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

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1013319'
_audit_update_record             
;
2015-04-22 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H10 Cl4 Mo N2 O 1-, C6 H16 N 1+'
_chemical_formula_sum            'C18 H26 Cl4 Mo N3 O'
_chemical_formula_weight         538.16

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   12.2120(7)
_cell_length_b                   11.9077(7)
_cell_length_c                   17.0761(9)
_cell_angle_alpha                90
_cell_angle_beta                 102.0140(9)
_cell_angle_gamma                90
_cell_volume                     2428.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5278
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      25.80

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow/brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_F_000             1092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.993
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            18535
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.100
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4758
_reflns_number_gt                3548
_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 SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_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)+(0.0735P)²+2.7809P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4758
_refine_ls_number_parameters     338
_refine_ls_number_restraints     305
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1372
_refine_ls_wR_factor_gt          0.1218
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.051
_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 0.31593(3) 0.61451(4) 0.38615(2) 0.03883(16) Uani 1 1 d D . . . .
Cl1 Cl 0.44833(10) 0.48567(9) 0.34139(6) 0.0386(3) Uani 1 1 d . . . . .
Cl2 Cl 0.48860(10) 0.71228(10) 0.45735(7) 0.0421(3) Uani 1 1 d . . . . .
Cl3 Cl 0.21193(13) 0.74071(14) 0.44702(9) 0.0393(4) Uani 0.805(4) 1 d D U P A 1
Cl4 Cl 0.31014(13) 0.72914(12) 0.27069(8) 0.0581(4) Uani 1 1 d . . . . .
N1 N 0.3464(3) 0.5156(4) 0.4989(3) 0.0388(9) Uani 1 1 d . . . . .
H1A H 0.381(4) 0.466(5) 0.492(3) 0.047 Uiso 1 1 d . U . . .
H1B H 0.394(4) 0.549(4) 0.532(3) 0.047 Uiso 1 1 d . U . . .
N2 N 0.2136(6) 0.5184(7) 0.3489(4) 0.0428(16) Uani 0.805(4) 1 d D U P A 1
C1 C 0.2520(4) 0.4850(4) 0.5329(3) 0.0392(10) Uani 1 1 d . . . . .
C2 C 0.2224(5) 0.5478(5) 0.5933(3) 0.0533(13) Uani 1 1 d . . . . .
H2 H 0.2669 0.6100 0.6156 0.064 Uiso 0.805(4) 1 calc R U P . .
C3 C 0.1270(5) 0.5192(6) 0.6214(3) 0.0649(16) Uani 1 1 d . . . . .
H3 H 0.1057 0.5632 0.6622 0.078 Uiso 1 1 calc R U . . .
C4 C 0.0641(5) 0.4294(5) 0.5912(3) 0.0592(15) Uani 1 1 d . . . . .
H4 H -0.0017 0.4119 0.6103 0.071 Uiso 1 1 calc R U . . .
C5 C 0.0943(5) 0.3641(5) 0.5339(4) 0.0623(16) Uani 1 1 d . . . . .
H5 H 0.0510 0.3000 0.5139 0.075 Uiso 1 1 calc R U . . .
C6 C 0.1896(4) 0.3917(4) 0.5044(3) 0.0472(12) Uani 1 1 d . . . . .
O1 O 0.2236(4) 0.3270(3) 0.4438(3) 0.0505(11) Uani 0.805(4) 1 d . U P A 1
C7 C 0.1475(5) 0.4248(7) 0.3210(4) 0.0461(13) Uani 0.805(4) 1 d D U P A 1
C8 C 0.1516(5) 0.3315(6) 0.3677(4) 0.0528(14) Uani 0.805(4) 1 d D U P A 1
C9 C 0.0858(7) 0.2370(7) 0.3365(5) 0.078(2) Uani 0.805(4) 1 d D U P A 1
H9 H 0.0873 0.1708 0.3677 0.093 Uiso 0.805(4) 1 calc R U P A 1
C10 C 0.0209(7) 0.2422(7) 0.2621(5) 0.079(2) Uani 0.805(4) 1 d D U P A 1
H10 H -0.0226 0.1785 0.2417 0.095 Uiso 0.805(4) 1 calc R U P A 1
C11 C 0.0155(7) 0.3346(8) 0.2154(5) 0.079(2) Uani 0.805(4) 1 d D U P A 1
H11 H -0.0318 0.3358 0.1637 0.095 Uiso 0.805(4) 1 calc R U P A 1
C12 C 0.0793(5) 0.4267(7) 0.2438(4) 0.0577(16) Uani 0.805(4) 1 d D U P A 1
H12 H 0.0774 0.4916 0.2112 0.069 Uiso 0.805(4) 1 calc R U P A 1
Cl3X Cl 0.1693(9) 0.5072(10) 0.3191(6) 0.064(3) Uani 0.195(4) 1 d D U P A -2
N2X N 0.227(3) 0.713(2) 0.418(2) 0.071(8) Uani 0.195(4) 1 d D U P A -2
O1X O 0.2464(17) 0.6827(17) 0.5791(11) 0.062(5) Uani 0.195(4) 1 d . U P A -2
C7X C 0.166(2) 0.794(2) 0.4668(14) 0.060(5) Uani 0.195(4) 1 d D U P A -2
C8X C 0.1808(17) 0.7735(17) 0.5480(13) 0.057(5) Uani 0.195(4) 1 d D U P A -2
C9X C 0.1301(16) 0.8419(17) 0.5982(13) 0.046(5) Uani 0.195(4) 1 d D U P A -2
H9X H 0.1496 0.8332 0.6547 0.056 Uiso 0.195(4) 1 calc R U P A -2
C10X C 0.0537(17) 0.9198(18) 0.5651(12) 0.049(5) Uani 0.195(4) 1 d D U P A -2
H10X H 0.0027 0.9485 0.5952 0.058 Uiso 0.195(4) 1 calc R U P A -2
C11X C 0.049(2) 0.957(2) 0.4900(14) 0.062(6) Uani 0.195(4) 1 d D U P A -2
H11X H 0.0109 1.0249 0.4718 0.074 Uiso 0.195(4) 1 calc R U P A -2
C12X C 0.102(3) 0.892(2) 0.4386(15) 0.074(7) Uani 0.195(4) 1 d D U P A -2
H12X H 0.0953 0.9139 0.3843 0.088 Uiso 0.195(4) 1 calc R U P A -2
N3 N 0.5081(5) 0.5953(3) 0.1827(3) 0.0608(14) Uani 1 1 d . . . . .
H3A H 0.479(5) 0.572(5) 0.227(4) 0.073 Uiso 1 1 d . U . . .
C13 C 0.4128(7) 0.6000(5) 0.1106(3) 0.076(2) Uani 1 1 d . . . . .
H13A H 0.4439 0.6086 0.0619 0.091 Uiso 1 1 calc R U . . .
H13B H 0.3665 0.6670 0.1150 0.091 Uiso 1 1 calc R U . . .
C14 C 0.3379(9) 0.4959(7) 0.1014(4) 0.115(3) Uani 1 1 d . . . . .
H14A H 0.3832 0.4289 0.0976 0.173 Uiso 1 1 calc R U . . .
H14B H 0.2796 0.5028 0.0526 0.173 Uiso 1 1 calc R U . . .
H14C H 0.3030 0.4892 0.1479 0.173 Uiso 1 1 calc R U . . .
C15 C 0.5863(7) 0.4978(5) 0.1830(4) 0.079(2) Uani 1 1 d . . . . .
H15A H 0.5428 0.4270 0.1767 0.095 Uiso 1 1 calc R U . . .
H15B H 0.6400 0.4950 0.2351 0.095 Uiso 1 1 calc R U . . .
C16 C 0.6505(8) 0.5074(6) 0.1157(5) 0.096(3) Uani 1 1 d . . . . .
H16A H 0.5985 0.5270 0.0657 0.144 Uiso 1 1 calc R U . . .
H16B H 0.6865 0.4355 0.1093 0.144 Uiso 1 1 calc R U . . .
H16C H 0.7077 0.5660 0.1290 0.144 Uiso 1 1 calc R U . . .
C17 C 0.5664(5) 0.7070(4) 0.1951(3) 0.0599(15) Uani 1 1 d . . . . .
H17A H 0.6023 0.7220 0.1493 0.072 Uiso 1 1 calc R U . . .
H17B H 0.5099 0.7664 0.1958 0.072 Uiso 1 1 calc R U . . .
C18 C 0.6537(6) 0.7138(5) 0.2712(4) 0.0695(17) Uani 1 1 d . . . . .
H18A H 0.6192 0.6982 0.3169 0.104 Uiso 1 1 calc R U . . .
H18B H 0.6864 0.7893 0.2766 0.104 Uiso 1 1 calc R U . . .
H18C H 0.7126 0.6584 0.2696 0.104 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 N2 1.717(7) . ?
Mo1 N2X 1.759(18) . ?
Mo1 N1 2.222(4) . ?
Mo1 Cl3X 2.302(11) . ?
Mo1 Cl3 2.3454(18) . ?
Mo1 Cl4 2.3869(13) . ?
Mo1 Cl1 2.4631(12) . ?
Mo1 Cl2 2.4926(12) . ?
N1 C1 1.442(6) . ?
N1 H1A 0.75(5) . ?
N1 H1B 0.82(5) . ?
N2 C7 1.400(9) . ?
C1 C6 1.378(7) . ?
C1 C2 1.381(7) . ?
C2 C3 1.391(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.354(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.361(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.400(7) . ?
C5 H5 0.9500 . ?
C6 O1 1.419(6) . ?
O1 C8 1.409(8) . ?
C7 C8 1.363(11) . ?
C7 C12 1.405(9) . ?
C8 C9 1.420(8) . ?
C9 C10 1.352(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.351(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.374(9) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N2X C7X 1.56(3) . ?
O1X C8X 1.38(3) . ?
C7X C8X 1.383(19) . ?
C7X C12X 1.427(19) . ?
C8X C9X 1.414(16) . ?
C9X C10X 1.354(16) . ?
C9X H9X 0.9500 . ?
C10X C11X 1.346(16) . ?
C10X H10X 0.9500 . ?
C11X C12X 1.430(16) . ?
C11X H11X 0.9500 . ?
C12X H12X 0.9500 . ?
N3 C17 1.503(7) . ?
N3 C15 1.503(7) . ?
N3 C13 1.509(9) . ?
N3 H3A 0.93(6) . ?
C13 C14 1.528(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.523(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.501(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Mo1 N1 86.9(3) . . ?
N2X Mo1 N1 95.1(10) . . ?
N2X Mo1 Cl3X 93.3(13) . . ?
N1 Mo1 Cl3X 96.3(3) . . ?
N2 Mo1 Cl3 99.9(3) . . ?
N1 Mo1 Cl3 87.94(12) . . ?
N2 Mo1 Cl4 100.4(3) . . ?
N2X Mo1 Cl4 87.6(10) . . ?
N1 Mo1 Cl4 171.87(11) . . ?
Cl3X Mo1 Cl4 91.2(3) . . ?
Cl3 Mo1 Cl4 94.24(5) . . ?
N2 Mo1 Cl1 86.8(3) . . ?
N2X Mo1 Cl1 176.6(11) . . ?
N1 Mo1 Cl1 86.36(11) . . ?
Cl3X Mo1 Cl1 89.6(3) . . ?
Cl3 Mo1 Cl1 170.96(5) . . ?
Cl4 Mo1 Cl1 90.48(4) . . ?
N2 Mo1 Cl2 165.7(3) . . ?
N2X Mo1 Cl2 93.0(13) . . ?
N1 Mo1 Cl2 81.53(11) . . ?
Cl3X Mo1 Cl2 173.5(3) . . ?
Cl3 Mo1 Cl2 88.03(5) . . ?
Cl4 Mo1 Cl2 90.71(5) . . ?
Cl1 Mo1 Cl2 84.20(4) . . ?
C1 N1 Mo1 118.6(3) . . ?
C1 N1 H1A 113(4) . . ?
Mo1 N1 H1A 106(4) . . ?
C1 N1 H1B 110(4) . . ?
Mo1 N1 H1B 108(4) . . ?
H1A N1 H1B 99(5) . . ?
C7 N2 Mo1 168.7(6) . . ?
C6 C1 C2 119.3(4) . . ?
C6 C1 N1 119.4(4) . . ?
C2 C1 N1 121.3(4) . . ?
C1 C2 C3 119.6(5) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 120.7(5) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 120.5(5) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 119.7(5) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 120.1(5) . . ?
C1 C6 O1 118.2(4) . . ?
C5 C6 O1 121.7(5) . . ?
C8 O1 C6 115.5(5) . . ?
C8 C7 N2 120.1(6) . . ?
C8 C7 C12 120.3(6) . . ?
N2 C7 C12 119.6(7) . . ?
C7 C8 O1 120.7(5) . . ?
C7 C8 C9 118.5(7) . . ?
O1 C8 C9 120.8(7) . . ?
C10 C9 C8 119.4(8) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C11 C10 C9 122.6(7) . . ?
C11 C10 H10 118.7 . . ?
C9 C10 H10 118.7 . . ?
C10 C11 C12 119.2(8) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
C11 C12 C7 120.0(8) . . ?
C11 C12 H12 120.0 . . ?
C7 C12 H12 120.0 . . ?
C7X N2X Mo1 166(3) . . ?
C8X C7X C12X 115.6(19) . . ?
C8X C7X N2X 117(2) . . ?
C12X C7X N2X 128(2) . . ?
C7X C8X O1X 117.8(18) . . ?
C7X C8X C9X 121.6(18) . . ?
O1X C8X C9X 120.6(18) . . ?
C10X C9X C8X 119.5(17) . . ?
C10X C9X H9X 120.3 . . ?
C8X C9X H9X 120.3 . . ?
C11X C10X C9X 120.9(18) . . ?
C11X C10X H10X 119.5 . . ?
C9X C10X H10X 119.5 . . ?
C10X C11X C12X 118.0(18) . . ?
C10X C11X H11X 121.0 . . ?
C12X C11X H11X 121.0 . . ?
C7X C12X C11X 121.6(18) . . ?
C7X C12X H12X 119.2 . . ?
C11X C12X H12X 119.2 . . ?
C17 N3 C15 113.6(5) . . ?
C17 N3 C13 110.2(4) . . ?
C15 N3 C13 114.4(5) . . ?
C17 N3 H3A 113(4) . . ?
C15 N3 H3A 96(4) . . ?
C13 N3 H3A 108(4) . . ?
N3 C13 C14 113.4(5) . . ?
N3 C13 H13A 108.9 . . ?
C14 C13 H13A 108.9 . . ?
N3 C13 H13B 108.9 . . ?
C14 C13 H13B 108.9 . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 C16 111.5(5) . . ?
N3 C15 H15A 109.3 . . ?
C16 C15 H15A 109.3 . . ?
N3 C15 H15B 109.3 . . ?
C16 C15 H15B 109.3 . . ?
H15A C15 H15B 108.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N3 113.6(5) . . ?
C18 C17 H17A 108.8 . . ?
N3 C17 H17A 108.8 . . ?
C18 C17 H17B 108.8 . . ?
N3 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2X Mo1 N2_a C7_a -156(3) . . . . ?
N1 Mo1 N2 C7 -62(3) . . . . ?
Cl3X Mo1 N2 C7 132(5) . . . . ?
Cl3 Mo1 N2 C7 -149(3) . . . . ?
Cl4 Mo1 N2 C7 115(3) . . . . ?
Cl1 Mo1 N2 C7 25(3) . . . . ?
Cl2 Mo1 N2 C7 -26(4) . . . . ?
Mo1 N1 C1 C6 82.9(5) . . . . ?
Mo1 N1 C1 C2 -96.8(5) . . . . ?
C6 C1 C2 C3 -3.3(8) . . . . ?
N1 C1 C2 C3 176.4(5) . . . . ?
C1 C2 C3 C4 1.2(9) . . . . ?
C2 C3 C4 C5 1.3(10) . . . . ?
C3 C4 C5 C6 -1.7(9) . . . . ?
C2 C1 C6 C5 2.9(8) . . . . ?
N1 C1 C6 C5 -176.8(5) . . . . ?
C2 C1 C6 O1 -178.4(5) . . . . ?
N1 C1 C6 O1 2.0(7) . . . . ?
C4 C5 C6 C1 -0.4(9) . . . . ?
C4 C5 C6 O1 -179.1(5) . . . . ?
C1 C6 O1 C8 -111.0(6) . . . . ?
C5 C6 O1 C8 67.7(7) . . . . ?
Mo1 N2 C7 C8 54(3) . . . . ?
Mo1 N2 C7 C12 -125(3) . . . . ?
N2 C7 C8 O1 -1.2(9) . . . . ?
C12 C7 C8 O1 177.1(5) . . . . ?
N2 C7 C8 C9 -178.2(7) . . . . ?
C12 C7 C8 C9 0.1(9) . . . . ?
C6 O1 C8 C7 73.9(7) . . . . ?
C6 O1 C8 C9 -109.2(6) . . . . ?
C7 C8 C9 C10 -0.3(11) . . . . ?
O1 C8 C9 C10 -177.3(7) . . . . ?
C8 C9 C10 C11 -0.2(12) . . . . ?
C9 C10 C11 C12 0.9(13) . . . . ?
C10 C11 C12 C7 -1.2(11) . . . . ?
C8 C7 C12 C11 0.7(10) . . . . ?
N2 C7 C12 C11 179.0(7) . . . . ?
N2 Mo1 N2X C7X 117(10) . . . . ?
N1 Mo1 N2X C7X 30(11) . . . . ?
Cl3X Mo1 N2X C7X 127(10) . . . . ?
Cl3 Mo1 N2X C7X 1(4) . . . . ?
Cl4 Mo1 N2X C7X -142(10) . . . . ?
Cl2 Mo1 N2X C7X -52(10) . . . . ?
Mo1 N2X C7X C8X -20(11) . . . . ?
Mo1 N2X C7X C12X 156(9) . . . . ?
C12X C7X C8X O1X -177(2) . . . . ?
N2X C7X C8X O1X -1(3) . . . . ?
C12X C7X C8X C9X 3.4(19) . . . . ?
N2X C7X C8X C9X 180(2) . . . . ?
C7X C8X C9X C10X 9.1(18) . . . . ?
O1X C8X C9X C10X -170(2) . . . . ?
C8X C9X C10X C11X -20(3) . . . . ?
C9X C10X C11X C12X 18(4) . . . . ?
C8X C7X C12X C11X -6(3) . . . . ?
N2X C7X C12X C11X 179(3) . . . . ?
C10X C11X C12X C7X -4(4) . . . . ?
C17 N3 C13 C14 -171.0(6) . . . . ?
C15 N3 C13 C14 59.5(8) . . . . ?
C17 N3 C15 C16 -61.3(8) . . . . ?
C13 N3 C15 C16 66.5(8) . . . . ?
C15 N3 C17 C18 -56.9(6) . . . . ?
C13 N3 C17 C18 173.2(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Cl2 0.75(5) 2.69(5) 3.370(5) 152(5) 3_666
N1 H1A Cl1 0.75(5) 2.86(5) 3.211(4) 111(5) .
N1 H1B Cl1 0.82(5) 2.61(5) 3.297(4) 142(5) 3_666
N3 H3A Cl1 0.93(6) 2.31(6) 3.225(4) 165(5) .
N3 H3A Cl4 0.93(6) 3.00(6) 3.486(5) 114(4) .

_refine_diff_density_max         0.947
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.102

_shelxl_version_number           2014-3

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_3.2MeCN
_database_code_depnum_ccdc_archive 'CCDC 1013320'
_audit_update_record             
;
2015-04-22 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H72 Cl3 Mo4 N11 O6 Si, 2(C2 H3 N)'
_chemical_formula_sum            'C67 H78 Cl3 Mo4 N13 O6 Si'
_chemical_formula_weight         1679.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cl Cl 0.1484 0.1585 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   12.7371(4)
_cell_length_b                   25.9749(8)
_cell_length_c                   24.2388(8)
_cell_angle_alpha                90
_cell_angle_beta                 100.0667(5)
_cell_angle_gamma                90
_cell_volume                     7895.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    32505
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      28.83

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red/purple'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_F_000             3408
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.790
_exptl_crystal_size_mid          0.610
_exptl_crystal_size_min          0.590
_exptl_absorpt_coefficient_mu    0.791
_shelx_estimated_absorpt_T_min   0.574
_shelx_estimated_absorpt_T_max   0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_process_details   'SADABS V2.03, SHELDRICK, G.M.'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            68759
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.785
_diffrn_reflns_theta_max         28.970
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             18926
_reflns_number_gt                14618
_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 SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_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)+(0.0382P)²+26.0973P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18926
_refine_ls_number_parameters     1017
_refine_ls_number_restraints     318
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1271
_refine_ls_wR_factor_gt          0.1100
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.156
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.37602(3) 0.68538(2) 0.41028(2) 0.03117(9) Uani 1 1 d . . . . .
Cl1 Cl 0.47977(8) 0.76127(6) 0.38799(4) 0.0469(3) Uani 1 1 d . . . . .
Mo2 Mo 0.12562(2) 0.65812(2) 0.38076(2) 0.02279(8) Uani 1 1 d . . . . .
Cl2 Cl 0.06631(7) 0.71517(4) 0.45372(4) 0.02756(19) Uani 1 1 d . . . . .
Mo3 Mo 0.26484(3) 0.66896(2) 0.27648(2) 0.03294(10) Uani 1 1 d . . . . .
Cl3 Cl 0.40974(8) 0.72215(6) 0.25030(4) 0.0484(3) Uani 1 1 d . . . . .
Mo4 Mo 0.12472(3) 0.76546(2) 0.31288(2) 0.02658(8) Uani 1 1 d . . . . .
O1 O 0.2390(2) 0.71382(12) 0.35252(10) 0.0282(6) Uani 1 1 d . . . . .
N1 N 0.4807(3) 0.65934(18) 0.45576(15) 0.0425(10) Uani 1 1 d D U . . .
C1 C 0.5825(6) 0.6451(3) 0.4901(3) 0.0372(19) Uani 0.628(8) 1 d D U P A 1
C2 C 0.6416(8) 0.6134(4) 0.4527(4) 0.054(3) Uani 0.628(8) 1 d D U P A 1
H2A H 0.7108 0.6028 0.4739 0.081 Uiso 0.628(8) 1 calc R U P A 1
H2B H 0.5995 0.5828 0.4396 0.081 Uiso 0.628(8) 1 calc R U P A 1
H2C H 0.6525 0.6342 0.4204 0.081 Uiso 0.628(8) 1 calc R U P A 1
C3 C 0.6486(7) 0.6915(4) 0.5121(4) 0.068(3) Uani 0.628(8) 1 d D U P A 1
H3A H 0.7158 0.6800 0.5348 0.102 Uiso 0.628(8) 1 calc R U P A 1
H3B H 0.6636 0.7122 0.4805 0.102 Uiso 0.628(8) 1 calc R U P A 1
H3C H 0.6090 0.7124 0.5352 0.102 Uiso 0.628(8) 1 calc R U P A 1
C4 C 0.5541(8) 0.6122(5) 0.5375(4) 0.067(3) Uani 0.628(8) 1 d D U P A 1
H4A H 0.6197 0.6013 0.5622 0.101 Uiso 0.628(8) 1 calc R U P A 1
H4B H 0.5103 0.6324 0.5590 0.101 Uiso 0.628(8) 1 calc R U P A 1
H4C H 0.5142 0.5817 0.5218 0.101 Uiso 0.628(8) 1 calc R U P A 1
C1X C 0.5628(9) 0.6225(5) 0.4880(5) 0.047(3) Uani 0.372(8) 1 d D U P A 2
C2X C 0.5364(13) 0.5648(5) 0.4859(7) 0.074(4) Uani 0.372(8) 1 d D U P A 2
H2D H 0.5261 0.5529 0.4470 0.111 Uiso 0.372(8) 1 calc R U P A 2
H2E H 0.5953 0.5458 0.5083 0.111 Uiso 0.372(8) 1 calc R U P A 2
H2F H 0.4710 0.5590 0.5011 0.111 Uiso 0.372(8) 1 calc R U P A 2
C3X C 0.6633(14) 0.6344(11) 0.4637(10) 0.094(7) Uani 0.372(8) 1 d D U P A 2
H3D H 0.6520 0.6243 0.4241 0.141 Uiso 0.372(8) 1 calc R U P A 2
H3E H 0.6785 0.6714 0.4669 0.141 Uiso 0.372(8) 1 calc R U P A 2
H3F H 0.7237 0.6151 0.4844 0.141 Uiso 0.372(8) 1 calc R U P A 2
C4X C 0.5774(14) 0.6377(7) 0.5496(5) 0.049(4) Uani 0.372(8) 1 d D U P A 2
H4D H 0.6298 0.6148 0.5717 0.074 Uiso 0.372(8) 1 calc R U P A 2
H4E H 0.6027 0.6733 0.5540 0.074 Uiso 0.372(8) 1 calc R U P A 2
H4F H 0.5091 0.6347 0.5626 0.074 Uiso 0.372(8) 1 calc R U P A 2
N2 N 0.0421(2) 0.61061(13) 0.39681(12) 0.0247(7) Uani 1 1 d D . . . .
C5 C -0.0330(3) 0.57368(16) 0.41289(16) 0.0302(8) Uani 1 1 d D . . . .
C6 C 0.0079(4) 0.51914(18) 0.4075(2) 0.0447(11) Uani 1 1 d D . . . .
H6A H 0.0154 0.5127 0.3686 0.054 Uiso 1 1 calc R U . . .
H6B H -0.0428 0.4945 0.4186 0.054 Uiso 1 1 calc R U . . .
H6C H 0.0773 0.5151 0.4319 0.054 Uiso 1 1 calc R U . . .
C7 C -0.0420(4) 0.5859(2) 0.47388(18) 0.0419(11) Uani 1 1 d D . . . .
H7A H 0.0276 0.5811 0.4979 0.050 Uiso 1 1 calc R U . . .
H7B H -0.0941 0.5627 0.4861 0.050 Uiso 1 1 calc R U . . .
H7C H -0.0652 0.6216 0.4765 0.050 Uiso 1 1 calc R U . . .
C8 C -0.1396(3) 0.5820(2) 0.3733(2) 0.0415(11) Uani 1 1 d D . . . .
H8A H -0.1638 0.6174 0.3769 0.050 Uiso 1 1 calc R U . . .
H8B H -0.1928 0.5580 0.3831 0.050 Uiso 1 1 calc R U . . .
H8C H -0.1302 0.5758 0.3346 0.050 Uiso 1 1 calc R U . . .
N3 N 0.2665(3) 0.62971(18) 0.21995(14) 0.0411(10) Uani 1 1 d D . . . .
C9 C 0.2723(4) 0.5995(3) 0.16963(19) 0.0545(15) Uani 1 1 d D . . . .
C10 C 0.3446(5) 0.6296(3) 0.1372(2) 0.077(2) Uani 1 1 d D . . . .
H10A H 0.3172 0.6646 0.1304 0.116 Uiso 1 1 calc R U . . .
H10B H 0.3462 0.6125 0.1013 0.116 Uiso 1 1 calc R U . . .
H10C H 0.4169 0.6308 0.1591 0.116 Uiso 1 1 calc R U . . .
C11 C 0.3168(6) 0.5467(3) 0.1871(2) 0.077(2) Uani 1 1 d . . . . .
H11C H 0.3885 0.5503 0.2092 0.116 Uiso 1 1 calc R U . . .
H11D H 0.3202 0.5260 0.1537 0.116 Uiso 1 1 calc R U . . .
H11E H 0.2704 0.5296 0.2098 0.116 Uiso 1 1 calc R U . . .
C12 C 0.1605(5) 0.5955(3) 0.1351(2) 0.0646(18) Uani 1 1 d . . . . .
H12A H 0.1135 0.5779 0.1570 0.097 Uiso 1 1 calc R U . . .
H12B H 0.1631 0.5761 0.1007 0.097 Uiso 1 1 calc R U . . .
H12C H 0.1328 0.6302 0.1253 0.097 Uiso 1 1 calc R U . . .
O2 O 0.1515(2) 0.81013(12) 0.37845(11) 0.0314(6) Uani 1 1 d D U . . .
Si1 Si 0.09933(13) 0.85750(5) 0.40888(5) 0.0441(3) Uani 1 1 d D U . . .
C14 C 0.0507(12) 0.9072(5) 0.3566(6) 0.047(3) Uani 0.64(2) 1 d D U P B 1
H14A H 0.0194 0.9356 0.3749 0.071 Uiso 0.64(2) 1 calc R U P B 1
H14B H 0.1103 0.9201 0.3399 0.071 Uiso 0.64(2) 1 calc R U P B 1
H14C H -0.0035 0.8923 0.3273 0.071 Uiso 0.64(2) 1 calc R U P B 1
C15 C -0.0040(15) 0.8400(4) 0.4474(8) 0.077(4) Uani 0.64(2) 1 d D U P B 1
H15A H -0.0298 0.8709 0.4640 0.115 Uiso 0.64(2) 1 calc R U P B 1
H15B H -0.0631 0.8238 0.4220 0.115 Uiso 0.64(2) 1 calc R U P B 1
H15C H 0.0247 0.8157 0.4772 0.115 Uiso 0.64(2) 1 calc R U P B 1
C16 C 0.2174(12) 0.8841(5) 0.4614(6) 0.075(4) Uani 0.64(2) 1 d D U P B 1
H16A H 0.1933 0.9131 0.4819 0.112 Uiso 0.64(2) 1 calc R U P B 1
H16B H 0.2459 0.8569 0.4879 0.112 Uiso 0.64(2) 1 calc R U P B 1
H16C H 0.2732 0.8958 0.4412 0.112 Uiso 0.64(2) 1 calc R U P B 1
C14X C 0.078(2) 0.9159(7) 0.3659(11) 0.050(6) Uani 0.36(2) 1 d D U P B 2
H14D H 0.0465 0.9427 0.3865 0.075 Uiso 0.36(2) 1 calc R U P B 2
H14E H 0.1461 0.9280 0.3575 0.075 Uiso 0.36(2) 1 calc R U P B 2
H14F H 0.0292 0.9082 0.3309 0.075 Uiso 0.36(2) 1 calc R U P B 2
C15X C -0.0417(13) 0.8379(7) 0.4172(12) 0.056(5) Uani 0.36(2) 1 d D U P B 2
H15D H -0.0745 0.8658 0.4354 0.083 Uiso 0.36(2) 1 calc R U P B 2
H15E H -0.0845 0.8311 0.3802 0.083 Uiso 0.36(2) 1 calc R U P B 2
H15F H -0.0385 0.8068 0.4403 0.083 Uiso 0.36(2) 1 calc R U P B 2
C16X C 0.173(2) 0.8689(10) 0.4804(7) 0.068(6) Uani 0.36(2) 1 d D U P B 2
H16D H 0.1394 0.8975 0.4975 0.103 Uiso 0.36(2) 1 calc R U P B 2
H16E H 0.1705 0.8378 0.5030 0.103 Uiso 0.36(2) 1 calc R U P B 2
H16F H 0.2469 0.8776 0.4789 0.103 Uiso 0.36(2) 1 calc R U P B 2
N4 N 0.3201(3) 0.75166(16) 0.46425(14) 0.0320(8) Uani 1 1 d D . . . .
H4G H 0.319(4) 0.7804(13) 0.4458(19) 0.038 Uiso 1 1 d D U . . .
H4H H 0.253(2) 0.7466(19) 0.466(2) 0.038 Uiso 1 1 d D U . . .
C17 C 0.3823(3) 0.7561(2) 0.51896(18) 0.0377(10) Uani 1 1 d . . . . .
C18 C 0.4658(4) 0.7905(3) 0.5321(2) 0.0557(15) Uani 1 1 d . . . . .
H18 H 0.4803 0.8147 0.5051 0.067 Uiso 1 1 calc R U . . .
C19 C 0.5281(4) 0.7894(3) 0.5851(2) 0.0635(18) Uani 1 1 d . . . . .
H19 H 0.5854 0.8131 0.5943 0.076 Uiso 1 1 calc R U . . .
C20 C 0.5079(4) 0.7543(3) 0.6246(2) 0.0561(15) Uani 1 1 d . . . . .
H20 H 0.5530 0.7530 0.6602 0.067 Uiso 1 1 calc R U . . .
C21 C 0.4224(4) 0.7209(2) 0.61271(18) 0.0438(12) Uani 1 1 d . . . . .
H21 H 0.4068 0.6977 0.6405 0.053 Uiso 1 1 calc R U . . .
C22 C 0.3595(3) 0.72161(19) 0.55976(16) 0.0340(10) Uani 1 1 d . . . . .
O3 O 0.2675(2) 0.69272(12) 0.54490(11) 0.0317(6) Uani 1 1 d . . . . .
C23 C 0.2666(3) 0.61706(17) 0.48663(16) 0.0296(9) Uani 1 1 d . . . . .
C24 C 0.2740(3) 0.63956(18) 0.53983(16) 0.0325(9) Uani 1 1 d . . . . .
C25 C 0.2776(4) 0.6095(2) 0.58738(18) 0.0446(12) Uani 1 1 d . . . . .
H25 H 0.2797 0.6254 0.6228 0.054 Uiso 1 1 calc R U . . .
C26 C 0.2782(5) 0.5570(2) 0.5835(2) 0.0600(16) Uani 1 1 d . . . . .
H26 H 0.2819 0.5365 0.6163 0.072 Uiso 1 1 calc R U . . .
C27 C 0.2733(5) 0.5338(2) 0.5318(2) 0.0599(16) Uani 1 1 d . . . . .
H27 H 0.2744 0.4973 0.5290 0.072 Uiso 1 1 calc R U . . .
C28 C 0.2669(4) 0.56373(19) 0.48401(19) 0.0430(11) Uani 1 1 d . . . . .
H28 H 0.2626 0.5474 0.4486 0.052 Uiso 1 1 calc R U . . .
N5 N 0.2580(2) 0.64647(14) 0.43662(12) 0.0270(7) Uani 1 1 d . . . . .
N6 N 0.3850(3) 0.64553(16) 0.34523(14) 0.0349(9) Uani 1 1 d . . . . .
C29 C 0.4459(3) 0.6027(2) 0.33384(17) 0.0420(12) Uani 1 1 d . . . . .
C30 C 0.5407(3) 0.6090(3) 0.3128(2) 0.0539(15) Uani 1 1 d . . . . .
H30 H 0.5676 0.6426 0.3084 0.065 Uiso 1 1 calc R U . . .
C31 C 0.5954(4) 0.5662(3) 0.2983(2) 0.066(2) Uani 1 1 d . . . . .
H31 H 0.6591 0.5707 0.2836 0.079 Uiso 1 1 calc R U . . .
C32 C 0.5584(4) 0.5178(3) 0.3052(2) 0.068(2) Uani 1 1 d . . . . .
H32 H 0.5966 0.4889 0.2949 0.081 Uiso 1 1 calc R U . . .
C33 C 0.4653(4) 0.5100(3) 0.3269(2) 0.0560(16) Uani 1 1 d . . . . .
H33 H 0.4411 0.4762 0.3328 0.067 Uiso 1 1 calc R U . . .
C34 C 0.4088(3) 0.5529(2) 0.33986(18) 0.0440(13) Uani 1 1 d . . . . .
O4 O 0.3140(2) 0.54686(14) 0.36109(12) 0.0403(8) Uani 1 1 d . . . . .
C35 C 0.1496(3) 0.57166(19) 0.30114(17) 0.0339(9) Uani 1 1 d . . . . .
C36 C 0.2235(4) 0.5334(2) 0.32174(18) 0.0391(11) Uani 1 1 d . . . . .
C37 C 0.2042(4) 0.4823(2) 0.3074(2) 0.0504(13) Uani 1 1 d . . . . .
H37 H 0.2533 0.4564 0.3228 0.060 Uiso 1 1 calc R U . . .
C38 C 0.1122(5) 0.4692(2) 0.2700(2) 0.0552(14) Uani 1 1 d . . . . .
H38 H 0.0990 0.4343 0.2595 0.066 Uiso 1 1 calc R U . . .
C39 C 0.0404(4) 0.5066(2) 0.2484(2) 0.0461(12) Uani 1 1 d . . . . .
H39 H -0.0219 0.4974 0.2226 0.055 Uiso 1 1 calc R U . . .
C40 C 0.0582(3) 0.55777(19) 0.26387(17) 0.0364(10) Uani 1 1 d . . . . .
H40 H 0.0078 0.5833 0.2490 0.044 Uiso 1 1 calc R U . . .
N7 N 0.1701(3) 0.62359(15) 0.31676(13) 0.0294(7) Uani 1 1 d . . . . .
N8 N 0.1580(2) 0.71751(15) 0.24667(13) 0.0312(8) Uani 1 1 d . . . . .
C41 C 0.0967(3) 0.71960(19) 0.19244(16) 0.0345(10) Uani 1 1 d . . . . .
C42 C 0.1362(4) 0.7425(2) 0.14802(17) 0.0460(13) Uani 1 1 d . . . . .
H42 H 0.2071 0.7553 0.1538 0.055 Uiso 1 1 calc R U . . .
C43 C 0.0726(4) 0.7467(3) 0.09545(19) 0.0617(17) Uani 1 1 d . . . . .
H43 H 0.0995 0.7629 0.0657 0.074 Uiso 1 1 calc R U . . .
C44 C -0.0302(5) 0.7272(3) 0.0865(2) 0.0663(19) Uani 1 1 d . . . . .
H44 H -0.0740 0.7304 0.0507 0.080 Uiso 1 1 calc R U . . .
C45 C -0.0692(4) 0.7032(2) 0.12953(18) 0.0501(14) Uani 1 1 d . . . . .
H45 H -0.1394 0.6894 0.1231 0.060 Uiso 1 1 calc R U . . .
C46 C -0.0065(3) 0.6991(2) 0.18196(17) 0.0370(10) Uani 1 1 d . . . . .
O5 O -0.0385(2) 0.67012(12) 0.22491(11) 0.0325(6) Uani 1 1 d . . . . .
C47 C -0.0798(3) 0.70990(16) 0.30732(16) 0.0257(8) Uani 1 1 d . . . . .
C48 C -0.1147(3) 0.69048(17) 0.25360(17) 0.0298(9) Uani 1 1 d . . . . .
C49 C -0.2219(3) 0.6877(2) 0.23147(19) 0.0404(11) Uani 1 1 d . . . . .
H49 H -0.2445 0.6738 0.1951 0.048 Uiso 1 1 calc R U . . .
C50 C -0.2964(3) 0.7050(2) 0.2621(2) 0.0510(14) Uani 1 1 d . . . . .
H50 H -0.3701 0.7040 0.2465 0.061 Uiso 1 1 calc R U . . .
C51 C -0.2634(3) 0.7239(2) 0.3158(2) 0.0469(13) Uani 1 1 d . . . . .
H51 H -0.3149 0.7354 0.3370 0.056 Uiso 1 1 calc R U . . .
C52 C -0.1559(3) 0.72610(18) 0.33881(18) 0.0331(9) Uani 1 1 d . . . . .
H52 H -0.1340 0.7386 0.3759 0.040 Uiso 1 1 calc R U . . .
N9 N 0.0302(2) 0.71358(13) 0.32933(12) 0.0228(6) Uani 1 1 d . . . . .
N10 N 0.0383(3) 0.80329(15) 0.26561(14) 0.0324(8) Uani 1 1 d . . . . .
C53 C -0.0148(4) 0.82831(19) 0.21852(18) 0.0389(10) Uani 1 1 d . . . . .
C54 C -0.1254(4) 0.8265(2) 0.2033(2) 0.0444(12) Uani 1 1 d . . . . .
H54 H -0.1671 0.8096 0.2267 0.053 Uiso 1 1 calc R U . . .
C55 C -0.1744(4) 0.8496(2) 0.1538(2) 0.0548(14) Uani 1 1 d . . . . .
H55 H -0.2498 0.8484 0.1433 0.066 Uiso 1 1 calc R U . . .
C56 C -0.1133(5) 0.8744(3) 0.1193(2) 0.0666(18) Uani 1 1 d . . . . .
H56 H -0.1474 0.8895 0.0852 0.080 Uiso 1 1 calc R U . . .
C57 C -0.0032(5) 0.8772(3) 0.1345(2) 0.0637(18) Uani 1 1 d . . . . .
H57 H 0.0380 0.8945 0.1112 0.076 Uiso 1 1 calc R U . . .
C58 C 0.0459(4) 0.8543(2) 0.18404(19) 0.0467(13) Uani 1 1 d . . . . .
O6 O 0.1570(3) 0.85284(15) 0.19760(13) 0.0485(9) Uani 1 1 d . . . . .
C59 C 0.2683(3) 0.8642(2) 0.28571(19) 0.0411(11) Uani 1 1 d . . . . .
C60 C 0.2044(4) 0.8864(2) 0.2400(2) 0.0461(13) Uani 1 1 d . . . . .
C61 C 0.1946(4) 0.9389(2) 0.2343(2) 0.0566(15) Uani 1 1 d . . . . .
H61 H 0.1504 0.9534 0.2025 0.068 Uiso 1 1 calc R U . . .
C62 C 0.2494(5) 0.9704(3) 0.2752(3) 0.0606(16) Uani 1 1 d . . . . .
H62 H 0.2414 1.0067 0.2719 0.073 Uiso 1 1 calc R U . . .
C63 C 0.3155(4) 0.9497(3) 0.3207(3) 0.0594(15) Uani 1 1 d . . . . .
H63 H 0.3545 0.9717 0.3482 0.071 Uiso 1 1 calc R U . . .
C64 C 0.3252(4) 0.8964(2) 0.3263(2) 0.0496(13) Uani 1 1 d . . . . .
H64 H 0.3706 0.8820 0.3579 0.059 Uiso 1 1 calc R U . . .
N11 N 0.2739(3) 0.80967(18) 0.29129(16) 0.0383(9) Uani 1 1 d D . . . .
H11A H 0.325(3) 0.800(2) 0.3179(17) 0.046 Uiso 1 1 d D U . . .
H11B H 0.281(4) 0.7939(19) 0.2607(15) 0.046 Uiso 1 1 d D U . . .
N12 N -0.4241(9) 0.8777(4) 0.1951(4) 0.147(4) Uani 1 1 d D . . . .
C65 C -0.4204(7) 0.8650(3) 0.2385(3) 0.081(2) Uani 1 1 d D . . . .
C66 C -0.4123(9) 0.8481(6) 0.2936(4) 0.177(7) Uani 1 1 d D . . . .
H66A H -0.4515 0.8157 0.2942 0.266 Uiso 1 1 calc R U . . .
H66B H -0.4426 0.8741 0.3156 0.266 Uiso 1 1 calc R U . . .
H66C H -0.3371 0.8425 0.3098 0.266 Uiso 1 1 calc R U . . .
N13 N 0.277(2) 1.0913(9) 0.3929(10) 0.095(7) Uani 0.329(8) 1 d D U P C 1
C67 C 0.204(2) 1.0727(8) 0.4013(11) 0.091(8) Uani 0.329(8) 1 d D U P C 1
C68 C 0.1166(17) 1.0498(8) 0.4244(9) 0.079(6) Uani 0.329(8) 1 d D U P C 1
H68A H 0.1441 1.0357 0.4616 0.119 Uiso 0.329(8) 1 calc R U P C 1
H68B H 0.0840 1.0222 0.3997 0.119 Uiso 0.329(8) 1 calc R U P C 1
H68C H 0.0629 1.0762 0.4275 0.119 Uiso 0.329(8) 1 calc R U P C 1
N13X N 0.327(3) 1.0864(16) 0.372(2) 0.096(16) Uani 0.171(8) 1 d D U P C 2
C67X C 0.388(2) 1.0725(10) 0.4061(13) 0.052(8) Uani 0.171(8) 1 d D U P C 2
C68X C 0.476(3) 1.0524(16) 0.4443(16) 0.077(12) Uani 0.171(8) 1 d D U P C 2
H68D H 0.5247 1.0348 0.4233 0.115 Uiso 0.171(8) 1 calc R U P C 2
H68E H 0.4507 1.0280 0.4697 0.115 Uiso 0.171(8) 1 calc R U P C 2
H68F H 0.5140 1.0807 0.4660 0.115 Uiso 0.171(8) 1 calc R U P C 2
N14 N 0.566(2) 0.9119(10) 0.4343(10) 0.131(10) Uani 0.314(4) 1 d D U P A 1
C69 C 0.6246(19) 0.8806(9) 0.4491(8) 0.079(6) Uani 0.314(4) 1 d D U P A 1
C70 C 0.6975(18) 0.8398(9) 0.4676(10) 0.069(5) Uani 0.314(4) 1 d D U P A 1
H70A H 0.7309 0.8458 0.5066 0.103 Uiso 0.314(4) 1 calc R U P A 1
H70B H 0.7526 0.8385 0.4440 0.103 Uiso 0.314(4) 1 calc R U P A 1
H70C H 0.6590 0.8069 0.4649 0.103 Uiso 0.314(4) 1 calc R U P A 1
N14X N 0.716(2) 0.8563(9) 0.488(2) 0.090(11) Uani 0.186(4) 1 d D U P A 2
C69X C 0.724(2) 0.8152(9) 0.4881(16) 0.053(8) Uani 0.186(4) 1 d D U P A 2
C70X C 0.7402(19) 0.7610(9) 0.4849(12) 0.050(6) Uani 0.186(4) 1 d D U P A 2
H70D H 0.8037 0.7543 0.4683 0.075 Uiso 0.186(4) 1 calc R U P A 2
H70E H 0.6778 0.7453 0.4616 0.075 Uiso 0.186(4) 1 calc R U P A 2
H70F H 0.7501 0.7461 0.5226 0.075 Uiso 0.186(4) 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 N1 1.713(4) . ?
Mo1 N6 1.906(3) . ?
Mo1 N5 2.006(3) . ?
Mo1 O1 2.168(3) . ?
Mo1 N4 2.347(4) . ?
Mo1 Cl1 2.4846(13) . ?
Mo2 N2 1.718(3) . ?
Mo2 N7 1.959(3) . ?
Mo2 N5 1.993(3) . ?
Mo2 N9 2.139(3) . ?
Mo2 O1 2.234(3) . ?
Mo2 Cl2 2.5224(10) . ?
Mo3 N3 1.711(4) . ?
Mo3 N8 1.903(4) . ?
Mo3 N7 2.052(4) . ?
Mo3 N6 2.145(3) . ?
Mo3 O1 2.253(3) . ?
Mo3 Cl3 2.4754(12) . ?
Mo4 N10 1.746(4) . ?
Mo4 N9 1.895(3) . ?
Mo4 O2 1.949(3) . ?
Mo4 O1 2.086(3) . ?
Mo4 N8 2.132(4) . ?
Mo4 N11 2.356(4) . ?
N1 C1 1.461(7) . ?
N1 C1X 1.527(11) . ?
C1 C3 1.514(11) . ?
C1 C2 1.516(10) . ?
C1 C4 1.526(10) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C1X C4X 1.524(12) . ?
C1X C3X 1.531(15) . ?
C1X C2X 1.534(13) . ?
C2X H2D 0.9800 . ?
C2X H2E 0.9800 . ?
C2X H2F 0.9800 . ?
C3X H3D 0.9800 . ?
C3X H3E 0.9800 . ?
C3X H3F 0.9800 . ?
C4X H4D 0.9800 . ?
C4X H4E 0.9800 . ?
C4X H4F 0.9800 . ?
N2 C5 1.455(5) . ?
C5 C6 1.523(6) . ?
C5 C8 1.535(6) . ?
C5 C7 1.536(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N3 C9 1.464(5) . ?
C9 C11 1.515(9) . ?
C9 C12 1.524(7) . ?
C9 C10 1.527(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11C 0.9800 . ?
C11 H11D 0.9800 . ?
C11 H11E 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O2 Si1 1.634(3) . ?
Si1 C15 1.800(9) . ?
Si1 C14X 1.833(12) . ?
Si1 C14 1.838(8) . ?
Si1 C16X 1.845(12) . ?
Si1 C15X 1.912(13) . ?
Si1 C16 1.921(9) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C14X H14D 0.9800 . ?
C14X H14E 0.9800 . ?
C14X H14F 0.9800 . ?
C15X H15D 0.9800 . ?
C15X H15E 0.9800 . ?
C15X H15F 0.9800 . ?
C16X H16D 0.9800 . ?
C16X H16E 0.9800 . ?
C16X H16F 0.9800 . ?
N4 C17 1.425(5) . ?
N4 H4G 0.87(3) . ?
N4 H4H 0.87(3) . ?
C17 C18 1.383(7) . ?
C17 C22 1.401(7) . ?
C18 C19 1.388(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.379(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.382(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.389(6) . ?
C21 H21 0.9500 . ?
C22 O3 1.385(5) . ?
O3 C24 1.390(5) . ?
C23 C28 1.387(7) . ?
C23 C24 1.404(5) . ?
C23 N5 1.421(5) . ?
C24 C25 1.387(6) . ?
C25 C26 1.367(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.382(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.386(7) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
N6 C29 1.411(6) . ?
C29 C34 1.392(8) . ?
C29 C30 1.400(6) . ?
C30 C31 1.390(8) . ?
C30 H30 0.9500 . ?
C31 C32 1.362(10) . ?
C31 H31 0.9500 . ?
C32 C33 1.394(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.392(7) . ?
C33 H33 0.9500 . ?
C34 O4 1.402(5) . ?
O4 C36 1.406(5) . ?
C35 C40 1.391(6) . ?
C35 C36 1.400(6) . ?
C35 N7 1.413(6) . ?
C36 C37 1.383(7) . ?
C37 C38 1.392(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.374(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.389(7) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
N8 C41 1.408(5) . ?
C41 C42 1.398(6) . ?
C41 C46 1.399(6) . ?
C42 C43 1.390(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.385(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.381(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.382(6) . ?
C45 H45 0.9500 . ?
C46 O5 1.402(5) . ?
O5 C48 1.394(5) . ?
C47 C48 1.395(6) . ?
C47 C52 1.399(6) . ?
C47 N9 1.413(5) . ?
C48 C49 1.378(5) . ?
C49 C50 1.378(7) . ?
C49 H49 0.9500 . ?
C50 C51 1.385(7) . ?
C50 H50 0.9500 . ?
C51 C52 1.387(6) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
N10 C53 1.383(5) . ?
C53 C54 1.393(6) . ?
C53 C58 1.406(6) . ?
C54 C55 1.389(7) . ?
C54 H54 0.9500 . ?
C55 C56 1.394(8) . ?
C55 H55 0.9500 . ?
C56 C57 1.388(8) . ?
C56 H56 0.9500 . ?
C57 C58 1.387(7) . ?
C57 H57 0.9500 . ?
C58 O6 1.397(6) . ?
O6 C60 1.401(6) . ?
C59 C60 1.382(7) . ?
C59 C64 1.395(7) . ?
C59 N11 1.423(7) . ?
C60 C61 1.374(8) . ?
C61 C62 1.376(9) . ?
C61 H61 0.9500 . ?
C62 C63 1.375(8) . ?
C62 H62 0.9500 . ?
C63 C64 1.396(9) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
N11 H11A 0.86(3) . ?
N11 H11B 0.86(3) . ?
N12 C65 1.093(9) . ?
C65 C66 1.395(10) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
N13 C67 1.104(17) . ?
C67 C68 1.455(18) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
N13X C67X 1.092(18) . ?
C67X C68X 1.428(18) . ?
C68X H68D 0.9800 . ?
C68X H68E 0.9800 . ?
C68X H68F 0.9800 . ?
N14 C69 1.119(17) . ?
C69 C70 1.430(18) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
N14X C69X 1.074(18) . ?
C69X C70X 1.426(18) . ?
C70X H70D 0.9800 . ?
C70X H70E 0.9800 . ?
C70X H70F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Mo1 N6 99.51(16) . . ?
N1 Mo1 N5 97.94(17) . . ?
N6 Mo1 N5 98.42(15) . . ?
N1 Mo1 O1 176.54(18) . . ?
N6 Mo1 O1 79.00(13) . . ?
N5 Mo1 O1 79.26(11) . . ?
N1 Mo1 N4 102.04(15) . . ?
N6 Mo1 N4 158.04(14) . . ?
N5 Mo1 N4 82.82(13) . . ?
O1 Mo1 N4 79.71(11) . . ?
N1 Mo1 Cl1 93.99(16) . . ?
N6 Mo1 Cl1 98.04(12) . . ?
N5 Mo1 Cl1 157.75(10) . . ?
O1 Mo1 Cl1 89.31(8) . . ?
N4 Mo1 Cl1 76.34(10) . . ?
N2 Mo2 N7 97.27(15) . . ?
N2 Mo2 N5 102.76(14) . . ?
N7 Mo2 N5 98.11(13) . . ?
N2 Mo2 N9 107.74(13) . . ?
N7 Mo2 N9 93.46(13) . . ?
N5 Mo2 N9 145.62(14) . . ?
N2 Mo2 O1 173.50(13) . . ?
N7 Mo2 O1 76.25(13) . . ?
N5 Mo2 O1 77.94(12) . . ?
N9 Mo2 O1 73.57(11) . . ?
N2 Mo2 Cl2 89.43(11) . . ?
N7 Mo2 Cl2 170.97(11) . . ?
N5 Mo2 Cl2 86.24(9) . . ?
N9 Mo2 Cl2 78.68(8) . . ?
O1 Mo2 Cl2 97.07(8) . . ?
N3 Mo3 N8 101.47(17) . . ?
N3 Mo3 N7 97.44(17) . . ?
N8 Mo3 N7 96.90(13) . . ?
N3 Mo3 N6 110.25(16) . . ?
N8 Mo3 N6 148.12(14) . . ?
N7 Mo3 N6 82.33(13) . . ?
N3 Mo3 O1 170.89(14) . . ?
N8 Mo3 O1 76.75(12) . . ?
N7 Mo3 O1 74.07(12) . . ?
N6 Mo3 O1 72.40(12) . . ?
N3 Mo3 Cl3 90.76(14) . . ?
N8 Mo3 Cl3 92.78(11) . . ?
N7 Mo3 Cl3 165.80(9) . . ?
N6 Mo3 Cl3 83.95(11) . . ?
O1 Mo3 Cl3 98.23(8) . . ?
N10 Mo4 N9 100.81(14) . . ?
N10 Mo4 O2 101.56(15) . . ?
N9 Mo4 O2 106.18(12) . . ?
N10 Mo4 O1 166.67(14) . . ?
N9 Mo4 O1 82.16(12) . . ?
O2 Mo4 O1 89.94(12) . . ?
N10 Mo4 N8 91.15(15) . . ?
N9 Mo4 N8 87.71(13) . . ?
O2 Mo4 N8 158.80(12) . . ?
O1 Mo4 N8 75.91(12) . . ?
N10 Mo4 N11 91.16(15) . . ?
N9 Mo4 N11 163.71(15) . . ?
O2 Mo4 N11 81.85(13) . . ?
O1 Mo4 N11 83.73(13) . . ?
N8 Mo4 N11 80.99(14) . . ?
Mo4 O1 Mo1 159.21(16) . . ?
Mo4 O1 Mo2 96.97(10) . . ?
Mo1 O1 Mo2 94.13(11) . . ?
Mo4 O1 Mo3 98.38(10) . . ?
Mo1 O1 Mo3 97.80(11) . . ?
Mo2 O1 Mo3 96.33(11) . . ?
C1 N1 Mo1 168.5(5) . . ?
C1X N1 Mo1 164.2(6) . . ?
N1 C1 C3 112.5(7) . . ?
N1 C1 C2 106.3(6) . . ?
C3 C1 C2 109.8(8) . . ?
N1 C1 C4 105.5(6) . . ?
C3 C1 C4 111.7(8) . . ?
C2 C1 C4 110.8(9) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
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 . . ?
C4X C1X N1 107.1(9) . . ?
C4X C1X C3X 111.0(13) . . ?
N1 C1X C3X 102.8(12) . . ?
C4X C1X C2X 105.9(12) . . ?
N1 C1X C2X 117.9(10) . . ?
C3X C1X C2X 112.2(13) . . ?
C1X C2X H2D 109.5 . . ?
C1X C2X H2E 109.5 . . ?
H2D C2X H2E 109.5 . . ?
C1X C2X H2F 109.5 . . ?
H2D C2X H2F 109.5 . . ?
H2E C2X H2F 109.5 . . ?
C1X C3X H3D 109.5 . . ?
C1X C3X H3E 109.5 . . ?
H3D C3X H3E 109.5 . . ?
C1X C3X H3F 109.5 . . ?
H3D C3X H3F 109.5 . . ?
H3E C3X H3F 109.5 . . ?
C1X C4X H4D 109.5 . . ?
C1X C4X H4E 109.5 . . ?
H4D C4X H4E 109.5 . . ?
C1X C4X H4F 109.5 . . ?
H4D C4X H4F 109.5 . . ?
H4E C4X H4F 109.5 . . ?
C5 N2 Mo2 175.1(3) . . ?
N2 C5 C6 109.9(3) . . ?
N2 C5 C8 106.9(3) . . ?
C6 C5 C8 110.8(4) . . ?
N2 C5 C7 106.5(3) . . ?
C6 C5 C7 111.0(4) . . ?
C8 C5 C7 111.5(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 N3 Mo3 175.4(4) . . ?
N3 C9 C11 108.9(4) . . ?
N3 C9 C12 108.4(4) . . ?
C11 C9 C12 111.2(6) . . ?
N3 C9 C10 106.1(5) . . ?
C11 C9 C10 112.2(5) . . ?
C12 C9 C10 110.0(5) . . ?
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 . . ?
C9 C11 H11C 109.5 . . ?
C9 C11 H11D 109.5 . . ?
H11C C11 H11D 109.5 . . ?
C9 C11 H11E 109.5 . . ?
H11C C11 H11E 109.5 . . ?
H11D C11 H11E 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 O2 Mo4 142.15(18) . . ?
O2 Si1 C15 115.8(4) . . ?
O2 Si1 C14X 113.5(9) . . ?
O2 Si1 C14 109.4(5) . . ?
C15 Si1 C14 110.2(7) . . ?
O2 Si1 C16X 111.5(6) . . ?
C14X Si1 C16X 113.7(10) . . ?
O2 Si1 C15X 108.1(6) . . ?
C14X Si1 C15X 103.3(9) . . ?
C16X Si1 C15X 105.9(9) . . ?
O2 Si1 C16 103.7(5) . . ?
C15 Si1 C16 107.8(6) . . ?
C14 Si1 C16 109.5(5) . . ?
Si1 C14 H14A 109.5 . . ?
Si1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C14X H14D 109.5 . . ?
Si1 C14X H14E 109.5 . . ?
H14D C14X H14E 109.5 . . ?
Si1 C14X H14F 109.5 . . ?
H14D C14X H14F 109.5 . . ?
H14E C14X H14F 109.5 . . ?
Si1 C15X H15D 109.5 . . ?
Si1 C15X H15E 109.5 . . ?
H15D C15X H15E 109.5 . . ?
Si1 C15X H15F 109.5 . . ?
H15D C15X H15F 109.5 . . ?
H15E C15X H15F 109.5 . . ?
Si1 C16X H16D 109.5 . . ?
Si1 C16X H16E 109.5 . . ?
H16D C16X H16E 109.5 . . ?
Si1 C16X H16F 109.5 . . ?
H16D C16X H16F 109.5 . . ?
H16E C16X H16F 109.5 . . ?
C17 N4 Mo1 113.8(3) . . ?
C17 N4 H4G 111(3) . . ?
Mo1 N4 H4G 109(3) . . ?
C17 N4 H4H 110(3) . . ?
Mo1 N4 H4H 108(3) . . ?
H4G N4 H4H 103(5) . . ?
C18 C17 C22 119.7(4) . . ?
C18 C17 N4 123.1(4) . . ?
C22 C17 N4 117.1(4) . . ?
C17 C18 C19 119.5(5) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.3 . . ?
C20 C19 C18 120.7(5) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 120.4(5) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C20 C21 C22 119.4(5) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
O3 C22 C21 123.9(4) . . ?
O3 C22 C17 115.6(4) . . ?
C21 C22 C17 120.2(4) . . ?
C22 O3 C24 120.0(3) . . ?
C28 C23 C24 117.2(4) . . ?
C28 C23 N5 119.9(4) . . ?
C24 C23 N5 122.9(4) . . ?
C25 C24 O3 118.7(4) . . ?
C25 C24 C23 121.1(4) . . ?
O3 C24 C23 120.0(4) . . ?
C26 C25 C24 120.3(5) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 119.8(5) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
C26 C27 C28 120.0(5) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 C23 121.5(4) . . ?
C27 C28 H28 119.2 . . ?
C23 C28 H28 119.2 . . ?
C23 N5 Mo2 126.2(3) . . ?
C23 N5 Mo1 126.3(3) . . ?
Mo2 N5 Mo1 107.42(15) . . ?
C29 N6 Mo1 134.8(3) . . ?
C29 N6 Mo3 114.4(3) . . ?
Mo1 N6 Mo3 110.52(17) . . ?
C34 C29 C30 118.5(5) . . ?
C34 C29 N6 120.3(4) . . ?
C30 C29 N6 121.1(5) . . ?
C31 C30 C29 120.0(6) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C32 C31 C30 120.6(5) . . ?
C32 C31 H31 119.7 . . ?
C30 C31 H31 119.7 . . ?
C31 C32 C33 121.0(5) . . ?
C31 C32 H32 119.5 . . ?
C33 C32 H32 119.5 . . ?
C34 C33 C32 118.5(7) . . ?
C34 C33 H33 120.8 . . ?
C32 C33 H33 120.8 . . ?
C33 C34 C29 121.4(5) . . ?
C33 C34 O4 120.4(5) . . ?
C29 C34 O4 118.2(4) . . ?
C34 O4 C36 115.8(3) . . ?
C40 C35 C36 118.8(4) . . ?
C40 C35 N7 121.1(4) . . ?
C36 C35 N7 120.1(4) . . ?
C37 C36 C35 120.9(4) . . ?
C37 C36 O4 119.9(4) . . ?
C35 C36 O4 119.0(4) . . ?
C36 C37 C38 119.3(5) . . ?
C36 C37 H37 120.3 . . ?
C38 C37 H37 120.3 . . ?
C39 C38 C37 120.4(5) . . ?
C39 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
C38 C39 C40 120.4(5) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
C39 C40 C35 120.2(4) . . ?
C39 C40 H40 119.9 . . ?
C35 C40 H40 119.9 . . ?
C35 N7 Mo2 125.7(3) . . ?
C35 N7 Mo3 121.1(2) . . ?
Mo2 N7 Mo3 112.91(18) . . ?
C41 N8 Mo3 128.6(3) . . ?
C41 N8 Mo4 122.0(3) . . ?
Mo3 N8 Mo4 108.93(14) . . ?
C42 C41 C46 118.4(4) . . ?
C42 C41 N8 121.3(4) . . ?
C46 C41 N8 120.3(4) . . ?
C43 C42 C41 120.6(4) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C44 C43 C42 119.9(4) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C45 C44 C43 120.1(4) . . ?
C45 C44 H44 119.9 . . ?
C43 C44 H44 119.9 . . ?
C44 C45 C46 120.2(4) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C45 C46 C41 120.8(4) . . ?
C45 C46 O5 121.8(4) . . ?
C41 C46 O5 117.1(4) . . ?
C48 O5 C46 119.1(3) . . ?
C48 C47 C52 118.7(4) . . ?
C48 C47 N9 120.7(3) . . ?
C52 C47 N9 120.6(4) . . ?
C49 C48 O5 121.0(4) . . ?
C49 C48 C47 121.0(4) . . ?
O5 C48 C47 117.8(3) . . ?
C48 C49 C50 120.1(4) . . ?
C48 C49 H49 120.0 . . ?
C50 C49 H49 120.0 . . ?
C49 C50 C51 119.9(4) . . ?
C49 C50 H50 120.1 . . ?
C51 C50 H50 120.1 . . ?
C50 C51 C52 120.5(4) . . ?
C50 C51 H51 119.7 . . ?
C52 C51 H51 119.7 . . ?
C51 C52 C47 119.8(4) . . ?
C51 C52 H52 120.1 . . ?
C47 C52 H52 120.1 . . ?
C47 N9 Mo4 126.4(3) . . ?
C47 N9 Mo2 126.8(3) . . ?
Mo4 N9 Mo2 106.52(13) . . ?
C53 N10 Mo4 165.3(3) . . ?
N10 C53 C54 121.9(4) . . ?
N10 C53 C58 118.4(4) . . ?
C54 C53 C58 119.6(4) . . ?
C55 C54 C53 119.7(5) . . ?
C55 C54 H54 120.2 . . ?
C53 C54 H54 120.2 . . ?
C54 C55 C56 120.2(5) . . ?
C54 C55 H55 119.9 . . ?
C56 C55 H55 119.9 . . ?
C57 C56 C55 120.7(5) . . ?
C57 C56 H56 119.7 . . ?
C55 C56 H56 119.7 . . ?
C58 C57 C56 119.2(5) . . ?
C58 C57 H57 120.4 . . ?
C56 C57 H57 120.4 . . ?
C57 C58 O6 120.0(4) . . ?
C57 C58 C53 120.6(5) . . ?
O6 C58 C53 119.1(4) . . ?
C58 O6 C60 116.4(4) . . ?
C60 C59 C64 118.4(5) . . ?
C60 C59 N11 120.3(5) . . ?
C64 C59 N11 121.2(4) . . ?
C61 C60 C59 121.7(5) . . ?
C61 C60 O6 121.7(5) . . ?
C59 C60 O6 116.5(5) . . ?
C60 C61 C62 119.6(5) . . ?
C60 C61 H61 120.2 . . ?
C62 C61 H61 120.2 . . ?
C63 C62 C61 120.5(6) . . ?
C63 C62 H62 119.8 . . ?
C61 C62 H62 119.8 . . ?
C62 C63 C64 119.9(6) . . ?
C62 C63 H63 120.1 . . ?
C64 C63 H63 120.1 . . ?
C59 C64 C63 120.0(5) . . ?
C59 C64 H64 120.0 . . ?
C63 C64 H64 120.0 . . ?
C59 N11 Mo4 118.5(3) . . ?
C59 N11 H11A 112(4) . . ?
Mo4 N11 H11A 103(4) . . ?
C59 N11 H11B 114(4) . . ?
Mo4 N11 H11B 100(4) . . ?
H11A N11 H11B 109(5) . . ?
N12 C65 C66 178.0(12) . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N13 C67 C68 168(3) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
N13X C67X C68X 171(5) . . ?
C67X C68X H68D 109.5 . . ?
C67X C68X H68E 109.5 . . ?
H68D C68X H68E 109.5 . . ?
C67X C68X H68F 109.5 . . ?
H68D C68X H68F 109.5 . . ?
H68E C68X H68F 109.5 . . ?
N14 C69 C70 179(3) . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
N14X C69X C70X 176(4) . . ?
C69X C70X H70D 109.5 . . ?
C69X C70X H70E 109.5 . . ?
H70D C70X H70E 109.5 . . ?
C69X C70X H70F 109.5 . . ?
H70D C70X H70F 109.5 . . ?
H70E C70X H70F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N6 Mo1 N1 C1_a 89(2) . . . . ?
N5 Mo1 N1 C1 -171(2) . . . . ?
N4 Mo1 N1 C1 -87(2) . . . . ?
Cl1 Mo1 N1 C1 -10(2) . . . . ?
N6 Mo1 N1 C1X -38(2) . . . . ?
N5 Mo1 N1 C1X 62(2) . . . . ?
N4 Mo1 N1 C1X 146(2) . . . . ?
Cl1 Mo1 N1 C1X -137(2) . . . . ?
C1X N1 C1 C3 -171.1(19) . . . . ?
Mo1 N1 C1 C3 41(2) . . . . ?
C1X N1 C1 C2 68.6(16) . . . . ?
Mo1 N1 C1 C2 -80(2) . . . . ?
C1X N1 C1 C4 -49.1(14) . . . . ?
Mo1 N1 C1 C4 162.7(19) . . . . ?
C1 N1 C1X C4X 64.8(15) . . . . ?
Mo1 N1 C1X C4X -138.0(17) . . . . ?
C1 N1 C1X C3X -52.2(17) . . . . ?
Mo1 N1 C1X C3X 105(2) . . . . ?
C1 N1 C1X C2X -176(2) . . . . ?
Mo1 N1 C1X C2X -19(3) . . . . ?
Mo4 O2 Si1 C15 78.4(9) . . . . ?
Mo4 O2 Si1 C14X -61.0(10) . . . . ?
Mo4 O2 Si1 C14 -46.9(6) . . . . ?
Mo4 O2 Si1 C16X 169.0(12) . . . . ?
Mo4 O2 Si1 C15X 53.0(9) . . . . ?
Mo4 O2 Si1 C16 -163.7(6) . . . . ?
Mo1 N4 C17 C18 96.5(5) . . . . ?
Mo1 N4 C17 C22 -80.2(4) . . . . ?
C22 C17 C18 C19 2.0(8) . . . . ?
N4 C17 C18 C19 -174.5(5) . . . . ?
C17 C18 C19 C20 0.2(10) . . . . ?
C18 C19 C20 C21 -2.5(9) . . . . ?
C19 C20 C21 C22 2.6(8) . . . . ?
C20 C21 C22 O3 -174.8(4) . . . . ?
C20 C21 C22 C17 -0.4(7) . . . . ?
C18 C17 C22 O3 172.9(4) . . . . ?
N4 C17 C22 O3 -10.3(6) . . . . ?
C18 C17 C22 C21 -1.9(7) . . . . ?
N4 C17 C22 C21 174.8(4) . . . . ?
C21 C22 O3 C24 -70.1(5) . . . . ?
C17 C22 O3 C24 115.2(4) . . . . ?
C22 O3 C24 C25 85.9(5) . . . . ?
C22 O3 C24 C23 -100.2(4) . . . . ?
C28 C23 C24 C25 -2.3(6) . . . . ?
N5 C23 C24 C25 177.2(4) . . . . ?
C28 C23 C24 O3 -176.1(4) . . . . ?
N5 C23 C24 O3 3.4(6) . . . . ?
O3 C24 C25 C26 176.4(5) . . . . ?
C23 C24 C25 C26 2.6(8) . . . . ?
C24 C25 C26 C27 -1.1(9) . . . . ?
C25 C26 C27 C28 -0.6(10) . . . . ?
C26 C27 C28 C23 0.9(9) . . . . ?
C24 C23 C28 C27 0.6(7) . . . . ?
N5 C23 C28 C27 -178.9(5) . . . . ?
C28 C23 N5 Mo2 76.3(5) . . . . ?
C24 C23 N5 Mo2 -103.1(4) . . . . ?
C28 C23 N5 Mo1 -105.4(4) . . . . ?
C24 C23 N5 Mo1 75.2(5) . . . . ?
Mo1 N6 C29 C34 89.2(5) . . . . ?
Mo3 N6 C29 C34 -84.7(4) . . . . ?
Mo1 N6 C29 C30 -95.1(5) . . . . ?
Mo3 N6 C29 C30 91.0(4) . . . . ?
C34 C29 C30 C31 0.2(7) . . . . ?
N6 C29 C30 C31 -175.6(4) . . . . ?
C29 C30 C31 C32 -0.9(8) . . . . ?
C30 C31 C32 C33 -0.2(8) . . . . ?
C31 C32 C33 C34 2.1(8) . . . . ?
C32 C33 C34 C29 -2.9(7) . . . . ?
C32 C33 C34 O4 179.1(4) . . . . ?
C30 C29 C34 C33 1.8(7) . . . . ?
N6 C29 C34 C33 177.6(4) . . . . ?
C30 C29 C34 O4 179.8(4) . . . . ?
N6 C29 C34 O4 -4.3(6) . . . . ?
C33 C34 O4 C36 -76.8(5) . . . . ?
C29 C34 O4 C36 105.1(5) . . . . ?
C40 C35 C36 C37 -2.8(7) . . . . ?
N7 C35 C36 C37 179.3(4) . . . . ?
C40 C35 C36 O4 -177.6(4) . . . . ?
N7 C35 C36 O4 4.5(6) . . . . ?
C34 O4 C36 C37 84.4(6) . . . . ?
C34 O4 C36 C35 -100.7(5) . . . . ?
C35 C36 C37 C38 2.7(8) . . . . ?
O4 C36 C37 C38 177.5(5) . . . . ?
C36 C37 C38 C39 -1.0(8) . . . . ?
C37 C38 C39 C40 -0.7(8) . . . . ?
C38 C39 C40 C35 0.6(7) . . . . ?
C36 C35 C40 C39 1.1(7) . . . . ?
N7 C35 C40 C39 179.0(4) . . . . ?
C40 C35 N7 Mo2 90.5(4) . . . . ?
C36 C35 N7 Mo2 -91.6(4) . . . . ?
C40 C35 N7 Mo3 -95.3(4) . . . . ?
C36 C35 N7 Mo3 82.5(4) . . . . ?
Mo3 N8 C41 C42 -83.2(6) . . . . ?
Mo4 N8 C41 C42 106.2(5) . . . . ?
Mo3 N8 C41 C46 97.5(5) . . . . ?
Mo4 N8 C41 C46 -73.2(6) . . . . ?
C46 C41 C42 C43 2.8(9) . . . . ?
N8 C41 C42 C43 -176.5(5) . . . . ?
C41 C42 C43 C44 -1.3(10) . . . . ?
C42 C43 C44 C45 -0.6(11) . . . . ?
C43 C44 C45 C46 0.9(11) . . . . ?
C44 C45 C46 C41 0.7(9) . . . . ?
C44 C45 C46 O5 -172.8(6) . . . . ?
C42 C41 C46 C45 -2.5(8) . . . . ?
N8 C41 C46 C45 176.8(5) . . . . ?
C42 C41 C46 O5 171.3(5) . . . . ?
N8 C41 C46 O5 -9.4(7) . . . . ?
C45 C46 O5 C48 -76.9(6) . . . . ?
C41 C46 O5 C48 109.3(5) . . . . ?
C46 O5 C48 C49 81.2(5) . . . . ?
C46 O5 C48 C47 -103.9(4) . . . . ?
C52 C47 C48 C49 0.7(6) . . . . ?
N9 C47 C48 C49 -178.7(4) . . . . ?
C52 C47 C48 O5 -174.1(4) . . . . ?
N9 C47 C48 O5 6.4(6) . . . . ?
O5 C48 C49 C50 175.7(4) . . . . ?
C47 C48 C49 C50 1.1(7) . . . . ?
C48 C49 C50 C51 -1.8(8) . . . . ?
C49 C50 C51 C52 0.8(8) . . . . ?
C50 C51 C52 C47 1.0(8) . . . . ?
C48 C47 C52 C51 -1.7(6) . . . . ?
N9 C47 C52 C51 177.7(4) . . . . ?
C48 C47 N9 Mo4 79.1(5) . . . . ?
C52 C47 N9 Mo4 -100.4(4) . . . . ?
C48 C47 N9 Mo2 -94.2(4) . . . . ?
C52 C47 N9 Mo2 86.4(4) . . . . ?
N10 Mo4 N9 C47 -0.3(3) . . . . ?
O2 Mo4 N9 C47 105.2(3) . . . . ?
O1 Mo4 N9 C47 -167.1(3) . . . . ?
N8 Mo4 N9 C47 -91.0(3) . . . . ?
N11 Mo4 N9 C47 -136.9(4) . . . . ?
N10 Mo4 N9 Mo2 174.09(15) . . . . ?
O2 Mo4 N9 Mo2 -80.38(15) . . . . ?
O1 Mo4 N9 Mo2 7.27(12) . . . . ?
N8 Mo4 N9 Mo2 83.36(14) . . . . ?
N11 Mo4 N9 Mo2 37.5(5) . . . . ?
N9 Mo4 N10 C53 -110.9(13) . . . . ?
O2 Mo4 N10 C53 139.9(13) . . . . ?
O1 Mo4 N10 C53 -9.2(17) . . . . ?
N8 Mo4 N10 C53 -23.1(13) . . . . ?
N11 Mo4 N10 C53 57.9(13) . . . . ?
Mo4 N10 C53 C54 128.9(11) . . . . ?
Mo4 N10 C53 C58 -48.2(15) . . . . ?
N10 C53 C54 C55 -176.0(5) . . . . ?
C58 C53 C54 C55 1.2(8) . . . . ?
C53 C54 C55 C56 0.0(9) . . . . ?
C54 C55 C56 C57 -1.1(11) . . . . ?
C55 C56 C57 C58 0.9(11) . . . . ?
C56 C57 C58 O6 174.5(6) . . . . ?
C56 C57 C58 C53 0.4(10) . . . . ?
N10 C53 C58 C57 175.8(5) . . . . ?
C54 C53 C58 C57 -1.4(9) . . . . ?
N10 C53 C58 O6 1.7(8) . . . . ?
C54 C53 C58 O6 -175.6(5) . . . . ?
C57 C58 O6 C60 106.2(6) . . . . ?
C53 C58 O6 C60 -79.5(6) . . . . ?
C64 C59 C60 C61 -1.2(7) . . . . ?
N11 C59 C60 C61 177.9(4) . . . . ?
C64 C59 C60 O6 174.0(4) . . . . ?
N11 C59 C60 O6 -7.0(6) . . . . ?
C58 O6 C60 C61 -62.3(6) . . . . ?
C58 O6 C60 C59 122.6(5) . . . . ?
C59 C60 C61 C62 -0.1(8) . . . . ?
O6 C60 C61 C62 -175.0(4) . . . . ?
C60 C61 C62 C63 1.6(8) . . . . ?
C61 C62 C63 C64 -1.6(8) . . . . ?
C60 C59 C64 C63 1.1(7) . . . . ?
N11 C59 C64 C63 -178.0(4) . . . . ?
C62 C63 C64 C59 0.3(8) . . . . ?
C60 C59 N11 Mo4 -71.3(5) . . . . ?
C64 C59 N11 Mo4 107.7(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N4 H4G O2 0.87(3) 2.57(4) 3.112(5) 122(4) .
N4 H4H Cl2 0.87(3) 2.48(3) 3.336(4) 165(4) .
N11 H11A Cl1 0.86(3) 2.58(3) 3.435(4) 172(5) .
N11 H11B Cl3 0.86(3) 2.52(5) 3.122(5) 127(4) .

_refine_diff_density_max         1.510
_refine_diff_density_min         -1.355
_refine_diff_density_rms         0.112

_shelxl_version_number           2014-3


#===END



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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 1061146'
_audit_update_record             
;
2015-04-22 deposited with the CCDC.
2015-06-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H18 Cl2 Mo N2 O3'
_chemical_formula_sum            'C16 H18 Cl2 Mo N2 O3'
_chemical_formula_weight         453.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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'

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

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

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

_cell_length_a                   14.6075(3)
_cell_length_b                   15.3236(3)
_cell_length_c                   32.3586(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7243.1(2)
_cell_formula_units_Z            16
_cell_measurement_temperature    148(2)
_cell_measurement_reflns_used    12724
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      3.033

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_F_000             3648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.036
_shelx_estimated_absorpt_T_min   0.746
_shelx_estimated_absorpt_T_max   0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      148(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47115
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         2.878
_diffrn_reflns_theta_max         29.139
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8867
_reflns_number_gt                6660
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0241P)²+7.8279P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_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         8867
_refine_ls_number_parameters     437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0791
_refine_ls_wR_factor_gt          0.0692
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.61293(2) 0.35274(2) 0.30607(2) 0.01791(7) Uani 1 1 d . . . . .
Cl1 Cl 0.52643(6) 0.45162(5) 0.26378(2) 0.02756(18) Uani 1 1 d . . . . .
Cl2 Cl 0.73955(6) 0.26913(5) 0.33209(2) 0.02825(18) Uani 1 1 d . . . . .
N1 N 0.58158(17) 0.39508(16) 0.35385(8) 0.0217(6) Uani 1 1 d . . . . .
C1 C 0.5336(2) 0.39263(19) 0.39071(9) 0.0192(6) Uani 1 1 d . . . . .
C2 C 0.5730(2) 0.4237(2) 0.42743(10) 0.0277(7) Uani 1 1 d . . . . .
H2 H 0.6307 0.4523 0.4268 0.033 Uiso 1 1 calc R U . . .
C3 C 0.5272(3) 0.4124(2) 0.46451(10) 0.0331(9) Uani 1 1 d . . . . .
H3 H 0.5546 0.4318 0.4895 0.040 Uiso 1 1 calc R U . . .
C4 C 0.4422(3) 0.3733(2) 0.46544(10) 0.0332(8) Uani 1 1 d . . . . .
H4 H 0.4121 0.3651 0.4912 0.040 Uiso 1 1 calc R U . . .
C5 C 0.4001(2) 0.3459(2) 0.42911(9) 0.0260(7) Uani 1 1 d . . . . .
H5 H 0.3404 0.3212 0.4297 0.031 Uiso 1 1 calc R U . . .
C6 C 0.4465(2) 0.35516(19) 0.39201(9) 0.0197(6) Uani 1 1 d . . . . .
O1 O 0.40521(14) 0.33119(13) 0.35473(6) 0.0200(4) Uani 1 1 d . . . . .
N2 N 0.53825(17) 0.26430(15) 0.30188(7) 0.0194(5) Uani 1 1 d . . . . .
C7 C 0.4701(2) 0.21089(19) 0.31733(9) 0.0190(6) Uani 1 1 d . . . . .
C8 C 0.4044(2) 0.24322(19) 0.34543(9) 0.0185(6) Uani 1 1 d . . . . .
C9 C 0.3383(2) 0.1883(2) 0.36165(9) 0.0232(7) Uani 1 1 d . . . . .
H9 H 0.2937 0.2106 0.3802 0.028 Uiso 1 1 calc R U . . .
C10 C 0.3372(2) 0.1005(2) 0.35080(10) 0.0258(7) Uani 1 1 d . . . . .
H10 H 0.2926 0.0626 0.3624 0.031 Uiso 1 1 calc R U . . .
C11 C 0.4009(2) 0.0680(2) 0.32325(10) 0.0248(7) Uani 1 1 d . . . . .
H11 H 0.4000 0.0079 0.3160 0.030 Uiso 1 1 calc R U . . .
C12 C 0.4659(2) 0.12264(19) 0.30613(9) 0.0227(7) Uani 1 1 d . . . . .
H12 H 0.5083 0.1001 0.2866 0.027 Uiso 1 1 calc R U . . .
C13 C 0.7238(3) 0.5420(2) 0.31400(12) 0.0419(10) Uani 1 1 d . . . . .
H13A H 0.7835 0.5711 0.3132 0.063 Uiso 1 1 calc R U . . .
H13B H 0.7039 0.5356 0.3428 0.063 Uiso 1 1 calc R U . . .
H13C H 0.6789 0.5771 0.2988 0.063 Uiso 1 1 calc R U . . .
O2 O 0.73114(15) 0.45725(13) 0.29522(6) 0.0260(5) Uani 1 1 d . . . . .
C14 C 0.7627(2) 0.4639(2) 0.25316(10) 0.0319(8) Uani 1 1 d . . . . .
H14A H 0.8215 0.4959 0.2521 0.038 Uiso 1 1 calc R U . . .
H14B H 0.7173 0.4959 0.2362 0.038 Uiso 1 1 calc R U . . .
C15 C 0.7748(2) 0.3733(2) 0.23688(10) 0.0305(8) Uani 1 1 d . . . . .
H15A H 0.7897 0.3753 0.2070 0.037 Uiso 1 1 calc R U . . .
H15B H 0.8258 0.3440 0.2515 0.037 Uiso 1 1 calc R U . . .
O3 O 0.69120(14) 0.32587(14) 0.24323(6) 0.0240(5) Uani 1 1 d . . . . .
C16 C 0.6994(2) 0.2381(2) 0.22825(10) 0.0341(8) Uani 1 1 d . . . . .
H16A H 0.7070 0.2390 0.1982 0.051 Uiso 1 1 calc R U . . .
H16B H 0.6440 0.2053 0.2354 0.051 Uiso 1 1 calc R U . . .
H16C H 0.7527 0.2102 0.2410 0.051 Uiso 1 1 calc R U . . .
Mo2 Mo 0.43244(2) 0.75867(2) 0.41408(2) 0.01865(7) Uani 1 1 d . . . . .
Cl3 Cl 0.33111(5) 0.85905(5) 0.37998(2) 0.02445(17) Uani 1 1 d . . . . .
Cl4 Cl 0.56564(6) 0.66912(5) 0.42409(2) 0.03002(18) Uani 1 1 d . . . . .
N3 N 0.44186(17) 0.81372(16) 0.46103(8) 0.0232(6) Uani 1 1 d . . . . .
C17 C 0.4238(2) 0.82420(19) 0.50278(9) 0.0203(6) Uani 1 1 d . . . . .
C18 C 0.4891(2) 0.8622(2) 0.52878(10) 0.0256(7) Uani 1 1 d . . . . .
H18 H 0.5450 0.8833 0.5176 0.031 Uiso 1 1 calc R U . . .
C19 C 0.4723(2) 0.8691(2) 0.57083(10) 0.0278(7) Uani 1 1 d . . . . .
H19 H 0.5175 0.8933 0.5885 0.033 Uiso 1 1 calc R U . . .
C20 C 0.3902(2) 0.8408(2) 0.58697(10) 0.0288(7) Uani 1 1 d . . . . .
H20 H 0.3791 0.8459 0.6158 0.035 Uiso 1 1 calc R U . . .
C21 C 0.3235(2) 0.8049(2) 0.56154(9) 0.0257(7) Uani 1 1 d . . . . .
H21 H 0.2667 0.7864 0.5728 0.031 Uiso 1 1 calc R U . . .
C22 C 0.3404(2) 0.79616(18) 0.51987(9) 0.0193(6) Uani 1 1 d . . . . .
O4 O 0.27278(13) 0.76499(13) 0.49328(6) 0.0198(4) Uani 1 1 d . . . . .
N4 N 0.35212(17) 0.67852(15) 0.42677(7) 0.0207(5) Uani 1 1 d . . . . .
C23 C 0.2993(2) 0.63337(18) 0.45484(9) 0.0187(6) Uani 1 1 d . . . . .
C24 C 0.2631(2) 0.67444(18) 0.49001(9) 0.0190(6) Uani 1 1 d . . . . .
C25 C 0.2147(2) 0.6277(2) 0.51923(9) 0.0239(7) Uani 1 1 d . . . . .
H25 H 0.1898 0.6563 0.5427 0.029 Uiso 1 1 calc R U . . .
C26 C 0.2028(2) 0.5384(2) 0.51390(10) 0.0281(7) Uani 1 1 d . . . . .
H26 H 0.1715 0.5056 0.5344 0.034 Uiso 1 1 calc R U . . .
C27 C 0.2359(2) 0.4967(2) 0.47895(10) 0.0276(7) Uani 1 1 d . . . . .
H27 H 0.2260 0.4359 0.4752 0.033 Uiso 1 1 calc R U . . .
C28 C 0.2836(2) 0.54377(19) 0.44958(10) 0.0246(7) Uani 1 1 d . . . . .
H28 H 0.3059 0.5152 0.4256 0.030 Uiso 1 1 calc R U . . .
C29 C 0.5604(3) 0.9274(2) 0.38722(11) 0.0356(9) Uani 1 1 d . . . . .
H29A H 0.6216 0.9422 0.3770 0.053 Uiso 1 1 calc R U . . .
H29B H 0.5591 0.9332 0.4174 0.053 Uiso 1 1 calc R U . . .
H29C H 0.5153 0.9669 0.3749 0.053 Uiso 1 1 calc R U . . .
O5 O 0.53904(14) 0.83968(13) 0.37610(6) 0.0235(5) Uani 1 1 d . . . . .
C30 C 0.5323(2) 0.8278(2) 0.33199(9) 0.0284(7) Uani 1 1 d . . . . .
H30A H 0.5867 0.8528 0.3181 0.034 Uiso 1 1 calc R U . . .
H30B H 0.4770 0.8573 0.3212 0.034 Uiso 1 1 calc R U . . .
C31 C 0.5269(2) 0.7320(2) 0.32418(10) 0.0287(7) Uani 1 1 d . . . . .
H31A H 0.5203 0.7206 0.2942 0.034 Uiso 1 1 calc R U . . .
H31B H 0.5834 0.7029 0.3340 0.034 Uiso 1 1 calc R U . . .
O6 O 0.44844(14) 0.69911(13) 0.34624(6) 0.0229(5) Uani 1 1 d . . . . .
C32 C 0.4397(2) 0.6057(2) 0.34120(11) 0.0334(8) Uani 1 1 d . . . . .
H32A H 0.4378 0.5914 0.3117 0.050 Uiso 1 1 calc R U . . .
H32B H 0.3831 0.5858 0.3545 0.050 Uiso 1 1 calc R U . . .
H32C H 0.4923 0.5766 0.3540 0.050 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 N1 1.738(2) . ?
Mo1 N2 1.745(2) . ?
Mo1 O3 2.369(2) . ?
Mo1 O2 2.381(2) . ?
Mo1 Cl1 2.4012(8) . ?
Mo1 Cl2 2.4024(8) . ?
N1 C1 1.384(4) . ?
C1 C6 1.397(4) . ?
C1 C2 1.403(4) . ?
C2 C3 1.385(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C6 O1 1.398(3) . ?
O1 C8 1.381(3) . ?
N2 C7 1.382(4) . ?
C7 C12 1.401(4) . ?
C7 C8 1.412(4) . ?
C8 C9 1.385(4) . ?
C9 C10 1.391(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 O2 1.438(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
O2 C14 1.440(4) . ?
C14 C15 1.495(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 O3 1.436(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
O3 C16 1.434(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
Mo2 N3 1.743(2) . ?
Mo2 N4 1.748(2) . ?
Mo2 O5 2.340(2) . ?
Mo2 O6 2.389(2) . ?
Mo2 Cl4 2.4029(8) . ?
Mo2 Cl3 2.4030(8) . ?
N3 C17 1.386(4) . ?
C17 C18 1.399(4) . ?
C17 C22 1.405(4) . ?
C18 C19 1.387(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.389(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.377(4) . ?
C21 H21 0.9500 . ?
C22 O4 1.394(3) . ?
O4 C24 1.399(3) . ?
N4 C23 1.378(4) . ?
C23 C28 1.402(4) . ?
C23 C24 1.404(4) . ?
C24 C25 1.382(4) . ?
C25 C26 1.390(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.387(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.381(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 O5 1.426(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O5 C30 1.442(4) . ?
C30 C31 1.491(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 O6 1.442(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
O6 C32 1.447(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Mo1 N2 101.21(11) . . ?
N1 Mo1 O3 162.86(10) . . ?
N2 Mo1 O3 95.74(9) . . ?
N1 Mo1 O2 94.08(10) . . ?
N2 Mo1 O2 164.63(9) . . ?
O3 Mo1 O2 68.92(7) . . ?
N1 Mo1 Cl1 97.63(8) . . ?
N2 Mo1 Cl1 96.71(8) . . ?
O3 Mo1 Cl1 82.78(5) . . ?
O2 Mo1 Cl1 82.71(6) . . ?
N1 Mo1 Cl2 95.18(9) . . ?
N2 Mo1 Cl2 95.42(8) . . ?
O3 Mo1 Cl2 80.60(5) . . ?
O2 Mo1 Cl2 81.49(6) . . ?
Cl1 Mo1 Cl2 160.30(3) . . ?
C1 N1 Mo1 152.9(2) . . ?
N1 C1 C6 119.9(3) . . ?
N1 C1 C2 120.9(3) . . ?
C6 C1 C2 119.2(3) . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C4 C3 C2 120.6(3) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 119.0(3) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C1 120.9(3) . . ?
C5 C6 O1 120.6(3) . . ?
C1 C6 O1 118.4(3) . . ?
C8 O1 C6 116.6(2) . . ?
C7 N2 Mo1 151.9(2) . . ?
N2 C7 C12 120.6(3) . . ?
N2 C7 C8 121.0(3) . . ?
C12 C7 C8 118.4(3) . . ?
O1 C8 C9 121.1(3) . . ?
O1 C8 C7 118.5(3) . . ?
C9 C8 C7 120.3(3) . . ?
C8 C9 C10 120.0(3) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 120.2(3) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.3(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C7 120.7(3) . . ?
C11 C12 H12 119.6 . . ?
C7 C12 H12 119.6 . . ?
O2 C13 H13A 109.5 . . ?
O2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C13 O2 C14 111.1(2) . . ?
C13 O2 Mo1 119.4(2) . . ?
C14 O2 Mo1 114.75(18) . . ?
O2 C14 C15 107.8(3) . . ?
O2 C14 H14A 110.2 . . ?
C15 C14 H14A 110.2 . . ?
O2 C14 H14B 110.2 . . ?
C15 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O3 C15 C14 108.6(3) . . ?
O3 C15 H15A 110.0 . . ?
C14 C15 H15A 110.0 . . ?
O3 C15 H15B 110.0 . . ?
C14 C15 H15B 110.0 . . ?
H15A C15 H15B 108.4 . . ?
C16 O3 C15 110.8(2) . . ?
C16 O3 Mo1 119.56(18) . . ?
C15 O3 Mo1 116.45(17) . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 Mo2 N4 100.85(11) . . ?
N3 Mo2 O5 98.54(10) . . ?
N4 Mo2 O5 160.56(9) . . ?
N3 Mo2 O6 167.98(10) . . ?
N4 Mo2 O6 90.75(9) . . ?
O5 Mo2 O6 69.81(7) . . ?
N3 Mo2 Cl4 95.45(9) . . ?
N4 Mo2 Cl4 96.35(8) . . ?
O5 Mo2 Cl4 80.50(6) . . ?
O6 Mo2 Cl4 80.01(5) . . ?
N3 Mo2 Cl3 97.99(9) . . ?
N4 Mo2 Cl3 98.29(8) . . ?
O5 Mo2 Cl3 80.17(6) . . ?
O6 Mo2 Cl3 83.28(5) . . ?
Cl4 Mo2 Cl3 157.86(3) . . ?
C17 N3 Mo2 153.0(2) . . ?
N3 C17 C18 120.3(3) . . ?
N3 C17 C22 120.9(3) . . ?
C18 C17 C22 118.8(3) . . ?
C19 C18 C17 120.1(3) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C20 C19 C18 120.1(3) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 120.7(3) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.7 . . ?
C22 C21 C20 119.5(3) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C21 C22 O4 120.7(3) . . ?
C21 C22 C17 120.7(3) . . ?
O4 C22 C17 118.4(3) . . ?
C22 O4 C24 117.3(2) . . ?
C23 N4 Mo2 152.1(2) . . ?
N4 C23 C28 120.2(3) . . ?
N4 C23 C24 121.3(3) . . ?
C28 C23 C24 118.4(3) . . ?
C25 C24 O4 121.0(3) . . ?
C25 C24 C23 121.0(3) . . ?
O4 C24 C23 117.9(2) . . ?
C24 C25 C26 119.3(3) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C27 C26 C25 120.8(3) . . ?
C27 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C28 C27 C26 119.8(3) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C27 C28 C23 120.7(3) . . ?
C27 C28 H28 119.7 . . ?
C23 C28 H28 119.7 . . ?
O5 C29 H29A 109.5 . . ?
O5 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O5 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C29 O5 C30 112.6(2) . . ?
C29 O5 Mo2 120.87(19) . . ?
C30 O5 Mo2 114.05(18) . . ?
O5 C30 C31 107.2(2) . . ?
O5 C30 H30A 110.3 . . ?
C31 C30 H30A 110.3 . . ?
O5 C30 H30B 110.3 . . ?
C31 C30 H30B 110.3 . . ?
H30A C30 H30B 108.5 . . ?
O6 C31 C30 107.6(2) . . ?
O6 C31 H31A 110.2 . . ?
C30 C31 H31A 110.2 . . ?
O6 C31 H31B 110.2 . . ?
C30 C31 H31B 110.2 . . ?
H31A C31 H31B 108.5 . . ?
C31 O6 C32 111.1(2) . . ?
C31 O6 Mo2 113.53(18) . . ?
C32 O6 Mo2 118.23(18) . . ?
O6 C32 H32A 109.5 . . ?
O6 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O6 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Mo1 N1 C1 7.5(5) . . . . ?
O3 Mo1 N1 C1 -163.8(3) . . . . ?
O2 Mo1 N1 C1 -170.9(5) . . . . ?
Cl1 Mo1 N1 C1 105.9(5) . . . . ?
Cl2 Mo1 N1 C1 -89.1(5) . . . . ?
Mo1 N1 C1 C6 -33.4(6) . . . . ?
Mo1 N1 C1 C2 143.6(4) . . . . ?
N1 C1 C2 C3 -173.5(3) . . . . ?
C6 C1 C2 C3 3.5(4) . . . . ?
C1 C2 C3 C4 -2.0(5) . . . . ?
C2 C3 C4 C5 -1.1(5) . . . . ?
C3 C4 C5 C6 2.6(5) . . . . ?
C4 C5 C6 C1 -1.0(5) . . . . ?
C4 C5 C6 O1 -177.7(3) . . . . ?
N1 C1 C6 C5 175.0(3) . . . . ?
C2 C1 C6 C5 -2.1(4) . . . . ?
N1 C1 C6 O1 -8.2(4) . . . . ?
C2 C1 C6 O1 174.8(2) . . . . ?
C5 C6 O1 C8 -79.2(3) . . . . ?
C1 C6 O1 C8 103.9(3) . . . . ?
N1 Mo1 N2 C7 -2.9(5) . . . . ?
O3 Mo1 N2 C7 174.5(4) . . . . ?
O2 Mo1 N2 C7 171.0(3) . . . . ?
Cl1 Mo1 N2 C7 -102.1(5) . . . . ?
Cl2 Mo1 N2 C7 93.5(5) . . . . ?
Mo1 N2 C7 C12 -149.0(4) . . . . ?
Mo1 N2 C7 C8 29.6(6) . . . . ?
C6 O1 C8 C9 82.7(3) . . . . ?
C6 O1 C8 C7 -100.3(3) . . . . ?
N2 C7 C8 O1 5.0(4) . . . . ?
C12 C7 C8 O1 -176.4(3) . . . . ?
N2 C7 C8 C9 -178.0(3) . . . . ?
C12 C7 C8 C9 0.6(4) . . . . ?
O1 C8 C9 C10 178.0(3) . . . . ?
C7 C8 C9 C10 1.0(4) . . . . ?
C8 C9 C10 C11 -1.2(5) . . . . ?
C9 C10 C11 C12 -0.2(5) . . . . ?
C10 C11 C12 C7 1.9(5) . . . . ?
N2 C7 C12 C11 176.5(3) . . . . ?
C8 C7 C12 C11 -2.1(4) . . . . ?
C13 O2 C14 C15 176.0(3) . . . . ?
Mo1 O2 C14 C15 -44.8(3) . . . . ?
O2 C14 C15 O3 53.3(3) . . . . ?
C14 C15 O3 C16 -179.8(3) . . . . ?
C14 C15 O3 Mo1 -38.6(3) . . . . ?
N4 Mo2 N3 C17 7.0(5) . . . . ?
O5 Mo2 N3 C17 -171.7(5) . . . . ?
O6 Mo2 N3 C17 -157.7(4) . . . . ?
Cl4 Mo2 N3 C17 -90.6(5) . . . . ?
Cl3 Mo2 N3 C17 107.1(5) . . . . ?
Mo2 N3 C17 C18 147.2(4) . . . . ?
Mo2 N3 C17 C22 -32.1(7) . . . . ?
N3 C17 C18 C19 -177.2(3) . . . . ?
C22 C17 C18 C19 2.1(4) . . . . ?
C17 C18 C19 C20 -1.8(5) . . . . ?
C18 C19 C20 C21 0.2(5) . . . . ?
C19 C20 C21 C22 1.0(5) . . . . ?
C20 C21 C22 O4 -176.3(3) . . . . ?
C20 C21 C22 C17 -0.8(5) . . . . ?
N3 C17 C22 C21 178.5(3) . . . . ?
C18 C17 C22 C21 -0.8(4) . . . . ?
N3 C17 C22 O4 -5.9(4) . . . . ?
C18 C17 C22 O4 174.8(3) . . . . ?
C21 C22 O4 C24 -83.8(3) . . . . ?
C17 C22 O4 C24 100.5(3) . . . . ?
N3 Mo2 N4 C23 -9.3(5) . . . . ?
O5 Mo2 N4 C23 166.9(3) . . . . ?
O6 Mo2 N4 C23 167.6(5) . . . . ?
Cl4 Mo2 N4 C23 87.5(5) . . . . ?
Cl3 Mo2 N4 C23 -109.1(5) . . . . ?
Mo2 N4 C23 C28 -143.4(4) . . . . ?
Mo2 N4 C23 C24 34.0(6) . . . . ?
C22 O4 C24 C25 81.1(3) . . . . ?
C22 O4 C24 C23 -102.7(3) . . . . ?
N4 C23 C24 C25 -176.2(3) . . . . ?
C28 C23 C24 C25 1.3(4) . . . . ?
N4 C23 C24 O4 7.6(4) . . . . ?
C28 C23 C24 O4 -174.9(3) . . . . ?
O4 C24 C25 C26 176.9(3) . . . . ?
C23 C24 C25 C26 0.9(5) . . . . ?
C24 C25 C26 C27 -2.4(5) . . . . ?
C25 C26 C27 C28 1.8(5) . . . . ?
C26 C27 C28 C23 0.4(5) . . . . ?
N4 C23 C28 C27 175.6(3) . . . . ?
C24 C23 C28 C27 -1.9(4) . . . . ?
C29 O5 C30 C31 169.9(3) . . . . ?
Mo2 O5 C30 C31 -47.6(3) . . . . ?
O5 C30 C31 O6 58.1(3) . . . . ?
C30 C31 O6 C32 -178.4(3) . . . . ?
C30 C31 O6 Mo2 -42.2(3) . . . . ?

_refine_diff_density_max         0.681
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.106

_exptl_crystal_recrystallization_method 
'From the mother liquor of trimethylsilyl chloride and 1,2-dimethoxyethane'
