A nitronyl nitroxide complex of nickel(II) with nitrate as a ligand
Yoshida, Takafumi; Suzuki, Takayoshi; Kaizaki, Sumio; Acta Crystallographica Section C 57 (2001) 1274–1276; doi:10.1107/S0108270101013725

data_2012337
_publ_section_title
;
 A nitronyl nitroxide complex of nickel(II) with nitrate as a ligand
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1274
_journal_page_last               1276
_journal_paper_doi               10.1107/S0108270101013725
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac
'[Ni (N O3) (C6 H16 N2) (C12 H16 N3 O2)] P F6, C H2 Cl2'
_chemical_formula_moiety         'C18 H32 N6 Ni O5 1+, F6 P 1-, C H2 Cl2'
_chemical_formula_sum            'C19 H34 Cl2 F6 N6 Ni O5 P'
_chemical_formula_weight         701.08
_chemical_name_common            '[Ni(NO~3~)(tmen)(NIT2py)]PF6.CH2Cl2'
_chemical_name_systematic
;
[4,5-Dihydro-4,4,5,5-tetramethyl-2-(2-pyridyl-\kN)imidazol-1-oxyl
3-oxide-\kO^3^](nitrato-\k^2^O,O')(N,N,N',N'-tetramethyl-1,2-ethanediamine-
\k^2^N,N')nickel(II) hexafluorophophate dichloromethane solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.305(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6307(18)
_cell_length_b                   26.690(6)
_cell_length_c                   13.119(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.7
_cell_volume                     2952.6(10)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
'MSC/AFC Diffractometer Control Software (Rigaku, 1985)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation and Rigaku, 2000)'
_computing_molecular_graphics    'ORTEP (Johnson, 1970)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .0385
_diffrn_reflns_av_sigmaI/netI    .1099
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9114
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        .39
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .971
_exptl_absorpt_correction_T_max  .881
_exptl_absorpt_correction_T_min  .802
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Coppens et al., 1965)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1444
_exptl_crystal_size_max          .26
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .10
_refine_diff_density_max         .748
_refine_diff_density_min         -.618
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         8605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .995
_refine_ls_R_factor_all          .1634
_refine_ls_R_factor_gt           .0473
_refine_ls_shift/su_max          .017
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0634P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1535
_reflns_number_gt                3922
_reflns_number_total             8605
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            oa1122.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2012337
_cod_database_fobs_code          2012337