# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2009

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zjw-2
_audit_block_doi                 10.5517/ccnzhdh
_database_code_depnum_ccdc_archive 'CCDC 625127'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/b909213g 2009
_audit_update_record             
;
2006-10-24 deposited with the CCDC.
2015-08-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C52 H48 N16 O12 Pr2, 2(C12 H4 N4), 2(H2 O), H2 O'
_chemical_formula_sum            'C76 H62 N24 O15 Pr2'
_chemical_formula_weight         1833.32

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           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                   11.849(2)
_cell_length_b                   13.655(2)
_cell_length_c                   13.996(2)
_cell_angle_alpha                105.744(2)
_cell_angle_beta                 102.464(2)
_cell_angle_gamma                100.294(2)
_cell_volume                     2059.3(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5922
_cell_measurement_theta_min      5.16
_cell_measurement_theta_max      51.17

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.221
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             924
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8005
_exptl_absorpt_correction_T_max  0.8177
_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       'ω 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            11477
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         26.10
_reflns_number_total             7889
_reflns_number_gt                7192
_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          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.1033P)²+5.4087P] where P=(Fo²+2Fc²)/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         7889
_refine_ls_number_parameters     565
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0545
_refine_ls_wR_factor_ref         0.1672
_refine_ls_wR_factor_gt          0.1626
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_restrained_S_all      1.102
_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 0.9379(5) 0.5365(4) 0.8522(4) 0.0301(11) Uani 1 1 d . . .
C2 C 1.0795(5) 0.4309(5) 0.8490(4) 0.0329(12) Uani 1 1 d . . .
C3 C 0.9917(5) 0.4668(4) 0.7927(4) 0.0294(11) Uani 1 1 d . . .
C4 C 0.9575(5) 0.4368(4) 0.6824(4) 0.0285(11) Uani 1 1 d . . .
C5 C 0.8694(5) 0.4758(4) 0.6289(4) 0.0295(11) Uani 1 1 d . . .
H1 H 0.8309 0.5192 0.6663 0.035 Uiso 1 1 calc R . .
C6 C 0.8398(5) 0.4511(4) 0.5240(4) 0.0316(12) Uani 1 1 d . . .
C7 C 0.8961(5) 0.3844(4) 0.4640(4) 0.0303(11) Uani 1 1 d . . .
C8 C 0.9825(5) 0.3434(5) 0.5170(4) 0.0347(12) Uani 1 1 d . . .
C9 C 1.0125(5) 0.3697(4) 0.6225(4) 0.0317(12) Uani 1 1 d . . .
C10 C 0.8671(5) 0.3592(4) 0.3547(4) 0.0331(12) Uani 1 1 d . . .
C11 C 0.9260(6) 0.2977(5) 0.2941(5) 0.0417(14) Uani 1 1 d . . .
C12 C 0.7810(6) 0.3988(5) 0.3001(4) 0.0392(14) Uani 1 1 d . . .
C13 C 0.5139(5) 0.8016(5) 0.8690(4) 0.0333(12) Uani 1 1 d . . .
C14 C 0.3738(6) 0.9064(5) 0.9001(5) 0.0390(13) Uani 1 1 d . . .
C15 C 0.4216(5) 0.8449(4) 0.8288(4) 0.0315(11) Uani 1 1 d . . .
C16 C 0.3795(5) 0.8267(4) 0.7203(4) 0.0311(11) Uani 1 1 d . . .
C17 C 0.2927(5) 0.8745(4) 0.6776(4) 0.0310(11) Uani 1 1 d . . .
C18 C 0.2560(5) 0.8583(4) 0.5742(4) 0.0313(11) Uani 1 1 d . . .
C19 C 0.3029(5) 0.7916(4) 0.5037(4) 0.0311(11) Uani 1 1 d . . .
C20 C 0.3878(5) 0.7425(5) 0.5462(5) 0.0351(12) Uani 1 1 d . . .
C21 C 0.4257(5) 0.7610(5) 0.6501(5) 0.0349(12) Uani 1 1 d . . .
H8 H 0.4835 0.7294 0.6755 0.042 Uiso 1 1 calc R . .
C22 C 0.2654(6) 0.7729(5) 0.3959(5) 0.0367(13) Uani 1 1 d . . .
C23 C 0.3104(6) 0.7029(5) 0.3256(5) 0.0427(14) Uani 1 1 d . . .
C24 C 0.1836(6) 0.8204(5) 0.3479(5) 0.0414(14) Uani 1 1 d . . .
C25 C 0.6715(9) 0.6746(8) 0.3764(7) 0.073(2) Uani 1 1 d . . .
C26 C 0.7504(9) 0.7382(8) 0.5559(7) 0.067(2) Uani 1 1 d . . .
C27 C 0.6660(8) 0.6610(7) 0.4710(8) 0.068(2) Uani 1 1 d . . .
C28 C 0.5840(8) 0.5790(7) 0.4861(7) 0.063(2) Uani 1 1 d . . .
C29 C 0.5877(8) 0.5738(7) 0.5835(6) 0.059(2) Uani 1 1 d . . .
H9 H 0.6462 0.6226 0.6402 0.070 Uiso 1 1 calc R . .
C30 C 0.4935(8) 0.5024(7) 0.4010(6) 0.065(2) Uani 1 1 d . . .
H10 H 0.4891 0.5037 0.3342 0.078 Uiso 1 1 calc R . .
C31 C 0.5200(6) 0.0966(5) 0.7844(5) 0.0452(15) Uani 1 1 d . . .
C32 C 0.6535(6) -0.0173(5) 0.7593(5) 0.0414(14) Uani 1 1 d . . .
C33 C 0.5703(6) 0.0315(5) 0.7154(5) 0.0395(13) Uani 1 1 d . . .
C34 C 0.5355(5) 0.0167(4) 0.6083(5) 0.0343(12) Uani 1 1 d . . .
C35 C 0.5844(6) -0.0479(5) 0.5393(5) 0.0381(13) Uani 1 1 d . . .
C36 C 0.4488(6) 0.0640(5) 0.5647(5) 0.0388(13) Uani 1 1 d . . .
C37 C 1.0975(11) 0.8097(10) 1.0325(9) 0.097(4) Uani 1 1 d . . .
H13 H 1.1410 0.8832 1.0618 0.116 Uiso 1 1 calc R . .
H14 H 1.0662 0.7948 0.9586 0.116 Uiso 1 1 calc R . .
C38 C 1.1818(9) 0.7453(14) 1.0493(11) 0.144(7) Uani 1 1 d . . .
H15 H 1.2338 0.7755 1.1184 0.215 Uiso 1 1 calc R . .
H17 H 1.2284 0.7431 1.0008 0.215 Uiso 1 1 calc R . .
H16 H 1.1384 0.6753 1.0396 0.215 Uiso 1 1 calc R . .
H2 H 0.786(5) 0.479(5) 0.489(5) 0.025(14) Uiso 1 1 d . . .
H3 H 1.024(6) 0.297(5) 0.484(5) 0.031(16) Uiso 1 1 d . . .
H4 H 1.064(7) 0.338(6) 0.658(6) 0.05(2) Uiso 1 1 d . . .
H5 H 0.260(5) 0.909(4) 0.718(4) 0.017(13) Uiso 1 1 d . . .
H6 H 0.200(6) 0.888(5) 0.539(5) 0.035(16) Uiso 1 1 d . . .
H7 H 0.418(7) 0.682(6) 0.486(7) 0.06(2) Uiso 1 1 d . . .
H11 H 0.637(7) -0.082(6) 0.566(6) 0.05(2) Uiso 1 1 d . . .
H12 H 0.425(7) 0.104(6) 0.621(6) 0.06(2) Uiso 1 1 d . . .
N1 N 0.8942(5) 0.5930(4) 0.8976(4) 0.0397(12) Uani 1 1 d . . .
N2 N 1.1507(5) 0.4024(5) 0.8960(4) 0.0446(13) Uani 1 1 d . . .
N3 N 0.7116(6) 0.4302(6) 0.2545(5) 0.0657(19) Uani 1 1 d . . .
N4 N 0.9751(7) 0.2500(6) 0.2441(5) 0.0646(18) Uani 1 1 d . . .
N5 N 0.5886(5) 0.7679(4) 0.9014(4) 0.0428(12) Uani 1 1 d . . .
N6 N 0.3328(6) 0.9563(6) 0.9573(5) 0.0605(17) Uani 1 1 d . . .
N7 N 0.3422(7) 0.6462(5) 0.2690(5) 0.0626(17) Uani 1 1 d . . .
N8 N 0.1188(6) 0.8566(6) 0.3047(5) 0.0639(18) Uani 1 1 d . . .
N9 N 0.6790(11) 0.6891(10) 0.3005(8) 0.111(3) Uani 1 1 d . . .
N10 N 0.8226(10) 0.8039(9) 0.6199(8) 0.101(3) Uani 1 1 d . . .
N11 N 0.4780(7) 0.1490(6) 0.8362(6) 0.0676(19) Uani 1 1 d . . .
N12 N 0.7194(6) -0.0603(6) 0.7913(5) 0.0589(16) Uani 1 1 d . . .
O1 O 0.9968(4) 0.7940(4) 1.0764(4) 0.0528(12) Uani 1 1 d . . .
H18 H 1.0305 0.8140 1.1410 0.063 Uiso 1 1 d R . .
O2 O 0.8132(6) 0.8057(6) 1.1871(5) 0.084(2) Uani 1 1 d . . .
H19 H 0.8093 0.8546 1.2379 0.101 Uiso 1 1 d R . .
H20 H 0.8459 0.7635 1.2112 0.101 Uiso 1 1 d R . .
O3 O 0.6004(5) 0.6733(4) 1.0609(4) 0.0527(12) Uani 1 1 d . . .
H21 H 0.6266 0.6625 1.1177 0.063 Uiso 1 1 d R . .
H22 H 0.5610 0.7193 1.0720 0.063 Uiso 1 1 d R . .
O4 O 0.8186(5) 0.9093(4) 1.0329(5) 0.0745(18) Uani 1 1 d . . .
H23 H 0.7708 0.9454 1.0159 0.089 Uiso 1 1 d R . .
H24 H 0.8853 0.9347 1.0246 0.089 Uiso 1 1 d R . .
O5 O 0.6454(5) 0.5474(4) 0.8793(4) 0.0625(15) Uani 1 1 d . . .
H25 H 0.5918 0.5708 0.8484 0.075 Uiso 1 1 d R . .
H26 H 0.6572 0.4972 0.8343 0.075 Uiso 1 1 d R . .
O6 O 0.8094(6) 0.7576(5) 0.8361(5) 0.0685(16) Uani 1 1 d . . .
H27 H 0.8462 0.7392 0.7909 0.082 Uiso 1 1 d R . .
H28 H 0.7625 0.7922 0.8145 0.082 Uiso 1 1 d R . .
O7 O 0.4238(5) 0.5234(5) 0.8997(5) 0.0778(19) Uani 1 1 d . . .
H29 H 0.4307 0.4605 0.8851 0.093 Uiso 1 1 d R . .
H30 H 0.4933 0.5639 0.9166 0.093 Uiso 1 1 d R . .
O8 O 0.9932(10) 0.0241(8) 0.2105(12) 0.106(6) Uani 0.50 1 d P . .
H31 H 0.9348 -0.0132 0.1586 0.127 Uiso 0.50 1 d PR . .
H32 H 1.0294 -0.0172 0.2326 0.127 Uiso 0.50 1 d PR . .
Pr1 Pr 0.77981(3) 0.71715(2) 0.99413(2) 0.02962(13) Uani 1 1 d . . .


_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 N1 1.133(7) . ?
C1 C3 1.423(8) . ?
C2 N2 1.147(8) . ?
C2 C3 1.408(8) . ?
C3 C4 1.429(7) . ?
C4 C9 1.414(8) . ?
C4 C5 1.418(7) . ?
C5 C6 1.363(8) . ?
C5 H1 0.9300 . ?
C6 C7 1.422(8) . ?
C6 H2 0.92(6) . ?
C7 C8 1.420(8) . ?
C7 C10 1.422(8) . ?
C8 C9 1.369(8) . ?
C8 H3 0.95(7) . ?
C9 H4 0.94(8) . ?
C10 C11 1.411(9) . ?
C10 C12 1.415(9) . ?
C11 N4 1.147(9) . ?
C12 N3 1.148(9) . ?
C13 N5 1.134(7) . ?
C13 C15 1.417(8) . ?
C14 N6 1.154(9) . ?
C14 C15 1.407(8) . ?
C15 C16 1.428(8) . ?
C16 C21 1.414(8) . ?
C16 C17 1.425(8) . ?
C17 C18 1.361(8) . ?
C17 H5 0.84(6) . ?
C18 C19 1.429(8) . ?
C18 H6 0.95(7) . ?
C19 C22 1.414(8) . ?
C19 C20 1.419(8) . ?
C20 C21 1.363(8) . ?
C20 H7 1.17(9) . ?
C21 H8 0.9300 . ?
C22 C24 1.412(9) . ?
C22 C23 1.435(9) . ?
C23 N7 1.127(9) . ?
C24 N8 1.139(9) . ?
C25 N9 1.150(13) . ?
C25 C27 1.400(13) . ?
C26 N10 1.139(13) . ?
C26 C27 1.398(14) . ?
C27 C28 1.438(13) . ?
C28 C29 1.376(12) . ?
C28 C30 1.427(12) . ?
C29 C30 1.382(13) 2_666 ?
C29 H9 0.9300 . ?
C30 C29 1.382(13) 2_666 ?
C30 H10 0.9300 . ?
C31 N11 1.134(9) . ?
C31 C33 1.431(9) . ?
C32 N12 1.145(9) . ?
C32 C33 1.410(9) . ?
C33 C34 1.414(9) . ?
C34 C35 1.417(9) . ?
C34 C36 1.423(8) . ?
C35 C36 1.367(9) 2_656 ?
C35 H11 0.92(8) . ?
C36 C35 1.367(9) 2_656 ?
C36 H12 0.96(8) . ?
C37 O1 1.465(14) . ?
C37 C38 1.466(18) . ?
C37 H13 0.9700 . ?
C37 H14 0.9700 . ?
C38 H15 0.9600 . ?
C38 H17 0.9600 . ?
C38 H16 0.9600 . ?
N1 Pr1 2.628(5) . ?
N2 Pr1 2.646(5) 2_767 ?
N5 Pr1 2.660(5) . ?
O1 Pr1 2.478(5) . ?
O1 H18 0.8503 . ?
O2 Pr1 2.552(6) . ?
O2 H19 0.8481 . ?
O2 H20 0.8512 . ?
O3 Pr1 2.541(5) . ?
O3 H21 0.8497 . ?
O3 H22 0.8490 . ?
O4 Pr1 2.465(5) . ?
O4 H23 0.8518 . ?
O4 H24 0.8490 . ?
O5 Pr1 2.459(5) . ?
O5 H25 0.8496 . ?
O5 H26 0.8499 . ?
O6 Pr1 2.500(5) . ?
O6 H27 0.8519 . ?
O6 H28 0.8500 . ?
O7 H29 0.8499 . ?
O7 H30 0.8500 . ?
O8 H31 0.8500 . ?
O8 H32 0.8501 . ?
Pr1 N2 2.646(5) 2_767 ?

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
N1 C1 C3 178.3(6) . . ?
N2 C2 C3 179.2(6) . . ?
C2 C3 C1 116.0(5) . . ?
C2 C3 C4 123.2(5) . . ?
C1 C3 C4 120.9(5) . . ?
C9 C4 C5 117.4(5) . . ?
C9 C4 C3 121.4(5) . . ?
C5 C4 C3 121.2(5) . . ?
C6 C5 C4 121.6(5) . . ?
C6 C5 H1 119.2 . . ?
C4 C5 H1 119.2 . . ?
C5 C6 C7 121.0(5) . . ?
C5 C6 H2 122(4) . . ?
C7 C6 H2 117(4) . . ?
C8 C7 C10 120.9(5) . . ?
C8 C7 C6 117.6(5) . . ?
C10 C7 C6 121.5(5) . . ?
C9 C8 C7 120.9(5) . . ?
C9 C8 H3 115(4) . . ?
C7 C8 H3 124(4) . . ?
C8 C9 C4 121.5(5) . . ?
C8 C9 H4 121(5) . . ?
C4 C9 H4 117(5) . . ?
C11 C10 C12 115.5(5) . . ?
C11 C10 C7 122.5(5) . . ?
C12 C10 C7 121.9(5) . . ?
N4 C11 C10 178.1(8) . . ?
N3 C12 C10 179.0(8) . . ?
N5 C13 C15 179.3(7) . . ?
N6 C14 C15 178.8(7) . . ?
C14 C15 C13 117.2(5) . . ?
C14 C15 C16 121.7(5) . . ?
C13 C15 C16 121.0(5) . . ?
C21 C16 C17 116.8(5) . . ?
C21 C16 C15 120.5(5) . . ?
C17 C16 C15 122.7(5) . . ?
C18 C17 C16 121.8(5) . . ?
C18 C17 H5 120(4) . . ?
C16 C17 H5 118(4) . . ?
C17 C18 C19 121.0(5) . . ?
C17 C18 H6 128(4) . . ?
C19 C18 H6 111(4) . . ?
C22 C19 C20 120.9(5) . . ?
C22 C19 C18 122.1(5) . . ?
C20 C19 C18 117.1(5) . . ?
C21 C20 C19 121.4(5) . . ?
C21 C20 H7 123(4) . . ?
C19 C20 H7 116(4) . . ?
C20 C21 C16 121.9(5) . . ?
C20 C21 H8 119.1 . . ?
C16 C21 H8 119.1 . . ?
C24 C22 C19 124.3(6) . . ?
C24 C22 C23 114.2(5) . . ?
C19 C22 C23 121.5(6) . . ?
N7 C23 C22 177.9(8) . . ?
N8 C24 C22 176.6(8) . . ?
N9 C25 C27 177.5(13) . . ?
N10 C26 C27 174.8(12) . . ?
C26 C27 C25 113.2(9) . . ?
C26 C27 C28 120.2(9) . . ?
C25 C27 C28 126.6(9) . . ?
C29 C28 C30 117.6(9) . . ?
C29 C28 C27 121.2(9) . . ?
C30 C28 C27 121.2(8) . . ?
C28 C29 C30 121.5(8) . 2_666 ?
C28 C29 H9 119.2 . . ?
C30 C29 H9 119.2 2_666 . ?
C29 C30 C28 120.8(8) 2_666 . ?
C29 C30 H10 119.6 2_666 . ?
C28 C30 H10 119.6 . . ?
N11 C31 C33 177.7(8) . . ?
N12 C32 C33 177.2(8) . . ?
C32 C33 C34 122.4(6) . . ?
C32 C33 C31 116.9(6) . . ?
C34 C33 C31 120.6(6) . . ?
C33 C34 C35 121.1(5) . . ?
C33 C34 C36 121.8(6) . . ?
C35 C34 C36 117.1(6) . . ?
C36 C35 C34 121.9(6) 2_656 . ?
C36 C35 H11 120(5) 2_656 . ?
C34 C35 H11 118(5) . . ?
C35 C36 C34 120.9(6) 2_656 . ?
C35 C36 H12 132(5) 2_656 . ?
C34 C36 H12 107(5) . . ?
O1 C37 C38 115.4(11) . . ?
O1 C37 H13 108.4 . . ?
C38 C37 H13 108.4 . . ?
O1 C37 H14 108.4 . . ?
C38 C37 H14 108.4 . . ?
H13 C37 H14 107.5 . . ?
C37 C38 H15 109.5 . . ?
C37 C38 H17 109.5 . . ?
H15 C38 H17 109.5 . . ?
C37 C38 H16 109.5 . . ?
H15 C38 H16 109.5 . . ?
H17 C38 H16 109.5 . . ?
C1 N1 Pr1 176.4(5) . . ?
C2 N2 Pr1 153.0(5) . 2_767 ?
C13 N5 Pr1 171.8(5) . . ?
C37 O1 Pr1 131.8(5) . . ?
C37 O1 H18 103.1 . . ?
Pr1 O1 H18 125.0 . . ?
Pr1 O2 H19 152.1 . . ?
Pr1 O2 H20 100.1 . . ?
H19 O2 H20 107.8 . . ?
Pr1 O3 H21 106.6 . . ?
Pr1 O3 H22 117.0 . . ?
H21 O3 H22 107.8 . . ?
Pr1 O4 H23 128.8 . . ?
Pr1 O4 H24 111.3 . . ?
H23 O4 H24 107.6 . . ?
Pr1 O5 H25 98.0 . . ?
Pr1 O5 H26 131.2 . . ?
H25 O5 H26 107.8 . . ?
Pr1 O6 H27 138.2 . . ?
Pr1 O6 H28 113.5 . . ?
H27 O6 H28 107.5 . . ?
H29 O7 H30 107.7 . . ?
H31 O8 H32 107.7 . . ?
O5 Pr1 O4 144.21(19) . . ?
O5 Pr1 O1 138.24(17) . . ?
O4 Pr1 O1 72.08(18) . . ?
O5 Pr1 O6 87.9(2) . . ?
O4 Pr1 O6 72.3(2) . . ?
O1 Pr1 O6 88.0(2) . . ?
O5 Pr1 O3 70.05(18) . . ?
O4 Pr1 O3 103.1(2) . . ?
O1 Pr1 O3 134.50(17) . . ?
O6 Pr1 O3 134.88(18) . . ?
O5 Pr1 O2 129.3(2) . . ?
O4 Pr1 O2 70.3(2) . . ?
O1 Pr1 O2 71.4(2) . . ?
O6 Pr1 O2 141.3(2) . . ?
O3 Pr1 O2 64.9(2) . . ?
O5 Pr1 N1 67.83(17) . . ?
O4 Pr1 N1 126.7(2) . . ?
O1 Pr1 N1 72.10(17) . . ?
O6 Pr1 N1 68.26(17) . . ?
O3 Pr1 N1 130.18(17) . . ?
O2 Pr1 N1 130.2(2) . . ?
O5 Pr1 N2 81.6(2) . 2_767 ?
O4 Pr1 N2 132.7(2) . 2_767 ?
O1 Pr1 N2 74.22(18) . 2_767 ?
O6 Pr1 N2 138.14(17) . 2_767 ?
O3 Pr1 N2 78.52(17) . 2_767 ?
O2 Pr1 N2 68.1(2) . 2_767 ?
N1 Pr1 N2 70.25(16) . 2_767 ?
O5 Pr1 N5 75.84(18) . . ?
O4 Pr1 N5 69.53(18) . . ?
O1 Pr1 N5 139.99(18) . . ?
O6 Pr1 N5 70.08(18) . . ?
O3 Pr1 N5 66.62(17) . . ?
O2 Pr1 N5 105.1(2) . . ?
N1 Pr1 N5 124.62(16) . . ?
N2 Pr1 N5 143.19(18) 2_767 . ?

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
O8 H32 N8 0.85 2.50 3.346(14) 174.2 1_645
O8 H31 O4 0.85 1.88 2.724(11) 172.3 1_544
O7 H30 O3 0.85 2.12 2.755(8) 131.0 .
O7 H30 O5 0.85 2.01 2.674(8) 133.7 .
O7 H29 O3 0.85 2.16 2.862(8) 139.6 2_667
O6 H28 N12 0.85 2.25 3.036(8) 153.4 1_565
O6 H27 N4 0.85 2.26 3.010(9) 146.5 2_766
O5 H26 N7 0.85 2.10 2.934(8) 167.9 2_666
O5 H25 N5 0.85 2.60 3.150(7) 123.6 .
O4 H23 N6 0.85 1.99 2.784(8) 154.5 2_677
O3 H22 N11 0.85 2.10 2.884(8) 153.9 2_667
O3 H21 O7 0.85 2.43 2.862(8) 112.0 2_667
O3 H21 N9 0.85 2.41 3.217(11) 159.3 1_556
O2 H20 N2 0.85 2.37 2.909(9) 122.1 2_767
O1 H18 N8 0.85 2.17 3.019(8) 176.8 1_656

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        26.10
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         2.868
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.164
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zjw-1
_audit_block_doi                 10.5517/ccnzhfj
_database_code_depnum_ccdc_archive 'CCDC 625128'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/b909213g 2009
_audit_update_record             
;
2006-10-24 deposited with the CCDC.
2015-08-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C52 H48 La2 N16 O12, 2(C12 H4 N4), 4(H2 O), H2 O'
_chemical_formula_sum            'C76 H66 La2 N24 O17'
_chemical_formula_weight         1865.35

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           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                   11.8868(14)
_cell_length_b                   13.6725(15)
_cell_length_c                   14.0053(16)
_cell_angle_alpha                105.727(2)
_cell_angle_beta                 102.179(2)
_cell_angle_gamma                100.520(2)
_cell_volume                     2070.9(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3953
_cell_measurement_theta_min      6.15
_cell_measurement_theta_max      51.47

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             940
_exptl_absorpt_coefficient_mu    1.098
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6920
_exptl_absorpt_correction_T_max  0.7934
_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       'ω 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            11600
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         26.06
_reflns_number_total             7981
_reflns_number_gt                6790
_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          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0837P)²+2.6806P] where P=(Fo²+2Fc²)/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         7981
_refine_ls_number_parameters     542
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1485
_refine_ls_wR_factor_gt          0.1400
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.005
_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 0.4388(5) 0.0360(4) 0.8508(4) 0.0328(12) Uani 1 1 d . . .
C2 C 0.5793(5) -0.0694(4) 0.8475(4) 0.0336(12) Uani 1 1 d . . .
C3 C 0.4918(5) -0.0332(4) 0.7916(4) 0.0325(11) Uani 1 1 d . . .
C4 C 0.4577(4) -0.0625(4) 0.6811(4) 0.0286(10) Uani 1 1 d . . .
C5 C 0.3704(4) -0.0239(4) 0.6282(4) 0.0300(11) Uani 1 1 d . . .
H1 H 0.3326 0.0200 0.6656 0.036 Uiso 1 1 calc R . .
C6 C 0.3404(5) -0.0494(4) 0.5233(4) 0.0316(11) Uani 1 1 d . . .
H2 H 0.2824 -0.0227 0.4908 0.038 Uiso 1 1 calc R . .
C7 C 0.3956(5) -0.1159(4) 0.4629(4) 0.0306(11) Uani 1 1 d . . .
C8 C 0.4817(5) -0.1562(4) 0.5157(4) 0.0350(12) Uani 1 1 d . . .
H3 H 0.5186 -0.2010 0.4781 0.042 Uiso 1 1 calc R . .
C9 C 0.5117(5) -0.1304(4) 0.6208(4) 0.0324(11) Uani 1 1 d . . .
H4 H 0.5688 -0.1579 0.6533 0.039 Uiso 1 1 calc R . .
C10 C 0.3656(5) -0.1404(4) 0.3542(4) 0.0340(12) Uani 1 1 d . . .
C11 C 0.4246(5) -0.2018(5) 0.2930(4) 0.0419(14) Uani 1 1 d . . .
C12 C 0.2809(5) -0.1007(5) 0.3006(4) 0.0419(14) Uani 1 1 d . . .
C13 C 0.0135(5) 0.3026(4) 0.8681(4) 0.0347(12) Uani 1 1 d . . .
C14 C -0.1259(5) 0.4070(5) 0.9000(4) 0.0407(13) Uani 1 1 d . . .
C15 C -0.0788(5) 0.3451(4) 0.8276(4) 0.0332(11) Uani 1 1 d . . .
C16 C -0.1201(5) 0.3268(4) 0.7198(4) 0.0314(11) Uani 1 1 d . . .
C17 C -0.2067(5) 0.3750(4) 0.6786(4) 0.0325(11) Uani 1 1 d . . .
H5 H -0.2386 0.4185 0.7230 0.039 Uiso 1 1 calc R . .
C18 C -0.2440(5) 0.3584(4) 0.5742(4) 0.0341(12) Uani 1 1 d . . .
H6 H -0.3004 0.3909 0.5493 0.041 Uiso 1 1 calc R . .
C19 C -0.1976(5) 0.2922(4) 0.5041(4) 0.0335(11) Uani 1 1 d . . .
C20 C -0.1120(5) 0.2440(4) 0.5462(4) 0.0372(12) Uani 1 1 d . . .
H7 H -0.0812 0.1991 0.5021 0.045 Uiso 1 1 calc R . .
C21 C -0.0741(5) 0.2617(4) 0.6496(4) 0.0352(12) Uani 1 1 d . . .
H8 H -0.0165 0.2302 0.6744 0.042 Uiso 1 1 calc R . .
C22 C -0.2343(5) 0.2735(4) 0.3968(4) 0.0373(12) Uani 1 1 d . . .
C23 C -0.1895(5) 0.2036(5) 0.3269(4) 0.0420(13) Uani 1 1 d . . .
C24 C -0.3153(6) 0.3208(5) 0.3497(4) 0.0434(14) Uani 1 1 d . . .
C25 C 0.1696(8) 0.1746(7) 0.3751(6) 0.070(2) Uani 1 1 d . . .
C26 C 0.2517(7) 0.2389(7) 0.5565(6) 0.063(2) Uani 1 1 d . . .
C27 C 0.1645(7) 0.1607(6) 0.4714(6) 0.0603(18) Uani 1 1 d . . .
C28 C 0.0834(6) 0.0799(6) 0.4860(5) 0.0582(18) Uani 1 1 d . . .
C29 C 0.0874(7) 0.0728(6) 0.5838(5) 0.0570(18) Uani 1 1 d . . .
H9 H 0.1462 0.1208 0.6404 0.068 Uiso 1 1 calc R . .
C30 C -0.0072(7) 0.0028(6) 0.4010(5) 0.0613(19) Uani 1 1 d . . .
H10 H -0.0115 0.0042 0.3343 0.074 Uiso 1 1 calc R . .
C31 C 0.0206(6) 0.5964(5) 0.7831(5) 0.0458(14) Uani 1 1 d . . .
C32 C 0.1531(5) 0.4823(5) 0.7576(4) 0.0428(14) Uani 1 1 d . . .
C33 C 0.0703(5) 0.5319(5) 0.7146(5) 0.0398(13) Uani 1 1 d . . .
C34 C 0.0356(5) 0.5168(4) 0.6075(5) 0.0384(13) Uani 1 1 d . . .
C35 C 0.0844(5) 0.4520(5) 0.5385(4) 0.0403(13) Uani 1 1 d . . .
H11 H 0.1407 0.4197 0.5642 0.048 Uiso 1 1 calc R . .
C36 C -0.0498(5) 0.5637(4) 0.5651(5) 0.0404(13) Uani 1 1 d . . .
H12 H -0.0834 0.6063 0.6085 0.048 Uiso 1 1 calc R . .
C37 C 0.6001(11) 0.3072(9) 1.0329(8) 0.113(4) Uani 1 1 d . . .
H13 H 0.6448 0.3803 1.0603 0.136 Uiso 1 1 calc R . .
H14 H 0.5674 0.2914 0.9593 0.136 Uiso 1 1 calc R . .
C38 C 0.6843(9) 0.2422(13) 1.0482(10) 0.151(6) Uani 1 1 d . . .
H15 H 0.7416 0.2756 1.1143 0.227 Uiso 1 1 calc R . .
H17 H 0.7245 0.2344 0.9950 0.227 Uiso 1 1 calc R . .
H16 H 0.6415 0.1742 1.0453 0.227 Uiso 1 1 calc R . .
La1 La 0.28029(3) 0.21850(2) 0.99503(2) 0.03091(12) Uani 1 1 d . . .
N1 N -0.1676(6) 0.4554(5) 0.9568(5) 0.0634(16) Uani 1 1 d . . .
N2 N 0.0888(4) 0.2693(4) 0.9000(4) 0.0450(12) Uani 1 1 d . . .
N3 N 0.6502(5) -0.0982(4) 0.8931(4) 0.0470(13) Uani 1 1 d . . .
N4 N 0.4729(6) -0.2504(5) 0.2427(4) 0.0632(16) Uani 1 1 d . . .
N5 N 0.2119(5) -0.0691(5) 0.2557(5) 0.0649(17) Uani 1 1 d . . .
N6 N -0.1575(6) 0.1476(5) 0.2694(5) 0.0627(16) Uani 1 1 d . . .
N7 N -0.3815(6) 0.3568(5) 0.3074(5) 0.0659(17) Uani 1 1 d . . .
N8 N 0.3237(8) 0.3035(7) 0.6200(6) 0.096(2) Uani 1 1 d . . .
N9 N 0.1780(9) 0.1908(8) 0.3010(6) 0.108(3) Uani 1 1 d . . .
N10 N 0.3955(4) 0.0930(4) 0.8974(3) 0.0414(11) Uani 1 1 d . . .
N11 N 0.2192(5) 0.4399(5) 0.7894(4) 0.0611(15) Uani 1 1 d . . .
N12 N -0.0195(6) 0.6495(5) 0.8366(5) 0.0685(17) Uani 1 1 d . . .
O1 O 0.5000(4) 0.2960(4) 1.0792(4) 0.0566(12) Uani 1 1 d . . .
H18 H 0.5140 0.3098 1.1442 0.068 Uiso 1 1 d R . .
O2 O 0.3115(6) 0.3076(5) 1.1888(4) 0.0858(18) Uani 1 1 d . . .
H19 H 0.3154 0.3729 1.2076 0.103 Uiso 1 1 d R . .
H20 H 0.3305 0.2905 1.2429 0.103 Uiso 1 1 d R . .
O3 O 0.0968(4) 0.1726(4) 1.0604(3) 0.0531(11) Uani 1 1 d . . .
H21 H 0.1310 0.1692 1.1187 0.064 Uiso 1 1 d R . .
H22 H 0.0705 0.2273 1.0711 0.064 Uiso 1 1 d R . .
O4 O 0.3220(5) 0.4133(4) 1.0334(4) 0.0764(16) Uani 1 1 d . . .
H24 H 0.3859 0.4548 1.0357 0.092 Uiso 1 1 d R . .
H23 H 0.2644 0.4376 1.0117 0.092 Uiso 1 1 d R . .
O5 O 0.1436(4) 0.0447(4) 0.8784(4) 0.0629(13) Uani 1 1 d . . .
H25 H 0.0968 0.0707 0.8439 0.075 Uiso 1 1 d R . .
H26 H 0.1701 0.0038 0.8363 0.075 Uiso 1 1 d R . .
O6 O 0.3126(5) 0.2604(4) 0.8350(4) 0.0684(15) Uani 1 1 d . . .
H28 H 0.2676 0.2745 0.7875 0.082 Uiso 1 1 d R . .
H27 H 0.3522 0.2209 0.8070 0.082 Uiso 1 1 d R . .
O7 O 0.9241(4) 0.0238(5) 0.8991(4) 0.0764(16) Uani 1 1 d . . .
H29 H 0.8984 -0.0423 0.8890 0.092 Uiso 1 1 d R . .
H30 H 1.0000 0.0347 0.9083 0.092 Uiso 1 1 d R . .
O8 O 0.4515(14) 0.4595(12) 0.4650(17) 0.157(8) Uani 0.50 1 d P . 1
H31 H 0.3808 0.4207 0.4439 0.188 Uiso 0.50 1 d PR . 1
H32 H 0.4845 0.4434 0.4167 0.188 Uiso 0.50 1 d PR . 1
O9 O 0.4917(9) 0.5223(6) 0.2175(11) 0.264(9) Uani 1 1 d . . .
H34 H 0.5617 0.5226 0.2480 0.317 Uiso 1 1 d R . .
H33 H 0.4895 0.5858 0.2258 0.317 Uiso 1 1 d R . .


_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 N10 1.144(7) . ?
C1 C3 1.411(7) . ?
C2 N3 1.142(7) . ?
C2 C3 1.412(7) . ?
C3 C4 1.436(7) . ?
C4 C5 1.411(7) . ?
C4 C9 1.418(7) . ?
C5 C6 1.365(7) . ?
C5 H1 0.9300 . ?
C6 C7 1.417(7) . ?
C6 H2 0.9300 . ?
C7 C8 1.416(7) . ?
C7 C10 1.417(7) . ?
C8 C9 1.367(7) . ?
C8 H3 0.9300 . ?
C9 H4 0.9300 . ?
C10 C12 1.405(8) . ?
C10 C11 1.419(8) . ?
C11 N4 1.149(8) . ?
C12 N5 1.146(8) . ?
C13 N2 1.139(7) . ?
C13 C15 1.420(7) . ?
C14 N1 1.148(8) . ?
C14 C15 1.416(8) . ?
C15 C16 1.421(7) . ?
C16 C21 1.410(7) . ?
C16 C17 1.426(7) . ?
C17 C18 1.376(7) . ?
C17 H5 0.9300 . ?
C18 C19 1.421(8) . ?
C18 H6 0.9300 . ?
C19 C22 1.410(7) . ?
C19 C20 1.421(7) . ?
C20 C21 1.360(7) . ?
C20 H7 0.9300 . ?
C21 H8 0.9300 . ?
C22 C24 1.403(8) . ?
C22 C23 1.433(8) . ?
C23 N6 1.132(8) . ?
C24 N7 1.146(8) . ?
C25 N9 1.138(10) . ?
C25 C27 1.424(11) . ?
C26 N8 1.132(11) . ?
C26 C27 1.422(11) . ?
C27 C28 1.417(11) . ?
C28 C29 1.391(10) . ?
C28 C30 1.433(10) . ?
C29 C30 1.367(11) 2_556 ?
C29 H9 0.9300 . ?
C30 C29 1.367(11) 2_556 ?
C30 H10 0.9300 . ?
C31 N12 1.140(8) . ?
C31 C33 1.420(9) . ?
C32 N11 1.145(8) . ?
C32 C33 1.416(8) . ?
C33 C34 1.414(8) . ?
C34 C36 1.409(8) . ?
C34 C35 1.420(8) . ?
C35 C36 1.367(8) 2_566 ?
C35 H11 0.9300 . ?
C36 C35 1.367(8) 2_566 ?
C36 H12 0.9300 . ?
C37 O1 1.474(14) . ?
C37 C38 1.475(17) . ?
C37 H13 0.9700 . ?
C37 H14 0.9700 . ?
C38 H15 0.9600 . ?
C38 H17 0.9600 . ?
C38 H16 0.9600 . ?
La1 O4 2.501(5) . ?
La1 O5 2.514(5) . ?
La1 O1 2.520(5) . ?
La1 O6 2.546(4) . ?
La1 O2 2.569(5) . ?
La1 O3 2.577(4) . ?
La1 N10 2.659(5) . ?
La1 N3 2.681(5) 2_657 ?
La1 N2 2.690(5) . ?
N3 La1 2.681(5) 2_657 ?
O1 H18 0.8501 . ?
O2 H19 0.8499 . ?
O2 H20 0.8500 . ?
O3 H21 0.8500 . ?
O3 H22 0.8500 . ?
O4 H24 0.8500 . ?
O4 H23 0.8499 . ?
O5 H25 0.8501 . ?
O5 H26 0.8500 . ?
O6 H28 0.8500 . ?
O6 H27 0.8499 . ?
O7 H29 0.8606 . ?
O7 H30 0.8623 . ?
O8 O8 1.41(3) 2_666 ?
O8 H31 0.8500 . ?
O8 H32 0.8500 . ?
O9 H34 0.8500 . ?
O9 H33 0.8501 . ?

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
N10 C1 C3 178.7(6) . . ?
N3 C2 C3 179.6(6) . . ?
C1 C3 C2 116.2(4) . . ?
C1 C3 C4 120.6(4) . . ?
C2 C3 C4 123.2(5) . . ?
C5 C4 C9 117.3(4) . . ?
C5 C4 C3 121.5(5) . . ?
C9 C4 C3 121.2(4) . . ?
C6 C5 C4 121.5(5) . . ?
C6 C5 H1 119.2 . . ?
C4 C5 H1 119.2 . . ?
C5 C6 C7 121.3(5) . . ?
C5 C6 H2 119.3 . . ?
C7 C6 H2 119.3 . . ?
C8 C7 C10 121.7(5) . . ?
C8 C7 C6 117.3(4) . . ?
C10 C7 C6 121.0(5) . . ?
C9 C8 C7 121.3(5) . . ?
C9 C8 H3 119.4 . . ?
C7 C8 H3 119.4 . . ?
C8 C9 C4 121.3(5) . . ?
C8 C9 H4 119.3 . . ?
C4 C9 H4 119.3 . . ?
C12 C10 C7 122.5(5) . . ?
C12 C10 C11 115.5(5) . . ?
C7 C10 C11 121.9(5) . . ?
N4 C11 C10 179.0(7) . . ?
N5 C12 C10 179.2(7) . . ?
N2 C13 C15 178.9(6) . . ?
N1 C14 C15 177.8(7) . . ?
C14 C15 C13 116.6(5) . . ?
C14 C15 C16 122.3(5) . . ?
C13 C15 C16 121.1(5) . . ?
C21 C16 C15 120.8(5) . . ?
C21 C16 C17 117.4(5) . . ?
C15 C16 C17 121.7(5) . . ?
C18 C17 C16 121.2(5) . . ?
C18 C17 H5 119.4 . . ?
C16 C17 H5 119.4 . . ?
C17 C18 C19 121.0(5) . . ?
C17 C18 H6 119.5 . . ?
C19 C18 H6 119.5 . . ?
C22 C19 C18 122.2(5) . . ?
C22 C19 C20 120.6(5) . . ?
C18 C19 C20 117.2(5) . . ?
C21 C20 C19 121.7(5) . . ?
C21 C20 H7 119.2 . . ?
C19 C20 H7 119.2 . . ?
C20 C21 C16 121.6(5) . . ?
C20 C21 H8 119.2 . . ?
C16 C21 H8 119.2 . . ?
C24 C22 C19 123.9(5) . . ?
C24 C22 C23 114.7(5) . . ?
C19 C22 C23 121.4(5) . . ?
N6 C23 C22 177.7(7) . . ?
N7 C24 C22 177.2(7) . . ?
N9 C25 C27 176.2(11) . . ?
N8 C26 C27 175.8(10) . . ?
C28 C27 C26 121.2(7) . . ?
C28 C27 C25 126.1(7) . . ?
C26 C27 C25 112.7(7) . . ?
C29 C28 C27 121.4(7) . . ?
C29 C28 C30 117.0(7) . . ?
C27 C28 C30 121.6(7) . . ?
C30 C29 C28 121.8(7) 2_556 . ?
C30 C29 H9 119.1 2_556 . ?
C28 C29 H9 119.1 . . ?
C29 C30 C28 121.1(7) 2_556 . ?
C29 C30 H10 119.4 2_556 . ?
C28 C30 H10 119.4 . . ?
N12 C31 C33 178.4(7) . . ?
N11 C32 C33 177.8(7) . . ?
C34 C33 C32 122.0(5) . . ?
C34 C33 C31 120.6(5) . . ?
C32 C33 C31 117.4(5) . . ?
C36 C34 C33 121.6(5) . . ?
C36 C34 C35 117.5(5) . . ?
C33 C34 C35 120.9(5) . . ?
C36 C35 C34 121.0(5) 2_566 . ?
C36 C35 H11 119.5 2_566 . ?
C34 C35 H11 119.5 . . ?
C35 C36 C34 121.6(5) 2_566 . ?
C35 C36 H12 119.2 2_566 . ?
C34 C36 H12 119.2 . . ?
O1 C37 C38 117.3(10) . . ?
O1 C37 H13 108.0 . . ?
C38 C37 H13 108.0 . . ?
O1 C37 H14 108.0 . . ?
C38 C37 H14 108.0 . . ?
H13 C37 H14 107.2 . . ?
C37 C38 H15 109.5 . . ?
C37 C38 H17 109.5 . . ?
H15 C38 H17 109.5 . . ?
C37 C38 H16 109.5 . . ?
H15 C38 H16 109.5 . . ?
H17 C38 H16 109.5 . . ?
O4 La1 O5 144.61(17) . . ?
O4 La1 O1 71.87(16) . . ?
O5 La1 O1 138.00(15) . . ?
O4 La1 O6 71.68(19) . . ?
O5 La1 O6 88.35(18) . . ?
O1 La1 O6 88.02(17) . . ?
O4 La1 O2 70.6(2) . . ?
O5 La1 O2 128.96(19) . . ?
O1 La1 O2 71.53(18) . . ?
O6 La1 O2 141.1(2) . . ?
O4 La1 O3 104.02(18) . . ?
O5 La1 O3 69.38(16) . . ?
O1 La1 O3 134.94(15) . . ?
O6 La1 O3 134.59(15) . . ?
O2 La1 O3 65.25(18) . . ?
O4 La1 N10 126.02(18) . . ?
O5 La1 N10 67.72(15) . . ?
O1 La1 N10 72.15(15) . . ?
O6 La1 N10 68.21(15) . . ?
O2 La1 N10 130.58(17) . . ?
O3 La1 N10 129.84(15) . . ?
O4 La1 N3 132.50(17) . 2_657 ?
O5 La1 N3 81.63(17) . 2_657 ?
O1 La1 N3 73.72(17) . 2_657 ?
O6 La1 N3 138.17(15) . 2_657 ?
O2 La1 N3 68.03(18) . 2_657 ?
O3 La1 N3 78.85(15) . 2_657 ?
N10 La1 N3 70.41(15) . 2_657 ?
O4 La1 N2 69.95(16) . . ?
O5 La1 N2 75.89(16) . . ?
O1 La1 N2 140.22(16) . . ?
O6 La1 N2 69.85(16) . . ?
O2 La1 N2 105.24(18) . . ?
O3 La1 N2 66.59(15) . . ?
N10 La1 N2 124.10(15) . . ?
N3 La1 N2 143.57(17) 2_657 . ?
C13 N2 La1 171.8(5) . . ?
C2 N3 La1 152.7(5) . 2_657 ?
C1 N10 La1 175.9(4) . . ?
C37 O1 La1 130.3(5) . . ?
C37 O1 H18 119.6 . . ?
La1 O1 H18 109.6 . . ?
La1 O2 H19 116.1 . . ?
La1 O2 H20 135.4 . . ?
H19 O2 H20 107.7 . . ?
La1 O3 H21 99.6 . . ?
La1 O3 H22 105.4 . . ?
H21 O3 H22 107.7 . . ?
La1 O4 H24 127.4 . . ?
La1 O4 H23 117.0 . . ?
H24 O4 H23 107.7 . . ?
La1 O5 H25 95.4 . . ?
La1 O5 H26 118.8 . . ?
H25 O5 H26 107.7 . . ?
La1 O6 H28 132.4 . . ?
La1 O6 H27 109.6 . . ?
H28 O6 H27 107.7 . . ?
H29 O7 H30 105.6 . . ?
O8 O8 H31 155.4 2_666 . ?
O8 O8 H32 96.8 2_666 . ?
H31 O8 H32 107.7 . . ?
H34 O9 H33 107.7 . . ?

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
O1 H18 N7 0.85 2.21 3.021(8) 158.6 1_656
O2 H19 O9 0.85 2.60 3.173(13) 126.1 1_556
O2 H20 N9 0.85 2.48 3.005(11) 121.1 1_556
O3 H21 N9 0.85 2.42 3.231(9) 160.2 1_556
O3 H22 N12 0.85 2.10 2.883(8) 153.5 2_567
O4 H23 N1 0.85 2.03 2.791(8) 147.9 2_567
O5 H25 N2 0.85 2.64 3.203(7) 124.9 .
O5 H26 N6 0.85 2.15 2.928(7) 151.7 2_556
O6 H28 N11 0.85 2.43 3.034(7) 128.9 .
O6 H28 N8 0.85 2.68 3.245(10) 125.4 .
O6 H27 N4 0.85 2.33 2.987(8) 134.4 2_656
O6 H27 N10 0.85 2.49 2.919(7) 112.5 .
O7 H29 O3 0.86 2.09 2.870(7) 149.6 2_657
O7 H30 O5 0.86 1.83 2.658(7) 159.8 1_655
O8 H32 N7 0.85 2.65 3.459(18) 159.9 1_655
O9 H34 N8 0.85 2.51 2.952(11) 113.3 2_666
O9 H33 N4 0.85 2.24 3.086(11) 176.8 1_565

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        26.06
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.916
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.132
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zjw-4
_audit_block_doi                 10.5517/ccnzhgk
_database_code_depnum_ccdc_archive 'CCDC 625129'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/b909213g 2009
_audit_update_record             
;
2006-10-24 deposited with the CCDC.
2015-08-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C48 H36 Dy2 N16 O10, 2(C12 H4 N4), 4(H2 O), H4 O'
_chemical_formula_sum            'C72 H56 Dy2 N24 O15'
_chemical_formula_weight         1822.41

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.824(2)
_cell_length_b                   13.307(3)
_cell_length_c                   13.760(3)
_cell_angle_alpha                106.16(3)
_cell_angle_beta                 102.66(3)
_cell_angle_gamma                99.98(3)
_cell_volume                     1964.5(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    16699
_cell_measurement_theta_min      6.18
_cell_measurement_theta_max      55.04

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             908
_exptl_absorpt_coefficient_mu    1.966
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5182
_exptl_absorpt_correction_T_max  0.8143
_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       'ω 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            19121
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.48
_reflns_number_total             8872
_reflns_number_gt                7679
_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          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0669P)²+3.7456P] where P=(Fo²+2Fc²)/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         8872
_refine_ls_number_parameters     558
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_ref         0.1255
_refine_ls_wR_factor_gt          0.1200
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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 0.5224(4) 0.7981(4) 0.8753(3) 0.0281(9) Uani 1 1 d . . .
C2 C 0.4281(4) 0.8415(4) 0.8372(3) 0.0291(9) Uani 1 1 d . . .
C3 C 0.3780(4) 0.9004(4) 0.9121(4) 0.0315(10) Uani 1 1 d . . .
C4 C 0.3834(4) 0.8267(4) 0.7283(3) 0.0270(9) Uani 1 1 d . . .
C5 C 0.2943(4) 0.8776(4) 0.6906(3) 0.0293(9) Uani 1 1 d . . .
C6 C 0.2554(4) 0.8644(4) 0.5856(4) 0.0295(9) Uani 1 1 d . . .
C7 C 0.2990(4) 0.7978(4) 0.5100(4) 0.0297(9) Uani 1 1 d . . .
C8 C 0.3869(5) 0.7471(4) 0.5481(4) 0.0328(10) Uani 1 1 d . . .
C9 C 0.4277(4) 0.7616(4) 0.6530(4) 0.0300(9) Uani 1 1 d . . .
C10 C 0.2586(5) 0.7833(4) 0.4017(4) 0.0340(10) Uani 1 1 d . . .
C11 C 0.1730(5) 0.8344(5) 0.3620(4) 0.0429(12) Uani 1 1 d . . .
C12 C 0.2975(5) 0.7120(5) 0.3250(4) 0.0392(11) Uani 1 1 d . . .
C13 C 0.9408(4) 0.5337(4) 0.8503(3) 0.0298(9) Uani 1 1 d . . .
C14 C 0.9890(4) 0.4592(4) 0.7897(3) 0.0264(9) Uani 1 1 d . . .
C15 C 1.0693(5) 0.4128(4) 0.8438(3) 0.0318(10) Uani 1 1 d . . .
C16 C 0.9575(4) 0.4323(4) 0.6773(3) 0.0243(8) Uani 1 1 d . . .
C17 C 0.8698(4) 0.4757(4) 0.6256(3) 0.0267(9) Uani 1 1 d . . .
C18 C 0.8395(4) 0.4518(4) 0.5179(3) 0.0269(9) Uani 1 1 d . . .
C19 C 0.8932(4) 0.3836(4) 0.4553(3) 0.0267(9) Uani 1 1 d . . .
C20 C 0.9797(4) 0.3391(4) 0.5071(4) 0.0290(9) Uani 1 1 d . . .
C21 C 1.0100(4) 0.3626(4) 0.6139(3) 0.0283(9) Uani 1 1 d . . .
C22 C 0.8628(4) 0.3593(4) 0.3447(3) 0.0309(10) Uani 1 1 d . . .
C23 C 0.7770(5) 0.4022(4) 0.2910(4) 0.0357(11) Uani 1 1 d . . .
C24 C 0.9207(5) 0.2957(4) 0.2806(4) 0.0326(10) Uani 1 1 d . . .
C25 C 0.5910(5) 0.5723(4) 0.5851(4) 0.0393(12) Uani 1 1 d . . .
H9 H 0.6523 0.6206 0.6423 0.047 Uiso 1 1 calc R . .
C26 C 0.5830(5) 0.5804(4) 0.4826(4) 0.0385(11) Uani 1 1 d . . .
C27 C 0.4875(5) 0.5034(5) 0.3984(4) 0.0406(12) Uani 1 1 d . . .
C28 C 0.6592(6) 0.6722(5) 0.3677(5) 0.0524(15) Uani 1 1 d . . .
C29 C 0.6635(5) 0.6610(5) 0.4667(4) 0.0441(13) Uani 1 1 d . . .
C30 C 0.7572(6) 0.7405(5) 0.5507(5) 0.0495(14) Uani 1 1 d . . .
C31 C 0.5857(5) -0.0492(4) 0.5379(4) 0.0314(10) Uani 1 1 d . . .
C32 C 0.5382(4) 0.0173(4) 0.6099(4) 0.0297(9) Uani 1 1 d . . .
C33 C 0.4502(5) 0.0654(4) 0.5671(4) 0.0332(10) Uani 1 1 d . . .
C34 C 0.6586(5) -0.0197(4) 0.7608(4) 0.0386(11) Uani 1 1 d . . .
C35 C 0.5734(5) 0.0313(4) 0.7184(4) 0.0328(10) Uani 1 1 d . . .
C36 C 0.5217(5) 0.0934(4) 0.7902(4) 0.0362(11) Uani 1 1 d . . .
Dy1 Dy 0.78976(2) 0.719234(19) 0.986144(15) 0.03155(9) Uani 1 1 d . . .
H1 H 0.255(5) 0.915(5) 0.742(5) 0.040(15) Uiso 1 1 d . . .
H2 H 0.213(5) 0.902(5) 0.559(4) 0.038(15) Uiso 1 1 d . . .
H3 H 0.415(5) 0.705(4) 0.500(4) 0.027(13) Uiso 1 1 d . . .
H4 H 0.495(6) 0.730(5) 0.674(5) 0.059(19) Uiso 1 1 d . . .
H5 H 0.833(4) 0.517(4) 0.667(4) 0.022(12) Uiso 1 1 d . . .
H6 H 0.788(6) 0.489(6) 0.479(6) 0.06(2) Uiso 1 1 d . . .
H7 H 1.011(5) 0.294(4) 0.467(4) 0.027(13) Uiso 1 1 d . . .
H8 H 1.075(5) 0.336(5) 0.642(5) 0.042(16) Uiso 1 1 d . . .
H10 H 0.483(5) 0.513(4) 0.332(5) 0.036(14) Uiso 1 1 d . . .
H11 H 0.633(6) -0.081(5) 0.564(5) 0.049(17) Uiso 1 1 d . . .
H12 H 0.421(5) 0.099(4) 0.609(4) 0.028(13) Uiso 1 1 d . . .
N1 N 0.5995(4) 0.7629(4) 0.9050(3) 0.0377(10) Uani 1 1 d . . .
N2 N 0.3344(5) 0.9469(5) 0.9698(4) 0.0535(13) Uani 1 1 d . . .
N3 N 0.1024(6) 0.8761(5) 0.3315(5) 0.0721(18) Uani 1 1 d . . .
N4 N 0.3279(6) 0.6558(5) 0.2624(4) 0.0594(14) Uani 1 1 d . . .
N5 N 0.7070(5) 0.4345(5) 0.2460(4) 0.0601(14) Uani 1 1 d . . .
N6 N 0.9682(5) 0.2466(4) 0.2284(4) 0.0504(12) Uani 1 1 d . . .
N7 N 0.8991(4) 0.5950(4) 0.8988(3) 0.0403(10) Uani 1 1 d . . .
N8 N 1.1329(5) 0.3762(4) 0.8914(3) 0.0442(11) Uani 1 1 d . . .
N9 N 0.6600(8) 0.6831(6) 0.2883(5) 0.090(2) Uani 1 1 d . . .
N10 N 0.8323(5) 0.8061(5) 0.6178(5) 0.0628(15) Uani 1 1 d . . .
N11 N 0.7256(6) -0.0616(5) 0.7937(4) 0.0605(15) Uani 1 1 d . . .
N12 N 0.4776(5) 0.1424(5) 0.8460(4) 0.0575(14) Uani 1 1 d . . .
O1 O 0.6555(4) 0.5514(4) 0.8896(4) 0.0578(11) Uani 1 1 d . . .
H14 H 0.6598 0.5038 0.8364 0.069 Uiso 1 1 d R . .
H13 H 0.6084 0.5330 0.9043 0.069 Uiso 1 1 d R . .
O2 O 0.8188(4) 0.7687(4) 0.8411(3) 0.0505(10) Uani 1 1 d . . .
H16 H 0.8729 0.7605 0.8105 0.061 Uiso 1 1 d R . .
H15 H 0.7905 0.8226 0.8215 0.061 Uiso 1 1 d R . .
O3 O 0.9923(4) 0.8097(4) 1.0629(4) 0.0679(13) Uani 1 1 d . . .
H18 H 1.0539 0.8322 1.1148 0.082 Uiso 1 1 d R . .
H17 H 1.0344 0.8179 1.0300 0.082 Uiso 1 1 d R . .
O4 O 0.6738(6) 0.7230(6) 1.1018(4) 0.089(2) Uani 1 1 d . . .
H19 H 0.6123 0.6439 1.0697 0.107 Uiso 1 1 d R . .
H20 H 0.6305 0.7577 1.1244 0.107 Uiso 1 1 d R . .
O5 O 0.8107(5) 0.9068(4) 1.0607(4) 0.0791(17) Uani 1 1 d . . .
H21 H 0.7738 0.9526 1.0486 0.095 Uiso 1 1 d R . .
H22 H 0.8788 0.9231 1.0506 0.095 Uiso 1 1 d R . .
O6 O 0.5598(6) 0.4710(7) 0.0822(6) 0.121(3) Uani 1 1 d . . .
H24 H 0.6041 0.4692 0.1383 0.145 Uiso 1 1 d R . .
H23 H 0.6099 0.5431 0.0815 0.145 Uiso 1 1 d R . .
O7 O 0.9596(7) 0.0067(5) 0.2502(6) 0.054(3) Uani 0.50 1 d P . .
H25 H 0.9650 0.0736 0.2622 0.064 Uiso 1 1 d R . .
H26 H 1.0166 0.0004 0.2945 0.064 Uiso 1 1 d R . .
O8 O 0.2024(8) 0.7435(15) 0.0438(9) 0.277(10) Uani 1 1 d . . .
H27 H 0.1888 0.6821 -0.0027 0.333 Uiso 1 1 d R . .
H28 H 0.2778 0.7697 0.0657 0.333 Uiso 1 1 d R . .


_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 N1 1.144(6) . ?
C1 C2 1.410(6) . ?
C2 C3 1.417(6) . ?
C2 C4 1.420(6) . ?
C3 N2 1.138(7) . ?
C4 C9 1.411(6) . ?
C4 C5 1.428(6) . ?
C5 C6 1.367(6) . ?
C5 H1 0.99(6) . ?
C6 C7 1.419(6) . ?
C6 H2 0.86(6) . ?
C7 C10 1.408(6) . ?
C7 C8 1.418(6) . ?
C8 C9 1.365(6) . ?
C8 H3 0.91(5) . ?
C9 H4 0.98(7) . ?
C10 C11 1.411(7) . ?
C10 C12 1.425(7) . ?
C11 N3 1.148(8) . ?
C12 N4 1.141(7) . ?
C13 N7 1.155(6) . ?
C13 C14 1.396(6) . ?
C14 C15 1.409(6) . ?
C14 C16 1.432(6) . ?
C15 N8 1.149(6) . ?
C16 C21 1.411(6) . ?
C16 C17 1.424(6) . ?
C17 C18 1.376(6) . ?
C17 H5 0.91(5) . ?
C18 C19 1.404(6) . ?
C18 H6 1.01(7) . ?
C19 C22 1.413(6) . ?
C19 C20 1.424(6) . ?
C20 C21 1.365(6) . ?
C20 H7 0.88(5) . ?
C21 H8 0.96(6) . ?
C22 C23 1.417(7) . ?
C22 C24 1.419(7) . ?
C23 N5 1.140(7) . ?
C24 N6 1.140(7) . ?
C25 C27 1.351(8) 2_666 ?
C25 C26 1.428(7) . ?
C25 H9 0.9300 . ?
C26 C29 1.404(8) . ?
C26 C27 1.426(8) . ?
C27 C25 1.351(8) 2_666 ?
C27 H10 0.94(6) . ?
C28 N9 1.143(9) . ?
C28 C29 1.403(8) . ?
C29 C30 1.426(9) . ?
C30 N10 1.152(9) . ?
C31 C33 1.357(7) 2_656 ?
C31 C32 1.417(6) . ?
C31 H11 0.83(7) . ?
C32 C35 1.408(6) . ?
C32 C33 1.418(6) . ?
C33 C31 1.357(7) 2_656 ?
C33 H12 0.80(6) . ?
C34 N11 1.130(7) . ?
C34 C35 1.420(7) . ?
C35 C36 1.421(7) . ?
C36 N12 1.140(7) . ?
Dy1 O4 2.313(5) . ?
Dy1 O1 2.339(5) . ?
Dy1 O3 2.342(5) . ?
Dy1 O2 2.343(4) . ?
Dy1 O5 2.365(5) . ?
Dy1 N7 2.483(4) . ?
Dy1 N8 2.491(4) 2_767 ?
Dy1 N1 2.521(4) . ?
Dy1 H22 2.5527 . ?
N8 Dy1 2.491(4) 2_767 ?
O1 H14 0.8420 . ?
O1 H13 0.6633 . ?
O2 H16 0.8450 . ?
O2 H15 0.9225 . ?
O3 H18 0.8413 . ?
O3 H17 0.7563 . ?
O4 H19 1.0806 . ?
O4 H20 0.8012 . ?
O5 H21 0.8408 . ?
O5 H22 0.8494 . ?
O6 H24 0.8418 . ?
O6 H23 1.0402 . ?
O7 H25 0.8465 . ?
O7 H26 0.8370 . ?
O8 H27 0.8500 . ?
O8 H28 0.8499 . ?

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
N1 C1 C2 179.1(5) . . ?
C1 C2 C3 117.3(4) . . ?
C1 C2 C4 122.0(4) . . ?
C3 C2 C4 120.7(4) . . ?
N2 C3 C2 177.8(5) . . ?
C9 C4 C2 120.6(4) . . ?
C9 C4 C5 117.5(4) . . ?
C2 C4 C5 122.0(4) . . ?
C6 C5 C4 120.7(4) . . ?
C6 C5 H1 121(3) . . ?
C4 C5 H1 117(3) . . ?
C5 C6 C7 121.6(4) . . ?
C5 C6 H2 126(4) . . ?
C7 C6 H2 112(4) . . ?
C10 C7 C8 120.9(4) . . ?
C10 C7 C6 121.9(4) . . ?
C8 C7 C6 117.2(4) . . ?
C9 C8 C7 121.3(4) . . ?
C9 C8 H3 122(3) . . ?
C7 C8 H3 117(3) . . ?
C8 C9 C4 121.6(4) . . ?
C8 C9 H4 116(4) . . ?
C4 C9 H4 122(4) . . ?
C7 C10 C11 122.1(5) . . ?
C7 C10 C12 122.0(5) . . ?
C11 C10 C12 115.9(4) . . ?
N3 C11 C10 178.6(7) . . ?
N4 C12 C10 178.8(6) . . ?
N7 C13 C14 178.6(5) . . ?
C13 C14 C15 117.2(4) . . ?
C13 C14 C16 120.6(4) . . ?
C15 C14 C16 122.2(4) . . ?
N8 C15 C14 177.2(5) . . ?
C21 C16 C17 117.6(4) . . ?
C21 C16 C14 122.3(4) . . ?
C17 C16 C14 120.0(4) . . ?
C18 C17 C16 120.8(4) . . ?
C18 C17 H5 123(3) . . ?
C16 C17 H5 116(3) . . ?
C17 C18 C19 121.3(4) . . ?
C17 C18 H6 124(4) . . ?
C19 C18 H6 115(4) . . ?
C18 C19 C22 121.5(4) . . ?
C18 C19 C20 117.7(4) . . ?
C22 C19 C20 120.8(4) . . ?
C21 C20 C19 121.1(4) . . ?
C21 C20 H7 121(3) . . ?
C19 C20 H7 117(3) . . ?
C20 C21 C16 121.3(4) . . ?
C20 C21 H8 115(4) . . ?
C16 C21 H8 124(4) . . ?
C19 C22 C23 122.0(4) . . ?
C19 C22 C24 122.4(4) . . ?
C23 C22 C24 115.4(4) . . ?
N5 C23 C22 178.4(6) . . ?
N6 C24 C22 178.4(6) . . ?
C27 C25 C26 122.1(5) 2_666 . ?
C27 C25 H9 118.9 2_666 . ?
C26 C25 H9 118.9 . . ?
C29 C26 C27 122.3(5) . . ?
C29 C26 C25 121.6(5) . . ?
C27 C26 C25 116.0(5) . . ?
C25 C27 C26 121.9(5) 2_666 . ?
C25 C27 H10 124(3) 2_666 . ?
C26 C27 H10 114(4) . . ?
N9 C28 C29 177.5(9) . . ?
C28 C29 C26 123.7(6) . . ?
C28 C29 C30 113.4(6) . . ?
C26 C29 C30 122.9(5) . . ?
N10 C30 C29 178.8(7) . . ?
C33 C31 C32 121.7(4) 2_656 . ?
C33 C31 H11 123(4) 2_656 . ?
C32 C31 H11 115(4) . . ?
C35 C32 C31 121.4(4) . . ?
C35 C32 C33 121.5(4) . . ?
C31 C32 C33 117.0(4) . . ?
C31 C33 C32 121.3(4) 2_656 . ?
C31 C33 H12 123(4) 2_656 . ?
C32 C33 H12 115(4) . . ?
N11 C34 C35 179.1(7) . . ?
C32 C35 C34 121.6(4) . . ?
C32 C35 C36 121.7(4) . . ?
C34 C35 C36 116.6(4) . . ?
N12 C36 C35 178.3(6) . . ?
O4 Dy1 O1 83.7(2) . . ?
O4 Dy1 O3 115.6(2) . . ?
O1 Dy1 O3 144.70(17) . . ?
O4 Dy1 O2 145.07(15) . . ?
O1 Dy1 O2 96.71(17) . . ?
O3 Dy1 O2 83.67(18) . . ?
O4 Dy1 O5 78.3(2) . . ?
O1 Dy1 O5 145.50(17) . . ?
O3 Dy1 O5 69.72(18) . . ?
O2 Dy1 O5 82.41(19) . . ?
O4 Dy1 N7 137.54(18) . . ?
O1 Dy1 N7 71.10(16) . . ?
O3 Dy1 N7 75.32(17) . . ?
O2 Dy1 N7 73.36(14) . . ?
O5 Dy1 N7 139.2(2) . . ?
O4 Dy1 N8 72.01(15) . 2_767 ?
O1 Dy1 N8 84.28(17) . 2_767 ?
O3 Dy1 N8 75.21(19) . 2_767 ?
O2 Dy1 N8 142.90(14) . 2_767 ?
O5 Dy1 N8 116.84(18) . 2_767 ?
N7 Dy1 N8 71.97(14) . 2_767 ?
O4 Dy1 N1 73.01(16) . . ?
O1 Dy1 N1 75.01(16) . . ?
O3 Dy1 N1 137.16(17) . . ?
O2 Dy1 N1 73.41(14) . . ?
O5 Dy1 N1 71.71(16) . . ?
N7 Dy1 N1 128.50(14) . . ?
N8 Dy1 N1 140.89(16) 2_767 . ?
O4 Dy1 H22 95.6 . . ?
O1 Dy1 H22 159.3 . . ?
O3 Dy1 H22 53.3 . . ?
O2 Dy1 H22 72.1 . . ?
O5 Dy1 H22 19.4 . . ?
N7 Dy1 H22 119.8 . . ?
N8 Dy1 H22 115.2 2_767 . ?
N1 Dy1 H22 85.0 . . ?
C1 N1 Dy1 170.0(4) . . ?
C13 N7 Dy1 173.8(4) . . ?
C15 N8 Dy1 160.8(4) . 2_767 ?
Dy1 O1 H14 128.4 . . ?
Dy1 O1 H13 122.0 . . ?
H14 O1 H13 109.5 . . ?
Dy1 O2 H16 129.1 . . ?
Dy1 O2 H15 124.1 . . ?
H16 O2 H15 103.5 . . ?
Dy1 O3 H18 150.4 . . ?
Dy1 O3 H17 122.0 . . ?
H18 O3 H17 86.1 . . ?
Dy1 O4 H19 103.7 . . ?
Dy1 O4 H20 138.9 . . ?
H19 O4 H20 99.2 . . ?
Dy1 O5 H21 137.0 . . ?
Dy1 O5 H22 92.9 . . ?
H21 O5 H22 107.5 . . ?
H24 O6 H23 97.2 . . ?
H25 O7 H26 107.5 . . ?
H27 O8 H28 107.7 . . ?

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
O1 H14 N4 0.84 2.23 3.029(7) 158.7 2_666
O1 H13 O6 0.66 2.03 2.637(9) 152.5 2_666
O2 H16 N6 0.85 2.07 2.903(7) 166.5 2_766
O2 H15 N11 0.92 1.93 2.848(6) 174.0 1_565
O3 H17 O8 0.76 2.36 2.816(16) 119.8 1_656
O4 H19 O6 1.08 2.34 3.303(11) 147.4 1_556
O4 H19 O6 1.08 2.47 3.395(11) 142.4 2_666
O4 H20 N12 0.80 2.02 2.808(7) 167.0 2_667
O5 H21 N2 0.84 2.03 2.865(7) 170.8 2_677
O6 H24 N5 0.84 1.92 2.743(8) 167.1 .
O6 H23 O4 1.04 2.30 3.303(11) 161.4 1_554
O7 H25 N6 0.85 2.47 3.275(8) 159.5 .
O7 H25 N10 0.85 2.55 2.993(9) 113.9 2_766
O7 H26 N3 0.84 2.20 2.897(8) 140.5 1_645

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.464
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.149
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zjw-3
_audit_block_doi                 10.5517/ccnzhkn
_database_code_depnum_ccdc_archive 'CCDC 625132'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/b909213g 2009
_audit_update_record             
;
2006-10-24 deposited with the CCDC.
2015-08-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H36 Gd2 N16 O10, 2(C12 H4 N4), 6(H2 O)'
_chemical_formula_sum            'C72 H56 Gd2 N24 O16'
_chemical_formula_weight         1827.91

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'
Gd Gd -0.1653 3.9035 '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                   11.848(2)
_cell_length_b                   13.338(3)
_cell_length_c                   13.786(3)
_cell_angle_alpha                106.21(3)
_cell_angle_beta                 102.56(3)
_cell_angle_gamma                100.34(3)
_cell_volume                     1973.8(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15717
_cell_measurement_theta_min      6.17
_cell_measurement_theta_max      54.96

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    1.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6407
_exptl_absorpt_correction_T_max  0.7372
_exptl_absorpt_process_details   
;
Higashi, T. (1995). Program for
Absorption Correction Correction. Rigaku Corporation, Tokyo, Japan.
;

_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       'ω scans'
_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            18907
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.48
_reflns_number_total             8778
_reflns_number_gt                7145
_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, 1997)'
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0803P)²+1.5046P] where P=(Fo²+2Fc²)/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         8778
_refine_ls_number_parameters     507
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1459
_refine_ls_wR_factor_gt          0.1358
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O8 O 0.2712 0.3121 0.9827 0.108(6) Uiso 0.40 1 d P A 4
H28 H 0.3162 0.3637 1.0373 0.162 Uiso 0.40 1 d PR A 4
H27 H 0.2103 0.3314 0.9553 0.162 Uiso 0.40 1 d PR A 4
O8' O 0.3007 1.2281(8) 0.9566 0.094(3) Uiso 0.60 1 d P B 3
H28' H 0.2840 1.1737 0.9022 0.142 Uiso 0.60 1 d PR B 3
H27' H 0.3415 1.2203 1.0107 0.142 Uiso 0.60 1 d PR B 3
O3' O 0.8159(8) 0.2623(7) -0.1117(6) 0.0411(17) Uiso 0.50 1 d P C 2
H29' H 0.8492 0.2161 -0.0921 0.062 Uiso 0.50 1 d PR C 2
H30' H 0.7414 0.2110 -0.1697 0.062 Uiso 0.50 1 d PR C 2
O3 O 0.8679(9) 0.3123(9) -0.0760(8) 0.056(2) Uiso 0.50 1 d P D 1
H29 H 0.9146 0.3844 -0.0112 0.084 Uiso 0.50 1 d PR D 1
H30 H 0.9098 0.2447 -0.0806 0.084 Uiso 0.50 1 d PR D 1
C1 C 0.9769(5) 0.2006(4) 0.1271(4) 0.0313(10) Uani 1 1 d . E 1
C2 C 1.0710(5) 0.1576(4) 0.1636(4) 0.0300(10) Uani 1 1 d . E 1
C3 C 1.1213(5) 0.1007(4) 0.0899(4) 0.0366(12) Uani 1 1 d . E 1
C4 C 1.1160(5) 0.1718(4) 0.2732(4) 0.0304(10) Uani 1 1 d . E 1
C5 C 1.0717(5) 0.2375(4) 0.3493(4) 0.0331(11) Uani 1 1 d . E 1
H1 H 1.0137 0.2714 0.3274 0.040 Uiso 1 1 calc R E 1
C6 C 1.1132(5) 0.2513(4) 0.4532(4) 0.0341(11) Uani 1 1 d . E 1
H2 H 1.0831 0.2949 0.5012 0.041 Uiso 1 1 calc R E 1
C7 C 1.2012(5) 0.2014(4) 0.4908(4) 0.0333(11) Uani 1 1 d . E 1
C8 C 1.2441(5) 0.1351(4) 0.4150(4) 0.0321(10) Uani 1 1 d . E 1
H3 H 1.3006 0.0999 0.4370 0.038 Uiso 1 1 calc R E 1
C9 C 1.2043(5) 0.1219(4) 0.3104(4) 0.0301(10) Uani 1 1 d . E 1
H4 H 1.2358 0.0795 0.2628 0.036 Uiso 1 1 calc R E 1
C10 C 1.3294(6) 0.1663(5) 0.6384(5) 0.0453(14) Uani 1 1 d . E 1
C11 C 1.2425(5) 0.2166(4) 0.5991(4) 0.0355(11) Uani 1 1 d . E 1
C12 C 1.2031(6) 0.2867(5) 0.6755(4) 0.0432(13) Uani 1 1 d . E 1
C13 C 0.5561(5) 0.4634(4) 0.1477(4) 0.0326(11) Uani 1 1 d . F 1
C14 C 0.5073(5) 0.5372(4) 0.2089(4) 0.0297(10) Uani 1 1 d . F 1
C15 C 0.4286(5) 0.5826(4) 0.1558(4) 0.0354(11) Uani 1 1 d . F 1
C16 C 0.5424(5) 0.5663(4) 0.3222(4) 0.0286(10) Uani 1 1 d . F 1
C17 C 0.6290(5) 0.5236(4) 0.3734(4) 0.0301(10) Uani 1 1 d . F 1
H5 H 0.6653 0.4782 0.3335 0.036 Uiso 1 1 calc R F 1
C18 C 0.6604(5) 0.5477(4) 0.4797(4) 0.0303(10) Uani 1 1 d . F 1
H6 H 0.7182 0.5188 0.5113 0.036 Uiso 1 1 calc R F 1
C19 C 0.6069(4) 0.6157(4) 0.5434(3) 0.0281(10) Uani 1 1 d . F 1
C20 C 0.5203(5) 0.6592(4) 0.4919(4) 0.0322(11) Uani 1 1 d . F 1
H7 H 0.4842 0.7050 0.5316 0.039 Uiso 1 1 calc R F 1
C21 C 0.4894(5) 0.6348(4) 0.3855(4) 0.0295(10) Uani 1 1 d . F 1
H8 H 0.4320 0.6639 0.3538 0.035 Uiso 1 1 calc R F 1
C22 C 0.7248(5) 0.5976(4) 0.7070(4) 0.0366(11) Uani 1 1 d . F 1
C23 C 0.6380(5) 0.6404(4) 0.6542(4) 0.0327(11) Uani 1 1 d . F 1
C24 C 0.5815(5) 0.7041(4) 0.7188(4) 0.0377(12) Uani 1 1 d . F 1
C25 C 0.1614(6) -0.0163(5) 0.7621(4) 0.0416(13) Uani 1 1 d . G 1
C26 C 0.0756(5) 0.0321(4) 0.7190(4) 0.0363(12) Uani 1 1 d . G 1
C27 C 0.0240(5) 0.0954(4) 0.7898(4) 0.0387(12) Uani 1 1 d . G 1
C28 C 0.0388(5) 0.0177(4) 0.6094(4) 0.0337(11) Uani 1 1 d . . 1
C29 C -0.0497(5) 0.0651(4) 0.5674(4) 0.0349(11) Uani 1 1 d . H 1
H9 H -0.0834 0.1078 0.6127 0.042 Uiso 1 1 calc R H 1
C30 C -0.0862(5) 0.0497(4) 0.4625(4) 0.0350(11) Uani 1 1 d . . 1
H10 H -0.1427 0.0835 0.4375 0.042 Uiso 1 1 calc R . 1
C31 C 0.2562(7) 0.7406(6) 0.5523(6) 0.0537(16) Uani 1 1 d . I 1
C32 C 0.1627(6) 0.6621(5) 0.4673(5) 0.0461(14) Uani 1 1 d . I 1
C33 C 0.1592(7) 0.6729(6) 0.3683(5) 0.0566(17) Uani 1 1 d . I 1
C34 C 0.0822(6) 0.5803(5) 0.4829(4) 0.0413(13) Uani 1 1 d . I 1
C35 C -0.0119(6) 0.5048(5) 0.3988(5) 0.0445(14) Uani 1 1 d . . 1
H11 H -0.0202 0.5075 0.3310 0.053 Uiso 1 1 calc R . 1
C36 C 0.0918(6) 0.5730(5) 0.5849(4) 0.0439(13) Uani 1 1 d . . 1
H12 H 0.1533 0.6216 0.6418 0.053 Uiso 1 1 calc R . 1
Gd1 Gd 0.70930(2) 0.27853(2) 0.011014(18) 0.03490(11) Uani 1 1 d . . 1
N1 N 0.8991(5) 0.2349(4) 0.0966(4) 0.0423(11) Uani 1 1 d . E 1
N2 N 1.1659(5) 0.0544(5) 0.0308(4) 0.0578(15) Uani 1 1 d . E 1
N3 N 1.3985(7) 0.1249(6) 0.6688(6) 0.077(2) Uani 1 1 d . E 1
N4 N 1.1738(6) 0.3438(5) 0.7382(4) 0.0614(15) Uani 1 1 d . E 1
N5 N 0.5967(5) 0.4025(4) 0.0999(3) 0.0409(11) Uani 1 1 d . F 1
N6 N 0.3640(5) 0.6201(4) 0.1081(4) 0.0499(13) Uani 1 1 d . . 1
N7 N 0.7929(6) 0.5671(5) 0.7523(5) 0.0612(15) Uani 1 1 d . F 1
N8 N 0.5338(5) 0.7538(4) 0.7705(4) 0.0527(13) Uani 1 1 d . F 1
N9 N 0.2287(6) -0.0591(5) 0.7950(4) 0.0615(16) Uani 1 1 d . G 1
N10 N -0.0181(6) 0.1436(5) 0.8458(4) 0.0601(15) Uani 1 1 d . G 1
N11 N 0.3327(6) 0.8060(5) 0.6189(6) 0.0695(17) Uani 1 1 d . I 1
N12 N 0.1633(9) 0.6864(7) 0.2907(6) 0.096(3) Uani 1 1 d . I 1
O1 O 0.5038(5) 0.1878(4) -0.0686(5) 0.0755(15) Uani 1 1 d . J 1
H13 H 0.4827 0.1224 -0.1099 0.113 Uiso 1 1 d R J 1
H14 H 0.4434 0.2032 -0.0495 0.113 Uiso 1 1 d R J 1
O2 O 0.6844(6) 0.0869(4) -0.0582(5) 0.0869(19) Uani 1 1 d . K 1
H15 H 0.7252 0.0473 -0.0359 0.130 Uiso 1 1 d R K 1
H16 H 0.6476 0.0556 -0.1236 0.130 Uiso 1 1 d R K 1
O4 O 0.8445(4) 0.4479(4) 0.1128(4) 0.0642(13) Uani 1 1 d . L 1
H19 H 0.8433 0.5104 0.1496 0.096 Uiso 1 1 d R L 1
H20 H 0.9168 0.4442 0.1258 0.096 Uiso 1 1 d R L 1
O5 O 0.6772(4) 0.2294(4) 0.1581(3) 0.0568(12) Uani 1 1 d . M 1
H21 H 0.6207 0.2435 0.1821 0.085 Uiso 1 1 d R M 1
H22 H 0.6927 0.1713 0.1647 0.085 Uiso 1 1 d R M 1
O6 O 0.0611(6) 0.4771(7) 0.0905(6) 0.116(3) Uani 1 1 d . N 1
H23 H 0.0923 0.4607 0.1453 0.173 Uiso 1 1 d R N 1
H24 H 0.0747 0.4314 0.0374 0.173 Uiso 1 1 d R N 1
O7 O 0.5379(7) 0.9901(5) 0.7469(6) 0.125(3) Uani 1 1 d . O 1
H25 H 0.5209 0.9848 0.8033 0.187 Uiso 1 1 d R O 1
H26 H 0.5315 0.9267 0.7065 0.187 Uiso 1 1 d R O 1


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O8 H28 0.8530 . ?
O8 H27 0.8556 . ?
O8' H28' 0.8425 . ?
O8' H27' 0.8402 . ?
O3' H29' 0.8619 . ?
O3' H30' 1.0281 . ?
O3' H30 1.1915 . ?
O3 Gd1 2.481(9) . ?
O3 H29' 1.2090 . ?
O3 H29 1.0702 . ?
O3 H30 1.0974 . ?
C1 N1 1.152(7) . ?
C1 C2 1.405(7) . ?
C2 C3 1.399(7) . ?
C2 C4 1.434(7) . ?
C3 N2 1.161(7) . ?
C4 C9 1.417(7) . ?
C4 C5 1.427(7) . ?
C5 C6 1.357(7) . ?
C5 H1 0.9300 . ?
C6 C7 1.416(7) . ?
C6 H2 0.9300 . ?
C7 C11 1.410(7) . ?
C7 C8 1.417(7) . ?
C8 C9 1.366(7) . ?
C8 H3 0.9300 . ?
C9 H4 0.9300 . ?
C10 N3 1.137(9) . ?
C10 C11 1.419(8) . ?
C11 C12 1.423(8) . ?
C12 N4 1.142(8) . ?
C13 N5 1.142(6) . ?
C13 C14 1.403(7) . ?
C14 C15 1.388(7) . ?
C14 C16 1.443(6) . ?
C15 N6 1.171(7) . ?
C16 C21 1.411(6) . ?
C16 C17 1.412(7) . ?
C17 C18 1.360(7) . ?
C17 H5 0.9300 . ?
C18 C19 1.415(7) . ?
C18 H6 0.9300 . ?
C19 C23 1.418(6) . ?
C19 C20 1.420(7) . ?
C20 C21 1.359(7) . ?
C20 H7 0.9300 . ?
C21 H8 0.9300 . ?
C22 N7 1.117(7) . ?
C22 C23 1.424(8) . ?
C23 C24 1.415(7) . ?
C24 N8 1.146(7) . ?
C25 N9 1.148(7) . ?
C25 C26 1.410(8) . ?
C26 C27 1.423(7) . ?
C26 C28 1.426(7) . ?
C27 N10 1.124(7) . ?
C28 C29 1.419(7) . ?
C28 C30 1.425(7) 2_556 ?
C29 C30 1.360(7) . ?
C29 H9 0.9300 . ?
C30 C28 1.425(7) 2_556 ?
C30 H10 0.9300 . ?
C31 N11 1.154(9) . ?
C31 C32 1.425(10) . ?
C32 C33 1.404(9) . ?
C32 C34 1.412(9) . ?
C33 N12 1.144(9) . ?
C34 C35 1.410(9) . ?
C34 C36 1.417(8) . ?
C35 C36 1.376(9) 2_566 ?
C35 H11 0.9300 . ?
C36 C35 1.376(9) 2_566 ?
C36 H12 0.9300 . ?
Gd1 O4 2.365(5) . ?
Gd1 O1 2.374(5) . ?
Gd1 O5 2.383(4) . ?
Gd1 O2 2.403(5) . ?
Gd1 N6 2.514(5) 2_665 ?
Gd1 N5 2.527(4) . ?
Gd1 N1 2.546(5) . ?
Gd1 H29' 2.5147 . ?
Gd1 H30' 2.5382 . ?
N6 Gd1 2.514(5) 2_665 ?
O1 H13 0.8547 . ?
O1 H14 0.8541 . ?
O2 H15 0.8517 . ?
O2 H16 0.8556 . ?
O4 H19 0.8500 . ?
O4 H20 0.8500 . ?
O5 H21 0.8361 . ?
O5 H22 0.8517 . ?
O6 H23 0.8693 . ?
O6 H24 0.8779 . ?
O7 H25 0.8628 . ?
O7 H26 0.8524 . ?

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
H28 O8 H27 109.8 . . ?
H28' O8' H27' 113.3 . . ?
H29' O3' H30' 100.2 . . ?
H29' O3' H30 36.2 . . ?
H30' O3' H30 128.2 . . ?
Gd1 O3 H29' 77.6 . . ?
Gd1 O3 H29 90.4 . . ?
H29' O3 H29 136.6 . . ?
Gd1 O3 H30 105.5 . . ?
H29' O3 H30 35.5 . . ?
H29 O3 H30 114.8 . . ?
N1 C1 C2 179.3(6) . . ?
C3 C2 C1 118.1(5) . . ?
C3 C2 C4 120.3(4) . . ?
C1 C2 C4 121.5(4) . . ?
N2 C3 C2 178.1(6) . . ?
C9 C4 C5 117.4(4) . . ?
C9 C4 C2 122.3(4) . . ?
C5 C4 C2 120.3(4) . . ?
C6 C5 C4 120.9(5) . . ?
C6 C5 H1 119.6 . . ?
C4 C5 H1 119.6 . . ?
C5 C6 C7 121.9(5) . . ?
C5 C6 H2 119.1 . . ?
C7 C6 H2 119.1 . . ?
C11 C7 C6 120.8(5) . . ?
C11 C7 C8 121.9(5) . . ?
C6 C7 C8 117.2(4) . . ?
C9 C8 C7 121.4(5) . . ?
C9 C8 H3 119.3 . . ?
C7 C8 H3 119.3 . . ?
C8 C9 C4 121.2(4) . . ?
C8 C9 H4 119.4 . . ?
C4 C9 H4 119.4 . . ?
N3 C10 C11 179.2(8) . . ?
C7 C11 C10 121.9(5) . . ?
C7 C11 C12 121.9(5) . . ?
C10 C11 C12 116.2(5) . . ?
N4 C12 C11 178.6(7) . . ?
N5 C13 C14 178.3(5) . . ?
C15 C14 C13 117.0(4) . . ?
C15 C14 C16 122.6(4) . . ?
C13 C14 C16 120.4(4) . . ?
N6 C15 C14 177.7(5) . . ?
C21 C16 C17 117.5(4) . . ?
C21 C16 C14 121.8(4) . . ?
C17 C16 C14 120.6(4) . . ?
C18 C17 C16 121.4(4) . . ?
C18 C17 H5 119.3 . . ?
C16 C17 H5 119.3 . . ?
C17 C18 C19 121.2(4) . . ?
C17 C18 H6 119.4 . . ?
C19 C18 H6 119.4 . . ?
C18 C19 C23 121.7(4) . . ?
C18 C19 C20 117.4(4) . . ?
C23 C19 C20 120.9(4) . . ?
C21 C20 C19 121.0(4) . . ?
C21 C20 H7 119.5 . . ?
C19 C20 H7 119.5 . . ?
C20 C21 C16 121.4(4) . . ?
C20 C21 H8 119.3 . . ?
C16 C21 H8 119.3 . . ?
N7 C22 C23 177.0(6) . . ?
C24 C23 C19 122.6(5) . . ?
C24 C23 C22 115.7(5) . . ?
C19 C23 C22 121.6(5) . . ?
N8 C24 C23 178.6(6) . . ?
N9 C25 C26 177.6(7) . . ?
C25 C26 C27 117.0(5) . . ?
C25 C26 C28 122.6(5) . . ?
C27 C26 C28 120.4(5) . . ?
N10 C27 C26 178.6(7) . . ?
C29 C28 C30 117.8(5) . 2_556 ?
C29 C28 C26 121.6(4) . . ?
C30 C28 C26 120.6(5) 2_556 . ?
C30 C29 C28 121.5(4) . . ?
C30 C29 H9 119.2 . . ?
C28 C29 H9 119.2 . . ?
C29 C30 C28 120.7(5) . 2_556 ?
C29 C30 H10 119.7 . . ?
C28 C30 H10 119.7 2_556 . ?
N11 C31 C32 177.8(7) . . ?
C33 C32 C34 123.7(6) . . ?
C33 C32 C31 114.3(6) . . ?
C34 C32 C31 122.0(6) . . ?
N12 C33 C32 175.6(9) . . ?
C35 C34 C32 121.5(5) . . ?
C35 C34 C36 117.6(5) . . ?
C32 C34 C36 120.9(6) . . ?
C36 C35 C34 121.1(5) 2_566 . ?
C36 C35 H11 119.4 2_566 . ?
C34 C35 H11 119.4 . . ?
C35 C36 C34 121.3(6) 2_566 . ?
C35 C36 H12 119.4 2_566 . ?
C34 C36 H12 119.4 . . ?
O4 Gd1 O1 144.10(18) . . ?
O4 Gd1 O5 95.24(18) . . ?
O1 Gd1 O5 84.00(19) . . ?
O4 Gd1 O2 145.90(19) . . ?
O1 Gd1 O2 69.5(2) . . ?
O5 Gd1 O2 80.3(2) . . ?
O4 Gd1 O3 71.3(3) . . ?
O1 Gd1 O3 128.3(3) . . ?
O5 Gd1 O3 141.0(3) . . ?
O2 Gd1 O3 91.0(3) . . ?
O4 Gd1 N6 83.59(19) . 2_665 ?
O1 Gd1 N6 75.8(2) . 2_665 ?
O5 Gd1 N6 141.94(15) . 2_665 ?
O2 Gd1 N6 120.40(19) . 2_665 ?
O3 Gd1 N6 74.5(3) . 2_665 ?
O4 Gd1 N5 71.02(17) . . ?
O1 Gd1 N5 74.68(18) . . ?
O5 Gd1 N5 72.18(14) . . ?
O2 Gd1 N5 136.5(2) . . ?
O3 Gd1 N5 131.2(3) . . ?
N6 Gd1 N5 71.54(15) 2_665 . ?
O4 Gd1 N1 74.72(17) . . ?
O1 Gd1 N1 137.42(18) . . ?
O5 Gd1 N1 72.82(15) . . ?
O2 Gd1 N1 71.65(18) . . ?
O3 Gd1 N1 68.4(3) . . ?
N6 Gd1 N1 141.32(17) 2_665 . ?
N5 Gd1 N1 127.58(15) . . ?
O4 Gd1 H29' 94.3 . . ?
O1 Gd1 H29' 115.4 . . ?
O5 Gd1 H29' 125.4 . . ?
O2 Gd1 H29' 63.2 . . ?
O3 Gd1 H29' 28.0 . . ?
N6 Gd1 H29' 92.6 2_665 . ?
N5 Gd1 H29' 159.1 . . ?
N1 Gd1 H29' 58.4 . . ?
O4 Gd1 H30' 110.9 . . ?
O1 Gd1 H30' 87.7 . . ?
O5 Gd1 H30' 144.8 . . ?
O2 Gd1 H30' 64.8 . . ?
O3 Gd1 H30' 41.7 . . ?
N6 Gd1 H30' 66.9 2_665 . ?
N5 Gd1 H30' 137.7 . . ?
N1 Gd1 H30' 91.3 . . ?
H29' Gd1 H30' 33.4 . . ?
C1 N1 Gd1 170.5(5) . . ?
C13 N5 Gd1 173.3(5) . . ?
C15 N6 Gd1 159.9(5) . 2_665 ?
Gd1 O1 H13 120.6 . . ?
Gd1 O1 H14 128.5 . . ?
H13 O1 H14 108.3 . . ?
Gd1 O2 H15 129.7 . . ?
Gd1 O2 H16 117.0 . . ?
H15 O2 H16 109.6 . . ?
Gd1 O4 H19 139.1 . . ?
Gd1 O4 H20 112.2 . . ?
H19 O4 H20 107.7 . . ?
Gd1 O5 H21 120.6 . . ?
Gd1 O5 H22 118.6 . . ?
H21 O5 H22 112.4 . . ?
H23 O6 H24 104.9 . . ?
H25 O7 H26 108.0 . . ?

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
O2 H15 N2 0.85 2.04 2.855(7) 160.6 2_755
O2 H16 O7 0.86 1.83 2.671(9) 166.7 1_544
O4 H19 N4 0.85 2.19 3.034(7) 169.5 2_766
O4 H20 O6 0.85 1.89 2.624(9) 144.1 1_655
O5 H21 N8 0.84 2.08 2.900(7) 168.8 2_666
O5 H22 N9 0.85 2.04 2.870(7) 165.1 2_656
O6 H23 N7 0.87 1.90 2.736(8) 160.3 2_666
O7 H26 N11 0.85 2.43 2.937(10) 118.6 .

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.671
_refine_diff_density_rms         0.156
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zjw-6
_audit_block_doi                 10.5517/ccnzhlp
_database_code_depnum_ccdc_archive 'CCDC 625133'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/b909213g 2009
_audit_update_record             
;
2006-10-24 deposited with the CCDC.
2015-08-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H30 Lu N12 O8'
_chemical_formula_weight         945.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n '
_symmetry_space_group_name_Hall  '-P 2yn '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.033(2)
_cell_length_b                   25.381(5)
_cell_length_c                   15.298(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.57(3)
_cell_angle_gamma                90.00
_cell_volume                     4181.3(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    31800
_cell_measurement_theta_min      6.01
_cell_measurement_theta_max      54.96

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1884
_exptl_absorpt_coefficient_mu    2.424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4518
_exptl_absorpt_correction_T_max  0.5887
_exptl_absorpt_process_details   
;
Higashi, T. (1995). Program for
Absorption Correction Correction. Rigaku Corporation, Tokyo, Japan.
;

_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       'ω scans'
_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            38964
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         28.28
_reflns_number_total             9352
_reflns_number_gt                7651
_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, 1997)'
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ?

_refine_special_details          
;
1. the 'isor' commands were used to restrain the ADPs, such as
isor 0.001 o8
isor 0.001 o9
isor 0.001 c37
isor 0.001 c38
isor 0.001 n10
isor 0.001 n11
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0417P)²+6.7335P] where P=(Fo²+2Fc²)/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         9352
_refine_ls_number_parameters     545
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0878
_refine_ls_wR_factor_gt          0.0821
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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
C37 C 0.854(2) 0.2565(8) 0.4245(16) 0.140(7) Uani 0.50 1 d PU . .
H13 H 0.8192 0.2833 0.3822 0.210 Uiso 0.50 1 calc PR . .
H14 H 0.8289 0.2224 0.3999 0.210 Uiso 0.50 1 calc PR . .
H15 H 0.9431 0.2589 0.4371 0.210 Uiso 0.50 1 calc PR . .
O8 O 0.5201(7) 0.3860(3) 0.5741(5) 0.0657(19) Uani 0.50 1 d PU . .
H16 H 0.5562 0.4001 0.6207 0.098 Uiso 0.50 1 calc PR . .
O9 O 0.8176(10) 0.2627(4) 0.4937(7) 0.087(3) Uani 0.50 1 d PU . .
H20 H 0.7968 0.2341 0.5109 0.131 Uiso 0.50 1 calc PR . .
O7 O 0.0548(3) 0.29029(13) 0.1944(2) 0.0490(7) Uani 1 1 d . . .
H33 H 0.0295 0.3200 0.2105 0.073 Uiso 1 1 d R . .
H34 H -0.0033 0.2679 0.1905 0.073 Uiso 1 1 d R . .
C1 C 0.6119(4) 0.18372(15) 0.2905(3) 0.0364(9) Uani 1 1 d . . .
C2 C 0.6947(4) 0.16199(15) 0.2458(3) 0.0370(9) Uani 1 1 d . . .
C3 C 0.7764(4) 0.19647(17) 0.2188(3) 0.0441(10) Uani 1 1 d . . .
C4 C 0.6964(3) 0.10621(15) 0.2322(3) 0.0329(8) Uani 1 1 d . . .
C5 C 0.6137(4) 0.07284(16) 0.2621(3) 0.0364(9) Uani 1 1 d . . .
H1 H 0.5566 0.0873 0.2919 0.044 Uiso 1 1 calc R . .
C6 C 0.6137(4) 0.01990(16) 0.2492(3) 0.0379(9) Uani 1 1 d . . .
H2 H 0.5555 -0.0007 0.2693 0.045 Uiso 1 1 calc R . .
C7 C 0.6980(3) -0.00441(16) 0.2070(3) 0.0351(8) Uani 1 1 d . . .
C8 C 0.7802(4) 0.02891(17) 0.1770(3) 0.0384(9) Uani 1 1 d . . .
H83 H 0.8376 0.0144 0.1476 0.046 Uiso 1 1 calc R . .
C9 C 0.7799(3) 0.08230(16) 0.1891(3) 0.0353(8) Uani 1 1 d . . .
H94 H 0.8369 0.1030 0.1679 0.042 Uiso 1 1 calc R . .
C10 C 0.6975(4) -0.05962(18) 0.1954(3) 0.0459(10) Uani 1 1 d . . .
C11 C 0.6133(5) -0.09255(19) 0.2249(4) 0.0542(12) Uani 1 1 d . . .
C12 C 0.7827(5) -0.0856(2) 0.1560(4) 0.0602(14) Uani 1 1 d . . .
C13 C 0.2347(3) 0.17141(14) 0.5429(2) 0.0299(8) Uani 1 1 d . . .
C14 C 0.0834(4) 0.18404(16) 0.6265(3) 0.0431(10) Uani 1 1 d . . .
C15 C 0.1528(3) 0.14861(15) 0.5883(3) 0.0321(8) Uani 1 1 d . . .
C16 C 0.1363(3) 0.09304(14) 0.5924(2) 0.0289(7) Uani 1 1 d . . .
C17 C 0.0472(3) 0.06998(15) 0.6319(2) 0.0299(8) Uani 1 1 d . . .
H5 H -0.0029 0.0914 0.6586 0.036 Uiso 1 1 calc R . .
C18 C 0.0316(3) 0.01664(15) 0.6325(2) 0.0299(8) Uani 1 1 d . . .
H6 H -0.0289 0.0028 0.6598 0.036 Uiso 1 1 calc R . .
C19 C 0.1032(3) -0.01816(14) 0.5934(2) 0.0283(7) Uani 1 1 d . . .
C20 C 0.1937(3) 0.00544(15) 0.5557(3) 0.0327(8) Uani 1 1 d . . .
H7 H 0.2453 -0.0159 0.5302 0.039 Uiso 1 1 calc R . .
C21 C 0.2094(3) 0.05846(15) 0.5547(3) 0.0331(8) Uani 1 1 d . . .
H8 H 0.2707 0.0722 0.5281 0.040 Uiso 1 1 calc R . .
C22 C 0.0877(3) -0.07356(15) 0.5920(3) 0.0329(8) Uani 1 1 d . . .
C23 C -0.0026(4) -0.09876(15) 0.6279(3) 0.0362(9) Uani 1 1 d . . .
C24 C 0.1600(4) -0.10738(16) 0.5518(3) 0.0371(9) Uani 1 1 d . . .
C25 C 0.9006(5) 0.3752(3) 0.5969(4) 0.0672(15) Uani 1 1 d . . .
C26 C 0.9773(5) 0.3931(3) 0.5443(4) 0.0659(15) Uani 1 1 d . . .
C27 C 1.0506(6) 0.3540(3) 0.5182(4) 0.082(2) Uani 1 1 d . . .
C28 C 0.9880(5) 0.4447(3) 0.5206(3) 0.0641(16) Uani 1 1 d . . .
C29 C 1.0730(4) 0.4635(3) 0.4739(3) 0.0646(16) Uani 1 1 d . . .
H9 H 1.1250 0.4389 0.4556 0.078 Uiso 1 1 calc R . .
C30 C 1.0868(5) 0.5138(3) 0.4529(3) 0.0647(16) Uani 1 1 d . . .
H10 H 1.1461 0.5225 0.4204 0.078 Uiso 1 1 calc R . .
C31 C 0.2581(6) 1.0120(3) 0.2696(5) 0.0801(19) Uani 1 1 d . . .
C32 C 0.3179(5) 0.9741(2) 0.3337(5) 0.0678(17) Uani 1 1 d . . .
C33 C 0.2785(5) 0.9212(2) 0.3116(4) 0.0691(16) Uani 1 1 d . . .
C34 C 0.4088(5) 0.98672(19) 0.4157(4) 0.0593(15) Uani 1 1 d . . .
C35 C 0.4683(5) 0.94777(19) 0.4800(5) 0.0673(18) Uani 1 1 d . . .
H11 H 0.4489 0.9125 0.4677 0.081 Uiso 1 1 calc R . .
C36 C 0.5549(5) 0.96009(19) 0.5609(5) 0.0662(17) Uani 1 1 d . . .
H12 H 0.5887 0.9330 0.5995 0.079 Uiso 1 1 calc R . .
Lu1 Lu 0.407157(14) 0.237583(6) 0.407709(10) 0.02736(6) Uani 1 1 d . . .
N1 N 0.5439(3) 0.19937(13) 0.3289(2) 0.0391(8) Uani 1 1 d . . .
N2 N 0.8434(5) 0.22409(17) 0.1958(3) 0.0662(13) Uani 1 1 d . . .
N3 N 0.5458(5) -0.11908(19) 0.2485(4) 0.0787(15) Uani 1 1 d . . .
N4 N 0.8511(5) -0.1070(2) 0.1259(5) 0.098(2) Uani 1 1 d . . .
N5 N 0.2996(3) 0.19028(13) 0.5051(2) 0.0366(7) Uani 1 1 d . . .
N6 N 0.0256(5) 0.21228(18) 0.6572(4) 0.0740(15) Uani 1 1 d . . .
N7 N -0.0756(4) -0.11960(16) 0.6559(3) 0.0526(10) Uani 1 1 d . . .
N8 N 0.2191(4) -0.13411(16) 0.5207(3) 0.0536(10) Uani 1 1 d . . .
N9 N 0.8390(5) 0.3599(2) 0.6425(4) 0.0869(16) Uani 1 1 d . . .
N10 N 1.1131(6) 0.3221(3) 0.4971(5) 0.1042(19) Uani 1 1 d U . .
N11 N 0.2043(7) 1.0413(3) 0.2149(5) 0.113(2) Uani 1 1 d U . .
N12 N 0.2442(5) 0.8797(2) 0.2920(4) 0.0874(17) Uani 1 1 d . . .
O1 O 0.3017(3) 0.16772(12) 0.3224(2) 0.0519(8) Uani 1 1 d . . .
H21 H 0.2306 0.1554 0.3274 0.078 Uiso 1 1 d R . .
H22 H 0.3049 0.1651 0.2675 0.078 Uiso 1 1 d R . .
O2 O 0.5621(3) 0.19355(12) 0.5162(2) 0.0441(7) Uani 1 1 d . . .
H23 H 0.5684 0.2038 0.5685 0.066 Uiso 1 1 d R . .
H24 H 0.6296 0.1816 0.5075 0.066 Uiso 1 1 d R . .
O3 O 0.2074(3) 0.27059(15) 0.3679(2) 0.0617(10) Uani 1 1 d . . .
H25 H 0.1623 0.2759 0.3164 0.093 Uiso 1 1 d R . .
H26 H 0.1799 0.2867 0.4075 0.093 Uiso 1 1 d R . .
O4 O 0.4046(3) 0.29363(13) 0.5239(2) 0.0556(9) Uani 1 1 d . . .
H27 H 0.4423 0.3224 0.5420 0.083 Uiso 1 1 d R . .
H28 H 0.3453 0.2888 0.5497 0.083 Uiso 1 1 d R . .
O5 O 0.3723(3) 0.28178(14) 0.2726(2) 0.0557(9) Uani 1 1 d . . .
H29 H 0.3380 0.3115 0.2576 0.084 Uiso 1 1 d R . .
H30 H 0.4206 0.2750 0.2378 0.084 Uiso 1 1 d R . .
O6 O 0.5782(3) 0.29479(12) 0.4333(2) 0.0549(8) Uani 1 1 d . . .
H31 H 0.6520 0.2834 0.4539 0.082 Uiso 1 1 d R . .
H32 H 0.5776 0.3249 0.4129 0.082 Uiso 1 1 d R . .
C38 C 0.4706(18) 0.4239(8) 0.5129(14) 0.137(7) Uani 0.50 1 d PU . .
H17 H 0.4782 0.4577 0.5416 0.206 Uiso 0.50 1 calc PR . .
H18 H 0.3844 0.4163 0.4891 0.206 Uiso 0.50 1 calc PR . .
H19 H 0.5143 0.4241 0.4651 0.206 Uiso 0.50 1 calc PR . .


_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
C37 O9 1.22(2) . ?
C37 H13 0.9600 . ?
C37 H14 0.9600 . ?
C37 H15 0.9600 . ?
O8 C38 1.37(2) . ?
O8 H16 0.8200 . ?
O9 H20 0.8200 . ?
O7 H33 0.8594 . ?
O7 H34 0.8484 . ?
C1 N1 1.120(5) . ?
C1 C2 1.371(5) . ?
C2 C3 1.382(5) . ?
C2 C4 1.431(5) . ?
C3 N2 1.129(6) . ?
C4 C9 1.384(5) . ?
C4 C5 1.393(5) . ?
C5 C6 1.358(5) . ?
C5 H1 0.9300 . ?
C6 C7 1.388(5) . ?
C6 H2 0.9300 . ?
C7 C8 1.388(6) . ?
C7 C10 1.412(6) . ?
C8 C9 1.368(6) . ?
C8 H83 0.9300 . ?
C9 H94 0.9300 . ?
C10 C12 1.388(7) . ?
C10 C11 1.396(7) . ?
C11 N3 1.120(7) . ?
C12 N4 1.108(7) . ?
C13 N5 1.121(5) . ?
C13 C15 1.381(5) . ?
C14 N6 1.128(6) . ?
C14 C15 1.389(5) . ?
C15 C16 1.425(5) . ?
C16 C17 1.390(5) . ?
C16 C21 1.398(5) . ?
C17 C18 1.365(5) . ?
C17 H5 0.9300 . ?
C18 C19 1.403(5) . ?
C18 H6 0.9300 . ?
C19 C20 1.393(5) . ?
C19 C22 1.416(5) . ?
C20 C21 1.357(5) . ?
C20 H7 0.9300 . ?
C21 H8 0.9300 . ?
C22 C23 1.394(5) . ?
C22 C24 1.401(5) . ?
C23 N7 1.123(5) . ?
C24 N8 1.118(5) . ?
C25 N9 1.143(7) . ?
C25 C26 1.366(8) . ?
C26 C28 1.372(9) . ?
C26 C27 1.392(8) . ?
C27 N10 1.154(8) . ?
C28 C29 1.380(7) . ?
C28 C30 1.449(8) 3_766 ?
C29 C30 1.335(8) . ?
C29 H9 0.9300 . ?
C30 C28 1.449(8) 3_766 ?
C30 H10 0.9300 . ?
C31 N11 1.179(9) . ?
C31 C32 1.429(9) . ?
C32 C33 1.427(7) . ?
C32 C34 1.461(8) . ?
C33 N12 1.139(7) . ?
C34 C36 1.431(7) 3_676 ?
C34 C35 1.447(8) . ?
C35 C36 1.424(9) . ?
C35 H11 0.9300 . ?
C36 C34 1.431(7) 3_676 ?
C36 H12 0.9300 . ?
Lu1 O4 2.282(3) . ?
Lu1 O5 2.309(3) . ?
Lu1 O3 2.312(3) . ?
Lu1 N1 2.337(3) . ?
Lu1 O6 2.346(3) . ?
Lu1 O1 2.353(3) . ?
Lu1 O2 2.385(3) . ?
Lu1 N5 2.417(3) . ?
O1 H21 0.8630 . ?
O1 H22 0.8509 . ?
O2 H23 0.8301 . ?
O2 H24 0.8420 . ?
O3 H25 0.8464 . ?
O3 H26 0.8404 . ?
O4 H27 0.8555 . ?
O4 H28 0.8434 . ?
O5 H29 0.8534 . ?
O5 H30 0.8484 . ?
O6 H31 0.8564 . ?
O6 H32 0.8259 . ?
C38 H17 0.9600 . ?
C38 H18 0.9600 . ?
C38 H19 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
O9 C37 H13 109.5 . . ?
O9 C37 H14 109.5 . . ?
H13 C37 H14 109.5 . . ?
O9 C37 H15 109.5 . . ?
H13 C37 H15 109.5 . . ?
H14 C37 H15 109.5 . . ?
C38 O8 H16 109.5 . . ?
C37 O9 H20 109.5 . . ?
H33 O7 H34 108.6 . . ?
N1 C1 C2 176.9(4) . . ?
C1 C2 C3 116.3(4) . . ?
C1 C2 C4 120.1(3) . . ?
C3 C2 C4 123.5(3) . . ?
N2 C3 C2 178.9(5) . . ?
C9 C4 C5 116.2(4) . . ?
C9 C4 C2 122.3(3) . . ?
C5 C4 C2 121.6(3) . . ?
C6 C5 C4 122.2(3) . . ?
C6 C5 H1 118.9 . . ?
C4 C5 H1 118.9 . . ?
C5 C6 C7 121.9(4) . . ?
C5 C6 H2 119.0 . . ?
C7 C6 H2 119.0 . . ?
C6 C7 C8 115.8(4) . . ?
C6 C7 C10 121.0(4) . . ?
C8 C7 C10 123.2(4) . . ?
C9 C8 C7 122.5(4) . . ?
C9 C8 H83 118.7 . . ?
C7 C8 H83 118.7 . . ?
C8 C9 C4 121.4(4) . . ?
C8 C9 H94 119.3 . . ?
C4 C9 H94 119.3 . . ?
C12 C10 C11 114.7(4) . . ?
C12 C10 C7 122.7(4) . . ?
C11 C10 C7 122.6(4) . . ?
N3 C11 C10 179.8(7) . . ?
N4 C12 C10 178.5(7) . . ?
N5 C13 C15 178.9(5) . . ?
N6 C14 C15 178.9(5) . . ?
C13 C15 C14 114.9(3) . . ?
C13 C15 C16 122.7(3) . . ?
C14 C15 C16 122.4(3) . . ?
C17 C16 C21 116.1(3) . . ?
C17 C16 C15 123.0(3) . . ?
C21 C16 C15 120.9(3) . . ?
C18 C17 C16 121.5(3) . . ?
C18 C17 H5 119.2 . . ?
C16 C17 H5 119.2 . . ?
C17 C18 C19 122.5(3) . . ?
C17 C18 H6 118.7 . . ?
C19 C18 H6 118.7 . . ?
C20 C19 C18 115.3(3) . . ?
C20 C19 C22 121.1(3) . . ?
C18 C19 C22 123.6(3) . . ?
C21 C20 C19 122.4(3) . . ?
C21 C20 H7 118.8 . . ?
C19 C20 H7 118.8 . . ?
C20 C21 C16 122.1(3) . . ?
C20 C21 H8 118.9 . . ?
C16 C21 H8 118.9 . . ?
C23 C22 C24 114.6(4) . . ?
C23 C22 C19 123.0(3) . . ?
C24 C22 C19 122.4(3) . . ?
N7 C23 C22 179.0(5) . . ?
N8 C24 C22 179.0(5) . . ?
N9 C25 C26 178.2(7) . . ?
C25 C26 C28 124.9(5) . . ?
C25 C26 C27 113.9(6) . . ?
C28 C26 C27 121.1(5) . . ?
N10 C27 C26 178.9(9) . . ?
C26 C28 C29 125.0(5) . . ?
C26 C28 C30 122.2(5) . 3_766 ?
C29 C28 C30 112.8(6) . 3_766 ?
C30 C29 C28 125.5(6) . . ?
C30 C29 H9 117.3 . . ?
C28 C29 H9 117.3 . . ?
C29 C30 C28 121.7(5) . 3_766 ?
C29 C30 H10 119.1 . . ?
C28 C30 H10 119.1 3_766 . ?
N11 C31 C32 176.6(8) . . ?
C33 C32 C31 113.5(6) . . ?
C33 C32 C34 121.8(6) . . ?
C31 C32 C34 124.7(5) . . ?
N12 C33 C32 177.9(8) . . ?
C36 C34 C35 114.5(5) 3_676 . ?
C36 C34 C32 121.6(6) 3_676 . ?
C35 C34 C32 123.9(5) . . ?
C36 C35 C34 124.1(5) . . ?
C36 C35 H11 118.0 . . ?
C34 C35 H11 118.0 . . ?
C35 C36 C34 121.5(6) . 3_676 ?
C35 C36 H12 119.3 . . ?
C34 C36 H12 119.3 3_676 . ?
O4 Lu1 O5 111.51(13) . . ?
O4 Lu1 O3 78.86(13) . . ?
O5 Lu1 O3 67.97(11) . . ?
O4 Lu1 N1 141.21(12) . . ?
O5 Lu1 N1 74.94(11) . . ?
O3 Lu1 N1 134.41(12) . . ?
O4 Lu1 O6 68.29(11) . . ?
O5 Lu1 O6 79.61(13) . . ?
O3 Lu1 O6 120.40(13) . . ?
N1 Lu1 O6 75.91(12) . . ?
O4 Lu1 O1 144.41(10) . . ?
O5 Lu1 O1 84.49(13) . . ?
O3 Lu1 O1 78.41(13) . . ?
N1 Lu1 O1 72.43(11) . . ?
O6 Lu1 O1 147.30(11) . . ?
O4 Lu1 O2 83.02(12) . . ?
O5 Lu1 O2 143.59(10) . . ?
O3 Lu1 O2 148.28(11) . . ?
N1 Lu1 O2 73.70(11) . . ?
O6 Lu1 O2 75.24(11) . . ?
O1 Lu1 O2 103.04(11) . . ?
O4 Lu1 N5 74.83(11) . . ?
O5 Lu1 N5 141.70(12) . . ?
O3 Lu1 N5 76.96(12) . . ?
N1 Lu1 N5 124.81(11) . . ?
O6 Lu1 N5 133.63(12) . . ?
O1 Lu1 N5 73.60(11) . . ?
O2 Lu1 N5 73.27(11) . . ?
C1 N1 Lu1 176.2(3) . . ?
C13 N5 Lu1 170.0(3) . . ?
Lu1 O1 H21 125.0 . . ?
Lu1 O1 H22 119.0 . . ?
H21 O1 H22 107.0 . . ?
Lu1 O2 H23 115.0 . . ?
Lu1 O2 H24 125.8 . . ?
H23 O2 H24 111.9 . . ?
Lu1 O3 H25 129.5 . . ?
Lu1 O3 H26 117.3 . . ?
H25 O3 H26 111.3 . . ?
Lu1 O4 H27 134.1 . . ?
Lu1 O4 H28 114.5 . . ?
H27 O4 H28 110.2 . . ?
Lu1 O5 H29 130.4 . . ?
Lu1 O5 H30 117.3 . . ?
H29 O5 H30 108.2 . . ?
Lu1 O6 H31 121.2 . . ?
Lu1 O6 H32 124.7 . . ?
H31 O6 H32 112.5 . . ?
O8 C38 H17 109.5 . . ?
O8 C38 H18 109.5 . . ?
H17 C38 H18 109.5 . . ?
O8 C38 H19 109.5 . . ?
H17 C38 H19 109.5 . . ?
H18 C38 H19 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
O8 H16 N11 0.82 2.44 3.205(11) 156.6 4_676
O9 H20 N8 0.82 2.58 3.289(10) 145.1 3_656
O7 H34 N2 0.85 2.04 2.878(5) 169.1 1_455
O1 H21 N7 0.86 2.00 2.861(5) 173.7 3_556
O1 H22 N9 0.85 2.12 2.954(6) 164.8 4_565
O2 H24 N8 0.84 2.18 3.002(5) 167.1 3_656
O3 H25 O7 0.85 2.02 2.861(5) 178.8 .
O3 H26 N10 0.84 1.92 2.756(8) 178.4 1_455
O4 H27 O8 0.86 1.84 2.698(8) 176.5 .
O4 H28 N2 0.84 2.26 2.889(6) 131.0 4_566
O4 H28 N10 0.84 2.65 3.235(7) 127.6 1_455
O5 H29 N12 0.85 2.02 2.872(6) 173.7 2_545
O5 H30 N6 0.85 1.89 2.702(5) 158.5 4_665
O6 H31 O9 0.86 1.87 2.726(11) 175.4 .
O6 H32 N4 0.83 2.04 2.819(6) 157.3 2_655

_diffrn_measured_fraction_theta_max 0.900
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.900
_refine_diff_density_max         1.664
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.102

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_zjw-5
_audit_block_doi                 10.5517/ccnzhmq
_database_code_depnum_ccdc_archive 'CCDC 625134'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/b909213g 2009
_audit_update_record             
;
2006-10-24 deposited with the CCDC.
2015-08-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
2(C24 H20 Er N8 O6), 2(C12 H4 N4), C H4 O, C H5 O, 2(H2 O)
;
_chemical_formula_sum            'C37 H30.50 Er N12 O8'
_chemical_formula_weight         938.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n '
_symmetry_space_group_name_Hall  '-P 2yn '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.053(2)
_cell_length_b                   25.483(5)
_cell_length_c                   15.384(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.63(3)
_cell_angle_gamma                90.00
_cell_volume                     4151.9(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    30293
_cell_measurement_theta_min      5.98
_cell_measurement_theta_max      54.92

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.36
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1874
_exptl_absorpt_coefficient_mu    2.085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4552
_exptl_absorpt_correction_T_max  0.5207
_exptl_absorpt_process_details   
;
Higashi, T. (1995). Program for
Absorption Correction Correction. Rigaku Corporation, Tokyo, Japan.
;

_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       'ω scans'
_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            40103
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         27.46
_reflns_number_total             9474
_reflns_number_gt                7461
_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, 1997)'
_computing_structure_refinement  SHELXL-97

_refine_special_details          
;
1. The 'isor' comounds were used to restrain ADPs, such as
isor 0.001 n11
isor 0.001 n10
isor 0.001 c38
isor 0.001 c37
isor 0.001 o9
isor 0.001 o8

Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² 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/[σ²(Fo²)+(0.0472P)²+8.2066P] where P=(Fo²+2Fc²)/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         9474
_refine_ls_number_parameters     545
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.1000
_refine_ls_wR_factor_gt          0.0925
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
C37 C 0.8684(18) 0.2556(7) 0.4207(12) 0.096(5) Uani 0.50 1 d PU . .
H13 H 0.8275 0.2777 0.3703 0.143 Uiso 0.50 1 calc PR . .
H14 H 0.8527 0.2195 0.4033 0.143 Uiso 0.50 1 calc PR . .
H15 H 0.9576 0.2621 0.4383 0.143 Uiso 0.50 1 calc PR . .
O8 O 0.5174(9) 0.3864(4) 0.5750(6) 0.070(2) Uani 0.50 1 d PU . .
H16 H 0.5749 0.3995 0.6152 0.104 Uiso 0.50 1 calc PR . .
O9 O 0.8235(10) 0.2658(4) 0.4893(7) 0.072(2) Uani 0.50 1 d PU . .
H20 H 0.8046 0.2382 0.5096 0.109 Uiso 1 1 calc R . .
O7 O 0.0545(3) 0.29016(14) 0.1940(2) 0.0494(8) Uani 1 1 d . . .
H33 H 0.0258 0.3201 0.2043 0.074 Uiso 1 1 d R . .
H34 H -0.0021 0.2670 0.1885 0.074 Uiso 1 1 d R . .
C1 C 0.6114(5) 0.18287(17) 0.2887(3) 0.0367(10) Uani 1 1 d . . .
C2 C 0.6936(5) 0.16070(17) 0.2438(3) 0.0360(10) Uani 1 1 d . . .
C3 C 0.7754(5) 0.19484(19) 0.2166(4) 0.0457(12) Uani 1 1 d . . .
C4 C 0.6956(4) 0.10520(17) 0.2314(3) 0.0330(9) Uani 1 1 d . . .
C5 C 0.6130(4) 0.07175(18) 0.2609(3) 0.0355(10) Uani 1 1 d . . .
H1 H 0.5571 0.0863 0.2893 0.043 Uiso 1 1 calc R . .
C6 C 0.6130(4) 0.01908(18) 0.2488(3) 0.0359(10) Uani 1 1 d . . .
H2 H 0.5565 -0.0015 0.2684 0.043 Uiso 1 1 calc R . .
C7 C 0.6975(4) -0.00534(18) 0.2071(3) 0.0346(9) Uani 1 1 d . . .
C8 C 0.7804(4) 0.02782(19) 0.1775(3) 0.0364(10) Uani 1 1 d . . .
H83 H 0.8370 0.0131 0.1499 0.044 Uiso 1 1 calc R . .
C9 C 0.7792(4) 0.08139(17) 0.1888(3) 0.0320(9) Uani 1 1 d . . .
H94 H 0.8342 0.1022 0.1681 0.038 Uiso 1 1 calc R . .
C10 C 0.6973(5) -0.06003(19) 0.1965(4) 0.0432(11) Uani 1 1 d . . .
C11 C 0.6129(6) -0.0931(2) 0.2259(4) 0.0516(13) Uani 1 1 d . . .
C12 C 0.7825(6) -0.0859(2) 0.1582(4) 0.0575(15) Uani 1 1 d . . .
C13 C 0.2339(4) 0.17095(15) 0.5432(3) 0.0276(8) Uani 1 1 d . . .
C14 C 0.0820(5) 0.18365(18) 0.6254(3) 0.0404(11) Uani 1 1 d . . .
C15 C 0.1515(4) 0.14826(16) 0.5878(3) 0.0297(9) Uani 1 1 d . . .
C16 C 0.1362(4) 0.09297(16) 0.5918(3) 0.0272(8) Uani 1 1 d . . .
C17 C 0.0463(4) 0.06972(16) 0.6312(3) 0.0279(8) Uani 1 1 d . . .
H5 H -0.0025 0.0912 0.6568 0.034 Uiso 1 1 calc R . .
C18 C 0.0311(4) 0.01673(16) 0.6318(3) 0.0279(8) Uani 1 1 d . . .
H6 H -0.0281 0.0027 0.6578 0.033 Uiso 1 1 calc R . .
C19 C 0.1036(4) -0.01797(16) 0.5937(3) 0.0260(8) Uani 1 1 d . . .
C20 C 0.1942(4) 0.00566(16) 0.5555(3) 0.0308(9) Uani 1 1 d . . .
H7 H 0.2438 -0.0157 0.5305 0.037 Uiso 1 1 calc R . .
C21 C 0.2095(4) 0.05857(17) 0.5550(3) 0.0301(9) Uani 1 1 d . . .
H8 H 0.2695 0.0726 0.5298 0.036 Uiso 1 1 calc R . .
C22 C 0.0883(4) -0.07281(17) 0.5923(3) 0.0305(9) Uani 1 1 d . . .
C23 C -0.0023(4) -0.09828(17) 0.6279(3) 0.0347(10) Uani 1 1 d . . .
C24 C 0.1614(4) -0.10629(17) 0.5525(3) 0.0339(9) Uani 1 1 d . . .
C25 C 0.9004(7) 0.3754(3) 0.5962(4) 0.0735(19) Uani 1 1 d . . .
C26 C 0.9767(6) 0.3944(3) 0.5442(4) 0.0673(18) Uani 1 1 d . . .
C27 C 1.0520(8) 0.3551(4) 0.5192(5) 0.098(3) Uani 1 1 d . . .
C28 C 0.9883(6) 0.4447(3) 0.5195(4) 0.071(2) Uani 1 1 d . . .
C29 C 1.0731(6) 0.4639(3) 0.4755(4) 0.0683(19) Uani 1 1 d . . .
H9 H 1.1253 0.4393 0.4598 0.082 Uiso 1 1 calc R . .
C30 C 1.0880(5) 0.5134(3) 0.4536(4) 0.0661(19) Uani 1 1 d . . .
H10 H 1.1454 0.5219 0.4218 0.079 Uiso 1 1 calc R . .
C31 C 0.2597(9) 1.0116(3) 0.2715(7) 0.090(3) Uani 1 1 d . . .
C32 C 0.3180(7) 0.9738(2) 0.3349(6) 0.074(2) Uani 1 1 d . . .
C33 C 0.2784(7) 0.9211(3) 0.3119(6) 0.079(2) Uani 1 1 d . . .
C34 C 0.4074(7) 0.9870(2) 0.4154(5) 0.066(2) Uani 1 1 d . . .
C35 C 0.4701(7) 0.9479(2) 0.4814(6) 0.075(2) Uani 1 1 d . . .
H11 H 0.4510 0.9127 0.4682 0.090 Uiso 1 1 calc R . .
C36 C 0.5554(7) 0.9603(2) 0.5616(6) 0.074(2) Uani 1 1 d . . .
H12 H 0.5901 0.9336 0.6024 0.088 Uiso 1 1 calc R . .
Er1 Er 0.407016(17) 0.237438(7) 0.407114(12) 0.02523(7) Uani 1 1 d . . .
N1 N 0.5433(4) 0.19877(14) 0.3263(3) 0.0379(9) Uani 1 1 d . . .
N2 N 0.8423(6) 0.2224(2) 0.1936(4) 0.0661(15) Uani 1 1 d . . .
N3 N 0.5456(6) -0.1194(2) 0.2491(4) 0.0779(17) Uani 1 1 d . . .
N4 N 0.8515(7) -0.1077(2) 0.1287(5) 0.094(2) Uani 1 1 d . . .
N5 N 0.2986(4) 0.18944(14) 0.5055(2) 0.0350(8) Uani 1 1 d . . .
N6 N 0.0236(5) 0.2118(2) 0.6554(4) 0.0696(16) Uani 1 1 d . . .
N7 N -0.0745(5) -0.11898(18) 0.6559(3) 0.0535(12) Uani 1 1 d . . .
N8 N 0.2204(5) -0.13308(17) 0.5217(3) 0.0513(11) Uani 1 1 d . . .
N9 N 0.8387(6) 0.3602(3) 0.6419(5) 0.095(2) Uani 1 1 d . . .
N10 N 1.1155(8) 0.3235(3) 0.4974(5) 0.113(2) Uani 1 1 d U . .
N11 N 0.2046(9) 1.0410(4) 0.2167(6) 0.125(3) Uani 1 1 d U . .
N12 N 0.2443(7) 0.8797(2) 0.2930(5) 0.095(2) Uani 1 1 d . . .
O1 O 0.2991(4) 0.16725(14) 0.3210(2) 0.0541(10) Uani 1 1 d . . .
H21 H 0.2328 0.1543 0.3303 0.081 Uiso 1 1 d R . .
H22 H 0.2943 0.1658 0.2656 0.081 Uiso 1 1 d R . .
O2 O 0.5652(3) 0.19316(13) 0.5163(2) 0.0439(8) Uani 1 1 d . . .
H23 H 0.5702 0.2011 0.5697 0.066 Uiso 1 1 d R . .
H24 H 0.6307 0.1800 0.5093 0.066 Uiso 1 1 d R . .
O3 O 0.2056(4) 0.27198(17) 0.3673(2) 0.0604(12) Uani 1 1 d . . .
H25 H 0.1468 0.2703 0.3178 0.091 Uiso 1 1 d R . .
H26 H 0.1802 0.2887 0.4064 0.091 Uiso 1 1 d R . .
O4 O 0.4053(4) 0.29339(14) 0.5244(2) 0.0559(10) Uani 1 1 d . . .
H27 H 0.4442 0.3219 0.5385 0.084 Uiso 1 1 d R . .
H28 H 0.3513 0.2884 0.5524 0.084 Uiso 1 1 d R . .
O5 O 0.3717(3) 0.28175(15) 0.2707(2) 0.0528(10) Uani 1 1 d . . .
H29 H 0.3420 0.3130 0.2626 0.079 Uiso 1 1 d R . .
H30 H 0.4190 0.2779 0.2357 0.079 Uiso 1 1 d R . .
O6 O 0.5800(3) 0.29499(13) 0.4329(3) 0.0513(9) Uani 1 1 d . . .
H31 H 0.6553 0.2835 0.4512 0.077 Uiso 1 1 d R . .
H32 H 0.5763 0.3234 0.4056 0.077 Uiso 1 1 d R . .
C38 C 0.458(2) 0.4283(8) 0.5044(14) 0.123(7) Uani 0.50 1 d PU . .
H17 H 0.4502 0.4606 0.5347 0.185 Uiso 0.50 1 calc PR . .
H18 H 0.3754 0.4169 0.4693 0.185 Uiso 0.50 1 calc PR . .
H19 H 0.5100 0.4338 0.4650 0.185 Uiso 0.50 1 calc PR . .


_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
C37 O9 1.314(19) . ?
C37 H13 0.9600 . ?
C37 H14 0.9600 . ?
C37 H15 0.9600 . ?
O8 C38 1.53(2) . ?
O8 H16 0.8200 . ?
O9 H20 0.8200 . ?
O7 H33 0.8579 . ?
O7 H34 0.8463 . ?
C1 N1 1.146(5) . ?
C1 C2 1.407(6) . ?
C2 C3 1.403(7) . ?
C2 C4 1.428(6) . ?
C3 N2 1.146(7) . ?
C4 C9 1.414(6) . ?
C4 C5 1.416(6) . ?
C5 C6 1.355(6) . ?
C5 H1 0.9300 . ?
C6 C7 1.419(6) . ?
C6 H2 0.9300 . ?
C7 C10 1.403(6) . ?
C7 C8 1.414(7) . ?
C8 C9 1.377(6) . ?
C8 H83 0.9300 . ?
C9 H94 0.9300 . ?
C10 C12 1.410(7) . ?
C10 C11 1.423(8) . ?
C11 N3 1.132(8) . ?
C12 N4 1.137(8) . ?
C13 N5 1.143(5) . ?
C13 C15 1.412(5) . ?
C14 N6 1.146(6) . ?
C14 C15 1.412(6) . ?
C15 C16 1.423(6) . ?
C16 C21 1.417(6) . ?
C16 C17 1.432(5) . ?
C17 C18 1.361(6) . ?
C17 H5 0.9300 . ?
C18 C19 1.427(6) . ?
C18 H6 0.9300 . ?
C19 C22 1.407(6) . ?
C19 C20 1.431(5) . ?
C20 C21 1.359(6) . ?
C20 H7 0.9300 . ?
C21 H8 0.9300 . ?
C22 C23 1.427(6) . ?
C22 C24 1.428(6) . ?
C23 N7 1.139(6) . ?
C24 N8 1.138(6) . ?
C25 N9 1.176(8) . ?
C25 C26 1.405(9) . ?
C26 C28 1.354(10) . ?
C26 C27 1.424(10) . ?
C27 N10 1.178(10) . ?
C28 C29 1.393(9) . ?
C28 C30 1.490(9) 3_766 ?
C29 C30 1.328(10) . ?
C29 H9 0.9300 . ?
C30 C28 1.490(9) 3_766 ?
C30 H10 0.9300 . ?
C31 N11 1.162(11) . ?
C31 C32 1.389(12) . ?
C32 C34 1.387(10) . ?
C32 C33 1.427(9) . ?
C33 N12 1.128(8) . ?
C34 C36 1.419(8) 3_676 ?
C34 C35 1.450(11) . ?
C35 C36 1.358(11) . ?
C35 H11 0.9300 . ?
C36 C34 1.419(8) 3_676 ?
C36 H12 0.9300 . ?
Er1 O4 2.304(3) . ?
Er1 O3 2.307(3) . ?
Er1 O5 2.316(3) . ?
Er1 O2 2.339(3) . ?
Er1 O1 2.339(3) . ?
Er1 O6 2.352(3) . ?
Er1 N1 2.421(4) . ?
Er1 N5 2.502(3) . ?
O1 H21 0.8515 . ?
O1 H22 0.8392 . ?
O2 H23 0.8324 . ?
O2 H24 0.8323 . ?
O3 H25 0.8490 . ?
O3 H26 0.8475 . ?
O4 H27 0.8392 . ?
O4 H28 0.8406 . ?
O5 H29 0.8581 . ?
O5 H30 0.8562 . ?
O6 H31 0.8502 . ?
O6 H32 0.8318 . ?
C38 H17 0.9600 . ?
C38 H18 0.9600 . ?
C38 H19 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
O9 C37 H13 109.5 . . ?
O9 C37 H14 109.5 . . ?
H13 C37 H14 109.5 . . ?
O9 C37 H15 109.5 . . ?
H13 C37 H15 109.5 . . ?
H14 C37 H15 109.5 . . ?
C38 O8 H16 109.5 . . ?
C37 O9 H20 109.5 . . ?
H33 O7 H34 109.6 . . ?
N1 C1 C2 177.0(5) . . ?
C3 C2 C1 117.4(4) . . ?
C3 C2 C4 122.6(4) . . ?
C1 C2 C4 120.0(4) . . ?
N2 C3 C2 179.3(6) . . ?
C9 C4 C5 117.2(4) . . ?
C9 C4 C2 121.6(4) . . ?
C5 C4 C2 121.2(4) . . ?
C6 C5 C4 121.8(4) . . ?
C6 C5 H1 119.1 . . ?
C4 C5 H1 119.1 . . ?
C5 C6 C7 121.5(4) . . ?
C5 C6 H2 119.2 . . ?
C7 C6 H2 119.2 . . ?
C10 C7 C8 122.4(4) . . ?
C10 C7 C6 120.6(4) . . ?
C8 C7 C6 117.0(4) . . ?
C9 C8 C7 121.4(4) . . ?
C9 C8 H83 119.3 . . ?
C7 C8 H83 119.3 . . ?
C8 C9 C4 121.0(4) . . ?
C8 C9 H94 119.5 . . ?
C4 C9 H94 119.5 . . ?
C7 C10 C12 122.2(5) . . ?
C7 C10 C11 122.0(5) . . ?
C12 C10 C11 115.7(5) . . ?
N3 C11 C10 179.8(8) . . ?
N4 C12 C10 178.4(8) . . ?
N5 C13 C15 178.6(5) . . ?
N6 C14 C15 178.7(6) . . ?
C14 C15 C13 116.1(4) . . ?
C14 C15 C16 121.9(4) . . ?
C13 C15 C16 121.9(4) . . ?
C21 C16 C15 120.4(4) . . ?
C21 C16 C17 117.3(4) . . ?
C15 C16 C17 122.3(4) . . ?
C18 C17 C16 121.0(4) . . ?
C18 C17 H5 119.5 . . ?
C16 C17 H5 119.5 . . ?
C17 C18 C19 121.8(4) . . ?
C17 C18 H6 119.1 . . ?
C19 C18 H6 119.1 . . ?
C22 C19 C18 122.8(4) . . ?
C22 C19 C20 120.5(4) . . ?
C18 C19 C20 116.7(4) . . ?
C21 C20 C19 121.5(4) . . ?
C21 C20 H7 119.3 . . ?
C19 C20 H7 119.3 . . ?
C20 C21 C16 121.7(4) . . ?
C20 C21 H8 119.2 . . ?
C16 C21 H8 119.2 . . ?
C19 C22 C23 122.7(4) . . ?
C19 C22 C24 121.3(4) . . ?
C23 C22 C24 116.0(4) . . ?
N7 C23 C22 179.4(5) . . ?
N8 C24 C22 179.3(5) . . ?
N9 C25 C26 178.0(9) . . ?
C28 C26 C25 127.4(7) . . ?
C28 C26 C27 118.8(7) . . ?
C25 C26 C27 113.8(7) . . ?
N10 C27 C26 178.3(11) . . ?
C26 C28 C29 126.9(7) . . ?
C26 C28 C30 119.6(6) . 3_766 ?
C29 C28 C30 113.4(7) . 3_766 ?
C30 C29 C28 127.4(7) . . ?
C30 C29 H9 116.3 . . ?
C28 C29 H9 116.3 . . ?
C29 C30 C28 119.2(6) . 3_766 ?
C29 C30 H10 120.4 . . ?
C28 C30 H10 120.4 3_766 . ?
N11 C31 C32 175.7(10) . . ?
C34 C32 C31 121.8(7) . . ?
C34 C32 C33 122.6(7) . . ?
C31 C32 C33 115.5(8) . . ?
N12 C33 C32 178.4(9) . . ?
C32 C34 C36 122.2(7) . 3_676 ?
C32 C34 C35 122.3(6) . . ?
C36 C34 C35 115.5(7) 3_676 . ?
C36 C35 C34 123.0(6) . . ?
C36 C35 H11 118.5 . . ?
C34 C35 H11 118.5 . . ?
C35 C36 C34 121.5(7) . 3_676 ?
C35 C36 H12 119.2 . . ?
C34 C36 H12 119.2 3_676 . ?
O4 Er1 O3 75.42(15) . . ?
O4 Er1 O5 111.78(14) . . ?
O3 Er1 O5 70.99(12) . . ?
O4 Er1 O2 84.71(14) . . ?
O3 Er1 O2 147.19(12) . . ?
O5 Er1 O2 141.58(12) . . ?
O4 Er1 O1 143.08(12) . . ?
O3 Er1 O1 81.06(15) . . ?
O5 Er1 O1 86.17(14) . . ?
O2 Er1 O1 101.14(13) . . ?
O4 Er1 O6 70.77(13) . . ?
O3 Er1 O6 118.88(15) . . ?
O5 Er1 O6 76.50(14) . . ?
O2 Er1 O6 77.01(13) . . ?
O1 Er1 O6 146.15(12) . . ?
O4 Er1 N1 143.13(14) . . ?
O3 Er1 N1 135.55(13) . . ?
O5 Er1 N1 72.59(12) . . ?
O2 Er1 N1 74.08(12) . . ?
O1 Er1 N1 71.90(13) . . ?
O6 Er1 N1 75.21(13) . . ?
O4 Er1 N5 73.52(12) . . ?
O3 Er1 N5 75.77(13) . . ?
O5 Er1 N5 143.21(13) . . ?
O2 Er1 N5 73.66(12) . . ?
O1 Er1 N5 73.37(12) . . ?
O6 Er1 N5 135.25(13) . . ?
N1 Er1 N5 126.02(12) . . ?
C1 N1 Er1 176.4(4) . . ?
C13 N5 Er1 170.3(4) . . ?
Er1 O1 H21 121.6 . . ?
Er1 O1 H22 118.8 . . ?
H21 O1 H22 110.3 . . ?
Er1 O2 H23 114.6 . . ?
Er1 O2 H24 126.8 . . ?
H23 O2 H24 114.3 . . ?
Er1 O3 H25 130.6 . . ?
Er1 O3 H26 119.6 . . ?
H25 O3 H26 109.7 . . ?
Er1 O4 H27 128.2 . . ?
Er1 O4 H28 118.4 . . ?
H27 O4 H28 112.6 . . ?
Er1 O5 H29 122.8 . . ?
Er1 O5 H30 122.6 . . ?
H29 O5 H30 107.1 . . ?
Er1 O6 H31 120.8 . . ?
Er1 O6 H32 122.5 . . ?
H31 O6 H32 111.7 . . ?
O8 C38 H17 109.5 . . ?
O8 C38 H18 109.5 . . ?
H17 C38 H18 109.5 . . ?
O8 C38 H19 109.5 . . ?
H17 C38 H19 109.5 . . ?
H18 C38 H19 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
O6 H32 N4 0.83 2.06 2.834(6) 154.7 2_655
O6 H31 O9 0.85 1.84 2.686(11) 174.0 .
O5 H30 N6 0.86 1.94 2.773(5) 165.5 4_665
O5 H29 N12 0.86 2.02 2.849(7) 163.8 2_545
O4 H28 N10 0.84 2.65 3.203(9) 124.3 1_455
O4 H28 N2 0.84 2.22 2.909(6) 139.3 4_566
O4 H27 O8 0.84 1.85 2.684(10) 174.2 .
O3 H26 N10 0.85 1.96 2.804(9) 176.4 1_455
O3 H25 O7 0.85 1.95 2.750(5) 156.0 .
O2 H24 N8 0.83 2.19 3.016(6) 169.0 3_656
O1 H22 N9 0.84 2.20 2.994(7) 158.0 4_565
O1 H21 N7 0.85 2.03 2.882(6) 175.1 3_556
O7 H34 N2 0.85 2.08 2.912(6) 166.4 1_455
O8 H16 N11 0.82 2.35 3.142(14) 163.4 4_676

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.700
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.112
