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_1512750
_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
'C44 H42 B2 F2 Fe N6 O7 S, 3(C6 H6), 0.25(C8 H18)'
_chemical_formula_sum            'C64 H64.5 B2 F2 Fe N6 O7 S'
_chemical_formula_weight         1177.25
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.566(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.457(5)
_cell_length_b                   12.344(3)
_cell_length_c                   25.909(6)
_cell_measurement_reflns_used    880
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.66
_cell_measurement_theta_min      2.29
_cell_volume                     6767(3)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.1319
_diffrn_reflns_av_sigmaI/netI    0.1770
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            45558
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2466
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         11806
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1816
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0505P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                4470
_reflns_number_total             11806
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ICA-2013-394-269-281-1.cif
_cod_data_source_block           fin
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C64 H64.50 B2 F2 Fe N6 O7 S'
_cod_database_code               1512750