Phenoxyl radical FeIII complex of cis,cis-1,3,5-tris(3',5'-di-tert-butylsalicylaldimino)cyclohexane, spectro-electrochemical and structural studies
Alison K. Nairn; Rajiv Bhalla; Simon P. Foxon; Xiaoming Liu; Lesley J. Yellowlees; Bruce C. Gilbert; Paul H. Walton; J. Chem. Soc., Dalton Trans.  (2002) 1253–1255; doi:10.1039/b200571a

data_7011498
_publ_section_title
;
 Phenoxyl radical FeIII complex of
 cis,cis-1,3,5-tris(3',5'-di-tert-butylsalicylaldimino)cyclohexane,
 spectro-electrochemical and structural studies
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1253
_journal_page_last               1255
_journal_paper_doi               10.1039/b200571a
_journal_year                    2002
_chemical_formula_moiety         '2(C51 H72 Fe N3 O3), C H2 Cl2'
_chemical_formula_sum            'C103 H146 Cl2 Fe2 N6 O6'
_chemical_formula_weight         1746.92
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             1998-06-22
_audit_creation_method           SHELXL-97
_audit_update_record
;
?
;
_cell_angle_alpha                92.62(8)
_cell_angle_beta                 108.58(6)
_cell_angle_gamma                101.36(8)
_cell_formula_units_Z            2
_cell_length_a                   16.709(18)
_cell_length_b                   19.77(2)
_cell_length_c                   16.444(12)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      6.510
_cell_measurement_theta_min      4.125
_cell_volume                     5014(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_molecular_graphics    'teXsan (MSC, 1992-1997)'
_computing_publication_material  'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF92 (Beurskens, P.T., et al, 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC6s'
_diffrn_measurement_method       \w--2\q
_diffrn_orient_matrix_UB_11      -0.04107
_diffrn_orient_matrix_UB_12      0.03038
_diffrn_orient_matrix_UB_13      -0.02413
_diffrn_orient_matrix_UB_21      0.01219
_diffrn_orient_matrix_UB_22      -0.00335
_diffrn_orient_matrix_UB_23      -0.05559
_diffrn_orient_matrix_UB_31      -0.04859
_diffrn_orient_matrix_UB_32      -0.04199
_diffrn_orient_matrix_UB_33      -0.02235
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1186
_diffrn_reflns_av_sigmaI/netI    0.3677
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14079
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        22.90
_diffrn_reflns_theta_max         22.90
_diffrn_reflns_theta_min         1.78
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.621
_diffrn_standards_interval_count 3
_diffrn_standards_number         150
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.8905
_exptl_absorpt_correction_T_min  0.7971
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         13519
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.3183
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.2111
_reflns_number_gt                3529
_reflns_number_total             13523
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            b200571a.txt
_cod_data_source_block           shelxl
_cod_database_code               7011498