# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2006
data_global
_journal_name_full Chem.Commun.
_journal_coden_Cambridge 0182
_audit_creation_method
;
manual editing of the CIF file
created by SHELXTL Ver. 6.10
and processed with modiCIfer-09152005.
;
_publ_contact_author_name 'Robert W. McGaff'
_publ_contact_author_address
;
Chemistry
University of Wisconsin-La Crosse
4021 Cowley Hall
1725 State Street
La Crosse
Wisconsin
54601
UNITED STATES OF AMERICA
;
_publ_contact_author_email MCGAFF.ROBE@UWLAX.EDU
_publ_section_title
;
Chiral iron(III) and cobalt(III) complexes containing
a new pentadentate "helmet" phthalocyaninato ligand
;
loop_
_publ_author_name
'Robert W. McGaff'
'Matthew J. Bierman'
'Ilia Guzei'
'Heidi M. Kieler'
'Peter J. Liska'
data_mcg014
_database_code_depnum_ccdc_archive 'CCDC 606957'
_publ_section_references
;
Allen, F.H. (2002). Acta Cryst. B58, 380-388.
Bruker-AXS. (2003). SADABS (Version 2.05), SAINT
(Version 6.22),
SHELXTL (Version 6.10), and SMART
(Version 5.622). Bruker-AXS
Inc., Madison, WI, USA.
Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M.,
Macrae, C. F., McCabe, P., Pearson, J,
& Taylor, R. (2002). Acta Cryst. B58, 389-397.
Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc.
97, 1358-1367.
Frisch, M. J., Trucks, G. W.,
Schlegel, H. B., Scuseria, G. E., Robb, M. A., Cheeseman,
J. R., Montgomery, Jr., J. A., Vreven, T., Kudin, K. N., Burant,
J. C., Millam, J. M., Iyengar, S. S., Tomasi, J., Barone, V.,
Mennucci, B. et al. (2004).
Gaussian 03, Revision C.02,
Gaussian, Inc., Wallingford, CT, USA.
;
_publ_section_acknowledgements
;
We thank the National Science Foundation for financial support.
The manuscript was prepared with the beta test version 1.0.0.
of program publCIF to be released by the IUCr and Ilia A. Guzei's
program modiCIFer to be released by University of Wisconsin-Madison.
;
_publ_section_figure_captions
;
Figure 1. Molecular structure of (I). The thermal ellipsoids are
shown at 50% probability level.
;
_publ_section_exptl_prep
;
;
_publ_section_exptl_refinement
;
All H-atoms were placed in idealized locations and
refined as riding with appropriate thermal displacement
coefficients U~iso~(H) = 1.2 or 1.5 times U~eq~(bearing atom).
Default effective X-H distances for T = -173.0 C
AFIX m = C1 C2 C3 C4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16
d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95
;
#3. data
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C43 H32 Co N11 O3'
_chemical_formula_sum 'C43 H32 Co N11 O3'
_chemical_formula_weight 809.73
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 1 21/n 1 '
_symmetry_space_group_name_Hall '-P 2yn '
_symmetry_int_tables_number 14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.9142(7)
_cell_length_b 13.6308(7)
_cell_length_c 18.7876(9)
_cell_angle_alpha 90.00
_cell_angle_beta 109.9950(10)
_cell_angle_gamma 90.00
_cell_volume 3589.2(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 11459
_cell_measurement_theta_min 2.1421
_cell_measurement_theta_max 26.3721
_exptl_crystal_description block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.38
_exptl_crystal_size_mid 0.34
_exptl_crystal_size_min 0.29
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.498
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1672
_exptl_absorpt_coefficient_mu 0.539
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker-AXS, 2003)
;
_exptl_absorpt_correction_T_min 0.8213
_exptl_absorpt_correction_T_max 0.8593
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type Mo-K\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker CCD-1000 area detector'
_diffrn_measurement_method '0.30\% \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 29092
_diffrn_reflns_av_R_equivalents 0.0291
_diffrn_reflns_av_sigmaI/netI 0.0249
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 2.08
_diffrn_reflns_theta_max 26.39
_reflns_number_total 7332
_reflns_number_gt 6283
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_cell_refinement 'SAINT Ver. 6.22 (Bruker-AXS, 2003)'
_computing_data_reduction 'SAINT Ver. 6.22'
_computing_structure_solution 'SHELXTL Ver. 6.10 (Bruker-AXS, 2003)'
_computing_structure_refinement 'SHELXTL Ver. 6.10'
_computing_molecular_graphics 'SHELXTL Ver. 6.10'
_computing_publication_material 'SHELXTL Ver. 6.10'
_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^)+(0.0595P)^2^+2.9298P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7332
_refine_ls_number_parameters 531
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0465
_refine_ls_R_factor_gt 0.0384
_refine_ls_wR_factor_ref 0.1077
_refine_ls_wR_factor_gt 0.1019
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_restrained_S_all 1.028
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.541501(18) 0.455900(19) 0.760028(14) 0.01603(9) Uani 1 1 d . . .
N1 N 0.58238(12) 0.45652(12) 0.67481(9) 0.0194(3) Uani 1 1 d . . .
N2 N 0.44439(12) 0.38079(13) 0.58347(9) 0.0218(4) Uani 1 1 d . . .
N3 N 0.41738(12) 0.43397(12) 0.69621(9) 0.0188(3) Uani 1 1 d . . .
N4 N 0.33179(12) 0.43619(12) 0.78751(9) 0.0199(3) Uani 1 1 d . . .
N5 N 0.50338(11) 0.44331(12) 0.84606(9) 0.0175(3) Uani 1 1 d . . .
N6 N 0.65895(12) 0.43613(12) 0.94337(9) 0.0200(4) Uani 1 1 d . . .
N7 N 0.66318(11) 0.49100(12) 0.82350(9) 0.0172(3) Uani 1 1 d . . .
N8 N 0.74315(12) 0.52027(12) 0.73069(9) 0.0199(3) Uani 1 1 d . . .
N9 N 0.34219(11) 0.58322(13) 0.72069(9) 0.0192(3) Uani 1 1 d . . .
N10 N 0.51337(11) 0.58906(12) 0.75052(9) 0.0172(3) Uani 1 1 d . . .
N11 N 0.67090(11) 0.65443(12) 0.77274(9) 0.0182(3) Uani 1 1 d . . .
O1 O 0.57204(10) 0.31280(10) 0.76509(8) 0.0213(3) Uani 1 1 d . . .
H1O H 0.6306 0.3035 0.7743 0.032 Uiso 1 1 calc R . .
O2 O 0.74885(11) 0.77807(12) 0.69815(9) 0.0300(3) Uani 1 1 d . . .
H2O H 0.7307 0.7422 0.7270 0.045 Uiso 1 1 calc R . .
O3 O 0.17504(12) 0.64884(16) 0.74599(12) 0.0492(5) Uani 1 1 d . . .
H3O H 0.2231 0.6363 0.7339 0.074 Uiso 1 1 calc R . .
C1 C 0.67629(14) 0.47653(15) 0.67822(11) 0.0202(4) Uani 1 1 d . . .
C2 C 0.68657(15) 0.43799(15) 0.60762(11) 0.0217(4) Uani 1 1 d . . .
C3 C 0.76359(16) 0.43753(16) 0.58258(12) 0.0252(4) Uani 1 1 d . . .
H3 H 0.8236 0.4642 0.6123 0.030 Uiso 1 1 calc R . .
C4 C 0.74905(17) 0.39595(17) 0.51155(13) 0.0298(5) Uani 1 1 d . . .
H4 H 0.8005 0.3935 0.4927 0.036 Uiso 1 1 calc R . .
C5 C 0.66099(18) 0.35818(17) 0.46801(12) 0.0300(5) Uani 1 1 d . . .
H5 H 0.6535 0.3303 0.4200 0.036 Uiso 1 1 calc R . .
C6 C 0.58344(17) 0.36025(16) 0.49307(12) 0.0265(5) Uani 1 1 d . . .
H6 H 0.5228 0.3357 0.4628 0.032 Uiso 1 1 calc R . .
C7 C 0.59841(15) 0.39969(15) 0.56409(11) 0.0223(4) Uani 1 1 d . . .
C8 C 0.53438(15) 0.41101(15) 0.60877(11) 0.0204(4) Uani 1 1 d . . .
C9 C 0.38894(14) 0.40395(14) 0.62567(11) 0.0199(4) Uani 1 1 d . . .
C10 C 0.28382(15) 0.40238(15) 0.59475(12) 0.0220(4) Uani 1 1 d . . .
C11 C 0.22094(16) 0.36808(16) 0.52629(12) 0.0269(5) Uani 1 1 d . . .
H11 H 0.2433 0.3388 0.4896 0.032 Uiso 1 1 calc R . .
C12 C 0.12409(16) 0.37823(17) 0.51357(13) 0.0310(5) Uani 1 1 d . . .
H12 H 0.0792 0.3540 0.4678 0.037 Uiso 1 1 calc R . .
C13 C 0.09169(16) 0.42305(17) 0.56644(13) 0.0293(5) Uani 1 1 d . . .
H13 H 0.0250 0.4296 0.5560 0.035 Uiso 1 1 calc R . .
C14 C 0.15522(15) 0.45878(16) 0.63468(12) 0.0250(4) Uani 1 1 d . . .
H14 H 0.1330 0.4908 0.6704 0.030 Uiso 1 1 calc R . .
C15 C 0.25163(14) 0.44586(15) 0.64844(11) 0.0212(4) Uani 1 1 d . . .
C16 C 0.33796(13) 0.47477(15) 0.71658(11) 0.0194(4) Uani 1 1 d . . .
C17 C 0.40983(14) 0.42494(14) 0.84351(11) 0.0188(4) Uani 1 1 d . . .
C18 C 0.41523(14) 0.38773(14) 0.91901(11) 0.0200(4) Uani 1 1 d . . .
C19 C 0.34592(15) 0.35836(15) 0.94812(12) 0.0227(4) Uani 1 1 d . . .
H19 H 0.2801 0.3613 0.9184 0.027 Uiso 1 1 calc R . .
C20 C 0.37620(16) 0.32420(16) 1.02262(12) 0.0252(4) Uani 1 1 d . . .
H20 H 0.3301 0.3030 1.0439 0.030 Uiso 1 1 calc R . .
C21 C 0.47255(16) 0.32057(16) 1.06634(12) 0.0254(4) Uani 1 1 d . . .
H21 H 0.4913 0.2957 1.1166 0.030 Uiso 1 1 calc R . .
C22 C 0.54212(15) 0.35287(15) 1.03754(11) 0.0226(4) Uani 1 1 d . . .
H22 H 0.6079 0.3522 1.0676 0.027 Uiso 1 1 calc R . .
C23 C 0.51153(14) 0.38584(14) 0.96348(11) 0.0193(4) Uani 1 1 d . . .
C24 C 0.56550(14) 0.42327(14) 0.91644(11) 0.0181(4) Uani 1 1 d . . .
C25 C 0.69953(13) 0.48167(14) 0.89720(11) 0.0186(4) Uani 1 1 d . . .
C26 C 0.79285(14) 0.53093(15) 0.92599(11) 0.0201(4) Uani 1 1 d . . .
C27 C 0.85759(15) 0.54032(16) 0.99924(12) 0.0243(4) Uani 1 1 d . . .
H27 H 0.8468 0.5101 1.0412 0.029 Uiso 1 1 calc R . .
C28 C 0.93904(15) 0.59608(17) 1.00831(12) 0.0273(5) Uani 1 1 d . . .
H28 H 0.9851 0.6037 1.0575 0.033 Uiso 1 1 calc R . .
C29 C 0.95431(15) 0.64067(16) 0.94705(13) 0.0268(5) Uani 1 1 d . . .
H29 H 1.0109 0.6777 0.9550 0.032 Uiso 1 1 calc R . .
C30 C 0.88792(14) 0.63208(15) 0.87391(12) 0.0229(4) Uani 1 1 d . . .
H30 H 0.8978 0.6635 0.8321 0.028 Uiso 1 1 calc R . .
C31 C 0.80743(14) 0.57629(15) 0.86459(11) 0.0198(4) Uani 1 1 d . . .
C32 C 0.71959(14) 0.55894(14) 0.79470(11) 0.0186(4) Uani 1 1 d . . .
C33 C 0.42283(14) 0.62767(15) 0.73375(11) 0.0189(4) Uani 1 1 d . . .
C34 C 0.43197(14) 0.73559(15) 0.72896(10) 0.0186(4) Uani 1 1 d . . .
C35 C 0.36420(15) 0.80963(15) 0.71437(11) 0.0219(4) Uani 1 1 d . . .
H35 H 0.2996 0.7958 0.7083 0.026 Uiso 1 1 calc R . .
C36 C 0.39477(15) 0.90484(16) 0.70902(12) 0.0245(4) Uani 1 1 d . . .
H36 H 0.3498 0.9569 0.6979 0.029 Uiso 1 1 calc R . .
C37 C 0.49000(16) 0.92551(16) 0.71958(12) 0.0249(4) Uani 1 1 d . . .
H37 H 0.5087 0.9914 0.7158 0.030 Uiso 1 1 calc R . .
C38 C 0.55833(15) 0.85130(15) 0.73561(11) 0.0215(4) Uani 1 1 d . . .
H38 H 0.6234 0.8653 0.7436 0.026 Uiso 1 1 calc R . .
C39 C 0.52740(14) 0.75625(15) 0.73949(11) 0.0188(4) Uani 1 1 d . . .
C40 C 0.57922(14) 0.66122(14) 0.75570(10) 0.0175(4) Uani 1 1 d . . .
C41 C 0.53548(19) 0.23841(18) 0.80216(15) 0.0367(6) Uani 1 1 d . . .
H41A H 0.5631 0.2471 0.8572 0.055 Uiso 1 1 calc R . .
H41B H 0.5526 0.1735 0.7884 0.055 Uiso 1 1 calc R . .
H41C H 0.4659 0.2440 0.7861 0.055 Uiso 1 1 calc R . .
C42 C 0.69138(18) 0.75974(19) 0.62166(13) 0.0358(5) Uani 1 1 d . . .
H42A H 0.6272 0.7862 0.6121 0.054 Uiso 1 1 calc R . .
H42B H 0.6873 0.6889 0.6123 0.054 Uiso 1 1 calc R . .
H42C H 0.7200 0.7915 0.5878 0.054 Uiso 1 1 calc R . .
C43 C 0.2039(2) 0.6672(2) 0.82396(18) 0.0541(8) Uani 1 1 d . . .
H43A H 0.2504 0.7209 0.8370 0.081 Uiso 1 1 calc R . .
H43B H 0.2332 0.6080 0.8519 0.081 Uiso 1 1 calc R . .
H43C H 0.1483 0.6856 0.8375 0.081 Uiso 1 1 calc R . .
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
Co 0.01577(14) 0.01770(15) 0.01471(14) -0.00011(9) 0.00534(10) -0.00038(10)
N1 0.0201(8) 0.0202(8) 0.0181(8) -0.0016(6) 0.0070(7) -0.0016(7)
N2 0.0255(9) 0.0211(9) 0.0185(8) -0.0015(7) 0.0071(7) -0.0010(7)
N3 0.0194(8) 0.0192(8) 0.0181(8) 0.0007(6) 0.0066(7) -0.0016(6)
N4 0.0182(8) 0.0228(9) 0.0186(8) 0.0010(7) 0.0063(7) -0.0014(7)
N5 0.0167(8) 0.0191(8) 0.0168(8) -0.0002(6) 0.0060(6) -0.0006(6)
N6 0.0192(8) 0.0223(9) 0.0177(8) 0.0013(6) 0.0051(7) 0.0013(7)
N7 0.0160(8) 0.0180(8) 0.0181(8) -0.0004(6) 0.0065(6) 0.0012(6)
N8 0.0202(8) 0.0217(8) 0.0195(8) 0.0011(7) 0.0091(7) 0.0016(7)
N9 0.0180(8) 0.0227(9) 0.0164(8) 0.0003(7) 0.0053(6) -0.0004(7)
N10 0.0158(8) 0.0196(8) 0.0163(8) 0.0005(6) 0.0056(6) 0.0002(6)
N11 0.0169(8) 0.0197(8) 0.0178(8) 0.0001(6) 0.0056(6) 0.0003(6)
O1 0.0208(7) 0.0202(7) 0.0234(7) 0.0008(6) 0.0083(6) -0.0006(6)
O2 0.0253(8) 0.0292(8) 0.0378(9) 0.0047(7) 0.0138(7) -0.0040(6)
O3 0.0265(9) 0.0548(12) 0.0624(13) -0.0205(10) 0.0100(9) 0.0062(8)
C1 0.0228(10) 0.0197(10) 0.0208(10) 0.0035(8) 0.0109(8) 0.0030(8)
C2 0.0282(11) 0.0188(10) 0.0200(10) 0.0033(8) 0.0108(8) 0.0037(8)
C3 0.0281(11) 0.0252(11) 0.0252(11) 0.0046(8) 0.0130(9) 0.0025(9)
C4 0.0382(13) 0.0299(12) 0.0291(12) 0.0044(9) 0.0216(10) 0.0059(10)
C5 0.0446(14) 0.0284(12) 0.0210(11) 0.0003(9) 0.0164(10) 0.0035(10)
C6 0.0355(12) 0.0231(11) 0.0216(10) 0.0001(8) 0.0107(9) -0.0001(9)
C7 0.0283(11) 0.0189(10) 0.0216(10) 0.0022(8) 0.0110(9) 0.0026(8)
C8 0.0278(10) 0.0172(9) 0.0163(9) 0.0020(7) 0.0077(8) 0.0014(8)
C9 0.0227(10) 0.0164(9) 0.0187(10) 0.0002(7) 0.0047(8) -0.0019(8)
C10 0.0225(10) 0.0194(10) 0.0218(10) 0.0028(8) 0.0046(8) -0.0029(8)
C11 0.0296(11) 0.0260(11) 0.0221(11) -0.0016(8) 0.0048(9) -0.0037(9)
C12 0.0287(11) 0.0325(12) 0.0245(11) -0.0013(9) -0.0004(9) -0.0085(9)
C13 0.0200(10) 0.0318(12) 0.0310(12) 0.0046(9) 0.0019(9) -0.0055(9)
C14 0.0226(10) 0.0273(11) 0.0236(11) 0.0030(8) 0.0061(8) -0.0033(8)
C15 0.0214(10) 0.0207(10) 0.0189(10) 0.0036(8) 0.0037(8) -0.0043(8)
C16 0.0154(9) 0.0229(10) 0.0182(9) 0.0008(8) 0.0036(7) -0.0023(8)
C17 0.0209(10) 0.0178(9) 0.0196(10) -0.0011(7) 0.0095(8) -0.0011(8)
C18 0.0230(10) 0.0192(10) 0.0187(10) -0.0017(7) 0.0082(8) 0.0000(8)
C19 0.0222(10) 0.0250(11) 0.0220(10) -0.0024(8) 0.0087(8) -0.0024(8)
C20 0.0300(11) 0.0264(11) 0.0246(11) -0.0012(8) 0.0160(9) -0.0033(9)
C21 0.0353(12) 0.0252(11) 0.0174(10) 0.0008(8) 0.0114(9) 0.0001(9)
C22 0.0245(10) 0.0231(10) 0.0191(10) -0.0010(8) 0.0060(8) 0.0011(8)
C23 0.0218(10) 0.0174(9) 0.0200(10) -0.0024(7) 0.0087(8) -0.0003(8)
C24 0.0214(10) 0.0160(9) 0.0170(9) -0.0002(7) 0.0068(8) 0.0014(7)
C25 0.0174(9) 0.0189(9) 0.0194(9) -0.0001(7) 0.0062(8) 0.0029(7)
C26 0.0176(9) 0.0202(10) 0.0223(10) -0.0008(8) 0.0064(8) 0.0024(8)
C27 0.0212(10) 0.0274(11) 0.0218(10) 0.0009(8) 0.0042(8) 0.0023(8)
C28 0.0221(10) 0.0307(12) 0.0238(11) -0.0023(9) 0.0011(8) -0.0002(9)
C29 0.0199(10) 0.0248(11) 0.0347(12) -0.0043(9) 0.0082(9) -0.0029(8)
C30 0.0205(10) 0.0220(10) 0.0267(11) 0.0001(8) 0.0085(8) 0.0015(8)
C31 0.0168(9) 0.0200(10) 0.0216(10) -0.0022(8) 0.0051(8) 0.0034(8)
C32 0.0167(9) 0.0186(10) 0.0208(10) 0.0004(7) 0.0069(8) -0.0006(7)
C33 0.0192(9) 0.0240(10) 0.0135(9) 0.0011(7) 0.0052(7) 0.0018(8)
C34 0.0197(9) 0.0220(10) 0.0137(9) -0.0004(7) 0.0050(7) 0.0002(8)
C35 0.0203(10) 0.0262(11) 0.0188(10) 0.0010(8) 0.0061(8) 0.0023(8)
C36 0.0251(11) 0.0251(11) 0.0233(10) 0.0022(8) 0.0083(8) 0.0077(9)
C37 0.0304(11) 0.0197(10) 0.0256(11) 0.0008(8) 0.0109(9) 0.0005(8)
C38 0.0223(10) 0.0218(10) 0.0215(10) -0.0004(8) 0.0089(8) -0.0009(8)
C39 0.0205(9) 0.0223(10) 0.0140(9) 0.0000(7) 0.0064(7) 0.0010(8)
C40 0.0201(9) 0.0192(10) 0.0137(9) -0.0009(7) 0.0064(7) -0.0009(8)
C41 0.0431(14) 0.0291(12) 0.0429(14) -0.0004(10) 0.0212(12) -0.0014(11)
C42 0.0405(14) 0.0382(14) 0.0318(12) 0.0021(10) 0.0164(11) -0.0029(11)
C43 0.0355(14) 0.0541(18) 0.065(2) -0.0277(15) 0.0068(13) 0.0016(13)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co N3 1.8536(17) . yes
Co N10 1.8577(17) . yes
Co N7 1.8612(16) . yes
Co N5 1.8956(16) . yes
Co N1 1.8982(17) . yes
Co O1 1.9978(14) . yes
N1 C8 1.353(3) . ?
N1 C1 1.407(3) . ?
N2 C8 1.327(3) . ?
N2 C9 1.364(3) . ?
N3 C9 1.311(3) . ?
N3 C16 1.473(3) . ?
N4 C17 1.284(3) . ?
N4 C16 1.465(3) . ?
N5 C24 1.358(2) . ?
N5 C17 1.402(2) . ?
N6 C24 1.322(3) . ?
N6 C25 1.365(3) . ?
N7 C25 1.309(2) . ?
N7 C32 1.473(2) . ?
N8 C1 1.284(3) . ?
N8 C32 1.462(2) . ?
N9 C33 1.293(3) . ?
N9 C16 1.481(3) . ?
N10 C40 1.370(3) . ?
N10 C33 1.382(3) . ?
N11 C40 1.297(2) . ?
N11 C32 1.479(2) . ?
O1 C41 1.439(3) . ?
O1 H1O 0.8400 . ?
O2 C42 1.421(3) . ?
O2 H2O 0.8400 . ?
O3 C43 1.401(4) . ?
O3 H3O 0.8400 . ?
C1 C2 1.482(3) . ?
C2 C3 1.382(3) . ?
C2 C7 1.391(3) . ?
C3 C4 1.397(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.384(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.479(3) . ?
C9 C10 1.474(3) . ?
C10 C11 1.388(3) . ?
C10 C15 1.389(3) . ?
C11 C12 1.388(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.386(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.396(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.525(3) . ?
C17 C18 1.482(3) . ?
C18 C19 1.384(3) . ?
C18 C23 1.393(3) . ?
C19 C20 1.396(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.391(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.395(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.383(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.475(3) . ?
C25 C26 1.472(3) . ?
C26 C31 1.390(3) . ?
C26 C27 1.391(3) . ?
C27 C28 1.393(3) . ?
C27 H27 0.9500 . ?
C28 C29 1.388(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.397(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.381(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.523(3) . ?
C33 C34 1.483(3) . ?
C34 C35 1.388(3) . ?
C34 C39 1.397(3) . ?
C35 C36 1.391(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.394(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.394(3) . ?
C37 H37 0.9500 . ?
C38 C39 1.385(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.486(3) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
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_3
_geom_angle_publ_flag
N3 Co N10 87.28(7) . . yes
N3 Co N7 174.36(7) . . yes
N10 Co N7 87.08(7) . . yes
N3 Co N5 90.72(7) . . yes
N10 Co N5 92.68(7) . . yes
N7 Co N5 89.31(7) . . yes
N3 Co N1 89.59(7) . . yes
N10 Co N1 92.39(7) . . yes
N7 Co N1 90.87(7) . . yes
N5 Co N1 174.93(7) . . yes
N3 Co O1 91.97(7) . . yes
N10 Co O1 177.17(6) . . yes
N7 Co O1 93.67(6) . . yes
N5 Co O1 90.06(6) . . yes
N1 Co O1 84.88(6) . . yes
C8 N1 C1 109.71(17) . . ?
C8 N1 Co 123.35(14) . . ?
C1 N1 Co 124.36(13) . . ?
C8 N2 C9 117.38(17) . . ?
C9 N3 C16 111.69(16) . . ?
C9 N3 Co 127.62(14) . . ?
C16 N3 Co 119.02(13) . . ?
C17 N4 C16 117.85(17) . . ?
C24 N5 C17 109.69(16) . . ?
C24 N5 Co 123.02(13) . . ?
C17 N5 Co 124.90(13) . . ?
C24 N6 C25 117.11(17) . . ?
C25 N7 C32 111.56(16) . . ?
C25 N7 Co 127.82(14) . . ?
C32 N7 Co 118.72(12) . . ?
C1 N8 C32 117.19(17) . . ?
C33 N9 C16 119.87(17) . . ?
C40 N10 C33 111.33(17) . . ?
C40 N10 Co 124.19(13) . . ?
C33 N10 Co 124.41(14) . . ?
C40 N11 C32 120.50(16) . . ?
C41 O1 Co 126.38(13) . . ?
C41 O1 H1O 109.5 . . ?
Co O1 H1O 111.2 . . ?
C42 O2 H2O 109.5 . . ?
C43 O3 H3O 109.5 . . ?
N8 C1 N1 128.65(18) . . ?
N8 C1 C2 124.10(18) . . ?
N1 C1 C2 107.24(17) . . ?
C3 C2 C7 121.8(2) . . ?
C3 C2 C1 131.2(2) . . ?
C7 C2 C1 107.04(18) . . ?
C2 C3 C4 116.8(2) . . ?
C2 C3 H3 121.6 . . ?
C4 C3 H3 121.6 . . ?
C5 C4 C3 121.4(2) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 121.5(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C7 C6 C5 117.1(2) . . ?
C7 C6 H6 121.4 . . ?
C5 C6 H6 121.4 . . ?
C6 C7 C2 121.4(2) . . ?
C6 C7 C8 131.7(2) . . ?
C2 C7 C8 106.92(18) . . ?
N2 C8 N1 128.63(19) . . ?
N2 C8 C7 122.31(18) . . ?
N1 C8 C7 109.05(18) . . ?
N3 C9 N2 127.51(18) . . ?
N3 C9 C10 109.61(18) . . ?
N2 C9 C10 122.83(18) . . ?
C11 C10 C15 121.6(2) . . ?
C11 C10 C9 131.3(2) . . ?
C15 C10 C9 107.02(17) . . ?
C12 C11 C10 117.4(2) . . ?
C12 C11 H11 121.3 . . ?
C10 C11 H11 121.3 . . ?
C13 C12 C11 121.2(2) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 121.2(2) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C13 117.6(2) . . ?
C15 C14 H14 121.2 . . ?
C13 C14 H14 121.2 . . ?
C14 C15 C10 120.94(19) . . ?
C14 C15 C16 130.53(19) . . ?
C10 C15 C16 108.52(18) . . ?
N4 C16 N3 114.03(16) . . ?
N4 C16 N9 109.02(16) . . ?
N3 C16 N9 111.53(15) . . ?
N4 C16 C15 111.92(16) . . ?
N3 C16 C15 101.98(16) . . ?
N9 C16 C15 108.10(16) . . ?
N4 C17 N5 128.27(18) . . ?
N4 C17 C18 124.23(18) . . ?
N5 C17 C18 107.50(16) . . ?
C19 C18 C23 120.92(19) . . ?
C19 C18 C17 132.36(19) . . ?
C23 C18 C17 106.72(17) . . ?
C18 C19 C20 117.63(19) . . ?
C18 C19 H19 121.2 . . ?
C20 C19 H19 121.2 . . ?
C21 C20 C19 121.25(19) . . ?
C21 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C20 C21 C22 120.98(19) . . ?
C20 C21 H21 119.5 . . ?
C22 C21 H21 119.5 . . ?
C23 C22 C21 117.36(19) . . ?
C23 C22 H22 121.3 . . ?
C21 C22 H22 121.3 . . ?
C22 C23 C18 121.82(19) . . ?
C22 C23 C24 130.96(19) . . ?
C18 C23 C24 107.22(17) . . ?
N6 C24 N5 128.69(18) . . ?
N6 C24 C23 122.44(17) . . ?
N5 C24 C23 108.83(17) . . ?
N7 C25 N6 127.08(18) . . ?
N7 C25 C26 110.00(17) . . ?
N6 C25 C26 122.89(17) . . ?
C31 C26 C27 121.85(19) . . ?
C31 C26 C25 107.13(17) . . ?
C27 C26 C25 130.93(19) . . ?
C26 C27 C28 116.9(2) . . ?
C26 C27 H27 121.5 . . ?
C28 C27 H27 121.5 . . ?
C29 C28 C27 121.4(2) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C28 C29 C30 121.1(2) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 H29 119.4 . . ?
C31 C30 C29 117.6(2) . . ?
C31 C30 H30 121.2 . . ?
C29 C30 H30 121.2 . . ?
C30 C31 C26 121.05(19) . . ?
C30 C31 C32 130.47(19) . . ?
C26 C31 C32 108.30(17) . . ?
N8 C32 N7 113.81(16) . . ?
N8 C32 N11 108.73(15) . . ?
N7 C32 N11 111.60(15) . . ?
N8 C32 C31 112.80(16) . . ?
N7 C32 C31 102.23(15) . . ?
N11 C32 C31 107.43(15) . . ?
N9 C33 N10 129.64(19) . . ?
N9 C33 C34 123.52(18) . . ?
N10 C33 C34 106.78(17) . . ?
C35 C34 C39 121.28(19) . . ?
C35 C34 C33 131.11(19) . . ?
C39 C34 C33 107.57(17) . . ?
C34 C35 C36 117.29(19) . . ?
C34 C35 H35 121.4 . . ?
C36 C35 H35 121.4 . . ?
C35 C36 C37 121.44(19) . . ?
C35 C36 H36 119.3 . . ?
C37 C36 H36 119.3 . . ?
C38 C37 C36 121.2(2) . . ?
C38 C37 H37 119.4 . . ?
C36 C37 H37 119.4 . . ?
C39 C38 C37 117.26(19) . . ?
C39 C38 H38 121.4 . . ?
C37 C38 H38 121.4 . . ?
C38 C39 C34 121.50(18) . . ?
C38 C39 C40 131.83(18) . . ?
C34 C39 C40 106.65(17) . . ?
N11 C40 N10 129.51(18) . . ?
N11 C40 C39 122.93(18) . . ?
N10 C40 C39 107.55(16) . . ?
O1 C41 H41A 109.5 . . ?
O1 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O1 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O2 C42 H42A 109.5 . . ?
O2 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O2 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O3 C43 H43A 109.5 . . ?
O3 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O3 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
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
N3 Co N1 C8 -24.23(16) . . . . ?
N10 Co N1 C8 -111.49(16) . . . . ?
N7 Co N1 C8 161.39(16) . . . . ?
N5 Co N1 C8 69.4(8) . . . . ?
O1 Co N1 C8 67.78(16) . . . . ?
N3 Co N1 C1 175.88(16) . . . . ?
N10 Co N1 C1 88.62(16) . . . . ?
N7 Co N1 C1 1.50(16) . . . . ?
N5 Co N1 C1 -90.5(8) . . . . ?
O1 Co N1 C1 -92.10(16) . . . . ?
N10 Co N3 C9 108.59(18) . . . . ?
N7 Co N3 C9 110.9(7) . . . . ?
N5 Co N3 C9 -158.76(18) . . . . ?
N1 Co N3 C9 16.18(18) . . . . ?
O1 Co N3 C9 -68.68(17) . . . . ?
N10 Co N3 C16 -55.37(14) . . . . ?
N7 Co N3 C16 -53.0(8) . . . . ?
N5 Co N3 C16 37.27(14) . . . . ?
N1 Co N3 C16 -147.78(14) . . . . ?
O1 Co N3 C16 127.35(14) . . . . ?
N3 Co N5 C24 160.14(16) . . . . ?
N10 Co N5 C24 -112.55(16) . . . . ?
N7 Co N5 C24 -25.50(16) . . . . ?
N1 Co N5 C24 66.6(8) . . . . ?
O1 Co N5 C24 68.17(15) . . . . ?
N3 Co N5 C17 -0.46(16) . . . . ?
N10 Co N5 C17 86.86(16) . . . . ?
N7 Co N5 C17 173.91(16) . . . . ?
N1 Co N5 C17 -94.0(8) . . . . ?
O1 Co N5 C17 -92.43(16) . . . . ?
N3 Co N7 C25 104.3(7) . . . . ?
N10 Co N7 C25 106.64(17) . . . . ?
N5 Co N7 C25 13.93(17) . . . . ?
N1 Co N7 C25 -161.01(17) . . . . ?
O1 Co N7 C25 -76.09(17) . . . . ?
N3 Co N7 C32 -58.6(7) . . . . ?
N10 Co N7 C32 -56.25(14) . . . . ?
N5 Co N7 C32 -148.97(14) . . . . ?
N1 Co N7 C32 36.10(14) . . . . ?
O1 Co N7 C32 121.02(13) . . . . ?
N3 Co N10 C40 -150.85(16) . . . . ?
N7 Co N10 C40 29.38(15) . . . . ?
N5 Co N10 C40 118.56(15) . . . . ?
N1 Co N10 C40 -61.37(16) . . . . ?
N3 Co N10 C33 25.89(16) . . . . ?
N7 Co N10 C33 -153.88(16) . . . . ?
N5 Co N10 C33 -64.70(16) . . . . ?
N1 Co N10 C33 115.37(16) . . . . ?
N3 Co O1 C41 -69.57(18) . . . . ?
N7 Co O1 C41 110.47(17) . . . . ?
N5 Co O1 C41 21.15(18) . . . . ?
N1 Co O1 C41 -158.99(18) . . . . ?
C32 N8 C1 N1 -2.9(3) . . . . ?
C32 N8 C1 C2 176.51(18) . . . . ?
C8 N1 C1 N8 178.6(2) . . . . ?
Co N1 C1 N8 -19.2(3) . . . . ?
C8 N1 C1 C2 -0.9(2) . . . . ?
Co N1 C1 C2 161.37(13) . . . . ?
N8 C1 C2 C3 1.1(4) . . . . ?
N1 C1 C2 C3 -179.4(2) . . . . ?
N8 C1 C2 C7 -177.61(19) . . . . ?
N1 C1 C2 C7 1.9(2) . . . . ?
C7 C2 C3 C4 -0.5(3) . . . . ?
C1 C2 C3 C4 -179.1(2) . . . . ?
C2 C3 C4 C5 0.8(3) . . . . ?
C3 C4 C5 C6 0.1(3) . . . . ?
C4 C5 C6 C7 -1.4(3) . . . . ?
C5 C6 C7 C2 1.7(3) . . . . ?
C5 C6 C7 C8 -178.1(2) . . . . ?
C3 C2 C7 C6 -0.8(3) . . . . ?
C1 C2 C7 C6 178.10(19) . . . . ?
C3 C2 C7 C8 179.06(19) . . . . ?
C1 C2 C7 C8 -2.1(2) . . . . ?
C9 N2 C8 N1 5.4(3) . . . . ?
C9 N2 C8 C7 -173.33(18) . . . . ?
C1 N1 C8 N2 -179.3(2) . . . . ?
Co N1 C8 N2 18.2(3) . . . . ?
C1 N1 C8 C7 -0.4(2) . . . . ?
Co N1 C8 C7 -162.87(13) . . . . ?
C6 C7 C8 N2 0.4(3) . . . . ?
C2 C7 C8 N2 -179.41(18) . . . . ?
C6 C7 C8 N1 -178.6(2) . . . . ?
C2 C7 C8 N1 1.6(2) . . . . ?
C16 N3 C9 N2 165.87(19) . . . . ?
Co N3 C9 N2 0.9(3) . . . . ?
C16 N3 C9 C10 -11.5(2) . . . . ?
Co N3 C9 C10 -176.44(13) . . . . ?
C8 N2 C9 N3 -16.0(3) . . . . ?
C8 N2 C9 C10 161.01(18) . . . . ?
N3 C9 C10 C11 -173.2(2) . . . . ?
N2 C9 C10 C11 9.3(3) . . . . ?
N3 C9 C10 C15 7.7(2) . . . . ?
N2 C9 C10 C15 -169.77(18) . . . . ?
C15 C10 C11 C12 -0.4(3) . . . . ?
C9 C10 C11 C12 -179.4(2) . . . . ?
C10 C11 C12 C13 1.5(3) . . . . ?
C11 C12 C13 C14 -0.6(4) . . . . ?
C12 C13 C14 C15 -1.5(3) . . . . ?
C13 C14 C15 C10 2.5(3) . . . . ?
C13 C14 C15 C16 -179.3(2) . . . . ?
C11 C10 C15 C14 -1.6(3) . . . . ?
C9 C10 C15 C14 177.53(18) . . . . ?
C11 C10 C15 C16 179.81(19) . . . . ?
C9 C10 C15 C16 -1.0(2) . . . . ?
C17 N4 C16 N3 41.3(2) . . . . ?
C17 N4 C16 N9 -84.1(2) . . . . ?
C17 N4 C16 C15 156.39(18) . . . . ?
C9 N3 C16 N4 131.10(18) . . . . ?
Co N3 C16 N4 -62.52(19) . . . . ?
C9 N3 C16 N9 -104.88(18) . . . . ?
Co N3 C16 N9 61.50(19) . . . . ?
C9 N3 C16 C15 10.3(2) . . . . ?
Co N3 C16 C15 176.66(12) . . . . ?
C33 N9 C16 N4 102.5(2) . . . . ?
C33 N9 C16 N3 -24.3(2) . . . . ?
C33 N9 C16 C15 -135.65(18) . . . . ?
C14 C15 C16 N4 54.3(3) . . . . ?
C10 C15 C16 N4 -127.35(18) . . . . ?
C14 C15 C16 N3 176.6(2) . . . . ?
C10 C15 C16 N3 -5.1(2) . . . . ?
C14 C15 C16 N9 -65.8(3) . . . . ?
C10 C15 C16 N9 112.57(18) . . . . ?
C16 N4 C17 N5 -1.3(3) . . . . ?
C16 N4 C17 C18 179.35(18) . . . . ?
C24 N5 C17 N4 179.1(2) . . . . ?
Co N5 C17 N4 -18.2(3) . . . . ?
C24 N5 C17 C18 -1.5(2) . . . . ?
Co N5 C17 C18 161.28(13) . . . . ?
N4 C17 C18 C19 -0.5(4) . . . . ?
N5 C17 C18 C19 -180.0(2) . . . . ?
N4 C17 C18 C23 179.70(19) . . . . ?
N5 C17 C18 C23 0.2(2) . . . . ?
C23 C18 C19 C20 -1.8(3) . . . . ?
C17 C18 C19 C20 178.4(2) . . . . ?
C18 C19 C20 C21 0.6(3) . . . . ?
C19 C20 C21 C22 1.3(3) . . . . ?
C20 C21 C22 C23 -1.8(3) . . . . ?
C21 C22 C23 C18 0.5(3) . . . . ?
C21 C22 C23 C24 -179.3(2) . . . . ?
C19 C18 C23 C22 1.4(3) . . . . ?
C17 C18 C23 C22 -178.81(18) . . . . ?
C19 C18 C23 C24 -178.81(18) . . . . ?
C17 C18 C23 C24 1.0(2) . . . . ?
C25 N6 C24 N5 5.0(3) . . . . ?
C25 N6 C24 C23 -172.62(18) . . . . ?
C17 N5 C24 N6 -175.75(19) . . . . ?
Co N5 C24 N6 21.1(3) . . . . ?
C17 N5 C24 C23 2.2(2) . . . . ?
Co N5 C24 C23 -161.03(13) . . . . ?
C22 C23 C24 N6 -4.1(3) . . . . ?
C18 C23 C24 N6 176.08(18) . . . . ?
C22 C23 C24 N5 177.8(2) . . . . ?
C18 C23 C24 N5 -2.0(2) . . . . ?
C32 N7 C25 N6 170.10(18) . . . . ?
Co N7 C25 N6 6.2(3) . . . . ?
C32 N7 C25 C26 -8.3(2) . . . . ?
Co N7 C25 C26 -172.18(13) . . . . ?
C24 N6 C25 N7 -19.8(3) . . . . ?
C24 N6 C25 C26 158.34(18) . . . . ?
N7 C25 C26 C31 3.8(2) . . . . ?
N6 C25 C26 C31 -174.67(18) . . . . ?
N7 C25 C26 C27 -179.7(2) . . . . ?
N6 C25 C26 C27 1.8(3) . . . . ?
C31 C26 C27 C28 -1.1(3) . . . . ?
C25 C26 C27 C28 -177.2(2) . . . . ?
C26 C27 C28 C29 0.5(3) . . . . ?
C27 C28 C29 C30 0.6(3) . . . . ?
C28 C29 C30 C31 -1.1(3) . . . . ?
C29 C30 C31 C26 0.4(3) . . . . ?
C29 C30 C31 C32 174.9(2) . . . . ?
C27 C26 C31 C30 0.7(3) . . . . ?
C25 C26 C31 C30 177.58(18) . . . . ?
C27 C26 C31 C32 -174.85(18) . . . . ?
C25 C26 C31 C32 2.0(2) . . . . ?
C1 N8 C32 N7 44.0(2) . . . . ?
C1 N8 C32 N11 -81.1(2) . . . . ?
C1 N8 C32 C31 159.87(18) . . . . ?
C25 N7 C32 N8 130.95(17) . . . . ?
Co N7 C32 N8 -63.52(19) . . . . ?
C25 N7 C32 N11 -105.53(18) . . . . ?
Co N7 C32 N11 60.00(19) . . . . ?
C25 N7 C32 C31 9.0(2) . . . . ?
Co N7 C32 C31 174.55(12) . . . . ?
C40 N11 C32 N8 103.4(2) . . . . ?
C40 N11 C32 N7 -22.9(2) . . . . ?
C40 N11 C32 C31 -134.21(18) . . . . ?
C30 C31 C32 N8 56.0(3) . . . . ?
C26 C31 C32 N8 -128.98(18) . . . . ?
C30 C31 C32 N7 178.7(2) . . . . ?
C26 C31 C32 N7 -6.4(2) . . . . ?
C30 C31 C32 N11 -63.8(3) . . . . ?
C26 C31 C32 N11 111.22(18) . . . . ?
C16 N9 C33 N10 -4.9(3) . . . . ?
C16 N9 C33 C34 171.74(17) . . . . ?
C40 N10 C33 N9 176.12(19) . . . . ?
Co N10 C33 N9 -1.0(3) . . . . ?
C40 N10 C33 C34 -1.0(2) . . . . ?
Co N10 C33 C34 -178.10(12) . . . . ?
N9 C33 C34 C35 3.3(3) . . . . ?
N10 C33 C34 C35 -179.40(19) . . . . ?
N9 C33 C34 C39 -174.48(18) . . . . ?
N10 C33 C34 C39 2.9(2) . . . . ?
C39 C34 C35 C36 1.4(3) . . . . ?
C33 C34 C35 C36 -176.09(19) . . . . ?
C34 C35 C36 C37 -1.4(3) . . . . ?
C35 C36 C37 C38 0.3(3) . . . . ?
C36 C37 C38 C39 0.9(3) . . . . ?
C37 C38 C39 C34 -1.0(3) . . . . ?
C37 C38 C39 C40 -179.3(2) . . . . ?
C35 C34 C39 C38 -0.2(3) . . . . ?
C33 C34 C39 C38 177.82(18) . . . . ?
C35 C34 C39 C40 178.53(17) . . . . ?
C33 C34 C39 C40 -3.5(2) . . . . ?
C32 N11 C40 N10 -3.7(3) . . . . ?
C32 N11 C40 C39 174.76(17) . . . . ?
C33 N10 C40 N11 177.55(19) . . . . ?
Co N10 C40 N11 -5.3(3) . . . . ?
C33 N10 C40 C39 -1.1(2) . . . . ?
Co N10 C40 C39 175.98(12) . . . . ?
C38 C39 C40 N11 2.7(3) . . . . ?
C34 C39 C40 N11 -175.87(18) . . . . ?
C38 C39 C40 N10 -178.5(2) . . . . ?
C34 C39 C40 N10 2.9(2) . . . . ?
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
O2 H2O N11 0.84 1.87 2.696(2) 168.3 .
O3 H3O N9 0.84 2.01 2.837(2) 168.0 .
O1 H1O O2 0.84 1.73 2.564(2) 174.0 2_646
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 26.39
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 1.251
_refine_diff_density_min -0.354
_refine_diff_density_rms 0.069
# File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison.
#===END
data_mcg018
_database_code_depnum_ccdc_archive 'CCDC 606958'
_publ_section_references
;
Allen, F.H. (2002). Acta Cryst. B58, 380-388.
Bruker-AXS. (2003). SADABS (Version 2.05), SAINT
(Version 6.22),
SHELXTL (Version 6.10), and SMART
(Version 5.622). Bruker-AXS
Inc., Madison, WI, USA.
Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M.,
Macrae, C. F., McCabe, P., Pearson, J,
& Taylor, R. (2002). Acta Cryst. B58, 389-397.
Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc.
97, 1358-1367.
Frisch, M. J., Trucks, G. W.,
Schlegel, H. B., Scuseria, G. E., Robb, M. A., Cheeseman,
J. R., Montgomery, Jr., J. A., Vreven, T., Kudin, K. N., Burant,
J. C., Millam, J. M., Iyengar, S. S., Tomasi, J., Barone, V.,
Mennucci, B. et al. (2004).
Gaussian 03, Revision C.02,
Gaussian, Inc., Wallingford, CT, USA.
;
_publ_section_acknowledgements
;
We thank the National Science Foundation for financial support.
The manuscript was prepared with the beta test version 1.0.0.
of program publCIF to be released by the IUCr and Ilia A. Guzei's
program modiCIFer to be released by University of Wisconsin-Madison.
;
_publ_section_figure_captions
;
Figure 1. Molecular structure of (I). The thermal ellipsoids are
shown at 50% probability level.
;
_publ_section_exptl_prep
;
;
_publ_section_exptl_refinement
;
All H-atoms were placed in idealized locations and
refined as riding with appropriate thermal displacement
coefficients U~iso~(H) = 1.2 or 1.5 times U~eq~(bearing atom).
Default effective X-H distances for T = -173.0 C
AFIX m = C1 C2 C3 C4 4[N] 3[N] 15[B] 8[O] 9 9[N] 16
d(X-H) = 1.00 0.99 0.98 0.95 0.88 0.91 1.12 0.84 0.95 0.88 0.95
;
#3. data
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C43 H32.38 Fe N11 O3.19'
_chemical_formula_sum 'C43 H32.38 Fe N11 O3.19'
_chemical_formula_weight 810.07
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 1 21/n 1 '
_symmetry_space_group_name_Hall '-P 2yn '
_symmetry_int_tables_number 14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.9070(9)
_cell_length_b 13.6717(8)
_cell_length_c 18.8658(12)
_cell_angle_alpha 90.00
_cell_angle_beta 109.8550(10)
_cell_angle_gamma 90.00
_cell_volume 3616.4(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 19198
_cell_measurement_theta_min 2.2955
_cell_measurement_theta_max 26.3780
_exptl_crystal_description block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.28
_exptl_crystal_size_min 0.23
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.488
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1676
_exptl_absorpt_coefficient_mu 0.478
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker-AXS, 2003)
;
_exptl_absorpt_correction_T_min 0.8244
_exptl_absorpt_correction_T_max 0.8980
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type Mo-K\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker CCD-1000 area detector'
_diffrn_measurement_method '0.30\% \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 39149
_diffrn_reflns_av_R_equivalents 0.0260
_diffrn_reflns_av_sigmaI/netI 0.0179
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 1.88
_diffrn_reflns_theta_max 26.38
_reflns_number_total 7398
_reflns_number_gt 6565
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_cell_refinement 'SAINT Ver. 6.22 (Bruker-AXS, 2003)'
_computing_data_reduction 'SAINT Ver. 6.22'
_computing_structure_solution 'SHELXTL Ver. 6.10 (Bruker-AXS, 2003)'
_computing_structure_refinement 'SHELXTL Ver. 6.10'
_computing_molecular_graphics 'SHELXTL Ver. 6.10'
_computing_publication_material 'SHELXTL Ver. 6.10'
_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^)+(0.0426P)^2^+2.7160P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7398
_refine_ls_number_parameters 553
_refine_ls_number_restraints 3
_refine_ls_R_factor_all 0.0366
_refine_ls_R_factor_gt 0.0311
_refine_ls_wR_factor_ref 0.0847
_refine_ls_wR_factor_gt 0.0804
_refine_ls_goodness_of_fit_ref 1.024
_refine_ls_restrained_S_all 1.024
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.541561(14) 0.453254(15) 0.760610(11) 0.01301(7) Uani 1 1 d . A 1
N1 N 0.58309(9) 0.45297(9) 0.67556(7) 0.0154(3) Uani 1 1 d . A 1
N2 N 0.44288(9) 0.38240(10) 0.58359(7) 0.0171(3) Uani 1 1 d . A 1
N3 N 0.41619(9) 0.43242(9) 0.69671(7) 0.0153(3) Uani 1 1 d . A 1
N4 N 0.33148(9) 0.43381(9) 0.78870(7) 0.0160(3) Uani 1 1 d . A 1
N5 N 0.50305(9) 0.44063(9) 0.84657(7) 0.0146(3) Uani 1 1 d . A 1
N6 N 0.65857(9) 0.43850(9) 0.94360(7) 0.0161(3) Uani 1 1 d . A 1
N7 N 0.66387(9) 0.48935(9) 0.82356(7) 0.0142(2) Uani 1 1 d . A 1
N8 N 0.74370(9) 0.51669(10) 0.73036(7) 0.0161(3) Uani 1 1 d . A 1
N9 N 0.34241(9) 0.58104(10) 0.72234(7) 0.0153(3) Uani 1 1 d . A 1
N10 N 0.51338(9) 0.58658(9) 0.75080(7) 0.0146(3) Uani 1 1 d . A 1
N11 N 0.67087(9) 0.65124(9) 0.77135(7) 0.0153(3) Uani 1 1 d . A 1
O1 O 0.57241(8) 0.31046(8) 0.76713(6) 0.0181(2) Uani 1 1 d D A 1
H1A H 0.6307(3) 0.2982(14) 0.7775(10) 0.022 Uiso 1 1 d D B 1
H1B H 0.542(2) 0.284(6) 0.793(4) 0.022 Uiso 0.19 1 d PD C 1
O2 O 0.74889(8) 0.77423(9) 0.69661(7) 0.0243(3) Uani 1 1 d . D 1
H2 H 0.7309 0.7375 0.7249 0.036 Uiso 1 1 calc R D 1
O3 O 0.17538(9) 0.64714(12) 0.74763(9) 0.0456(4) Uani 1 1 d . E 1
H3 H 0.2224 0.6265 0.7370 0.068 Uiso 1 1 calc R E 1
C1 C 0.67705(11) 0.47242(11) 0.67834(9) 0.0159(3) Uani 1 1 d . A 1
C2 C 0.68634(11) 0.43506(11) 0.60767(9) 0.0173(3) Uani 1 1 d . A 1
C3 C 0.76304(12) 0.43396(12) 0.58198(9) 0.0199(3) Uani 1 1 d . A 1
H3A H 0.8236 0.4590 0.6118 0.024 Uiso 1 1 calc R A 1
C4 C 0.74778(12) 0.39465(12) 0.51066(9) 0.0228(3) Uani 1 1 d . A 1
H4A H 0.7990 0.3922 0.4915 0.027 Uiso 1 1 calc R A 1
C5 C 0.65868(13) 0.35889(12) 0.46696(9) 0.0235(3) Uani 1 1 d . A 1
H5A H 0.6503 0.3324 0.4186 0.028 Uiso 1 1 calc R A 1
C6 C 0.58149(12) 0.36114(12) 0.49276(9) 0.0207(3) Uani 1 1 d . A 1
H6A H 0.5205 0.3377 0.4626 0.025 Uiso 1 1 calc R A 1
C7 C 0.59718(11) 0.39885(11) 0.56403(9) 0.0176(3) Uani 1 1 d . A 1
C8 C 0.53347(11) 0.41005(11) 0.60881(8) 0.0160(3) Uani 1 1 d . A 1
C9 C 0.38746(11) 0.40450(11) 0.62593(8) 0.0159(3) Uani 1 1 d . A 1
C10 C 0.28231(11) 0.40339(11) 0.59568(9) 0.0173(3) Uani 1 1 d . A 1
C11 C 0.21911(12) 0.37045(12) 0.52730(9) 0.0210(3) Uani 1 1 d . A 1
H11A H 0.2412 0.3423 0.4902 0.025 Uiso 1 1 calc R A 1
C12 C 0.12214(12) 0.38034(13) 0.51529(10) 0.0245(4) Uani 1 1 d . A 1
H12A H 0.0770 0.3571 0.4696 0.029 Uiso 1 1 calc R A 1
C13 C 0.09022(11) 0.42359(13) 0.56884(9) 0.0230(3) Uani 1 1 d . A 1
H13A H 0.0236 0.4302 0.5589 0.028 Uiso 1 1 calc R A 1
C14 C 0.15421(11) 0.45770(12) 0.63727(9) 0.0196(3) Uani 1 1 d . A 1
H14A H 0.1323 0.4884 0.6736 0.023 Uiso 1 1 calc R A 1
C15 C 0.25065(11) 0.44501(11) 0.65011(8) 0.0164(3) Uani 1 1 d . A 1
C16 C 0.33737(10) 0.47263(11) 0.71795(8) 0.0157(3) Uani 1 1 d . A 1
C17 C 0.40942(11) 0.42199(11) 0.84430(8) 0.0151(3) Uani 1 1 d . A 1
C18 C 0.41535(11) 0.38558(11) 0.91988(8) 0.0164(3) Uani 1 1 d . A 1
C19 C 0.34644(11) 0.35555(11) 0.94925(9) 0.0185(3) Uani 1 1 d . A 1
H19A H 0.2806 0.3571 0.9197 0.022 Uiso 1 1 calc R A 1
C20 C 0.37697(12) 0.32294(12) 1.02380(9) 0.0203(3) Uani 1 1 d . A 1
H20A H 0.3312 0.3012 1.0452 0.024 Uiso 1 1 calc R A 1
C21 C 0.47340(12) 0.32174(12) 1.06738(9) 0.0210(3) Uani 1 1 d . A 1
H21A H 0.4924 0.2982 1.1177 0.025 Uiso 1 1 calc R A 1
C22 C 0.54248(11) 0.35453(12) 1.03829(9) 0.0190(3) Uani 1 1 d . A 1
H22A H 0.6082 0.3553 1.0682 0.023 Uiso 1 1 calc R A 1
C23 C 0.51173(11) 0.38594(11) 0.96419(8) 0.0159(3) Uani 1 1 d . A 1
C24 C 0.56535(11) 0.42355(11) 0.91693(8) 0.0153(3) Uani 1 1 d . A 1
C25 C 0.69970(10) 0.48229(11) 0.89734(8) 0.0153(3) Uani 1 1 d . A 1
C26 C 0.79290(11) 0.53177(11) 0.92526(9) 0.0165(3) Uani 1 1 d . A 1
C27 C 0.85758(11) 0.54286(12) 0.99772(9) 0.0192(3) Uani 1 1 d . A 1
H27A H 0.8467 0.5139 1.0399 0.023 Uiso 1 1 calc R A 1
C28 C 0.93912(11) 0.59804(12) 1.00626(9) 0.0221(3) Uani 1 1 d . A 1
H28A H 0.9850 0.6067 1.0551 0.027 Uiso 1 1 calc R A 1
C29 C 0.95453(11) 0.64078(12) 0.94436(10) 0.0217(3) Uani 1 1 d . A 1
H29A H 1.0110 0.6776 0.9516 0.026 Uiso 1 1 calc R A 1
C30 C 0.88841(11) 0.63043(11) 0.87181(9) 0.0187(3) Uani 1 1 d . A 1
H30A H 0.8984 0.6604 0.8297 0.022 Uiso 1 1 calc R A 1
C31 C 0.80784(10) 0.57498(11) 0.86343(9) 0.0163(3) Uani 1 1 d . A 1
C32 C 0.72011(10) 0.55620(11) 0.79401(9) 0.0155(3) Uani 1 1 d . A 1
C33 C 0.42281(11) 0.62549(11) 0.73447(8) 0.0150(3) Uani 1 1 d . A 1
C34 C 0.43188(11) 0.73297(11) 0.72867(8) 0.0152(3) Uani 1 1 d . A 1
C35 C 0.36434(11) 0.80679(12) 0.71361(8) 0.0176(3) Uani 1 1 d . A 1
H35A H 0.2998 0.7933 0.7082 0.021 Uiso 1 1 calc R A 1
C36 C 0.39470(12) 0.90163(12) 0.70672(9) 0.0212(3) Uani 1 1 d . A 1
H36A H 0.3497 0.9536 0.6951 0.025 Uiso 1 1 calc R A 1
C37 C 0.48975(12) 0.92168(12) 0.71650(10) 0.0230(3) Uani 1 1 d . A 1
H37A H 0.5084 0.9871 0.7116 0.028 Uiso 1 1 calc R A 1
C38 C 0.55820(11) 0.84766(12) 0.73332(9) 0.0190(3) Uani 1 1 d . A 1
H38A H 0.6233 0.8615 0.7409 0.023 Uiso 1 1 calc R A 1
C39 C 0.52756(10) 0.75326(11) 0.73851(8) 0.0157(3) Uani 1 1 d . A 1
C40 C 0.57925(11) 0.65863(11) 0.75500(8) 0.0145(3) Uani 1 1 d . A 1
C41 C 0.53398(15) 0.23510(15) 0.80195(13) 0.0242(4) Uani 0.81 1 d P A 1
H41A H 0.5614 0.2412 0.8569 0.036 Uiso 0.81 1 calc PR A 1
H41B H 0.5499 0.1708 0.7866 0.036 Uiso 0.81 1 calc PR A 1
H41C H 0.4645 0.2420 0.7860 0.036 Uiso 0.81 1 calc PR A 1
C42 C 0.69186(13) 0.75677(14) 0.62029(10) 0.0295(4) Uani 1 1 d . D 1
H42A H 0.6281 0.7842 0.6106 0.044 Uiso 1 1 calc R D 1
H42B H 0.6868 0.6862 0.6108 0.044 Uiso 1 1 calc R D 1
H42C H 0.7214 0.7879 0.5869 0.044 Uiso 1 1 calc R D 1
C43 C 0.20353(15) 0.66646(19) 0.82518(14) 0.0508(6) Uani 1 1 d . E 1
H43A H 0.2493 0.7207 0.8378 0.076 Uiso 1 1 calc R E 1
H43B H 0.2335 0.6080 0.8534 0.076 Uiso 1 1 calc R E 1
H43C H 0.1475 0.6842 0.8384 0.076 Uiso 1 1 calc R E 1
O4 O 0.5001(5) 0.1981(5) 0.8459(4) 0.0261(14) Uani 0.19 1 d P F 2
H4B H 0.4426 0.1856 0.8390 0.039 Uiso 0.19 1 calc PR F 2
C44 C 0.5451(8) 0.1133(7) 0.8294(6) 0.035(2) Uani 0.19 1 d P F 2
H44A H 0.5138 0.0949 0.7765 0.052 Uiso 0.19 1 calc PR F 2
H44B H 0.5400 0.0592 0.8619 0.052 Uiso 0.19 1 calc PR F 2
H44C H 0.6126 0.1274 0.8384 0.052 Uiso 0.19 1 calc PR F 2
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
Fe 0.01168(11) 0.01530(12) 0.01192(11) -0.00052(8) 0.00382(8) -0.00010(8)
N1 0.0136(6) 0.0173(6) 0.0150(6) -0.0009(5) 0.0046(5) -0.0010(5)
N2 0.0171(6) 0.0181(6) 0.0159(6) -0.0010(5) 0.0053(5) -0.0013(5)
N3 0.0148(6) 0.0168(6) 0.0145(6) 0.0000(5) 0.0054(5) -0.0013(5)
N4 0.0147(6) 0.0184(6) 0.0154(6) -0.0002(5) 0.0058(5) -0.0009(5)
N5 0.0123(6) 0.0168(6) 0.0143(6) -0.0006(5) 0.0040(5) -0.0005(5)
N6 0.0148(6) 0.0173(6) 0.0151(6) 0.0004(5) 0.0038(5) 0.0005(5)
N7 0.0128(6) 0.0153(6) 0.0152(6) -0.0004(5) 0.0057(5) 0.0006(5)
N8 0.0153(6) 0.0179(6) 0.0160(6) 0.0012(5) 0.0065(5) 0.0012(5)
N9 0.0133(6) 0.0196(7) 0.0126(6) 0.0000(5) 0.0037(5) 0.0003(5)
N10 0.0126(6) 0.0177(6) 0.0132(6) 0.0005(5) 0.0040(5) 0.0001(5)
N11 0.0135(6) 0.0173(6) 0.0150(6) 0.0001(5) 0.0044(5) 0.0004(5)
O1 0.0165(5) 0.0180(6) 0.0210(6) 0.0005(4) 0.0078(4) -0.0006(4)
O2 0.0188(6) 0.0257(6) 0.0289(6) 0.0043(5) 0.0088(5) -0.0044(5)
O3 0.0195(6) 0.0532(9) 0.0580(10) -0.0269(8) 0.0052(6) 0.0075(6)
C1 0.0162(7) 0.0160(7) 0.0172(7) 0.0032(6) 0.0080(6) 0.0024(6)
C2 0.0209(8) 0.0156(7) 0.0165(7) 0.0024(6) 0.0078(6) 0.0022(6)
C3 0.0203(8) 0.0205(8) 0.0213(8) 0.0032(6) 0.0104(6) 0.0016(6)
C4 0.0283(9) 0.0230(8) 0.0231(8) 0.0038(7) 0.0165(7) 0.0047(7)
C5 0.0341(9) 0.0215(8) 0.0184(8) 0.0000(6) 0.0134(7) 0.0021(7)
C6 0.0257(8) 0.0187(8) 0.0178(8) 0.0004(6) 0.0076(6) -0.0001(6)
C7 0.0208(8) 0.0155(7) 0.0182(7) 0.0027(6) 0.0086(6) 0.0014(6)
C8 0.0201(8) 0.0145(7) 0.0138(7) 0.0014(6) 0.0062(6) 0.0013(6)
C9 0.0169(7) 0.0140(7) 0.0154(7) 0.0007(6) 0.0037(6) -0.0022(6)
C10 0.0166(7) 0.0163(7) 0.0177(7) 0.0021(6) 0.0044(6) -0.0024(6)
C11 0.0218(8) 0.0204(8) 0.0189(8) -0.0022(6) 0.0045(6) -0.0033(6)
C12 0.0211(8) 0.0266(9) 0.0198(8) -0.0023(7) -0.0008(6) -0.0058(7)
C13 0.0137(7) 0.0265(9) 0.0253(8) 0.0020(7) 0.0021(6) -0.0030(6)
C14 0.0166(7) 0.0222(8) 0.0192(8) 0.0018(6) 0.0051(6) -0.0020(6)
C15 0.0155(7) 0.0166(7) 0.0148(7) 0.0026(6) 0.0024(6) -0.0029(6)
C16 0.0119(7) 0.0197(8) 0.0147(7) 0.0002(6) 0.0035(6) -0.0011(6)
C17 0.0156(7) 0.0145(7) 0.0167(7) -0.0016(6) 0.0073(6) -0.0006(6)
C18 0.0186(7) 0.0147(7) 0.0157(7) -0.0013(6) 0.0058(6) 0.0000(6)
C19 0.0184(7) 0.0192(8) 0.0189(8) -0.0020(6) 0.0077(6) -0.0017(6)
C20 0.0250(8) 0.0201(8) 0.0195(8) -0.0014(6) 0.0123(6) -0.0025(6)
C21 0.0287(9) 0.0206(8) 0.0145(7) 0.0005(6) 0.0084(6) -0.0002(7)
C22 0.0206(8) 0.0192(8) 0.0156(7) -0.0005(6) 0.0043(6) 0.0007(6)
C23 0.0184(7) 0.0138(7) 0.0171(7) -0.0023(6) 0.0079(6) -0.0007(6)
C24 0.0179(7) 0.0131(7) 0.0146(7) -0.0007(6) 0.0053(6) 0.0016(6)
C25 0.0132(7) 0.0148(7) 0.0167(7) -0.0006(6) 0.0034(6) 0.0031(6)
C26 0.0137(7) 0.0158(7) 0.0196(8) -0.0012(6) 0.0051(6) 0.0019(6)
C27 0.0164(7) 0.0208(8) 0.0184(8) -0.0001(6) 0.0030(6) 0.0025(6)
C28 0.0169(8) 0.0244(8) 0.0202(8) -0.0034(6) 0.0002(6) 0.0006(6)
C29 0.0141(7) 0.0205(8) 0.0286(9) -0.0032(7) 0.0048(6) -0.0017(6)
C30 0.0159(7) 0.0177(7) 0.0226(8) -0.0003(6) 0.0065(6) 0.0008(6)
C31 0.0126(7) 0.0170(7) 0.0180(7) -0.0018(6) 0.0036(6) 0.0032(6)
C32 0.0124(7) 0.0167(7) 0.0176(7) -0.0001(6) 0.0054(6) -0.0003(6)
C33 0.0147(7) 0.0211(8) 0.0092(7) -0.0001(5) 0.0039(5) 0.0021(6)
C34 0.0158(7) 0.0195(8) 0.0100(7) -0.0004(6) 0.0038(5) -0.0003(6)
C35 0.0156(7) 0.0221(8) 0.0147(7) 0.0006(6) 0.0047(6) 0.0023(6)
C36 0.0215(8) 0.0217(8) 0.0208(8) 0.0025(6) 0.0074(6) 0.0064(6)
C37 0.0257(8) 0.0179(8) 0.0262(9) 0.0029(7) 0.0100(7) -0.0005(6)
C38 0.0176(7) 0.0200(8) 0.0202(8) -0.0001(6) 0.0074(6) -0.0015(6)
C39 0.0154(7) 0.0201(8) 0.0116(7) 0.0003(6) 0.0046(6) 0.0015(6)
C40 0.0161(7) 0.0170(7) 0.0101(7) -0.0005(5) 0.0040(5) -0.0006(6)
C41 0.0288(11) 0.0172(10) 0.0314(11) 0.0001(9) 0.0165(9) -0.0029(8)
C42 0.0319(10) 0.0318(10) 0.0272(9) 0.0003(7) 0.0131(8) -0.0029(8)
C43 0.0285(10) 0.0539(14) 0.0614(15) -0.0316(12) 0.0040(10) 0.0019(10)
O4 0.024(3) 0.032(4) 0.022(3) -0.003(3) 0.008(3) 0.003(3)
C44 0.040(6) 0.026(5) 0.038(6) -0.004(4) 0.013(5) 0.007(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe N10 1.8656(13) . yes
Fe N3 1.8700(13) . yes
Fe N7 1.8728(13) . yes
Fe N5 1.9032(13) . yes
Fe N1 1.9060(13) . yes
Fe O1 1.9999(11) . yes
N1 C8 1.358(2) . ?
N1 C1 1.4090(19) . ?
N2 C8 1.325(2) . ?
N2 C9 1.364(2) . ?
N3 C9 1.313(2) . ?
N3 C16 1.4708(19) . ?
N4 C17 1.284(2) . ?
N4 C16 1.4664(19) . ?
N5 C24 1.3570(19) . ?
N5 C17 1.4051(19) . ?
N6 C24 1.323(2) . ?
N6 C25 1.364(2) . ?
N7 C25 1.3141(19) . ?
N7 C32 1.4719(19) . ?
N8 C1 1.286(2) . ?
N8 C32 1.4643(19) . ?
N9 C33 1.293(2) . ?
N9 C16 1.485(2) . ?
N10 C40 1.374(2) . ?
N10 C33 1.3850(19) . ?
N11 C40 1.2978(19) . ?
N11 C32 1.4822(19) . ?
O1 C41 1.441(2) . ?
O1 H1A 0.8400(11) . ?
O1 H1B 0.8400(11) . ?
O2 C42 1.422(2) . ?
O2 H2 0.8400 . ?
O3 C43 1.403(3) . ?
O3 H3 0.8400 . ?
C1 C2 1.477(2) . ?
C2 C3 1.385(2) . ?
C2 C7 1.395(2) . ?
C3 C4 1.394(2) . ?
C3 H3A 0.9500 . ?
C4 C5 1.392(3) . ?
C4 H4A 0.9500 . ?
C5 C6 1.394(2) . ?
C5 H5A 0.9500 . ?
C6 C7 1.384(2) . ?
C6 H6A 0.9500 . ?
C7 C8 1.478(2) . ?
C9 C10 1.475(2) . ?
C10 C11 1.389(2) . ?
C10 C15 1.389(2) . ?
C11 C12 1.392(2) . ?
C11 H11A 0.9500 . ?
C12 C13 1.387(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.399(2) . ?
C13 H13A 0.9500 . ?
C14 C15 1.385(2) . ?
C14 H14A 0.9500 . ?
C15 C16 1.526(2) . ?
C17 C18 1.484(2) . ?
C18 C19 1.385(2) . ?
C18 C23 1.395(2) . ?
C19 C20 1.396(2) . ?
C19 H19A 0.9500 . ?
C20 C21 1.393(2) . ?
C20 H20A 0.9500 . ?
C21 C22 1.395(2) . ?
C21 H21A 0.9500 . ?
C22 C23 1.383(2) . ?
C22 H22A 0.9500 . ?
C23 C24 1.477(2) . ?
C25 C26 1.472(2) . ?
C26 C27 1.388(2) . ?
C26 C31 1.391(2) . ?
C27 C28 1.393(2) . ?
C27 H27A 0.9500 . ?
C28 C29 1.393(2) . ?
C28 H28A 0.9500 . ?
C29 C30 1.396(2) . ?
C29 H29A 0.9500 . ?
C30 C31 1.383(2) . ?
C30 H30A 0.9500 . ?
C31 C32 1.526(2) . ?
C33 C34 1.483(2) . ?
C34 C35 1.385(2) . ?
C34 C39 1.402(2) . ?
C35 C36 1.394(2) . ?
C35 H35A 0.9500 . ?
C36 C37 1.393(2) . ?
C36 H36A 0.9500 . ?
C37 C38 1.395(2) . ?
C37 H37A 0.9500 . ?
C38 C39 1.384(2) . ?
C38 H38A 0.9500 . ?
C39 C40 1.484(2) . ?
C41 H1B 0.72(6) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
O4 C44 1.427(11) . ?
O4 H4B 0.8400 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
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_3
_geom_angle_publ_flag
N10 Fe N3 86.72(6) . . yes
N10 Fe N7 86.76(5) . . yes
N3 Fe N7 173.48(6) . . yes
N10 Fe N5 92.88(5) . . yes
N3 Fe N5 90.62(5) . . yes
N7 Fe N5 89.66(5) . . yes
N10 Fe N1 92.58(5) . . yes
N3 Fe N1 89.78(5) . . yes
N7 Fe N1 90.56(5) . . yes
N5 Fe N1 174.54(6) . . yes
N10 Fe O1 177.73(5) . . yes
N3 Fe O1 92.84(5) . . yes
N7 Fe O1 93.68(5) . . yes
N5 Fe O1 89.35(5) . . yes
N1 Fe O1 85.19(5) . . yes
C8 N1 C1 109.72(13) . . ?
C8 N1 Fe 123.45(10) . . ?
C1 N1 Fe 124.84(10) . . ?
C8 N2 C9 118.20(13) . . ?
C9 N3 C16 111.78(12) . . ?
C9 N3 Fe 127.54(11) . . ?
C16 N3 Fe 118.91(10) . . ?
C17 N4 C16 118.16(13) . . ?
C24 N5 C17 109.97(12) . . ?
C24 N5 Fe 123.01(10) . . ?
C17 N5 Fe 125.06(10) . . ?
C24 N6 C25 117.83(13) . . ?
C25 N7 C32 111.58(12) . . ?
C25 N7 Fe 127.61(11) . . ?
C32 N7 Fe 118.72(10) . . ?
C1 N8 C32 117.44(13) . . ?
C33 N9 C16 120.35(13) . . ?
C40 N10 C33 111.16(13) . . ?
C40 N10 Fe 124.22(10) . . ?
C33 N10 Fe 124.54(11) . . ?
C40 N11 C32 121.00(13) . . ?
C41 O1 Fe 127.39(11) . . ?
C41 O1 H1A 106.9(13) . . ?
Fe O1 H1A 114.0(13) . . ?
C41 O1 H1B 21(6) . . ?
Fe O1 H1B 107(6) . . ?
H1A O1 H1B 119.4(6) . . ?
C42 O2 H2 109.5 . . ?
C43 O3 H3 109.5 . . ?
N8 C1 N1 128.15(14) . . ?
N8 C1 C2 124.49(14) . . ?
N1 C1 C2 107.33(13) . . ?
C3 C2 C7 121.59(15) . . ?
C3 C2 C1 131.38(15) . . ?
C7 C2 C1 107.02(13) . . ?
C2 C3 C4 117.28(15) . . ?
C2 C3 H3A 121.4 . . ?
C4 C3 H3A 121.4 . . ?
C5 C4 C3 121.13(15) . . ?
C5 C4 H4A 119.4 . . ?
C3 C4 H4A 119.4 . . ?
C4 C5 C6 121.35(15) . . ?
C4 C5 H5A 119.3 . . ?
C6 C5 H5A 119.3 . . ?
C7 C6 C5 117.42(15) . . ?
C7 C6 H6A 121.3 . . ?
C5 C6 H6A 121.3 . . ?
C6 C7 C2 121.22(15) . . ?
C6 C7 C8 131.66(15) . . ?
C2 C7 C8 107.12(13) . . ?
N2 C8 N1 128.59(14) . . ?
N2 C8 C7 122.65(14) . . ?
N1 C8 C7 108.75(13) . . ?
N3 C9 N2 127.37(14) . . ?
N3 C9 C10 109.46(13) . . ?
N2 C9 C10 123.14(13) . . ?
C11 C10 C15 121.72(15) . . ?
C11 C10 C9 131.24(15) . . ?
C15 C10 C9 107.03(13) . . ?
C10 C11 C12 117.33(15) . . ?
C10 C11 H11A 121.3 . . ?
C12 C11 H11A 121.3 . . ?
C13 C12 C11 121.15(15) . . ?
C13 C12 H12A 119.4 . . ?
C11 C12 H12A 119.4 . . ?
C12 C13 C14 121.28(15) . . ?
C12 C13 H13A 119.4 . . ?
C14 C13 H13A 119.4 . . ?
C15 C14 C13 117.47(15) . . ?
C15 C14 H14A 121.3 . . ?
C13 C14 H14A 121.3 . . ?
C14 C15 C10 121.00(14) . . ?
C14 C15 C16 130.46(14) . . ?
C10 C15 C16 108.53(13) . . ?
N4 C16 N3 114.39(12) . . ?
N4 C16 N9 109.15(12) . . ?
N3 C16 N9 110.99(12) . . ?
N4 C16 C15 112.23(12) . . ?
N3 C16 C15 101.92(12) . . ?
N9 C16 C15 107.84(12) . . ?
N4 C17 N5 128.02(14) . . ?
N4 C17 C18 124.70(14) . . ?
N5 C17 C18 107.28(12) . . ?
C19 C18 C23 120.94(14) . . ?
C19 C18 C17 132.34(14) . . ?
C23 C18 C17 106.72(13) . . ?
C18 C19 C20 117.75(15) . . ?
C18 C19 H19A 121.1 . . ?
C20 C19 H19A 121.1 . . ?
C21 C20 C19 121.08(15) . . ?
C21 C20 H20A 119.5 . . ?
C19 C20 H20A 119.5 . . ?
C20 C21 C22 121.04(15) . . ?
C20 C21 H21A 119.5 . . ?
C22 C21 H21A 119.5 . . ?
C23 C22 C21 117.50(15) . . ?
C23 C22 H22A 121.2 . . ?
C21 C22 H22A 121.2 . . ?
C22 C23 C18 121.65(14) . . ?
C22 C23 C24 131.03(14) . . ?
C18 C23 C24 107.32(13) . . ?
N6 C24 N5 128.82(14) . . ?
N6 C24 C23 122.54(13) . . ?
N5 C24 C23 108.62(13) . . ?
N7 C25 N6 126.92(14) . . ?
N7 C25 C26 109.88(13) . . ?
N6 C25 C26 123.19(14) . . ?
C27 C26 C31 121.59(15) . . ?
C27 C26 C25 131.16(15) . . ?
C31 C26 C25 107.18(13) . . ?
C26 C27 C28 117.40(15) . . ?
C26 C27 H27A 121.3 . . ?
C28 C27 H27A 121.3 . . ?
C27 C28 C29 121.08(15) . . ?
C27 C28 H28A 119.5 . . ?
C29 C28 H28A 119.5 . . ?
C28 C29 C30 121.13(15) . . ?
C28 C29 H29A 119.4 . . ?
C30 C29 H29A 119.4 . . ?
C31 C30 C29 117.66(15) . . ?
C31 C30 H30A 121.2 . . ?
C29 C30 H30A 121.2 . . ?
C30 C31 C26 121.13(14) . . ?
C30 C31 C32 130.40(14) . . ?
C26 C31 C32 108.28(13) . . ?
N8 C32 N7 114.07(12) . . ?
N8 C32 N11 108.67(12) . . ?
N7 C32 N11 111.32(12) . . ?
N8 C32 C31 113.05(12) . . ?
N7 C32 C31 102.23(12) . . ?
N11 C32 C31 107.23(12) . . ?
N9 C33 N10 129.34(15) . . ?
N9 C33 C34 123.70(14) . . ?
N10 C33 C34 106.89(13) . . ?
C35 C34 C39 121.26(14) . . ?
C35 C34 C33 131.22(14) . . ?
C39 C34 C33 107.48(13) . . ?
C34 C35 C36 117.42(14) . . ?
C34 C35 H35A 121.3 . . ?
C36 C35 H35A 121.3 . . ?
C37 C36 C35 121.25(15) . . ?
C37 C36 H36A 119.4 . . ?
C35 C36 H36A 119.4 . . ?
C36 C37 C38 121.33(15) . . ?
C36 C37 H37A 119.3 . . ?
C38 C37 H37A 119.3 . . ?
C39 C38 C37 117.34(14) . . ?
C39 C38 H38A 121.3 . . ?
C37 C38 H38A 121.3 . . ?
C38 C39 C34 121.37(14) . . ?
C38 C39 C40 131.90(14) . . ?
C34 C39 C40 106.73(13) . . ?
N11 C40 N10 129.16(14) . . ?
N11 C40 C39 123.19(14) . . ?
N10 C40 C39 107.64(12) . . ?
O1 C41 H1B 24(5) . . ?
C44 O4 H4B 109.5 . . ?
O4 C44 H44A 109.5 . . ?
O4 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O4 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
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
N10 Fe N1 C8 -109.05(12) . . . . ?
N3 Fe N1 C8 -22.34(12) . . . . ?
N7 Fe N1 C8 164.18(12) . . . . ?
N5 Fe N1 C8 71.9(6) . . . . ?
O1 Fe N1 C8 70.53(12) . . . . ?
N10 Fe N1 C1 88.68(12) . . . . ?
N3 Fe N1 C1 175.38(12) . . . . ?
N7 Fe N1 C1 1.90(12) . . . . ?
N5 Fe N1 C1 -90.3(6) . . . . ?
O1 Fe N1 C1 -91.75(12) . . . . ?
N10 Fe N3 C9 107.15(14) . . . . ?
N7 Fe N3 C9 107.6(5) . . . . ?
N5 Fe N3 C9 -160.00(14) . . . . ?
N1 Fe N3 C9 14.55(14) . . . . ?
O1 Fe N3 C9 -70.62(13) . . . . ?
N10 Fe N3 C16 -56.35(11) . . . . ?
N7 Fe N3 C16 -55.9(5) . . . . ?
N5 Fe N3 C16 36.50(11) . . . . ?
N1 Fe N3 C16 -148.95(11) . . . . ?
O1 Fe N3 C16 125.88(11) . . . . ?
N10 Fe N5 C24 -110.55(12) . . . . ?
N3 Fe N5 C24 162.70(12) . . . . ?
N7 Fe N5 C24 -23.82(12) . . . . ?
N1 Fe N5 C24 68.5(6) . . . . ?
O1 Fe N5 C24 69.87(12) . . . . ?
N10 Fe N5 C17 87.01(12) . . . . ?
N3 Fe N5 C17 0.27(12) . . . . ?
N7 Fe N5 C17 173.75(12) . . . . ?
N1 Fe N5 C17 -94.0(6) . . . . ?
O1 Fe N5 C17 -92.57(12) . . . . ?
N10 Fe N7 C25 105.26(13) . . . . ?
N3 Fe N7 C25 104.8(5) . . . . ?
N5 Fe N7 C25 12.35(13) . . . . ?
N1 Fe N7 C25 -162.19(13) . . . . ?
O1 Fe N7 C25 -76.97(13) . . . . ?
N10 Fe N7 C32 -56.83(11) . . . . ?
N3 Fe N7 C32 -57.3(5) . . . . ?
N5 Fe N7 C32 -149.73(11) . . . . ?
N1 Fe N7 C32 35.72(11) . . . . ?
O1 Fe N7 C32 120.94(10) . . . . ?
N3 Fe N10 C40 -150.25(12) . . . . ?
N7 Fe N10 C40 29.80(12) . . . . ?
N5 Fe N10 C40 119.29(12) . . . . ?
N1 Fe N10 C40 -60.61(12) . . . . ?
N3 Fe N10 C33 26.22(12) . . . . ?
N7 Fe N10 C33 -153.73(12) . . . . ?
N5 Fe N10 C33 -64.24(12) . . . . ?
N1 Fe N10 C33 115.85(12) . . . . ?
N3 Fe O1 C41 -66.99(14) . . . . ?
N7 Fe O1 C41 113.21(14) . . . . ?
N5 Fe O1 C41 23.60(14) . . . . ?
N1 Fe O1 C41 -156.54(15) . . . . ?
C32 N8 C1 N1 -2.7(2) . . . . ?
C32 N8 C1 C2 175.07(14) . . . . ?
C8 N1 C1 N8 176.21(15) . . . . ?
Fe N1 C1 N8 -19.4(2) . . . . ?
C8 N1 C1 C2 -1.90(16) . . . . ?
Fe N1 C1 C2 162.44(10) . . . . ?
N8 C1 C2 C3 2.8(3) . . . . ?
N1 C1 C2 C3 -179.00(16) . . . . ?
N8 C1 C2 C7 -175.61(15) . . . . ?
N1 C1 C2 C7 2.58(17) . . . . ?
C7 C2 C3 C4 -0.3(2) . . . . ?
C1 C2 C3 C4 -178.54(16) . . . . ?
C2 C3 C4 C5 0.6(2) . . . . ?
C3 C4 C5 C6 0.1(3) . . . . ?
C4 C5 C6 C7 -1.0(2) . . . . ?
C5 C6 C7 C2 1.3(2) . . . . ?
C5 C6 C7 C8 -178.46(16) . . . . ?
C3 C2 C7 C6 -0.7(2) . . . . ?
C1 C2 C7 C6 177.95(14) . . . . ?
C3 C2 C7 C8 179.16(14) . . . . ?
C1 C2 C7 C8 -2.23(17) . . . . ?
C9 N2 C8 N1 5.1(2) . . . . ?
C9 N2 C8 C7 -173.66(14) . . . . ?
C1 N1 C8 N2 -178.37(15) . . . . ?
Fe N1 C8 N2 17.0(2) . . . . ?
C1 N1 C8 C7 0.53(17) . . . . ?
Fe N1 C8 C7 -164.08(10) . . . . ?
C6 C7 C8 N2 -0.1(3) . . . . ?
C2 C7 C8 N2 -179.89(14) . . . . ?
C6 C7 C8 N1 -179.07(16) . . . . ?
C2 C7 C8 N1 1.13(17) . . . . ?
C16 N3 C9 N2 165.98(15) . . . . ?
Fe N3 C9 N2 1.5(2) . . . . ?
C16 N3 C9 C10 -11.90(17) . . . . ?
Fe N3 C9 C10 -176.37(10) . . . . ?
C8 N2 C9 N3 -15.3(2) . . . . ?
C8 N2 C9 C10 162.28(14) . . . . ?
N3 C9 C10 C11 -172.77(16) . . . . ?
N2 C9 C10 C11 9.2(3) . . . . ?
N3 C9 C10 C15 7.82(17) . . . . ?
N2 C9 C10 C15 -170.17(14) . . . . ?
C15 C10 C11 C12 -0.3(2) . . . . ?
C9 C10 C11 C12 -179.60(16) . . . . ?
C10 C11 C12 C13 1.6(3) . . . . ?
C11 C12 C13 C14 -0.9(3) . . . . ?
C12 C13 C14 C15 -1.2(2) . . . . ?
C13 C14 C15 C10 2.4(2) . . . . ?
C13 C14 C15 C16 -179.45(15) . . . . ?
C11 C10 C15 C14 -1.8(2) . . . . ?
C9 C10 C15 C14 177.70(14) . . . . ?
C11 C10 C15 C16 179.73(14) . . . . ?
C9 C10 C15 C16 -0.79(17) . . . . ?
C17 N4 C16 N3 41.19(19) . . . . ?
C17 N4 C16 N9 -83.84(16) . . . . ?
C17 N4 C16 C15 156.68(14) . . . . ?
C9 N3 C16 N4 132.15(13) . . . . ?
Fe N3 C16 N4 -61.89(15) . . . . ?
C9 N3 C16 N9 -103.81(14) . . . . ?
Fe N3 C16 N9 62.16(14) . . . . ?
C9 N3 C16 C15 10.79(16) . . . . ?
Fe N3 C16 C15 176.76(9) . . . . ?
C33 N9 C16 N4 102.88(15) . . . . ?
C33 N9 C16 N3 -24.10(18) . . . . ?
C33 N9 C16 C15 -134.95(14) . . . . ?
C14 C15 C16 N4 53.4(2) . . . . ?
C10 C15 C16 N4 -128.35(14) . . . . ?
C14 C15 C16 N3 176.19(16) . . . . ?
C10 C15 C16 N3 -5.52(16) . . . . ?
C14 C15 C16 N9 -66.9(2) . . . . ?
C10 C15 C16 N9 111.39(14) . . . . ?
C16 N4 C17 N5 -0.9(2) . . . . ?
C16 N4 C17 C18 178.63(14) . . . . ?
C24 N5 C17 N4 176.81(15) . . . . ?
Fe N5 C17 N4 -18.8(2) . . . . ?
C24 N5 C17 C18 -2.78(16) . . . . ?
Fe N5 C17 C18 161.60(10) . . . . ?
N4 C17 C18 C19 1.0(3) . . . . ?
N5 C17 C18 C19 -179.40(16) . . . . ?
N4 C17 C18 C23 -178.46(15) . . . . ?
N5 C17 C18 C23 1.15(16) . . . . ?
C23 C18 C19 C20 -1.9(2) . . . . ?
C17 C18 C19 C20 178.69(16) . . . . ?
C18 C19 C20 C21 0.7(2) . . . . ?
C19 C20 C21 C22 1.0(2) . . . . ?
C20 C21 C22 C23 -1.5(2) . . . . ?
C21 C22 C23 C18 0.3(2) . . . . ?
C21 C22 C23 C24 -179.42(15) . . . . ?
C19 C18 C23 C22 1.4(2) . . . . ?
C17 C18 C23 C22 -179.05(14) . . . . ?
C19 C18 C23 C24 -178.78(14) . . . . ?
C17 C18 C23 C24 0.75(16) . . . . ?
C25 N6 C24 N5 4.4(2) . . . . ?
C25 N6 C24 C23 -173.71(14) . . . . ?
C17 N5 C24 N6 -175.05(15) . . . . ?
Fe N5 C24 N6 20.2(2) . . . . ?
C17 N5 C24 C23 3.27(17) . . . . ?
Fe N5 C24 C23 -161.49(10) . . . . ?
C22 C23 C24 N6 -4.3(3) . . . . ?
C18 C23 C24 N6 175.96(14) . . . . ?
C22 C23 C24 N5 177.28(16) . . . . ?
C18 C23 C24 N5 -2.49(17) . . . . ?
C32 N7 C25 N6 169.87(14) . . . . ?
Fe N7 C25 N6 6.7(2) . . . . ?
C32 N7 C25 C26 -8.73(17) . . . . ?
Fe N7 C25 C26 -171.87(10) . . . . ?
C24 N6 C25 N7 -19.0(2) . . . . ?
C24 N6 C25 C26 159.41(14) . . . . ?
N7 C25 C26 C27 -179.17(16) . . . . ?
N6 C25 C26 C27 2.2(3) . . . . ?
N7 C25 C26 C31 3.95(17) . . . . ?
N6 C25 C26 C31 -174.72(14) . . . . ?
C31 C26 C27 C28 -0.8(2) . . . . ?
C25 C26 C27 C28 -177.35(15) . . . . ?
C26 C27 C28 C29 0.4(2) . . . . ?
C27 C28 C29 C30 0.5(3) . . . . ?
C28 C29 C30 C31 -1.0(2) . . . . ?
C29 C30 C31 C26 0.5(2) . . . . ?
C29 C30 C31 C32 174.85(15) . . . . ?
C27 C26 C31 C30 0.4(2) . . . . ?
C25 C26 C31 C30 177.63(14) . . . . ?
C27 C26 C31 C32 -175.05(14) . . . . ?
C25 C26 C31 C32 2.19(16) . . . . ?
C1 N8 C32 N7 43.99(18) . . . . ?
C1 N8 C32 N11 -80.85(16) . . . . ?
C1 N8 C32 C31 160.23(13) . . . . ?
C25 N7 C32 N8 131.91(13) . . . . ?
Fe N7 C32 N8 -63.28(14) . . . . ?
C25 N7 C32 N11 -104.67(14) . . . . ?
Fe N7 C32 N11 60.13(14) . . . . ?
C25 N7 C32 C31 9.53(16) . . . . ?
Fe N7 C32 C31 174.34(9) . . . . ?
C40 N11 C32 N8 103.92(15) . . . . ?
C40 N11 C32 N7 -22.53(19) . . . . ?
C40 N11 C32 C31 -133.57(14) . . . . ?
C30 C31 C32 N8 55.3(2) . . . . ?
C26 C31 C32 N8 -129.83(14) . . . . ?
C30 C31 C32 N7 178.38(15) . . . . ?
C26 C31 C32 N7 -6.75(15) . . . . ?
C30 C31 C32 N11 -64.4(2) . . . . ?
C26 C31 C32 N11 110.42(14) . . . . ?
C16 N9 C33 N10 -5.7(2) . . . . ?
C16 N9 C33 C34 170.76(13) . . . . ?
C40 N10 C33 N9 176.10(14) . . . . ?
Fe N10 C33 N9 -0.8(2) . . . . ?
C40 N10 C33 C34 -0.81(16) . . . . ?
Fe N10 C33 C34 -177.68(9) . . . . ?
N9 C33 C34 C35 3.0(3) . . . . ?
N10 C33 C34 C35 -179.89(15) . . . . ?
N9 C33 C34 C39 -174.50(14) . . . . ?
N10 C33 C34 C39 2.63(16) . . . . ?
C39 C34 C35 C36 1.6(2) . . . . ?
C33 C34 C35 C36 -175.59(15) . . . . ?
C34 C35 C36 C37 -1.6(2) . . . . ?
C35 C36 C37 C38 0.2(3) . . . . ?
C36 C37 C38 C39 1.2(2) . . . . ?
C37 C38 C39 C34 -1.2(2) . . . . ?
C37 C38 C39 C40 179.92(15) . . . . ?
C35 C34 C39 C38 -0.2(2) . . . . ?
C33 C34 C39 C38 177.56(14) . . . . ?
C35 C34 C39 C40 178.92(13) . . . . ?
C33 C34 C39 C40 -3.29(16) . . . . ?
C32 N11 C40 N10 -4.2(2) . . . . ?
C32 N11 C40 C39 174.48(13) . . . . ?
C33 N10 C40 N11 177.59(15) . . . . ?
Fe N10 C40 N11 -5.5(2) . . . . ?
C33 N10 C40 C39 -1.22(16) . . . . ?
Fe N10 C40 C39 175.66(9) . . . . ?
C38 C39 C40 N11 3.0(3) . . . . ?
C34 C39 C40 N11 -176.04(14) . . . . ?
C38 C39 C40 N10 -178.11(16) . . . . ?
C34 C39 C40 N10 2.86(16) . . . . ?
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
O2 H2 N11 0.84 1.87 2.6986(17) 169.0 .
O3 H3 N9 0.84 2.00 2.8374(19) 174.2 .
O1 H1A O2 0.8400(11) 1.724(2) 2.5634(15) 177.3(19) 2_646
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 26.38
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.397
_refine_diff_density_min -0.350
_refine_diff_density_rms 0.055
# File processed with modiCIFer Dec. 16,2005. I.A.Guzei, UW-Madison.
#===END
data_mcgaff20
_database_code_depnum_ccdc_archive 'CCDC 606959'
_publ_section_references
;
Allen, F.H. (2002). Acta Cryst. B58, 380-388.
Bruker-AXS. (2000-2003) SADABS V.2.05, SAINT V.6.22, SHELXTL V.6.10
& SMART 5.622 Software Reference Manuals.
Bruker-AXS, Madison, Wisconsin, USA.
Bruno, I. J., Cole, J. C., Edgington, P. R., Kessler, M.,
Macrae, C. F., McCabe, P., Pearson, J,
& Taylor, R. (2002). Acta Cryst. B58, 389-397.
Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367.
Frisch, M. J., Trucks, G. W.,
Schlegel, H. B., Scuseria, G. E., Robb, M. A., Cheeseman,
J. R., Montgomery, Jr., J. A., Vreven, T., Kudin, K. N., Burant,
J. C., Millam, J. M., Iyengar, S. S., Tomasi, J., Barone, V.,
Mennucci, B., Cossi, M., Scalmani, G., Rega, N., Petersson,
G. A., Nakatsuji, H., Hada, M., Ehara, M., Toyota, K., Fukuda,
R., Hasegawa, J., Ishida, M., Nakajima, T., Honda, Y., Kitao,
O., Nakai, H., Klene, M., Li, X., Knox, J. E., Hratchian, H. P.,
Cross, J. B., Bakken, V., Adamo, C., Jaramillo, J., Gomperts, R.,
Stratmann, R. E., Yazyev, O., Austin, A. J., Cammi, R., Pomelli,
C., Ochterski, J. W., Ayala, P. Y., Morokuma, K., Voth, G. A.,
Salvador, P., Dannenberg, J. J., Zakrzewski, V. G., Dapprich, S.,
Daniels, A. D., Strain, M. C., Farkas, O., Malick, D. K., Rabuck,
A. D., Raghavachari, K., Foresman, J. B., Ortiz, J. V., Cui, Q.,
Baboul, A. G., Clifford, S., Cioslowski, J., Stefanov, B. B.,
Liu, G., Liashenko, A., Piskorz, P., Komaromi, I., Martin, R.
L., Fox, D. J., Keith, T., Al-Laham, M. A., Peng, C. Y.,
Nanayakkara, A., Challacombe, M., Gill, P. M. W., Johnson,
B., Chen, W., Wong, M. W., Gonzalez, C., & Pople, J. A.,
Gaussian 03, Revision C.02,
Gaussian, Inc., Wallingford CT, (2004).
;
_publ_section_acknowledgements
;
We thank the National Science Foundation for financial support.
;
_publ_section_figure_captions
;
Figure 1. Molecular structure of 1. The thermal ellipsoids are
shown at 50% probability level.
;
_publ_section_exptl_prep
;
;
_publ_section_exptl_refinement
;
All H-atoms bound to carbon were placed in idealized locations and
refined as riding with
d(C-H) = 0.95\%A, U~iso~(H) = 1.2U~eq~(C)
for aromatic carbon atoms,
d(C-H) = 0.98\%A, U~iso~(H) = 1.5U~eq~(C)
for methyl groups,
d(O-H) = 0.84\%A, U~iso~(H) = 1.5U~eq~(O)
for H atoms on O3,
and d(O-H) = 0.82\%A, U~iso~
independently refined for H atoms attached to atom O4.
;
#3. data
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C51 H37 Fe N12 O4'
_chemical_formula_sum 'C51 H37 Fe N12 O4'
_chemical_formula_weight 937.78
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'C 1 2/c 1 '
_symmetry_space_group_name_Hall '-C 2yc '
_symmetry_int_tables_number 15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'
_cell_length_a 22.597(2)
_cell_length_b 21.775(2)
_cell_length_c 19.6275(18)
_cell_angle_alpha 90.00
_cell_angle_beta 107.0650(10)
_cell_angle_gamma 90.00
_cell_volume 9232.4(15)
_cell_formula_units_Z 8
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 17927
_cell_measurement_theta_min 2.1708
_cell_measurement_theta_max 26.3805
_exptl_crystal_description needle
_exptl_crystal_colour red
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.35
_exptl_crystal_size_min 0.31
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.349
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3880
_exptl_absorpt_coefficient_mu 0.387
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker-AXS, 2003)
;
_exptl_absorpt_correction_T_min 0.8733
_exptl_absorpt_correction_T_max 0.8895
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type Mo-K\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker CCD-1000 area detector'
_diffrn_measurement_method '0.30\% \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 47453
_diffrn_reflns_av_R_equivalents 0.0338
_diffrn_reflns_av_sigmaI/netI 0.0267
_diffrn_reflns_limit_h_min -28
_diffrn_reflns_limit_h_max 28
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 1.53
_diffrn_reflns_theta_max 26.44
_reflns_number_total 9488
_reflns_number_gt 7928
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_cell_refinement 'SAINT Ver. 6.22 (Bruker-AXS, 2003)'
_computing_data_reduction 'SAINT Ver. 6.22'
_computing_structure_solution 'SHELXTL Ver. 6.10 (Bruker-AXS, 2003)'
_computing_structure_refinement 'SHELXTL Ver. 6.10 '
_computing_molecular_graphics 'SHELXTL Ver. 6.10 '
_computing_publication_material 'SHELXTL Ver. 6.10 '
_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^)+(0.0610P)^2^+1.5766P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9488
_refine_ls_number_parameters 533
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0422
_refine_ls_R_factor_gt 0.0355
_refine_ls_wR_factor_ref 0.0996
_refine_ls_wR_factor_gt 0.0966
_refine_ls_goodness_of_fit_ref 1.088
_refine_ls_restrained_S_all 1.088
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.743570(9) 0.066629(9) 0.063306(10) 0.01978(7) Uani 1 1 d . . .
O1 O 0.82806(6) -0.11443(5) -0.12978(6) 0.0332(3) Uani 1 1 d . . .
H1 H 0.8134 -0.1046 -0.1728 0.050 Uiso 1 1 calc R . .
N1 N 0.66840(6) 0.02058(6) 0.04131(7) 0.0237(3) Uani 1 1 d . . .
N2 N 0.70431(7) -0.06644(6) 0.11851(8) 0.0315(3) Uani 1 1 d . . .
N3 N 0.77516(6) 0.01779(6) 0.14427(6) 0.0231(3) Uani 1 1 d . . .
N4 N 0.87757(6) 0.06624(6) 0.19561(6) 0.0237(3) Uani 1 1 d . . .
N5 N 0.82082(5) 0.10840(5) 0.08160(6) 0.0201(2) Uani 1 1 d . . .
N6 N 0.79939(5) 0.16998(5) -0.02516(6) 0.0200(2) Uani 1 1 d . . .
N7 N 0.70840(5) 0.12275(5) -0.00922(6) 0.0200(2) Uani 1 1 d . . .
N8 N 0.60008(6) 0.08507(6) -0.04807(7) 0.0239(3) Uani 1 1 d . . .
N9 N 0.78834(6) 0.09568(6) 0.23427(7) 0.0259(3) Uani 1 1 d . . .
N10 N 0.71551(6) 0.12048(5) 0.12279(6) 0.0222(3) Uani 1 1 d . . .
N11 N 0.62793(6) 0.16763(5) 0.03505(7) 0.0236(3) Uani 1 1 d . . .
N12 N 0.77232(6) 0.00923(6) -0.00092(6) 0.0219(3) Uani 1 1 d . . .
C1 C 0.61496(7) 0.03439(7) -0.01433(8) 0.0242(3) Uani 1 1 d . . .
C2 C 0.57547(7) -0.02146(7) -0.02785(8) 0.0269(3) Uani 1 1 d . . .
C3 C 0.51760(7) -0.03262(8) -0.07488(9) 0.0296(3) Uani 1 1 d . . .
H3 H 0.4966 -0.0023 -0.1080 0.036 Uiso 1 1 calc R . .
C4 C 0.49134(8) -0.09008(8) -0.07180(10) 0.0357(4) Uani 1 1 d . . .
H4 H 0.4517 -0.0992 -0.1035 0.043 Uiso 1 1 calc R . .
C5 C 0.52213(9) -0.13409(8) -0.02316(11) 0.0434(5) Uani 1 1 d . . .
H5 H 0.5031 -0.1728 -0.0222 0.052 Uiso 1 1 calc R . .
C6 C 0.58037(9) -0.12280(8) 0.02435(11) 0.0415(4) Uani 1 1 d . . .
H6 H 0.6014 -0.1531 0.0575 0.050 Uiso 1 1 calc R . .
C7 C 0.60644(8) -0.06549(7) 0.02122(9) 0.0310(4) Uani 1 1 d . . .
C8 C 0.66479(7) -0.03738(7) 0.06452(9) 0.0274(3) Uani 1 1 d . . .
C9 C 0.75324(8) -0.03462(7) 0.15991(8) 0.0276(3) Uani 1 1 d . . .
C10 C 0.78965(8) -0.05469(7) 0.23169(9) 0.0294(3) Uani 1 1 d . . .
C11 C 0.78833(8) -0.10874(8) 0.26880(9) 0.0348(4) Uani 1 1 d . . .
H11 H 0.7595 -0.1404 0.2491 0.042 Uiso 1 1 calc R . .
C12 C 0.83081(9) -0.11460(8) 0.33573(9) 0.0364(4) Uani 1 1 d . . .
H12 H 0.8307 -0.1508 0.3628 0.044 Uiso 1 1 calc R . .
C13 C 0.87344(9) -0.06853(8) 0.36390(9) 0.0359(4) Uani 1 1 d . . .
H13 H 0.9023 -0.0740 0.4096 0.043 Uiso 1 1 calc R . .
C14 C 0.87469(8) -0.01439(8) 0.32640(8) 0.0323(4) Uani 1 1 d . . .
H14 H 0.9040 0.0170 0.3456 0.039 Uiso 1 1 calc R . .
C15 C 0.83173(8) -0.00816(7) 0.26051(8) 0.0280(3) Uani 1 1 d . . .
C16 C 0.81985(7) 0.04467(7) 0.20737(8) 0.0244(3) Uani 1 1 d . . .
C17 C 0.87429(7) 0.09445(7) 0.13722(8) 0.0223(3) Uani 1 1 d . . .
C18 C 0.92800(7) 0.12039(7) 0.11809(7) 0.0227(3) Uani 1 1 d . . .
C19 C 0.99122(7) 0.11874(7) 0.15167(8) 0.0280(3) Uani 1 1 d . . .
H19 H 1.0078 0.0966 0.1948 0.034 Uiso 1 1 calc R . .
C20 C 1.02940(7) 0.15059(8) 0.12002(9) 0.0317(4) Uani 1 1 d . . .
H20 H 1.0729 0.1497 0.1417 0.038 Uiso 1 1 calc R . .
C21 C 1.00544(7) 0.18379(8) 0.05726(9) 0.0306(3) Uani 1 1 d . . .
H21 H 1.0327 0.2057 0.0373 0.037 Uiso 1 1 calc R . .
C22 C 0.94181(7) 0.18512(7) 0.02352(8) 0.0251(3) Uani 1 1 d . . .
H22 H 0.9250 0.2078 -0.0192 0.030 Uiso 1 1 calc R . .
C23 C 0.90415(7) 0.15230(7) 0.05448(7) 0.0217(3) Uani 1 1 d . . .
C24 C 0.83628(6) 0.14432(6) 0.03283(7) 0.0202(3) Uani 1 1 d . . .
C25 C 0.73714(7) 0.16220(6) -0.03908(7) 0.0204(3) Uani 1 1 d . . .
C26 C 0.69140(7) 0.19832(6) -0.09300(7) 0.0214(3) Uani 1 1 d . . .
C27 C 0.69892(7) 0.23698(7) -0.14588(8) 0.0248(3) Uani 1 1 d . . .
H27 H 0.7389 0.2473 -0.1490 0.030 Uiso 1 1 calc R . .
C28 C 0.64547(7) 0.26013(7) -0.19436(8) 0.0286(3) Uani 1 1 d . . .
H28 H 0.6488 0.2866 -0.2316 0.034 Uiso 1 1 calc R . .
C29 C 0.58730(7) 0.24486(7) -0.18867(8) 0.0294(3) Uani 1 1 d . . .
H29 H 0.5515 0.2611 -0.2223 0.035 Uiso 1 1 calc R . .
C30 C 0.58012(7) 0.20629(7) -0.13483(8) 0.0269(3) Uani 1 1 d . . .
H30 H 0.5403 0.1962 -0.1311 0.032 Uiso 1 1 calc R . .
C31 C 0.63322(7) 0.18332(6) -0.08716(8) 0.0227(3) Uani 1 1 d . . .
C32 C 0.64150(6) 0.13762(7) -0.02644(8) 0.0223(3) Uani 1 1 d . . .
C33 C 0.74019(7) 0.12562(7) 0.19389(8) 0.0246(3) Uani 1 1 d . . .
C34 C 0.70346(8) 0.17148(7) 0.22064(8) 0.0287(3) Uani 1 1 d . . .
C35 C 0.71037(9) 0.19620(8) 0.28794(9) 0.0380(4) Uani 1 1 d . . .
H35 H 0.7438 0.1846 0.3279 0.046 Uiso 1 1 calc R . .
C36 C 0.66589(10) 0.23882(9) 0.29410(10) 0.0466(5) Uani 1 1 d . . .
H36 H 0.6698 0.2570 0.3392 0.056 Uiso 1 1 calc R . .
C37 C 0.61661(10) 0.25529(9) 0.23671(10) 0.0435(5) Uani 1 1 d . . .
H37 H 0.5867 0.2836 0.2432 0.052 Uiso 1 1 calc R . .
C38 C 0.61021(8) 0.23082(7) 0.16918(9) 0.0334(4) Uani 1 1 d . . .
H38 H 0.5766 0.2422 0.1293 0.040 Uiso 1 1 calc R . .
C39 C 0.65470(8) 0.18932(7) 0.16226(8) 0.0277(3) Uani 1 1 d . . .
C40 C 0.66303(7) 0.15809(6) 0.09850(8) 0.0236(3) Uani 1 1 d . . .
C41 C 0.73905(7) 0.00100(7) -0.06981(8) 0.0236(3) Uani 1 1 d . . .
H41 H 0.7021 0.0241 -0.0880 0.028 Uiso 1 1 calc R . .
C42 C 0.75585(7) -0.03898(7) -0.11480(8) 0.0259(3) Uani 1 1 d . . .
H42 H 0.7310 -0.0424 -0.1630 0.031 Uiso 1 1 calc R . .
C43 C 0.80975(7) -0.07513(7) -0.09013(8) 0.0260(3) Uani 1 1 d . . .
C44 C 0.84453(7) -0.06581(7) -0.01849(8) 0.0281(3) Uani 1 1 d . . .
H44 H 0.8818 -0.0881 0.0012 0.034 Uiso 1 1 calc R . .
C45 C 0.82453(7) -0.02449(7) 0.02280(8) 0.0265(3) Uani 1 1 d . . .
H45 H 0.8489 -0.0193 0.0709 0.032 Uiso 1 1 calc R . .
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
Fe 0.02196(12) 0.01955(12) 0.01920(12) -0.00044(8) 0.00818(9) -0.00242(8)
O1 0.0438(7) 0.0359(6) 0.0203(5) 0.0008(5) 0.0099(5) 0.0165(5)
N1 0.0249(6) 0.0212(6) 0.0274(7) -0.0021(5) 0.0112(5) -0.0032(5)
N2 0.0349(8) 0.0222(7) 0.0370(8) 0.0017(6) 0.0099(6) -0.0048(6)
N3 0.0265(6) 0.0225(6) 0.0220(6) 0.0001(5) 0.0097(5) -0.0012(5)
N4 0.0271(7) 0.0256(7) 0.0177(6) 0.0008(5) 0.0055(5) -0.0028(5)
N5 0.0227(6) 0.0227(6) 0.0144(6) 0.0001(5) 0.0047(5) -0.0016(5)
N6 0.0203(6) 0.0219(6) 0.0173(6) -0.0010(5) 0.0048(5) -0.0022(5)
N7 0.0198(6) 0.0216(6) 0.0195(6) -0.0023(5) 0.0070(5) -0.0017(5)
N8 0.0214(6) 0.0232(6) 0.0285(7) -0.0037(5) 0.0096(5) -0.0031(5)
N9 0.0340(7) 0.0235(6) 0.0238(6) 0.0005(5) 0.0142(6) -0.0045(5)
N10 0.0254(6) 0.0216(6) 0.0220(6) -0.0009(5) 0.0107(5) -0.0032(5)
N11 0.0240(6) 0.0214(6) 0.0284(7) -0.0028(5) 0.0124(5) -0.0045(5)
N12 0.0224(6) 0.0237(6) 0.0198(6) 0.0002(5) 0.0064(5) 0.0000(5)
C1 0.0228(7) 0.0249(8) 0.0284(8) -0.0054(6) 0.0128(6) -0.0023(6)
C2 0.0280(8) 0.0243(7) 0.0325(8) -0.0057(6) 0.0154(7) -0.0038(6)
C3 0.0270(8) 0.0309(8) 0.0352(9) -0.0072(7) 0.0157(7) -0.0049(6)
C4 0.0314(9) 0.0360(9) 0.0419(10) -0.0084(8) 0.0142(8) -0.0130(7)
C5 0.0449(11) 0.0311(9) 0.0529(12) -0.0022(8) 0.0123(9) -0.0179(8)
C6 0.0430(10) 0.0284(9) 0.0508(11) 0.0026(8) 0.0100(9) -0.0090(8)
C7 0.0306(9) 0.0275(8) 0.0371(9) -0.0032(7) 0.0133(7) -0.0060(6)
C8 0.0298(8) 0.0213(7) 0.0347(9) -0.0023(6) 0.0152(7) -0.0041(6)
C9 0.0332(9) 0.0229(8) 0.0294(8) 0.0018(6) 0.0133(7) 0.0002(6)
C10 0.0378(9) 0.0258(8) 0.0276(8) 0.0039(6) 0.0141(7) 0.0009(7)
C11 0.0431(10) 0.0271(8) 0.0378(9) 0.0057(7) 0.0176(8) 0.0006(7)
C12 0.0526(11) 0.0281(8) 0.0343(9) 0.0111(7) 0.0219(8) 0.0084(8)
C13 0.0513(11) 0.0354(9) 0.0229(8) 0.0065(7) 0.0139(8) 0.0090(8)
C14 0.0444(10) 0.0318(9) 0.0223(8) 0.0030(7) 0.0124(7) 0.0010(7)
C15 0.0377(9) 0.0269(8) 0.0227(8) 0.0035(6) 0.0138(7) 0.0017(7)
C16 0.0306(8) 0.0252(7) 0.0181(7) 0.0021(6) 0.0082(6) -0.0018(6)
C17 0.0252(7) 0.0218(7) 0.0189(7) -0.0019(6) 0.0050(6) -0.0012(6)
C18 0.0251(7) 0.0259(7) 0.0169(7) -0.0003(6) 0.0060(6) -0.0010(6)
C19 0.0274(8) 0.0332(8) 0.0208(7) 0.0019(6) 0.0028(6) 0.0013(6)
C20 0.0202(8) 0.0410(9) 0.0310(8) 0.0024(7) 0.0029(6) -0.0002(7)
C21 0.0257(8) 0.0370(9) 0.0307(8) 0.0050(7) 0.0108(7) -0.0023(7)
C22 0.0234(8) 0.0302(8) 0.0210(7) 0.0040(6) 0.0056(6) -0.0009(6)
C23 0.0217(7) 0.0243(7) 0.0190(7) -0.0012(6) 0.0058(6) 0.0006(6)
C24 0.0230(7) 0.0205(7) 0.0181(7) -0.0029(5) 0.0077(6) -0.0035(5)
C25 0.0236(7) 0.0200(7) 0.0180(7) -0.0033(5) 0.0068(6) -0.0010(6)
C26 0.0226(7) 0.0201(7) 0.0200(7) -0.0047(6) 0.0041(6) -0.0024(6)
C27 0.0253(8) 0.0230(7) 0.0240(7) -0.0011(6) 0.0039(6) -0.0031(6)
C28 0.0306(8) 0.0264(8) 0.0247(8) 0.0025(6) 0.0015(6) -0.0017(6)
C29 0.0250(8) 0.0280(8) 0.0283(8) -0.0014(7) -0.0026(6) 0.0021(6)
C30 0.0213(7) 0.0264(8) 0.0310(8) -0.0045(6) 0.0047(6) -0.0006(6)
C31 0.0261(8) 0.0186(7) 0.0236(7) -0.0058(6) 0.0073(6) -0.0021(6)
C32 0.0204(7) 0.0204(7) 0.0264(7) -0.0019(6) 0.0071(6) -0.0014(6)
C33 0.0337(8) 0.0219(7) 0.0227(7) 0.0005(6) 0.0152(6) -0.0072(6)
C34 0.0406(9) 0.0235(8) 0.0276(8) 0.0000(6) 0.0186(7) -0.0046(7)
C35 0.0571(12) 0.0340(9) 0.0276(9) -0.0007(7) 0.0199(8) 0.0025(8)
C36 0.0762(14) 0.0389(10) 0.0323(10) -0.0037(8) 0.0280(10) 0.0084(10)
C37 0.0640(13) 0.0354(10) 0.0404(10) 0.0022(8) 0.0297(10) 0.0126(9)
C38 0.0454(10) 0.0265(8) 0.0355(9) 0.0033(7) 0.0232(8) 0.0019(7)
C39 0.0391(9) 0.0213(7) 0.0290(8) -0.0006(6) 0.0199(7) -0.0053(6)
C40 0.0267(8) 0.0184(7) 0.0302(8) -0.0015(6) 0.0151(6) -0.0052(6)
C41 0.0245(7) 0.0252(8) 0.0209(7) 0.0011(6) 0.0066(6) 0.0020(6)
C42 0.0295(8) 0.0296(8) 0.0170(7) 0.0001(6) 0.0045(6) 0.0046(6)
C43 0.0304(8) 0.0261(8) 0.0235(8) 0.0013(6) 0.0112(6) 0.0034(6)
C44 0.0268(8) 0.0318(8) 0.0240(8) 0.0007(6) 0.0047(6) 0.0075(6)
C45 0.0246(8) 0.0297(8) 0.0228(7) -0.0017(6) 0.0030(6) 0.0032(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe N7 1.8675(12) . ?
Fe N3 1.8709(12) . ?
Fe N10 1.8907(12) . ?
Fe N5 1.9068(12) . ?
Fe N1 1.9096(12) . ?
Fe N12 2.0134(12) . ?
O1 C43 1.3033(18) . ?
O1 H1 0.8400 . ?
N1 C8 1.3524(19) . ?
N1 C1 1.403(2) . ?
N2 C8 1.329(2) . ?
N2 C9 1.355(2) . ?
N3 C9 1.3156(19) . ?
N3 C16 1.4705(19) . ?
N4 C17 1.2830(19) . ?
N4 C16 1.4670(19) . ?
N5 C24 1.3587(18) . ?
N5 C17 1.4034(18) . ?
N6 C24 1.3215(19) . ?
N6 C25 1.3623(18) . ?
N7 C25 1.3141(18) . ?
N7 C32 1.4848(18) . ?
N8 C1 1.280(2) . ?
N8 C32 1.4602(18) . ?
N9 C33 1.316(2) . ?
N9 C16 1.497(2) . ?
N10 C33 1.3470(19) . ?
N10 C40 1.4044(19) . ?
N11 C40 1.282(2) . ?
N11 C32 1.4815(18) . ?
N12 C45 1.3513(19) . ?
N12 C41 1.3524(18) . ?
C1 C2 1.485(2) . ?
C2 C3 1.383(2) . ?
C2 C7 1.393(2) . ?
C3 C4 1.394(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.389(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.476(2) . ?
C9 C10 1.474(2) . ?
C10 C11 1.389(2) . ?
C10 C15 1.391(2) . ?
C11 C12 1.387(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.388(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.395(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.377(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.523(2) . ?
C17 C18 1.484(2) . ?
C18 C19 1.387(2) . ?
C18 C23 1.392(2) . ?
C19 C20 1.388(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.393(2) . ?
C20 H20 0.9500 . ?
C21 C22 1.396(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.381(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.476(2) . ?
C25 C26 1.471(2) . ?
C26 C27 1.385(2) . ?
C26 C31 1.392(2) . ?
C27 C28 1.394(2) . ?
C27 H27 0.9500 . ?
C28 C29 1.392(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.396(2) . ?
C29 H29 0.9500 . ?
C30 C31 1.381(2) . ?
C30 H30 0.9500 . ?
C31 C32 1.521(2) . ?
C33 C34 1.489(2) . ?
C34 C39 1.392(2) . ?
C34 C35 1.392(2) . ?
C35 C36 1.399(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.379(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.396(2) . ?
C37 H37 0.9500 . ?
C38 C39 1.388(2) . ?
C38 H38 0.9500 . ?
C39 C40 1.484(2) . ?
C41 C42 1.371(2) . ?
C41 H41 0.9500 . ?
C42 C43 1.411(2) . ?
C42 H42 0.9500 . ?
C43 C44 1.410(2) . ?
C44 C45 1.373(2) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
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_3
_geom_angle_publ_flag
N7 Fe N3 172.06(5) . . ?
N7 Fe N10 85.41(5) . . ?
N3 Fe N10 86.65(5) . . ?
N7 Fe N5 89.58(5) . . ?
N3 Fe N5 90.65(5) . . ?
N10 Fe N5 92.43(5) . . ?
N7 Fe N1 91.14(5) . . ?
N3 Fe N1 89.19(5) . . ?
N10 Fe N1 91.61(5) . . ?
N5 Fe N1 175.95(5) . . ?
N7 Fe N12 94.14(5) . . ?
N3 Fe N12 93.79(5) . . ?
N10 Fe N12 179.25(5) . . ?
N5 Fe N12 88.18(5) . . ?
N1 Fe N12 87.79(5) . . ?
C43 O1 H1 109.5 . . ?
C8 N1 C1 109.83(12) . . ?
C8 N1 Fe 123.47(11) . . ?
C1 N1 Fe 124.67(10) . . ?
C8 N2 C9 118.28(13) . . ?
C9 N3 C16 111.18(12) . . ?
C9 N3 Fe 127.98(11) . . ?
C16 N3 Fe 119.05(9) . . ?
C17 N4 C16 118.21(13) . . ?
C24 N5 C17 109.39(12) . . ?
C24 N5 Fe 123.53(10) . . ?
C17 N5 Fe 125.08(9) . . ?
C24 N6 C25 118.25(12) . . ?
C25 N7 C32 111.07(12) . . ?
C25 N7 Fe 127.75(10) . . ?
C32 N7 Fe 119.56(9) . . ?
C1 N8 C32 118.46(13) . . ?
C33 N9 C16 123.38(12) . . ?
C33 N10 C40 110.79(12) . . ?
C33 N10 Fe 125.41(10) . . ?
C40 N10 Fe 123.70(10) . . ?
C40 N11 C32 120.20(12) . . ?
C45 N12 C41 116.45(12) . . ?
C45 N12 Fe 122.08(10) . . ?
C41 N12 Fe 121.43(10) . . ?
N8 C1 N1 128.54(13) . . ?
N8 C1 C2 124.09(14) . . ?
N1 C1 C2 107.36(13) . . ?
C3 C2 C7 121.68(15) . . ?
C3 C2 C1 131.60(15) . . ?
C7 C2 C1 106.64(14) . . ?
C2 C3 C4 117.40(16) . . ?
C2 C3 H3 121.3 . . ?
C4 C3 H3 121.3 . . ?
C5 C4 C3 121.07(16) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 121.54(16) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 117.29(17) . . ?
C7 C6 H6 121.4 . . ?
C5 C6 H6 121.4 . . ?
C6 C7 C2 121.02(16) . . ?
C6 C7 C8 131.76(16) . . ?
C2 C7 C8 107.18(13) . . ?
N2 C8 N1 128.34(14) . . ?
N2 C8 C7 122.65(14) . . ?
N1 C8 C7 108.97(14) . . ?
N3 C9 N2 126.91(15) . . ?
N3 C9 C10 109.72(14) . . ?
N2 C9 C10 123.37(14) . . ?
C11 C10 C15 121.42(16) . . ?
C11 C10 C9 131.34(16) . . ?
C15 C10 C9 107.22(13) . . ?
C12 C11 C10 117.34(16) . . ?
C12 C11 H11 121.3 . . ?
C10 C11 H11 121.3 . . ?
C11 C12 C13 121.14(15) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C12 C13 C14 121.33(17) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C13 117.45(16) . . ?
C15 C14 H14 121.3 . . ?
C13 C14 H14 121.3 . . ?
C14 C15 C10 121.30(15) . . ?
C14 C15 C16 130.67(15) . . ?
C10 C15 C16 108.04(14) . . ?
N4 C16 N3 114.68(11) . . ?
N4 C16 N9 110.78(12) . . ?
N3 C16 N9 108.20(12) . . ?
N4 C16 C15 111.32(13) . . ?
N3 C16 C15 102.45(12) . . ?
N9 C16 C15 108.99(11) . . ?
N4 C17 N5 127.55(13) . . ?
N4 C17 C18 124.83(13) . . ?
N5 C17 C18 107.59(12) . . ?
C19 C18 C23 120.86(14) . . ?
C19 C18 C17 132.45(14) . . ?
C23 C18 C17 106.67(12) . . ?
C18 C19 C20 117.60(14) . . ?
C18 C19 H19 121.2 . . ?
C20 C19 H19 121.2 . . ?
C19 C20 C21 121.58(15) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C20 C21 C22 120.61(14) . . ?
C20 C21 H21 119.7 . . ?
C22 C21 H21 119.7 . . ?
C23 C22 C21 117.55(14) . . ?
C23 C22 H22 121.2 . . ?
C21 C22 H22 121.2 . . ?
C22 C23 C18 121.77(14) . . ?
C22 C23 C24 131.02(14) . . ?
C18 C23 C24 107.19(12) . . ?
N6 C24 N5 128.51(13) . . ?
N6 C24 C23 122.52(12) . . ?
N5 C24 C23 108.97(12) . . ?
N7 C25 N6 127.46(13) . . ?
N7 C25 C26 109.60(12) . . ?
N6 C25 C26 122.94(12) . . ?
C27 C26 C31 122.07(14) . . ?
C27 C26 C25 130.48(13) . . ?
C31 C26 C25 107.25(12) . . ?
C26 C27 C28 117.33(14) . . ?
C26 C27 H27 121.3 . . ?
C28 C27 H27 121.3 . . ?
C29 C28 C27 120.53(15) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C30 121.80(14) . . ?
C28 C29 H29 119.1 . . ?
C30 C29 H29 119.1 . . ?
C31 C30 C29 117.38(14) . . ?
C31 C30 H30 121.3 . . ?
C29 C30 H30 121.3 . . ?
C30 C31 C26 120.88(14) . . ?
C30 C31 C32 130.57(14) . . ?
C26 C31 C32 108.43(12) . . ?
N8 C32 N11 108.32(11) . . ?
N8 C32 N7 114.71(11) . . ?
N11 C32 N7 110.55(11) . . ?
N8 C32 C31 111.34(12) . . ?
N11 C32 C31 110.03(11) . . ?
N7 C32 C31 101.76(11) . . ?
N9 C33 N10 126.92(14) . . ?
N9 C33 C34 124.61(14) . . ?
N10 C33 C34 108.47(13) . . ?
C39 C34 C35 120.97(15) . . ?
C39 C34 C33 106.59(13) . . ?
C35 C34 C33 132.45(16) . . ?
C34 C35 C36 117.07(17) . . ?
C34 C35 H35 121.5 . . ?
C36 C35 H35 121.5 . . ?
C37 C36 C35 122.02(17) . . ?
C37 C36 H36 119.0 . . ?
C35 C36 H36 119.0 . . ?
C36 C37 C38 120.68(17) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
C39 C38 C37 117.72(17) . . ?
C39 C38 H38 121.1 . . ?
C37 C38 H38 121.1 . . ?
C38 C39 C34 121.50(15) . . ?
C38 C39 C40 130.98(16) . . ?
C34 C39 C40 107.49(14) . . ?
N11 C40 N10 130.11(13) . . ?
N11 C40 C39 123.33(14) . . ?
N10 C40 C39 106.53(13) . . ?
N12 C41 C42 123.40(14) . . ?
N12 C41 H41 118.3 . . ?
C42 C41 H41 118.3 . . ?
C41 C42 C43 120.50(14) . . ?
C41 C42 H42 119.7 . . ?
C43 C42 H42 119.7 . . ?
O1 C43 C44 120.55(14) . . ?
O1 C43 C42 123.69(14) . . ?
C44 C43 C42 115.75(13) . . ?
C45 C44 C43 119.95(14) . . ?
C45 C44 H44 120.0 . . ?
C43 C44 H44 120.0 . . ?
N12 C45 C44 123.92(14) . . ?
N12 C45 H45 118.0 . . ?
C44 C45 H45 118.0 . . ?
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
N7 Fe N1 C8 164.14(12) . . . . ?
N3 Fe N1 C8 -23.80(12) . . . . ?
N10 Fe N1 C8 -110.42(12) . . . . ?
N5 Fe N1 C8 63.9(8) . . . . ?
N12 Fe N1 C8 70.03(12) . . . . ?
N7 Fe N1 C1 2.02(12) . . . . ?
N3 Fe N1 C1 174.09(12) . . . . ?
N10 Fe N1 C1 87.47(12) . . . . ?
N5 Fe N1 C1 -98.2(7) . . . . ?
N12 Fe N1 C1 -92.08(12) . . . . ?
N7 Fe N3 C9 106.5(4) . . . . ?
N10 Fe N3 C9 105.66(13) . . . . ?
N5 Fe N3 C9 -161.95(13) . . . . ?
N1 Fe N3 C9 14.00(13) . . . . ?
N12 Fe N3 C9 -73.73(13) . . . . ?
N7 Fe N3 C16 -56.9(4) . . . . ?
N10 Fe N3 C16 -57.67(11) . . . . ?
N5 Fe N3 C16 34.72(11) . . . . ?
N1 Fe N3 C16 -149.33(11) . . . . ?
N12 Fe N3 C16 122.94(10) . . . . ?
N7 Fe N5 C24 -22.56(11) . . . . ?
N3 Fe N5 C24 165.37(11) . . . . ?
N10 Fe N5 C24 -107.95(11) . . . . ?
N1 Fe N5 C24 77.7(8) . . . . ?
N12 Fe N5 C24 71.60(11) . . . . ?
N7 Fe N5 C17 175.23(11) . . . . ?
N3 Fe N5 C17 3.17(12) . . . . ?
N10 Fe N5 C17 89.84(12) . . . . ?
N1 Fe N5 C17 -84.5(7) . . . . ?
N12 Fe N5 C17 -90.61(12) . . . . ?
N3 Fe N7 C25 105.3(4) . . . . ?
N10 Fe N7 C25 106.08(12) . . . . ?
N5 Fe N7 C25 13.61(12) . . . . ?
N1 Fe N7 C25 -162.40(12) . . . . ?
N12 Fe N7 C25 -74.53(12) . . . . ?
N3 Fe N7 C32 -58.8(4) . . . . ?
N10 Fe N7 C32 -58.05(10) . . . . ?
N5 Fe N7 C32 -150.52(10) . . . . ?
N1 Fe N7 C32 33.47(10) . . . . ?
N12 Fe N7 C32 121.34(10) . . . . ?
N7 Fe N10 C33 -154.93(12) . . . . ?
N3 Fe N10 C33 24.96(12) . . . . ?
N5 Fe N10 C33 -65.55(12) . . . . ?
N1 Fe N10 C33 114.05(12) . . . . ?
N7 Fe N10 C40 29.17(11) . . . . ?
N3 Fe N10 C40 -150.93(11) . . . . ?
N5 Fe N10 C40 118.56(11) . . . . ?
N1 Fe N10 C40 -61.84(11) . . . . ?
N7 Fe N12 C45 147.56(12) . . . . ?
N3 Fe N12 C45 -32.41(12) . . . . ?
N5 Fe N12 C45 58.11(12) . . . . ?
N1 Fe N12 C45 -121.45(12) . . . . ?
N7 Fe N12 C41 -34.61(11) . . . . ?
N3 Fe N12 C41 145.41(11) . . . . ?
N5 Fe N12 C41 -124.06(11) . . . . ?
N1 Fe N12 C41 56.37(11) . . . . ?
C32 N8 C1 N1 -2.3(2) . . . . ?
C32 N8 C1 C2 176.26(13) . . . . ?
C8 N1 C1 N8 177.02(15) . . . . ?
Fe N1 C1 N8 -18.8(2) . . . . ?
C8 N1 C1 C2 -1.75(16) . . . . ?
Fe N1 C1 C2 162.44(9) . . . . ?
N8 C1 C2 C3 -0.9(3) . . . . ?
N1 C1 C2 C3 177.91(15) . . . . ?
N8 C1 C2 C7 -177.59(14) . . . . ?
N1 C1 C2 C7 1.25(16) . . . . ?
C7 C2 C3 C4 -0.5(2) . . . . ?
C1 C2 C3 C4 -176.70(15) . . . . ?
C2 C3 C4 C5 0.3(2) . . . . ?
C3 C4 C5 C6 -0.1(3) . . . . ?
C4 C5 C6 C7 0.1(3) . . . . ?
C5 C6 C7 C2 -0.3(3) . . . . ?
C5 C6 C7 C8 176.99(18) . . . . ?
C3 C2 C7 C6 0.5(2) . . . . ?
C1 C2 C7 C6 177.58(16) . . . . ?
C3 C2 C7 C8 -177.39(14) . . . . ?
C1 C2 C7 C8 -0.33(17) . . . . ?
C9 N2 C8 N1 4.5(2) . . . . ?
C9 N2 C8 C7 -172.96(15) . . . . ?
C1 N1 C8 N2 -176.22(15) . . . . ?
Fe N1 C8 N2 19.4(2) . . . . ?
C1 N1 C8 C7 1.56(17) . . . . ?
Fe N1 C8 C7 -162.86(10) . . . . ?
C6 C7 C8 N2 -0.4(3) . . . . ?
C2 C7 C8 N2 177.19(14) . . . . ?
C6 C7 C8 N1 -178.34(18) . . . . ?
C2 C7 C8 N1 -0.74(17) . . . . ?
C16 N3 C9 N2 168.13(15) . . . . ?
Fe N3 C9 N2 3.7(2) . . . . ?
C16 N3 C9 C10 -10.99(17) . . . . ?
Fe N3 C9 C10 -175.39(10) . . . . ?
C8 N2 C9 N3 -17.1(2) . . . . ?
C8 N2 C9 C10 161.87(15) . . . . ?
N3 C9 C10 C11 -173.28(17) . . . . ?
N2 C9 C10 C11 7.6(3) . . . . ?
N3 C9 C10 C15 4.88(18) . . . . ?
N2 C9 C10 C15 -174.28(15) . . . . ?
C15 C10 C11 C12 -0.2(2) . . . . ?
C9 C10 C11 C12 177.73(16) . . . . ?
C10 C11 C12 C13 -0.9(2) . . . . ?
C11 C12 C13 C14 0.8(3) . . . . ?
C12 C13 C14 C15 0.4(2) . . . . ?
C13 C14 C15 C10 -1.5(2) . . . . ?
C13 C14 C15 C16 178.66(16) . . . . ?
C11 C10 C15 C14 1.4(2) . . . . ?
C9 C10 C15 C14 -176.94(14) . . . . ?
C11 C10 C15 C16 -178.69(15) . . . . ?
C9 C10 C15 C16 2.93(17) . . . . ?
C17 N4 C16 N3 40.97(18) . . . . ?
C17 N4 C16 N9 -81.85(16) . . . . ?
C17 N4 C16 C15 156.70(13) . . . . ?
C9 N3 C16 N4 132.88(13) . . . . ?
Fe N3 C16 N4 -61.15(15) . . . . ?
C9 N3 C16 N9 -102.91(14) . . . . ?
Fe N3 C16 N9 63.06(13) . . . . ?
C9 N3 C16 C15 12.14(16) . . . . ?
Fe N3 C16 C15 178.10(9) . . . . ?
C33 N9 C16 N4 102.41(15) . . . . ?
C33 N9 C16 N3 -24.10(18) . . . . ?
C33 N9 C16 C15 -134.78(14) . . . . ?
C14 C15 C16 N4 48.1(2) . . . . ?
C10 C15 C16 N4 -131.75(14) . . . . ?
C14 C15 C16 N3 171.14(16) . . . . ?
C10 C15 C16 N3 -8.71(16) . . . . ?
C14 C15 C16 N9 -74.4(2) . . . . ?
C10 C15 C16 N9 105.76(14) . . . . ?
C16 N4 C17 N5 0.8(2) . . . . ?
C16 N4 C17 C18 178.41(13) . . . . ?
C24 N5 C17 N4 173.45(14) . . . . ?
Fe N5 C17 N4 -22.2(2) . . . . ?
C24 N5 C17 C18 -4.52(15) . . . . ?
Fe N5 C17 C18 159.81(9) . . . . ?
N4 C17 C18 C19 4.4(3) . . . . ?
N5 C17 C18 C19 -177.60(16) . . . . ?
N4 C17 C18 C23 -174.01(14) . . . . ?
N5 C17 C18 C23 4.03(16) . . . . ?
C23 C18 C19 C20 0.8(2) . . . . ?
C17 C18 C19 C20 -177.38(16) . . . . ?
C18 C19 C20 C21 0.8(2) . . . . ?
C19 C20 C21 C22 -1.1(3) . . . . ?
C20 C21 C22 C23 -0.3(2) . . . . ?
C21 C22 C23 C18 1.9(2) . . . . ?
C21 C22 C23 C24 179.93(15) . . . . ?
C19 C18 C23 C22 -2.2(2) . . . . ?
C17 C18 C23 C22 176.41(13) . . . . ?
C19 C18 C23 C24 179.35(14) . . . . ?
C17 C18 C23 C24 -2.05(16) . . . . ?
C25 N6 C24 N5 2.1(2) . . . . ?
C25 N6 C24 C23 -177.16(13) . . . . ?
C17 N5 C24 N6 -176.11(14) . . . . ?
Fe N5 C24 N6 19.3(2) . . . . ?
C17 N5 C24 C23 3.28(15) . . . . ?
Fe N5 C24 C23 -161.35(9) . . . . ?
C22 C23 C24 N6 0.5(2) . . . . ?
C18 C23 C24 N6 178.77(13) . . . . ?
C22 C23 C24 N5 -178.93(15) . . . . ?
C18 C23 C24 N5 -0.66(16) . . . . ?
C32 N7 C25 N6 167.14(13) . . . . ?
Fe N7 C25 N6 1.9(2) . . . . ?
C32 N7 C25 C26 -13.66(15) . . . . ?
Fe N7 C25 C26 -178.89(9) . . . . ?
C24 N6 C25 N7 -13.8(2) . . . . ?
C24 N6 C25 C26 167.14(13) . . . . ?
N7 C25 C26 C27 -167.37(14) . . . . ?
N6 C25 C26 C27 11.9(2) . . . . ?
N7 C25 C26 C31 7.42(16) . . . . ?
N6 C25 C26 C31 -173.34(13) . . . . ?
C31 C26 C27 C28 -0.8(2) . . . . ?
C25 C26 C27 C28 173.32(14) . . . . ?
C26 C27 C28 C29 0.5(2) . . . . ?
C27 C28 C29 C30 0.1(2) . . . . ?
C28 C29 C30 C31 -0.3(2) . . . . ?
C29 C30 C31 C26 0.0(2) . . . . ?
C29 C30 C31 C32 -175.48(14) . . . . ?
C27 C26 C31 C30 0.6(2) . . . . ?
C25 C26 C31 C30 -174.76(13) . . . . ?
C27 C26 C31 C32 176.97(13) . . . . ?
C25 C26 C31 C32 1.64(15) . . . . ?
C1 N8 C32 N11 -82.75(15) . . . . ?
C1 N8 C32 N7 41.27(18) . . . . ?
C1 N8 C32 C31 156.15(13) . . . . ?
C40 N11 C32 N8 101.13(15) . . . . ?
C40 N11 C32 N7 -25.34(17) . . . . ?
C40 N11 C32 C31 -136.96(13) . . . . ?
C25 N7 C32 N8 134.18(13) . . . . ?
Fe N7 C32 N8 -59.21(14) . . . . ?
C25 N7 C32 N11 -102.99(13) . . . . ?
Fe N7 C32 N11 63.61(13) . . . . ?
C25 N7 C32 C31 13.85(14) . . . . ?
Fe N7 C32 C31 -179.54(9) . . . . ?
C30 C31 C32 N8 44.5(2) . . . . ?
C26 C31 C32 N8 -131.47(12) . . . . ?
C30 C31 C32 N11 -75.65(19) . . . . ?
C26 C31 C32 N11 108.43(13) . . . . ?
C30 C31 C32 N7 167.13(15) . . . . ?
C26 C31 C32 N7 -8.80(14) . . . . ?
C16 N9 C33 N10 -7.1(2) . . . . ?
C16 N9 C33 C34 172.65(13) . . . . ?
C40 N10 C33 N9 177.91(14) . . . . ?
Fe N10 C33 N9 1.6(2) . . . . ?
C40 N10 C33 C34 -1.86(16) . . . . ?
Fe N10 C33 C34 -178.21(9) . . . . ?
N9 C33 C34 C39 -176.26(14) . . . . ?
N10 C33 C34 C39 3.52(16) . . . . ?
N9 C33 C34 C35 3.9(3) . . . . ?
N10 C33 C34 C35 -176.33(17) . . . . ?
C39 C34 C35 C36 0.8(2) . . . . ?
C33 C34 C35 C36 -179.38(17) . . . . ?
C34 C35 C36 C37 1.0(3) . . . . ?
C35 C36 C37 C38 -1.7(3) . . . . ?
C36 C37 C38 C39 0.5(3) . . . . ?
C37 C38 C39 C34 1.3(2) . . . . ?
C37 C38 C39 C40 -176.40(16) . . . . ?
C35 C34 C39 C38 -2.0(2) . . . . ?
C33 C34 C39 C38 178.16(14) . . . . ?
C35 C34 C39 C40 176.21(14) . . . . ?
C33 C34 C39 C40 -3.66(16) . . . . ?
C32 N11 C40 N10 -1.6(2) . . . . ?
C32 N11 C40 C39 176.20(12) . . . . ?
C33 N10 C40 N11 177.68(14) . . . . ?
Fe N10 C40 N11 -5.9(2) . . . . ?
C33 N10 C40 C39 -0.40(15) . . . . ?
Fe N10 C40 C39 176.02(9) . . . . ?
C38 C39 C40 N11 2.3(3) . . . . ?
C34 C39 C40 N11 -175.59(13) . . . . ?
C38 C39 C40 N10 -179.41(15) . . . . ?
C34 C39 C40 N10 2.65(16) . . . . ?
C45 N12 C41 C42 0.0(2) . . . . ?
Fe N12 C41 C42 -177.91(12) . . . . ?
N12 C41 C42 C43 1.0(2) . . . . ?
C41 C42 C43 O1 179.30(15) . . . . ?
C41 C42 C43 C44 -1.6(2) . . . . ?
O1 C43 C44 C45 -179.66(15) . . . . ?
C42 C43 C44 C45 1.2(2) . . . . ?
C41 N12 C45 C44 -0.4(2) . . . . ?
Fe N12 C45 C44 177.48(12) . . . . ?
C43 C44 C45 N12 -0.2(2) . . . . ?
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
O1 H1 N9 0.84 1.75 2.5860(16) 170.4 2_554
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 26.44
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 0.431
_refine_diff_density_min -0.309
_refine_diff_density_rms 0.048
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.002 0.006 -0.010 3111.4 616.2
_platon_squeeze_details
;
The volume occupied by solvent is 33.7 percent of the unit cell.
;
# File processed with modiCIFer ver.11012005. I.A.Guzei, UW-Madison.
#===END