Toward Soluble 5,10-Diheterotruxenes: Synthesis and Reactivity of 5,10-Dioxatruxenes, 5,10-Dithiatruxenes, and 5,10-Diazatruxenes.
Górski, Krzysztof; Mech-Piskorz, Justyna; Leśniewska, Barbara; Pietraszkiewicz, Oksana; Pietraszkiewicz, Marek; The Journal of organic chemistry 85 (2020) 4672–4681; doi:10.1021/acs.joc.9b03387

data_4038135
_publ_section_title
;
 Toward Soluble 5,10-Diheterotruxenes: Synthesis and Reactivity of
 5,10-Dioxatruxenes, 5,10-Dithiatruxenes, and 5,10-Diazatruxenes.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              4672
_journal_page_last               4681
_journal_paper_doi               10.1021/acs.joc.9b03387
_journal_volume                  85
_journal_year                    2020
_chemical_formula_moiety         '2(C29 H24 N2), C3 H6 O'
_chemical_formula_sum            'C61 H54 N4 O'
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_space_group_name_Hall           'I -4'
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_a                   28.0572(4)
_cell_length_b                   28.0572(4)
_cell_length_c                   5.2734(1)
_cell_measurement_reflns_used    6042
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      69.7540
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_cell_volume                     4151.25(11)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -25
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_diffrn_reflns_limit_l_min       -6
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_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.026
_diffrn_reflns_theta_min         2.227
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       needle
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 1529 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         3817
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0962P)^2^+1.1315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.741
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                3718
_reflns_number_total             3817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b03387_si_001.cif
_cod_data_source_block           kg_net_net_c_aceton_2
_cod_depositor_comments
'Adding full bibliography for 4038128--4038135.cif.'
_cod_original_cell_volume        4151.26(14)
_cod_database_code               4038135
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.885
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              6095
_shelx_hkl_checksum              52426