . . ?
C63 Mo C64 91.35(6) . . ?
C61 Mo P3 174.56(6) . . ?
C62 Mo P3 94.19(5) . . ?
C65 Mo P3 86.41(5) . . ?
C63 Mo P3 93.35(4) . . ?
C64 Mo P3 88.69(4) . . ?
O61 C61 Mo 179.30(18) . . ?
O62 C62 Mo 176.13(19) . . ?
O63 C63 Mo 177.62(16) . . ?
O64 C64 Mo 177.93(14) . . ?
O65 C65 Mo 176.36(17) . . ?

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 C1 C2 -67.86(14) . . . . ?
C21 P1 C1 C2 50.71(15) . . . . ?
P3 P1 C1 C2 165.65(12) . . . . ?
C11 P1 C1 C5 109.35(10) . . . . ?
C21 P1 C1 C5 -132.08(10) . . . . ?
P3 P1 C1 C5 -17.14(10) . . . . ?
C5 C1 C2 C3 0.49(14) . . . . ?
P1 C1 C2 C3 177.92(10) . . . . ?
C1 C2 C3 C4 -0.84(14) . . . . ?
C1 C2 C3 C51 175.12(12) . . . . ?
C2 C3 C4 C5 0.87(14) . . . . ?
C51 C3 C4 C5 -175.01(12) . . . . ?
C3 C4 C5 C1 -0.57(14) . . . . ?
C3 C4 C5 P2 176.74(10) . . . . ?
C2 C1 C5 C4 0.05(14) . . . . ?
P1 C1 C5 C4 -177.82(9) . . . . ?
C2 C1 C5 P2 -177.73(9) . . . . ?
P1 C1 C5 P2 4.39(14) . . . . ?
C31 P2 C5 C4 66.99(14) . . . . ?
C41 P2 C5 C4 -50.90(15) . . . . ?
P3 P2 C5 C4 -166.30(12) . . . . ?
C31 P2 C5 C1 -115.92(10) . . . . ?
C41 P2 C5 C1 126.18(10) . . . . ?
P3 P2 C5 C1 10.78(10) . . . . ?
C1 P1 C11 C16 90.34(15) . . . . ?
C21 P1 C11 C16 -31.04(16) . . . . ?
P3 P1 C11 C16 -151.35(14) . . . . ?
C1 P1 C11 C12 -81.37(14) . . . . ?
C21 P1 C11 C12 157.25(13) . . . . ?
P3 P1 C11 C12 36.93(15) . . . . ?
C16 C11 C12 C13 2.0(3) . . . . ?
P1 C11 C12 C13 173.83(17) . . . . ?
C11 C12 C13 C14 -0.9(3) . . . . ?
C12 C13 C14 C15 -0.9(4) . . . . ?
C13 C14 C15 C16 1.6(4) . . . . ?
C12 C11 C16 C15 -1.3(3) . . . . ?
P1 C11 C16 C15 -172.99(19) . . . . ?
C14 C15 C16 C11 -0.5(4) . . . . ?
C1 P1 C21 C22 4.52(13) . . . . ?
C11 P1 C21 C22 125.41(12) . . . . ?
P3 P1 C21 C22 -108.00(11) . . . . ?
C1 P1 C21 C26 -179.46(11) . . . . ?
C11 P1 C21 C26 -58.58(13) . . . . ?
P3 P1 C21 C26 68.01(12) . . . . ?
C26 C21 C22 C23 -0.2(2) . . . . ?
P1 C21 C22 C23 175.89(12) . . . . ?
C21 C22 C23 C24 -0.7(2) . . . . ?
C22 C23 C24 C25 0.9(3) . . . . ?
C23 C24 C25 C26 -0.2(2) . . . . ?
C24 C25 C26 C21 -0.7(2) . . . . ?
C22 C21 C26 C25 0.9(2) . . . . ?
P1 C21 C26 C25 -175.15(12) . . . . ?
C5 P2 C31 C32 24.19(14) . . . . ?
C41 P2 C31 C32 146.26(12) . . . . ?
P3 P2 C31 C32 -94.69(12) . . . . ?
C5 P2 C31 C36 -158.16(11) . . . . ?
C41 P2 C31 C36 -36.09(13) . . . . ?
P3 P2 C31 C36 82.96(12) . . . . ?
C36 C31 C32 C33 -0.2(2) . . . . ?
P2 C31 C32 C33 177.43(14) . . . . ?
C31 C32 C33 C34 0.9(3) . . . . ?
C32 C33 C34 C35 -0.9(3) . . . . ?
C33 C34 C35 C36 0.2(3) . . . . ?
C34 C35 C36 C31 0.5(3) . . . . ?
C32 C31 C36 C35 -0.5(2) . . . . ?
P2 C31 C36 C35 -178.10(12) . . . . ?
C5 P2 C41 C42 -99.25(12) . . . . ?
C31 P2 C41 C42 139.50(12) . . . . ?
P3 P2 C41 C42 14.00(13) . . . . ?
C5 P2 C41 C46 76.06(13) . . . . ?
C31 P2 C41 C46 -45.18(13) . . . . ?
P3 P2 C41 C46 -170.69(11) . . . . ?
C46 C41 C42 C43 0.3(2) . . . . ?
P2 C41 C42 C43 175.64(13) . . . . ?
C41 C42 C43 C44 -0.5(3) . . . . ?
C42 C43 C44 C45 0.3(3) . . . . ?
C43 C44 C45 C46 0.1(3) . . . . ?
C42 C41 C46 C45 0.0(2) . . . . ?
P2 C41 C46 C45 -175.31(13) . . . . ?
C44 C45 C46 C41 -0.3(3) . . . . ?
C2 C3 C51 C54 147.54(16) . . . . ?
C4 C3 C51 C54 -37.2(2) . . . . ?
C2 C3 C51 C52 -89.75(18) . . . . ?
C4 C3 C51 C52 85.47(19) . . . . ?
C2 C3 C51 C53 27.51(19) . . . . ?
C4 C3 C51 C53 -157.27(15) . . . . ?

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
_geom_hbond_publ_flag
C12 H12 O63 0.95 2.65 3.442(2) 140.9 . yes

_refine_diff_density_max         0.472
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.060

####################################################################### 
# 
# 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_shelx_CCDC6
_database_code_depnum_ccdc_archive 'CCDC 1578541'
_audit_update_record             
;
2017-10-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT094_shelx               
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       2.99 Report
RESPONSE: Residual electron density around W atom due to truncation because of the heavy atom
;
# Added during the CSD deposition process: Friday 06 October 2017 04:48 PM
# end Validation Reply Form

_audit_creation_date             2017-07-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C38 H31 O5 P3 W'
_chemical_formula_sum            'C38 H31 O5 P3 W'
_chemical_formula_weight         844.39
_chemical_melting_point          ?
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'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3304(11)
_cell_length_b                   11.7799(11)
_cell_length_c                   15.1089(14)
_cell_angle_alpha                91.631(3)
_cell_angle_beta                 100.807(3)
_cell_angle_gamma                114.414(3)
_cell_volume                     1791.0(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9352
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      3.05
_shelx_estimated_absorpt_T_max   0.893
_shelx_estimated_absorpt_T_min   0.382
_exptl_absorpt_coefficient_mu    3.400
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1178 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.7065.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.351
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.034
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            89946
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.224
_diffrn_reflns_theta_min         3.048
_diffrn_ambient_temperature      170.19
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8444
_reflns_number_total             9717
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         4.111
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.137
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         9717
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0371
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0397P)²+4.4580P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0938
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46)
2.b Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
P1 P 0.62108(9) 0.55901(8) 0.77985(6) 0.01838(17) Uani 1 1 d . . . . .
P2 P 0.69161(9) 0.33924(8) 0.73460(6) 0.01849(18) Uani 1 1 d . . . . .
P3 P 0.79316(9) 0.51908(9) 0.81803(7) 0.02005(18) Uani 1 1 d . . . . .
C1 C 0.4924(3) 0.4121(3) 0.7365(3) 0.0200(7) Uani 1 1 d . . . . .
C2 C 0.5254(4) 0.3099(3) 0.7192(3) 0.0195(7) Uani 1 1 d . . . . .
C3 C 0.4065(4) 0.2029(3) 0.6878(3) 0.0216(7) Uani 1 1 d . . . . .
H3 H 0.398660 0.121593 0.670000 0.026 Uiso 1 1 calc R . . . .
C4 C 0.3002(4) 0.2360(3) 0.6869(3) 0.0206(7) Uani 1 1 d . . . . .
C5 C 0.3537(4) 0.3649(3) 0.7158(3) 0.0232(7) Uani 1 1 d . . . . .
H5 H 0.304146 0.412249 0.720440 0.028 Uiso 1 1 calc R . . . .
C11 C 0.6290(4) 0.6725(3) 0.7005(3) 0.0232(7) Uani 1 1 d . . . . .
C12 C 0.5766(4) 0.6312(4) 0.6087(3) 0.0334(9) Uani 1 1 d . . . . .
H12 H 0.534479 0.543890 0.588212 0.040 Uiso 1 1 calc R . . . .
C13 C 0.5859(5) 0.7177(5) 0.5469(3) 0.0421(11) Uani 1 1 d . . . . .
H13 H 0.549779 0.689566 0.484089 0.051 Uiso 1 1 calc R . . . .
C14 C 0.6472(5) 0.8443(5) 0.5765(3) 0.0418(11) Uani 1 1 d . . . . .
H14 H 0.653572 0.903182 0.533834 0.050 Uiso 1 1 calc R . . . .
C15 C 0.6995(5) 0.8863(4) 0.6674(3) 0.0390(11) Uani 1 1 d . . . . .
H15 H 0.740897 0.973746 0.687323 0.047 Uiso 1 1 calc R . . . .
C16 C 0.6919(4) 0.8010(4) 0.7301(3) 0.0287(8) Uani 1 1 d . . . . .
H16 H 0.729249 0.829820 0.792682 0.034 Uiso 1 1 calc R . . . .
C21 C 0.5988(4) 0.6234(3) 0.8824(3) 0.0264(8) Uani 1 1 d . . . . .
C22 C 0.6650(5) 0.6146(4) 0.9667(3) 0.0358(10) Uani 1 1 d . . . . .
H22 H 0.727443 0.579435 0.971038 0.043 Uiso 1 1 calc R . . . .
C23 C 0.6406(6) 0.6568(5) 1.0451(4) 0.0528(15) Uani 1 1 d . . . . .
H23 H 0.687083 0.651190 1.102828 0.063 Uiso 1 1 calc R . . . .
C24 C 0.5505(7) 0.7061(5) 1.0397(4) 0.0610(18) Uani 1 1 d . . . . .
H24 H 0.533940 0.734176 1.093614 0.073 Uiso 1 1 calc R . . . .
C25 C 0.4829(7) 0.7158(5) 0.9560(5) 0.0593(18) Uani 1 1 d . . . . .
H25 H 0.420536 0.750925 0.952605 0.071 Uiso 1 1 calc R . . . .
C26 C 0.5065(5) 0.6737(4) 0.8764(4) 0.0403(11) Uani 1 1 d . . . . .
H26 H 0.459839 0.679536 0.818767 0.048 Uiso 1 1 calc R . . . .
C31 C 0.7359(4) 0.3273(4) 0.6270(3) 0.0252(8) Uani 1 1 d . . . . .
C32 C 0.7603(5) 0.4277(5) 0.5761(3) 0.0399(11) Uani 1 1 d . . . . .
H32 H 0.761553 0.503635 0.600340 0.048 Uiso 1 1 calc R . . . .
C33 C 0.7828(7) 0.4169(6) 0.4894(4) 0.0579(16) Uani 1 1 d . . . . .
H33 H 0.802839 0.486436 0.455368 0.069 Uiso 1 1 calc R . . . .
C34 C 0.7761(7) 0.3056(7) 0.4533(4) 0.0600(16) Uani 1 1 d . . . . .
H34 H 0.790480 0.298055 0.393926 0.072 Uiso 1 1 calc R . . . .
C35 C 0.7486(8) 0.2053(7) 0.5026(4) 0.069(2) Uani 1 1 d . . . . .
H35 H 0.742894 0.128181 0.477021 0.083 Uiso 1 1 calc R . . . .
C36 C 0.7290(7) 0.2163(5) 0.5896(4) 0.0513(15) Uani 1 1 d . . . . .
H36 H 0.710808 0.146726 0.623693 0.062 Uiso 1 1 calc R . . . .
C41 C 0.7274(4) 0.2267(3) 0.8001(3) 0.0209(7) Uani 1 1 d . . . . .
C42 C 0.8551(4) 0.2329(4) 0.8201(3) 0.0310(9) Uani 1 1 d . . . . .
H42 H 0.923167 0.292471 0.795390 0.037 Uiso 1 1 calc R . . . .
C43 C 0.8825(5) 0.1520(5) 0.8761(3) 0.0369(10) Uani 1 1 d . . . . .
H43 H 0.969931 0.156814 0.890311 0.044 Uiso 1 1 calc R . . . .
C44 C 0.7840(5) 0.0644(4) 0.9113(3) 0.0337(9) Uani 1 1 d . . . . .
H44 H 0.803865 0.009534 0.949929 0.040 Uiso 1 1 calc R . . . .
C45 C 0.6571(5) 0.0560(4) 0.8908(3) 0.0380(10) Uani 1 1 d . . . . .
H45 H 0.588893 -0.005325 0.914403 0.046 Uiso 1 1 calc R . . . .
C46 C 0.6292(4) 0.1375(4) 0.8356(3) 0.0294(9) Uani 1 1 d . . . . .
H46 H 0.541623 0.132187 0.821864 0.035 Uiso 1 1 calc R . . . .
C51 C 0.1543(4) 0.1448(4) 0.6646(3) 0.0261(8) Uani 1 1 d . . . . .
C52 C 0.1134(5) 0.0980(6) 0.7516(4) 0.0605(17) Uani 1 1 d . . . . .
H52A H 0.121004 0.168371 0.792052 0.091 Uiso 1 1 calc GR . . . .
H52B H 0.171486 0.061334 0.781544 0.091 Uiso 1 1 calc GR . . . .
H52C H 0.021167 0.034158 0.737223 0.091 Uiso 1 1 calc GR . . . .
C53 C 0.0696(5) 0.2052(5) 0.6185(5) 0.0589(17) Uani 1 1 d . . . . .
H53A H 0.073389 0.271708 0.661021 0.088 Uiso 1 1 calc GR . . . .
H53B H -0.022491 0.141950 0.598887 0.088 Uiso 1 1 calc GR . . . .
H53C H 0.102528 0.241430 0.565605 0.088 Uiso 1 1 calc GR . . . .
C54 C 0.1325(5) 0.0305(5) 0.6015(4) 0.0523(15) Uani 1 1 d . . . . .
H54A H 0.037012 -0.022695 0.581323 0.079 Uiso 1 1 calc GR . . . .
H54B H 0.175741 -0.017602 0.634207 0.079 Uiso 1 1 calc GR . . . .
H54C H 0.170627 0.058656 0.548683 0.079 Uiso 1 1 calc GR . . . .
W W 1.02080(2) 0.68423(2) 0.80437(2) 0.02466(6) Uani 1 1 d . . . . .
C61 C 1.2027(5) 0.8144(5) 0.8068(4) 0.0444(12) Uani 1 1 d . . . . .
O61 O 1.3069(4) 0.8890(4) 0.8088(4) 0.0747(15) Uani 1 1 d . . . . .
C62 C 0.9852(4) 0.8160(4) 0.8721(3) 0.0310(9) Uani 1 1 d . . . . .
O62 O 0.9681(4) 0.8896(3) 0.9102(3) 0.0478(9) Uani 1 1 d . . . . .
C63 C 0.9488(4) 0.7253(4) 0.6816(3) 0.0333(9) Uani 1 1 d . . . . .
O63 O 0.9094(4) 0.7474(4) 0.6124(3) 0.0545(10) Uani 1 1 d . . . . .
C64 C 1.0676(5) 0.5597(4) 0.7408(4) 0.0387(11) Uani 1 1 d . . . . .
O64 O 1.1003(5) 0.4939(4) 0.7075(3) 0.0671(13) Uani 1 1 d . . . . .
C65 C 1.0938(4) 0.6354(4) 0.9236(3) 0.0353(10) Uani 1 1 d . . . . .
O65 O 1.1388(5) 0.6084(4) 0.9884(3) 0.0623(11) 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
P1 P3 2.1696(13) . ?
P1 C1 1.744(4) . ?
P1 C11 1.807(4) . ?
P1 C21 1.810(4) . ?
P2 P3 2.1656(13) . ?
P2 C2 1.736(4) . ?
P2 C31 1.807(4) . ?
P2 C41 1.809(4) . ?
P3 W 2.5601(10) . ?
C1 C2 1.431(5) . ?
C1 C5 1.400(5) . ?
C2 C3 1.397(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.410(5) . ?
C4 C5 1.401(5) . ?
C4 C51 1.517(5) . ?
C5 H5 0.9500 . ?
C11 C12 1.389(6) . ?
C11 C16 1.395(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.386(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.377(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.378(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.388(6) . ?
C16 H16 0.9500 . ?
C21 C22 1.382(6) . ?
C21 C26 1.391(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.390(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.359(10) . ?
C24 H24 0.9500 . ?
C24 C25 1.384(10) . ?
C25 H25 0.9500 . ?
C25 C26 1.400(7) . ?
C26 H26 0.9500 . ?
C31 C32 1.389(6) . ?
C31 C36 1.377(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.392(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.371(9) . ?
C34 H34 0.9500 . ?
C34 C35 1.372(9) . ?
C35 H35 0.9500 . ?
C35 C36 1.384(7) . ?
C36 H36 0.9500 . ?
C41 C42 1.392(5) . ?
C41 C46 1.386(5) . ?
C42 H42 0.9500 . ?
C42 C43 1.383(6) . ?
C43 H43 0.9500 . ?
C43 C44 1.377(7) . ?
C44 H44 0.9500 . ?
C44 C45 1.374(7) . ?
C45 H45 0.9500 . ?
C45 C46 1.383(6) . ?
C46 H46 0.9500 . ?
C51 C52 1.518(7) . ?
C51 C53 1.501(6) . ?
C51 C54 1.532(6) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
W C61 1.989(5) . ?
W C62 2.050(4) . ?
W C63 2.037(5) . ?
W C64 2.027(5) . ?
W C65 2.038(5) . ?
C61 O61 1.138(6) . ?
C62 O62 1.128(6) . ?
C63 O63 1.139(6) . ?
C64 O64 1.130(6) . ?
C65 O65 1.134(6) . ?

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 P1 P3 103.45(12) . . ?
C1 P1 C11 111.21(18) . . ?
C1 P1 C21 112.34(18) . . ?
C11 P1 P3 117.57(13) . . ?
C11 P1 C21 105.42(18) . . ?
C21 P1 P3 106.97(15) . . ?
C2 P2 P3 103.18(12) . . ?
C2 P2 C31 111.01(18) . . ?
C2 P2 C41 111.37(17) . . ?
C31 P2 P3 117.49(14) . . ?
C31 P2 C41 106.83(18) . . ?
C41 P2 P3 106.95(13) . . ?
P1 P3 W 118.97(5) . . ?
P2 P3 P1 91.37(5) . . ?
P2 P3 W 123.04(5) . . ?
C2 C1 P1 118.5(3) . . ?
C5 C1 P1 134.0(3) . . ?
C5 C1 C2 107.5(3) . . ?
C1 C2 P2 118.8(3) . . ?
C3 C2 P2 133.5(3) . . ?
C3 C2 C1 107.6(3) . . ?
C2 C3 H3 125.8 . . ?
C2 C3 C4 108.3(3) . . ?
C4 C3 H3 125.8 . . ?
C3 C4 C51 125.1(3) . . ?
C5 C4 C3 108.0(3) . . ?
C5 C4 C51 126.7(3) . . ?
C1 C5 C4 108.5(3) . . ?
C1 C5 H5 125.7 . . ?
C4 C5 H5 125.7 . . ?
C12 C11 P1 119.4(3) . . ?
C12 C11 C16 119.8(4) . . ?
C16 C11 P1 120.8(3) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.9(4) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.1(5) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 119.8 . . ?
C13 C14 C15 120.5(4) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C16 120.1(4) . . ?
C16 C15 H15 119.9 . . ?
C11 C16 H16 120.2 . . ?
C15 C16 C11 119.6(4) . . ?
C15 C16 H16 120.2 . . ?
C22 C21 P1 120.8(3) . . ?
C22 C21 C26 119.6(4) . . ?
C26 C21 P1 119.5(4) . . ?
C21 C22 H22 119.8 . . ?
C21 C22 C23 120.3(5) . . ?
C23 C22 H22 119.8 . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.3(6) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 119.8 . . ?
C23 C24 C25 120.4(5) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 119.9(6) . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 119.4(5) . . ?
C21 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C32 C31 P2 118.6(3) . . ?
C36 C31 P2 121.4(3) . . ?
C36 C31 C32 119.4(4) . . ?
C31 C32 H32 120.1 . . ?
C31 C32 C33 119.8(5) . . ?
C33 C32 H32 120.1 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 C32 120.0(5) . . ?
C34 C33 H33 120.0 . . ?
C33 C34 H34 119.9 . . ?
C33 C34 C35 120.2(5) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 119.9 . . ?
C34 C35 C36 120.2(5) . . ?
C36 C35 H35 119.9 . . ?
C31 C36 C35 120.4(5) . . ?
C31 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C42 C41 P2 120.8(3) . . ?
C46 C41 P2 120.0(3) . . ?
C46 C41 C42 119.1(4) . . ?
C41 C42 H42 120.1 . . ?
C43 C42 C41 119.8(4) . . ?
C43 C42 H42 120.1 . . ?
C42 C43 H43 119.8 . . ?
C44 C43 C42 120.4(4) . . ?
C44 C43 H43 119.8 . . ?
C43 C44 H44 119.8 . . ?
C45 C44 C43 120.4(4) . . ?
C45 C44 H44 119.8 . . ?
C44 C45 H45 120.2 . . ?
C44 C45 C46 119.6(4) . . ?
C46 C45 H45 120.2 . . ?
C41 C46 H46 119.6 . . ?
C45 C46 C41 120.8(4) . . ?
C45 C46 H46 119.6 . . ?
C4 C51 C52 108.9(4) . . ?
C4 C51 C54 110.0(3) . . ?
C52 C51 C54 107.4(4) . . ?
C53 C51 C4 111.3(4) . . ?
C53 C51 C52 110.7(5) . . ?
C53 C51 C54 108.5(4) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C61 W P3 174.44(17) . . ?
C61 W C62 88.8(2) . . ?
C61 W C63 91.4(2) . . ?
C61 W C64 88.1(2) . . ?
C61 W C65 88.9(2) . . ?
C62 W P3 88.69(12) . . ?
C63 W P3 93.63(12) . . ?
C63 W C62 91.77(18) . . ?
C63 W C65 176.93(19) . . ?
C64 W P3 94.19(13) . . ?
C64 W C62 176.59(19) . . ?
C64 W C63 89.9(2) . . ?
C64 W C65 87.1(2) . . ?
C65 W P3 86.13(13) . . ?
C65 W C62 91.28(18) . . ?
O61 C61 W 179.6(6) . . ?
O62 C62 W 178.7(4) . . ?
O63 C63 W 179.0(5) . . ?
O64 C64 W 176.5(5) . . ?
O65 C65 W 177.0(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 P2 -4.4(4) . . . . ?
P1 C1 C2 C3 178.2(3) . . . . ?
P1 C1 C5 C4 -176.8(3) . . . . ?
P1 C11 C12 C13 -178.0(4) . . . . ?
P1 C11 C16 C15 178.4(4) . . . . ?
P1 C21 C22 C23 -175.7(4) . . . . ?
P1 C21 C26 C25 175.7(4) . . . . ?
P2 C2 C3 C4 -178.0(3) . . . . ?
P2 C31 C32 C33 -174.2(4) . . . . ?
P2 C31 C36 C35 172.5(5) . . . . ?
P2 C41 C42 C43 175.0(4) . . . . ?
P2 C41 C46 C45 -175.7(4) . . . . ?
P3 P1 C1 C2 -11.3(3) . . . . ?
P3 P1 C1 C5 165.8(4) . . . . ?
P3 P1 C11 C12 95.1(3) . . . . ?
P3 P1 C11 C16 -82.2(3) . . . . ?
P3 P1 C21 C22 -13.7(4) . . . . ?
P3 P1 C21 C26 171.2(3) . . . . ?
P3 P2 C2 C1 17.7(3) . . . . ?
P3 P2 C2 C3 -165.7(4) . . . . ?
P3 P2 C31 C32 -39.1(4) . . . . ?
P3 P2 C31 C36 149.5(4) . . . . ?
P3 P2 C41 C42 -68.2(3) . . . . ?
P3 P2 C41 C46 107.9(3) . . . . ?
C1 P1 C11 C12 -23.8(4) . . . . ?
C1 P1 C11 C16 158.8(3) . . . . ?
C1 P1 C21 C22 99.2(4) . . . . ?
C1 P1 C21 C26 -75.9(4) . . . . ?
C1 C2 C3 C4 -1.2(4) . . . . ?
C2 P2 C31 C32 79.3(4) . . . . ?
C2 P2 C31 C36 -92.1(4) . . . . ?
C2 P2 C41 C42 179.8(3) . . . . ?
C2 P2 C41 C46 -4.1(4) . . . . ?
C2 C1 C5 C4 0.6(4) . . . . ?
C2 C3 C4 C5 1.5(4) . . . . ?
C2 C3 C4 C51 -174.8(4) . . . . ?
C3 C4 C5 C1 -1.3(4) . . . . ?
C3 C4 C51 C52 90.3(5) . . . . ?
C3 C4 C51 C53 -147.4(5) . . . . ?
C3 C4 C51 C54 -27.1(6) . . . . ?
C5 C1 C2 P2 177.8(3) . . . . ?
C5 C1 C2 C3 0.4(4) . . . . ?
C5 C4 C51 C52 -85.3(5) . . . . ?
C5 C4 C51 C53 37.0(6) . . . . ?
C5 C4 C51 C54 157.3(4) . . . . ?
C11 P1 C1 C2 115.8(3) . . . . ?
C11 P1 C1 C5 -67.1(4) . . . . ?
C11 P1 C21 C22 -139.6(3) . . . . ?
C11 P1 C21 C26 45.3(4) . . . . ?
C11 C12 C13 C14 0.2(8) . . . . ?
C12 C11 C16 C15 1.0(6) . . . . ?
C12 C13 C14 C15 -0.2(8) . . . . ?
C13 C14 C15 C16 0.7(8) . . . . ?
C14 C15 C16 C11 -1.1(7) . . . . ?
C16 C11 C12 C13 -0.6(7) . . . . ?
C21 P1 C1 C2 -126.3(3) . . . . ?
C21 P1 C1 C5 50.8(5) . . . . ?
C21 P1 C11 C12 -145.8(3) . . . . ?
C21 P1 C11 C16 36.8(4) . . . . ?
C21 C22 C23 C24 0.6(8) . . . . ?
C22 C21 C26 C25 0.6(7) . . . . ?
C22 C23 C24 C25 -0.5(9) . . . . ?
C23 C24 C25 C26 0.5(9) . . . . ?
C24 C25 C26 C21 -0.5(8) . . . . ?
C26 C21 C22 C23 -0.6(7) . . . . ?
C31 P2 C2 C1 -109.0(3) . . . . ?
C31 P2 C2 C3 67.6(4) . . . . ?
C31 P2 C41 C42 58.4(4) . . . . ?
C31 P2 C41 C46 -125.5(3) . . . . ?
C31 C32 C33 C34 2.4(9) . . . . ?
C32 C31 C36 C35 1.1(9) . . . . ?
C32 C33 C34 C35 -0.7(11) . . . . ?
C33 C34 C35 C36 -0.8(12) . . . . ?
C34 C35 C36 C31 0.6(11) . . . . ?
C36 C31 C32 C33 -2.6(8) . . . . ?
C41 P2 C2 C1 132.1(3) . . . . ?
C41 P2 C2 C3 -51.3(4) . . . . ?
C41 P2 C31 C32 -159.1(4) . . . . ?
C41 P2 C31 C36 29.5(5) . . . . ?
C41 C42 C43 C44 0.7(7) . . . . ?
C42 C41 C46 C45 0.5(6) . . . . ?
C42 C43 C44 C45 0.3(7) . . . . ?
C43 C44 C45 C46 -1.0(7) . . . . ?
C44 C45 C46 C41 0.6(7) . . . . ?
C46 C41 C42 C43 -1.1(6) . . . . ?
C51 C4 C5 C1 174.9(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
