Synthesis, Magnetic Properties, and Electronic Spectra of Bis(β-diketonato)chromium(III) and Nickel(II) Complexes with a Chelated Imino Nitroxide Radical: X-ray Structures of [Cr(acaMe)2(IM2py)]PF6 and [Ni(acac)2(IM2py)]
Yasunori Tsukahara; Takayuki Kamatani; Atsushi Iino; Takayoshi Suzuki; Sumio Kaizaki; Inorganic Chemistry 41 (2002) 4363–4370; doi:10.1021/ic011282m

data_4318359
_publ_section_title
;
 Synthesis, Magnetic Properties, and Electronic Spectra of
 Bis(\b-diketonato)chromium(III) and Nickel(II) Complexes with a Chelated
 Imino Nitroxide Radical: X-ray Structures of [Cr(acaMe)2(IM2py)]PF6 and
 [Ni(acac)2(IM2py)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4363
_journal_page_last               4370
_journal_paper_doi               10.1021/ic011282m
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         '(Ni (C5 H7 O2)2 (C12 H16 N3 O))'
_chemical_formula_sum            'C22 H30 N3 Ni O5'
_chemical_formula_weight         475.20
_chemical_name_common            '[Ni(acac)~2~(IM2py)]'
_chemical_name_systematic
;
Bis(pentane-2,4-dionato)(2-(2'-pyridyl)-4,4,5,5-tetramethyl-4,5-dihydro-1H-
imidazol-1-oxy)nickel(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.445(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.018(3)
_cell_length_b                   10.095(3)
_cell_length_c                   17.972(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     4900.2(19)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  AFC5R
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71072
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.1427
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7269
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        1.31
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.961
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         7143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1951
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                2846
_reflns_number_total             7143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic011282m_2.cif
_cod_data_source_block           kama2
_cod_original_cell_volume        4900.3(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4318359