# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1041890'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;

#================================================================   

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H26 Cl2 Eu K N2 O11'
_chemical_formula_weight         732.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   Pc

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

_cell_length_a                   7.671(5)
_cell_length_b                   6.820(5)
_cell_length_c                   25.658(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.011(10)
_cell_angle_gamma                90.00
_cell_volume                     1339.2(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2269
_cell_measurement_theta_min      1.59
_cell_measurement_theta_max      24.84

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             728
_exptl_absorpt_coefficient_mu    2.755
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6827
_exptl_absorpt_correction_T_max  0.7334
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2269
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.59
_diffrn_reflns_theta_max         24.84
_reflns_number_total             2269
_reflns_number_gt                1897
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0217P)²+86.2274P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(9)
_refine_ls_number_reflns         2269
_refine_ls_number_parameters     334
_refine_ls_number_restraints     252
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0883
_refine_ls_wR_factor_ref         0.2189
_refine_ls_wR_factor_gt          0.1973
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.034
_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
Eu1 Eu 0.4473(2) 0.53412(13) 0.73131(12) 0.0290(2) Uani 1 1 d . . .
O1 O 0.350(2) 0.645(3) 0.8080(6) 0.044(4) Uani 1 1 d U . .
O4 O 0.5354(18) 0.651(2) 0.6497(5) 0.026(3) Uani 1 1 d U . .
O2 O 0.4287(18) 0.458(2) 0.8814(6) 0.039(4) Uani 1 1 d U . .
H2 H 0.4639 0.3813 0.8600 0.058 Uiso 1 1 calc R . .
C17 C 0.599(3) 0.737(3) 0.5175(8) 0.0278(13) Uani 1 1 d U . .
H17A H 0.5417 0.6302 0.5017 0.033 Uiso 1 1 calc R . .
C8 C 0.271(3) 0.772(3) 0.8900(8) 0.027(4) Uani 1 1 d U . .
N1 N 0.152(2) 1.078(3) 0.8936(7) 0.039(4) Uani 1 1 d U . .
C18 C 0.703(3) 0.908(3) 0.5920(9) 0.035(4) Uani 1 1 d U . .
H18A H 0.7288 0.9084 0.6280 0.042 Uiso 1 1 calc R . .
C15 C 0.733(2) 1.0738(18) 0.5077(6) 0.033(4) Uani 1 1 d DU . .
C9 C 0.347(3) 0.610(4) 0.8562(10) 0.046(5) Uani 1 1 d U . .
N2 N 0.746(2) 1.073(3) 0.5638(7) 0.0261(14) Uani 1 1 d U . .
C6 C 0.234(3) 0.907(4) 0.9711(9) 0.040(5) Uani 1 1 d U . .
C13 C 0.783(3) 1.220(2) 0.4262(5) 0.040(5) Uani 1 1 d DU . .
H13A H 0.8204 1.3213 0.4053 0.048 Uiso 1 1 calc R . .
C3 C 0.108(3) 1.235(2) 0.9741(5) 0.046(5) Uani 1 1 d DU . .
H3A H 0.0580 1.3427 0.9564 0.055 Uiso 1 1 calc R . .
C7 C 0.216(3) 0.943(3) 0.8690(8) 0.024(4) Uani 1 1 d U . .
H7A H 0.2274 0.9619 0.8335 0.029 Uiso 1 1 calc R . .
C16 C 0.666(2) 0.909(2) 0.4833(4) 0.016(3) Uani 1 1 d DU . .
C14 C 0.781(3) 1.233(3) 0.4792(5) 0.043(5) Uani 1 1 d DU . .
H14A H 0.8118 1.3503 0.4961 0.051 Uiso 1 1 calc R . .
C5 C 0.251(3) 0.927(2) 1.0303(8) 0.052(5) Uani 1 1 d DU . .
H5A H 0.2984 0.8224 1.0498 0.062 Uiso 1 1 calc R . .
C2 C 0.129(2) 1.241(2) 1.0273(5) 0.030(4) Uani 1 1 d DU . .
H2A H 0.0945 1.3531 1.0445 0.037 Uiso 1 1 calc R . .
C4 C 0.157(3) 1.076(2) 0.9456(8) 0.034(4) Uani 1 1 d DU . .
C1 C 0.200(2) 1.089(2) 1.0564(7) 0.040(5) Uani 1 1 d DU . .
H1A H 0.2120 1.0953 1.0926 0.048 Uiso 1 1 calc R . .
C19 C 0.624(3) 0.747(4) 0.5697(9) 0.033(5) Uani 1 1 d U . .
C11 C 0.659(2) 0.886(2) 0.4309(4) 0.018(4) Uani 1 1 d DU . .
H11A H 0.6143 0.7752 0.4135 0.021 Uiso 1 1 calc R . .
C6A C 0.282(3) 0.758(3) 0.9453(9) 0.030(3) Uani 1 1 d U . .
H6AA H 0.3222 0.6447 0.9622 0.036 Uiso 1 1 calc R . .
K1 K 0.9382(6) 0.4141(9) 0.8455(2) 0.0453(16) Uani 1 1 d U . .
Cl2 Cl -0.0485(13) 0.9926(7) 0.7397(3) 0.0537(18) Uani 1 1 d U . .
O3 O 0.5170(18) 0.441(2) 0.5849(5) 0.027(3) Uani 1 1 d U . .
C12 C 0.726(3) 1.044(2) 0.4068(8) 0.045(5) Uani 1 1 d DU . .
H12A H 0.7334 1.0291 0.3710 0.054 Uiso 1 1 calc R . .
C10 C 0.545(3) 0.599(3) 0.6041(8) 0.025(4) Uani 1 1 d U . .
Cl1 Cl 0.9582(9) 0.4024(12) 0.6163(3) 0.053(2) Uani 1 1 d U . .
O1W O 0.6939(19) 0.687(2) 0.7809(6) 0.037(4) Uani 1 1 d U . .
H1WA H 0.6483 0.7833 0.8042 0.045 Uiso 1 1 calc R . .
H1WB H 0.7624 0.7575 0.7566 0.045 Uiso 1 1 calc R . .
O2W O 0.6805(18) 0.318(2) 0.6977(6) 0.0341(13) Uani 1 1 d U . .
H2WA H 0.6467 0.2796 0.6625 0.051 Uiso 1 1 d R . .
H2WB H 0.6953 0.2039 0.7193 0.051 Uiso 1 1 d R . .
O3W O 0.173(2) 0.666(3) 0.6981(7) 0.0473(14) Uani 1 1 d U . .
H3WA H 0.1416 0.6108 0.6643 0.071 Uiso 1 1 d R . .
H3WB H 0.1833 0.8056 0.6951 0.071 Uiso 1 1 d R . .
O4W O 0.202(2) 0.343(3) 0.7560(7) 0.052(4) Uani 1 1 d U . .
H4WB H 0.1760 0.3771 0.7910 0.077 Uiso 1 1 d R . .
H4WC H 0.2321 0.2066 0.7547 0.077 Uiso 1 1 d R . .
O5W O 0.456(4) 0.9154(16) 0.7350(11) 0.039(3) Uani 1 1 d U . .
H5WA H 0.3610 0.9679 0.7130 0.059 Uiso 1 1 d R . .
H5WB H 0.5648 0.9612 0.7231 0.059 Uiso 1 1 d R . .
O6W O 0.5741(18) 0.293(2) 0.8006(6) 0.0312(13) Uani 1 1 d U . .
H6WA H 0.5807 0.1635 0.7851 0.037 Uiso 1 1 calc R . .
H6WB H 0.4963 0.2849 0.8287 0.037 Uiso 1 1 calc R . .
O7 O 0.3506(18) 0.272(2) 0.6671(6) 0.031(4) Uani 1 1 d . . .
H7 H 0.2491 0.3159 0.6463 0.046 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
Eu1 O1 2.282(17) . ?
Eu1 O4 2.383(14) . ?
Eu1 O3W 2.392(17) . ?
Eu1 O4W 2.409(19) . ?
Eu1 O1W 2.439(15) . ?
Eu1 O7 2.510(16) . ?
Eu1 O2W 2.515(15) . ?
Eu1 O6W 2.564(15) . ?
Eu1 O5W 2.603(11) . ?
Eu1 K1 4.679(6) . ?
O1 C9 1.26(3) . ?
O4 C10 1.23(3) . ?
O2 C9 1.35(3) . ?
O2 H2 0.8200 . ?
C17 C19 1.34(3) . ?
C17 C16 1.57(3) . ?
C17 H17A 0.9300 . ?
C8 C7 1.34(3) . ?
C8 C6A 1.42(3) . ?
C8 C9 1.54(3) . ?
N1 C7 1.24(3) . ?
N1 C4 1.33(3) . ?
N1 K1 3.03(2) 1_465 ?
C18 C19 1.36(3) . ?
C18 N2 1.39(3) . ?
C18 H18A 0.9300 . ?
C15 C16 1.365(15) . ?
C15 C14 1.377(16) . ?
C15 N2 1.44(2) . ?
C9 K1 3.40(3) 1_455 ?
C6 C6A 1.28(3) . ?
C6 C4 1.43(3) . ?
C6 C5 1.52(3) . ?
C13 C12 1.361(16) . ?
C13 C14 1.365(15) . ?
C13 K1 3.503(16) 2_574 ?
C13 H13A 0.9300 . ?
C3 C2 1.365(14) . ?
C3 C4 1.378(16) . ?
C3 H3A 0.9300 . ?
C7 H7A 0.9300 . ?
C16 C11 1.352(14) . ?
C14 H14A 0.9300 . ?
C5 C1 1.363(16) . ?
C5 H5A 0.9300 . ?
C2 C1 1.369(16) . ?
C2 H2A 0.9300 . ?
C1 H1A 0.9300 . ?
C19 C10 1.50(3) . ?
C11 C12 1.361(15) . ?
C11 H11A 0.9300 . ?
C6A H6AA 0.9300 . ?
K1 N1 3.03(2) 1_645 ?
K1 O1W 3.049(16) . ?
K1 O6W 3.060(15) . ?
K1 O4W 3.202(19) 1_655 ?
K1 C9 3.40(3) 1_655 ?
K1 C13 3.503(16) 2_575 ?
O3 C10 1.19(3) . ?
C12 H12A 0.9300 . ?
O1W H1WA 0.9700 . ?
O1W H1WB 0.9700 . ?
O2W H2WA 0.9602 . ?
O2W H2WB 0.9600 . ?
O3W H3WA 0.9602 . ?
O3W H3WB 0.9600 . ?
O4W K1 3.202(19) 1_455 ?
O4W H4WB 0.9599 . ?
O4W H4WC 0.9600 . ?
O5W H5WA 0.9600 . ?
O5W H5WB 0.9601 . ?
O6W H6WA 0.9700 . ?
O6W H6WB 0.9700 . ?
O7 H7 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 O4 140.9(5) . . ?
O1 Eu1 O3W 81.4(6) . . ?
O4 Eu1 O3W 81.8(5) . . ?
O1 Eu1 O4W 69.1(6) . . ?
O4 Eu1 O4W 133.5(6) . . ?
O3W Eu1 O4W 67.2(6) . . ?
O1 Eu1 O1W 72.4(6) . . ?
O4 Eu1 O1W 93.3(5) . . ?
O3W Eu1 O1W 131.1(5) . . ?
O4W Eu1 O1W 133.3(6) . . ?
O1 Eu1 O7 134.7(5) . . ?
O4 Eu1 O7 75.6(5) . . ?
O3W Eu1 O7 79.7(6) . . ?
O4W Eu1 O7 65.6(6) . . ?
O1W Eu1 O7 146.1(5) . . ?
O1 Eu1 O2W 140.6(5) . . ?
O4 Eu1 O2W 69.1(5) . . ?
O3W Eu1 O2W 136.7(5) . . ?
O4W Eu1 O2W 111.2(5) . . ?
O1W Eu1 O2W 83.4(5) . . ?
O7 Eu1 O2W 62.8(5) . . ?
O1 Eu1 O6W 75.3(6) . . ?
O4 Eu1 O6W 135.0(5) . . ?
O3W Eu1 O6W 140.4(5) . . ?
O4W Eu1 O6W 74.7(5) . . ?
O1W Eu1 O6W 70.8(5) . . ?
O7 Eu1 O6W 94.5(4) . . ?
O2W Eu1 O6W 67.5(5) . . ?
O1 Eu1 O5W 69.3(8) . . ?
O4 Eu1 O5W 71.8(7) . . ?
O3W Eu1 O5W 70.0(8) . . ?
O4W Eu1 O5W 123.3(8) . . ?
O1W Eu1 O5W 62.4(7) . . ?
O7 Eu1 O5W 137.9(7) . . ?
O2W Eu1 O5W 125.4(7) . . ?
O6W Eu1 O5W 127.5(7) . . ?
O1 Eu1 K1 79.4(4) . . ?
O4 Eu1 K1 110.1(4) . . ?
O3W Eu1 K1 159.9(4) . . ?
O4W Eu1 K1 110.4(4) . . ?
O1W Eu1 K1 35.7(4) . . ?
O7 Eu1 K1 118.3(3) . . ?
O2W Eu1 K1 63.4(3) . . ?
O6W Eu1 K1 37.2(3) . . ?
O5W Eu1 K1 97.7(6) . . ?
C9 O1 Eu1 144.3(17) . . ?
C10 O4 Eu1 140.9(15) . . ?
C9 O2 H2 109.5 . . ?
C19 C17 C16 119.2(19) . . ?
C19 C17 H17A 120.4 . . ?
C16 C17 H17A 120.4 . . ?
C7 C8 C6A 117(2) . . ?
C7 C8 C9 121(2) . . ?
C6A C8 C9 121(2) . . ?
C7 N1 C4 121(2) . . ?
C7 N1 K1 125.3(15) . 1_465 ?
C4 N1 K1 113.2(13) . 1_465 ?
C19 C18 N2 123(2) . . ?
C19 C18 H18A 118.3 . . ?
N2 C18 H18A 118.3 . . ?
C16 C15 C14 120.8(14) . . ?
C16 C15 N2 117.1(13) . . ?
C14 C15 N2 122.2(14) . . ?
O1 C9 O2 125(2) . . ?
O1 C9 C8 117(2) . . ?
O2 C9 C8 117(2) . . ?
O1 C9 K1 94.3(15) . 1_455 ?
O2 C9 K1 97.5(15) . 1_455 ?
C8 C9 K1 86.8(13) . 1_455 ?
C18 N2 C15 121.5(17) . . ?
C6A C6 C4 122(2) . . ?
C6A C6 C5 125(2) . . ?
C4 C6 C5 112.9(19) . . ?
C12 C13 C14 113.3(15) . . ?
C12 C13 K1 121.9(10) . 2_574 ?
C14 C13 K1 124.8(11) . 2_574 ?
C12 C13 H13A 123.3 . . ?
C14 C13 H13A 123.3 . . ?
K1 C13 H13A 2.7 2_574 . ?
C2 C3 C4 122.3(16) . . ?
C2 C3 H3A 118.8 . . ?
C4 C3 H3A 118.8 . . ?
N1 C7 C8 124(2) . . ?
N1 C7 H7A 117.8 . . ?
C8 C7 H7A 117.8 . . ?
C11 C16 C15 122.8(14) . . ?
C11 C16 C17 118.3(13) . . ?
C15 C16 C17 118.9(12) . . ?
C13 C14 C15 120.0(15) . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C1 C5 C6 123.6(18) . . ?
C1 C5 H5A 118.2 . . ?
C6 C5 H5A 118.2 . . ?
C3 C2 C1 122.6(15) . . ?
C3 C2 H2A 118.7 . . ?
C1 C2 H2A 118.7 . . ?
N1 C4 C3 122.1(17) . . ?
N1 C4 C6 116.7(17) . . ?
C3 C4 C6 120.9(18) . . ?
C5 C1 C2 117.7(16) . . ?
C5 C1 H1A 121.1 . . ?
C2 C1 H1A 121.1 . . ?
C17 C19 C18 119(2) . . ?
C17 C19 C10 121(2) . . ?
C18 C19 C10 119(2) . . ?
C16 C11 C12 111.5(14) . . ?
C16 C11 H11A 124.2 . . ?
C12 C11 H11A 124.2 . . ?
C6 C6A C8 118(2) . . ?
C6 C6A H6AA 121.1 . . ?
C8 C6A H6AA 121.1 . . ?
N1 K1 O1W 168.0(5) 1_645 . ?
N1 K1 O6W 113.7(5) 1_645 . ?
O1W K1 O6W 56.6(4) . . ?
N1 K1 O4W 80.0(5) 1_645 1_655 ?
O1W K1 O4W 95.6(5) . 1_655 ?
O6W K1 O4W 107.2(5) . 1_655 ?
N1 K1 C9 78.2(6) 1_645 1_655 ?
O1W K1 C9 109.4(6) . 1_655 ?
O6W K1 C9 161.5(6) . 1_655 ?
O4W K1 C9 59.5(6) 1_655 1_655 ?
N1 K1 C13 119.6(5) 1_645 2_575 ?
O1W K1 C13 70.4(4) . 2_575 ?
O6W K1 C13 94.4(4) . 2_575 ?
O4W K1 C13 142.1(5) 1_655 2_575 ?
C9 K1 C13 91.2(6) 1_655 2_575 ?
N1 K1 Eu1 140.9(4) 1_645 . ?
O1W K1 Eu1 27.8(3) . . ?
O6W K1 Eu1 30.5(3) . . ?
O4W K1 Eu1 95.7(3) 1_655 . ?
C9 K1 Eu1 132.7(5) 1_655 . ?
C13 K1 Eu1 87.3(3) 2_575 . ?
C11 C12 C13 131.0(17) . . ?
C11 C12 H12A 114.5 . . ?
C13 C12 H12A 114.5 . . ?
O3 C10 O4 129(2) . . ?
O3 C10 C19 116(2) . . ?
O4 C10 C19 114(2) . . ?
Eu1 O1W K1 116.5(6) . . ?
Eu1 O1W H1WA 108.2 . . ?
K1 O1W H1WA 108.2 . . ?
Eu1 O1W H1WB 108.2 . . ?
K1 O1W H1WB 108.2 . . ?
H1WA O1W H1WB 107.3 . . ?
Eu1 O2W H2WA 109.4 . . ?
Eu1 O2W H2WB 109.6 . . ?
H2WA O2W H2WB 109.5 . . ?
Eu1 O3W H3WA 109.3 . . ?
Eu1 O3W H3WB 108.9 . . ?
H3WA O3W H3WB 109.5 . . ?
Eu1 O4W K1 130.7(7) . 1_455 ?
Eu1 O4W H4WB 109.5 . . ?
K1 O4W H4WB 27.2 1_455 . ?
Eu1 O4W H4WC 108.8 . . ?
K1 O4W H4WC 109.7 1_455 . ?
H4WB O4W H4WC 109.5 . . ?
Eu1 O5W H5WA 109.6 . . ?
Eu1 O5W H5WB 109.5 . . ?
H5WA O5W H5WB 109.5 . . ?
Eu1 O6W K1 112.3(5) . . ?
Eu1 O6W H6WA 109.1 . . ?
K1 O6W H6WA 109.1 . . ?
Eu1 O6W H6WB 109.1 . . ?
K1 O6W H6WB 109.1 . . ?
H6WA O6W H6WB 107.9 . . ?
Eu1 O7 H7 109.3 . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        24.84
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.712
_refine_diff_density_min         -2.058
_refine_diff_density_rms         0.301
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1041891'
_audit_update_record             
;
2015-03-03 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;

#================================================================    

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H27 Cl Eu N5 O6'
_chemical_formula_weight         789.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1063(4)
_cell_length_b                   11.3995(5)
_cell_length_c                   14.9133(6)
_cell_angle_alpha                111.9660(10)
_cell_angle_beta                 91.3200(10)
_cell_angle_gamma                111.1270(10)
_cell_volume                     1605.93(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5948
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      25.76

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.151
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_exptl_absorpt_coefficient_mu    2.090
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14047
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         25.76
_reflns_number_total             5948
_reflns_number_gt                5301
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0350P)²+2.9435P] 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         5948
_refine_ls_number_parameters     410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0757
_refine_ls_wR_factor_gt          0.0657
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.017
_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
Eu1 Eu 1.081799(17) 0.845139(19) 0.439241(13) 0.01254(7) Uani 1 1 d . . .
N1 N 1.0277(3) 0.6408(3) 0.2688(2) 0.0213(7) Uani 1 1 d . . .
N2 N 1.2553(3) 0.8686(3) 0.3214(2) 0.0181(7) Uani 1 1 d . . .
N3 N 0.9089(4) 0.8526(4) 0.0488(3) 0.0337(9) Uani 1 1 d . . .
N4 N 0.4033(3) 0.6779(3) 0.3859(3) 0.0206(7) Uani 1 1 d . . .
N5 N 0.6364(7) 0.6405(8) 0.1239(5) 0.088(2) Uiso 1 1 d . . .
Cl1 Cl 1.23341(10) 0.66603(11) 0.62868(8) 0.0272(2) Uani 1 1 d . . .
O1 O 1.0067(3) 0.9235(3) 0.3359(2) 0.0274(7) Uani 1 1 d . . .
O2 O 0.9284(3) 1.0873(3) 0.39208(19) 0.0223(6) Uani 1 1 d . . .
O3 O 0.8513(2) 0.7389(3) 0.4200(2) 0.0219(6) Uani 1 1 d . . .
O4 O 1.2056(3) 1.0821(3) 0.5138(2) 0.0226(6) Uani 1 1 d . . .
O5 O 1.2787(2) 0.8321(3) 0.4998(2) 0.0209(6) Uani 1 1 d . . .
H5A H 1.2707 0.8214 0.5531 0.031 Uiso 1 1 d R . .
H5D H 1.3443 0.9064 0.5104 0.031 Uiso 1 1 d R . .
O6 O 1.0195(3) 0.6304(3) 0.4660(2) 0.0219(6) Uani 1 1 d . . .
H6A H 0.9640 0.6284 0.5042 0.033 Uiso 1 1 d R . .
H6D H 1.0875 0.6285 0.4918 0.033 Uiso 1 1 d R . .
C1 C 1.3655(4) 0.9796(4) 0.3449(3) 0.0219(9) Uani 1 1 d . . .
H1A H 1.3767 1.0587 0.4025 0.026 Uiso 1 1 calc R . .
C2 C 1.4670(4) 0.9874(5) 0.2896(3) 0.0290(10) Uani 1 1 d . . .
H2A H 1.5438 1.0699 0.3094 0.035 Uiso 1 1 calc R . .
C3 C 1.4527(4) 0.8741(5) 0.2071(3) 0.0311(10) Uani 1 1 d . . .
H3B H 1.5205 0.8756 0.1694 0.037 Uiso 1 1 calc R . .
C4 C 1.3362(4) 0.7551(5) 0.1789(3) 0.0260(9) Uani 1 1 d . . .
C5 C 1.3139(5) 0.6321(5) 0.0928(4) 0.0443(14) Uani 1 1 d . . .
H5B H 1.3794 0.6309 0.0531 0.053 Uiso 1 1 calc R . .
C6 C 1.2024(5) 0.5188(6) 0.0673(4) 0.0486(15) Uani 1 1 d . . .
H6B H 1.1908 0.4387 0.0103 0.058 Uiso 1 1 calc R . .
C7 C 1.1009(5) 0.5170(5) 0.1249(3) 0.0355(11) Uani 1 1 d . . .
C8 C 0.9810(5) 0.4022(5) 0.1004(4) 0.0483(15) Uani 1 1 d . . .
H8A H 0.9647 0.3197 0.0440 0.058 Uiso 1 1 calc R . .
C9 C 0.8893(5) 0.4107(5) 0.1580(4) 0.0492(15) Uani 1 1 d . . .
H9A H 0.8072 0.3347 0.1414 0.059 Uiso 1 1 calc R . .
C10 C 0.9156(4) 0.5311(5) 0.2415(3) 0.0320(11) Uani 1 1 d . . .
H10A H 0.8499 0.5348 0.2809 0.038 Uiso 1 1 calc R . .
C11 C 1.1196(4) 0.6361(4) 0.2101(3) 0.0212(9) Uani 1 1 d . . .
C12 C 1.2396(4) 0.7563(4) 0.2377(3) 0.0199(8) Uani 1 1 d . . .
C13 C 0.9417(4) 0.8810(5) 0.1415(3) 0.0270(10) Uani 1 1 d . . .
H13A H 0.9938 0.8384 0.1568 0.032 Uiso 1 1 calc R . .
C14 C 0.9061(4) 0.9699(4) 0.2209(3) 0.0168(8) Uani 1 1 d . . .
C15 C 0.8270(4) 1.0285(4) 0.1995(3) 0.0181(8) Uani 1 1 d . . .
H15A H 0.8004 1.0883 0.2508 0.022 Uiso 1 1 calc R . .
C16 C 0.7856(4) 0.9987(4) 0.1003(3) 0.0211(9) Uani 1 1 d . . .
C17 C 0.7013(4) 1.0519(5) 0.0726(3) 0.0312(10) Uani 1 1 d . . .
H17A H 0.6677 1.1070 0.1213 0.037 Uiso 1 1 calc R . .
C18 C 0.6675(5) 1.0243(6) -0.0248(4) 0.0417(13) Uani 1 1 d . . .
H18A H 0.6118 1.0614 -0.0431 0.050 Uiso 1 1 calc R . .
C19 C 0.7158(6) 0.9409(6) -0.0971(4) 0.0491(14) Uani 1 1 d . . .
H19A H 0.6931 0.9229 -0.1642 0.059 Uiso 1 1 calc R . .
C20 C 0.7946(5) 0.8857(6) -0.0725(3) 0.0412(12) Uani 1 1 d . . .
H20A H 0.8256 0.8291 -0.1225 0.049 Uiso 1 1 calc R . .
C21 C 0.8309(4) 0.9116(5) 0.0266(3) 0.0292(10) Uani 1 1 d . . .
C22 C 0.9499(3) 0.9956(4) 0.3244(3) 0.0163(8) Uani 1 1 d . . .
C23 C 0.5306(4) 0.7498(4) 0.4044(3) 0.0192(8) Uani 1 1 d . . .
H23A H 0.5609 0.8440 0.4149 0.023 Uiso 1 1 calc R . .
C24 C 0.6250(4) 0.6958(4) 0.4095(3) 0.0155(8) Uani 1 1 d . . .
C25 C 0.5828(4) 0.5599(4) 0.3936(3) 0.0163(8) Uani 1 1 d . . .
H25A H 0.6446 0.5207 0.3958 0.020 Uiso 1 1 calc R . .
C26 C 0.4471(4) 0.4786(4) 0.3740(3) 0.0169(8) Uani 1 1 d . . .
C27 C 0.3956(4) 0.3380(4) 0.3598(3) 0.0225(9) Uani 1 1 d . . .
H27A H 0.4535 0.2941 0.3611 0.027 Uiso 1 1 calc R . .
C28 C 0.2626(4) 0.2656(4) 0.3443(3) 0.0256(9) Uani 1 1 d . . .
H28A H 0.2288 0.1717 0.3352 0.031 Uiso 1 1 calc R . .
C29 C 0.1765(4) 0.3288(4) 0.3417(3) 0.0275(10) Uani 1 1 d . . .
H29A H 0.0846 0.2774 0.3312 0.033 Uiso 1 1 calc R . .
C30 C 0.2223(4) 0.4634(4) 0.3541(3) 0.0232(9) Uani 1 1 d . . .
H30A H 0.1623 0.5044 0.3513 0.028 Uiso 1 1 calc R . .
C31 C 0.3593(4) 0.5417(4) 0.3712(3) 0.0189(8) Uani 1 1 d . . .
C32 C 0.7674(4) 0.7913(4) 0.4402(3) 0.0165(8) Uani 1 1 d . . .
C33 C 0.4854(9) 0.4112(10) 0.1261(7) 0.108(3) Uiso 1 1 d . . .
H33A H 0.4353 0.3506 0.0594 0.163 Uiso 1 1 calc R . .
H33B H 0.4250 0.4276 0.1714 0.163 Uiso 1 1 calc R . .
H33C H 0.5357 0.3674 0.1464 0.163 Uiso 1 1 calc R . .
C34 C 0.5745(7) 0.5412(8) 0.1276(5) 0.0714(19) Uiso 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
Eu1 O1 2.319(3) . ?
Eu1 O4 2.330(3) . ?
Eu1 O2 2.358(3) 2_776 ?
Eu1 O3 2.361(3) . ?
Eu1 O5 2.421(3) . ?
Eu1 O6 2.480(3) . ?
Eu1 N1 2.596(3) . ?
Eu1 N2 2.647(3) . ?
Eu1 Eu1 4.3636(4) 2_776 ?
N1 C10 1.324(5) . ?
N1 C11 1.362(5) . ?
N2 C1 1.324(5) . ?
N2 C12 1.364(5) . ?
N3 C13 1.306(6) . ?
N3 C21 1.373(6) . ?
N4 C23 1.313(5) . ?
N4 C31 1.376(5) . ?
N5 C34 1.116(9) . ?
O1 C22 1.256(5) . ?
O2 C22 1.253(5) . ?
O2 Eu1 2.358(3) 2_776 ?
O3 C32 1.262(4) . ?
O4 C32 1.258(5) 2_776 ?
O5 H5A 0.8500 . ?
O5 H5D 0.8500 . ?
O6 H6A 0.8501 . ?
O6 H6D 0.8499 . ?
C1 C2 1.408(6) . ?
C1 H1A 0.9500 . ?
C2 C3 1.364(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.404(6) . ?
C3 H3B 0.9500 . ?
C4 C12 1.402(5) . ?
C4 C5 1.436(6) . ?
C5 C6 1.343(7) . ?
C5 H5B 0.9500 . ?
C6 C7 1.432(6) . ?
C6 H6B 0.9500 . ?
C7 C11 1.413(6) . ?
C7 C8 1.408(7) . ?
C8 C9 1.355(7) . ?
C8 H8A 0.9500 . ?
C9 C10 1.391(6) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C12 1.435(6) . ?
C13 C14 1.413(5) . ?
C13 H13A 0.9500 . ?
C14 C15 1.375(5) . ?
C14 C22 1.492(5) . ?
C15 C16 1.413(5) . ?
C15 H15A 0.9500 . ?
C16 C17 1.412(6) . ?
C16 C21 1.421(6) . ?
C17 C18 1.377(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.408(8) . ?
C18 H18A 0.9500 . ?
C19 C20 1.361(8) . ?
C19 H19A 0.9500 . ?
C20 C21 1.412(6) . ?
C20 H20A 0.9500 . ?
C23 C24 1.407(5) . ?
C23 H23A 0.9500 . ?
C24 C25 1.369(5) . ?
C24 C32 1.500(5) . ?
C25 C26 1.410(5) . ?
C25 H25A 0.9500 . ?
C26 C31 1.413(5) . ?
C26 C27 1.421(5) . ?
C27 C28 1.370(6) . ?
C27 H27A 0.9500 . ?
C28 C29 1.397(6) . ?
C28 H28A 0.9500 . ?
C29 C30 1.367(6) . ?
C29 H29A 0.9500 . ?
C30 C31 1.417(5) . ?
C30 H30A 0.9500 . ?
C32 O4 1.258(5) 2_776 ?
C33 C34 1.447(11) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 O4 77.39(10) . . ?
O1 Eu1 O2 125.54(10) . 2_776 ?
O4 Eu1 O2 74.03(10) . 2_776 ?
O1 Eu1 O3 76.72(10) . . ?
O4 Eu1 O3 124.91(9) . . ?
O2 Eu1 O3 83.14(10) 2_776 . ?
O1 Eu1 O5 141.42(10) . . ?
O4 Eu1 O5 83.71(10) . . ?
O2 Eu1 O5 79.38(9) 2_776 . ?
O3 Eu1 O5 140.33(10) . . ?
O1 Eu1 O6 138.38(10) . . ?
O4 Eu1 O6 142.97(10) . . ?
O2 Eu1 O6 74.97(9) 2_776 . ?
O3 Eu1 O6 70.08(9) . . ?
O5 Eu1 O6 71.08(9) . . ?
O1 Eu1 N1 77.86(11) . . ?
O4 Eu1 N1 139.10(10) . . ?
O2 Eu1 N1 146.36(10) 2_776 . ?
O3 Eu1 N1 79.46(10) . . ?
O5 Eu1 N1 96.15(10) . . ?
O6 Eu1 N1 72.11(10) . . ?
O1 Eu1 N2 75.12(10) . . ?
O4 Eu1 N2 79.92(10) . . ?
O2 Eu1 N2 140.52(10) 2_776 . ?
O3 Eu1 N2 136.34(10) . . ?
O5 Eu1 N2 68.60(10) . . ?
O6 Eu1 N2 113.47(9) . . ?
N1 Eu1 N2 62.49(10) . . ?
O1 Eu1 Eu1 60.89(7) . 2_776 ?
O4 Eu1 Eu1 55.47(7) . 2_776 ?
O2 Eu1 Eu1 64.69(7) 2_776 2_776 ?
O3 Eu1 Eu1 69.45(7) . 2_776 ?
O5 Eu1 Eu1 130.67(7) . 2_776 ?
O6 Eu1 Eu1 125.00(6) . 2_776 ?
N1 Eu1 Eu1 132.45(8) . 2_776 ?
N2 Eu1 Eu1 121.49(7) . 2_776 ?
C10 N1 C11 118.0(3) . . ?
C10 N1 Eu1 120.7(3) . . ?
C11 N1 Eu1 120.9(2) . . ?
C1 N2 C12 117.4(3) . . ?
C1 N2 Eu1 123.1(2) . . ?
C12 N2 Eu1 119.1(2) . . ?
C13 N3 C21 117.1(4) . . ?
C23 N4 C31 118.1(3) . . ?
C22 O1 Eu1 148.4(3) . . ?
C22 O2 Eu1 138.8(3) . 2_776 ?
C32 O3 Eu1 130.4(2) . . ?
C32 O4 Eu1 159.5(2) 2_776 . ?
Eu1 O5 H5A 109.3 . . ?
Eu1 O5 H5D 109.3 . . ?
H5A O5 H5D 109.5 . . ?
Eu1 O6 H6A 109.4 . . ?
Eu1 O6 H6D 109.4 . . ?
H6A O6 H6D 109.5 . . ?
N2 C1 C2 124.0(4) . . ?
N2 C1 H1A 118.0 . . ?
C2 C1 H1A 118.0 . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 H2A 120.7 . . ?
C1 C2 H2A 120.7 . . ?
C2 C3 C4 119.0(4) . . ?
C2 C3 H3B 120.5 . . ?
C4 C3 H3B 120.5 . . ?
C12 C4 C3 118.7(4) . . ?
C12 C4 C5 119.1(4) . . ?
C3 C4 C5 122.2(4) . . ?
C6 C5 C4 121.5(4) . . ?
C6 C5 H5B 119.3 . . ?
C4 C5 H5B 119.3 . . ?
C5 C6 C7 120.9(4) . . ?
C5 C6 H6B 119.6 . . ?
C7 C6 H6B 119.6 . . ?
C11 C7 C8 117.6(4) . . ?
C11 C7 C6 119.2(4) . . ?
C8 C7 C6 123.3(4) . . ?
C9 C8 C7 119.3(4) . . ?
C9 C8 H8A 120.4 . . ?
C7 C8 H8A 120.4 . . ?
C8 C9 C10 119.8(5) . . ?
C8 C9 H9A 120.1 . . ?
C10 C9 H9A 120.1 . . ?
N1 C10 C9 123.2(4) . . ?
N1 C10 H10A 118.4 . . ?
C9 C10 H10A 118.4 . . ?
N1 C11 C7 122.1(4) . . ?
N1 C11 C12 118.2(3) . . ?
C7 C11 C12 119.7(4) . . ?
N2 C12 C4 122.3(4) . . ?
N2 C12 C11 118.1(3) . . ?
C4 C12 C11 119.7(4) . . ?
N3 C13 C14 125.5(4) . . ?
N3 C13 H13A 117.2 . . ?
C14 C13 H13A 117.2 . . ?
C15 C14 C13 117.8(4) . . ?
C15 C14 C22 121.2(3) . . ?
C13 C14 C22 120.9(4) . . ?
C14 C15 C16 119.2(3) . . ?
C14 C15 H15A 120.4 . . ?
C16 C15 H15A 120.4 . . ?
C17 C16 C15 122.4(4) . . ?
C17 C16 C21 119.5(4) . . ?
C15 C16 C21 118.1(4) . . ?
C18 C17 C16 120.4(5) . . ?
C18 C17 H17A 119.8 . . ?
C16 C17 H17A 119.8 . . ?
C17 C18 C19 119.8(5) . . ?
C17 C18 H18A 120.1 . . ?
C19 C18 H18A 120.1 . . ?
C20 C19 C18 121.0(4) . . ?
C20 C19 H19A 119.5 . . ?
C18 C19 H19A 119.5 . . ?
C19 C20 C21 120.8(5) . . ?
C19 C20 H20A 119.6 . . ?
C21 C20 H20A 119.6 . . ?
N3 C21 C20 119.3(4) . . ?
N3 C21 C16 122.2(4) . . ?
C20 C21 C16 118.6(4) . . ?
O2 C22 O1 125.6(4) . . ?
O2 C22 C14 117.8(3) . . ?
O1 C22 C14 116.6(3) . . ?
N4 C23 C24 124.0(4) . . ?
N4 C23 H23A 118.0 . . ?
C24 C23 H23A 118.0 . . ?
C25 C24 C23 118.6(3) . . ?
C25 C24 C32 122.2(3) . . ?
C23 C24 C32 119.0(3) . . ?
C24 C25 C26 119.5(3) . . ?
C24 C25 H25A 120.2 . . ?
C26 C25 H25A 120.2 . . ?
C31 C26 C25 118.0(3) . . ?
C31 C26 C27 119.0(3) . . ?
C25 C26 C27 122.9(4) . . ?
C28 C27 C26 120.2(4) . . ?
C28 C27 H27A 119.9 . . ?
C26 C27 H27A 119.9 . . ?
C27 C28 C29 120.4(4) . . ?
C27 C28 H28A 119.8 . . ?
C29 C28 H28A 119.8 . . ?
C30 C29 C28 121.1(4) . . ?
C30 C29 H29A 119.5 . . ?
C28 C29 H29A 119.5 . . ?
C29 C30 C31 120.0(4) . . ?
C29 C30 H30A 120.0 . . ?
C31 C30 H30A 120.0 . . ?
N4 C31 C26 121.7(3) . . ?
N4 C31 C30 119.0(4) . . ?
C26 C31 C30 119.3(4) . . ?
O3 C32 O4 124.8(3) . 2_776 ?
O3 C32 C24 117.9(3) . . ?
O4 C32 C24 117.3(3) 2_776 . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C34 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N5 C34 C33 174.9(9) . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.116
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1041892'
_audit_update_record             
;
2015-03-03 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;

#================================================================    

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H22 Eu N5 O8'
_chemical_formula_weight         756.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

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                   14.8782(13)
_cell_length_b                   13.0813(9)
_cell_length_c                   17.2576(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.253(2)
_cell_angle_gamma                90.00
_cell_volume                     3151.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5684
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      25.40

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.151
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_exptl_absorpt_coefficient_mu    2.049
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17077
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_sigmaI/netI    0.0729
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.11
_diffrn_reflns_theta_max         25.40
_reflns_number_total             5684
_reflns_number_gt                3532
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0872P)²+7.3053P] 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         5684
_refine_ls_number_parameters     415
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1690
_refine_ls_wR_factor_gt          0.1378
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_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
Eu1 Eu 0.51565(3) 0.87409(3) 0.06618(3) 0.03728(18) Uani 1 1 d . . .
N1 N 0.0752(11) 0.8271(10) -0.1887(8) 0.103(4) Uani 1 1 d . . .
N2 N 0.5878(8) 0.8863(10) 0.4571(6) 0.093(4) Uani 1 1 d . . .
N3 N 0.4565(6) 0.6851(6) 0.0637(4) 0.044(2) Uani 1 1 d . . .
N4 N 0.6429(6) 0.7372(6) 0.1366(4) 0.048(2) Uani 1 1 d . . .
N5 N 0.5512(7) 0.8690(7) -0.0890(5) 0.059(2) Uani 1 1 d . . .
O1 O 0.3564(4) 0.8830(5) -0.0296(4) 0.0442(15) Uani 1 1 d . . .
O2 O 0.3371(5) 1.0388(5) -0.0868(4) 0.0522(17) Uani 1 1 d . . .
O3 O 0.5782(5) 0.9006(5) 0.2162(4) 0.0479(17) Uani 1 1 d . . .
O4 O 0.4261(5) 0.8605(5) 0.1643(4) 0.0496(17) Uani 1 1 d . . .
O5 O 0.4782(5) 1.0484(4) 0.0702(4) 0.0427(15) Uani 1 1 d . . .
O6 O 0.5585(5) 0.7889(5) -0.0453(4) 0.0497(17) Uani 1 1 d . . .
O7 O 0.5806(11) 0.8623(9) -0.1657(7) 0.140(5) Uani 1 1 d . . .
C1 C 0.1712(11) 0.8485(13) -0.1431(9) 0.092(4) Uani 1 1 d . . .
H1 H 0.2159 0.7938 -0.1326 0.110 Uiso 1 1 calc R . .
C2 C 0.2025(8) 0.9364(9) -0.1148(6) 0.054(3) Uani 1 1 d . . .
C3 C 0.1417(10) 1.0238(14) -0.1296(9) 0.100(5) Uani 1 1 d . . .
H3 H 0.1666 1.0895 -0.1101 0.120 Uiso 1 1 calc R . .
C4 C 0.0421(12) 1.0093(15) -0.1749(10) 0.104(5) Uani 1 1 d . . .
C5 C -0.0262(14) 1.0897(16) -0.1998(13) 0.136(7) Uani 1 1 d . . .
H5 H -0.0064 1.1590 -0.1901 0.163 Uiso 1 1 calc R . .
C6 C -0.1179(16) 1.067(2) -0.2369(13) 0.207(13) Uani 1 1 d DU . .
H6 H -0.1642 1.1198 -0.2476 0.248 Uiso 1 1 calc R . .
C7 C -0.1525(15) 0.955(2) -0.2633(11) 0.181(12) Uani 1 1 d DU . .
H7 H -0.2179 0.9381 -0.2908 0.217 Uiso 1 1 calc R . .
C8 C -0.0858(10) 0.8901(13) -0.2450(8) 0.088(4) Uani 1 1 d . . .
H8 H -0.1039 0.8218 -0.2621 0.106 Uiso 1 1 calc R . .
C9 C 0.0089(13) 0.9064(12) -0.2036(10) 0.097(5) Uani 1 1 d . . .
C10 C 0.3069(7) 0.9532(8) -0.0737(6) 0.044(2) Uani 1 1 d . . .
C11 C 0.5822(9) 0.8875(11) 0.3804(7) 0.084(4) Uani 1 1 d . . .
H11 H 0.6404 0.8952 0.3698 0.100 Uiso 1 1 calc R . .
C12 C 0.4957(7) 0.8783(8) 0.3099(6) 0.048(2) Uani 1 1 d . . .
C13 C 0.4134(9) 0.8657(8) 0.3271(7) 0.060(3) Uani 1 1 d . . .
H13 H 0.3539 0.8596 0.2830 0.072 Uiso 1 1 calc R . .
C14 C 0.4150(9) 0.8616(9) 0.4098(7) 0.063(3) Uani 1 1 d . . .
C15 C 0.3337(10) 0.8446(11) 0.4302(8) 0.086(4) Uani 1 1 d . . .
H15 H 0.2731 0.8389 0.3875 0.103 Uiso 1 1 calc R . .
C16 C 0.3397(12) 0.8362(13) 0.5082(9) 0.099(5) Uani 1 1 d . . .
H16 H 0.2840 0.8216 0.5212 0.119 Uiso 1 1 calc R . .
C17 C 0.4292(14) 0.8490(12) 0.5721(10) 0.105(5) Uani 1 1 d . . .
H17 H 0.4326 0.8455 0.6281 0.126 Uiso 1 1 calc R . .
C18 C 0.5110(11) 0.8664(12) 0.5548(8) 0.098(5) Uani 1 1 d . . .
H18 H 0.5709 0.8744 0.5981 0.117 Uiso 1 1 calc R . .
C19 C 0.5049(10) 0.8722(12) 0.4733(7) 0.084(4) Uani 1 1 d . . .
C20 C 0.4997(7) 0.8795(7) 0.2256(5) 0.039(2) Uani 1 1 d . . .
C21 C 0.3646(8) 0.6596(8) 0.0336(6) 0.053(3) Uani 1 1 d . . .
H21 H 0.3184 0.7121 0.0128 0.064 Uiso 1 1 calc R . .
C22 C 0.3326(8) 0.5575(8) 0.0312(6) 0.058(3) Uani 1 1 d . . .
H22 H 0.2662 0.5420 0.0087 0.070 Uiso 1 1 calc R . .
C23 C 0.3982(9) 0.4816(8) 0.0613(6) 0.059(3) Uani 1 1 d . . .
H23 H 0.3777 0.4126 0.0590 0.071 Uiso 1 1 calc R . .
C24 C 0.4955(9) 0.5054(8) 0.0957(6) 0.055(3) Uani 1 1 d . . .
C25 C 0.5686(10) 0.4295(8) 0.1295(7) 0.061(3) Uani 1 1 d . . .
H25 H 0.5516 0.3592 0.1263 0.073 Uiso 1 1 calc R . .
C26 C 0.6607(9) 0.4569(8) 0.1656(7) 0.059(3) Uani 1 1 d . . .
H26 H 0.7080 0.4058 0.1879 0.071 Uiso 1 1 calc R . .
C27 C 0.6885(8) 0.5617(8) 0.1709(6) 0.053(3) Uani 1 1 d . . .
C28 C 0.7825(8) 0.5934(7) 0.2137(6) 0.055(3) Uani 1 1 d . . .
H28 H 0.8307 0.5445 0.2399 0.066 Uiso 1 1 calc R . .
C29 C 0.8044(8) 0.6940(8) 0.2174(6) 0.061(3) Uani 1 1 d . . .
H29 H 0.8676 0.7169 0.2469 0.073 Uiso 1 1 calc R . .
C30 C 0.7323(7) 0.7636(7) 0.1770(6) 0.054(3) Uani 1 1 d . . .
H30 H 0.7486 0.8339 0.1787 0.065 Uiso 1 1 calc R . .
C31 C 0.5214(7) 0.6103(7) 0.0971(6) 0.042(2) Uani 1 1 d . . .
C32 C 0.6194(7) 0.6369(6) 0.1343(5) 0.040(2) Uani 1 1 d . . .
OW1 O -0.204(2) 1.205(5) -0.121(4) 0.91(7) Uani 1 1 d . . .
HW1B H -0.2039 1.2642 -0.1416 1.371 Uiso 1 1 d R . .
HW1C H -0.2432 1.1668 -0.1571 1.371 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
Eu1 O5 2.354(6) . ?
Eu1 O1 2.376(6) . ?
Eu1 O2 2.384(7) 3_675 ?
Eu1 O3 2.454(6) . ?
Eu1 O6 2.491(6) . ?
Eu1 O4 2.497(6) . ?
Eu1 N4 2.584(7) . ?
Eu1 O5 2.593(6) 3_675 ?
Eu1 N3 2.620(7) . ?
Eu1 Eu1 3.9433(9) 3_675 ?
N1 C9 1.392(19) . ?
N1 C1 1.399(18) . ?
N2 C11 1.298(15) . ?
N2 C19 1.369(17) . ?
N3 C21 1.326(12) . ?
N3 C31 1.355(12) . ?
N4 C30 1.316(12) . ?
N4 C32 1.355(11) . ?
N5 O5 1.251(10) 3_675 ?
N5 O6 1.273(10) . ?
N5 O7 1.534(13) . ?
O1 C10 1.256(11) . ?
O2 C10 1.256(11) . ?
O2 Eu1 2.384(7) 3_675 ?
O3 C20 1.264(11) . ?
O4 C20 1.257(10) . ?
O5 N5 1.251(10) 3_675 ?
O5 Eu1 2.593(6) 3_675 ?
C1 C2 1.273(18) . ?
C1 H1 0.9500 . ?
C2 C3 1.425(18) . ?
C2 C10 1.483(14) . ?
C3 C4 1.429(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.42(2) . ?
C4 C9 1.46(2) . ?
C5 C6 1.33(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.560(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.26(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.36(2) . ?
C8 H8 0.9500 . ?
C11 C12 1.438(15) . ?
C11 H11 0.9500 . ?
C12 C13 1.367(15) . ?
C12 C20 1.476(12) . ?
C13 C14 1.419(14) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(17) . ?
C14 C19 1.412(18) . ?
C15 C16 1.323(18) . ?
C15 H15 0.9500 . ?
C16 C17 1.42(2) . ?
C16 H16 0.9500 . ?
C17 C18 1.37(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.381(16) . ?
C18 H18 0.9500 . ?
C21 C22 1.413(14) . ?
C21 H21 0.9500 . ?
C22 C23 1.363(15) . ?
C22 H22 0.9500 . ?
C23 C24 1.396(15) . ?
C23 H23 0.9500 . ?
C24 C31 1.423(13) . ?
C24 C25 1.439(15) . ?
C25 C26 1.343(15) . ?
C25 H25 0.9500 . ?
C26 C27 1.425(14) . ?
C26 H26 0.9500 . ?
C27 C28 1.400(15) . ?
C27 C32 1.404(13) . ?
C28 C29 1.352(15) . ?
C28 H28 0.9500 . ?
C29 C30 1.395(13) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.418(13) . ?
OW1 HW1B 0.8498 . ?
OW1 HW1C 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
O5 Eu1 O1 77.5(2) . . ?
O5 Eu1 O2 75.4(2) . 3_675 ?
O1 Eu1 O2 136.4(2) . 3_675 ?
O5 Eu1 O3 80.8(2) . . ?
O1 Eu1 O3 130.5(2) . . ?
O2 Eu1 O3 77.4(2) 3_675 . ?
O5 Eu1 O6 125.6(2) . . ?
O1 Eu1 O6 86.8(2) . . ?
O2 Eu1 O6 82.0(2) 3_675 . ?
O3 Eu1 O6 140.7(2) . . ?
O5 Eu1 O4 82.1(2) . . ?
O1 Eu1 O4 80.6(2) . . ?
O2 Eu1 O4 127.7(2) 3_675 . ?
O3 Eu1 O4 52.5(2) . . ?
O6 Eu1 O4 146.3(2) . . ?
O5 Eu1 N4 143.1(2) . . ?
O1 Eu1 N4 138.8(2) . . ?
O2 Eu1 N4 77.0(2) 3_675 . ?
O3 Eu1 N4 69.7(2) . . ?
O6 Eu1 N4 73.2(2) . . ?
O4 Eu1 N4 96.2(2) . . ?
O5 Eu1 O5 74.4(2) . 3_675 ?
O1 Eu1 O5 71.9(2) . 3_675 ?
O2 Eu1 O5 68.2(2) 3_675 3_675 ?
O3 Eu1 O5 141.5(2) . 3_675 ?
O6 Eu1 O5 51.30(19) . 3_675 ?
O4 Eu1 O5 146.9(2) . 3_675 ?
N4 Eu1 O5 116.6(2) . 3_675 ?
O5 Eu1 N3 146.4(2) . . ?
O1 Eu1 N3 77.7(2) . . ?
O2 Eu1 N3 137.7(2) 3_675 . ?
O3 Eu1 N3 98.8(2) . . ?
O6 Eu1 N3 74.9(2) . . ?
O4 Eu1 N3 71.9(2) . . ?
N4 Eu1 N3 62.7(3) . . ?
O5 Eu1 N3 118.1(2) 3_675 . ?
O5 Eu1 Eu1 39.29(15) . 3_675 ?
O1 Eu1 Eu1 70.53(14) . 3_675 ?
O2 Eu1 Eu1 66.75(15) 3_675 3_675 ?
O3 Eu1 Eu1 114.76(15) . 3_675 ?
O6 Eu1 Eu1 86.37(15) . 3_675 ?
O4 Eu1 Eu1 117.94(16) . 3_675 ?
N4 Eu1 Eu1 140.52(19) . 3_675 ?
O5 Eu1 Eu1 35.09(13) 3_675 3_675 ?
N3 Eu1 Eu1 143.84(16) . 3_675 ?
C9 N1 C1 118.3(14) . . ?
C11 N2 C19 117.8(11) . . ?
C21 N3 C31 118.1(8) . . ?
C21 N3 Eu1 122.6(6) . . ?
C31 N3 Eu1 119.2(6) . . ?
C30 N4 C32 118.3(8) . . ?
C30 N4 Eu1 120.6(6) . . ?
C32 N4 Eu1 121.2(6) . . ?
O5 N5 O6 121.6(8) 3_675 . ?
O5 N5 O7 120.2(9) 3_675 . ?
O6 N5 O7 118.2(9) . . ?
C10 O1 Eu1 133.8(6) . . ?
C10 O2 Eu1 140.0(6) . 3_675 ?
C20 O3 Eu1 94.3(5) . . ?
C20 O4 Eu1 92.5(5) . . ?
N5 O5 Eu1 162.3(6) 3_675 . ?
N5 O5 Eu1 91.3(5) 3_675 3_675 ?
Eu1 O5 Eu1 105.6(2) . 3_675 ?
N5 O6 Eu1 95.5(5) . . ?
C2 C1 N1 124.3(15) . . ?
C2 C1 H1 117.8 . . ?
N1 C1 H1 117.8 . . ?
C1 C2 C3 122.0(12) . . ?
C1 C2 C10 120.1(12) . . ?
C3 C2 C10 117.5(11) . . ?
C2 C3 C4 117.7(15) . . ?
C2 C3 H3 121.1 . . ?
C4 C3 H3 121.1 . . ?
C5 C4 C3 124.4(18) . . ?
C5 C4 C9 117.2(16) . . ?
C3 C4 C9 118.2(17) . . ?
C6 C5 C4 119(2) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C7 122(2) . . ?
C5 C6 H6 118.9 . . ?
C7 C6 H6 118.9 . . ?
C8 C7 C6 114(2) . . ?
C8 C7 H7 123.0 . . ?
C6 C7 H7 123.0 . . ?
C7 C8 C9 127.5(19) . . ?
C7 C8 H8 116.3 . . ?
C9 C8 H8 116.3 . . ?
C8 C9 N1 121.3(16) . . ?
C8 C9 C4 119.4(16) . . ?
N1 C9 C4 119.3(16) . . ?
O1 C10 O2 126.1(8) . . ?
O1 C10 C2 118.6(9) . . ?
O2 C10 C2 115.2(9) . . ?
N2 C11 C12 125.8(12) . . ?
N2 C11 H11 117.1 . . ?
C12 C11 H11 117.1 . . ?
C13 C12 C11 115.7(9) . . ?
C13 C12 C20 124.1(9) . . ?
C11 C12 C20 120.2(9) . . ?
C12 C13 C14 121.2(11) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C19 119.5(11) . . ?
C15 C14 C13 123.2(12) . . ?
C19 C14 C13 117.3(11) . . ?
C16 C15 C14 120.9(14) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 119.8(15) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C18 C17 C16 121.1(14) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 118.8(14) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
N2 C19 C18 118.0(13) . . ?
N2 C19 C14 122.3(11) . . ?
C18 C19 C14 119.8(13) . . ?
O4 C20 O3 120.6(8) . . ?
O4 C20 C12 120.5(8) . . ?
O3 C20 C12 118.9(8) . . ?
N3 C21 C22 122.6(10) . . ?
N3 C21 H21 118.7 . . ?
C22 C21 H21 118.7 . . ?
C23 C22 C21 119.2(10) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 120.0(10) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C31 117.2(10) . . ?
C23 C24 C25 123.1(10) . . ?
C31 C24 C25 119.7(10) . . ?
C26 C25 C24 120.7(10) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C27 120.9(10) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
C28 C27 C32 118.2(9) . . ?
C28 C27 C26 122.2(10) . . ?
C32 C27 C26 119.6(11) . . ?
C29 C28 C27 119.6(10) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 118.7(10) . . ?
C28 C29 H29 120.7 . . ?
C30 C29 H29 120.7 . . ?
N4 C30 C29 123.7(9) . . ?
N4 C30 H30 118.2 . . ?
C29 C30 H30 118.2 . . ?
N3 C31 C32 119.0(8) . . ?
N3 C31 C24 122.7(9) . . ?
C32 C31 C24 118.3(9) . . ?
N4 C32 C27 121.6(9) . . ?
N4 C32 C31 117.8(8) . . ?
C27 C32 C31 120.6(9) . . ?
HW1B OW1 HW1C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.40
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         1.573
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.159
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1041893'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;

#================================================================   

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H28 Eu N3 O11'
_chemical_formula_weight         758.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.842(5)
_cell_length_b                   11.416(7)
_cell_length_c                   16.613(10)
_cell_angle_alpha                81.716(7)
_cell_angle_beta                 87.825(7)
_cell_angle_gamma                79.381(7)
_cell_volume                     1446.5(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5019
_cell_measurement_theta_min      1.83
_cell_measurement_theta_max      25.02

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    2.237
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7023
_exptl_absorpt_correction_T_max  0.7751
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10171
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.02
_reflns_number_total             5019
_reflns_number_gt                4569
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0420P)²+25.1437P] 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         5019
_refine_ls_number_parameters     406
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1667
_refine_ls_wR_factor_gt          0.1645
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_restrained_S_all      1.193
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.003

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
Eu1 Eu 0.02229(7) 0.14581(4) 0.10893(3) 0.02244(18) Uani 1 1 d . . .
O1 O 0.0575(10) -0.1701(7) 0.0253(4) 0.0336(17) Uani 1 1 d . . .
O2 O 0.0010(10) -0.0602(6) 0.1271(4) 0.0352(18) Uani 1 1 d . . .
O4 O -0.0013(11) 0.1967(7) 0.2471(5) 0.0417(19) Uani 1 1 d . . .
O5 O 0.5290(10) 0.3092(7) 0.0140(5) 0.0380(18) Uani 1 1 d . . .
O6 O 0.4965(11) 0.1722(7) -0.0648(5) 0.0383(19) Uani 1 1 d . . .
O7 O 0.2812(10) 0.0587(7) 0.0384(5) 0.0375(18) Uani 1 1 d . . .
H7A H 0.2605 0.0657 -0.0121 0.056 Uiso 1 1 d R . .
H7C H 0.3631 0.0957 0.0453 0.056 Uiso 1 1 d R . .
O8 O 0.2270(10) 0.2831(7) 0.1037(5) 0.0386(19) Uani 1 1 d . . .
H8A H 0.2356 0.3172 0.0551 0.058 Uiso 1 1 d R . .
H8C H 0.3256 0.2437 0.1195 0.058 Uiso 1 1 d R . .
O9 O -0.2810(10) 0.1339(7) 0.1300(5) 0.044(2) Uani 1 1 d . . .
H9A H -0.3299 0.1426 0.0842 0.065 Uiso 1 1 d R . .
H9D H -0.3293 0.1894 0.1568 0.065 Uiso 1 1 d R . .
O10 O -0.1477(10) 0.3489(6) 0.0818(5) 0.0389(19) Uani 1 1 d . . .
H10B H -0.2360 0.3546 0.1133 0.058 Uiso 1 1 d R . .
H10C H -0.0858 0.3995 0.0904 0.058 Uiso 1 1 d R . .
OW1 O -0.4452(11) -0.0434(7) 0.1937(5) 0.044(2) Uani 1 1 d . . .
HW1A H -0.5046 -0.0467 0.1526 0.066 Uiso 1 1 d R . .
HW1C H -0.5084 -0.0035 0.2267 0.066 Uiso 1 1 d R . .
C1 C -0.0719(13) -0.2536(8) 0.1415(7) 0.028(2) Uani 1 1 d U . .
C2 C -0.1343(14) -0.2432(9) 0.2230(6) 0.030(2) Uani 1 1 d U . .
H2A H -0.1294 -0.1733 0.2447 0.036 Uiso 1 1 calc R . .
C3 C -0.2018(14) -0.3351(10) 0.2705(7) 0.031(2) Uani 1 1 d . . .
C4 C -0.2624(18) -0.3321(11) 0.3507(8) 0.047(3) Uani 1 1 d . . .
H4A H -0.2618 -0.2636 0.3748 0.056 Uiso 1 1 calc R . .
C5 C -0.3232(17) -0.4287(12) 0.3948(8) 0.049(3) Uani 1 1 d . . .
H5A H -0.3630 -0.4251 0.4480 0.058 Uiso 1 1 calc R . .
C6 C -0.3239(18) -0.5305(11) 0.3589(9) 0.052(3) Uani 1 1 d . . .
H6A H -0.3646 -0.5954 0.3887 0.063 Uiso 1 1 calc R . .
C7 C -0.2657(16) -0.5387(10) 0.2795(8) 0.045(3) Uani 1 1 d . . .
H7B H -0.2683 -0.6081 0.2567 0.054 Uiso 1 1 calc R . .
C8 C -0.2029(15) -0.4419(10) 0.2338(7) 0.035(3) Uani 1 1 d . . .
C9 C -0.0874(14) -0.3593(9) 0.1144(7) 0.032(2) Uani 1 1 d . . .
H9B H -0.0523 -0.3670 0.0610 0.038 Uiso 1 1 calc R . .
C10 C -0.0020(12) -0.1494(9) 0.0977(6) 0.023(2) Uani 1 1 d . . .
C11 C 0.6387(13) 0.4602(9) -0.1209(6) 0.028(2) Uani 1 1 d . . .
H11A H 0.6104 0.4897 -0.0718 0.034 Uiso 1 1 calc R . .
C12 C 0.6095(13) 0.3436(9) -0.1259(6) 0.027(2) Uani 1 1 d . . .
C13 C 0.6479(14) 0.3012(10) -0.1984(6) 0.031(2) Uani 1 1 d . . .
H13A H 0.6305 0.2246 -0.2045 0.038 Uiso 1 1 calc R . .
C14 C 0.7139(14) 0.3733(10) -0.2640(7) 0.033(2) Uani 1 1 d . . .
C15 C 0.7587(17) 0.3342(11) -0.3409(7) 0.043(3) Uani 1 1 d . . .
H15A H 0.7413 0.2588 -0.3498 0.051 Uiso 1 1 calc R . .
C16 C 0.8269(18) 0.4065(12) -0.4016(7) 0.048(3) Uani 1 1 d . . .
H16A H 0.8602 0.3793 -0.4510 0.057 Uiso 1 1 calc R . .
C17 C 0.8463(18) 0.5233(12) -0.3886(8) 0.049(3) Uani 1 1 d . . .
H17A H 0.8871 0.5740 -0.4308 0.059 Uiso 1 1 calc R . .
C18 C 0.8070(15) 0.5620(11) -0.3165(7) 0.039(3) Uani 1 1 d . . .
H18A H 0.8242 0.6380 -0.3087 0.047 Uiso 1 1 calc R . .
C19 C 0.7399(14) 0.4883(10) -0.2526(7) 0.033(2) Uani 1 1 d . . .
C20 C 0.5384(13) 0.2703(10) -0.0546(7) 0.031(2) Uani 1 1 d . . .
C21 C 0.1588(14) 0.0841(10) 0.3620(6) 0.032(2) Uani 1 1 d . . .
C22 C 0.2767(15) -0.0156(10) 0.3905(7) 0.035(3) Uani 1 1 d . . .
H22A H 0.3379 -0.0643 0.3548 0.042 Uiso 1 1 calc R . .
C23 C 0.3041(17) -0.0434(11) 0.4765(7) 0.041(3) Uani 1 1 d . . .
C24 C 0.4179(18) -0.1481(12) 0.5111(8) 0.049(3) Uani 1 1 d . . .
H24A H 0.4805 -0.2003 0.4779 0.059 Uiso 1 1 calc R . .
C25 C 0.435(2) -0.1714(14) 0.5927(9) 0.061(4) Uani 1 1 d . . .
H25A H 0.5098 -0.2399 0.6154 0.073 Uiso 1 1 calc R . .
C26 C 0.343(2) -0.0960(15) 0.6426(9) 0.065(5) Uani 1 1 d . . .
H26A H 0.3573 -0.1144 0.6986 0.078 Uiso 1 1 calc R . .
C27 C 0.231(2) 0.0067(14) 0.6115(7) 0.055(4) Uani 1 1 d . . .
H27A H 0.1690 0.0567 0.6463 0.065 Uiso 1 1 calc R . .
C28 C 0.2094(17) 0.0353(11) 0.5273(7) 0.042(3) Uani 1 1 d . . .
C29 C 0.0716(16) 0.1587(11) 0.4173(7) 0.038(3) Uani 1 1 d . . .
H29A H -0.0065 0.2270 0.3965 0.045 Uiso 1 1 calc R . .
C30 C 0.1205(14) 0.1125(10) 0.2741(6) 0.032(2) Uani 1 1 d . . .
N1 N -0.1463(12) -0.4503(8) 0.1558(6) 0.034(2) Uani 1 1 d . . .
N2 N 0.7010(12) 0.5303(7) -0.1780(6) 0.032(2) Uani 1 1 d . . .
N3 N 0.0945(14) 0.1372(10) 0.4970(6) 0.046(3) Uani 1 1 d . . .
O3 O 0.2064(11) 0.0480(7) 0.2245(5) 0.0403(19) 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
Eu1 O1 2.303(7) 2 ?
Eu1 O2 2.363(7) . ?
Eu1 O9 2.417(8) . ?
Eu1 O7 2.428(7) . ?
Eu1 O4 2.440(8) . ?
Eu1 O8 2.433(7) . ?
Eu1 O10 2.441(7) . ?
Eu1 O3 2.453(8) . ?
Eu1 C30 2.832(11) . ?
O1 C10 1.312(12) . ?
O1 Eu1 2.303(7) 2 ?
O2 C10 1.196(12) . ?
O4 C30 1.268(14) . ?
O5 C20 1.275(13) . ?
O6 C20 1.259(13) . ?
O7 H7A 0.8501 . ?
O7 H7C 0.8499 . ?
O8 H8A 0.8500 . ?
O8 H8C 0.8500 . ?
O9 H9A 0.8501 . ?
O9 H9D 0.8499 . ?
O10 H10B 0.8500 . ?
O10 H10C 0.8499 . ?
OW1 HW1A 0.8501 . ?
OW1 HW1C 0.8499 . ?
C1 C9 1.375(14) . ?
C1 C2 1.436(15) . ?
C1 C10 1.484(13) . ?
C2 C3 1.392(15) . ?
C2 H2A 0.9300 . ?
C3 C4 1.400(16) . ?
C3 C8 1.441(15) . ?
C4 C5 1.383(17) . ?
C4 H4A 0.9300 . ?
C5 C6 1.382(19) . ?
C5 H5A 0.9300 . ?
C6 C7 1.389(18) . ?
C6 H6A 0.9300 . ?
C7 C8 1.404(15) . ?
C7 H7B 0.9300 . ?
C8 N1 1.364(15) . ?
C9 N1 1.308(14) . ?
C9 H9B 0.9300 . ?
C11 N2 1.293(13) . ?
C11 C12 1.406(14) . ?
C11 H11A 0.9300 . ?
C12 C13 1.364(15) . ?
C12 C20 1.501(14) . ?
C13 C14 1.410(15) . ?
C13 H13A 0.9300 . ?
C14 C19 1.405(15) . ?
C14 C15 1.424(15) . ?
C15 C16 1.367(17) . ?
C15 H15A 0.9300 . ?
C16 C17 1.417(18) . ?
C16 H16A 0.9300 . ?
C17 C18 1.341(17) . ?
C17 H17A 0.9300 . ?
C18 C19 1.405(15) . ?
C18 H18A 0.9300 . ?
C19 N2 1.395(14) . ?
C21 C22 1.366(16) . ?
C21 C29 1.414(15) . ?
C21 C30 1.480(15) . ?
C22 C23 1.434(16) . ?
C22 H22A 0.9300 . ?
C23 C28 1.414(18) . ?
C23 C24 1.415(18) . ?
C24 C25 1.350(19) . ?
C24 H24A 0.9300 . ?
C25 C26 1.37(2) . ?
C25 H25A 0.9300 . ?
C26 C27 1.38(2) . ?
C26 H26A 0.9300 . ?
C27 C28 1.399(17) . ?
C27 H27A 0.9300 . ?
C28 N3 1.378(17) . ?
C29 N3 1.323(15) . ?
C29 H29A 0.9300 . ?
C30 O3 1.274(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 O2 91.9(3) 2 . ?
O1 Eu1 O9 81.6(3) 2 . ?
O2 Eu1 O9 72.7(3) . . ?
O1 Eu1 O7 75.4(3) 2 . ?
O2 Eu1 O7 78.1(3) . . ?
O9 Eu1 O7 141.9(3) . . ?
O1 Eu1 O4 154.0(3) 2 . ?
O2 Eu1 O4 103.5(3) . . ?
O9 Eu1 O4 83.3(3) . . ?
O7 Eu1 O4 127.8(3) . . ?
O1 Eu1 O8 101.5(3) 2 . ?
O2 Eu1 O8 143.3(3) . . ?
O9 Eu1 O8 142.7(3) . . ?
O7 Eu1 O8 72.6(3) . . ?
O4 Eu1 O8 78.5(3) . . ?
O1 Eu1 O10 74.5(3) 2 . ?
O2 Eu1 O10 143.2(3) . . ?
O9 Eu1 O10 71.6(3) . . ?
O7 Eu1 O10 128.3(3) . . ?
O4 Eu1 O10 80.8(3) . . ?
O8 Eu1 O10 73.6(3) . . ?
O1 Eu1 O3 152.8(3) 2 . ?
O2 Eu1 O3 73.2(3) . . ?
O9 Eu1 O3 113.9(3) . . ?
O7 Eu1 O3 79.3(3) . . ?
O4 Eu1 O3 53.2(3) . . ?
O8 Eu1 O3 79.9(3) . . ?
O10 Eu1 O3 130.6(3) . . ?
O1 Eu1 C30 179.2(3) 2 . ?
O2 Eu1 C30 87.3(3) . . ?
O9 Eu1 C30 98.2(3) . . ?
O7 Eu1 C30 104.4(3) . . ?
O4 Eu1 C30 26.5(3) . . ?
O8 Eu1 C30 79.1(3) . . ?
O10 Eu1 C30 106.2(3) . . ?
O3 Eu1 C30 26.7(3) . . ?
C10 O1 Eu1 142.5(6) . 2 ?
C10 O2 Eu1 148.9(7) . . ?
C30 O4 Eu1 94.2(6) . . ?
Eu1 O7 H7A 109.3 . . ?
Eu1 O7 H7C 109.3 . . ?
H7A O7 H7C 109.5 . . ?
Eu1 O8 H8A 109.3 . . ?
Eu1 O8 H8C 109.3 . . ?
H8A O8 H8C 109.5 . . ?
Eu1 O9 H9A 109.3 . . ?
Eu1 O9 H9D 109.3 . . ?
H9A O9 H9D 109.5 . . ?
Eu1 O10 H10B 109.3 . . ?
Eu1 O10 H10C 109.3 . . ?
H10B O10 H10C 109.5 . . ?
HW1A OW1 HW1C 109.5 . . ?
C9 C1 C2 114.8(9) . . ?
C9 C1 C10 128.9(11) . . ?
C2 C1 C10 116.4(9) . . ?
C3 C2 C1 121.8(9) . . ?
C3 C2 H2A 119.1 . . ?
C1 C2 H2A 119.1 . . ?
C2 C3 C4 124.9(10) . . ?
C2 C3 C8 116.3(10) . . ?
C4 C3 C8 118.7(10) . . ?
C5 C4 C3 121.6(12) . . ?
C5 C4 H4A 119.2 . . ?
C3 C4 H4A 119.2 . . ?
C4 C5 C6 119.1(12) . . ?
C4 C5 H5A 120.4 . . ?
C6 C5 H5A 120.4 . . ?
C5 C6 C7 121.9(11) . . ?
C5 C6 H6A 119.0 . . ?
C7 C6 H6A 119.0 . . ?
C6 C7 C8 119.8(11) . . ?
C6 C7 H7B 120.1 . . ?
C8 C7 H7B 120.1 . . ?
N1 C8 C7 119.6(11) . . ?
N1 C8 C3 121.6(10) . . ?
C7 C8 C3 118.8(11) . . ?
N1 C9 C1 126.9(11) . . ?
N1 C9 H9B 116.6 . . ?
C1 C9 H9B 116.6 . . ?
O2 C10 O1 125.7(9) . . ?
O2 C10 C1 122.9(9) . . ?
O1 C10 C1 111.4(9) . . ?
N2 C11 C12 126.1(10) . . ?
N2 C11 H11A 116.9 . . ?
C12 C11 H11A 116.9 . . ?
C13 C12 C11 116.9(9) . . ?
C13 C12 C20 122.0(9) . . ?
C11 C12 C20 121.1(9) . . ?
C12 C13 C14 120.2(10) . . ?
C12 C13 H13A 119.9 . . ?
C14 C13 H13A 119.9 . . ?
C19 C14 C13 118.6(10) . . ?
C19 C14 C15 118.3(10) . . ?
C13 C14 C15 123.1(10) . . ?
C16 C15 C14 120.7(11) . . ?
C16 C15 H15A 119.7 . . ?
C14 C15 H15A 119.7 . . ?
C15 C16 C17 119.3(11) . . ?
C15 C16 H16A 120.4 . . ?
C17 C16 H16A 120.4 . . ?
C18 C17 C16 121.3(11) . . ?
C18 C17 H17A 119.4 . . ?
C16 C17 H17A 119.3 . . ?
C17 C18 C19 120.4(11) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
N2 C19 C18 119.3(10) . . ?
N2 C19 C14 120.7(10) . . ?
C18 C19 C14 120.0(11) . . ?
O6 C20 O5 123.5(10) . . ?
O6 C20 C12 118.5(9) . . ?
O5 C20 C12 117.9(9) . . ?
C22 C21 C29 119.5(10) . . ?
C22 C21 C30 120.1(10) . . ?
C29 C21 C30 120.4(11) . . ?
C21 C22 C23 118.5(11) . . ?
C21 C22 H22A 120.8 . . ?
C23 C22 H22A 120.8 . . ?
C28 C23 C24 119.9(12) . . ?
C28 C23 C22 118.1(11) . . ?
C24 C23 C22 122.0(12) . . ?
C25 C24 C23 119.3(15) . . ?
C25 C24 H24A 120.3 . . ?
C23 C24 H24A 120.3 . . ?
C24 C25 C26 121.3(15) . . ?
C24 C25 H25A 119.3 . . ?
C26 C25 H25A 119.3 . . ?
C25 C26 C27 121.3(13) . . ?
C25 C26 H26A 119.4 . . ?
C27 C26 H26A 119.4 . . ?
C26 C27 C28 119.6(14) . . ?
C26 C27 H27A 120.2 . . ?
C28 C27 H27A 120.2 . . ?
N3 C28 C27 119.1(13) . . ?
N3 C28 C23 122.4(11) . . ?
C27 C28 C23 118.5(13) . . ?
N3 C29 C21 123.9(12) . . ?
N3 C29 H29A 118.0 . . ?
C21 C29 H29A 118.0 . . ?
O4 C30 O3 118.9(10) . . ?
O4 C30 C21 121.4(10) . . ?
O3 C30 C21 119.6(10) . . ?
O4 C30 Eu1 59.2(5) . . ?
O3 C30 Eu1 59.8(6) . . ?
C21 C30 Eu1 173.2(7) . . ?
C9 N1 C8 118.6(9) . . ?
C11 N2 C19 117.5(9) . . ?
C29 N3 C28 117.6(11) . . ?
C30 O3 Eu1 93.5(7) . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         2.519
_refine_diff_density_min         -2.008
_refine_diff_density_rms         0.189
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1041894'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;

#================================================================   
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H28 N3 O11 Sm'
_chemical_formula_weight         756.91

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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.8460(16)
_cell_length_b                   11.390(2)
_cell_length_c                   16.620(3)
_cell_angle_alpha                81.81(3)
_cell_angle_beta                 87.79(3)
_cell_angle_gamma                79.34(3)
_cell_volume                     1444.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6534
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             758
_exptl_absorpt_coefficient_mu    2.101
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7022
_exptl_absorpt_correction_T_max  0.7434
_exptl_absorpt_process_details   ?

_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  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14302
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6534
_reflns_number_gt                5660
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0467P)²+0.0000P] 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         6534
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0875
_refine_ls_wR_factor_gt          0.0838
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.52209(2) 0.645848(17) 0.109189(10) 0.02140(7) Uani 1 1 d . . .
O1 O 0.5015(4) 0.6968(3) 0.24915(17) 0.0410(7) Uani 1 1 d . . .
O2 O 0.7066(4) 0.5474(3) 0.22546(16) 0.0371(7) Uani 1 1 d . . .
O3 O 0.4423(4) 0.6706(3) -0.02628(15) 0.0317(6) Uani 1 1 d . . .
O4 O 0.4999(4) 0.4396(3) 0.12678(16) 0.0340(7) Uani 1 1 d . . .
O5 O 0.9724(4) 0.1904(3) -0.01292(17) 0.0363(7) Uani 1 1 d . . .
O6 O 1.0035(4) 0.3269(3) 0.06536(18) 0.0368(7) Uani 1 1 d . . .
O7 O 0.7828(4) 0.5593(3) 0.03807(18) 0.0373(7) Uani 1 1 d . . .
H7A H 0.7623 0.5663 -0.0124 0.056 Uiso 1 1 d R . .
H7D H 0.8121 0.4851 0.0567 0.056 Uiso 1 1 d R . .
O8 O 0.3487(4) 0.8506(3) 0.08253(18) 0.0364(7) Uani 1 1 d . . .
H8A H 0.3162 0.8645 0.0333 0.055 Uiso 1 1 d R . .
H8C H 0.2603 0.8558 0.1139 0.055 Uiso 1 1 d R . .
O9 O 0.2158(4) 0.6353(3) 0.12956(19) 0.0418(8) Uani 1 1 d . . .
H9B H 0.2061 0.5671 0.1558 0.063 Uiso 1 1 d R . .
H9C H 0.1678 0.6909 0.1565 0.063 Uiso 1 1 d R . .
O10 O 0.7279(4) 0.7823(3) 0.10239(19) 0.0409(8) Uani 1 1 d . . .
H10A H 0.7355 0.8162 0.0537 0.061 Uiso 1 1 d R . .
H10B H 0.6928 0.8356 0.1332 0.061 Uiso 1 1 d R . .
N1 N 0.5953(6) 0.6371(4) 0.4977(2) 0.0466(10) Uani 1 1 d . . .
N2 N 0.6482(5) 0.9511(3) -0.1564(2) 0.0332(8) Uani 1 1 d . . .
N3 N 0.7989(5) -0.0308(3) 0.1792(2) 0.0330(8) Uani 1 1 d . . .
C1 C 0.5709(6) 0.6588(4) 0.4183(2) 0.0370(10) Uani 1 1 d . . .
H1B H 0.4915 0.7267 0.3977 0.044 Uiso 1 1 calc R . .
C2 C 0.6600(6) 0.5835(4) 0.3624(2) 0.0317(9) Uani 1 1 d . . .
C3 C 0.7780(6) 0.4846(4) 0.3921(2) 0.0322(9) Uani 1 1 d . . .
H3B H 0.8412 0.4363 0.3566 0.039 Uiso 1 1 calc R . .
C4 C 0.8037(6) 0.4559(4) 0.4766(2) 0.0377(10) Uani 1 1 d . . .
C5 C 0.9194(8) 0.3518(5) 0.5119(3) 0.0495(13) Uani 1 1 d . . .
H5A H 0.9821 0.2994 0.4788 0.059 Uiso 1 1 calc R . .
C6 C 0.9388(8) 0.3285(5) 0.5941(3) 0.0562(16) Uani 1 1 d . . .
H6A H 1.0164 0.2611 0.6168 0.067 Uiso 1 1 calc R . .
C7 C 0.8424(9) 0.4054(6) 0.6443(3) 0.0629(18) Uani 1 1 d . . .
H7B H 0.8550 0.3877 0.7004 0.075 Uiso 1 1 calc R . .
C8 C 0.7306(8) 0.5056(6) 0.6126(3) 0.0551(15) Uani 1 1 d . . .
H8B H 0.6677 0.5558 0.6470 0.066 Uiso 1 1 calc R . .
C9 C 0.7094(6) 0.5340(4) 0.5272(2) 0.0399(11) Uani 1 1 d . . .
C10 C 0.6207(5) 0.6117(4) 0.2741(2) 0.0276(8) Uani 1 1 d . . .
C11 C 0.5852(6) 0.8595(4) -0.1150(2) 0.0301(8) Uani 1 1 d . . .
H11A H 0.5457 0.8665 -0.0621 0.036 Uiso 1 1 calc R . .
C12 C 0.5746(5) 0.7529(3) -0.1460(2) 0.0250(7) Uani 1 1 d . . .
C13 C 0.6321(5) 0.7420(4) -0.2237(2) 0.0305(8) Uani 1 1 d . . .
H13A H 0.6262 0.6726 -0.2460 0.037 Uiso 1 1 calc R . .
C14 C 0.7011(5) 0.8377(4) -0.2702(2) 0.0299(8) Uani 1 1 d . . .
C15 C 0.7622(6) 0.8317(4) -0.3517(3) 0.0408(11) Uani 1 1 d . . .
H15A H 0.7609 0.7629 -0.3758 0.049 Uiso 1 1 calc R . .
C16 C 0.8229(7) 0.9282(5) -0.3944(3) 0.0455(11) Uani 1 1 d . . .
H16A H 0.8650 0.9241 -0.4472 0.055 Uiso 1 1 calc R . .
C17 C 0.8222(6) 1.0313(4) -0.3595(3) 0.0456(12) Uani 1 1 d . . .
H17A H 0.8616 1.0963 -0.3899 0.055 Uiso 1 1 calc R . .
C18 C 0.7644(6) 1.0404(4) -0.2807(3) 0.0421(11) Uani 1 1 d . . .
H18A H 0.7653 1.1106 -0.2583 0.050 Uiso 1 1 calc R . .
C19 C 0.7038(5) 0.9419(4) -0.2343(2) 0.0298(8) Uani 1 1 d . . .
C20 C 0.5005(5) 0.6528(3) -0.0960(2) 0.0250(8) Uani 1 1 d . . .
C21 C 0.8620(5) 0.0394(4) 0.1203(2) 0.0313(9) Uani 1 1 d . . .
H21A H 0.8894 0.0099 0.0711 0.038 Uiso 1 1 calc R . .
C22 C 0.8908(5) 0.1564(4) 0.1265(2) 0.0278(8) Uani 1 1 d . . .
C23 C 0.8532(6) 0.1987(4) 0.1992(2) 0.0320(9) Uani 1 1 d . . .
H23A H 0.8735 0.2746 0.2059 0.038 Uiso 1 1 calc R . .
C24 C 0.7834(5) 0.1273(4) 0.2641(2) 0.0305(8) Uani 1 1 d . . .
C25 C 0.7371(6) 0.1676(5) 0.3402(3) 0.0419(11) Uani 1 1 d . . .
H25A H 0.7500 0.2445 0.3485 0.050 Uiso 1 1 calc R . .
C26 C 0.6733(7) 0.0933(5) 0.4016(3) 0.0475(12) Uani 1 1 d . . .
H26A H 0.6439 0.1196 0.4516 0.057 Uiso 1 1 calc R . .
C27 C 0.6525(7) -0.0211(5) 0.3892(3) 0.0483(12) Uani 1 1 d . . .
H27A H 0.6101 -0.0709 0.4315 0.058 Uiso 1 1 calc R . .
C28 C 0.6928(6) -0.0620(4) 0.3164(3) 0.0378(10) Uani 1 1 d . . .
H28A H 0.6764 -0.1386 0.3092 0.045 Uiso 1 1 calc R . .
C29 C 0.7594(5) 0.0117(4) 0.2520(2) 0.0297(8) Uani 1 1 d . . .
C30 C 0.9606(5) 0.2301(4) 0.0548(2) 0.0284(8) Uani 1 1 d . . .
OW1 O 0.0529(4) 0.4575(3) 0.1923(2) 0.0418(7) Uani 1 1 d . . .
HW1B H 0.0902 0.3864 0.2156 0.063 Uiso 1 1 d R . .
HW1C H -0.0102 0.4973 0.2255 0.063 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
Sm1 O3 2.325(3) . ?
Sm1 O4 2.364(3) . ?
Sm1 O10 2.429(3) . ?
Sm1 O9 2.436(3) . ?
Sm1 O7 2.440(3) . ?
Sm1 O8 2.462(3) . ?
Sm1 O2 2.467(3) . ?
Sm1 O1 2.469(3) . ?
Sm1 C10 2.830(4) . ?
O1 C10 1.251(5) . ?
O2 C10 1.260(5) . ?
O3 C20 1.259(5) . ?
O4 C20 1.233(5) 2_665 ?
O5 C30 1.265(5) . ?
O6 C30 1.248(5) . ?
O7 H7A 0.8500 . ?
O7 H7D 0.8500 . ?
O8 H8A 0.8501 . ?
O8 H8C 0.8499 . ?
O9 H9B 0.8501 . ?
O9 H9C 0.8499 . ?
O10 H10A 0.8501 . ?
O10 H10B 0.8500 . ?
N1 C1 1.322(6) . ?
N1 C9 1.379(7) . ?
N2 C11 1.330(5) . ?
N2 C19 1.364(5) . ?
N3 C21 1.315(5) . ?
N3 C29 1.369(5) . ?
C1 C2 1.429(6) . ?
C1 H1B 0.9300 . ?
C2 C3 1.363(6) . ?
C2 C10 1.490(5) . ?
C3 C4 1.411(5) . ?
C3 H3B 0.9300 . ?
C4 C9 1.402(7) . ?
C4 C5 1.421(7) . ?
C5 C6 1.362(7) . ?
C5 H5A 0.9300 . ?
C6 C7 1.397(9) . ?
C6 H6A 0.9300 . ?
C7 C8 1.357(9) . ?
C7 H7B 0.9300 . ?
C8 C9 1.420(6) . ?
C8 H8B 0.9300 . ?
C11 C12 1.403(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.365(5) . ?
C12 C20 1.506(5) . ?
C13 C14 1.422(5) . ?
C13 H13A 0.9300 . ?
C14 C19 1.407(6) . ?
C14 C15 1.426(6) . ?
C15 C16 1.372(6) . ?
C15 H15A 0.9300 . ?
C16 C17 1.381(7) . ?
C16 H16A 0.9300 . ?
C17 C18 1.381(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.415(5) . ?
C18 H18A 0.9300 . ?
C20 O4 1.233(5) 2_665 ?
C21 C22 1.412(5) . ?
C21 H21A 0.9300 . ?
C22 C23 1.365(6) . ?
C22 C30 1.503(5) . ?
C23 C24 1.413(5) . ?
C23 H23A 0.9300 . ?
C24 C29 1.407(6) . ?
C24 C25 1.418(6) . ?
C25 C26 1.370(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.387(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.363(7) . ?
C27 H27A 0.9300 . ?
C28 C29 1.409(6) . ?
C28 H28A 0.9300 . ?
OW1 HW1B 0.8500 . ?
OW1 HW1C 0.8500 . ?

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
O3 Sm1 O4 91.84(10) . . ?
O3 Sm1 O10 100.76(11) . . ?
O4 Sm1 O10 143.18(12) . . ?
O3 Sm1 O9 81.37(11) . . ?
O4 Sm1 O9 72.83(11) . . ?
O10 Sm1 O9 142.95(12) . . ?
O3 Sm1 O7 75.27(11) . . ?
O4 Sm1 O7 78.58(10) . . ?
O10 Sm1 O7 71.61(11) . . ?
O9 Sm1 O7 142.19(11) . . ?
O3 Sm1 O8 74.50(11) . . ?
O4 Sm1 O8 142.57(11) . . ?
O10 Sm1 O8 74.22(11) . . ?
O9 Sm1 O8 70.77(11) . . ?
O7 Sm1 O8 128.39(10) . . ?
O3 Sm1 O2 152.88(11) . . ?
O4 Sm1 O2 73.41(11) . . ?
O10 Sm1 O2 80.23(11) . . ?
O9 Sm1 O2 114.27(10) . . ?
O7 Sm1 O2 79.48(10) . . ?
O8 Sm1 O2 130.53(10) . . ?
O3 Sm1 O1 154.57(11) . . ?
O4 Sm1 O1 103.63(10) . . ?
O10 Sm1 O1 78.88(11) . . ?
O9 Sm1 O1 84.06(12) . . ?
O7 Sm1 O1 127.14(11) . . ?
O8 Sm1 O1 81.07(11) . . ?
O2 Sm1 O1 52.53(10) . . ?
O3 Sm1 C10 179.10(11) . . ?
O4 Sm1 C10 87.31(11) . . ?
O10 Sm1 C10 79.77(11) . . ?
O9 Sm1 C10 98.66(11) . . ?
O7 Sm1 C10 104.25(12) . . ?
O8 Sm1 C10 106.37(12) . . ?
O2 Sm1 C10 26.40(11) . . ?
O1 Sm1 C10 26.20(11) . . ?
C10 O1 Sm1 93.2(2) . . ?
C10 O2 Sm1 93.1(2) . . ?
C20 O3 Sm1 142.5(3) . . ?
C20 O4 Sm1 148.5(2) 2_665 . ?
Sm1 O7 H7A 109.4 . . ?
Sm1 O7 H7D 109.4 . . ?
H7A O7 H7D 109.5 . . ?
Sm1 O8 H8A 109.4 . . ?
Sm1 O8 H8C 109.3 . . ?
H8A O8 H8C 109.5 . . ?
Sm1 O9 H9B 109.3 . . ?
Sm1 O9 H9C 109.3 . . ?
H9B O9 H9C 109.5 . . ?
Sm1 O10 H10A 109.4 . . ?
Sm1 O10 H10B 109.3 . . ?
H10A O10 H10B 109.5 . . ?
C1 N1 C9 117.3(4) . . ?
C11 N2 C19 118.1(3) . . ?
C21 N3 C29 118.1(4) . . ?
N1 C1 C2 123.4(5) . . ?
N1 C1 H1B 118.3 . . ?
C2 C1 H1B 118.3 . . ?
C3 C2 C1 118.6(4) . . ?
C3 C2 C10 121.2(4) . . ?
C1 C2 C10 120.2(4) . . ?
C2 C3 C4 119.8(4) . . ?
C2 C3 H3B 120.1 . . ?
C4 C3 H3B 120.1 . . ?
C9 C4 C3 117.8(4) . . ?
C9 C4 C5 119.4(4) . . ?
C3 C4 C5 122.8(5) . . ?
C6 C5 C4 120.2(6) . . ?
C6 C5 H5A 119.9 . . ?
C4 C5 H5A 119.9 . . ?
C5 C6 C7 120.2(6) . . ?
C5 C6 H6A 119.9 . . ?
C7 C6 H6A 119.9 . . ?
C8 C7 C6 121.0(5) . . ?
C8 C7 H7B 119.5 . . ?
C6 C7 H7B 119.5 . . ?
C7 C8 C9 120.3(6) . . ?
C7 C8 H8B 119.8 . . ?
C9 C8 H8B 119.8 . . ?
N1 C9 C4 122.9(4) . . ?
N1 C9 C8 118.3(5) . . ?
C4 C9 C8 118.8(5) . . ?
O1 C10 O2 120.8(4) . . ?
O1 C10 C2 120.1(4) . . ?
O2 C10 C2 119.1(4) . . ?
O1 C10 Sm1 60.6(2) . . ?
O2 C10 Sm1 60.5(2) . . ?
C2 C10 Sm1 173.7(2) . . ?
N2 C11 C12 124.1(4) . . ?
N2 C11 H11A 117.9 . . ?
C12 C11 H11A 117.9 . . ?
C13 C12 C11 118.2(3) . . ?
C13 C12 C20 120.3(3) . . ?
C11 C12 C20 121.4(3) . . ?
C12 C13 C14 119.6(4) . . ?
C12 C13 H13A 120.2 . . ?
C14 C13 H13A 120.2 . . ?
C19 C14 C13 118.0(4) . . ?
C19 C14 C15 119.8(4) . . ?
C13 C14 C15 122.1(4) . . ?
C16 C15 C14 119.4(4) . . ?
C16 C15 H15A 120.3 . . ?
C14 C15 H15A 120.3 . . ?
C15 C16 C17 120.5(4) . . ?
C15 C16 H16A 119.7 . . ?
C17 C16 H16A 119.7 . . ?
C18 C17 C16 121.7(4) . . ?
C18 C17 H17A 119.1 . . ?
C16 C17 H17A 119.1 . . ?
C17 C18 C19 119.4(4) . . ?
C17 C18 H18A 120.3 . . ?
C19 C18 H18A 120.3 . . ?
N2 C19 C14 121.8(3) . . ?
N2 C19 C18 119.1(4) . . ?
C14 C19 C18 119.1(4) . . ?
O4 C20 O3 125.2(3) 2_665 . ?
O4 C20 C12 117.6(3) 2_665 . ?
O3 C20 C12 117.2(3) . . ?
N3 C21 C22 124.5(4) . . ?
N3 C21 H21A 117.8 . . ?
C22 C21 H21A 117.8 . . ?
C23 C22 C21 117.7(3) . . ?
C23 C22 C30 122.2(4) . . ?
C21 C22 C30 120.2(4) . . ?
C22 C23 C24 120.0(4) . . ?
C22 C23 H23A 120.0 . . ?
C24 C23 H23A 120.0 . . ?
C29 C24 C23 118.0(4) . . ?
C29 C24 C25 119.3(4) . . ?
C23 C24 C25 122.7(4) . . ?
C26 C25 C24 120.0(4) . . ?
C26 C25 H25A 120.0 . . ?
C24 C25 H25A 120.0 . . ?
C25 C26 C27 120.1(5) . . ?
C25 C26 H26A 119.9 . . ?
C27 C26 H26A 119.9 . . ?
C28 C27 C26 121.4(4) . . ?
C28 C27 H27A 119.3 . . ?
C26 C27 H27A 119.3 . . ?
C27 C28 C29 120.1(4) . . ?
C27 C28 H28A 120.0 . . ?
C29 C28 H28A 120.0 . . ?
N3 C29 C24 121.7(3) . . ?
N3 C29 C28 119.2(4) . . ?
C24 C29 C28 119.1(4) . . ?
O6 C30 O5 123.7(3) . . ?
O6 C30 C22 118.2(4) . . ?
O5 C30 C22 118.1(3) . . ?
HW1B OW1 HW1C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.122
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1041895'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;

#================================================================   

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H28 Gd N3 O11'
_chemical_formula_weight         763.80

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.8374(16)
_cell_length_b                   11.382(2)
_cell_length_c                   16.602(3)
_cell_angle_alpha                81.96(3)
_cell_angle_beta                 87.88(3)
_cell_angle_gamma                79.49(3)
_cell_volume                     1441.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6446
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      27.48

_exptl_crystal_description       yellow
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.639
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.102
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             762
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7371
_exptl_absorpt_correction_T_max  0.7846
_exptl_absorpt_process_details   ?

_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  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14076
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.47
_reflns_number_total             6446
_reflns_number_gt                5998
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1000P)²+0.0000P] 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         6446
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.1075
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_restrained_S_all      0.925
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001

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
Gd1 Gd 0.976851(18) 0.354442(12) 0.391233(8) 0.02075(8) Uani 1 1 d . . .
N1 N 0.8532(4) 0.0488(3) 0.6557(2) 0.0319(7) Uani 1 1 d . . .
N2 N 0.9044(6) 0.3619(4) 0.0035(2) 0.0465(10) Uani 1 1 d . . .
N3 N 0.2981(5) -0.0305(3) 0.6783(2) 0.0344(7) Uani 1 1 d . . .
O1 O 0.7925(4) 0.4526(3) 0.27569(16) 0.0365(6) Uani 1 1 d . . .
O2 O 1.0013(4) 0.3043(3) 0.25248(17) 0.0399(7) Uani 1 1 d . . .
O3 O 1.0579(4) 0.3306(3) 0.52527(16) 0.0323(6) Uani 1 1 d . . .
O4 O 1.0003(4) 0.5589(2) 0.37385(16) 0.0329(6) Uani 1 1 d . . .
O5 O 0.4713(4) 0.1905(3) 0.48613(18) 0.0350(6) Uani 1 1 d . . .
O6 O 0.5040(4) 0.3278(3) 0.56484(17) 0.0361(6) Uani 1 1 d . . .
O7 O 1.1469(4) 0.1509(2) 0.41797(19) 0.0374(6) Uani 1 1 d . . .
H7A H 1.1790 0.1371 0.4673 0.056 Uiso 1 1 d R . .
H7D H 1.2356 0.1451 0.3868 0.056 Uiso 1 1 d R . .
O8 O 0.7185(4) 0.4402(2) 0.46120(17) 0.0344(6) Uani 1 1 d . . .
H8A H 0.7390 0.4332 0.5117 0.052 Uiso 1 1 d R . .
H8C H 0.6895 0.5144 0.4426 0.052 Uiso 1 1 d R . .
O9 O 0.7739(4) 0.2183(3) 0.39781(18) 0.0385(7) Uani 1 1 d . . .
H9A H 0.7657 0.1847 0.4465 0.058 Uiso 1 1 d R . .
H9B H 0.6751 0.2575 0.3821 0.058 Uiso 1 1 d R . .
O10 O 1.2794(4) 0.3640(3) 0.3687(2) 0.0400(7) Uani 1 1 d . . .
H10A H 1.3294 0.3553 0.4143 0.060 Uiso 1 1 d R . .
H10C H 1.2891 0.4321 0.3423 0.060 Uiso 1 1 d R . .
OW1 O 1.4461(4) 0.5416(3) 0.3069(2) 0.0396(7) Uani 1 1 d . . .
HW1A H 1.5058 0.5451 0.3479 0.059 Uiso 1 1 d R . .
HW1C H 1.4091 0.6126 0.2835 0.059 Uiso 1 1 d R . .
C1 C 0.9149(5) 0.1404(3) 0.6144(2) 0.0281(7) Uani 1 1 d . . .
H1B H 0.9545 0.1334 0.5615 0.034 Uiso 1 1 calc R . .
C2 C 0.9244(4) 0.2480(3) 0.6457(2) 0.0246(7) Uani 1 1 d . . .
C3 C 0.8672(5) 0.2579(3) 0.7231(2) 0.0281(7) Uani 1 1 d . . .
H3B H 0.8727 0.3276 0.7454 0.034 Uiso 1 1 calc R . .
C4 C 0.7997(5) 0.1634(3) 0.7698(2) 0.0299(8) Uani 1 1 d . . .
C5 C 0.7394(6) 0.1677(4) 0.8506(3) 0.0418(10) Uani 1 1 d . . .
H5A H 0.7422 0.2361 0.8750 0.050 Uiso 1 1 calc R . .
C6 C 0.6770(6) 0.0731(4) 0.8934(3) 0.0447(10) Uani 1 1 d . . .
H6A H 0.6332 0.0785 0.9458 0.054 Uiso 1 1 calc R . .
C7 C 0.6785(6) -0.0318(4) 0.8588(3) 0.0462(11) Uani 1 1 d . . .
H7B H 0.6408 -0.0971 0.8896 0.055 Uiso 1 1 calc R . .
C8 C 0.7345(6) -0.0406(4) 0.7801(3) 0.0390(9) Uani 1 1 d . . .
H8B H 0.7324 -0.1104 0.7573 0.047 Uiso 1 1 calc R . .
C9 C 0.7958(5) 0.0589(3) 0.7342(2) 0.0291(7) Uani 1 1 d . . .
C10 C 0.9982(4) 0.3479(3) 0.5954(2) 0.0236(6) Uani 1 1 d . . .
C11 C 0.9288(6) 0.3410(4) 0.0834(2) 0.0375(9) Uani 1 1 d . . .
H11A H 1.0087 0.2737 0.1042 0.045 Uiso 1 1 calc R . .
C12 C 0.8397(5) 0.4157(4) 0.1383(2) 0.0303(8) Uani 1 1 d . . .
C13 C 0.7230(5) 0.5155(4) 0.1094(2) 0.0320(8) Uani 1 1 d . . .
H13A H 0.6614 0.5643 0.1451 0.038 Uiso 1 1 calc R . .
C14 C 0.6964(6) 0.5441(4) 0.0243(2) 0.0365(9) Uani 1 1 d . . .
C15 C 0.5802(6) 0.6489(4) -0.0109(3) 0.0448(10) Uani 1 1 d . . .
H15A H 0.5168 0.7012 0.0221 0.054 Uiso 1 1 calc R . .
C16 C 0.5633(8) 0.6713(5) -0.0927(3) 0.0559(14) Uani 1 1 d . . .
H16A H 0.4868 0.7392 -0.1155 0.067 Uiso 1 1 calc R . .
C17 C 0.6581(8) 0.5947(6) -0.1435(3) 0.0610(17) Uani 1 1 d . . .
H17A H 0.6458 0.6131 -0.1996 0.073 Uiso 1 1 calc R . .
C18 C 0.7685(8) 0.4932(5) -0.1118(3) 0.0560(15) Uani 1 1 d . . .
H18A H 0.8292 0.4419 -0.1463 0.067 Uiso 1 1 calc R . .
C19 C 0.7910(7) 0.4657(5) -0.0265(3) 0.0409(10) Uani 1 1 d . . .
C20 C 0.8807(5) 0.3880(4) 0.2271(2) 0.0285(8) Uani 1 1 d . . .
C21 C 0.3610(5) 0.0400(3) 0.6195(2) 0.0302(7) Uani 1 1 d . . .
H21A H 0.3870 0.0109 0.5700 0.036 Uiso 1 1 calc R . .
C22 C 0.3921(4) 0.1566(3) 0.6260(2) 0.0253(7) Uani 1 1 d . . .
C23 C 0.3520(5) 0.1999(4) 0.6986(2) 0.0303(8) Uani 1 1 d . . .
H23A H 0.3688 0.2769 0.7050 0.036 Uiso 1 1 calc R . .
C24 C 0.2848(5) 0.1269(3) 0.7641(2) 0.0284(7) Uani 1 1 d . . .
C25 C 0.2383(6) 0.1672(4) 0.8406(3) 0.0417(10) Uani 1 1 d . . .
H25A H 0.2504 0.2442 0.8492 0.050 Uiso 1 1 calc R . .
C26 C 0.1752(7) 0.0917(5) 0.9017(3) 0.0493(12) Uani 1 1 d . . .
H26A H 0.1461 0.1177 0.9519 0.059 Uiso 1 1 calc R . .
C27 C 0.1546(7) -0.0222(4) 0.8894(3) 0.0460(11) Uani 1 1 d . . .
H27A H 0.1143 -0.0726 0.9320 0.055 Uiso 1 1 calc R . .
C28 C 0.1921(6) -0.0626(4) 0.8158(3) 0.0394(9) Uani 1 1 d . . .
H28A H 0.1720 -0.1382 0.8079 0.047 Uiso 1 1 calc R . .
C29 C 0.2615(5) 0.0108(3) 0.7520(2) 0.0290(7) Uani 1 1 d . . .
C30 C 0.4602(5) 0.2307(3) 0.5539(2) 0.0277(7) 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
Gd1 O3 2.303(3) . ?
Gd1 O4 2.345(3) . ?
Gd1 O9 2.405(3) . ?
Gd1 O10 2.407(3) . ?
Gd1 O8 2.413(3) . ?
Gd1 O2 2.442(3) . ?
Gd1 O7 2.444(3) . ?
Gd1 O1 2.456(3) . ?
Gd1 C20 2.810(4) . ?
N1 C1 1.323(5) . ?
N1 C9 1.375(5) . ?
N2 C11 1.330(5) . ?
N2 C19 1.385(7) . ?
N3 C21 1.315(5) . ?
N3 C29 1.373(5) . ?
O1 C20 1.269(5) . ?
O2 C20 1.252(5) . ?
O3 C10 1.267(4) . ?
O4 C10 1.241(4) 2_766 ?
O5 C30 1.267(5) . ?
O6 C30 1.254(5) . ?
O7 H7A 0.8500 . ?
O7 H7D 0.8500 . ?
O8 H8A 0.8501 . ?
O8 H8C 0.8500 . ?
O9 H9A 0.8500 . ?
O9 H9B 0.8499 . ?
O10 H10A 0.8499 . ?
O10 H10C 0.8500 . ?
OW1 HW1A 0.8500 . ?
OW1 HW1C 0.8500 . ?
C1 C2 1.411(5) . ?
C1 H1B 0.9300 . ?
C2 C3 1.358(5) . ?
C2 C10 1.504(4) . ?
C3 C4 1.408(5) . ?
C3 H3B 0.9300 . ?
C4 C9 1.407(5) . ?
C4 C5 1.409(6) . ?
C5 C6 1.363(6) . ?
C5 H5A 0.9300 . ?
C6 C7 1.393(7) . ?
C6 H6A 0.9300 . ?
C7 C8 1.373(7) . ?
C7 H7B 0.9300 . ?
C8 C9 1.423(5) . ?
C8 H8B 0.9300 . ?
C10 O4 1.241(4) 2_766 ?
C11 C12 1.412(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.363(6) . ?
C12 C20 1.498(5) . ?
C13 C14 1.419(5) . ?
C13 H13A 0.9300 . ?
C14 C19 1.407(7) . ?
C14 C15 1.429(7) . ?
C15 C16 1.352(7) . ?
C15 H15A 0.9300 . ?
C16 C17 1.395(9) . ?
C16 H16A 0.9300 . ?
C17 C18 1.364(9) . ?
C17 H17A 0.9300 . ?
C18 C19 1.418(6) . ?
C18 H18A 0.9300 . ?
C21 C22 1.412(5) . ?
C21 H21A 0.9300 . ?
C22 C23 1.370(5) . ?
C22 C30 1.504(5) . ?
C23 C24 1.419(5) . ?
C23 H23A 0.9300 . ?
C24 C25 1.423(6) . ?
C24 C29 1.409(5) . ?
C25 C26 1.373(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.379(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.368(6) . ?
C27 H27A 0.9300 . ?
C28 C29 1.412(5) . ?
C28 H28A 0.9300 . ?

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
O3 Gd1 O4 91.62(10) . . ?
O3 Gd1 O9 101.07(11) . . ?
O4 Gd1 O9 143.64(11) . . ?
O3 Gd1 O10 81.96(11) . . ?
O4 Gd1 O10 72.97(11) . . ?
O9 Gd1 O10 142.15(11) . . ?
O3 Gd1 O8 75.76(11) . . ?
O4 Gd1 O8 78.73(10) . . ?
O9 Gd1 O8 71.81(10) . . ?
O10 Gd1 O8 143.20(11) . . ?
O3 Gd1 O2 153.99(11) . . ?
O4 Gd1 O2 103.24(10) . . ?
O9 Gd1 O2 79.53(11) . . ?
O10 Gd1 O2 82.18(12) . . ?
O8 Gd1 O2 127.68(11) . . ?
O3 Gd1 O7 74.42(11) . . ?
O4 Gd1 O7 142.76(10) . . ?
O9 Gd1 O7 73.57(11) . . ?
O10 Gd1 O7 71.01(11) . . ?
O8 Gd1 O7 128.15(10) . . ?
O2 Gd1 O7 80.98(10) . . ?
O3 Gd1 O1 152.85(10) . . ?
O4 Gd1 O1 73.39(11) . . ?
O9 Gd1 O1 80.43(11) . . ?
O10 Gd1 O1 113.63(10) . . ?
O8 Gd1 O1 79.11(10) . . ?
O2 Gd1 O1 53.16(10) . . ?
O7 Gd1 O1 130.67(10) . . ?
O3 Gd1 C20 178.82(10) . . ?
O4 Gd1 C20 87.26(10) . . ?
O9 Gd1 C20 80.06(11) . . ?
O10 Gd1 C20 97.36(11) . . ?
O8 Gd1 C20 104.35(11) . . ?
O2 Gd1 C20 26.40(11) . . ?
O7 Gd1 C20 106.29(11) . . ?
O1 Gd1 C20 26.83(11) . . ?
C1 N1 C9 118.0(3) . . ?
C11 N2 C19 117.2(4) . . ?
C21 N3 C29 118.2(3) . . ?
C20 O1 Gd1 92.3(2) . . ?
C20 O2 Gd1 93.4(2) . . ?
C10 O3 Gd1 141.8(3) . . ?
C10 O4 Gd1 148.8(2) 2_766 . ?
Gd1 O7 H7A 109.3 . . ?
Gd1 O7 H7D 109.4 . . ?
H7A O7 H7D 109.5 . . ?
Gd1 O8 H8A 109.3 . . ?
Gd1 O8 H8C 109.4 . . ?
H8A O8 H8C 109.5 . . ?
Gd1 O9 H9A 109.6 . . ?
Gd1 O9 H9B 109.3 . . ?
H9A O9 H9B 109.5 . . ?
Gd1 O10 H10A 109.3 . . ?
Gd1 O10 H10C 109.3 . . ?
H10A O10 H10C 109.5 . . ?
HW1A OW1 HW1C 109.5 . . ?
N1 C1 C2 124.0(3) . . ?
N1 C1 H1B 118.0 . . ?
C2 C1 H1B 118.0 . . ?
C3 C2 C1 117.9(3) . . ?
C3 C2 C10 121.0(3) . . ?
C1 C2 C10 121.1(3) . . ?
C2 C3 C4 120.6(3) . . ?
C2 C3 H3B 119.7 . . ?
C4 C3 H3B 119.7 . . ?
C3 C4 C9 117.9(4) . . ?
C3 C4 C5 123.3(4) . . ?
C9 C4 C5 118.7(4) . . ?
C6 C5 C4 120.9(4) . . ?
C6 C5 H5A 119.6 . . ?
C4 C5 H5A 119.6 . . ?
C5 C6 C7 120.2(4) . . ?
C5 C6 H6A 119.9 . . ?
C7 C6 H6A 119.9 . . ?
C8 C7 C6 121.4(4) . . ?
C8 C7 H7B 119.3 . . ?
C6 C7 H7B 119.3 . . ?
C7 C8 C9 118.9(4) . . ?
C7 C8 H8B 120.6 . . ?
C9 C8 H8B 120.6 . . ?
N1 C9 C4 121.6(3) . . ?
N1 C9 C8 118.5(4) . . ?
C4 C9 C8 119.9(4) . . ?
O4 C10 O3 124.3(3) 2_766 . ?
O4 C10 C2 117.7(3) 2_766 . ?
O3 C10 C2 118.0(3) . . ?
N2 C11 C12 123.4(4) . . ?
N2 C11 H11A 118.3 . . ?
C12 C11 H11A 118.3 . . ?
C13 C12 C11 119.6(4) . . ?
C13 C12 C20 120.6(4) . . ?
C11 C12 C20 119.7(4) . . ?
C12 C13 C14 119.3(4) . . ?
C12 C13 H13A 120.4 . . ?
C14 C13 H13A 120.4 . . ?
C19 C14 C15 119.6(4) . . ?
C19 C14 C13 117.8(4) . . ?
C15 C14 C13 122.7(4) . . ?
C16 C15 C14 119.4(5) . . ?
C16 C15 H15A 120.3 . . ?
C14 C15 H15A 120.3 . . ?
C15 C16 C17 121.3(5) . . ?
C15 C16 H16A 119.3 . . ?
C17 C16 H16A 119.3 . . ?
C18 C17 C16 120.8(4) . . ?
C18 C17 H17A 119.6 . . ?
C16 C17 H17A 119.6 . . ?
C17 C18 C19 120.0(5) . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
N2 C19 C14 122.7(4) . . ?
N2 C19 C18 118.5(5) . . ?
C14 C19 C18 118.9(5) . . ?
O2 C20 O1 120.8(4) . . ?
O2 C20 C12 120.7(4) . . ?
O1 C20 C12 118.5(4) . . ?
O2 C20 Gd1 60.2(2) . . ?
O1 C20 Gd1 60.9(2) . . ?
C12 C20 Gd1 174.3(3) . . ?
N3 C21 C22 124.8(3) . . ?
N3 C21 H21A 117.6 . . ?
C22 C21 H21A 117.6 . . ?
C23 C22 C21 117.5(3) . . ?
C23 C22 C30 122.2(3) . . ?
C21 C22 C30 120.2(3) . . ?
C22 C23 C24 119.8(3) . . ?
C22 C23 H23A 120.1 . . ?
C24 C23 H23A 120.1 . . ?
C23 C24 C25 122.5(4) . . ?
C23 C24 C29 118.4(4) . . ?
C25 C24 C29 119.1(4) . . ?
C26 C25 C24 119.6(4) . . ?
C26 C25 H25A 120.2 . . ?
C24 C25 H25A 120.2 . . ?
C25 C26 C27 120.7(4) . . ?
C25 C26 H26A 119.6 . . ?
C27 C26 H26A 119.6 . . ?
C28 C27 C26 121.4(4) . . ?
C28 C27 H27A 119.3 . . ?
C26 C27 H27A 119.3 . . ?
C27 C28 C29 119.8(4) . . ?
C27 C28 H28A 120.1 . . ?
C29 C28 H28A 120.1 . . ?
N3 C29 C28 119.3(4) . . ?
N3 C29 C24 121.3(3) . . ?
C28 C29 C24 119.3(4) . . ?
O6 C30 O5 124.1(3) . . ?
O6 C30 C22 117.9(3) . . ?
O5 C30 C22 118.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.447
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.182
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1041896'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;

#================================================================   

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H28 N3 O11 Tb'
_chemical_formula_weight         765.48

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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.834(3)
_cell_length_b                   11.385(4)
_cell_length_c                   16.574(6)
_cell_angle_alpha                81.799(4)
_cell_angle_beta                 87.851(4)
_cell_angle_gamma                79.435(4)
_cell_volume                     1438.2(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5398
_cell_measurement_theta_min      1.24
_cell_measurement_theta_max      26.95

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.146
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             764
_exptl_absorpt_coefficient_mu    2.528
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10506
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.24
_diffrn_reflns_theta_max         26.95
_reflns_number_total             5398
_reflns_number_gt                4976
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0000P)²+118.8712P] 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         5398
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.1029
_refine_ls_wR_factor_ref         0.2228
_refine_ls_wR_factor_gt          0.2206
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_restrained_S_all      1.214
_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
Tb1 Tb 0.47667(11) 0.35432(7) 0.39140(5) 0.0205(3) Uani 1 1 d . . .
N1 N 0.405(3) 0.3627(19) 0.0030(13) 0.050(5) Uani 1 1 d . . .
N2 N 0.642(3) 0.9538(19) 0.3447(13) 0.050(5) Uani 1 1 d . . .
N3 N 0.199(2) 1.0312(15) 0.3213(10) 0.035(4) Uani 1 1 d . . .
O1 O 0.295(2) 0.4535(13) 0.2765(9) 0.040(3) Uani 1 1 d . . .
O2 O 0.500(2) 0.3040(14) 0.2539(9) 0.043(4) Uani 1 1 d . . .
O3 O 0.5583(18) 0.3308(12) 0.5243(7) 0.031(3) Uani 1 1 d . . .
O4 O 0.498(2) 0.5598(12) 0.3749(8) 0.039(3) Uani 1 1 d . . .
O5 O -0.003(2) 0.6723(13) 0.4360(9) 0.038(3) Uani 1 1 d . . .
O6 O 0.0273(19) 0.8103(12) 0.5144(8) 0.036(3) Uani 1 1 d . . .
O7 O 0.2201(19) 0.4388(12) 0.4613(9) 0.038(3) Uani 1 1 d . . .
H7C H 0.1898 0.5128 0.4423 0.056 Uiso 1 1 d R . .
H7D H 0.1387 0.4011 0.4545 0.056 Uiso 1 1 d R . .
O8 O 0.7781(19) 0.3653(14) 0.3695(9) 0.043(4) Uani 1 1 d . . .
H8C H 0.8260 0.3093 0.3428 0.064 Uiso 1 1 d R . .
H8D H 0.7875 0.4333 0.3426 0.064 Uiso 1 1 d R . .
O9 O 0.2740(18) 0.2174(12) 0.3971(9) 0.036(3) Uani 1 1 d . . .
H9B H 0.1752 0.2564 0.3811 0.054 Uiso 1 1 d R . .
H9C H 0.3100 0.1641 0.3663 0.054 Uiso 1 1 d R . .
O10 O 0.635(2) 0.1558(11) 0.4147(9) 0.044(4) Uani 1 1 d . . .
H10B H 0.5709 0.1065 0.4060 0.065 Uiso 1 1 d R . .
H10C H 0.7229 0.1492 0.3828 0.065 Uiso 1 1 d R . .
OW1 O 0.946(2) 0.5420(15) 0.3083(10) 0.050(4) Uani 1 1 d . . .
HW1A H 1.0044 0.5456 0.3496 0.075 Uiso 1 1 d R . .
HW1B H 1.0093 0.5018 0.2755 0.075 Uiso 1 1 d R . .
C1 C 0.427(3) 0.343(2) 0.0830(12) 0.037(5) Uani 1 1 d . . .
H1B H 0.5068 0.2747 0.1037 0.045 Uiso 1 1 calc R . .
C2 C 0.341(3) 0.4153(18) 0.1392(13) 0.035(5) Uani 1 1 d . . .
C3 C 0.223(3) 0.5152(19) 0.1097(12) 0.034(4) Uani 1 1 d . . .
H3B H 0.1612 0.5644 0.1451 0.041 Uiso 1 1 calc R . .
C4 C 0.196(3) 0.543(2) 0.0241(13) 0.041(5) Uani 1 1 d . . .
C5 C 0.086(3) 0.645(2) -0.0104(15) 0.049(6) Uani 1 1 d . . .
H5A H 0.0223 0.6975 0.0225 0.059 Uiso 1 1 calc R . .
C6 C 0.071(5) 0.669(3) -0.0942(19) 0.074(10) Uani 1 1 d . . .
H6A H -0.0024 0.7384 -0.1173 0.089 Uiso 1 1 calc R . .
C7 C 0.160(4) 0.595(3) -0.1426(15) 0.062(8) Uani 1 1 d . . .
H7B H 0.1453 0.6129 -0.1987 0.074 Uiso 1 1 calc R . .
C8 C 0.268(4) 0.495(3) -0.1122(13) 0.060(8) Uani 1 1 d . . .
H8B H 0.3308 0.4455 -0.1471 0.071 Uiso 1 1 calc R . .
C9 C 0.289(3) 0.465(2) -0.0251(14) 0.042(5) Uani 1 1 d . . .
C10 C 0.379(3) 0.3854(18) 0.2266(11) 0.029(4) Uani 1 1 d . . .
C11 C 0.584(3) 0.858(2) 0.3865(16) 0.050(6) Uani 1 1 d . . .
H11A H 0.5461 0.8614 0.4401 0.060 Uiso 1 1 calc R . .
C12 C 0.580(3) 0.753(2) 0.3519(16) 0.050(6) Uani 1 1 d . . .
C13 C 0.636(3) 0.741(2) 0.2799(15) 0.050(6) Uani 1 1 d . . .
H13A H 0.6334 0.6694 0.2595 0.060 Uiso 1 1 calc R . .
C14 C 0.700(2) 0.8340(17) 0.2313(12) 0.030(4) Uani 1 1 d . . .
C15 C 0.762(3) 0.8306(19) 0.1493(13) 0.040(5) Uani 1 1 d . . .
H15A H 0.7612 0.7625 0.1244 0.048 Uiso 1 1 calc R . .
C16 C 0.822(3) 0.926(2) 0.1079(15) 0.050(6) Uani 1 1 d . . .
H16A H 0.8643 0.9225 0.0549 0.061 Uiso 1 1 calc R . .
C17 C 0.823(3) 1.029(2) 0.1424(17) 0.055(7) Uani 1 1 d . . .
H17A H 0.8627 1.0936 0.1118 0.066 Uiso 1 1 calc R . .
C18 C 0.765(3) 1.038(2) 0.2208(15) 0.045(6) Uani 1 1 d . . .
H18A H 0.7694 1.1083 0.2431 0.054 Uiso 1 1 calc R . .
C19 C 0.700(3) 0.9426(19) 0.2676(13) 0.037(5) Uani 1 1 d . . .
C20 C 0.508(3) 0.642(2) 0.4010(16) 0.050(6) Uani 1 1 d . . .
C21 C 0.138(3) 0.9590(17) 0.3799(13) 0.032(4) Uani 1 1 d . . .
H21A H 0.1118 0.9883 0.4294 0.038 Uiso 1 1 calc R . .
C22 C 0.109(2) 0.8424(15) 0.3753(12) 0.026(4) Uani 1 1 d . . .
C23 C 0.147(3) 0.8029(17) 0.3022(12) 0.030(4) Uani 1 1 d . . .
H23A H 0.1280 0.7267 0.2951 0.036 Uiso 1 1 calc R . .
C24 C 0.213(3) 0.8732(18) 0.2376(12) 0.033(4) Uani 1 1 d . . .
C25 C 0.260(3) 0.833(2) 0.1586(13) 0.044(5) Uani 1 1 d . . .
H25A H 0.2441 0.7567 0.1496 0.053 Uiso 1 1 calc R . .
C26 C 0.326(3) 0.907(2) 0.0977(13) 0.049(6) Uani 1 1 d . . .
H26A H 0.3583 0.8803 0.0480 0.059 Uiso 1 1 calc R . .
C27 C 0.345(3) 1.023(2) 0.1099(14) 0.048(6) Uani 1 1 d . . .
H27A H 0.3843 1.0743 0.0674 0.058 Uiso 1 1 calc R . .
C28 C 0.306(3) 1.0613(19) 0.1839(13) 0.036(5) Uani 1 1 d . . .
H28A H 0.3250 1.1369 0.1921 0.043 Uiso 1 1 calc R . .
C29 C 0.238(2) 0.9891(17) 0.2470(12) 0.029(4) Uani 1 1 d . . .
C30 C 0.036(2) 0.7688(17) 0.4467(12) 0.027(4) 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
Tb1 O3 2.282(12) . ?
Tb1 O4 2.353(14) . ?
Tb1 O10 2.358(14) . ?
Tb1 O7 2.396(14) . ?
Tb1 O8 2.399(15) . ?
Tb1 O9 2.411(12) . ?
Tb1 O2 2.419(15) . ?
Tb1 O1 2.433(15) . ?
N1 C1 1.32(3) . ?
N1 C9 1.37(3) . ?
N2 C11 1.35(3) . ?
N2 C19 1.35(3) . ?
N3 C21 1.31(2) . ?
N3 C29 1.39(3) . ?
O1 C10 1.29(2) . ?
O2 C10 1.25(2) . ?
O3 C20 1.38(3) 2_666 ?
O4 C20 1.10(3) . ?
O5 C30 1.23(2) . ?
O6 C30 1.27(2) . ?
O7 H7C 0.8500 . ?
O7 H7D 0.8500 . ?
O8 H8C 0.8500 . ?
O8 H8D 0.8500 . ?
O9 H9B 0.8500 . ?
O9 H9C 0.8499 . ?
O10 H10B 0.8500 . ?
O10 H10C 0.8500 . ?
OW1 HW1A 0.8500 . ?
OW1 HW1B 0.8501 . ?
C1 C2 1.41(3) . ?
C1 H1B 0.9300 . ?
C2 C3 1.37(3) . ?
C2 C10 1.47(3) . ?
C3 C4 1.42(3) . ?
C3 H3B 0.9300 . ?
C4 C9 1.38(3) . ?
C4 C5 1.38(3) . ?
C5 C6 1.38(4) . ?
C5 H5A 0.9300 . ?
C6 C7 1.33(4) . ?
C6 H6A 0.9300 . ?
C7 C8 1.33(4) . ?
C7 H7B 0.9300 . ?
C8 C9 1.44(3) . ?
C8 H8B 0.9300 . ?
C11 C12 1.40(3) . ?
C11 H11A 0.9300 . ?
C12 C13 1.27(3) . ?
C12 C20 1.59(4) . ?
C13 C14 1.39(3) . ?
C13 H13A 0.9300 . ?
C14 C15 1.43(3) . ?
C14 C19 1.45(3) . ?
C15 C16 1.35(3) . ?
C15 H15A 0.9300 . ?
C16 C17 1.37(4) . ?
C16 H16A 0.9300 . ?
C17 C18 1.37(3) . ?
C17 H17A 0.9300 . ?
C18 C19 1.41(3) . ?
C18 H18A 0.9300 . ?
C20 O3 1.38(3) 2_666 ?
C21 C22 1.40(2) . ?
C21 H21A 0.9300 . ?
C22 C23 1.36(3) . ?
C22 C30 1.51(3) . ?
C23 C24 1.39(3) . ?
C23 H23A 0.9300 . ?
C24 C29 1.40(3) . ?
C24 C25 1.46(3) . ?
C25 C26 1.37(3) . ?
C25 H25A 0.9300 . ?
C26 C27 1.40(3) . ?
C26 H26A 0.9300 . ?
C27 C28 1.36(3) . ?
C27 H27A 0.9300 . ?
C28 C29 1.39(3) . ?
C28 H28A 0.9300 . ?

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
O3 Tb1 O4 91.1(5) . . ?
O3 Tb1 O10 75.9(5) . . ?
O4 Tb1 O10 144.4(6) . . ?
O3 Tb1 O7 75.8(5) . . ?
O4 Tb1 O7 78.4(5) . . ?
O10 Tb1 O7 127.8(5) . . ?
O3 Tb1 O8 81.5(5) . . ?
O4 Tb1 O8 72.9(5) . . ?
O10 Tb1 O8 72.5(5) . . ?
O7 Tb1 O8 142.8(5) . . ?
O3 Tb1 O9 101.7(5) . . ?
O4 Tb1 O9 143.6(5) . . ?
O10 Tb1 O9 72.0(5) . . ?
O7 Tb1 O9 72.1(5) . . ?
O8 Tb1 O9 142.3(5) . . ?
O3 Tb1 O2 153.9(5) . . ?
O4 Tb1 O2 104.0(5) . . ?
O10 Tb1 O2 79.6(5) . . ?
O7 Tb1 O2 127.6(5) . . ?
O8 Tb1 O2 82.8(5) . . ?
O9 Tb1 O2 78.7(5) . . ?
O3 Tb1 O1 152.8(5) . . ?
O4 Tb1 O1 73.1(5) . . ?
O10 Tb1 O1 129.4(5) . . ?
O7 Tb1 O1 79.3(5) . . ?
O8 Tb1 O1 113.3(5) . . ?
O9 Tb1 O1 80.8(5) . . ?
O2 Tb1 O1 53.3(5) . . ?
C1 N1 C9 115(2) . . ?
C11 N2 C19 116(2) . . ?
C21 N3 C29 117.6(16) . . ?
C10 O1 Tb1 93.3(11) . . ?
C10 O2 Tb1 95.2(11) . . ?
C20 O3 Tb1 140.0(14) 2_666 . ?
C20 O4 Tb1 150.4(17) . . ?
Tb1 O7 H7C 109.5 . . ?
Tb1 O7 H7D 109.5 . . ?
H7C O7 H7D 109.5 . . ?
Tb1 O8 H8C 109.5 . . ?
Tb1 O8 H8D 109.5 . . ?
H8C O8 H8D 109.5 . . ?
Tb1 O9 H9B 109.5 . . ?
Tb1 O9 H9C 109.5 . . ?
H9B O9 H9C 109.5 . . ?
Tb1 O10 H10B 109.5 . . ?
Tb1 O10 H10C 109.5 . . ?
H10B O10 H10C 109.5 . . ?
HW1A OW1 HW1B 109.5 . . ?
N1 C1 C2 125(2) . . ?
N1 C1 H1B 117.3 . . ?
C2 C1 H1B 117.3 . . ?
C3 C2 C1 118(2) . . ?
C3 C2 C10 121.4(19) . . ?
C1 C2 C10 121(2) . . ?
C2 C3 C4 119(2) . . ?
C2 C3 H3B 120.5 . . ?
C4 C3 H3B 120.5 . . ?
C9 C4 C5 120(2) . . ?
C9 C4 C3 118(2) . . ?
C5 C4 C3 122(2) . . ?
C6 C5 C4 119(3) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C7 C6 C5 121(3) . . ?
C7 C6 H6A 119.3 . . ?
C5 C6 H6A 119.3 . . ?
C6 C7 C8 121(2) . . ?
C6 C7 H7B 119.3 . . ?
C8 C7 H7B 119.3 . . ?
C7 C8 C9 120(3) . . ?
C7 C8 H8B 120.0 . . ?
C9 C8 H8B 120.0 . . ?
N1 C9 C4 124(2) . . ?
N1 C9 C8 118(2) . . ?
C4 C9 C8 118(2) . . ?
O2 C10 O1 118.1(17) . . ?
O2 C10 C2 122.6(18) . . ?
O1 C10 C2 118.8(18) . . ?
N2 C11 C12 122(2) . . ?
N2 C11 H11A 118.9 . . ?
C12 C11 H11A 118.9 . . ?
C13 C12 C11 122(3) . . ?
C13 C12 C20 116(2) . . ?
C11 C12 C20 122(2) . . ?
C12 C13 C14 121(2) . . ?
C12 C13 H13A 119.6 . . ?
C14 C13 H13A 119.6 . . ?
C13 C14 C15 125(2) . . ?
C13 C14 C19 116.4(19) . . ?
C15 C14 C19 118.4(18) . . ?
C16 C15 C14 120(2) . . ?
C16 C15 H15A 119.9 . . ?
C14 C15 H15A 119.9 . . ?
C15 C16 C17 121(2) . . ?
C15 C16 H16A 119.3 . . ?
C17 C16 H16A 119.3 . . ?
C18 C17 C16 122(2) . . ?
C18 C17 H17A 119.1 . . ?
C16 C17 H17A 119.1 . . ?
C17 C18 C19 120(2) . . ?
C17 C18 H18A 119.9 . . ?
C19 C18 H18A 119.9 . . ?
N2 C19 C18 120(2) . . ?
N2 C19 C14 122(2) . . ?
C18 C19 C14 118.2(19) . . ?
O4 C20 O3 126(2) . 2_666 ?
O4 C20 C12 124(2) . . ?
O3 C20 C12 110(2) 2_666 . ?
N3 C21 C22 126.4(19) . . ?
N3 C21 H21A 116.8 . . ?
C22 C21 H21A 116.8 . . ?
C23 C22 C21 115.3(17) . . ?
C23 C22 C30 123.1(16) . . ?
C21 C22 C30 121.5(17) . . ?
C22 C23 C24 121.7(18) . . ?
C22 C23 H23A 119.2 . . ?
C24 C23 H23A 119.2 . . ?
C23 C24 C29 119.5(18) . . ?
C23 C24 C25 123.3(19) . . ?
C29 C24 C25 117.2(18) . . ?
C26 C25 C24 120(2) . . ?
C26 C25 H25A 120.0 . . ?
C24 C25 H25A 120.0 . . ?
C25 C26 C27 120(2) . . ?
C25 C26 H26A 119.8 . . ?
C27 C26 H26A 119.8 . . ?
C28 C27 C26 120(2) . . ?
C28 C27 H27A 119.8 . . ?
C26 C27 H27A 119.8 . . ?
C27 C28 C29 121(2) . . ?
C27 C28 H28A 119.5 . . ?
C29 C28 H28A 119.5 . . ?
C28 C29 N3 119.6(18) . . ?
C28 C29 C24 121.0(19) . . ?
N3 C29 C24 119.4(17) . . ?
O5 C30 O6 125.4(18) . . ?
O5 C30 C22 118.2(17) . . ?
O6 C30 C22 116.3(16) . . ?

_diffrn_measured_fraction_theta_max 0.866
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         7.986
_refine_diff_density_min         -4.436
_refine_diff_density_rms         0.335
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1041897'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;

#================================================================   
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H28 Dy N3 O11'
_chemical_formula_weight         769.05

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.8379(16)
_cell_length_b                   11.390(2)
_cell_length_c                   16.582(3)
_cell_angle_alpha                81.94(3)
_cell_angle_beta                 87.87(3)
_cell_angle_gamma                79.35(3)
_cell_volume                     1440.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6510
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.132
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             766
_exptl_absorpt_coefficient_mu    2.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7371
_exptl_absorpt_correction_T_max  0.7846
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14168
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6510
_reflns_number_gt                5697
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0505P)²+1.0625P] 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         6510
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0960
_refine_ls_wR_factor_gt          0.0920
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.02304(3) 0.145651(17) 0.608776(11) 0.02050(8) Uani 1 1 d . . .
N1 N 0.1451(5) 0.4507(3) 0.3445(2) 0.0283(8) Uani 1 1 d . . .
N2 N 0.0949(6) 0.1373(4) 0.9967(3) 0.0390(10) Uani 1 1 d . . .
N3 N 0.7006(5) 0.5310(4) 0.3215(3) 0.0309(9) Uani 1 1 d . . .
O1 O 0.2065(4) 0.0471(3) 0.72455(19) 0.0334(8) Uani 1 1 d . . .
O2 O -0.0010(5) 0.1952(3) 0.7481(2) 0.0350(8) Uani 1 1 d . . .
O3 O -0.0575(4) 0.1697(3) 0.47457(18) 0.0277(7) Uani 1 1 d . . .
O4 O 0.0002(5) -0.0591(3) 0.62637(19) 0.0298(7) Uani 1 1 d . . .
O5 O 0.5294(4) 0.3094(3) 0.5138(2) 0.0319(7) Uani 1 1 d . . .
O6 O 0.4964(5) 0.1725(3) 0.4353(2) 0.0332(7) Uani 1 1 d . . .
O7 O -0.1473(4) 0.3494(3) 0.5815(2) 0.0327(7) Uani 1 1 d . . .
H7A H -0.1794 0.3632 0.5321 0.049 Uiso 1 1 d R . .
H7C H -0.2362 0.3552 0.6127 0.049 Uiso 1 1 d R . .
O8 O 0.2800(4) 0.0585(3) 0.5388(2) 0.0309(7) Uani 1 1 d . . .
H8A H 0.2596 0.0655 0.4881 0.046 Uiso 1 1 d R . .
H8C H 0.3621 0.0952 0.5460 0.046 Uiso 1 1 d R . .
O9 O -0.2790(4) 0.1349(3) 0.6313(2) 0.0360(8) Uani 1 1 d . . .
H9A H -0.3289 0.1438 0.5857 0.054 Uiso 1 1 d R . .
H9C H -0.3265 0.1906 0.6585 0.054 Uiso 1 1 d R . .
O10 O 0.2267(4) 0.2807(3) 0.6027(2) 0.0347(8) Uani 1 1 d . . .
H10A H 0.2347 0.3144 0.5539 0.052 Uiso 1 1 d R . .
H10C H 0.1916 0.3341 0.6335 0.052 Uiso 1 1 d R . .
OW1 O -0.4443(4) -0.0426(3) 0.6928(2) 0.0364(8) Uani 1 1 d . . .
HW1A H -0.5039 -0.0459 0.6516 0.055 Uiso 1 1 d R . .
HW1C H -0.5074 -0.0025 0.7260 0.055 Uiso 1 1 d R . .
C1 C 0.0862(6) 0.3594(4) 0.3858(3) 0.0265(9) Uani 1 1 d . . .
H1B H 0.0495 0.3656 0.4393 0.032 Uiso 1 1 calc R . .
C2 C 0.0749(5) 0.2519(4) 0.3541(3) 0.0211(8) Uani 1 1 d . . .
C3 C 0.1328(6) 0.2419(4) 0.2769(3) 0.0250(9) Uani 1 1 d . . .
H3B H 0.1281 0.1720 0.2547 0.030 Uiso 1 1 calc R . .
C4 C 0.2002(6) 0.3364(4) 0.2301(3) 0.0270(9) Uani 1 1 d . . .
C5 C 0.2616(7) 0.3328(5) 0.1483(3) 0.0370(11) Uani 1 1 d . . .
H5A H 0.2611 0.2645 0.1236 0.044 Uiso 1 1 calc R . .
C6 C 0.3201(8) 0.4278(5) 0.1069(3) 0.0428(13) Uani 1 1 d . . .
H6A H 0.3613 0.4241 0.0539 0.051 Uiso 1 1 calc R . .
C7 C 0.3200(7) 0.5311(5) 0.1420(4) 0.0421(13) Uani 1 1 d . . .
H7B H 0.3590 0.5960 0.1115 0.051 Uiso 1 1 calc R . .
C8 C 0.2646(7) 0.5403(4) 0.2195(3) 0.0364(11) Uani 1 1 d . . .
H8B H 0.2667 0.6103 0.2421 0.044 Uiso 1 1 calc R . .
C9 C 0.2036(6) 0.4418(4) 0.2659(3) 0.0265(9) Uani 1 1 d . . .
C10 C 0.0002(5) 0.1516(4) 0.4044(3) 0.0216(8) Uani 1 1 d . . .
C11 C 0.0732(7) 0.1584(5) 0.9171(3) 0.0340(11) Uani 1 1 d . . .
H11A H -0.0049 0.2267 0.8962 0.041 Uiso 1 1 calc R . .
C12 C 0.1606(6) 0.0844(4) 0.8619(3) 0.0264(9) Uani 1 1 d . . .
C13 C 0.2780(6) -0.0149(4) 0.8906(3) 0.0292(10) Uani 1 1 d . . .
H13A H 0.3401 -0.0632 0.8547 0.035 Uiso 1 1 calc R . .
C14 C 0.3053(7) -0.0441(5) 0.9759(3) 0.0321(10) Uani 1 1 d . . .
C15 C 0.4200(8) -0.1483(5) 1.0107(3) 0.0425(13) Uani 1 1 d . . .
H15A H 0.4844 -0.2002 0.9777 0.051 Uiso 1 1 calc R . .
C16 C 0.4351(9) -0.1716(6) 1.0940(4) 0.0516(16) Uani 1 1 d . . .
H16A H 0.5095 -0.2404 1.1171 0.062 Uiso 1 1 calc R . .
C17 C 0.3413(9) -0.0944(7) 1.1443(3) 0.0553(18) Uani 1 1 d . . .
H17A H 0.3544 -0.1118 1.2005 0.066 Uiso 1 1 calc R . .
C18 C 0.2307(9) 0.0061(6) 1.1123(3) 0.0488(15) Uani 1 1 d . . .
H18A H 0.1682 0.0569 1.1465 0.059 Uiso 1 1 calc R . .
C19 C 0.2099(7) 0.0341(5) 1.0261(3) 0.0371(12) Uani 1 1 d . . .
C20 C 0.1197(6) 0.1116(4) 0.7732(3) 0.0257(9) Uani 1 1 d . . .
C21 C 0.6382(6) 0.4604(4) 0.3802(3) 0.0264(9) Uani 1 1 d . . .
H21A H 0.6114 0.4893 0.4298 0.032 Uiso 1 1 calc R . .
C22 C 0.6091(5) 0.3444(4) 0.3732(3) 0.0248(9) Uani 1 1 d . . .
C23 C 0.6473(6) 0.3010(4) 0.3013(3) 0.0267(9) Uani 1 1 d . . .
H23A H 0.6298 0.2242 0.2951 0.032 Uiso 1 1 calc R . .
C24 C 0.7138(6) 0.3733(4) 0.2361(3) 0.0259(9) Uani 1 1 d . . .
C25 C 0.7630(7) 0.3335(5) 0.1590(3) 0.0392(12) Uani 1 1 d . . .
H25A H 0.7534 0.2559 0.1508 0.047 Uiso 1 1 calc R . .
C26 C 0.8229(7) 0.4071(5) 0.0983(3) 0.0409(12) Uani 1 1 d . . .
H26A H 0.8494 0.3814 0.0478 0.049 Uiso 1 1 calc R . .
C27 C 0.8454(7) 0.5228(5) 0.1112(3) 0.0429(13) Uani 1 1 d . . .
H27A H 0.8878 0.5728 0.0690 0.051 Uiso 1 1 calc R . .
C28 C 0.8061(7) 0.5624(5) 0.1844(3) 0.0367(11) Uani 1 1 d . . .
H28A H 0.8233 0.6386 0.1923 0.044 Uiso 1 1 calc R . .
C29 C 0.7398(6) 0.4886(4) 0.2479(3) 0.0258(9) Uani 1 1 d . . .
C30 C 0.5394(5) 0.2687(4) 0.4465(3) 0.0252(9) 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
Dy1 O3 2.301(3) . ?
Dy1 O4 2.349(3) . ?
Dy1 O10 2.403(3) . ?
Dy1 O9 2.406(3) . ?
Dy1 O8 2.408(3) . ?
Dy1 O7 2.445(3) . ?
Dy1 O2 2.446(3) . ?
Dy1 O1 2.453(3) . ?
Dy1 C20 2.812(4) . ?
N1 C1 1.311(6) . ?
N1 C9 1.377(6) . ?
N2 C11 1.319(6) . ?
N2 C19 1.382(7) . ?
N3 C21 1.313(6) . ?
N3 C29 1.379(6) . ?
O1 C20 1.263(6) . ?
O2 C20 1.249(6) . ?
O3 C10 1.263(5) . ?
O4 C10 1.233(5) 2_556 ?
O5 C30 1.262(6) . ?
O6 C30 1.243(6) . ?
O7 H7A 0.8501 . ?
O7 H7C 0.8499 . ?
O8 H8A 0.8501 . ?
O8 H8C 0.8500 . ?
O9 H9A 0.8500 . ?
O9 H9C 0.8501 . ?
O10 H10A 0.8500 . ?
O10 H10C 0.8500 . ?
OW1 HW1A 0.8501 . ?
OW1 HW1C 0.8501 . ?
C1 C2 1.417(6) . ?
C1 H1B 0.9300 . ?
C2 C3 1.355(6) . ?
C2 C10 1.511(6) . ?
C3 C4 1.409(6) . ?
C3 H3B 0.9300 . ?
C4 C5 1.425(7) . ?
C4 C9 1.416(7) . ?
C5 C6 1.343(7) . ?
C5 H5A 0.9300 . ?
C6 C7 1.383(9) . ?
C6 H6A 0.9300 . ?
C7 C8 1.353(8) . ?
C7 H7B 0.9300 . ?
C8 C9 1.417(6) . ?
C8 H8B 0.9300 . ?
C10 O4 1.233(5) 2_556 ?
C11 C12 1.405(7) . ?
C11 H11A 0.9300 . ?
C12 C13 1.359(7) . ?
C12 C20 1.494(6) . ?
C13 C14 1.421(6) . ?
C13 H13A 0.9300 . ?
C14 C19 1.401(8) . ?
C14 C15 1.415(7) . ?
C15 C16 1.374(8) . ?
C15 H15A 0.9300 . ?
C16 C17 1.390(10) . ?
C16 H16A 0.9300 . ?
C17 C18 1.356(10) . ?
C17 H17A 0.9300 . ?
C18 C19 1.429(7) . ?
C18 H18A 0.9300 . ?
C21 C22 1.403(6) . ?
C21 H21A 0.9300 . ?
C22 C23 1.357(7) . ?
C22 C30 1.533(6) . ?
C23 C24 1.409(6) . ?
C23 H23A 0.9300 . ?
C24 C29 1.407(7) . ?
C24 C25 1.431(7) . ?
C25 C26 1.345(7) . ?
C25 H25A 0.9300 . ?
C26 C27 1.408(8) . ?
C26 H26A 0.9300 . ?
C27 C28 1.359(8) . ?
C27 H27A 0.9300 . ?
C28 C29 1.398(7) . ?
C28 H28A 0.9300 . ?

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
O3 Dy1 O4 91.76(12) . . ?
O3 Dy1 O10 101.18(13) . . ?
O4 Dy1 O10 143.32(12) . . ?
O3 Dy1 O9 82.09(13) . . ?
O4 Dy1 O9 72.63(12) . . ?
O10 Dy1 O9 142.72(12) . . ?
O3 Dy1 O8 75.55(12) . . ?
O4 Dy1 O8 78.27(12) . . ?
O10 Dy1 O8 72.17(12) . . ?
O9 Dy1 O8 142.46(13) . . ?
O3 Dy1 O7 74.26(12) . . ?
O4 Dy1 O7 142.82(12) . . ?
O10 Dy1 O7 73.84(12) . . ?
O9 Dy1 O7 71.42(12) . . ?
O8 Dy1 O7 128.33(12) . . ?
O3 Dy1 O2 154.21(11) . . ?
O4 Dy1 O2 103.03(12) . . ?
O10 Dy1 O2 79.48(13) . . ?
O9 Dy1 O2 82.35(13) . . ?
O8 Dy1 O2 127.78(12) . . ?
O7 Dy1 O2 81.34(12) . . ?
O3 Dy1 O1 152.87(11) . . ?
O4 Dy1 O1 73.18(13) . . ?
O10 Dy1 O1 80.33(13) . . ?
O9 Dy1 O1 113.26(12) . . ?
O8 Dy1 O1 79.29(11) . . ?
O7 Dy1 O1 130.85(12) . . ?
O2 Dy1 O1 52.92(11) . . ?
O3 Dy1 C20 178.86(12) . . ?
O4 Dy1 C20 87.11(13) . . ?
O10 Dy1 C20 79.86(13) . . ?
O9 Dy1 C20 97.38(13) . . ?
O8 Dy1 C20 104.39(13) . . ?
O7 Dy1 C20 106.56(13) . . ?
O2 Dy1 C20 26.31(12) . . ?
O1 Dy1 C20 26.66(12) . . ?
C1 N1 C9 118.6(4) . . ?
C11 N2 C19 116.5(4) . . ?
C21 N3 C29 118.0(4) . . ?
C20 O1 Dy1 92.7(3) . . ?
C20 O2 Dy1 93.4(3) . . ?
C10 O3 Dy1 142.4(3) . . ?
C10 O4 Dy1 148.6(3) 2_556 . ?
Dy1 O7 H7A 109.5 . . ?
Dy1 O7 H7C 109.2 . . ?
H7A O7 H7C 109.5 . . ?
Dy1 O8 H8A 109.4 . . ?
Dy1 O8 H8C 109.3 . . ?
H8A O8 H8C 109.5 . . ?
Dy1 O9 H9A 109.3 . . ?
Dy1 O9 H9C 109.5 . . ?
H9A O9 H9C 109.5 . . ?
Dy1 O10 H10A 109.3 . . ?
Dy1 O10 H10C 109.4 . . ?
H10A O10 H10C 109.5 . . ?
HW1A OW1 HW1C 109.5 . . ?
N1 C1 C2 124.1(4) . . ?
N1 C1 H1B 117.9 . . ?
C2 C1 H1B 117.9 . . ?
C3 C2 C1 117.7(4) . . ?
C3 C2 C10 120.9(4) . . ?
C1 C2 C10 121.4(4) . . ?
C2 C3 C4 120.6(4) . . ?
C2 C3 H3B 119.7 . . ?
C4 C3 H3B 119.7 . . ?
C3 C4 C5 123.7(4) . . ?
C3 C4 C9 118.0(4) . . ?
C5 C4 C9 118.3(4) . . ?
C6 C5 C4 120.2(5) . . ?
C6 C5 H5A 119.9 . . ?
C4 C5 H5A 119.9 . . ?
C5 C6 C7 121.0(5) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
C8 C7 C6 121.9(5) . . ?
C8 C7 H7B 119.1 . . ?
C6 C7 H7B 119.1 . . ?
C7 C8 C9 119.1(5) . . ?
C7 C8 H8B 120.5 . . ?
C9 C8 H8B 120.5 . . ?
N1 C9 C8 119.5(4) . . ?
N1 C9 C4 120.9(4) . . ?
C8 C9 C4 119.5(4) . . ?
O4 C10 O3 125.3(4) 2_556 . ?
O4 C10 C2 117.6(4) 2_556 . ?
O3 C10 C2 117.1(4) . . ?
N2 C11 C12 124.2(5) . . ?
N2 C11 H11A 117.9 . . ?
C12 C11 H11A 117.9 . . ?
C13 C12 C11 119.2(4) . . ?
C13 C12 C20 120.4(4) . . ?
C11 C12 C20 120.4(4) . . ?
C12 C13 C14 119.5(4) . . ?
C12 C13 H13A 120.3 . . ?
C14 C13 H13A 120.3 . . ?
C19 C14 C15 120.0(5) . . ?
C19 C14 C13 117.1(5) . . ?
C15 C14 C13 122.9(5) . . ?
C16 C15 C14 119.1(6) . . ?
C16 C15 H15A 120.4 . . ?
C14 C15 H15A 120.4 . . ?
C15 C16 C17 121.3(6) . . ?
C15 C16 H16A 119.3 . . ?
C17 C16 H16A 119.4 . . ?
C18 C17 C16 120.6(5) . . ?
C18 C17 H17A 119.7 . . ?
C16 C17 H17A 119.7 . . ?
C17 C18 C19 120.3(6) . . ?
C17 C18 H18A 119.9 . . ?
C19 C18 H18A 119.9 . . ?
N2 C19 C14 123.4(4) . . ?
N2 C19 C18 117.9(5) . . ?
C14 C19 C18 118.7(5) . . ?
O2 C20 O1 120.7(4) . . ?
O2 C20 C12 120.4(4) . . ?
O1 C20 C12 118.9(4) . . ?
O2 C20 Dy1 60.3(2) . . ?
O1 C20 Dy1 60.6(2) . . ?
C12 C20 Dy1 174.5(3) . . ?
N3 C21 C22 124.4(4) . . ?
N3 C21 H21A 117.8 . . ?
C22 C21 H21A 117.8 . . ?
C23 C22 C21 118.6(4) . . ?
C23 C22 C30 121.4(4) . . ?
C21 C22 C30 120.0(4) . . ?
C22 C23 C24 119.4(4) . . ?
C22 C23 H23A 120.3 . . ?
C24 C23 H23A 120.3 . . ?
C29 C24 C23 118.8(4) . . ?
C29 C24 C25 117.9(4) . . ?
C23 C24 C25 123.2(5) . . ?
C26 C25 C24 120.8(5) . . ?
C26 C25 H25A 119.6 . . ?
C24 C25 H25A 119.6 . . ?
C25 C26 C27 120.1(5) . . ?
C25 C26 H26A 119.9 . . ?
C27 C26 H26A 119.9 . . ?
C28 C27 C26 120.9(5) . . ?
C28 C27 H27A 119.6 . . ?
C26 C27 H27A 119.6 . . ?
C27 C28 C29 120.0(5) . . ?
C27 C28 H28A 120.0 . . ?
C29 C28 H28A 120.0 . . ?
N3 C29 C24 121.0(4) . . ?
N3 C29 C28 118.9(4) . . ?
C24 C29 C28 120.1(4) . . ?
O6 C30 O5 125.0(4) . . ?
O6 C30 C22 117.9(4) . . ?
O5 C30 C22 117.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.072
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.152
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1041898'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;

#================================================================   
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H28 Ho N3 O11'
_chemical_formula_weight         771.48

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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.821(3)
_cell_length_b                   11.361(3)
_cell_length_c                   16.558(5)
_cell_angle_alpha                81.889(4)
_cell_angle_beta                 88.034(12)
_cell_angle_gamma                79.629(3)
_cell_volume                     1432.7(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5468
_cell_measurement_theta_min      1.24
_cell_measurement_theta_max      26.90

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.136
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    2.831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7371
_exptl_absorpt_correction_T_max  0.7846
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10835
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.24
_diffrn_reflns_theta_max         26.90
_reflns_number_total             5468
_reflns_number_gt                4728
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0640P)²+1.8791P] 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     SHELXL
_refine_ls_extinction_coef       0.0031(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5468
_refine_ls_number_parameters     408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_ref         0.1257
_refine_ls_wR_factor_gt          0.1166
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_restrained_S_all      1.165
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.97602(4) 0.35457(3) 0.391810(18) 0.02209(14) Uani 1 1 d . . .
O1 O 1.0012(7) 0.3052(5) 0.2549(3) 0.0393(13) Uani 1 1 d . . .
O2 O 0.7938(7) 0.4517(5) 0.2785(3) 0.0371(12) Uani 1 1 d . . .
O3 O 0.9999(7) 0.5568(4) 0.3749(3) 0.0335(12) Uani 1 1 d . . .
O4 O 1.0594(7) 0.3320(5) 0.5232(3) 0.0355(15) Uani 1 1 d . . .
O5 O 1.2744(7) 0.3635(5) 0.3697(3) 0.0409(13) Uani 1 1 d . . .
H5C H 1.3205 0.3077 0.3425 0.061 Uiso 1 1 d R . .
H5D H 1.2842 0.4317 0.3431 0.061 Uiso 1 1 d R . .
O6 O 1.1435(7) 0.1547(5) 0.4169(3) 0.0356(12) Uani 1 1 d . . .
H6A H 1.1762 0.1403 0.4663 0.053 Uiso 1 1 d R . .
H6C H 1.0811 0.1039 0.4081 0.053 Uiso 1 1 d R . .
O7 O 0.7725(7) 0.2220(5) 0.3974(3) 0.0406(13) Uani 1 1 d . . .
H7A H 0.7644 0.1880 0.4462 0.061 Uiso 1 1 d R . .
H7D H 0.8071 0.1686 0.3665 0.061 Uiso 1 1 d R . .
O8 O 0.7216(6) 0.4395(4) 0.4613(3) 0.0341(12) Uani 1 1 d . . .
H8A H 0.7424 0.4323 0.5120 0.051 Uiso 1 1 d R . .
H8C H 0.6931 0.5139 0.4427 0.051 Uiso 1 1 d R . .
O9 O 0.4683(7) 0.1915(5) 0.4860(3) 0.0355(12) Uani 1 1 d . . .
O10 O 0.5063(7) 0.3287(5) 0.5640(3) 0.0366(12) Uani 1 1 d . . .
N1 N 0.9047(10) 0.3618(7) 0.0051(4) 0.0472(19) Uani 1 1 d . . .
N2 N 1.1446(8) 0.9513(5) 0.3452(4) 0.0344(15) Uani 1 1 d . . .
N3 N 0.2977(8) -0.0311(5) 0.6784(4) 0.0314(14) Uani 1 1 d . . .
C1 C 0.9290(11) 0.3408(8) 0.0849(5) 0.0389(19) Uani 1 1 d . . .
H1B H 1.0085 0.2731 0.1058 0.047 Uiso 1 1 calc R . .
C2 C 0.8414(10) 0.4148(7) 0.1401(4) 0.0327(17) Uani 1 1 d . . .
C3 C 0.7238(11) 0.5152(7) 0.1106(5) 0.0350(18) Uani 1 1 d . . .
H3B H 0.6623 0.5640 0.1464 0.042 Uiso 1 1 calc R . .
C4 C 0.6968(11) 0.5441(7) 0.0262(5) 0.0364(19) Uani 1 1 d . . .
C5 C 0.5817(13) 0.6482(8) -0.0100(6) 0.053(2) Uani 1 1 d . . .
H5B H 0.5189 0.7006 0.0231 0.064 Uiso 1 1 calc R . .
C6 C 0.5620(14) 0.6721(9) -0.0916(6) 0.059(3) Uani 1 1 d . . .
H6B H 0.4850 0.7399 -0.1144 0.070 Uiso 1 1 calc R . .
C7 C 0.6574(15) 0.5948(11) -0.1415(6) 0.065(3) Uani 1 1 d . . .
H7B H 0.6443 0.6129 -0.1978 0.078 Uiso 1 1 calc R . .
C8 C 0.7693(14) 0.4934(10) -0.1108(5) 0.056(3) Uani 1 1 d . . .
H8B H 0.8314 0.4434 -0.1456 0.067 Uiso 1 1 calc R . .
C9 C 0.7902(12) 0.4649(8) -0.0247(5) 0.042(2) Uani 1 1 d . . .
C10 C 0.8796(10) 0.3883(7) 0.2296(5) 0.0315(17) Uani 1 1 d . . .
C11 C 1.0838(9) 0.8592(6) 0.3872(5) 0.0293(16) Uani 1 1 d . . .
H11A H 1.0448 0.8664 0.4403 0.035 Uiso 1 1 calc R . .
C12 C 1.0749(8) 0.7510(6) 0.3563(4) 0.0194(13) Uani 1 1 d . . .
C13 C 1.1312(9) 0.7413(6) 0.2777(4) 0.0281(15) Uani 1 1 d . . .
H13A H 1.1244 0.6716 0.2555 0.034 Uiso 1 1 calc R . .
C14 C 1.1993(10) 0.8355(7) 0.2304(5) 0.0322(17) Uani 1 1 d . . .
C15 C 1.2624(11) 0.8308(8) 0.1498(5) 0.042(2) Uani 1 1 d . . .
H15A H 1.2645 0.7613 0.1257 0.051 Uiso 1 1 calc R . .
C16 C 1.3199(12) 0.9275(8) 0.1075(5) 0.049(2) Uani 1 1 d . . .
H16A H 1.3584 0.9246 0.0539 0.059 Uiso 1 1 calc R . .
C17 C 1.3222(11) 1.0298(8) 0.1427(5) 0.046(2) Uani 1 1 d . . .
H17A H 1.3651 1.0940 0.1127 0.056 Uiso 1 1 calc R . .
C18 C 1.2631(10) 1.0400(7) 0.2208(5) 0.0399(19) Uani 1 1 d . . .
H18A H 1.2646 1.1104 0.2432 0.048 Uiso 1 1 calc R . .
C19 C 1.2001(9) 0.9419(6) 0.2666(5) 0.0305(16) Uani 1 1 d . . .
C20 C 1.0014(9) 0.6501(6) 0.4052(5) 0.0249(15) Uani 1 1 d . . .
H20A H 0.962(5) 0.6568(11) 0.452(6) 0.030 Uiso 1 1 d R . .
C21 C 0.3601(10) 0.0402(7) 0.6183(5) 0.0325(17) Uani 1 1 d . . .
H21A H 0.3841 0.0114 0.5686 0.039 Uiso 1 1 calc R . .
C22 C 0.3924(9) 0.1570(6) 0.6250(4) 0.0270(15) Uani 1 1 d . . .
C23 C 0.3529(9) 0.2003(6) 0.6988(4) 0.0289(15) Uani 1 1 d . . .
H23A H 0.3711 0.2770 0.7055 0.035 Uiso 1 1 calc R . .
C24 C 0.2850(9) 0.1274(7) 0.7637(5) 0.0302(16) Uani 1 1 d . . .
C25 C 0.2391(11) 0.1662(8) 0.8398(5) 0.041(2) Uani 1 1 d . . .
H25A H 0.2522 0.2432 0.8483 0.050 Uiso 1 1 calc R . .
C26 C 0.1756(12) 0.0921(8) 0.9016(5) 0.048(2) Uani 1 1 d . . .
H26A H 0.1481 0.1184 0.9520 0.057 Uiso 1 1 calc R . .
C27 C 0.1521(11) -0.0223(8) 0.8890(5) 0.046(2) Uani 1 1 d . . .
H27A H 0.1078 -0.0716 0.9312 0.055 Uiso 1 1 calc R . .
C28 C 0.1930(11) -0.0640(7) 0.8156(5) 0.0386(18) Uani 1 1 d . . .
H28A H 0.1758 -0.1407 0.8083 0.046 Uiso 1 1 calc R . .
C29 C 0.2617(9) 0.0104(6) 0.7509(4) 0.0294(16) Uani 1 1 d . . .
C30 C 0.4613(9) 0.2305(6) 0.5537(4) 0.0287(15) Uani 1 1 d . . .
OW1 O 0.4462(7) 0.5401(5) 0.3074(3) 0.0410(13) Uani 1 1 d . . .
HW1A H 0.3853 0.5618 0.3480 0.062 Uiso 1 1 d R . .
HW1B H 0.4550 0.6020 0.2731 0.062 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
Ho1 O4 2.259(5) . ?
Ho1 O3 2.315(5) . ?
Ho1 O5 2.367(5) . ?
Ho1 O7 2.372(5) . ?
Ho1 O8 2.383(5) . ?
Ho1 O1 2.405(5) . ?
Ho1 O6 2.397(5) . ?
Ho1 O2 2.409(5) . ?
O1 C10 1.251(9) . ?
O2 C10 1.257(9) . ?
O3 C20 1.237(8) . ?
O4 C20 1.292(9) 2_766 ?
O5 H5C 0.8500 . ?
O5 H5D 0.8500 . ?
O6 H6A 0.8500 . ?
O6 H6C 0.8500 . ?
O7 H7A 0.8500 . ?
O7 H7D 0.8500 . ?
O8 H8A 0.8499 . ?
O8 H8C 0.8500 . ?
O9 C30 1.257(9) . ?
O10 C30 1.264(9) . ?
N1 C1 1.324(10) . ?
N1 C9 1.381(12) . ?
N2 C11 1.324(9) . ?
N2 C19 1.369(10) . ?
N3 C21 1.328(9) . ?
N3 C29 1.353(9) . ?
C1 C2 1.406(11) . ?
C1 H1B 0.9300 . ?
C2 C3 1.372(11) . ?
C2 C10 1.499(10) . ?
C3 C4 1.404(10) . ?
C3 H3B 0.9300 . ?
C4 C9 1.411(12) . ?
C4 C5 1.422(12) . ?
C5 C6 1.349(13) . ?
C5 H5B 0.9300 . ?
C6 C7 1.393(16) . ?
C6 H6B 0.9300 . ?
C7 C8 1.361(16) . ?
C7 H7B 0.9300 . ?
C8 C9 1.424(11) . ?
C8 H8B 0.9300 . ?
C11 C12 1.411(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.372(9) . ?
C12 C20 1.497(9) . ?
C13 C14 1.409(10) . ?
C13 H13A 0.9300 . ?
C14 C15 1.412(10) . ?
C14 C19 1.425(10) . ?
C15 C16 1.357(11) . ?
C15 H15A 0.9300 . ?
C16 C17 1.375(12) . ?
C16 H16A 0.9300 . ?
C17 C18 1.372(12) . ?
C17 H17A 0.9300 . ?
C18 C19 1.412(10) . ?
C18 H18A 0.9300 . ?
C20 O4 1.292(9) 2_766 ?
C20 H20A 0.8271 . ?
C21 C22 1.415(10) . ?
C21 H21A 0.9300 . ?
C22 C23 1.384(10) . ?
C22 C30 1.491(10) . ?
C23 C24 1.412(10) . ?
C23 H23A 0.9300 . ?
C24 C25 1.407(11) . ?
C24 C29 1.419(10) . ?
C25 C26 1.369(11) . ?
C25 H25A 0.9300 . ?
C26 C27 1.390(12) . ?
C26 H26A 0.9300 . ?
C27 C28 1.372(12) . ?
C27 H27A 0.9300 . ?
C28 C29 1.421(10) . ?
C28 H28A 0.9300 . ?
OW1 HW1A 0.8500 . ?
OW1 HW1B 0.8500 . ?

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
O4 Ho1 O3 91.00(18) . . ?
O4 Ho1 O5 81.3(2) . . ?
O3 Ho1 O5 73.12(19) . . ?
O4 Ho1 O7 102.24(19) . . ?
O3 Ho1 O7 143.0(2) . . ?
O5 Ho1 O7 142.5(2) . . ?
O4 Ho1 O8 76.08(19) . . ?
O3 Ho1 O8 78.55(18) . . ?
O5 Ho1 O8 143.14(19) . . ?
O7 Ho1 O8 71.62(18) . . ?
O4 Ho1 O1 153.5(2) . . ?
O3 Ho1 O1 103.33(18) . . ?
O5 Ho1 O1 81.77(19) . . ?
O7 Ho1 O1 79.63(19) . . ?
O8 Ho1 O1 128.21(18) . . ?
O4 Ho1 O6 74.91(18) . . ?
O3 Ho1 O6 142.61(19) . . ?
O5 Ho1 O6 70.62(18) . . ?
O7 Ho1 O6 74.35(19) . . ?
O8 Ho1 O6 128.63(18) . . ?
O1 Ho1 O6 80.32(18) . . ?
O4 Ho1 O2 152.81(19) . . ?
O3 Ho1 O2 73.42(18) . . ?
O5 Ho1 O2 113.83(19) . . ?
O7 Ho1 O2 79.78(19) . . ?
O8 Ho1 O2 79.01(18) . . ?
O1 Ho1 O2 53.67(18) . . ?
O6 Ho1 O2 130.49(17) . . ?
C10 O1 Ho1 93.2(4) . . ?
C10 O2 Ho1 92.8(5) . . ?
C20 O3 Ho1 149.3(5) . . ?
C20 O4 Ho1 141.2(5) 2_766 . ?
Ho1 O5 H5C 109.4 . . ?
Ho1 O5 H5D 109.3 . . ?
H5C O5 H5D 109.5 . . ?
Ho1 O6 H6A 109.3 . . ?
Ho1 O6 H6C 109.3 . . ?
H6A O6 H6C 109.5 . . ?
Ho1 O7 H7A 109.2 . . ?
Ho1 O7 H7D 109.3 . . ?
H7A O7 H7D 109.5 . . ?
Ho1 O8 H8A 109.3 . . ?
Ho1 O8 H8C 109.3 . . ?
H8A O8 H8C 109.5 . . ?
C1 N1 C9 117.1(7) . . ?
C11 N2 C19 118.3(6) . . ?
C21 N3 C29 118.2(6) . . ?
N1 C1 C2 123.8(8) . . ?
N1 C1 H1B 118.1 . . ?
C2 C1 H1B 118.1 . . ?
C3 C2 C1 119.0(7) . . ?
C3 C2 C10 119.8(7) . . ?
C1 C2 C10 121.1(8) . . ?
C2 C3 C4 119.6(8) . . ?
C2 C3 H3B 120.2 . . ?
C4 C3 H3B 120.2 . . ?
C3 C4 C9 117.6(8) . . ?
C3 C4 C5 123.6(8) . . ?
C9 C4 C5 118.9(8) . . ?
C6 C5 C4 121.1(10) . . ?
C6 C5 H5B 119.5 . . ?
C4 C5 H5B 119.5 . . ?
C5 C6 C7 119.7(10) . . ?
C5 C6 H6B 120.2 . . ?
C7 C6 H6B 120.2 . . ?
C8 C7 C6 122.2(9) . . ?
C8 C7 H7B 118.9 . . ?
C6 C7 H7B 118.9 . . ?
C7 C8 C9 119.3(10) . . ?
C7 C8 H8B 120.4 . . ?
C9 C8 H8B 120.4 . . ?
N1 C9 C4 122.8(7) . . ?
N1 C9 C8 118.3(9) . . ?
C4 C9 C8 118.9(9) . . ?
O1 C10 O2 120.2(7) . . ?
O1 C10 C2 119.5(7) . . ?
O2 C10 C2 120.2(7) . . ?
N2 C11 C12 123.9(7) . . ?
N2 C11 H11A 118.0 . . ?
C12 C11 H11A 118.0 . . ?
C13 C12 C11 117.8(6) . . ?
C13 C12 C20 119.8(6) . . ?
C11 C12 C20 122.3(6) . . ?
C12 C13 C14 120.8(6) . . ?
C12 C13 H13A 119.6 . . ?
C14 C13 H13A 119.6 . . ?
C13 C14 C15 123.9(7) . . ?
C13 C14 C19 117.0(7) . . ?
C15 C14 C19 119.1(7) . . ?
C16 C15 C14 119.9(8) . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 120.0 . . ?
C15 C16 C17 121.0(8) . . ?
C15 C16 H16A 119.5 . . ?
C17 C16 H16A 119.5 . . ?
C18 C17 C16 121.9(7) . . ?
C18 C17 H17A 119.0 . . ?
C16 C17 H17A 119.0 . . ?
C17 C18 C19 118.9(7) . . ?
C17 C18 H18A 120.5 . . ?
C19 C18 H18A 120.5 . . ?
N2 C19 C18 118.9(7) . . ?
N2 C19 C14 122.0(6) . . ?
C18 C19 C14 119.1(7) . . ?
O3 C20 O4 124.2(7) . 2_766 ?
O3 C20 C12 119.1(7) . . ?
O4 C20 C12 116.8(6) 2_766 . ?
O3 C20 H20A 120.5 . . ?
O4 C20 H20A 3.7 2_766 . ?
C12 C20 H20A 120.4 . . ?
N3 C21 C22 124.3(7) . . ?
N3 C21 H21A 117.8 . . ?
C22 C21 H21A 117.8 . . ?
C23 C22 C21 117.5(7) . . ?
C23 C22 C30 122.2(6) . . ?
C21 C22 C30 120.2(6) . . ?
C22 C23 C24 119.6(6) . . ?
C22 C23 H23A 120.2 . . ?
C24 C23 H23A 120.2 . . ?
C23 C24 C25 122.8(7) . . ?
C23 C24 C29 118.1(7) . . ?
C25 C24 C29 119.1(7) . . ?
C26 C25 C24 121.0(8) . . ?
C26 C25 H25A 119.5 . . ?
C24 C25 H25A 119.5 . . ?
C25 C26 C27 119.9(8) . . ?
C25 C26 H26A 120.1 . . ?
C27 C26 H26A 120.1 . . ?
C28 C27 C26 121.4(8) . . ?
C28 C27 H27A 119.3 . . ?
C26 C27 H27A 119.3 . . ?
C27 C28 C29 119.8(7) . . ?
C27 C28 H28A 120.1 . . ?
C29 C28 H28A 120.1 . . ?
N3 C29 C28 119.0(7) . . ?
N3 C29 C24 122.1(6) . . ?
C28 C29 C24 118.8(7) . . ?
O10 C30 O9 123.8(7) . . ?
O10 C30 C22 118.6(6) . . ?
O9 C30 C22 117.6(6) . . ?
HW1A OW1 HW1B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.886
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.189
