New Insights into the Aggregation of Silver Pyrazolides Using Sterically Hindered Bidentate Pyrazole Ligands
James J. Henkelis; Colin A. Kilner; Malcolm A. Halcrow; Chem.Commun. 47 (2011) 5187–; doi:10.1039/c1cc00054c

data_7106324
_publ_section_title
;
 New Insights into the Aggregation of Silver Pyrazolides Using Sterically
 Hindered Bidentate Pyrazole Ligands
;
_journal_name_full               Chem.Commun.
_journal_page_first              5187
_journal_paper_doi               10.1039/c1cc00054c
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C96 H112 Ag10 N24, 2 Cl'
_chemical_formula_sum            'C96 H112 Ag10 Cl2 N24'
_chemical_formula_weight         2751.70
_chemical_name_systematic
;
Octakis[3-{pyrid-2-yl}-5-tertbutylpyrazolyl]decasilver(I)
dichloride
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 100.925(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.170(2)
_cell_length_b                   17.8880(14)
_cell_length_c                   24.0804(18)
_cell_measurement_reflns_used    116871
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      1.41
_cell_volume                     10645.5(14)
_computing_cell_refinement       'APEX 2 software, Bruker Nonius 2004'
_computing_data_collection       'APEX 2 software, Bruker Nonius 2004'
_computing_data_reduction        'SAINT, Bruker Nonius 2004'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean '120 microns'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker X8 Apex diffractometer'
_diffrn_measurement_method       'Rotation images'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            116871
_diffrn_reflns_theta_full        28.11
_diffrn_reflns_theta_max         28.11
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    1.851
_exptl_absorpt_correction_T_max  1.075
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2002). SADABS v. 2.03. University of
G/ottingen, Germany.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             5352
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.895
_refine_diff_density_min         -2.249
_refine_diff_density_rms         0.334
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         12807
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0838
_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^)+(0.1286P)^2^+454.9295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2603
_refine_ls_wR_factor_ref         0.2860
_reflns_number_gt                9389
_reflns_number_total             12807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc00054c.txt
_cod_data_source_block           jjh4_(compound_3)
_cod_original_cell_volume        10645.3(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7106324