# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_bjc1_0m
_database_code_depnum_ccdc_archive 'CCDC 1062076'
_audit_update_record             
;
2015-04-28 deposited with the CCDC.
2017-12-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H16 Eu N2 O7'
_chemical_formula_weight         632.38

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'
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           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   9.6425(4)
_cell_length_b                   16.8872(8)
_cell_length_c                   15.5921(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.998(3)
_cell_angle_gamma                90.00
_cell_volume                     2370.33(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.29
_cell_measurement_theta_max      25.01

_exptl_crystal_description       pale
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.058
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1244
_exptl_absorpt_coefficient_mu    2.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_process_details   SADABS

_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  '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            30788
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4159
_reflns_number_gt                3325
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0236P)²+4.0083P] 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         4159
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0642
_refine_ls_wR_factor_gt          0.0586
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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
Eu1 Eu 0.79207(2) 0.975254(12) 0.611178(15) 0.02577(8) Uani 1 1 d . . .
O1 O 0.9015(3) 1.06874(18) 0.5386(2) 0.0384(8) Uani 1 1 d . . .
O2 O 0.9387(3) 0.91263(17) 0.5340(2) 0.0372(8) Uani 1 1 d . . .
O3 O 0.6173(3) 0.90584(17) 0.4939(2) 0.0342(7) Uani 1 1 d . . .
O4 O 0.8661(3) 1.04302(19) 0.7564(2) 0.0431(9) Uani 1 1 d . . .
O5 O 1.0483(3) 0.9845(2) 0.7294(2) 0.0429(8) Uani 1 1 d . . .
O6 O 0.6254(3) 1.07886(18) 0.5714(2) 0.0381(8) Uani 1 1 d . . .
O7 O 1.4154(4) 0.9369(2) 1.0604(2) 0.0593(11) Uani 1 1 d . . .
N1 N 0.8561(4) 0.8420(2) 0.6962(3) 0.0361(9) Uani 1 1 d . . .
N2 N 0.6019(4) 0.9200(2) 0.6820(2) 0.0325(9) Uani 1 1 d . . .
C1 C 0.9819(6) 0.8049(3) 0.7052(4) 0.0523(14) Uani 1 1 d . . .
H1 H 1.0452 0.8279 0.6792 0.063 Uiso 1 1 calc R . .
C2 C 1.0236(7) 0.7337(3) 0.7513(4) 0.0594(16) Uani 1 1 d . . .
H2 H 1.1137 0.7101 0.7573 0.071 Uiso 1 1 calc R . .
C3 C 0.9301(8) 0.6993(3) 0.7876(4) 0.0636(17) Uani 1 1 d . . .
H3 H 0.9567 0.6518 0.8195 0.076 Uiso 1 1 calc R . .
C4 C 0.7954(7) 0.7344(3) 0.7773(3) 0.0483(14) Uani 1 1 d . . .
C5 C 0.6895(9) 0.6997(4) 0.8099(4) 0.075(2) Uani 1 1 d . . .
H5 H 0.7105 0.6511 0.8397 0.090 Uiso 1 1 calc R . .
C6 C 0.5611(8) 0.7351(4) 0.7987(4) 0.0725(19) Uani 1 1 d . . .
H6 H 0.4924 0.7096 0.8185 0.087 Uiso 1 1 calc R . .
C7 C 0.5261(6) 0.8117(4) 0.7570(4) 0.0519(14) Uani 1 1 d . . .
C8 C 0.3981(7) 0.8543(4) 0.7491(4) 0.0680(18) Uani 1 1 d . . .
H8 H 0.3291 0.8325 0.7714 0.082 Uiso 1 1 calc R . .
C9 C 0.3731(6) 0.9258(4) 0.7100(4) 0.0621(17) Uani 1 1 d . . .
H9 H 0.2883 0.9543 0.7056 0.075 Uiso 1 1 calc R . .
C10 C 0.4774(5) 0.9569(3) 0.6757(3) 0.0475(14) Uani 1 1 d . . .
H10 H 0.4583 1.0060 0.6470 0.057 Uiso 1 1 calc R . .
C11 C 0.6270(5) 0.8474(3) 0.7226(3) 0.0361(11) Uani 1 1 d . . .
C12 C 0.7622(5) 0.8076(3) 0.7317(3) 0.0341(11) Uani 1 1 d . . .
C13 C 0.4861(5) 0.8803(2) 0.4712(3) 0.0270(10) Uani 1 1 d . . .
C14 C 0.4631(5) 0.7966(3) 0.4936(3) 0.0308(11) Uani 1 1 d . . .
C15 C 0.5823(5) 0.7442(3) 0.5221(3) 0.0372(12) Uani 1 1 d . . .
H15 H 0.6765 0.7619 0.5276 0.045 Uiso 1 1 calc R . .
C16 C 0.3243(5) 0.7697(3) 0.4868(3) 0.0384(12) Uani 1 1 d . . .
H16 H 0.2439 0.8043 0.4689 0.046 Uiso 1 1 calc R . .
C17 C 0.3037(5) 0.6915(3) 0.5065(4) 0.0482(14) Uani 1 1 d . . .
H17 H 0.2098 0.6735 0.5010 0.058 Uiso 1 1 calc R . .
C18 C 0.5628(5) 0.6662(3) 0.5423(3) 0.0435(13) Uani 1 1 d . . .
H18 H 0.6428 0.6314 0.5609 0.052 Uiso 1 1 calc R . .
C19 C 1.4234(6) 0.8591(3) 1.0344(3) 0.0433(13) Uani 1 1 d . . .
C20 C 1.2530(6) 1.0363(3) 1.0696(4) 0.0486(13) Uani 1 1 d . . .
H20 H 1.3062 1.0390 1.1325 0.058 Uiso 1 1 calc R . .
C21 C 1.1348(6) 1.0871(3) 1.0290(4) 0.0508(14) Uani 1 1 d . . .
H21 H 1.1109 1.1254 1.0644 0.061 Uiso 1 1 calc R . .
C22 C 1.0534(5) 1.0815(3) 0.9375(3) 0.0435(12) Uani 1 1 d . . .
H22 H 0.9718 1.1145 0.9113 0.052 Uiso 1 1 calc R . .
C23 C 1.0910(5) 1.0275(3) 0.8835(3) 0.0358(11) Uani 1 1 d . . .
C24 C 0.9979(5) 1.0186(3) 0.7834(3) 0.0351(11) Uani 1 1 d . . .
C25 C 1.2122(5) 0.9782(3) 0.9227(3) 0.0374(11) Uani 1 1 d . . .
H25 H 1.2405 0.9427 0.8863 0.045 Uiso 1 1 calc R . .
C26 C 1.2909(5) 0.9820(3) 1.0164(3) 0.0405(12) Uani 1 1 d . . .
C27 C 0.9884(4) 1.0453(2) 0.5012(3) 0.0273(11) 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 O6 2.305(3) . ?
Eu1 O3 2.313(3) . ?
Eu1 O1 2.397(3) . ?
Eu1 O2 2.405(3) . ?
Eu1 O4 2.405(3) . ?
Eu1 O5 2.503(3) . ?
Eu1 N1 2.572(4) . ?
Eu1 N2 2.628(4) . ?
Eu1 C24 2.804(5) . ?
Eu1 C27 3.201(4) . ?
Eu1 C27 3.214(4) 3_776 ?
O1 C27 1.244(5) . ?
O2 C27 1.256(5) 3_776 ?
O3 C13 1.261(5) . ?
O4 C24 1.257(5) . ?
O5 C24 1.253(5) . ?
O6 C13 1.250(5) 3_676 ?
O7 C26 1.379(6) . ?
O7 C19 1.385(6) . ?
N1 C1 1.327(6) . ?
N1 C12 1.350(6) . ?
N2 C10 1.324(6) . ?
N2 C11 1.361(6) . ?
C1 C2 1.385(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.354(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.384(8) . ?
C3 H3 0.9300 . ?
C4 C12 1.404(6) . ?
C4 C5 1.419(8) . ?
C5 C6 1.329(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.432(8) . ?
C6 H6 0.9300 . ?
C7 C8 1.395(8) . ?
C7 C11 1.405(7) . ?
C8 C9 1.336(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.399(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.428(7) . ?
C13 O6 1.250(5) 3_676 ?
C13 C14 1.491(6) . ?
C14 C16 1.382(6) . ?
C14 C15 1.391(6) . ?
C15 C18 1.383(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.385(6) . ?
C16 H16 0.9300 . ?
C17 C19 1.376(7) 4_475 ?
C17 H17 0.9300 . ?
C18 C19 1.373(7) 4_475 ?
C18 H18 0.9300 . ?
C19 C18 1.373(7) 4_676 ?
C19 C17 1.376(7) 4_676 ?
C20 C26 1.372(7) . ?
C20 C21 1.385(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.364(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.375(6) . ?
C22 H22 0.9300 . ?
C23 C25 1.385(6) . ?
C23 C24 1.504(6) . ?
C25 C26 1.386(6) . ?
C25 H25 0.9300 . ?
C27 O2 1.256(5) 3_776 ?
C27 C27 1.548(8) 3_776 ?
C27 Eu1 3.214(4) 3_776 ?

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
O6 Eu1 O3 86.10(11) . . ?
O6 Eu1 O1 75.85(10) . . ?
O3 Eu1 O1 106.24(11) . . ?
O6 Eu1 O2 132.64(11) . . ?
O3 Eu1 O2 76.93(10) . . ?
O1 Eu1 O2 67.42(10) . . ?
O6 Eu1 O4 80.51(11) . . ?
O3 Eu1 O4 150.66(11) . . ?
O1 Eu1 O4 95.68(11) . . ?
O2 Eu1 O4 130.60(10) . . ?
O6 Eu1 O5 124.04(11) . . ?
O3 Eu1 O5 149.46(11) . . ?
O1 Eu1 O5 79.69(11) . . ?
O2 Eu1 O5 78.09(11) . . ?
O4 Eu1 O5 52.81(10) . . ?
O6 Eu1 N1 144.88(12) . . ?
O3 Eu1 N1 86.36(11) . . ?
O1 Eu1 N1 139.01(11) . . ?
O2 Eu1 N1 78.33(11) . . ?
O4 Eu1 N1 89.74(11) . . ?
O5 Eu1 N1 71.57(11) . . ?
O6 Eu1 N2 81.84(11) . . ?
O3 Eu1 N2 74.46(11) . . ?
O1 Eu1 N2 157.53(11) . . ?
O2 Eu1 N2 132.70(11) . . ?
O4 Eu1 N2 77.85(11) . . ?
O5 Eu1 N2 111.49(11) . . ?
N1 Eu1 N2 63.10(12) . . ?
O6 Eu1 C24 104.21(13) . . ?
O3 Eu1 C24 162.64(12) . . ?
O1 Eu1 C24 89.99(12) . . ?
O2 Eu1 C24 104.62(12) . . ?
O4 Eu1 C24 26.53(12) . . ?
O5 Eu1 C24 26.53(11) . . ?
N1 Eu1 C24 77.18(12) . . ?
N2 Eu1 C24 92.95(12) . . ?
O6 Eu1 C27 93.71(10) . . ?
O3 Eu1 C27 99.60(10) . . ?
O1 Eu1 C27 19.73(10) . . ?
O2 Eu1 C27 47.78(10) . . ?
O4 Eu1 C27 107.18(11) . . ?
O5 Eu1 C27 75.75(11) . . ?
N1 Eu1 C27 121.37(11) . . ?
N2 Eu1 C27 172.74(10) . . ?
C24 Eu1 C27 93.71(12) . . ?
O6 Eu1 C27 117.85(10) . 3_776 ?
O3 Eu1 C27 87.12(10) . 3_776 ?
O1 Eu1 C27 47.62(10) . 3_776 ?
O2 Eu1 C27 19.91(9) . 3_776 ?
O4 Eu1 C27 122.22(11) . 3_776 ?
O5 Eu1 C27 74.86(10) . 3_776 ?
N1 Eu1 C27 95.94(11) . 3_776 ?
N2 Eu1 C27 152.40(11) . 3_776 ?
C24 Eu1 C27 99.88(12) . 3_776 ?
C27 Eu1 C27 27.92(14) . 3_776 ?
C27 O1 Eu1 119.7(3) . . ?
C27 O2 Eu1 119.4(3) 3_776 . ?
C13 O3 Eu1 140.2(3) . . ?
C24 O4 Eu1 94.7(3) . . ?
C24 O5 Eu1 90.3(3) . . ?
C13 O6 Eu1 161.1(3) 3_676 . ?
C26 O7 C19 120.5(4) . . ?
C1 N1 C12 118.3(4) . . ?
C1 N1 Eu1 120.6(3) . . ?
C12 N1 Eu1 121.1(3) . . ?
C10 N2 C11 117.6(4) . . ?
C10 N2 Eu1 123.6(3) . . ?
C11 N2 Eu1 118.7(3) . . ?
N1 C1 C2 123.3(5) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C3 C2 C1 118.5(5) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 120.3(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C12 118.0(5) . . ?
C3 C4 C5 123.2(5) . . ?
C12 C4 C5 118.8(5) . . ?
C6 C5 C4 121.6(6) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C7 121.5(6) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C11 117.2(5) . . ?
C8 C7 C6 124.2(5) . . ?
C11 C7 C6 118.6(5) . . ?
C9 C8 C7 121.1(5) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 118.4(5) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 H9 120.8 . . ?
N2 C10 C9 123.5(5) . . ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
N2 C11 C7 122.1(5) . . ?
N2 C11 C12 118.4(4) . . ?
C7 C11 C12 119.5(5) . . ?
N1 C12 C4 121.5(5) . . ?
N1 C12 C11 118.6(4) . . ?
C4 C12 C11 119.9(5) . . ?
O6 C13 O3 123.1(4) 3_676 . ?
O6 C13 C14 118.4(4) 3_676 . ?
O3 C13 C14 118.5(4) . . ?
C16 C14 C15 118.8(4) . . ?
C16 C14 C13 121.1(4) . . ?
C15 C14 C13 120.1(4) . . ?
C18 C15 C14 120.9(4) . . ?
C18 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C14 C16 C17 120.6(4) . . ?
C14 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C19 C17 C16 119.4(5) 4_475 . ?
C19 C17 H17 120.3 4_475 . ?
C16 C17 H17 120.3 . . ?
C19 C18 C15 119.0(5) 4_475 . ?
C19 C18 H18 120.5 4_475 . ?
C15 C18 H18 120.5 . . ?
C18 C19 C17 121.2(5) 4_676 4_676 ?
C18 C19 O7 115.1(4) 4_676 . ?
C17 C19 O7 123.6(5) 4_676 . ?
C26 C20 C21 119.5(5) . . ?
C26 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C22 C21 C20 120.4(5) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 120.5(5) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C22 C23 C25 119.7(4) . . ?
C22 C23 C24 120.7(4) . . ?
C25 C23 C24 119.5(4) . . ?
O5 C24 O4 121.0(4) . . ?
O5 C24 C23 120.8(4) . . ?
O4 C24 C23 118.1(4) . . ?
O5 C24 Eu1 63.2(2) . . ?
O4 C24 Eu1 58.7(2) . . ?
C23 C24 Eu1 167.0(3) . . ?
C23 C25 C26 119.6(4) . . ?
C23 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C20 C26 O7 116.2(4) . . ?
C20 C26 C25 120.3(5) . . ?
O7 C26 C25 123.3(4) . . ?
O1 C27 O2 126.9(4) . 3_776 ?
O1 C27 C27 117.0(5) . 3_776 ?
O2 C27 C27 116.1(5) 3_776 3_776 ?
O1 C27 Eu1 40.6(2) . . ?
O2 C27 Eu1 167.0(3) 3_776 . ?
C27 C27 Eu1 76.5(3) 3_776 . ?
O1 C27 Eu1 167.2(3) . 3_776 ?
O2 C27 Eu1 40.7(2) 3_776 3_776 ?
C27 C27 Eu1 75.6(3) 3_776 3_776 ?
Eu1 C27 Eu1 152.08(14) . 3_776 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 Eu1 O1 C27 -154.3(3) . . . . ?
O3 Eu1 O1 C27 -72.7(3) . . . . ?
O2 Eu1 O1 C27 -4.8(3) . . . . ?
O4 Eu1 O1 C27 127.0(3) . . . . ?
O5 Eu1 O1 C27 76.5(3) . . . . ?
N1 Eu1 O1 C27 30.9(4) . . . . ?
N2 Eu1 O1 C27 -161.2(3) . . . . ?
C24 Eu1 O1 C27 101.1(3) . . . . ?
C27 Eu1 O1 C27 -2.4(3) 3_776 . . . ?
O6 Eu1 O2 C27 47.3(4) . . . 3_776 ?
O3 Eu1 O2 C27 119.3(3) . . . 3_776 ?
O1 Eu1 O2 C27 5.3(3) . . . 3_776 ?
O4 Eu1 O2 C27 -72.3(3) . . . 3_776 ?
O5 Eu1 O2 C27 -78.4(3) . . . 3_776 ?
N1 Eu1 O2 C27 -151.7(3) . . . 3_776 ?
N2 Eu1 O2 C27 173.3(3) . . . 3_776 ?
C24 Eu1 O2 C27 -78.5(3) . . . 3_776 ?
C27 Eu1 O2 C27 3.1(3) . . . 3_776 ?
O6 Eu1 O3 C13 -62.4(4) . . . . ?
O1 Eu1 O3 C13 -136.4(4) . . . . ?
O2 Eu1 O3 C13 162.2(5) . . . . ?
O4 Eu1 O3 C13 0.3(6) . . . . ?
O5 Eu1 O3 C13 126.3(4) . . . . ?
N1 Eu1 O3 C13 83.3(4) . . . . ?
N2 Eu1 O3 C13 20.2(4) . . . . ?
C24 Eu1 O3 C13 64.9(6) . . . . ?
C27 Eu1 O3 C13 -155.5(4) . . . . ?
C27 Eu1 O3 C13 179.4(4) 3_776 . . . ?
O6 Eu1 O4 C24 -153.1(3) . . . . ?
O3 Eu1 O4 C24 142.9(3) . . . . ?
O1 Eu1 O4 C24 -78.5(3) . . . . ?
O2 Eu1 O4 C24 -13.5(3) . . . . ?
O5 Eu1 O4 C24 -6.0(3) . . . . ?
N1 Eu1 O4 C24 60.8(3) . . . . ?
N2 Eu1 O4 C24 123.3(3) . . . . ?
C27 Eu1 O4 C24 -62.1(3) . . . . ?
C27 Eu1 O4 C24 -36.1(3) 3_776 . . . ?
O6 Eu1 O5 C24 46.4(3) . . . . ?
O3 Eu1 O5 C24 -144.1(3) . . . . ?
O1 Eu1 O5 C24 111.4(3) . . . . ?
O2 Eu1 O5 C24 -179.8(3) . . . . ?
O4 Eu1 O5 C24 6.0(3) . . . . ?
N1 Eu1 O5 C24 -98.3(3) . . . . ?
N2 Eu1 O5 C24 -48.3(3) . . . . ?
C27 Eu1 O5 C24 131.2(3) . . . . ?
C27 Eu1 O5 C24 160.0(3) 3_776 . . . ?
O3 Eu1 O6 C13 -7.4(9) . . . 3_676 ?
O1 Eu1 O6 C13 100.5(9) . . . 3_676 ?
O2 Eu1 O6 C13 60.9(9) . . . 3_676 ?
O4 Eu1 O6 C13 -161.2(9) . . . 3_676 ?
O5 Eu1 O6 C13 167.3(9) . . . 3_676 ?
N1 Eu1 O6 C13 -85.4(9) . . . 3_676 ?
N2 Eu1 O6 C13 -82.2(9) . . . 3_676 ?
C24 Eu1 O6 C13 -173.2(9) . . . 3_676 ?
C27 Eu1 O6 C13 92.0(9) . . . 3_676 ?
C27 Eu1 O6 C13 77.3(9) 3_776 . . 3_676 ?
O6 Eu1 N1 C1 -174.7(3) . . . . ?
O3 Eu1 N1 C1 107.3(4) . . . . ?
O1 Eu1 N1 C1 -3.4(5) . . . . ?
O2 Eu1 N1 C1 29.9(4) . . . . ?
O4 Eu1 N1 C1 -101.8(4) . . . . ?
O5 Eu1 N1 C1 -51.2(4) . . . . ?
N2 Eu1 N1 C1 -178.2(4) . . . . ?
C24 Eu1 N1 C1 -78.2(4) . . . . ?
C27 Eu1 N1 C1 8.3(4) . . . . ?
C27 Eu1 N1 C1 20.6(4) 3_776 . . . ?
O6 Eu1 N1 C12 6.1(4) . . . . ?
O3 Eu1 N1 C12 -71.8(3) . . . . ?
O1 Eu1 N1 C12 177.5(3) . . . . ?
O2 Eu1 N1 C12 -149.2(3) . . . . ?
O4 Eu1 N1 C12 79.1(3) . . . . ?
O5 Eu1 N1 C12 129.6(3) . . . . ?
N2 Eu1 N1 C12 2.6(3) . . . . ?
C24 Eu1 N1 C12 102.7(3) . . . . ?
C27 Eu1 N1 C12 -170.8(3) . . . . ?
C27 Eu1 N1 C12 -158.5(3) 3_776 . . . ?
O6 Eu1 N2 C10 2.2(4) . . . . ?
O3 Eu1 N2 C10 -85.9(4) . . . . ?
O1 Eu1 N2 C10 9.1(5) . . . . ?
O2 Eu1 N2 C10 -140.8(4) . . . . ?
O4 Eu1 N2 C10 84.2(4) . . . . ?
O5 Eu1 N2 C10 125.7(4) . . . . ?
N1 Eu1 N2 C10 -179.8(4) . . . . ?
C24 Eu1 N2 C10 106.2(4) . . . . ?
C27 Eu1 N2 C10 -50.3(10) . . . . ?
C27 Eu1 N2 C10 -135.8(4) 3_776 . . . ?
O6 Eu1 N2 C11 178.0(3) . . . . ?
O3 Eu1 N2 C11 89.8(3) . . . . ?
O1 Eu1 N2 C11 -175.2(3) . . . . ?
O2 Eu1 N2 C11 35.0(4) . . . . ?
O4 Eu1 N2 C11 -100.0(3) . . . . ?
O5 Eu1 N2 C11 -58.6(3) . . . . ?
N1 Eu1 N2 C11 -4.1(3) . . . . ?
C24 Eu1 N2 C11 -78.1(3) . . . . ?
C27 Eu1 N2 C11 125.4(8) . . . . ?
C27 Eu1 N2 C11 39.9(4) 3_776 . . . ?
C12 N1 C1 C2 -1.8(8) . . . . ?
Eu1 N1 C1 C2 179.0(4) . . . . ?
N1 C1 C2 C3 1.4(9) . . . . ?
C1 C2 C3 C4 0.8(9) . . . . ?
C2 C3 C4 C12 -2.4(8) . . . . ?
C2 C3 C4 C5 177.1(6) . . . . ?
C3 C4 C5 C6 -179.9(6) . . . . ?
C12 C4 C5 C6 -0.5(9) . . . . ?
C4 C5 C6 C7 -2.9(11) . . . . ?
C5 C6 C7 C8 -175.4(6) . . . . ?
C5 C6 C7 C11 3.8(9) . . . . ?
C11 C7 C8 C9 0.3(9) . . . . ?
C6 C7 C8 C9 179.4(6) . . . . ?
C7 C8 C9 C10 0.9(9) . . . . ?
C11 N2 C10 C9 1.3(7) . . . . ?
Eu1 N2 C10 C9 177.1(4) . . . . ?
C8 C9 C10 N2 -1.8(9) . . . . ?
C10 N2 C11 C7 0.0(7) . . . . ?
Eu1 N2 C11 C7 -176.0(3) . . . . ?
C10 N2 C11 C12 -178.7(4) . . . . ?
Eu1 N2 C11 C12 5.3(5) . . . . ?
C8 C7 C11 N2 -0.8(7) . . . . ?
C6 C7 C11 N2 -180.0(5) . . . . ?
C8 C7 C11 C12 177.9(5) . . . . ?
C6 C7 C11 C12 -1.3(7) . . . . ?
C1 N1 C12 C4 0.1(7) . . . . ?
Eu1 N1 C12 C4 179.2(3) . . . . ?
C1 N1 C12 C11 179.7(4) . . . . ?
Eu1 N1 C12 C11 -1.1(5) . . . . ?
C3 C4 C12 N1 2.0(7) . . . . ?
C5 C4 C12 N1 -177.5(5) . . . . ?
C3 C4 C12 C11 -177.6(5) . . . . ?
C5 C4 C12 C11 2.9(7) . . . . ?
N2 C11 C12 N1 -2.9(6) . . . . ?
C7 C11 C12 N1 178.4(4) . . . . ?
N2 C11 C12 C4 176.8(4) . . . . ?
C7 C11 C12 C4 -1.9(7) . . . . ?
Eu1 O3 C13 O6 86.3(6) . . . 3_676 ?
Eu1 O3 C13 C14 -95.7(5) . . . . ?
O6 C13 C14 C16 -14.5(6) 3_676 . . . ?
O3 C13 C14 C16 167.4(4) . . . . ?
O6 C13 C14 C15 165.7(4) 3_676 . . . ?
O3 C13 C14 C15 -12.4(6) . . . . ?
C16 C14 C15 C18 0.8(7) . . . . ?
C13 C14 C15 C18 -179.3(4) . . . . ?
C15 C14 C16 C17 -1.1(7) . . . . ?
C13 C14 C16 C17 179.0(4) . . . . ?
C14 C16 C17 C19 1.0(8) . . . 4_475 ?
C14 C15 C18 C19 -0.4(7) . . . 4_475 ?
C26 O7 C19 C18 146.5(5) . . . 4_676 ?
C26 O7 C19 C17 -36.4(8) . . . 4_676 ?
C26 C20 C21 C22 2.3(8) . . . . ?
C20 C21 C22 C23 -2.6(8) . . . . ?
C21 C22 C23 C25 0.3(7) . . . . ?
C21 C22 C23 C24 177.4(5) . . . . ?
Eu1 O5 C24 O4 -10.8(4) . . . . ?
Eu1 O5 C24 C23 165.8(4) . . . . ?
Eu1 O4 C24 O5 11.3(5) . . . . ?
Eu1 O4 C24 C23 -165.4(4) . . . . ?
C22 C23 C24 O5 162.8(4) . . . . ?
C25 C23 C24 O5 -20.1(7) . . . . ?
C22 C23 C24 O4 -20.5(7) . . . . ?
C25 C23 C24 O4 156.6(4) . . . . ?
C22 C23 C24 Eu1 -92.8(15) . . . . ?
C25 C23 C24 Eu1 84.3(15) . . . . ?
O6 Eu1 C24 O5 -141.8(3) . . . . ?
O3 Eu1 C24 O5 93.2(5) . . . . ?
O1 Eu1 C24 O5 -66.4(3) . . . . ?
O2 Eu1 C24 O5 0.2(3) . . . . ?
O4 Eu1 C24 O5 -169.2(4) . . . . ?
N1 Eu1 C24 O5 74.3(3) . . . . ?
N2 Eu1 C24 O5 135.9(3) . . . . ?
C27 Eu1 C24 O5 -47.0(3) . . . . ?
C27 Eu1 C24 O5 -19.6(3) 3_776 . . . ?
O6 Eu1 C24 O4 27.4(3) . . . . ?
O3 Eu1 C24 O4 -97.7(5) . . . . ?
O1 Eu1 C24 O4 102.8(3) . . . . ?
O2 Eu1 C24 O4 169.4(3) . . . . ?
O5 Eu1 C24 O4 169.2(4) . . . . ?
N1 Eu1 C24 O4 -116.5(3) . . . . ?
N2 Eu1 C24 O4 -54.9(3) . . . . ?
C27 Eu1 C24 O4 122.2(3) . . . . ?
C27 Eu1 C24 O4 149.6(3) 3_776 . . . ?
O6 Eu1 C24 C23 107.0(15) . . . . ?
O3 Eu1 C24 C23 -18.1(18) . . . . ?
O1 Eu1 C24 C23 -177.7(15) . . . . ?
O2 Eu1 C24 C23 -111.0(15) . . . . ?
O4 Eu1 C24 C23 79.5(15) . . . . ?
O5 Eu1 C24 C23 -111.3(16) . . . . ?
N1 Eu1 C24 C23 -36.9(15) . . . . ?
N2 Eu1 C24 C23 24.6(15) . . . . ?
C27 Eu1 C24 C23 -158.3(15) . . . . ?
C27 Eu1 C24 C23 -130.8(15) 3_776 . . . ?
C22 C23 C25 C26 2.3(7) . . . . ?
C24 C23 C25 C26 -174.9(4) . . . . ?
C21 C20 C26 O7 175.9(5) . . . . ?
C21 C20 C26 C25 0.3(8) . . . . ?
C19 O7 C26 C20 146.2(5) . . . . ?
C19 O7 C26 C25 -38.4(7) . . . . ?
C23 C25 C26 C20 -2.6(7) . . . . ?
C23 C25 C26 O7 -177.9(4) . . . . ?
Eu1 O1 C27 O2 -175.0(3) . . . 3_776 ?
Eu1 O1 C27 C27 4.1(6) . . . 3_776 ?
Eu1 O1 C27 Eu1 172.1(11) . . . 3_776 ?
O6 Eu1 C27 O1 25.0(3) . . . . ?
O3 Eu1 C27 O1 111.6(3) . . . . ?
O2 Eu1 C27 O1 174.0(4) . . . . ?
O4 Eu1 C27 O1 -56.2(3) . . . . ?
O5 Eu1 C27 O1 -99.3(3) . . . . ?
N1 Eu1 C27 O1 -156.8(3) . . . . ?
N2 Eu1 C27 O1 76.9(9) . . . . ?
C24 Eu1 C27 O1 -79.6(3) . . . . ?
C27 Eu1 C27 O1 176.3(5) 3_776 . . . ?
O6 Eu1 C27 O2 43.0(13) . . . 3_776 ?
O3 Eu1 C27 O2 129.7(13) . . . 3_776 ?
O1 Eu1 C27 O2 18.1(11) . . . 3_776 ?
O2 Eu1 C27 O2 -167.9(13) . . . 3_776 ?
O4 Eu1 C27 O2 -38.2(13) . . . 3_776 ?
O5 Eu1 C27 O2 -81.2(13) . . . 3_776 ?
N1 Eu1 C27 O2 -138.7(13) . . . 3_776 ?
N2 Eu1 C27 O2 95.0(15) . . . 3_776 ?
C24 Eu1 C27 O2 -61.5(13) . . . 3_776 ?
C27 Eu1 C27 O2 -165.7(15) 3_776 . . 3_776 ?
O6 Eu1 C27 C27 -151.3(3) . . . 3_776 ?
O3 Eu1 C27 C27 -64.7(3) . . . 3_776 ?
O1 Eu1 C27 C27 -176.3(5) . . . 3_776 ?
O2 Eu1 C27 C27 -2.3(2) . . . 3_776 ?
O4 Eu1 C27 C27 127.5(3) . . . 3_776 ?
O5 Eu1 C27 C27 84.5(3) . . . 3_776 ?
N1 Eu1 C27 C27 26.9(3) . . . 3_776 ?
N2 Eu1 C27 C27 -99.4(9) . . . 3_776 ?
C24 Eu1 C27 C27 104.2(3) . . . 3_776 ?
O6 Eu1 C27 Eu1 -151.3(3) . . . 3_776 ?
O3 Eu1 C27 Eu1 -64.7(3) . . . 3_776 ?
O1 Eu1 C27 Eu1 -176.3(5) . . . 3_776 ?
O2 Eu1 C27 Eu1 -2.3(2) . . . 3_776 ?
O4 Eu1 C27 Eu1 127.5(3) . . . 3_776 ?
O5 Eu1 C27 Eu1 84.5(3) . . . 3_776 ?
N1 Eu1 C27 Eu1 26.9(3) . . . 3_776 ?
N2 Eu1 C27 Eu1 -99.4(9) . . . 3_776 ?
C24 Eu1 C27 Eu1 104.2(3) . . . 3_776 ?
C27 Eu1 C27 Eu1 0.0 3_776 . . 3_776 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.099

####################################################################### 
# 
# 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_aaa
_database_code_depnum_ccdc_archive 'CCDC 1414237'
_audit_update_record             
;
2017-10-23 deposited with the CCDC.
2017-12-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H16 N2 O7 Sm'
_chemical_formula_weight         630.77

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           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                   9.6600(19)
_cell_length_b                   16.880(3)
_cell_length_c                   15.120(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.77(3)
_cell_angle_gamma                90.00
_cell_volume                     2372.7(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.131
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240
_exptl_absorpt_coefficient_mu    2.527
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.5629
_exptl_absorpt_correction_T_max  0.7331
_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  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37270
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4167
_reflns_number_gt                3535
_reflns_threshold_expression     >2sigma(I)

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

_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)+(0.0341P)²+2.0316P] 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         4167
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0260
_refine_ls_wR_factor_ref         0.0638
_refine_ls_wR_factor_gt          0.0598
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.179880(17) 0.024676(10) 0.888188(12) 0.02509(8) Uani 1 1 d . . .
O1 O 0.3179(3) 0.01560(16) 0.76997(19) 0.0408(7) Uani 1 1 d . . .
N2 N -0.0818(3) 0.08075(19) 0.8180(2) 0.0320(7) Uani 1 1 d . . .
O3 O 0.4050(3) 0.08746(14) 0.96555(18) 0.0370(6) Uani 1 1 d . . .
C4 C 0.2135(4) -0.0184(2) 0.7154(3) 0.0332(9) Uani 1 1 d . . .
O5 O 0.3629(2) -0.06898(14) 0.96174(18) 0.0369(6) Uani 1 1 d . . .
O6 O 0.1228(3) 0.09484(14) 1.00619(17) 0.0336(6) Uani 1 1 d . . .
N7 N 0.1578(3) 0.15880(18) 0.8031(2) 0.0365(7) Uani 1 1 d . . .
C8 C 0.0153(4) 0.1198(2) 1.0299(2) 0.0279(8) Uani 1 1 d . . .
C9 C -0.0297(4) 0.2038(2) 1.0066(2) 0.0303(8) Uani 1 1 d . . .
C10 C 0.2068(4) -0.0276(2) 0.6154(3) 0.0346(9) Uani 1 1 d . . .
C11 C 0.2894(4) 0.0217(2) 0.5765(3) 0.0380(9) Uani 1 1 d . . .
H11 H 0.3544 0.0570 0.6129 0.046 Uiso 1 1 calc R . .
O12 O 0.0526(3) -0.07928(15) 0.92756(18) 0.0394(6) Uani 1 1 d . . .
O13 O 0.3548(4) 0.06250(17) 0.4394(2) 0.0597(9) Uani 1 1 d . . .
C14 C 0.2739(5) 0.0177(2) 0.4835(3) 0.0402(10) Uani 1 1 d . . .
C15 C 0.0605(4) 0.2562(2) 0.9776(3) 0.0382(9) Uani 1 1 d . . .
H15 H 0.1488 0.2384 0.9719 0.046 Uiso 1 1 calc R . .
O16 O 0.1089(3) -0.04319(17) 0.74262(19) 0.0447(7) Uani 1 1 d . . .
C17 C -0.1997(4) 0.0440(3) 0.8244(3) 0.0466(11) Uani 1 1 d . . .
H17 H -0.1897 -0.0053 0.8529 0.056 Uiso 1 1 calc R . .
C18 C 0.0283(4) 0.1935(2) 0.7681(2) 0.0349(9) Uani 1 1 d . . .
C19 C 0.1157(4) -0.0816(2) 0.5615(3) 0.0420(10) Uani 1 1 d . . .
H19 H 0.0602 -0.1146 0.5874 0.050 Uiso 1 1 calc R . .
C20 C -0.2402(6) 0.2659(3) 0.7029(4) 0.0719(16) Uani 1 1 d . . .
H20 H -0.3285 0.2916 0.6840 0.086 Uiso 1 1 calc R . .
C21 C 0.5124(4) 0.0456(2) 1.0009(2) 0.0300(9) Uani 1 1 d . . .
C22 C 0.0204(5) 0.3341(2) 0.9573(3) 0.0425(10) Uani 1 1 d . . .
H22 H 0.0815 0.3687 0.9382 0.051 Uiso 1 1 calc R . .
C23 C 0.1828(5) -0.0373(2) 0.4297(3) 0.0473(11) Uani 1 1 d . . .
H23 H 0.1739 -0.0403 0.3669 0.057 Uiso 1 1 calc R . .
C24 C -0.0976(4) 0.1534(2) 0.7778(2) 0.0357(9) Uani 1 1 d . . .
C25 C 0.1401(6) 0.3022(3) 0.7127(3) 0.0623(14) Uani 1 1 d . . .
H25 H 0.1347 0.3502 0.6817 0.075 Uiso 1 1 calc R . .
C28 C 0.0159(5) 0.2669(2) 0.7226(3) 0.0503(11) Uani 1 1 d . . .
C29 C 0.2689(6) 0.2675(3) 0.7479(3) 0.0589(13) Uani 1 1 d . . .
H29 H 0.3528 0.2910 0.7417 0.071 Uiso 1 1 calc R . .
C30 C 0.3900(5) 0.1401(2) 0.4655(3) 0.0423(10) Uani 1 1 d . . .
C31 C 0.2737(5) 0.1959(3) 0.7935(3) 0.0500(11) Uani 1 1 d . . .
H31 H 0.3631 0.1726 0.8187 0.060 Uiso 1 1 calc R . .
C33 C 0.1058(5) -0.0873(3) 0.4696(3) 0.0499(11) Uani 1 1 d . . .
H33 H 0.0464 -0.1255 0.4341 0.060 Uiso 1 1 calc R . .
C34 C -0.1627(4) 0.2305(2) 1.0135(3) 0.0377(9) Uani 1 1 d . . .
H34 H -0.2244 0.1959 1.0320 0.045 Uiso 1 1 calc R . .
C35 C -0.2332(5) 0.1894(3) 0.7441(3) 0.0506(11) Uani 1 1 d . . .
C41 C 0.2966(5) 0.1914(2) 0.4929(3) 0.0467(11) Uani 1 1 d . . .
H41 H 0.2078 0.1735 0.4974 0.056 Uiso 1 1 calc R . .
C1 C -0.3369(4) 0.0746(3) 0.7913(3) 0.0603(13) Uani 1 1 d . . .
H1 H -0.4167 0.0459 0.7962 0.072 Uiso 1 1 calc R . .
C3 C -0.3525(5) 0.1464(4) 0.7518(3) 0.0675(15) Uani 1 1 d . . .
H3 H -0.4441 0.1677 0.7293 0.081 Uiso 1 1 calc R . .
C5 C -0.1230(7) 0.3018(3) 0.6906(4) 0.0745(16) Uani 1 1 d . . .
H5 H -0.1326 0.3505 0.6607 0.089 Uiso 1 1 calc 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 O12 2.311(2) . ?
Sm1 O6 2.329(2) . ?
Sm1 O5 2.407(2) . ?
Sm1 O16 2.410(3) . ?
Sm1 O3 2.416(2) . ?
Sm1 O1 2.508(3) . ?
Sm1 N7 2.584(3) . ?
Sm1 N2 2.637(3) . ?
Sm1 C4 2.814(4) . ?
O1 C4 1.255(5) . ?
N2 C17 1.323(5) . ?
N2 C24 1.358(5) . ?
O3 C21 1.249(4) . ?
C4 O16 1.261(4) . ?
C4 C10 1.504(5) . ?
O5 C21 1.248(4) 3_657 ?
O6 C8 1.260(4) . ?
N7 C31 1.325(5) . ?
N7 C18 1.352(5) . ?
C8 O12 1.242(4) 3_557 ?
C8 C9 1.497(5) . ?
C9 C34 1.391(5) . ?
C9 C15 1.392(5) . ?
C10 C19 1.372(5) . ?
C10 C11 1.390(5) . ?
C11 C14 1.374(6) . ?
O12 C8 1.242(4) 3_557 ?
O13 C14 1.383(5) . ?
O13 C30 1.383(5) . ?
C14 C23 1.382(6) . ?
C15 C22 1.382(5) . ?
C17 C1 1.383(6) . ?
C18 C28 1.407(6) . ?
C18 C24 1.434(5) . ?
C19 C33 1.369(5) . ?
C20 C5 1.341(7) . ?
C20 C35 1.427(7) . ?
C21 O5 1.248(4) 3_657 ?
C21 C21 1.557(7) 3_657 ?
C22 C30 1.370(6) 4_566 ?
C23 C33 1.370(6) . ?
C24 C35 1.408(5) . ?
C25 C29 1.348(7) . ?
C25 C28 1.384(7) . ?
C28 C5 1.424(7) . ?
C29 C31 1.386(6) . ?
C30 C22 1.370(6) 4_665 ?
C30 C41 1.393(5) . ?
C34 C41 1.386(6) 4_566 ?
C35 C3 1.393(7) . ?
C41 C34 1.386(6) 4_665 ?
C1 C3 1.342(7) . ?

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
O12 Sm1 O6 86.31(9) . . ?
O12 Sm1 O5 75.97(9) . . ?
O6 Sm1 O5 106.08(9) . . ?
O12 Sm1 O16 80.51(9) . . ?
O6 Sm1 O16 150.88(9) . . ?
O5 Sm1 O16 95.78(10) . . ?
O12 Sm1 O3 132.84(9) . . ?
O6 Sm1 O3 77.01(9) . . ?
O5 Sm1 O3 67.24(8) . . ?
O16 Sm1 O3 130.24(9) . . ?
O12 Sm1 O1 124.06(9) . . ?
O6 Sm1 O1 149.23(9) . . ?
O5 Sm1 O1 79.82(9) . . ?
O16 Sm1 O1 52.73(9) . . ?
O3 Sm1 O1 77.82(9) . . ?
O12 Sm1 N7 144.65(10) . . ?
O6 Sm1 N7 86.05(9) . . ?
O5 Sm1 N7 139.16(9) . . ?
O16 Sm1 N7 89.84(10) . . ?
O3 Sm1 N7 78.37(10) . . ?
O1 Sm1 N7 71.74(9) . . ?
O12 Sm1 N2 81.80(9) . . ?
O6 Sm1 N2 74.06(9) . . ?
O5 Sm1 N2 157.68(9) . . ?
O16 Sm1 N2 78.42(10) . . ?
O3 Sm1 N2 132.50(9) . . ?
O1 Sm1 N2 111.84(9) . . ?
N7 Sm1 N2 62.91(10) . . ?
O12 Sm1 C4 104.26(10) . . ?
O6 Sm1 C4 162.48(10) . . ?
O5 Sm1 C4 90.21(10) . . ?
O16 Sm1 C4 26.51(10) . . ?
O3 Sm1 C4 104.31(10) . . ?
O1 Sm1 C4 26.49(10) . . ?
N7 Sm1 C4 77.24(10) . . ?
N2 Sm1 C4 93.38(10) . . ?
C4 O1 Sm1 90.5(2) . . ?
C17 N2 C24 117.5(3) . . ?
C17 N2 Sm1 123.5(3) . . ?
C24 N2 Sm1 118.9(2) . . ?
C21 O3 Sm1 119.5(2) . . ?
O1 C4 O16 120.6(4) . . ?
O1 C4 C10 121.0(3) . . ?
O16 C4 C10 118.3(3) . . ?
O1 C4 Sm1 63.0(2) . . ?
O16 C4 Sm1 58.6(2) . . ?
C10 C4 Sm1 167.4(3) . . ?
C21 O5 Sm1 120.0(2) 3_657 . ?
C8 O6 Sm1 140.6(2) . . ?
C31 N7 C18 118.2(3) . . ?
C31 N7 Sm1 120.7(3) . . ?
C18 N7 Sm1 121.1(2) . . ?
O12 C8 O6 123.7(3) 3_557 . ?
O12 C8 C9 118.9(3) 3_557 . ?
O6 C8 C9 117.3(3) . . ?
C34 C9 C15 119.2(3) . . ?
C34 C9 C8 120.2(3) . . ?
C15 C9 C8 120.6(3) . . ?
C19 C10 C11 119.7(4) . . ?
C19 C10 C4 120.8(3) . . ?
C11 C10 C4 119.4(3) . . ?
C14 C11 C10 119.2(4) . . ?
C8 O12 Sm1 160.9(2) 3_557 . ?
C14 O13 C30 120.5(3) . . ?
C11 C14 C23 120.7(4) . . ?
C11 C14 O13 123.3(4) . . ?
C23 C14 O13 115.8(4) . . ?
C22 C15 C9 120.8(4) . . ?
C4 O16 Sm1 94.9(2) . . ?
N2 C17 C1 123.9(4) . . ?
N7 C18 C28 121.3(4) . . ?
N7 C18 C24 118.4(3) . . ?
C28 C18 C24 120.3(4) . . ?
C33 C19 C10 120.5(4) . . ?
C5 C20 C35 121.9(5) . . ?
O5 C21 O3 127.1(3) 3_657 . ?
O5 C21 C21 116.4(4) 3_657 3_657 ?
O3 C21 C21 116.5(4) . 3_657 ?
C30 C22 C15 119.5(4) 4_566 . ?
C33 C23 C14 119.3(4) . . ?
N2 C24 C35 122.2(4) . . ?
N2 C24 C18 118.5(3) . . ?
C35 C24 C18 119.4(4) . . ?
C29 C25 C28 120.3(4) . . ?
C25 C28 C18 118.1(4) . . ?
C25 C28 C5 123.4(4) . . ?
C18 C28 C5 118.5(4) . . ?
C25 C29 C31 118.6(5) . . ?
C22 C30 O13 115.9(4) 4_665 . ?
C22 C30 C41 120.9(4) 4_665 . ?
O13 C30 C41 123.0(4) . . ?
N7 C31 C29 123.4(4) . . ?
C19 C33 C23 120.5(4) . . ?
C41 C34 C9 120.1(4) 4_566 . ?
C3 C35 C24 117.0(4) . . ?
C3 C35 C20 124.5(4) . . ?
C24 C35 C20 118.5(4) . . ?
C34 C41 C30 119.4(4) 4_665 . ?
C3 C1 C17 118.6(4) . . ?
C1 C3 C35 120.8(4) . . ?
C20 C5 C28 121.3(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12 Sm1 O1 C4 46.4(2) . . . . ?
O6 Sm1 O1 C4 -144.0(2) . . . . ?
O5 Sm1 O1 C4 111.6(2) . . . . ?
O16 Sm1 O1 C4 6.2(2) . . . . ?
O3 Sm1 O1 C4 -179.7(2) . . . . ?
N7 Sm1 O1 C4 -98.1(2) . . . . ?
N2 Sm1 O1 C4 -48.5(2) . . . . ?
O12 Sm1 N2 C17 2.3(3) . . . . ?
O6 Sm1 N2 C17 -86.1(3) . . . . ?
O5 Sm1 N2 C17 7.5(5) . . . . ?
O16 Sm1 N2 C17 84.3(3) . . . . ?
O3 Sm1 N2 C17 -140.8(3) . . . . ?
O1 Sm1 N2 C17 125.8(3) . . . . ?
N7 Sm1 N2 C17 -179.9(3) . . . . ?
C4 Sm1 N2 C17 106.3(3) . . . . ?
O12 Sm1 N2 C24 178.2(3) . . . . ?
O6 Sm1 N2 C24 89.7(3) . . . . ?
O5 Sm1 N2 C24 -176.7(2) . . . . ?
O16 Sm1 N2 C24 -99.9(3) . . . . ?
O3 Sm1 N2 C24 35.1(3) . . . . ?
O1 Sm1 N2 C24 -58.3(3) . . . . ?
N7 Sm1 N2 C24 -4.1(2) . . . . ?
C4 Sm1 N2 C24 -77.9(3) . . . . ?
O12 Sm1 O3 C21 46.8(3) . . . . ?
O6 Sm1 O3 C21 119.1(3) . . . . ?
O5 Sm1 O3 C21 5.2(3) . . . . ?
O16 Sm1 O3 C21 -72.5(3) . . . . ?
O1 Sm1 O3 C21 -78.7(3) . . . . ?
N7 Sm1 O3 C21 -152.3(3) . . . . ?
N2 Sm1 O3 C21 172.7(2) . . . . ?
C4 Sm1 O3 C21 -78.9(3) . . . . ?
Sm1 O1 C4 O16 -11.1(4) . . . . ?
Sm1 O1 C4 C10 166.3(3) . . . . ?
O12 Sm1 C4 O1 -141.8(2) . . . . ?
O6 Sm1 C4 O1 92.5(4) . . . . ?
O5 Sm1 C4 O1 -66.2(2) . . . . ?
O16 Sm1 C4 O1 -168.8(4) . . . . ?
O3 Sm1 C4 O1 0.3(2) . . . . ?
N7 Sm1 C4 O1 74.6(2) . . . . ?
N2 Sm1 C4 O1 135.8(2) . . . . ?
O12 Sm1 C4 O16 27.1(2) . . . . ?
O6 Sm1 C4 O16 -98.7(4) . . . . ?
O5 Sm1 C4 O16 102.6(2) . . . . ?
O3 Sm1 C4 O16 169.1(2) . . . . ?
O1 Sm1 C4 O16 168.8(4) . . . . ?
N7 Sm1 C4 O16 -116.6(2) . . . . ?
N2 Sm1 C4 O16 -55.3(2) . . . . ?
O12 Sm1 C4 C10 106.4(12) . . . . ?
O6 Sm1 C4 C10 -19.4(14) . . . . ?
O5 Sm1 C4 C10 -178.1(12) . . . . ?
O16 Sm1 C4 C10 79.3(12) . . . . ?
O3 Sm1 C4 C10 -111.5(12) . . . . ?
O1 Sm1 C4 C10 -111.8(13) . . . . ?
N7 Sm1 C4 C10 -37.3(12) . . . . ?
N2 Sm1 C4 C10 24.0(12) . . . . ?
O12 Sm1 O5 C21 -154.7(3) . . . 3_657 ?
O6 Sm1 O5 C21 -72.9(3) . . . 3_657 ?
O16 Sm1 O5 C21 126.6(3) . . . 3_657 ?
O3 Sm1 O5 C21 -4.9(2) . . . 3_657 ?
O1 Sm1 O5 C21 76.1(3) . . . 3_657 ?
N7 Sm1 O5 C21 30.1(3) . . . 3_657 ?
N2 Sm1 O5 C21 -160.0(3) . . . 3_657 ?
C4 Sm1 O5 C21 100.6(3) . . . 3_657 ?
O12 Sm1 O6 C8 -61.0(4) . . . . ?
O5 Sm1 O6 C8 -135.3(4) . . . . ?
O16 Sm1 O6 C8 1.9(5) . . . . ?
O3 Sm1 O6 C8 163.4(4) . . . . ?
O1 Sm1 O6 C8 127.5(4) . . . . ?
N7 Sm1 O6 C8 84.4(4) . . . . ?
N2 Sm1 O6 C8 21.5(4) . . . . ?
C4 Sm1 O6 C8 66.9(5) . . . . ?
O12 Sm1 N7 C31 -174.3(3) . . . . ?
O6 Sm1 N7 C31 107.8(3) . . . . ?
O5 Sm1 N7 C31 -2.4(4) . . . . ?
O16 Sm1 N7 C31 -101.1(3) . . . . ?
O3 Sm1 N7 C31 30.3(3) . . . . ?
O1 Sm1 N7 C31 -50.6(3) . . . . ?
N2 Sm1 N7 C31 -178.1(3) . . . . ?
C4 Sm1 N7 C31 -77.5(3) . . . . ?
O12 Sm1 N7 C18 6.5(4) . . . . ?
O6 Sm1 N7 C18 -71.5(3) . . . . ?
O5 Sm1 N7 C18 178.4(2) . . . . ?
O16 Sm1 N7 C18 79.7(3) . . . . ?
O3 Sm1 N7 C18 -149.0(3) . . . . ?
O1 Sm1 N7 C18 130.1(3) . . . . ?
N2 Sm1 N7 C18 2.6(3) . . . . ?
C4 Sm1 N7 C18 103.2(3) . . . . ?
Sm1 O6 C8 O12 85.2(5) . . . 3_557 ?
Sm1 O6 C8 C9 -96.2(4) . . . . ?
O12 C8 C9 C34 -14.4(5) 3_557 . . . ?
O6 C8 C9 C34 166.9(3) . . . . ?
O12 C8 C9 C15 165.8(3) 3_557 . . . ?
O6 C8 C9 C15 -12.9(5) . . . . ?
O1 C4 C10 C19 162.6(4) . . . . ?
O16 C4 C10 C19 -20.0(5) . . . . ?
Sm1 C4 C10 C19 -92.2(12) . . . . ?
O1 C4 C10 C11 -20.3(5) . . . . ?
O16 C4 C10 C11 157.1(4) . . . . ?
Sm1 C4 C10 C11 84.9(13) . . . . ?
C19 C10 C11 C14 2.6(6) . . . . ?
C4 C10 C11 C14 -174.5(4) . . . . ?
O6 Sm1 O12 C8 -8.1(7) . . . 3_557 ?
O5 Sm1 O12 C8 99.5(7) . . . 3_557 ?
O16 Sm1 O12 C8 -162.1(7) . . . 3_557 ?
O3 Sm1 O12 C8 60.4(8) . . . 3_557 ?
O1 Sm1 O12 C8 166.6(7) . . . 3_557 ?
N7 Sm1 O12 C8 -86.0(8) . . . 3_557 ?
N2 Sm1 O12 C8 -82.5(7) . . . 3_557 ?
C4 Sm1 O12 C8 -173.9(7) . . . 3_557 ?
C10 C11 C14 C23 -3.2(6) . . . . ?
C10 C11 C14 O13 -177.7(4) . . . . ?
C30 O13 C14 C11 -38.2(6) . . . . ?
C30 O13 C14 C23 147.1(4) . . . . ?
C34 C9 C15 C22 1.1(6) . . . . ?
C8 C9 C15 C22 -179.1(4) . . . . ?
O1 C4 O16 Sm1 11.6(4) . . . . ?
C10 C4 O16 Sm1 -165.9(3) . . . . ?
O12 Sm1 O16 C4 -153.4(2) . . . . ?
O6 Sm1 O16 C4 142.3(2) . . . . ?
O5 Sm1 O16 C4 -78.8(2) . . . . ?
O3 Sm1 O16 C4 -13.8(3) . . . . ?
O1 Sm1 O16 C4 -6.2(2) . . . . ?
N7 Sm1 O16 C4 60.7(2) . . . . ?
N2 Sm1 O16 C4 123.1(2) . . . . ?
C24 N2 C17 C1 1.2(6) . . . . ?
Sm1 N2 C17 C1 177.1(3) . . . . ?
C31 N7 C18 C28 0.0(6) . . . . ?
Sm1 N7 C18 C28 179.3(3) . . . . ?
C31 N7 C18 C24 179.6(4) . . . . ?
Sm1 N7 C18 C24 -1.1(4) . . . . ?
C11 C10 C19 C33 0.2(6) . . . . ?
C4 C10 C19 C33 177.3(4) . . . . ?
Sm1 O3 C21 O5 175.6(3) . . . 3_657 ?
Sm1 O3 C21 C21 -5.2(5) . . . 3_657 ?
C9 C15 C22 C30 -0.3(6) . . . 4_566 ?
C11 C14 C23 C33 1.0(7) . . . . ?
O13 C14 C23 C33 175.9(4) . . . . ?
C17 N2 C24 C35 0.3(6) . . . . ?
Sm1 N2 C24 C35 -175.8(3) . . . . ?
C17 N2 C24 C18 -178.6(3) . . . . ?
Sm1 N2 C24 C18 5.3(4) . . . . ?
N7 C18 C24 N2 -2.9(5) . . . . ?
C28 C18 C24 N2 176.7(3) . . . . ?
N7 C18 C24 C35 178.3(3) . . . . ?
C28 C18 C24 C35 -2.2(6) . . . . ?
C29 C25 C28 C18 -1.4(7) . . . . ?
C29 C25 C28 C5 177.3(5) . . . . ?
N7 C18 C28 C25 1.3(6) . . . . ?
C24 C18 C28 C25 -178.2(4) . . . . ?
N7 C18 C28 C5 -177.5(4) . . . . ?
C24 C18 C28 C5 3.0(6) . . . . ?
C28 C25 C29 C31 0.2(8) . . . . ?
C14 O13 C30 C22 147.0(4) . . . 4_665 ?
C14 O13 C30 C41 -37.0(6) . . . . ?
C18 N7 C31 C29 -1.3(6) . . . . ?
Sm1 N7 C31 C29 179.4(4) . . . . ?
C25 C29 C31 N7 1.2(8) . . . . ?
C10 C19 C33 C23 -2.4(7) . . . . ?
C14 C23 C33 C19 1.8(7) . . . . ?
C15 C9 C34 C41 -0.9(6) . . . 4_566 ?
C8 C9 C34 C41 179.3(4) . . . 4_566 ?
N2 C24 C35 C3 -1.4(6) . . . . ?
C18 C24 C35 C3 177.4(4) . . . . ?
N2 C24 C35 C20 179.9(4) . . . . ?
C18 C24 C35 C20 -1.3(6) . . . . ?
C5 C20 C35 C3 -174.5(5) . . . . ?
C5 C20 C35 C24 4.0(8) . . . . ?
C22 C30 C41 C34 -1.0(7) 4_665 . . 4_665 ?
O13 C30 C41 C34 -176.7(4) . . . 4_665 ?
N2 C17 C1 C3 -1.5(8) . . . . ?
C17 C1 C3 C35 0.1(8) . . . . ?
C24 C35 C3 C1 1.2(7) . . . . ?
C20 C35 C3 C1 179.8(5) . . . . ?
C35 C20 C5 C28 -3.3(9) . . . . ?
C25 C28 C5 C20 -179.0(5) . . . . ?
C18 C28 C5 C20 -0.3(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.093

####################################################################### 
# 
# 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_ww
_database_code_depnum_ccdc_archive 'CCDC 1407683'
_audit_update_record             
;
2015-06-19 deposited with the CCDC.
2017-12-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H6 K O11 Tb'
_chemical_formula_weight         428.11

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   22.5075(14)
_cell_length_b                   7.4564(5)
_cell_length_c                   12.6990(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.339(2)
_cell_angle_gamma                90.00
_cell_volume                     2108.7(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_exptl_absorpt_coefficient_mu    7.154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3150
_exptl_absorpt_correction_T_max  0.3434
_exptl_absorpt_process_details   sadabs

_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-CCD
_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            10840
_diffrn_reflns_av_R_equivalents  0.0867
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1850
_reflns_number_gt                1475
_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)+(0.0266P)²+370.6359P] 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         1850
_refine_ls_number_parameters     154
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0656
_refine_ls_wR_factor_ref         0.1580
_refine_ls_wR_factor_gt          0.1491
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.078
_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 0.13729(3) 0.00205(9) 0.51430(4) 0.01331(15) Uani 1 1 d U . .
K1 K 0.08132(18) 0.5006(5) 0.3742(3) 0.0408(9) Uani 1 1 d U . .
C1 C 0.1529(6) -0.080(2) 0.2704(10) 0.024(3) Uani 1 1 d U . .
C2 C 0.1111(6) 0.0800(18) 0.2576(9) 0.014(3) Uani 1 1 d U . .
C3 C -0.0018(6) -0.0963(18) 0.4746(9) 0.016(3) Uani 1 1 d U . .
C4 C 0.2291(5) 0.3305(18) 0.4903(10) 0.016(3) Uani 1 1 d U . .
O1 O 0.1727(5) -0.1377(18) 0.1876(8) 0.041(3) Uani 1 1 d U . .
O1W O -0.0418(5) 0.4930(18) 0.3484(9) 0.045(3) Uani 1 1 d U . .
H1WB H -0.0570 0.5949 0.3823 0.054 Uiso 1 1 d R . .
H1WA H -0.0555 0.3858 0.3791 0.054 Uiso 1 1 d R . .
O2 O 0.1644(5) -0.1519(17) 0.3594(8) 0.041(3) Uani 1 1 d U . .
O2W O 0.1880(6) 0.4884(19) 0.2381(9) 0.053(3) Uani 1 1 d U . .
H2WB H 0.1867 0.5939 0.1945 0.079 Uiso 1 1 d R . .
H2WA H 0.2255 0.4842 0.2849 0.079 Uiso 1 1 d R . .
O3 O 0.0977(4) 0.1380(13) 0.1663(7) 0.021(2) Uani 1 1 d U . .
O3W O 0.1762(4) -0.2894(13) 0.5548(8) 0.026(2) Uani 1 1 d U . .
H3WB H 0.1699 -0.3214 0.6256 0.039 Uiso 1 1 d R . .
H3WA H 0.2185 -0.2902 0.5506 0.039 Uiso 1 1 d R . .
O4 O 0.0956(5) 0.1377(14) 0.3413(7) 0.028(2) Uani 1 1 d U . .
O5 O -0.0512(4) -0.1706(13) 0.4607(7) 0.018(2) Uani 1 1 d U . .
O6 O 0.0465(4) -0.1591(13) 0.4544(7) 0.019(2) Uani 1 1 d U . .
O7 O 0.1745(4) 0.3010(14) 0.4895(8) 0.029(2) Uani 1 1 d U . .
O8 O 0.2538(5) 0.4735(14) 0.4754(10) 0.037(3) Uani 1 1 d U . .


_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 O5 2.369(9) 5_556 ?
Tb1 O3W 2.371(10) . ?
Tb1 O6 2.398(9) . ?
Tb1 O7 2.418(11) . ?
Tb1 O2 2.431(11) . ?
Tb1 O8 2.443(11) 7_556 ?
Tb1 O1 2.448(10) 6_556 ?
Tb1 O3 2.471(9) 6_556 ?
Tb1 O4 2.477(10) . ?
Tb1 K1 4.233(4) . ?
Tb1 K1 4.253(4) 1_545 ?
K1 O1W 2.744(12) . ?
K1 O4 2.763(11) . ?
K1 O7 2.804(11) . ?
K1 O1W 2.838(12) 2 ?
K1 O6 2.885(10) 1_565 ?
K1 O2W 3.156(14) . ?
K1 O2 3.217(14) 1_565 ?
K1 O3W 3.295(11) 1_565 ?
K1 O5 3.364(10) 5_556 ?
K1 Tb1 4.253(4) 1_565 ?
K1 K1 4.472(7) 2 ?
C1 O2 1.242(17) . ?
C1 O1 1.274(17) . ?
C1 C2 1.515(19) . ?
C2 O3 1.233(15) . ?
C2 O4 1.244(16) . ?
C3 O5 1.232(16) . ?
C3 O6 1.243(16) . ?
C3 C3 1.57(3) 5_556 ?
C4 O8 1.230(17) . ?
C4 O7 1.246(16) . ?
C4 C4 1.52(3) 7_556 ?
O1 Tb1 2.448(10) 6 ?
O1W K1 2.838(12) 2 ?
O2 K1 3.217(14) 1_545 ?
O3 Tb1 2.471(9) 6 ?
O3W K1 3.295(11) 1_545 ?
O5 Tb1 2.369(9) 5_556 ?
O5 K1 3.364(10) 5_556 ?
O6 K1 2.885(10) 1_545 ?
O8 Tb1 2.443(11) 7_556 ?

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 Tb1 O3W 137.8(3) 5_556 . ?
O5 Tb1 O6 68.4(3) 5_556 . ?
O3W Tb1 O6 83.2(3) . . ?
O5 Tb1 O7 80.4(3) 5_556 . ?
O3W Tb1 O7 138.5(3) . . ?
O6 Tb1 O7 135.7(3) . . ?
O5 Tb1 O2 131.7(3) 5_556 . ?
O3W Tb1 O2 67.3(4) . . ?
O6 Tb1 O2 79.0(4) . . ?
O7 Tb1 O2 101.4(4) . . ?
O5 Tb1 O8 141.9(3) 5_556 7_556 ?
O3W Tb1 O8 73.8(3) . 7_556 ?
O6 Tb1 O8 149.0(3) . 7_556 ?
O7 Tb1 O8 64.8(3) . 7_556 ?
O2 Tb1 O8 73.2(4) . 7_556 ?
O5 Tb1 O1 80.0(4) 5_556 6_556 ?
O3W Tb1 O1 97.0(4) . 6_556 ?
O6 Tb1 O1 130.1(3) . 6_556 ?
O7 Tb1 O1 70.3(4) . 6_556 ?
O2 Tb1 O1 146.6(4) . 6_556 ?
O8 Tb1 O1 74.2(4) 7_556 6_556 ?
O5 Tb1 O3 74.1(3) 5_556 6_556 ?
O3W Tb1 O3 66.9(3) . 6_556 ?
O6 Tb1 O3 69.4(3) . 6_556 ?
O7 Tb1 O3 131.5(3) . 6_556 ?
O2 Tb1 O3 126.4(4) . 6_556 ?
O8 Tb1 O3 117.5(4) 7_556 6_556 ?
O1 Tb1 O3 65.1(3) 6_556 6_556 ?
O5 Tb1 O4 71.9(3) 5_556 . ?
O3W Tb1 O4 130.4(3) . . ?
O6 Tb1 O4 74.2(3) . . ?
O7 Tb1 O4 66.5(3) . . ?
O2 Tb1 O4 65.3(3) . . ?
O8 Tb1 O4 105.4(4) 7_556 . ?
O1 Tb1 O4 131.4(4) 6_556 . ?
O3 Tb1 O4 137.1(3) 6_556 . ?
O5 Tb1 K1 52.5(2) 5_556 . ?
O3W Tb1 K1 166.9(2) . . ?
O6 Tb1 K1 96.8(2) . . ?
O7 Tb1 K1 39.0(2) . . ?
O2 Tb1 K1 99.7(3) . . ?
O8 Tb1 K1 101.1(3) 7_556 . ?
O1 Tb1 K1 93.1(3) 6_556 . ?
O3 Tb1 K1 125.5(2) 6_556 . ?
O4 Tb1 K1 38.5(2) . . ?
O5 Tb1 K1 108.9(2) 5_556 1_545 ?
O3W Tb1 K1 50.4(3) . 1_545 ?
O6 Tb1 K1 40.5(2) . 1_545 ?
O7 Tb1 K1 147.5(3) . 1_545 ?
O2 Tb1 K1 48.7(3) . 1_545 ?
O8 Tb1 K1 108.8(3) 7_556 1_545 ?
O1 Tb1 K1 141.0(3) 6_556 1_545 ?
O3 Tb1 K1 80.6(2) 6_556 1_545 ?
O4 Tb1 K1 86.4(2) . 1_545 ?
K1 Tb1 K1 122.97(9) . 1_545 ?
O1W K1 O4 95.7(4) . . ?
O1W K1 O7 135.9(4) . . ?
O4 K1 O7 57.7(3) . . ?
O1W K1 O1W 73.5(4) . 2 ?
O4 K1 O1W 81.7(3) . 2 ?
O7 K1 O1W 127.7(4) . 2 ?
O1W K1 O6 74.8(3) . 1_565 ?
O4 K1 O6 163.3(3) . 1_565 ?
O7 K1 O6 120.2(3) . 1_565 ?
O1W K1 O6 107.9(3) 2 1_565 ?
O1W K1 O2W 140.3(3) . . ?
O4 K1 O2W 77.0(4) . . ?
O7 K1 O2W 72.5(3) . . ?
O1W K1 O2W 66.9(3) 2 . ?
O6 K1 O2W 119.1(3) 1_565 . ?
O1W K1 O2 126.5(4) . 1_565 ?
O4 K1 O2 134.3(3) . 1_565 ?
O7 K1 O2 93.5(3) . 1_565 ?
O1W K1 O2 93.4(3) 2 1_565 ?
O6 K1 O2 60.2(3) 1_565 1_565 ?
O2W K1 O2 59.8(3) . 1_565 ?
O1W K1 O3W 129.4(3) . 1_565 ?
O4 K1 O3W 119.5(3) . 1_565 ?
O7 K1 O3W 61.9(3) . 1_565 ?
O1W K1 O3W 141.3(3) 2 1_565 ?
O6 K1 O3W 61.2(2) 1_565 1_565 ?
O2W K1 O3W 85.8(3) . 1_565 ?
O2 K1 O3W 48.3(3) 1_565 1_565 ?
O1W K1 O5 76.6(3) . 5_556 ?
O4 K1 O5 54.3(3) . 5_556 ?
O7 K1 O5 59.3(3) . 5_556 ?
O1W K1 O5 122.9(3) 2 5_556 ?
O6 K1 O5 109.5(3) 1_565 5_556 ?
O2W K1 O5 123.9(3) . 5_556 ?
O2 K1 O5 142.8(3) 1_565 5_556 ?
O3W K1 O5 94.7(2) 1_565 5_556 ?
O1W K1 Tb1 105.4(3) . . ?
O4 K1 Tb1 33.9(2) . . ?
O7 K1 Tb1 32.9(2) . . ?
O1W K1 Tb1 115.6(3) 2 . ?
O6 K1 Tb1 134.7(2) 1_565 . ?
O2W K1 Tb1 90.1(3) . . ?
O2 K1 Tb1 126.3(2) 1_565 . ?
O3W K1 Tb1 90.08(18) 1_565 . ?
O5 K1 Tb1 33.96(16) 5_556 . ?
O1W K1 Tb1 107.5(3) . 1_565 ?
O4 K1 Tb1 152.9(2) . 1_565 ?
O7 K1 Tb1 95.4(2) . 1_565 ?
O1W K1 Tb1 117.7(3) 2 1_565 ?
O6 K1 Tb1 32.67(18) 1_565 1_565 ?
O2W K1 Tb1 93.0(3) . 1_565 ?
O2 K1 Tb1 34.6(2) 1_565 1_565 ?
O3W K1 Tb1 33.69(17) 1_565 1_565 ?
O5 K1 Tb1 117.17(18) 5_556 1_565 ?
Tb1 K1 Tb1 122.97(8) . 1_565 ?
O1W K1 K1 37.5(2) . 2 ?
O4 K1 K1 89.7(2) . 2 ?
O7 K1 K1 147.3(2) . 2 ?
O1W K1 K1 36.0(2) 2 2 ?
O6 K1 K1 90.70(19) 1_565 2 ?
O2W K1 K1 102.9(2) . 2 ?
O2 K1 K1 112.5(2) 1_565 2 ?
O3W K1 K1 150.78(18) 1_565 2 ?
O5 K1 K1 102.78(18) 5_556 2 ?
Tb1 K1 K1 117.37(6) . 2 ?
Tb1 K1 K1 117.23(5) 1_565 2 ?
O2 C1 O1 123.6(14) . . ?
O2 C1 C2 118.8(12) . . ?
O1 C1 C2 117.5(12) . . ?
O3 C2 O4 128.4(13) . . ?
O3 C2 C1 116.2(11) . . ?
O4 C2 C1 115.4(11) . . ?
O5 C3 O6 126.8(13) . . ?
O5 C3 C3 117.5(14) . 5_556 ?
O6 C3 C3 115.7(14) . 5_556 ?
O8 C4 O7 128.3(13) . . ?
O8 C4 C4 115.1(14) . 7_556 ?
O7 C4 C4 116.6(15) . 7_556 ?
C1 O1 Tb1 119.7(9) . 6 ?
K1 O1W K1 106.5(4) . 2 ?
C1 O2 Tb1 119.3(10) . . ?
C1 O2 K1 110.7(10) . 1_545 ?
Tb1 O2 K1 96.7(4) . 1_545 ?
C2 O3 Tb1 121.3(9) . 6 ?
Tb1 O3W K1 95.9(3) . 1_545 ?
C2 O4 Tb1 120.0(9) . . ?
C2 O4 K1 121.5(9) . . ?
Tb1 O4 K1 107.6(3) . . ?
C3 O5 Tb1 118.8(9) . 5_556 ?
C3 O5 K1 119.9(8) . 5_556 ?
Tb1 O5 K1 93.6(3) 5_556 5_556 ?
C3 O6 Tb1 118.4(8) . . ?
C3 O6 K1 134.0(8) . 1_545 ?
Tb1 O6 K1 106.8(3) . 1_545 ?
C4 O7 Tb1 121.4(9) . . ?
C4 O7 K1 124.9(9) . . ?
Tb1 O7 K1 108.1(4) . . ?
C4 O8 Tb1 122.0(9) . 7_556 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.914
_refine_diff_density_min         -2.869
_refine_diff_density_rms         0.282
####################################################################### 
# 
# 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_ww_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1407682'
_audit_update_record             
;
2015-06-19 deposited with the CCDC.
2017-12-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H16 Gd N2 O7'
_chemical_formula_weight         637.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/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                   9.6274(4)
_cell_length_b                   16.8937(7)
_cell_length_c                   15.1022(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.6510(10)
_cell_angle_gamma                90.00
_cell_volume                     2365.19(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    2.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6129
_exptl_absorpt_correction_T_max  0.6740
_exptl_absorpt_process_details   sadabs

_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-CCD
_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            30914
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4158
_reflns_number_gt                3310
_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)+(0.0352P)²+4.5417P] 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         4158
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0783
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.31878(2) 0.024918(14) 0.610754(16) 0.02611(10) Uani 1 1 d . . .
N1 N 0.3378(5) 0.1575(2) 0.6945(3) 0.0348(10) Uani 1 1 d . . .
N2 N 0.5789(4) 0.0795(3) 0.6816(3) 0.0329(10) Uani 1 1 d . . .
O1 O 0.3904(4) -0.0418(2) 0.7554(2) 0.0453(10) Uani 1 1 d . . .
O2 O 0.1802(4) 0.0155(2) 0.7282(3) 0.0435(10) Uani 1 1 d . . .
O3 O 0.1447(5) 0.0633(2) 1.0601(3) 0.0593(12) Uani 1 1 d . . .
O4 O 0.0550(4) 0.4222(2) 0.9286(3) 0.0405(9) Uani 1 1 d . . .
O5 O -0.1238(4) 0.4061(2) 0.9938(2) 0.0341(8) Uani 1 1 d . . .
O7 O -0.0958(4) -0.0876(2) 0.4668(2) 0.0371(9) Uani 1 1 d . . .
O8 O 0.1376(3) -0.0688(2) 0.5386(2) 0.0372(9) Uani 1 1 d . . .
C1 C 0.2212(7) 0.1941(3) 0.7040(4) 0.0496(16) Uani 1 1 d . . .
H1A H 0.1318 0.1709 0.6785 0.060 Uiso 1 1 calc R . .
C2 C 0.2257(8) 0.2660(4) 0.7504(5) 0.0595(18) Uani 1 1 d . . .
H2A H 0.1412 0.2896 0.7558 0.071 Uiso 1 1 calc R . .
C3 C 0.3546(9) 0.3004(4) 0.7873(4) 0.062(2) Uani 1 1 d . . .
H3A H 0.3596 0.3478 0.8194 0.074 Uiso 1 1 calc R . .
C4 C 0.4799(7) 0.2654(3) 0.7773(4) 0.0498(16) Uani 1 1 d . . .
C5 C 0.6194(9) 0.3003(4) 0.8108(5) 0.074(2) Uani 1 1 d . . .
H5A H 0.6285 0.3486 0.8414 0.088 Uiso 1 1 calc R . .
C6 C 0.7377(8) 0.2647(5) 0.7988(5) 0.072(2) Uani 1 1 d . . .
H6A H 0.8263 0.2903 0.8183 0.086 Uiso 1 1 calc R . .
C7 C 0.7307(7) 0.1884(4) 0.7569(4) 0.0511(16) Uani 1 1 d . . .
C8 C 0.8506(7) 0.1454(5) 0.7492(5) 0.068(2) Uani 1 1 d . . .
H8A H 0.9423 0.1669 0.7718 0.082 Uiso 1 1 calc R . .
C9 C 0.8358(6) 0.0737(5) 0.7098(4) 0.0619(19) Uani 1 1 d . . .
H9A H 0.9162 0.0452 0.7052 0.074 Uiso 1 1 calc R . .
C10 C 0.6974(6) 0.0429(4) 0.6759(4) 0.0486(16) Uani 1 1 d . . .
H10A H 0.6879 -0.0064 0.6476 0.058 Uiso 1 1 calc R . .
C11 C 0.5942(6) 0.1522(3) 0.7220(3) 0.0369(13) Uani 1 1 d . . .
C12 C 0.4678(6) 0.1920(3) 0.7315(3) 0.0345(12) Uani 1 1 d . . .
C13 C 0.2848(6) -0.0179(3) 0.7828(4) 0.0343(12) Uani 1 1 d . . .
C14 C 0.2918(6) -0.0278(3) 0.8831(4) 0.0368(12) Uani 1 1 d . . .
C15 C 0.3839(6) -0.0816(3) 0.9367(4) 0.0422(14) Uani 1 1 d . . .
H15A H 0.4392 -0.1146 0.9104 0.051 Uiso 1 1 calc R . .
C16 C 0.3945(7) -0.0868(4) 1.0287(4) 0.0509(16) Uani 1 1 d . . .
H16A H 0.4545 -0.1249 1.0641 0.061 Uiso 1 1 calc R . .
C17 C 0.3176(7) -0.0365(4) 1.0698(4) 0.0493(16) Uani 1 1 d . . .
H17A H 0.3279 -0.0390 1.1327 0.059 Uiso 1 1 calc R . .
C18 C 0.2252(6) 0.0177(3) 1.0157(4) 0.0393(13) Uani 1 1 d . . .
C20 C 0.2095(6) 0.0221(3) 0.9226(4) 0.0383(13) Uani 1 1 d . . .
H20A H 0.1451 0.0579 0.8864 0.046 Uiso 1 1 calc R . .
C21 C 0.1103(7) 0.1404(3) 1.0341(4) 0.0420(14) Uani 1 1 d . . .
C22 C 0.2034(6) 0.1917(3) 1.0071(4) 0.0477(15) Uani 1 1 d . . .
H22A H 0.2929 0.1738 1.0032 0.057 Uiso 1 1 calc R . .
C23 C 0.1631(6) 0.2696(3) 0.9861(4) 0.0411(14) Uani 1 1 d . . .
H23A H 0.2250 0.3037 0.9668 0.049 Uiso 1 1 calc R . .
C24 C 0.0309(5) 0.2971(3) 0.9936(3) 0.0307(12) Uani 1 1 d . . .
C25 C -0.0607(6) 0.2451(3) 1.0223(4) 0.0401(14) Uani 1 1 d . . .
H25A H -0.1495 0.2629 1.0276 0.048 Uiso 1 1 calc R . .
C26 C -0.0202(6) 0.1675(3) 1.0428(4) 0.0419(14) Uani 1 1 d . . .
H26A H -0.0813 0.1334 1.0627 0.050 Uiso 1 1 calc R . .
C27 C -0.0137(5) 0.3807(3) 0.9711(3) 0.0293(11) Uani 1 1 d . . .
C28 C 0.0120(5) -0.0452(3) 0.5012(3) 0.0279(12) 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 O4 2.287(3) 2_546 ?
Gd1 O5 2.304(3) 4_665 ?
Gd1 O1 2.388(4) . ?
Gd1 O8 2.390(3) . ?
Gd1 O7 2.397(3) 3_556 ?
Gd1 O2 2.495(4) . ?
Gd1 N1 2.555(4) . ?
Gd1 N2 2.612(4) . ?
Gd1 C13 2.800(5) . ?
N1 C1 1.322(7) . ?
N1 C12 1.357(6) . ?
N2 C10 1.322(7) . ?
N2 C11 1.361(7) . ?
O1 C13 1.262(6) . ?
O2 C13 1.251(6) . ?
O3 C21 1.376(6) . ?
O3 C18 1.386(6) . ?
O4 C27 1.252(6) . ?
O4 Gd1 2.287(3) 2_556 ?
O5 C27 1.273(6) . ?
O5 Gd1 2.304(3) 4_566 ?
O7 C28 1.253(6) . ?
O7 Gd1 2.397(3) 3_556 ?
O8 C28 1.253(5) . ?
C1 C2 1.396(8) . ?
C1 H1A 0.9300 . ?
C2 C3 1.348(9) . ?
C2 H2A 0.9300 . ?
C3 C4 1.388(9) . ?
C3 H3A 0.9300 . ?
C4 C12 1.409(8) . ?
C4 C5 1.428(9) . ?
C5 C6 1.342(10) . ?
C5 H5A 0.9300 . ?
C6 C7 1.429(10) . ?
C6 H6A 0.9300 . ?
C7 C8 1.396(9) . ?
C7 C11 1.416(8) . ?
C8 C9 1.340(10) . ?
C8 H8A 0.9300 . ?
C9 C10 1.393(8) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.431(7) . ?
C13 C14 1.507(8) . ?
C14 C15 1.372(7) . ?
C14 C20 1.396(7) . ?
C15 C16 1.369(7) . ?
C15 H15A 0.9300 . ?
C16 C17 1.380(8) . ?
C16 H16A 0.9300 . ?
C17 C18 1.380(8) . ?
C17 H17A 0.9300 . ?
C18 C20 1.376(8) . ?
C20 H20A 0.9300 . ?
C21 C26 1.377(8) . ?
C21 C22 1.383(8) . ?
C22 C23 1.385(8) . ?
C22 H22A 0.9300 . ?
C23 C24 1.388(7) . ?
C23 H23A 0.9300 . ?
C24 C25 1.393(7) . ?
C24 C27 1.490(7) . ?
C25 C26 1.379(8) . ?
C25 H25A 0.9300 . ?
C26 H26A 0.9300 . ?
C28 C28 1.543(9) 3_556 ?

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 Gd1 O5 86.05(12) 2_546 4_665 ?
O4 Gd1 O1 80.61(13) 2_546 . ?
O5 Gd1 O1 150.44(12) 4_665 . ?
O4 Gd1 O8 75.67(12) 2_546 . ?
O5 Gd1 O8 106.39(12) 4_665 . ?
O1 Gd1 O8 95.74(13) . . ?
O4 Gd1 O7 132.60(13) 2_546 3_556 ?
O5 Gd1 O7 76.72(12) 4_665 3_556 ?
O1 Gd1 O7 130.92(12) . 3_556 ?
O8 Gd1 O7 67.81(12) . 3_556 ?
O4 Gd1 O2 124.01(13) 2_546 . ?
O5 Gd1 O2 149.51(12) 4_665 . ?
O1 Gd1 O2 52.96(12) . . ?
O8 Gd1 O2 79.47(13) . . ?
O7 Gd1 O2 78.20(12) 3_556 . ?
O4 Gd1 N1 145.28(13) 2_546 . ?
O5 Gd1 N1 86.33(13) 4_665 . ?
O1 Gd1 N1 89.78(13) . . ?
O8 Gd1 N1 138.80(13) . . ?
O7 Gd1 N1 77.86(13) 3_556 . ?
O2 Gd1 N1 71.62(13) . . ?
O4 Gd1 N2 81.76(13) 2_546 . ?
O5 Gd1 N2 74.56(12) 4_665 . ?
O1 Gd1 N2 77.49(13) . . ?
O8 Gd1 N2 157.24(13) . . ?
O7 Gd1 N2 132.65(13) 3_556 . ?
O2 Gd1 N2 111.63(13) . . ?
N1 Gd1 N2 63.56(14) . . ?
O4 Gd1 C13 104.36(14) 2_546 . ?
O5 Gd1 C13 162.56(14) 4_665 . ?
O1 Gd1 C13 26.69(14) . . ?
O8 Gd1 C13 89.92(14) . . ?
O7 Gd1 C13 104.74(14) 3_556 . ?
O2 Gd1 C13 26.54(13) . . ?
N1 Gd1 C13 77.15(14) . . ?
N2 Gd1 C13 92.86(14) . . ?
C1 N1 C12 118.1(5) . . ?
C1 N1 Gd1 120.9(4) . . ?
C12 N1 Gd1 121.0(3) . . ?
C10 N2 C11 117.4(5) . . ?
C10 N2 Gd1 123.9(4) . . ?
C11 N2 Gd1 118.6(3) . . ?
C13 O1 Gd1 95.2(3) . . ?
C13 O2 Gd1 90.4(3) . . ?
C21 O3 C18 120.7(4) . . ?
C27 O4 Gd1 161.5(3) . 2_556 ?
C27 O5 Gd1 140.0(3) . 4_566 ?
C28 O7 Gd1 118.9(3) . 3_556 ?
C28 O8 Gd1 119.4(3) . . ?
N1 C1 C2 123.2(6) . . ?
N1 C1 H1A 118.4 . . ?
C2 C1 H1A 118.4 . . ?
C3 C2 C1 118.9(6) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 120.1(6) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 C12 118.0(6) . . ?
C3 C4 C5 123.2(6) . . ?
C12 C4 C5 118.8(6) . . ?
C6 C5 C4 121.2(6) . . ?
C6 C5 H5A 119.4 . . ?
C4 C5 H5A 119.4 . . ?
C5 C6 C7 121.5(6) . . ?
C5 C6 H6A 119.2 . . ?
C7 C6 H6A 119.2 . . ?
C8 C7 C11 116.7(6) . . ?
C8 C7 C6 124.4(6) . . ?
C11 C7 C6 118.9(6) . . ?
C9 C8 C7 121.1(6) . . ?
C9 C8 H8A 119.4 . . ?
C7 C8 H8A 119.4 . . ?
C8 C9 C10 118.5(6) . . ?
C8 C9 H9A 120.7 . . ?
C10 C9 H9A 120.7 . . ?
N2 C10 C9 123.9(6) . . ?
N2 C10 H10A 118.0 . . ?
C9 C10 H10A 118.0 . . ?
N2 C11 C7 122.3(5) . . ?
N2 C11 C12 118.5(5) . . ?
C7 C11 C12 119.2(5) . . ?
N1 C12 C4 121.7(5) . . ?
N1 C12 C11 118.2(5) . . ?
C4 C12 C11 120.2(5) . . ?
O2 C13 O1 120.3(5) . . ?
O2 C13 C14 121.5(5) . . ?
O1 C13 C14 118.2(5) . . ?
O2 C13 Gd1 63.0(3) . . ?
O1 C13 Gd1 58.2(3) . . ?
C14 C13 Gd1 167.6(4) . . ?
C15 C14 C20 120.0(5) . . ?
C15 C14 C13 120.8(5) . . ?
C20 C14 C13 119.1(5) . . ?
C16 C15 C14 120.0(5) . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 120.0 . . ?
C15 C16 C17 121.0(6) . . ?
C15 C16 H16A 119.5 . . ?
C17 C16 H16A 119.5 . . ?
C16 C17 C18 118.8(5) . . ?
C16 C17 H17A 120.6 . . ?
C18 C17 H17A 120.6 . . ?
C20 C18 C17 121.0(5) . . ?
C20 C18 O3 122.9(5) . . ?
C17 C18 O3 116.0(5) . . ?
C18 C20 C14 119.1(5) . . ?
C18 C20 H20A 120.5 . . ?
C14 C20 H20A 120.5 . . ?
O3 C21 C26 116.3(5) . . ?
O3 C21 C22 123.5(5) . . ?
C26 C21 C22 120.0(5) . . ?
C21 C22 C23 119.9(5) . . ?
C21 C22 H22A 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C22 C23 C24 120.3(5) . . ?
C22 C23 H23A 119.8 . . ?
C24 C23 H23A 119.8 . . ?
C23 C24 C25 119.1(5) . . ?
C23 C24 C27 120.8(5) . . ?
C25 C24 C27 120.1(5) . . ?
C26 C25 C24 120.3(5) . . ?
C26 C25 H25A 119.9 . . ?
C24 C25 H25A 119.9 . . ?
C21 C26 C25 120.3(5) . . ?
C21 C26 H26A 119.9 . . ?
C25 C26 H26A 119.9 . . ?
O4 C27 O5 123.0(5) . . ?
O4 C27 C24 119.2(5) . . ?
O5 C27 C24 117.8(4) . . ?
O7 C28 O8 126.5(4) . . ?
O7 C28 C28 117.0(5) . 3_556 ?
O8 C28 C28 116.5(5) . 3_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Gd1 N1 C1 -174.3(4) 2_546 . . . ?
O5 Gd1 N1 C1 108.0(4) 4_665 . . . ?
O1 Gd1 N1 C1 -101.3(4) . . . . ?
O8 Gd1 N1 C1 -2.8(5) . . . . ?
O7 Gd1 N1 C1 30.9(4) 3_556 . . . ?
O2 Gd1 N1 C1 -50.6(4) . . . . ?
N2 Gd1 N1 C1 -177.4(5) . . . . ?
C13 Gd1 N1 C1 -77.6(4) . . . . ?
O4 Gd1 N1 C12 4.9(5) 2_546 . . . ?
O5 Gd1 N1 C12 -72.7(4) 4_665 . . . ?
O1 Gd1 N1 C12 78.0(4) . . . . ?
O8 Gd1 N1 C12 176.4(3) . . . . ?
O7 Gd1 N1 C12 -149.9(4) 3_556 . . . ?
O2 Gd1 N1 C12 128.7(4) . . . . ?
N2 Gd1 N1 C12 1.9(3) . . . . ?
C13 Gd1 N1 C12 101.7(4) . . . . ?
O4 Gd1 N2 C10 2.1(4) 2_546 . . . ?
O5 Gd1 N2 C10 -86.1(4) 4_665 . . . ?
O1 Gd1 N2 C10 84.2(4) . . . . ?
O8 Gd1 N2 C10 9.5(6) . . . . ?
O7 Gd1 N2 C10 -140.7(4) 3_556 . . . ?
O2 Gd1 N2 C10 125.5(4) . . . . ?
N1 Gd1 N2 C10 -179.7(5) . . . . ?
C13 Gd1 N2 C10 106.2(4) . . . . ?
O4 Gd1 N2 C11 177.8(4) 2_546 . . . ?
O5 Gd1 N2 C11 89.7(4) 4_665 . . . ?
O1 Gd1 N2 C11 -100.0(4) . . . . ?
O8 Gd1 N2 C11 -174.7(3) . . . . ?
O7 Gd1 N2 C11 35.0(4) 3_556 . . . ?
O2 Gd1 N2 C11 -58.8(4) . . . . ?
N1 Gd1 N2 C11 -4.0(3) . . . . ?
C13 Gd1 N2 C11 -78.1(4) . . . . ?
O4 Gd1 O1 C13 -152.7(3) 2_546 . . . ?
O5 Gd1 O1 C13 143.0(3) 4_665 . . . ?
O8 Gd1 O1 C13 -78.3(3) . . . . ?
O7 Gd1 O1 C13 -12.8(4) 3_556 . . . ?
O2 Gd1 O1 C13 -6.1(3) . . . . ?
N1 Gd1 O1 C13 60.8(3) . . . . ?
N2 Gd1 O1 C13 123.7(3) . . . . ?
O4 Gd1 O2 C13 47.1(3) 2_546 . . . ?
O5 Gd1 O2 C13 -143.9(3) 4_665 . . . ?
O1 Gd1 O2 C13 6.1(3) . . . . ?
O8 Gd1 O2 C13 111.7(3) . . . . ?
O7 Gd1 O2 C13 -179.1(3) 3_556 . . . ?
N1 Gd1 O2 C13 -98.1(3) . . . . ?
N2 Gd1 O2 C13 -47.6(3) . . . . ?
O4 Gd1 O8 C28 -154.5(4) 2_546 . . . ?
O5 Gd1 O8 C28 -73.1(4) 4_665 . . . ?
O1 Gd1 O8 C28 126.7(3) . . . . ?
O7 Gd1 O8 C28 -5.3(3) 3_556 . . . ?
O2 Gd1 O8 C28 76.1(3) . . . . ?
N1 Gd1 O8 C28 30.5(4) . . . . ?
N2 Gd1 O8 C28 -162.1(3) . . . . ?
C13 Gd1 O8 C28 100.6(4) . . . . ?
C12 N1 C1 C2 -0.4(9) . . . . ?
Gd1 N1 C1 C2 178.9(5) . . . . ?
N1 C1 C2 C3 0.4(10) . . . . ?
C1 C2 C3 C4 1.2(10) . . . . ?
C2 C3 C4 C12 -2.7(9) . . . . ?
C2 C3 C4 C5 177.0(6) . . . . ?
C3 C4 C5 C6 -179.3(7) . . . . ?
C12 C4 C5 C6 0.4(10) . . . . ?
C4 C5 C6 C7 -3.6(12) . . . . ?
C5 C6 C7 C8 -174.6(7) . . . . ?
C5 C6 C7 C11 4.1(11) . . . . ?
C11 C7 C8 C9 0.6(10) . . . . ?
C6 C7 C8 C9 179.3(7) . . . . ?
C7 C8 C9 C10 0.4(11) . . . . ?
C11 N2 C10 C9 1.0(9) . . . . ?
Gd1 N2 C10 C9 176.8(5) . . . . ?
C8 C9 C10 N2 -1.3(10) . . . . ?
C10 N2 C11 C7 0.1(8) . . . . ?
Gd1 N2 C11 C7 -175.9(4) . . . . ?
C10 N2 C11 C12 -178.1(5) . . . . ?
Gd1 N2 C11 C12 5.8(6) . . . . ?
C8 C7 C11 N2 -0.9(8) . . . . ?
C6 C7 C11 N2 -179.7(6) . . . . ?
C8 C7 C11 C12 177.4(5) . . . . ?
C6 C7 C11 C12 -1.4(8) . . . . ?
C1 N1 C12 C4 -1.2(8) . . . . ?
Gd1 N1 C12 C4 179.5(4) . . . . ?
C1 N1 C12 C11 179.5(5) . . . . ?
Gd1 N1 C12 C11 0.2(6) . . . . ?
C3 C4 C12 N1 2.7(8) . . . . ?
C5 C4 C12 N1 -177.0(5) . . . . ?
C3 C4 C12 C11 -178.0(5) . . . . ?
C5 C4 C12 C11 2.3(8) . . . . ?
N2 C11 C12 N1 -4.1(7) . . . . ?
C7 C11 C12 N1 177.6(5) . . . . ?
N2 C11 C12 C4 176.6(5) . . . . ?
C7 C11 C12 C4 -1.7(8) . . . . ?
Gd1 O2 C13 O1 -10.8(5) . . . . ?
Gd1 O2 C13 C14 166.7(4) . . . . ?
Gd1 O1 C13 O2 11.3(5) . . . . ?
Gd1 O1 C13 C14 -166.3(4) . . . . ?
O4 Gd1 C13 O2 -141.2(3) 2_546 . . . ?
O5 Gd1 C13 O2 93.5(5) 4_665 . . . ?
O1 Gd1 C13 O2 -169.1(5) . . . . ?
O8 Gd1 C13 O2 -66.0(3) . . . . ?
O7 Gd1 C13 O2 1.0(3) 3_556 . . . ?
N1 Gd1 C13 O2 74.5(3) . . . . ?
N2 Gd1 C13 O2 136.6(3) . . . . ?
O4 Gd1 C13 O1 27.8(3) 2_546 . . . ?
O5 Gd1 C13 O1 -97.4(5) 4_665 . . . ?
O8 Gd1 C13 O1 103.0(3) . . . . ?
O7 Gd1 C13 O1 170.0(3) 3_556 . . . ?
O2 Gd1 C13 O1 169.1(5) . . . . ?
N1 Gd1 C13 O1 -116.4(3) . . . . ?
N2 Gd1 C13 O1 -54.4(3) . . . . ?
O4 Gd1 C13 C14 104.4(18) 2_546 . . . ?
O5 Gd1 C13 C14 -21(2) 4_665 . . . ?
O1 Gd1 C13 C14 76.5(18) . . . . ?
O8 Gd1 C13 C14 179.6(18) . . . . ?
O7 Gd1 C13 C14 -113.5(18) 3_556 . . . ?
O2 Gd1 C13 C14 -114.4(19) . . . . ?
N1 Gd1 C13 C14 -39.9(18) . . . . ?
N2 Gd1 C13 C14 22.2(18) . . . . ?
O2 C13 C14 C15 162.3(5) . . . . ?
O1 C13 C14 C15 -20.1(8) . . . . ?
Gd1 C13 C14 C15 -89.8(18) . . . . ?
O2 C13 C14 C20 -21.7(8) . . . . ?
O1 C13 C14 C20 155.9(5) . . . . ?
Gd1 C13 C14 C20 86.2(19) . . . . ?
C20 C14 C15 C16 0.5(8) . . . . ?
C13 C14 C15 C16 176.4(5) . . . . ?
C14 C15 C16 C17 -2.5(9) . . . . ?
C15 C16 C17 C18 2.3(9) . . . . ?
C16 C17 C18 C20 -0.2(9) . . . . ?
C16 C17 C18 O3 176.2(5) . . . . ?
C21 O3 C18 C20 -37.6(8) . . . . ?
C21 O3 C18 C17 146.0(6) . . . . ?
C17 C18 C20 C14 -1.7(8) . . . . ?
O3 C18 C20 C14 -177.9(5) . . . . ?
C15 C14 C20 C18 1.6(8) . . . . ?
C13 C14 C20 C18 -174.4(5) . . . . ?
C18 O3 C21 C26 147.3(5) . . . . ?
C18 O3 C21 C22 -37.7(9) . . . . ?
O3 C21 C22 C23 -177.0(5) . . . . ?
C26 C21 C22 C23 -2.1(9) . . . . ?
C21 C22 C23 C24 1.3(9) . . . . ?
C22 C23 C24 C25 -0.2(8) . . . . ?
C22 C23 C24 C27 -179.9(5) . . . . ?
C23 C24 C25 C26 0.0(8) . . . . ?
C27 C24 C25 C26 179.7(5) . . . . ?
O3 C21 C26 C25 177.1(5) . . . . ?
C22 C21 C26 C25 1.9(9) . . . . ?
C24 C25 C26 C21 -0.8(9) . . . . ?
Gd1 O4 C27 O5 52.7(13) 2_556 . . . ?
Gd1 O4 C27 C24 -129.5(9) 2_556 . . . ?
Gd1 O5 C27 O4 -86.0(6) 4_566 . . . ?
Gd1 O5 C27 C24 96.2(5) 4_566 . . . ?
C23 C24 C27 O4 13.8(7) . . . . ?
C25 C24 C27 O4 -166.0(5) . . . . ?
C23 C24 C27 O5 -168.4(5) . . . . ?
C25 C24 C27 O5 11.9(7) . . . . ?
Gd1 O7 C28 O8 -175.2(4) 3_556 . . . ?
Gd1 O7 C28 C28 5.8(7) 3_556 . . 3_556 ?
Gd1 O8 C28 O7 -174.5(4) . . . . ?
Gd1 O8 C28 C28 4.5(7) . . . 3_556 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.110
####################################################################### 
# 
# 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 1581053'
_audit_update_record             
;
2017-10-20 deposited with the CCDC.
2017-12-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H16 Dy N2 O7'
_chemical_formula_weight         642.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_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                   9.5712(5)
_cell_length_b                   16.8671(9)
_cell_length_c                   15.0395(8)
_cell_angle_alpha                90
_cell_angle_beta                 105.5706(16)
_cell_angle_gamma                90
_cell_volume                     2338.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9900
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      26.67

_exptl_crystal_description       rod
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.826
_exptl_crystal_F_000             1256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.387
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.089
_exptl_absorpt_coefficient_mu    3.247
_shelx_estimated_absorpt_T_min   0.366
_shelx_estimated_absorpt_T_max   0.761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33472
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_av_R_equivalents  0.1005
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.061
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5381
_reflns_number_gt                4003
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0900P)²+0.1783P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5381
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.1359
_refine_ls_wR_factor_gt          0.1173
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.994
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O4 O 0.4433(5) 0.4234(2) 0.0707(3) 0.0371(10) Uani 1 1 d . . . . .
O5 O 0.6228(4) 0.4072(2) 0.0058(3) 0.0322(9) Uani 1 1 d . . . . .
Dy1 Dy 0.18246(3) 0.02527(2) 0.39020(2) 0.02539(12) Uani 1 1 d . . . . .
C1 C 0.2162(7) -0.0177(4) 0.2195(5) 0.0348(15) Uani 1 1 d . . . . .
O2 O 0.3216(5) 0.0159(3) 0.2739(4) 0.0434(12) Uani 1 1 d . . . . .
C2 C 0.2086(7) -0.0274(3) 0.1187(5) 0.0317(14) Uani 1 1 d . . . . .
O1 O 0.1104(5) -0.0413(3) 0.2466(3) 0.0447(12) Uani 1 1 d . . . . .
C5 C 0.1817(8) -0.0366(4) -0.0691(5) 0.0445(17) Uani 1 1 d . . . . .
H5 H 0.1701 -0.0388 -0.1324 0.053 Uiso 1 1 calc R U . . .
C3 C 0.2912(8) 0.0222(4) 0.0788(5) 0.0384(16) Uani 1 1 d . . . . .
H3 H 0.3563 0.0579 0.1149 0.046 Uiso 1 1 calc R U . . .
C7 C 0.1158(7) -0.0818(4) 0.0647(4) 0.0382(15) Uani 1 1 d . . . . .
H7 H 0.0599 -0.1149 0.0909 0.046 Uiso 1 1 calc R U . . .
C4 C 0.2750(9) 0.0175(4) -0.0154(5) 0.0423(17) Uani 1 1 d . . . . .
C6 C 0.1064(8) -0.0870(4) -0.0278(5) 0.0477(18) Uani 1 1 d . . . . .
H6 H 0.0474 -0.1256 -0.0632 0.057 Uiso 1 1 calc R U . . .
N1 N -0.0764(5) 0.0792(3) 0.3180(3) 0.0334(12) Uani 1 1 d . . . . .
N2 N 0.1662(6) 0.1568(3) 0.3067(4) 0.0360(12) Uani 1 1 d . . . . .
C24 C -0.1956(8) 0.0415(5) 0.3242(5) 0.0480(19) Uani 1 1 d . . . . .
H24 H -0.1860 -0.0076 0.3533 0.058 Uiso 1 1 calc R U . . .
C15 C 0.2860(9) 0.1931(4) 0.2982(6) 0.0493(19) Uani 1 1 d . . . . .
H15 H 0.3755 0.1698 0.3248 0.059 Uiso 1 1 calc R U . . .
C25 C -0.0908(7) 0.1512(4) 0.2778(4) 0.0363(15) Uani 1 1 d . . . . .
C26 C 0.0365(7) 0.1912(4) 0.2694(4) 0.0330(14) Uani 1 1 d . . . . .
O3 O 0.3556(7) 0.0631(3) -0.0592(4) 0.0586(15) Uani 1 1 d . . . . .
C13 C 0.2954(8) 0.1925(4) -0.0062(5) 0.0464(18) Uani 1 1 d . . . . .
H13 H 0.2061 0.1742 -0.0013 0.056 Uiso 1 1 calc R U . . .
C8 C 0.3895(8) 0.1409(4) -0.0338(5) 0.0410(16) Uani 1 1 d . . . . .
C9 C 0.5215(8) 0.1680(4) -0.0424(5) 0.0398(16) Uani 1 1 d . . . . .
H9 H 0.5832 0.1338 -0.0621 0.048 Uiso 1 1 calc R U . . .
C12 C 0.3345(7) 0.2711(4) 0.0139(4) 0.0372(15) Uani 1 1 d . . . . .
H12 H 0.2713 0.3055 0.0319 0.045 Uiso 1 1 calc R U . . .
C17 C 0.1504(12) 0.2988(5) 0.2118(6) 0.064(3) Uani 1 1 d . . . . .
H17 H 0.1455 0.3455 0.1781 0.077 Uiso 1 1 calc R U . . .
C18 C 0.0228(9) 0.2641(4) 0.2219(5) 0.0480(18) Uani 1 1 d . . . . .
C21 C -0.2280(8) 0.1872(5) 0.2429(5) 0.0500(19) Uani 1 1 d . . . . .
C23 C -0.3349(8) 0.0730(6) 0.2888(6) 0.059(2) Uani 1 1 d . . . . .
H23 H -0.4163 0.0444 0.2926 0.071 Uiso 1 1 calc R U . . .
C22 C -0.3490(8) 0.1444(6) 0.2496(5) 0.062(2) Uani 1 1 d . . . . .
H22 H -0.4410 0.1660 0.2264 0.074 Uiso 1 1 calc R U . . .
C19 C -0.1149(11) 0.2992(5) 0.1887(6) 0.071(3) Uani 1 1 d . . . . .
H19 H -0.1232 0.3480 0.1590 0.086 Uiso 1 1 calc R U . . .
C16 C 0.2819(10) 0.2649(5) 0.2508(5) 0.059(2) Uani 1 1 d . . . . .
H16 H 0.3670 0.2889 0.2460 0.070 Uiso 1 1 calc R U . . .
C20 C -0.2348(10) 0.2630(5) 0.1995(6) 0.068(2) Uani 1 1 d . . . . .
H20 H -0.3242 0.2880 0.1782 0.082 Uiso 1 1 calc R U . . .
C11 C 0.4696(7) 0.2982(3) 0.0068(4) 0.0316(13) Uani 1 1 d . . . . .
C10 C 0.5613(8) 0.2455(4) -0.0219(4) 0.0387(16) Uani 1 1 d . . . . .
H10 H 0.6508 0.2632 -0.0273 0.046 Uiso 1 1 calc R U . . .
C14 C 0.5139(6) 0.3822(3) 0.0286(4) 0.0281(13) Uani 1 1 d . . . . .
O6 O 0.3614(4) -0.0683(2) 0.4605(3) 0.0334(10) Uani 1 1 d . . . . .
O7 O 0.4035(4) 0.0874(2) 0.4683(3) 0.0368(10) Uani 1 1 d . . . . .
C27 C 0.4873(7) -0.0456(3) 0.4978(4) 0.0286(13) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4 C14 1.253(7) . ?
O4 Dy1 2.264(4) 2 ?
O5 C14 1.255(7) . ?
O5 Dy1 2.275(4) 4_665 ?
Dy1 O4 2.264(4) 2_545 ?
Dy1 O5 2.275(4) 4_566 ?
Dy1 O6 2.360(4) . ?
Dy1 O1 2.367(5) . ?
Dy1 O7 2.370(4) . ?
Dy1 O2 2.471(5) . ?
Dy1 N2 2.534(5) . ?
Dy1 N1 2.588(5) . ?
C1 O2 1.252(8) . ?
C1 O1 1.253(8) . ?
C1 C2 1.507(9) . ?
C2 C7 1.380(9) . ?
C2 C3 1.393(9) . ?
C5 C6 1.367(10) . ?
C5 C4 1.376(10) . ?
C5 H5 0.9300 . ?
C3 C4 1.386(10) . ?
C3 H3 0.9300 . ?
C7 C6 1.373(9) . ?
C7 H7 0.9300 . ?
C4 O3 1.377(8) . ?
C6 H6 0.9300 . ?
N1 C24 1.331(9) . ?
N1 C25 1.347(8) . ?
N2 C15 1.335(9) . ?
N2 C26 1.348(8) . ?
C24 C23 1.401(10) . ?
C24 H24 0.9300 . ?
C15 C16 1.401(11) . ?
C15 H15 0.9300 . ?
C25 C21 1.414(9) . ?
C25 C26 1.428(9) . ?
C26 C18 1.411(9) . ?
O3 C8 1.380(8) . ?
C13 C12 1.388(9) . ?
C13 C8 1.393(9) . ?
C13 H13 0.9300 . ?
C8 C9 1.382(10) . ?
C9 C10 1.373(9) . ?
C9 H9 0.9300 . ?
C12 C11 1.402(9) . ?
C12 H12 0.9300 . ?
C17 C16 1.363(13) . ?
C17 C18 1.399(12) . ?
C17 H17 0.9300 . ?
C18 C19 1.409(11) . ?
C21 C22 1.391(11) . ?
C21 C20 1.429(12) . ?
C23 C22 1.332(12) . ?
C23 H23 0.9300 . ?
C22 H22 0.9300 . ?
C19 C20 1.347(12) . ?
C19 H19 0.9300 . ?
C16 H16 0.9300 . ?
C20 H20 0.9300 . ?
C11 C10 1.397(9) . ?
C11 C14 1.491(8) . ?
C10 H10 0.9300 . ?
O6 C27 1.245(7) . ?
O7 C27 1.250(7) 3_656 ?
C27 O7 1.250(7) 3_656 ?
C27 C27 1.555(11) 3_656 ?

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
C14 O4 Dy1 161.5(4) . 2 ?
C14 O5 Dy1 140.8(4) . 4_665 ?
O4 Dy1 O5 85.50(15) 2_545 4_566 ?
O4 Dy1 O6 75.45(15) 2_545 . ?
O5 Dy1 O6 107.03(15) 4_566 . ?
O4 Dy1 O1 80.31(16) 2_545 . ?
O5 Dy1 O1 149.67(15) 4_566 . ?
O6 Dy1 O1 95.19(16) . . ?
O4 Dy1 O7 132.26(16) 2_545 . ?
O5 Dy1 O7 76.92(15) 4_566 . ?
O6 Dy1 O7 68.25(13) . . ?
O1 Dy1 O7 131.68(16) . . ?
O4 Dy1 O2 124.08(15) 2_545 . ?
O5 Dy1 O2 150.00(15) 4_566 . ?
O6 Dy1 O2 79.07(16) . . ?
O1 Dy1 O2 53.45(16) . . ?
O7 Dy1 O2 78.48(16) . . ?
O4 Dy1 N2 145.80(16) 2_545 . ?
O5 Dy1 N2 86.89(16) 4_566 . ?
O6 Dy1 N2 138.44(16) . . ?
O1 Dy1 N2 89.96(17) . . ?
O7 Dy1 N2 77.69(16) . . ?
O2 Dy1 N2 71.23(16) . . ?
O4 Dy1 N1 81.93(16) 2_545 . ?
O5 Dy1 N1 74.71(15) 4_566 . ?
O6 Dy1 N1 157.03(16) . . ?
O1 Dy1 N1 76.84(16) . . ?
O7 Dy1 N1 132.77(17) . . ?
O2 Dy1 N1 111.27(16) . . ?
N2 Dy1 N1 63.90(17) . . ?
O2 C1 O1 120.8(6) . . ?
O2 C1 C2 121.3(6) . . ?
O1 C1 C2 117.9(6) . . ?
C1 O2 Dy1 89.9(4) . . ?
C7 C2 C3 119.7(6) . . ?
C7 C2 C1 120.9(6) . . ?
C3 C2 C1 119.3(6) . . ?
C1 O1 Dy1 94.8(4) . . ?
C6 C5 C4 119.0(7) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C4 C3 C2 119.1(6) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C6 C7 C2 119.7(6) . . ?
C6 C7 H7 120.1 . . ?
C2 C7 H7 120.1 . . ?
C5 C4 O3 116.7(7) . . ?
C5 C4 C3 120.9(7) . . ?
O3 C4 C3 122.3(7) . . ?
C5 C6 C7 121.5(7) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C24 N1 C25 118.4(6) . . ?
C24 N1 Dy1 123.0(5) . . ?
C25 N1 Dy1 118.4(4) . . ?
C15 N2 C26 118.8(6) . . ?
C15 N2 Dy1 120.5(5) . . ?
C26 N2 Dy1 120.6(4) . . ?
N1 C24 C23 122.6(7) . . ?
N1 C24 H24 118.7 . . ?
C23 C24 H24 118.7 . . ?
N2 C15 C16 122.5(7) . . ?
N2 C15 H15 118.8 . . ?
C16 C15 H15 118.8 . . ?
N1 C25 C21 121.8(6) . . ?
N1 C25 C26 118.6(6) . . ?
C21 C25 C26 119.6(6) . . ?
N2 C26 C18 122.4(6) . . ?
N2 C26 C25 118.2(5) . . ?
C18 C26 C25 119.4(6) . . ?
C4 O3 C8 121.3(5) . . ?
C12 C13 C8 120.2(6) . . ?
C12 C13 H13 119.9 . . ?
C8 C13 H13 119.9 . . ?
O3 C8 C9 116.2(6) . . ?
O3 C8 C13 123.6(7) . . ?
C9 C8 C13 120.1(6) . . ?
C10 C9 C8 120.0(6) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C13 C12 C11 119.7(6) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C16 C17 C18 120.6(7) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C17 C18 C19 123.1(8) . . ?
C17 C18 C26 117.1(7) . . ?
C19 C18 C26 119.8(8) . . ?
C22 C21 C25 117.3(7) . . ?
C22 C21 C20 124.1(7) . . ?
C25 C21 C20 118.6(7) . . ?
C22 C23 C24 118.9(8) . . ?
C22 C23 H23 120.5 . . ?
C24 C23 H23 120.5 . . ?
C23 C22 C21 120.9(7) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C20 C19 C18 120.9(8) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C17 C16 C15 118.6(8) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C19 C20 C21 121.6(8) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C10 C11 C12 119.0(6) . . ?
C10 C11 C14 120.5(6) . . ?
C12 C11 C14 120.5(6) . . ?
C9 C10 C11 121.0(6) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
O4 C14 O5 123.6(5) . . ?
O4 C14 C11 118.6(6) . . ?
O5 C14 C11 117.8(5) . . ?
C27 O6 Dy1 119.6(4) . . ?
C27 O7 Dy1 119.3(3) 3_656 . ?
O6 C27 O7 127.8(5) . 3_656 ?
O6 C27 C27 116.4(6) . 3_656 ?
O7 C27 C27 115.9(6) 3_656 3_656 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 O2 Dy1 -10.6(6) . . . . ?
C2 C1 O2 Dy1 166.2(5) . . . . ?
O2 C1 C2 C7 162.3(6) . . . . ?
O1 C1 C2 C7 -20.8(9) . . . . ?
O2 C1 C2 C3 -21.1(9) . . . . ?
O1 C1 C2 C3 155.8(6) . . . . ?
O2 C1 O1 Dy1 11.1(7) . . . . ?
C2 C1 O1 Dy1 -165.8(5) . . . . ?
C7 C2 C3 C4 2.0(10) . . . . ?
C1 C2 C3 C4 -174.7(6) . . . . ?
C3 C2 C7 C6 0.5(10) . . . . ?
C1 C2 C7 C6 177.1(6) . . . . ?
C6 C5 C4 O3 175.7(7) . . . . ?
C6 C5 C4 C3 -1.1(12) . . . . ?
C2 C3 C4 C5 -1.7(11) . . . . ?
C2 C3 C4 O3 -178.3(6) . . . . ?
C4 C5 C6 C7 3.6(12) . . . . ?
C2 C7 C6 C5 -3.3(11) . . . . ?
C25 N1 C24 C23 1.5(11) . . . . ?
Dy1 N1 C24 C23 176.9(6) . . . . ?
C26 N2 C15 C16 -1.1(11) . . . . ?
Dy1 N2 C15 C16 178.5(6) . . . . ?
C24 N1 C25 C21 0.3(9) . . . . ?
Dy1 N1 C25 C21 -175.3(5) . . . . ?
C24 N1 C25 C26 -178.9(6) . . . . ?
Dy1 N1 C25 C26 5.6(7) . . . . ?
C15 N2 C26 C18 -0.1(9) . . . . ?
Dy1 N2 C26 C18 -179.6(5) . . . . ?
C15 N2 C26 C25 179.1(6) . . . . ?
Dy1 N2 C26 C25 -0.5(7) . . . . ?
N1 C25 C26 N2 -3.5(9) . . . . ?
C21 C25 C26 N2 177.4(6) . . . . ?
N1 C25 C26 C18 175.7(6) . . . . ?
C21 C25 C26 C18 -3.5(9) . . . . ?
C5 C4 O3 C8 145.1(7) . . . . ?
C3 C4 O3 C8 -38.1(11) . . . . ?
C4 O3 C8 C9 147.3(7) . . . . ?
C4 O3 C8 C13 -36.8(11) . . . . ?
C12 C13 C8 O3 -176.7(7) . . . . ?
C12 C13 C8 C9 -0.9(11) . . . . ?
O3 C8 C9 C10 177.6(6) . . . . ?
C13 C8 C9 C10 1.4(10) . . . . ?
C8 C13 C12 C11 -0.4(11) . . . . ?
C16 C17 C18 C19 175.4(8) . . . . ?
C16 C17 C18 C26 -3.4(12) . . . . ?
N2 C26 C18 C17 2.2(10) . . . . ?
C25 C26 C18 C17 -176.9(6) . . . . ?
N2 C26 C18 C19 -176.6(7) . . . . ?
C25 C26 C18 C19 4.3(10) . . . . ?
N1 C25 C21 C22 -1.6(10) . . . . ?
C26 C25 C21 C22 177.6(6) . . . . ?
N1 C25 C21 C20 -178.8(6) . . . . ?
C26 C25 C21 C20 0.4(10) . . . . ?
N1 C24 C23 C22 -2.0(13) . . . . ?
C24 C23 C22 C21 0.6(13) . . . . ?
C25 C21 C22 C23 1.1(12) . . . . ?
C20 C21 C22 C23 178.1(8) . . . . ?
C17 C18 C19 C20 179.4(8) . . . . ?
C26 C18 C19 C20 -1.9(13) . . . . ?
C18 C17 C16 C15 2.4(13) . . . . ?
N2 C15 C16 C17 -0.1(12) . . . . ?
C18 C19 C20 C21 -1.4(14) . . . . ?
C22 C21 C20 C19 -174.9(9) . . . . ?
C25 C21 C20 C19 2.1(12) . . . . ?
C13 C12 C11 C10 1.1(10) . . . . ?
C13 C12 C11 C14 -179.6(6) . . . . ?
C8 C9 C10 C11 -0.7(11) . . . . ?
C12 C11 C10 C9 -0.5(10) . . . . ?
C14 C11 C10 C9 -179.8(6) . . . . ?
Dy1 O4 C14 O5 50.2(16) 2 . . . ?
Dy1 O4 C14 C11 -131.8(11) 2 . . . ?
Dy1 O5 C14 O4 -85.7(8) 4_665 . . . ?
Dy1 O5 C14 C11 96.3(7) 4_665 . . . ?
C10 C11 C14 O4 -166.4(6) . . . . ?
C12 C11 C14 O4 14.3(9) . . . . ?
C10 C11 C14 O5 11.8(9) . . . . ?
C12 C11 C14 O5 -167.5(6) . . . . ?
Dy1 O6 C27 O7 -174.2(5) . . . 3_656 ?
Dy1 O6 C27 C27 5.4(9) . . . 3_656 ?

_refine_diff_density_max         2.145
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.156

_shelxl_version_number           2013-4

