Preparation, structure and characterization of a series of vanadates
Guo, Hai-Yang; Zhang, Ting-Ting; Lin, Po-Han; Xiao-Zhang, Xiao-Zhang; Cui, Xiao-Bing; Huo, Qi-Sheng; Xu, Ji-Qing; CrystEngComm 19 (2017) 265–; doi:10.1039/C6CE02205G

data_7227152
_publ_section_title
;
 Preparation, structure and characterization of a series of vanadates
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              265
_journal_paper_doi               10.1039/C6CE02205G
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C51 H82 Cl N16 O42 V16 Zn3.5'
_chemical_formula_weight         2670.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-10-13 deposited with the CCDC.
2016-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                106.6560(10)
_cell_angle_beta                 92.9500(10)
_cell_angle_gamma                110.7850(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3655(9)
_cell_length_b                   17.7584(11)
_cell_length_c                   21.0540(14)
_cell_measurement_reflns_used    6615
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5389
_cell_measurement_theta_min      2.3836
_cell_volume                     4410.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28362
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.365
_diffrn_reflns_theta_min         1.877
_exptl_absorpt_coefficient_mu    2.662
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_description       block
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.880
_refine_diff_density_min         -1.843
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1186
_refine_ls_number_reflns         20617
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0860P)^2^+6.8878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13776
_reflns_number_total             20617
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02205g2.cif
_cod_data_source_block           shelx_1
_cod_depositor_comments
'Adding full bibliography for 7227152--7227155.cif.'
_cod_original_formula_sum        'C51 H82 Cl N16 O42 V16 Zn3.50'
_cod_database_code               7227152
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.618
_shelx_estimated_absorpt_t_max   0.707
_shelx_res_checksum              23195