Spectroscopic and Structural Properties of Bridge-Functionalized Dinuclear Coinage-Metal (Cu, Ag, and Au) NHC Complexes: A Comparative Study
Zhong, Rui; Pöthig, Alexander; Mayer, David C.; Jandl, Christian; Altmann, Philipp J.; Herrmann, Wolfgang A.; Kühn, Fritz E.; Organometallics  (2015) 150128111349001–; doi:10.1021/om5012402

data_4085869
_publ_section_title
;
 Spectroscopic and Structural Properties of Bridge-Functionalized
 Dinuclear Coinage-Metal (Cu, Ag, and Au) NHC Complexes: A Comparative
 Study
;
_journal_name_full               Organometallics
_journal_page_first              150128111349001
_journal_paper_doi               10.1021/om5012402
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C20 H28 Au2 N8 O2, 2(F6 P), O'
_chemical_formula_sum            'C20 H28 Au2 F12 N8 O3 P2'
_chemical_formula_weight         1112.38
_space_group_IT_number           46
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      46
_symmetry_space_group_name_Hall  'I 2 -2a'
_symmetry_space_group_name_H-M   'I m a 2'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3460(4)
_cell_length_b                   15.9879(4)
_cell_length_c                   16.7956(5)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.2917
_cell_measurement_theta_min      2.5479
_cell_volume                     3583.75(18)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX II Control Software (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement
'SHELXL2013 (Sheldrick, 2013), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50298
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    8.364
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.124
_platon_squeeze_details
;
The unit cell contains 4 diethyl ether molecules which have been treated as a 
diffuse contribution to the overall scattering without specific atom positions 
by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.500
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3422
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0133
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0125P)^2^+5.0386P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0292
_refine_ls_wR_factor_ref         0.0295
_reflns_number_gt                3309
_reflns_number_total             3422
_reflns_threshold_expression     i>2\s(i)
_cod_data_source_file            om5012402_si_002.cif
_cod_data_source_block           compound_4
_cod_database_code               4085869