Unprecedented Large Temperature Dependence of Silver(I)‒Silver(I) Distances in Some N-Heterocyclic Carbene Silver(I) Complex Salts
Kriechbaum, Margit; Hölbling, Johanna; Stammler, Hans-Georg; List, Manuela; Berger, Raphael J. F.; Monkowius, Uwe; Organometallics 32 (2013) 2876–; doi:10.1021/om300932r

data_4080660
_publ_section_title
;
 Unprecedented Large Temperature Dependence of Silver(I)--Silver(I)
 Distances in Some N-Heterocyclic Carbene Silver(I) Complex Salts
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2876
_journal_paper_doi               10.1021/om300932r
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C18 H32 Ag F6 N4 P'
_chemical_formula_weight         557.32
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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            32
_cell_length_a                   9.5037(12)
_cell_length_b                   24.321(3)
_cell_length_c                   83.460(10)
_cell_measurement_reflns_used    9814
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.7
_cell_measurement_theta_min      4.2
_cell_volume                     19291(4)
_computing_cell_refinement       'APEX 2, Bruker AXS'
_computing_data_collection       'APEX 2, Bruker AXS'
_computing_data_reduction        'APEX 2, Bruker AXS'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Bruker AXS X8 Prospector Ultra with APEX II'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'Quazar Montel multilayer optic Montel200'
_diffrn_radiation_source         'I\mS Incoatec Microfocus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2529
_diffrn_reflns_av_sigmaI/netI    0.1153
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       96
_diffrn_reflns_limit_l_min       -95
_diffrn_reflns_number            51508
_diffrn_reflns_theta_full        63.00
_diffrn_reflns_theta_max         63.00
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    7.863
_exptl_absorpt_correction_T_max  0.4757
_exptl_absorpt_correction_T_min  0.3466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             9088
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.765
_refine_diff_density_min         -3.063
_refine_diff_density_rms         0.241
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         14215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.1071
_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^)+(0.0928P)^2^+636.8818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2503
_refine_ls_wR_factor_ref         0.2545
_reflns_number_gt                13270
_reflns_number_total             14215
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300932r_si_002.cif
_cod_data_source_block           iPr2Im2AgPF6_100K
_cod_original_sg_symbol_H-M      C2221
_cod_database_code               4080660