Late-Metal Nitrosyl Cations: Synthesis and Reactivity of [Ni(NO)(MeNO2)3][PF6]
Ashley M. Wright; Guang Wu; Trevor W. Hayton; Inorganic Chemistry 50 (2011) 11746–11753; doi:10.1021/ic201821t

data_4326914
_publ_section_title
;
 Late-Metal Nitrosyl Cations: Synthesis and Reactivity of
 [Ni(NO)(MeNO2)3][PF6]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11746
_journal_page_last               11753
_journal_paper_doi               10.1021/ic201821t
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C4 H9 F6 N4 Ni O7 P'
_chemical_formula_weight         428.83
_chemical_name_systematic
; 
tris nitromethane nitrosyl nickel hexafluorophosphate
;
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.4863(5)
_cell_length_b                   17.4863(5)
_cell_length_c                   8.5815(5)
_cell_measurement_temperature    150(2)
_cell_volume                     2272.43(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD detector'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19641
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    1.491
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.382
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_description       needle
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         3093
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                2439
_reflns_number_total             3093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201821t_si_001_1.cif
_cod_data_source_block           complex_1
_cod_original_cell_volume        2272.42(16)
_cod_database_code               4326914