A vanadium(IV) pyrazolate metal-organic polyhedron with permanent porosity and adsorption selectivity
A. W. Augustyniak; M. Fandzloch; M. Domingo; I. Lakomsk; J. A. R. Navarro; Chem.Commun. 51 (2015) 14724–; doi:10.1039/C5cc05913E

data_7117831
_publ_section_title
;
 A vanadium(IV) pyrazolate metal-organic polyhedron with permanent
 porosity and adsorption selectivity
;
_journal_name_full               Chem.Commun.
_journal_page_first              14724
_journal_paper_doi               10.1039/C5cc05913E
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C84 H60 N24 O40 V12'
_chemical_formula_weight         2656.84
_chemical_name_common            'Vanadium MOP'
_chemical_name_systematic        'Vanadium benzenebipyrazolate'
_space_group_IT_number           217
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-11 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   20.084(5)
_cell_length_b                   20.084(5)
_cell_length_c                   20.084(5)
_cell_measurement_reflns_used    1171
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.50
_cell_measurement_theta_min      2.87
_cell_volume                     8101(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1431
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9445
_diffrn_reflns_theta_full        17.28
_diffrn_reflns_theta_max         17.28
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2632
_exptl_crystal_preparation       'Magnetic properties, Adsorption'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.250
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1041P)^2^+3.3487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1648
_reflns_number_gt                467
_reflns_number_total             497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc05913e2.cif.txt
_cod_data_source_block           jg15
_cod_original_sg_symbol_H-M      I-43m
_cod_database_code               7117831