Metalloradical-Catalyzed Aliphatic Carbon-Carbon Activation of Cyclooctane
Yun Wai Chan; Kin Shing Chan; Journal of the American Chemical Society 132 (2010) 6920–6922; doi:10.1021/ja101586w

data_4102432
_publ_section_title
;
 Metalloradical-Catalyzed Aliphatic Carbon-Carbon Activation of
 Cyclooctane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6920
_journal_page_last               6922
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C56 H53 N4 Rh'
_chemical_formula_weight         884.93
_chemical_name_systematic
; 
 ? 
;
_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                65.745(4)
_cell_angle_beta                 77.764(4)
_cell_angle_gamma                82.348(4)
_cell_formula_units_Z            2
_cell_length_a                   10.578(2)
_cell_length_b                   14.574(3)
_cell_length_c                   16.226(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2225.9(8)
_computing_cell_refinement       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_collection       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_reduction        'BRUKER SMART CCD DIFFRACTOMETER'
_computing_molecular_graphics    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'BRUKER SMART CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12098
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.616130
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7803
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0631P)^2^+1.7635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                6645
_reflns_number_total             7803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja101586w_si_001.cif
_cod_data_source_block           YWC467.1
_cod_original_cell_volume        2225.8(9)
_cod_database_code               4102432
_cod_depositor_comments
;
Adding numbers of non-modelled hydrogens to _atom_site_attached_hydrogens
values.

Andrius Merkys
2015-09-15
;
_journal_paper_doi 10.1021/ja101586w