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_4318358
_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         'C24 H34 Cr N3 O5 1+, F6 P 1-'
_chemical_formula_sum            'C24 H34 Cr F6 N3 O5 P'
_chemical_formula_weight         641.51
_chemical_name_common            '[Cr(acaMe)2(IM2py)]PF~6~'
_chemical_name_systematic
;
Bis(3-Methyl-pentane-2,4-dionato)(2-(2-pyridyl)-4,4,5,5-tetramethyl
imidazoline-1-oxy)chromium(III) Hexafluorophosphate
;
_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'
_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                 94.473(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7128(4)
_cell_length_b                   15.7194(5)
_cell_length_c                   17.1131(6)
_cell_measurement_reflns_used    21360
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.8
_cell_volume                     2873.05(17)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    'ORTEP in teXsan Ver. 1.11'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11176
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2173
_refine_ls_wR_factor_ref         0.2382
_reflns_number_gt                3798
_reflns_number_total             6498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic011282m_1.cif
_cod_data_source_block           acaMeIM
_cod_database_code               4318358