Indirect evidence for a Ni<sup>III</sup>-oxyl oxidant in the reaction of a Ni<sup>II</sup> complex with peracid.
Pirovano, Paolo; Berry, Abigail R.; Swart, Marcel; McDonald, Aidan R.; Dalton transactions (Cambridge, England : 2003) 47 (2017) 246–250; doi:10.1039/c7dt03316h

data_7044896
_publ_section_title
;
 Indirect evidence for a Ni<sup>III</sup>-oxyl oxidant in the reaction of
 a Ni<sup>II</sup> complex with peracid.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              246
_journal_page_last               250
_journal_paper_doi               10.1039/c7dt03316h
_journal_volume                  47
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C31 H37 N3 O2, C2 H6 O'
_chemical_formula_sum            'C33 H43 N3 O3'
_chemical_formula_weight         529.70
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-07-26 deposited with the CCDC.
2017-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   8.7435(4)
_cell_length_b                   8.7435(4)
_cell_length_c                   69.045(3)
_cell_measurement_reflns_used    5368
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.28
_cell_measurement_theta_min      3.84
_cell_volume                     4571.2(4)
_computing_cell_refinement       'SAINT V8.35A (Buker, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2015) '
_computing_data_reduction        'SAINT V8.35A (Buker, 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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       82
_diffrn_reflns_limit_l_min       -82
_diffrn_reflns_number            26441
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.386
_diffrn_reflns_theta_min         3.841
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0936 before and 0.0731 after correction.
The Ratio of minimum to maximum transmission is 0.7514.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1716
_exptl_crystal_recrystallization_method 'crystallized from EtOH in an NMR tube'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 1992 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5575
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0688P)^2^+0.9525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.976
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                4864
_reflns_number_total             5575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03316h2.cif
_cod_data_source_block           tcd590b
_cod_depositor_comments
'Adding full bibliography for 7044896--7044898.cif.'
_cod_original_cell_volume        4571.2(5)
_cod_database_code               7044896
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C16-C16A
 0.3 with sigma of 0.01
 C19-C19A
 0.4 with sigma of 0.01
 C16A-C11 \\sim C16-C11
 with sigma of 0.002
 O37-C38 \\sim O37-C38A
 with sigma of 0.002
 C39A-C38A \\sim C39-C38
 with sigma of 0.002
 C20-C19 \\sim C20A-C19A
 with sigma of 0.01
 C21-C19 \\sim C21A-C19A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C16A) = Uanis(C17A) = Uanis(C18A) = Uanis(C17) = Uanis(C16) = Uanis(C18)
Uanis(C19A) = Uanis(C20A) = Uanis(C21A) = Uanis(C19) = Uanis(C20) = Uanis(C21)
Uanis(C38A) = Uanis(C39A) = Uanis(C38) = Uanis(C39)
4. Others
 Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36A)=Sof(H36A)=
 Sof(H36B)=Sof(H36C)=1-FVAR(1)
 Sof(H34)=Sof(C36)=Sof(H36D)=Sof(H36E)=Sof(H36F)=Sof(C35)=Sof(H35D)=Sof(H35E)=
 Sof(H35F)=FVAR(1)
 Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(2)
 Sof(C17)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C16)=Sof(H16)=Sof(C18)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=FVAR(2)
 Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21A)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=1-FVAR(3)
 Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=FVAR(3)
 Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(C39A)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=1-FVAR(4)
 Sof(H37)=Sof(C38)=Sof(H38C)=Sof(H38D)=Sof(C39)=Sof(H39D)=Sof(H39E)=Sof(H39F)=
 FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C34(H34A), C34(H34), C16A(H16A), C19A(H19A), C16(H16), C19(H19)
5.b Secondary CH2 refined with riding coordinates:
 C38A(H38A,H38B), C38(H38C,H38D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14), C27(H27), C28(H28),
 C29(H29), N9(H9)
5.d Tetrahedral OH refined with riding coordinates:
 O37(H37A), O37(H37)
5.e Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C17A(H17A,H17B,H17C), C18A(H18A,
 H18B,H18C), C20A(H20A,H20B,H20C), C21A(H21A,H21B,H21C), C35A(H35A,H35B,H35C),
 C36A(H36A,H36B,H36C), C39A(H39A,H39B,H39C), C36(H36D,H36E,H36F), C17(H17D,H17E,
 H17F), C18(H18D,H18E,H18F), C20(H20D,H20E,H20F), C21(H21D,H21E,H21F), C35(H35D,
 H35E,H35F), C39(H39D,H39E,H39F)
;
_shelx_res_checksum              56427
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'mounted in oil on a MItegen holder'
_olex2_submission_original_sample_id PP499
_olex2_submission_special_instructions 'No special instructions were received'