#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:26:03 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179721 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/23/7002335.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_7002335
loop_
_publ_author_name
'Wriedt, Mario'
'Sellmer, Sina'
'Näther, Christian'
_publ_section_title
;
 Coordination polymer changing its magnetic properties and colour by
 thermal decomposition: synthesis, structure and properties of new
 thiocyanato iron(ii) coordination polymers based on
 4,4'-bipyridine as ligand
;
_journal_issue                   38
_journal_name_full               'Dalton Transactions'
_journal_page_first              7975
_journal_page_last               7984
_journal_paper_doi               10.1039/b907645j
_journal_year                    2009
_chemical_formula_moiety         'C12 H8 Fe N4 S2'
_chemical_formula_sum            'C12 H8 Fe N4 S2'
_chemical_formula_weight         328.19
_chemical_name_systematic
;
poly[bis(μ2-thiocyanato-N,S)-(μ2-4,4'-bipyridine-N,N')-iron(II)]
;
_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                 112.087(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1738(10)
_cell_length_b                   11.5606(12)
_cell_length_c                   11.4572(10)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      5.7
_cell_volume                     1371.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Phi 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6331
_diffrn_reflns_theta_full        27.81
_diffrn_reflns_theta_max         27.81
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.393
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0063(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0325
_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)+(0.0524P)²+0.9860P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                1309
_reflns_number_total             1623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b907645j.txt
_cod_data_source_block           for_compound_3
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7002335
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.01523(3) 0.7500 0.02023(16) Uani 1 2 d S . .
N1 N 0.5000 0.20682(19) 0.7500 0.0236(5) Uani 1 2 d S . .
N2 N 0.5000 0.8224(2) 0.7500 0.0303(6) Uani 1 2 d S . .
C1 C 0.5790(2) 0.26766(18) 0.7094(2) 0.0315(5) Uani 1 1 d . . .
H1 H 0.6351 0.2275 0.6813 0.038 Uiso 1 1 calc R . .
C2 C 0.5811(2) 0.38761(17) 0.7073(2) 0.0310(5) Uani 1 1 d . . .
H2 H 0.6368 0.4259 0.6773 0.037 Uiso 1 1 calc R . .
C3 C 0.5000 0.4503(2) 0.7500 0.0219(5) Uani 1 2 d S . .
C4 C 0.5000 0.5787(2) 0.7500 0.0252(6) Uani 1 2 d S . .
C5 C 0.4757(3) 0.64152(18) 0.8419(2) 0.0377(6) Uani 1 1 d . . .
H5 H 0.4583 0.6034 0.9053 0.045 Uiso 1 1 calc R . .
C6 C 0.4774(3) 0.76106(19) 0.8387(2) 0.0410(6) Uani 1 1 d . . .
H6 H 0.4619 0.8012 0.9019 0.049 Uiso 1 1 calc R . .
N11 N 0.38291(18) -0.01469(14) 0.35795(18) 0.0250(4) Uani 1 1 d . . .
C11 C 0.34357(19) -0.00203(15) 0.4369(2) 0.0217(4) Uani 1 1 d . . .
S11 S 0.28875(6) 0.01838(7) 0.54959(6) 0.0400(2) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0312(2) 0.0171(2) 0.0191(2) 0.000 0.01725(17) 0.000
N1 0.0300(12) 0.0175(11) 0.0287(13) 0.000 0.0173(10) 0.000
N2 0.0481(15) 0.0203(11) 0.0291(14) 0.000 0.0222(12) 0.000
C1 0.0395(12) 0.0210(10) 0.0474(15) -0.0057(9) 0.0315(11) -0.0023(8)
C2 0.0404(12) 0.0200(10) 0.0451(14) -0.0035(8) 0.0302(11) -0.0069(8)
C3 0.0272(14) 0.0160(11) 0.0237(14) 0.000 0.0108(11) 0.000
C4 0.0320(15) 0.0191(13) 0.0281(15) 0.000 0.0153(12) 0.000
C5 0.0691(16) 0.0201(10) 0.0372(13) 0.0046(9) 0.0353(12) 0.0051(10)
C6 0.0771(18) 0.0221(10) 0.0400(14) 0.0017(9) 0.0405(14) 0.0071(10)
N11 0.0313(9) 0.0275(8) 0.0213(8) -0.0003(7) 0.0158(7) 0.0014(6)
C11 0.0244(9) 0.0220(9) 0.0206(9) 0.0006(7) 0.0106(7) -0.0010(7)
S11 0.0286(3) 0.0763(5) 0.0221(3) -0.0059(3) 0.0175(2) -0.0022(3)
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'
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
_geom_angle_publ_flag
N11 Fe1 N11 179.66(9) 6_556 5_656 ?
N11 Fe1 N1 90.17(5) 6_556 . ?
N11 Fe1 N1 90.17(5) 5_656 . ?
N11 Fe1 N2 89.83(5) 6_556 1_545 ?
N11 Fe1 N2 89.83(5) 5_656 1_545 ?
N1 Fe1 N2 180.0 . 1_545 ?
N11 Fe1 S11 92.26(5) 6_556 2_656 ?
N11 Fe1 S11 87.74(5) 5_656 2_656 ?
N1 Fe1 S11 89.198(18) . 2_656 ?
N2 Fe1 S11 90.802(18) 1_545 2_656 ?
N11 Fe1 S11 87.74(5) 6_556 . ?
N11 Fe1 S11 92.26(5) 5_656 . ?
N1 Fe1 S11 89.198(18) . . ?
N2 Fe1 S11 90.802(18) 1_545 . ?
S11 Fe1 S11 178.40(4) 2_656 . ?
C1 N1 C1 116.7(2) 2_656 . ?
C1 N1 Fe1 121.63(12) 2_656 . ?
C1 N1 Fe1 121.63(12) . . ?
C6 N2 C6 116.0(3) . 2_656 ?
C6 N2 Fe1 121.99(13) . 1_565 ?
C6 N2 Fe1 121.99(13) 2_656 1_565 ?
N1 C1 C2 123.20(19) . . ?
C3 C2 C1 119.98(19) . . ?
C2 C3 C2 116.9(2) 2_656 . ?
C2 C3 C4 121.55(12) 2_656 . ?
C2 C3 C4 121.55(12) . . ?
C5 C4 C5 116.9(3) . 2_656 ?
C5 C4 C3 121.55(13) . . ?
C5 C4 C3 121.55(13) 2_656 . ?
C6 C5 C4 119.6(2) . . ?
N2 C6 C5 123.9(2) . . ?
C11 N11 Fe1 164.16(17) . 5_656 ?
N11 C11 S11 178.95(18) . . ?
C11 S11 Fe1 102.08(8) . . ?
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 N11 2.1114(18) 6_556 ?
Fe1 N11 2.1114(18) 5_656 ?
Fe1 N1 2.215(2) . ?
Fe1 N2 2.229(2) 1_545 ?
Fe1 S11 2.6018(7) 2_656 ?
Fe1 S11 2.6018(7) . ?
N1 C1 1.341(2) 2_656 ?
N1 C1 1.341(2) . ?
N2 C6 1.339(3) . ?
N2 C6 1.339(3) 2_656 ?
N2 Fe1 2.229(2) 1_565 ?
C1 C2 1.387(3) . ?
C2 C3 1.385(2) . ?
C3 C2 1.385(2) 2_656 ?
C3 C4 1.485(4) . ?
C4 C5 1.387(3) . ?
C4 C5 1.387(3) 2_656 ?
C5 C6 1.383(3) . ?
N11 C11 1.154(3) . ?
N11 Fe1 2.1114(18) 5_656 ?
C11 S11 1.641(2) . ?
