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_7013612
_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         'C22 H30 Cl Cr N3 O6, 0.5(H2 O)'
_chemical_formula_sum            'C22 H31 Cl Cr N3 O6.5'
_chemical_formula_weight         528.95
_chemical_name_common
;
cis-Chlorobis(pentane-2,4-dionato)(4,4,5,5-tetramethyl-2-(3-
pyridyl)imidazolin-1-oxyl 3-oxide)chromium(iii) Hemihydrate
;
_chemical_name_systematic
;
cis-Chlorobis(pentane-2,4-dionato)(4,4,5,5-tetramethyl-2-(3-pyridyl)imidazolin-
1-oxyl 3-oxide)chromium(III) Hemihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                64.436(14)
_cell_angle_beta                 89.618(17)
_cell_angle_gamma                67.315(15)
_cell_formula_units_Z            2
_cell_length_a                   11.195(2)
_cell_length_b                   11.638(3)
_cell_length_c                   12.362(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     1315.6(5)
_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 5R'
_diffrn_measurement_device_type  'Rigaku 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     0.71069
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0887
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8023
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0.18
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            dark_blue
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details centrosymmetric
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment
'constr except for the H atoms of hydrated molecule which did not included'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         7694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                3787
_reflns_number_total             7694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b310571g.txt
_cod_data_source_block           ClNIT3py
_cod_original_cell_volume        1315.6(4)
_cod_database_code               7013612