Highlycis-Selective Rh(I)-Catalyzed Cyclopropanation Reactions
Marianne Lenes Rosenberg; Klára Vlašaná; Nalinava Sen Gupta; David Wragg; Mats Tilset; Journal of Organic Chemistry 76 (2011) 2465–2470; doi:10.1021/jo102140z

data_4026181
_publ_section_title
;
 Highlycis-Selective Rh(I)-Catalyzed Cyclopropanation Reactions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2465
_journal_page_last               2470
_journal_paper_doi               10.1021/jo102140z
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C32 H12 B F24, C26 H27 N3 Rh'
_chemical_formula_sum            'C58 H39 B F24 N3 Rh'
_chemical_formula_weight         1347.64
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.355(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.846(3)
_cell_length_b                   16.285(3)
_cell_length_c                   18.584(5)
_cell_measurement_reflns_used    3860
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20.11
_cell_measurement_theta_min      2.16
_cell_volume                     5703(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond (Crystal impact, 2009)'
_computing_publication_material  'Platon (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.752
_diffrn_measured_fraction_theta_max 0.752
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_sigmaI/netI    0.1324
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10560
_diffrn_reflns_theta_full        22.78
_diffrn_reflns_theta_max         22.78
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Sheldrick, 2004'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       plate
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         3027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1442P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2099
_refine_ls_wR_factor_ref         0.2361
_reflns_number_gt                1664
_reflns_number_total             3027
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo102140z_si_001.cif
_cod_data_source_block           addsym1
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