Hydrothermal syntheses, crystal structures and characterization of new vanadoborates: The novel decorated cage cluster [V6B22O44(OH)10]
Liu, Xing; Zhou, Jian; An, Litao; Chen, Rong; Hu, Feilong; Tang, Qiuling; Journal of Solid State Chemistry 201 (2013) 79–84; doi:10.1016/j.jssc.2013.02.021

data_1562656
_publ_section_title
;
 Hydrothermal syntheses, crystal structures and characterization of new
 vanadoborates: The novel decorated cage cluster [V6B22O44(OH)10]
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              79
_journal_page_last               84
_journal_paper_doi               10.1016/j.jssc.2013.02.021
_journal_volume                  201
_journal_year                    2013
_chemical_formula_moiety         '(B22 H10 O54 V6), 2(C6 H22 N4), 4.5(H2 O)'
_chemical_formula_sum            'C12 H63 B22 N8 O58.5 V6'
_chemical_formula_weight         1799.12
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.9670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.135(3)
_cell_length_b                   12.5320(13)
_cell_length_c                   23.237(4)
_cell_measurement_temperature    296(2)
_cell_volume                     6149.0(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17148
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  0.8334
_exptl_absorpt_correction_T_min  0.7332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.725
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         5458
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1177P)^2^+46.9986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1867
_refine_ls_wR_factor_ref         0.1974
_reflns_number_gt                4604
_reflns_number_total             5458
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-201-79.CIF
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C12 H63 B22 N8 O58.5 V6 '
_cod_database_code               1562656