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_4088301
_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_sum            'C75 H74 Cl26 N16 Rh4'
_chemical_formula_weight         2532.84
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.0240(10)
_cell_angle_beta                 98.1250(10)
_cell_angle_gamma                107.7150(10)
_cell_formula_units_Z            1
_cell_length_a                   11.4534(2)
_cell_length_b                   11.7735(2)
_cell_length_c                   18.7545(3)
_cell_measurement_reflns_used    14328
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.467
_cell_measurement_theta_min      2.403
_cell_volume                     2361.91(7)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52977
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.535
_diffrn_reflns_theta_min         2.007
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2012)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1258
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.240
_refine_diff_density_min         -2.214
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         14361
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+3.8100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11711
_reflns_number_total             14361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00993_si_002.cif
_cod_data_source_block           '[5]'
_cod_original_cell_volume        2361.90(7)
_cod_database_code               4088301
_shelx_estimated_absorpt_t_min   0.650
_shelx_estimated_absorpt_t_max   0.891