Clathrochelate monoribbed-functionalized iron(ii) α-dioximates: synthetic pathways and structural and electrochemical features
Voloshin, Yan Z.; Zavodnik, Valery E.; Varzatskii, Oleg A.; Belsky, Vitaly K.; Palchik, Aleksei V.; Strizhakova, Nataly G.; Vorontsov, Ivan I.; Antipin, Mikhail Yu.; Journal of the Chemical Society, Dalton Transactions  (2002) 1193–; doi:10.1039/b107021p

data_7702699
_publ_section_title
;
 Clathrochelate monoribbed-functionalized iron(ii) \a-dioximates:
 synthetic pathways and structural and electrochemical features
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1193
_journal_paper_doi               10.1039/b107021p
_journal_year                    2002
_chemical_formula_sum            'C32 H26 B2 F2 Fe N6 O6 S2'
_chemical_formula_weight         770.18
_chemical_name_systematic
;
1,8-Bis(fluoroboro)-2,7,9,14,15,20-hexaoxa-3,6,10,13,16,19-hexaaza-
4,5,11,12-tetraphenyl-17,18-methylthiobicyclo-[6.6.6]eicosa-3,5,10,12,16,18-
hexaene iron(II)
;
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9930(10)
_cell_length_b                   9.9930(10)
_cell_length_c                   34.575(7)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      2
_cell_volume                     3452.7(9)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        XCAD4NEW
_computing_molecular_graphics    'SHELXTL PLUS 5.0'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.752
_diffrn_measured_fraction_theta_max 0.752
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\q/2\q scans'
_diffrn_radiation_monochromator  filter
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2639
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        6.8
_diffrn_standards_interval_time  100
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  0.8258
_exptl_absorpt_correction_T_min  0.7802
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1348P)^2^+3.0994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1697
_reflns_number_gt                2401
_reflns_number_total             2402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107021p.txt
_cod_data_source_block           13
_cod_original_sg_symbol_H-M      P4(1)2(1)2
_cod_database_code               7702699