Rhodium-catalyzed intramolecular cyclization for synthesizing thiodihydropyrans.
Wang, Yunxiao; Xu, Ze-Feng; Chen, Jing; Yu, Mingming; Guo, Sheng-Rong; Li, Chuan-Ying; Organic & biomolecular chemistry 22 (2024) 6695–6698; doi:10.1039/d4ob01150c

data_7160084
_publ_section_title
;
 Rhodium-catalyzed intramolecular cyclization for synthesizing
 thiodihydropyrans.
;
_journal_issue                   33
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6695
_journal_page_last               6698
_journal_paper_doi               10.1039/d4ob01150c
_journal_volume                  22
_journal_year                    2024
_chemical_formula_sum            'C40 H42 N2 O6 S4'
_chemical_formula_weight         774.99
_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
;
2024-07-30 deposited with the CCDC.	2024-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.111(3)
_cell_length_b                   11.691(4)
_cell_length_c                   20.374(7)
_cell_measurement_reflns_used    640
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.58
_cell_measurement_theta_min      2.41
_cell_volume                     1932.0(12)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.648
_diffrn_measured_fraction_theta_max 0.685
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_Laue_measured_fraction_full 0.648
_diffrn_reflns_Laue_measured_fraction_max 0.685
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8271
_diffrn_reflns_point_group_measured_fraction_full 0.648
_diffrn_reflns_point_group_measured_fraction_max 0.685
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         0.999
_exptl_absorpt_coefficient_mu    0.295
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3241
_reflns_number_total             6120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ob01150c2.cif
_cod_data_source_block           WYX3136_0m_a
_cod_depositor_comments          'Adding full bibliography for 7160084.cif.'
_cod_original_cell_volume        1931.9(12)
_cod_database_code               7160084
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              68465