A 3D POM‒MOF composite based on Ni(ΙΙ) ion and 2,2′-bipyridyl-3,3′-dicarboxylic acid: Crystal structure and proton conductivity
Wei, Meilin; Wang, Xiaoxiang; Sun, Jingjing; Duan, Xianying; Journal of Solid State Chemistry 202 (2013) 200–206; doi:10.1016/j.jssc.2013.03.041

data_1562632
_publ_section_title
;
 A 3D POM--MOF composite based on Ni(\I\I) ion and
 2,2&#x2032;-bipyridyl-3,3&#x2032;-dicarboxylic acid: Crystal structure
 and proton conductivity
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              200
_journal_page_last               206
_journal_paper_doi               10.1016/j.jssc.2013.03.041
_journal_volume                  202
_journal_year                    2013
_chemical_formula_sum            'C24 H39 N4 Ni2 O60 P W12'
_chemical_formula_weight         3698.18
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.523(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9156(12)
_cell_length_b                   16.1295(17)
_cell_length_c                   22.701(3)
_cell_measurement_reflns_used    3877
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      2.53
_cell_volume                     3984.4(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15073
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    17.823
_exptl_absorpt_correction_T_max  0.056
_exptl_absorpt_correction_T_min  0.013
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3300
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.689
_refine_diff_density_min         -2.436
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         6987
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                5057
_reflns_number_total             6987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-202-200.cif
_cod_data_source_block           1
_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_cell_volume        3984.4(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1562632
_cod_database_fobs_code 1562632