Reversible Redox Activity in Multicomponent Metal-Organic Frameworks Constructed from Trinuclear Copper Pyrazolate Building Blocks.
Tu, Binbin; Pang, Qingqing; Xu, Huoshu; Li, Xiaomin; Wang, Yulin; Ma, Zhen; Weng, Linhong; Li, Qiaowei; Journal of the American Chemical Society 139 (2017) 7998–8007; doi:10.1021/jacs.7b03578

data_4126371
_publ_section_title
;
 Reversible Redox Activity in Multicomponent Metal-Organic Frameworks
 Constructed from Trinuclear Copper Pyrazolate Building Blocks.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7998
_journal_page_last               8007
_journal_paper_doi               10.1021/jacs.7b03578
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C40 H20 Cu9 N20 O24 Zn6'
_chemical_formula_weight         2128.84
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.220(2)
_cell_length_b                   30.220(2)
_cell_length_c                   34.323(6)
_cell_measurement_reflns_used    587
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      48.267
_cell_measurement_theta_min      2.056
_cell_volume                     31345(6)
_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  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0701
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            42424
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        51.703
_diffrn_reflns_theta_max         51.703
_diffrn_reflns_theta_min         1.948
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.586
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8264
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.468
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8340
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.492
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0881
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+86.5792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2128
_refine_ls_wR_factor_ref         0.2247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5796
_reflns_number_total             8340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03578_si_003.cif
_cod_data_source_block           FDM-5
_cod_original_cell_volume        31346(7)
_cod_database_code               4126371
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              41557
_shelx_hkl_checksum              19199