Additive-controlled chemodivergent multi-component domino reaction between salicylaldehydes and Morita-Baylis-Hillman (MBH) carbonates.
Dan Xu, ?; Li, Xiaoxuan; Cai, Yifei; Chen, Yushuang; Xin, Yu; Chen, Jing; Yao, Hui; Huang, Nianyu; Wang, Nengzhong; Chemical communications (Cambridge, England) 61 (2025) 15433–15436; doi:10.1039/d5cc04624f

data_7134919
_publ_section_title
;
 Additive-controlled chemodivergent multi-component domino reaction
 between salicylaldehydes and Morita-Baylis-Hillman (MBH) carbonates.
;
_journal_issue                   79
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15433
_journal_page_last               15436
_journal_paper_doi               10.1039/d5cc04624f
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C26 H26 Cl2 O6'
_chemical_formula_sum            'C26 H26 Cl2 O6'
_chemical_formula_weight         505.37
_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             2024-01-07
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-06-11 deposited with the CCDC.	2025-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                72.926(2)
_cell_angle_beta                 87.247(3)
_cell_angle_gamma                81.392(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5461(3)
_cell_length_b                   11.5957(4)
_cell_length_c                   13.2007(3)
_cell_measurement_reflns_used    9053
_cell_measurement_temperature    99.97(18)
_cell_measurement_theta_max      73.8880
_cell_measurement_theta_min      4.0590
_cell_volume                     1236.41(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(18)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.957
_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    -33.00  17.00   0.50    0.50    --    0.00 -82.00 -30.00  100
  2  \w    -18.00  29.00   0.50    0.50    --    0.00 -77.00-180.00   94
  3  \w    -45.00  -9.00   0.50    0.50    --    0.00 -77.00   0.00   72
  4  \w    -27.00  31.00   0.50    0.50    --    0.00 -82.00  90.00  116
  5  \w    -45.00  11.00   0.50    0.50    --    0.00 -77.00-120.00  112
  6  \w     60.00 126.00   0.50    0.50    --   95.80 -82.00-120.00  132
  7  \w     27.00 119.00   0.50    0.50    --   95.80 -61.00   0.00  184
  8  \w      6.00 119.00   0.50    0.50    --   95.80 -61.00 150.00  226
  9  \w     50.00 116.00   0.50    0.50    --   95.80 -15.00 -30.00  132
 10  \w     35.00 127.00   0.50    0.50    --   95.80 -82.00 150.00  184
 11  \w     25.00  94.00   0.50    0.50    --   95.80 -30.00-120.00  138
 12  \w      6.00  96.00   0.50    0.50    --   95.80 -77.00 -60.00  180
 13  \w     12.00  37.00   0.50    0.50    --   95.80 -82.00  90.00   50
 14  \w     61.00 104.00   0.50    0.50    --   95.80 -82.00  90.00   86
 15  \w    109.00 141.00   0.50    0.50    --   95.80  30.00 -30.00   64
 16  \w      6.00 127.00   0.50    0.50    --   95.80 -82.00   0.00  242
 17  \w    133.00 185.00   0.50    0.50    --   95.80  15.00-180.00  104
 18  \w     72.00 165.00   0.50    0.50    --   95.80  61.00 150.00  186
 19  \w     75.00 181.00   0.50    0.50    --   95.80  15.00 -90.00  212
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1618942000
_diffrn_orient_matrix_UB_12      -0.0462167000
_diffrn_orient_matrix_UB_13      0.0168019000
_diffrn_orient_matrix_UB_21      0.0121132000
_diffrn_orient_matrix_UB_22      -0.0195394000
_diffrn_orient_matrix_UB_23      0.1200994000
_diffrn_orient_matrix_UB_31      -0.0829719000
_diffrn_orient_matrix_UB_32      0.1311314000
_diffrn_orient_matrix_UB_33      -0.0140931000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12025
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.349
_diffrn_reflns_theta_min         3.503
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0524
_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^)+(0.1057P)^2^+0.4478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4416
_reflns_number_total             4839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04624f2.cif
_cod_data_source_block           xud-26
_cod_depositor_comments
'Adding full bibliography for 7134919--7134920.cif.'
_cod_database_code               7134919
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Cl'
_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 C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1A)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C20(H20A,H20B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C11(H11), C12(H12), C16(H16), C17(H17), C28(H28), C29(H29),
 C30(H30)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C)
2.e Idealised tetrahedral OH refined as rotating group:
 O6(H6), O1(H1)
;
_shelx_res_checksum              89437
_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 5.575
_oxdiff_exptl_absorpt_empirical_full_min 0.599