# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and 
#  data retrieval see:
#                         www.ccdc.cam.ac.uk 
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively. 
#
####################################################################### 

data_squeezed
_database_code_depnum_ccdc_archive 'CCDC 870607'
#TrackingRef 'cif-complex1.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H84 Dy4 N12 O12'
_chemical_formula_weight         2247.75
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'
Dy Dy -0.1892 4.4098 '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                   13.4782(4)
_cell_length_b                   14.0136(4)
_cell_length_c                   15.7024(4)
_cell_angle_alpha                69.4210(10)
_cell_angle_beta                 79.1840(10)
_cell_angle_gamma                63.0890(10)
_cell_volume                     2474.46(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9923
_cell_measurement_theta_min      2.625
_cell_measurement_theta_max      28.246
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    3.046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5564
_exptl_absorpt_correction_T_max  0.8701
_exptl_absorpt_process_details   sadabs
_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  'CCD area detector'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41055
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         28.31
_reflns_number_total             12089
_reflns_number_gt                9785
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART APEXll'
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_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^)+(0.0294P)^2^+0.1324P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12089
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0769
_refine_ls_wR_factor_gt          0.0737
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.715818(13) 0.798352(13) 0.239194(11) 0.01659(5) Uani 1 1 d . . .
Dy2 Dy 0.943230(12) 0.535113(12) 0.384206(11) 0.01476(5) Uani 1 1 d . . .
C17 C 0.4600(3) 0.9654(3) 0.2830(2) 0.0200(8) Uani 1 1 d . . .
C31 C 1.0409(3) 0.7215(3) 0.1341(3) 0.0262(9) Uani 1 1 d . . .
H31 H 1.0605 0.7512 0.1710 0.031 Uiso 1 1 calc R . .
C33 C 0.8587(3) 0.3534(3) 0.3675(2) 0.0176(7) Uani 1 1 d . . .
C26 C 0.8443(3) 0.5966(3) 0.1339(3) 0.0265(9) Uani 1 1 d . . .
H26 H 0.8484 0.5435 0.1074 0.032 Uiso 1 1 calc R . .
C39 C 1.0336(3) 0.3369(3) 0.2700(2) 0.0194(8) Uani 1 1 d . . .
H39 H 1.0842 0.2998 0.2288 0.023 Uiso 1 1 calc R . .
C41 C 1.2129(3) 0.4366(3) 0.3081(3) 0.0216(8) Uani 1 1 d . . .
H41A H 1.2433 0.3656 0.3583 0.026 Uiso 1 1 calc R . .
H41B H 1.2756 0.4552 0.2762 0.026 Uiso 1 1 calc R . .
C2 C 0.6506(3) 0.6001(3) 0.5071(2) 0.0234(8) Uani 1 1 d . . .
H2 H 0.6840 0.5302 0.4947 0.028 Uiso 1 1 calc R . .
C1 C 0.6845(3) 0.6860(3) 0.4556(2) 0.0187(8) Uani 1 1 d . . .
C9 C 0.8317(3) 0.9658(3) 0.2420(2) 0.0240(8) Uani 1 1 d . . .
H9A H 0.8497 1.0314 0.2125 0.029 Uiso 1 1 calc R . .
H9B H 0.8976 0.9026 0.2751 0.029 Uiso 1 1 calc R . .
C22 C 0.4191(3) 0.8829(3) 0.3275(2) 0.0202(8) Uani 1 1 d . . .
C47 C 0.9536(3) 0.7886(3) 0.4786(2) 0.0186(7) Uani 1 1 d . . .
H47 H 0.8940 0.7906 0.5223 0.022 Uiso 1 1 calc R . .
C48 C 1.0092(3) 0.6961(3) 0.4455(2) 0.0157(7) Uani 1 1 d . . .
C24 C 0.6086(3) 0.6063(3) 0.2905(3) 0.0249(9) Uani 1 1 d . . .
H24A H 0.5440 0.5881 0.2974 0.030 Uiso 1 1 calc R . .
H24B H 0.6561 0.5559 0.3435 0.030 Uiso 1 1 calc R . .
C6 C 0.6362(3) 0.7870(3) 0.4771(2) 0.0195(8) Uani 1 1 d . . .
C42 C 1.1628(3) 0.6017(3) 0.3434(2) 0.0193(8) Uani 1 1 d . . .
H42 H 1.2336 0.5962 0.3160 0.023 Uiso 1 1 calc R . .
C43 C 1.0971(3) 0.6953(3) 0.3801(2) 0.0172(7) Uani 1 1 d . . .
C8 C 0.7340(3) 0.9941(3) 0.3072(2) 0.0251(9) Uani 1 1 d . . .
H8A H 0.7518 1.0145 0.3549 0.030 Uiso 1 1 calc R . .
H8B H 0.6688 1.0590 0.2746 0.030 Uiso 1 1 calc R . .
C7 C 0.6664(3) 0.8808(3) 0.4283(2) 0.0209(8) Uani 1 1 d . . .
H7 H 0.6532 0.9335 0.4587 0.025 Uiso 1 1 calc R . .
C32 C 0.9592(3) 0.6800(3) 0.1659(2) 0.0208(8) Uani 1 1 d . . .
C23 C 0.4715(3) 0.7706(3) 0.3209(2) 0.0208(8) Uani 1 1 d . . .
H23 H 0.4299 0.7266 0.3438 0.025 Uiso 1 1 calc R . .
C37 C 0.9438(3) 0.2167(3) 0.2840(3) 0.0288(9) Uani 1 1 d . . .
H37 H 0.9995 0.1851 0.2425 0.035 Uiso 1 1 calc R . .
C3 C 0.5696(3) 0.6162(3) 0.5754(3) 0.0263(9) Uani 1 1 d . . .
H3 H 0.5464 0.5581 0.6084 0.032 Uiso 1 1 calc R . .
C20 C 0.2660(3) 1.0125(3) 0.3957(3) 0.0279(9) Uani 1 1 d . . .
H20 H 0.2006 1.0283 0.4338 0.034 Uiso 1 1 calc R . .
C30 C 1.0938(3) 0.7196(3) 0.0486(3) 0.0339(10) Uani 1 1 d . . .
H30 H 1.1490 0.7480 0.0278 0.041 Uiso 1 1 calc R . .
C10 C 0.8302(3) 0.9743(3) 0.0901(3) 0.0237(8) Uani 1 1 d . . .
H10 H 0.8673 1.0213 0.0796 0.028 Uiso 1 1 calc R . .
C5 C 0.5557(3) 0.8004(3) 0.5483(2) 0.0245(8) Uani 1 1 d . . .
H5 H 0.5242 0.8684 0.5636 0.029 Uiso 1 1 calc R . .
C4 C 0.5217(3) 0.7163(3) 0.5963(3) 0.0307(9) Uani 1 1 d . . .
H4 H 0.4658 0.7270 0.6433 0.037 Uiso 1 1 calc R . .
C45 C 1.0712(3) 0.8762(3) 0.3854(2) 0.0204(8) Uani 1 1 d . . .
H45 H 1.0913 0.9377 0.3646 0.025 Uiso 1 1 calc R . .
C25 C 0.6740(3) 0.5890(3) 0.2039(3) 0.0293(9) Uani 1 1 d . . .
H25A H 0.7080 0.5083 0.2085 0.035 Uiso 1 1 calc R . .
H25B H 0.6241 0.6313 0.1518 0.035 Uiso 1 1 calc R . .
C46 C 0.9844(3) 0.8770(3) 0.4486(2) 0.0206(8) Uani 1 1 d . . .
H46 H 0.9454 0.9391 0.4717 0.025 Uiso 1 1 calc R . .
C16 C 0.7467(3) 0.8994(3) 0.0130(3) 0.0253(9) Uani 1 1 d . . .
C38 C 0.9435(3) 0.3050(3) 0.3070(2) 0.0186(8) Uani 1 1 d . . .
C40 C 1.1556(3) 0.4223(3) 0.2424(2) 0.0211(8) Uani 1 1 d . . .
H40A H 1.1367 0.4883 0.1871 0.025 Uiso 1 1 calc R . .
H40B H 1.2060 0.3546 0.2240 0.025 Uiso 1 1 calc R . .
C44 C 1.1279(3) 0.7852(3) 0.3533(2) 0.0202(8) Uani 1 1 d . . .
H44 H 1.1894 0.7831 0.3118 0.024 Uiso 1 1 calc R . .
C34 C 0.7787(3) 0.3092(3) 0.4025(2) 0.0211(8) Uani 1 1 d . . .
H34 H 0.7207 0.3408 0.4426 0.025 Uiso 1 1 calc R . .
C21 C 0.3216(3) 0.9105(3) 0.3829(3) 0.0257(9) Uani 1 1 d . . .
H21 H 0.2938 0.8551 0.4126 0.031 Uiso 1 1 calc R . .
C18 C 0.4000(3) 1.0721(3) 0.2967(3) 0.0235(8) Uani 1 1 d . . .
H18 H 0.4254 1.1292 0.2669 0.028 Uiso 1 1 calc R . .
C19 C 0.3061(3) 1.0948(3) 0.3519(3) 0.0281(9) Uani 1 1 d . . .
H19 H 0.2680 1.1669 0.3606 0.034 Uiso 1 1 calc R . .
C27 C 0.9314(3) 0.6371(3) 0.1095(3) 0.0237(8) Uani 1 1 d . . .
C29 C 1.0662(3) 0.6765(3) -0.0061(3) 0.0356(10) Uani 1 1 d . . .
H29 H 1.1018 0.6756 -0.0643 0.043 Uiso 1 1 calc R . .
C28 C 0.9873(3) 0.6352(3) 0.0247(3) 0.0308(9) Uani 1 1 d . . .
H28 H 0.9697 0.6044 -0.0124 0.037 Uiso 1 1 calc R . .
C11 C 0.8111(3) 0.9569(3) 0.0106(2) 0.0240(8) Uani 1 1 d . . .
C35 C 0.7835(3) 0.2213(3) 0.3797(3) 0.0263(9) Uani 1 1 d . . .
H35 H 0.7297 0.1918 0.4054 0.032 Uiso 1 1 calc R . .
C13 C 0.8473(4) 0.9858(3) -0.1511(3) 0.0379(11) Uani 1 1 d . . .
H13 H 0.8822 1.0139 -0.2063 0.045 Uiso 1 1 calc R . .
C36 C 0.8653(3) 0.1750(3) 0.3200(3) 0.0331(10) Uani 1 1 d . . .
H36 H 0.8672 0.1147 0.3040 0.040 Uiso 1 1 calc R . .
C12 C 0.8600(3) 0.9987(3) -0.0716(3) 0.0329(10) Uani 1 1 d . . .
H12 H 0.9032 1.0372 -0.0727 0.039 Uiso 1 1 calc R . .
C15 C 0.7341(3) 0.8888(3) -0.0698(3) 0.0340(10) Uani 1 1 d . . .
H15 H 0.6907 0.8511 -0.0702 0.041 Uiso 1 1 calc R . .
C14 C 0.7827(4) 0.9312(3) -0.1501(3) 0.0385(11) Uani 1 1 d . . .
H14 H 0.7722 0.9232 -0.2049 0.046 Uiso 1 1 calc R . .
N5 N 1.0537(2) 0.4107(2) 0.28648(19) 0.0164(6) Uani 1 1 d . . .
N6 N 1.1332(2) 0.5268(2) 0.34490(19) 0.0174(6) Uani 1 1 d . . .
N1 N 0.7089(2) 0.8967(2) 0.34835(19) 0.0188(6) Uani 1 1 d . . .
N3 N 0.5697(2) 0.7240(2) 0.2868(2) 0.0208(7) Uani 1 1 d . . .
N2 N 0.8033(2) 0.9344(2) 0.17297(19) 0.0181(6) Uani 1 1 d . . .
N4 N 0.7620(2) 0.6291(2) 0.1898(2) 0.0225(7) Uani 1 1 d . . .
O1 O 0.76165(18) 0.67006(18) 0.38815(15) 0.0163(5) Uani 1 1 d . . .
O3 O 0.54895(19) 0.94639(19) 0.22921(16) 0.0205(5) Uani 1 1 d . . .
O6 O 0.98223(18) 0.60772(18) 0.47924(15) 0.0170(5) Uani 1 1 d . . .
O5 O 0.85333(19) 0.43628(19) 0.39068(16) 0.0192(5) Uani 1 1 d . . .
O4 O 0.90995(19) 0.68063(19) 0.24891(15) 0.0189(5) Uani 1 1 d . . .
O2 O 0.6986(2) 0.8582(2) 0.08884(16) 0.0256(6) Uani 1 1 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
Dy1 0.01447(9) 0.01503(9) 0.02113(10) -0.00704(7) -0.00031(7) -0.00590(7)
Dy2 0.01342(9) 0.01261(8) 0.01900(10) -0.00610(7) 0.00115(7) -0.00579(7)
C17 0.0162(19) 0.0208(19) 0.022(2) -0.0061(16) -0.0032(15) -0.0067(15)
C31 0.021(2) 0.022(2) 0.027(2) -0.0035(17) 0.0010(17) -0.0058(16)
C33 0.0187(18) 0.0138(17) 0.0195(19) -0.0019(14) -0.0076(15) -0.0059(14)
C26 0.026(2) 0.0190(19) 0.032(2) -0.0104(17) -0.0045(18) -0.0041(16)
C39 0.0182(18) 0.0194(18) 0.0189(19) -0.0088(15) 0.0019(15) -0.0053(15)
C41 0.0147(18) 0.0206(19) 0.030(2) -0.0114(16) 0.0032(16) -0.0066(15)
C2 0.020(2) 0.024(2) 0.027(2) -0.0058(17) -0.0029(16) -0.0106(16)
C1 0.0139(18) 0.0190(18) 0.022(2) -0.0051(15) -0.0043(15) -0.0049(15)
C9 0.030(2) 0.025(2) 0.026(2) -0.0080(17) -0.0009(17) -0.0182(18)
C22 0.0157(18) 0.0229(19) 0.021(2) -0.0044(16) -0.0047(15) -0.0079(15)
C47 0.0159(18) 0.0206(18) 0.0192(19) -0.0072(15) 0.0038(15) -0.0084(15)
C48 0.0141(17) 0.0133(16) 0.0181(18) -0.0027(14) -0.0036(14) -0.0048(14)
C24 0.026(2) 0.0191(19) 0.036(2) -0.0126(17) 0.0008(18) -0.0125(16)
C6 0.0154(18) 0.0208(19) 0.0202(19) -0.0058(15) -0.0034(15) -0.0051(15)
C42 0.0153(18) 0.0216(19) 0.023(2) -0.0073(16) -0.0006(15) -0.0091(15)
C43 0.0162(18) 0.0164(17) 0.0213(19) -0.0062(15) -0.0014(15) -0.0083(15)
C8 0.037(2) 0.0202(19) 0.023(2) -0.0074(16) -0.0009(17) -0.0152(18)
C7 0.023(2) 0.0145(17) 0.024(2) -0.0109(15) -0.0056(16) -0.0012(15)
C32 0.0127(18) 0.0178(18) 0.023(2) -0.0007(15) -0.0017(15) -0.0029(14)
C23 0.0198(19) 0.0224(19) 0.021(2) -0.0049(16) -0.0019(16) -0.0103(16)
C37 0.028(2) 0.029(2) 0.037(2) -0.0196(19) 0.0018(18) -0.0128(18)
C3 0.018(2) 0.031(2) 0.030(2) -0.0075(18) 0.0037(17) -0.0145(17)
C20 0.022(2) 0.037(2) 0.027(2) -0.0186(19) 0.0068(17) -0.0097(18)
C30 0.024(2) 0.028(2) 0.032(2) -0.0008(19) 0.0067(18) -0.0052(18)
C10 0.022(2) 0.0192(19) 0.031(2) -0.0060(17) -0.0026(17) -0.0095(16)
C5 0.0175(19) 0.026(2) 0.023(2) -0.0081(17) -0.0031(16) -0.0014(16)
C4 0.0146(19) 0.045(3) 0.023(2) -0.0052(19) 0.0042(16) -0.0098(18)
C45 0.022(2) 0.0181(18) 0.023(2) -0.0045(15) -0.0014(16) -0.0111(16)
C25 0.030(2) 0.024(2) 0.042(3) -0.0161(19) -0.0046(19) -0.0120(18)
C46 0.024(2) 0.0147(17) 0.025(2) -0.0075(15) -0.0038(16) -0.0082(15)
C16 0.027(2) 0.0199(19) 0.024(2) -0.0078(16) -0.0084(17) -0.0022(16)
C38 0.0175(18) 0.0140(17) 0.023(2) -0.0062(15) -0.0047(15) -0.0034(14)
C40 0.0192(19) 0.0161(18) 0.026(2) -0.0088(15) 0.0050(16) -0.0060(15)
C44 0.0153(18) 0.0200(18) 0.028(2) -0.0088(16) 0.0010(15) -0.0093(15)
C34 0.0209(19) 0.0196(18) 0.022(2) -0.0054(15) -0.0026(16) -0.0076(15)
C21 0.026(2) 0.029(2) 0.026(2) -0.0075(17) -0.0037(17) -0.0157(18)
C18 0.0168(19) 0.0202(19) 0.034(2) -0.0111(17) 0.0011(17) -0.0069(15)
C19 0.024(2) 0.027(2) 0.034(2) -0.0156(18) -0.0043(18) -0.0059(17)
C27 0.022(2) 0.0197(19) 0.024(2) -0.0093(16) 0.0014(16) -0.0032(16)
C29 0.034(2) 0.034(2) 0.020(2) -0.0065(19) 0.0062(19) -0.003(2)
C28 0.029(2) 0.031(2) 0.022(2) -0.0121(18) 0.0019(18) -0.0023(18)
C11 0.026(2) 0.0187(19) 0.020(2) -0.0041(16) -0.0018(16) -0.0042(16)
C35 0.027(2) 0.026(2) 0.035(2) -0.0119(18) -0.0020(18) -0.0160(18)
C13 0.052(3) 0.031(2) 0.018(2) -0.0069(18) 0.005(2) -0.010(2)
C36 0.035(2) 0.030(2) 0.050(3) -0.024(2) 0.002(2) -0.0188(19)
C12 0.037(2) 0.026(2) 0.030(2) -0.0018(18) 0.0002(19) -0.0139(19)
C15 0.038(3) 0.033(2) 0.026(2) -0.0097(19) -0.012(2) -0.006(2)
C14 0.048(3) 0.034(2) 0.021(2) -0.0101(19) -0.008(2) -0.004(2)
N5 0.0135(15) 0.0140(14) 0.0205(16) -0.0069(12) 0.0016(12) -0.0043(12)
N6 0.0138(15) 0.0138(14) 0.0228(17) -0.0067(13) 0.0002(12) -0.0035(12)
N1 0.0188(16) 0.0183(15) 0.0192(16) -0.0063(13) -0.0015(13) -0.0069(13)
N3 0.0235(17) 0.0173(15) 0.0239(17) -0.0055(13) -0.0036(14) -0.0100(13)
N2 0.0183(16) 0.0185(15) 0.0197(16) -0.0067(13) -0.0014(13) -0.0087(13)
N4 0.0257(17) 0.0177(15) 0.0271(18) -0.0074(14) -0.0025(14) -0.0105(14)
O1 0.0151(12) 0.0143(12) 0.0183(13) -0.0052(10) 0.0018(10) -0.0060(10)
O3 0.0154(13) 0.0158(12) 0.0263(14) -0.0038(11) 0.0014(11) -0.0060(10)
O6 0.0162(12) 0.0154(12) 0.0201(13) -0.0052(10) 0.0017(10) -0.0081(10)
O5 0.0191(13) 0.0173(12) 0.0262(14) -0.0094(11) 0.0016(11) -0.0107(11)
O4 0.0176(13) 0.0179(13) 0.0183(13) -0.0051(10) 0.0023(10) -0.0065(10)
O2 0.0346(16) 0.0255(14) 0.0191(14) -0.0047(11) -0.0049(12) -0.0147(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
Dy1 O2 2.229(2) . ?
Dy1 O3 2.251(2) . ?
Dy1 O4 2.378(2) . ?
Dy1 O1 2.380(2) . ?
Dy1 N3 2.506(3) . ?
Dy1 N2 2.507(3) . ?
Dy1 N1 2.516(3) . ?
Dy1 N4 2.528(3) . ?
Dy1 Dy2 3.8298(2) . ?
Dy2 O5 2.184(2) . ?
Dy2 O4 2.315(2) . ?
Dy2 O6 2.320(2) . ?
Dy2 O1 2.325(2) . ?
Dy2 O6 2.363(2) 2_766 ?
Dy2 N6 2.477(3) . ?
Dy2 N5 2.507(3) . ?
Dy2 Dy2 3.8398(3) 2_766 ?
C17 O3 1.308(4) . ?
C17 C22 1.412(5) . ?
C17 C18 1.415(5) . ?
C31 C30 1.401(5) . ?
C31 C32 1.404(5) . ?
C33 O5 1.303(4) . ?
C33 C34 1.411(5) . ?
C33 C38 1.418(5) . ?
C26 N4 1.291(5) . ?
C26 C27 1.458(5) . ?
C39 N5 1.296(4) . ?
C39 C38 1.434(5) . ?
C41 N6 1.462(4) . ?
C41 C40 1.512(5) . ?
C2 C3 1.379(5) . ?
C2 C1 1.410(5) . ?
C1 O1 1.340(4) . ?
C1 C6 1.401(5) . ?
C9 N2 1.470(4) . ?
C9 C8 1.498(5) . ?
C22 C21 1.407(5) . ?
C22 C23 1.438(5) . ?
C47 C46 1.382(4) . ?
C47 C48 1.400(4) . ?
C48 O6 1.350(4) . ?
C48 C43 1.412(5) . ?
C24 N3 1.470(4) . ?
C24 C25 1.508(5) . ?
C6 C5 1.403(5) . ?
C6 C7 1.464(5) . ?
C42 N6 1.274(4) . ?
C42 C43 1.458(5) . ?
C43 C44 1.404(4) . ?
C8 N1 1.453(4) . ?
C7 N1 1.266(4) . ?
C32 O4 1.349(4) . ?
C32 C27 1.409(5) . ?
C23 N3 1.289(4) . ?
C37 C36 1.372(5) . ?
C37 C38 1.405(5) . ?
C3 C4 1.384(5) . ?
C20 C21 1.349(5) . ?
C20 C19 1.401(5) . ?
C30 C29 1.389(6) . ?
C10 N2 1.278(4) . ?
C10 C11 1.440(5) . ?
C5 C4 1.380(5) . ?
C45 C44 1.376(5) . ?
C45 C46 1.383(5) . ?
C25 N4 1.478(4) . ?
C16 O2 1.318(4) . ?
C16 C15 1.409(5) . ?
C16 C11 1.416(5) . ?
C40 N5 1.468(4) . ?
C34 C35 1.371(5) . ?
C18 C19 1.367(5) . ?
C27 C28 1.404(5) . ?
C29 C28 1.366(6) . ?
C11 C12 1.394(5) . ?
C35 C36 1.382(5) . ?
C13 C12 1.374(5) . ?
C13 C14 1.389(6) . ?
C15 C14 1.374(6) . ?
O6 Dy2 2.363(2) 2_766 ?
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 Dy1 O3 80.87(9) . . ?
O2 Dy1 O4 100.18(9) . . ?
O3 Dy1 O4 163.54(8) . . ?
O2 Dy1 O1 158.72(8) . . ?
O3 Dy1 O1 115.14(8) . . ?
O4 Dy1 O1 68.64(8) . . ?
O2 Dy1 N3 99.21(9) . . ?
O3 Dy1 N3 72.38(9) . . ?
O4 Dy1 N3 123.18(9) . . ?
O1 Dy1 N3 74.34(8) . . ?
O2 Dy1 N2 72.72(9) . . ?
O3 Dy1 N2 88.24(9) . . ?
O4 Dy1 N2 76.55(8) . . ?
O1 Dy1 N2 119.48(8) . . ?
N3 Dy1 N2 160.13(9) . . ?
O2 Dy1 N1 131.57(9) . . ?
O3 Dy1 N1 71.87(9) . . ?
O4 Dy1 N1 96.09(8) . . ?
O1 Dy1 N1 69.04(8) . . ?
N3 Dy1 N1 109.14(9) . . ?
N2 Dy1 N1 67.32(9) . . ?
O2 Dy1 N4 72.63(9) . . ?
O3 Dy1 N4 125.75(9) . . ?
O4 Dy1 N4 69.48(8) . . ?
O1 Dy1 N4 86.30(9) . . ?
N3 Dy1 N4 66.55(10) . . ?
N2 Dy1 N4 125.23(9) . . ?
N1 Dy1 N4 154.89(9) . . ?
O2 Dy1 Dy2 128.85(7) . . ?
O3 Dy1 Dy2 149.90(6) . . ?
O4 Dy1 Dy2 34.76(5) . . ?
O1 Dy1 Dy2 35.04(5) . . ?
N3 Dy1 Dy2 95.15(7) . . ?
N2 Dy1 Dy2 104.05(6) . . ?
N1 Dy1 Dy2 87.46(6) . . ?
N4 Dy1 Dy2 68.89(7) . . ?
O5 Dy2 O4 110.28(8) . . ?
O5 Dy2 O6 138.59(8) . . ?
O4 Dy2 O6 101.58(8) . . ?
O5 Dy2 O1 80.63(8) . . ?
O4 Dy2 O1 70.66(8) . . ?
O6 Dy2 O1 85.88(8) . . ?
O5 Dy2 O6 82.69(8) . 2_766 ?
O4 Dy2 O6 165.84(8) . 2_766 ?
O6 Dy2 O6 69.86(9) . 2_766 ?
O1 Dy2 O6 118.54(8) . 2_766 ?
O5 Dy2 N6 138.60(9) . . ?
O4 Dy2 N6 80.08(8) . . ?
O6 Dy2 N6 71.42(8) . . ?
O1 Dy2 N6 138.36(8) . . ?
O6 Dy2 N6 86.37(8) 2_766 . ?
O5 Dy2 N5 73.68(9) . . ?
O4 Dy2 N5 85.02(8) . . ?
O6 Dy2 N5 136.33(8) . . ?
O1 Dy2 N5 135.63(8) . . ?
O6 Dy2 N5 93.60(8) 2_766 . ?
N6 Dy2 N5 67.31(9) . . ?
O5 Dy2 Dy1 90.20(6) . . ?
O4 Dy2 Dy1 35.86(6) . . ?
O6 Dy2 Dy1 101.37(5) . . ?
O1 Dy2 Dy1 36.00(6) . . ?
O6 Dy2 Dy1 154.54(5) 2_766 . ?
N6 Dy2 Dy1 114.16(6) . . ?
N5 Dy2 Dy1 107.86(6) . . ?
O5 Dy2 Dy2 112.02(6) . 2_766 ?
O4 Dy2 Dy2 135.89(6) . 2_766 ?
O6 Dy2 Dy2 35.30(5) . 2_766 ?
O1 Dy2 Dy2 104.52(6) . 2_766 ?
O6 Dy2 Dy2 34.57(5) 2_766 2_766 ?
N6 Dy2 Dy2 76.62(7) . 2_766 ?
N5 Dy2 Dy2 118.40(6) . 2_766 ?
Dy1 Dy2 Dy2 132.441(7) . 2_766 ?
O3 C17 C22 122.1(3) . . ?
O3 C17 C18 120.1(3) . . ?
C22 C17 C18 117.8(3) . . ?
C30 C31 C32 120.6(4) . . ?
O5 C33 C34 120.2(3) . . ?
O5 C33 C38 121.9(3) . . ?
C34 C33 C38 117.9(3) . . ?
N4 C26 C27 123.4(3) . . ?
N5 C39 C38 127.2(3) . . ?
N6 C41 C40 109.5(3) . . ?
C3 C2 C1 120.8(4) . . ?
O1 C1 C6 121.4(3) . . ?
O1 C1 C2 120.2(3) . . ?
C6 C1 C2 118.4(3) . . ?
N2 C9 C8 108.6(3) . . ?
C21 C22 C17 118.7(3) . . ?
C21 C22 C23 117.1(3) . . ?
C17 C22 C23 124.2(3) . . ?
C46 C47 C48 120.8(3) . . ?
O6 C48 C47 120.0(3) . . ?
O6 C48 C43 121.3(3) . . ?
C47 C48 C43 118.7(3) . . ?
N3 C24 C25 109.1(3) . . ?
C1 C6 C5 119.7(3) . . ?
C1 C6 C7 122.6(3) . . ?
C5 C6 C7 117.7(3) . . ?
N6 C42 C43 125.3(3) . . ?
C44 C43 C48 118.8(3) . . ?
C44 C43 C42 117.9(3) . . ?
C48 C43 C42 123.1(3) . . ?
N1 C8 C9 108.5(3) . . ?
N1 C7 C6 124.6(3) . . ?
O4 C32 C31 120.1(3) . . ?
O4 C32 C27 121.5(3) . . ?
C31 C32 C27 118.5(3) . . ?
N3 C23 C22 126.0(3) . . ?
C36 C37 C38 121.5(4) . . ?
C2 C3 C4 120.6(4) . . ?
C21 C20 C19 119.0(4) . . ?
C29 C30 C31 120.4(4) . . ?
N2 C10 C11 128.0(3) . . ?
C4 C5 C6 120.9(4) . . ?
C5 C4 C3 119.5(4) . . ?
C44 C45 C46 119.0(3) . . ?
N4 C25 C24 108.8(3) . . ?
C47 C46 C45 121.0(3) . . ?
O2 C16 C15 120.5(4) . . ?
O2 C16 C11 122.2(3) . . ?
C15 C16 C11 117.3(4) . . ?
C37 C38 C33 119.0(3) . . ?
C37 C38 C39 116.7(3) . . ?
C33 C38 C39 124.2(3) . . ?
N5 C40 C41 109.4(3) . . ?
C45 C44 C43 121.7(3) . . ?
C35 C34 C33 121.1(3) . . ?
C20 C21 C22 122.6(4) . . ?
C19 C18 C17 121.5(3) . . ?
C18 C19 C20 120.4(4) . . ?
C28 C27 C32 119.3(3) . . ?
C28 C27 C26 117.7(3) . . ?
C32 C27 C26 123.0(3) . . ?
C28 C29 C30 119.3(4) . . ?
C29 C28 C27 121.9(4) . . ?
C12 C11 C16 119.6(4) . . ?
C12 C11 C10 117.3(3) . . ?
C16 C11 C10 123.1(3) . . ?
C34 C35 C36 120.9(3) . . ?
C12 C13 C14 119.4(4) . . ?
C37 C36 C35 119.4(3) . . ?
C13 C12 C11 121.6(4) . . ?
C14 C15 C16 121.9(4) . . ?
C15 C14 C13 120.1(4) . . ?
C39 N5 C40 115.5(3) . . ?
C39 N5 Dy2 128.8(2) . . ?
C40 N5 Dy2 115.72(19) . . ?
C42 N6 C41 117.2(3) . . ?
C42 N6 Dy2 125.4(2) . . ?
C41 N6 Dy2 116.8(2) . . ?
C7 N1 C8 119.1(3) . . ?
C7 N1 Dy1 124.8(2) . . ?
C8 N1 Dy1 114.7(2) . . ?
C23 N3 C24 116.8(3) . . ?
C23 N3 Dy1 127.4(2) . . ?
C24 N3 Dy1 114.9(2) . . ?
C10 N2 C9 117.4(3) . . ?
C10 N2 Dy1 129.2(2) . . ?
C9 N2 Dy1 113.3(2) . . ?
C26 N4 C25 118.6(3) . . ?
C26 N4 Dy1 121.9(2) . . ?
C25 N4 Dy1 117.1(2) . . ?
C1 O1 Dy2 132.5(2) . . ?
C1 O1 Dy1 118.54(19) . . ?
Dy2 O1 Dy1 108.96(9) . . ?
C17 O3 Dy1 132.8(2) . . ?
C48 O6 Dy2 121.4(2) . . ?
C48 O6 Dy2 121.45(19) . 2_766 ?
Dy2 O6 Dy2 110.14(9) . 2_766 ?
C33 O5 Dy2 143.8(2) . . ?
C32 O4 Dy2 129.5(2) . . ?
C32 O4 Dy1 111.58(19) . . ?
Dy2 O4 Dy1 109.38(9) . . ?
C16 O2 Dy1 140.4(2) . . ?
_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.128
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.467 0.000 503.9 64.1
_platon_squeeze_details          
;
;


data_complex2
_database_code_depnum_ccdc_archive 'CCDC 870608'
#TrackingRef 'cif-complex2.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H84 Ho4 N12 O12'
_chemical_formula_weight         2257.47
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'
Ho Ho -0.2175 4.6783 '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                   13.4575(4)
_cell_length_b                   13.9789(4)
_cell_length_c                   15.7353(5)
_cell_angle_alpha                68.9730(10)
_cell_angle_beta                 78.8160(10)
_cell_angle_gamma                63.3230(10)
_cell_volume                     2466.99(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9837
_cell_measurement_theta_min      2.5185
_cell_measurement_theta_max      28.294
_exptl_crystal_description       plate
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1108
_exptl_absorpt_coefficient_mu    3.234
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.5756
_exptl_absorpt_correction_T_max  0.8815
_exptl_absorpt_process_details   SADABS
_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  'CCD area detector'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41181
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.39
_diffrn_reflns_theta_max         28.30
_reflns_number_total             12021
_reflns_number_gt                10225
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART APEXll'
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_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^)+(0.0359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12021
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0751
_refine_ls_wR_factor_gt          0.0723
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Ho1 Ho 0.217317(12) 0.797152(11) 0.240937(10) 0.01336(5) Uani 1 1 d . . .
Ho2 Ho 0.444720(11) 0.535235(11) 0.384307(10) 0.01184(5) Uani 1 1 d . . .
C1 C 0.1875(3) 0.6827(3) 0.4567(2) 0.0157(7) Uani 1 1 d . . .
C2 C 0.1535(3) 0.5962(3) 0.5088(2) 0.0195(7) Uani 1 1 d . . .
H2 H 0.1874 0.5259 0.4972 0.023 Uiso 1 1 calc R . .
C3 C 0.0713(3) 0.6126(3) 0.5768(3) 0.0258(8) Uani 1 1 d . . .
H3 H 0.0479 0.5540 0.6099 0.031 Uiso 1 1 calc R . .
C4 C 0.0218(3) 0.7135(3) 0.5978(3) 0.0273(8) Uani 1 1 d . . .
H4 H -0.0347 0.7241 0.6446 0.033 Uiso 1 1 calc R . .
C5 C 0.0568(3) 0.7975(3) 0.5490(2) 0.0223(8) Uani 1 1 d . . .
H5 H 0.0254 0.8656 0.5642 0.027 Uiso 1 1 calc R . .
C6 C 0.1368(3) 0.7855(3) 0.4782(2) 0.0180(7) Uani 1 1 d . . .
C7 C 0.1677(3) 0.8799(3) 0.4290(2) 0.0189(7) Uani 1 1 d . . .
H7 H 0.1544 0.9329 0.4589 0.023 Uiso 1 1 calc R . .
C8 C 0.2365(3) 0.9935(3) 0.3067(2) 0.0218(8) Uani 1 1 d . . .
H8A H 0.2547 1.0140 0.3539 0.026 Uiso 1 1 calc R . .
H8B H 0.1714 1.0585 0.2742 0.026 Uiso 1 1 calc R . .
C9 C 0.3351(3) 0.9644(3) 0.2403(2) 0.0214(8) Uani 1 1 d . . .
H9A H 0.3538 1.0300 0.2096 0.026 Uiso 1 1 calc R . .
H9B H 0.4008 0.9009 0.2731 0.026 Uiso 1 1 calc R . .
C10 C 0.3303(3) 0.9745(3) 0.0894(2) 0.0207(8) Uani 1 1 d . . .
H10 H 0.3666 1.0228 0.0778 0.025 Uiso 1 1 calc R . .
C11 C 0.3101(3) 0.9557(3) 0.0111(2) 0.0214(8) Uani 1 1 d . . .
C12 C 0.3593(3) 0.9979(3) -0.0729(3) 0.0302(9) Uani 1 1 d . . .
H12 H 0.4034 1.0362 -0.0751 0.036 Uiso 1 1 calc R . .
C13 C 0.3453(4) 0.9853(3) -0.1512(3) 0.0363(10) Uani 1 1 d . . .
H13 H 0.3796 1.0137 -0.2072 0.044 Uiso 1 1 calc R . .
C14 C 0.2794(3) 0.9297(3) -0.1477(3) 0.0326(10) Uani 1 1 d . . .
H14 H 0.2685 0.9210 -0.2018 0.039 Uiso 1 1 calc R . .
C15 C 0.2309(3) 0.8878(3) -0.0673(2) 0.0269(9) Uani 1 1 d . . .
H15 H 0.1869 0.8501 -0.0668 0.032 Uiso 1 1 calc R . .
C16 C 0.2440(3) 0.8989(3) 0.0144(2) 0.0213(8) Uani 1 1 d . . .
C17 C -0.0376(3) 0.9666(3) 0.2830(2) 0.0166(7) Uani 1 1 d . . .
C18 C -0.0976(3) 1.0740(3) 0.2962(2) 0.0215(8) Uani 1 1 d . . .
H18 H -0.0713 1.1311 0.2666 0.026 Uiso 1 1 calc R . .
C19 C -0.1926(3) 1.0970(3) 0.3509(2) 0.0247(8) Uani 1 1 d . . .
H19 H -0.2303 1.1693 0.3590 0.030 Uiso 1 1 calc R . .
C20 C -0.2345(3) 1.0165(3) 0.3945(3) 0.0267(8) Uani 1 1 d . . .
H20 H -0.3007 1.0331 0.4318 0.032 Uiso 1 1 calc R . .
C21 C -0.1780(3) 0.9119(3) 0.3825(2) 0.0240(8) Uani 1 1 d . . .
H21 H -0.2067 0.8567 0.4119 0.029 Uiso 1 1 calc R . .
C22 C -0.0806(3) 0.8843(3) 0.3289(2) 0.0168(7) Uani 1 1 d . . .
C23 C -0.0269(3) 0.7704(3) 0.3225(2) 0.0190(7) Uani 1 1 d . . .
H23 H -0.0687 0.7262 0.3452 0.023 Uiso 1 1 calc R . .
C24 C 0.1094(3) 0.6057(3) 0.2940(3) 0.0219(8) Uani 1 1 d . . .
H24A H 0.0447 0.5869 0.3021 0.026 Uiso 1 1 calc R . .
H24B H 0.1572 0.5555 0.3467 0.026 Uiso 1 1 calc R . .
C25 C 0.1742(3) 0.5880(3) 0.2071(3) 0.0235(8) Uani 1 1 d . . .
H25A H 0.2076 0.5071 0.2122 0.028 Uiso 1 1 calc R . .
H25B H 0.1241 0.6302 0.1552 0.028 Uiso 1 1 calc R . .
C26 C 0.3440(3) 0.5969(3) 0.1363(2) 0.0222(8) Uani 1 1 d . . .
H26 H 0.3481 0.5434 0.1103 0.027 Uiso 1 1 calc R . .
C27 C 0.4306(3) 0.6377(3) 0.1102(2) 0.0211(8) Uani 1 1 d . . .
C28 C 0.4866(3) 0.6368(3) 0.0251(3) 0.0288(9) Uani 1 1 d . . .
H28 H 0.4691 0.6060 -0.0119 0.035 Uiso 1 1 calc R . .
C29 C 0.5662(3) 0.6793(3) -0.0062(3) 0.0318(9) Uani 1 1 d . . .
H29 H 0.6020 0.6789 -0.0645 0.038 Uiso 1 1 calc R . .
C30 C 0.5934(3) 0.7222(3) 0.0475(3) 0.0295(9) Uani 1 1 d . . .
H30 H 0.6479 0.7519 0.0260 0.035 Uiso 1 1 calc R . .
C31 C 0.5415(3) 0.7225(3) 0.1330(2) 0.0227(8) Uani 1 1 d . . .
H31 H 0.5622 0.7511 0.1700 0.027 Uiso 1 1 calc R . .
C32 C 0.4593(3) 0.6812(3) 0.1654(2) 0.0178(7) Uani 1 1 d . . .
C33 C 0.3598(3) 0.3537(3) 0.3679(2) 0.0169(7) Uani 1 1 d . . .
C34 C 0.2789(3) 0.3085(3) 0.4029(2) 0.0196(7) Uani 1 1 d . . .
H34 H 0.2209 0.3390 0.4435 0.024 Uiso 1 1 calc R . .
C35 C 0.2833(3) 0.2216(3) 0.3790(3) 0.0249(8) Uani 1 1 d . . .
H35 H 0.2291 0.1920 0.4042 0.030 Uiso 1 1 calc R . .
C36 C 0.3661(3) 0.1757(3) 0.3181(3) 0.0294(9) Uani 1 1 d . . .
H36 H 0.3673 0.1163 0.3013 0.035 Uiso 1 1 calc R . .
C37 C 0.4455(3) 0.2172(3) 0.2829(3) 0.0252(8) Uani 1 1 d . . .
H37 H 0.5021 0.1857 0.2419 0.030 Uiso 1 1 calc R . .
C38 C 0.4445(3) 0.3064(3) 0.3066(2) 0.0159(7) Uani 1 1 d . . .
C39 C 0.5337(3) 0.3392(3) 0.2702(2) 0.0194(7) Uani 1 1 d . . .
H39 H 0.5839 0.3026 0.2287 0.023 Uiso 1 1 calc R . .
C40 C 0.6572(3) 0.4246(3) 0.2421(2) 0.0173(7) Uani 1 1 d . . .
H40A H 0.6387 0.4909 0.1865 0.021 Uiso 1 1 calc R . .
H40B H 0.7075 0.3569 0.2238 0.021 Uiso 1 1 calc R . .
C41 C 0.7144(3) 0.4389(3) 0.3070(2) 0.0183(7) Uani 1 1 d . . .
H41A H 0.7454 0.3673 0.3569 0.022 Uiso 1 1 calc R . .
H41B H 0.7766 0.4588 0.2745 0.022 Uiso 1 1 calc R . .
C42 C 0.6633(3) 0.6043(3) 0.3431(2) 0.0163(7) Uani 1 1 d . . .
H42 H 0.7336 0.6003 0.3150 0.020 Uiso 1 1 calc R . .
C43 C 0.5965(3) 0.6974(3) 0.3811(2) 0.0156(7) Uani 1 1 d . . .
C44 C 0.6269(3) 0.7879(3) 0.3530(2) 0.0159(7) Uani 1 1 d . . .
H44 H 0.6877 0.7873 0.3105 0.019 Uiso 1 1 calc R . .
C45 C 0.5693(3) 0.8786(3) 0.3864(2) 0.0182(7) Uani 1 1 d . . .
H45 H 0.5899 0.9402 0.3664 0.022 Uiso 1 1 calc R . .
C46 C 0.4822(3) 0.8785(3) 0.4489(2) 0.0179(7) Uani 1 1 d . . .
H46 H 0.4421 0.9408 0.4715 0.022 Uiso 1 1 calc R . .
C47 C 0.4523(3) 0.7886(3) 0.4790(2) 0.0156(7) Uani 1 1 d . . .
H47 H 0.3927 0.7894 0.5229 0.019 Uiso 1 1 calc R . .
C48 C 0.5086(3) 0.6965(2) 0.4458(2) 0.0137(7) Uani 1 1 d . . .
N1 N 0.2111(2) 0.8951(2) 0.34875(19) 0.0172(6) Uani 1 1 d . . .
N2 N 0.3043(2) 0.9329(2) 0.17271(19) 0.0163(6) Uani 1 1 d . . .
N3 N 0.0707(2) 0.7240(2) 0.28941(19) 0.0174(6) Uani 1 1 d . . .
N4 N 0.2622(2) 0.6282(2) 0.1920(2) 0.0204(6) Uani 1 1 d . . .
N5 N 0.5556(2) 0.4127(2) 0.28616(18) 0.0139(6) Uani 1 1 d . . .
N6 N 0.6339(2) 0.5285(2) 0.34503(18) 0.0146(6) Uani 1 1 d . . .
O1 O 0.26454(18) 0.66797(17) 0.38913(15) 0.0138(5) Uani 1 1 d . . .
O2 O 0.19651(19) 0.85747(18) 0.09106(16) 0.0211(5) Uani 1 1 d . . .
O3 O 0.05181(18) 0.94660(17) 0.22976(15) 0.0175(5) Uani 1 1 d . . .
O4 O 0.41030(17) 0.68138(17) 0.24917(15) 0.0157(5) Uani 1 1 d . . .
O5 O 0.35484(17) 0.43553(17) 0.39179(15) 0.0157(5) Uani 1 1 d . . .
O6 O 0.48190(17) 0.60738(17) 0.48006(15) 0.0137(5) Uani 1 1 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
Ho1 0.01204(8) 0.01273(7) 0.01521(9) -0.00465(6) -0.00120(6) -0.00453(6)
Ho2 0.01092(8) 0.01066(7) 0.01352(9) -0.00380(6) 0.00003(6) -0.00428(6)
C1 0.0164(18) 0.0153(15) 0.0135(18) -0.0022(13) -0.0044(14) -0.0051(13)
C2 0.0171(18) 0.0243(17) 0.0167(19) -0.0044(15) 0.0002(15) -0.0100(15)
C3 0.021(2) 0.031(2) 0.025(2) -0.0027(17) -0.0011(16) -0.0150(16)
C4 0.019(2) 0.037(2) 0.022(2) -0.0088(17) 0.0021(16) -0.0092(17)
C5 0.0168(19) 0.0219(17) 0.021(2) -0.0072(15) -0.0014(15) -0.0010(14)
C6 0.0147(17) 0.0193(16) 0.0154(18) -0.0046(14) -0.0067(14) -0.0012(13)
C7 0.0193(18) 0.0146(15) 0.0206(19) -0.0097(14) -0.0057(15) -0.0002(13)
C8 0.033(2) 0.0151(16) 0.021(2) -0.0073(14) -0.0033(16) -0.0111(15)
C9 0.023(2) 0.0244(18) 0.025(2) -0.0075(16) 0.0007(16) -0.0168(15)
C10 0.0184(19) 0.0186(16) 0.024(2) -0.0042(15) -0.0008(16) -0.0083(14)
C11 0.027(2) 0.0159(16) 0.0126(18) -0.0016(14) -0.0033(15) -0.0030(15)
C12 0.036(2) 0.0249(19) 0.023(2) -0.0050(17) 0.0030(18) -0.0099(17)
C13 0.050(3) 0.027(2) 0.015(2) -0.0013(17) 0.0057(19) -0.0080(19)
C14 0.038(2) 0.030(2) 0.018(2) -0.0093(17) -0.0080(18) 0.0001(18)
C15 0.029(2) 0.0265(19) 0.020(2) -0.0098(16) -0.0074(17) -0.0022(16)
C16 0.0214(19) 0.0159(16) 0.019(2) -0.0038(15) -0.0039(16) -0.0012(14)
C17 0.0139(17) 0.0203(16) 0.0124(18) -0.0024(14) -0.0044(14) -0.0048(14)
C18 0.0193(19) 0.0197(17) 0.026(2) -0.0088(15) -0.0006(16) -0.0078(14)
C19 0.021(2) 0.0236(18) 0.028(2) -0.0119(16) -0.0024(17) -0.0041(15)
C20 0.021(2) 0.035(2) 0.025(2) -0.0159(18) 0.0074(16) -0.0098(17)
C21 0.022(2) 0.0282(19) 0.023(2) -0.0060(16) -0.0006(16) -0.0128(16)
C22 0.0112(17) 0.0237(17) 0.0151(18) -0.0056(14) -0.0017(14) -0.0069(14)
C23 0.0175(18) 0.0240(17) 0.0175(19) -0.0038(15) -0.0001(15) -0.0125(15)
C24 0.0184(19) 0.0154(16) 0.036(2) -0.0088(16) -0.0016(16) -0.0099(14)
C25 0.0205(19) 0.0205(17) 0.033(2) -0.0139(16) -0.0034(17) -0.0064(15)
C26 0.0209(19) 0.0186(16) 0.024(2) -0.0109(15) -0.0062(16) -0.0004(14)
C27 0.0197(19) 0.0186(16) 0.0170(19) -0.0066(15) 0.0008(15) -0.0008(14)
C28 0.026(2) 0.028(2) 0.019(2) -0.0078(16) -0.0004(17) -0.0003(16)
C29 0.028(2) 0.030(2) 0.022(2) -0.0081(17) 0.0067(18) -0.0023(17)
C30 0.022(2) 0.0265(19) 0.024(2) -0.0012(17) 0.0089(17) -0.0064(16)
C31 0.024(2) 0.0177(17) 0.019(2) -0.0004(15) -0.0025(16) -0.0059(15)
C32 0.0135(17) 0.0147(15) 0.0148(18) -0.0005(14) -0.0005(14) -0.0003(13)
C33 0.0193(18) 0.0121(14) 0.0180(19) -0.0035(13) -0.0099(15) -0.0028(13)
C34 0.0187(18) 0.0149(15) 0.023(2) -0.0027(14) -0.0037(15) -0.0068(14)
C35 0.026(2) 0.0233(18) 0.033(2) -0.0094(17) -0.0028(17) -0.0161(16)
C36 0.029(2) 0.028(2) 0.045(3) -0.0244(19) 0.0020(19) -0.0152(17)
C37 0.027(2) 0.0249(18) 0.030(2) -0.0148(16) -0.0015(17) -0.0106(16)
C38 0.0191(18) 0.0133(15) 0.0152(18) -0.0037(13) -0.0046(14) -0.0058(13)
C39 0.0206(19) 0.0167(16) 0.0182(19) -0.0083(14) -0.0045(15) -0.0019(14)
C40 0.0143(17) 0.0180(16) 0.0187(19) -0.0069(14) 0.0025(14) -0.0061(13)
C41 0.0143(17) 0.0171(16) 0.024(2) -0.0085(15) 0.0012(15) -0.0064(13)
C42 0.0127(17) 0.0163(15) 0.0195(19) -0.0046(14) -0.0016(14) -0.0059(13)
C43 0.0158(18) 0.0141(15) 0.0160(18) -0.0022(13) -0.0029(14) -0.0065(13)
C44 0.0104(16) 0.0199(16) 0.0174(18) -0.0053(14) 0.0049(14) -0.0090(13)
C45 0.0195(18) 0.0127(15) 0.024(2) -0.0032(14) -0.0042(15) -0.0089(13)
C46 0.0199(18) 0.0126(15) 0.0223(19) -0.0075(14) -0.0011(15) -0.0059(13)
C47 0.0149(17) 0.0154(15) 0.0141(18) -0.0029(13) 0.0018(14) -0.0063(13)
C48 0.0120(16) 0.0117(14) 0.0152(18) -0.0003(13) -0.0046(14) -0.0044(12)
N1 0.0181(15) 0.0152(13) 0.0174(16) -0.0036(12) -0.0059(12) -0.0052(11)
N2 0.0159(15) 0.0152(13) 0.0185(16) -0.0061(12) 0.0010(12) -0.0068(11)
N3 0.0155(15) 0.0160(13) 0.0203(16) -0.0042(12) -0.0057(12) -0.0054(11)
N4 0.0223(16) 0.0159(13) 0.0240(17) -0.0072(12) -0.0082(13) -0.0053(12)
N5 0.0143(14) 0.0120(12) 0.0140(15) -0.0036(11) -0.0005(12) -0.0046(11)
N6 0.0107(14) 0.0145(13) 0.0157(15) -0.0039(11) -0.0015(12) -0.0029(11)
O1 0.0111(11) 0.0137(10) 0.0141(12) -0.0043(9) 0.0027(9) -0.0044(9)
O2 0.0247(14) 0.0192(12) 0.0169(13) -0.0037(10) -0.0044(11) -0.0070(10)
O3 0.0122(12) 0.0177(11) 0.0183(13) -0.0036(10) 0.0008(10) -0.0045(9)
O4 0.0135(12) 0.0159(11) 0.0142(12) -0.0043(9) 0.0027(10) -0.0047(9)
O5 0.0139(12) 0.0132(11) 0.0199(13) -0.0058(10) -0.0002(10) -0.0051(9)
O6 0.0145(12) 0.0115(10) 0.0156(12) -0.0034(9) -0.0005(10) -0.0067(9)
_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
Ho1 O2 2.229(2) . ?
Ho1 O3 2.251(2) . ?
Ho1 O4 2.364(2) . ?
Ho1 O1 2.372(2) . ?
Ho1 N2 2.484(3) . ?
Ho1 N3 2.487(3) . ?
Ho1 N1 2.504(3) . ?
Ho1 N4 2.526(3) . ?
Ho1 Ho2 3.8144(2) . ?
Ho2 O5 2.182(2) . ?
Ho2 O1 2.306(2) . ?
Ho2 O4 2.308(2) . ?
Ho2 O6 2.318(2) . ?
Ho2 O6 2.345(2) 2_666 ?
Ho2 N6 2.468(3) . ?
Ho2 N5 2.501(2) . ?
Ho2 Ho2 3.8278(3) 2_666 ?
C1 O1 1.335(4) . ?
C1 C2 1.408(4) . ?
C1 C6 1.422(4) . ?
C2 C3 1.382(5) . ?
C3 C4 1.396(5) . ?
C4 C5 1.378(5) . ?
C5 C6 1.392(5) . ?
C6 C7 1.466(5) . ?
C7 N1 1.271(4) . ?
C8 N1 1.459(4) . ?
C8 C9 1.517(5) . ?
C9 N2 1.472(4) . ?
C10 N2 1.280(4) . ?
C10 C11 1.443(4) . ?
C11 C12 1.409(5) . ?
C11 C16 1.419(5) . ?
C12 C13 1.365(5) . ?
C13 C14 1.401(6) . ?
C14 C15 1.363(5) . ?
C15 C16 1.402(5) . ?
C16 O2 1.315(4) . ?
C17 O3 1.305(4) . ?
C17 C18 1.421(4) . ?
C17 C22 1.421(4) . ?
C18 C19 1.372(5) . ?
C19 C20 1.386(5) . ?
C20 C21 1.377(5) . ?
C21 C22 1.388(5) . ?
C22 C23 1.456(4) . ?
C23 N3 1.276(4) . ?
C24 N3 1.473(4) . ?
C24 C25 1.509(5) . ?
C25 N4 1.473(4) . ?
C26 N4 1.281(4) . ?
C26 C27 1.447(5) . ?
C27 C28 1.405(5) . ?
C27 C32 1.412(5) . ?
C28 C29 1.378(5) . ?
C29 C30 1.374(5) . ?
C30 C31 1.392(5) . ?
C31 C32 1.400(5) . ?
C32 O4 1.355(4) . ?
C33 O5 1.298(3) . ?
C33 C38 1.421(4) . ?
C33 C34 1.423(5) . ?
C34 C35 1.369(4) . ?
C35 C36 1.399(5) . ?
C36 C37 1.372(5) . ?
C37 C38 1.418(4) . ?
C38 C39 1.420(5) . ?
C39 N5 1.302(4) . ?
C40 N5 1.460(4) . ?
C40 C41 1.506(4) . ?
C41 N6 1.473(4) . ?
C42 N6 1.275(4) . ?
C42 C43 1.469(4) . ?
C43 C44 1.399(4) . ?
C43 C48 1.404(4) . ?
C44 C45 1.385(4) . ?
C45 C46 1.377(5) . ?
C46 C47 1.385(4) . ?
C47 C48 1.400(4) . ?
C48 O6 1.348(3) . ?
O6 Ho2 2.345(2) 2_666 ?
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 Ho1 O3 79.65(8) . . ?
O2 Ho1 O4 100.91(8) . . ?
O3 Ho1 O4 162.69(8) . . ?
O2 Ho1 O1 158.43(7) . . ?
O3 Ho1 O1 116.28(8) . . ?
O4 Ho1 O1 68.43(8) . . ?
O2 Ho1 N2 73.19(9) . . ?
O3 Ho1 N2 87.48(8) . . ?
O4 Ho1 N2 76.29(8) . . ?
O1 Ho1 N2 119.64(8) . . ?
O2 Ho1 N3 97.98(9) . . ?
O3 Ho1 N3 72.64(8) . . ?
O4 Ho1 N3 123.97(8) . . ?
O1 Ho1 N3 74.96(8) . . ?
N2 Ho1 N3 159.56(9) . . ?
O2 Ho1 N1 131.89(8) . . ?
O3 Ho1 N1 71.85(8) . . ?
O4 Ho1 N1 96.05(8) . . ?
O1 Ho1 N1 69.22(8) . . ?
N2 Ho1 N1 67.72(9) . . ?
N3 Ho1 N1 108.97(9) . . ?
O2 Ho1 N4 72.30(8) . . ?
O3 Ho1 N4 125.89(8) . . ?
O4 Ho1 N4 69.78(8) . . ?
O1 Ho1 N4 86.26(8) . . ?
N2 Ho1 N4 124.91(9) . . ?
N3 Ho1 N4 66.86(9) . . ?
N1 Ho1 N4 155.07(9) . . ?
O2 Ho1 Ho2 129.32(6) . . ?
O3 Ho1 Ho2 150.70(6) . . ?
O4 Ho1 Ho2 34.77(5) . . ?
O1 Ho1 Ho2 34.80(5) . . ?
N2 Ho1 Ho2 103.95(6) . . ?
N3 Ho1 Ho2 95.91(6) . . ?
N1 Ho1 Ho2 87.43(6) . . ?
N4 Ho1 Ho2 69.15(6) . . ?
O5 Ho2 O1 80.48(7) . . ?
O5 Ho2 O4 109.96(8) . . ?
O1 Ho2 O4 70.51(8) . . ?
O5 Ho2 O6 137.81(8) . . ?
O1 Ho2 O6 85.48(7) . . ?
O4 Ho2 O6 102.23(7) . . ?
O5 Ho2 O6 82.47(7) . 2_666 ?
O1 Ho2 O6 118.27(8) . 2_666 ?
O4 Ho2 O6 166.46(7) . 2_666 ?
O6 Ho2 O6 69.67(8) . 2_666 ?
O5 Ho2 N6 138.88(8) . . ?
O1 Ho2 N6 138.42(8) . . ?
O4 Ho2 N6 80.68(8) . . ?
O6 Ho2 N6 71.77(8) . . ?
O6 Ho2 N6 86.36(8) 2_666 . ?
O5 Ho2 N5 74.12(8) . . ?
O1 Ho2 N5 135.76(8) . . ?
O4 Ho2 N5 84.86(8) . . ?
O6 Ho2 N5 136.65(8) . . ?
O6 Ho2 N5 93.80(8) 2_666 . ?
N6 Ho2 N5 67.29(8) . . ?
O5 Ho2 Ho1 89.99(5) . . ?
O1 Ho2 Ho1 35.95(5) . . ?
O4 Ho2 Ho1 35.74(5) . . ?
O6 Ho2 Ho1 101.42(5) . . ?
O6 Ho2 Ho1 154.21(5) 2_666 . ?
N6 Ho2 Ho1 114.54(6) . . ?
N5 Ho2 Ho1 107.85(6) . . ?
O5 Ho2 Ho2 111.62(6) . 2_666 ?
O1 Ho2 Ho2 104.03(5) . 2_666 ?
O4 Ho2 Ho2 136.38(5) . 2_666 ?
O6 Ho2 Ho2 35.07(5) . 2_666 ?
O6 Ho2 Ho2 34.60(5) 2_666 2_666 ?
N6 Ho2 Ho2 76.80(6) . 2_666 ?
N5 Ho2 Ho2 118.75(6) . 2_666 ?
Ho1 Ho2 Ho2 132.193(6) . 2_666 ?
O1 C1 C2 120.6(3) . . ?
O1 C1 C6 121.6(3) . . ?
C2 C1 C6 117.8(3) . . ?
C3 C2 C1 120.7(3) . . ?
C2 C3 C4 121.3(3) . . ?
C5 C4 C3 118.5(3) . . ?
C4 C5 C6 121.8(3) . . ?
C5 C6 C1 119.9(3) . . ?
C5 C6 C7 118.1(3) . . ?
C1 C6 C7 122.0(3) . . ?
N1 C7 C6 123.9(3) . . ?
N1 C8 C9 108.0(3) . . ?
N2 C9 C8 107.8(3) . . ?
N2 C10 C11 126.9(3) . . ?
C12 C11 C16 119.2(3) . . ?
C12 C11 C10 116.8(3) . . ?
C16 C11 C10 123.9(3) . . ?
C13 C12 C11 121.7(4) . . ?
C12 C13 C14 118.9(4) . . ?
C15 C14 C13 120.8(4) . . ?
C14 C15 C16 121.9(4) . . ?
O2 C16 C15 120.7(3) . . ?
O2 C16 C11 121.7(3) . . ?
C15 C16 C11 117.6(3) . . ?
O3 C17 C18 120.6(3) . . ?
O3 C17 C22 122.4(3) . . ?
C18 C17 C22 117.0(3) . . ?
C19 C18 C17 121.4(3) . . ?
C18 C19 C20 121.1(3) . . ?
C21 C20 C19 118.5(3) . . ?
C20 C21 C22 122.4(3) . . ?
C21 C22 C17 119.6(3) . . ?
C21 C22 C23 117.7(3) . . ?
C17 C22 C23 122.8(3) . . ?
N3 C23 C22 126.6(3) . . ?
N3 C24 C25 109.4(3) . . ?
N4 C25 C24 108.4(3) . . ?
N4 C26 C27 124.3(3) . . ?
C28 C27 C32 118.4(3) . . ?
C28 C27 C26 118.6(3) . . ?
C32 C27 C26 123.0(3) . . ?
C29 C28 C27 121.8(4) . . ?
C30 C29 C28 119.5(4) . . ?
C29 C30 C31 120.5(4) . . ?
C30 C31 C32 120.8(3) . . ?
O4 C32 C31 120.0(3) . . ?
O4 C32 C27 121.1(3) . . ?
C31 C32 C27 118.9(3) . . ?
O5 C33 C38 122.1(3) . . ?
O5 C33 C34 120.2(3) . . ?
C38 C33 C34 117.7(3) . . ?
C35 C34 C33 121.0(3) . . ?
C34 C35 C36 121.3(3) . . ?
C37 C36 C35 119.3(3) . . ?
C36 C37 C38 121.2(3) . . ?
C37 C38 C39 116.7(3) . . ?
C37 C38 C33 119.5(3) . . ?
C39 C38 C33 123.7(3) . . ?
N5 C39 C38 128.5(3) . . ?
N5 C40 C41 109.5(3) . . ?
N6 C41 C40 109.5(3) . . ?
N6 C42 C43 125.0(3) . . ?
C44 C43 C48 119.8(3) . . ?
C44 C43 C42 117.0(3) . . ?
C48 C43 C42 123.1(3) . . ?
C45 C44 C43 120.8(3) . . ?
C46 C45 C44 119.4(3) . . ?
C45 C46 C47 120.7(3) . . ?
C46 C47 C48 121.0(3) . . ?
O6 C48 C47 119.6(3) . . ?
O6 C48 C43 121.9(3) . . ?
C47 C48 C43 118.3(3) . . ?
C7 N1 C8 118.6(3) . . ?
C7 N1 Ho1 125.0(2) . . ?
C8 N1 Ho1 114.7(2) . . ?
C10 N2 C9 116.3(3) . . ?
C10 N2 Ho1 129.8(2) . . ?
C9 N2 Ho1 113.8(2) . . ?
C23 N3 C24 116.9(3) . . ?
C23 N3 Ho1 127.8(2) . . ?
C24 N3 Ho1 114.5(2) . . ?
C26 N4 C25 119.2(3) . . ?
C26 N4 Ho1 121.4(2) . . ?
C25 N4 Ho1 117.0(2) . . ?
C39 N5 C40 116.2(3) . . ?
C39 N5 Ho2 127.6(2) . . ?
C40 N5 Ho2 116.20(18) . . ?
C42 N6 C41 117.1(3) . . ?
C42 N6 Ho2 125.4(2) . . ?
C41 N6 Ho2 116.80(19) . . ?
C1 O1 Ho2 132.64(19) . . ?
C1 O1 Ho1 118.11(18) . . ?
Ho2 O1 Ho1 109.25(9) . . ?
C16 O2 Ho1 139.8(2) . . ?
C17 O3 Ho1 132.9(2) . . ?
C32 O4 Ho2 129.29(18) . . ?
C32 O4 Ho1 111.65(18) . . ?
Ho2 O4 Ho1 109.49(9) . . ?
C33 O5 Ho2 143.5(2) . . ?
C48 O6 Ho2 120.72(18) . . ?
C48 O6 Ho2 121.78(18) . 2_666 ?
Ho2 O6 Ho2 110.33(8) . 2_666 ?
_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.276
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.150
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 -0.027 0.000 508.4 195.1
_platon_squeeze_details          
;
;


data_squeezed
_database_code_depnum_ccdc_archive 'CCDC 878594'
#TrackingRef 'cif-complex3.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H84 Eu4 N12 O12'
_chemical_formula_weight         2205.59
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'
Eu Eu -0.1578 3.6682 '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                   13.5175(3)
_cell_length_b                   14.1326(3)
_cell_length_c                   15.6344(3)
_cell_angle_alpha                69.8550(10)
_cell_angle_beta                 79.2150(10)
_cell_angle_gamma                62.7980(10)
_cell_volume                     2492.34(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6692
_cell_measurement_theta_min      2.229
_cell_measurement_theta_max      25.328
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1092
_exptl_absorpt_coefficient_mu    2.543
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.7535
_exptl_absorpt_correction_T_max  0.9253
_exptl_absorpt_process_details   SADABS
_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  'CCD area detector'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41673
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0887
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         28.41
_reflns_number_total             11870
_reflns_number_gt                8283
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker SMART APEXll'
_computing_cell_refinement       'Bruker SMART APEXll'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    WingX
_computing_publication_material  WingX
_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^)+(0.0316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11870
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.0861
_refine_ls_wR_factor_gt          0.0791
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_restrained_S_all      0.948
_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
Eu2 Eu 0.940942(18) 0.536632(18) 0.382018(16) 0.01648(7) Uani 1 1 d . . .
Eu1 Eu 0.711278(18) 0.803260(19) 0.235796(16) 0.01765(7) Uani 1 1 d . . .
N1 N 0.7026(3) 0.9012(3) 0.3493(3) 0.0209(9) Uani 1 1 d . . .
N2 N 0.8011(3) 0.9390(3) 0.1743(3) 0.0201(9) Uani 1 1 d . . .
N3 N 0.5649(3) 0.7273(3) 0.2862(3) 0.0223(9) Uani 1 1 d . . .
N4 N 0.7568(3) 0.6322(3) 0.1850(3) 0.0208(9) Uani 1 1 d . . .
N5 N 1.0531(3) 0.4088(3) 0.2831(2) 0.0181(9) Uani 1 1 d . . .
N6 N 1.1348(3) 0.5244(3) 0.3411(2) 0.0169(8) Uani 1 1 d . . .
O1 O 0.7589(2) 0.6746(2) 0.3865(2) 0.0185(7) Uani 1 1 d . . .
O2 O 0.7033(3) 0.8652(3) 0.0817(2) 0.0250(8) Uani 1 1 d . . .
O3 O 0.5405(2) 0.9497(2) 0.2249(2) 0.0219(8) Uani 1 1 d . . .
O4 O 0.9075(2) 0.6801(2) 0.24357(19) 0.0167(7) Uani 1 1 d . . .
O5 O 0.8501(2) 0.4383(2) 0.3860(2) 0.0200(7) Uani 1 1 d . . .
O6 O 0.9850(2) 0.6073(2) 0.4794(2) 0.0169(7) Uani 1 1 d . . .
C1 C 0.6837(4) 0.6887(4) 0.4558(3) 0.0184(10) Uani 1 1 d . . .
C2 C 0.6522(4) 0.6042(4) 0.5067(3) 0.0246(12) Uani 1 1 d . . .
H2 H 0.6864 0.5349 0.4935 0.029 Uiso 1 1 calc R . .
C3 C 0.5709(4) 0.6192(4) 0.5769(3) 0.0278(12) Uani 1 1 d . . .
H3 H 0.5482 0.5615 0.6095 0.033 Uiso 1 1 calc R . .
C4 C 0.5229(4) 0.7194(4) 0.5990(3) 0.0304(13) Uani 1 1 d . . .
H4 H 0.4681 0.7299 0.6470 0.036 Uiso 1 1 calc R . .
C5 C 0.5551(4) 0.8007(4) 0.5517(3) 0.0244(11) Uani 1 1 d . . .
H5 H 0.5238 0.8675 0.5683 0.029 Uiso 1 1 calc R . .
C6 C 0.6334(4) 0.7902(4) 0.4786(3) 0.0221(11) Uani 1 1 d . . .
C7 C 0.6626(4) 0.8835(4) 0.4307(3) 0.0203(11) Uani 1 1 d . . .
H7A H 0.6509 0.9344 0.4625 0.024 Uiso 1 1 calc R . .
C8 C 0.7276(4) 0.9985(4) 0.3097(3) 0.0274(12) Uani 1 1 d . . .
H8A H 0.7437 1.0187 0.3585 0.033 Uiso 1 1 calc R . .
H8B H 0.6630 1.0630 0.2763 0.033 Uiso 1 1 calc R . .
C9 C 0.8271(4) 0.9688(4) 0.2457(3) 0.0303(13) Uani 1 1 d . . .
H9A H 0.8464 1.0329 0.2179 0.036 Uiso 1 1 calc R . .
H9B H 0.8918 0.9052 0.2797 0.036 Uiso 1 1 calc R . .
C10 C 0.8296(4) 0.9810(4) 0.0928(3) 0.0222(11) Uani 1 1 d . . .
H10 H 0.8645 1.0285 0.0851 0.027 Uiso 1 1 calc R . .
C11 C 0.8144(4) 0.9643(4) 0.0109(3) 0.0224(11) Uani 1 1 d . . .
C12 C 0.8673(4) 1.0075(4) -0.0709(3) 0.0306(13) Uani 1 1 d . . .
H12 H 0.9103 1.0443 -0.0690 0.037 Uiso 1 1 calc R . .
C13 C 0.8567(4) 0.9966(4) -0.1517(4) 0.0352(14) Uani 1 1 d . . .
H13 H 0.8933 1.0243 -0.2056 0.042 Uiso 1 1 calc R . .
C14 C 0.7925(5) 0.9451(4) -0.1542(4) 0.0375(15) Uani 1 1 d . . .
H14 H 0.7832 0.9398 -0.2109 0.045 Uiso 1 1 calc R . .
C15 C 0.7414(4) 0.9010(4) -0.0767(3) 0.0296(13) Uani 1 1 d . . .
H15 H 0.6982 0.8655 -0.0809 0.036 Uiso 1 1 calc R . .
C16 C 0.7519(4) 0.9075(4) 0.0081(3) 0.0248(12) Uani 1 1 d . . .
C17 C 0.4523(4) 0.9683(4) 0.2809(3) 0.0209(11) Uani 1 1 d . . .
C18 C 0.3903(4) 1.0749(4) 0.2937(3) 0.0262(12) Uani 1 1 d . . .
H18 H 0.4124 1.1331 0.2612 0.031 Uiso 1 1 calc R . .
C19 C 0.2988(4) 1.0958(4) 0.3525(3) 0.0287(12) Uani 1 1 d . . .
H19 H 0.2599 1.1675 0.3612 0.034 Uiso 1 1 calc R . .
C20 C 0.2626(4) 1.0142(4) 0.3990(3) 0.0269(12) Uani 1 1 d . . .
H20 H 0.1987 1.0297 0.4389 0.032 Uiso 1 1 calc R . .
C21 C 0.3198(4) 0.9101(4) 0.3870(3) 0.0259(12) Uani 1 1 d . . .
H21 H 0.2946 0.8541 0.4187 0.031 Uiso 1 1 calc R . .
C22 C 0.4143(4) 0.8854(4) 0.3293(3) 0.0200(11) Uani 1 1 d . . .
C23 C 0.4687(4) 0.7719(4) 0.3214(3) 0.0228(11) Uani 1 1 d . . .
H23 H 0.4282 0.7277 0.3448 0.027 Uiso 1 1 calc R . .
C24 C 0.6057(4) 0.6096(4) 0.2896(3) 0.0248(11) Uani 1 1 d . . .
H24A H 0.5420 0.5903 0.2983 0.030 Uiso 1 1 calc R . .
H24B H 0.6549 0.5605 0.3417 0.030 Uiso 1 1 calc R . .
C25 C 0.6694(4) 0.5917(4) 0.2015(3) 0.0242(11) Uani 1 1 d . . .
H25A H 0.7038 0.5116 0.2060 0.029 Uiso 1 1 calc R . .
H25B H 0.6181 0.6330 0.1502 0.029 Uiso 1 1 calc R . .
C26 C 0.8364(4) 0.5986(4) 0.1312(3) 0.0267(12) Uani 1 1 d . . .
H26 H 0.8401 0.5444 0.1063 0.032 Uiso 1 1 calc R . .
C27 C 0.9246(4) 0.6379(4) 0.1040(3) 0.0235(11) Uani 1 1 d . . .
C28 C 0.9786(4) 0.6352(4) 0.0186(3) 0.0272(12) Uani 1 1 d . . .
H28 H 0.9605 0.6044 -0.0182 0.033 Uiso 1 1 calc R . .
C29 C 1.0582(4) 0.6766(4) -0.0131(3) 0.0300(13) Uani 1 1 d . . .
H29 H 1.0920 0.6770 -0.0721 0.036 Uiso 1 1 calc R . .
C30 C 1.0882(4) 0.7173(4) 0.0417(3) 0.0283(12) Uani 1 1 d . . .
H30 H 1.1440 0.7441 0.0210 0.034 Uiso 1 1 calc R . .
C31 C 1.0371(4) 0.7190(4) 0.1264(3) 0.0241(11) Uani 1 1 d . . .
H31 H 1.0578 0.7480 0.1630 0.029 Uiso 1 1 calc R . .
C32 C 0.9551(4) 0.6789(4) 0.1602(3) 0.0215(11) Uani 1 1 d . . .
C33 C 0.8565(4) 0.3543(4) 0.3653(3) 0.0175(10) Uani 1 1 d . . .
C34 C 0.7765(4) 0.3114(4) 0.3991(3) 0.0211(11) Uani 1 1 d . . .
H34 H 0.7162 0.3460 0.4366 0.025 Uiso 1 1 calc R . .
C35 C 0.7829(4) 0.2212(4) 0.3796(3) 0.0259(12) Uani 1 1 d . . .
H35 H 0.7281 0.1936 0.4045 0.031 Uiso 1 1 calc R . .
C36 C 0.8692(4) 0.1698(4) 0.3236(4) 0.0318(13) Uani 1 1 d . . .
H36 H 0.8735 0.1075 0.3099 0.038 Uiso 1 1 calc R . .
C37 C 0.9475(4) 0.2100(4) 0.2885(3) 0.0262(12) Uani 1 1 d . . .
H37 H 1.0066 0.1742 0.2506 0.031 Uiso 1 1 calc R . .
C38 C 0.9438(4) 0.3020(4) 0.3063(3) 0.0193(10) Uani 1 1 d . . .
C39 C 1.0347(4) 0.3334(4) 0.2694(3) 0.0199(11) Uani 1 1 d . . .
H39 H 1.0871 0.2936 0.2303 0.024 Uiso 1 1 calc R . .
C40 C 1.1541(4) 0.4205(4) 0.2374(3) 0.0195(11) Uani 1 1 d . . .
H40A H 1.1341 0.4860 0.1824 0.023 Uiso 1 1 calc R . .
H40B H 1.2044 0.3534 0.2183 0.023 Uiso 1 1 calc R . .
C41 C 1.2123(4) 0.4348(4) 0.3030(3) 0.0210(11) Uani 1 1 d . . .
H41A H 1.2429 0.3644 0.3529 0.025 Uiso 1 1 calc R . .
H41B H 1.2750 0.4522 0.2705 0.025 Uiso 1 1 calc R . .
C42 C 1.1660(4) 0.5970(4) 0.3409(3) 0.0168(10) Uani 1 1 d . . .
H42 H 1.2369 0.5905 0.3137 0.020 Uiso 1 1 calc R . .
C43 C 1.1008(4) 0.6900(4) 0.3796(3) 0.0183(10) Uani 1 1 d . . .
C44 C 1.1331(4) 0.7772(4) 0.3527(3) 0.0210(11) Uani 1 1 d . . .
H44 H 1.1940 0.7739 0.3103 0.025 Uiso 1 1 calc R . .
C45 C 1.0797(4) 0.8673(4) 0.3855(3) 0.0202(11) Uani 1 1 d . . .
H45 H 1.1023 0.9262 0.3654 0.024 Uiso 1 1 calc R . .
C46 C 0.9914(4) 0.8709(4) 0.4490(3) 0.0220(11) Uani 1 1 d . . .
H46 H 0.9530 0.9330 0.4721 0.026 Uiso 1 1 calc R . .
C47 C 0.9599(4) 0.7845(4) 0.4782(3) 0.0209(11) Uani 1 1 d . . .
H47 H 0.9000 0.7880 0.5217 0.025 Uiso 1 1 calc R . .
C48 C 1.0135(4) 0.6916(4) 0.4456(3) 0.0165(10) Uani 1 1 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
Eu2 0.01393(13) 0.01318(13) 0.02176(14) -0.00574(10) 0.00064(10) -0.00536(10)
Eu1 0.01441(13) 0.01503(13) 0.02361(15) -0.00673(11) -0.00006(10) -0.00585(10)
N1 0.021(2) 0.018(2) 0.022(2) -0.0058(18) -0.0006(18) -0.0072(18)
N2 0.020(2) 0.023(2) 0.018(2) -0.0072(18) -0.0013(17) -0.0085(18)
N3 0.016(2) 0.017(2) 0.031(2) -0.0074(18) 0.0012(18) -0.0050(18)
N4 0.021(2) 0.015(2) 0.025(2) -0.0065(18) -0.0021(18) -0.0058(18)
N5 0.013(2) 0.015(2) 0.022(2) -0.0036(17) -0.0019(16) -0.0034(17)
N6 0.014(2) 0.0116(19) 0.020(2) -0.0032(16) -0.0026(16) -0.0021(16)
O1 0.0138(17) 0.0175(17) 0.0228(18) -0.0095(14) 0.0061(14) -0.0053(14)
O2 0.028(2) 0.0228(19) 0.0198(19) -0.0025(15) -0.0061(15) -0.0082(16)
O3 0.0123(17) 0.0171(17) 0.0292(19) -0.0038(15) 0.0007(14) -0.0031(14)
O4 0.0157(17) 0.0148(16) 0.0168(17) -0.0052(13) 0.0037(13) -0.0054(14)
O5 0.0179(17) 0.0166(17) 0.0264(19) -0.0100(15) 0.0004(14) -0.0059(14)
O6 0.0166(17) 0.0145(16) 0.0192(17) -0.0047(14) 0.0003(13) -0.0069(14)
C1 0.013(2) 0.018(3) 0.020(3) -0.002(2) -0.002(2) -0.005(2)
C2 0.023(3) 0.025(3) 0.030(3) -0.006(2) -0.001(2) -0.014(2)
C3 0.024(3) 0.040(3) 0.024(3) -0.006(2) 0.002(2) -0.021(3)
C4 0.023(3) 0.038(3) 0.026(3) -0.007(3) 0.007(2) -0.014(3)
C5 0.016(3) 0.027(3) 0.025(3) -0.012(2) 0.000(2) -0.002(2)
C6 0.019(3) 0.020(3) 0.023(3) -0.003(2) -0.004(2) -0.005(2)
C7 0.021(3) 0.018(2) 0.020(3) -0.008(2) -0.001(2) -0.005(2)
C8 0.041(3) 0.018(3) 0.027(3) -0.008(2) -0.001(2) -0.014(2)
C9 0.035(3) 0.034(3) 0.032(3) -0.008(3) 0.003(2) -0.026(3)
C10 0.019(3) 0.020(3) 0.028(3) -0.007(2) 0.004(2) -0.011(2)
C11 0.018(3) 0.023(3) 0.014(3) -0.003(2) -0.002(2) 0.000(2)
C12 0.029(3) 0.024(3) 0.033(3) -0.004(2) 0.000(2) -0.010(2)
C13 0.037(3) 0.030(3) 0.018(3) -0.002(2) 0.004(2) -0.003(3)
C14 0.038(3) 0.030(3) 0.027(3) -0.012(3) -0.007(3) 0.005(3)
C15 0.031(3) 0.034(3) 0.022(3) -0.011(2) -0.010(2) -0.007(3)
C16 0.025(3) 0.017(3) 0.020(3) -0.003(2) -0.008(2) 0.002(2)
C17 0.017(3) 0.020(3) 0.025(3) -0.005(2) -0.008(2) -0.006(2)
C18 0.022(3) 0.018(3) 0.036(3) -0.005(2) -0.004(2) -0.008(2)
C19 0.020(3) 0.026(3) 0.036(3) -0.013(2) -0.001(2) -0.004(2)
C20 0.017(3) 0.041(3) 0.027(3) -0.020(3) 0.006(2) -0.011(2)
C21 0.024(3) 0.025(3) 0.032(3) -0.006(2) -0.005(2) -0.013(2)
C22 0.016(2) 0.017(2) 0.022(3) -0.001(2) -0.007(2) -0.004(2)
C23 0.020(3) 0.025(3) 0.025(3) -0.003(2) -0.003(2) -0.014(2)
C24 0.020(3) 0.015(2) 0.039(3) -0.004(2) -0.003(2) -0.009(2)
C25 0.023(3) 0.014(2) 0.038(3) -0.010(2) -0.004(2) -0.007(2)
C26 0.029(3) 0.019(3) 0.032(3) -0.006(2) -0.012(2) -0.007(2)
C27 0.017(3) 0.020(3) 0.027(3) -0.006(2) -0.001(2) -0.002(2)
C28 0.024(3) 0.024(3) 0.026(3) -0.009(2) -0.005(2) -0.001(2)
C29 0.030(3) 0.026(3) 0.020(3) -0.002(2) 0.005(2) -0.006(2)
C30 0.022(3) 0.020(3) 0.036(3) -0.007(2) 0.003(2) -0.006(2)
C31 0.022(3) 0.022(3) 0.022(3) -0.008(2) 0.004(2) -0.006(2)
C32 0.017(3) 0.010(2) 0.030(3) 0.001(2) -0.004(2) -0.003(2)
C33 0.018(2) 0.013(2) 0.022(3) -0.004(2) -0.007(2) -0.005(2)
C34 0.019(3) 0.023(3) 0.025(3) -0.008(2) -0.002(2) -0.011(2)
C35 0.028(3) 0.021(3) 0.033(3) -0.009(2) -0.001(2) -0.014(2)
C36 0.036(3) 0.025(3) 0.047(4) -0.018(3) -0.001(3) -0.019(3)
C37 0.026(3) 0.020(3) 0.034(3) -0.013(2) 0.000(2) -0.008(2)
C38 0.017(2) 0.011(2) 0.029(3) -0.005(2) -0.005(2) -0.003(2)
C39 0.018(3) 0.019(3) 0.019(3) -0.006(2) -0.003(2) -0.004(2)
C40 0.017(2) 0.018(2) 0.021(3) -0.010(2) 0.005(2) -0.004(2)
C41 0.015(2) 0.018(3) 0.029(3) -0.010(2) 0.002(2) -0.005(2)
C42 0.013(2) 0.018(2) 0.019(3) -0.004(2) 0.0028(19) -0.008(2)
C43 0.012(2) 0.017(2) 0.023(3) -0.005(2) -0.004(2) -0.004(2)
C44 0.019(3) 0.025(3) 0.025(3) -0.009(2) 0.002(2) -0.014(2)
C45 0.020(3) 0.017(2) 0.026(3) -0.001(2) -0.004(2) -0.012(2)
C46 0.023(3) 0.021(3) 0.027(3) -0.012(2) -0.002(2) -0.010(2)
C47 0.017(3) 0.019(3) 0.025(3) -0.006(2) -0.001(2) -0.006(2)
C48 0.018(2) 0.014(2) 0.017(2) 0.0014(19) -0.0039(19) -0.008(2)
_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
Eu2 O5 2.218(3) . ?
Eu2 O1 2.346(3) . ?
Eu2 O4 2.347(3) . ?
Eu2 O6 2.366(3) . ?
Eu2 O6 2.398(3) 2_766 ?
Eu2 N6 2.519(4) . ?
Eu2 N5 2.548(4) . ?
Eu2 C48 3.252(4) . ?
Eu2 Eu1 3.8846(3) . ?
Eu2 Eu2 3.9106(5) 2_766 ?
Eu1 O2 2.267(3) . ?
Eu1 O3 2.276(3) . ?
Eu1 O1 2.413(3) . ?
Eu1 O4 2.415(3) . ?
Eu1 N3 2.543(4) . ?
Eu1 N2 2.550(4) . ?
Eu1 N1 2.558(4) . ?
Eu1 N4 2.575(4) . ?
Eu1 C32 3.166(5) . ?
N1 C7 1.273(5) . ?
N1 C8 1.466(6) . ?
N2 C10 1.276(5) . ?
N2 C9 1.468(6) . ?
N3 C23 1.271(5) . ?
N3 C24 1.478(5) . ?
N4 C26 1.249(6) . ?
N4 C25 1.480(5) . ?
N5 C39 1.291(5) . ?
N5 C40 1.470(5) . ?
N6 C42 1.274(5) . ?
N6 C41 1.459(5) . ?
O1 C1 1.341(5) . ?
O2 C16 1.310(5) . ?
O3 C17 1.318(5) . ?
O4 C32 1.344(5) . ?
O5 C33 1.296(5) . ?
O6 C48 1.326(5) . ?
O6 Eu2 2.398(3) 2_766 ?
C1 C2 1.387(6) . ?
C1 C6 1.419(6) . ?
C2 C3 1.398(6) . ?
C3 C4 1.399(7) . ?
C4 C5 1.344(6) . ?
C5 C6 1.403(6) . ?
C6 C7 1.463(6) . ?
C8 C9 1.503(6) . ?
C10 C11 1.446(6) . ?
C11 C16 1.420(7) . ?
C11 C12 1.427(6) . ?
C12 C13 1.364(7) . ?
C13 C14 1.378(7) . ?
C14 C15 1.376(7) . ?
C15 C16 1.399(6) . ?
C17 C22 1.415(6) . ?
C17 C18 1.416(6) . ?
C18 C19 1.374(6) . ?
C19 C20 1.380(7) . ?
C20 C21 1.375(6) . ?
C21 C22 1.395(6) . ?
C22 C23 1.467(6) . ?
C24 C25 1.516(6) . ?
C26 C27 1.471(7) . ?
C27 C28 1.401(6) . ?
C27 C32 1.408(6) . ?
C28 C29 1.386(7) . ?
C29 C30 1.383(7) . ?
C30 C31 1.376(6) . ?
C31 C32 1.406(6) . ?
C33 C34 1.407(6) . ?
C33 C38 1.433(6) . ?
C34 C35 1.373(6) . ?
C35 C36 1.392(6) . ?
C36 C37 1.364(6) . ?
C37 C38 1.400(6) . ?
C38 C39 1.447(6) . ?
C40 C41 1.517(6) . ?
C42 C43 1.469(6) . ?
C43 C44 1.396(6) . ?
C43 C48 1.412(6) . ?
C44 C45 1.370(6) . ?
C45 C46 1.395(6) . ?
C46 C47 1.379(6) . ?
C47 C48 1.400(6) . ?
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
O5 Eu2 O1 81.74(10) . . ?
O5 Eu2 O4 108.79(11) . . ?
O1 Eu2 O4 70.73(10) . . ?
O5 Eu2 O6 139.93(11) . . ?
O1 Eu2 O6 86.37(10) . . ?
O4 Eu2 O6 102.95(10) . . ?
O5 Eu2 O6 82.75(10) . 2_766 ?
O1 Eu2 O6 118.39(10) . 2_766 ?
O4 Eu2 O6 166.84(10) . 2_766 ?
O6 Eu2 O6 69.67(11) . 2_766 ?
O5 Eu2 N6 137.33(11) . . ?
O1 Eu2 N6 138.20(11) . . ?
O4 Eu2 N6 80.37(11) . . ?
O6 Eu2 N6 71.13(11) . . ?
O6 Eu2 N6 86.83(11) 2_766 . ?
O5 Eu2 N5 72.73(11) . . ?
O1 Eu2 N5 136.39(11) . . ?
O4 Eu2 N5 84.62(11) . . ?
O6 Eu2 N5 135.12(11) . . ?
O6 Eu2 N5 93.14(10) 2_766 . ?
N6 Eu2 N5 66.66(12) . . ?
O5 Eu2 C48 158.02(11) . . ?
O1 Eu2 C48 85.38(11) . . ?
O4 Eu2 C48 83.36(10) . . ?
O6 Eu2 C48 20.48(10) . . ?
O6 Eu2 C48 87.85(11) 2_766 . ?
N6 Eu2 C48 61.32(11) . . ?
N5 Eu2 C48 127.83(11) . . ?
O5 Eu2 Eu1 90.30(7) . . ?
O1 Eu2 Eu1 35.85(7) . . ?
O4 Eu2 Eu1 35.92(7) . . ?
O6 Eu2 Eu1 101.97(7) . . ?
O6 Eu2 Eu1 154.24(7) 2_766 . ?
N6 Eu2 Eu1 114.19(8) . . ?
N5 Eu2 Eu1 108.48(8) . . ?
C48 Eu2 Eu1 89.62(7) . . ?
O5 Eu2 Eu2 112.69(8) . 2_766 ?
O1 Eu2 Eu2 104.67(7) . 2_766 ?
O4 Eu2 Eu2 137.11(7) . 2_766 ?
O6 Eu2 Eu2 35.10(7) . 2_766 ?
O6 Eu2 Eu2 34.57(7) 2_766 2_766 ?
N6 Eu2 Eu2 76.72(8) . 2_766 ?
N5 Eu2 Eu2 117.54(8) . 2_766 ?
C48 Eu2 Eu2 53.85(7) . 2_766 ?
Eu1 Eu2 Eu2 132.667(10) . 2_766 ?
O2 Eu1 O3 81.98(11) . . ?
O2 Eu1 O1 159.11(10) . . ?
O3 Eu1 O1 115.63(10) . . ?
O2 Eu1 O4 97.06(10) . . ?
O3 Eu1 O4 166.67(10) . . ?
O1 Eu1 O4 68.48(9) . . ?
O2 Eu1 N3 103.65(12) . . ?
O3 Eu1 N3 71.69(11) . . ?
O1 Eu1 N3 73.70(11) . . ?
O4 Eu1 N3 121.20(11) . . ?
O2 Eu1 N2 71.36(12) . . ?
O3 Eu1 N2 89.66(11) . . ?
O1 Eu1 N2 117.47(11) . . ?
O4 Eu1 N2 77.51(11) . . ?
N3 Eu1 N2 161.29(12) . . ?
O2 Eu1 N1 130.44(12) . . ?
O3 Eu1 N1 73.18(11) . . ?
O1 Eu1 N1 68.42(11) . . ?
O4 Eu1 N1 98.01(11) . . ?
N3 Eu1 N1 107.94(12) . . ?
N2 Eu1 N1 66.42(12) . . ?
O2 Eu1 N4 74.10(11) . . ?
O3 Eu1 N4 123.77(11) . . ?
O1 Eu1 N4 86.23(11) . . ?
O4 Eu1 N4 68.13(11) . . ?
N3 Eu1 N4 66.03(12) . . ?
N2 Eu1 N4 126.91(12) . . ?
N1 Eu1 N4 154.41(12) . . ?
O2 Eu1 C32 73.82(12) . . ?
O3 Eu1 C32 152.75(11) . . ?
O1 Eu1 C32 90.76(10) . . ?
O4 Eu1 C32 23.25(10) . . ?
N3 Eu1 C32 125.81(12) . . ?
N2 Eu1 C32 71.04(12) . . ?
N1 Eu1 C32 113.70(12) . . ?
N4 Eu1 C32 61.29(12) . . ?
O2 Eu1 Eu2 127.35(8) . . ?
O3 Eu1 Eu2 150.28(8) . . ?
O1 Eu1 Eu2 34.72(7) . . ?
O4 Eu1 Eu2 34.75(7) . . ?
N3 Eu1 Eu2 93.86(8) . . ?
N2 Eu1 Eu2 103.47(8) . . ?
N1 Eu1 Eu2 87.63(8) . . ?
N4 Eu1 Eu2 68.64(8) . . ?
C32 Eu1 Eu2 56.14(8) . . ?
C7 N1 C8 118.6(4) . . ?
C7 N1 Eu1 125.5(3) . . ?
C8 N1 Eu1 114.9(3) . . ?
C10 N2 C9 116.2(4) . . ?
C10 N2 Eu1 130.2(3) . . ?
C9 N2 Eu1 113.5(3) . . ?
C23 N3 C24 116.9(4) . . ?
C23 N3 Eu1 127.6(3) . . ?
C24 N3 Eu1 114.5(3) . . ?
C26 N4 C25 118.4(4) . . ?
C26 N4 Eu1 122.5(3) . . ?
C25 N4 Eu1 117.2(3) . . ?
C39 N5 C40 115.6(4) . . ?
C39 N5 Eu2 128.7(3) . . ?
C40 N5 Eu2 115.7(3) . . ?
C42 N6 C41 117.8(4) . . ?
C42 N6 Eu2 125.1(3) . . ?
C41 N6 Eu2 116.6(3) . . ?
C1 O1 Eu2 130.8(3) . . ?
C1 O1 Eu1 119.7(2) . . ?
Eu2 O1 Eu1 109.43(11) . . ?
C16 O2 Eu1 142.0(3) . . ?
C17 O3 Eu1 132.1(3) . . ?
C32 O4 Eu2 130.5(3) . . ?
C32 O4 Eu1 111.6(2) . . ?
Eu2 O4 Eu1 109.33(11) . . ?
C33 O5 Eu2 144.5(3) . . ?
C48 O6 Eu2 120.9(3) . . ?
C48 O6 Eu2 121.9(3) . 2_766 ?
Eu2 O6 Eu2 110.33(11) . 2_766 ?
O1 C1 C2 120.5(4) . . ?
O1 C1 C6 121.2(4) . . ?
C2 C1 C6 118.3(4) . . ?
C1 C2 C3 121.1(5) . . ?
C2 C3 C4 119.9(5) . . ?
C5 C4 C3 119.4(5) . . ?
C4 C5 C6 122.3(5) . . ?
C5 C6 C1 119.0(4) . . ?
C5 C6 C7 118.4(4) . . ?
C1 C6 C7 122.6(4) . . ?
N1 C7 C6 124.5(4) . . ?
N1 C8 C9 107.8(4) . . ?
N2 C9 C8 109.1(4) . . ?
N2 C10 C11 127.2(5) . . ?
C16 C11 C12 119.5(5) . . ?
C16 C11 C10 123.9(4) . . ?
C12 C11 C10 116.6(5) . . ?
C13 C12 C11 120.7(5) . . ?
C12 C13 C14 119.3(5) . . ?
C15 C14 C13 121.7(5) . . ?
C14 C15 C16 121.2(5) . . ?
O2 C16 C15 120.9(5) . . ?
O2 C16 C11 121.6(4) . . ?
C15 C16 C11 117.5(5) . . ?
O3 C17 C22 122.7(4) . . ?
O3 C17 C18 120.1(4) . . ?
C22 C17 C18 117.2(4) . . ?
C19 C18 C17 121.1(5) . . ?
C18 C19 C20 121.0(5) . . ?
C21 C20 C19 119.4(5) . . ?
C20 C21 C22 121.2(5) . . ?
C21 C22 C17 120.1(4) . . ?
C21 C22 C23 116.6(4) . . ?
C17 C22 C23 123.3(4) . . ?
N3 C23 C22 125.9(4) . . ?
N3 C24 C25 109.7(4) . . ?
N4 C25 C24 108.8(4) . . ?
N4 C26 C27 123.9(5) . . ?
C28 C27 C32 119.4(5) . . ?
C28 C27 C26 118.3(5) . . ?
C32 C27 C26 122.3(4) . . ?
C29 C28 C27 121.1(5) . . ?
C30 C29 C28 119.7(5) . . ?
C31 C30 C29 119.9(5) . . ?
C30 C31 C32 121.9(5) . . ?
O4 C32 C31 120.7(4) . . ?
O4 C32 C27 121.3(4) . . ?
C31 C32 C27 118.0(4) . . ?
O4 C32 Eu1 45.18(19) . . ?
C31 C32 Eu1 128.4(3) . . ?
C27 C32 Eu1 96.1(3) . . ?
O5 C33 C34 121.1(4) . . ?
O5 C33 C38 121.8(4) . . ?
C34 C33 C38 117.1(4) . . ?
C35 C34 C33 122.1(4) . . ?
C34 C35 C36 120.3(5) . . ?
C37 C36 C35 119.2(5) . . ?
C36 C37 C38 122.2(5) . . ?
C37 C38 C33 119.0(4) . . ?
C37 C38 C39 117.3(4) . . ?
C33 C38 C39 123.5(4) . . ?
N5 C39 C38 127.9(4) . . ?
N5 C40 C41 109.0(4) . . ?
N6 C41 C40 110.5(3) . . ?
N6 C42 C43 125.2(4) . . ?
C44 C43 C48 119.5(4) . . ?
C44 C43 C42 117.0(4) . . ?
C48 C43 C42 123.4(4) . . ?
C45 C44 C43 122.1(4) . . ?
C44 C45 C46 118.8(4) . . ?
C47 C46 C45 120.1(4) . . ?
C46 C47 C48 122.0(4) . . ?
O6 C48 C47 120.1(4) . . ?
O6 C48 C43 122.4(4) . . ?
C47 C48 C43 117.5(4) . . ?
O6 C48 Eu2 38.65(19) . . ?
C47 C48 Eu2 136.9(3) . . ?
C43 C48 Eu2 96.2(3) . . ?
_diffrn_measured_fraction_theta_max 0.949
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.147
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.971 0.500 510.0 115.5
2 0.451 0.056 0.982 8.2 1.1
3 0.560 0.931 0.022 6.9 0.6
_platon_squeeze_details          
;
;