Combining Pyrazolate and N-Heterocyclic Carbene Coordination Motifs: Synthesis and Characterization of a Double-Crowned Silver Complex
Scheele, Ulrich J.; Georgiou, Maria; John, Michael; Dechert, Sebastian; Meyer, Franc; Organometallics 27 (2008) 5146–; doi:10.1021/om800487e

data_4071961
_publ_section_title
;
 Combining Pyrazolate and N-Heterocyclic Carbene Coordination Motifs:
 Synthesis and Characterization of a Double-Crowned Silver Complex
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5146
_journal_paper_doi               10.1021/om800487e
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C58 H62 Ag4 N12 2+, 2(F6 P -), 4(C3 H6 O)'
_chemical_formula_sum            'C70 H86 Ag4 F12 N12 O4 P2'
_chemical_formula_weight         1880.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.361(3)
_cell_angle_beta                 68.893(3)
_cell_angle_gamma                80.629(3)
_cell_formula_units_Z            1
_cell_length_a                   12.5681(5)
_cell_length_b                   12.9967(5)
_cell_length_c                   14.3012(6)
_cell_measurement_reflns_used    23394
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      1.68
_cell_volume                     1947.95(15)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23394
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.114
_exptl_absorpt_correction_T_max  0.8155
_exptl_absorpt_correction_T_min  0.6622
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         8462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0397P)^2^+2.2052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0745
_reflns_number_gt                7426
_reflns_number_total             8462
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800487e_si_002.cif
_cod_data_source_block           3-mg1
_cod_original_cell_volume        1947.95(14)
_cod_database_code               4071961