Charge-Delocalized κ2C,N-NHC-Amine Complexes of Rhodium, Iridium, and Ruthenium
Jansen, Eveline; Lutz, Martin; Bruin, Bas de; Elsevier, Cornelis J.; Organometallics 33 (2014) 2853–; doi:10.1021/om5003599

data_4083345
_publ_section_title
;
 Charge-Delocalized \k2C,N-NHC-Amine Complexes of Rhodium, Iridium, and
 Ruthenium
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2853
_journal_paper_doi               10.1021/om5003599
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C52 H66 Cl3 N12 Ru2, F6 P, 2(C4 H8 O)'
_chemical_formula_sum            'C60 H82 Cl3 F6 N12 O2 P Ru2'
_chemical_formula_weight         1456.83
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                72.473(1)
_cell_angle_beta                 76.223(1)
_cell_angle_gamma                69.686(1)
_cell_formula_units_Z            2
_cell_length_a                   14.6524(3)
_cell_length_b                   15.6351(2)
_cell_length_c                   15.7371(2)
_cell_measurement_reflns_used    43279
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.73
_cell_volume                     3187.87(9)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, SADABS-2012/1'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            54212
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.729
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         14639
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+3.1462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12471
_reflns_number_total             14639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5003599_si_002.cif
_cod_data_source_block           l0581a
_cod_depositor_comments
'Adding full bibliography for 4083343--4083345.cif.'
_cod_database_code               4083345
_shelxl_version_number           2013-4
_shelx_res_checksum              45026
_shelx_hkl_checksum              46472