Visible-light-mediated β-acylative divergent alkene difunctionalization with Katritzky salt/CO2
Nandi, Shantanu; Das, Pritha; Das, Subhodeep; Mondal, Shuvam; Jana, Ranjan; Green Chemistry 25 (2023) 3633–3643; doi:10.1039/D3GC00143A

data_7246560
_publ_section_title
;
 Visible-light-mediated \b-acylative divergent alkene difunctionalization
 with Katritzky salt/CO2
;
_journal_issue                   9
_journal_name_full               'Green Chemistry'
_journal_page_first              3633
_journal_page_last               3643
_journal_paper_doi               10.1039/D3GC00143A
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C30 H28 O3'
_chemical_formula_sum            'C30 H28 O3'
_chemical_formula_weight         436.52
_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             2021-09-23
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;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-03-22 deposited with the CCDC.	2023-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                102.012(3)
_cell_angle_beta                 94.177(2)
_cell_angle_gamma                110.290(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7371(9)
_cell_length_b                   10.1536(10)
_cell_length_c                   12.7652(12)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      64.93
_cell_measurement_theta_min      3.59
_cell_volume                     1143.27(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28980
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        64.966
_diffrn_reflns_theta_max         64.966
_diffrn_reflns_theta_min         3.585
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.4872
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic whiteish colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             464
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/hexane'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         3779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0676
_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^)+(0.1272P)^2^+0.5761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.1918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3635
_reflns_number_total             3779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3gc00143a2.cif
_cod_data_source_block           pd_4_72_0m_a
_cod_depositor_comments
'Adding full bibliography for 7246560--7246561.cif.'
_cod_database_code               7246560
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.763
_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
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C12(H12), C14(H14), C11(H11), C5(H5), C23(H23), C21(H21), C25(H25),
 C2(H2), C1(H1), C20(H20), C22(H22), C19(H19), C3(H3), C28(H28), C26(H26),
 C29(H29), C6(H6)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              55027
_olex2_submission_special_instructions 'No special instructions were received'