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_1564202
_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_sum            'C22 H28 N3 Ni O'
_chemical_formula_weight         409.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-05-11 deposited with the CCDC.	2021-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                67.393(17)
_cell_angle_beta                 84.22(2)
_cell_angle_gamma                78.271(17)
_cell_formula_units_Z            2
_cell_length_a                   8.631(6)
_cell_length_b                   9.896(6)
_cell_length_c                   12.698(8)
_cell_measurement_reflns_used    1234
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.78
_cell_measurement_theta_min      2.27
_cell_volume                     980.0(11)
_computing_cell_refinement       'SAINT V8.38A (BrukerNano, 2017)'
_computing_data_collection       'BIS v6.2.9 (BrukerNano, 2018)'
_computing_data_reduction        'SAINT V8.38A (BrukerNano, 2017)'
_computing_publication_material  'APEX3 v2018.1-0 (BrukerNano, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
'0.50 degree frames measured for 5 and 9 seconds each'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2083
_diffrn_reflns_av_unetI/netI     0.2827
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12098
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.262
_diffrn_reflns_theta_min         2.266
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick; 2018'
_exptl_crystal_colour            teal
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       needle
_exptl_crystal_F_000             434
_exptl_crystal_size_max          0.021
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.004
_refine_diff_density_max         2.711
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3478
_refine_ls_number_restraints     211
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.2105
_refine_ls_R_factor_gt           0.1238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1533P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2828
_refine_ls_wR_factor_ref         0.3484
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1648
_reflns_number_total             3478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02846d3.cif
_cod_data_source_block           20016
_cod_original_cell_volume        979.9(11)
_cod_database_code               1564202
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              57211
_shelx_hkl_checksum              16071