Interaction of Dichloride Iron(II) Clathrochelate with Dimercaptomaleodinitrile: Synthesis of the Precursor Monoribbed-Functionalized Phthalocyaninoclathrochelates and the Unexpected Formation of a New Thiophene-Containing Heterocyclic System in the Ribbed Chelate Fragment of the Clathrochelate Framework
Yan Z. Voloshin; Oleg A. Varzatskii; Alexander S. Belov; Zoya A. Starikova; Kyrill Y. Suponitsky; Valentin V. Novikov; Yurii N. Bubnov; Inorganic Chemistry 47 (2008) 2155–2161; doi:10.1021/ic701452g

data_4304081
_publ_section_title
;
Interaction of Dichloride Iron(II) Clathrochelate with
Dimercaptomaleodinitrile: Synthesis of the Precursor
Monoribbed-Functionalized Phthalocyaninoclathrochelates and the Unexpected
Formation of a New Thiophene-Containing Heterocyclic System in the Ribbed
Chelate Fragment of the Clathrochelate Framework
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2155
_journal_page_last               2161
_journal_paper_doi               10.1021/ic701452g
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
'C35 H21 B2 F2 Fe N9 O8 S2, 2.5(C3 H6 O), 0.5(C7 H16)'
_chemical_formula_sum            'C46 H44 B2 F2 Fe N9 O10.5 S2'
_chemical_formula_weight         1070.49
_chemical_name_systematic
; 
 ? 
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.312(2)
_cell_angle_beta                 80.917(2)
_cell_angle_gamma                68.869(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9309(10)
_cell_length_b                   11.9718(10)
_cell_length_c                   19.2325(16)
_cell_measurement_reflns_used    2810
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      2.23
_cell_volume                     2511.7(4)
_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, 1998)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART APEX2 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  0.0722
_diffrn_reflns_av_sigmaI/netI    0.1023
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25811
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.325
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         10785
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0350P)^2^+6.8500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1575
_reflns_number_gt                6598
_reflns_number_total             10785
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic701452g_si_002_2.cif
_cod_data_source_block           comp3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C46 H44 B2 F2 Fe N9 O10.50 S2'
_cod_database_code               4304081