Nickel-mediated N‒N bond formation and N2O liberation via nitrogen oxyanion reduction
Beagan, Daniel M.; Cabelof, Alyssa C.; Pink, Maren; Carta, Veronica; Gao, Xinfeng; Caulton, Kenneth G.; Chemical Science  (2021) –; doi:10.1039/D1SC02846D

data_1564205
_publ_section_title
;
 Nickel-mediated N--N bond formation and N2O liberation via nitrogen
 oxyanion reduction
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02846D
_journal_year                    2021
_chemical_formula_moiety         'C22.967 H28 Cl0.033 F2.9 N3 Ni O3.9 S0.967'
_chemical_formula_sum            'C22.97 H28 Cl0.03 F2.9 N3 Ni O3.9 S0.97'
_chemical_formula_weight         554.56
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-02-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-05-11 deposited with the CCDC.	2021-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.9590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4858(3)
_cell_length_b                   19.4001(6)
_cell_length_c                   12.4864(4)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    133.0
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.34
_cell_volume                     2631.35(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      133.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker VENTURE D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1185
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            92275
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.019
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       plate
_exptl_crystal_F_000             1153
_exptl_crystal_preparation       synthesized
_exptl_crystal_recrystallization_method 'vapor diffusion of pentane into THF'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         6025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0403P)^2^+2.8604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4579
_reflns_number_total             6025
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02846d3.cif
_cod_data_source_block           mo_21006_0m_a
_cod_original_formula_sum        'C22.97 H28 Cl0.03 F2.90 N3 Ni O3.90 S0.97'
_cod_database_code               1564205
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.832
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cl1) = Uanis(O2)
3. Others
 Sof(Cl1)=1-FVAR(1)
 Sof(S1)=Sof(O2)=Sof(O3)=Sof(F2)=Sof(O4)=Sof(F3)=Sof(F1)=Sof(C23)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C17(H17), C6(H6), C20(H20)
4.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C11(H11A,H11B,H11C), C16(H16A,H16B,
 H16C), C5(H5A,H5B,H5C), C22(H22A,H22B,H22C), C1(H1A,H1B,H1C), C19(H19A,H19B,
 H19C)
;
_shelx_res_checksum              5436
_shelx_hkl_checksum              96710
_olex2_submission_special_instructions 'No special instructions were received'