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_4128055
_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         'C58 H72 F12 N4 Ni2 O2'
_chemical_formula_sum            'C58 H72 F12 N4 Ni2 O2'
_chemical_formula_weight         1202.61
_chemical_name_systematic        {[iPr2NNF6]NiOH}2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                82.6440(10)
_cell_angle_beta                 76.3840(10)
_cell_angle_gamma                65.6130(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6731(10)
_cell_length_b                   13.2679(11)
_cell_length_c                   20.9329(18)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.37
_cell_volume                     2868.0(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4, (Bruker, 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-4 (Bruker, 2014) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  15197
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41401
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.578
_diffrn_reflns_theta_min         1.686
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6112
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_id                15197
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         14532
_refine_ls_number_restraints     938
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+2.7200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11002
_reflns_number_total             14532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09769_si_006.cif
_cod_data_source_block           NiOH
_cod_database_code               4128055
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.803
_shelx_estimated_absorpt_t_max   0.897
_shelx_res_checksum              52952
_shelx_hkl_checksum              49614