Synthesis of Homoleptic and Heteroleptic Bis-N-heterocylic Carbene Group 11 Complexes
Lazreg, Faïma; Cordes, David B.; Slawin, Alexandra M. Z.; Cazin, Catherine S. J.; Organometallics 34 (2015) 419–; doi:10.1021/om500882t

data_4085255
_publ_section_title
;
 Synthesis of Homoleptic and Heteroleptic Bis-N-heterocylic Carbene Group
 11 Complexes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              419
_journal_paper_doi               10.1021/om500882t
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C56 H78 Ag B F4 N4 O0.5'
_chemical_formula_sum            'C56 H78 Ag B F4 N4 O0.5'
_chemical_formula_weight         1009.93
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 103.637(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   19.598(6)
_cell_length_b                   12.678(4)
_cell_length_c                   21.866(7)
_cell_measurement_reflns_used    8546
_cell_measurement_temperature    93
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.61
_cell_volume                     5280(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b28'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b28 (Rigaku, 2013)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b28'
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Superflip (Palatinus, et al., 2007)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40362
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.389
_diffrn_reflns_theta_min         1.606
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2136.00
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.01
_refine_diff_density_min         -0.58
_refine_ls_abs_structure_details
;
 Flack x determined using 5697 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.467(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     1230
_refine_ls_number_reflns         18375
_refine_ls_number_restraints     8
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0349P)^2^+7.7557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                15125
_reflns_number_total             18375
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om500882t_si_002.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 4085255--4085264.cif.'
_cod_original_cell_volume        5279(3)
_cod_database_code               4085255