Trichalcogenasumanenes containing various chalcogen atoms: synthesis, structure, properties, and chemical reactivity
Wang, Shitao; Shang, Jihai; Yan, Chaoxian; Wang, Wenbo; Yuan, Chengshan; Zhang, Hao-Li; Shao, Xiangfeng; Organic Chemistry Frontiers 6 (2019) 263–; doi:10.1039/C8QO01220B

data_1554542
_publ_section_title
;
 Trichalcogenasumanenes containing various chalcogen atoms: synthesis,
 structure, properties, and chemical reactivity
;
_journal_issue                   2
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              263
_journal_paper_doi               10.1039/C8QO01220B
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C42 H54 O6 S2 Se'
_chemical_formula_sum            'C42 H54 O6 S2 Se'
_chemical_formula_weight         797.93
_chemical_melting_point          419
_chemical_name_common            2S1Se
_chemical_name_systematic        2S1Se
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-09-14 deposited with the CCDC.
2018-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                86.466(5)
_cell_angle_beta                 83.674(5)
_cell_angle_gamma                83.298(5)
_cell_formula_units_Z            8
_cell_length_a                   14.2625(6)
_cell_length_b                   18.0213(12)
_cell_length_c                   31.3062(19)
_cell_measurement_reflns_used    2197
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      18.1050
_cell_measurement_theta_min      3.6940
_cell_volume                     7933.2(8)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    Mercury
_computing_publication_material  Mercury
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      173(1)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2024
_diffrn_reflns_av_unetI/netI     0.4495
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            72965
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.570
_diffrn_reflns_theta_min         3.241
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.033
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1861
_refine_ls_number_reflns         35946
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.3577
_refine_ls_R_factor_gt           0.1279
_refine_ls_shift/su_max          3.607
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0697P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.3316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9760
_reflns_number_total             35946
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qo01220b2.cif
_cod_data_source_block           2S1Se
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               1554542
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.79939
_shelx_estimated_absorpt_t_max   1.00000
_shelx_res_checksum              52128
_shelx_hkl_checksum              2972