#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:14:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179368 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/65/4326593.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_4326593
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 Se4'
_chemical_formula_weight         2111.30
_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                 116.933(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.6930(19)
_cell_length_b                   22.608(2)
_cell_length_c                   17.2911(16)
_cell_measurement_temperature    100(2)
_cell_volume                     7908.9(12)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    0.0586
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6852
_diffrn_reflns_theta_full        24.62
_diffrn_reflns_theta_max         24.62
_diffrn_reflns_theta_min         1.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.062
_exptl_absorpt_correction_T_max  0.8619
_exptl_absorpt_correction_T_min  0.7493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Twinabs
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0444
_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)+(0.0594P)²+16.6439P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1103
_reflns_number_gt                5613
_reflns_number_total             6853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200932w_si_002_2.cif
_cod_data_source_block           NCSe@100K
_cod_database_code               4326593
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 0.09312(6) 0.7500 0.0095(3) Uani 1 2 d S
Fe2 Fe 1.0000 0.09258(6) 0.7500 0.0095(3) Uani 1 2 d S
Se1 Se 0.40333(4) 0.08663(3) 0.43374(4) 0.02303(18) Uani 1 1 d .
Se2 Se 0.92540(4) 0.09666(3) 0.42847(4) 0.02264(18) Uani 1 1 d .
N1 N 0.5869(2) 0.0931(2) 0.7462(3) 0.0102(11) Uani 1 1 d .
N3 N 0.5000 0.1808(3) 0.7500 0.0081(15) Uani 1 2 d S
N2 N 0.5000 0.0053(3) 0.7500 0.0118(16) Uani 1 2 d S
N4 N 0.4551(2) 0.0931(2) 0.6243(3) 0.0114(11) Uani 1 1 d .
N5 N 0.8994(3) 0.0895(2) 0.7452(3) 0.0150(12) Uani 1 1 d .
N7 N 0.5000 0.4949(3) 0.7500 0.0121(16) Uani 1 2 d S
N8 N 0.9566(2) 0.0963(2) 0.6138(3) 0.0119(11) Uani 1 1 d .
N6 N 0.5000 -0.3087(3) 0.7500 0.0105(16) Uani 1 2 d S
C1 C 0.5963(3) 0.0629(3) 0.6856(4) 0.0152(15) Uani 1 1 d .
H1 H 0.5601 0.0411 0.6438 0.018 Uiso 1 1 calc R
C2 C 0.6553(3) 0.0615(3) 0.6803(4) 0.0168(15) Uani 1 1 d .
H2 H 0.6587 0.0407 0.6347 0.020 Uiso 1 1 calc R
C3 C 0.7099(3) 0.0914(3) 0.7439(4) 0.0146(14) Uani 1 1 d .
C4 C 0.7008(3) 0.1225(3) 0.8063(4) 0.0156(14) Uani 1 1 d .
H4 H 0.7365 0.1440 0.8496 0.019 Uiso 1 1 calc R
C5 C 0.6394(3) 0.1222(3) 0.8055(4) 0.0157(15) Uani 1 1 d .
H5 H 0.6342 0.1438 0.8492 0.019 Uiso 1 1 calc R
C6 C 0.7752(3) 0.0903(3) 0.7431(4) 0.0149(14) Uani 1 1 d .
C7 C 0.7823(3) 0.1072(3) 0.6706(4) 0.0180(16) Uani 1 1 d .
H7 H 0.7448 0.1187 0.6189 0.022 Uiso 1 1 calc R
C8 C 0.8447(3) 0.1071(3) 0.6744(4) 0.0145(14) Uani 1 1 d .
H8 H 0.8491 0.1199 0.6250 0.017 Uiso 1 1 calc R
C9 C 0.8916(3) 0.0713(3) 0.8135(4) 0.0188(15) Uani 1 1 d .
H9 H 0.9293 0.0573 0.8631 0.023 Uiso 1 1 calc R
C10 C 0.8314(3) 0.0719(3) 0.8152(4) 0.0160(15) Uani 1 1 d .
H10 H 0.8286 0.0597 0.8659 0.019 Uiso 1 1 calc R
C11 C 0.5536(3) -0.0262(3) 0.8063(4) 0.0163(14) Uani 1 1 d .
H11 H 0.5914 -0.0054 0.8468 0.020 Uiso 1 1 calc R
C12 C 0.5547(3) -0.0873(3) 0.8064(4) 0.0194(15) Uani 1 1 d .
H12 H 0.5934 -0.1077 0.8455 0.023 Uiso 1 1 calc R
C13 C 0.5000 -0.1189(4) 0.7500 0.0116(19) Uani 1 2 d S
C14 C 0.5000 -0.1841(4) 0.7500 0.016(2) Uani 1 2 d S
C15 C 0.5443(3) -0.2162(3) 0.7306(4) 0.0148(14) Uani 1 1 d .
H15 H 0.5759 -0.1963 0.7181 0.018 Uiso 1 1 calc R
C16 C 0.5414(3) -0.2771(3) 0.7298(4) 0.0164(15) Uani 1 1 d .
H16 H 0.5705 -0.2981 0.7140 0.020 Uiso 1 1 calc R
C17 C 0.4867(3) 0.2127(3) 0.8065(4) 0.0132(14) Uani 1 1 d .
H17 H 0.4768 0.1916 0.8467 0.016 Uiso 1 1 calc R
C18 C 0.4866(3) 0.2732(3) 0.8100(4) 0.0144(14) Uani 1 1 d .
H18 H 0.4776 0.2932 0.8519 0.017 Uiso 1 1 calc R
C19 C 0.5000 0.3048(4) 0.7500 0.015(2) Uani 1 2 d S
C20 C 0.5000 0.3706(4) 0.7500 0.0099(18) Uani 1 2 d S
C21 C 0.5304(3) 0.4028(3) 0.8270(4) 0.0170(14) Uani 1 1 d .
H21 H 0.5514 0.3830 0.8813 0.020 Uiso 1 1 calc R
C22 C 0.5295(3) 0.4635(3) 0.8232(4) 0.0189(15) Uani 1 1 d .
H22 H 0.5513 0.4846 0.8763 0.023 Uiso 1 1 calc R
C23 C 0.4343(3) 0.0901(3) 0.5507(4) 0.0150(14) Uani 1 1 d .
C24 C 0.9441(3) 0.0969(3) 0.5408(4) 0.0152(15) Uani 1 1 d .
C25 C 0.6247(3) 0.2459(3) 0.0678(4) 0.0218(16) Uani 1 1 d .
H25A H 0.5981 0.2090 0.0580 0.026 Uiso 1 1 calc R
C26 C 0.5970(3) 0.2430(3) 0.5314(4) 0.0219(16) Uani 1 1 d .
H26A H 0.5704 0.2779 0.5326 0.026 Uiso 1 1 calc R
C27 C 0.7191(4) 0.3866(3) 0.8698(5) 0.0258(17) Uani 1 1 d .
H27A H 0.7644 0.3817 0.8745 0.031 Uiso 1 1 calc R
C28 C 0.7463(4) 0.4036(4) 0.6090(5) 0.0327(19) Uani 1 1 d .
H28A H 0.7000 0.3948 0.5980 0.039 Uiso 1 1 calc R
Cl1 Cl 0.68197(8) 0.25057(9) 0.17975(12) 0.0281(4) Uani 1 1 d .
Cl2 Cl 0.66755(10) 0.24260(10) 0.00486(13) 0.0368(5) Uani 1 1 d .
Cl3 Cl 0.57085(9) 0.30697(8) 0.03745(12) 0.0256(4) Uani 1 1 d .
Cl4 Cl 0.62661(10) 0.25717(9) 0.45481(12) 0.0326(5) Uani 1 1 d .
Cl5 Cl 0.66269(10) 0.23385(9) 0.63575(12) 0.0373(5) Uani 1 1 d .
Cl6 Cl 0.54512(9) 0.18081(8) 0.50012(12) 0.0290(4) Uani 1 1 d .
Cl7 Cl 0.68403(12) 0.45072(10) 0.80975(15) 0.0446(6) Uani 1 1 d .
Cl8 Cl 0.67148(9) 0.32457(9) 0.81552(13) 0.0342(5) Uani 1 1 d .
Cl9 Cl 0.72607(12) 0.39178(10) 0.97426(13) 0.0467(6) Uani 1 1 d .
Cl10 Cl 0.79548(10) 0.41076(12) 0.72132(13) 0.0462(6) Uani 1 1 d .
Cl11 Cl 0.77484(10) 0.34434(9) 0.56872(14) 0.0406(5) Uani 1 1 d .
Cl12 Cl 0.74585(13) 0.46887(11) 0.55502(16) 0.0533(6) 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 0.0033 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'
Se Se -0.0929 2.2259 '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
N4 Fe1 N4 180.0(5) 2_656 .
N4 Fe1 N3 89.99(16) 2_656 .
N4 Fe1 N3 89.99(16) . .
N4 Fe1 N2 90.01(16) 2_656 .
N4 Fe1 N2 90.01(16) . .
N3 Fe1 N2 180.000(1) . .
N4 Fe1 N1 89.4(2) 2_656 2_656
N4 Fe1 N1 90.6(2) . 2_656
N3 Fe1 N1 90.04(15) . 2_656
N2 Fe1 N1 89.96(16) . 2_656
N4 Fe1 N1 90.6(2) 2_656 .
N4 Fe1 N1 89.4(2) . .
N3 Fe1 N1 90.04(16) . .
N2 Fe1 N1 89.96(15) . .
N1 Fe1 N1 179.9(3) 2_656 .
N8 Fe2 N8 175.4(3) . 2_756
N8 Fe2 N7 92.29(15) . 3_545
N8 Fe2 N7 92.29(15) 2_756 3_545
N8 Fe2 N6 87.70(15) . 3
N8 Fe2 N6 87.71(15) 2_756 3
N7 Fe2 N6 179.997(1) 3_545 3
N8 Fe2 N5 89.7(2) . 2_756
N8 Fe2 N5 90.5(2) 2_756 2_756
N7 Fe2 N5 88.22(15) 3_545 2_756
N6 Fe2 N5 91.77(15) 3 2_756
N8 Fe2 N5 90.5(2) . .
N8 Fe2 N5 89.7(2) 2_756 .
N7 Fe2 N5 88.22(15) 3_545 .
N6 Fe2 N5 91.78(15) 3 .
N5 Fe2 N5 176.4(3) 2_756 .
C5 N1 C1 116.5(5) . .
C5 N1 Fe1 121.4(4) . .
C1 N1 Fe1 122.1(4) . .
C17 N3 C17 115.7(8) . 2_656
C17 N3 Fe1 122.2(4) . .
C17 N3 Fe1 122.2(4) 2_656 .
C11 N2 C11 117.2(8) . 2_656
C11 N2 Fe1 121.4(4) . .
C11 N2 Fe1 121.4(4) 2_656 .
C23 N4 Fe1 172.8(5) . .
C9 N5 C8 117.2(5) . .
C9 N5 Fe2 121.1(4) . .
C8 N5 Fe2 121.8(4) . .
C22 N7 C22 115.8(8) . 2_656
C22 N7 Fe2 122.1(4) . 3_455
C22 N7 Fe2 122.1(4) 2_656 3_455
C24 N8 Fe2 167.9(5) . .
C16 N6 C16 115.9(8) 2_656 .
C16 N6 Fe2 122.0(4) 2_656 3_445
C16 N6 Fe2 122.0(4) . 3_445
N1 C1 C2 124.3(6) . .
C1 C2 C3 118.3(6) . .
C4 C3 C2 117.9(6) . .
C4 C3 C6 121.2(6) . .
C2 C3 C6 120.9(6) . .
C3 C4 C5 119.6(6) . .
N1 C5 C4 123.3(6) . .
C10 C6 C7 117.3(6) . .
C10 C6 C3 120.8(6) . .
C7 C6 C3 121.9(6) . .
C8 C7 C6 119.4(6) . .
N5 C8 C7 122.9(6) . .
N5 C9 C10 123.0(6) . .
C9 C10 C6 120.1(6) . .
N2 C11 C12 122.2(6) . .
C13 C12 C11 120.4(6) . .
C12 C13 C12 117.7(8) . 2_656
C12 C13 C14 121.2(4) . .
C12 C13 C14 121.2(4) 2_656 .
C15 C14 C15 117.4(8) . 2_656
C15 C14 C13 121.3(4) . .
C15 C14 C13 121.3(4) 2_656 .
C16 C15 C14 119.0(6) . .
N6 C16 C15 124.2(6) . .
N3 C17 C18 124.7(6) . .
C17 C18 C19 118.1(6) . .
C18 C19 C18 118.8(8) . 2_656
C18 C19 C20 120.6(4) . .
C18 C19 C20 120.6(4) 2_656 .
C21 C20 C21 117.2(8) . 2_656
C21 C20 C19 121.4(4) . .
C21 C20 C19 121.4(4) 2_656 .
C22 C21 C20 119.0(6) . .
N7 C22 C21 124.5(7) . .
N4 C23 Se1 178.3(6) . .
N8 C24 Se2 179.0(6) . .
Cl3 C25 Cl2 110.7(4) . .
Cl3 C25 Cl1 110.2(4) . .
Cl2 C25 Cl1 109.8(4) . .
Cl6 C26 Cl5 111.1(4) . .
Cl6 C26 Cl4 110.2(4) . .
Cl5 C26 Cl4 111.0(4) . .
Cl9 C27 Cl7 111.3(4) . .
Cl9 C27 Cl8 110.6(4) . .
Cl7 C27 Cl8 109.9(4) . .
Cl12 C28 Cl10 111.2(5) . .
Cl12 C28 Cl11 110.2(4) . .
Cl10 C28 Cl11 110.2(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N4 1.938(5) 2_656
Fe1 N4 1.938(5) .
Fe1 N3 1.982(7) .
Fe1 N2 1.986(7) .
Fe1 N1 2.003(4) 2_656
Fe1 N1 2.003(4) .
Fe2 N8 2.104(5) .
Fe2 N8 2.104(5) 2_756
Fe2 N7 2.208(7) 3_545
Fe2 N6 2.233(7) 3
Fe2 N5 2.247(5) 2_756
Fe2 N5 2.247(5) .
Se1 C23 1.817(6) .
Se2 C24 1.791(7) .
N1 C5 1.341(8) .
N1 C1 1.346(8) .
N3 C17 1.353(7) .
N3 C17 1.353(7) 2_656
N2 C11 1.363(7) .
N2 C11 1.363(7) 2_656
N4 C23 1.142(8) .
N5 C9 1.335(8) .
N5 C8 1.350(8) .
N7 C22 1.337(8) .
N7 C22 1.337(8) 2_656
N7 Fe2 2.208(7) 3_455
N8 C24 1.160(8) .
N6 C16 1.346(7) 2_656
N6 C16 1.346(8) .
N6 Fe2 2.233(7) 3_445
C1 C2 1.382(9) .
C2 C3 1.403(10) .
C3 C4 1.379(9) .
C3 C6 1.490(8) .
C4 C5 1.389(9) .
C6 C10 1.383(9) .
C6 C7 1.387(9) .
C7 C8 1.386(9) .
C9 C10 1.380(9) .
C11 C12 1.383(9) .
C12 C13 1.381(8) .
C13 C12 1.381(8) 2_656
C13 C14 1.472(13) .
C14 C15 1.398(8) .
C14 C15 1.398(8) 2_656
C15 C16 1.379(9) .
C17 C18 1.370(9) .
C18 C19 1.402(8) .
C19 C18 1.402(8) 2_656
C19 C20 1.488(12) .
C20 C21 1.394(8) .
C20 C21 1.394(8) 2_656
C21 C22 1.374(10) .
C25 Cl3 1.758(7) .
C25 Cl2 1.760(7) .
C25 Cl1 1.780(7) .
C26 Cl6 1.755(7) .
C26 Cl5 1.756(7) .
C26 Cl4 1.764(7) .
C27 Cl9 1.745(8) .
C27 Cl7 1.749(7) .
C27 Cl8 1.760(8) .
C28 Cl12 1.743(8) .
C28 Cl10 1.754(8) .
C28 Cl11 1.763(8) .
