Synthesis and Reactivity of 5-Heterotruxenes Containing Sulfur or Nitrogen as the Heteroatom.
Górski, Krzysztof; Mech-Piskorz, Justyna; Leśniewska, Barbara; Pietraszkiewicz, Oksana; Pietraszkiewicz, Marek; The Journal of organic chemistry 84 (2019) 11553–11561; doi:10.1021/acs.joc.9b01397

data_4034487
_publ_section_title
;
 Synthesis and Reactivity of 5-Heterotruxenes Containing Sulfur or
 Nitrogen as the Heteroatom.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11553
_journal_page_last               11561
_journal_paper_doi               10.1021/acs.joc.9b01397
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C34 H32 S'
_chemical_formula_sum            'C34 H32 S'
_chemical_formula_weight         472.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90.0
_cell_angle_beta                 95.052(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   17.2366(3)
_cell_length_b                   7.2333(1)
_cell_length_c                   41.0092(8)
_cell_measurement_reflns_used    8914
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      69.8886
_cell_measurement_theta_min      3.2107
_cell_volume                     5093.06(15)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      99.9(2)
_diffrn_detector_area_resol_mean 16.2974
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            19542
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         6.204
_exptl_absorpt_coefficient_mu    1.264
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21b (release 03-02-2012 CrysAlis171 .NET)
(compiled Feb  3 2012,10:37:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       needles
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         8974
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0354P)^2^+34.2751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1930
_refine_ls_wR_factor_ref         0.1957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7872
_reflns_number_total             8974
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b01397_si_004.cif
_cod_data_source_block           JM_Cu_2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4034487
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.518
_shelx_estimated_absorpt_t_max   0.884
_shelx_res_checksum              54367
_shelx_hkl_checksum              34805