Synthesis of Spirocyclic Diarylfluorenes by One-Pot Twofold SNAr Reactions of Diaryl Sulfones with Diarylmethanes.
Bhanuchandra, M.; Yorimitsu, Hideki; Osuka, Atsuhiro; Organic letters 18 (2016) 384–387; doi:10.1021/acs.orglett.5b03384

data_1542668
_publ_section_title
;
 Synthesis of Spirocyclic Diarylfluorenes by One-Pot Twofold SNAr
 Reactions of Diaryl Sulfones with Diarylmethanes.
;
_journal_issue                   3
_journal_name_full               'Organic letters'
_journal_page_first              384
_journal_page_last               387
_journal_paper_doi               10.1021/acs.orglett.5b03384
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C42 H32 S'
_chemical_formula_sum            'C42 H32 S'
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_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                108.620(6)
_cell_angle_beta                 98.945(7)
_cell_angle_gamma                90.295(5)
_cell_formula_units_Z            4
_cell_length_a                   8.3170(15)
_cell_length_b                   16.040(3)
_cell_length_c                   23.373(5)
_cell_measurement_reflns_used    2954
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      25.3
_cell_volume                     2913.9(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_unetI/netI     0.0266
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_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
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_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.361
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_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.200
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_refine_diff_density_max         1.120
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         10295
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0850P)^2^+2.7269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1467
_refine_ls_wR_factor_ref         0.1513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8873
_reflns_number_total             10295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5b03384_si_003.cif
_cod_data_source_block           f2plus
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

2019-01-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C42 H32 S)'
_cod_original_formula_sum        'C84 H64 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1137.47
_cod_database_code               1542668
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.795
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              40104
_shelx_hkl_checksum              41174