Chiral cyclopentadienylruthenium sulfoxide catalysts for asymmetric redox bicycloisomerization.
Trost, Barry M.; Ryan, Michael C.; Rao, Meera; Beilstein journal of organic chemistry 12 (2016) 1136–1152; doi:10.3762/bjoc.12.110

data_4031991
_publ_section_title
;
 Chiral cyclopentadienylruthenium sulfoxide catalysts for asymmetric redox
 bicycloisomerization.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              1136
_journal_page_last               1152
_journal_paper_doi               10.3762/bjoc.12.110
_journal_volume                  12
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H41 N O4 S'
_chemical_formula_sum            'C26 H41 N O4 S'
_chemical_formula_weight         463.66
_chemical_name_systematic
;
 ?
;
_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   geom
_atom_sites_solution_primary     vecmap
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                104.549(2)
_cell_angle_beta                 95.9357(14)
_cell_angle_gamma                105.2328(15)
_cell_formula_units_Z            1
_cell_length_a                   5.8864(3)
_cell_length_b                   9.2540(6)
_cell_length_c                   12.6617(7)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.98
_cell_measurement_theta_min      3.67
_cell_volume                     633.46(6)
_computing_cell_refinement       'Bruker SAINT v8.32B'
_computing_data_collection       'Bruker APEX-II v2013-10.0'
_computing_data_reduction        'Bruker SAINT v8.32B'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20537
_diffrn_reflns_point_group_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.975
_diffrn_reflns_theta_min         3.667
_diffrn_source                   'Incoatec micro-focus'
_exptl_absorpt_coefficient_mu    1.377
_exptl_absorpt_correction_T_max  0.9572
_exptl_absorpt_correction_T_min  0.8230
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       block
_exptl_crystal_F_000             252
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.139
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 2147 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.075(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4568
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+0.0377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.917
_reflns_Friedel_fraction_full    0.892
_reflns_Friedel_fraction_max     0.878
_reflns_number_gt                4538
_reflns_number_total             4568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1860-5397-12-110-S2.cif
_cod_data_source_block           su1401
_cod_depositor_comments          'Adding full bibliography for 4031991.cif.'
_cod_database_code               4031991
_shelx_estimated_absorpt_t_min   0.800
_shelx_estimated_absorpt_t_max   0.886
_diffrn_source_monochromator     'MONTEL Multi-layer'
_shelxl_version_number           2014-3
_shelx_res_checksum              83935
_shelx_hkl_checksum              45146