Nitrosyl Linkage Isomers: NO Coupling to N<sub>2</sub>O at a Mononuclear Site.
Kundu, Subrata; Phu, Phan N.; Ghosh, Pokhraj; Kozimor, Stosh A.; Bertke, Jeffery A.; Stieber, S Chantal E; Warren, Timothy H.; Journal of the American Chemical Society 141 (2019) 1415–1419; doi:10.1021/jacs.8b09769

data_4128054
_publ_contact_author             'Timothy H. Warren'
_publ_section_title
;
 Nitrosyl Linkage Isomers: NO Coupling to N<sub>2</sub>O at a Mononuclear
 Site.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1415
_journal_page_last               1419
_journal_paper_doi               10.1021/jacs.8b09769
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C29 H35 F6 N4 Ni O2, C18 H36 K N2 O6'
_chemical_formula_sum            'C47 H71 F6 K N6 Ni O8'
_chemical_formula_weight         1059.90
_chemical_name_systematic        '[iPr2NNF6]NiO2N2-K[2.2.2-Kryptofix]'
_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_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.692(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5729(8)
_cell_length_b                   38.111(3)
_cell_length_c                   13.4355(9)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9795
_cell_measurement_theta_min      2.2635
_cell_volume                     5236.7(7)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker APEXII'
_computing_molecular_graphics
'XSEED; Barbour, L. J. (2001) J. Supramol. Chem. 1, 189-191.'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57168
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         29.194
_diffrn_reflns_theta_min         2.242
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS based on Blessing's method; Blessing, Acta Cryst. (1995) A51 33-38'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.403
_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     630
_refine_ls_number_reflns         13952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0386P)^2^+0.8121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9381
_reflns_number_total             13952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09769_si_005.cif
_cod_data_source_block           NiONNOKKryptofix
_cod_original_cell_volume        5236.8(6)
_cod_database_code               4128054
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.854
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              61843
_shelx_hkl_checksum              796