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_7230866
_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         '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/[\s^2^(Fo^2^)+(0.0085P)^2^+15.3152P] where P=(Fo^2^+2Fc^2^)/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
_shelx_res_checksum              52866