Synthesis, Structure, and Solution Properties of [(mim-TASN)FeCl2]+ and Its μ-Oxo Derivative
Jinlan Cui; Mark S. Mashuta; Robert M. Buchanan; Craig A. Grapperhaus; Inorganic Chemistry 49 (2010) 10427–10435; doi:10.1021/ic1012999

data_4317011
_publ_contact_author_email       grapperhaus@louisville.edu
_publ_contact_author_fax         '(502)852-8149 '
_publ_contact_author_phone       '(502)852-5932 '
_publ_section_title
;
 Synthesis, Structure, and Solution Properties of [(mim-TASN)FeCl2]+ and
 Its \m-Oxo Derivative
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10427
_journal_page_last               10435
_journal_paper_doi               10.1021/ic1012999
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C11 H20 Cl2 Fe N4 S, Cl4 Fe'
_chemical_formula_sum            'C11 H20 Cl6 Fe2 N4 S'
_chemical_formula_weight         564.77
_chemical_name_common
; 
 dichloro(4-((1-methyl-1H-imidazol-2-yl)methyl)-
 1-thia-4,7-diazacyclononane)iron(III) tetrachloroferrate(III)
;
_chemical_name_systematic
; 
 dichloro(4-((1-methyl-1H-imidazol-2-yl)methyl)-
 1-thia-4,7-diazacyclononane)iron(III) tetrachloroferrate(III)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
  Jan_22_2010 text and data added by Mark S. Mashuta
  Feb_1_2010 text and data added by Mark S. Mashuta
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.2420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0605(6)
_cell_length_b                   10.4331(5)
_cell_length_c                   16.1935(7)
_cell_measurement_reflns_used    5254
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.56
_cell_volume                     2070.27(16)
_computing_cell_refinement       'SAINT 6.36 (Bruker, 2002)'
_computing_data_collection       'SMART 5.628 (Bruker, 2002)'
_computing_data_reduction        'SAINT 6.36 (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'SMART APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18134
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.279
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, (1996).
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0318P)^2^+1.3222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                4294
_reflns_number_total             4911
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic1012999_si_002_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4317011