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_4107311
_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            'C90 H108 Ag18 N36'
_chemical_formula_weight         3635.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           122
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_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                   27.1756(8)
_cell_length_b                   27.1756(8)
_cell_length_c                   81.019(3)
_cell_measurement_temperature    123(2)
_cell_volume                     59834(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -96
_diffrn_reflns_number            75674
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    2.340
_exptl_absorpt_correction_T_max  0.6519
_exptl_absorpt_correction_T_min  0.5924
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   REQABA
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       block-like
_exptl_crystal_F_000             27936
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         5.147
_refine_diff_density_min         -2.308
_refine_diff_density_rms         0.427
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.441
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         25968
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.437
_refine_ls_R_factor_all          0.1741
_refine_ls_R_factor_gt           0.1664
_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^)+(0.0300P)^2^+9000.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3831
_refine_ls_wR_factor_ref         0.3870
_reflns_number_gt                23345
_reflns_number_total             25968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075408b-file008.cif
_cod_data_source_block           1-Ag-I
_cod_original_cell_volume        59833(3)
_cod_database_code               4107311