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_4518346
_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_moiety         'C96 H64 F12 N4 O14 Rh2, 2(C H Cl3)'
_chemical_formula_sum            'C98 H66 Cl6 F12 N4 O14 Rh2'
_chemical_formula_weight         2170.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4646(3)
_cell_length_b                   23.7613(5)
_cell_length_c                   26.3686(6)
_cell_measurement_reflns_used    123019
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.499
_cell_measurement_theta_min      1.714
_cell_volume                     9062.8(3)
_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 0.946
_diffrn_measured_fraction_theta_max 0.939
_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  0.0901
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            123019
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.714
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.939
_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    1.590
_exptl_crystal_description       prism
_exptl_crystal_F_000             4376
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.436
_refine_diff_density_min         -1.590
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details
;
 Flack x determined using 4299 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1231
_refine_ls_number_reflns         15087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0001P)^2^+54.2612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    0.859
_reflns_Friedel_fraction_max     0.841
_reflns_number_gt                11237
_reflns_number_total             15087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c03689_si_005.cif
_cod_data_source_block           rh
_cod_database_code               4518346
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              29441
_shelx_hkl_checksum              37926