#------------------------------------------------------------------------------
#$Date: 2018-08-14 11:04:39 +0300 (Tue, 14 Aug 2018) $
#$Revision: 209668 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/30/01/2300106.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_2300106
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                 117.59(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9348(7)
_cell_length_b                   21.9329(16)
_cell_length_c                   11.484(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    200.0(10)
_cell_measurement_theta_max      26.8
_cell_measurement_theta_min      21.5
_cell_volume                     2441.0(12)
_computing_cell_refinement       'Enraf Nonius Software V5'
_computing_data_collection       'Enraf Nonius Software V5'
_computing_data_reduction        'Corinc (Dräger, 1971)'
_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      200.0(10)
_diffrn_detector_area_resol_mean 'point detector'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CAD4 Enraf Nonius'
_diffrn_measurement_method       θ/2ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5190
_diffrn_reflns_theta_full        73.62
_diffrn_reflns_theta_max         73.62
_diffrn_reflns_theta_min         4.03
_diffrn_standards_decay_%        2.9
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.151
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.150
_refine_diff_density_min         -1.283
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0757
_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)+(0.1071P)²+2.3150P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.1991
_reflns_number_gt                3585
_reflns_number_total             4939
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             2300095
_cod_data_source_file            aj5030.cif
_cod_data_source_block           fepic200
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+2.3150P] 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^)+(0.1071P)^2^+2.3150P] 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        2441.0(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2300106
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 0.02826(7) 0.13452(3) 0.80631(7) 0.0252(2) Uani d . 1 . . Fe
Cl2 0.25376(13) 0.27338(6) 1.07564(14) 0.0414(3) Uani d . 1 . . Cl
Cl1 -0.13745(12) 0.06834(6) 1.05956(12) 0.0327(3) Uani d . 1 . . Cl
N6 -0.1474(4) 0.19467(19) 0.7692(4) 0.0292(9) Uani d . 1 . . N
N4 0.2416(4) 0.10346(19) 0.8798(5) 0.0333(9) Uani d . 1 . . N
N1 -0.0694(4) 0.04893(18) 0.8119(4) 0.0286(9) Uani d . 1 . . N
H1A -0.1122 0.0528 0.8686 0.034 Uiso d R 1 . . H
H1B 0.0036 0.0205 0.8356 0.034 Uiso d R 1 . . H
N5 0.0884(4) 0.22268(19) 0.7611(4) 0.0317(9) Uani d . 1 . . N
H5A 0.1397 0.2374 0.8499 0.038 Uiso d R 1 . . H
H5B 0.1676 0.2251 0.7358 0.038 Uiso d R 1 . . H
N3 0.1093(4) 0.1376(2) 1.0195(4) 0.0329(9) Uani d . 1 . . N
H3A 0.0466 0.1326 1.0354 0.039 Uiso d R 1 . . H
H3B 0.1311 0.1777 1.0268 0.039 Uiso d R 1 . . H
N2 -0.0571(4) 0.09854(19) 0.6039(4) 0.0287(9) Uani d . 1 . . N
C2 -0.1430(5) 0.0509(2) 0.5757(5) 0.0296(10) Uani d . 1 . . C
C15 -0.2613(6) 0.2875(3) 0.6678(6) 0.0415(13) Uani d . 1 . . C
H15 -0.2627 0.3240 0.6226 0.050 Uiso calc R 1 . . H
O32 0.3060(7) 0.3868(3) 0.9371(8) 0.109(3) Uani d . 1 . . O
H32 0.279(3) 0.340(5) 0.985(5) 0.163 Uiso calc R 1 . . H
C18 -0.2509(5) 0.1836(2) 0.7985(5) 0.0354(11) Uani d . 1 . . C
H18 -0.2467 0.1475 0.8460 0.042 Uiso calc R 1 . . H
C5 -0.0731(6) 0.0900(3) 0.3890(5) 0.0407(13) Uani d . 1 . . C
H5 -0.0475 0.1045 0.3254 0.049 Uiso calc R 1 . . H
C8 0.3076(5) 0.0909(2) 1.0106(6) 0.0333(11) Uani d . 1 . . C
C13 -0.0335(6) 0.2599(2) 0.6768(6) 0.0389(13) Uani d . 1 . . C
H13A -0.0616 0.2507 0.5834 0.047 Uiso calc R 1 . . H
H13B -0.0090 0.3036 0.6920 0.047 Uiso calc R 1 . . H
C11 0.4551(6) 0.0886(3) 0.8723(8) 0.0511(17) Uani d . 1 . . C
H11 0.5041 0.0886 0.8222 0.061 Uiso calc R 1 . . H
C3 -0.1977(6) 0.0212(3) 0.4551(5) 0.0400(12) Uani d . 1 . . C
H3 -0.2590 -0.0122 0.4378 0.048 Uiso calc R 1 . . H
C14 -0.1520(5) 0.2471(2) 0.7054(5) 0.0324(11) Uani d . 1 . . C
C16 -0.3675(6) 0.2745(3) 0.6961(7) 0.0444(14) Uani d . 1 . . C
H16 -0.4436 0.3016 0.6696 0.053 Uiso calc R 1 . . H
C1 -0.1786(6) 0.0313(3) 0.6830(5) 0.0382(12) Uani d . 1 . . C
H1AA -0.2665 0.0505 0.6683 0.046 Uiso calc R 1 . . H
H1BB -0.1909 -0.0135 0.6799 0.046 Uiso calc R 1 . . H
C9 0.4465(5) 0.0765(3) 1.0741(7) 0.0438(14) Uani d . 1 . . C
H9 0.4904 0.0675 1.1654 0.053 Uiso calc R 1 . . H
C6 -0.0228(6) 0.1174(3) 0.5098(5) 0.0355(11) Uani d . 1 . . C
H6 0.0386 0.1509 0.5287 0.043 Uiso calc R 1 . . H
C4 -0.1620(6) 0.0409(3) 0.3613(6) 0.0451(14) Uani d . 1 . . C
H4 -0.1979 0.0211 0.2784 0.054 Uiso calc R 1 . . H
C7 0.2204(5) 0.0921(3) 1.0793(5) 0.0372(12) Uani d . 1 . . C
H7A 0.1796 0.0513 1.0742 0.045 Uiso calc R 1 . . H
H7B 0.2786 0.1022 1.1731 0.045 Uiso calc R 1 . . H
C12 0.3165(6) 0.1022(3) 0.8145(7) 0.0425(13) Uani d . 1 . . C
H12 0.2712 0.1112 0.7232 0.051 Uiso calc R 1 . . H
C17 -0.3626(5) 0.2215(3) 0.7636(6) 0.0410(13) Uani d . 1 . . C
H17 -0.4343 0.2117 0.7852 0.049 Uiso calc R 1 . . H
C31 0.4467(9) 0.3881(4) 0.9739(11) 0.086(3) Uani d . 1 . . C
H31A 0.4982 0.3884 1.0710 0.103 Uiso calc R 1 . . H
H31B 0.4674 0.4269 0.9424 0.103 Uiso calc R 1 . . H
C30 0.4979(11) 0.3391(6) 0.9270(9) 0.111(4) Uani d . 1 . . C
H30A 0.4950 0.3012 0.9709 0.167 Uiso calc R 1 . . H
H30B 0.5933 0.3478 0.9460 0.167 Uiso calc R 1 . . H
H30C 0.4405 0.3348 0.8319 0.167 Uiso calc R 1 . . H
C10 0.5213(6) 0.0750(3) 1.0049(8) 0.0527(17) Uani d . 1 . . C
H10 0.6166 0.0649 1.0476 0.063 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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 . . 168.06(16) ?
N1 Fe1 N3 . . 86.73(16) ?
N5 Fe1 N3 . . 103.24(17) ?
N1 Fe1 N4 . . 99.79(16) ?
N5 Fe1 N4 . . 89.01(16) ?
N3 Fe1 N4 . . 76.76(16) ?
N1 Fe1 N6 . . 97.27(15) ?
N5 Fe1 N6 . . 75.81(15) ?
N3 Fe1 N6 . . 93.62(16) ?
N4 Fe1 N6 . . 159.82(16) ?
N1 Fe1 N2 . . 75.46(15) ?
N5 Fe1 N2 . . 95.36(16) ?
N3 Fe1 N2 . . 160.68(16) ?
N4 Fe1 N2 . . 98.64(16) ?
N6 Fe1 N2 . . 95.99(16) ?
C18 N6 C14 . . 117.7(4) ?
C18 N6 Fe1 . . 127.1(3) ?
C14 N6 Fe1 . . 115.1(3) ?
C12 N4 C8 . . 117.6(5) ?
C12 N4 Fe1 . . 127.4(4) ?
C8 N4 Fe1 . . 114.5(3) ?
C1 N1 Fe1 . . 112.4(3) ?
C13 N5 Fe1 . . 111.4(3) ?
C7 N3 Fe1 . . 108.7(3) ?
C2 N2 C6 . . 117.7(4) ?
C2 N2 Fe1 . . 116.1(3) ?
C6 N2 Fe1 . . 126.0(4) ?
N2 C2 C3 . . 122.4(5) ?
N2 C2 C1 . . 116.1(4) ?
C3 C2 C1 . . 121.5(5) ?
C16 C15 C14 . . 119.7(5) ?
N6 C18 C17 . . 123.7(5) ?
C6 C5 C4 . . 118.8(5) ?
N4 C8 C9 . . 121.3(5) ?
N4 C8 C7 . . 116.0(4) ?
C9 C8 C7 . . 122.7(5) ?
N5 C13 C14 . . 111.2(4) ?
C12 C11 C10 . . 118.4(6) ?
C4 C3 C2 . . 119.1(5) ?
N6 C14 C15 . . 121.5(5) ?
N6 C14 C13 . . 117.2(4) ?
C15 C14 C13 . . 121.3(5) ?
C15 C16 C17 . . 119.3(5) ?
N1 C1 C2 . . 110.6(4) ?
C10 C9 C8 . . 120.1(6) ?
N2 C6 C5 . . 122.8(5) ?
C3 C4 C5 . . 119.2(5) ?
N3 C7 C8 . . 110.9(4) ?
N4 C12 C11 . . 123.8(6) ?
C18 C17 C16 . . 118.0(5) ?
O32 C31 C30 . . 116.2(10) ?
C9 C10 C11 . . 118.8(5) ?
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 . 2.175(4) ?
Fe1 N5 . 2.181(4) ?
Fe1 N3 . 2.185(4) ?
Fe1 N4 . 2.190(4) ?
Fe1 N6 . 2.203(4) ?
Fe1 N2 . 2.210(4) ?
N6 C18 . 1.344(6) ?
N6 C14 . 1.352(6) ?
N4 C12 . 1.342(6) ?
N4 C8 . 1.360(7) ?
N1 C1 . 1.459(6) ?
N5 C13 . 1.477(7) ?
N3 C7 . 1.472(6) ?
N2 C2 . 1.340(6) ?
N2 C6 . 1.362(6) ?
C2 C3 . 1.390(7) ?
C2 C1 . 1.516(7) ?
C15 C16 . 1.374(8) ?
C15 C14 . 1.386(7) ?
O32 C31 . 1.395(10) ?
C18 C17 . 1.375(7) ?
C5 C6 . 1.372(8) ?
C5 C4 . 1.386(8) ?
C8 C9 . 1.383(7) ?
C8 C7 . 1.493(7) ?
C13 C14 . 1.503(7) ?
C11 C12 . 1.377(8) ?
C11 C10 . 1.382(10) ?
C3 C4 . 1.375(8) ?
C16 C17 . 1.383(8) ?
C9 C10 . 1.379(9) ?
C31 C30 . 1.426(13) ?
