Chiral (SO)‒N‒(SO) Sulfoxide Pincer Complexes of Mg, Rh, and Ir: N‒H Activation and Selective Sulfoxide Reduction upon Ligand Coordination
Locke, Harald; Herrera, Alberto; Heinemann, Frank W.; Linden, Anthony; Frieß, Sibylle; Schmid, Bernhard; Dorta, Romano; Organometallics 34 (2015) 1925–; doi:10.1021/acs.organomet.5b00178

data_4085779
_publ_section_title
;
 Chiral (SO)--N--(SO) Sulfoxide Pincer Complexes of Mg, Rh, and Ir: N--H
 Activation and Selective Sulfoxide Reduction upon Ligand Coordination
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1925
_journal_paper_doi               10.1021/acs.organomet.5b00178
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H39 Cl3 N O Rh S2, 3.5(C6 H6)'
_chemical_formula_sum            'C55 H60 Cl3 N O Rh S2'
_chemical_formula_weight         1024.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                73.207(4)
_cell_angle_beta                 89.745(5)
_cell_angle_gamma                72.852(5)
_cell_formula_units_Z            2
_cell_length_a                   12.4011(8)
_cell_length_b                   13.7958(8)
_cell_length_c                   16.2240(9)
_cell_measurement_reflns_used    388
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     2529.3(3)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 \f- and \w-rotations with 2.00 \% and 30 sec per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            151238
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1066
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack H D (1983), Acta Cryst. A39, 876-881
 12808 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   0.059(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         25616
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+1.9635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0583
_reflns_number_gt                22502
_reflns_number_total             25616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00178_si_001.cif
_cod_data_source_block           rd1403_p1
_cod_depositor_comments
'Adding full bibliography for 4085777--4085779.cif.'
_cod_original_sg_symbol_Hall     P1
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4085779