Synthesis, crystal structure and spectroscopic studies of a series of hexavanadate hybrids with multiple functional groups
Huang, Bo; Xiao, Zicheng; Wu, Baolin; Hu, Xiaokang; Hu, Xunliang; Wu, Pingfan; Wei, Yongge; Inorganic Chemistry Frontiers 4 (2017) 165–; doi:10.1039/C6QI00302H

data_4349533
_publ_section_title
;
 Synthesis, crystal structure and spectroscopic studies of a series of
 hexavanadate hybrids with multiple functional groups
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              165
_journal_paper_doi               10.1039/C6QI00302H
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C50 H94 N2 O23 V6'
_chemical_formula_weight         1396.91
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-08-05 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.020(2)
_cell_length_b                   15.154(3)
_cell_length_c                   19.352(4)
_cell_measurement_reflns_used    9365
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.6960
_cell_measurement_theta_min      4.9900
_cell_volume                     3205.1(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      99.99(10)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'micro-focus sealed X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20587
_diffrn_reflns_theta_full        76.8031
_diffrn_reflns_theta_max         76.80
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    7.687
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5479
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.383
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6676
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.391
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0717P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1420
_reflns_number_gt                5849
_reflns_number_total             6676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00302h2.cif
_cod_data_source_block           zyt-1
_cod_original_cell_volume        3205.0(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349533