# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
_journal_year ?
_journal_volume ?
_journal_page_first ?
_publ_contact_author_email atasio@ucy.ac.cy
_publ_contact_author_name 'Anastasios Tasiopoulos'
_publ_author_name A.Tasiopoulos
# end Validation Reply Form
# Attachment '- 2.cif'
data_ck3-sqz
_database_code_depnum_ccdc_archive 'CCDC 836723'
#TrackingRef '- 2.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C47 H95 Fe5 N4 O20'
_chemical_formula_sum 'C47 H95 Fe5 N4 O20'
_chemical_formula_weight 1315.52
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'
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 17.3966(2)
_cell_length_b 19.0674(3)
_cell_length_c 19.9009(3)
_cell_angle_alpha 90.00
_cell_angle_beta 96.0880(10)
_cell_angle_gamma 90.00
_cell_volume 6564.06(16)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 13541
_cell_measurement_theta_min 3.1041
_cell_measurement_theta_max 30.4088
_exptl_crystal_description prism
_exptl_crystal_colour 'translucent brown-purple'
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.331
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2780
_exptl_absorpt_coefficient_mu 1.144
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.811
_exptl_absorpt_correction_T_max 0.901
_exptl_absorpt_process_details
'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur-3 with Sapphire CCD'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 16.0288
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 53073
_diffrn_reflns_av_R_equivalents 0.0536
_diffrn_reflns_av_sigmaI/netI 0.0988
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 3.11
_diffrn_reflns_theta_max 27.50
_reflns_number_total 15054
_reflns_number_gt 8602
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics
;
PLATON (Spek, 2008), ORTEP-3 (Farrugia, 1997)
;
_computing_publication_material 'WINGX (Farrugia, 1999)'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436.
Farrugia, L. J. (1997). ORTEP-3 for Windows. J.Appl. Cryst.
30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838.
Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford
Diffraction Ltd, Abingdon, Oxford, England.
Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany.
Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands.
;
_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^)+(0.0334P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens 'geom & difmap'
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 15054
_refine_ls_number_parameters 730
_refine_ls_number_restraints 20
_refine_ls_R_factor_all 0.0764
_refine_ls_R_factor_gt 0.0396
_refine_ls_wR_factor_ref 0.0822
_refine_ls_wR_factor_gt 0.0781
_refine_ls_goodness_of_fit_ref 0.882
_refine_ls_restrained_S_all 0.886
_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
C1 C 0.52278(17) 0.43605(15) 0.29469(13) 0.0236(7) Uani 1 1 d . . .
C2 C 0.55630(17) 0.51014(15) 0.29908(15) 0.0260(7) Uani 1 1 d . . .
C3 C 0.5227(2) 0.54820(17) 0.35594(18) 0.0528(10) Uani 1 1 d . . .
H3A H 0.4675 0.5500 0.3468 0.079 Uiso 1 1 calc R . .
H3B H 0.5430 0.5950 0.3595 0.079 Uiso 1 1 calc R . .
H3C H 0.5364 0.5237 0.3976 0.079 Uiso 1 1 calc R . .
C4 C 0.53132(19) 0.54718(16) 0.23147(16) 0.0426(9) Uani 1 1 d . . .
H4A H 0.4759 0.5499 0.2247 0.064 Uiso 1 1 calc R . .
H4B H 0.5498 0.5211 0.1952 0.064 Uiso 1 1 calc R . .
H4C H 0.5527 0.5936 0.2324 0.064 Uiso 1 1 calc R . .
C5 C 0.64439(17) 0.50843(16) 0.31061(17) 0.0398(9) Uani 1 1 d . . .
H5A H 0.6639 0.5555 0.3143 0.060 Uiso 1 1 calc R . .
H5B H 0.6643 0.4853 0.2733 0.060 Uiso 1 1 calc R . .
H5C H 0.6603 0.4834 0.3516 0.060 Uiso 1 1 calc R . .
C6 C 0.69882(17) 0.27318(15) 0.22244(14) 0.0247(7) Uani 1 1 d . . .
C7 C 0.74313(17) 0.29442(17) 0.16374(15) 0.0318(8) Uani 1 1 d . . .
C8 C 0.6891(2) 0.3125(3) 0.10117(19) 0.0856(16) Uani 1 1 d . . .
H8A H 0.6596 0.2717 0.0864 0.128 Uiso 1 1 calc R . .
H8B H 0.7188 0.3277 0.0659 0.128 Uiso 1 1 calc R . .
H8C H 0.6547 0.3493 0.1117 0.128 Uiso 1 1 calc R . .
C9 C 0.7931(3) 0.3580(2) 0.1860(2) 0.0847(15) Uani 1 1 d . . .
H9A H 0.7606 0.3957 0.1978 0.127 Uiso 1 1 calc R . .
H9B H 0.8217 0.3725 0.1497 0.127 Uiso 1 1 calc R . .
H9C H 0.8285 0.3456 0.2245 0.127 Uiso 1 1 calc R . .
C10 C 0.7960(2) 0.2351(2) 0.1476(2) 0.0718(13) Uani 1 1 d . . .
H10A H 0.8310 0.2244 0.1869 0.108 Uiso 1 1 calc R . .
H10B H 0.8248 0.2489 0.1113 0.108 Uiso 1 1 calc R . .
H10C H 0.7656 0.1944 0.1345 0.108 Uiso 1 1 calc R . .
C11 C 0.57385(18) 0.13237(15) 0.24790(14) 0.0257(7) Uani 1 1 d . . .
C12 C 0.55303(19) 0.07338(16) 0.19731(16) 0.0359(8) Uani 1 1 d . . .
C13 C 0.4681(2) 0.0593(2) 0.1915(2) 0.0764(14) Uani 1 1 d . . .
H13A H 0.4406 0.0997 0.1729 0.115 Uiso 1 1 calc R . .
H13B H 0.4528 0.0495 0.2355 0.115 Uiso 1 1 calc R . .
H13C H 0.4564 0.0197 0.1625 0.115 Uiso 1 1 calc R . .
C14 C 0.5781(3) 0.0970(2) 0.13026(17) 0.0703(13) Uani 1 1 d . . .
H14A H 0.5627 0.0626 0.0962 0.106 Uiso 1 1 calc R . .
H14B H 0.6333 0.1022 0.1344 0.106 Uiso 1 1 calc R . .
H14C H 0.5542 0.1411 0.1176 0.106 Uiso 1 1 calc R . .
C15 C 0.5964(3) 0.00695(19) 0.2212(2) 0.0755(14) Uani 1 1 d . . .
H15A H 0.5907 -0.0009 0.2681 0.113 Uiso 1 1 calc R . .
H15B H 0.6502 0.0122 0.2155 0.113 Uiso 1 1 calc R . .
H15C H 0.5756 -0.0323 0.1951 0.113 Uiso 1 1 calc R . .
C16 C 0.85488(19) 0.25937(19) 0.39840(18) 0.0420(9) Uani 1 1 d . . .
C17 C 0.8850(2) 0.3299(2) 0.4285(2) 0.0546(11) Uani 1 1 d . . .
C18 C 0.8291(2) 0.38788(19) 0.4030(2) 0.0663(12) Uani 1 1 d . . .
H18A H 0.7786 0.3776 0.4157 0.099 Uiso 1 1 calc R . .
H18B H 0.8268 0.3908 0.3547 0.099 Uiso 1 1 calc R . .
H18C H 0.8467 0.4318 0.4225 0.099 Uiso 1 1 calc R . .
C19 C 0.9651(2) 0.3451(2) 0.4059(3) 0.0891(16) Uani 1 1 d U . .
H19A H 0.9807 0.3918 0.4191 0.134 Uiso 1 1 calc R . .
H19B H 0.9627 0.3408 0.3577 0.134 Uiso 1 1 calc R . .
H19C H 1.0018 0.3121 0.4268 0.134 Uiso 1 1 calc R . .
C20 C 0.8883(3) 0.3268(2) 0.5057(2) 0.0837(15) Uani 1 1 d U . .
H20A H 0.9030 0.3719 0.5244 0.126 Uiso 1 1 calc R . .
H20B H 0.9256 0.2923 0.5228 0.126 Uiso 1 1 calc R . .
H20C H 0.8383 0.3143 0.5183 0.126 Uiso 1 1 calc R . .
C21 C 0.30639(16) 0.36042(15) 0.39529(15) 0.0233(7) Uani 1 1 d . . .
C22 C 0.25094(17) 0.40373(16) 0.43352(14) 0.0287(7) Uani 1 1 d . . .
C23 C 0.2907(2) 0.42635(19) 0.50147(16) 0.0527(10) Uani 1 1 d . . .
H23A H 0.3077 0.3857 0.5273 0.079 Uiso 1 1 calc R . .
H23B H 0.2551 0.4525 0.5254 0.079 Uiso 1 1 calc R . .
H23C H 0.3345 0.4552 0.4948 0.079 Uiso 1 1 calc R . .
C24 C 0.2216(2) 0.46739(19) 0.39374(18) 0.0643(12) Uani 1 1 d . . .
H24A H 0.1848 0.4918 0.4179 0.097 Uiso 1 1 calc R . .
H24B H 0.1971 0.4529 0.3504 0.097 Uiso 1 1 calc R . .
H24C H 0.2641 0.4980 0.3875 0.097 Uiso 1 1 calc R . .
C25 C 0.1829(2) 0.3559(2) 0.4449(2) 0.0644(12) Uani 1 1 d . . .
H25A H 0.2014 0.3159 0.4710 0.097 Uiso 1 1 calc R . .
H25B H 0.1579 0.3407 0.4021 0.097 Uiso 1 1 calc R . .
H25C H 0.1466 0.3813 0.4688 0.097 Uiso 1 1 calc R . .
C26 C 0.30519(15) 0.19915(15) 0.28446(15) 0.0242(7) Uani 1 1 d . . .
C27 C 0.24528(19) 0.14600(17) 0.25360(17) 0.0406(9) Uani 1 1 d . . .
C28 C 0.2297(2) 0.15590(17) 0.17846(17) 0.0562(11) Uani 1 1 d . . .
H28A H 0.2755 0.1451 0.1576 0.084 Uiso 1 1 calc R . .
H28B H 0.2149 0.2037 0.1689 0.084 Uiso 1 1 calc R . .
H28C H 0.1886 0.1252 0.1610 0.084 Uiso 1 1 calc R . .
C29 C 0.1707(2) 0.1611(2) 0.2888(2) 0.0696(13) Uani 1 1 d . . .
H29A H 0.1296 0.1311 0.2700 0.104 Uiso 1 1 calc R . .
H29B H 0.1558 0.2092 0.2817 0.104 Uiso 1 1 calc R . .
H29C H 0.1810 0.1522 0.3364 0.104 Uiso 1 1 calc R . .
C30 C 0.2702(2) 0.07107(16) 0.26994(17) 0.0514(10) Uani 1 1 d . . .
H30A H 0.2316 0.0393 0.2499 0.077 Uiso 1 1 calc R . .
H30B H 0.2765 0.0646 0.3181 0.077 Uiso 1 1 calc R . .
H30C H 0.3184 0.0619 0.2522 0.077 Uiso 1 1 calc R . .
C31 C 0.61354(17) 0.16648(14) 0.60089(14) 0.0247(7) Uani 1 1 d . . .
C32 C 0.56731(17) 0.15832(16) 0.66233(14) 0.0287(7) Uani 1 1 d . . .
C33 C 0.52644(18) 0.22876(17) 0.66995(16) 0.0401(8) Uani 1 1 d . . .
H33A H 0.4922 0.2381 0.6299 0.060 Uiso 1 1 calc R . .
H33B H 0.5643 0.2655 0.6765 0.060 Uiso 1 1 calc R . .
H33C H 0.4973 0.2268 0.7082 0.060 Uiso 1 1 calc R . .
C34 C 0.50598(19) 0.10176(18) 0.65065(17) 0.0457(9) Uani 1 1 d . . .
H34A H 0.4708 0.1136 0.6119 0.069 Uiso 1 1 calc R . .
H34B H 0.4781 0.0982 0.6896 0.069 Uiso 1 1 calc R . .
H34C H 0.5302 0.0576 0.6431 0.069 Uiso 1 1 calc R . .
C35 C 0.62038(18) 0.14117(18) 0.72590(15) 0.0421(9) Uani 1 1 d . . .
H35A H 0.5913 0.1421 0.7643 0.063 Uiso 1 1 calc R . .
H35B H 0.6612 0.1752 0.7319 0.063 Uiso 1 1 calc R . .
H35C H 0.6422 0.0953 0.7217 0.063 Uiso 1 1 calc R . .
C36 C 0.35694(17) 0.41558(16) 0.13422(14) 0.0310(8) Uani 1 1 d . . .
H36A H 0.3927 0.4528 0.1493 0.037 Uiso 1 1 calc R . .
H36B H 0.3188 0.4348 0.1001 0.037 Uiso 1 1 calc R . .
C37 C 0.40019(17) 0.35735(17) 0.10380(14) 0.0357(8) Uani 1 1 d . . .
H37A H 0.4121 0.3720 0.0594 0.043 Uiso 1 1 calc R . .
H37B H 0.3666 0.3167 0.0978 0.043 Uiso 1 1 calc R . .
C38 C 0.47513(18) 0.33568(17) 0.14541(14) 0.0360(8) Uani 1 1 d . . .
H38A H 0.5008 0.3004 0.1207 0.043 Uiso 1 1 calc R . .
H38B H 0.5091 0.3761 0.1514 0.043 Uiso 1 1 calc R . .
C39 C 0.70527(18) 0.09003(16) 0.47045(15) 0.0359(8) Uani 1 1 d . . .
H39A H 0.6671 0.0639 0.4923 0.043 Uiso 1 1 calc R . .
H39B H 0.7398 0.1122 0.5056 0.043 Uiso 1 1 calc R . .
C40 C 0.7506(2) 0.03995(18) 0.43333(18) 0.0511(10) Uani 1 1 d . . .
H40A H 0.7741 0.0065 0.4660 0.061 Uiso 1 1 calc R . .
H40B H 0.7142 0.0141 0.4024 0.061 Uiso 1 1 calc R . .
C41 C 0.8105(2) 0.0653(2) 0.39521(19) 0.0615(12) Uani 1 1 d . . .
H41A H 0.8361 0.0251 0.3776 0.074 Uiso 1 1 calc R . .
H41B H 0.8485 0.0897 0.4259 0.074 Uiso 1 1 calc R . .
C42 C 0.36427(18) 0.10217(16) 0.47495(17) 0.0358(8) Uani 1 1 d . . .
H42A H 0.3256 0.0946 0.4368 0.043 Uiso 1 1 calc R . .
H42B H 0.3447 0.0824 0.5147 0.043 Uiso 1 1 calc R . .
C43 C 0.43712(17) 0.06458(15) 0.46239(15) 0.0315(8) Uani 1 1 d . . .
H43A H 0.4250 0.0152 0.4559 0.038 Uiso 1 1 calc R . .
H43B H 0.4733 0.0685 0.5028 0.038 Uiso 1 1 calc R . .
C44 C 0.47754(17) 0.08929(14) 0.40279(14) 0.0257(7) Uani 1 1 d . . .
H44A H 0.5246 0.0624 0.4009 0.031 Uiso 1 1 calc R . .
H44B H 0.4443 0.0807 0.3613 0.031 Uiso 1 1 calc R . .
C45 C 0.50806(16) 0.35267(14) 0.47642(14) 0.0269(7) Uani 1 1 d . . .
H45A H 0.4624 0.3703 0.4949 0.032 Uiso 1 1 calc R . .
H45B H 0.5096 0.3734 0.4321 0.032 Uiso 1 1 calc R . .
C46 C 0.57908(17) 0.37493(16) 0.52159(15) 0.0317(8) Uani 1 1 d . . .
H46A H 0.5781 0.3526 0.5653 0.038 Uiso 1 1 calc R . .
H46B H 0.5769 0.4252 0.5284 0.038 Uiso 1 1 calc R . .
C47 C 0.65460(17) 0.35714(15) 0.49449(16) 0.0319(8) Uani 1 1 d . . .
H47A H 0.6520 0.3710 0.4474 0.038 Uiso 1 1 calc R . .
H47B H 0.6961 0.3833 0.5194 0.038 Uiso 1 1 calc R . .
O1 O 0.44934(10) 0.43097(9) 0.28471(9) 0.0231(4) Uani 1 1 d . . .
O2 O 0.56906(10) 0.38503(9) 0.30087(9) 0.0224(4) Uani 1 1 d . . .
O3 O 0.62827(11) 0.28713(10) 0.21958(9) 0.0264(5) Uani 1 1 d . . .
O4 O 0.73771(11) 0.24362(12) 0.27125(10) 0.0394(6) Uani 1 1 d . . .
O5 O 0.52650(11) 0.18078(10) 0.25118(9) 0.0257(5) Uani 1 1 d . . .
O6 O 0.64036(12) 0.12929(10) 0.28009(10) 0.0348(5) Uani 1 1 d . . .
O7 O 0.78412(11) 0.24535(11) 0.40835(10) 0.0328(5) Uani 1 1 d . . .
O8 O 0.89554(13) 0.22121(14) 0.36781(14) 0.0627(8) Uani 1 1 d . . .
O9 O 0.33808(10) 0.30884(10) 0.42691(9) 0.0258(5) Uani 1 1 d . . .
O10 O 0.31686(10) 0.37854(10) 0.33632(9) 0.0260(5) Uani 1 1 d . . .
O11 O 0.31297(10) 0.25535(10) 0.25301(9) 0.0260(5) Uani 1 1 d . . .
O12 O 0.33828(11) 0.18405(10) 0.34176(10) 0.0277(5) Uani 1 1 d . . .
O13 O 0.57355(10) 0.16449(10) 0.54296(9) 0.0252(5) Uani 1 1 d . . .
O14 O 0.68421(11) 0.17713(11) 0.60933(9) 0.0317(5) Uani 1 1 d . . .
O15 O 0.46329(10) 0.30890(9) 0.20891(8) 0.0215(4) Uani 1 1 d . . .
O16 O 0.66716(10) 0.14269(9) 0.43006(9) 0.0214(4) Uani 1 1 d . . .
O17 O 0.49606(10) 0.16166(9) 0.40738(9) 0.0192(4) Uani 1 1 d . . .
O18 O 0.50235(10) 0.27834(9) 0.46972(9) 0.0210(4) Uani 1 1 d . . .
O19 O 0.45473(9) 0.28799(9) 0.33342(8) 0.0176(4) Uani 1 1 d . . .
O20 O 0.61475(10) 0.25049(9) 0.36423(8) 0.0196(4) Uani 1 1 d . . .
Fe1 Fe 0.38880(2) 0.33810(2) 0.269750(19) 0.02047(10) Uani 1 1 d . . .
Fe2 Fe 0.54771(2) 0.27927(2) 0.288335(19) 0.01882(10) Uani 1 1 d . . .
Fe3 Fe 0.70081(2) 0.19252(2) 0.35042(2) 0.02405(11) Uani 1 1 d . . .
Fe4 Fe 0.41851(2) 0.23763(2) 0.403060(19) 0.02033(10) Uani 1 1 d . . .
Fe5 Fe 0.58773(2) 0.21122(2) 0.452528(19) 0.01941(10) Uani 1 1 d . . .
N1 N 0.31815(14) 0.39022(13) 0.19160(12) 0.0249(6) Uani 1 1 d D . .
H1N H 0.2987(16) 0.4257(12) 0.2086(14) 0.037 Uiso 1 1 d D . .
H2N H 0.2815(14) 0.3654(14) 0.1750(14) 0.037 Uiso 1 1 d D . .
N2 N 0.78593(16) 0.11230(16) 0.33867(14) 0.0358(7) Uani 1 1 d D . .
H3N H 0.7694(19) 0.0893(16) 0.3032(12) 0.054 Uiso 1 1 d D . .
H4N H 0.8213(15) 0.1344(16) 0.3262(17) 0.054 Uiso 1 1 d D . .
N3 N 0.37595(15) 0.17800(15) 0.48501(14) 0.0348(7) Uani 1 1 d D . .
H5N H 0.3351(13) 0.1950(16) 0.4952(16) 0.052 Uiso 1 1 d D . .
H6N H 0.4091(16) 0.1778(17) 0.5191(13) 0.052 Uiso 1 1 d D . .
N4 N 0.67156(14) 0.28178(14) 0.50024(12) 0.0258(6) Uani 1 1 d D . .
H7N H 0.6866(17) 0.2670(14) 0.5415(10) 0.039 Uiso 1 1 d D . .
H8N H 0.7137(12) 0.2744(15) 0.4823(14) 0.039 Uiso 1 1 d D . .
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
C1 0.0264(17) 0.0324(18) 0.0124(15) -0.0025(12) 0.0034(13) -0.0029(14)
C2 0.0264(17) 0.0224(16) 0.0300(18) -0.0033(13) 0.0067(14) -0.0051(13)
C3 0.061(3) 0.040(2) 0.061(3) -0.0233(18) 0.021(2) -0.0095(19)
C4 0.041(2) 0.0321(19) 0.055(2) 0.0074(17) 0.0045(18) -0.0035(16)
C5 0.034(2) 0.0289(19) 0.056(2) 0.0004(16) 0.0038(17) -0.0102(15)
C6 0.0213(17) 0.0286(18) 0.0241(17) -0.0027(13) 0.0026(13) -0.0021(14)
C7 0.0200(16) 0.048(2) 0.0285(18) 0.0119(15) 0.0075(14) 0.0021(15)
C8 0.050(3) 0.162(5) 0.048(3) 0.048(3) 0.022(2) 0.017(3)
C9 0.103(4) 0.081(3) 0.076(3) 0.009(3) 0.038(3) -0.037(3)
C10 0.077(3) 0.089(3) 0.058(3) 0.023(2) 0.048(2) 0.023(3)
C11 0.0302(18) 0.0282(18) 0.0196(17) -0.0002(13) 0.0071(14) -0.0023(15)
C12 0.037(2) 0.0316(19) 0.038(2) -0.0106(15) 0.0016(16) 0.0024(16)
C13 0.061(3) 0.078(3) 0.090(3) -0.053(3) 0.010(3) -0.027(2)
C14 0.109(4) 0.071(3) 0.033(2) -0.017(2) 0.016(2) -0.018(3)
C15 0.114(4) 0.040(2) 0.072(3) -0.018(2) 0.006(3) 0.004(3)
C16 0.0220(19) 0.057(2) 0.046(2) 0.0225(19) 0.0012(17) -0.0006(18)
C17 0.031(2) 0.059(3) 0.071(3) 0.028(2) -0.008(2) -0.0192(19)
C18 0.047(2) 0.055(3) 0.100(3) 0.015(2) 0.024(2) -0.009(2)
C19 0.033(2) 0.067(3) 0.169(5) 0.037(3) 0.023(3) -0.006(2)
C20 0.077(3) 0.077(3) 0.091(3) 0.013(3) -0.020(3) -0.035(3)
C21 0.0186(16) 0.0260(17) 0.0248(17) -0.0006(13) -0.0001(13) -0.0029(13)
C22 0.0272(18) 0.0342(18) 0.0250(17) -0.0027(14) 0.0045(14) 0.0108(15)
C23 0.052(2) 0.067(3) 0.039(2) -0.0155(19) 0.0011(19) 0.017(2)
C24 0.083(3) 0.067(3) 0.044(2) -0.002(2) 0.010(2) 0.049(2)
C25 0.039(2) 0.076(3) 0.083(3) -0.020(2) 0.029(2) 0.000(2)
C26 0.0146(15) 0.0254(17) 0.0324(18) 0.0016(14) 0.0010(13) 0.0004(13)
C27 0.037(2) 0.035(2) 0.045(2) 0.0101(16) -0.0142(17) -0.0097(16)
C28 0.075(3) 0.032(2) 0.055(3) 0.0014(18) -0.026(2) -0.0154(19)
C29 0.028(2) 0.085(3) 0.094(3) 0.016(3) -0.003(2) -0.017(2)
C30 0.073(3) 0.0282(19) 0.049(2) 0.0072(16) -0.011(2) -0.0137(19)
C31 0.0253(17) 0.0247(17) 0.0241(17) 0.0017(13) 0.0021(14) 0.0023(14)
C32 0.0279(18) 0.0385(19) 0.0198(16) 0.0012(14) 0.0036(13) 0.0017(15)
C33 0.035(2) 0.052(2) 0.0344(19) -0.0068(16) 0.0083(16) 0.0066(17)
C34 0.047(2) 0.056(2) 0.038(2) 0.0037(17) 0.0210(17) -0.0112(19)
C35 0.038(2) 0.062(2) 0.0271(19) 0.0100(17) 0.0078(16) 0.0090(18)
C36 0.0268(18) 0.041(2) 0.0234(17) 0.0100(14) -0.0038(14) -0.0016(15)
C37 0.0330(19) 0.058(2) 0.0158(16) 0.0067(15) 0.0017(14) 0.0091(17)
C38 0.0343(19) 0.053(2) 0.0210(17) 0.0042(15) 0.0053(15) 0.0088(17)
C39 0.043(2) 0.0311(18) 0.036(2) 0.0131(15) 0.0133(16) 0.0133(16)
C40 0.054(2) 0.050(2) 0.054(2) 0.0205(19) 0.027(2) 0.0278(19)
C41 0.060(3) 0.067(3) 0.063(3) 0.030(2) 0.032(2) 0.035(2)
C42 0.033(2) 0.0332(19) 0.043(2) 0.0102(15) 0.0130(16) -0.0042(15)
C43 0.0306(18) 0.0272(18) 0.0366(19) 0.0094(14) 0.0027(15) -0.0029(14)
C44 0.0267(17) 0.0242(17) 0.0258(17) -0.0006(13) 0.0008(14) -0.0013(13)
C45 0.0270(17) 0.0278(18) 0.0249(17) -0.0055(13) -0.0012(14) 0.0073(14)
C46 0.0366(19) 0.0283(18) 0.0298(18) -0.0073(14) 0.0009(15) -0.0013(15)
C47 0.0304(18) 0.0315(19) 0.0335(19) -0.0059(14) 0.0018(15) -0.0056(15)
O1 0.0200(11) 0.0255(11) 0.0236(11) -0.0001(9) 0.0016(9) 0.0003(9)
O2 0.0209(11) 0.0227(11) 0.0236(11) 0.0000(9) 0.0020(9) 0.0022(9)
O3 0.0225(11) 0.0362(12) 0.0210(11) 0.0032(9) 0.0047(9) 0.0038(10)
O4 0.0218(12) 0.0636(16) 0.0344(13) 0.0216(11) 0.0098(10) 0.0098(11)
O5 0.0217(11) 0.0262(11) 0.0282(12) -0.0065(9) -0.0015(9) 0.0020(9)
O6 0.0312(13) 0.0376(13) 0.0344(13) -0.0105(10) -0.0019(10) 0.0123(10)
O7 0.0173(11) 0.0437(14) 0.0372(13) 0.0076(10) 0.0018(10) -0.0026(10)
O8 0.0243(14) 0.081(2) 0.085(2) 0.0077(16) 0.0141(14) 0.0026(14)
O9 0.0211(11) 0.0314(12) 0.0259(11) 0.0055(9) 0.0066(9) 0.0076(9)
O10 0.0212(11) 0.0323(12) 0.0250(12) 0.0034(9) 0.0043(9) 0.0077(9)
O11 0.0193(11) 0.0309(12) 0.0265(11) 0.0025(9) -0.0043(9) -0.0044(9)
O12 0.0213(11) 0.0319(12) 0.0280(12) 0.0086(9) -0.0060(9) -0.0046(9)
O13 0.0228(11) 0.0339(12) 0.0187(11) 0.0047(9) 0.0013(9) -0.0002(9)
O14 0.0233(12) 0.0462(14) 0.0246(12) 0.0061(10) -0.0015(9) -0.0005(10)
O15 0.0218(11) 0.0288(11) 0.0140(10) 0.0006(8) 0.0024(8) 0.0023(9)
O16 0.0184(10) 0.0255(11) 0.0208(11) 0.0033(8) 0.0042(8) 0.0042(9)
O17 0.0172(10) 0.0196(10) 0.0209(10) 0.0001(8) 0.0019(8) 0.0002(8)
O18 0.0176(10) 0.0259(11) 0.0192(10) -0.0010(8) 0.0012(8) 0.0008(9)
O19 0.0135(9) 0.0219(10) 0.0171(10) 0.0023(8) 0.0003(8) 0.0015(8)
O20 0.0146(10) 0.0251(11) 0.0189(10) 0.0017(8) 0.0013(8) 0.0006(8)
Fe1 0.0173(2) 0.0249(2) 0.0190(2) 0.00167(18) 0.00075(17) 0.00146(18)
Fe2 0.0164(2) 0.0235(2) 0.0168(2) -0.00046(17) 0.00254(17) 0.00136(17)
Fe3 0.0169(2) 0.0341(3) 0.0217(2) 0.00477(19) 0.00486(18) 0.00436(19)
Fe4 0.0152(2) 0.0269(2) 0.0189(2) 0.00226(18) 0.00197(17) 0.00211(18)
Fe5 0.0151(2) 0.0258(2) 0.0172(2) 0.00063(18) 0.00096(16) 0.00088(18)
N1 0.0232(15) 0.0259(15) 0.0245(15) -0.0014(11) -0.0019(12) 0.0001(12)
N2 0.0267(17) 0.050(2) 0.0323(17) 0.0076(14) 0.0112(13) 0.0138(14)
N3 0.0286(17) 0.0394(18) 0.0385(18) 0.0111(14) 0.0144(13) 0.0098(14)
N4 0.0192(14) 0.0336(15) 0.0240(14) -0.0002(12) 0.0001(11) -0.0001(12)
_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
C1 O2 1.260(3) . ?
C1 O1 1.276(3) . ?
C1 C2 1.527(4) . ?
C2 C3 1.513(4) . ?
C2 C5 1.526(4) . ?
C2 C4 1.541(4) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 O3 1.251(3) . ?
C6 O4 1.257(3) . ?
C6 C7 1.521(4) . ?
C7 C10 1.513(4) . ?
C7 C8 1.518(4) . ?
C7 C9 1.530(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 O5 1.244(3) . ?
C11 O6 1.263(3) . ?
C11 C12 1.527(4) . ?
C12 C13 1.494(5) . ?
C12 C14 1.516(4) . ?
C12 C15 1.524(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 O8 1.221(4) . ?
C16 O7 1.295(4) . ?
C16 C17 1.542(5) . ?
C17 C18 1.523(5) . ?
C17 C20 1.533(5) . ?
C17 C19 1.535(5) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O10 1.255(3) . ?
C21 O9 1.262(3) . ?
C21 C22 1.532(4) . ?
C22 C24 1.508(4) . ?
C22 C23 1.515(4) . ?
C22 C25 1.530(4) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 O11 1.255(3) . ?
C26 O12 1.255(3) . ?
C26 C27 1.535(4) . ?
C27 C28 1.503(4) . ?
C27 C30 1.518(4) . ?
C27 C29 1.565(5) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 O14 1.240(3) . ?
C31 O13 1.282(3) . ?
C31 C32 1.541(4) . ?
C32 C34 1.517(4) . ?
C32 C35 1.520(4) . ?
C32 C33 1.535(4) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 N1 1.469(4) . ?
C36 C37 1.504(4) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.525(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 O15 1.398(3) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 O16 1.407(3) . ?
C39 C40 1.484(4) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.436(4) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 N2 1.466(4) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 N3 1.471(4) . ?
C42 C43 1.500(4) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.517(4) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 O17 1.418(3) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 O18 1.426(3) . ?
C45 C46 1.510(4) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.511(4) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 N4 1.469(4) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
O1 Fe1 2.0656(18) . ?
O2 Fe2 2.0608(18) . ?
O3 Fe2 2.0654(19) . ?
O4 Fe3 2.015(2) . ?
O5 Fe2 2.0376(18) . ?
O6 Fe3 2.051(2) . ?
O7 Fe3 2.022(2) . ?
O9 Fe4 2.0413(19) . ?
O10 Fe1 2.0658(19) . ?
O11 Fe1 2.0611(19) . ?
O12 Fe4 2.0296(19) . ?
O13 Fe5 2.0463(18) . ?
O15 Fe1 1.9461(18) . ?
O15 Fe2 2.1171(17) . ?
O16 Fe5 1.9869(18) . ?
O16 Fe3 1.9885(18) . ?
O17 Fe4 1.9752(17) . ?
O17 Fe5 1.9847(17) . ?
O18 Fe5 2.0172(18) . ?
O18 Fe4 2.0198(18) . ?
O19 Fe4 1.8507(17) . ?
O19 Fe1 1.8776(16) . ?
O19 Fe2 1.9382(17) . ?
O20 Fe2 1.8892(17) . ?
O20 Fe3 1.9042(18) . ?
O20 Fe5 2.0111(17) . ?
Fe1 N1 2.124(2) . ?
Fe1 Fe2 2.9698(5) . ?
Fe3 N2 2.159(3) . ?
Fe4 N3 2.181(3) . ?
Fe5 N4 2.132(2) . ?
N1 H1N 0.844(17) . ?
N1 H2N 0.834(17) . ?
N2 H3N 0.854(17) . ?
N2 H4N 0.807(17) . ?
N3 H5N 0.825(17) . ?
N3 H6N 0.842(17) . ?
N4 H7N 0.881(17) . ?
N4 H8N 0.861(17) . ?
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
O2 C1 O1 125.1(3) . . ?
O2 C1 C2 118.2(2) . . ?
O1 C1 C2 116.7(3) . . ?
C3 C2 C5 111.0(3) . . ?
C3 C2 C1 108.1(2) . . ?
C5 C2 C1 111.1(2) . . ?
C3 C2 C4 109.7(3) . . ?
C5 C2 C4 109.1(3) . . ?
C1 C2 C4 107.7(2) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O3 C6 O4 125.1(3) . . ?
O3 C6 C7 118.9(3) . . ?
O4 C6 C7 116.0(3) . . ?
C10 C7 C8 109.4(3) . . ?
C10 C7 C6 109.4(3) . . ?
C8 C7 C6 111.7(3) . . ?
C10 C7 C9 108.3(3) . . ?
C8 C7 C9 110.0(3) . . ?
C6 C7 C9 107.9(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O5 C11 O6 125.7(3) . . ?
O5 C11 C12 118.0(3) . . ?
O6 C11 C12 116.1(3) . . ?
C13 C12 C14 111.1(3) . . ?
C13 C12 C11 110.3(3) . . ?
C14 C12 C11 106.9(3) . . ?
C13 C12 C15 109.1(3) . . ?
C14 C12 C15 110.0(3) . . ?
C11 C12 C15 109.4(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O8 C16 O7 124.3(3) . . ?
O8 C16 C17 121.5(3) . . ?
O7 C16 C17 114.2(3) . . ?
C18 C17 C20 108.5(4) . . ?
C18 C17 C19 109.4(3) . . ?
C20 C17 C19 111.3(3) . . ?
C18 C17 C16 108.9(3) . . ?
C20 C17 C16 109.3(3) . . ?
C19 C17 C16 109.4(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O10 C21 O9 125.6(3) . . ?
O10 C21 C22 118.5(3) . . ?
O9 C21 C22 115.9(3) . . ?
C24 C22 C23 109.7(3) . . ?
C24 C22 C25 109.4(3) . . ?
C23 C22 C25 108.9(3) . . ?
C24 C22 C21 111.7(3) . . ?
C23 C22 C21 110.2(2) . . ?
C25 C22 C21 106.9(2) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O11 C26 O12 125.8(3) . . ?
O11 C26 C27 117.9(3) . . ?
O12 C26 C27 116.0(3) . . ?
C28 C27 C30 110.4(3) . . ?
C28 C27 C26 111.0(3) . . ?
C30 C27 C26 111.7(3) . . ?
C28 C27 C29 110.6(3) . . ?
C30 C27 C29 108.0(3) . . ?
C26 C27 C29 105.0(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O14 C31 O13 124.2(3) . . ?
O14 C31 C32 120.2(3) . . ?
O13 C31 C32 115.6(2) . . ?
C34 C32 C35 109.2(3) . . ?
C34 C32 C33 108.2(3) . . ?
C35 C32 C33 110.7(2) . . ?
C34 C32 C31 111.6(2) . . ?
C35 C32 C31 111.1(2) . . ?
C33 C32 C31 106.0(2) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N1 C36 C37 111.1(2) . . ?
N1 C36 H36A 109.4 . . ?
C37 C36 H36A 109.4 . . ?
N1 C36 H36B 109.4 . . ?
C37 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
C36 C37 C38 114.6(3) . . ?
C36 C37 H37A 108.6 . . ?
C38 C37 H37A 108.6 . . ?
C36 C37 H37B 108.6 . . ?
C38 C37 H37B 108.6 . . ?
H37A C37 H37B 107.6 . . ?
O15 C38 C37 113.0(2) . . ?
O15 C38 H38A 109.0 . . ?
C37 C38 H38A 109.0 . . ?
O15 C38 H38B 109.0 . . ?
C37 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
O16 C39 C40 114.7(3) . . ?
O16 C39 H39A 108.6 . . ?
C40 C39 H39A 108.6 . . ?
O16 C39 H39B 108.6 . . ?
C40 C39 H39B 108.6 . . ?
H39A C39 H39B 107.6 . . ?
C41 C40 C39 120.0(3) . . ?
C41 C40 H40A 107.3 . . ?
C39 C40 H40A 107.3 . . ?
C41 C40 H40B 107.3 . . ?
C39 C40 H40B 107.3 . . ?
H40A C40 H40B 106.9 . . ?
C40 C41 N2 116.2(3) . . ?
C40 C41 H41A 108.2 . . ?
N2 C41 H41A 108.2 . . ?
C40 C41 H41B 108.2 . . ?
N2 C41 H41B 108.2 . . ?
H41A C41 H41B 107.4 . . ?
N3 C42 C43 112.7(2) . . ?
N3 C42 H42A 109.1 . . ?
C43 C42 H42A 109.1 . . ?
N3 C42 H42B 109.1 . . ?
C43 C42 H42B 109.1 . . ?
H42A C42 H42B 107.8 . . ?
C42 C43 C44 116.9(2) . . ?
C42 C43 H43A 108.1 . . ?
C44 C43 H43A 108.1 . . ?
C42 C43 H43B 108.1 . . ?
C44 C43 H43B 108.1 . . ?
H43A C43 H43B 107.3 . . ?
O17 C44 C43 111.9(2) . . ?
O17 C44 H44A 109.2 . . ?
C43 C44 H44A 109.2 . . ?
O17 C44 H44B 109.2 . . ?
C43 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
O18 C45 C46 112.3(2) . . ?
O18 C45 H45A 109.1 . . ?
C46 C45 H45A 109.1 . . ?
O18 C45 H45B 109.1 . . ?
C46 C45 H45B 109.1 . . ?
H45A C45 H45B 107.9 . . ?
C45 C46 C47 114.3(2) . . ?
C45 C46 H46A 108.7 . . ?
C47 C46 H46A 108.7 . . ?
C45 C46 H46B 108.7 . . ?
C47 C46 H46B 108.7 . . ?
H46A C46 H46B 107.6 . . ?
N4 C47 C46 111.5(2) . . ?
N4 C47 H47A 109.3 . . ?
C46 C47 H47A 109.3 . . ?
N4 C47 H47B 109.3 . . ?
C46 C47 H47B 109.3 . . ?
H47A C47 H47B 108.0 . . ?
C1 O1 Fe1 125.06(18) . . ?
C1 O2 Fe2 129.67(18) . . ?
C6 O3 Fe2 133.29(18) . . ?
C6 O4 Fe3 129.14(19) . . ?
C11 O5 Fe2 127.43(18) . . ?
C11 O6 Fe3 133.99(19) . . ?
C16 O7 Fe3 130.6(2) . . ?
C21 O9 Fe4 132.55(18) . . ?
C21 O10 Fe1 130.90(18) . . ?
C26 O11 Fe1 132.36(18) . . ?
C26 O12 Fe4 130.57(18) . . ?
C31 O13 Fe5 132.32(18) . . ?
C38 O15 Fe1 129.01(17) . . ?
C38 O15 Fe2 127.96(16) . . ?
Fe1 O15 Fe2 93.83(7) . . ?
C39 O16 Fe5 129.59(17) . . ?
C39 O16 Fe3 129.45(17) . . ?
Fe5 O16 Fe3 97.80(8) . . ?
C44 O17 Fe4 124.16(16) . . ?
C44 O17 Fe5 131.20(16) . . ?
Fe4 O17 Fe5 100.54(8) . . ?
C45 O18 Fe5 126.96(16) . . ?
C45 O18 Fe4 118.79(15) . . ?
Fe5 O18 Fe4 97.94(8) . . ?
Fe4 O19 Fe1 122.50(9) . . ?
Fe4 O19 Fe2 132.01(9) . . ?
Fe1 O19 Fe2 102.20(8) . . ?
Fe2 O20 Fe3 118.77(9) . . ?
Fe2 O20 Fe5 128.68(9) . . ?
Fe3 O20 Fe5 99.80(8) . . ?
O19 Fe1 O15 82.81(7) . . ?
O19 Fe1 O11 93.10(7) . . ?
O15 Fe1 O11 97.90(8) . . ?
O19 Fe1 O1 94.21(7) . . ?
O15 Fe1 O1 88.39(7) . . ?
O11 Fe1 O1 170.90(7) . . ?
O19 Fe1 O10 97.21(7) . . ?
O15 Fe1 O10 173.90(8) . . ?
O11 Fe1 O10 88.19(8) . . ?
O1 Fe1 O10 85.52(7) . . ?
O19 Fe1 N1 175.41(9) . . ?
O15 Fe1 N1 92.87(9) . . ?
O11 Fe1 N1 85.93(8) . . ?
O1 Fe1 N1 87.20(8) . . ?
O10 Fe1 N1 87.25(9) . . ?
O19 Fe1 Fe2 39.64(5) . . ?
O15 Fe1 Fe2 45.34(5) . . ?
O11 Fe1 Fe2 107.60(5) . . ?
O1 Fe1 Fe2 81.50(5) . . ?
O10 Fe1 Fe2 132.87(5) . . ?
N1 Fe1 Fe2 136.60(7) . . ?
O20 Fe2 O19 97.45(7) . . ?
O20 Fe2 O5 95.46(7) . . ?
O19 Fe2 O5 96.84(8) . . ?
O20 Fe2 O2 95.71(7) . . ?
O19 Fe2 O2 90.50(7) . . ?
O5 Fe2 O2 165.73(7) . . ?
O20 Fe2 O3 98.40(7) . . ?
O19 Fe2 O3 163.47(7) . . ?
O5 Fe2 O3 86.33(8) . . ?
O2 Fe2 O3 83.28(7) . . ?
O20 Fe2 O15 174.25(7) . . ?
O19 Fe2 O15 77.04(7) . . ?
O5 Fe2 O15 83.71(7) . . ?
O2 Fe2 O15 86.05(7) . . ?
O3 Fe2 O15 87.24(7) . . ?
O20 Fe2 Fe1 134.17(6) . . ?
O19 Fe2 Fe1 38.17(5) . . ?
O5 Fe2 Fe1 99.94(5) . . ?
O2 Fe2 Fe1 78.40(5) . . ?
O3 Fe2 Fe1 125.32(5) . . ?
O15 Fe2 Fe1 40.83(5) . . ?
O20 Fe3 O16 81.95(7) . . ?
O20 Fe3 O4 98.79(8) . . ?
O16 Fe3 O4 178.40(8) . . ?
O20 Fe3 O7 98.94(8) . . ?
O16 Fe3 O7 92.14(8) . . ?
O4 Fe3 O7 86.35(8) . . ?
O20 Fe3 O6 94.92(8) . . ?
O16 Fe3 O6 95.17(8) . . ?
O4 Fe3 O6 86.19(9) . . ?
O7 Fe3 O6 165.11(8) . . ?
O16 Fe3 N2 90.63(9) . . ?
O4 Fe3 N2 88.79(9) . . ?
O7 Fe3 N2 87.49(10) . . ?
O6 Fe3 N2 79.49(10) . . ?
O19 Fe4 O17 97.34(7) . . ?
O19 Fe4 O18 90.75(7) . . ?
O17 Fe4 O18 79.10(7) . . ?
O19 Fe4 O12 94.48(7) . . ?
O17 Fe4 O12 94.59(7) . . ?
O18 Fe4 O12 172.29(7) . . ?
O19 Fe4 O9 97.20(7) . . ?
O17 Fe4 O9 163.64(7) . . ?
O18 Fe4 O9 93.25(7) . . ?
O12 Fe4 O9 91.72(8) . . ?
O19 Fe4 N3 179.83(10) . . ?
O17 Fe4 N3 82.51(9) . . ?
O18 Fe4 N3 89.31(9) . . ?
O12 Fe4 N3 85.45(10) . . ?
O9 Fe4 N3 82.96(9) . . ?
O17 Fe5 O16 97.45(7) . . ?
O17 Fe5 O20 91.88(7) . . ?
O16 Fe5 O20 79.38(7) . . ?
O17 Fe5 O18 78.94(7) . . ?
O16 Fe5 O18 176.03(7) . . ?
O20 Fe5 O18 99.00(7) . . ?
O17 Fe5 O13 91.42(7) . . ?
O16 Fe5 O13 93.62(7) . . ?
O20 Fe5 O13 172.59(7) . . ?
O18 Fe5 O13 88.14(7) . . ?
O17 Fe5 N4 168.79(9) . . ?
O16 Fe5 N4 93.21(9) . . ?
O20 Fe5 N4 86.67(8) . . ?
O18 Fe5 N4 90.30(8) . . ?
O13 Fe5 N4 91.35(9) . . ?
C36 N1 Fe1 116.46(18) . . ?
C36 N1 H1N 107(2) . . ?
Fe1 N1 H1N 108(2) . . ?
C36 N1 H2N 106(2) . . ?
Fe1 N1 H2N 113(2) . . ?
H1N N1 H2N 107(3) . . ?
C41 N2 Fe3 119.8(2) . . ?
C41 N2 H3N 111(2) . . ?
Fe3 N2 H3N 106(2) . . ?
C41 N2 H4N 113(3) . . ?
Fe3 N2 H4N 103(3) . . ?
H3N N2 H4N 102(3) . . ?
C42 N3 Fe4 117.6(2) . . ?
C42 N3 H5N 108(2) . . ?
Fe4 N3 H5N 110(2) . . ?
C42 N3 H6N 100(2) . . ?
Fe4 N3 H6N 110(2) . . ?
H5N N3 H6N 110(3) . . ?
C47 N4 Fe5 117.41(18) . . ?
C47 N4 H7N 115.1(19) . . ?
Fe5 N4 H7N 109.5(19) . . ?
C47 N4 H8N 107(2) . . ?
Fe5 N4 H8N 107(2) . . ?
H7N N4 H8N 99(3) . . ?
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
O2 C1 C2 C3 -122.0(3) . . . . ?
O1 C1 C2 C5 -179.6(2) . . . . ?
O2 C1 C2 C4 119.5(3) . . . . ?
O3 C6 C7 C10 -137.0(3) . . . . ?
O4 C6 C7 C8 165.7(3) . . . . ?
O3 C6 C7 C9 105.4(3) . . . . ?
O6 C11 C12 C13 149.2(3) . . . . ?
O5 C11 C12 C14 86.2(3) . . . . ?
O6 C11 C12 C14 -89.9(3) . . . . ?
O6 C11 C12 C15 29.2(4) . . . . ?
O8 C16 C17 C18 126.5(4) . . . . ?
O8 C16 C17 C20 -115.2(4) . . . . ?
O7 C16 C17 C19 -172.8(3) . . . . ?
O9 C21 C22 C24 175.2(3) . . . . ?
O10 C21 C22 C23 -126.8(3) . . . . ?
O10 C21 C22 C25 115.0(3) . . . . ?
O12 C26 C27 C28 -160.8(3) . . . . ?
O11 C26 C27 C30 147.6(3) . . . . ?
O11 C26 C27 C29 -95.6(3) . . . . ?
O14 C31 C32 C34 -140.8(3) . . . . ?
O13 C31 C32 C35 164.2(3) . . . . ?
O14 C31 C32 C33 101.6(3) . . . . ?
C2 C1 O1 Fe1 175.32(17) . . . . ?
C2 C1 O2 Fe2 -172.96(17) . . . . ?
C7 C6 O3 Fe2 -172.33(19) . . . . ?
C7 C6 O4 Fe3 -168.2(2) . . . . ?
C12 C11 O5 Fe2 -158.8(2) . . . . ?
C12 C11 O6 Fe3 177.9(2) . . . . ?
C17 C16 O7 Fe3 147.3(2) . . . . ?
C22 C21 O9 Fe4 -176.82(18) . . . . ?
C22 C21 O10 Fe1 177.09(18) . . . . ?
C27 C26 O11 Fe1 -175.2(2) . . . . ?
C27 C26 O12 Fe4 -178.5(2) . . . . ?
C32 C31 O13 Fe5 149.21(19) . . . . ?
C37 C38 O15 Fe2 -174.69(18) . . . . ?
C40 C39 O16 Fe5 169.2(2) . . . . ?
C46 C45 O18 Fe4 -172.98(18) . . . . ?
Fe4 O19 Fe1 O15 -145.15(11) . . . . ?
Fe2 O19 Fe1 O11 114.16(8) . . . . ?
Fe4 O19 Fe1 O1 127.00(11) . . . . ?
Fe2 O19 Fe1 O10 -157.27(8) . . . . ?
Fe4 O19 Fe1 Fe2 -161.73(15) . . . . ?
C38 O15 Fe1 O19 -162.8(2) . . . . ?
C38 O15 Fe1 O11 105.1(2) . . . . ?
Fe2 O15 Fe1 O11 -106.98(7) . . . . ?
Fe2 O15 Fe1 O1 79.62(7) . . . . ?
Fe2 O15 Fe1 N1 166.73(8) . . . . ?
C38 O15 Fe1 Fe2 -147.9(3) . . . . ?
C26 O11 Fe1 O15 96.9(3) . . . . ?
C26 O11 Fe1 N1 -170.8(3) . . . . ?
C1 O1 Fe1 O10 135.4(2) . . . . ?
C1 O1 Fe1 N1 -137.1(2) . . . . ?
C21 O10 Fe1 O11 75.2(2) . . . . ?
C21 O10 Fe1 O1 -111.4(2) . . . . ?
C21 O10 Fe1 N1 161.2(2) . . . . ?
Fe3 O20 Fe2 O19 151.21(10) . . . . ?
Fe3 O20 Fe2 O2 -117.54(10) . . . . ?
Fe5 O20 Fe2 O2 108.96(12) . . . . ?
Fe5 O20 Fe2 O3 -167.02(11) . . . . ?
Fe3 O20 Fe2 Fe1 163.10(5) . . . . ?
Fe1 O19 Fe2 O20 166.16(8) . . . . ?
Fe4 O19 Fe2 O5 61.76(13) . . . . ?
Fe1 O19 Fe2 O5 -97.39(8) . . . . ?
Fe4 O19 Fe2 O2 -130.50(12) . . . . ?
Fe1 O19 Fe2 O2 70.34(8) . . . . ?
Fe4 O19 Fe2 O3 162.0(2) . . . . ?
Fe4 O19 Fe2 O15 143.67(13) . . . . ?
Fe4 O19 Fe2 Fe1 159.16(17) . . . . ?
C11 O5 Fe2 O19 -140.2(2) . . . . ?
C11 O5 Fe2 O2 99.4(4) . . . . ?
C11 O5 Fe2 O3 56.1(2) . . . . ?
C11 O5 Fe2 O15 143.7(2) . . . . ?
C11 O5 Fe2 Fe1 -178.7(2) . . . . ?
C1 O2 Fe2 O20 -138.4(2) . . . . ?
C1 O2 Fe2 O3 123.8(2) . . . . ?
C6 O3 Fe2 O19 168.0(3) . . . . ?
C6 O3 Fe2 O5 -90.3(3) . . . . ?
C6 O3 Fe2 O2 99.5(3) . . . . ?
C6 O3 Fe2 O15 -174.1(3) . . . . ?
C6 O3 Fe2 Fe1 170.1(2) . . . . ?
C38 O15 Fe2 O19 163.1(2) . . . . ?
C38 O15 Fe2 O5 -98.4(2) . . . . ?
Fe1 O15 Fe2 O5 113.15(8) . . . . ?
Fe1 O15 Fe2 O2 -76.80(8) . . . . ?
Fe1 O15 Fe2 O3 -160.25(8) . . . . ?
C38 O15 Fe2 Fe1 148.5(3) . . . . ?
O15 Fe1 Fe2 O20 -175.86(11) . . . . ?
O11 Fe1 Fe2 O20 -92.21(10) . . . . ?
O1 Fe1 Fe2 O20 87.95(9) . . . . ?
N1 Fe1 Fe2 O20 164.66(12) . . . . ?
O15 Fe1 Fe2 O19 -156.55(11) . . . . ?
O1 Fe1 Fe2 O19 107.26(9) . . . . ?
N1 Fe1 Fe2 O19 -176.03(13) . . . . ?
O19 Fe1 Fe2 O5 88.44(10) . . . . ?
O1 Fe1 Fe2 O5 -164.30(7) . . . . ?
O10 Fe1 Fe2 O5 119.97(9) . . . . ?
N1 Fe1 Fe2 O5 -87.60(11) . . . . ?
O19 Fe1 Fe2 O2 -105.99(10) . . . . ?
O15 Fe1 Fe2 O2 97.47(9) . . . . ?
O11 Fe1 Fe2 O2 -178.89(8) . . . . ?
N1 Fe1 Fe2 O2 77.98(11) . . . . ?
O19 Fe1 Fe2 O3 -179.02(11) . . . . ?
O11 Fe1 Fe2 O3 108.08(9) . . . . ?
O10 Fe1 Fe2 O3 -147.48(10) . . . . ?
O19 Fe1 Fe2 O15 156.55(11) . . . . ?
O11 Fe1 Fe2 O15 83.64(9) . . . . ?
O1 Fe1 Fe2 O15 -96.19(9) . . . . ?
O10 Fe1 Fe2 O15 -171.92(11) . . . . ?
Fe2 O20 Fe3 O16 -136.98(11) . . . . ?
Fe5 O20 Fe3 O4 -170.62(8) . . . . ?
Fe2 O20 Fe3 O7 132.11(10) . . . . ?
Fe5 O20 Fe3 O7 -82.96(8) . . . . ?
Fe5 O20 Fe3 O6 102.49(8) . . . . ?
C39 O16 Fe3 O20 -169.1(2) . . . . ?
C39 O16 Fe3 O7 -70.3(2) . . . . ?
Fe5 O16 Fe3 O7 90.73(8) . . . . ?
C39 O16 Fe3 O6 96.7(2) . . . . ?
Fe5 O16 Fe3 O6 -102.26(8) . . . . ?
Fe5 O16 Fe3 N2 178.24(10) . . . . ?
C6 O4 Fe3 O7 -135.5(3) . . . . ?
C6 O4 Fe3 N2 136.9(3) . . . . ?
C16 O7 Fe3 O20 -140.1(3) . . . . ?
C16 O7 Fe3 O16 137.7(3) . . . . ?
C11 O6 Fe3 O16 92.6(3) . . . . ?
C11 O6 Fe3 O4 -88.2(3) . . . . ?
C11 O6 Fe3 O7 -148.3(3) . . . . ?
C11 O6 Fe3 N2 -177.7(3) . . . . ?
Fe1 O19 Fe4 O17 146.74(10) . . . . ?
Fe1 O19 Fe4 O18 -134.16(11) . . . . ?
Fe2 O19 Fe4 O12 -104.13(13) . . . . ?
Fe2 O19 Fe4 O9 163.57(12) . . . . ?
C44 O17 Fe4 O19 -125.62(19) . . . . ?
Fe5 O17 Fe4 O19 75.00(8) . . . . ?
C44 O17 Fe4 O18 145.03(19) . . . . ?
Fe5 O17 Fe4 O12 170.13(8) . . . . ?
Fe5 O17 Fe4 O9 -77.5(3) . . . . ?
Fe5 O17 Fe4 N3 -105.08(10) . . . . ?
C45 O18 Fe4 O19 56.96(19) . . . . ?
Fe5 O18 Fe4 O19 -83.33(8) . . . . ?
C45 O18 Fe4 O17 154.30(19) . . . . ?
Fe5 O18 Fe4 O9 179.42(8) . . . . ?
C45 O18 Fe4 N3 -123.20(19) . . . . ?
C26 O12 Fe4 O17 -122.0(2) . . . . ?
C26 O12 Fe4 N3 155.9(3) . . . . ?
C21 O9 Fe4 O17 170.1(3) . . . . ?
C21 O9 Fe4 O18 108.8(2) . . . . ?
C21 O9 Fe4 N3 -162.3(3) . . . . ?
Fe4 O17 Fe5 O16 -163.97(7) . . . . ?
C44 O17 Fe5 O20 118.4(2) . . . . ?
Fe4 O17 Fe5 O20 -84.44(8) . . . . ?
C44 O17 Fe5 O18 -142.8(2) . . . . ?
Fe4 O17 Fe5 O13 102.19(8) . . . . ?
C44 O17 Fe5 N4 -159.3(4) . . . . ?
C39 O16 Fe5 O17 -100.8(2) . . . . ?
Fe3 O16 Fe5 O17 98.15(8) . . . . ?
C39 O16 Fe5 O20 168.7(2) . . . . ?
Fe3 O16 Fe5 O13 -169.93(8) . . . . ?
C39 O16 Fe5 N4 82.6(2) . . . . ?
Fe3 O16 Fe5 N4 -78.37(9) . . . . ?
Fe3 O20 Fe5 O17 -105.24(8) . . . . ?
Fe2 O20 Fe5 O16 131.80(13) . . . . ?
Fe3 O20 Fe5 O18 175.66(7) . . . . ?
Fe2 O20 Fe5 N4 -134.30(13) . . . . ?
C45 O18 Fe5 O17 -149.5(2) . . . . ?
Fe4 O18 Fe5 O20 76.22(8) . . . . ?
C45 O18 Fe5 O13 118.72(19) . . . . ?
Fe4 O18 Fe5 O13 -105.76(8) . . . . ?
Fe4 O18 Fe5 N4 162.89(9) . . . . ?
C31 O13 Fe5 O17 176.3(2) . . . . ?
C31 O13 Fe5 O18 -104.9(2) . . . . ?
O11 Fe1 N1 C36 -123.8(2) . . . . ?
O10 Fe1 N1 C36 147.8(2) . . . . ?
O4 Fe3 N2 C41 160.1(3) . . . . ?
O6 Fe3 N2 C41 -113.6(3) . . . . ?
O18 Fe4 N3 C42 -128.6(2) . . . . ?
O9 Fe4 N3 C42 138.1(2) . . . . ?
O16 Fe5 N4 C47 146.4(2) . . . . ?
O13 Fe5 N4 C47 -119.8(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.597
_refine_diff_density_min -0.388
_refine_diff_density_rms 0.072
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
N1 H2N O14 0.834(17) 2.181(18) 2.992(3) 164(3) 4_565
N2 H4N O8 0.807(17) 2.21(3) 2.837(4) 135(3) .
N4 H7N O14 0.881(17) 2.18(2) 2.940(3) 144(3) .
N4 H8N O7 0.861(17) 2.09(2) 2.902(3) 158(3) .
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 0.000 0.000 0.500 204 33 ' '
2 0.000 0.500 0.500 24 2 ' '
3 0.500 0.500 0.000 204 33 ' '
4 0.500 0.000 0.000 24 2 ' '
_platon_squeeze_details
;
The crystal structure contains lattice water molecules which
appear to be highly disordered and it was not possible to model
their position and distribution reliably. Therefore, the SQUEEZE
procedure of PLATON (van der Sluis & Spek, 1990; Spek, 2001)
was employed to remove the contribution of the electron density
associated with the disordered solvent from the intensity data.
The solvent-free model and intensity data were used for the final
results reported here.
;
# start Validation Reply Form
_vrf_PLAT220_ck3-sqz
;
RESPONSE: All atomic species have been correctly identified.
However, this alert is due to the higher thermal ellipsoids of some
carbon and oxygen atoms of the pivalic ligands of the complex.
;
_vrf_PLAT605_ck3-sqz
;
PROBLEM: _Structure Contains Solvent Accessible VOIDS of . 212.00 A**3
RESPONSE: The crystal structure contains some lattice water molecules
which appear to be highly disordered and it was not possible to model
their position and distribution reliably. Therefore, the SQUEEZE
procedure of PLATON (van der Sluis & Spek, 1990; Spek, 2001)
was employed to remove the contribution of the electron density
associated with the disordered solvent from the intensity data.
The solvent-free model and intensity data were used for the final
results reported here.
;
data_ck7-sqz
_database_code_depnum_ccdc_archive 'CCDC 836724'
#TrackingRef '- 1.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C61 H67 Fe5 N4 O20, C2 H3 N'
_chemical_formula_sum 'C63 H70 Fe5 N5 O20'
_chemical_formula_weight 1496.49
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'
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 12.2398(2)
_cell_length_b 25.8362(4)
_cell_length_c 21.8856(3)
_cell_angle_alpha 90.00
_cell_angle_beta 91.4364(13)
_cell_angle_gamma 90.00
_cell_volume 6918.71(18)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 17765
_cell_measurement_theta_min 3.0162
_cell_measurement_theta_max 27.4999
_exptl_crystal_description prism
_exptl_crystal_colour grey-brown
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.11
_exptl_crystal_size_min 0.07
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.437
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3092
_exptl_absorpt_coefficient_mu 1.097
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.874
_exptl_absorpt_correction_T_max 0.930
_exptl_absorpt_process_details
'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur-3 with Sapphire CCD'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 16.0288
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 55637
_diffrn_reflns_av_R_equivalents 0.0481
_diffrn_reflns_av_sigmaI/netI 0.0783
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -33
_diffrn_reflns_limit_k_max 31
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 3.03
_diffrn_reflns_theta_max 27.50
_reflns_number_total 15800
_reflns_number_gt 10049
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics
;
PLATON (Spek, 2008), ORTEP-3 (Farrugia, 1997)
;
_computing_publication_material 'WINGX (Farrugia, 1999)'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436.
Farrugia, L. J. (1997). ORTEP-3 for Windows. J.Appl. Cryst.
30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838.
Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford
Diffraction Ltd, Abingdon, Oxford, England.
Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany.
Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands.
;
_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^)+(0.0322P)^2^] 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 15800
_refine_ls_number_parameters 873
_refine_ls_number_restraints 29
_refine_ls_R_factor_all 0.0655
_refine_ls_R_factor_gt 0.0347
_refine_ls_wR_factor_ref 0.0747
_refine_ls_wR_factor_gt 0.0709
_refine_ls_goodness_of_fit_ref 0.912
_refine_ls_restrained_S_all 0.914
_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
Fe1 Fe 0.59194(3) 0.231776(13) 0.492081(16) 0.01655(8) Uani 1 1 d . . .
Fe2 Fe 0.83303(3) 0.241420(13) 0.495384(16) 0.01590(8) Uani 1 1 d . . .
Fe3 Fe 1.08553(3) 0.204083(13) 0.508319(16) 0.01651(8) Uani 1 1 d . . .
Fe4 Fe 0.71057(3) 0.137737(13) 0.571448(15) 0.01627(8) Uani 1 1 d . . .
Fe5 Fe 0.95011(3) 0.156673(13) 0.604903(16) 0.01658(8) Uani 1 1 d . . .
O1 O 0.60454(12) 0.29738(6) 0.54508(7) 0.0211(4) Uani 1 1 d . . .
O2 O 0.78874(12) 0.30213(6) 0.55075(7) 0.0215(4) Uani 1 1 d . . .
O3 O 0.92384(12) 0.29871(6) 0.45384(7) 0.0208(4) Uani 1 1 d . . .
O4 O 1.08103(12) 0.25640(6) 0.43894(7) 0.0194(4) Uani 1 1 d . . .
O5 O 0.86917(12) 0.19307(6) 0.42509(7) 0.0194(4) Uani 1 1 d . . .
O6 O 1.02957(12) 0.15280(6) 0.44401(7) 0.0183(4) Uani 1 1 d . . .
O7 O 1.14590(12) 0.26057(6) 0.56287(7) 0.0213(4) Uani 1 1 d . . .
O8 O 1.28258(13) 0.29673(7) 0.51187(8) 0.0285(4) Uani 1 1 d . . .
O9 O 0.57085(12) 0.15411(6) 0.61785(7) 0.0192(4) Uani 1 1 d . . .
O10 O 0.48076(12) 0.20975(6) 0.55597(7) 0.0203(4) Uani 1 1 d . . .
O11 O 0.55583(12) 0.16561(6) 0.44272(7) 0.0192(4) Uani 1 1 d . . .
O12 O 0.62913(12) 0.10151(6) 0.49995(7) 0.0196(4) Uani 1 1 d . . .
O13 O 0.99324(13) 0.10217(6) 0.66594(7) 0.0224(4) Uani 1 1 d . . .
O14 O 0.86154(13) 0.06924(6) 0.72454(7) 0.0233(4) Uani 1 1 d . . .
O15 O 0.70147(12) 0.26066(6) 0.43868(7) 0.0175(4) Uani 1 1 d . . .
O16 O 1.09691(12) 0.14673(6) 0.56871(7) 0.0170(4) Uani 1 1 d . . .
O17 O 0.85678(12) 0.11240(6) 0.54898(7) 0.0165(4) Uani 1 1 d . . .
O18 O 0.80512(12) 0.16772(6) 0.64008(7) 0.0186(4) Uani 1 1 d . A .
O19 O 0.71477(12) 0.20026(6) 0.52947(7) 0.0161(4) Uani 1 1 d . . .
O20 O 0.94643(12) 0.21392(6) 0.54464(7) 0.0157(4) Uani 1 1 d . . .
C1 C 0.69398(19) 0.31767(9) 0.56361(11) 0.0196(6) Uani 1 1 d . . .
C2 C 0.68683(19) 0.36329(10) 0.60502(11) 0.0219(6) Uani 1 1 d . . .
C3 C 0.5884(2) 0.37598(11) 0.63141(13) 0.0380(8) Uani 1 1 d . . .
H3 H 0.5261 0.3565 0.6224 0.046 Uiso 1 1 calc R . .
C4 C 0.5828(2) 0.41753(13) 0.67104(15) 0.0497(9) Uani 1 1 d . . .
H4 H 0.5168 0.4257 0.6888 0.060 Uiso 1 1 calc R . .
C5 C 0.6737(2) 0.44684(12) 0.68440(14) 0.0427(8) Uani 1 1 d . . .
H5 H 0.6698 0.4745 0.7114 0.051 Uiso 1 1 calc R . .
C6 C 0.7713(2) 0.43479(11) 0.65722(14) 0.0388(8) Uani 1 1 d . . .
H6 H 0.8329 0.4549 0.6654 0.047 Uiso 1 1 calc R . .
C7 C 0.7779(2) 0.39329(10) 0.61823(13) 0.0328(7) Uani 1 1 d . . .
H7 H 0.8442 0.3853 0.6006 0.039 Uiso 1 1 calc R . .
C8 C 1.01766(19) 0.29507(9) 0.43221(11) 0.0187(5) Uani 1 1 d . . .
C9 C 1.05862(18) 0.33891(9) 0.39446(11) 0.0185(5) Uani 1 1 d . . .
C10 C 0.9996(2) 0.38478(10) 0.38955(13) 0.0292(6) Uani 1 1 d . . .
H10 H 0.9352 0.3886 0.4107 0.035 Uiso 1 1 calc R . .
C11 C 1.0363(2) 0.42464(11) 0.35343(14) 0.0362(7) Uani 1 1 d . . .
H11 H 0.9967 0.4553 0.3505 0.043 Uiso 1 1 calc R . .
C12 C 1.1319(2) 0.41906(11) 0.32152(13) 0.0323(7) Uani 1 1 d . . .
H12 H 1.1561 0.4459 0.2969 0.039 Uiso 1 1 calc R . .
C13 C 1.1912(2) 0.37386(10) 0.32615(12) 0.0296(7) Uani 1 1 d . . .
H13 H 1.2553 0.3701 0.3047 0.036 Uiso 1 1 calc R . .
C14 C 1.1551(2) 0.33409(10) 0.36285(12) 0.0259(6) Uani 1 1 d . . .
H14 H 1.1959 0.3038 0.3664 0.031 Uiso 1 1 calc R . .
C15 C 0.93739(19) 0.15726(9) 0.41685(11) 0.0174(5) Uani 1 1 d . . .
C16 C 0.90676(19) 0.11787(9) 0.36969(11) 0.0179(5) Uani 1 1 d . . .
C17 C 0.80474(19) 0.11962(10) 0.34099(11) 0.0233(6) Uani 1 1 d . . .
H17 H 0.7554 0.1453 0.3515 0.028 Uiso 1 1 calc R . .
C18 C 0.7758(2) 0.08379(10) 0.29720(12) 0.0307(7) Uani 1 1 d . . .
H18 H 0.7072 0.0853 0.2780 0.037 Uiso 1 1 calc R . .
C19 C 0.8486(2) 0.04566(10) 0.28174(12) 0.0322(7) Uani 1 1 d . . .
H19 H 0.8291 0.0214 0.2520 0.039 Uiso 1 1 calc R . .
C20 C 0.9504(2) 0.04326(10) 0.31022(12) 0.0319(7) Uani 1 1 d . . .
H20 H 0.9992 0.0173 0.2999 0.038 Uiso 1 1 calc R . .
C21 C 0.9797(2) 0.07943(10) 0.35411(12) 0.0262(6) Uani 1 1 d . . .
H21 H 1.0483 0.0779 0.3732 0.031 Uiso 1 1 calc R . .
C22 C 1.21018(18) 0.29850(9) 0.54995(11) 0.0187(5) Uani 1 1 d . . .
C23 C 1.19279(19) 0.34725(9) 0.58488(11) 0.0218(6) Uani 1 1 d . . .
C24 C 1.0946(2) 0.35756(10) 0.61252(12) 0.0304(7) Uani 1 1 d . . .
H24 H 1.0374 0.3340 0.6091 0.036 Uiso 1 1 calc R . .
C25 C 1.0815(2) 0.40275(11) 0.64510(14) 0.0383(8) Uani 1 1 d . . .
H25 H 1.0155 0.4096 0.6636 0.046 Uiso 1 1 calc R . .
C26 C 1.1660(2) 0.43773(11) 0.65027(13) 0.0368(7) Uani 1 1 d . . .
H26 H 1.1569 0.4681 0.6724 0.044 Uiso 1 1 calc R . .
C27 C 1.2636(2) 0.42801(10) 0.62286(13) 0.0356(7) Uani 1 1 d . . .
H27 H 1.3206 0.4517 0.6265 0.043 Uiso 1 1 calc R . .
C28 C 1.2770(2) 0.38316(10) 0.59005(12) 0.0284(6) Uani 1 1 d . . .
H28 H 1.3429 0.3768 0.5712 0.034 Uiso 1 1 calc R . .
C29 C 0.50080(18) 0.18941(9) 0.60752(11) 0.0180(5) Uani 1 1 d . . .
C30 C 0.43762(18) 0.20838(9) 0.66081(11) 0.0187(5) Uani 1 1 d . . .
C31 C 0.4387(2) 0.18115(10) 0.71570(11) 0.0259(6) Uani 1 1 d . . .
H31 H 0.4769 0.1501 0.7191 0.031 Uiso 1 1 calc R . .
C32 C 0.3830(2) 0.20016(11) 0.76513(12) 0.0306(7) Uani 1 1 d . . .
H32 H 0.3832 0.1817 0.8016 0.037 Uiso 1 1 calc R . .
C33 C 0.3271(2) 0.24661(11) 0.76036(13) 0.0338(7) Uani 1 1 d . . .
H33 H 0.2891 0.2592 0.7935 0.041 Uiso 1 1 calc R . .
C34 C 0.3277(2) 0.27409(11) 0.70646(13) 0.0340(7) Uani 1 1 d . . .
H34 H 0.2916 0.3057 0.7036 0.041 Uiso 1 1 calc R . .
C35 C 0.3820(2) 0.25485(10) 0.65653(12) 0.0256(6) Uani 1 1 d . . .
H35 H 0.3811 0.2733 0.6200 0.031 Uiso 1 1 calc R . .
C36 C 0.58154(18) 0.11888(10) 0.45228(11) 0.0181(5) Uani 1 1 d . . .
C37 C 0.55206(18) 0.08119(9) 0.40238(11) 0.0198(6) Uani 1 1 d . . .
C38 C 0.48749(19) 0.09653(10) 0.35322(11) 0.0255(6) Uani 1 1 d . . .
H38 H 0.4604 0.1301 0.3514 0.031 Uiso 1 1 calc R . .
C39 C 0.4628(2) 0.06192(11) 0.30644(12) 0.0328(7) Uani 1 1 d . . .
H39 H 0.4183 0.0722 0.2736 0.039 Uiso 1 1 calc R . .
C40 C 0.5039(2) 0.01239(11) 0.30852(13) 0.0339(7) Uani 1 1 d . . .
H40 H 0.4882 -0.0105 0.2767 0.041 Uiso 1 1 calc R . .
C41 C 0.5677(2) -0.00329(11) 0.35709(13) 0.0341(7) Uani 1 1 d . . .
H41 H 0.5953 -0.0368 0.3584 0.041 Uiso 1 1 calc R . .
C42 C 0.5914(2) 0.03098(10) 0.40462(12) 0.0276(6) Uani 1 1 d . . .
H42 H 0.6338 0.0201 0.4380 0.033 Uiso 1 1 calc R . .
C43 C 0.9563(2) 0.08356(9) 0.71608(11) 0.0201(6) Uani 1 1 d . . .
C44 C 1.0410(2) 0.07747(9) 0.76668(11) 0.0204(6) Uani 1 1 d . . .
C45 C 1.1507(2) 0.08786(9) 0.75686(13) 0.0285(6) Uani 1 1 d . . .
H45 H 1.1724 0.0995 0.7188 0.034 Uiso 1 1 calc R . .
C46 C 1.2279(2) 0.08087(10) 0.80389(15) 0.0374(8) Uani 1 1 d . . .
H46 H 1.3012 0.0875 0.7970 0.045 Uiso 1 1 calc R . .
C47 C 1.1968(3) 0.06439(10) 0.86002(15) 0.0417(8) Uani 1 1 d . . .
H47 H 1.2489 0.0596 0.8912 0.050 Uiso 1 1 calc R . .
C48 C 1.0873(3) 0.05471(10) 0.87063(13) 0.0379(7) Uani 1 1 d . . .
H48 H 1.0657 0.0440 0.9091 0.045 Uiso 1 1 calc R . .
C49 C 1.0107(2) 0.06099(9) 0.82394(12) 0.0274(6) Uani 1 1 d . . .
H49 H 0.9376 0.0540 0.8311 0.033 Uiso 1 1 calc R . .
C50 C 0.48327(19) 0.31179(9) 0.40267(12) 0.0238(6) Uani 1 1 d . . .
H50A H 0.4929 0.3410 0.4301 0.029 Uiso 1 1 calc R . .
H50B H 0.4210 0.3190 0.3757 0.029 Uiso 1 1 calc R . .
C51 C 0.58480(19) 0.30560(10) 0.36491(11) 0.0221(6) Uani 1 1 d . . .
H51A H 0.5798 0.2732 0.3425 0.027 Uiso 1 1 calc R . .
H51B H 0.5871 0.3335 0.3353 0.027 Uiso 1 1 calc R . .
C52 C 0.68993(19) 0.30595(9) 0.40274(11) 0.0220(6) Uani 1 1 d . . .
H52A H 0.7514 0.3087 0.3758 0.026 Uiso 1 1 calc R . .
H52B H 0.6909 0.3360 0.4293 0.026 Uiso 1 1 calc R . .
C53 C 1.28372(19) 0.12996(9) 0.48310(12) 0.0244(6) Uani 1 1 d . . .
H53A H 1.3595 0.1280 0.4714 0.029 Uiso 1 1 calc R . .
H53B H 1.2402 0.1102 0.4537 0.029 Uiso 1 1 calc R . .
C54 C 1.27227(19) 0.10703(10) 0.54504(12) 0.0262(6) Uani 1 1 d . . .
H54A H 1.3089 0.1294 0.5747 0.031 Uiso 1 1 calc R . .
H54B H 1.3093 0.0738 0.5461 0.031 Uiso 1 1 calc R . .
C55 C 1.15516(18) 0.09916(9) 0.56419(12) 0.0231(6) Uani 1 1 d . . .
H55A H 1.1178 0.0770 0.5346 0.028 Uiso 1 1 calc R . .
H55B H 1.1552 0.0817 0.6035 0.028 Uiso 1 1 calc R . .
C56 C 0.7314(2) 0.01693(9) 0.58930(12) 0.0254(6) Uani 1 1 d . . .
H56A H 0.6832 0.0112 0.5541 0.030 Uiso 1 1 calc R . .
H56B H 0.7233 -0.0121 0.6170 0.030 Uiso 1 1 calc R . .
C57 C 0.84833(19) 0.01949(9) 0.56873(12) 0.0234(6) Uani 1 1 d . . .
H57A H 0.8668 -0.0134 0.5502 0.028 Uiso 1 1 calc R . .
H57B H 0.8958 0.0240 0.6045 0.028 Uiso 1 1 calc R . .
C58 C 0.87168(19) 0.06229(9) 0.52371(11) 0.0207(6) Uani 1 1 d . . .
H58A H 0.9464 0.0590 0.5104 0.025 Uiso 1 1 calc R . .
H58B H 0.8237 0.0584 0.4881 0.025 Uiso 1 1 calc R . .
C59 C 0.9542(2) 0.24574(12) 0.70098(15) 0.0470(9) Uani 1 1 d . . .
H59A H 0.9474 0.2308 0.7414 0.056 Uiso 0.285(6) 1 calc PR A 1
H59B H 0.9928 0.2782 0.7065 0.056 Uiso 0.285(6) 1 calc PR A 1
H59C H 0.9962 0.2618 0.7341 0.056 Uiso 0.715(6) 1 calc PR A 2
H59D H 0.9294 0.2732 0.6737 0.056 Uiso 0.715(6) 1 calc PR A 2
C60A C 0.8566(7) 0.2573(3) 0.6822(4) 0.018(2) Uani 0.285(6) 1 d P A 1
H60A H 0.8605 0.2723 0.6417 0.021 Uiso 0.285(6) 1 calc PR A 1
H60B H 0.8278 0.2836 0.7091 0.021 Uiso 0.285(6) 1 calc PR A 1
C60B C 0.8583(3) 0.22105(16) 0.72668(17) 0.0307(12) Uani 0.715(6) 1 d P A 2
H60C H 0.8278 0.2440 0.7569 0.037 Uiso 0.715(6) 1 calc PR A 2
H60D H 0.8812 0.1896 0.7475 0.037 Uiso 0.715(6) 1 calc PR A 2
C61 C 0.7693(2) 0.20764(12) 0.67933(13) 0.0358(7) Uani 1 1 d . . .
H61A H 0.7612 0.1938 0.7202 0.043 Uiso 0.285(6) 1 calc PR A 1
H61B H 0.6982 0.2199 0.6650 0.043 Uiso 0.285(6) 1 calc PR A 1
H61C H 0.7041 0.1964 0.6999 0.043 Uiso 0.715(6) 1 calc PR A 2
H61D H 0.7509 0.2382 0.6554 0.043 Uiso 0.715(6) 1 calc PR A 2
N1 N 0.46111(16) 0.26452(8) 0.43883(10) 0.0190(5) Uani 1 1 d . . .
H1N H 0.409(2) 0.2734(10) 0.4623(12) 0.029 Uiso 1 1 d . . .
H2N H 0.440(2) 0.2433(10) 0.4122(12) 0.029 Uiso 1 1 d . . .
N2 N 1.24769(17) 0.18473(8) 0.48188(10) 0.0191(5) Uani 1 1 d . . .
H3N H 1.252(2) 0.1943(10) 0.4451(12) 0.029 Uiso 1 1 d . . .
H4N H 1.295(2) 0.2001(10) 0.5035(12) 0.029 Uiso 1 1 d . . .
N3 N 0.69937(18) 0.06524(8) 0.62043(10) 0.0220(5) Uani 1 1 d D . .
H5N H 0.7377(19) 0.0691(10) 0.6522(9) 0.033 Uiso 1 1 d D . .
H6N H 0.633(2) 0.0613(10) 0.6354(12) 0.033 Uiso 1 1 d . . .
N4 N 1.02689(17) 0.21154(9) 0.66734(10) 0.0218(5) Uani 1 1 d D A .
H7N H 1.0658(19) 0.2287(9) 0.6463(11) 0.033 Uiso 1 1 d D . .
H8N H 1.070(2) 0.1944(10) 0.6922(12) 0.033 Uiso 1 1 d . . .
N5 N 0.2805(3) 0.19220(13) 0.34069(13) 0.0678(9) Uani 1 1 d U . .
C62 C 0.1988(3) 0.19422(13) 0.31581(15) 0.0472(9) Uani 1 1 d U . .
C63 C 0.0956(3) 0.19886(14) 0.28383(16) 0.0600(10) Uani 1 1 d U . .
H63A H 0.0396 0.2066 0.3124 0.090 Uiso 1 1 calc R . .
H63B H 0.0786 0.1669 0.2634 0.090 Uiso 1 1 calc R . .
H63C H 0.0994 0.2262 0.2543 0.090 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
Fe1 0.01291(18) 0.01740(19) 0.0194(2) 0.00177(15) 0.00220(14) 0.00070(14)
Fe2 0.01225(17) 0.01531(19) 0.0203(2) -0.00009(15) 0.00285(14) 0.00057(14)
Fe3 0.01284(17) 0.01523(19) 0.0216(2) -0.00049(15) 0.00225(14) 0.00057(14)
Fe4 0.01370(17) 0.01615(19) 0.01901(19) 0.00123(15) 0.00117(14) -0.00006(14)
Fe5 0.01392(18) 0.01664(19) 0.0192(2) -0.00058(15) 0.00099(14) 0.00036(14)
O1 0.0161(9) 0.0204(10) 0.0270(10) -0.0044(8) 0.0029(7) 0.0015(7)
O2 0.0163(9) 0.0191(10) 0.0292(10) -0.0053(8) 0.0038(7) 0.0006(7)
O3 0.0153(9) 0.0170(9) 0.0301(10) 0.0032(8) 0.0047(7) 0.0005(7)
O4 0.0160(9) 0.0173(9) 0.0250(10) 0.0029(7) 0.0034(7) 0.0019(7)
O5 0.0168(9) 0.0195(10) 0.0218(10) -0.0014(7) 0.0011(7) 0.0048(7)
O6 0.0166(9) 0.0176(9) 0.0207(9) -0.0034(7) -0.0003(7) 0.0014(7)
O7 0.0209(9) 0.0190(9) 0.0242(10) -0.0015(8) 0.0015(7) -0.0053(7)
O8 0.0183(9) 0.0282(11) 0.0395(12) -0.0043(9) 0.0086(8) -0.0029(8)
O9 0.0144(8) 0.0210(10) 0.0224(10) 0.0032(7) 0.0039(7) 0.0020(7)
O10 0.0148(9) 0.0261(10) 0.0201(10) 0.0039(8) 0.0025(7) -0.0001(7)
O11 0.0189(9) 0.0181(10) 0.0206(10) -0.0001(7) -0.0009(7) -0.0004(7)
O12 0.0195(9) 0.0204(10) 0.0189(10) 0.0027(7) -0.0025(7) -0.0018(7)
O13 0.0223(9) 0.0226(10) 0.0225(10) 0.0046(8) 0.0029(8) 0.0037(7)
O14 0.0188(9) 0.0274(10) 0.0237(10) 0.0031(8) 0.0008(7) 0.0001(8)
O15 0.0157(8) 0.0173(9) 0.0196(9) 0.0048(7) 0.0032(7) 0.0011(7)
O16 0.0137(8) 0.0144(9) 0.0229(10) -0.0005(7) 0.0006(7) 0.0023(7)
O17 0.0172(9) 0.0135(9) 0.0191(9) -0.0030(7) 0.0010(7) 0.0003(7)
O18 0.0153(9) 0.0226(10) 0.0179(9) -0.0028(7) 0.0014(7) 0.0005(7)
O19 0.0121(8) 0.0160(9) 0.0204(9) 0.0026(7) 0.0018(7) -0.0012(7)
O20 0.0136(8) 0.0156(9) 0.0177(9) -0.0009(7) 0.0011(7) -0.0004(7)
C1 0.0193(14) 0.0185(14) 0.0211(14) 0.0021(11) 0.0033(11) 0.0014(11)
C2 0.0207(13) 0.0198(14) 0.0251(15) -0.0045(12) -0.0011(11) 0.0045(11)
C3 0.0273(16) 0.0386(19) 0.048(2) -0.0165(15) 0.0059(14) 0.0039(13)
C4 0.0328(18) 0.056(2) 0.060(2) -0.0273(18) 0.0069(16) 0.0107(16)
C5 0.0442(19) 0.0370(19) 0.046(2) -0.0219(15) -0.0103(15) 0.0168(15)
C6 0.0339(17) 0.0289(17) 0.053(2) -0.0163(15) -0.0101(14) 0.0022(13)
C7 0.0265(15) 0.0301(17) 0.0417(18) -0.0103(14) 0.0000(13) 0.0076(12)
C8 0.0205(13) 0.0180(14) 0.0175(14) -0.0018(11) -0.0002(10) -0.0048(11)
C9 0.0139(12) 0.0187(13) 0.0227(14) 0.0020(11) -0.0011(10) -0.0004(10)
C10 0.0187(14) 0.0263(16) 0.0428(18) 0.0049(13) 0.0037(12) -0.0001(11)
C11 0.0261(16) 0.0242(16) 0.058(2) 0.0122(15) 0.0017(14) 0.0040(12)
C12 0.0317(16) 0.0289(17) 0.0363(18) 0.0138(13) -0.0006(13) -0.0096(13)
C13 0.0234(14) 0.0299(17) 0.0360(17) 0.0030(13) 0.0094(12) -0.0035(12)
C14 0.0231(14) 0.0223(15) 0.0327(16) 0.0033(12) 0.0064(12) -0.0002(11)
C15 0.0177(13) 0.0174(13) 0.0174(13) 0.0031(11) 0.0058(10) -0.0024(11)
C16 0.0224(13) 0.0151(13) 0.0163(13) 0.0014(10) 0.0032(10) -0.0011(10)
C17 0.0206(14) 0.0245(15) 0.0249(15) -0.0014(12) 0.0048(11) -0.0001(11)
C18 0.0267(15) 0.0307(17) 0.0344(17) -0.0068(13) -0.0036(12) -0.0039(12)
C19 0.0462(18) 0.0194(15) 0.0303(17) -0.0058(12) -0.0101(14) -0.0034(13)
C20 0.0422(18) 0.0181(15) 0.0351(17) -0.0077(13) -0.0067(14) 0.0088(13)
C21 0.0304(15) 0.0205(15) 0.0273(16) -0.0018(12) -0.0066(12) 0.0065(12)
C22 0.0147(12) 0.0161(14) 0.0252(15) 0.0012(11) -0.0013(10) 0.0016(10)
C23 0.0206(13) 0.0204(14) 0.0242(15) 0.0034(11) -0.0028(11) 0.0002(11)
C24 0.0254(15) 0.0243(16) 0.0416(18) -0.0073(13) 0.0031(12) -0.0027(12)
C25 0.0288(16) 0.0406(19) 0.045(2) -0.0140(15) 0.0012(14) 0.0059(14)
C26 0.0469(19) 0.0243(16) 0.0387(19) -0.0115(14) -0.0091(15) 0.0066(14)
C27 0.0393(18) 0.0209(16) 0.046(2) -0.0020(14) -0.0052(14) -0.0068(13)
C28 0.0254(15) 0.0219(15) 0.0380(17) 0.0020(13) 0.0007(12) -0.0027(12)
C29 0.0150(13) 0.0173(14) 0.0217(15) -0.0007(11) 0.0010(10) -0.0059(10)
C30 0.0129(12) 0.0234(14) 0.0200(14) -0.0003(11) 0.0025(10) -0.0007(10)
C31 0.0226(14) 0.0285(16) 0.0269(16) 0.0031(12) 0.0049(11) 0.0046(11)
C32 0.0317(16) 0.0373(18) 0.0230(15) 0.0026(13) 0.0063(12) 0.0049(13)
C33 0.0315(16) 0.0420(19) 0.0284(17) -0.0026(14) 0.0122(13) 0.0101(13)
C34 0.0354(17) 0.0332(17) 0.0337(18) 0.0009(14) 0.0053(13) 0.0118(13)
C35 0.0268(14) 0.0303(16) 0.0195(14) 0.0025(12) 0.0004(11) 0.0032(12)
C36 0.0099(12) 0.0235(15) 0.0212(14) -0.0002(11) 0.0040(10) -0.0024(10)
C37 0.0153(13) 0.0245(14) 0.0197(14) -0.0005(11) 0.0027(10) -0.0050(11)
C38 0.0217(14) 0.0313(16) 0.0237(15) 0.0001(12) 0.0027(11) -0.0019(12)
C39 0.0314(16) 0.045(2) 0.0216(16) -0.0012(14) -0.0048(12) -0.0086(14)
C40 0.0416(18) 0.0354(18) 0.0248(17) -0.0110(13) 0.0021(13) -0.0147(14)
C41 0.0414(18) 0.0252(16) 0.0356(18) -0.0097(13) 0.0005(14) -0.0053(13)
C42 0.0317(16) 0.0240(15) 0.0268(16) 0.0008(12) -0.0049(12) -0.0023(12)
C43 0.0261(14) 0.0104(13) 0.0237(15) -0.0014(11) -0.0002(11) 0.0045(11)
C44 0.0267(14) 0.0093(13) 0.0250(15) -0.0044(11) -0.0048(11) 0.0024(10)
C45 0.0287(15) 0.0183(15) 0.0385(18) -0.0088(12) -0.0035(13) 0.0027(11)
C46 0.0312(16) 0.0191(16) 0.061(2) -0.0118(15) -0.0168(15) 0.0041(12)
C47 0.056(2) 0.0184(16) 0.049(2) -0.0033(14) -0.0318(17) 0.0049(14)
C48 0.063(2) 0.0205(16) 0.0296(17) 0.0013(13) -0.0189(15) -0.0011(14)
C49 0.0367(16) 0.0168(14) 0.0284(16) -0.0014(12) -0.0072(13) -0.0009(12)
C50 0.0178(13) 0.0211(14) 0.0324(16) 0.0058(12) 0.0005(11) 0.0027(11)
C51 0.0229(14) 0.0220(15) 0.0215(14) 0.0094(11) 0.0022(11) -0.0001(11)
C52 0.0214(14) 0.0219(15) 0.0230(15) 0.0051(11) 0.0066(11) -0.0004(11)
C53 0.0158(13) 0.0216(15) 0.0362(17) -0.0035(12) 0.0081(11) 0.0040(11)
C54 0.0197(14) 0.0201(15) 0.0388(17) 0.0015(12) 0.0013(12) 0.0050(11)
C55 0.0192(13) 0.0176(14) 0.0328(16) 0.0021(11) 0.0047(11) 0.0046(11)
C56 0.0314(15) 0.0141(14) 0.0307(16) 0.0025(11) -0.0003(12) -0.0044(11)
C57 0.0270(14) 0.0144(14) 0.0285(16) -0.0027(11) -0.0033(11) 0.0026(11)
C58 0.0207(13) 0.0170(14) 0.0242(15) -0.0041(11) -0.0001(11) 0.0005(10)
C59 0.0309(17) 0.050(2) 0.060(2) -0.0372(17) 0.0123(16) -0.0095(15)
C60A 0.022(5) 0.013(5) 0.018(5) -0.006(4) -0.007(4) 0.003(4)
C60B 0.031(2) 0.037(3) 0.025(2) -0.0155(19) 0.0072(17) -0.0054(18)
C61 0.0207(15) 0.053(2) 0.0336(17) -0.0227(15) 0.0065(12) 0.0007(13)
N1 0.0148(11) 0.0223(13) 0.0201(13) 0.0008(10) 0.0036(9) 0.0013(9)
N2 0.0161(11) 0.0196(12) 0.0217(13) -0.0020(10) 0.0009(9) -0.0012(9)
N3 0.0207(12) 0.0229(12) 0.0225(13) 0.0029(10) 0.0018(10) -0.0011(10)
N4 0.0212(12) 0.0234(13) 0.0208(13) -0.0020(10) -0.0004(9) -0.0013(9)
N5 0.066(2) 0.098(3) 0.0399(18) 0.0082(17) 0.0106(15) 0.0407(18)
C62 0.056(2) 0.052(2) 0.0334(19) 0.0111(16) 0.0100(16) 0.0223(18)
C63 0.061(2) 0.056(2) 0.062(3) 0.0176(19) -0.0081(19) -0.0145(19)
_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
Fe1 O19 1.8792(15) . ?
Fe1 O15 1.9491(15) . ?
Fe1 O10 2.0558(15) . ?
Fe1 O1 2.0575(16) . ?
Fe1 O11 2.0642(16) . ?
Fe1 N1 2.132(2) . ?
Fe1 Fe2 2.9605(4) . ?
Fe2 O20 1.8758(15) . ?
Fe2 O19 1.9588(15) . ?
Fe2 O5 2.0389(16) . ?
Fe2 O2 2.0628(16) . ?
Fe2 O15 2.0689(16) . ?
Fe2 O3 2.0744(15) . ?
Fe3 O20 1.9139(14) . ?
Fe3 O16 1.9881(16) . ?
Fe3 O7 2.0141(16) . ?
Fe3 O4 2.0326(16) . ?
Fe3 O6 2.0389(16) . ?
Fe3 N2 2.141(2) . ?
Fe4 O19 1.8596(15) . ?
Fe4 O17 1.9792(15) . ?
Fe4 O18 2.0269(16) . ?
Fe4 O9 2.0547(15) . ?
Fe4 O12 2.0591(16) . ?
Fe4 N3 2.164(2) . ?
Fe5 O18 1.9729(15) . ?
Fe5 O20 1.9813(16) . ?
Fe5 O16 1.9983(15) . ?
Fe5 O13 2.0027(16) . ?
Fe5 O17 2.0103(16) . ?
Fe5 N4 2.167(2) . ?
O1 C1 1.271(3) . ?
O2 C1 1.266(3) . ?
O3 C8 1.257(3) . ?
O4 C8 1.271(3) . ?
O5 C15 1.262(3) . ?
O6 C15 1.267(3) . ?
O7 C22 1.293(3) . ?
O8 C22 1.233(3) . ?
O9 C29 1.268(3) . ?
O10 C29 1.263(3) . ?
O11 C36 1.264(3) . ?
O12 C36 1.264(3) . ?
O13 C43 1.290(3) . ?
O14 C43 1.235(3) . ?
O15 C52 1.415(3) . ?
O16 C55 1.426(3) . ?
O17 C58 1.421(3) . ?
O18 C61 1.419(3) . ?
C1 C2 1.491(3) . ?
C2 C7 1.383(3) . ?
C2 C3 1.388(3) . ?
C3 C4 1.383(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.371(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.383(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.374(4) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.496(3) . ?
C9 C14 1.389(3) . ?
C9 C10 1.390(3) . ?
C10 C11 1.380(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.386(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.377(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.383(3) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.491(3) . ?
C16 C21 1.383(3) . ?
C16 C17 1.384(3) . ?
C17 C18 1.373(3) . ?
C17 H17 0.9300 . ?
C18 C19 1.376(4) . ?
C18 H18 0.9300 . ?
C19 C20 1.380(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.381(3) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.491(3) . ?
C23 C24 1.384(3) . ?
C23 C28 1.389(3) . ?
C24 C25 1.380(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.376(4) . ?
C25 H25 0.9300 . ?
C26 C27 1.374(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.375(4) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C30 1.498(3) . ?
C30 C35 1.382(3) . ?
C30 C31 1.392(3) . ?
C31 C32 1.383(3) . ?
C31 H31 0.9300 . ?
C32 C33 1.385(4) . ?
C32 H32 0.9300 . ?
C33 C34 1.377(4) . ?
C33 H33 0.9300 . ?
C34 C35 1.386(3) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.500(3) . ?
C37 C38 1.377(3) . ?
C37 C42 1.384(3) . ?
C38 C39 1.387(3) . ?
C38 H38 0.9300 . ?
C39 C40 1.376(4) . ?
C39 H39 0.9300 . ?
C40 C41 1.365(4) . ?
C40 H40 0.9300 . ?
C41 C42 1.391(3) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 C44 1.507(3) . ?
C44 C49 1.383(3) . ?
C44 C45 1.391(3) . ?
C45 C46 1.391(4) . ?
C45 H45 0.9300 . ?
C46 C47 1.363(4) . ?
C46 H46 0.9300 . ?
C47 C48 1.389(4) . ?
C47 H47 0.9300 . ?
C48 C49 1.379(4) . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
C50 N1 1.484(3) . ?
C50 C51 1.518(3) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 C52 1.513(3) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 N2 1.482(3) . ?
C53 C54 1.489(3) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 C55 1.517(3) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 N3 1.480(3) . ?
C56 C57 1.513(3) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 C58 1.513(3) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 C60A 1.288(8) . ?
C59 C60B 1.461(4) . ?
C59 N4 1.466(3) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C59 H59C 0.9700 . ?
C59 H59D 0.9700 . ?
C60A C61 1.671(8) . ?
C60A H60A 0.9700 . ?
C60A H60B 0.9700 . ?
C60B C61 1.525(4) . ?
C60B H60C 0.9700 . ?
C60B H60D 0.9700 . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C61 H61C 0.9700 . ?
C61 H61D 0.9700 . ?
N1 H1N 0.86(2) . ?
N1 H2N 0.84(3) . ?
N2 H3N 0.84(3) . ?
N2 H4N 0.84(3) . ?
N3 H5N 0.835(16) . ?
N3 H6N 0.89(2) . ?
N4 H7N 0.804(16) . ?
N4 H8N 0.87(3) . ?
N5 C62 1.128(4) . ?
C62 C63 1.434(4) . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
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
O19 Fe1 O15 82.66(6) . . ?
O19 Fe1 O10 96.88(6) . . ?
O15 Fe1 O10 172.25(7) . . ?
O19 Fe1 O1 93.65(7) . . ?
O15 Fe1 O1 88.84(6) . . ?
O10 Fe1 O1 83.46(6) . . ?
O19 Fe1 O11 91.57(6) . . ?
O15 Fe1 O11 98.32(6) . . ?
O10 Fe1 O11 89.42(6) . . ?
O1 Fe1 O11 171.63(6) . . ?
O19 Fe1 N1 172.66(8) . . ?
O15 Fe1 N1 92.22(7) . . ?
O10 Fe1 N1 88.90(7) . . ?
O1 Fe1 N1 91.49(8) . . ?
O11 Fe1 N1 83.95(8) . . ?
O19 Fe1 Fe2 40.51(4) . . ?
O15 Fe1 Fe2 44.13(5) . . ?
O10 Fe1 Fe2 133.08(5) . . ?
O1 Fe1 Fe2 81.74(4) . . ?
O11 Fe1 Fe2 106.42(4) . . ?
N1 Fe1 Fe2 135.61(6) . . ?
O20 Fe2 O19 96.82(6) . . ?
O20 Fe2 O5 91.73(6) . . ?
O19 Fe2 O5 97.53(6) . . ?
O20 Fe2 O2 98.75(7) . . ?
O19 Fe2 O2 88.94(6) . . ?
O5 Fe2 O2 166.97(7) . . ?
O20 Fe2 O15 171.64(7) . . ?
O19 Fe2 O15 77.73(6) . . ?
O5 Fe2 O15 82.81(6) . . ?
O2 Fe2 O15 87.57(6) . . ?
O20 Fe2 O3 97.20(6) . . ?
O19 Fe2 O3 164.46(6) . . ?
O5 Fe2 O3 88.72(6) . . ?
O2 Fe2 O3 82.33(6) . . ?
O15 Fe2 O3 89.04(6) . . ?
O20 Fe2 Fe1 134.82(5) . . ?
O19 Fe2 Fe1 38.55(4) . . ?
O5 Fe2 Fe1 99.50(4) . . ?
O2 Fe2 Fe1 78.57(4) . . ?
O15 Fe2 Fe1 40.99(4) . . ?
O3 Fe2 Fe1 126.44(5) . . ?
O20 Fe3 O16 82.59(6) . . ?
O20 Fe3 O7 88.55(6) . . ?
O16 Fe3 O7 97.32(7) . . ?
O20 Fe3 O4 102.37(6) . . ?
O16 Fe3 O4 172.92(6) . . ?
O7 Fe3 O4 87.92(7) . . ?
O20 Fe3 O6 94.94(6) . . ?
O16 Fe3 O6 89.51(6) . . ?
O7 Fe3 O6 172.70(7) . . ?
O4 Fe3 O6 85.07(6) . . ?
O20 Fe3 N2 169.68(8) . . ?
O16 Fe3 N2 87.46(7) . . ?
O7 Fe3 N2 90.03(7) . . ?
O4 Fe3 N2 87.78(7) . . ?
O6 Fe3 N2 87.67(7) . . ?
O19 Fe4 O17 97.37(6) . . ?
O19 Fe4 O18 90.68(7) . . ?
O17 Fe4 O18 78.90(6) . . ?
O19 Fe4 O9 95.68(6) . . ?
O17 Fe4 O9 163.71(7) . . ?
O18 Fe4 O9 91.25(6) . . ?
O19 Fe4 O12 92.19(7) . . ?
O17 Fe4 O12 94.84(6) . . ?
O18 Fe4 O12 173.41(6) . . ?
O9 Fe4 O12 94.37(6) . . ?
O19 Fe4 N3 177.94(7) . . ?
O17 Fe4 N3 84.59(7) . . ?
O18 Fe4 N3 90.33(7) . . ?
O9 Fe4 N3 82.50(7) . . ?
O12 Fe4 N3 87.00(7) . . ?
O18 Fe5 O20 98.40(6) . . ?
O18 Fe5 O16 179.01(7) . . ?
O20 Fe5 O16 80.66(6) . . ?
O18 Fe5 O13 93.79(6) . . ?
O20 Fe5 O13 165.95(6) . . ?
O16 Fe5 O13 87.10(6) . . ?
O18 Fe5 O17 79.45(6) . . ?
O20 Fe5 O17 90.94(6) . . ?
O16 Fe5 O17 100.86(6) . . ?
O13 Fe5 O17 98.18(7) . . ?
O18 Fe5 N4 92.26(7) . . ?
O20 Fe5 N4 86.20(8) . . ?
O16 Fe5 N4 87.36(7) . . ?
O13 Fe5 N4 86.36(8) . . ?
O17 Fe5 N4 170.75(7) . . ?
C1 O1 Fe1 124.86(15) . . ?
C1 O2 Fe2 128.88(15) . . ?
C8 O3 Fe2 128.06(15) . . ?
C8 O4 Fe3 127.90(15) . . ?
C15 O5 Fe2 135.53(16) . . ?
C15 O6 Fe3 122.99(15) . . ?
C22 O7 Fe3 129.50(15) . . ?
C29 O9 Fe4 128.85(15) . . ?
C29 O10 Fe1 127.28(14) . . ?
C36 O11 Fe1 130.95(16) . . ?
C36 O12 Fe4 132.06(16) . . ?
C43 O13 Fe5 137.48(15) . . ?
C52 O15 Fe1 126.12(13) . . ?
C52 O15 Fe2 126.69(13) . . ?
Fe1 O15 Fe2 94.88(7) . . ?
C55 O16 Fe3 128.56(14) . . ?
C55 O16 Fe5 126.48(13) . . ?
Fe3 O16 Fe5 96.84(6) . . ?
C58 O17 Fe4 121.57(13) . . ?
C58 O17 Fe5 132.74(14) . . ?
Fe4 O17 Fe5 99.44(7) . . ?
C61 O18 Fe5 129.51(14) . . ?
C61 O18 Fe4 123.17(14) . . ?
Fe5 O18 Fe4 99.09(7) . . ?
Fe4 O19 Fe1 124.04(8) . . ?
Fe4 O19 Fe2 133.60(8) . . ?
Fe1 O19 Fe2 100.93(7) . . ?
Fe2 O20 Fe3 117.69(8) . . ?
Fe2 O20 Fe5 132.03(8) . . ?
Fe3 O20 Fe5 99.89(7) . . ?
O2 C1 O1 125.8(2) . . ?
O2 C1 C2 117.0(2) . . ?
O1 C1 C2 117.2(2) . . ?
C7 C2 C3 119.0(2) . . ?
C7 C2 C1 120.7(2) . . ?
C3 C2 C1 120.3(2) . . ?
C4 C3 C2 120.1(3) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 120.7(3) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 119.2(3) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C7 C6 C5 120.5(3) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C2 120.5(2) . . ?
C6 C7 H7 119.8 . . ?
C2 C7 H7 119.8 . . ?
O3 C8 O4 125.2(2) . . ?
O3 C8 C9 118.3(2) . . ?
O4 C8 C9 116.6(2) . . ?
C14 C9 C10 119.0(2) . . ?
C14 C9 C8 120.5(2) . . ?
C10 C9 C8 120.5(2) . . ?
C11 C10 C9 120.3(2) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.1(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 120.1(2) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 119.8(2) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C9 120.7(2) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
O5 C15 O6 125.7(2) . . ?
O5 C15 C16 116.3(2) . . ?
O6 C15 C16 117.9(2) . . ?
C21 C16 C17 119.4(2) . . ?
C21 C16 C15 120.5(2) . . ?
C17 C16 C15 120.0(2) . . ?
C18 C17 C16 120.6(2) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C19 119.8(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C18 C19 C20 120.3(3) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C19 C20 C21 119.9(2) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C16 120.0(2) . . ?
C20 C21 H21 120.0 . . ?
C16 C21 H21 120.0 . . ?
O8 C22 O7 124.9(2) . . ?
O8 C22 C23 119.5(2) . . ?
O7 C22 C23 115.6(2) . . ?
C24 C23 C28 119.1(2) . . ?
C24 C23 C22 121.5(2) . . ?
C28 C23 C22 119.4(2) . . ?
C25 C24 C23 120.2(2) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C26 C25 C24 120.1(3) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C27 C26 C25 120.3(3) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 119.9(3) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 H27 120.1 . . ?
C27 C28 C23 120.5(2) . . ?
C27 C28 H28 119.7 . . ?
C23 C28 H28 119.7 . . ?
O10 C29 O9 125.0(2) . . ?
O10 C29 C30 117.8(2) . . ?
O9 C29 C30 117.2(2) . . ?
C35 C30 C31 119.4(2) . . ?
C35 C30 C29 119.6(2) . . ?
C31 C30 C29 120.8(2) . . ?
C32 C31 C30 120.1(2) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C33 120.1(3) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C34 C33 C32 119.9(2) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 120.3(3) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
C30 C35 C34 120.2(2) . . ?
C30 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
O11 C36 O12 125.7(2) . . ?
O11 C36 C37 116.4(2) . . ?
O12 C36 C37 117.9(2) . . ?
C38 C37 C42 119.3(2) . . ?
C38 C37 C36 120.3(2) . . ?
C42 C37 C36 120.4(2) . . ?
C37 C38 C39 120.1(3) . . ?
C37 C38 H38 120.0 . . ?
C39 C38 H38 120.0 . . ?
C40 C39 C38 120.2(3) . . ?
C40 C39 H39 119.9 . . ?
C38 C39 H39 119.9 . . ?
C41 C40 C39 120.3(3) . . ?
C41 C40 H40 119.9 . . ?
C39 C40 H40 119.9 . . ?
C40 C41 C42 119.9(3) . . ?
C40 C41 H41 120.1 . . ?
C42 C41 H41 120.1 . . ?
C37 C42 C41 120.3(3) . . ?
C37 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
O14 C43 O13 126.1(2) . . ?
O14 C43 C44 119.4(2) . . ?
O13 C43 C44 114.5(2) . . ?
C49 C44 C45 118.8(2) . . ?
C49 C44 C43 120.2(2) . . ?
C45 C44 C43 121.0(2) . . ?
C44 C45 C46 120.0(3) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
C47 C46 C45 120.5(3) . . ?
C47 C46 H46 119.7 . . ?
C45 C46 H46 119.7 . . ?
C46 C47 C48 119.9(3) . . ?
C46 C47 H47 120.0 . . ?
C48 C47 H47 120.0 . . ?
C49 C48 C47 119.7(3) . . ?
C49 C48 H48 120.1 . . ?
C47 C48 H48 120.1 . . ?
C48 C49 C44 121.0(3) . . ?
C48 C49 H49 119.5 . . ?
C44 C49 H49 119.5 . . ?
N1 C50 C51 111.51(19) . . ?
N1 C50 H50A 109.3 . . ?
C51 C50 H50A 109.3 . . ?
N1 C50 H50B 109.3 . . ?
C51 C50 H50B 109.3 . . ?
H50A C50 H50B 108.0 . . ?
C52 C51 C50 113.5(2) . . ?
C52 C51 H51A 108.9 . . ?
C50 C51 H51A 108.9 . . ?
C52 C51 H51B 108.9 . . ?
C50 C51 H51B 108.9 . . ?
H51A C51 H51B 107.7 . . ?
O15 C52 C51 111.77(19) . . ?
O15 C52 H52A 109.3 . . ?
C51 C52 H52A 109.3 . . ?
O15 C52 H52B 109.3 . . ?
C51 C52 H52B 109.3 . . ?
H52A C52 H52B 107.9 . . ?
N2 C53 C54 111.2(2) . . ?
N2 C53 H53A 109.4 . . ?
C54 C53 H53A 109.4 . . ?
N2 C53 H53B 109.4 . . ?
C54 C53 H53B 109.4 . . ?
H53A C53 H53B 108.0 . . ?
C53 C54 C55 114.6(2) . . ?
C53 C54 H54A 108.6 . . ?
C55 C54 H54A 108.6 . . ?
C53 C54 H54B 108.6 . . ?
C55 C54 H54B 108.6 . . ?
H54A C54 H54B 107.6 . . ?
O16 C55 C54 112.41(19) . . ?
O16 C55 H55A 109.1 . . ?
C54 C55 H55A 109.1 . . ?
O16 C55 H55B 109.1 . . ?
C54 C55 H55B 109.1 . . ?
H55A C55 H55B 107.9 . . ?
N3 C56 C57 111.3(2) . . ?
N3 C56 H56A 109.4 . . ?
C57 C56 H56A 109.4 . . ?
N3 C56 H56B 109.4 . . ?
C57 C56 H56B 109.4 . . ?
H56A C56 H56B 108.0 . . ?
C56 C57 C58 114.9(2) . . ?
C56 C57 H57A 108.5 . . ?
C58 C57 H57A 108.5 . . ?
C56 C57 H57B 108.5 . . ?
C58 C57 H57B 108.5 . . ?
H57A C57 H57B 107.5 . . ?
O17 C58 C57 112.59(19) . . ?
O17 C58 H58A 109.1 . . ?
C57 C58 H58A 109.1 . . ?
O17 C58 H58B 109.1 . . ?
C57 C58 H58B 109.1 . . ?
H58A C58 H58B 107.8 . . ?
C60A C59 C60B 58.5(4) . . ?
C60A C59 N4 123.4(4) . . ?
C60B C59 N4 115.7(3) . . ?
C60A C59 H59A 106.5 . . ?
C60B C59 H59A 52.2 . . ?
N4 C59 H59A 106.5 . . ?
C60A C59 H59B 106.5 . . ?
C60B C59 H59B 136.4 . . ?
N4 C59 H59B 106.5 . . ?
H59A C59 H59B 106.5 . . ?
C60A C59 H59C 127.5 . . ?
C60B C59 H59C 108.4 . . ?
N4 C59 H59C 108.4 . . ?
H59A C59 H59C 63.0 . . ?
C60A C59 H59D 50.3 . . ?
C60B C59 H59D 108.4 . . ?
N4 C59 H59D 108.4 . . ?
H59A C59 H59D 145.1 . . ?
H59B C59 H59D 65.7 . . ?
H59C C59 H59D 107.4 . . ?
C59 C60A C61 114.9(6) . . ?
C59 C60A H60A 108.6 . . ?
C61 C60A H60A 108.6 . . ?
C59 C60A H60B 108.6 . . ?
C61 C60A H60B 108.6 . . ?
H60A C60A H60B 107.5 . . ?
C59 C60B C61 113.9(3) . . ?
C59 C60B H60C 108.8 . . ?
C61 C60B H60C 108.8 . . ?
C59 C60B H60D 108.8 . . ?
C61 C60B H60D 108.8 . . ?
H60C C60B H60D 107.7 . . ?
O18 C61 C60B 110.5(2) . . ?
O18 C61 C60A 112.0(3) . . ?
C60B C61 C60A 49.8(3) . . ?
O18 C61 H61A 109.2 . . ?
C60B C61 H61A 63.0 . . ?
C60A C61 H61A 109.2 . . ?
O18 C61 H61B 109.2 . . ?
C60B C61 H61B 140.0 . . ?
C60A C61 H61B 109.2 . . ?
H61A C61 H61B 107.9 . . ?
O18 C61 H61C 109.6 . . ?
C60B C61 H61C 109.6 . . ?
C60A C61 H61C 138.1 . . ?
H61A C61 H61C 50.1 . . ?
H61B C61 H61C 60.4 . . ?
O18 C61 H61D 109.6 . . ?
C60B C61 H61D 109.6 . . ?
C60A C61 H61D 62.3 . . ?
H61A C61 H61D 140.4 . . ?
H61B C61 H61D 50.7 . . ?
H61C C61 H61D 108.1 . . ?
C50 N1 Fe1 118.25(15) . . ?
C50 N1 H1N 104.3(17) . . ?
Fe1 N1 H1N 109.8(17) . . ?
C50 N1 H2N 103.0(18) . . ?
Fe1 N1 H2N 109.4(18) . . ?
H1N N1 H2N 112(2) . . ?
C53 N2 Fe3 119.71(15) . . ?
C53 N2 H3N 105.8(18) . . ?
Fe3 N2 H3N 105.5(17) . . ?
C53 N2 H4N 103.8(18) . . ?
Fe3 N2 H4N 111.8(17) . . ?
H3N N2 H4N 110(2) . . ?
C56 N3 Fe4 118.76(15) . . ?
C56 N3 H5N 109.6(19) . . ?
Fe4 N3 H5N 105.5(19) . . ?
C56 N3 H6N 109.2(17) . . ?
Fe4 N3 H6N 110.6(17) . . ?
H5N N3 H6N 102(2) . . ?
C59 N4 Fe5 116.87(17) . . ?
C59 N4 H7N 109(2) . . ?
Fe5 N4 H7N 105(2) . . ?
C59 N4 H8N 111.1(18) . . ?
Fe5 N4 H8N 107.9(18) . . ?
H7N N4 H8N 106(3) . . ?
N5 C62 C63 177.8(4) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
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
N1 H1N O8 0.86(2) 2.00(3) 2.863(3) 176(2) 1_455
N2 H3N N5 0.84(3) 2.32(3) 3.132(4) 161(2) 1_655
N2 H4N O10 0.84(3) 2.53(3) 3.310(3) 155(2) 1_655
N3 H5N O14 0.835(16) 2.164(18) 2.986(3) 168(3) .
N4 H7N O7 0.804(16) 2.250(18) 3.020(3) 161(3) .
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max 0.367
_refine_diff_density_min -0.321
_refine_diff_density_rms 0.068
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 -0.010 0.000 0.000 264 34 ' '
2 -0.010 0.500 0.500 264 34 ' '
3 0.133 0.326 0.768 7 0 ' '
4 0.367 0.826 0.731 7 1 ' '
5 0.633 0.174 0.268 7 1 ' '
6 0.867 0.674 0.231 7 1 ' '
_platon_squeeze_details
;
The crystal structure contains a second acetonitrile
molecule of crystallization which was highly disordered;
attemps to model it with a chemically reasonable geometry
were unsuccessful. Therefore, the SQUEEZE procedure of PLATON
(van der Sluis & Spek, 1990; Spek, 2001) was employed to remove
the contribution of the electron density associated with this
solvent molecule from the intensity data. The solvent-free model
and intensity data were used for the final results reported here.
;
# start Validation Reply Form
_vrf_PLAT605_ck7-sqz
;
PROBLEM: _Structure Contains Solvent Accessible VOIDS of . 265.00 A**3
RESPONSE: The crystal structure contains a second acetonitrile
molecule of crystallization which is highly disordered;
attemps to model it with a chemically reasonable geometry
were unsuccessful. Therefore, the SQUEEZE procedure of PLATON
(van der Sluis & Spek, 1990; Spek, 2001) was employed to remove
the contribution of the electron density associated with this
solvent molecule from the intensity data. The solvent-free model
and intensity data were used for the final results reported here.
;
#===END
# Attachment '- 4.cif'
data_ck9
_database_code_depnum_ccdc_archive 'CCDC 836725'
#TrackingRef '- 4.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C59 H111 Fe5 N4 O20, 0.3(H2 O)'
_chemical_formula_sum 'C59 H111.60 Fe5 N4 O20.30'
_chemical_formula_weight 1481.17
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 21/n'
_symmetry_space_group_name_Hall '-P 2yn'
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 14.2040(5)
_cell_length_b 19.9979(7)
_cell_length_c 25.9433(8)
_cell_angle_alpha 90.00
_cell_angle_beta 95.698(3)
_cell_angle_gamma 90.00
_cell_volume 7332.8(4)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 5374
_cell_measurement_theta_min 3.6563
_cell_measurement_theta_max 30.4139
_exptl_crystal_description plate
_exptl_crystal_colour 'dark brown'
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.006
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.342
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3144
_exptl_absorpt_coefficient_mu 1.033
_exptl_absorpt_correction_T_min 0.98216
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur-3 with Sapphire CCD'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 16.0288
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 61887
_diffrn_reflns_av_R_equivalents 0.1184
_diffrn_reflns_av_sigmaI/netI 0.1529
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_theta_min 2.84
_diffrn_reflns_theta_max 25.00
_reflns_number_total 12878
_reflns_number_gt 6721
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997'
_computing_molecular_graphics
'PLATON (Spek, 1990); MERCURY (Bruno et al. 2002)'
_computing_publication_material 'WINGX (Farrugia, 1999)'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838.
Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford
Diffraction Ltd, Abingdon, Oxford, England.
Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany.
Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands.
;
_refine_special_details
;
Atoms C37-C38-C39, C42-C43-C44 and C47-C48-C49 of the t-butyl groups of three
pivalic ligands are disordered over two sites with domain ratio: 25:75, 30:70
and 22:78, respectively.
;
_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^)+(0.0663P)^2^+1.5582P] 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 12878
_refine_ls_number_parameters 907
_refine_ls_number_restraints 138
_refine_ls_R_factor_all 0.1402
_refine_ls_R_factor_gt 0.0669
_refine_ls_wR_factor_ref 0.1634
_refine_ls_wR_factor_gt 0.1477
_refine_ls_goodness_of_fit_ref 1.015
_refine_ls_restrained_S_all 1.018
_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
C1 C 0.9443(5) 0.1616(4) 0.7149(2) 0.051(2) Uani 1 1 d . . .
H1A H 0.9207 0.1979 0.7349 0.061 Uiso 1 1 calc R . .
H1B H 0.8968 0.1266 0.7123 0.061 Uiso 1 1 calc R . .
C2 C 1.0316(6) 0.1352(5) 0.7431(3) 0.067(3) Uani 1 1 d . . .
H2A H 1.0171 0.1173 0.7761 0.081 Uiso 1 1 calc R . .
H2B H 1.0766 0.1714 0.7499 0.081 Uiso 1 1 calc R . .
C3 C 1.0765(6) 0.0802(4) 0.7125(3) 0.067(3) Uani 1 1 d . . .
H3A H 1.0356 0.0412 0.7095 0.081 Uiso 1 1 calc R . .
H3B H 1.1369 0.0670 0.7304 0.081 Uiso 1 1 calc R . .
C4 C 1.0908(6) 0.1071(4) 0.6587(3) 0.064(2) Uani 1 1 d . . .
H4A H 1.1365 0.1433 0.6619 0.077 Uiso 1 1 calc R . .
H4B H 1.1158 0.0719 0.6382 0.077 Uiso 1 1 calc R . .
C5 C 1.0002(6) 0.1317(4) 0.6322(3) 0.056(2) Uani 1 1 d . . .
H5 H 0.9560 0.0940 0.6305 0.067 Uiso 1 1 calc R . .
C6 C 1.0011(5) 0.1583(4) 0.5763(3) 0.051(2) Uani 1 1 d . . .
H6A H 1.0438 0.1960 0.5756 0.061 Uiso 1 1 calc R . .
H6B H 1.0215 0.1236 0.5538 0.061 Uiso 1 1 calc R . .
C7 C 0.7262(5) 0.1096(4) 0.2864(3) 0.0397(18) Uani 1 1 d . . .
H7A H 0.7301 0.0734 0.3114 0.048 Uiso 1 1 calc R . .
H7B H 0.7901 0.1222 0.2802 0.048 Uiso 1 1 calc R . .
C8 C 0.6728(5) 0.0858(4) 0.2357(3) 0.050(2) Uani 1 1 d . . .
H8A H 0.6766 0.1198 0.2093 0.059 Uiso 1 1 calc R . .
H8B H 0.7025 0.0455 0.2241 0.059 Uiso 1 1 calc R . .
C9 C 0.5704(5) 0.0714(4) 0.2417(3) 0.046(2) Uani 1 1 d . . .
H9A H 0.5662 0.0334 0.2646 0.056 Uiso 1 1 calc R . .
H9B H 0.5378 0.0599 0.2083 0.056 Uiso 1 1 calc R . .
C10 C 0.5228(5) 0.1311(4) 0.2636(2) 0.0399(18) Uani 1 1 d . . .
H10A H 0.4587 0.1193 0.2700 0.048 Uiso 1 1 calc R . .
H10B H 0.5192 0.1673 0.2386 0.048 Uiso 1 1 calc R . .
C11 C 0.5771(4) 0.1544(3) 0.3138(2) 0.0290(16) Uani 1 1 d . . .
H11 H 0.5751 0.1179 0.3389 0.035 Uiso 1 1 calc R . .
C12 C 0.5363(4) 0.2158(3) 0.3375(2) 0.0312(16) Uani 1 1 d . . .
H12A H 0.5227 0.2500 0.3113 0.037 Uiso 1 1 calc R . .
H12B H 0.4779 0.2045 0.3519 0.037 Uiso 1 1 calc R . .
C13 C 0.6288(6) 0.4116(4) 0.3744(3) 0.046(2) Uani 1 1 d . . .
H13A H 0.5604 0.4151 0.3700 0.055 Uiso 1 1 calc R . .
H13B H 0.6477 0.3818 0.3478 0.055 Uiso 1 1 calc R . .
C14 C 0.6716(7) 0.4809(4) 0.3669(3) 0.069(3) Uani 1 1 d . . .
H14A H 0.7397 0.4769 0.3671 0.082 Uiso 1 1 calc R . .
H14B H 0.6466 0.4989 0.3336 0.082 Uiso 1 1 calc R . .
C15 C 0.6489(7) 0.5283(4) 0.4096(3) 0.069(3) Uani 1 1 d . . .
H15A H 0.6815 0.5704 0.4062 0.082 Uiso 1 1 calc R . .
H15B H 0.5814 0.5371 0.4068 0.082 Uiso 1 1 calc R . .
C16 C 0.6797(6) 0.4975(4) 0.4618(3) 0.063(2) Uani 1 1 d . . .
H16A H 0.7481 0.4933 0.4660 0.076 Uiso 1 1 calc R . .
H16B H 0.6613 0.5266 0.4890 0.076 Uiso 1 1 calc R . .
C17 C 0.6355(5) 0.4294(3) 0.4669(3) 0.0394(18) Uani 1 1 d . . .
H17 H 0.5668 0.4359 0.4634 0.047 Uiso 1 1 calc R . .
C18 C 0.6607(5) 0.3933(3) 0.5170(2) 0.0316(17) Uani 1 1 d . . .
H18A H 0.7288 0.3880 0.5231 0.038 Uiso 1 1 calc R . .
H18B H 0.6393 0.4187 0.5455 0.038 Uiso 1 1 calc R . .
C19 C 0.4315(5) 0.2696(4) 0.6143(3) 0.0390(18) Uani 1 1 d . . .
H19A H 0.4554 0.3120 0.6282 0.047 Uiso 1 1 calc R . .
H19B H 0.4529 0.2349 0.6389 0.047 Uiso 1 1 calc R . .
C20 C 0.3236(5) 0.2714(4) 0.6088(3) 0.052(2) Uani 1 1 d . . .
H20A H 0.3013 0.2753 0.6428 0.063 Uiso 1 1 calc R . .
H20B H 0.3019 0.3103 0.5887 0.063 Uiso 1 1 calc R . .
C21 C 0.2839(5) 0.2101(4) 0.5830(3) 0.052(2) Uani 1 1 d . . .
H21A H 0.2156 0.2144 0.5772 0.063 Uiso 1 1 calc R . .
H21B H 0.2981 0.1721 0.6056 0.063 Uiso 1 1 calc R . .
C22 C 0.3235(5) 0.1977(3) 0.5314(3) 0.0429(19) Uani 1 1 d . . .
H22A H 0.3030 0.2329 0.5072 0.052 Uiso 1 1 calc R . .
H22B H 0.2996 0.1555 0.5169 0.052 Uiso 1 1 calc R . .
C23 C 0.4306(5) 0.1957(3) 0.5389(3) 0.0373(18) Uani 1 1 d . . .
H23 H 0.4487 0.1577 0.5616 0.045 Uiso 1 1 calc R . .
C24 C 0.4757(4) 0.1849(3) 0.4884(2) 0.0341(17) Uani 1 1 d . . .
H24A H 0.4762 0.1375 0.4806 0.041 Uiso 1 1 calc R . .
H24B H 0.4379 0.2072 0.4603 0.041 Uiso 1 1 calc R . .
C25 C 0.9344(4) 0.3293(3) 0.5586(3) 0.0309(16) Uani 1 1 d . . .
C26 C 1.0020(5) 0.3895(4) 0.5602(3) 0.047(2) Uani 1 1 d . . .
C27 C 0.9516(6) 0.4488(4) 0.5814(3) 0.073(3) Uani 1 1 d . . .
H27A H 0.9958 0.4846 0.5888 0.109 Uiso 1 1 calc R . .
H27B H 0.9254 0.4359 0.6126 0.109 Uiso 1 1 calc R . .
H27C H 0.9017 0.4634 0.5563 0.109 Uiso 1 1 calc R . .
C28 C 1.0866(6) 0.3733(5) 0.5965(4) 0.084(3) Uani 1 1 d U . .
H28A H 1.1210 0.3374 0.5825 0.126 Uiso 1 1 calc R . .
H28B H 1.0668 0.3599 0.6293 0.126 Uiso 1 1 calc R . .
H28C H 1.1266 0.4119 0.6011 0.126 Uiso 1 1 calc R . .
C29 C 1.0277(7) 0.4051(5) 0.5066(4) 0.095(3) Uani 1 1 d U . .
H29A H 1.0569 0.4484 0.5065 0.143 Uiso 1 1 calc R . .
H29B H 0.9716 0.4049 0.4827 0.143 Uiso 1 1 calc R . .
H29C H 1.0710 0.3719 0.4964 0.143 Uiso 1 1 calc R . .
C30 C 0.9350(5) 0.1701(3) 0.4103(3) 0.0338(17) Uani 1 1 d . . .
C31 C 1.0214(5) 0.1280(4) 0.4000(3) 0.0401(18) Uani 1 1 d . . .
C32 C 1.1117(5) 0.1597(4) 0.4247(3) 0.068(3) Uani 1 1 d . . .
H32A H 1.1629 0.1285 0.4242 0.102 Uiso 1 1 calc R . .
H32B H 1.1039 0.1717 0.4598 0.102 Uiso 1 1 calc R . .
H32C H 1.1255 0.1991 0.4056 0.102 Uiso 1 1 calc R . .
C33 C 1.0084(5) 0.0609(4) 0.4261(3) 0.059(2) Uani 1 1 d . . .
H33A H 0.9514 0.0401 0.4108 0.089 Uiso 1 1 calc R . .
H33B H 1.0042 0.0677 0.4624 0.089 Uiso 1 1 calc R . .
H33C H 1.0615 0.0326 0.4214 0.089 Uiso 1 1 calc R . .
C34 C 1.0275(6) 0.1162(5) 0.3428(3) 0.072(3) Uani 1 1 d . . .
H34A H 1.0393 0.1579 0.3263 0.109 Uiso 1 1 calc R . .
H34B H 0.9689 0.0977 0.3276 0.109 Uiso 1 1 calc R . .
H34C H 1.0781 0.0856 0.3384 0.109 Uiso 1 1 calc R . .
C35 C 0.7350(4) 0.0954(3) 0.4505(3) 0.0252(15) Uani 1 1 d . A .
C36 C 0.7072(5) 0.0240(3) 0.4623(2) 0.0306(16) Uani 1 1 d D . .
C37A C 0.688(2) 0.0214(15) 0.5207(7) 0.047(8) Uani 0.25 1 d PDU A 1
H37A H 0.6699 -0.0231 0.5293 0.070 Uiso 0.25 1 calc PR A 1
H37B H 0.6387 0.0521 0.5266 0.070 Uiso 0.25 1 calc PR A 1
H37C H 0.7450 0.0335 0.5419 0.070 Uiso 0.25 1 calc PR A 1
C38A C 0.614(2) 0.0026(14) 0.4331(12) 0.048(8) Uani 0.25 1 d PU A 1
H38A H 0.6001 -0.0426 0.4422 0.072 Uiso 0.25 1 calc PR A 1
H38B H 0.6190 0.0052 0.3965 0.072 Uiso 0.25 1 calc PR A 1
H38C H 0.5645 0.0316 0.4421 0.072 Uiso 0.25 1 calc PR A 1
C39A C 0.7939(16) -0.0200(13) 0.4563(12) 0.044(8) Uani 0.25 1 d PDU A 1
H39A H 0.7792 -0.0657 0.4635 0.066 Uiso 0.25 1 calc PR A 1
H39B H 0.8459 -0.0053 0.4800 0.066 Uiso 0.25 1 calc PR A 1
H39C H 0.8108 -0.0165 0.4215 0.066 Uiso 0.25 1 calc PR A 1
C37B C 0.6126(7) 0.0257(5) 0.4838(4) 0.048(3) Uani 0.75 1 d P A 2
H37D H 0.5670 0.0469 0.4592 0.072 Uiso 0.75 1 calc PR A 2
H37E H 0.6179 0.0505 0.5156 0.072 Uiso 0.75 1 calc PR A 2
H37F H 0.5926 -0.0191 0.4901 0.072 Uiso 0.75 1 calc PR A 2
C38B C 0.6963(6) -0.0163(4) 0.4106(3) 0.039(2) Uani 0.75 1 d PD A 2
H38D H 0.6481 0.0039 0.3871 0.059 Uiso 0.75 1 calc PR A 2
H38E H 0.6789 -0.0616 0.4174 0.059 Uiso 0.75 1 calc PR A 2
H38F H 0.7553 -0.0160 0.3954 0.059 Uiso 0.75 1 calc PR A 2
C39B C 0.7823(8) -0.0089(5) 0.4981(5) 0.058(3) Uani 0.75 1 d PU A 2
H39D H 0.7633 -0.0537 0.5052 0.088 Uiso 0.75 1 calc PR A 2
H39E H 0.7914 0.0159 0.5299 0.088 Uiso 0.75 1 calc PR A 2
H39F H 0.8405 -0.0099 0.4822 0.088 Uiso 0.75 1 calc PR A 2
C40 C 0.7940(6) 0.3018(4) 0.2936(3) 0.051(2) Uani 1 1 d . A .
C41 C 0.8847(6) 0.3402(4) 0.2823(3) 0.063(2) Uani 1 1 d DU . .
C42A C 0.956(3) 0.364(2) 0.3256(12) 0.117(17) Uani 0.30 1 d PDU B 1
H42A H 0.9608 0.3320 0.3532 0.175 Uiso 0.30 1 calc PR B 1
H42B H 0.9357 0.4063 0.3384 0.175 Uiso 0.30 1 calc PR B 1
H42C H 1.0166 0.3696 0.3127 0.175 Uiso 0.30 1 calc PR B 1
C43A C 0.850(3) 0.3935(13) 0.2432(7) 0.081(11) Uani 0.30 1 d PDU B 1
H43A H 0.8196 0.3724 0.2127 0.121 Uiso 0.30 1 calc PR B 1
H43B H 0.9024 0.4197 0.2342 0.121 Uiso 0.30 1 calc PR B 1
H43C H 0.8052 0.4220 0.2580 0.121 Uiso 0.30 1 calc PR B 1
C44A C 0.930(2) 0.2826(11) 0.2542(11) 0.070(9) Uani 0.30 1 d PDU B 1
H44A H 0.8859 0.2654 0.2272 0.104 Uiso 0.30 1 calc PR B 1
H44B H 0.9487 0.2476 0.2785 0.104 Uiso 0.30 1 calc PR B 1
H44C H 0.9854 0.2989 0.2394 0.104 Uiso 0.30 1 calc PR B 1
C42B C 0.9055(11) 0.3925(7) 0.3246(5) 0.083(5) Uani 0.70 1 d PDU B 2
H42D H 0.8543 0.4239 0.3234 0.124 Uiso 0.70 1 calc PR B 2
H42E H 0.9630 0.4157 0.3193 0.124 Uiso 0.70 1 calc PR B 2
H42F H 0.9125 0.3709 0.3578 0.124 Uiso 0.70 1 calc PR B 2
C43B C 0.8709(11) 0.3754(7) 0.2300(4) 0.063(4) Uani 0.70 1 d PDU B 2
H43D H 0.8171 0.4046 0.2291 0.094 Uiso 0.70 1 calc PR B 2
H43E H 0.8605 0.3427 0.2029 0.094 Uiso 0.70 1 calc PR B 2
H43F H 0.9263 0.4011 0.2250 0.094 Uiso 0.70 1 calc PR B 2
C44B C 0.9685(10) 0.2920(8) 0.2860(7) 0.110(6) Uani 0.70 1 d PDU B 2
H44D H 1.0246 0.3156 0.2789 0.165 Uiso 0.70 1 calc PR B 2
H44E H 0.9561 0.2567 0.2611 0.165 Uiso 0.70 1 calc PR B 2
H44F H 0.9773 0.2733 0.3202 0.165 Uiso 0.70 1 calc PR B 2
C45 C 0.4022(5) 0.3413(3) 0.4375(3) 0.0315(17) Uani 1 1 d . C .
C46 C 0.3169(4) 0.3574(3) 0.3978(2) 0.0332(17) Uani 1 1 d DU . .
C47A C 0.251(3) 0.4111(19) 0.4163(13) 0.046(10) Uani 0.22 1 d PU C 1
H47A H 0.2171 0.3931 0.4434 0.070 Uiso 0.22 1 calc PR C 1
H47B H 0.2069 0.4250 0.3879 0.070 Uiso 0.22 1 calc PR C 1
H47C H 0.2878 0.4489 0.4293 0.070 Uiso 0.22 1 calc PR C 1
C48A C 0.353(2) 0.3828(17) 0.3475(8) 0.038(9) Uani 0.22 1 d PDU C 1
H48A H 0.4080 0.3582 0.3407 0.058 Uiso 0.22 1 calc PR C 1
H48B H 0.3679 0.4295 0.3510 0.058 Uiso 0.22 1 calc PR C 1
H48C H 0.3042 0.3768 0.3194 0.058 Uiso 0.22 1 calc PR C 1
C49A C 0.263(3) 0.2935(13) 0.3819(16) 0.069(11) Uani 0.22 1 d PDU C 1
H49A H 0.3020 0.2645 0.3639 0.104 Uiso 0.22 1 calc PR C 1
H49B H 0.2068 0.3046 0.3596 0.104 Uiso 0.22 1 calc PR C 1
H49C H 0.2448 0.2713 0.4123 0.104 Uiso 0.22 1 calc PR C 1
C47B C 0.2241(7) 0.3649(7) 0.4259(4) 0.063(3) Uani 0.78 1 d PU C 2
H47D H 0.2094 0.3229 0.4411 0.094 Uiso 0.78 1 calc PR C 2
H47E H 0.1727 0.3781 0.4012 0.094 Uiso 0.78 1 calc PR C 2
H47F H 0.2337 0.3982 0.4525 0.094 Uiso 0.78 1 calc PR C 2
C48B C 0.3372(9) 0.4207(6) 0.3711(5) 0.080(4) Uani 0.78 1 d PU C 2
H48D H 0.3454 0.4562 0.3961 0.120 Uiso 0.78 1 calc PR C 2
H48E H 0.2853 0.4312 0.3458 0.120 Uiso 0.78 1 calc PR C 2
H48F H 0.3939 0.4157 0.3543 0.120 Uiso 0.78 1 calc PR C 2
C49B C 0.3017(8) 0.3009(5) 0.3583(4) 0.055(3) Uani 0.78 1 d PU C 2
H49D H 0.2904 0.2599 0.3758 0.083 Uiso 0.78 1 calc PR C 2
H49E H 0.3571 0.2962 0.3402 0.083 Uiso 0.78 1 calc PR C 2
H49F H 0.2482 0.3111 0.3340 0.083 Uiso 0.78 1 calc PR C 2
C50 C 0.7044(5) 0.3124(3) 0.6617(2) 0.0269(15) Uani 1 1 d . . .
C51 C 0.6994(5) 0.3647(3) 0.7036(2) 0.0320(16) Uani 1 1 d . . .
C52 C 0.7282(5) 0.3315(4) 0.7568(2) 0.045(2) Uani 1 1 d . . .
H52A H 0.7917 0.3149 0.7577 0.067 Uiso 1 1 calc R . .
H52B H 0.6860 0.2951 0.7618 0.067 Uiso 1 1 calc R . .
H52C H 0.7246 0.3639 0.7838 0.067 Uiso 1 1 calc R . .
C53 C 0.7725(5) 0.4184(3) 0.6937(3) 0.0443(19) Uani 1 1 d . . .
H53A H 0.7748 0.4514 0.7206 0.066 Uiso 1 1 calc R . .
H53B H 0.7548 0.4394 0.6608 0.066 Uiso 1 1 calc R . .
H53C H 0.8336 0.3981 0.6933 0.066 Uiso 1 1 calc R . .
C54 C 0.5999(5) 0.3950(4) 0.7019(3) 0.047(2) Uani 1 1 d . . .
H54A H 0.5558 0.3609 0.7097 0.070 Uiso 1 1 calc R . .
H54B H 0.5818 0.4126 0.6680 0.070 Uiso 1 1 calc R . .
H54C H 0.5998 0.4302 0.7271 0.070 Uiso 1 1 calc R . .
C55 C 0.6794(5) 0.1292(3) 0.6308(2) 0.0292(16) Uani 1 1 d . . .
C56 C 0.6480(5) 0.0682(3) 0.6593(3) 0.0381(18) Uani 1 1 d . . .
C57 C 0.6521(5) 0.0900(4) 0.7161(3) 0.059(2) Uani 1 1 d . . .
H57A H 0.6191 0.1316 0.7184 0.088 Uiso 1 1 calc R . .
H57B H 0.7168 0.0954 0.7299 0.088 Uiso 1 1 calc R . .
H57C H 0.6227 0.0564 0.7357 0.088 Uiso 1 1 calc R . .
C58 C 0.7169(6) 0.0092(4) 0.6537(3) 0.069(3) Uani 1 1 d . . .
H58A H 0.7170 -0.0022 0.6178 0.104 Uiso 1 1 calc R . .
H58B H 0.6969 -0.0287 0.6725 0.104 Uiso 1 1 calc R . .
H58C H 0.7796 0.0220 0.6675 0.104 Uiso 1 1 calc R . .
C59 C 0.5479(5) 0.0481(4) 0.6395(3) 0.051(2) Uani 1 1 d . . .
H59A H 0.5286 0.0108 0.6592 0.077 Uiso 1 1 calc R . .
H59B H 0.5457 0.0359 0.6037 0.077 Uiso 1 1 calc R . .
H59C H 0.5059 0.0851 0.6432 0.077 Uiso 1 1 calc R . .
N1 N 0.9569(4) 0.1864(3) 0.6620(2) 0.0358(14) Uani 1 1 d D . .
H1 H 0.996(4) 0.218(3) 0.659(3) 0.054 Uiso 1 1 d D . .
N2 N 0.6781(4) 0.1674(3) 0.3075(2) 0.0311(13) Uani 1 1 d D . .
H2 H 0.677(5) 0.202(2) 0.288(2) 0.047 Uiso 1 1 d D . .
N3 N 0.6575(4) 0.3830(3) 0.4245(2) 0.0319(14) Uani 1 1 d D . .
H3 H 0.7159(19) 0.381(3) 0.436(2) 0.048 Uiso 1 1 d D . .
N4 N 0.4721(4) 0.2567(3) 0.5647(2) 0.0301(13) Uani 1 1 d D . .
H4 H 0.465(5) 0.287(2) 0.5412(19) 0.045 Uiso 1 1 d D . .
O1 O 0.9075(3) 0.1779(2) 0.56014(15) 0.0296(10) Uani 1 1 d . . .
O2 O 0.6041(3) 0.2401(2) 0.37742(14) 0.0273(10) Uani 1 1 d . . .
O3 O 0.6161(3) 0.32991(19) 0.51364(14) 0.0233(10) Uani 1 1 d . . .
O4 O 0.5698(3) 0.2099(2) 0.49158(14) 0.0284(10) Uani 1 1 d . . .
O5 O 0.9150(3) 0.3068(2) 0.60173(16) 0.0340(11) Uani 1 1 d . . .
O6 O 0.9024(3) 0.3075(2) 0.51490(16) 0.0333(11) Uani 1 1 d . . .
O7 O 0.9370(3) 0.1982(2) 0.45351(17) 0.0418(12) Uani 1 1 d . . .
O8 O 0.8691(3) 0.1729(2) 0.37538(17) 0.0410(12) Uani 1 1 d . . .
O9 O 0.7852(3) 0.1247(2) 0.48593(17) 0.0357(11) Uani 1 1 d . . .
O10 O 0.7066(3) 0.1197(2) 0.40778(16) 0.0322(11) Uani 1 1 d . . .
O11 O 0.7844(3) 0.2909(2) 0.34165(17) 0.0402(12) Uani 1 1 d . . .
O12 O 0.7405(4) 0.2821(3) 0.2577(2) 0.0662(17) Uani 1 1 d . . .
O13 O 0.4742(3) 0.3163(2) 0.41851(15) 0.0286(10) Uani 1 1 d . . .
O14 O 0.3967(3) 0.3519(2) 0.48416(17) 0.0380(12) Uani 1 1 d . . .
O15 O 0.6418(3) 0.3114(2) 0.62422(15) 0.0321(11) Uani 1 1 d . . .
O16 O 0.7759(3) 0.2741(2) 0.66627(14) 0.0287(10) Uani 1 1 d . . .
O17 O 0.6176(3) 0.1669(2) 0.60715(15) 0.0308(11) Uani 1 1 d . . .
O18 O 0.7675(3) 0.1395(2) 0.63438(16) 0.0342(11) Uani 1 1 d . . .
O19 O 0.7496(3) 0.23690(19) 0.55358(14) 0.0240(10) Uani 1 1 d . . .
O20 O 0.7423(3) 0.2545(2) 0.44506(14) 0.0250(10) Uani 1 1 d . . .
Fe1 Fe 0.83588(6) 0.22139(5) 0.61130(3) 0.0264(2) Uani 1 1 d . A .
Fe2 Fe 0.82839(6) 0.22016(5) 0.49711(3) 0.0267(2) Uani 1 1 d . A .
Fe3 Fe 0.73850(6) 0.21254(5) 0.37921(3) 0.0259(2) Uani 1 1 d . A .
Fe4 Fe 0.60468(6) 0.28516(4) 0.44448(3) 0.0256(2) Uani 1 1 d . A .
Fe5 Fe 0.62318(6) 0.25113(5) 0.56044(3) 0.0253(2) Uani 1 1 d . A .
O21 O 0.8719(14) 0.3811(9) 0.4238(8) 0.082(6) Uani 0.30 1 d P . .
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
C1 0.045(5) 0.083(7) 0.024(4) 0.006(4) 0.000(4) 0.019(4)
C2 0.076(7) 0.074(7) 0.051(5) 0.012(5) 0.006(5) 0.024(5)
C3 0.076(7) 0.066(6) 0.058(6) 0.008(5) 0.003(5) 0.027(5)
C4 0.061(6) 0.073(7) 0.058(6) -0.005(5) 0.001(5) 0.020(5)
C5 0.051(5) 0.084(7) 0.031(4) -0.004(4) -0.008(4) 0.030(5)
C6 0.045(5) 0.074(6) 0.034(4) -0.004(4) 0.000(4) 0.021(4)
C7 0.033(4) 0.045(5) 0.041(4) -0.014(4) 0.003(3) 0.000(4)
C8 0.050(5) 0.057(5) 0.042(5) -0.021(4) 0.010(4) 0.006(4)
C9 0.042(5) 0.047(5) 0.049(5) -0.025(4) -0.003(4) -0.007(4)
C10 0.035(4) 0.044(5) 0.039(4) -0.012(4) -0.009(3) 0.003(4)
C11 0.024(4) 0.032(4) 0.030(4) -0.004(3) 0.000(3) -0.004(3)
C12 0.034(4) 0.041(4) 0.016(3) -0.005(3) -0.011(3) 0.000(3)
C13 0.060(5) 0.036(5) 0.042(5) 0.008(4) 0.003(4) -0.002(4)
C14 0.084(7) 0.047(6) 0.074(6) 0.026(5) 0.000(5) -0.010(5)
C15 0.090(7) 0.030(5) 0.085(7) 0.011(5) 0.008(6) -0.014(5)
C16 0.086(7) 0.030(5) 0.070(6) -0.004(4) -0.004(5) -0.014(5)
C17 0.038(4) 0.028(4) 0.051(5) 0.002(4) -0.001(4) -0.005(3)
C18 0.035(4) 0.024(4) 0.033(4) -0.005(3) -0.009(3) -0.005(3)
C19 0.038(4) 0.042(5) 0.038(4) 0.002(3) 0.009(3) -0.005(3)
C20 0.035(5) 0.045(5) 0.076(6) -0.004(4) 0.004(4) -0.004(4)
C21 0.024(4) 0.065(6) 0.068(6) 0.009(5) 0.003(4) -0.004(4)
C22 0.035(4) 0.030(4) 0.060(5) 0.007(4) -0.011(4) -0.014(3)
C23 0.044(5) 0.027(4) 0.040(4) 0.006(3) 0.000(3) -0.010(3)
C24 0.032(4) 0.028(4) 0.041(4) -0.004(3) -0.005(3) -0.012(3)
C25 0.029(4) 0.028(4) 0.036(4) 0.004(4) 0.001(3) -0.001(3)
C26 0.043(5) 0.053(5) 0.043(5) -0.002(4) 0.001(4) -0.025(4)
C27 0.082(7) 0.038(5) 0.099(7) -0.009(5) 0.008(6) -0.015(5)
C28 0.045(5) 0.081(6) 0.122(7) 0.008(5) -0.009(5) -0.030(5)
C29 0.119(7) 0.085(6) 0.089(6) -0.019(5) 0.042(5) -0.043(6)
C30 0.041(5) 0.026(4) 0.036(5) 0.001(4) 0.015(4) -0.008(3)
C31 0.037(5) 0.047(5) 0.036(4) -0.005(4) 0.002(3) 0.006(4)
C32 0.031(5) 0.071(7) 0.102(7) -0.008(5) 0.012(5) 0.000(4)
C33 0.043(5) 0.048(5) 0.083(6) -0.007(5) -0.008(4) 0.012(4)
C34 0.063(6) 0.101(8) 0.056(6) -0.009(5) 0.018(5) 0.035(5)
C35 0.017(4) 0.025(4) 0.035(4) 0.000(3) 0.009(3) 0.005(3)
C36 0.029(4) 0.020(4) 0.043(4) 0.007(3) 0.003(3) 0.003(3)
C37A 0.048(11) 0.045(11) 0.047(11) 0.005(9) -0.004(9) -0.003(9)
C38A 0.051(11) 0.037(11) 0.053(11) 0.000(9) -0.003(9) 0.001(9)
C39A 0.048(11) 0.041(11) 0.044(11) -0.004(9) 0.005(9) 0.000(9)
C37B 0.054(7) 0.038(6) 0.054(7) 0.005(5) 0.010(6) -0.017(5)
C38B 0.035(6) 0.025(5) 0.058(6) -0.011(5) 0.005(5) 0.000(4)
C39B 0.062(6) 0.034(5) 0.075(7) 0.020(5) -0.013(5) -0.009(5)
C40 0.077(6) 0.030(5) 0.045(5) 0.002(4) 0.005(5) -0.006(4)
C41 0.060(6) 0.059(6) 0.073(6) 0.015(5) 0.023(5) -0.017(5)
C42A 0.117(19) 0.117(19) 0.115(18) 0.003(10) 0.006(10) -0.007(10)
C43A 0.087(14) 0.073(13) 0.084(13) 0.013(9) 0.019(9) -0.008(9)
C44A 0.065(12) 0.074(12) 0.072(12) 0.009(9) 0.019(9) -0.014(9)
C42B 0.072(8) 0.080(8) 0.095(8) 0.004(7) 0.003(7) -0.039(7)
C43B 0.060(7) 0.058(7) 0.075(7) 0.002(6) 0.027(6) -0.003(6)
C44B 0.092(9) 0.109(9) 0.135(10) 0.047(8) 0.043(8) -0.006(8)
C45 0.034(5) 0.014(4) 0.045(5) 0.001(3) -0.004(4) -0.002(3)
C46 0.026(4) 0.034(4) 0.036(4) -0.003(3) -0.012(3) 0.001(3)
C47A 0.051(17) 0.048(17) 0.039(15) 0.006(14) 0.002(13) 0.009(14)
C48A 0.037(11) 0.041(11) 0.036(11) 0.000(8) -0.005(8) 0.012(8)
C49A 0.071(17) 0.058(14) 0.076(18) 0.005(13) -0.009(14) -0.026(13)
C47B 0.040(7) 0.080(8) 0.068(7) -0.008(7) 0.001(5) 0.021(6)
C48B 0.067(8) 0.059(8) 0.107(9) 0.031(7) -0.026(7) 0.006(7)
C49B 0.052(5) 0.061(5) 0.050(5) -0.012(4) -0.009(4) 0.015(4)
C50 0.024(4) 0.025(4) 0.032(4) -0.003(3) 0.005(3) -0.002(3)
C51 0.032(4) 0.035(4) 0.028(4) -0.006(3) -0.002(3) 0.004(3)
C52 0.056(5) 0.051(5) 0.026(4) -0.003(4) 0.001(3) 0.008(4)
C53 0.051(5) 0.036(5) 0.045(5) -0.008(4) 0.002(4) -0.009(4)
C54 0.041(5) 0.055(5) 0.043(5) -0.010(4) -0.002(4) 0.013(4)
C55 0.030(4) 0.030(4) 0.027(4) 0.002(3) 0.001(3) -0.003(3)
C56 0.035(4) 0.038(5) 0.042(5) 0.019(4) 0.011(3) 0.008(4)
C57 0.040(5) 0.091(7) 0.046(5) 0.031(5) 0.010(4) 0.013(4)
C58 0.076(7) 0.036(5) 0.100(7) 0.031(5) 0.031(5) 0.017(5)
C59 0.052(5) 0.038(5) 0.065(5) 0.017(4) 0.015(4) -0.010(4)
N1 0.030(4) 0.050(4) 0.027(3) 0.003(3) 0.002(3) 0.017(3)
N2 0.033(3) 0.028(4) 0.032(3) -0.008(3) 0.006(3) -0.005(3)
N3 0.040(4) 0.028(3) 0.028(3) 0.003(3) 0.003(3) -0.004(3)
N4 0.029(3) 0.024(3) 0.036(4) 0.000(3) 0.001(3) -0.001(3)
O1 0.020(2) 0.035(3) 0.033(3) -0.004(2) 0.000(2) 0.006(2)
O2 0.028(3) 0.029(3) 0.024(2) -0.0011(19) -0.0049(19) 0.006(2)
O3 0.024(2) 0.021(2) 0.024(2) -0.0006(19) -0.0026(18) 0.0014(19)
O4 0.034(3) 0.021(2) 0.028(2) 0.001(2) -0.006(2) -0.002(2)
O5 0.032(3) 0.036(3) 0.034(3) 0.002(2) 0.003(2) -0.008(2)
O6 0.036(3) 0.032(3) 0.031(3) -0.002(2) -0.001(2) -0.006(2)
O7 0.038(3) 0.054(3) 0.035(3) -0.010(2) 0.007(2) 0.003(2)
O8 0.022(3) 0.065(4) 0.035(3) -0.013(2) 0.001(2) -0.002(2)
O9 0.043(3) 0.021(3) 0.040(3) 0.001(2) -0.011(2) 0.003(2)
O10 0.042(3) 0.023(3) 0.030(3) 0.003(2) -0.004(2) -0.001(2)
O11 0.049(3) 0.039(3) 0.034(3) 0.004(2) 0.011(2) -0.020(2)
O12 0.084(4) 0.071(4) 0.040(3) 0.010(3) -0.008(3) -0.035(3)
O13 0.028(3) 0.028(3) 0.029(2) -0.002(2) -0.004(2) 0.008(2)
O14 0.038(3) 0.043(3) 0.032(3) -0.007(2) -0.001(2) 0.005(2)
O15 0.036(3) 0.037(3) 0.022(2) -0.005(2) -0.001(2) 0.001(2)
O16 0.021(2) 0.040(3) 0.024(2) 0.001(2) -0.0035(19) 0.003(2)
O17 0.032(3) 0.029(3) 0.031(3) 0.010(2) 0.003(2) 0.006(2)
O18 0.035(3) 0.028(3) 0.037(3) 0.005(2) -0.005(2) 0.005(2)
O19 0.020(2) 0.031(3) 0.021(2) 0.0001(19) 0.0015(17) 0.0012(19)
O20 0.029(2) 0.022(2) 0.024(2) -0.0007(19) 0.0024(19) 0.001(2)
Fe1 0.0244(5) 0.0290(5) 0.0253(5) 0.0004(4) -0.0008(4) 0.0019(4)
Fe2 0.0259(5) 0.0281(5) 0.0253(5) -0.0020(4) -0.0011(4) -0.0006(4)
Fe3 0.0265(5) 0.0249(5) 0.0260(5) -0.0020(4) 0.0013(4) -0.0033(4)
Fe4 0.0299(5) 0.0213(5) 0.0248(5) -0.0015(4) -0.0016(4) -0.0001(4)
Fe5 0.0235(5) 0.0256(5) 0.0259(5) 0.0001(4) -0.0019(4) -0.0005(4)
O21 0.082(16) 0.057(13) 0.101(16) 0.018(12) -0.014(12) -0.020(11)
_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
C1 C2 1.473(10) . ?
C1 N1 1.488(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.532(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.527(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.482(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N1 1.506(9) . ?
C5 C6 1.545(9) . ?
C5 H5 0.9800 . ?
C6 O1 1.409(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N2 1.475(8) . ?
C7 C8 1.528(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.505(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.511(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.519(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.484(8) . ?
C11 C12 1.514(9) . ?
C11 H11 0.9800 . ?
C12 O2 1.426(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N3 1.443(8) . ?
C13 C14 1.533(10) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.516(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.512(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.510(9) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 N3 1.495(8) . ?
C17 C18 1.498(9) . ?
C17 H17 0.9800 . ?
C18 O3 1.417(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N4 1.483(8) . ?
C19 C20 1.526(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.481(10) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.524(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.514(9) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 N4 1.486(8) . ?
C23 C24 1.530(9) . ?
C23 H23 0.9800 . ?
C24 O4 1.421(7) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 O6 1.257(7) . ?
C25 O5 1.263(7) . ?
C25 C26 1.538(9) . ?
C26 C28 1.488(11) . ?
C26 C29 1.505(10) . ?
C26 C27 1.516(11) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 O8 1.237(8) . ?
C30 O7 1.252(7) . ?
C30 C31 1.533(9) . ?
C31 C34 1.512(9) . ?
C31 C32 1.514(10) . ?
C31 C33 1.523(10) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 O10 1.240(7) . ?
C35 O9 1.252(7) . ?
C35 C36 1.520(8) . ?
C36 C39B 1.495(11) . ?
C36 C38A 1.52(3) . ?
C36 C37B 1.505(11) . ?
C36 C39A 1.533(17) . ?
C36 C38B 1.560(9) . ?
C36 C37A 1.564(17) . ?
C37A H37A 0.9600 . ?
C37A H37B 0.9600 . ?
C37A H37C 0.9600 . ?
C38A H38A 0.9600 . ?
C38A H38B 0.9600 . ?
C38A H38C 0.9600 . ?
C39A H39A 0.9600 . ?
C39A H39B 0.9600 . ?
C39A H39C 0.9600 . ?
C37B H37D 0.9600 . ?
C37B H37E 0.9600 . ?
C37B H37F 0.9600 . ?
C38B H38D 0.9600 . ?
C38B H38E 0.9600 . ?
C38B H38F 0.9600 . ?
C39B H39D 0.9600 . ?
C39B H39E 0.9600 . ?
C39B H39F 0.9600 . ?
C40 O12 1.209(9) . ?
C40 O11 1.286(8) . ?
C40 C41 1.554(11) . ?
C41 C42A 1.514(10) . ?
C41 C43A 1.519(10) . ?
C41 C43B 1.524(8) . ?
C41 C42B 1.524(9) . ?
C41 C44B 1.528(9) . ?
C41 C44A 1.541(10) . ?
C42A H42A 0.9600 . ?
C42A H42B 0.9600 . ?
C42A H42C 0.9600 . ?
C43A H43A 0.9600 . ?
C43A H43B 0.9600 . ?
C43A H43C 0.9600 . ?
C44A H44A 0.9600 . ?
C44A H44B 0.9600 . ?
C44A H44C 0.9600 . ?
C42B H42D 0.9600 . ?
C42B H42E 0.9600 . ?
C42B H42F 0.9600 . ?
C43B H43D 0.9600 . ?
C43B H43E 0.9600 . ?
C43B H43F 0.9600 . ?
C44B H44D 0.9600 . ?
C44B H44E 0.9600 . ?
C44B H44F 0.9600 . ?
C45 O14 1.238(7) . ?
C45 O13 1.280(7) . ?
C45 C46 1.546(9) . ?
C46 C48B 1.485(12) . ?
C46 C49A 1.527(10) . ?
C46 C49B 1.526(11) . ?
C46 C48A 1.531(10) . ?
C46 C47A 1.53(3) . ?
C46 C47B 1.575(12) . ?
C47A H47A 0.9600 . ?
C47A H47B 0.9600 . ?
C47A H47C 0.9600 . ?
C48A H48A 0.9600 . ?
C48A H48B 0.9600 . ?
C48A H48C 0.9600 . ?
C49A H49A 0.9600 . ?
C49A H49B 0.9600 . ?
C49A H49C 0.9600 . ?
C47B H47D 0.9600 . ?
C47B H47E 0.9600 . ?
C47B H47F 0.9600 . ?
C48B H48D 0.9600 . ?
C48B H48E 0.9600 . ?
C48B H48F 0.9600 . ?
C49B H49D 0.9600 . ?
C49B H49E 0.9600 . ?
C49B H49F 0.9600 . ?
C50 O15 1.251(7) . ?
C50 O16 1.268(7) . ?
C50 C51 1.516(9) . ?
C51 C54 1.534(9) . ?
C51 C53 1.533(9) . ?
C51 C52 1.548(9) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 O17 1.268(7) . ?
C55 O18 1.263(7) . ?
C55 C56 1.515(9) . ?
C56 C59 1.518(9) . ?
C56 C57 1.533(10) . ?
C56 C58 1.549(9) . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
N1 Fe1 2.174(5) . ?
N1 H1 0.85(2) . ?
N2 Fe3 2.167(5) . ?
N2 H2 0.85(2) . ?
N3 Fe4 2.177(5) . ?
N3 H3 0.85(2) . ?
N4 Fe5 2.163(5) . ?
N4 H4 0.85(2) . ?
O1 Fe1 1.955(4) . ?
O1 Fe2 2.070(4) . ?
O2 Fe4 1.959(4) . ?
O2 Fe3 1.983(4) . ?
O3 Fe5 1.985(4) . ?
O3 Fe4 1.997(4) . ?
O4 Fe4 2.031(4) . ?
O4 Fe5 2.044(4) . ?
O5 Fe1 2.072(4) . ?
O6 Fe2 2.066(4) . ?
O7 Fe2 2.049(4) . ?
O8 Fe3 2.030(4) . ?
O9 Fe2 2.018(4) . ?
O10 Fe3 2.066(4) . ?
O11 Fe3 1.988(4) . ?
O13 Fe4 2.007(4) . ?
O15 Fe5 2.043(4) . ?
O16 Fe1 2.028(4) . ?
O17 Fe5 2.082(4) . ?
O18 Fe1 2.025(4) . ?
O19 Fe5 1.844(4) . ?
O19 Fe1 1.864(4) . ?
O19 Fe2 1.959(4) . ?
O20 Fe2 1.861(4) . ?
O20 Fe3 1.899(4) . ?
O20 Fe4 2.048(4) . ?
Fe1 Fe2 2.9539(12) . ?
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
C2 C1 N1 113.8(6) . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
N1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C1 C2 C3 112.0(7) . . ?
C1 C2 H2A 109.2 . . ?
C3 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
C3 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C2 C3 C4 108.7(7) . . ?
C2 C3 H3A 110.0 . . ?
C4 C3 H3A 110.0 . . ?
C2 C3 H3B 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.3 . . ?
C5 C4 C3 110.7(7) . . ?
C5 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
C4 C5 N1 112.5(6) . . ?
C4 C5 C6 117.6(7) . . ?
N1 C5 C6 105.9(6) . . ?
C4 C5 H5 106.8 . . ?
N1 C5 H5 106.8 . . ?
C6 C5 H5 106.8 . . ?
O1 C6 C5 106.3(6) . . ?
O1 C6 H6A 110.5 . . ?
C5 C6 H6A 110.5 . . ?
O1 C6 H6B 110.5 . . ?
C5 C6 H6B 110.5 . . ?
H6A C6 H6B 108.7 . . ?
N2 C7 C8 110.8(6) . . ?
N2 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C9 C8 C7 111.8(6) . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
C8 C9 C10 111.2(6) . . ?
C8 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C9 C10 C11 110.8(6) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N2 C11 C12 108.4(5) . . ?
N2 C11 C10 111.9(5) . . ?
C12 C11 C10 114.5(5) . . ?
N2 C11 H11 107.2 . . ?
C12 C11 H11 107.2 . . ?
C10 C11 H11 107.2 . . ?
O2 C12 C11 108.2(5) . . ?
O2 C12 H12A 110.0 . . ?
C11 C12 H12A 110.0 . . ?
O2 C12 H12B 110.0 . . ?
C11 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
N3 C13 C14 113.0(6) . . ?
N3 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
N3 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C15 C14 C13 110.9(7) . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C14 109.7(7) . . ?
C16 C15 H15A 109.7 . . ?
C14 C15 H15A 109.7 . . ?
C16 C15 H15B 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C17 C16 C15 111.0(6) . . ?
C17 C16 H16A 109.4 . . ?
C15 C16 H16A 109.4 . . ?
C17 C16 H16B 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
N3 C17 C18 106.8(5) . . ?
N3 C17 C16 112.1(6) . . ?
C18 C17 C16 116.4(6) . . ?
N3 C17 H17 107.0 . . ?
C18 C17 H17 107.0 . . ?
C16 C17 H17 107.0 . . ?
O3 C18 C17 108.1(5) . . ?
O3 C18 H18A 110.1 . . ?
C17 C18 H18A 110.1 . . ?
O3 C18 H18B 110.1 . . ?
C17 C18 H18B 110.1 . . ?
H18A C18 H18B 108.4 . . ?
N4 C19 C20 113.4(6) . . ?
N4 C19 H19A 108.9 . . ?
C20 C19 H19A 108.9 . . ?
N4 C19 H19B 108.9 . . ?
C20 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C21 C20 C19 110.9(6) . . ?
C21 C20 H20A 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C20 C21 C22 112.0(6) . . ?
C20 C21 H21A 109.2 . . ?
C22 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
C22 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C21 C22 C23 110.2(5) . . ?
C21 C22 H22A 109.6 . . ?
C23 C22 H22A 109.6 . . ?
C21 C22 H22B 109.6 . . ?
C23 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
N4 C23 C22 112.7(5) . . ?
N4 C23 C24 108.7(5) . . ?
C22 C23 C24 113.2(5) . . ?
N4 C23 H23 107.3 . . ?
C22 C23 H23 107.3 . . ?
C24 C23 H23 107.3 . . ?
O4 C24 C23 111.9(5) . . ?
O4 C24 H24A 109.2 . . ?
C23 C24 H24A 109.2 . . ?
O4 C24 H24B 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
O6 C25 O5 125.7(6) . . ?
O6 C25 C26 117.8(6) . . ?
O5 C25 C26 116.5(6) . . ?
C28 C26 C29 112.1(7) . . ?
C28 C26 C27 108.8(7) . . ?
C29 C26 C27 110.0(7) . . ?
C28 C26 C25 108.0(6) . . ?
C29 C26 C25 110.2(6) . . ?
C27 C26 C25 107.8(6) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O8 C30 O7 125.8(6) . . ?
O8 C30 C31 117.2(6) . . ?
O7 C30 C31 117.0(6) . . ?
C34 C31 C32 110.6(7) . . ?
C34 C31 C33 108.6(7) . . ?
C32 C31 C33 108.4(6) . . ?
C34 C31 C30 112.4(6) . . ?
C32 C31 C30 110.8(6) . . ?
C33 C31 C30 105.8(6) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O10 C35 O9 125.7(6) . . ?
O10 C35 C36 118.7(6) . . ?
O9 C35 C36 115.6(6) . . ?
C39B C36 C38A 135.9(12) . . ?
C39B C36 C37B 112.9(7) . . ?
C38A C36 C37B 55.0(12) . . ?
C39B C36 C35 110.8(6) . . ?
C38A C36 C35 113.2(12) . . ?
C37B C36 C35 108.2(6) . . ?
C38A C36 C39A 117.1(17) . . ?
C37B C36 C39A 143.8(13) . . ?
C35 C36 C39A 106.9(12) . . ?
C39B C36 C38B 108.1(7) . . ?
C38A C36 C38B 54.4(12) . . ?
C37B C36 C38B 108.3(7) . . ?
C35 C36 C38B 108.5(6) . . ?
C39A C36 C38B 68.1(12) . . ?
C39B C36 C37A 64.2(12) . . ?
C38A C36 C37A 104.5(17) . . ?
C37B C36 C37A 53.0(11) . . ?
C35 C36 C37A 107.4(12) . . ?
C39A C36 C37A 107.2(17) . . ?
C38B C36 C37A 143.5(12) . . ?
C36 C37A H37A 109.5 . . ?
C36 C37A H37B 109.5 . . ?
H37A C37A H37B 109.5 . . ?
C36 C37A H37C 109.5 . . ?
H37A C37A H37C 109.5 . . ?
H37B C37A H37C 109.5 . . ?
C36 C38A H38A 109.5 . . ?
C36 C38A H38B 109.5 . . ?
H38A C38A H38B 109.5 . . ?
C36 C38A H38C 109.5 . . ?
H38A C38A H38C 109.5 . . ?
H38B C38A H38C 109.5 . . ?
C36 C39A H39A 109.5 . . ?
C36 C39A H39B 109.5 . . ?
H39A C39A H39B 109.5 . . ?
C36 C39A H39C 109.5 . . ?
H39A C39A H39C 109.5 . . ?
H39B C39A H39C 109.5 . . ?
C36 C37B H37D 109.5 . . ?
C36 C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
C36 C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
C36 C38B H38D 109.5 . . ?
C36 C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C36 C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C36 C39B H39D 109.5 . . ?
C36 C39B H39E 109.5 . . ?
H39D C39B H39E 109.5 . . ?
C36 C39B H39F 109.5 . . ?
H39D C39B H39F 109.5 . . ?
H39E C39B H39F 109.5 . . ?
O12 C40 O11 125.0(8) . . ?
O12 C40 C41 119.0(7) . . ?
O11 C40 C41 115.9(7) . . ?
C42A C41 C43A 115(3) . . ?
C42A C41 C43B 122.2(19) . . ?
C43A C41 C42B 91.6(14) . . ?
C43B C41 C42B 108.9(10) . . ?
C42A C41 C44B 72.2(19) . . ?
C43A C41 C44B 133.2(12) . . ?
C43B C41 C44B 112.2(10) . . ?
C42B C41 C44B 107.1(11) . . ?
C42A C41 C44A 108(2) . . ?
C43A C41 C44A 109.5(14) . . ?
C43B C41 C44A 87.0(14) . . ?
C42B C41 C44A 142.4(16) . . ?
C42A C41 C40 121.5(19) . . ?
C43A C41 C40 104.5(18) . . ?
C43B C41 C40 111.2(9) . . ?
C42B C41 C40 108.0(8) . . ?
C44B C41 C40 109.3(8) . . ?
C44A C41 C40 96.7(13) . . ?
C41 C42A H42A 109.5 . . ?
C41 C42A H42B 109.5 . . ?
H42A C42A H42B 109.5 . . ?
C41 C42A H42C 109.5 . . ?
H42A C42A H42C 109.5 . . ?
H42B C42A H42C 109.5 . . ?
C41 C43A H43A 109.5 . . ?
C41 C43A H43B 109.5 . . ?
H43A C43A H43B 109.5 . . ?
C41 C43A H43C 109.5 . . ?
H43A C43A H43C 109.5 . . ?
H43B C43A H43C 109.5 . . ?
C41 C44A H44A 109.5 . . ?
C41 C44A H44B 109.5 . . ?
H44A C44A H44B 109.5 . . ?
C41 C44A H44C 109.5 . . ?
H44A C44A H44C 109.5 . . ?
H44B C44A H44C 109.5 . . ?
C41 C42B H42D 109.5 . . ?
C41 C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
C41 C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?
C41 C43B H43D 109.5 . . ?
C41 C43B H43E 109.5 . . ?
H43D C43B H43E 109.5 . . ?
C41 C43B H43F 109.5 . . ?
H43D C43B H43F 109.5 . . ?
H43E C43B H43F 109.5 . . ?
C41 C44B H44D 109.5 . . ?
C41 C44B H44E 109.5 . . ?
H44D C44B H44E 109.5 . . ?
C41 C44B H44F 109.5 . . ?
H44D C44B H44F 109.5 . . ?
H44E C44B H44F 109.5 . . ?
O14 C45 O13 125.0(6) . . ?
O14 C45 C46 119.7(6) . . ?
O13 C45 C46 115.3(6) . . ?
C48B C46 C49A 134.8(18) . . ?
C48B C46 C49B 109.9(8) . . ?
C49A C46 C48A 104(2) . . ?
C49B C46 C48A 73.2(14) . . ?
C48B C46 C47A 72.6(15) . . ?
C49A C46 C47A 111(2) . . ?
C49B C46 C47A 132.9(16) . . ?
C48A C46 C47A 107.4(19) . . ?
C48B C46 C45 108.2(6) . . ?
C49A C46 C45 110.3(17) . . ?
C49B C46 C45 110.0(6) . . ?
C48A C46 C45 109.5(13) . . ?
C47A C46 C45 113.5(14) . . ?
C48B C46 C47B 110.2(8) . . ?
C49A C46 C47B 77.3(19) . . ?
C49B C46 C47B 108.2(7) . . ?
C48A C46 C47B 136.5(14) . . ?
C45 C46 C47B 110.3(6) . . ?
C46 C47A H47A 109.5 . . ?
C46 C47A H47B 109.5 . . ?
H47A C47A H47B 109.5 . . ?
C46 C47A H47C 109.5 . . ?
H47A C47A H47C 109.5 . . ?
H47B C47A H47C 109.5 . . ?
C46 C48A H48A 109.5 . . ?
C46 C48A H48B 109.5 . . ?
H48A C48A H48B 109.5 . . ?
C46 C48A H48C 109.5 . . ?
H48A C48A H48C 109.5 . . ?
H48B C48A H48C 109.5 . . ?
C46 C49A H49A 109.5 . . ?
C46 C49A H49B 109.5 . . ?
H49A C49A H49B 109.5 . . ?
C46 C49A H49C 109.5 . . ?
H49A C49A H49C 109.5 . . ?
H49B C49A H49C 109.5 . . ?
C46 C47B H47D 109.5 . . ?
C46 C47B H47E 109.5 . . ?
H47D C47B H47E 109.5 . . ?
C46 C47B H47F 109.5 . . ?
H47D C47B H47F 109.5 . . ?
H47E C47B H47F 109.5 . . ?
C46 C48B H48D 109.5 . . ?
C46 C48B H48E 109.5 . . ?
H48D C48B H48E 109.5 . . ?
C46 C48B H48F 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C46 C49B H49D 109.5 . . ?
C46 C49B H49E 109.5 . . ?
H49D C49B H49E 109.5 . . ?
C46 C49B H49F 109.5 . . ?
H49D C49B H49F 109.5 . . ?
H49E C49B H49F 109.5 . . ?
O15 C50 O16 124.3(6) . . ?
O15 C50 C51 119.2(6) . . ?
O16 C50 C51 116.3(6) . . ?
C50 C51 C54 111.1(5) . . ?
C50 C51 C53 106.3(5) . . ?
C54 C51 C53 110.9(6) . . ?
C50 C51 C52 108.4(5) . . ?
C54 C51 C52 110.8(5) . . ?
C53 C51 C52 109.1(6) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O17 C55 O18 124.9(6) . . ?
O17 C55 C56 119.4(6) . . ?
O18 C55 C56 115.6(6) . . ?
C55 C56 C59 111.1(5) . . ?
C55 C56 C57 104.9(6) . . ?
C59 C56 C57 110.1(6) . . ?
C55 C56 C58 110.4(6) . . ?
C59 C56 C58 110.3(7) . . ?
C57 C56 C58 110.0(6) . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C56 C59 H59A 109.5 . . ?
C56 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C56 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C1 N1 C5 108.9(6) . . ?
C1 N1 Fe1 120.3(4) . . ?
C5 N1 Fe1 105.2(4) . . ?
C1 N1 H1 118(5) . . ?
C5 N1 H1 101(5) . . ?
Fe1 N1 H1 101(5) . . ?
C7 N2 C11 113.1(5) . . ?
C7 N2 Fe3 119.2(4) . . ?
C11 N2 Fe3 106.4(4) . . ?
C7 N2 H2 112(5) . . ?
C11 N2 H2 104(5) . . ?
Fe3 N2 H2 99(5) . . ?
C13 N3 C17 110.9(5) . . ?
C13 N3 Fe4 119.8(4) . . ?
C17 N3 Fe4 106.3(4) . . ?
C13 N3 H3 121(5) . . ?
C17 N3 H3 92(5) . . ?
Fe4 N3 H3 102(5) . . ?
C19 N4 C23 111.3(5) . . ?
C19 N4 Fe5 121.7(4) . . ?
C23 N4 Fe5 106.6(4) . . ?
C19 N4 H4 118(5) . . ?
C23 N4 H4 104(5) . . ?
Fe5 N4 H4 92(5) . . ?
C6 O1 Fe1 117.5(4) . . ?
C6 O1 Fe2 140.5(4) . . ?
Fe1 O1 Fe2 94.39(17) . . ?
C12 O2 Fe4 138.1(4) . . ?
C12 O2 Fe3 120.1(3) . . ?
Fe4 O2 Fe3 100.82(17) . . ?
C18 O3 Fe5 132.7(3) . . ?
C18 O3 Fe4 116.9(3) . . ?
Fe5 O3 Fe4 100.86(18) . . ?
C24 O4 Fe4 120.6(4) . . ?
C24 O4 Fe5 117.2(3) . . ?
Fe4 O4 Fe5 97.76(17) . . ?
C25 O5 Fe1 124.7(4) . . ?
C25 O6 Fe2 128.8(4) . . ?
C30 O7 Fe2 129.7(4) . . ?
C30 O8 Fe3 127.6(4) . . ?
C35 O9 Fe2 133.8(4) . . ?
C35 O10 Fe3 127.6(4) . . ?
C40 O11 Fe3 132.9(5) . . ?
C45 O13 Fe4 137.5(4) . . ?
C50 O15 Fe5 131.6(4) . . ?
C50 O16 Fe1 129.5(4) . . ?
C55 O17 Fe5 134.3(4) . . ?
C55 O18 Fe1 127.7(4) . . ?
Fe5 O19 Fe1 121.1(2) . . ?
Fe5 O19 Fe2 137.1(2) . . ?
Fe1 O19 Fe2 101.15(18) . . ?
Fe2 O20 Fe3 116.6(2) . . ?
Fe2 O20 Fe4 132.4(2) . . ?
Fe3 O20 Fe4 100.58(17) . . ?
O19 Fe1 O1 82.74(17) . . ?
O19 Fe1 O18 94.33(17) . . ?
O1 Fe1 O18 97.98(18) . . ?
O19 Fe1 O16 100.95(16) . . ?
O1 Fe1 O16 172.75(18) . . ?
O18 Fe1 O16 88.01(17) . . ?
O19 Fe1 O5 95.04(17) . . ?
O1 Fe1 O5 87.70(17) . . ?
O18 Fe1 O5 169.59(17) . . ?
O16 Fe1 O5 85.77(17) . . ?
O19 Fe1 N1 163.08(19) . . ?
O1 Fe1 N1 80.43(19) . . ?
O18 Fe1 N1 86.3(2) . . ?
O16 Fe1 N1 95.97(18) . . ?
O5 Fe1 N1 86.1(2) . . ?
O19 Fe1 Fe2 40.59(12) . . ?
O1 Fe1 Fe2 44.33(12) . . ?
O18 Fe1 Fe2 108.62(12) . . ?
O16 Fe1 Fe2 137.22(12) . . ?
O5 Fe1 Fe2 81.53(12) . . ?
N1 Fe1 Fe2 123.47(15) . . ?
O20 Fe2 O19 95.55(16) . . ?
O20 Fe2 O9 94.40(17) . . ?
O19 Fe2 O9 94.64(17) . . ?
O20 Fe2 O7 98.92(17) . . ?
O19 Fe2 O7 165.21(17) . . ?
O9 Fe2 O7 87.29(19) . . ?
O20 Fe2 O6 97.63(18) . . ?
O19 Fe2 O6 90.24(17) . . ?
O9 Fe2 O6 166.52(18) . . ?
O7 Fe2 O6 84.87(18) . . ?
O20 Fe2 O1 171.88(17) . . ?
O19 Fe2 O1 77.56(16) . . ?
O9 Fe2 O1 82.02(17) . . ?
O7 Fe2 O1 88.22(17) . . ?
O6 Fe2 O1 86.79(17) . . ?
O20 Fe2 Fe1 132.87(12) . . ?
O19 Fe2 Fe1 38.26(11) . . ?
O9 Fe2 Fe1 97.59(13) . . ?
O7 Fe2 Fe1 126.95(13) . . ?
O6 Fe2 Fe1 78.58(12) . . ?
O1 Fe2 Fe1 41.28(11) . . ?
O20 Fe3 O2 80.79(16) . . ?
O20 Fe3 O11 96.38(18) . . ?
O2 Fe3 O11 97.57(18) . . ?
O20 Fe3 O8 105.79(18) . . ?
O2 Fe3 O8 171.93(18) . . ?
O11 Fe3 O8 86.45(19) . . ?
O20 Fe3 O10 93.58(17) . . ?
O2 Fe3 O10 90.74(17) . . ?
O11 Fe3 O10 167.92(18) . . ?
O8 Fe3 O10 84.27(18) . . ?
O20 Fe3 N2 158.44(19) . . ?
O2 Fe3 N2 78.33(18) . . ?
O11 Fe3 N2 91.63(19) . . ?
O8 Fe3 N2 94.63(19) . . ?
O10 Fe3 N2 81.45(18) . . ?
O2 Fe4 O3 175.55(17) . . ?
O2 Fe4 O13 85.55(16) . . ?
O3 Fe4 O13 98.77(16) . . ?
O2 Fe4 O4 102.31(17) . . ?
O3 Fe4 O4 78.15(16) . . ?
O13 Fe4 O4 99.19(17) . . ?
O2 Fe4 O20 77.80(16) . . ?
O3 Fe4 O20 97.76(16) . . ?
O13 Fe4 O20 160.83(16) . . ?
O4 Fe4 O20 93.64(16) . . ?
O2 Fe4 N3 100.03(19) . . ?
O3 Fe4 N3 79.13(18) . . ?
O13 Fe4 N3 88.28(19) . . ?
O4 Fe4 N3 156.90(18) . . ?
O20 Fe4 N3 85.37(19) . . ?
O19 Fe5 O3 93.11(16) . . ?
O19 Fe5 O15 96.91(17) . . ?
O3 Fe5 O15 91.24(16) . . ?
O19 Fe5 O4 97.68(17) . . ?
O3 Fe5 O4 78.11(16) . . ?
O15 Fe5 O4 162.36(17) . . ?
O19 Fe5 O17 91.43(17) . . ?
O3 Fe5 O17 174.72(17) . . ?
O15 Fe5 O17 90.88(17) . . ?
O4 Fe5 O17 98.61(17) . . ?
O19 Fe5 N4 173.51(19) . . ?
O3 Fe5 N4 90.01(18) . . ?
O15 Fe5 N4 88.70(19) . . ?
O4 Fe5 N4 77.40(18) . . ?
O17 Fe5 N4 85.21(18) . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 0.812
_refine_diff_density_min -0.581
_refine_diff_density_rms 0.090
# start Validation Reply Form
_vrf_PLAT220_ck9
;
RESPONSE: This is due to the disorder of the t-butyl moieties of
three pivalic ligands of the complex.
;
_vrf_PLAT222_ck9
;
RESPONSE: This is due to the disorder of the t-butyl moieties of
three pivalic ligands of the complex.
;
_vrf_PLAT430_ck9
;
RESPONSE: This short distance assumes a strong H-bonding between
the partially occupied O21 crystallization water molecule (whose
H-atoms have not been located in the course of the X-ray analysis)
and O6 oxygen of a pivalic ligand.
;
_vrf_PLAT311_ck9
;
RESPONSE: See comment above.
;
_vrf_PLAT731_ck9
;
RESPONSE: The distance has been restrainted by means of a DFIX instruction.
;
_vrf_PLAT041_ck9
;
RESPONSE: The missing (not located by a difference synthesis) hydrogen
atoms of the O21 crystallization water molecule have been included
in the sum and moiety formula and the Mr, Dx, Mu and F(000) have been
modified accordingly. These modifications account for the differences
detected in the relevant data items.
;
_vrf_FORMU01_ck9
;
RESPONSE: See comment above.
;
_vrf_PLAT301_ck9
;
RESPONSE: See _refine_special_details.
;
# end Validation Reply Form
#===END
# Attachment '- 3.cif'
data_ck11
_database_code_depnum_ccdc_archive 'CCDC 836726'
#TrackingRef '- 3.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety '(C73 H83 Fe5 N4 O20), 1.3(C2 H3 N), (H2 O)'
_chemical_formula_sum 'C75.60 H88.90 Fe5 N5.30 O21'
_chemical_formula_weight 1687.07
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/c 1'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 24.0638(5)
_cell_length_b 14.2734(2)
_cell_length_c 25.8406(6)
_cell_angle_alpha 90.00
_cell_angle_beta 111.120(2)
_cell_angle_gamma 90.00
_cell_volume 8279.3(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 16638
_cell_measurement_theta_min 3.1880
_cell_measurement_theta_max 30.3952
_exptl_crystal_description prism
_exptl_crystal_colour 'dark grey-purple'
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.353
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3510
_exptl_absorpt_coefficient_mu 0.926
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.756
_exptl_absorpt_correction_T_max 0.910
_exptl_absorpt_process_details
'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur-3 with Sapphire CCD'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 16.0288
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 56769
_diffrn_reflns_av_R_equivalents 0.0514
_diffrn_reflns_av_sigmaI/netI 0.1128
_diffrn_reflns_limit_h_min -29
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_theta_min 3.20
_diffrn_reflns_theta_max 26.00
_reflns_number_total 16146
_reflns_number_gt 8037
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics
;
PLATON (Spek, 2008), ORTEP-3 (Farrugia, 1997)
;
_computing_publication_material 'WINGX (Farrugia, 1999)'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436.
Farrugia, L. J. (1997). ORTEP-3 for Windows. J.Appl. Cryst.
30, 565.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838.
Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford
Diffraction Ltd, Abingdon, Oxford, England.
Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany.
Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands.
;
_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^)+(0.0692P)^2^] 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 16146
_refine_ls_number_parameters 1007
_refine_ls_number_restraints 106
_refine_ls_R_factor_all 0.1113
_refine_ls_R_factor_gt 0.0538
_refine_ls_wR_factor_ref 0.1390
_refine_ls_wR_factor_gt 0.1300
_refine_ls_goodness_of_fit_ref 0.948
_refine_ls_restrained_S_all 0.973
_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
N1 N 0.68432(19) -0.1796(3) 0.44413(19) 0.0563(12) Uani 1 1 d D . .
H1N H 0.7135(18) -0.1858(18) 0.4762(12) 0.084 Uiso 1 1 d D . .
N2 N 0.70500(18) 0.4658(3) 0.33003(17) 0.0421(10) Uani 1 1 d D . .
H2N H 0.7328(17) 0.497(3) 0.3553(16) 0.063 Uiso 1 1 d D . .
N3 N 0.78575(16) -0.0052(3) 0.23177(16) 0.0356(9) Uani 1 1 d D . .
H3N H 0.8177(13) 0.025(3) 0.2394(19) 0.053 Uiso 1 1 d D . .
N4 N 0.88476(16) 0.2317(3) 0.40530(16) 0.0407(10) Uani 1 1 d D . .
H4N H 0.868(2) 0.227(3) 0.4299(16) 0.061 Uiso 1 1 d D . .
O1 O 0.78935(13) -0.0738(2) 0.47122(12) 0.0395(8) Uani 1 1 d . . .
O2 O 0.78986(13) 0.0833(2) 0.47769(12) 0.0398(8) Uani 1 1 d . . .
O3 O 0.68846(14) 0.1961(2) 0.45470(12) 0.0450(8) Uani 1 1 d . . .
O4 O 0.67232(15) 0.3343(2) 0.41075(14) 0.0486(9) Uani 1 1 d . . .
O5 O 0.64234(12) 0.1432(2) 0.33751(13) 0.0397(8) Uani 1 1 d . . .
O6 O 0.65547(13) 0.2812(2) 0.30170(12) 0.0402(8) Uani 1 1 d . . .
O7 O 0.79032(15) 0.3802(2) 0.43443(14) 0.0531(9) Uani 1 1 d . . .
O8 O 0.76938(17) 0.5289(3) 0.44565(15) 0.0599(10) Uani 1 1 d . . .
O9 O 0.81983(13) -0.11540(19) 0.33587(12) 0.0349(7) Uani 1 1 d . . .
O10 O 0.77115(13) -0.19311(19) 0.38223(13) 0.0382(8) Uani 1 1 d . . .
O11 O 0.65262(13) -0.1299(2) 0.32482(13) 0.0392(8) Uani 1 1 d . . .
O12 O 0.69709(13) -0.0820(2) 0.26623(12) 0.0384(8) Uani 1 1 d . . .
O13 O 0.85425(13) 0.23843(19) 0.28308(13) 0.0389(8) Uani 1 1 d . . .
O14 O 0.89464(13) 0.1164(2) 0.25452(13) 0.0403(8) Uani 1 1 d . . .
O15 O 0.67347(13) 0.0035(2) 0.42091(12) 0.0396(8) Uani 1 1 d . . .
O16 O 0.77764(13) 0.3339(2) 0.32110(13) 0.0386(8) Uani 1 1 d . . .
O17 O 0.74325(12) 0.13019(19) 0.27505(12) 0.0324(7) Uani 1 1 d . . .
O18 O 0.84292(12) 0.07657(18) 0.34789(12) 0.0310(7) Uani 1 1 d . . .
O19 O 0.74157(12) 0.01220(18) 0.36606(11) 0.0330(7) Uani 1 1 d . . .
O20 O 0.76153(12) 0.20715(19) 0.38224(12) 0.0351(7) Uani 1 1 d . . .
Fe1 Fe 0.71841(3) -0.09262(4) 0.39685(3) 0.03525(18) Uani 1 1 d . . .
Fe2 Fe 0.71895(3) 0.11508(4) 0.40421(3) 0.03588(18) Uani 1 1 d . . .
Fe3 Fe 0.72697(3) 0.32816(5) 0.36734(3) 0.03867(19) Uani 1 1 d . . .
Fe4 Fe 0.77001(3) 0.00120(4) 0.30877(3) 0.03117(16) Uani 1 1 d . . .
Fe5 Fe 0.80798(3) 0.20496(4) 0.33132(3) 0.03296(17) Uani 1 1 d . . .
C1 C 0.8112(2) 0.0026(4) 0.49422(19) 0.0378(11) Uani 1 1 d . . .
C2 C 0.8660(2) -0.0030(4) 0.54399(19) 0.0386(12) Uani 1 1 d . . .
C3 C 0.8879(2) -0.0901(4) 0.5670(2) 0.0463(13) Uani 1 1 d . . .
H3 H 0.8676 -0.1443 0.5509 0.056 Uiso 1 1 calc R . .
C4 C 0.9391(2) -0.0967(4) 0.6133(2) 0.0538(15) Uani 1 1 d . . .
H4 H 0.9528 -0.1550 0.6287 0.065 Uiso 1 1 calc R . .
C5 C 0.9700(2) -0.0172(4) 0.6365(2) 0.0550(15) Uani 1 1 d . . .
H5 H 1.0049 -0.0220 0.6674 0.066 Uiso 1 1 calc R . .
C6 C 0.9494(2) 0.0707(4) 0.6143(2) 0.0569(15) Uani 1 1 d . . .
H6 H 0.9707 0.1243 0.6302 0.068 Uiso 1 1 calc R . .
C7 C 0.8971(2) 0.0780(4) 0.5681(2) 0.0477(13) Uani 1 1 d . . .
H7 H 0.8829 0.1365 0.5534 0.057 Uiso 1 1 calc R . .
C8 C 0.6682(2) 0.2787(4) 0.4464(2) 0.0461(13) Uani 1 1 d . . .
C9 C 0.6368(2) 0.3140(4) 0.4841(2) 0.0476(13) Uani 1 1 d . . .
C10 C 0.6223(2) 0.2543(4) 0.5187(2) 0.0595(15) Uani 1 1 d . . .
H10 H 0.6325 0.1913 0.5200 0.071 Uiso 1 1 calc R . .
C11 C 0.5923(3) 0.2873(4) 0.5519(2) 0.0698(18) Uani 1 1 d . . .
H11 H 0.5819 0.2462 0.5748 0.084 Uiso 1 1 calc R . .
C12 C 0.5781(3) 0.3802(5) 0.5512(3) 0.0751(19) Uani 1 1 d . . .
H12 H 0.5578 0.4017 0.5733 0.090 Uiso 1 1 calc R . .
C13 C 0.5940(3) 0.4433(4) 0.5170(3) 0.0709(17) Uani 1 1 d . . .
H13 H 0.5853 0.5068 0.5172 0.085 Uiso 1 1 calc R . .
C14 C 0.6229(2) 0.4091(4) 0.4830(2) 0.0590(15) Uani 1 1 d . . .
H14 H 0.6329 0.4495 0.4595 0.071 Uiso 1 1 calc R . .
C15 C 0.6317(2) 0.2023(4) 0.2984(2) 0.0382(12) Uani 1 1 d . . .
C16 C 0.5841(2) 0.1757(4) 0.2444(2) 0.0441(13) Uani 1 1 d . . .
C17 C 0.5606(2) 0.0859(5) 0.2367(2) 0.0637(16) Uani 1 1 d . . .
H17 H 0.5755 0.0413 0.2645 0.076 Uiso 1 1 calc R . .
C18 C 0.5150(3) 0.0625(5) 0.1876(3) 0.084(2) Uani 1 1 d . . .
H18 H 0.4993 0.0022 0.1825 0.100 Uiso 1 1 calc R . .
C19 C 0.4928(3) 0.1285(6) 0.1464(3) 0.079(2) Uani 1 1 d . . .
H19 H 0.4619 0.1129 0.1137 0.095 Uiso 1 1 calc R . .
C20 C 0.5164(3) 0.2186(6) 0.1538(2) 0.0693(18) Uani 1 1 d . . .
H20 H 0.5014 0.2634 0.1261 0.083 Uiso 1 1 calc R . .
C21 C 0.5623(2) 0.2409(4) 0.2025(2) 0.0553(15) Uani 1 1 d . . .
H21 H 0.5788 0.3007 0.2071 0.066 Uiso 1 1 calc R . .
C22 C 0.7956(2) 0.4537(4) 0.4622(2) 0.0469(13) Uani 1 1 d D . .
C23 C 0.8399(2) 0.4472(4) 0.5213(2) 0.0447(13) Uani 1 1 d D . .
C24 C 0.8489(2) 0.3634(4) 0.5494(2) 0.0524(14) Uani 1 1 d . . .
H24 H 0.8287 0.3104 0.5313 0.063 Uiso 1 1 calc R . .
C25 C 0.8874(3) 0.3562(4) 0.6041(2) 0.0584(15) Uani 1 1 d . . .
H25 H 0.8920 0.2997 0.6231 0.070 Uiso 1 1 calc R . .
C26 C 0.9183(2) 0.4340(5) 0.6294(2) 0.0617(16) Uani 1 1 d . . .
H26 H 0.9446 0.4302 0.6659 0.074 Uiso 1 1 calc R . .
C27 C 0.9109(2) 0.5180(4) 0.6014(2) 0.0598(16) Uani 1 1 d . . .
H27 H 0.9328 0.5702 0.6190 0.072 Uiso 1 1 calc R . .
C28 C 0.8715(2) 0.5250(4) 0.5480(2) 0.0548(14) Uani 1 1 d . . .
H28 H 0.8661 0.5822 0.5296 0.066 Uiso 1 1 calc R . .
C29 C 0.81215(19) -0.1850(3) 0.36267(19) 0.0334(11) Uani 1 1 d . . .
C30 C 0.85607(19) -0.2634(3) 0.37279(18) 0.0336(11) Uani 1 1 d . . .
C31 C 0.9026(2) -0.2560(3) 0.3543(2) 0.0434(12) Uani 1 1 d . . .
H31 H 0.9066 -0.2024 0.3355 0.052 Uiso 1 1 calc R . .
C32 C 0.9438(2) -0.3280(4) 0.3635(2) 0.0559(15) Uani 1 1 d . . .
H32 H 0.9751 -0.3228 0.3506 0.067 Uiso 1 1 calc R . .
C33 C 0.9383(2) -0.4073(3) 0.3917(2) 0.0470(13) Uani 1 1 d . . .
H33 H 0.9660 -0.4554 0.3979 0.056 Uiso 1 1 calc R . .
C34 C 0.8919(2) -0.4155(3) 0.4110(2) 0.0437(12) Uani 1 1 d . . .
H34 H 0.8883 -0.4688 0.4302 0.052 Uiso 1 1 calc R . .
C35 C 0.8504(2) -0.3431(3) 0.40117(19) 0.0390(12) Uani 1 1 d . . .
H35 H 0.8188 -0.3483 0.4137 0.047 Uiso 1 1 calc R . .
C36 C 0.6541(2) -0.1177(3) 0.2767(2) 0.0385(12) Uani 1 1 d . . .
C37 C 0.6004(2) -0.1463(4) 0.2284(2) 0.0477(13) Uani 1 1 d . . .
C38 C 0.5505(2) -0.1786(4) 0.2363(2) 0.0704(18) Uani 1 1 d . . .
H38 H 0.5502 -0.1860 0.2720 0.084 Uiso 1 1 calc R . .
C39 C 0.5011(3) -0.2000(6) 0.1912(3) 0.112(3) Uani 1 1 d U . .
H39 H 0.4667 -0.2190 0.1967 0.135 Uiso 1 1 calc R . .
C40 C 0.5004(3) -0.1942(6) 0.1371(3) 0.107(2) Uani 1 1 d U . .
H40 H 0.4666 -0.2100 0.1070 0.128 Uiso 1 1 calc R . .
C41 C 0.5513(3) -0.1644(5) 0.1299(3) 0.096(2) Uani 1 1 d U . .
H41 H 0.5519 -0.1601 0.0942 0.115 Uiso 1 1 calc R . .
C42 C 0.6014(3) -0.1407(4) 0.1745(2) 0.0710(18) Uani 1 1 d . . .
H42 H 0.6357 -0.1211 0.1690 0.085 Uiso 1 1 calc R . .
C43 C 0.89357(19) 0.1998(3) 0.26707(18) 0.0342(11) Uani 1 1 d . . .
C44 C 0.94074(18) 0.2657(3) 0.26349(17) 0.0297(10) Uani 1 1 d . . .
C45 C 0.9346(2) 0.3601(3) 0.26614(19) 0.0413(12) Uani 1 1 d . . .
H45 H 0.9006 0.3845 0.2702 0.050 Uiso 1 1 calc R . .
C46 C 0.9786(2) 0.4207(3) 0.26281(19) 0.0452(13) Uani 1 1 d . . .
H46 H 0.9729 0.4852 0.2628 0.054 Uiso 1 1 calc R . .
C47 C 1.0300(2) 0.3859(4) 0.25951(18) 0.0427(12) Uani 1 1 d . . .
H47 H 1.0597 0.4264 0.2584 0.051 Uiso 1 1 calc R . .
C48 C 1.0375(2) 0.2921(4) 0.25789(19) 0.0454(13) Uani 1 1 d . . .
H48 H 1.0726 0.2683 0.2558 0.054 Uiso 1 1 calc R . .
C49 C 0.9923(2) 0.2303(3) 0.25932(18) 0.0382(12) Uani 1 1 d . . .
H49 H 0.9972 0.1660 0.2575 0.046 Uiso 1 1 calc R . .
C50 C 0.6764(4) -0.2780(4) 0.4413(3) 0.099(2) Uani 1 1 d DU . .
H50A H 0.7135 -0.3060 0.4421 0.119 Uiso 1 1 calc R . .
H50B H 0.6465 -0.2926 0.4054 0.119 Uiso 1 1 calc R . .
C51 C 0.6593(3) -0.3248(4) 0.4834(3) 0.0772(19) Uani 1 1 d . . .
H51A H 0.6949 -0.3353 0.5158 0.093 Uiso 1 1 calc R . .
H51B H 0.6427 -0.3856 0.4693 0.093 Uiso 1 1 calc R . .
C52 C 0.6141(4) -0.2716(6) 0.5013(3) 0.120(3) Uani 1 1 d U . .
H52A H 0.5745 -0.2823 0.4742 0.144 Uiso 1 1 calc R . .
H52B H 0.6150 -0.2964 0.5365 0.144 Uiso 1 1 calc R . .
C53 C 0.6255(3) -0.1681(4) 0.5071(3) 0.0773(19) Uani 1 1 d . . .
H53A H 0.5895 -0.1370 0.5068 0.093 Uiso 1 1 calc R . .
H53B H 0.6563 -0.1561 0.5429 0.093 Uiso 1 1 calc R . .
C54 C 0.6439(3) -0.1258(5) 0.4636(3) 0.089(2) Uani 1 1 d . . .
H54 H 0.6068 -0.1300 0.4313 0.107 Uiso 1 1 calc R . .
C55 C 0.6557(3) -0.0177(4) 0.4662(3) 0.0741(18) Uani 1 1 d . . .
H55A H 0.6198 0.0165 0.4631 0.089 Uiso 1 1 calc R . .
H55B H 0.6868 -0.0009 0.5009 0.089 Uiso 1 1 calc R . .
C56 C 0.6466(2) 0.5090(4) 0.3213(2) 0.0618(16) Uani 1 1 d . . .
H56A H 0.6402 0.5111 0.3563 0.074 Uiso 1 1 calc R . .
H56B H 0.6153 0.4708 0.2958 0.074 Uiso 1 1 calc R . .
C57 C 0.6429(3) 0.6080(4) 0.2981(3) 0.0724(18) Uani 1 1 d . . .
H57A H 0.6702 0.6483 0.3260 0.087 Uiso 1 1 calc R . .
H57B H 0.6029 0.6321 0.2896 0.087 Uiso 1 1 calc R . .
C58 C 0.6584(3) 0.6103(4) 0.2457(3) 0.0759(19) Uani 1 1 d . . .
H58A H 0.6280 0.5774 0.2160 0.091 Uiso 1 1 calc R . .
H58B H 0.6594 0.6747 0.2341 0.091 Uiso 1 1 calc R . .
C59 C 0.7183(2) 0.5649(3) 0.2565(2) 0.0561(15) Uani 1 1 d . . .
H59A H 0.7492 0.6021 0.2831 0.067 Uiso 1 1 calc R . .
H59B H 0.7262 0.5627 0.2223 0.067 Uiso 1 1 calc R . .
C60 C 0.7197(2) 0.4667(3) 0.2788(2) 0.0433(12) Uani 1 1 d . . .
H60 H 0.6890 0.4302 0.2505 0.052 Uiso 1 1 calc R . .
C61 C 0.7782(2) 0.4166(3) 0.2910(2) 0.0416(12) Uani 1 1 d . . .
H61A H 0.7837 0.4010 0.2567 0.050 Uiso 1 1 calc R . .
H61B H 0.8108 0.4567 0.3127 0.050 Uiso 1 1 calc R . .
C62 C 0.7929(2) -0.0981(3) 0.2092(2) 0.0432(12) Uani 1 1 d . . .
H62A H 0.7582 -0.1362 0.2051 0.052 Uiso 1 1 calc R . .
H62B H 0.8274 -0.1293 0.2354 0.052 Uiso 1 1 calc R . .
C63 C 0.8005(3) -0.0908(4) 0.1533(2) 0.0585(16) Uani 1 1 d . . .
H63A H 0.8011 -0.1533 0.1387 0.070 Uiso 1 1 calc R . .
H63B H 0.8384 -0.0613 0.1584 0.070 Uiso 1 1 calc R . .
C64 C 0.7502(2) -0.0340(4) 0.1113(2) 0.0582(15) Uani 1 1 d . . .
H64A H 0.7585 -0.0255 0.0775 0.070 Uiso 1 1 calc R . .
H64B H 0.7129 -0.0677 0.1020 0.070 Uiso 1 1 calc R . .
C65 C 0.7451(2) 0.0607(4) 0.1357(2) 0.0503(14) Uani 1 1 d . . .
H65A H 0.7808 0.0969 0.1411 0.060 Uiso 1 1 calc R . .
H65B H 0.7115 0.0946 0.1100 0.060 Uiso 1 1 calc R . .
C66 C 0.7366(2) 0.0502(3) 0.19041(19) 0.0389(12) Uani 1 1 d . . .
H66 H 0.6993 0.0160 0.1835 0.047 Uiso 1 1 calc R . .
C67 C 0.7319(2) 0.1417(3) 0.21707(18) 0.0386(12) Uani 1 1 d . . .
H67A H 0.7604 0.1857 0.2123 0.046 Uiso 1 1 calc R . .
H67B H 0.6923 0.1675 0.1990 0.046 Uiso 1 1 calc R . .
C68 C 0.9172(2) 0.3223(3) 0.4135(2) 0.0488(13) Uani 1 1 d . . .
H68A H 0.8893 0.3732 0.4096 0.059 Uiso 1 1 calc R . .
H68B H 0.9341 0.3296 0.3848 0.059 Uiso 1 1 calc R . .
C69 C 0.9666(2) 0.3289(4) 0.4698(2) 0.0551(15) Uani 1 1 d . . .
H69A H 0.9493 0.3305 0.4983 0.066 Uiso 1 1 calc R . .
H69B H 0.9884 0.3868 0.4719 0.066 Uiso 1 1 calc R . .
C70 C 1.0096(2) 0.2463(4) 0.4804(2) 0.0533(14) Uani 1 1 d . . .
H70A H 1.0375 0.2489 0.5184 0.064 Uiso 1 1 calc R . .
H70B H 1.0321 0.2512 0.4560 0.064 Uiso 1 1 calc R . .
C71 C 0.9763(2) 0.1512(3) 0.47035(19) 0.0442(13) Uani 1 1 d . . .
H71A H 0.9594 0.1411 0.4988 0.053 Uiso 1 1 calc R . .
H71B H 1.0042 0.1008 0.4727 0.053 Uiso 1 1 calc R . .
C72 C 0.92638(19) 0.1502(3) 0.41275(19) 0.0368(11) Uani 1 1 d . . .
H72 H 0.9453 0.1567 0.3851 0.044 Uiso 1 1 calc R . .
C73 C 0.88948(19) 0.0628(3) 0.39905(19) 0.0374(12) Uani 1 1 d . . .
H73A H 0.9138 0.0099 0.3967 0.045 Uiso 1 1 calc R . .
H73B H 0.8734 0.0499 0.4278 0.045 Uiso 1 1 calc R . .
N5 N 0.6993(5) 0.0766(8) 0.6325(4) 0.158(4) Uani 0.80 1 d PU . .
C74 C 0.7334(5) 0.1201(7) 0.6230(4) 0.102(3) Uani 0.80 1 d PU . .
C75 C 0.7728(4) 0.1699(7) 0.6036(4) 0.109(3) Uani 0.80 1 d PU . .
H75A H 0.7704 0.1452 0.5683 0.164 Uiso 0.80 1 calc PR . .
H75B H 0.8128 0.1633 0.6297 0.164 Uiso 0.80 1 calc PR . .
H75C H 0.7620 0.2349 0.5997 0.164 Uiso 0.80 1 calc PR . .
N6 N 0.5327(6) 0.0469(13) 0.5936(7) 0.192(7) Uani 0.50 1 d PDU . .
C76 C 0.5149(6) 0.0233(9) 0.6278(6) 0.107(5) Uani 0.50 1 d PDU . .
C77 C 0.4847(7) -0.0277(11) 0.6577(6) 0.122(5) Uani 0.50 1 d PDU . .
H77A H 0.5043 -0.0169 0.6967 0.183 Uiso 0.50 1 calc PR . .
H77B H 0.4855 -0.0934 0.6501 0.183 Uiso 0.50 1 calc PR . .
H77C H 0.4441 -0.0069 0.6463 0.183 Uiso 0.50 1 calc PR . .
O21A O 0.7841(5) 0.8576(8) 0.6204(5) 0.160(4) Uani 0.55 1 d PU . .
O21B O 0.8414(5) 0.9176(8) 0.6934(5) 0.123(4) Uani 0.45 1 d PU . .
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
N1 0.058(3) 0.045(3) 0.080(4) 0.027(2) 0.041(3) 0.015(2)
N2 0.046(3) 0.042(2) 0.041(3) 0.000(2) 0.020(2) 0.010(2)
N3 0.028(2) 0.043(2) 0.041(2) -0.007(2) 0.020(2) -0.0101(19)
N4 0.029(2) 0.048(2) 0.049(3) -0.007(2) 0.018(2) 0.0034(19)
O1 0.0363(19) 0.046(2) 0.040(2) 0.0066(17) 0.0176(16) 0.0060(16)
O2 0.0411(19) 0.046(2) 0.0363(19) 0.0027(16) 0.0194(16) 0.0081(16)
O3 0.053(2) 0.051(2) 0.040(2) 0.0069(17) 0.0279(17) 0.0171(18)
O4 0.062(2) 0.051(2) 0.048(2) 0.0134(18) 0.0370(19) 0.0214(18)
O5 0.0290(18) 0.050(2) 0.044(2) 0.0068(17) 0.0174(16) 0.0102(15)
O6 0.0370(19) 0.044(2) 0.045(2) 0.0104(17) 0.0224(16) 0.0119(17)
O7 0.058(2) 0.050(2) 0.049(2) -0.0059(19) 0.0181(19) 0.0112(18)
O8 0.073(3) 0.050(2) 0.057(2) 0.0054(19) 0.024(2) -0.002(2)
O9 0.0360(18) 0.0298(17) 0.046(2) 0.0025(15) 0.0229(16) 0.0000(14)
O10 0.0344(18) 0.0356(18) 0.054(2) 0.0048(15) 0.0265(17) 0.0032(14)
O11 0.0328(18) 0.0479(19) 0.043(2) 0.0072(16) 0.0215(16) -0.0009(15)
O12 0.0336(18) 0.0458(19) 0.043(2) -0.0060(15) 0.0221(16) -0.0095(15)
O13 0.0350(18) 0.0358(18) 0.055(2) 0.0030(15) 0.0278(17) 0.0006(15)
O14 0.043(2) 0.0330(19) 0.055(2) -0.0051(16) 0.0295(17) -0.0029(15)
O15 0.0396(18) 0.0463(19) 0.0445(19) 0.0114(16) 0.0293(16) 0.0094(16)
O16 0.0389(19) 0.0332(17) 0.054(2) 0.0040(16) 0.0292(17) 0.0081(15)
O17 0.0270(17) 0.0374(17) 0.0345(19) -0.0008(14) 0.0129(15) 0.0003(14)
O18 0.0256(17) 0.0298(17) 0.0389(19) -0.0006(14) 0.0134(15) 0.0010(13)
O19 0.0335(17) 0.0350(17) 0.0378(18) 0.0038(14) 0.0216(15) 0.0035(14)
O20 0.0327(17) 0.0403(18) 0.0379(18) 0.0032(15) 0.0195(15) 0.0073(14)
Fe1 0.0322(4) 0.0389(4) 0.0408(4) 0.0064(3) 0.0205(3) 0.0040(3)
Fe2 0.0365(4) 0.0403(4) 0.0375(4) 0.0055(3) 0.0213(3) 0.0099(3)
Fe3 0.0414(4) 0.0401(4) 0.0414(4) 0.0036(3) 0.0233(4) 0.0114(3)
Fe4 0.0275(3) 0.0344(4) 0.0368(4) 0.0005(3) 0.0179(3) 0.0004(3)
Fe5 0.0306(4) 0.0327(4) 0.0403(4) -0.0011(3) 0.0185(3) 0.0029(3)
C1 0.041(3) 0.047(3) 0.035(3) 0.002(3) 0.024(2) 0.005(3)
C2 0.036(3) 0.055(3) 0.032(3) 0.002(3) 0.021(2) 0.012(3)
C3 0.046(3) 0.057(3) 0.036(3) -0.005(3) 0.016(3) 0.015(3)
C4 0.057(4) 0.065(4) 0.034(3) 0.001(3) 0.010(3) 0.027(3)
C5 0.049(3) 0.081(4) 0.032(3) -0.008(3) 0.011(3) 0.019(3)
C6 0.058(4) 0.068(4) 0.041(3) -0.009(3) 0.014(3) 0.005(3)
C7 0.049(3) 0.055(3) 0.043(3) 0.002(3) 0.020(3) 0.007(3)
C8 0.035(3) 0.062(4) 0.044(3) -0.005(3) 0.017(3) 0.010(3)
C9 0.054(3) 0.050(3) 0.051(3) 0.002(3) 0.034(3) 0.012(3)
C10 0.070(4) 0.054(3) 0.067(4) 0.006(3) 0.040(3) 0.017(3)
C11 0.096(5) 0.063(4) 0.082(5) 0.002(3) 0.070(4) 0.005(4)
C12 0.085(5) 0.083(5) 0.084(5) -0.004(4) 0.064(4) 0.008(4)
C13 0.081(4) 0.067(4) 0.087(5) -0.005(4) 0.057(4) 0.012(3)
C14 0.065(4) 0.059(4) 0.066(4) -0.002(3) 0.038(3) 0.007(3)
C15 0.028(3) 0.055(3) 0.040(3) 0.006(3) 0.023(2) 0.017(3)
C16 0.033(3) 0.065(4) 0.042(3) 0.002(3) 0.023(3) 0.012(3)
C17 0.045(4) 0.091(5) 0.053(4) 0.001(3) 0.014(3) 0.003(3)
C18 0.056(4) 0.113(6) 0.074(5) -0.014(5) 0.014(4) -0.014(4)
C19 0.052(4) 0.139(7) 0.046(4) -0.002(5) 0.017(3) 0.023(5)
C20 0.061(4) 0.109(6) 0.041(4) 0.011(4) 0.022(3) 0.025(4)
C21 0.050(4) 0.082(4) 0.040(3) 0.005(3) 0.024(3) 0.012(3)
C22 0.053(4) 0.047(3) 0.054(4) 0.003(3) 0.036(3) -0.001(3)
C23 0.046(3) 0.052(3) 0.046(3) -0.002(3) 0.027(3) 0.010(3)
C24 0.057(4) 0.057(4) 0.049(4) -0.001(3) 0.025(3) 0.012(3)
C25 0.065(4) 0.063(4) 0.057(4) 0.008(3) 0.034(3) 0.020(3)
C26 0.057(4) 0.083(5) 0.051(4) -0.010(4) 0.026(3) 0.021(4)
C27 0.058(4) 0.072(4) 0.057(4) -0.019(3) 0.029(3) 0.004(3)
C28 0.060(4) 0.060(4) 0.053(4) -0.003(3) 0.030(3) -0.002(3)
C29 0.025(3) 0.037(3) 0.037(3) -0.006(2) 0.010(2) 0.002(2)
C30 0.029(3) 0.036(3) 0.034(3) -0.005(2) 0.009(2) -0.001(2)
C31 0.043(3) 0.042(3) 0.053(3) 0.009(2) 0.026(3) 0.009(2)
C32 0.057(4) 0.051(3) 0.071(4) 0.019(3) 0.038(3) 0.017(3)
C33 0.046(3) 0.039(3) 0.057(3) 0.000(3) 0.019(3) 0.018(2)
C34 0.048(3) 0.034(3) 0.055(3) -0.002(2) 0.026(3) 0.004(2)
C35 0.033(3) 0.037(3) 0.050(3) -0.005(2) 0.019(2) -0.002(2)
C36 0.031(3) 0.042(3) 0.048(3) 0.000(2) 0.021(3) -0.001(2)
C37 0.031(3) 0.066(4) 0.049(3) -0.002(3) 0.019(3) -0.012(3)
C38 0.040(3) 0.117(5) 0.053(4) 0.011(4) 0.015(3) -0.031(3)
C39 0.071(4) 0.177(7) 0.094(5) 0.021(5) 0.037(4) -0.060(4)
C40 0.080(4) 0.151(5) 0.087(5) 0.009(4) 0.026(4) -0.050(4)
C41 0.076(4) 0.152(6) 0.063(4) -0.015(4) 0.031(4) -0.055(4)
C42 0.048(4) 0.114(5) 0.055(4) -0.016(4) 0.022(3) -0.039(3)
C43 0.028(3) 0.042(3) 0.034(3) 0.005(2) 0.013(2) -0.002(2)
C44 0.027(3) 0.036(3) 0.028(3) 0.002(2) 0.013(2) 0.002(2)
C45 0.029(3) 0.045(3) 0.054(3) 0.010(2) 0.020(3) 0.002(2)
C46 0.048(3) 0.037(3) 0.046(3) 0.007(2) 0.011(3) -0.003(3)
C47 0.035(3) 0.057(4) 0.036(3) 0.007(3) 0.013(2) -0.008(3)
C48 0.035(3) 0.065(4) 0.040(3) -0.002(3) 0.018(2) -0.003(3)
C49 0.041(3) 0.039(3) 0.039(3) -0.003(2) 0.020(2) -0.003(2)
C50 0.146(6) 0.084(5) 0.097(5) -0.010(4) 0.079(5) -0.031(4)
C51 0.108(5) 0.062(4) 0.077(4) 0.009(3) 0.052(4) -0.029(4)
C52 0.159(6) 0.118(5) 0.120(5) 0.017(4) 0.094(5) -0.001(5)
C53 0.094(5) 0.077(4) 0.084(5) 0.016(4) 0.061(4) -0.007(4)
C54 0.113(6) 0.092(5) 0.097(5) 0.019(4) 0.080(5) 0.011(4)
C55 0.084(5) 0.079(5) 0.082(5) 0.019(4) 0.058(4) 0.008(4)
C56 0.063(4) 0.067(4) 0.068(4) 0.013(3) 0.039(3) 0.034(3)
C57 0.095(5) 0.053(4) 0.085(5) 0.024(3) 0.052(4) 0.042(3)
C58 0.097(5) 0.069(4) 0.078(5) 0.025(3) 0.050(4) 0.039(4)
C59 0.070(4) 0.052(3) 0.057(4) 0.016(3) 0.035(3) 0.019(3)
C60 0.050(3) 0.040(3) 0.046(3) 0.005(2) 0.025(3) 0.012(2)
C61 0.047(3) 0.034(3) 0.051(3) 0.000(2) 0.026(3) 0.005(2)
C62 0.046(3) 0.043(3) 0.051(3) -0.004(2) 0.031(3) -0.009(2)
C63 0.075(4) 0.059(3) 0.063(4) -0.020(3) 0.051(3) -0.010(3)
C64 0.059(4) 0.071(4) 0.054(4) -0.014(3) 0.033(3) -0.018(3)
C65 0.046(3) 0.064(4) 0.043(3) 0.002(3) 0.020(3) -0.011(3)
C66 0.029(3) 0.052(3) 0.039(3) -0.002(2) 0.017(2) -0.011(2)
C67 0.037(3) 0.046(3) 0.031(3) 0.007(2) 0.011(2) -0.001(2)
C68 0.037(3) 0.039(3) 0.065(4) -0.013(3) 0.014(3) 0.000(2)
C69 0.044(3) 0.050(3) 0.070(4) -0.025(3) 0.020(3) -0.005(3)
C70 0.036(3) 0.073(4) 0.045(3) -0.018(3) 0.007(3) -0.002(3)
C71 0.036(3) 0.058(3) 0.039(3) 0.000(3) 0.013(3) 0.008(3)
C72 0.033(3) 0.038(3) 0.040(3) -0.002(2) 0.014(2) 0.002(2)
C73 0.028(3) 0.043(3) 0.040(3) 0.005(2) 0.010(2) 0.005(2)
N5 0.156(7) 0.181(8) 0.135(7) 0.079(6) 0.051(6) -0.002(6)
C74 0.123(9) 0.095(7) 0.080(7) 0.024(6) 0.027(6) 0.000(6)
C75 0.097(7) 0.113(8) 0.139(9) -0.048(7) 0.068(6) -0.006(6)
N6 0.176(9) 0.209(10) 0.208(10) 0.040(7) 0.091(7) -0.037(7)
C76 0.091(8) 0.098(9) 0.125(9) 0.011(7) 0.031(7) 0.039(7)
C77 0.119(10) 0.129(10) 0.122(10) 0.032(8) 0.049(8) 0.031(8)
O21A 0.147(6) 0.149(6) 0.211(7) 0.055(5) 0.096(6) 0.027(5)
O21B 0.111(6) 0.146(7) 0.147(7) -0.001(5) 0.087(5) 0.021(5)
_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
N1 C50 1.416(5) . ?
N1 C54 1.463(7) . ?
N1 Fe1 2.105(4) . ?
N1 H1N 0.876(10) . ?
N2 C60 1.489(6) . ?
N2 C56 1.477(6) . ?
N2 Fe3 2.168(4) . ?
N2 H2N 0.87(2) . ?
N3 C62 1.484(5) . ?
N3 C66 1.502(6) . ?
N3 Fe4 2.157(4) . ?
N3 H3N 0.840(19) . ?
N4 C68 1.486(6) . ?
N4 C72 1.501(5) . ?
N4 Fe5 2.161(4) . ?
N4 H4N 0.870(19) . ?
O1 C1 1.262(5) . ?
O1 Fe1 2.077(3) . ?
O2 C1 1.271(5) . ?
O2 Fe2 2.095(3) . ?
O3 C8 1.263(6) . ?
O3 Fe2 2.066(3) . ?
O4 C8 1.247(6) . ?
O4 Fe3 2.015(3) . ?
O5 C15 1.269(5) . ?
O5 Fe2 2.059(3) . ?
O6 C15 1.253(5) . ?
O6 Fe3 2.045(3) . ?
O7 C22 1.251(6) . ?
O7 Fe3 1.994(4) . ?
O8 C22 1.240(6) . ?
O9 C29 1.262(5) . ?
O9 Fe4 2.023(3) . ?
O10 C29 1.265(5) . ?
O10 Fe1 2.039(3) . ?
O11 C36 1.269(5) . ?
O11 Fe1 2.032(3) . ?
O12 C36 1.266(5) . ?
O12 Fe4 2.075(3) . ?
O13 C43 1.285(5) . ?
O13 Fe5 2.006(3) . ?
O14 C43 1.237(5) . ?
O15 C55 1.415(6) . ?
O15 Fe1 1.981(3) . ?
O15 Fe2 2.064(3) . ?
O16 C61 1.416(5) . ?
O16 Fe5 1.962(3) . ?
O16 Fe3 1.993(3) . ?
O17 C67 1.432(5) . ?
O17 Fe5 2.012(3) . ?
O17 Fe4 2.039(3) . ?
O18 C73 1.405(5) . ?
O18 Fe4 1.995(3) . ?
O18 Fe5 1.997(3) . ?
O19 Fe4 1.848(3) . ?
O19 Fe1 1.871(3) . ?
O19 Fe2 1.952(3) . ?
O20 Fe2 1.875(3) . ?
O20 Fe3 1.895(3) . ?
O20 Fe5 2.011(3) . ?
Fe1 Fe2 2.9704(9) . ?
C1 C2 1.476(6) . ?
C2 C7 1.396(6) . ?
C2 C3 1.397(6) . ?
C3 C4 1.377(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.394(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.392(7) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.519(6) . ?
C9 C10 1.368(7) . ?
C9 C14 1.396(7) . ?
C10 C11 1.388(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.367(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.407(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.391(7) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.500(7) . ?
C16 C21 1.380(7) . ?
C16 C17 1.386(7) . ?
C17 C18 1.387(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.376(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.391(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.379(7) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.519(6) . ?
C23 C24 1.374(7) . ?
C23 C28 1.382(7) . ?
C24 C25 1.386(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.365(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.378(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.368(7) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C30 1.497(6) . ?
C30 C31 1.370(6) . ?
C30 C35 1.386(6) . ?
C31 C32 1.388(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.379(6) . ?
C32 H32 0.9300 . ?
C33 C34 1.381(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.396(6) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.495(6) . ?
C37 C38 1.369(7) . ?
C37 C42 1.403(7) . ?
C38 C39 1.367(8) . ?
C38 H38 0.9300 . ?
C39 C40 1.393(9) . ?
C39 H39 0.9300 . ?
C40 C41 1.370(8) . ?
C40 H40 0.9300 . ?
C41 C42 1.378(8) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 C44 1.502(6) . ?
C44 C45 1.361(6) . ?
C44 C49 1.378(6) . ?
C45 C46 1.394(6) . ?
C45 H45 0.9300 . ?
C46 C47 1.363(6) . ?
C46 H46 0.9300 . ?
C47 C48 1.354(6) . ?
C47 H47 0.9300 . ?
C48 C49 1.411(6) . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
C50 C51 1.457(7) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 C52 1.529(9) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 C53 1.500(9) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C53 C54 1.478(7) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 C55 1.566(8) . ?
C54 H54 0.9800 . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 C57 1.525(7) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 C58 1.529(7) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 C59 1.511(7) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 C60 1.511(6) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 C61 1.508(6) . ?
C60 H60 0.9800 . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 C63 1.524(6) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C63 C64 1.534(7) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C64 C65 1.515(7) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C65 C66 1.507(6) . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C66 C67 1.500(6) . ?
C66 H66 0.9800 . ?
C67 H67A 0.9700 . ?
C67 H67B 0.9700 . ?
C68 C69 1.513(7) . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C69 C70 1.527(7) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C70 C71 1.549(7) . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
C71 C72 1.540(6) . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C72 C73 1.498(6) . ?
C72 H72 0.9800 . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
N5 C74 1.125(12) . ?
C74 C75 1.413(12) . ?
C75 H75A 0.9600 . ?
C75 H75B 0.9600 . ?
C75 H75C 0.9600 . ?
N6 C76 1.162(4) . ?
C76 C77 1.435(5) . ?
C77 H77A 0.9600 . ?
C77 H77B 0.9600 . ?
C77 H77C 0.9600 . ?
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
C50 N1 C54 116.5(5) . . ?
C50 N1 Fe1 128.9(4) . . ?
C54 N1 Fe1 109.6(3) . . ?
C50 N1 H1N 89.8(16) . . ?
C54 N1 H1N 98(4) . . ?
Fe1 N1 H1N 105(3) . . ?
C60 N2 C56 112.3(4) . . ?
C60 N2 Fe3 107.8(3) . . ?
C56 N2 Fe3 120.8(3) . . ?
C60 N2 H2N 107(4) . . ?
C56 N2 H2N 110(3) . . ?
Fe3 N2 H2N 97(3) . . ?
C62 N3 C66 111.3(4) . . ?
C62 N3 Fe4 119.0(3) . . ?
C66 N3 Fe4 106.2(2) . . ?
C62 N3 H3N 109(3) . . ?
C66 N3 H3N 109(3) . . ?
Fe4 N3 H3N 102(3) . . ?
C68 N4 C72 111.3(3) . . ?
C68 N4 Fe5 121.2(3) . . ?
C72 N4 Fe5 107.1(3) . . ?
C68 N4 H4N 109(3) . . ?
C72 N4 H4N 108(3) . . ?
Fe5 N4 H4N 99(3) . . ?
C1 O1 Fe1 127.7(3) . . ?
C1 O2 Fe2 126.8(3) . . ?
C8 O3 Fe2 128.1(3) . . ?
C8 O4 Fe3 128.6(3) . . ?
C15 O5 Fe2 131.2(3) . . ?
C15 O6 Fe3 125.4(3) . . ?
C22 O7 Fe3 134.3(3) . . ?
C29 O9 Fe4 130.7(3) . . ?
C29 O10 Fe1 129.5(3) . . ?
C36 O11 Fe1 125.0(3) . . ?
C36 O12 Fe4 135.8(3) . . ?
C43 O13 Fe5 137.4(3) . . ?
C55 O15 Fe1 118.2(3) . . ?
C55 O15 Fe2 132.8(3) . . ?
Fe1 O15 Fe2 94.49(12) . . ?
C61 O16 Fe5 141.2(3) . . ?
C61 O16 Fe3 119.5(2) . . ?
Fe5 O16 Fe3 99.16(13) . . ?
C67 O17 Fe5 120.1(2) . . ?
C67 O17 Fe4 117.6(2) . . ?
Fe5 O17 Fe4 97.30(12) . . ?
C73 O18 Fe4 131.2(2) . . ?
C73 O18 Fe5 117.5(2) . . ?
Fe4 O18 Fe5 99.25(12) . . ?
Fe4 O19 Fe1 121.71(14) . . ?
Fe1 O19 Fe2 101.94(13) . . ?
Fe2 O20 Fe3 116.91(14) . . ?
Fe2 O20 Fe5 132.87(15) . . ?
Fe3 O20 Fe5 100.83(13) . . ?
O19 Fe1 O15 81.91(12) . . ?
O19 Fe1 O11 94.20(12) . . ?
O15 Fe1 O11 97.80(12) . . ?
O19 Fe1 O10 100.55(12) . . ?
O15 Fe1 O10 172.88(13) . . ?
O11 Fe1 O10 88.71(12) . . ?
O19 Fe1 O1 91.05(12) . . ?
O15 Fe1 O1 88.83(12) . . ?
O11 Fe1 O1 172.05(12) . . ?
O10 Fe1 O1 84.47(12) . . ?
O19 Fe1 N1 163.06(15) . . ?
O15 Fe1 N1 81.70(14) . . ?
O11 Fe1 N1 92.24(16) . . ?
O10 Fe1 N1 95.23(14) . . ?
O1 Fe1 N1 84.35(15) . . ?
O19 Fe1 Fe2 40.01(8) . . ?
O15 Fe1 Fe2 43.84(8) . . ?
O11 Fe1 Fe2 107.71(9) . . ?
O10 Fe1 Fe2 136.50(8) . . ?
O1 Fe1 Fe2 80.12(9) . . ?
N1 Fe1 Fe2 123.05(12) . . ?
O20 Fe2 O19 95.29(12) . . ?
O20 Fe2 O5 91.83(12) . . ?
O19 Fe2 O5 93.01(12) . . ?
O20 Fe2 O15 172.96(12) . . ?
O19 Fe2 O15 77.91(11) . . ?
O5 Fe2 O15 86.74(12) . . ?
O20 Fe2 O3 98.96(12) . . ?
O19 Fe2 O3 165.27(12) . . ?
O5 Fe2 O3 90.27(12) . . ?
O15 Fe2 O3 87.95(12) . . ?
O20 Fe2 O2 94.05(12) . . ?
O19 Fe2 O2 90.62(12) . . ?
O5 Fe2 O2 172.78(12) . . ?
O15 Fe2 O2 87.92(12) . . ?
O3 Fe2 O2 84.68(12) . . ?
O20 Fe2 Fe1 132.08(9) . . ?
O19 Fe2 Fe1 38.04(8) . . ?
O5 Fe2 Fe1 99.16(9) . . ?
O15 Fe2 Fe1 41.67(8) . . ?
O3 Fe2 Fe1 127.23(9) . . ?
O2 Fe2 Fe1 79.95(9) . . ?
O20 Fe3 O16 80.85(12) . . ?
O20 Fe3 O7 91.20(13) . . ?
O16 Fe3 O7 93.71(13) . . ?
O20 Fe3 O4 104.67(12) . . ?
O16 Fe3 O4 174.44(13) . . ?
O7 Fe3 O4 87.00(14) . . ?
O20 Fe3 O6 92.66(12) . . ?
O16 Fe3 O6 91.71(12) . . ?
O7 Fe3 O6 173.79(13) . . ?
O4 Fe3 O6 87.32(13) . . ?
O20 Fe3 N2 159.21(14) . . ?
O16 Fe3 N2 78.46(13) . . ?
O7 Fe3 N2 92.09(15) . . ?
O4 Fe3 N2 96.01(14) . . ?
O6 Fe3 N2 86.02(14) . . ?
O19 Fe4 O18 93.45(12) . . ?
O19 Fe4 O9 97.86(12) . . ?
O18 Fe4 O9 87.99(11) . . ?
O19 Fe4 O17 96.58(11) . . ?
O18 Fe4 O17 79.30(11) . . ?
O9 Fe4 O17 161.28(12) . . ?
O19 Fe4 O12 89.22(12) . . ?
O18 Fe4 O12 176.70(11) . . ?
O9 Fe4 O12 89.73(12) . . ?
O17 Fe4 O12 102.34(11) . . ?
O19 Fe4 N3 168.90(13) . . ?
O18 Fe4 N3 94.33(12) . . ?
O9 Fe4 N3 90.31(13) . . ?
O17 Fe4 N3 77.15(13) . . ?
O12 Fe4 N3 83.30(12) . . ?
O16 Fe5 O18 175.43(13) . . ?
O16 Fe5 O13 87.47(12) . . ?
O18 Fe5 O13 93.82(11) . . ?
O16 Fe5 O17 104.27(12) . . ?
O18 Fe5 O17 79.90(11) . . ?
O13 Fe5 O17 97.80(12) . . ?
O16 Fe5 O20 78.81(12) . . ?
O18 Fe5 O20 99.46(11) . . ?
O13 Fe5 O20 165.30(12) . . ?
O17 Fe5 O20 90.75(11) . . ?
O16 Fe5 N4 96.40(14) . . ?
O18 Fe5 N4 79.21(13) . . ?
O13 Fe5 N4 91.07(13) . . ?
O17 Fe5 N4 157.78(14) . . ?
O20 Fe5 N4 85.30(13) . . ?
O1 C1 O2 125.2(4) . . ?
O1 C1 C2 116.9(4) . . ?
O2 C1 C2 117.9(5) . . ?
C7 C2 C3 119.1(4) . . ?
C7 C2 C1 120.8(5) . . ?
C3 C2 C1 120.1(5) . . ?
C4 C3 C2 120.9(5) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 119.9(5) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.6(5) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 119.9(5) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C2 C7 C6 119.7(5) . . ?
C2 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
O4 C8 O3 126.3(4) . . ?
O4 C8 C9 116.9(5) . . ?
O3 C8 C9 116.8(5) . . ?
C10 C9 C14 120.2(5) . . ?
C10 C9 C8 121.1(5) . . ?
C14 C9 C8 118.8(5) . . ?
C9 C10 C11 120.3(5) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C12 C11 C10 120.2(5) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 120.5(5) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C12 C13 C14 118.8(6) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C9 C14 C13 120.0(5) . . ?
C9 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
O6 C15 O5 125.9(5) . . ?
O6 C15 C16 117.9(5) . . ?
O5 C15 C16 116.2(5) . . ?
C21 C16 C17 119.5(5) . . ?
C21 C16 C15 120.4(5) . . ?
C17 C16 C15 120.1(5) . . ?
C16 C17 C18 120.0(6) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 120.1(7) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 120.1(6) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C19 C20 C21 119.4(6) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C16 C21 C20 120.9(6) . . ?
C16 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
O8 C22 O7 126.5(5) . . ?
O8 C22 C23 119.0(5) . . ?
O7 C22 C23 114.5(5) . . ?
C24 C23 C28 118.8(5) . . ?
C24 C23 C22 120.3(5) . . ?
C28 C23 C22 120.9(5) . . ?
C23 C24 C25 121.5(5) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C26 C25 C24 118.5(5) . . ?
C26 C25 H25 120.8 . . ?
C24 C25 H25 120.8 . . ?
C25 C26 C27 120.8(6) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
C28 C27 C26 120.2(6) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C23 120.1(5) . . ?
C27 C28 H28 119.9 . . ?
C23 C28 H28 119.9 . . ?
O9 C29 O10 125.5(4) . . ?
O9 C29 C30 116.8(4) . . ?
O10 C29 C30 117.7(4) . . ?
C31 C30 C35 119.7(4) . . ?
C31 C30 C29 119.7(4) . . ?
C35 C30 C29 120.5(4) . . ?
C30 C31 C32 120.5(4) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C33 119.9(5) . . ?
C31 C32 H32 120.1 . . ?
C33 C32 H32 120.1 . . ?
C34 C33 C32 120.3(4) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 119.3(4) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C30 C35 C34 120.2(4) . . ?
C30 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
O11 C36 O12 125.3(4) . . ?
O11 C36 C37 117.4(4) . . ?
O12 C36 C37 117.3(4) . . ?
C38 C37 C42 119.9(5) . . ?
C38 C37 C36 120.5(5) . . ?
C42 C37 C36 119.6(4) . . ?
C37 C38 C39 119.1(6) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
C38 C39 C40 122.3(6) . . ?
C38 C39 H39 118.8 . . ?
C40 C39 H39 118.8 . . ?
C41 C40 C39 117.9(7) . . ?
C41 C40 H40 121.1 . . ?
C39 C40 H40 121.1 . . ?
C40 C41 C42 121.1(6) . . ?
C40 C41 H41 119.4 . . ?
C42 C41 H41 119.4 . . ?
C41 C42 C37 119.6(5) . . ?
C41 C42 H42 120.2 . . ?
C37 C42 H42 120.2 . . ?
O14 C43 O13 125.8(4) . . ?
O14 C43 C44 119.9(4) . . ?
O13 C43 C44 114.3(4) . . ?
C45 C44 C49 118.9(4) . . ?
C45 C44 C43 121.2(4) . . ?
C49 C44 C43 119.8(4) . . ?
C44 C45 C46 120.9(4) . . ?
C44 C45 H45 119.6 . . ?
C46 C45 H45 119.6 . . ?
C47 C46 C45 120.2(5) . . ?
C47 C46 H46 119.9 . . ?
C45 C46 H46 119.9 . . ?
C48 C47 C46 119.8(5) . . ?
C48 C47 H47 120.1 . . ?
C46 C47 H47 120.1 . . ?
C47 C48 C49 120.2(5) . . ?
C47 C48 H48 119.9 . . ?
C49 C48 H48 119.9 . . ?
C44 C49 C48 119.8(4) . . ?
C44 C49 H49 120.1 . . ?
C48 C49 H49 120.1 . . ?
N1 C50 C51 119.0(5) . . ?
N1 C50 H50A 107.6 . . ?
C51 C50 H50A 107.6 . . ?
N1 C50 H50B 107.6 . . ?
C51 C50 H50B 107.6 . . ?
H50A C50 H50B 107.0 . . ?
C50 C51 C52 115.0(6) . . ?
C50 C51 H51A 108.5 . . ?
C52 C51 H51A 108.5 . . ?
C50 C51 H51B 108.5 . . ?
C52 C51 H51B 108.5 . . ?
H51A C51 H51B 107.5 . . ?
C53 C52 C51 113.3(6) . . ?
C53 C52 H52A 108.9 . . ?
C51 C52 H52A 108.9 . . ?
C53 C52 H52B 108.9 . . ?
C51 C52 H52B 108.9 . . ?
H52A C52 H52B 107.7 . . ?
C54 C53 C52 114.8(6) . . ?
C54 C53 H53A 108.6 . . ?
C52 C53 H53A 108.6 . . ?
C54 C53 H53B 108.6 . . ?
C52 C53 H53B 108.6 . . ?
H53A C53 H53B 107.5 . . ?
N1 C54 C53 117.8(5) . . ?
N1 C54 C55 113.6(5) . . ?
C53 C54 C55 118.0(5) . . ?
N1 C54 H54 101.0 . . ?
C53 C54 H54 101.0 . . ?
C55 C54 H54 101.0 . . ?
O15 C55 C54 106.3(5) . . ?
O15 C55 H55A 110.5 . . ?
C54 C55 H55A 110.5 . . ?
O15 C55 H55B 110.5 . . ?
C54 C55 H55B 110.5 . . ?
H55A C55 H55B 108.7 . . ?
N2 C56 C57 111.3(4) . . ?
N2 C56 H56A 109.4 . . ?
C57 C56 H56A 109.4 . . ?
N2 C56 H56B 109.4 . . ?
C57 C56 H56B 109.4 . . ?
H56A C56 H56B 108.0 . . ?
C56 C57 C58 111.8(4) . . ?
C56 C57 H57A 109.3 . . ?
C58 C57 H57A 109.3 . . ?
C56 C57 H57B 109.3 . . ?
C58 C57 H57B 109.3 . . ?
H57A C57 H57B 107.9 . . ?
C59 C58 C57 110.3(5) . . ?
C59 C58 H58A 109.6 . . ?
C57 C58 H58A 109.6 . . ?
C59 C58 H58B 109.6 . . ?
C57 C58 H58B 109.6 . . ?
H58A C58 H58B 108.1 . . ?
C58 C59 C60 110.9(4) . . ?
C58 C59 H59A 109.5 . . ?
C60 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
C60 C59 H59B 109.5 . . ?
H59A C59 H59B 108.0 . . ?
N2 C60 C61 108.2(4) . . ?
N2 C60 C59 111.5(4) . . ?
C61 C60 C59 114.2(4) . . ?
N2 C60 H60 107.5 . . ?
C61 C60 H60 107.5 . . ?
C59 C60 H60 107.5 . . ?
O16 C61 C60 108.5(4) . . ?
O16 C61 H61A 110.0 . . ?
C60 C61 H61A 110.0 . . ?
O16 C61 H61B 110.0 . . ?
C60 C61 H61B 110.0 . . ?
H61A C61 H61B 108.4 . . ?
N3 C62 C63 112.5(4) . . ?
N3 C62 H62A 109.1 . . ?
C63 C62 H62A 109.1 . . ?
N3 C62 H62B 109.1 . . ?
C63 C62 H62B 109.1 . . ?
H62A C62 H62B 107.8 . . ?
C62 C63 C64 111.9(4) . . ?
C62 C63 H63A 109.2 . . ?
C64 C63 H63A 109.2 . . ?
C62 C63 H63B 109.2 . . ?
C64 C63 H63B 109.2 . . ?
H63A C63 H63B 107.9 . . ?
C65 C64 C63 109.8(4) . . ?
C65 C64 H64A 109.7 . . ?
C63 C64 H64A 109.7 . . ?
C65 C64 H64B 109.7 . . ?
C63 C64 H64B 109.7 . . ?
H64A C64 H64B 108.2 . . ?
C66 C65 C64 111.1(4) . . ?
C66 C65 H65A 109.4 . . ?
C64 C65 H65A 109.4 . . ?
C66 C65 H65B 109.4 . . ?
C64 C65 H65B 109.4 . . ?
H65A C65 H65B 108.0 . . ?
C67 C66 N3 107.6(4) . . ?
C67 C66 C65 113.7(4) . . ?
N3 C66 C65 112.5(4) . . ?
C67 C66 H66 107.6 . . ?
N3 C66 H66 107.6 . . ?
C65 C66 H66 107.6 . . ?
O17 C67 C66 111.2(3) . . ?
O17 C67 H67A 109.4 . . ?
C66 C67 H67A 109.4 . . ?
O17 C67 H67B 109.4 . . ?
C66 C67 H67B 109.4 . . ?
H67A C67 H67B 108.0 . . ?
N4 C68 C69 112.4(4) . . ?
N4 C68 H68A 109.1 . . ?
C69 C68 H68A 109.1 . . ?
N4 C68 H68B 109.1 . . ?
C69 C68 H68B 109.1 . . ?
H68A C68 H68B 107.9 . . ?
C68 C69 C70 111.8(4) . . ?
C68 C69 H69A 109.3 . . ?
C70 C69 H69A 109.3 . . ?
C68 C69 H69B 109.3 . . ?
C70 C69 H69B 109.3 . . ?
H69A C69 H69B 107.9 . . ?
C69 C70 C71 111.8(4) . . ?
C69 C70 H70A 109.3 . . ?
C71 C70 H70A 109.3 . . ?
C69 C70 H70B 109.3 . . ?
C71 C70 H70B 109.3 . . ?
H70A C70 H70B 107.9 . . ?
C70 C71 C72 110.2(4) . . ?
C70 C71 H71A 109.6 . . ?
C72 C71 H71A 109.6 . . ?
C70 C71 H71B 109.6 . . ?
C72 C71 H71B 109.6 . . ?
H71A C71 H71B 108.1 . . ?
N4 C72 C73 107.7(4) . . ?
N4 C72 C71 111.7(4) . . ?
C73 C72 C71 115.2(4) . . ?
N4 C72 H72 107.3 . . ?
C73 C72 H72 107.3 . . ?
C71 C72 H72 107.3 . . ?
O18 C73 C72 108.0(4) . . ?
O18 C73 H73A 110.1 . . ?
C72 C73 H73A 110.1 . . ?
O18 C73 H73B 110.1 . . ?
C72 C73 H73B 110.1 . . ?
H73A C73 H73B 108.4 . . ?
N5 C74 C75 172.1(13) . . ?
C74 C75 H75A 109.5 . . ?
C74 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C74 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
N6 C76 C77 162.5(15) . . ?
C76 C77 H77A 109.5 . . ?
C76 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C76 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 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
Fe4 O19 Fe1 O15 -158.92(19) . . . . ?
Fe2 O19 Fe1 O15 15.46(13) . . . . ?
Fe4 O19 Fe1 O11 -61.62(18) . . . . ?
Fe2 O19 Fe1 O11 112.76(13) . . . . ?
Fe4 O19 Fe1 O10 27.85(19) . . . . ?
Fe2 O19 Fe1 O10 -157.77(12) . . . . ?
Fe4 O19 Fe1 O1 112.42(18) . . . . ?
Fe2 O19 Fe1 O1 -73.21(13) . . . . ?
Fe4 O19 Fe1 N1 -173.7(5) . . . . ?
Fe2 O19 Fe1 N1 0.7(6) . . . . ?
Fe4 O19 Fe1 Fe2 -174.4(3) . . . . ?
C55 O15 Fe1 O19 -158.9(4) . . . . ?
Fe2 O15 Fe1 O19 -14.33(12) . . . . ?
C55 O15 Fe1 O11 107.9(4) . . . . ?
Fe2 O15 Fe1 O11 -107.49(12) . . . . ?
C55 O15 Fe1 O1 -67.7(4) . . . . ?
Fe2 O15 Fe1 O1 76.91(13) . . . . ?
C55 O15 Fe1 N1 16.8(4) . . . . ?
Fe2 O15 Fe1 N1 161.37(17) . . . . ?
C55 O15 Fe1 Fe2 -144.6(4) . . . . ?
C36 O11 Fe1 O19 32.9(4) . . . . ?
C36 O11 Fe1 O15 115.3(3) . . . . ?
C36 O11 Fe1 O10 -67.6(3) . . . . ?
C36 O11 Fe1 N1 -162.8(4) . . . . ?
C36 O11 Fe1 Fe2 71.3(3) . . . . ?
C29 O10 Fe1 O19 6.0(4) . . . . ?
C29 O10 Fe1 O11 100.1(4) . . . . ?
C29 O10 Fe1 O1 -84.0(4) . . . . ?
C29 O10 Fe1 N1 -167.8(4) . . . . ?
C29 O10 Fe1 Fe2 -14.7(4) . . . . ?
C1 O1 Fe1 O19 36.2(3) . . . . ?
C1 O1 Fe1 O15 -45.7(3) . . . . ?
C1 O1 Fe1 O10 136.7(3) . . . . ?
C1 O1 Fe1 N1 -127.5(4) . . . . ?
C1 O1 Fe1 Fe2 -2.5(3) . . . . ?
C50 N1 Fe1 O19 173.3(5) . . . . ?
C54 N1 Fe1 O19 19.6(8) . . . . ?
C50 N1 Fe1 O15 158.5(6) . . . . ?
C54 N1 Fe1 O15 4.9(4) . . . . ?
C50 N1 Fe1 O11 60.9(6) . . . . ?
C54 N1 Fe1 O11 -92.7(4) . . . . ?
C50 N1 Fe1 O10 -28.0(6) . . . . ?
C54 N1 Fe1 O10 178.4(4) . . . . ?
C50 N1 Fe1 O1 -111.9(6) . . . . ?
C54 N1 Fe1 O1 94.5(4) . . . . ?
C50 N1 Fe1 Fe2 173.8(5) . . . . ?
C54 N1 Fe1 Fe2 20.2(5) . . . . ?
Fe3 O20 Fe2 O19 144.50(16) . . . . ?
Fe5 O20 Fe2 O19 5.2(2) . . . . ?
Fe3 O20 Fe2 O5 51.30(17) . . . . ?
Fe5 O20 Fe2 O5 -88.0(2) . . . . ?
Fe3 O20 Fe2 O3 -39.26(18) . . . . ?
Fe5 O20 Fe2 O3 -178.59(19) . . . . ?
Fe3 O20 Fe2 O2 -124.51(16) . . . . ?
Fe5 O20 Fe2 O2 96.2(2) . . . . ?
Fe3 O20 Fe2 Fe1 155.39(8) . . . . ?
Fe5 O20 Fe2 Fe1 16.1(3) . . . . ?
Fe4 O19 Fe2 O20 -20.0(2) . . . . ?
Fe1 O19 Fe2 O20 166.85(13) . . . . ?
Fe4 O19 Fe2 O5 72.1(2) . . . . ?
Fe1 O19 Fe2 O5 -101.03(14) . . . . ?
Fe4 O19 Fe2 O15 158.1(2) . . . . ?
Fe1 O19 Fe2 O15 -15.02(12) . . . . ?
Fe4 O19 Fe2 O3 174.7(4) . . . . ?
Fe1 O19 Fe2 O3 1.6(6) . . . . ?
Fe4 O19 Fe2 O2 -114.2(2) . . . . ?
Fe1 O19 Fe2 O2 72.73(14) . . . . ?
Fe4 O19 Fe2 Fe1 173.1(3) . . . . ?
C15 O5 Fe2 O20 -0.4(4) . . . . ?
C15 O5 Fe2 O19 -95.8(4) . . . . ?
C15 O5 Fe2 O15 -173.5(4) . . . . ?
C15 O5 Fe2 O3 98.6(4) . . . . ?
C15 O5 Fe2 Fe1 -133.5(4) . . . . ?
C55 O15 Fe2 O19 149.8(4) . . . . ?
Fe1 O15 Fe2 O19 13.89(12) . . . . ?
C55 O15 Fe2 O5 -116.4(4) . . . . ?
Fe1 O15 Fe2 O5 107.68(13) . . . . ?
C55 O15 Fe2 O3 -26.0(4) . . . . ?
Fe1 O15 Fe2 O3 -161.93(13) . . . . ?
C55 O15 Fe2 O2 58.7(4) . . . . ?
Fe1 O15 Fe2 O2 -77.18(13) . . . . ?
C55 O15 Fe2 Fe1 135.9(5) . . . . ?
C8 O3 Fe2 O20 41.5(4) . . . . ?
C8 O3 Fe2 O19 -153.4(5) . . . . ?
C8 O3 Fe2 O5 -50.4(4) . . . . ?
C8 O3 Fe2 O15 -137.2(4) . . . . ?
C8 O3 Fe2 O2 134.7(4) . . . . ?
C8 O3 Fe2 Fe1 -152.2(4) . . . . ?
C1 O2 Fe2 O20 -128.4(3) . . . . ?
C1 O2 Fe2 O19 -33.1(3) . . . . ?
C1 O2 Fe2 O15 44.8(3) . . . . ?
C1 O2 Fe2 O3 132.9(3) . . . . ?
C1 O2 Fe2 Fe1 3.6(3) . . . . ?
O19 Fe1 Fe2 O20 -17.77(18) . . . . ?
O15 Fe1 Fe2 O20 -175.38(18) . . . . ?
O11 Fe1 Fe2 O20 -92.66(15) . . . . ?
O10 Fe1 Fe2 O20 14.93(18) . . . . ?
O1 Fe1 Fe2 O20 85.91(14) . . . . ?
N1 Fe1 Fe2 O20 162.47(19) . . . . ?
O15 Fe1 Fe2 O19 -157.60(19) . . . . ?
O11 Fe1 Fe2 O19 -74.89(16) . . . . ?
O10 Fe1 Fe2 O19 32.70(18) . . . . ?
O1 Fe1 Fe2 O19 103.69(16) . . . . ?
N1 Fe1 Fe2 O19 -179.8(2) . . . . ?
O19 Fe1 Fe2 O5 83.13(16) . . . . ?
O15 Fe1 Fe2 O5 -74.47(15) . . . . ?
O11 Fe1 Fe2 O5 8.24(12) . . . . ?
O10 Fe1 Fe2 O5 115.83(15) . . . . ?
O1 Fe1 Fe2 O5 -173.18(12) . . . . ?
N1 Fe1 Fe2 O5 -96.63(17) . . . . ?
O19 Fe1 Fe2 O15 157.60(19) . . . . ?
O11 Fe1 Fe2 O15 82.71(15) . . . . ?
O10 Fe1 Fe2 O15 -169.70(18) . . . . ?
O1 Fe1 Fe2 O15 -98.71(15) . . . . ?
N1 Fe1 Fe2 O15 -22.2(2) . . . . ?
O19 Fe1 Fe2 O3 -179.49(18) . . . . ?
O15 Fe1 Fe2 O3 22.91(17) . . . . ?
O11 Fe1 Fe2 O3 105.62(15) . . . . ?
O10 Fe1 Fe2 O3 -146.79(17) . . . . ?
O1 Fe1 Fe2 O3 -75.80(14) . . . . ?
N1 Fe1 Fe2 O3 0.75(19) . . . . ?
O19 Fe1 Fe2 O2 -104.13(16) . . . . ?
O15 Fe1 Fe2 O2 98.26(15) . . . . ?
O11 Fe1 Fe2 O2 -179.02(12) . . . . ?
O10 Fe1 Fe2 O2 -71.43(15) . . . . ?
O1 Fe1 Fe2 O2 -0.45(11) . . . . ?
N1 Fe1 Fe2 O2 76.11(17) . . . . ?
Fe2 O20 Fe3 O16 -155.52(18) . . . . ?
Fe5 O20 Fe3 O16 -4.61(12) . . . . ?
Fe2 O20 Fe3 O7 110.92(17) . . . . ?
Fe5 O20 Fe3 O7 -98.17(14) . . . . ?
Fe2 O20 Fe3 O4 23.7(2) . . . . ?
Fe5 O20 Fe3 O4 174.62(13) . . . . ?
Fe2 O20 Fe3 O6 -64.21(17) . . . . ?
Fe5 O20 Fe3 O6 86.70(13) . . . . ?
Fe2 O20 Fe3 N2 -150.0(3) . . . . ?
Fe5 O20 Fe3 N2 0.9(5) . . . . ?
C61 O16 Fe3 O20 -179.2(3) . . . . ?
Fe5 O16 Fe3 O20 4.70(13) . . . . ?
C61 O16 Fe3 O7 -88.6(3) . . . . ?
Fe5 O16 Fe3 O7 95.32(14) . . . . ?
C61 O16 Fe3 O6 88.4(3) . . . . ?
Fe5 O16 Fe3 O6 -87.72(14) . . . . ?
C61 O16 Fe3 N2 2.8(3) . . . . ?
Fe5 O16 Fe3 N2 -173.30(16) . . . . ?
C22 O7 Fe3 O20 -163.6(4) . . . . ?
C22 O7 Fe3 O16 115.5(4) . . . . ?
C22 O7 Fe3 O4 -59.0(5) . . . . ?
C22 O7 Fe3 N2 36.9(5) . . . . ?
C8 O4 Fe3 O20 10.3(5) . . . . ?
C8 O4 Fe3 O7 -80.2(4) . . . . ?
C8 O4 Fe3 O6 102.3(4) . . . . ?
C8 O4 Fe3 N2 -172.0(4) . . . . ?
C15 O6 Fe3 O20 33.9(3) . . . . ?
C15 O6 Fe3 O16 114.8(3) . . . . ?
C15 O6 Fe3 O4 -70.7(3) . . . . ?
C15 O6 Fe3 N2 -166.9(3) . . . . ?
C60 N2 Fe3 O20 16.4(6) . . . . ?
C56 N2 Fe3 O20 147.3(4) . . . . ?
C60 N2 Fe3 O16 22.0(3) . . . . ?
C56 N2 Fe3 O16 152.9(4) . . . . ?
C60 N2 Fe3 O7 115.3(3) . . . . ?
C56 N2 Fe3 O7 -113.7(4) . . . . ?
C60 N2 Fe3 O4 -157.5(3) . . . . ?
C56 N2 Fe3 O4 -26.6(4) . . . . ?
C60 N2 Fe3 O6 -70.6(3) . . . . ?
C56 N2 Fe3 O6 60.3(4) . . . . ?
Fe1 O19 Fe4 O18 -128.31(17) . . . . ?
Fe2 O19 Fe4 O18 59.6(2) . . . . ?
Fe1 O19 Fe4 O9 -39.87(19) . . . . ?
Fe2 O19 Fe4 O9 148.1(2) . . . . ?
Fe1 O19 Fe4 O17 152.08(16) . . . . ?
Fe2 O19 Fe4 O17 -20.0(2) . . . . ?
Fe1 O19 Fe4 O12 49.75(18) . . . . ?
Fe2 O19 Fe4 O12 -122.3(2) . . . . ?
Fe1 O19 Fe4 N3 97.2(7) . . . . ?
Fe2 O19 Fe4 N3 -74.9(7) . . . . ?
C73 O18 Fe4 O19 59.5(3) . . . . ?
Fe5 O18 Fe4 O19 -80.38(13) . . . . ?
C73 O18 Fe4 O9 -38.3(3) . . . . ?
Fe5 O18 Fe4 O9 -178.14(13) . . . . ?
C73 O18 Fe4 O17 155.5(3) . . . . ?
Fe5 O18 Fe4 O17 15.67(11) . . . . ?
C73 O18 Fe4 N3 -128.5(3) . . . . ?
Fe5 O18 Fe4 N3 91.70(14) . . . . ?
C29 O9 Fe4 O19 32.8(4) . . . . ?
C29 O9 Fe4 O18 126.0(4) . . . . ?
C29 O9 Fe4 O17 172.9(4) . . . . ?
C29 O9 Fe4 O12 -56.4(4) . . . . ?
C29 O9 Fe4 N3 -139.7(4) . . . . ?
C67 O17 Fe4 O19 -153.7(3) . . . . ?
Fe5 O17 Fe4 O19 76.81(13) . . . . ?
C67 O17 Fe4 O18 114.0(3) . . . . ?
Fe5 O17 Fe4 O18 -15.48(11) . . . . ?
C67 O17 Fe4 O9 66.0(5) . . . . ?
Fe5 O17 Fe4 O9 -63.5(4) . . . . ?
C67 O17 Fe4 O12 -63.0(3) . . . . ?
Fe5 O17 Fe4 O12 167.45(11) . . . . ?
C67 O17 Fe4 N3 17.0(3) . . . . ?
Fe5 O17 Fe4 N3 -112.49(14) . . . . ?
C36 O12 Fe4 O19 -5.8(4) . . . . ?
C36 O12 Fe4 O9 92.1(4) . . . . ?
C36 O12 Fe4 O17 -102.3(4) . . . . ?
C36 O12 Fe4 N3 -177.6(4) . . . . ?
C62 N3 Fe4 O19 -105.4(7) . . . . ?
C66 N3 Fe4 O19 21.1(8) . . . . ?
C62 N3 Fe4 O18 120.2(3) . . . . ?
C66 N3 Fe4 O18 -113.3(3) . . . . ?
C62 N3 Fe4 O9 32.2(3) . . . . ?
C66 N3 Fe4 O9 158.7(3) . . . . ?
C62 N3 Fe4 O17 -161.8(3) . . . . ?
C66 N3 Fe4 O17 -35.4(3) . . . . ?
C62 N3 Fe4 O12 -57.5(3) . . . . ?
C66 N3 Fe4 O12 69.0(3) . . . . ?
C61 O16 Fe5 O13 6.3(5) . . . . ?
Fe3 O16 Fe5 O13 -179.15(14) . . . . ?
C61 O16 Fe5 O17 -91.1(5) . . . . ?
Fe3 O16 Fe5 O17 83.44(14) . . . . ?
C61 O16 Fe5 O20 -179.0(5) . . . . ?
Fe3 O16 Fe5 O20 -4.46(12) . . . . ?
C61 O16 Fe5 N4 97.1(5) . . . . ?
Fe3 O16 Fe5 N4 -88.36(15) . . . . ?
C73 O18 Fe5 O13 100.0(3) . . . . ?
Fe4 O18 Fe5 O13 -113.12(13) . . . . ?
C73 O18 Fe5 O17 -162.7(3) . . . . ?
Fe4 O18 Fe5 O17 -15.86(12) . . . . ?
C73 O18 Fe5 O20 -73.6(3) . . . . ?
Fe4 O18 Fe5 O20 73.21(13) . . . . ?
C73 O18 Fe5 N4 9.7(3) . . . . ?
Fe4 O18 Fe5 N4 156.52(15) . . . . ?
C43 O13 Fe5 O16 173.8(4) . . . . ?
C43 O13 Fe5 O18 -1.8(4) . . . . ?
C43 O13 Fe5 O17 -82.1(4) . . . . ?
C43 O13 Fe5 O20 152.8(5) . . . . ?
C43 O13 Fe5 N4 77.4(4) . . . . ?
C67 O17 Fe5 O16 69.5(3) . . . . ?
Fe4 O17 Fe5 O16 -162.69(11) . . . . ?
C67 O17 Fe5 O18 -112.4(3) . . . . ?
Fe4 O17 Fe5 O18 15.43(11) . . . . ?
C67 O17 Fe5 O13 -19.9(3) . . . . ?
Fe4 O17 Fe5 O13 107.95(12) . . . . ?
C67 O17 Fe5 O20 148.2(3) . . . . ?
Fe4 O17 Fe5 O20 -84.05(12) . . . . ?
C67 O17 Fe5 N4 -132.5(4) . . . . ?
Fe4 O17 Fe5 N4 -4.7(4) . . . . ?
Fe2 O20 Fe5 O16 148.4(2) . . . . ?
Fe3 O20 Fe5 O16 4.71(13) . . . . ?
Fe2 O20 Fe5 O18 -35.9(2) . . . . ?
Fe3 O20 Fe5 O18 -179.58(12) . . . . ?
Fe2 O20 Fe5 O13 169.8(4) . . . . ?
Fe3 O20 Fe5 O13 26.1(5) . . . . ?
Fe2 O20 Fe5 O17 44.0(2) . . . . ?
Fe3 O20 Fe5 O17 -99.69(13) . . . . ?
Fe2 O20 Fe5 N4 -114.1(2) . . . . ?
Fe3 O20 Fe5 N4 102.20(15) . . . . ?
C68 N4 Fe5 O16 -34.1(3) . . . . ?
C72 N4 Fe5 O16 -163.3(3) . . . . ?
C68 N4 Fe5 O18 147.1(3) . . . . ?
C72 N4 Fe5 O18 18.0(3) . . . . ?
C68 N4 Fe5 O13 53.4(3) . . . . ?
C72 N4 Fe5 O13 -75.7(3) . . . . ?
C68 N4 Fe5 O17 167.3(3) . . . . ?
C72 N4 Fe5 O17 38.1(5) . . . . ?
C68 N4 Fe5 O20 -112.3(3) . . . . ?
C72 N4 Fe5 O20 118.5(3) . . . . ?
Fe1 O1 C1 O2 6.2(6) . . . . ?
Fe1 O1 C1 C2 -173.3(3) . . . . ?
Fe2 O2 C1 O1 -6.9(6) . . . . ?
Fe2 O2 C1 C2 172.7(3) . . . . ?
O1 C1 C2 C7 172.2(4) . . . . ?
O2 C1 C2 C7 -7.4(6) . . . . ?
O1 C1 C2 C3 -6.7(6) . . . . ?
O2 C1 C2 C3 173.7(4) . . . . ?
C7 C2 C3 C4 0.7(7) . . . . ?
C1 C2 C3 C4 179.6(4) . . . . ?
C2 C3 C4 C5 -1.4(7) . . . . ?
C3 C4 C5 C6 1.0(8) . . . . ?
C4 C5 C6 C7 0.2(8) . . . . ?
C3 C2 C7 C6 0.5(7) . . . . ?
C1 C2 C7 C6 -178.5(4) . . . . ?
C5 C6 C7 C2 -0.9(7) . . . . ?
Fe3 O4 C8 O3 -16.2(8) . . . . ?
Fe3 O4 C8 C9 162.7(3) . . . . ?
Fe2 O3 C8 O4 -13.8(8) . . . . ?
Fe2 O3 C8 C9 167.3(3) . . . . ?
O4 C8 C9 C10 170.1(5) . . . . ?
O3 C8 C9 C10 -10.8(7) . . . . ?
O4 C8 C9 C14 -9.9(7) . . . . ?
O3 C8 C9 C14 169.1(5) . . . . ?
C14 C9 C10 C11 1.6(9) . . . . ?
C8 C9 C10 C11 -178.5(5) . . . . ?
C9 C10 C11 C12 -1.2(9) . . . . ?
C10 C11 C12 C13 -0.5(10) . . . . ?
C11 C12 C13 C14 1.8(10) . . . . ?
C10 C9 C14 C13 -0.2(8) . . . . ?
C8 C9 C14 C13 179.9(5) . . . . ?
C12 C13 C14 C9 -1.5(9) . . . . ?
Fe3 O6 C15 O5 10.1(6) . . . . ?
Fe3 O6 C15 C16 -173.0(3) . . . . ?
Fe2 O5 C15 O6 -31.8(6) . . . . ?
Fe2 O5 C15 C16 151.2(3) . . . . ?
O6 C15 C16 C21 -8.1(6) . . . . ?
O5 C15 C16 C21 169.1(4) . . . . ?
O6 C15 C16 C17 173.6(4) . . . . ?
O5 C15 C16 C17 -9.3(6) . . . . ?
C21 C16 C17 C18 -1.0(8) . . . . ?
C15 C16 C17 C18 177.4(5) . . . . ?
C16 C17 C18 C19 -0.2(9) . . . . ?
C17 C18 C19 C20 0.6(9) . . . . ?
C18 C19 C20 C21 0.2(9) . . . . ?
C17 C16 C21 C20 1.8(7) . . . . ?
C15 C16 C21 C20 -176.6(4) . . . . ?
C19 C20 C21 C16 -1.4(8) . . . . ?
Fe3 O7 C22 O8 -23.8(8) . . . . ?
Fe3 O7 C22 C23 157.5(3) . . . . ?
O8 C22 C23 C24 150.0(5) . . . . ?
O7 C22 C23 C24 -31.3(6) . . . . ?
O8 C22 C23 C28 -29.6(7) . . . . ?
O7 C22 C23 C28 149.2(5) . . . . ?
C28 C23 C24 C25 2.0(7) . . . . ?
C22 C23 C24 C25 -177.5(4) . . . . ?
C23 C24 C25 C26 -2.3(8) . . . . ?
C24 C25 C26 C27 0.7(8) . . . . ?
C25 C26 C27 C28 1.1(8) . . . . ?
C26 C27 C28 C23 -1.4(8) . . . . ?
C24 C23 C28 C27 -0.1(7) . . . . ?
C22 C23 C28 C27 179.4(4) . . . . ?
Fe4 O9 C29 O10 -5.2(7) . . . . ?
Fe4 O9 C29 C30 175.9(3) . . . . ?
Fe1 O10 C29 O9 -17.9(7) . . . . ?
Fe1 O10 C29 C30 161.0(3) . . . . ?
O9 C29 C30 C31 1.6(6) . . . . ?
O10 C29 C30 C31 -177.4(4) . . . . ?
O9 C29 C30 C35 -179.0(4) . . . . ?
O10 C29 C30 C35 2.0(6) . . . . ?
C35 C30 C31 C32 0.4(7) . . . . ?
C29 C30 C31 C32 179.8(4) . . . . ?
C30 C31 C32 C33 -0.5(8) . . . . ?
C31 C32 C33 C34 0.1(8) . . . . ?
C32 C33 C34 C35 0.4(7) . . . . ?
C31 C30 C35 C34 0.1(7) . . . . ?
C29 C30 C35 C34 -179.3(4) . . . . ?
C33 C34 C35 C30 -0.5(7) . . . . ?
Fe1 O11 C36 O12 1.2(6) . . . . ?
Fe1 O11 C36 C37 -177.7(3) . . . . ?
Fe4 O12 C36 O11 -19.0(7) . . . . ?
Fe4 O12 C36 C37 159.9(3) . . . . ?
O11 C36 C37 C38 4.1(7) . . . . ?
O12 C36 C37 C38 -174.9(5) . . . . ?
O11 C36 C37 C42 -175.4(5) . . . . ?
O12 C36 C37 C42 5.6(7) . . . . ?
C42 C37 C38 C39 -3.7(10) . . . . ?
C36 C37 C38 C39 176.9(6) . . . . ?
C37 C38 C39 C40 3.0(12) . . . . ?
C38 C39 C40 C41 -1.1(13) . . . . ?
C39 C40 C41 C42 -0.2(12) . . . . ?
C40 C41 C42 C37 -0.5(11) . . . . ?
C38 C37 C42 C41 2.5(9) . . . . ?
C36 C37 C42 C41 -178.0(6) . . . . ?
Fe5 O13 C43 O14 38.9(7) . . . . ?
Fe5 O13 C43 C44 -141.9(3) . . . . ?
O14 C43 C44 C45 166.8(4) . . . . ?
O13 C43 C44 C45 -12.5(6) . . . . ?
O14 C43 C44 C49 -15.5(6) . . . . ?
O13 C43 C44 C49 165.2(4) . . . . ?
C49 C44 C45 C46 2.2(7) . . . . ?
C43 C44 C45 C46 180.0(4) . . . . ?
C44 C45 C46 C47 -3.2(7) . . . . ?
C45 C46 C47 C48 1.9(7) . . . . ?
C46 C47 C48 C49 0.3(7) . . . . ?
C45 C44 C49 C48 0.0(7) . . . . ?
C43 C44 C49 C48 -177.8(4) . . . . ?
C47 C48 C49 C44 -1.3(7) . . . . ?
C54 N1 C50 C51 -35.9(9) . . . . ?
Fe1 N1 C50 C51 171.9(5) . . . . ?
N1 C50 C51 C52 39.0(10) . . . . ?
C50 C51 C52 C53 -40.5(9) . . . . ?
C51 C52 C53 C54 40.5(9) . . . . ?
C50 N1 C54 C53 35.6(9) . . . . ?
Fe1 N1 C54 C53 -167.1(5) . . . . ?
C50 N1 C54 C55 179.5(6) . . . . ?
Fe1 N1 C54 C55 -23.2(7) . . . . ?
C52 C53 C54 N1 -38.7(9) . . . . ?
C52 C53 C54 C55 179.0(6) . . . . ?
Fe1 O15 C55 C54 -32.0(6) . . . . ?
Fe2 O15 C55 C54 -160.1(4) . . . . ?
N1 C54 C55 O15 35.2(7) . . . . ?
C53 C54 C55 O15 179.0(6) . . . . ?
C60 N2 C56 C57 -54.8(6) . . . . ?
Fe3 N2 C56 C57 176.3(4) . . . . ?
N2 C56 C57 C58 53.6(7) . . . . ?
C56 C57 C58 C59 -53.8(7) . . . . ?
C57 C58 C59 C60 55.0(7) . . . . ?
C56 N2 C60 C61 -177.0(4) . . . . ?
Fe3 N2 C60 C61 -41.5(4) . . . . ?
C56 N2 C60 C59 56.6(5) . . . . ?
Fe3 N2 C60 C59 -167.9(3) . . . . ?
C58 C59 C60 N2 -56.6(6) . . . . ?
C58 C59 C60 C61 -179.6(5) . . . . ?
Fe5 O16 C61 C60 147.2(4) . . . . ?
Fe3 O16 C61 C60 -26.7(5) . . . . ?
N2 C60 C61 O16 44.1(5) . . . . ?
C59 C60 C61 O16 169.0(4) . . . . ?
C66 N3 C62 C63 53.1(5) . . . . ?
Fe4 N3 C62 C63 177.1(3) . . . . ?
N3 C62 C63 C64 -53.4(5) . . . . ?
C62 C63 C64 C65 53.7(5) . . . . ?
C63 C64 C65 C66 -55.3(5) . . . . ?
C62 N3 C66 C67 179.0(3) . . . . ?
Fe4 N3 C66 C67 48.1(4) . . . . ?
C62 N3 C66 C65 -55.1(5) . . . . ?
Fe4 N3 C66 C65 174.0(3) . . . . ?
C64 C65 C66 C67 179.3(4) . . . . ?
C64 C65 C66 N3 56.7(5) . . . . ?
Fe5 O17 C67 C66 123.6(3) . . . . ?
Fe4 O17 C67 C66 5.7(4) . . . . ?
N3 C66 C67 O17 -36.1(5) . . . . ?
C65 C66 C67 O17 -161.2(4) . . . . ?
C72 N4 C68 C69 -56.9(5) . . . . ?
Fe5 N4 C68 C69 175.8(3) . . . . ?
N4 C68 C69 C70 54.3(6) . . . . ?
C68 C69 C70 C71 -51.9(6) . . . . ?
C69 C70 C71 C72 51.9(5) . . . . ?
C68 N4 C72 C73 -175.2(4) . . . . ?
Fe5 N4 C72 C73 -40.6(4) . . . . ?
C68 N4 C72 C71 57.4(5) . . . . ?
Fe5 N4 C72 C71 -168.0(3) . . . . ?
C70 C71 C72 N4 -54.6(5) . . . . ?
C70 C71 C72 C73 -177.9(4) . . . . ?
Fe4 O18 C73 C72 -169.4(3) . . . . ?
Fe5 O18 C73 C72 -35.3(4) . . . . ?
N4 C72 C73 O18 49.2(5) . . . . ?
C71 C72 C73 O18 174.5(4) . . . . ?
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
N2 H2N O8 0.87(2) 2.23(4) 2.967(5) 143(5) .
N3 H3N O14 0.840(19) 2.18(2) 3.019(5) 174(5) .
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full 26.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max 1.053
_refine_diff_density_min -0.551
_refine_diff_density_rms 0.083
# start Validation Reply Form
_vrf_PLAT220_ck11
;
RESPONSE: All atomic species have been correctly identified.
However, this alert is due to the higher thermal ellipsoids of some
carbon atoms of the ligands of the complex.
;
_vrf_PLAT041_ck11
;
RESPONSE: The missing (not located by a difference synthesis) H-atoms
of the crystallization water molecule have been included
in the sum and moiety formula and the Mr, Dx, and F(000) have been
modified accordingly. These modifications account for the differences
detected in the relevant data items.
;
_vrf_PLAT042_ck11
;
RESPONSE: See comment above.
;
# end Validation Reply Form
_vrf_PLAT068_ck11
;
RESPONSE: See comment above.
;
_vrf_PLAT311_ck11
;
RESPONSE: It was not possible to locate the H-atoms of the
disordered lattice water molecule O21 (O21A: 55%, O21B: 45%)
from a difference map.
;
_vrf_FORMU01_ck11
;
RESPONSE: Hydrogen atoms not located by the X-ray analysis have been included
in the chemical formula; this accounts for the difference between formula and
atom_site contents.
;
# end Validation Reply Form
#===END
# Attachment '- 5.cif'
data_ck43
_database_code_depnum_ccdc_archive 'CCDC 836727'
#TrackingRef '- 5.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C51 H98 Cl Fe5 N2 O22, C5 H10 O2'
_chemical_formula_sum 'C56 H108 Cl Fe5 N2 O24'
_chemical_formula_weight 1508.14
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'
Cl Cl 0.1484 0.1585 '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 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 16.4685(8)
_cell_length_b 18.6761(7)
_cell_length_c 24.3627(9)
_cell_angle_alpha 90.00
_cell_angle_beta 102.958(5)
_cell_angle_gamma 90.00
_cell_volume 7302.4(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 4179
_cell_measurement_theta_min 3.1116
_cell_measurement_theta_max 30.2616
_exptl_crystal_description prism
_exptl_crystal_colour 'light purple'
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.372
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3188
_exptl_absorpt_coefficient_mu 1.077
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.98520
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details
'Empirical absorption correction (CrysAlis RED, Oxford Diffraction)'
_exptl_special_details ?
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray source'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur-3 with Sapphire CCD'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 16.0288
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 12906
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.3118
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 3.21
_diffrn_reflns_theta_max 25.08
_reflns_number_total 12906
_reflns_number_gt 4766
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics
;ORTEP-3 for Windows (Farrugia, 1997); PLATON (Spek, 1990);
MERCURY (Bruno et al. 2002)
;
_computing_publication_material 'WINGX (Farrugia, 1999)'
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435-436.
Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838.
Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford
Diffraction Ltd, Abingdon, Oxford, England.
Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany.
Spek, A. L. (2008). PLATON. University of Utrecht, The Netherlands.
;
_refine_special_details
;
Atoms C9-C10-C11 and C24-C25-C26 of the t-butyl groups of two pivalic
ligands are disordered over two sites (50:50).
The structure was refined as a non-merohedral twin with a ratio of the
twin components of 0.88:0.12.
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^)+(0.0201P)^2^] 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 12906
_refine_ls_number_parameters 880
_refine_ls_number_restraints 149
_refine_ls_R_factor_all 0.1828
_refine_ls_R_factor_gt 0.0660
_refine_ls_wR_factor_ref 0.1102
_refine_ls_wR_factor_gt 0.0962
_refine_ls_goodness_of_fit_ref 0.840
_refine_ls_restrained_S_all 0.851
_refine_ls_shift/su_max 0.000
_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
Fe1 Fe 0.74123(7) 0.31100(5) 0.32435(4) 0.0234(3) Uani 1 1 d . A .
Fe2 Fe 0.77198(6) 0.22096(6) 0.20478(4) 0.0213(3) Uani 1 1 d . A .
Fe3 Fe 0.91759(7) 0.21032(6) 0.30398(4) 0.0241(3) Uani 1 1 d . A .
Fe4 Fe 0.75712(7) 0.15519(5) 0.33592(4) 0.0219(3) Uani 1 1 d . A .
Fe5 Fe 0.71384(7) 0.24656(6) 0.44889(4) 0.0274(3) Uani 1 1 d . A .
Cl Cl 0.83332(13) 0.21447(11) 0.51602(7) 0.0399(6) Uani 1 1 d . . .
C1 C 0.8152(5) 0.1403(4) 0.1037(3) 0.030(2) Uani 1 1 d . A .
H1A H 0.8131 0.1401 0.0636 0.036 Uiso 1 1 calc R . .
H1B H 0.7889 0.0968 0.1128 0.036 Uiso 1 1 calc R . .
C2 C 0.9041(5) 0.1417(4) 0.1356(3) 0.035(2) Uani 1 1 d . . .
H2A H 0.9256 0.1897 0.1335 0.042 Uiso 1 1 calc R . .
H2B H 0.9359 0.1099 0.1169 0.042 Uiso 1 1 calc R . .
C3 C 0.9190(5) 0.1201(4) 0.1971(3) 0.037(2) Uani 1 1 d . . .
H3A H 0.8993 0.0714 0.1995 0.044 Uiso 1 1 calc R . .
H3B H 0.9784 0.1206 0.2134 0.044 Uiso 1 1 calc R . .
C4 C 0.9925(6) 0.0816(5) 0.4580(4) 0.078(3) Uani 1 1 d DU . .
H4A H 1.0465 0.0754 0.4489 0.094 Uiso 1 1 calc R . .
H4B H 0.9962 0.0608 0.4950 0.094 Uiso 1 1 calc R . .
C5 C 0.9313(6) 0.0400(5) 0.4172(4) 0.065(3) Uani 1 1 d DU . .
H5A H 0.8798 0.0388 0.4303 0.078 Uiso 1 1 calc R . .
H5B H 0.9515 -0.0088 0.4177 0.078 Uiso 1 1 calc R . .
C6 C 0.9111(5) 0.0649(4) 0.3575(3) 0.033(2) Uani 1 1 d . . .
H6A H 0.9611 0.0627 0.3428 0.040 Uiso 1 1 calc R . .
H6B H 0.8704 0.0327 0.3353 0.040 Uiso 1 1 calc R . .
C7 C 0.6759(5) 0.3514(5) 0.2077(4) 0.028(2) Uani 1 1 d . A .
C8 C 0.6183(6) 0.4077(4) 0.1717(3) 0.035(2) Uani 1 1 d D . .
C9A C 0.5293(9) 0.3765(10) 0.1571(8) 0.057(6) Uani 0.50 1 d PDU A 1
H9A1 H 0.5077 0.3744 0.1906 0.086 Uiso 0.50 1 calc PR A 1
H9A2 H 0.5305 0.3293 0.1419 0.086 Uiso 0.50 1 calc PR A 1
H9A3 H 0.4941 0.4067 0.1298 0.086 Uiso 0.50 1 calc PR A 1
C10A C 0.6472(11) 0.4151(10) 0.1156(6) 0.046(5) Uani 0.50 1 d PDU A 1
H10A H 0.6193 0.4550 0.0946 0.069 Uiso 0.50 1 calc PR A 1
H10B H 0.6340 0.3721 0.0939 0.069 Uiso 0.50 1 calc PR A 1
H10C H 0.7063 0.4230 0.1236 0.069 Uiso 0.50 1 calc PR A 1
C11A C 0.6259(14) 0.4790(9) 0.1997(8) 0.078(7) Uani 0.50 1 d PDU A 1
H11A H 0.5822 0.5098 0.1802 0.117 Uiso 0.50 1 calc PR A 1
H11B H 0.6790 0.4997 0.1989 0.117 Uiso 0.50 1 calc PR A 1
H11C H 0.6213 0.4735 0.2381 0.117 Uiso 0.50 1 calc PR A 1
C9B C 0.5586(13) 0.3752(11) 0.1225(8) 0.085(8) Uani 0.50 1 d PDU A 2
H9B1 H 0.5277 0.3377 0.1355 0.128 Uiso 0.50 1 calc PR A 2
H9B2 H 0.5889 0.3558 0.0966 0.128 Uiso 0.50 1 calc PR A 2
H9B3 H 0.5208 0.4114 0.1039 0.128 Uiso 0.50 1 calc PR A 2
C10B C 0.6710(12) 0.4666(10) 0.1536(9) 0.065(6) Uani 0.50 1 d PU A 2
H10D H 0.6352 0.5035 0.1342 0.098 Uiso 0.50 1 calc PR A 2
H10E H 0.7032 0.4468 0.1289 0.098 Uiso 0.50 1 calc PR A 2
H10F H 0.7078 0.4865 0.1862 0.098 Uiso 0.50 1 calc PR A 2
C11B C 0.5667(12) 0.4414(10) 0.2101(7) 0.055(6) Uani 0.50 1 d PU A 2
H11D H 0.6032 0.4653 0.2409 0.083 Uiso 0.50 1 calc PR A 2
H11E H 0.5364 0.4046 0.2244 0.083 Uiso 0.50 1 calc PR A 2
H11F H 0.5283 0.4753 0.1890 0.083 Uiso 0.50 1 calc PR A 2
C12 C 0.5904(5) 0.2189(5) 0.2944(3) 0.025(2) Uani 1 1 d U A .
C13 C 0.4958(5) 0.2080(4) 0.2781(3) 0.032(2) Uani 1 1 d . . .
C14 C 0.4707(5) 0.1540(4) 0.3179(3) 0.047(3) Uani 1 1 d . . .
H14A H 0.4113 0.1473 0.3081 0.070 Uiso 1 1 calc R . .
H14B H 0.4870 0.1713 0.3559 0.070 Uiso 1 1 calc R . .
H14C H 0.4978 0.1091 0.3149 0.070 Uiso 1 1 calc R . .
C15 C 0.4510(4) 0.2766(4) 0.2810(3) 0.046(2) Uani 1 1 d . . .
H15A H 0.4634 0.3095 0.2537 0.069 Uiso 1 1 calc R . .
H15B H 0.4687 0.2967 0.3180 0.069 Uiso 1 1 calc R . .
H15C H 0.3921 0.2678 0.2732 0.069 Uiso 1 1 calc R . .
C16 C 0.4746(5) 0.1775(5) 0.2183(3) 0.055(3) Uani 1 1 d . . .
H16A H 0.5014 0.1319 0.2179 0.083 Uiso 1 1 calc R . .
H16B H 0.4936 0.2098 0.1933 0.083 Uiso 1 1 calc R . .
H16C H 0.4153 0.1715 0.2063 0.083 Uiso 1 1 calc R . .
C17 C 0.7061(5) 0.0781(4) 0.2261(3) 0.023(2) Uani 1 1 d . A .
C18 C 0.6667(6) 0.0081(4) 0.2001(3) 0.030(2) Uani 1 1 d . . .
C19 C 0.6106(6) -0.0195(5) 0.2379(4) 0.074(3) Uani 1 1 d . . .
H19A H 0.5726 0.0176 0.2430 0.111 Uiso 1 1 calc R . .
H19B H 0.6444 -0.0331 0.2739 0.111 Uiso 1 1 calc R . .
H19C H 0.5798 -0.0603 0.2206 0.111 Uiso 1 1 calc R . .
C20 C 0.6140(5) 0.0199(4) 0.1416(3) 0.054(3) Uani 1 1 d . . .
H20A H 0.6478 0.0397 0.1180 0.081 Uiso 1 1 calc R . .
H20B H 0.5695 0.0524 0.1433 0.081 Uiso 1 1 calc R . .
H20C H 0.5911 -0.0250 0.1263 0.081 Uiso 1 1 calc R . .
C21 C 0.7351(6) -0.0435(4) 0.1978(4) 0.075(3) Uani 1 1 d . . .
H21A H 0.7116 -0.0896 0.1863 0.112 Uiso 1 1 calc R . .
H21B H 0.7717 -0.0472 0.2343 0.112 Uiso 1 1 calc R . .
H21C H 0.7658 -0.0268 0.1711 0.112 Uiso 1 1 calc R . .
C22 C 0.9107(5) 0.3281(4) 0.2209(3) 0.021(2) Uani 1 1 d . A .
C23 C 0.9513(6) 0.3934(4) 0.2012(3) 0.039(2) Uani 1 1 d D . .
C24A C 0.8940(11) 0.4319(10) 0.1526(7) 0.056(7) Uani 0.50 1 d PDU B 1
H24A H 0.9247 0.4688 0.1385 0.083 Uiso 0.50 1 calc PR B 1
H24B H 0.8485 0.4530 0.1654 0.083 Uiso 0.50 1 calc PR B 1
H24C H 0.8728 0.3983 0.1230 0.083 Uiso 0.50 1 calc PR B 1
C25A C 1.0216(12) 0.3586(10) 0.1750(9) 0.086(7) Uani 0.50 1 d PDU B 1
H25A H 0.9966 0.3365 0.1397 0.129 Uiso 0.50 1 calc PR B 1
H25B H 1.0510 0.3232 0.2004 0.129 Uiso 0.50 1 calc PR B 1
H25C H 1.0598 0.3951 0.1691 0.129 Uiso 0.50 1 calc PR B 1
C26A C 0.9938(16) 0.4408(11) 0.2471(8) 0.086(8) Uani 0.50 1 d PDU B 1
H26A H 1.0205 0.4792 0.2317 0.129 Uiso 0.50 1 calc PR B 1
H26B H 1.0348 0.4140 0.2733 0.129 Uiso 0.50 1 calc PR B 1
H26C H 0.9537 0.4602 0.2662 0.129 Uiso 0.50 1 calc PR B 1
C24B C 0.9297(12) 0.3997(10) 0.1401(6) 0.050(6) Uani 0.50 1 d PDU B 2
H24D H 0.9435 0.4469 0.1294 0.074 Uiso 0.50 1 calc PR B 2
H24E H 0.8710 0.3917 0.1267 0.074 Uiso 0.50 1 calc PR B 2
H24F H 0.9602 0.3648 0.1239 0.074 Uiso 0.50 1 calc PR B 2
C25B C 1.0392(9) 0.4026(10) 0.2321(7) 0.044(5) Uani 0.50 1 d PDU B 2
H25D H 1.0722 0.3639 0.2229 0.066 Uiso 0.50 1 calc PR B 2
H25E H 1.0421 0.4025 0.2719 0.066 Uiso 0.50 1 calc PR B 2
H25F H 1.0602 0.4472 0.2215 0.066 Uiso 0.50 1 calc PR B 2
C26B C 0.9089(12) 0.4597(8) 0.2232(8) 0.063(6) Uani 0.50 1 d PDU B 2
H26D H 0.9311 0.5030 0.2112 0.094 Uiso 0.50 1 calc PR B 2
H26E H 0.9199 0.4584 0.2636 0.094 Uiso 0.50 1 calc PR B 2
H26F H 0.8498 0.4580 0.2081 0.094 Uiso 0.50 1 calc PR B 2
C27 C 1.0967(4) 0.1777(5) 0.3512(3) 0.048(2) Uani 1 1 d DU A .
C28 C 1.1813(6) 0.1859(6) 0.3338(4) 0.062(3) Uani 1 1 d D . .
C29 C 1.2491(7) 0.1439(6) 0.3746(4) 0.104(4) Uani 1 1 d U . .
H29A H 1.2573 0.1643 0.4116 0.157 Uiso 1 1 calc R . .
H29B H 1.3003 0.1463 0.3620 0.157 Uiso 1 1 calc R . .
H29C H 1.2323 0.0948 0.3757 0.157 Uiso 1 1 calc R . .
C30 C 1.2111(7) 0.2614(6) 0.3399(5) 0.121(4) Uani 1 1 d U . .
H30A H 1.1664 0.2928 0.3230 0.181 Uiso 1 1 calc R . .
H30B H 1.2565 0.2671 0.3214 0.181 Uiso 1 1 calc R . .
H30C H 1.2297 0.2728 0.3791 0.181 Uiso 1 1 calc R . .
C31 C 1.1718(7) 0.1618(7) 0.2718(4) 0.130(5) Uani 1 1 d DU . .
H31A H 1.1620 0.1111 0.2690 0.195 Uiso 1 1 calc R . .
H31B H 1.2219 0.1729 0.2596 0.195 Uiso 1 1 calc R . .
H31C H 1.1256 0.1865 0.2484 0.195 Uiso 1 1 calc R . .
C32 C 0.9210(5) 0.3368(4) 0.3796(3) 0.024(2) Uani 1 1 d U A .
C33 C 0.9812(5) 0.3850(4) 0.4194(3) 0.032(2) Uani 1 1 d . . .
C34 C 0.9624(6) 0.4613(4) 0.4059(4) 0.068(3) Uani 1 1 d . . .
H34A H 0.9693 0.4712 0.3685 0.103 Uiso 1 1 calc R . .
H34B H 0.9997 0.4909 0.4324 0.103 Uiso 1 1 calc R . .
H34C H 0.9060 0.4714 0.4079 0.103 Uiso 1 1 calc R . .
C35 C 1.0697(6) 0.3675(5) 0.4172(4) 0.073(3) Uani 1 1 d . . .
H35A H 1.0761 0.3721 0.3791 0.109 Uiso 1 1 calc R . .
H35B H 1.0824 0.3193 0.4300 0.109 Uiso 1 1 calc R . .
H35C H 1.1069 0.4000 0.4410 0.109 Uiso 1 1 calc R . .
C36 C 0.9692(6) 0.3680(4) 0.4781(3) 0.060(3) Uani 1 1 d . . .
H36A H 1.0008 0.4012 0.5047 0.090 Uiso 1 1 calc R . .
H36B H 0.9879 0.3201 0.4883 0.090 Uiso 1 1 calc R . .
H36C H 0.9112 0.3720 0.4786 0.090 Uiso 1 1 calc R . .
C37 C 0.7055(5) 0.4002(4) 0.4172(4) 0.027(2) Uani 1 1 d . A .
C38 C 0.6821(5) 0.4744(4) 0.4372(3) 0.031(2) Uani 1 1 d . . .
C39 C 0.7565(6) 0.5061(4) 0.4762(3) 0.060(3) Uani 1 1 d . . .
H39A H 0.7733 0.4759 0.5086 0.090 Uiso 1 1 calc R . .
H39B H 0.7426 0.5528 0.4879 0.090 Uiso 1 1 calc R . .
H39C H 0.8013 0.5101 0.4571 0.090 Uiso 1 1 calc R . .
C40 C 0.6138(6) 0.4631(4) 0.4692(4) 0.067(3) Uani 1 1 d . . .
H40A H 0.5633 0.4489 0.4434 0.100 Uiso 1 1 calc R . .
H40B H 0.6045 0.5069 0.4875 0.100 Uiso 1 1 calc R . .
H40C H 0.6304 0.4263 0.4970 0.100 Uiso 1 1 calc R . .
C41 C 0.6487(6) 0.5221(4) 0.3869(3) 0.062(3) Uani 1 1 d . . .
H41A H 0.6922 0.5317 0.3674 0.092 Uiso 1 1 calc R . .
H41B H 0.6294 0.5663 0.3994 0.092 Uiso 1 1 calc R . .
H41C H 0.6033 0.4984 0.3618 0.092 Uiso 1 1 calc R . .
C42 C 0.5786(6) 0.2703(4) 0.4759(3) 0.031(2) Uani 1 1 d . A .
C43 C 0.4933(5) 0.2777(5) 0.4904(3) 0.033(2) Uani 1 1 d . . .
C44 C 0.4610(5) 0.2007(4) 0.4912(3) 0.051(3) Uani 1 1 d . . .
H44A H 0.4980 0.1739 0.5199 0.076 Uiso 1 1 calc R . .
H44B H 0.4585 0.1787 0.4552 0.076 Uiso 1 1 calc R . .
H44C H 0.4063 0.2013 0.4988 0.076 Uiso 1 1 calc R . .
C45 C 0.5033(5) 0.3140(4) 0.5474(3) 0.045(3) Uani 1 1 d . . .
H45A H 0.4502 0.3164 0.5574 0.068 Uiso 1 1 calc R . .
H45B H 0.5247 0.3615 0.5455 0.068 Uiso 1 1 calc R . .
H45C H 0.5414 0.2869 0.5754 0.068 Uiso 1 1 calc R . .
C46 C 0.4322(5) 0.3194(5) 0.4472(3) 0.054(3) Uani 1 1 d . . .
H46A H 0.4342 0.3029 0.4102 0.080 Uiso 1 1 calc R . .
H46B H 0.4462 0.3693 0.4505 0.080 Uiso 1 1 calc R . .
H46C H 0.3770 0.3126 0.4531 0.080 Uiso 1 1 calc R . .
C47 C 0.6967(5) 0.0877(5) 0.4294(3) 0.029(2) Uani 1 1 d . A .
C48 C 0.6775(6) 0.0163(4) 0.4556(3) 0.035(2) Uani 1 1 d . . .
C49 C 0.5924(5) 0.0194(4) 0.4684(3) 0.048(3) Uani 1 1 d . . .
H49A H 0.5516 0.0287 0.4343 0.072 Uiso 1 1 calc R . .
H49B H 0.5910 0.0571 0.4950 0.072 Uiso 1 1 calc R . .
H49C H 0.5804 -0.0255 0.4840 0.072 Uiso 1 1 calc R . .
C50 C 0.7433(6) 0.0087(5) 0.5100(4) 0.068(3) Uani 1 1 d . . .
H50A H 0.7415 0.0497 0.5335 0.102 Uiso 1 1 calc R . .
H50B H 0.7974 0.0054 0.5016 0.102 Uiso 1 1 calc R . .
H50C H 0.7327 -0.0339 0.5294 0.102 Uiso 1 1 calc R . .
C51 C 0.6818(6) -0.0466(4) 0.4160(4) 0.058(3) Uani 1 1 d . . .
H51A H 0.6426 -0.0391 0.3808 0.087 Uiso 1 1 calc R . .
H51B H 0.6684 -0.0902 0.4329 0.087 Uiso 1 1 calc R . .
H51C H 0.7370 -0.0499 0.4095 0.087 Uiso 1 1 calc R . .
O1 O 0.8782(3) 0.1661(2) 0.22948(17) 0.0224(13) Uani 1 1 d . . .
O2 O 0.8794(3) 0.1354(2) 0.35142(17) 0.0205(13) Uani 1 1 d . . .
O3 O 0.7204(3) 0.3710(2) 0.2544(2) 0.0253(14) Uani 1 1 d . . .
O4 O 0.6769(3) 0.2891(3) 0.18659(18) 0.0237(13) Uani 1 1 d . . .
O5 O 0.6200(3) 0.2802(3) 0.29499(17) 0.0225(13) Uani 1 1 d . . .
O6 O 0.6348(3) 0.1614(2) 0.30506(18) 0.0218(13) Uani 1 1 d . . .
O7 O 0.7454(3) 0.0758(2) 0.27681(19) 0.0237(13) Uani 1 1 d . . .
O8 O 0.6990(3) 0.1339(2) 0.19620(19) 0.0214(13) Uani 1 1 d . . .
O9 O 0.8409(3) 0.3081(2) 0.19118(19) 0.0249(13) Uani 1 1 d . . .
O10 O 0.9483(3) 0.3006(3) 0.2674(2) 0.0297(14) Uani 1 1 d . . .
O11 O 1.0375(3) 0.1710(2) 0.31396(17) 0.0159(12) Uani 1 1 d DU . .
O12 O 1.1008(4) 0.1774(3) 0.4053(2) 0.076(2) Uani 1 1 d D . .
O13 O 0.9427(3) 0.2716(3) 0.37502(18) 0.0259(13) Uani 1 1 d . . .
O14 O 0.8508(3) 0.3612(2) 0.3546(2) 0.0293(14) Uani 1 1 d . . .
O15 O 0.6947(3) 0.3882(2) 0.3655(2) 0.0280(14) Uani 1 1 d . . .
O16 O 0.7325(3) 0.3544(3) 0.45616(19) 0.0321(15) Uani 1 1 d . . .
O17 O 0.5843(3) 0.2716(3) 0.4249(2) 0.0340(14) Uani 1 1 d . . .
O18 O 0.6449(3) 0.2602(3) 0.51297(19) 0.0335(15) Uani 1 1 d . . .
O19 O 0.7407(3) 0.0833(2) 0.39313(19) 0.0262(14) Uani 1 1 d . . .
O20 O 0.6717(3) 0.1444(3) 0.44769(19) 0.0325(15) Uani 1 1 d . . .
O21 O 0.7911(3) 0.2327(2) 0.28668(17) 0.0182(12) Uani 1 1 d . . .
O22 O 0.7510(3) 0.2381(2) 0.38291(17) 0.0229(13) Uani 1 1 d . . .
N1 N 0.7688(4) 0.2029(4) 0.1176(3) 0.0236(16) Uani 1 1 d D . .
H1 H 0.792(4) 0.232(3) 0.099(2) 0.035 Uiso 1 1 d D . .
H2 H 0.7170(16) 0.195(4) 0.105(3) 0.035 Uiso 1 1 d D . .
N2 N 0.9773(5) 0.1600(4) 0.4620(3) 0.053(2) Uani 1 1 d U . .
O23 O 0.2025(4) 0.2202(4) 0.4982(3) 0.107(3) Uani 1 1 d D . .
O24 O 0.1105(5) 0.1785(5) 0.5471(3) 0.105(3) Uani 1 1 d D . .
C52 C 0.1711(7) 0.2109(6) 0.5440(5) 0.079(4) Uani 1 1 d D . .
C53 C 0.2149(8) 0.2482(6) 0.5973(6) 0.097(4) Uani 1 1 d DU . .
C54 C 0.2251(8) 0.2008(6) 0.6502(4) 0.124(5) Uani 1 1 d . . .
H54A H 0.1729 0.1784 0.6508 0.186 Uiso 1 1 calc R . .
H54B H 0.2426 0.2298 0.6833 0.186 Uiso 1 1 calc R . .
H54C H 0.2663 0.1646 0.6494 0.186 Uiso 1 1 calc R . .
C55 C 0.1651(8) 0.3169(6) 0.6040(5) 0.143(6) Uani 1 1 d DU . .
H55A H 0.1629 0.3476 0.5721 0.214 Uiso 1 1 calc R . .
H55B H 0.1921 0.3415 0.6377 0.214 Uiso 1 1 calc R . .
H55C H 0.1095 0.3041 0.6063 0.214 Uiso 1 1 calc R . .
C56 C 0.3032(7) 0.2683(7) 0.5912(5) 0.156(6) Uani 1 1 d D . .
H56A H 0.3385 0.2269 0.5983 0.235 Uiso 1 1 calc R . .
H56B H 0.3253 0.3052 0.6179 0.235 Uiso 1 1 calc R . .
H56C H 0.3008 0.2854 0.5537 0.235 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
Fe1 0.0316(8) 0.0188(7) 0.0190(6) -0.0006(6) 0.0038(6) 0.0018(6)
Fe2 0.0261(8) 0.0206(7) 0.0173(6) -0.0002(6) 0.0053(6) -0.0014(6)
Fe3 0.0248(7) 0.0266(8) 0.0195(6) 0.0014(6) 0.0019(5) -0.0013(6)
Fe4 0.0291(8) 0.0197(7) 0.0172(7) 0.0007(6) 0.0056(6) 0.0002(6)
Fe5 0.0377(8) 0.0266(7) 0.0183(6) -0.0019(6) 0.0071(6) 0.0022(6)
Cl 0.0509(15) 0.0476(15) 0.0191(11) 0.0015(11) 0.0035(10) 0.0133(13)
C1 0.036(6) 0.027(6) 0.029(5) 0.005(4) 0.015(5) 0.009(5)
C2 0.037(6) 0.036(6) 0.036(5) -0.002(4) 0.017(5) 0.022(5)
C3 0.047(6) 0.037(6) 0.027(5) -0.009(4) 0.009(5) 0.018(5)
C4 0.104(7) 0.052(4) 0.061(6) 0.003(5) -0.016(6) 0.029(6)
C5 0.087(7) 0.053(6) 0.055(6) 0.000(5) 0.013(6) 0.022(5)
C6 0.030(6) 0.033(6) 0.038(6) 0.003(5) 0.010(5) 0.002(5)
C7 0.024(6) 0.030(6) 0.037(6) 0.007(5) 0.021(5) 0.003(5)
C8 0.046(7) 0.025(6) 0.032(6) 0.008(5) 0.004(5) 0.019(5)
C9A 0.050(10) 0.059(10) 0.060(9) 0.014(8) 0.007(8) 0.013(8)
C10A 0.050(9) 0.047(9) 0.039(8) 0.028(7) 0.006(7) 0.012(7)
C11A 0.079(11) 0.066(10) 0.081(10) 0.001(8) 0.001(8) 0.021(8)
C9B 0.081(11) 0.080(11) 0.084(11) 0.001(9) -0.004(9) 0.029(9)
C10B 0.069(10) 0.059(10) 0.068(9) 0.016(8) 0.017(8) 0.010(8)
C11B 0.055(9) 0.053(9) 0.062(9) 0.001(8) 0.022(8) 0.027(8)
C12 0.028(3) 0.030(3) 0.021(3) 0.001(3) 0.011(2) 0.001(3)
C13 0.030(6) 0.038(6) 0.028(5) -0.001(5) 0.002(4) 0.007(5)
C14 0.026(6) 0.049(6) 0.067(7) -0.010(6) 0.014(5) 0.000(5)
C15 0.019(5) 0.070(7) 0.045(6) 0.005(5) -0.003(4) 0.011(5)
C16 0.033(6) 0.083(8) 0.041(6) -0.013(5) -0.009(5) 0.008(5)
C17 0.014(5) 0.032(6) 0.026(5) 0.002(5) 0.012(4) 0.004(4)
C18 0.051(7) 0.017(5) 0.021(5) -0.003(4) 0.004(5) -0.012(5)
C19 0.086(9) 0.061(7) 0.075(8) -0.009(6) 0.018(7) -0.048(6)
C20 0.061(7) 0.031(6) 0.063(7) -0.013(5) 0.000(6) -0.014(5)
C21 0.072(8) 0.033(6) 0.105(9) -0.037(6) -0.010(7) 0.012(6)
C22 0.029(6) 0.022(5) 0.016(5) -0.001(4) 0.012(4) -0.001(4)
C23 0.049(7) 0.029(6) 0.036(6) 0.015(5) 0.005(5) -0.018(5)
C24A 0.058(10) 0.047(10) 0.062(10) 0.004(8) 0.015(8) -0.004(8)
C25A 0.091(11) 0.078(10) 0.097(10) 0.026(8) 0.039(9) -0.025(8)
C26A 0.095(11) 0.078(11) 0.086(11) 0.015(9) 0.022(9) -0.027(9)
C24B 0.058(10) 0.059(10) 0.034(9) 0.004(7) 0.017(8) -0.017(8)
C25B 0.035(9) 0.045(9) 0.051(9) 0.015(7) 0.008(7) -0.024(7)
C26B 0.066(10) 0.047(9) 0.075(10) 0.014(8) 0.014(8) -0.011(8)
C27 0.040(4) 0.053(5) 0.048(4) 0.001(4) 0.001(3) 0.002(4)
C28 0.046(7) 0.091(9) 0.052(7) -0.004(6) 0.018(6) -0.003(6)
C29 0.074(7) 0.132(8) 0.102(7) 0.017(6) 0.008(6) 0.018(6)
C30 0.105(8) 0.086(8) 0.180(10) -0.025(8) 0.050(7) -0.047(7)
C31 0.122(9) 0.183(10) 0.093(8) -0.003(8) 0.039(8) -0.012(8)
C32 0.029(5) 0.027(4) 0.019(4) 0.003(4) 0.014(4) -0.006(4)
C33 0.031(6) 0.018(5) 0.042(6) -0.009(4) -0.004(5) -0.011(5)
C34 0.082(8) 0.046(7) 0.060(7) -0.013(6) -0.020(6) -0.016(6)
C35 0.049(8) 0.075(8) 0.088(8) -0.046(6) 0.004(6) -0.022(6)
C36 0.067(8) 0.055(7) 0.047(7) -0.013(5) -0.009(6) -0.019(6)
C37 0.024(6) 0.024(6) 0.031(6) -0.010(5) -0.001(5) -0.014(4)
C38 0.038(6) 0.027(6) 0.023(5) -0.005(4) 0.000(5) 0.009(5)
C39 0.090(9) 0.032(6) 0.048(6) -0.018(5) -0.005(6) 0.014(6)
C40 0.072(8) 0.054(7) 0.083(8) -0.012(6) 0.036(7) 0.024(6)
C41 0.103(9) 0.040(6) 0.039(6) -0.004(5) 0.012(6) 0.033(6)
C42 0.055(7) 0.022(5) 0.017(5) -0.002(4) 0.011(5) -0.004(5)
C43 0.030(6) 0.040(6) 0.032(5) -0.005(5) 0.010(5) -0.003(5)
C44 0.047(6) 0.069(8) 0.040(6) -0.016(5) 0.018(5) -0.010(6)
C45 0.045(6) 0.064(7) 0.028(5) -0.021(5) 0.011(5) -0.008(5)
C46 0.025(6) 0.081(8) 0.053(6) -0.004(6) 0.007(5) 0.006(5)
C47 0.042(7) 0.032(6) 0.013(5) 0.006(4) 0.008(5) 0.002(5)
C48 0.043(7) 0.035(6) 0.029(5) 0.013(5) 0.015(5) 0.001(5)
C49 0.070(8) 0.031(6) 0.053(6) 0.011(5) 0.036(6) -0.011(5)
C50 0.070(8) 0.069(8) 0.064(7) 0.045(6) 0.014(6) -0.011(6)
C51 0.085(8) 0.021(6) 0.077(7) 0.006(5) 0.038(7) -0.008(5)
O1 0.027(3) 0.032(3) 0.013(3) -0.003(2) 0.012(3) -0.002(3)
O2 0.032(4) 0.016(3) 0.011(3) 0.000(2) 0.000(3) 0.002(3)
O3 0.043(4) 0.011(3) 0.022(3) -0.002(3) 0.007(3) -0.004(3)
O4 0.029(3) 0.023(3) 0.018(3) -0.003(3) 0.003(3) 0.009(3)
O5 0.033(3) 0.019(3) 0.017(3) 0.004(3) 0.007(2) 0.001(3)
O6 0.029(4) 0.024(3) 0.015(3) -0.001(3) 0.009(3) -0.002(3)
O7 0.036(4) 0.023(3) 0.012(3) 0.002(3) 0.006(3) 0.000(3)
O8 0.026(3) 0.019(3) 0.018(3) -0.002(3) 0.003(3) 0.001(3)
O9 0.031(4) 0.019(3) 0.023(3) 0.007(3) 0.002(3) -0.001(3)
O10 0.031(4) 0.035(4) 0.025(3) 0.001(3) 0.009(3) -0.004(3)
O11 0.0186(19) 0.0188(19) 0.0106(18) -0.0008(15) 0.0042(15) -0.0078(16)
O12 0.072(5) 0.109(6) 0.046(4) 0.007(4) 0.007(4) 0.017(4)
O13 0.031(3) 0.023(3) 0.021(3) -0.003(3) 0.000(3) 0.003(3)
O14 0.033(4) 0.025(4) 0.028(3) 0.000(3) 0.002(3) 0.001(3)
O15 0.040(4) 0.027(4) 0.016(3) -0.004(3) 0.003(3) 0.005(3)
O16 0.049(4) 0.033(4) 0.011(3) -0.002(3) 0.001(3) 0.005(3)
O17 0.038(4) 0.041(4) 0.024(3) -0.003(3) 0.009(3) -0.004(3)
O18 0.040(4) 0.046(4) 0.012(3) -0.009(3) 0.001(3) 0.002(3)
O19 0.037(4) 0.020(3) 0.022(3) 0.000(3) 0.006(3) 0.003(3)
O20 0.050(4) 0.027(4) 0.024(3) -0.006(3) 0.017(3) -0.004(3)
O21 0.019(3) 0.014(3) 0.022(3) 0.004(2) 0.005(2) 0.000(2)
O22 0.020(3) 0.023(3) 0.021(3) 0.004(3) -0.004(2) -0.006(3)
N1 0.024(4) 0.031(5) 0.018(4) 0.001(3) 0.009(4) -0.002(4)
N2 0.080(6) 0.049(4) 0.027(4) -0.003(4) 0.003(4) 0.032(5)
O23 0.097(6) 0.128(7) 0.105(6) 0.022(5) 0.043(5) -0.010(5)
O24 0.073(6) 0.145(8) 0.097(6) 0.018(5) 0.015(5) -0.026(6)
C52 0.072(10) 0.096(11) 0.071(9) 0.015(8) 0.019(8) -0.019(8)
C53 0.091(11) 0.103(11) 0.089(10) -0.031(9) 0.003(9) 0.015(8)
C54 0.185(15) 0.103(11) 0.068(9) 0.004(8) -0.004(9) 0.030(10)
C55 0.165(15) 0.133(13) 0.114(11) 0.003(9) -0.003(10) 0.063(10)
C56 0.088(12) 0.178(16) 0.190(15) -0.081(12) 0.004(11) 0.016(11)
_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
Fe1 O22 1.953(4) . ?
Fe1 O21 1.998(4) . ?
Fe1 O15 2.004(5) . ?
Fe1 O3 2.005(5) . ?
Fe1 O14 2.021(5) . ?
Fe1 O5 2.046(5) . ?
Fe1 Fe4 2.9296(14) . ?
Fe2 O21 1.961(4) . ?
Fe2 O4 1.989(5) . ?
Fe2 O1 2.000(5) . ?
Fe2 O8 2.005(5) . ?
Fe2 O9 2.053(5) . ?
Fe2 N1 2.139(6) . ?
Fe3 O1 1.967(4) . ?
Fe3 O2 2.004(4) . ?
Fe3 O10 2.024(5) . ?
Fe3 O13 2.038(5) . ?
Fe3 O11 2.068(5) . ?
Fe3 O21 2.073(4) . ?
Fe4 O22 1.941(5) . ?
Fe4 O6 1.989(5) . ?
Fe4 O19 1.996(5) . ?
Fe4 O2 1.998(5) . ?
Fe4 O21 2.037(4) . ?
Fe4 O7 2.045(5) . ?
Fe5 O22 1.850(4) . ?
Fe5 O20 2.028(5) . ?
Fe5 O16 2.038(5) . ?
Fe5 O17 2.133(5) . ?
Fe5 O18 2.141(5) . ?
Fe5 Cl 2.337(2) . ?
Fe5 C42 2.499(9) . ?
C1 N1 1.476(9) . ?
C1 C2 1.495(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.519(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 O1 1.431(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.469(8) . ?
C4 N2 1.492(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.492(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 O2 1.413(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 O3 1.262(9) . ?
C7 O4 1.274(8) . ?
C7 C8 1.548(10) . ?
C8 C11A 1.489(14) . ?
C8 C9B 1.497(15) . ?
C8 C10B 1.527(18) . ?
C8 C11B 1.533(16) . ?
C8 C9A 1.543(14) . ?
C8 C10A 1.551(13) . ?
C9A H9A1 0.9600 . ?
C9A H9A2 0.9600 . ?
C9A H9A3 0.9600 . ?
C10A H10A 0.9600 . ?
C10A H10B 0.9600 . ?
C10A H10C 0.9600 . ?
C11A H11A 0.9600 . ?
C11A H11B 0.9600 . ?
C11A H11C 0.9600 . ?
C9B H9B1 0.9600 . ?
C9B H9B2 0.9600 . ?
C9B H9B3 0.9600 . ?
C10B H10D 0.9600 . ?
C10B H10E 0.9600 . ?
C10B H10F 0.9600 . ?
C11B H11D 0.9600 . ?
C11B H11E 0.9600 . ?
C11B H11F 0.9600 . ?
C12 O5 1.242(8) . ?
C12 O6 1.292(8) . ?
C12 C13 1.533(10) . ?
C13 C15 1.487(9) . ?
C13 C14 1.520(9) . ?
C13 C16 1.530(9) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O8 1.262(8) . ?
C17 O7 1.261(8) . ?
C17 C18 1.532(10) . ?
C18 C21 1.493(10) . ?
C18 C20 1.510(9) . ?
C18 C19 1.532(10) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O9 1.270(8) . ?
C22 O10 1.269(8) . ?
C22 C23 1.519(10) . ?
C23 C24B 1.456(13) . ?
C23 C25B 1.484(13) . ?
C23 C26A 1.474(15) . ?
C23 C24A 1.521(14) . ?
C23 C26B 1.573(14) . ?
C23 C25A 1.580(15) . ?
C24A H24A 0.9600 . ?
C24A H24B 0.9600 . ?
C24A H24C 0.9600 . ?
C25A H25A 0.9600 . ?
C25A H25B 0.9600 . ?
C25A H25C 0.9600 . ?
C26A H26A 0.9600 . ?
C26A H26B 0.9600 . ?
C26A H26C 0.9600 . ?
C24B H24D 0.9600 . ?
C24B H24E 0.9600 . ?
C24B H24F 0.9600 . ?
C25B H25D 0.9600 . ?
C25B H25E 0.9600 . ?
C25B H25F 0.9600 . ?
C26B H26D 0.9600 . ?
C26B H26E 0.9600 . ?
C26B H26F 0.9600 . ?
C27 O11 1.180(4) . ?
C27 O12 1.305(4) . ?
C27 C28 1.552(10) . ?
C28 C30 1.489(11) . ?
C28 C29 1.533(12) . ?
C28 C31 1.551(8) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 O14 1.265(8) . ?
C32 O13 1.281(8) . ?
C32 C33 1.517(10) . ?
C33 C34 1.481(10) . ?
C33 C35 1.506(10) . ?
C33 C36 1.521(10) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 O15 1.251(8) . ?
C37 O16 1.282(8) . ?
C37 C38 1.547(10) . ?
C38 C39 1.494(10) . ?
C38 C41 1.516(9) . ?
C38 C40 1.521(10) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 O18 1.265(8) . ?
C42 O17 1.267(7) . ?
C42 C43 1.530(10) . ?
C43 C46 1.501(10) . ?
C43 C44 1.535(10) . ?
C43 C45 1.521(9) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 O20 1.254(8) . ?
C47 O19 1.265(8) . ?
C47 C48 1.542(10) . ?
C48 C49 1.503(10) . ?
C48 C50 1.520(10) . ?
C48 C51 1.531(10) . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
N1 H1 0.86(2) . ?
N1 H2 0.85(2) . ?
O23 C52 1.344(7) . ?
O24 C52 1.182(7) . ?
C52 C53 1.506(13) . ?
C53 C54 1.542(13) . ?
C53 C56 1.541(8) . ?
C53 C55 1.550(8) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
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
O22 Fe1 O21 81.39(18) . . ?
O22 Fe1 O15 96.56(19) . . ?
O21 Fe1 O15 177.3(2) . . ?
O22 Fe1 O3 169.0(2) . . ?
O21 Fe1 O3 91.60(18) . . ?
O15 Fe1 O3 90.7(2) . . ?
O22 Fe1 O14 97.88(19) . . ?
O21 Fe1 O14 94.67(19) . . ?
O15 Fe1 O14 83.9(2) . . ?
O3 Fe1 O14 91.1(2) . . ?
O22 Fe1 O5 88.46(18) . . ?
O21 Fe1 O5 95.91(18) . . ?
O15 Fe1 O5 85.68(19) . . ?
O3 Fe1 O5 83.8(2) . . ?
O14 Fe1 O5 168.4(2) . . ?
O22 Fe1 Fe4 41.06(13) . . ?
O21 Fe1 Fe4 43.98(12) . . ?
O15 Fe1 Fe4 134.62(15) . . ?
O3 Fe1 Fe4 129.18(14) . . ?
O14 Fe1 Fe4 111.89(15) . . ?
O5 Fe1 Fe4 79.24(13) . . ?
O21 Fe2 O4 95.39(17) . . ?
O21 Fe2 O1 79.69(17) . . ?
O4 Fe2 O1 170.6(2) . . ?
O21 Fe2 O8 98.79(18) . . ?
O4 Fe2 O8 94.1(2) . . ?
O1 Fe2 O8 94.54(19) . . ?
O21 Fe2 O9 96.13(18) . . ?
O4 Fe2 O9 83.88(19) . . ?
O1 Fe2 O9 88.67(19) . . ?
O8 Fe2 O9 165.07(19) . . ?
O21 Fe2 N1 171.9(2) . . ?
O4 Fe2 N1 92.1(2) . . ?
O1 Fe2 N1 92.5(2) . . ?
O8 Fe2 N1 83.6(2) . . ?
O9 Fe2 N1 81.7(2) . . ?
O1 Fe3 O2 99.06(18) . . ?
O1 Fe3 O10 90.39(19) . . ?
O2 Fe3 O10 167.84(19) . . ?
O1 Fe3 O13 168.9(2) . . ?
O2 Fe3 O13 86.11(18) . . ?
O10 Fe3 O13 83.31(19) . . ?
O1 Fe3 O11 93.92(18) . . ?
O2 Fe3 O11 95.71(18) . . ?
O10 Fe3 O11 91.23(18) . . ?
O13 Fe3 O11 95.33(18) . . ?
O1 Fe3 O21 77.78(18) . . ?
O2 Fe3 O21 80.03(18) . . ?
O10 Fe3 O21 94.64(18) . . ?
O13 Fe3 O21 93.58(18) . . ?
O11 Fe3 O21 169.84(17) . . ?
O22 Fe4 O6 89.65(18) . . ?
O22 Fe4 O19 95.22(19) . . ?
O6 Fe4 O19 91.08(19) . . ?
O22 Fe4 O2 102.68(18) . . ?
O6 Fe4 O2 167.00(18) . . ?
O19 Fe4 O2 91.87(19) . . ?
O22 Fe4 O21 80.69(17) . . ?
O6 Fe4 O21 97.15(18) . . ?
O19 Fe4 O21 170.75(19) . . ?
O2 Fe4 O21 81.03(18) . . ?
O22 Fe4 O7 169.70(19) . . ?
O6 Fe4 O7 81.31(19) . . ?
O19 Fe4 O7 89.91(18) . . ?
O2 Fe4 O7 86.04(19) . . ?
O21 Fe4 O7 95.46(18) . . ?
O22 Fe4 Fe1 41.36(12) . . ?
O6 Fe4 Fe1 81.05(14) . . ?
O19 Fe4 Fe1 135.36(15) . . ?
O2 Fe4 Fe1 105.44(14) . . ?
O21 Fe4 Fe1 42.93(12) . . ?
O7 Fe4 Fe1 131.28(14) . . ?
O22 Fe5 O20 94.91(19) . . ?
O22 Fe5 O16 95.02(19) . . ?
O20 Fe5 O16 167.1(2) . . ?
O22 Fe5 O17 106.61(19) . . ?
O20 Fe5 O17 83.4(2) . . ?
O16 Fe5 O17 85.9(2) . . ?
O22 Fe5 O18 167.4(2) . . ?
O20 Fe5 O18 83.50(19) . . ?
O16 Fe5 O18 85.0(2) . . ?
O17 Fe5 O18 60.84(18) . . ?
O22 Fe5 Cl 101.28(15) . . ?
O20 Fe5 Cl 90.03(16) . . ?
O16 Fe5 Cl 96.07(16) . . ?
O17 Fe5 Cl 151.77(15) . . ?
O18 Fe5 Cl 91.20(15) . . ?
O22 Fe5 C42 137.0(2) . . ?
O20 Fe5 C42 81.3(2) . . ?
O16 Fe5 C42 85.9(2) . . ?
O17 Fe5 C42 30.47(19) . . ?
O18 Fe5 C42 30.41(18) . . ?
Cl Fe5 C42 121.4(2) . . ?
N1 C1 C2 111.4(6) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 C3 115.5(7) . . ?
C1 C2 H2A 108.4 . . ?
C3 C2 H2A 108.4 . . ?
C1 C2 H2B 108.4 . . ?
C3 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
O1 C3 C2 113.1(6) . . ?
O1 C3 H3A 109.0 . . ?
C2 C3 H3A 109.0 . . ?
O1 C3 H3B 109.0 . . ?
C2 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C5 C4 N2 117.6(8) . . ?
C5 C4 H4A 107.9 . . ?
N2 C4 H4A 107.9 . . ?
C5 C4 H4B 107.9 . . ?
N2 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
C4 C5 C6 117.6(8) . . ?
C4 C5 H5A 107.9 . . ?
C6 C5 H5A 107.9 . . ?
C4 C5 H5B 107.9 . . ?
C6 C5 H5B 107.9 . . ?
H5A C5 H5B 107.2 . . ?
O2 C6 C5 112.9(6) . . ?
O2 C6 H6A 109.0 . . ?
C5 C6 H6A 109.0 . . ?
O2 C6 H6B 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
O3 C7 O4 124.8(8) . . ?
O3 C7 C8 118.2(7) . . ?
O4 C7 C8 117.0(8) . . ?
C11A C8 C9B 134.5(12) . . ?
C11A C8 C10B 59.6(10) . . ?
C9B C8 C10B 112.0(13) . . ?
C11A C8 C11B 49.7(9) . . ?
C9B C8 C11B 107.4(13) . . ?
C10B C8 C11B 108.0(12) . . ?
C11A C8 C7 111.7(10) . . ?
C9B C8 C7 112.8(10) . . ?
C10B C8 C7 109.7(10) . . ?
C11B C8 C7 106.6(8) . . ?
C11A C8 C9A 114.8(13) . . ?
C10B C8 C9A 141.0(11) . . ?
C11B C8 C9A 70.5(11) . . ?
C7 C8 C9A 107.7(9) . . ?
C11A C8 C10A 108.2(12) . . ?
C9B C8 C10A 66.9(11) . . ?
C10B C8 C10A 51.2(9) . . ?
C11B C8 C10A 145.3(10) . . ?
C7 C8 C10A 106.9(8) . . ?
C9A C8 C10A 107.2(11) . . ?
C8 C9A H9A1 109.5 . . ?
C8 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C8 C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C8 C10A H10A 109.5 . . ?
C8 C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C8 C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C8 C11A H11A 109.5 . . ?
C8 C11A H11B 109.5 . . ?
H11A C11A H11B 109.5 . . ?
C8 C11A H11C 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
C8 C9B H9B1 109.5 . . ?
C8 C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C8 C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C8 C10B H10D 109.5 . . ?
C8 C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C8 C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C8 C11B H11D 109.5 . . ?
C8 C11B H11E 109.5 . . ?
H11D C11B H11E 109.5 . . ?
C8 C11B H11F 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
O5 C12 O6 124.1(8) . . ?
O5 C12 C13 119.9(8) . . ?
O6 C12 C13 116.0(7) . . ?
C15 C13 C14 109.4(7) . . ?
C15 C13 C12 111.1(7) . . ?
C14 C13 C12 109.3(6) . . ?
C15 C13 C16 110.9(7) . . ?
C14 C13 C16 108.8(7) . . ?
C12 C13 C16 107.3(6) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O8 C17 O7 123.7(7) . . ?
O8 C17 C18 119.4(7) . . ?
O7 C17 C18 116.9(7) . . ?
C21 C18 C20 109.6(7) . . ?
C21 C18 C17 108.3(7) . . ?
C20 C18 C17 111.5(6) . . ?
C21 C18 C19 111.5(7) . . ?
C20 C18 C19 108.7(7) . . ?
C17 C18 C19 107.2(6) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O9 C22 O10 126.0(7) . . ?
O9 C22 C23 117.5(7) . . ?
O10 C22 C23 116.4(7) . . ?
C24B C23 C25B 119.7(12) . . ?
C24B C23 C26A 133.8(12) . . ?
C25B C23 C26A 45.8(10) . . ?
C24B C23 C22 111.4(9) . . ?
C25B C23 C22 112.4(9) . . ?
C26A C23 C22 114.2(10) . . ?
C25B C23 C24A 134.7(11) . . ?
C26A C23 C24A 114.3(13) . . ?
C22 C23 C24A 112.7(10) . . ?
C24B C23 C26B 104.9(12) . . ?
C25B C23 C26B 101.2(11) . . ?
C26A C23 C26B 56.0(11) . . ?
C22 C23 C26B 105.3(9) . . ?
C24A C23 C26B 69.3(10) . . ?
C24B C23 C25A 69.8(11) . . ?
C25B C23 C25A 62.1(10) . . ?
C26A C23 C25A 106.7(14) . . ?
C22 C23 C25A 102.3(9) . . ?
C24A C23 C25A 105.2(11) . . ?
C26B C23 C25A 151.8(11) . . ?
C23 C24A H24A 109.5 . . ?
C23 C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C23 C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C23 C25A H25A 109.5 . . ?
C23 C25A H25B 109.5 . . ?
H25A C25A H25B 109.5 . . ?
C23 C25A H25C 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
C23 C26A H26A 109.5 . . ?
C23 C26A H26B 109.5 . . ?
H26A C26A H26B 109.5 . . ?
C23 C26A H26C 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C23 C24B H24D 109.5 . . ?
C23 C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C23 C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C23 C25B H25D 109.5 . . ?
C23 C25B H25E 109.5 . . ?
H25D C25B H25E 109.5 . . ?
C23 C25B H25F 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
C23 C26B H26D 109.5 . . ?
C23 C26B H26E 109.5 . . ?
H26D C26B H26E 109.5 . . ?
C23 C26B H26F 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
O11 C27 O12 128.5(8) . . ?
O11 C27 C28 116.1(7) . . ?
O12 C27 C28 115.4(6) . . ?
C30 C28 C29 104.1(9) . . ?
C30 C28 C27 111.3(8) . . ?
C29 C28 C27 110.0(7) . . ?
C30 C28 C31 109.2(9) . . ?
C29 C28 C31 112.5(9) . . ?
C27 C28 C31 109.7(8) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O14 C32 O13 122.9(8) . . ?
O14 C32 C33 119.3(7) . . ?
O13 C32 C33 117.7(8) . . ?
C34 C33 C32 110.8(7) . . ?
C34 C33 C35 110.8(8) . . ?
C32 C33 C35 110.3(7) . . ?
C34 C33 C36 110.2(7) . . ?
C32 C33 C36 105.9(6) . . ?
C35 C33 C36 108.7(7) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O15 C37 O16 125.0(7) . . ?
O15 C37 C38 119.2(7) . . ?
O16 C37 C38 115.7(7) . . ?
C39 C38 C41 112.2(7) . . ?
C39 C38 C40 108.9(7) . . ?
C41 C38 C40 108.7(7) . . ?
C39 C38 C37 109.2(7) . . ?
C41 C38 C37 110.0(7) . . ?
C40 C38 C37 107.7(7) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O18 C42 O17 117.5(8) . . ?
O18 C42 C43 122.6(7) . . ?
O17 C42 C43 119.9(8) . . ?
O18 C42 Fe5 59.0(4) . . ?
O17 C42 Fe5 58.6(4) . . ?
C43 C42 Fe5 174.6(6) . . ?
C46 C43 C42 113.0(7) . . ?
C46 C43 C44 108.4(7) . . ?
C42 C43 C44 104.9(6) . . ?
C46 C43 C45 109.2(7) . . ?
C42 C43 C45 109.5(7) . . ?
C44 C43 C45 111.9(7) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O20 C47 O19 126.0(8) . . ?
O20 C47 C48 118.0(7) . . ?
O19 C47 C48 115.8(7) . . ?
C49 C48 C50 109.8(7) . . ?
C49 C48 C51 109.7(7) . . ?
C50 C48 C51 110.7(7) . . ?
C49 C48 C47 109.8(7) . . ?
C50 C48 C47 105.7(7) . . ?
C51 C48 C47 111.1(7) . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C3 O1 Fe3 131.4(4) . . ?
C3 O1 Fe2 129.0(4) . . ?
Fe3 O1 Fe2 98.5(2) . . ?
C6 O2 Fe4 121.7(4) . . ?
C6 O2 Fe3 123.7(4) . . ?
Fe4 O2 Fe3 101.3(2) . . ?
C7 O3 Fe1 124.0(5) . . ?
C7 O4 Fe2 125.1(5) . . ?
C12 O5 Fe1 127.8(5) . . ?
C12 O6 Fe4 127.1(5) . . ?
C17 O7 Fe4 127.7(5) . . ?
C17 O8 Fe2 129.3(5) . . ?
C22 O9 Fe2 127.1(5) . . ?
C22 O10 Fe3 127.6(5) . . ?
C27 O11 Fe3 131.0(5) . . ?
C32 O13 Fe3 126.9(5) . . ?
C32 O14 Fe1 130.8(5) . . ?
C37 O15 Fe1 130.4(5) . . ?
C37 O16 Fe5 125.1(5) . . ?
C42 O17 Fe5 90.9(5) . . ?
C42 O18 Fe5 90.6(4) . . ?
C47 O19 Fe4 129.3(5) . . ?
C47 O20 Fe5 131.4(5) . . ?
Fe2 O21 Fe1 124.1(2) . . ?
Fe2 O21 Fe4 121.1(2) . . ?
Fe1 O21 Fe4 93.09(17) . . ?
Fe2 O21 Fe3 96.28(17) . . ?
Fe1 O21 Fe3 123.5(2) . . ?
Fe4 O21 Fe3 97.65(18) . . ?
Fe5 O22 Fe4 130.7(2) . . ?
Fe5 O22 Fe1 125.9(2) . . ?
Fe4 O22 Fe1 97.58(19) . . ?
C1 N1 Fe2 117.0(5) . . ?
C1 N1 H1 94(5) . . ?
Fe2 N1 H1 120(5) . . ?
C1 N1 H2 108(5) . . ?
Fe2 N1 H2 100(5) . . ?
H1 N1 H2 118(7) . . ?
O24 C52 O23 127.2(11) . . ?
O24 C52 C53 115.5(10) . . ?
O23 C52 C53 117.2(9) . . ?
C52 C53 C54 113.3(10) . . ?
C52 C53 C56 108.1(10) . . ?
C54 C53 C56 106.9(11) . . ?
C52 C53 C55 108.2(10) . . ?
C54 C53 C55 110.4(10) . . ?
C56 C53 C55 109.9(10) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full 25.08
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max 0.731
_refine_diff_density_min -0.523
_refine_diff_density_rms 0.098
# start Validation Reply Form
_vrf_PLAT220_ck43
;
RESPONSE: This is due to the disorder of the t-butyl groups of
two pivalic ligands of the complex.
;
_vrf_PLAT026_ck43
;
RESPONSE: Several crystals of the title compound were carefully
tested on the X-rays at 100 K. The diffraction quality of the
crystals has proven to be moderate and structure determination was
eventually carried out by means of the best data set collected.
As a necessary compromise between resolution and data completeness
we have used data up to 50 degrees with a completeness of 99.4%.
The structure was refined as a non-merohedral twin with a 88:12
domain ratio and the quality of the final analysis is certainly
not as good as from an equivalent single crystal.
;
_vrf_PLAT430_ck43
;
RESPONSE: Those short distances (O12...O23 and O24...N2) assume strong
hydrogen-bonding; however, the H-atoms attached to the relevant atoms
have not been located in the course of the X-ray analysis.
;
_vrf_PLAT309_ck43
;
RESPONSE: See above.
;
_vrf_PLAT731_ck43
;
RESPONSE: This distance has been restrainted by means of a DFIX
instruction.
;
_vrf_PLAT041_ck43
;
RESPONSE: The missing (not located by a difference synthesis) H-atoms
of the monodentate and lattice pivalic molecules as well as those of
the N2 amino group have been included in the sum and moiety formula and
the Mr, Dx and F(000) have been modified accordingly.
These modifications account for the differences detected in the relevant
data items.
;
_vrf_FORMU01_ck43
;
RESPONSE: See Response for PLAT041_ALERT 1 C
;
# end Validation Reply Form