#------------------------------------------------------------------------------
#$Date: 2018-06-13 15:16:51 +0300 (Wed, 13 Jun 2018) $
#$Revision: 208321 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/08/7230866.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_7230866
loop_
_publ_author_name
'Muravieva, Viktoria K.'
'Gayfulin, Yakov M.'
'Lemoine, Pierric'
'Cordier, stéphane'
'Naumov, Nikolay G.'
_publ_section_title
;
 Stabilization of interpenetrating cluster-based frameworks promoted by
 N-H…X hydrogen bonds: synthesis, structures and properties of
 {[Cd(NH3)4]3[Re3Mo3Se8(CN)6]}X (X = Cl, Br and I)
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C8CE00527C
_journal_year                    2018
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C6 H36 Br Cd3 Mo3 N18 Re3 Se8'
_chemical_formula_sum            'C6 H36 Br Cd3 Mo3 N18 Re3 Se8'
_chemical_formula_weight         2255.74
_chemical_name_systematic        {[Cd(NH3)4]3[Re3Mo3Se8(CN)6]}Br
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2018-02-20 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   15.2258(10)
_cell_length_b                   15.2258(10)
_cell_length_c                   15.3834(11)
_cell_measurement_reflns_used    8736
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.68
_cell_measurement_wavelength     0.71073
_cell_volume                     3088.5(4)
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2017)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14709
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.066
_exptl_absorpt_coefficient_mu    19.249
_exptl_absorpt_correction_T_max  0.177
_exptl_absorpt_correction_T_min  0.123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    3.638
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3000
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: aqueous ammonia'
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.000168(11)
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0148
_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)+(0.0085P)²+15.3152P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0340
_refine_ls_wR_factor_ref         0.0349
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1440
_reflns_number_total             1571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00527c2.cif
_cod_data_source_block           PLM34
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        3088.5(5)
_cod_database_code               7230866
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Mo1 Mo 0.03186(2) 0.11268(2) 0.07020(2) 0.01010(6) Uani 0.5 1 d . . P
Re1 Re 0.03186(2) 0.11268(2) 0.07020(2) 0.01010(6) Uani 0.5 1 d . . P
Se1 Se 0.0000 0.0000 0.20303(3) 0.01339(10) Uani 1 3 d S T P
Se2 Se 0.21634(2) 0.15514(2) 0.06796(2) 0.01406(7) Uani 1 1 d . . .
C1 C 0.0710(2) 0.2449(2) 0.14772(18) 0.0173(6) Uani 1 1 d . . .
N1 N 0.0948(2) 0.3156(2) 0.18978(18) 0.0267(6) Uani 1 1 d . . .
Cd1 Cd 0.1667 0.3333 0.3333 0.01921(8) Uani 1 2 d S . P
N2 N 0.0137(2) 0.1952(2) 0.3738(2) 0.0355(7) Uani 1 1 d . . .
H2A H 0.0243 0.1468 0.3946 0.053 Uiso 1 1 calc R U .
H2B H -0.0271 0.1718 0.3278 0.053 Uiso 1 1 calc R U .
H2C H -0.0151 0.2139 0.4147 0.053 Uiso 1 1 calc R U .
N3 N 0.0965(3) 0.4356(3) 0.3675(2) 0.0411(8) Uani 1 1 d . . .
H3A H 0.1446 0.4944 0.3892 0.062 Uiso 1 1 calc R U .
H3B H 0.0475 0.4043 0.4067 0.062 Uiso 1 1 calc R U .
H3C H 0.0709 0.4470 0.3197 0.062 Uiso 1 1 calc R U .
Br1 Br 0.0000 0.0000 0.5000 0.0476(3) Uani 1 6 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'
N N 0.0061 0.0033 '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'
Br Br -0.2901 2.4595 '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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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 Se2 92.26(8) . 2
C1 Mo1 Se2 90.90(8) . .
Se2 Mo1 Se2 176.835(10) 2 .
C1 Mo1 Se2 90.11(8) . 12
Se2 Mo1 Se2 90.122(7) 2 12
Se2 Mo1 Se2 90.108(7) . 12
C1 Mo1 Se1 93.20(8) . .
Se2 Mo1 Se1 89.800(7) 2 .
Se2 Mo1 Se1 89.787(7) . .
Se2 Mo1 Se1 176.686(10) 12 .
C1 Mo1 Re1 134.33(8) . 12
Se2 Mo1 Re1 58.754(7) 2 12
Se2 Mo1 Re1 118.861(9) . 12
Se2 Mo1 Re1 58.673(9) 12 12
Se1 Mo1 Re1 118.631(8) . 12
C1 Mo1 Mo1 134.33(8) . 12
Se2 Mo1 Mo1 58.754(7) 2 12
Se2 Mo1 Mo1 118.861(9) . 12
Se2 Mo1 Mo1 58.673(9) 12 12
Se1 Mo1 Mo1 118.631(8) . 12
Re1 Mo1 Mo1 0.0 12 12
C1 Mo1 Mo1 133.37(8) . 11
Se2 Mo1 Mo1 118.871(9) 2 11
Se2 Mo1 Mo1 58.744(7) . 11
Se2 Mo1 Mo1 58.658(10) 12 11
Se1 Mo1 Mo1 118.631(8) . 11
Re1 Mo1 Mo1 60.1 12 11
Mo1 Mo1 Mo1 60.128(9) 12 11
C1 Mo1 Re1 133.37(8) . 11
Se2 Mo1 Re1 118.871(9) 2 11
Se2 Mo1 Re1 58.744(7) . 11
Se2 Mo1 Re1 58.658(10) 12 11
Se1 Mo1 Re1 118.631(8) . 11
Re1 Mo1 Re1 60.128(9) 12 11
Mo1 Mo1 Re1 60.128(9) 12 11
Mo1 Mo1 Re1 0.000(7) 11 11
C1 Mo1 Mo1 135.63(8) . 3
Se2 Mo1 Mo1 118.629(9) 2 3
Se2 Mo1 Mo1 58.613(9) . 3
Se2 Mo1 Mo1 118.583(8) 12 3
Se1 Mo1 Mo1 58.703(6) . 3
Re1 Mo1 Mo1 90.0 12 3
Mo1 Mo1 Mo1 90.0 12 3
Mo1 Mo1 Mo1 59.936(4) 11 3
Re1 Mo1 Mo1 59.9 11 3
C1 Mo1 Re1 135.63(8) . 3
Se2 Mo1 Re1 118.629(9) 2 3
Se2 Mo1 Re1 58.613(9) . 3
Se2 Mo1 Re1 118.583(8) 12 3
Se1 Mo1 Re1 58.703(6) . 3
Re1 Mo1 Re1 90.0 12 3
Mo1 Mo1 Re1 90.0 12 3
Mo1 Mo1 Re1 59.936(4) 11 3
Re1 Mo1 Re1 59.936(4) 11 3
Mo1 Mo1 Re1 0.000(7) 3 3
C1 Mo1 Mo1 136.62(8) . 2
Se2 Mo1 Mo1 58.634(9) 2 2
Se2 Mo1 Mo1 118.608(9) . 2
Se2 Mo1 Mo1 118.597(8) 12 2
Se1 Mo1 Mo1 58.704(6) . 2
Re1 Mo1 Mo1 59.9 12 2
Mo1 Mo1 Mo1 59.935(4) 12 2
Mo1 Mo1 Mo1 90.0 11 2
Re1 Mo1 Mo1 90.0 11 2
Mo1 Mo1 Mo1 60.0 3 2
Re1 Mo1 Mo1 60.0 3 2
Re1 Se1 Mo1 0.0 3 3
Re1 Se1 Re1 62.594(12) 3 2
Mo1 Se1 Re1 62.594(12) 3 2
Re1 Se1 Mo1 62.6 3 2
Mo1 Se1 Mo1 62.594(12) 3 2
Re1 Se1 Mo1 0.0 2 2
Re1 Se1 Mo1 62.6 3 .
Mo1 Se1 Mo1 62.591(12) 3 .
Re1 Se1 Mo1 62.6 2 .
Mo1 Se1 Mo1 62.592(12) 2 .
Re1 Se2 Mo1 0.0 3 3
Re1 Se2 Mo1 62.8 3 .
Mo1 Se2 Mo1 62.751(9) 3 .
Re1 Se2 Mo1 62.6 3 11
Mo1 Se2 Mo1 62.591(9) 3 11
Mo1 Se2 Mo1 62.584(9) . 11
Re1 Se2 Re1 62.591(9) 3 11
Mo1 Se2 Re1 62.591(9) 3 11
Mo1 Se2 Re1 62.6 . 11
Mo1 Se2 Re1 0.000(13) 11 11
N1 C1 Mo1 177.8(3) . .
C1 N1 Cd1 122.1(2) . .
N2 Cd1 N2 180.0 . 16
N2 Cd1 N3 87.55(13) . .
N2 Cd1 N3 92.45(13) 16 .
N2 Cd1 N3 92.45(13) . 16
N2 Cd1 N3 87.55(13) 16 16
N3 Cd1 N3 180.0 . 16
N2 Cd1 N1 87.17(11) . .
N2 Cd1 N1 92.83(11) 16 .
N3 Cd1 N1 87.03(11) . .
N3 Cd1 N1 92.97(11) 16 .
N2 Cd1 N1 92.83(11) . 16
N2 Cd1 N1 87.17(11) 16 16
N3 Cd1 N1 92.97(11) . 16
N3 Cd1 N1 87.03(11) 16 16
N1 Cd1 N1 180.0 . 16
Cd1 N2 H2A 109.5 . .
Cd1 N2 H2B 109.5 . .
H2A N2 H2B 109.5 . .
Cd1 N2 H2C 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
Cd1 N3 H3A 109.5 . .
Cd1 N3 H3B 109.5 . .
H3A N3 H3B 109.5 . .
Cd1 N3 H3C 109.5 . .
H3A N3 H3C 109.5 . .
H3B N3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mo1 C1 2.152(3) .
Mo1 Se2 2.5476(3) 2
Mo1 Se2 2.5482(3) .
Mo1 Se2 2.5501(3) 12
Mo1 Se1 2.5537(4) .
Mo1 Re1 2.6480(3) 12
Mo1 Mo1 2.6480(3) 12
Mo1 Mo1 2.6480(3) 11
Mo1 Re1 2.6480(3) 11
Mo1 Mo1 2.6531(3) 3
Mo1 Re1 2.6531(3) 3
Mo1 Mo1 2.6531(3) 2
Se1 Re1 2.5537(4) 3
Se1 Mo1 2.5537(4) 3
Se1 Re1 2.5537(4) 2
Se1 Mo1 2.5537(4) 2
Se2 Re1 2.5475(3) 3
Se2 Mo1 2.5475(3) 3
Se2 Mo1 2.5501(3) 11
Se2 Re1 2.5501(3) 11
C1 N1 1.148(4) .
N1 Cd1 2.419(3) .
Cd1 N2 2.310(3) .
Cd1 N2 2.310(3) 16
Cd1 N3 2.346(3) .
Cd1 N3 2.347(3) 16
Cd1 N1 2.419(3) 16
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
N3 H3A 0.8900 .
N3 H3B 0.8900 .
N3 H3C 0.8900 .
