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_4349531
_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            'C58 H106 N2 O27 V6'
_chemical_formula_weight         1569.09
_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
;
2016-06-13 deposited with the CCDC.
2016-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.354(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.5756(3)
_cell_length_b                   15.3260(4)
_cell_length_c                   20.1152(5)
_cell_measurement_reflns_used    5576
_cell_measurement_temperature    104.1
_cell_measurement_theta_max      29.2569
_cell_measurement_theta_min      2.9854
_cell_volume                     3498.75(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      104.1
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17371
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.32
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.9050
_exptl_absorpt_correction_T_min  0.8832
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.126
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         8064
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0726P)^2^+5.1297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                6176
_reflns_number_total             8064
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00302h2.cif
_cod_data_source_block           exp_3912
_cod_original_cell_volume        3498.75(15)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4349531