#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:35:30 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228887 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/06/7230695.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7230695
loop_
_publ_author_name
'Daigre, Gilles'
'Lemoine, Pierric'
'Pham, Thi Diep'
'Demange, Valérie'
'Gautier, Régis'
'Naumov, Nikolay G.'
'Ledneva, Alexandra'
'Amela-Cortes, Maria'
'Dumait, Noée'
'Audebrand, Nathalie'
'Cordier, Stéphane'
_publ_section_title
;
 Low dimensional solids based on Mo6 cluster cyanides and Mn2+, Mn3+ or
 Cd2+ metal ions: crystal chemistry, magnetic and optical properties
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              3396
_journal_paper_doi               10.1039/C8CE00113H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C6 Br6 Cd Mo6 N6 O4 Se2'
_chemical_formula_weight         1545.54
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-10-28 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.2807(5)
_cell_length_b                   13.2807(5)
_cell_length_c                   14.1753(6)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.28
_cell_volume                     2165.23(15)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8186
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.521
_diffrn_reflns_theta_min         2.280
_diffrn_source                   'Incoatec microfocus sealed tube'
_exptl_absorpt_coefficient_mu    14.093
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.556
_exptl_crystal_description       prism
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.773
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.238
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.27(3)
_refine_ls_extinction_coef       0.0024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         3283
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0001P)²+46.5696P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2963
_reflns_number_total             3283
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00113h2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7230695--7230700.cif.'
_cod_original_cell_volume        2165.23(19)
_cod_database_code               7230695
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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'
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
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
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'
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
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) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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) .
