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_4034488
_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 O S'
_chemical_formula_sum            'C34 H32 O S'
_chemical_formula_weight         488.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.4446(2)
_cell_length_b                   16.2063(2)
_cell_length_c                   21.8323(3)
_cell_measurement_reflns_used    8167
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      71.8130
_cell_measurement_theta_min      4.5580
_cell_volume                     5110.80(12)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0231
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15893
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.566
_diffrn_reflns_theta_max         66.566
_diffrn_reflns_theta_min         6.128
_exptl_absorpt_coefficient_mu    1.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39825
_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    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.373
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4489
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0659P)^2^+11.2591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4288
_reflns_number_total             4489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b01397_si_002.cif
_cod_data_source_block           jmp_so_3
_cod_database_code               4034488
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.736
_shelx_estimated_absorpt_t_max   0.828
_shelx_res_checksum              99392
_shelx_hkl_checksum              21281