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_1544980
_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         'C24 H19 Br O6'
_chemical_formula_sum            'C24 H19 Br O6'
_chemical_formula_weight         483.30
_chemical_melting_point          289.0(10)
_chemical_name_common
(7aR*,12bS*)-6-Bromo-5,12b-dihydroxy-4,13-dimethoxy-7a-methyl-7H-naphth[2,1:b]fluolene-8,13-dione
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.6981(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3377(2)
_cell_length_b                   7.86830(10)
_cell_length_c                   16.5282(3)
_cell_measurement_reflns_used    3647
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.01
_cell_volume                     1959.98(5)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16608
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    2.139
_exptl_absorpt_correction_T_max  0.8145
_exptl_absorpt_correction_T_min  0.6743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998) Private communication
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         3647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.8431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                3375
_reflns_number_total             3647
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b03541_si_003.cif
_cod_data_source_block           kk034
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '288-290' was changed to '289.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 1544980--1544981.cif.
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               1544980