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_4085778
_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         'C42 H52 N O2 Rh S2, 0.5(C5 H12)'
_chemical_formula_sum            'C44.5 H58 N O2 Rh S2'
_chemical_formula_weight         805.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.6511(16)
_cell_length_b                   19.562(2)
_cell_length_c                   30.787(4)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.47
_cell_volume                     8221.4(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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 83.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            124047
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2008'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3400
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack H D (1983), Acta Cryst. A39, 876-881
 8944 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   -0.024(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         19603
_refine_ls_number_restraints     143
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+5.7455P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                17689
_reflns_number_total             19603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00178_si_001.cif
_cod_data_source_block           rd1407
_cod_depositor_comments
;
Adding full bibliography for 4085777--4085779.cif.

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C89 H116 N2 O4 Rh2 S4'
_cod_original_formula_weight         1611.90
_cod_original_formula_moiety         '2(C42 H52 N O2 Rh S2), C5 H12'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        8221.4(16)
_cod_original_sg_symbol_Hall     P2ac2ab
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4085778