#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/42/2014274.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2014274
loop_
_publ_author_name
'Batten, Michael P.'
'Canty, Allan J.'
'Cavell, Kingsley J.'
'Rüther, Thomas'
'Skelton, Brian W.'
'White, Allan H.'
_publ_section_title
;Tris[bis(1-methyl-1H-imidazol-2-yl)methanone-κ²N³]iron(II)
 dichloride 5.5-hydrate,
 cis-bis[bis(1-methyl-1H-imidazol-2-yl)methanone-κ²N³]dichloroiron(II)
 (ca 153 K) and
 di-μ-chloro-bis{[bis(1-methyl-1H-imidazol-2-yl)methanone-κ²N³]chloroiron(II)}
 methanol disolvate (ca 300 K)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m316
_journal_page_last               m319
_journal_paper_doi               10.1107/S0108270104010881
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Fe2 Cl4 (C9 H10 N4 O)2], 2C H4 O1'
_chemical_formula_moiety         'C18 H16 Cl4 Fe2 N8 O2, 2(C H4 O)'
_chemical_formula_sum            'C20 H24 Cl4 Fe2 N8 O4'
_chemical_formula_weight         693.97
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                93.175(5)
_cell_angle_beta                 108.871(4)
_cell_angle_gamma                113.923(4)
_cell_formula_units_Z            1
_cell_length_a                   8.358(3)
_cell_length_b                   9.215(3)
_cell_length_c                   10.650(4)
_cell_measurement_reflns_used    2043
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.35
_cell_measurement_theta_min      2.48
_cell_volume                     692.8(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    Xtal3.5
_computing_publication_material  'BONDLA and CIFIO in Xtal3.5'
_computing_structure_refinement  'CRYLSQ in Xtal3.5'
_computing_structure_solution
;
Xtal3.5 (Hall et al., 1995)
;
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .024
_diffrn_reflns_av_sigmaI/netI    .078
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6649
_diffrn_reflns_theta_full        27.04
_diffrn_reflns_theta_max         27.04
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  (SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             352
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .1
_refine_diff_density_max         1.520
_refine_diff_density_min         -.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   .958
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2085
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .091
_refine_ls_R_factor_gt           .067
_refine_ls_shift/su_max          .018
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
   w = 1/(σ²(F^^2) +  0.58F²)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .155
_refine_ls_wR_factor_ref         .146
_reflns_number_gt                2200
_reflns_number_total             3012
_reflns_threshold_expression     'I > 2.00 σ(I)'
_cod_data_source_file            ta1447.cif
_cod_data_source_block           III
_cod_original_sg_symbol_Hall     -p_1
_cod_original_sg_symbol_H-M      P_-1
_cod_database_code               2014274
_cod_database_fobs_code          2014274
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe .52639(18) .63381(14) .37401(12) .0405(5) Uani ? ? 1.00000 ? ?
Cl1 .5077(4) .6406(3) .5995(3) .0689(12) Uani ? ? 1.00000 ? ?
Cl2 .2435(3) .6145(3) .2333(2) .0584(11) Uani ? ? 1.00000 ? ?
N11 .7129(9) .8896(8) .4305(7) .043(3) Uani ? ? 1.00000 ? ?
C12 .8073(11) .9828(9) .3613(8) .040(3) Uani ? ? 1.00000 ? ?
N13 .8715(10) 1.1419(8) .4142(7) .044(3) Uani ? ? 1.00000 ? ?
C131 .9800(15) 1.2867(10) .3711(11) .063(5) Uani ? ? 1.00000 ? ?
C14 .8134(13) 1.1497(10) .5187(9) .050(4) Uani ? ? 1.00000 ? ?
C15 .7174(13) .9954(10) .5285(9) .049(4) Uani ? ? 1.00000 ? ?
C10 .8387(12) .9261(10) .2440(9) .044(3) Uani ? ? 1.00000 ? ?
O10 .9179(10) 1.0235(7) .1847(7) .064(3) Uani ? ? 1.00000 ? ?
N21 .6779(10) .6310(8) .2457(7) .046(3) Uani ? ? 1.00000 ? ?
C22 .7774(11) .7526(9) .1985(8) .040(3) Uani ? ? 1.00000 ? ?
N23 .8176(10) .6939(8) .0993(7) .046(3) Uani ? ? 1.00000 ? ?
C231 .9235(15) .7813(12) .0180(10) .065(5) Uani ? ? 1.00000 ? ?
C24 .7427(15) .5300(12) .0846(10) .058(4) Uani ? ? 1.00000 ? ?
C25 .6561(15) .4921(11) .1741(10) .058(4) Uani ? ? 1.00000 ? ?
O1 .4474(10) .0533(8) .1629(8) .0080(16) Uiso ? ? .50000 ? ?
C1 .455(2) -.013(2) .0634(14) .025(3) Uiso ? ? .50000 ? ?
O1' .4692(13) .0480(12) .1112(12) .024(2) Uiso ? ? .50000 ? ?
C1' .420(2) -.092(2) .0331(17) .044(4) Uiso ? ? .50000 ? ?
H131a 1.02863 1.38466 .43644 .09300 Uiso ? ? 1.00000 ? ?
H131b .90677 1.29622 .28556 .09300 Uiso ? ? 1.00000 ? ?
H131c 1.08898 1.28050 .36278 .09300 Uiso ? ? 1.00000 ? ?
H14 .84069 1.24822 .57651 .05900 Uiso ? ? 1.00000 ? ?
H15 .65962 .96324 .59471 .06000 Uiso ? ? 1.00000 ? ?
H231a .84394 .80462 -.05571 .09700 Uiso ? ? 1.00000 ? ?
H231b .97004 .71568 -.01825 .09700 Uiso ? ? 1.00000 ? ?
H231c 1.02933 .88003 .07354 .09700 Uiso ? ? 1.00000 ? ?
H24 .74984 .45442 .02253 .06800 Uiso ? ? 1.00000 ? ?
H25 .58783 .38331 .18410 .07000 Uiso ? ? 1.00000 ? ?
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Cl .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Fe .301 .845 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Fe Cl2 . 104.48(13) yes
Cl1 Fe N11 . 90.4(2) yes
Cl1 Fe N21 . 149.8(2) ?
Cl1 Fe Cl1 '2 666' 80.68(11) yes
Cl2 Fe N11 . 104.4(2) yes
Cl2 Fe N21 . 105.6(2) yes
Cl2 Fe Cl1 '2 666' 109.42(10) yes
N11 Fe N21 . 83.5(3) yes
N11 Fe Cl1 '2 666' 146.2(2) yes
N21 Fe Cl1 '2 666' 88.0(2) yes
Fe Cl1 Fe '2 666' 99.32(12) yes
Fe N11 C12 . 128.7(6) ?
Fe N11 C15 . 123.7(6) ?
C12 N11 C15 . 105.6(7) ?
N11 C12 N13 . 110.3(9) ?
N11 C12 C10 . 126.6(7) ?
N13 C12 C10 . 123.1(8) ?
C12 N13 C131 . 129.4(9) ?
C12 N13 C14 . 107.3(7) ?
C131 N13 C14 . 123.3(8) ?
N13 C131 H131a . 112.1 ?
N13 C131 H131b . 112.0 ?
N13 C131 H131c . 109.9 ?
H131a C131 H131b . 108.9 ?
H131a C131 H131c . 105.9 ?
H131b C131 H131c . 107.8 ?
N13 C14 C15 . 107.1(9) ?
N13 C14 H14 . 125.7 ?
C15 C14 H14 . 127.1 ?
N11 C15 C14 . 109.7(9) ?
N11 C15 H15 . 124.7 ?
C14 C15 H15 . 125.6 ?
C12 C10 O10 . 120.2(8) ?
C12 C10 C22 . 120.1(8) ?
O10 C10 C22 . 119.7(9) ?
Fe N21 C22 . 129.0(7) ?
Fe N21 C25 . 123.8(6) ?
C22 N21 C25 . 106.0(9) ?
C10 C22 N21 . 126.8(9) ?
C10 C22 N23 . 123.0(8) ?
N21 C22 N23 . 110.2(8) ?
C22 N23 C231 . 129.8(8) ?
C22 N23 C24 . 107.4(8) ?
C231 N23 C24 . 122.8(10) ?
N23 C231 H231a . 110.4 ?
N23 C231 H231b . 110.1 ?
N23 C231 H231c . 110.1 ?
H231a C231 H231b . 108.4 ?
H231a C231 H231c . 109.7 ?
H231b C231 H231c . 108.1 ?
N23 C24 C25 . 106.9(10) ?
N23 C24 H24 . 126.8 ?
C25 C24 H24 . 126.3 ?
N21 C25 C24 . 109.5(8) ?
N21 C25 H25 . 125.6 ?
C24 C25 H25 . 124.9 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe Cl1 . . 2.455(4) yes
Fe Cl2 . . 2.282(3) yes
Fe N11 . . 2.146(6) yes
Fe N21 . . 2.148(10) yes
Fe Cl1 . '2 666' 2.470(3) yes
N11 C12 . . 1.342(12) ?
N11 C15 . . 1.368(13) ?
C12 N13 . . 1.353(11) ?
C12 C10 . . 1.467(15) ?
N13 C131 . . 1.473(12) ?
N13 C14 . . 1.359(14) ?
C131 H131a . . .957 ?
C131 H131b . . .951 ?
C131 H131c . . .967 ?
C14 C15 . . 1.350(12) ?
C14 H14 . . .967 ?
C15 H15 . . .972 ?
C10 O10 . . 1.222(12) ?
C10 C22 . . 1.464(12) ?
N21 C22 . . 1.333(11) ?
N21 C25 . . 1.366(14) ?
C22 N23 . . 1.355(14) ?
N23 C231 . . 1.475(15) ?
N23 C24 . . 1.357(12) ?
C231 H231a . . .949 ?
C231 H231b . . .964 ?
C231 H231c . . .953 ?
C24 C25 . . 1.354(18) ?
C24 H24 . . .966 ?
C25 H25 . . .964 ?
O1 C1 . . 1.22(2) ?
O1' C1' . . 1.33(2) ?
