# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_2
_database_code_depnum_ccdc_archive 'CCDC 1491993'
_audit_update_record             
;
2017-04-30 deposited with the CCDC.
2017-05-03 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         ?
_chemical_formula_sum            'C8 H20 Cl8 Mo2 N2 O2'
_chemical_formula_weight         651.74

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'

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

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

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

_cell_length_a                   8.449(3)
_cell_length_b                   13.113(4)
_cell_length_c                   9.937(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.064(3)
_cell_angle_gamma                90
_cell_volume                     1076.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5052
_cell_measurement_theta_min      2.609
_cell_measurement_theta_max      28.290

_exptl_crystal_description       needle
_exptl_crystal_colour            green-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_F_000             636
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.161
_shelx_estimated_absorpt_T_min   0.684
_shelx_estimated_absorpt_T_max   0.813
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6842
_exptl_absorpt_correction_T_max  0.8129
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1378 (selected reflections only, before parameter refinement)
 R(int) =  0.0638 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11565
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.609
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2351
_reflns_number_gt                2053
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+(0.0272P)²+0.9275P] 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         2351
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0682
_refine_ls_wR_factor_gt          0.0648
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
C1 C 0.3531(4) 0.2127(3) 0.4106(4) 0.0334(8) Uani 1 1 d . . . . .
H1A H 0.3484 0.2721 0.4711 0.040 Uiso 1 1 calc R U . . .
H1B H 0.4481 0.1708 0.4527 0.040 Uiso 1 1 calc R U . . .
C2 C 0.2014(4) 0.1506(3) 0.3975(3) 0.0319(7) Uani 1 1 d . . . . .
H2A H 0.1905 0.1273 0.4888 0.048 Uiso 1 1 calc R U . . .
H2B H 0.1077 0.1926 0.3567 0.048 Uiso 1 1 calc R U . . .
H2C H 0.2071 0.0915 0.3384 0.048 Uiso 1 1 calc R U . . .
C3 C 0.3330(6) 0.3368(3) 0.2248(5) 0.0558(11) Uani 1 1 d . . . . .
H3 H 0.2980 0.3866 0.2817 0.067 Uiso 1 1 calc R U . . .
C4 C 0.3418(5) 0.3648(3) 0.0835(4) 0.0378(8) Uani 1 1 d . . . . .
H4A H 0.3081 0.4359 0.0663 0.057 Uiso 1 1 calc R U . . .
H4B H 0.4533 0.3567 0.0714 0.057 Uiso 1 1 calc R U . . .
H4C H 0.2700 0.3204 0.0186 0.057 Uiso 1 1 calc R U . . .
Cl1 Cl 0.32022(9) 0.58061(6) 0.47142(8) 0.03025(19) Uani 1 1 d . . . . .
Cl2 Cl 0.22485(10) 0.70175(6) 0.73099(8) 0.02914(18) Uani 1 1 d . . . . .
Cl3 Cl 0.01340(10) 0.50880(7) 0.80222(8) 0.0339(2) Uani 1 1 d . . . . .
Cl4 Cl 0.08118(9) 0.38670(5) 0.52548(8) 0.02458(17) Uani 1 1 d . . . . .
Mo1 Mo 0.19882(3) 0.53228(2) 0.65652(3) 0.02106(9) Uani 1 1 d . . . . .
N1 N 0.3706(4) 0.2481(3) 0.2738(4) 0.0474(8) Uani 1 1 d . . . . .
H1 H 0.4100 0.2046 0.2218 0.057 Uiso 1 1 calc R U . . .
O1 O 0.3572(3) 0.47711(17) 0.7545(2) 0.0336(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.472(5) . ?
C1 C2 1.501(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 N1 1.276(5) . ?
C3 C4 1.467(6) . ?
C3 H3 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
Cl1 Mo1 2.3718(10) . ?
Cl2 Mo1 2.3380(11) . ?
Cl3 Mo1 2.3650(10) . ?
Cl4 Mo1 2.4055(9) . ?
Mo1 O1 1.648(2) . ?
N1 H1 0.8800 . ?

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 C1 C2 109.8(3) . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
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 . . ?
N1 C3 C4 122.3(4) . . ?
N1 C3 H3 118.8 . . ?
C4 C3 H3 118.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O1 Mo1 Cl2 102.66(9) . . ?
O1 Mo1 Cl3 98.09(9) . . ?
Cl2 Mo1 Cl3 87.74(3) . . ?
O1 Mo1 Cl1 98.42(9) . . ?
Cl2 Mo1 Cl1 87.95(3) . . ?
Cl3 Mo1 Cl1 163.47(3) . . ?
O1 Mo1 Cl4 99.44(9) . . ?
Cl2 Mo1 Cl4 157.89(3) . . ?
Cl3 Mo1 Cl4 88.65(3) . . ?
Cl1 Mo1 Cl4 89.37(3) . . ?
C3 N1 C1 125.1(4) . . ?
C3 N1 H1 117.5 . . ?
C1 N1 H1 117.5 . . ?

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
C4 C3 N1 C1 -175.3(4) . . . . ?
C2 C1 N1 C3 99.5(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 H1 Cl4 0.88 2.92 3.770(3) 163.7 4_665
N1 H1 Cl3 0.88 2.99 3.569(4) 125.1 4_665
N1 H1 Cl1 0.88 2.92 3.423(4) 117.7 2_545

_refine_diff_density_max         0.756
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.097

####################################################################### 
# 
# 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 1491992'
_audit_update_record             
;
2017-04-30 deposited with the CCDC.
2017-05-03 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         ?
_chemical_formula_sum            'C4 H7 Cl5 Mo N'
_chemical_formula_weight         342.30

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

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

_cell_length_a                   11.8263(17)
_cell_length_b                   8.2825(12)
_cell_length_c                   10.2388(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1002.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5841
_cell_measurement_theta_min      3.0025
_cell_measurement_theta_max      28.4955

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_F_000             660
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    2.577
_shelx_estimated_absorpt_T_min   0.640
_shelx_estimated_absorpt_T_max   0.747
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6403
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1423 (selected reflections only, before parameter refinement)
 R(int) =  0.0584 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10237
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.003
_diffrn_reflns_theta_max         26.990
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2180
_reflns_number_gt                2096
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+(0.0092P)²+0.3630P] 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 941 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2180
_refine_ls_number_parameters     100
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0227
_refine_ls_wR_factor_ref         0.0398
_refine_ls_wR_factor_gt          0.0392
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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
C1 C 0.9745(4) 0.7389(6) 1.0100(5) 0.0156(10) Uani 1 1 d . . . . .
H1 H 1.0163 0.8309 1.0372 0.019 Uiso 1 1 calc R U . . .
C2 C 0.9934(4) 0.5766(6) 1.0667(5) 0.0181(11) Uani 1 1 d . . . . .
H2A H 0.9641 0.5699 1.1571 0.022 Uiso 1 1 calc R U . . .
H2B H 1.0747 0.5478 1.0664 0.022 Uiso 1 1 calc R U . . .
C3 C 0.9252(4) 0.4680(6) 0.9733(5) 0.0195(11) Uani 1 1 d . . . . .
H3A H 0.9759 0.4108 0.9118 0.023 Uiso 1 1 calc R U . . .
H3B H 0.8805 0.3873 1.0225 0.023 Uiso 1 1 calc R U . . .
C4 C 0.8480(4) 0.5852(6) 0.9007(5) 0.0203(11) Uani 1 1 d . . . . .
H4A H 0.8456 0.5590 0.8064 0.024 Uiso 1 1 calc R U . . .
H4B H 0.7702 0.5804 0.9362 0.024 Uiso 1 1 calc R U . . .
Cl1 Cl 0.66602(9) 0.85092(13) 0.80248(13) 0.0171(3) Uani 1 1 d . . . . .
Cl2 Cl 0.89908(10) 0.82572(14) 0.64077(12) 0.0181(3) Uani 1 1 d . . . . .
Cl3 Cl 1.02697(8) 1.07026(12) 0.83135(15) 0.0168(2) Uani 1 1 d . . . . .
Cl4 Cl 0.80745(10) 1.05111(14) 1.02806(12) 0.0170(2) Uani 1 1 d . . . . .
Cl5 Cl 0.78103(10) 1.19781(14) 0.71978(13) 0.0207(3) Uani 1 1 d . . . . .
Mo1 Mo 0.84423(3) 0.96729(4) 0.82098(5) 0.01187(9) Uani 1 1 d . . . . .
N1 N 0.8978(3) 0.7466(5) 0.9218(4) 0.0134(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.281(6) . ?
C1 C2 1.481(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.541(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.526(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N1 1.477(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
Cl1 Mo1 2.3252(11) . ?
Cl2 Mo1 2.2804(13) . ?
Cl3 Mo1 2.3257(11) . ?
Cl4 Mo1 2.2730(13) . ?
Cl5 Mo1 2.2973(12) . ?
Mo1 N1 2.193(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 115.4(4) . . ?
N1 C1 H1 122.3 . . ?
C2 C1 H1 122.3 . . ?
C1 C2 C3 102.0(4) . . ?
C1 C2 H2A 111.4 . . ?
C3 C2 H2A 111.4 . . ?
C1 C2 H2B 111.4 . . ?
C3 C2 H2B 111.4 . . ?
H2A C2 H2B 109.2 . . ?
C4 C3 C2 104.1(4) . . ?
C4 C3 H3A 110.9 . . ?
C2 C3 H3A 110.9 . . ?
C4 C3 H3B 110.9 . . ?
C2 C3 H3B 110.9 . . ?
H3A C3 H3B 109.0 . . ?
N1 C4 C3 105.4(4) . . ?
N1 C4 H4A 110.7 . . ?
C3 C4 H4A 110.7 . . ?
N1 C4 H4B 110.7 . . ?
C3 C4 H4B 110.7 . . ?
H4A C4 H4B 108.8 . . ?
N1 Mo1 Cl4 82.56(10) . . ?
N1 Mo1 Cl2 82.55(10) . . ?
Cl4 Mo1 Cl2 165.07(5) . . ?
N1 Mo1 Cl5 177.62(11) . . ?
Cl4 Mo1 Cl5 96.01(5) . . ?
Cl2 Mo1 Cl5 98.91(5) . . ?
N1 Mo1 Cl1 87.41(10) . . ?
Cl4 Mo1 Cl1 91.67(4) . . ?
Cl2 Mo1 Cl1 88.78(5) . . ?
Cl5 Mo1 Cl1 90.74(4) . . ?
N1 Mo1 Cl3 90.89(10) . . ?
Cl4 Mo1 Cl3 91.33(5) . . ?
Cl2 Mo1 Cl3 87.78(5) . . ?
Cl5 Mo1 Cl3 91.04(4) . . ?
Cl1 Mo1 Cl3 176.33(5) . . ?
C1 N1 C4 109.9(4) . . ?
C1 N1 Mo1 125.3(3) . . ?
C4 N1 Mo1 124.8(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
N1 C1 C2 C3 11.0(5) . . . . ?
C1 C2 C3 C4 -16.6(5) . . . . ?
C2 C3 C4 N1 17.2(5) . . . . ?
C2 C1 N1 C4 0.0(6) . . . . ?
C2 C1 N1 Mo1 178.3(3) . . . . ?
C3 C4 N1 C1 -11.3(5) . . . . ?
C3 C4 N1 Mo1 170.4(3) . . . . ?

_refine_diff_density_max         0.416
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.083

####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1511407'
_audit_update_record             
;
2017-04-30 deposited with the CCDC.
2017-05-03 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         ?
_chemical_formula_sum            'C12 H32 Cl9.60 Mo2 N2 O0.40'
_chemical_formula_weight         742.99

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

_cell_length_a                   13.8611(7)
_cell_length_b                   13.6266(7)
_cell_length_c                   14.1240(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2667.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9971
_cell_measurement_theta_min      2.5435
_cell_measurement_theta_max      29.2245

_exptl_crystal_description       prism
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.850
_exptl_crystal_F_000             1474
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    1.907
_shelx_estimated_absorpt_T_min   0.725
_shelx_estimated_absorpt_T_max   0.790
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6743
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1504 (selected reflections only, before parameter refinement)
 R(int) =  0.0494 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30112
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.544
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2888
_reflns_number_gt                2770
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+99.2501P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2888
_refine_ls_number_parameters     124
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0803
_refine_ls_wR_factor_ref         0.1913
_refine_ls_wR_factor_gt          0.1909
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_restrained_S_all      1.212
_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 0.99553(9) 0.86680(9) 0.04057(9) 0.0160(3) Uani 0.8 1 d . . P A .
Cl1 Cl 0.97864(17) 0.8038(2) 0.19162(17) 0.0253(5) Uani 1 1 d . . . . .
Cl2 Cl 1.16221(16) 0.87492(19) 0.05861(17) 0.0242(5) Uani 1 1 d . . . . .
Cl3 Cl 1.0019(3) 0.7217(2) -0.0321(3) 0.0352(7) Uani 0.8 1 d . . P A 1
Cl4 Cl 0.82810(16) 0.88077(19) 0.02335(16) 0.0214(5) Uani 1 1 d . . . . .
Cl5 Cl 0.98994(16) 1.04214(17) 0.11006(16) 0.0190(5) Uani 1 1 d . . . . .
N1 N 0.7438(6) 0.9269(6) 0.8107(5) 0.0186(16) Uani 1 1 d . . . . .
H1 H 0.7822 0.9485 0.8585 0.022 Uiso 1 1 d R U . . .
C1 C 0.7831(7) 0.8284(7) 0.7824(7) 0.0203(19) Uani 1 1 d . . . . .
H1A H 0.7801 0.7837 0.8375 0.024 Uiso 1 1 calc R U . . .
H1B H 0.8518 0.8359 0.7645 0.024 Uiso 1 1 calc R U . . .
C2 C 0.7291(8) 0.7825(8) 0.7008(7) 0.028(2) Uani 1 1 d . . . . .
H2A H 0.7588 0.7194 0.6847 0.042 Uiso 1 1 calc R U . . .
H2B H 0.7319 0.8263 0.6458 0.042 Uiso 1 1 calc R U . . .
H2C H 0.6617 0.7721 0.7190 0.042 Uiso 1 1 calc R U . . .
C3 C 0.7468(7) 1.0018(7) 0.7318(6) 0.0212(19) Uani 1 1 d . . . . .
H3A H 0.7273 1.0665 0.7574 0.025 Uiso 1 1 calc R U . . .
H3B H 0.6994 0.9831 0.6826 0.025 Uiso 1 1 calc R U . . .
C4 C 0.8458(7) 1.0110(8) 0.6868(7) 0.025(2) Uani 1 1 d . . . . .
H4A H 0.8470 1.0686 0.6452 0.038 Uiso 1 1 calc R U . . .
H4B H 0.8596 0.9519 0.6496 0.038 Uiso 1 1 calc R U . . .
H4C H 0.8946 1.0185 0.7365 0.038 Uiso 1 1 calc R U . . .
C5 C 0.6425(7) 0.9157(8) 0.8516(7) 0.022(2) Uani 1 1 d . . . . .
H5A H 0.5977 0.8966 0.8002 0.026 Uiso 1 1 calc R U . . .
H5B H 0.6429 0.8621 0.8990 0.026 Uiso 1 1 calc R U . . .
C6 C 0.6057(8) 1.0076(8) 0.8977(8) 0.029(2) Uani 1 1 d . . . . .
H6A H 0.5425 0.9948 0.9263 0.044 Uiso 1 1 calc R U . . .
H6B H 0.5994 1.0594 0.8500 0.044 Uiso 1 1 calc R U . . .
H6C H 0.6510 1.0286 0.9469 0.044 Uiso 1 1 calc R U . . .
Mo2 Mo 0.9946(4) 0.8320(4) 0.0262(4) 0.0160(3) Uani 0.2 1 d . . P A .
O3 O 1.0019(3) 0.7217(2) -0.0321(3) 0.0352(7) Uani 0.2 1 d . . 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 Mo2 0.516(5) . ?
Mo1 O3 2.229(3) . ?
Mo1 Cl3 2.229(3) . ?
Mo1 Cl1 2.312(3) . ?
Mo1 Cl2 2.327(3) . ?
Mo1 Cl4 2.341(3) . ?
Mo1 Cl5 2.471(3) 5_775 ?
Mo1 Cl5 2.584(3) . ?
Cl1 Mo2 2.379(6) . ?
Cl2 Mo2 2.439(6) . ?
Cl3 Mo2 1.717(6) . ?
Cl4 Mo2 2.401(6) . ?
Cl5 Mo1 2.471(3) 5_775 ?
Cl5 Mo2 2.586(6) 5_775 ?
N1 C1 1.503(12) . ?
N1 C3 1.511(12) . ?
N1 C5 1.527(12) . ?
N1 H1 0.9081 . ?
C1 C2 1.509(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.518(13) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.501(14) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
Mo2 O3 1.717(6) . ?
Mo2 Cl5 2.586(6) 5_775 ?

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
Mo2 Mo1 O3 5.6(7) . . ?
Mo2 Mo1 Cl3 5.6(7) . . ?
Mo2 Mo1 Cl1 91.2(7) . . ?
O3 Mo1 Cl1 95.69(12) . . ?
Cl3 Mo1 Cl1 95.69(12) . . ?
Mo2 Mo1 Cl2 96.5(8) . . ?
O3 Mo1 Cl2 93.06(12) . . ?
Cl3 Mo1 Cl2 93.06(12) . . ?
Cl1 Mo1 Cl2 90.99(10) . . ?
Mo2 Mo1 Cl4 90.5(8) . . ?
O3 Mo1 Cl4 93.64(12) . . ?
Cl3 Mo1 Cl4 93.64(12) . . ?
Cl1 Mo1 Cl4 91.47(9) . . ?
Cl2 Mo1 Cl4 172.61(11) . . ?
Mo2 Mo1 Cl5 97.1(8) . 5_775 ?
O3 Mo1 Cl5 92.63(11) . 5_775 ?
Cl3 Mo1 Cl5 92.63(11) . 5_775 ?
Cl1 Mo1 Cl5 171.63(10) . 5_775 ?
Cl2 Mo1 Cl5 89.40(9) . 5_775 ?
Cl4 Mo1 Cl5 87.16(8) . 5_775 ?
Mo2 Mo1 Cl5 176.7(8) . . ?
O3 Mo1 Cl5 174.89(12) . . ?
Cl3 Mo1 Cl5 174.89(12) . . ?
Cl1 Mo1 Cl5 89.42(9) . . ?
Cl2 Mo1 Cl5 86.80(9) . . ?
Cl4 Mo1 Cl5 86.25(9) . . ?
Cl5 Mo1 Cl5 82.25(8) 5_775 . ?
Mo1 Cl1 Mo2 12.52(12) . . ?
Mo1 Cl2 Mo2 12.12(12) . . ?
Mo2 Cl3 Mo1 1.7(2) . . ?
Mo1 Cl4 Mo2 12.40(12) . . ?
Mo1 Cl5 Mo1 97.75(8) 5_775 . ?
Mo1 Cl5 Mo2 11.41(12) 5_775 5_775 ?
Mo1 Cl5 Mo2 109.14(15) . 5_775 ?
C1 N1 C3 113.4(7) . . ?
C1 N1 C5 110.1(8) . . ?
C3 N1 C5 111.8(7) . . ?
C1 N1 H1 106.0 . . ?
C3 N1 H1 108.3 . . ?
C5 N1 H1 106.8 . . ?
N1 C1 C2 113.2(8) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
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 . . ?
N1 C3 C4 112.9(8) . . ?
N1 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
N1 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N1 113.1(8) . . ?
C6 C5 H5A 108.9 . . ?
N1 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
N1 C5 H5B 108.9 . . ?
H5A C5 H5B 107.8 . . ?
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 . . ?
Mo1 Mo2 O3 172.7(10) . . ?
Mo1 Mo2 Cl3 172.7(10) . . ?
Mo1 Mo2 Cl1 76.3(7) . . ?
O3 Mo2 Cl1 109.5(3) . . ?
Cl3 Mo2 Cl1 109.5(3) . . ?
Mo1 Mo2 Cl4 77.1(7) . . ?
O3 Mo2 Cl4 106.9(3) . . ?
Cl3 Mo2 Cl4 106.9(3) . . ?
Cl1 Mo2 Cl4 88.4(2) . . ?
Mo1 Mo2 Cl2 71.4(7) . . ?
O3 Mo2 Cl2 104.1(3) . . ?
Cl3 Mo2 Cl2 104.1(3) . . ?
Cl1 Mo2 Cl2 86.7(2) . . ?
Cl4 Mo2 Cl2 148.5(3) . . ?
Mo1 Mo2 Cl5 71.5(7) . 5_775 ?
O3 Mo2 Cl5 102.7(3) . 5_775 ?
Cl3 Mo2 Cl5 102.7(3) . 5_775 ?
Cl1 Mo2 Cl5 147.8(3) . 5_775 ?
Cl4 Mo2 Cl5 83.35(19) . 5_775 ?
Cl2 Mo2 Cl5 84.37(19) . 5_775 ?
Mo2 O3 Mo1 1.7(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 Cl2 0.91 2.78 3.520(9) 138.9 5_776
N1 H1 Cl4 0.91 2.58 3.283(8) 134.3 1_556
C1 H1B Cl1 0.99 2.79 3.498(10) 129.1 7_576
C2 H2A Cl4 0.98 2.83 3.622(11) 138.9 7_576
C3 H3B Cl4 0.99 2.94 3.508(10) 117.4 2_675
C3 H3B Cl5 0.99 2.84 3.753(10) 153.8 2_675
C4 H4C Cl5 0.98 2.82 3.734(10) 155.8 5_776
C5 H5B Cl3 0.99 2.94 3.715(10) 135.6 4_466
C6 H6C Cl2 0.98 2.90 3.646(11) 133.3 5_776

_refine_diff_density_max         2.147
_refine_diff_density_min         -2.430
_refine_diff_density_rms         0.253

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

data_6
_database_code_depnum_ccdc_archive 'CCDC 1511406'
_audit_update_record             
;
2017-04-30 deposited with the CCDC.
2017-05-03 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         ?
_chemical_formula_sum            'C43 H42 Cl8 Mo N2'
_chemical_formula_weight         966.32

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'
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'

_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                   10.0833(9)
_cell_length_b                   13.2029(10)
_cell_length_c                   16.6033(12)
_cell_angle_alpha                90
_cell_angle_beta                 103.818(6)
_cell_angle_gamma                90
_cell_volume                     2146.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3427
_cell_measurement_theta_min      2.5265
_cell_measurement_theta_max      25.4345

_exptl_crystal_description       needle
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.837
_shelx_estimated_absorpt_T_min   0.892
_shelx_estimated_absorpt_T_max   0.921
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8918
_exptl_absorpt_correction_T_max  0.9210
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1219 (selected reflections only, before parameter refinement)
 R(int) =  0.0768 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30144
_diffrn_reflns_av_unetI/netI     0.1445
_diffrn_reflns_av_R_equivalents  0.2415
_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       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.994
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_full        25.025
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3791
_reflns_number_gt                1622
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+(0.0834P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3791
_refine_ls_number_parameters     253
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1822
_refine_ls_R_factor_gt           0.0627
_refine_ls_wR_factor_ref         0.1941
_refine_ls_wR_factor_gt          0.1378
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.970
_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 1.0000 0.5000 0.5000 0.0565(4) Uani 1 2 d S . P . .
Cl1 Cl 0.8005(3) 0.41974(18) 0.42234(13) 0.0742(8) Uani 1 1 d . . . . .
Cl2 Cl 1.1016(3) 0.33933(16) 0.53285(13) 0.0701(7) Uani 1 1 d . . . . .
Cl3 Cl 1.0841(2) 0.50493(16) 0.37541(11) 0.0616(6) Uani 1 1 d . . . . .
N1 N 0.9488(8) 0.2006(5) 0.2684(4) 0.067(2) Uani 1 1 d . . . . .
C1 C 0.9495(9) 0.2901(6) 0.2132(5) 0.061(2) Uani 1 1 d . . . . .
H1A H 0.9842 0.3497 0.2480 0.073 Uiso 1 1 calc R U . . .
H1B H 1.0132 0.2765 0.1775 0.073 Uiso 1 1 calc R U . . .
C2 C 0.8360(11) 0.1675(9) 0.2848(7) 0.105(4) Uani 1 1 d . . . . .
H2 H 0.7535 0.2006 0.2583 0.126 Uiso 1 1 calc R U . . .
C3 C 1.0777(11) 0.1948(9) 0.3361(6) 0.098(4) Uani 1 1 d . . . . .
H3A H 1.0750 0.2490 0.3769 0.118 Uiso 1 1 calc R U . . .
H3B H 1.0788 0.1291 0.3651 0.118 Uiso 1 1 calc R U . . .
C11 C 0.8127(9) 0.3147(6) 0.1597(5) 0.050(2) Uani 1 1 d . . . . .
C12 C 0.7625(10) 0.2642(7) 0.0847(5) 0.064(3) Uani 1 1 d . . . . .
H12 H 0.8150 0.2118 0.0682 0.077 Uiso 1 1 calc R U . . .
C13 C 0.6383(11) 0.2896(8) 0.0347(6) 0.079(3) Uani 1 1 d . . . . .
H13 H 0.6056 0.2549 -0.0163 0.094 Uiso 1 1 calc R U . . .
C14 C 0.5607(11) 0.3647(9) 0.0577(7) 0.086(3) Uani 1 1 d . . . . .
H14 H 0.4745 0.3825 0.0230 0.103 Uiso 1 1 calc R U . . .
C15 C 0.6109(11) 0.4142(7) 0.1326(7) 0.079(3) Uani 1 1 d . . . . .
H15 H 0.5581 0.4662 0.1494 0.095 Uiso 1 1 calc R U . . .
C16 C 0.7350(10) 0.3893(7) 0.1824(5) 0.064(2) Uani 1 1 d . . . . .
H16 H 0.7676 0.4241 0.2334 0.077 Uiso 1 1 calc R U . . .
C21 C 0.8264(9) 0.0830(7) 0.3410(5) 0.065(3) Uani 1 1 d . . . . .
C22 C 0.7847(8) -0.0112(7) 0.3086(5) 0.059(2) Uani 1 1 d . . . . .
H22 H 0.7648 -0.0215 0.2503 0.071 Uiso 1 1 calc R U . . .
C23 C 0.7716(9) -0.0912(6) 0.3608(5) 0.059(2) Uani 1 1 d . . . . .
H23 H 0.7459 -0.1565 0.3384 0.070 Uiso 1 1 calc R U . . .
C24 C 0.7963(9) -0.0751(7) 0.4453(5) 0.060(2) Uani 1 1 d . . . . .
H24 H 0.7890 -0.1294 0.4815 0.073 Uiso 1 1 calc R U . . .
C25 C 0.8315(11) 0.0204(7) 0.4766(5) 0.079(3) Uani 1 1 d . . . . .
H25 H 0.8452 0.0319 0.5345 0.094 Uiso 1 1 calc R U . . .
C26 C 0.8472(11) 0.0995(7) 0.4256(6) 0.082(3) Uani 1 1 d . . . . .
H26 H 0.8721 0.1648 0.4482 0.098 Uiso 1 1 calc R U . . .
C31 C 1.2073(10) 0.2045(8) 0.3090(6) 0.064(3) Uani 1 1 d . . . . .
C32 C 1.3018(13) 0.2767(7) 0.3470(6) 0.081(3) Uani 1 1 d . . . . .
H32 H 1.2827 0.3214 0.3876 0.097 Uiso 1 1 calc R U . . .
C33 C 1.4282(13) 0.2816(9) 0.3232(7) 0.090(3) Uani 1 1 d . . . . .
H33 H 1.4955 0.3300 0.3476 0.108 Uiso 1 1 calc R U . . .
C34 C 1.4515(13) 0.2152(10) 0.2644(8) 0.099(4) Uani 1 1 d . . . . .
H34 H 1.5372 0.2166 0.2501 0.119 Uiso 1 1 calc R U . . .
C35 C 1.3554(17) 0.1475(11) 0.2261(8) 0.116(5) Uani 1 1 d . . . . .
H35 H 1.3717 0.1048 0.1834 0.139 Uiso 1 1 calc R U . . .
C36 C 1.2365(15) 0.1419(8) 0.2496(7) 0.091(4) Uani 1 1 d . . . . .
H36 H 1.1708 0.0929 0.2242 0.109 Uiso 1 1 calc R U . . .
C101 C 0.414(3) 0.036(2) 0.0207(13) 0.150 Uiso 0.5 1 d D U P A -1
H10A H 0.3279 0.0100 0.0310 0.180 Uiso 0.5 1 calc R U P A -1
H10B H 0.3987 0.1049 -0.0041 0.180 Uiso 0.5 1 calc R U P A -1
Cl11 Cl 0.5506(8) 0.0355(6) 0.1134(6) 0.136(3) Uani 0.5 1 d D . P A -1
Cl12 Cl 0.4841(11) -0.0465(9) -0.0410(7) 0.168(4) Uani 0.5 1 d D . P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 Cl2 2.362(2) 3_766 ?
Mo1 Cl2 2.362(2) . ?
Mo1 Cl1 2.365(2) 3_766 ?
Mo1 Cl1 2.365(2) . ?
Mo1 Cl3 2.4169(17) . ?
Mo1 Cl3 2.4169(17) 3_766 ?
N1 C2 1.306(11) . ?
N1 C1 1.496(10) . ?
N1 C3 1.504(11) . ?
C1 C11 1.487(11) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C21 1.473(12) . ?
C2 H2 0.9500 . ?
C3 C31 1.486(13) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C11 C16 1.367(11) . ?
C11 C12 1.396(10) . ?
C12 C13 1.368(11) . ?
C12 H12 0.9500 . ?
C13 C14 1.373(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(13) . ?
C14 H14 0.9500 . ?
C15 C16 1.365(13) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C21 C22 1.380(11) . ?
C21 C26 1.386(11) . ?
C22 C23 1.393(11) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(10) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(12) . ?
C24 H24 0.9500 . ?
C25 C26 1.378(12) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C31 C36 1.372(14) . ?
C31 C32 1.388(12) . ?
C32 C33 1.423(14) . ?
C32 H32 0.9500 . ?
C33 C34 1.373(15) . ?
C33 H33 0.9500 . ?
C34 C35 1.359(16) . ?
C34 H34 0.9500 . ?
C35 C36 1.349(16) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C101 Cl12 1.757(17) . ?
C101 Cl11 1.803(18) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Mo1 Cl2 180.00(12) 3_766 . ?
Cl2 Mo1 Cl1 89.38(9) 3_766 3_766 ?
Cl2 Mo1 Cl1 90.62(9) . 3_766 ?
Cl2 Mo1 Cl1 90.62(9) 3_766 . ?
Cl2 Mo1 Cl1 89.38(9) . . ?
Cl1 Mo1 Cl1 180.0 3_766 . ?
Cl2 Mo1 Cl3 89.99(7) 3_766 . ?
Cl2 Mo1 Cl3 90.01(7) . . ?
Cl1 Mo1 Cl3 91.59(8) 3_766 . ?
Cl1 Mo1 Cl3 88.41(8) . . ?
Cl2 Mo1 Cl3 90.01(7) 3_766 3_766 ?
Cl2 Mo1 Cl3 89.99(7) . 3_766 ?
Cl1 Mo1 Cl3 88.41(8) 3_766 3_766 ?
Cl1 Mo1 Cl3 91.59(8) . 3_766 ?
Cl3 Mo1 Cl3 180.0 . 3_766 ?
C2 N1 C1 121.6(8) . . ?
C2 N1 C3 117.9(7) . . ?
C1 N1 C3 111.6(7) . . ?
C11 C1 N1 113.5(7) . . ?
C11 C1 H1A 108.9 . . ?
N1 C1 H1A 108.9 . . ?
C11 C1 H1B 108.9 . . ?
N1 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
N1 C2 C21 125.3(9) . . ?
N1 C2 H2 117.3 . . ?
C21 C2 H2 117.3 . . ?
C31 C3 N1 115.8(8) . . ?
C31 C3 H3A 108.3 . . ?
N1 C3 H3A 108.3 . . ?
C31 C3 H3B 108.3 . . ?
N1 C3 H3B 108.3 . . ?
H3A C3 H3B 107.4 . . ?
C16 C11 C12 118.7(8) . . ?
C16 C11 C1 120.2(8) . . ?
C12 C11 C1 121.1(8) . . ?
C13 C12 C11 120.6(9) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 120.5(9) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C13 C14 C15 118.6(9) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
C16 C15 C14 121.0(9) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C11 120.6(9) . . ?
C15 C16 H16 119.7 . . ?
C11 C16 H16 119.7 . . ?
C22 C21 C26 119.6(8) . . ?
C22 C21 C2 119.7(9) . . ?
C26 C21 C2 120.4(9) . . ?
C21 C22 C23 120.4(7) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C24 C23 C22 119.6(8) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C25 C24 C23 119.5(8) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 121.3(8) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C25 C26 C21 119.5(9) . . ?
C25 C26 H26 120.3 . . ?
C21 C26 H26 120.3 . . ?
C36 C31 C32 119.9(11) . . ?
C36 C31 C3 121.4(11) . . ?
C32 C31 C3 118.7(11) . . ?
C31 C32 C33 117.9(11) . . ?
C31 C32 H32 121.0 . . ?
C33 C32 H32 121.0 . . ?
C34 C33 C32 119.0(11) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C35 C34 C33 121.9(13) . . ?
C35 C34 H34 119.0 . . ?
C33 C34 H34 119.0 . . ?
C36 C35 C34 118.9(13) . . ?
C36 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
C35 C36 C31 122.3(12) . . ?
C35 C36 H36 118.9 . . ?
C31 C36 H36 118.9 . . ?
Cl12 C101 Cl11 99.4(12) . . ?
Cl12 C101 H10A 111.9 . . ?
Cl11 C101 H10A 111.9 . . ?
Cl12 C101 H10B 111.9 . . ?
Cl11 C101 H10B 111.9 . . ?
H10A C101 H10B 109.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 C1 C11 -18.6(13) . . . . ?
C3 N1 C1 C11 -165.1(8) . . . . ?
C1 N1 C2 C21 -177.3(9) . . . . ?
C3 N1 C2 C21 -32.8(17) . . . . ?
C2 N1 C3 C31 163.0(10) . . . . ?
C1 N1 C3 C31 -49.2(12) . . . . ?
N1 C1 C11 C16 98.1(9) . . . . ?
N1 C1 C11 C12 -83.4(10) . . . . ?
C16 C11 C12 C13 0.5(13) . . . . ?
C1 C11 C12 C13 -178.0(8) . . . . ?
C11 C12 C13 C14 -0.3(15) . . . . ?
C12 C13 C14 C15 -0.1(16) . . . . ?
C13 C14 C15 C16 0.3(16) . . . . ?
C14 C15 C16 C11 -0.1(15) . . . . ?
C12 C11 C16 C15 -0.3(13) . . . . ?
C1 C11 C16 C15 178.2(8) . . . . ?
N1 C2 C21 C22 -100.8(13) . . . . ?
N1 C2 C21 C26 84.9(16) . . . . ?
C26 C21 C22 C23 -3.9(14) . . . . ?
C2 C21 C22 C23 -178.3(9) . . . . ?
C21 C22 C23 C24 2.1(13) . . . . ?
C22 C23 C24 C25 1.0(14) . . . . ?
C23 C24 C25 C26 -2.3(15) . . . . ?
C24 C25 C26 C21 0.4(17) . . . . ?
C22 C21 C26 C25 2.7(15) . . . . ?
C2 C21 C26 C25 177.0(10) . . . . ?
N1 C3 C31 C36 -55.3(13) . . . . ?
N1 C3 C31 C32 126.8(9) . . . . ?
C36 C31 C32 C33 -1.0(13) . . . . ?
C3 C31 C32 C33 176.9(8) . . . . ?
C31 C32 C33 C34 -0.2(14) . . . . ?
C32 C33 C34 C35 2.5(18) . . . . ?
C33 C34 C35 C36 -3.5(19) . . . . ?
C34 C35 C36 C31 2.3(18) . . . . ?
C32 C31 C36 C35 0.0(16) . . . . ?
C3 C31 C36 C35 -177.9(10) . . . . ?

_refine_diff_density_max         0.530
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.098

####################################################################### 
# 
# 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_5a
_database_code_depnum_ccdc_archive 'CCDC 1491994'
_audit_update_record             
;
2017-04-30 deposited with the CCDC.
2017-05-03 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         ?
_chemical_formula_sum            'C12 H22 Cl8 Mo2 N2'
_chemical_formula_weight         669.79

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'
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'

_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                   6.6315(17)
_cell_length_b                   7.648(2)
_cell_length_c                   11.839(3)
_cell_angle_alpha                106.915(2)
_cell_angle_beta                 96.903(3)
_cell_angle_gamma                102.798(3)
_cell_volume                     549.1(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3678
_cell_measurement_theta_min      2.8715
_cell_measurement_theta_max      27.950

_exptl_crystal_description       prism
_exptl_crystal_colour            red-brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_F_000             328
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    2.115
_shelx_estimated_absorpt_T_min   0.689
_shelx_estimated_absorpt_T_max   0.785
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6894
_exptl_absorpt_correction_T_max  0.7854
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1381 (selected reflections only, before parameter refinement)
 R(int) =  0.0527 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6004
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.834
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2382
_reflns_number_gt                2142
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_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)+(0.0287P)²+0.4297P] 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         2382
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0760
_refine_ls_wR_factor_gt          0.0728
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_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
C1 C 0.2404(5) 0.3514(5) 0.7678(3) 0.0171(7) Uani 1 1 d . . . . .
H1 H 0.3258 0.2948 0.8154 0.021 Uiso 1 1 calc R U . . .
C2 C 0.2312(6) 0.2539(5) 0.6327(3) 0.0213(8) Uani 1 1 d . . . . .
H2A H 0.3726 0.2921 0.6140 0.026 Uiso 1 1 calc R U . . .
H2B H 0.1921 0.1145 0.6145 0.026 Uiso 1 1 calc R U . . .
C3 C 0.0727(6) 0.3055(5) 0.5536(3) 0.0231(8) Uani 1 1 d . . . . .
H3A H 0.0644 0.2333 0.4681 0.028 Uiso 1 1 calc R U . . .
H3B H 0.1214 0.4424 0.5641 0.028 Uiso 1 1 calc R U . . .
C4 C -0.1481(6) 0.2621(6) 0.5844(3) 0.0236(8) Uani 1 1 d . . . . .
H4A H -0.2472 0.2985 0.5318 0.028 Uiso 1 1 calc R U . . .
H4B H -0.2009 0.1242 0.5699 0.028 Uiso 1 1 calc R U . . .
C5 C -0.1377(6) 0.3719(5) 0.7159(3) 0.0211(8) Uani 1 1 d . . . . .
H5A H -0.0959 0.5098 0.7283 0.025 Uiso 1 1 calc R U . . .
H5B H -0.2793 0.3399 0.7356 0.025 Uiso 1 1 calc R U . . .
C6 C 0.0193(5) 0.3263(5) 0.8003(3) 0.0192(7) Uani 1 1 d . . . . .
H6A H -0.0358 0.1936 0.7978 0.023 Uiso 1 1 calc R U . . .
H6B H 0.0321 0.4101 0.8837 0.023 Uiso 1 1 calc R U . . .
Cl1 Cl 0.61047(14) 0.81103(13) 0.68573(8) 0.0231(2) Uani 1 1 d . . . . .
Cl2 Cl 0.77604(13) 0.76061(12) 0.94725(7) 0.01944(19) Uani 1 1 d . . . . .
Cl3 Cl 0.35257(12) 0.83857(11) 1.04342(7) 0.01587(18) Uani 1 1 d . . . . .
Cl4 Cl 0.18194(13) 0.88618(12) 0.78654(7) 0.01818(18) Uani 1 1 d . . . . .
Mo1 Mo 0.46771(4) 0.78558(4) 0.84954(2) 0.01395(10) Uani 1 1 d . . . . .
N1 N 0.3435(4) 0.5513(4) 0.8000(2) 0.0149(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.444(4) . ?
C1 C2 1.543(5) . ?
C1 C6 1.546(5) . ?
C1 H1 1.0000 . ?
C2 C3 1.517(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.540(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.524(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.522(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
Cl1 Mo1 2.2966(10) . ?
Cl2 Mo1 2.2996(10) . ?
Cl3 Mo1 2.4562(10) . ?
Cl3 Mo1 2.6996(10) 2_677 ?
Cl4 Mo1 2.3194(9) . ?
Mo1 N1 1.689(3) . ?
Mo1 Cl3 2.6996(11) 2_677 ?

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 C1 C2 109.2(3) . . ?
N1 C1 C6 109.3(3) . . ?
C2 C1 C6 112.5(3) . . ?
N1 C1 H1 108.6 . . ?
C2 C1 H1 108.6 . . ?
C6 C1 H1 108.6 . . ?
C3 C2 C1 111.9(3) . . ?
C3 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C2 C3 C4 111.7(3) . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C5 C4 C3 109.9(3) . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C6 C5 C4 111.7(3) . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 107.9 . . ?
C5 C6 C1 113.1(3) . . ?
C5 C6 H6A 109.0 . . ?
C1 C6 H6A 109.0 . . ?
C5 C6 H6B 109.0 . . ?
C1 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
Mo1 Cl3 Mo1 100.97(3) . 2_677 ?
N1 Mo1 Cl1 100.17(9) . . ?
N1 Mo1 Cl2 96.13(9) . . ?
Cl1 Mo1 Cl2 92.40(4) . . ?
N1 Mo1 Cl4 96.69(9) . . ?
Cl1 Mo1 Cl4 91.70(3) . . ?
Cl2 Mo1 Cl4 165.62(3) . . ?
N1 Mo1 Cl3 93.20(9) . . ?
Cl1 Mo1 Cl3 166.62(3) . . ?
Cl2 Mo1 Cl3 86.61(3) . . ?
Cl4 Mo1 Cl3 86.22(3) . . ?
N1 Mo1 Cl3 172.23(9) . 2_677 ?
Cl1 Mo1 Cl3 87.60(3) . 2_677 ?
Cl2 Mo1 Cl3 83.26(3) . 2_677 ?
Cl4 Mo1 Cl3 83.15(3) . 2_677 ?
Cl3 Mo1 Cl3 79.03(3) . 2_677 ?
C1 N1 Mo1 175.3(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -72.1(4) . . . . ?
C6 C1 C2 C3 49.4(4) . . . . ?
C1 C2 C3 C4 -55.0(4) . . . . ?
C2 C3 C4 C5 58.8(4) . . . . ?
C3 C4 C5 C6 -57.2(4) . . . . ?
C4 C5 C6 C1 52.8(4) . . . . ?
N1 C1 C6 C5 72.9(4) . . . . ?
C2 C1 C6 C5 -48.5(4) . . . . ?

_refine_diff_density_max         0.882
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.131

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1491991'
_audit_update_record             
;
2017-04-30 deposited with the CCDC.
2017-05-03 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         ?
_chemical_formula_sum            'C14 H39 Cl8 Mo2 N6'
_chemical_formula_weight         766.99

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'
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'

_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                   7.9913(5)
_cell_length_b                   27.2271(15)
_cell_length_c                   13.7004(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.321(4)
_cell_angle_gamma                90
_cell_volume                     2980.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8143
_cell_measurement_theta_min      2.549
_cell_measurement_theta_max      28.010

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_F_000             1540
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.574
_shelx_estimated_absorpt_T_min   0.754
_shelx_estimated_absorpt_T_max   0.859
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7542
_exptl_absorpt_correction_T_max  0.8585
_exptl_absorpt_process_details   
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.1300 (selected reflections only, before parameter refinement)
 R(int) =  0.0665 (selected reflections only, after parameter refinement)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34636
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         0.748
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5833
_reflns_number_gt                5255
_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       'APEX3 (Bruker AXS, 2015)'
_computing_cell_refinement       'APEX3 (Bruker AXS, 2015)'
_computing_data_reduction        'SAINT (Bruker AXS, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1996)'
_computing_publication_material  'XCIF 2014/2 (Bruker AXS, 2014)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²+18.0525P] 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         5833
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1092
_refine_ls_wR_factor_gt          0.1042
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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 0.22919(6) 0.60370(2) 0.75604(4) 0.01711(12) Uani 1 1 d . . . . .
Cl1 Cl 0.49164(18) 0.62304(5) 0.68169(11) 0.0245(3) Uani 1 1 d . . . . .
Cl2 Cl -0.02567(18) 0.57822(5) 0.83748(11) 0.0265(3) Uani 1 1 d . . . . .
Cl3 Cl 0.23888(19) 0.52641(5) 0.67487(10) 0.0243(3) Uani 1 1 d . . . . .
C1 C 0.5511(7) 0.5736(2) 0.8925(5) 0.0265(13) Uani 1 1 d . . . . .
H1A H 0.5959 0.6033 0.8618 0.040 Uiso 1 1 calc R U . . .
H1B H 0.5968 0.5705 0.9588 0.040 Uiso 1 1 calc R U . . .
H1C H 0.5831 0.5447 0.8541 0.040 Uiso 1 1 calc R U . . .
C2 C 0.3054(8) 0.5311(2) 0.9440(4) 0.0237(13) Uani 1 1 d . . . . .
H2A H 0.1831 0.5320 0.9482 0.036 Uiso 1 1 calc R U . . .
H2B H 0.3397 0.5027 0.9050 0.036 Uiso 1 1 calc R U . . .
H2C H 0.3535 0.5284 1.0098 0.036 Uiso 1 1 calc R U . . .
N1 N 0.3662(6) 0.57688(17) 0.8970(4) 0.0196(10) Uani 1 1 d . . . . .
C3 C 0.3094(8) 0.6210(2) 0.9515(4) 0.0210(12) Uani 1 1 d . . . . .
H3A H 0.3992 0.6330 0.9955 0.025 Uiso 1 1 calc R U . . .
H3B H 0.2098 0.6131 0.9911 0.025 Uiso 1 1 calc R U . . .
N2 N 0.2674(6) 0.65917(16) 0.8763(4) 0.0224(10) Uani 1 1 d . . . . .
C4 C 0.4068(8) 0.6951(2) 0.8654(5) 0.0284(14) Uani 1 1 d . . . . .
H4A H 0.5082 0.6778 0.8449 0.043 Uiso 1 1 calc R U . . .
H4B H 0.3763 0.7196 0.8161 0.043 Uiso 1 1 calc R U . . .
H4C H 0.4276 0.7114 0.9280 0.043 Uiso 1 1 calc R U . . .
C5 C 0.1170(8) 0.6879(2) 0.9076(5) 0.0304(15) Uani 1 1 d . . . . .
H5A H 0.0218 0.6656 0.9157 0.046 Uiso 1 1 calc R U . . .
H5B H 0.1411 0.7044 0.9698 0.046 Uiso 1 1 calc R U . . .
H5C H 0.0898 0.7126 0.8579 0.046 Uiso 1 1 calc R U . . .
N3 N 0.1020(6) 0.64401(17) 0.6688(4) 0.0222(10) Uani 1 1 d . . . . .
C6 C -0.0698(8) 0.6328(2) 0.6337(5) 0.0332(15) Uani 1 1 d . . . . .
H6A H -0.1002 0.5993 0.6531 0.050 Uiso 1 1 calc R U . . .
H6B H -0.1488 0.6562 0.6623 0.050 Uiso 1 1 calc R U . . .
H6C H -0.0738 0.6355 0.5624 0.050 Uiso 1 1 calc R U . . .
C7 C 0.1486(8) 0.6940(2) 0.6401(5) 0.0301(14) Uani 1 1 d . . . . .
H7A H 0.2621 0.7011 0.6635 0.045 Uiso 1 1 calc R U . . .
H7B H 0.1449 0.6967 0.5688 0.045 Uiso 1 1 calc R U . . .
H7C H 0.0699 0.7174 0.6687 0.045 Uiso 1 1 calc R U . . .
Mo2 Mo 0.25892(6) 0.61909(2) 0.25886(4) 0.02010(12) Uani 1 1 d . . . . .
Cl4 Cl 0.4820(2) 0.57803(6) 0.17629(11) 0.0292(3) Uani 1 1 d . . . . .
Cl5 Cl 0.0757(2) 0.67025(6) 0.35418(12) 0.0308(3) Uani 1 1 d . . . . .
Cl6 Cl 0.3337(2) 0.69137(5) 0.17181(12) 0.0336(4) Uani 1 1 d . . . . .
C8 C 0.3253(9) 0.5151(2) 0.3603(5) 0.0318(15) Uani 1 1 d . . . . .
H8A H 0.4374 0.5197 0.3331 0.048 Uiso 1 1 calc R U . . .
H8B H 0.3337 0.4966 0.4215 0.048 Uiso 1 1 calc R U . . .
H8C H 0.2556 0.4969 0.3137 0.048 Uiso 1 1 calc R U . . .
C9 C 0.0786(8) 0.5541(3) 0.4209(5) 0.0336(15) Uani 1 1 d . . . . .
H9A H 0.0225 0.5853 0.4349 0.050 Uiso 1 1 calc R U . . .
H9B H 0.0121 0.5354 0.3735 0.050 Uiso 1 1 calc R U . . .
H9C H 0.0902 0.5351 0.4813 0.050 Uiso 1 1 calc R U . . .
N4 N 0.2480(7) 0.56411(17) 0.3797(3) 0.0228(10) Uani 1 1 d . . . . .
C10 C 0.3485(7) 0.5936(2) 0.4512(4) 0.0216(12) Uani 1 1 d . . . . .
H10A H 0.2740 0.6125 0.4947 0.026 Uiso 1 1 calc R U . . .
H10B H 0.4197 0.5718 0.4917 0.026 Uiso 1 1 calc R U . . .
N5 N 0.4532(6) 0.62712(17) 0.3923(4) 0.0221(11) Uani 1 1 d . . . . .
C11 C 0.6259(8) 0.6084(2) 0.3837(5) 0.0283(14) Uani 1 1 d . . . . .
H11A H 0.6923 0.6312 0.3445 0.042 Uiso 1 1 calc R U . . .
H11B H 0.6760 0.6054 0.4489 0.042 Uiso 1 1 calc R U . . .
H11C H 0.6240 0.5761 0.3520 0.042 Uiso 1 1 calc R U . . .
C12 C 0.4666(9) 0.6768(2) 0.4365(5) 0.0282(14) Uani 1 1 d . . . . .
H12A H 0.3544 0.6908 0.4437 0.042 Uiso 1 1 calc R U . . .
H12B H 0.5204 0.6743 0.5007 0.042 Uiso 1 1 calc R U . . .
H12C H 0.5337 0.6980 0.3941 0.042 Uiso 1 1 calc R U . . .
N6 N 0.0974(6) 0.59275(18) 0.1903(3) 0.0245(11) Uani 1 1 d . . . . .
C13 C -0.0279(11) 0.5621(3) 0.1507(6) 0.050(2) Uani 1 1 d . . . . .
H13A H -0.0807 0.5785 0.0948 0.075 Uiso 1 1 calc R U . . .
H13B H 0.0223 0.5311 0.1293 0.075 Uiso 1 1 calc R U . . .
H13C H -0.1125 0.5555 0.2005 0.075 Uiso 1 1 calc R U . . .
C21 C 0.7808(11) 0.7031(3) 0.1609(6) 0.058(2) Uani 1 1 d . . . . .
H21A H 0.6937 0.6775 0.1670 0.069 Uiso 1 1 calc R U . . .
H21B H 0.8914 0.6876 0.1715 0.069 Uiso 1 1 calc R U . . .
Cl7 Cl 0.7488(2) 0.74864(6) 0.24774(14) 0.0456(4) Uani 1 1 d . . . . .
Cl8 Cl 0.7717(3) 0.73026(10) 0.03935(16) 0.0650(6) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 N3 1.911(5) . ?
Mo1 N2 2.255(5) . ?
Mo1 N1 2.332(5) . ?
Mo1 Cl3 2.3817(14) . ?
Mo1 Cl1 2.3953(15) . ?
Mo1 Cl2 2.4289(15) . ?
C1 N1 1.482(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.486(7) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N1 C3 1.487(7) . ?
C3 N2 1.500(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N2 C4 1.490(8) . ?
N2 C5 1.499(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
N3 C7 1.465(8) . ?
N3 C6 1.484(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
Mo2 N6 1.746(5) . ?
Mo2 N4 2.235(5) . ?
Mo2 Cl6 2.3790(16) . ?
Mo2 Cl4 2.3941(16) . ?
Mo2 N5 2.402(5) . ?
Mo2 Cl5 2.4103(16) . ?
C8 N4 1.495(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.494(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
N4 C10 1.496(7) . ?
C10 N5 1.481(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
N5 C11 1.477(8) . ?
N5 C12 1.485(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N6 C13 1.409(9) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C21 Cl7 1.738(9) . ?
C21 Cl8 1.822(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Mo1 N2 98.13(19) . . ?
N3 Mo1 N1 160.61(18) . . ?
N2 Mo1 N1 62.85(16) . . ?
N3 Mo1 Cl3 103.54(15) . . ?
N2 Mo1 Cl3 158.21(13) . . ?
N1 Mo1 Cl3 95.37(12) . . ?
N3 Mo1 Cl1 94.12(15) . . ?
N2 Mo1 Cl1 92.76(13) . . ?
N1 Mo1 Cl1 90.73(13) . . ?
Cl3 Mo1 Cl1 87.98(5) . . ?
N3 Mo1 Cl2 90.39(15) . . ?
N2 Mo1 Cl2 88.06(13) . . ?
N1 Mo1 Cl2 85.48(13) . . ?
Cl3 Mo1 Cl2 89.52(5) . . ?
Cl1 Mo1 Cl2 175.26(5) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 N1 C2 107.2(5) . . ?
C1 N1 C3 112.1(5) . . ?
C2 N1 C3 111.0(4) . . ?
C1 N1 Mo1 116.7(4) . . ?
C2 N1 Mo1 117.9(4) . . ?
C3 N1 Mo1 91.1(3) . . ?
N1 C3 N2 106.4(4) . . ?
N1 C3 H3A 110.4 . . ?
N2 C3 H3A 110.4 . . ?
N1 C3 H3B 110.4 . . ?
N2 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
C4 N2 C5 106.7(5) . . ?
C4 N2 C3 111.0(5) . . ?
C5 N2 C3 110.0(5) . . ?
C4 N2 Mo1 117.7(4) . . ?
C5 N2 Mo1 117.0(4) . . ?
C3 N2 Mo1 93.8(3) . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 N3 C6 109.9(5) . . ?
C7 N3 Mo1 124.5(4) . . ?
C6 N3 Mo1 124.9(4) . . ?
N3 C6 H6A 109.5 . . ?
N3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N6 Mo2 N4 95.3(2) . . ?
N6 Mo2 Cl6 104.89(17) . . ?
N4 Mo2 Cl6 159.50(13) . . ?
N6 Mo2 Cl4 95.98(17) . . ?
N4 Mo2 Cl4 93.99(14) . . ?
Cl6 Mo2 Cl4 87.68(6) . . ?
N6 Mo2 N5 156.9(2) . . ?
N4 Mo2 N5 61.62(17) . . ?
Cl6 Mo2 N5 98.23(12) . . ?
Cl4 Mo2 N5 85.54(13) . . ?
N6 Mo2 Cl5 94.56(17) . . ?
N4 Mo2 Cl5 87.66(14) . . ?
Cl6 Mo2 Cl5 87.06(6) . . ?
Cl4 Mo2 Cl5 169.13(6) . . ?
N5 Mo2 Cl5 85.81(13) . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 H9A 109.5 . . ?
N4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C9 N4 C8 106.3(5) . . ?
C9 N4 C10 109.6(5) . . ?
C8 N4 C10 111.9(5) . . ?
C9 N4 Mo2 116.1(4) . . ?
C8 N4 Mo2 116.6(4) . . ?
C10 N4 Mo2 95.9(3) . . ?
N5 C10 N4 106.1(4) . . ?
N5 C10 H10A 110.5 . . ?
N4 C10 H10A 110.5 . . ?
N5 C10 H10B 110.5 . . ?
N4 C10 H10B 110.5 . . ?
H10A C10 H10B 108.7 . . ?
C11 N5 C10 111.2(5) . . ?
C11 N5 C12 106.4(5) . . ?
C10 N5 C12 112.3(5) . . ?
C11 N5 Mo2 120.6(4) . . ?
C10 N5 Mo2 89.6(3) . . ?
C12 N5 Mo2 116.0(4) . . ?
N5 C11 H11A 109.5 . . ?
N5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 H12A 109.5 . . ?
N5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C13 N6 Mo2 166.3(5) . . ?
N6 C13 H13A 109.5 . . ?
N6 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N6 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Cl7 C21 Cl8 109.4(5) . . ?
Cl7 C21 H21A 109.8 . . ?
Cl8 C21 H21A 109.8 . . ?
Cl7 C21 H21B 109.8 . . ?
Cl8 C21 H21B 109.8 . . ?
H21A C21 H21B 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C3 N2 98.2(5) . . . . ?
C2 N1 C3 N2 -141.9(5) . . . . ?
Mo1 N1 C3 N2 -21.3(4) . . . . ?
N1 C3 N2 C4 -99.5(5) . . . . ?
N1 C3 N2 C5 142.7(5) . . . . ?
N1 C3 N2 Mo1 22.1(4) . . . . ?
C9 N4 C10 N5 -144.9(5) . . . . ?
C8 N4 C10 N5 97.4(5) . . . . ?
Mo2 N4 C10 N5 -24.4(5) . . . . ?
N4 C10 N5 C11 -100.4(5) . . . . ?
N4 C10 N5 C12 140.6(5) . . . . ?
N4 C10 N5 Mo2 22.5(4) . . . . ?
N4 Mo2 N6 C13 -12(2) . . . . ?
Cl6 Mo2 N6 C13 172(2) . . . . ?
Cl4 Mo2 N6 C13 83(2) . . . . ?
N5 Mo2 N6 C13 -10(2) . . . . ?
Cl5 Mo2 N6 C13 -100(2) . . . . ?

_refine_diff_density_max         1.293
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.118

