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_2021257
_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          '(C8 H20 N1)5 [V12 O32 (N3)], C1 H3 N1 O2'
_chemical_formula_moiety         '5(C8 H20 N1 +), N3 O32 V12 5-, C1 H3 N1 O2'
_chemical_formula_sum            'C41 H103 N9 O34 V12'
_chemical_formula_weight         1877.60
_chemical_name_systematic
;
Pentakis(tetraethylammonium) azidododecavanadate nitromethane monosolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.3672(11)
_cell_length_b                   13.0801(5)
_cell_length_c                   20.6502(8)
_cell_measurement_reflns_used    31221
_cell_measurement_temperature    83(2)
_cell_measurement_theta_max      27.5027
_cell_measurement_theta_min      3.0902
_cell_volume                     7122.0(5)
_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 7.314
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            76477
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         3.090
_exptl_absorpt_coefficient_mu    1.585
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(NUMABS; Rigaku, 1999)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.241
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.435
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 6803 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.022(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         16085
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0378P)^2^+4.2487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                15235
_reflns_number_total             16085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jr3005sup1.cif
_cod_data_source_block           1
_cod_database_code               2021257
_cod_database_fobs_code          2021257
_shelx_estimated_absorpt_t_min   0.742
_shelx_estimated_absorpt_t_max   0.742
_shelx_hkl_checksum              80212
_shelx_res_checksum              36531
_shelxl_version_number           2.014