Highly Porous 4,8-Connected Metal-Organic Frameworks: Synthesis, Characterization, and Hydrogen Uptake
David J. Mihalcik; Teng Zhang; Liqing Ma; Wenbin Lin; Inorganic Chemistry 51 (2012) 2503–2508; doi:10.1021/ic2024296

data_4328416
_publ_section_title
;
 Highly Porous 4,8-Connected Metal-Organic Frameworks: Synthesis,
 Characterization, and Hydrogen Uptake
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2503
_journal_page_last               2508
_journal_paper_doi               10.1021/ic2024296
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C77 H12 Cu4 O22'
_chemical_formula_weight         1543.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           75
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4'
_symmetry_space_group_name_H-M   'P 4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.02890(10)
_cell_length_b                   19.02890(10)
_cell_length_c                   21.9107(3)
_cell_measurement_reflns_used    5113
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      50.21
_cell_measurement_theta_min      2.32
_cell_volume                     7933.84(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16071
_diffrn_reflns_theta_full        50.45
_diffrn_reflns_theta_max         50.45
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.9737
_exptl_absorpt_correction_T_min  0.7160
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.646
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         7594
_refine_ls_number_restraints     227
_refine_ls_restrained_S_all      0.817
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0300P)^2^+8.4779P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                5159
_reflns_number_total             7594
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2024296_si_001_3.cif
_cod_data_source_block           MOF-3
_cod_database_code               4328416