Synthesis and Reactivity of Bicyclo[3.2.1]octanoid-Derived Cyclopropanes
John R. Goodell; Jennifer L. Poole; Aaron B. Beeler; Jeffrey Aubé; John A. Porco; Journal of Organic Chemistry 76 (2011) 9792–9800; doi:10.1021/jo2018922

data_4026776
_publ_section_title
;
 Synthesis and Reactivity of Bicyclo[3.2.1]octanoid-Derived Cyclopropanes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9792
_journal_page_last               9800
_journal_paper_doi               10.1021/jo2018922
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C26 H26 Br N O4'
_chemical_formula_weight         496.39
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                72.210(7)
_cell_angle_beta                 86.597(8)
_cell_angle_gamma                76.128(8)
_cell_formula_units_Z            2
_cell_length_a                   7.867(4)
_cell_length_b                   11.447(6)
_cell_length_c                   13.759(7)
_cell_measurement_reflns_used    6012
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.959
_cell_measurement_theta_min      2.667
_cell_volume                     1145.3(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0858
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10050
_diffrn_reflns_theta_full        29.06
_diffrn_reflns_theta_max         29.06
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        0.00
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       'Rectangular parallelepiped'
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0485
_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^)+(0.1086P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                4587
_reflns_number_total             5356
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2018922_si_003.cif
_cod_data_source_block           compound41
_cod_original_cell_volume        1145.2(10)
_cod_database_code               4026776