# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Guillet, Gary'
'Sloane, Forrest'
'Abboud, Khalil'
'Murray, Leslie'

_publ_contact_author_name        'Murray, Leslie'
_publ_contact_author_email       murray@chem.ufl.edu

_publ_section_title              
;
Synthesis and characterization of a
tris(2-hydroxyphenyl)methane-based cryptand and its triiron(III) complex
;

# Attachment '- Cryptand.cif'

data_gui10
_database_code_depnum_ccdc_archive 'CCDC 866977'
#TrackingRef '- Cryptand.cif'

_audit_update_record             
;
2011-10-18 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C101 H129 N9 O17'
_chemical_formula_weight         1741.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.9708(2)
_cell_length_b                   19.0228(3)
_cell_length_c                   19.2837(3)
_cell_angle_alpha                73.327(1)
_cell_angle_beta                 67.465(1)
_cell_angle_gamma                66.260(1)
_cell_volume                     5504.66(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6065
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      67.66

_exptl_crystal_description       needles
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1868
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8635
_exptl_absorpt_correction_T_max  0.9891
_exptl_absorpt_process_details   
'based on measured indexed crystal faces, Bruker SHELXTL v6.14 (Bruker 2008)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'I\mS microsource'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        <1
_diffrn_reflns_number            67204
_diffrn_reflns_av_R_equivalents  0.0957
_diffrn_reflns_av_sigmaI/netI    0.1084
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         66.50
_reflns_number_total             18677
_reflns_number_gt                9470
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_cell_refinement       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
All H atoms were positioned geometrically ( C---H = 0.93/1.00 \%A) and allowed
to ride with <i>U</i>~iso~(H)= 1.2/1.5<i>U</i>~eq~(C).
Methyl ones were allowed to rotate around the corresponding C---C.

. The molecule has two disordered parts. O5 and O5? are refined with their site
occupation factors constrained to add to one. The isopropyl group on C29 is
also disordered and refined similarly. The asymmetric unit consists of the
molecule, three thf, two water solvent molecules and three pentane solvent
molecules. The pentane molecules are disordered in a channel and could not be
modeled properly, thus program SQUEEZE, a part of the PLATON package of
crystallographic software, was used to calculate the solvent disorder area and
remove its contribution to the overall intensity data. All amino protons we
obtained from a Difference Fourier map and refined freely. The water protons
were also obtained from a Difference Fourier map, but were refined riding on
their parent O atoms. Two of the three thf solvent molecules are disordered.
The O14 molecule has all C and H atoms disordered while the O15 molecule is
wholly disordered. In each case, the disorder was refined in two parts with
their site occupations factors dependently refined.
;

_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^)+(0.0809P)^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         18677
_refine_ls_number_parameters     1173
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1609
_refine_ls_wR_factor_gt          0.1448
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_restrained_S_all      0.842
_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
O1 O 0.77141(18) 1.55922(17) -0.22671(16) 0.0740(8) Uani 1 1 d . . .
O2 O 1.16013(16) 1.47590(12) -0.51680(12) 0.0507(6) Uani 1 1 d . . .
O3 O 1.37411(13) 1.10028(11) -0.49552(12) 0.0422(5) Uani 1 1 d . . .
O4 O 0.51190(15) 1.40562(13) -0.24149(13) 0.0559(6) Uani 1 1 d . . .
O5 O 0.7668(2) 1.01109(19) -0.10526(19) 0.0413(13) Uiso 0.695(10) 1 d P A 1
O5' O 0.7191(7) 1.0404(5) -0.0785(5) 0.063(3) Uiso 0.305(10) 1 d P A 2
O6 O 0.99777(16) 1.15126(16) 0.00578(12) 0.0617(7) Uani 1 1 d . A .
O7 O 1.35437(16) 1.14051(15) -0.26791(13) 0.0590(6) Uani 1 1 d . . .
O8 O 0.58221(14) 1.23260(12) -0.36028(12) 0.0482(5) Uani 1 1 d . . .
O9 O 0.92106(18) 1.22152(14) -0.67996(14) 0.0679(7) Uani 1 1 d . . .
O10 O 1.18654(15) 0.89977(11) -0.50131(12) 0.0499(6) Uani 1 1 d . . .
O11 O 1.30798(13) 0.95661(11) -0.26199(11) 0.0376(5) Uani 1 1 d . . .
O12 O 0.60649(14) 1.45128(11) -0.47010(12) 0.0415(5) Uani 1 1 d . . .
N1 N 0.80062(19) 1.48928(16) -0.31829(16) 0.0422(6) Uani 1 1 d . . .
H1 H 0.835(2) 1.4753(17) -0.3558(18) 0.029(8) Uiso 1 1 d . . .
N2 N 0.96297(17) 1.49873(13) -0.37525(14) 0.0405(6) Uani 1 1 d . . .
N3 N 1.11565(18) 1.38071(14) -0.42653(16) 0.0408(6) Uani 1 1 d . . .
H3 H 1.077(3) 1.377(2) -0.383(3) 0.078(14) Uiso 1 1 d . . .
N4 N 0.77119(17) 1.13313(16) -0.15844(14) 0.0439(7) Uani 1 1 d . A .
H4 H 0.785(3) 1.169(2) -0.152(2) 0.079(13) Uiso 1 1 d . . .
N5 N 0.87442(16) 1.10409(14) -0.06787(14) 0.0406(6) Uani 1 1 d . . .
N6 N 1.02308(17) 1.13478(16) -0.11480(14) 0.0425(6) Uani 1 1 d . A .
H6 H 1.007(2) 1.116(2) -0.137(2) 0.056(10) Uiso 1 1 d . . .
N7 N 0.91473(17) 1.21512(13) -0.55789(15) 0.0374(6) Uani 1 1 d . . .
H7 H 0.934(2) 1.1857(19) -0.521(2) 0.048(9) Uiso 1 1 d . . .
N8 N 1.04271(16) 1.07500(13) -0.56663(13) 0.0365(6) Uani 1 1 d . . .
N9 N 1.11832(17) 1.01422(14) -0.45524(14) 0.0375(6) Uani 1 1 d . . .
H9 H 1.0852(19) 1.0619(18) -0.4616(16) 0.032(8) Uiso 1 1 d . . .
C1 C 0.8173(2) 1.53348(18) -0.2870(2) 0.0482(8) Uani 1 1 d . . .
C2 C 0.8999(2) 1.54906(17) -0.32844(19) 0.0454(8) Uani 1 1 d . . .
C3 C 0.9096(2) 1.61213(18) -0.3153(2) 0.0544(9) Uani 1 1 d . . .
H3A H 0.8652 1.6445 -0.2803 0.065 Uiso 1 1 calc R . .
C4 C 0.9860(2) 1.62696(19) -0.3547(2) 0.0577(9) Uani 1 1 d . . .
H4A H 0.9945 1.6701 -0.3473 0.069 Uiso 1 1 calc R . .
C5 C 1.0493(2) 1.57845(18) -0.4046(2) 0.0515(9) Uani 1 1 d . . .
H5A H 1.1009 1.5891 -0.4337 0.062 Uiso 1 1 calc R . .
C6 C 1.0366(2) 1.51338(16) -0.41178(18) 0.0414(7) Uani 1 1 d . . .
C7 C 1.1097(2) 1.45520(17) -0.45835(17) 0.0401(7) Uani 1 1 d . . .
C8 C 1.18232(19) 1.31220(16) -0.44890(17) 0.0366(7) Uani 1 1 d . . .
C9 C 1.19078(19) 1.24601(16) -0.39307(16) 0.0362(7) Uani 1 1 d . . .
H9A H 1.1519 1.2494 -0.3431 0.043 Uiso 1 1 calc R . .
C10 C 1.25405(19) 1.17605(15) -0.40870(16) 0.0340(6) Uani 1 1 d . . .
C11 C 1.30997(19) 1.17102(16) -0.48267(17) 0.0369(7) Uani 1 1 d . . .
C12 C 1.3056(2) 1.23713(17) -0.53930(17) 0.0401(7) Uani 1 1 d . . .
C13 C 1.2402(2) 1.30692(17) -0.52130(17) 0.0401(7) Uani 1 1 d . . .
H13A H 1.2353 1.3516 -0.5595 0.048 Uiso 1 1 calc R . .
C14 C 1.26631(19) 1.10572(16) -0.34601(16) 0.0356(6) Uani 1 1 d . A .
H14A H 1.3290 1.0821 -0.3532 0.043 Uiso 1 1 calc R . .
C15 C 1.3674(2) 1.05831(18) -0.54355(19) 0.0466(8) Uani 1 1 d . . .
H15A H 1.3931 1.0770 -0.5977 0.056 Uiso 1 1 calc R . .
H15B H 1.3067 1.0668 -0.5350 0.056 Uiso 1 1 calc R . .
C16 C 1.4140(3) 0.9733(2) -0.5238(2) 0.0608(10) Uani 1 1 d . . .
H16A H 1.4142 0.9442 -0.5583 0.091 Uiso 1 1 calc R . .
H16B H 1.3853 0.9544 -0.4713 0.091 Uiso 1 1 calc R . .
H16C H 1.4729 0.9660 -0.5289 0.091 Uiso 1 1 calc R . .
C17 C 1.3718(2) 1.2347(2) -0.61656(19) 0.0554(9) Uani 1 1 d . . .
H17A H 1.4163 1.1821 -0.6153 0.066 Uiso 1 1 calc R . .
C18 C 1.4157(3) 1.2943(3) -0.6336(3) 0.0956(16) Uani 1 1 d . . .
H18A H 1.4448 1.2824 -0.5958 0.143 Uiso 1 1 calc R . .
H18B H 1.3729 1.3464 -0.6315 0.143 Uiso 1 1 calc R . .
H18C H 1.4574 1.2924 -0.6844 0.143 Uiso 1 1 calc R . .
C19 C 1.3329(3) 1.2440(3) -0.6778(2) 0.0928(14) Uani 1 1 d . . .
H19A H 1.3027 1.2065 -0.6628 0.139 Uiso 1 1 calc R . .
H19B H 1.3784 1.2346 -0.7260 0.139 Uiso 1 1 calc R . .
H19C H 1.2927 1.2969 -0.6838 0.139 Uiso 1 1 calc R . .
C20 C 0.7269(2) 1.46744(17) -0.29441(17) 0.0410(7) Uani 1 1 d . . .
C21 C 0.7286(2) 1.41479(16) -0.33295(16) 0.0366(7) Uani 1 1 d . . .
H21A H 0.7785 1.3945 -0.3726 0.044 Uiso 1 1 calc R . .
C22 C 0.6576(2) 1.39150(16) -0.31386(17) 0.0390(7) Uani 1 1 d . . .
C23 C 0.5844(2) 1.42429(18) -0.25624(18) 0.0448(8) Uani 1 1 d . . .
C24 C 0.5815(2) 1.47764(18) -0.21822(19) 0.0499(8) Uani 1 1 d . B .
C25 C 0.6536(2) 1.49863(19) -0.23761(18) 0.0492(8) Uani 1 1 d . . .
H25A H 0.6527 1.5347 -0.2117 0.059 Uiso 1 1 calc R . .
C26 C 0.6576(2) 1.33452(17) -0.35540(17) 0.0393(7) Uani 1 1 d . A .
H26A H 0.5982 1.3521 -0.3581 0.047 Uiso 1 1 calc R . .
C27 C 0.4978(2) 1.3438(2) -0.1793(2) 0.0600(9) Uani 1 1 d . . .
H27A H 0.4777 1.3622 -0.1300 0.072 Uiso 1 1 calc R . .
H27B H 0.5514 1.2991 -0.1819 0.072 Uiso 1 1 calc R . .
C28 C 0.4307(3) 1.3202(3) -0.1870(3) 0.0876(14) Uani 1 1 d . . .
H28A H 0.4180 1.2791 -0.1449 0.131 Uiso 1 1 calc R . .
H28B H 0.4521 1.3010 -0.2354 0.131 Uiso 1 1 calc R . .
H28C H 0.3786 1.3654 -0.1857 0.131 Uiso 1 1 calc R . .
C29 C 0.5001(3) 1.5167(2) -0.1599(2) 0.0675(10) Uani 1 1 d . . .
H29A H 0.4726 1.4764 -0.1292 0.081 Uiso 0.538(10) 1 calc PR B 1
H29B H 0.4588 1.4923 -0.1568 0.081 Uiso 0.462(10) 1 d PR B 2
C30 C 0.5206(4) 1.5494(4) -0.1009(4) 0.056(2) Uiso 0.538(10) 1 d P B 1
H30A H 0.5636 1.5075 -0.0796 0.083 Uiso 0.538(10) 1 calc PR B 1
H30B H 0.4681 1.5674 -0.0597 0.083 Uiso 0.538(10) 1 calc PR B 1
H30C H 0.5422 1.5927 -0.1285 0.083 Uiso 0.538(10) 1 calc PR B 1
C31 C 0.4404(4) 1.5782(4) -0.1921(4) 0.0456(19) Uiso 0.538(10) 1 d P B 1
H31A H 0.4305 1.5601 -0.2295 0.068 Uiso 0.538(10) 1 calc PR B 1
H31B H 0.4628 1.6214 -0.2172 0.068 Uiso 0.538(10) 1 calc PR B 1
H31C H 0.3866 1.5957 -0.1521 0.068 Uiso 0.538(10) 1 calc PR B 1
C30' C 0.4995(6) 1.5059(6) -0.0894(6) 0.074(3) Uiso 0.462(10) 1 d P B 2
H30D H 0.5101 1.4507 -0.0680 0.111 Uiso 0.462(10) 1 calc PR B 2
H30E H 0.4438 1.5367 -0.0594 0.111 Uiso 0.462(10) 1 calc PR B 2
H30F H 0.5442 1.5222 -0.0883 0.111 Uiso 0.462(10) 1 calc PR B 2
C31' C 0.4581(7) 1.6062(7) -0.1973(6) 0.074(3) Uiso 0.462(10) 1 d P B 2
H31D H 0.4574 1.6070 -0.2481 0.111 Uiso 0.462(10) 1 calc PR B 2
H31E H 0.4921 1.6374 -0.2012 0.111 Uiso 0.462(10) 1 calc PR B 2
H31F H 0.3995 1.6280 -0.1651 0.111 Uiso 0.462(10) 1 calc PR B 2
C32 C 0.7775(2) 1.07225(19) -0.10402(18) 0.0475(8) Uani 1 1 d . . .
C33 C 0.8126(2) 1.07322(17) -0.04512(17) 0.0413(7) Uani 1 1 d . A .
C34 C 0.7803(2) 1.04049(18) 0.02956(18) 0.0474(8) Uani 1 1 d . . .
H34A H 0.7365 1.0187 0.0430 0.057 Uiso 1 1 calc R A .
C35 C 0.8130(2) 1.04031(19) 0.08346(18) 0.0498(8) Uani 1 1 d . A .
H35A H 0.7914 1.0195 0.1352 0.060 Uiso 1 1 calc R . .
C36 C 0.8780(2) 1.0711(2) 0.06082(17) 0.0505(8) Uani 1 1 d . . .
H36A H 0.9024 1.0713 0.0967 0.061 Uiso 1 1 calc R A .
C37 C 0.9070(2) 1.10171(18) -0.01475(16) 0.0415(7) Uani 1 1 d . A .
C38 C 0.9799(2) 1.13223(19) -0.04037(18) 0.0462(8) Uani 1 1 d . . .
C39 C 1.10350(19) 1.14521(16) -0.15346(16) 0.0374(7) Uani 1 1 d . . .
C40 C 1.14220(19) 1.12849(16) -0.22638(16) 0.0364(7) Uani 1 1 d . A .
H40A H 1.1116 1.1163 -0.2495 0.044 Uiso 1 1 calc R . .
C41 C 1.22436(19) 1.12888(15) -0.26714(16) 0.0359(7) Uani 1 1 d . . .
C42 C 1.2679(2) 1.14883(18) -0.23311(17) 0.0428(8) Uani 1 1 d . A .
C43 C 1.2292(2) 1.16802(18) -0.16000(17) 0.0450(8) Uani 1 1 d . . .
C44 C 1.1462(2) 1.16648(18) -0.11966(18) 0.0463(8) Uani 1 1 d . A .
H44A H 1.1191 1.1797 -0.0699 0.056 Uiso 1 1 calc R . .
C45 C 1.3810(3) 1.1940(2) -0.3304(2) 0.0645(10) Uani 1 1 d . . .
H45A H 1.3749 1.1853 -0.3759 0.077 Uiso 1 1 calc R . .
H45B H 1.4422 1.1847 -0.3402 0.077 Uiso 1 1 calc R . .
C46 C 1.3329(3) 1.2733(2) -0.3190(2) 0.0729(11) Uani 1 1 d . . .
H46A H 1.3537 1.3083 -0.3642 0.109 Uiso 1 1 calc R . .
H46B H 1.3399 1.2826 -0.2748 0.109 Uiso 1 1 calc R . .
H46C H 1.2723 1.2831 -0.3102 0.109 Uiso 1 1 calc R . .
C47 C 1.2766(3) 1.1896(2) -0.1223(2) 0.058(1) Uani 1 1 d . A .
H47A H 1.3304 1.1954 -0.1618 0.070 Uiso 1 1 calc R . .
C48 C 1.3016(3) 1.1248(3) -0.0594(2) 0.0879(16) Uani 1 1 d . . .
H48A H 1.3362 1.0762 -0.0803 0.132 Uiso 1 1 calc R A .
H48B H 1.2500 1.1182 -0.0194 0.132 Uiso 1 1 calc R . .
H48C H 1.3348 1.1380 -0.0380 0.132 Uiso 1 1 calc R . .
C49 C 1.2239(3) 1.2676(3) -0.0936(3) 0.0943(16) Uani 1 1 d . . .
H49A H 1.2076 1.3075 -0.1354 0.141 Uiso 1 1 calc R A .
H49B H 1.2579 1.2826 -0.0746 0.141 Uiso 1 1 calc R . .
H49C H 1.1723 1.2627 -0.0524 0.141 Uiso 1 1 calc R . .
C50 C 0.7275(2) 1.15408(17) -0.21271(17) 0.0412(7) Uani 1 1 d . . .
C51 C 0.7195(2) 1.22662(17) -0.25861(17) 0.0401(7) Uani 1 1 d . A .
H51A H 0.7468 1.2586 -0.2551 0.048 Uiso 1 1 calc R . .
C52 C 0.6729(2) 1.25293(17) -0.30913(17) 0.0395(7) Uani 1 1 d . . .
C53 C 0.6341(2) 1.20376(17) -0.31377(18) 0.0422(7) Uani 1 1 d . A .
C54 C 0.6416(2) 1.13154(18) -0.26890(19) 0.0466(8) Uani 1 1 d . . .
C55 C 0.6879(2) 1.10717(18) -0.21833(19) 0.0474(8) Uani 1 1 d . A .
H55A H 0.6928 1.0578 -0.1870 0.057 Uiso 1 1 calc R . .
C56 C 0.6227(2) 1.2100(2) -0.4345(2) 0.0548(9) Uani 1 1 d . . .
H56A H 0.6322 1.1543 -0.4309 0.066 Uiso 1 1 calc R . .
H56B H 0.6786 1.2186 -0.4579 0.066 Uiso 1 1 calc R . .
C57 C 0.5648(4) 1.2588(4) -0.4808(3) 0.1107(19) Uani 1 1 d . . .
H57A H 0.5916 1.2469 -0.5328 0.166 Uiso 1 1 calc R . .
H57B H 0.5538 1.3139 -0.4819 0.166 Uiso 1 1 calc R . .
H57C H 0.5108 1.2480 -0.4584 0.166 Uiso 1 1 calc R . .
C58 C 0.5962(3) 1.0795(2) -0.2710(2) 0.0606(11) Uani 1 1 d . A .
H58A H 0.5623 1.1083 -0.3073 0.073 Uiso 1 1 calc R . .
C59 C 0.5336(3) 1.0641(3) -0.1922(3) 0.0854(15) Uani 1 1 d . . .
H59A H 0.5018 1.0341 -0.1950 0.128 Uiso 1 1 calc R A .
H59B H 0.4936 1.1138 -0.1757 0.128 Uiso 1 1 calc R . .
H59C H 0.5654 1.0347 -0.1557 0.128 Uiso 1 1 calc R . .
C60 C 0.6597(3) 1.0047(2) -0.2996(3) 0.0746(13) Uani 1 1 d . . .
H60A H 0.6986 1.0168 -0.3497 0.112 Uiso 1 1 calc R A .
H60B H 0.6290 0.9743 -0.3038 0.112 Uiso 1 1 calc R . .
H60C H 0.6924 0.9744 -0.2640 0.112 Uiso 1 1 calc R . .
C61 C 0.9461(2) 1.18679(17) -0.62402(18) 0.0438(8) Uani 1 1 d . . .
C62 C 1.0119(2) 1.10791(17) -0.62612(17) 0.0396(7) Uani 1 1 d . . .
C63 C 1.0375(2) 1.07098(18) -0.68798(18) 0.0440(7) Uani 1 1 d . . .
H63A H 1.0154 1.0967 -0.7295 0.053 Uiso 1 1 calc R . .
C64 C 1.0950(2) 0.99712(18) -0.68845(18) 0.0467(8) Uani 1 1 d . . .
H64A H 1.1122 0.9703 -0.7296 0.056 Uiso 1 1 calc R . .
C65 C 1.1276(2) 0.96222(17) -0.62788(17) 0.0439(7) Uani 1 1 d . . .
H65A H 1.1681 0.9112 -0.6269 0.053 Uiso 1 1 calc R . .
C66 C 1.0998(2) 1.00331(16) -0.56866(16) 0.0370(7) Uani 1 1 d . . .
C67 C 1.1387(2) 0.96665(16) -0.50461(17) 0.0385(7) Uani 1 1 d . . .
C68 C 1.16350(19) 0.99740(16) -0.40208(16) 0.0362(7) Uani 1 1 d . . .
C69 C 1.18700(18) 1.05631(16) -0.39718(16) 0.0350(6) Uani 1 1 d . A .
H69A H 1.1688 1.1066 -0.4253 0.042 Uiso 1 1 calc R . .
C70 C 1.23700(18) 1.04248(16) -0.35148(16) 0.0342(6) Uani 1 1 d . . .
C71 C 1.26052(19) 0.96850(16) -0.30965(16) 0.0351(6) Uani 1 1 d . A .
C72 C 1.2337(2) 0.90950(16) -0.31026(17) 0.0380(7) Uani 1 1 d . . .
C73 C 1.1853(2) 0.92518(16) -0.35862(16) 0.0383(7) Uani 1 1 d . A .
H73A H 1.1673 0.8857 -0.3614 0.046 Uiso 1 1 calc R . .
C74 C 1.3987(2) 0.92241(19) -0.29411(19) 0.0455(7) Uani 1 1 d . . .
H74A H 1.4190 0.9520 -0.3447 0.055 Uiso 1 1 calc R . .
H74B H 1.4132 0.8680 -0.3001 0.055 Uiso 1 1 calc R . .
C75 C 1.4395(3) 0.9248(3) -0.2409(2) 0.0711(11) Uani 1 1 d . . .
H75A H 1.5016 0.9014 -0.2608 0.107 Uiso 1 1 calc R . .
H75B H 1.4184 0.8958 -0.1909 0.107 Uiso 1 1 calc R . .
H75C H 1.4253 0.9790 -0.2360 0.107 Uiso 1 1 calc R . .
C76 C 1.2565(2) 0.82996(17) -0.26184(18) 0.0474(8) Uani 1 1 d . A .
H76A H 1.2846 0.8325 -0.2272 0.057 Uiso 1 1 calc R . .
C77 C 1.1779(3) 0.8068(2) -0.2127(2) 0.0612(10) Uani 1 1 d . . .
H77A H 1.1364 0.8481 -0.1829 0.092 Uiso 1 1 calc R A .
H77B H 1.1947 0.7584 -0.1782 0.092 Uiso 1 1 calc R . .
H77C H 1.1522 0.7992 -0.2453 0.092 Uiso 1 1 calc R . .
C78 C 1.3193(3) 0.76889(18) -0.3108(2) 0.0626(10) Uani 1 1 d . . .
H78A H 1.3704 0.7834 -0.3408 0.094 Uiso 1 1 calc R A .
H78B H 1.2931 0.7649 -0.3451 0.094 Uiso 1 1 calc R . .
H78C H 1.3352 0.7186 -0.2784 0.094 Uiso 1 1 calc R . .
C79 C 0.83981(19) 1.27820(16) -0.53755(17) 0.0362(7) Uani 1 1 d . . .
C80 C 0.7920(2) 1.27836(16) -0.46057(17) 0.0370(7) Uani 1 1 d . A .
H80A H 0.8127 1.2375 -0.4236 0.044 Uiso 1 1 calc R . .
C81 C 0.71512(19) 1.33668(16) -0.43719(16) 0.0365(7) Uani 1 1 d . . .
C82 C 0.68652(19) 1.39766(16) -0.49270(17) 0.0366(7) Uani 1 1 d . A .
C83 C 0.7342(2) 1.39911(16) -0.56989(17) 0.0372(7) Uani 1 1 d . . .
C84 C 0.8104(2) 1.33983(16) -0.59154(17) 0.0384(7) Uani 1 1 d . A .
H84A H 0.8433 1.3409 -0.6437 0.046 Uiso 1 1 calc R . .
C85 C 0.6023(2) 1.52480(17) -0.45992(19) 0.0482(8) Uani 1 1 d . . .
H85A H 0.6148 1.5586 -0.5096 0.058 Uiso 1 1 calc R . .
H85B H 0.6441 1.5173 -0.4346 0.058 Uiso 1 1 calc R . .
C86 C 0.5134(3) 1.5604(2) -0.4115(2) 0.0625(10) Uani 1 1 d . . .
H86A H 0.5068 1.6113 -0.4032 0.094 Uiso 1 1 calc R . .
H86B H 0.5022 1.5264 -0.3625 0.094 Uiso 1 1 calc R . .
H86C H 0.4728 1.5667 -0.4371 0.094 Uiso 1 1 calc R . .
C87 C 0.7033(2) 1.46380(17) -0.63123(17) 0.0434(7) Uani 1 1 d . A .
H87A H 0.6436 1.4965 -0.6071 0.052 Uiso 1 1 calc R . .
C88 C 0.7025(2) 1.43023(19) -0.69458(19) 0.0546(9) Uani 1 1 d . . .
H88A H 0.6680 1.3958 -0.6722 0.082 Uiso 1 1 calc R A .
H88B H 0.7611 1.4007 -0.7211 0.082 Uiso 1 1 calc R . .
H88C H 0.6781 1.4728 -0.7308 0.082 Uiso 1 1 calc R . .
C89 C 0.7597(3) 1.51565(19) -0.6645(2) 0.0603(10) Uani 1 1 d . . .
H89A H 0.7587 1.5373 -0.6236 0.090 Uiso 1 1 calc R A .
H89B H 0.7380 1.5581 -0.7022 0.090 Uiso 1 1 calc R . .
H89C H 0.8184 1.4846 -0.6888 0.090 Uiso 1 1 calc R . .
O13 O 1.00207(14) 1.17442(11) -0.43406(12) 0.0482(5) Uani 1 1 d D . .
C90 C 0.9602(2) 1.1803(2) -0.3539(2) 0.0565(9) Uani 1 1 d D . .
H90A H 0.9939 1.1384 -0.3226 0.068 Uiso 1 1 calc R . .
H90B H 0.9024 1.1764 -0.3375 0.068 Uiso 1 1 calc R . .
C91 C 0.9549(2) 1.2598(2) -0.3463(2) 0.0650(11) Uani 1 1 d D . .
H91A H 0.8987 1.2859 -0.3118 0.078 Uiso 1 1 calc R . .
H91B H 1.0003 1.2550 -0.3264 0.078 Uiso 1 1 calc R . .
C92 C 0.9670(3) 1.3040(2) -0.4247(2) 0.0623(10) Uani 1 1 d D . .
H92A H 0.9910 1.3451 -0.4319 0.075 Uiso 1 1 calc R . .
H92B H 0.9128 1.3277 -0.4375 0.075 Uiso 1 1 calc R . .
C93 C 1.0291(2) 1.24111(18) -0.4705(2) 0.0570(9) Uani 1 1 d D . .
H93A H 1.0278 1.2563 -0.5237 0.068 Uiso 1 1 calc R . .
H93B H 1.0878 1.2301 -0.4704 0.068 Uiso 1 1 calc R . .
O14 O 1.03801(19) 1.35102(15) -0.26140(15) 0.0711(7) Uani 1 1 d . C .
C94 C 1.0825(4) 1.3767(4) -0.2323(3) 0.1010(17) Uani 1 1 d . . .
H94A H 1.1179 1.4053 -0.2738 0.121 Uiso 0.514(17) 1 calc PR C 1
H94B H 1.1200 1.3320 -0.2064 0.121 Uiso 0.514(17) 1 calc PR C 1
H94C H 1.1344 1.3340 -0.2247 0.121 Uiso 0.486(17) 1 d PR C 2
H94D H 1.0990 1.4213 -0.2670 0.121 Uiso 0.486(17) 1 d PR C 2
C95 C 1.0147(6) 1.4294(7) -0.1769(7) 0.078(3) Uiso 0.514(17) 1 d P C 1
H95A H 0.9818 1.4788 -0.2020 0.093 Uiso 0.514(17) 1 calc PR C 1
H95B H 1.0376 1.4400 -0.1431 0.093 Uiso 0.514(17) 1 calc PR C 1
C96 C 0.9591(6) 1.3670(7) -0.1320(5) 0.072(3) Uiso 0.514(17) 1 d P C 1
H96A H 0.9896 1.3201 -0.1022 0.086 Uiso 0.514(17) 1 calc PR C 1
H96B H 0.9009 1.3920 -0.0995 0.086 Uiso 0.514(17) 1 calc PR C 1
C95' C 1.0197(10) 1.3935(12) -0.1496(10) 0.125(5) Uiso 0.486(17) 1 d P C 2
H95C H 1.0336 1.3471 -0.1111 0.150 Uiso 0.486(17) 1 calc PR C 2
H95D H 1.0248 1.4377 -0.1365 0.150 Uiso 0.486(17) 1 calc PR C 2
C96' C 0.9387(7) 1.4109(9) -0.1519(7) 0.085(4) Uiso 0.486(17) 1 d P C 2
H96C H 0.9156 1.4654 -0.1753 0.102 Uiso 0.486(17) 1 calc PR C 2
H96D H 0.8989 1.4007 -0.1009 0.102 Uiso 0.486(17) 1 calc PR C 2
C97 C 0.9591(3) 1.3505(3) -0.2050(2) 0.0716(11) Uani 1 1 d . . .
H97A H 0.9521 1.2993 -0.1958 0.086 Uiso 0.514(17) 1 calc PR C 1
H97B H 0.9111 1.3908 -0.2221 0.086 Uiso 0.514(17) 1 calc PR C 1
H97C H 0.9136 1.3660 -0.2287 0.086 Uiso 0.486(17) 1 d PR C 2
H97D H 0.9637 1.2984 -0.1741 0.086 Uiso 0.486(17) 1 d PR C 2
O15 O 0.7370(4) 1.2800(3) -0.1098(3) 0.1124(10) Uiso 0.720(4) 1 d PD D 1
C98 C 0.7783(6) 1.3090(5) -0.0799(5) 0.1124(10) Uiso 0.720(4) 1 d PD D 1
H98A H 0.7693 1.3647 -0.1009 0.135 Uiso 0.720(4) 1 calc PR D 1
H98B H 0.8404 1.2805 -0.0951 0.135 Uiso 0.720(4) 1 calc PR D 1
C99 C 0.7434(6) 1.2995(6) 0.0041(5) 0.1124(10) Uiso 0.720(4) 1 d PD D 1
H99A H 0.7182 1.3506 0.0216 0.135 Uiso 0.720(4) 1 calc PR D 1
H99B H 0.7890 1.2658 0.0274 0.135 Uiso 0.720(4) 1 calc PR D 1
C100 C 0.6768(6) 1.2629(6) 0.0250(5) 0.1124(10) Uiso 0.720(4) 1 d PD D 1
H10A H 0.6267 1.2847 0.0674 0.135 Uiso 0.720(4) 1 calc PR D 1
H10B H 0.6996 1.2058 0.0388 0.135 Uiso 0.720(4) 1 calc PR D 1
C101 C 0.6536(6) 1.2873(7) -0.0544(5) 0.1124(10) Uiso 0.720(4) 1 d PD D 1
H10C H 0.6287 1.2514 -0.0587 0.135 Uiso 0.720(4) 1 calc PR D 1
H10D H 0.6137 1.3412 -0.0595 0.135 Uiso 0.720(4) 1 calc PR D 1
O15' O 0.6425(9) 1.2633(8) 0.0020(9) 0.1124(10) Uiso 0.280(4) 1 d PD D 2
C102 C 0.6677(19) 1.2991(15) -0.0795(10) 0.1124(10) Uiso 0.280(4) 1 d PD D 2
H10E H 0.7011 1.2567 -0.1105 0.135 Uiso 0.280(4) 1 calc PR D 2
H10F H 0.6152 1.3291 -0.0944 0.135 Uiso 0.280(4) 1 calc PR D 2
C103 C 0.7171(15) 1.3497(13) -0.0985(10) 0.1124(10) Uiso 0.280(4) 1 d PD D 2
H10G H 0.6845 1.4038 -0.1155 0.135 Uiso 0.280(4) 1 calc PR D 2
H10H H 0.7711 1.3324 -0.1395 0.135 Uiso 0.280(4) 1 calc PR D 2
C104 C 0.7349(15) 1.3440(13) -0.0255(11) 0.1124(10) Uiso 0.280(4) 1 d PD D 2
H10I H 0.6999 1.3919 -0.0025 0.135 Uiso 0.280(4) 1 calc PR D 2
H10J H 0.7959 1.3354 -0.0354 0.135 Uiso 0.280(4) 1 calc PR D 2
C105 C 0.7098(16) 1.2731(13) 0.0273(12) 0.1124(10) Uiso 0.280(4) 1 d PD D 2
H10K H 0.6855 1.2819 0.0809 0.135 Uiso 0.280(4) 1 calc PR D 2
H10L H 0.7607 1.2256 0.0231 0.135 Uiso 0.280(4) 1 calc PR D 2
O16 O 1.02545(15) 1.02539(13) -0.20937(12) 0.0518(6) Uani 1 1 d . . .
H16' H 1.0745 0.9896 -0.2495 0.078 Uiso 1 1 d R . .
H16" H 0.9830 1.0019 -0.1829 0.078 Uiso 1 1 d R . .
O17 O 0.94097(17) 0.91772(15) -0.13019(13) 0.0637(7) Uani 1 1 d . . .
H17' H 0.9439 0.9097 -0.0813 0.096 Uiso 1 1 d R . .
H17" H 0.8991 0.8991 -0.1259 0.096 Uiso 1 1 d 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
O1 0.0778(19) 0.0878(19) 0.0717(19) -0.0411(15) -0.0043(15) -0.0403(15)
O2 0.0729(17) 0.0472(12) 0.0391(13) 0.0046(10) -0.0165(12) -0.0351(12)
O3 0.0435(13) 0.0425(11) 0.0466(13) -0.0080(9) -0.0182(11) -0.0151(10)
O4 0.0459(15) 0.0607(14) 0.0577(16) 0.0073(11) -0.0163(12) -0.0252(11)
O6 0.0698(17) 0.1001(19) 0.0380(13) -0.0142(12) -0.0212(12) -0.0433(14)
O7 0.0642(17) 0.0852(17) 0.0500(15) -0.0062(12) -0.0163(13) -0.0506(14)
O8 0.0560(15) 0.0495(12) 0.0556(14) 0.0065(10) -0.0372(12) -0.0245(10)
O9 0.095(2) 0.0560(14) 0.0552(16) -0.0116(11) -0.0534(15) 0.0037(13)
O10 0.0699(16) 0.0350(12) 0.0517(14) -0.0053(9) -0.0364(12) -0.0081(11)
O11 0.0432(13) 0.0424(11) 0.0355(11) 0.0004(9) -0.0226(10) -0.0167(9)
O12 0.0496(14) 0.0340(11) 0.0458(13) 0.0014(9) -0.0237(11) -0.0154(9)
N1 0.0531(18) 0.0471(15) 0.0338(16) -0.0087(13) -0.0092(14) -0.0260(13)
N2 0.0528(18) 0.0370(13) 0.0415(15) 0.0016(11) -0.0227(13) -0.0220(12)
N3 0.0454(17) 0.0347(13) 0.0410(17) 0.0025(11) -0.0127(14) -0.0181(12)
N4 0.0615(19) 0.0463(15) 0.0408(16) 0.0136(12) -0.0322(14) -0.0327(13)
N5 0.0446(16) 0.0495(14) 0.0330(14) 0.0028(11) -0.0186(12) -0.0209(12)
N6 0.0537(18) 0.0581(17) 0.0308(15) -0.0050(12) -0.0205(13) -0.0274(13)
N7 0.0506(17) 0.0319(13) 0.0389(15) 0.0012(11) -0.0270(13) -0.0148(11)
N8 0.0490(16) 0.0358(13) 0.0368(14) 0.0011(10) -0.0244(12) -0.0198(11)
N9 0.0517(17) 0.0296(13) 0.0402(15) 0.0000(11) -0.0283(13) -0.0125(12)
C1 0.057(2) 0.0424(17) 0.053(2) -0.0114(15) -0.0197(18) -0.0192(15)
C2 0.055(2) 0.0368(17) 0.055(2) -0.0062(15) -0.0243(17) -0.0187(15)
C3 0.064(2) 0.0385(17) 0.071(2) -0.0141(16) -0.025(2) -0.0186(16)
C4 0.065(3) 0.0409(18) 0.081(3) -0.0112(18) -0.028(2) -0.0242(17)
C5 0.060(2) 0.0402(18) 0.067(2) -0.0022(16) -0.0258(19) -0.0268(16)
C6 0.053(2) 0.0320(15) 0.0499(19) 0.0029(13) -0.0281(17) -0.0194(14)
C7 0.060(2) 0.0419(17) 0.0346(18) 0.0071(13) -0.0263(17) -0.0304(15)
C8 0.0437(19) 0.0332(15) 0.0379(18) -0.0004(12) -0.0162(15) -0.0177(13)
C9 0.0413(19) 0.0410(16) 0.0321(16) 0.0017(12) -0.0139(14) -0.0218(14)
C10 0.0386(18) 0.0315(15) 0.0401(18) 0.0028(12) -0.0208(14) -0.0172(12)
C11 0.0337(18) 0.0408(16) 0.0406(18) -0.0051(13) -0.0128(14) -0.0160(13)
C12 0.0438(19) 0.0421(17) 0.0388(18) 0.0006(13) -0.0153(15) -0.0206(14)
C13 0.048(2) 0.0408(16) 0.0371(18) 0.0056(13) -0.0172(15) -0.0242(14)
C14 0.0400(18) 0.0353(15) 0.0365(17) 0.0007(12) -0.0174(14) -0.0162(13)
C15 0.051(2) 0.0512(18) 0.048(2) -0.0118(15) -0.0162(16) -0.0222(15)
C16 0.070(3) 0.056(2) 0.072(3) -0.0193(18) -0.034(2) -0.0185(18)
C17 0.057(2) 0.0495(19) 0.043(2) 0.0000(15) -0.0039(17) -0.0171(16)
C18 0.067(3) 0.071(3) 0.111(4) -0.006(3) 0.019(3) -0.034(2)
C19 0.096(4) 0.109(4) 0.044(3) -0.008(2) -0.019(3) -0.009(3)
C20 0.054(2) 0.0392(16) 0.0337(18) 0.0050(13) -0.0179(16) -0.0227(14)
C21 0.0426(19) 0.0382(15) 0.0322(17) 0.0000(12) -0.0139(14) -0.0180(13)
C22 0.046(2) 0.0369(15) 0.0356(18) 0.0073(13) -0.0197(15) -0.0175(13)
C23 0.044(2) 0.0455(17) 0.0421(19) 0.0096(15) -0.0147(16) -0.0223(15)
C24 0.056(2) 0.0451(18) 0.040(2) 0.0024(15) -0.0081(17) -0.0209(15)
C25 0.064(2) 0.0440(17) 0.0395(19) -0.0067(14) -0.0111(17) -0.0220(16)
C26 0.0430(19) 0.0420(16) 0.0408(18) 0.0054(13) -0.0220(15) -0.0212(13)
C27 0.054(2) 0.063(2) 0.061(2) 0.0050(18) -0.0115(19) -0.0325(18)
C28 0.067(3) 0.098(3) 0.109(4) 0.000(3) -0.025(3) -0.050(3)
C29 0.070(3) 0.063(2) 0.059(3) -0.0141(19) 0.005(2) -0.032(2)
C32 0.057(2) 0.0531(19) 0.044(2) 0.0147(15) -0.0259(17) -0.0341(16)
C33 0.047(2) 0.0441(16) 0.0356(18) 0.0083(13) -0.0223(15) -0.0182(14)
C34 0.046(2) 0.0532(19) 0.041(2) 0.0098(15) -0.0179(16) -0.0219(15)
C35 0.054(2) 0.0567(19) 0.0279(18) 0.0075(14) -0.0151(16) -0.0151(16)
C36 0.056(2) 0.069(2) 0.0301(18) -0.0034(15) -0.0183(16) -0.0220(17)
C37 0.046(2) 0.0568(19) 0.0240(16) -0.0012(13) -0.0152(14) -0.0187(15)
C38 0.051(2) 0.060(2) 0.038(2) -0.0057(15) -0.0218(16) -0.0226(16)
C39 0.0458(19) 0.0414(16) 0.0356(17) 0.0034(13) -0.0198(15) -0.0243(14)
C40 0.048(2) 0.0371(15) 0.0364(17) 0.0026(12) -0.0245(15) -0.0208(13)
C41 0.049(2) 0.0303(14) 0.0368(17) 0.0059(12) -0.0232(15) -0.0195(13)
C42 0.053(2) 0.0502(18) 0.0397(19) 0.0059(14) -0.0225(16) -0.0319(15)
C43 0.059(2) 0.0523(18) 0.0412(19) 0.0022(14) -0.0247(17) -0.0337(16)
C44 0.067(2) 0.0537(19) 0.0364(18) -0.0017(14) -0.0244(17) -0.0333(17)
C45 0.070(3) 0.066(2) 0.073(3) -0.002(2) -0.034(2) -0.033(2)
C46 0.085(3) 0.062(2) 0.082(3) -0.011(2) -0.041(3) -0.020(2)
C47 0.074(3) 0.077(2) 0.050(2) -0.0053(18) -0.0256(19) -0.049(2)
C48 0.122(4) 0.138(4) 0.060(3) 0.021(3) -0.057(3) -0.094(4)
C49 0.095(4) 0.130(4) 0.104(4) -0.057(3) -0.024(3) -0.062(3)
C50 0.051(2) 0.0424(16) 0.0417(18) 0.0085(13) -0.0275(16) -0.0237(14)
C51 0.0466(19) 0.0433(16) 0.0419(18) 0.0055(13) -0.0228(15) -0.0258(14)
C52 0.0435(19) 0.0447(16) 0.0384(18) 0.0062(13) -0.0215(15) -0.0228(14)
C53 0.046(2) 0.0481(17) 0.0453(19) 0.0103(14) -0.0298(16) -0.0252(14)
C54 0.054(2) 0.0436(17) 0.060(2) 0.0079(15) -0.0330(18) -0.0293(15)
C55 0.060(2) 0.0449(17) 0.053(2) 0.0135(15) -0.0324(18) -0.0321(16)
C56 0.072(3) 0.059(2) 0.056(2) 0.0016(17) -0.034(2) -0.0372(18)
C57 0.125(5) 0.150(5) 0.058(3) 0.019(3) -0.055(3) -0.045(4)
C58 0.075(3) 0.060(2) 0.076(3) 0.0200(19) -0.049(2) -0.047(2)
C59 0.093(4) 0.100(3) 0.097(3) 0.008(3) -0.037(3) -0.075(3)
C60 0.101(3) 0.066(2) 0.096(3) -0.001(2) -0.055(3) -0.050(2)
C61 0.056(2) 0.0404(17) 0.048(2) -0.0044(14) -0.0309(17) -0.0168(14)
C62 0.051(2) 0.0386(16) 0.0390(18) 0.0000(13) -0.0242(15) -0.0193(14)
C63 0.056(2) 0.0457(18) 0.0406(19) -0.0014(14) -0.0285(16) -0.0172(15)
C64 0.060(2) 0.0474(18) 0.0431(19) -0.0077(14) -0.0277(17) -0.0168(16)
C65 0.056(2) 0.0389(16) 0.0450(19) -0.0039(14) -0.0253(16) -0.0166(14)
C66 0.050(2) 0.0334(15) 0.0358(17) 0.0030(12) -0.0223(15) -0.0190(14)
C67 0.052(2) 0.0335(16) 0.0381(18) -0.0003(13) -0.0230(15) -0.0163(14)
C68 0.0463(19) 0.0356(15) 0.0351(17) -0.0022(12) -0.0215(14) -0.0155(13)
C69 0.0419(18) 0.0347(15) 0.0316(16) 0.0022(12) -0.0173(14) -0.0152(13)
C70 0.0396(18) 0.0373(15) 0.0318(16) -0.0014(12) -0.0148(14) -0.0179(12)
C71 0.0402(18) 0.0386(15) 0.0319(16) -0.0010(12) -0.0188(14) -0.0139(13)
C72 0.0468(19) 0.0345(15) 0.0379(17) -0.0023(12) -0.0209(15) -0.0131(13)
C73 0.054(2) 0.0313(14) 0.0408(18) -0.0016(12) -0.0257(15) -0.0168(13)
C74 0.043(2) 0.0498(18) 0.045(2) -0.0020(14) -0.0201(16) -0.0140(14)
C75 0.053(3) 0.098(3) 0.079(3) -0.027(2) -0.031(2) -0.022(2)
C76 0.070(2) 0.0376(16) 0.049(2) 0.0067(14) -0.0399(19) -0.0209(15)
C77 0.099(3) 0.054(2) 0.053(2) 0.0153(17) -0.043(2) -0.044(2)
C78 0.083(3) 0.0364(17) 0.078(3) -0.0031(17) -0.053(2) -0.0073(17)
C79 0.0472(19) 0.0325(15) 0.0431(18) 0.0000(12) -0.0268(15) -0.0188(13)
C80 0.052(2) 0.0349(15) 0.0392(18) 0.0069(12) -0.0304(15) -0.0227(14)
C81 0.0450(19) 0.0357(15) 0.0405(18) 0.0048(13) -0.0251(15) -0.0208(14)
C82 0.0444(19) 0.0315(15) 0.0433(19) 0.0008(13) -0.0242(15) -0.0162(13)
C83 0.049(2) 0.0333(15) 0.0408(18) 0.0043(12) -0.0264(15) -0.0197(14)
C84 0.051(2) 0.0344(15) 0.0381(17) 0.0064(13) -0.0228(15) -0.0214(14)
C85 0.065(2) 0.0361(16) 0.051(2) -0.0026(14) -0.0303(18) -0.0150(15)
C86 0.077(3) 0.050(2) 0.063(3) -0.0082(17) -0.034(2) -0.0114(18)
C87 0.057(2) 0.0366(16) 0.0418(19) 0.0080(13) -0.0268(16) -0.0189(14)
C88 0.074(3) 0.0482(18) 0.043(2) 0.0036(15) -0.0329(19) -0.0142(16)
C89 0.076(3) 0.0456(19) 0.061(2) 0.0169(17) -0.032(2) -0.0287(18)
O13 0.0651(15) 0.0378(11) 0.0537(14) -0.0052(10) -0.0321(12) -0.0168(10)
C90 0.059(2) 0.062(2) 0.054(2) -0.0102(17) -0.0293(19) -0.0127(17)
C91 0.059(2) 0.070(2) 0.087(3) -0.036(2) -0.032(2) -0.0162(19)
C92 0.068(3) 0.0472(19) 0.086(3) -0.0080(19) -0.039(2) -0.0200(18)
C93 0.071(3) 0.0396(18) 0.077(3) -0.0038(17) -0.043(2) -0.0191(17)
O14 0.077(2) 0.0693(16) 0.0556(17) -0.0028(13) -0.0158(15) -0.0217(14)
C94 0.084(4) 0.145(5) 0.084(4) 0.009(3) -0.036(3) -0.056(3)
C97 0.083(3) 0.084(3) 0.048(2) -0.008(2) -0.009(2) -0.040(2)
O16 0.0609(16) 0.0630(14) 0.0442(13) -0.0079(10) -0.0172(12) -0.0321(12)
O17 0.086(2) 0.0791(17) 0.0457(14) 0.0078(12) -0.0316(14) -0.0475(15)

_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
O1 C1 1.241(4) . ?
O2 C7 1.223(4) . ?
O3 C11 1.387(4) . ?
O3 C15 1.448(3) . ?
O4 C23 1.391(4) . ?
O4 C27 1.443(4) . ?
O5 C32 1.261(4) . ?
O5' C32 1.287(9) . ?
O6 C38 1.234(3) . ?
O7 C42 1.397(4) . ?
O7 C45 1.401(4) . ?
O8 C53 1.387(3) . ?
O8 C56 1.436(4) . ?
O9 C61 1.235(3) . ?
O10 C67 1.215(4) . ?
O11 C71 1.396(3) . ?
O11 C74 1.438(4) . ?
O12 C82 1.376(4) . ?
O12 C85 1.436(3) . ?
N1 C1 1.339(4) . ?
N1 C20 1.416(4) . ?
N1 H1 0.78(3) . ?
N2 C6 1.339(4) . ?
N2 C2 1.362(4) . ?
N3 C7 1.351(4) . ?
N3 C8 1.410(4) . ?
N3 H3 0.86(4) . ?
N4 C32 1.320(4) . ?
N4 C50 1.417(3) . ?
N4 H4 0.86(4) . ?
N5 C33 1.332(4) . ?
N5 C37 1.344(3) . ?
N6 C38 1.342(4) . ?
N6 C39 1.416(4) . ?
N6 H6 0.81(4) . ?
N7 C61 1.354(4) . ?
N7 C79 1.404(4) . ?
N7 H7 0.86(3) . ?
N8 C66 1.337(4) . ?
N8 C62 1.345(3) . ?
N9 C67 1.349(4) . ?
N9 C68 1.433(3) . ?
N9 H9 0.87(3) . ?
C1 C2 1.496(5) . ?
C2 C3 1.382(4) . ?
C3 C4 1.389(5) . ?
C3 H3A 0.9500 . ?
C4 C5 1.377(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.398(4) . ?
C5 H5A 0.9500 . ?
C6 C7 1.501(5) . ?
C8 C13 1.387(4) . ?
C8 C9 1.400(4) . ?
C9 C10 1.380(4) . ?
C9 H9A 0.9500 . ?
C10 C11 1.398(4) . ?
C10 C14 1.529(4) . ?
C11 C12 1.407(4) . ?
C12 C13 1.400(5) . ?
C12 C17 1.508(5) . ?
C13 H13A 0.9500 . ?
C14 C41 1.521(4) . ?
C14 C70 1.537(4) . ?
C14 H14A 1.0000 . ?
C15 C16 1.504(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.524(5) . ?
C17 C19 1.525(6) . ?
C17 H17A 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C25 1.387(5) . ?
C20 C21 1.393(4) . ?
C21 C22 1.401(4) . ?
C21 H21A 0.9500 . ?
C22 C23 1.404(5) . ?
C22 C26 1.521(4) . ?
C23 C24 1.388(5) . ?
C24 C25 1.392(5) . ?
C24 C29 1.517(5) . ?
C25 H25A 0.9500 . ?
C26 C81 1.518(4) . ?
C26 C52 1.527(4) . ?
C26 H26A 1.0000 . ?
C27 C28 1.513(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30' 1.310(9) . ?
C29 C31 1.411(7) . ?
C29 C31' 1.634(11) . ?
C29 C30 1.651(8) . ?
C29 H29A 1.0000 . ?
C29 H29B 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H29B 1.5306 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C30' H30D 0.9800 . ?
C30' H30E 0.9800 . ?
C30' H30F 0.9800 . ?
C31' H31D 0.9800 . ?
C31' H31E 0.9800 . ?
C31' H31F 0.9800 . ?
C32 C33 1.504(4) . ?
C33 C34 1.391(4) . ?
C34 C35 1.375(4) . ?
C34 H34A 0.9500 . ?
C35 C36 1.384(5) . ?
C35 H35A 0.9500 . ?
C36 C37 1.382(4) . ?
C36 H36A 0.9500 . ?
C37 C38 1.500(4) . ?
C39 C40 1.375(4) . ?
C39 C44 1.400(4) . ?
C40 C41 1.383(4) . ?
C40 H40A 0.9500 . ?
C41 C42 1.401(4) . ?
C42 C43 1.394(5) . ?
C43 C44 1.401(5) . ?
C43 C47 1.534(4) . ?
C44 H44A 0.9500 . ?
C45 C46 1.439(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.519(5) . ?
C47 C49 1.531(6) . ?
C47 H47A 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C55 1.393(4) . ?
C50 C51 1.395(4) . ?
C51 C52 1.383(4) . ?
C51 H51A 0.9500 . ?
C52 C53 1.410(4) . ?
C53 C54 1.383(4) . ?
C54 C55 1.382(4) . ?
C54 C58 1.531(4) . ?
C55 H55A 0.9500 . ?
C56 C57 1.484(6) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C60 1.515(6) . ?
C58 C59 1.536(6) . ?
C58 H58A 1.0000 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.491(4) . ?
C62 C63 1.388(4) . ?
C63 C64 1.368(5) . ?
C63 H63A 0.9500 . ?
C64 C65 1.384(4) . ?
C64 H64A 0.9500 . ?
C65 C66 1.388(4) . ?
C65 H65A 0.9500 . ?
C66 C67 1.508(4) . ?
C68 C73 1.379(4) . ?
C68 C69 1.384(4) . ?
C69 C70 1.392(4) . ?
C69 H69A 0.9500 . ?
C70 C71 1.393(4) . ?
C71 C72 1.392(4) . ?
C72 C73 1.404(4) . ?
C72 C76 1.521(4) . ?
C73 H73A 0.9500 . ?
C74 C75 1.491(4) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 C78 1.508(5) . ?
C76 C77 1.523(5) . ?
C76 H76A 1.0000 . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 C84 1.400(4) . ?
C79 C80 1.402(4) . ?
C80 C81 1.385(4) . ?
C80 H80A 0.9500 . ?
C81 C82 1.409(4) . ?
C82 C83 1.403(4) . ?
C83 C84 1.382(4) . ?
C83 C87 1.530(4) . ?
C84 H84A 0.9500 . ?
C85 C86 1.494(5) . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C87 C89 1.535(4) . ?
C87 C88 1.539(4) . ?
C87 H87A 1.0000 . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
O13 C93 1.436(4) . ?
O13 C90 1.453(4) . ?
C90 C91 1.524(5) . ?
C90 H90A 0.9900 . ?
C90 H90B 0.9900 . ?
C91 C92 1.485(5) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 C93 1.494(5) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C93 H93A 0.9900 . ?
C93 H93B 0.9900 . ?
O14 C94 1.417(5) . ?
O14 C97 1.421(5) . ?
C94 C95 1.504(11) . ?
C94 C95' 1.593(17) . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
C94 H94C 0.9900 . ?
C94 H94D 0.9899 . ?
C95 C96 1.692(16) . ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C96 C97 1.527(9) . ?
C96 H96A 0.9900 . ?
C96 H96B 0.9900 . ?
C95' C96' 1.373(18) . ?
C95' H95C 0.9900 . ?
C95' H95D 0.9900 . ?
C96' C97 1.596(11) . ?
C96' H96C 0.9900 . ?
C96' H96D 0.9900 . ?
C97 H97A 0.9900 . ?
C97 H97B 0.9900 . ?
C97 H97C 0.9900 . ?
C97 H97D 0.9898 . ?
O15 C98 1.424(8) . ?
O15 C101 1.448(10) . ?
C98 C99 1.481(10) . ?
C98 H98A 0.9900 . ?
C98 H98B 0.9900 . ?
C99 C100 1.49(1) . ?
C99 H99A 0.9900 . ?
C99 H99B 0.9900 . ?
C100 C101 1.631(10) . ?
C100 H10A 0.9900 . ?
C100 H10B 0.9900 . ?
C101 H10C 0.9900 . ?
C101 H10D 0.9900 . ?
O15' C102 1.491(15) . ?
O15' C105 1.556(15) . ?
C102 C103 1.443(15) . ?
C102 H10E 0.9900 . ?
C102 H10F 0.9900 . ?
C103 C104 1.525(15) . ?
C103 H10G 0.9900 . ?
C103 H10H 0.9900 . ?
C104 C105 1.551(15) . ?
C104 H10I 0.9900 . ?
C104 H10J 0.9900 . ?
C105 H10K 0.9900 . ?
C105 H10L 0.9900 . ?
O16 H16' 1.0660 . ?
O16 H16" 0.9412 . ?
O17 H17' 0.9294 . ?
O17 H17" 0.9219 . ?

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
C11 O3 C15 115.9(2) . . ?
C23 O4 C27 116.5(2) . . ?
C42 O7 C45 121.2(3) . . ?
C53 O8 C56 114.8(3) . . ?
C71 O11 C74 114.6(2) . . ?
C82 O12 C85 116.8(2) . . ?
C1 N1 C20 128.6(3) . . ?
C1 N1 H1 116(2) . . ?
C20 N1 H1 115(2) . . ?
C6 N2 C2 117.5(2) . . ?
C7 N3 C8 128.3(3) . . ?
C7 N3 H3 113(3) . . ?
C8 N3 H3 118(3) . . ?
C32 N4 C50 128.2(2) . . ?
C32 N4 H4 114(3) . . ?
C50 N4 H4 116(3) . . ?
C33 N5 C37 116.8(3) . . ?
C38 N6 C39 128.5(2) . . ?
C38 N6 H6 113(2) . . ?
C39 N6 H6 116(3) . . ?
C61 N7 C79 125.3(2) . . ?
C61 N7 H7 117(2) . . ?
C79 N7 H7 116(2) . . ?
C66 N8 C62 117.0(2) . . ?
C67 N9 C68 123.4(3) . . ?
C67 N9 H9 120.1(19) . . ?
C68 N9 H9 114.8(19) . . ?
O1 C1 N1 125.0(3) . . ?
O1 C1 C2 119.5(3) . . ?
N1 C1 C2 115.4(3) . . ?
N2 C2 C3 123.2(3) . . ?
N2 C2 C1 118.3(2) . . ?
C3 C2 C1 118.5(3) . . ?
C2 C3 C4 118.3(3) . . ?
C2 C3 H3A 120.9 . . ?
C4 C3 H3A 120.9 . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
C4 C5 C6 119.1(3) . . ?
C4 C5 H5A 120.5 . . ?
C6 C5 H5A 120.5 . . ?
N2 C6 C5 122.4(3) . . ?
N2 C6 C7 118.6(2) . . ?
C5 C6 C7 118.8(3) . . ?
O2 C7 N3 125.4(3) . . ?
O2 C7 C6 121.1(3) . . ?
N3 C7 C6 113.3(3) . . ?
C13 C8 C9 118.6(3) . . ?
C13 C8 N3 124.4(3) . . ?
C9 C8 N3 116.9(3) . . ?
C10 C9 C8 121.7(3) . . ?
C10 C9 H9A 119.1 . . ?
C8 C9 H9A 119.1 . . ?
C9 C10 C11 118.9(2) . . ?
C9 C10 C14 121.2(3) . . ?
C11 C10 C14 119.9(3) . . ?
O3 C11 C10 117.1(2) . . ?
O3 C11 C12 121.8(3) . . ?
C10 C11 C12 120.8(3) . . ?
C13 C12 C11 118.4(3) . . ?
C13 C12 C17 120.2(3) . . ?
C11 C12 C17 121.4(3) . . ?
C8 C13 C12 121.4(3) . . ?
C8 C13 H13A 119.3 . . ?
C12 C13 H13A 119.3 . . ?
C41 C14 C10 112.1(2) . . ?
C41 C14 C70 111.0(2) . . ?
C10 C14 C70 112.9(2) . . ?
C41 C14 H14A 106.8 . . ?
C10 C14 H14A 106.8 . . ?
C70 C14 H14A 106.8 . . ?
O3 C15 C16 108.0(3) . . ?
O3 C15 H15A 110.1 . . ?
C16 C15 H15A 110.1 . . ?
O3 C15 H15B 110.1 . . ?
C16 C15 H15B 110.1 . . ?
H15A C15 H15B 108.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C17 C18 111.0(3) . . ?
C12 C17 C19 110.9(3) . . ?
C18 C17 C19 112.6(4) . . ?
C12 C17 H17A 107.4 . . ?
C18 C17 H17A 107.4 . . ?
C19 C17 H17A 107.4 . . ?
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 . . ?
C25 C20 C21 119.9(3) . . ?
C25 C20 N1 122.8(3) . . ?
C21 C20 N1 117.2(3) . . ?
C20 C21 C22 120.7(3) . . ?
C20 C21 H21A 119.6 . . ?
C22 C21 H21A 119.6 . . ?
C21 C22 C23 117.9(3) . . ?
C21 C22 C26 121.7(3) . . ?
C23 C22 C26 120.3(2) . . ?
C24 C23 O4 120.3(3) . . ?
C24 C23 C22 121.8(3) . . ?
O4 C23 C22 117.7(3) . . ?
C23 C24 C25 118.9(3) . . ?
C23 C24 C29 121.2(3) . . ?
C25 C24 C29 119.8(3) . . ?
C20 C25 C24 120.7(3) . . ?
C20 C25 H25A 119.6 . . ?
C24 C25 H25A 119.6 . . ?
C81 C26 C22 113.8(2) . . ?
C81 C26 C52 113.6(3) . . ?
C22 C26 C52 111.3(2) . . ?
C81 C26 H26A 105.8 . . ?
C22 C26 H26A 105.8 . . ?
C52 C26 H26A 105.8 . . ?
O4 C27 C28 106.6(3) . . ?
O4 C27 H27A 110.4 . . ?
C28 C27 H27A 110.4 . . ?
O4 C27 H27B 110.4 . . ?
C28 C27 H27B 110.4 . . ?
H27A C27 H27B 108.6 . . ?
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 . . ?
C30' C29 C31 124.7(6) . . ?
C30' C29 C24 119.1(6) . . ?
C31 C29 C24 113.7(4) . . ?
C30' C29 C31' 116.4(6) . . ?
C31 C29 C31' 24.9(4) . . ?
C24 C29 C31' 108.9(5) . . ?
C30' C29 C30 36.4(5) . . ?
C31 C29 C30 108.9(4) . . ?
C24 C29 C30 111.3(4) . . ?
C31' C29 C30 89.6(5) . . ?
C30' C29 H29A 71.4 . . ?
C31 C29 H29A 107.6 . . ?
C24 C29 H29A 107.6 . . ?
C31' C29 H29A 130.0 . . ?
C30 C29 H29A 107.6 . . ?
C30' C29 H29B 104.3 . . ?
C31 C29 H29B 76.7 . . ?
C24 C29 H29B 104.1 . . ?
C31' C29 H29B 101.6 . . ?
C30 C29 H29B 136.9 . . ?
H29A C29 H29B 36.2 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
C29 C31 H29B 39.5 . . ?
C29 C31 H31A 109.5 . . ?
H29B C31 H31A 81.7 . . ?
C29 C31 H31B 109.5 . . ?
H29B C31 H31B 147.5 . . ?
C29 C31 H31C 109.5 . . ?
H29B C31 H31C 94.2 . . ?
C29 C30' H30D 109.5 . . ?
C29 C30' H30E 109.5 . . ?
H30D C30' H30E 109.5 . . ?
C29 C30' H30F 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?
C29 C31' H31D 109.5 . . ?
C29 C31' H31E 109.5 . . ?
H31D C31' H31E 109.5 . . ?
C29 C31' H31F 109.5 . . ?
H31D C31' H31F 109.5 . . ?
H31E C31' H31F 109.5 . . ?
O5 C32 O5' 39.8(4) . . ?
O5 C32 N4 123.4(3) . . ?
O5' C32 N4 118.7(5) . . ?
O5 C32 C33 119.6(3) . . ?
O5' C32 C33 114.7(5) . . ?
N4 C32 C33 116.3(3) . . ?
N5 C33 C34 123.7(3) . . ?
N5 C33 C32 117.9(3) . . ?
C34 C33 C32 118.4(3) . . ?
C35 C34 C33 118.7(3) . . ?
C35 C34 H34A 120.7 . . ?
C33 C34 H34A 120.7 . . ?
C34 C35 C36 118.6(3) . . ?
C34 C35 H35A 120.7 . . ?
C36 C35 H35A 120.7 . . ?
C37 C36 C35 118.9(3) . . ?
C37 C36 H36A 120.5 . . ?
C35 C36 H36A 120.5 . . ?
N5 C37 C36 123.3(3) . . ?
N5 C37 C38 117.4(3) . . ?
C36 C37 C38 119.3(2) . . ?
O6 C38 N6 124.6(3) . . ?
O6 C38 C37 120.5(3) . . ?
N6 C38 C37 114.9(2) . . ?
C40 C39 C44 119.9(3) . . ?
C40 C39 N6 116.6(2) . . ?
C44 C39 N6 123.4(3) . . ?
C39 C40 C41 121.9(2) . . ?
C39 C40 H40A 119.0 . . ?
C41 C40 H40A 119.0 . . ?
C40 C41 C42 118.4(3) . . ?
C40 C41 C14 120.1(2) . . ?
C42 C41 C14 121.5(3) . . ?
C43 C42 O7 118.5(2) . . ?
C43 C42 C41 120.7(3) . . ?
O7 C42 C41 120.4(3) . . ?
C42 C43 C44 119.8(2) . . ?
C42 C43 C47 121.0(3) . . ?
C44 C43 C47 119.3(3) . . ?
C39 C44 C43 119.3(3) . . ?
C39 C44 H44A 120.4 . . ?
C43 C44 H44A 120.4 . . ?
O7 C45 C46 112.6(4) . . ?
O7 C45 H45A 109.1 . . ?
C46 C45 H45A 109.1 . . ?
O7 C45 H45B 109.1 . . ?
C46 C45 H45B 109.1 . . ?
H45A C45 H45B 107.8 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 C49 112.0(4) . . ?
C48 C47 C43 110.5(3) . . ?
C49 C47 C43 111.2(3) . . ?
C48 C47 H47A 107.7 . . ?
C49 C47 H47A 107.7 . . ?
C43 C47 H47A 107.7 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C55 C50 C51 119.2(2) . . ?
C55 C50 N4 122.4(2) . . ?
C51 C50 N4 118.3(2) . . ?
C52 C51 C50 121.3(2) . . ?
C52 C51 H51A 119.3 . . ?
C50 C51 H51A 119.3 . . ?
C51 C52 C53 118.0(2) . . ?
C51 C52 C26 122.1(2) . . ?
C53 C52 C26 119.7(2) . . ?
C54 C53 O8 120.6(2) . . ?
C54 C53 C52 121.4(2) . . ?
O8 C53 C52 117.8(2) . . ?
C55 C54 C53 119.3(2) . . ?
C55 C54 C58 119.0(3) . . ?
C53 C54 C58 121.6(3) . . ?
C54 C55 C50 120.8(3) . . ?
C54 C55 H55A 119.6 . . ?
C50 C55 H55A 119.6 . . ?
O8 C56 C57 107.0(4) . . ?
O8 C56 H56A 110.3 . . ?
C57 C56 H56A 110.3 . . ?
O8 C56 H56B 110.3 . . ?
C57 C56 H56B 110.3 . . ?
H56A C56 H56B 108.6 . . ?
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 . . ?
C60 C58 C54 111.3(3) . . ?
C60 C58 C59 111.9(3) . . ?
C54 C58 C59 110.1(3) . . ?
C60 C58 H58A 107.8 . . ?
C54 C58 H58A 107.8 . . ?
C59 C58 H58A 107.8 . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O9 C61 N7 123.6(3) . . ?
O9 C61 C62 119.9(3) . . ?
N7 C61 C62 116.4(3) . . ?
N8 C62 C63 122.9(3) . . ?
N8 C62 C61 118.0(3) . . ?
C63 C62 C61 119.1(3) . . ?
C64 C63 C62 119.3(3) . . ?
C64 C63 H63A 120.3 . . ?
C62 C63 H63A 120.3 . . ?
C63 C64 C65 118.7(3) . . ?
C63 C64 H64A 120.6 . . ?
C65 C64 H64A 120.6 . . ?
C64 C65 C66 118.6(3) . . ?
C64 C65 H65A 120.7 . . ?
C66 C65 H65A 120.7 . . ?
N8 C66 C65 123.5(3) . . ?
N8 C66 C67 118.1(2) . . ?
C65 C66 C67 118.4(3) . . ?
O10 C67 N9 124.6(3) . . ?
O10 C67 C66 120.4(3) . . ?
N9 C67 C66 114.9(2) . . ?
C73 C68 C69 120.6(2) . . ?
C73 C68 N9 122.1(2) . . ?
C69 C68 N9 117.3(2) . . ?
C68 C69 C70 120.6(2) . . ?
C68 C69 H69A 119.7 . . ?
C70 C69 H69A 119.7 . . ?
C69 C70 C71 118.0(2) . . ?
C69 C70 C14 122.2(2) . . ?
C71 C70 C14 119.8(2) . . ?
C72 C71 C70 122.5(2) . . ?
C72 C71 O11 120.2(2) . . ?
C70 C71 O11 117.2(2) . . ?
C71 C72 C73 117.6(2) . . ?
C71 C72 C76 122.2(2) . . ?
C73 C72 C76 120.1(2) . . ?
C68 C73 C72 120.5(2) . . ?
C68 C73 H73A 119.7 . . ?
C72 C73 H73A 119.7 . . ?
O11 C74 C75 107.2(3) . . ?
O11 C74 H74A 110.3 . . ?
C75 C74 H74A 110.3 . . ?
O11 C74 H74B 110.3 . . ?
C75 C74 H74B 110.3 . . ?
H74A C74 H74B 108.5 . . ?
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 . . ?
C78 C76 C72 110.8(3) . . ?
C78 C76 C77 110.2(3) . . ?
C72 C76 C77 112.2(3) . . ?
C78 C76 H76A 107.8 . . ?
C72 C76 H76A 107.8 . . ?
C77 C76 H76A 107.8 . . ?
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 . . ?
C76 C78 H78A 109.5 . . ?
C76 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C76 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C84 C79 C80 119.1(3) . . ?
C84 C79 N7 122.3(3) . . ?
C80 C79 N7 118.6(2) . . ?
C81 C80 C79 121.5(3) . . ?
C81 C80 H80A 119.3 . . ?
C79 C80 H80A 119.3 . . ?
C80 C81 C82 118.4(3) . . ?
C80 C81 C26 122.7(2) . . ?
C82 C81 C26 118.7(3) . . ?
O12 C82 C83 120.7(2) . . ?
O12 C82 C81 118.0(3) . . ?
C83 C82 C81 121.0(3) . . ?
C84 C83 C82 119.3(3) . . ?
C84 C83 C87 118.9(3) . . ?
C82 C83 C87 121.8(3) . . ?
C83 C84 C79 120.8(3) . . ?
C83 C84 H84A 119.6 . . ?
C79 C84 H84A 119.6 . . ?
O12 C85 C86 106.1(3) . . ?
O12 C85 H85A 110.5 . . ?
C86 C85 H85A 110.5 . . ?
O12 C85 H85B 110.5 . . ?
C86 C85 H85B 110.5 . . ?
H85A C85 H85B 108.7 . . ?
C85 C86 H86A 109.5 . . ?
C85 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C85 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C83 C87 C89 110.0(2) . . ?
C83 C87 C88 111.3(2) . . ?
C89 C87 C88 110.5(3) . . ?
C83 C87 H87A 108.3 . . ?
C89 C87 H87A 108.3 . . ?
C88 C87 H87A 108.3 . . ?
C87 C88 H88A 109.5 . . ?
C87 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C87 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C87 C89 H89A 109.5 . . ?
C87 C89 H89B 109.5 . . ?
H89A C89 H89B 109.5 . . ?
C87 C89 H89C 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
C93 O13 C90 107.9(2) . . ?
O13 C90 C91 105.2(3) . . ?
O13 C90 H90A 110.7 . . ?
C91 C90 H90A 110.7 . . ?
O13 C90 H90B 110.7 . . ?
C91 C90 H90B 110.7 . . ?
H90A C90 H90B 108.8 . . ?
C92 C91 C90 104.8(3) . . ?
C92 C91 H91A 110.8 . . ?
C90 C91 H91A 110.8 . . ?
C92 C91 H91B 110.8 . . ?
C90 C91 H91B 110.8 . . ?
H91A C91 H91B 108.9 . . ?
C91 C92 C93 101.2(3) . . ?
C91 C92 H92A 111.5 . . ?
C93 C92 H92A 111.5 . . ?
C91 C92 H92B 111.5 . . ?
C93 C92 H92B 111.5 . . ?
H92A C92 H92B 109.4 . . ?
O13 C93 C92 105.3(3) . . ?
O13 C93 H93A 110.7 . . ?
C92 C93 H93A 110.7 . . ?
O13 C93 H93B 110.7 . . ?
C92 C93 H93B 110.7 . . ?
H93A C93 H93B 108.8 . . ?
C94 O14 C97 108.2(3) . . ?
O14 C94 C95 105.7(5) . . ?
O14 C94 C95' 104.1(6) . . ?
C95 C94 C95' 27.1(6) . . ?
O14 C94 H94A 110.6 . . ?
C95 C94 H94A 110.6 . . ?
C95' C94 H94A 133.0 . . ?
O14 C94 H94B 110.6 . . ?
C95 C94 H94B 110.6 . . ?
C95' C94 H94B 86.7 . . ?
H94A C94 H94B 108.7 . . ?
O14 C94 H94C 110.4 . . ?
C95 C94 H94C 127.8 . . ?
C95' C94 H94C 106.2 . . ?
H94A C94 H94C 90.6 . . ?
H94B C94 H94C 20.4 . . ?
O14 C94 H94D 111.3 . . ?
C95 C94 H94D 90.8 . . ?
C95' C94 H94D 115.5 . . ?
H94A C94 H94D 21.1 . . ?
H94B C94 H94D 124.7 . . ?
H94C C94 H94D 109.0 . . ?
C94 C95 C96 94.6(7) . . ?
C94 C95 H95A 112.8 . . ?
C96 C95 H95A 112.8 . . ?
C94 C95 H95B 112.8 . . ?
C96 C95 H95B 112.8 . . ?
H95A C95 H95B 110.3 . . ?
C97 C96 C95 94.9(7) . . ?
C97 C96 H96A 112.8 . . ?
C95 C96 H96A 112.8 . . ?
C97 C96 H96B 112.8 . . ?
C95 C96 H96B 112.8 . . ?
H96A C96 H96B 110.2 . . ?
C96' C95' C94 106.3(12) . . ?
C96' C95' H95C 110.5 . . ?
C94 C95' H95C 110.5 . . ?
C96' C95' H95D 110.5 . . ?
C94 C95' H95D 110.5 . . ?
H95C C95' H95D 108.7 . . ?
C95' C96' C97 98.8(10) . . ?
C95' C96' H96C 112.0 . . ?
C97 C96' H96C 112.0 . . ?
C95' C96' H96D 112.0 . . ?
C97 C96' H96D 112.0 . . ?
H96C C96' H96D 109.7 . . ?
O14 C97 C96 108.2(4) . . ?
O14 C97 C96' 105.7(5) . . ?
C96 C97 C96' 30.0(4) . . ?
O14 C97 H97A 110.1 . . ?
C96 C97 H97A 110.1 . . ?
C96' C97 H97A 134.6 . . ?
O14 C97 H97B 110.1 . . ?
C96 C97 H97B 110.1 . . ?
C96' C97 H97B 83.8 . . ?
H97A C97 H97B 108.4 . . ?
O14 C97 H97C 110.5 . . ?
C96 C97 H97C 132.4 . . ?
C96' C97 H97C 111.3 . . ?
H97A C97 H97C 81.2 . . ?
H97B C97 H97C 29.5 . . ?
O14 C97 H97D 111.1 . . ?
C96 C97 H97D 81.0 . . ?
C96' C97 H97D 109.3 . . ?
H97A C97 H97D 31.0 . . ?
H97B C97 H97D 130.9 . . ?
H97C C97 H97D 108.9 . . ?
C98 O15 C101 105.3(6) . . ?
O15 C98 C99 110.1(6) . . ?
O15 C98 H98A 109.6 . . ?
C99 C98 H98A 109.6 . . ?
O15 C98 H98B 109.6 . . ?
C99 C98 H98B 109.6 . . ?
H98A C98 H98B 108.2 . . ?
C98 C99 C100 106.0(7) . . ?
C98 C99 H99A 110.5 . . ?
C100 C99 H99A 110.5 . . ?
C98 C99 H99B 110.5 . . ?
C100 C99 H99B 110.5 . . ?
H99A C99 H99B 108.7 . . ?
C99 C100 C101 100.7(6) . . ?
C99 C100 H10A 111.6 . . ?
C101 C100 H10A 111.6 . . ?
C99 C100 H10B 111.6 . . ?
C101 C100 H10B 111.6 . . ?
H10A C100 H10B 109.4 . . ?
O15 C101 C100 101.2(7) . . ?
O15 C101 H10C 111.5 . . ?
C100 C101 H10C 111.5 . . ?
O15 C101 H10D 111.5 . . ?
C100 C101 H10D 111.5 . . ?
H10C C101 H10D 109.3 . . ?
C102 O15' C105 98.9(11) . . ?
C103 C102 O15' 116.1(13) . . ?
C103 C102 H10E 108.3 . . ?
O15' C102 H10E 108.3 . . ?
C103 C102 H10F 108.3 . . ?
O15' C102 H10F 108.3 . . ?
H10E C102 H10F 107.4 . . ?
C102 C103 C104 105.3(12) . . ?
C102 C103 H10G 110.7 . . ?
C104 C103 H10G 110.7 . . ?
C102 C103 H10H 110.7 . . ?
C104 C103 H10H 110.7 . . ?
H10G C103 H10H 108.8 . . ?
C103 C104 C105 104.4(12) . . ?
C103 C104 H10I 110.9 . . ?
C105 C104 H10I 110.9 . . ?
C103 C104 H10J 110.9 . . ?
C105 C104 H10J 110.9 . . ?
H10I C104 H10J 108.9 . . ?
C104 C105 O15' 107.7(12) . . ?
C104 C105 H10K 110.2 . . ?
O15' C105 H10K 110.2 . . ?
C104 C105 H10L 110.2 . . ?
O15' C105 H10L 110.2 . . ?
H10K C105 H10L 108.5 . . ?
H16' O16 H16" 108.3 . . ?
H17' O17 H17" 106.1 . . ?

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 H1 O2 0.78(3) 2.34(3) 2.915(4) 131(3) 2_784
N1 H1 N2 0.78(3) 2.39(3) 2.757(4) 110(2) .
N3 H3 O14 0.86(4) 2.14(4) 2.933(4) 152(4) .
N6 H6 N5 0.81(4) 2.31(3) 2.720(3) 112(3) .
N6 H6 O16 0.81(4) 2.37(4) 3.115(3) 154(3) .
N7 H7 O13 0.86(3) 2.35(3) 3.098(3) 146(3) .
N9 H9 O13 0.87(3) 2.14(3) 2.958(3) 158(3) .
O16 H16" O17 0.94 1.90 2.786(3) 155.3 .
O17 H17' O6 0.93 1.95 2.783(3) 148.8 2_775

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        66.50
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.052

# 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 0.071 0.429 0.000 1041 273 ' '
2 0.452 0.375 0.635 7 0 ' '
3 0.548 0.625 0.365 7 0 ' '
_platon_squeeze_details          
;
;

# Attachment '- TriironComplex.cif'

data_gui6
_database_code_depnum_ccdc_archive 'CCDC 866978'
#TrackingRef '- TriironComplex.cif'

_audit_update_record             
;
2011-07-06 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C101.50 H107 Cl6 Fe3 K3 N15.50 O12, C4 H10 O1'

_chemical_formula_sum            'C105.50 H117 Cl6 Fe3 K3 N15.50 O13'
_chemical_formula_weight         2307.70

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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           Cubic
_symmetry_space_group_name_H-M   P213

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   22.8525(16)
_cell_length_b                   22.8525(16)
_cell_length_c                   22.8525(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11934.4(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9994
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      23.26

_exptl_crystal_description       irregular
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4798
_exptl_absorpt_coefficient_mu    0.66
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.8786
_exptl_absorpt_correction_T_max  0.8964
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            91754
_diffrn_reflns_av_R_equivalents  0.1080
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.26
_diffrn_reflns_theta_max         23.38
_reflns_number_total             5832
_reflns_number_gt                4639
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker APEX2 DUO(Bruker, 2008)'
_computing_cell_refinement       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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.

The asymmetric unit consists of a 1/3 Fe3 complex and a 1/3 diethyl ether
solvent molecule (each is located on a 3-fold axis of symmetry). The latter is
disordered and could not be modeled properly, thus program SQUEEZE, a part of
the PLATON package of crystallographic software, was used to calculate the
solvent disorder area and remove its contribution to the overall intensity
data.
;

_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^)+(0.1088P)^2^+1.3063P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_number_reflns         5832
_refine_ls_number_parameters     408
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0597
_refine_ls_wR_factor_ref         0.1684
_refine_ls_wR_factor_gt          0.1588
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.079
_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 0.48107(3) 0.38010(4) 0.61933(4) 0.0311(2) Uani 1 1 d . . .
K1 K 0.49057(9) 0.27559(8) 0.27654(8) 0.0716(6) Uani 1 1 d . B .
Cl1 Cl 0.54085(8) 0.30597(8) 0.63847(8) 0.0555(5) Uani 1 1 d . . .
Cl2 Cl 0.51424(7) 0.42441(7) 0.54073(7) 0.0404(4) Uani 1 1 d . . .
O1 O 0.3204(3) 0.2965(3) 0.5930(3) 0.098(2) Uani 1 1 d . . .
O2 O 0.4826(3) 0.4791(3) 0.7722(2) 0.0809(18) Uani 1 1 d . . .
O3 O 0.7095(2) 0.5731(2) 0.6862(3) 0.0722(18) Uani 1 1 d . . .
O4 O 0.4003(2) 0.2505(2) 0.3500(2) 0.0587(14) Uani 1 1 d . . .
N1 N 0.4110(2) 0.3365(2) 0.5785(2) 0.0408(13) Uani 1 1 d . . .
N2 N 0.4114(2) 0.3813(2) 0.6791(2) 0.0373(12) Uani 1 1 d . . .
N3 N 0.5040(2) 0.4419(2) 0.6810(2) 0.0359(12) Uani 1 1 d . . .
C1 C 0.3638(3) 0.3250(3) 0.6101(3) 0.054(2) Uani 1 1 d . . .
C2 C 0.3634(3) 0.3507(3) 0.6680(3) 0.0477(18) Uani 1 1 d . . .
C3 C 0.3191(3) 0.3482(4) 0.7088(4) 0.064(2) Uani 1 1 d . . .
H3A H 0.2847 0.3259 0.7014 0.077 Uiso 1 1 calc R . .
C4 C 0.3253(3) 0.3782(4) 0.7597(4) 0.069(2) Uani 1 1 d . . .
H4A H 0.2951 0.3766 0.7882 0.083 Uiso 1 1 calc R . .
C5 C 0.3729(4) 0.4097(4) 0.7705(3) 0.065(2) Uani 1 1 d . . .
H5A H 0.3770 0.4304 0.8063 0.079 Uiso 1 1 calc R . .
C6 C 0.4173(3) 0.4118(3) 0.7277(3) 0.0436(17) Uani 1 1 d . . .
C7 C 0.4716(3) 0.4474(3) 0.7296(3) 0.0462(17) Uani 1 1 d . . .
C8 C 0.5564(3) 0.4742(3) 0.6804(3) 0.0372(15) Uani 1 1 d . . .
C9 C 0.5617(2) 0.5254(3) 0.6467(3) 0.0328(14) Uani 1 1 d . A .
H9A H 0.5304 0.5372 0.6220 0.039 Uiso 1 1 calc R . .
C10 C 0.6132(3) 0.5595(3) 0.6490(2) 0.0329(14) Uani 1 1 d . . .
C11 C 0.6593(3) 0.5397(3) 0.6831(3) 0.0481(18) Uani 1 1 d . A .
C12 C 0.6547(3) 0.4884(3) 0.7173(3) 0.0509(18) Uani 1 1 d . . .
C13 C 0.6035(3) 0.4575(3) 0.7150(3) 0.0483(18) Uani 1 1 d . A .
H13A H 0.6000 0.4231 0.7381 0.058 Uiso 1 1 calc R . .
C14 C 0.6170(2) 0.6170(2) 0.6170(2) 0.036(2) Uani 0.33 1 d P A .
H14A H 0.6413 0.6413 0.6413 0.043 Uiso 1 3 d SR . .
C15 C 0.7546(7) 0.5565(7) 0.6548(7) 0.084(3) Uiso 0.60 1 d P A 1
H15A H 0.7485 0.5669 0.6132 0.101 Uiso 0.60 1 calc PR A 1
H15B H 0.7598 0.5136 0.6577 0.101 Uiso 0.60 1 calc PR A 1
C16 C 0.8084(7) 0.5880(7) 0.6789(7) 0.084(3) Uiso 0.60 1 d P A 1
H16A H 0.8431 0.5762 0.6566 0.126 Uiso 0.60 1 calc PR A 1
H16B H 0.8137 0.5777 0.7202 0.126 Uiso 0.60 1 calc PR A 1
H16C H 0.8029 0.6304 0.6754 0.126 Uiso 0.60 1 calc PR A 1
C15' C 0.7214(11) 0.6104(11) 0.7243(11) 0.084(3) Uiso 0.40 1 d P A 2
H15C H 0.7385 0.5907 0.7588 0.101 Uiso 0.40 1 calc PR A 2
H15D H 0.6849 0.6301 0.7369 0.101 Uiso 0.40 1 calc PR A 2
C16' C 0.7640(11) 0.6558(11) 0.7017(11) 0.084(3) Uiso 0.40 1 d P A 2
H16D H 0.7709 0.6853 0.7321 0.126 Uiso 0.40 1 calc PR A 2
H16E H 0.7476 0.6747 0.6669 0.126 Uiso 0.40 1 calc PR A 2
H16F H 0.8011 0.6368 0.6916 0.126 Uiso 0.40 1 calc PR A 2
C17 C 0.7053(4) 0.4698(4) 0.7579(4) 0.078(3) Uani 1 1 d . A .
C18 C 0.7100(8) 0.4100(8) 0.7704(8) 0.088(3) Uiso 0.60 1 d P A 1
H18A H 0.7279 0.3898 0.7371 0.133 Uiso 0.60 1 calc PR A 1
H18B H 0.6709 0.3938 0.7777 0.133 Uiso 0.60 1 calc PR A 1
H18C H 0.7344 0.4045 0.8053 0.133 Uiso 0.60 1 calc PR A 1
C19 C 0.6983(8) 0.4906(8) 0.8178(8) 0.088(3) Uiso 0.60 1 d P A 1
H19A H 0.7218 0.5261 0.8235 0.133 Uiso 0.60 1 calc PR A 1
H19B H 0.7114 0.4603 0.8452 0.133 Uiso 0.60 1 calc PR A 1
H19C H 0.6570 0.4996 0.8251 0.133 Uiso 0.60 1 calc PR A 1
C18' C 0.7229(12) 0.4078(11) 0.7383(12) 0.088(3) Uiso 0.40 1 d P A 2
H18D H 0.7397 0.4095 0.6989 0.133 Uiso 0.40 1 calc PR A 2
H18E H 0.6883 0.3825 0.7381 0.133 Uiso 0.40 1 calc PR A 2
H18F H 0.7521 0.3919 0.7655 0.133 Uiso 0.40 1 calc PR A 2
C19' C 0.6738(12) 0.4720(12) 0.8296(12) 0.088(3) Uiso 0.40 1 d P A 2
H19D H 0.6622 0.5123 0.8389 0.133 Uiso 0.40 1 calc PR A 2
H19E H 0.7025 0.4584 0.8583 0.133 Uiso 0.40 1 calc PR A 2
H19F H 0.6392 0.4466 0.8308 0.133 Uiso 0.40 1 calc PR A 2
C20 C 0.4109(3) 0.3150(3) 0.5207(3) 0.0417(16) Uani 1 1 d . . .
C21 C 0.3939(3) 0.3505(3) 0.4750(3) 0.0365(15) Uani 1 1 d . B .
H21A H 0.3855 0.3905 0.4826 0.044 Uiso 1 1 calc R . .
C22 C 0.3887(3) 0.3297(3) 0.4187(3) 0.0420(16) Uani 1 1 d . . .
C23 C 0.4033(3) 0.2701(3) 0.4087(4) 0.053(2) Uani 1 1 d . B .
C24 C 0.4224(3) 0.2336(3) 0.4524(3) 0.0489(18) Uani 1 1 d . . .
C25 C 0.4260(3) 0.2572(3) 0.5091(4) 0.0509(18) Uani 1 1 d . B .
H25A H 0.4390 0.2330 0.5403 0.061 Uiso 1 1 calc R . .
C26 C 0.3684(3) 0.3684(3) 0.3684(3) 0.049(3) Uani 0.33 1 d P B .
H26A H 0.3442 0.3442 0.3442 0.059 Uiso 1 3 d SR . .
C27 C 0.3554(8) 0.2111(8) 0.3429(9) 0.072(3) Uiso 0.60 1 d P B 1
H27A H 0.3179 0.2324 0.3388 0.087 Uiso 0.60 1 calc PR B 1
H27B H 0.3527 0.1857 0.3778 0.087 Uiso 0.60 1 calc PR B 1
C28 C 0.3655(7) 0.1740(7) 0.2894(7) 0.072(3) Uiso 0.60 1 d P B 1
H28A H 0.3329 0.1465 0.2847 0.108 Uiso 0.60 1 calc PR B 1
H28B H 0.4021 0.1521 0.2940 0.108 Uiso 0.60 1 calc PR B 1
H28C H 0.3682 0.1992 0.2548 0.108 Uiso 0.60 1 calc PR B 1
C27' C 0.3439(12) 0.2245(13) 0.3331(13) 0.072(3) Uiso 0.40 1 d P B 2
H27C H 0.3137 0.2555 0.3335 0.087 Uiso 0.40 1 calc PR B 2
H27D H 0.3328 0.1949 0.3628 0.087 Uiso 0.40 1 calc PR B 2
C28' C 0.3441(10) 0.1958(10) 0.2736(10) 0.072(3) Uiso 0.40 1 d P B 2
H28D H 0.3047 0.1815 0.2645 0.108 Uiso 0.40 1 calc PR B 2
H28E H 0.3716 0.1629 0.2737 0.108 Uiso 0.40 1 calc PR B 2
H28F H 0.3561 0.2244 0.2440 0.108 Uiso 0.40 1 calc PR B 2
C29 C 0.4398(4) 0.1695(3) 0.4409(4) 0.071(3) Uani 1 1 d . B .
C30 C 0.3960(7) 0.1313(7) 0.4670(6) 0.070(2) Uiso 0.60 1 d P B 1
H30A H 0.3622 0.1283 0.4407 0.105 Uiso 0.60 1 calc PR B 1
H30B H 0.3834 0.1476 0.5046 0.105 Uiso 0.60 1 calc PR B 1
H30C H 0.4128 0.0924 0.4731 0.105 Uiso 0.60 1 calc PR B 1
C31 C 0.5034(7) 0.1553(8) 0.4705(6) 0.070(2) Uiso 0.60 1 d P B 1
H31A H 0.5340 0.1769 0.4496 0.105 Uiso 0.60 1 calc PR B 1
H31B H 0.5113 0.1132 0.4679 0.105 Uiso 0.60 1 calc PR B 1
H31C H 0.5029 0.1673 0.5117 0.105 Uiso 0.60 1 calc PR B 1
C30' C 0.4073(11) 0.1270(11) 0.4899(10) 0.070(2) Uiso 0.40 1 d P B 2
H30D H 0.3650 0.1268 0.4829 0.105 Uiso 0.40 1 calc PR B 2
H30E H 0.4151 0.1420 0.5293 0.105 Uiso 0.40 1 calc PR B 2
H30F H 0.4225 0.0870 0.4866 0.105 Uiso 0.40 1 calc PR B 2
C31' C 0.5008(11) 0.1587(12) 0.4452(10) 0.070(2) Uiso 0.40 1 d P B 2
H31D H 0.5218 0.1840 0.4177 0.105 Uiso 0.40 1 calc PR B 2
H31E H 0.5088 0.1177 0.4358 0.105 Uiso 0.40 1 calc PR B 2
H31F H 0.5140 0.1670 0.4852 0.105 Uiso 0.40 1 calc PR B 2
N4 N 0.5502(9) 0.2773(9) 0.3945(9) 0.065(5) Uiso 0.33 1 d P . .
C32 C 0.5701(10) 0.2945(10) 0.4395(11) 0.051(6) Uiso 0.33 1 d P B .
C33 C 0.5986(15) 0.3070(15) 0.4862(15) 0.081(11) Uiso 0.33 1 d P . .
H33A H 0.5783 0.3356 0.5080 0.122 Uiso 0.33 1 d PR B .
H33B H 0.6037 0.2719 0.5092 0.122 Uiso 0.33 1 d PR . .
H33C H 0.6372 0.3215 0.4757 0.122 Uiso 0.33 1 d PR . .
N5 N 0.4458(4) 0.2397(4) 0.1695(4) 0.098(3) Uani 1 1 d D . .
C34 C 0.4341(4) 0.2112(4) 0.1304(4) 0.063(2) Uani 1 1 d D B .
C35 C 0.4230(4) 0.1714(4) 0.0854(4) 0.082(3) Uani 1 1 d D . .
H35A H 0.3937 0.1880 0.0602 0.123 Uiso 1 1 d R B .
H35B H 0.4581 0.1646 0.0634 0.123 Uiso 1 1 d R . .
H35C H 0.4090 0.1351 0.1011 0.123 Uiso 1 1 d R . .
N6 N 0.5494(9) 0.1727(13) 0.3049(13) 0.108(9) Uiso 0.33 1 d PD . .
C36 C 0.5949(11) 0.1612(16) 0.3243(15) 0.112(11) Uiso 0.33 1 d PD B .
C37 C 0.6452(9) 0.1452(9) 0.3548(9) 0.083(9) Uiso 0.50 3 d SPD . .
H37A H 0.6784 0.1484 0.3276 0.124 Uiso 0.17 1 d PR B .
H37B H 0.6504 0.1742 0.3846 0.124 Uiso 0.17 1 d PR . .
H37C H 0.6416 0.1080 0.3691 0.124 Uiso 0.17 1 d PR . .
N7 N 0.5245(7) 0.1593(6) 0.2658(6) 0.077(4) Uiso 0.50 1 d PD B .
C38 C 0.5269(6) 0.1219(6) 0.2348(6) 0.046(3) Uiso 0.50 1 d PD . .
C39 C 0.5261(9) 0.0771(8) 0.1913(7) 0.053(5) Uiso 0.50 1 d PD B .
H39A H 0.5534 0.0468 0.2013 0.079 Uiso 0.50 1 d PR . .
H39B H 0.4874 0.0609 0.1887 0.079 Uiso 0.50 1 d PR . .
H39C H 0.5367 0.0940 0.1544 0.079 Uiso 0.50 1 d PR . .

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 0.0279(5) 0.0333(5) 0.0321(5) 0.0060(4) -0.0012(4) -0.0040(4)
K1 0.0932(14) 0.0563(11) 0.0654(11) -0.0232(9) 0.0075(11) -0.0094(10)
Cl1 0.0574(11) 0.0539(11) 0.0553(11) 0.0123(9) -0.0043(9) 0.0188(9)
Cl2 0.0404(9) 0.0423(9) 0.0384(9) 0.0082(7) 0.0008(7) -0.0082(7)
O1 0.071(4) 0.135(6) 0.089(5) -0.025(4) 0.022(4) -0.067(4)
O2 0.084(4) 0.111(5) 0.048(3) -0.038(3) 0.012(3) -0.025(4)
O3 0.058(3) 0.046(3) 0.112(5) 0.005(3) -0.049(3) -0.019(3)
O4 0.063(3) 0.047(3) 0.066(3) -0.023(3) -0.001(3) -0.023(2)
N1 0.031(3) 0.045(3) 0.046(3) 0.004(3) -0.002(3) -0.018(3)
N2 0.033(3) 0.046(3) 0.032(3) 0.013(3) 0.000(2) -0.001(3)
N3 0.039(3) 0.039(3) 0.029(3) 0.001(2) -0.006(2) -0.013(2)
C1 0.046(4) 0.056(5) 0.058(5) 0.002(4) 0.002(4) -0.029(4)
C2 0.032(4) 0.048(4) 0.062(5) 0.021(4) 0.003(3) -0.012(3)
C3 0.045(5) 0.089(6) 0.058(5) 0.014(5) 0.010(4) -0.016(4)
C4 0.047(5) 0.086(6) 0.074(6) 0.027(5) 0.043(4) -0.002(5)
C5 0.063(5) 0.088(6) 0.045(4) 0.009(4) 0.017(4) -0.003(5)
C6 0.045(4) 0.056(4) 0.030(4) 0.007(3) 0.012(3) 0.006(3)
C7 0.047(4) 0.054(4) 0.037(4) 0.000(3) 0.005(3) -0.006(3)
C8 0.037(4) 0.044(4) 0.031(3) -0.009(3) -0.002(3) -0.002(3)
C9 0.028(3) 0.043(4) 0.028(3) -0.004(3) 0.001(3) -0.001(3)
C10 0.034(3) 0.037(3) 0.028(3) -0.004(3) -0.003(3) -0.004(3)
C11 0.033(4) 0.058(5) 0.053(4) 0.002(4) -0.014(3) -0.018(3)
C12 0.046(4) 0.048(4) 0.059(5) 0.008(4) -0.023(4) -0.001(4)
C13 0.057(5) 0.044(4) 0.043(4) 0.015(3) -0.018(4) -0.012(3)
C14 0.036(2) 0.036(2) 0.036(2) -0.012(3) -0.012(3) -0.012(3)
C17 0.074(6) 0.050(5) 0.109(7) 0.006(5) -0.056(5) -0.003(4)
C20 0.032(3) 0.039(4) 0.054(4) -0.003(3) 0.001(3) -0.015(3)
C21 0.035(4) 0.030(3) 0.045(4) -0.006(3) -0.008(3) -0.008(3)
C22 0.036(4) 0.036(4) 0.054(4) -0.011(3) -0.009(3) -0.015(3)
C23 0.036(4) 0.048(5) 0.075(5) -0.020(4) 0.004(4) -0.014(3)
C24 0.050(4) 0.043(4) 0.053(5) -0.001(4) 0.007(4) -0.012(3)
C25 0.044(4) 0.041(4) 0.068(5) 0.004(4) 0.001(4) -0.012(3)
C26 0.049(3) 0.049(3) 0.049(3) -0.016(3) -0.016(3) -0.016(3)
C29 0.072(6) 0.031(4) 0.109(7) -0.004(4) 0.012(5) -0.004(4)
N5 0.097(6) 0.111(7) 0.086(6) -0.039(6) 0.009(5) 0.000(5)
C34 0.079(6) 0.061(5) 0.050(5) -0.008(4) 0.001(4) 0.008(4)
C35 0.087(7) 0.095(7) 0.065(6) -0.021(5) 0.003(5) -0.028(6)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 2.063(5) . ?
Fe1 N2 2.098(5) . ?
Fe1 N1 2.104(5) . ?
Fe1 Cl2 2.1968(17) . ?
Fe1 Cl1 2.2198(19) . ?
K1 O1 2.595(7) 5 ?
K1 O4 2.722(5) . ?
K1 N5 2.775(9) . ?
K1 N7 2.778(14) . ?
K1 N6 2.79(2) . ?
K1 N4 3.02(2) . ?
K1 C21 3.209(6) 5 ?
K1 C20 3.287(6) 5 ?
K1 C22 3.295(7) 5 ?
K1 C23 3.469(7) 5 ?
K1 C25 3.491(7) 5 ?
O1 C1 1.248(8) . ?
O1 K1 2.595(7) 9 ?
O2 C7 1.239(8) . ?
O3 C15' 1.25(2) . ?
O3 C15 1.311(16) . ?
O3 C11 1.381(8) . ?
O4 C27 1.37(2) . ?
O4 C23 1.417(9) . ?
O4 C27' 1.47(3) . ?
N1 C1 1.325(9) . ?
N1 C20 1.411(9) . ?
N2 C6 1.319(8) . ?
N2 C2 1.325(8) . ?
N3 C7 1.342(8) . ?
N3 C8 1.405(8) . ?
C1 C2 1.449(10) . ?
C2 C3 1.377(10) . ?
C3 C4 1.359(12) . ?
C3 H3A 0.9500 . ?
C4 C5 1.326(12) . ?
C4 H4A 0.9500 . ?
C5 C6 1.409(10) . ?
C5 H5A 0.9500 . ?
C6 C7 1.485(10) . ?
C8 C13 1.390(9) . ?
C8 C9 1.407(9) . ?
C9 C10 1.412(8) . ?
C9 H9A 0.9500 . ?
C10 C11 1.388(9) . ?
C10 C14 1.506(6) . ?
C11 C12 1.412(10) . ?
C12 C13 1.368(10) . ?
C12 C17 1.544(10) . ?
C13 H13A 0.9500 . ?
C14 C10 1.506(6) 9 ?
C14 C10 1.506(6) 5 ?
C14 H14A 0.9599 . ?
C15 C16 1.53(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C15' C16' 1.51(3) . ?
C15' H15C 0.9900 . ?
C15' H15D 0.9900 . ?
C16' H16D 0.9800 . ?
C16' H16E 0.9800 . ?
C16' H16F 0.9800 . ?
C17 C18 1.400(19) . ?
C17 C19 1.46(2) . ?
C17 C18' 1.54(3) . ?
C17 C19' 1.79(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C18' H18D 0.9800 . ?
C18' H18E 0.9800 . ?
C18' H18F 0.9800 . ?
C19' H19D 0.9800 . ?
C19' H19E 0.9800 . ?
C19' H19F 0.9800 . ?
C20 C21 1.378(9) . ?
C20 C25 1.391(9) . ?
C20 K1 3.287(6) 9 ?
C21 C22 1.376(9) . ?
C21 K1 3.209(6) 9 ?
C21 H21A 0.9500 . ?
C22 C23 1.421(10) . ?
C22 C26 1.523(7) . ?
C22 K1 3.295(7) 9 ?
C23 C24 1.372(11) . ?
C23 K1 3.469(7) 9 ?
C24 C25 1.404(11) . ?
C24 C29 1.541(11) . ?
C25 K1 3.491(7) 9 ?
C25 H25A 0.9500 . ?
C26 C22 1.523(7) 9 ?
C26 C22 1.523(7) 5 ?
C26 H26A 0.9599 . ?
C27 C28 1.50(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C27' C28' 1.51(4) . ?
C27' H27C 0.9900 . ?
C27' H27D 0.9900 . ?
C28' H28D 0.9800 . ?
C28' H28E 0.9800 . ?
C28' H28F 0.9800 . ?
C29 C31' 1.42(3) . ?
C29 C30 1.456(18) . ?
C29 C31 1.635(18) . ?
C29 C30' 1.66(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C30' H30D 0.9800 . ?
C30' H30E 0.9800 . ?
C30' H30F 0.9800 . ?
C31' H31D 0.9800 . ?
C31' H31E 0.9800 . ?
C31' H31F 0.9800 . ?
N4 C32 1.19(3) . ?
C32 C39 0.87(3) 11_556 ?
C32 C33 1.28(4) . ?
C32 C38 1.56(3) 11_556 ?
C33 C39 0.57(3) 11_556 ?
C33 C38 1.13(3) 11_556 ?
C33 H33A 0.9599 . ?
C33 H33B 0.9601 . ?
C33 H33C 0.9599 . ?
N5 C34 1.137(9) . ?
C34 C35 1.396(11) . ?
C35 H35A 0.9602 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
N6 N7 1.10(3) . ?
N6 C36 1.160(17) . ?
C36 C37 1.394(17) . ?
C37 C36 1.394(17) 11_556 ?
C37 C36 1.394(17) 8_645 ?
C37 H37A 0.9838 . ?
C37 H37B 0.9581 . ?
C37 H37C 0.9149 . ?
N7 C38 1.112(13) . ?
C38 C33 1.13(3) 8_645 ?
C38 C39 1.427(15) . ?
C38 C32 1.56(3) 8_645 ?
C39 C33 0.57(3) 8_645 ?
C39 C32 0.87(3) 8_645 ?
C39 H39A 0.9601 . ?
C39 H39B 0.9598 . ?
C39 H39C 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
N3 Fe1 N2 74.9(2) . . ?
N3 Fe1 N1 145.1(2) . . ?
N2 Fe1 N1 73.6(2) . . ?
N3 Fe1 Cl2 98.91(15) . . ?
N2 Fe1 Cl2 142.00(15) . . ?
N1 Fe1 Cl2 96.80(15) . . ?
N3 Fe1 Cl1 103.41(15) . . ?
N2 Fe1 Cl1 110.42(15) . . ?
N1 Fe1 Cl1 101.22(16) . . ?
Cl2 Fe1 Cl1 107.49(7) . . ?
O1 K1 O4 131.2(2) 5 . ?
O1 K1 N5 127.2(3) 5 . ?
O4 K1 N5 101.6(2) . . ?
O1 K1 N7 98.1(3) 5 . ?
O4 K1 N7 93.7(3) . . ?
N5 K1 N7 75.1(4) . . ?
O1 K1 N6 81.8(5) 5 . ?
O4 K1 N6 92.5(6) . . ?
N5 K1 N6 97.7(6) . . ?
N7 K1 N6 22.8(6) . . ?
O1 K1 N4 55.3(4) 5 . ?
O4 K1 N4 78.1(4) . . ?
N5 K1 N4 163.1(4) . . ?
N7 K1 N4 88.0(5) . . ?
N6 K1 N4 65.5(7) . . ?
O1 K1 C21 71.02(17) 5 5 ?
O4 K1 C21 76.63(15) . 5 ?
N5 K1 C21 132.2(2) . 5 ?
N7 K1 C21 152.0(3) . 5 ?
N6 K1 C21 130.0(6) . 5 ?
N4 K1 C21 64.5(4) . 5 ?
O1 K1 C20 52.63(17) 5 5 ?
O4 K1 C20 101.08(16) . 5 ?
N5 K1 C20 126.2(2) . 5 ?
N7 K1 C20 149.8(4) . 5 ?
N6 K1 C20 129.1(6) . 5 ?
N4 K1 C20 69.8(4) . 5 ?
C21 K1 C20 24.45(16) 5 5 ?
O1 K1 C22 94.29(17) 5 5 ?
O4 K1 C22 63.91(16) . 5 ?
N5 K1 C22 111.9(2) . 5 ?
N7 K1 C22 157.2(3) . 5 ?
N6 K1 C22 144.8(6) . 5 ?
N4 K1 C22 83.4(4) . 5 ?
C21 K1 C22 24.39(15) 5 5 ?
C20 K1 C22 42.91(17) 5 5 ?
O1 K1 C23 99.29(19) 5 5 ?
O4 K1 C23 78.18(18) . 5 ?
N5 K1 C23 90.7(2) . 5 ?
N7 K1 C23 162.0(3) . 5 ?
N6 K1 C23 168.6(6) . 5 ?
N4 K1 C23 105.7(4) . 5 ?
C21 K1 C23 41.73(16) 5 5 ?
C20 K1 C23 48.15(17) 5 5 ?
C22 K1 C23 24.08(17) 5 5 ?
O1 K1 C25 61.60(19) 5 5 ?
O4 K1 C25 112.21(17) . 5 ?
N5 K1 C25 102.9(2) . 5 ?
N7 K1 C25 153.7(3) . 5 ?
N6 K1 C25 143.4(5) . 5 ?
N4 K1 C25 92.6(4) . 5 ?
C21 K1 C25 41.47(16) 5 5 ?
C20 K1 C25 23.44(16) 5 5 ?
C22 K1 C25 48.30(17) 5 5 ?
C23 K1 C25 39.80(19) 5 5 ?
C1 O1 K1 133.4(5) . 9 ?
C15' O3 C15 114.1(14) . . ?
C15' O3 C11 126.5(13) . . ?
C15 O3 C11 117.7(9) . . ?
C27 O4 C23 110.9(10) . . ?
C27 O4 C27' 18.2(14) . . ?
C23 O4 C27' 114.8(12) . . ?
C27 O4 K1 129.1(9) . . ?
C23 O4 K1 118.7(4) . . ?
C27' O4 K1 126.0(12) . . ?
C1 N1 C20 116.1(5) . . ?
C1 N1 Fe1 118.2(5) . . ?
C20 N1 Fe1 125.6(4) . . ?
C6 N2 C2 121.6(6) . . ?
C6 N2 Fe1 118.5(4) . . ?
C2 N2 Fe1 119.8(5) . . ?
C7 N3 C8 115.4(5) . . ?
C7 N3 Fe1 119.3(4) . . ?
C8 N3 Fe1 124.7(4) . . ?
O1 C1 N1 125.4(7) . . ?
O1 C1 C2 119.5(6) . . ?
N1 C1 C2 115.0(6) . . ?
N2 C2 C3 120.1(7) . . ?
N2 C2 C1 112.5(6) . . ?
C3 C2 C1 127.3(6) . . ?
C4 C3 C2 118.8(7) . . ?
C4 C3 H3A 120.6 . . ?
C2 C3 H3A 120.6 . . ?
C5 C4 C3 121.2(7) . . ?
C5 C4 H4A 119.4 . . ?
C3 C4 H4A 119.4 . . ?
C4 C5 C6 118.8(8) . . ?
C4 C5 H5A 120.6 . . ?
C6 C5 H5A 120.6 . . ?
N2 C6 C5 119.5(7) . . ?
N2 C6 C7 113.5(5) . . ?
C5 C6 C7 127.0(7) . . ?
O2 C7 N3 126.4(6) . . ?
O2 C7 C6 120.9(6) . . ?
N3 C7 C6 112.7(6) . . ?
C13 C8 N3 120.7(6) . . ?
C13 C8 C9 118.2(6) . . ?
N3 C8 C9 121.0(5) . . ?
C8 C9 C10 120.8(6) . . ?
C8 C9 H9A 119.6 . . ?
C10 C9 H9A 119.6 . . ?
C11 C10 C9 118.2(6) . . ?
C11 C10 C14 120.9(6) . . ?
C9 C10 C14 120.8(6) . . ?
O3 C11 C10 118.6(6) . . ?
O3 C11 C12 119.6(6) . . ?
C10 C11 C12 121.7(6) . . ?
C13 C12 C11 118.1(6) . . ?
C13 C12 C17 121.5(7) . . ?
C11 C12 C17 120.4(6) . . ?
C12 C13 C8 122.9(6) . . ?
C12 C13 H13A 118.6 . . ?
C8 C13 H13A 118.6 . . ?
C10 C14 C10 113.6(3) 9 . ?
C10 C14 C10 113.6(3) 9 5 ?
C10 C14 C10 113.6(3) . 5 ?
C10 C14 H14A 104.9 9 . ?
C10 C14 H14A 104.9 . . ?
C10 C14 H14A 104.9 5 . ?
O3 C15 C16 107.4(13) . . ?
O3 C15 H15A 110.2 . . ?
C16 C15 H15A 110.2 . . ?
O3 C15 H15B 110.2 . . ?
C16 C15 H15B 110.2 . . ?
H15A C15 H15B 108.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3 C15' C16' 111.7(19) . . ?
O3 C15' H15C 109.3 . . ?
C16' C15' H15C 109.3 . . ?
O3 C15' H15D 109.3 . . ?
C16' C15' H15D 109.3 . . ?
H15C C15' H15D 107.9 . . ?
C15' C16' H16D 109.5 . . ?
C15' C16' H16E 109.5 . . ?
H16D C16' H16E 109.5 . . ?
C15' C16' H16F 109.5 . . ?
H16D C16' H16F 109.5 . . ?
H16E C16' H16F 109.5 . . ?
C18 C17 C19 97.8(12) . . ?
C18 C17 C18' 30.8(11) . . ?
C19 C17 C18' 127.1(14) . . ?
C18 C17 C12 116.6(10) . . ?
C19 C17 C12 113.1(10) . . ?
C18' C17 C12 105.9(12) . . ?
C18 C17 C19' 82.7(13) . . ?
C19 C17 C19' 24.2(11) . . ?
C18' C17 C19' 113.5(15) . . ?
C12 C17 C19' 103.9(11) . . ?
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 C18' H18D 109.5 . . ?
C17 C18' H18E 109.5 . . ?
H18D C18' H18E 109.5 . . ?
C17 C18' H18F 109.5 . . ?
H18D C18' H18F 109.5 . . ?
H18E C18' H18F 109.5 . . ?
C17 C19' H19D 109.5 . . ?
C17 C19' H19E 109.5 . . ?
H19D C19' H19E 109.5 . . ?
C17 C19' H19F 109.5 . . ?
H19D C19' H19F 109.5 . . ?
H19E C19' H19F 109.5 . . ?
C21 C20 C25 119.0(7) . . ?
C21 C20 N1 120.3(6) . . ?
C25 C20 N1 120.6(6) . . ?
C21 C20 K1 74.6(4) . 9 ?
C25 C20 K1 86.5(4) . 9 ?
N1 C20 K1 106.9(4) . 9 ?
C22 C21 C20 121.9(6) . . ?
C22 C21 K1 81.3(4) . 9 ?
C20 C21 K1 81.0(4) . 9 ?
C22 C21 H21A 119.1 . . ?
C20 C21 H21A 119.1 . . ?
K1 C21 H21A 108.5 9 . ?
C21 C22 C23 117.4(7) . . ?
C21 C22 C26 122.1(6) . . ?
C23 C22 C26 120.5(6) . . ?
C21 C22 K1 74.3(4) . 9 ?
C23 C22 K1 84.8(4) . 9 ?
C26 C22 K1 110.6(4) . 9 ?
C24 C23 O4 120.8(7) . . ?
C24 C23 C22 122.7(7) . . ?
O4 C23 C22 116.4(7) . . ?
C24 C23 K1 84.3(5) . 9 ?
O4 C23 K1 118.9(4) . 9 ?
C22 C23 K1 71.1(4) . 9 ?
C23 C24 C25 117.2(7) . . ?
C23 C24 C29 122.4(7) . . ?
C25 C24 C29 120.4(7) . . ?
C20 C25 C24 121.7(7) . . ?
C20 C25 K1 70.0(4) . 9 ?
C24 C25 K1 83.1(4) . 9 ?
C20 C25 H25A 119.2 . . ?
C24 C25 H25A 119.2 . . ?
K1 C25 H25A 118.3 9 . ?
C22 C26 C22 112.7(4) 9 . ?
C22 C26 C22 112.7(4) 9 5 ?
C22 C26 C22 112.7(4) . 5 ?
C22 C26 H26A 106.1 9 . ?
C22 C26 H26A 106.1 . . ?
C22 C26 H26A 106.1 5 . ?
O4 C27 C28 110.5(14) . . ?
O4 C27 H27A 109.5 . . ?
C28 C27 H27A 109.5 . . ?
O4 C27 H27B 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
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 . . ?
O4 C27' C28' 114(2) . . ?
O4 C27' H27C 108.7 . . ?
C28' C27' H27C 108.7 . . ?
O4 C27' H27D 108.7 . . ?
C28' C27' H27D 108.7 . . ?
H27C C27' H27D 107.6 . . ?
C27' C28' H28D 109.5 . . ?
C27' C28' H28E 109.5 . . ?
H28D C28' H28E 109.5 . . ?
C27' C28' H28F 109.5 . . ?
H28D C28' H28F 109.5 . . ?
H28E C28' H28F 109.5 . . ?
C31' C29 C30 122.9(14) . . ?
C31' C29 C24 114.0(12) . . ?
C30 C29 C24 108.8(9) . . ?
C31' C29 C31 20.6(11) . . ?
C30 C29 C31 108.9(10) . . ?
C24 C29 C31 110.3(8) . . ?
C31' C29 C30' 107.0(14) . . ?
C30 C29 C30' 20.7(10) . . ?
C24 C29 C30' 109.(1) . . ?
C31 C29 C30' 90.2(11) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C30' H30D 109.5 . . ?
C29 C30' H30E 109.5 . . ?
H30D C30' H30E 109.5 . . ?
C29 C30' H30F 109.5 . . ?
H30D C30' H30F 109.5 . . ?
H30E C30' H30F 109.5 . . ?
C29 C31' H31D 109.5 . . ?
C29 C31' H31E 109.5 . . ?
H31D C31' H31E 109.5 . . ?
C29 C31' H31F 109.5 . . ?
H31D C31' H31F 109.5 . . ?
H31E C31' H31F 109.5 . . ?
C32 N4 K1 161.3(18) . . ?
C39 C32 N4 168(3) 11_556 . ?
C39 C32 C33 21(2) 11_556 . ?
N4 C32 C33 170(3) . . ?
C39 C32 C38 64.8(18) 11_556 11_556 ?
N4 C32 C38 125(2) . 11_556 ?
C33 C32 C38 45.7(17) . 11_556 ?
C39 C33 C38 110(5) 11_556 11_556 ?
C39 C33 C32 33(3) 11_556 . ?
C38 C33 C32 80(2) 11_556 . ?
C39 C33 H33A 76.2 11_556 . ?
C38 C33 H33A 162.5 11_556 . ?
C32 C33 H33A 108.7 . . ?
C39 C33 H33B 114.8 11_556 . ?
C38 C33 H33B 53.0 11_556 . ?
C32 C33 H33B 109.6 . . ?
H33A C33 H33B 109.5 . . ?
C39 C33 H33C 130.2 11_556 . ?
C38 C33 H33C 79.5 11_556 . ?
C32 C33 H33C 110.1 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C34 N5 K1 161.4(8) . . ?
N5 C34 C35 173.9(10) . . ?
C34 C35 H35A 108.2 . . ?
C34 C35 H35B 109.8 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 110.4 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N7 N6 C36 135(4) . . ?
N7 N6 K1 78.2(14) . . ?
C36 N6 K1 135(3) . . ?
N6 C36 C37 172(4) . . ?
C36 C37 C36 119.9(3) 11_556 . ?
C36 C37 C36 119.9(3) 11_556 8_645 ?
C36 C37 C36 119.9(3) . 8_645 ?
C36 C37 H37A 106.4 11_556 . ?
C36 C37 H37A 107.5 . . ?
C36 C37 H37A 60.6 8_645 . ?
C36 C37 H37B 15.1 11_556 . ?
C36 C37 H37B 106.1 . . ?
C36 C37 H37B 134.1 8_645 . ?
H37A C37 H37B 107.7 . . ?
C36 C37 H37C 101.2 11_556 . ?
C36 C37 H37C 110.4 . . ?
C36 C37 H37C 51.0 8_645 . ?
H37A C37 H37C 111.3 . . ?
H37B C37 H37C 113.6 . . ?
N6 N7 C38 135(2) . . ?
N6 N7 K1 78.9(16) . . ?
C38 N7 K1 143.6(13) . . ?
N7 C38 C33 152(2) . 8_645 ?
N7 C38 C39 174.4(19) . . ?
C33 C38 C39 22.0(18) 8_645 . ?
N7 C38 C32 151.6(18) . 8_645 ?
C33 C38 C32 54(2) 8_645 8_645 ?
C39 C38 C32 33.3(10) . 8_645 ?
C33 C39 C32 126(5) 8_645 8_645 ?
C33 C39 C38 48(4) 8_645 . ?
C32 C39 C38 82(2) 8_645 . ?
C33 C39 H39A 158.6 8_645 . ?
C32 C39 H39A 35.7 8_645 . ?
C38 C39 H39A 110.2 . . ?
C33 C39 H39B 83.4 8_645 . ?
C32 C39 H39B 142.0 8_645 . ?
C38 C39 H39B 109.4 . . ?
H39A C39 H39B 109.5 . . ?
C33 C39 H39C 80.6 8_645 . ?
C32 C39 H39C 100.0 8_645 . ?
C38 C39 H39C 108.7 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        23.38
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.076

# 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 0.017 0.017 0.017 239 67 ' '
2 -0.017 0.517 0.483 239 67 ' '
3 0.217 0.217 0.217 7 0 ' '
4 0.283 0.783 0.717 7 0 ' '
5 0.483 -0.017 0.517 239 67 ' '
6 0.517 0.483 -0.017 239 67 ' '
7 0.717 0.283 0.783 7 0 ' '
8 0.783 0.717 0.283 7 0 ' '
_platon_squeeze_details          
;
;