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_7106325
_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         'C64 H64 Ag4 N12, 2.7[H2 O]'
_chemical_formula_sum            'C64 H69.4 Ag4 N12 O2.7'
_chemical_formula_weight         1481.40
_chemical_name_systematic
;
Tetrakis[3-isoquinolinyl-5-tertbutylpyrazolido]tetrasilver(I)
hydrate (3/2.7)
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 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            8
_cell_length_a                   18.6771(12)
_cell_length_b                   44.784(3)
_cell_length_c                   17.1502(11)
_cell_measurement_reflns_used    49319
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.87
_cell_measurement_theta_min      2.11
_cell_volume                     14345.0(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49319
_diffrn_reflns_theta_full        28.87
_diffrn_reflns_theta_max         28.87
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.123
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.671
_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    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             5976
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         9369
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0789P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                8111
_reflns_number_total             9369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc00054c.txt
_cod_data_source_block           jjh38a_(compound_4)
_cod_original_cell_volume        14344.9(15)
_cod_original_formula_sum        'C64 H69.40 Ag4 N12 O2.70'
_cod_database_code               7106325