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_1552907
_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         'C48 H77 K N2 Ni O8, 2(C6H6)'
_chemical_formula_sum            'C60 H89 K N2 Ni O8'
_chemical_formula_weight         1064.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-06-04 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.289(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.875(6)
_cell_length_b                   11.044(3)
_cell_length_c                   26.136(8)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      1.64
_cell_volume                     5909(3)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.969
_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  0.0834
_diffrn_reflns_av_unetI/netI     0.1434
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24126
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.441
_diffrn_reflns_theta_min         0.995
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.995
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         11782
_refine_ls_number_restraints     624
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1961
_refine_ls_R_factor_gt           0.1112
_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^)+(0.0930P)^2^+44.2287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2693
_refine_ls_wR_factor_ref         0.3112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6253
_reflns_number_total             11782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02536c2.cif
_cod_data_source_block           NH_6_125_plates_0m_a
_cod_database_code               1552907
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              78754