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_7116425
_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_moiety         '3(C35 H42 N5 O2 Rh), C4 H8 O'
_chemical_formula_sum            'C109 H134 N15 O7 Rh3'
_chemical_formula_weight         2075.03
_chemical_name_systematic        Compound3b
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2014-08-07 deposited with the CCDC.
2014-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0110(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7612(5)
_cell_length_b                   21.6015(5)
_cell_length_c                   23.3468(5)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.98
_cell_measurement_theta_min      2.19
_cell_volume                     10974.7(4)
_computing_cell_refinement       'SAINT, Bruker 2012'
_computing_data_collection       'APEX2, Bruker 2012'
_computing_data_reduction        'SAINT, Bruker 2012'
_computing_molecular_graphics    'Mercury 3.3, CCDC 2013'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'AUTOSTRUCTURE, Bruker 2012'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SMART APEX II Duo'
_diffrn_measurement_method       '\w/\p scans'
_diffrn_radiation_monochromator  'Quazar MX'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            262129
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.067
_diffrn_reflns_theta_min         1.589
_diffrn_source                   'Incoatec I\muS Microsource'
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1, Bruker 2012'
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             4336
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane, thf'
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.127
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.9188
_refine_diff_density_max         2.151
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1288
_refine_ls_number_reflns         19427
_refine_ls_number_restraints     1333
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0606P)^2^+31.3792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14852
_reflns_number_total             19427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc07154a2a.cif
_cod_data_source_block           compound3b
_cod_database_code               7116425
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.939
_shelxl_version_number           2014/6
_shelx_res_checksum              72515
_shelx_fab_checksum              21283