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)
Muravieva, Viktoria K.; Gayfulin, Yakov M.; Lemoine, Pierric; Cordier, stéphane; Naumov, Nikolay G.; CrystEngComm  (2018) –; doi:10.1039/C8CE00527C

data_7230863
_publ_section_title
;
 Stabilization of interpenetrating cluster-based frameworks promoted by
 N-H&#x2026;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         'C12 H66 Cd5 Mo6 N34 O5 Re6 Se16'
_chemical_formula_sum            'C12 H66 Cd5 Mo6 N34 O5 Re6 Se16'
_chemical_formula_weight         4285.18
_chemical_name_systematic
{[Cd(NH3)5]2[Cd(NH3)4]3[Re3Mo3Se8(CN)6]2}\^A.5H2O
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2018-05-31 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                85.142(4)
_cell_angle_beta                 86.718(4)
_cell_angle_gamma                88.258(4)
_cell_formula_units_Z            2
_cell_length_a                   10.2664(8)
_cell_length_b                   17.7456(11)
_cell_length_c                   22.3759(14)
_cell_measurement_reflns_used    5693
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.52
_cell_measurement_wavelength     0.71073
_cell_volume                     4053.9(5)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2014)'
_computing_molecular_graphics
'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2018)'
_computing_structure_refinement  'SHELXL-2014_7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.1354
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         2.949
_exptl_absorpt_coefficient_mu    18.317
_exptl_absorpt_correction_T_max  0.481
_exptl_absorpt_correction_T_min  0.307
_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    3.519
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.448
_refine_diff_density_min         -2.851
_refine_diff_density_rms         0.407
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         17950
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1420
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0474P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1453
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9447
_reflns_number_total             17950
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ce00527c2.cif
_cod_data_source_block           PL39_150K
_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_database_code               7230863
_shelx_res_checksum              45266