Preparation of Rhodium(III) Di-NHC Chelate Complexes Featuring Two Different NHC Donors via a Mild NaOAc-Assisted C‒H Activation
Aznarez, Francisco; Sanz Miguel, Pablo J.; Tan, Tristan T. Y.; Hahn, F. Ekkehardt; Organometallics 35 (2016) 410–; doi:10.1021/acs.organomet.5b00993

data_4088300
_publ_section_title
;
 Preparation of Rhodium(III) Di-NHC Chelate Complexes Featuring Two
 Different NHC Donors via a Mild NaOAc-Assisted C--H Activation
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              410
_journal_paper_doi               10.1021/acs.organomet.5b00993
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C18 H21 Cl6 N4 Rh'
_chemical_formula_sum            'C18 H21 Cl6 N4 Rh'
_chemical_formula_weight         609
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-21T09:41:59-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.211(2)
_cell_length_b                   12.9088(15)
_cell_length_c                   20.443(2)
_cell_measurement_reflns_used    8600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.37
_cell_volume                     4541.9(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            47377
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.58
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.472
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         6084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0928
_reflns_number_gt                4696
_reflns_number_total             6084
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00993_si_002.cif
_cod_data_source_block           '[4]'
_cod_original_cell_volume        4541.8(9)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4088300