# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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 1575376'
_audit_update_record             
;
2017-10-28 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Br6 Cd Mo6 N6 O4 Se2'
_chemical_formula_weight         1545.54

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_H-M_alt        'P 31 2 1'
_space_group_name_Hall           'P 31 2"'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'

_cell_length_a                   13.2807(5)
_cell_length_b                   13.2807(5)
_cell_length_c                   14.1753(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2165.23(19)
_cell_formula_units_Z            3
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9971
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      27.49

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.556
_exptl_crystal_F_000             2064
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    14.093
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5392
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8186
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.280
_diffrn_reflns_theta_max         27.521
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             3283
_reflns_number_gt                2963
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.994

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+46.5696P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.27(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3283
_refine_ls_number_parameters     131
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1212
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
Cd1 Cd 0.000000 0.61319(14) 0.666667 0.0318(4) Uani 1 2 d S T P . .
Mo4 Mo 0.27507(14) 0.43127(14) 0.53613(9) 0.0249(3) Uani 1 1 d . . . . .
Mo2 Mo 0.37583(14) 0.33165(16) 0.62665(9) 0.0282(3) Uani 1 1 d . . . . .
Mo3 Mo 0.21337(16) 0.21337(16) 0.500000 0.0283(5) Uani 1 2 d DS T P . .
Mo1 Mo 0.49382(16) 0.49382(16) 0.500000 0.0341(5) Uani 1 2 d DS T P . .
Br1 Br 0.43575(19) 0.54615(19) 0.66001(15) 0.0434(5) Uani 0.75 1 d . . P . .
Se1 Se 0.43575(19) 0.54615(19) 0.66001(15) 0.0434(5) Uani 0.25 1 d . . P . .
Br2 Br 0.16058(17) 0.27008(19) 0.66070(13) 0.0387(5) Uani 0.75 1 d . . P . .
Se2 Se 0.16058(17) 0.27008(19) 0.66070(13) 0.0387(5) Uani 0.25 1 d . . P . .
Br3 Br 0.11659(19) 0.3126(2) 0.41034(15) 0.0447(6) Uani 0.75 1 d . . P . .
Se3 Se 0.11659(19) 0.3126(2) 0.41034(15) 0.0447(6) Uani 0.25 1 d . . P . .
Br4 Br 0.3932(2) 0.59074(19) 0.41108(17) 0.0508(6) Uani 0.75 1 d . . P . .
Se4 Se 0.3932(2) 0.59074(19) 0.41108(17) 0.0508(6) Uani 0.25 1 d . . P . .
N4 N 0.1274(19) 0.5634(19) 0.6077(13) 0.051(5) Uani 1 1 d . . . . .
C4 C 0.183(2) 0.521(2) 0.5808(13) 0.048(5) Uani 1 1 d . . . . .
O2 O 0.3106(11) 0.8401(15) 0.5025(8) 0.045(4) Uani 1 1 d . . . . .
C2 C -0.0884(19) 0.599(3) 0.4453(15) 0.058(6) Uani 1 1 d . . . . .
O1 O 0.124(2) 0.8046(17) 0.6155(19) 0.102(9) Uani 1 1 d . . . . .
N2 N -0.0938(18) 0.584(2) 0.5238(13) 0.070(7) Uani 1 1 d . . . . .
C1 C 0.659(2) 0.659(2) 0.500000 0.181(15) Uiso 1 2 d DS . P . .
N1 N 0.745(3) 0.745(3) 0.500000 0.181(15) Uiso 1 2 d DS . P . .
C3 C 0.051(2) 0.051(2) 0.500000 0.181(15) Uiso 1 2 d DS . P . .
N3 N -0.036(2) -0.036(2) 0.500000 0.181(15) Uiso 1 2 d DS . 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
Cd1 N4 2.262(17) 6_556 ?
Cd1 N4 2.262(17) . ?
Cd1 N2 2.31(2) 6_556 ?
Cd1 N2 2.31(2) . ?
Cd1 O1 2.347(18) 6_556 ?
Cd1 O1 2.348(18) . ?
Mo4 C4 2.18(2) . ?
Mo4 Br1 2.590(2) . ?
Mo4 Br2 2.599(2) . ?
Mo4 Br4 2.601(3) . ?
Mo4 Br3 2.603(3) . ?
Mo4 Mo3 2.634(2) . ?
Mo4 Mo2 2.638(2) . ?
Mo4 Mo1 2.642(2) . ?
Mo2 C2 2.21(2) 2_665 ?
Mo2 Br1 2.589(3) . ?
Mo2 Br2 2.595(2) . ?
Mo2 Br3 2.596(3) 4_556 ?
Mo2 Br4 2.602(3) 4_556 ?
Mo2 Mo1 2.635(2) . ?
Mo2 Mo3 2.6375(19) . ?
Mo3 C3 2.16(3) . ?
Mo3 Br3 2.588(2) 4_556 ?
Mo3 Br3 2.588(2) . ?
Mo3 Br2 2.6030(19) . ?
Mo3 Br2 2.6030(19) 4_556 ?
Mo1 C1 2.19(3) . ?
Mo1 Br4 2.599(3) 4_556 ?
Mo1 Br4 2.599(3) . ?
Mo1 Br1 2.5996(19) 4_556 ?
Mo1 Br1 2.5996(19) . ?
N4 C4 1.19(3) . ?
C2 N2 1.13(3) . ?
C1 N1 1.14(3) . ?
C3 N3 1.148(14) . ?

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
N4 Cd1 N4 96.4(11) 6_556 . ?
N4 Cd1 N2 92.7(8) 6_556 6_556 ?
N4 Cd1 N2 95.2(8) . 6_556 ?
N4 Cd1 N2 95.2(8) 6_556 . ?
N4 Cd1 N2 92.7(8) . . ?
N2 Cd1 N2 168.1(15) 6_556 . ?
N4 Cd1 O1 88.9(8) 6_556 6_556 ?
N4 Cd1 O1 174.4(8) . 6_556 ?
N2 Cd1 O1 86.4(9) 6_556 6_556 ?
N2 Cd1 O1 84.9(10) . 6_556 ?
N4 Cd1 O1 174.4(8) 6_556 . ?
N4 Cd1 O1 88.9(8) . . ?
N2 Cd1 O1 84.9(10) 6_556 . ?
N2 Cd1 O1 86.4(9) . . ?
O1 Cd1 O1 85.8(12) 6_556 . ?
C4 Mo4 Br1 90.2(6) . . ?
C4 Mo4 Br2 89.7(7) . . ?
Br1 Mo4 Br2 89.71(8) . . ?
C4 Mo4 Br4 91.6(7) . . ?
Br1 Mo4 Br4 89.92(10) . . ?
Br2 Mo4 Br4 178.61(9) . . ?
C4 Mo4 Br3 91.4(6) . . ?
Br1 Mo4 Br3 178.36(9) . . ?
Br2 Mo4 Br3 90.21(9) . . ?
Br4 Mo4 Br3 90.12(9) . . ?
C4 Mo4 Mo3 134.7(8) . . ?
Br1 Mo4 Mo3 119.41(7) . . ?
Br2 Mo4 Mo3 59.65(6) . . ?
Br4 Mo4 Mo3 119.46(7) . . ?
Br3 Mo4 Mo3 59.22(7) . . ?
C4 Mo4 Mo2 134.0(5) . . ?
Br1 Mo4 Mo2 59.37(7) . . ?
Br2 Mo4 Mo2 59.41(6) . . ?
Br4 Mo4 Mo2 119.30(9) . . ?
Br3 Mo4 Mo2 119.26(8) . . ?
Mo3 Mo4 Mo2 60.04(5) . . ?
C4 Mo4 Mo1 135.4(8) . . ?
Br1 Mo4 Mo1 59.58(6) . . ?
Br2 Mo4 Mo1 119.28(7) . . ?
Br4 Mo4 Mo1 59.42(7) . . ?
Br3 Mo4 Mo1 119.12(7) . . ?
Mo3 Mo4 Mo1 89.82(6) . . ?
Mo2 Mo4 Mo1 59.87(5) . . ?
C2 Mo2 Br1 88.1(7) 2_665 . ?
C2 Mo2 Br2 89.4(7) 2_665 . ?
Br1 Mo2 Br2 89.82(8) . . ?
C2 Mo2 Br3 93.2(7) 2_665 4_556 ?
Br1 Mo2 Br3 178.55(9) . 4_556 ?
Br2 Mo2 Br3 89.51(9) . 4_556 ?
C2 Mo2 Br4 91.7(7) 2_665 4_556 ?
Br1 Mo2 Br4 90.38(9) . 4_556 ?
Br2 Mo2 Br4 178.85(9) . 4_556 ?
Br3 Mo2 Br4 90.26(9) 4_556 4_556 ?
C2 Mo2 Mo1 133.9(9) 2_665 . ?
Br1 Mo2 Mo1 59.68(6) . . ?
Br2 Mo2 Mo1 119.70(7) . . ?
Br3 Mo2 Mo1 119.65(7) 4_556 . ?
Br4 Mo2 Mo1 59.51(7) 4_556 . ?
C2 Mo2 Mo3 136.1(9) 2_665 . ?
Br1 Mo2 Mo3 119.30(8) . . ?
Br2 Mo2 Mo3 59.65(6) . . ?
Br3 Mo2 Mo3 59.26(6) 4_556 . ?
Br4 Mo2 Mo3 119.30(7) 4_556 . ?
Mo1 Mo2 Mo3 89.89(6) . . ?
C2 Mo2 Mo4 132.4(6) 2_665 . ?
Br1 Mo2 Mo4 59.40(7) . . ?
Br2 Mo2 Mo4 59.56(6) . . ?
Br3 Mo2 Mo4 119.16(8) 4_556 . ?
Br4 Mo2 Mo4 119.64(9) 4_556 . ?
Mo1 Mo2 Mo4 60.14(5) . . ?
Mo3 Mo2 Mo4 59.90(5) . . ?
C2 Mo2 Mo4 137.5(6) 2_665 4_556 ?
Br1 Mo2 Mo4 119.75(8) . 4_556 ?
Br2 Mo2 Mo4 119.49(8) . 4_556 ?
Br3 Mo2 Mo4 59.58(7) 4_556 4_556 ?
Br4 Mo2 Mo4 59.46(6) 4_556 4_556 ?
Mo1 Mo2 Mo4 60.07(5) . 4_556 ?
Mo3 Mo2 Mo4 59.84(5) . 4_556 ?
Mo4 Mo2 Mo4 90.07(6) . 4_556 ?
C3 Mo3 Br3 90.36(7) . 4_556 ?
C3 Mo3 Br3 90.36(7) . . ?
Br3 Mo3 Br3 179.29(14) 4_556 . ?
C3 Mo3 Br2 90.57(6) . . ?
Br3 Mo3 Br2 89.52(7) 4_556 . ?
Br3 Mo3 Br2 90.47(7) . . ?
C3 Mo3 Br2 90.57(6) . 4_556 ?
Br3 Mo3 Br2 90.47(7) 4_556 4_556 ?
Br3 Mo3 Br2 89.52(7) . 4_556 ?
Br2 Mo3 Br2 178.86(13) . 4_556 ?
C3 Mo3 Mo4 134.82(4) . . ?
Br3 Mo3 Mo4 119.62(8) 4_556 . ?
Br3 Mo3 Mo4 59.80(6) . . ?
Br2 Mo3 Mo4 59.52(6) . . ?
Br2 Mo3 Mo4 119.55(8) 4_556 . ?
C3 Mo3 Mo4 134.82(4) . 4_556 ?
Br3 Mo3 Mo4 59.80(6) 4_556 4_556 ?
Br3 Mo3 Mo4 119.62(8) . 4_556 ?
Br2 Mo3 Mo4 119.55(8) . 4_556 ?
Br2 Mo3 Mo4 59.52(6) 4_556 4_556 ?
Mo4 Mo3 Mo4 90.36(9) . 4_556 ?
C3 Mo3 Mo2 134.97(4) . 4_556 ?
Br3 Mo3 Mo2 119.85(8) 4_556 4_556 ?
Br3 Mo3 Mo2 59.57(7) . 4_556 ?
Br2 Mo3 Mo2 119.70(8) . 4_556 ?
Br2 Mo3 Mo2 59.37(6) 4_556 4_556 ?
Mo4 Mo3 Mo2 60.18(5) . 4_556 ?
Mo4 Mo3 Mo2 60.05(6) 4_556 4_556 ?
C3 Mo3 Mo2 134.97(4) . . ?
Br3 Mo3 Mo2 59.57(7) 4_556 . ?
Br3 Mo3 Mo2 119.85(8) . . ?
Br2 Mo3 Mo2 59.37(6) . . ?
Br2 Mo3 Mo2 119.70(8) 4_556 . ?
Mo4 Mo3 Mo2 60.05(6) . . ?
Mo4 Mo3 Mo2 60.18(5) 4_556 . ?
Mo2 Mo3 Mo2 90.05(9) 4_556 . ?
C1 Mo1 Br4 90.55(7) . 4_556 ?
C1 Mo1 Br4 90.55(7) . . ?
Br4 Mo1 Br4 178.91(15) 4_556 . ?
C1 Mo1 Br1 90.84(6) . 4_556 ?
Br4 Mo1 Br1 89.77(7) 4_556 4_556 ?
Br4 Mo1 Br1 90.22(7) . 4_556 ?
C1 Mo1 Br1 90.84(6) . . ?
Br4 Mo1 Br1 90.21(7) 4_556 . ?
Br4 Mo1 Br1 89.77(7) . . ?
Br1 Mo1 Br1 178.32(13) 4_556 . ?
C1 Mo1 Mo2 134.92(4) . 4_556 ?
Br4 Mo1 Mo2 119.50(8) 4_556 4_556 ?
Br4 Mo1 Mo2 59.61(7) . 4_556 ?
Br1 Mo1 Mo2 59.29(6) 4_556 4_556 ?
Br1 Mo1 Mo2 119.34(8) . 4_556 ?
C1 Mo1 Mo2 134.91(4) . . ?
Br4 Mo1 Mo2 59.61(7) 4_556 . ?
Br4 Mo1 Mo2 119.50(8) . . ?
Br1 Mo1 Mo2 119.34(8) 4_556 . ?
Br1 Mo1 Mo2 59.29(6) . . ?
Mo2 Mo1 Mo2 90.17(9) 4_556 . ?
C1 Mo1 Mo4 135.00(4) . . ?
Br4 Mo1 Mo4 119.60(8) 4_556 . ?
Br4 Mo1 Mo4 59.51(6) . . ?
Br1 Mo1 Mo4 119.40(8) 4_556 . ?
Br1 Mo1 Mo4 59.22(6) . . ?
Mo2 Mo1 Mo4 60.12(6) 4_556 . ?
Mo2 Mo1 Mo4 59.99(6) . . ?
C1 Mo1 Mo4 134.99(4) . 4_556 ?
Br4 Mo1 Mo4 59.51(6) 4_556 4_556 ?
Br4 Mo1 Mo4 119.60(8) . 4_556 ?
Br1 Mo1 Mo4 59.22(6) 4_556 4_556 ?
Br1 Mo1 Mo4 119.40(8) . 4_556 ?
Mo2 Mo1 Mo4 59.99(6) 4_556 4_556 ?
Mo2 Mo1 Mo4 60.12(6) . 4_556 ?
Mo4 Mo1 Mo4 90.01(9) . 4_556 ?
Mo2 Br1 Mo4 61.23(6) . . ?
Mo2 Br1 Mo1 61.03(6) . . ?
Mo4 Br1 Mo1 61.20(6) . . ?
Mo2 Br2 Mo4 61.03(6) . . ?
Mo2 Br2 Mo3 60.98(6) . . ?
Mo4 Br2 Mo3 60.83(6) . . ?
Mo3 Br3 Mo2 61.17(7) . 4_556 ?
Mo3 Br3 Mo4 60.98(7) . . ?
Mo2 Br3 Mo4 61.11(6) 4_556 . ?
Mo1 Br4 Mo4 61.07(7) . . ?
Mo1 Br4 Mo2 60.88(7) . 4_556 ?
Mo4 Br4 Mo2 61.06(6) . 4_556 ?
C4 N4 Cd1 170(2) . . ?
N4 C4 Mo4 176(2) . . ?
N2 C2 Mo2 168(2) . 3_564 ?
C2 N2 Cd1 149.0(19) . . ?
N1 C1 Mo1 180(3) . . ?
N3 C3 Mo3 180.0(17) . . ?

_refine_diff_density_max         1.773
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.238

####################################################################### 
# 
# 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_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1575378'
_audit_update_record             
;
2017-09-19 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Residual Density  1.01A From     Cs1       3.72 eA-3
RESPONSE: There is a residual density close to the heavy Cs atom. It does not correspond to any relevant atom. That compound is isostructural to related Se compound Csx[trans-MnIIxMnIII(1-x)(H2O)2][Mo6Br6Se2(CN)6] so we are confident with the proposed formula. We do not have better data to proceed to another refinement.
;
_vrf_PLAT975_shelx               
;
PROBLEM: Check Calcd Residual Density  0.81A From      O1       2.31 eA-3
RESPONSE: indeed we can enter a H atom at this position and restrain its distance to O1 to reliable value. It does not improve the refinement. More important we can not find any other H atom close to O1 to complete the expected water molecule. That compound is isostructural to related Se compound Csx[trans-MnIIxMnIII(1-x)(H2O)2][Mo6Br6Se2(CN)6] so we are confident with the proposed formula. We do not have better data to proceed to another refinement.
;
_vrf_PLAT971_shelx_2             
;
PROBLEM: Check Calcd Residual Density  0.94A From     Cs1       2.61 eA-3
RESPONSE: As for alerte PLAT971. There is a residual density close to the heavy Cs atom. It does not correspond to any relevant atom. That compound is isostructural to related Se compound Csx[trans-MnIIxMnIII(1-x)(H2O)2][Mo6Br6Se2(CN)6] so we are confident with the proposed formula. We do not have better data to proceed to another refinement.
;
# Added during the CSD deposition process: Tuesday 19 September 2017 05:51 PM
# end Validation Reply Form


_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            'C6 Br6 Cs0.68 Mn Mo6 N6 O2 S2'
_chemical_formula_weight         1451.99

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'

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

_cell_length_a                   19.5490(8)
_cell_length_b                   10.3084(4)
_cell_length_c                   13.7398(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2768.83(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      39.89

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.483
_exptl_crystal_F_000             2600
_exptl_transmission_factor_min   0.5406
_exptl_transmission_factor_max   0.7479
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    12.770
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microfocus sealed tube'
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector_area_resol_mean '(CMOS) PHOTON 100'
_diffrn_reflns_number            15682
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.460
_diffrn_reflns_theta_max         40.355
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             4642
_reflns_number_gt                3353
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0488P)²+22.7688P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00060(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4642
_refine_ls_number_parameters     88
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.1123
_refine_ls_wR_factor_gt          0.1044
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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 0.30244(2) 0.7500 0.63651(3) 0.01017(7) Uani 1 2 d S T P . .
Mo2 Mo 0.30696(2) 0.62257(2) 0.80194(2) 0.01138(6) Uani 1 1 d . . . . .
Br1 Br 0.41123(3) 0.7500 0.74095(5) 0.01586(12) Uani 0.5 2 d S T P . .
S1 S 0.41123(3) 0.7500 0.74095(5) 0.01586(12) Uani 0.5 2 d S T P . .
Br2 Br 0.30045(2) 0.49724(3) 0.63801(3) 0.01578(8) Uani 0.8334 1 d . . P . .
S2 S 0.30045(2) 0.49724(3) 0.63801(3) 0.01578(8) Uani 0.1666 1 d . . P . .
Br3 Br 0.19028(3) 0.7500 0.53507(4) 0.01478(10) Uani 0.8335 2 d S T P . .
S3 S 0.19028(3) 0.7500 0.53507(4) 0.01478(10) Uani 0.1665 2 d S T P . .
C1 C 0.3686(3) 0.7500 0.5076(4) 0.0193(8) Uani 1 2 d S T P . .
C2 C 0.3788(2) 0.4749(4) 0.8554(3) 0.0247(7) Uani 1 1 d . . . . .
N2 N 0.42058(19) 0.3999(4) 0.8754(3) 0.0317(8) Uani 1 1 d . . . . .
N1 N 0.4073(3) 0.7500 0.4427(4) 0.0321(11) Uani 1 2 d S T P . .
Mn1 Mn 0.5000 0.2500 0.87747(7) 0.01245(16) Uani 1 4 d S T P . .
O1 O 0.5000 0.2500 0.7151(5) 0.052(3) Uani 1 4 d S T P . .
O2 O 0.5000 0.2871(11) 1.0384(6) 0.041(3) Uani 0.5 2 d S T P . .
Cs1 Cs 0.5000 1.01520(12) 0.42753(14) 0.0429(3) Uani 0.3371 2 d S T 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
Mo1 C1 2.193(5) . ?
Mo1 Br1 2.5654(7) . ?
Mo1 Br3 2.5981(6) . ?
Mo1 S2 2.6059(4) 11_575 ?
Mo1 Br2 2.6059(4) 11_575 ?
Mo1 Br2 2.6060(4) . ?
Mo1 Mo2 2.6267(4) . ?
Mo1 Mo2 2.6267(4) 11_575 ?
Mo1 Mo2 2.6484(4) 7_546 ?
Mo2 C2 2.197(4) . ?
Mo2 Br1 2.5657(6) . ?
Mo2 S3 2.5968(5) 13_566 ?
Mo2 Br3 2.5968(5) 13_566 ?
Mo2 Br2 2.5998(4) . ?
Mo2 S2 2.5998(4) 7_546 ?
Mo2 Br2 2.5998(4) 7_546 ?
Mo2 Mo2 2.6271(5) 11_575 ?
Mo2 Mo2 2.6450(5) 7_546 ?
Br1 Mo2 2.5658(6) 11_575 ?
Br1 Cs1 3.7720(15) 10_556 ?
Br1 Cs1 3.7720(15) 9_676 ?
Br2 Mo2 2.5998(4) 7_546 ?
Br2 Cs1 4.0078(6) 10_556 ?
Br3 Mo2 2.5968(5) 13_566 ?
Br3 Mo2 2.5968(5) 7_546 ?
C1 N1 1.170(7) . ?
C1 Cs1 3.640(4) 9_676 ?
C1 Cs1 3.640(4) 10_556 ?
C1 Cs1 3.909(4) . ?
C1 Cs1 3.909(4) 2_665 ?
C2 N2 1.158(5) . ?
N2 Mn1 2.191(3) . ?
N1 Cs1 3.286(3) . ?
N1 Cs1 3.286(3) 2_665 ?
N1 Cs1 3.510(5) 9_676 ?
N1 Cs1 3.510(5) 10_556 ?
Mn1 N2 2.191(3) 11_565 ?
Mn1 N2 2.191(3) 12_655 ?
Mn1 N2 2.191(3) 2_655 ?
Mn1 O1 2.231(7) . ?
Mn1 O2 2.244(9) . ?
Mn1 O2 2.244(9) 2_655 ?
O1 Cs1 3.363(4) 9_666 ?
O1 Cs1 3.363(4) 10_556 ?
O2 O2 0.77(2) 2_655 ?
Cs1 Cs1 2.016(4) 9_676 ?
Cs1 N1 3.286(3) 2_665 ?
Cs1 O1 3.363(4) 9_666 ?
Cs1 N1 3.510(5) 9_676 ?
Cs1 N1 3.510(5) 10_566 ?
Cs1 C1 3.640(4) 9_676 ?
Cs1 C1 3.640(4) 10_566 ?
Cs1 Br1 3.7721(15) 10_566 ?
Cs1 S1 3.7721(15) 10_566 ?
Cs1 Br1 3.7721(15) 9_676 ?
Cs1 S1 3.7721(15) 9_676 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Mo1 Br1 87.86(14) . . ?
C1 Mo1 Br3 93.70(14) . . ?
Br1 Mo1 Br3 178.43(2) . . ?
C1 Mo1 S2 90.869(11) . 11_575 ?
Br1 Mo1 S2 90.456(11) . 11_575 ?
Br3 Mo1 S2 89.521(11) . 11_575 ?
C1 Mo1 Br2 90.869(11) . 11_575 ?
Br1 Mo1 Br2 90.456(11) . 11_575 ?
Br3 Mo1 Br2 89.521(11) . 11_575 ?
S2 Mo1 Br2 0.0 11_575 11_575 ?
C1 Mo1 Br2 90.869(11) . . ?
Br1 Mo1 Br2 90.457(11) . . ?
Br3 Mo1 Br2 89.520(11) . . ?
S2 Mo1 Br2 178.1 11_575 . ?
Br2 Mo1 Br2 178.07(2) 11_575 . ?
C1 Mo1 Mo2 132.76(10) . . ?
Br1 Mo1 Mo2 59.214(15) . . ?
Br3 Mo1 Mo2 119.508(15) . . ?
S2 Mo1 Mo2 119.583(15) 11_575 . ?
Br2 Mo1 Mo2 119.583(15) 11_575 . ?
Br2 Mo1 Mo2 59.581(11) . . ?
C1 Mo1 Mo2 132.76(10) . 11_575 ?
Br1 Mo1 Mo2 59.215(15) . 11_575 ?
Br3 Mo1 Mo2 119.508(15) . 11_575 ?
S2 Mo1 Mo2 59.581(11) 11_575 11_575 ?
Br2 Mo1 Mo2 59.581(11) 11_575 11_575 ?
Br2 Mo1 Mo2 119.583(15) . 11_575 ?
Mo2 Mo1 Mo2 60.010(14) . 11_575 ?
C1 Mo1 Mo2 137.23(10) . 7_546 ?
Br1 Mo1 Mo2 119.393(18) . 7_546 ?
Br3 Mo1 Mo2 59.323(13) . 7_546 ?
S2 Mo1 Mo2 118.773(15) 11_575 7_546 ?
Br2 Mo1 Mo2 118.773(15) 11_575 7_546 ?
Br2 Mo1 Mo2 59.305(11) . 7_546 ?
Mo2 Mo1 Mo2 60.185(12) . 7_546 ?
Mo2 Mo1 Mo2 89.933(13) 11_575 7_546 ?
C2 Mo2 Br1 87.48(11) . . ?
C2 Mo2 S3 92.78(11) . 13_566 ?
Br1 Mo2 S3 90.355(18) . 13_566 ?
C2 Mo2 Br3 92.78(11) . 13_566 ?
Br1 Mo2 Br3 90.355(18) . 13_566 ?
S3 Mo2 Br3 0.0 13_566 13_566 ?
C2 Mo2 Br2 88.68(11) . . ?
Br1 Mo2 Br2 90.589(17) . . ?
S3 Mo2 Br2 178.296(17) 13_566 . ?
Br3 Mo2 Br2 178.296(17) 13_566 . ?
C2 Mo2 S2 93.78(11) . 7_546 ?
Br1 Mo2 S2 178.739(18) . 7_546 ?
S3 Mo2 S2 89.683(15) 13_566 7_546 ?
Br3 Mo2 S2 89.683(15) 13_566 7_546 ?
Br2 Mo2 S2 89.3 . 7_546 ?
C2 Mo2 Br2 93.78(11) . 7_546 ?
Br1 Mo2 Br2 178.739(18) . 7_546 ?
S3 Mo2 Br2 89.683(15) 13_566 7_546 ?
Br3 Mo2 Br2 89.683(15) 13_566 7_546 ?
Br2 Mo2 Br2 89.342(17) . 7_546 ?
S2 Mo2 Br2 0.0 7_546 7_546 ?
C2 Mo2 Mo1 131.09(11) . . ?
Br1 Mo2 Mo1 59.204(17) . . ?
S3 Mo2 Mo1 119.602(12) 13_566 . ?
Br3 Mo2 Mo1 119.602(12) 13_566 . ?
Br2 Mo2 Mo1 59.813(11) . . ?
S2 Mo2 Mo1 119.738(15) 7_546 . ?
Br2 Mo2 Mo1 119.738(15) 7_546 . ?
C2 Mo2 Mo2 133.83(12) . 11_575 ?
Br1 Mo2 Mo2 59.206(9) . 11_575 ?
S3 Mo2 Mo2 59.612(8) 13_566 11_575 ?
Br3 Mo2 Mo2 59.612(8) 13_566 11_575 ?
Br2 Mo2 Mo2 119.801(10) . 11_575 ?
S2 Mo2 Mo2 119.798(10) 7_546 11_575 ?
Br2 Mo2 Mo2 119.798(10) 7_546 11_575 ?
Mo1 Mo2 Mo2 59.995(7) . 11_575 ?
C2 Mo2 Mo2 135.94(12) . 7_546 ?
Br1 Mo2 Mo2 119.512(19) . 7_546 ?
S3 Mo2 Mo2 118.872(16) 13_566 7_546 ?
Br3 Mo2 Mo2 118.872(16) 13_566 7_546 ?
Br2 Mo2 Mo2 59.424(12) . 7_546 ?
S2 Mo2 Mo2 59.423(12) 7_546 7_546 ?
Br2 Mo2 Mo2 59.423(12) 7_546 7_546 ?
Mo1 Mo2 Mo2 60.315(11) . 7_546 ?
Mo2 Mo2 Mo2 90.0 11_575 7_546 ?
Mo1 Br1 Mo2 61.582(16) . . ?
Mo1 Br1 Mo2 61.582(16) . 11_575 ?
Mo2 Br1 Mo2 61.589(19) . 11_575 ?
Mo1 Br1 Cs1 92.19(2) . 10_556 ?
Mo2 Br1 Cs1 103.736(17) . 10_556 ?
Mo2 Br1 Cs1 153.44(3) 11_575 10_556 ?
Mo1 Br1 Cs1 92.19(2) . 9_676 ?
Mo2 Br1 Cs1 153.44(3) . 9_676 ?
Mo2 Br1 Cs1 103.737(17) 11_575 9_676 ?
Cs1 Br1 Cs1 79.83(4) 10_556 9_676 ?
Mo2 Br2 Mo2 61.153(13) . 7_546 ?
Mo2 Br2 Mo1 60.606(12) . . ?
Mo2 Br2 Mo1 61.161(12) 7_546 . ?
Mo2 Br2 Cs1 97.13(3) . 10_556 ?
Mo2 Br2 Cs1 146.56(2) 7_546 10_556 ?
Mo1 Br2 Cs1 86.42(2) . 10_556 ?
Mo2 Br3 Mo2 60.774(16) 13_566 7_546 ?
Mo2 Br3 Mo1 61.302(13) 13_566 . ?
Mo2 Br3 Mo1 61.302(13) 7_546 . ?
N1 C1 Mo1 175.9(5) . . ?
N1 C1 Cs1 74.4(3) . 9_676 ?
Mo1 C1 Cs1 102.62(14) . 9_676 ?
N1 C1 Cs1 74.4(3) . 10_556 ?
Mo1 C1 Cs1 102.62(14) . 10_556 ?
Cs1 C1 Cs1 83.36(11) 9_676 10_556 ?
N1 C1 Cs1 50.24(17) . . ?
Mo1 C1 Cs1 127.94(11) . . ?
Cs1 C1 Cs1 30.71(6) 9_676 . ?
Cs1 C1 Cs1 94.04(12) 10_556 . ?
N1 C1 Cs1 50.24(17) . 2_665 ?
Mo1 C1 Cs1 127.94(11) . 2_665 ?
Cs1 C1 Cs1 94.04(12) 9_676 2_665 ?
Cs1 C1 Cs1 30.71(6) 10_556 2_665 ?
Cs1 C1 Cs1 88.75(11) . 2_665 ?
N2 C2 Mo2 173.1(4) . . ?
C2 N2 Mn1 167.0(4) . . ?
C1 N1 Cs1 113.9(2) . . ?
C1 N1 Cs1 113.9(2) . 2_665 ?
Cs1 N1 Cs1 112.59(16) . 2_665 ?
C1 N1 Cs1 86.9(3) . 9_676 ?
Cs1 N1 Cs1 34.31(7) . 9_676 ?
Cs1 N1 Cs1 108.73(17) 2_665 9_676 ?
C1 N1 Cs1 86.9(3) . 10_556 ?
Cs1 N1 Cs1 108.73(17) . 10_556 ?
Cs1 N1 Cs1 34.31(7) 2_665 10_556 ?
Cs1 N1 Cs1 87.18(15) 9_676 10_556 ?
N2 Mn1 N2 89.7(2) . 11_565 ?
N2 Mn1 N2 90.3(2) . 12_655 ?
N2 Mn1 N2 178.5(2) 11_565 12_655 ?
N2 Mn1 N2 178.5(2) . 2_655 ?
N2 Mn1 N2 90.3(2) 11_565 2_655 ?
N2 Mn1 N2 89.7(2) 12_655 2_655 ?
N2 Mn1 O1 89.24(12) . . ?
N2 Mn1 O1 89.24(12) 11_565 . ?
N2 Mn1 O1 89.24(12) 12_655 . ?
N2 Mn1 O1 89.24(12) 2_655 . ?
N2 Mn1 O2 83.8(2) . . ?
N2 Mn1 O2 97.7(2) 11_565 . ?
N2 Mn1 O2 83.8(2) 12_655 . ?
N2 Mn1 O2 97.7(2) 2_655 . ?
O1 Mn1 O2 170.2(3) . . ?
N2 Mn1 O2 97.7(2) . 2_655 ?
N2 Mn1 O2 83.8(2) 11_565 2_655 ?
N2 Mn1 O2 97.7(2) 12_655 2_655 ?
N2 Mn1 O2 83.8(2) 2_655 2_655 ?
O1 Mn1 O2 170.2(3) . 2_655 ?
O2 Mn1 O2 19.6(6) . 2_655 ?
Mn1 O1 Cs1 125.63(10) . 9_666 ?
Mn1 O1 Cs1 125.63(10) . 10_556 ?
Cs1 O1 Cs1 108.7(2) 9_666 10_556 ?
O2 O2 Mn1 80.2(3) 2_655 . ?
Cs1 Cs1 N1 78.94(12) 9_676 2_665 ?
Cs1 Cs1 N1 78.94(12) 9_676 . ?
N1 Cs1 N1 66.92(17) 2_665 . ?
Cs1 Cs1 O1 116.69(13) 9_676 9_666 ?
N1 Cs1 O1 50.26(11) 2_665 9_666 ?
N1 Cs1 O1 50.26(11) . 9_666 ?
Cs1 Cs1 N1 66.75(10) 9_676 9_676 ?
N1 Cs1 N1 104.89(13) 2_665 9_676 ?
N1 Cs1 N1 145.69(7) . 9_676 ?
O1 Cs1 N1 148.92(8) 9_666 9_676 ?
Cs1 Cs1 N1 66.75(10) 9_676 10_566 ?
N1 Cs1 N1 145.69(7) 2_665 10_566 ?
N1 Cs1 N1 104.89(13) . 10_566 ?
O1 Cs1 N1 148.92(8) 9_666 10_566 ?
N1 Cs1 N1 62.15(16) 9_676 10_566 ?
Cs1 Cs1 C1 82.04(10) 9_676 9_676 ?
N1 Cs1 C1 98.55(10) 2_665 9_676 ?
N1 Cs1 C1 157.93(14) . 9_676 ?
O1 Cs1 C1 133.09(8) 9_666 9_676 ?
N1 Cs1 C1 18.72(11) 9_676 9_676 ?
N1 Cs1 C1 77.36(11) 10_566 9_676 ?
Cs1 Cs1 C1 82.04(10) 9_676 10_566 ?
N1 Cs1 C1 157.93(14) 2_665 10_566 ?
N1 Cs1 C1 98.55(10) . 10_566 ?
O1 Cs1 C1 133.09(8) 9_666 10_566 ?
N1 Cs1 C1 77.36(11) 9_676 10_566 ?
N1 Cs1 C1 18.72(11) 10_566 10_566 ?
C1 Cs1 C1 89.75(12) 9_676 10_566 ?
Cs1 Cs1 Br1 134.91(7) 9_676 10_566 ?
N1 Cs1 Br1 145.72(11) 2_665 10_566 ?
N1 Cs1 Br1 108.60(10) . 10_566 ?
O1 Cs1 Br1 99.44(10) 9_666 10_566 ?
N1 Cs1 Br1 96.13(8) 9_676 10_566 ?
N1 Cs1 Br1 68.40(8) 10_566 10_566 ?
C1 Cs1 Br1 92.76(7) 9_676 10_566 ?
C1 Cs1 Br1 53.05(8) 10_566 10_566 ?
Cs1 Cs1 S1 134.91(7) 9_676 10_566 ?
N1 Cs1 S1 145.72(11) 2_665 10_566 ?
N1 Cs1 S1 108.60(10) . 10_566 ?
O1 Cs1 S1 99.44(10) 9_666 10_566 ?
N1 Cs1 S1 96.13(8) 9_676 10_566 ?
N1 Cs1 S1 68.40(8) 10_566 10_566 ?
C1 Cs1 S1 92.76(7) 9_676 10_566 ?
C1 Cs1 S1 53.05(8) 10_566 10_566 ?
Br1 Cs1 S1 0.000(17) 10_566 10_566 ?
Cs1 Cs1 Br1 134.91(7) 9_676 9_676 ?
N1 Cs1 Br1 108.60(10) 2_665 9_676 ?
N1 Cs1 Br1 145.72(11) . 9_676 ?
O1 Cs1 Br1 99.44(10) 9_666 9_676 ?
N1 Cs1 Br1 68.40(8) 9_676 9_676 ?
N1 Cs1 Br1 96.13(8) 10_566 9_676 ?
C1 Cs1 Br1 53.05(8) 9_676 9_676 ?
C1 Cs1 Br1 92.76(7) 10_566 9_676 ?
Br1 Cs1 Br1 54.79(3) 10_566 9_676 ?
S1 Cs1 Br1 54.8 10_566 9_676 ?
Cs1 Cs1 S1 134.91(7) 9_676 9_676 ?
N1 Cs1 S1 108.60(10) 2_665 9_676 ?
N1 Cs1 S1 145.72(11) . 9_676 ?
O1 Cs1 S1 99.44(10) 9_666 9_676 ?
N1 Cs1 S1 68.40(8) 9_676 9_676 ?
N1 Cs1 S1 96.13(8) 10_566 9_676 ?
C1 Cs1 S1 53.05(8) 9_676 9_676 ?
C1 Cs1 S1 92.76(7) 10_566 9_676 ?
Br1 Cs1 S1 54.79(3) 10_566 9_676 ?
S1 Cs1 S1 54.79(3) 10_566 9_676 ?
Br1 Cs1 S1 0.000(16) 9_676 9_676 ?

_refine_diff_density_max         3.638
_refine_diff_density_min         -2.197
_refine_diff_density_rms         0.279

####################################################################### 
# 
# 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_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1575377'
_audit_update_record             
;
2017-10-26 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT975_shelx               
;
PROBLEM: Check Calcd Residual Density  0.84A From      O2       2.43 eA-3
RESPONSE: There is a residual density close to O2 atom that could be assigned  to H atoms but the second H atom is missing.
;
# Added during the CSD deposition process: Thursday 26 October 2017 08:54 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Br8 Mn Mo6 N6 O2'
_chemical_formula_weight         1457.98

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'

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

_cell_length_a                   19.5758(7)
_cell_length_b                   10.4102(4)
_cell_length_c                   13.7808(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2808.36(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9618
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      27.40

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.448
_exptl_crystal_F_000             2604
_exptl_transmission_factor_min   0.5969
_exptl_transmission_factor_max   0.7456
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.042
_exptl_absorpt_coefficient_mu    14.424
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
'Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microfocus sealed tube'
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images, thin slices'
_diffrn_detector_area_resol_mean '(CMOS) PHOTON 100'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_reflns_number            13490
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.956
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1749
_reflns_number_gt                1709
_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.
 
  PLAT975 Type_2 Test for positive density near N or O:
  There is an alert level A with chckcif. Indeed there is 
  a residual density close to O2 atom that could be assigned
  to H atoms but the second H atom is missing.
;

_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+243.9835P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.00033(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1749
_refine_ls_number_parameters     80
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.1276
_refine_ls_wR_factor_gt          0.1274
_refine_ls_goodness_of_fit_ref   1.367
_refine_ls_restrained_S_all      1.367
_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 0.20052(6) 0.250000 0.63443(9) 0.0104(3) Uani 1 2 d S T P . .
Mo2 Mo 0.30751(5) 0.37651(9) 0.70034(6) 0.0148(2) Uani 1 1 d . . . . .
Br1 Br 0.31393(8) 0.250000 0.53823(11) 0.0247(4) Uani 1 2 d S T P . .
Br2 Br 0.20186(7) 0.49917(11) 0.63655(9) 0.0261(3) Uani 1 1 d . . . . .
Br3 Br 0.08827(8) 0.250000 0.73367(12) 0.0253(4) Uani 1 2 d S T P . .
Mn1 Mn 0.500000 0.750000 0.6355(3) 0.0184(7) Uani 1 4 d S T P . .
O2 O 0.500000 0.750000 0.799(2) 0.058(7) Uani 1 4 d S T P . .
O1 O 0.500000 0.750000 0.4707(15) 0.058(7) Uani 1 4 d S T P . .
N2 N 0.4197(6) 0.5995(13) 0.6297(10) 0.044(3) Uani 1 1 d . . . . .
C1 C 0.1395(9) 0.250000 0.5007(12) 0.021(3) Uani 1 2 d S T P . .
C2 C 0.3793(7) 0.5253(15) 0.6478(10) 0.035(3) Uani 1 1 d . . . . .
N1 N 0.1049(10) 0.250000 0.4328(13) 0.040(4) Uani 1 2 d S T 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
Mo1 C1 2.196(16) . ?
Mo1 Br1 2.586(2) . ?
Mo1 Br3 2.588(2) . ?
Mo1 Br2 2.5942(12) . ?
Mo1 Br2 2.5943(12) 11_565 ?
Mo1 Mo2 2.6350(14) 7_546 ?
Mo1 Mo2 2.6350(14) 13_556 ?
Mo1 Mo2 2.6356(14) . ?
Mo1 Mo2 2.6356(14) 11_565 ?
Mo2 C2 2.213(14) . ?
Mo2 Br2 2.5847(15) . ?
Mo2 Br2 2.5916(15) 7_546 ?
Mo2 Br3 2.5931(17) 13_556 ?
Mo2 Br1 2.5964(16) . ?
Mo2 Mo2 2.6340(19) 11_565 ?
Mo2 Mo2 2.6349(18) 7_546 ?
Mn1 N2 2.222(12) . ?
Mn1 N2 2.222(12) 2_665 ?
Mn1 N2 2.222(12) 12_655 ?
Mn1 N2 2.222(12) 11_575 ?
Mn1 O2 2.25(3) . ?
Mn1 O1 2.27(2) . ?
N2 C2 1.133(18) . ?
C1 N1 1.16(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Mo1 Br1 92.1(5) . . ?
C1 Mo1 Br3 89.0(5) . . ?
Br1 Mo1 Br3 178.95(7) . . ?
C1 Mo1 Br2 90.86(4) . . ?
Br1 Mo1 Br2 89.83(4) . . ?
Br3 Mo1 Br2 90.15(4) . . ?
C1 Mo1 Br2 90.86(4) . 11_565 ?
Br1 Mo1 Br2 89.83(4) . 11_565 ?
Br3 Mo1 Br2 90.15(4) . 11_565 ?
Br2 Mo1 Br2 178.26(8) . 11_565 ?
C1 Mo1 Mo2 133.8(3) . 7_546 ?
Br1 Mo1 Mo2 119.62(5) . 7_546 ?
Br3 Mo1 Mo2 59.52(4) . 7_546 ?
Br2 Mo1 Mo2 59.41(4) . 7_546 ?
Br2 Mo1 Mo2 119.38(5) 11_565 7_546 ?
C1 Mo1 Mo2 133.8(3) . 13_556 ?
Br1 Mo1 Mo2 119.62(5) . 13_556 ?
Br3 Mo1 Mo2 59.52(4) . 13_556 ?
Br2 Mo1 Mo2 119.38(5) . 13_556 ?
Br2 Mo1 Mo2 59.41(4) 11_565 13_556 ?
Mo2 Mo1 Mo2 59.97(5) 7_546 13_556 ?
C1 Mo1 Mo2 136.2(3) . . ?
Br1 Mo1 Mo2 59.63(4) . . ?
Br3 Mo1 Mo2 119.51(5) . . ?
Br2 Mo1 Mo2 59.23(4) . . ?
Br2 Mo1 Mo2 119.19(5) 11_565 . ?
Mo2 Mo1 Mo2 59.99(4) 7_546 . ?
Mo2 Mo1 Mo2 89.96(4) 13_556 . ?
C1 Mo1 Mo2 136.2(3) . 11_565 ?
Br1 Mo1 Mo2 59.63(4) . 11_565 ?
Br3 Mo1 Mo2 119.51(5) . 11_565 ?
Br2 Mo1 Mo2 119.19(5) . 11_565 ?
Br2 Mo1 Mo2 59.23(4) 11_565 11_565 ?
Mo2 Mo1 Mo2 89.96(4) 7_546 11_565 ?
Mo2 Mo1 Mo2 59.99(4) 13_556 11_565 ?
Mo2 Mo1 Mo2 59.96(5) . 11_565 ?
C2 Mo2 Br2 92.9(4) . . ?
C2 Mo2 Br2 89.1(4) . 7_546 ?
Br2 Mo2 Br2 89.71(6) . 7_546 ?
C2 Mo2 Br3 88.3(4) . 13_556 ?
Br2 Mo2 Br3 178.74(6) . 13_556 ?
Br2 Mo2 Br3 90.10(5) 7_546 13_556 ?
C2 Mo2 Br1 92.4(4) . . ?
Br2 Mo2 Br1 89.81(5) . . ?
Br2 Mo2 Br1 178.42(6) 7_546 . ?
Br3 Mo2 Br1 90.35(6) 13_556 . ?
C2 Mo2 Mo2 134.4(4) . 11_565 ?
Br2 Mo2 Mo2 119.61(3) . 11_565 ?
Br2 Mo2 Mo2 119.52(3) 7_546 11_565 ?
Br3 Mo2 Mo2 59.48(3) 13_556 11_565 ?
Br1 Mo2 Mo2 59.52(3) . 11_565 ?
C2 Mo2 Mo2 135.4(4) . 7_546 ?
Br2 Mo2 Mo2 59.53(4) . 7_546 ?
Br2 Mo2 Mo2 59.27(4) 7_546 7_546 ?
Br3 Mo2 Mo2 119.35(6) 13_556 7_546 ?
Br1 Mo2 Mo2 119.23(6) . 7_546 ?
Mo2 Mo2 Mo2 90.000(1) 11_565 7_546 ?
C2 Mo2 Mo1 132.1(3) . 13_556 ?
Br2 Mo2 Mo1 119.55(5) . 13_556 ?
Br2 Mo2 Mo1 59.51(4) 7_546 13_556 ?
Br3 Mo2 Mo1 59.34(5) 13_556 13_556 ?
Br1 Mo2 Mo1 119.53(4) . 13_556 ?
Mo2 Mo2 Mo1 60.01(2) 11_565 13_556 ?
Mo2 Mo2 Mo1 60.02(4) 7_546 13_556 ?
C2 Mo2 Mo1 137.9(3) . . ?
Br2 Mo2 Mo1 59.59(4) . . ?
Br2 Mo2 Mo1 119.26(5) 7_546 . ?
Br3 Mo2 Mo1 119.49(4) 13_556 . ?
Br1 Mo2 Mo1 59.23(5) . . ?
Mo2 Mo2 Mo1 60.02(2) 11_565 . ?
Mo2 Mo2 Mo1 59.99(4) 7_546 . ?
Mo1 Mo2 Mo1 90.04(4) 13_556 . ?
Mo1 Br1 Mo2 61.14(4) . . ?
Mo1 Br1 Mo2 61.14(4) . 11_565 ?
Mo2 Br1 Mo2 60.96(5) . 11_565 ?
Mo2 Br2 Mo2 61.20(4) . 7_546 ?
Mo2 Br2 Mo1 61.18(4) . . ?
Mo2 Br2 Mo1 61.08(4) 7_546 . ?
Mo1 Br3 Mo2 61.14(4) . 7_546 ?
Mo1 Br3 Mo2 61.14(4) . 13_556 ?
Mo2 Br3 Mo2 61.05(5) 7_546 13_556 ?
N2 Mn1 N2 175.9(7) . 2_665 ?
N2 Mn1 N2 90.1(8) . 12_655 ?
N2 Mn1 N2 89.7(8) 2_665 12_655 ?
N2 Mn1 N2 89.7(8) . 11_575 ?
N2 Mn1 N2 90.1(8) 2_665 11_575 ?
N2 Mn1 N2 175.9(7) 12_655 11_575 ?
N2 Mn1 O2 92.1(4) . . ?
N2 Mn1 O2 92.1(4) 2_665 . ?
N2 Mn1 O2 92.1(4) 12_655 . ?
N2 Mn1 O2 92.1(4) 11_575 . ?
N2 Mn1 O1 87.9(4) . . ?
N2 Mn1 O1 87.9(4) 2_665 . ?
N2 Mn1 O1 87.9(4) 12_655 . ?
N2 Mn1 O1 87.9(4) 11_575 . ?
O2 Mn1 O1 180.0 . . ?
C2 N2 Mn1 165.2(13) . . ?
N1 C1 Mo1 177.1(17) . . ?
N2 C2 Mo2 172.8(12) . . ?

_refine_diff_density_max         2.309
_refine_diff_density_min         -2.091
_refine_diff_density_rms         0.329

####################################################################### 
# 
# 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_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1578316'
_audit_update_record             
;
2017-10-05 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Br8 Fe Mo6 N6 O2'
_chemical_formula_weight         1458.89

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'

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

_cell_length_a                   19.473(4)
_cell_length_b                   10.3173(17)
_cell_length_c                   13.749(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2762.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4815
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      27.53

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.508
_exptl_crystal_F_000             2608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    14.733
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4679
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5410
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.234
_diffrn_reflns_theta_max         27.547
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1761
_reflns_number_gt                1412
_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       'SAINT (Bruker, 2014); XPREP (Sheldrick, 2014)'
_computing_cell_refinement       'APEX2 (Bruker, 2014); SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014); XPREP (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1803P)²+2961.3667P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0006(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1761
_refine_ls_number_parameters     68
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1789
_refine_ls_R_factor_gt           0.1526
_refine_ls_wR_factor_ref         0.4529
_refine_ls_wR_factor_gt          0.4307
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_restrained_S_all      1.116
_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 0.2000(2) 0.250000 0.6350(3) 0.0103(10) Uani 1 2 d S T P . .
Mo2 Mo 0.30791(17) 0.3780(3) 0.7005(2) 0.0154(9) Uani 1 1 d . . . . .
Br1 Br 0.3140(3) 0.250000 0.5382(4) 0.0222(14) Uani 1 2 d S T P . .
Br2 Br 0.2016(2) 0.5000(4) 0.6365(3) 0.0216(11) Uani 1 1 d . . . . .
Br3 Br 0.0877(3) 0.250000 0.7332(4) 0.0217(14) Uani 1 2 d S T P . .
Fe Fe 0.500000 0.750000 0.6376(10) 0.021(3) Uani 1 4 d S T P . .
O2 O 0.500000 0.750000 0.790(6) 0.08(4) Uani 1 4 d S T P . .
O1 O 0.500000 0.750000 0.476(6) 0.04(2) Uani 1 4 d S T P . .
N2 N 0.421(2) 0.607(4) 0.631(3) 0.030(8) Uiso 1 1 d . . . . .
C1 C 0.139(2) 0.250000 0.503(4) 0.010(9) Uiso 1 2 d S . P . .
C2 C 0.380(2) 0.521(4) 0.648(3) 0.025(9) Uiso 1 1 d . . . . .
N1 N 0.106(4) 0.250000 0.432(5) 0.039(16) Uani 1 2 d S T 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
Mo1 C1 2.16(5) . ?
Mo1 Br3 2.571(7) . ?
Mo1 Br2 2.580(4) . ?
Mo1 Br2 2.580(4) 11_565 ?
Mo1 Br1 2.588(7) . ?
Mo1 Mo2 2.624(5) 7_546 ?
Mo1 Mo2 2.624(5) 13_556 ?
Mo1 Mo2 2.640(5) 11_565 ?
Mo1 Mo2 2.640(5) . ?
Mo2 C2 2.15(5) . ?
Mo2 Br2 2.577(6) 7_546 ?
Mo2 Br2 2.578(5) . ?
Mo2 Br3 2.591(6) 13_556 ?
Mo2 Br1 2.595(6) . ?
Mo2 Mo2 2.635(7) 7_546 ?
Mo2 Mo2 2.641(7) 11_565 ?
Fe O2 2.10(9) . ?
Fe N2 2.14(4) . ?
Fe N2 2.14(4) 2_665 ?
Fe N2 2.14(4) 12_655 ?
Fe N2 2.14(4) 11_575 ?
Fe O1 2.22(8) . ?
N2 C2 1.22(6) . ?
C1 N1 1.18(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Mo1 Br3 88.6(13) . . ?
C1 Mo1 Br2 90.76(15) . . ?
Br3 Mo1 Br2 90.33(14) . . ?
C1 Mo1 Br2 90.76(15) . 11_565 ?
Br3 Mo1 Br2 90.33(14) . 11_565 ?
Br2 Mo1 Br2 178.4(3) . 11_565 ?
C1 Mo1 Br1 92.2(13) . . ?
Br3 Mo1 Br1 179.3(3) . . ?
Br2 Mo1 Br1 89.66(14) . . ?
Br2 Mo1 Br1 89.66(14) 11_565 . ?
C1 Mo1 Mo2 133.6(9) . 7_546 ?
Br3 Mo1 Mo2 59.82(16) . 7_546 ?
Br2 Mo1 Mo2 59.36(14) . 7_546 ?
Br2 Mo1 Mo2 119.8(2) 11_565 7_546 ?
Br1 Mo1 Mo2 119.57(19) . 7_546 ?
C1 Mo1 Mo2 133.6(9) . 13_556 ?
Br3 Mo1 Mo2 59.82(16) . 13_556 ?
Br2 Mo1 Mo2 119.8(2) . 13_556 ?
Br2 Mo1 Mo2 59.36(14) 11_565 13_556 ?
Br1 Mo1 Mo2 119.57(19) . 13_556 ?
Mo2 Mo1 Mo2 60.44(18) 7_546 13_556 ?
C1 Mo1 Mo2 136.1(9) . 11_565 ?
Br3 Mo1 Mo2 119.9(2) . 11_565 ?
Br2 Mo1 Mo2 119.21(19) . 11_565 ?
Br2 Mo1 Mo2 59.18(13) 11_565 11_565 ?
Br1 Mo1 Mo2 59.51(15) . 11_565 ?
Mo2 Mo1 Mo2 90.26(17) 7_546 11_565 ?
Mo2 Mo1 Mo2 60.06(15) 13_556 11_565 ?
C1 Mo1 Mo2 136.1(9) . . ?
Br3 Mo1 Mo2 119.9(2) . . ?
Br2 Mo1 Mo2 59.18(13) . . ?
Br2 Mo1 Mo2 119.21(19) 11_565 . ?
Br1 Mo1 Mo2 59.51(15) . . ?
Mo2 Mo1 Mo2 60.06(15) 7_546 . ?
Mo2 Mo1 Mo2 90.26(17) 13_556 . ?
Mo2 Mo1 Mo2 60.03(18) 11_565 . ?
C2 Mo2 Br2 90.2(12) . 7_546 ?
C2 Mo2 Br2 94.2(12) . . ?
Br2 Mo2 Br2 90.0(2) 7_546 . ?
C2 Mo2 Br3 87.6(12) . 13_556 ?
Br2 Mo2 Br3 89.95(18) 7_546 13_556 ?
Br2 Mo2 Br3 178.27(19) . 13_556 ?
C2 Mo2 Br1 91.7(12) . . ?
Br2 Mo2 Br1 178.0(2) 7_546 . ?
Br2 Mo2 Br1 89.55(19) . . ?
Br3 Mo2 Br1 90.4(2) 13_556 . ?
C2 Mo2 Mo1 132.1(12) . 13_556 ?
Br2 Mo2 Mo1 59.47(13) 7_546 13_556 ?
Br2 Mo2 Mo1 119.51(19) . 13_556 ?
Br3 Mo2 Mo1 59.07(17) 13_556 13_556 ?
Br1 Mo2 Mo1 119.18(15) . 13_556 ?
C2 Mo2 Mo2 136.7(12) . 7_546 ?
Br2 Mo2 Mo2 59.28(14) 7_546 7_546 ?
Br2 Mo2 Mo2 59.25(15) . 7_546 ?
Br3 Mo2 Mo2 119.3(2) 13_556 7_546 ?
Br1 Mo2 Mo2 118.9(2) . 7_546 ?
Mo1 Mo2 Mo2 60.27(14) 13_556 7_546 ?
C2 Mo2 Mo1 138.1(12) . . ?
Br2 Mo2 Mo1 118.94(18) 7_546 . ?
Br2 Mo2 Mo1 59.25(13) . . ?
Br3 Mo2 Mo1 119.33(15) 13_556 . ?
Br1 Mo2 Mo1 59.25(17) . . ?
Mo1 Mo2 Mo1 89.74(17) 13_556 . ?
Mo2 Mo2 Mo1 59.67(15) 7_546 . ?
C2 Mo2 Mo2 133.1(12) . 11_565 ?
Br2 Mo2 Mo2 119.25(13) 7_546 11_565 ?
Br2 Mo2 Mo2 119.24(12) . 11_565 ?
Br3 Mo2 Mo2 59.35(9) 13_556 11_565 ?
Br1 Mo2 Mo2 59.41(10) . 11_565 ?
Mo1 Mo2 Mo2 59.78(9) 13_556 11_565 ?
Mo2 Mo2 Mo2 90.000(1) 7_546 11_565 ?
Mo1 Mo2 Mo2 59.98(9) . 11_565 ?
Mo1 Br1 Mo2 61.24(17) . . ?
Mo1 Br1 Mo2 61.24(17) . 11_565 ?
Mo2 Br1 Mo2 61.2(2) . 11_565 ?
Mo2 Br2 Mo2 61.47(16) 7_546 . ?
Mo2 Br2 Mo1 61.17(17) 7_546 . ?
Mo2 Br2 Mo1 61.57(15) . . ?
Mo1 Br3 Mo2 61.11(16) . 7_546 ?
Mo1 Br3 Mo2 61.11(16) . 13_556 ?
Mo2 Br3 Mo2 61.30(19) 7_546 13_556 ?
O2 Fe N2 92.2(12) . . ?
O2 Fe N2 92.3(12) . 2_665 ?
N2 Fe N2 176(2) . 2_665 ?
O2 Fe N2 92.3(12) . 12_655 ?
N2 Fe N2 92(2) . 12_655 ?
N2 Fe N2 88(2) 2_665 12_655 ?
O2 Fe N2 92.3(12) . 11_575 ?
N2 Fe N2 88(2) . 11_575 ?
N2 Fe N2 92(2) 2_665 11_575 ?
N2 Fe N2 175(2) 12_655 11_575 ?
O2 Fe O1 180.00(2) . . ?
N2 Fe O1 87.8(12) . . ?
N2 Fe O1 87.7(12) 2_665 . ?
N2 Fe O1 87.7(12) 12_655 . ?
N2 Fe O1 87.7(12) 11_575 . ?
C2 N2 Fe 166(4) . . ?
N1 C1 Mo1 180(5) . . ?
N2 C2 Mo2 171(4) . . ?

_refine_diff_density_max         7.217
_refine_diff_density_min         -6.091
_refine_diff_density_rms         1.040

####################################################################### 
# 
# 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_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1575380'
_audit_update_record             
;
2017-10-08 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Br6 Cd Mo6 N6 O4 S2'
_chemical_formula_weight         1451.74

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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      trigonal
_space_group_IT_number           152
_space_group_name_H-M_alt        'P 31 2 1'
_space_group_name_Hall           'P 31 2"'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'

_cell_length_a                   13.2013(6)
_cell_length_b                   13.2013(6)
_cell_length_c                   14.1296(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2132.5(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7038
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      27.47

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.391
_exptl_crystal_F_000             1956
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    11.896
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5470
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8908
_diffrn_reflns_av_unetI/netI     0.1229
_diffrn_reflns_av_R_equivalents  0.0869
_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       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.292
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3250
_reflns_number_gt                2338
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.999

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0357P)²+11.2059P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0005(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.38(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3250
_refine_ls_number_parameters     131
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_ref         0.1352
_refine_ls_wR_factor_gt          0.1273
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_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
Cd1 Cd 0.000000 0.61524(15) 0.666667 0.0300(5) Uani 1 2 d S T P . .
Mo4 Mo 0.27543(15) 0.43189(16) 0.53577(12) 0.0244(4) Uani 1 1 d . . . . .
Mo2 Mo 0.37626(16) 0.33206(17) 0.62653(11) 0.0290(4) Uani 1 1 d . . . . .
Mo3 Mo 0.21355(18) 0.21355(18) 0.500000 0.0291(6) Uani 1 2 d S T P . .
Mo1 Mo 0.49465(19) 0.49465(19) 0.500000 0.0335(7) Uani 1 2 d S T P . .
Br1 Br 0.4362(2) 0.5471(2) 0.65938(19) 0.0404(7) Uani 0.75 1 d . . P . .
S1 S 0.4362(2) 0.5471(2) 0.65938(19) 0.0404(7) Uani 0.25 1 d . . P . .
Br2 Br 0.1602(2) 0.2703(2) 0.66055(17) 0.0368(6) Uani 0.75 1 d . . P . .
S2 S 0.1602(2) 0.2703(2) 0.66055(17) 0.0368(6) Uani 0.25 1 d . . P . .
Br3 Br 0.1158(2) 0.3124(3) 0.41028(19) 0.0382(7) Uani 0.75 1 d . . P . .
S3 S 0.1158(2) 0.3124(3) 0.41028(19) 0.0382(7) Uani 0.25 1 d . . P . .
Br4 Br 0.3945(3) 0.5926(2) 0.4109(2) 0.0438(7) Uani 0.75 1 d . . P . .
S4 S 0.3945(3) 0.5926(2) 0.4109(2) 0.0438(7) Uani 0.25 1 d . . P . .
N4 N 0.1262(17) 0.5637(18) 0.6065(13) 0.045(5) Uani 1 1 d . . . . .
C4 C 0.180(2) 0.520(2) 0.5825(15) 0.045(6) Uani 1 1 d . . . . .
O2 O 0.3099(15) 0.850(2) 0.5028(11) 0.074(6) Uani 1 1 d . . . . .
C2 C -0.086(2) 0.595(3) 0.4421(15) 0.062(8) Uani 1 1 d . . . . .
O1 O 0.123(2) 0.8074(18) 0.613(2) 0.111(10) Uani 1 1 d . . . . .
N2 N -0.0914(19) 0.587(3) 0.5230(16) 0.083(8) Uani 1 1 d . . . . .
C1 C 0.658(8) 0.658(8) 0.500000 0.177(14) Uiso 1 2 d S . P . .
N1 N 0.748(6) 0.748(6) 0.500000 0.177(14) Uiso 1 2 d S . P . .
N3 N -0.022(5) -0.022(5) 0.500000 0.177(14) Uiso 1 2 d DS . P . .
C3 C 0.065(5) 0.065(5) 0.500000 0.177(14) Uiso 1 2 d DS . 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
Cd1 N4 2.256(17) 6_556 ?
Cd1 N4 2.256(17) . ?
Cd1 N2 2.30(2) . ?
Cd1 N2 2.30(2) 6_556 ?
Cd1 O1 2.35(2) 6_556 ?
Cd1 O1 2.35(2) . ?
Mo4 C4 2.20(2) . ?
Mo4 Br1 2.577(3) . ?
Mo4 Br2 2.594(3) . ?
Mo4 Br4 2.598(3) . ?
Mo4 Br3 2.598(3) . ?
Mo4 Mo3 2.622(2) . ?
Mo4 Mo2 2.628(2) 4_556 ?
Mo4 Mo2 2.628(2) . ?
Mo2 C2 2.16(2) 2_665 ?
Mo2 Br1 2.580(3) . ?
Mo2 Br2 2.589(3) . ?
Mo2 Br3 2.594(3) 4_556 ?
Mo2 Br4 2.600(3) 4_556 ?
Mo2 Mo1 2.625(2) . ?
Mo2 Mo3 2.626(2) . ?
Mo3 C3 1.96(7) . ?
Mo3 Br3 2.581(3) 4_556 ?
Mo3 Br3 2.581(3) . ?
Mo3 Br2 2.594(2) 4_556 ?
Mo3 Br2 2.594(2) . ?
Mo1 C1 2.15(10) . ?
Mo1 Br1 2.585(2) 4_556 ?
Mo1 Br1 2.585(2) . ?
Mo1 Br4 2.591(3) 4_556 ?
Mo1 Br4 2.591(3) . ?
N4 C4 1.16(3) . ?
C2 N2 1.15(3) . ?
C1 N1 1.19(10) . ?
N3 C3 1.148(14) . ?

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
N4 Cd1 N4 95.8(11) 6_556 . ?
N4 Cd1 N2 96.3(9) 6_556 . ?
N4 Cd1 N2 91.5(8) . . ?
N4 Cd1 N2 91.5(8) 6_556 6_556 ?
N4 Cd1 N2 96.3(9) . 6_556 ?
N2 Cd1 N2 168.2(17) . 6_556 ?
N4 Cd1 O1 89.4(8) 6_556 6_556 ?
N4 Cd1 O1 174.6(8) . 6_556 ?
N2 Cd1 O1 86.5(11) . 6_556 ?
N2 Cd1 O1 84.9(10) 6_556 6_556 ?
N4 Cd1 O1 174.6(8) 6_556 . ?
N4 Cd1 O1 89.4(8) . . ?
N2 Cd1 O1 84.9(10) . . ?
N2 Cd1 O1 86.5(11) 6_556 . ?
O1 Cd1 O1 85.4(12) 6_556 . ?
C4 Mo4 Br1 90.4(6) . . ?
C4 Mo4 Br2 88.6(6) . . ?
Br1 Mo4 Br2 89.76(10) . . ?
C4 Mo4 Br4 92.6(6) . . ?
Br1 Mo4 Br4 89.70(11) . . ?
Br2 Mo4 Br4 178.72(11) . . ?
C4 Mo4 Br3 91.1(6) . . ?
Br1 Mo4 Br3 178.51(10) . . ?
Br2 Mo4 Br3 90.02(10) . . ?
Br4 Mo4 Br3 90.48(10) . . ?
C4 Mo4 Mo3 133.8(7) . . ?
Br1 Mo4 Mo3 119.43(9) . . ?
Br2 Mo4 Mo3 59.65(7) . . ?
Br4 Mo4 Mo3 119.69(9) . . ?
Br3 Mo4 Mo3 59.25(7) . . ?
C4 Mo4 Mo2 136.7(6) . 4_556 ?
Br1 Mo4 Mo2 119.40(9) . 4_556 ?
Br2 Mo4 Mo2 119.68(9) . 4_556 ?
Br4 Mo4 Mo2 59.67(7) . 4_556 ?
Br3 Mo4 Mo2 59.51(8) . 4_556 ?
Mo3 Mo4 Mo2 60.03(5) . 4_556 ?
C4 Mo4 Mo2 133.4(6) . . ?
Br1 Mo4 Mo2 59.41(8) . . ?
Br2 Mo4 Mo2 59.45(7) . . ?
Br4 Mo4 Mo2 119.30(10) . . ?
Br3 Mo4 Mo2 119.27(10) . . ?
Mo3 Mo4 Mo2 60.02(6) . . ?
Mo2 Mo4 Mo2 89.97(7) 4_556 . ?
C2 Mo2 Br1 86.9(8) 2_665 . ?
C2 Mo2 Br2 90.3(8) 2_665 . ?
Br1 Mo2 Br2 89.80(9) . . ?
C2 Mo2 Br3 94.5(8) 2_665 4_556 ?
Br1 Mo2 Br3 178.43(11) . 4_556 ?
Br2 Mo2 Br3 89.43(10) . 4_556 ?
C2 Mo2 Br4 90.8(8) 2_665 4_556 ?
Br1 Mo2 Br4 90.20(10) . 4_556 ?
Br2 Mo2 Br4 178.95(11) . 4_556 ?
Br3 Mo2 Br4 90.54(9) 4_556 4_556 ?
C2 Mo2 Mo1 132.3(9) 2_665 . ?
Br1 Mo2 Mo1 59.54(7) . . ?
Br2 Mo2 Mo1 119.71(9) . . ?
Br3 Mo2 Mo1 119.77(8) 4_556 . ?
Br4 Mo2 Mo1 59.45(8) 4_556 . ?
C2 Mo2 Mo3 137.6(9) 2_665 . ?
Br1 Mo2 Mo3 119.18(9) . . ?
Br2 Mo2 Mo3 59.66(7) . . ?
Br3 Mo2 Mo3 59.25(7) 4_556 . ?
Br4 Mo2 Mo3 119.48(8) 4_556 . ?
Mo1 Mo2 Mo3 89.93(7) . . ?
C2 Mo2 Mo4 137.8(7) 2_665 4_556 ?
Br1 Mo2 Mo4 119.64(9) . 4_556 ?
Br2 Mo2 Mo4 119.54(9) . 4_556 ?
Br3 Mo2 Mo4 59.68(8) 4_556 4_556 ?
Br4 Mo2 Mo4 59.60(8) 4_556 4_556 ?
Mo1 Mo2 Mo4 60.10(5) . 4_556 ?
Mo3 Mo2 Mo4 59.88(5) . 4_556 ?
C2 Mo2 Mo4 132.1(7) 2_665 . ?
Br1 Mo2 Mo4 59.31(8) . . ?
Br2 Mo2 Mo4 59.61(7) . . ?
Br3 Mo2 Mo4 119.13(9) 4_556 . ?
Br4 Mo2 Mo4 119.54(10) 4_556 . ?
Mo1 Mo2 Mo4 60.10(5) . . ?
Mo3 Mo2 Mo4 59.88(5) . . ?
Mo4 Mo2 Mo4 90.03(7) 4_556 . ?
C3 Mo3 Br3 90.15(8) . 4_556 ?
C3 Mo3 Br3 90.15(8) . . ?
Br3 Mo3 Br3 179.70(17) 4_556 . ?
C3 Mo3 Br2 90.50(8) . 4_556 ?
Br3 Mo3 Br2 90.39(8) 4_556 4_556 ?
Br3 Mo3 Br2 89.60(8) . 4_556 ?
C3 Mo3 Br2 90.51(8) . . ?
Br3 Mo3 Br2 89.60(8) 4_556 . ?
Br3 Mo3 Br2 90.40(8) . . ?
Br2 Mo3 Br2 178.99(16) 4_556 . ?
C3 Mo3 Mo4 134.86(5) . . ?
Br3 Mo3 Mo4 119.85(9) 4_556 . ?
Br3 Mo3 Mo4 59.91(7) . . ?
Br2 Mo3 Mo4 119.55(9) 4_556 . ?
Br2 Mo3 Mo4 59.62(7) . . ?
C3 Mo3 Mo4 134.86(5) . 4_556 ?
Br3 Mo3 Mo4 59.91(7) 4_556 4_556 ?
Br3 Mo3 Mo4 119.85(9) . 4_556 ?
Br2 Mo3 Mo4 59.62(7) 4_556 4_556 ?
Br2 Mo3 Mo4 119.55(9) . 4_556 ?
Mo4 Mo3 Mo4 90.28(9) . 4_556 ?
C3 Mo3 Mo2 134.97(5) . . ?
Br3 Mo3 Mo2 59.75(8) 4_556 . ?
Br3 Mo3 Mo2 120.01(9) . . ?
Br2 Mo3 Mo2 119.71(9) 4_556 . ?
Br2 Mo3 Mo2 59.46(7) . . ?
Mo4 Mo3 Mo2 60.10(6) . . ?
Mo4 Mo3 Mo2 60.09(6) 4_556 . ?
C3 Mo3 Mo2 134.98(5) . 4_556 ?
Br3 Mo3 Mo2 120.01(9) 4_556 4_556 ?
Br3 Mo3 Mo2 59.75(8) . 4_556 ?
Br2 Mo3 Mo2 59.46(7) 4_556 4_556 ?
Br2 Mo3 Mo2 119.71(9) . 4_556 ?
Mo4 Mo3 Mo2 60.09(6) . 4_556 ?
Mo4 Mo3 Mo2 60.10(6) 4_556 4_556 ?
Mo2 Mo3 Mo2 90.05(10) . 4_556 ?
C1 Mo1 Br1 90.88(8) . 4_556 ?
C1 Mo1 Br1 90.88(8) . . ?
Br1 Mo1 Br1 178.25(16) 4_556 . ?
C1 Mo1 Br4 90.32(8) . 4_556 ?
Br1 Mo1 Br4 89.70(9) 4_556 4_556 ?
Br1 Mo1 Br4 90.29(9) . 4_556 ?
C1 Mo1 Br4 90.32(8) . . ?
Br1 Mo1 Br4 90.29(9) 4_556 . ?
Br1 Mo1 Br4 89.70(9) . . ?
Br4 Mo1 Br4 179.37(17) 4_556 . ?
C1 Mo1 Mo2 134.95(5) . 4_556 ?
Br1 Mo1 Mo2 59.35(7) 4_556 4_556 ?
Br1 Mo1 Mo2 119.22(9) . 4_556 ?
Br4 Mo1 Mo2 119.69(9) 4_556 4_556 ?
Br4 Mo1 Mo2 59.79(7) . 4_556 ?
C1 Mo1 Mo2 134.95(5) . . ?
Br1 Mo1 Mo2 119.22(9) 4_556 . ?
Br1 Mo1 Mo2 59.35(7) . . ?
Br4 Mo1 Mo2 59.79(7) 4_556 . ?
Br4 Mo1 Mo2 119.69(9) . . ?
Mo2 Mo1 Mo2 90.10(10) 4_556 . ?
C1 Mo1 Mo4 135.04(5) . . ?
Br1 Mo1 Mo4 119.35(9) 4_556 . ?
Br1 Mo1 Mo4 59.22(7) . . ?
Br4 Mo1 Mo4 119.80(10) 4_556 . ?
Br4 Mo1 Mo4 59.68(7) . . ?
Mo2 Mo1 Mo4 60.00(6) 4_556 . ?
Mo2 Mo1 Mo4 60.01(6) . . ?
C1 Mo1 Mo4 135.04(5) . 4_556 ?
Br1 Mo1 Mo4 59.22(7) 4_556 4_556 ?
Br1 Mo1 Mo4 119.35(9) . 4_556 ?
Br4 Mo1 Mo4 59.68(7) 4_556 4_556 ?
Br4 Mo1 Mo4 119.80(10) . 4_556 ?
Mo2 Mo1 Mo4 60.01(6) 4_556 4_556 ?
Mo2 Mo1 Mo4 60.00(6) . 4_556 ?
Mo4 Mo1 Mo4 89.92(10) . 4_556 ?
Mo4 Br1 Mo2 61.28(7) . . ?
Mo4 Br1 Mo1 61.28(8) . . ?
Mo2 Br1 Mo1 61.11(7) . . ?
Mo2 Br2 Mo4 60.94(7) . . ?
Mo2 Br2 Mo3 60.88(7) . . ?
Mo4 Br2 Mo3 60.72(7) . . ?
Mo3 Br3 Mo2 61.00(8) . 4_556 ?
Mo3 Br3 Mo4 60.84(8) . . ?
Mo2 Br3 Mo4 60.81(7) 4_556 . ?
Mo1 Br4 Mo4 60.92(8) . . ?
Mo1 Br4 Mo2 60.76(8) . 4_556 ?
Mo4 Br4 Mo2 60.73(7) . 4_556 ?
C4 N4 Cd1 169(2) . . ?
N4 C4 Mo4 178(2) . . ?
N2 C2 Mo2 170(2) . 3_564 ?
C2 N2 Cd1 150(2) . . ?
N1 C1 Mo1 180(7) . . ?
N3 C3 Mo3 180.0 . . ?

_refine_diff_density_max         1.560
_refine_diff_density_min         -1.676
_refine_diff_density_rms         0.263

####################################################################### 
# 
# 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_CCDC5
_database_code_depnum_ccdc_archive 'CCDC 1575379'
_audit_update_record             
;
2017-10-28 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 Br6 Cs0.82 Mn Mo6 N6 O2 Se2'
_chemical_formula_weight         1564.73

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'

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

_cell_length_a                   19.6163(10)
_cell_length_b                   10.2909(7)
_cell_length_c                   13.8615(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2798.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2045
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.714
_exptl_crystal_F_000             2776
_exptl_transmission_factor_min   0.5413
_exptl_transmission_factor_max   0.7456
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    15.272
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5413
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
'Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector_area_resol_mean 'CCD plate'
_diffrn_reflns_number            4299
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.465
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1742
_reflns_number_gt                1274
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0290P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1742
_refine_ls_number_parameters     85
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0702
_refine_ls_wR_factor_gt          0.0648
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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 0.30167(3) 0.750000 0.63643(5) 0.01702(16) Uani 1 2 d S T P . .
Mo2 Mo 0.30704(2) 0.62183(5) 0.80109(3) 0.01804(13) Uani 1 1 d . . . . .
Br1 Br 0.41143(3) 0.750000 0.73925(6) 0.0289(2) Uani 0.75 2 d S T P . .
Se1 Se 0.41143(3) 0.750000 0.73925(6) 0.0289(2) Uani 0.25 2 d S T P . .
Br2 Br 0.29971(3) 0.49657(6) 0.63816(5) 0.02877(17) Uani 0.75 1 d . . P . .
Se2 Se 0.29971(3) 0.49657(6) 0.63816(5) 0.02877(17) Uani 0.25 1 d . . P . .
Br3 Br 0.18944(4) 0.750000 0.53715(6) 0.0278(2) Uani 0.75 2 d S T P . .
Se3 Se 0.18944(4) 0.750000 0.53715(6) 0.0278(2) Uani 0.25 2 d S T P . .
C1 C 0.3676(4) 0.750000 0.5089(6) 0.032(2) Uani 1 2 d S T P . .
C2 C 0.3785(3) 0.4738(6) 0.8543(5) 0.0354(16) Uani 1 1 d . . . . .
N2 N 0.4208(2) 0.3998(5) 0.8740(4) 0.0436(15) Uani 1 1 d . . . . .
N1 N 0.4070(4) 0.750000 0.4459(6) 0.054(2) Uani 1 2 d S T P . .
Mn1 Mn 0.500000 0.250000 0.87469(12) 0.0183(4) Uani 1 4 d S T P . .
O1 O 0.500000 0.250000 0.7114(6) 0.062(3) Uani 1 4 d S T P . .
O2 O 0.500000 0.250000 1.0349(6) 0.094(5) Uani 1 4 d S T P . .
Cs1 Cs 0.500000 1.0104(2) 0.43955(19) 0.0879(8) Uani 0.4078 2 d S T 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
Mo1 C1 2.191(8) . ?
Mo1 Br1 2.5819(9) . ?
Mo1 Br3 2.5962(9) . ?
Mo1 Br2 2.6084(6) 11_575 ?
Mo1 Br2 2.6084(6) . ?
Mo1 Mo2 2.6382(7) . ?
Mo1 Mo2 2.6382(7) 11_575 ?
Mo1 Mo2 2.6528(6) 7_546 ?
Mo1 Mo2 2.6528(6) 13_566 ?
Mo2 C2 2.198(6) . ?
Mo2 Br1 2.5822(7) . ?
Mo2 Br2 2.5991(7) 7_546 ?
Mo2 Br3 2.6023(9) 13_566 ?
Mo2 Br2 2.6043(8) . ?
Mo2 Mo2 2.6380(10) 11_575 ?
Mo2 Mo2 2.6483(8) 7_546 ?
Br1 Cs1 3.904(2) 10_556 ?
Br1 Cs1 3.904(2) 9_676 ?
Br2 Cs1 4.0764(9) 10_556 ?
C1 N1 1.166(10) . ?
C1 Cs1 3.652(6) 9_676 ?
C1 Cs1 3.652(6) 10_556 ?
C1 Cs1 3.853(5) . ?
C1 Cs1 3.853(5) 2_665 ?
C2 N2 1.159(7) . ?
N2 Mn1 2.188(5) . ?
N1 Cs1 3.243(5) . ?
N1 Cs1 3.243(5) 2_665 ?
N1 Cs1 3.454(6) 9_676 ?
N1 Cs1 3.454(6) 10_556 ?
Mn1 O2 2.221(9) . ?
Mn1 O1 2.263(9) . ?
O1 Cs1 3.400(6) 9_666 ?
O1 Cs1 3.400(6) 10_556 ?
Cs1 Cs1 1.689(5) 9_676 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Mo1 Br1 87.3(2) . . ?
C1 Mo1 Br3 94.2(2) . . ?
Br1 Mo1 Br3 178.51(4) . . ?
C1 Mo1 Br2 90.923(18) . 11_575 ?
Br1 Mo1 Br2 90.414(17) . 11_575 ?
Br3 Mo1 Br2 89.562(17) . 11_575 ?
C1 Mo1 Br2 90.924(18) . . ?
Br1 Mo1 Br2 90.414(17) . . ?
Br3 Mo1 Br2 89.563(17) . . ?
Br2 Mo1 Br2 178.01(3) 11_575 . ?
C1 Mo1 Mo2 132.42(15) . . ?
Br1 Mo1 Mo2 59.28(2) . . ?
Br3 Mo1 Mo2 119.50(3) . . ?
Br2 Mo1 Mo2 119.51(3) 11_575 . ?
Br2 Mo1 Mo2 59.519(19) . . ?
C1 Mo1 Mo2 132.42(15) . 11_575 ?
Br1 Mo1 Mo2 59.28(2) . 11_575 ?
Br3 Mo1 Mo2 119.50(3) . 11_575 ?
Br2 Mo1 Mo2 59.519(19) 11_575 11_575 ?
Br2 Mo1 Mo2 119.51(3) . 11_575 ?
Mo2 Mo1 Mo2 60.00(3) . 11_575 ?
C1 Mo1 Mo2 137.57(14) . 7_546 ?
Br1 Mo1 Mo2 119.35(3) . 7_546 ?
Br3 Mo1 Mo2 59.43(2) . 7_546 ?
Br2 Mo1 Mo2 118.84(2) 11_575 7_546 ?
Br2 Mo1 Mo2 59.203(17) . 7_546 ?
Mo2 Mo1 Mo2 60.07(2) . 7_546 ?
Mo2 Mo1 Mo2 89.90(2) 11_575 7_546 ?
C1 Mo1 Mo2 137.57(14) . 13_566 ?
Br1 Mo1 Mo2 119.35(3) . 13_566 ?
Br3 Mo1 Mo2 59.43(2) . 13_566 ?
Br2 Mo1 Mo2 59.203(17) 11_575 13_566 ?
Br2 Mo1 Mo2 118.84(2) . 13_566 ?
Mo2 Mo1 Mo2 89.90(2) . 13_566 ?
Mo2 Mo1 Mo2 60.07(2) 11_575 13_566 ?
Mo2 Mo1 Mo2 59.63(2) 7_546 13_566 ?
C2 Mo2 Br1 87.70(15) . . ?
C2 Mo2 Br2 93.51(15) . 7_546 ?
Br1 Mo2 Br2 178.79(3) . 7_546 ?
C2 Mo2 Br3 92.59(17) . 13_566 ?
Br1 Mo2 Br3 90.35(3) . 13_566 ?
Br2 Mo2 Br3 89.63(2) 7_546 13_566 ?
C2 Mo2 Br2 89.04(17) . . ?
Br1 Mo2 Br2 90.50(2) . . ?
Br2 Mo2 Br2 89.49(3) 7_546 . ?
Br3 Mo2 Br2 178.19(3) 13_566 . ?
C2 Mo2 Mo2 133.89(17) . 11_575 ?
Br1 Mo2 Mo2 59.282(13) . 11_575 ?
Br2 Mo2 Mo2 119.731(17) 7_546 11_575 ?
Br3 Mo2 Mo2 59.546(14) 13_566 11_575 ?
Br2 Mo2 Mo2 119.666(18) . 11_575 ?
C2 Mo2 Mo1 131.49(16) . . ?
Br1 Mo2 Mo1 59.27(2) . . ?
Br2 Mo2 Mo1 119.74(2) 7_546 . ?
Br3 Mo2 Mo1 119.54(2) 13_566 . ?
Br2 Mo2 Mo1 59.671(19) . . ?
Mo2 Mo2 Mo1 60.002(13) 11_575 . ?
C2 Mo2 Mo2 135.92(17) . 7_546 ?
Br1 Mo2 Mo2 119.51(3) . 7_546 ?
Br2 Mo2 Mo2 59.50(2) 7_546 7_546 ?
Br3 Mo2 Mo2 118.90(3) 13_566 7_546 ?
Br2 Mo2 Mo2 59.309(19) . 7_546 ?
Mo2 Mo2 Mo2 90.0 11_575 7_546 ?
Mo1 Mo2 Mo2 60.239(19) . 7_546 ?
C2 Mo2 Mo1 138.39(16) . 13_566 ?
Br1 Mo2 Mo1 119.46(2) . 13_566 ?
Br2 Mo2 Mo1 59.547(18) 7_546 13_566 ?
Br3 Mo2 Mo1 59.20(2) 13_566 13_566 ?
Br2 Mo2 Mo1 119.00(2) . 13_566 ?
Mo2 Mo2 Mo1 60.184(12) 11_575 13_566 ?
Mo1 Mo2 Mo1 90.10(2) . 13_566 ?
Mo2 Mo2 Mo1 59.692(19) 7_546 13_566 ?
Mo1 Br1 Mo2 61.44(2) . . ?
Mo1 Br1 Mo2 61.44(2) . 11_575 ?
Mo2 Br1 Mo2 61.44(3) . 11_575 ?
Mo1 Br1 Cs1 91.19(3) . 10_556 ?
Mo2 Br1 Cs1 103.95(3) . 10_556 ?
Mo2 Br1 Cs1 152.41(3) 11_575 10_556 ?
Mo1 Br1 Cs1 91.19(3) . 9_676 ?
Mo2 Br1 Cs1 152.41(3) . 9_676 ?
Mo2 Br1 Cs1 103.95(3) 11_575 9_676 ?
Cs1 Br1 Cs1 78.34(6) 10_556 9_676 ?
Mo2 Br2 Mo2 61.19(2) 7_546 . ?
Mo2 Br2 Mo1 61.25(2) 7_546 . ?
Mo2 Br2 Mo1 60.81(2) . . ?
Mo2 Br2 Cs1 147.65(4) 7_546 10_556 ?
Mo2 Br2 Cs1 99.13(4) . 10_556 ?
Mo1 Br2 Cs1 87.05(3) . 10_556 ?
Mo1 Br3 Mo2 61.37(2) . 13_566 ?
Mo1 Br3 Mo2 61.37(2) . 7_546 ?
Mo2 Br3 Mo2 60.91(3) 13_566 7_546 ?
N1 C1 Mo1 174.7(7) . . ?
N1 C1 Cs1 71.1(4) . 9_676 ?
Mo1 C1 Cs1 105.2(2) . 9_676 ?
N1 C1 Cs1 71.1(4) . 10_556 ?
Mo1 C1 Cs1 105.2(2) . 10_556 ?
Cs1 C1 Cs1 84.95(16) 9_676 10_556 ?
N1 C1 Cs1 50.7(2) . . ?
Mo1 C1 Cs1 126.82(18) . . ?
Cs1 C1 Cs1 25.84(9) 9_676 . ?
Cs1 C1 Cs1 92.24(16) 10_556 . ?
N1 C1 Cs1 50.7(2) . 2_665 ?
Mo1 C1 Cs1 126.82(18) . 2_665 ?
Cs1 C1 Cs1 92.24(16) 9_676 2_665 ?
Cs1 C1 Cs1 25.84(9) 10_556 2_665 ?
Cs1 C1 Cs1 88.12(16) . 2_665 ?
N2 C2 Mo2 172.4(5) . . ?
C2 N2 Mn1 166.4(6) . . ?
C1 N1 Cs1 113.1(3) . . ?
C1 N1 Cs1 113.1(3) . 2_665 ?
Cs1 N1 Cs1 111.4(2) . 2_665 ?
C1 N1 Cs1 90.3(4) . 9_676 ?
Cs1 N1 Cs1 29.00(10) . 9_676 ?
Cs1 N1 Cs1 107.8(2) 2_665 9_676 ?
C1 N1 Cs1 90.3(4) . 10_556 ?
Cs1 N1 Cs1 107.8(2) . 10_556 ?
Cs1 N1 Cs1 29.00(10) 2_665 10_556 ?
Cs1 N1 Cs1 91.1(2) 9_676 10_556 ?
N2 Mn1 N2 90.4(3) . 12_655 ?
N2 Mn1 N2 89.6(3) . 11_565 ?
N2 Mn1 N2 179.5(3) 12_655 11_565 ?
N2 Mn1 N2 179.5(3) . 2_655 ?
N2 Mn1 N2 89.6(3) 12_655 2_655 ?
N2 Mn1 N2 90.4(3) 11_565 2_655 ?
N2 Mn1 O2 90.24(16) . . ?
N2 Mn1 O2 90.24(16) 12_655 . ?
N2 Mn1 O2 90.24(16) 11_565 . ?
N2 Mn1 O2 90.24(16) 2_655 . ?
N2 Mn1 O1 89.76(16) . . ?
N2 Mn1 O1 89.76(16) 12_655 . ?
N2 Mn1 O1 89.76(16) 11_565 . ?
N2 Mn1 O1 89.76(16) 2_655 . ?
O2 Mn1 O1 180.0 . . ?
Mn1 O1 Cs1 127.99(13) . 9_666 ?
Mn1 O1 Cs1 127.99(13) . 10_556 ?
Cs1 O1 Cs1 104.0(3) 9_666 10_556 ?
Cs1 Cs1 N1 82.45(19) 9_676 . ?
Cs1 Cs1 N1 82.45(19) 9_676 2_665 ?
N1 Cs1 N1 68.5(2) . 2_665 ?
Cs1 Cs1 O1 120.7(2) 9_676 9_666 ?
N1 Cs1 O1 50.62(16) . 9_666 ?
N1 Cs1 O1 50.62(16) 2_665 9_666 ?
Cs1 Cs1 N1 68.55(17) 9_676 9_676 ?
N1 Cs1 N1 151.00(10) . 9_676 ?
N1 Cs1 N1 106.3(2) 2_665 9_676 ?
O1 Cs1 N1 147.73(12) 9_666 9_676 ?
Cs1 Cs1 N1 68.55(17) 9_676 10_566 ?
N1 Cs1 N1 106.3(2) . 10_566 ?
N1 Cs1 N1 151.00(10) 2_665 10_566 ?
O1 Cs1 N1 147.73(12) 9_666 10_566 ?
N1 Cs1 N1 63.8(2) 9_676 10_566 ?
Cs1 Cs1 C1 83.76(17) 9_676 9_676 ?
N1 Cs1 C1 162.32(19) . 9_676 ?
N1 Cs1 C1 98.77(15) 2_665 9_676 ?
O1 Cs1 C1 130.74(12) 9_666 9_676 ?
N1 Cs1 C1 18.61(16) 9_676 9_676 ?
N1 Cs1 C1 78.68(16) 10_566 9_676 ?
Cs1 Cs1 C1 83.76(17) 9_676 10_566 ?
N1 Cs1 C1 98.77(15) . 10_566 ?
N1 Cs1 C1 162.32(19) 2_665 10_566 ?
O1 Cs1 C1 130.74(12) 9_666 10_566 ?
N1 Cs1 C1 78.68(16) 9_676 10_566 ?
N1 Cs1 C1 18.61(16) 10_566 10_566 ?
C1 Cs1 C1 90.65(17) 9_676 10_566 ?
Cs1 Cs1 C1 70.40(16) 9_676 2_665 ?
N1 Cs1 C1 78.34(16) . 2_665 ?
N1 Cs1 C1 16.15(15) 2_665 2_665 ?
O1 Cs1 C1 66.76(14) 9_666 2_665 ?
N1 Cs1 C1 91.47(14) 9_676 2_665 ?
N1 Cs1 C1 137.54(18) 10_566 2_665 ?
C1 Cs1 C1 86.65(15) 9_676 2_665 ?
C1 Cs1 C1 154.16(9) 10_566 2_665 ?
Cs1 Cs1 C1 70.40(16) 9_676 . ?
N1 Cs1 C1 16.15(15) . . ?
N1 Cs1 C1 78.34(16) 2_665 . ?
O1 Cs1 C1 66.76(14) 9_666 . ?
N1 Cs1 C1 137.54(18) 9_676 . ?
N1 Cs1 C1 91.47(14) 10_566 . ?
C1 Cs1 C1 154.16(9) 9_676 . ?
C1 Cs1 C1 86.65(15) 10_566 . ?
C1 Cs1 C1 84.74(17) 2_665 . ?
Cs1 Cs1 Br1 135.20(13) 9_676 10_566 ?
N1 Cs1 Br1 106.78(14) . 10_566 ?
N1 Cs1 Br1 142.14(17) 2_665 10_566 ?
O1 Cs1 Br1 96.15(12) 9_666 10_566 ?
N1 Cs1 Br1 94.36(11) 9_676 10_566 ?
N1 Cs1 Br1 66.79(12) 10_566 10_566 ?
C1 Cs1 Br1 90.81(11) 9_676 10_566 ?
C1 Cs1 Br1 51.78(13) 10_566 10_566 ?
C1 Cs1 Br1 153.83(14) 2_665 10_566 ?
C1 Cs1 Br1 107.32(11) . 10_566 ?
Cs1 Cs1 Br1 135.20(13) 9_676 9_676 ?
N1 Cs1 Br1 142.14(17) . 9_676 ?
N1 Cs1 Br1 106.78(14) 2_665 9_676 ?
O1 Cs1 Br1 96.15(12) 9_666 9_676 ?
N1 Cs1 Br1 66.79(12) 9_676 9_676 ?
N1 Cs1 Br1 94.36(11) 10_566 9_676 ?
C1 Cs1 Br1 51.78(13) 9_676 9_676 ?
C1 Cs1 Br1 90.81(11) 10_566 9_676 ?
C1 Cs1 Br1 107.32(11) 2_665 9_676 ?
C1 Cs1 Br1 153.83(14) . 9_676 ?
Br1 Cs1 Br1 52.85(4) 10_566 9_676 ?

_refine_diff_density_max         1.697
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.189

