Harmonization of an incompatible aqueous aldol condensation/oxa-Michael addition/reduction cascade process over a core–shell-structured thermoresponsive catalyst
Su, Yu; Wang, Chengyi; Chen, Qipeng; Zhu, Yuanli; Deng, Shaomin; Yang, Shoujin; Jin, Ronghua; Liu, Guohua; Green Chemistry 25 (2023) 6859–6868; doi:10.1039/D3GC01670F

data_7247129
_publ_section_title
;
 Harmonization of an incompatible aqueous aldol condensation/oxa-Michael
 addition/reduction cascade process over a core--shell-structured
 thermoresponsive catalyst
;
_journal_issue                   17
_journal_name_full               'Green Chemistry'
_journal_page_first              6859
_journal_page_last               6868
_journal_paper_doi               10.1039/D3GC01670F
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_sum            'C16 H16 O2'
_chemical_formula_weight         240.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2022-12-19 deposited with the CCDC.	2023-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.231(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9068(17)
_cell_length_b                   4.8812(7)
_cell_length_c                   22.718(4)
_cell_measurement_reflns_used    1988
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      53.946
_cell_measurement_theta_min      4.783
_cell_volume                     1316.8(4)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.997
_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  0.0722
_diffrn_reflns_av_unetI/netI     0.0860
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
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_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12932
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.715
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.070
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_refine_diff_density_max         0.269
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
; 
 Flack x determined using 667 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.0(10)
_refine_ls_extinction_coef       0.016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         4440
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.0702
_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^)+(0.0642P)^2^+0.4554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.2035
_reflns_Friedel_coverage         0.700
_reflns_Friedel_fraction_full    0.879
_reflns_Friedel_fraction_max     0.905
_reflns_number_gt                2296
_reflns_number_total             4440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3gc01670f2.cif
_cod_data_source_block           mo_d8v22531_0m
_cod_depositor_comments          'Adding full bibliography for 7247129.cif.'
_cod_original_cell_volume        1316.8(3)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7247129
_shelx_estimated_absorpt_t_min   0.985
_shelx_estimated_absorpt_t_max   0.996
_shelxl_version_number           2013-4
_shelx_res_checksum              94454
_shelx_hkl_checksum              4652