# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
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#
# 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.
#
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# fide research purposes only. It may contain copyright material
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data_c
_database_code_depnum_ccdc_archive 'CCDC 841488'
#TrackingRef 'CCDC 841488.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C23 H34 Cl2 Dy N2 O5, 3(C H4 O), Cl'
_chemical_formula_sum 'C26 H46 Cl3 Dy N2 O8'
_chemical_formula_weight 783.50
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'
Cl Cl 0.1484 0.1585 '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'
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'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M 'P b c a'
_symmetry_space_group_name_Hall '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
_cell_length_a 17.182(3)
_cell_length_b 17.970(4)
_cell_length_c 22.695(4)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 7007(2)
_cell_formula_units_Z 8
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 24926
_cell_measurement_theta_min 3.13
_cell_measurement_theta_max 27.44
_exptl_crystal_description block
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.14
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.11
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.485
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3176
_exptl_absorpt_coefficient_mu 2.404
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7295
_exptl_absorpt_correction_T_max 0.7779
_exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID'
_diffrn_measurement_method '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 48697
_diffrn_reflns_av_R_equivalents 0.0562
_diffrn_reflns_av_sigmaI/netI 0.0406
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_theta_min 3.13
_diffrn_reflns_theta_max 27.42
_reflns_number_total 7915
_reflns_number_gt 5104
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement 'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Diamond (Crystl Impact GbR, 2005)'
_computing_publication_material SHELXL-97
_refine_special_details
;
simu 0.01 o8 o8'
simu 0.01 c26 c26'
size 0.14 0.12 0.11
isor 0.01 o8 o8' c26 c26'
dfix 1.50 0.01 o8 c26 o8' c26'
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^)+(0.0251P)^2^+6.3296P] 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 7915
_refine_ls_number_parameters 385
_refine_ls_number_restraints 38
_refine_ls_R_factor_all 0.0693
_refine_ls_R_factor_gt 0.0342
_refine_ls_wR_factor_ref 0.0783
_refine_ls_wR_factor_gt 0.0677
_refine_ls_goodness_of_fit_ref 1.003
_refine_ls_restrained_S_all 1.007
_refine_ls_shift/su_max 0.004
_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
O8' O 0.3366(16) 0.5933(18) 0.1739(13) 0.271(10) Uani 0.383(11) 1 d PDU A 1
H8' H 0.3704 0.6167 0.1914 0.407 Uiso 0.383(11) 1 d PR A 1
C26' C 0.2797(18) 0.5583(18) 0.2164(14) 0.224(10) Uani 0.383(11) 1 d PDU A 1
H26A H 0.2996 0.5664 0.2554 0.336 Uiso 0.383(11) 1 d PR A 1
H26B H 0.2799 0.5060 0.2078 0.336 Uiso 0.383(11) 1 d PR A 1
H26C H 0.2274 0.5769 0.2140 0.336 Uiso 0.383(11) 1 d PR A 1
O8 O 0.2992(13) 0.6357(9) 0.1813(8) 0.307(8) Uani 0.617(11) 1 d PDU A 2
H8 H 0.3410 0.6228 0.1954 0.461 Uiso 0.617(11) 1 d PR A 2
C26 C 0.2679(8) 0.5730(8) 0.1453(6) 0.142(5) Uani 0.617(11) 1 d PDU A 2
H26D H 0.2226 0.5533 0.1646 0.212 Uiso 0.617(11) 1 d PR A 2
H26E H 0.3061 0.5345 0.1412 0.212 Uiso 0.617(11) 1 d PR A 2
H26F H 0.2538 0.5914 0.1071 0.212 Uiso 0.617(11) 1 d PR A 2
Dy1 Dy 0.505934(9) 0.754833(9) 0.894528(7) 0.03888(6) Uani 1 1 d . . .
Cl1 Cl 0.59226(6) 0.87634(6) 0.89786(5) 0.0598(3) Uani 1 1 d . . .
Cl2 Cl 0.42390(7) 0.63308(6) 0.87489(5) 0.0619(3) Uani 1 1 d . . .
Cl3 Cl 0.19115(8) 0.72449(12) 0.75111(7) 0.1125(6) Uani 1 1 d . . .
C1 C 0.0641(3) 0.9157(3) 0.8764(2) 0.0630(12) Uani 1 1 d . . .
H1A H 0.0645 0.9488 0.8449 0.076 Uiso 1 1 calc R . .
C2 C 0.3093(2) 0.5354(2) 0.9946(2) 0.0544(11) Uani 1 1 d . . .
H2D H 0.3421 0.5397 0.9600 0.065 Uiso 1 1 calc R . .
H2B H 0.3428 0.5292 1.0287 0.065 Uiso 1 1 calc R . .
C3 C 0.2566(2) 0.4674(3) 0.9884(2) 0.0611(13) Uani 1 1 d . . .
H3A H 0.2883 0.4235 0.9821 0.073 Uiso 1 1 calc R . .
H3B H 0.2276 0.4604 1.0247 0.073 Uiso 1 1 calc R . .
C4 C 0.3835(3) 0.8884(3) 1.1217(2) 0.0755(15) Uani 1 1 d . . .
H4A H 0.3763 0.9155 1.1562 0.091 Uiso 1 1 calc R . .
C5 C 0.4359(3) 0.9133(3) 1.0790(2) 0.0678(14) Uani 1 1 d . . .
H5A H 0.4635 0.9571 1.0855 0.081 Uiso 1 1 calc R . .
C6 C 0.4475(2) 0.8745(2) 1.0279(2) 0.0567(11) Uani 1 1 d . . .
H6A H 0.4827 0.8923 1.0002 0.068 Uiso 1 1 calc R . .
C7 C 0.2056(2) 0.6157(2) 0.94887(17) 0.0421(9) Uani 1 1 d . . .
H7A H 0.2366 0.6201 0.9128 0.051 Uiso 1 1 calc R . .
C8 C 0.1532(2) 0.5472(2) 0.9442(2) 0.0547(11) Uani 1 1 d . . .
H8A H 0.1210 0.5438 0.9792 0.066 Uiso 1 1 calc R . .
H8B H 0.1191 0.5526 0.9105 0.066 Uiso 1 1 calc R . .
C9 C 0.2005(3) 0.4762(2) 0.9378(2) 0.0628(12) Uani 1 1 d . . .
H9A H 0.1656 0.4337 0.9366 0.075 Uiso 1 1 calc R . .
H9B H 0.2292 0.4775 0.9010 0.075 Uiso 1 1 calc R . .
C10 C 0.3429(3) 0.8242(3) 1.1126(2) 0.0673(13) Uani 1 1 d . . .
H10A H 0.3085 0.8073 1.1413 0.081 Uiso 1 1 calc R . .
C11 C 0.0222(3) 0.9323(2) 0.9277(2) 0.0606(12) Uani 1 1 d . . .
H11A H -0.0062 0.9763 0.9297 0.073 Uiso 1 1 calc R . .
C12 C 0.3071(2) 0.7178(2) 1.05179(18) 0.0486(10) Uani 1 1 d . . .
H12A H 0.2714 0.7065 1.0812 0.058 Uiso 1 1 calc R . .
C13 C 0.1506(2) 0.7338(2) 0.91586(18) 0.0462(10) Uani 1 1 d . . .
H13A H 0.1757 0.7257 0.8801 0.055 Uiso 1 1 calc R . .
C14 C 0.1061(2) 0.8000(2) 0.92130(16) 0.0409(9) Uani 1 1 d . . .
C15 C 0.1044(3) 0.8505(3) 0.8732(2) 0.0591(12) Uani 1 1 d . . .
H15A H 0.1313 0.8389 0.8388 0.071 Uiso 1 1 calc R . .
C16 C 0.4753(3) 0.7402(4) 0.7410(2) 0.103(2) Uani 1 1 d . . .
H16A H 0.4613 0.7820 0.7168 0.154 Uiso 1 1 calc R . .
H16B H 0.4290 0.7180 0.7569 0.154 Uiso 1 1 calc R . .
H16C H 0.5026 0.7042 0.7175 0.154 Uiso 1 1 calc R . .
C17 C 0.3268(3) 0.8138(3) 0.8486(2) 0.0795(16) Uani 1 1 d . . .
H17A H 0.3018 0.8478 0.8220 0.119 Uiso 1 1 calc R . .
H17B H 0.3017 0.8161 0.8864 0.119 Uiso 1 1 calc R . .
H17C H 0.3229 0.7641 0.8333 0.119 Uiso 1 1 calc R . .
C18 C 0.0221(2) 0.8849(2) 0.97517(19) 0.0498(10) Uani 1 1 d . . .
H18A H -0.0071 0.8970 1.0083 0.060 Uiso 1 1 calc R . .
C19 C 0.2607(2) 0.6065(2) 1.00162(18) 0.0447(9) Uani 1 1 d . . .
H19A H 0.2293 0.6018 1.0374 0.054 Uiso 1 1 calc R . .
C20 C 0.4821(4) 0.5107(5) 0.2733(3) 0.134(3) Uani 1 1 d . . .
H20C H 0.4757 0.5304 0.2343 0.202 Uiso 1 1 calc R . .
H20B H 0.4847 0.4574 0.2714 0.202 Uiso 1 1 calc R . .
H20A H 0.5293 0.5297 0.2902 0.202 Uiso 1 1 calc R . .
C21 C 0.6375(3) 0.6095(3) 0.8808(2) 0.0815(16) Uani 1 1 d . . .
H21A H 0.6900 0.5989 0.8692 0.122 Uiso 1 1 calc R . .
H21B H 0.6026 0.5760 0.8611 0.122 Uiso 1 1 calc R . .
H21C H 0.6325 0.6033 0.9227 0.122 Uiso 1 1 calc R . .
C22 C 0.4064(2) 0.8071(2) 1.01634(18) 0.0446(9) Uani 1 1 d . . .
C23 C 0.3526(2) 0.7829(2) 1.05951(19) 0.0480(10) Uani 1 1 d . . .
C24 C 0.0659(2) 0.8177(2) 0.97459(17) 0.0401(8) Uani 1 1 d . . .
C25 C 0.2203(5) 0.4629(7) 0.2745(4) 0.196(5) Uani 1 1 d . . .
H25C H 0.2053 0.5039 0.2991 0.295 Uiso 1 1 calc R . .
H25B H 0.1852 0.4220 0.2808 0.295 Uiso 1 1 calc R . .
H25A H 0.2184 0.4778 0.2340 0.295 Uiso 1 1 calc R . .
N1 N 0.31092(17) 0.67273(18) 1.00752(15) 0.0454(8) Uani 1 1 d . . .
H1C H 0.3386 0.6788 0.9757 0.054 Uiso 1 1 d R . .
N2 N 0.15939(17) 0.68351(18) 0.95650(14) 0.0411(7) Uani 1 1 d . . .
H2C H 0.1243 0.6977 0.9915 0.049 Uiso 1 1 d R . .
O1 O 0.2971(4) 0.4405(4) 0.2890(3) 0.188(3) Uani 1 1 d . . .
H1B H 0.3140 0.3977 0.2757 0.281 Uiso 1 1 d R . .
O2 O 0.4210(3) 0.5311(3) 0.3070(2) 0.1256(17) Uani 1 1 d . . .
H2A H 0.3754 0.5345 0.2900 0.188 Uiso 1 1 d R . .
O3 O 0.61878(18) 0.68323(18) 0.86551(13) 0.0646(9) Uani 1 1 d . . .
H3C H 0.6623 0.7057 0.8554 0.097 Uiso 1 1 d R . .
O4 O 0.41588(14) 0.77015(16) 0.96736(12) 0.0507(7) Uani 1 1 d . . .
O5 O 0.40727(16) 0.83369(18) 0.85491(14) 0.0635(9) Uani 1 1 d . . .
H5B H 0.4207 0.8542 0.8217 0.095 Uiso 1 1 d R . .
O6 O 0.06976(14) 0.77434(15) 1.02027(11) 0.0457(6) Uani 1 1 d . . .
O7 O 0.52387(17) 0.76440(19) 0.78775(13) 0.0672(9) Uani 1 1 d . . .
H7B H 0.5649 0.7390 0.7787 0.101 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
O8' 0.284(12) 0.268(12) 0.261(11) 0.000(9) -0.008(9) 0.003(9)
C26' 0.228(12) 0.225(12) 0.220(12) -0.015(9) -0.006(9) -0.007(9)
O8 0.322(11) 0.319(11) 0.280(10) 0.013(9) -0.013(8) -0.007(9)
C26 0.141(8) 0.150(9) 0.134(8) 0.009(7) -0.002(7) 0.020(7)
Dy1 0.03875(9) 0.03760(10) 0.04030(9) 0.00050(8) -0.00354(8) -0.00383(8)
Cl1 0.0622(6) 0.0494(6) 0.0679(7) 0.0069(6) -0.0130(6) -0.0179(5)
Cl2 0.0714(7) 0.0490(6) 0.0653(7) -0.0059(5) -0.0053(6) -0.0198(6)
Cl3 0.0776(9) 0.1779(18) 0.0819(10) -0.0482(11) -0.0258(8) 0.0157(10)
C1 0.075(3) 0.058(3) 0.056(3) 0.019(2) -0.005(2) 0.009(2)
C2 0.043(2) 0.043(2) 0.077(3) 0.009(2) 0.005(2) 0.0098(19)
C3 0.057(3) 0.040(2) 0.086(4) 0.009(2) 0.011(3) 0.005(2)
C4 0.073(3) 0.076(4) 0.077(3) -0.036(3) 0.007(3) -0.001(3)
C5 0.057(3) 0.054(3) 0.093(4) -0.024(3) -0.001(3) -0.001(2)
C6 0.048(2) 0.049(3) 0.073(3) -0.012(2) 0.001(2) -0.0017(19)
C7 0.0408(19) 0.037(2) 0.049(2) -0.0016(18) 0.0067(18) 0.0044(16)
C8 0.047(2) 0.049(3) 0.068(3) -0.009(2) 0.002(2) -0.0043(19)
C9 0.065(3) 0.044(3) 0.079(3) -0.011(2) 0.007(3) -0.004(2)
C10 0.060(3) 0.083(4) 0.059(3) -0.018(3) 0.015(2) -0.007(2)
C11 0.063(3) 0.047(3) 0.073(3) 0.008(2) -0.005(3) 0.010(2)
C12 0.044(2) 0.052(3) 0.050(2) 0.000(2) 0.0085(19) 0.0004(18)
C13 0.0432(19) 0.054(3) 0.041(2) -0.0049(19) -0.0007(17) -0.0006(18)
C14 0.043(2) 0.042(2) 0.037(2) 0.0009(17) -0.0042(17) 0.0017(17)
C15 0.072(3) 0.059(3) 0.046(2) 0.008(2) 0.004(2) 0.009(2)
C16 0.096(4) 0.161(7) 0.051(3) -0.014(4) -0.015(3) -0.015(4)
C17 0.054(3) 0.084(4) 0.101(4) -0.008(3) -0.023(3) 0.006(3)
C18 0.048(2) 0.044(2) 0.057(3) 0.003(2) 0.004(2) 0.0059(18)
C19 0.0366(19) 0.042(2) 0.056(2) 0.0023(19) 0.0046(19) 0.0004(16)
C20 0.105(5) 0.192(9) 0.107(5) -0.047(6) 0.023(5) 0.006(5)
C21 0.083(4) 0.064(3) 0.098(4) 0.015(3) 0.017(3) 0.026(3)
C22 0.0342(18) 0.047(2) 0.053(2) -0.006(2) -0.0052(18) 0.0053(16)
C23 0.044(2) 0.048(2) 0.053(3) -0.006(2) 0.001(2) -0.0012(18)
C24 0.0390(19) 0.040(2) 0.041(2) 0.0013(18) -0.0037(17) -0.0045(16)
C25 0.099(6) 0.324(15) 0.166(9) -0.034(9) 0.003(7) -0.040(8)
N1 0.0381(16) 0.048(2) 0.050(2) -0.0012(16) 0.0050(15) -0.0023(15)
N2 0.0371(15) 0.0432(19) 0.0431(19) -0.0056(15) 0.0026(14) 0.0053(14)
O1 0.143(5) 0.232(7) 0.188(6) -0.080(5) 0.016(5) -0.063(5)
O2 0.102(3) 0.124(4) 0.151(4) -0.054(3) 0.023(3) -0.020(3)
O3 0.0685(19) 0.062(2) 0.063(2) 0.0172(16) 0.0146(16) 0.0187(16)
O4 0.0461(14) 0.0542(18) 0.0519(16) -0.0095(14) 0.0021(13) -0.0048(13)
O5 0.0480(16) 0.071(2) 0.072(2) 0.0130(17) -0.0021(16) 0.0069(15)
O6 0.0504(14) 0.0465(16) 0.0403(14) 0.0044(12) 0.0050(13) 0.0050(12)
O7 0.0587(16) 0.096(3) 0.0466(16) 0.0032(17) -0.0074(14) 0.0093(17)
_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
O8' C26' 1.510(10) . ?
O8' H8' 0.8200 . ?
O8' H8 0.7249 . ?
O8' H26E 1.3923 . ?
C26' H26A 0.9600 . ?
C26' H26B 0.9600 . ?
C26' H26C 0.9600 . ?
O8 C26 1.491(9) . ?
O8 H8' 1.2906 . ?
O8 H8 0.8200 . ?
C26 H26D 0.9600 . ?
C26 H26E 0.9600 . ?
C26 H26F 0.9600 . ?
Dy1 O4 2.281(3) . ?
Dy1 O6 2.284(3) 3_567 ?
Dy1 O5 2.385(3) . ?
Dy1 O3 2.418(3) . ?
Dy1 O7 2.449(3) . ?
Dy1 Cl2 2.6404(11) . ?
Dy1 Cl1 2.6407(11) . ?
C1 C15 1.363(6) . ?
C1 C11 1.402(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.527(6) . ?
C2 C19 1.535(5) . ?
C2 H2D 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C9 1.508(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C10 1.364(6) . ?
C4 C5 1.395(7) . ?
C4 H4A 0.9300 . ?
C5 C6 1.370(6) . ?
C5 H5A 0.9300 . ?
C6 C22 1.425(5) . ?
C6 H6A 0.9300 . ?
C7 N2 1.464(4) . ?
C7 C8 1.529(5) . ?
C7 C19 1.536(5) . ?
C7 H7A 0.9800 . ?
C8 C9 1.520(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C23 1.425(6) . ?
C10 H10A 0.9300 . ?
C11 C18 1.372(6) . ?
C11 H11A 0.9300 . ?
C12 N1 1.292(5) . ?
C12 C23 1.419(6) . ?
C12 H12A 0.9300 . ?
C13 N2 1.300(5) . ?
C13 C14 1.419(5) . ?
C13 H13A 0.9300 . ?
C14 C15 1.421(5) . ?
C14 C24 1.429(5) . ?
C15 H15A 0.9300 . ?
C16 O7 1.419(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 O5 1.436(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C24 1.423(5) . ?
C18 H18A 0.9300 . ?
C19 N1 1.476(5) . ?
C19 H19A 0.9800 . ?
C20 O2 1.350(7) . ?
C20 H20C 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20A 0.9600 . ?
C21 O3 1.407(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O4 1.305(4) . ?
C22 C23 1.415(5) . ?
C24 O6 1.298(4) . ?
C25 O1 1.417(9) . ?
C25 H25C 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25A 0.9600 . ?
N1 H1C 0.8713 . ?
N2 H2C 1.0290 . ?
O1 H1B 0.8747 . ?
O2 H2A 0.8759 . ?
O3 H3C 0.8803 . ?
O5 H5B 0.8710 . ?
O6 Dy1 2.284(3) 3_467 ?
O7 H7B 0.8651 . ?
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
C26' O8' H8' 111.3 . . ?
C26' O8' H8 86.6 . . ?
H8' O8' H8 39.1 . . ?
C26' O8' H26E 77.4 . . ?
H8' O8' H26E 156.0 . . ?
H8 O8' H26E 162.3 . . ?
O8' C26' H26A 107.2 . . ?
O8' C26' H26B 105.9 . . ?
H26A C26' H26B 109.5 . . ?
O8' C26' H26C 115.2 . . ?
H26A C26' H26C 109.5 . . ?
H26B C26' H26C 109.5 . . ?
C26 O8 H8' 103.9 . . ?
C26 O8 H8 108.4 . . ?
H8' O8 H8 13.0 . . ?
O8 C26 H26D 108.8 . . ?
O8 C26 H26E 110.6 . . ?
H26D C26 H26E 109.5 . . ?
O8 C26 H26F 109.1 . . ?
H26D C26 H26F 109.5 . . ?
H26E C26 H26F 109.5 . . ?
O4 Dy1 O6 74.92(10) . 3_567 ?
O4 Dy1 O5 73.70(10) . . ?
O6 Dy1 O5 142.81(10) 3_567 . ?
O4 Dy1 O3 143.66(10) . . ?
O6 Dy1 O3 73.95(10) 3_567 . ?
O5 Dy1 O3 141.55(10) . . ?
O4 Dy1 O7 142.57(10) . . ?
O6 Dy1 O7 142.51(9) 3_567 . ?
O5 Dy1 O7 71.02(10) . . ?
O3 Dy1 O7 70.55(10) . . ?
O4 Dy1 Cl2 81.96(7) . . ?
O6 Dy1 Cl2 102.06(7) 3_567 . ?
O5 Dy1 Cl2 92.82(8) . . ?
O3 Dy1 Cl2 86.62(9) . . ?
O7 Dy1 Cl2 87.61(8) . . ?
O4 Dy1 Cl1 105.10(7) . . ?
O6 Dy1 Cl1 84.02(7) 3_567 . ?
O5 Dy1 Cl1 85.34(8) . . ?
O3 Dy1 Cl1 89.85(9) . . ?
O7 Dy1 Cl1 84.24(8) . . ?
Cl2 Dy1 Cl1 171.80(4) . . ?
C15 C1 C11 119.3(4) . . ?
C15 C1 H1A 120.4 . . ?
C11 C1 H1A 120.4 . . ?
C3 C2 C19 110.6(3) . . ?
C3 C2 H2D 109.5 . . ?
C19 C2 H2D 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C19 C2 H2B 109.5 . . ?
H2D C2 H2B 108.1 . . ?
C9 C3 C2 111.5(4) . . ?
C9 C3 H3A 109.3 . . ?
C2 C3 H3A 109.3 . . ?
C9 C3 H3B 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C10 C4 C5 119.8(5) . . ?
C10 C4 H4A 120.1 . . ?
C5 C4 H4A 120.1 . . ?
C6 C5 C4 121.2(5) . . ?
C6 C5 H5A 119.4 . . ?
C4 C5 H5A 119.4 . . ?
C5 C6 C22 121.1(4) . . ?
C5 C6 H6A 119.5 . . ?
C22 C6 H6A 119.5 . . ?
N2 C7 C8 111.0(3) . . ?
N2 C7 C19 109.4(3) . . ?
C8 C7 C19 109.2(3) . . ?
N2 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C19 C7 H7A 109.1 . . ?
C9 C8 C7 111.6(3) . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C3 C9 C8 110.8(4) . . ?
C3 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C3 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C4 C10 C23 120.5(5) . . ?
C4 C10 H10A 119.7 . . ?
C23 C10 H10A 119.7 . . ?
C18 C11 C1 121.3(4) . . ?
C18 C11 H11A 119.3 . . ?
C1 C11 H11A 119.3 . . ?
N1 C12 C23 125.8(4) . . ?
N1 C12 H12A 117.1 . . ?
C23 C12 H12A 117.1 . . ?
N2 C13 C14 125.7(4) . . ?
N2 C13 H13A 117.2 . . ?
C14 C13 H13A 117.2 . . ?
C13 C14 C15 118.6(4) . . ?
C13 C14 C24 121.4(4) . . ?
C15 C14 C24 119.9(4) . . ?
C1 C15 C14 121.2(4) . . ?
C1 C15 H15A 119.4 . . ?
C14 C15 H15A 119.4 . . ?
O7 C16 H16A 109.5 . . ?
O7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C17 H17A 109.5 . . ?
O5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C11 C18 C24 121.3(4) . . ?
C11 C18 H18A 119.4 . . ?
C24 C18 H18A 119.4 . . ?
N1 C19 C2 111.3(3) . . ?
N1 C19 C7 110.1(3) . . ?
C2 C19 C7 110.2(3) . . ?
N1 C19 H19A 108.4 . . ?
C2 C19 H19A 108.4 . . ?
C7 C19 H19A 108.4 . . ?
O2 C20 H20C 109.5 . . ?
O2 C20 H20B 109.5 . . ?
H20C C20 H20B 109.5 . . ?
O2 C20 H20A 109.5 . . ?
H20C C20 H20A 109.5 . . ?
H20B C20 H20A 109.5 . . ?
O3 C21 H21A 109.5 . . ?
O3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C22 C23 121.0(4) . . ?
O4 C22 C6 121.8(4) . . ?
C23 C22 C6 117.2(4) . . ?
C22 C23 C12 121.9(4) . . ?
C22 C23 C10 120.2(4) . . ?
C12 C23 C10 118.0(4) . . ?
O6 C24 C18 121.9(4) . . ?
O6 C24 C14 121.1(3) . . ?
C18 C24 C14 116.9(4) . . ?
O1 C25 H25C 109.5 . . ?
O1 C25 H25B 109.5 . . ?
H25C C25 H25B 109.5 . . ?
O1 C25 H25A 109.5 . . ?
H25C C25 H25A 109.5 . . ?
H25B C25 H25A 109.5 . . ?
C12 N1 C19 123.1(3) . . ?
C12 N1 H1C 126.4 . . ?
C19 N1 H1C 110.2 . . ?
C13 N2 C7 123.8(3) . . ?
C13 N2 H2C 107.9 . . ?
C7 N2 H2C 128.0 . . ?
C25 O1 H1B 118.6 . . ?
C20 O2 H2A 117.7 . . ?
C21 O3 Dy1 128.1(3) . . ?
C21 O3 H3C 107.6 . . ?
Dy1 O3 H3C 120.5 . . ?
C22 O4 Dy1 139.8(2) . . ?
C17 O5 Dy1 125.0(3) . . ?
C17 O5 H5B 105.9 . . ?
Dy1 O5 H5B 113.0 . . ?
C24 O6 Dy1 142.1(2) . 3_467 ?
C16 O7 Dy1 130.1(3) . . ?
C16 O7 H7B 98.1 . . ?
Dy1 O7 H7B 107.4 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7B Cl3 0.87 2.29 3.091(3) 154.6 6_657
O5 H5B O2 0.87 2.09 2.673(5) 123.8 8_576
O3 H3C Cl3 0.88 2.49 3.017(3) 119.0 6_657
O2 H2A O1 0.88 2.16 2.712(7) 120.5 .
O1 H1B Cl3 0.87 2.27 3.093(7) 157.3 2_564
N2 H2C Cl1 1.03 2.90 3.662(3) 131.8 3_467
N2 H2C O6 1.03 1.79 2.670(4) 141.3 .
N1 H1C Cl2 0.87 2.84 3.652(3) 156.0 .
N1 H1C O4 0.87 2.12 2.674(4) 120.8 .
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full 27.42
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max 0.471
_refine_diff_density_min -0.700
_refine_diff_density_rms 0.076
data_zj-5-2dy
_database_code_depnum_ccdc_archive 'CCDC 856826'
#TrackingRef 'CCDC 856826.CIF'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C61 H64 Dy2 N6 O7'
_chemical_formula_sum 'C61 H64 Dy2 N6 O7'
_chemical_formula_weight 1318.18
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 monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 12.389(3)
_cell_length_b 22.590(4)
_cell_length_c 22.464(7)
_cell_angle_alpha 90.00
_cell_angle_beta 119.74(2)
_cell_angle_gamma 90.00
_cell_volume 5459(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 44216
_cell_measurement_theta_min 3.13
_cell_measurement_theta_max 27.50
_exptl_crystal_description block
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.33
_exptl_crystal_size_min 0.30
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.604
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2640
_exptl_absorpt_coefficient_mu 2.776
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.4416
_exptl_absorpt_correction_T_max 0.4857
_exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID'
_diffrn_measurement_method '\w scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 51103
_diffrn_reflns_av_R_equivalents 0.0465
_diffrn_reflns_av_sigmaI/netI 0.0418
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_theta_min 3.15
_diffrn_reflns_theta_max 27.48
_reflns_number_total 12480
_reflns_number_gt 10277
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement 'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material SHELXL-97
_refine_special_details
;
delu 0.02 c51 c52
simu 0.01 0.02 $c
dfix 0.85 0.01 o7 h71
FREE C50' H49B
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^)+(0.0000P)^2^+17.3867P] 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 12480
_refine_ls_number_parameters 726
_refine_ls_number_restraints 446
_refine_ls_R_factor_all 0.0503
_refine_ls_R_factor_gt 0.0391
_refine_ls_wR_factor_ref 0.0816
_refine_ls_wR_factor_gt 0.0785
_refine_ls_goodness_of_fit_ref 1.127
_refine_ls_restrained_S_all 1.130
_refine_ls_shift/su_max 0.003
_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 0.18166(2) 0.740049(9) 0.602447(10) 0.02794(5) Uani 1 1 d . . .
Dy2 Dy 0.49647(2) 0.713473(10) 0.771227(10) 0.03347(6) Uani 1 1 d . A .
O1 O 0.3157(3) 0.79846(14) 0.58499(17) 0.0386(7) Uani 1 1 d . . .
O2 O 0.1525(3) 0.69576(15) 0.50828(17) 0.0436(8) Uani 1 1 d . . .
O3 O 0.3206(3) 0.77326(13) 0.71322(15) 0.0365(7) Uani 1 1 d . . .
O4 O 0.3518(3) 0.67404(13) 0.66325(15) 0.0339(7) Uani 1 1 d . . .
O5 O 0.5434(3) 0.77221(15) 0.85701(16) 0.0420(8) Uani 1 1 d . . .
O6 O 0.6962(3) 0.70094(16) 0.80898(18) 0.0508(9) Uani 1 1 d . . .
O7 O 0.5364(4) 0.7728(2) 0.6954(2) 0.0593(11) Uani 1 1 d D . .
H71 H 0.480(5) 0.788(3) 0.659(2) 0.089 Uiso 1 1 d D . .
N1 N 0.0996(4) 0.84473(16) 0.58255(19) 0.0361(9) Uani 1 1 d . . .
N2 N -0.0469(4) 0.75584(17) 0.51233(18) 0.0376(9) Uani 1 1 d . . .
N3 N 0.0842(4) 0.72787(17) 0.68345(19) 0.0368(9) Uani 1 1 d . . .
N4 N 0.1022(4) 0.63847(17) 0.61046(19) 0.0354(9) Uani 1 1 d . . .
N5 N 0.3936(5) 0.6712(2) 0.8312(2) 0.0547(12) Uani 1 1 d . . .
N6 N 0.5462(5) 0.60631(19) 0.8070(2) 0.0500(11) Uani 1 1 d . . .
C1 C 0.3244(5) 0.8512(2) 0.5640(2) 0.0372(10) Uani 1 1 d U . .
C2 C 0.4180(5) 0.8635(2) 0.5475(3) 0.0457(12) Uani 1 1 d U . .
H2 H 0.4720 0.8335 0.5508 0.055 Uiso 1 1 calc R . .
C3 C 0.4311(6) 0.9189(3) 0.5266(3) 0.0543(14) Uani 1 1 d U . .
H3 H 0.4939 0.9256 0.5161 0.065 Uiso 1 1 calc R . .
C4 C 0.3537(6) 0.9645(3) 0.5208(3) 0.0576(15) Uani 1 1 d U . .
H4 H 0.3640 1.0019 0.5070 0.069 Uiso 1 1 calc R . .
C5 C 0.2609(5) 0.9540(2) 0.5356(3) 0.0503(13) Uani 1 1 d U . .
H5 H 0.2083 0.9850 0.5317 0.060 Uiso 1 1 calc R . .
C6 C 0.2422(5) 0.8983(2) 0.5566(2) 0.0404(11) Uani 1 1 d U . .
C7 C 0.1349(5) 0.8915(2) 0.5653(3) 0.0445(12) Uani 1 1 d U . .
H7 H 0.0860 0.9250 0.5574 0.053 Uiso 1 1 calc R . .
C8 C -0.0210(5) 0.8443(2) 0.5800(3) 0.0441(11) Uani 1 1 d U . .
H8 H -0.0099 0.8203 0.6190 0.053 Uiso 1 1 calc R . .
C9 C -0.0771(6) 0.9026(3) 0.5849(3) 0.0545(14) Uani 1 1 d U . .
H9A H -0.0927 0.9276 0.5464 0.065 Uiso 1 1 calc R . .
H9B H -0.0195 0.9229 0.6268 0.065 Uiso 1 1 calc R . .
C10 C -0.1985(6) 0.8908(3) 0.5845(3) 0.0715(17) Uani 1 1 d U . .
H10A H -0.1810 0.8690 0.6256 0.086 Uiso 1 1 calc R . .
H10B H -0.2360 0.9282 0.5853 0.086 Uiso 1 1 calc R . .
C11 C -0.2884(6) 0.8563(3) 0.5229(4) 0.0739(18) Uani 1 1 d U . .
H11A H -0.3159 0.8808 0.4825 0.089 Uiso 1 1 calc R . .
H11B H -0.3607 0.8469 0.5272 0.089 Uiso 1 1 calc R . .
C12 C -0.2342(5) 0.7990(3) 0.5131(3) 0.0589(14) Uani 1 1 d U . .
H12A H -0.2920 0.7818 0.4690 0.071 Uiso 1 1 calc R . .
H12B H -0.2223 0.7710 0.5485 0.071 Uiso 1 1 calc R . .
C13 C -0.1103(5) 0.8106(2) 0.5163(3) 0.0457(12) Uani 1 1 d U . .
H13 H -0.1271 0.8353 0.4767 0.055 Uiso 1 1 calc R . .
C14 C -0.1095(5) 0.7255(2) 0.4575(2) 0.0441(12) Uani 1 1 d U . .
H14 H -0.1910 0.7374 0.4284 0.053 Uiso 1 1 calc R . .
C15 C -0.0664(5) 0.6750(2) 0.4366(2) 0.0489(13) Uani 1 1 d U . .
C16 C -0.1573(7) 0.6385(3) 0.3856(3) 0.0751(19) Uani 1 1 d U . .
H16 H -0.2410 0.6465 0.3691 0.090 Uiso 1 1 calc R . .
C17 C -0.1233(8) 0.5911(3) 0.3598(4) 0.089(2) Uani 1 1 d U . .
H17 H -0.1839 0.5661 0.3277 0.106 Uiso 1 1 calc R . .
C18 C 0.0009(8) 0.5809(3) 0.3818(3) 0.078(2) Uani 1 1 d U . .
H18 H 0.0228 0.5498 0.3627 0.094 Uiso 1 1 calc R . .
C19 C 0.0927(7) 0.6156(3) 0.4313(3) 0.0614(15) Uani 1 1 d U . .
H19 H 0.1756 0.6076 0.4454 0.074 Uiso 1 1 calc R . .
C20 C 0.0620(6) 0.6635(2) 0.4610(2) 0.0440(12) Uani 1 1 d U . .
C21 C 0.2853(5) 0.8199(2) 0.7365(2) 0.0410(11) Uani 1 1 d U . .
C22 C 0.3493(6) 0.8739(2) 0.7494(3) 0.0573(15) Uani 1 1 d U . .
H22 H 0.4154 0.8775 0.7410 0.069 Uiso 1 1 calc R . .
C23 C 0.3151(8) 0.9214(3) 0.7743(3) 0.081(2) Uani 1 1 d U . .
H23 H 0.3554 0.9575 0.7809 0.097 Uiso 1 1 calc R . .
C24 C 0.2209(8) 0.9156(3) 0.7897(4) 0.088(2) Uani 1 1 d U . .
H24 H 0.1996 0.9477 0.8078 0.106 Uiso 1 1 calc R . .
C25 C 0.1585(7) 0.8632(3) 0.7788(3) 0.0746(19) Uani 1 1 d U . .
H25 H 0.0966 0.8596 0.7906 0.090 Uiso 1 1 calc R . .
C26 C 0.1873(5) 0.8151(3) 0.7500(2) 0.0496(13) Uani 1 1 d U . .
C27 C 0.1125(5) 0.7613(3) 0.7350(3) 0.0487(13) Uani 1 1 d U . .
H27 H 0.0838 0.7508 0.7648 0.058 Uiso 1 1 calc R . .
C28 C 0.0121(5) 0.6737(2) 0.6771(3) 0.0469(12) Uani 1 1 d U . .
H28 H 0.0650 0.6482 0.7162 0.056 Uiso 1 1 calc R . .
C29 C -0.1077(6) 0.6839(3) 0.6786(3) 0.0662(16) Uani 1 1 d U . .
H29A H -0.0886 0.7028 0.7215 0.079 Uiso 1 1 calc R . .
H29B H -0.1608 0.7104 0.6416 0.079 Uiso 1 1 calc R . .
C30 C -0.1767(7) 0.6265(4) 0.6713(4) 0.0814(19) Uani 1 1 d U . .
H30A H -0.1287 0.6023 0.7117 0.098 Uiso 1 1 calc R . .
H30B H -0.2559 0.6352 0.6684 0.098 Uiso 1 1 calc R . .
C31 C -0.1990(6) 0.5924(3) 0.6087(4) 0.0792(19) Uani 1 1 d U . .
H31A H -0.2583 0.6138 0.5681 0.095 Uiso 1 1 calc R . .
H31B H -0.2351 0.5543 0.6086 0.095 Uiso 1 1 calc R . .
C32 C -0.0815(6) 0.5829(3) 0.6057(3) 0.0598(15) Uani 1 1 d U . .
H32A H -0.1019 0.5644 0.5624 0.072 Uiso 1 1 calc R . .
H32B H -0.0272 0.5563 0.6423 0.072 Uiso 1 1 calc R . .
C33 C -0.0140(5) 0.6405(2) 0.6127(3) 0.0449(12) Uani 1 1 d U . .
H33 H -0.0713 0.6653 0.5740 0.054 Uiso 1 1 calc R . .
C34 C 0.1473(5) 0.5891(2) 0.6046(2) 0.0422(11) Uani 1 1 d U . .
H34 H 0.0991 0.5554 0.5973 0.051 Uiso 1 1 calc R . .
C35 C 0.2659(5) 0.5811(2) 0.6082(2) 0.0394(10) Uani 1 1 d U . .
C36 C 0.2873(6) 0.5269(2) 0.5843(3) 0.0538(14) Uani 1 1 d U . .
H36 H 0.2236 0.4992 0.5650 0.065 Uiso 1 1 calc R . .
C37 C 0.3988(7) 0.5142(3) 0.5888(3) 0.0631(15) Uani 1 1 d U . .
H37 H 0.4099 0.4787 0.5716 0.076 Uiso 1 1 calc R . .
C38 C 0.4944(6) 0.5543(3) 0.6189(3) 0.0582(14) Uani 1 1 d U . .
H38 H 0.5713 0.5456 0.6231 0.070 Uiso 1 1 calc R . .
C39 C 0.4765(5) 0.6073(2) 0.6427(3) 0.0451(12) Uani 1 1 d U . .
H39 H 0.5423 0.6339 0.6629 0.054 Uiso 1 1 calc R . .
C40 C 0.3639(5) 0.62267(19) 0.6378(2) 0.0345(10) Uani 1 1 d U . .
C41 C 0.4972(5) 0.7888(2) 0.8965(2) 0.0451(12) Uani 1 1 d U A .
C42 C 0.5327(6) 0.8432(3) 0.9305(3) 0.0642(16) Uani 1 1 d U . .
H42 H 0.5877 0.8674 0.9249 0.077 Uiso 1 1 calc R . .
C43 C 0.4862(7) 0.8614(4) 0.9726(3) 0.0765(19) Uani 1 1 d U . .
H43 H 0.5093 0.8981 0.9941 0.092 Uiso 1 1 calc R . .
C44 C 0.4066(7) 0.8260(4) 0.9831(3) 0.0761(18) Uani 1 1 d U . .
H44 H 0.3776 0.8382 1.0122 0.091 Uiso 1 1 calc R . .
C45 C 0.3711(6) 0.7731(3) 0.9507(3) 0.0665(16) Uani 1 1 d U A .
H45 H 0.3167 0.7495 0.9575 0.080 Uiso 1 1 calc R . .
C46 C 0.4138(5) 0.7527(3) 0.9069(3) 0.0518(13) Uani 1 1 d U . .
C47 C 0.3743(6) 0.6952(3) 0.8767(3) 0.0615(15) Uani 1 1 d U A .
H47 H 0.3296 0.6729 0.8918 0.074 Uiso 1 1 calc R . .
C48 C 0.3436(7) 0.6107(3) 0.8022(4) 0.0484(17) Uani 0.769(8) 1 d PU A 1
H48 H 0.2971 0.6134 0.7520 0.058 Uiso 0.769(8) 1 calc PR A 1
C50 C 0.2214(9) 0.5195(4) 0.7905(5) 0.074(3) Uani 0.769(8) 1 d PU A 1
H50A H 0.1684 0.5000 0.8048 0.089 Uiso 0.769(8) 1 calc PR A 1
H50B H 0.1744 0.5247 0.7411 0.089 Uiso 0.769(8) 1 calc PR A 1
C51 C 0.3334(10) 0.4820(4) 0.8091(5) 0.079(3) Uani 0.769(8) 1 d PU A 1
H51A H 0.3758 0.4738 0.8579 0.094 Uiso 0.769(8) 1 calc PR A 1
H51B H 0.3071 0.4445 0.7850 0.094 Uiso 0.769(8) 1 calc PR A 1
C53 C 0.4584(8) 0.5733(3) 0.8235(4) 0.0519(18) Uani 0.769(8) 1 d PU A 1
H53 H 0.4999 0.5684 0.8734 0.062 Uiso 0.769(8) 1 calc PR A 1
C48' C 0.403(2) 0.6067(11) 0.8480(13) 0.051(3) Uani 0.231(8) 1 d PU A 2
H48' H 0.4687 0.5961 0.8943 0.061 Uiso 0.231(8) 1 calc PR A 2
C50' C 0.270(3) 0.5212(13) 0.8407(15) 0.075(4) Uani 0.231(8) 1 d PU A 2
H50C H 0.1949 0.5070 0.8391 0.091 Uiso 0.231(8) 1 calc PR A 2
H50D H 0.3407 0.5125 0.8854 0.091 Uiso 0.231(8) 1 calc PR A 2
C51' C 0.286(4) 0.4952(17) 0.7861(18) 0.075(4) Uani 0.231(8) 1 d PU A 2
H51C H 0.2188 0.5089 0.7423 0.090 Uiso 0.231(8) 1 calc PR A 2
H51D H 0.2787 0.4525 0.7875 0.090 Uiso 0.231(8) 1 calc PR A 2
C53' C 0.419(3) 0.5813(12) 0.7896(15) 0.055(4) Uani 0.231(8) 1 d PU A 2
H53' H 0.3543 0.5960 0.7450 0.066 Uiso 0.231(8) 1 calc PR A 2
C49 C 0.2625(6) 0.5816(3) 0.8263(3) 0.0679(17) Uani 1 1 d U . .
H49A H 0.1901 0.6059 0.8144 0.081 Uiso 1 1 calc R A 1
H49B H 0.3084 0.5768 0.8758 0.081 Uiso 1 1 calc R A 1
C52 C 0.4213(6) 0.5117(3) 0.7912(3) 0.0675(17) Uani 1 1 d U . .
H52A H 0.3825 0.5152 0.7418 0.081 Uiso 1 1 calc R A 1
H52B H 0.4953 0.4875 0.8071 0.081 Uiso 1 1 calc R A 1
C54 C 0.6496(7) 0.5785(3) 0.8263(3) 0.0636(17) Uani 1 1 d U A .
H54 H 0.6501 0.5387 0.8368 0.076 Uiso 1 1 calc R . .
C55 C 0.7631(6) 0.6010(3) 0.8335(3) 0.0576(14) Uani 1 1 d U . .
C56 C 0.8627(7) 0.5604(3) 0.8544(3) 0.0773(19) Uani 1 1 d U A .
H56 H 0.8486 0.5202 0.8564 0.093 Uiso 1 1 calc R . .
C57 C 0.9788(8) 0.5795(4) 0.8715(4) 0.088(2) Uani 1 1 d U . .
H57 H 1.0429 0.5523 0.8845 0.106 Uiso 1 1 calc R A .
C58 C 1.0019(7) 0.6389(4) 0.8696(3) 0.0774(19) Uani 1 1 d U A .
H58 H 1.0820 0.6516 0.8827 0.093 Uiso 1 1 calc R . .
C59 C 0.9059(6) 0.6798(3) 0.8482(3) 0.0612(15) Uani 1 1 d U . .
H59 H 0.9225 0.7198 0.8468 0.073 Uiso 1 1 calc R A .
C60 C 0.7838(5) 0.6618(3) 0.8286(2) 0.0484(13) Uani 1 1 d U A .
C61 C 0.6420(7) 0.7836(4) 0.6891(5) 0.114(4) Uani 1 1 d . . .
H61A H 0.7152 0.7716 0.7304 0.171 Uiso 1 1 calc R . .
H61B H 0.6470 0.8251 0.6814 0.171 Uiso 1 1 calc R . .
H61C H 0.6358 0.7614 0.6510 0.171 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.02788(11) 0.02566(10) 0.02837(10) 0.00036(8) 0.01250(8) 0.00089(8)
Dy2 0.02995(11) 0.03274(11) 0.03098(11) 0.00099(8) 0.00998(8) -0.00111(9)
O1 0.0370(19) 0.0310(17) 0.0521(19) 0.0095(14) 0.0253(16) 0.0022(14)
O2 0.053(2) 0.043(2) 0.0431(18) -0.0080(15) 0.0307(17) -0.0032(17)
O3 0.0364(18) 0.0333(18) 0.0338(16) -0.0045(13) 0.0128(14) 0.0012(14)
O4 0.0308(17) 0.0289(16) 0.0360(16) -0.0019(13) 0.0120(13) 0.0019(13)
O5 0.0313(18) 0.054(2) 0.0375(17) -0.0061(15) 0.0146(14) -0.0037(15)
O6 0.040(2) 0.044(2) 0.058(2) 0.0042(17) 0.0157(17) 0.0084(17)
O7 0.034(2) 0.078(3) 0.063(2) 0.030(2) 0.0223(18) 0.0004(19)
N1 0.032(2) 0.030(2) 0.042(2) -0.0004(16) 0.0154(17) 0.0025(16)
N2 0.035(2) 0.035(2) 0.0327(19) 0.0006(16) 0.0094(16) 0.0017(17)
N3 0.035(2) 0.042(2) 0.0344(19) 0.0051(17) 0.0176(17) 0.0043(17)
N4 0.032(2) 0.036(2) 0.039(2) -0.0008(16) 0.0179(17) -0.0038(17)
N5 0.066(3) 0.042(3) 0.067(3) 0.007(2) 0.041(3) -0.005(2)
N6 0.054(3) 0.041(2) 0.048(2) 0.003(2) 0.020(2) 0.003(2)
C1 0.039(3) 0.034(2) 0.033(2) 0.0006(18) 0.0137(19) -0.004(2)
C2 0.044(3) 0.045(3) 0.050(3) 0.003(2) 0.026(2) -0.006(2)
C3 0.055(3) 0.054(3) 0.054(3) 0.006(2) 0.027(2) -0.014(3)
C4 0.062(3) 0.045(3) 0.059(3) 0.012(2) 0.025(3) -0.015(3)
C5 0.052(3) 0.035(3) 0.057(3) 0.006(2) 0.021(2) -0.003(2)
C6 0.044(3) 0.031(2) 0.041(2) 0.0025(19) 0.016(2) -0.002(2)
C7 0.046(3) 0.030(2) 0.048(3) 0.003(2) 0.016(2) 0.005(2)
C8 0.040(3) 0.043(3) 0.049(3) 0.003(2) 0.021(2) 0.008(2)
C9 0.053(3) 0.053(3) 0.056(3) 0.000(2) 0.026(2) 0.016(3)
C10 0.060(4) 0.080(4) 0.081(4) 0.001(3) 0.040(3) 0.024(3)
C11 0.045(3) 0.091(4) 0.085(4) 0.001(3) 0.033(3) 0.020(3)
C12 0.037(3) 0.072(4) 0.065(3) 0.002(3) 0.024(2) 0.005(3)
C13 0.036(3) 0.051(3) 0.043(2) 0.003(2) 0.014(2) 0.006(2)
C14 0.041(3) 0.046(3) 0.033(2) -0.001(2) 0.009(2) -0.004(2)
C15 0.059(3) 0.041(3) 0.036(2) -0.004(2) 0.014(2) -0.008(2)
C16 0.084(4) 0.062(4) 0.051(3) -0.017(3) 0.012(3) -0.014(3)
C17 0.111(5) 0.060(4) 0.065(4) -0.028(3) 0.022(4) -0.018(4)
C18 0.116(5) 0.049(3) 0.063(4) -0.021(3) 0.041(4) -0.008(4)
C19 0.092(4) 0.047(3) 0.052(3) -0.009(2) 0.041(3) 0.002(3)
C20 0.068(3) 0.034(2) 0.036(2) -0.0018(19) 0.030(2) -0.004(2)
C21 0.048(3) 0.035(2) 0.027(2) -0.0037(18) 0.0086(19) 0.007(2)
C22 0.065(4) 0.040(3) 0.048(3) -0.010(2) 0.013(3) -0.003(3)
C23 0.091(5) 0.047(3) 0.071(4) -0.022(3) 0.014(3) 0.000(3)
C24 0.098(5) 0.066(4) 0.077(4) -0.034(3) 0.025(4) 0.017(4)
C25 0.078(4) 0.075(4) 0.061(3) -0.022(3) 0.027(3) 0.017(3)
C26 0.055(3) 0.054(3) 0.034(2) -0.007(2) 0.017(2) 0.011(2)
C27 0.048(3) 0.062(3) 0.040(3) 0.004(2) 0.025(2) 0.014(3)
C28 0.039(3) 0.057(3) 0.052(3) 0.011(2) 0.028(2) 0.002(2)
C29 0.056(3) 0.082(4) 0.078(4) 0.012(3) 0.046(3) 0.004(3)
C30 0.060(4) 0.101(5) 0.102(4) 0.014(4) 0.055(3) -0.011(3)
C31 0.056(4) 0.087(4) 0.093(4) 0.012(4) 0.035(3) -0.019(3)
C32 0.046(3) 0.060(3) 0.072(3) 0.007(3) 0.027(3) -0.014(3)
C33 0.037(3) 0.046(3) 0.053(3) 0.008(2) 0.023(2) -0.005(2)
C34 0.048(3) 0.032(2) 0.040(2) -0.002(2) 0.017(2) -0.009(2)
C35 0.051(3) 0.028(2) 0.042(2) 0.0003(18) 0.025(2) 0.002(2)
C36 0.072(4) 0.030(2) 0.062(3) -0.008(2) 0.035(3) -0.003(2)
C37 0.089(4) 0.037(3) 0.077(4) -0.005(3) 0.052(3) 0.012(3)
C38 0.066(4) 0.046(3) 0.077(3) 0.010(3) 0.047(3) 0.019(3)
C39 0.050(3) 0.039(3) 0.052(3) 0.006(2) 0.029(2) 0.007(2)
C40 0.043(3) 0.029(2) 0.033(2) 0.0052(17) 0.0192(19) 0.0071(19)
C41 0.035(3) 0.060(3) 0.032(2) -0.002(2) 0.0103(19) 0.006(2)
C42 0.053(3) 0.078(4) 0.054(3) -0.018(3) 0.021(3) -0.003(3)
C43 0.063(4) 0.096(5) 0.062(3) -0.031(3) 0.025(3) 0.003(3)
C44 0.070(4) 0.108(5) 0.056(3) -0.013(3) 0.035(3) 0.008(4)
C45 0.066(4) 0.092(4) 0.053(3) 0.007(3) 0.039(3) 0.009(3)
C46 0.050(3) 0.066(3) 0.042(2) 0.006(2) 0.024(2) 0.007(2)
C47 0.070(4) 0.063(4) 0.065(3) 0.017(3) 0.044(3) 0.001(3)
C48 0.048(4) 0.050(3) 0.041(3) 0.006(3) 0.017(3) -0.008(3)
C50 0.069(5) 0.062(4) 0.057(4) 0.014(3) 0.005(4) -0.024(4)
C51 0.075(5) 0.051(4) 0.063(4) 0.015(3) -0.002(4) -0.021(4)
C53 0.052(4) 0.044(3) 0.044(3) 0.007(3) 0.011(3) -0.009(3)
C48' 0.051(5) 0.050(5) 0.044(5) 0.012(5) 0.018(5) -0.011(5)
C50' 0.070(6) 0.059(6) 0.062(5) 0.013(5) 0.005(5) -0.021(5)
C51' 0.070(6) 0.054(6) 0.062(6) 0.010(5) 0.003(5) -0.018(5)
C53' 0.055(6) 0.047(5) 0.046(5) 0.009(5) 0.012(5) -0.012(5)
C49 0.062(3) 0.066(3) 0.062(3) 0.016(3) 0.020(3) -0.016(3)
C52 0.068(4) 0.048(3) 0.058(3) 0.002(3) 0.010(3) -0.006(3)
C54 0.081(4) 0.044(3) 0.057(3) 0.010(3) 0.027(3) 0.018(3)
C55 0.064(3) 0.059(3) 0.045(3) 0.010(2) 0.023(2) 0.023(3)
C56 0.079(4) 0.080(4) 0.071(4) 0.021(3) 0.035(3) 0.039(4)
C57 0.075(4) 0.104(5) 0.080(4) 0.018(4) 0.034(3) 0.046(4)
C58 0.051(3) 0.115(5) 0.067(3) 0.003(4) 0.029(3) 0.028(4)
C59 0.046(3) 0.085(4) 0.049(3) -0.006(3) 0.022(2) 0.013(3)
C60 0.047(3) 0.061(3) 0.030(2) 0.002(2) 0.014(2) 0.012(3)
C61 0.050(5) 0.164(9) 0.125(7) 0.081(7) 0.041(5) 0.013(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.202(3) . ?
Dy1 O1 2.302(3) . ?
Dy1 O3 2.339(3) . ?
Dy1 O4 2.382(3) . ?
Dy1 N1 2.525(4) . ?
Dy1 N4 2.538(4) . ?
Dy1 N2 2.560(4) . ?
Dy1 N3 2.650(4) . ?
Dy1 Dy2 3.9085(14) . ?
Dy2 O5 2.168(3) . ?
Dy2 O6 2.200(4) . ?
Dy2 O3 2.335(3) . ?
Dy2 O4 2.361(3) . ?
Dy2 O7 2.404(4) . ?
Dy2 N5 2.461(5) . ?
Dy2 N6 2.529(4) . ?
O1 C1 1.304(5) . ?
O2 C20 1.317(6) . ?
O3 C21 1.343(5) . ?
O4 C40 1.334(5) . ?
O5 C41 1.327(6) . ?
O6 C60 1.297(6) . ?
O7 C61 1.405(8) . ?
O7 H71 0.847(10) . ?
N1 C7 1.276(6) . ?
N1 C8 1.466(6) . ?
N2 C14 1.280(6) . ?
N2 C13 1.492(6) . ?
N3 C27 1.278(6) . ?
N3 C28 1.479(6) . ?
N4 C34 1.283(6) . ?
N4 C33 1.465(6) . ?
N5 C47 1.280(7) . ?
N5 C48' 1.49(2) . ?
N5 C48 1.509(8) . ?
N6 C54 1.294(8) . ?
N6 C53 1.508(9) . ?
N6 C53' 1.53(3) . ?
C1 C2 1.410(7) . ?
C1 C6 1.424(7) . ?
C2 C3 1.374(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.368(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.403(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.445(7) . ?
C7 H7 0.9300 . ?
C8 C13 1.510(7) . ?
C8 C9 1.519(7) . ?
C8 H8 0.9800 . ?
C9 C10 1.523(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.494(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.523(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.523(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13 0.9800 . ?
C14 C15 1.434(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.406(7) . ?
C15 C20 1.426(8) . ?
C16 C17 1.378(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.383(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.376(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.419(7) . ?
C19 H19 0.9300 . ?
C21 C26 1.395(8) . ?
C21 C22 1.405(7) . ?
C22 C23 1.371(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.377(11) . ?
C23 H23 0.9300 . ?
C24 C25 1.368(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.399(8) . ?
C25 H25 0.9300 . ?
C26 C27 1.463(8) . ?
C27 H27 0.9300 . ?
C28 C33 1.516(7) . ?
C28 C29 1.519(7) . ?
C28 H28 0.9800 . ?
C29 C30 1.517(9) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.503(10) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.505(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.513(7) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33 0.9800 . ?
C34 C35 1.442(7) . ?
C34 H34 0.9300 . ?
C35 C40 1.413(7) . ?
C35 C36 1.413(7) . ?
C36 C37 1.366(8) . ?
C36 H36 0.9300 . ?
C37 C38 1.373(9) . ?
C37 H37 0.9300 . ?
C38 C39 1.374(7) . ?
C38 H38 0.9300 . ?
C39 C40 1.388(7) . ?
C39 H39 0.9300 . ?
C41 C42 1.398(8) . ?
C41 C46 1.423(8) . ?
C42 C43 1.393(9) . ?
C42 H42 0.9300 . ?
C43 C44 1.378(10) . ?
C43 H43 0.9300 . ?
C44 C45 1.354(9) . ?
C44 H44 0.9300 . ?
C45 C46 1.405(8) . ?
C45 H45 0.9300 . ?
C46 C47 1.435(8) . ?
C47 H47 0.9300 . ?
C48 C49 1.509(9) . ?
C48 C53 1.513(12) . ?
C48 H48 0.9800 . ?
C50 C51 1.497(16) . ?
C50 C49 1.571(11) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 C52 1.494(12) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C53 C52 1.531(9) . ?
C53 H53 0.9800 . ?
C48' C53' 1.53(4) . ?
C48' C49 1.66(3) . ?
C48' H48' 0.9800 . ?
C50' C49 1.39(3) . ?
C50' C51' 1.46(6) . ?
C50' H50C 0.9700 . ?
C50' H50D 0.9700 . ?
C51' C52 1.67(4) . ?
C51' H51C 0.9700 . ?
C51' H51D 0.9700 . ?
C53' C52 1.57(3) . ?
C53' H53' 0.9800 . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C54 C55 1.426(9) . ?
C54 H54 0.9300 . ?
C55 C60 1.411(8) . ?
C55 C56 1.417(8) . ?
C56 C57 1.361(11) . ?
C56 H56 0.9300 . ?
C57 C58 1.376(11) . ?
C57 H57 0.9300 . ?
C58 C59 1.391(9) . ?
C58 H58 0.9300 . ?
C59 C60 1.410(8) . ?
C59 H59 0.9300 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 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
O2 Dy1 O1 83.42(13) . . ?
O2 Dy1 O3 148.38(13) . . ?
O1 Dy1 O3 77.58(12) . . ?
O2 Dy1 O4 86.76(12) . . ?
O1 Dy1 O4 87.05(11) . . ?
O3 Dy1 O4 67.40(10) . . ?
O2 Dy1 N1 113.31(13) . . ?
O1 Dy1 N1 72.19(12) . . ?
O3 Dy1 N1 84.67(11) . . ?
O4 Dy1 N1 148.40(12) . . ?
O2 Dy1 N4 76.86(13) . . ?
O1 Dy1 N4 150.26(12) . . ?
O3 Dy1 N4 108.74(12) . . ?
O4 Dy1 N4 69.97(12) . . ?
N1 Dy1 N4 136.30(13) . . ?
O2 Dy1 N2 73.35(13) . . ?
O1 Dy1 N2 113.19(12) . . ?
O3 Dy1 N2 137.59(12) . . ?
O4 Dy1 N2 149.03(11) . . ?
N1 Dy1 N2 62.57(12) . . ?
N4 Dy1 N2 82.31(12) . . ?
O2 Dy1 N3 134.33(13) . . ?
O1 Dy1 N3 142.13(12) . . ?
O3 Dy1 N3 69.41(12) . . ?
O4 Dy1 N3 96.67(11) . . ?
N1 Dy1 N3 86.46(13) . . ?
N4 Dy1 N3 62.13(12) . . ?
N2 Dy1 N3 81.70(13) . . ?
O2 Dy1 Dy2 118.13(10) . . ?
O1 Dy1 Dy2 78.24(8) . . ?
O3 Dy1 Dy2 33.22(8) . . ?
O4 Dy1 Dy2 34.35(7) . . ?
N1 Dy1 Dy2 115.85(9) . . ?
N4 Dy1 Dy2 91.60(9) . . ?
N2 Dy1 Dy2 165.55(9) . . ?
N3 Dy1 Dy2 83.87(9) . . ?
O5 Dy2 O6 88.96(13) . . ?
O5 Dy2 O3 84.64(12) . . ?
O6 Dy2 O3 148.12(13) . . ?
O5 Dy2 O4 151.17(12) . . ?
O6 Dy2 O4 118.87(13) . . ?
O3 Dy2 O4 67.81(10) . . ?
O5 Dy2 O7 103.28(15) . . ?
O6 Dy2 O7 75.97(14) . . ?
O3 Dy2 O7 75.22(13) . . ?
O4 Dy2 O7 78.51(13) . . ?
O5 Dy2 N5 74.58(15) . . ?
O6 Dy2 N5 121.86(15) . . ?
O3 Dy2 N5 86.38(15) . . ?
O4 Dy2 N5 94.63(15) . . ?
O7 Dy2 N5 161.60(15) . . ?
O5 Dy2 N6 112.81(14) . . ?
O6 Dy2 N6 72.80(15) . . ?
O3 Dy2 N6 138.06(14) . . ?
O4 Dy2 N6 84.64(12) . . ?
O7 Dy2 N6 131.00(16) . . ?
N5 Dy2 N6 64.21(16) . . ?
O5 Dy2 Dy1 117.82(9) . . ?
O6 Dy2 Dy1 141.63(10) . . ?
O3 Dy2 Dy1 33.28(7) . . ?
O4 Dy2 Dy1 34.70(7) . . ?
O7 Dy2 Dy1 71.59(9) . . ?
N5 Dy2 Dy1 92.99(12) . . ?
N6 Dy2 Dy1 115.08(10) . . ?
C1 O1 Dy1 141.3(3) . . ?
C20 O2 Dy1 134.0(3) . . ?
C21 O3 Dy2 129.1(3) . . ?
C21 O3 Dy1 117.1(3) . . ?
Dy2 O3 Dy1 113.51(12) . . ?
C40 O4 Dy2 125.3(3) . . ?
C40 O4 Dy1 123.7(3) . . ?
Dy2 O4 Dy1 110.96(12) . . ?
C41 O5 Dy2 138.9(3) . . ?
C60 O6 Dy2 144.2(4) . . ?
C61 O7 Dy2 134.2(4) . . ?
C61 O7 H71 101(5) . . ?
Dy2 O7 H71 123(5) . . ?
C7 N1 C8 119.4(4) . . ?
C7 N1 Dy1 131.4(4) . . ?
C8 N1 Dy1 108.2(3) . . ?
C14 N2 C13 114.6(4) . . ?
C14 N2 Dy1 126.2(4) . . ?
C13 N2 Dy1 118.5(3) . . ?
C27 N3 C28 117.2(4) . . ?
C27 N3 Dy1 123.2(4) . . ?
C28 N3 Dy1 118.6(3) . . ?
C34 N4 C33 121.1(4) . . ?
C34 N4 Dy1 125.0(3) . . ?
C33 N4 Dy1 113.3(3) . . ?
C47 N5 C48' 103.6(11) . . ?
C47 N5 C48 122.0(5) . . ?
C48' N5 C48 35.9(10) . . ?
C47 N5 Dy2 128.7(4) . . ?
C48' N5 Dy2 121.2(11) . . ?
C48 N5 Dy2 109.1(4) . . ?
C54 N6 C53 113.2(6) . . ?
C54 N6 C53' 129.0(12) . . ?
C53 N6 C53' 26.4(10) . . ?
C54 N6 Dy2 128.0(4) . . ?
C53 N6 Dy2 117.4(4) . . ?
C53' N6 Dy2 102.4(11) . . ?
O1 C1 C2 120.1(5) . . ?
O1 C1 C6 122.9(5) . . ?
C2 C1 C6 117.0(5) . . ?
C3 C2 C1 121.5(5) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C4 C3 C2 121.4(6) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 118.8(5) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C4 C5 C6 122.4(6) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C5 C6 C1 118.9(5) . . ?
C5 C6 C7 117.2(5) . . ?
C1 C6 C7 123.9(4) . . ?
N1 C7 C6 127.3(5) . . ?
N1 C7 H7 116.3 . . ?
C6 C7 H7 116.3 . . ?
N1 C8 C13 107.1(4) . . ?
N1 C8 C9 119.0(5) . . ?
C13 C8 C9 111.0(4) . . ?
N1 C8 H8 106.3 . . ?
C13 C8 H8 106.3 . . ?
C9 C8 H8 106.3 . . ?
C8 C9 C10 109.6(5) . . ?
C8 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
C8 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
C11 C10 C9 112.1(5) . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10B 109.2 . . ?
C9 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C10 C11 C12 113.4(5) . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 C13 110.7(5) . . ?
C11 C12 H12A 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N2 C13 C8 108.3(4) . . ?
N2 C13 C12 113.8(5) . . ?
C8 C13 C12 112.3(5) . . ?
N2 C13 H13 107.4 . . ?
C8 C13 H13 107.4 . . ?
C12 C13 H13 107.4 . . ?
N2 C14 C15 126.5(5) . . ?
N2 C14 H14 116.7 . . ?
C15 C14 H14 116.7 . . ?
C16 C15 C20 119.8(6) . . ?
C16 C15 C14 117.1(6) . . ?
C20 C15 C14 122.9(5) . . ?
C17 C16 C15 120.6(7) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 119.8(7) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 121.4(7) . . ?
C19 C18 H18 119.3 . . ?
C17 C18 H18 119.3 . . ?
C18 C19 C20 120.6(7) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
O2 C20 C19 118.8(6) . . ?
O2 C20 C15 123.4(5) . . ?
C19 C20 C15 117.7(5) . . ?
O3 C21 C26 120.7(5) . . ?
O3 C21 C22 120.1(5) . . ?
C26 C21 C22 119.1(5) . . ?
C23 C22 C21 120.4(7) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C22 C23 C24 120.1(7) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 120.7(6) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 120.2(7) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 119.3(6) . . ?
C21 C26 C27 122.3(5) . . ?
C25 C26 C27 118.3(6) . . ?
N3 C27 C26 123.9(5) . . ?
N3 C27 H27 118.0 . . ?
C26 C27 H27 118.0 . . ?
N3 C28 C33 109.5(4) . . ?
N3 C28 C29 115.0(5) . . ?
C33 C28 C29 110.4(5) . . ?
N3 C28 H28 107.2 . . ?
C33 C28 H28 107.2 . . ?
C29 C28 H28 107.2 . . ?
C30 C29 C28 111.9(6) . . ?
C30 C29 H29A 109.2 . . ?
C28 C29 H29A 109.2 . . ?
C30 C29 H29B 109.2 . . ?
C28 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
C31 C30 C29 111.8(6) . . ?
C31 C30 H30A 109.3 . . ?
C29 C30 H30A 109.3 . . ?
C31 C30 H30B 109.3 . . ?
C29 C30 H30B 109.3 . . ?
H30A C30 H30B 107.9 . . ?
C30 C31 C32 112.5(6) . . ?
C30 C31 H31A 109.1 . . ?
C32 C31 H31A 109.1 . . ?
C30 C31 H31B 109.1 . . ?
C32 C31 H31B 109.1 . . ?
H31A C31 H31B 107.8 . . ?
C31 C32 C33 111.7(5) . . ?
C31 C32 H32A 109.3 . . ?
C33 C32 H32A 109.3 . . ?
C31 C32 H32B 109.3 . . ?
C33 C32 H32B 109.3 . . ?
H32A C32 H32B 107.9 . . ?
N4 C33 C32 118.2(5) . . ?
N4 C33 C28 107.4(4) . . ?
C32 C33 C28 111.7(5) . . ?
N4 C33 H33 106.3 . . ?
C32 C33 H33 106.3 . . ?
C28 C33 H33 106.3 . . ?
N4 C34 C35 125.9(5) . . ?
N4 C34 H34 117.0 . . ?
C35 C34 H34 117.0 . . ?
C40 C35 C36 118.4(5) . . ?
C40 C35 C34 123.8(4) . . ?
C36 C35 C34 117.7(5) . . ?
C37 C36 C35 121.9(6) . . ?
C37 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
C36 C37 C38 119.4(5) . . ?
C36 C37 H37 120.3 . . ?
C38 C37 H37 120.3 . . ?
C37 C38 C39 120.0(6) . . ?
C37 C38 H38 120.0 . . ?
C39 C38 H38 120.0 . . ?
C38 C39 C40 122.5(6) . . ?
C38 C39 H39 118.7 . . ?
C40 C39 H39 118.7 . . ?
O4 C40 C39 120.4(4) . . ?
O4 C40 C35 121.8(4) . . ?
C39 C40 C35 117.8(4) . . ?
O5 C41 C42 119.3(5) . . ?
O5 C41 C46 122.5(5) . . ?
C42 C41 C46 118.2(5) . . ?
C43 C42 C41 120.4(7) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C44 C43 C42 121.1(7) . . ?
C44 C43 H43 119.4 . . ?
C42 C43 H43 119.4 . . ?
C45 C44 C43 119.3(6) . . ?
C45 C44 H44 120.4 . . ?
C43 C44 H44 120.4 . . ?
C44 C45 C46 122.1(7) . . ?
C44 C45 H45 118.9 . . ?
C46 C45 H45 118.9 . . ?
C45 C46 C41 118.9(6) . . ?
C45 C46 C47 118.0(6) . . ?
C41 C46 C47 123.1(5) . . ?
N5 C47 C46 127.4(6) . . ?
N5 C47 H47 116.3 . . ?
C46 C47 H47 116.3 . . ?
N5 C48 C49 116.3(6) . . ?
N5 C48 C53 104.4(6) . . ?
C49 C48 C53 109.4(6) . . ?
N5 C48 H48 108.8 . . ?
C49 C48 H48 108.8 . . ?
C53 C48 H48 108.8 . . ?
C51 C50 C49 110.1(7) . . ?
C51 C50 H50A 109.6 . . ?
C49 C50 H50A 109.6 . . ?
C51 C50 H50B 109.6 . . ?
C49 C50 H50B 109.6 . . ?
H50A C50 H50B 108.2 . . ?
C52 C51 C50 111.6(7) . . ?
C52 C51 H51A 109.3 . . ?
C50 C51 H51A 109.3 . . ?
C52 C51 H51B 109.3 . . ?
C50 C51 H51B 109.3 . . ?
H51A C51 H51B 108.0 . . ?
N6 C53 C48 109.0(6) . . ?
N6 C53 C52 114.6(7) . . ?
C48 C53 C52 110.1(6) . . ?
N6 C53 H53 107.6 . . ?
C48 C53 H53 107.6 . . ?
C52 C53 H53 107.6 . . ?
N5 C48' C53' 100.2(18) . . ?
N5 C48' C49 108.6(17) . . ?
C53' C48' C49 100.7(18) . . ?
N5 C48' H48' 115.2 . . ?
C53' C48' H48' 115.2 . . ?
C49 C48' H48' 115.2 . . ?
C49 C50' C51' 103(3) . . ?
C49 C50' H50C 111.2 . . ?
C51' C50' H50C 111.2 . . ?
C49 C50' H50D 111.2 . . ?
C51' C50' H50D 111.2 . . ?
H50C C50' H50D 109.1 . . ?
C50' C51' C52 114(2) . . ?
C50' C51' H51C 108.8 . . ?
C52 C51' H51C 108.8 . . ?
C50' C51' H51D 108.8 . . ?
C52 C51' H51D 108.8 . . ?
H51C C51' H51D 107.7 . . ?
N6 C53' C48' 101.3(19) . . ?
N6 C53' C52 111(2) . . ?
C48' C53' C52 111(2) . . ?
N6 C53' H53' 110.9 . . ?
C48' C53' H53' 110.9 . . ?
C52 C53' H53' 110.9 . . ?
C50' C49 C48 121.9(17) . . ?
C50' C49 C50 38.1(12) . . ?
C48 C49 C50 108.0(7) . . ?
C50' C49 C48' 109.0(17) . . ?
C48 C49 C48' 33.6(8) . . ?
C50 C49 C48' 118.8(12) . . ?
C50' C49 H49A 124.4 . . ?
C48 C49 H49A 110.1 . . ?
C50 C49 H49A 110.1 . . ?
C48' C49 H49A 125.5 . . ?
C50' C49 H49B 72.0 . . ?
C48 C49 H49B 110.1 . . ?
C50 C49 H49B 110.1 . . ?
C48' C49 H49B 76.7 . . ?
H49A C49 H49B 108.4 . . ?
C51 C52 C53 111.6(7) . . ?
C51 C52 C53' 116.8(13) . . ?
C53 C52 C53' 25.8(9) . . ?
C51 C52 C51' 22.3(12) . . ?
C53 C52 C51' 106.9(15) . . ?
C53' C52 C51' 102.6(19) . . ?
C51 C52 H52A 109.3 . . ?
C53 C52 H52A 109.3 . . ?
C53' C52 H52A 84.2 . . ?
C51' C52 H52A 91.7 . . ?
C51 C52 H52B 109.3 . . ?
C53 C52 H52B 109.3 . . ?
C53' C52 H52B 124.9 . . ?
C51' C52 H52B 129.4 . . ?
H52A C52 H52B 108.0 . . ?
N6 C54 C55 128.6(6) . . ?
N6 C54 H54 115.7 . . ?
C55 C54 H54 115.7 . . ?
C60 C55 C56 119.5(7) . . ?
C60 C55 C54 122.9(5) . . ?
C56 C55 C54 117.1(6) . . ?
C57 C56 C55 120.9(8) . . ?
C57 C56 H56 119.6 . . ?
C55 C56 H56 119.6 . . ?
C56 C57 C58 120.5(7) . . ?
C56 C57 H57 119.8 . . ?
C58 C57 H57 119.8 . . ?
C57 C58 C59 120.2(7) . . ?
C57 C58 H58 119.9 . . ?
C59 C58 H58 119.9 . . ?
C58 C59 C60 121.1(7) . . ?
C58 C59 H59 119.5 . . ?
C60 C59 H59 119.5 . . ?
O6 C60 C59 119.7(6) . . ?
O6 C60 C55 122.5(6) . . ?
C59 C60 C55 117.8(6) . . ?
O7 C61 H61A 109.5 . . ?
O7 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
O7 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H71 O1 0.847(10) 1.89(3) 2.690(5) 156(7) .
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 1.048
_refine_diff_density_min -1.126
_refine_diff_density_rms 0.112