#------------------------------------------------------------------------------
#$Date: 2017-07-10 18:33:26 +0300 (Mon, 10 Jul 2017) $
#$Revision: 198601 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/76/2007681.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_2007681
loop_
_publ_author_name
'Karsten, Peter'
'Strähle, Joachim'
_publ_section_title
;
 Bis(1,8-diazabicyclo[5.4.0]undec-7-en-8-ium)
 trans-Dichlorotetra(pyridine-N)iron(II) Dichloride
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1406
_journal_page_last               1408
_journal_paper_doi               10.1107/S0108270198005873
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          '(C9 H17 N2)2 [Fe Cl2 (C5 H5 N1)4] Cl2'
_chemical_formula_moiety         'C20 H20 Cl2 Fe N4 , 2(C9 H17 N2) , 2Cl'
_chemical_formula_sum            'C38 H54 Cl4 Fe N8'
_chemical_formula_weight         820.54
_chemical_name_systematic
;
 trans-Bis(chloro)tetrakis(pyridine)iron(II)
Di(1,8-diazabicyclo[5.4.0]undec-7-ene hydrochloride)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                93.626(12)
_cell_angle_beta                 101.703(11)
_cell_angle_gamma                101.479(10)
_cell_formula_units_Z            1
_cell_length_a                   7.2582(14)
_cell_length_b                   9.585(2)
_cell_length_c                   15.470(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      15.5
_cell_volume                     1026.8(4)
_computing_cell_refinement
'SET4 (de Boer & Duisenberg, 1984) in CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'SDP (Enraf-Nonius, 1985)'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1994)'
_computing_publication_material
;
SHELXL93. Computations were performed on a DEC VAX Station 3100,
a CONVEX C3860 and a Pentium 120 PC
;
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.129
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4384
_diffrn_reflns_theta_max         64.84
_diffrn_reflns_theta_min         5.29
_diffrn_standards_decay_%        0.8
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.629
_exptl_absorpt_correction_T_max  0.570
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.824
_refine_diff_density_min         -1.138
_refine_ls_extinction_coef       0.033(2)
_refine_ls_extinction_method     SHELXL93
_refine_ls_goodness_of_fit_all   1.117
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    'H atoms calculated at idealized positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_restrained_S_obs      1.128
_refine_ls_R_factor_all          0.060
_refine_ls_R_factor_gt           0.054
_refine_ls_shift/su_max          <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0819P)²+0.9531P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.161
_refine_ls_wR_factor_ref         0.154
_reflns_number_gt                3140
_reflns_number_total             3497
_reflns_threshold_expression     F>2σ(F)
_cod_data_source_file            av1020.cif
_cod_data_source_block           av1020
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value '\y scan' was replaced with
the value 'psi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        1026.7(3)
_cod_original_formula_sum        'C38 H54 Cl4 Fe1 N8'
_cod_database_code               2007681
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_group
_atom_site_type_symbol
Fe1 0 0 0 0.0336(3) Uani d S 1 . Fe
Cl1 -0.22128(11) 0.06550(10) 0.08369(5) 0.0401(3) Uani d . 1 . Cl
Cl2 0.74453(14) 0.68453(11) 0.39128(7) 0.0556(3) Uani d . 1 . Cl
N1 0.1385(4) -0.1033(3) 0.1178(2) 0.0377(7) Uani d . 1 . N
N2 0.1962(4) 0.2204(3) 0.0423(2) 0.0384(7) Uani d . 1 . N
N10 -0.1519(4) 0.1539(4) 0.3825(2) 0.0419(7) Uani d . 1 . N
N11 -0.2247(5) 0.3701(4) 0.4191(2) 0.0505(8) Uani d . 1 . N
H100 -0.233(6) 0.458(6) 0.406(3) 0.051(12) Uiso d . 1 . H
C11 0.0311(5) -0.1735(4) 0.1688(2) 0.0404(8) Uani d . 1 . C
H11 -0.1008(5) -0.1774(4) 0.1551(2) 0.049 Uiso calc R 1 . H
C12 0.1037(6) -0.2401(5) 0.2401(3) 0.0466(9) Uani d . 1 . C
H12 0.0226(6) -0.2885(5) 0.2731(3) 0.056 Uiso calc R 1 . H
C13 0.3003(6) -0.2335(5) 0.2617(3) 0.0483(9) Uani d . 1 . C
H13 0.3545(6) -0.2772(5) 0.3096(3) 0.058 Uiso calc R 1 . H
C14 0.4135(5) -0.1608(5) 0.2106(3) 0.0474(9) Uani d . 1 . C
H14 0.5461(5) -0.1537(5) 0.2239(3) 0.057 Uiso calc R 1 . H
C15 0.3289(5) -0.0987(4) 0.1396(2) 0.0422(8) Uani d . 1 . C
H15 0.4070(5) -0.0512(4) 0.1051(2) 0.051 Uiso calc R 1 . H
C21 0.3893(5) 0.2413(5) 0.0583(3) 0.0459(9) Uani d . 1 . C
H21 0.4437(5) 0.1644(5) 0.0460(3) 0.055 Uiso calc R 1 . H
C22 0.5100(6) 0.3715(5) 0.0922(3) 0.0595(11) Uani d . 1 . C
H22 0.6429(6) 0.3809(5) 0.1037(3) 0.071 Uiso calc R 1 . H
C23 0.4330(7) 0.4870(5) 0.1089(4) 0.0657(13) Uani d . 1 . C
H23 0.5120(7) 0.5756(5) 0.1323(4) 0.079 Uiso calc R 1 . H
C24 0.2353(6) 0.4685(5) 0.0903(3) 0.0577(11) Uani d . 1 . C
H24 0.1784(6) 0.5453(5) 0.0996(3) 0.069 Uiso calc R 1 . H
C25 0.1239(5) 0.3359(5) 0.0578(3) 0.0457(9) Uani d . 1 . C
H25 -0.0094(5) 0.3250(5) 0.0457(3) 0.055 Uiso calc R 1 . H
C31 -0.2036(6) 0.0950(5) 0.4621(3) 0.0498(9) Uani d . 1 . C
H31A -0.0898(6) 0.1116(5) 0.5100(3) 0.060 Uiso calc R 1 . H
H31B -0.2538(6) -0.0075(5) 0.4495(3) 0.060 Uiso calc R 1 . H
C32 -0.3521(6) 0.1649(5) 0.4899(3) 0.0549(10) Uani d . 1 . C
H32A -0.3741(6) 0.1343(5) 0.5462(3) 0.066 Uiso calc R 1 . H
H32B -0.4727(6) 0.1353(5) 0.4461(3) 0.066 Uiso calc R 1 . H
C33 -0.2885(7) 0.3243(5) 0.4989(3) 0.0571(11) Uani d . 1 . C
H33A -0.3944(7) 0.3677(5) 0.5072(3) 0.069 Uiso calc R 1 . H
H33B -0.1836(7) 0.3557(5) 0.5506(3) 0.069 Uiso calc R 1 . H
C34 -0.1577(5) 0.2874(4) 0.3677(2) 0.0446(9) Uani d . 1 . C
C35 -0.0784(7) 0.3512(5) 0.2936(3) 0.0565(11) Uani d . 1 . C
H35A -0.1164(7) 0.4417(5) 0.2851(3) 0.068 Uiso calc R 1 . H
H35B -0.1330(7) 0.2877(5) 0.2392(3) 0.068 Uiso calc R 1 . H
C36 0.1413(7) 0.3762(5) 0.3120(3) 0.0633(12) Uani d . 1 . C
H36A 0.1884(7) 0.4489(5) 0.2762(3) 0.076 Uiso calc R 1 . H
H36B 0.1929(7) 0.4135(5) 0.3738(3) 0.076 Uiso calc R 1 . H
C37 0.2183(7) 0.2447(5) 0.2933(3) 0.0583(11) Uani d . 1 . C
H37A 0.3580(7) 0.2714(5) 0.3060(3) 0.070 Uiso calc R 1 . H
H37B 0.1741(7) 0.2110(5) 0.2306(3) 0.070 Uiso calc R 1 . H
C38 0.1583(6) 0.1228(5) 0.3466(3) 0.0502(10) Uani d . 1 . C
H38A 0.2071(6) 0.1552(5) 0.4093(3) 0.060 Uiso calc R 1 . H
H38B 0.2176(6) 0.0446(5) 0.3324(3) 0.060 Uiso calc R 1 . H
C39 -0.0581(5) 0.0671(4) 0.3298(2) 0.0438(9) Uani d . 1 . C
H39A -0.1136(5) 0.0668(4) 0.2672(2) 0.053 Uiso calc R 1 . H
H39B -0.0842(5) -0.0309(4) 0.3442(2) 0.053 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'
N N 0.0311 0.0180 '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'
Cl Cl 0.3639 0.7018 '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'
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
Cl1 Fe1 Cl1 . 2 180.0 yes
Cl1 Fe1 N1 . . 89.81(7) yes
Cl1 Fe1 N1 . 2 90.19(7) yes
Cl1 Fe1 N1 2 . 90.19(7) yes
Cl1 Fe1 N1 2 2 89.81(7) no
Cl1 Fe1 N2 . . 89.75(7) yes
Cl1 Fe1 N2 . 2 90.25(7) yes
Cl1 Fe1 N2 2 . 90.25(7) yes
Cl1 Fe1 N2 2 2 89.75(7) no
N1 Fe1 N1 . 2 180.0 yes
N1 Fe1 N2 . . 95.23(11) yes
N1 Fe1 N2 . 2 84.77(11) yes
N1 Fe1 N2 2 . 84.77(11) yes
N1 Fe1 N2 2 2 95.23(11) no
N2 Fe1 N2 . 2 180.0 yes
Fe1 N1 C11 . . 120.6(2) yes
Fe1 N1 C15 . . 122.8(2) yes
Fe1 N2 C21 . . 122.4(2) yes
Fe1 N2 C25 . . 121.1(2) yes
N1 C11 C12 . . 124.0(3) yes
C11 C12 C13 . . 118.5(4) yes
C12 C13 C14 . . 118.4(4) yes
C13 C14 C15 . . 119.4(4) yes
C14 C15 N1 . . 123.1(3) yes
C15 N1 C11 . . 116.6(3) yes
N2 C21 C22 . . 123.0(4) yes
C21 C22 C23 . . 119.5(4) yes
C22 C23 C24 . . 118.3(4) yes
C23 C24 C25 . . 119.1(4) yes
C24 C25 N2 . . 123.6(3) yes
C25 N2 C21 . . 116.4(3) yes
N10 C31 C32 . . 109.9(3) yes
N10 C34 C35 . . 120.3(3) yes
N10 C39 C38 . . 112.7(3) yes
N10 C34 N11 . . 121.7(4) yes
N11 C33 C32 . . 110.0(3) yes
N11 C34 C35 . . 117.8(4) yes
C31 N10 C34 . . 121.3(3) yes
C31 N10 C39 . . 116.6(3) yes
C34 N10 C39 . . 121.0(3) yes
C33 N11 C34 . . 122.9(4) yes
C31 C32 C33 . . 110.8(4) yes
C34 C35 C36 . . 112.1(3) yes
C35 C36 C37 . . 114.8(4) yes
C36 C37 C38 . . 114.1(4) yes
C37 C38 C39 . . 113.9(3) yes
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 Cl1 . 2.4067(8) yes
Fe1 Cl1 2 2.4067(8) yes
Fe1 N1 . 2.279(3) yes
Fe1 N1 2 2.279(3) yes
Fe1 N2 . 2.273(3) yes
Fe1 N2 2 2.273(3) yes
N1 C11 . 1.338(5) yes
N1 C15 . 1.345(4) yes
N2 C21 . 1.344(4) yes
N2 C25 . 1.344(5) yes
N10 C34 . 1.322(5) yes
N10 C31 . 1.472(5) yes
N10 C39 . 1.478(5) yes
N11 C34 . 1.314(5) yes
N11 C33 . 1.466(6) yes
C11 C12 . 1.374(5) yes
C12 C13 . 1.386(5) yes
C13 C14 . 1.375(6) yes
C14 C15 . 1.375(5) yes
C21 C22 . 1.377(6) yes
C22 C23 . 1.369(7) yes
C23 C24 . 1.378(6) yes
C24 C25 . 1.367(6) yes
C31 C32 . 1.494(6) yes
C32 C33 . 1.495(7) yes
C34 C35 . 1.495(6) yes
C35 C36 . 1.528(7) yes
C36 C37 . 1.512(7) yes
C37 C38 . 1.517(7) yes
C38 C39 . 1.517(6) yes
