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_4128053
_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_absolute_configuration ad
_chemical_formula_moiety         'C45 H67 F6 K N3 Ni O8'
_chemical_formula_sum            'C45 H67 F6 K N3 Ni O8'
_chemical_formula_weight         989.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.014(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0758(8)
_cell_length_b                   13.7250(6)
_cell_length_c                   20.4222(9)
_cell_measurement_reflns_used    7765
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.46
_cell_volume                     5066.6(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 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  15053
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0777
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33636
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.384
_diffrn_reflns_theta_min         0.997
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6176
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.320
_refine_diff_density_max         1.565
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 4853 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
 Flack (1983),  7806 Friedels
;
_refine_ls_abs_structure_Flack   0.018(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1454
_refine_ls_number_reflns         17499
_refine_ls_number_restraints     1188
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+1.7061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    0.882
_reflns_Friedel_fraction_max     0.877
_reflns_number_gt                13716
_reflns_number_total             17499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09769_si_003.cif
_cod_data_source_block           NiNOK18C6
_cod_database_code               4128053
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.771
_shelx_estimated_absorpt_t_max   0.847
_shelx_res_checksum              79855
_shelx_hkl_checksum              84130