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_4107310
_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            'C222 H276 Ag30 N60'
_chemical_formula_weight         7021.13
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/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                   61.7239(11)
_cell_length_b                   61.7239(11)
_cell_length_c                   26.9189(5)
_cell_measurement_temperature    153(2)
_cell_volume                     102557(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0817
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_max       64
_diffrn_reflns_limit_h_min       -75
_diffrn_reflns_limit_k_max       76
_diffrn_reflns_limit_k_min       -74
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            278836
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    2.289
_exptl_absorpt_correction_T_max  0.8942
_exptl_absorpt_correction_T_min  0.7252
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   REQABA
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_description       prism
_exptl_crystal_F_000             55008
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2868
_refine_ls_number_reflns         50234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+954.6649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                38393
_reflns_number_total             50234
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075408b-file007.cif
_cod_data_source_block           1-Ag.M
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4107310