Syntheses and post-functionalization of tri-substituted polyalkoxohexavanadates containing tris(alkoxo) ligands
Wei, Yongge; Xiao, Zicheng; Hu, Xunliang; Hu, Xiaokang; Huang, Bo; Cheng, Min; Wu, Pingfan; Lin, Xinjun; Dalton Trans.  (2017) –; doi:10.1039/C7DT01543G

data_7043285
_publ_section_title
;
 Syntheses and post-functionalization of tri-substituted
 polyalkoxohexavanadates containing tris(alkoxo) ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01543G
_journal_year                    2017
_chemical_formula_sum            'C12 H30 N3 Na2 O22 V6'
_chemical_formula_weight         920.02
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_Hall           'I 2 2 3'
_space_group_name_H-M_alt        'I 2 3'
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-06-01 deposited with the CCDC.
2017-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.168(2)
_cell_length_b                   19.168(2)
_cell_length_c                   19.168(2)
_cell_measurement_reflns_used    3055
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.665
_cell_measurement_theta_min      2.603
_cell_volume                     7042.6(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27422
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.272
_diffrn_reflns_theta_min         1.502
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5302
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1140 before and 0.0866 after correction.
The Ratio of minimum to maximum transmission is 0.7113.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       block
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 837 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2403
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0536P)^2^+10.2242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1987
_reflns_number_total             2403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01543g2.cif
_cod_data_source_block           03241_sq
_cod_original_cell_volume        7042(2)
_cod_database_code               7043285
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              82078
_shelx_fab_checksum              76249