Structure, spectral and electrochemical properties of the 2,6-di-tert-butylphenol-functionalized iron and cobalt(II) clathrochelates and their phenylsulfide analogs
Alexander S. Belov; Irina G. Belaya; Valentin V. Novikov; Zoya A. Starikova; Ernest V. Polshin; Alexander V. Dolganov; Ekaterina G. Lebed; Inorganica Chimica Acta 394 (2013) 269–281; doi:10.1016/j.ica.2012.08.014

data_1512752
_publ_section_title
;
 Structure, spectral and electrochemical properties of the
 2,6-di-tert-butylphenol-functionalized iron and cobalt(II)
 clathrochelates and their phenylsulfide analogs
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              269
_journal_page_last               281
_journal_paper_doi               10.1016/j.ica.2012.08.014
_journal_volume                  394
_journal_year                    2013
_chemical_formula_moiety         'C42 H30 B2 F2 Fe N6 O6 S2, 4(C6 H6)'
_chemical_formula_sum            'C66 H54 B2 F2 Fe N6 O6 S2'
_chemical_formula_weight         1206.74
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                102.485(4)
_cell_angle_beta                 94.611(4)
_cell_angle_gamma                117.329(4)
_cell_formula_units_Z            2
_cell_length_a                   12.298(3)
_cell_length_b                   13.410(3)
_cell_length_c                   20.975(4)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     2935.3(11)
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0973
_diffrn_reflns_av_sigmaI/netI    0.2068
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32312
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     646
_refine_ls_number_reflns         15407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.2472
_refine_ls_R_factor_gt           0.0781
_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^)+(0.0010P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1151
_reflns_number_gt                4922
_reflns_number_total             15407
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ICA-2013-394-269-281-3.cif
_cod_data_source_block           fin
_cod_original_cell_volume        2935.4(10)
_cod_database_code               1512752