Csp3-Csp3 and Csp3-H Bond Activation of 1,1-Disubstituted Cyclopentane
Chisato Mukai; Yuu Ohta; Yuki Oura; Yasuaki Kawaguchi; Fuyuhiko Inagaki; Journal of the American Chemical Society 134 (2012) 19580–19583; doi:10.1021/ja309830p

data_4118956
_publ_contact_author_address
;Division of Pharmaceutical Sciences, Graduate School of Medical Sciences
Kanazawa University
Kakuma-machi
Kanazawa
920-1192 Japan
;
_publ_contact_author_email       mukai@p.kanazawa-u.ac.jp
_publ_contact_author_fax         (+81)76-234-4410
_publ_contact_author_name        'Professor Chisato Mukai'
_publ_contact_author_phone       (+81)76-234-4411
_publ_section_title
;
 Csp3-Csp3 and Csp3-H Bond Activation of 1,1-Disubstituted Cyclopentane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19580
_journal_page_last               19583
_journal_paper_doi               10.1021/ja309830p
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C36 H34 N2 O10 S'
_chemical_formula_sum            'C36 H34 N2 O10 S'
_chemical_formula_weight         686.73
_chemical_melting_point          467
_chemical_name_systematic
;11,11-Bis(p-nitrobenzoyloxymethyl)-3-methyl-13-
phenylsulfonylbicyclo[7.4.0]trideca-1(13),2,8-triene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-09-10
_audit_creation_method           'by CrystalStructure 4.0'
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.491(10)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   6.523(3)
_cell_length_b                   18.230(8)
_cell_length_c                   28.472(11)
_cell_measurement_reflns_used    6871
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.09
_cell_volume                     3370(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0935
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            29415
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_source                   'seald x-ray tube'
_diffrn_source_type              'R-AXIS RAPID'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1440.00
_exptl_crystal_recrystallization_method benzene-hexane
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     445
_refine_ls_number_reflns         7637
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0737
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1126P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2457
_reflns_number_gt                3120
_reflns_number_total             7637
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja309830p_si_002.cif
_cod_data_source_block           seimitsu28-3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4118956