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_4128056
_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 N3 Ni O'
_chemical_formula_sum            'C29 H35 F6 N3 Ni O'
_chemical_formula_weight         614.31
_chemical_name_systematic        '[iPr2NNF6]NiNO'
_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                 109.3490(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5093(9)
_cell_length_b                   16.6592(11)
_cell_length_c                   13.9913(9)
_cell_measurement_reflns_used    9754
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.243
_cell_measurement_theta_min      2.1895
_cell_volume                     2970.9(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            82800
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         1.816
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6156
_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            green
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         7351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+1.7125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6411
_reflns_number_total             7351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09769_si_002.cif
_cod_data_source_block           NiNO
_cod_database_code               4128056
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.739
_shelx_estimated_absorpt_t_max   0.864
_shelx_res_checksum              3426
_shelx_hkl_checksum              536