Conformational Control in Dirhodium(II) Paddlewheel Catalysts Supported by Chalcogen-Bonding Interactions for Stereoselective Intramolecular C‒H Insertion Reactions
Murai, Takuya; Lu, Wenjie; Kuribayashi, Toshifumi; Morisaki, Kazuhiro; Ueda, Yoshihiro; Hamada, Shohei; Kobayashi, Yusuke; Sasamori, Takahiro; Tokitoh, Norihiro; Kawabata, Takeo; Furuta, Takumi; ACS Catalysis  (2020) 568–578; doi:10.1021/acscatal.0c03689

data_4518345
_publ_section_title
;
 Conformational Control in Dirhodium(II) Paddlewheel Catalysts Supported
 by Chalcogen-Bonding Interactions for Stereoselective Intramolecular C--H
 Insertion Reactions
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              568
_journal_page_last               578
_journal_paper_doi               10.1021/acscatal.0c03689
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_sum            'C118 H75 Cl18 F12 N4 O16.5 Rh2 S8'
_chemical_formula_weight         3141.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.0449(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.9330(7)
_cell_length_b                   17.5225(6)
_cell_length_c                   24.1606(7)
_cell_measurement_reflns_used    82940
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      24.995
_cell_measurement_theta_min      1.539
_cell_volume                     13087.3(7)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrystalClear
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics
'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.922
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            82940
_diffrn_reflns_point_group_measured_fraction_full 0.869
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.539
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 MULABS - Empirical Correction for Absorption Anisotropy.
 Blessing, R. H., Acta Cryst., A51, 33-38 (1995).
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       prism
_exptl_crystal_F_000             6300
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 6238 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1735
_refine_ls_number_reflns         20019
_refine_ls_number_restraints     329
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+78.1888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    0.813
_reflns_Friedel_fraction_max     0.813
_reflns_number_gt                15475
_reflns_number_total             20019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c03689_si_006.cif
_cod_data_source_block           thiorh
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C118 H75 Cl18 F12 N4 O16.50 Rh2 S8'
_cod_database_code               4518345
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.733
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              93147
_shelx_hkl_checksum              20462