Chiral Rhodium(III) Complex-Catalyzed Cascade Michael-Alkylation Reactions: Enantioselective Synthesis of Cyclopropanes.
Sun, Gui-Jun; Gong, Jun; Kang, Qiang; The Journal of organic chemistry 82 (2017) 796–803; doi:10.1021/acs.joc.6b02583

data_4032207
_publ_section_title
;
 Chiral Rhodium(III) Complex-Catalyzed Cascade Michael-Alkylation
 Reactions: Enantioselective Synthesis of Cyclopropanes.
;
_journal_issue                   1
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              796
_journal_page_last               803
_journal_paper_doi               10.1021/acs.joc.6b02583
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C41 H37.5 B F10 N4.5 O2 Rh'
_chemical_formula_weight         928.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 118.298(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2276(4)
_cell_length_b                   13.4508(3)
_cell_length_c                   13.5559(4)
_cell_measurement_reflns_used    5203
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3630
_cell_measurement_theta_min      4.9140
_cell_volume                     2123.65(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.5594
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8678
_diffrn_reflns_point_group_measured_fraction_full 0.649
_diffrn_reflns_point_group_measured_fraction_max 0.621
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.549
_diffrn_reflns_theta_min         3.703
_exptl_absorpt_coefficient_mu    3.995
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       prism
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Flack x determined using 1134 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         5316
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0559P)^2^+0.8090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.294
_reflns_Friedel_fraction_full    0.322
_reflns_Friedel_fraction_max     0.295
_reflns_number_gt                5133
_reflns_number_total             5316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b02583_si_003.cif
_cod_data_source_block           Rh-3
_cod_original_cell_volume        2123.65(12)
_cod_original_formula_sum        'C41 H37.50 B F10 N4.50 O2 Rh'
_cod_database_code               4032207
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.586
_shelx_estimated_absorpt_t_max   0.741
_oxdiff_exptl_absorpt_empirical_full_min 0.807
_oxdiff_exptl_absorpt_empirical_full_max 1.351
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              36850
_shelx_hkl_checksum              56107