#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/95/2019520.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_2019520
loop_
_publ_author_name
'Lutz, Martin'
'Huang, Yuxing'
'Moret, Marc-Etienne'
'Klein Gebbink, Robertus J. M.'
_publ_section_title
;
 Phase transitions and twinned low-temperature structures of
 tetraethylammonium tetrachloridoferrate(III)
;
_journal_coeditor_code           GZ3264
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              470
_journal_page_last               476
_journal_paper_doi               10.1107/S2053229614007955
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '(C8 H20 N) [Fe Cl4]'
_chemical_formula_moiety         'C8 H20 N +, Cl4 Fe -'
_chemical_formula_sum            'C8 H20 Cl4 Fe N'
_chemical_formula_weight         327.90
_chemical_name_systematic
;
Tetraethylammonium tetrachloridoferrate(III)
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   24.5130(6)
_cell_length_b                   24.5130(6)
_cell_length_c                   13.0356(5)
_cell_measurement_reflns_used    54564
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.56
_cell_volume                     6783.5(4)
_computing_cell_refinement       'Peakref (Schreurs, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction
'Eval15 (Schreurs et al., 2010) and SADABS (Sheldrick, 2012)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'manual editing of the SHELXL output'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            75629
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         1.562
_exptl_absorpt_coefficient_mu    1.679
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             3042
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         10366
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0386P)²+1.8713P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                8945
_reflns_number_total             10366
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gz3264sup1.cif
_cod_data_source_block           Ib
_cod_depositor_comments
'Adding full bibliography for 2019519--2019522.cif.'
_cod_original_cell_volume        6783.5(5)
_cod_database_code               2019520
_cod_database_fobs_code          2019520
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2.013
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, 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_occupancy
N N1 0.4403(2) 0.2207(2) 0.5833(5) 0.0306(13) Uani d 1
C C11 0.3821(3) 0.1560(3) 0.5953(5) 0.0551(18) Uani d 1
H H11A 0.3784 0.1309 0.5345 0.066 Uiso calc 1
H H11B 0.3883 0.1352 0.6547 0.066 Uiso calc 1
C C21 0.3212(4) 0.1560(3) 0.6091(6) 0.065(3) Uani d 1
H H21A 0.3276 0.1893 0.6564 0.097 Uiso calc 1
H H21B 0.2895 0.1157 0.6365 0.097 Uiso calc 1
H H21C 0.3072 0.1631 0.5434 0.097 Uiso calc 1
C C31 0.4484(4) 0.2584(3) 0.6780(5) 0.0600(17) Uani d 1
H H31A 0.4526 0.2360 0.7369 0.072 Uiso calc 1
H H31B 0.4102 0.2611 0.6883 0.072 Uiso calc 1
C C41 0.5046(3) 0.3245(4) 0.6758(7) 0.068(2) Uani d 1
H H41A 0.5431 0.3225 0.6788 0.102 Uiso calc 1
H H41B 0.5027 0.3480 0.7343 0.102 Uiso calc 1
H H41C 0.5039 0.3453 0.6129 0.102 Uiso calc 1
C C51 0.4964(3) 0.2122(3) 0.5650(5) 0.0502(15) Uani d 1
H H51A 0.5335 0.2536 0.5521 0.060 Uiso calc 1
H H51B 0.4887 0.1867 0.5030 0.060 Uiso calc 1
C C61 0.5117(4) 0.1801(4) 0.6554(7) 0.079(3) Uani d 1
H H61A 0.5105 0.1994 0.7197 0.119 Uiso calc 1
H H61B 0.5533 0.1855 0.6457 0.119 Uiso calc 1
H H61C 0.4807 0.1356 0.6570 0.119 Uiso calc 1
C C71 0.4329(3) 0.2544(3) 0.4953(4) 0.0529(17) Uani d 1
H H71A 0.4717 0.2952 0.4875 0.063 Uiso calc 1
H H71B 0.3986 0.2627 0.5100 0.063 Uiso calc 1
C C81 0.4186(5) 0.2170(4) 0.3908(6) 0.068(2) Uani d 1
H H81A 0.4553 0.2146 0.3698 0.101 Uiso calc 1
H H81B 0.4084 0.2386 0.3384 0.101 Uiso calc 1
H H81C 0.3832 0.1747 0.4001 0.101 Uiso calc 1
N N2 0.2260(2) 0.10845(19) 0.0871(4) 0.0263(12) Uani d 1
C C12 0.2195(3) 0.1384(3) 0.1860(4) 0.0383(13) Uani d 1
H H12A 0.2171 0.1119 0.2439 0.046 Uiso calc 1
H H12B 0.2577 0.1795 0.1948 0.046 Uiso calc 1
C C22 0.1629(3) 0.1479(4) 0.1904(5) 0.058(2) Uani d 1
H H22A 0.1684 0.1801 0.1416 0.088 Uiso calc 1
H H22B 0.1590 0.1609 0.2590 0.088 Uiso calc 1
H H22C 0.1251 0.1086 0.1735 0.088 Uiso calc 1
C C32 0.2836(2) 0.1016(2) 0.0990(4) 0.0308(12) Uani d 1
H H32A 0.2851 0.0772 0.0406 0.037 Uiso calc 1
H H32B 0.2782 0.0767 0.1610 0.037 Uiso calc 1
C C42 0.3474(3) 0.1622(3) 0.1062(5) 0.0462(17) Uani d 1
H H42A 0.3521 0.1895 0.0491 0.069 Uiso calc 1
H H42B 0.3808 0.1519 0.1040 0.069 Uiso calc 1
H H42C 0.3498 0.1835 0.1702 0.069 Uiso calc 1
C C52 0.1688(3) 0.0441(3) 0.0678(5) 0.0374(13) Uani d 1
H H52A 0.1323 0.0496 0.0572 0.045 Uiso calc 1
H H52B 0.1757 0.0272 0.0041 0.045 Uiso calc 1
C C62 0.1532(3) -0.0035(4) 0.1507(4) 0.0465(15) Uani d 1
H H62A 0.1907 -0.0052 0.1690 0.070 Uiso calc 1
H H62B 0.1209 -0.0445 0.1265 0.070 Uiso calc 1
H H62C 0.1378 0.0083 0.2104 0.070 Uiso calc 1
C C72 0.2332(3) 0.1518(2) -0.0031(4) 0.0332(13) Uani d 1
H H72A 0.1942 0.1536 -0.0088 0.040 Uiso calc 1
H H72B 0.2672 0.1944 0.0132 0.040 Uiso calc 1
C C82 0.2465(3) 0.1341(3) -0.1035(5) 0.0443(16) Uani d 1
H H82A 0.2849 0.1319 -0.0994 0.066 Uiso calc 1
H H82B 0.2517 0.1653 -0.1542 0.066 Uiso calc 1
H H82C 0.2118 0.0933 -0.1234 0.066 Uiso calc 1
N N3 0.5579(2) 0.1076(2) 0.0842(4) 0.0273(12) Uani d 1
C C13 0.5644(3) 0.0495(3) 0.0986(5) 0.0533(18) Uani d 1
H H13A 0.5894 0.0548 0.1603 0.064 Uiso calc 1
H H13B 0.5871 0.0455 0.0398 0.064 Uiso calc 1
C C23 0.5005(4) -0.0111(4) 0.1086(5) 0.066(3) Uani d 1
H H23A 0.4752 -0.0051 0.1597 0.098 Uiso calc 1
H H23B 0.5070 -0.0454 0.1294 0.098 Uiso calc 1
H H23C 0.4789 -0.0210 0.0430 0.098 Uiso calc 1
C C33 0.5298(3) 0.1180(3) 0.1804(5) 0.0462(15) Uani d 1
H H33A 0.4894 0.0799 0.1942 0.055 Uiso calc 1
H H33B 0.5579 0.1240 0.2382 0.055 Uiso calc 1
C C43 0.5193(3) 0.1730(3) 0.1758(7) 0.058(2) Uani d 1
H H43A 0.5592 0.2117 0.1853 0.086 Uiso calc 1
H H43B 0.4903 0.1692 0.2295 0.086 Uiso calc 1
H H43C 0.5018 0.1738 0.1095 0.086 Uiso calc 1
C C53 0.6236(2) 0.1631(3) 0.0666(5) 0.0461(14) Uani d 1
H H53A 0.6403 0.1553 0.0034 0.055 Uiso calc 1
H H53B 0.6201 0.2007 0.0554 0.055 Uiso calc 1
C C63 0.6709(4) 0.1771(4) 0.1517(6) 0.067(3) Uani d 1
H H63A 0.6505 0.1716 0.2176 0.101 Uiso calc 1
H H63B 0.7053 0.2201 0.1453 0.101 Uiso calc 1
H H63C 0.6874 0.1485 0.1466 0.101 Uiso calc 1
C C73 0.5187(3) 0.1018(3) -0.0061(4) 0.0452(14) Uani d 1
H H73A 0.5179 0.1412 -0.0139 0.054 Uiso calc 1
H H73B 0.4754 0.0682 0.0071 0.054 Uiso calc 1
C C83 0.5414(4) 0.0874(6) -0.1086(6) 0.065(2) Uani d 1
H H83A 0.5829 0.1220 -0.1254 0.098 Uiso calc 1
H H83B 0.5121 0.0821 -0.1630 0.098 Uiso calc 1
H H83C 0.5433 0.0490 -0.1013 0.098 Uiso calc 1
Fe Fe1 0.33737(4) 0.00273(4) 0.33582(7) 0.0309(3) Uani d 1
Cl Cl11 0.34314(9) -0.00199(9) 0.16880(12) 0.0561(5) Uani d 1
Cl Cl21 0.28054(8) 0.04653(8) 0.37520(14) 0.0416(4) Uani d 1
Cl Cl31 0.29398(9) -0.09301(9) 0.39937(15) 0.0476(4) Uani d 1
Cl Cl41 0.43228(9) 0.06036(9) 0.39996(15) 0.0495(5) Uani d 1
Fe Fe2 0.33198(4) 0.00257(4) 0.83363(8) 0.0343(3) Uani d 1
Cl Cl12 0.31821(9) -0.00591(9) 0.66663(12) 0.0527(4) Uani d 1
Cl Cl22 0.23922(8) -0.03776(9) 0.90686(15) 0.0445(4) Uani d 1
Cl Cl32 0.37979(9) -0.04888(9) 0.87898(15) 0.0477(5) Uani d 1
Cl Cl42 0.38968(9) 0.10216(8) 0.87606(16) 0.0490(5) Uani d 1
Fe Fe3 0.6667 0.3333 0.35736(15) 0.0378(5) Uani d 1
Cl Cl13 0.6667 0.3333 0.1895(3) 0.0494(11) Uani d 1
Cl Cl23 0.62767(10) 0.23610(10) 0.41246(14) 0.0596(6) Uani d 1
Fe Fe4 0.0000 0.0000 0.86279(12) 0.0346(4) Uani d 1
Cl Cl14 0.0000 0.0000 0.6938(2) 0.0467(8) Uani d 1
Cl Cl24 0.06233(8) 0.09662(9) 0.91781(13) 0.0459(4) Uani d 1
Fe Fe5 0.6667 0.3333 0.85790(15) 0.0395(5) Uani d 1
Cl Cl15 0.6667 0.3333 0.6898(3) 0.0532(11) Uani d 1
Cl Cl25 0.56964(10) 0.27434(10) 0.91285(14) 0.0594(5) Uani d 1
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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_orient_matrix_type
_diffrn_orient_matrix_UB_11
_diffrn_orient_matrix_UB_12
_diffrn_orient_matrix_UB_13
_diffrn_orient_matrix_UB_21
_diffrn_orient_matrix_UB_22
_diffrn_orient_matrix_UB_23
_diffrn_orient_matrix_UB_31
_diffrn_orient_matrix_UB_32
_diffrn_orient_matrix_UB_33
'Nonius RMAT' -0.0007468 0.0364094 -0.0331586 -0.0437700 -0.0289410 -0.0250654
-0.0173985 0.0074731 0.0644811
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
C71 N1 C31 . . 108.2(4) ?
C71 N1 C51 . . 109.3(5) ?
C31 N1 C51 . . 111.6(5) ?
C71 N1 C11 . . 110.5(5) ?
C31 N1 C11 . . 108.9(5) ?
C51 N1 C11 . . 108.4(4) ?
C21 C11 N1 . . 115.2(5) ?
C21 C11 H11A . . 108.5 ?
N1 C11 H11A . . 108.5 ?
C21 C11 H11B . . 108.5 ?
N1 C11 H11B . . 108.5 ?
H11A C11 H11B . . 107.5 ?
C11 C21 H21A . . 109.5 ?
C11 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C11 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
N1 C31 C41 . . 114.5(6) ?
N1 C31 H31A . . 108.6 ?
C41 C31 H31A . . 108.6 ?
N1 C31 H31B . . 108.6 ?
C41 C31 H31B . . 108.6 ?
H31A C31 H31B . . 107.6 ?
C31 C41 H41A . . 109.5 ?
C31 C41 H41B . . 109.5 ?
H41A C41 H41B . . 109.5 ?
C31 C41 H41C . . 109.5 ?
H41A C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
N1 C51 C61 . . 114.5(6) ?
N1 C51 H51A . . 108.6 ?
C61 C51 H51A . . 108.6 ?
N1 C51 H51B . . 108.6 ?
C61 C51 H51B . . 108.6 ?
H51A C51 H51B . . 107.6 ?
C51 C61 H61A . . 109.5 ?
C51 C61 H61B . . 109.5 ?
H61A C61 H61B . . 109.5 ?
C51 C61 H61C . . 109.5 ?
H61A C61 H61C . . 109.5 ?
H61B C61 H61C . . 109.5 ?
N1 C71 C81 . . 113.5(5) ?
N1 C71 H71A . . 108.9 ?
C81 C71 H71A . . 108.9 ?
N1 C71 H71B . . 108.9 ?
C81 C71 H71B . . 108.9 ?
H71A C71 H71B . . 107.7 ?
C71 C81 H81A . . 109.5 ?
C71 C81 H81B . . 109.5 ?
H81A C81 H81B . . 109.5 ?
C71 C81 H81C . . 109.5 ?
H81A C81 H81C . . 109.5 ?
H81B C81 H81C . . 109.5 ?
C32 N2 C52 . . 109.3(4) ?
C32 N2 C12 . . 107.1(5) ?
C52 N2 C12 . . 112.0(5) ?
C32 N2 C72 . . 111.5(4) ?
C52 N2 C72 . . 108.6(4) ?
C12 N2 C72 . . 108.4(4) ?
C22 C12 N2 . . 115.3(5) ?
C22 C12 H12A . . 108.4 ?
N2 C12 H12A . . 108.4 ?
C22 C12 H12B . . 108.4 ?
N2 C12 H12B . . 108.4 ?
H12A C12 H12B . . 107.5 ?
C12 C22 H22A . . 109.5 ?
C12 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C12 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
N2 C32 C42 . . 117.3(5) ?
N2 C32 H32A . . 108.0 ?
C42 C32 H32A . . 108.0 ?
N2 C32 H32B . . 108.0 ?
C42 C32 H32B . . 108.0 ?
H32A C32 H32B . . 107.2 ?
C32 C42 H42A . . 109.5 ?
C32 C42 H42B . . 109.5 ?
H42A C42 H42B . . 109.5 ?
C32 C42 H42C . . 109.5 ?
H42A C42 H42C . . 109.5 ?
H42B C42 H42C . . 109.5 ?
C62 C52 N2 . . 115.8(5) ?
C62 C52 H52A . . 108.3 ?
N2 C52 H52A . . 108.3 ?
C62 C52 H52B . . 108.3 ?
N2 C52 H52B . . 108.3 ?
H52A C52 H52B . . 107.4 ?
C52 C62 H62A . . 109.5 ?
C52 C62 H62B . . 109.5 ?
H62A C62 H62B . . 109.5 ?
C52 C62 H62C . . 109.5 ?
H62A C62 H62C . . 109.5 ?
H62B C62 H62C . . 109.5 ?
C82 C72 N2 . . 116.3(4) ?
C82 C72 H72A . . 108.2 ?
N2 C72 H72A . . 108.2 ?
C82 C72 H72B . . 108.2 ?
N2 C72 H72B . . 108.2 ?
H72A C72 H72B . . 107.4 ?
C72 C82 H82A . . 109.5 ?
C72 C82 H82B . . 109.5 ?
H82A C82 H82B . . 109.5 ?
C72 C82 H82C . . 109.5 ?
H82A C82 H82C . . 109.5 ?
H82B C82 H82C . . 109.5 ?
C73 N3 C33 . . 110.3(4) ?
C73 N3 C53 . . 108.2(5) ?
C33 N3 C53 . . 110.1(5) ?
C73 N3 C13 . . 112.0(5) ?
C33 N3 C13 . . 109.0(5) ?
C53 N3 C13 . . 107.2(4) ?
N3 C13 C23 . . 112.5(5) ?
N3 C13 H13A . . 109.1 ?
C23 C13 H13A . . 109.1 ?
N3 C13 H13B . . 109.1 ?
C23 C13 H13B . . 109.1 ?
H13A C13 H13B . . 107.8 ?
C13 C23 H23A . . 109.5 ?
C13 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C13 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C43 C33 N3 . . 114.6(6) ?
C43 C33 H33A . . 108.6 ?
N3 C33 H33A . . 108.6 ?
C43 C33 H33B . . 108.6 ?
N3 C33 H33B . . 108.6 ?
H33A C33 H33B . . 107.6 ?
C33 C43 H43A . . 109.5 ?
C33 C43 H43B . . 109.5 ?
H43A C43 H43B . . 109.5 ?
C33 C43 H43C . . 109.5 ?
H43A C43 H43C . . 109.5 ?
H43B C43 H43C . . 109.5 ?
C63 C53 N3 . . 116.2(5) ?
C63 C53 H53A . . 108.2 ?
N3 C53 H53A . . 108.2 ?
C63 C53 H53B . . 108.2 ?
N3 C53 H53B . . 108.2 ?
H53A C53 H53B . . 107.4 ?
C53 C63 H63A . . 109.5 ?
C53 C63 H63B . . 109.5 ?
H63A C63 H63B . . 109.5 ?
C53 C63 H63C . . 109.5 ?
H63A C63 H63C . . 109.5 ?
H63B C63 H63C . . 109.5 ?
N3 C73 C83 . . 114.6(5) ?
N3 C73 H73A . . 108.6 ?
C83 C73 H73A . . 108.6 ?
N3 C73 H73B . . 108.6 ?
C83 C73 H73B . . 108.6 ?
H73A C73 H73B . . 107.6 ?
C73 C83 H83A . . 109.5 ?
C73 C83 H83B . . 109.5 ?
H83A C83 H83B . . 109.5 ?
C73 C83 H83C . . 109.5 ?
H83A C83 H83C . . 109.5 ?
H83B C83 H83C . . 109.5 ?
Cl11 Fe1 Cl41 . . 109.70(9) y
Cl11 Fe1 Cl31 . . 109.15(8) y
Cl41 Fe1 Cl31 . . 109.56(8) y
Cl11 Fe1 Cl21 . . 109.33(8) y
Cl41 Fe1 Cl21 . . 108.82(8) y
Cl31 Fe1 Cl21 . . 110.26(7) y
Cl32 Fe2 Cl22 . . 110.84(8) y
Cl32 Fe2 Cl42 . . 109.88(7) y
Cl22 Fe2 Cl42 . . 109.76(8) y
Cl32 Fe2 Cl12 . . 108.32(8) y
Cl22 Fe2 Cl12 . . 108.24(8) y
Cl42 Fe2 Cl12 . . 109.76(8) y
Cl13 Fe3 Cl23 . . 109.07(7) y
Cl13 Fe3 Cl23 . 3_655 109.07(7) ?
Cl23 Fe3 Cl23 . 3_655 109.87(7) y
Cl13 Fe3 Cl23 . 5_665 109.07(7) ?
Cl23 Fe3 Cl23 . 5_665 109.87(7) ?
Cl23 Fe3 Cl23 3_655 5_665 109.87(7) ?
Cl24 Fe4 Cl24 . 3 109.91(6) y
Cl24 Fe4 Cl24 . 5 109.91(6) ?
Cl24 Fe4 Cl24 3 5 109.91(6) ?
Cl24 Fe4 Cl14 . . 109.03(6) y
Cl24 Fe4 Cl14 3 . 109.03(6) ?
Cl24 Fe4 Cl14 5 . 109.03(6) ?
Cl15 Fe5 Cl25 . 3_655 109.04(8) ?
Cl15 Fe5 Cl25 . 5_665 109.04(8) ?
Cl25 Fe5 Cl25 3_655 5_665 109.90(7) ?
Cl15 Fe5 Cl25 . . 109.04(8) y
Cl25 Fe5 Cl25 3_655 . 109.90(7) y
Cl25 Fe5 Cl25 5_665 . 109.90(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
N1 C71 . 1.476(8) ?
N1 C31 . 1.494(8) ?
N1 C51 . 1.511(7) ?
N1 C11 . 1.521(7) ?
C11 C21 . 1.505(10) ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C21 H21A . 0.9700 ?
C21 H21B . 0.9700 ?
C21 H21C . 0.9700 ?
C31 C41 . 1.514(10) ?
C31 H31A . 0.9800 ?
C31 H31B . 0.9800 ?
C41 H41A . 0.9700 ?
C41 H41B . 0.9700 ?
C41 H41C . 0.9700 ?
C51 C61 . 1.562(10) ?
C51 H51A . 0.9800 ?
C51 H51B . 0.9800 ?
C61 H61A . 0.9700 ?
C61 H61B . 0.9700 ?
C61 H61C . 0.9700 ?
C71 C81 . 1.581(9) ?
C71 H71A . 0.9800 ?
C71 H71B . 0.9800 ?
C81 H81A . 0.9700 ?
C81 H81B . 0.9700 ?
C81 H81C . 0.9700 ?
N2 C32 . 1.511(6) ?
N2 C52 . 1.518(6) ?
N2 C12 . 1.531(7) ?
N2 C72 . 1.536(7) ?
C12 C22 . 1.519(9) ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C22 H22A . 0.9700 ?
C22 H22B . 0.9700 ?
C22 H22C . 0.9700 ?
C32 C42 . 1.528(8) ?
C32 H32A . 0.9800 ?
C32 H32B . 0.9800 ?
C42 H42A . 0.9700 ?
C42 H42B . 0.9700 ?
C42 H42C . 0.9700 ?
C52 C62 . 1.493(8) ?
C52 H52A . 0.9800 ?
C52 H52B . 0.9800 ?
C62 H62A . 0.9700 ?
C62 H62B . 0.9700 ?
C62 H62C . 0.9700 ?
C72 C82 . 1.467(8) ?
C72 H72A . 0.9800 ?
C72 H72B . 0.9800 ?
C82 H82A . 0.9700 ?
C82 H82B . 0.9700 ?
C82 H82C . 0.9700 ?
N3 C73 . 1.481(7) ?
N3 C33 . 1.512(7) ?
N3 C53 . 1.518(7) ?
N3 C13 . 1.523(7) ?
C13 C23 . 1.532(10) ?
C13 H13A . 0.9800 ?
C13 H13B . 0.9800 ?
C23 H23A . 0.9700 ?
C23 H23B . 0.9700 ?
C23 H23C . 0.9700 ?
C33 C43 . 1.495(9) ?
C33 H33A . 0.9800 ?
C33 H33B . 0.9800 ?
C43 H43A . 0.9700 ?
C43 H43B . 0.9700 ?
C43 H43C . 0.9700 ?
C53 C63 . 1.515(9) ?
C53 H53A . 0.9800 ?
C53 H53B . 0.9800 ?
C63 H63A . 0.9700 ?
C63 H63B . 0.9700 ?
C63 H63C . 0.9700 ?
C73 C83 . 1.555(9) ?
C73 H73A . 0.9800 ?
C73 H73B . 0.9800 ?
C83 H83A . 0.9700 ?
C83 H83B . 0.9700 ?
C83 H83C . 0.9700 ?
Fe1 Cl11 . 2.1886(17) y
Fe1 Cl41 . 2.196(2) y
Fe1 Cl31 . 2.198(2) y
Fe1 Cl21 . 2.2026(18) y
Fe2 Cl32 . 2.189(2) y
Fe2 Cl22 . 2.1933(18) y
Fe2 Cl42 . 2.1940(19) y
Fe2 Cl12 . 2.1968(19) y
Fe3 Cl13 . 2.188(4) y
Fe3 Cl23 . 2.198(2) y
Fe3 Cl23 3_655 2.198(2) ?
Fe3 Cl23 5_665 2.198(2) ?
Fe4 Cl24 . 2.1999(19) y
Fe4 Cl24 3 2.1999(19) ?
Fe4 Cl24 5 2.1999(19) ?
Fe4 Cl14 . 2.202(4) y
Fe5 Cl15 . 2.191(4) y
Fe5 Cl25 3_655 2.196(2) ?
Fe5 Cl25 5_665 2.196(2) ?
Fe5 Cl25 . 2.196(2) 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
C71 N1 C11 C21 -57.5(8)
C31 N1 C11 C21 61.2(8)
C51 N1 C11 C21 -177.2(6)
C71 N1 C31 C41 -59.3(8)
C51 N1 C31 C41 60.9(7)
C11 N1 C31 C41 -179.4(6)
C71 N1 C51 C61 176.9(6)
C31 N1 C51 C61 57.4(7)
C11 N1 C51 C61 -62.6(8)
C31 N1 C71 C81 -175.4(7)
C51 N1 C71 C81 62.9(8)
C11 N1 C71 C81 -56.3(8)
C32 N2 C12 C22 -178.5(5)
C52 N2 C12 C22 -58.7(7)
C72 N2 C12 C22 61.1(6)
C52 N2 C32 C42 172.9(5)
C12 N2 C32 C42 -65.6(6)
C72 N2 C32 C42 52.8(7)
C32 N2 C52 C62 60.7(7)
C12 N2 C52 C62 -57.9(7)
C72 N2 C52 C62 -177.5(5)
C32 N2 C72 C82 56.3(6)
C52 N2 C72 C82 -64.2(6)
C12 N2 C72 C82 174.0(5)
C73 N3 C13 C23 -56.9(7)
C33 N3 C13 C23 65.5(6)
C53 N3 C13 C23 -175.4(5)
C73 N3 C33 C43 -55.2(7)
C53 N3 C33 C43 64.1(6)
C13 N3 C33 C43 -178.5(6)
C73 N3 C53 C63 179.5(6)
C33 N3 C53 C63 58.9(7)
C13 N3 C53 C63 -59.5(7)
C33 N3 C73 C83 -176.9(7)
C53 N3 C73 C83 62.7(8)
C13 N3 C73 C83 -55.3(8)
