Direct O<sub>2</sub> mediated oxidation of a Ni(II)N<sub>3</sub>O structural model complex for the active site of nickel acireductone dioxygenase (Ni-ARD): characterization, biomimetic reactivity, and enzymatic implications.
Kirsch, Kelsey E.; Little, Mary E.; Cundari, Thomas R.; El-Shaer, Emily; Barone, Georgia; Lynch, Vincent M.; Toledo, Santiago A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17852–17863; doi:10.1039/d4dt02538e

data_7717210
_publ_section_title
;
 Direct O<sub>2</sub> mediated oxidation of a Ni(II)N<sub>3</sub>O
 structural model complex for the active site of nickel acireductone
 dioxygenase (Ni-ARD): characterization, biomimetic reactivity, and
 enzymatic implications.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17852
_journal_page_last               17863
_journal_paper_doi               10.1039/d4dt02538e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C22 H30 F3 N3 Ni O4 S'
_chemical_formula_sum            'C22 H30 F3 N3 Ni O4 S'
_chemical_formula_weight         548.26
_chemical_name_common            NiIIN3OOPhtbuPy
_chemical_name_systematic
'[NiII (N-(ethyl-N?Me2)(Py)(2-t-ButPhOH))(OTf)]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
_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             2021-10-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2024-08-05 deposited with the CCDC.	2024-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                93.7250(8)
_cell_angle_beta                 110.0474(10)
_cell_angle_gamma                99.7261(9)
_cell_formula_units_Z            2
_cell_length_a                   9.39775(11)
_cell_length_b                   10.41762(10)
_cell_length_c                   13.43710(11)
_cell_measurement_reflns_used    11866
_cell_measurement_temperature    99.98(19)
_cell_measurement_theta_max      75.9060
_cell_measurement_theta_min      3.5620
_cell_volume                     1207.28(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Shelxtl-Plus/XP, Bruker AXS, Inc. 2009'
_computing_publication_material  'Shelxtl-Plus, Bruker AXS, Inc. 2009'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(19)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -83.00   7.00   0.50    1.00    --  -48.32 103.00  69.00  180
  2  \w   -106.00 -33.00   0.50    4.00    -- -105.12 103.00  69.00  146
  3  \w    -43.00  24.00   0.50    1.00    --  -48.32  38.00   0.00  134
  4  \w     84.00 177.00   0.50    4.00    --  105.12 103.00  69.00  186
  5  \w     -7.00  83.00   0.50    1.00    --   48.32-103.00 -33.00  180
  6  \w    -70.00  24.00   0.50    1.00    --  -48.32  77.00  30.00  188
  7  \w   -177.00 -95.00   0.50    4.00    -- -105.12 -15.00  30.00  164
  8  \w     74.00 121.00   0.50    1.00    --   48.32 125.00   0.00   94
  9  \w    -25.00  26.00   0.50    1.00    --   48.32 -19.00   0.00  102
 10  \w     74.00 121.00   0.50    1.00    --   48.32 125.00 -90.00   94
 11  \w   -111.00 -33.00   0.50    4.00    -- -105.12 125.00 120.00  156
 12  \w    -71.00 -33.00   0.50    4.00    -- -105.12  61.00 150.00   76
 13  \w   -177.00 -94.00   0.50    4.00    -- -105.12 -45.00   0.00  166
 14  \w   -177.00 -94.00   0.50    4.00    -- -105.12 -45.00  30.00  166
 15  \w   -177.00 -84.00   0.50    4.00    -- -105.12-103.00 -33.00  186
 16  \w     39.00  71.00   0.50    4.00    --  105.12 -61.00-120.00   64
 17  \w     33.00  98.00   0.50    4.00    --  105.12 -95.00 -30.00  130
 18  \w     33.00  69.00   0.50    4.00    --  105.12 -61.00-150.00   72
 19  \w     40.00 103.00   0.50    4.00    --  105.12 -95.00  60.00  126
 20  \w     96.00 173.00   0.50    4.00    --  105.12  45.00-150.00  154
 21  \w     35.00 110.00   0.50    4.00    --  105.12-125.00 -60.00  150
 22  \w     43.00 111.00   0.50    4.00    --  105.12-125.00-120.00  136
 23  \w     34.00 103.00   0.50    4.00    --  105.12 -95.00   0.00  138
 24  \w     81.00 107.00   0.50    4.00    --  105.12-103.00 -33.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1263494000
_diffrn_orient_matrix_UB_12      -0.0257744000
_diffrn_orient_matrix_UB_13      -0.1124055000
_diffrn_orient_matrix_UB_21      0.0840036000
_diffrn_orient_matrix_UB_22      -0.0982476000
_diffrn_orient_matrix_UB_23      -0.0358945000
_diffrn_orient_matrix_UB_31      -0.0935526000
_diffrn_orient_matrix_UB_32      -0.1122398000
_diffrn_orient_matrix_UB_33      0.0351927000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13150
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.413
_diffrn_reflns_theta_min         3.533
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76066
_exptl_absorpt_correction_type   'gaussian and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       prism
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00080(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4821
_refine_ls_number_restraints     337
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0468P)^2^+0.7630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4728
_reflns_number_total             4821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02538e2.cif
_cod_data_source_block           ni-n3o-triflate
_cod_depositor_comments
'Adding full bibliography for 7717208--7717210.cif.'
_cod_database_code               7717210
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O F S Ni'
_reflns_odcompleteness_completeness 99.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C22-F1 = C22-F2 = C22-F3 = C22A-F1A = C22A-F2A = C22A-F3A
 1.34 with sigma of 0.02
 S1-C22 \\sim S1-C22A
 with sigma of 0.01
 S1-F1 \\sim S1-F2 \\sim S1-F3 \\sim S1-F1A \\sim S1-F2A \\sim S1-F3A
 with sigma of 0.01
 F1-F2 \\sim F1-F3 \\sim F2-F3 \\sim F1A-F2A \\sim F1A-F3A \\sim F2A-F3A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F1A \\sim F3A \\sim F3 \\sim F2 \\sim F2A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
O1 \\sim O2 \\sim O3 \\sim O1A \\sim O2A \\sim O3A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C22) = Uanis(C22A)
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(C22A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C22)=FVAR(1)
 Sof(O2A)=Sof(O1A)=Sof(O3A)=1-FVAR(2)
 Sof(O1)=Sof(O3)=Sof(O2)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C9(H9A,H9B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              55661
_shelx_hkl_checksum              68805
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.264
_oxdiff_exptl_absorpt_empirical_full_min 0.555