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

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

Data_la_final
_database_code_depnum_ccdc_archive 'CCDC 1052999'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H27 Cl La N5 O14'
_chemical_formula_weight         855.93

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'
Cl Cl 0.1484 0.1585 '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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.55740(10)
_cell_length_b                   12.6056(2)
_cell_length_c                   18.9892(3)
_cell_angle_alpha                106.1310(10)
_cell_angle_beta                 98.9710(10)
_cell_angle_gamma                100.4790(10)
_cell_volume                     2108.78(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11263
_cell_measurement_theta_min      3.1060
_cell_measurement_theta_max      29.0480

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.029
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28175
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         29.31
_reflns_number_total             10138
_reflns_number_gt                8730
_reflns_threshold_expression     >2sigma(I)


_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1105P)²+5.0822P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10138
_refine_ls_number_parameters     447
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0596
_refine_ls_wR_factor_ref         0.1841
_refine_ls_wR_factor_gt          0.1769
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.002 0.500 0.000 596.6 10.1
_platon_squeeze_details          
;
;

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 -0.23318(3) -0.01821(2) -0.003855(13) 0.02508(11) Uani 1 1 d . . .
O1 O -0.3095(4) 0.0227(4) 0.11957(19) 0.0360(8) Uani 1 1 d . . .
O2 O -0.5402(4) 0.0311(3) 0.08820(19) 0.0335(8) Uani 1 1 d . . .
N2 N 0.0004(5) 0.1475(4) 0.6786(2) 0.0284(8) Uani 1 1 d . . .
O5 O -0.0025(4) 0.8890(3) 0.9256(2) 0.0342(8) Uani 1 1 d . . .
O6 O -0.2394(4) 0.8140(4) 0.8833(2) 0.0436(10) Uani 1 1 d . . .
O4 O -0.1421(4) 0.0673(4) 0.9013(2) 0.0409(9) Uani 1 1 d . . .
N3 N -0.0428(5) 0.6089(4) 0.6747(2) 0.0325(9) Uani 1 1 d . . .
O3 O 0.1026(4) 0.1239(4) 0.9354(2) 0.0378(8) Uani 1 1 d . . .
C10 C -0.0780(5) 0.2322(4) 0.5775(3) 0.0266(9) Uani 1 1 d . . .
C11 C -0.0191(5) 0.3483(4) 0.6023(2) 0.0273(9) Uani 1 1 d . . .
C8 C -0.2875(5) 0.2588(5) 0.5016(3) 0.0352(12) Uani 1 1 d . . .
C12 C -0.0914(5) 0.4200(4) 0.5747(3) 0.0287(9) Uani 1 1 d . . .
O8 O -0.2776(5) 0.1809(4) 0.0271(3) 0.0496(11) Uani 1 1 d . . .
C2 C -0.4319(5) 0.0809(4) 0.2171(3) 0.0271(9) Uani 1 1 d . . .
C13 C -0.2265(6) 0.3749(5) 0.5228(3) 0.0345(11) Uani 1 1 d . . .
C4 C -0.5566(5) 0.1403(5) 0.3159(3) 0.0336(11) Uani 1 1 d . . .
H4 H -0.6439 0.1513 0.3317 0.040 Uiso 1 1 calc R . .
O9 O 0.4004(9) -0.3668(7) -0.2887(5) 0.1003(16) Uani 1 1 d . . .
C3 C -0.5579(5) 0.0992(5) 0.2406(3) 0.0325(11) Uani 1 1 d . . .
H3 H -0.6460 0.0833 0.2044 0.039 Uiso 1 1 calc R . .
C9 C -0.2160(5) 0.1852(5) 0.5272(3) 0.0314(10) Uani 1 1 d . . .
C20 C -0.0120(6) 0.1227(5) 0.8160(3) 0.0341(11) Uani 1 1 d . . .
C6 C -0.3049(5) 0.1021(5) 0.2719(3) 0.0306(10) Uani 1 1 d . . .
H6 H -0.2177 0.0869 0.2578 0.037 Uiso 1 1 calc R . .
C18 C -0.1255(5) 0.1451(5) 0.7016(3) 0.0323(10) Uani 1 1 d . . .
H18 H -0.2083 0.1534 0.6707 0.039 Uiso 1 1 calc R . .
C23 C -0.0180(6) 0.1033(5) 0.8914(3) 0.0361(11) Uani 1 1 d . . .
C5 C -0.3083(5) 0.1454(5) 0.3466(3) 0.0328(11) Uani 1 1 d . . .
H5 H -0.2221 0.1614 0.3840 0.039 Uiso 1 1 calc R . .
C1 C -0.4280(5) 0.0404(4) 0.1343(3) 0.0280(9) Uani 1 1 d . . .
C16 C 0.1241(6) 0.3975(5) 0.6595(3) 0.0372(11) Uani 1 1 d . . .
H16A H 0.1463 0.3407 0.6830 0.056 Uiso 1 1 calc R . .
H16B H 0.1167 0.4652 0.6981 0.056 Uiso 1 1 calc R . .
H16C H 0.2021 0.4184 0.6344 0.056 Uiso 1 1 calc R . .
C19 C -0.1345(6) 0.1305(5) 0.7701(3) 0.0343(11) Uani 1 1 d . . .
H19 H -0.2245 0.1259 0.7858 0.041 Uiso 1 1 calc R . .
C17 C 0.0074(6) 0.1533(4) 0.6003(3) 0.0323(10) Uani 1 1 d . . .
H17A H 0.1106 0.1792 0.5984 0.039 Uiso 1 1 calc R . .
H17B H -0.0309 0.0761 0.5637 0.039 Uiso 1 1 calc R . .
C21 C 0.1171(6) 0.1281(6) 0.7908(4) 0.0424(13) Uani 1 1 d . . .
H21 H 0.2029 0.1238 0.8217 0.051 Uiso 1 1 calc R . .
C27 C -0.0835(6) 0.7410(4) 0.8079(3) 0.0334(11) Uani 1 1 d . . .
C26 C 0.0559(6) 0.7371(5) 0.7975(3) 0.0385(12) Uani 1 1 d . . .
H26 H 0.1384 0.7798 0.8365 0.046 Uiso 1 1 calc R . .
C24 C -0.0203(7) 0.5463(5) 0.5998(3) 0.0378(12) Uani 1 1 d . . .
H24A H 0.0857 0.5565 0.6020 0.045 Uiso 1 1 calc R . .
H24B H -0.0608 0.5795 0.5620 0.045 Uiso 1 1 calc R . .
O7 O -0.4221(5) -0.1971(4) -0.0069(3) 0.0577(13) Uani 1 1 d . . .
C30 C -0.1102(6) 0.8196(5) 0.8777(3) 0.0355(11) Uani 1 1 d . . .
C29 C -0.1774(6) 0.6086(5) 0.6851(3) 0.0381(12) Uani 1 1 d . . .
H29 H -0.2583 0.5623 0.6462 0.046 Uiso 1 1 calc R . .
C15 C -0.2789(8) 0.0594(6) 0.5017(4) 0.0597(19) Uani 1 1 d . . .
H15A H -0.3640 0.0394 0.4603 0.090 Uiso 1 1 calc R . .
H15B H -0.3086 0.0368 0.5436 0.090 Uiso 1 1 calc R . .
H15C H -0.2053 0.0196 0.4847 0.090 Uiso 1 1 calc R . .
C28 C -0.2014(6) 0.6740(5) 0.7511(3) 0.0393(12) Uani 1 1 d . . .
H28 H -0.2981 0.6732 0.7576 0.047 Uiso 1 1 calc R . .
C22 C 0.1207(6) 0.1396(5) 0.7213(4) 0.0406(13) Uani 1 1 d . . .
H22 H 0.2085 0.1418 0.7035 0.049 Uiso 1 1 calc R . .
C7 C -0.4373(6) 0.2091(7) 0.4492(3) 0.0485(16) Uani 1 1 d . . .
H7A H -0.4898 0.1461 0.4638 0.058 Uiso 1 1 calc R . .
H7B H -0.4937 0.2684 0.4555 0.058 Uiso 1 1 calc R . .
C25 C 0.0738(6) 0.6709(5) 0.7303(3) 0.0394(12) Uani 1 1 d . . .
H25 H 0.1694 0.6685 0.7228 0.047 Uiso 1 1 calc R . .
C14 C -0.3082(8) 0.4504(7) 0.4897(3) 0.0532(17) Uani 1 1 d . . .
H14A H -0.3403 0.4153 0.4351 0.080 Uiso 1 1 calc R . .
H14B H -0.2431 0.5255 0.5011 0.080 Uiso 1 1 calc R . .
H14C H -0.3933 0.4584 0.5117 0.080 Uiso 1 1 calc R . .
N5 N 0.4224(12) -0.3717(9) -0.2282(6) 0.102(3) Uani 1 1 d . . .
O10 O 0.3844(9) -0.3111(7) -0.1717(5) 0.1003(16) Uani 1 1 d . . .
Cl1 Cl -0.4964(4) -0.1352(3) 0.3197(2) 0.1211(11) Uiso 1 1 d . . .
N4 N -0.1002(4) -0.1603(4) 0.6020(3) 0.0268(9) Uani 1 1 d . . .
O13 O -0.2155(10) -0.211(2) 0.5762(5) 0.341(16) Uani 1 1 d . . .
O12 O -0.0424(14) -0.1547(15) 0.6559(12) 0.269(12) Uani 1 1 d . . .
O14 O -0.0152(18) -0.1215(13) 0.5761(7) 0.192(6) Uani 1 1 d . . .
N1 N -0.4307(5) 0.1650(4) 0.3671(2) 0.0331(9) Uani 1 1 d . . .
O11 O 0.4853(11) -0.4520(9) -0.2152(6) 0.124(3) 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 2.435(3) 2_455 ?
La1 O3 2.466(4) 2_556 ?
La1 O5 2.493(3) 2_566 ?
La1 O1 2.508(3) . ?
La1 O4 2.527(4) 1_554 ?
La1 O6 2.542(4) 1_544 ?
La1 O8 2.544(4) . ?
La1 O7 2.601(5) . ?
La1 O5 3.002(4) 1_544 ?
La1 C30 3.124(5) 1_544 ?
O1 C1 1.252(6) . ?
O2 C1 1.240(6) . ?
O2 La1 2.435(3) 2_455 ?
N2 C22 1.336(7) . ?
N2 C18 1.341(6) . ?
N2 C17 1.521(6) . ?
O5 C30 1.261(6) . ?
O5 La1 2.493(3) 2_566 ?
O5 La1 3.002(4) 1_566 ?
O6 C30 1.247(6) . ?
O6 La1 2.542(4) 1_566 ?
O4 C23 1.253(7) . ?
O4 La1 2.527(4) 1_556 ?
N3 C29 1.331(7) . ?
N3 C25 1.351(7) . ?
N3 C24 1.492(6) . ?
O3 C23 1.251(6) . ?
O3 La1 2.466(4) 2_556 ?
C10 C11 1.385(7) . ?
C10 C9 1.419(6) . ?
C10 C17 1.504(7) . ?
C11 C12 1.394(7) . ?
C11 C16 1.514(7) . ?
C8 C13 1.390(8) . ?
C8 C9 1.393(8) . ?
C8 C7 1.522(7) . ?
C12 C13 1.410(7) . ?
C12 C24 1.518(8) . ?
C2 C3 1.383(6) . ?
C2 C6 1.401(6) . ?
C2 C1 1.520(6) . ?
C13 C14 1.536(8) . ?
C4 N1 1.350(6) . ?
C4 C3 1.376(7) . ?
O9 N5 1.156(11) . ?
C9 C15 1.499(8) . ?
C20 C19 1.383(7) . ?
C20 C21 1.388(7) . ?
C20 C23 1.526(7) . ?
C6 C5 1.379(7) . ?
C18 C19 1.376(7) . ?
C5 N1 1.333(6) . ?
C21 C22 1.373(8) . ?
C27 C28 1.385(7) . ?
C27 C26 1.385(7) . ?
C27 C30 1.507(7) . ?
C26 C25 1.371(8) . ?
C30 La1 3.124(5) 1_566 ?
C29 C28 1.373(7) . ?
C7 N1 1.518(6) . ?
N5 O10 1.278(12) . ?
N5 O11 1.327(13) . ?
N4 O12 1.063(16) . ?
N4 O13 1.125(14) . ?
N4 O14 1.120(19) . ?

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 O3 143.70(14) 2_455 2_556 ?
O2 La1 O5 144.82(13) 2_455 2_566 ?
O3 La1 O5 71.35(13) 2_556 2_566 ?
O2 La1 O1 100.68(11) 2_455 . ?
O3 La1 O1 75.71(12) 2_556 . ?
O5 La1 O1 83.04(12) 2_566 . ?
O2 La1 O4 77.97(12) 2_455 1_554 ?
O3 La1 O4 125.35(12) 2_556 1_554 ?
O5 La1 O4 79.57(13) 2_566 1_554 ?
O1 La1 O4 145.18(14) . 1_554 ?
O2 La1 O6 77.94(12) 2_455 1_544 ?
O3 La1 O6 82.45(14) 2_556 1_544 ?
O5 La1 O6 121.06(12) 2_566 1_544 ?
O1 La1 O6 139.98(15) . 1_544 ?
O4 La1 O6 74.37(15) 1_554 1_544 ?
O2 La1 O8 73.27(13) 2_455 . ?
O3 La1 O8 135.83(14) 2_556 . ?
O5 La1 O8 74.53(13) 2_566 . ?
O1 La1 O8 73.05(15) . . ?
O4 La1 O8 73.33(15) 1_554 . ?
O6 La1 O8 140.29(15) 1_544 . ?
O2 La1 O7 72.05(14) 2_455 . ?
O3 La1 O7 72.57(14) 2_556 . ?
O5 La1 O7 140.07(15) 2_566 . ?
O1 La1 O7 71.97(16) . . ?
O4 La1 O7 136.88(16) 1_554 . ?
O6 La1 O7 69.63(16) 1_544 . ?
O8 La1 O7 124.07(15) . . ?
O2 La1 O5 116.98(10) 2_455 1_544 ?
O3 La1 O5 65.19(12) 2_556 1_544 ?
O5 La1 O5 74.93(12) 2_566 1_544 ?
O1 La1 O5 139.44(11) . 1_544 ?
O4 La1 O5 63.03(12) 1_554 1_544 ?
O6 La1 O5 46.13(11) 1_544 1_544 ?
O8 La1 O5 130.12(14) . 1_544 ?
O7 La1 O5 104.56(13) . 1_544 ?
O2 La1 C30 96.48(13) 2_455 1_544 ?
O3 La1 C30 74.02(14) 2_556 1_544 ?
O5 La1 C30 98.53(13) 2_566 1_544 ?
O1 La1 C30 147.35(14) . 1_544 ?
O4 La1 C30 65.71(15) 1_554 1_544 ?
O6 La1 C30 22.56(13) 1_544 1_544 ?
O8 La1 C30 139.03(16) . 1_544 ?
O7 La1 C30 87.44(16) . 1_544 ?
O5 La1 C30 23.64(11) 1_544 1_544 ?
C1 O1 La1 129.5(3) . . ?
C1 O2 La1 176.5(3) . 2_455 ?
C22 N2 C18 122.0(4) . . ?
C22 N2 C17 117.8(4) . . ?
C18 N2 C17 120.1(4) . . ?
C30 O5 La1 170.6(3) . 2_566 ?
C30 O5 La1 83.7(3) . 1_566 ?
La1 O5 La1 105.07(12) 2_566 1_566 ?
C30 O6 La1 106.0(3) . 1_566 ?
C23 O4 La1 134.0(3) . 1_556 ?
C29 N3 C25 120.4(4) . . ?
C29 N3 C24 119.9(5) . . ?
C25 N3 C24 119.7(4) . . ?
C23 O3 La1 136.0(4) . 2_556 ?
C11 C10 C9 120.6(5) . . ?
C11 C10 C17 120.3(4) . . ?
C9 C10 C17 119.0(5) . . ?
C10 C11 C12 120.2(4) . . ?
C10 C11 C16 119.8(5) . . ?
C12 C11 C16 120.0(5) . . ?
C13 C8 C9 122.1(5) . . ?
C13 C8 C7 119.7(5) . . ?
C9 C8 C7 118.2(5) . . ?
C11 C12 C13 120.2(5) . . ?
C11 C12 C24 119.0(5) . . ?
C13 C12 C24 120.8(5) . . ?
C3 C2 C6 118.2(4) . . ?
C3 C2 C1 121.9(4) . . ?
C6 C2 C1 119.9(4) . . ?
C8 C13 C12 118.7(5) . . ?
C8 C13 C14 119.4(5) . . ?
C12 C13 C14 121.9(6) . . ?
N1 C4 C3 119.7(4) . . ?
C4 C3 C2 120.5(4) . . ?
C8 C9 C10 118.1(5) . . ?
C8 C9 C15 122.1(5) . . ?
C10 C9 C15 119.8(6) . . ?
C19 C20 C21 118.7(5) . . ?
C19 C20 C23 121.4(5) . . ?
C21 C20 C23 119.8(5) . . ?
C5 C6 C2 119.1(4) . . ?
N2 C18 C19 119.9(5) . . ?
O3 C23 O4 128.0(5) . . ?
O3 C23 C20 115.6(5) . . ?
O4 C23 C20 116.4(5) . . ?
N1 C5 C6 121.0(4) . . ?
O2 C1 O1 126.3(4) . . ?
O2 C1 C2 117.3(4) . . ?
O1 C1 C2 116.4(4) . . ?
C18 C19 C20 119.7(5) . . ?
C10 C17 N2 113.0(4) . . ?
C22 C21 C20 119.9(5) . . ?
C28 C27 C26 118.8(5) . . ?
C28 C27 C30 119.2(5) . . ?
C26 C27 C30 122.0(5) . . ?
C25 C26 C27 119.4(5) . . ?
N3 C24 C12 113.0(4) . . ?
O6 C30 O5 123.9(5) . . ?
O6 C30 C27 117.3(5) . . ?
O5 C30 C27 118.8(4) . . ?
O6 C30 La1 51.5(3) . 1_566 ?
O5 C30 La1 72.7(3) . 1_566 ?
C27 C30 La1 166.3(4) . 1_566 ?
N3 C29 C28 121.2(5) . . ?
C29 C28 C27 119.4(5) . . ?
N2 C22 C21 119.8(5) . . ?
N1 C7 C8 113.2(4) . . ?
N3 C25 C26 120.7(5) . . ?
O9 N5 O10 126.6(11) . . ?
O9 N5 O11 118.4(11) . . ?
O10 N5 O11 114.9(9) . . ?
O12 N4 O13 123.8(11) . . ?
O12 N4 O14 104.5(11) . . ?
O13 N4 O14 130.6(10) . . ?
C5 N1 C4 121.3(4) . . ?
C5 N1 C7 121.6(4) . . ?
C4 N1 C7 117.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        29.31
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.945
_refine_diff_density_min         -2.558
_refine_diff_density_rms         0.161
####################################################################### 
# 
# 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_ce_final
_database_code_depnum_ccdc_archive 'CCDC 1053000'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H27 Ce Cl N5 O14'
_chemical_formula_weight         857.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Ce Ce -1.8482 9.6596 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   9.5251(3)
_cell_length_b                   12.5605(4)
_cell_length_c                   18.9231(6)
_cell_angle_alpha                106.077(3)
_cell_angle_beta                 98.874(3)
_cell_angle_gamma                100.643(3)
_cell_volume                     2086.80(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8857
_cell_measurement_theta_min      3.7610
_cell_measurement_theta_max      73.5410

_exptl_crystal_description       block
_exptl_crystal_colour            orange-yellow
_exptl_crystal_size_max          0.0793
_exptl_crystal_size_mid          0.0542
_exptl_crystal_size_min          0.0321
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             858
_exptl_absorpt_coefficient_mu    9.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_T_max  0.736
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15762
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.77
_diffrn_reflns_theta_max         73.63
_reflns_number_total             8067
_reflns_number_gt                7472
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1275P)²+1.6970P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8067
_refine_ls_number_parameters     439
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1698
_refine_ls_wR_factor_gt          0.1652
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.001 0.500 0.000 560.6 138.6
_platon_squeeze_details          
;
;
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 -0.76587(2) -0.98221(2) -0.996089(12) 0.02684(13) Uani 1 1 d . . .
O1 O -0.5422(4) -0.9706(4) -0.91245(19) 0.0353(8) Uani 1 1 d . . .
O2 O -0.3112(4) -0.9797(4) -0.88135(19) 0.0385(9) Uani 1 1 d . . .
O5 O 0.0020(4) -0.1087(3) -0.0758(2) 0.0388(8) Uani 1 1 d . . .
N1 N -0.4319(5) -0.8407(5) -0.6329(3) 0.0390(6) Uani 1 1 d . . .
O6 O -0.2368(4) -0.1811(4) -0.1164(2) 0.0463(10) Uani 1 1 d . . .
N2 N 0.0051(5) -0.8470(4) -0.3178(3) 0.0325(9) Uani 1 1 d . . .
O3 O 0.1063(4) -0.8732(4) -0.0613(2) 0.0427(9) Uani 1 1 d . . .
O4 O -0.1396(4) -0.9293(4) -0.0951(2) 0.0433(9) Uani 1 1 d . . .
N3 N -0.0451(5) -0.3896(4) -0.3269(3) 0.0375(10) Uani 1 1 d . . .
C10 C -0.0759(5) -0.7676(4) -0.4215(3) 0.0298(10) Uani 1 1 d . . .
C30 C -0.1085(6) -0.1766(5) -0.1228(3) 0.0383(11) Uani 1 1 d . . .
C2 C -0.4338(5) -0.9234(4) -0.7831(3) 0.0296(10) Uani 1 1 d . . .
C12 C -0.0946(6) -0.5811(5) -0.4267(3) 0.0346(11) Uani 1 1 d . . .
C1 C -0.4299(5) -0.9621(4) -0.8660(3) 0.0304(10) Uani 1 1 d . . .
C11 C -0.0191(5) -0.6515(4) -0.3977(3) 0.0302(10) Uani 1 1 d . . .
O7 O -0.5771(5) -0.8018(4) -0.9895(3) 0.0586(12) Uani 1 1 d . . .
C6 C -0.5601(6) -0.9036(6) -0.7596(3) 0.0416(8) Uani 1 1 d . . .
H6 H -0.6482 -0.9181 -0.7957 0.050 Uiso 1 1 calc R . .
C8 C -0.2894(6) -0.7466(6) -0.4983(3) 0.0416(8) Uani 1 1 d . . .
C3 C -0.3077(5) -0.9039(5) -0.7288(3) 0.0338(10) Uani 1 1 d . . .
H3 H -0.2205 -0.9192 -0.7433 0.041 Uiso 1 1 calc R . .
C5 C -0.5576(6) -0.8630(5) -0.6843(3) 0.0390(12) Uani 1 1 d . . .
H5 H -0.6445 -0.8505 -0.6682 0.047 Uiso 1 1 calc R . .
C13 C -0.2293(6) -0.6273(5) -0.4771(3) 0.0385(12) Uani 1 1 d . . .
C4 C -0.3100(6) -0.8619(6) -0.6532(3) 0.0387(12) Uani 1 1 d . . .
H4 H -0.2241 -0.8483 -0.6158 0.046 Uiso 1 1 calc R . .
C27 C -0.0838(6) -0.2580(5) -0.1947(3) 0.0391(12) Uani 1 1 d . . .
C20 C -0.0087(6) -0.8737(5) -0.1808(3) 0.0375(11) Uani 1 1 d . . .
C9 C -0.2138(6) -0.8168(5) -0.4717(3) 0.0360(11) Uani 1 1 d . . .
C22 C -0.1211(6) -0.8522(5) -0.2955(3) 0.0391(11) Uani 1 1 d . . .
H22 H -0.2050 -0.8470 -0.3275 0.047 Uiso 1 1 calc R . .
C17 C 0.0111(6) -0.8450(5) -0.3979(3) 0.0359(11) Uani 1 1 d . . .
H17A H 0.1143 -0.8191 -0.4005 0.043 Uiso 1 1 calc R . .
H17B H -0.0275 -0.9234 -0.4335 0.043 Uiso 1 1 calc R . .
C19 C 0.1224(7) -0.8665(6) -0.2054(4) 0.0463(14) Uani 1 1 d . . .
H19 H 0.2081 -0.8700 -0.1738 0.056 Uiso 1 1 calc R . .
C21 C -0.1306(6) -0.8652(5) -0.2269(3) 0.0382(11) Uani 1 1 d . . .
H21 H -0.2207 -0.8683 -0.2109 0.046 Uiso 1 1 calc R . .
C16 C 0.1241(6) -0.5986(5) -0.3406(3) 0.0424(13) Uani 1 1 d . . .
H16A H 0.1627 -0.6586 -0.3264 0.064 Uiso 1 1 calc R . .
H16B H 0.1080 -0.5448 -0.2958 0.064 Uiso 1 1 calc R . .
H16C H 0.1945 -0.5580 -0.3626 0.064 Uiso 1 1 calc R . .
C26 C 0.0549(7) -0.2606(5) -0.2053(4) 0.0460(14) Uani 1 1 d . . .
H26 H 0.1377 -0.2165 -0.1665 0.055 Uiso 1 1 calc R . .
C28 C -0.2025(6) -0.3238(5) -0.2502(3) 0.0432(13) Uani 1 1 d . . .
H28 H -0.2988 -0.3231 -0.2428 0.052 Uiso 1 1 calc R . .
C25 C 0.0728(7) -0.3274(5) -0.2722(4) 0.0438(13) Uani 1 1 d . . .
H25 H 0.1683 -0.3299 -0.2802 0.053 Uiso 1 1 calc R . .
C29 C -0.1814(7) -0.3904(5) -0.3163(3) 0.0443(13) Uani 1 1 d . . .
H29 H -0.2632 -0.4373 -0.3548 0.053 Uiso 1 1 calc R . .
C24 C -0.0250(8) -0.4546(5) -0.4028(3) 0.0446(13) Uani 1 1 d . . .
H24A H 0.0811 -0.4438 -0.4016 0.053 Uiso 1 1 calc R . .
H24B H -0.0677 -0.4224 -0.4409 0.053 Uiso 1 1 calc R . .
C23 C -0.0140(6) -0.8928(5) -0.1051(4) 0.0415(12) Uani 1 1 d . . .
C18 C 0.1288(6) -0.8545(6) -0.2749(4) 0.0464(14) Uani 1 1 d . . .
H18 H 0.2172 -0.8515 -0.2925 0.056 Uiso 1 1 calc R . .
C7 C -0.4389(6) -0.7976(6) -0.5496(3) 0.0416(8) Uani 1 1 d . . .
H7A H -0.4971 -0.7393 -0.5429 0.050 Uiso 1 1 calc R . .
H7B H -0.4895 -0.8619 -0.5351 0.050 Uiso 1 1 calc R . .
C14 C -0.3154(9) -0.5562(8) -0.5118(4) 0.0583(18) Uani 1 1 d . . .
H14A H -0.3971 -0.5449 -0.4871 0.087 Uiso 1 1 calc R . .
H14B H -0.3535 -0.5962 -0.5657 0.087 Uiso 1 1 calc R . .
H14C H -0.2510 -0.4819 -0.5048 0.087 Uiso 1 1 calc R . .
C15 C -0.2732(9) -0.9454(7) -0.4967(4) 0.064(2) Uani 1 1 d . . .
H15A H -0.3751 -0.9651 -0.5244 0.096 Uiso 1 1 calc R . .
H15B H -0.2685 -0.9715 -0.4523 0.096 Uiso 1 1 calc R . .
H15C H -0.2142 -0.9826 -0.5294 0.096 Uiso 1 1 calc R . .
O8 O -0.7231(5) -1.1799(4) -1.0280(3) 0.0506(11) Uani 1 1 d . . .
N4 N -0.1015(6) -0.1611(5) -0.3985(3) 0.0390(6) Uani 1 1 d D . .
O14 O 0.3778(8) -0.3157(9) -0.1719(4) 0.104(3) Uani 1 1 d . . .
O12 O 0.4011(6) -0.3633(5) -0.2889(3) 0.0634(14) Uani 1 1 d . . .
N5 N 0.4196(5) -0.3701(5) -0.2242(3) 0.0390(6) Uani 1 1 d . . .
O13 O 0.4868(10) -0.4454(8) -0.2125(6) 0.107(3) Uani 1 1 d . . .
O11 O -0.2207(10) -0.2472(10) -0.4270(5) 0.120(3) Uani 1 1 d . . .
O10 O -0.0131(12) -0.1149(10) -0.4290(7) 0.216(9) Uani 1 1 d D . .
O9 O -0.0587(15) -0.1289(12) -0.3292(3) 0.218(9) Uani 1 1 d D . .
Cl1 Cl -0.4988(2) -1.1479(3) -0.67610(19) 0.1066(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
Ce1 O1 2.405(3) . ?
Ce1 O3 2.444(4) 1_454 ?
Ce1 O5 2.457(4) 1_444 ?
Ce1 O2 2.487(3) 2_433 ?
Ce1 O4 2.489(4) 2_434 ?
Ce1 O6 2.507(4) 2_444 ?
Ce1 O8 2.513(4) . ?
Ce1 O7 2.580(5) . ?
O1 C1 1.243(6) . ?
O2 C1 1.253(6) . ?
O2 Ce1 2.487(3) 2_433 ?
O5 C30 1.259(7) . ?
O5 Ce1 2.457(4) 1_666 ?
N1 C4 1.327(7) . ?
N1 C5 1.351(7) . ?
N1 C7 1.534(7) . ?
O6 C30 1.239(7) . ?
O6 Ce1 2.507(4) 2_444 ?
N2 C22 1.330(7) . ?
N2 C18 1.358(8) . ?
N2 C17 1.532(7) . ?
O3 C23 1.245(7) . ?
O3 Ce1 2.443(4) 1_656 ?
O4 C23 1.263(7) . ?
O4 Ce1 2.489(4) 2_434 ?
N3 C29 1.342(8) . ?
N3 C25 1.345(8) . ?
N3 C24 1.504(7) . ?
C10 C11 1.375(7) . ?
C10 C9 1.414(7) . ?
C10 C17 1.501(8) . ?
C30 C27 1.539(8) . ?
C2 C6 1.385(7) . ?
C2 C3 1.390(7) . ?
C2 C1 1.517(6) . ?
C12 C13 1.390(8) . ?
C12 C11 1.409(8) . ?
C12 C24 1.512(8) . ?
C11 C16 1.510(7) . ?
C6 C5 1.369(7) . ?
C8 C9 1.384(9) . ?
C8 C13 1.418(9) . ?
C8 C7 1.508(7) . ?
C3 C4 1.386(7) . ?
C13 C14 1.527(9) . ?
C27 C28 1.368(8) . ?
C27 C26 1.371(8) . ?
C20 C21 1.380(8) . ?
C20 C19 1.394(8) . ?
C20 C23 1.524(8) . ?
C9 C15 1.520(9) . ?
C22 C21 1.368(8) . ?
C19 C18 1.375(9) . ?
C26 C25 1.366(8) . ?
C28 C29 1.366(8) . ?
N4 O10 1.2384(10) . ?
N4 O9 1.2384(10) . ?
N4 O11 1.335(12) . ?
O14 N5 1.206(8) . ?
O12 N5 1.238(8) . ?
N5 O13 1.284(9) . ?

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 Ce1 O3 143.14(15) . 1_454 ?
O1 Ce1 O5 145.22(14) . 1_444 ?
O3 Ce1 O5 71.51(14) 1_454 1_444 ?
O1 Ce1 O2 100.81(12) . 2_433 ?
O3 Ce1 O2 76.28(14) 1_454 2_433 ?
O5 Ce1 O2 82.33(13) 1_444 2_433 ?
O1 Ce1 O4 78.61(13) . 2_434 ?
O3 Ce1 O4 124.68(13) 1_454 2_434 ?
O5 Ce1 O4 79.53(15) 1_444 2_434 ?
O2 Ce1 O4 144.85(16) 2_433 2_434 ?
O1 Ce1 O6 78.28(13) . 2_444 ?
O3 Ce1 O6 81.52(15) 1_454 2_444 ?
O5 Ce1 O6 120.83(13) 1_444 2_444 ?
O2 Ce1 O6 140.45(16) 2_433 2_444 ?
O4 Ce1 O6 74.38(16) 2_434 2_444 ?
O1 Ce1 O8 73.39(14) . . ?
O3 Ce1 O8 136.69(15) 1_454 . ?
O5 Ce1 O8 74.53(14) 1_444 . ?
O2 Ce1 O8 73.26(16) 2_433 . ?
O4 Ce1 O8 72.99(16) 2_434 . ?
O6 Ce1 O8 140.14(16) 2_444 . ?
O1 Ce1 O7 71.77(15) . . ?
O3 Ce1 O7 72.36(15) 1_454 . ?
O5 Ce1 O7 139.93(16) 1_444 . ?
O2 Ce1 O7 72.78(17) 2_433 . ?
O4 Ce1 O7 136.84(17) 2_434 . ?
O6 Ce1 O7 69.46(17) 2_444 . ?
O8 Ce1 O7 124.71(16) . . ?
C1 O1 Ce1 176.6(3) . . ?
C1 O2 Ce1 129.8(3) . 2_433 ?
C30 O5 Ce1 173.1(4) . 1_666 ?
C4 N1 C5 121.6(5) . . ?
C4 N1 C7 121.3(5) . . ?
C5 N1 C7 117.0(4) . . ?
C30 O6 Ce1 107.6(3) . 2_444 ?
C22 N2 C18 122.6(5) . . ?
C22 N2 C17 120.0(5) . . ?
C18 N2 C17 117.1(5) . . ?
C23 O3 Ce1 135.5(4) . 1_656 ?
C23 O4 Ce1 134.8(4) . 2_434 ?
C29 N3 C25 121.3(5) . . ?
C29 N3 C24 118.9(5) . . ?
C25 N3 C24 119.7(5) . . ?
C11 C10 C9 120.7(5) . . ?
C11 C10 C17 120.5(5) . . ?
C9 C10 C17 118.8(5) . . ?
O6 C30 O5 124.7(5) . . ?
O6 C30 C27 117.2(5) . . ?
O5 C30 C27 118.0(5) . . ?
C6 C2 C3 118.5(4) . . ?
C6 C2 C1 121.5(4) . . ?
C3 C2 C1 119.9(4) . . ?
C13 C12 C11 120.5(5) . . ?
C13 C12 C24 120.9(5) . . ?
C11 C12 C24 118.6(5) . . ?
O1 C1 O2 125.7(4) . . ?
O1 C1 C2 117.7(4) . . ?
O2 C1 C2 116.5(4) . . ?
C10 C11 C12 119.9(5) . . ?
C10 C11 C16 120.6(5) . . ?
C12 C11 C16 119.5(5) . . ?
C5 C6 C2 119.9(5) . . ?
C9 C8 C13 121.1(5) . . ?
C9 C8 C7 119.4(6) . . ?
C13 C8 C7 119.6(6) . . ?
C4 C3 C2 119.5(5) . . ?
N1 C5 C6 120.2(5) . . ?
C12 C13 C8 118.7(5) . . ?
C12 C13 C14 123.2(6) . . ?
C8 C13 C14 118.1(6) . . ?
N1 C4 C3 120.2(5) . . ?
C28 C27 C26 120.0(6) . . ?
C28 C27 C30 119.0(5) . . ?
C26 C27 C30 120.9(5) . . ?
C21 C20 C19 118.7(5) . . ?
C21 C20 C23 122.0(5) . . ?
C19 C20 C23 119.3(5) . . ?
C8 C9 C10 119.0(5) . . ?
C8 C9 C15 121.8(6) . . ?
C10 C9 C15 119.2(6) . . ?
N2 C22 C21 120.4(5) . . ?
C10 C17 N2 112.2(4) . . ?
C18 C19 C20 120.5(6) . . ?
C22 C21 C20 119.6(5) . . ?
C25 C26 C27 119.3(6) . . ?
C29 C28 C27 119.5(6) . . ?
N3 C25 C26 119.9(5) . . ?
N3 C29 C28 120.0(6) . . ?
N3 C24 C12 113.5(4) . . ?
O3 C23 O4 127.8(5) . . ?
O3 C23 C20 116.1(5) . . ?
O4 C23 C20 116.1(5) . . ?
N2 C18 C19 118.1(5) . . ?
C8 C7 N1 112.6(4) . . ?
O10 N4 O9 111.6(9) . . ?
O10 N4 O11 131.8(9) . . ?
O9 N4 O11 116.0(7) . . ?
O14 N5 O12 126.8(7) . . ?
O14 N5 O13 116.8(7) . . ?
O12 N5 O13 116.3(6) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        73.63
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         2.613
_refine_diff_density_min         -2.380
_refine_diff_density_rms         0.148
####################################################################### 
# 
# 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_pr_final
_database_code_depnum_ccdc_archive 'CCDC 1053001'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H27 Cl N5 O14 Pr'
_chemical_formula_weight         857.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -2.4164 10.2820 '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                   9.5300(3)
_cell_length_b                   12.5401(4)
_cell_length_c                   18.8719(6)
_cell_angle_alpha                105.932(3)
_cell_angle_beta                 98.860(2)
_cell_angle_gamma                100.482(2)
_cell_volume                     2082.30(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8734
_cell_measurement_theta_min      4.8020
_cell_measurement_theta_max      73.1470

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.0723
_exptl_crystal_size_mid          0.0451
_exptl_crystal_size_min          0.0273
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             860
_exptl_absorpt_coefficient_mu    10.111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.458
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15822
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.77
_diffrn_reflns_theta_max         73.85
_reflns_number_total             8023
_reflns_number_gt                7213
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1196P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8023
_refine_ls_number_parameters     439
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1637
_refine_ls_wR_factor_gt          0.1593
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.028 0.000 0.500 563.0 154.4
_platon_squeeze_details          
;
;

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
Pr1 Pr -0.23418(3) 0.48222(2) 0.496364(12) 0.02345(12) Uani 1 1 d . . .
O6 O -0.5437(4) -0.4702(4) -0.41333(19) 0.0332(8) Uani 1 1 d . . .
O5 O -0.3133(4) -0.4802(4) -0.38256(19) 0.0346(9) Uani 1 1 d . . .
N2 N 0.0035(5) -0.3481(4) 0.1816(3) 0.0266(9) Uani 1 1 d . . .
N3 N -0.4327(5) -0.3371(5) -0.1337(3) 0.0331(6) Uani 1 1 d . . .
N1 N -0.0430(5) 0.1100(4) 0.1741(3) 0.0309(10) Uani 1 1 d . . .
O1 O -0.2332(4) 0.3198(4) 0.3856(2) 0.0397(10) Uani 1 1 d . . .
C8 C -0.0946(6) -0.0799(5) 0.0733(3) 0.0282(11) Uani 1 1 d . . .
C9 C -0.0201(5) -0.1508(4) 0.1016(3) 0.0252(10) Uani 1 1 d . . .
C30 C -0.4319(6) -0.4619(5) -0.3673(3) 0.0263(10) Uani 1 1 d . . .
O2 O 0.0063(4) 0.3913(3) 0.4249(2) 0.0342(8) Uani 1 1 d . . .
C10 C -0.0774(6) -0.2681(4) 0.0780(3) 0.0265(10) Uani 1 1 d . . .
O3 O -0.1388(4) -0.4306(4) 0.4050(2) 0.0394(10) Uani 1 1 d . . .
C13 C -0.2274(6) -0.1242(5) 0.0225(3) 0.0330(12) Uani 1 1 d . . .
C2 C -0.0793(6) 0.2434(5) 0.3074(3) 0.0308(11) Uani 1 1 d . . .
C12 C -0.2898(6) -0.2443(6) 0.0013(3) 0.0345(12) Uani 1 1 d . . .
C26 C -0.3086(6) -0.4018(5) -0.2293(3) 0.0297(11) Uani 1 1 d . . .
H26 H -0.2216 -0.4180 -0.2437 0.036 Uiso 1 1 calc R . .
C28 C -0.5605(6) -0.4021(5) -0.2600(3) 0.0314(11) Uani 1 1 d . . .
H28 H -0.6490 -0.4172 -0.2959 0.038 Uiso 1 1 calc R . .
O8 O -0.4204(5) 0.3028(4) 0.4912(3) 0.0534(12) Uani 1 1 d . . .
C27 C -0.4343(5) -0.4214(5) -0.2837(3) 0.0268(10) Uani 1 1 d . . .
C1 C -0.1042(6) 0.3239(5) 0.3785(3) 0.0343(12) Uani 1 1 d . . .
C29 C -0.5571(6) -0.3610(5) -0.1844(3) 0.0342(12) Uani 1 1 d . . .
H29 H -0.6441 -0.3495 -0.1680 0.041 Uiso 1 1 calc R . .
C11 C -0.2135(6) -0.3155(5) 0.0284(3) 0.0313(11) Uani 1 1 d . . .
C15 C 0.1244(6) -0.1005(5) 0.1588(3) 0.0363(12) Uani 1 1 d . . .
H15A H 0.1624 -0.1621 0.1714 0.055 Uiso 1 1 calc R . .
H15B H 0.1091 -0.0482 0.2047 0.055 Uiso 1 1 calc R . .
H15C H 0.1947 -0.0586 0.1374 0.055 Uiso 1 1 calc R . .
C21 C -0.1309(6) -0.3657(5) 0.2736(3) 0.0341(12) Uani 1 1 d . . .
H21 H -0.2205 -0.3686 0.2899 0.041 Uiso 1 1 calc R . .
C20 C -0.0104(6) -0.3748(5) 0.3187(3) 0.0333(12) Uani 1 1 d . . .
C17 C 0.0091(6) -0.3455(5) 0.1011(3) 0.0323(11) Uani 1 1 d . . .
H17A H 0.1120 -0.3198 0.0983 0.039 Uiso 1 1 calc R . .
H17B H -0.0296 -0.4237 0.0654 0.039 Uiso 1 1 calc R . .
C6 C 0.0579(7) 0.2368(5) 0.2966(4) 0.0393(13) Uani 1 1 d . . .
H6 H 0.1412 0.2775 0.3357 0.047 Uiso 1 1 calc R . .
C25 C -0.3110(6) -0.3585(5) -0.1541(3) 0.0333(12) Uani 1 1 d . . .
H25 H -0.2250 -0.3440 -0.1166 0.040 Uiso 1 1 calc R . .
C5 C 0.0738(7) 0.1708(5) 0.2288(3) 0.0381(13) Uani 1 1 d . . .
H5 H 0.1691 0.1682 0.2203 0.046 Uiso 1 1 calc R . .
C7 C -0.0245(7) 0.0458(5) 0.0971(3) 0.0345(12) Uani 1 1 d . . .
H7A H -0.0679 0.0789 0.0595 0.041 Uiso 1 1 calc R . .
H7B H 0.0811 0.0560 0.0975 0.041 Uiso 1 1 calc R . .
C19 C 0.1207(7) -0.3688(6) 0.2940(4) 0.0418(14) Uani 1 1 d . . .
H19 H 0.2061 -0.3737 0.3252 0.050 Uiso 1 1 calc R . .
C18 C 0.1254(7) -0.3558(6) 0.2243(4) 0.0434(15) Uani 1 1 d . . .
H18 H 0.2136 -0.3524 0.2066 0.052 Uiso 1 1 calc R . .
C22 C -0.1227(6) -0.3523(5) 0.2039(3) 0.0321(11) Uani 1 1 d . . .
H22 H -0.2064 -0.3460 0.1722 0.039 Uiso 1 1 calc R . .
C3 C -0.2007(6) 0.1771(5) 0.2516(3) 0.0367(13) Uani 1 1 d . . .
H3 H -0.2967 0.1778 0.2594 0.044 Uiso 1 1 calc R . .
C14 C -0.3133(9) -0.0520(8) -0.0112(3) 0.054(2) Uani 1 1 d . . .
H14A H -0.3988 -0.0456 0.0112 0.081 Uiso 1 1 calc R . .
H14B H -0.3455 -0.0882 -0.0659 0.081 Uiso 1 1 calc R . .
H14C H -0.2508 0.0243 -0.0006 0.081 Uiso 1 1 calc R . .
C4 C -0.1785(7) 0.1095(5) 0.1840(3) 0.0365(12) Uani 1 1 d . . .
H4 H -0.2598 0.0632 0.1451 0.044 Uiso 1 1 calc R . .
C24 C -0.4383(6) -0.2928(5) -0.0497(3) 0.0331(6) Uani 1 1 d . . .
H24A H -0.4947 -0.2331 -0.0429 0.040 Uiso 1 1 calc R . .
H24B H -0.4904 -0.3563 -0.0349 0.040 Uiso 1 1 calc R . .
C16 C -0.2763(8) -0.4432(7) 0.0033(4) 0.057(2) Uani 1 1 d . . .
H16A H -0.2036 -0.4828 -0.0158 0.086 Uiso 1 1 calc R . .
H16B H -0.3641 -0.4632 -0.0368 0.086 Uiso 1 1 calc R . .
H16C H -0.3017 -0.4661 0.0462 0.086 Uiso 1 1 calc R . .
O4 O 0.1067(4) -0.3745(4) 0.4386(2) 0.0373(9) Uani 1 1 d . . .
C23 C -0.0155(6) -0.3941(5) 0.3951(3) 0.0331(6) Uani 1 1 d . . .
O7 O -0.2785(5) 0.6773(4) 0.5261(3) 0.0472(11) Uani 1 1 d . . .
Cl1 Cl -0.5006(3) -0.3583(3) 0.1779(2) 0.1159(12) Uani 1 1 d . . .
N5 N -0.0987(5) 0.3391(5) 0.1022(3) 0.0331(6) Uani 1 1 d . . .
O11 O -0.5976(5) 0.1346(4) 0.2116(3) 0.0500(11) Uani 1 1 d . . .
O9 O -0.5086(10) 0.0526(9) 0.2875(6) 0.120(2) Uani 1 1 d . . .
O10 O -0.6217(7) 0.1830(8) 0.3285(3) 0.092(3) Uani 1 1 d . . .
N4 N -0.5787(8) 0.1271(6) 0.2758(5) 0.0628(17) Uani 1 1 d . . .
O12 O -0.101(4) 0.3873(13) 0.0775(9) 0.57(4) Uani 1 1 d . . .
O14 O -0.0567(10) 0.3707(9) 0.1692(6) 0.120(2) Uani 1 1 d . . .
O13 O -0.2198(9) 0.2522(9) 0.0727(4) 0.106(3) 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
Pr1 O6 2.385(4) 2_455 ?
Pr1 O4 2.420(4) 2_556 ?
Pr1 O2 2.429(4) 2_566 ?
Pr1 O5 2.466(3) 1_566 ?
Pr1 O3 2.481(4) 1_565 ?
Pr1 O7 2.485(5) . ?
Pr1 O1 2.489(4) . ?
Pr1 O8 2.568(5) . ?
O6 C30 1.235(6) . ?
O6 Pr1 2.385(4) 2_455 ?
O5 C30 1.253(6) . ?
O5 Pr1 2.466(3) 1_544 ?
N2 C22 1.331(7) . ?
N2 C18 1.342(8) . ?
N2 C17 1.538(6) . ?
N3 C25 1.326(7) . ?
N3 C29 1.332(7) . ?
N3 C24 1.542(7) . ?
N1 C4 1.333(7) . ?
N1 C5 1.338(8) . ?
N1 C7 1.508(7) . ?
O1 C1 1.250(7) . ?
C8 C13 1.381(8) . ?
C8 C9 1.397(8) . ?
C8 C7 1.506(8) . ?
C9 C10 1.390(7) . ?
C9 C15 1.521(7) . ?
C30 C27 1.525(6) . ?
O2 C1 1.255(7) . ?
O2 Pr1 2.429(4) 2_566 ?
C10 C11 1.397(7) . ?
C10 C17 1.492(8) . ?
O3 C23 1.242(7) . ?
O3 Pr1 2.481(4) 1_545 ?
C13 C12 1.432(9) . ?
C13 C14 1.524(8) . ?
C2 C6 1.368(8) . ?
C2 C3 1.390(8) . ?
C2 C1 1.523(7) . ?
C12 C11 1.401(9) . ?
C12 C24 1.498(8) . ?
C26 C25 1.379(7) . ?
C26 C27 1.388(7) . ?
C28 C29 1.371(7) . ?
C28 C27 1.385(7) . ?
C11 C16 1.514(9) . ?
C21 C20 1.363(8) . ?
C21 C22 1.382(8) . ?
C20 C19 1.395(7) . ?
C20 C23 1.533(7) . ?
C6 C5 1.367(8) . ?
C19 C18 1.376(9) . ?
C3 C4 1.395(8) . ?
O4 C23 1.258(7) . ?
O4 Pr1 2.420(4) 2_556 ?
N5 O12 0.858(16) . ?
N5 O14 1.195(11) . ?
N5 O13 1.357(10) . ?
O11 N4 1.229(9) . ?
O9 N4 1.289(12) . ?
O10 N4 1.223(9) . ?
O12 O14 1.794(17) . ?

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 Pr1 O4 143.06(15) 2_455 2_556 ?
O6 Pr1 O2 144.95(15) 2_455 2_566 ?
O4 Pr1 O2 71.84(14) 2_556 2_566 ?
O6 Pr1 O5 100.14(12) 2_455 1_566 ?
O4 Pr1 O5 76.78(13) 2_556 1_566 ?
O2 Pr1 O5 82.73(13) 2_566 1_566 ?
O6 Pr1 O3 79.13(13) 2_455 1_565 ?
O4 Pr1 O3 124.09(13) 2_556 1_565 ?
O2 Pr1 O3 79.25(15) 2_566 1_565 ?
O5 Pr1 O3 145.18(16) 1_566 1_565 ?
O6 Pr1 O7 73.01(15) 2_455 . ?
O4 Pr1 O7 137.27(15) 2_556 . ?
O2 Pr1 O7 74.45(14) 2_566 . ?
O5 Pr1 O7 73.57(16) 1_566 . ?
O3 Pr1 O7 73.00(16) 1_565 . ?
O6 Pr1 O1 78.95(14) 2_455 . ?
O4 Pr1 O1 80.91(15) 2_556 . ?
O2 Pr1 O1 120.57(13) 2_566 . ?
O5 Pr1 O1 140.32(15) 1_566 . ?
O3 Pr1 O1 74.19(16) 1_565 . ?
O7 Pr1 O1 140.03(16) . . ?
O6 Pr1 O8 71.90(16) 2_455 . ?
O4 Pr1 O8 72.20(15) 2_556 . ?
O2 Pr1 O8 139.86(16) 2_566 . ?
O5 Pr1 O8 72.22(16) 1_566 . ?
O3 Pr1 O8 137.18(17) 1_565 . ?
O7 Pr1 O8 124.71(16) . . ?
O1 Pr1 O8 69.88(16) . . ?
C30 O6 Pr1 176.8(3) . 2_455 ?
C30 O5 Pr1 130.2(3) . 1_544 ?
C22 N2 C18 122.7(5) . . ?
C22 N2 C17 119.5(5) . . ?
C18 N2 C17 117.5(4) . . ?
C25 N3 C29 121.5(5) . . ?
C25 N3 C24 120.9(5) . . ?
C29 N3 C24 117.4(4) . . ?
C4 N1 C5 121.5(5) . . ?
C4 N1 C7 117.8(5) . . ?
C5 N1 C7 120.5(5) . . ?
C1 O1 Pr1 108.6(3) . . ?
C13 C8 C9 121.0(5) . . ?
C13 C8 C7 120.4(5) . . ?
C9 C8 C7 118.6(5) . . ?
C10 C9 C8 120.5(5) . . ?
C10 C9 C15 119.2(5) . . ?
C8 C9 C15 120.4(5) . . ?
O6 C30 O5 126.2(5) . . ?
O6 C30 C27 117.8(4) . . ?
O5 C30 C27 116.0(4) . . ?
C1 O2 Pr1 173.8(4) . 2_566 ?
C9 C10 C11 120.2(5) . . ?
C9 C10 C17 120.7(5) . . ?
C11 C10 C17 119.0(5) . . ?
C23 O3 Pr1 135.3(4) . 1_545 ?
C8 C13 C12 118.5(5) . . ?
C8 C13 C14 123.6(6) . . ?
C12 C13 C14 117.9(6) . . ?
C6 C2 C3 119.7(5) . . ?
C6 C2 C1 122.0(5) . . ?
C3 C2 C1 118.3(5) . . ?
C11 C12 C13 120.4(5) . . ?
C11 C12 C24 120.3(5) . . ?
C13 C12 C24 119.3(5) . . ?
C25 C26 C27 119.4(5) . . ?
C29 C28 C27 119.7(5) . . ?
C28 C27 C26 118.3(5) . . ?
C28 C27 C30 121.3(5) . . ?
C26 C27 C30 120.4(4) . . ?
O1 C1 O2 124.8(5) . . ?
O1 C1 C2 117.7(5) . . ?
O2 C1 C2 117.5(5) . . ?
N3 C29 C28 120.5(5) . . ?
C10 C11 C12 119.4(5) . . ?
C10 C11 C16 120.1(6) . . ?
C12 C11 C16 120.4(6) . . ?
C20 C21 C22 120.0(5) . . ?
C21 C20 C19 119.1(5) . . ?
C21 C20 C23 121.8(5) . . ?
C19 C20 C23 119.0(5) . . ?
C10 C17 N2 112.2(4) . . ?
C5 C6 C2 119.3(6) . . ?
N3 C25 C26 120.5(5) . . ?
N1 C5 C6 120.9(5) . . ?
C8 C7 N1 113.1(4) . . ?
C18 C19 C20 119.6(6) . . ?
N2 C18 C19 119.1(5) . . ?
N2 C22 C21 119.5(5) . . ?
C2 C3 C4 118.6(5) . . ?
N1 C4 C3 119.8(6) . . ?
C12 C24 N3 113.0(4) . . ?
C23 O4 Pr1 135.5(4) . 2_556 ?
O3 C23 O4 128.6(5) . . ?
O3 C23 C20 116.1(5) . . ?
O4 C23 C20 115.3(5) . . ?
O12 N5 O14 120.9(12) . . ?
O12 N5 O13 109(2) . . ?
O14 N5 O13 117.0(7) . . ?
O10 N4 O11 125.6(8) . . ?
O10 N4 O9 118.0(9) . . ?
O11 N4 O9 116.3(8) . . ?
N5 O12 O14 34.9(8) . . ?
N5 O14 O12 24.2(6) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        73.85
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         2.582
_refine_diff_density_min         -1.685
_refine_diff_density_rms         0.145
####################################################################### 
# 
# 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_Nd_final
_database_code_depnum_ccdc_archive 'CCDC 1053002'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H27 Cl N5 Nd O14'
_chemical_formula_weight         861.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.52970(10)
_cell_length_b                   12.6996(3)
_cell_length_c                   18.8203(3)
_cell_angle_alpha                106.347(2)
_cell_angle_beta                 98.6300(10)
_cell_angle_gamma                100.059(2)
_cell_volume                     2103.64(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12617
_cell_measurement_theta_min      3.0950
_cell_measurement_theta_max      28.0620

_exptl_crystal_description       block
_exptl_crystal_colour            blue-violet
_exptl_crystal_size_max          0.0803
_exptl_crystal_size_mid          0.0511
_exptl_crystal_size_min          0.0337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             862
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20573
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         28.27
_reflns_number_total             8882
_reflns_number_gt                7985
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1224P)²+7.6186P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8882
_refine_ls_number_parameters     433
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0634
_refine_ls_wR_factor_ref         0.1857
_refine_ls_wR_factor_gt          0.1799
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.006 0.500 0.000 588.8 32.1
_platon_squeeze_details          
;
;
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
Nd1 Nd -0.23335(3) 0.98368(2) -0.003316(13) 0.01757(13) Uani 1 1 d . . .
O6 O -0.5458(4) 0.0301(4) -0.9132(2) 0.0256(9) Uani 1 1 d . . .
N2 N 0.0005(5) 0.1483(4) -0.3201(3) 0.0226(10) Uani 1 1 d . . .
O5 O -0.3134(4) 0.0244(4) -0.8826(2) 0.0305(10) Uani 1 1 d . . .
O3 O -0.1392(4) 0.0652(4) -0.0960(2) 0.0297(9) Uani 1 1 d . . .
O2 O 0.0087(4) 0.8909(4) -0.0739(2) 0.0271(9) Uani 1 1 d . . .
N1 N -0.0413(6) 0.6073(4) -0.3254(3) 0.0262(10) Uani 1 1 d . . .
O1 O -0.2302(5) 0.8229(4) -0.1122(2) 0.0313(10) Uani 1 1 d . . .
O4 O 0.1053(4) 0.1200(4) -0.0635(2) 0.0283(9) Uani 1 1 d . . .
N3 N -0.4337(5) 0.1672(5) -0.6334(3) 0.0272(11) Uani 1 1 d . . .
C10 C -0.0801(6) 0.2317(5) -0.4220(3) 0.0213(11) Uani 1 1 d . . .
C30 C -0.4325(6) 0.0414(5) -0.8671(3) 0.0205(10) Uani 1 1 d . . .
C27 C -0.4350(6) 0.0825(5) -0.7837(3) 0.0212(11) Uani 1 1 d . . .
C8 C -0.0946(6) 0.4182(5) -0.4259(3) 0.0221(11) Uani 1 1 d . . .
C28 C -0.5624(6) 0.1021(5) -0.7598(3) 0.0254(12) Uani 1 1 d . . .
H28 H -0.6512 0.0861 -0.7956 0.030 Uiso 1 1 calc R . .
O9 O 0.4002(9) -0.3685(8) -0.2899(5) 0.0829(10) Uani 1 1 d . . .
O7 O -0.4161(5) 0.8096(4) -0.0062(3) 0.0434(12) Uani 1 1 d . . .
C25 C -0.3125(6) 0.1457(5) -0.6539(3) 0.0269(12) Uani 1 1 d . . .
H25 H -0.2270 0.1597 -0.6163 0.032 Uiso 1 1 calc R . .
C13 C -0.2277(7) 0.3753(6) -0.4766(3) 0.0278(12) Uani 1 1 d . . .
C9 C -0.0205(6) 0.3467(5) -0.3975(3) 0.0206(10) Uani 1 1 d . . .
C12 C -0.2904(6) 0.2580(6) -0.4977(3) 0.0295(13) Uani 1 1 d . . .
C11 C -0.2180(6) 0.1861(5) -0.4715(3) 0.0269(12) Uani 1 1 d . . .
C1 C -0.1025(6) 0.8235(5) -0.1200(3) 0.0247(11) Uani 1 1 d . . .
C20 C -0.0114(6) 0.1185(5) -0.1833(3) 0.0263(12) Uani 1 1 d . . .
O8 O -0.2798(6) 1.1753(4) 0.0252(3) 0.0463(13) Uani 1 1 d . . .
C26 C -0.3090(6) 0.1028(5) -0.7296(3) 0.0238(11) Uani 1 1 d . . .
H26 H -0.2216 0.0874 -0.7442 0.029 Uiso 1 1 calc R . .
C6 C 0.0592(7) 0.7376(5) -0.2029(4) 0.0309(13) Uani 1 1 d . . .
H6 H 0.1423 0.7811 -0.1647 0.037 Uiso 1 1 calc R . .
C23 C -0.0167(7) 0.1002(6) -0.1071(3) 0.0305(9) Uani 1 1 d . . .
C3 C -0.1981(7) 0.6756(5) -0.2467(3) 0.0301(13) Uani 1 1 d . . .
H3 H -0.2942 0.6760 -0.2388 0.036 Uiso 1 1 calc R . .
C15 C 0.1230(7) 0.3962(6) -0.3405(4) 0.0319(13) Uani 1 1 d . . .
H15A H 0.1576 0.3360 -0.3251 0.048 Uiso 1 1 calc R . .
H15B H 0.1090 0.4525 -0.2960 0.048 Uiso 1 1 calc R . .
H15C H 0.1952 0.4320 -0.3636 0.048 Uiso 1 1 calc R . .
C17 C 0.0067(7) 0.1537(5) -0.3996(3) 0.0280(12) Uani 1 1 d . . .
H17A H 0.1096 0.1792 -0.4020 0.034 Uiso 1 1 calc R . .
H17B H -0.0310 0.0770 -0.4364 0.034 Uiso 1 1 calc R . .
C18 C -0.1258(6) 0.1436(5) -0.2969(4) 0.0280(12) Uani 1 1 d . . .
H18 H -0.2097 0.1503 -0.3281 0.034 Uiso 1 1 calc R . .
C2 C -0.0793(6) 0.7425(5) -0.1909(3) 0.0255(12) Uani 1 1 d . . .
C29 C -0.5572(6) 0.1452(6) -0.6832(3) 0.0297(13) Uani 1 1 d . . .
H29 H -0.6431 0.1592 -0.6661 0.036 Uiso 1 1 calc R . .
C21 C 0.1180(7) 0.1252(6) -0.2085(4) 0.0339(14) Uani 1 1 d . . .
H21 H 0.2039 0.1208 -0.1776 0.041 Uiso 1 1 calc R . .
C19 C -0.1336(6) 0.1293(5) -0.2284(3) 0.0267(12) Uani 1 1 d . . .
H19 H -0.2229 0.1267 -0.2116 0.032 Uiso 1 1 calc R . .
C5 C 0.0759(7) 0.6692(5) -0.2707(4) 0.0321(13) Uani 1 1 d . . .
H5 H 0.1710 0.6656 -0.2791 0.039 Uiso 1 1 calc R . .
C4 C -0.1770(7) 0.6085(5) -0.3138(3) 0.0279(12) Uani 1 1 d . . .
H4 H -0.2587 0.5627 -0.3521 0.033 Uiso 1 1 calc R . .
C7 C -0.0210(7) 0.5431(5) -0.4012(3) 0.0294(13) Uani 1 1 d . . .
H7A H 0.0847 0.5510 -0.3999 0.035 Uiso 1 1 calc R . .
H7B H -0.0609 0.5763 -0.4393 0.035 Uiso 1 1 calc R . .
C24 C -0.4409(7) 0.2109(6) -0.5496(3) 0.0305(9) Uani 1 1 d . . .
H24A H -0.4966 0.2706 -0.5425 0.037 Uiso 1 1 calc R . .
H24B H -0.4938 0.1485 -0.5351 0.037 Uiso 1 1 calc R . .
C14 C -0.3109(9) 0.4484(8) -0.5095(4) 0.0441(18) Uani 1 1 d . . .
H14A H -0.3924 0.4603 -0.4844 0.066 Uiso 1 1 calc R . .
H14B H -0.3484 0.4108 -0.5640 0.066 Uiso 1 1 calc R . .
H14C H -0.2454 0.5214 -0.5014 0.066 Uiso 1 1 calc R . .
C22 C 0.1217(7) 0.1382(6) -0.2786(4) 0.0327(14) Uani 1 1 d . . .
H22 H 0.2090 0.1401 -0.2972 0.039 Uiso 1 1 calc R . .
C16 C -0.2824(9) 0.0609(7) -0.4972(4) 0.049(2) Uani 1 1 d . . .
H16A H -0.3811 0.0446 -0.5276 0.074 Uiso 1 1 calc R . .
H16B H -0.2863 0.0354 -0.4528 0.074 Uiso 1 1 calc R . .
H16C H -0.2215 0.0212 -0.5278 0.074 Uiso 1 1 calc R . .
Cl1 Cl -0.5021(3) 0.1332(3) -0.3197(2) 0.0901(10) Uani 1 1 d . . .
O10 O 0.3820(7) -0.3145(8) -0.1716(4) 0.078(2) Uani 1 1 d . . .
N4 N 0.4233(8) -0.3734(6) -0.2250(5) 0.0578(19) Uani 1 1 d . . .
O11 O 0.4900(8) -0.4459(7) -0.2139(5) 0.080(2) Uani 1 1 d . . .
N5 N -0.0992(11) -0.1636(10) -0.4009(6) 0.0829(10) Uani 1 1 d . . .
O13 O -0.2145(9) -0.2539(8) -0.4274(5) 0.0829(10) Uani 1 1 d . . .
O14 O -0.0084(9) -0.1088(8) -0.4258(5) 0.0829(10) Uani 1 1 d . . .
O12 O -0.0461(9) -0.1418(8) -0.3331(5) 0.0829(10) 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
Nd1 O6 2.377(4) 2_464 ?
Nd1 O2 2.409(4) 2_575 ?
Nd1 O4 2.415(4) 2_565 ?
Nd1 O5 2.450(4) 1_566 ?
Nd1 O1 2.461(4) . ?
Nd1 O3 2.466(4) 1_565 ?
Nd1 O8 2.474(5) . ?
Nd1 O7 2.546(5) . ?
O6 C30 1.239(7) . ?
O6 Nd1 2.377(4) 2_464 ?
N2 C18 1.338(7) . ?
N2 C22 1.340(8) . ?
N2 C17 1.526(7) . ?
O5 C30 1.254(7) . ?
O5 Nd1 2.450(4) 1_544 ?
O3 C23 1.244(7) . ?
O3 Nd1 2.466(4) 1_545 ?
O2 C1 1.264(7) . ?
O2 Nd1 2.409(4) 2_575 ?
N1 C4 1.346(8) . ?
N1 C5 1.348(8) . ?
N1 C7 1.490(7) . ?
O1 C1 1.247(7) . ?
O4 C23 1.259(7) . ?
O4 Nd1 2.415(4) 2_565 ?
N3 C25 1.320(8) . ?
N3 C29 1.322(8) . ?
N3 C24 1.535(7) . ?
C10 C9 1.386(8) . ?
C10 C11 1.412(8) . ?
C10 C17 1.503(8) . ?
C30 C27 1.513(7) . ?
C27 C26 1.387(8) . ?
C27 C28 1.395(7) . ?
C8 C13 1.385(8) . ?
C8 C9 1.412(8) . ?
C8 C7 1.523(8) . ?
C28 C29 1.381(8) . ?
O9 N4 1.230(11) . ?
C25 C26 1.381(8) . ?
C13 C12 1.420(10) . ?
C13 C14 1.521(9) . ?
C9 C15 1.515(8) . ?
C12 C11 1.387(9) . ?
C12 C24 1.523(8) . ?
C11 C16 1.509(10) . ?
C1 C2 1.510(8) . ?
C20 C21 1.384(8) . ?
C20 C19 1.386(8) . ?
C20 C23 1.522(8) . ?
C6 C5 1.376(9) . ?
C6 C2 1.382(8) . ?
C3 C4 1.375(8) . ?
C3 C2 1.383(8) . ?
C18 C19 1.362(8) . ?
C21 C22 1.381(9) . ?
O10 N4 1.234(10) . ?
N4 O11 1.252(10) . ?
N5 O12 1.233(12) . ?
N5 O14 1.244(12) . ?
N5 O13 1.358(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Nd1 O2 144.72(15) 2_464 2_575 ?
O6 Nd1 O4 143.16(15) 2_464 2_565 ?
O2 Nd1 O4 71.99(15) 2_575 2_565 ?
O6 Nd1 O5 99.97(13) 2_464 1_566 ?
O2 Nd1 O5 83.01(14) 2_575 1_566 ?
O4 Nd1 O5 76.88(15) 2_565 1_566 ?
O6 Nd1 O1 78.95(14) 2_464 . ?
O2 Nd1 O1 120.48(14) 2_575 . ?
O4 Nd1 O1 81.08(15) 2_565 . ?
O5 Nd1 O1 140.47(16) 1_566 . ?
O6 Nd1 O3 79.08(14) 2_464 1_565 ?
O2 Nd1 O3 79.11(15) 2_575 1_565 ?
O4 Nd1 O3 124.05(14) 2_565 1_565 ?
O5 Nd1 O3 145.29(16) 1_566 1_565 ?
O1 Nd1 O3 73.90(16) . 1_565 ?
O6 Nd1 O8 73.09(15) 2_464 . ?
O2 Nd1 O8 74.30(15) 2_575 . ?
O4 Nd1 O8 136.95(16) 2_565 . ?
O5 Nd1 O8 73.14(18) 1_566 . ?
O1 Nd1 O8 140.23(17) . . ?
O3 Nd1 O8 73.48(18) 1_565 . ?
O6 Nd1 O7 72.09(16) 2_464 . ?
O2 Nd1 O7 139.89(16) 2_575 . ?
O4 Nd1 O7 72.12(15) 2_565 . ?
O5 Nd1 O7 71.95(17) 1_566 . ?
O1 Nd1 O7 70.21(17) . . ?
O3 Nd1 O7 137.30(17) 1_565 . ?
O8 Nd1 O7 124.45(18) . . ?
C30 O6 Nd1 176.8(4) . 2_464 ?
C18 N2 C22 122.4(5) . . ?
C18 N2 C17 120.0(5) . . ?
C22 N2 C17 117.3(5) . . ?
C30 O5 Nd1 131.0(3) . 1_544 ?
C23 O3 Nd1 136.0(4) . 1_545 ?
C1 O2 Nd1 174.1(4) . 2_575 ?
C4 N1 C5 120.5(5) . . ?
C4 N1 C7 119.5(5) . . ?
C5 N1 C7 119.9(5) . . ?
C1 O1 Nd1 110.0(3) . . ?
C23 O4 Nd1 135.8(4) . 2_565 ?
C25 N3 C29 122.2(5) . . ?
C25 N3 C24 121.2(5) . . ?
C29 N3 C24 116.4(5) . . ?
C9 C10 C11 120.7(5) . . ?
C9 C10 C17 119.7(5) . . ?
C11 C10 C17 119.4(5) . . ?
O6 C30 O5 126.2(5) . . ?
O6 C30 C27 117.7(5) . . ?
O5 C30 C27 116.1(5) . . ?
C26 C27 C28 118.8(5) . . ?
C26 C27 C30 120.1(5) . . ?
C28 C27 C30 121.0(5) . . ?
C13 C8 C9 120.9(5) . . ?
C13 C8 C7 121.2(5) . . ?
C9 C8 C7 117.9(5) . . ?
C29 C28 C27 118.8(5) . . ?
N3 C25 C26 120.6(5) . . ?
C8 C13 C12 118.6(6) . . ?
C8 C13 C14 122.9(6) . . ?
C12 C13 C14 118.5(6) . . ?
C10 C9 C8 119.5(5) . . ?
C10 C9 C15 120.6(5) . . ?
C8 C9 C15 119.8(5) . . ?
C11 C12 C13 121.3(5) . . ?
C11 C12 C24 119.5(6) . . ?
C13 C12 C24 119.1(6) . . ?
C12 C11 C10 118.8(6) . . ?
C12 C11 C16 121.0(6) . . ?
C10 C11 C16 120.2(6) . . ?
O1 C1 O2 124.1(5) . . ?
O1 C1 C2 118.0(5) . . ?
O2 C1 C2 117.8(5) . . ?
C21 C20 C19 118.7(5) . . ?
C21 C20 C23 119.7(5) . . ?
C19 C20 C23 121.6(5) . . ?
C25 C26 C27 118.9(5) . . ?
C5 C6 C2 119.5(6) . . ?
O3 C23 O4 127.8(5) . . ?
O3 C23 C20 116.9(5) . . ?
O4 C23 C20 115.3(5) . . ?
C4 C3 C2 119.9(6) . . ?
C10 C17 N2 112.9(5) . . ?
N2 C18 C19 119.8(5) . . ?
C6 C2 C3 118.9(5) . . ?
C6 C2 C1 121.2(5) . . ?
C3 C2 C1 119.9(5) . . ?
N3 C29 C28 120.6(5) . . ?
C22 C21 C20 119.7(6) . . ?
C18 C19 C20 120.0(5) . . ?
N1 C5 C6 120.8(6) . . ?
N1 C4 C3 120.4(5) . . ?
N1 C7 C8 113.2(5) . . ?
C12 C24 N3 112.5(4) . . ?
N2 C22 C21 119.2(5) . . ?
O9 N4 O10 124.6(9) . . ?
O9 N4 O11 116.6(9) . . ?
O10 N4 O11 118.8(9) . . ?
O12 N5 O14 105.6(10) . . ?
O12 N5 O13 113.1(9) . . ?
O14 N5 O13 139.0(11) . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        28.27
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         5.186
_refine_diff_density_min         -3.434
_refine_diff_density_rms         0.196
####################################################################### 
# 
# 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_eu_final
_database_code_depnum_ccdc_archive 'CCDC 1053003'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H27 Cl Eu N5 O14'
_chemical_formula_weight         868.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   9.4977(3)
_cell_length_b                   12.6270(4)
_cell_length_c                   18.7072(4)
_cell_angle_alpha                106.096(2)
_cell_angle_beta                 98.452(2)
_cell_angle_gamma                100.275(2)
_cell_volume                     2074.70(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10191
_cell_measurement_theta_min      3.7150
_cell_measurement_theta_max      73.5240

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.0810
_exptl_crystal_size_mid          0.0594
_exptl_crystal_size_min          0.0302
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             868
_exptl_absorpt_coefficient_mu    11.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15562
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.74
_diffrn_reflns_theta_max         73.91
_reflns_number_total             8035
_reflns_number_gt                7542
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1957P)²+0.6267P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8035
_refine_ls_number_parameters     423
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0847
_refine_ls_wR_factor_ref         0.2270
_refine_ls_wR_factor_gt          0.2217
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.005 0.500 0.000 604.9 206.9
_platon_squeeze_details          
;
;
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.23517(3) 0.01618(2) 0.003045(15) 0.01193(17) Uani 1 1 d . . .
O1 O 0.4505(5) 0.0286(4) 0.0857(2) 0.0238(9) Uani 1 1 d . . .
N2 N 1.0053(7) 0.1521(5) 0.6826(4) 0.0290(12) Uani 1 1 d . . .
N3 N 0.9564(7) 0.6082(4) 0.6732(3) 0.0239(12) Uani 1 1 d . . .
O2 O 0.6825(5) 0.0212(5) 0.1155(3) 0.0287(11) Uani 1 1 d . . .
O6 O 0.7765(5) 0.8287(4) 0.8891(3) 0.0269(10) Uani 1 1 d . . .
O5 O 1.0183(5) 0.8912(4) 0.9251(3) 0.0245(9) Uani 1 1 d . . .
O4 O 0.8628(5) 0.0672(4) 0.9075(3) 0.0272(10) Uani 1 1 d . . .
O3 O 1.1079(5) 0.1214(4) 0.9409(3) 0.0273(10) Uani 1 1 d . . .
C10 C 0.9198(7) 0.2324(5) 0.5784(3) 0.0202(12) Uani 1 1 d . . .
C30 C 0.9038(7) 0.8281(6) 0.8806(4) 0.0229(13) Uani 1 1 d . . .
O7 O 0.4152(6) 0.1907(5) 0.0089(3) 0.0369(12) Uani 1 1 d . . .
C2 C 0.5630(7) 0.0792(7) 0.2156(4) 0.0276(7) Uani 1 1 d . . .
O11 O 0.4032(7) -0.3668(6) -0.2879(4) 0.0440(15) Uani 1 1 d . . .
N1 N 0.5659(7) 0.1651(6) 0.3671(3) 0.0281(13) Uani 1 1 d . . .
C12 C 0.9028(8) 0.4184(6) 0.5735(4) 0.0229(13) Uani 1 1 d . . .
C8 C 0.7066(7) 0.2556(7) 0.5028(4) 0.0276(7) Uani 1 1 d . . .
C3 C 0.4364(7) 0.1006(6) 0.2399(3) 0.0224(13) Uani 1 1 d . . .
H3 H 0.3485 0.0881 0.2040 0.027 Uiso 1 1 calc R . .
C13 C 0.7685(8) 0.3718(6) 0.5229(4) 0.0273(14) Uani 1 1 d . . .
C11 C 0.9787(6) 0.3476(5) 0.6026(3) 0.0158(11) Uani 1 1 d . . .
O8 O 0.2830(6) -0.1729(5) -0.0256(3) 0.0404(13) Uani 1 1 d . . .
C6 C 0.6888(7) 0.0984(6) 0.2696(4) 0.0228(12) Uani 1 1 d . . .
H6 H 0.7764 0.0835 0.2545 0.027 Uiso 1 1 calc R . .
C1 C 0.5648(6) 0.0386(5) 0.1316(3) 0.0172(11) Uani 1 1 d . . .
C5 C 0.6854(7) 0.1398(6) 0.3463(4) 0.0264(14) Uani 1 1 d . . .
H5 H 0.7700 0.1500 0.3839 0.032 Uiso 1 1 calc R . .
C26 C 1.0615(8) 0.7394(6) 0.7966(4) 0.0281(14) Uani 1 1 d . . .
H26 H 1.1455 0.7821 0.8347 0.034 Uiso 1 1 calc R . .
C27 C 0.9218(8) 0.7436(6) 0.8081(4) 0.0280(14) Uani 1 1 d . . .
C22 C 0.8787(7) 0.1465(6) 0.7051(4) 0.0244(13) Uani 1 1 d . . .
H22 H 0.7948 0.1518 0.6729 0.029 Uiso 1 1 calc R . .
C4 C 0.4401(8) 0.1403(7) 0.3168(4) 0.0281(15) Uani 1 1 d . . .
H4 H 0.3527 0.1502 0.3341 0.034 Uiso 1 1 calc R . .
C21 C 0.8681(7) 0.1328(6) 0.7761(4) 0.0240(13) Uani 1 1 d . . .
H21 H 0.7787 0.1306 0.7933 0.029 Uiso 1 1 calc R . .
C28 C 0.8020(8) 0.6775(6) 0.7542(4) 0.0314(15) Uani 1 1 d . . .
H28 H 0.7064 0.6782 0.7634 0.038 Uiso 1 1 calc R . .
C19 C 1.1220(8) 0.1314(7) 0.7950(5) 0.0318(16) Uani 1 1 d . . .
H19 H 1.2093 0.1291 0.8261 0.038 Uiso 1 1 calc R . .
C20 C 0.9940(7) 0.1225(6) 0.8209(4) 0.0262(14) Uani 1 1 d . . .
C9 C 0.7834(8) 0.1836(6) 0.5293(4) 0.0272(14) Uani 1 1 d . . .
C16 C 1.1221(7) 0.4001(6) 0.6579(4) 0.0276(7) Uani 1 1 d . . .
H16A H 1.1614 0.3409 0.6729 0.041 Uiso 1 1 calc R . .
H16B H 1.1074 0.4552 0.7031 0.041 Uiso 1 1 calc R . .
H16C H 1.1913 0.4386 0.6340 0.041 Uiso 1 1 calc R . .
C17 C 1.0083(8) 0.1552(5) 0.6021(4) 0.0249(13) Uani 1 1 d . . .
H17A H 1.1110 0.1806 0.5984 0.030 Uiso 1 1 calc R . .
H17B H 0.9700 0.0775 0.5663 0.030 Uiso 1 1 calc R . .
O9 O 0.3886(13) -0.3078(12) -0.1695(6) 0.099(2) Uani 1 1 d . . .
N4 N 0.4242(10) -0.3718(8) -0.2240(6) 0.056(2) Uani 1 1 d . . .
C25 C 1.0739(8) 0.6695(6) 0.7263(4) 0.0296(15) Uani 1 1 d . . .
H25 H 1.1684 0.6658 0.7163 0.036 Uiso 1 1 calc R . .
C24 C 0.9745(9) 0.5434(6) 0.5970(4) 0.0305(15) Uani 1 1 d . . .
H24A H 1.0803 0.5522 0.5972 0.037 Uiso 1 1 calc R . .
H24B H 0.9322 0.5760 0.5588 0.037 Uiso 1 1 calc R . .
C29 C 0.8214(9) 0.6109(6) 0.6873(5) 0.0330(16) Uani 1 1 d . . .
H29 H 0.7382 0.5652 0.6496 0.040 Uiso 1 1 calc R . .
Cl1 Cl 0.5209(14) -0.5678(13) -0.3631(7) 0.247(5) Uiso 1 1 d . . .
C18 C 1.1250(8) 0.1437(7) 0.7236(5) 0.0327(16) Uani 1 1 d . . .
H18 H 1.2127 0.1461 0.7047 0.039 Uiso 1 1 calc R . .
C23 C 0.9870(7) 0.1023(6) 0.8961(4) 0.0249(13) Uani 1 1 d . . .
C14 C 0.6824(11) 0.4472(9) 0.4898(5) 0.047(2) Uani 1 1 d . . .
H14A H 0.6131 0.4703 0.5216 0.070 Uiso 1 1 calc R . .
H14B H 0.6289 0.4041 0.4379 0.070 Uiso 1 1 calc R . .
H14C H 0.7510 0.5145 0.4890 0.070 Uiso 1 1 calc R . .
C7 C 0.5567(7) 0.2051(7) 0.4510(4) 0.0276(7) Uani 1 1 d . . .
H7A H 0.4972 0.2626 0.4587 0.033 Uiso 1 1 calc R . .
H7B H 0.5070 0.1402 0.4650 0.033 Uiso 1 1 calc R . .
C15 C 0.7215(11) 0.0580(9) 0.5043(5) 0.051(3) Uani 1 1 d . . .
H15A H 0.7796 0.0195 0.4709 0.076 Uiso 1 1 calc R . .
H15B H 0.6200 0.0408 0.4767 0.076 Uiso 1 1 calc R . .
H15C H 0.7246 0.0318 0.5490 0.076 Uiso 1 1 calc R . .
O10 O 0.4899(12) -0.4467(10) -0.2130(7) 0.089(3) Uani 1 1 d . . .
N5 N -0.0992(7) -0.1627(5) -0.3996(4) 0.0283(12) Uiso 1 1 d . . .
O12 O -0.2151(12) -0.2529(12) -0.4282(6) 0.099(2) Uani 1 1 d . . .
O14 O -0.0138(19) -0.1127(14) -0.4276(8) 0.129(5) Uani 1 1 d . . .
O13 O -0.0534(13) -0.1320(12) -0.3259(6) 0.099(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.327(5) . ?
Eu1 O5 2.354(4) 1_444 ?
Eu1 O3 2.366(5) 1_454 ?
Eu1 O2 2.411(5) 2_655 ?
Eu1 O4 2.420(4) 2_656 ?
Eu1 O6 2.422(4) 2_666 ?
Eu1 O8 2.438(5) . ?
Eu1 O7 2.502(5) . ?
Eu1 C30 3.122(6) 2_666 ?
Eu1 Eu1 4.3942(5) 2 ?
O1 C1 1.245(8) . ?
N2 C18 1.312(10) . ?
N2 C22 1.328(9) . ?
N2 C17 1.522(9) . ?
N3 C25 1.330(10) . ?
N3 C29 1.351(10) . ?
N3 C24 1.485(8) . ?
O2 C1 1.241(8) . ?
O2 Eu1 2.411(5) 2_655 ?
O6 C30 1.244(8) . ?
O6 Eu1 2.423(4) 2_666 ?
O5 C30 1.252(8) . ?
O5 Eu1 2.354(4) 1_666 ?
O4 C23 1.254(8) . ?
O4 Eu1 2.420(4) 2_656 ?
O3 C23 1.259(8) . ?
O3 Eu1 2.366(5) 1_656 ?
C10 C11 1.379(8) . ?
C10 C9 1.398(9) . ?
C10 C17 1.509(9) . ?
C30 C27 1.529(9) . ?
C30 Eu1 3.122(6) 2_666 ?
C2 C6 1.383(9) . ?
C2 C3 1.391(10) . ?
C2 C1 1.516(8) . ?
O11 N4 1.203(12) . ?
N1 C5 1.316(10) . ?
N1 C4 1.335(10) . ?
N1 C7 1.532(8) . ?
C12 C13 1.391(10) . ?
C12 C11 1.414(9) . ?
C12 C24 1.514(10) . ?
C8 C13 1.401(11) . ?
C8 C9 1.409(11) . ?
C8 C7 1.515(9) . ?
C3 C4 1.379(9) . ?
C13 C14 1.554(10) . ?
C11 C16 1.500(8) . ?
C6 C5 1.391(9) . ?
C26 C27 1.383(10) . ?
C26 C25 1.400(9) . ?
C27 C28 1.366(11) . ?
C22 C21 1.401(9) . ?
C21 C20 1.404(9) . ?
C28 C29 1.360(10) . ?
C19 C20 1.370(10) . ?
C19 C18 1.392(11) . ?
C20 C23 1.508(9) . ?
C9 C15 1.502(11) . ?
O9 N4 1.244(15) . ?
N4 O10 1.268(13) . ?
N5 O14 1.208(16) . ?
N5 O13 1.306(13) . ?
N5 O12 1.355(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 O5 144.03(17) . 1_444 ?
O1 Eu1 O3 143.15(17) . 1_454 ?
O5 Eu1 O3 72.73(16) 1_444 1_454 ?
O1 Eu1 O2 99.90(16) . 2_655 ?
O5 Eu1 O2 82.43(17) 1_444 2_655 ?
O3 Eu1 O2 78.62(18) 1_454 2_655 ?
O1 Eu1 O4 79.63(16) . 2_656 ?
O5 Eu1 O4 78.81(18) 1_444 2_656 ?
O3 Eu1 O4 122.12(16) 1_454 2_656 ?
O2 Eu1 O4 145.29(19) 2_655 2_656 ?
O1 Eu1 O6 80.01(16) . 2_666 ?
O5 Eu1 O6 120.01(16) 1_444 2_666 ?
O3 Eu1 O6 79.27(18) 1_454 2_666 ?
O2 Eu1 O6 141.42(19) 2_655 2_666 ?
O4 Eu1 O6 73.11(18) 2_656 2_666 ?
O1 Eu1 O8 72.67(18) . . ?
O5 Eu1 O8 73.83(17) 1_444 . ?
O3 Eu1 O8 138.39(19) 1_454 . ?
O2 Eu1 O8 73.1(2) 2_655 . ?
O4 Eu1 O8 73.8(2) 2_656 . ?
O6 Eu1 O8 140.1(2) 2_666 . ?
O1 Eu1 O7 72.12(18) . . ?
O5 Eu1 O7 140.28(18) 1_444 . ?
O3 Eu1 O7 72.41(17) 1_454 . ?
O2 Eu1 O7 72.6(2) 2_655 . ?
O4 Eu1 O7 137.13(19) 2_656 . ?
O6 Eu1 O7 70.77(19) 2_666 . ?
O8 Eu1 O7 124.6(2) . . ?
O1 Eu1 C30 97.89(17) . 2_666 ?
O5 Eu1 C30 98.46(17) 1_444 2_666 ?
O3 Eu1 C30 71.00(18) 1_454 2_666 ?
O2 Eu1 C30 147.68(19) 2_655 2_666 ?
O4 Eu1 C30 64.72(18) 2_656 2_666 ?
O6 Eu1 C30 21.56(17) 2_666 2_666 ?
O8 Eu1 C30 138.5(2) . 2_666 ?
O7 Eu1 C30 87.68(19) . 2_666 ?
O1 Eu1 Eu1 140.33(11) . 2 ?
O5 Eu1 Eu1 44.33(12) 1_444 2 ?
O3 Eu1 Eu1 60.72(11) 1_454 2 ?
O2 Eu1 Eu1 118.62(11) 2_655 2 ?
O4 Eu1 Eu1 63.59(11) 2_656 2 ?
O6 Eu1 Eu1 75.69(11) 2_666 2 ?
O8 Eu1 Eu1 108.18(14) . 2 ?
O7 Eu1 Eu1 126.16(13) . 2 ?
C30 Eu1 Eu1 54.16(12) 2_666 2 ?
C1 O1 Eu1 177.8(5) . . ?
C18 N2 C22 123.2(6) . . ?
C18 N2 C17 118.0(6) . . ?
C22 N2 C17 118.5(6) . . ?
C25 N3 C29 119.9(6) . . ?
C25 N3 C24 119.6(6) . . ?
C29 N3 C24 120.4(6) . . ?
C1 O2 Eu1 131.8(4) . 2_655 ?
C30 O6 Eu1 112.7(4) . 2_666 ?
C30 O5 Eu1 176.2(5) . 1_666 ?
C23 O4 Eu1 136.8(4) . 2_656 ?
C23 O3 Eu1 136.1(4) . 1_656 ?
C11 C10 C9 122.3(6) . . ?
C11 C10 C17 119.3(6) . . ?
C9 C10 C17 118.4(6) . . ?
O6 C30 O5 126.2(6) . . ?
O6 C30 C27 116.8(6) . . ?
O5 C30 C27 117.0(6) . . ?
O6 C30 Eu1 45.7(3) . 2_666 ?
O5 C30 Eu1 80.7(4) . 2_666 ?
C27 C30 Eu1 161.3(5) . 2_666 ?
C6 C2 C3 118.8(6) . . ?
C6 C2 C1 120.4(6) . . ?
C3 C2 C1 120.8(6) . . ?
C5 N1 C4 121.8(6) . . ?
C5 N1 C7 121.4(6) . . ?
C4 N1 C7 116.0(6) . . ?
C13 C12 C11 119.8(6) . . ?
C13 C12 C24 122.2(6) . . ?
C11 C12 C24 118.0(6) . . ?
C13 C8 C9 120.5(6) . . ?
C13 C8 C7 120.4(7) . . ?
C9 C8 C7 119.0(7) . . ?
C4 C3 C2 119.1(6) . . ?
C12 C13 C8 120.1(6) . . ?
C12 C13 C14 121.1(7) . . ?
C8 C13 C14 118.8(7) . . ?
C10 C11 C12 119.1(6) . . ?
C10 C11 C16 122.0(6) . . ?
C12 C11 C16 118.8(6) . . ?
C2 C6 C5 119.2(6) . . ?
O2 C1 O1 126.3(6) . . ?
O2 C1 C2 116.1(5) . . ?
O1 C1 C2 117.5(6) . . ?
N1 C5 C6 120.4(6) . . ?
C27 C26 C25 117.2(7) . . ?
C28 C27 C26 120.7(6) . . ?
C28 C27 C30 120.4(6) . . ?
C26 C27 C30 118.7(6) . . ?
N2 C22 C21 120.4(6) . . ?
N1 C4 C3 120.3(6) . . ?
C22 C21 C20 117.8(6) . . ?
C29 C28 C27 119.2(7) . . ?
C20 C19 C18 120.5(7) . . ?
C19 C20 C21 118.9(6) . . ?
C19 C20 C23 121.2(6) . . ?
C21 C20 C23 120.0(6) . . ?
C10 C9 C8 118.0(6) . . ?
C10 C9 C15 121.1(8) . . ?
C8 C9 C15 120.9(7) . . ?
C10 C17 N2 113.4(5) . . ?
O11 N4 O9 124.5(10) . . ?
O11 N4 O10 116.1(10) . . ?
O9 N4 O10 119.4(11) . . ?
N3 C25 C26 121.5(6) . . ?
N3 C24 C12 113.5(5) . . ?
N3 C29 C28 121.4(7) . . ?
N2 C18 C19 119.2(7) . . ?
O4 C23 O3 126.7(6) . . ?
O4 C23 C20 117.3(6) . . ?
O3 C23 C20 115.9(6) . . ?
C8 C7 N1 112.0(5) . . ?
O14 N5 O13 110.3(11) . . ?
O14 N5 O12 133.9(11) . . ?
O13 N5 O12 114.9(9) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        73.91
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         3.875
_refine_diff_density_min         -4.665
_refine_diff_density_rms         0.248
####################################################################### 
# 
# 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_tb_final
_database_code_depnum_ccdc_archive 'CCDC 1053004'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H27 Cl N5 O14 Tb'
_chemical_formula_weight         875.94

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   9.53070(10)
_cell_length_b                   12.7016(3)
_cell_length_c                   18.8199(3)
_cell_angle_alpha                106.349(2)
_cell_angle_beta                 98.6290(10)
_cell_angle_gamma                100.060(2)
_cell_volume                     2104.13(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7009
_cell_measurement_theta_min      4.8050
_cell_measurement_theta_max      73.4400

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.0825
_exptl_crystal_size_mid          0.0545
_exptl_crystal_size_min          0.0350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    1.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.862
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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_reflns_number            20569
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         28.27
_reflns_number_total             8879
_reflns_number_gt                7977
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1185P)²+10.0078P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8882
_refine_ls_number_parameters     439
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0622
_refine_ls_wR_factor_ref         0.1828
_refine_ls_wR_factor_gt          0.1771
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.006 0.500 0.000 589.8 28.8
_platon_squeeze_details          
;
;
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 -0.23336(3) 0.98367(2) -0.003313(13) 0.01807(12) Uani 1 1 d . . .
N2 N 0.0003(5) 0.1482(4) -0.3202(3) 0.0169(9) Uani 1 1 d . . .
O6 O -0.3136(4) 0.0240(4) -0.8828(2) 0.0244(10) Uani 1 1 d . . .
O4 O -0.1391(4) 0.0653(4) -0.0960(2) 0.0234(9) Uani 1 1 d . . .
O2 O 0.0087(4) 0.8907(4) -0.0738(2) 0.0207(8) Uani 1 1 d . . .
N1 N -0.0418(6) 0.6074(4) -0.3252(3) 0.0193(10) Uani 1 1 d . . .
O1 O -0.2302(5) 0.8227(4) -0.1122(2) 0.0248(9) Uani 1 1 d . . .
O3 O 0.1053(4) 0.1200(4) -0.0634(2) 0.0222(9) Uani 1 1 d . . .
N3 N -0.4334(6) 0.1668(5) -0.6321(3) 0.0281(7) Uani 1 1 d . . .
C10 C -0.0800(6) 0.2310(5) -0.4223(3) 0.0159(11) Uani 1 1 d . . .
C30 C -0.4333(6) 0.0418(5) -0.8672(3) 0.0145(10) Uani 1 1 d . . .
C27 C -0.4354(6) 0.0820(5) -0.7840(3) 0.0158(10) Uani 1 1 d . . .
C8 C -0.0945(6) 0.4184(5) -0.4257(3) 0.0164(11) Uani 1 1 d . . .
C28 C -0.5621(6) 0.1022(5) -0.7596(3) 0.0197(12) Uani 1 1 d . . .
H28 H -0.6505 0.0870 -0.7956 0.024 Uiso 1 1 calc R . .
O9 O 0.4007(6) -0.3680(5) -0.2890(3) 0.0406(13) Uani 1 1 d . . .
O8 O -0.4162(5) 0.8095(4) -0.0063(3) 0.0364(12) Uani 1 1 d . . .
C25 C -0.3108(6) 0.1461(6) -0.6540(3) 0.0212(12) Uani 1 1 d . . .
H25 H -0.2241 0.1615 -0.6169 0.025 Uiso 1 1 calc R . .
C13 C -0.2282(7) 0.3750(6) -0.4767(3) 0.0222(12) Uani 1 1 d . . .
C9 C -0.0207(6) 0.3471(5) -0.3974(3) 0.0146(10) Uani 1 1 d . . .
C12 C -0.2909(6) 0.2586(6) -0.4979(3) 0.0233(13) Uani 1 1 d . . .
C11 C -0.2182(6) 0.1861(5) -0.4717(3) 0.0209(12) Uani 1 1 d . . .
C1 C -0.1021(6) 0.8232(5) -0.1202(3) 0.0193(11) Uani 1 1 d . . .
C20 C -0.0115(6) 0.1189(5) -0.1831(3) 0.0203(12) Uani 1 1 d . . .
O7 O -0.2801(6) 1.1747(4) 0.0252(3) 0.0389(13) Uani 1 1 d . . .
C26 C -0.3089(6) 0.1029(5) -0.7294(3) 0.0184(11) Uani 1 1 d . . .
H26 H -0.2218 0.0874 -0.7443 0.022 Uiso 1 1 calc R . .
C3 C 0.0593(7) 0.7374(5) -0.2028(4) 0.0257(13) Uani 1 1 d . . .
H3 H 0.1424 0.7807 -0.1645 0.031 Uiso 1 1 calc R . .
C23 C -0.0167(6) 0.1004(5) -0.1070(3) 0.0209(12) Uani 1 1 d . . .
C6 C -0.1981(7) 0.6758(5) -0.2467(3) 0.0237(13) Uani 1 1 d . . .
H6 H -0.2940 0.6765 -0.2386 0.028 Uiso 1 1 calc R . .
C15 C 0.1230(7) 0.3963(5) -0.3405(4) 0.0254(13) Uani 1 1 d . . .
H15A H 0.1603 0.3354 -0.3275 0.038 Uiso 1 1 calc R . .
H15B H 0.1081 0.4493 -0.2947 0.038 Uiso 1 1 calc R . .
H15C H 0.1935 0.4359 -0.3626 0.038 Uiso 1 1 calc R . .
C17 C 0.0066(7) 0.1540(5) -0.3996(3) 0.0213(12) Uani 1 1 d . . .
H17A H 0.1095 0.1801 -0.4019 0.026 Uiso 1 1 calc R . .
H17B H -0.0304 0.0774 -0.4365 0.026 Uiso 1 1 calc R . .
C18 C -0.1262(6) 0.1439(5) -0.2968(4) 0.0221(12) Uani 1 1 d . . .
H18 H -0.2101 0.1510 -0.3279 0.027 Uiso 1 1 calc R . .
C2 C -0.0795(6) 0.7424(5) -0.1912(3) 0.0197(11) Uani 1 1 d . . .
C29 C -0.5590(6) 0.1441(6) -0.6836(3) 0.0244(13) Uani 1 1 d . . .
H29 H -0.6456 0.1573 -0.6671 0.029 Uiso 1 1 calc R . .
C21 C 0.1178(7) 0.1251(6) -0.2087(4) 0.0279(14) Uani 1 1 d . . .
H21 H 0.2037 0.1203 -0.1780 0.033 Uiso 1 1 calc R . .
C19 C -0.1339(6) 0.1295(5) -0.2282(3) 0.0206(12) Uani 1 1 d . . .
H19 H -0.2232 0.1267 -0.2114 0.025 Uiso 1 1 calc R . .
C4 C 0.0756(7) 0.6688(5) -0.2707(4) 0.0252(13) Uani 1 1 d . . .
H4 H 0.1706 0.6648 -0.2792 0.030 Uiso 1 1 calc R . .
C5 C -0.1778(7) 0.6082(5) -0.3139(3) 0.0236(12) Uani 1 1 d . . .
H5 H -0.2596 0.5622 -0.3522 0.028 Uiso 1 1 calc R . .
C7 C -0.0210(7) 0.5430(5) -0.4013(3) 0.0227(12) Uani 1 1 d . . .
H7A H 0.0846 0.5510 -0.3999 0.027 Uiso 1 1 calc R . .
H7B H -0.0610 0.5761 -0.4394 0.027 Uiso 1 1 calc R . .
C24 C -0.4407(7) 0.2107(7) -0.5497(3) 0.0338(17) Uani 1 1 d . . .
H24A H -0.4933 0.1486 -0.5348 0.041 Uiso 1 1 calc R . .
H24B H -0.4968 0.2702 -0.5430 0.041 Uiso 1 1 calc R . .
C14 C -0.3119(8) 0.4481(7) -0.5099(4) 0.0371(18) Uani 1 1 d . . .
H14A H -0.3882 0.4653 -0.4818 0.056 Uiso 1 1 calc R . .
H14B H -0.3566 0.4075 -0.5633 0.056 Uiso 1 1 calc R . .
H14C H -0.2449 0.5184 -0.5058 0.056 Uiso 1 1 calc R . .
C22 C 0.1218(7) 0.1382(6) -0.2784(4) 0.0258(13) Uani 1 1 d . . .
H22 H 0.2094 0.1403 -0.2968 0.031 Uiso 1 1 calc R . .
C16 C -0.2824(9) 0.0608(7) -0.4969(4) 0.043(2) Uani 1 1 d . . .
H16A H -0.2821 0.0352 -0.4524 0.064 Uiso 1 1 calc R . .
H16B H -0.2240 0.0212 -0.5293 0.064 Uiso 1 1 calc R . .
H16C H -0.3828 0.0447 -0.5254 0.064 Uiso 1 1 calc R . .
Cl1 Cl -0.5021(3) 0.1333(3) -0.3196(2) 0.0805(9) Uani 1 1 d . . .
N5 N -0.0983(6) -0.1627(5) -0.3999(3) 0.0281(7) Uani 1 1 d . . .
O10 O 0.3830(7) -0.3133(8) -0.1716(4) 0.068(2) Uani 1 1 d . . .
N4 N 0.4238(6) -0.3728(5) -0.2246(3) 0.0281(7) Uani 1 1 d . . .
O11 O 0.4900(7) -0.4466(6) -0.2142(4) 0.0537(9) Uani 1 1 d . . .
O5 O -0.5460(7) 0.0302(6) -0.9131(4) 0.0537(9) Uani 1 1 d . . .
O12 O -0.0090(7) -0.1093(6) -0.4261(4) 0.0537(9) Uani 1 1 d . . .
O14 O -0.2127(11) -0.2507(11) -0.4269(5) 0.098(3) Uani 1 1 d . . .
O13 O -0.0349(15) -0.1551(15) -0.3473(12) 0.237(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 O5 2.377(7) 2_464 ?
Tb1 O2 2.409(4) 2_575 ?
Tb1 O3 2.414(4) 2_565 ?
Tb1 O6 2.448(4) 1_566 ?
Tb1 O1 2.462(4) . ?
Tb1 O7 2.467(5) . ?
Tb1 O4 2.468(4) 1_565 ?
Tb1 O8 2.547(5) . ?
N2 C18 1.342(7) . ?
N2 C22 1.346(8) . ?
N2 C17 1.526(7) . ?
O6 C30 1.262(7) . ?
O6 Tb1 2.448(4) 1_544 ?
O4 C23 1.242(7) . ?
O4 Tb1 2.468(4) 1_545 ?
O2 C1 1.265(7) . ?
O2 Tb1 2.409(4) 2_575 ?
N1 C5 1.346(8) . ?
N1 C4 1.347(8) . ?
N1 C7 1.497(7) . ?
O1 C1 1.252(7) . ?
O3 C23 1.259(7) . ?
O3 Tb1 2.415(4) 2_565 ?
N3 C25 1.339(8) . ?
N3 C29 1.353(8) . ?
N3 C24 1.511(8) . ?
C10 C9 1.397(8) . ?
C10 C11 1.413(8) . ?
C10 C17 1.493(8) . ?
C30 O5 1.232(8) . ?
C30 C27 1.507(7) . ?
C27 C26 1.393(7) . ?
C27 C28 1.395(7) . ?
C8 C13 1.392(8) . ?
C8 C9 1.407(8) . ?
C8 C7 1.520(8) . ?
C28 C29 1.372(8) . ?
O9 N4 1.219(8) . ?
C25 C26 1.375(8) . ?
C13 C12 1.411(10) . ?
C13 C14 1.523(9) . ?
C9 C15 1.515(7) . ?
C12 C11 1.395(9) . ?
C12 C24 1.518(8) . ?
C11 C16 1.510(9) . ?
C1 C2 1.508(8) . ?
C20 C21 1.387(8) . ?
C20 C19 1.387(8) . ?
C20 C23 1.521(8) . ?
C3 C4 1.376(9) . ?
C3 C2 1.382(8) . ?
C6 C5 1.376(8) . ?
C6 C2 1.378(8) . ?
C18 C19 1.365(8) . ?
C21 C22 1.373(9) . ?
N5 O13 1.050(15) . ?
N5 O12 1.241(9) . ?
N5 O14 1.335(13) . ?
O10 N4 1.229(8) . ?
N4 O11 1.259(9) . ?
O5 Tb1 2.377(7) 2_464 ?
O12 O13 1.774(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Tb1 O2 144.7(2) 2_464 2_575 ?
O5 Tb1 O3 143.1(2) 2_464 2_565 ?
O2 Tb1 O3 72.07(15) 2_575 2_565 ?
O5 Tb1 O6 99.99(18) 2_464 1_566 ?
O2 Tb1 O6 83.16(14) 2_575 1_566 ?
O3 Tb1 O6 76.86(15) 2_565 1_566 ?
O5 Tb1 O1 78.91(19) 2_464 . ?
O2 Tb1 O1 120.48(14) 2_575 . ?
O3 Tb1 O1 81.01(15) 2_565 . ?
O6 Tb1 O1 140.31(16) 1_566 . ?
O5 Tb1 O7 73.1(2) 2_464 . ?
O2 Tb1 O7 74.34(15) 2_575 . ?
O3 Tb1 O7 136.98(16) 2_565 . ?
O6 Tb1 O7 73.15(18) 1_566 . ?
O1 Tb1 O7 140.31(17) . . ?
O5 Tb1 O4 79.05(19) 2_464 1_565 ?
O2 Tb1 O4 79.03(15) 2_575 1_565 ?
O3 Tb1 O4 124.06(14) 2_565 1_565 ?
O6 Tb1 O4 145.37(16) 1_566 1_565 ?
O1 Tb1 O4 73.98(16) . 1_565 ?
O7 Tb1 O4 73.54(18) . 1_565 ?
O5 Tb1 O8 72.0(2) 2_464 . ?
O2 Tb1 O8 140.02(16) 2_575 . ?
O3 Tb1 O8 72.15(15) 2_565 . ?
O6 Tb1 O8 71.88(18) 1_566 . ?
O1 Tb1 O8 70.14(17) . . ?
O7 Tb1 O8 124.34(18) . . ?
O4 Tb1 O8 137.26(17) 1_565 . ?
C18 N2 C22 122.3(5) . . ?
C18 N2 C17 120.0(5) . . ?
C22 N2 C17 117.5(5) . . ?
C30 O6 Tb1 130.9(3) . 1_544 ?
C23 O4 Tb1 135.9(4) . 1_545 ?
C1 O2 Tb1 173.8(4) . 2_575 ?
C5 N1 C4 121.0(5) . . ?
C5 N1 C7 119.4(5) . . ?
C4 N1 C7 119.5(5) . . ?
C1 O1 Tb1 110.1(3) . . ?
C23 O3 Tb1 135.9(4) . 2_565 ?
C25 N3 C29 120.9(6) . . ?
C25 N3 C24 122.2(5) . . ?
C29 N3 C24 116.8(5) . . ?
C9 C10 C11 120.2(5) . . ?
C9 C10 C17 119.7(5) . . ?
C11 C10 C17 120.0(5) . . ?
O5 C30 O6 126.1(5) . . ?
O5 C30 C27 118.1(5) . . ?
O6 C30 C27 115.8(4) . . ?
C26 C27 C28 118.2(5) . . ?
C26 C27 C30 120.6(5) . . ?
C28 C27 C30 121.2(5) . . ?
C13 C8 C9 120.7(5) . . ?
C13 C8 C7 121.2(5) . . ?
C9 C8 C7 118.0(5) . . ?
C29 C28 C27 119.9(5) . . ?
N3 C25 C26 120.8(5) . . ?
C8 C13 C12 118.8(6) . . ?
C8 C13 C14 123.0(6) . . ?
C12 C13 C14 118.2(6) . . ?
C10 C9 C8 119.8(5) . . ?
C10 C9 C15 120.3(5) . . ?
C8 C9 C15 120.0(5) . . ?
C11 C12 C13 121.3(5) . . ?
C11 C12 C24 119.0(6) . . ?
C13 C12 C24 119.7(6) . . ?
C12 C11 C10 119.0(5) . . ?
C12 C11 C16 121.3(6) . . ?
C10 C11 C16 119.7(6) . . ?
O1 C1 O2 123.7(5) . . ?
O1 C1 C2 118.0(5) . . ?
O2 C1 C2 118.3(5) . . ?
C21 C20 C19 118.5(5) . . ?
C21 C20 C23 119.9(5) . . ?
C19 C20 C23 121.5(5) . . ?
C25 C26 C27 119.7(5) . . ?
C4 C3 C2 119.1(6) . . ?
O4 C23 O3 127.9(5) . . ?
O4 C23 C20 116.8(5) . . ?
O3 C23 C20 115.3(5) . . ?
C5 C6 C2 120.1(6) . . ?
C10 C17 N2 113.3(5) . . ?
N2 C18 C19 119.7(5) . . ?
C6 C2 C3 119.2(5) . . ?
C6 C2 C1 119.9(5) . . ?
C3 C2 C1 120.8(5) . . ?
N3 C29 C28 120.4(5) . . ?
C22 C21 C20 120.1(6) . . ?
C18 C19 C20 120.1(5) . . ?
N1 C4 C3 120.6(5) . . ?
N1 C5 C6 119.8(6) . . ?
N1 C7 C8 113.0(5) . . ?
N3 C24 C12 112.6(5) . . ?
N2 C22 C21 119.3(5) . . ?
O13 N5 O12 101.2(10) . . ?
O13 N5 O14 115.3(9) . . ?
O12 N5 O14 137.1(7) . . ?
O9 N4 O10 124.1(7) . . ?
O9 N4 O11 116.1(6) . . ?
O10 N4 O11 119.8(7) . . ?
C30 O5 Tb1 176.7(5) . 2_464 ?
N5 O12 O13 35.5(4) . . ?
N5 O13 O12 43.3(8) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        28.27
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         6.070
_refine_diff_density_min         -4.504
_refine_diff_density_rms         0.220
####################################################################### 
# 
# 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_dy_final
_database_code_depnum_ccdc_archive 'CCDC 1053005'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H27 Cl Dy N5 O14'
_chemical_formula_weight         879.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   9.4727(2)
_cell_length_b                   12.6520(4)
_cell_length_c                   18.6017(6)
_cell_angle_alpha                106.106(3)
_cell_angle_beta                 98.088(2)
_cell_angle_gamma                100.255(2)
_cell_volume                     2064.63(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10279
_cell_measurement_theta_min      4.8270
_cell_measurement_theta_max      73.5230

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.0903
_exptl_crystal_size_mid          0.0611
_exptl_crystal_size_min          0.0407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             874
_exptl_absorpt_coefficient_mu    10.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_T_max  0.644
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15375
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.73
_diffrn_reflns_theta_max         73.81
_reflns_number_total             8016
_reflns_number_gt                7584
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1499P)²+4.0441P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8016
_refine_ls_number_parameters     445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0714
_refine_ls_wR_factor_ref         0.1965
_refine_ls_wR_factor_gt          0.1930
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.010 0.000 0.500 562.4 155.0
_platon_squeeze_details          
;
;
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.76384(3) -0.51563(2) 0.497148(14) 0.01110(15) Uani 1 1 d . . .
O6 O 1.5516(4) 0.4682(4) 1.4147(2) 0.0190(8) Uani 1 1 d . . .
N2 N 0.9956(6) 0.3485(4) 0.8172(3) 0.0172(10) Uani 1 1 d . . .
O1 O 0.9757(4) -0.3919(3) 0.5743(2) 0.0209(9) Uani 1 1 d . . .
O4 O 0.8895(4) 0.3830(4) 0.5597(2) 0.0215(9) Uani 1 1 d . . .
O5 O 1.3196(5) 0.4791(4) 1.3867(2) 0.0245(10) Uani 1 1 d . . .
O2 O 1.2185(5) -0.3323(4) 0.6077(2) 0.0230(9) Uani 1 1 d . . .
N3 N 1.4388(6) 0.3372(5) 1.1332(3) 0.0227(11) Uani 1 1 d . . .
C8 C 1.0987(7) 0.0819(5) 0.9264(3) 0.0192(11) Uani 1 1 d . . .
C27 C 1.4398(6) 0.4201(5) 1.2851(3) 0.0150(10) Uani 1 1 d . . .
O8 O 0.5887(5) -0.6891(4) 0.4909(3) 0.0318(11) Uani 1 1 d . . .
N1 N 1.0439(6) -0.1079(4) 0.8262(3) 0.0210(10) Uani 1 1 d . . .
C10 C 1.0804(6) 0.2684(5) 0.9213(3) 0.0161(11) Uani 1 1 d . . .
C1 C 1.0905(7) -0.3293(5) 0.6175(4) 0.0214(12) Uani 1 1 d . . .
C30 C 1.4391(6) 0.4609(5) 1.3706(3) 0.0160(11) Uani 1 1 d . . .
C28 C 1.5658(6) 0.3981(6) 1.2604(3) 0.0219(12) Uani 1 1 d . . .
H28 H 1.6538 0.4107 1.2963 0.026 Uiso 1 1 calc R . .
C2 C 1.0752(7) -0.2439(5) 0.6895(4) 0.0224(12) Uani 1 1 d . . .
C11 C 1.2187(7) 0.3156(6) 0.9707(3) 0.0244(13) Uani 1 1 d . . .
C13 C 1.2329(8) 0.1279(6) 0.9771(3) 0.0263(14) Uani 1 1 d . . .
C26 C 1.3142(6) 0.4021(5) 1.2312(3) 0.0197(11) Uani 1 1 d . . .
H26 H 1.2277 0.4194 1.2472 0.024 Uiso 1 1 calc R . .
C12 C 1.2953(11) 0.2455(9) 0.9975(5) 0.0491(9) Uani 1 1 d . . .
C29 C 1.5625(7) 0.3579(6) 1.1835(4) 0.0258(13) Uani 1 1 d . . .
H29 H 1.6493 0.3448 1.1661 0.031 Uiso 1 1 calc R . .
C15 C 0.8781(7) 0.1021(5) 0.8424(4) 0.0262(14) Uani 1 1 d . . .
H15A H 0.8330 0.1631 0.8346 0.039 Uiso 1 1 calc R . .
H15B H 0.8128 0.0537 0.8627 0.039 Uiso 1 1 calc R . .
H15C H 0.8948 0.0571 0.7935 0.039 Uiso 1 1 calc R . .
C25 C 1.3142(6) 0.3591(6) 1.1540(3) 0.0216(12) Uani 1 1 d . . .
H25 H 1.2280 0.3454 1.1167 0.026 Uiso 1 1 calc R . .
C6 C 1.1971(7) -0.1783(5) 0.7445(4) 0.0242(13) Uani 1 1 d . . .
H6 H 1.2927 -0.1806 0.7352 0.029 Uiso 1 1 calc R . .
C21 C 0.8754(7) 0.3704(7) 0.7046(4) 0.0312(15) Uani 1 1 d . . .
H21 H 0.7886 0.3743 0.6739 0.037 Uiso 1 1 calc R . .
C3 C 0.9370(7) -0.2371(5) 0.7043(4) 0.0246(13) Uani 1 1 d . . .
H3 H 0.8518 -0.2798 0.6671 0.030 Uiso 1 1 calc R . .
C19 C 1.1304(7) 0.3677(6) 0.7233(4) 0.0230(12) Uani 1 1 d . . .
H19 H 1.2201 0.3710 0.7057 0.028 Uiso 1 1 calc R . .
C4 C 0.9251(7) -0.1682(5) 0.7727(4) 0.0250(13) Uani 1 1 d . . .
H4 H 0.8307 -0.1629 0.7829 0.030 Uiso 1 1 calc R . .
C23 C 1.0116(7) 0.3992(5) 0.6024(3) 0.0206(12) Uani 1 1 d . . .
C9 C 1.0216(6) 0.1518(5) 0.8980(3) 0.0155(10) Uani 1 1 d . . .
C18 C 1.1222(7) 0.3531(5) 0.7930(4) 0.0219(12) Uani 1 1 d . . .
H18 H 1.2065 0.3462 0.8241 0.026 Uiso 1 1 calc R . .
C17 C 0.9916(7) 0.3450(5) 0.8984(3) 0.0216(12) Uani 1 1 d . . .
H17A H 1.0292 0.4224 0.9345 0.026 Uiso 1 1 calc R . .
H17B H 0.8887 0.3191 0.9021 0.026 Uiso 1 1 calc R . .
C16 C 1.2795(10) 0.4416(7) 0.9950(5) 0.046(2) Uani 1 1 d . . .
H16A H 1.2229 0.4799 1.0300 0.069 Uiso 1 1 calc R . .
H16B H 1.2729 0.4675 0.9499 0.069 Uiso 1 1 calc R . .
H16C H 1.3822 0.4592 1.0210 0.069 Uiso 1 1 calc R . .
C5 C 1.1790(7) -0.1105(5) 0.8121(4) 0.0255(13) Uani 1 1 d . . .
H5 H 1.2624 -0.0647 0.8495 0.031 Uiso 1 1 calc R . .
C22 C 0.8733(7) 0.3573(6) 0.7757(4) 0.0275(14) Uani 1 1 d . . .
H22 H 0.7856 0.3546 0.7951 0.033 Uiso 1 1 calc R . .
C20 C 1.0058(6) 0.3778(5) 0.6785(3) 0.0197(12) Uani 1 1 d . . .
C7 C 1.0270(8) -0.0422(5) 0.9038(4) 0.0258(13) Uani 1 1 d . . .
H7A H 1.0703 -0.0746 0.9420 0.031 Uiso 1 1 calc R . .
H7B H 0.9214 -0.0507 0.9046 0.031 Uiso 1 1 calc R . .
C24 C 1.4467(10) 0.2969(9) 1.0492(5) 0.0491(9) Uani 1 1 d . . .
H24A H 1.5068 0.2397 1.0413 0.059 Uiso 1 1 calc R . .
H24B H 1.4957 0.3615 1.0346 0.059 Uiso 1 1 calc R . .
C14 C 1.3194(10) 0.0547(8) 1.0102(4) 0.0415(19) Uani 1 1 d . . .
H14A H 1.2557 -0.0198 1.0012 0.062 Uiso 1 1 calc R . .
H14B H 1.3548 0.0913 1.0653 0.062 Uiso 1 1 calc R . .
H14C H 1.4030 0.0458 0.9853 0.062 Uiso 1 1 calc R . .
O3 O 1.1361(5) 0.4353(4) 0.5912(3) 0.0235(9) Uani 1 1 d . . .
O7 O 0.7148(6) -0.3297(4) 0.5236(3) 0.0376(13) Uani 1 1 d . . .
O9 O 0.4055(6) 0.1316(5) 0.2122(3) 0.0399(13) Uani 1 1 d . . .
N5 N 0.1003(9) 0.6648(8) 0.9010(4) 0.0491(9) Uani 1 1 d . . .
N4 N 0.4260(9) 0.1291(7) 0.2788(5) 0.053(2) Uani 1 1 d . . .
O11 O 0.3883(10) 0.1911(10) 0.3313(4) 0.086(3) Uani 1 1 d . . .
O10 O 0.4903(11) 0.0516(9) 0.2887(7) 0.094(3) Uani 1 1 d . . .
O13 O 0.0162(7) 0.6121(6) 0.9278(3) 0.0491(9) Uani 1 1 d . . .
O12 O 0.0428(17) 0.6513(17) 0.8430(13) 0.270(16) Uani 1 1 d . . .
Cl1 Cl 0.5006(3) 0.6444(4) 0.1774(2) 0.0967(13) Uani 1 1 d . . .
O14 O 0.2145(9) 0.7570(9) 0.9310(5) 0.076(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O6 2.290(4) 1_444 ?
Dy1 O1 2.316(4) . ?
Dy1 O4 2.324(4) 1_545 ?
Dy1 O5 2.358(4) 2_757 ?
Dy1 O3 2.378(4) 2_756 ?
Dy1 O2 2.379(4) 2_746 ?
Dy1 O7 2.408(5) . ?
Dy1 O8 2.468(5) . ?
O6 C30 1.223(7) . ?
O6 Dy1 2.290(4) 1_666 ?
N2 C18 1.336(8) . ?
N2 C22 1.339(8) . ?
N2 C17 1.528(7) . ?
O1 C1 1.245(7) . ?
O4 C23 1.255(7) . ?
O4 Dy1 2.324(4) 1_565 ?
O5 C30 1.254(7) . ?
O5 Dy1 2.358(4) 2_757 ?
O2 C1 1.257(8) . ?
O2 Dy1 2.379(4) 2_746 ?
N3 C29 1.327(8) . ?
N3 C25 1.344(8) . ?
N3 C24 1.521(9) . ?
C8 C13 1.392(9) . ?
C8 C9 1.406(8) . ?
C8 C7 1.509(8) . ?
C27 C26 1.383(8) . ?
C27 C28 1.384(8) . ?
C27 C30 1.531(7) . ?
N1 C4 1.340(9) . ?
N1 C5 1.347(9) . ?
N1 C7 1.498(8) . ?
C10 C9 1.400(8) . ?
C10 C11 1.412(8) . ?
C10 C17 1.499(8) . ?
C1 C2 1.513(9) . ?
C28 C29 1.373(9) . ?
C2 C6 1.387(9) . ?
C2 C3 1.388(9) . ?
C11 C12 1.390(12) . ?
C11 C16 1.509(10) . ?
C13 C12 1.421(13) . ?
C13 C14 1.534(9) . ?
C26 C25 1.388(8) . ?
C12 C24 1.529(14) . ?
C15 C9 1.500(8) . ?
C6 C5 1.364(9) . ?
C21 C22 1.381(9) . ?
C21 C20 1.386(9) . ?
C3 C4 1.361(9) . ?
C19 C18 1.370(9) . ?
C19 C20 1.392(8) . ?
C23 O3 1.254(7) . ?
C23 C20 1.521(8) . ?
O3 Dy1 2.378(4) 2_756 ?
O9 N4 1.237(11) . ?
N5 O12 1.091(17) . ?
N5 O13 1.198(10) . ?
N5 O14 1.364(13) . ?
N4 O11 1.213(12) . ?
N4 O10 1.284(12) . ?
O13 O12 1.82(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
O6 Dy1 O1 144.83(16) 1_444 . ?
O6 Dy1 O4 142.53(16) 1_444 1_545 ?
O1 Dy1 O4 72.55(15) . 1_545 ?
O6 Dy1 O5 99.83(14) 1_444 2_757 ?
O1 Dy1 O5 82.41(16) . 2_757 ?
O4 Dy1 O5 78.56(16) 1_545 2_757 ?
O6 Dy1 O3 80.65(15) 1_444 2_756 ?
O1 Dy1 O3 78.61(16) . 2_756 ?
O4 Dy1 O3 121.40(15) 1_545 2_756 ?
O5 Dy1 O3 145.72(18) 2_757 2_756 ?
O6 Dy1 O2 80.27(15) 1_444 2_746 ?
O1 Dy1 O2 119.41(15) . 2_746 ?
O4 Dy1 O2 78.83(16) 1_545 2_746 ?
O5 Dy1 O2 141.42(17) 2_757 2_746 ?
O3 Dy1 O2 72.76(16) 2_756 2_746 ?
O6 Dy1 O7 73.26(16) 1_444 . ?
O1 Dy1 O7 73.85(16) . . ?
O4 Dy1 O7 138.51(17) 1_545 . ?
O5 Dy1 O7 73.5(2) 2_757 . ?
O3 Dy1 O7 73.90(19) 2_756 . ?
O2 Dy1 O7 140.12(18) 2_746 . ?
O6 Dy1 O8 71.59(16) 1_444 . ?
O1 Dy1 O8 140.23(16) . . ?
O4 Dy1 O8 72.23(15) 1_545 . ?
O5 Dy1 O8 73.06(18) 2_757 . ?
O3 Dy1 O8 136.80(17) 2_756 . ?
O2 Dy1 O8 70.45(17) 2_746 . ?
O7 Dy1 O8 125.51(19) . . ?
C30 O6 Dy1 179.2(4) . 1_666 ?
C18 N2 C22 122.6(5) . . ?
C18 N2 C17 119.5(5) . . ?
C22 N2 C17 117.6(5) . . ?
C1 O1 Dy1 176.9(4) . . ?
C23 O4 Dy1 137.5(4) . 1_565 ?
C30 O5 Dy1 131.9(4) . 2_757 ?
C1 O2 Dy1 115.1(4) . 2_746 ?
C29 N3 C25 122.5(5) . . ?
C29 N3 C24 116.8(6) . . ?
C25 N3 C24 120.4(6) . . ?
C13 C8 C9 120.4(6) . . ?
C13 C8 C7 121.7(6) . . ?
C9 C8 C7 117.8(5) . . ?
C26 C27 C28 118.8(5) . . ?
C26 C27 C30 120.8(5) . . ?
C28 C27 C30 120.4(5) . . ?
C4 N1 C5 120.4(5) . . ?
C4 N1 C7 120.0(5) . . ?
C5 N1 C7 119.5(6) . . ?
C9 C10 C11 120.6(6) . . ?
C9 C10 C17 119.8(5) . . ?
C11 C10 C17 119.4(5) . . ?
O1 C1 O2 125.9(6) . . ?
O1 C1 C2 117.2(6) . . ?
O2 C1 C2 116.9(5) . . ?
O6 C30 O5 127.7(5) . . ?
O6 C30 C27 117.1(5) . . ?
O5 C30 C27 115.2(5) . . ?
C29 C28 C27 119.3(6) . . ?
C6 C2 C3 118.8(6) . . ?
C6 C2 C1 121.2(6) . . ?
C3 C2 C1 119.8(5) . . ?
C12 C11 C10 119.5(7) . . ?
C12 C11 C16 121.0(8) . . ?
C10 C11 C16 119.5(7) . . ?
C8 C13 C12 119.7(6) . . ?
C8 C13 C14 122.0(7) . . ?
C12 C13 C14 118.3(7) . . ?
C27 C26 C25 120.2(6) . . ?
C11 C12 C13 120.2(8) . . ?
C11 C12 C24 119.1(9) . . ?
C13 C12 C24 120.7(8) . . ?
N3 C29 C28 120.5(6) . . ?
N3 C25 C26 118.5(5) . . ?
C5 C6 C2 119.7(6) . . ?
C22 C21 C20 119.2(6) . . ?
C4 C3 C2 119.1(6) . . ?
C18 C19 C20 119.2(6) . . ?
N1 C4 C3 121.4(6) . . ?
O3 C23 O4 128.0(5) . . ?
O3 C23 C20 116.5(5) . . ?
O4 C23 C20 115.4(5) . . ?
C10 C9 C8 119.5(5) . . ?
C10 C9 C15 120.0(5) . . ?
C8 C9 C15 120.5(5) . . ?
N2 C18 C19 120.0(6) . . ?
C10 C17 N2 112.8(5) . . ?
N1 C5 C6 120.5(6) . . ?
N2 C22 C21 119.6(6) . . ?
C21 C20 C19 119.4(5) . . ?
C21 C20 C23 119.6(5) . . ?
C19 C20 C23 121.0(5) . . ?
N1 C7 C8 113.3(5) . . ?
N3 C24 C12 112.3(7) . . ?
C23 O3 Dy1 137.5(4) . 2_756 ?
O12 N5 O13 105.0(12) . . ?
O12 N5 O14 116.4(10) . . ?
O13 N5 O14 134.2(8) . . ?
O11 N4 O9 125.1(9) . . ?
O11 N4 O10 121.0(10) . . ?
O9 N4 O10 113.8(9) . . ?
N5 O13 O12 35.4(5) . . ?
N5 O12 O13 39.5(9) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        73.81
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         2.904
_refine_diff_density_min         -4.636
_refine_diff_density_rms         0.209
####################################################################### 
# 
# 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_ho_final
_database_code_depnum_ccdc_archive 'CCDC 1053006'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H27 Cl Ho N5 O14'
_chemical_formula_weight         881.95

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -14.9734 3.7046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   9.4644(2)
_cell_length_b                   12.7206(3)
_cell_length_c                   18.5539(5)
_cell_angle_alpha                106.206(2)
_cell_angle_beta                 97.893(2)
_cell_angle_gamma                100.266(2)
_cell_volume                     2068.88(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9757
_cell_measurement_theta_min      4.8280
_cell_measurement_theta_max      73.5330

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.029
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             876
_exptl_absorpt_coefficient_mu    4.715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13861
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.72
_diffrn_reflns_theta_max         73.74
_reflns_number_total             8012
_reflns_number_gt                7675
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.1578P)²+8.0145P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8012
_refine_ls_number_parameters     428
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0783
_refine_ls_wR_factor_ref         0.2197
_refine_ls_wR_factor_gt          0.2181
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.001

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.007 0.000 0.500 561.3 157.8
_platon_squeeze_details          
;
;

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 0.26384(3) 0.48509(3) 0.497279(17) 0.01622(18) Uani 1 1 d . . .
Cl1 Cl 0.0001(2) -0.3565(2) 0.17881(16) 0.0735(7) Uani 1 1 d . . .
O1 O 0.2840(4) 0.3333(3) 0.3943(2) 0.0253(8) Uani 1 1 d . . .
N1 N 0.4581(6) 0.1063(4) 0.1741(3) 0.0267(10) Uani 1 1 d . . .
C1 C 0.4017(6) -0.0831(4) 0.0740(3) 0.0245(11) Uani 1 1 d . . .
O2 O 0.5267(4) 0.3913(3) 0.4269(2) 0.0258(8) Uani 1 1 d . . .
N2 N 0.5041(5) -0.3506(4) 0.1808(3) 0.0234(9) Uani 1 1 d . . .
C2 C 0.4778(5) -0.1530(4) 0.1022(3) 0.0197(9) Uani 1 1 d . . .
O3 O 0.3645(4) -0.4380(3) 0.4077(2) 0.0260(8) Uani 1 1 d . . .
N3 N 0.0608(6) -0.3357(5) -0.1320(3) 0.0369(7) Uani 1 1 d . . .
C3 C 0.4186(6) -0.2694(4) 0.0781(3) 0.0211(10) Uani 1 1 d . . .
O4 O 0.6110(4) -0.3865(3) 0.4387(2) 0.0269(8) Uani 1 1 d . . .
N4 N -0.0741(6) 0.1265(5) 0.2787(3) 0.0369(7) Uani 1 1 d . . .
C4 C 0.2819(6) -0.3150(5) 0.0299(3) 0.0270(11) Uani 1 1 d . . .
O5 O 0.1796(4) -0.4762(4) -0.38683(19) 0.0287(9) Uani 1 1 d . . .
N5 N 0.4034(6) 0.3352(5) 0.0983(3) 0.0369(7) Uani 1 1 d . . .
C5 C 0.2059(6) -0.2435(5) 0.0038(3) 0.0287(12) Uani 1 1 d . . .
O6 O -0.0532(4) -0.4671(3) -0.41471(19) 0.0241(8) Uani 1 1 d . . .
C6 C 0.2660(7) -0.1279(5) 0.0235(3) 0.0311(13) Uani 1 1 d . . .
O11 O -0.0099(11) 0.0527(9) 0.2915(6) 0.101(3) Uani 1 1 d . . .
C7 C 0.4721(8) 0.0399(5) 0.0967(3) 0.0320(12) Uani 1 1 d . . .
H7A H 0.5774 0.0484 0.0948 0.038 Uiso 1 1 calc R . .
H7B H 0.4275 0.0718 0.0586 0.038 Uiso 1 1 calc R . .
O10 O -0.1082(10) 0.1901(8) 0.3325(6) 0.0963(13) Uani 1 1 d . . .
C8 C 0.5085(6) -0.3455(5) 0.1008(3) 0.0308(9) Uani 1 1 d . . .
H8A H 0.6115 -0.3188 0.0974 0.037 Uiso 1 1 calc R . .
H8B H 0.4721 -0.4222 0.0641 0.037 Uiso 1 1 calc R . .
O9 O -0.0930(10) 0.1302(8) 0.2128(6) 0.0963(13) Uani 1 1 d . . .
C9 C 0.0556(6) -0.2912(5) -0.0473(3) 0.0308(9) Uani 1 1 d . . .
H9A H -0.0008 -0.2318 -0.0400 0.037 Uiso 1 1 calc R . .
H9B H 0.0031 -0.3530 -0.0315 0.037 Uiso 1 1 calc R . .
O13 O 0.2871(9) 0.2384(8) 0.0684(5) 0.088(2) Uani 1 1 d . . .
C10 C 0.6207(7) -0.1037(5) 0.1578(3) 0.0318(12) Uani 1 1 d . . .
H10A H 0.6622 -0.1643 0.1685 0.048 Uiso 1 1 calc R . .
H10B H 0.6047 -0.0543 0.2055 0.048 Uiso 1 1 calc R . .
H10C H 0.6888 -0.0601 0.1357 0.048 Uiso 1 1 calc R . .
O14 O 0.3391(9) 0.3900(8) 0.0690(6) 0.0963(13) Uani 1 1 d . . .
C11 C 0.2168(9) -0.4393(6) 0.0045(4) 0.0486(18) Uani 1 1 d . . .
H11A H 0.2914 -0.4802 -0.0116 0.073 Uiso 1 1 calc R . .
H11B H 0.1342 -0.4583 -0.0385 0.073 Uiso 1 1 calc R . .
H11C H 0.1824 -0.4605 0.0470 0.073 Uiso 1 1 calc R . .
O12 O 0.4882(10) 0.3216(8) 0.1338(6) 0.0963(13) Uani 1 1 d . . .
C12 C 0.1821(9) -0.0546(7) -0.0085(4) 0.0480(18) Uani 1 1 d . . .
H12A H 0.1339 -0.0954 -0.0618 0.072 Uiso 1 1 calc R . .
H12B H 0.2500 0.0145 -0.0063 0.072 Uiso 1 1 calc R . .
H12C H 0.1080 -0.0356 0.0219 0.072 Uiso 1 1 calc R . .
C13 C 0.5776(7) 0.1669(5) 0.2274(4) 0.0313(12) Uani 1 1 d . . .
H13 H 0.6722 0.1625 0.2170 0.038 Uiso 1 1 calc R . .
C14 C 0.5641(6) 0.2354(5) 0.2972(4) 0.0306(12) Uani 1 1 d . . .
H14 H 0.6490 0.2760 0.3353 0.037 Uiso 1 1 calc R . .
C15 C 0.4274(6) 0.2446(4) 0.3114(3) 0.0256(11) Uani 1 1 d . . .
C16 C 0.3037(6) 0.1780(5) 0.2570(3) 0.0290(11) Uani 1 1 d . . .
H16 H 0.2083 0.1802 0.2671 0.035 Uiso 1 1 calc R . .
C17 C 0.3216(7) 0.1093(5) 0.1888(3) 0.0299(12) Uani 1 1 d . . .
H17 H 0.2380 0.0636 0.1516 0.036 Uiso 1 1 calc R . .
C18 C 0.4113(6) 0.3285(4) 0.3838(3) 0.0235(10) Uani 1 1 d . . .
C19 C 0.6258(6) -0.3601(5) 0.2226(4) 0.0309(12) Uani 1 1 d . . .
H19 H 0.7139 -0.3570 0.2033 0.037 Uiso 1 1 calc R . .
C20 C 0.6233(7) -0.3744(6) 0.2929(4) 0.0336(13) Uani 1 1 d . . .
H20 H 0.7101 -0.3795 0.3230 0.040 Uiso 1 1 calc R . .
C21 C 0.4940(6) -0.3812(4) 0.3202(3) 0.0231(10) Uani 1 1 d . . .
C22 C 0.3696(6) -0.3705(5) 0.2757(3) 0.0275(11) Uani 1 1 d . . .
H22 H 0.2799 -0.3741 0.2935 0.033 Uiso 1 1 calc R . .
C23 C 0.3773(6) -0.3547(5) 0.2068(3) 0.0273(11) Uani 1 1 d . . .
H23 H 0.2928 -0.3466 0.1766 0.033 Uiso 1 1 calc R . .
C24 C 0.4879(6) -0.4036(4) 0.3958(3) 0.0240(10) Uani 1 1 d . . .
C25 C 0.1846(5) -0.3565(5) -0.1546(3) 0.0260(11) Uani 1 1 d . . .
H25 H 0.2715 -0.3421 -0.1175 0.031 Uiso 1 1 calc R . .
C26 C 0.1859(6) -0.3983(5) -0.2310(3) 0.0232(10) Uani 1 1 d . . .
H26 H 0.2729 -0.4143 -0.2471 0.028 Uiso 1 1 calc R . .
C27 C 0.0590(5) -0.4172(4) -0.2847(3) 0.0188(9) Uani 1 1 d . . .
C28 C -0.0672(6) -0.3966(5) -0.2595(3) 0.0271(11) Uani 1 1 d . . .
H28 H -0.1560 -0.4117 -0.2954 0.032 Uiso 1 1 calc R . .
C29 C -0.0635(6) -0.3538(6) -0.1818(3) 0.0316(13) Uani 1 1 d . . .
H29 H -0.1491 -0.3375 -0.1641 0.038 Uiso 1 1 calc R . .
C30 C 0.0610(5) -0.4580(4) -0.3701(3) 0.0196(9) Uani 1 1 d . . .
O8 O 0.0910(5) 0.3143(4) 0.4931(3) 0.0373(10) Uani 1 1 d . . .
O7 O 0.2155(5) 0.6678(4) 0.5206(3) 0.0423(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 O6 2.275(3) 2 ?
Ho1 O2 2.295(4) 2_666 ?
Ho1 O4 2.316(4) 2_656 ?
Ho1 O5 2.350(3) 1_566 ?
Ho1 O1 2.364(4) . ?
Ho1 O3 2.374(4) 1_565 ?
Ho1 O7 2.381(4) . ?
Ho1 O8 2.451(4) . ?
O1 C18 1.257(7) . ?
N1 C13 1.344(8) . ?
N1 C17 1.362(8) . ?
N1 C7 1.486(7) . ?
C1 C6 1.400(8) . ?
C1 C2 1.403(7) . ?
C1 C7 1.502(8) . ?
O2 C18 1.251(6) . ?
O2 Ho1 2.295(4) 2_666 ?
N2 C19 1.341(7) . ?
N2 C23 1.351(7) . ?
N2 C8 1.510(7) . ?
C2 C3 1.404(7) . ?
C2 C10 1.496(7) . ?
O3 C24 1.244(7) . ?
O3 Ho1 2.374(4) 1_545 ?
N3 C29 1.334(8) . ?
N3 C25 1.342(7) . ?
N3 C9 1.526(7) . ?
C3 C4 1.391(7) . ?
C3 C8 1.504(8) . ?
O4 C24 1.263(7) . ?
O4 Ho1 2.316(4) 2_656 ?
N4 O10 1.218(11) . ?
N4 O9 1.227(11) . ?
N4 O11 1.263(10) . ?
C4 C5 1.401(8) . ?
C4 C11 1.502(8) . ?
O5 C30 1.248(6) . ?
O5 Ho1 2.350(3) 1_544 ?
N5 O12 1.037(10) . ?
N5 O14 1.194(10) . ?
N5 O13 1.415(11) . ?
C5 C6 1.402(9) . ?
C5 C9 1.514(8) . ?
O6 C30 1.234(6) . ?
O6 Ho1 2.275(3) 2 ?
C6 C12 1.515(8) . ?
C13 C14 1.381(8) . ?
C14 C15 1.374(8) . ?
C15 C16 1.397(8) . ?
C15 C18 1.510(7) . ?
C16 C17 1.374(8) . ?
C19 C20 1.370(8) . ?
C20 C21 1.385(8) . ?
C21 C22 1.392(7) . ?
C21 C24 1.514(7) . ?
C22 C23 1.359(8) . ?
C25 C26 1.372(7) . ?
C26 C27 1.388(7) . ?
C27 C28 1.382(7) . ?
C27 C30 1.528(6) . ?
C28 C29 1.385(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Ho1 O2 144.72(15) 2 2_666 ?
O6 Ho1 O4 142.45(15) 2 2_656 ?
O2 Ho1 O4 72.74(14) 2_666 2_656 ?
O6 Ho1 O5 99.76(13) 2 1_566 ?
O2 Ho1 O5 82.55(14) 2_666 1_566 ?
O4 Ho1 O5 78.56(14) 2_656 1_566 ?
O6 Ho1 O1 80.56(13) 2 . ?
O2 Ho1 O1 119.08(13) 2_666 . ?
O4 Ho1 O1 78.64(14) 2_656 . ?
O5 Ho1 O1 141.50(15) 1_566 . ?
O6 Ho1 O3 80.78(13) 2 1_565 ?
O2 Ho1 O3 78.44(14) 2_666 1_565 ?
O4 Ho1 O3 121.31(13) 2_656 1_565 ?
O5 Ho1 O3 145.86(16) 1_566 1_565 ?
O1 Ho1 O3 72.56(14) . 1_565 ?
O6 Ho1 O7 73.19(15) 2 . ?
O2 Ho1 O7 73.73(15) 2_666 . ?
O4 Ho1 O7 138.83(16) 2_656 . ?
O5 Ho1 O7 74.05(18) 1_566 . ?
O1 Ho1 O7 139.75(16) . . ?
O3 Ho1 O7 73.52(17) 1_565 . ?
O6 Ho1 O8 71.82(15) 2 . ?
O2 Ho1 O8 140.14(15) 2_666 . ?
O4 Ho1 O8 71.93(14) 2_656 . ?
O5 Ho1 O8 72.92(16) 1_566 . ?
O1 Ho1 O8 70.71(15) . . ?
O3 Ho1 O8 136.94(15) 1_565 . ?
O7 Ho1 O8 125.99(17) . . ?
C18 O1 Ho1 116.4(3) . . ?
C13 N1 C17 120.4(5) . . ?
C13 N1 C7 120.8(5) . . ?
C17 N1 C7 118.7(5) . . ?
C6 C1 C2 120.7(5) . . ?
C6 C1 C7 120.9(5) . . ?
C2 C1 C7 118.3(5) . . ?
C18 O2 Ho1 176.5(4) . 2_666 ?
C19 N2 C23 121.2(5) . . ?
C19 N2 C8 118.2(5) . . ?
C23 N2 C8 120.4(5) . . ?
C1 C2 C3 119.5(5) . . ?
C1 C2 C10 120.2(5) . . ?
C3 C2 C10 120.4(5) . . ?
C24 O3 Ho1 137.9(3) . 1_545 ?
C29 N3 C25 122.2(5) . . ?
C29 N3 C9 116.7(5) . . ?
C25 N3 C9 121.1(5) . . ?
C4 C3 C2 120.6(5) . . ?
C4 C3 C8 119.9(5) . . ?
C2 C3 C8 119.3(5) . . ?
C24 O4 Ho1 137.4(4) . 2_656 ?
O10 N4 O9 125.3(8) . . ?
O10 N4 O11 118.1(8) . . ?
O9 N4 O11 116.6(8) . . ?
C3 C4 C5 119.0(5) . . ?
C3 C4 C11 121.1(6) . . ?
C5 C4 C11 120.0(6) . . ?
C30 O5 Ho1 132.7(3) . 1_544 ?
O12 N5 O14 155.4(10) . . ?
O12 N5 O13 111.3(8) . . ?
O14 N5 O13 93.1(7) . . ?
C4 C5 C6 121.6(5) . . ?
C4 C5 C9 119.8(6) . . ?
C6 C5 C9 118.6(5) . . ?
C30 O6 Ho1 179.6(4) . 2 ?
C1 C6 C5 118.4(5) . . ?
C1 C6 C12 121.9(6) . . ?
C5 C6 C12 119.7(6) . . ?
N1 C7 C1 114.5(5) . . ?
C3 C8 N2 113.2(4) . . ?
C5 C9 N3 113.2(5) . . ?
N1 C13 C14 120.7(5) . . ?
C15 C14 C13 119.6(5) . . ?
C14 C15 C16 119.3(5) . . ?
C14 C15 C18 120.2(5) . . ?
C16 C15 C18 120.4(5) . . ?
C17 C16 C15 119.2(5) . . ?
N1 C17 C16 120.6(5) . . ?
O2 C18 O1 125.2(5) . . ?
O2 C18 C15 116.9(5) . . ?
O1 C18 C15 117.8(5) . . ?
N2 C19 C20 120.1(5) . . ?
C19 C20 C21 119.8(5) . . ?
C20 C21 C22 118.8(5) . . ?
C20 C21 C24 120.2(5) . . ?
C22 C21 C24 121.0(5) . . ?
C23 C22 C21 119.6(5) . . ?
N2 C23 C22 120.5(5) . . ?
O3 C24 O4 128.0(5) . . ?
O3 C24 C21 117.0(5) . . ?
O4 C24 C21 115.0(5) . . ?
N3 C25 C26 120.0(5) . . ?
C25 C26 C27 119.5(5) . . ?
C28 C27 C26 119.0(4) . . ?
C28 C27 C30 121.0(4) . . ?
C26 C27 C30 120.0(4) . . ?
C27 C28 C29 119.6(5) . . ?
N3 C29 C28 119.6(5) . . ?
O6 C30 O5 127.3(4) . . ?
O6 C30 C27 116.7(4) . . ?
O5 C30 C27 115.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        73.74
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         3.520
_refine_diff_density_min         -2.596
_refine_diff_density_rms         0.195
####################################################################### 
# 
# 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_yb_final
_database_code_depnum_ccdc_archive 'CCDC 1053007'
_audit_update_record             
;
2015-03-10 deposited with the CCDC.
2015-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H27 Cl N5 O14 Yb'
_chemical_formula_weight         890.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Yb Yb -7.2108 4.4329 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   9.4951(3)
_cell_length_b                   12.5595(4)
_cell_length_c                   18.9191(6)
_cell_angle_alpha                106.107(3)
_cell_angle_beta                 98.869(2)
_cell_angle_gamma                100.650(3)
_cell_volume                     2079.23(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8857
_cell_measurement_theta_min      3.74
_cell_measurement_theta_max      73.56

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.0563
_exptl_crystal_size_mid          0.0372
_exptl_crystal_size_min          0.0251
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             882
_exptl_absorpt_coefficient_mu    5.298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10762
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.77
_diffrn_reflns_theta_max         74.23
_reflns_number_total             7962
_reflns_number_gt                6872
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33'
_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)+(0.1124P)²+12.8534P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7962
_refine_ls_number_parameters     439
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0632
_refine_ls_wR_factor_ref         0.1842
_refine_ls_wR_factor_gt          0.1816
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.001 0.500 0.000 560.6 138.6
_platon_squeeze_details          
;
;
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
Yb1 Yb -0.76587(3) -0.98219(3) -0.996087(15) 0.02357(14) Uani 1 1 d . . .
O1 O -0.5422(5) -0.9705(4) -0.9123(2) 0.0280(9) Uani 1 1 d . . .
O2 O -0.3110(5) -0.9796(5) -0.8812(2) 0.0315(10) Uani 1 1 d . . .
O5 O 0.0024(5) -0.1088(4) -0.0757(3) 0.0315(10) Uani 1 1 d . . .
N1 N -0.4322(6) -0.8411(6) -0.6327(3) 0.0316(7) Uani 1 1 d . . .
O6 O -0.2365(5) -0.1812(5) -0.1163(3) 0.0380(12) Uani 1 1 d . . .
N2 N 0.0054(6) -0.8471(5) -0.3181(3) 0.0265(11) Uani 1 1 d . . .
O3 O 0.1065(5) -0.8729(5) -0.0612(3) 0.0351(11) Uani 1 1 d . . .
O4 O -0.1395(5) -0.9289(5) -0.0950(3) 0.0356(11) Uani 1 1 d . . .
N3 N -0.0455(7) -0.3896(5) -0.3273(3) 0.0308(12) Uani 1 1 d . . .
C10 C -0.0759(6) -0.7677(5) -0.4216(3) 0.0231(12) Uani 1 1 d . . .
C30 C -0.1084(7) -0.1768(6) -0.1230(4) 0.0310(14) Uani 1 1 d . . .
C2 C -0.4341(6) -0.9236(6) -0.7830(3) 0.0235(12) Uani 1 1 d . . .
C12 C -0.0945(8) -0.5809(6) -0.4267(3) 0.0281(13) Uani 1 1 d . . .
C1 C -0.4301(7) -0.9621(6) -0.8660(3) 0.0245(12) Uani 1 1 d . . .
C11 C -0.0192(6) -0.6515(5) -0.3978(3) 0.0240(12) Uani 1 1 d . . .
O7 O -0.5772(6) -0.8017(5) -0.9895(4) 0.0501(14) Uani 1 1 d . . .
C6 C -0.5596(7) -0.9036(7) -0.7596(3) 0.0354(9) Uani 1 1 d . . .
H6 H -0.6478 -0.9178 -0.7958 0.042 Uiso 1 1 calc R . .
C8 C -0.2890(7) -0.7465(7) -0.4984(3) 0.0354(9) Uani 1 1 d . . .
C3 C -0.3076(6) -0.9036(6) -0.7288(3) 0.0267(13) Uani 1 1 d . . .
H3 H -0.2200 -0.9188 -0.7434 0.032 Uiso 1 1 calc R . .
C5 C -0.5578(7) -0.8633(7) -0.6842(3) 0.0335(15) Uani 1 1 d . . .
H5 H -0.6451 -0.8509 -0.6682 0.040 Uiso 1 1 calc R . .
C13 C -0.2299(8) -0.6280(7) -0.4775(3) 0.0318(14) Uani 1 1 d . . .
C4 C -0.3100(7) -0.8615(7) -0.6534(3) 0.0322(15) Uani 1 1 d . . .
H4 H -0.2234 -0.8471 -0.6160 0.039 Uiso 1 1 calc R . .
C27 C -0.0838(7) -0.2575(6) -0.1946(4) 0.0317(14) Uani 1 1 d . . .
C20 C -0.0087(7) -0.8735(6) -0.1809(4) 0.0306(14) Uani 1 1 d . . .
C9 C -0.2135(7) -0.8170(6) -0.4716(3) 0.0287(13) Uani 1 1 d . . .
C22 C -0.1213(7) -0.8522(6) -0.2956(4) 0.0320(14) Uani 1 1 d . . .
H22 H -0.2055 -0.8467 -0.3275 0.038 Uiso 1 1 calc R . .
C17 C 0.0117(8) -0.8448(6) -0.3974(4) 0.0292(13) Uani 1 1 d . . .
H17A H 0.1153 -0.8186 -0.3998 0.035 Uiso 1 1 calc R . .
H17B H -0.0264 -0.9233 -0.4330 0.035 Uiso 1 1 calc R . .
C19 C 0.1220(8) -0.8665(7) -0.2054(5) 0.0387(17) Uani 1 1 d . . .
H19 H 0.2080 -0.8700 -0.1738 0.046 Uiso 1 1 calc R . .
C21 C -0.1309(7) -0.8652(6) -0.2268(4) 0.0312(14) Uani 1 1 d . . .
H21 H -0.2213 -0.8684 -0.2109 0.037 Uiso 1 1 calc R . .
C16 C 0.1245(7) -0.5983(6) -0.3405(4) 0.0357(15) Uani 1 1 d . . .
H16A H 0.1637 -0.6583 -0.3265 0.054 Uiso 1 1 calc R . .
H16B H 0.1080 -0.5450 -0.2955 0.054 Uiso 1 1 calc R . .
H16C H 0.1950 -0.5571 -0.3623 0.054 Uiso 1 1 calc R . .
C26 C 0.0554(8) -0.2602(6) -0.2049(4) 0.0382(16) Uani 1 1 d . . .
H26 H 0.1385 -0.2160 -0.1661 0.046 Uiso 1 1 calc R . .
C28 C -0.2023(8) -0.3242(7) -0.2501(4) 0.0367(16) Uani 1 1 d . . .
H28 H -0.2989 -0.3241 -0.2425 0.044 Uiso 1 1 calc R . .
C25 C 0.0728(8) -0.3276(6) -0.2721(4) 0.0373(16) Uani 1 1 d . . .
H25 H 0.1686 -0.3306 -0.2799 0.045 Uiso 1 1 calc R . .
C29 C -0.1820(8) -0.3906(7) -0.3162(4) 0.0365(15) Uani 1 1 d . . .
H29 H -0.2644 -0.4376 -0.3545 0.044 Uiso 1 1 calc R . .
C24 C -0.0253(9) -0.4547(6) -0.4029(4) 0.0363(16) Uani 1 1 d . . .
H24A H 0.0811 -0.4437 -0.4017 0.044 Uiso 1 1 calc R . .
H24B H -0.0683 -0.4228 -0.4411 0.044 Uiso 1 1 calc R . .
C23 C -0.0144(8) -0.8925(7) -0.1053(4) 0.0351(15) Uani 1 1 d . . .
C18 C 0.1282(8) -0.8547(7) -0.2749(5) 0.0386(16) Uani 1 1 d . . .
H18 H 0.2170 -0.8518 -0.2924 0.046 Uiso 1 1 calc R . .
C7 C -0.4390(7) -0.7979(7) -0.5498(3) 0.0354(9) Uani 1 1 d . . .
H7A H -0.4976 -0.7397 -0.5431 0.042 Uiso 1 1 calc R . .
H7B H -0.4897 -0.8621 -0.5352 0.042 Uiso 1 1 calc R . .
C14 C -0.3151(10) -0.5559(9) -0.5113(4) 0.051(2) Uani 1 1 d . . .
H14A H -0.3958 -0.5433 -0.4858 0.077 Uiso 1 1 calc R . .
H14B H -0.3550 -0.5957 -0.5652 0.077 Uiso 1 1 calc R . .
H14C H -0.2493 -0.4822 -0.5047 0.077 Uiso 1 1 calc R . .
C15 C -0.2746(11) -0.9443(8) -0.4967(5) 0.055(2) Uani 1 1 d . . .
H15A H -0.3739 -0.9634 -0.5279 0.083 Uiso 1 1 calc R . .
H15B H -0.2783 -0.9699 -0.4525 0.083 Uiso 1 1 calc R . .
H15C H -0.2115 -0.9824 -0.5262 0.083 Uiso 1 1 calc R . .
O8 O -0.7229(6) -1.1791(5) -1.0281(3) 0.0433(13) Uani 1 1 d . . .
N4 N -0.1008(7) -0.1607(6) -0.3986(3) 0.0316(7) Uani 1 1 d D . .
O14 O 0.3786(9) -0.3165(10) -0.1724(4) 0.094(3) Uani 1 1 d . . .
O12 O 0.4008(7) -0.3628(6) -0.2883(4) 0.0545(16) Uani 1 1 d . . .
N5 N 0.4195(6) -0.3705(6) -0.2244(3) 0.0316(7) Uani 1 1 d . . .
O13 O 0.4858(11) -0.4460(9) -0.2135(7) 0.094(3) Uani 1 1 d . . .
O11 O -0.2164(13) -0.2442(13) -0.4264(6) 0.115(4) Uani 1 1 d . . .
O10 O -0.0075(14) -0.1194(14) -0.4289(8) 0.176(8) Uani 1 1 d D . .
O9 O -0.0583(16) -0.1307(13) -0.3292(4) 0.218(11) Uani 1 1 d D . .
Cl1 Cl -0.4990(3) -1.1478(3) -0.6760(2) 0.0960(12) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O1 2.400(4) . ?
Yb1 O3 2.442(5) 1_454 ?
Yb1 O5 2.448(5) 1_444 ?
Yb1 O2 2.487(4) 2_433 ?
Yb1 O4 2.489(5) 2_434 ?
Yb1 O8 2.503(5) . ?
Yb1 O6 2.506(5) 2_444 ?
Yb1 O7 2.576(6) . ?
Yb1 O5 3.037(5) 2_444 ?
Yb1 C30 3.115(6) 2_444 ?
Yb1 Yb1 4.3608(6) 2_333 ?
O1 C1 1.238(8) . ?
O2 C1 1.252(7) . ?
O2 Yb1 2.487(4) 2_433 ?
O5 C30 1.262(8) . ?
O5 Yb1 2.448(4) 1_666 ?
O5 Yb1 3.037(5) 2_444 ?
N1 C4 1.326(8) . ?
N1 C5 1.348(9) . ?
N1 C7 1.526(8) . ?
O6 C30 1.235(8) . ?
O6 Yb1 2.506(5) 2_444 ?
N2 C22 1.333(9) . ?
N2 C18 1.350(9) . ?
N2 C17 1.519(8) . ?
O3 C23 1.250(9) . ?
O3 Yb1 2.442(5) 1_656 ?
O4 C23 1.256(9) . ?
O4 Yb1 2.489(5) 2_434 ?
N3 C29 1.343(9) . ?
N3 C25 1.350(10) . ?
N3 C24 1.499(8) . ?
C10 C11 1.376(9) . ?
C10 C9 1.407(8) . ?
C10 C17 1.505(9) . ?
C30 C27 1.529(9) . ?
C30 Yb1 3.115(6) 2_444 ?
C2 C6 1.375(9) . ?
C2 C3 1.387(8) . ?
C2 C1 1.517(7) . ?
C12 C13 1.395(10) . ?
C12 C11 1.407(9) . ?
C12 C24 1.508(10) . ?
C11 C16 1.513(8) . ?
C6 C5 1.372(9) . ?
C8 C9 1.388(11) . ?
C8 C13 1.408(11) . ?
C8 C7 1.509(9) . ?
C3 C4 1.384(8) . ?
C13 C14 1.522(10) . ?
C27 C28 1.368(10) . ?
C27 C26 1.370(10) . ?
C20 C21 1.378(9) . ?
C20 C19 1.387(9) . ?
C20 C23 1.520(9) . ?
C9 C15 1.507(11) . ?
C22 C21 1.371(10) . ?
C19 C18 1.374(11) . ?
C26 C25 1.371(10) . ?
C28 C29 1.361(10) . ?
N4 O10 1.2385(10) . ?
N4 O9 1.2384(10) . ?
N4 O11 1.292(15) . ?
O14 N5 1.193(10) . ?
O12 N5 1.228(9) . ?
N5 O13 1.275(11) . ?

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 Yb1 O3 143.05(18) . 1_454 ?
O1 Yb1 O5 145.07(17) . 1_444 ?
O3 Yb1 O5 71.76(17) 1_454 1_444 ?
O1 Yb1 O2 101.04(14) . 2_433 ?
O3 Yb1 O2 76.21(16) 1_454 2_433 ?
O5 Yb1 O2 82.16(16) 1_444 2_433 ?
O1 Yb1 O4 78.45(15) . 2_434 ?
O3 Yb1 O4 124.85(15) 1_454 2_434 ?
O5 Yb1 O4 79.51(17) 1_444 2_434 ?
O2 Yb1 O4 144.71(19) 2_433 2_434 ?
O1 Yb1 O8 73.43(17) . . ?
O3 Yb1 O8 136.73(18) 1_454 . ?
O5 Yb1 O8 74.38(17) 1_444 . ?
O2 Yb1 O8 73.19(19) 2_433 . ?
O4 Yb1 O8 72.94(19) 2_434 . ?
O1 Yb1 O6 78.28(16) . 2_444 ?
O3 Yb1 O6 81.39(18) 1_454 2_444 ?
O5 Yb1 O6 120.91(15) 1_444 2_444 ?
O2 Yb1 O6 140.47(19) 2_433 2_444 ?
O4 Yb1 O6 74.51(19) 2_434 2_444 ?
O8 Yb1 O6 140.26(19) . 2_444 ?
O1 Yb1 O7 71.95(19) . . ?
O3 Yb1 O7 72.12(18) 1_454 . ?
O5 Yb1 O7 139.90(19) 1_444 . ?
O2 Yb1 O7 72.9(2) 2_433 . ?
O4 Yb1 O7 136.9(2) 2_434 . ?
O8 Yb1 O7 124.8(2) . . ?
O6 Yb1 O7 69.4(2) 2_444 . ?
O1 Yb1 O5 116.84(13) . 2_444 ?
O3 Yb1 O5 64.91(15) 1_454 2_444 ?
O5 Yb1 O5 75.20(15) 1_444 2_444 ?
O2 Yb1 O5 139.39(14) 2_433 2_444 ?
O4 Yb1 O5 62.69(15) 2_434 2_444 ?
O8 Yb1 O5 129.61(17) . 2_444 ?
O6 Yb1 O5 45.71(13) 2_444 2_444 ?
O7 Yb1 O5 104.26(17) . 2_444 ?
O1 Yb1 C30 96.44(16) . 2_444 ?
O3 Yb1 C30 73.33(18) 1_454 2_444 ?
O5 Yb1 C30 98.79(17) 1_444 2_444 ?
O2 Yb1 C30 147.44(18) 2_433 2_444 ?
O4 Yb1 C30 65.77(19) 2_434 2_444 ?
O8 Yb1 C30 138.7(2) . 2_444 ?
O6 Yb1 C30 22.16(17) 2_444 2_444 ?
O7 Yb1 C30 87.0(2) . 2_444 ?
O5 Yb1 C30 23.62(15) 2_444 2_444 ?
O1 Yb1 Yb1 140.78(10) . 2_333 ?
O3 Yb1 Yb1 61.90(11) 1_454 2_333 ?
O5 Yb1 Yb1 42.33(11) 1_444 2_333 ?
O2 Yb1 Yb1 116.88(10) 2_433 2_333 ?
O4 Yb1 Yb1 65.06(10) 2_434 2_333 ?
O8 Yb1 Yb1 107.03(13) . 2_333 ?
O6 Yb1 Yb1 78.58(11) 2_444 2_333 ?
O7 Yb1 Yb1 126.94(13) . 2_333 ?
O5 Yb1 Yb1 32.87(8) 2_444 2_333 ?
C30 Yb1 Yb1 56.48(13) 2_444 2_333 ?
C1 O1 Yb1 176.6(4) . . ?
C1 O2 Yb1 129.7(4) . 2_433 ?
C30 O5 Yb1 173.0(4) . 1_666 ?
C30 O5 Yb1 81.7(4) . 2_444 ?
Yb1 O5 Yb1 104.80(15) 1_666 2_444 ?
C4 N1 C5 121.1(6) . . ?
C4 N1 C7 121.6(5) . . ?
C5 N1 C7 117.2(5) . . ?
C30 O6 Yb1 107.9(4) . 2_444 ?
C22 N2 C18 122.1(6) . . ?
C22 N2 C17 120.1(6) . . ?
C18 N2 C17 117.5(5) . . ?
C23 O3 Yb1 135.5(5) . 1_656 ?
C23 O4 Yb1 135.1(4) . 2_434 ?
C29 N3 C25 120.7(6) . . ?
C29 N3 C24 119.2(6) . . ?
C25 N3 C24 120.0(6) . . ?
C11 C10 C9 120.7(6) . . ?
C11 C10 C17 120.4(6) . . ?
C9 C10 C17 118.8(6) . . ?
O6 C30 O5 124.4(6) . . ?
O6 C30 C27 117.4(6) . . ?
O5 C30 C27 118.2(6) . . ?
O6 C30 Yb1 50.0(3) . 2_444 ?
O5 C30 Yb1 74.7(4) . 2_444 ?
C27 C30 Yb1 165.4(4) . 2_444 ?
C6 C2 C3 118.6(5) . . ?
C6 C2 C1 121.5(5) . . ?
C3 C2 C1 119.8(5) . . ?
C13 C12 C11 120.1(6) . . ?
C13 C12 C24 121.0(6) . . ?
C11 C12 C24 118.9(6) . . ?
O1 C1 O2 125.7(5) . . ?
O1 C1 C2 117.8(5) . . ?
O2 C1 C2 116.4(5) . . ?
C10 C11 C12 120.2(6) . . ?
C10 C11 C16 120.5(6) . . ?
C12 C11 C16 119.3(6) . . ?
C5 C6 C2 120.1(6) . . ?
C9 C8 C13 121.5(6) . . ?
C9 C8 C7 119.1(7) . . ?
C13 C8 C7 119.4(7) . . ?
C4 C3 C2 119.4(6) . . ?
N1 C5 C6 120.1(6) . . ?
C12 C13 C8 118.7(6) . . ?
C12 C13 C14 122.3(7) . . ?
C8 C13 C14 119.0(7) . . ?
N1 C4 C3 120.6(6) . . ?
C28 C27 C26 119.8(7) . . ?
C28 C27 C30 119.3(6) . . ?
C26 C27 C30 120.8(6) . . ?
C21 C20 C19 118.6(6) . . ?
C21 C20 C23 121.8(6) . . ?
C19 C20 C23 119.5(6) . . ?
C8 C9 C10 118.7(6) . . ?
C8 C9 C15 121.2(7) . . ?
C10 C9 C15 120.1(7) . . ?
N2 C22 C21 120.4(6) . . ?
C10 C17 N2 112.5(5) . . ?
C18 C19 C20 120.5(7) . . ?
C22 C21 C20 119.6(6) . . ?
C27 C26 C25 118.9(7) . . ?
C29 C28 C27 120.0(7) . . ?
N3 C25 C26 120.4(6) . . ?
N3 C29 C28 120.0(7) . . ?
N3 C24 C12 113.7(5) . . ?
O3 C23 O4 127.2(7) . . ?
O3 C23 C20 116.1(6) . . ?
O4 C23 C20 116.6(6) . . ?
N2 C18 C19 118.7(6) . . ?
C8 C7 N1 112.6(5) . . ?
O10 N4 O9 111.9(11) . . ?
O10 N4 O11 131.2(10) . . ?
O9 N4 O11 115.2(9) . . ?
O14 N5 O12 126.4(8) . . ?
O14 N5 O13 117.2(9) . . ?
O12 N5 O13 116.3(7) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        74.23
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         3.137
_refine_diff_density_min         -2.562
_refine_diff_density_rms         0.195
