Electronic Control of Metal-Centered Chirality in η5:κS-Indenyl-Sulfanyl and -Sulfinyl Rhodacycles of 2-Phenylpyridine
Baker, Robert W.; Turner, Peter; Luck, Ian J.; Organometallics 34 (2015) 1751–; doi:10.1021/acs.organomet.5b00255

data_4087547
_publ_section_title
;
 Electronic Control of Metal-Centered Chirality in
 \h5:\kS-Indenyl-Sulfanyl and -Sulfinyl Rhodacycles of 2-Phenylpyridine
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1751
_journal_paper_doi               10.1021/acs.organomet.5b00255
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C33 H27 Cl2 F6 N O Rh S Sb'
_chemical_formula_weight         895.18
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.576(2)
_cell_angle_beta                 87.844(2)
_cell_angle_gamma                76.751(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0569(3)
_cell_length_b                   9.0206(3)
_cell_length_c                   22.9236(8)
_cell_measurement_temperature    150(2)
_cell_volume                     1614.22(10)
_computing_cell_refinement       'SAINT (Bruker-AXS,2012)'
_computing_data_collection       'APEX (Bruker-AXS,2012)'
_computing_data_reduction        'SAINT and XPREP (Bruker-AXS,2012)'
_computing_molecular_graphics
;
  xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999)
  ORTEPII  (Johnson,C.K., 1976). 
  WinGX (Farrugia, 1999)
  shelXle (H&#x00FC;bschle,C.B., et al., 2011) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_crystal_treatment
;
attached with Exxon Paratone N, to a short length 
of fibre supported on a thin piece of copper wire 
inserted in a copper mounting pin.  The crystal was 
quenched in a cold nitrogen gas stream from an 
Oxford Cryosystems Cryostream. 
;
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  APEXII-FR591
_diffrn_measurement_method       \w+\f
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            64692
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         35.09
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS (Sheldrick, 1996)
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'prismatic fragment'
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.070
_refine_diff_density_min         -1.569
_refine_diff_density_rms         0.235
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.054(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         24095
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0325
_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^)+(0.05P)^2^P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                22854
_reflns_number_total             24095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00255_si_001.cif
_cod_data_source_block           rwb13pt1a_sad
_cod_database_code               4087547