Synthesis and structural characterization of tube-type tetradecavanadates
Kuwajima, Sho; Arai, Yuta; Kitajima, Hiromasa; Kikukawa, Yuji; Hayashi, Yoshihito; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S2053229618008914

data_2021259
_publ_section_title
;
 Synthesis and structural characterization of tube-type tetradecavanadates
;
_journal_coeditor_code           JR3005
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618008914
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '(N1 H4)7 [V14 O38 (O C N)], 6C2 H6 O S'
_chemical_formula_moiety         '7(N1 H4 +), C1 N1 O39 V14 7-, 6(C2 H6 O S)'
_chemical_formula_sum            'C13 H64 N8 O45 S6 V14'
_chemical_formula_weight         1958.24
_chemical_name_systematic
;
Heptaammonium cyanatotetradecavanadate dimethyl sulfoxide hexasolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 116.537(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.352(6)
_cell_length_b                   24.753(6)
_cell_length_c                   14.561(5)
_cell_measurement_reflns_used    12134
_cell_measurement_temperature    83(2)
_cell_measurement_theta_max      27.5399
_cell_measurement_theta_min      3.1275
_cell_volume                     6240(3)
_computing_cell_refinement
;
CrystalClear (Rigaku/MSC, 2006)
;
_computing_data_collection
;
CrystalClear (Rigaku/MSC, 2006)
;
_computing_data_reduction
;
CrystalClear (Rigaku/MSC, 2006)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      83(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33228
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_min         3.128
_exptl_absorpt_coefficient_mu    2.295
_exptl_absorpt_correction_T_max  0.8919
_exptl_absorpt_correction_T_min  0.6556
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(NUMABS; Rigaku, 1999)
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.084
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.319
_refine_diff_density_min         -1.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7133
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0965P)^2^+17.6756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1456
_reflns_number_gt                6028
_reflns_number_total             7133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3005sup1.cif
_cod_data_source_block           3
_cod_database_code               2021259
_shelx_estimated_absorpt_t_min   0.657
_shelx_estimated_absorpt_t_max   0.657
_shelx_hkl_checksum              63462
_shelx_res_checksum              5429
_shelxl_version_number           2.014
_cod_database_fobs_code 2021259