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_1512751
_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_sum            'C101 H151 B2 Fe N6 O12 S6'
_chemical_formula_weight         1911.11
_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                80.973(7)
_cell_angle_beta                 89.983(5)
_cell_angle_gamma                61.829(5)
_cell_formula_units_Z            2
_cell_length_a                   14.370(4)
_cell_length_b                   15.159(5)
_cell_length_c                   30.681(8)
_cell_measurement_temperature    393(2)
_cell_volume                     5798(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      393(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0596
_diffrn_reflns_av_sigmaI/netI    0.1008
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            67044
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         0.67
_exptl_absorpt_coefficient_mu    0.292
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2054
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1153
_refine_ls_number_reflns         32936
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1540
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.531
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+7.0640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1839
_refine_ls_wR_factor_ref         0.2086
_reflns_number_gt                18037
_reflns_number_total             32936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-269-281-2.cif
_cod_data_source_block           fin
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512751