C‒H Activation Induced by Oxidative Addition of N‒O Bonds in Oxime Esters: Formation of Rhodacycles and Cycloaddition with Alkynes
Shimbayashi, Takuya; Okamoto, Kazuhiro; Ohe, Kouichi; Organometallics 35 (2016) 2026–; doi:10.1021/acs.organomet.6b00311

data_4088695
_publ_section_title
;
 C--H Activation Induced by Oxidative Addition of N--O Bonds in Oxime
 Esters: Formation of Rhodacycles and Cycloaddition with Alkynes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2026
_journal_paper_doi               10.1021/acs.organomet.6b00311
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C79 H75 Cl2 N P2 Rh'
_chemical_formula_sum            'C79 H75 Cl2 N P2 Rh'
_chemical_formula_weight         1274.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                106.500(4)
_cell_angle_beta                 94.464(3)
_cell_angle_gamma                109.530(6)
_cell_formula_units_Z            2
_cell_length_a                   13.788(6)
_cell_length_b                   14.476(6)
_cell_length_c                   18.584(7)
_cell_measurement_reflns_used    8147
_cell_measurement_temperature    143
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.07
_cell_volume                     3290(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      143
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27071
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.519
_diffrn_reflns_theta_min         3.066
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1330.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.80
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     766
_refine_ls_number_reflns         14498
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.2925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9649
_reflns_number_total             14498
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om6b00311_si_002.cif
_cod_data_source_block           3
_cod_database_code               4088695
_shelxl_version_number           2014-3
_shelx_res_checksum              44836
_shelx_hkl_checksum              48088