Crystal structure of a phenoxyl radical complex relevant to the metal site of the galactose oxidase enzyme: A facile one-pot synthesis, evidence for hydrogen atom transfer and DNA cleavage <i>via</i> self-activation.
Singh, Ovender; Singh, Anshu; Maji, Ankur; Chauhan, Rahul; Gupta, Puneet; Ghosh, Kaushik; Dalton transactions (Cambridge, England : 2003) 53 (2024) 986–995; doi:10.1039/d3dt03282e

data_7714563
_publ_section_title
;
 Crystal structure of a phenoxyl radical complex relevant to the metal
 site of the galactose oxidase enzyme: A facile one-pot synthesis,
 evidence for hydrogen atom transfer and DNA cleavage <i>via</i>
 self-activation.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              986
_journal_page_last               995
_journal_paper_doi               10.1039/d3dt03282e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C47 H55 Cu0.922 N6 O5'
_chemical_formula_sum            'C47 H55 Cu0.922 N6 O5'
_chemical_formula_weight         842.587
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2023-10-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-06 deposited with the CCDC.	2023-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.321(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.281(1)
_cell_length_b                   11.9133(5)
_cell_length_c                   18.1460(8)
_cell_measurement_reflns_used    9810
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      23.106
_cell_measurement_theta_min      2.269
_cell_volume                     5107.8(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      105.00
_diffrn_measured_fraction_theta_full 0.9970
_diffrn_measured_fraction_theta_max 0.9889
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.9970
_diffrn_reflns_Laue_measured_fraction_max 0.9889
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            173918
_diffrn_reflns_point_group_measured_fraction_full 0.9970
_diffrn_reflns_point_group_measured_fraction_max 0.9889
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0909 before and 0.0708 after correction.
The Ratio of minimum to maximum transmission is 0.8781.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic orangish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       block
_exptl_crystal_F_000             1785.350
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.8022
_refine_diff_density_min         -0.5512
_refine_diff_density_rms         0.1247
_refine_ls_d_res_high            0.7466
_refine_ls_d_res_low             10.6376
_refine_ls_goodness_of_fit_ref   1.0972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    86
_refine_ls_number_parameters     555
_refine_ls_number_reflns         12696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0972
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1016P)^2^+2.6603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1981
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              31
_reflns_limit_h_min              -32
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                8178
_reflns_number_total             12696
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt03282e2.cif
_cod_data_source_block           ms_rj_001_0401_0ma_a
_cod_depositor_comments
'Adding full bibliography for 7714562--7714563.cif.'
_cod_database_code               7714563
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12),
 C14(H14), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C29(H29),
  C31(H31), C33(H33)
1.b Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C28(H28a,H28b,H28c), C36(H36a,H36b,H36c), C37(H37a,H37b,
 H37c), C38(H38a,H38b,H38c), C39(H39a,H39b,H39c), C41(H41a,H41b,H41c), C43(H43a,
 H43b,H43c), C44(H44a,H44b,H44c), C45(H45a,H45b,H45c), C46(H46a,H46b,H46c),
 C47(H47a,H47b,H47c)
;
_olex2_submission_special_instructions 'No special instructions were received'