A fully reduced {V18IVO42} host and VO43–, Cl– as guest anions: synthesis, characterization and proton conductivity
Mulkapuri, Sateesh; Kurapati, Sathish Kumar; Mukhopadhyay, Subhabrata -; Das, Samar K.; New Journal of Chemistry 43 (2019) 17670–17679; doi:10.1039/C9NJ01918A

data_7058509
_publ_section_title
;
 A fully reduced {V18IVO42} host and VO43--, Cl-- as guest anions:
 synthesis, characterization and proton conductivity
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17670
_journal_page_last               17679
_journal_paper_doi               10.1039/C9NJ01918A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'O42 V18 4(N2) Cl 22(O) 5(Na)'
_chemical_formula_sum            'Cl N8 Na5 O64 V18'
_chemical_formula_weight         2203.40
_chemical_name_systematic        'Compound 2'
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   None
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-03-30 deposited with the CCDC.    2019-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   12.8267(8)
_cell_length_b                   12.8267(8)
_cell_length_c                   33.368(2)
_cell_measurement_reflns_used    9284
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      26.375
_cell_measurement_theta_min      2.203
_cell_volume                     4754.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            45165
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.375
_diffrn_reflns_theta_min         2.203
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.719
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3162
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.341
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0389P)^2^+10.5131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6360
_reflns_number_total             6492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj01918a2.cif
_cod_data_source_block           skd275
_cod_original_cell_volume        4754.3(7)
_cod_database_code               7058509
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              76091