Enantiopure Aromatic Saddles Bearing the Fenestrindane Core.
Wong, Wai-Shing; Tse, Ho-Wing; Cheung, Enoch; Kuck, Dietmar; Chow, Hak-Fun; The Journal of organic chemistry 84 (2019) 869–878; doi:10.1021/acs.joc.8b02719

data_4036008
_publ_section_title
;
 Enantiopure Aromatic Saddles Bearing the Fenestrindane Core.
;
_journal_issue                   2
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              869
_journal_page_last               878
_journal_paper_doi               10.1021/acs.joc.8b02719
_journal_volume                  84
_journal_year                    2019
_chemical_formula_sum            'C30 H26 Br2 O5'
_chemical_formula_weight         626.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 102.2757(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.3754(3)
_cell_length_b                   19.0360(9)
_cell_length_c                   10.9599(6)
_cell_measurement_reflns_used    394
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     1299.70(11)
_computing_cell_refinement       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_collection       'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_data_reduction        'BRUKER D8VENTURE DIFFRACTOMETER'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'BRUKER D8VENTURE DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEGA SCAN'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32835
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.913
_diffrn_reflns_theta_min         2.863
_exptl_absorpt_coefficient_mu    3.158
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4372
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 2433 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.038(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6150
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.4082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                5519
_reflns_number_total             6150
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b02719_si_002.cif
_cod_data_source_block           dibromofenestranone
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4036008
_shelx_estimated_absorpt_t_min   0.301
_shelx_estimated_absorpt_t_max   0.451
_shelxl_version_number           2014/6
_shelx_res_checksum              6485
_shelx_hkl_checksum              27202