#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/62/2016261.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2016261
loop_
_publ_author_name
'Collins, Sibrina N.'
'Krause, Jeanette A.'
'Regis, Morrisa'
'Ball, P. J.'
'Connick, William B.'
_publ_section_title
;
 Self-assembly of a one-dimensional iron(II) coordination polymer with
 p-phenylenebis(picolinaldimine)
;
_journal_coeditor_code           GZ3097
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m528
_journal_page_last               m530
_journal_paper_doi               10.1107/S0108270107040796
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Fe Cl2 (C18 H14 N4)], 2C H4 O'
_chemical_formula_moiety         'C18 H14 Cl2 Fe N4, 2(C H4 O)'
_chemical_formula_sum            'C20 H22 Cl2 Fe N4 O2'
_chemical_formula_weight         477.17
_chemical_name_systematic
;
catena-Poly[[[dichloridoiron(II)]-μ-N,N'-bis(2-pyridylmethylene)benzene-\
1,4-diamine] methanol solvate]
;
_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                 128.152(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.646(3)
_cell_length_b                   9.3893(13)
_cell_length_c                   13.4869(19)
_cell_measurement_reflns_used    3685
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.76
_cell_measurement_theta_min      2.74
_cell_volume                     2055.9(5)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL and DIAMOND (Brandenburg, 2007)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2003)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0.75
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Platinum 200'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77500
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14014
_diffrn_reflns_theta_full        31.10
_diffrn_reflns_theta_max         31.10
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.283
_exptl_absorpt_correction_T_max  0.9873
_exptl_absorpt_correction_T_min  0.9565
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Blessing, 1995)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.765
_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     131
_refine_ls_number_reflns         2546
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0673P)²+3.4071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                2096
_reflns_number_total             2546
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            gz3097.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2016261
_cod_database_fobs_code          2016261
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.0000 0.18136(6) 0.2500 0.02424(18) Uani d S 1 . .
Cl Cl1 0.05342(5) 0.01125(8) 0.18386(7) 0.0359(2) Uani d . 1 . .
N N1 0.11058(14) 0.2288(3) 0.4396(2) 0.0256(5) Uani d . 1 . .
N N2 0.06189(14) 0.3638(3) 0.2290(2) 0.0256(5) Uani d . 1 . .
C C1 0.13654(18) 0.1586(3) 0.5444(3) 0.0317(6) Uani d . 1 . .
H H1 0.1060 0.0783 0.5376 0.038 Uiso calc R 1 . .
C C2 0.2065(2) 0.1986(4) 0.6629(3) 0.0384(7) Uani d . 1 . .
H H2 0.2236 0.1457 0.7355 0.046 Uiso calc R 1 . .
C C3 0.2509(2) 0.3155(4) 0.6744(3) 0.0390(7) Uani d . 1 . .
H H3 0.2989 0.3445 0.7547 0.047 Uiso calc R 1 . .
C C4 0.22415(18) 0.3903(3) 0.5662(3) 0.0335(6) Uani d . 1 . .
H H4 0.2533 0.4717 0.5711 0.040 Uiso calc R 1 . .
C C5 0.15458(17) 0.3440(3) 0.4519(3) 0.0270(5) Uani d . 1 . .
C C6 0.12394(18) 0.4161(3) 0.3333(3) 0.0303(6) Uani d . 1 . .
H H6 0.1499 0.5002 0.3342 0.036 Uiso calc R 1 . .
C C7 0.03157(16) 0.4355(3) 0.1139(2) 0.0269(5) Uani d . 1 . .
C C8 0.01959(18) 0.5820(3) 0.1012(3) 0.0299(6) Uani d . 1 . .
H H8 0.0326 0.6376 0.1703 0.036 Uiso calc R 1 . .
C C9 -0.01138(18) 0.6468(3) -0.0124(3) 0.0298(6) Uani d . 1 . .
H H9 -0.0189 0.7471 -0.0211 0.036 Uiso calc R 1 . .
O O10A 0.1566(5) -0.2242(7) 0.3795(6) 0.0837(15) Uiso d PD 0.714(11) A 1
O O10B 0.1192(11) -0.2584(17) 0.3628(12) 0.0837(15) Uiso d PD 0.286(11) A 2
H H10 0.1032 -0.2030 0.3089 0.126 Uiso d . 1 . .
C C10 0.1559(3) -0.2049(5) 0.4795(5) 0.0675(12) Uani d D 1 . .
H H10A 0.1488 -0.3051 0.4913 0.101 Uiso d P 0.71 A 3
H H10B 0.1068 -0.1446 0.4379 0.101 Uiso d P 0.71 A 3
H H10C 0.2106 -0.1632 0.5414 0.101 Uiso d P 0.71 A 3
H H10D 0.1573 -0.2724 0.5362 0.101 Uiso d P 0.29 A 4
H H10E 0.1247 -0.1283 0.4819 0.101 Uiso d P 0.29 A 4
H H10F 0.2121 -0.1670 0.5321 0.101 Uiso d P 0.29 A 4
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0020 '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 -0.0031 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1408 0.1896 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.2064 0.9932 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O -0.0041 0.0074 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Fe1 N1 2 . 156.38(13) y
N1 Fe1 N2 . 2 87.79(8) y
N1 Fe1 N2 . . 74.21(8) y
N2 Fe1 N2 2 . 81.25(12) y
N1 Fe1 Cl1 . 2 95.08(6) y
N1 Fe1 Cl1 . . 100.57(6) y
N2 Fe1 Cl1 2 . 167.39(6) y
N2 Fe1 Cl1 . . 91.87(6) y
Cl1 Fe1 Cl1 2 . 96.73(4) y
C1 N1 C5 . . 117.7(2) ?
C1 N1 Fe1 . . 125.9(2) ?
C5 N1 Fe1 . . 116.36(17) ?
C6 N2 C7 . . 118.8(2) ?
C6 N2 Fe1 . . 114.44(18) ?
C7 N2 Fe1 . . 126.15(17) ?
N1 C1 C2 . . 122.5(3) ?
N1 C1 H1 . . 118.8 ?
C2 C1 H1 . . 118.8 ?
C3 C2 C1 . . 119.5(3) ?
C3 C2 H2 . . 120.3 ?
C1 C2 H2 . . 120.3 ?
C2 C3 C4 . . 118.7(3) ?
C2 C3 H3 . . 120.7 ?
C4 C3 H3 . . 120.7 ?
C5 C4 C3 . . 118.6(3) ?
C5 C4 H4 . . 120.7 ?
C3 C4 H4 . . 120.7 ?
N1 C5 C4 . . 123.1(3) ?
N1 C5 C6 . . 115.4(2) ?
C4 C5 C6 . . 121.5(3) ?
N2 C6 C5 . . 119.0(3) ?
N2 C6 H6 . . 120.5 ?
C5 C6 H6 . . 120.5 ?
C8 C7 C9 . 5_565 120.3(2) ?
C8 C7 N2 . . 121.6(2) ?
C9 C7 N2 5_565 . 118.0(3) ?
C9 C8 C7 . . 119.8(3) ?
C9 C8 H8 . . 120.1 ?
C7 C8 H8 . . 120.1 ?
C8 C9 C7 . 5_565 119.8(3) ?
C8 C9 H9 . . 120.1 ?
C7 C9 H9 5_565 . 120.1 ?
C10 O10A H10 . . 104.6 ?
C10 O10B H10 . . 116.5 ?
O10B C10 H10A . . 78.4 ?
O10A C10 H10A . . 97.2 ?
O10B C10 H10B . . 84.9 ?
O10A C10 H10B . . 98.6 ?
H10A C10 H10B . . 116.3 ?
O10B C10 H10C . . 131.4 ?
O10A C10 H10C . . 100.6 ?
H10A C10 H10C . . 117.0 ?
H10B C10 H10C . . 119.8 ?
O10B C10 H10D . . 113.2 ?
O10A C10 H10D . . 132.1 ?
O10B C10 H10E . . 113.8 ?
O10A C10 H10E . . 122.5 ?
H10D C10 H10E . . 98.7 ?
O10B C10 H10F . . 122.6 ?
O10A C10 H10F . . 91.8 ?
H10D C10 H10F . . 102.7 ?
H10E C10 H10F . . 102.7 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N1 . 2.177(2) y
Fe1 N2 . 2.257(2) y
Fe1 Cl1 . 2.4040(8) y
N1 C1 . 1.335(3) ?
N1 C5 . 1.355(4) ?
N2 C6 . 1.278(4) ?
N2 C7 . 1.433(3) ?
C1 C2 . 1.390(4) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.375(5) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.390(4) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.376(4) ?
C4 H4 . 0.9500 ?
C5 C6 . 1.472(4) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.390(4) ?
C7 C9 5_565 1.393(4) ?
C8 C9 . 1.384(4) ?
C8 H8 . 0.9500 ?
C9 C7 5_565 1.393(4) ?
C9 H9 . 0.9500 ?
O10A C10 . 1.370(7) ?
O10A H10 . 0.9306 ?
O10B C10 . 1.353(13) ?
O10B H10 . 0.7827 ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9801 ?
C10 H10C . 0.9801 ?
C10 H10D . 0.9800 ?
C10 H10E . 0.9800 ?
C10 H10F . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O10A H10 Cl1 1_555 0.93 2.41 3.073(6) 128 y
O10B H10 Cl1 1_555 0.78 2.41 3.167(15) 163 y
C1 H1 Cl1 2_555 0.95 2.83 3.443(3) 123 y
C6 H6 O10B 1_565 0.95 2.46 3.091(16) 125 y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N1 Fe1 N1 C1 2 . 140.7(2)
N2 Fe1 N1 C1 2 . 100.9(2)
N2 Fe1 N1 C1 . . -177.6(2)
Cl1 Fe1 N1 C1 2 . 9.2(2)
Cl1 Fe1 N1 C1 1 . -88.6(2)
Cl1 Fe1 N1 C1 . . -88.6(2)
N1 Fe1 N1 C5 2 . -36.28(18)
N2 Fe1 N1 C5 2 . -76.1(2)
N2 Fe1 N1 C5 . . 5.42(19)
Cl1 Fe1 N1 C5 2 . -167.80(19)
Cl1 Fe1 N1 C5 1 . 94.38(19)
Cl1 Fe1 N1 C5 . . 94.38(19)
N1 Fe1 N2 C6 2 . 157.6(2)
N1 Fe1 N2 C6 . . -7.0(2)
N2 Fe1 N2 C6 2 . 83.2(2)
Cl1 Fe1 N2 C6 2 . 25.7(4)
Cl1 Fe1 N2 C6 1 . -107.4(2)
Cl1 Fe1 N2 C6 . . -107.4(2)
N1 Fe1 N2 C7 2 . -13.3(2)
N1 Fe1 N2 C7 . . -177.8(2)
N2 Fe1 N2 C7 2 . -87.6(2)
Cl1 Fe1 N2 C7 2 . -145.2(2)
Cl1 Fe1 N2 C7 1 . 81.8(2)
Cl1 Fe1 N2 C7 . . 81.8(2)
C5 N1 C1 C2 . . -0.7(4)
Fe1 N1 C1 C2 . . -177.7(2)
N1 C1 C2 C3 . . 0.6(5)
C1 C2 C3 C4 . . -0.1(5)
C2 C3 C4 C5 . . -0.3(5)
C1 N1 C5 C4 . . 0.3(4)
Fe1 N1 C5 C4 . . 177.6(2)
C1 N1 C5 C6 . . 179.2(2)
Fe1 N1 C5 C6 . . -3.6(3)
C3 C4 C5 N1 . . 0.2(5)
C3 C4 C5 C6 . . -178.6(3)
C7 N2 C6 C5 . . 179.1(2)
Fe1 N2 C6 C5 . . 7.6(3)
N1 C5 C6 N2 . . -2.9(4)
C4 C5 C6 N2 . . 175.9(3)
C6 N2 C7 C8 . . -46.3(4)
Fe1 N2 C7 C8 . . 124.2(2)
C6 N2 C7 C9 . 5_565 136.0(3)
Fe1 N2 C7 C9 . 5_565 -53.6(3)
C9 C7 C8 C9 5_565 . -1.0(5)
N2 C7 C8 C9 . . -178.7(3)
C7 C8 C9 C7 . 5_565 1.0(5)
