Apically linked iron(II) α-dioximate and α-oximehydrazonate bis-clathrochelates: synthesis, structure and electrocatalytic properties.
Belaya, Irina G.; Svidlov, Semen V.; Dolganov, Alexander V.; Zelinskii, Genrikh E.; Potapova, Tamara V.; Vologzhanina, Anna V.; Varzatskii, Oleg A.; Bubnov, Yurii N.; Voloshin, Yan Z.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 13667–13678; doi:10.1039/c3dt50881a

data_7023164
_publ_section_title
;
 Apically linked iron(II) \a-dioximate and \a-oximehydrazonate
 bis-clathrochelates: synthesis, structure and electrocatalytic
 properties.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13667
_journal_page_last               13678
_journal_paper_doi               10.1039/c3dt50881a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C50 H70 B4 Fe2 N12 O12, 2(C H2 Cl2)'
_chemical_formula_sum            'C52 H74 B4 Cl4 Fe2 N12 O12'
_chemical_formula_weight         1355.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                110.849(7)
_cell_angle_beta                 104.086(7)
_cell_angle_gamma                104.756(5)
_cell_formula_units_Z            1
_cell_length_a                   9.866(2)
_cell_length_b                   13.363(3)
_cell_length_c                   13.750(5)
_cell_measurement_reflns_used    789
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.76
_cell_measurement_theta_min      2.49
_cell_volume                     1522.2(7)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Apex 2 CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1432
_diffrn_reflns_av_unetI/netI     0.1637
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19293
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.706
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.722
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_description       plate
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0100P)^2^]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3388
_reflns_number_total             5979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt50881a.txt
_cod_data_source_block           Fe2Nx6B2Bu2BC6H4B
_cod_original_cell_volume        1522.2(8)
_cod_database_code               7023164
_shelxl_version_number           2013-2