Nickel(II) complexes with covalently attached quinols rely on ligand-derived redox couples to catalyze superoxide dismutation.
Boothe, Robert; Oppelt, Julian; Franke, Alicja; Moore, Jamonica L.; Squarcina, Andrea; Zahl, Achim; Senft, Laura; Kellner, Ina; Awalah, Akudo L.; Bradford, Alisabeth; Obisesan, Segun V.; Schwartz, Dean D.; Ivanović-Burmazović, Ivana; Goldsmith, Christian R.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3733–3749; doi:10.1039/d4dt03331k

data_7717898
_publ_section_title
;
 Nickel(II) complexes with covalently attached quinols rely on
 ligand-derived redox couples to catalyze superoxide dismutation.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3733
_journal_page_last               3749
_journal_paper_doi               10.1039/d4dt03331k
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C32 H36 N6 Ni O4, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C38 H42 F6 N8 Ni O10 S2'
_chemical_formula_weight         1007.62
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_Int_Tables_number      19
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2024-10-14 deposited with the CCDC.	2025-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8113(6)
_cell_length_b                   17.4024(9)
_cell_length_c                   20.1442(10)
_cell_measurement_reflns_used    9718
_cell_measurement_temperature    180.45
_cell_measurement_theta_max      27.384
_cell_measurement_theta_min      2.218
_cell_volume                     4491.1(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2011 (Burla et al., 2007)'
_diffrn_ambient_temperature      180.45
_diffrn_measured_fraction_theta_full 0.9950
_diffrn_measured_fraction_theta_max 0.9929
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            105753
_diffrn_reflns_theta_full        27.4363
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.6274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1140 before and 0.0790 after correction.
The Ratio of minimum to maximum transmission is 0.8433.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.4901
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             2083.6651
_exptl_crystal_recrystallization_method
'Concentrated solution of acetonitrile was layered with ether at room temperature.'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.6587
_refine_diff_density_min         -1.3151
_refine_diff_density_rms         0.1113
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.11(2)
_refine_ls_d_res_high            0.7713
_refine_ls_d_res_low             13.1689
_refine_ls_goodness_of_fit_ref   1.0429
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     597
_refine_ls_number_reflns         10173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0429
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+20.0796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.990
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              26
_reflns_limit_l_min              -25
_reflns_number_gt                9748
_reflns_number_total             10173
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4dt03331k2.cif
_cod_data_source_block           goldsmith070915_0m
_cod_depositor_comments
'Adding full bibliography for 7717897--7717898.cif.'
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               7717898
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 c15(H15a,H15b), c23(H23a,H23b), c16(H16a,H16b), c14(H14a,H14b), c6(H6a,H6b),
 c7(H7a,H7b)
2.b Aromatic/amide H refined with riding coordinates:
 c28(H28), c27(H27), c26(H26), c25(H25), c22(H22), c20(H20), c19(H19), c1(H1a),
  c2(H2a), c3(H3a), c4(H4a), c12(H12), c11(H11), c9(H9)
2.c Idealised Me refined as rotating group:
 c32(H32a,H32b,H32c), c30(H30a,H30b,H30c), c2s(H2sa,H2sb,H2sc), c4s(H4sa,H4sb,
 H4sc)
2.d Idealised tetrahedral OH refined as rotating group:
 o3(H3), o2(H2)
;
_olex2_exptl_crystal_mounting_method
'Large prism was cut into an irrigular fragment at room temperature under paratone-n. The fragment was mounted directly onto a quartz fiber and placed into -90 degree C coldstream.'
_olex2_submission_special_instructions 'No special instructions were received'