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_4085868
_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_formula_moiety         'C20 H28 Cu2 N8 O2, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C22 H31 Cu2 F12 N9 O2 P2'
_chemical_formula_weight         870.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.959(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5412(4)
_cell_length_b                   12.1285(3)
_cell_length_c                   21.8264(6)
_cell_measurement_reflns_used    9710
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.3297
_cell_measurement_theta_min      2.4679
_cell_volume                     3307.50(16)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement
'SHELXL97 (Sheldrick, 2008), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'MONTEL optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67240
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         6040
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0308P)^2^+7.0297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                5425
_reflns_number_total             6040
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om5012402_si_002.cif
_cod_data_source_block           compound_3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4085868