Rh-Catalyzed Intermolecular Reactions of Cyclic α-Diazocarbonyl Compounds with Selectivity over Tertiary C-H Bond Migration
Andrew DeAngelis; Olga Dmitrenko; Joseph M. Fox; Journal of the American Chemical Society 134 (2012) 11035–11043; doi:10.1021/ja3046712

data_4118198
_publ_section_title
;
 Rh-Catalyzed Intermolecular Reactions of Cyclic \a-Diazocarbonyl
 Compounds with Selectivity over Tertiary C-H Bond Migration
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11035
_journal_page_last               11043
_journal_paper_doi               10.1021/ja3046712
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C48 H96 O10 Rh2'
_chemical_formula_weight         1039.07
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.342(3)
_cell_angle_beta                 81.058(3)
_cell_angle_gamma                65.693(3)
_cell_formula_units_Z            2
_cell_length_a                   11.214(2)
_cell_length_b                   12.161(2)
_cell_length_c                   21.670(4)
_cell_measurement_reflns_used    1020
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      23.59
_cell_measurement_theta_min      2.35
_cell_volume                     2660.0(8)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_sigmaI/netI    0.0863
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35053
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.9354
_exptl_absorpt_correction_T_min  0.8126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       plate
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.317
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         13208
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                9405
_reflns_number_total             13208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3046712_si_005.cif
_cod_data_source_block           joef100
_cod_original_cell_volume        2660.1(8)
_cod_database_code               4118198