Synthesis of Divergent Benzo[ b]fluorenones through Cycloaromatization Reactions of 1,5-Enynols and 1,5-Diynols.
Yan, Bingyu; Fu, Yang; Zhu, Hui; Chen, Zhiyuan; The Journal of organic chemistry 84 (2019) 4246–4262; doi:10.1021/acs.joc.9b00231

data_4034232
_publ_section_title
;
 Synthesis of Divergent Benzo[ b]fluorenones through Cycloaromatization
 Reactions of 1,5-Enynols and 1,5-Diynols.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              4246
_journal_page_last               4262
_journal_paper_doi               10.1021/acs.joc.9b00231
_journal_volume                  84
_journal_year                    2019
_chemical_formula_sum            'C31 H21 F O2'
_chemical_formula_weight         444.48
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_symmetry_cell_setting           triclinic
_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                108.113(2)
_cell_angle_beta                 90.803(2)
_cell_angle_gamma                96.502(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6236(14)
_cell_length_b                   11.458(2)
_cell_length_c                   14.056(3)
_cell_measurement_reflns_used    3455
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.69
_cell_volume                     1157.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_sigmaI/netI    0.0289
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_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
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_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9850
_exptl_absorpt_correction_T_min  0.9785
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.306
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_refine_ls_number_parameters     309
_refine_ls_number_reflns         5220
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_refine_ls_R_factor_all          0.0847
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_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0930P)^2^+0.0411P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1680
_reflns_number_gt                3404
_reflns_number_total             5220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo9b00231_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1157.8(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4034232