Synthesis, magnetic properties, and electronic spectra of mixed ligand bis(β-diketonato)chromium(III) complexes with a chelated nitronyl nitroxide radical: X-ray structure of [Cr(dpm)2(NIT2py)]PF6
Yasunori Tsukahara; Atsushi Iino; Takafumi Yoshida; Takayoshi Suzuki; Sumio Kaizaki; J. Chem. Soc., Dalton Trans.  (2002) 181–187; doi:10.1039/b104092h

data_7010810
_publ_section_title
;
 Synthesis, magnetic properties, and electronic spectra of mixed ligand
 bis(\b-diketonato)chromium(III) complexes with a chelated nitronyl
 nitroxide radical: X-ray structure of [Cr(dpm)2(NIT2py)]PF6
;
_journal_issue                   2
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              181
_journal_page_last               187
_journal_paper_doi               10.1039/b104092h
_journal_year                    2002
_chemical_formula_moiety         '(Cr (C11 H19 O2)2 (C12 H16 N3 O2)) (F6 P)'
_chemical_formula_sum            'C34 H54 Cr F6 N3 O6 P'
_chemical_formula_weight         797.77
_chemical_melting_point          ?
_chemical_name_common            '[Cr(dpm)~2~(NIT2-py)]PF~6~'
_chemical_name_systematic
; 
Bis(2,2,6,6-tetramethylhepta-3,5-dionato)(2-(2'-(pyridyl)-4,4,5,5-tetramethyl-
4,5-dihydro-1H-imidazolyl-3-oxide-1-oxyl)chromium(III) Hexafluorophosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 137.029(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.940(4)
_cell_length_b                   31.191(12)
_cell_length_c                   13.960(4)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14.7
_cell_measurement_theta_min      12.6
_cell_volume                     4137(3)
_computing_cell_refinement       WinAFC
_computing_data_collection       WinAFC
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_molecular_graphics    'ORTEP in 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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_sigmaI/netI    0.3907
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10474
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        1.71
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0005(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.3712
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1269P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2958
_reflns_number_gt                2121
_reflns_number_total             9464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b104092h.txt
_cod_data_source_block           CrdbmNIT2py
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        4137(2)
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               7010810