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_1552906
_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         'C47 H77 K N2 Ni O6 S2, 2(C7 H8)'
_chemical_formula_sum            'C61 H93 K N2 Ni O6 S2'
_chemical_formula_weight         1112.30
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-06-04 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                80.905(4)
_cell_angle_beta                 87.457(4)
_cell_angle_gamma                62.801(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8138(16)
_cell_length_b                   13.3400(17)
_cell_length_c                   20.566(3)
_cell_measurement_reflns_used    371
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      1.76
_cell_volume                     3085.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12552
_diffrn_reflns_theta_full        26.47
_diffrn_reflns_theta_max         26.47
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  0.9901
_exptl_absorpt_correction_T_min  0.9070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.355
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         12552
_refine_ls_number_restraints     443
_refine_ls_restrained_S_all      1.614
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+7.0044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1642
_reflns_number_gt                8895
_reflns_number_total             12552
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8sc02536c2.cif
_cod_data_source_block           n_a
_cod_original_cell_volume        3085.8(7)
_cod_database_code               1552906