Selective rearrangement of terminal epoxides into methylketones catalysed by a nucleophilic rhodium-NHC-pincer complex
Eva Jurgens; Barbara Wucher; Frank Rominger; Karl W. Tornroos; Doris Kunz; Chem.Commun. 51 (2015) 1897–; doi:10.1039/C4cc07154A

data_7116424
_publ_section_title
;
 Selective rearrangement of terminal epoxides into methylketones catalysed
 by a nucleophilic rhodium-NHC-pincer complex
;
_journal_name_full               Chem.Commun.
_journal_page_first              1897
_journal_paper_doi               10.1039/C4cc07154A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C40.67 H53.33 N5 O4.17 Rh'
_chemical_formula_weight         781.79
_chemical_name_systematic        Compound3a
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-08-07 deposited with the CCDC.
2014-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   34.6494(7)
_cell_length_b                   34.6494(7)
_cell_length_c                   16.6624(4)
_cell_measurement_temperature    200(2)
_cell_volume                     17324.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.675
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1525
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_Laue_measured_fraction_full 0.675
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37533
_diffrn_reflns_point_group_measured_fraction_full 0.675
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         21.973
_diffrn_reflns_theta_min         1.826
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  0.9574
_exptl_absorpt_correction_T_min  0.5959
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             7392
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.103
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         4695
_refine_ls_number_restraints     901
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.1148
_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^)+(0.0001P)^2^+844.2532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2441
_refine_ls_wR_factor_ref         0.2580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3575
_reflns_number_total             4695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc07154a2a.cif
_cod_data_source_block           compound3a
_cod_original_cell_volume        17324.4(8)
_cod_database_code               7116424
_shelx_estimated_absorpt_t_min   0.895
_shelx_estimated_absorpt_t_max   0.953
_shelxl_version_number           2014-3
_shelx_res_checksum              71309