#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:35:30 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228887 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/07/7230700.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_7230700
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 Cs0.82 Mn Mo6 N6 O2 Se2'
_chemical_formula_weight         1564.73
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_space_group_name_H-M   'I m m a'
_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                90
_cell_formula_units_Z            4
_cell_length_a                   19.6163(10)
_cell_length_b                   10.2909(7)
_cell_length_c                   13.8615(8)
_cell_measurement_reflns_used    2045
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.46
_cell_volume                     2798.2(3)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4299
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_min         2.465
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    15.272
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.714
_exptl_crystal_description       prism
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.5413
_refine_diff_density_max         1.697
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0300
_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)+(0.0290P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1274
_reflns_number_total             1742
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00113h2.cif
_cod_data_source_block           shelx_CCDC5
_cod_depositor_comments
'Adding full bibliography for 7230695--7230700.cif.'
_cod_database_code               7230700
_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'
'-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'
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
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
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'
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
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
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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
