Heteroleptic Cu(I) Bis-diimine Complexes of 6,6'-Dimesityl-2,2'-bipyridine: A Structural, Theoretical and Spectroscopic Study
Michael G. Fraser; Holly van der Salm; Scott A. Cameron; Allan G. Blackman; Keith C. Gordon; Inorganic Chemistry 52 (2013) 2980–2992; doi:10.1021/ic302393p

data_4334121
_publ_section_title
;
 Heteroleptic Cu(I) Bis-diimine Complexes of
 6,6'-Dimesityl-2,2'-bipyridine: A Structural, Theoretical and
 Spectroscopic Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2980
_journal_page_last               2992
_journal_paper_doi               10.1021/ic302393p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C46 H54 B Br2 Cu F4 N4 O2'
_chemical_formula_weight         1005.10
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   13.823(5)
_cell_length_b                   15.613(5)
_cell_length_c                   21.150(5)
_cell_measurement_reflns_used    6688
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      24.66
_cell_measurement_theta_min      2.42
_cell_volume                     4565(2)
_computing_cell_refinement       'ApexII and SAINT (Bruker, 2001)'
_computing_data_collection       'ApexII (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'WinGX (Farrrugia, 1999)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      89(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker KAppa ApexII area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53494
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    2.287
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.599329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       Block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.470(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         9381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0355P)^2^+11.6860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                7511
_reflns_number_total             9381
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302393p_si_003_3.cif
_cod_data_source_block           Br2
_cod_database_code               4334121