Synthesis and reactivity of a nickel(ii) thioperoxide complex: demonstration of sulfide-mediated N<sub>2</sub>O reduction.
Hartmann, Nathaniel J.; Wu, Guang; Hayton, Trevor W.; Chemical science 9 (2018) 6580–6588; doi:10.1039/c8sc02536c

data_1549613
_publ_section_title
;
 Synthesis and reactivity of a nickel(ii) thioperoxide complex:
 demonstration of sulfide-mediated N<sub>2</sub>O reduction.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              6580
_journal_page_last               6588
_journal_paper_doi               10.1039/c8sc02536c
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C53 H89 K N4 Ni O6 S'
_chemical_formula_sum            'C53 H89 K N4 Ni O6 S'
_chemical_formula_weight         1008.15
_chemical_name_systematic
'(Sulfido)- (N,N'-bis(2,6-di-isopropylphenyl)-2,2,6,6-tetramethylheptane-3,5-di-iminato)-(4,7,13,16,21,24-Hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)-nickel(II)-potassium'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1jqjkb
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-01 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.126(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7125(6)
_cell_length_b                   22.4934(11)
_cell_length_c                   20.0532(12)
_cell_measurement_temperature    100(2)
_cell_volume                     5606.2(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1187
_diffrn_reflns_av_unetI/netI     0.1281
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35206
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.502
_diffrn_reflns_theta_min         1.378
_exptl_absorpt_coefficient_mu    0.506
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2184
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         11559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0579P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6720
_reflns_number_total             11559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02536c2.cif
_cod_data_source_block           complex_5
_cod_depositor_comments
'Adding full bibliography for 1549610--1549615.cif.'
_cod_database_code               1549613
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              23180