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_4088302
_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         'C16 H16 Cl4 N4 Rh, C H2 Cl2'
_chemical_formula_sum            'C17 H20 Cl7 N4 Rh'
_chemical_formula_weight         631.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 113.4460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0614(2)
_cell_length_b                   16.4011(3)
_cell_length_c                   13.7065(3)
_cell_measurement_reflns_used    25632
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.596
_cell_measurement_theta_min      3.194
_cell_volume                     2281.31(8)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25632
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         29.596
_diffrn_reflns_theta_min         3.194
_exptl_absorpt_coefficient_mu    1.582
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2012)
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_description       Block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.280
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         6389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+2.5046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5833
_reflns_number_total             6389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00993_si_002.cif
_cod_data_source_block           '[6]'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088302
_shelx_estimated_absorpt_t_min   0.530
_shelx_estimated_absorpt_t_max   0.666