# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1545161'

_audit_update_record             
;
2017-07-07 deposited with the CCDC.
2017-07-10 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         'C35 H34 Cl2 Fe P2 S'
_chemical_formula_sum            'C35 H34 Cl2 Fe P2 S'
_chemical_formula_weight         675.37

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'
Cl Cl 0.1484 0.1585 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

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

_cell_length_a                   18.571(14)
_cell_length_b                   17.955(14)
_cell_length_c                   9.942(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.48(2)
_cell_angle_gamma                90
_cell_volume                     3315(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293
_cell_measurement_reflns_used    5818
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.578

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_F_000             1400
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device       'XtaLABmini: Fixed Chi 2 circle'
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.2523
	          2theta: 29.8876
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.2523
	          2theta: 29.8876
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.2523
	          2theta: 29.8876

;
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14024
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.578
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5818
_reflns_number_gt                5310
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
;
Olex2, OlexSys Ltd,
Version 1.2
(compiled Mar  28 2017)
;
_computing_publication_material  
;
publCIF, IUCr,
Version 1.9.20_c
;
_refine_special_details          
;
 Refined as a 2-component inversion 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)+(0.0796P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5818
_refine_ls_number_parameters     372
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0483
_refine_ls_wR_factor_ref         0.1414
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_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
Cl2 Cl 0.13238(12) 0.26057(12) 0.4337(2) 0.0481(5) Uani 1 1 d . . . . .
C2 C -0.0362(4) 0.3047(4) 0.9270(7) 0.0337(16) Uani 1 1 d . . . . .
P2 P -0.02181(10) 0.36463(10) 0.65014(17) 0.0271(4) Uani 1 1 d . . . . .
C6 C -0.1634(4) 0.1654(5) 1.0308(8) 0.045(2) Uani 1 1 d . . . . .
C5 C -0.0901(5) 0.3043(5) 1.0450(8) 0.0433(19) Uani 1 1 d . . . . .
H02C H -0.097093 0.356460 1.074438 0.052 Uiso 1 1 calc R U . . .
H02D H -0.067400 0.277209 1.121031 0.052 Uiso 1 1 calc R U . . .
C30 C -0.0947(4) 0.4037(4) 0.5459(7) 0.0298(15) Uani 1 1 d . . . . .
C31 C -0.1202(4) 0.3632(4) 0.4364(8) 0.0377(17) Uani 1 1 d . . . . .
H31 H -0.097599 0.317570 0.413225 0.045 Uiso 1 1 calc R U . . .
C32 C -0.1791(5) 0.3892(5) 0.3591(8) 0.0442(19) Uani 1 1 d . . . . .
H32 H -0.196234 0.361067 0.284424 0.053 Uiso 1 1 calc R U . . .
C33 C -0.2123(4) 0.4567(5) 0.3931(9) 0.0450(19) Uani 1 1 d . . . . .
H33 H -0.252370 0.474308 0.342406 0.054 Uiso 1 1 calc R U . . .
C34 C -0.1865(4) 0.4969(5) 0.4995(9) 0.0446(19) Uani 1 1 d . . . . .
H34 H -0.208442 0.543048 0.521736 0.054 Uiso 1 1 calc R U . . .
C35 C -0.1284(4) 0.4710(5) 0.5763(9) 0.0421(18) Uani 1 1 d . . . . .
H35 H -0.111505 0.499668 0.650409 0.050 Uiso 1 1 calc R U . . .
C4 C -0.0132(4) 0.2227(4) 0.8997(7) 0.0328(15) Uani 1 1 d . . . . .
H02A H -0.055273 0.196468 0.860208 0.039 Uiso 1 1 calc R U . . .
H02B H -0.002866 0.199051 0.987682 0.039 Uiso 1 1 calc R U . . .
C3 C -0.0735(4) 0.3426(4) 0.8031(7) 0.0327(15) Uani 1 1 d . . . . .
H01A H -0.094844 0.389870 0.835270 0.039 Uiso 1 1 calc R U . . .
H01B H -0.114063 0.310174 0.775266 0.039 Uiso 1 1 calc R U . . .
C19 C 0.1935(4) 0.2828(4) 0.8351(8) 0.0389(17) Uani 1 1 d . . . . .
H19 H 0.188428 0.300260 0.745315 0.047 Uiso 1 1 calc R U . . .
C9 C -0.1480(6) 0.0102(6) 1.0413(13) 0.069(3) Uani 1 1 d . . . . .
H9 H -0.141568 -0.042254 1.041626 0.083 Uiso 1 1 calc R U . . .
C8 C -0.1158(6) 0.0565(7) 1.1436(12) 0.072(3) Uani 1 1 d . . . . .
H8 H -0.088377 0.035371 1.215023 0.086 Uiso 1 1 calc R U . . .
C7 C -0.1264(5) 0.1352(6) 1.1348(10) 0.053(2) Uani 1 1 d . . . . .
H7 H -0.107107 0.166651 1.202918 0.064 Uiso 1 1 calc R U . . .
C21 C 0.2602(5) 0.2810(6) 1.0449(9) 0.049(2) Uani 1 1 d . . . . .
H21 H 0.299079 0.298554 1.098833 0.058 Uiso 1 1 calc R U . . .
C24 C 0.0367(4) 0.4434(4) 0.6913(6) 0.0285(14) Uani 1 1 d . . . . .
C11 C -0.1933(5) 0.1201(5) 0.9364(11) 0.057(2) Uani 1 1 d . . . . .
H11 H -0.218844 0.141474 0.862743 0.069 Uiso 1 1 calc R U . . .
C10 C -0.1875(5) 0.0441(5) 0.9453(11) 0.060(3) Uani 1 1 d . . . . .
H10 H -0.212411 0.014185 0.881185 0.071 Uiso 1 1 calc R U . . .
C12 C 0.0704(4) 0.1028(4) 0.7883(7) 0.0294(14) Uani 1 1 d . . . . .
C22 C 0.2111(5) 0.2284(6) 1.0968(9) 0.049(2) Uani 1 1 d . . . . .
H22 H 0.217473 0.209311 1.185197 0.059 Uiso 1 1 calc R U . . .
C13 C 0.1160(4) 0.0712(4) 0.6934(8) 0.0368(17) Uani 1 1 d . . . . .
H13 H 0.140554 0.102474 0.631842 0.044 Uiso 1 1 calc R U . . .
C25 C 0.0163(4) 0.5027(4) 0.7736(7) 0.0324(16) Uani 1 1 d . . . . .
H25 H -0.029589 0.502035 0.815287 0.039 Uiso 1 1 calc R U . . .
C18 C 0.1435(4) 0.2330(4) 0.8883(8) 0.0344(16) Uani 1 1 d . . . . .
C17 C 0.0346(5) 0.0565(4) 0.8763(8) 0.0402(17) Uani 1 1 d . . . . .
H17 H 0.002701 0.077079 0.940531 0.048 Uiso 1 1 calc R U . . .
C16 C 0.0452(5) -0.0201(5) 0.8713(9) 0.049(2) Uani 1 1 d . . . . .
H16 H 0.020720 -0.051189 0.933210 0.059 Uiso 1 1 calc R U . . .
C15 C 0.0904(5) -0.0517(4) 0.7785(9) 0.0435(19) Uani 1 1 d . . . . .
H15 H 0.097292 -0.104108 0.776240 0.052 Uiso 1 1 calc R U . . .
C14 C 0.1260(4) -0.0056(5) 0.6878(9) 0.045(2) Uani 1 1 d . . . . .
H14 H 0.156924 -0.026513 0.622246 0.054 Uiso 1 1 calc R U . . .
C20 C 0.2510(4) 0.3065(5) 0.9155(9) 0.052(2) Uani 1 1 d . . . . .
H01C H 0.284606 0.341048 0.880047 0.062 Uiso 1 1 calc R U . . .
C27 C 0.1292(4) 0.5654(5) 0.7369(8) 0.0418(18) Uani 1 1 d . . . . .
H01D H 0.160065 0.606881 0.751458 0.050 Uiso 1 1 calc R U . . .
C29 C 0.1049(4) 0.4457(4) 0.6321(7) 0.0336(16) Uani 1 1 d . . . . .
H01E H 0.119803 0.406102 0.575459 0.040 Uiso 1 1 calc R U . . .
Fe1 Fe 0.03748(6) 0.25209(5) 0.56591(10) 0.0286(3) Uani 1 1 d . . . . .
C1 C 0.0273(5) 0.3525(4) 0.9817(8) 0.0391(17) Uani 1 1 d . . . . .
H01G H 0.065459 0.354632 0.914283 0.059 Uiso 1 1 calc R U . . .
H01I H 0.046340 0.329914 1.064457 0.059 Uiso 1 1 calc R U . . .
H01J H 0.010254 0.402962 1.000935 0.059 Uiso 1 1 calc R U . . .
S1 S -0.17806(12) 0.26394(13) 1.0150(3) 0.0498(6) Uani 1 1 d . . . . .
P1 P 0.06438(10) 0.20512(10) 0.79000(17) 0.0283(4) Uani 1 1 d . . . . .
Cl1 Cl -0.05486(11) 0.17655(11) 0.5148(3) 0.0520(6) Uani 1 1 d . . . . .
C23 C 0.1540(4) 0.2050(5) 1.0181(8) 0.0398(18) Uani 1 1 d . . . . .
H23 H 0.121271 0.169269 1.052703 0.048 Uiso 1 1 calc R U . . .
C28 C 0.1512(4) 0.5060(5) 0.6557(8) 0.0415(18) Uani 1 1 d . . . . .
H28 H 0.197687 0.506522 0.616583 0.050 Uiso 1 1 calc R U . . .
C26 C 0.0623(4) 0.5629(4) 0.7954(7) 0.0342(16) Uani 1 1 d . . . . .
H26 H 0.047371 0.602746 0.851409 0.041 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
Cl2 Fe1 2.213(3) . ?
C2 C5 1.549(10) . ?
C2 C1 1.553(11) . ?
C2 C4 1.557(10) . ?
C2 C3 1.564(10) . ?
P2 C24 1.827(7) . ?
P2 C30 1.838(7) . ?
P2 C3 1.848(7) . ?
P2 Fe1 2.452(2) . ?
C6 C7 1.350(13) . ?
C6 C11 1.358(13) . ?
C6 S1 1.797(9) . ?
C5 S1 1.810(9) . ?
C5 H02C 0.9900 . ?
C5 H02D 0.9900 . ?
C30 C31 1.388(10) . ?
C30 C35 1.395(10) . ?
C31 C32 1.412(12) . ?
C31 H31 0.9500 . ?
C32 C33 1.402(12) . ?
C32 H32 0.9500 . ?
C33 C34 1.364(12) . ?
C33 H33 0.9500 . ?
C34 C35 1.397(11) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C4 P1 1.842(8) . ?
C4 H02A 0.9900 . ?
C4 H02B 0.9900 . ?
C3 H01A 0.9900 . ?
C3 H01B 0.9900 . ?
C19 C20 1.395(12) . ?
C19 C18 1.396(11) . ?
C19 H19 0.9500 . ?
C9 C10 1.344(16) . ?
C9 C8 1.440(17) . ?
C9 H9 0.9500 . ?
C8 C7 1.428(15) . ?
C8 H8 0.9500 . ?
C7 H7 0.9500 . ?
C21 C20 1.374(14) . ?
C21 C22 1.413(14) . ?
C21 H21 0.9500 . ?
C24 C25 1.398(10) . ?
C24 C29 1.402(10) . ?
C11 C10 1.372(14) . ?
C11 H11 0.9500 . ?
C10 H10 0.9500 . ?
C12 C17 1.382(10) . ?
C12 C13 1.393(10) . ?
C12 P1 1.841(7) . ?
C22 C23 1.378(12) . ?
C22 H22 0.9500 . ?
C13 C14 1.393(11) . ?
C13 H13 0.9500 . ?
C25 C26 1.394(10) . ?
C25 H25 0.9500 . ?
C18 C23 1.397(11) . ?
C18 P1 1.828(8) . ?
C17 C16 1.390(12) . ?
C17 H17 0.9500 . ?
C16 C15 1.375(13) . ?
C16 H16 0.9500 . ?
C15 C14 1.395(13) . ?
C15 H15 0.9500 . ?
C14 H14 0.9500 . ?
C20 H01C 0.9500 . ?
C27 C26 1.376(11) . ?
C27 C28 1.401(12) . ?
C27 H01D 0.9500 . ?
C29 C28 1.401(11) . ?
C29 H01E 0.9500 . ?
Fe1 Cl1 2.241(3) . ?
Fe1 P1 2.430(3) . ?
C1 H01G 0.9800 . ?
C1 H01I 0.9800 . ?
C1 H01J 0.9800 . ?
C23 H23 0.9500 . ?
C28 H28 0.9500 . ?
C26 H26 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
C5 C2 C1 103.3(6) . . ?
C5 C2 C4 107.9(6) . . ?
C1 C2 C4 112.0(6) . . ?
C5 C2 C3 108.3(6) . . ?
C1 C2 C3 111.4(6) . . ?
C4 C2 C3 113.2(6) . . ?
C24 P2 C30 105.4(3) . . ?
C24 P2 C3 107.0(3) . . ?
C30 P2 C3 99.2(3) . . ?
C24 P2 Fe1 116.5(2) . . ?
C30 P2 Fe1 116.9(2) . . ?
C3 P2 Fe1 110.1(2) . . ?
C7 C6 C11 119.4(10) . . ?
C7 C6 S1 122.6(7) . . ?
C11 C6 S1 117.9(7) . . ?
C2 C5 S1 117.7(6) . . ?
C2 C5 H02C 107.9 . . ?
S1 C5 H02C 107.9 . . ?
C2 C5 H02D 107.9 . . ?
S1 C5 H02D 107.9 . . ?
H02C C5 H02D 107.2 . . ?
C31 C30 C35 118.2(7) . . ?
C31 C30 P2 119.1(6) . . ?
C35 C30 P2 122.6(6) . . ?
C30 C31 C32 120.8(7) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 H31 119.6 . . ?
C33 C32 C31 119.6(8) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 119.5(7) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 120.8(8) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 H34 119.6 . . ?
C30 C35 C34 121.1(8) . . ?
C30 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C2 C4 P1 118.8(5) . . ?
C2 C4 H02A 107.6 . . ?
P1 C4 H02A 107.6 . . ?
C2 C4 H02B 107.6 . . ?
P1 C4 H02B 107.6 . . ?
H02A C4 H02B 107.0 . . ?
C2 C3 P2 120.7(5) . . ?
C2 C3 H01A 107.1 . . ?
P2 C3 H01A 107.1 . . ?
C2 C3 H01B 107.1 . . ?
P2 C3 H01B 107.1 . . ?
H01A C3 H01B 106.8 . . ?
C20 C19 C18 119.1(8) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
C10 C9 C8 117.5(10) . . ?
C10 C9 H9 121.3 . . ?
C8 C9 H9 121.3 . . ?
C7 C8 C9 118.1(9) . . ?
C7 C8 H8 120.9 . . ?
C9 C8 H8 120.9 . . ?
C6 C7 C8 120.9(10) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C20 C21 C22 119.3(8) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C25 C24 C29 118.2(7) . . ?
C25 C24 P2 123.9(6) . . ?
C29 C24 P2 117.8(5) . . ?
C6 C11 C10 121.3(11) . . ?
C6 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C9 C10 C11 122.5(11) . . ?
C9 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C17 C12 C13 118.8(7) . . ?
C17 C12 P1 124.4(6) . . ?
C13 C12 P1 116.8(6) . . ?
C23 C22 C21 119.5(8) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C12 C13 C14 120.8(8) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C26 C25 C24 120.8(7) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C19 C18 C23 119.5(7) . . ?
C19 C18 P1 120.4(6) . . ?
C23 C18 P1 120.0(6) . . ?
C12 C17 C16 120.3(8) . . ?
C12 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C15 C16 C17 121.3(8) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C16 C15 C14 118.9(8) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C13 C14 C15 119.9(8) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C21 C20 C19 121.5(8) . . ?
C21 C20 H01C 119.2 . . ?
C19 C20 H01C 119.2 . . ?
C26 C27 C28 119.1(7) . . ?
C26 C27 H01D 120.4 . . ?
C28 C27 H01D 120.4 . . ?
C28 C29 C24 120.6(7) . . ?
C28 C29 H01E 119.7 . . ?
C24 C29 H01E 119.7 . . ?
Cl2 Fe1 Cl1 121.24(11) . . ?
Cl2 Fe1 P1 114.20(10) . . ?
Cl1 Fe1 P1 98.57(9) . . ?
Cl2 Fe1 P2 120.55(8) . . ?
Cl1 Fe1 P2 103.37(10) . . ?
P1 Fe1 P2 93.57(9) . . ?
C2 C1 H01G 109.5 . . ?
C2 C1 H01I 109.5 . . ?
H01G C1 H01I 109.5 . . ?
C2 C1 H01J 109.5 . . ?
H01G C1 H01J 109.5 . . ?
H01I C1 H01J 109.5 . . ?
C6 S1 C5 104.1(4) . . ?
C18 P1 C12 103.3(3) . . ?
C18 P1 C4 105.4(3) . . ?
C12 P1 C4 103.0(3) . . ?
C18 P1 Fe1 123.6(3) . . ?
C12 P1 Fe1 110.5(2) . . ?
C4 P1 Fe1 109.1(3) . . ?
C22 C23 C18 121.0(8) . . ?
C22 C23 H23 119.5 . . ?
C18 C23 H23 119.5 . . ?
C27 C28 C29 120.2(7) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C27 C26 C25 121.0(7) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?

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
C1 C2 C5 S1 172.2(5) . . . . ?
C4 C2 C5 S1 -69.0(8) . . . . ?
C3 C2 C5 S1 53.9(8) . . . . ?
C24 P2 C30 C31 140.4(6) . . . . ?
C3 P2 C30 C31 -109.0(6) . . . . ?
Fe1 P2 C30 C31 9.2(7) . . . . ?
C24 P2 C30 C35 -42.9(7) . . . . ?
C3 P2 C30 C35 67.7(7) . . . . ?
Fe1 P2 C30 C35 -174.2(5) . . . . ?
C35 C30 C31 C32 -0.8(11) . . . . ?
P2 C30 C31 C32 176.0(6) . . . . ?
C30 C31 C32 C33 0.2(12) . . . . ?
C31 C32 C33 C34 0.8(12) . . . . ?
C32 C33 C34 C35 -1.1(13) . . . . ?
C31 C30 C35 C34 0.6(11) . . . . ?
P2 C30 C35 C34 -176.1(6) . . . . ?
C33 C34 C35 C30 0.4(13) . . . . ?
C5 C2 C4 P1 -167.4(6) . . . . ?
C1 C2 C4 P1 -54.3(8) . . . . ?
C3 C2 C4 P1 72.8(8) . . . . ?
C5 C2 C3 P2 171.8(5) . . . . ?
C1 C2 C3 P2 58.8(8) . . . . ?
C4 C2 C3 P2 -68.6(8) . . . . ?
C24 P2 C3 C2 -72.5(6) . . . . ?
C30 P2 C3 C2 178.2(6) . . . . ?
Fe1 P2 C3 C2 55.0(6) . . . . ?
C10 C9 C8 C7 -1.6(14) . . . . ?
C11 C6 C7 C8 2.6(13) . . . . ?
S1 C6 C7 C8 -180.0(7) . . . . ?
C9 C8 C7 C6 -2.3(14) . . . . ?
C30 P2 C24 C25 67.2(6) . . . . ?
C3 P2 C24 C25 -37.8(7) . . . . ?
Fe1 P2 C24 C25 -161.4(5) . . . . ?
C30 P2 C24 C29 -110.1(6) . . . . ?
C3 P2 C24 C29 145.0(6) . . . . ?
Fe1 P2 C24 C29 21.4(6) . . . . ?
C7 C6 C11 C10 0.8(14) . . . . ?
S1 C6 C11 C10 -176.7(7) . . . . ?
C8 C9 C10 C11 5.0(15) . . . . ?
C6 C11 C10 C9 -4.9(15) . . . . ?
C20 C21 C22 C23 -1.6(14) . . . . ?
C17 C12 C13 C14 -0.6(12) . . . . ?
P1 C12 C13 C14 177.7(6) . . . . ?
C29 C24 C25 C26 0.5(10) . . . . ?
P2 C24 C25 C26 -176.7(5) . . . . ?
C20 C19 C18 C23 -3.3(12) . . . . ?
C20 C19 C18 P1 176.1(6) . . . . ?
C13 C12 C17 C16 1.2(12) . . . . ?
P1 C12 C17 C16 -177.0(7) . . . . ?
C12 C17 C16 C15 -0.8(13) . . . . ?
C17 C16 C15 C14 -0.2(13) . . . . ?
C12 C13 C14 C15 -0.4(13) . . . . ?
C16 C15 C14 C13 0.8(13) . . . . ?
C22 C21 C20 C19 1.3(14) . . . . ?
C18 C19 C20 C21 1.1(13) . . . . ?
C25 C24 C29 C28 0.3(11) . . . . ?
P2 C24 C29 C28 177.7(6) . . . . ?
C7 C6 S1 C5 47.8(8) . . . . ?
C11 C6 S1 C5 -134.8(7) . . . . ?
C2 C5 S1 C6 80.5(7) . . . . ?
C19 C18 P1 C12 124.8(6) . . . . ?
C23 C18 P1 C12 -55.8(7) . . . . ?
C19 C18 P1 C4 -127.5(6) . . . . ?
C23 C18 P1 C4 51.9(7) . . . . ?
C19 C18 P1 Fe1 -1.2(8) . . . . ?
C23 C18 P1 Fe1 178.2(5) . . . . ?
C17 C12 P1 C18 96.1(7) . . . . ?
C13 C12 P1 C18 -82.1(6) . . . . ?
C17 C12 P1 C4 -13.5(7) . . . . ?
C13 C12 P1 C4 168.4(6) . . . . ?
C17 C12 P1 Fe1 -129.9(6) . . . . ?
C13 C12 P1 Fe1 52.0(6) . . . . ?
C2 C4 P1 C18 72.1(6) . . . . ?
C2 C4 P1 C12 180.0(6) . . . . ?
C2 C4 P1 Fe1 -62.7(6) . . . . ?
C21 C22 C23 C18 -0.6(14) . . . . ?
C19 C18 C23 C22 3.0(12) . . . . ?
P1 C18 C23 C22 -176.4(7) . . . . ?
C26 C27 C28 C29 1.5(12) . . . . ?
C24 C29 C28 C27 -1.3(12) . . . . ?
C28 C27 C26 C25 -0.7(12) . . . . ?
C24 C25 C26 C27 -0.3(11) . . . . ?

_refine_diff_density_max         1.618
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.120




_publcif_funding_html            
;
;
####################################################################### 
# 
# 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_AP464f
_database_code_depnum_ccdc_archive 'CCDC 1545162'

_audit_update_record             
;
2017-06-22 deposited with the CCDC.
2017-07-10 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 H34 Mo O3 P2 S, C4 H8 O'
_chemical_formula_sum            'C42 H42 Mo O4 P2 S'
_chemical_formula_weight         800.69

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'
Mo Mo -0.0483 2.7339 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.2574(7)
_cell_length_b                   17.4761(9)
_cell_length_c                   21.2556(15)
_cell_angle_alpha                90
_cell_angle_beta                 100.417(7)
_cell_angle_gamma                90
_cell_volume                     3747.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5399
_cell_measurement_theta_min      4.2040
_cell_measurement_theta_max      75.9530

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_F_000             1856
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 11 4 0.0476
-1 -11 -4 0.0470
0 1 -13 0.0386
0 -1 13 0.0258
6 3 -6 0.1005
0 11 4 0.0314
0 -11 -4 0.0349
-7 0 0 0.1694
7 -1 0 0.1121
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.064
_exptl_absorpt_coefficient_mu    4.520
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_T_max  0.786
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_reflns_number            37465
_diffrn_reflns_av_unetI/netI     0.0974
_diffrn_reflns_av_R_equivalents  0.1243
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.296
_diffrn_reflns_theta_max         77.145
_diffrn_reflns_theta_full        71.9829
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7773
_reflns_number_gt                5583
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
;
Olex2, OlexSys Ltd,
Version 1.2
(compiled Mar  28 2017)
;
_computing_publication_material  
;
publCIF, IUCr,
Version 1.9.20_c
;
_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)+(0.1012P)²+9.4760P] 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         7773
_refine_ls_number_parameters     452
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0711
_refine_ls_wR_factor_ref         0.2124
_refine_ls_wR_factor_gt          0.1810
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.52109(4) 0.20686(3) 0.32259(2) 0.02357(16) Uani 1 1 d . . . . .
S1 S 0.41270(14) 0.07618(8) 0.29837(7) 0.0288(3) Uani 1 1 d . . . . .
P1 P 0.55881(14) 0.20837(8) 0.20882(7) 0.0256(3) Uani 1 1 d . . . . .
P2 P 0.72532(14) 0.12201(8) 0.34159(7) 0.0257(3) Uani 1 1 d . . . . .
O1 O 0.6673(5) 0.3564(3) 0.3739(2) 0.0398(10) Uani 1 1 d . . . . .
O2 O 0.2761(5) 0.3157(3) 0.2854(2) 0.0408(11) Uani 1 1 d . . . . .
O3 O 0.4577(4) 0.2017(3) 0.4604(2) 0.0370(10) Uani 1 1 d . . . . .
C1 C 0.6171(5) 0.3005(3) 0.3529(3) 0.0266(11) Uani 1 1 d . . . . .
C2 C 0.3634(6) 0.2745(3) 0.2983(3) 0.0295(12) Uani 1 1 d . . . . .
C3 C 0.4814(5) 0.2013(3) 0.4108(3) 0.0225(10) Uani 1 1 d . . . . .
C4 C 0.6536(6) -0.0200(4) 0.1807(3) 0.0347(13) Uani 1 1 d . . . . .
H4A H 0.725925 -0.004215 0.159141 0.052 Uiso 1 1 calc R U . . .
H4B H 0.575967 -0.033911 0.148677 0.052 Uiso 1 1 calc R U . . .
H4C H 0.681816 -0.064283 0.208124 0.052 Uiso 1 1 calc R U . . .
C5 C 0.6171(6) 0.0472(3) 0.2223(3) 0.0306(12) Uani 1 1 d . . . . .
C6 C 0.5165(6) 0.0118(3) 0.2596(3) 0.0317(12) Uani 1 1 d . . . . .
H6A H 0.566183 -0.021780 0.293121 0.038 Uiso 1 1 calc R U . . .
H6B H 0.456490 -0.021519 0.229686 0.038 Uiso 1 1 calc R U . . .
C7 C 0.5547(6) 0.1104(3) 0.1760(3) 0.0302(12) Uani 1 1 d . . . . .
H7A H 0.461099 0.096518 0.159839 0.036 Uiso 1 1 calc R U . . .
H7B H 0.600818 0.110799 0.138919 0.036 Uiso 1 1 calc R U . . .
C8 C 0.7466(6) 0.0718(4) 0.2671(3) 0.0307(12) Uani 1 1 d . . . . .
H8A H 0.796654 0.105795 0.242712 0.037 Uiso 1 1 calc R U . . .
H8B H 0.801317 0.025628 0.279011 0.037 Uiso 1 1 calc R U . . .
C9 C 0.2556(6) 0.0676(4) 0.2455(3) 0.0321(12) Uani 1 1 d . . . . .
C10 C 0.1916(7) -0.0024(4) 0.2423(3) 0.0413(15) Uani 1 1 d . . . . .
H10 H 0.231269 -0.044772 0.266472 0.050 Uiso 1 1 calc R U . . .
C11 C 0.0687(7) -0.0093(5) 0.2033(3) 0.0432(16) Uani 1 1 d . . . . .
H11 H 0.024858 -0.057419 0.200403 0.052 Uiso 1 1 calc R U . . .
C12 C 0.0087(6) 0.0509(5) 0.1689(3) 0.0435(16) Uani 1 1 d . . . . .
H12 H -0.075882 0.044799 0.142503 0.052 Uiso 1 1 calc R U . . .
C13 C 0.0728(7) 0.1213(4) 0.1729(3) 0.0398(15) Uani 1 1 d . . . . .
H13 H 0.031993 0.163628 0.148998 0.048 Uiso 1 1 calc R U . . .
C14 C 0.1958(6) 0.1300(4) 0.2115(3) 0.0323(12) Uani 1 1 d . . . . .
H14 H 0.238991 0.178241 0.214661 0.039 Uiso 1 1 calc R U . . .
C15 C 0.4338(6) 0.2600(4) 0.1495(3) 0.0306(12) Uani 1 1 d . . . . .
C16 C 0.3399(7) 0.2236(5) 0.1029(3) 0.0399(15) Uani 1 1 d . . . . .
H16 H 0.342721 0.169569 0.098125 0.048 Uiso 1 1 calc R U . . .
C17 C 0.2431(8) 0.2657(5) 0.0639(4) 0.0484(17) Uani 1 1 d . . . . .
H17 H 0.178006 0.240582 0.033369 0.058 Uiso 1 1 calc R U . . .
C18 C 0.2419(7) 0.3439(5) 0.0696(3) 0.0459(17) Uani 1 1 d . . . . .
H18 H 0.176575 0.372760 0.042144 0.055 Uiso 1 1 calc R U . . .
C19 C 0.3342(8) 0.3816(5) 0.1148(4) 0.0499(18) Uani 1 1 d . . . . .
H19 H 0.332142 0.435793 0.118294 0.060 Uiso 1 1 calc R U . . .
C20 C 0.4308(7) 0.3389(4) 0.1555(3) 0.0403(15) Uani 1 1 d . . . . .
H20 H 0.493938 0.364118 0.186887 0.048 Uiso 1 1 calc R U . . .
C21 C 0.7118(6) 0.2493(4) 0.1891(3) 0.0300(12) Uani 1 1 d . . . . .
C22 C 0.7309(7) 0.2523(4) 0.1255(3) 0.0378(14) Uani 1 1 d . . . . .
H22 H 0.664595 0.233455 0.091975 0.045 Uiso 1 1 calc R U . . .
C23 C 0.8478(7) 0.2831(4) 0.1117(3) 0.0411(16) Uani 1 1 d . . . . .
H23 H 0.861728 0.284427 0.068697 0.049 Uiso 1 1 calc R U . . .
C24 C 0.9437(7) 0.3119(4) 0.1601(4) 0.0416(16) Uani 1 1 d . . . . .
H24 H 1.022025 0.334025 0.150105 0.050 Uiso 1 1 calc R U . . .
C25 C 0.9264(6) 0.3088(4) 0.2225(3) 0.0362(13) Uani 1 1 d . . . . .
H25 H 0.994074 0.326765 0.255758 0.043 Uiso 1 1 calc R U . . .
C26 C 0.8091(6) 0.2791(3) 0.2372(3) 0.0304(12) Uani 1 1 d . . . . .
H26 H 0.795510 0.279127 0.280248 0.036 Uiso 1 1 calc R U . . .
C27 C 0.8851(6) 0.1687(3) 0.3681(3) 0.0296(12) Uani 1 1 d . . . . .
C28 C 0.9985(6) 0.1550(4) 0.3421(3) 0.0350(13) Uani 1 1 d . . . . .
H28 H 0.995980 0.118981 0.308431 0.042 Uiso 1 1 calc R U . . .
C29 C 1.1142(7) 0.1936(4) 0.3654(3) 0.0397(15) Uani 1 1 d . . . . .
H29 H 1.190701 0.184026 0.347284 0.048 Uiso 1 1 calc R U . . .
C30 C 1.1212(7) 0.2456(4) 0.4143(4) 0.0463(17) Uani 1 1 d . . . . .
H30 H 1.201461 0.272460 0.429085 0.056 Uiso 1 1 calc R U . . .
C31 C 1.0113(6) 0.2589(4) 0.4419(4) 0.0428(16) Uani 1 1 d . . . . .
H31 H 1.016534 0.293885 0.476494 0.051 Uiso 1 1 calc R U . . .
C32 C 0.8926(6) 0.2209(4) 0.4190(3) 0.0348(13) Uani 1 1 d . . . . .
H32 H 0.816832 0.230290 0.437820 0.042 Uiso 1 1 calc R U . . .
C33 C 0.7409(6) 0.0426(4) 0.3994(3) 0.0316(12) Uani 1 1 d . . . . .
C34 C 0.8584(7) -0.0002(4) 0.4124(3) 0.0387(14) Uani 1 1 d . . . . .
H34 H 0.928939 0.011115 0.390482 0.046 Uiso 1 1 calc R U . . .
C35 C 0.8723(7) -0.0589(4) 0.4572(4) 0.0433(16) Uani 1 1 d . . . . .
H35 H 0.950881 -0.088891 0.464695 0.052 Uiso 1 1 calc R U . . .
C36 C 0.7722(8) -0.0736(4) 0.4905(3) 0.0421(15) Uani 1 1 d . . . . .
H36 H 0.783083 -0.112301 0.522410 0.051 Uiso 1 1 calc R U . . .
C37 C 0.6560(8) -0.0323(4) 0.4778(3) 0.0442(16) Uani 1 1 d . . . . .
H37 H 0.585878 -0.043708 0.500037 0.053 Uiso 1 1 calc R U . . .
C38 C 0.6410(7) 0.0257(4) 0.4328(3) 0.0377(14) Uani 1 1 d . . . . .
H38 H 0.560948 0.054269 0.424763 0.045 Uiso 1 1 calc R U . . .
O4 O 0.2499(13) 0.4214(8) 0.5301(5) 0.136(4) Uani 1 1 d . . . . .
C39 C 0.197(3) 0.4909(15) 0.4918(10) 0.194(12) Uani 1 1 d . . . . .
H39A H 0.099153 0.490158 0.481202 0.232 Uiso 1 1 calc R U . . .
H39B H 0.226379 0.538723 0.515131 0.232 Uiso 1 1 calc R U . . .
C40 C 0.254(2) 0.4837(14) 0.4358(10) 0.200(14) Uani 1 1 d . . . . .
H40A H 0.293219 0.533287 0.426588 0.241 Uiso 1 1 calc R U . . .
H40B H 0.183625 0.470698 0.399026 0.241 Uiso 1 1 calc R U . . .
C41 C 0.3562(16) 0.4246(7) 0.4434(6) 0.100(4) Uani 1 1 d . . . . .
H41A H 0.442751 0.446744 0.438626 0.120 Uiso 1 1 calc R U . . .
H41B H 0.332597 0.383832 0.411016 0.120 Uiso 1 1 calc R U . . .
C42 C 0.3623(17) 0.3938(7) 0.5084(5) 0.098(4) Uani 1 1 d . . . . .
H42A H 0.361840 0.337141 0.507532 0.118 Uiso 1 1 calc R U . . .
H42B H 0.444122 0.411191 0.536904 0.118 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C1 1.958(6) . ?
Mo1 C3 1.992(5) . ?
Mo1 C2 1.994(6) . ?
Mo1 P1 2.5174(15) . ?
Mo1 P2 2.5386(15) . ?
Mo1 S1 2.5515(15) . ?
S1 C9 1.797(6) . ?
S1 C6 1.843(6) . ?
P1 C21 1.841(6) . ?
P1 C7 1.847(6) . ?
P1 C15 1.860(6) . ?
P2 C27 1.826(6) . ?
P2 C33 1.841(6) . ?
P2 C8 1.858(6) . ?
O1 C1 1.155(8) . ?
O2 C2 1.143(8) . ?
O3 C3 1.124(7) . ?
C4 C5 1.556(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C7 1.539(8) . ?
C5 C6 1.539(8) . ?
C5 C8 1.548(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.384(9) . ?
C9 C14 1.388(9) . ?
C10 C11 1.384(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.363(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.391(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(9) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C20 1.386(10) . ?
C15 C16 1.404(9) . ?
C16 C17 1.385(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.373(12) . ?
C17 H17 0.9500 . ?
C18 C19 1.388(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.405(10) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.394(9) . ?
C21 C22 1.402(9) . ?
C22 C23 1.393(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.384(11) . ?
C23 H23 0.9500 . ?
C24 C25 1.371(10) . ?
C24 H24 0.9500 . ?
C25 C26 1.396(8) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.396(9) . ?
C27 C32 1.408(9) . ?
C28 C29 1.377(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.373(11) . ?
C29 H29 0.9500 . ?
C30 C31 1.382(11) . ?
C30 H30 0.9500 . ?
C31 C32 1.395(9) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.380(9) . ?
C33 C34 1.402(9) . ?
C34 C35 1.390(10) . ?
C34 H34 0.9500 . ?
C35 C36 1.373(10) . ?
C35 H35 0.9500 . ?
C36 C37 1.378(11) . ?
C36 H36 0.9500 . ?
C37 C38 1.383(10) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
O4 C42 1.402(17) . ?
O4 C39 1.51(2) . ?
C39 C40 1.42(2) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C41 1.46(2) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.474(16) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Mo1 C3 84.7(2) . . ?
C1 Mo1 C2 85.7(2) . . ?
C3 Mo1 C2 88.7(2) . . ?
C1 Mo1 P1 98.72(17) . . ?
C3 Mo1 P1 176.34(15) . . ?
C2 Mo1 P1 90.20(18) . . ?
C1 Mo1 P2 94.85(16) . . ?
C3 Mo1 P2 97.19(15) . . ?
C2 Mo1 P2 174.07(18) . . ?
P1 Mo1 P2 83.87(5) . . ?
C1 Mo1 S1 171.68(17) . . ?
C3 Mo1 S1 89.45(16) . . ?
C2 Mo1 S1 100.08(18) . . ?
P1 Mo1 S1 87.28(5) . . ?
P2 Mo1 S1 79.99(5) . . ?
C9 S1 C6 101.3(3) . . ?
C9 S1 Mo1 120.6(2) . . ?
C6 S1 Mo1 111.8(2) . . ?
C21 P1 C7 103.7(3) . . ?
C21 P1 C15 99.7(3) . . ?
C7 P1 C15 103.2(3) . . ?
C21 P1 Mo1 120.6(2) . . ?
C7 P1 Mo1 110.9(2) . . ?
C15 P1 Mo1 116.67(19) . . ?
C27 P2 C33 99.5(3) . . ?
C27 P2 C8 103.7(3) . . ?
C33 P2 C8 101.8(3) . . ?
C27 P2 Mo1 117.2(2) . . ?
C33 P2 Mo1 121.1(2) . . ?
C8 P2 Mo1 111.15(19) . . ?
O1 C1 Mo1 174.9(5) . . ?
O2 C2 Mo1 177.3(6) . . ?
O3 C3 Mo1 176.7(5) . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C7 C5 C6 112.2(5) . . ?
C7 C5 C8 113.8(5) . . ?
C6 C5 C8 112.1(5) . . ?
C7 C5 C4 107.0(5) . . ?
C6 C5 C4 104.0(5) . . ?
C8 C5 C4 106.9(5) . . ?
C5 C6 S1 118.7(4) . . ?
C5 C6 H6A 107.6 . . ?
S1 C6 H6A 107.6 . . ?
C5 C6 H6B 107.6 . . ?
S1 C6 H6B 107.6 . . ?
H6A C6 H6B 107.1 . . ?
C5 C7 P1 116.5(4) . . ?
C5 C7 H7A 108.2 . . ?
P1 C7 H7A 108.2 . . ?
C5 C7 H7B 108.2 . . ?
P1 C7 H7B 108.2 . . ?
H7A C7 H7B 107.3 . . ?
C5 C8 P2 115.8(4) . . ?
C5 C8 H8A 108.3 . . ?
P2 C8 H8A 108.3 . . ?
C5 C8 H8B 108.3 . . ?
P2 C8 H8B 108.3 . . ?
H8A C8 H8B 107.4 . . ?
C10 C9 C14 120.5(6) . . ?
C10 C9 S1 117.9(5) . . ?
C14 C9 S1 121.5(5) . . ?
C11 C10 C9 118.6(7) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C12 C11 C10 121.9(7) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C11 C12 C13 119.2(6) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C14 C13 C12 120.2(7) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C9 119.6(6) . . ?
C13 C14 H14 120.2 . . ?
C9 C14 H14 120.2 . . ?
C20 C15 C16 119.5(6) . . ?
C20 C15 P1 116.4(5) . . ?
C16 C15 P1 124.0(5) . . ?
C17 C16 C15 120.5(7) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C18 C17 C16 119.6(7) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C19 121.2(7) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C18 C19 C20 119.4(8) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C15 C20 C19 119.8(7) . . ?
C15 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C26 C21 C22 119.2(6) . . ?
C26 C21 P1 120.3(4) . . ?
C22 C21 P1 120.5(5) . . ?
C23 C22 C21 119.5(6) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C24 C23 C22 120.5(6) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 120.4(6) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 119.9(7) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 120.4(6) . . ?
C21 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C28 C27 C32 118.8(6) . . ?
C28 C27 P2 124.6(5) . . ?
C32 C27 P2 116.6(5) . . ?
C29 C28 C27 120.0(7) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 121.4(7) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C29 C30 C31 119.8(7) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
C30 C31 C32 120.0(7) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C27 120.0(6) . . ?
C31 C32 H32 120.0 . . ?
C27 C32 H32 120.0 . . ?
C38 C33 C34 118.4(6) . . ?
C38 C33 P2 121.4(5) . . ?
C34 C33 P2 120.1(5) . . ?
C35 C34 C33 120.5(6) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C36 C35 C34 119.8(7) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C37 120.2(7) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C36 C37 C38 120.2(7) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C33 C38 C37 120.9(7) . . ?
C33 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
C42 O4 C39 109.6(13) . . ?
C40 C39 O4 102.7(16) . . ?
C40 C39 H39A 111.2 . . ?
O4 C39 H39A 111.2 . . ?
C40 C39 H39B 111.2 . . ?
O4 C39 H39B 111.2 . . ?
H39A C39 H39B 109.1 . . ?
C39 C40 C41 111.5(16) . . ?
C39 C40 H40A 109.3 . . ?
C41 C40 H40A 109.3 . . ?
C39 C40 H40B 109.3 . . ?
C41 C40 H40B 109.3 . . ?
H40A C40 H40B 108.0 . . ?
C40 C41 C42 105.6(14) . . ?
C40 C41 H41A 110.6 . . ?
C42 C41 H41A 110.6 . . ?
C40 C41 H41B 110.6 . . ?
C42 C41 H41B 110.6 . . ?
H41A C41 H41B 108.7 . . ?
O4 C42 C41 106.5(13) . . ?
O4 C42 H42A 110.4 . . ?
C41 C42 H42A 110.4 . . ?
O4 C42 H42B 110.4 . . ?
C41 C42 H42B 110.4 . . ?
H42A C42 H42B 108.6 . . ?

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
C7 C5 C6 S1 -48.3(6) . . . . ?
C8 C5 C6 S1 81.2(6) . . . . ?
C4 C5 C6 S1 -163.6(4) . . . . ?
C9 S1 C6 C5 105.3(5) . . . . ?
Mo1 S1 C6 C5 -24.4(5) . . . . ?
C6 C5 C7 P1 88.8(6) . . . . ?
C8 C5 C7 P1 -39.9(6) . . . . ?
C4 C5 C7 P1 -157.8(4) . . . . ?
C21 P1 C7 C5 93.0(5) . . . . ?
C15 P1 C7 C5 -163.3(4) . . . . ?
Mo1 P1 C7 C5 -37.7(5) . . . . ?
C7 C5 C8 P2 85.2(6) . . . . ?
C6 C5 C8 P2 -43.5(6) . . . . ?
C4 C5 C8 P2 -156.8(4) . . . . ?
C27 P2 C8 C5 -162.3(4) . . . . ?
C33 P2 C8 C5 94.7(5) . . . . ?
Mo1 P2 C8 C5 -35.5(5) . . . . ?
C6 S1 C9 C10 66.5(6) . . . . ?
Mo1 S1 C9 C10 -169.6(4) . . . . ?
C6 S1 C9 C14 -117.1(5) . . . . ?
Mo1 S1 C9 C14 6.8(6) . . . . ?
C14 C9 C10 C11 1.7(10) . . . . ?
S1 C9 C10 C11 178.1(5) . . . . ?
C9 C10 C11 C12 -1.0(11) . . . . ?
C10 C11 C12 C13 0.2(11) . . . . ?
C11 C12 C13 C14 -0.2(11) . . . . ?
C12 C13 C14 C9 0.9(10) . . . . ?
C10 C9 C14 C13 -1.7(10) . . . . ?
S1 C9 C14 C13 -178.0(5) . . . . ?
C21 P1 C15 C20 -62.5(5) . . . . ?
C7 P1 C15 C20 -169.2(5) . . . . ?
Mo1 P1 C15 C20 69.0(5) . . . . ?
C21 P1 C15 C16 121.4(6) . . . . ?
C7 P1 C15 C16 14.7(6) . . . . ?
Mo1 P1 C15 C16 -107.1(5) . . . . ?
C20 C15 C16 C17 -1.3(10) . . . . ?
P1 C15 C16 C17 174.7(5) . . . . ?
C15 C16 C17 C18 2.0(11) . . . . ?
C16 C17 C18 C19 -1.4(11) . . . . ?
C17 C18 C19 C20 0.0(11) . . . . ?
C16 C15 C20 C19 -0.1(10) . . . . ?
P1 C15 C20 C19 -176.3(5) . . . . ?
C18 C19 C20 C15 0.7(11) . . . . ?
C7 P1 C21 C26 -123.9(5) . . . . ?
C15 P1 C21 C26 129.8(5) . . . . ?
Mo1 P1 C21 C26 0.8(6) . . . . ?
C7 P1 C21 C22 57.3(6) . . . . ?
C15 P1 C21 C22 -48.9(6) . . . . ?
Mo1 P1 C21 C22 -178.0(4) . . . . ?
C26 C21 C22 C23 1.6(9) . . . . ?
P1 C21 C22 C23 -179.7(5) . . . . ?
C21 C22 C23 C24 -1.1(10) . . . . ?
C22 C23 C24 C25 1.6(11) . . . . ?
C23 C24 C25 C26 -2.5(10) . . . . ?
C22 C21 C26 C25 -2.5(9) . . . . ?
P1 C21 C26 C25 178.7(5) . . . . ?
C24 C25 C26 C21 3.0(10) . . . . ?
C33 P2 C27 C28 94.4(6) . . . . ?
C8 P2 C27 C28 -10.3(6) . . . . ?
Mo1 P2 C27 C28 -133.2(5) . . . . ?
C33 P2 C27 C32 -84.5(5) . . . . ?
C8 P2 C27 C32 170.8(5) . . . . ?
Mo1 P2 C27 C32 48.0(5) . . . . ?
C32 C27 C28 C29 -1.5(9) . . . . ?
P2 C27 C28 C29 179.6(5) . . . . ?
C27 C28 C29 C30 0.3(10) . . . . ?
C28 C29 C30 C31 1.3(11) . . . . ?
C29 C30 C31 C32 -1.7(11) . . . . ?
C30 C31 C32 C27 0.4(11) . . . . ?
C28 C27 C32 C31 1.1(10) . . . . ?
P2 C27 C32 C31 -179.9(5) . . . . ?
C27 P2 C33 C38 131.6(6) . . . . ?
C8 P2 C33 C38 -122.1(6) . . . . ?
Mo1 P2 C33 C38 1.7(7) . . . . ?
C27 P2 C33 C34 -45.6(6) . . . . ?
C8 P2 C33 C34 60.7(6) . . . . ?
Mo1 P2 C33 C34 -175.6(5) . . . . ?
C38 C33 C34 C35 1.1(11) . . . . ?
P2 C33 C34 C35 178.4(6) . . . . ?
C33 C34 C35 C36 -2.2(12) . . . . ?
C34 C35 C36 C37 2.7(12) . . . . ?
C35 C36 C37 C38 -2.0(12) . . . . ?
C34 C33 C38 C37 -0.3(11) . . . . ?
P2 C33 C38 C37 -177.6(6) . . . . ?
C36 C37 C38 C33 0.8(12) . . . . ?
C42 O4 C39 C40 20(3) . . . . ?
O4 C39 C40 C41 -11(3) . . . . ?
C39 C40 C41 C42 0(3) . . . . ?
C39 O4 C42 C41 -20.3(19) . . . . ?
C40 C41 C42 O4 12.6(19) . . . . ?

_refine_diff_density_max         1.681
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.152




_publcif_funding_html            
;
;
####################################################################### 
# 
# 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_14
_database_code_depnum_ccdc_archive 'CCDC 1545379'

_audit_update_record             
;
2017-06-22 deposited with the CCDC.
2017-07-10 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         'C44 H39 Mo O3 P3'
_chemical_formula_sum            'C44 H39 Mo O3 P3'
_chemical_formula_weight         804.60

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'
Mo Mo -1.6832 0.6857 '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      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   17.9235(14)
_cell_length_b                   17.9235(14)
_cell_length_c                   10.2589(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2854.2(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    170
_cell_measurement_reflns_used    7047
_cell_measurement_theta_min      3.2530
_cell_measurement_theta_max      29.4230

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_F_000             1242
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean 8.4171
_diffrn_reflns_number            17979
_diffrn_reflns_av_unetI/netI     0.1352
_diffrn_reflns_av_R_equivalents  0.1558
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.291
_diffrn_reflns_theta_max         36.580
_diffrn_reflns_theta_full        26.3154
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4527
_reflns_number_gt                3385
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_max     0.724
_reflns_Friedel_fraction_full    0.998

_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
;
Olex2, OlexSys Ltd,
Version 1.2
(compiled Mar  28 2017)
;
_computing_publication_material  
;
publCIF, IUCr,
Version 1.9.20_c
;
_refine_special_details          
;
 Refined as a 2-component 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)+(0.1271P)²+10.0897P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1136 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.08(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4527
_refine_ls_number_parameters     151
_refine_ls_number_restraints     118
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0938
_refine_ls_wR_factor_ref         0.2400
_refine_ls_wR_factor_gt          0.2094
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.053
_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
Mo1 Mo 1.000000 1.000000 0.92203(9) 0.0196(3) Uani 1 3 d S T P . .
P5 P 1.1040(2) 1.1133(2) 1.0769(3) 0.0254(7) Uani 1 1 d . . . . .
C1 C 1.000000 1.000000 1.437(2) 0.039(4) Uani 1 3 d S TU P . .
H1A H 0.942057 0.965372 1.468629 0.058 Uiso 0.3333 1 calc R U P . .
H1B H 1.023315 1.057943 1.468630 0.058 Uiso 0.3333 1 calc R U P . .
H1C H 1.034628 0.976685 1.468629 0.058 Uiso 0.3333 1 calc R U P . .
C2 C 1.000000 1.000000 1.2874(17) 0.030(3) Uani 1 3 d S TU P . .
C3 C 1.0935(8) 1.0692(9) 1.2441(13) 0.029(3) Uani 1 1 d . U . . .
H3A H 1.129976 1.043606 1.250359 0.035 Uiso 1 1 calc R U . . .
H3B H 1.115417 1.116696 1.305351 0.035 Uiso 1 1 calc R U . . .
C4 C 1.2178(8) 1.1610(8) 1.0362(12) 0.0253(16) Uani 1 1 d . U . . .
C5 C 1.2461(10) 1.2138(10) 0.9268(15) 0.034(3) Uani 1 1 d . U . . .
H5 H 1.207152 1.224487 0.882195 0.041 Uiso 1 1 calc R U . . .
C6 C 1.3296(11) 1.2510(11) 0.8820(17) 0.042(3) Uani 1 1 d . U . . .
H6 H 1.347486 1.287809 0.810406 0.050 Uiso 1 1 calc R U . . .
C7 C 1.3873(13) 1.2318(15) 0.948(2) 0.056(4) Uani 1 1 d . U . . .
H7 H 1.443389 1.254071 0.917406 0.067 Uiso 1 1 calc R U . . .
C8 C 1.3624(11) 1.1842(19) 1.0477(17) 0.049(3) Uani 1 1 d . U . . .
H8 H 1.402065 1.173651 1.090026 0.058 Uiso 1 1 calc R U . . .
C9 C 1.2786(10) 1.1464(12) 1.0988(14) 0.035(3) Uani 1 1 d . U . . .
H9 H 1.263848 1.112217 1.173096 0.042 Uiso 1 1 calc R U . . .
C10 C 1.1042(12) 1.2138(6) 1.1092(11) 0.029(2) Uani 1 1 d . U . . .
C11 C 1.1610(11) 1.2739(10) 1.1980(17) 0.045(4) Uani 1 1 d . U . . .
H11 H 1.196548 1.260231 1.246035 0.055 Uiso 1 1 calc R U . . .
C12 C 1.1670(15) 1.3524(9) 1.2183(16) 0.046(4) Uani 1 1 d . U . . .
H12 H 1.205613 1.390349 1.279480 0.056 Uiso 1 1 calc R U . . .
C13 C 1.1158(12) 1.3752(9) 1.1478(17) 0.044(4) Uani 1 1 d . U . . .
H13 H 1.118721 1.427821 1.161890 0.053 Uiso 1 1 calc R U . . .
C14 C 1.0606(11) 1.3187(9) 1.0569(16) 0.040(3) Uani 1 1 d . U . . .
H14 H 1.026276 1.333646 1.008181 0.048 Uiso 1 1 calc R U . . .
C15 C 1.0548(8) 1.2398(9) 1.0362(14) 0.032(3) Uani 1 1 d . U . . .
H15 H 1.017489 1.203142 0.972645 0.038 Uiso 1 1 calc R U . . .
O1A O 0.8845(8) 0.8570(9) 0.7240(14) 0.0253(16) Uani 0.77(3) 1 d . . P A 1
C1A C 0.9230(13) 0.9045(12) 0.8017(19) 0.0253(16) Uani 0.77(3) 1 d . U P A 1
O1B O 0.889(3) 0.831(3) 0.758(5) 0.0253(16) Uani 0.23(3) 1 d . . P A 2
C1B C 0.933(4) 0.885(3) 0.802(6) 0.0253(16) Uani 0.23(3) 1 d . 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
Mo1 C1A 1.999(16) 3_675 ?
Mo1 C1A 1.999(17) 2_765 ?
Mo1 C1A 1.999(17) . ?
Mo1 C1B 2.17(5) 3_675 ?
Mo1 C1B 2.17(5) 2_765 ?
Mo1 C1B 2.17(5) . ?
Mo1 P5 2.518(4) . ?
Mo1 P5 2.518(4) 2_765 ?
Mo1 P5 2.518(4) 3_675 ?
P5 C4 1.822(14) . ?
P5 C10 1.829(14) . ?
P5 C3 1.859(14) . ?
C1 C2 1.54(3) . ?
C2 C3 1.570(14) . ?
C2 C3 1.570(14) 3_675 ?
C2 C3 1.570(14) 2_765 ?
C4 C5 1.39(2) . ?
C4 C9 1.40(2) . ?
C5 C6 1.38(2) . ?
C6 C7 1.41(3) . ?
C7 C8 1.26(3) . ?
C8 C9 1.40(2) . ?
C10 C11 1.389(19) . ?
C10 C15 1.41(2) . ?
C11 C12 1.37(2) . ?
C12 C13 1.38(3) . ?
C13 C14 1.37(2) . ?
C14 C15 1.38(2) . ?
O1A C1A 1.117(19) . ?
O1B C1B 1.00(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
C1A Mo1 C1A 85.8(9) 3_675 2_765 ?
C1A Mo1 C1A 85.8(9) 3_675 . ?
C1A Mo1 C1A 85.8(9) 2_765 . ?
C1A Mo1 C1B 11.6(19) 3_675 3_675 ?
C1A Mo1 C1B 95.6(16) 2_765 3_675 ?
C1A Mo1 C1B 80.3(19) . 3_675 ?
C1A Mo1 C1B 80.3(19) 3_675 2_765 ?
C1A Mo1 C1B 11.6(19) 2_765 2_765 ?
C1A Mo1 C1B 95.6(16) . 2_765 ?
C1B Mo1 C1B 91(2) 3_675 2_765 ?
C1B Mo1 C1B 91(2) 3_675 . ?
C1B Mo1 C1B 91(2) 2_765 . ?
C1A Mo1 P5 98.3(6) 3_675 . ?
C1A Mo1 P5 91.6(6) 2_765 . ?
C1A Mo1 P5 175.0(6) . . ?
C1B Mo1 P5 104.2(19) 3_675 . ?
C1B Mo1 P5 82.4(16) 2_765 . ?
C1B Mo1 P5 163.4(19) . . ?
C1A Mo1 P5 91.6(6) 3_675 2_765 ?
C1A Mo1 P5 175.0(6) 2_765 2_765 ?
C1A Mo1 P5 98.3(6) . 2_765 ?
C1B Mo1 P5 82.4(16) 3_675 2_765 ?
C1B Mo1 P5 163.4(19) 2_765 2_765 ?
C1B Mo1 P5 104.2(19) . 2_765 ?
P5 Mo1 P5 84.42(12) . 2_765 ?
C1A Mo1 P5 175.0(6) 3_675 3_675 ?
C1A Mo1 P5 98.3(6) 2_765 3_675 ?
C1A Mo1 P5 91.6(6) . 3_675 ?
P5 Mo1 P5 84.42(12) . 3_675 ?
P5 Mo1 P5 84.42(12) 2_765 3_675 ?
C4 P5 C10 97.4(7) . . ?
C4 P5 C3 105.2(6) . . ?
C10 P5 C3 101.6(6) . . ?
C4 P5 Mo1 115.9(4) . . ?
C10 P5 Mo1 123.0(6) . . ?
C3 P5 Mo1 111.2(5) . . ?
C1 C2 C3 106.4(8) . . ?
C1 C2 C3 106.4(8) . 3_675 ?
C3 C2 C3 112.3(7) . 3_675 ?
C1 C2 C3 106.4(8) . 2_765 ?
C3 C2 C3 112.3(7) . 2_765 ?
C3 C2 C3 112.3(7) 3_675 2_765 ?
C2 C3 P5 116.0(9) . . ?
C5 C4 C9 116.4(14) . . ?
C5 C4 P5 116.5(11) . . ?
C9 C4 P5 127.0(11) . . ?
C6 C5 C4 122.5(16) . . ?
C5 C6 C7 118.2(16) . . ?
C8 C7 C6 119.8(18) . . ?
C7 C8 C9 124(2) . . ?
C4 C9 C8 119.0(16) . . ?
C11 C10 C15 115.5(12) . . ?
C11 C10 P5 121.5(15) . . ?
C15 C10 P5 122.6(10) . . ?
C12 C11 C10 123.1(17) . . ?
C11 C12 C13 120.0(15) . . ?
C14 C13 C12 118.7(14) . . ?
C13 C14 C15 121.2(17) . . ?
C14 C15 C10 121.4(13) . . ?
O1A C1A Mo1 172.7(17) . . ?
O1B C1B Mo1 166(6) . . ?

_refine_diff_density_max         4.006
_refine_diff_density_min         -1.697
_refine_diff_density_rms         0.221




_publcif_funding_html            
;
;
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1545160'

_audit_update_record             
;
2017-06-22 deposited with the CCDC.
2017-07-10 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         'C39 H40 N2 Ni P2 S, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C41 H43 B2 F8 N3 Ni P2 S'
_chemical_formula_weight         904.11

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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

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

_cell_length_a                   25.31933(15)
_cell_length_b                   9.23175(6)
_cell_length_c                   17.87030(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4177.04(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    106.7(2)
_cell_measurement_reflns_used    14743
_cell_measurement_theta_min      4.2520
_cell_measurement_theta_max      73.9480
_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_F_000             1864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.052
_exptl_absorpt_coefficient_mu    2.470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84940
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      106.7(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_reflns_number            19119
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.4915
_diffrn_reflns_theta_max         74.1005
_diffrn_reflns_theta_full        66.9682
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_point_group_measured_fraction_full 0.904
_reflns_number_total             7554
_reflns_number_gt                7518
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.731
_reflns_Friedel_fraction_max     0.777
_reflns_Friedel_fraction_full    0.802

_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
;
Olex2, OlexSys Ltd,
Version 1.2
(compiled Mar  28 2017)  
;
_cumputing_publication_material  
;
publCIF, IUCr,
Version 1.9.20_c
;
_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)+(0.0378P)²+1.3471P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3146 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7554
_refine_ls_number_parameters     554
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0626
_refine_ls_wR_factor_gt          0.0625
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
Ni1 Ni 0.58689(2) 0.90180(4) 0.30694(3) 0.02003(10) Uani 1 1 d . . . . .
P2 P 0.51123(2) 0.97796(5) 0.26135(4) 0.01972(12) Uani 1 1 d . . . . .
P3 P 0.62695(2) 1.10201(5) 0.27337(3) 0.01811(12) Uani 1 1 d . . . . .
S4 S 0.55905(2) 1.17545(6) 0.01666(4) 0.02472(12) Uani 1 1 d . . . . .
F5 F 0.41864(6) 0.37362(17) 0.58729(11) 0.0374(4) Uani 1 1 d . . . . .
F6 F 0.33471(6) 0.28556(18) 0.58730(11) 0.0369(4) Uani 1 1 d . . . . .
F7 F 0.39606(6) 0.19230(18) 0.66670(12) 0.0418(4) Uani 1 1 d . . . . .
N8 N 0.55217(7) 0.7380(2) 0.34858(13) 0.0240(4) Uani 1 1 d . . . . .
F9 F 0.36461(8) 0.4216(2) 0.68460(13) 0.0550(5) Uani 1 1 d . . . . .
N10 N 0.65226(7) 0.8398(2) 0.34884(13) 0.0248(4) Uani 1 1 d . . . . .
C11 C 0.61944(10) 1.2491(3) 0.48778(16) 0.0290(5) Uani 1 1 d . . . . .
H11 H 0.614117 1.208157 0.534718 0.035 Uiso 1 1 calc R U . . .
C12 C 0.69708(8) 1.0749(2) 0.25345(15) 0.0219(5) Uani 1 1 d . . . . .
C13 C 0.69213(9) 0.8134(2) 0.37497(15) 0.0247(5) Uani 1 1 d . . . . .
C14 C 0.43142(9) 0.7754(3) 0.28763(16) 0.0268(5) Uani 1 1 d . . . . .
H14 H 0.425699 0.825512 0.332056 0.032 Uiso 1 1 calc R U . . .
C15 C 0.62917(10) 1.3970(3) 0.48094(17) 0.0302(6) Uani 1 1 d . . . . .
H15 H 0.629910 1.455605 0.523263 0.036 Uiso 1 1 calc R U . . .
C16 C 0.52620(9) 1.3361(2) 0.22894(15) 0.0219(5) Uani 1 1 d . . . . .
H16A H 0.531500 1.303023 0.279304 0.033 Uiso 1 1 calc R U . . .
H16B H 0.489175 1.350985 0.220264 0.033 Uiso 1 1 calc R U . . .
H16C H 0.544769 1.425693 0.221629 0.033 Uiso 1 1 calc R U . . .
C17 C 0.61775(9) 1.1636(3) 0.42420(15) 0.0244(5) Uani 1 1 d . . . . .
H17 H 0.611199 1.064868 0.428793 0.029 Uiso 1 1 calc R U . . .
C19 C 0.44798(10) 0.6257(3) 0.15500(18) 0.0315(6) Uani 1 1 d . . . . .
H19 H 0.453512 0.575499 0.110569 0.038 Uiso 1 1 calc R U . . .
C20 C 0.54716(8) 1.2226(2) 0.17416(14) 0.0191(4) Uani 1 1 d . . . . .
C21 C 0.60623(8) 1.1928(2) 0.18783(14) 0.0197(4) Uani 1 1 d . . . . .
H21A H 0.624441 1.285184 0.185807 0.024 Uiso 1 1 calc R U . . .
H21B H 0.619008 1.135606 0.146065 0.024 Uiso 1 1 calc R U . . .
C23 C 0.73534(9) 1.1392(3) 0.29852(18) 0.0316(6) Uani 1 1 d . . . . .
H23 H 0.725529 1.195929 0.339224 0.038 Uiso 1 1 calc R U . . .
C24 C 0.40181(9) 0.6522(3) 0.27109(18) 0.0319(6) Uani 1 1 d . . . . .
H24 H 0.376430 0.619795 0.304804 0.038 Uiso 1 1 calc R U . . .
C25 C 0.45173(10) 1.1731(3) 0.44919(17) 0.0306(6) Uani 1 1 d . . . . .
H25 H 0.460730 1.182109 0.499427 0.037 Uiso 1 1 calc R U . . .
C26 C 0.48397(9) 1.0937(2) 0.40098(16) 0.0257(5) Uani 1 1 d . . . . .
H26 H 0.514274 1.049001 0.419203 0.031 Uiso 1 1 calc R U . . .
C27 C 0.39294(9) 1.2258(3) 0.34715(19) 0.0330(6) Uani 1 1 d . . . . .
H27 H 0.362451 1.269951 0.329223 0.040 Uiso 1 1 calc R U . . .
C28 C 0.40628(10) 1.2386(3) 0.42221(19) 0.0330(6) Uani 1 1 d . . . . .
H28 H 0.384707 1.291083 0.454429 0.040 Uiso 1 1 calc R U . . .
C29 C 0.74332(10) 0.7819(3) 0.40735(18) 0.0345(6) Uani 1 1 d . . . . .
H29A H 0.767682 0.857635 0.394554 0.052 Uiso 1 1 calc R U . . .
H29B H 0.756079 0.691288 0.388171 0.052 Uiso 1 1 calc R U . . .
H29C H 0.740120 0.775896 0.460793 0.052 Uiso 1 1 calc R U . . .
C30 C 0.40987(9) 0.5779(3) 0.20518(18) 0.0321(6) Uani 1 1 d . . . . .
H30 H 0.389852 0.496114 0.194319 0.039 Uiso 1 1 calc R U . . .
C31 C 0.63599(9) 1.3718(3) 0.34677(15) 0.0239(5) Uani 1 1 d . . . . .
H31 H 0.641552 1.413006 0.299941 0.029 Uiso 1 1 calc R U . . .
C32 C 0.62571(8) 1.2231(2) 0.35348(14) 0.0210(5) Uani 1 1 d . . . . .
C33 C 0.73298(13) 1.2770(5) -0.0189(2) 0.0579(10) Uani 1 1 d . . . . .
H33 H 0.768578 1.297453 -0.026175 0.069 Uiso 1 1 calc R U . . .
C34 C 0.63776(10) 1.4566(3) 0.41060(16) 0.0285(5) Uani 1 1 d . . . . .
H34 H 0.644814 1.555079 0.406326 0.034 Uiso 1 1 calc R U . . .
C35 C 0.71188(10) 0.9880(3) 0.19398(17) 0.0324(6) Uani 1 1 d . . . . .
H35 H 0.686283 0.942573 0.164949 0.039 Uiso 1 1 calc R U . . .
C37 C 0.51518(8) 1.0805(2) 0.17487(15) 0.0210(5) Uani 1 1 d . . . . .
H37A H 0.529986 1.017279 0.136916 0.025 Uiso 1 1 calc R U . . .
H37B H 0.479401 1.103314 0.159491 0.025 Uiso 1 1 calc R U . . .
C39 C 0.46977(8) 0.8234(2) 0.23703(15) 0.0230(5) Uani 1 1 d . . . . .
C40 C 0.42475(9) 1.1477(3) 0.29890(18) 0.0293(5) Uani 1 1 d . . . . .
H40 H 0.415652 1.139152 0.248679 0.035 Uiso 1 1 calc R U . . .
C41 C 0.47088(8) 1.0814(2) 0.32601(15) 0.0235(5) Uani 1 1 d . . . . .
C42 C 0.47793(9) 0.7483(2) 0.17090(16) 0.0271(5) Uani 1 1 d . . . . .
H42 H 0.503422 0.779826 0.137150 0.032 Uiso 1 1 calc R U . . .
C43 C 0.62714(10) 1.2162(3) 0.00348(14) 0.0262(5) Uani 1 1 d . . . . .
C45 C 0.54080(9) 1.2898(2) 0.09563(14) 0.0215(5) Uani 1 1 d . . . . .
H45A H 0.561982 1.377227 0.093536 0.026 Uiso 1 1 calc R U . . .
H45B H 0.504184 1.318307 0.089477 0.026 Uiso 1 1 calc R U . . .
C47 C 0.66426(12) 1.1051(3) 0.00689(18) 0.0391(7) Uani 1 1 d . . . . .
H47 H 0.653694 1.010531 0.016744 0.047 Uiso 1 1 calc R U . . .
B48 B 0.37793(11) 0.3196(3) 0.6319(2) 0.0312(7) Uani 1 1 d . . . . .
C51 C 0.76511(10) 0.9687(3) 0.17769(19) 0.0399(7) Uani 1 1 d . . . . .
H51 H 0.775124 0.910937 0.137469 0.048 Uiso 1 1 calc R U . . .
C52 C 0.71712(13) 1.1371(5) -0.0046(2) 0.0532(9) Uani 1 1 d . . . . .
H52 H 0.742107 1.063349 -0.002525 0.064 Uiso 1 1 calc R U . . .
C53 C 0.64331(11) 1.3570(3) -0.01119(17) 0.0350(6) Uani 1 1 d . . . . .
H53 H 0.618506 1.431221 -0.013363 0.042 Uiso 1 1 calc R U . . .
C55 C 0.69608(13) 1.3874(4) -0.0226(2) 0.0480(8) Uani 1 1 d . . . . .
H55 H 0.706810 1.481720 -0.032657 0.058 Uiso 1 1 calc R U . . .
C56 C 0.78854(10) 1.1175(3) 0.2818(2) 0.0405(7) Uani 1 1 d . . . . .
H56 H 0.814356 1.159124 0.311918 0.049 Uiso 1 1 calc R U . . .
C59 C 0.80318(10) 1.0352(4) 0.2212(2) 0.0412(7) Uani 1 1 d . . . . .
H59 H 0.838739 1.024156 0.209489 0.049 Uiso 1 1 calc R U . . .
C3 C 0.53119(9) 0.6444(2) 0.37669(14) 0.0218(5) Uani 1 1 d . . . . .
C1 C 0.50346(10) 0.5246(2) 0.41171(16) 0.0262(5) Uani 1 1 d . . . . .
H1A H 0.470382 0.509225 0.386681 0.039 Uiso 1 1 calc R U . . .
H1B H 0.497097 0.546733 0.463411 0.039 Uiso 1 1 calc R U . . .
H1C H 0.524582 0.438462 0.408178 0.039 Uiso 1 1 calc R U . . .
F1 F 0.83641(9) 0.7715(5) 0.03548(16) 0.1086(13) Uani 1 1 d . . . . .
F3 F 0.88958(16) 0.7837(5) 0.1373(2) 0.0454(9) Uani 0.5 1 d . . P A 1
B4 B 0.88559(14) 0.7959(4) 0.06109(19) 0.0376(7) Uani 1 1 d . . . . .
F2 F 0.88877(16) 0.9361(4) 0.0977(3) 0.0572(11) Uani 0.5 1 d . . P A 2
F4 F 0.91819(14) 0.6856(5) 0.0301(2) 0.0464(9) Uani 0.5 1 d . . P A 1
F8 F 0.92093(19) 0.8108(9) 0.0028(3) 0.085(2) Uani 0.5 1 d . . P A 2
N1 N 0.77940(12) 0.5359(3) 0.28784(19) 0.0548(8) Uani 1 1 d . . . . .
C2 C 0.76044(17) 0.4715(7) 0.1505(2) 0.0910(19) Uani 1 1 d . . . . .
H2A H 0.778775 0.538002 0.118338 0.137 Uiso 1 1 calc R U . . .
H2B H 0.723188 0.477341 0.140941 0.137 Uiso 1 1 calc R U . . .
H2C H 0.772528 0.374751 0.140810 0.137 Uiso 1 1 calc R U . . .
C4 C 0.77076(12) 0.5085(4) 0.2279(2) 0.0461(8) Uani 1 1 d . . . . .
F10 F 0.9010(2) 0.7035(6) 0.1108(4) 0.0775(18) Uani 0.5 1 d . . P A 2
F11 F 0.8982(6) 0.9149(6) 0.0382(4) 0.214(7) Uani 0.5 1 d . . P A 1


_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
Ni1 N8 1.901(2) . ?
Ni1 N10 1.905(2) . ?
Ni1 P3 2.1921(6) . ?
Ni1 P2 2.1972(6) . ?
P2 C41 1.814(2) . ?
P2 C37 1.815(2) . ?
P2 C39 1.824(2) . ?
P3 C32 1.817(3) . ?
P3 C21 1.821(2) . ?
P3 C12 1.828(2) . ?
S4 C43 1.780(2) . ?
S4 C45 1.822(3) . ?
F5 B48 1.395(4) . ?
F6 B48 1.389(3) . ?
F7 B48 1.407(3) . ?
N8 C3 1.132(3) . ?
F9 B48 1.375(4) . ?
N10 C13 1.139(3) . ?
C11 C17 1.384(4) . ?
C11 C15 1.392(4) . ?
C11 H11 0.9300 . ?
C12 C35 1.383(4) . ?
C12 C23 1.393(4) . ?
C13 C29 1.449(3) . ?
C14 C24 1.395(3) . ?
C14 C39 1.399(3) . ?
C14 H14 0.9300 . ?
C15 C34 1.389(4) . ?
C15 H15 0.9300 . ?
C16 C20 1.529(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C32 1.393(4) . ?
C17 H17 0.9300 . ?
C19 C30 1.389(4) . ?
C19 C42 1.392(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.540(3) . ?
C20 C37 1.542(3) . ?
C20 C45 1.543(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C23 C56 1.394(3) . ?
C23 H23 0.9300 . ?
C24 C30 1.378(5) . ?
C24 H24 0.9300 . ?
C25 C28 1.386(4) . ?
C25 C26 1.395(4) . ?
C25 H25 0.9300 . ?
C26 C41 1.385(4) . ?
C26 H26 0.9300 . ?
C27 C40 1.383(4) . ?
C27 C28 1.388(5) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30 0.9300 . ?
C31 C34 1.384(4) . ?
C31 C32 1.403(3) . ?
C31 H31 0.9300 . ?
C33 C52 1.377(6) . ?
C33 C55 1.384(6) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 C51 1.390(3) . ?
C35 H35 0.9300 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C39 C42 1.386(4) . ?
C40 C41 1.405(3) . ?
C40 H40 0.9300 . ?
C42 H42 0.9300 . ?
C43 C53 1.388(4) . ?
C43 C47 1.392(4) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C47 C52 1.386(4) . ?
C47 H47 0.9300 . ?
C51 C59 1.382(4) . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?
C53 C55 1.380(4) . ?
C53 H53 0.9300 . ?
C55 H55 0.9300 . ?
C56 C59 1.373(5) . ?
C56 H56 0.9300 . ?
C59 H59 0.9300 . ?
C3 C1 1.452(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
F1 B4 1.346(4) . ?
F3 B4 1.370(5) . ?
B4 F11 1.215(8) . ?
B4 F10 1.292(6) . ?
B4 F8 1.380(6) . ?
B4 F4 1.423(5) . ?
B4 F2 1.452(5) . ?
N1 C4 1.123(5) . ?
C2 C4 1.448(6) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?

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
N8 Ni1 N10 90.51(8) . . ?
N8 Ni1 P3 172.72(8) . . ?
N10 Ni1 P3 87.64(6) . . ?
N8 Ni1 P2 89.80(6) . . ?
N10 Ni1 P2 178.29(8) . . ?
P3 Ni1 P2 91.84(2) . . ?
C41 P2 C37 107.40(11) . . ?
C41 P2 C39 103.85(11) . . ?
C37 P2 C39 103.70(11) . . ?
C41 P2 Ni1 115.04(9) . . ?
C37 P2 Ni1 115.75(7) . . ?
C39 P2 Ni1 109.86(7) . . ?
C32 P3 C21 111.93(10) . . ?
C32 P3 C12 104.74(11) . . ?
C21 P3 C12 100.35(11) . . ?
C32 P3 Ni1 107.16(8) . . ?
C21 P3 Ni1 118.99(7) . . ?
C12 P3 Ni1 112.78(7) . . ?
C43 S4 C45 103.05(11) . . ?
C3 N8 Ni1 176.4(2) . . ?
C13 N10 Ni1 174.84(19) . . ?
C17 C11 C15 119.5(3) . . ?
C17 C11 H11 120.2 . . ?
C15 C11 H11 120.2 . . ?
C35 C12 C23 120.2(2) . . ?
C35 C12 P3 119.48(18) . . ?
C23 C12 P3 120.3(2) . . ?
N10 C13 C29 178.9(3) . . ?
C24 C14 C39 119.6(3) . . ?
C24 C14 H14 120.2 . . ?
C39 C14 H14 120.2 . . ?
C34 C15 C11 119.7(3) . . ?
C34 C15 H15 120.2 . . ?
C11 C15 H15 120.2 . . ?
C20 C16 H16A 109.5 . . ?
C20 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C20 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C17 C32 121.0(2) . . ?
C11 C17 H17 119.5 . . ?
C32 C17 H17 119.5 . . ?
C30 C19 C42 120.3(3) . . ?
C30 C19 H19 119.8 . . ?
C42 C19 H19 119.8 . . ?
C16 C20 C21 110.95(19) . . ?
C16 C20 C37 113.32(19) . . ?
C21 C20 C37 110.91(17) . . ?
C16 C20 C45 105.69(17) . . ?
C21 C20 C45 108.50(18) . . ?
C37 C20 C45 107.15(19) . . ?
C20 C21 P3 119.68(16) . . ?
C20 C21 H21A 107.4 . . ?
P3 C21 H21A 107.4 . . ?
C20 C21 H21B 107.4 . . ?
P3 C21 H21B 107.4 . . ?
H21A C21 H21B 106.9 . . ?
C12 C23 C56 119.1(3) . . ?
C12 C23 H23 120.4 . . ?
C56 C23 H23 120.4 . . ?
C30 C24 C14 120.5(2) . . ?
C30 C24 H24 119.8 . . ?
C14 C24 H24 119.8 . . ?
C28 C25 C26 120.0(3) . . ?
C28 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C41 C26 C25 120.0(2) . . ?
C41 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C40 C27 C28 120.3(2) . . ?
C40 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C25 C28 C27 120.1(2) . . ?
C25 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C13 C29 H29A 109.5 . . ?
C13 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C13 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C24 C30 C19 119.8(2) . . ?
C24 C30 H30 120.1 . . ?
C19 C30 H30 120.1 . . ?
C34 C31 C32 119.3(2) . . ?
C34 C31 H31 120.4 . . ?
C32 C31 H31 120.4 . . ?
C17 C32 C31 119.4(2) . . ?
C17 C32 P3 118.37(17) . . ?
C31 C32 P3 122.1(2) . . ?
C52 C33 C55 120.2(3) . . ?
C52 C33 H33 119.9 . . ?
C55 C33 H33 119.9 . . ?
C31 C34 C15 121.1(2) . . ?
C31 C34 H34 119.4 . . ?
C15 C34 H34 119.4 . . ?
C12 C35 C51 119.9(3) . . ?
C12 C35 H35 120.1 . . ?
C51 C35 H35 120.1 . . ?
C20 C37 P2 118.67(18) . . ?
C20 C37 H37A 107.6 . . ?
P2 C37 H37A 107.6 . . ?
C20 C37 H37B 107.6 . . ?
P2 C37 H37B 107.6 . . ?
H37A C37 H37B 107.1 . . ?
C42 C39 C14 119.8(2) . . ?
C42 C39 P2 120.57(17) . . ?
C14 C39 P2 119.5(2) . . ?
C27 C40 C41 119.8(3) . . ?
C27 C40 H40 120.1 . . ?
C41 C40 H40 120.1 . . ?
C26 C41 C40 119.8(2) . . ?
C26 C41 P2 121.64(17) . . ?
C40 C41 P2 118.6(2) . . ?
C39 C42 C19 120.0(2) . . ?
C39 C42 H42 120.0 . . ?
C19 C42 H42 120.0 . . ?
C53 C43 C47 119.9(3) . . ?
C53 C43 S4 120.6(2) . . ?
C47 C43 S4 119.5(2) . . ?
C20 C45 S4 116.44(15) . . ?
C20 C45 H45A 108.2 . . ?
S4 C45 H45A 108.2 . . ?
C20 C45 H45B 108.2 . . ?
S4 C45 H45B 108.2 . . ?
H45A C45 H45B 107.3 . . ?
C52 C47 C43 119.2(3) . . ?
C52 C47 H47 120.4 . . ?
C43 C47 H47 120.4 . . ?
F9 B48 F6 110.8(2) . . ?
F9 B48 F5 109.1(2) . . ?
F6 B48 F5 109.6(3) . . ?
F9 B48 F7 110.5(3) . . ?
F6 B48 F7 108.8(2) . . ?
F5 B48 F7 108.1(2) . . ?
C59 C51 C35 120.1(3) . . ?
C59 C51 H51 120.0 . . ?
C35 C51 H51 120.0 . . ?
C33 C52 C47 120.6(3) . . ?
C33 C52 H52 119.7 . . ?
C47 C52 H52 119.7 . . ?
C55 C53 C43 120.2(3) . . ?
C55 C53 H53 119.9 . . ?
C43 C53 H53 119.9 . . ?
C53 C55 C33 119.8(3) . . ?
C53 C55 H55 120.1 . . ?
C33 C55 H55 120.1 . . ?
C59 C56 C23 120.6(3) . . ?
C59 C56 H56 119.7 . . ?
C23 C56 H56 119.7 . . ?
C56 C59 C51 120.1(2) . . ?
C56 C59 H59 120.0 . . ?
C51 C59 H59 120.0 . . ?
N8 C3 C1 178.9(3) . . ?
C3 C1 H1A 109.5 . . ?
C3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
F11 B4 F1 106.2(7) . . ?
F10 B4 F1 113.7(4) . . ?
F11 B4 F3 112.9(5) . . ?
F1 B4 F3 113.1(4) . . ?
F10 B4 F8 112.9(5) . . ?
F1 B4 F8 111.1(3) . . ?
F11 B4 F4 111.4(7) . . ?
F1 B4 F4 106.5(3) . . ?
F3 B4 F4 106.6(3) . . ?
F10 B4 F2 105.2(4) . . ?
F1 B4 F2 110.7(3) . . ?
F8 B4 F2 102.4(5) . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C4 C2 179.0(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
C32 P3 C12 C35 -179.2(2) . . . . ?
C21 P3 C12 C35 -63.0(2) . . . . ?
Ni1 P3 C12 C35 64.6(2) . . . . ?
C32 P3 C12 C23 1.9(2) . . . . ?
C21 P3 C12 C23 118.0(2) . . . . ?
Ni1 P3 C12 C23 -114.32(19) . . . . ?
C17 C11 C15 C34 -0.9(4) . . . . ?
C15 C11 C17 C32 0.1(4) . . . . ?
C16 C20 C21 P3 68.4(2) . . . . ?
C37 C20 C21 P3 -58.5(3) . . . . ?
C45 C20 C21 P3 -175.92(15) . . . . ?
C32 P3 C21 C20 -76.63(19) . . . . ?
C12 P3 C21 C20 172.74(17) . . . . ?
Ni1 P3 C21 C20 49.3(2) . . . . ?
C35 C12 C23 C56 1.5(4) . . . . ?
P3 C12 C23 C56 -179.6(2) . . . . ?
C39 C14 C24 C30 -0.4(4) . . . . ?
C28 C25 C26 C41 0.6(3) . . . . ?
C26 C25 C28 C27 -0.3(4) . . . . ?
C40 C27 C28 C25 0.1(4) . . . . ?
C14 C24 C30 C19 0.4(4) . . . . ?
C42 C19 C30 C24 -0.2(4) . . . . ?
C11 C17 C32 C31 0.5(3) . . . . ?
C11 C17 C32 P3 176.24(18) . . . . ?
C34 C31 C32 C17 -0.3(3) . . . . ?
C34 C31 C32 P3 -175.90(17) . . . . ?
C21 P3 C32 C17 152.55(16) . . . . ?
C12 P3 C32 C17 -99.62(18) . . . . ?
Ni1 P3 C32 C17 20.40(18) . . . . ?
C21 P3 C32 C31 -31.8(2) . . . . ?
C12 P3 C32 C31 76.0(2) . . . . ?
Ni1 P3 C32 C31 -163.97(16) . . . . ?
C32 C31 C34 C15 -0.5(4) . . . . ?
C11 C15 C34 C31 1.1(4) . . . . ?
C23 C12 C35 C51 -2.1(4) . . . . ?
P3 C12 C35 C51 179.0(2) . . . . ?
C16 C20 C37 P2 -60.5(2) . . . . ?
C21 C20 C37 P2 65.1(2) . . . . ?
C45 C20 C37 P2 -176.69(15) . . . . ?
C41 P2 C37 C20 69.71(18) . . . . ?
C39 P2 C37 C20 179.26(16) . . . . ?
Ni1 P2 C37 C20 -60.35(18) . . . . ?
C24 C14 C39 C42 0.1(3) . . . . ?
C24 C14 C39 P2 -176.23(18) . . . . ?
C41 P2 C39 C42 156.89(19) . . . . ?
C37 P2 C39 C42 44.7(2) . . . . ?
Ni1 P2 C39 C42 -79.56(19) . . . . ?
C41 P2 C39 C14 -26.8(2) . . . . ?
C37 P2 C39 C14 -138.90(18) . . . . ?
Ni1 P2 C39 C14 96.79(18) . . . . ?
C28 C27 C40 C41 -0.2(4) . . . . ?
C25 C26 C41 C40 -0.7(3) . . . . ?
C25 C26 C41 P2 -179.43(17) . . . . ?
C27 C40 C41 C26 0.5(3) . . . . ?
C27 C40 C41 P2 179.25(18) . . . . ?
C37 P2 C41 C26 -138.76(18) . . . . ?
C39 P2 C41 C26 111.79(19) . . . . ?
Ni1 P2 C41 C26 -8.3(2) . . . . ?
C37 P2 C41 C40 42.5(2) . . . . ?
C39 P2 C41 C40 -66.9(2) . . . . ?
Ni1 P2 C41 C40 172.96(15) . . . . ?
C14 C39 C42 C19 0.1(3) . . . . ?
P2 C39 C42 C19 176.40(18) . . . . ?
C30 C19 C42 C39 0.0(4) . . . . ?
C45 S4 C43 C53 -58.7(2) . . . . ?
C45 S4 C43 C47 122.3(2) . . . . ?
C16 C20 C45 S4 -176.63(14) . . . . ?
C21 C20 C45 S4 64.3(2) . . . . ?
C37 C20 C45 S4 -55.5(2) . . . . ?
C43 S4 C45 C20 -90.25(18) . . . . ?
C53 C43 C47 C52 -0.1(4) . . . . ?
S4 C43 C47 C52 179.0(2) . . . . ?
C12 C35 C51 C59 0.5(5) . . . . ?
C55 C33 C52 C47 -0.4(6) . . . . ?
C43 C47 C52 C33 0.2(5) . . . . ?
C47 C43 C53 C55 0.1(4) . . . . ?
S4 C43 C53 C55 -178.9(3) . . . . ?
C43 C53 C55 C33 -0.4(5) . . . . ?
C52 C33 C55 C53 0.5(6) . . . . ?
C12 C23 C56 C59 0.7(4) . . . . ?
C23 C56 C59 C51 -2.3(5) . . . . ?
C35 C51 C59 C56 1.6(5) . . . . ?

_refine_diff_density_max         0.513
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.038




_publcif_funding_html            
;
;
####################################################################### 
# 
# 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_12
_database_code_depnum_ccdc_archive 'CCDC 1545163'

_audit_update_record             
;
2017-06-22 deposited with the CCDC.
2017-07-10 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         'C32 H29 Mo O3 P S2'
_chemical_formula_sum            'C32 H29 Mo O3 P S2'
_chemical_formula_weight         652.58

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'
Mo Mo -1.6832 0.6857 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.9008(6)
_cell_length_b                   16.6383(11)
_cell_length_c                   15.8862(9)
_cell_angle_alpha                90
_cell_angle_beta                 97.751(6)
_cell_angle_gamma                90
_cell_volume                     2855.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    8202
_cell_measurement_theta_min      3.1680
_cell_measurement_theta_max      26.3060

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_F_000             1336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95176
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -129.50   68.50   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000    1.0000  290.0000 198

#__ type_ start__ end____ width___ exp.time_
  2 omega  -79.00  117.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000   11.0000  280.0000 196

#__ type_ start__ end____ width___ exp.time_
  3 phi    300.00  330.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -40.0000 -109.0000     -     30

#__ type_ start__ end____ width___ exp.time_
  4 omega  -24.50   34.50   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000   91.0000   90.0000 59

#__ type_ start__ end____ width___ exp.time_
  5 omega   32.00  138.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       40.0000 -179.0000  340.0000 106

#__ type_ start__ end____ width___ exp.time_
  6 omega  -16.50  111.50   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000   51.0000    0.0000 128

#__ type_ start__ end____ width___ exp.time_
  7 phi    130.00  160.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
   0.0000  -40.0000    1.0000     -     30

#__ type_ start__ end____ width___ exp.time_
  8 omega   11.00   41.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000 -129.0000  190.0000 30

#__ type_ start__ end____ width___ exp.time_
  9 omega  -78.00   61.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       20.0000  -79.0000  320.0000 139

#__ type_ start__ end____ width___ exp.time_
 10 omega   56.00  109.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       10.0000  151.0000   20.0000 53

;
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean 8.4171
_diffrn_reflns_number            41654
_diffrn_reflns_av_unetI/netI     0.0797
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.9898
_diffrn_reflns_theta_max         25.6809
_diffrn_reflns_theta_full        25.6263
_diffrn_measured_fraction_theta_max 0.9973
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5407
_reflns_number_gt                3982
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
;
Olex2, OlexSys Ltd,
Version 1.2
(compiled Mar  28 2017)
;
_computing_publication_material  
;
publCIF, IUCr,
Version 1.9.20_c
;
_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)+(0.0225P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5407
_refine_ls_number_parameters     353
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.0868
_refine_ls_wR_factor_gt          0.0762
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.20347(3) 0.65746(2) 0.77265(2) 0.02220(11) Uani 1 1 d . . . . .
S1 S 0.04086(8) 0.64890(5) 0.64232(6) 0.0245(2) Uani 1 1 d . . . . .
P1 P 0.28997(8) 0.54106(6) 0.69648(6) 0.0208(2) Uani 1 1 d . . . . .
S2 S 0.06637(9) 0.55335(6) 0.83674(6) 0.0275(2) Uani 1 1 d . . . . .
O2 O 0.0913(3) 0.79333(16) 0.87452(17) 0.0472(8) Uani 1 1 d . . . . .
C36 C 0.3311(3) 0.4849(2) 0.5345(2) 0.0259(9) Uani 1 1 d . . . . .
H36 H 0.325366 0.433619 0.557009 0.031 Uiso 1 1 calc R U . . .
O3 O 0.3511(3) 0.79255(16) 0.69701(17) 0.0398(7) Uani 1 1 d . . . . .
C24 C 0.6664(4) 0.4554(2) 0.8332(2) 0.0384(11) Uani 1 1 d . . . . .
H24 H 0.742459 0.440025 0.862479 0.046 Uiso 1 1 calc R U . . .
C35 C 0.3536(3) 0.4937(2) 0.4505(2) 0.0288(9) Uani 1 1 d . . . . .
H35 H 0.360557 0.448602 0.416966 0.035 Uiso 1 1 calc R U . . .
C33 C 0.3526(3) 0.6361(2) 0.4669(2) 0.0301(9) Uani 1 1 d . . . . .
H33 H 0.360846 0.687254 0.444580 0.036 Uiso 1 1 calc R U . . .
C32 C 0.3276(3) 0.6273(2) 0.5492(2) 0.0275(9) Uani 1 1 d . . . . .
H32 H 0.317677 0.672798 0.581598 0.033 Uiso 1 1 calc R U . . .
C25 C 0.6517(3) 0.5307(2) 0.7981(2) 0.0325(10) Uani 1 1 d . . . . .
H25 H 0.718185 0.566157 0.802831 0.039 Uiso 1 1 calc R U . . .
C13 C 0.2940(3) 0.7412(2) 0.7230(2) 0.0253(9) Uani 1 1 d . . . . .
C55 C 0.1233(4) 0.3672(2) 0.9999(2) 0.0385(11) Uani 1 1 d . . . . .
H55 H 0.074667 0.331280 1.025779 0.046 Uiso 1 1 calc R U . . .
C52 C 0.2679(4) 0.4741(2) 0.9248(2) 0.0326(10) Uani 1 1 d . . . . .
H52 H 0.316870 0.510687 0.900182 0.039 Uiso 1 1 calc R U . . .
C5 C -0.0205(3) 0.3994(2) 0.6301(2) 0.0327(10) Uani 1 1 d . . . . .
H5A H -0.108666 0.406137 0.624027 0.049 Uiso 1 1 calc R U . . .
H5B H 0.002651 0.353122 0.664769 0.049 Uiso 1 1 calc R U . . .
H5C H 0.005069 0.391923 0.575083 0.049 Uiso 1 1 calc R U . . .
C53 C 0.3234(4) 0.4152(2) 0.9786(2) 0.0435(12) Uani 1 1 d . . . . .
H53 H 0.409209 0.412138 0.990121 0.052 Uiso 1 1 calc R U . . .
C41 C -0.1123(3) 0.6833(2) 0.6521(2) 0.0258(9) Uani 1 1 d . . . . .
C34 C 0.3654(3) 0.5692(2) 0.4176(2) 0.0291(9) Uani 1 1 d . . . . .
H34 H 0.381961 0.575225 0.362042 0.035 Uiso 1 1 calc R U . . .
C51 C 0.1409(4) 0.4789(2) 0.9073(2) 0.0282(9) Uani 1 1 d . . . . .
C23 C 0.5686(4) 0.4027(2) 0.8250(3) 0.0381(11) Uani 1 1 d . . . . .
H23 H 0.578800 0.351646 0.848582 0.046 Uiso 1 1 calc R U . . .
C3 C 0.0135(3) 0.5438(2) 0.6083(2) 0.0246(9) Uani 1 1 d . . . . .
H3A H -0.073254 0.539156 0.585325 0.030 Uiso 1 1 calc R U . . .
H3B H 0.060752 0.534287 0.561729 0.030 Uiso 1 1 calc R U . . .
C1 C 0.1838(3) 0.4554(2) 0.6931(2) 0.0219(8) Uani 1 1 d . . . . .
H1A H 0.205273 0.417734 0.650820 0.026 Uiso 1 1 calc R U . . .
H1B H 0.197465 0.428487 0.747693 0.026 Uiso 1 1 calc R U . . .
C22 C 0.4548(3) 0.4251(2) 0.7817(2) 0.0295(9) Uani 1 1 d . . . . .
H22 H 0.389377 0.388768 0.776101 0.035 Uiso 1 1 calc R U . . .
C46 C -0.1893(4) 0.7026(2) 0.5783(3) 0.0362(10) Uani 1 1 d . . . . .
H46 H -0.163177 0.694072 0.525678 0.043 Uiso 1 1 calc R U . . .
C21 C 0.4379(3) 0.5016(2) 0.7467(2) 0.0232(8) Uani 1 1 d . . . . .
C2 C 0.0433(3) 0.4749(2) 0.6725(2) 0.0245(9) Uani 1 1 d . . . . .
C56 C 0.0674(4) 0.4261(2) 0.9467(2) 0.0358(10) Uani 1 1 d . . . . .
H56 H -0.018408 0.430521 0.937364 0.043 Uiso 1 1 calc R U . . .
C43 C -0.2671(4) 0.7317(2) 0.7336(3) 0.0411(11) Uani 1 1 d . . . . .
H43 H -0.292777 0.742178 0.786037 0.049 Uiso 1 1 calc R U . . .
C45 C -0.3061(4) 0.7347(2) 0.5832(3) 0.0437(12) Uani 1 1 d . . . . .
H45 H -0.358663 0.746640 0.533713 0.052 Uiso 1 1 calc R U . . .
C31 C 0.3170(3) 0.5517(2) 0.5848(2) 0.0227(8) Uani 1 1 d . . . . .
C26 C 0.5384(3) 0.5538(2) 0.7560(2) 0.0272(9) Uani 1 1 d . . . . .
H26 H 0.529027 0.605327 0.733238 0.033 Uiso 1 1 calc R U . . .
C12 C 0.1283(4) 0.7421(2) 0.8354(2) 0.0309(9) Uani 1 1 d . . . . .
C42 C -0.1513(3) 0.6986(2) 0.7297(3) 0.0341(10) Uani 1 1 d . . . . .
H42 H -0.099533 0.686723 0.779626 0.041 Uiso 1 1 calc R U . . .
C54 C 0.2503(5) 0.3611(3) 1.0149(3) 0.0467(12) Uani 1 1 d . . . . .
H54 H 0.286972 0.320321 1.049722 0.056 Uiso 1 1 calc R U . . .
C4 C -0.0157(3) 0.4898(2) 0.7537(2) 0.0301(9) Uani 1 1 d . . . . .
H4A H -0.028806 0.437860 0.778863 0.036 Uiso 1 1 calc R U . . .
H4B H -0.096745 0.513313 0.736988 0.036 Uiso 1 1 calc R U . . .
C44 C -0.3436(4) 0.7488(2) 0.6603(3) 0.0397(11) Uani 1 1 d . . . . .
H44 H -0.421804 0.770237 0.663077 0.048 Uiso 1 1 calc R U . . .
O1 O 0.4263(3) 0.67219(18) 0.91641(19) 0.0562(9) Uani 1 1 d . . . . .
C11 C 0.3413(4) 0.6630(2) 0.8644(3) 0.0344(10) 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
Mo1 C13 1.936(4) . ?
Mo1 C11 1.949(4) . ?
Mo1 C12 1.967(4) . ?
Mo1 P1 2.5322(10) . ?
Mo1 S1 2.5414(9) . ?
Mo1 S2 2.5848(10) . ?
S1 C41 1.791(4) . ?
S1 C3 1.842(3) . ?
P1 C21 1.823(3) . ?
P1 C1 1.832(3) . ?
P1 C31 1.846(4) . ?
S2 C51 1.790(4) . ?
S2 C4 1.828(4) . ?
O2 C12 1.159(4) . ?
C36 C31 1.390(5) . ?
C36 C35 1.396(5) . ?
C36 H36 0.9300 . ?
O3 C13 1.164(4) . ?
C24 C23 1.372(5) . ?
C24 C25 1.372(5) . ?
C24 H24 0.9300 . ?
C35 C34 1.374(5) . ?
C35 H35 0.9300 . ?
C33 C34 1.378(5) . ?
C33 C32 1.380(5) . ?
C33 H33 0.9300 . ?
C32 C31 1.389(5) . ?
C32 H32 0.9300 . ?
C25 C26 1.378(5) . ?
C25 H25 0.9300 . ?
C55 C54 1.377(6) . ?
C55 C56 1.381(5) . ?
C55 H55 0.9300 . ?
C52 C51 1.377(5) . ?
C52 C53 1.385(5) . ?
C52 H52 0.9300 . ?
C5 C2 1.546(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C53 C54 1.380(6) . ?
C53 H53 0.9300 . ?
C41 C42 1.382(5) . ?
C41 C46 1.384(5) . ?
C34 H34 0.9300 . ?
C51 C56 1.393(5) . ?
C23 C22 1.385(5) . ?
C23 H23 0.9300 . ?
C3 C2 1.540(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C1 C2 1.556(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C22 C21 1.392(5) . ?
C22 H22 0.9300 . ?
C46 C45 1.393(5) . ?
C46 H46 0.9300 . ?
C21 C26 1.390(5) . ?
C2 C4 1.537(5) . ?
C56 H56 0.9300 . ?
C43 C44 1.368(5) . ?
C43 C42 1.386(5) . ?
C43 H43 0.9300 . ?
C45 C44 1.362(6) . ?
C45 H45 0.9300 . ?
C26 H26 0.9300 . ?
C42 H42 0.9300 . ?
C54 H54 0.9300 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C44 H44 0.9300 . ?
O1 C11 1.165(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Mo1 C11 83.52(16) . . ?
C13 Mo1 C12 87.74(15) . . ?
C11 Mo1 C12 85.35(15) . . ?
C13 Mo1 P1 96.49(11) . . ?
C11 Mo1 P1 95.41(11) . . ?
C12 Mo1 P1 175.77(11) . . ?
C13 Mo1 S1 92.65(10) . . ?
C11 Mo1 S1 173.93(12) . . ?
C12 Mo1 S1 99.24(11) . . ?
P1 Mo1 S1 80.30(3) . . ?
C13 Mo1 S2 175.16(10) . . ?
C11 Mo1 S2 99.50(12) . . ?
C12 Mo1 S2 88.75(12) . . ?
P1 Mo1 S2 87.02(3) . . ?
S1 Mo1 S2 84.64(3) . . ?
C41 S1 C3 102.29(16) . . ?
C41 S1 Mo1 117.86(13) . . ?
C3 S1 Mo1 111.07(11) . . ?
C21 P1 C1 104.55(16) . . ?
C21 P1 C31 102.05(16) . . ?
C1 P1 C31 103.21(16) . . ?
C21 P1 Mo1 115.51(11) . . ?
C1 P1 Mo1 109.54(12) . . ?
C31 P1 Mo1 120.26(12) . . ?
C51 S2 C4 100.84(17) . . ?
C51 S2 Mo1 118.21(14) . . ?
C4 S2 Mo1 110.89(12) . . ?
C31 C36 C35 120.8(3) . . ?
C31 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
C23 C24 C25 119.8(4) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C34 C35 C36 119.9(4) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C34 C33 C32 120.0(4) . . ?
C34 C33 H33 120.0 . . ?
C32 C33 H33 120.0 . . ?
C33 C32 C31 121.4(4) . . ?
C33 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
C24 C25 C26 120.1(4) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
O3 C13 Mo1 176.7(3) . . ?
C54 C55 C56 120.6(4) . . ?
C54 C55 H55 119.7 . . ?
C56 C55 H55 119.7 . . ?
C51 C52 C53 120.6(4) . . ?
C51 C52 H52 119.7 . . ?
C53 C52 H52 119.7 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C54 C53 C52 119.4(4) . . ?
C54 C53 H53 120.3 . . ?
C52 C53 H53 120.3 . . ?
C42 C41 C46 119.2(4) . . ?
C42 C41 S1 122.6(3) . . ?
C46 C41 S1 117.8(3) . . ?
C35 C34 C33 120.0(4) . . ?
C35 C34 H34 120.0 . . ?
C33 C34 H34 120.0 . . ?
C52 C51 C56 119.7(4) . . ?
C52 C51 S2 121.7(3) . . ?
C56 C51 S2 118.6(3) . . ?
C24 C23 C22 120.6(4) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C2 C3 S1 120.1(2) . . ?
C2 C3 H3A 107.3 . . ?
S1 C3 H3A 107.3 . . ?
C2 C3 H3B 107.3 . . ?
S1 C3 H3B 107.3 . . ?
H3A C3 H3B 106.9 . . ?
C2 C1 P1 116.4(2) . . ?
C2 C1 H1A 108.2 . . ?
P1 C1 H1A 108.2 . . ?
C2 C1 H1B 108.2 . . ?
P1 C1 H1B 108.2 . . ?
H1A C1 H1B 107.3 . . ?
C23 C22 C21 120.3(4) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C41 C46 C45 119.8(4) . . ?
C41 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C26 C21 C22 118.0(3) . . ?
C26 C21 P1 117.3(3) . . ?
C22 C21 P1 124.5(3) . . ?
C4 C2 C3 111.2(3) . . ?
C4 C2 C5 106.4(3) . . ?
C3 C2 C5 105.9(3) . . ?
C4 C2 C1 111.6(3) . . ?
C3 C2 C1 114.0(3) . . ?
C5 C2 C1 107.1(3) . . ?
C55 C56 C51 119.3(4) . . ?
C55 C56 H56 120.3 . . ?
C51 C56 H56 120.3 . . ?
C44 C43 C42 119.9(4) . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C44 C45 C46 120.3(4) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C32 C31 C36 117.9(3) . . ?
C32 C31 P1 120.7(3) . . ?
C36 C31 P1 121.3(3) . . ?
C25 C26 C21 121.2(3) . . ?
C25 C26 H26 119.4 . . ?
C21 C26 H26 119.4 . . ?
O2 C12 Mo1 175.8(3) . . ?
C41 C42 C43 120.3(4) . . ?
C41 C42 H42 119.8 . . ?
C43 C42 H42 119.8 . . ?
C55 C54 C53 120.2(4) . . ?
C55 C54 H54 119.9 . . ?
C53 C54 H54 119.9 . . ?
C2 C4 S2 118.6(3) . . ?
C2 C4 H4A 107.7 . . ?
S2 C4 H4A 107.7 . . ?
C2 C4 H4B 107.7 . . ?
S2 C4 H4B 107.7 . . ?
H4A C4 H4B 107.1 . . ?
C45 C44 C43 120.4(4) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
O1 C11 Mo1 174.4(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
C31 C36 C35 C34 1.7(5) . . . . ?
C34 C33 C32 C31 1.2(6) . . . . ?
C23 C24 C25 C26 1.1(6) . . . . ?
C51 C52 C53 C54 -0.1(6) . . . . ?
C3 S1 C41 C42 108.8(3) . . . . ?
Mo1 S1 C41 C42 -13.3(4) . . . . ?
C3 S1 C41 C46 -77.7(3) . . . . ?
Mo1 S1 C41 C46 160.2(2) . . . . ?
C36 C35 C34 C33 -1.3(5) . . . . ?
C32 C33 C34 C35 -0.2(5) . . . . ?
C53 C52 C51 C56 2.6(6) . . . . ?
C53 C52 C51 S2 -179.0(3) . . . . ?
C4 S2 C51 C52 118.1(3) . . . . ?
Mo1 S2 C51 C52 -2.9(4) . . . . ?
C4 S2 C51 C56 -63.5(3) . . . . ?
Mo1 S2 C51 C56 175.6(2) . . . . ?
C25 C24 C23 C22 -0.2(6) . . . . ?
C41 S1 C3 C2 -103.0(3) . . . . ?
Mo1 S1 C3 C2 23.7(3) . . . . ?
C21 P1 C1 C2 166.4(3) . . . . ?
C31 P1 C1 C2 -87.2(3) . . . . ?
Mo1 P1 C1 C2 42.1(3) . . . . ?
C24 C23 C22 C21 -0.6(6) . . . . ?
C42 C41 C46 C45 -1.9(6) . . . . ?
S1 C41 C46 C45 -175.6(3) . . . . ?
C23 C22 C21 C26 0.6(5) . . . . ?
C23 C22 C21 P1 -174.5(3) . . . . ?
C1 P1 C21 C26 178.4(3) . . . . ?
C31 P1 C21 C26 71.2(3) . . . . ?
Mo1 P1 C21 C26 -61.1(3) . . . . ?
C1 P1 C21 C22 -6.4(4) . . . . ?
C31 P1 C21 C22 -113.7(3) . . . . ?
Mo1 P1 C21 C22 114.0(3) . . . . ?
S1 C3 C2 C4 50.7(4) . . . . ?
S1 C3 C2 C5 165.9(3) . . . . ?
S1 C3 C2 C1 -76.5(4) . . . . ?
P1 C1 C2 C4 -91.4(3) . . . . ?
P1 C1 C2 C3 35.6(4) . . . . ?
P1 C1 C2 C5 152.5(2) . . . . ?
C54 C55 C56 C51 0.9(6) . . . . ?
C52 C51 C56 C55 -3.0(6) . . . . ?
S2 C51 C56 C55 178.6(3) . . . . ?
C41 C46 C45 C44 1.4(6) . . . . ?
C33 C32 C31 C36 -0.7(5) . . . . ?
C33 C32 C31 P1 177.5(3) . . . . ?
C35 C36 C31 C32 -0.8(5) . . . . ?
C35 C36 C31 P1 -178.9(3) . . . . ?
C21 P1 C31 C32 -109.5(3) . . . . ?
C1 P1 C31 C32 142.2(3) . . . . ?
Mo1 P1 C31 C32 19.9(3) . . . . ?
C21 P1 C31 C36 68.6(3) . . . . ?
C1 P1 C31 C36 -39.7(3) . . . . ?
Mo1 P1 C31 C36 -162.0(2) . . . . ?
C24 C25 C26 C21 -1.1(6) . . . . ?
C22 C21 C26 C25 0.3(5) . . . . ?
P1 C21 C26 C25 175.7(3) . . . . ?
C46 C41 C42 C43 1.1(6) . . . . ?
S1 C41 C42 C43 174.5(3) . . . . ?
C44 C43 C42 C41 0.4(6) . . . . ?
C56 C55 C54 C53 1.6(6) . . . . ?
C52 C53 C54 C55 -2.0(6) . . . . ?
C3 C2 C4 S2 -83.9(3) . . . . ?
C5 C2 C4 S2 161.2(2) . . . . ?
C1 C2 C4 S2 44.7(4) . . . . ?
C51 S2 C4 C2 -97.9(3) . . . . ?
Mo1 S2 C4 C2 28.2(3) . . . . ?
C46 C45 C44 C43 0.1(7) . . . . ?
C42 C43 C44 C45 -1.0(6) . . . . ?

_refine_diff_density_max         0.709
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.098




_publcif_funding_html            
;
;
####################################################################### 
# 
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 1545164'

_audit_update_record             
;
2017-07-05 deposited with the CCDC.
2017-07-10 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         '2(C26 H24 Mo O3 S3), C4 H8 O'
_chemical_formula_sum            'C56 H56 Mo2 O7 S6'
_chemical_formula_weight         1225.24

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'
Mo Mo -0.0483 2.7339 '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'
S S 0.3331 0.5567 '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                   9.9426(4)
_cell_length_b                   10.0256(4)
_cell_length_c                   15.2661(6)
_cell_angle_alpha                73.959(3)
_cell_angle_beta                 73.188(3)
_cell_angle_gamma                74.464(3)
_cell_volume                     1370.46(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(10)
_cell_measurement_reflns_used    8163
_cell_measurement_theta_min      4.6600
_cell_measurement_theta_max      75.7820

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_F_000             628
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    6.291
_exptl_absorpt_correction_T_min  0.57451
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_reflns_number            14246
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.688
_diffrn_reflns_theta_max         76.398
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             5540
_reflns_number_gt                5241
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    
;
Olex2, OlexSys Ltd,
Version 1.2
(compiled Mar  28 2017)
;
_computing_publication_material  
;
publCIF, IUCr,
Version 1.9.20_c
;
_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)+(0.0520P)²+2.5992P] 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         5540
_refine_ls_number_parameters     311
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0922
_refine_ls_wR_factor_gt          0.0901
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
Mo01 Mo 0.28544(2) 0.61378(2) 0.19860(2) 0.01509(8) Uani 1 1 d . . . . .
S002 S 0.15994(6) 0.53373(7) 0.10296(4) 0.01729(13) Uani 1 1 d . . . . .
O2 O 0.3439(10) 0.0199(10) 0.4806(6) 0.084(2) Uiso 0.5 1 d . . P . .
S003 S 0.48242(6) 0.42238(7) 0.12760(4) 0.01709(13) Uani 1 1 d . . . . .
S004 S 0.21680(7) 0.40817(7) 0.33330(4) 0.01824(14) Uani 1 1 d . . . . .
O005 O 0.3738(2) 0.8651(2) 0.03820(14) 0.0239(4) Uani 1 1 d . . . . .
C1A C 0.4946(7) -0.0317(7) 0.4388(5) 0.0820(17) Uiso 1 1 d . . . . .
H1AA H 0.492094 -0.098313 0.404078 0.098 Uiso 1 1 calc R U . . .
H1BA H 0.523575 0.049352 0.391902 0.098 Uiso 1 1 calc R U . . .
C5A C 0.6138(13) -0.0954(12) 0.4784(9) 0.159(4) Uiso 1 1 d . . . . .
H5A H 0.592313 -0.180287 0.524284 0.191 Uiso 1 1 calc R U . . .
H6A H 0.694074 -0.125542 0.429290 0.191 Uiso 1 1 calc R U . . .
O006 O 0.0413(2) 0.8494(2) 0.27698(16) 0.0268(4) Uani 1 1 d . . . . .
O007 O 0.4598(2) 0.7049(3) 0.30400(16) 0.0309(5) Uani 1 1 d . . . . .
C008 C 0.3974(3) 0.6668(3) 0.26549(19) 0.0210(5) Uani 1 1 d . . . . .
C009 C 0.0284(3) 0.4220(3) 0.38690(19) 0.0203(5) Uani 1 1 d . . . . .
C00A C -0.1326(3) 0.5753(3) 0.1101(2) 0.0209(5) Uani 1 1 d . . . . .
H00A H -0.122734 0.477354 0.123478 0.025 Uiso 1 1 calc R U . . .
C00B C -0.0304(3) 0.7829(3) 0.0758(2) 0.0223(6) Uani 1 1 d . . . . .
H00B H 0.047937 0.822838 0.067365 0.027 Uiso 1 1 calc R U . . .
C00C C -0.2810(3) 0.8102(3) 0.0814(2) 0.0236(6) Uani 1 1 d . . . . .
H00C H -0.369961 0.868187 0.076520 0.028 Uiso 1 1 calc R U . . .
C00D C 0.1288(3) 0.7598(3) 0.24787(19) 0.0202(5) Uani 1 1 d . . . . .
C00E C -0.0152(3) 0.6355(3) 0.09695(18) 0.0177(5) Uani 1 1 d . . . . .
C00F C 0.6131(3) 0.3209(3) 0.19350(19) 0.0191(5) Uani 1 1 d . . . . .
C00G C 0.3433(3) 0.7686(3) 0.09569(19) 0.0182(5) Uani 1 1 d . . . . .
C00H C -0.2648(3) 0.6642(3) 0.1028(2) 0.0237(6) Uani 1 1 d . . . . .
H00H H -0.343956 0.624640 0.112496 0.028 Uiso 1 1 calc R U . . .
C00I C 0.1294(3) 0.3543(3) 0.1566(2) 0.0196(5) Uani 1 1 d . . . . .
H00D H 0.048799 0.357553 0.210550 0.024 Uiso 1 1 calc R U . . .
H00E H 0.104320 0.318086 0.111968 0.024 Uiso 1 1 calc R U . . .
C00J C -0.1631(3) 0.8694(3) 0.0673(2) 0.0253(6) Uani 1 1 d . . . . .
H00J H -0.172927 0.967460 0.052180 0.030 Uiso 1 1 calc R U . . .
C00K C 0.2620(3) 0.2518(3) 0.1879(2) 0.0200(5) Uani 1 1 d . . . . .
C00L C -0.0751(3) 0.5277(3) 0.3491(2) 0.0232(6) Uani 1 1 d . . . . .
H00L H -0.048470 0.590567 0.292773 0.028 Uiso 1 1 calc R U . . .
C00M C 0.4038(3) 0.2812(3) 0.1192(2) 0.0205(5) Uani 1 1 d . . . . .
H00F H 0.389190 0.302585 0.056219 0.025 Uiso 1 1 calc R U . . .
H00G H 0.475035 0.193642 0.125709 0.025 Uiso 1 1 calc R U . . .
C00N C 0.6028(3) 0.3324(3) 0.2838(2) 0.0242(6) Uani 1 1 d . . . . .
H00N H 0.525610 0.393468 0.313099 0.029 Uiso 1 1 calc R U . . .
C00O C -0.0106(3) 0.3277(3) 0.4709(2) 0.0254(6) Uani 1 1 d . . . . .
H00O H 0.059029 0.257846 0.496242 0.030 Uiso 1 1 calc R U . . .
C00P C 0.7303(3) 0.2329(3) 0.1485(2) 0.0263(6) Uani 1 1 d . . . . .
H00P H 0.738562 0.228491 0.087055 0.032 Uiso 1 1 calc R U . . .
C00Q C 0.2609(3) 0.2446(3) 0.2900(2) 0.0211(5) Uani 1 1 d . . . . .
H00I H 0.355294 0.194581 0.299733 0.025 Uiso 1 1 calc R U . . .
H00K H 0.193570 0.186025 0.329884 0.025 Uiso 1 1 calc R U . . .
C00R C -0.2188(3) 0.5386(4) 0.3962(2) 0.0291(6) Uani 1 1 d . . . . .
H00R H -0.288487 0.608812 0.371183 0.035 Uiso 1 1 calc R U . . .
C00S C -0.1549(4) 0.3387(4) 0.5171(2) 0.0297(7) Uani 1 1 d . . . . .
H00S H -0.182077 0.274442 0.572588 0.036 Uiso 1 1 calc R U . . .
C00T C 0.2540(3) 0.1015(3) 0.1843(2) 0.0262(6) Uani 1 1 d . . . . .
H00M H 0.268917 0.096026 0.120285 0.039 Uiso 1 1 calc R U . . .
H00Q H 0.161309 0.082466 0.218756 0.039 Uiso 1 1 calc R U . . .
H00T H 0.326916 0.032868 0.211582 0.039 Uiso 1 1 calc R U . . .
C00U C 0.7099(4) 0.2512(3) 0.3301(2) 0.0289(6) Uani 1 1 d . . . . .
H00U H 0.704254 0.258738 0.390493 0.035 Uiso 1 1 calc R U . . .
C00V C 0.8245(4) 0.1596(3) 0.2868(2) 0.0313(7) Uani 1 1 d . . . . .
H00V H 0.894035 0.103714 0.318616 0.038 Uiso 1 1 calc R U . . .
C00W C 0.8351(4) 0.1514(4) 0.1958(3) 0.0328(7) Uani 1 1 d . . . . .
H00W H 0.912761 0.091087 0.166282 0.039 Uiso 1 1 calc R U . . .
C00X C -0.2583(3) 0.4453(4) 0.4803(2) 0.0311(7) Uani 1 1 d . . . . .
H00X H -0.354268 0.454054 0.512239 0.037 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
Mo01 C00G 1.954(3) . ?
Mo01 C008 1.959(3) . ?
Mo01 C00D 1.961(3) . ?
Mo01 S004 2.5579(7) . ?
Mo01 S002 2.5634(6) . ?
Mo01 S003 2.5692(7) . ?
S002 C00E 1.781(3) . ?
S002 C00I 1.826(3) . ?
O2 C5A 1.313(13) 2_656 ?
O2 C1A 1.461(11) . ?
S003 C00F 1.794(3) . ?
S003 C00M 1.839(3) . ?
S004 C009 1.798(3) . ?
S004 C00Q 1.834(3) . ?
O005 C00G 1.154(3) . ?
C1A C5A 1.404(12) . ?
C1A C5A 1.936(13) 2_656 ?
C1A H1AA 0.9700 . ?
C1A H1BA 0.9700 . ?
C5A H5A 0.9700 . ?
C5A H6A 0.9700 . ?
O006 C00D 1.157(4) . ?
O007 C008 1.157(4) . ?
C009 C00O 1.388(4) . ?
C009 C00L 1.392(4) . ?
C00A C00H 1.392(4) . ?
C00A C00E 1.393(4) . ?
C00A H00A 0.9300 . ?
C00B C00J 1.390(4) . ?
C00B C00E 1.398(4) . ?
C00B H00B 0.9300 . ?
C00C C00H 1.385(4) . ?
C00C C00J 1.389(4) . ?
C00C H00C 0.9300 . ?
C00F C00N 1.387(4) . ?
C00F C00P 1.390(4) . ?
C00H H00H 0.9300 . ?
C00I C00K 1.546(4) . ?
C00I H00D 0.9700 . ?
C00I H00E 0.9700 . ?
C00J H00J 0.9300 . ?
C00K C00Q 1.538(4) . ?
C00K C00M 1.540(4) . ?
C00K C00T 1.547(4) . ?
C00L C00R 1.391(4) . ?
C00L H00L 0.9300 . ?
C00M H00F 0.9700 . ?
C00M H00G 0.9700 . ?
C00N C00U 1.396(4) . ?
C00N H00N 0.9300 . ?
C00O C00S 1.393(4) . ?
C00O H00O 0.9300 . ?
C00P C00W 1.388(4) . ?
C00P H00P 0.9300 . ?
C00Q H00I 0.9700 . ?
C00Q H00K 0.9700 . ?
C00R C00X 1.386(5) . ?
C00R H00R 0.9300 . ?
C00S C00X 1.388(5) . ?
C00S H00S 0.9300 . ?
C00T H00M 0.9600 . ?
C00T H00Q 0.9600 . ?
C00T H00T 0.9600 . ?
C00U C00V 1.385(5) . ?
C00U H00U 0.9300 . ?
C00V C00W 1.386(5) . ?
C00V H00V 0.9300 . ?
C00W H00W 0.9300 . ?
C00X H00X 0.9300 . ?

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
C00G Mo01 C008 85.86(11) . . ?
C00G Mo01 C00D 85.59(11) . . ?
C008 Mo01 C00D 85.02(11) . . ?
C00G Mo01 S004 178.47(8) . . ?
C008 Mo01 S004 93.27(8) . . ?
C00D Mo01 S004 95.58(8) . . ?
C00G Mo01 S002 93.04(8) . . ?
C008 Mo01 S002 174.97(8) . . ?
C00D Mo01 S002 99.81(8) . . ?
S004 Mo01 S002 87.72(2) . . ?
C00G Mo01 S003 93.81(8) . . ?
C008 Mo01 S003 98.12(8) . . ?
C00D Mo01 S003 176.76(8) . . ?
S004 Mo01 S003 85.06(2) . . ?
S002 Mo01 S003 77.03(2) . . ?
C00E S002 C00I 103.39(12) . . ?
C00E S002 Mo01 114.58(9) . . ?
C00I S002 Mo01 110.92(9) . . ?
C5A O2 C1A 88.3(8) 2_656 . ?
C00F S003 C00M 100.80(13) . . ?
C00F S003 Mo01 117.64(10) . . ?
C00M S003 Mo01 110.43(9) . . ?
C009 S004 C00Q 101.98(13) . . ?
C009 S004 Mo01 116.07(9) . . ?
C00Q S004 Mo01 110.15(9) . . ?
C5A C1A O2 131.9(8) . . ?
C5A C1A C5A 100.7(7) . 2_656 ?
O2 C1A C5A 42.7(5) . 2_656 ?
C5A C1A H1AA 104.3 . . ?
O2 C1A H1AA 104.3 . . ?
C5A C1A H1AA 146.9 2_656 . ?
C5A C1A H1BA 104.3 . . ?
O2 C1A H1BA 104.3 . . ?
C5A C1A H1BA 88.7 2_656 . ?
H1AA C1A H1BA 105.6 . . ?
O2 C5A C1A 118.0(10) 2_656 . ?
O2 C5A C1A 49.0(6) 2_656 2_656 ?
C1A C5A C1A 79.3(7) . 2_656 ?
O2 C5A H5A 107.8 2_656 . ?
C1A C5A H5A 107.8 . . ?
C1A C5A H5A 94.4 2_656 . ?
O2 C5A H6A 107.8 2_656 . ?
C1A C5A H6A 107.8 . . ?
C1A C5A H6A 153.3 2_656 . ?
H5A C5A H6A 107.2 . . ?
O007 C008 Mo01 176.6(3) . . ?
C00O C009 C00L 120.6(3) . . ?
C00O C009 S004 117.5(2) . . ?
C00L C009 S004 121.8(2) . . ?
C00H C00A C00E 118.9(3) . . ?
C00H C00A H00A 120.5 . . ?
C00E C00A H00A 120.5 . . ?
C00J C00B C00E 119.8(2) . . ?
C00J C00B H00B 120.1 . . ?
C00E C00B H00B 120.1 . . ?
C00H C00C C00J 119.4(3) . . ?
C00H C00C H00C 120.3 . . ?
C00J C00C H00C 120.3 . . ?
O006 C00D Mo01 176.7(2) . . ?
C00A C00E C00B 120.2(2) . . ?
C00A C00E S002 123.3(2) . . ?
C00B C00E S002 116.4(2) . . ?
C00N C00F C00P 120.6(3) . . ?
C00N C00F S003 122.5(2) . . ?
C00P C00F S003 116.8(2) . . ?
O005 C00G Mo01 176.2(2) . . ?
C00C C00H C00A 121.3(3) . . ?
C00C C00H H00H 119.3 . . ?
C00A C00H H00H 119.3 . . ?
C00K C00I S002 112.65(18) . . ?
C00K C00I H00D 109.1 . . ?
S002 C00I H00D 109.1 . . ?
C00K C00I H00E 109.1 . . ?
S002 C00I H00E 109.1 . . ?
H00D C00I H00E 107.8 . . ?
C00C C00J C00B 120.3(3) . . ?
C00C C00J H00J 119.8 . . ?
C00B C00J H00J 119.8 . . ?
C00Q C00K C00M 112.7(2) . . ?
C00Q C00K C00I 112.9(2) . . ?
C00M C00K C00I 112.3(2) . . ?
C00Q C00K C00T 106.0(2) . . ?
C00M C00K C00T 105.5(2) . . ?
C00I C00K C00T 106.8(2) . . ?
C00R C00L C009 119.5(3) . . ?
C00R C00L H00L 120.3 . . ?
C009 C00L H00L 120.3 . . ?
C00K C00M S003 119.49(19) . . ?
C00K C00M H00F 107.4 . . ?
S003 C00M H00F 107.4 . . ?
C00K C00M H00G 107.4 . . ?
S003 C00M H00G 107.4 . . ?
H00F C00M H00G 107.0 . . ?
C00F C00N C00U 119.2(3) . . ?
C00F C00N H00N 120.4 . . ?
C00U C00N H00N 120.4 . . ?
C009 C00O C00S 119.5(3) . . ?
C009 C00O H00O 120.3 . . ?
C00S C00O H00O 120.3 . . ?
C00W C00P C00F 119.6(3) . . ?
C00W C00P H00P 120.2 . . ?
C00F C00P H00P 120.2 . . ?
C00K C00Q S004 120.06(19) . . ?
C00K C00Q H00I 107.3 . . ?
S004 C00Q H00I 107.3 . . ?
C00K C00Q H00K 107.3 . . ?
S004 C00Q H00K 107.3 . . ?
H00I C00Q H00K 106.9 . . ?
C00X C00R C00L 120.2(3) . . ?
C00X C00R H00R 119.9 . . ?
C00L C00R H00R 119.9 . . ?
C00X C00S C00O 120.1(3) . . ?
C00X C00S H00S 119.9 . . ?
C00O C00S H00S 119.9 . . ?
C00K C00T H00M 109.5 . . ?
C00K C00T H00Q 109.5 . . ?
H00M C00T H00Q 109.5 . . ?
C00K C00T H00T 109.5 . . ?
H00M C00T H00T 109.5 . . ?
H00Q C00T H00T 109.5 . . ?
C00V C00U C00N 120.5(3) . . ?
C00V C00U H00U 119.8 . . ?
C00N C00U H00U 119.8 . . ?
C00U C00V C00W 119.8(3) . . ?
C00U C00V H00V 120.1 . . ?
C00W C00V H00V 120.1 . . ?
C00V C00W C00P 120.4(3) . . ?
C00V C00W H00W 119.8 . . ?
C00P C00W H00W 119.8 . . ?
C00R C00X C00S 120.1(3) . . ?
C00R C00X H00X 119.9 . . ?
C00S C00X H00X 119.9 . . ?

_refine_diff_density_max         1.495
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.097




_publcif_funding_html            
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