# Electronic Supplementary Material (ESI) for RSC Advances.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1528897'
_audit_update_record             
;
2017-01-21 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H13 Cl N2 O4 Y'
_chemical_formula_sum            'C17 H13 Cl N2 O4 Y'
_chemical_formula_weight         433.65

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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   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                   8.1640(4)
_cell_length_b                   12.4878(6)
_cell_length_c                   16.1848(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.013(2)
_cell_angle_gamma                90.00
_cell_volume                     1646.00(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2927
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             868
_exptl_absorpt_coefficient_mu    3.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6844
_exptl_absorpt_correction_T_max  0.7546
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_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 Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            134409
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0062
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.72
_diffrn_reflns_theta_max         25.10
_reflns_number_total             2927
_reflns_number_gt                2854
_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)+(0.0784P)²+4.6763P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.027(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2927
_refine_ls_number_parameters     227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1307
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_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
Y1 Y 0.51477(4) 0.37240(3) 0.43559(2) 0.0146(2) Uani 1 1 d . . .
Cl1 Cl 0.3807(2) 0.36234(11) 0.28332(9) 0.0498(4) Uani 1 1 d . . .
O4 O -0.2656(4) 0.4856(3) 0.4129(2) 0.0462(9) Uani 1 1 d . . .
O1 O 0.4009(4) 0.5410(3) 0.4308(2) 0.0428(8) Uani 1 1 d . . .
O3 O -0.2966(5) 0.6360(3) 0.4852(3) 0.0489(10) Uani 1 1 d . . .
O2 O 0.3220(5) 0.7038(3) 0.4512(2) 0.0470(9) Uani 1 1 d . . .
N1 N 0.4232(5) 0.1772(3) 0.4273(3) 0.0380(9) Uani 1 1 d . . .
N2 N 0.7141(5) 0.2467(3) 0.3721(3) 0.0400(10) Uani 1 1 d . . .
C1 C 0.2804(7) 0.1423(4) 0.4516(4) 0.0437(12) Uani 1 1 d . . .
H1A H 0.2110 0.1915 0.4745 0.052 Uiso 1 1 calc R . .
C2 C 0.2296(7) 0.0374(5) 0.4447(4) 0.0501(13) Uani 1 1 d . . .
H2A H 0.1282 0.0174 0.4626 0.060 Uiso 1 1 calc R . .
C3 C 0.3281(7) -0.0375(4) 0.4115(4) 0.0481(13) Uani 1 1 d . . .
H3A H 0.2950 -0.1086 0.4065 0.058 Uiso 1 1 calc R . .
C4 C 0.4796(7) -0.0046(4) 0.3854(3) 0.0417(11) Uani 1 1 d . . .
C5 C 0.5928(8) -0.0787(4) 0.3520(4) 0.0517(14) Uani 1 1 d . . .
H5A H 0.5661 -0.1510 0.3484 0.062 Uiso 1 1 calc R . .
C6 C 0.7379(7) -0.0443(4) 0.3259(4) 0.0498(13) Uani 1 1 d . . .
H6A H 0.8099 -0.0934 0.3048 0.060 Uiso 1 1 calc R . .
C7 C 0.7811(7) 0.0659(4) 0.3302(3) 0.0429(12) Uani 1 1 d . . .
C8 C 0.9270(7) 0.1042(5) 0.3005(4) 0.0496(13) Uani 1 1 d . . .
H8A H 0.9981 0.0576 0.2761 0.060 Uiso 1 1 calc R . .
C9 C 0.9640(7) 0.2101(5) 0.3076(4) 0.0522(14) Uani 1 1 d . . .
H9A H 1.0611 0.2365 0.2886 0.063 Uiso 1 1 calc R . .
C10 C 0.8543(7) 0.2789(5) 0.3438(4) 0.0463(13) Uani 1 1 d . . .
H10A H 0.8812 0.3511 0.3484 0.056 Uiso 1 1 calc R . .
C11 C 0.5222(6) 0.1042(4) 0.3936(3) 0.0364(11) Uani 1 1 d . . .
C12 C 0.6752(7) 0.1401(4) 0.3646(3) 0.0366(11) Uani 1 1 d . . .
C13 C 0.3143(6) 0.6210(3) 0.4080(3) 0.0322(11) Uani 1 1 d . . .
C14 C 0.1961(7) 0.6117(4) 0.3334(3) 0.0395(11) Uani 1 1 d . . .
H14A H 0.2461 0.5712 0.2907 0.047 Uiso 1 1 calc R . .
H14B H 0.1699 0.6826 0.3117 0.047 Uiso 1 1 calc R . .
C15 C 0.0375(6) 0.5555(4) 0.3562(3) 0.0407(11) Uani 1 1 d . . .
H15A H -0.0271 0.5363 0.3058 0.049 Uiso 1 1 calc R . .
H15B H 0.0659 0.4899 0.3860 0.049 Uiso 1 1 calc R . .
C16 C -0.0656(8) 0.6255(4) 0.4093(5) 0.0584(18) Uani 1 1 d . . .
H16A H -0.0336 0.6949 0.4237 0.070 Uiso 1 1 calc R . .
C17 C -0.2215(6) 0.5780(4) 0.4378(3) 0.0400(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
Y1 O3 2.269(4) 3_566 ?
Y1 O1 2.301(4) . ?
Y1 O4 2.333(3) 1_655 ?
Y1 O2 2.387(4) 3_666 ?
Y1 O1 2.472(4) 3_666 ?
Y1 N2 2.531(4) . ?
Y1 N1 2.550(4) . ?
Y1 Cl1 2.6287(15) . ?
Y1 C13 2.805(6) 3_666 ?
Y1 Y1 3.8252(6) 3_666 ?
O4 C17 1.266(6) . ?
O4 Y1 2.333(3) 1_455 ?
O1 C13 1.264(6) . ?
O1 Y1 2.472(4) 3_666 ?
O3 C17 1.247(6) . ?
O3 Y1 2.269(4) 3_566 ?
O2 C13 1.248(6) . ?
O2 Y1 2.387(4) 3_666 ?
N1 C1 1.330(7) . ?
N1 C11 1.359(7) . ?
N2 C10 1.324(7) . ?
N2 C12 1.371(6) . ?
C1 C2 1.377(8) . ?
C1 H1A 0.9300 . ?
C2 C3 1.367(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.397(8) . ?
C3 H3A 0.9300 . ?
C4 C11 1.406(7) . ?
C4 C5 1.440(8) . ?
C5 C6 1.355(9) . ?
C5 H5A 0.9300 . ?
C6 C7 1.421(8) . ?
C6 H6A 0.9300 . ?
C7 C8 1.399(8) . ?
C7 C12 1.409(7) . ?
C8 C9 1.360(8) . ?
C8 H8A 0.9300 . ?
C9 C10 1.399(8) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.436(8) . ?
C13 C14 1.496(8) . ?
C13 Y1 2.805(6) 3_666 ?
C14 C15 1.540(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.521(8) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.505(8) . ?
C16 H16A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Y1 O1 74.34(13) 3_566 . ?
O3 Y1 O4 139.43(13) 3_566 1_655 ?
O1 Y1 O4 75.71(13) . 1_655 ?
O3 Y1 O2 88.05(16) 3_566 3_666 ?
O1 Y1 O2 126.40(13) . 3_666 ?
O4 Y1 O2 88.20(14) 1_655 3_666 ?
O3 Y1 O1 73.00(14) 3_566 3_666 ?
O1 Y1 O1 73.51(14) . 3_666 ?
O4 Y1 O1 72.68(13) 1_655 3_666 ?
O2 Y1 O1 52.89(13) 3_666 3_666 ?
O3 Y1 N2 138.89(13) 3_566 . ?
O1 Y1 N2 145.48(14) . . ?
O4 Y1 N2 77.82(14) 1_655 . ?
O2 Y1 N2 73.98(14) 3_666 . ?
O1 Y1 N2 118.62(13) 3_666 . ?
O3 Y1 N1 75.30(13) 3_566 . ?
O1 Y1 N1 139.15(14) . . ?
O4 Y1 N1 142.84(13) 1_655 . ?
O2 Y1 N1 78.76(13) 3_666 . ?
O1 Y1 N1 121.78(13) 3_666 . ?
N2 Y1 N1 65.19(13) . . ?
O3 Y1 Cl1 103.64(13) 3_566 . ?
O1 Y1 Cl1 82.61(10) . . ?
O4 Y1 Cl1 98.95(11) 1_655 . ?
O2 Y1 Cl1 150.93(10) 3_666 . ?
O1 Y1 Cl1 155.95(9) 3_666 . ?
N2 Y1 Cl1 80.03(11) . . ?
N1 Y1 Cl1 78.69(10) . . ?
O3 Y1 C13 81.47(17) 3_566 3_666 ?
O1 Y1 C13 100.23(13) . 3_666 ?
O4 Y1 C13 77.59(14) 1_655 3_666 ?
O2 Y1 C13 26.27(12) 3_666 3_666 ?
O1 Y1 C13 26.76(12) 3_666 3_666 ?
N2 Y1 C13 95.26(14) . 3_666 ?
N1 Y1 C13 101.59(13) . 3_666 ?
Cl1 Y1 C13 174.72(11) . 3_666 ?
O3 Y1 Y1 69.43(9) 3_566 3_666 ?
O1 Y1 Y1 38.29(9) . 3_666 ?
O4 Y1 Y1 70.07(9) 1_655 3_666 ?
O2 Y1 Y1 88.11(9) 3_666 3_666 ?
O1 Y1 Y1 35.22(8) 3_666 3_666 ?
N2 Y1 Y1 143.63(10) . 3_666 ?
N1 Y1 Y1 142.69(10) . 3_666 ?
Cl1 Y1 Y1 120.85(3) . 3_666 ?
C13 Y1 Y1 61.96(9) 3_666 3_666 ?
C17 O4 Y1 135.0(3) . 1_455 ?
C13 O1 Y1 161.7(3) . . ?
C13 O1 Y1 91.5(3) . 3_666 ?
Y1 O1 Y1 106.49(14) . 3_666 ?
C17 O3 Y1 139.5(3) . 3_566 ?
C13 O2 Y1 95.9(3) . 3_666 ?
C1 N1 C11 117.2(4) . . ?
C1 N1 Y1 123.9(3) . . ?
C11 N1 Y1 118.8(3) . . ?
C10 N2 C12 117.7(5) . . ?
C10 N2 Y1 123.2(3) . . ?
C12 N2 Y1 119.1(3) . . ?
N1 C1 C2 123.6(5) . . ?
N1 C1 H1A 118.2 . . ?
C2 C1 H1A 118.2 . . ?
C3 C2 C1 120.0(5) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 118.4(5) . . ?
C2 C3 H3A 120.8 . . ?
C4 C3 H3A 120.8 . . ?
C3 C4 C11 118.3(5) . . ?
C3 C4 C5 122.0(5) . . ?
C11 C4 C5 119.7(5) . . ?
C6 C5 C4 120.8(5) . . ?
C6 C5 H5A 119.6 . . ?
C4 C5 H5A 119.6 . . ?
C5 C6 C7 120.7(5) . . ?
C5 C6 H6A 119.6 . . ?
C7 C6 H6A 119.6 . . ?
C8 C7 C12 118.1(5) . . ?
C8 C7 C6 121.9(5) . . ?
C12 C7 C6 120.0(5) . . ?
C9 C8 C7 119.6(5) . . ?
C9 C8 H8A 120.2 . . ?
C7 C8 H8A 120.2 . . ?
C8 C9 C10 119.1(5) . . ?
C8 C9 H9A 120.4 . . ?
C10 C9 H9A 120.4 . . ?
N2 C10 C9 123.5(5) . . ?
N2 C10 H10A 118.2 . . ?
C9 C10 H10A 118.2 . . ?
N1 C11 C4 122.4(5) . . ?
N1 C11 C12 118.5(4) . . ?
C4 C11 C12 119.1(5) . . ?
N2 C12 C7 121.9(5) . . ?
N2 C12 C11 118.4(5) . . ?
C7 C12 C11 119.7(5) . . ?
O2 C13 O1 119.1(5) . . ?
O2 C13 C14 121.3(4) . . ?
O1 C13 C14 119.4(4) . . ?
O2 C13 Y1 57.8(3) . 3_666 ?
O1 C13 Y1 61.7(3) . 3_666 ?
C14 C13 Y1 169.2(4) . 3_666 ?
C13 C14 C15 110.4(4) . . ?
C13 C14 H14A 109.6 . . ?
C15 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
C15 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
C16 C15 C14 112.3(4) . . ?
C16 C15 H15A 109.1 . . ?
C14 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
C14 C15 H15B 109.1 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 C15 117.3(5) . . ?
C17 C16 H16A 121.3 . . ?
C15 C16 H16A 121.3 . . ?
O3 C17 O4 125.7(5) . . ?
O3 C17 C16 114.9(5) . . ?
O4 C17 C16 119.3(5) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.125
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1528899'
_audit_update_record             
;
2017-01-21 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H34 Ce2 N4 O12'
_chemical_formula_sum            'C39 H34 Ce2 N4 O12'
_chemical_formula_weight         1030.94

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.8586(18)
_cell_length_b                   13.565(3)
_cell_length_c                   16.392(3)
_cell_angle_alpha                84.12(3)
_cell_angle_beta                 83.86(3)
_cell_angle_gamma                75.14(3)
_cell_volume                     1887.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(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          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
_exptl_absorpt_coefficient_mu    2.452
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.3286
_exptl_absorpt_correction_T_max  0.4627
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14486
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         18.03
_reflns_number_total             2610
_reflns_number_gt                2208
_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)+(0.0322P)²+1.3999P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2610
_refine_ls_number_parameters     514
_refine_ls_number_restraints     654
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0242
_refine_ls_wR_factor_ref         0.0582
_refine_ls_wR_factor_gt          0.0539
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      0.995
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.089761(9) 0.361479(6) 0.453845(5) 0.01986(3) Uani 1 1 d . . .
Ce2 Ce -0.139742(9) 0.141721(6) -0.024950(5) 0.02079(3) Uani 1 1 d . . .
O1 O 0.06335(11) 0.20465(7) 0.39439(6) 0.0365(4) Uani 1 1 d . . .
O2 O 0.20509(11) 0.29441(7) 0.31794(6) 0.0367(4) Uani 1 1 d . . .
O3 O 0.03841(11) 0.20265(7) 0.06271(6) 0.0367(4) Uani 1 1 d . . .
O4 O 0.10211(10) 0.03831(6) 0.05138(6) 0.0283(3) Uani 1 1 d . . .
O5 O 0.10466(10) 0.45270(7) 0.57098(6) 0.0256(3) Uani 1 1 d . . .
O6 O 0.12172(11) 0.57147(7) 0.64702(6) 0.0392(4) Uani 1 1 d . . .
O7 O 0.75253(10) 0.51700(7) 0.59717(6) 0.0326(4) Uani 1 1 d . . .
O8 O 0.84576(10) 0.36933(7) 0.53911(6) 0.0284(4) Uani 1 1 d . . .
O9 O -0.41236(10) 0.17995(7) -0.07008(6) 0.0351(4) Uani 1 1 d . . .
O10 O -0.22545(11) 0.16595(8) -0.17033(6) 0.0433(4) Uani 1 1 d . . .
O11 O -0.76388(11) -0.05464(7) -0.09824(6) 0.0346(4) Uani 1 1 d . . .
O12 O -0.90187(10) 0.10756(7) -0.11673(6) 0.0305(4) Uani 1 1 d . . .
N1 N 0.15931(13) 0.20248(8) 0.57236(7) 0.0305(5) Uani 1 1 d . . .
N2 N 0.38852(12) 0.25560(8) 0.47146(7) 0.0299(5) Uani 1 1 d . . .
N3 N -0.13837(14) 0.33330(9) -0.07785(8) 0.0366(5) Uani 1 1 d . . .
N4 N -0.30849(13) 0.29685(9) 0.06057(7) 0.0308(5) Uani 1 1 d . . .
C1 C 0.12617(16) 0.11815(10) 0.07701(9) 0.0237(4) Uani 1 1 d U . .
C2 C 0.26958(16) 0.10203(11) 0.12110(9) 0.0324(5) Uani 1 1 d U . .
H2A H 0.3561 0.1093 0.0813 0.039 Uiso 1 1 calc R . .
H2B H 0.2948 0.0325 0.1462 0.039 Uiso 1 1 calc R . .
C3 C 0.25559(17) 0.17432(10) 0.18649(9) 0.0292(4) Uani 1 1 d U . .
H3A H 0.3568 0.1630 0.2082 0.035 Uiso 1 1 calc R . .
H3B H 0.2286 0.2439 0.1615 0.035 Uiso 1 1 calc R . .
C4 C 0.13653(17) 0.16366(11) 0.25610(9) 0.0352(5) Uani 1 1 d U . .
H4A H 0.1561 0.0922 0.2764 0.042 Uiso 1 1 calc R . .
H4B H 0.0337 0.1829 0.2352 0.042 Uiso 1 1 calc R . .
C5 C 0.13346(16) 0.22640(11) 0.32728(9) 0.0285(5) Uani 1 1 d U . .
C6 C 0.17383(16) 0.48507(11) 0.62292(9) 0.0244(5) Uani 1 1 d U . .
C7 C 0.31997(15) 0.41712(11) 0.65360(9) 0.0302(5) Uani 1 1 d U . .
H7A H 0.3264 0.3468 0.6436 0.036 Uiso 1 1 calc R . .
H7B H 0.3188 0.4210 0.7124 0.036 Uiso 1 1 calc R . .
C8 C 0.45943(16) 0.44945(12) 0.61028(10) 0.0406(5) Uani 1 1 d U . .
H8A H 0.4501 0.5197 0.6215 0.049 Uiso 1 1 calc R . .
H8B H 0.4541 0.4488 0.5515 0.049 Uiso 1 1 calc R . .
C9 C 0.61954(15) 0.38724(11) 0.63138(10) 0.0307(5) Uani 1 1 d U . .
H9A H 0.6320 0.3171 0.6189 0.037 Uiso 1 1 calc R . .
H9B H 0.6269 0.3871 0.6900 0.037 Uiso 1 1 calc R . .
C10 C 0.75190(15) 0.42774(11) 0.58484(9) 0.0250(5) Uani 1 1 d U . .
C11 C -0.36724(16) 0.18033(10) -0.14534(9) 0.0249(5) Uani 1 1 d U . .
C12 C -0.48512(15) 0.19957(12) -0.20816(9) 0.0322(5) Uani 1 1 d U . .
H12A H -0.4405 0.1569 -0.2530 0.039 Uiso 1 1 calc R . .
H12B H -0.5015 0.2702 -0.2304 0.039 Uiso 1 1 calc R . .
C13 C -0.64357(16) 0.18003(10) -0.17812(9) 0.0294(4) Uani 1 1 d U . .
H13A H -0.6913 0.2236 -0.1342 0.035 Uiso 1 1 calc R . .
H13B H -0.7115 0.1975 -0.2228 0.035 Uiso 1 1 calc R . .
C14 C -0.62878(16) 0.06942(10) -0.14706(9) 0.0256(4) Uani 1 1 d U . .
H14A H -0.5749 0.0270 -0.1907 0.031 Uiso 1 1 calc R . .
H14B H -0.5625 0.0540 -0.1017 0.031 Uiso 1 1 calc R . .
C15 C -0.77604(16) 0.03890(10) -0.11899(8) 0.0246(5) Uani 1 1 d U . .
C16 C 0.04812(18) 0.17432(11) 0.62145(9) 0.0384(5) Uani 1 1 d U . .
H16A H -0.0537 0.2148 0.6193 0.046 Uiso 1 1 calc R . .
C17 C 0.07336(18) 0.08726(11) 0.67678(10) 0.0401(5) Uani 1 1 d U . .
H17A H -0.0088 0.0709 0.7111 0.048 Uiso 1 1 calc R . .
C18 C 0.21939(17) 0.02825(11) 0.67886(10) 0.0397(4) Uani 1 1 d U . .
H18A H 0.2384 -0.0308 0.7144 0.048 Uiso 1 1 calc R . .
C19 C 0.34234(17) 0.05306(11) 0.62949(9) 0.0362(4) Uani 1 1 d U . .
C20 C 0.50116(17) -0.00410(12) 0.63055(10) 0.0417(4) Uani 1 1 d U . .
H20A H 0.5261 -0.0641 0.6647 0.050 Uiso 1 1 calc R . .
C21 C 0.61452(19) 0.02703(11) 0.58339(9) 0.0439(4) Uani 1 1 d U . .
H21A H 0.7174 -0.0113 0.5864 0.053 Uiso 1 1 calc R . .
C22 C 0.58442(18) 0.11612(11) 0.52892(10) 0.0386(4) Uani 1 1 d U . .
C23 C 0.69974(18) 0.15055(11) 0.47744(10) 0.0431(4) Uani 1 1 d U . .
H23A H 0.8047 0.1168 0.4807 0.052 Uiso 1 1 calc R . .
C24 C 0.65992(18) 0.23146(11) 0.42371(10) 0.0439(5) Uani 1 1 d U . .
H24A H 0.7354 0.2539 0.3882 0.053 Uiso 1 1 calc R . .
C25 C 0.50102(17) 0.28155(11) 0.42242(10) 0.0399(5) Uani 1 1 d U . .
H25A H 0.4734 0.3371 0.3841 0.048 Uiso 1 1 calc R . .
C26 C 0.42876(17) 0.17343(11) 0.52547(9) 0.0340(4) Uani 1 1 d U . .
C27 C 0.30829(17) 0.14266(11) 0.57600(9) 0.0332(4) Uani 1 1 d U . .
C28 C -0.40318(18) 0.28185(12) 0.12581(10) 0.0445(5) Uani 1 1 d U . .
H28A H -0.4127 0.2156 0.1407 0.053 Uiso 1 1 calc R . .
C29 C -0.4902(2) 0.35983(12) 0.17406(11) 0.0543(5) Uani 1 1 d U . .
H29A H -0.5576 0.3457 0.2187 0.065 Uiso 1 1 calc R . .
C30 C -0.47416(19) 0.45476(12) 0.15467(11) 0.0528(4) Uani 1 1 d U . .
H30A H -0.5298 0.5076 0.1863 0.063 Uiso 1 1 calc R . .
C31 C -0.37424(19) 0.47470(12) 0.08715(11) 0.0465(4) Uani 1 1 d U . .
C32 C -0.3495(2) 0.57394(12) 0.06157(11) 0.0555(4) Uani 1 1 d U . .
H32A H -0.4007 0.6288 0.0922 0.067 Uiso 1 1 calc R . .
C33 C -0.2571(2) 0.58979(13) -0.00344(11) 0.0588(4) Uani 1 1 d U . .
H33A H -0.2425 0.6551 -0.0174 0.071 Uiso 1 1 calc R . .
C34 C -0.1802(2) 0.51086(12) -0.05216(12) 0.0555(4) Uani 1 1 d U . .
C35 C -0.0883(2) 0.52404(13) -0.12480(12) 0.0650(5) Uani 1 1 d U . .
H35A H -0.0673 0.5874 -0.1402 0.078 Uiso 1 1 calc R . .
C36 C -0.0301(2) 0.44730(13) -0.17240(12) 0.0688(5) Uani 1 1 d U . .
H36A H 0.0277 0.4577 -0.2219 0.083 Uiso 1 1 calc R . .
C37 C -0.0562(2) 0.35028(12) -0.14782(11) 0.0579(5) Uani 1 1 d U . .
H37A H -0.0148 0.2969 -0.1814 0.069 Uiso 1 1 calc R . .
C38 C -0.29359(18) 0.39369(11) 0.03978(10) 0.0418(4) Uani 1 1 d U . .
C39 C -0.19950(19) 0.41159(11) -0.03176(11) 0.0437(4) 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
Ce1 O5 2.4208(12) . ?
Ce1 O8 2.4298(12) 1_455 ?
Ce1 O7 2.4530(12) 2_666 ?
Ce1 O1 2.5019(12) . ?
Ce1 O2 2.5073(12) . ?
Ce1 O6 2.5595(13) 2_566 ?
Ce1 O5 2.6830(12) 2_566 ?
Ce1 N2 2.6981(13) . ?
Ce1 N1 2.7425(15) . ?
Ce1 C5 2.8382(17) . ?
Ce1 C6 2.9945(17) 2_566 ?
Ce1 Ce1 4.0654(13) 2_566 ?
Ce2 O11 2.4210(12) 2_455 ?
Ce2 O12 2.4254(12) 1_655 ?
Ce2 O4 2.4558(11) 2 ?
Ce2 O9 2.5119(11) . ?
Ce2 O10 2.5421(12) . ?
Ce2 O3 2.5760(13) . ?
Ce2 O4 2.6069(13) . ?
Ce2 N3 2.6566(14) . ?
Ce2 N4 2.6779(15) . ?
Ce2 C11 2.8858(17) . ?
Ce2 C1 2.9649(17) . ?
Ce2 Ce2 4.0606(14) 2 ?
O1 C5 1.2508(17) . ?
O2 C5 1.2360(19) . ?
O3 C1 1.2248(15) . ?
O4 C1 1.2750(18) . ?
O4 Ce2 2.4558(11) 2 ?
O5 C6 1.2725(19) . ?
O5 Ce1 2.6830(12) 2_566 ?
O6 C6 1.2334(17) . ?
O6 Ce1 2.5595(13) 2_566 ?
O7 C10 1.2493(18) . ?
O7 Ce1 2.4530(12) 2_666 ?
O8 C10 1.2376(16) . ?
O8 Ce1 2.4298(12) 1_655 ?
O9 C11 1.2555(17) . ?
O10 C11 1.2506(17) . ?
O11 C15 1.2597(17) . ?
O11 Ce2 2.4210(12) 2_455 ?
O12 C15 1.2559(15) . ?
O12 Ce2 2.4254(12) 1_455 ?
N1 C16 1.313(2) . ?
N1 C27 1.3644(18) . ?
N2 C25 1.309(2) . ?
N2 C26 1.3472(18) . ?
N3 C37 1.324(2) . ?
N3 C39 1.332(2) . ?
N4 C28 1.319(2) . ?
N4 C38 1.359(2) . ?
C1 C2 1.485(2) . ?
C2 C3 1.500(2) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.491(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.507(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C6 C7 1.4869(19) . ?
C6 Ce1 2.9945(17) 2_566 ?
C7 C8 1.500(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.5082(19) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.520(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 C12 1.501(2) . ?
C12 C13 1.516(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.511(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.481(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C16 C17 1.398(2) . ?
C16 H16A 0.9300 . ?
C17 C18 1.337(2) . ?
C17 H17A 0.9300 . ?
C18 C19 1.378(2) . ?
C18 H18A 0.9300 . ?
C19 C27 1.410(2) . ?
C19 C20 1.423(2) . ?
C20 C21 1.330(2) . ?
C20 H20A 0.9300 . ?
C21 C22 1.412(2) . ?
C21 H21A 0.9300 . ?
C22 C23 1.398(2) . ?
C22 C26 1.402(2) . ?
C23 C24 1.332(2) . ?
C23 H23A 0.9300 . ?
C24 C25 1.399(2) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9300 . ?
C26 C27 1.403(2) . ?
C28 C29 1.400(2) . ?
C28 H28A 0.9300 . ?
C29 C30 1.334(2) . ?
C29 H29A 0.9300 . ?
C30 C31 1.391(2) . ?
C30 H30A 0.9300 . ?
C31 C38 1.405(2) . ?
C31 C32 1.433(2) . ?
C32 C33 1.307(2) . ?
C32 H32A 0.9300 . ?
C33 C34 1.390(2) . ?
C33 H33A 0.9300 . ?
C34 C35 1.392(3) . ?
C34 C39 1.403(2) . ?
C35 C36 1.328(3) . ?
C35 H35A 0.9300 . ?
C36 C37 1.405(3) . ?
C36 H36A 0.9300 . ?
C37 H37A 0.9300 . ?
C38 C39 1.402(2) . ?

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 Ce1 O8 73.99(4) . 1_455 ?
O5 Ce1 O7 74.26(4) . 2_666 ?
O8 Ce1 O7 135.62(4) 1_455 2_666 ?
O5 Ce1 O1 150.76(3) . . ?
O8 Ce1 O1 90.33(4) 1_455 . ?
O7 Ce1 O1 130.51(4) 2_666 . ?
O5 Ce1 O2 150.03(3) . . ?
O8 Ce1 O2 135.89(4) 1_455 . ?
O7 Ce1 O2 78.99(4) 2_666 . ?
O1 Ce1 O2 51.67(4) . . ?
O5 Ce1 O6 122.17(4) . 2_566 ?
O8 Ce1 O6 76.10(4) 1_455 2_566 ?
O7 Ce1 O6 95.83(4) 2_666 2_566 ?
O1 Ce1 O6 75.64(4) . 2_566 ?
O2 Ce1 O6 73.44(4) . 2_566 ?
O5 Ce1 O5 74.51(4) . 2_566 ?
O8 Ce1 O5 70.54(4) 1_455 2_566 ?
O7 Ce1 O5 71.64(3) 2_666 2_566 ?
O1 Ce1 O5 123.94(4) . 2_566 ?
O2 Ce1 O5 109.59(4) . 2_566 ?
O6 Ce1 O5 49.05(4) 2_566 2_566 ?
O5 Ce1 N2 88.08(4) . . ?
O8 Ce1 N2 133.05(4) 1_455 . ?
O7 Ce1 N2 75.38(4) 2_666 . ?
O1 Ce1 N2 84.95(4) . . ?
O2 Ce1 N2 72.13(4) . . ?
O6 Ce1 N2 145.48(4) 2_566 . ?
O5 Ce1 N2 145.77(4) 2_566 . ?
O5 Ce1 N1 79.22(4) . . ?
O8 Ce1 N1 75.03(4) 1_455 . ?
O7 Ce1 N1 127.37(4) 2_666 . ?
O1 Ce1 N1 72.85(4) . . ?
O2 Ce1 N1 107.51(4) . . ?
O6 Ce1 N1 136.60(4) 2_566 . ?
O5 Ce1 N1 141.14(4) 2_566 . ?
N2 Ce1 N1 58.94(4) . . ?
O5 Ce1 C5 167.68(3) . . ?
O8 Ce1 C5 112.63(5) 1_455 . ?
O7 Ce1 C5 104.77(4) 2_666 . ?
O1 Ce1 C5 26.13(4) . . ?
O2 Ce1 C5 25.79(4) . . ?
O6 Ce1 C5 70.09(4) 2_566 . ?
O5 Ce1 C5 117.16(4) 2_566 . ?
N2 Ce1 C5 79.87(5) . . ?
N1 Ce1 C5 92.26(4) . . ?
O5 Ce1 C6 98.46(4) . 2_566 ?
O8 Ce1 C6 69.74(4) 1_455 2_566 ?
O7 Ce1 C6 85.24(4) 2_666 2_566 ?
O1 Ce1 C6 98.95(4) . 2_566 ?
O2 Ce1 C6 92.48(4) . 2_566 ?
O6 Ce1 C6 24.06(4) 2_566 2_566 ?
O5 Ce1 C6 25.14(4) 2_566 2_566 ?
N2 Ce1 C6 157.08(4) . 2_566 ?
N1 Ce1 C6 143.81(4) . 2_566 ?
C5 Ce1 C6 93.67(5) . 2_566 ?
O5 Ce1 Ce1 39.50(3) . 2_566 ?
O8 Ce1 Ce1 67.41(4) 1_455 2_566 ?
O7 Ce1 Ce1 68.32(3) 2_666 2_566 ?
O1 Ce1 Ce1 152.63(2) . 2_566 ?
O2 Ce1 Ce1 137.49(3) . 2_566 ?
O6 Ce1 Ce1 83.37(3) 2_566 2_566 ?
O5 Ce1 Ce1 35.02(2) 2_566 2_566 ?
N2 Ce1 Ce1 121.71(4) . 2_566 ?
N1 Ce1 Ce1 113.74(3) . 2_566 ?
C5 Ce1 Ce1 152.01(3) . 2_566 ?
C6 Ce1 Ce1 59.34(4) 2_566 2_566 ?
O11 Ce2 O12 134.94(4) 2_455 1_655 ?
O11 Ce2 O4 72.20(4) 2_455 2 ?
O12 Ce2 O4 76.68(4) 1_655 2 ?
O11 Ce2 O9 87.02(4) 2_455 . ?
O12 Ce2 O9 124.74(4) 1_655 . ?
O4 Ce2 O9 89.51(4) 2 . ?
O11 Ce2 O10 130.34(4) 2_455 . ?
O12 Ce2 O10 73.53(4) 1_655 . ?
O4 Ce2 O10 80.67(4) 2 . ?
O9 Ce2 O10 51.37(4) . . ?
O11 Ce2 O3 88.84(4) 2_455 . ?
O12 Ce2 O3 81.59(4) 1_655 . ?
O4 Ce2 O3 123.05(4) 2 . ?
O9 Ce2 O3 143.92(3) . . ?
O10 Ce2 O3 140.48(4) . . ?
O11 Ce2 O4 72.30(4) 2_455 . ?
O12 Ce2 O4 68.05(4) 1_655 . ?
O4 Ce2 O4 73.38(5) 2 . ?
O9 Ce2 O4 156.24(3) . . ?
O10 Ce2 O4 137.41(4) . . ?
O3 Ce2 O4 49.67(3) . . ?
O11 Ce2 N3 136.68(4) 2_455 . ?
O12 Ce2 N3 81.32(4) 1_655 . ?
O4 Ce2 N3 150.56(4) 2 . ?
O9 Ce2 N3 87.15(5) . . ?
O10 Ce2 N3 74.45(5) . . ?
O3 Ce2 N3 71.78(4) . . ?
O4 Ce2 N3 115.86(4) . . ?
O11 Ce2 N4 77.27(4) 2_455 . ?
O12 Ce2 N4 137.05(4) 1_655 . ?
O4 Ce2 N4 146.02(4) 2 . ?
O9 Ce2 N4 74.18(4) . . ?
O10 Ce2 N4 109.30(4) . . ?
O3 Ce2 N4 69.95(4) . . ?
O4 Ce2 N4 111.14(4) . . ?
N3 Ce2 N4 59.86(4) . . ?
O11 Ce2 C11 109.18(4) 2_455 . ?
O12 Ce2 C11 99.09(4) 1_655 . ?
O4 Ce2 C11 84.29(5) 2 . ?
O9 Ce2 C11 25.72(4) . . ?
O10 Ce2 C11 25.65(4) . . ?
O3 Ce2 C11 151.47(4) . . ?
O4 Ce2 C11 156.14(4) . . ?
N3 Ce2 C11 80.10(5) . . ?
N4 Ce2 C11 92.06(4) . . ?
O11 Ce2 C1 80.49(4) 2_455 . ?
O12 Ce2 C1 72.92(4) 1_655 . ?
O4 Ce2 C1 98.80(5) 2 . ?
O9 Ce2 C1 162.04(3) . . ?
O10 Ce2 C1 145.58(4) . . ?
O3 Ce2 C1 24.26(3) . . ?
O4 Ce2 C1 25.43(4) . . ?
N3 Ce2 C1 93.10(5) . . ?
N4 Ce2 C1 90.41(4) . . ?
C11 Ce2 C1 170.32(4) . . ?
O11 Ce2 Ce2 67.66(3) 2_455 2 ?
O12 Ce2 Ce2 67.70(4) 1_655 2 ?
O4 Ce2 Ce2 37.97(3) 2 2 ?
O9 Ce2 Ce2 125.62(3) . 2 ?
O10 Ce2 Ce2 112.00(4) . 2 ?
O3 Ce2 Ce2 85.09(3) . 2 ?
O4 Ce2 Ce2 35.42(3) . 2 ?
N3 Ce2 Ce2 143.77(3) . 2 ?
N4 Ce2 Ce2 137.14(3) . 2 ?
C11 Ce2 Ce2 121.80(4) . 2 ?
C1 Ce2 Ce2 60.84(4) . 2 ?
C5 O1 Ce1 92.12(9) . . ?
C5 O2 Ce1 92.23(9) . . ?
C1 O3 Ce2 95.96(10) . . ?
C1 O4 Ce2 160.13(8) . 2 ?
C1 O4 Ce2 93.18(7) . . ?
Ce2 O4 Ce2 106.62(5) 2 . ?
C6 O5 Ce1 155.38(8) . . ?
C6 O5 Ce1 91.25(8) . 2_566 ?
Ce1 O5 Ce1 105.49(4) . 2_566 ?
C6 O6 Ce1 98.15(9) . 2_566 ?
C10 O7 Ce1 136.72(9) . 2_666 ?
C10 O8 Ce1 139.65(10) . 1_655 ?
C11 O9 Ce2 94.02(9) . . ?
C11 O10 Ce2 92.72(9) . . ?
C15 O11 Ce2 131.67(9) . 2_455 ?
C15 O12 Ce2 135.12(9) . 1_455 ?
C16 N1 C27 117.54(12) . . ?
C16 N1 Ce1 121.09(9) . . ?
C27 N1 Ce1 120.95(9) . . ?
C25 N2 C26 117.49(12) . . ?
C25 N2 Ce1 118.84(9) . . ?
C26 N2 Ce1 123.58(9) . . ?
C37 N3 C39 118.15(14) . . ?
C37 N3 Ce2 118.78(10) . . ?
C39 N3 Ce2 122.45(10) . . ?
C28 N4 C38 117.77(13) . . ?
C28 N4 Ce2 121.68(10) . . ?
C38 N4 Ce2 120.49(9) . . ?
O3 C1 O4 121.12(14) . . ?
O3 C1 C2 123.07(14) . . ?
O4 C1 C2 115.75(11) . . ?
O3 C1 Ce2 59.79(8) . . ?
O4 C1 Ce2 61.39(7) . . ?
C2 C1 Ce2 174.38(9) . . ?
C1 C2 C3 114.21(11) . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
C3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
C4 C3 C2 114.13(14) . . ?
C4 C3 H3A 108.7 . . ?
C2 C3 H3A 108.7 . . ?
C4 C3 H3B 108.7 . . ?
C2 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 C5 115.15(14) . . ?
C3 C4 H4A 108.5 . . ?
C5 C4 H4A 108.5 . . ?
C3 C4 H4B 108.5 . . ?
C5 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
O2 C5 O1 122.75(14) . . ?
O2 C5 C4 118.82(13) . . ?
O1 C5 C4 118.37(14) . . ?
O2 C5 Ce1 61.98(8) . . ?
O1 C5 Ce1 61.75(8) . . ?
C4 C5 Ce1 172.33(9) . . ?
O6 C6 O5 120.82(12) . . ?
O6 C6 C7 120.40(14) . . ?
O5 C6 C7 118.77(13) . . ?
O6 C6 Ce1 57.79(7) . 2_566 ?
O5 C6 Ce1 63.61(7) . 2_566 ?
C7 C6 Ce1 171.63(10) . 2_566 ?
C6 C7 C8 109.64(12) . . ?
C6 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
C6 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?
C7 C8 C9 117.48(13) . . ?
C7 C8 H8A 107.9 . . ?
C9 C8 H8A 107.9 . . ?
C7 C8 H8B 107.9 . . ?
C9 C8 H8B 107.9 . . ?
H8A C8 H8B 107.2 . . ?
C8 C9 C10 112.97(12) . . ?
C8 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
O8 C10 O7 127.49(14) . . ?
O8 C10 C9 116.80(13) . . ?
O7 C10 C9 115.71(12) . . ?
O10 C11 O9 121.89(14) . . ?
O10 C11 C12 118.20(13) . . ?
O9 C11 C12 119.91(12) . . ?
O10 C11 Ce2 61.63(8) . . ?
O9 C11 Ce2 60.26(8) . . ?
C12 C11 Ce2 179.56(10) . . ?
C11 C12 C13 116.26(12) . . ?
C11 C12 H12A 108.2 . . ?
C13 C12 H12A 108.2 . . ?
C11 C12 H12B 108.2 . . ?
C13 C12 H12B 108.2 . . ?
H12A C12 H12B 107.4 . . ?
C14 C13 C12 111.41(11) . . ?
C14 C13 H13A 109.3 . . ?
C12 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
C12 C13 H13B 109.3 . . ?
H13A C13 H13B 108.0 . . ?
C15 C14 C13 116.98(11) . . ?
C15 C14 H14A 108.1 . . ?
C13 C14 H14A 108.1 . . ?
C15 C14 H14B 108.1 . . ?
C13 C14 H14B 108.1 . . ?
H14A C14 H14B 107.3 . . ?
O12 C15 O11 125.26(14) . . ?
O12 C15 C14 118.05(12) . . ?
O11 C15 C14 116.69(11) . . ?
N1 C16 C17 124.04(13) . . ?
N1 C16 H16A 118.0 . . ?
C17 C16 H16A 118.0 . . ?
C18 C17 C16 117.92(15) . . ?
C18 C17 H17A 121.0 . . ?
C16 C17 H17A 121.0 . . ?
C17 C18 C19 121.39(14) . . ?
C17 C18 H18A 119.3 . . ?
C19 C18 H18A 119.3 . . ?
C18 C19 C27 117.49(13) . . ?
C18 C19 C20 124.41(14) . . ?
C27 C19 C20 118.08(14) . . ?
C21 C20 C19 120.93(14) . . ?
C21 C20 H20A 119.5 . . ?
C19 C20 H20A 119.5 . . ?
C20 C21 C22 122.43(14) . . ?
C20 C21 H21A 118.8 . . ?
C22 C21 H21A 118.8 . . ?
C23 C22 C26 117.69(13) . . ?
C23 C22 C21 124.21(14) . . ?
C26 C22 C21 118.09(15) . . ?
C24 C23 C22 120.30(14) . . ?
C24 C23 H23A 119.8 . . ?
C22 C23 H23A 119.8 . . ?
C23 C24 C25 117.93(15) . . ?
C23 C24 H24A 121.0 . . ?
C25 C24 H24A 121.0 . . ?
N2 C25 C24 124.53(14) . . ?
N2 C25 H25A 117.7 . . ?
C24 C25 H25A 117.7 . . ?
N2 C26 C22 121.91(14) . . ?
N2 C26 C27 117.86(12) . . ?
C22 C26 C27 120.14(13) . . ?
N1 C27 C26 118.09(13) . . ?
N1 C27 C19 121.60(14) . . ?
C26 C27 C19 120.31(13) . . ?
N4 C28 C29 123.89(15) . . ?
N4 C28 H28A 118.1 . . ?
C29 C28 H28A 118.1 . . ?
C30 C29 C28 118.59(16) . . ?
C30 C29 H29A 120.7 . . ?
C28 C29 H29A 120.7 . . ?
C29 C30 C31 119.94(15) . . ?
C29 C30 H30A 120.0 . . ?
C31 C30 H30A 120.0 . . ?
C30 C31 C38 118.75(15) . . ?
C30 C31 C32 123.98(15) . . ?
C38 C31 C32 117.27(15) . . ?
C33 C32 C31 122.01(16) . . ?
C33 C32 H32A 119.0 . . ?
C31 C32 H32A 119.0 . . ?
C32 C33 C34 121.26(17) . . ?
C32 C33 H33A 119.4 . . ?
C34 C33 H33A 119.4 . . ?
C33 C34 C35 123.99(17) . . ?
C33 C34 C39 120.24(16) . . ?
C35 C34 C39 115.68(16) . . ?
C36 C35 C34 120.86(18) . . ?
C36 C35 H35A 119.6 . . ?
C34 C35 H35A 119.6 . . ?
C35 C36 C37 119.83(18) . . ?
C35 C36 H36A 120.1 . . ?
C37 C36 H36A 120.1 . . ?
N3 C37 C36 121.39(16) . . ?
N3 C37 H37A 119.3 . . ?
C36 C37 H37A 119.3 . . ?
N4 C38 C39 118.34(14) . . ?
N4 C38 C31 121.03(14) . . ?
C39 C38 C31 120.61(15) . . ?
N3 C39 C38 117.43(15) . . ?
N3 C39 C34 124.02(15) . . ?
C38 C39 C34 118.51(15) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        18.03
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.068
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1528902'
_audit_update_record             
;
2017-01-21 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H24 La2 O15, 5(H2 O)'
_chemical_formula_sum            'C15 H34 La2 O20'
_chemical_formula_weight         812.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.076(2)
_cell_length_b                   9.867(3)
_cell_length_c                   16.303(4)
_cell_angle_alpha                103.349(16)
_cell_angle_beta                 104.110(9)
_cell_angle_gamma                98.526(10)
_cell_volume                     1345.0(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4781
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.006
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             796
_exptl_absorpt_coefficient_mu    3.219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6987
_exptl_absorpt_correction_T_max  0.7828
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_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 Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            49759
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4781
_reflns_number_gt                4548
_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)+(0.0415P)²+2.7318P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0081(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4781
_refine_ls_number_parameters     342
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0791
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_restrained_S_all      1.180
_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
La1 La 0.69213(2) 0.45144(2) 0.598112(12) 0.01385(10) Uani 1 1 d . . .
La2 La 0.84842(2) 0.42670(2) 0.864327(12) 0.01506(10) Uani 1 1 d . . .
O1W O 1.0202(4) 0.6711(4) 0.8933(2) 0.0401(8) Uani 1 1 d . . .
H1WB H 1.0711 0.6683 0.8558 0.048 Uiso 1 1 d R . .
H1WC H 1.0848 0.6945 0.9444 0.048 Uiso 1 1 d R . .
O1 O 0.6981(4) 0.2153(3) 0.7428(2) 0.0414(8) Uani 1 1 d . . .
O2W O 0.7914(4) 0.2230(3) 0.5464(2) 0.0323(7) Uani 1 1 d . . .
H2WB H 0.8546 0.2074 0.5893 0.039 Uiso 1 1 d R . .
H2WC H 0.8363 0.2300 0.5071 0.039 Uiso 1 1 d R . .
O2 O 0.5332(4) 0.2580(3) 0.6325(2) 0.0353(7) Uani 1 1 d . . .
O3 O 0.7621(3) -0.2747(3) 0.64299(18) 0.0273(6) Uani 1 1 d . . .
O3W O 0.7649(4) 0.4550(4) 0.4585(2) 0.0331(7) Uani 1 1 d . . .
O4 O 0.5595(3) -0.3580(3) 0.52672(16) 0.0202(5) Uani 1 1 d . . .
O4W O 0.8414(6) -0.0232(6) 0.9405(4) 0.0929(16) Uani 1 1 d . . .
H4WC H 0.8180 0.0566 0.9390 0.111 Uiso 1 1 d R . .
H4WD H 0.8795 -0.0506 0.8984 0.111 Uiso 1 1 d R . .
O5 O 0.7584(3) 0.2440(3) 0.94335(19) 0.0269(6) Uani 1 1 d . . .
O5W O 0.9728(6) -0.1267(5) 0.8024(3) 0.0757(14) Uani 1 1 d . . .
H5WC H 0.9078 -0.1703 0.7526 0.091 Uiso 1 1 d R . .
H5WD H 0.9895 -0.1869 0.8315 0.091 Uiso 1 1 d R . .
O6 O 0.5833(3) 0.3571(3) 0.8898(2) 0.0324(7) Uani 1 1 d . . .
O6W O 0.1998(5) 0.2194(5) 0.5774(3) 0.0682(12) Uani 1 1 d . . .
H6WA H 0.2923 0.2672 0.5902 0.082 Uiso 1 1 d R . .
H6WD H 0.1827 0.1454 0.5346 0.082 Uiso 1 1 d R . .
O7 O 0.1082(3) 0.4269(3) 0.97591(18) 0.0262(6) Uani 1 1 d . . .
O7W O 0.0079(5) 0.1065(4) 0.6634(2) 0.0508(9) Uani 1 1 d . . .
H7WC H 0.0246 0.1556 0.7163 0.061 Uiso 1 1 d R . .
H7WD H 0.0706 0.1473 0.6409 0.061 Uiso 1 1 d R . .
O8 O 0.0446(3) 0.2608(3) 0.85126(18) 0.0328(7) Uani 1 1 d . . .
O8W O 0.9469(5) 0.1772(4) 0.4147(3) 0.0564(10) Uani 1 1 d . . .
H8WC H 0.9586 0.2546 0.4001 0.068 Uiso 1 1 d R . .
H8WD H 1.0186 0.1867 0.4616 0.068 Uiso 1 1 d R . .
O9 O 0.6818(3) 0.5521(3) 0.7778(2) 0.0284(6) Uani 1 1 d . . .
O10 O 0.4860(3) 0.5471(3) 0.66773(17) 0.0234(6) Uani 1 1 d . . .
O11 O -0.0758(3) 0.4445(3) 0.72570(18) 0.0267(6) Uani 1 1 d . . .
O12 O 0.0021(3) 0.5417(3) 0.63185(19) 0.0282(6) Uani 1 1 d . . .
C1 C 0.5718(4) 0.1837(4) 0.6833(2) 0.0202(8) Uani 1 1 d . . .
C2 C 0.4583(5) 0.0484(4) 0.6722(3) 0.0319(9) Uani 1 1 d . . .
H2A H 0.3774 0.0275 0.6169 0.038 Uiso 1 1 calc R . .
H2B H 0.4095 0.0631 0.7193 0.038 Uiso 1 1 calc R . .
C3 C 0.5334(6) -0.0791(4) 0.6728(3) 0.0331(10) Uani 1 1 d . . .
H3A H 0.6093 -0.0614 0.7296 0.040 Uiso 1 1 calc R . .
H3B H 0.4543 -0.1626 0.6649 0.040 Uiso 1 1 calc R . .
C4 C 0.6130(5) -0.1086(4) 0.6010(3) 0.0257(8) Uani 1 1 d . . .
H4A H 0.5459 -0.1027 0.5463 0.031 Uiso 1 1 calc R . .
H4B H 0.7087 -0.0375 0.6168 0.031 Uiso 1 1 calc R . .
C5 C 0.6486(4) -0.2545(4) 0.5888(2) 0.0182(7) Uani 1 1 d . . .
C6 C 0.6177(4) 0.2572(4) 0.9198(2) 0.0222(8) Uani 1 1 d . . .
C7 C 0.4925(5) 0.1436(4) 0.9256(3) 0.0321(10) Uani 1 1 d . . .
H7A H 0.5125 0.1417 0.9865 0.039 Uiso 1 1 calc R . .
H7B H 0.5005 0.0517 0.8917 0.039 Uiso 1 1 calc R . .
C8 C 0.3257(5) 0.1624(4) 0.8929(3) 0.0309(9) Uani 1 1 d . . .
H8A H 0.3114 0.1844 0.8369 0.037 Uiso 1 1 calc R . .
H8B H 0.2535 0.0734 0.8835 0.037 Uiso 1 1 calc R . .
C9 C 0.2889(5) 0.2800(5) 0.9575(3) 0.0282(9) Uani 1 1 d . . .
H9A H 0.2874 0.2497 1.0099 0.034 Uiso 1 1 calc R . .
H9B H 0.3726 0.3636 0.9747 0.034 Uiso 1 1 calc R . .
C10 C 0.1385(4) 0.3222(4) 0.9249(2) 0.0193(7) Uani 1 1 d . . .
C11 C 0.5500(4) 0.5787(4) 0.7489(2) 0.0176(7) Uani 1 1 d . . .
C12 C 0.4742(5) 0.6530(5) 0.8133(3) 0.0271(9) Uani 1 1 d . . .
H12A H 0.5339 0.7501 0.8404 0.032 Uiso 1 1 calc R . .
H12B H 0.4795 0.6056 0.8595 0.032 Uiso 1 1 calc R . .
C13 C 0.3051(4) 0.6579(4) 0.7745(3) 0.0257(8) Uani 1 1 d . . .
H13A H 0.2953 0.6926 0.7228 0.031 Uiso 1 1 calc R . .
H13B H 0.2725 0.7233 0.8173 0.031 Uiso 1 1 calc R . .
C14 C 0.1998(4) 0.5092(5) 0.7490(3) 0.0281(9) Uani 1 1 d . . .
H14A H 0.2422 0.4420 0.7129 0.034 Uiso 1 1 calc R . .
H14B H 0.2011 0.4804 0.8021 0.034 Uiso 1 1 calc R . .
C15 C 0.0342(4) 0.5010(4) 0.6998(2) 0.0202(8) Uani 1 1 d . . .
H3WB H 0.681(7) 0.445(6) 0.411(4) 0.047(15) Uiso 1 1 d . . .
H3WA H 0.837(7) 0.448(6) 0.446(3) 0.035(15) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O2 2.472(3) . ?
La1 O3W 2.527(3) . ?
La1 O4 2.540(3) 2_656 ?
La1 O3 2.568(3) 1_565 ?
La1 O2W 2.588(3) . ?
La1 O11 2.596(3) 1_655 ?
La1 O10 2.597(3) . ?
La1 O12 2.699(3) 1_655 ?
La1 O4 2.709(3) 1_565 ?
La1 O9 2.897(3) . ?
La1 C5 3.019(4) 1_565 ?
La1 C15 3.048(4) 1_655 ?
La2 O1 2.463(3) . ?
La2 O9 2.476(3) . ?
La2 O1W 2.543(3) . ?
La2 O11 2.553(3) 1_655 ?
La2 O6 2.562(3) . ?
La2 O7 2.573(3) 2_667 ?
La2 O5 2.593(3) . ?
La2 O7 2.603(3) 1_655 ?
La2 O8 2.605(3) 1_655 ?
La2 C6 2.930(4) . ?
La2 C10 2.996(4) 1_655 ?
O1W H1WB 0.8501 . ?
O1W H1WC 0.8500 . ?
O1 C1 1.251(5) . ?
O2W H2WB 0.8500 . ?
O2W H2WC 0.8499 . ?
O2 C1 1.249(5) . ?
O3 C5 1.257(5) . ?
O3 La1 2.568(3) 1_545 ?
O3W H3WB 0.92(6) . ?
O3W H3WA 0.74(6) . ?
O4 C5 1.265(4) . ?
O4 La1 2.540(3) 2_656 ?
O4 La1 2.709(3) 1_545 ?
O4W H4WC 0.8500 . ?
O4W H4WD 0.8500 . ?
O5 C6 1.276(5) . ?
O5W H5WC 0.8500 . ?
O5W H5WD 0.8500 . ?
O6 C6 1.244(5) . ?
O6W H6WA 0.8499 . ?
O6W H6WD 0.8502 . ?
O7 C10 1.278(5) . ?
O7 La2 2.573(3) 2_667 ?
O7 La2 2.603(3) 1_455 ?
O7W H7WC 0.8500 . ?
O7W H7WD 0.8499 . ?
O8 C10 1.244(5) . ?
O8 La2 2.605(3) 1_455 ?
O8W H8WC 0.8500 . ?
O8W H8WD 0.8500 . ?
O9 C11 1.264(5) . ?
O10 C11 1.252(5) . ?
O11 C15 1.278(5) . ?
O11 La2 2.553(3) 1_455 ?
O11 La1 2.596(3) 1_455 ?
O12 C15 1.248(5) . ?
O12 La1 2.699(3) 1_455 ?
C1 C2 1.505(6) . ?
C2 C3 1.517(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.515(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.501(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 La1 3.019(4) 1_545 ?
C6 C7 1.510(6) . ?
C7 C8 1.532(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.513(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.496(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 La2 2.996(4) 1_455 ?
C11 C12 1.503(5) . ?
C12 C13 1.523(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.532(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.502(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 La1 3.048(4) 1_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 La1 O3W 129.84(12) . . ?
O2 La1 O4 72.50(10) . 2_656 ?
O3W La1 O4 73.83(10) . 2_656 ?
O2 La1 O3 138.62(10) . 1_565 ?
O3W La1 O3 87.97(11) . 1_565 ?
O4 La1 O3 110.46(8) 2_656 1_565 ?
O2 La1 O2W 73.62(10) . . ?
O3W La1 O2W 71.20(11) . . ?
O4 La1 O2W 91.44(9) 2_656 . ?
O3 La1 O2W 144.49(10) 1_565 . ?
O2 La1 O11 88.12(10) . 1_655 ?
O3W La1 O11 113.07(10) . 1_655 ?
O4 La1 O11 157.73(9) 2_656 1_655 ?
O3 La1 O11 91.27(9) 1_565 1_655 ?
O2W La1 O11 72.18(10) . 1_655 ?
O2 La1 O10 69.60(10) . . ?
O3W La1 O10 134.54(10) . . ?
O4 La1 O10 76.45(9) 2_656 . ?
O3 La1 O10 71.23(10) 1_565 . ?
O2W La1 O10 143.19(10) . . ?
O11 La1 O10 107.50(9) 1_655 . ?
O2 La1 O12 132.71(10) . 1_655 ?
O3W La1 O12 68.76(10) . 1_655 ?
O4 La1 O12 142.54(9) 2_656 1_655 ?
O3 La1 O12 70.60(9) 1_565 1_655 ?
O2W La1 O12 75.06(10) . 1_655 ?
O11 La1 O12 48.63(9) 1_655 1_655 ?
O10 La1 O12 133.50(10) . 1_655 ?
O2 La1 O4 120.97(10) . 1_565 ?
O3W La1 O4 70.70(10) . 1_565 ?
O4 La1 O4 61.84(9) 2_656 1_565 ?
O3 La1 O4 48.88(8) 1_565 1_565 ?
O2W La1 O4 138.20(9) . 1_565 ?
O11 La1 O4 140.13(9) 1_655 1_565 ?
O10 La1 O4 65.13(8) . 1_565 ?
O12 La1 O4 106.01(8) 1_655 1_565 ?
O2 La1 O9 71.50(10) . . ?
O3W La1 O9 158.64(11) . . ?
O4 La1 O9 119.87(8) 2_656 . ?
O3 La1 O9 72.15(9) 1_565 . ?
O2W La1 O9 121.36(9) . . ?
O11 La1 O9 61.15(8) 1_655 . ?
O10 La1 O9 46.39(8) . . ?
O12 La1 O9 96.56(8) 1_655 . ?
O4 La1 O9 100.26(8) 1_565 . ?
O2 La1 C5 131.93(10) . 1_565 ?
O3W La1 C5 80.67(11) . 1_565 ?
O4 La1 C5 86.15(9) 2_656 1_565 ?
O3 La1 C5 24.32(9) 1_565 1_565 ?
O2W La1 C5 151.28(10) . 1_565 ?
O11 La1 C5 115.50(10) 1_655 1_565 ?
O10 La1 C5 63.64(9) . 1_565 ?
O12 La1 C5 89.65(9) 1_655 1_565 ?
O4 La1 C5 24.77(9) 1_565 1_565 ?
O9 La1 C5 83.92(9) . 1_565 ?
O2 La1 C15 110.77(11) . 1_655 ?
O3W La1 C15 90.54(10) . 1_655 ?
O4 La1 C15 160.09(9) 2_656 1_655 ?
O3 La1 C15 80.53(9) 1_565 1_655 ?
O2W La1 C15 71.52(10) . 1_655 ?
O11 La1 C15 24.54(10) 1_655 1_655 ?
O10 La1 C15 123.38(9) . 1_655 ?
O12 La1 C15 24.10(9) 1_655 1_655 ?
O4 La1 C15 125.08(9) 1_565 1_655 ?
O9 La1 C15 78.82(9) . 1_655 ?
C5 La1 C15 103.74(10) 1_565 1_655 ?
O1 La2 O9 82.98(11) . . ?
O1 La2 O1W 141.23(12) . . ?
O9 La2 O1W 75.50(10) . . ?
O1 La2 O11 71.53(11) . 1_655 ?
O9 La2 O11 67.82(10) . 1_655 ?
O1W La2 O11 70.58(11) . 1_655 ?
O1 La2 O6 72.75(11) . . ?
O9 La2 O6 76.59(10) . . ?
O1W La2 O6 130.46(11) . . ?
O11 La2 O6 131.73(9) 1_655 . ?
O1 La2 O7 147.16(11) . 2_667 ?
O9 La2 O7 102.78(10) . 2_667 ?
O1W La2 O7 70.24(10) . 2_667 ?
O11 La2 O7 140.82(10) 1_655 2_667 ?
O6 La2 O7 77.19(10) . 2_667 ?
O1 La2 O5 76.09(11) . . ?
O9 La2 O5 126.61(9) . . ?
O1W La2 O5 142.29(10) . . ?
O11 La2 O5 142.39(10) 1_655 . ?
O6 La2 O5 50.46(9) . . ?
O7 La2 O5 74.70(10) 2_667 . ?
O1 La2 O7 122.81(10) . 1_655 ?
O9 La2 O7 150.33(10) . 1_655 ?
O1W La2 O7 74.93(10) . 1_655 ?
O11 La2 O7 104.20(9) 1_655 1_655 ?
O6 La2 O7 122.27(9) . 1_655 ?
O7 La2 O7 64.48(10) 2_667 1_655 ?
O5 La2 O7 77.84(9) . 1_655 ?
O1 La2 O8 75.87(10) . 1_655 ?
O9 La2 O8 141.55(10) . 1_655 ?
O1W La2 O8 101.85(11) . 1_655 ?
O11 La2 O8 75.10(10) 1_655 1_655 ?
O6 La2 O8 125.05(10) . 1_655 ?
O7 La2 O8 112.44(9) 2_667 1_655 ?
O5 La2 O8 78.94(10) . 1_655 ?
O7 La2 O8 49.54(9) 1_655 1_655 ?
O1 La2 C6 69.50(12) . . ?
O9 La2 C6 100.82(10) . . ?
O1W La2 C6 145.72(11) . . ?
O11 La2 C6 140.47(10) 1_655 . ?
O6 La2 C6 25.04(10) . . ?
O7 La2 C6 77.67(10) 2_667 . ?
O5 La2 C6 25.79(10) . . ?
O7 La2 C6 102.09(10) 1_655 . ?
O8 La2 C6 101.26(11) 1_655 . ?
O1 La2 C10 99.26(11) . 1_655 ?
O9 La2 C10 154.82(10) . 1_655 ?
O1W La2 C10 88.01(11) . 1_655 ?
O11 La2 C10 88.95(9) 1_655 1_655 ?
O6 La2 C10 128.19(9) . 1_655 ?
O7 La2 C10 88.95(9) 2_667 1_655 ?
O5 La2 C10 77.77(9) . 1_655 ?
O7 La2 C10 25.14(9) 1_655 1_655 ?
O8 La2 C10 24.41(9) 1_655 1_655 ?
C6 La2 C10 103.44(10) . 1_655 ?
La2 O1W H1WB 109.6 . . ?
La2 O1W H1WC 109.7 . . ?
H1WB O1W H1WC 108.2 . . ?
C1 O1 La2 136.5(3) . . ?
La1 O2W H2WB 110.9 . . ?
La1 O2W H2WC 110.9 . . ?
H2WB O2W H2WC 109.0 . . ?
C1 O2 La1 130.4(3) . . ?
C5 O3 La1 98.4(2) . 1_545 ?
La1 O3W H3WB 114(3) . . ?
La1 O3W H3WA 132(4) . . ?
H3WB O3W H3WA 113(5) . . ?
C5 O4 La1 148.2(2) . 2_656 ?
C5 O4 La1 91.5(2) . 1_545 ?
La1 O4 La1 118.16(9) 2_656 1_545 ?
H4WC O4W H4WD 108.5 . . ?
C6 O5 La2 92.0(2) . . ?
H5WC O5W H5WD 108.3 . . ?
C6 O6 La2 94.3(2) . . ?
H6WA O6W H6WD 110.8 . . ?
C10 O7 La2 146.6(2) . 2_667 ?
C10 O7 La2 94.9(2) . 1_455 ?
La2 O7 La2 115.52(10) 2_667 1_455 ?
H7WC O7W H7WD 108.6 . . ?
C10 O8 La2 95.7(2) . 1_455 ?
H8WC O8W H8WD 108.3 . . ?
C11 O9 La2 150.0(3) . . ?
C11 O9 La1 89.2(2) . . ?
La2 O9 La1 106.09(10) . . ?
C11 O10 La1 104.0(2) . . ?
C15 O11 La2 142.4(2) . 1_455 ?
C15 O11 La1 97.9(2) . 1_455 ?
La2 O11 La1 113.29(10) 1_455 1_455 ?
C15 O12 La1 93.8(2) . 1_455 ?
O2 C1 O1 124.1(4) . . ?
O2 C1 C2 117.6(4) . . ?
O1 C1 C2 118.3(4) . . ?
C1 C2 C3 113.2(4) . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 . . ?
C3 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C4 C3 C2 112.1(3) . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C5 C4 C3 110.0(3) . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
O3 C5 O4 120.2(3) . . ?
O3 C5 C4 119.8(3) . . ?
O4 C5 C4 119.8(3) . . ?
O3 C5 La1 57.30(18) . 1_545 ?
O4 C5 La1 63.76(19) . 1_545 ?
C4 C5 La1 167.4(3) . 1_545 ?
O6 C6 O5 121.4(4) . . ?
O6 C6 C7 120.7(3) . . ?
O5 C6 C7 117.8(3) . . ?
O6 C6 La2 60.7(2) . . ?
O5 C6 La2 62.2(2) . . ?
C7 C6 La2 165.3(3) . . ?
C6 C7 C8 115.2(4) . . ?
C6 C7 H7A 108.5 . . ?
C8 C7 H7A 108.5 . . ?
C6 C7 H7B 108.5 . . ?
C8 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C9 C8 C7 112.1(4) . . ?
C9 C8 H8A 109.2 . . ?
C7 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
C7 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C10 C9 C8 115.8(3) . . ?
C10 C9 H9A 108.3 . . ?
C8 C9 H9A 108.3 . . ?
C10 C9 H9B 108.3 . . ?
C8 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
O8 C10 O7 119.8(3) . . ?
O8 C10 C9 122.8(3) . . ?
O7 C10 C9 117.4(3) . . ?
O8 C10 La2 59.89(19) . 1_455 ?
O7 C10 La2 59.94(19) . 1_455 ?
C9 C10 La2 176.3(3) . 1_455 ?
O10 C11 O9 120.3(3) . . ?
O10 C11 C12 120.7(3) . . ?
O9 C11 C12 119.0(3) . . ?
C11 C12 C13 115.4(3) . . ?
C11 C12 H12A 108.4 . . ?
C13 C12 H12A 108.4 . . ?
C11 C12 H12B 108.4 . . ?
C13 C12 H12B 108.4 . . ?
H12A C12 H12B 107.5 . . ?
C12 C13 C14 110.6(3) . . ?
C12 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C15 C14 C13 113.9(3) . . ?
C15 C14 H14A 108.8 . . ?
C13 C14 H14A 108.8 . . ?
C15 C14 H14B 108.8 . . ?
C13 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
O12 C15 O11 119.5(3) . . ?
O12 C15 C14 121.2(3) . . ?
O11 C15 C14 119.1(3) . . ?
O12 C15 La1 62.07(19) . 1_455 ?
O11 C15 La1 57.51(19) . 1_455 ?
C14 C15 La1 174.1(3) . 1_455 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.400
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.125
####################################################################### 
# 
# 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 1528901'
_audit_update_record             
;
2017-01-21 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H34 Ho2 N4 O12'
_chemical_formula_sum            'C39 H34 Ho2 N4 O12'
_chemical_formula_weight         1080.56

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.7671(5)
_cell_length_b                   13.4002(7)
_cell_length_c                   16.4124(11)
_cell_angle_alpha                83.911(2)
_cell_angle_beta                 84.424(2)
_cell_angle_gamma                75.048(2)
_cell_volume                     1847.46(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    6519
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1052
_exptl_absorpt_coefficient_mu    4.324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1518
_exptl_absorpt_correction_T_max  0.2892
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      297(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 Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17479
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0857
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         25.10
_reflns_number_total             6519
_reflns_number_gt                4419
_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)+(0.0114P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6519
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0532
_refine_ls_wR_factor_gt          0.0450
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_restrained_S_all      0.959
_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
Ho1 Ho 0.08382(3) 0.36283(2) 0.453279(19) 0.02172(9) Uani 1 1 d . . .
Ho2 Ho -0.13526(3) 0.139375(19) -0.024297(19) 0.01976(9) Uani 1 1 d . . .
C1 C -0.3558(7) 0.1765(4) -0.1417(4) 0.0223(15) Uani 1 1 d . . .
C2 C -0.7755(7) 0.0407(4) -0.1119(4) 0.0208(14) Uani 1 1 d . . .
C3 C -0.4009(8) 0.2732(5) 0.1242(5) 0.040(2) Uani 1 1 d . . .
H3A H -0.4110 0.2061 0.1391 0.048 Uiso 1 1 calc R . .
C4 C -0.1826(7) 0.5234(5) 0.3817(4) 0.0256(15) Uani 1 1 d . . .
C5 C -0.7668(7) 0.5729(4) 0.4129(4) 0.0234(15) Uani 1 1 d . . .
C6 C 0.1170(7) 0.1115(4) 0.0806(4) 0.0221(14) Uani 1 1 d . . .
C7 C -0.4783(7) 0.2014(4) -0.2048(4) 0.0299(16) Uani 1 1 d . . .
H7A H -0.4368 0.1600 -0.2508 0.036 Uiso 1 1 calc R . .
H7B H -0.4941 0.2737 -0.2252 0.036 Uiso 1 1 calc R . .
C8 C 0.4219(7) 0.1812(4) 0.5175(4) 0.0281(16) Uani 1 1 d . . .
C9 C -0.6259(7) 0.0696(4) -0.1432(4) 0.0277(16) Uani 1 1 d . . .
H9A H -0.5779 0.0276 -0.1880 0.033 Uiso 1 1 calc R . .
H9B H -0.5538 0.0512 -0.0996 0.033 Uiso 1 1 calc R . .
C10 C -0.6339(6) 0.6124(4) 0.3635(4) 0.0259(15) Uani 1 1 d . . .
H10A H -0.6334 0.6004 0.3062 0.031 Uiso 1 1 calc R . .
H10B H -0.6538 0.6865 0.3670 0.031 Uiso 1 1 calc R . .
C11 C -0.6395(7) 0.1819(4) -0.1730(4) 0.0283(16) Uani 1 1 d . . .
H11A H -0.6840 0.2250 -0.1283 0.034 Uiso 1 1 calc R . .
H11B H -0.7111 0.2017 -0.2168 0.034 Uiso 1 1 calc R . .
C12 C 0.6470(8) 0.2440(5) 0.4120(5) 0.0428(19) Uani 1 1 d . . .
H12A H 0.7206 0.2683 0.3760 0.051 Uiso 1 1 calc R . .
C13 C 0.2415(7) 0.1767(4) 0.1917(4) 0.0280(16) Uani 1 1 d . . .
H13A H 0.3424 0.1670 0.2149 0.034 Uiso 1 1 calc R . .
H13B H 0.2140 0.2462 0.1646 0.034 Uiso 1 1 calc R . .
C14 C 0.3031(8) 0.1482(4) 0.5719(4) 0.0271(16) Uani 1 1 d . . .
C15 C 0.3457(8) 0.0601(5) 0.6272(4) 0.0331(18) Uani 1 1 d . . .
C16 C -0.3324(7) 0.5872(4) 0.3464(4) 0.0281(16) Uani 1 1 d . . .
H16A H -0.3317 0.5744 0.2893 0.034 Uiso 1 1 calc R . .
H16B H -0.3395 0.6603 0.3489 0.034 Uiso 1 1 calc R . .
C17 C 0.5827(8) 0.1266(5) 0.5215(4) 0.0343(18) Uani 1 1 d . . .
C18 C 0.1169(7) 0.1674(4) 0.2609(4) 0.0331(17) Uani 1 1 d . . .
H18A H 0.0134 0.1882 0.2390 0.040 Uiso 1 1 calc R . .
H18B H 0.1344 0.0953 0.2822 0.040 Uiso 1 1 calc R . .
C19 C 0.2596(7) 0.0991(4) 0.1282(4) 0.0300(17) Uani 1 1 d . . .
H19A H 0.3487 0.1049 0.0897 0.036 Uiso 1 1 calc R . .
H19B H 0.2847 0.0298 0.1559 0.036 Uiso 1 1 calc R . .
C20 C 0.4854(8) 0.2903(5) 0.4104(4) 0.0366(18) Uani 1 1 d . . .
H20A H 0.4534 0.3443 0.3703 0.044 Uiso 1 1 calc R . .
C21 C 0.1175(8) 0.2323(4) 0.3304(4) 0.0287(16) Uani 1 1 d . . .
C22 C 0.0422(8) 0.1746(5) 0.6186(5) 0.0407(19) Uani 1 1 d . . .
H22A H -0.0621 0.2132 0.6161 0.049 Uiso 1 1 calc R . .
C23 C 0.6207(9) 0.0369(5) 0.5790(5) 0.049(2) Uani 1 1 d . . .
H23A H 0.7258 0.0002 0.5823 0.059 Uiso 1 1 calc R . .
C24 C -0.1945(8) 0.4030(5) -0.0339(4) 0.0319(17) Uani 1 1 d . . .
C25 C -0.4735(7) 0.5591(5) 0.3946(4) 0.0375(18) Uani 1 1 d . . .
H25A H -0.4740 0.5750 0.4510 0.045 Uiso 1 1 calc R . .
H25B H -0.4593 0.4848 0.3953 0.045 Uiso 1 1 calc R . .
C26 C -0.2890(7) 0.3862(4) 0.0396(4) 0.0288(17) Uani 1 1 d . . .
C27 C 0.6934(8) 0.1614(5) 0.4687(5) 0.047(2) Uani 1 1 d . . .
H27A H 0.8003 0.1287 0.4715 0.056 Uiso 1 1 calc R . .
C28 C 0.5095(9) 0.0050(5) 0.6274(5) 0.045(2) Uani 1 1 d . . .
H28A H 0.5385 -0.0549 0.6625 0.054 Uiso 1 1 calc R . .
C29 C 0.0718(9) 0.0897(5) 0.6757(4) 0.048(2) Uani 1 1 d . . .
H29A H -0.0091 0.0731 0.7112 0.058 Uiso 1 1 calc R . .
C30 C -0.0531(8) 0.3407(5) -0.1525(4) 0.0413(19) Uani 1 1 d . . .
H30A H -0.0126 0.2861 -0.1853 0.050 Uiso 1 1 calc R . .
C31 C -0.4885(8) 0.3516(5) 0.1725(4) 0.049(2) Uani 1 1 d . . .
H31A H -0.5588 0.3383 0.2160 0.059 Uiso 1 1 calc R . .
C32 C -0.0288(9) 0.4375(5) -0.1807(5) 0.065(3) Uani 1 1 d . . .
H32A H 0.0257 0.4472 -0.2312 0.078 Uiso 1 1 calc R . .
C33 C 0.2247(9) 0.0307(5) 0.6782(5) 0.044(2) Uani 1 1 d . . .
H33A H 0.2479 -0.0290 0.7139 0.053 Uiso 1 1 calc R . .
C34 C -0.3698(9) 0.4696(5) 0.0845(5) 0.0421(19) Uani 1 1 d . . .
C35 C -0.2470(10) 0.5855(5) -0.0076(6) 0.061(3) Uani 1 1 d . . .
H35A H -0.2294 0.6510 -0.0212 0.073 Uiso 1 1 calc R . .
C36 C -0.4653(9) 0.4484(5) 0.1524(5) 0.054(2) Uani 1 1 d . . .
H36A H -0.5154 0.5015 0.1853 0.064 Uiso 1 1 calc R . .
C37 C -0.3417(10) 0.5697(5) 0.0588(6) 0.060(3) Uani 1 1 d . . .
H37A H -0.3910 0.6253 0.0894 0.072 Uiso 1 1 calc R . .
C38 C -0.0863(9) 0.5169(5) -0.1329(6) 0.062(3) Uani 1 1 d . . .
H38A H -0.0684 0.5816 -0.1502 0.074 Uiso 1 1 calc R . .
C39 C -0.1728(9) 0.5036(5) -0.0576(5) 0.048(2) Uani 1 1 d . . .
N1 N 0.1496(6) 0.2055(3) 0.5672(3) 0.0309(13) Uani 1 1 d . . .
N2 N 0.3742(6) 0.2632(4) 0.4614(3) 0.0287(13) Uani 1 1 d . . .
N3 N -0.1306(6) 0.3222(4) -0.0815(3) 0.0306(13) Uani 1 1 d . . .
N4 N -0.3053(6) 0.2872(3) 0.0592(3) 0.0274(13) Uani 1 1 d . . .
O1 O -0.1233(5) 0.5597(3) 0.4368(3) 0.0351(11) Uani 1 1 d . . .
O2 O -0.1205(5) 0.4348(3) 0.3606(3) 0.0346(12) Uani 1 1 d . . .
O3 O -0.7806(5) 0.4854(3) 0.3973(3) 0.0289(11) Uani 1 1 d . . .
O4 O -0.8521(5) 0.6289(3) 0.4648(3) 0.0270(11) Uani 1 1 d . . .
O5 O 0.0465(5) 0.2132(3) 0.3990(3) 0.0344(11) Uani 1 1 d . . .
O6 O 0.1854(5) 0.3046(3) 0.3192(3) 0.0325(11) Uani 1 1 d . . .
O7 O 0.0266(5) 0.1986(3) 0.0636(3) 0.0319(11) Uani 1 1 d . . .
O8 O -0.7640(5) -0.0546(3) -0.0900(2) 0.0279(10) Uani 1 1 d . . .
O9 O 0.0952(5) 0.0308(3) 0.0544(3) 0.0267(11) Uani 1 1 d . . .
O10 O -0.9008(4) 0.1121(3) -0.1066(3) 0.0266(11) Uani 1 1 d . . .
O11 O -0.2134(5) 0.1619(3) -0.1664(3) 0.0340(11) Uani 1 1 d . . .
O12 O -0.3996(5) 0.1761(3) -0.0660(3) 0.0321(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
Ho1 O1 2.270(4) 2_566 ?
Ho1 O4 2.309(4) 2_466 ?
Ho1 O3 2.331(4) 1_655 ?
Ho1 O5 2.386(4) . ?
Ho1 O2 2.404(4) . ?
Ho1 O6 2.423(4) . ?
Ho1 N2 2.561(5) . ?
Ho1 N1 2.650(5) . ?
Ho1 C21 2.753(6) . ?
Ho1 O1 2.793(4) . ?
Ho1 C4 2.978(6) . ?
Ho2 O8 2.309(4) 2_455 ?
Ho2 O9 2.315(3) 2 ?
Ho2 O10 2.316(4) 1_655 ?
Ho2 O12 2.394(4) . ?
Ho2 O7 2.438(4) . ?
Ho2 O11 2.461(4) . ?
Ho2 N3 2.538(5) . ?
Ho2 O9 2.541(4) . ?
Ho2 N4 2.584(5) . ?
Ho2 C1 2.779(6) . ?
Ho2 C6 2.859(6) . ?
Ho2 Ho2 3.9214(5) 2 ?
C1 O11 1.247(7) . ?
C1 O12 1.264(7) . ?
C1 C7 1.516(8) . ?
C2 O10 1.259(6) . ?
C2 O8 1.270(6) . ?
C2 C9 1.491(8) . ?
C3 N4 1.319(8) . ?
C3 C31 1.401(8) . ?
C3 H3A 0.9300 . ?
C4 O2 1.242(6) . ?
C4 O1 1.282(6) . ?
C4 C16 1.501(7) . ?
C5 O4 1.253(7) . ?
C5 O3 1.264(6) . ?
C5 C10 1.529(8) . ?
C6 O7 1.251(6) . ?
C6 O9 1.269(6) . ?
C6 C19 1.502(7) . ?
C7 C11 1.535(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.361(7) . ?
C8 C17 1.415(8) . ?
C8 C14 1.433(9) . ?
C9 C11 1.511(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C25 1.514(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C27 1.370(9) . ?
C12 C20 1.394(8) . ?
C12 H12A 0.9300 . ?
C13 C18 1.515(8) . ?
C13 C19 1.519(7) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 N1 1.371(7) . ?
C14 C15 1.403(8) . ?
C15 C33 1.398(9) . ?
C15 C28 1.436(9) . ?
C16 C25 1.511(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C27 1.377(9) . ?
C17 C23 1.435(9) . ?
C18 C21 1.508(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N2 1.320(8) . ?
C20 H20A 0.9300 . ?
C21 O6 1.251(7) . ?
C21 O5 1.267(7) . ?
C22 N1 1.320(8) . ?
C22 C29 1.382(8) . ?
C22 H22A 0.9300 . ?
C23 C28 1.325(10) . ?
C23 H23A 0.9300 . ?
C24 N3 1.371(7) . ?
C24 C39 1.418(8) . ?
C24 C26 1.427(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 N4 1.373(7) . ?
C26 C34 1.399(8) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
C29 C33 1.371(9) . ?
C29 H29A 0.9300 . ?
C30 N3 1.323(8) . ?
C30 C32 1.392(8) . ?
C30 H30A 0.9300 . ?
C31 C36 1.367(9) . ?
C31 H31A 0.9300 . ?
C32 C38 1.351(9) . ?
C32 H32A 0.9300 . ?
C33 H33A 0.9300 . ?
C34 C36 1.376(10) . ?
C34 C37 1.438(9) . ?
C35 C37 1.338(11) . ?
C35 C39 1.422(10) . ?
C35 H35A 0.9300 . ?
C36 H36A 0.9300 . ?
C37 H37A 0.9300 . ?
C38 C39 1.405(10) . ?
C38 H38A 0.9300 . ?
O1 Ho1 2.270(4) 2_566 ?
O3 Ho1 2.331(4) 1_455 ?
O4 Ho1 2.309(4) 2_466 ?
O8 Ho2 2.309(4) 2_455 ?
O9 Ho2 2.315(3) 2 ?
O10 Ho2 2.316(4) 1_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ho1 O4 77.21(14) 2_566 2_466 ?
O1 Ho1 O3 75.61(15) 2_566 1_655 ?
O4 Ho1 O3 133.97(13) 2_466 1_655 ?
O1 Ho1 O5 148.86(15) 2_566 . ?
O4 Ho1 O5 88.70(14) 2_466 . ?
O3 Ho1 O5 131.04(15) 1_655 . ?
O1 Ho1 O2 124.65(14) 2_566 . ?
O4 Ho1 O2 76.14(15) 2_466 . ?
O3 Ho1 O2 89.86(14) 1_655 . ?
O5 Ho1 O2 77.02(14) . . ?
O1 Ho1 O6 146.96(15) 2_566 . ?
O4 Ho1 O6 135.74(13) 2_466 . ?
O3 Ho1 O6 76.72(14) 1_655 . ?
O5 Ho1 O6 54.32(14) . . ?
O2 Ho1 O6 72.69(14) . . ?
O1 Ho1 N2 84.98(15) 2_566 . ?
O4 Ho1 N2 135.95(16) 2_466 . ?
O3 Ho1 N2 77.21(15) 1_655 . ?
O5 Ho1 N2 86.32(14) . . ?
O2 Ho1 N2 143.88(17) . . ?
O6 Ho1 N2 71.55(15) . . ?
O1 Ho1 N1 77.35(14) 2_566 . ?
O4 Ho1 N1 74.26(15) 2_466 . ?
O3 Ho1 N1 132.88(15) 1_655 . ?
O5 Ho1 N1 72.10(15) . . ?
O2 Ho1 N1 137.18(15) . . ?
O6 Ho1 N1 109.87(14) . . ?
N2 Ho1 N1 62.57(17) . . ?
O1 Ho1 C21 163.76(16) 2_566 . ?
O4 Ho1 C21 112.33(17) 2_466 . ?
O3 Ho1 C21 103.71(18) 1_655 . ?
O5 Ho1 C21 27.38(16) . . ?
O2 Ho1 C21 71.34(16) . . ?
O6 Ho1 C21 27.03(16) . . ?
N2 Ho1 C21 79.12(17) . . ?
N1 Ho1 C21 92.29(17) . . ?
O1 Ho1 O1 76.12(14) 2_566 . ?
O4 Ho1 O1 68.43(13) 2_466 . ?
O3 Ho1 O1 69.41(13) 1_655 . ?
O5 Ho1 O1 124.38(13) . . ?
O2 Ho1 O1 49.08(12) . . ?
O6 Ho1 O1 110.22(13) . . ?
N2 Ho1 O1 144.70(13) . . ?
N1 Ho1 O1 137.94(15) . . ?
C21 Ho1 O1 119.20(15) . . ?
O1 Ho1 C4 101.03(16) 2_566 . ?
O4 Ho1 C4 69.33(15) 2_466 . ?
O3 Ho1 C4 80.33(15) 1_655 . ?
O5 Ho1 C4 99.63(16) . . ?
O2 Ho1 C4 23.75(13) . . ?
O6 Ho1 C4 91.71(16) . . ?
N2 Ho1 C4 154.50(17) . . ?
N1 Ho1 C4 142.87(16) . . ?
C21 Ho1 C4 94.77(17) . . ?
O1 Ho1 C4 25.40(13) . . ?
O8 Ho2 O9 73.89(14) 2_455 2 ?
O8 Ho2 O10 136.40(13) 2_455 1_655 ?
O9 Ho2 O10 77.26(13) 2 1_655 ?
O8 Ho2 O12 83.90(15) 2_455 . ?
O9 Ho2 O12 89.60(13) 2 . ?
O10 Ho2 O12 128.03(15) 1_655 . ?
O8 Ho2 O7 89.26(14) 2_455 . ?
O9 Ho2 O7 124.48(12) 2 . ?
O10 Ho2 O7 80.86(14) 1_655 . ?
O12 Ho2 O7 141.73(13) . . ?
O8 Ho2 O11 128.85(13) 2_455 . ?
O9 Ho2 O11 78.30(13) 2 . ?
O10 Ho2 O11 74.43(14) 1_655 . ?
O12 Ho2 O11 53.63(14) . . ?
O7 Ho2 O11 141.47(14) . . ?
O8 Ho2 N3 139.59(15) 2_455 . ?
O9 Ho2 N3 145.56(16) 2 . ?
O10 Ho2 N3 77.78(15) 1_655 . ?
O12 Ho2 N3 87.39(14) . . ?
O7 Ho2 N3 73.83(14) . . ?
O11 Ho2 N3 72.38(15) . . ?
O8 Ho2 O9 71.71(13) 2_455 . ?
O9 Ho2 O9 72.41(14) 2 . ?
O10 Ho2 O9 68.79(14) 1_655 . ?
O12 Ho2 O9 152.76(14) . . ?
O7 Ho2 O9 52.11(11) . . ?
O11 Ho2 O9 136.87(13) . . ?
N3 Ho2 O9 119.04(14) . . ?
O8 Ho2 N4 75.82(15) 2_455 . ?
O9 Ho2 N4 146.30(16) 2 . ?
O10 Ho2 N4 136.17(14) 1_655 . ?
O12 Ho2 N4 72.74(14) . . ?
O7 Ho2 N4 69.08(14) . . ?
O11 Ho2 N4 110.65(14) . . ?
N3 Ho2 N4 63.92(17) . . ?
O9 Ho2 N4 111.33(14) . . ?
O8 Ho2 C1 106.98(16) 2_455 . ?
O9 Ho2 C1 82.97(14) 2 . ?
O10 Ho2 C1 101.06(17) 1_655 . ?
O12 Ho2 C1 26.98(16) . . ?
O7 Ho2 C1 151.67(14) . . ?
O11 Ho2 C1 26.65(16) . . ?
N3 Ho2 C1 78.94(16) . . ?
O9 Ho2 C1 154.79(14) . . ?
N4 Ho2 C1 92.10(17) . . ?
O8 Ho2 C6 80.30(16) 2_455 . ?
O9 Ho2 C6 98.70(15) 2 . ?
O10 Ho2 C6 72.51(16) 1_655 . ?
O12 Ho2 C6 159.31(16) . . ?
O7 Ho2 C6 25.78(12) . . ?
O11 Ho2 C6 146.62(16) . . ?
N3 Ho2 C6 96.02(16) . . ?
O9 Ho2 C6 26.35(12) . . ?
N4 Ho2 C6 90.40(15) . . ?
C1 Ho2 C6 172.68(18) . . ?
O8 Ho2 Ho2 68.45(9) 2_455 2 ?
O9 Ho2 Ho2 38.15(9) 2 2 ?
O10 Ho2 Ho2 68.61(9) 1_655 2 ?
O12 Ho2 Ho2 124.90(9) . 2 ?
O7 Ho2 Ho2 86.35(8) . 2 ?
O11 Ho2 Ho2 110.69(9) . 2 ?
N3 Ho2 Ho2 143.28(11) . 2 ?
O9 Ho2 Ho2 34.25(8) . 2 ?
N4 Ho2 Ho2 136.63(12) . 2 ?
C1 Ho2 Ho2 120.94(11) . 2 ?
C6 Ho2 Ho2 60.56(11) . 2 ?
O11 C1 O12 121.5(6) . . ?
O11 C1 C7 118.5(6) . . ?
O12 C1 C7 119.9(6) . . ?
O11 C1 Ho2 62.3(3) . . ?
O12 C1 Ho2 59.3(3) . . ?
C7 C1 Ho2 177.6(4) . . ?
O10 C2 O8 125.4(6) . . ?
O10 C2 C9 118.1(5) . . ?
O8 C2 C9 116.4(5) . . ?
N4 C3 C31 125.1(6) . . ?
N4 C3 H3A 117.5 . . ?
C31 C3 H3A 117.5 . . ?
O2 C4 O1 120.2(5) . . ?
O2 C4 C16 120.7(5) . . ?
O1 C4 C16 119.0(6) . . ?
O2 C4 Ho1 51.2(3) . . ?
O1 C4 Ho1 69.2(3) . . ?
C16 C4 Ho1 168.8(4) . . ?
O4 C5 O3 125.7(6) . . ?
O4 C5 C10 118.1(5) . . ?
O3 C5 C10 116.3(6) . . ?
O7 C6 O9 120.6(5) . . ?
O7 C6 C19 121.6(5) . . ?
O9 C6 C19 117.7(5) . . ?
O7 C6 Ho2 58.0(3) . . ?
O9 C6 Ho2 62.7(3) . . ?
C19 C6 Ho2 174.3(5) . . ?
C1 C7 C11 114.8(5) . . ?
C1 C7 H7A 108.6 . . ?
C11 C7 H7A 108.6 . . ?
C1 C7 H7B 108.6 . . ?
C11 C7 H7B 108.6 . . ?
H7A C7 H7B 107.5 . . ?
N2 C8 C17 122.2(7) . . ?
N2 C8 C14 118.0(6) . . ?
C17 C8 C14 119.8(6) . . ?
C2 C9 C11 116.8(5) . . ?
C2 C9 H9A 108.1 . . ?
C11 C9 H9A 108.1 . . ?
C2 C9 H9B 108.1 . . ?
C11 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C25 C10 C5 111.8(5) . . ?
C25 C10 H10A 109.3 . . ?
C5 C10 H10A 109.3 . . ?
C25 C10 H10B 109.3 . . ?
C5 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
C9 C11 C7 111.8(5) . . ?
C9 C11 H11A 109.2 . . ?
C7 C11 H11A 109.2 . . ?
C9 C11 H11B 109.2 . . ?
C7 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C27 C12 C20 117.5(7) . . ?
C27 C12 H12A 121.2 . . ?
C20 C12 H12A 121.2 . . ?
C18 C13 C19 113.6(5) . . ?
C18 C13 H13A 108.8 . . ?
C19 C13 H13A 108.8 . . ?
C18 C13 H13B 108.8 . . ?
C19 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
N1 C14 C15 122.5(7) . . ?
N1 C14 C8 117.5(6) . . ?
C15 C14 C8 120.0(6) . . ?
C33 C15 C14 117.5(6) . . ?
C33 C15 C28 124.1(7) . . ?
C14 C15 C28 118.4(7) . . ?
C4 C16 C25 109.6(5) . . ?
C4 C16 H16A 109.7 . . ?
C25 C16 H16A 109.7 . . ?
C4 C16 H16B 109.7 . . ?
C25 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
C27 C17 C8 117.9(7) . . ?
C27 C17 C23 123.8(7) . . ?
C8 C17 C23 118.2(7) . . ?
C21 C18 C13 113.3(5) . . ?
C21 C18 H18A 108.9 . . ?
C13 C18 H18A 108.9 . . ?
C21 C18 H18B 108.9 . . ?
C13 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
C6 C19 C13 115.1(5) . . ?
C6 C19 H19A 108.5 . . ?
C13 C19 H19A 108.5 . . ?
C6 C19 H19B 108.5 . . ?
C13 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
N2 C20 C12 124.9(7) . . ?
N2 C20 H20A 117.6 . . ?
C12 C20 H20A 117.6 . . ?
O6 C21 O5 121.3(6) . . ?
O6 C21 C18 119.8(6) . . ?
O5 C21 C18 118.9(6) . . ?
O6 C21 Ho1 61.6(3) . . ?
O5 C21 Ho1 60.0(3) . . ?
C18 C21 Ho1 173.5(4) . . ?
N1 C22 C29 125.5(7) . . ?
N1 C22 H22A 117.2 . . ?
C29 C22 H22A 117.2 . . ?
C28 C23 C17 121.6(7) . . ?
C28 C23 H23A 119.2 . . ?
C17 C23 H23A 119.2 . . ?
N3 C24 C39 121.3(7) . . ?
N3 C24 C26 119.2(6) . . ?
C39 C24 C26 119.4(6) . . ?
C16 C25 C10 116.2(5) . . ?
C16 C25 H25A 108.2 . . ?
C10 C25 H25A 108.2 . . ?
C16 C25 H25B 108.2 . . ?
C10 C25 H25B 108.2 . . ?
H25A C25 H25B 107.4 . . ?
N4 C26 C34 122.8(7) . . ?
N4 C26 C24 116.6(6) . . ?
C34 C26 C24 120.4(6) . . ?
C12 C27 C17 120.4(7) . . ?
C12 C27 H27A 119.8 . . ?
C17 C27 H27A 119.8 . . ?
C23 C28 C15 121.9(7) . . ?
C23 C28 H28A 119.0 . . ?
C15 C28 H28A 119.0 . . ?
C33 C29 C22 117.6(7) . . ?
C33 C29 H29A 121.2 . . ?
C22 C29 H29A 121.2 . . ?
N3 C30 C32 123.7(7) . . ?
N3 C30 H30A 118.2 . . ?
C32 C30 H30A 118.2 . . ?
C36 C31 C3 116.5(7) . . ?
C36 C31 H31A 121.7 . . ?
C3 C31 H31A 121.7 . . ?
C38 C32 C30 118.4(8) . . ?
C38 C32 H32A 120.8 . . ?
C30 C32 H32A 120.8 . . ?
C29 C33 C15 120.2(7) . . ?
C29 C33 H33A 119.9 . . ?
C15 C33 H33A 119.9 . . ?
C36 C34 C26 117.3(6) . . ?
C36 C34 C37 124.9(7) . . ?
C26 C34 C37 117.8(7) . . ?
C37 C35 C39 120.9(7) . . ?
C37 C35 H35A 119.6 . . ?
C39 C35 H35A 119.6 . . ?
C31 C36 C34 121.7(7) . . ?
C31 C36 H36A 119.1 . . ?
C34 C36 H36A 119.1 . . ?
C35 C37 C34 122.2(7) . . ?
C35 C37 H37A 118.9 . . ?
C34 C37 H37A 118.9 . . ?
C32 C38 C39 121.1(7) . . ?
C32 C38 H38A 119.4 . . ?
C39 C38 H38A 119.4 . . ?
C38 C39 C24 117.0(7) . . ?
C38 C39 C35 124.0(7) . . ?
C24 C39 C35 119.0(8) . . ?
C22 N1 C14 116.6(6) . . ?
C22 N1 Ho1 124.1(4) . . ?
C14 N1 Ho1 119.2(4) . . ?
C20 N2 C8 116.9(6) . . ?
C20 N2 Ho1 120.5(4) . . ?
C8 N2 Ho1 122.6(4) . . ?
C30 N3 C24 118.5(5) . . ?
C30 N3 Ho2 121.8(4) . . ?
C24 N3 Ho2 119.3(4) . . ?
C3 N4 C26 116.5(6) . . ?
C3 N4 Ho2 124.2(4) . . ?
C26 N4 Ho2 119.2(5) . . ?
C4 O1 Ho1 165.4(4) . 2_566 ?
C4 O1 Ho1 85.4(3) . . ?
Ho1 O1 Ho1 103.88(14) 2_566 . ?
C4 O2 Ho1 105.0(4) . . ?
C5 O3 Ho1 138.1(4) . 1_455 ?
C5 O4 Ho1 139.0(4) . 2_466 ?
C21 O5 Ho1 92.6(3) . . ?
C21 O6 Ho1 91.4(4) . . ?
C6 O7 Ho2 96.3(3) . . ?
C2 O8 Ho2 132.7(4) . 2_455 ?
C6 O9 Ho2 161.1(4) . 2 ?
C6 O9 Ho2 90.9(3) . . ?
Ho2 O9 Ho2 107.59(14) 2 . ?
C2 O10 Ho2 135.9(4) . 1_455 ?
C1 O11 Ho2 91.1(4) . . ?
C1 O12 Ho2 93.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.498
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.159
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1528898'
_audit_update_record             
;
2017-01-21 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H14 Cl N2 O4 Tm'
_chemical_formula_sum            'C17 H14 Cl N2 O4 Tm'
_chemical_formula_weight         514.68

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'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   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                   8.1381(11)
_cell_length_b                   12.4629(16)
_cell_length_c                   16.161(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.034(5)
_cell_angle_gamma                90.00
_cell_volume                     1635.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    2967
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      25.40

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             992
_exptl_absorpt_coefficient_mu    5.615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1497
_exptl_absorpt_correction_T_max  0.2681
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      297(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 Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9275
_diffrn_reflns_av_R_equivalents  0.1161
_diffrn_reflns_av_sigmaI/netI    0.1172
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.40
_reflns_number_total             2967
_reflns_number_gt                1817
_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)+(0.0172P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2967
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.0719
_refine_ls_wR_factor_gt          0.0594
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_restrained_S_all      0.950
_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
Tm1 Tm 0.51461(5) 0.62761(3) 0.43553(3) 0.01783(11) Uani 1 1 d . . .
O1 O 0.5984(8) 0.5405(5) 0.5684(4) 0.0242(17) Uani 1 1 d . . .
O2 O 0.6779(8) 0.7043(5) 0.5476(4) 0.0264(17) Uani 1 1 d . . .
O3 O 1.2981(7) 0.6356(5) 0.5134(4) 0.0281(15) Uani 1 1 d . . .
O4 O 1.2666(7) 0.4856(5) 0.5870(4) 0.0255(16) Uani 1 1 d . . .
N1 N 0.7133(9) 0.7516(6) 0.3729(5) 0.0225(19) Uani 1 1 d . . .
N2 N 0.4225(9) 0.8219(6) 0.4267(5) 0.022(2) Uani 1 1 d . . .
C1 C 0.5947(13) 1.0771(7) 0.3519(6) 0.033(3) Uani 1 1 d . . .
H1A H 0.5685 1.1496 0.3478 0.039 Uiso 1 1 calc R . .
C2 C 0.9658(12) 0.7864(7) 0.3079(6) 0.032(3) Uani 1 1 d . . .
H2A H 1.0631 0.7590 0.2896 0.038 Uiso 1 1 calc R . .
C3 C 0.8523(12) 0.7208(8) 0.3433(6) 0.031(3) Uani 1 1 d . . .
H3A H 0.8767 0.6480 0.3463 0.037 Uiso 1 1 calc R . .
C4 C 0.2283(12) 0.9616(7) 0.4449(6) 0.030(3) Uani 1 1 d . . .
H4A H 0.1263 0.9812 0.4627 0.036 Uiso 1 1 calc R . .
C5 C 0.9278(12) 0.8944(8) 0.3010(6) 0.033(3) Uani 1 1 d . . .
H5A H 1.0002 0.9411 0.2772 0.040 Uiso 1 1 calc R . .
C6 C 0.3264(12) 1.0368(8) 0.4123(6) 0.032(3) Uani 1 1 d . . .
H6A H 0.2924 1.1079 0.4075 0.038 Uiso 1 1 calc R . .
C7 C 0.7374(13) 1.0434(8) 0.3261(6) 0.031(3) Uani 1 1 d . . .
H7A H 0.8096 1.0929 0.3055 0.037 Uiso 1 1 calc R . .
C8 C 0.2803(11) 0.8553(7) 0.4518(6) 0.025(2) Uani 1 1 d . . .
H8A H 0.2119 0.8056 0.4751 0.030 Uiso 1 1 calc R . .
C9 C 0.5217(11) 0.8958(6) 0.3935(5) 0.021(2) Uani 1 1 d . . .
C10 C 0.4804(11) 1.0049(7) 0.3858(6) 0.021(2) Uani 1 1 d . . .
C11 C 0.9619(11) 0.5573(7) 0.6429(6) 0.024(2) Uani 1 1 d . . .
H11A H 1.0270 0.5378 0.6933 0.029 Uiso 1 1 calc R . .
H11B H 0.9335 0.4915 0.6131 0.029 Uiso 1 1 calc R . .
C12 C 0.6742(10) 0.8596(7) 0.3649(5) 0.022(2) Uani 1 1 d . . .
C13 C 1.0658(10) 0.6250(9) 0.5904(6) 0.039(3) Uani 1 1 d . . .
H13A H 1.0951 0.6896 0.6215 0.046 Uiso 1 1 calc R . .
H13B H 0.9974 0.6469 0.5418 0.046 Uiso 1 1 calc R . .
C14 C 0.8029(10) 0.6109(7) 0.6668(5) 0.021(2) Uani 1 1 d . . .
H14A H 0.7534 0.5683 0.7087 0.025 Uiso 1 1 calc R . .
H14B H 0.8278 0.6814 0.6901 0.025 Uiso 1 1 calc R . .
C15 C 0.7816(12) 0.9334(7) 0.3295(6) 0.025(2) Uani 1 1 d . . .
C16 C 0.6843(10) 0.6217(9) 0.5919(5) 0.019(2) Uani 1 1 d . . .
C17 C 1.2214(12) 0.5782(7) 0.5612(6) 0.028(2) Uani 1 1 d . . .
Cl1 Cl 0.3810(3) 0.6374(2) 0.28388(15) 0.0330(6) 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
Tm1 O3 2.238(6) 1_455 ?
Tm1 O1 2.287(6) 3_666 ?
Tm1 O4 2.320(6) 3_766 ?
Tm1 O2 2.371(6) . ?
Tm1 O1 2.460(6) . ?
Tm1 N1 2.501(8) . ?
Tm1 N2 2.536(7) . ?
Tm1 Cl1 2.613(2) . ?
Tm1 C16 2.795(9) . ?
Tm1 Tm1 3.8192(9) 3_666 ?
O1 C16 1.272(11) . ?
O1 Tm1 2.287(6) 3_666 ?
O2 C16 1.254(11) . ?
O3 C17 1.251(11) . ?
O3 Tm1 2.238(6) 1_655 ?
O4 C17 1.273(10) . ?
O4 Tm1 2.320(6) 3_766 ?
N1 C3 1.316(12) . ?
N1 C12 1.387(11) . ?
N2 C8 1.320(11) . ?
N2 C9 1.360(11) . ?
C1 C7 1.329(13) . ?
C1 C10 1.431(12) . ?
C1 H1A 0.9300 . ?
C2 C5 1.384(13) . ?
C2 C3 1.386(12) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
C4 C6 1.361(13) . ?
C4 C8 1.393(12) . ?
C4 H4A 0.9300 . ?
C5 C15 1.394(13) . ?
C5 H5A 0.9300 . ?
C6 C10 1.409(13) . ?
C6 H6A 0.9300 . ?
C7 C15 1.417(12) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C9 C10 1.405(11) . ?
C9 C12 1.427(12) . ?
C11 C13 1.499(12) . ?
C11 C14 1.530(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C15 1.416(12) . ?
C13 C17 1.501(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C16 1.500(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Tm1 O1 74.1(2) 1_455 3_666 ?
O3 Tm1 O4 139.3(2) 1_455 3_766 ?
O1 Tm1 O4 75.5(2) 3_666 3_766 ?
O3 Tm1 O2 88.5(2) 1_455 . ?
O1 Tm1 O2 126.4(2) 3_666 . ?
O4 Tm1 O2 88.3(2) 3_766 . ?
O3 Tm1 O1 73.1(2) 1_455 . ?
O1 Tm1 O1 72.9(2) 3_666 . ?
O4 Tm1 O1 72.5(2) 3_766 . ?
O2 Tm1 O1 53.49(19) . . ?
O3 Tm1 N1 139.2(2) 1_455 . ?
O1 Tm1 N1 145.6(2) 3_666 . ?
O4 Tm1 N1 77.7(2) 3_766 . ?
O2 Tm1 N1 73.5(2) . . ?
O1 Tm1 N1 118.6(2) . . ?
O3 Tm1 N2 75.4(2) 1_455 . ?
O1 Tm1 N2 139.2(2) 3_666 . ?
O4 Tm1 N2 143.0(2) 3_766 . ?
O2 Tm1 N2 78.8(2) . . ?
O1 Tm1 N2 122.2(2) . . ?
N1 Tm1 N2 65.4(2) . . ?
O3 Tm1 Cl1 103.49(17) 1_455 . ?
O1 Tm1 Cl1 82.89(17) 3_666 . ?
O4 Tm1 Cl1 98.89(17) 3_766 . ?
O2 Tm1 Cl1 150.64(16) . . ?
O1 Tm1 Cl1 155.63(15) . . ?
N1 Tm1 Cl1 80.22(18) . . ?
N2 Tm1 Cl1 78.52(19) . . ?
O3 Tm1 C16 81.4(2) 1_455 . ?
O1 Tm1 C16 100.0(3) 3_666 . ?
O4 Tm1 C16 77.9(2) 3_766 . ?
O2 Tm1 C16 26.5(3) . . ?
O1 Tm1 C16 27.1(2) . . ?
N1 Tm1 C16 95.2(3) . . ?
N2 Tm1 C16 101.6(3) . . ?
Cl1 Tm1 C16 174.89(19) . . ?
O3 Tm1 Tm1 69.42(16) 1_455 3_666 ?
O1 Tm1 Tm1 38.00(16) 3_666 3_666 ?
O4 Tm1 Tm1 69.95(15) 3_766 3_666 ?
O2 Tm1 Tm1 88.40(15) . 3_666 ?
O1 Tm1 Tm1 34.92(14) . 3_666 ?
N1 Tm1 Tm1 143.33(17) . 3_666 ?
N2 Tm1 Tm1 142.80(19) . 3_666 ?
Cl1 Tm1 Tm1 120.84(6) . 3_666 ?
C16 Tm1 Tm1 62.0(2) . 3_666 ?
C16 O1 Tm1 161.5(6) . 3_666 ?
C16 O1 Tm1 91.3(5) . . ?
Tm1 O1 Tm1 107.1(2) 3_666 . ?
C16 O2 Tm1 96.0(6) . . ?
C17 O3 Tm1 140.2(6) . 1_655 ?
C17 O4 Tm1 135.0(6) . 3_766 ?
C3 N1 C12 116.5(8) . . ?
C3 N1 Tm1 124.3(6) . . ?
C12 N1 Tm1 119.1(6) . . ?
C8 N2 C9 117.7(8) . . ?
C8 N2 Tm1 123.1(6) . . ?
C9 N2 Tm1 119.2(6) . . ?
C7 C1 C10 121.8(9) . . ?
C7 C1 H1A 119.1 . . ?
C10 C1 H1A 119.1 . . ?
C5 C2 C3 117.1(9) . . ?
C5 C2 H2A 121.5 . . ?
C3 C2 H2A 121.5 . . ?
N1 C3 C2 126.4(9) . . ?
N1 C3 H3A 116.8 . . ?
C2 C3 H3A 116.8 . . ?
C6 C4 C8 120.2(9) . . ?
C6 C4 H4A 119.9 . . ?
C8 C4 H4A 119.9 . . ?
C2 C5 C15 120.2(9) . . ?
C2 C5 H5A 119.9 . . ?
C15 C5 H5A 119.9 . . ?
C4 C6 C10 118.8(9) . . ?
C4 C6 H6A 120.6 . . ?
C10 C6 H6A 120.6 . . ?
C1 C7 C15 121.2(10) . . ?
C1 C7 H7A 119.4 . . ?
C15 C7 H7A 119.4 . . ?
N2 C8 C4 122.9(9) . . ?
N2 C8 H8A 118.5 . . ?
C4 C8 H8A 118.5 . . ?
N2 C9 C10 123.1(8) . . ?
N2 C9 C12 117.9(8) . . ?
C10 C9 C12 119.0(8) . . ?
C9 C10 C6 117.3(9) . . ?
C9 C10 C1 119.0(9) . . ?
C6 C10 C1 123.7(8) . . ?
C13 C11 C14 114.6(7) . . ?
C13 C11 H11A 108.6 . . ?
C14 C11 H11A 108.6 . . ?
C13 C11 H11B 108.6 . . ?
C14 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
N1 C12 C15 121.6(8) . . ?
N1 C12 C9 118.4(8) . . ?
C15 C12 C9 120.1(8) . . ?
C11 C13 C17 118.8(9) . . ?
C11 C13 H13A 107.6 . . ?
C17 C13 H13A 107.6 . . ?
C11 C13 H13B 107.6 . . ?
C17 C13 H13B 107.6 . . ?
H13A C13 H13B 107.1 . . ?
C16 C14 C11 110.0(7) . . ?
C16 C14 H14A 109.7 . . ?
C11 C14 H14A 109.7 . . ?
C16 C14 H14B 109.7 . . ?
C11 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C5 C15 C12 118.2(8) . . ?
C5 C15 C7 123.0(9) . . ?
C12 C15 C7 118.8(9) . . ?
O2 C16 O1 118.9(8) . . ?
O2 C16 C14 122.2(9) . . ?
O1 C16 C14 118.6(9) . . ?
O2 C16 Tm1 57.5(5) . . ?
O1 C16 Tm1 61.6(5) . . ?
C14 C16 Tm1 168.8(6) . . ?
O3 C17 O4 125.1(9) . . ?
O3 C17 C13 116.2(8) . . ?
O4 C17 C13 118.7(9) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.40
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.867
_refine_diff_density_rms         0.223
####################################################################### 
# 
# 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 1528900'
_audit_update_record             
;
2017-01-21 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H34 N4 O12 Tb2'
_chemical_formula_sum            'C39 H34 N4 O12 Tb2'
_chemical_formula_weight         1068.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.7895(4)
_cell_length_b                   13.4391(7)
_cell_length_c                   16.4098(9)
_cell_angle_alpha                83.909(2)
_cell_angle_beta                 84.340(2)
_cell_angle_gamma                74.984(2)
_cell_volume                     1856.50(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    6573
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1044
_exptl_absorpt_coefficient_mu    3.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2199
_exptl_absorpt_correction_T_max  0.3385
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      300(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 Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18336
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_sigmaI/netI    0.0790
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         25.10
_reflns_number_total             6573
_reflns_number_gt                4606
_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)+(0.0179P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6573
_refine_ls_number_parameters     514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0561
_refine_ls_wR_factor_gt          0.0487
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_restrained_S_all      0.963
_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
Tb1 Tb 0.91518(3) 0.13657(2) 0.046521(17) 0.01995(8) Uani 1 1 d . . .
Tb2 Tb 1.13610(3) 0.360183(19) 0.524327(17) 0.01869(8) Uani 1 1 d . . .
O1 O 0.8107(4) 0.1967(3) 0.1802(2) 0.0331(10) Uani 1 1 d . . .
O2 O 0.9503(4) 0.2880(3) 0.1009(2) 0.0345(10) Uani 1 1 d . . .
O3 O 0.9706(4) 0.3005(3) 0.4364(2) 0.0312(10) Uani 1 1 d . . .
O4 O 0.9045(4) 0.4676(3) 0.4461(2) 0.0259(9) Uani 1 1 d . . .
O5 O 1.1212(4) 0.0676(3) 0.1426(2) 0.0333(10) Uani 1 1 d . . .
O6 O 1.1162(4) -0.0550(3) 0.0655(2) 0.0280(9) Uani 1 1 d . . .
O7 O 1.8488(4) -0.1290(3) 0.0355(2) 0.0259(9) Uani 1 1 d . . .
O8 O 1.7727(4) 0.0157(3) 0.1009(2) 0.0292(10) Uani 1 1 d . . .
O9 O 1.7634(4) 0.5543(3) 0.5916(2) 0.0286(9) Uani 1 1 d . . .
O10 O 1.9011(4) 0.3881(3) 0.6087(2) 0.0259(9) Uani 1 1 d . . .
O11 O 1.4022(4) 0.3233(3) 0.5667(3) 0.0322(10) Uani 1 1 d . . .
O12 O 1.2152(4) 0.3380(3) 0.6670(2) 0.0358(10) Uani 1 1 d . . .
N1 N 0.6220(5) 0.2385(3) 0.0361(3) 0.0270(11) Uani 1 1 d . . .
N2 N 0.8495(5) 0.2938(3) -0.0686(3) 0.0256(11) Uani 1 1 d . . .
N3 N 1.1327(5) 0.1755(3) 0.5815(3) 0.0305(12) Uani 1 1 d . . .
N4 N 1.3056(5) 0.2113(3) 0.4402(3) 0.0277(12) Uani 1 1 d . . .
C1 C 0.9582(7) 0.3242(4) -0.1193(4) 0.0384(16) Uani 1 1 d . . .
H1A H 1.0623 0.2855 -0.1171 0.046 Uiso 1 1 calc R . .
C2 C 0.9271(7) 0.4107(5) -0.1760(4) 0.0425(17) Uani 1 1 d . . .
H2A H 1.0081 0.4275 -0.2111 0.051 Uiso 1 1 calc R . .
C3 C 0.7770(7) 0.4700(5) -0.1792(4) 0.0412(17) Uani 1 1 d . . .
H3A H 0.7539 0.5294 -0.2150 0.049 Uiso 1 1 calc R . .
C4 C 0.6573(7) 0.4402(5) -0.1274(4) 0.0371(16) Uani 1 1 d . . .
C5 C 0.4950(8) 0.4972(5) -0.1283(4) 0.0486(18) Uani 1 1 d . . .
H5A H 0.4683 0.5572 -0.1634 0.058 Uiso 1 1 calc R . .
C6 C 0.3809(7) 0.4665(5) -0.0799(5) 0.0481(19) Uani 1 1 d . . .
H6A H 0.2765 0.5044 -0.0829 0.058 Uiso 1 1 calc R . .
C7 C 0.4172(6) 0.3762(5) -0.0238(4) 0.0341(15) Uani 1 1 d . . .
C8 C 0.3046(7) 0.3415(5) 0.0289(4) 0.0425(18) Uani 1 1 d . . .
H8A H 0.1981 0.3746 0.0260 0.051 Uiso 1 1 calc R . .
C9 C 0.3493(6) 0.2596(5) 0.0847(4) 0.0437(18) Uani 1 1 d . . .
H9A H 0.2743 0.2364 0.1203 0.052 Uiso 1 1 calc R . .
C10 C 0.5109(6) 0.2100(4) 0.0878(4) 0.0359(16) Uani 1 1 d . . .
H10A H 0.5414 0.1554 0.1275 0.043 Uiso 1 1 calc R . .
C11 C 0.6971(6) 0.3516(4) -0.0730(4) 0.0275(14) Uani 1 1 d . . .
C12 C 0.5768(6) 0.3195(4) -0.0194(4) 0.0265(14) Uani 1 1 d . . .
C13 C 1.0543(7) 0.1586(5) 0.6524(4) 0.0487(19) Uani 1 1 d . . .
H13A H 1.0141 0.2130 0.6854 0.058 Uiso 1 1 calc R . .
C14 C 1.0300(8) 0.0613(5) 0.6792(5) 0.069(3) Uani 1 1 d . . .
H14A H 0.9749 0.0517 0.7295 0.082 Uiso 1 1 calc R . .
C15 C 1.0864(8) -0.0188(5) 0.6322(6) 0.071(3) Uani 1 1 d . . .
H15A H 1.0667 -0.0829 0.6489 0.086 Uiso 1 1 calc R . .
C16 C 1.1752(7) -0.0044(4) 0.5576(5) 0.0479(19) Uani 1 1 d . . .
C17 C 1.2499(8) -0.0857(5) 0.5070(5) 0.064(2) Uani 1 1 d . . .
H17A H 1.2323 -0.1510 0.5206 0.077 Uiso 1 1 calc R . .
C18 C 1.3435(8) -0.0709(5) 0.4415(5) 0.057(2) Uani 1 1 d . . .
H18A H 1.3941 -0.1267 0.4115 0.068 Uiso 1 1 calc R . .
C19 C 1.3695(7) 0.0296(5) 0.4150(4) 0.0395(17) Uani 1 1 d . . .
C20 C 1.4700(7) 0.0502(5) 0.3473(4) 0.0497(19) Uani 1 1 d . . .
H20A H 1.5242 -0.0031 0.3155 0.060 Uiso 1 1 calc R . .
C21 C 1.4891(7) 0.1468(5) 0.3277(4) 0.0457(18) Uani 1 1 d . . .
H21A H 1.5576 0.1606 0.2835 0.055 Uiso 1 1 calc R . .
C22 C 1.4024(6) 0.2256(4) 0.3758(4) 0.0346(16) Uani 1 1 d . . .
H22A H 1.4139 0.2922 0.3615 0.042 Uiso 1 1 calc R . .
C23 C 1.1944(6) 0.0963(4) 0.5346(4) 0.0314(15) Uani 1 1 d . . .
C24 C 1.2901(6) 0.1128(4) 0.4601(4) 0.0297(15) Uani 1 1 d . . .
C25 C 0.8796(6) 0.2690(4) 0.1698(4) 0.0273(14) Uani 1 1 d . . .
C26 C 0.8782(6) 0.3330(4) 0.2391(4) 0.0364(16) Uani 1 1 d . . .
H26A H 0.8605 0.4049 0.2177 0.044 Uiso 1 1 calc R . .
H26B H 0.9815 0.3126 0.2609 0.044 Uiso 1 1 calc R . .
C27 C 0.7543(6) 0.3243(4) 0.3089(3) 0.0285(14) Uani 1 1 d . . .
H27A H 0.7808 0.2546 0.3353 0.034 Uiso 1 1 calc R . .
H27B H 0.6531 0.3352 0.2860 0.034 Uiso 1 1 calc R . .
C28 C 0.7377(6) 0.4002(4) 0.3736(4) 0.0302(15) Uani 1 1 d . . .
H28A H 0.7109 0.4698 0.3470 0.036 Uiso 1 1 calc R . .
H28B H 0.6502 0.3931 0.4128 0.036 Uiso 1 1 calc R . .
C29 C 0.8826(6) 0.3873(4) 0.4203(3) 0.0231(13) Uani 1 1 d . . .
C30 C 1.7617(6) -0.0719(4) 0.0862(3) 0.0234(13) Uani 1 1 d . . .
C31 C 1.6295(5) -0.1123(4) 0.1351(3) 0.0262(14) Uani 1 1 d . . .
H31A H 1.6480 -0.1856 0.1295 0.031 Uiso 1 1 calc R . .
H31B H 1.6306 -0.1030 0.1929 0.031 Uiso 1 1 calc R . .
C32 C 1.4698(5) -0.0564(5) 0.1057(4) 0.0364(16) Uani 1 1 d . . .
H32A H 1.4691 -0.0689 0.0486 0.044 Uiso 1 1 calc R . .
H32B H 1.4565 0.0172 0.1078 0.044 Uiso 1 1 calc R . .
C33 C 1.3292(5) -0.0861(4) 0.1530(4) 0.0267(14) Uani 1 1 d . . .
H33A H 1.3360 -0.1585 0.1483 0.032 Uiso 1 1 calc R . .
H33B H 1.3293 -0.0762 0.2107 0.032 Uiso 1 1 calc R . .
C34 C 1.1788(5) -0.0202(4) 0.1194(3) 0.0230(13) Uani 1 1 d . . .
C35 C 1.3584(6) 0.3222(4) 0.6423(4) 0.0238(13) Uani 1 1 d . . .
C36 C 1.4799(6) 0.2990(4) 0.7056(4) 0.0292(14) Uani 1 1 d . . .
H36A H 1.4960 0.2271 0.7267 0.035 Uiso 1 1 calc R . .
H36B H 1.4375 0.3410 0.7511 0.035 Uiso 1 1 calc R . .
C37 C 1.6409(5) 0.3186(4) 0.6739(4) 0.0275(14) Uani 1 1 d . . .
H37A H 1.7121 0.2996 0.7177 0.033 Uiso 1 1 calc R . .
H37B H 1.6861 0.2756 0.6293 0.033 Uiso 1 1 calc R . .
C38 C 1.6248(5) 0.4306(4) 0.6439(3) 0.0237(13) Uani 1 1 d . . .
H38A H 1.5767 0.4727 0.6887 0.028 Uiso 1 1 calc R . .
H38B H 1.5530 0.4485 0.6003 0.028 Uiso 1 1 calc R . .
C39 C 1.7765(6) 0.4589(4) 0.6122(3) 0.0207(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
Tb1 O6 2.311(4) 2_755 ?
Tb1 O7 2.344(3) 2_855 ?
Tb1 O8 2.351(3) 1_455 ?
Tb1 O2 2.408(3) . ?
Tb1 O1 2.430(4) . ?
Tb1 O5 2.452(4) . ?
Tb1 N1 2.599(4) . ?
Tb1 N2 2.665(4) . ?
Tb1 O6 2.726(4) . ?
Tb1 C25 2.776(6) . ?
Tb1 C34 2.953(5) . ?
Tb1 Tb1 3.9917(5) 2_755 ?
Tb2 O9 2.334(4) 2_866 ?
Tb2 O10 2.339(3) 1_455 ?
Tb2 O4 2.344(3) 2_766 ?
Tb2 O11 2.418(3) . ?
Tb2 O3 2.471(3) . ?
Tb2 O12 2.473(4) . ?
Tb2 O4 2.545(3) . ?
Tb2 N3 2.565(4) . ?
Tb2 N4 2.601(4) . ?
Tb2 C35 2.801(6) . ?
Tb2 C29 2.866(5) . ?
Tb2 Tb2 3.9453(5) 2_766 ?
O1 C25 1.261(6) . ?
O2 C25 1.269(6) . ?
O3 C29 1.240(6) . ?
O4 C29 1.266(5) . ?
O4 Tb2 2.344(3) 2_766 ?
O5 C34 1.242(6) . ?
O6 C34 1.273(6) . ?
O6 Tb1 2.311(4) 2_755 ?
O7 C30 1.254(6) . ?
O7 Tb1 2.344(3) 2_855 ?
O8 C30 1.256(6) . ?
O8 Tb1 2.351(3) 1_655 ?
O9 C39 1.269(6) . ?
O9 Tb2 2.334(4) 2_866 ?
O10 C39 1.252(6) . ?
O10 Tb2 2.339(3) 1_655 ?
O11 C35 1.261(6) . ?
O12 C35 1.254(6) . ?
N1 C10 1.334(7) . ?
N1 C12 1.345(7) . ?
N2 C1 1.322(7) . ?
N2 C11 1.368(6) . ?
N3 C13 1.322(7) . ?
N3 C23 1.346(7) . ?
N4 C22 1.319(7) . ?
N4 C24 1.367(6) . ?
C1 C2 1.395(8) . ?
C1 H1A 0.9300 . ?
C2 C3 1.356(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.399(8) . ?
C3 H3A 0.9300 . ?
C4 C11 1.398(8) . ?
C4 C5 1.435(8) . ?
C5 C6 1.340(9) . ?
C5 H5A 0.9300 . ?
C6 C7 1.429(8) . ?
C6 H6A 0.9300 . ?
C7 C8 1.389(8) . ?
C7 C12 1.417(7) . ?
C8 C9 1.355(8) . ?
C8 H8A 0.9300 . ?
C9 C10 1.408(7) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.432(7) . ?
C13 C14 1.397(8) . ?
C13 H13A 0.9300 . ?
C14 C15 1.351(10) . ?
C14 H14A 0.9300 . ?
C15 C16 1.409(10) . ?
C15 H15A 0.9300 . ?
C16 C23 1.414(7) . ?
C16 C17 1.424(9) . ?
C17 C18 1.318(9) . ?
C17 H17A 0.9300 . ?
C18 C19 1.443(8) . ?
C18 H18A 0.9300 . ?
C19 C24 1.398(8) . ?
C19 C20 1.400(8) . ?
C20 C21 1.354(8) . ?
C20 H20A 0.9300 . ?
C21 C22 1.403(7) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C23 C24 1.445(8) . ?
C25 C26 1.495(7) . ?
C26 C27 1.517(7) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.520(7) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.513(7) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C30 C31 1.530(6) . ?
C31 C32 1.509(6) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.513(6) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.507(7) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C35 C36 1.515(7) . ?
C36 C37 1.537(6) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C38 1.508(7) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.509(6) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?

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 Tb1 O7 76.44(12) 2_755 2_855 ?
O6 Tb1 O8 75.36(13) 2_755 1_455 ?
O7 Tb1 O8 135.06(11) 2_855 1_455 ?
O6 Tb1 O2 149.00(13) 2_755 . ?
O7 Tb1 O2 88.40(12) 2_855 . ?
O8 Tb1 O2 131.22(13) 1_455 . ?
O6 Tb1 O1 148.12(11) 2_755 . ?
O7 Tb1 O1 135.33(12) 2_855 . ?
O8 Tb1 O1 77.21(12) 1_455 . ?
O2 Tb1 O1 54.04(12) . . ?
O6 Tb1 O5 124.46(12) 2_755 . ?
O7 Tb1 O5 76.11(13) 2_855 . ?
O8 Tb1 O5 92.10(13) 1_455 . ?
O2 Tb1 O5 76.07(13) . . ?
O1 Tb1 O5 72.24(13) . . ?
O6 Tb1 N1 86.35(13) 2_755 . ?
O7 Tb1 N1 135.41(14) 2_855 . ?
O8 Tb1 N1 76.33(13) 1_455 . ?
O2 Tb1 N1 85.87(13) . . ?
O1 Tb1 N1 71.58(13) . . ?
O5 Tb1 N1 143.62(14) . . ?
O6 Tb1 N2 77.90(13) 2_755 . ?
O7 Tb1 N2 74.31(12) 2_855 . ?
O8 Tb1 N2 131.23(12) 1_455 . ?
O2 Tb1 N2 71.97(13) . . ?
O1 Tb1 N2 109.42(13) . . ?
O5 Tb1 N2 136.51(12) . . ?
N1 Tb1 N2 61.88(13) . . ?
O6 Tb1 O6 75.45(13) 2_755 . ?
O7 Tb1 O6 69.17(11) 2_855 . ?
O8 Tb1 O6 70.31(11) 1_455 . ?
O2 Tb1 O6 124.35(12) . . ?
O1 Tb1 O6 109.93(12) . . ?
O5 Tb1 O6 49.80(11) . . ?
N1 Tb1 O6 145.00(11) . . ?
N2 Tb1 O6 138.70(12) . . ?
O6 Tb1 C25 165.15(13) 2_755 . ?
O7 Tb1 C25 111.73(14) 2_855 . ?
O8 Tb1 C25 104.18(15) 1_455 . ?
O2 Tb1 C25 27.17(14) . . ?
O1 Tb1 C25 26.99(13) . . ?
O5 Tb1 C25 70.28(14) . . ?
N1 Tb1 C25 79.20(14) . . ?
N2 Tb1 C25 92.13(15) . . ?
O6 Tb1 C25 118.70(14) . . ?
O6 Tb1 C34 100.26(15) 2_755 . ?
O7 Tb1 C34 69.34(13) 2_855 . ?
O8 Tb1 C34 82.14(13) 1_455 . ?
O2 Tb1 C34 99.35(14) . . ?
O1 Tb1 C34 91.72(14) . . ?
O5 Tb1 C34 24.39(13) . . ?
N1 Tb1 C34 155.11(14) . . ?
N2 Tb1 C34 142.88(13) . . ?
O6 Tb1 C34 25.51(12) . . ?
C25 Tb1 C34 94.33(16) . . ?
O6 Tb1 Tb1 41.37(9) 2_755 2_755 ?
O7 Tb1 Tb1 67.76(8) 2_855 2_755 ?
O8 Tb1 Tb1 67.89(8) 1_455 2_755 ?
O2 Tb1 Tb1 151.82(9) . 2_755 ?
O1 Tb1 Tb1 136.41(9) . 2_755 ?
O5 Tb1 Tb1 83.50(9) . 2_755 ?
N1 Tb1 Tb1 121.50(9) . 2_755 ?
N2 Tb1 Tb1 113.05(9) . 2_755 ?
O6 Tb1 Tb1 34.08(8) . 2_755 ?
C25 Tb1 Tb1 152.56(11) . 2_755 ?
C34 Tb1 Tb1 59.13(11) . 2_755 ?
O9 Tb2 O10 136.42(12) 2_866 1_455 ?
O9 Tb2 O4 73.60(12) 2_866 2_766 ?
O10 Tb2 O4 77.16(12) 1_455 2_766 ?
O9 Tb2 O11 84.27(13) 2_866 . ?
O10 Tb2 O11 127.31(13) 1_455 . ?
O4 Tb2 O11 89.62(12) 2_766 . ?
O9 Tb2 O3 89.45(13) 2_866 . ?
O10 Tb2 O3 80.92(12) 1_455 . ?
O4 Tb2 O3 124.13(12) 2_766 . ?
O11 Tb2 O3 142.25(12) . . ?
O9 Tb2 O12 128.85(12) 2_866 . ?
O10 Tb2 O12 74.06(12) 1_455 . ?
O4 Tb2 O12 78.51(13) 2_766 . ?
O11 Tb2 O12 53.28(12) . . ?
O3 Tb2 O12 141.34(12) . . ?
O9 Tb2 O4 71.85(12) 2_866 . ?
O10 Tb2 O4 68.91(12) 1_455 . ?
O4 Tb2 O4 72.46(13) 2_766 . ?
O11 Tb2 O4 153.24(12) . . ?
O3 Tb2 O4 51.71(11) . . ?
O12 Tb2 O4 136.86(12) . . ?
O9 Tb2 N3 139.27(14) 2_866 . ?
O10 Tb2 N3 78.15(13) 1_455 . ?
O4 Tb2 N3 146.21(15) 2_766 . ?
O11 Tb2 N3 87.28(13) . . ?
O3 Tb2 N3 73.59(14) . . ?
O12 Tb2 N3 72.76(14) . . ?
O4 Tb2 N3 118.69(12) . . ?
O9 Tb2 N4 76.06(13) 2_866 . ?
O10 Tb2 N4 136.18(12) 1_455 . ?
O4 Tb2 N4 146.38(13) 2_766 . ?
O11 Tb2 N4 73.19(13) . . ?
O3 Tb2 N4 69.17(12) . . ?
O12 Tb2 N4 110.76(13) . . ?
O4 Tb2 N4 111.13(13) . . ?
N3 Tb2 N4 63.37(15) . . ?
O9 Tb2 C35 107.21(14) 2_866 . ?
O10 Tb2 C35 100.64(15) 1_455 . ?
O4 Tb2 C35 83.40(13) 2_766 . ?
O11 Tb2 C35 26.69(13) . . ?
O3 Tb2 C35 151.51(13) . . ?
O12 Tb2 C35 26.59(13) . . ?
O4 Tb2 C35 155.18(13) . . ?
N3 Tb2 C35 78.87(14) . . ?
N4 Tb2 C35 92.11(15) . . ?
O9 Tb2 C29 80.48(14) 2_866 . ?
O10 Tb2 C29 72.71(14) 1_455 . ?
O4 Tb2 C29 98.62(14) 2_766 . ?
O11 Tb2 C29 159.81(14) . . ?
O3 Tb2 C29 25.52(12) . . ?
O12 Tb2 C29 146.42(13) . . ?
O4 Tb2 C29 26.21(12) . . ?
N3 Tb2 C29 95.67(15) . . ?
N4 Tb2 C29 90.26(14) . . ?
C35 Tb2 C29 172.29(15) . . ?
O9 Tb2 Tb2 68.37(8) 2_866 2_766 ?
O10 Tb2 Tb2 68.65(9) 1_455 2_766 ?
O4 Tb2 Tb2 37.96(9) 2_766 2_766 ?
O11 Tb2 Tb2 124.89(9) . 2_766 ?
O3 Tb2 Tb2 86.19(8) . 2_766 ?
O12 Tb2 Tb2 110.63(9) . 2_766 ?
O4 Tb2 Tb2 34.51(7) . 2_766 ?
N3 Tb2 Tb2 143.45(9) . 2_766 ?
N4 Tb2 Tb2 136.66(11) . 2_766 ?
C35 Tb2 Tb2 121.14(10) . 2_766 ?
C29 Tb2 Tb2 60.68(11) . 2_766 ?
C25 O1 Tb1 92.0(3) . . ?
C25 O2 Tb1 92.8(3) . . ?
C29 O3 Tb2 95.3(3) . . ?
C29 O4 Tb2 160.9(3) . 2_766 ?
C29 O4 Tb2 91.2(3) . . ?
Tb2 O4 Tb2 107.54(13) 2_766 . ?
C34 O5 Tb1 101.0(3) . . ?
C34 O6 Tb1 162.0(3) . 2_755 ?
C34 O6 Tb1 87.3(3) . . ?
Tb1 O6 Tb1 104.55(13) 2_755 . ?
C30 O7 Tb1 138.5(3) . 2_855 ?
C30 O8 Tb1 137.9(3) . 1_655 ?
C39 O9 Tb2 131.6(3) . 2_866 ?
C39 O10 Tb2 134.8(3) . 1_655 ?
C35 O11 Tb2 93.8(3) . . ?
C35 O12 Tb2 91.4(3) . . ?
C10 N1 C12 118.2(5) . . ?
C10 N1 Tb1 119.1(4) . . ?
C12 N1 Tb1 122.7(3) . . ?
C1 N2 C11 117.0(5) . . ?
C1 N2 Tb1 123.6(4) . . ?
C11 N2 Tb1 119.3(4) . . ?
C13 N3 C23 119.1(5) . . ?
C13 N3 Tb2 120.6(4) . . ?
C23 N3 Tb2 119.8(4) . . ?
C22 N4 C24 117.0(5) . . ?
C22 N4 Tb2 123.6(4) . . ?
C24 N4 Tb2 119.4(4) . . ?
N2 C1 C2 124.3(6) . . ?
N2 C1 H1A 117.9 . . ?
C2 C1 H1A 117.9 . . ?
C3 C2 C1 119.1(6) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 118.8(6) . . ?
C2 C3 H3A 120.6 . . ?
C4 C3 H3A 120.6 . . ?
C11 C4 C3 119.0(6) . . ?
C11 C4 C5 118.8(6) . . ?
C3 C4 C5 122.2(6) . . ?
C6 C5 C4 121.7(7) . . ?
C6 C5 H5A 119.1 . . ?
C4 C5 H5A 119.1 . . ?
C5 C6 C7 121.0(6) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
C8 C7 C12 117.4(6) . . ?
C8 C7 C6 123.7(6) . . ?
C12 C7 C6 119.0(6) . . ?
C9 C8 C7 120.3(6) . . ?
C9 C8 H8A 119.9 . . ?
C7 C8 H8A 119.9 . . ?
C8 C9 C10 119.0(6) . . ?
C8 C9 H9A 120.5 . . ?
C10 C9 H9A 120.5 . . ?
N1 C10 C9 122.5(6) . . ?
N1 C10 H10A 118.7 . . ?
C9 C10 H10A 118.7 . . ?
N2 C11 C4 121.9(5) . . ?
N2 C11 C12 118.1(5) . . ?
C4 C11 C12 120.0(5) . . ?
N1 C12 C7 122.6(6) . . ?
N1 C12 C11 117.9(5) . . ?
C7 C12 C11 119.5(6) . . ?
N3 C13 C14 121.9(6) . . ?
N3 C13 H13A 119.1 . . ?
C14 C13 H13A 119.1 . . ?
C15 C14 C13 120.2(7) . . ?
C15 C14 H14A 119.9 . . ?
C13 C14 H14A 119.9 . . ?
C14 C15 C16 119.4(6) . . ?
C14 C15 H15A 120.3 . . ?
C16 C15 H15A 120.3 . . ?
C15 C16 C23 117.0(6) . . ?
C15 C16 C17 123.6(6) . . ?
C23 C16 C17 119.3(6) . . ?
C18 C17 C16 121.7(6) . . ?
C18 C17 H17A 119.2 . . ?
C16 C17 H17A 119.2 . . ?
C17 C18 C19 121.8(7) . . ?
C17 C18 H18A 119.1 . . ?
C19 C18 H18A 119.1 . . ?
C24 C19 C20 117.2(6) . . ?
C24 C19 C18 118.2(6) . . ?
C20 C19 C18 124.6(6) . . ?
C21 C20 C19 120.6(6) . . ?
C21 C20 H20A 119.7 . . ?
C19 C20 H20A 119.7 . . ?
C20 C21 C22 118.0(6) . . ?
C20 C21 H21A 121.0 . . ?
C22 C21 H21A 121.0 . . ?
N4 C22 C21 124.2(6) . . ?
N4 C22 H22A 117.9 . . ?
C21 C22 H22A 117.9 . . ?
N3 C23 C16 122.3(6) . . ?
N3 C23 C24 119.2(5) . . ?
C16 C23 C24 118.4(6) . . ?
N4 C24 C19 123.0(6) . . ?
N4 C24 C23 116.5(5) . . ?
C19 C24 C23 120.4(5) . . ?
O1 C25 O2 120.7(5) . . ?
O1 C25 C26 119.7(5) . . ?
O2 C25 C26 119.6(5) . . ?
O1 C25 Tb1 61.0(3) . . ?
O2 C25 Tb1 60.1(3) . . ?
C26 C25 Tb1 173.5(4) . . ?
C25 C26 C27 114.5(4) . . ?
C25 C26 H26A 108.6 . . ?
C27 C26 H26A 108.6 . . ?
C25 C26 H26B 108.6 . . ?
C27 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C26 C27 C28 114.4(4) . . ?
C26 C27 H27A 108.7 . . ?
C28 C27 H27A 108.7 . . ?
C26 C27 H27B 108.7 . . ?
C28 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C29 C28 C27 115.2(4) . . ?
C29 C28 H28A 108.5 . . ?
C27 C28 H28A 108.5 . . ?
C29 C28 H28B 108.5 . . ?
C27 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
O3 C29 O4 121.7(5) . . ?
O3 C29 C28 120.9(5) . . ?
O4 C29 C28 117.3(5) . . ?
O3 C29 Tb2 59.1(3) . . ?
O4 C29 Tb2 62.6(3) . . ?
C28 C29 Tb2 173.9(4) . . ?
O7 C30 O8 126.1(5) . . ?
O7 C30 C31 117.3(5) . . ?
O8 C30 C31 116.6(5) . . ?
C32 C31 C30 111.4(4) . . ?
C32 C31 H31A 109.3 . . ?
C30 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
C30 C31 H31B 109.3 . . ?
H31A C31 H31B 108.0 . . ?
C31 C32 C33 115.9(5) . . ?
C31 C32 H32A 108.3 . . ?
C33 C32 H32A 108.3 . . ?
C31 C32 H32B 108.3 . . ?
C33 C32 H32B 108.3 . . ?
H32A C32 H32B 107.4 . . ?
C34 C33 C32 109.7(4) . . ?
C34 C33 H33A 109.7 . . ?
C32 C33 H33A 109.7 . . ?
C34 C33 H33B 109.7 . . ?
C32 C33 H33B 109.7 . . ?
H33A C33 H33B 108.2 . . ?
O5 C34 O6 121.4(5) . . ?
O5 C34 C33 119.7(5) . . ?
O6 C34 C33 118.9(5) . . ?
O5 C34 Tb1 54.6(3) . . ?
O6 C34 Tb1 67.2(3) . . ?
C33 C34 Tb1 170.0(3) . . ?
O12 C35 O11 121.4(5) . . ?
O12 C35 C36 118.4(5) . . ?
O11 C35 C36 120.1(5) . . ?
O12 C35 Tb2 62.0(3) . . ?
O11 C35 Tb2 59.5(3) . . ?
C36 C35 Tb2 178.6(4) . . ?
C35 C36 C37 115.0(5) . . ?
C35 C36 H36A 108.5 . . ?
C37 C36 H36A 108.5 . . ?
C35 C36 H36B 108.5 . . ?
C37 C36 H36B 108.5 . . ?
H36A C36 H36B 107.5 . . ?
C38 C37 C36 111.1(4) . . ?
C38 C37 H37A 109.4 . . ?
C36 C37 H37A 109.4 . . ?
C38 C37 H37B 109.4 . . ?
C36 C37 H37B 109.4 . . ?
H37A C37 H37B 108.0 . . ?
C37 C38 C39 115.6(4) . . ?
C37 C38 H38A 108.4 . . ?
C39 C38 H38A 108.4 . . ?
C37 C38 H38B 108.4 . . ?
C39 C38 H38B 108.4 . . ?
H38A C38 H38B 107.4 . . ?
O10 C39 O9 126.4(5) . . ?
O10 C39 C38 118.3(5) . . ?
O9 C39 C38 115.3(5) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.144
