# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1873381'
_audit_update_record             
;
2018-10-15 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H10 K N6 O Re S4'
_chemical_formula_weight         607.80

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'
K K 0.2009 0.2494 '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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

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

_cell_length_a                   26.040(5)
_cell_length_b                   7.5510(15)
_cell_length_c                   9.5600(19)
_cell_angle_alpha                90
_cell_angle_beta                 92.54(3)
_cell_angle_gamma                90
_cell_volume                     1877.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    10423
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      58.5

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.150
_exptl_crystal_F_000             1160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.106
_exptl_absorpt_coefficient_mu    7.151
_shelx_estimated_absorpt_T_min   0.381
_shelx_estimated_absorpt_T_max   0.518
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6333
_exptl_absorpt_correction_T_max  0.9253
_exptl_absorpt_process_details   'face indexed'

_exptl_special_details           
;
programs X-Red32 and X-Shape by STOE & Cie GmbH 2010
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            10423
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.566
_diffrn_reflns_theta_max         29.235
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2731
_reflns_number_gt                2352
_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       'X-Area by STOE & Cie GmbH 2010'
_computing_cell_refinement       'X-Area by STOE & Cie GmbH 2010'
_computing_data_reduction        'X-Area by STOE & Cie GmbH 2010'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XP Version 5.1 by Bruker AXS 1998'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'

_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)+(0.0562P)²+13.9820P] 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         2731
_refine_ls_number_parameters     129
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.1093
_refine_ls_wR_factor_gt          0.1018
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.09869(2) 0.5000 0.37216(4) 0.03352(12) Uani 1 2 d S T P . .
K1 K 0.13517(8) 0.0000 0.9113(2) 0.0392(4) Uani 1 2 d S T P . .
S1 S 0.14688(6) 0.70906(19) 0.25721(17) 0.0380(3) Uani 1 1 d . . . . .
S2 S 0.10399(6) 0.29109(19) 0.55053(17) 0.0390(3) Uani 1 1 d . . . . .
O1 O 0.0388(3) 0.5000 0.3005(8) 0.0546(18) Uani 1 2 d S T P . .
N1 N 0.1892(2) 0.6862(7) 0.0110(6) 0.0404(11) Uani 1 1 d . . . . .
N2 N 0.0764(2) 0.3139(7) 0.8140(5) 0.0379(11) Uani 1 1 d . . . . .
N3 N 0.0542(4) 0.0000 1.0855(10) 0.058(2) Uani 1 2 d S T P . .
N4 N 0.2140(4) 0.0000 0.7132(10) 0.054(2) Uani 1 2 d S T P . .
C1 C 0.1717(2) 0.5937(7) 0.1168(6) 0.0336(11) Uani 1 1 d . . . . .
C2 C 0.2085(3) 0.5912(9) -0.0927(7) 0.0426(14) Uani 1 1 d . . . . .
H2 H 0.2226 0.6519 -0.1691 0.051 Uiso 1 1 calc R U . . .
C3 C 0.0869(2) 0.4069(8) 0.7009(7) 0.0373(12) Uani 1 1 d . . . . .
C4 C 0.0626(2) 0.4088(9) 0.9257(6) 0.0404(13) Uani 1 1 d . . . . .
H4 H 0.0526 0.3479 1.0071 0.048 Uiso 1 1 calc R U . . .
C5 C 0.0341(4) 0.0000 1.1895(10) 0.0410(19) Uani 1 2 d S T P . .
C6 C 0.0103(4) 0.0000 1.3221(10) 0.046(2) Uani 1 2 d S T P . .
H6A H 0.0312 -0.0700 1.3897 0.068 Uiso 0.5 1 calc R U P . .
H6B H -0.0241 -0.0519 1.3111 0.068 Uiso 0.5 1 calc R U P . .
H6C H 0.0076 0.1219 1.3562 0.068 Uiso 0.5 1 calc R U P . .
C7 C 0.2288(4) 0.0000 0.6045(10) 0.0409(19) Uani 1 2 d S T P . .
C8 C 0.2462(5) 0.0000 0.4606(11) 0.058(3) Uani 1 2 d S T P . .
H8A H 0.2220 0.0678 0.4004 0.088 Uiso 0.5 1 calc R U P . .
H8B H 0.2479 -0.1221 0.4264 0.088 Uiso 0.5 1 calc R U P . .
H8C H 0.2804 0.0543 0.4589 0.088 Uiso 0.5 1 calc R U P . .


_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
Re1 O1 1.676(8) . ?
Re1 S2 2.3226(16) . ?
Re1 S2 2.3226(16) 6_565 ?
Re1 S1 2.3230(16) 6_565 ?
Re1 S1 2.3231(16) . ?
K1 N3 2.743(10) . ?
K1 N4 2.853(9) . ?
K1 N1 2.896(6) 6_566 ?
K1 N1 2.896(6) 1_546 ?
K1 N2 2.950(5) 6 ?
K1 N2 2.950(5) . ?
S1 C1 1.748(6) . ?
S1 K1 3.971(2) 1_564 ?
S2 C3 1.757(7) . ?
N1 C1 1.326(8) . ?
N1 C2 1.339(9) . ?
N1 K1 2.896(6) 1_564 ?
N2 C3 1.328(8) . ?
N2 C4 1.348(8) . ?
N3 C5 1.144(13) . ?
N4 C7 1.124(13) . ?
C1 C1 1.416(11) 6_565 ?
C1 K1 3.743(6) 1_564 ?
C2 C2 1.378(13) 6_565 ?
C2 K1 3.630(7) 1_564 ?
C2 H2 0.9500 . ?
C3 C3 1.406(12) 6_565 ?
C4 C4 1.377(14) 6_565 ?
C4 H4 0.9500 . ?
C5 C6 1.436(13) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.467(15) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 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
O1 Re1 S2 108.90(19) . . ?
O1 Re1 S2 108.90(19) . 6_565 ?
S2 Re1 S2 85.56(8) . 6_565 ?
O1 Re1 S1 108.63(19) . 6_565 ?
S2 Re1 S1 82.53(6) . 6_565 ?
S2 Re1 S1 142.48(6) 6_565 6_565 ?
O1 Re1 S1 108.63(19) . . ?
S2 Re1 S1 142.48(6) . . ?
S2 Re1 S1 82.53(6) 6_565 . ?
S1 Re1 S1 85.62(8) 6_565 . ?
N3 K1 N4 175.8(3) . . ?
N3 K1 N1 100.09(17) . 6_566 ?
N4 K1 N1 82.25(16) . 6_566 ?
N3 K1 N1 100.09(17) . 1_546 ?
N4 K1 N1 82.25(16) . 1_546 ?
N1 K1 N1 109.8(2) 6_566 1_546 ?
N3 K1 N2 77.85(17) . 6 ?
N4 K1 N2 99.75(16) . 6 ?
N1 K1 N2 177.75(16) 6_566 6 ?
N1 K1 N2 71.61(15) 1_546 6 ?
N3 K1 N2 77.84(17) . . ?
N4 K1 N2 99.75(16) . . ?
N1 K1 N2 71.61(15) 6_566 . ?
N1 K1 N2 177.75(16) 1_546 . ?
N2 K1 N2 106.9(2) 6 . ?
C1 S1 Re1 104.5(2) . . ?
C1 S1 K1 69.72(19) . 1_564 ?
Re1 S1 K1 138.31(7) . 1_564 ?
C3 S2 Re1 104.7(2) . . ?
C3 S2 K1 68.3(2) . . ?
Re1 S2 K1 167.26(6) . . ?
C1 N1 C2 115.8(5) . . ?
C1 N1 K1 120.2(4) . 1_564 ?
C2 N1 K1 112.7(4) . 1_564 ?
C3 N2 C4 115.8(6) . . ?
C3 N2 K1 124.0(4) . . ?
C4 N2 K1 109.3(4) . . ?
C5 N3 K1 157.2(9) . . ?
C7 N4 K1 154.2(9) . . ?
N1 C1 C1 121.8(3) . 6_565 ?
N1 C1 S1 118.3(4) . . ?
C1 C1 S1 119.88(19) 6_565 . ?
N1 C1 K1 41.9(3) . 1_564 ?
C1 C1 K1 145.04(9) 6_565 1_564 ?
S1 C1 K1 84.3(2) . 1_564 ?
N1 C2 C2 122.4(4) . 6_565 ?
N1 C2 K1 47.4(3) . 1_564 ?
C2 C2 K1 148.24(11) 6_565 1_564 ?
N1 C2 H2 118.8 . . ?
C2 C2 H2 118.8 6_565 . ?
K1 C2 H2 79.7 1_564 . ?
N2 C3 C3 121.9(4) . 6_565 ?
N2 C3 S2 118.2(5) . . ?
C3 C3 S2 119.8(2) 6_565 . ?
N2 C3 K1 39.4(3) . . ?
C3 C3 K1 142.89(9) 6_565 . ?
S2 C3 K1 86.6(2) . . ?
N2 C4 C4 122.1(4) . 6_565 ?
N2 C4 K1 50.2(3) . . ?
C4 C4 K1 148.38(11) 6_565 . ?
N2 C4 H4 118.9 . . ?
C4 C4 H4 118.9 6_565 . ?
K1 C4 H4 77.4 . . ?
N3 C5 C6 178.2(11) . . ?
N3 C5 K1 16.2(6) . . ?
C6 C5 K1 162.1(7) . . ?
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 . . ?
N4 C7 C8 177.9(11) . . ?
N4 C7 K1 18.6(6) . . ?
C8 C7 K1 159.2(7) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

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 C1 -2.3(7) . . . 6_565 ?
K1 N1 C1 C1 138.8(2) 1_564 . . 6_565 ?
C2 N1 C1 S1 179.1(5) . . . . ?
K1 N1 C1 S1 -39.7(6) 1_564 . . . ?
C2 N1 C1 K1 -141.1(7) . . . 1_564 ?
Re1 S1 C1 N1 162.0(4) . . . . ?
K1 S1 C1 N1 25.4(4) 1_564 . . . ?
Re1 S1 C1 C1 -16.57(17) . . . 6_565 ?
K1 S1 C1 C1 -153.18(17) 1_564 . . 6_565 ?
Re1 S1 C1 K1 136.61(8) . . . 1_564 ?
C1 N1 C2 C2 2.3(7) . . . 6_565 ?
K1 N1 C2 C2 -141.69(18) 1_564 . . 6_565 ?
C1 N1 C2 K1 144.0(7) . . . 1_564 ?
C4 N2 C3 C3 4.0(6) . . . 6_565 ?
K1 N2 C3 C3 -136.2(2) . . . 6_565 ?
C4 N2 C3 S2 -178.9(4) . . . . ?
K1 N2 C3 S2 40.9(6) . . . . ?
C4 N2 C3 K1 140.2(7) . . . . ?
Re1 S2 C3 N2 166.6(4) . . . . ?
K1 S2 C3 N2 -24.6(4) . . . . ?
Re1 S2 C3 C3 -16.26(18) . . . 6_565 ?
K1 S2 C3 C3 152.53(19) . . . 6_565 ?
Re1 S2 C3 K1 -168.79(7) . . . . ?
C3 N2 C4 C4 -4.0(6) . . . 6_565 ?
K1 N2 C4 C4 141.78(16) . . . 6_565 ?
C3 N2 C4 K1 -145.8(6) . . . . ?

_refine_diff_density_max         4.233
_refine_diff_density_min         -2.423
_refine_diff_density_rms         0.192

_shelxl_version_number           2013-3

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

data_NCS200C
_database_code_depnum_ccdc_archive 'CCDC 1873382'
_audit_update_record             
;
2018-10-15 deposited with the CCDC.
2019-01-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H46 Mo N6 O2 S4'
_chemical_formula_weight         674.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   9.5168(19)
_cell_length_b                   13.590(3)
_cell_length_c                   12.011(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.25(3)
_cell_angle_gamma                90
_cell_volume                     1549.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    17863
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      58.9

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             708
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.448
_exptl_crystal_size_mid          0.432
_exptl_crystal_size_min          0.337
_exptl_absorpt_coefficient_mu    0.725
_shelx_estimated_absorpt_T_min   0.737
_shelx_estimated_absorpt_T_max   0.792
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.9086
_exptl_absorpt_correction_T_max  0.9879
_exptl_absorpt_process_details   'face indexed'
_exptl_absorpt_special_details   
; 
programs X-Red32 and X-Shape by STOE & Cie GmbH 2010
;
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            17816
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.700
_diffrn_reflns_theta_max         29.457
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             8328
_reflns_number_gt                8014
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_max     0.946
_reflns_Friedel_fraction_full    0.982

_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_cell_refinement       'X-Area by STOE & Cie GmbH 2010'
_computing_data_reduction        'X-Area by STOE & Cie GmbH 2010'
_computing_structure_solution    'SHELXT-2016 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016 (Sheldrick, 2016)'
_computing_molecular_graphics    'XP Version 5.1 by Bruker AXS 1998'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'

_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)+(0.0699P)²+1.2556P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0140(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3565 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8328
_refine_ls_number_parameters     351
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0949
_refine_ls_wR_factor_gt          0.0863
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_restrained_S_all      0.913
_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 0.32520(3) 0.42103(2) 0.73101(2) 0.01643(9) Uani 1 1 d . . . . .
S1 S 0.13339(11) 0.44774(6) 0.59409(8) 0.02109(19) Uani 1 1 d . . . . .
S2 S 0.23610(10) 0.56541(7) 0.81448(8) 0.02025(18) Uani 1 1 d . . . . .
S3 S 0.27447(10) 0.25129(7) 0.69924(7) 0.02034(18) Uani 1 1 d . . . . .
S4 S 0.38669(10) 0.36797(6) 0.91820(8) 0.01984(18) Uani 1 1 d . . . . .
O1 O 0.4757(3) 0.4492(2) 0.6720(2) 0.0249(6) Uani 1 1 d . . . . .
N1 N 0.0009(4) 0.6123(3) 0.5298(3) 0.0257(7) Uani 1 1 d . . . . .
N2 N 0.0883(4) 0.7153(3) 0.7249(3) 0.0239(6) Uani 1 1 d . . . . .
N3 N 0.3408(4) 0.0891(2) 0.8150(3) 0.0233(6) Uani 1 1 d . . . . .
N4 N 0.4478(4) 0.1928(3) 1.0045(3) 0.0237(6) Uani 1 1 d . . . . .
C1 C 0.0805(4) 0.5698(3) 0.6107(3) 0.0193(6) Uani 1 1 d . . . . .
C2 C 0.1256(4) 0.6220(3) 0.7097(3) 0.0193(7) Uani 1 1 d . . . . .
C3 C 0.0103(5) 0.7580(3) 0.6408(4) 0.0276(8) Uani 1 1 d . . . . .
H3 H -0.016194 0.824986 0.647811 0.033 Uiso 1 1 calc R U . . .
C4 C -0.0328(5) 0.7075(3) 0.5442(4) 0.0281(8) Uani 1 1 d . . . . .
H4 H -0.087548 0.740858 0.486565 0.034 Uiso 1 1 calc R U . . .
C5 C 0.3427(4) 0.1874(3) 0.8172(3) 0.0181(6) Uani 1 1 d . . . . .
C6 C 0.3953(4) 0.2395(3) 0.9139(3) 0.0181(6) Uani 1 1 d . . . . .
C7 C 0.3969(5) 0.0432(3) 0.9075(4) 0.0253(8) Uani 1 1 d . . . . .
H7 H 0.399477 -0.026686 0.908565 0.030 Uiso 1 1 calc R U . . .
C8 C 0.4501(5) 0.0935(3) 0.9997(3) 0.0245(7) Uani 1 1 d . . . . .
H8 H 0.489873 0.057563 1.062182 0.029 Uiso 1 1 calc R U . . .
N5 N 0.9060(4) 0.3070(3) 0.9255(3) 0.0218(6) Uani 1 1 d . . . . .
C9 C 0.9188(5) 0.3789(4) 0.8305(4) 0.0297(8) Uani 1 1 d . . . . .
H9A H 1.007665 0.416095 0.844916 0.036 Uiso 1 1 calc R U . . .
H9B H 0.926398 0.340796 0.760973 0.036 Uiso 1 1 calc R U . . .
C10 C 0.8004(6) 0.4512(4) 0.8113(5) 0.0402(11) Uani 1 1 d . . . . .
H10A H 0.712509 0.415818 0.791088 0.060 Uiso 1 1 calc R U . . .
H10B H 0.820846 0.495989 0.750592 0.060 Uiso 1 1 calc R U . . .
H10C H 0.790569 0.489199 0.879662 0.060 Uiso 1 1 calc R U . . .
C11 C 1.0279(5) 0.2363(3) 0.9184(4) 0.0269(8) Uani 1 1 d . . . . .
H11A H 1.116305 0.274809 0.919467 0.032 Uiso 1 1 calc R U . . .
H11B H 1.016507 0.201499 0.845916 0.032 Uiso 1 1 calc R U . . .
C12 C 1.0427(6) 0.1602(4) 1.0112(5) 0.0415(12) Uani 1 1 d . . . . .
H12A H 1.055392 0.193595 1.083565 0.062 Uiso 1 1 calc R U . . .
H12B H 1.124730 0.118422 1.000941 0.062 Uiso 1 1 calc R U . . .
H12C H 0.957635 0.119400 1.008990 0.062 Uiso 1 1 calc R U . . .
C13 C 0.9127(5) 0.3589(3) 1.0370(4) 0.0281(8) Uani 1 1 d . . . . .
H13A H 0.887684 0.311350 1.094758 0.034 Uiso 1 1 calc R U . . .
H13B H 0.841008 0.411825 1.033678 0.034 Uiso 1 1 calc R U . . .
C14 C 1.0547(6) 0.4035(4) 1.0728(4) 0.0393(11) Uani 1 1 d . . . . .
H14A H 1.123712 0.350894 1.088448 0.059 Uiso 1 1 calc R U . . .
H14B H 1.046841 0.443104 1.140301 0.059 Uiso 1 1 calc R U . . .
H14C H 1.085437 0.445521 1.012895 0.059 Uiso 1 1 calc R U . . .
C15 C 0.7657(5) 0.2534(4) 0.9157(5) 0.0358(10) Uani 1 1 d . . . . .
H15A H 0.764226 0.205221 0.977380 0.043 Uiso 1 1 calc R U . . .
H15B H 0.689550 0.301706 0.925055 0.043 Uiso 1 1 calc R U . . .
C16 C 0.7347(6) 0.2000(6) 0.8062(7) 0.0581(19) Uani 1 1 d . . . . .
H16A H 0.728878 0.247634 0.744796 0.087 Uiso 1 1 calc R U . . .
H16B H 0.644959 0.164842 0.807544 0.087 Uiso 1 1 calc R U . . .
H16C H 0.810369 0.152778 0.795263 0.087 Uiso 1 1 calc R U . . .
N6 N 0.4909(4) 0.8184(3) 0.6192(3) 0.0236(6) Uani 1 1 d . . . . .
C17 C 0.4774(5) 0.7556(3) 0.5150(4) 0.0284(8) Uani 1 1 d . . . . .
H17A H 0.567539 0.720585 0.508066 0.034 Uiso 1 1 calc R U . . .
H17B H 0.461483 0.799183 0.449271 0.034 Uiso 1 1 calc R U . . .
C18 C 0.3597(6) 0.6805(4) 0.5127(5) 0.0399(11) Uani 1 1 d . . . . .
H18A H 0.375002 0.636122 0.576739 0.060 Uiso 1 1 calc R U . . .
H18B H 0.358523 0.642400 0.443361 0.060 Uiso 1 1 calc R U . . .
H18C H 0.269254 0.714413 0.516463 0.060 Uiso 1 1 calc R U . . .
C19 C 0.5145(5) 0.7557(3) 0.7237(4) 0.0307(9) Uani 1 1 d . . . . .
H19A H 0.527492 0.799934 0.789101 0.037 Uiso 1 1 calc R U . . .
H19B H 0.428481 0.716309 0.732297 0.037 Uiso 1 1 calc R U . . .
C20 C 0.6381(7) 0.6872(4) 0.7250(5) 0.0429(12) Uani 1 1 d . . . . .
H20A H 0.622769 0.639068 0.664517 0.064 Uiso 1 1 calc R U . . .
H20B H 0.648396 0.652751 0.796800 0.064 Uiso 1 1 calc R U . . .
H20C H 0.723805 0.724947 0.714458 0.064 Uiso 1 1 calc R U . . .
C21 C 0.6169(5) 0.8847(3) 0.6058(4) 0.0272(8) Uani 1 1 d . . . . .
H21A H 0.700179 0.842578 0.596975 0.033 Uiso 1 1 calc R U . . .
H21B H 0.599140 0.922819 0.535958 0.033 Uiso 1 1 calc R U . . .
C22 C 0.6523(6) 0.9554(4) 0.6992(5) 0.0409(11) Uani 1 1 d . . . . .
H22A H 0.575275 1.002817 0.703376 0.061 Uiso 1 1 calc R U . . .
H22B H 0.739328 0.990420 0.685583 0.061 Uiso 1 1 calc R U . . .
H22C H 0.665336 0.919185 0.769768 0.061 Uiso 1 1 calc R U . . .
C23 C 0.3592(5) 0.8793(4) 0.6317(4) 0.0311(9) Uani 1 1 d . . . . .
H23A H 0.280989 0.834096 0.645954 0.037 Uiso 1 1 calc R U . . .
H23B H 0.375756 0.921891 0.698275 0.037 Uiso 1 1 calc R U . . .
C24 C 0.3135(7) 0.9428(6) 0.5342(5) 0.0554(18) Uani 1 1 d . . . . .
H24A H 0.389742 0.988261 0.519117 0.083 Uiso 1 1 calc R U . . .
H24B H 0.229847 0.980398 0.551091 0.083 Uiso 1 1 calc R U . . .
H24C H 0.291034 0.901382 0.468535 0.083 Uiso 1 1 calc R U . . .
O2 O -0.0393(5) 0.5390(4) 0.2969(3) 0.0454(9) Uani 1 1 d D . . . .
H1O2 H -0.128(6) 0.552(5) 0.277(6) 0.040(17) Uiso 1 1 d D . . . .
H2O2 H -0.018(9) 0.562(7) 0.364(5) 0.06(3) Uiso 1 1 d 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 O1 1.688(3) . ?
Mo1 S3 2.3818(10) . ?
Mo1 S2 2.3875(10) . ?
Mo1 S4 2.3923(11) . ?
Mo1 S1 2.3923(12) . ?
S1 C1 1.749(4) . ?
S2 C2 1.756(4) . ?
S3 C5 1.745(4) . ?
S4 C6 1.749(4) . ?
N1 C1 1.320(5) . ?
N1 C4 1.348(5) . ?
N2 C2 1.332(5) . ?
N2 C3 1.340(6) . ?
N3 C5 1.335(5) . ?
N3 C7 1.350(5) . ?
N4 C6 1.326(5) . ?
N4 C8 1.352(5) . ?
C1 C2 1.424(5) . ?
C3 C4 1.384(6) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.420(5) . ?
C7 C8 1.366(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
N5 C13 1.512(5) . ?
N5 C9 1.513(5) . ?
N5 C11 1.514(5) . ?
N5 C15 1.518(6) . ?
C9 C10 1.500(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.520(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.514(7) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.512(8) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N6 C17 1.513(5) . ?
N6 C21 1.517(5) . ?
N6 C23 1.518(6) . ?
N6 C19 1.520(5) . ?
C17 C18 1.514(7) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.499(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.496(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.493(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
O2 H1O2 0.88(6) . ?
O2 H2O2 0.88(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 S3 108.70(10) . . ?
O1 Mo1 S2 109.18(10) . . ?
S3 Mo1 S2 142.11(4) . . ?
O1 Mo1 S4 107.88(11) . . ?
S3 Mo1 S4 83.75(3) . . ?
S2 Mo1 S4 85.57(3) . . ?
O1 Mo1 S1 107.73(11) . . ?
S3 Mo1 S1 84.35(3) . . ?
S2 Mo1 S1 83.53(3) . . ?
S4 Mo1 S1 144.38(4) . . ?
C1 S1 Mo1 106.09(13) . . ?
C2 S2 Mo1 105.76(13) . . ?
C5 S3 Mo1 107.05(13) . . ?
C6 S4 Mo1 106.36(13) . . ?
C1 N1 C4 117.1(4) . . ?
C2 N2 C3 116.6(4) . . ?
C5 N3 C7 116.3(4) . . ?
C6 N4 C8 116.7(4) . . ?
N1 C1 C2 121.2(3) . . ?
N1 C1 S1 119.1(3) . . ?
C2 C1 S1 119.8(3) . . ?
N2 C2 C1 121.4(3) . . ?
N2 C2 S2 118.1(3) . . ?
C1 C2 S2 120.5(3) . . ?
N2 C3 C4 122.0(4) . . ?
N2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
N1 C4 C3 121.7(4) . . ?
N1 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
N3 C5 C6 121.2(3) . . ?
N3 C5 S3 118.5(3) . . ?
C6 C5 S3 120.2(3) . . ?
N4 C6 C5 121.4(3) . . ?
N4 C6 S4 118.0(3) . . ?
C5 C6 S4 120.5(3) . . ?
N3 C7 C8 122.4(4) . . ?
N3 C7 H7 118.8 . . ?
C8 C7 H7 118.8 . . ?
N4 C8 C7 121.9(4) . . ?
N4 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C13 N5 C9 111.5(3) . . ?
C13 N5 C11 111.3(3) . . ?
C9 N5 C11 105.2(3) . . ?
C13 N5 C15 105.8(3) . . ?
C9 N5 C15 111.7(4) . . ?
C11 N5 C15 111.4(3) . . ?
C10 C9 N5 116.0(4) . . ?
C10 C9 H9A 108.3 . . ?
N5 C9 H9A 108.3 . . ?
C10 C9 H9B 108.3 . . ?
N5 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
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 . . ?
N5 C11 C12 114.9(4) . . ?
N5 C11 H11A 108.5 . . ?
C12 C11 H11A 108.5 . . ?
N5 C11 H11B 108.5 . . ?
C12 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N5 C13 C14 114.7(4) . . ?
N5 C13 H13A 108.6 . . ?
C14 C13 H13A 108.6 . . ?
N5 C13 H13B 108.6 . . ?
C14 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
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 . . ?
C16 C15 N5 114.3(4) . . ?
C16 C15 H15A 108.7 . . ?
N5 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
N5 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
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 . . ?
C17 N6 C21 105.5(3) . . ?
C17 N6 C23 111.7(4) . . ?
C21 N6 C23 110.6(3) . . ?
C17 N6 C19 111.4(3) . . ?
C21 N6 C19 110.5(3) . . ?
C23 N6 C19 107.3(3) . . ?
N6 C17 C18 114.4(4) . . ?
N6 C17 H17A 108.7 . . ?
C18 C17 H17A 108.7 . . ?
N6 C17 H17B 108.7 . . ?
C18 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
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 . . ?
C20 C19 N6 115.2(4) . . ?
C20 C19 H19A 108.5 . . ?
N6 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
N6 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 N6 115.9(4) . . ?
C22 C21 H21A 108.3 . . ?
N6 C21 H21A 108.3 . . ?
C22 C21 H21B 108.3 . . ?
N6 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 N6 115.6(4) . . ?
C24 C23 H23A 108.4 . . ?
N6 C23 H23A 108.4 . . ?
C24 C23 H23B 108.4 . . ?
N6 C23 H23B 108.4 . . ?
H23A C23 H23B 107.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
H1O2 O2 H2O2 109(8) . . ?

_refine_diff_density_max         0.930
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.100

