# Electronic Supplementary Material (ESI) for Dalton Transactions
# 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. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
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#  except for the purpose of generating routine backup copies 
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data_zxy-1
_database_code_depnum_ccdc_archive 'CCDC 905489'
#TrackingRef '1-La.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C34 H36 La N7 O13), (C H4 O)'
_chemical_formula_sum            'C69 H76 La2 N14 O27'
_chemical_formula_weight         1811.26
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'
La La -0.2871 2.4523 '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                   10.0985(10)
_cell_length_b                   37.415(4)
_cell_length_c                   10.9657(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.4810(10)
_cell_angle_gamma                90.00
_cell_volume                     3800.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27355
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.42
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1836
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7619
_exptl_absorpt_correction_T_max  0.8079
_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            20570
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6645
_reflns_number_gt                6355
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP (Sheldrick, 1993)'
_computing_publication_material  SHELXL-97
_refine_special_details          
;
OMIT 1 2 0
OMIT -1 1 2
OMIT -3.00 50.00
dfix 1.50 0.01 o14 c35
dfix 0.85 0.01 h6 n1 h13 n2 h24 n3 h31 n4
isor 0.01 c21 c22 o14
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^)+(0.0076P)^2^+7.0312P] 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         6645
_refine_ls_number_parameters     506
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.0932
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.353
_refine_ls_restrained_S_all      1.357
_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
C1 C 0.6426(5) 0.96129(13) 0.7364(5) 0.0413(12) Uani 1 1 d . . .
C2 C 0.7662(6) 0.94936(15) 0.7201(6) 0.0535(14) Uani 1 1 d . . .
H1 H 0.8046 0.9270 0.7524 0.064 Uiso 1 1 calc R . .
C3 C 0.8314(7) 0.97048(18) 0.6564(6) 0.0635(17) Uani 1 1 d . . .
H2 H 0.9107 0.9616 0.6432 0.076 Uiso 1 1 calc R . .
C4 C 0.7819(7) 1.00437(18) 0.6121(6) 0.0661(18) Uani 1 1 d . . .
H3 H 0.8280 1.0182 0.5703 0.079 Uiso 1 1 calc R . .
C5 C 0.6648(7) 1.01742(16) 0.6299(5) 0.0600(16) Uani 1 1 d . . .
H4 H 0.6316 1.0403 0.6004 0.072 Uiso 1 1 calc R . .
C6 C 0.5935(6) 0.99670(14) 0.6923(5) 0.0467(13) Uani 1 1 d . . .
C7 C 0.4707(6) 1.01142(14) 0.7065(5) 0.0518(14) Uani 1 1 d . . .
H5 H 0.4436 1.0346 0.6762 0.062 Uiso 1 1 calc R . .
C8 C 0.2681(6) 1.00948(15) 0.7747(6) 0.0575(15) Uani 1 1 d . . .
H7 H 0.1811 0.9986 0.7104 0.069 Uiso 1 1 calc R . .
H8 H 0.2628 1.0350 0.7586 0.069 Uiso 1 1 calc R . .
C9 C 0.2780(6) 1.00230(15) 0.9134(6) 0.0552(14) Uani 1 1 d . . .
H10 H 0.3647 1.0135 0.9767 0.066 Uiso 1 1 calc R . .
H9B H 0.2871 0.9767 0.9296 0.066 Uiso 1 1 calc R . .
C10 C 0.1490(6) 1.01584(15) 0.9376(6) 0.0593(16) Uani 1 1 d . . .
H11 H 0.0611 1.0059 0.8714 0.071 Uiso 1 1 calc R . .
H12 H 0.1566 1.0081 1.0245 0.071 Uiso 1 1 calc R . .
C11 C 0.0376(6) 1.07277(17) 0.8436(6) 0.0619(17) Uani 1 1 d . . .
H14 H -0.0425 1.0600 0.7875 0.074 Uiso 1 1 calc R . .
C12 C 0.0354(6) 1.11013(17) 0.8269(5) 0.0531(14) Uani 1 1 d . . .
C13 C -0.0862(7) 1.1258(2) 0.7255(6) 0.0720(19) Uani 1 1 d . . .
H15 H -0.1646 1.1115 0.6761 0.086 Uiso 1 1 calc R . .
C14 C -0.0908(7) 1.1612(2) 0.6987(6) 0.080(2) Uani 1 1 d . . .
H16 H -0.1714 1.1712 0.6319 0.096 Uiso 1 1 calc R . .
C15 C 0.0273(8) 1.1823(2) 0.7731(7) 0.078(2) Uani 1 1 d . . .
H17 H 0.0253 1.2066 0.7545 0.093 Uiso 1 1 calc R . .
C16 C 0.1464(6) 1.16815(17) 0.8731(6) 0.0629(16) Uani 1 1 d . . .
H18 H 0.2238 1.1831 0.9200 0.076 Uiso 1 1 calc R . .
C17 C 0.1547(5) 1.13170(15) 0.9066(5) 0.0462(13) Uani 1 1 d . . .
C18 C 0.5445(5) 0.78560(13) 0.8815(5) 0.0443(12) Uani 1 1 d . . .
C19 C 0.6342(7) 0.77722(16) 0.8147(6) 0.0631(16) Uani 1 1 d . . .
H19 H 0.6730 0.7956 0.7820 0.076 Uiso 1 1 calc R . .
C20 C 0.6649(9) 0.74240(19) 0.7971(8) 0.091(2) Uani 1 1 d . . .
H20 H 0.7259 0.7374 0.7542 0.109 Uiso 1 1 calc R . .
C21 C 0.6058(9) 0.71441(19) 0.8426(8) 0.091(2) Uani 1 1 d U . .
H21 H 0.6262 0.6909 0.8291 0.109 Uiso 1 1 calc R . .
C22 C 0.5195(8) 0.72149(17) 0.9059(7) 0.079(2) Uani 1 1 d U . .
H22 H 0.4824 0.7027 0.9380 0.095 Uiso 1 1 calc R . .
C23 C 0.4836(6) 0.75691(14) 0.9250(6) 0.0525(14) Uani 1 1 d . . .
C24 C 0.3840(7) 0.76251(16) 0.9845(6) 0.0617(16) Uani 1 1 d . . .
H23 H 0.3479 0.7424 1.0109 0.074 Uiso 1 1 calc R . .
C25 C 0.2277(7) 0.7980(2) 1.0584(7) 0.079(2) Uani 1 1 d . . .
H26 H 0.2562 0.8169 1.1241 0.095 Uiso 1 1 calc R . .
H25 H 0.2183 0.7761 1.1017 0.095 Uiso 1 1 calc R . .
C26 C 0.0786(7) 0.8075(2) 0.9437(8) 0.085(2) Uani 1 1 d . . .
H27 H 0.0673 0.7941 0.8645 0.102 Uiso 1 1 calc R . .
H28 H 0.0011 0.8008 0.9700 0.102 Uiso 1 1 calc R . .
C27 C 0.0689(6) 0.84608(19) 0.9135(6) 0.0679(17) Uani 1 1 d . . .
H30 H 0.0761 0.8595 0.9916 0.082 Uiso 1 1 calc R . .
H29 H 0.1490 0.8530 0.8910 0.082 Uiso 1 1 calc R . .
C28 C -0.0785(6) 0.86124(17) 0.6815(6) 0.0618(16) Uani 1 1 d . . .
H32 H 0.0060 0.8608 0.6668 0.074 Uiso 1 1 calc R . .
C29 C -0.2079(5) 0.86865(14) 0.5725(5) 0.0459(12) Uani 1 1 d . . .
C30 C -0.2011(7) 0.87553(15) 0.4480(6) 0.0558(15) Uani 1 1 d . . .
H33 H -0.1124 0.8749 0.4410 0.067 Uiso 1 1 calc R . .
C31 C -0.3227(7) 0.88309(16) 0.3384(6) 0.0617(16) Uani 1 1 d . . .
H34 H -0.3182 0.8878 0.2569 0.074 Uiso 1 1 calc R . .
C32 C -0.4542(7) 0.88363(17) 0.3520(6) 0.0640(17) Uani 1 1 d . . .
H35 H -0.5380 0.8885 0.2775 0.077 Uiso 1 1 calc R . .
C33 C -0.4651(6) 0.87735(15) 0.4702(5) 0.0509(13) Uani 1 1 d . . .
H36 H -0.5553 0.8778 0.4742 0.061 Uiso 1 1 calc R . .
C34 C -0.3420(5) 0.87023(12) 0.5860(5) 0.0392(11) Uani 1 1 d . . .
La1 La 0.49386(3) 0.879383(7) 0.81365(3) 0.03200(9) Uani 1 1 d . . .
N1 N 0.3945(5) 0.99478(11) 0.7587(4) 0.0495(11) Uani 1 1 d D . .
H6 H 0.4169 0.9736 0.7880 0.074 Uiso 1 1 d RD . .
N2 N 0.1421(5) 1.05480(13) 0.9306(5) 0.0564(12) Uani 1 1 d D . .
H13 H 0.2129 1.0681 0.9758 0.085 Uiso 1 1 d RD . .
N3 N 0.3396(5) 0.79331(13) 1.0049(5) 0.0573(12) Uani 1 1 d D . .
H24 H 0.3777 0.8113 0.9842 0.086 Uiso 1 1 d RD . .
N4 N -0.0683(5) 0.85490(14) 0.8019(5) 0.0625(13) Uani 1 1 d D . .
H31 H -0.1519 0.8525 0.8028 0.094 Uiso 1 1 d RD . .
N5 N 0.2188(5) 0.92096(10) 0.6253(4) 0.0427(10) Uani 1 1 d . . .
N6 N 0.2660(5) 0.82194(11) 0.6428(4) 0.0460(10) Uani 1 1 d . . .
N7 N 0.3984(5) 0.90918(13) 1.0309(4) 0.0500(11) Uani 1 1 d . . .
O1 O 0.5786(4) 0.94145(9) 0.7947(4) 0.0473(9) Uani 1 1 d . . .
O2 O 0.2647(4) 1.11815(9) 1.0045(3) 0.0502(9) Uani 1 1 d . . .
O3 O 0.5176(4) 0.81858(9) 0.9010(3) 0.0466(8) Uani 1 1 d . . .
O4 O -0.3479(4) 0.86551(9) 0.7010(3) 0.0437(8) Uani 1 1 d . . .
O5 O 0.3062(4) 0.90791(10) 0.5812(4) 0.0531(9) Uani 1 1 d . . .
O6 O 0.1034(4) 0.93372(11) 0.5492(4) 0.0650(11) Uani 1 1 d . . .
O7 O 0.2549(4) 0.92061(9) 0.7490(3) 0.0491(9) Uani 1 1 d . . .
O8 O 0.3723(4) 0.82805(10) 0.6148(4) 0.0549(10) Uani 1 1 d . . .
O9 O 0.1883(5) 0.79610(11) 0.5980(5) 0.0848(15) Uani 1 1 d . . .
O10 O 0.2427(4) 0.84379(9) 0.7192(4) 0.0485(9) Uani 1 1 d . . .
O11 O 0.4860(4) 0.92744(10) 1.0020(4) 0.0568(10) Uani 1 1 d . . .
O12 O 0.3256(5) 0.92213(12) 1.0862(4) 0.0780(14) Uani 1 1 d . . .
O13 O 0.3884(4) 0.87657(10) 0.9985(4) 0.0531(9) Uani 1 1 d . . .
O14 O 1.031(3) 0.7657(11) 0.696(3) 0.334(15) Uiso 0.50 1 d PD . .
H14A H 1.0936 0.7600 0.6695 0.501 Uiso 0.50 1 calc PR . .
C35 C 0.891(3) 0.7712(8) 0.580(3) 0.223(14) Uiso 0.50 1 d PD . .
H35A H 0.8232 0.7823 0.6092 0.335 Uiso 0.50 1 calc PR . .
H35B H 0.8536 0.7485 0.5400 0.335 Uiso 0.50 1 calc PR . .
H35C H 0.9060 0.7862 0.5156 0.335 Uiso 0.50 1 calc PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.042(3) 0.044(3) 0.039(3) -0.009(2) 0.017(2) -0.013(2)
C2 0.055(4) 0.049(3) 0.068(4) -0.010(3) 0.036(3) -0.012(3)
C3 0.059(4) 0.078(4) 0.063(4) -0.026(3) 0.035(3) -0.029(3)
C4 0.071(5) 0.075(4) 0.057(4) -0.002(3) 0.030(3) -0.036(4)
C5 0.066(4) 0.052(3) 0.051(3) 0.006(3) 0.012(3) -0.020(3)
C6 0.052(3) 0.041(3) 0.045(3) 0.000(2) 0.016(3) -0.010(2)
C7 0.055(4) 0.039(3) 0.051(3) -0.003(2) 0.010(3) -0.006(3)
C8 0.047(3) 0.053(3) 0.065(4) -0.008(3) 0.015(3) 0.010(3)
C9 0.051(4) 0.047(3) 0.064(4) -0.013(3) 0.020(3) -0.001(3)
C10 0.050(4) 0.059(4) 0.068(4) -0.025(3) 0.022(3) -0.017(3)
C11 0.031(3) 0.078(4) 0.066(4) -0.035(3) 0.009(3) -0.003(3)
C12 0.033(3) 0.078(4) 0.045(3) -0.018(3) 0.013(2) 0.007(3)
C13 0.042(4) 0.102(6) 0.054(4) -0.017(4) 0.000(3) 0.015(4)
C14 0.055(4) 0.121(7) 0.048(4) 0.010(4) 0.005(3) 0.029(4)
C15 0.070(5) 0.092(5) 0.067(4) 0.029(4) 0.022(4) 0.026(4)
C16 0.046(4) 0.076(4) 0.056(4) 0.010(3) 0.010(3) 0.003(3)
C17 0.033(3) 0.064(4) 0.042(3) -0.001(3) 0.015(2) 0.010(2)
C18 0.037(3) 0.039(3) 0.051(3) 0.007(2) 0.012(2) 0.004(2)
C19 0.061(4) 0.051(3) 0.086(5) 0.008(3) 0.039(4) 0.009(3)
C20 0.103(6) 0.067(5) 0.130(7) 0.000(4) 0.077(6) 0.021(4)
C21 0.110(6) 0.055(4) 0.121(6) 0.001(4) 0.059(5) 0.016(4)
C22 0.091(5) 0.044(3) 0.105(5) 0.012(3) 0.043(4) 0.000(3)
C23 0.052(3) 0.041(3) 0.062(4) 0.012(3) 0.020(3) 0.003(3)
C24 0.059(4) 0.052(4) 0.075(4) 0.020(3) 0.027(3) -0.004(3)
C25 0.062(4) 0.106(6) 0.093(5) 0.040(4) 0.054(4) 0.024(4)
C26 0.055(4) 0.103(6) 0.115(6) 0.037(5) 0.053(4) 0.019(4)
C27 0.045(4) 0.092(5) 0.071(4) -0.009(4) 0.027(3) 0.003(3)
C28 0.047(4) 0.082(4) 0.069(4) -0.004(3) 0.036(3) 0.001(3)
C29 0.033(3) 0.057(3) 0.054(3) -0.003(3) 0.024(3) -0.002(2)
C30 0.056(4) 0.063(4) 0.065(4) -0.006(3) 0.042(3) -0.004(3)
C31 0.076(5) 0.068(4) 0.056(4) 0.008(3) 0.042(4) 0.007(3)
C32 0.067(4) 0.081(4) 0.051(3) 0.012(3) 0.031(3) 0.018(3)
C33 0.047(3) 0.061(3) 0.054(3) 0.002(3) 0.031(3) 0.007(3)
C34 0.037(3) 0.038(3) 0.047(3) -0.002(2) 0.022(2) -0.001(2)
La1 0.02842(15) 0.03409(15) 0.03632(15) 0.00045(11) 0.01588(12) 0.00015(11)
N1 0.050(3) 0.038(2) 0.057(3) -0.005(2) 0.018(2) 0.003(2)
N2 0.037(3) 0.059(3) 0.067(3) -0.026(2) 0.014(2) -0.004(2)
N3 0.046(3) 0.063(3) 0.067(3) 0.022(3) 0.027(2) 0.008(2)
N4 0.035(3) 0.094(4) 0.062(3) 0.000(3) 0.023(2) 0.006(3)
N5 0.040(3) 0.035(2) 0.053(3) 0.003(2) 0.018(2) 0.0000(19)
N6 0.042(3) 0.043(2) 0.050(3) -0.004(2) 0.015(2) 0.002(2)
N7 0.057(3) 0.059(3) 0.037(2) 0.000(2) 0.022(2) 0.009(2)
O1 0.048(2) 0.0367(19) 0.069(2) -0.0004(17) 0.0350(19) -0.0043(16)
O2 0.036(2) 0.053(2) 0.048(2) -0.0001(17) 0.0025(17) -0.0007(16)
O3 0.050(2) 0.0347(19) 0.058(2) 0.0065(16) 0.0240(18) 0.0045(16)
O4 0.0364(19) 0.057(2) 0.0454(19) 0.0012(16) 0.0242(16) 0.0006(16)
O5 0.049(2) 0.065(2) 0.049(2) 0.0027(18) 0.0235(19) 0.0117(19)
O6 0.038(2) 0.075(3) 0.073(3) 0.015(2) 0.013(2) 0.017(2)
O7 0.053(2) 0.054(2) 0.043(2) -0.0035(17) 0.0216(18) 0.0070(18)
O8 0.049(2) 0.067(3) 0.055(2) -0.0021(19) 0.028(2) 0.0103(19)
O9 0.083(3) 0.055(3) 0.105(4) -0.032(3) 0.025(3) -0.032(2)
O10 0.037(2) 0.055(2) 0.057(2) -0.0126(18) 0.0226(18) -0.0016(17)
O11 0.058(3) 0.052(2) 0.062(2) -0.0077(19) 0.027(2) -0.0090(19)
O12 0.104(4) 0.085(3) 0.069(3) 0.006(2) 0.060(3) 0.029(3)
O13 0.060(3) 0.052(2) 0.057(2) -0.0048(18) 0.034(2) -0.0059(19)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.306(5) . ?
C1 C2 1.402(7) . ?
C1 C6 1.430(7) . ?
C2 C3 1.383(7) . ?
C2 H1 0.9300 . ?
C3 C4 1.379(9) . ?
C3 H2 0.9300 . ?
C4 C5 1.364(9) . ?
C4 H3 0.9300 . ?
C5 C6 1.407(7) . ?
C5 H4 0.9300 . ?
C6 C7 1.421(8) . ?
C7 N1 1.287(7) . ?
C7 H5 0.9300 . ?
C8 N1 1.463(7) . ?
C8 C9 1.508(8) . ?
C8 H7 0.9700 . ?
C8 H8 0.9700 . ?
C9 C10 1.516(7) . ?
C9 H10 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.460(7) . ?
C10 H11 0.9700 . ?
C10 H12 0.9700 . ?
C11 N2 1.293(7) . ?
C11 C12 1.409(8) . ?
C11 H14 0.9300 . ?
C12 C13 1.414(8) . ?
C12 C17 1.424(7) . ?
C13 C14 1.354(10) . ?
C13 H15 0.9300 . ?
C14 C15 1.391(10) . ?
C14 H16 0.9300 . ?
C15 C16 1.371(8) . ?
C15 H17 0.9300 . ?
C16 C17 1.406(8) . ?
C16 H18 0.9300 . ?
C17 O2 1.301(6) . ?
C18 O3 1.299(6) . ?
C18 C19 1.409(7) . ?
C18 C23 1.411(7) . ?
C19 C20 1.371(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.393(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.339(9) . ?
C21 H21 0.9300 . ?
C22 C23 1.411(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.416(8) . ?
C24 N3 1.288(7) . ?
C24 H23 0.9300 . ?
C25 N3 1.476(7) . ?
C25 C26 1.571(9) . ?
C25 H26 0.9700 . ?
C25 H25 0.9700 . ?
C26 C27 1.475(9) . ?
C26 H27 0.9700 . ?
C26 H28 0.9700 . ?
C27 N4 1.474(7) . ?
C27 H30 0.9700 . ?
C27 H29 0.9700 . ?
C28 N4 1.304(7) . ?
C28 C29 1.403(8) . ?
C28 H32 0.9300 . ?
C29 C30 1.417(7) . ?
C29 C34 1.420(6) . ?
C30 C31 1.362(8) . ?
C30 H33 0.9300 . ?
C31 C32 1.394(8) . ?
C31 H34 0.9300 . ?
C32 C33 1.364(7) . ?
C32 H35 0.9300 . ?
C33 C34 1.403(7) . ?
C33 H36 0.9300 . ?
C34 O4 1.298(5) . ?
La1 O4 2.434(3) 1_655 ?
La1 O3 2.443(3) . ?
La1 O2 2.461(3) 3_677 ?
La1 O1 2.512(3) . ?
La1 O13 2.641(3) . ?
La1 O10 2.681(3) . ?
La1 O7 2.709(4) . ?
La1 O5 2.716(4) . ?
La1 O11 2.763(4) . ?
La1 O8 2.796(4) . ?
N1 H6 0.8503 . ?
N2 H13 0.8500 . ?
N3 H24 0.8489 . ?
N4 H31 0.8539 . ?
N5 O6 1.228(5) . ?
N5 O7 1.257(5) . ?
N5 O5 1.261(5) . ?
N6 O9 1.218(5) . ?
N6 O8 1.249(5) . ?
N6 O10 1.257(5) . ?
N7 O12 1.224(5) . ?
N7 O11 1.254(6) . ?
N7 O13 1.264(5) . ?
O2 La1 2.461(3) 3_677 ?
O4 La1 2.434(3) 1_455 ?
O14 C35 1.495(10) . ?
O14 H14A 0.8200 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 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
O1 C1 C2 121.4(5) . . ?
O1 C1 C6 121.3(5) . . ?
C2 C1 C6 117.3(5) . . ?
C3 C2 C1 120.6(6) . . ?
C3 C2 H1 119.7 . . ?
C1 C2 H1 119.7 . . ?
C4 C3 C2 121.7(6) . . ?
C4 C3 H2 119.2 . . ?
C2 C3 H2 119.2 . . ?
C5 C4 C3 119.5(5) . . ?
C5 C4 H3 120.3 . . ?
C3 C4 H3 120.3 . . ?
C4 C5 C6 120.9(6) . . ?
C4 C5 H4 119.6 . . ?
C6 C5 H4 119.6 . . ?
C5 C6 C7 118.5(5) . . ?
C5 C6 C1 119.9(5) . . ?
C7 C6 C1 121.5(5) . . ?
N1 C7 C6 124.3(5) . . ?
N1 C7 H5 117.9 . . ?
C6 C7 H5 117.9 . . ?
N1 C8 C9 110.1(5) . . ?
N1 C8 H7 109.6 . . ?
C9 C8 H7 109.6 . . ?
N1 C8 H8 109.6 . . ?
C9 C8 H8 109.6 . . ?
H7 C8 H8 108.2 . . ?
C8 C9 C10 113.6(5) . . ?
C8 C9 H10 108.8 . . ?
C10 C9 H10 108.8 . . ?
C8 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H10 C9 H9B 107.7 . . ?
N2 C10 C9 110.6(5) . . ?
N2 C10 H11 109.5 . . ?
C9 C10 H11 109.5 . . ?
N2 C10 H12 109.5 . . ?
C9 C10 H12 109.5 . . ?
H11 C10 H12 108.1 . . ?
N2 C11 C12 125.3(5) . . ?
N2 C11 H14 117.4 . . ?
C12 C11 H14 117.4 . . ?
C11 C12 C13 118.5(6) . . ?
C11 C12 C17 121.1(5) . . ?
C13 C12 C17 120.4(6) . . ?
C14 C13 C12 121.3(6) . . ?
C14 C13 H15 119.3 . . ?
C12 C13 H15 119.3 . . ?
C13 C14 C15 118.7(6) . . ?
C13 C14 H16 120.6 . . ?
C15 C14 H16 120.6 . . ?
C16 C15 C14 121.7(7) . . ?
C16 C15 H17 119.2 . . ?
C14 C15 H17 119.2 . . ?
C15 C16 C17 121.7(6) . . ?
C15 C16 H18 119.2 . . ?
C17 C16 H18 119.2 . . ?
O2 C17 C16 122.4(5) . . ?
O2 C17 C12 121.4(5) . . ?
C16 C17 C12 116.2(5) . . ?
O3 C18 C19 121.1(5) . . ?
O3 C18 C23 121.3(5) . . ?
C19 C18 C23 117.6(5) . . ?
C20 C19 C18 120.9(6) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C19 C20 C21 120.7(7) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C22 C21 C20 119.8(7) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 121.4(6) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C22 C23 C18 119.5(6) . . ?
C22 C23 C24 118.6(5) . . ?
C18 C23 C24 121.9(5) . . ?
N3 C24 C23 124.9(5) . . ?
N3 C24 H23 117.5 . . ?
C23 C24 H23 117.5 . . ?
N3 C25 C26 110.5(5) . . ?
N3 C25 H26 109.6 . . ?
C26 C25 H26 109.6 . . ?
N3 C25 H25 109.6 . . ?
C26 C25 H25 109.6 . . ?
H26 C25 H25 108.1 . . ?
C27 C26 C25 111.1(6) . . ?
C27 C26 H27 109.4 . . ?
C25 C26 H27 109.4 . . ?
C27 C26 H28 109.4 . . ?
C25 C26 H28 109.4 . . ?
H27 C26 H28 108.0 . . ?
N4 C27 C26 111.2(6) . . ?
N4 C27 H30 109.4 . . ?
C26 C27 H30 109.4 . . ?
N4 C27 H29 109.4 . . ?
C26 C27 H29 109.4 . . ?
H30 C27 H29 108.0 . . ?
N4 C28 C29 124.7(5) . . ?
N4 C28 H32 117.6 . . ?
C29 C28 H32 117.6 . . ?
C28 C29 C30 118.1(5) . . ?
C28 C29 C34 121.5(5) . . ?
C30 C29 C34 120.4(5) . . ?
C31 C30 C29 121.0(5) . . ?
C31 C30 H33 119.5 . . ?
C29 C30 H33 119.5 . . ?
C30 C31 C32 118.1(5) . . ?
C30 C31 H34 121.0 . . ?
C32 C31 H34 121.0 . . ?
C33 C32 C31 122.7(6) . . ?
C33 C32 H35 118.7 . . ?
C31 C32 H35 118.7 . . ?
C32 C33 C34 121.0(5) . . ?
C32 C33 H36 119.5 . . ?
C34 C33 H36 119.5 . . ?
O4 C34 C33 122.5(4) . . ?
O4 C34 C29 120.7(5) . . ?
C33 C34 C29 116.8(4) . . ?
O4 La1 O3 91.07(11) 1_655 . ?
O4 La1 O2 77.31(12) 1_655 3_677 ?
O3 La1 O2 78.83(12) . 3_677 ?
O4 La1 O1 80.84(11) 1_655 . ?
O3 La1 O1 155.49(12) . . ?
O2 La1 O1 76.83(12) 3_677 . ?
O4 La1 O13 158.18(12) 1_655 . ?
O3 La1 O13 70.64(12) . . ?
O2 La1 O13 87.25(12) 3_677 . ?
O1 La1 O13 110.82(11) . . ?
O4 La1 O10 114.16(11) 1_655 . ?
O3 La1 O10 67.60(12) . . ?
O2 La1 O10 144.22(12) 3_677 . ?
O1 La1 O10 136.75(12) . . ?
O13 La1 O10 70.61(11) . . ?
O4 La1 O7 133.24(11) 1_655 . ?
O3 La1 O7 124.82(11) . . ?
O2 La1 O7 133.01(11) 3_677 . ?
O1 La1 O7 75.48(11) . . ?
O13 La1 O7 68.53(11) . . ?
O10 La1 O7 64.85(11) . . ?
O4 La1 O5 87.77(11) 1_655 . ?
O3 La1 O5 131.06(12) . . ?
O2 La1 O5 147.27(12) 3_677 . ?
O1 La1 O5 72.08(12) . . ?
O13 La1 O5 113.08(12) . . ?
O10 La1 O5 68.51(11) . . ?
O7 La1 O5 46.79(10) . . ?
O4 La1 O11 137.60(12) 1_655 . ?
O3 La1 O11 109.90(11) . . ?
O2 La1 O11 71.59(12) 3_677 . ?
O1 La1 O11 64.70(11) . . ?
O13 La1 O11 46.51(11) . . ?
O10 La1 O11 107.92(11) . . ?
O7 La1 O11 62.43(11) . . ?
O5 La1 O11 103.22(11) . . ?
O4 La1 O8 68.33(11) 1_655 . ?
O3 La1 O8 67.06(11) . . ?
O2 La1 O8 130.03(11) 3_677 . ?
O1 La1 O8 128.95(11) . . ?
O13 La1 O8 112.65(11) . . ?
O10 La1 O8 45.84(10) . . ?
O7 La1 O8 96.81(11) . . ?
O5 La1 O8 67.21(11) . . ?
O11 La1 O8 153.56(11) . . ?
C7 N1 C8 125.2(5) . . ?
C7 N1 H6 120.1 . . ?
C8 N1 H6 114.7 . . ?
C11 N2 C10 124.4(5) . . ?
C11 N2 H13 112.0 . . ?
C10 N2 H13 122.9 . . ?
C24 N3 C25 123.3(5) . . ?
C24 N3 H24 115.8 . . ?
C25 N3 H24 120.9 . . ?
C28 N4 C27 123.4(5) . . ?
C28 N4 H31 110.5 . . ?
C27 N4 H31 125.0 . . ?
O6 N5 O7 121.7(4) . . ?
O6 N5 O5 120.7(4) . . ?
O7 N5 O5 117.6(4) . . ?
O9 N6 O8 121.6(5) . . ?
O9 N6 O10 121.5(5) . . ?
O8 N6 O10 116.8(4) . . ?
O12 N7 O11 122.2(5) . . ?
O12 N7 O13 121.7(5) . . ?
O11 N7 O13 116.1(4) . . ?
C1 O1 La1 144.8(3) . . ?
C17 O2 La1 154.0(3) . 3_677 ?
C18 O3 La1 144.5(3) . . ?
C34 O4 La1 139.3(3) . 1_455 ?
N5 O5 La1 97.2(3) . . ?
N5 O7 La1 97.7(3) . . ?
N6 O8 La1 95.0(3) . . ?
N6 O10 La1 100.4(3) . . ?
N7 O11 La1 93.9(3) . . ?
N7 O13 La1 99.5(3) . . ?
C35 O14 H14A 109.5 . . ?
O14 C35 H35A 109.5 . . ?
O14 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
O14 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 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
O14 H14A O9 0.82 1.99 2.52(4) 121.6 1_655
N1 H6 O1 0.85 2.01 2.647(5) 131.5 .
N1 H6 O7 0.85 2.50 3.095(6) 128.1 .
N2 H13 O2 0.85 1.94 2.647(6) 140.5 .
N2 H13 O1 0.85 2.58 3.206(6) 131.0 3_677
N3 H24 O3 0.85 1.98 2.656(6) 135.6 .
N3 H24 O13 0.85 2.45 3.159(6) 141.8 .
N4 H31 O4 0.85 1.91 2.620(6) 140.1 .
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.068


data_yb
_database_code_depnum_ccdc_archive 'CCDC 905490'
#TrackingRef '7-Yb.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H72 Yb2 N14 O26, 2(C H2 Cl2), 2(C H4 O)'
_chemical_formula_sum            'C72 H84 Cl4 N14 O28 Yb2'
_chemical_formula_weight         2081.41
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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   10.963(2)
_cell_length_b                   10.998(2)
_cell_length_c                   18.653(4)
_cell_angle_alpha                92.00(3)
_cell_angle_beta                 106.70(3)
_cell_angle_gamma                92.49(3)
_cell_volume                     2149.4(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18009
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.52
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1046
_exptl_absorpt_coefficient_mu    2.372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5575
_exptl_absorpt_correction_T_max  0.6523
_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            21274
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.48
_reflns_number_total             9774
_reflns_number_gt                8142
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_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          
;
omit 3 -3 1
omit 2 -4 6
omit 1 -4 2
omit 1 1 3
omit 3 -3 4
omit -2 2 1
dfix 0.90 0.01 n1 h111 n2 h121 n3 h131
dfix 1.72 0.01 c35 cl1 c35 cl2
dfix 1.50 0.01 c36 o14
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^)+(0.0988P)^2^+1.5765P] 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         9774
_refine_ls_number_parameters     542
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0536
_refine_ls_wR_factor_ref         0.1559
_refine_ls_wR_factor_gt          0.1466
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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
C1 C 0.2020(5) 0.6974(5) 0.2184(3) 0.0335(11) Uani 1 1 d . . .
C2 C 0.1912(6) 0.8010(6) 0.1746(4) 0.0459(14) Uani 1 1 d . . .
H2 H 0.2606 0.8293 0.1595 0.055 Uiso 1 1 calc R . .
C3 C 0.0798(7) 0.8602(6) 0.1540(4) 0.0538(16) Uani 1 1 d . . .
H3 H 0.0754 0.9288 0.1258 0.065 Uiso 1 1 calc R . .
C4 C -0.0267(7) 0.8198(7) 0.1746(4) 0.0560(18) Uani 1 1 d . . .
H4 H -0.1017 0.8607 0.1596 0.067 Uiso 1 1 calc R . .
C5 C -0.0212(6) 0.7203(7) 0.2166(4) 0.0481(15) Uani 1 1 d . . .
H5 H -0.0927 0.6931 0.2301 0.058 Uiso 1 1 calc R . .
C6 C 0.0934(5) 0.6579(5) 0.2400(3) 0.0339(11) Uani 1 1 d . . .
C7 C 0.0954(5) 0.5592(5) 0.2864(3) 0.0372(12) Uani 1 1 d . . .
H7 H 0.0202 0.5385 0.2978 0.045 Uiso 1 1 calc R . .
C8 C 0.1946(6) 0.4012(5) 0.3688(3) 0.0378(12) Uani 1 1 d . . .
H8A H 0.2180 0.3248 0.3504 0.045 Uiso 1 1 calc R . .
H8B H 0.1102 0.3887 0.3751 0.045 Uiso 1 1 calc R . .
C9 C 0.2905(6) 0.4405(5) 0.4445(3) 0.0375(12) Uani 1 1 d . . .
H9A H 0.2983 0.3740 0.4781 0.045 Uiso 1 1 calc R . .
H9B H 0.3735 0.4585 0.4374 0.045 Uiso 1 1 calc R . .
C10 C 0.2495(6) 0.5520(6) 0.4797(3) 0.0410(13) Uani 1 1 d . . .
H10A H 0.2343 0.6164 0.4445 0.049 Uiso 1 1 calc R . .
H10B H 0.1705 0.5320 0.4914 0.049 Uiso 1 1 calc R . .
C11 C 0.3922(6) 0.7054(5) 0.5649(3) 0.0364(11) Uani 1 1 d . . .
H11 H 0.3606 0.7635 0.5303 0.044 Uiso 1 1 calc R . .
C12 C 0.4874(6) 0.7452(5) 0.6336(3) 0.0357(11) Uani 1 1 d . . .
C13 C 0.5247(8) 0.8716(5) 0.6426(4) 0.0555(18) Uani 1 1 d . . .
H13 H 0.4892 0.9242 0.6052 0.067 Uiso 1 1 calc R . .
C14 C 0.6141(9) 0.9142(6) 0.7073(5) 0.070(2) Uani 1 1 d . . .
H14 H 0.6386 0.9968 0.7142 0.085 Uiso 1 1 calc R . .
C15 C 0.6676(8) 0.8366(6) 0.7618(4) 0.059(2) Uani 1 1 d . . .
H15 H 0.7288 0.8679 0.8048 0.071 Uiso 1 1 calc R . .
C16 C 0.6338(6) 0.7134(5) 0.7551(3) 0.0405(12) Uani 1 1 d . . .
H16 H 0.6718 0.6628 0.7932 0.049 Uiso 1 1 calc R . .
C17 C 0.5404(5) 0.6646(5) 0.6896(3) 0.0311(10) Uani 1 1 d . . .
C18 C 0.4249(6) 0.4938(7) 0.0909(3) 0.0466(14) Uani 1 1 d . . .
C19 C 0.3416(7) 0.5746(8) 0.0489(4) 0.0604(19) Uani 1 1 d . . .
H19 H 0.3329 0.6498 0.0708 0.072 Uiso 1 1 calc R . .
C20 C 0.2726(8) 0.5458(12) -0.0236(5) 0.087(3) Uani 1 1 d . . .
H20 H 0.2184 0.6013 -0.0509 0.105 Uiso 1 1 calc R . .
C21 C 0.2838(9) 0.4319(14) -0.0570(5) 0.099(4) Uani 1 1 d . . .
H21 H 0.2364 0.4125 -0.1064 0.119 Uiso 1 1 calc R . .
C22 C 0.3598(9) 0.3528(11) -0.0197(5) 0.081(3) Uani 1 1 d . . .
H22 H 0.3663 0.2784 -0.0432 0.097 Uiso 1 1 calc R . .
C23 C 0.4338(6) 0.3786(7) 0.0570(4) 0.0505(16) Uani 1 1 d . . .
C24 C 0.5160(8) 0.2921(8) 0.0948(5) 0.063(2) Uani 1 1 d . . .
H24 H 0.5144 0.2173 0.0695 0.076 Uiso 1 1 calc R . .
C25 C 0.6752(9) 0.2156(7) 0.2039(6) 0.067(2) Uani 1 1 d . . .
H25A H 0.6467 0.1358 0.1795 0.080 Uiso 1 1 calc R . .
H25B H 0.6651 0.2147 0.2539 0.080 Uiso 1 1 calc R . .
C26 C 0.8126(9) 0.2384(9) 0.2101(5) 0.071(2) Uani 1 1 d . . .
H26A H 0.8408 0.3192 0.2330 0.085 Uiso 1 1 calc R . .
H26B H 0.8236 0.2362 0.1603 0.085 Uiso 1 1 calc R . .
C27 C 0.8956(10) 0.1443(9) 0.2568(5) 0.079(3) Uani 1 1 d . . .
H27A H 0.8625 0.0630 0.2367 0.095 Uiso 1 1 calc R . .
H27B H 0.9818 0.1550 0.2530 0.095 Uiso 1 1 calc R . .
C28 C 0.8535(7) 0.0720(7) 0.3659(5) 0.062(2) Uani 1 1 d . . .
H28 H 0.8152 0.0029 0.3366 0.074 Uiso 1 1 calc R . .
C29 C 0.8577(7) 0.0766(7) 0.4430(5) 0.0590(19) Uani 1 1 d . . .
C30 C 0.8003(8) -0.0143(10) 0.4747(7) 0.082(3) Uani 1 1 d . . .
H30 H 0.7584 -0.0817 0.4448 0.098 Uiso 1 1 calc R . .
C31 C 0.8043(11) -0.0065(14) 0.5496(8) 0.103(4) Uani 1 1 d . . .
H31 H 0.7638 -0.0665 0.5699 0.123 Uiso 1 1 calc R . .
C32 C 0.8699(10) 0.0922(12) 0.5933(6) 0.087(3) Uani 1 1 d . . .
H32 H 0.8730 0.0976 0.6436 0.105 Uiso 1 1 calc R . .
C33 C 0.9280(11) 0.1789(10) 0.5670(6) 0.080(3) Uani 1 1 d . . .
H33 H 0.9738 0.2417 0.5996 0.096 Uiso 1 1 calc R . .
C34 C 0.9234(9) 0.1796(8) 0.4926(5) 0.070(2) Uani 1 1 d . . .
C35 C 0.0516(15) 0.3175(7) 0.0322(6) 0.105(4) Uani 1 1 d D . .
H35A H -0.0201 0.3361 -0.0096 0.126 Uiso 1 1 calc R . .
H35B H 0.1276 0.3221 0.0154 0.126 Uiso 1 1 calc R . .
Cl1 Cl 0.0686(3) 0.4257(3) 0.10417(17) 0.0996(9) Uani 1 1 d D . .
Cl2 Cl 0.0279(6) 0.1727(3) 0.0568(3) 0.168(2) Uani 1 1 d D . .
N1 N 0.1926(4) 0.4941(4) 0.3148(3) 0.0353(10) Uani 1 1 d D . .
H111 H 0.249(5) 0.504(7) 0.289(4) 0.053 Uiso 1 1 d D . .
N2 N 0.3487(5) 0.5947(4) 0.5487(2) 0.0350(10) Uani 1 1 d D . .
H121 H 0.399(6) 0.544(5) 0.579(3) 0.052 Uiso 1 1 d D . .
N3 N 0.5937(6) 0.3071(5) 0.1616(4) 0.0555(15) Uani 1 1 d D . .
H131 H 0.586(9) 0.384(3) 0.176(6) 0.083 Uiso 1 1 d D . .
N4 N 0.8986(7) 0.1556(6) 0.3352(4) 0.0681(18) Uani 1 1 d . . .
N5 N 0.4958(6) 0.7874(5) 0.3957(3) 0.0451(12) Uani 1 1 d . . .
N6 N 0.6102(6) 0.8348(5) 0.1866(3) 0.0450(12) Uani 1 1 d . . .
N7 N 0.7864(4) 0.5548(5) 0.3435(3) 0.0384(10) Uani 1 1 d . . .
O1 O 0.3067(4) 0.6400(4) 0.2381(2) 0.0395(9) Uani 1 1 d . . .
O2 O 0.5079(4) 0.5484(3) 0.6809(2) 0.0393(9) Uani 1 1 d . . .
O3 O 0.4957(4) 0.5218(4) 0.1600(2) 0.0435(10) Uani 1 1 d . . .
O4 O 0.9748(9) 0.2692(5) 0.4670(4) 0.096(2) Uani 1 1 d . . .
H4A H 0.9547 0.2617 0.4211 0.144 Uiso 1 1 calc R . .
O5 O 0.4777(4) 0.6738(4) 0.3953(2) 0.0419(9) Uani 1 1 d . . .
O6 O 0.4843(9) 0.8548(5) 0.4464(4) 0.091(2) Uani 1 1 d . . .
O7 O 0.5288(5) 0.8293(4) 0.3419(3) 0.0499(11) Uani 1 1 d . . .
O8 O 0.4930(4) 0.8055(5) 0.1757(3) 0.0524(11) Uani 1 1 d . . .
O9 O 0.6454(6) 0.9124(5) 0.1502(4) 0.0699(16) Uani 1 1 d . . .
O10 O 0.6876(4) 0.7789(5) 0.2353(3) 0.0544(12) Uani 1 1 d . . .
O11 O 0.7273(4) 0.6241(4) 0.3760(2) 0.0396(9) Uani 1 1 d . . .
O12 O 0.8896(4) 0.5163(6) 0.3765(3) 0.0635(14) Uani 1 1 d . . .
O13 O 0.7332(4) 0.5271(4) 0.2749(3) 0.0488(11) Uani 1 1 d . . .
O14 O 0.411(3) 1.012(3) 0.0633(16) 0.382(16) Uiso 1 1 d D . .
H14A H 0.4578 0.9567 0.0801 0.572 Uiso 1 1 d R . .
C36 C 0.3008(18) 0.9524(16) 0.0075(10) 0.143(6) Uiso 1 1 d D . .
H36A H 0.2266 0.9583 0.0247 0.215 Uiso 1 1 calc R . .
H36B H 0.3158 0.8681 0.0002 0.215 Uiso 1 1 calc R . .
H36C H 0.2874 0.9918 -0.0390 0.215 Uiso 1 1 calc R . .
Yb1 Yb 0.52568(2) 0.63605(2) 0.269269(14) 0.03612(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
C1 0.030(2) 0.039(3) 0.031(2) 0.000(2) 0.007(2) 0.004(2)
C2 0.039(3) 0.043(3) 0.056(4) 0.016(3) 0.012(3) 0.005(3)
C3 0.055(4) 0.045(3) 0.059(4) 0.013(3) 0.010(3) 0.011(3)
C4 0.043(3) 0.059(4) 0.062(4) 0.000(3) 0.005(3) 0.023(3)
C5 0.029(3) 0.067(4) 0.051(4) 0.003(3) 0.013(2) 0.015(3)
C6 0.025(2) 0.045(3) 0.029(2) -0.004(2) 0.0052(19) 0.001(2)
C7 0.030(2) 0.050(3) 0.033(3) -0.004(2) 0.012(2) -0.008(2)
C8 0.042(3) 0.038(3) 0.034(3) 0.006(2) 0.014(2) -0.005(2)
C9 0.046(3) 0.038(3) 0.030(3) 0.010(2) 0.011(2) 0.008(2)
C10 0.039(3) 0.055(3) 0.029(3) 0.002(2) 0.008(2) 0.005(3)
C11 0.043(3) 0.037(3) 0.034(3) 0.013(2) 0.015(2) 0.012(2)
C12 0.045(3) 0.026(2) 0.035(3) 0.002(2) 0.010(2) 0.007(2)
C13 0.074(5) 0.026(3) 0.059(4) 0.011(3) 0.008(4) 0.001(3)
C14 0.086(6) 0.028(3) 0.081(6) -0.004(3) 0.002(5) -0.013(3)
C15 0.069(4) 0.034(3) 0.058(4) -0.007(3) -0.004(3) -0.010(3)
C16 0.049(3) 0.035(3) 0.037(3) 0.002(2) 0.011(2) 0.008(2)
C17 0.036(2) 0.030(2) 0.030(2) 0.005(2) 0.014(2) 0.008(2)
C18 0.039(3) 0.069(4) 0.032(3) 0.004(3) 0.013(2) -0.006(3)
C19 0.046(3) 0.088(5) 0.043(4) 0.016(4) 0.005(3) -0.003(4)
C20 0.050(4) 0.152(10) 0.047(5) 0.035(6) -0.005(4) -0.018(6)
C21 0.064(5) 0.188(13) 0.031(4) -0.002(6) 0.000(4) -0.050(7)
C22 0.065(5) 0.130(8) 0.043(4) -0.036(5) 0.019(4) -0.036(6)
C23 0.041(3) 0.073(4) 0.037(3) -0.013(3) 0.014(3) -0.011(3)
C24 0.066(5) 0.064(4) 0.067(5) -0.025(4) 0.035(4) -0.015(4)
C25 0.076(5) 0.048(4) 0.087(6) 0.011(4) 0.037(5) 0.019(4)
C26 0.077(5) 0.080(5) 0.063(5) 0.006(4) 0.028(4) 0.026(5)
C27 0.088(6) 0.081(6) 0.074(6) 0.008(5) 0.028(5) 0.032(5)
C28 0.050(4) 0.056(4) 0.068(5) -0.009(4) -0.001(3) 0.018(3)
C29 0.043(3) 0.057(4) 0.075(5) 0.005(4) 0.011(3) 0.016(3)
C30 0.053(4) 0.079(6) 0.104(8) -0.002(6) 0.009(5) 0.002(4)
C31 0.078(7) 0.136(11) 0.108(9) 0.051(8) 0.041(7) 0.020(7)
C32 0.074(6) 0.115(9) 0.072(6) 0.007(6) 0.016(5) 0.040(6)
C33 0.092(7) 0.072(5) 0.071(6) 0.002(5) 0.011(5) 0.035(5)
C34 0.070(5) 0.058(4) 0.073(5) -0.005(4) 0.004(4) 0.026(4)
C35 0.161(12) 0.078(6) 0.104(9) 0.010(6) 0.080(9) 0.020(7)
Cl1 0.0832(16) 0.112(2) 0.0879(18) -0.0176(16) 0.0032(14) 0.0018(15)
Cl2 0.254(6) 0.087(2) 0.123(3) 0.022(2) -0.009(3) 0.007(3)
N1 0.033(2) 0.044(2) 0.029(2) 0.0020(19) 0.0107(18) -0.005(2)
N2 0.041(2) 0.040(2) 0.024(2) 0.0078(18) 0.0095(18) 0.005(2)
N3 0.062(4) 0.045(3) 0.066(4) -0.006(3) 0.030(3) 0.011(3)
N4 0.076(4) 0.060(4) 0.065(4) 0.001(3) 0.011(3) 0.019(3)
N5 0.059(3) 0.035(2) 0.048(3) 0.001(2) 0.027(3) 0.005(2)
N6 0.057(3) 0.036(2) 0.050(3) 0.008(2) 0.028(3) -0.001(2)
N7 0.031(2) 0.045(3) 0.043(3) 0.015(2) 0.014(2) 0.006(2)
O1 0.0287(17) 0.047(2) 0.044(2) 0.0139(18) 0.0121(16) 0.0054(17)
O2 0.053(2) 0.0268(17) 0.033(2) 0.0052(15) 0.0045(17) -0.0013(17)
O3 0.050(2) 0.050(2) 0.0284(19) 0.0009(17) 0.0081(17) 0.008(2)
O4 0.144(7) 0.047(3) 0.082(5) -0.003(3) 0.012(5) -0.006(4)
O5 0.053(2) 0.0328(19) 0.044(2) 0.0051(17) 0.0213(19) -0.0018(18)
O6 0.164(7) 0.051(3) 0.088(4) -0.016(3) 0.088(5) -0.004(4)
O7 0.079(3) 0.0282(18) 0.054(3) 0.0043(18) 0.037(2) 0.003(2)
O8 0.044(2) 0.060(3) 0.054(3) 0.027(2) 0.013(2) 0.002(2)
O9 0.084(4) 0.053(3) 0.084(4) 0.032(3) 0.040(3) -0.003(3)
O10 0.038(2) 0.058(3) 0.074(3) 0.026(2) 0.023(2) 0.008(2)
O11 0.0334(18) 0.047(2) 0.039(2) 0.0029(17) 0.0109(16) 0.0038(17)
O12 0.035(2) 0.098(4) 0.059(3) 0.024(3) 0.012(2) 0.022(2)
O13 0.051(2) 0.051(2) 0.045(2) -0.0003(19) 0.013(2) 0.018(2)
Yb1 0.03674(14) 0.03566(14) 0.03781(15) 0.00742(9) 0.01268(10) 0.00462(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
C1 O1 1.299(7) . ?
C1 C2 1.414(8) . ?
C1 C6 1.418(8) . ?
C2 C3 1.371(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.390(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.362(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.422(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.409(8) . ?
C7 N1 1.302(8) . ?
C7 H7 0.9300 . ?
C8 N1 1.457(7) . ?
C8 C9 1.533(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.516(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.472(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.282(8) . ?
C11 C12 1.441(8) . ?
C11 H11 0.9300 . ?
C12 C17 1.405(7) . ?
C12 C13 1.422(8) . ?
C13 C14 1.370(11) . ?
C13 H13 0.9300 . ?
C14 C15 1.366(11) . ?
C14 H14 0.9300 . ?
C15 C16 1.381(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.420(8) . ?
C16 H16 0.9300 . ?
C17 O2 1.303(6) . ?
C18 O3 1.318(7) . ?
C18 C19 1.395(11) . ?
C18 C23 1.416(10) . ?
C19 C20 1.365(11) . ?
C19 H19 0.9300 . ?
C20 C21 1.405(18) . ?
C20 H20 0.9300 . ?
C21 C22 1.307(17) . ?
C21 H21 0.9300 . ?
C22 C23 1.439(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.404(12) . ?
C24 N3 1.291(11) . ?
C24 H24 0.9300 . ?
C25 N3 1.470(10) . ?
C25 C26 1.487(13) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.533(12) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 N4 1.455(12) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 N4 1.256(12) . ?
C28 C29 1.423(12) . ?
C28 H28 0.9300 . ?
C29 C30 1.395(14) . ?
C29 C34 1.460(11) . ?
C30 C31 1.385(17) . ?
C30 H30 0.9300 . ?
C31 C32 1.376(17) . ?
C31 H31 0.9300 . ?
C32 C33 1.310(16) . ?
C32 H32 0.9300 . ?
C33 C34 1.374(14) . ?
C33 H33 0.9300 . ?
C34 O4 1.288(12) . ?
C35 Cl2 1.702(8) . ?
C35 Cl1 1.726(8) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
N1 H111 0.894(10) . ?
N2 H121 0.893(10) . ?
N3 H131 0.895(10) . ?
N5 O6 1.219(7) . ?
N5 O7 1.256(7) . ?
N5 O5 1.256(6) . ?
N5 Yb1 2.943(5) . ?
N6 O9 1.225(7) . ?
N6 O10 1.251(7) . ?
N6 O8 1.267(7) . ?
N6 Yb1 2.982(5) . ?
N7 O12 1.224(7) . ?
N7 O13 1.265(7) . ?
N7 O11 1.266(6) . ?
N7 Yb1 2.987(5) . ?
O1 Yb1 2.305(4) . ?
O2 Yb1 2.319(4) 2_666 ?
O3 Yb1 2.289(4) . ?
O4 H4A 0.8200 . ?
O5 Yb1 2.577(4) . ?
O7 Yb1 2.474(4) . ?
O8 Yb1 2.564(5) . ?
O10 Yb1 2.548(5) . ?
O11 Yb1 2.526(4) . ?
O13 Yb1 2.594(4) . ?
O14 C36 1.459(10) . ?
O14 H14A 0.8200 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
Yb1 O2 2.319(4) 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
O1 C1 C2 121.7(5) . . ?
O1 C1 C6 120.9(5) . . ?
C2 C1 C6 117.4(5) . . ?
C3 C2 C1 121.0(6) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 121.3(7) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 120.0(6) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.2(6) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C1 122.1(5) . . ?
C7 C6 C5 117.7(5) . . ?
C1 C6 C5 120.2(6) . . ?
N1 C7 C6 126.1(5) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
N1 C8 C9 110.2(4) . . ?
N1 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 . . ?
N1 C8 H8B 109.6 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C10 C9 C8 111.5(5) . . ?
C10 C9 H9A 109.3 . . ?
C8 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
C8 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 C9 110.4(5) . . ?
N2 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
N2 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
N2 C11 C12 123.9(5) . . ?
N2 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
C17 C12 C13 121.2(5) . . ?
C17 C12 C11 122.3(5) . . ?
C13 C12 C11 116.5(5) . . ?
C14 C13 C12 118.7(6) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C15 C14 C13 120.7(6) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 122.3(6) . . ?
C14 C15 H15 118.9 . . ?
C16 C15 H15 118.9 . . ?
C15 C16 C17 119.4(6) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
O2 C17 C12 121.3(5) . . ?
O2 C17 C16 121.0(5) . . ?
C12 C17 C16 117.7(5) . . ?
O3 C18 C19 122.3(7) . . ?
O3 C18 C23 119.5(6) . . ?
C19 C18 C23 118.2(6) . . ?
C20 C19 C18 121.4(9) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C19 C20 C21 119.9(10) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 120.9(8) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 121.4(10) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C24 C23 C18 122.1(6) . . ?
C24 C23 C22 119.6(8) . . ?
C18 C23 C22 118.2(8) . . ?
N3 C24 C23 125.8(7) . . ?
N3 C24 H24 117.1 . . ?
C23 C24 H24 117.1 . . ?
N3 C25 C26 113.4(7) . . ?
N3 C25 H25A 108.9 . . ?
C26 C25 H25A 108.9 . . ?
N3 C25 H25B 108.9 . . ?
C26 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
C25 C26 C27 112.1(9) . . ?
C25 C26 H26A 109.2 . . ?
C27 C26 H26A 109.2 . . ?
C25 C26 H26B 109.2 . . ?
C27 C26 H26B 109.2 . . ?
H26A C26 H26B 107.9 . . ?
N4 C27 C26 111.9(7) . . ?
N4 C27 H27A 109.2 . . ?
C26 C27 H27A 109.2 . . ?
N4 C27 H27B 109.2 . . ?
C26 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
N4 C28 C29 123.9(8) . . ?
N4 C28 H28 118.0 . . ?
C29 C28 H28 118.0 . . ?
C30 C29 C28 122.8(8) . . ?
C30 C29 C34 116.9(9) . . ?
C28 C29 C34 120.3(8) . . ?
C31 C30 C29 121.5(10) . . ?
C31 C30 H30 119.2 . . ?
C29 C30 H30 119.2 . . ?
C32 C31 C30 118.3(11) . . ?
C32 C31 H31 120.9 . . ?
C30 C31 H31 120.9 . . ?
C33 C32 C31 122.9(11) . . ?
C33 C32 H32 118.6 . . ?
C31 C32 H32 118.6 . . ?
C32 C33 C34 121.9(11) . . ?
C32 C33 H33 119.1 . . ?
C34 C33 H33 119.1 . . ?
O4 C34 C33 121.0(9) . . ?
O4 C34 C29 120.6(9) . . ?
C33 C34 C29 118.5(10) . . ?
Cl2 C35 Cl1 113.4(6) . . ?
Cl2 C35 H35A 108.9 . . ?
Cl1 C35 H35A 108.9 . . ?
Cl2 C35 H35B 108.9 . . ?
Cl1 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
C7 N1 C8 124.3(5) . . ?
C7 N1 H111 109(5) . . ?
C8 N1 H111 126(5) . . ?
C11 N2 C10 125.0(5) . . ?
C11 N2 H121 111(5) . . ?
C10 N2 H121 122(5) . . ?
C24 N3 C25 126.7(7) . . ?
C24 N3 H131 105(7) . . ?
C25 N3 H131 129(7) . . ?
C28 N4 C27 121.6(8) . . ?
O6 N5 O7 120.8(5) . . ?
O6 N5 O5 122.1(6) . . ?
O7 N5 O5 117.0(5) . . ?
O6 N5 Yb1 177.0(5) . . ?
O7 N5 Yb1 56.2(3) . . ?
O5 N5 Yb1 60.9(3) . . ?
O9 N6 O10 122.0(6) . . ?
O9 N6 O8 121.4(6) . . ?
O10 N6 O8 116.5(5) . . ?
O9 N6 Yb1 177.0(5) . . ?
O10 N6 Yb1 57.9(3) . . ?
O8 N6 Yb1 58.7(3) . . ?
O12 N7 O13 121.4(5) . . ?
O12 N7 O11 122.1(5) . . ?
O13 N7 O11 116.5(5) . . ?
O12 N7 Yb1 175.8(4) . . ?
O13 N7 Yb1 59.9(3) . . ?
O11 N7 Yb1 56.8(3) . . ?
C1 O1 Yb1 151.6(4) . . ?
C17 O2 Yb1 150.5(4) . 2_666 ?
C18 O3 Yb1 148.4(4) . . ?
C34 O4 H4A 109.5 . . ?
N5 O5 Yb1 93.9(3) . . ?
N5 O7 Yb1 98.9(3) . . ?
N6 O8 Yb1 96.3(3) . . ?
N6 O10 Yb1 97.5(3) . . ?
N7 O11 Yb1 98.4(3) . . ?
N7 O13 Yb1 95.1(3) . . ?
C36 O14 H14A 105.6 . . ?
O14 C36 H36A 109.5 . . ?
O14 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
O14 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O3 Yb1 O1 86.70(16) . . ?
O3 Yb1 O2 84.64(15) . 2_666 ?
O1 Yb1 O2 83.75(15) . 2_666 ?
O3 Yb1 O7 153.14(16) . . ?
O1 Yb1 O7 85.71(17) . . ?
O2 Yb1 O7 119.99(15) 2_666 . ?
O3 Yb1 O11 120.56(15) . . ?
O1 Yb1 O11 144.66(15) . . ?
O2 Yb1 O11 77.57(14) 2_666 . ?
O7 Yb1 O11 78.28(16) . . ?
O3 Yb1 O10 90.81(18) . . ?
O1 Yb1 O10 129.97(15) . . ?
O2 Yb1 O10 145.73(16) 2_666 . ?
O7 Yb1 O10 74.72(17) . . ?
O11 Yb1 O10 75.70(15) . . ?
O3 Yb1 O8 79.96(17) . . ?
O1 Yb1 O8 80.99(15) . . ?
O2 Yb1 O8 158.85(15) 2_666 . ?
O7 Yb1 O8 73.42(17) . . ?
O11 Yb1 O8 122.88(14) . . ?
O10 Yb1 O8 49.53(15) . . ?
O3 Yb1 O5 150.16(15) . . ?
O1 Yb1 O5 75.38(15) . . ?
O2 Yb1 O5 70.05(14) 2_666 . ?
O7 Yb1 O5 50.14(14) . . ?
O11 Yb1 O5 70.14(14) . . ?
O10 Yb1 O5 119.00(16) . . ?
O8 Yb1 O5 119.42(16) . . ?
O3 Yb1 O13 71.22(15) . . ?
O1 Yb1 O13 151.94(15) . . ?
O2 Yb1 O13 77.30(16) 2_666 . ?
O7 Yb1 O13 121.69(16) . . ?
O11 Yb1 O13 49.70(14) . . ?
O10 Yb1 O13 69.13(16) . . ?
O8 Yb1 O13 110.79(16) . . ?
O5 Yb1 O13 116.08(15) . . ?
O3 Yb1 N5 165.85(16) . . ?
O1 Yb1 N5 79.23(16) . . ?
O2 Yb1 N5 95.19(15) 2_666 . ?
O7 Yb1 N5 24.94(15) . . ?
O11 Yb1 N5 72.98(15) . . ?
O10 Yb1 N5 97.08(17) . . ?
O8 Yb1 N5 96.25(17) . . ?
O5 Yb1 N5 25.21(14) . . ?
O13 Yb1 N5 122.60(16) . . ?
O3 Yb1 N6 84.46(16) . . ?
O1 Yb1 N6 105.79(16) . . ?
O2 Yb1 N6 165.04(16) 2_666 . ?
O7 Yb1 N6 72.95(15) . . ?
O11 Yb1 N6 99.34(15) . . ?
O10 Yb1 N6 24.57(15) . . ?
O8 Yb1 N6 24.97(15) . . ?
O5 Yb1 N6 123.05(14) . . ?
O13 Yb1 N6 89.50(16) . . ?
N5 Yb1 N6 97.89(15) . . ?
O3 Yb1 N7 95.84(15) . . ?
O1 Yb1 N7 158.20(14) . . ?
O2 Yb1 N7 74.97(15) 2_666 . ?
O7 Yb1 N7 100.70(17) . . ?
O11 Yb1 N7 24.80(14) . . ?
O10 Yb1 N7 71.74(14) . . ?
O8 Yb1 N7 120.79(14) . . ?
O5 Yb1 N7 92.65(15) . . ?
O13 Yb1 N7 24.96(14) . . ?
N5 Yb1 N7 97.77(16) . . ?
N6 Yb1 N7 96.00(15) . . ?
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
O4 H4A N4 0.82 1.88 2.609(10) 147.1 .
N3 H131 O13 0.895(10) 2.52(7) 3.182(8) 131(8) .
N3 H131 O3 0.895(10) 1.83(5) 2.634(7) 149(9) .
N2 H121 O11 0.893(10) 2.57(7) 3.032(7) 113(6) 2_666
N2 H121 O2 0.893(10) 1.94(5) 2.661(6) 137(6) .
N1 H111 O2 0.894(10) 2.66(6) 3.316(7) 131(6) 2_666
N1 H111 O1 0.894(10) 1.97(5) 2.683(6) 136(7) .
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.681
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.171


data_zxy-2
_database_code_depnum_ccdc_archive 'CCDC 905491'
#TrackingRef '2-Pr.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C34 H36 N7 O13 Pr), (C H4 O)'
_chemical_formula_sum            'C69 H76 N14 O27 Pr2'
_chemical_formula_weight         1815.26
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'
Pr Pr -0.2180 2.8214 '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                   10.0985(10)
_cell_length_b                   37.415(4)
_cell_length_c                   10.9657(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.4810(10)
_cell_angle_gamma                90.00
_cell_volume                     3800.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27355
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.42
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1844
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7619
_exptl_absorpt_correction_T_max  0.8079
_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            20575
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.45
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6647
_reflns_number_gt                6357
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation, 1998)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        
'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP (Sheldrick, 1993)'
_computing_publication_material  SHELXL-97
_refine_special_details          
;
OMIT -3.00 50.00
dfix 0.85 0.01 h6 n1 h13 n2 h24 n3 h31 n4
dfix 1.50 0.01 o14 c35
isor 0.01 c21 c22 o14
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^)+(0.0159P)^2^+11.8761P] 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         6647
_refine_ls_number_parameters     514
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1055
_refine_ls_wR_factor_gt          0.1044
_refine_ls_goodness_of_fit_ref   1.256
_refine_ls_restrained_S_all      1.258
_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
C1 C 0.6427(6) 0.96127(14) 0.7365(5) 0.0382(12) Uani 1 1 d . . .
C2 C 0.7661(7) 0.94935(16) 0.7201(6) 0.0497(15) Uani 1 1 d . . .
H1 H 0.8046 0.9270 0.7523 0.060 Uiso 1 1 calc R . .
C3 C 0.8313(7) 0.9706(2) 0.6563(6) 0.0604(19) Uani 1 1 d . . .
H2 H 0.9105 0.9617 0.6429 0.073 Uiso 1 1 calc R . .
C4 C 0.7819(8) 1.0045(2) 0.6121(6) 0.0623(19) Uani 1 1 d . . .
H3 H 0.8281 1.0183 0.5705 0.075 Uiso 1 1 calc R . .
C5 C 0.6651(8) 1.01740(17) 0.6298(6) 0.0564(17) Uani 1 1 d . . .
H4 H 0.6318 1.0403 0.6002 0.068 Uiso 1 1 calc R . .
C6 C 0.5934(6) 0.99668(15) 0.6923(5) 0.0436(13) Uani 1 1 d . . .
C7 C 0.4706(7) 1.01138(16) 0.7067(6) 0.0484(15) Uani 1 1 d . . .
H5 H 0.4435 1.0346 0.6764 0.058 Uiso 1 1 calc R . .
C8 C 0.2681(7) 1.00947(17) 0.7748(6) 0.0535(16) Uani 1 1 d . . .
H7 H 0.1810 0.9986 0.7104 0.064 Uiso 1 1 calc R . .
H8 H 0.2627 1.0350 0.7586 0.064 Uiso 1 1 calc R . .
C9 C 0.2778(7) 1.00233(16) 0.9134(6) 0.0518(15) Uani 1 1 d . . .
H10 H 0.3646 1.0135 0.9767 0.062 Uiso 1 1 calc R . .
H9B H 0.2867 0.9768 0.9295 0.062 Uiso 1 1 calc R . .
C10 C 0.1489(7) 1.01595(17) 0.9376(7) 0.0556(17) Uani 1 1 d . . .
H11 H 0.0610 1.0060 0.8715 0.067 Uiso 1 1 calc R . .
H12 H 0.1566 1.0082 1.0246 0.067 Uiso 1 1 calc R . .
C11 C 0.0379(6) 1.07278(19) 0.8439(7) 0.0588(18) Uani 1 1 d . . .
H14 H -0.0423 1.0600 0.7879 0.071 Uiso 1 1 calc R . .
C12 C 0.0354(6) 1.11013(18) 0.8267(6) 0.0497(16) Uani 1 1 d . . .
C13 C -0.0860(7) 1.1258(2) 0.7256(7) 0.067(2) Uani 1 1 d . . .
H15 H -0.1644 1.1115 0.6763 0.080 Uiso 1 1 calc R . .
C14 C -0.0907(8) 1.1610(3) 0.6988(7) 0.076(2) Uani 1 1 d . . .
H16 H -0.1713 1.1710 0.6318 0.091 Uiso 1 1 calc R . .
C15 C 0.0270(9) 1.1822(2) 0.7728(7) 0.074(2) Uani 1 1 d . . .
H17 H 0.0248 1.2065 0.7539 0.089 Uiso 1 1 calc R . .
C16 C 0.1464(7) 1.16813(19) 0.8730(6) 0.0593(17) Uani 1 1 d . . .
H18 H 0.2236 1.1831 0.9199 0.071 Uiso 1 1 calc R . .
C17 C 0.1548(6) 1.13167(16) 0.9066(5) 0.0431(13) Uani 1 1 d . . .
C18 C 0.5446(6) 0.78561(14) 0.8817(6) 0.0411(13) Uani 1 1 d . . .
C19 C 0.6339(7) 0.77724(17) 0.8145(7) 0.0591(17) Uani 1 1 d . . .
H19 H 0.6726 0.7956 0.7818 0.071 Uiso 1 1 calc R . .
C20 C 0.6643(10) 0.7424(2) 0.7968(9) 0.085(3) Uani 1 1 d . . .
H20 H 0.7251 0.7374 0.7538 0.102 Uiso 1 1 calc R . .
C21 C 0.6055(10) 0.7144(2) 0.8423(9) 0.086(2) Uani 1 1 d U . .
H21 H 0.6256 0.6908 0.8284 0.103 Uiso 1 1 calc R . .
C22 C 0.5197(9) 0.72151(18) 0.9062(8) 0.074(2) Uani 1 1 d U . .
H22 H 0.4832 0.7027 0.9388 0.089 Uiso 1 1 calc R . .
C23 C 0.4835(7) 0.75692(15) 0.9251(6) 0.0489(15) Uani 1 1 d . . .
C24 C 0.3840(7) 0.76258(18) 0.9845(7) 0.0579(17) Uani 1 1 d . . .
H23 H 0.3479 0.7425 1.0109 0.070 Uiso 1 1 calc R . .
C25 C 0.2275(8) 0.7980(2) 1.0579(8) 0.075(2) Uani 1 1 d . . .
H26 H 0.2562 0.8169 1.1240 0.089 Uiso 1 1 calc R . .
H25 H 0.2178 0.7761 1.1010 0.089 Uiso 1 1 calc R . .
C26 C 0.0791(8) 0.8077(2) 0.9440(9) 0.081(2) Uani 1 1 d . . .
H27 H 0.0674 0.7942 0.8648 0.097 Uiso 1 1 calc R . .
H28 H 0.0017 0.8010 0.9705 0.097 Uiso 1 1 calc R . .
C27 C 0.0688(7) 0.8460(2) 0.9133(7) 0.0635(19) Uani 1 1 d . . .
H30 H 0.1489 0.8530 0.8908 0.076 Uiso 1 1 calc R . .
H29 H 0.0760 0.8594 0.9913 0.076 Uiso 1 1 calc R . .
C28 C -0.0784(7) 0.86124(19) 0.6819(7) 0.0575(17) Uani 1 1 d . . .
H32 H 0.0062 0.8608 0.6674 0.069 Uiso 1 1 calc R . .
C29 C -0.2078(6) 0.86865(16) 0.5725(6) 0.0429(13) Uani 1 1 d . . .
C30 C -0.2014(7) 0.87556(17) 0.4479(6) 0.0523(16) Uani 1 1 d . . .
H33 H -0.1127 0.8749 0.4408 0.063 Uiso 1 1 calc R . .
C31 C -0.3225(8) 0.88313(18) 0.3388(7) 0.0579(17) Uani 1 1 d . . .
H34 H -0.3178 0.8878 0.2573 0.070 Uiso 1 1 calc R . .
C32 C -0.4541(8) 0.88368(19) 0.3522(6) 0.0599(18) Uani 1 1 d . . .
H35 H -0.5378 0.8886 0.2777 0.072 Uiso 1 1 calc R . .
C33 C -0.4649(7) 0.87732(16) 0.4705(6) 0.0470(14) Uani 1 1 d . . .
H36 H -0.5552 0.8777 0.4745 0.056 Uiso 1 1 calc R . .
C34 C -0.3422(6) 0.87025(14) 0.5860(5) 0.0362(12) Uani 1 1 d . . .
Pr1 Pr 0.49385(3) 0.879384(7) 0.81366(3) 0.03234(10) Uani 1 1 d . . .
N1 N 0.3944(5) 0.99479(12) 0.7586(5) 0.0457(12) Uani 1 1 d D . .
H6 H 0.4168 0.9736 0.7879 0.069 Uiso 1 1 d RD . .
N2 N 0.1419(5) 1.05472(14) 0.9305(5) 0.0522(13) Uani 1 1 d D . .
H13 H 0.2127 1.0680 0.9758 0.078 Uiso 1 1 d RD . .
N3 N 0.3396(5) 0.79330(15) 1.0050(5) 0.0534(13) Uani 1 1 d D . .
H24 H 0.3777 0.8113 0.9843 0.080 Uiso 1 1 d RD . .
N4 N -0.0680(5) 0.85490(16) 0.8019(5) 0.0576(14) Uani 1 1 d D . .
H31 H -0.1517 0.8525 0.8028 0.086 Uiso 1 1 d RD . .
N5 N 0.2188(5) 0.92096(11) 0.6253(5) 0.0397(11) Uani 1 1 d . . .
N6 N 0.2659(5) 0.82197(12) 0.6426(5) 0.0426(11) Uani 1 1 d . . .
N7 N 0.3985(6) 0.90920(14) 1.0309(4) 0.0464(12) Uani 1 1 d . . .
O1 O 0.5787(4) 0.94149(9) 0.7945(4) 0.0437(9) Uani 1 1 d . . .
O2 O 0.2646(4) 1.11815(10) 1.0044(4) 0.0463(10) Uani 1 1 d . . .
O3 O 0.5177(4) 0.81855(9) 0.9012(4) 0.0429(9) Uani 1 1 d . . .
O4 O -0.3479(4) 0.86552(10) 0.7009(4) 0.0402(9) Uani 1 1 d . . .
O5 O 0.3060(4) 0.90791(11) 0.5812(4) 0.0491(10) Uani 1 1 d . . .
O6 O 0.1037(4) 0.93372(12) 0.5495(5) 0.0608(12) Uani 1 1 d . . .
O7 O 0.2548(4) 0.92060(10) 0.7489(4) 0.0454(9) Uani 1 1 d . . .
O8 O 0.3722(4) 0.82805(11) 0.6148(4) 0.0511(10) Uani 1 1 d . . .
O9 O 0.1884(6) 0.79612(13) 0.5980(5) 0.0793(16) Uani 1 1 d . . .
O10 O 0.2427(4) 0.84377(10) 0.7191(4) 0.0447(9) Uani 1 1 d . . .
O11 O 0.4859(5) 0.92740(11) 1.0022(4) 0.0528(10) Uani 1 1 d . . .
O12 O 0.3257(6) 0.92214(13) 1.0862(5) 0.0726(15) Uani 1 1 d . . .
O13 O 0.3885(5) 0.87663(11) 0.9986(4) 0.0490(10) Uani 1 1 d . . .
O14 O 1.029(3) 0.7646(8) 0.692(3) 0.299(16) Uani 0.50 1 d PDU . .
H40 H 1.0867 0.7801 0.6920 0.449 Uiso 0.50 1 d PRD . .
C35 C 0.889(3) 0.7713(8) 0.577(4) 0.24(2) Uani 0.50 1 d PD . .
H37 H 0.8258 0.7840 0.6089 0.357 Uiso 0.50 1 d PR . .
H38 H 0.8456 0.7488 0.5404 0.357 Uiso 0.50 1 d PR . .
H39 H 0.9032 0.7852 0.5102 0.357 Uiso 0.50 1 d PR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.039(3) 0.041(3) 0.036(3) -0.009(2) 0.015(2) -0.013(2)
C2 0.051(4) 0.045(3) 0.063(4) -0.009(3) 0.034(3) -0.012(3)
C3 0.054(4) 0.077(5) 0.059(4) -0.027(4) 0.032(3) -0.029(4)
C4 0.067(5) 0.071(5) 0.053(4) -0.003(3) 0.029(4) -0.036(4)
C5 0.063(4) 0.048(4) 0.047(4) 0.006(3) 0.009(3) -0.019(3)
C6 0.048(4) 0.038(3) 0.041(3) -0.001(2) 0.014(3) -0.010(3)
C7 0.051(4) 0.036(3) 0.047(3) -0.003(3) 0.007(3) -0.006(3)
C8 0.044(4) 0.050(4) 0.060(4) -0.007(3) 0.013(3) 0.009(3)
C9 0.047(4) 0.043(3) 0.061(4) -0.013(3) 0.018(3) -0.001(3)
C10 0.046(4) 0.056(4) 0.064(4) -0.025(3) 0.021(3) -0.017(3)
C11 0.029(3) 0.076(5) 0.063(4) -0.036(4) 0.009(3) -0.004(3)
C12 0.031(3) 0.075(4) 0.042(3) -0.018(3) 0.012(3) 0.007(3)
C13 0.038(4) 0.096(6) 0.050(4) -0.016(4) 0.000(3) 0.014(4)
C14 0.050(5) 0.119(7) 0.044(4) 0.010(4) 0.003(3) 0.029(5)
C15 0.067(5) 0.089(6) 0.063(5) 0.029(4) 0.022(4) 0.027(4)
C16 0.042(4) 0.074(5) 0.053(4) 0.009(3) 0.009(3) 0.002(3)
C17 0.031(3) 0.060(4) 0.039(3) -0.001(3) 0.015(3) 0.010(3)
C18 0.034(3) 0.037(3) 0.047(3) 0.007(2) 0.010(3) 0.004(2)
C19 0.058(4) 0.047(4) 0.081(5) 0.008(3) 0.036(4) 0.008(3)
C20 0.095(6) 0.066(5) 0.120(7) 0.000(5) 0.071(6) 0.020(5)
C21 0.102(6) 0.052(4) 0.113(6) 0.001(4) 0.053(5) 0.015(4)
C22 0.085(5) 0.042(4) 0.099(5) 0.011(4) 0.039(4) -0.001(3)
C23 0.048(4) 0.037(3) 0.058(4) 0.011(3) 0.017(3) 0.004(3)
C24 0.055(4) 0.050(4) 0.069(4) 0.020(3) 0.025(4) -0.005(3)
C25 0.057(5) 0.100(6) 0.087(5) 0.038(5) 0.051(4) 0.022(4)
C26 0.052(5) 0.099(6) 0.109(7) 0.035(5) 0.050(5) 0.018(4)
C27 0.043(4) 0.085(5) 0.067(4) -0.009(4) 0.027(3) 0.002(4)
C28 0.043(4) 0.076(5) 0.066(4) -0.005(4) 0.035(3) 0.001(3)
C29 0.031(3) 0.053(3) 0.051(3) -0.003(3) 0.023(3) -0.002(3)
C30 0.052(4) 0.059(4) 0.062(4) -0.005(3) 0.040(4) -0.003(3)
C31 0.072(5) 0.064(4) 0.052(4) 0.007(3) 0.040(4) 0.006(4)
C32 0.063(4) 0.075(5) 0.048(4) 0.011(3) 0.028(3) 0.016(4)
C33 0.044(3) 0.056(4) 0.051(3) 0.002(3) 0.030(3) 0.006(3)
C34 0.033(3) 0.035(3) 0.045(3) -0.002(2) 0.021(3) -0.001(2)
Pr1 0.02877(16) 0.03444(17) 0.03664(17) 0.00048(12) 0.01600(13) 0.00014(12)
N1 0.046(3) 0.035(3) 0.052(3) -0.005(2) 0.016(2) 0.003(2)
N2 0.033(3) 0.055(3) 0.063(3) -0.026(3) 0.013(3) -0.004(2)
N3 0.042(3) 0.060(3) 0.062(3) 0.022(3) 0.024(3) 0.007(3)
N4 0.031(3) 0.087(4) 0.059(3) 0.000(3) 0.022(3) 0.005(3)
N5 0.036(3) 0.031(2) 0.051(3) 0.003(2) 0.017(2) -0.001(2)
N6 0.039(3) 0.039(3) 0.046(3) -0.003(2) 0.013(2) 0.002(2)
N7 0.054(3) 0.055(3) 0.033(2) 0.000(2) 0.020(2) 0.009(3)
O1 0.044(2) 0.034(2) 0.064(3) -0.0004(18) 0.033(2) -0.0039(17)
O2 0.032(2) 0.049(2) 0.045(2) -0.0004(18) 0.0015(18) -0.0010(17)
O3 0.046(2) 0.032(2) 0.053(2) 0.0062(17) 0.0223(19) 0.0040(17)
O4 0.033(2) 0.053(2) 0.042(2) 0.0008(17) 0.0223(17) 0.0002(17)
O5 0.045(2) 0.061(3) 0.045(2) 0.0025(19) 0.022(2) 0.011(2)
O6 0.036(2) 0.071(3) 0.068(3) 0.015(2) 0.012(2) 0.016(2)
O7 0.048(2) 0.050(2) 0.040(2) -0.0035(18) 0.0202(19) 0.0064(19)
O8 0.046(3) 0.062(3) 0.051(2) -0.002(2) 0.026(2) 0.010(2)
O9 0.077(4) 0.051(3) 0.098(4) -0.030(3) 0.023(3) -0.029(3)
O10 0.033(2) 0.051(2) 0.053(2) -0.0117(19) 0.0208(19) -0.0020(18)
O11 0.055(3) 0.048(2) 0.058(3) -0.008(2) 0.025(2) -0.008(2)
O12 0.098(4) 0.079(3) 0.064(3) 0.006(3) 0.056(3) 0.028(3)
O13 0.055(3) 0.050(2) 0.052(2) -0.004(2) 0.031(2) -0.006(2)
O14 0.301(18) 0.302(18) 0.298(18) 0.001(10) 0.124(11) -0.012(10)
C35 0.16(3) 0.17(3) 0.32(5) 0.06(3) 0.03(3) -0.02(3)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.303(6) . ?
C1 C2 1.402(8) . ?
C1 C6 1.430(8) . ?
C2 C3 1.385(8) . ?
C2 H1 0.9300 . ?
C3 C4 1.378(10) . ?
C3 H2 0.9300 . ?
C4 C5 1.359(10) . ?
C4 H3 0.9300 . ?
C5 C6 1.410(8) . ?
C5 H4 0.9300 . ?
C6 C7 1.422(8) . ?
C7 N1 1.285(7) . ?
C7 H5 0.9300 . ?
C8 N1 1.463(7) . ?
C8 C9 1.508(9) . ?
C8 H7 0.9700 . ?
C8 H8 0.9700 . ?
C9 C10 1.516(8) . ?
C9 H10 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.453(8) . ?
C10 H11 0.9700 . ?
C10 H12 0.9700 . ?
C11 N2 1.291(8) . ?
C11 C12 1.409(9) . ?
C11 H14 0.9300 . ?
C12 C13 1.412(9) . ?
C12 C17 1.424(8) . ?
C13 C14 1.346(11) . ?
C13 H15 0.9300 . ?
C14 C15 1.390(11) . ?
C14 H16 0.9300 . ?
C15 C16 1.372(9) . ?
C15 H17 0.9300 . ?
C16 C17 1.407(9) . ?
C16 H18 0.9300 . ?
C17 O2 1.300(7) . ?
C18 O3 1.298(6) . ?
C18 C19 1.408(8) . ?
C18 C23 1.412(8) . ?
C19 C20 1.371(9) . ?
C19 H19 0.9300 . ?
C20 C21 1.391(11) . ?
C20 H20 0.9300 . ?
C21 C22 1.340(11) . ?
C21 H21 0.9300 . ?
C22 C23 1.411(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.414(9) . ?
C24 N3 1.286(8) . ?
C24 H23 0.9300 . ?
C25 N3 1.474(8) . ?
C25 C26 1.564(10) . ?
C25 H26 0.9700 . ?
C25 H25 0.9700 . ?
C26 C27 1.467(10) . ?
C26 H27 0.9700 . ?
C26 H28 0.9700 . ?
C27 N4 1.472(8) . ?
C27 H30 0.9700 . ?
C27 H29 0.9700 . ?
C28 N4 1.299(8) . ?
C28 C29 1.405(9) . ?
C28 H32 0.9300 . ?
C29 C30 1.418(8) . ?
C29 C34 1.424(7) . ?
C30 C31 1.357(9) . ?
C30 H33 0.9300 . ?
C31 C32 1.395(9) . ?
C31 H34 0.9300 . ?
C32 C33 1.365(8) . ?
C32 H35 0.9300 . ?
C33 C34 1.399(8) . ?
C33 H36 0.9300 . ?
C34 O4 1.296(6) . ?
Pr1 O4 2.434(3) 1_655 ?
Pr1 O3 2.444(3) . ?
Pr1 O2 2.462(4) 3_677 ?
Pr1 O1 2.514(4) . ?
Pr1 O13 2.641(4) . ?
Pr1 O10 2.681(4) . ?
Pr1 O7 2.710(4) . ?
Pr1 O5 2.717(4) . ?
Pr1 O11 2.765(4) . ?
Pr1 O8 2.796(4) . ?
N1 H6 0.8503 . ?
N2 H13 0.8500 . ?
N3 H24 0.8489 . ?
N4 H31 0.8539 . ?
N5 O6 1.226(6) . ?
N5 O7 1.255(6) . ?
N5 O5 1.260(6) . ?
N6 O9 1.217(6) . ?
N6 O8 1.249(6) . ?
N6 O10 1.256(6) . ?
N7 O12 1.224(6) . ?
N7 O11 1.250(6) . ?
N7 O13 1.262(6) . ?
O2 Pr1 2.462(4) 3_677 ?
O4 Pr1 2.434(3) 1_455 ?
O14 C35 1.495(9) . ?
O14 H40 0.8200 . ?
C35 H37 0.9600 . ?
C35 H38 0.9600 . ?
C35 H39 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
O1 C1 C2 121.4(5) . . ?
O1 C1 C6 121.2(5) . . ?
C2 C1 C6 117.3(5) . . ?
C3 C2 C1 120.6(6) . . ?
C3 C2 H1 119.7 . . ?
C1 C2 H1 119.7 . . ?
C4 C3 C2 121.8(7) . . ?
C4 C3 H2 119.1 . . ?
C2 C3 H2 119.1 . . ?
C5 C4 C3 119.4(6) . . ?
C5 C4 H3 120.3 . . ?
C3 C4 H3 120.3 . . ?
C4 C5 C6 121.1(6) . . ?
C4 C5 H4 119.5 . . ?
C6 C5 H4 119.5 . . ?
C5 C6 C7 118.7(6) . . ?
C5 C6 C1 119.8(6) . . ?
C7 C6 C1 121.4(5) . . ?
N1 C7 C6 124.4(6) . . ?
N1 C7 H5 117.8 . . ?
C6 C7 H5 117.8 . . ?
N1 C8 C9 110.2(5) . . ?
N1 C8 H7 109.6 . . ?
C9 C8 H7 109.6 . . ?
N1 C8 H8 109.6 . . ?
C9 C8 H8 109.6 . . ?
H7 C8 H8 108.1 . . ?
C8 C9 C10 113.6(5) . . ?
C8 C9 H10 108.8 . . ?
C10 C9 H10 108.8 . . ?
C8 C9 H9B 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H10 C9 H9B 107.7 . . ?
N2 C10 C9 110.7(5) . . ?
N2 C10 H11 109.5 . . ?
C9 C10 H11 109.5 . . ?
N2 C10 H12 109.5 . . ?
C9 C10 H12 109.5 . . ?
H11 C10 H12 108.1 . . ?
N2 C11 C12 125.7(6) . . ?
N2 C11 H14 117.1 . . ?
C12 C11 H14 117.1 . . ?
C11 C12 C13 118.8(6) . . ?
C11 C12 C17 120.9(6) . . ?
C13 C12 C17 120.3(7) . . ?
C14 C13 C12 121.5(7) . . ?
C14 C13 H15 119.2 . . ?
C12 C13 H15 119.2 . . ?
C13 C14 C15 118.9(7) . . ?
C13 C14 H16 120.5 . . ?
C15 C14 H16 120.5 . . ?
C16 C15 C14 121.5(8) . . ?
C16 C15 H17 119.2 . . ?
C14 C15 H17 119.2 . . ?
C15 C16 C17 121.6(7) . . ?
C15 C16 H18 119.2 . . ?
C17 C16 H18 119.2 . . ?
O2 C17 C16 122.4(6) . . ?
O2 C17 C12 121.5(6) . . ?
C16 C17 C12 116.1(6) . . ?
O3 C18 C19 121.2(5) . . ?
O3 C18 C23 121.2(5) . . ?
C19 C18 C23 117.6(5) . . ?
C20 C19 C18 120.8(6) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 120.9(7) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 H20 119.5 . . ?
C22 C21 C20 119.6(7) . . ?
C22 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C21 C22 C23 121.5(7) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C22 C23 C18 119.4(6) . . ?
C22 C23 C24 118.8(6) . . ?
C18 C23 C24 121.8(5) . . ?
N3 C24 C23 125.1(6) . . ?
N3 C24 H23 117.4 . . ?
C23 C24 H23 117.4 . . ?
N3 C25 C26 110.8(6) . . ?
N3 C25 H26 109.5 . . ?
C26 C25 H26 109.5 . . ?
N3 C25 H25 109.5 . . ?
C26 C25 H25 109.5 . . ?
H26 C25 H25 108.1 . . ?
C27 C26 C25 111.5(7) . . ?
C27 C26 H27 109.3 . . ?
C25 C26 H27 109.3 . . ?
C27 C26 H28 109.3 . . ?
C25 C26 H28 109.3 . . ?
H27 C26 H28 108.0 . . ?
C26 C27 N4 111.6(6) . . ?
C26 C27 H30 109.3 . . ?
N4 C27 H30 109.3 . . ?
C26 C27 H29 109.3 . . ?
N4 C27 H29 109.3 . . ?
H30 C27 H29 108.0 . . ?
N4 C28 C29 125.0(6) . . ?
N4 C28 H32 117.5 . . ?
C29 C28 H32 117.5 . . ?
C28 C29 C30 118.3(5) . . ?
C28 C29 C34 121.3(5) . . ?
C30 C29 C34 120.3(5) . . ?
C31 C30 C29 121.1(6) . . ?
C31 C30 H33 119.4 . . ?
C29 C30 H33 119.4 . . ?
C30 C31 C32 118.1(6) . . ?
C30 C31 H34 120.9 . . ?
C32 C31 H34 120.9 . . ?
C33 C32 C31 122.5(6) . . ?
C33 C32 H35 118.7 . . ?
C31 C32 H35 118.7 . . ?
C32 C33 C34 121.1(6) . . ?
C32 C33 H36 119.5 . . ?
C34 C33 H36 119.5 . . ?
O4 C34 C33 122.6(5) . . ?
O4 C34 C29 120.6(5) . . ?
C33 C34 C29 116.8(5) . . ?
O4 Pr1 O3 91.11(12) 1_655 . ?
O4 Pr1 O2 77.33(13) 1_655 3_677 ?
O3 Pr1 O2 78.81(13) . 3_677 ?
O4 Pr1 O1 80.80(12) 1_655 . ?
O3 Pr1 O1 155.49(14) . . ?
O2 Pr1 O1 76.86(13) 3_677 . ?
O4 Pr1 O13 158.22(13) 1_655 . ?
O3 Pr1 O13 70.66(13) . . ?
O2 Pr1 O13 87.22(13) 3_677 . ?
O1 Pr1 O13 110.80(12) . . ?
O4 Pr1 O10 114.13(12) 1_655 . ?
O3 Pr1 O10 67.60(13) . . ?
O2 Pr1 O10 144.22(13) 3_677 . ?
O1 Pr1 O10 136.74(13) . . ?
O13 Pr1 O10 70.68(12) . . ?
O4 Pr1 O7 133.21(12) 1_655 . ?
O3 Pr1 O7 124.80(13) . . ?
O2 Pr1 O7 133.04(12) 3_677 . ?
O1 Pr1 O7 75.50(12) . . ?
O13 Pr1 O7 68.53(12) . . ?
O10 Pr1 O7 64.84(12) . . ?
O4 Pr1 O5 87.78(12) 1_655 . ?
O3 Pr1 O5 131.05(13) . . ?
O2 Pr1 O5 147.31(13) 3_677 . ?
O1 Pr1 O5 72.08(13) . . ?
O13 Pr1 O5 113.04(13) . . ?
O10 Pr1 O5 68.47(12) . . ?
O7 Pr1 O5 46.73(11) . . ?
O4 Pr1 O11 137.64(13) 1_655 . ?
O3 Pr1 O11 109.82(13) . . ?
O2 Pr1 O11 71.59(13) 3_677 . ?
O1 Pr1 O11 64.80(12) . . ?
O13 Pr1 O11 46.40(12) . . ?
O10 Pr1 O11 107.91(12) . . ?
O7 Pr1 O11 62.47(12) . . ?
O5 Pr1 O11 103.24(12) . . ?
O4 Pr1 O8 68.34(12) 1_655 . ?
O3 Pr1 O8 67.07(13) . . ?
O2 Pr1 O8 130.04(12) 3_677 . ?
O1 Pr1 O8 128.92(13) . . ?
O13 Pr1 O8 112.69(12) . . ?
O10 Pr1 O8 45.81(11) . . ?
O7 Pr1 O8 96.77(12) . . ?
O5 Pr1 O8 67.21(12) . . ?
O11 Pr1 O8 153.52(12) . . ?
C7 N1 C8 125.3(5) . . ?
C7 N1 H6 120.0 . . ?
C8 N1 H6 114.7 . . ?
C11 N2 C10 124.8(5) . . ?
C11 N2 H13 111.8 . . ?
C10 N2 H13 122.8 . . ?
C24 N3 C25 123.5(6) . . ?
C24 N3 H24 115.7 . . ?
C25 N3 H24 120.8 . . ?
C28 N4 C27 123.5(5) . . ?
C28 N4 H31 110.5 . . ?
C27 N4 H31 124.9 . . ?
O6 N5 O7 121.7(5) . . ?
O6 N5 O5 120.6(5) . . ?
O7 N5 O5 117.7(4) . . ?
O9 N6 O8 121.6(5) . . ?
O9 N6 O10 121.6(5) . . ?
O8 N6 O10 116.9(5) . . ?
O12 N7 O11 122.2(5) . . ?
O12 N7 O13 121.6(5) . . ?
O11 N7 O13 116.2(5) . . ?
C1 O1 Pr1 144.8(3) . . ?
C17 O2 Pr1 154.0(4) . 3_677 ?
C18 O3 Pr1 144.5(4) . . ?
C34 O4 Pr1 139.2(3) . 1_455 ?
N5 O5 Pr1 97.2(3) . . ?
N5 O7 Pr1 97.7(3) . . ?
N6 O8 Pr1 95.0(3) . . ?
N6 O10 Pr1 100.5(3) . . ?
N7 O11 Pr1 93.9(3) . . ?
N7 O13 Pr1 99.6(3) . . ?
C35 O14 H40 108.6 . . ?
O14 C35 H37 108.9 . . ?
O14 C35 H38 109.0 . . ?
H37 C35 H38 109.5 . . ?
O14 C35 H39 110.5 . . ?
H37 C35 H39 109.5 . . ?
H38 C35 H39 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
N4 H31 O4 0.85 1.91 2.623(6) 140.1 .
N3 H24 O13 0.85 2.45 3.162(7) 141.8 .
N3 H24 O3 0.85 1.98 2.655(6) 135.6 .
N2 H13 O1 0.85 2.59 3.208(7) 131.1 3_677
N2 H13 O2 0.85 1.94 2.650(6) 140.5 .
N1 H6 O7 0.85 2.50 3.096(6) 128.1 .
N1 H6 O1 0.85 2.01 2.648(6) 131.4 .
O14 H40 O9 0.82 1.82 2.52(3) 142.2 1_655
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.079


data_zxy-3
_database_code_depnum_ccdc_archive 'CCDC 905492'
#TrackingRef '3-Nd.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H72 N14 Nd2 O26, 2(C H2 Cl2), 2(C H4 O)'
_chemical_formula_sum            'C72 H84 Cl4 N14 Nd2 O28'
_chemical_formula_weight         2023.81
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   10.991(3)
_cell_length_b                   11.023(4)
_cell_length_c                   18.690(7)
_cell_angle_alpha                91.897(12)
_cell_angle_beta                 106.900(11)
_cell_angle_gamma                92.541(10)
_cell_volume                     2162.0(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13400
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.47
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1026
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7566
_exptl_absorpt_correction_T_max  0.7811
_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            16890
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_unetI/netI     0.1516
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7535
_reflns_number_gt                4511
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_data_reduction        
'CrystalStructure (Rigaku/MSC 2002 <i>CrystalStructure</i>)'
_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 (Sheldrick, 2008)'
_refine_special_details          
;
dfix 1.50 0.01 o14 c36
isor 0.01 o14 c36 c35 cl1 cl2
dfix 1.72 0.01 h114 c36
dfix 0.82 0.01 o14 h114
omit 1 -3 4
omit -3 50
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^)+(0.0634P)^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         7535
_refine_ls_number_parameters     541
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0652
_refine_ls_wR_factor_ref         0.1490
_refine_ls_wR_factor_gt          0.1261
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.992
_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
C1 C 0.5724(9) 0.5072(11) 0.4080(7) 0.061(3) Uani 1 1 d . A 1
C2 C 0.6554(10) 0.4266(12) 0.4505(7) 0.079(4) Uani 1 1 d . A 1
H2 H 0.6625 0.3504 0.4296 0.095 Uiso 1 1 calc R A 1
C3 C 0.7271(12) 0.4584(17) 0.5228(9) 0.103(5) Uani 1 1 d . A 1
H3 H 0.7828 0.4037 0.5497 0.123 Uiso 1 1 calc R A 1
C4 C 0.7179(14) 0.569(2) 0.5559(9) 0.123(7) Uani 1 1 d . A 1
H4 H 0.7650 0.5865 0.6055 0.148 Uiso 1 1 calc R A 1
C5 C 0.6430(14) 0.6515(16) 0.5186(8) 0.104(5) Uani 1 1 d . A 1
H5 H 0.6404 0.7279 0.5406 0.125 Uiso 1 1 calc R A 1
C6 C 0.5668(10) 0.6197(13) 0.4438(7) 0.074(3) Uani 1 1 d . A 1
N1 N 0.4052(9) 0.6936(8) 0.3390(6) 0.075(3) Uani 1 1 d . A 1
H103 H 0.3967 0.6212 0.3189 0.090 Uiso 1 1 calc R A 1
C8 C 0.3238(11) 0.7850(11) 0.2919(8) 0.094(4) Uani 1 1 d . A 1
H8A H 0.3322 0.7796 0.2416 0.113 Uiso 1 1 calc R A 1
H8B H 0.3531 0.8663 0.3130 0.113 Uiso 1 1 calc R A 1
C9 C 0.1853(12) 0.7625(13) 0.2884(8) 0.100(4) Uani 1 1 d . A 1
H9A H 0.1769 0.7654 0.3386 0.120 Uiso 1 1 calc R A 1
H9B H 0.1547 0.6824 0.2655 0.120 Uiso 1 1 calc R A 1
C10 C 0.1051(13) 0.8599(13) 0.2421(8) 0.102(4) Uani 1 1 d . A 1
H10A H 0.0189 0.8525 0.2459 0.122 Uiso 1 1 calc R A 1
H10B H 0.1414 0.9403 0.2617 0.122 Uiso 1 1 calc R A 1
N2 N 0.1030(10) 0.8439(10) 0.1646(6) 0.091(3) Uani 1 1 d . A 1
H104 H 0.0723 0.7768 0.1398 0.109 Uiso 1 1 calc R A 1
C12 C 0.1387(11) 0.9195(12) 0.0541(8) 0.077(4) Uani 1 1 d . A 1
C13 C 0.1983(13) 1.0125(16) 0.0264(9) 0.109(5) Uani 1 1 d . A 1
H13 H 0.2394 1.0782 0.0579 0.131 Uiso 1 1 calc R A 1
C14 C 0.1971(15) 1.0082(18) -0.0468(13) 0.121(6) Uani 1 1 d . A 1
H14 H 0.2416 1.0685 -0.0643 0.145 Uiso 1 1 calc R A 1
C15 C 0.1300(17) 0.915(2) -0.0950(9) 0.118(6) Uani 1 1 d . A 1
H15 H 0.1231 0.9145 -0.1458 0.142 Uiso 1 1 calc R A 1
C16 C 0.0737(16) 0.8223(15) -0.0666(9) 0.120(6) Uani 1 1 d . A 1
H16 H 0.0319 0.7578 -0.0990 0.144 Uiso 1 1 calc R A 1
C17 C 0.0757(13) 0.8196(13) 0.0076(9) 0.089(4) Uani 1 1 d . A 1
C18 C 0.5408(8) 0.6640(9) 0.1896(5) 0.048(2) Uani 1 1 d . B 1
C19 C 0.6323(9) 0.7126(8) 0.2536(6) 0.052(2) Uani 1 1 d . B 1
H19 H 0.6696 0.6616 0.2915 0.062 Uiso 1 1 calc R B 1
C20 C 0.6687(10) 0.8356(9) 0.2617(6) 0.072(3) Uani 1 1 d . B 1
H20 H 0.7304 0.8665 0.3047 0.086 Uiso 1 1 calc R B 1
C21 C 0.6124(13) 0.9129(10) 0.2053(8) 0.093(4) Uani 1 1 d . B 1
H21 H 0.6363 0.9955 0.2113 0.111 Uiso 1 1 calc R B 1
C22 C 0.5247(11) 0.8704(10) 0.1426(7) 0.078(3) Uani 1 1 d . B 1
H22 H 0.4887 0.9231 0.1054 0.093 Uiso 1 1 calc R B 1
C23 C 0.4866(9) 0.7448(8) 0.1327(5) 0.045(2) Uani 1 1 d . B 1
N3 N 0.3469(7) 0.5950(7) 0.0479(4) 0.0455(18) Uani 1 1 d . B 1
H101 H 0.3759 0.5410 0.0796 0.055 Uiso 1 1 calc R B 1
C25 C 0.2498(9) 0.5552(9) -0.0208(5) 0.055(2) Uani 1 1 d . B 1
H25A H 0.2365 0.6199 -0.0558 0.066 Uiso 1 1 calc R B 1
H25B H 0.1700 0.5359 -0.0103 0.066 Uiso 1 1 calc R B 1
C26 C 0.2921(8) 0.4431(8) -0.0551(5) 0.049(2) Uani 1 1 d . B 1
H26A H 0.2993 0.3769 -0.0215 0.059 Uiso 1 1 calc R B 1
H26B H 0.3752 0.4610 -0.0619 0.059 Uiso 1 1 calc R B 1
C27 C 0.1964(9) 0.4048(8) -0.1307(5) 0.055(3) Uani 1 1 d . B 1
H27A H 0.2197 0.3286 -0.1492 0.066 Uiso 1 1 calc R B 1
H27B H 0.1123 0.3921 -0.1245 0.066 Uiso 1 1 calc R B 1
N4 N 0.1935(6) 0.4970(7) -0.1850(4) 0.0472(19) Uani 1 1 d . B 1
H102 H 0.2607 0.5101 -0.1990 0.057 Uiso 1 1 calc R B 1
C29 C 0.0941(8) 0.6584(9) -0.2603(5) 0.048(2) Uani 1 1 d . B 1
C30 C -0.0192(8) 0.7226(10) -0.2831(6) 0.061(3) Uani 1 1 d . B 1
H30 H -0.0894 0.6971 -0.2680 0.073 Uiso 1 1 calc R B 1
C31 C -0.0272(9) 0.8197(10) -0.3261(6) 0.067(3) Uani 1 1 d . B 1
H31 H -0.1025 0.8598 -0.3414 0.080 Uiso 1 1 calc R B 1
C32 C 0.0789(10) 0.8586(10) -0.3471(6) 0.072(3) Uani 1 1 d . B 1
H32 H 0.0737 0.9258 -0.3764 0.087 Uiso 1 1 calc R B 1
C33 C 0.1918(9) 0.8007(9) -0.3257(6) 0.060(3) Uani 1 1 d . B 1
H33 H 0.2612 0.8299 -0.3402 0.072 Uiso 1 1 calc R B 1
C34 C 0.2029(8) 0.6971(8) -0.2818(5) 0.048(2) Uani 1 1 d . B 1
Nd1 Nd 0.47264(5) 0.36275(5) 0.23065(3) 0.04027(17) Uani 1 1 d . . 1
C7 C 0.4861(12) 0.7076(12) 0.4053(8) 0.083(4) Uani 1 1 d . A 1
H7 H 0.4915 0.7832 0.4300 0.099 Uiso 1 1 calc R A 1
C11 C 0.1454(11) 0.9267(12) 0.1339(8) 0.084(4) Uani 1 1 d . A 1
H11 H 0.1831 0.9964 0.1626 0.101 Uiso 1 1 calc R A 1
C24 C 0.3930(9) 0.7054(9) 0.0650(5) 0.053(3) Uani 1 1 d . B 1
H24 H 0.3626 0.7636 0.0302 0.064 Uiso 1 1 calc R B 1
C28 C 0.0963(8) 0.5607(8) -0.2135(5) 0.047(2) Uani 1 1 d . B 1
H28 H 0.0214 0.5399 -0.2020 0.057 Uiso 1 1 calc R B 1
N5 N 0.2114(7) 0.4467(7) 0.1556(5) 0.053(2) Uani 1 1 d . C 1
N6 N 0.5036(8) 0.2124(8) 0.1033(5) 0.064(2) Uani 1 1 d . D 1
N7 N 0.3883(8) 0.1623(7) 0.3140(5) 0.061(2) Uani 1 1 d . E 1
O1 O 0.5017(6) 0.4785(6) 0.3399(4) 0.0610(18) Uani 1 1 d . A 1
O2 O 0.0228(11) 0.7294(9) 0.0342(6) 0.125(3) Uani 1 1 d . A 1
O3 O 0.5072(6) 0.5479(5) 0.1804(3) 0.0535(16) Uani 1 1 d . B 1
O4 O 0.3074(5) 0.6401(6) -0.2623(3) 0.0517(17) Uani 1 1 d . . 1
O5 O 0.2632(7) 0.4729(6) 0.2246(4) 0.0665(19) Uani 1 1 d . C 1
O6 O 0.1075(6) 0.4853(7) 0.1225(4) 0.084(3) Uani 1 1 d . C 1
O7 O 0.2680(5) 0.3786(6) 0.1223(4) 0.0548(17) Uani 1 1 d . C 1
O8 O 0.5218(6) 0.3258(6) 0.1044(4) 0.0572(18) Uani 1 1 d . D 1
O9 O 0.5167(10) 0.1465(8) 0.0532(5) 0.120(4) Uani 1 1 d . D 1
O10 O 0.4701(7) 0.1686(6) 0.1574(4) 0.070(2) Uani 1 1 d . D 1
O11 O 0.3101(6) 0.2166(6) 0.2641(4) 0.071(2) Uani 1 1 d . E 1
O12 O 0.3531(8) 0.0855(7) 0.3500(5) 0.096(3) Uani 1 1 d . E 1
O13 O 0.5053(6) 0.1928(6) 0.3256(4) 0.067(2) Uani 1 1 d . E 1
C35 C 0.0513(15) 0.3157(14) 0.5336(9) 0.121(5) Uani 1 1 d U F 1
H35A H -0.0206 0.3336 0.4917 0.146 Uiso 1 1 calc R F 1
H35B H 0.1268 0.3209 0.5167 0.146 Uiso 1 1 calc R F 1
Cl1 Cl 0.0679(4) 0.4241(4) 0.6036(3) 0.1317(15) Uani 1 1 d U F 1
Cl2 Cl 0.0299(7) 0.1747(5) 0.5569(3) 0.212(3) Uani 1 1 d U F 1
O14 O 0.6924(19) 0.083(2) 0.5031(12) 0.331(11) Uani 1 1 d DU G 1
H114 H 0.6189 0.1126 0.4965 0.497 Uiso 1 1 d RD G 1
C36 C 0.638(2) -0.010(2) 0.4426(14) 0.269(13) Uani 1 1 d DU G 1
H36A H 0.5633 -0.0504 0.4494 0.404 Uiso 1 1 d R G 1
H36B H 0.7013 -0.0685 0.4443 0.404 Uiso 1 1 d R G 1
H36C H 0.6170 0.0264 0.3950 0.404 Uiso 1 1 d R G 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.049(6) 0.075(8) 0.066(8) 0.003(7) 0.027(6) -0.003(6)
C2 0.063(7) 0.112(10) 0.054(8) 0.020(7) 0.005(6) -0.008(7)
C3 0.065(8) 0.150(16) 0.091(13) 0.029(11) 0.018(9) -0.012(9)
C4 0.072(10) 0.22(2) 0.067(11) 0.000(14) 0.007(9) -0.037(13)
C5 0.090(10) 0.156(16) 0.058(9) -0.041(10) 0.020(8) -0.036(10)
C6 0.048(6) 0.113(11) 0.063(8) 0.001(8) 0.020(6) 0.004(7)
N1 0.084(7) 0.062(6) 0.089(8) -0.018(6) 0.044(6) 0.008(5)
C8 0.091(9) 0.065(8) 0.138(13) 0.002(8) 0.047(9) 0.020(7)
C9 0.094(9) 0.123(12) 0.096(11) 0.010(9) 0.041(9) 0.033(8)
C10 0.095(10) 0.111(12) 0.099(12) -0.001(9) 0.026(9) 0.031(8)
N2 0.108(8) 0.067(7) 0.091(9) 0.005(6) 0.018(7) 0.018(6)
C12 0.062(7) 0.068(8) 0.100(11) 0.022(8) 0.017(7) 0.023(6)
C13 0.080(9) 0.137(15) 0.094(12) -0.008(11) 0.000(9) 0.016(9)
C14 0.079(10) 0.133(16) 0.146(18) 0.023(14) 0.023(12) 0.020(10)
C15 0.120(13) 0.155(18) 0.081(12) 0.025(13) 0.018(11) 0.073(13)
C16 0.159(15) 0.101(13) 0.095(13) 0.011(10) 0.017(12) 0.075(11)
C17 0.091(9) 0.068(9) 0.097(12) -0.023(9) 0.014(9) 0.006(7)
C18 0.049(5) 0.063(7) 0.039(6) 0.012(5) 0.019(5) 0.011(5)
C19 0.058(6) 0.042(6) 0.052(6) 0.003(5) 0.009(5) 0.014(5)
C20 0.086(8) 0.048(7) 0.066(8) -0.014(6) 0.000(6) -0.007(6)
C21 0.118(11) 0.039(7) 0.109(12) 0.009(8) 0.014(10) -0.007(7)
C22 0.080(8) 0.062(8) 0.079(9) 0.019(7) 0.003(7) -0.004(6)
C23 0.063(6) 0.030(5) 0.042(6) 0.001(4) 0.016(5) 0.003(4)
N3 0.055(4) 0.043(5) 0.036(4) 0.005(4) 0.009(4) 0.002(4)
C25 0.052(5) 0.062(7) 0.044(6) 0.000(5) 0.003(5) 0.004(5)
C26 0.053(5) 0.053(6) 0.042(6) 0.014(5) 0.014(5) 0.010(4)
C27 0.066(6) 0.051(6) 0.052(6) 0.004(5) 0.025(5) -0.007(5)
N4 0.043(4) 0.060(5) 0.040(4) 0.012(4) 0.015(4) 0.002(4)
C29 0.039(5) 0.065(6) 0.039(5) 0.001(5) 0.010(4) 0.000(4)
C30 0.043(5) 0.079(8) 0.062(7) -0.001(6) 0.018(5) 0.003(5)
C31 0.047(5) 0.070(7) 0.081(8) 0.013(7) 0.012(6) 0.018(5)
C32 0.082(8) 0.058(7) 0.074(8) 0.020(6) 0.016(7) 0.017(6)
C33 0.047(5) 0.064(7) 0.073(7) 0.030(6) 0.019(5) 0.012(5)
C34 0.043(5) 0.053(6) 0.046(6) -0.002(5) 0.012(5) -0.005(4)
Nd1 0.0399(3) 0.0408(3) 0.0419(3) 0.0082(2) 0.0138(2) 0.00446(18)
C7 0.091(9) 0.090(10) 0.068(9) -0.055(8) 0.035(8) -0.026(8)
C11 0.070(8) 0.076(9) 0.091(11) -0.011(8) 0.000(7) 0.013(7)
C24 0.058(6) 0.054(7) 0.054(7) 0.013(5) 0.026(5) 0.004(5)
C28 0.040(5) 0.059(6) 0.040(6) 0.000(5) 0.011(4) -0.013(4)
N5 0.039(4) 0.067(6) 0.057(6) 0.018(5) 0.020(4) 0.007(4)
N6 0.073(6) 0.061(6) 0.067(6) 0.003(5) 0.035(5) 0.008(5)
N7 0.067(6) 0.048(5) 0.081(7) 0.008(5) 0.043(5) -0.006(4)
O1 0.062(4) 0.069(5) 0.046(4) 0.005(4) 0.005(4) 0.013(4)
O2 0.163(10) 0.072(7) 0.120(9) -0.003(6) 0.013(7) 0.002(6)
O3 0.074(4) 0.031(4) 0.048(4) 0.006(3) 0.006(3) -0.002(3)
O4 0.026(3) 0.070(4) 0.061(4) 0.018(4) 0.013(3) 0.006(3)
O5 0.075(5) 0.066(5) 0.060(5) -0.003(4) 0.019(4) 0.022(4)
O6 0.055(4) 0.116(7) 0.090(6) 0.032(5) 0.028(4) 0.033(4)
O7 0.048(3) 0.061(4) 0.054(4) 0.006(4) 0.011(3) 0.013(3)
O8 0.075(4) 0.044(4) 0.060(5) 0.005(3) 0.034(4) -0.003(3)
O9 0.207(11) 0.081(6) 0.109(8) -0.015(6) 0.107(8) -0.002(6)
O10 0.111(6) 0.044(4) 0.074(5) 0.003(4) 0.056(5) 0.001(4)
O11 0.059(4) 0.069(5) 0.086(6) 0.027(5) 0.024(4) -0.002(4)
O12 0.118(7) 0.073(5) 0.115(7) 0.039(5) 0.062(6) -0.002(5)
O13 0.064(4) 0.073(5) 0.069(5) 0.033(4) 0.024(4) 0.005(4)
C35 0.138(9) 0.115(9) 0.119(9) 0.008(7) 0.049(7) 0.007(7)
Cl1 0.111(3) 0.155(4) 0.114(3) -0.016(3) 0.014(3) 0.002(3)
Cl2 0.297(7) 0.128(4) 0.171(5) 0.036(4) 0.004(5) 0.004(4)
O14 0.352(14) 0.351(15) 0.306(14) 0.024(10) 0.122(10) 0.005(9)
C36 0.286(16) 0.248(16) 0.269(16) 0.049(10) 0.074(10) -0.013(10)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.303(12) . ?
C1 C2 1.397(14) . ?
C1 C6 1.402(15) . ?
C2 C3 1.377(18) . ?
C2 H2 0.9300 . ?
C3 C4 1.37(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.33(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.427(17) . ?
C5 H5 0.9300 . ?
C6 C7 1.412(16) . ?
N1 C7 1.299(14) . ?
N1 C8 1.506(14) . ?
N1 H103 0.8600 . ?
C8 C9 1.513(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.543(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.447(15) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N2 C11 1.237(14) . ?
N2 H104 0.8600 . ?
C12 C13 1.386(18) . ?
C12 C17 1.402(17) . ?
C12 C11 1.473(17) . ?
C13 C14 1.36(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.38(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.37(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.381(19) . ?
C16 H16 0.9300 . ?
C17 O2 1.313(15) . ?
C18 O3 1.307(11) . ?
C18 C19 1.393(13) . ?
C18 C23 1.421(11) . ?
C19 C20 1.388(13) . ?
C19 H19 0.9300 . ?
C20 C21 1.397(15) . ?
C20 H20 0.9300 . ?
C21 C22 1.338(16) . ?
C21 H21 0.9300 . ?
C22 C23 1.418(13) . ?
C22 H22 0.9300 . ?
C23 C24 1.421(13) . ?
N3 C24 1.290(11) . ?
N3 C25 1.451(11) . ?
N3 H101 0.8600 . ?
C25 C26 1.525(12) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.529(13) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 N4 1.454(10) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
N4 C28 1.296(10) . ?
N4 H102 0.8600 . ?
C29 C28 1.407(11) . ?
C29 C34 1.420(11) . ?
C29 C30 1.422(12) . ?
C30 C31 1.351(13) . ?
C30 H30 0.9300 . ?
C31 C32 1.390(13) . ?
C31 H31 0.9300 . ?
C32 C33 1.381(12) . ?
C32 H32 0.9300 . ?
C33 C34 1.417(12) . ?
C33 H33 0.9300 . ?
C34 O4 1.298(9) . ?
Nd1 O1 2.305(7) . ?
Nd1 O4 2.317(5) 2_665 ?
Nd1 O3 2.336(5) . ?
Nd1 O10 2.497(7) . ?
Nd1 O7 2.569(6) . ?
Nd1 O11 2.576(6) . ?
Nd1 O13 2.587(6) . ?
Nd1 O8 2.594(6) . ?
Nd1 O5 2.625(6) . ?
Nd1 N6 2.965(9) . ?
Nd1 N5 3.008(8) . ?
Nd1 N7 3.009(7) . ?
C7 H7 0.9300 . ?
C11 H11 0.9300 . ?
C24 H24 0.9300 . ?
C28 H28 0.9300 . ?
N5 O6 1.231(9) . ?
N5 O7 1.254(9) . ?
N5 O5 1.267(10) . ?
N6 O9 1.212(10) . ?
N6 O8 1.255(10) . ?
N6 O10 1.275(9) . ?
N7 O12 1.216(9) . ?
N7 O11 1.259(10) . ?
N7 O13 1.268(9) . ?
O4 Nd1 2.317(5) 2_665 ?
C35 Cl2 1.652(14) . ?
C35 Cl1 1.707(16) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
O14 C36 1.470(10) . ?
O14 H114 0.8629 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 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
O1 C1 C2 122.1(12) . . ?
O1 C1 C6 122.0(10) . . ?
C2 C1 C6 115.9(12) . . ?
C3 C2 C1 120.9(14) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C4 C3 C2 121.3(16) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.4 . . ?
C5 C4 C3 121.3(18) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 118.1(17) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 H5 120.9 . . ?
C1 C6 C7 120.1(11) . . ?
C1 C6 C5 122.4(13) . . ?
C7 C6 C5 117.5(14) . . ?
C7 N1 C8 129.8(12) . . ?
C7 N1 H103 115.1 . . ?
C8 N1 H103 115.1 . . ?
N1 C8 C9 111.0(10) . . ?
N1 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
C9 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C8 C9 C10 109.8(11) . . ?
C8 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
C8 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C9 109.5(10) . . ?
N2 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
N2 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
C11 N2 C10 120.0(13) . . ?
C11 N2 H104 120.0 . . ?
C10 N2 H104 120.0 . . ?
C13 C12 C17 120.9(14) . . ?
C13 C12 C11 118.4(14) . . ?
C17 C12 C11 120.7(12) . . ?
C14 C13 C12 120.4(17) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 120.1(18) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C16 C15 C14 118.7(17) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
C15 C16 C17 123.6(18) . . ?
C15 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
O2 C17 C16 122.9(15) . . ?
O2 C17 C12 121.0(14) . . ?
C16 C17 C12 116.1(15) . . ?
O3 C18 C19 121.9(8) . . ?
O3 C18 C23 120.5(9) . . ?
C19 C18 C23 117.6(9) . . ?
C20 C19 C18 121.2(9) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
C19 C20 C21 119.8(11) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 121.2(11) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C21 C22 C23 120.0(11) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C24 117.3(9) . . ?
C22 C23 C18 120.2(10) . . ?
C24 C23 C18 122.5(9) . . ?
C24 N3 C25 125.0(8) . . ?
C24 N3 H101 117.5 . . ?
C25 N3 H101 117.5 . . ?
N3 C25 C26 109.3(7) . . ?
N3 C25 H25A 109.8 . . ?
C26 C25 H25A 109.8 . . ?
N3 C25 H25B 109.8 . . ?
C26 C25 H25B 109.8 . . ?
H25A C25 H25B 108.3 . . ?
C25 C26 C27 110.5(7) . . ?
C25 C26 H26A 109.5 . . ?
C27 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C27 C26 H26B 109.5 . . ?
H26A C26 H26B 108.1 . . ?
N4 C27 C26 110.9(7) . . ?
N4 C27 H27A 109.5 . . ?
C26 C27 H27A 109.5 . . ?
N4 C27 H27B 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.0 . . ?
C28 N4 C27 124.2(7) . . ?
C28 N4 H102 117.9 . . ?
C27 N4 H102 117.9 . . ?
C28 C29 C34 121.8(8) . . ?
C28 C29 C30 118.0(7) . . ?
C34 C29 C30 120.1(8) . . ?
C31 C30 C29 121.4(8) . . ?
C31 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
C30 C31 C32 118.9(9) . . ?
C30 C31 H31 120.6 . . ?
C32 C31 H31 120.6 . . ?
C33 C32 C31 122.0(9) . . ?
C33 C32 H32 119.0 . . ?
C31 C32 H32 119.0 . . ?
C32 C33 C34 120.7(8) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
O4 C34 C33 121.6(7) . . ?
O4 C34 C29 121.6(7) . . ?
C33 C34 C29 116.9(8) . . ?
O1 Nd1 O4 86.9(2) . 2_665 ?
O1 Nd1 O3 84.4(2) . . ?
O4 Nd1 O3 83.3(2) 2_665 . ?
O1 Nd1 O10 153.7(2) . . ?
O4 Nd1 O10 85.8(2) 2_665 . ?
O3 Nd1 O10 119.6(2) . . ?
O1 Nd1 O7 119.4(2) . . ?
O4 Nd1 O7 144.65(19) 2_665 . ?
O3 Nd1 O7 76.9(2) . . ?
O10 Nd1 O7 79.2(2) . . ?
O1 Nd1 O11 91.4(2) . . ?
O4 Nd1 O11 129.9(2) 2_665 . ?
O3 Nd1 O11 146.4(2) . . ?
O10 Nd1 O11 74.3(2) . . ?
O7 Nd1 O11 76.3(2) . . ?
O1 Nd1 O13 80.1(2) . . ?
O4 Nd1 O13 81.31(19) 2_665 . ?
O3 Nd1 O13 158.6(2) . . ?
O10 Nd1 O13 73.8(2) . . ?
O7 Nd1 O13 123.6(2) . . ?
O11 Nd1 O13 49.2(2) . . ?
O1 Nd1 O8 149.8(2) . . ?
O4 Nd1 O8 75.1(2) 2_665 . ?
O3 Nd1 O8 69.7(2) . . ?
O10 Nd1 O8 50.14(19) . . ?
O7 Nd1 O8 70.6(2) . . ?
O11 Nd1 O8 118.8(2) . . ?
O13 Nd1 O8 119.8(2) . . ?
O1 Nd1 O5 70.7(2) . . ?
O4 Nd1 O5 151.6(2) 2_665 . ?
O3 Nd1 O5 77.5(2) . . ?
O10 Nd1 O5 121.9(2) . . ?
O7 Nd1 O5 49.1(2) . . ?
O11 Nd1 O5 69.7(2) . . ?
O13 Nd1 O5 110.6(2) . . ?
O8 Nd1 O5 116.2(2) . . ?
O1 Nd1 N6 166.1(2) . . ?
O4 Nd1 N6 79.2(2) 2_665 . ?
O3 Nd1 N6 94.6(2) . . ?
O10 Nd1 N6 25.2(2) . . ?
O7 Nd1 N6 73.6(2) . . ?
O11 Nd1 N6 96.9(2) . . ?
O13 Nd1 N6 96.9(2) . . ?
O8 Nd1 N6 24.97(18) . . ?
O5 Nd1 N6 122.7(2) . . ?
O1 Nd1 N5 95.1(2) . . ?
O4 Nd1 N5 157.54(19) 2_665 . ?
O3 Nd1 N5 74.7(2) . . ?
O10 Nd1 N5 101.2(3) . . ?
O7 Nd1 N5 24.4(2) . . ?
O11 Nd1 N5 72.5(2) . . ?
O13 Nd1 N5 121.10(19) . . ?
O8 Nd1 N5 92.9(2) . . ?
O5 Nd1 N5 24.8(2) . . ?
N6 Nd1 N5 98.0(2) . . ?
O1 Nd1 N7 84.7(2) . . ?
O4 Nd1 N7 105.9(2) 2_665 . ?
O3 Nd1 N7 165.4(2) . . ?
O10 Nd1 N7 73.1(2) . . ?
O7 Nd1 N7 100.1(2) . . ?
O11 Nd1 N7 24.5(2) . . ?
O13 Nd1 N7 24.8(2) . . ?
O8 Nd1 N7 123.2(2) . . ?
O5 Nd1 N7 89.7(2) . . ?
N6 Nd1 N7 98.3(2) . . ?
N5 Nd1 N7 96.6(2) . . ?
N1 C7 C6 126.7(12) . . ?
N1 C7 H7 116.7 . . ?
C6 C7 H7 116.7 . . ?
N2 C11 C12 122.8(13) . . ?
N2 C11 H11 118.6 . . ?
C12 C11 H11 118.6 . . ?
N3 C24 C23 125.0(9) . . ?
N3 C24 H24 117.5 . . ?
C23 C24 H24 117.5 . . ?
N4 C28 C29 125.7(7) . . ?
N4 C28 H28 117.1 . . ?
C29 C28 H28 117.1 . . ?
O6 N5 O7 121.0(9) . . ?
O6 N5 O5 121.0(8) . . ?
O7 N5 O5 118.0(7) . . ?
O6 N5 Nd1 176.3(6) . . ?
O7 N5 Nd1 57.8(4) . . ?
O5 N5 Nd1 60.4(4) . . ?
O9 N6 O8 122.1(8) . . ?
O9 N6 O10 120.8(9) . . ?
O8 N6 O10 117.1(8) . . ?
O9 N6 Nd1 177.0(7) . . ?
O8 N6 Nd1 60.7(5) . . ?
O10 N6 Nd1 56.4(5) . . ?
O12 N7 O11 121.5(8) . . ?
O12 N7 O13 121.8(9) . . ?
O11 N7 O13 116.7(7) . . ?
O12 N7 Nd1 176.8(7) . . ?
O11 N7 Nd1 58.1(4) . . ?
O13 N7 Nd1 58.7(4) . . ?
C1 O1 Nd1 148.0(7) . . ?
C18 O3 Nd1 150.1(6) . . ?
C34 O4 Nd1 151.4(6) . 2_665 ?
N5 O5 Nd1 94.8(5) . . ?
N5 O7 Nd1 97.8(5) . . ?
N6 O8 Nd1 94.3(5) . . ?
N6 O10 Nd1 98.4(6) . . ?
N7 O11 Nd1 97.4(5) . . ?
N7 O13 Nd1 96.6(5) . . ?
Cl2 C35 Cl1 114.9(9) . . ?
Cl2 C35 H35A 108.6 . . ?
Cl1 C35 H35A 108.6 . . ?
Cl2 C35 H35B 108.6 . . ?
Cl1 C35 H35B 108.5 . . ?
H35A C35 H35B 107.5 . . ?
C36 O14 H114 91.0 . . ?
O14 C36 H36A 110.4 . . ?
O14 C36 H36B 108.0 . . ?
H36A C36 H36B 109.5 . . ?
O14 C36 H36C 110.1 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H103 O1 0.86 1.98 2.639(11) 133.2 .
N1 H103 O5 0.86 2.45 3.210(13) 147.0 .
N2 H104 O2 0.86 1.94 2.599(16) 133.0 .
N3 H101 O3 0.86 2.01 2.672(9) 133.1 .
N3 H101 O7 0.86 2.39 3.019(9) 130.6 .
N4 H102 O4 0.86 2.03 2.677(8) 131.5 .
N4 H102 O3 0.86 2.58 3.325(9) 144.8 2_665
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.119


data_zxy-4
_database_code_depnum_ccdc_archive 'CCDC 905493'
#TrackingRef '4-Sm.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H72 N14 O26 Sm2, 2(C H2 Cl2), 2(C H4 O)'
_chemical_formula_sum            'C72 H84 Cl4 N14 O28 Sm2'
_chemical_formula_weight         2036.03
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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   10.958(2)
_cell_length_b                   10.997(2)
_cell_length_c                   18.676(4)
_cell_angle_alpha                91.91(3)
_cell_angle_beta                 106.88(3)
_cell_angle_gamma                92.56(3)
_cell_volume                     2148.9(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16285
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.47
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1030
_exptl_absorpt_coefficient_mu    1.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5653
_exptl_absorpt_correction_T_max  0.6635
_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            21218
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.1033
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.47
_reflns_number_total             9748
_reflns_number_gt                7080
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_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          
;
dfix 1.50 0.01 c36 o14
dfix 0.90 0.01 n1 h111 n2 h121 n3 h131
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^)+(0.0482P)^2^+3.8466P] 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         9748
_refine_ls_number_parameters     542
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0592
_refine_ls_wR_factor_ref         0.1443
_refine_ls_wR_factor_gt          0.1272
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2035(6) 0.6970(6) 0.2182(4) 0.0439(14) Uani 1 1 d . . .
C2 C 0.1913(7) 0.8018(6) 0.1751(5) 0.0589(19) Uani 1 1 d . . .
H2 H 0.2609 0.8317 0.1607 0.071 Uiso 1 1 calc R . .
C3 C 0.0786(8) 0.8605(7) 0.1539(5) 0.066(2) Uani 1 1 d . . .
H3 H 0.0737 0.9285 0.1251 0.079 Uiso 1 1 calc R . .
C4 C -0.0267(8) 0.8209(7) 0.1745(5) 0.067(2) Uani 1 1 d . . .
H4 H -0.1017 0.8620 0.1598 0.080 Uiso 1 1 calc R . .
C5 C -0.0204(7) 0.7211(7) 0.2165(4) 0.0555(18) Uani 1 1 d . . .
H5 H -0.0917 0.6945 0.2304 0.067 Uiso 1 1 calc R . .
C6 C 0.0933(6) 0.6573(6) 0.2393(4) 0.0434(14) Uani 1 1 d . . .
C7 C 0.0954(6) 0.5596(6) 0.2864(4) 0.0481(15) Uani 1 1 d . . .
H7 H 0.0204 0.5391 0.2980 0.058 Uiso 1 1 calc R . .
C8 C 0.1953(7) 0.4018(6) 0.3697(4) 0.0483(16) Uani 1 1 d . . .
H8A H 0.2181 0.3252 0.3512 0.058 Uiso 1 1 calc R . .
H8B H 0.1110 0.3897 0.3762 0.058 Uiso 1 1 calc R . .
C9 C 0.2910(7) 0.4404(6) 0.4442(4) 0.0471(15) Uani 1 1 d . . .
H9A H 0.3739 0.4581 0.4367 0.057 Uiso 1 1 calc R . .
H9B H 0.2991 0.3738 0.4777 0.057 Uiso 1 1 calc R . .
C10 C 0.2513(7) 0.5530(6) 0.4803(4) 0.0502(16) Uani 1 1 d . . .
H10A H 0.2370 0.6179 0.4453 0.060 Uiso 1 1 calc R . .
H10B H 0.1717 0.5336 0.4914 0.060 Uiso 1 1 calc R . .
C11 C 0.3933(6) 0.7055(6) 0.5658(4) 0.0458(15) Uani 1 1 d . . .
H11 H 0.3611 0.7635 0.5312 0.055 Uiso 1 1 calc R . .
C12 C 0.4871(7) 0.7465(5) 0.6328(4) 0.0447(15) Uani 1 1 d . . .
C13 C 0.5271(8) 0.8712(6) 0.6433(5) 0.064(2) Uani 1 1 d . . .
H13 H 0.4926 0.9245 0.6061 0.077 Uiso 1 1 calc R . .
C14 C 0.6138(10) 0.9131(7) 0.7060(6) 0.078(3) Uani 1 1 d . . .
H14 H 0.6383 0.9958 0.7121 0.094 Uiso 1 1 calc R . .
C15 C 0.6686(9) 0.8367(6) 0.7625(5) 0.067(2) Uani 1 1 d . . .
H15 H 0.7292 0.8682 0.8058 0.080 Uiso 1 1 calc R . .
C16 C 0.6331(7) 0.7131(6) 0.7545(4) 0.0510(16) Uani 1 1 d . . .
H16 H 0.6708 0.6619 0.7923 0.061 Uiso 1 1 calc R . .
C17 C 0.5415(6) 0.6656(5) 0.6903(4) 0.0402(14) Uani 1 1 d . . .
C18 C 0.4263(7) 0.4922(7) 0.0916(4) 0.0559(18) Uani 1 1 d . . .
C19 C 0.3423(8) 0.5735(9) 0.0481(5) 0.071(2) Uani 1 1 d . . .
H19 H 0.3343 0.6495 0.0691 0.086 Uiso 1 1 calc R . .
C20 C 0.2734(10) 0.5433(13) -0.0236(6) 0.097(3) Uani 1 1 d . . .
H20 H 0.2197 0.5995 -0.0506 0.117 Uiso 1 1 calc R . .
C21 C 0.2804(11) 0.4316(15) -0.0578(5) 0.106(4) Uani 1 1 d . . .
H21 H 0.2316 0.4123 -0.1069 0.127 Uiso 1 1 calc R . .
C22 C 0.3593(11) 0.3514(11) -0.0186(6) 0.090(3) Uani 1 1 d . . .
H22 H 0.3650 0.2762 -0.0413 0.108 Uiso 1 1 calc R . .
C23 C 0.4339(8) 0.3784(8) 0.0565(5) 0.065(2) Uani 1 1 d . . .
C24 C 0.5141(9) 0.2917(8) 0.0952(5) 0.072(2) Uani 1 1 d . . .
H24 H 0.5096 0.2157 0.0709 0.087 Uiso 1 1 calc R . .
C25 C 0.6747(9) 0.2148(8) 0.2057(6) 0.080(3) Uani 1 1 d . . .
H25A H 0.6454 0.1346 0.1821 0.097 Uiso 1 1 calc R . .
H25B H 0.6651 0.2156 0.2557 0.097 Uiso 1 1 calc R . .
C26 C 0.8133(9) 0.2376(9) 0.2111(6) 0.083(3) Uani 1 1 d . . .
H26A H 0.8428 0.3177 0.2346 0.100 Uiso 1 1 calc R . .
H26B H 0.8231 0.2364 0.1611 0.100 Uiso 1 1 calc R . .
C27 C 0.8948(11) 0.1419(10) 0.2563(6) 0.098(3) Uani 1 1 d . . .
H27A H 0.8593 0.0611 0.2365 0.118 Uiso 1 1 calc R . .
H27B H 0.9808 0.1507 0.2519 0.118 Uiso 1 1 calc R . .
C28 C 0.8517(8) 0.0709(8) 0.3659(6) 0.078(3) Uani 1 1 d . . .
H28 H 0.8118 0.0021 0.3367 0.093 Uiso 1 1 calc R . .
C29 C 0.8579(8) 0.0781(8) 0.4444(6) 0.072(2) Uani 1 1 d . . .
C30 C 0.7989(9) -0.0129(10) 0.4745(7) 0.093(3) Uani 1 1 d . . .
H30 H 0.7559 -0.0789 0.4436 0.111 Uiso 1 1 calc R . .
C31 C 0.8020(13) -0.0083(13) 0.5486(9) 0.115(4) Uani 1 1 d . . .
H31 H 0.7599 -0.0693 0.5672 0.138 Uiso 1 1 calc R . .
C32 C 0.8678(12) 0.0870(14) 0.5944(7) 0.104(4) Uani 1 1 d . . .
H32 H 0.8716 0.0901 0.6448 0.125 Uiso 1 1 calc R . .
C33 C 0.9281(12) 0.1778(10) 0.5670(7) 0.100(4) Uani 1 1 d . . .
H33 H 0.9741 0.2408 0.5995 0.120 Uiso 1 1 calc R . .
C34 C 0.9219(9) 0.1779(9) 0.4917(6) 0.078(3) Uani 1 1 d . . .
C35 C 0.0530(13) 0.3162(10) 0.0330(7) 0.111(4) Uani 1 1 d . . .
H35A H -0.0189 0.3339 -0.0091 0.133 Uiso 1 1 calc R . .
H35B H 0.1292 0.3222 0.0165 0.133 Uiso 1 1 calc R . .
Cl1 Cl 0.0679(3) 0.4248(3) 0.10387(19) 0.1177(10) Uani 1 1 d . . .
Cl2 Cl 0.0317(6) 0.1733(4) 0.0564(3) 0.196(2) Uani 1 1 d . . .
N1 N 0.1933(5) 0.4956(5) 0.3151(3) 0.0463(13) Uani 1 1 d D . .
H111 H 0.260(5) 0.513(7) 0.298(4) 0.069 Uiso 1 1 d D . .
N2 N 0.3484(6) 0.5942(5) 0.5486(3) 0.0459(12) Uani 1 1 d D . .
H121 H 0.388(7) 0.548(6) 0.586(3) 0.069 Uiso 1 1 d D . .
N3 N 0.5943(7) 0.3074(6) 0.1619(4) 0.0660(18) Uani 1 1 d D . .
H131 H 0.586(9) 0.379(4) 0.185(5) 0.099 Uiso 1 1 d D . .
N4 N 0.8989(8) 0.1556(7) 0.3355(5) 0.081(2) Uani 1 1 d . . .
N5 N 0.4957(6) 0.7883(5) 0.3960(4) 0.0575(16) Uani 1 1 d . . .
N6 N 0.6097(6) 0.8334(5) 0.1863(4) 0.0534(15) Uani 1 1 d . . .
N7 N 0.7872(5) 0.5544(5) 0.3434(3) 0.0489(13) Uani 1 1 d . . .
O1 O 0.3076(4) 0.6396(4) 0.2381(3) 0.0494(11) Uani 1 1 d . . .
O2 O 0.5087(5) 0.5486(4) 0.6809(3) 0.0508(11) Uani 1 1 d . . .
O3 O 0.4952(5) 0.5213(4) 0.1598(3) 0.0536(12) Uani 1 1 d . . .
O4 O 0.9755(11) 0.2690(6) 0.4664(5) 0.120(3) Uani 1 1 d . . .
H4A H 0.9653 0.2567 0.4214 0.180 Uiso 1 1 calc R . .
O5 O 0.4771(5) 0.6737(4) 0.3951(3) 0.0534(12) Uani 1 1 d . . .
O6 O 0.4850(8) 0.8542(5) 0.4465(4) 0.104(3) Uani 1 1 d . . .
O7 O 0.5283(6) 0.8291(4) 0.3415(3) 0.0629(15) Uani 1 1 d . . .
O8 O 0.4938(5) 0.8070(5) 0.1758(3) 0.0644(14) Uani 1 1 d . . .
O9 O 0.6442(6) 0.9116(5) 0.1500(4) 0.088(2) Uani 1 1 d . . .
O10 O 0.6879(5) 0.7790(5) 0.2356(3) 0.0666(15) Uani 1 1 d . . .
O11 O 0.7278(4) 0.6246(4) 0.3756(3) 0.0510(11) Uani 1 1 d . . .
O12 O 0.8899(5) 0.5157(6) 0.3766(3) 0.0738(17) Uani 1 1 d . . .
O13 O 0.7332(5) 0.5265(5) 0.2750(3) 0.0597(13) Uani 1 1 d . . .
O14 O 0.620(2) -0.009(2) 0.9328(13) 0.396(14) Uiso 1 1 d D . .
H14A H 0.6719 -0.0511 0.9207 0.595 Uiso 1 1 d R . .
C36 C 0.698(2) 0.0582(18) 1.0003(11) 0.199(8) Uiso 1 1 d D . .
H36A H 0.7863 0.0464 1.0066 0.299 Uiso 1 1 calc R . .
H36B H 0.6748 0.0291 1.0429 0.299 Uiso 1 1 calc R . .
H36C H 0.6827 0.1433 0.9960 0.299 Uiso 1 1 calc R . .
Sm1 Sm 0.52570(3) 0.63608(3) 0.269291(19) 0.03624(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
C1 0.037(3) 0.051(3) 0.040(4) 0.005(3) 0.005(3) 0.001(3)
C2 0.054(4) 0.057(4) 0.067(5) 0.014(4) 0.020(4) -0.002(3)
C3 0.059(5) 0.055(4) 0.080(6) 0.016(4) 0.012(5) 0.014(4)
C4 0.053(5) 0.070(5) 0.072(6) 0.004(4) 0.007(4) 0.020(4)
C5 0.042(4) 0.067(4) 0.057(5) -0.002(4) 0.012(4) 0.006(3)
C6 0.034(3) 0.053(4) 0.041(4) 0.002(3) 0.008(3) 0.000(3)
C7 0.037(3) 0.069(4) 0.040(4) -0.001(3) 0.013(3) -0.001(3)
C8 0.059(4) 0.044(3) 0.044(4) 0.008(3) 0.020(3) -0.008(3)
C9 0.050(4) 0.054(4) 0.037(4) 0.008(3) 0.011(3) 0.005(3)
C10 0.046(4) 0.065(4) 0.039(4) 0.003(3) 0.010(3) 0.008(3)
C11 0.045(4) 0.047(3) 0.050(4) 0.012(3) 0.019(3) 0.013(3)
C12 0.051(4) 0.041(3) 0.043(4) 0.007(3) 0.015(3) 0.009(3)
C13 0.077(6) 0.040(3) 0.068(5) 0.013(3) 0.007(5) -0.001(4)
C14 0.092(7) 0.045(4) 0.085(7) 0.008(4) 0.006(6) -0.010(4)
C15 0.078(6) 0.046(4) 0.067(5) -0.003(4) 0.007(5) -0.008(4)
C16 0.058(4) 0.048(4) 0.045(4) 0.007(3) 0.011(4) 0.005(3)
C17 0.043(3) 0.040(3) 0.041(4) 0.004(3) 0.018(3) 0.006(3)
C18 0.045(4) 0.082(5) 0.041(4) 0.008(4) 0.013(3) -0.008(4)
C19 0.064(5) 0.098(6) 0.052(5) 0.018(4) 0.015(4) 0.006(5)
C20 0.063(6) 0.160(11) 0.059(6) 0.036(7) 0.002(5) -0.008(7)
C21 0.074(7) 0.193(13) 0.036(5) -0.003(7) -0.001(5) -0.037(8)
C22 0.084(7) 0.119(8) 0.062(6) -0.024(6) 0.024(6) -0.037(6)
C23 0.052(4) 0.088(6) 0.050(5) -0.013(4) 0.014(4) -0.013(4)
C24 0.075(6) 0.075(5) 0.076(6) -0.023(5) 0.040(5) -0.015(5)
C25 0.086(7) 0.061(5) 0.104(8) 0.010(5) 0.041(6) 0.018(5)
C26 0.087(7) 0.085(6) 0.087(7) 0.002(5) 0.038(6) 0.025(5)
C27 0.102(8) 0.104(8) 0.096(8) -0.004(6) 0.037(7) 0.040(6)
C28 0.054(5) 0.067(5) 0.097(8) -0.010(5) -0.001(5) 0.010(4)
C29 0.057(5) 0.066(5) 0.090(7) 0.007(5) 0.012(5) 0.016(4)
C30 0.064(6) 0.096(7) 0.108(9) 0.006(7) 0.010(6) -0.009(5)
C31 0.095(9) 0.131(11) 0.125(12) 0.045(9) 0.035(9) 0.017(8)
C32 0.089(8) 0.137(11) 0.084(8) 0.011(8) 0.015(7) 0.046(8)
C33 0.123(10) 0.085(7) 0.085(8) 0.003(6) 0.016(7) 0.043(7)
C34 0.076(6) 0.073(6) 0.077(7) -0.003(5) 0.007(5) 0.022(5)
C35 0.141(11) 0.108(8) 0.101(9) 0.013(7) 0.064(9) -0.004(7)
Cl1 0.096(2) 0.135(3) 0.105(2) -0.018(2) 0.0065(18) 0.0030(19)
Cl2 0.289(7) 0.102(3) 0.147(4) 0.028(2) -0.015(4) 0.001(3)
N1 0.045(3) 0.058(3) 0.038(3) 0.007(2) 0.016(3) -0.006(3)
N2 0.052(3) 0.048(3) 0.035(3) 0.009(2) 0.008(3) 0.006(3)
N3 0.077(5) 0.062(4) 0.066(5) -0.001(3) 0.032(4) 0.010(4)
N4 0.086(6) 0.076(5) 0.078(6) -0.005(4) 0.018(5) 0.018(4)
N5 0.070(4) 0.048(3) 0.061(4) 0.000(3) 0.030(4) 0.000(3)
N6 0.057(4) 0.044(3) 0.068(4) 0.012(3) 0.032(3) -0.002(3)
N7 0.038(3) 0.060(3) 0.052(4) 0.016(3) 0.015(3) 0.004(3)
O1 0.032(2) 0.061(3) 0.058(3) 0.018(2) 0.014(2) 0.006(2)
O2 0.064(3) 0.034(2) 0.046(3) 0.0082(19) 0.004(2) -0.001(2)
O3 0.065(3) 0.061(3) 0.032(2) 0.001(2) 0.010(2) 0.007(2)
O4 0.186(9) 0.059(4) 0.097(6) 0.000(4) 0.015(6) -0.011(5)
O5 0.065(3) 0.042(2) 0.059(3) 0.008(2) 0.027(3) -0.002(2)
O6 0.174(8) 0.065(4) 0.106(6) -0.018(4) 0.096(6) -0.008(4)
O7 0.096(4) 0.038(2) 0.069(4) 0.006(2) 0.046(3) 0.000(2)
O8 0.055(3) 0.069(3) 0.069(4) 0.030(3) 0.017(3) 0.000(3)
O9 0.096(5) 0.071(4) 0.112(5) 0.042(4) 0.049(4) -0.002(3)
O10 0.047(3) 0.072(3) 0.084(4) 0.025(3) 0.023(3) 0.004(3)
O11 0.043(3) 0.059(3) 0.052(3) 0.002(2) 0.015(2) 0.003(2)
O12 0.046(3) 0.104(4) 0.074(4) 0.026(3) 0.015(3) 0.032(3)
O13 0.052(3) 0.073(3) 0.054(3) 0.000(3) 0.013(3) 0.017(3)
Sm1 0.03549(16) 0.03566(16) 0.03893(18) 0.00881(11) 0.01201(13) 0.00346(11)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.292(7) . ?
C1 C2 1.417(9) . ?
C1 C6 1.431(8) . ?
C2 C3 1.379(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.362(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.420(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.407(9) . ?
C7 N1 1.300(8) . ?
C7 H7 0.9300 . ?
C8 N1 1.472(8) . ?
C8 C9 1.513(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.530(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.448(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.292(8) . ?
C11 C12 1.414(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.410(9) . ?
C12 C17 1.429(8) . ?
C13 C14 1.329(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.383(12) . ?
C14 H14 0.9300 . ?
C15 C16 1.388(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.389(9) . ?
C16 H16 0.9300 . ?
C17 O2 1.312(7) . ?
C18 O3 1.299(9) . ?
C18 C23 1.411(11) . ?
C18 C19 1.412(11) . ?
C19 C20 1.354(13) . ?
C19 H19 0.9300 . ?
C20 C21 1.381(16) . ?
C20 H20 0.9300 . ?
C21 C22 1.343(16) . ?
C21 H21 0.9300 . ?
C22 C23 1.417(13) . ?
C22 H22 0.9300 . ?
C23 C24 1.399(12) . ?
C24 N3 1.301(11) . ?
C24 H24 0.9300 . ?
C25 N3 1.483(11) . ?
C25 C26 1.501(13) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.524(13) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 N4 1.469(12) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 N4 1.274(12) . ?
C28 C29 1.447(13) . ?
C28 H28 0.9300 . ?
C29 C30 1.388(13) . ?
C29 C34 1.408(13) . ?
C30 C31 1.372(16) . ?
C30 H30 0.9300 . ?
C31 C32 1.366(17) . ?
C31 H31 0.9300 . ?
C32 C33 1.367(16) . ?
C32 H32 0.9300 . ?
C33 C34 1.389(14) . ?
C33 H33 0.9300 . ?
C34 O4 1.309(12) . ?
C35 Cl2 1.670(11) . ?
C35 Cl1 1.720(11) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
N1 H111 0.897(10) . ?
N2 H121 0.898(10) . ?
N3 H131 0.900(10) . ?
N5 O6 1.205(7) . ?
N5 O7 1.262(7) . ?
N5 O5 1.266(7) . ?
N5 Sm1 2.958(6) . ?
N6 O9 1.226(7) . ?
N6 O8 1.246(7) . ?
N6 O10 1.250(8) . ?
N6 Sm1 2.972(5) . ?
N7 O12 1.220(7) . ?
N7 O13 1.262(7) . ?
N7 O11 1.274(7) . ?
N7 Sm1 2.990(6) . ?
O1 Sm1 2.292(4) . ?
O2 Sm1 2.323(4) 2_666 ?
O3 Sm1 2.297(4) . ?
O4 H4A 0.8200 . ?
O5 Sm1 2.580(4) . ?
O7 Sm1 2.471(5) . ?
O8 Sm1 2.574(5) . ?
O10 Sm1 2.548(5) . ?
O11 Sm1 2.520(5) . ?
O13 Sm1 2.598(5) . ?
O14 C36 1.455(10) . ?
O14 H14A 0.8200 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
Sm1 O2 2.323(4) 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
O1 C1 C2 122.8(6) . . ?
O1 C1 C6 121.1(6) . . ?
C2 C1 C6 116.1(6) . . ?
C3 C2 C1 121.6(7) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C4 C3 C2 121.6(7) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C5 C4 C3 119.6(7) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.0(7) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C7 C6 C5 117.9(6) . . ?
C7 C6 C1 121.8(6) . . ?
C5 C6 C1 120.2(6) . . ?
N1 C7 C6 125.7(6) . . ?
N1 C7 H7 117.2 . . ?
C6 C7 H7 117.2 . . ?
N1 C8 C9 110.1(5) . . ?
N1 C8 H8A 109.6 . . ?
C9 C8 H8A 109.6 . . ?
N1 C8 H8B 109.6 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 C10 111.8(5) . . ?
C8 C9 H9A 109.3 . . ?
C10 C9 H9A 109.3 . . ?
C8 C9 H9B 109.3 . . ?
C10 C9 H9B 109.3 . . ?
H9A C9 H9B 107.9 . . ?
N2 C10 C9 111.1(5) . . ?
N2 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
N2 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N2 C11 C12 125.6(6) . . ?
N2 C11 H11 117.2 . . ?
C12 C11 H11 117.2 . . ?
C13 C12 C11 119.0(6) . . ?
C13 C12 C17 119.1(7) . . ?
C11 C12 C17 121.9(6) . . ?
C14 C13 C12 120.5(7) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 121.6(8) . . ?
C13 C14 H14 119.2 . . ?
C15 C14 H14 119.2 . . ?
C14 C15 C16 120.0(8) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 120.4(7) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
O2 C17 C16 121.3(6) . . ?
O2 C17 C12 120.3(6) . . ?
C16 C17 C12 118.4(6) . . ?
O3 C18 C23 121.6(7) . . ?
O3 C18 C19 122.0(8) . . ?
C23 C18 C19 116.4(8) . . ?
C20 C19 C18 121.5(10) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C19 C20 C21 122.0(11) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C22 C21 C20 118.6(10) . . ?
C22 C21 H21 120.7 . . ?
C20 C21 H21 120.7 . . ?
C21 C22 C23 121.7(10) . . ?
C21 C22 H22 119.2 . . ?
C23 C22 H22 119.2 . . ?
C24 C23 C18 120.6(8) . . ?
C24 C23 C22 119.7(9) . . ?
C18 C23 C22 119.8(9) . . ?
N3 C24 C23 126.1(8) . . ?
N3 C24 H24 116.9 . . ?
C23 C24 H24 116.9 . . ?
N3 C25 C26 112.0(8) . . ?
N3 C25 H25A 109.2 . . ?
C26 C25 H25A 109.2 . . ?
N3 C25 H25B 109.2 . . ?
C26 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
C25 C26 C27 111.4(9) . . ?
C25 C26 H26A 109.3 . . ?
C27 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
C27 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
N4 C27 C26 110.4(7) . . ?
N4 C27 H27A 109.6 . . ?
C26 C27 H27A 109.6 . . ?
N4 C27 H27B 109.6 . . ?
C26 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
N4 C28 C29 122.2(9) . . ?
N4 C28 H28 118.9 . . ?
C29 C28 H28 118.9 . . ?
C30 C29 C34 118.5(10) . . ?
C30 C29 C28 120.5(10) . . ?
C34 C29 C28 121.1(9) . . ?
C31 C30 C29 121.9(12) . . ?
C31 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
C32 C31 C30 119.1(13) . . ?
C32 C31 H31 120.5 . . ?
C30 C31 H31 120.5 . . ?
C31 C32 C33 120.7(12) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 H32 119.6 . . ?
C32 C33 C34 121.3(12) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 H33 119.4 . . ?
O4 C34 C33 119.9(10) . . ?
O4 C34 C29 121.7(10) . . ?
C33 C34 C29 118.4(11) . . ?
Cl2 C35 Cl1 114.5(7) . . ?
Cl2 C35 H35A 108.6 . . ?
Cl1 C35 H35A 108.6 . . ?
Cl2 C35 H35B 108.6 . . ?
Cl1 C35 H35B 108.6 . . ?
H35A C35 H35B 107.6 . . ?
C7 N1 C8 123.9(5) . . ?
C7 N1 H111 114(5) . . ?
C8 N1 H111 122(5) . . ?
C11 N2 C10 125.3(6) . . ?
C11 N2 H121 108(5) . . ?
C10 N2 H121 127(5) . . ?
C24 N3 C25 127.0(8) . . ?
C24 N3 H131 112(6) . . ?
C25 N3 H131 120(6) . . ?
C28 N4 C27 120.2(9) . . ?
O6 N5 O7 122.1(6) . . ?
O6 N5 O5 122.1(6) . . ?
O7 N5 O5 115.9(5) . . ?
O6 N5 Sm1 177.5(5) . . ?
O7 N5 Sm1 55.4(3) . . ?
O5 N5 Sm1 60.4(3) . . ?
O9 N6 O8 120.4(7) . . ?
O9 N6 O10 121.9(7) . . ?
O8 N6 O10 117.7(5) . . ?
O9 N6 Sm1 177.6(5) . . ?
O8 N6 Sm1 59.5(3) . . ?
O10 N6 Sm1 58.3(3) . . ?
O12 N7 O13 121.8(6) . . ?
O12 N7 O11 122.1(6) . . ?
O13 N7 O11 116.2(5) . . ?
O12 N7 Sm1 175.3(4) . . ?
O13 N7 Sm1 59.9(3) . . ?
O11 N7 Sm1 56.5(3) . . ?
C1 O1 Sm1 151.3(4) . . ?
C17 O2 Sm1 149.9(4) . 2_666 ?
C18 O3 Sm1 149.3(5) . . ?
C34 O4 H4A 109.5 . . ?
N5 O5 Sm1 94.3(4) . . ?
N5 O7 Sm1 99.7(4) . . ?
N6 O8 Sm1 95.8(4) . . ?
N6 O10 Sm1 97.0(4) . . ?
N7 O11 Sm1 98.6(4) . . ?
N7 O13 Sm1 95.2(3) . . ?
C36 O14 H14A 103.3 . . ?
O14 C36 H36A 109.5 . . ?
O14 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
O14 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O1 Sm1 O3 86.61(18) . . ?
O1 Sm1 O2 83.47(16) . 2_666 ?
O3 Sm1 O2 84.57(16) . 2_666 ?
O1 Sm1 O7 85.59(18) . . ?
O3 Sm1 O7 153.12(17) . . ?
O2 Sm1 O7 119.93(16) 2_666 . ?
O1 Sm1 O11 144.88(15) . . ?
O3 Sm1 O11 120.46(16) . . ?
O2 Sm1 O11 77.91(16) 2_666 . ?
O7 Sm1 O11 78.48(18) . . ?
O1 Sm1 O10 130.07(16) . . ?
O3 Sm1 O10 90.93(19) . . ?
O2 Sm1 O10 145.92(17) 2_666 . ?
O7 Sm1 O10 74.80(17) . . ?
O11 Sm1 O10 75.43(17) . . ?
O1 Sm1 O8 81.29(16) . . ?
O3 Sm1 O8 80.26(18) . . ?
O2 Sm1 O8 159.04(18) 2_666 . ?
O7 Sm1 O8 73.14(17) . . ?
O11 Sm1 O8 122.38(17) . . ?
O10 Sm1 O8 49.31(17) . . ?
O1 Sm1 O5 75.21(17) . . ?
O3 Sm1 O5 149.98(17) . . ?
O2 Sm1 O5 69.98(15) 2_666 . ?
O7 Sm1 O5 50.14(15) . . ?
O11 Sm1 O5 70.52(15) . . ?
O10 Sm1 O5 119.07(17) . . ?
O8 Sm1 O5 119.23(16) . . ?
O1 Sm1 O13 151.67(17) . . ?
O3 Sm1 O13 71.07(17) . . ?
O2 Sm1 O13 77.39(17) 2_666 . ?
O7 Sm1 O13 122.08(19) . . ?
O11 Sm1 O13 49.71(16) . . ?
O10 Sm1 O13 69.24(17) . . ?
O8 Sm1 O13 110.73(17) . . ?
O5 Sm1 O13 116.33(16) . . ?
O1 Sm1 N5 79.23(18) . . ?
O3 Sm1 N5 165.77(18) . . ?
O2 Sm1 N5 95.18(16) 2_666 . ?
O7 Sm1 N5 24.87(15) . . ?
O11 Sm1 N5 73.17(17) . . ?
O10 Sm1 N5 97.03(18) . . ?
O8 Sm1 N5 96.00(17) . . ?
O5 Sm1 N5 25.27(14) . . ?
O13 Sm1 N5 122.82(18) . . ?
O1 Sm1 N6 105.83(17) . . ?
O3 Sm1 N6 84.26(17) . . ?
O2 Sm1 N6 164.99(15) 2_666 . ?
O7 Sm1 N6 73.24(15) . . ?
O11 Sm1 N6 99.28(17) . . ?
O10 Sm1 N6 24.68(16) . . ?
O8 Sm1 N6 24.66(16) . . ?
O5 Sm1 N6 123.34(15) . . ?
O13 Sm1 N6 89.50(16) . . ?
N5 Sm1 N6 98.10(16) . . ?
O1 Sm1 N7 158.21(15) . . ?
O3 Sm1 N7 95.62(17) . . ?
O2 Sm1 N7 75.20(16) 2_666 . ?
O7 Sm1 N7 101.09(19) . . ?
O11 Sm1 N7 24.91(15) . . ?
O10 Sm1 N7 71.65(16) . . ?
O8 Sm1 N7 120.48(16) . . ?
O5 Sm1 N7 93.05(16) . . ?
O13 Sm1 N7 24.86(15) . . ?
N5 Sm1 N7 98.08(18) . . ?
N6 Sm1 N7 95.97(16) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H111 O1 0.897(10) 1.96(5) 2.676(7) 136(7) .
N1 H111 O2 0.897(10) 2.57(5) 3.303(7) 139(6) 2_666
N2 H121 O2 0.898(10) 1.87(5) 2.661(7) 145(7) .
N2 H121 O11 0.898(10) 2.47(7) 3.037(7) 121(6) 2_666
N3 H131 O3 0.900(10) 1.89(7) 2.632(8) 138(9) .
N3 H131 O13 0.900(10) 2.47(7) 3.170(9) 135(8) .
O4 H4A N4 0.82 1.86 2.598(11) 148.5 .
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.180
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.126


data_zxy-5
_database_code_depnum_ccdc_archive 'CCDC 905494'
#TrackingRef '5-Eu.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H84 Cl4 Eu2 N14 O28'
_chemical_formula_sum            'C72 H84 Cl4 Eu2 N14 O28'
_chemical_formula_weight         2039.25
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   10.959(2)
_cell_length_b                   10.986(2)
_cell_length_c                   18.638(4)
_cell_angle_alpha                91.99(3)
_cell_angle_beta                 106.84(3)
_cell_angle_gamma                92.56(3)
_cell_volume                     2142.9(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16963
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.54
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1032
_exptl_absorpt_coefficient_mu    1.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6188
_exptl_absorpt_correction_T_max  0.7482
_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            20575
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         27.49
_reflns_number_total             9521
_reflns_number_gt                7614
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_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          
;
dfix 0.90 0.01 n1 h111 n2 h121 n3 h131
dfix 1.50 0.01 c36 o14
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^)+(0.0525P)^2^+0.9797P] 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         9521
_refine_ls_number_parameters     542
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1125
_refine_ls_wR_factor_gt          0.1039
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2040(4) 0.6973(4) 0.2182(3) 0.0428(10) Uani 1 1 d . . .
C2 C 0.1921(5) 0.8016(5) 0.1754(3) 0.0562(13) Uani 1 1 d . . .
H2 H 0.2619 0.8316 0.1613 0.067 Uiso 1 1 calc R . .
C3 C 0.0810(6) 0.8597(5) 0.1542(4) 0.0636(15) Uani 1 1 d . . .
H3 H 0.0764 0.9277 0.1254 0.076 Uiso 1 1 calc R . .
C4 C -0.0263(5) 0.8192(5) 0.1748(4) 0.0649(15) Uani 1 1 d . . .
H4 H -0.1012 0.8603 0.1601 0.078 Uiso 1 1 calc R . .
C5 C -0.0203(5) 0.7198(5) 0.2163(3) 0.0558(13) Uani 1 1 d . . .
H5 H -0.0920 0.6921 0.2295 0.067 Uiso 1 1 calc R . .
C6 C 0.0934(4) 0.6575(4) 0.2399(3) 0.0433(10) Uani 1 1 d . . .
C7 C 0.0963(5) 0.5581(4) 0.2865(3) 0.0463(11) Uani 1 1 d . . .
H7 H 0.0211 0.5367 0.2979 0.056 Uiso 1 1 calc R . .
C8 C 0.1960(5) 0.4009(4) 0.3693(3) 0.0487(12) Uani 1 1 d . . .
H8A H 0.2203 0.3248 0.3508 0.058 Uiso 1 1 calc R . .
H8B H 0.1115 0.3873 0.3752 0.058 Uiso 1 1 calc R . .
C9 C 0.2900(5) 0.4396(4) 0.4444(3) 0.0483(11) Uani 1 1 d . . .
H9A H 0.3735 0.4569 0.4378 0.058 Uiso 1 1 calc R . .
H9B H 0.2969 0.3729 0.4779 0.058 Uiso 1 1 calc R . .
C10 C 0.2504(5) 0.5514(5) 0.4801(3) 0.0498(11) Uani 1 1 d . . .
H10A H 0.2355 0.6159 0.4448 0.060 Uiso 1 1 calc R . .
H10B H 0.1712 0.5319 0.4916 0.060 Uiso 1 1 calc R . .
C11 C 0.3924(5) 0.7052(4) 0.5654(3) 0.0456(11) Uani 1 1 d . . .
H11 H 0.3600 0.7633 0.5308 0.055 Uiso 1 1 calc R . .
C12 C 0.4871(5) 0.7452(4) 0.6333(3) 0.0440(11) Uani 1 1 d . . .
C13 C 0.5247(6) 0.8711(5) 0.6429(4) 0.0639(15) Uani 1 1 d . . .
H13 H 0.4883 0.9238 0.6056 0.077 Uiso 1 1 calc R . .
C14 C 0.6129(7) 0.9144(5) 0.7059(5) 0.083(2) Uani 1 1 d . . .
H14 H 0.6370 0.9972 0.7121 0.100 Uiso 1 1 calc R . .
C15 C 0.6683(6) 0.8370(5) 0.7614(4) 0.0681(16) Uani 1 1 d . . .
H15 H 0.7305 0.8683 0.8042 0.082 Uiso 1 1 calc R . .
C16 C 0.6326(5) 0.7134(4) 0.7545(3) 0.0494(12) Uani 1 1 d . . .
H16 H 0.6699 0.6628 0.7928 0.059 Uiso 1 1 calc R . .
C17 C 0.5412(4) 0.6651(4) 0.6902(3) 0.0402(10) Uani 1 1 d . . .
C18 C 0.4259(5) 0.4942(5) 0.0921(3) 0.0540(13) Uani 1 1 d . . .
C19 C 0.3403(6) 0.5747(7) 0.0492(4) 0.0694(16) Uani 1 1 d . . .
H19 H 0.3305 0.6495 0.0712 0.083 Uiso 1 1 calc R . .
C20 C 0.2719(7) 0.5465(9) -0.0229(4) 0.095(3) Uani 1 1 d . . .
H20 H 0.2176 0.6027 -0.0494 0.114 Uiso 1 1 calc R . .
C21 C 0.2814(7) 0.4350(10) -0.0579(4) 0.098(3) Uani 1 1 d . . .
H21 H 0.2353 0.4174 -0.1079 0.118 Uiso 1 1 calc R . .
C22 C 0.3584(7) 0.3526(8) -0.0185(4) 0.088(2) Uani 1 1 d . . .
H22 H 0.3620 0.2765 -0.0410 0.106 Uiso 1 1 calc R . .
C23 C 0.4332(6) 0.3798(6) 0.0560(3) 0.0618(15) Uani 1 1 d . . .
C24 C 0.5148(6) 0.2918(6) 0.0952(4) 0.0726(19) Uani 1 1 d . . .
H24 H 0.5110 0.2159 0.0707 0.087 Uiso 1 1 calc R . .
C25 C 0.6750(7) 0.2156(6) 0.2046(5) 0.078(2) Uani 1 1 d . . .
H25A H 0.6452 0.1353 0.1811 0.094 Uiso 1 1 calc R . .
H25B H 0.6663 0.2166 0.2549 0.094 Uiso 1 1 calc R . .
C26 C 0.8125(7) 0.2370(6) 0.2095(4) 0.0767(18) Uani 1 1 d . . .
H26A H 0.8425 0.3177 0.2323 0.092 Uiso 1 1 calc R . .
H26B H 0.8221 0.2340 0.1594 0.092 Uiso 1 1 calc R . .
C27 C 0.8936(8) 0.1419(7) 0.2557(5) 0.090(2) Uani 1 1 d . . .
H27A H 0.8581 0.0609 0.2361 0.108 Uiso 1 1 calc R . .
H27B H 0.9796 0.1503 0.2513 0.108 Uiso 1 1 calc R . .
C28 C 0.8532(6) 0.0703(6) 0.3660(4) 0.0754(18) Uani 1 1 d . . .
H28 H 0.8163 0.0000 0.3373 0.090 Uiso 1 1 calc R . .
C29 C 0.8568(6) 0.0783(6) 0.4433(4) 0.0661(15) Uani 1 1 d . . .
C30 C 0.7989(7) -0.0146(8) 0.4747(6) 0.098(3) Uani 1 1 d . . .
H30 H 0.7570 -0.0819 0.4444 0.118 Uiso 1 1 calc R . .
C31 C 0.8035(9) -0.0075(10) 0.5500(6) 0.108(3) Uani 1 1 d . . .
H31 H 0.7621 -0.0679 0.5696 0.129 Uiso 1 1 calc R . .
C32 C 0.8691(9) 0.0887(9) 0.5949(6) 0.102(3) Uani 1 1 d . . .
H32 H 0.8738 0.0929 0.6456 0.123 Uiso 1 1 calc R . .
C33 C 0.9270(9) 0.1776(8) 0.5667(5) 0.093(2) Uani 1 1 d . . .
H33 H 0.9721 0.2416 0.5988 0.111 Uiso 1 1 calc R . .
C34 C 0.9217(7) 0.1773(6) 0.4917(4) 0.0761(18) Uani 1 1 d . . .
C35 C 0.0509(10) 0.3165(8) 0.0327(6) 0.113(3) Uani 1 1 d . . .
H35A H -0.0216 0.3348 -0.0089 0.136 Uiso 1 1 calc R . .
H35B H 0.1262 0.3221 0.0155 0.136 Uiso 1 1 calc R . .
Cl1 Cl 0.0684(2) 0.4247(2) 0.10401(15) 0.1134(7) Uani 1 1 d . . .
Cl2 Cl 0.0292(5) 0.1728(3) 0.0562(2) 0.1869(17) Uani 1 1 d . . .
N1 N 0.1930(4) 0.4945(4) 0.3148(2) 0.0443(9) Uani 1 1 d D . .
H111 H 0.263(4) 0.509(5) 0.300(3) 0.066 Uiso 1 1 d D . .
N2 N 0.3488(4) 0.5942(4) 0.5488(2) 0.0449(9) Uani 1 1 d D . .
H121 H 0.383(5) 0.539(4) 0.583(3) 0.067 Uiso 1 1 d D . .
N3 N 0.5936(5) 0.3073(4) 0.1616(3) 0.0632(13) Uani 1 1 d D . .
H131 H 0.601(7) 0.385(2) 0.179(4) 0.095 Uiso 1 1 d D . .
N4 N 0.8985(6) 0.1556(5) 0.3348(4) 0.0788(15) Uani 1 1 d . . .
N5 N 0.4961(5) 0.7868(4) 0.3956(3) 0.0551(11) Uani 1 1 d . . .
N6 N 0.6098(5) 0.8329(4) 0.1867(3) 0.0533(11) Uani 1 1 d . . .
N7 N 0.7859(4) 0.5547(4) 0.3432(3) 0.0486(10) Uani 1 1 d . . .
O1 O 0.3078(3) 0.6402(3) 0.2381(2) 0.0491(8) Uani 1 1 d . . .
O2 O 0.5082(3) 0.5481(3) 0.6809(2) 0.0497(8) Uani 1 1 d . . .
O3 O 0.4949(3) 0.5215(3) 0.1603(2) 0.0532(8) Uani 1 1 d . . .
O4 O 0.9747(7) 0.2689(4) 0.4664(3) 0.110(2) Uani 1 1 d . . .
H4A H 0.9520 0.2639 0.4204 0.165 Uiso 1 1 calc R . .
O5 O 0.4770(4) 0.6728(3) 0.3949(2) 0.0526(9) Uani 1 1 d . . .
O6 O 0.4838(6) 0.8543(4) 0.4457(3) 0.104(2) Uani 1 1 d . . .
O7 O 0.5285(4) 0.8285(3) 0.3407(2) 0.0610(11) Uani 1 1 d . . .
O8 O 0.4922(4) 0.8050(4) 0.1755(2) 0.0624(10) Uani 1 1 d . . .
O9 O 0.6444(5) 0.9117(4) 0.1506(3) 0.0861(15) Uani 1 1 d . . .
O10 O 0.6875(3) 0.7770(4) 0.2356(3) 0.0651(11) Uani 1 1 d . . .
O11 O 0.7261(3) 0.6249(3) 0.3757(2) 0.0505(8) Uani 1 1 d . . .
O12 O 0.8889(4) 0.5176(4) 0.3762(3) 0.0730(12) Uani 1 1 d . . .
O13 O 0.7321(4) 0.5262(3) 0.2746(2) 0.0599(9) Uani 1 1 d . . .
O14 O 0.3839(19) 0.0088(18) 0.0687(11) 0.387(10) Uiso 1 1 d D . .
H14A H 0.3323 0.0507 0.0807 0.581 Uiso 1 1 d R . .
C36 C 0.3034(15) -0.0535(14) 0.0014(9) 0.199(6) Uiso 1 1 d D . .
H36A H 0.2168 -0.0319 -0.0063 0.298 Uiso 1 1 calc R . .
H36B H 0.3082 -0.1400 0.0061 0.298 Uiso 1 1 calc R . .
H36C H 0.3315 -0.0301 -0.0407 0.298 Uiso 1 1 calc R . .
Eu1 Eu 0.52542(2) 0.635750(19) 0.269309(13) 0.03523(8) 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
C1 0.038(2) 0.050(2) 0.037(3) -0.006(2) 0.007(2) -0.004(2)
C2 0.048(3) 0.055(3) 0.064(4) 0.013(3) 0.013(3) 0.002(2)
C3 0.062(3) 0.058(3) 0.068(4) 0.014(3) 0.011(3) 0.012(3)
C4 0.048(3) 0.072(4) 0.069(4) -0.001(3) 0.006(3) 0.022(3)
C5 0.041(2) 0.073(3) 0.053(3) -0.002(3) 0.014(2) 0.011(2)
C6 0.032(2) 0.055(3) 0.040(3) -0.003(2) 0.008(2) 0.004(2)
C7 0.040(2) 0.060(3) 0.040(3) -0.006(2) 0.015(2) -0.004(2)
C8 0.057(3) 0.049(2) 0.042(3) 0.005(2) 0.019(2) -0.007(2)
C9 0.055(3) 0.048(2) 0.044(3) 0.010(2) 0.016(2) 0.005(2)
C10 0.048(3) 0.063(3) 0.039(3) 0.006(2) 0.012(2) 0.011(2)
C11 0.049(3) 0.044(2) 0.047(3) 0.011(2) 0.017(2) 0.013(2)
C12 0.052(3) 0.036(2) 0.047(3) 0.0018(19) 0.018(2) 0.006(2)
C13 0.079(4) 0.040(2) 0.066(4) 0.014(2) 0.008(3) 0.001(3)
C14 0.102(5) 0.039(3) 0.093(6) 0.001(3) 0.008(4) -0.012(3)
C15 0.073(4) 0.054(3) 0.062(4) -0.014(3) 0.000(3) -0.007(3)
C16 0.053(3) 0.045(2) 0.051(3) 0.005(2) 0.014(2) 0.006(2)
C17 0.046(2) 0.038(2) 0.039(3) 0.0044(18) 0.016(2) 0.0042(19)
C18 0.041(2) 0.078(3) 0.042(3) 0.008(3) 0.011(2) -0.002(2)
C19 0.057(3) 0.097(4) 0.050(4) 0.017(3) 0.008(3) 0.001(3)
C20 0.060(4) 0.160(8) 0.054(5) 0.031(5) 0.002(3) -0.020(5)
C21 0.069(4) 0.173(9) 0.038(4) -0.001(5) -0.002(3) -0.037(5)
C22 0.079(5) 0.127(6) 0.052(4) -0.025(4) 0.019(4) -0.032(5)
C23 0.057(3) 0.082(4) 0.044(3) -0.012(3) 0.015(3) -0.008(3)
C24 0.073(4) 0.078(4) 0.069(5) -0.027(3) 0.031(4) -0.014(3)
C25 0.088(5) 0.057(3) 0.102(6) 0.007(3) 0.043(4) 0.022(3)
C26 0.082(4) 0.083(4) 0.074(5) 0.007(4) 0.034(4) 0.023(4)
C27 0.089(5) 0.103(5) 0.080(6) -0.005(4) 0.025(4) 0.034(4)
C28 0.063(4) 0.067(4) 0.082(5) -0.011(3) 0.000(4) 0.015(3)
C29 0.052(3) 0.069(3) 0.070(5) 0.003(3) 0.005(3) 0.012(3)
C30 0.065(4) 0.109(6) 0.110(8) -0.002(5) 0.011(5) 0.002(4)
C31 0.089(6) 0.132(8) 0.112(8) 0.041(6) 0.040(6) 0.020(6)
C32 0.098(6) 0.125(7) 0.081(6) -0.002(6) 0.017(5) 0.053(6)
C33 0.104(6) 0.085(5) 0.081(6) 0.002(4) 0.009(5) 0.034(5)
C34 0.085(5) 0.067(4) 0.074(5) 0.000(3) 0.017(4) 0.021(3)
C35 0.143(8) 0.105(6) 0.110(8) 0.003(5) 0.068(7) -0.007(6)
Cl1 0.0926(14) 0.1316(18) 0.0991(18) -0.0184(14) 0.0041(13) 0.0055(13)
Cl2 0.280(5) 0.0969(17) 0.141(3) 0.0203(18) -0.006(3) 0.004(2)
N1 0.042(2) 0.053(2) 0.039(2) 0.0034(17) 0.0140(18) -0.0047(19)
N2 0.049(2) 0.052(2) 0.033(2) 0.0096(17) 0.0095(18) 0.0050(19)
N3 0.069(3) 0.058(3) 0.066(4) -0.005(2) 0.026(3) 0.009(2)
N4 0.084(4) 0.077(3) 0.070(4) 0.002(3) 0.012(3) 0.018(3)
N5 0.071(3) 0.044(2) 0.058(3) -0.001(2) 0.033(3) 0.000(2)
N6 0.061(3) 0.046(2) 0.061(3) 0.007(2) 0.031(3) 0.001(2)
N7 0.041(2) 0.058(2) 0.049(3) 0.014(2) 0.015(2) 0.0043(19)
O1 0.0340(15) 0.0578(19) 0.056(2) 0.0140(16) 0.0114(16) 0.0067(15)
O2 0.064(2) 0.0346(15) 0.043(2) 0.0068(13) 0.0045(17) -0.0013(15)
O3 0.058(2) 0.061(2) 0.036(2) 0.0001(16) 0.0065(17) 0.0117(17)
O4 0.166(6) 0.062(3) 0.085(4) -0.003(3) 0.013(4) -0.006(3)
O5 0.065(2) 0.0415(17) 0.056(2) 0.0054(15) 0.0248(19) 0.0031(16)
O6 0.182(6) 0.059(2) 0.102(4) -0.019(2) 0.096(4) -0.006(3)
O7 0.090(3) 0.0382(16) 0.067(3) 0.0054(16) 0.042(2) 0.0032(18)
O8 0.054(2) 0.069(2) 0.064(3) 0.025(2) 0.015(2) 0.0049(19)
O9 0.105(4) 0.068(3) 0.100(4) 0.033(2) 0.052(3) -0.007(3)
O10 0.0448(19) 0.069(2) 0.087(3) 0.030(2) 0.025(2) 0.0049(18)
O11 0.0441(17) 0.0577(19) 0.048(2) -0.0001(16) 0.0113(16) 0.0033(16)
O12 0.0422(19) 0.107(3) 0.073(3) 0.027(2) 0.015(2) 0.029(2)
O13 0.061(2) 0.064(2) 0.053(3) -0.0008(18) 0.013(2) 0.0161(19)
Eu1 0.03486(11) 0.03530(11) 0.03620(13) 0.00628(8) 0.01065(9) 0.00388(8)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.288(6) . ?
C1 C2 1.408(7) . ?
C1 C6 1.440(6) . ?
C2 C3 1.361(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.398(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.353(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.412(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.415(7) . ?
C7 N1 1.287(6) . ?
C7 H7 0.9300 . ?
C8 N1 1.465(6) . ?
C8 C9 1.513(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.516(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.462(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.283(6) . ?
C11 C12 1.425(7) . ?
C11 H11 0.9300 . ?
C12 C17 1.414(7) . ?
C12 C13 1.416(6) . ?
C13 C14 1.342(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.380(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.387(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.390(7) . ?
C16 H16 0.9300 . ?
C17 O2 1.312(5) . ?
C18 O3 1.294(6) . ?
C18 C19 1.411(8) . ?
C18 C23 1.421(8) . ?
C19 C20 1.353(9) . ?
C19 H19 0.9300 . ?
C20 C21 1.390(12) . ?
C20 H20 0.9300 . ?
C21 C22 1.352(12) . ?
C21 H21 0.9300 . ?
C22 C23 1.406(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.420(10) . ?
C24 N3 1.287(9) . ?
C24 H24 0.9300 . ?
C25 N3 1.475(9) . ?
C25 C26 1.491(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.525(10) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 N4 1.461(9) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 N4 1.275(9) . ?
C28 C29 1.429(10) . ?
C28 H28 0.9300 . ?
C29 C30 1.409(10) . ?
C29 C34 1.413(9) . ?
C30 C31 1.390(13) . ?
C30 H30 0.9300 . ?
C31 C32 1.363(12) . ?
C31 H31 0.9300 . ?
C32 C33 1.344(12) . ?
C32 H32 0.9300 . ?
C33 C34 1.381(11) . ?
C33 H33 0.9300 . ?
C34 O4 1.309(8) . ?
C35 Cl2 1.678(9) . ?
C35 Cl1 1.714(9) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
N1 H111 0.898(10) . ?
N2 H121 0.898(10) . ?
N3 H131 0.900(10) . ?
N5 O6 1.214(6) . ?
N5 O5 1.259(5) . ?
N5 O7 1.269(5) . ?
N5 Eu1 2.934(4) . ?
N6 O9 1.228(5) . ?
N6 O10 1.252(6) . ?
N6 O8 1.266(5) . ?
N6 Eu1 2.965(4) . ?
N7 O12 1.215(6) . ?
N7 O13 1.264(6) . ?
N7 O11 1.278(5) . ?
N7 Eu1 2.978(4) . ?
O1 Eu1 2.289(3) . ?
O2 Eu1 2.310(3) 2_666 ?
O3 Eu1 2.282(4) . ?
O4 H4A 0.8200 . ?
O5 Eu1 2.569(4) . ?
O7 Eu1 2.455(3) . ?
O8 Eu1 2.562(4) . ?
O10 Eu1 2.535(3) . ?
O11 Eu1 2.509(4) . ?
O13 Eu1 2.590(4) . ?
O14 C36 1.437(9) . ?
O14 H14A 0.8193 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
Eu1 O2 2.310(3) 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
O1 C1 C2 122.8(4) . . ?
O1 C1 C6 120.9(4) . . ?
C2 C1 C6 116.3(5) . . ?
C3 C2 C1 121.8(5) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
C2 C3 C4 121.4(5) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 119.6(5) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.8(5) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C7 118.3(4) . . ?
C5 C6 C1 120.2(5) . . ?
C7 C6 C1 121.5(4) . . ?
N1 C7 C6 126.2(4) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
N1 C8 C9 110.8(4) . . ?
N1 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C8 C9 C10 112.2(4) . . ?
C8 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
N2 C10 C9 111.1(4) . . ?
N2 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
N2 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
N2 C11 C12 124.3(5) . . ?
N2 C11 H11 117.9 . . ?
C12 C11 H11 117.9 . . ?
C17 C12 C13 120.1(5) . . ?
C17 C12 C11 122.7(4) . . ?
C13 C12 C11 117.2(5) . . ?
C14 C13 C12 119.9(6) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.6(5) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C16 121.1(6) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C15 C16 C17 120.0(5) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
O2 C17 C16 121.6(4) . . ?
O2 C17 C12 120.3(4) . . ?
C16 C17 C12 118.1(4) . . ?
O3 C18 C19 122.7(6) . . ?
O3 C18 C23 121.1(5) . . ?
C19 C18 C23 116.2(6) . . ?
C20 C19 C18 122.0(8) . . ?
C20 C19 H19 119.0 . . ?
C18 C19 H19 119.0 . . ?
C19 C20 C21 121.2(8) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C22 C21 C20 119.1(7) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C21 C22 C23 121.2(8) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 H22 119.4 . . ?
C22 C23 C24 119.7(7) . . ?
C22 C23 C18 120.1(7) . . ?
C24 C23 C18 120.2(5) . . ?
N3 C24 C23 126.1(6) . . ?
N3 C24 H24 117.0 . . ?
C23 C24 H24 117.0 . . ?
N3 C25 C26 113.1(5) . . ?
N3 C25 H25A 109.0 . . ?
C26 C25 H25A 109.0 . . ?
N3 C25 H25B 109.0 . . ?
C26 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C25 C26 C27 111.4(6) . . ?
C25 C26 H26A 109.3 . . ?
C27 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
C27 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
N4 C27 C26 111.4(6) . . ?
N4 C27 H27A 109.4 . . ?
C26 C27 H27A 109.4 . . ?
N4 C27 H27B 109.4 . . ?
C26 C27 H27B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
N4 C28 C29 122.7(6) . . ?
N4 C28 H28 118.6 . . ?
C29 C28 H28 118.6 . . ?
C30 C29 C34 117.4(7) . . ?
C30 C29 C28 121.1(7) . . ?
C34 C29 C28 121.5(6) . . ?
C31 C30 C29 121.1(8) . . ?
C31 C30 H30 119.4 . . ?
C29 C30 H30 119.4 . . ?
C32 C31 C30 119.4(9) . . ?
C32 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C33 C32 C31 120.7(9) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C32 C33 C34 122.3(8) . . ?
C32 C33 H33 118.9 . . ?
C34 C33 H33 118.9 . . ?
O4 C34 C33 119.9(7) . . ?
O4 C34 C29 121.0(7) . . ?
C33 C34 C29 119.1(7) . . ?
Cl2 C35 Cl1 114.5(5) . . ?
Cl2 C35 H35A 108.6 . . ?
Cl1 C35 H35A 108.6 . . ?
Cl2 C35 H35B 108.6 . . ?
Cl1 C35 H35B 108.6 . . ?
H35A C35 H35B 107.6 . . ?
C7 N1 C8 124.4(4) . . ?
C7 N1 H111 117(4) . . ?
C8 N1 H111 118(4) . . ?
C11 N2 C10 125.2(4) . . ?
C11 N2 H121 116(4) . . ?
C10 N2 H121 118(4) . . ?
C24 N3 C25 126.9(6) . . ?
C24 N3 H131 112(5) . . ?
C25 N3 H131 121(5) . . ?
C28 N4 C27 120.4(6) . . ?
O6 N5 O5 122.2(4) . . ?
O6 N5 O7 121.1(4) . . ?
O5 N5 O7 116.6(4) . . ?
O6 N5 Eu1 176.7(4) . . ?
O5 N5 Eu1 60.9(2) . . ?
O7 N5 Eu1 55.7(2) . . ?
O9 N6 O10 122.3(5) . . ?
O9 N6 O8 120.4(5) . . ?
O10 N6 O8 117.2(4) . . ?
O9 N6 Eu1 177.9(4) . . ?
O10 N6 Eu1 58.0(2) . . ?
O8 N6 Eu1 59.3(2) . . ?
O12 N7 O13 121.7(5) . . ?
O12 N7 O11 121.9(5) . . ?
O13 N7 O11 116.4(4) . . ?
O12 N7 Eu1 176.0(3) . . ?
O13 N7 Eu1 60.1(2) . . ?
O11 N7 Eu1 56.5(2) . . ?
C1 O1 Eu1 151.6(3) . . ?
C17 O2 Eu1 149.9(3) . 2_666 ?
C18 O3 Eu1 148.6(4) . . ?
C34 O4 H4A 109.5 . . ?
N5 O5 Eu1 93.8(3) . . ?
N5 O7 Eu1 99.0(3) . . ?
N6 O8 Eu1 95.5(3) . . ?
N6 O10 Eu1 97.3(3) . . ?
N7 O11 Eu1 98.4(3) . . ?
N7 O13 Eu1 94.9(3) . . ?
C36 O14 H14A 100.7 . . ?
O14 C36 H36A 109.5 . . ?
O14 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
O14 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O3 Eu1 O1 86.69(14) . . ?
O3 Eu1 O2 84.66(13) . 2_666 ?
O1 Eu1 O2 83.89(13) . 2_666 ?
O3 Eu1 O7 152.80(14) . . ?
O1 Eu1 O7 85.52(14) . . ?
O2 Eu1 O7 120.25(12) 2_666 . ?
O3 Eu1 O11 120.75(12) . . ?
O1 Eu1 O11 144.70(12) . . ?
O2 Eu1 O11 77.73(12) 2_666 . ?
O7 Eu1 O11 78.33(14) . . ?
O3 Eu1 O10 90.75(14) . . ?
O1 Eu1 O10 130.11(13) . . ?
O2 Eu1 O10 145.45(13) 2_666 . ?
O7 Eu1 O10 74.74(13) . . ?
O11 Eu1 O10 75.39(13) . . ?
O3 Eu1 O8 79.96(13) . . ?
O1 Eu1 O8 80.74(12) . . ?
O2 Eu1 O8 158.79(13) 2_666 . ?
O7 Eu1 O8 73.08(13) . . ?
O11 Eu1 O8 122.82(12) . . ?
O10 Eu1 O8 49.89(13) . . ?
O3 Eu1 O5 149.85(12) . . ?
O1 Eu1 O5 75.19(13) . . ?
O2 Eu1 O5 69.82(11) 2_666 . ?
O7 Eu1 O5 50.64(11) . . ?
O11 Eu1 O5 70.27(12) . . ?
O10 Eu1 O5 119.37(13) . . ?
O8 Eu1 O5 119.48(12) . . ?
O3 Eu1 O13 71.01(13) . . ?
O1 Eu1 O13 151.84(13) . . ?
O2 Eu1 O13 77.26(13) 2_666 . ?
O7 Eu1 O13 122.06(14) . . ?
O11 Eu1 O13 50.07(12) . . ?
O10 Eu1 O13 68.92(12) . . ?
O8 Eu1 O13 110.86(13) . . ?
O5 Eu1 O13 116.36(13) . . ?
O3 Eu1 N5 165.84(14) . . ?
O1 Eu1 N5 79.21(14) . . ?
O2 Eu1 N5 95.08(12) 2_666 . ?
O7 Eu1 N5 25.30(11) . . ?
O11 Eu1 N5 72.79(13) . . ?
O10 Eu1 N5 97.27(13) . . ?
O8 Eu1 N5 96.30(13) . . ?
O5 Eu1 N5 25.35(10) . . ?
O13 Eu1 N5 122.80(14) . . ?
O3 Eu1 N6 84.34(13) . . ?
O1 Eu1 N6 105.73(13) . . ?
O2 Eu1 N6 164.91(12) 2_666 . ?
O7 Eu1 N6 72.83(12) . . ?
O11 Eu1 N6 99.20(13) . . ?
O10 Eu1 N6 24.76(13) . . ?
O8 Eu1 N6 25.15(13) . . ?
O5 Eu1 N6 123.42(11) . . ?
O13 Eu1 N6 89.40(13) . . ?
N5 Eu1 N6 98.11(12) . . ?
O3 Eu1 N7 95.71(13) . . ?
O1 Eu1 N7 158.47(11) . . ?
O2 Eu1 N7 75.07(12) 2_666 . ?
O7 Eu1 N7 101.02(14) . . ?
O11 Eu1 N7 25.11(12) . . ?
O10 Eu1 N7 71.35(12) . . ?
O8 Eu1 N7 120.77(11) . . ?
O5 Eu1 N7 92.99(13) . . ?
O13 Eu1 N7 25.01(12) . . ?
N5 Eu1 N7 97.90(14) . . ?
N6 Eu1 N7 95.80(12) . . ?
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
O4 H4A N4 0.82 1.89 2.602(8) 144.8 .
N3 H131 O13 0.900(10) 2.40(5) 3.162(7) 143(7) .
N3 H131 O3 0.900(10) 1.91(5) 2.631(6) 136(7) .
N2 H121 O11 0.898(10) 2.39(4) 3.029(5) 128(4) 2_666
N2 H121 O2 0.898(10) 1.94(4) 2.653(6) 135(5) .
N1 H111 O2 0.898(10) 2.54(4) 3.308(5) 144(5) 2_666
N1 H111 O1 0.898(10) 2.01(5) 2.684(5) 131(5) .
_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.102


data_zxy-6
_database_code_depnum_ccdc_archive 'CCDC 905495'
#TrackingRef '6-Gd.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H72 Gd2 N14 O26, 2(C H2 Cl2), 2(C H4 O)'
_chemical_formula_sum            'C72 H84 Cl4 Gd2 N14 O28'
_chemical_formula_weight         2049.83
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'
Gd Gd -0.1653 3.9035 '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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   10.948(4)
_cell_length_b                   10.978(3)
_cell_length_c                   18.649(8)
_cell_angle_alpha                91.970(14)
_cell_angle_beta                 106.730(14)
_cell_angle_gamma                92.560(12)
_cell_volume                     2141.7(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13611
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.49
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1034
_exptl_absorpt_coefficient_mu    1.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6705
_exptl_absorpt_correction_T_max  0.7822
_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            14284
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7318
_reflns_number_gt                5826
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 <i>RAPID-AUTO</i>)'
_computing_data_reduction        
'CrystalStructure (Rigaku/MSC 2002 <i>CrystalStructure</i>)'
_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 (Sheldrick, 2008)'
_refine_special_details          
;
OMIT -3.00 50.00
OMIT -1 -1 3
OMIT -6 -3 13
OMIT -3 -1 10
OMIT -1 -3 11
OMIT 0 -8 8
OMIT -3 -3 9
OMIT -5 -3 11
OMIT -3 7 0
OMIT -3 -5 12
OMIT -1 -2 8
OMIT 0 -9 10
OMIT -2 -3 6
OMIT -1 -6 14
dfix 1.50 0.01 o14 c36
isor 0.01 o14 c36 c35 cl1 cl2
dfix 1.92 0.01 h114 c36
dfix 0.85 0.01 n2 h104 o14 h114 n4 h102 n3 h101
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^)+(0.0518P)^2^+3.3613P] 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         7318
_refine_ls_number_parameters     532
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0486
_refine_ls_wR_factor_ref         0.1174
_refine_ls_wR_factor_gt          0.1052
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5745(7) 0.5045(7) 0.4079(4) 0.0513(18) Uani 1 1 d . A 1
C2 C 0.6591(8) 0.4226(9) 0.4498(5) 0.067(2) Uani 1 1 d . A 1
H2 H 0.6675 0.3473 0.4278 0.080 Uiso 1 1 calc R A 1
C3 C 0.7290(9) 0.4517(12) 0.5221(6) 0.092(3) Uani 1 1 d . A 1
H3 H 0.7840 0.3958 0.5486 0.110 Uiso 1 1 calc R A 1
C4 C 0.7196(10) 0.5620(13) 0.5566(5) 0.092(4) Uani 1 1 d . A 1
H4 H 0.7676 0.5800 0.6061 0.110 Uiso 1 1 calc R A 1
C5 C 0.6416(10) 0.6436(11) 0.5193(6) 0.085(3) Uani 1 1 d . A 1
H5 H 0.6365 0.7179 0.5434 0.102 Uiso 1 1 calc R A 1
C6 C 0.5651(8) 0.6198(8) 0.4427(4) 0.059(2) Uani 1 1 d . A 1
N1 N 0.4056(7) 0.6921(6) 0.3378(4) 0.0625(18) Uani 1 1 d . A 1
H103 H 0.3995 0.6207 0.3162 0.075 Uiso 1 1 calc R A 1
C8 C 0.3258(9) 0.7849(8) 0.2956(6) 0.076(3) Uani 1 1 d . A 1
H8A H 0.3355 0.7854 0.2455 0.092 Uiso 1 1 calc R A 1
H8B H 0.3554 0.8647 0.3199 0.092 Uiso 1 1 calc R A 1
C9 C 0.1875(9) 0.7628(9) 0.2899(5) 0.080(3) Uani 1 1 d . A 1
H9A H 0.1768 0.7651 0.3398 0.096 Uiso 1 1 calc R A 1
H9B H 0.1578 0.6824 0.2667 0.096 Uiso 1 1 calc R A 1
C10 C 0.1078(10) 0.8585(9) 0.2440(6) 0.086(3) Uani 1 1 d . A 1
H10A H 0.0216 0.8509 0.2484 0.103 Uiso 1 1 calc R A 1
H10B H 0.1440 0.9392 0.2637 0.103 Uiso 1 1 calc R A 1
N2 N 0.1033(7) 0.8451(7) 0.1664(5) 0.076(2) Uani 1 1 d D A 1
H104 H 0.0704 0.7786 0.1412 0.092 Uiso 1 1 calc RD A 1
C12 C 0.1420(8) 0.9230(8) 0.0564(5) 0.069(2) Uani 1 1 d . A 1
C13 C 0.2027(9) 1.0141(10) 0.0260(7) 0.091(3) Uani 1 1 d . A 1
H13 H 0.2483 1.0792 0.0568 0.110 Uiso 1 1 calc R A 1
C14 C 0.1955(12) 1.0084(13) -0.0502(8) 0.108(4) Uani 1 1 d . A 1
H14 H 0.2337 1.0700 -0.0708 0.129 Uiso 1 1 calc R A 1
C15 C 0.1300(12) 0.9088(13) -0.0940(7) 0.103(4) Uani 1 1 d . A 1
H15 H 0.1252 0.9032 -0.1446 0.123 Uiso 1 1 calc R A 1
C16 C 0.0736(12) 0.8211(10) -0.0655(7) 0.096(3) Uani 1 1 d . A 1
H16 H 0.0288 0.7565 -0.0972 0.115 Uiso 1 1 calc R A 1
C17 C 0.0790(10) 0.8221(9) 0.0098(6) 0.078(3) Uani 1 1 d . A 1
C18 C 0.5412(6) 0.6644(5) 0.1906(4) 0.0368(14) Uani 1 1 d . B 1
C19 C 0.6324(7) 0.7125(6) 0.2547(4) 0.0471(16) Uani 1 1 d . B 1
H19 H 0.6697 0.6610 0.2925 0.057 Uiso 1 1 calc R B 1
C20 C 0.6688(9) 0.8352(7) 0.2634(5) 0.072(2) Uani 1 1 d . B 1
H20 H 0.7295 0.8658 0.3069 0.086 Uiso 1 1 calc R B 1
C21 C 0.6143(10) 0.9140(7) 0.2065(6) 0.079(3) Uani 1 1 d . B 1
H21 H 0.6399 0.9966 0.2124 0.095 Uiso 1 1 calc R B 1
C22 C 0.5248(8) 0.8709(6) 0.1430(5) 0.063(2) Uani 1 1 d . B 1
H22 H 0.4889 0.9237 0.1058 0.075 Uiso 1 1 calc R B 1
C23 C 0.4860(6) 0.7450(5) 0.1336(4) 0.0405(15) Uani 1 1 d . B 1
N3 N 0.3486(5) 0.5943(5) 0.0489(3) 0.0423(13) Uani 1 1 d D B 1
H101 H 0.3789 0.5407 0.0808 0.051 Uiso 1 1 calc RD B 1
C25 C 0.2505(7) 0.5515(6) -0.0203(4) 0.0477(16) Uani 1 1 d . B 1
H25A H 0.2361 0.6159 -0.0556 0.057 Uiso 1 1 calc R B 1
H25B H 0.1708 0.5319 -0.0091 0.057 Uiso 1 1 calc R B 1
C26 C 0.2918(7) 0.4392(6) -0.0551(4) 0.0465(16) Uani 1 1 d . B 1
H26A H 0.2993 0.3728 -0.0214 0.056 Uiso 1 1 calc R B 1
H26B H 0.3750 0.4570 -0.0623 0.056 Uiso 1 1 calc R B 1
C27 C 0.1959(7) 0.4005(6) -0.1302(4) 0.0494(17) Uani 1 1 d . B 1
H27A H 0.2191 0.3239 -0.1487 0.059 Uiso 1 1 calc R B 1
H27B H 0.1116 0.3879 -0.1237 0.059 Uiso 1 1 calc R B 1
N4 N 0.1931(5) 0.4934(5) -0.1848(3) 0.0441(13) Uani 1 1 d D B 1
H102 H 0.2606 0.5058 -0.1990 0.053 Uiso 1 1 calc RD B 1
C29 C 0.0935(6) 0.6574(6) -0.2608(4) 0.0432(15) Uani 1 1 d . B 1
C30 C -0.0190(7) 0.7199(7) -0.2825(4) 0.0533(18) Uani 1 1 d . B 1
H30 H -0.0892 0.6938 -0.2673 0.064 Uiso 1 1 calc R B 1
C31 C -0.0267(7) 0.8185(7) -0.3254(5) 0.062(2) Uani 1 1 d . B 1
H31 H -0.1025 0.8581 -0.3412 0.075 Uiso 1 1 calc R B 1
C32 C 0.0809(8) 0.8595(7) -0.3456(5) 0.063(2) Uani 1 1 d . B 1
H32 H 0.0759 0.9278 -0.3743 0.075 Uiso 1 1 calc R B 1
C33 C 0.1931(7) 0.8024(7) -0.3246(5) 0.0550(18) Uani 1 1 d . B 1
H33 H 0.2631 0.8327 -0.3387 0.066 Uiso 1 1 calc R B 1
C34 C 0.2039(6) 0.6974(6) -0.2815(4) 0.0419(15) Uani 1 1 d . B 1
Gd1 Gd 0.47463(3) 0.36424(3) 0.230482(19) 0.03404(11) Uani 1 1 d . . 1
C7 C 0.4842(9) 0.7084(8) 0.4046(5) 0.068(2) Uani 1 1 d . A 1
H7 H 0.4876 0.7840 0.4294 0.081 Uiso 1 1 calc R A 1
C11 C 0.1470(8) 0.9296(9) 0.1344(6) 0.073(2) Uani 1 1 d . A 1
H11 H 0.1845 0.9998 0.1630 0.087 Uiso 1 1 calc R A 1
C24 C 0.3930(7) 0.7050(6) 0.0655(4) 0.0447(16) Uani 1 1 d . B 1
H24 H 0.3623 0.7632 0.0307 0.054 Uiso 1 1 calc R B 1
C28 C 0.0977(6) 0.5579(6) -0.2133(4) 0.0423(15) Uani 1 1 d . B 1
H28 H 0.0227 0.5373 -0.2015 0.051 Uiso 1 1 calc R B 1
N5 N 0.2151(5) 0.4453(5) 0.1573(4) 0.0464(14) Uani 1 1 d . C 1
N6 N 0.5051(6) 0.2128(5) 0.1052(4) 0.0537(15) Uani 1 1 d . D 1
N7 N 0.3908(7) 0.1681(5) 0.3122(4) 0.0565(16) Uani 1 1 d . E 1
O1 O 0.5063(5) 0.4780(4) 0.3396(3) 0.0507(12) Uani 1 1 d . A 1
O2 O 0.0272(8) 0.7299(6) 0.0353(4) 0.107(2) Uani 1 1 d . A 1
O3 O 0.5074(5) 0.5470(4) 0.1808(3) 0.0492(11) Uani 1 1 d . B 1
O4 O 0.3085(4) 0.6395(4) -0.2614(3) 0.0488(11) Uani 1 1 d . . 1
O5 O 0.2690(5) 0.4741(5) 0.2254(3) 0.0563(13) Uani 1 1 d . C 1
O6 O 0.1114(5) 0.4810(6) 0.1239(3) 0.0730(16) Uani 1 1 d . C 1
O7 O 0.2748(4) 0.3749(4) 0.1249(3) 0.0484(11) Uani 1 1 d . C 1
O8 O 0.5233(5) 0.3271(4) 0.1054(3) 0.0503(12) Uani 1 1 d . D 1
O9 O 0.5164(8) 0.1454(5) 0.0544(4) 0.106(3) Uani 1 1 d . D 1
O10 O 0.4725(5) 0.1709(4) 0.1600(3) 0.0598(14) Uani 1 1 d . D 1
O11 O 0.3125(5) 0.2251(5) 0.2634(3) 0.0639(14) Uani 1 1 d . E 1
O12 O 0.3549(7) 0.0895(5) 0.3493(4) 0.088(2) Uani 1 1 d . E 1
O13 O 0.5070(5) 0.1967(5) 0.3233(3) 0.0596(13) Uani 1 1 d . E 1
C35 C 0.0524(13) 0.3163(10) 0.5332(7) 0.112(4) Uani 1 1 d U F 1
H35A H -0.0187 0.3353 0.4910 0.134 Uiso 1 1 calc R F 1
H35B H 0.1290 0.3209 0.5169 0.134 Uiso 1 1 calc R F 1
Cl1 Cl 0.0686(3) 0.4243(3) 0.60413(19) 0.1126(10) Uani 1 1 d U F 1
Cl2 Cl 0.0279(5) 0.1723(4) 0.5563(3) 0.1766(19) Uani 1 1 d U F 1
O14 O 0.6881(17) 0.0580(16) 0.4987(11) 0.291(9) Uiso 1 1 d D G 1
H114 H 0.6458 0.1222 0.4947 0.436 Uiso 1 1 d RD G 1
C36 C 0.635(2) -0.019(2) 0.4299(14) 0.293(14) Uiso 1 1 d D G 1
H36A H 0.5437 -0.0229 0.4171 0.440 Uiso 1 1 calc R G 1
H36B H 0.6657 -0.0992 0.4377 0.440 Uiso 1 1 calc R G 1
H36C H 0.6618 0.0161 0.3899 0.440 Uiso 1 1 calc R G 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.041(4) 0.076(5) 0.038(4) 0.008(4) 0.013(3) -0.003(4)
C2 0.054(5) 0.092(6) 0.050(5) 0.020(4) 0.008(4) 0.001(4)
C3 0.050(5) 0.154(11) 0.062(6) 0.027(7) 0.002(5) -0.006(6)
C4 0.064(6) 0.162(11) 0.040(5) 0.009(7) 0.003(5) -0.023(7)
C5 0.079(7) 0.113(8) 0.061(6) -0.032(6) 0.025(6) -0.031(6)
C6 0.059(5) 0.075(5) 0.044(4) -0.013(4) 0.021(4) -0.007(4)
N1 0.070(4) 0.053(4) 0.068(5) -0.007(3) 0.028(4) 0.007(3)
C8 0.080(6) 0.057(5) 0.102(8) 0.004(5) 0.040(6) 0.019(4)
C9 0.088(7) 0.095(7) 0.065(6) 0.007(5) 0.031(5) 0.025(5)
C10 0.090(7) 0.087(6) 0.086(7) 0.002(6) 0.030(6) 0.037(5)
N2 0.078(5) 0.070(5) 0.074(5) 0.000(4) 0.009(4) 0.020(4)
C12 0.053(5) 0.073(5) 0.075(6) 0.006(5) 0.005(5) 0.018(4)
C13 0.059(6) 0.093(7) 0.113(10) 0.005(7) 0.011(6) 0.002(5)
C14 0.091(9) 0.128(10) 0.118(11) 0.049(9) 0.046(8) 0.020(7)
C15 0.097(9) 0.124(10) 0.085(8) 0.004(8) 0.017(7) 0.054(8)
C16 0.113(9) 0.080(7) 0.093(9) 0.010(6) 0.024(7) 0.043(6)
C17 0.087(7) 0.068(6) 0.073(7) -0.005(5) 0.014(5) 0.016(5)
C18 0.040(4) 0.036(3) 0.038(4) 0.002(3) 0.018(3) 0.005(3)
C19 0.050(4) 0.048(4) 0.040(4) -0.001(3) 0.009(3) 0.005(3)
C20 0.076(6) 0.053(4) 0.073(6) -0.009(4) 0.005(5) -0.012(4)
C21 0.106(8) 0.043(4) 0.078(7) 0.003(4) 0.012(6) -0.012(5)
C22 0.083(6) 0.037(4) 0.061(5) 0.015(4) 0.008(5) 0.005(4)
C23 0.048(4) 0.037(3) 0.040(4) 0.009(3) 0.015(3) 0.008(3)
N3 0.046(3) 0.048(3) 0.034(3) 0.007(2) 0.011(3) 0.009(3)
C25 0.045(4) 0.059(4) 0.037(4) 0.002(3) 0.009(3) 0.006(3)
C26 0.053(4) 0.046(3) 0.040(4) 0.012(3) 0.012(3) 0.007(3)
C27 0.058(4) 0.052(4) 0.041(4) 0.006(3) 0.019(4) -0.008(3)
N4 0.040(3) 0.052(3) 0.042(3) 0.005(3) 0.015(3) -0.001(3)
C29 0.033(3) 0.056(4) 0.040(4) -0.004(3) 0.010(3) 0.005(3)
C30 0.040(4) 0.064(4) 0.057(5) 0.001(4) 0.016(4) 0.006(3)
C31 0.045(4) 0.068(5) 0.072(6) 0.009(4) 0.008(4) 0.027(4)
C32 0.066(5) 0.054(4) 0.065(5) 0.012(4) 0.011(4) 0.012(4)
C33 0.043(4) 0.057(4) 0.064(5) 0.019(4) 0.011(4) 0.008(3)
C34 0.035(4) 0.046(3) 0.039(4) 0.001(3) 0.002(3) 0.007(3)
Gd1 0.03371(17) 0.03361(16) 0.03600(18) 0.00684(12) 0.01114(13) 0.00391(11)
C7 0.070(6) 0.064(5) 0.075(6) -0.022(5) 0.037(5) -0.011(4)
C11 0.061(5) 0.066(5) 0.080(7) -0.008(5) 0.005(5) 0.011(4)
C24 0.054(4) 0.040(3) 0.044(4) 0.006(3) 0.017(4) 0.011(3)
C28 0.037(4) 0.053(4) 0.039(4) -0.002(3) 0.014(3) -0.001(3)
N5 0.042(3) 0.052(3) 0.051(4) 0.017(3) 0.021(3) 0.006(3)
N6 0.065(4) 0.044(3) 0.057(4) 0.001(3) 0.027(3) 0.006(3)
N7 0.069(5) 0.047(3) 0.062(4) 0.006(3) 0.033(4) -0.004(3)
O1 0.059(3) 0.059(3) 0.032(3) 0.000(2) 0.008(2) 0.010(2)
O2 0.150(7) 0.058(4) 0.097(6) 0.003(4) 0.012(5) -0.011(4)
O3 0.066(3) 0.035(2) 0.040(3) 0.007(2) 0.005(2) 0.003(2)
O4 0.033(2) 0.062(3) 0.054(3) 0.018(2) 0.014(2) 0.009(2)
O5 0.052(3) 0.066(3) 0.049(3) -0.002(3) 0.010(3) 0.019(2)
O6 0.041(3) 0.107(4) 0.073(4) 0.025(4) 0.014(3) 0.028(3)
O7 0.044(3) 0.053(3) 0.048(3) 0.002(2) 0.013(2) 0.005(2)
O8 0.069(3) 0.035(2) 0.052(3) 0.005(2) 0.026(3) 0.002(2)
O9 0.187(8) 0.057(3) 0.107(6) -0.027(4) 0.102(6) -0.015(4)
O10 0.093(4) 0.038(2) 0.063(3) 0.010(2) 0.044(3) 0.005(2)
O11 0.044(3) 0.070(3) 0.082(4) 0.025(3) 0.024(3) 0.006(3)
O12 0.100(5) 0.073(4) 0.107(5) 0.036(4) 0.051(5) -0.004(3)
O13 0.054(3) 0.061(3) 0.064(4) 0.022(3) 0.017(3) -0.003(3)
C35 0.129(8) 0.110(7) 0.112(7) 0.006(6) 0.061(6) 0.004(6)
Cl1 0.091(2) 0.129(2) 0.102(2) -0.0176(19) 0.0067(17) 0.0016(17)
Cl2 0.247(5) 0.103(2) 0.144(4) 0.023(2) -0.002(3) 0.003(3)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.293(8) . ?
C1 C2 1.408(11) . ?
C1 C6 1.424(10) . ?
C2 C3 1.364(13) . ?
C2 H2 0.9300 . ?
C3 C4 1.374(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.336(16) . ?
C4 H4 0.9300 . ?
C5 C6 1.440(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.413(13) . ?
N1 C7 1.296(11) . ?
N1 C8 1.469(11) . ?
N1 H103 0.8600 . ?
C8 C9 1.496(12) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.521(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.436(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N2 C11 1.268(12) . ?
N2 H104 0.8600 . ?
C12 C13 1.400(14) . ?
C12 C17 1.406(12) . ?
C12 C11 1.439(13) . ?
C13 C14 1.400(16) . ?
C13 H13 0.9300 . ?
C14 C15 1.381(16) . ?
C14 H14 0.9300 . ?
C15 C16 1.327(16) . ?
C15 H15 0.9300 . ?
C16 C17 1.388(15) . ?
C16 H16 0.9300 . ?
C17 O2 1.308(12) . ?
C18 O3 1.317(7) . ?
C18 C19 1.389(9) . ?
C18 C23 1.421(9) . ?
C19 C20 1.378(10) . ?
C19 H19 0.9300 . ?
C20 C21 1.406(13) . ?
C20 H20 0.9300 . ?
C21 C22 1.355(12) . ?
C21 H21 0.9300 . ?
C22 C23 1.417(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.421(9) . ?
N3 C24 1.283(8) . ?
N3 C25 1.467(8) . ?
N3 H101 0.8600 . ?
C25 C26 1.520(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.522(10) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 N4 1.461(9) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
N4 C28 1.283(9) . ?
N4 H102 0.8600 . ?
C29 C30 1.399(10) . ?
C29 C28 1.424(10) . ?
C29 C34 1.428(9) . ?
C30 C31 1.360(11) . ?
C30 H30 0.9300 . ?
C31 C32 1.397(11) . ?
C31 H31 0.9300 . ?
C32 C33 1.365(10) . ?
C32 H32 0.9300 . ?
C33 C34 1.418(10) . ?
C33 H33 0.9300 . ?
C34 O4 1.300(8) . ?
Gd1 O4 2.279(4) 2_665 ?
Gd1 O1 2.281(4) . ?
Gd1 O3 2.295(4) . ?
Gd1 O10 2.454(4) . ?
Gd1 O7 2.497(5) . ?
Gd1 O11 2.512(5) . ?
Gd1 O13 2.535(5) . ?
Gd1 O8 2.562(4) . ?
Gd1 O5 2.580(5) . ?
Gd1 N6 2.927(6) . ?
Gd1 N7 2.943(6) . ?
Gd1 N5 2.967(6) . ?
C7 H7 0.9300 . ?
C11 H11 0.9300 . ?
C24 H24 0.9300 . ?
C28 H28 0.9300 . ?
N5 O6 1.217(8) . ?
N5 O5 1.259(7) . ?
N5 O7 1.276(7) . ?
N6 O9 1.220(7) . ?
N6 O8 1.261(7) . ?
N6 O10 1.269(7) . ?
N7 O12 1.242(8) . ?
N7 O13 1.253(8) . ?
N7 O11 1.263(9) . ?
O4 Gd1 2.279(4) 2_665 ?
C35 Cl2 1.682(12) . ?
C35 Cl1 1.711(11) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
O14 C36 1.463(9) . ?
O14 H114 0.8535 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 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
O1 C1 C2 122.1(7) . . ?
O1 C1 C6 119.7(7) . . ?
C2 C1 C6 118.1(7) . . ?
C3 C2 C1 121.2(10) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 121.2(11) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 120.1(10) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.9(10) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C7 C6 C1 122.1(7) . . ?
C7 C6 C5 120.6(8) . . ?
C1 C6 C5 117.4(9) . . ?
C7 N1 C8 125.8(7) . . ?
C7 N1 H103 117.1 . . ?
C8 N1 H103 117.1 . . ?
N1 C8 C9 112.6(8) . . ?
N1 C8 H8A 109.1 . . ?
C9 C8 H8A 109.1 . . ?
N1 C8 H8B 109.1 . . ?
C9 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C8 C9 C10 111.0(8) . . ?
C8 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 C9 111.4(7) . . ?
N2 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
N2 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C11 N2 C10 121.2(8) . . ?
C11 N2 H104 119.4 . . ?
C10 N2 H104 119.4 . . ?
C13 C12 C17 118.8(10) . . ?
C13 C12 C11 121.0(9) . . ?
C17 C12 C11 120.2(9) . . ?
C14 C13 C12 120.7(11) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C15 C14 C13 118.1(12) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C16 C15 C14 121.6(12) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C17 122.4(12) . . ?
C15 C16 H16 118.8 . . ?
C17 C16 H16 118.8 . . ?
O2 C17 C16 119.6(10) . . ?
O2 C17 C12 122.1(9) . . ?
C16 C17 C12 118.2(10) . . ?
O3 C18 C19 121.9(6) . . ?
O3 C18 C23 119.8(6) . . ?
C19 C18 C23 118.3(6) . . ?
C20 C19 C18 121.2(8) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
C19 C20 C21 120.1(8) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 120.6(7) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C21 C22 C23 119.8(8) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C22 C23 C18 120.0(7) . . ?
C22 C23 C24 117.2(7) . . ?
C18 C23 C24 122.8(6) . . ?
C24 N3 C25 125.4(6) . . ?
C24 N3 H101 117.3 . . ?
C25 N3 H101 117.3 . . ?
N3 C25 C26 110.5(6) . . ?
N3 C25 H25A 109.5 . . ?
C26 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
C25 C26 C27 111.0(6) . . ?
C25 C26 H26A 109.4 . . ?
C27 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
C27 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
N4 C27 C26 110.7(5) . . ?
N4 C27 H27A 109.5 . . ?
C26 C27 H27A 109.5 . . ?
N4 C27 H27B 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C28 N4 C27 125.0(6) . . ?
C28 N4 H102 117.5 . . ?
C27 N4 H102 117.5 . . ?
C30 C29 C28 118.3(6) . . ?
C30 C29 C34 120.9(7) . . ?
C28 C29 C34 120.7(6) . . ?
C31 C30 C29 120.7(7) . . ?
C31 C30 H30 119.6 . . ?
C29 C30 H30 119.6 . . ?
C30 C31 C32 119.1(7) . . ?
C30 C31 H31 120.5 . . ?
C32 C31 H31 120.5 . . ?
C33 C32 C31 122.0(8) . . ?
C33 C32 H32 119.0 . . ?
C31 C32 H32 119.0 . . ?
C32 C33 C34 120.6(7) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
O4 C34 C33 122.4(6) . . ?
O4 C34 C29 121.0(6) . . ?
C33 C34 C29 116.6(6) . . ?
O4 Gd1 O1 86.23(17) 2_665 . ?
O4 Gd1 O3 83.89(17) 2_665 . ?
O1 Gd1 O3 84.78(17) . . ?
O4 Gd1 O10 85.45(18) 2_665 . ?
O1 Gd1 O10 152.21(18) . . ?
O3 Gd1 O10 120.53(16) . . ?
O4 Gd1 O7 144.74(16) 2_665 . ?
O1 Gd1 O7 121.12(16) . . ?
O3 Gd1 O7 77.64(16) . . ?
O10 Gd1 O7 78.67(18) . . ?
O4 Gd1 O11 130.70(18) 2_665 . ?
O1 Gd1 O11 90.93(18) . . ?
O3 Gd1 O11 144.86(18) . . ?
O10 Gd1 O11 74.81(17) . . ?
O7 Gd1 O11 74.93(18) . . ?
O4 Gd1 O13 80.95(17) 2_665 . ?
O1 Gd1 O13 79.75(17) . . ?
O3 Gd1 O13 158.95(17) . . ?
O10 Gd1 O13 72.77(17) . . ?
O7 Gd1 O13 122.71(16) . . ?
O11 Gd1 O13 50.27(18) . . ?
O4 Gd1 O8 75.18(17) 2_665 . ?
O1 Gd1 O8 149.74(16) . . ?
O3 Gd1 O8 69.88(15) . . ?
O10 Gd1 O8 50.85(14) . . ?
O7 Gd1 O8 70.35(16) . . ?
O11 Gd1 O8 119.31(17) . . ?
O13 Gd1 O8 119.48(15) . . ?
O4 Gd1 O5 151.49(17) 2_665 . ?
O1 Gd1 O5 71.29(17) . . ?
O3 Gd1 O5 76.96(17) . . ?
O10 Gd1 O5 122.48(18) . . ?
O7 Gd1 O5 50.14(15) . . ?
O11 Gd1 O5 68.68(17) . . ?
O13 Gd1 O5 110.89(17) . . ?
O8 Gd1 O5 116.43(17) . . ?
O4 Gd1 N6 79.09(17) 2_665 . ?
O1 Gd1 N6 165.22(18) . . ?
O3 Gd1 N6 95.27(16) . . ?
O10 Gd1 N6 25.38(15) . . ?
O7 Gd1 N6 73.09(17) . . ?
O11 Gd1 N6 97.31(17) . . ?
O13 Gd1 N6 96.10(17) . . ?
O8 Gd1 N6 25.47(15) . . ?
O5 Gd1 N6 123.17(17) . . ?
O4 Gd1 N7 105.84(19) 2_665 . ?
O1 Gd1 N7 84.44(17) . . ?
O3 Gd1 N7 164.94(16) . . ?
O10 Gd1 N7 72.47(16) . . ?
O7 Gd1 N7 99.11(18) . . ?
O11 Gd1 N7 25.22(18) . . ?
O13 Gd1 N7 25.06(17) . . ?
O8 Gd1 N7 123.26(15) . . ?
O5 Gd1 N7 89.62(18) . . ?
N6 Gd1 N7 97.83(16) . . ?
O4 Gd1 N5 158.33(16) 2_665 . ?
O1 Gd1 N5 96.02(17) . . ?
O3 Gd1 N5 74.89(16) . . ?
O10 Gd1 N5 101.41(18) . . ?
O7 Gd1 N5 25.18(14) . . ?
O11 Gd1 N5 70.91(17) . . ?
O13 Gd1 N5 120.69(16) . . ?
O8 Gd1 N5 93.12(16) . . ?
O5 Gd1 N5 25.01(14) . . ?
N6 Gd1 N5 98.26(18) . . ?
N7 Gd1 N5 95.83(18) . . ?
N1 C7 C6 124.9(7) . . ?
N1 C7 H7 117.5 . . ?
C6 C7 H7 117.5 . . ?
N2 C11 C12 123.8(9) . . ?
N2 C11 H11 118.1 . . ?
C12 C11 H11 118.1 . . ?
N3 C24 C23 124.5(7) . . ?
N3 C24 H24 117.8 . . ?
C23 C24 H24 117.8 . . ?
N4 C28 C29 127.5(6) . . ?
N4 C28 H28 116.2 . . ?
C29 C28 H28 116.2 . . ?
O6 N5 O5 122.4(6) . . ?
O6 N5 O7 121.4(6) . . ?
O5 N5 O7 116.2(6) . . ?
O6 N5 Gd1 176.1(5) . . ?
O5 N5 Gd1 60.0(3) . . ?
O7 N5 Gd1 56.3(3) . . ?
O9 N6 O8 121.9(6) . . ?
O9 N6 O10 121.3(6) . . ?
O8 N6 O10 116.8(5) . . ?
O9 N6 Gd1 177.3(5) . . ?
O8 N6 Gd1 60.9(3) . . ?
O10 N6 Gd1 56.0(3) . . ?
O12 N7 O13 121.1(8) . . ?
O12 N7 O11 121.9(7) . . ?
O13 N7 O11 116.9(6) . . ?
O12 N7 Gd1 176.9(5) . . ?
O13 N7 Gd1 59.0(3) . . ?
O11 N7 Gd1 58.0(3) . . ?
C1 O1 Gd1 149.0(5) . . ?
C18 O3 Gd1 149.5(4) . . ?
C34 O4 Gd1 151.2(4) . 2_665 ?
N5 O5 Gd1 95.0(4) . . ?
N5 O7 Gd1 98.5(4) . . ?
N6 O8 Gd1 93.7(4) . . ?
N6 O10 Gd1 98.6(3) . . ?
N7 O11 Gd1 96.8(4) . . ?
N7 O13 Gd1 96.0(4) . . ?
Cl2 C35 Cl1 114.4(7) . . ?
Cl2 C35 H35A 108.7 . . ?
Cl1 C35 H35A 108.7 . . ?
Cl2 C35 H35B 108.7 . . ?
Cl1 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
C36 O14 H114 107.9 . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H103 O1 0.86 1.98 2.638(8) 132.3 .
N1 H103 O5 0.86 2.39 3.145(8) 146.6 .
N2 H104 O2 0.86 1.94 2.605(10) 132.9 .
N3 H101 O3 0.86 1.98 2.656(7) 134.2 .
N3 H101 O7 0.86 2.40 3.031(7) 131.0 .
N4 H102 O4 0.86 2.05 2.688(7) 130.8 .
N4 H102 O3 0.86 2.56 3.308(7) 146.0 2_665
_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         1.196
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.115