Development of Anthrazoline Photocatalyst for Promoting Amination and Amidation Reactions
Wang, Danfeng; Huang, Hai; Zhu, Xiaolin; Chemical Communications  (2022) –; doi:10.1039/D1CC07315J

data_7129701
_publ_section_title
;
 Development of Anthrazoline Photocatalyst for Promoting Amination and
 Amidation Reactions
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC07315J
_journal_year                    2022
_chemical_formula_moiety         'C50 H32 N2'
_chemical_formula_sum            'C50 H32 N2'
_chemical_formula_weight         660.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.118(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.501(6)
_cell_length_b                   21.209(9)
_cell_length_c                   13.563(6)
_cell_measurement_reflns_used    8874
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      31.32
_cell_measurement_theta_min      2.29
_cell_volume                     3560(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.984
_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  0.0334
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            93709
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         1.795
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  0.9608
_exptl_absorpt_correction_T_min  0.8571
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0871 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.8921.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+1.8747P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5978
_reflns_number_total             7437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc07315j2.cif
_cod_data_source_block           zx12a_zxl_5b_0m
_cod_database_code               7129701
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C20(H20), C29(H29)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C15(H15), C17(H17), C18(H18), C23(H23), C25(H25), C27(H27),
 C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52)
;
_shelx_res_checksum              34584
_olex2_submission_special_instructions 'No special instructions were received'