# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1580360'
_audit_update_record             
;
2017-10-19 deposited with the CCDC.
2017-11-27 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         'C16 H19 Mo N2 O7, C24 H20 P'
_chemical_formula_sum            'C40 H39 Mo N2 O7 P'
_chemical_formula_weight         786.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5112(6)
_cell_length_b                   13.1936(7)
_cell_length_c                   13.8181(8)
_cell_angle_alpha                89.653(2)
_cell_angle_beta                 87.507(2)
_cell_angle_gamma                71.931(2)
_cell_volume                     1820.02(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    7211
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      30.53

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_F_000             812
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.457
_shelx_estimated_absorpt_T_min   0.804
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   
;
program SADABS, Bruker (2001).
;
_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            30917
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.475
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             6498
_reflns_number_gt                6106
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0417P)²+0.9729P] 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         6498
_refine_ls_number_parameters     464
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0743
_refine_ls_wR_factor_gt          0.0730
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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 1.09013(2) 0.20104(2) 0.25829(2) 0.02378(7) Uani 1 1 d . . . . .
O1 O 0.96550(13) 0.10708(11) 0.24350(9) 0.0294(3) Uani 1 1 d . . . . .
O2 O 1.08385(13) 0.19822(11) 0.09375(9) 0.0306(3) Uani 1 1 d . . . . .
O3 O 1.07920(15) 0.18651(13) 0.37934(9) 0.0379(3) Uani 1 1 d . . . . .
O4 O 0.93578(15) 0.32643(13) 0.23880(13) 0.0464(4) Uani 1 1 d . . . . .
O5 O 1.06280(16) 0.35101(12) 0.24498(12) 0.0441(4) Uani 1 1 d . . . . .
O6 O 1.27836(13) 0.17866(11) 0.23451(10) 0.0343(3) Uani 1 1 d . . . . .
O7 O 1.24610(14) 0.07838(11) 0.22604(11) 0.0363(3) Uani 1 1 d . . . . .
N1 N 0.74305(15) 0.05045(12) 0.08633(11) 0.0265(3) Uani 1 1 d . . . . .
N2 N 0.80098(15) 0.05111(12) 0.17542(10) 0.0242(3) Uani 1 1 d . . . . .
C1 C 0.90008(17) 0.09723(14) 0.16861(12) 0.0229(3) Uani 1 1 d . . . . .
C2 C 0.90996(18) 0.12639(14) 0.07115(12) 0.0232(4) Uani 1 1 d . . . . .
C3 C 0.80911(18) 0.09400(14) 0.02474(12) 0.0241(4) Uani 1 1 d . . . . .
C4 C 1.00730(18) 0.17508(14) 0.03704(12) 0.0245(4) Uani 1 1 d . . . . .
C5 C 1.02142(19) 0.19985(15) -0.06842(13) 0.0272(4) Uani 1 1 d . . . . .
H5A H 0.972595 0.161489 -0.106229 0.033 Uiso 1 1 calc R U . . .
H5B H 1.117271 0.172377 -0.089453 0.033 Uiso 1 1 calc R U . . .
C6 C 0.96814(19) 0.32053(16) -0.09256(14) 0.0317(4) Uani 1 1 d . . . . .
C7 C 1.0690(2) 0.37667(17) -0.06670(18) 0.0436(5) Uani 1 1 d . . . . .
H7A H 1.154451 0.343052 -0.102095 0.065 Uiso 1 1 calc R U . . .
H7B H 1.082366 0.371045 0.003114 0.065 Uiso 1 1 calc R U . . .
H7C H 1.034935 0.452001 -0.084484 0.065 Uiso 1 1 calc R U . . .
C8 C 0.8335(2) 0.37490(18) -0.03887(17) 0.0415(5) Uani 1 1 d . . . . .
H8A H 0.845761 0.371747 0.031108 0.062 Uiso 1 1 calc R U . . .
H8B H 0.768996 0.338146 -0.054584 0.062 Uiso 1 1 calc R U . . .
H8C H 0.799798 0.449548 -0.058840 0.062 Uiso 1 1 calc R U . . .
C9 C 0.9508(2) 0.3274(2) -0.20205(16) 0.0461(6) Uani 1 1 d . . . . .
H9A H 0.919511 0.402467 -0.221200 0.069 Uiso 1 1 calc R U . . .
H9B H 0.884970 0.292546 -0.219175 0.069 Uiso 1 1 calc R U . . .
H9C H 1.036895 0.291751 -0.235878 0.069 Uiso 1 1 calc R U . . .
C10 C 0.7701(2) 0.10046(16) -0.07868(13) 0.0311(4) Uani 1 1 d . . . . .
H10A H 0.696629 0.070221 -0.084933 0.047 Uiso 1 1 calc R U . . .
H10B H 0.847224 0.060192 -0.119907 0.047 Uiso 1 1 calc R U . . .
H10C H 0.740923 0.175201 -0.098827 0.047 Uiso 1 1 calc R U . . .
C11 C 0.74631(18) 0.01215(14) 0.25809(13) 0.0248(4) Uani 1 1 d . . . . .
C12 C 0.8295(2) -0.04215(16) 0.32978(14) 0.0340(4) Uani 1 1 d . . . . .
H12 H 0.923340 -0.053744 0.324012 0.041 Uiso 1 1 calc R U . . .
C13 C 0.7735(2) -0.07892(18) 0.40945(16) 0.0409(5) Uani 1 1 d . . . . .
H13 H 0.829419 -0.116891 0.458417 0.049 Uiso 1 1 calc R U . . .
C14 C 0.6365(2) -0.06096(17) 0.41859(15) 0.0393(5) Uani 1 1 d . . . . .
H14 H 0.598707 -0.085157 0.474331 0.047 Uiso 1 1 calc R U . . .
C15 C 0.5548(2) -0.00778(16) 0.34657(15) 0.0353(4) Uani 1 1 d . . . . .
H15 H 0.460909 0.004245 0.352859 0.042 Uiso 1 1 calc R U . . .
C16 C 0.60920(19) 0.02787(14) 0.26560(14) 0.0286(4) Uani 1 1 d . . . . .
H16 H 0.553380 0.062880 0.215384 0.034 Uiso 1 1 calc R U . . .
P1 P 0.52314(4) 0.63711(3) 0.30179(3) 0.02168(10) Uani 1 1 d . . . . .
C17 C 0.55093(18) 0.68911(14) 0.18501(12) 0.0244(4) Uani 1 1 d . . . . .
C18 C 0.58842(19) 0.78197(15) 0.17953(13) 0.0282(4) Uani 1 1 d . . . . .
H18 H 0.603500 0.814956 0.236969 0.034 Uiso 1 1 calc R U . . .
C19 C 0.60350(19) 0.82571(16) 0.08964(15) 0.0332(4) Uani 1 1 d . . . . .
H19 H 0.626138 0.890000 0.085685 0.040 Uiso 1 1 calc R U . . .
C20 C 0.5856(2) 0.77570(18) 0.00592(15) 0.0394(5) Uani 1 1 d . . . . .
H20 H 0.597367 0.805025 -0.055524 0.047 Uiso 1 1 calc R U . . .
C21 C 0.5505(2) 0.68306(19) 0.01163(15) 0.0435(5) Uani 1 1 d . . . . .
H21 H 0.538636 0.649000 -0.046149 0.052 Uiso 1 1 calc R U . . .
C22 C 0.5323(2) 0.63942(16) 0.10036(14) 0.0334(4) Uani 1 1 d . . . . .
H22 H 0.507446 0.576103 0.103652 0.040 Uiso 1 1 calc R U . . .
C23 C 0.51020(18) 0.50562(14) 0.28743(12) 0.0243(4) Uani 1 1 d . . . . .
C24 C 0.3883(2) 0.49565(16) 0.26012(15) 0.0328(4) Uani 1 1 d . . . . .
H24 H 0.313959 0.557623 0.251831 0.039 Uiso 1 1 calc R U . . .
C25 C 0.3755(2) 0.39595(17) 0.24512(15) 0.0372(5) Uani 1 1 d . . . . .
H25 H 0.292473 0.389124 0.226645 0.045 Uiso 1 1 calc R U . . .
C26 C 0.4840(2) 0.30630(17) 0.25715(16) 0.0405(5) Uani 1 1 d . . . . .
H26 H 0.475251 0.237642 0.247060 0.049 Uiso 1 1 calc R U . . .
C27 C 0.6052(2) 0.31550(17) 0.28375(17) 0.0425(5) Uani 1 1 d . . . . .
H27 H 0.679154 0.253173 0.291837 0.051 Uiso 1 1 calc R U . . .
C28 C 0.6196(2) 0.41503(15) 0.29867(15) 0.0333(4) Uani 1 1 d . . . . .
H28 H 0.703123 0.421364 0.316375 0.040 Uiso 1 1 calc R U . . .
C29 C 0.65919(18) 0.63442(14) 0.37707(13) 0.0246(4) Uani 1 1 d . . . . .
C30 C 0.79056(19) 0.58798(16) 0.34137(14) 0.0308(4) Uani 1 1 d . . . . .
H30 H 0.807826 0.559004 0.277604 0.037 Uiso 1 1 calc R U . . .
C31 C 0.8957(2) 0.58450(17) 0.39984(15) 0.0364(5) Uani 1 1 d . . . . .
H31 H 0.985436 0.551570 0.376581 0.044 Uiso 1 1 calc R U . . .
C32 C 0.8706(2) 0.62877(17) 0.49183(15) 0.0381(5) Uani 1 1 d . . . . .
H32 H 0.943215 0.627367 0.530920 0.046 Uiso 1 1 calc R U . . .
C33 C 0.7408(2) 0.67495(18) 0.52731(15) 0.0380(5) Uani 1 1 d . . . . .
H33 H 0.724374 0.705025 0.590674 0.046 Uiso 1 1 calc R U . . .
C34 C 0.6339(2) 0.67753(16) 0.47046(14) 0.0316(4) Uani 1 1 d . . . . .
H34 H 0.544423 0.708406 0.495030 0.038 Uiso 1 1 calc R U . . .
C35 C 0.36986(18) 0.71915(14) 0.36050(13) 0.0248(4) Uani 1 1 d . . . . .
C36 C 0.3116(2) 0.67591(16) 0.43626(14) 0.0331(4) Uani 1 1 d . . . . .
H36 H 0.347677 0.602582 0.451754 0.040 Uiso 1 1 calc R U . . .
C37 C 0.2013(2) 0.74022(18) 0.48868(15) 0.0385(5) Uani 1 1 d . . . . .
H37 H 0.161595 0.711136 0.540395 0.046 Uiso 1 1 calc R U . . .
C38 C 0.1488(2) 0.84698(17) 0.46576(16) 0.0395(5) Uani 1 1 d . . . . .
H38 H 0.073406 0.891023 0.502189 0.047 Uiso 1 1 calc R U . . .
C39 C 0.2053(2) 0.88996(16) 0.39027(16) 0.0381(5) Uani 1 1 d . . . . .
H39 H 0.168617 0.963296 0.375041 0.046 Uiso 1 1 calc R U . . .
C40 C 0.31577(19) 0.82617(15) 0.33655(13) 0.0283(4) Uani 1 1 d . . . . .
H40 H 0.353938 0.855310 0.284023 0.034 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 O3 1.6856(13) . ?
Mo1 O5 1.9181(15) . ?
Mo1 O6 1.9214(13) . ?
Mo1 O7 1.9506(14) . ?
Mo1 O4 1.9517(15) . ?
Mo1 O1 2.0806(12) . ?
Mo1 O2 2.2783(13) . ?
O1 C1 1.296(2) . ?
O2 C4 1.251(2) . ?
O4 O5 1.474(2) . ?
O6 O7 1.4707(19) . ?
N1 C3 1.314(2) . ?
N1 N2 1.398(2) . ?
N2 C1 1.359(2) . ?
N2 C11 1.421(2) . ?
C1 C2 1.407(2) . ?
C2 C4 1.430(3) . ?
C2 C3 1.436(2) . ?
C3 C10 1.498(2) . ?
C4 C5 1.503(2) . ?
C5 C6 1.555(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.524(3) . ?
C6 C9 1.530(3) . ?
C6 C8 1.534(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C16 1.390(3) . ?
C11 C12 1.392(3) . ?
C12 C13 1.381(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.380(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
P1 C23 1.7945(18) . ?
P1 C29 1.7961(18) . ?
P1 C17 1.7972(18) . ?
P1 C35 1.8002(18) . ?
C17 C22 1.395(3) . ?
C17 C18 1.399(3) . ?
C18 C19 1.390(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.384(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.383(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.382(3) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C28 1.391(3) . ?
C23 C24 1.396(3) . ?
C24 C25 1.381(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.380(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.383(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.385(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.395(3) . ?
C29 C30 1.395(3) . ?
C30 C31 1.387(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.382(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.379(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.390(3) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C40 1.393(3) . ?
C35 C36 1.396(3) . ?
C36 C37 1.383(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.384(3) . ?
C37 H37 0.9500 . ?
C38 C39 1.382(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.390(3) . ?
C39 H39 0.9500 . ?
C40 H40 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
O3 Mo1 O5 102.64(7) . . ?
O3 Mo1 O6 102.21(6) . . ?
O5 Mo1 O6 87.93(6) . . ?
O3 Mo1 O7 99.77(7) . . ?
O5 Mo1 O7 130.95(6) . . ?
O6 Mo1 O7 44.64(6) . . ?
O3 Mo1 O4 101.27(7) . . ?
O5 Mo1 O4 44.78(7) . . ?
O6 Mo1 O4 130.77(6) . . ?
O7 Mo1 O4 158.88(7) . . ?
O3 Mo1 O1 88.99(6) . . ?
O5 Mo1 O1 132.98(6) . . ?
O6 Mo1 O1 134.37(6) . . ?
O7 Mo1 O1 90.10(6) . . ?
O4 Mo1 O1 88.43(6) . . ?
O3 Mo1 O2 169.37(6) . . ?
O5 Mo1 O2 85.70(6) . . ?
O6 Mo1 O2 84.49(5) . . ?
O7 Mo1 O2 79.09(6) . . ?
O4 Mo1 O2 79.88(6) . . ?
O1 Mo1 O2 80.46(5) . . ?
C1 O1 Mo1 128.10(11) . . ?
C4 O2 Mo1 133.12(12) . . ?
O5 O4 Mo1 66.40(8) . . ?
O4 O5 Mo1 68.82(8) . . ?
O7 O6 Mo1 68.73(8) . . ?
O6 O7 Mo1 66.63(8) . . ?
C3 N1 N2 105.49(14) . . ?
C1 N2 N1 111.58(14) . . ?
C1 N2 C11 129.75(14) . . ?
N1 N2 C11 118.53(14) . . ?
O1 C1 N2 121.38(16) . . ?
O1 C1 C2 132.01(16) . . ?
N2 C1 C2 106.61(15) . . ?
C1 C2 C4 121.90(16) . . ?
C1 C2 C3 104.63(15) . . ?
C4 C2 C3 133.46(16) . . ?
N1 C3 C2 111.68(15) . . ?
N1 C3 C10 116.94(16) . . ?
C2 C3 C10 131.37(17) . . ?
O2 C4 C2 121.25(16) . . ?
O2 C4 C5 117.71(16) . . ?
C2 C4 C5 121.04(15) . . ?
C4 C5 C6 114.22(15) . . ?
C4 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
C4 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C7 C6 C9 108.94(18) . . ?
C7 C6 C8 109.37(18) . . ?
C9 C6 C8 109.89(17) . . ?
C7 C6 C5 110.74(16) . . ?
C9 C6 C5 106.38(17) . . ?
C8 C6 C5 111.45(16) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C3 C10 H10A 109.5 . . ?
C3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C16 C11 C12 120.67(17) . . ?
C16 C11 N2 119.08(16) . . ?
C12 C11 N2 120.25(17) . . ?
C13 C12 C11 118.97(19) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 120.6(2) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C15 C14 C13 120.00(19) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 C14 120.23(19) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C11 119.48(18) . . ?
C15 C16 H16 120.3 . . ?
C11 C16 H16 120.3 . . ?
C23 P1 C29 110.66(8) . . ?
C23 P1 C17 109.43(8) . . ?
C29 P1 C17 109.30(8) . . ?
C23 P1 C35 108.02(9) . . ?
C29 P1 C35 108.32(8) . . ?
C17 P1 C35 111.12(8) . . ?
C22 C17 C18 119.93(17) . . ?
C22 C17 P1 120.71(15) . . ?
C18 C17 P1 119.34(13) . . ?
C19 C18 C17 119.69(18) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C20 C19 C18 120.05(19) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C21 120.04(19) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 120.82(19) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C17 119.44(19) . . ?
C21 C22 H22 120.3 . . ?
C17 C22 H22 120.3 . . ?
C28 C23 C24 120.01(17) . . ?
C28 C23 P1 121.57(14) . . ?
C24 C23 P1 118.36(14) . . ?
C25 C24 C23 120.19(19) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C26 C25 C24 119.57(19) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C27 120.61(19) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C26 C27 C28 120.4(2) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C27 C28 C23 119.22(19) . . ?
C27 C28 H28 120.4 . . ?
C23 C28 H28 120.4 . . ?
C34 C29 C30 120.30(17) . . ?
C34 C29 P1 120.45(14) . . ?
C30 C29 P1 119.26(14) . . ?
C31 C30 C29 119.36(18) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
C32 C31 C30 120.3(2) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C33 C32 C31 120.52(19) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 120.08(19) . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C29 119.46(19) . . ?
C33 C34 H34 120.3 . . ?
C29 C34 H34 120.3 . . ?
C40 C35 C36 120.22(17) . . ?
C40 C35 P1 120.90(14) . . ?
C36 C35 P1 118.68(14) . . ?
C37 C36 C35 119.76(18) . . ?
C37 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C36 C37 C38 119.99(19) . . ?
C36 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
C39 C38 C37 120.48(19) . . ?
C39 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
C38 C39 C40 120.20(19) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C39 C40 C35 119.34(18) . . ?
C39 C40 H40 120.3 . . ?
C35 C40 H40 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 N2 C1 1.43(19) . . . . ?
C3 N1 N2 C11 177.59(15) . . . . ?
Mo1 O1 C1 N2 -165.86(12) . . . . ?
Mo1 O1 C1 C2 14.4(3) . . . . ?
N1 N2 C1 O1 179.09(15) . . . . ?
C11 N2 C1 O1 3.5(3) . . . . ?
N1 N2 C1 C2 -1.13(19) . . . . ?
C11 N2 C1 C2 -176.75(16) . . . . ?
O1 C1 C2 C4 1.3(3) . . . . ?
N2 C1 C2 C4 -178.40(16) . . . . ?
O1 C1 C2 C3 -179.86(19) . . . . ?
N2 C1 C2 C3 0.40(18) . . . . ?
N2 N1 C3 C2 -1.14(19) . . . . ?
N2 N1 C3 C10 178.13(15) . . . . ?
C1 C2 C3 N1 0.5(2) . . . . ?
C4 C2 C3 N1 179.08(18) . . . . ?
C1 C2 C3 C10 -178.64(18) . . . . ?
C4 C2 C3 C10 0.0(3) . . . . ?
Mo1 O2 C4 C2 -10.0(3) . . . . ?
Mo1 O2 C4 C5 170.19(12) . . . . ?
C1 C2 C4 O2 -3.3(3) . . . . ?
C3 C2 C4 O2 178.28(18) . . . . ?
C1 C2 C4 C5 176.44(16) . . . . ?
C3 C2 C4 C5 -2.0(3) . . . . ?
O2 C4 C5 C6 -72.7(2) . . . . ?
C2 C4 C5 C6 107.5(2) . . . . ?
C4 C5 C6 C7 78.7(2) . . . . ?
C4 C5 C6 C9 -163.09(17) . . . . ?
C4 C5 C6 C8 -43.3(2) . . . . ?
C1 N2 C11 C16 141.33(18) . . . . ?
N1 N2 C11 C16 -34.0(2) . . . . ?
C1 N2 C11 C12 -39.5(3) . . . . ?
N1 N2 C11 C12 145.16(17) . . . . ?
C16 C11 C12 C13 -1.0(3) . . . . ?
N2 C11 C12 C13 179.86(17) . . . . ?
C11 C12 C13 C14 -0.8(3) . . . . ?
C12 C13 C14 C15 1.4(3) . . . . ?
C13 C14 C15 C16 -0.2(3) . . . . ?
C14 C15 C16 C11 -1.5(3) . . . . ?
C12 C11 C16 C15 2.1(3) . . . . ?
N2 C11 C16 C15 -178.69(16) . . . . ?
C23 P1 C17 C22 13.17(19) . . . . ?
C29 P1 C17 C22 134.49(16) . . . . ?
C35 P1 C17 C22 -106.02(17) . . . . ?
C23 P1 C17 C18 -168.40(15) . . . . ?
C29 P1 C17 C18 -47.08(17) . . . . ?
C35 P1 C17 C18 72.41(17) . . . . ?
C22 C17 C18 C19 1.7(3) . . . . ?
P1 C17 C18 C19 -176.76(14) . . . . ?
C17 C18 C19 C20 -2.0(3) . . . . ?
C18 C19 C20 C21 1.1(3) . . . . ?
C19 C20 C21 C22 0.2(3) . . . . ?
C20 C21 C22 C17 -0.6(3) . . . . ?
C18 C17 C22 C21 -0.4(3) . . . . ?
P1 C17 C22 C21 178.02(16) . . . . ?
C29 P1 C23 C28 -23.93(18) . . . . ?
C17 P1 C23 C28 96.57(17) . . . . ?
C35 P1 C23 C28 -142.34(16) . . . . ?
C29 P1 C23 C24 158.93(15) . . . . ?
C17 P1 C23 C24 -80.57(17) . . . . ?
C35 P1 C23 C24 40.52(17) . . . . ?
C28 C23 C24 C25 0.6(3) . . . . ?
P1 C23 C24 C25 177.83(16) . . . . ?
C23 C24 C25 C26 -0.1(3) . . . . ?
C24 C25 C26 C27 -0.2(3) . . . . ?
C25 C26 C27 C28 0.0(4) . . . . ?
C26 C27 C28 C23 0.6(3) . . . . ?
C24 C23 C28 C27 -0.9(3) . . . . ?
P1 C23 C28 C27 -177.96(16) . . . . ?
C23 P1 C29 C34 -109.08(16) . . . . ?
C17 P1 C29 C34 130.35(15) . . . . ?
C35 P1 C29 C34 9.15(18) . . . . ?
C23 P1 C29 C30 70.43(17) . . . . ?
C17 P1 C29 C30 -50.14(17) . . . . ?
C35 P1 C29 C30 -171.34(15) . . . . ?
C34 C29 C30 C31 0.4(3) . . . . ?
P1 C29 C30 C31 -179.12(15) . . . . ?
C29 C30 C31 C32 -1.4(3) . . . . ?
C30 C31 C32 C33 1.3(3) . . . . ?
C31 C32 C33 C34 -0.2(3) . . . . ?
C32 C33 C34 C29 -0.9(3) . . . . ?
C30 C29 C34 C33 0.7(3) . . . . ?
P1 C29 C34 C33 -179.75(15) . . . . ?
C23 P1 C35 C40 -144.23(15) . . . . ?
C29 P1 C35 C40 95.87(16) . . . . ?
C17 P1 C35 C40 -24.19(18) . . . . ?
C23 P1 C35 C36 40.93(17) . . . . ?
C29 P1 C35 C36 -78.97(17) . . . . ?
C17 P1 C35 C36 160.97(15) . . . . ?
C40 C35 C36 C37 -1.2(3) . . . . ?
P1 C35 C36 C37 173.73(16) . . . . ?
C35 C36 C37 C38 0.2(3) . . . . ?
C36 C37 C38 C39 0.4(3) . . . . ?
C37 C38 C39 C40 0.0(3) . . . . ?
C38 C39 C40 C35 -0.9(3) . . . . ?
C36 C35 C40 C39 1.5(3) . . . . ?
P1 C35 C40 C39 -173.24(15) . . . . ?

_refine_diff_density_max         0.813
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.055

####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 1580363'
_audit_update_record             
;
2017-10-19 deposited with the CCDC.
2017-11-27 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         'C34 H42 Mo N4 O7'
_chemical_formula_sum            'C34 H42 Mo N4 O7'
_chemical_formula_weight         714.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_H-M_alt        'A b a 2'
_space_group_name_Hall           'A 2 -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'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'

_cell_length_a                   9.7458(2)
_cell_length_b                   20.3853(4)
_cell_length_c                   17.2757(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3432.18(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9072
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      30.45

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_F_000             1488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.434
_shelx_estimated_absorpt_T_min   0.846
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8456
_exptl_absorpt_correction_T_max  0.9182
_exptl_absorpt_process_details   
; 
program SADABS, Bruker (2001). 
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            11966
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.358
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.694
_diffrn_reflns_point_group_measured_fraction_full 0.694
_reflns_number_total             2157
_reflns_number_gt                2111
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.340
_reflns_Friedel_fraction_max     0.366
_reflns_Friedel_fraction_full    0.367

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0083P)²+4.5384P] 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 515 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.03(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         2157
_refine_ls_number_parameters     224
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0512
_refine_ls_wR_factor_gt          0.0510
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_restrained_S_all      1.164
_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 0.500000 0.000000 0.23890(4) 0.02564(10) Uani 1 2 d DS T P . .
O1 O 0.3476(2) 0.06521(11) 0.26343(15) 0.0335(7) Uani 1 1 d . U . . .
O2 O 0.6014(3) 0.04746(13) 0.33327(17) 0.0352(7) Uani 1 1 d . U . . .
O3 O 0.5997(8) 0.0410(4) 0.1754(6) 0.0264(18) Uani 0.5 1 d D U P A 1
O4 O 0.5450(6) 0.0781(3) 0.1828(4) 0.0415(14) Uani 0.5 1 d D U P A 2
O5 O 0.6478(8) 0.0287(5) 0.1773(7) 0.035(2) Uani 0.5 1 d D U P A 2
N1 N 0.2461(3) 0.15510(13) 0.32150(18) 0.0291(7) Uani 1 1 d . . . . .
N2 N 0.2772(3) 0.20401(14) 0.37555(19) 0.0329(7) Uani 1 1 d . . . . .
C1 C 0.3526(4) 0.11343(16) 0.3125(2) 0.0269(8) Uani 1 1 d . . . . .
C2 C 0.4567(4) 0.13405(16) 0.3634(2) 0.0271(8) Uani 1 1 d . . . . .
C3 C 0.4008(4) 0.19145(16) 0.4007(2) 0.0298(8) Uani 1 1 d . . . . .
C4 C 0.5803(4) 0.09970(16) 0.3720(2) 0.0292(8) Uani 1 1 d . . . . .
C5 C 0.6944(4) 0.12094(18) 0.4246(3) 0.0417(10) Uani 1 1 d . . . . .
H5A H 0.654244 0.141323 0.471449 0.050 Uiso 1 1 calc R U . . .
H5B H 0.749741 0.154792 0.397905 0.050 Uiso 1 1 calc R U . . .
C6 C 0.7887(4) 0.06512(18) 0.4494(3) 0.0370(9) Uani 1 1 d . . . . .
H6A H 0.823581 0.042272 0.402784 0.044 Uiso 1 1 calc R U . . .
H6B H 0.868485 0.083425 0.477557 0.044 Uiso 1 1 calc R U . . .
C7 C 0.7152(4) 0.01621(18) 0.5009(3) 0.0365(10) Uani 1 1 d . . . . .
H7A H 0.626820 0.004412 0.476354 0.044 Uiso 1 1 calc R U . . .
H7B H 0.694264 0.037676 0.550938 0.044 Uiso 1 1 calc R U . . .
C8 C 0.7955(4) -0.04671(18) 0.5169(2) 0.0364(9) Uani 1 1 d . . . . .
H8A H 0.815057 -0.068955 0.467148 0.044 Uiso 1 1 calc R U . . .
H8B H 0.884425 -0.035250 0.541069 0.044 Uiso 1 1 calc R U . . .
C9 C 0.7192(4) -0.0935(2) 0.5693(3) 0.0426(10) Uani 1 1 d . . . . .
H9A H 0.629230 -0.103783 0.545701 0.051 Uiso 1 1 calc R U . . .
H9B H 0.701619 -0.071374 0.619412 0.051 Uiso 1 1 calc R U . . .
C10 C 0.7954(5) -0.1571(2) 0.5845(3) 0.0559(13) Uani 1 1 d . . . . .
H10A H 0.805960 -0.181246 0.535821 0.084 Uiso 1 1 calc R U . . .
H10B H 0.743235 -0.183776 0.621379 0.084 Uiso 1 1 calc R U . . .
H10C H 0.886095 -0.147311 0.606064 0.084 Uiso 1 1 calc R U . . .
C11 C 0.4643(4) 0.23569(19) 0.4599(3) 0.0393(10) Uani 1 1 d . . . . .
H11A H 0.400950 0.271667 0.471703 0.059 Uiso 1 1 calc R U . . .
H11B H 0.550256 0.253680 0.439511 0.059 Uiso 1 1 calc R U . . .
H11C H 0.483112 0.210689 0.507135 0.059 Uiso 1 1 calc R U . . .
C12 C 0.1168(4) 0.15456(19) 0.2832(3) 0.0317(9) Uani 1 1 d . . . . .
C13 C 0.0478(4) 0.0960(2) 0.2707(3) 0.0423(11) Uani 1 1 d . . . . .
H13 H 0.084696 0.055582 0.288523 0.051 Uiso 1 1 calc R U . . .
C14 C -0.0770(4) 0.0981(2) 0.2315(4) 0.0509(12) Uani 1 1 d . . . . .
H14 H -0.124259 0.058290 0.220972 0.061 Uiso 1 1 calc R U . . .
C15 C -0.1327(5) 0.1564(3) 0.2078(3) 0.0542(14) Uani 1 1 d . . . . .
H15 H -0.218947 0.157066 0.182189 0.065 Uiso 1 1 calc R U . . .
C16 C -0.0637(5) 0.2135(2) 0.2213(3) 0.0542(16) Uani 1 1 d . . . . .
H16 H -0.102812 0.253759 0.204450 0.065 Uiso 1 1 calc R U . . .
C17 C 0.0616(4) 0.21427(18) 0.2587(3) 0.0402(13) Uani 1 1 d . . . . .
H17 H 0.108841 0.254325 0.267606 0.048 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 O3 1.687(9) . ?
Mo1 O3 1.687(9) 2_655 ?
Mo1 O5 1.884(10) 2_655 ?
Mo1 O5 1.884(10) . ?
Mo1 O4 1.915(6) . ?
Mo1 O4 1.915(6) 2_655 ?
Mo1 O1 2.038(2) 2_655 ?
Mo1 O1 2.038(2) . ?
Mo1 O2 2.138(3) 2_655 ?
Mo1 O2 2.138(3) . ?
O1 C1 1.299(4) . ?
O2 C4 1.275(4) . ?
O4 O5 1.424(7) . ?
N1 C1 1.350(4) . ?
N1 N2 1.399(4) . ?
N1 C12 1.424(5) . ?
N2 C3 1.306(5) . ?
C1 C2 1.406(5) . ?
C2 C4 1.401(5) . ?
C2 C3 1.442(5) . ?
C3 C11 1.497(5) . ?
C4 C5 1.500(5) . ?
C5 C6 1.524(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.517(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.528(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.511(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.517(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.386(6) . ?
C12 C17 1.396(5) . ?
C13 C14 1.393(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.370(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.365(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(5) . ?
C16 H16 0.9500 . ?
C17 H17 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
O3 Mo1 O3 98.9(7) . 2_655 ?
O3 Mo1 O5 103.1(3) . 2_655 ?
O3 Mo1 O5 15.9(3) 2_655 2_655 ?
O5 Mo1 O5 111.3(7) 2_655 . ?
O5 Mo1 O4 98.5(4) 2_655 . ?
O5 Mo1 O4 44.0(2) . . ?
O3 Mo1 O4 102.4(4) . 2_655 ?
O3 Mo1 O4 29.2(3) 2_655 2_655 ?
O3 Mo1 O1 92.2(2) . 2_655 ?
O3 Mo1 O1 103.4(3) 2_655 2_655 ?
O3 Mo1 O1 103.4(3) . . ?
O3 Mo1 O1 92.2(2) 2_655 . ?
O5 Mo1 O1 76.3(2) 2_655 . ?
O5 Mo1 O1 118.2(3) . . ?
O4 Mo1 O1 74.3(2) . . ?
O4 Mo1 O1 118.74(19) 2_655 . ?
O1 Mo1 O1 155.99(15) 2_655 . ?
O3 Mo1 O2 170.5(4) . 2_655 ?
O3 Mo1 O2 90.3(4) 2_655 2_655 ?
O1 Mo1 O2 83.28(10) 2_655 2_655 ?
O1 Mo1 O2 78.45(10) . 2_655 ?
O3 Mo1 O2 90.3(4) . . ?
O3 Mo1 O2 170.5(4) 2_655 . ?
O5 Mo1 O2 157.6(3) 2_655 . ?
O5 Mo1 O2 86.4(4) . . ?
O4 Mo1 O2 84.5(2) . . ?
O4 Mo1 O2 150.2(2) 2_655 . ?
O1 Mo1 O2 78.45(10) 2_655 . ?
O1 Mo1 O2 83.28(10) . . ?
O2 Mo1 O2 80.61(17) 2_655 . ?
C1 O1 Mo1 127.0(2) . . ?
C4 O2 Mo1 134.8(2) . . ?
O5 O4 Mo1 66.9(5) . . ?
O4 O5 Mo1 69.1(4) . . ?
C1 N1 N2 111.0(3) . . ?
C1 N1 C12 128.5(3) . . ?
N2 N1 C12 120.5(3) . . ?
C3 N2 N1 106.3(3) . . ?
O1 C1 N1 121.4(3) . . ?
O1 C1 C2 131.4(3) . . ?
N1 C1 C2 107.1(3) . . ?
C4 C2 C1 122.5(3) . . ?
C4 C2 C3 133.0(3) . . ?
C1 C2 C3 104.4(3) . . ?
N2 C3 C2 111.0(3) . . ?
N2 C3 C11 119.3(3) . . ?
C2 C3 C11 129.6(3) . . ?
O2 C4 C2 120.0(3) . . ?
O2 C4 C5 116.1(3) . . ?
C2 C4 C5 123.9(3) . . ?
C4 C5 C6 113.7(3) . . ?
C4 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C7 C6 C5 111.7(3) . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 C8 114.6(3) . . ?
C6 C7 H7A 108.6 . . ?
C8 C7 H7A 108.6 . . ?
C6 C7 H7B 108.6 . . ?
C8 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
C9 C8 C7 112.7(3) . . ?
C9 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
C9 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C8 C9 C10 113.7(4) . . ?
C8 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
C8 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C17 121.1(4) . . ?
C13 C12 N1 120.5(3) . . ?
C17 C12 N1 118.4(4) . . ?
C12 C13 C14 118.2(4) . . ?
C12 C13 H13 120.9 . . ?
C14 C13 H13 120.9 . . ?
C15 C14 C13 121.2(4) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C16 C15 C14 119.6(4) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C15 C16 C17 121.6(5) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C16 C17 C12 118.2(4) . . ?
C16 C17 H17 120.9 . . ?
C12 C17 H17 120.9 . . ?

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
O5 Mo1 O5 O4 80.0(5) 2_655 . . . ?
O4 Mo1 O5 O4 123.8(6) 2_655 . . . ?
O1 Mo1 O5 O4 -164.8(6) 2_655 . . . ?
O1 Mo1 O5 O4 -5.4(7) . . . . ?
O2 Mo1 O5 O4 -140.1(6) 2_655 . . . ?
O2 Mo1 O5 O4 -85.8(5) . . . . ?
C1 N1 N2 C3 -1.3(4) . . . . ?
C12 N1 N2 C3 179.7(3) . . . . ?
Mo1 O1 C1 N1 177.3(2) . . . . ?
Mo1 O1 C1 C2 -2.1(6) . . . . ?
N2 N1 C1 O1 -178.1(3) . . . . ?
C12 N1 C1 O1 0.8(6) . . . . ?
N2 N1 C1 C2 1.4(4) . . . . ?
C12 N1 C1 C2 -179.7(3) . . . . ?
O1 C1 C2 C4 -3.8(6) . . . . ?
N1 C1 C2 C4 176.8(3) . . . . ?
O1 C1 C2 C3 178.4(4) . . . . ?
N1 C1 C2 C3 -1.0(4) . . . . ?
N1 N2 C3 C2 0.6(4) . . . . ?
N1 N2 C3 C11 179.9(3) . . . . ?
C4 C2 C3 N2 -177.2(4) . . . . ?
C1 C2 C3 N2 0.2(4) . . . . ?
C4 C2 C3 C11 3.6(7) . . . . ?
C1 C2 C3 C11 -179.0(4) . . . . ?
Mo1 O2 C4 C2 10.4(6) . . . . ?
Mo1 O2 C4 C5 -168.8(3) . . . . ?
C1 C2 C4 O2 -0.4(6) . . . . ?
C3 C2 C4 O2 176.7(4) . . . . ?
C1 C2 C4 C5 178.8(4) . . . . ?
C3 C2 C4 C5 -4.1(7) . . . . ?
O2 C4 C5 C6 -24.2(5) . . . . ?
C2 C4 C5 C6 156.6(4) . . . . ?
C4 C5 C6 C7 -66.9(5) . . . . ?
C5 C6 C7 C8 170.2(3) . . . . ?
C6 C7 C8 C9 179.2(3) . . . . ?
C7 C8 C9 C10 178.6(4) . . . . ?
C1 N1 C12 C13 41.8(6) . . . . ?
N2 N1 C12 C13 -139.4(4) . . . . ?
C1 N1 C12 C17 -138.3(4) . . . . ?
N2 N1 C12 C17 40.5(5) . . . . ?
C17 C12 C13 C14 1.5(7) . . . . ?
N1 C12 C13 C14 -178.6(4) . . . . ?
C12 C13 C14 C15 -2.0(8) . . . . ?
C13 C14 C15 C16 1.5(9) . . . . ?
C14 C15 C16 C17 -0.3(8) . . . . ?
C15 C16 C17 C12 -0.2(6) . . . . ?
C13 C12 C17 C16 -0.4(6) . . . . ?
N1 C12 C17 C16 179.7(3) . . . . ?

_refine_diff_density_max         0.242
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.038



#==============================================================================0
# start Validation Reply Form



_vrf_PLAT915_10                  
;
PROBLEM:
Alert level B
PLAT915_ALERT_3_B No Flack x Check Done: Low Friedel Pair Coverage        37 %

RESPONSE: 
The measurement could not be completed to an acceptable percentage of Friedel
Pair coverage because of technical problems occurring during the measurement.
The low Friedel pair coverage of 37% can be accepted due to good values for 
the quality parameters.The Flack x parameter with a value of -0.03(3) clearly 
indicates the correct enantiomer. Refinement of the inverted structure yields 
a Flack x parameter of 1.03(3). 
;
####################################################################### 
# 
# 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 1580364'
_audit_update_record             
;
2017-10-19 deposited with the CCDC.
2017-11-27 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         'C34 H42 Mo N4 O6'
_chemical_formula_sum            'C34 H42 Mo N4 O6'
_chemical_formula_weight         698.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_H-M_alt        'A b a 2'
_space_group_name_Hall           'A 2 -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'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, z+1/2'

_cell_length_a                   9.5954(8)
_cell_length_b                   20.5989(14)
_cell_length_c                   17.1471(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3389.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    9978
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      30.51

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_F_000             1456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.436
_shelx_estimated_absorpt_T_min   0.845
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8450
_exptl_absorpt_correction_T_max  0.9179
_exptl_absorpt_process_details   
; 
program SADABS, Bruker (2001). 
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            16514
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.376
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_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             3066
_reflns_number_gt                2830
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0505P)²+5.7692P] 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 1263 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.01(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         3066
_refine_ls_number_parameters     206
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1050
_refine_ls_wR_factor_gt          0.1012
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.083
_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 0.000000 0.000000 0.37037(7) 0.0256(2) Uani 1 2 d S T P . .
O1 O 0.1493(4) 0.06554(18) 0.3460(2) 0.0259(8) Uani 1 1 d . . . . .
O2 O -0.1044(5) 0.04833(19) 0.2726(3) 0.0340(10) Uani 1 1 d . . . . .
O3 O -0.0992(5) 0.04480(19) 0.4311(3) 0.0358(10) Uani 1 1 d . . . . .
N1 N 0.2562(5) 0.1527(2) 0.2864(3) 0.0276(10) Uani 1 1 d . . . . .
N2 N 0.2290(5) 0.2013(2) 0.2315(3) 0.0322(11) Uani 1 1 d . . . . .
C1 C 0.1475(6) 0.1127(3) 0.2953(3) 0.0263(11) Uani 1 1 d . . . . .
C2 C 0.0447(6) 0.1337(3) 0.2434(3) 0.0276(11) Uani 1 1 d . . . . .
C3 C 0.1020(6) 0.1889(3) 0.2055(4) 0.0311(12) Uani 1 1 d . . . . .
C4 C -0.0832(6) 0.0994(3) 0.2340(3) 0.0285(12) Uani 1 1 d . . . . .
C5 C -0.1976(7) 0.1215(3) 0.1802(4) 0.0413(15) Uani 1 1 d . . . . .
H5A H -0.155283 0.141710 0.133433 0.050 Uiso 1 1 calc R U . . .
H5B H -0.253778 0.155117 0.206934 0.050 Uiso 1 1 calc R U . . .
C6 C -0.2934(6) 0.0666(3) 0.1544(4) 0.0365(14) Uani 1 1 d . . . . .
H6A H -0.330578 0.044336 0.201134 0.044 Uiso 1 1 calc R U . . .
H6B H -0.373206 0.085120 0.125355 0.044 Uiso 1 1 calc R U . . .
C7 C -0.2191(7) 0.0174(3) 0.1031(4) 0.0371(15) Uani 1 1 d . . . . .
H7A H -0.129253 0.005893 0.127911 0.045 Uiso 1 1 calc R U . . .
H7B H -0.197913 0.038024 0.052307 0.045 Uiso 1 1 calc R U . . .
C8 C -0.3011(7) -0.0446(3) 0.0884(4) 0.0365(14) Uani 1 1 d . . . . .
H8A H -0.320565 -0.065958 0.138948 0.044 Uiso 1 1 calc R U . . .
H8B H -0.391579 -0.033295 0.064216 0.044 Uiso 1 1 calc R U . . .
C9 C -0.2250(8) -0.0919(3) 0.0359(4) 0.0434(16) Uani 1 1 d . . . . .
H9A H -0.134692 -0.103212 0.060345 0.052 Uiso 1 1 calc R U . . .
H9B H -0.204804 -0.070236 -0.014386 0.052 Uiso 1 1 calc R U . . .
C10 C -0.3057(10) -0.1538(4) 0.0202(5) 0.0549(19) Uani 1 1 d . . . . .
H10A H -0.318844 -0.177579 0.069142 0.082 Uiso 1 1 calc R U . . .
H10B H -0.253493 -0.180932 -0.016630 0.082 Uiso 1 1 calc R U . . .
H10C H -0.396739 -0.143006 -0.002170 0.082 Uiso 1 1 calc R U . . .
C11 C 0.0407(8) 0.2332(3) 0.1455(4) 0.0375(14) Uani 1 1 d . . . . .
H11A H 0.104799 0.269304 0.135722 0.056 Uiso 1 1 calc R U . . .
H11B H -0.048512 0.250143 0.164364 0.056 Uiso 1 1 calc R U . . .
H11C H 0.025658 0.209022 0.096929 0.056 Uiso 1 1 calc R U . . .
C12 C 0.3880(6) 0.1525(3) 0.3251(4) 0.0269(13) Uani 1 1 d . . . . .
C13 C 0.4563(7) 0.0945(3) 0.3387(4) 0.0359(15) Uani 1 1 d . . . . .
H13 H 0.416953 0.054750 0.321238 0.043 Uiso 1 1 calc R U . . .
C14 C 0.5838(6) 0.0947(3) 0.3782(5) 0.0410(15) Uani 1 1 d . . . . .
H14 H 0.630113 0.055098 0.389617 0.049 Uiso 1 1 calc R U . . .
C15 C 0.6414(7) 0.1533(4) 0.4002(5) 0.0476(18) Uani 1 1 d . . . . .
H15 H 0.728999 0.153883 0.426026 0.057 Uiso 1 1 calc R U . . .
C16 C 0.5735(7) 0.2106(3) 0.3854(5) 0.049(2) Uani 1 1 d . . . . .
H16 H 0.615013 0.250445 0.400990 0.059 Uiso 1 1 calc R U . . .
C17 C 0.4452(7) 0.2114(3) 0.3480(4) 0.0408(18) Uani 1 1 d . . . . .
H17 H 0.397831 0.251073 0.338304 0.049 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 O3 1.686(4) 2 ?
Mo1 O3 1.686(4) . ?
Mo1 O1 2.012(4) 2 ?
Mo1 O1 2.012(4) . ?
Mo1 O2 2.192(4) 2 ?
Mo1 O2 2.192(4) . ?
O1 C1 1.305(7) . ?
O2 C4 1.260(7) . ?
N1 C1 1.337(7) . ?
N1 N2 1.399(6) . ?
N1 C12 1.428(8) . ?
N2 C3 1.322(8) . ?
C1 C2 1.396(9) . ?
C2 C3 1.421(8) . ?
C2 C4 1.425(8) . ?
C3 C11 1.496(8) . ?
C4 C5 1.505(8) . ?
C5 C6 1.522(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.520(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.522(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.513(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.517(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.382(8) . ?
C12 C17 1.388(8) . ?
C13 C14 1.398(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.379(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.373(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.389(9) . ?
C16 H16 0.9500 . ?
C17 H17 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
O3 Mo1 O3 103.7(3) 2 . ?
O3 Mo1 O1 99.35(18) 2 2 ?
O3 Mo1 O1 95.37(18) . 2 ?
O3 Mo1 O1 95.37(18) 2 . ?
O3 Mo1 O1 99.36(18) . . ?
O1 Mo1 O1 156.1(2) 2 . ?
O3 Mo1 O2 88.0(2) 2 2 ?
O3 Mo1 O2 168.3(2) . 2 ?
O1 Mo1 O2 82.08(15) 2 2 ?
O1 Mo1 O2 79.68(15) . 2 ?
O3 Mo1 O2 168.3(2) 2 . ?
O3 Mo1 O2 88.0(2) . . ?
O1 Mo1 O2 79.68(15) 2 . ?
O1 Mo1 O2 82.08(15) . . ?
O2 Mo1 O2 80.2(3) 2 . ?
C1 O1 Mo1 129.0(4) . . ?
C4 O2 Mo1 135.0(4) . . ?
C1 N1 N2 111.8(5) . . ?
C1 N1 C12 129.5(5) . . ?
N2 N1 C12 118.7(4) . . ?
C3 N2 N1 105.1(5) . . ?
O1 C1 N1 121.6(5) . . ?
O1 C1 C2 131.6(5) . . ?
N1 C1 C2 106.8(5) . . ?
C1 C2 C3 105.4(5) . . ?
C1 C2 C4 121.8(5) . . ?
C3 C2 C4 132.7(5) . . ?
N2 C3 C2 110.9(5) . . ?
N2 C3 C11 118.5(5) . . ?
C2 C3 C11 130.6(5) . . ?
O2 C4 C2 119.6(5) . . ?
O2 C4 C5 117.2(5) . . ?
C2 C4 C5 123.2(5) . . ?
C4 C5 C6 113.2(5) . . ?
C4 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.8 . . ?
C7 C6 C5 112.3(5) . . ?
C7 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 C8 114.4(5) . . ?
C6 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
C6 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
C9 C8 C7 112.9(5) . . ?
C9 C8 H8A 109.0 . . ?
C7 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C8 C9 C10 113.6(6) . . ?
C8 C9 H9A 108.8 . . ?
C10 C9 H9A 108.8 . . ?
C8 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C3 C11 H11A 109.5 . . ?
C3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C17 121.4(6) . . ?
C13 C12 N1 120.0(5) . . ?
C17 C12 N1 118.6(5) . . ?
C12 C13 C14 119.6(6) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C15 C14 C13 119.1(6) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C16 C15 C14 120.8(6) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 121.0(6) . . ?
C15 C16 H16 119.5 . . ?
C17 C16 H16 119.5 . . ?
C12 C17 C16 118.1(7) . . ?
C12 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?

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 N1 N2 C3 -1.6(6) . . . . ?
C12 N1 N2 C3 179.6(5) . . . . ?
Mo1 O1 C1 N1 179.7(4) . . . . ?
Mo1 O1 C1 C2 1.1(8) . . . . ?
N2 N1 C1 O1 -177.3(4) . . . . ?
C12 N1 C1 O1 1.3(9) . . . . ?
N2 N1 C1 C2 1.6(6) . . . . ?
C12 N1 C1 C2 -179.8(5) . . . . ?
O1 C1 C2 C3 177.7(6) . . . . ?
N1 C1 C2 C3 -1.0(6) . . . . ?
O1 C1 C2 C4 -5.2(9) . . . . ?
N1 C1 C2 C4 176.1(5) . . . . ?
N1 N2 C3 C2 0.9(6) . . . . ?
N1 N2 C3 C11 179.6(5) . . . . ?
C1 C2 C3 N2 0.0(6) . . . . ?
C4 C2 C3 N2 -176.6(6) . . . . ?
C1 C2 C3 C11 -178.4(6) . . . . ?
C4 C2 C3 C11 5.0(11) . . . . ?
Mo1 O2 C4 C2 10.6(9) . . . . ?
Mo1 O2 C4 C5 -168.7(5) . . . . ?
C1 C2 C4 O2 -0.9(9) . . . . ?
C3 C2 C4 O2 175.3(6) . . . . ?
C1 C2 C4 C5 178.4(6) . . . . ?
C3 C2 C4 C5 -5.4(10) . . . . ?
O2 C4 C5 C6 -24.3(8) . . . . ?
C2 C4 C5 C6 156.4(6) . . . . ?
C4 C5 C6 C7 -66.5(7) . . . . ?
C5 C6 C7 C8 169.0(5) . . . . ?
C6 C7 C8 C9 179.0(5) . . . . ?
C7 C8 C9 C10 -179.6(6) . . . . ?
C1 N1 C12 C13 41.8(9) . . . . ?
N2 N1 C12 C13 -139.8(6) . . . . ?
C1 N1 C12 C17 -138.7(6) . . . . ?
N2 N1 C12 C17 39.8(8) . . . . ?
C17 C12 C13 C14 1.9(11) . . . . ?
N1 C12 C13 C14 -178.6(7) . . . . ?
C12 C13 C14 C15 -2.4(13) . . . . ?
C13 C14 C15 C16 1.5(13) . . . . ?
C14 C15 C16 C17 0.1(12) . . . . ?
C13 C12 C17 C16 -0.3(10) . . . . ?
N1 C12 C17 C16 -179.8(6) . . . . ?
C15 C16 C17 C12 -0.7(11) . . . . ?

_refine_diff_density_max         1.081
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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 1580362'
_audit_update_record             
;
2017-10-19 deposited with the CCDC.
2017-11-27 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 H38 Mo N4 O7'
_chemical_formula_sum            'C32 H38 Mo N4 O7'
_chemical_formula_weight         686.60

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0124(4)
_cell_length_b                   13.5773(7)
_cell_length_c                   13.8352(7)
_cell_angle_alpha                78.094(2)
_cell_angle_beta                 73.696(2)
_cell_angle_gamma                82.144(2)
_cell_volume                     1584.29(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    213(2)
_cell_measurement_reflns_used    7194
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      28,43

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_F_000             712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.400
_exptl_absorpt_coefficient_mu    0.467
_shelx_estimated_absorpt_T_min   0.800
_shelx_estimated_absorpt_T_max   0.835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8001
_exptl_absorpt_correction_T_max  0.8352
_exptl_absorpt_process_details   
;
program SADABS, Bruker (2001).
;
_diffrn_ambient_temperature      213(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            29597
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.363
_diffrn_reflns_theta_max         25.246
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             5709
_reflns_number_gt                5180
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0346P)²+1.0721P] 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         5709
_refine_ls_number_parameters     433
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0749
_refine_ls_wR_factor_gt          0.0731
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.131
_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 0.30808(2) 0.25610(2) 0.26800(2) 0.03298(7) Uani 1 1 d D . . . .
O1 O 0.43847(19) 0.21369(14) 0.13564(12) 0.0460(4) Uani 1 1 d . U . . .
O2 O 0.52479(18) 0.23514(12) 0.30471(11) 0.0396(4) Uani 1 1 d . U . . .
O3 O 0.24670(19) 0.31638(13) 0.39754(13) 0.0466(4) Uani 1 1 d . U . . .
O4 O 0.40722(18) 0.39758(12) 0.20022(12) 0.0383(3) Uani 1 1 d . U . . .
O5A O 0.2655(4) 0.14055(14) 0.33524(19) 0.0452(7) Uani 0.693(4) 1 d D U P A 1
O6A O 0.1688(3) 0.2823(3) 0.18246(19) 0.0492(8) Uani 0.693(4) 1 d D U P A 1
O7A O 0.1044(2) 0.32107(19) 0.2743(2) 0.0527(7) Uani 0.693(4) 1 d D U P A 1
O5B O 0.1625(6) 0.3001(5) 0.2130(5) 0.0408(12) Uani 0.307(4) 1 d D U P A 2
O6B O 0.3197(8) 0.11236(16) 0.2845(5) 0.0600(13) Uani 0.307(4) 1 d D U P A 2
O7B O 0.2421(10) 0.1469(3) 0.3774(3) 0.0585(13) Uani 0.307(4) 1 d D U P A 2
N1 N 0.6497(2) 0.14148(14) 0.02785(13) 0.0365(4) Uani 1 1 d . . . . .
N2 N 0.8062(2) 0.11181(16) 0.02085(15) 0.0445(5) Uani 1 1 d . . . . .
N3 N 0.2348(2) 0.43204(16) 0.49938(16) 0.0462(5) Uani 1 1 d . . . . .
N4 N 0.2901(3) 0.52437(17) 0.49475(18) 0.0605(6) Uani 1 1 d . . . . .
C1 C 0.8331(3) 0.12837(19) 0.10360(18) 0.0415(5) Uani 1 1 d . . . . .
C2 C 0.6946(2) 0.16885(17) 0.16964(16) 0.0345(5) Uani 1 1 d . . . . .
C3 C 0.5813(2) 0.17719(16) 0.11492(16) 0.0341(5) Uani 1 1 d . . . . .
C4 C 0.9945(3) 0.1067(3) 0.1153(2) 0.0652(8) Uani 1 1 d . . . . .
H4A H 1.058797 0.074128 0.059756 0.098 Uiso 1 1 calc R U . . .
H4B H 0.993621 0.062354 0.180089 0.098 Uiso 1 1 calc R U . . .
H4C H 1.036135 0.169410 0.113555 0.098 Uiso 1 1 calc R U . . .
C5 C 0.6606(2) 0.19947(16) 0.26503(16) 0.0324(5) Uani 1 1 d . . . . .
C6 C 0.7751(3) 0.19509(17) 0.32647(17) 0.0361(5) Uani 1 1 d . . . . .
H6A H 0.764996 0.260044 0.349125 0.043 Uiso 1 1 calc R U . . .
H6B H 0.879928 0.186553 0.281700 0.043 Uiso 1 1 calc R U . . .
C7 C 0.7582(3) 0.10971(18) 0.42179(17) 0.0375(5) Uani 1 1 d . . . . .
C8 C 0.7981(4) 0.0063(2) 0.3902(2) 0.0558(7) Uani 1 1 d . . . . .
H8A H 0.904841 0.001442 0.349384 0.084 Uiso 1 1 calc R U . . .
H8B H 0.729665 -0.002583 0.350188 0.084 Uiso 1 1 calc R U . . .
H8C H 0.785372 -0.045825 0.450802 0.084 Uiso 1 1 calc R U . . .
C9 C 0.8714(3) 0.1269(2) 0.4797(2) 0.0580(7) Uani 1 1 d . . . . .
H9A H 0.867819 0.073392 0.538694 0.087 Uiso 1 1 calc R U . . .
H9B H 0.842509 0.191524 0.502339 0.087 Uiso 1 1 calc R U . . .
H9C H 0.975731 0.126616 0.434933 0.087 Uiso 1 1 calc R U . . .
C10 C 0.5942(3) 0.1141(2) 0.49270(19) 0.0482(6) Uani 1 1 d . . . . .
H10A H 0.590563 0.064463 0.554572 0.072 Uiso 1 1 calc R U . . .
H10B H 0.521618 0.099764 0.458317 0.072 Uiso 1 1 calc R U . . .
H10C H 0.566492 0.181043 0.510220 0.072 Uiso 1 1 calc R U . . .
C11 C 0.5856(3) 0.12675(16) -0.05106(16) 0.0371(5) Uani 1 1 d . . . . .
C12 C 0.4285(3) 0.1356(2) -0.04006(19) 0.0500(6) Uani 1 1 d . . . . .
H12 H 0.359636 0.153178 0.019961 0.060 Uiso 1 1 calc R U . . .
C13 C 0.3720(4) 0.1185(2) -0.1181(2) 0.0575(7) Uani 1 1 d . . . . .
H13 H 0.264464 0.125460 -0.110947 0.069 Uiso 1 1 calc R U . . .
C14 C 0.4703(4) 0.0918(2) -0.2051(2) 0.0594(8) Uani 1 1 d . . . . .
H14 H 0.430993 0.080323 -0.257583 0.071 Uiso 1 1 calc R U . . .
C15 C 0.6265(4) 0.0818(3) -0.2151(2) 0.0665(8) Uani 1 1 d . . . . .
H15 H 0.694586 0.062574 -0.274549 0.080 Uiso 1 1 calc R U . . .
C16 C 0.6859(3) 0.0996(2) -0.13879(19) 0.0556(7) Uani 1 1 d . . . . .
H16 H 0.793687 0.093254 -0.146704 0.067 Uiso 1 1 calc R U . . .
C17 C 0.3733(3) 0.5490(2) 0.4014(2) 0.0551(7) Uani 1 1 d . . . . .
C18 C 0.3758(3) 0.47463(18) 0.34019(19) 0.0414(5) Uani 1 1 d . . . . .
C19 C 0.2844(3) 0.40074(18) 0.40940(18) 0.0387(5) Uani 1 1 d . . . . .
C20 C 0.4516(5) 0.6452(3) 0.3732(3) 0.0907(13) Uani 1 1 d . . . . .
H20A H 0.444114 0.671402 0.434739 0.136 Uiso 1 1 calc R U . . .
H20B H 0.401477 0.694430 0.328296 0.136 Uiso 1 1 calc R U . . .
H20C H 0.559987 0.632145 0.338450 0.136 Uiso 1 1 calc R U . . .
C21 C 0.4334(3) 0.47118(17) 0.23589(18) 0.0382(5) Uani 1 1 d . . . . .
C22 C 0.5251(3) 0.55175(18) 0.16075(19) 0.0452(6) Uani 1 1 d . . . . .
H22A H 0.520801 0.608857 0.195010 0.054 Uiso 1 1 calc R U . . .
H22B H 0.475146 0.575834 0.104769 0.054 Uiso 1 1 calc R U . . .
C23 C 0.6974(3) 0.51832(19) 0.11449(19) 0.0446(6) Uani 1 1 d . . . . .
C24 C 0.7128(4) 0.4565(2) 0.0319(2) 0.0635(8) Uani 1 1 d . . . . .
H24A H 0.820809 0.433070 0.006794 0.095 Uiso 1 1 calc R U . . .
H24B H 0.675770 0.497969 -0.023973 0.095 Uiso 1 1 calc R U . . .
H24C H 0.651555 0.398792 0.060263 0.095 Uiso 1 1 calc R U . . .
C25 C 0.7685(3) 0.4578(2) 0.1980(2) 0.0597(7) Uani 1 1 d . . . . .
H25A H 0.716185 0.396560 0.227718 0.090 Uiso 1 1 calc R U . . .
H25B H 0.756920 0.497868 0.250554 0.090 Uiso 1 1 calc R U . . .
H25C H 0.877779 0.440430 0.168980 0.090 Uiso 1 1 calc R U . . .
C26 C 0.7817(4) 0.6141(2) 0.0662(3) 0.0684(9) Uani 1 1 d . . . . .
H26A H 0.888890 0.595763 0.032805 0.103 Uiso 1 1 calc R U . . .
H26B H 0.778043 0.652221 0.119082 0.103 Uiso 1 1 calc R U . . .
H26C H 0.731463 0.655152 0.016255 0.103 Uiso 1 1 calc R U . . .
C27 C 0.1338(3) 0.3872(2) 0.59285(19) 0.0469(6) Uani 1 1 d . . . . .
C28 C 0.0371(3) 0.4503(2) 0.6546(2) 0.0498(6) Uani 1 1 d . . . . .
H28 H 0.034922 0.520788 0.633630 0.060 Uiso 1 1 calc R U . . .
C29 C -0.0564(3) 0.4086(3) 0.7475(2) 0.0601(8) Uani 1 1 d . . . . .
H29 H -0.122043 0.451147 0.790131 0.072 Uiso 1 1 calc R U . . .
C30 C -0.0547(4) 0.3064(3) 0.7781(2) 0.0753(10) Uani 1 1 d . . . . .
H30 H -0.118898 0.278729 0.841467 0.090 Uiso 1 1 calc R U . . .
C31 C 0.0420(5) 0.2439(3) 0.7155(3) 0.0878(12) Uani 1 1 d . . . . .
H31 H 0.042676 0.173417 0.736203 0.105 Uiso 1 1 calc R U . . .
C32 C 0.1378(4) 0.2843(2) 0.6225(2) 0.0709(9) Uani 1 1 d . . . . .
H32 H 0.204609 0.241803 0.580305 0.085 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 O5B 1.678(2) . ?
Mo1 O5A 1.6839(16) . ?
Mo1 O6A 1.9081(17) . ?
Mo1 O6B 1.909(2) . ?
Mo1 O7B 1.912(2) . ?
Mo1 O7A 1.9118(16) . ?
Mo1 O1 2.0267(15) . ?
Mo1 O3 2.0280(15) . ?
Mo1 O2 2.1211(15) . ?
Mo1 O4 2.1502(15) . ?
O1 C3 1.289(3) . ?
O2 C5 1.266(3) . ?
O3 C19 1.292(3) . ?
O4 C21 1.277(3) . ?
O6A O7A 1.4162(18) . ?
O6B O7B 1.419(2) . ?
N1 C3 1.345(3) . ?
N1 N2 1.395(3) . ?
N1 C11 1.429(3) . ?
N2 C1 1.303(3) . ?
N3 C19 1.336(3) . ?
N3 N4 1.394(3) . ?
N3 C27 1.427(3) . ?
N4 C17 1.300(4) . ?
C1 C2 1.440(3) . ?
C1 C4 1.492(3) . ?
C2 C5 1.405(3) . ?
C2 C3 1.412(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C5 C6 1.499(3) . ?
C6 C7 1.553(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C8 1.523(3) . ?
C7 C10 1.528(3) . ?
C7 C9 1.530(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 C12 1.371(4) . ?
C11 C16 1.380(3) . ?
C12 C13 1.387(3) . ?
C12 H12 0.9400 . ?
C13 C14 1.363(4) . ?
C13 H13 0.9400 . ?
C14 C15 1.366(4) . ?
C14 H14 0.9400 . ?
C15 C16 1.384(4) . ?
C15 H15 0.9400 . ?
C16 H16 0.9400 . ?
C17 C18 1.440(3) . ?
C17 C20 1.498(4) . ?
C18 C21 1.398(3) . ?
C18 C19 1.410(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 C22 1.502(3) . ?
C22 C23 1.548(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C23 C25 1.516(3) . ?
C23 C24 1.518(4) . ?
C23 C26 1.530(4) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 H25C 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C27 C32 1.371(4) . ?
C27 C28 1.380(3) . ?
C28 C29 1.380(4) . ?
C28 H28 0.9400 . ?
C29 C30 1.364(5) . ?
C29 H29 0.9400 . ?
C30 C31 1.381(5) . ?
C30 H30 0.9400 . ?
C31 C32 1.385(4) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?

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
O5A Mo1 O6A 102.16(15) . . ?
O5B Mo1 O6B 106.1(3) . . ?
O5B Mo1 O7B 109.1(4) . . ?
O6B Mo1 O7B 43.62(7) . . ?
O5A Mo1 O7A 100.73(13) . . ?
O6A Mo1 O7A 43.52(6) . . ?
O5B Mo1 O1 90.1(3) . . ?
O5A Mo1 O1 98.20(11) . . ?
O6A Mo1 O1 76.49(9) . . ?
O6B Mo1 O1 71.34(19) . . ?
O7B Mo1 O1 114.8(2) . . ?
O7A Mo1 O1 119.53(9) . . ?
O5B Mo1 O3 103.4(2) . . ?
O5A Mo1 O3 91.50(11) . . ?
O6A Mo1 O3 118.02(9) . . ?
O6B Mo1 O3 116.91(19) . . ?
O7B Mo1 O3 74.3(2) . . ?
O7A Mo1 O3 74.67(9) . . ?
O1 Mo1 O3 160.51(7) . . ?
O5B Mo1 O2 163.1(3) . . ?
O5A Mo1 O2 89.96(11) . . ?
O6A Mo1 O2 157.21(10) . . ?
O6B Mo1 O2 86.1(2) . . ?
O7B Mo1 O2 87.8(3) . . ?
O7A Mo1 O2 152.97(9) . . ?
O1 Mo1 O2 82.78(6) . . ?
O3 Mo1 O2 80.35(6) . . ?
O5B Mo1 O4 87.5(3) . . ?
O5A Mo1 O4 166.08(11) . . ?
O6A Mo1 O4 91.65(12) . . ?
O6B Mo1 O4 150.8(2) . . ?
O7B Mo1 O4 154.6(2) . . ?
O7A Mo1 O4 90.45(9) . . ?
O1 Mo1 O4 83.19(7) . . ?
O3 Mo1 O4 83.42(6) . . ?
O2 Mo1 O4 76.43(6) . . ?
C3 O1 Mo1 127.96(14) . . ?
C5 O2 Mo1 135.84(14) . . ?
C19 O3 Mo1 127.41(15) . . ?
C21 O4 Mo1 134.23(15) . . ?
O7A O6A Mo1 68.38(10) . . ?
O6A O7A Mo1 68.10(10) . . ?
O7B O6B Mo1 68.28(11) . . ?
O6B O7B Mo1 68.10(11) . . ?
C3 N1 N2 110.92(18) . . ?
C3 N1 C11 130.30(19) . . ?
N2 N1 C11 118.72(17) . . ?
C1 N2 N1 106.55(18) . . ?
C19 N3 N4 111.5(2) . . ?
C19 N3 C27 129.7(2) . . ?
N4 N3 C27 118.76(19) . . ?
C17 N4 N3 105.8(2) . . ?
N2 C1 C2 111.3(2) . . ?
N2 C1 C4 118.3(2) . . ?
C2 C1 C4 130.4(2) . . ?
C5 C2 C3 121.92(19) . . ?
C5 C2 C1 134.2(2) . . ?
C3 C2 C1 103.87(19) . . ?
O1 C3 N1 122.0(2) . . ?
O1 C3 C2 130.6(2) . . ?
N1 C3 C2 107.38(18) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O2 C5 C2 120.00(19) . . ?
O2 C5 C6 114.99(19) . . ?
C2 C5 C6 125.00(19) . . ?
C5 C6 C7 115.33(18) . . ?
C5 C6 H6A 108.4 . . ?
C7 C6 H6A 108.4 . . ?
C5 C6 H6B 108.4 . . ?
C7 C6 H6B 108.4 . . ?
H6A C6 H6B 107.5 . . ?
C8 C7 C10 109.3(2) . . ?
C8 C7 C9 109.9(2) . . ?
C10 C7 C9 108.5(2) . . ?
C8 C7 C6 110.9(2) . . ?
C10 C7 C6 111.65(19) . . ?
C9 C7 C6 106.6(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C16 119.9(2) . . ?
C12 C11 N1 121.8(2) . . ?
C16 C11 N1 118.2(2) . . ?
C11 C12 C13 119.5(2) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 C12 120.9(3) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 119.3(3) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C14 C15 C16 120.9(3) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C11 C16 C15 119.4(3) . . ?
C11 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
N4 C17 C18 111.8(2) . . ?
N4 C17 C20 118.3(2) . . ?
C18 C17 C20 129.9(3) . . ?
C21 C18 C19 122.7(2) . . ?
C21 C18 C17 133.5(2) . . ?
C19 C18 C17 103.4(2) . . ?
O3 C19 N3 121.3(2) . . ?
O3 C19 C18 131.3(2) . . ?
N3 C19 C18 107.5(2) . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 C18 120.0(2) . . ?
O4 C21 C22 116.8(2) . . ?
C18 C21 C22 123.1(2) . . ?
C21 C22 C23 115.0(2) . . ?
C21 C22 H22A 108.5 . . ?
C23 C22 H22A 108.5 . . ?
C21 C22 H22B 108.5 . . ?
C23 C22 H22B 108.5 . . ?
H22A C22 H22B 107.5 . . ?
C25 C23 C24 110.2(2) . . ?
C25 C23 C26 109.5(2) . . ?
C24 C23 C26 108.8(2) . . ?
C25 C23 C22 110.0(2) . . ?
C24 C23 C22 110.8(2) . . ?
C26 C23 C22 107.4(2) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C32 C27 C28 121.0(3) . . ?
C32 C27 N3 120.9(2) . . ?
C28 C27 N3 118.1(2) . . ?
C27 C28 C29 119.1(3) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 120.8(3) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C31 119.6(3) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C32 120.4(3) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C27 C32 C31 119.1(3) . . ?
C27 C32 H32 120.5 . . ?
C31 C32 H32 120.5 . . ?

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
C3 N1 N2 C1 0.6(3) . . . . ?
C11 N1 N2 C1 -176.8(2) . . . . ?
C19 N3 N4 C17 0.1(3) . . . . ?
C27 N3 N4 C17 -177.7(2) . . . . ?
N1 N2 C1 C2 0.6(3) . . . . ?
N1 N2 C1 C4 -177.9(2) . . . . ?
N2 C1 C2 C5 -179.7(2) . . . . ?
C4 C1 C2 C5 -1.4(5) . . . . ?
N2 C1 C2 C3 -1.5(3) . . . . ?
C4 C1 C2 C3 176.8(3) . . . . ?
Mo1 O1 C3 N1 172.42(16) . . . . ?
Mo1 O1 C3 C2 -10.0(4) . . . . ?
N2 N1 C3 O1 176.5(2) . . . . ?
C11 N1 C3 O1 -6.4(4) . . . . ?
N2 N1 C3 C2 -1.6(2) . . . . ?
C11 N1 C3 C2 175.5(2) . . . . ?
C5 C2 C3 O1 2.4(4) . . . . ?
C1 C2 C3 O1 -176.1(2) . . . . ?
C5 C2 C3 N1 -179.7(2) . . . . ?
C1 C2 C3 N1 1.8(2) . . . . ?
Mo1 O2 C5 C2 4.9(3) . . . . ?
Mo1 O2 C5 C6 -175.92(14) . . . . ?
C3 C2 C5 O2 0.5(3) . . . . ?
C1 C2 C5 O2 178.4(2) . . . . ?
C3 C2 C5 C6 -178.6(2) . . . . ?
C1 C2 C5 C6 -0.7(4) . . . . ?
O2 C5 C6 C7 75.2(3) . . . . ?
C2 C5 C6 C7 -105.7(2) . . . . ?
C5 C6 C7 C8 67.2(3) . . . . ?
C5 C6 C7 C10 -54.9(3) . . . . ?
C5 C6 C7 C9 -173.2(2) . . . . ?
C3 N1 C11 C12 -9.6(4) . . . . ?
N2 N1 C11 C12 167.2(2) . . . . ?
C3 N1 C11 C16 172.6(2) . . . . ?
N2 N1 C11 C16 -10.6(3) . . . . ?
C16 C11 C12 C13 -0.9(4) . . . . ?
N1 C11 C12 C13 -178.7(2) . . . . ?
C11 C12 C13 C14 0.8(4) . . . . ?
C12 C13 C14 C15 0.0(5) . . . . ?
C13 C14 C15 C16 -0.8(5) . . . . ?
C12 C11 C16 C15 0.1(4) . . . . ?
N1 C11 C16 C15 178.0(2) . . . . ?
C14 C15 C16 C11 0.7(5) . . . . ?
N3 N4 C17 C18 0.4(3) . . . . ?
N3 N4 C17 C20 -178.9(3) . . . . ?
N4 C17 C18 C21 172.3(3) . . . . ?
C20 C17 C18 C21 -8.5(6) . . . . ?
N4 C17 C18 C19 -0.7(3) . . . . ?
C20 C17 C18 C19 178.4(3) . . . . ?
Mo1 O3 C19 N3 179.57(17) . . . . ?
Mo1 O3 C19 C18 -0.2(4) . . . . ?
N4 N3 C19 O3 179.7(2) . . . . ?
C27 N3 C19 O3 -2.8(4) . . . . ?
N4 N3 C19 C18 -0.5(3) . . . . ?
C27 N3 C19 C18 177.0(2) . . . . ?
C21 C18 C19 O3 6.5(4) . . . . ?
C17 C18 C19 O3 -179.5(3) . . . . ?
C21 C18 C19 N3 -173.3(2) . . . . ?
C17 C18 C19 N3 0.7(3) . . . . ?
Mo1 O4 C21 C18 -8.5(3) . . . . ?
Mo1 O4 C21 C22 172.32(15) . . . . ?
C19 C18 C21 O4 -1.9(4) . . . . ?
C17 C18 C21 O4 -173.8(3) . . . . ?
C19 C18 C21 C22 177.3(2) . . . . ?
C17 C18 C21 C22 5.4(4) . . . . ?
O4 C21 C22 C23 -68.4(3) . . . . ?
C18 C21 C22 C23 112.4(3) . . . . ?
C21 C22 C23 C25 -44.7(3) . . . . ?
C21 C22 C23 C24 77.5(3) . . . . ?
C21 C22 C23 C26 -163.8(2) . . . . ?
C19 N3 C27 C32 36.4(4) . . . . ?
N4 N3 C27 C32 -146.2(3) . . . . ?
C19 N3 C27 C28 -146.4(3) . . . . ?
N4 N3 C27 C28 30.9(4) . . . . ?
C32 C27 C28 C29 0.1(4) . . . . ?
N3 C27 C28 C29 -177.1(2) . . . . ?
C27 C28 C29 C30 -0.4(4) . . . . ?
C28 C29 C30 C31 0.1(5) . . . . ?
C29 C30 C31 C32 0.6(6) . . . . ?
C28 C27 C32 C31 0.5(5) . . . . ?
N3 C27 C32 C31 177.6(3) . . . . ?
C30 C31 C32 C27 -0.9(6) . . . . ?

_refine_diff_density_max         0.614
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.049

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1580361'
_audit_update_record             
;
2017-10-19 deposited with the CCDC.
2017-11-27 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         'C13 H8 F5 Mo N2 O7, C24 H20 P'
_chemical_formula_sum            'C37 H28 F5 Mo N2 O7 P'
_chemical_formula_weight         834.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1318(4)
_cell_length_b                   13.3189(6)
_cell_length_c                   13.8696(6)
_cell_angle_alpha                88.5380(10)
_cell_angle_beta                 84.4170(10)
_cell_angle_gamma                71.8310(10)
_cell_volume                     1769.85(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    7516
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      30.50

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_F_000             844
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.495
_shelx_estimated_absorpt_T_min   0.790
_shelx_estimated_absorpt_T_max   0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7900
_exptl_absorpt_correction_T_max  0.9075
_exptl_absorpt_process_details   
;
program SADABS, Bruker (2001).
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
 Bruker-Nonius X8kappa APEX II CCD area detector
;
_diffrn_measurement_method       'phi and omega scans with narrow frames'
_diffrn_detector_area_resol_mean 8.26
_diffrn_reflns_number            29875
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.609
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6358
_reflns_number_gt                6026
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0471P)²+1.1365P] 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         6358
_refine_ls_number_parameters     479
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0801
_refine_ls_wR_factor_gt          0.0787
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.049
_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 -0.10414(2) 0.29529(2) 0.22873(2) 0.02398(7) Uani 1 1 d . U . . .
F1 F 0.0221(2) 0.24998(14) 0.61833(10) 0.0627(5) Uani 1 1 d . . . . .
F2 F -0.09726(16) 0.16480(14) 0.55223(11) 0.0553(4) Uani 1 1 d . . . . .
F3 F 0.1371(2) 0.04756(14) 0.44551(15) 0.0752(5) Uani 1 1 d . . . . .
F4 F 0.1410(2) 0.03637(17) 0.59935(17) 0.0933(7) Uani 1 1 d . . . . .
F5 F 0.25863(18) 0.12503(16) 0.51794(18) 0.0818(6) Uani 1 1 d . . . . .
O1 O 0.03897(16) 0.37036(12) 0.25453(10) 0.0333(3) Uani 1 1 d . U . . .
O2 O -0.07217(17) 0.25140(14) 0.38999(11) 0.0389(4) Uani 1 1 d . U . . .
O3 O -0.10719(16) 0.33463(12) 0.11273(10) 0.0332(3) Uani 1 1 d . U . . .
O4 O 0.04878(18) 0.16359(14) 0.21825(14) 0.0489(4) Uani 1 1 d . U . . .
O5 O -0.08698(17) 0.14895(13) 0.21930(12) 0.0413(4) Uani 1 1 d . U . . .
O6 O -0.24924(18) 0.41306(14) 0.29274(13) 0.0452(4) Uani 1 1 d . U . . .
O7 O -0.29686(15) 0.32399(13) 0.27107(11) 0.0376(3) Uani 1 1 d . U . . .
N1 N 0.17640(18) 0.44296(14) 0.33304(12) 0.0290(4) Uani 1 1 d . . . . .
N2 N 0.22364(19) 0.44528(15) 0.42401(13) 0.0339(4) Uani 1 1 d . . . . .
C1 C 0.1661(2) 0.38742(17) 0.48058(15) 0.0311(4) Uani 1 1 d . . . . .
C2 C 0.0788(2) 0.34384(16) 0.42855(14) 0.0279(4) Uani 1 1 d . . . . .
C3 C 0.0898(2) 0.38422(16) 0.33289(14) 0.0261(4) Uani 1 1 d . . . . .
C4 C 0.1932(3) 0.3826(2) 0.58526(16) 0.0424(5) Uani 1 1 d . . . . .
H4A H 0.247285 0.429960 0.596766 0.064 Uiso 1 1 calc R U . . .
H4B H 0.245899 0.310112 0.601639 0.064 Uiso 1 1 calc R U . . .
H4C H 0.104179 0.404708 0.625787 0.064 Uiso 1 1 calc R U . . .
C5 C 0.0027(2) 0.27163(17) 0.44689(15) 0.0311(4) Uani 1 1 d . . . . .
C6 C 0.0162(3) 0.1995(2) 0.53688(17) 0.0407(5) Uani 1 1 d . . . . .
C7 C 0.1417(3) 0.0993(2) 0.5237(2) 0.0559(7) Uani 1 1 d . . . . .
C8 C 0.2366(2) 0.48638(16) 0.25146(15) 0.0285(4) Uani 1 1 d . . . . .
C9 C 0.3803(2) 0.46308(17) 0.23802(17) 0.0339(5) Uani 1 1 d . . . . .
H9 H 0.437108 0.421200 0.284007 0.041 Uiso 1 1 calc R U . . .
C10 C 0.4403(3) 0.50080(19) 0.15790(19) 0.0424(5) Uani 1 1 d . . . . .
H10 H 0.538873 0.483801 0.147551 0.051 Uiso 1 1 calc R U . . .
C11 C 0.3567(3) 0.5636(2) 0.09233(18) 0.0461(6) Uani 1 1 d . . . . .
H11 H 0.398063 0.589880 0.036990 0.055 Uiso 1 1 calc R U . . .
C12 C 0.2132(3) 0.5883(2) 0.10694(17) 0.0451(6) Uani 1 1 d . . . . .
H12 H 0.156616 0.632081 0.061846 0.054 Uiso 1 1 calc R U . . .
C13 C 0.1514(2) 0.54996(19) 0.18668(16) 0.0377(5) Uani 1 1 d . . . . .
H13 H 0.052784 0.566725 0.196865 0.045 Uiso 1 1 calc R U . . .
P1 P 0.46118(5) 0.85124(4) 0.20790(3) 0.02426(12) Uani 1 1 d . . . . .
C14 C 0.4382(2) 0.79602(17) 0.32478(14) 0.0286(4) Uani 1 1 d . . . . .
C15 C 0.3974(2) 0.70495(19) 0.33212(16) 0.0371(5) Uani 1 1 d . . . . .
H15 H 0.376906 0.675631 0.275839 0.045 Uiso 1 1 calc R U . . .
C16 C 0.3867(3) 0.6573(2) 0.42108(18) 0.0452(6) Uani 1 1 d . . . . .
H16 H 0.361019 0.594455 0.425793 0.054 Uiso 1 1 calc R U . . .
C17 C 0.4136(3) 0.7014(2) 0.50273(18) 0.0498(7) Uani 1 1 d . . . . .
H17 H 0.405692 0.669040 0.563960 0.060 Uiso 1 1 calc R U . . .
C18 C 0.4516(3) 0.7919(3) 0.49617(17) 0.0519(7) Uani 1 1 d . . . . .
H18 H 0.469419 0.821608 0.553169 0.062 Uiso 1 1 calc R U . . .
C19 C 0.4645(2) 0.8406(2) 0.40768(16) 0.0375(5) Uani 1 1 d . . . . .
H19 H 0.490856 0.903185 0.403733 0.045 Uiso 1 1 calc R U . . .
C20 C 0.6159(2) 0.77003(16) 0.13953(14) 0.0270(4) Uani 1 1 d . . . . .
C21 C 0.6716(2) 0.66322(17) 0.16052(16) 0.0331(5) Uani 1 1 d . . . . .
H21 H 0.633004 0.633371 0.214822 0.040 Uiso 1 1 calc R U . . .
C22 C 0.7842(3) 0.60067(19) 0.1012(2) 0.0452(6) Uani 1 1 d . . . . .
H22 H 0.821970 0.527511 0.114619 0.054 Uiso 1 1 calc R U . . .
C23 C 0.8416(2) 0.64432(19) 0.02284(19) 0.0436(6) Uani 1 1 d . . . . .
H23 H 0.917897 0.600795 -0.017686 0.052 Uiso 1 1 calc R U . . .
C24 C 0.7885(2) 0.7509(2) 0.00311(17) 0.0395(5) Uani 1 1 d . . . . .
H24 H 0.829516 0.780778 -0.050041 0.047 Uiso 1 1 calc R U . . .
C25 C 0.6756(2) 0.81400(17) 0.06095(16) 0.0348(5) Uani 1 1 d . . . . .
H25 H 0.638638 0.887163 0.047289 0.042 Uiso 1 1 calc R U . . .
C26 C 0.4819(2) 0.97933(16) 0.21899(14) 0.0275(4) Uani 1 1 d . . . . .
C27 C 0.6103(2) 0.98678(18) 0.24074(16) 0.0348(5) Uani 1 1 d . . . . .
H27 H 0.685266 0.924447 0.249949 0.042 Uiso 1 1 calc R U . . .
C28 C 0.6283(3) 1.08469(19) 0.24888(18) 0.0399(5) Uani 1 1 d . . . . .
H28 H 0.715266 1.089960 0.264275 0.048 Uiso 1 1 calc R U . . .
C29 C 0.5187(3) 1.17541(19) 0.23443(18) 0.0418(5) Uani 1 1 d . . . . .
H29 H 0.531475 1.242808 0.238557 0.050 Uiso 1 1 calc R U . . .
C30 C 0.3914(3) 1.16824(19) 0.21415(19) 0.0447(6) Uani 1 1 d . . . . .
H30 H 0.316508 1.230856 0.205789 0.054 Uiso 1 1 calc R U . . .
C31 C 0.3718(2) 1.07074(18) 0.20585(17) 0.0359(5) Uani 1 1 d . . . . .
H31 H 0.284129 1.066132 0.191333 0.043 Uiso 1 1 calc R U . . .
C32 C 0.3117(2) 0.86084(16) 0.14402(15) 0.0291(4) Uani 1 1 d . . . . .
C33 C 0.1801(2) 0.8887(2) 0.19508(18) 0.0415(5) Uani 1 1 d . . . . .
H33 H 0.169457 0.901001 0.262973 0.050 Uiso 1 1 calc R U . . .
C34 C 0.0643(3) 0.8980(2) 0.1450(2) 0.0534(7) Uani 1 1 d . . . . .
H34 H -0.026290 0.917781 0.178660 0.064 Uiso 1 1 calc R U . . .
C35 C 0.0809(3) 0.8787(2) 0.0465(2) 0.0548(7) Uani 1 1 d . . . . .
H35 H 0.001549 0.883984 0.013051 0.066 Uiso 1 1 calc R U . . .
C36 C 0.2102(3) 0.8522(2) -0.0033(2) 0.0541(7) Uani 1 1 d . . . . .
H36 H 0.220105 0.840135 -0.071191 0.065 Uiso 1 1 calc R U . . .
C37 C 0.3274(3) 0.8427(2) 0.04497(17) 0.0410(5) Uani 1 1 d . . . . .
H37 H 0.417353 0.824009 0.010421 0.049 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 O3 1.6795(14) . ?
Mo1 O7 1.9043(15) . ?
Mo1 O5 1.9087(16) . ?
Mo1 O4 1.9424(17) . ?
Mo1 O6 1.9465(17) . ?
Mo1 O1 2.0625(14) . ?
Mo1 O2 2.3249(15) . ?
F1 C6 1.345(3) . ?
F2 C6 1.364(3) . ?
F3 C7 1.311(4) . ?
F4 C7 1.327(3) . ?
F5 C7 1.327(3) . ?
O1 C3 1.288(2) . ?
O2 C5 1.236(3) . ?
O4 O5 1.447(2) . ?
O6 O7 1.461(2) . ?
N1 C3 1.345(3) . ?
N1 N2 1.397(2) . ?
N1 C8 1.428(3) . ?
N2 C1 1.308(3) . ?
C1 C2 1.451(3) . ?
C1 C4 1.500(3) . ?
C2 C5 1.412(3) . ?
C2 C3 1.426(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.546(3) . ?
C6 C7 1.530(4) . ?
C8 C9 1.385(3) . ?
C8 C13 1.388(3) . ?
C9 C10 1.374(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.383(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
P1 C14 1.788(2) . ?
P1 C26 1.795(2) . ?
P1 C32 1.797(2) . ?
P1 C20 1.798(2) . ?
C14 C19 1.393(3) . ?
C14 C15 1.397(3) . ?
C15 C16 1.383(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.376(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.374(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.388(3) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.392(3) . ?
C20 C25 1.399(3) . ?
C21 C22 1.390(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.383(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.383(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.384(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C31 1.394(3) . ?
C26 C27 1.397(3) . ?
C27 C28 1.381(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.388(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.378(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.383(3) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C37 1.386(3) . ?
C32 C33 1.392(3) . ?
C33 C34 1.391(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.381(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.366(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.389(3) . ?
C36 H36 0.9500 . ?
C37 H37 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
O3 Mo1 O7 102.84(7) . . ?
O3 Mo1 O5 102.93(7) . . ?
O7 Mo1 O5 89.21(7) . . ?
O3 Mo1 O4 101.23(8) . . ?
O7 Mo1 O4 131.28(7) . . ?
O5 Mo1 O4 44.12(7) . . ?
O3 Mo1 O6 101.31(8) . . ?
O7 Mo1 O6 44.57(7) . . ?
O5 Mo1 O6 131.59(7) . . ?
O4 Mo1 O6 157.28(8) . . ?
O3 Mo1 O1 92.21(6) . . ?
O7 Mo1 O1 132.27(7) . . ?
O5 Mo1 O1 131.41(7) . . ?
O4 Mo1 O1 87.94(7) . . ?
O6 Mo1 O1 88.34(7) . . ?
O3 Mo1 O2 171.30(6) . . ?
O7 Mo1 O2 84.06(6) . . ?
O5 Mo1 O2 82.25(7) . . ?
O4 Mo1 O2 77.51(7) . . ?
O6 Mo1 O2 79.78(7) . . ?
O1 Mo1 O2 79.17(5) . . ?
C3 O1 Mo1 131.63(13) . . ?
C5 O2 Mo1 132.38(14) . . ?
O5 O4 Mo1 66.70(9) . . ?
O4 O5 Mo1 69.17(10) . . ?
O7 O6 Mo1 66.19(9) . . ?
O6 O7 Mo1 69.25(9) . . ?
C3 N1 N2 112.04(16) . . ?
C3 N1 C8 127.64(17) . . ?
N2 N1 C8 119.61(16) . . ?
C1 N2 N1 106.11(17) . . ?
N2 C1 C2 111.36(18) . . ?
N2 C1 C4 116.72(19) . . ?
C2 C1 C4 131.8(2) . . ?
C5 C2 C3 118.62(18) . . ?
C5 C2 C1 137.33(19) . . ?
C3 C2 C1 103.82(18) . . ?
O1 C3 N1 120.87(18) . . ?
O1 C3 C2 132.39(19) . . ?
N1 C3 C2 106.67(17) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O2 C5 C2 124.71(19) . . ?
O2 C5 C6 111.69(19) . . ?
C2 C5 C6 123.31(19) . . ?
F1 C6 F2 106.6(2) . . ?
F1 C6 C7 109.6(2) . . ?
F2 C6 C7 105.2(2) . . ?
F1 C6 C5 112.6(2) . . ?
F2 C6 C5 109.99(18) . . ?
C7 C6 C5 112.5(2) . . ?
F3 C7 F4 108.3(3) . . ?
F3 C7 F5 110.1(3) . . ?
F4 C7 F5 108.4(2) . . ?
F3 C7 C6 110.8(2) . . ?
F4 C7 C6 109.8(3) . . ?
F5 C7 C6 109.5(2) . . ?
C9 C8 C13 121.1(2) . . ?
C9 C8 N1 118.97(19) . . ?
C13 C8 N1 119.92(19) . . ?
C10 C9 C8 119.7(2) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 119.8(2) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 120.3(2) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.6(2) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C8 118.5(2) . . ?
C12 C13 H13 120.8 . . ?
C8 C13 H13 120.8 . . ?
C14 P1 C26 110.60(10) . . ?
C14 P1 C32 108.83(10) . . ?
C26 P1 C32 110.18(9) . . ?
C14 P1 C20 110.89(9) . . ?
C26 P1 C20 106.93(10) . . ?
C32 P1 C20 109.41(10) . . ?
C19 C14 C15 119.9(2) . . ?
C19 C14 P1 120.95(17) . . ?
C15 C14 P1 119.16(16) . . ?
C16 C15 C14 120.2(2) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C17 C16 C15 119.7(2) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C18 C17 C16 120.4(2) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C19 121.1(2) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
C18 C19 C14 118.8(2) . . ?
C18 C19 H19 120.6 . . ?
C14 C19 H19 120.6 . . ?
C21 C20 C25 119.99(19) . . ?
C21 C20 P1 120.77(16) . . ?
C25 C20 P1 119.14(16) . . ?
C22 C21 C20 119.3(2) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C23 C22 C21 120.4(2) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C24 C23 C22 120.4(2) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 119.9(2) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C24 C25 C20 120.0(2) . . ?
C24 C25 H25 120.0 . . ?
C20 C25 H25 120.0 . . ?
C31 C26 C27 120.0(2) . . ?
C31 C26 P1 120.70(16) . . ?
C27 C26 P1 119.29(16) . . ?
C28 C27 C26 120.0(2) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 119.7(2) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C30 C29 C28 120.4(2) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 C31 120.6(2) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C30 C31 C26 119.3(2) . . ?
C30 C31 H31 120.3 . . ?
C26 C31 H31 120.3 . . ?
C37 C32 C33 120.6(2) . . ?
C37 C32 P1 120.27(17) . . ?
C33 C32 P1 119.09(16) . . ?
C34 C33 C32 118.9(2) . . ?
C34 C33 H33 120.6 . . ?
C32 C33 H33 120.6 . . ?
C35 C34 C33 120.2(3) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C36 C35 C34 120.7(2) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C35 C36 C37 120.3(3) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C32 C37 C36 119.4(2) . . ?
C32 C37 H37 120.3 . . ?
C36 C37 H37 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 N2 C1 0.1(2) . . . . ?
C8 N1 N2 C1 -170.95(18) . . . . ?
N1 N2 C1 C2 0.4(2) . . . . ?
N1 N2 C1 C4 -176.21(18) . . . . ?
N2 C1 C2 C5 173.4(2) . . . . ?
C4 C1 C2 C5 -10.7(4) . . . . ?
N2 C1 C2 C3 -0.7(2) . . . . ?
C4 C1 C2 C3 175.2(2) . . . . ?
Mo1 O1 C3 N1 -175.42(14) . . . . ?
Mo1 O1 C3 C2 8.0(3) . . . . ?
N2 N1 C3 O1 -177.94(18) . . . . ?
C8 N1 C3 O1 -7.8(3) . . . . ?
N2 N1 C3 C2 -0.5(2) . . . . ?
C8 N1 C3 C2 169.62(19) . . . . ?
C5 C2 C3 O1 2.2(3) . . . . ?
C1 C2 C3 O1 177.7(2) . . . . ?
C5 C2 C3 N1 -174.74(18) . . . . ?
C1 C2 C3 N1 0.7(2) . . . . ?
Mo1 O2 C5 C2 9.5(3) . . . . ?
Mo1 O2 C5 C6 -164.37(15) . . . . ?
C3 C2 C5 O2 -10.7(3) . . . . ?
C1 C2 C5 O2 175.8(2) . . . . ?
C3 C2 C5 C6 162.5(2) . . . . ?
C1 C2 C5 C6 -11.0(4) . . . . ?
O2 C5 C6 F1 -144.1(2) . . . . ?
C2 C5 C6 F1 41.8(3) . . . . ?
O2 C5 C6 F2 -25.5(3) . . . . ?
C2 C5 C6 F2 160.5(2) . . . . ?
O2 C5 C6 C7 91.4(2) . . . . ?
C2 C5 C6 C7 -82.6(3) . . . . ?
F1 C6 C7 F3 178.9(2) . . . . ?
F2 C6 C7 F3 64.7(3) . . . . ?
C5 C6 C7 F3 -55.0(3) . . . . ?
F1 C6 C7 F4 59.4(3) . . . . ?
F2 C6 C7 F4 -54.9(3) . . . . ?
C5 C6 C7 F4 -174.6(2) . . . . ?
F1 C6 C7 F5 -59.6(3) . . . . ?
F2 C6 C7 F5 -173.8(2) . . . . ?
C5 C6 C7 F5 66.5(3) . . . . ?
C3 N1 C8 C9 -124.6(2) . . . . ?
N2 N1 C8 C9 44.9(3) . . . . ?
C3 N1 C8 C13 54.7(3) . . . . ?
N2 N1 C8 C13 -135.7(2) . . . . ?
C13 C8 C9 C10 -1.9(3) . . . . ?
N1 C8 C9 C10 177.46(19) . . . . ?
C8 C9 C10 C11 1.4(3) . . . . ?
C9 C10 C11 C12 -0.2(4) . . . . ?
C10 C11 C12 C13 -0.6(4) . . . . ?
C11 C12 C13 C8 0.1(4) . . . . ?
C9 C8 C13 C12 1.1(3) . . . . ?
N1 C8 C13 C12 -178.2(2) . . . . ?
C26 P1 C14 C19 -12.5(2) . . . . ?
C32 P1 C14 C19 -133.70(18) . . . . ?
C20 P1 C14 C19 105.92(18) . . . . ?
C26 P1 C14 C15 169.46(17) . . . . ?
C32 P1 C14 C15 48.3(2) . . . . ?
C20 P1 C14 C15 -72.09(19) . . . . ?
C19 C14 C15 C16 -1.8(3) . . . . ?
P1 C14 C15 C16 176.27(18) . . . . ?
C14 C15 C16 C17 1.4(4) . . . . ?
C15 C16 C17 C18 -0.4(4) . . . . ?
C16 C17 C18 C19 -0.3(4) . . . . ?
C17 C18 C19 C14 0.0(4) . . . . ?
C15 C14 C19 C18 1.0(3) . . . . ?
P1 C14 C19 C18 -176.94(18) . . . . ?
C14 P1 C20 C21 23.4(2) . . . . ?
C26 P1 C20 C21 144.09(17) . . . . ?
C32 P1 C20 C21 -96.60(18) . . . . ?
C14 P1 C20 C25 -160.26(17) . . . . ?
C26 P1 C20 C25 -39.61(19) . . . . ?
C32 P1 C20 C25 79.70(19) . . . . ?
C25 C20 C21 C22 -1.7(3) . . . . ?
P1 C20 C21 C22 174.58(18) . . . . ?
C20 C21 C22 C23 0.8(4) . . . . ?
C21 C22 C23 C24 0.7(4) . . . . ?
C22 C23 C24 C25 -1.3(4) . . . . ?
C23 C24 C25 C20 0.4(4) . . . . ?
C21 C20 C25 C24 1.1(3) . . . . ?
P1 C20 C25 C24 -175.23(18) . . . . ?
C14 P1 C26 C31 -102.51(19) . . . . ?
C32 P1 C26 C31 17.8(2) . . . . ?
C20 P1 C26 C31 136.65(18) . . . . ?
C14 P1 C26 C27 77.69(19) . . . . ?
C32 P1 C26 C27 -161.95(17) . . . . ?
C20 P1 C26 C27 -43.14(19) . . . . ?
C31 C26 C27 C28 -0.2(3) . . . . ?
P1 C26 C27 C28 179.55(18) . . . . ?
C26 C27 C28 C29 -0.6(4) . . . . ?
C27 C28 C29 C30 1.4(4) . . . . ?
C28 C29 C30 C31 -1.4(4) . . . . ?
C29 C30 C31 C26 0.5(4) . . . . ?
C27 C26 C31 C30 0.3(3) . . . . ?
P1 C26 C31 C30 -179.50(19) . . . . ?
C14 P1 C32 C37 -143.61(18) . . . . ?
C26 P1 C32 C37 94.98(19) . . . . ?
C20 P1 C32 C37 -22.3(2) . . . . ?
C14 P1 C32 C33 37.6(2) . . . . ?
C26 P1 C32 C33 -83.8(2) . . . . ?
C20 P1 C32 C33 158.90(18) . . . . ?
C37 C32 C33 C34 0.0(4) . . . . ?
P1 C32 C33 C34 178.74(19) . . . . ?
C32 C33 C34 C35 0.8(4) . . . . ?
C33 C34 C35 C36 -1.2(4) . . . . ?
C34 C35 C36 C37 0.9(4) . . . . ?
C33 C32 C37 C36 -0.2(4) . . . . ?
P1 C32 C37 C36 -178.99(19) . . . . ?
C35 C36 C37 C32 -0.2(4) . . . . ?

_refine_diff_density_max         0.935
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.061


#==============================================================================0
# start Validation Reply Form



_vrf_PLAT232_2                   
;
PROBLEM:
Alert level B
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X)  Mo1    --  O6      ..     11.4 s.u.

RESPONSE: 
We believe that this effect is due to either uncorrected absorption effects 
or limited substitutional disorder of peroxido oxygen atoms. Attempts to model
these peroxido oxygen atoms over two or more distinct crystallographic positions 
did not lead to reasonable structural models. In view of crystal quality, the 
results of the refinement were satisfying. 
;
