Tetrakis(triethylenediamin-1-ium) dodeca-μ2-chlorido-hexakis(thiocyanato-κN)hexa-octahedro-niobate
Sperlich, Eric; Köckerling, Martin; IUCrData 8 (2023) x230398–; doi:10.1107/S241431462300398X

data_1569177
_publ_section_title
;
 Tetrakis(triethylenediamin-1-ium)
 dodeca-\m2-chlorido-hexakis(thiocyanato-\kN)hexa-octahedro-niobate
;
_journal_coeditor_code           WM4186
_journal_issue                   5
_journal_name_full               IUCrData
_journal_page_first              x230398
_journal_paper_doi               10.1107/S241431462300398X
_journal_volume                  8
_journal_year                    2023
_chemical_formula_iupac          '(C6 H13 N2)4 [Nb6 (N C S)6 Cl12]'
_chemical_formula_moiety         '4(C6 H13 N2 +), C6 N6 S6 Cl12 Nb6 4-'
_chemical_formula_sum            'C30 H52 Cl12 N14 Nb6 S6'
_chemical_formula_weight         1784.08
_chemical_name_systematic
;Tetrakis(triethylenediamin-1-ium)
dodeca-\m~2~-chlorido-hexakis(thiocyanato-\k<i>N</i>)hexa-<i>octahedro</i>-niobate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'ciftab-2016 (M. K\"ockerling, 2016)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   25.399(2)
_cell_length_b                   25.399(2)
_cell_length_c                   30.418(2)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.6065
_cell_measurement_theta_min      2.5405
_cell_volume                     16994(2)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2019)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            84629
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.618
_diffrn_reflns_theta_min         1.142
_exptl_absorpt_coefficient_mu    1.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             10512
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.032
_refine_diff_density_min         -1.794
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         13784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+223.5098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                11834
_reflns_number_total             13784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4186.cif
_cod_data_source_block           I
_cod_original_cell_volume        16993(3)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               1569177
_shelx_estimated_absorpt_t_min   0.588
_shelx_estimated_absorpt_t_max   0.693
_shelx_hkl_checksum              51735
_shelx_res_checksum              84210
_shelxl_version_number           201.4