Skeletal Rearrangements of Polycyclic α-Ketols.
Kawamura, Moe; Kamo, Shogo; Azuma, Shuhei; Kubo, Konomi; Sasamori, Takahiro; Tokitoh, Norihiro; Kuramochi, Kouji; Tsubaki, Kazunori; Organic letters 19 (2017) 301–303; doi:10.1021/acs.orglett.6b03541

data_1544981
_publ_section_title
;
 Skeletal Rearrangements of Polycyclic \a-Ketols.
;
_journal_issue                   2
_journal_name_full               'Organic letters'
_journal_page_first              301
_journal_page_last               303
_journal_paper_doi               10.1021/acs.orglett.6b03541
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C22 H13 Br O3'
_chemical_formula_sum            'C22 H13 Br O3'
_chemical_formula_weight         405.23
_chemical_melting_point          205
_chemical_name_common
6-Bromo-7a-methyl-7,7a-dihydro-5H-dibenzo[b,g]fluorene-5,8,13-trione
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                75.761(3)
_cell_angle_beta                 75.876(5)
_cell_angle_gamma                79.427(5)
_cell_formula_units_Z            2
_cell_length_a                   6.9248(4)
_cell_length_b                   10.1578(6)
_cell_length_c                   12.5321(6)
_cell_measurement_reflns_used    2958
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.09
_cell_volume                     821.43(8)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_publication_material  'Yadokari-XG 2011 (Wakita,Nemoto et al., 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6202
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    2.522
_exptl_absorpt_correction_T_max  0.6324
_exptl_absorpt_correction_T_min  0.4722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 MULABS - Empirical Correction for Absorption Anisotropy.
 Blessing, R. H., Acta Cryst., A51, 33-38 (1995).
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.340
_refine_diff_density_min         -1.349
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         2958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0927P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1190
_reflns_number_gt                2765
_reflns_number_total             2958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b03541_si_002.cif
_cod_data_source_block           kk85a
_cod_depositor_comments
'Adding full bibliography for 1544980--1544981.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1544981