Tetraaquadodekakis-μ~2~-chlorido-diiodido-<i>octahedro</i>-hexaniobium(12 <i>Nb</i>—<i>Nb</i>) tetrahydrofuran octasolvate
Schröder, Florian; Köckerling, Martin; IUCrData 7 (2022) x220618–; doi:10.1107/S2414314622006186

data_1567144
_publ_section_title
;
 Tetraaquadodekakis-\m~2~-chlorido-diiodido-<i>octahedro</i>-hexaniobium(12
 <i>Nb</i>---<i>Nb</i>) tetrahydrofuran octasolvate
;
_journal_coeditor_code           WM4165
_journal_issue                   6
_journal_name_full               IUCrData
_journal_page_first              x220618
_journal_paper_doi               10.1107/S2414314622006186
_journal_volume                  7
_journal_year                    2022
_chemical_formula_iupac          '[Nb6 Cl12 I2 (H2 O)4], 8C4 H8 O'
_chemical_formula_moiety         'H8 O4 Cl12 I2 Nb6, 8(C4 H8 O)'
_chemical_formula_sum            'C32 H72 Cl12 I2 Nb6 O12'
_chemical_formula_weight         1885.55
_chemical_name_systematic
;
Tetraaquadodekakis-\m~2~-chlorido-diiodido-<i>octahedro</i>-\
hexaniobium(12 <i>Nb</i>---<i>Nb</i>) tetrahydrofuran octasolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.3389(7)
_cell_length_b                   18.1968(7)
_cell_length_c                   34.0390(10)
_cell_measurement_reflns_used    9812
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.958
_cell_measurement_theta_min      2.4575
_cell_volume                     11978.5(7)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            94479
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.026
_diffrn_reflns_theta_min         1.594
_exptl_absorpt_coefficient_mu    2.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             7328
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         1.472
_refine_diff_density_min         -1.499
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         15885
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0359P)^2^+173.2937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                11673
_reflns_number_total             15885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4165sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        11978.6(8)
_cod_database_code               1567144
_shelx_estimated_absorpt_t_min   0.577
_shelx_estimated_absorpt_t_max   0.705
_shelx_hkl_checksum              12203
_shelx_res_checksum              30653
_shelxl_version_number           201.4
_cod_database_fobs_code 1567144