Rh-catalyzed chemodivergent [4+1]-annulation/allylation of sulfoxonium ylides with α-methylene-β-lactones: access to α-indanonyl/α-benzyl acrylates
Samantaray, Swati; Saha, Sharajit; Punniyamurthy, Tharmalingam; Chemical Communications  (2026) –; doi:10.1039/D5CC05716G

data_7135280
_publ_section_title
;
 Rh-catalyzed chemodivergent [4+1]-annulation/allylation of sulfoxonium
 ylides with \a-methylene-\b-lactones: access to \a-indanonyl/\a-benzyl
 acrylates
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D5CC05716G
_journal_year                    2026
_chemical_formula_moiety         'C17 H18 O3'
_chemical_formula_sum            'C17 H18 O3'
_chemical_formula_weight         270.31
_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     iterative
_audit_creation_date             2025-01-29
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2025-01-30 deposited with the CCDC.	2025-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                93.006(2)
_cell_angle_beta                 108.3900(10)
_cell_angle_gamma                93.186(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4589(6)
_cell_length_b                   9.2758(6)
_cell_length_c                   9.7016(6)
_cell_measurement_reflns_used    8781
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.311
_cell_measurement_theta_min      2.205
_cell_volume                     719.26(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      295.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16608
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.340
_diffrn_reflns_theta_min         2.205
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             288
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.7043
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0612
_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^)+(0.0572P)^2^+0.4006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2136
_reflns_number_total             2611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05716g2.cif
_cod_data_source_block           SS_450_0ma_a
_cod_database_code               7135280
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C13(H13A,H13B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C15(H15), C16(H16), C17(H17)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              91691
_olex2_submission_special_instructions 'No special instructions were received'