A bifunctional small molecular photocatalyst with a redox center and a Lewis acid site for one-pot tandem oxidation–acetalization
Rao, Cai-Hui; Ma, Shuai; Cui, Jing-Wang; Jia, Meng-Ze; Yao, Xin-Rong; Zhang, Jie; Green Chemistry 24 (2022) 5862–5868; doi:10.1039/D2GC01321E

data_7245136
_publ_section_title
;
 A bifunctional small molecular photocatalyst with a redox center and a
 Lewis acid site for one-pot tandem oxidation--acetalization
;
_journal_issue                   15
_journal_name_full               'Green Chemistry'
_journal_page_first              5862
_journal_page_last               5868
_journal_paper_doi               10.1039/D2GC01321E
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C24 H16 Cl N6, F6 P'
_chemical_formula_sum            'C24 H16 Cl F6 N6 P'
_chemical_formula_weight         568.85
_chemical_name_systematic        PTP-dq-PF6
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-02-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-18 deposited with the CCDC.	2022-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 78.05(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   15.627(3)
_cell_length_b                   21.005(8)
_cell_length_c                   21.972(6)
_cell_measurement_reflns_used    6737
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3900
_cell_measurement_theta_min      4.0760
_cell_volume                     7056(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.1418
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            51953
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.948
_diffrn_reflns_theta_min         3.517
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74554
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         17539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.2578
_refine_ls_R_factor_gt           0.0957
_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^)+(0.1520P)^2^+0.5260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2467
_refine_ls_wR_factor_ref         0.3531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5973
_reflns_number_total             17539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2gc01321e2.cif
_cod_data_source_block           PTP-dq-PF6
_cod_depositor_comments
;
        Adding full bibliography for 7245136.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C72 H48 Cl3 F18 N18 P3'
_cod_original_formula_weight         1706.54
_cod_original_formula_moiety         '3(C24 H16 Cl N6), 3(F6 P)'
_cod_original_formula_units_Z            4
_cod_database_code               7245136
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C13(H13), C16(H16),
 C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C35(H35), C38(H38),
 C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48),
  C50(H50), C51(H51), C53(H53), C54(H54), C56(H56), C57(H57), C59(H59),
 C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C69(H69), C70(H70), C71(H71),
  C72(H72)
;
_shelx_res_checksum              82057
_shelx_hkl_checksum              21428
_olex2_submission_special_instructions 'No special instructions were received'