# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
_journal_year ?
_journal_volume ?
_journal_page_first ?
_publ_contact_author_address # Address of author for correspondence
;
Crystal Structure Center, Chemical Physics,
Zernike Institute for Advanced Materials,
University of Groningen,
Nijenborgh 4,
NL-9747 AG Groningen, The Netherlands.
;
_publ_contact_author_email A.Meetsma@rug.nl
_publ_contact_author_fax '+31 50 3634441'
_publ_contact_author_phone '+31 50 3634368'
#===============================================================================
# 1. SUBMISSION DETAILS
_publ_contact_author_name # Name of author for correspondence
;
Drs. A. Meetsma
;
_publ_contact_letter # Include date of submission
;
Dat of submission : 2010-03-09 12:02:46
Consider this CIF submission for deposition of the
X-ray structure of a manuscript to be submitted to : Dalton
(Our Compound_Identification_Code : q1539)
;
# Publication choise FI, CI or EI for Inorganic
# FM, CM or EM for Metal-organic
# FO, CO or EO for Organic
_publ_requested_category ?
_publ_requested_coeditor_name ?
loop_
_publ_author_name
'Pijper, Dirk'
'Saisaha, Pattama'
'Alsters, Paul'
'Boer, Johannes'
'Hoen, Rob'
'Smit, Christian'
'Meetsma, Auke'
'Hage, Ronald'
'van Summeren, Ruben'
'Feringa, Ben'
'Browne, Wesley'
data_q1539
_database_code_depnum_ccdc_archive 'CCDC 768839'
#TrackingRef 'q1539.cif'
#==============================================================================
# 0. AUDIT DETAILS
_audit_creation_date '2010-03-09 11:02:46'
_audit_creation_method
;
PLATON
option (version :: 200110)
SHELXL97-2 & Manual Editing
;
_audit_update_record
;
?
2010-03-09 # Formatted by publCIF
;
#===============================================================================
_publ_section_exptl_refinement
;
Refinement was frustrated by a disorder problem: from the solution, it was
clear that the positions of one of the perchlorate anions was highly
disordered. The smeared electron density for O5 and O6 has been described by
two site occupancy factors with separately refined displacement parameters.
The s.o.f. of the major fraction of the component of the disorder model
refined to a value of 0.593(6). The atoms of the disordered anion showed
unrealistic displacement parameters when allowed to vary anisotropically,
suggesting dynamic disorder (dynamic means that the smeared electron density
is due to fluctuations of the atomic positions within each unit cell; the
disorder is compensated by the large displacement parameters).
The hydrogen atoms were generated by geometrical considerations, constrained to
idealized geometries, and allowed to ride on the carrier atom with an
isotropic displacement parameter related to the equivalent displacement
parameter of their carrier atoms, with U~iso~(H) = 1.2U~eq~(C)
or 1.5U~eq~(methyl C). The methyl-groups were refined as rigid groups,
which were allowed to rotate freely. Assigned values of bond distances for
secondary C---H~2~ = 0.99 \%A, methyl C---H~3~ = 0.98 \%A, aromatic C---H =
0.95 \%A and N---H = 0.93
;
_publ_section_related_literature
;
;
# Insert blank lines between references
_publ_section_references
;
Beurskens, P. T., Beurskens, G., de Gelder, R., Smits, J. M. M.,
Garc\'ia-Granda, S. & Gould, R. O. (2008). The DIRDIF08 program system,
Technical Report of the Crystallography Laboratory, University of Nijmegen,
The Netherlands.
Bruker, (2007). SMART (Version 5.632), SAINT-Plus (Version
7.46a) and SADABS (Version 2.10). Bruker AXS Inc., Madison, Wisconsin,
USA.
Meetsma, A. (2010). Extended version of the program PLUTO. University of
Groningen, The Netherlands. (unpublished).
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
Spek, A. L. (2003). J. Appl. Cryst. 36, 7--13.
;
_publ_section_figure_captions
;
Fig. 1. Perspective PLUTO drawings of the molecule illustrating the
configuration and the adopted numbering scheme.
Fig. 2. Molecular packing viewed down unit cell axes.
Fig. 3. Perspective ORTEP drawing of the title compound. Displacement
ellipsoids for non-H atoms are represented at the 50% probability level. The
H-atoms have been omitted to improve clarity.
;
_publ_section_acknowledgements
;
?
;
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C22 H28 Fe N5 O2, 0.5(C2 H3 N), 2(Cl O4)'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural ?
_chemical_formula_sum 'C23 H29.5 Cl2 Fe N5.5 O10'
_chemical_formula_iupac ?
_chemical_formula_weight 669.77
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Fe Fe 0.3463 0.8444 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_Int_Tables_number 15
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z
_cell_length_a 37.597(4)
_cell_length_b 9.1237(10)
_cell_length_c 16.3513(18)
_cell_angle_alpha 90
_cell_angle_beta 102.216(1)
_cell_angle_gamma 90
_cell_volume 5481.9(10)
_cell_formula_units_Z 8
_cell_measurement_temperature 100(1)
_cell_measurement_reflns_used 7754
_cell_measurement_theta_min 2.55
_cell_measurement_theta_max 29.17
_cell_special_details
;
The final unit cell was obtained from the xyz centroids of
7754 reflections after integration using the SAINTPLUS
software package (Bruker, 2007).
Reduced cell calculations did not indicate any higher metric lattice symmetry
and examination of the final atomic coordinates of the structure did not
yield extra symmetry elements (Spek, 1988; Le Page 1987, 1988)
;
_exptl_crystal_description platelet
_exptl_crystal_colour red
_exptl_crystal_size_max 0.44
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.17
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.623
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2768
_exptl_absorpt_coefficient_mu 0.812
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details '(SADABS, (Bruker, 2007))'
_exptl_absorpt_correction_T_min 0.6703
_exptl_absorpt_correction_T_max 0.8714
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
;
;
_diffrn_ambient_temperature 100(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine focus sealed Siemens Mo tube '
_diffrn_radiation_monochromator 'parallel mounted graphite'
_diffrn_radiation_detector
;
CCD area-detector
;
_diffrn_measurement_device_type
;
Bruker Smart Apex; CCD area detector
;
_diffrn_measurement_method '\f and \w scans'
_diffrn_special_details
;
Crystal into the cold nitrogen stream of the low-temparature unit
(KRYOFLEX, (Bruker, 2007)).
;
_diffrn_detector_area_resol_mean 66.06
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time .
_diffrn_standards_decay_% 0
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
# number of measured reflections (redundant set)
_diffrn_reflns_number 21142
_diffrn_reflns_av_R_equivalents 0.0328
_diffrn_reflns_av_sigmaI/netI 0.0322
_diffrn_reflns_limit_h_min -45
_diffrn_reflns_limit_h_max 46
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.55
_diffrn_reflns_theta_max 26.37
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_reduction_process
;
Intensity data were corrected for Lorentz and polarization
effects, decay and absorption and reduced to F~o~^2^
using SAINT-Plus & SADABS (Bruker, 2007).
;
# number of unique reflections
_reflns_number_total 5616
_reflns_number_gt 4780
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART (Bruker, 2007)'
_computing_cell_refinement 'SAINT-Plus (Bruker, 2007)'
_computing_data_reduction 'SAINT-Plus (Bruker, 2007)'
_computing_structure_solution
;
DIRDIF-08 (Beurskens et al., 2008)
;
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics
;
PLATON (Spek, 2003)
PLUTO (Meetsma, 2010)
;
_computing_publication_material 'PLATON (Spek, 2003)'
#===============================================================================
# 8. REFINEMENT DATA
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+10.23P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary direct
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details ?
_chemical_absolute_configuration .
_refine_ls_abs_structure_Flack ?
_refine_ls_number_reflns 5616
_refine_ls_number_parameters 397
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.0527
_refine_ls_R_factor_gt 0.0444
_refine_ls_wR_factor_ref 0.1118
_refine_ls_wR_factor_gt 0.1071
_refine_ls_goodness_of_fit_ref 1.058
_refine_ls_restrained_S_all 1.058
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.925
_refine_diff_density_min -0.489
_refine_diff_density_rms 0.083
_vrn_publ_code_number_frames 1800
_vrn_publ_code_frame_time_sec 10.0
_vrn_publ_code_meas_time_hour 7.8
#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe Uani 0.13041(1) 0.19943(4) 0.46519(2) 1.0 0.0192(1) . .
O1 O Uani 0.10032(4) 0.11840(19) 0.52803(11) 1.0 0.0250(5) . .
O2 O Uani 0.04471(6) 0.0412(2) 0.44658(13) 1.0 0.0383(6) . .
N1 N Uani 0.16507(5) 0.3069(2) 0.40815(13) 1.0 0.0196(6) . .
N2 N Uani 0.14764(5) 0.3478(2) 0.55609(13) 1.0 0.0216(6) . .
N3 N Uani 0.16771(6) 0.0457(2) 0.50684(13) 1.0 0.0233(6) . .
N4 N Uani 0.11681(6) 0.0578(2) 0.37295(13) 1.0 0.0232(6) . .
N5 N Uani 0.08808(5) 0.3280(2) 0.42049(13) 1.0 0.0214(6) . .
C1 C Uani 0.17650(7) 0.2664(3) 0.33831(16) 1.0 0.0229(7) . .
C2 C Uani 0.19894(7) 0.3529(3) 0.30173(16) 1.0 0.0261(8) . .
C3 C Uani 0.21076(7) 0.4863(3) 0.33852(16) 1.0 0.0252(8) . .
C4 C Uani 0.20028(6) 0.5271(3) 0.41129(16) 1.0 0.0235(7) . .
C5 C Uani 0.17756(6) 0.4360(3) 0.44467(15) 1.0 0.0216(7) . .
C6 C Uani 0.16402(7) 0.4760(3) 0.52160(17) 1.0 0.0269(8) . .
C7 C Uani 0.17019(7) 0.2940(3) 0.63742(16) 1.0 0.0294(8) . .
C8 C Uani 0.20071(7) 0.1922(3) 0.62691(17) 1.0 0.0295(8) . .
C9 C Uani 0.18644(7) 0.0414(3) 0.59690(17) 1.0 0.0302(8) . .
C10 C Uani 0.15056(7) -0.0979(3) 0.47973(18) 1.0 0.0283(8) . .
C11 C Uani 0.12829(7) -0.0803(3) 0.39263(17) 1.0 0.0265(8) . .
C12 C Uani 0.12014(7) -0.1931(3) 0.3350(2) 1.0 0.0343(9) . .
C13 C Uani 0.10033(8) -0.1641(3) 0.2555(2) 1.0 0.0367(9) . .
C14 C Uani 0.08959(7) -0.0205(3) 0.23423(18) 1.0 0.0338(9) . .
C15 C Uani 0.09796(7) 0.0869(3) 0.29466(17) 1.0 0.0282(8) . .
C16 C Uani 0.08544(7) 0.4436(3) 0.36793(16) 1.0 0.0248(8) . .
C17 C Uani 0.05359(7) 0.5228(3) 0.34362(18) 1.0 0.0314(8) . .
C18 C Uani 0.02332(7) 0.4825(3) 0.37414(18) 1.0 0.0320(8) . .
C19 C Uani 0.02564(7) 0.3630(3) 0.42690(18) 1.0 0.0310(8) . .
C20 C Uani 0.05834(7) 0.2873(3) 0.44845(17) 1.0 0.0254(8) . .
C21 C Uani 0.06353(7) 0.1500(3) 0.50029(19) 1.0 0.0304(8) . .
C22 C Uani 0.04296(10) -0.0961(3) 0.4887(2) 1.0 0.0499(11) . .
N7 N Uani 0.000 0.8142(5) 0.25000 1.000 0.086(2) . .
C23 C Uani 0.000 0.9399(5) 0.25000 1.000 0.0511(18) . .
C24 C Uani 0.000 1.0993(5) 0.25000 1.000 0.0387(12) . .
Cl1 Cl Uani 0.08839(2) 0.40624(10) 0.13549(5) 1.0 0.0504(3) . .
O3 O Uani 0.06026(5) 0.3238(2) 0.15909(13) 1.0 0.0368(7) . .
O4 O Uani 0.08841(8) 0.4048(4) 0.05213(17) 1.0 0.0892(13) . .
O5A O Uani 0.06998(17) 0.5636(4) 0.1281(3) 0.593(6) 0.078(2) . .
O6A O Uani 0.11740(18) 0.4176(11) 0.1961(5) 0.593(6) 0.101(3) . .
O5B O Uani 0.1108(3) 0.4985(8) 0.1940(6) 0.407(6) 0.054(3) . .
O6B O Uani 0.11926(14) 0.2749(6) 0.1403(4) 0.407(6) 0.049(2) . .
Cl2 Cl Uani 0.26521(2) 0.43644(7) 0.13258(4) 1.0 0.0259(2) . .
O7 O Uani 0.26464(5) 0.5270(2) 0.05931(12) 1.0 0.0331(6) . .
O8 O Uani 0.25443(6) 0.5236(2) 0.19628(13) 1.0 0.0406(7) . .
O9 O Uani 0.24024(6) 0.3159(2) 0.11052(15) 1.0 0.0441(7) . .
O10 O Uani 0.30145(5) 0.3815(2) 0.16266(13) 1.0 0.0395(7) . .
H1 H Uiso 0.16876 0.17457 0.31343 1.0 0.0275 . .
H2 H Uiso 0.20617 0.32164 0.25225 1.0 0.0314 . .
H3 H Uiso 0.22584 0.54865 0.31399 1.0 0.0303 . .
H4 H Uiso 0.20859 0.61678 0.43817 1.0 0.0282 . .
H6 H Uiso 0.18450 0.51433 0.56459 1.0 0.0322 . .
H6' H Uiso 0.14558 0.55466 0.50776 1.0 0.0322 . .
H7 H Uiso 0.15416 0.24189 0.66868 1.0 0.0352 . .
H7' H Uiso 0.18074 0.37942 0.67135 1.0 0.0352 . .
H8 H Uiso 0.21825 0.18250 0.68108 1.0 0.0354 . .
H8' H Uiso 0.21376 0.23505 0.586 1.000 0.0354 . .
H9 H Uiso 0.20695 -0.02882 0.60453 1.0 0.0362 . .
H9' H Uiso 0.16919 0.00714 0.63088 1.0 0.0362 . .
H10 H Uiso 0.13484 -0.12904 0.51807 1.0 0.0339 . .
H10' H Uiso 0.16954 -0.17342 0.48057 1.0 0.0339 . .
H12 H Uiso 0.12815 -0.28999 0.35016 1.0 0.0410 . .
H13 H Uiso 0.09412 -0.24097 0.21581 1.0 0.0440 . .
H14 H Uiso 0.07676 0.00296 0.17928 1.0 0.0405 . .
H15 H Uiso 0.09023 0.18458 0.28077 1.0 0.0338 . .
H16 H Uiso 0.10616 0.47152 0.34696 1.0 0.0298 . .
H17 H Uiso 0.05247 0.60362 0.30653 1.0 0.0377 . .
H18 H Uiso 0.00128 0.53630 0.35901 1.0 0.0384 . .
H19 H Uiso 0.00515 0.33298 0.44814 1.0 0.0371 . .
H21 H Uiso 0.05193 0.16235 0.54954 1.0 0.0365 . .
H22 H Uiso 0.06757 -0.13599 0.50687 1.0 0.0747 . .
H23' H Uiso 0.02797 -0.16531 0.45029 1.0 0.0747 . .
H31 H Uiso 0.12648 0.38381 0.56965 1.0 0.0259 . .
H32 H Uiso 0.18595 0.05843 0.47694 1.0 0.0280 . .
H222 H Uiso 0.03216 -0.08061 0.53751 1.0 0.0747 . .
H24 H Uiso -0.01852 1.13511 0.27920 0.5 0.0578 . .
H24' H Uiso -0.00546 1.13511 0.19219 0.5 0.0578 . .
H24" H Uiso 0.02399 1.13511 0.27862 0.5 0.0578 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0167(2) 0.0190(2) 0.0218(2) 0.0019(1) 0.0036(1) -0.0003(1)
O1 0.0175(8) 0.0277(9) 0.0296(10) 0.0074(7) 0.0044(7) 0.0005(7)
O2 0.0362(11) 0.0329(10) 0.0434(12) 0.0043(9) 0.0029(9) -0.0059(9)
N1 0.0166(10) 0.0204(9) 0.0213(10) 0.0026(8) 0.0028(8) 0.0015(8)
N2 0.0175(10) 0.0242(10) 0.0232(11) 0.0000(8) 0.0049(8) -0.0002(8)
N3 0.0206(10) 0.0236(10) 0.0258(11) 0.0054(9) 0.0053(9) 0.0010(8)
N4 0.0197(10) 0.0210(10) 0.0293(12) -0.0006(9) 0.0058(9) -0.0017(8)
N5 0.0181(10) 0.0213(10) 0.0235(11) -0.0007(8) 0.0012(8) -0.0010(8)
C1 0.0222(12) 0.0224(12) 0.0238(13) 0.0004(10) 0.0041(10) 0.0022(10)
C2 0.0228(13) 0.0341(14) 0.0223(13) 0.0024(11) 0.0065(10) 0.0039(10)
C3 0.0185(12) 0.0296(13) 0.0277(14) 0.0097(10) 0.0051(10) -0.0001(10)
C4 0.0172(12) 0.0236(12) 0.0285(14) 0.0023(10) 0.0019(10) -0.0005(9)
C5 0.0183(12) 0.0225(11) 0.0230(13) 0.0029(10) 0.0021(10) 0.0024(9)
C6 0.0265(13) 0.0267(12) 0.0288(14) -0.0048(10) 0.0089(11) -0.0066(10)
C7 0.0256(13) 0.0410(15) 0.0204(13) 0.0014(11) 0.0023(11) 0.0036(11)
C8 0.0224(13) 0.0394(15) 0.0246(14) 0.0043(11) 0.0005(11) 0.0024(11)
C9 0.0259(14) 0.0347(14) 0.0289(14) 0.0113(11) 0.0034(11) 0.0055(11)
C10 0.0257(14) 0.0195(12) 0.0411(16) 0.0047(11) 0.0105(12) 0.0034(10)
C11 0.0195(12) 0.0234(12) 0.0394(16) 0.0006(11) 0.0127(11) -0.0024(10)
C12 0.0250(14) 0.0219(13) 0.058(2) -0.0065(12) 0.0136(13) -0.0033(10)
C13 0.0255(14) 0.0360(15) 0.0506(19) -0.0181(13) 0.0129(13) -0.0074(12)
C14 0.0262(14) 0.0406(15) 0.0334(16) -0.0093(12) 0.0038(12) -0.0048(12)
C15 0.0252(13) 0.0290(13) 0.0298(14) -0.0013(11) 0.0043(11) -0.0020(10)
C16 0.0234(13) 0.0223(12) 0.0270(14) 0.0020(10) 0.0013(10) -0.0019(10)
C17 0.0293(14) 0.0230(12) 0.0386(16) 0.0052(11) -0.0001(12) 0.0004(11)
C18 0.0226(13) 0.0285(13) 0.0399(16) 0.0007(12) -0.0047(12) 0.0045(11)
C19 0.0188(12) 0.0308(14) 0.0419(16) 0.0019(12) 0.0032(12) -0.0015(11)
C20 0.0184(12) 0.0278(13) 0.0283(14) -0.0005(10) 0.0009(10) -0.0023(10)
C21 0.0178(12) 0.0329(14) 0.0398(16) 0.0070(12) 0.0045(11) -0.0021(11)
C22 0.0469(19) 0.0342(16) 0.063(2) 0.0122(15) -0.0012(17) -0.0119(14)
N7 0.047(3) 0.037(2) 0.158(6) 0.00 -0.015(3) 0.0000
C23 0.025(2) 0.045(3) 0.075(4) 0.00 -0.008(2) 0.0000
C24 0.034(2) 0.039(2) 0.039(2) 0.00 -0.0014(19) 0.0000
Cl1 0.0587(5) 0.0629(5) 0.0315(4) -0.0026(3) 0.0136(4) -0.0389(4)
O3 0.0247(10) 0.0405(11) 0.0468(13) 0.0135(9) 0.0114(9) -0.0018(8)
O4 0.070(2) 0.150(3) 0.0457(16) 0.0248(18) 0.0083(14) -0.049(2)
O5A 0.137(5) 0.0208(19) 0.065(3) 0.0051(19) -0.001(3) -0.016(2)
O6A 0.045(3) 0.173(9) 0.068(4) 0.063(6) -0.027(3) -0.059(5)
O5B 0.069(6) 0.045(4) 0.058(5) -0.022(4) 0.034(4) -0.031(4)
O6B 0.026(3) 0.050(4) 0.077(5) -0.019(3) 0.025(3) 0.003(2)
Cl2 0.0202(3) 0.0292(3) 0.0296(3) 0.0031(2) 0.0080(3) 0.0031(2)
O7 0.0289(10) 0.0449(11) 0.0257(10) 0.0045(8) 0.0063(8) -0.0052(9)
O8 0.0523(13) 0.0403(11) 0.0361(12) 0.0066(9) 0.0250(10) 0.0124(10)
O9 0.0339(12) 0.0331(11) 0.0624(15) 0.0053(10) 0.0038(10) -0.0047(9)
O10 0.0234(10) 0.0501(12) 0.0446(12) 0.0046(10) 0.0063(9) 0.0122(9)
#===============================================================================
# 10. MOLECULAR GEOMETRY
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All su's are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.8369(17) . . yes
Fe1 N1 2.011(2) . . yes
Fe1 N2 2.013(2) . . yes
Fe1 N3 1.998(2) . . yes
Fe1 N4 1.970(2) . . yes
Fe1 N5 1.988(2) . . yes
Cl1 O5B 1.412(9) . . yes
Cl1 O6B 1.659(6) . . yes
Cl1 O5A 1.587(4) . . yes
Cl1 O3 1.416(2) . . yes
Cl1 O4 1.363(3) . . yes
Cl1 O6A 1.313(8) . . yes
Cl2 O7 1.452(2) . . yes
Cl2 O8 1.435(2) . . yes
Cl2 O9 1.441(2) . . yes
Cl2 O10 1.437(2) . . yes
O1 C21 1.392(3) . . yes
O2 C21 1.412(3) . . yes
O2 C22 1.438(3) . . yes
N1 C1 1.354(3) . . yes
N1 C5 1.359(3) . . yes
N2 C6 1.487(3) . . yes
N2 C7 1.500(3) . . yes
N3 C9 1.492(3) . . yes
N3 C10 1.486(3) . . yes
N4 C11 1.349(3) . . yes
N4 C15 1.352(3) . . yes
N5 C16 1.351(3) . . yes
N5 C20 1.347(3) . . yes
N2 H31 0.93 . . no
N3 H32 0.93 . . no
N7 C23 1.147(6) . . yes
C1 C2 1.381(4) . . no
C2 C3 1.388(4) . . no
C3 C4 1.381(4) . . no
C4 C5 1.384(4) . . no
C5 C6 1.499(4) . . no
C7 C8 1.514(4) . . no
C8 C9 1.520(4) . . no
C10 C11 1.500(4) . . no
C11 C12 1.385(4) . . no
C12 C13 1.380(4) . . no
C13 C14 1.393(4) . . no
C14 C15 1.380(4) . . no
C16 C17 1.383(4) . . no
C17 C18 1.386(4) . . no
C18 C19 1.382(4) . . no
C19 C20 1.389(4) . . no
C20 C21 1.502(4) . . no
C1 H1 0.95 . . no
C2 H2 0.95 . . no
C3 H3 0.95 . . no
C4 H4 0.95 . . no
C6 H6 0.99 . . no
C6 H6' 0.99 . . no
C7 H7 0.99 . . no
C7 H7' 0.99 . . no
C8 H8' 0.99 . . no
C8 H8 0.99 . . no
C9 H9 0.99 . . no
C9 H9' 0.99 . . no
C10 H10' 0.99 . . no
C10 H10 0.99 . . no
C12 H12 0.95 . . no
C13 H13 0.95 . . no
C14 H14 0.95 . . no
C15 H15 0.95 . . no
C16 H16 0.95 . . no
C17 H17 0.95 . . no
C18 H18 0.95 . . no
C19 H19 0.95 . . no
C21 H21 1.00 . . no
C22 H222 0.98 . . no
C22 H22 0.98 . . no
C22 H23' 0.98 . . no
C23 C24 1.454(6) . . no
C24 H24" 0.98 . . no
C24 H24' 0.98 . . no
C24 H24" 0.98 . 2_555 no
C24 H24 0.98 . 2_555 no
C24 H24' 0.98 . 2_555 no
C24 H24 0.98 . . no
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 N1 172.72(8) . . . yes
O1 Fe1 N2 89.87(8) . . . yes
O1 Fe1 N3 89.87(8) . . . yes
O1 Fe1 N4 94.21(8) . . . yes
O1 Fe1 N5 84.45(8) . . . yes
N1 Fe1 N2 82.86(8) . . . yes
N1 Fe1 N3 91.34(8) . . . yes
N1 Fe1 N4 93.06(9) . . . yes
N1 Fe1 N5 95.09(8) . . . yes
N2 Fe1 N3 97.32(8) . . . yes
N2 Fe1 N4 175.71(9) . . . yes
N2 Fe1 N5 88.98(8) . . . yes
N3 Fe1 N4 81.39(8) . . . yes
N3 Fe1 N5 171.52(8) . . . yes
N4 Fe1 N5 92.73(9) . . . yes
O5B Cl1 O6B 95.0(4) . . . yes
O3 Cl1 O5B 120.3(4) . . . yes
O3 Cl1 O6B 99.1(2) . . . yes
O4 Cl1 O5A 91.4(2) . . . yes
O4 Cl1 O6A 125.4(4) . . . yes
O3 Cl1 O4 115.20(17) . . . yes
O3 Cl1 O5A 99.3(2) . . . yes
O3 Cl1 O6A 112.7(4) . . . yes
O5A Cl1 O6A 105.4(5) . . . yes
O4 Cl1 O5B 123.8(4) . . . yes
O4 Cl1 O6B 83.8(3) . . . yes
O7 Cl2 O8 109.05(11) . . . yes
O7 Cl2 O9 109.43(13) . . . yes
O7 Cl2 O10 109.16(12) . . . yes
O8 Cl2 O9 109.59(13) . . . yes
O9 Cl2 O10 109.85(12) . . . yes
O8 Cl2 O10 109.74(13) . . . yes
Fe1 O1 C21 114.94(16) . . . yes
C21 O2 C22 112.5(2) . . . yes
C1 N1 C5 117.7(2) . . . yes
Fe1 N1 C1 127.64(17) . . . yes
Fe1 N1 C5 114.62(16) . . . yes
C6 N2 C7 113.06(19) . . . yes
Fe1 N2 C6 110.07(16) . . . yes
Fe1 N2 C7 117.88(15) . . . yes
C9 N3 C10 110.83(19) . . . yes
Fe1 N3 C9 120.35(16) . . . yes
Fe1 N3 C10 106.75(16) . . . yes
Fe1 N4 C11 114.34(17) . . . yes
Fe1 N4 C15 126.54(17) . . . yes
C11 N4 C15 119.1(2) . . . yes
Fe1 N5 C16 129.80(17) . . . yes
Fe1 N5 C20 111.73(16) . . . yes
C16 N5 C20 118.5(2) . . . yes
C7 N2 H31 105 . . . no
C6 N2 H31 105 . . . no
Fe1 N2 H31 105 . . . no
Fe1 N3 H32 106 . . . no
C10 N3 H32 106 . . . no
C9 N3 H32 106 . . . no
N1 C1 C2 122.8(2) . . . yes
C1 C2 C3 118.8(2) . . . no
C2 C3 C4 119.1(2) . . . no
C3 C4 C5 119.4(2) . . . no
N1 C5 C4 122.1(2) . . . yes
C4 C5 C6 122.2(2) . . . no
N1 C5 C6 115.7(2) . . . yes
N2 C6 C5 111.6(2) . . . yes
N2 C7 C8 113.6(2) . . . yes
C7 C8 C9 111.6(2) . . . no
N3 C9 C8 110.8(2) . . . yes
N3 C10 C11 108.0(2) . . . yes
N4 C11 C12 121.2(2) . . . yes
C10 C11 C12 124.4(3) . . . no
N4 C11 C10 114.4(2) . . . yes
C11 C12 C13 119.7(3) . . . no
C12 C13 C14 119.1(3) . . . no
C13 C14 C15 118.6(3) . . . no
N4 C15 C14 122.2(2) . . . yes
N5 C16 C17 122.2(2) . . . yes
C16 C17 C18 119.0(3) . . . no
C17 C18 C19 119.1(3) . . . no
C18 C19 C20 119.1(3) . . . no
N5 C20 C21 113.8(2) . . . yes
C19 C20 C21 124.1(2) . . . no
N5 C20 C19 122.1(2) . . . yes
O2 C21 C20 104.3(2) . . . yes
O1 C21 C20 111.0(2) . . . yes
O1 C21 O2 112.9(2) . . . yes
N1 C1 H1 119 . . . no
C2 C1 H1 119 . . . no
C1 C2 H2 121 . . . no
C3 C2 H2 121 . . . no
C4 C3 H3 120 . . . no
C2 C3 H3 120 . . . no
C3 C4 H4 120 . . . no
C5 C4 H4 120 . . . no
N2 C6 H6' 109 . . . no
N2 C6 H6 109 . . . no
H6 C6 H6' 108 . . . no
C5 C6 H6 109 . . . no
C5 C6 H6' 109 . . . no
N2 C7 H7 109 . . . no
C8 C7 H7' 109 . . . no
N2 C7 H7' 109 . . . no
C8 C7 H7 109 . . . no
H7 C7 H7' 108 . . . no
C7 C8 H8 109 . . . no
C7 C8 H8' 109 . . . no
C9 C8 H8 109 . . . no
C9 C8 H8' 109 . . . no
H8 C8 H8' 108 . . . no
N3 C9 H9 109 . . . no
N3 C9 H9' 110 . . . no
C8 C9 H9 109 . . . no
C8 C9 H9' 109 . . . no
H9 C9 H9' 108 . . . no
N3 C10 H10 110 . . . no
N3 C10 H10' 110 . . . no
C11 C10 H10 110 . . . no
C11 C10 H10' 110 . . . no
H10 C10 H10' 108 . . . no
C11 C12 H12 120 . . . no
C13 C12 H12 120 . . . no
C12 C13 H13 120 . . . no
C14 C13 H13 120 . . . no
C15 C14 H14 121 . . . no
C13 C14 H14 121 . . . no
N4 C15 H15 119 . . . no
C14 C15 H15 119 . . . no
N5 C16 H16 119 . . . no
C17 C16 H16 119 . . . no
C18 C17 H17 120 . . . no
C16 C17 H17 121 . . . no
C17 C18 H18 120 . . . no
C19 C18 H18 120 . . . no
C20 C19 H19 120 . . . no
C18 C19 H19 120 . . . no
O2 C21 H21 109 . . . no
C20 C21 H21 109 . . . no
O1 C21 H21 109 . . . no
O2 C22 H22 109 . . . no
O2 C22 H23' 109 . . . no
H22 C22 H23' 109 . . . no
H22 C22 H222 110 . . . no
O2 C22 H222 109 . . . no
H23' C22 H222 109 . . . no
N7 C23 C24 180.00(1) . . . yes
H24' C24 H24" 56 2_555 . . no
H24" C24 H24" 141 . . 2_555 no
H24 C24 H24" 109 2_555 . 2_555 no
H24' C24 H24" 109 2_555 . 2_555 no
H24 C24 H24' 109 2_555 . 2_555 no
H24 C24 H24" 109 . . . no
H24 C24 H24 141 . . 2_555 no
H24 C24 H24' 56 . . 2_555 no
H24 C24 H24" 56 . . 2_555 no
H24' C24 H24" 109 . . . no
H24 C24 H24' 56 2_555 . . no
H24' C24 H24' 141 . . 2_555 no
H24' C24 H24" 56 . . 2_555 no
H24 C24 H24" 56 2_555 . . no
C23 C24 H24 109 . . . no
C23 C24 H24' 109 . . . no
C23 C24 H24" 109 . . . no
C23 C24 H24 109 . . 2_555 no
C23 C24 H24' 109 . . 2_555 no
C23 C24 H24" 109 . . 2_555 no
H24 C24 H24' 109 . . . no
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Fe1 O1 C21 105.65(17) . . . . no
N3 Fe1 O1 C21 -157.03(18) . . . . no
N4 Fe1 O1 C21 -75.68(18) . . . . no
N5 Fe1 O1 C21 16.67(17) . . . . no
N2 Fe1 N1 C1 169.3(2) . . . . no
N2 Fe1 N1 C5 -11.84(17) . . . . no
N3 Fe1 N1 C1 72.1(2) . . . . no
N3 Fe1 N1 C5 -109.05(17) . . . . no
N4 Fe1 N1 C1 -9.4(2) . . . . no
N4 Fe1 N1 C5 169.51(17) . . . . no
N5 Fe1 N1 C1 -102.4(2) . . . . no
N5 Fe1 N1 C5 76.49(17) . . . . no
O1 Fe1 N2 C6 -160.03(16) . . . . no
O1 Fe1 N2 C7 68.29(17) . . . . no
N1 Fe1 N2 C6 19.68(15) . . . . no
N1 Fe1 N2 C7 -112.00(17) . . . . no
N3 Fe1 N2 C6 110.12(16) . . . . no
N3 Fe1 N2 C7 -21.56(18) . . . . no
N5 Fe1 N2 C6 -75.58(16) . . . . no
N5 Fe1 N2 C7 152.74(17) . . . . no
O1 Fe1 N3 C9 -66.54(19) . . . . no
O1 Fe1 N3 C10 60.80(16) . . . . no
N1 Fe1 N3 C9 106.28(19) . . . . no
N1 Fe1 N3 C10 -126.37(16) . . . . no
N2 Fe1 N3 C9 23.31(19) . . . . no
N2 Fe1 N3 C10 150.65(16) . . . . no
N4 Fe1 N3 C9 -160.8(2) . . . . no
N4 Fe1 N3 C10 -33.48(16) . . . . no
O1 Fe1 N4 C11 -68.31(19) . . . . no
O1 Fe1 N4 C15 112.3(2) . . . . no
N1 Fe1 N4 C11 111.82(19) . . . . no
N1 Fe1 N4 C15 -67.6(2) . . . . no
N3 Fe1 N4 C11 20.92(19) . . . . no
N3 Fe1 N4 C15 -158.5(2) . . . . no
N5 Fe1 N4 C11 -152.93(19) . . . . no
N5 Fe1 N4 C15 27.6(2) . . . . no
O1 Fe1 N5 C16 174.4(2) . . . . no
O1 Fe1 N5 C20 -6.33(17) . . . . no
N1 Fe1 N5 C16 1.7(2) . . . . no
N1 Fe1 N5 C20 -179.04(18) . . . . no
N2 Fe1 N5 C16 84.4(2) . . . . no
N2 Fe1 N5 C20 -96.30(18) . . . . no
N4 Fe1 N5 C16 -91.7(2) . . . . no
N4 Fe1 N5 C20 87.64(18) . . . . no
Fe1 O1 C21 O2 94.0(2) . . . . no
Fe1 O1 C21 C20 -22.8(3) . . . . no
C22 O2 C21 O1 66.3(3) . . . . no
C22 O2 C21 C20 -173.1(2) . . . . no
Fe1 N1 C1 C2 176.36(19) . . . . no
C5 N1 C1 C2 -2.5(4) . . . . no
Fe1 N1 C5 C4 -176.95(19) . . . . no
Fe1 N1 C5 C6 0.8(3) . . . . no
C1 N1 C5 C4 2.0(4) . . . . no
C1 N1 C5 C6 179.8(2) . . . . no
Fe1 N2 C6 C5 -24.2(2) . . . . no
C7 N2 C6 C5 109.9(2) . . . . no
Fe1 N2 C7 C8 47.3(3) . . . . no
C6 N2 C7 C8 -83.1(3) . . . . no
Fe1 N3 C9 C8 -48.9(3) . . . . no
C10 N3 C9 C8 -174.3(2) . . . . no
Fe1 N3 C10 C11 40.0(2) . . . . no
C9 N3 C10 C11 172.7(2) . . . . no
Fe1 N4 C11 C10 -2.5(3) . . . . no
Fe1 N4 C11 C12 178.5(2) . . . . no
C15 N4 C11 C10 177.0(2) . . . . no
C15 N4 C11 C12 -2.0(4) . . . . no
Fe1 N4 C15 C14 -179.7(2) . . . . no
C11 N4 C15 C14 0.9(4) . . . . no
Fe1 N5 C16 C17 -179.3(2) . . . . no
C20 N5 C16 C17 1.5(4) . . . . no
Fe1 N5 C20 C19 178.6(2) . . . . no
Fe1 N5 C20 C21 -4.4(3) . . . . no
C16 N5 C20 C19 -2.0(4) . . . . no
C16 N5 C20 C21 175.0(2) . . . . no
N1 C1 C2 C3 0.9(4) . . . . no
C1 C2 C3 C4 1.2(4) . . . . no
C2 C3 C4 C5 -1.6(4) . . . . no
C3 C4 C5 N1 0.0(4) . . . . no
C3 C4 C5 C6 -177.7(2) . . . . no
N1 C5 C6 N2 15.7(3) . . . . no
C4 C5 C6 N2 -166.5(2) . . . . no
N2 C7 C8 C9 -74.2(3) . . . . no
C7 C8 C9 N3 73.6(3) . . . . no
N3 C10 C11 N4 -25.3(3) . . . . no
N3 C10 C11 C12 153.6(3) . . . . no
N4 C11 C12 C13 0.9(4) . . . . no
C10 C11 C12 C13 -178.0(3) . . . . no
C11 C12 C13 C14 1.4(4) . . . . no
C12 C13 C14 C15 -2.5(4) . . . . no
C13 C14 C15 N4 1.4(4) . . . . no
N5 C16 C17 C18 0.0(4) . . . . no
C16 C17 C18 C19 -1.0(4) . . . . no
C17 C18 C19 C20 0.5(4) . . . . no
C18 C19 C20 N5 1.0(4) . . . . no
C18 C19 C20 C21 -175.6(3) . . . . no
N5 C20 C21 O1 17.2(3) . . . . no
N5 C20 C21 O2 -104.8(3) . . . . no
C19 C20 C21 O1 -166.0(3) . . . . no
C19 C20 C21 O2 72.1(3) . . . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Fe1 H8' 3.35 . . no
Cl1 H31 2.74 . 4_564 no
Cl1 H15 3.11 . . no
Cl2 H32 3.03 . 6_555 no
Cl2 H6 3.04 . 4_564 no
O1 N2 2.722(3) . . no
O1 C9 3.271(3) . . no
O1 C10 2.953(3) . . no
O1 N3 2.711(3) . . no
O1 C20 2.385(3) . . no
O1 N5 2.573(3) . . no
O1 C11 3.206(3) . . no
O1 C7 3.268(3) . . no
O1 N4 2.790(3) . . no
O2 N5 3.160(3) . . no
O2 C24 3.340(2) . 1_545 no
O2 C24 3.340(2) . 2_545 no
O2 N4 3.194(3) . . no
O3 C15 3.204(3) . . no
O3 C18 3.398(3) . 2_555 no
O3 C19 3.258(3) . 2_555 no
O4 C20 3.352(4) . 4_564 no
O4 C6 3.180(4) . 4_564 no
O4 C22 3.343(5) . 4_554 no
O4 N2 3.162(4) . 4_564 no
O4 N5 3.250(4) . 4_564 no
O4 C16 3.295(4) . 4_564 no
O5A C13 3.288(5) . 1_565 no
O5A C20 3.182(5) . 4_564 no
O5A C21 3.323(5) . 4_564 no
O5B C7 3.209(10) . 4_564 no
O5B C13 3.288(8) . 1_565 no
O5B N2 3.208(10) . 4_564 no
O5B C16 3.224(10) . . no
O6A C16 3.290(8) . . no
O6A C1 3.172(9) . . no
O6A C2 3.239(8) . . no
O6B C14 3.405(6) . . no
O6B C15 3.288(7) . . no
O7 N3 2.972(3) . 6_555 no
O7 C4 3.079(3) . 4_564 no
O7 C1 3.302(3) . 6_555 no
O8 C3 3.136(3) . . no
O8 C2 3.358(3) . . no
O8 C8 3.335(3) . 4_564 no
O10 C11 2.988(3) . 6_555 no
O10 C12 3.018(3) . 6_555 no
O10 C10 3.239(3) . 6_555 no
O1 H31 2.65 . . no
O1 H22 2.62 . . no
O1 H10 2.63 . . no
O2 H24" 2.82 . 1_545 no
O2 H24' 2.58 . 2_545 no
O3 H19 2.70 . 2_555 no
O3 H15 2.43 . . no
O3 H24 2.67 . 2_545 no
O4 H6' 2.44 . 4_564 no
O4 H22 2.63 . 4_554 no
O4 H31 2.38 . 4_564 no
O5A H18 2.74 . 2_555 no
O5A H31 2.55 . 4_564 no
O5A H13 2.35 . 1_565 no
O5A H21 2.83 . 4_564 no
O5B H16 2.56 . . no
O5B H13 2.50 . 1_565 no
O5B H31 2.48 . 4_564 no
O6A H15 2.84 . . no
O6A H16 2.64 . . no
O6A H31 2.82 . 4_564 no
O6B H22 2.89 . 4_554 no
O6B H15 2.86 . . no
O6B H10 2.57 . 4_554 no
O7 H4 2.88 . 4_564 no
O7 H32 2.09 . 6_555 no
O8 H7' 2.85 . 4_564 no
O8 H3 2.41 . . no
O8 H2 2.87 . . no
O8 H8 2.78 . 7_556 no
O9 H2 2.88 . . no
O9 H4 2.88 . 4_564 no
O9 H6 2.59 . 4_564 no
O9 H9 2.90 . 4_554 no
O9 H3 2.90 . 6_545 no
O9 H4 2.88 . 6_545 no
O10 H10' 2.83 . 6_555 no
O10 H32 2.92 . 6_555 no
O10 H8 2.87 . 7_556 no
O10 H1 2.89 . 6_555 no
O10 H4 2.90 . 6_545 no
N1 C15 3.443(3) . . no
N1 N5 2.950(3) . . no
N1 C6 2.420(3) . . no
N1 N2 2.663(3) . . no
N1 N3 2.868(3) . . no
N1 N4 2.889(3) . . no
N1 C16 3.181(3) . . no
N2 N3 3.012(3) . . no
N2 N5 2.804(3) . . no
N2 N1 2.663(3) . . no
N2 O5B 3.208(10) . 4_565 no
N2 O1 2.722(3) . . no
N2 C5 2.470(3) . . no
N2 C9 3.159(3) . . no
N2 O4 3.162(4) . 4_565 no
N3 O7 2.972(3) . 6_545 no
N3 N2 3.012(3) . . no
N3 C7 3.101(3) . . no
N3 C11 2.415(3) . . no
N3 N1 2.868(3) . . no
N3 N4 2.587(3) . . no
N3 O1 2.711(3) . . no
N4 O2 3.194(3) . . no
N4 O1 2.790(3) . . no
N4 C20 3.448(3) . . no
N4 N5 2.864(3) . . no
N4 N1 2.889(3) . . no
N4 N3 2.587(3) . . no
N4 C1 3.085(3) . . no
N4 C10 2.396(3) . . no
N4 C21 3.290(4) . . no
N5 C6 3.273(3) . . no
N5 C5 3.447(3) . . no
N5 N4 2.864(3) . . no
N5 O2 3.160(3) . . no
N5 C15 3.088(3) . . no
N5 C21 2.388(3) . . no
N5 O1 2.573(3) . . no
N5 N1 2.950(3) . . no
N5 O4 3.250(4) . 4_565 no
N5 N2 2.804(3) . . no
N1 H32 2.58 . . no
N1 H16 2.69 . . no
N4 H1 2.59 . . no
N4 H32 2.79 . . no
N5 H15 2.65 . . no
N5 H31 2.61 . . no
N7 H17 2.77 . . no
N7 H17 2.77 . 2_555 no
C1 C15 3.320(4) . . no
C1 O6A 3.172(9) . . no
C1 O7 3.302(3) . 6_545 no
C2 O8 3.358(3) . . no
C2 O6A 3.239(8) . . no
C3 O8 3.136(3) . . no
C4 O7 3.079(3) . 4_565 no
C5 C16 3.426(4) . . no
C6 O4 3.180(4) . 4_565 no
C6 C16 3.462(4) . . no
C7 O5B 3.209(10) . 4_565 no
C8 O8 3.335(3) . 4_565 no
C10 O10 3.239(3) . 6_545 no
C11 O10 2.988(3) . 6_545 no
C12 O10 3.018(3) . 6_545 no
C13 O5B 3.288(8) . 1_545 no
C13 O5A 3.288(5) . 1_545 no
C14 C23 3.451(3) . 2_545 no
C14 O6B 3.405(6) . . no
C14 C23 3.451(3) . 1_545 no
C15 C16 3.534(4) . . no
C15 O6B 3.288(7) . . no
C15 C1 3.320(4) . . no
C15 O3 3.204(3) . . no
C16 O6A 3.290(8) . . no
C16 C5 3.426(4) . . no
C16 O5B 3.224(10) . . no
C16 C15 3.534(4) . . no
C16 C6 3.462(4) . . no
C16 O4 3.295(4) . 4_565 no
C18 O3 3.398(3) . 2_555 no
C19 O3 3.258(3) . 2_555 no
C20 O4 3.352(4) . 4_565 no
C20 O5A 3.182(5) . 4_565 no
C21 O5A 3.323(5) . 4_565 no
C22 O4 3.343(5) . 4_555 no
C23 C14 3.451(3) . 2_565 no
C23 C14 3.451(3) . 1_565 no
C24 O2 3.340(2) . 1_565 no
C24 O2 3.340(2) . 2_565 no
C1 H32 2.92 . . no
C2 H8 3.08 . 7_556 no
C3 H9 3.06 . 7_556 no
C3 H7' 2.99 . 4_564 no
C5 H16 2.84 . . no
C5 H8' 3.04 . . no
C6 H8' 2.93 . . no
C13 H7 2.80 . 4_554 no
C13 H17 3.01 . 1_545 no
C14 H24 2.99 . 2_545 no
C14 H24" 3.06 . 1_545 no
C15 H1 2.73 . . no
C15 H24 3.01 . 2_545 no
C15 H24" 2.77 . 1_545 no
C16 H6' 3.03 . . no
C16 H12 2.96 . 1_565 no
C16 H15 2.79 . . no
C19 H24' 2.84 . 2_545 no
C20 H31 3.02 . . no
C20 H24' 3.04 . 2_545 no
H1 N4 2.59 . . no
H1 O10 2.89 . 6_545 no
H1 C15 2.73 . . no
H2 O8 2.87 . . no
H2 O9 2.88 . . no
H3 O9 2.90 . 6_555 no
H3 O8 2.41 . . no
H4 O9 2.88 . 6_555 no
H4 O10 2.90 . 6_555 no
H4 H6 2.60 . . no
H4 H10' 2.59 . 1_565 no
H4 O7 2.88 . 4_565 no
H4 O9 2.88 . 4_565 no
H6 Cl2 3.04 . 4_565 no
H6 O9 2.59 . 4_565 no
H6 H7' 2.16 . . no
H6 H4 2.60 . . no
H6' O4 2.44 . 4_565 no
H6' C16 3.03 . . no
H7 H9' 2.33 . . no
H7 H13 2.53 . 4_555 no
H7 C13 2.80 . 4_555 no
H7' C3 2.99 . 4_565 no
H7' O8 2.85 . 4_565 no
H7' H6 2.16 . . no
H8 O10 2.87 . 7_556 no
H8 C2 3.08 . 7_556 no
H8 O8 2.78 . 7_556 no
H8' C6 2.93 . . no
H8' H32 2.47 . . no
H8' C5 3.04 . . no
H8' Fe1 3.35 . . no
H9 H10' 2.57 . . no
H9 C3 3.06 . 7_556 no
H9 O9 2.90 . 4_555 no
H9' H7 2.33 . . no
H9' H10 2.37 . . no
H10 O1 2.63 . . no
H10 O6B 2.57 . 4_555 no
H10 H22 2.50 . . no
H10 H9' 2.37 . . no
H10' H9 2.57 . . no
H10' H12 2.59 . . no
H10' O10 2.83 . 6_545 no
H10' H4 2.59 . 1_545 no
H12 C16 2.96 . 1_545 no
H12 H16 2.32 . 1_545 no
H12 H10' 2.59 . . no
H13 O5B 2.50 . 1_545 no
H13 O5A 2.35 . 1_545 no
H13 H7 2.53 . 4_554 no
H15 O3 2.43 . . no
H15 Cl1 3.11 . . no
H15 C16 2.79 . . no
H15 O6A 2.84 . . no
H15 N5 2.65 . . no
H15 H24" 2.52 . 1_545 no
H15 O6B 2.86 . . no
H16 O5B 2.56 . . no
H16 H12 2.32 . 1_565 no
H16 C5 2.84 . . no
H16 O6A 2.64 . . no
H16 N1 2.69 . . no
H17 C13 3.01 . 1_565 no
H17 N7 2.77 . . no
H17 N7 2.77 . . no
H18 O5A 2.74 . 2_555 no
H19 O3 2.70 . 2_555 no
H21 H222 2.33 . . no
H21 O5A 2.83 . 4_565 no
H22 O1 2.62 . . no
H22 O6B 2.89 . 4_555 no
H22 H10 2.50 . . no
H22 O4 2.63 . 4_555 no
H24 C14 2.99 . 2_565 no
H24 O3 2.67 . 2_565 no
H24 C15 3.01 . 2_565 no
H24' O2 2.58 . 2_565 no
H24' C19 2.84 . 2_565 no
H24' C20 3.04 . 2_565 no
H24" C14 3.06 . 1_565 no
H24" H15 2.52 . 1_565 no
H24" C15 2.77 . 1_565 no
H24" O2 2.82 . 1_565 no
H31 O6A 2.82 . 4_565 no
H31 C20 3.02 . . no
H31 Cl1 2.74 . 4_565 no
H31 O4 2.38 . 4_565 no
H31 O5B 2.48 . 4_565 no
H31 O5A 2.55 . 4_565 no
H32 H8' 2.47 . . no
H32 Cl2 3.03 . 6_545 no
H32 C1 2.92 . . no
H32 O10 2.92 . 6_545 no
H32 O7 2.09 . 6_545 no
H222 H21 2.33 . . no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
#
#D H A D - H H...A D...A D - H...A symm(A)
#
N2 H31 O4 0.9300 2.3800 3.162(4) 141 4_565 yes
N2 H31 O5A 0.9300 2.5500 3.467(6) 168 4_565 yes
N3 H32 O7 0.9300 2.0900 2.972(3) 159 6_545 yes
C1 H1 N4 0.9500 2.5900 3.085(3) 113 . yes
C3 H3 O8 0.9500 2.4100 3.136(3) 134 . yes
C6 H6 O9 0.9900 2.5900 3.488(4) 151 4_565 yes
C6 H6' O4 0.9900 2.4400 3.180(4) 131 4_565 yes
C13 H13 O5A 0.9500 2.3500 3.288(5) 170 1_545 yes
C15 H15 O3 0.9500 2.4300 3.204(3) 139 . yes
C24 H24' O2 0.9800 2.5800 3.340(2) 135 2_565 yes
#===END of Crystallographic Information File