Hexaaquadodeca-μ2-chlorido-octahedro-hexaniobium diiodide
Schröder, Florian; Köckerling, Martin; IUCrData 6 (2021) x210696–; doi:10.1107/S2414314621006969

data_1564221
_publ_section_title
;
 Hexaaquadodeca-\m2-chlorido-octahedro-hexaniobium diiodide
;
_journal_coeditor_code           BT4115
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x210696
_journal_paper_doi               10.1107/S2414314621006969
_journal_volume                  6
_journal_year                    2021
_chemical_formula_iupac          '[Nb6 Cl12 (H2 O)6] I2'
_chemical_formula_moiety         'H12 Cl12 I2 Nb6 O6'
_chemical_formula_sum            'Cl12 H12 I2 Nb6 O6'
_chemical_formula_weight         1344.76
_chemical_name_systematic
;
Hexaaquadodeca-\m~2~-chlorido-<i>octahedro</i>-hexaniobium diiodide
;
_space_group_crystal_system      trigonal
_space_group_IT_number           162
_space_group_name_Hall           '-P 3 2'
_space_group_name_H-M_alt        'P -3 1 m'
_atom_sites_solution_hydrogens   difmap
_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            1
_cell_length_a                   9.3911(8)
_cell_length_b                   9.3911(8)
_cell_length_c                   8.6576(9)
_cell_measurement_reflns_used    9268
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      34.863
_cell_measurement_theta_min      2.5045
_cell_volume                     661.24(11)
_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
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.998
_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  0.0314
_diffrn_reflns_av_unetI/netI     0.0062
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43489
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         34.949
_diffrn_reflns_theta_min         3.437
_exptl_absorpt_coefficient_mu    6.076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS, Bruker, 2017)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.377
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.813
_refine_ls_extinction_coef       0.0071(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.376
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     27
_refine_ls_number_reflns         1059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.376
_refine_ls_R_factor_all          0.0131
_refine_ls_R_factor_gt           0.0130
_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^)+(0.0050P)^2^+1.1433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0335
_reflns_number_gt                1058
_reflns_number_total             1059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4115sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        661.20(10)
_cod_original_formula_sum        'H12 Cl12 I2 Nb6 O6'
_cod_database_code               1564221
_cod_database_fobs_code          1564221
_shelx_estimated_absorpt_t_min   0.376
_shelx_estimated_absorpt_t_max   0.443
_shelx_hkl_checksum              72253
_shelx_res_checksum              86351
_shelxl_version_number           201.4