Template synthesis, X-ray structure, spectral and redox properties of the paramagnetic alkylboron-capped cobalt(II) clathrochelates and their diamagnetic iron(II)-containing analogs
Yan Z. Voloshin; Andrey Y. Lebedev; Valentin V. Novikov; Alexander V. Dolganov; Anna V. Vologzhanina; Ekaterina G. Lebed; Alexander A. Pavlov; Zoya A. Starikova; Michail I. Buzin; Yurii N. Bubnov; Inorganica Chimica Acta 399 (2013) 67–78; doi:

data_1516853
_publ_section_title
;
 Template synthesis, X-ray structure, spectral and redox properties of the
 paramagnetic alkylboron-capped cobalt(II) clathrochelates and their
 diamagnetic iron(II)-containing analogs
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              67
_journal_page_last               78
_journal_volume                  399
_journal_year                    2013
_chemical_formula_moiety         'C50 H48 B2 Fe N6 O6, C7 H16'
_chemical_formula_sum            'C57 H64 B2 Fe N6 O6'
_chemical_formula_weight         1006.61
_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                85.743(6)
_cell_angle_beta                 81.421(5)
_cell_angle_gamma                68.943(5)
_cell_formula_units_Z            2
_cell_length_a                   10.566(3)
_cell_length_b                   14.168(4)
_cell_length_c                   18.767(5)
_cell_measurement_reflns_used    468
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.86
_cell_measurement_theta_min      1.99
_cell_volume                     2591.8(12)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Apex II CCD area detector'
_diffrn_measurement_method       '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  0.0834
_diffrn_reflns_av_sigmaI/netI    0.1219
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24116
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.305
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         10141
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0123P)^2^+2.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                5856
_reflns_number_total             10141
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ICA-2013-399-67-78-2.CIF
_cod_data_source_block           final
_cod_original_cell_volume        2591.9(11)
_cod_database_code               1516853