#------------------------------------------------------------------------------
#$Date: 2018-08-14 11:04:39 +0300 (Tue, 14 Aug 2018) $
#$Revision: 209668 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/30/01/2300109.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_2300109
loop_
_publ_author_name
'Kusz, Joachim'
'Schollmeyer, Dieter'
'Spiering, Hartmunt'
'Gütlich, Philipp'
_publ_section_title
;
 The LIESST state of [Fe(pic)₃]Cl₂.EtOH -- the superstructure under
 continuous irradiation
;
_journal_coden_ASTM              JACGAR
_journal_issue                   3
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              528
_journal_page_last               536
_journal_paper_doi               10.1107/S0021889805009891
_journal_volume                  38
_journal_year                    2005
_chemical_formula_moiety         'C18 H24 Fe N6, C2 H6 O, 2(Cl)'
_chemical_formula_sum            'C20 H30 Cl2 Fe N6 O'
_chemical_formula_weight         497.25
_chemical_name_common
;
 tris(2-Picolylamine)-iron(ii) chloride ethanol solvate
;
_chemical_name_systematic
;
 tris(2-Picolylamine)-iron(ii) chloride ethanol solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 118.85(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.949(3)
_cell_length_b                   21.825(5)
_cell_length_c                   11.370(2)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    10.0(10)
_cell_measurement_theta_max      40
_cell_measurement_theta_min      30
_cell_volume                     2379.8(11)
_computing_cell_refinement       'STADI4 (Stoe, 1995)'
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      10.0(10)
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'CCD Oxford Diffraction'
_diffrn_measurement_method       φ-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1417
_diffrn_reflns_av_sigmaI/netI    0.1131
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19183
_diffrn_reflns_theta_full        27.80
_diffrn_reflns_theta_max         27.80
_diffrn_reflns_theta_min         3.83
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.948
_refine_diff_density_min         -1.423
_refine_ls_extinction_coef       0.0051(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.1643
_refine_ls_R_factor_gt           0.1392
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0740P)²+44.0563P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2916
_refine_ls_wR_factor_ref         0.3084
_reflns_number_gt                4081
_reflns_number_total             5279
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             2300098
_cod_data_source_file            aj5030.cif
_cod_data_source_block           fpic11hs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+44.0563P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+44.0563P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2379.9(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2300109
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_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
_atom_site_type_symbol
Fe1 0.02784(12) 0.13510(5) 0.80841(13) 0.0144(4) Uani d . 1 . . Fe
Cl2 0.2583(2) 0.27291(9) 1.0835(2) 0.0176(5) Uani d . 1 . . Cl
Cl1 -0.1442(2) 0.06714(9) 1.0540(2) 0.0165(5) Uani d . 1 . . Cl
N6 -0.1496(7) 0.1952(3) 0.7665(7) 0.0169(15) Uani d . 1 . . N
N4 0.2453(7) 0.1034(3) 0.8899(8) 0.0177(15) Uani d . 1 . . N
N1 -0.0713(7) 0.0489(3) 0.8111(7) 0.0149(14) Uani d . 1 . . N
H1A -0.1142 0.0527 0.8678 0.018 Uiso d R 1 . . H
H1B 0.0016 0.0204 0.8348 0.018 Uiso d R 1 . . H
N5 0.0889(7) 0.2236(3) 0.7640(7) 0.0146(14) Uani d . 1 . . N
H5A 0.1402 0.2383 0.8528 0.018 Uiso d R 1 . . H
H5B 0.1681 0.2260 0.7387 0.018 Uiso d R 1 . . H
N3 0.1088(7) 0.1378(3) 1.0259(8) 0.0177(15) Uani d . 1 . . N
H3A 0.0462 0.1329 1.0419 0.021 Uiso d R 1 . . H
H3B 0.1307 0.1780 1.0332 0.021 Uiso d R 1 . . H
N2 -0.0567(7) 0.0996(3) 0.6005(7) 0.0146(14) Uani d . 1 . . N
C2 -0.1458(8) 0.0510(4) 0.5700(9) 0.0136(16) Uani d . 1 . . C
C15 -0.2610(8) 0.2909(4) 0.6717(9) 0.0156(17) Uani d . 1 . . C
H15 -0.2602 0.3286 0.6303 0.019 Uiso calc R 1 . . H
O32 0.2989(6) 0.3873(3) 0.9360(7) 0.0213(14) Uani d . 1 . . O
H32 0.279(3) 0.354(5) 0.965(4) 0.032 Uiso calc R 1 . . H
C18 -0.2517(8) 0.1839(4) 0.7987(9) 0.0158(17) Uani d . 1 . . C
H18 -0.2470 0.1471 0.8454 0.019 Uiso calc R 1 . . H
C5 -0.0673(9) 0.0891(4) 0.3862(9) 0.0160(17) Uani d . 1 . . C
H5 -0.0402 0.1040 0.3237 0.019 Uiso calc R 1 . . H
C8 0.3077(8) 0.0897(4) 1.0211(8) 0.0137(16) Uani d . 1 . . C
C13 -0.0359(8) 0.2606(3) 0.6748(8) 0.0104(15) Uani d . 1 . . C
H13A -0.0665 0.2502 0.5799 0.012 Uiso calc R 1 . . H
H13B -0.0117 0.3047 0.6877 0.012 Uiso calc R 1 . . H
C11 0.4613(8) 0.0892(4) 0.8879(9) 0.0158(17) Uani d . 1 . . C
H11 0.5121 0.0895 0.8397 0.019 Uiso calc R 1 . . H
C3 -0.1947(8) 0.0197(4) 0.4495(9) 0.0174(17) Uani d . 1 . . C
H3 -0.2544 -0.0147 0.4312 0.021 Uiso calc R 1 . . H
C14 -0.1546(9) 0.2482(4) 0.7060(9) 0.0189(18) Uani d . 1 . . C
C16 -0.3675(9) 0.2773(4) 0.6992(10) 0.0194(18) Uani d . 1 . . C
H16 -0.4438 0.3047 0.6722 0.023 Uiso calc R 1 . . H
C1 -0.1830(9) 0.0329(4) 0.6757(9) 0.0185(18) Uani d . 1 . . C
H1AA -0.2702 0.0539 0.6586 0.022 Uiso calc R 1 . . H
H1BB -0.2000 -0.0118 0.6707 0.022 Uiso calc R 1 . . H
C9 0.4487(9) 0.0740(4) 1.0904(9) 0.0191(18) Uani d . 1 . . C
H9 0.4909 0.0633 1.1828 0.023 Uiso calc R 1 . . H
C6 -0.0188(8) 0.1172(4) 0.5105(8) 0.0134(16) Uani d . 1 . . C
H6 0.0444 0.1506 0.5323 0.016 Uiso calc R 1 . . H
C4 -0.1557(9) 0.0391(4) 0.3544(10) 0.0200(18) Uani d . 1 . . C
H4 -0.1888 0.0185 0.2709 0.024 Uiso calc R 1 . . H
C7 0.2164(8) 0.0899(4) 1.0862(9) 0.0165(17) Uani d . 1 . . C
H7A 0.1713 0.0494 1.0743 0.020 Uiso calc R 1 . . H
H7B 0.2741 0.0976 1.1837 0.020 Uiso calc R 1 . . H
C12 0.3191(9) 0.1040(4) 0.8237(9) 0.0177(17) Uani d . 1 . . C
H12 0.2738 0.1147 0.7313 0.021 Uiso calc R 1 . . H
C17 -0.3632(9) 0.2236(4) 0.7664(10) 0.0206(19) Uani d . 1 . . C
H17 -0.4336 0.2142 0.7896 0.025 Uiso calc R 1 . . H
C31 0.4464(9) 0.3895(4) 0.9810(9) 0.0212(19) Uani d . 1 . . C
H31A 0.4975 0.3902 1.0804 0.025 Uiso calc R 1 . . H
H31B 0.4682 0.4280 0.9488 0.025 Uiso calc R 1 . . H
C30 0.4973(10) 0.3359(5) 0.9324(11) 0.027(2) Uani d . 1 . . C
H30A 0.4939 0.2985 0.9785 0.041 Uiso calc R 1 . . H
H30B 0.5934 0.3435 0.9518 0.041 Uiso calc R 1 . . H
H30C 0.4375 0.3310 0.8354 0.041 Uiso calc R 1 . . H
C10 0.5270(8) 0.0741(4) 1.0245(9) 0.0188(18) Uani d . 1 . . C
H10 0.6233 0.0641 1.0710 0.023 Uiso calc R 1 . . H
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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Fe1 N5 . . 167.9(3) ?
N1 Fe1 N3 . . 86.6(3) ?
N5 Fe1 N3 . . 103.6(3) ?
N1 Fe1 N6 . . 97.1(3) ?
N5 Fe1 N6 . . 76.0(3) ?
N3 Fe1 N6 . . 93.6(3) ?
N1 Fe1 N4 . . 99.6(3) ?
N5 Fe1 N4 . . 89.2(3) ?
N3 Fe1 N4 . . 76.6(3) ?
N6 Fe1 N4 . . 159.9(3) ?
N1 Fe1 N2 . . 76.1(3) ?
N5 Fe1 N2 . . 94.5(3) ?
N3 Fe1 N2 . . 161.1(3) ?
N6 Fe1 N2 . . 96.1(3) ?
N4 Fe1 N2 . . 98.5(3) ?
C14 N6 C18 . . 117.6(7) ?
C14 N6 Fe1 . . 116.2(6) ?
C18 N6 Fe1 . . 126.2(6) ?
C8 N4 C12 . . 120.3(7) ?
C8 N4 Fe1 . . 113.8(5) ?
C12 N4 Fe1 . . 125.5(6) ?
C1 N1 Fe1 . . 110.9(5) ?
C13 N5 Fe1 . . 110.8(5) ?
C7 N3 Fe1 . . 107.7(5) ?
C6 N2 C2 . . 118.5(7) ?
C6 N2 Fe1 . . 126.3(6) ?
C2 N2 Fe1 . . 114.8(5) ?
N2 C2 C3 . . 121.3(8) ?
N2 C2 C1 . . 116.0(7) ?
C3 C2 C1 . . 122.6(7) ?
C16 C15 C14 . . 118.6(8) ?
N6 C18 C17 . . 123.1(8) ?
C4 C5 C6 . . 119.4(8) ?
N4 C8 C9 . . 120.9(8) ?
N4 C8 C7 . . 116.4(7) ?
C9 C8 C7 . . 122.7(8) ?
N5 C13 C14 . . 110.5(6) ?
C10 C11 C12 . . 118.6(8) ?
C2 C3 C4 . . 119.8(8) ?
N6 C14 C15 . . 123.1(8) ?
N6 C14 C13 . . 116.5(7) ?
C15 C14 C13 . . 120.5(7) ?
C15 C16 C17 . . 119.9(8) ?
N1 C1 C2 . . 111.5(7) ?
C10 C9 C8 . . 120.0(8) ?
N2 C6 C5 . . 123.0(8) ?
C5 C4 C3 . . 117.9(9) ?
N3 C7 C8 . . 110.2(7) ?
N4 C12 C11 . . 121.6(8) ?
C16 C17 C18 . . 117.6(8) ?
O32 C31 C30 . . 113.1(8) ?
C9 C10 C11 . . 118.7(8) ?
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 . 2.181(7) ?
Fe1 N5 . 2.182(7) ?
Fe1 N3 . 2.189(8) ?
Fe1 N6 . 2.197(7) ?
Fe1 N4 . 2.208(7) ?
Fe1 N2 . 2.221(7) ?
N6 C14 . 1.334(11) ?
N6 C18 . 1.356(11) ?
N4 C8 . 1.342(11) ?
N4 C12 . 1.344(11) ?
N1 C1 . 1.473(11) ?
N5 C13 . 1.487(10) ?
N3 C7 . 1.474(10) ?
N2 C6 . 1.333(10) ?
N2 C2 . 1.369(10) ?
C2 C3 . 1.386(12) ?
C2 C1 . 1.496(12) ?
C15 C16 . 1.376(12) ?
C15 C14 . 1.392(11) ?
O32 C31 . 1.440(10) ?
C18 C17 . 1.394(12) ?
C5 C4 . 1.386(12) ?
C5 C6 . 1.390(12) ?
C8 C9 . 1.395(11) ?
C8 C7 . 1.503(11) ?
C13 C14 . 1.528(11) ?
C11 C10 . 1.401(13) ?
C11 C12 . 1.401(11) ?
C3 C4 . 1.406(12) ?
C16 C17 . 1.389(12) ?
C9 C10 . 1.384(12) ?
C31 C30 . 1.510(13) ?
