#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:14:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179368 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/65/4326594.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_4326594
loop_
_publ_author_name
'Christopher J. Adams'
'M. Carmen Muñoz'
'Rachel E. Waddington'
'José Antonio Real'
_publ_section_title
;
 Cooperative Spin Transition in the Two-Dimensional Coordination Polymer
 [Fe(4,4'-bipyridine)2(NCX)2].4CHCl3 (X = S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10633
_journal_page_last               10642
_journal_paper_doi               10.1021/ic200932w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C52 H40 Cl24 Fe2 N12 S4'
_chemical_formula_weight         1923.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 117.757(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.6810(8)
_cell_length_b                   22.6170(6)
_cell_length_c                   17.2920(7)
_cell_measurement_temperature    120(1)
_cell_volume                     7849.7(6)
_computing_cell_refinement       'HKL DENZO'
_computing_data_collection       COLLECT
_computing_data_reduction        'HKL DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.1144
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25899
_diffrn_reflns_theta_full        28.95
_diffrn_reflns_theta_max         28.95
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_T_max  0.9485
_exptl_absorpt_correction_T_min  0.8779
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.412
_refine_diff_density_min         -1.410
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         9281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.1241
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0620P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                4667
_reflns_number_total             9281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200932w_si_002_3.cif
_cod_data_source_block           NCS@120K
_cod_original_cell_volume        7849.7(5)
_cod_database_code               4326594
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Fe1 Fe 0.5000 0.09408(4) 0.7500 0.01008(19) Uani 1 2 d S
Fe2 Fe 1.0000 0.09377(4) 0.7500 0.01003(19) Uani 1 2 d S
S1 S 0.39775(6) 0.08607(6) 0.44110(8) 0.0282(3) Uani 1 1 d .
S2 S 0.93126(6) 0.10472(6) 0.43987(8) 0.0313(3) Uani 1 1 d .
N1 N 0.58664(15) 0.09363(14) 0.7458(2) 0.0087(7) Uani 1 1 d .
N3 N 0.5000 0.1824(2) 0.7500 0.0110(11) Uani 1 2 d S
N2 N 0.5000 0.0062(2) 0.7500 0.0135(11) Uani 1 2 d S
N4 N 0.45217(16) 0.09363(15) 0.6225(2) 0.0123(8) Uani 1 1 d .
N5 N 0.89864(15) 0.09057(15) 0.7446(2) 0.0119(7) Uani 1 1 d .
N7 N 0.5000 0.4957(2) 0.7500 0.0132(11) Uani 1 2 d S
N8 N 0.95488(17) 0.09862(15) 0.6135(2) 0.0145(8) Uani 1 1 d .
N6 N 0.5000 -0.3071(2) 0.7500 0.0148(11) Uani 1 2 d S
C1 C 0.5946(2) 0.06399(19) 0.6833(3) 0.0151(10) Uani 1 1 d .
H1 H 0.5583 0.0438 0.6407 0.016(3) Uiso 1 1 calc R
C2 C 0.6536(2) 0.06224(19) 0.6798(3) 0.0146(10) Uani 1 1 d .
H2 H 0.6567 0.0410 0.6358 0.016(3) Uiso 1 1 calc R
C3 C 0.70896(18) 0.09221(18) 0.7421(3) 0.0101(9) Uani 1 1 d .
C4 C 0.7013(2) 0.12278(18) 0.8054(3) 0.0151(10) Uani 1 1 d .
H4 H 0.7371 0.1433 0.8483 0.016(3) Uiso 1 1 calc R
C5 C 0.6401(2) 0.12298(17) 0.8053(3) 0.0124(9) Uani 1 1 d .
H5 H 0.6359 0.1444 0.8484 0.016(3) Uiso 1 1 calc R
C6 C 0.77477(19) 0.09062(19) 0.7422(3) 0.0134(9) Uani 1 1 d .
C7 C 0.7813(2) 0.1058(2) 0.6694(3) 0.0200(10) Uani 1 1 d .
H7 H 0.7439 0.1161 0.6179 0.016(3) Uiso 1 1 calc R
C8 C 0.8431(2) 0.10572(19) 0.6728(3) 0.0183(10) Uani 1 1 d .
H8 H 0.8464 0.1167 0.6232 0.016(3) Uiso 1 1 calc R
C9 C 0.8921(2) 0.07407(19) 0.8148(3) 0.0161(10) Uani 1 1 d .
H9 H 0.9299 0.0621 0.8649 0.016(3) Uiso 1 1 calc R
C10 C 0.8317(2) 0.0742(2) 0.8155(3) 0.0180(10) Uani 1 1 d .
H10 H 0.8294 0.0632 0.8659 0.016(3) Uiso 1 1 calc R
C11 C 0.5542(2) -0.02480(18) 0.8044(3) 0.0167(10) Uani 1 1 d .
H11 H 0.5923 -0.0043 0.8425 0.016(3) Uiso 1 1 calc R
C12 C 0.5557(2) -0.08578(19) 0.8057(3) 0.0179(10) Uani 1 1 d .
H12 H 0.5944 -0.1054 0.8443 0.016(3) Uiso 1 1 calc R
C13 C 0.5000 -0.1182(3) 0.7500 0.0175(14) Uani 1 2 d S
C14 C 0.5000 -0.1832(3) 0.7500 0.0144(13) Uani 1 2 d S
C15 C 0.5449(2) -0.21468(19) 0.7337(3) 0.0189(10) Uani 1 1 d .
H15 H 0.5766 -0.1950 0.7234 0.016(3) Uiso 1 1 calc R
C16 C 0.5429(2) -0.27591(19) 0.7328(3) 0.0180(10) Uani 1 1 d .
H16 H 0.5727 -0.2964 0.7197 0.016(3) Uiso 1 1 calc R
C17 C 0.48811(19) 0.21330(18) 0.8073(3) 0.0121(9) Uani 1 1 d .
H17 H 0.4797 0.1927 0.8476 0.016(3) Uiso 1 1 calc R
C18 C 0.4878(2) 0.27433(18) 0.8094(3) 0.0138(9) Uani 1 1 d .
H18 H 0.4794 0.2940 0.8505 0.016(3) Uiso 1 1 calc R
C19 C 0.5000 0.3060(2) 0.7500 0.0122(13) Uani 1 2 d S
C20 C 0.5000 0.3715(3) 0.7500 0.0117(13) Uani 1 2 d S
C21 C 0.5262(2) 0.40346(19) 0.8277(3) 0.0174(10) Uani 1 1 d .
H21 H 0.5440 0.3839 0.8811 0.016(3) Uiso 1 1 calc R
C22 C 0.5257(2) 0.46461(19) 0.8249(3) 0.0188(10) Uani 1 1 d .
H22 H 0.5441 0.4852 0.8775 0.016(3) Uiso 1 1 calc R
C23 C 0.42913(19) 0.09035(19) 0.5480(3) 0.0144(9) Uani 1 1 d .
C24 C 0.9445(2) 0.10168(18) 0.5411(3) 0.0156(10) Uani 1 1 d .
C25 C 0.6284(2) 0.2422(2) 0.0725(3) 0.0266(12) Uani 1 1 d .
C26 C 0.5955(2) 0.2347(3) 0.5249(3) 0.0288(12) Uani 1 1 d .
C27 C 0.7163(2) 0.3874(2) 0.8665(3) 0.0269(12) Uani 1 1 d .
C28 C 0.7402(3) 0.4092(3) 0.6201(4) 0.0355(13) Uani 1 1 d .
Cl1 Cl 0.68456(6) 0.24784(6) 0.18426(8) 0.0326(3) Uani 1 1 d .
Cl2 Cl 0.67015(7) 0.24228(7) 0.00898(10) 0.0437(4) Uani 1 1 d .
Cl3 Cl 0.57105(6) 0.30214(5) 0.04052(8) 0.0297(3) Uani 1 1 d .
Cl4 Cl 0.63517(10) 0.23658(12) 0.46041(12) 0.0990(9) Uani 1 1 d .
Cl5 Cl 0.65361(7) 0.23132(6) 0.63625(8) 0.0413(4) Uani 1 1 d .
Cl6 Cl 0.54012(6) 0.17455(6) 0.49586(8) 0.0327(3) Uani 1 1 d .
Cl7 Cl 0.67843(8) 0.44999(7) 0.80417(12) 0.0605(5) Uani 1 1 d .
Cl8 Cl 0.66975(6) 0.32452(7) 0.81356(10) 0.0478(4) Uani 1 1 d .
Cl9 Cl 0.72305(9) 0.39305(7) 0.97043(10) 0.0594(5) Uani 1 1 d .
Cl10 Cl 0.79990(7) 0.41563(7) 0.72949(9) 0.0456(4) Uani 1 1 d .
Cl11 Cl 0.75451(13) 0.34588(8) 0.57484(12) 0.0934(8) Uani 1 1 d .
Cl12 Cl 0.74112(9) 0.47116(7) 0.56001(11) 0.0582(5) Uani 1 1 d .
H25 H 0.601(2) 0.211(2) 0.064(3) 0.027(14) Uiso 1 1 d .
H27 H 0.765(2) 0.382(2) 0.869(3) 0.028(13) Uiso 1 1 d .
H26 H 0.577(4) 0.272(3) 0.522(5) 0.09(3) Uiso 1 1 d .
H28 H 0.699(3) 0.403(3) 0.615(4) 0.054(19) Uiso 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 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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
N2 Fe1 N1 89.71(9) . 2_656
N3 Fe1 N1 90.29(9) . 2_656
N4 Fe1 N1 89.86(13) . .
N4 Fe1 N1 90.14(13) 2_656 .
N2 Fe1 N1 89.71(9) . .
N3 Fe1 N1 90.29(9) . .
N1 Fe1 N1 179.42(19) 2_656 .
N2 Fe1 N3 180.000(1) . .
N4 Fe1 N4 179.4(2) . 2_656
N4 Fe1 N2 89.70(10) . .
N4 Fe1 N2 89.70(10) 2_656 .
N4 Fe1 N3 90.30(10) . .
N4 Fe1 N3 90.30(10) 2_656 .
N4 Fe1 N1 90.14(13) . 2_656
N4 Fe1 N1 89.86(13) 2_656 2_656
N6 Fe2 N5 91.84(9) 3 2_756
N5 Fe2 N5 176.33(17) . 2_756
N8 Fe2 N5 90.09(13) . .
N8 Fe2 N5 90.11(13) 2_756 .
N7 Fe2 N5 88.16(9) 3_545 .
N6 Fe2 N5 91.84(9) 3 .
N8 Fe2 N5 90.11(13) . 2_756
N8 Fe2 N5 90.09(13) 2_756 2_756
N7 Fe2 N5 88.16(9) 3_545 2_756
N7 Fe2 N6 180.000(1) 3_545 3
N8 Fe2 N8 173.99(19) . 2_756
N8 Fe2 N7 93.00(10) . 3_545
N8 Fe2 N7 93.00(10) 2_756 3_545
N8 Fe2 N6 87.00(10) . 3
N8 Fe2 N6 87.00(10) 2_756 3
C5 N1 C1 116.6(3) . .
C5 N1 Fe1 121.4(3) . .
C1 N1 Fe1 122.0(3) . .
C17 N3 C17 117.1(5) 2_656 .
C17 N3 Fe1 121.4(3) 2_656 .
C17 N3 Fe1 121.4(3) . .
C11 N2 C11 117.2(5) 2_656 .
C11 N2 Fe1 121.4(2) 2_656 .
C11 N2 Fe1 121.4(2) . .
C23 N4 Fe1 173.4(3) . .
C8 N5 C9 117.2(4) . .
C8 N5 Fe2 122.1(3) . .
C9 N5 Fe2 120.7(3) . .
C22 N7 C22 117.0(5) 2_656 .
C22 N7 Fe2 121.5(3) 2_656 3_455
C22 N7 Fe2 121.5(3) . 3_455
C24 N8 Fe2 164.7(3) . .
C16 N6 C16 116.6(5) . 2_656
C16 N6 Fe2 121.7(3) . 3_445
C16 N6 Fe2 121.7(3) 2_656 3_445
N1 C1 C2 123.2(4) . .
N1 C1 H1 118.4 . .
C2 C1 H1 118.4 . .
C1 C2 C3 120.0(4) . .
C1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C4 C3 C2 117.3(4) . .
C4 C3 C6 120.6(4) . .
C2 C3 C6 122.0(4) . .
C3 C4 C5 119.9(4) . .
C3 C4 H4 120.0 . .
C5 C4 H4 120.0 . .
N1 C5 C4 123.0(4) . .
N1 C5 H5 118.5 . .
C4 C5 H5 118.5 . .
C10 C6 C7 117.1(4) . .
C10 C6 C3 121.1(4) . .
C7 C6 C3 121.8(4) . .
C8 C7 C6 120.1(4) . .
C8 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
N5 C8 C7 122.8(4) . .
N5 C8 H8 118.6 . .
C7 C8 H8 118.6 . .
N5 C9 C10 122.4(4) . .
N5 C9 H9 118.8 . .
C10 C9 H9 118.8 . .
C6 C10 C9 120.3(4) . .
C6 C10 H10 119.9 . .
C9 C10 H10 119.9 . .
N2 C11 C12 122.6(4) . .
N2 C11 H11 118.7 . .
C12 C11 H11 118.7 . .
C11 C12 C13 120.6(4) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
C12 C13 C12 116.2(5) . 2_656
C12 C13 C14 121.9(3) . .
C12 C13 C14 121.9(3) 2_656 .
C15 C14 C15 117.6(6) 2_656 .
C15 C14 C13 121.2(3) 2_656 .
C15 C14 C13 121.2(3) . .
C14 C15 C16 119.8(4) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
N6 C16 C15 123.1(4) . .
N6 C16 H16 118.5 . .
C15 C16 H16 118.5 . .
N3 C17 C18 123.1(4) . .
N3 C17 H17 118.4 . .
C18 C17 H17 118.4 . .
C17 C18 C19 119.5(4) . .
C17 C18 H18 120.2 . .
C19 C18 H18 120.2 . .
C18 C19 C18 117.6(5) 2_656 .
C18 C19 C20 121.2(3) 2_656 .
C18 C19 C20 121.2(3) . .
C21 C20 C21 117.4(5) 2_656 .
C21 C20 C19 121.3(3) 2_656 .
C21 C20 C19 121.3(3) . .
C22 C21 C20 119.6(4) . .
C22 C21 H21 120.2 . .
C20 C21 H21 120.2 . .
N7 C22 C21 123.3(4) . .
N7 C22 H22 118.4 . .
C21 C22 H22 118.4 . .
N4 C23 S1 178.6(4) . .
N8 C24 S2 178.6(4) . .
Cl2 C25 Cl1 111.3(3) . .
Cl2 C25 Cl3 109.6(3) . .
Cl1 C25 Cl3 109.7(3) . .
Cl2 C25 H25 115(3) . .
Cl1 C25 H25 109(3) . .
Cl3 C25 H25 101(3) . .
Cl4 C26 Cl5 111.0(3) . .
Cl4 C26 Cl6 110.6(3) . .
Cl5 C26 Cl6 110.5(3) . .
Cl4 C26 H26 107(5) . .
Cl5 C26 H26 101(4) . .
Cl6 C26 H26 116(5) . .
Cl9 C27 Cl7 111.2(3) . .
Cl9 C27 Cl8 110.0(3) . .
Cl7 C27 Cl8 109.4(3) . .
Cl9 C27 H27 111(2) . .
Cl7 C27 H27 109(2) . .
Cl8 C27 H27 106(2) . .
Cl11 C28 Cl12 109.7(3) . .
Cl11 C28 Cl10 110.1(3) . .
Cl12 C28 Cl10 111.1(3) . .
Cl11 C28 H28 103(4) . .
Cl12 C28 H28 111(4) . .
Cl10 C28 H28 111(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.000(3) 2_656
Fe1 N1 2.000(3) .
Fe1 N2 1.988(5) .
Fe1 N3 1.998(5) .
Fe1 N4 1.952(4) .
Fe1 N4 1.952(4) 2_656
Fe2 N5 2.258(3) .
Fe2 N5 2.258(3) 2_756
Fe2 N6 2.243(5) 3
Fe2 N7 2.218(5) 3_545
Fe2 N8 2.094(4) .
Fe2 N8 2.094(4) 2_756
S1 C23 1.645(5) .
S2 C24 1.634(5) .
N1 C5 1.345(5) .
N1 C1 1.353(5) .
N3 C17 1.338(5) 2_656
N3 C17 1.338(5) .
N2 C11 1.346(5) 2_656
N2 C11 1.346(5) .
N4 C23 1.145(5) .
N5 C8 1.337(5) .
N5 C9 1.343(5) .
N7 C22 1.345(5) 2_656
N7 C22 1.345(5) .
N7 Fe2 2.218(5) 3_455
N8 C24 1.162(5) .
N6 C16 1.342(5) .
N6 C16 1.342(5) 2_656
N6 Fe2 2.243(5) 3_445
C1 C2 1.367(6) .
C1 H1 0.9300 .
C2 C3 1.392(6) .
C2 H2 0.9300 .
C3 C4 1.372(6) .
C3 C6 1.493(5) .
C4 C5 1.387(6) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C10 1.374(6) .
C6 C7 1.378(6) .
C7 C8 1.374(6) .
C7 H7 0.9300 .
C8 H8 0.9300 .
C9 C10 1.376(6) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.380(6) .
C11 H11 0.9300 .
C12 C13 1.389(5) .
C12 H12 0.9300 .
C13 C12 1.389(5) 2_656
C13 C14 1.469(8) .
C14 C15 1.376(5) 2_656
C14 C15 1.376(5) .
C15 C16 1.385(6) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C17 C18 1.381(6) .
C17 H17 0.9300 .
C18 C19 1.383(5) .
C18 H18 0.9300 .
C19 C18 1.383(5) 2_656
C19 C20 1.480(8) .
C20 C21 1.392(5) 2_656
C20 C21 1.392(5) .
C21 C22 1.384(6) .
C21 H21 0.9300 .
C22 H22 0.9300 .
C25 Cl2 1.752(5) .
C25 Cl1 1.755(5) .
C25 Cl3 1.779(5) .
C25 H25 0.91(5) .
C26 Cl4 1.728(5) .
C26 Cl5 1.757(5) .
C26 Cl6 1.760(5) .
C26 H26 0.94(7) .
C27 Cl9 1.735(5) .
C27 Cl7 1.743(5) .
C27 Cl8 1.754(5) .
C27 H27 1.09(5) .
C28 Cl11 1.734(6) .
C28 Cl12 1.749(6) .
C28 Cl10 1.746(6) .
C28 H28 0.90(6) .
