#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:35:12 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179797 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/93/7009361.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7009361
loop_
_publ_author_name
'Abrahams, Brendan F.'
'Lu, Kevin D.'
'Moubaraki, Boujemaa'
'Murray, Keith S.'
'Robson, Richard'
_publ_section_title
;
 X-Ray diffraction and magnetic studies on a series of isostructural
 divalent metal chloranilates with zigzag polymeric chain structures
 and on a dinuclear iron(III) chloranilate †
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1793
_journal_paper_doi               10.1039/b000192i
_journal_year                    2000
_chemical_formula_sum            'C18 H16 Cl6 Fe2 O20'
_chemical_formula_weight         876.71
_chemical_name_systematic
;
 tetraaquatris(chloranilato)diiron(III) tetrahydrate
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.91(2)
_cell_angle_beta                 78.45(2)
_cell_angle_gamma                75.59(3)
_cell_formula_units_Z            1
_cell_length_a                   6.909(2)
_cell_length_b                   9.894(4)
_cell_length_c                   11.391(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.1
_cell_measurement_theta_min      9.8
_cell_volume                     720.5(4)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       ω:2θ
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3321
_diffrn_reflns_theta_full        75.17
_diffrn_reflns_theta_max         75.17
_diffrn_reflns_theta_min         4.06
_diffrn_standards_decay_%        'No obsevable decay'
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    14.039
_exptl_absorpt_correction_T_max  0.4179
_exptl_absorpt_correction_T_min  0.2166
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELX-76 (G. Sheldrick, 1976)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2852
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0454
_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/[σ²(Fo²)+(0.0887P)²+0.0959P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                2465
_reflns_number_total             2852
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b000192i.txt
_cod_data_source_block           fecankl2abs97
_cod_database_code               7009361
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.17939(8) 0.19912(5) 0.25406(5) 0.02048(17) Uani 1 1 d . . .
Cl1 Cl 0.12616(13) 0.10044(11) -0.14700(9) 0.0318(2) Uani 1 1 d . . .
O1 O 0.1617(4) 0.1624(3) 0.0906(2) 0.0242(5) Uani 1 1 d . . .
O2 O 0.4612(4) 0.0770(3) 0.2137(2) 0.0222(5) Uani 1 1 d . . .
C1 C 0.3136(5) 0.0852(4) 0.0426(3) 0.0197(6) Uani 1 1 d . . .
C2 C 0.4935(5) 0.0356(3) 0.1140(3) 0.0202(7) Uani 1 1 d . . .
C3 C 0.3298(5) 0.0464(4) -0.0680(3) 0.0215(7) Uani 1 1 d . . .
Cl2 Cl 0.24254(15) 0.38110(10) 0.60799(9) 0.0321(2) Uani 1 1 d . . .
Cl3 Cl 0.32021(16) 0.67676(10) 0.03912(9) 0.0332(2) Uani 1 1 d . . .
O3 O 0.2636(4) 0.3817(3) 0.1634(2) 0.0262(5) Uani 1 1 d . . .
O4 O 0.2452(4) 0.2573(3) 0.3924(2) 0.0249(5) Uani 1 1 d . . .
O5 O 0.2407(5) 0.6911(3) 0.4898(3) 0.0356(7) Uani 1 1 d . . .
O6 O 0.2945(5) 0.8114(3) 0.2500(3) 0.0337(6) Uani 1 1 d . . .
C4 C 0.2758(5) 0.4610(4) 0.2339(3) 0.0214(7) Uani 1 1 d . . .
C5 C 0.2637(5) 0.3888(4) 0.3683(3) 0.0215(7) Uani 1 1 d . . .
C6 C 0.2646(5) 0.4631(4) 0.4540(3) 0.0229(7) Uani 1 1 d . . .
C7 C 0.2631(5) 0.6130(4) 0.4186(4) 0.0246(7) Uani 1 1 d . . .
C8 C 0.2894(5) 0.6840(4) 0.2796(4) 0.0246(7) Uani 1 1 d . . .
C9 C 0.2990(6) 0.5998(4) 0.1936(3) 0.0238(7) Uani 1 1 d . . .
O7 O -0.1133(4) 0.3030(3) 0.2698(3) 0.0306(6) Uani 1 1 d D . .
H1 H -0.165(8) 0.309(6) 0.338(3) 0.054(12) Uiso 1 1 d D . .
H2 H -0.124(9) 0.372(4) 0.215(4) 0.054(12) Uiso 1 1 d D . .
O8 O 0.0906(4) 0.0269(3) 0.3620(3) 0.0270(6) Uani 1 1 d D . .
H3 H 0.172(7) -0.044(4) 0.355(6) 0.064(14) Uiso 1 1 d D . .
H4 H -0.025(5) 0.020(7) 0.376(6) 0.064(14) Uiso 1 1 d D . .
O9 O 0.2872(5) -0.0062(4) 0.5865(3) 0.0408(7) Uani 1 1 d . . .
O10 O 0.1885(6) 0.4507(4) 0.8972(3) 0.0472(8) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Fe1 O8 92.92(11) . . ?
O4 Fe1 O3 80.65(11) . . ?
O8 Fe1 O3 173.15(11) . . ?
O4 Fe1 O1 167.11(11) . . ?
O8 Fe1 O1 98.34(12) . . ?
O3 Fe1 O1 88.32(11) . . ?
O4 Fe1 O7 95.64(12) . . ?
O8 Fe1 O7 87.98(12) . . ?
O3 Fe1 O7 90.28(12) . . ?
O1 Fe1 O7 91.02(11) . . ?
O4 Fe1 O2 95.43(11) . . ?
O8 Fe1 O2 89.85(11) . . ?
O3 Fe1 O2 93.11(11) . . ?
O1 Fe1 O2 78.43(10) . . ?
O7 Fe1 O2 168.81(11) . . ?
C1 O1 Fe1 116.7(2) . . ?
C2 O2 Fe1 115.7(2) . . ?
O1 C1 C3 125.4(3) . . ?
O1 C1 C2 115.1(3) . . ?
C3 C1 C2 119.5(3) . . ?
O2 C2 C3 126.0(3) . 2_655 ?
O2 C2 C1 114.0(3) . . ?
C3 C2 C1 120.0(3) 2_655 . ?
C2 C3 C1 120.5(3) 2_655 . ?
C2 C3 Cl1 120.2(3) 2_655 . ?
C1 C3 Cl1 119.4(3) . . ?
C4 O3 Fe1 113.7(2) . . ?
C5 O4 Fe1 114.2(2) . . ?
O3 C4 C9 124.3(3) . . ?
O3 C4 C5 114.6(3) . . ?
C9 C4 C5 121.1(3) . . ?
O4 C5 C6 125.1(3) . . ?
O4 C5 C4 114.2(3) . . ?
C6 C5 C4 120.6(3) . . ?
C5 C6 C7 120.5(3) . . ?
C5 C6 Cl2 120.3(3) . . ?
C7 C6 Cl2 118.9(3) . . ?
O5 C7 C6 125.0(4) . . ?
O5 C7 C8 116.8(3) . . ?
C6 C7 C8 118.2(3) . . ?
O6 C8 C9 123.6(4) . . ?
O6 C8 C7 117.7(3) . . ?
C9 C8 C7 118.7(3) . . ?
C4 C9 C8 120.3(3) . . ?
C4 C9 Cl3 119.8(3) . . ?
C8 C9 Cl3 119.8(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O4 1.978(3) . ?
Fe1 O8 1.980(3) . ?
Fe1 O3 1.995(3) . ?
Fe1 O1 2.020(3) . ?
Fe1 O7 2.023(3) . ?
Fe1 O2 2.055(3) . ?
Cl1 C3 1.719(3) . ?
O1 C1 1.254(4) . ?
O2 C2 1.266(4) . ?
C1 C3 1.386(5) . ?
C1 C2 1.530(4) . ?
C2 C3 1.377(5) 2_655 ?
C3 C2 1.377(5) 2_655 ?
Cl2 C6 1.724(4) . ?
Cl3 C9 1.718(4) . ?
O3 C4 1.287(4) . ?
O4 C5 1.291(4) . ?
O5 C7 1.223(4) . ?
O6 C8 1.225(4) . ?
C4 C9 1.369(5) . ?
C4 C5 1.506(5) . ?
C5 C6 1.368(5) . ?
C6 C7 1.430(5) . ?
C7 C8 1.550(5) . ?
C8 C9 1.425(5) . ?
