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_7044898
_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_formula_moiety         ' C38 H41 Cl N3 Ni O4, C8 H20 N, C2 H3 N'
_chemical_formula_sum            'C48 H64 Cl N5 Ni O4'
_chemical_formula_weight         869.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-07-26 deposited with the CCDC.
2017-11-28 downloaded from the CCDC.
;
_cell_angle_alpha                110.6620(10)
_cell_angle_beta                 91.4110(10)
_cell_angle_gamma                106.7540(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2143(4)
_cell_length_b                   13.9431(5)
_cell_length_c                   16.1500(6)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.63
_cell_measurement_theta_min      2.68
_cell_volume                     2239.91(14)
_computing_cell_refinement       'SAINT+ Ver. 8.35A (Bruker, 2013)'
_computing_data_collection       'APEX2 Ver. 2015.9-0 (Bruker, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.35A (Bruker, 2013)'
_computing_molecular_graphics    'XP (Bruker, 2015)'
_computing_publication_material  'XCIF (Bruker, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.12
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker PHOTON 50 QUEST ECO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49339
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.633
_diffrn_reflns_theta_min         2.298
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2014/5 (Bruker, 2014/5) was used for absorption correction.
wR2(int) was 0.0494 before and 0.0443 after correction.
The Ratio of minimum to maximum transmission is 0.925.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       fragment
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         13768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0414P)^2^+1.4301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11396
_reflns_number_total             13768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03316h2.cif
_cod_data_source_block           tcd372
_cod_depositor_comments
'Adding full bibliography for 7044896--7044898.cif.'
_cod_database_code               7044898
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.872
_shelx_estimated_absorpt_t_max   0.943
_shelx_res_checksum              83446