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_4085777
_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 N O2 S2'
_chemical_formula_sum            'C34 H39 N O2 S2'
_chemical_formula_weight         557.81
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90.6518(12)
_cell_angle_beta                 107.7749(12)
_cell_angle_gamma                102.1293(13)
_cell_formula_units_Z            2
_cell_length_a                   9.76176(14)
_cell_length_b                   10.73671(17)
_cell_length_c                   15.8354(2)
_cell_measurement_reflns_used    37828
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      30.0240
_cell_measurement_theta_min      2.2860
_cell_volume                     1540.09(4)
_computing_cell_refinement
'CrysAlisPro, Version 1.171.37.31d (Agilent Technologies, 2014)'
_computing_data_collection
'CrysAlisPro, Version 1.171.37.31d (Agilent Technologies, 2014)'
_computing_data_reduction
'CrysAlisPro, Version 1.171.37.31d (Agilent Technologies, 2014)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-2014 and PLATON (Spek, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2008)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector                 'Atlas CCD camera on \k goniostat'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova, dual radiation diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.424
_diffrn_reflns_theta_min         2.230
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlisPro, Version 1.171.37.31d (Agilent Technologies, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       prism
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 6815 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.020(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         16643
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.2478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.838
_reflns_number_gt                15464
_reflns_number_total             16643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00178_si_001.cif
_cod_data_source_block           3
_cod_depositor_comments
;Adding full bibliography for 4085777--4085779.cif.

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geom & difmap' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        1540.10(4)
_cod_database_code               4085777
_shelx_res_checksum              98135
_shelx_hkl_checksum              81865