Time-dependent Rh(III)-catalyzed chemodivergent reactions of 2-pyridylthiophenes with nitroalkenes.
Wang, Cheng; Zhang, Qiang; Qin, Sisi; Lai, Zhimin; Liang, Taoyuan; Huang, Guan; Zhao, Shuangliang; Zhang, Zhuan; Chemical communications (Cambridge, England) 62 (2026) 1614–1617; doi:10.1039/d5cc06419h

data_7135503
_publ_section_title
;
 Time-dependent Rh(III)-catalyzed chemodivergent reactions of
 2-pyridylthiophenes with nitroalkenes.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1614
_journal_page_last               1617
_journal_paper_doi               10.1039/d5cc06419h
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C17 H13 F N2 O2 S'
_chemical_formula_sum            'C17 H13 F N2 O2 S'
_chemical_formula_weight         328.35
_chemical_name_systematic        844
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-08-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-08-04 deposited with the CCDC.	2025-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                103.401(5)
_cell_angle_beta                 106.506(5)
_cell_angle_gamma                98.916(5)
_cell_formula_units_Z            4
_cell_length_a                   9.8276(5)
_cell_length_b                   11.1008(7)
_cell_length_c                   15.5044(8)
_cell_measurement_reflns_used    3886
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.5140
_cell_measurement_theta_min      4.0800
_cell_volume                     1532.72(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0606
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.838
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      0.00  83.00   1.00    2.50    --   15.65  38.00  60.00   83
  2  \w     55.00  87.00   1.00    2.50    --   15.65  19.00 150.00   32
  3  \w     -2.00  23.00   1.00    2.50    --   15.65  19.00 150.00   25
  4  \w    -25.00  16.00   1.00    2.50    --  -16.59 -99.00  60.00   41
  5  \w    -53.00  -5.00   1.00    2.50    --   15.65 -19.00-120.00   48
  6  \w      5.00  40.00   1.00    2.50    --   15.65 -19.00-120.00   35
  7  \w    -14.00  19.00   1.00    2.50    --  -16.59 -99.00-120.00   33
  8  \w     -4.00  65.00   1.00    2.50    --   15.65-124.00-127.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0514176000
_diffrn_orient_matrix_UB_12      0.0538303000
_diffrn_orient_matrix_UB_13      0.0018955000
_diffrn_orient_matrix_UB_21      -0.0188659000
_diffrn_orient_matrix_UB_22      -0.0209969000
_diffrn_orient_matrix_UB_23      -0.0496252000
_diffrn_orient_matrix_UB_31      -0.0548030000
_diffrn_orient_matrix_UB_32      0.0351024000
_diffrn_orient_matrix_UB_33      -0.0046202000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12313
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.254
_diffrn_reflns_theta_min         3.726
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80443
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0455P)^2^+0.5614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4873
_reflns_number_total             6999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06419h2.cif
_cod_data_source_block           exp_12957
_cod_original_cell_volume        1532.72(16)
_cod_database_code               7135503
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.933
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9AA(H9AA), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C0BA(H0BA,H0BB)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C6BA(H6BA), C13(H13), C0AA(H0AA), C8(H8), C2BA(H2BA), C7AA(H7AA),
 C5BA(H5BA), C4(H4), C15(H15), C4BA(H4BA), C16(H16), C9(H9), C8AA(H8AA),
 C14(H14), C3AA(H3AA), C3(H3), C3BA(H3BA), C1(H1), C2AA(H2AA)
;
_shelx_res_checksum              81691
_shelx_hkl_checksum              73651
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.316
_oxdiff_exptl_absorpt_empirical_full_min 0.657