Cyclopenta[b]thiopyran and Cyclopenta[b]selenopyran Based Heteroarenes: Electronic Communication Between S- and/or Se-Fused Aromatics
Qiao, Yanjun; Lu, Yifan; Chen, Weinan; Chen, Yijing; Baumgarten, Martin; Zhou, Gang; Chemical Communications  (2019) –; doi:10.1039/C9CC01761E

data_7123267
_publ_section_title
;
 Cyclopenta[b]thiopyran and Cyclopenta[b]selenopyran Based Heteroarenes:
 Electronic Communication Between S- and/or Se-Fused Aromatics
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC01761E
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         ' C38 H44 S Se'
_chemical_formula_sum            'C38 H44 S Se'
_chemical_formula_weight         611.75
_chemical_name_common            QYJ-2
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-01-13 deposited with the CCDC.    2019-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                78.0360(10)
_cell_angle_beta                 87.3050(10)
_cell_angle_gamma                80.3540(10)
_cell_formula_units_Z            1
_cell_length_a                   4.9067(2)
_cell_length_b                   9.2799(3)
_cell_length_c                   17.3392(6)
_cell_measurement_reflns_used    8259
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.55
_cell_measurement_theta_min      2.61
_cell_volume                     761.39(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14459
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        66.651
_diffrn_reflns_theta_max         66.651
_diffrn_reflns_theta_min         2.605
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.484
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark Green'
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             322
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.930
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.456
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5191
_refine_ls_number_restraints     350
_refine_ls_restrained_S_all      1.435
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.1062
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3024
_refine_ls_wR_factor_ref         0.3353
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4240
_reflns_number_total             5191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc01761e2.cif
_cod_data_source_block           b_0m_b
_cod_original_formula_sum        ' C38 H44 S Se'
_cod_database_code               7123267
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              97157