(C~7~H~6~NS)~2~[Nb~6~Cl~18~]·2C~4~H~8~O: first niobium cluster with an <i>N</i>,<i>S</i>-heterocyclic cation
Sperlich, Eric; Köckerling, Martin; IUCrData 3 (2018) x181760–; doi:10.1107/S2414314618017601

data_1550374
_publ_section_title
;
 (C~7~H~6~NS)~2~[Nb~6~Cl~18~]&#x00B7;2C~4~H~8~O: first niobium cluster
 with an <i>N</i>,<i>S</i>-heterocyclic cation
;
_journal_coeditor_code           ZQ4033
_journal_issue                   12
_journal_name_full               IUCrData
_journal_page_first              x181760
_journal_paper_doi               10.1107/S2414314618017601
_journal_volume                  3
_journal_year                    2018
_chemical_formula_iupac          '(C7 H6 N1 S1)2 [Nb6 Cl18], 2C4 H8 O1'
_chemical_formula_moiety         '2(C7 H6 N1 S1 +), Cl18 Nb6 2-, 2(C4 H8 O1)'
_chemical_formula_sum            'C22 H28 Cl18 N2 Nb6 O2 S2'
_chemical_formula_weight         1612.14
_chemical_name_systematic
;
Bis(benzothiazolium)
dodeca-\m-chlorido-hexachlorido-<i>octahedro</i>-hexaniobium(12 <i>Nb---Nb</i>)
tetrahydrofuran disolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 102.5980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7110(3)
_cell_length_b                   24.1710(10)
_cell_length_c                   11.0653(4)
_cell_measurement_reflns_used    9607
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.875
_cell_measurement_theta_min      2.3955
_cell_volume                     2273.75(15)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008),
<i>DIAMOND</i> (Brandenburg & Putz, 2014)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_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  0.0448
_diffrn_reflns_av_unetI/netI     0.0149
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            102833
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.933
_diffrn_reflns_theta_min         2.396
_exptl_absorpt_coefficient_mu    2.607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2017)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.355
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.250
_refine_diff_density_min         -0.997
_refine_ls_extinction_coef       0.00216(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5454
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0133P)^2^+5.1918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0453
_refine_ls_wR_factor_ref         0.0472
_reflns_number_gt                4867
_reflns_number_total             5454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zq4033sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2273.8(2)
_cod_database_code               1550374
_shelx_estimated_absorpt_t_min   0.624
_shelx_estimated_absorpt_t_max   0.696
_shelx_hkl_checksum              34490
_shelx_res_checksum              40264
_cod_database_fobs_code 1550374