π-Extended and Six-Coordinate Iron(II) Complexes: Structures, Magnetic Properties, and the Electrochemical Synthesis of a Conducting Iron(II) Metallopolymer
Brandon Djukic; Takele Seda; Serge I. Gorelsky; Alan J. Lough; Martin T. Lemaire; Inorganic Chemistry 50 (2011) 7334–7343; doi:10.1021/ic2010503

data_4325832
_publ_section_title
;
 \p-Extended and Six-Coordinate Iron(II) Complexes: Structures, Magnetic
 Properties, and the Electrochemical Synthesis of a Conducting Iron(II)
 Metallopolymer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7334
_journal_page_last               7343
_journal_paper_doi               10.1021/ic2010503
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C50 H36 Fe N6 S2, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C50.5 H37 Cl Fe N6 S2'
_chemical_formula_weight         883.28
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.551(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3899(11)
_cell_length_b                   9.6294(6)
_cell_length_c                   26.6152(17)
_cell_measurement_reflns_used    29494
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.7
_cell_volume                     4293.7(5)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.1196
_diffrn_reflns_av_sigmaI/netI    0.1118
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29494
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  1.048
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995) 
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       needle
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         7436
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.0923
_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^)+(0.0700P)^2^+9.4468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2001
_refine_ls_wR_factor_ref         0.2482
_reflns_number_gt                3790
_reflns_number_total             7436
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic2010503_si_004.cif
_cod_data_source_block           k09136
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C50.50 H37 Cl Fe N6 S2'
_cod_database_code               4325832