Syntheses, structures, magnetic and spectroscopic properties of bis(pentane-2,4-dionato)chromium(iii) complexes incorporating 3- or 4-pyridyl-substituted nitronyl and imino nitroxides
Iino, Atsushi; Suzuki, Takayoshi; Kaizaki, Sumio; Dalton Transactions  (2003) 4604–; doi:10.1039/b310571g

data_7013615
_publ_section_title
;
 Syntheses, structures, magnetic and spectroscopic properties of
 bis(pentane-2,4-dionato)chromium(iii) complexes incorporating 3- or
 4-pyridyl-substituted nitronyl and imino nitroxides
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4604
_journal_paper_doi               10.1039/b310571g
_journal_year                    2003
_chemical_formula_moiety         'C20 H24 Cr N2 O4 1+, F6 P -1'
_chemical_formula_sum            'C20 H24 Cr F6 N2 O4 P'
_chemical_formula_weight         553.38
_chemical_name_common
;trans-bis(pentane-2,4-dionato)bis(pyridine)chromium(iii)
Hexafluorophosphate
;
_chemical_name_systematic
;
trans-bis(pentane-2,4-dionato)bis(pyridine)chromium(III) Hexafluorophosphate
;
_space_group_IT_number           98
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw 2bw'
_symmetry_space_group_name_H-M   'I 41 2 2'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8690(10)
_cell_length_b                   12.869
_cell_length_c                   15.1892(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.7
_cell_volume                     2515.5(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Rigaku AFC 7R'
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0086
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2055
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0.99
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack analysis; the parameter was 0.06(6)'
_refine_ls_abs_structure_Flack   0.06(6)
_refine_ls_extinction_coef       0.0044(9)
_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   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0872P)^2^+1.2340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                822
_reflns_number_total             1310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b310571g.txt
_cod_data_source_block           transpy
_cod_database_code               7013615