#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:14:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179368 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/65/4326592.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_4326592
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            'C26 H20 Cl12 Fe N6 Se2'
_chemical_formula_weight         1055.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 117.939(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.499(5)
_cell_length_b                   11.505(4)
_cell_length_c                   17.854(5)
_cell_measurement_temperature    200(2)
_cell_volume                     2086.7(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2164
_diffrn_reflns_theta_full        20.73
_diffrn_reflns_theta_max         20.73
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.902
_exptl_absorpt_correction_T_max  0.8685
_exptl_absorpt_correction_T_min  0.7601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   twinabs
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.231
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0530
_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)+(0.0950P)²+4.3759P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                1908
_reflns_number_total             2164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200932w_si_002_1.cif
_cod_data_source_block           NCSe@200K
_cod_original_cell_volume        2086.7(13)
_cod_database_code               4326592
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, 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
Se1 Se 0.67610(13) -0.31607(12) 0.06643(7) 0.0595(4) Uani 1 1 d .
Fe1 Fe 0.5000 -0.31338(16) -0.2500 0.0194(4) Uani 1 2 d S
N1 N 0.3080(6) -0.3137(6) -0.2480(5) 0.0240(15) Uani 1 1 d .
N2 N 0.5000 -0.1237(8) -0.2500 0.023(2) Uani 1 2 d S
N3 N 0.5000 -0.5089(8) -0.2500 0.020(2) Uani 1 2 d S
N4 N 0.5976(7) -0.3072(6) -0.1148(5) 0.0237(16) Uani 1 1 d .
C1 C 0.2028(9) -0.2704(9) -0.3126(6) 0.036(3) Uani 1 1 d .
H1A H 0.2121 -0.2375 -0.3583 0.044 Uiso 1 1 calc R
C2 C 0.0775(9) -0.2704(9) -0.3171(6) 0.039(3) Uani 1 1 d .
H2A H 0.0029 -0.2419 -0.3659 0.047 Uiso 1 1 calc R
C3 C 0.0660(9) -0.3122(9) -0.2498(6) 0.031(2) Uani 1 1 d .
C4 C 0.1750(10) -0.3568(9) -0.1813(7) 0.044(3) Uani 1 1 d .
H4A H 0.1698 -0.3870 -0.1334 0.053 Uiso 1 1 calc R
C5 C 0.2937(9) -0.3559(8) -0.1851(6) 0.034(2) Uani 1 1 d .
H5A H 0.3690 -0.3883 -0.1387 0.040 Uiso 1 1 calc R
C11 C 0.4597(9) -0.0616(8) -0.2040(6) 0.032(2) Uani 1 1 d .
H11A H 0.4294 -0.1024 -0.1702 0.039 Uiso 1 1 calc R
C12 C 0.4587(9) 0.0582(8) -0.2018(6) 0.031(2) Uani 1 1 d .
H12A H 0.4292 0.0971 -0.1669 0.038 Uiso 1 1 calc R
C13 C 0.5000 0.1208(11) -0.2500 0.026(3) Uani 1 2 d S
C17 C 0.5400(11) -0.5672(8) -0.1790(7) 0.044(3) Uani 1 1 d .
H17A H 0.5717 -0.5251 -0.1274 0.053 Uiso 1 1 calc R
C18 C 0.5382(10) -0.6878(8) -0.1762(6) 0.041(3) Uani 1 1 d .
H18A H 0.5629 -0.7269 -0.1240 0.049 Uiso 1 1 calc R
C19 C 0.5000 0.2499(11) -0.2500 0.024(3) Uani 1 2 d S
C23 C 0.6295(8) -0.3082(8) -0.0436(7) 0.027(2) Uani 1 1 d .
Cl1 Cl -0.0335(15) -0.6895(15) -0.0349(5) 0.221(6) Uani 0.68 1 d P
Cl2 Cl -0.1143(15) -0.5934(9) -0.1961(9) 0.195(8) Uani 0.68 1 d P
Cl3 Cl -0.1381(8) -0.8269(8) -0.1769(7) 0.162(4) Uani 0.68 1 d P
C25 C -0.0407(15) -0.6972(14) -0.1248(10) 0.093(5) Uani 1 1 d .
H25 H 0.0493 -0.7082 -0.1192 0.112 Uiso 1 1 d R
Cl1' Cl -0.135(3) -0.675(4) -0.2187(10) 0.27(2) Uani 0.32 1 d P
Cl2' Cl -0.088(2) -0.7843(13) -0.0737(12) 0.131(6) Uani 0.32 1 d P
Cl3' Cl -0.026(4) -0.5467(16) -0.070(2) 0.251(16) Uani 0.32 1 d P
Cl4 Cl 0.3766(4) -0.1175(3) -0.0236(2) 0.0740(10) Uani 1 1 d .
Cl5 Cl 0.1884(5) 0.0010(5) 0.0123(3) 0.1311(18) Uani 1 1 d .
Cl6 Cl 0.1559(4) -0.0094(4) -0.1593(2) 0.0997(13) Uani 1 1 d .
C26 C 0.2649(13) -0.0008(12) -0.0515(8) 0.066(3) Uani 1 1 d .
H26 H 0.3160 0.0730 -0.0413 0.080 Uiso 1 1 calc R
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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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
N4 Fe1 N4 176.2(4) . 2_654
N4 Fe1 N2 88.1(2) . .
N4 Fe1 N2 88.1(2) 2_654 .
N4 Fe1 N1 89.0(3) . .
N4 Fe1 N1 91.0(3) 2_654 .
N2 Fe1 N1 90.09(19) . .
N4 Fe1 N1 91.0(3) . 2_654
N4 Fe1 N1 89.0(3) 2_654 2_654
N2 Fe1 N1 90.09(19) . 2_654
N1 Fe1 N1 179.8(4) . 2_654
N4 Fe1 N3 91.9(2) . .
N4 Fe1 N3 91.9(2) 2_654 .
N2 Fe1 N3 180.000(2) . .
N1 Fe1 N3 89.91(19) . .
N1 Fe1 N3 89.91(19) 2_654 .
C5 N1 C1 117.4(7) . .
C5 N1 Fe1 122.8(6) . .
C1 N1 Fe1 119.8(6) . .
C11 N2 C11 114.7(11) 2_654 .
C11 N2 Fe1 122.6(5) 2_654 .
C11 N2 Fe1 122.6(5) . .
C17 N3 C17 118.5(11) . 2_654
C17 N3 Fe1 120.7(6) . .
C17 N3 Fe1 120.7(6) 2_654 .
C23 N4 Fe1 168.4(7) . .
N1 C1 C2 123.1(9) . .
N1 C1 H1A 118.4 . .
C2 C1 H1A 118.4 . .
C3 C2 C1 118.2(9) . .
C3 C2 H2A 120.9 . .
C1 C2 H2A 120.9 . .
C2 C3 C4 119.6(8) . .
C2 C3 C3 120.6(10) . 2_554
C4 C3 C3 119.9(10) . 2_554
C3 C4 C5 117.2(9) . .
C3 C4 H4A 121.4 . .
C5 C4 H4A 121.4 . .
N1 C5 C4 124.4(9) . .
N1 C5 H5A 117.8 . .
C4 C5 H5A 117.8 . .
N2 C11 C12 124.5(9) . .
N2 C11 H11A 117.8 . .
C12 C11 H11A 117.8 . .
C13 C12 C11 120.0(9) . .
C13 C12 H12A 120.0 . .
C11 C12 H12A 120.0 . .
C12 C13 C12 116.3(12) . 2_654
C12 C13 C19 121.8(6) . .
C12 C13 C19 121.8(6) 2_654 .
N3 C17 C18 122.8(9) . .
N3 C17 H17A 118.6 . .
C18 C17 H17A 118.6 . .
C19 C18 C17 119.2(9) 1_545 .
C19 C18 H18A 120.4 1_545 .
C17 C18 H18A 120.4 . .
C18 C19 C18 117.4(12) 1_565 2_664
C18 C19 C13 121.3(6) 1_565 .
C18 C19 C13 121.3(6) 2_664 .
N4 C23 Se1 177.5(9) . .
Cl2' Cl1 C25 68.0(10) . .
Cl2' Cl1 Cl3' 133.2(15) . .
C25 Cl1 Cl3' 71.1(12) . .
Cl1' Cl2 C25 64.9(15) . .
Cl1' Cl2 Cl3' 125.9(17) . .
C25 Cl2 Cl3' 62.4(10) . .
Cl2' Cl3 C25 53.8(8) . .
Cl2' Cl3 Cl1' 95.7(10) . .
C25 Cl3 Cl1' 48.2(8) . .
Cl1' C25 Cl1 141.3(19) . .
Cl1' C25 Cl2' 118.0(17) . .
Cl1 C25 Cl2' 47.7(8) . .
Cl1' C25 Cl2 36.3(18) . .
Cl1 C25 Cl2 120.5(14) . .
Cl2' C25 Cl2 133.9(14) . .
Cl1' C25 Cl3 68.5(18) . .
Cl1 C25 Cl3 106.9(11) . .
Cl2' C25 Cl3 59.6(10) . .
Cl2 C25 Cl3 103.0(10) . .
Cl1' C25 Cl3' 104(2) . .
Cl1 C25 Cl3' 59.3(12) . .
Cl2' C25 Cl3' 103.9(15) . .
Cl2 C25 Cl3' 68.8(12) . .
Cl3 C25 Cl3' 149.5(16) . .
Cl1' C25 H25 107.4 . .
Cl1 C25 H25 110.4 . .
Cl2' C25 H25 118.4 . .
Cl2 C25 H25 107.5 . .
Cl3 C25 H25 107.8 . .
Cl3' C25 H25 102.7 . .
Cl2 Cl1' C25 78.8(17) . .
Cl2 Cl1' Cl3 138.0(19) . .
C25 Cl1' Cl3 63.3(14) . .
Cl1 Cl2' C25 64.4(10) . .
Cl1 Cl2' Cl3 130.4(13) . .
C25 Cl2' Cl3 66.6(10) . .
Cl1 Cl3' C25 49.5(7) . .
Cl1 Cl3' Cl2 93.8(11) . .
C25 Cl3' Cl2 48.8(8) . .
Cl5 C26 Cl6 113.8(7) . .
Cl5 C26 Cl4 110.5(7) . .
Cl6 C26 Cl4 108.7(7) . .
Cl5 C26 H26 107.9 . .
Cl6 C26 H26 107.9 . .
Cl4 C26 H26 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 C23 1.779(11) .
Fe1 N4 2.133(8) .
Fe1 N4 2.133(8) 2_654
Fe1 N2 2.182(10) .
Fe1 N1 2.225(6) .
Fe1 N1 2.225(6) 2_654
Fe1 N3 2.250(10) .
N1 C5 1.302(11) .
N1 C1 1.317(12) .
N2 C11 1.326(11) 2_654
N2 C11 1.326(11) .
N3 C17 1.311(11) .
N3 C17 1.311(11) 2_654
N4 C23 1.147(10) .
C1 C2 1.405(13) .
C1 H1A 0.9500 .
C2 C3 1.357(13) .
C2 H2A 0.9500 .
C3 C4 1.376(14) .
C3 C3 1.515(17) 2_554
C4 C5 1.398(13) .
C4 H4A 0.9500 .
C5 H5A 0.9500 .
C11 C12 1.378(12) .
C11 H11A 0.9500 .
C12 C13 1.367(11) .
C12 H12A 0.9500 .
C13 C12 1.367(11) 2_654
C13 C19 1.486(16) .
C17 C18 1.389(13) .
C17 H17A 0.9500 .
C18 C19 1.378(12) 1_545
C18 H18A 0.9500 .
C19 C18 1.378(12) 1_565
C19 C18 1.378(12) 2_664
Cl1 Cl2' 1.288(19) .
Cl1 C25 1.571(17) .
Cl1 Cl3' 1.78(3) .
Cl2 Cl1' 1.00(5) .
Cl2 C25 1.659(16) .
Cl2 Cl3' 2.05(3) .
Cl3 Cl2' 1.73(2) .
Cl3 C25 1.836(18) .
Cl3 Cl1' 1.91(4) .
C25 Cl1' 1.53(2) .
C25 Cl2' 1.62(2) .
C25 Cl3' 1.95(3) .
C25 H25 1.0000 .
Cl4 C26 1.762(14) .
Cl5 C26 1.734(14) .
Cl6 C26 1.740(12) .
C26 H26 1.0000 .
