Supramolecular Isomerism, Framework Flexibility, Unsaturated Metal Center, and Porous Property of Ag(I)/Cu(I) 3,3',5,5'-Tetrametyl-4,4'-Bipyrazolate
Jie-Peng Zhang; Susumu Kitagawa; Journal of the American Chemical Society 130 (2008) 907–917; doi:10.1021/ja075408b

data_4107308
_publ_section_title
;
 Supramolecular Isomerism, Framework Flexibility, Unsaturated Metal
 Center, and Porous Property of Ag(I)/Cu(I)
 3,3',5,5'-Tetrametyl-4,4'-Bipyrazolate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              907
_journal_page_last               917
_journal_paper_doi               10.1021/ja075408b
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C60 H72 Ag12 N24'
_chemical_formula_weight         2423.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_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            16
_cell_length_a                   19.2056(5)
_cell_length_b                   47.9669(16)
_cell_length_c                   36.2063(9)
_cell_measurement_temperature    213(2)
_cell_volume                     33354.4(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '/w scan'
_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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49244
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    2.798
_exptl_absorpt_correction_T_max  0.6790
_exptl_absorpt_correction_T_min  0.5414
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   REQABA
_exptl_crystal_colour            plate-like
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_description       colorless
_exptl_crystal_F_000             18624
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         16191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0171P)^2^+400.8250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0975
_reflns_number_gt                12557
_reflns_number_total             16191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075408b-file005.cif
_cod_data_source_block           2-Ag
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               4107308