# 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_Comp5_Dy
_database_code_depnum_ccdc_archive 'CCDC 1054115'
_audit_update_record             
;
2015-11-10 deposited with the CCDC.
2015-11-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H33 Dy N3 O9'
_chemical_formula_weight         778.12

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3803(5)
_cell_length_b                   11.3508(6)
_cell_length_c                   12.9894(7)
_cell_angle_alpha                72.4350(10)
_cell_angle_beta                 89.8670(10)
_cell_angle_gamma                87.3720(10)
_cell_volume                     1457.47(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11541
_cell_measurement_theta_min      2.547
_cell_measurement_theta_max      28.325

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            White
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_F_000             780
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    2.628
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'

_exptl_special_details           
;
Crystal structure have some disorder problems. The crystal structure contains a percentage of voids occupied by disordered solvent molecules. We have used SQUEEZE routine to eliminate one crystallization DMF molecule.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17403
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.644
_diffrn_reflns_theta_max         28.403
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6697
_reflns_number_gt                6355
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker ApexII'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        'Bruker Apex II'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ViewerLite 5.0 (Acccelrys)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0266P)²+2.1053P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6697
_refine_ls_number_parameters     374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0584
_refine_ls_wR_factor_gt          0.0577
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.47900(2) 0.04557(2) 0.33970(2) 0.01108(4) Uani 1 1 d . . . . .
C1A C 0.4947(3) 0.2659(2) 0.1705(2) 0.0179(5) Uani 1 1 d . . . . .
C1B C 0.5093(2) -0.2453(2) 0.5059(2) 0.0131(5) Uani 1 1 d . . . . .
C1C C 0.2665(2) 0.0091(2) 0.5646(2) 0.0148(5) Uani 1 1 d . . . . .
C2A C 0.4982(3) 0.3853(3) 0.0857(2) 0.0216(6) Uani 1 1 d . . . . .
C2B C 0.5054(3) -0.3783(2) 0.5055(2) 0.0131(5) Uani 1 1 d . . . . .
C2C C 0.1295(3) 0.0046(3) 0.5301(2) 0.0176(5) Uani 1 1 d . . . . .
C2D C 0.1878(3) 0.0206(3) 0.2331(3) 0.0286(7) Uani 1 1 d . . . . .
H2D H 0.1917 0.0996 0.1846 0.034 Uiso 1 1 calc R U . . .
C2E C 0.5817(3) -0.1297(3) 0.1965(3) 0.0331(8) Uani 1 1 d . . . . .
H2E H 0.5684 -0.1921 0.2605 0.040 Uiso 1 1 calc R U . . .
C3A C 0.4481(3) 0.4949(3) 0.1021(3) 0.0282(7) Uani 1 1 d . . . . .
C3B C 0.3894(3) -0.4392(2) 0.5277(2) 0.0169(5) Uani 1 1 d . . . . .
C3C C 0.0767(3) 0.0977(3) 0.4408(2) 0.0185(5) Uani 1 1 d . . . . .
C4A C 0.3984(4) 0.4961(3) 0.2058(3) 0.0348(8) Uani 1 1 d . . . . .
H4A H 0.4000 0.4227 0.2625 0.042 Uiso 1 1 calc R U . . .
C4B C 0.2743(3) -0.3797(3) 0.5525(3) 0.0314(7) Uani 1 1 d . . . . .
H4B H 0.2762 -0.2992 0.5559 0.038 Uiso 1 1 calc R U . . .
C4C C 0.1497(3) 0.1989(3) 0.3800(2) 0.0220(6) Uani 1 1 d . . . . .
H4C H 0.2346 0.2040 0.4003 0.026 Uiso 1 1 calc R U . . .
C4D C 0.0669(5) -0.1624(5) 0.3037(4) 0.0568(11) Uani 1 1 d . . . . .
H4D1 H 0.1402 -0.1861 0.3516 0.085 Uiso 1 1 d R U . . .
H4D2 H 0.0591 -0.2210 0.2642 0.085 Uiso 1 1 d R U . . .
H4D3 H -0.0097 -0.1609 0.3449 0.085 Uiso 1 1 d R U . . .
C4E C 0.6795(4) -0.0707(5) 0.0219(4) 0.0594(13) Uani 1 1 d . . . . .
H4E1 H 0.6506 0.0104 0.0231 0.089 Uiso 1 1 d R U . . .
H4E2 H 0.6348 -0.0913 -0.0345 0.089 Uiso 1 1 d R U . . .
H4E3 H 0.7706 -0.0720 0.0088 0.089 Uiso 1 1 d R U . . .
C5A C 0.3498(5) 0.6011(4) 0.2222(3) 0.0489(11) Uani 1 1 d . . . . .
H5A H 0.3189 0.5997 0.2898 0.059 Uiso 1 1 calc R U . . .
C5B C 0.1619(3) -0.4393(4) 0.5711(4) 0.0498(11) Uani 1 1 d . . . . .
H5B H 0.0875 -0.3990 0.5862 0.060 Uiso 1 1 calc R U . . .
C5C C 0.0974(3) 0.2876(3) 0.2933(3) 0.0280(7) Uani 1 1 d . . . . .
H5C H 0.1468 0.3522 0.2544 0.034 Uiso 1 1 calc R U . . .
C5D C -0.0193(4) 0.0098(5) 0.1516(3) 0.0543(11) Uani 1 1 d . . . . .
H5D1 H -0.0004 0.0929 0.1110 0.081 Uiso 1 1 d R U . . .
H5D2 H -0.0995 0.0106 0.1884 0.081 Uiso 1 1 d R U . . .
H5D3 H -0.0259 -0.0393 0.1034 0.081 Uiso 1 1 d R U . . .
C5E C 0.7060(6) -0.2852(5) 0.1408(4) 0.0791(19) Uani 1 1 d . . . . .
H5E1 H 0.6898 -0.3341 0.2136 0.119 Uiso 1 1 d R U . . .
H5E2 H 0.7973 -0.2839 0.1288 0.119 Uiso 1 1 d R U . . .
H5E3 H 0.6654 -0.3204 0.0914 0.119 Uiso 1 1 d R U . . .
C6A C 0.3455(5) 0.7148(4) 0.1357(3) 0.0517(11) Uani 1 1 d . . . . .
H6A H 0.3103 0.7865 0.1472 0.062 Uiso 1 1 calc R U . . .
C6B C 0.1576(3) -0.5629(3) 0.5676(4) 0.0478(11) Uani 1 1 d . . . . .
H6B H 0.0803 -0.6030 0.5809 0.057 Uiso 1 1 calc R U . . .
C6C C -0.0327(3) 0.2817(3) 0.2619(3) 0.0287(7) Uani 1 1 d . . . . .
H6C H -0.0676 0.3426 0.2023 0.034 Uiso 1 1 calc R U . . .
C7A C 0.3923(4) 0.7191(3) 0.0372(3) 0.0399(9) Uani 1 1 d . . . . .
H7A H 0.3895 0.7940 -0.0177 0.048 Uiso 1 1 calc R U . . .
C7B C 0.2649(3) -0.6235(3) 0.5451(3) 0.0308(7) Uani 1 1 d . . . . .
H7B H 0.2606 -0.7050 0.5446 0.037 Uiso 1 1 calc R U . . .
C7C C -0.1067(3) 0.1886(3) 0.3176(2) 0.0229(6) Uani 1 1 d . . . . .
H7C H -0.1918 0.1870 0.2960 0.028 Uiso 1 1 calc R U . . .
C8A C 0.4461(3) 0.6103(3) 0.0161(3) 0.0301(7) Uani 1 1 d . . . . .
C8B C 0.3842(3) -0.5634(2) 0.5221(2) 0.0181(5) Uani 1 1 d . . . . .
C8C C -0.0552(3) 0.0924(3) 0.4095(2) 0.0191(5) Uani 1 1 d . . . . .
N3D N 0.0832(3) -0.0425(3) 0.2299(3) 0.0392(7) Uani 1 1 d . . . . .
N3E N 0.6536(3) -0.1590(3) 0.1236(2) 0.0439(8) Uani 1 1 d . . . . .
O1A O 0.38672(18) 0.21701(17) 0.19472(15) 0.0186(4) Uani 1 1 d . . . . .
O1B O 0.49139(18) -0.16635(16) 0.41492(14) 0.0156(4) Uani 1 1 d . . . . .
O1C O 0.35951(17) -0.00634(16) 0.50523(14) 0.0143(4) Uani 1 1 d . . . . .
O1D O 0.27815(19) -0.01837(19) 0.29515(16) 0.0218(4) Uani 1 1 d . . . . .
O1E O 0.52990(19) -0.02632(18) 0.18786(15) 0.0212(4) Uani 1 1 d . . . . .
O2A O 0.59665(19) 0.21370(18) 0.21748(16) 0.0203(4) Uani 1 1 d . . . . .
O2B O 0.53038(19) -0.22425(16) 0.59375(15) 0.0166(4) Uani 1 1 d . . . . .
O2C O 0.71245(18) -0.01943(19) 0.34393(15) 0.0199(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1B 2.3046(17) . ?
Dy1 O1D 2.3678(19) . ?
Dy1 O1E 2.4005(19) . ?
Dy1 O1C 2.4080(18) . ?
Dy1 O1A 2.4241(19) . ?
Dy1 O2B 2.4309(18) 2_656 ?
Dy1 O2A 2.4556(19) . ?
Dy1 O2C 2.4963(19) . ?
Dy1 O1C 2.5439(18) 2_656 ?
Dy1 C1A 2.798(3) . ?
Dy1 C1C 2.882(3) 2_656 ?
Dy1 Dy1 3.9962(3) 2_656 ?
C1A O2A 1.254(3) . ?
C1A O1A 1.270(3) . ?
C1A C2A 1.468(4) . ?
C1B O2B 1.256(3) . ?
C1B O1B 1.257(3) . ?
C1B C2B 1.513(3) . ?
C1C O2C 1.249(3) 2_656 ?
C1C O1C 1.273(3) . ?
C1C C2C 1.500(4) . ?
C1C Dy1 2.882(3) 2_656 ?
C2A C3A 1.401(4) . ?
C2A C8A 1.430(4) 2_665 ?
C2B C8B 1.398(4) 2_646 ?
C2B C3B 1.402(4) . ?
C2C C3C 1.404(4) . ?
C2C C8C 1.406(4) 2_556 ?
C2D O1D 1.215(4) . ?
C2D N3D 1.335(4) . ?
C2E O1E 1.241(4) . ?
C2E N3E 1.316(4) . ?
C3A C8A 1.443(4) . ?
C3A C4A 1.444(5) . ?
C3B C4B 1.430(4) . ?
C3B C8B 1.436(4) . ?
C3C C4C 1.430(4) . ?
C3C C8C 1.438(4) . ?
C4A C5A 1.349(5) . ?
C4B C5B 1.360(5) . ?
C4C C5C 1.358(4) . ?
C4D N3D 1.426(6) . ?
C4E N3E 1.430(6) . ?
C5A C6A 1.432(5) . ?
C5B C6B 1.420(5) . ?
C5C C6C 1.422(4) . ?
C5D N3D 1.450(5) . ?
C5E N3E 1.460(5) . ?
C6A C7A 1.355(5) . ?
C6B C7B 1.360(4) . ?
C6C C7C 1.356(4) . ?
C7A C8A 1.432(5) . ?
C7B C8B 1.429(4) . ?
C7C C8C 1.437(4) . ?
C8A C2A 1.430(4) 2_665 ?
C8B C2B 1.398(4) 2_646 ?
C8C C2C 1.406(4) 2_556 ?
O1C Dy1 2.5439(18) 2_656 ?
O2B Dy1 2.4310(18) 2_656 ?
O2C C1C 1.249(3) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1B Dy1 O1D 75.79(7) . . ?
O1B Dy1 O1E 77.13(7) . . ?
O1D Dy1 O1E 77.03(7) . . ?
O1B Dy1 O1C 71.56(6) . . ?
O1D Dy1 O1C 74.85(6) . . ?
O1E Dy1 O1C 141.98(6) . . ?
O1B Dy1 O1A 145.22(6) . . ?
O1D Dy1 O1A 73.78(7) . . ?
O1E Dy1 O1A 80.00(7) . . ?
O1C Dy1 O1A 115.30(6) . . ?
O1B Dy1 O2B 136.35(6) . 2_656 ?
O1D Dy1 O2B 115.82(7) . 2_656 ?
O1E Dy1 O2B 144.95(7) . 2_656 ?
O1C Dy1 O2B 71.77(6) . 2_656 ?
O1A Dy1 O2B 73.56(6) . 2_656 ?
O1B Dy1 O2A 140.89(7) . . ?
O1D Dy1 O2A 123.57(7) . . ?
O1E Dy1 O2A 75.59(7) . . ?
O1C Dy1 O2A 142.05(6) . . ?
O1A Dy1 O2A 53.51(6) . . ?
O2B Dy1 O2A 70.29(6) 2_656 . ?
O1B Dy1 O2C 73.68(7) . . ?
O1D Dy1 O2C 138.77(7) . . ?
O1E Dy1 O2C 69.69(6) . . ?
O1C Dy1 O2C 119.42(6) . . ?
O1A Dy1 O2C 121.60(6) . . ?
O2B Dy1 O2C 105.39(6) 2_656 . ?
O2A Dy1 O2C 70.85(6) . . ?
O1B Dy1 O1C 75.40(6) . 2_656 ?
O1D Dy1 O1C 141.68(6) . 2_656 ?
O1E Dy1 O1C 119.79(6) . 2_656 ?
O1C Dy1 O1C 72.43(6) . 2_656 ?
O1A Dy1 O1C 139.26(6) . 2_656 ?
O2B Dy1 O1C 71.60(6) 2_656 2_656 ?
O2A Dy1 O1C 94.65(6) . 2_656 ?
O2C Dy1 O1C 51.53(6) . 2_656 ?
O1B Dy1 C1A 154.34(7) . . ?
O1D Dy1 C1A 99.30(8) . . ?
O1E Dy1 C1A 77.23(7) . . ?
O1C Dy1 C1A 132.22(7) . . ?
O1A Dy1 C1A 26.94(7) . . ?
O2B Dy1 C1A 68.73(7) 2_656 . ?
O2A Dy1 C1A 26.60(7) . . ?
O2C Dy1 C1A 96.42(7) . . ?
O1C Dy1 C1A 117.37(7) 2_656 . ?
O1B Dy1 C1C 75.42(7) . 2_656 ?
O1D Dy1 C1C 151.17(7) . 2_656 ?
O1E Dy1 C1C 95.06(7) . 2_656 ?
O1C Dy1 C1C 97.36(7) . 2_656 ?
O1A Dy1 C1C 132.79(7) . 2_656 ?
O2B Dy1 C1C 86.63(7) 2_656 2_656 ?
O2A Dy1 C1C 79.64(7) . 2_656 ?
O2C Dy1 C1C 25.59(7) . 2_656 ?
O1C Dy1 C1C 26.19(7) 2_656 2_656 ?
C1A Dy1 C1C 105.97(8) . 2_656 ?
O1B Dy1 Dy1 69.45(4) . 2_656 ?
O1D Dy1 Dy1 110.00(5) . 2_656 ?
O1E Dy1 Dy1 142.27(5) . 2_656 ?
O1C Dy1 Dy1 37.36(4) . 2_656 ?
O1A Dy1 Dy1 137.71(5) . 2_656 ?
O2B Dy1 Dy1 67.08(4) 2_656 2_656 ?
O2A Dy1 Dy1 121.79(5) . 2_656 ?
O2C Dy1 Dy1 84.26(4) . 2_656 ?
O1C Dy1 Dy1 35.06(4) 2_656 2_656 ?
C1A Dy1 Dy1 134.23(5) . 2_656 ?
C1C Dy1 Dy1 60.40(5) 2_656 2_656 ?
O2A C1A O1A 121.1(2) . . ?
O2A C1A C2A 120.3(3) . . ?
O1A C1A C2A 118.7(3) . . ?
O2A C1A Dy1 61.28(14) . . ?
O1A C1A Dy1 59.88(13) . . ?
C2A C1A Dy1 176.5(2) . . ?
O2B C1B O1B 126.8(2) . . ?
O2B C1B C2B 118.6(2) . . ?
O1B C1B C2B 114.6(2) . . ?
O2C C1C O1C 120.6(2) 2_656 . ?
O2C C1C C2C 118.6(2) 2_656 . ?
O1C C1C C2C 120.6(2) . . ?
O2C C1C Dy1 59.67(13) 2_656 2_656 ?
O1C C1C Dy1 61.90(13) . 2_656 ?
C2C C1C Dy1 165.80(18) . 2_656 ?
C3A C2A C8A 119.3(3) . 2_665 ?
C3A C2A C1A 121.6(3) . . ?
C8A C2A C1A 119.1(3) 2_665 . ?
C8B C2B C3B 120.9(2) 2_646 . ?
C8B C2B C1B 119.5(2) 2_646 . ?
C3B C2B C1B 119.6(2) . . ?
C3C C2C C8C 121.3(2) . 2_556 ?
C3C C2C C1C 120.1(2) . . ?
C8C C2C C1C 118.6(2) 2_556 . ?
O1D C2D N3D 124.3(3) . . ?
O1E C2E N3E 126.0(3) . . ?
C2A C3A C8A 120.9(3) . . ?
C2A C3A C4A 121.1(3) . . ?
C8A C3A C4A 118.0(3) . . ?
C2B C3B C4B 121.8(2) . . ?
C2B C3B C8B 119.5(2) . . ?
C4B C3B C8B 118.7(3) . . ?
C2C C3C C4C 122.1(2) . . ?
C2C C3C C8C 119.3(3) . . ?
C4C C3C C8C 118.6(3) . . ?
C5A C4A C3A 121.5(3) . . ?
C5B C4B C3B 120.9(3) . . ?
C5C C4C C3C 121.3(3) . . ?
C4A C5A C6A 120.1(3) . . ?
C4B C5B C6B 120.3(3) . . ?
C4C C5C C6C 120.0(3) . . ?
C7A C6A C5A 120.7(3) . . ?
C7B C6B C5B 120.9(3) . . ?
C7C C6C C5C 121.1(3) . . ?
C6A C7A C8A 121.3(3) . . ?
C6B C7B C8B 120.7(3) . . ?
C6C C7C C8C 120.8(3) . . ?
C2A C8A C7A 121.8(3) 2_665 . ?
C2A C8A C3A 119.7(3) 2_665 . ?
C7A C8A C3A 118.4(3) . . ?
C2B C8B C7B 121.9(2) 2_646 . ?
C2B C8B C3B 119.6(2) 2_646 . ?
C7B C8B C3B 118.5(3) . . ?
C2C C8C C7C 122.4(3) 2_556 . ?
C2C C8C C3C 119.4(3) 2_556 . ?
C7C C8C C3C 118.2(3) . . ?
C2D N3D C4D 121.7(3) . . ?
C2D N3D C5D 120.8(4) . . ?
C4D N3D C5D 117.5(3) . . ?
C2E N3E C4E 121.8(3) . . ?
C2E N3E C5E 121.3(4) . . ?
C4E N3E C5E 116.8(4) . . ?
C1A O1A Dy1 93.18(16) . . ?
C1B O1B Dy1 139.00(16) . . ?
C1C O1C Dy1 153.31(17) . . ?
C1C O1C Dy1 91.91(15) . 2_656 ?
Dy1 O1C Dy1 107.57(6) . 2_656 ?
C2D O1D Dy1 139.7(2) . . ?
C2E O1E Dy1 123.37(19) . . ?
C1A O2A Dy1 92.12(16) . . ?
C1B O2B Dy1 136.89(16) . 2_656 ?
C1C O2C Dy1 94.74(15) 2_656 . ?

_refine_diff_density_max         1.965
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.100

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 0.000 0.500 1.000 216 39 ' '
_platon_squeeze_details          
;
;
# start Validation Reply Form
_vrf_CHEMW03_Comp5_Dy            
;
PROBLEM: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
RESPONSE: The crystal structure contains a percentage of voids occupied by
disordered solvent molecules. We have used SQUEZZE routine to eliminate
one DMF molecule.
;
# end Validation Reply Form


_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_Comp3_Gd
_database_code_depnum_ccdc_archive 'CCDC 1421044'
_audit_update_record             
;
2015-11-10 deposited with the CCDC.
2015-11-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H33 Gd N3 O9'
_chemical_formula_weight         772.87

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3541(12)
_cell_length_b                   11.3680(13)
_cell_length_c                   12.9160(15)
_cell_angle_alpha                72.8590(10)
_cell_angle_beta                 90.0280(10)
_cell_angle_gamma                87.2320(10)
_cell_volume                     1450.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3052
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      21.40

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            White
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    2.350
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'

_exptl_special_details           
;
Crystal structure have some disorder problems. The crystal structure contains a percentage of voids occupied by disordered solvent molecules. We have used SQUEEZE routine to eliminate one crystallization DMF molecule.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16568
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.650
_diffrn_reflns_theta_max         28.462
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6657
_reflns_number_gt                5419
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker ApexII'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        'Bruker Apex II'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ViewerLite 5.0 (Acccelrys)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0558P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6657
_refine_ls_number_parameters     374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0450
_refine_ls_wR_factor_ref         0.1030
_refine_ls_wR_factor_gt          0.0974
_refine_ls_goodness_of_fit_ref   0.943
_refine_ls_restrained_S_all      0.943
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.47833(2) 0.04611(2) 0.33838(2) 0.01707(8) Uani 1 1 d . . . . .
C1A C 0.4946(5) 0.2662(5) 0.1677(4) 0.0240(11) Uani 1 1 d . . . . .
C1B C 0.5105(5) -0.2463(4) 0.5046(4) 0.0192(10) Uani 1 1 d . . . . .
C1C C 0.2658(5) 0.0097(5) 0.5641(4) 0.0220(11) Uani 1 1 d . . . . .
C2A C 0.4983(5) 0.3848(5) 0.0843(4) 0.0278(12) Uani 1 1 d . . . . .
C2B C 0.5056(5) -0.3788(4) 0.5053(4) 0.0199(10) Uani 1 1 d . . . . .
C2C C 0.1295(6) 0.0048(5) 0.5313(5) 0.0307(13) Uani 1 1 d . . . . .
C2D C 0.1849(8) 0.0206(7) 0.2334(6) 0.0544(19) Uani 1 1 d . . . . .
H2D H 0.1866 0.1009 0.1878 0.065 Uiso 1 1 calc R U . . .
C2E C 0.5843(7) -0.1292(6) 0.1931(5) 0.0435(16) Uani 1 1 d . . . . .
H2E H 0.5726 -0.1917 0.2571 0.052 Uiso 1 1 calc R U . . .
C3A C 0.4486(6) 0.4941(5) 0.1030(5) 0.0371(14) Uani 1 1 d . . . . .
C3B C 0.3901(5) -0.4381(5) 0.5276(4) 0.0258(12) Uani 1 1 d . . . . .
C3C C 0.0762(5) 0.0971(5) 0.4418(5) 0.0303(12) Uani 1 1 d . . . . .
C4A C 0.3977(7) 0.4968(6) 0.2055(5) 0.0432(16) Uani 1 1 d . . . . .
H4A H 0.3984 0.4239 0.2622 0.052 Uiso 1 1 calc R U . . .
C4B C 0.2752(6) -0.3788(6) 0.5528(7) 0.055(2) Uani 1 1 d . . . . .
H4B H 0.2775 -0.2986 0.5569 0.067 Uiso 1 1 calc R U . . .
C4C C 0.1493(6) 0.1982(5) 0.3809(5) 0.0365(14) Uani 1 1 d . . . . .
H4C H 0.2346 0.2032 0.4013 0.044 Uiso 1 1 calc R U . . .
C4D C 0.0659(9) -0.1599(9) 0.3016(7) 0.084(3) Uani 1 1 d . . . . .
H4D1 H 0.1418 -0.1825 0.3472 0.126 Uiso 1 1 calc R U . . .
H4D2 H 0.0557 -0.2191 0.2628 0.126 Uiso 1 1 calc R U . . .
H4D3 H -0.0086 -0.1581 0.3455 0.126 Uiso 1 1 calc R U . . .
C4E C 0.6832(8) -0.0695(9) 0.0212(7) 0.075(3) Uani 1 1 d . . . . .
H4E1 H 0.6340 -0.0846 -0.0362 0.112 Uiso 1 1 calc R U . . .
H4E2 H 0.7738 -0.0755 0.0066 0.112 Uiso 1 1 calc R U . . .
H4E3 H 0.6602 0.0116 0.0259 0.112 Uiso 1 1 calc R U . . .
C5A C 0.3495(8) 0.6004(6) 0.2222(6) 0.060(2) Uani 1 1 d . . . . .
H5A H 0.3185 0.5989 0.2901 0.072 Uiso 1 1 calc R U . . .
C5B C 0.1644(7) -0.4361(7) 0.5707(9) 0.091(4) Uani 1 1 d . . . . .
H5B H 0.0903 -0.3949 0.5859 0.110 Uiso 1 1 calc R U . . .
C5C C 0.0967(6) 0.2865(6) 0.2944(6) 0.0474(17) Uani 1 1 d . . . . .
H5C H 0.1453 0.3517 0.2566 0.057 Uiso 1 1 calc R U . . .
C5D C -0.0218(9) 0.0099(10) 0.1526(7) 0.088(3) Uani 1 1 d . . . . .
H5D1 H -0.0074 0.0954 0.1186 0.131 Uiso 1 1 calc R U . . .
H5D2 H -0.1028 0.0027 0.1895 0.131 Uiso 1 1 calc R U . . .
H5D3 H -0.0239 -0.0325 0.0985 0.131 Uiso 1 1 calc R U . . .
C5E C 0.7114(10) -0.2827(9) 0.1359(8) 0.098(4) Uani 1 1 d . . . . .
H5E1 H 0.8028 -0.2800 0.1236 0.147 Uiso 1 1 calc R U . . .
H5E2 H 0.6714 -0.3183 0.0860 0.147 Uiso 1 1 calc R U . . .
H5E3 H 0.6963 -0.3319 0.2088 0.147 Uiso 1 1 calc R U . . .
C6A C 0.3450(8) 0.7130(6) 0.1371(6) 0.061(2) Uani 1 1 d . . . . .
H6A H 0.3099 0.7843 0.1497 0.074 Uiso 1 1 calc R U . . .
C6B C 0.1585(7) -0.5581(7) 0.5669(9) 0.091(4) Uani 1 1 d . . . . .
H6B H 0.0802 -0.5965 0.5789 0.109 Uiso 1 1 calc R U . . .
C6C C -0.0317(6) 0.2792(6) 0.2622(6) 0.0475(17) Uani 1 1 d . . . . .
H6C H -0.0661 0.3384 0.2012 0.057 Uiso 1 1 calc R U . . .
C7A C 0.3909(8) 0.7181(6) 0.0380(5) 0.0520(19) Uani 1 1 d . . . . .
H7A H 0.3867 0.7926 -0.0169 0.062 Uiso 1 1 calc R U . . .
C7B C 0.2649(6) -0.6204(6) 0.5460(7) 0.054(2) Uani 1 1 d . . . . .
H7B H 0.2599 -0.7021 0.5469 0.065 Uiso 1 1 calc R U . . .
C7C C -0.1062(6) 0.1878(5) 0.3180(5) 0.0359(14) Uani 1 1 d . . . . .
H7C H -0.1917 0.1867 0.2963 0.043 Uiso 1 1 calc R U . . .
C8A C 0.4462(6) 0.6093(5) 0.0171(5) 0.0384(14) Uani 1 1 d . . . . .
C8B C 0.3845(5) -0.5621(5) 0.5226(5) 0.0293(12) Uani 1 1 d . . . . .
C8C C -0.0551(6) 0.0925(5) 0.4105(4) 0.0320(13) Uani 1 1 d . . . . .
N3D N 0.0786(6) -0.0424(7) 0.2274(6) 0.068(2) Uani 1 1 d . . . . .
N3E N 0.6562(6) -0.1573(6) 0.1198(5) 0.0564(17) Uani 1 1 d . . . . .
O1A O 0.3865(3) 0.2183(3) 0.1907(3) 0.0244(8) Uani 1 1 d . . . . .
O1B O 0.4912(4) -0.1678(3) 0.4136(3) 0.0237(8) Uani 1 1 d . . . . .
O1C O 0.3586(3) -0.0073(3) 0.5062(3) 0.0204(7) Uani 1 1 d . . . . .
O1D O 0.2768(4) -0.0178(3) 0.2921(3) 0.0308(9) Uani 1 1 d . . . . .
O1E O 0.5303(4) -0.0275(3) 0.1855(3) 0.0299(9) Uani 1 1 d . . . . .
O2A O 0.5966(4) 0.2149(3) 0.2163(3) 0.0278(8) Uani 1 1 d . . . . .
O2B O 0.5328(3) -0.2247(3) 0.5925(3) 0.0234(8) Uani 1 1 d . . . . .
O2C O 0.7133(3) -0.0204(3) 0.3439(3) 0.0273(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1B 2.335(3) . ?
Gd1 O1D 2.374(4) . ?
Gd1 O1E 2.412(3) . ?
Gd1 O1C 2.430(3) . ?
Gd1 O2B 2.445(3) 2_656 ?
Gd1 O1A 2.448(3) . ?
Gd1 O2A 2.473(3) . ?
Gd1 O2C 2.507(4) . ?
Gd1 O1C 2.546(3) 2_656 ?
Gd1 C1A 2.817(5) . ?
Gd1 C1C 2.893(5) 2_656 ?
Gd1 Gd1 4.0130(7) 2_656 ?
C1A O2A 1.254(6) . ?
C1A O1A 1.265(6) . ?
C1A C2A 1.459(7) . ?
C1B O2B 1.254(6) . ?
C1B O1B 1.257(6) . ?
C1B C2B 1.507(6) . ?
C1C O2C 1.249(6) 2_656 ?
C1C O1C 1.260(6) . ?
C1C C2C 1.482(7) . ?
C1C Gd1 2.893(5) 2_656 ?
C2A C3A 1.408(8) . ?
C2A C8A 1.415(8) 2_665 ?
C2B C3B 1.389(7) . ?
C2B C8B 1.394(7) 2_646 ?
C2C C8C 1.405(8) 2_556 ?
C2C C3C 1.403(8) . ?
C2D O1D 1.198(9) . ?
C2D N3D 1.357(9) . ?
C2E O1E 1.237(7) . ?
C2E N3E 1.307(8) . ?
C3A C4A 1.433(8) . ?
C3A C8A 1.445(8) . ?
C3B C4B 1.424(8) . ?
C3B C8B 1.434(7) . ?
C3C C8C 1.426(8) . ?
C3C C4C 1.437(8) . ?
C4A C5A 1.333(9) . ?
C4B C5B 1.333(9) . ?
C4C C5C 1.356(8) . ?
C4D N3D 1.408(11) . ?
C4E N3E 1.405(10) . ?
C5A C6A 1.419(9) . ?
C5B C6B 1.407(10) . ?
C5C C6C 1.407(9) . ?
C5D N3D 1.403(11) . ?
C5E N3E 1.465(10) . ?
C6A C7A 1.352(9) . ?
C6B C7B 1.351(9) . ?
C6C C7C 1.353(8) . ?
C7A C8A 1.435(8) . ?
C7B C8B 1.424(8) . ?
C7C C8C 1.436(8) . ?
C8A C2A 1.415(8) 2_665 ?
C8B C2B 1.394(7) 2_646 ?
C8C C2C 1.405(8) 2_556 ?
O1C Gd1 2.546(3) 2_656 ?
O2B Gd1 2.445(3) 2_656 ?
O2C C1C 1.249(6) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1B Gd1 O1D 75.71(13) . . ?
O1B Gd1 O1E 76.71(12) . . ?
O1D Gd1 O1E 76.90(13) . . ?
O1B Gd1 O1C 71.16(11) . . ?
O1D Gd1 O1C 75.10(12) . . ?
O1E Gd1 O1C 141.49(12) . . ?
O1B Gd1 O2B 136.13(11) . 2_656 ?
O1D Gd1 O2B 115.66(12) . 2_656 ?
O1E Gd1 O2B 145.64(12) . 2_656 ?
O1C Gd1 O2B 71.69(11) . 2_656 ?
O1B Gd1 O1A 145.14(12) . . ?
O1D Gd1 O1A 74.04(12) . . ?
O1E Gd1 O1A 79.91(12) . . ?
O1C Gd1 O1A 116.35(11) . . ?
O2B Gd1 O1A 73.97(11) 2_656 . ?
O1B Gd1 O2A 141.02(12) . . ?
O1D Gd1 O2A 123.55(13) . . ?
O1E Gd1 O2A 76.03(12) . . ?
O1C Gd1 O2A 142.19(12) . . ?
O2B Gd1 O2A 70.52(12) 2_656 . ?
O1A Gd1 O2A 53.03(12) . . ?
O1B Gd1 O2C 73.40(12) . . ?
O1D Gd1 O2C 138.53(12) . . ?
O1E Gd1 O2C 69.61(12) . . ?
O1C Gd1 O2C 118.73(11) . . ?
O2B Gd1 O2C 105.78(12) 2_656 . ?
O1A Gd1 O2C 121.38(12) . . ?
O2A Gd1 O2C 71.27(12) . . ?
O1B Gd1 O1C 75.56(11) . 2_656 ?
O1D Gd1 O1C 142.05(12) . 2_656 ?
O1E Gd1 O1C 119.28(12) . 2_656 ?
O1C Gd1 O1C 72.50(12) . 2_656 ?
O2B Gd1 O1C 71.70(11) 2_656 2_656 ?
O1A Gd1 O1C 139.09(11) . 2_656 ?
O2A Gd1 O1C 94.31(11) . 2_656 ?
O2C Gd1 O1C 51.04(11) . 2_656 ?
O1B Gd1 C1A 153.99(13) . . ?
O1D Gd1 C1A 99.30(15) . . ?
O1E Gd1 C1A 77.30(13) . . ?
O1C Gd1 C1A 133.00(13) . . ?
O2B Gd1 C1A 69.31(13) 2_656 . ?
O1A Gd1 C1A 26.64(14) . . ?
O2A Gd1 C1A 26.42(13) . . ?
O2C Gd1 C1A 96.54(14) . . ?
O1C Gd1 C1A 117.18(13) 2_656 . ?
O1B Gd1 C1C 75.24(13) . 2_656 ?
O1D Gd1 C1C 150.91(13) . 2_656 ?
O1E Gd1 C1C 94.88(14) . 2_656 ?
O1C Gd1 C1C 96.88(13) . 2_656 ?
O2B Gd1 C1C 86.93(13) 2_656 2_656 ?
O1A Gd1 C1C 132.64(13) . 2_656 ?
O2A Gd1 C1C 79.89(13) . 2_656 ?
O2C Gd1 C1C 25.49(12) . 2_656 ?
O1C Gd1 C1C 25.79(12) 2_656 2_656 ?
C1A Gd1 C1C 106.10(15) . 2_656 ?
O1B Gd1 Gd1 69.28(8) . 2_656 ?
O1D Gd1 Gd1 110.15(9) . 2_656 ?
O1E Gd1 Gd1 141.63(9) . 2_656 ?
O1C Gd1 Gd1 37.23(8) . 2_656 ?
O2B Gd1 Gd1 67.08(8) 2_656 2_656 ?
O1A Gd1 Gd1 138.43(8) . 2_656 ?
O2A Gd1 Gd1 121.74(9) . 2_656 ?
O2C Gd1 Gd1 83.81(8) . 2_656 ?
O1C Gd1 Gd1 35.27(7) 2_656 2_656 ?
C1A Gd1 Gd1 134.64(10) . 2_656 ?
C1C Gd1 Gd1 60.09(10) 2_656 2_656 ?
O2A C1A O1A 121.4(5) . . ?
O2A C1A C2A 120.1(5) . . ?
O1A C1A C2A 118.5(5) . . ?
O2A C1A Gd1 61.3(3) . . ?
O1A C1A Gd1 60.2(3) . . ?
C2A C1A Gd1 175.9(4) . . ?
O2B C1B O1B 126.6(4) . . ?
O2B C1B C2B 118.1(4) . . ?
O1B C1B C2B 115.3(4) . . ?
O2C C1C O1C 120.4(5) 2_656 . ?
O2C C1C C2C 117.6(4) 2_656 . ?
O1C C1C C2C 121.7(5) . . ?
O2C C1C Gd1 59.7(3) 2_656 2_656 ?
O1C C1C Gd1 61.5(3) . 2_656 ?
C2C C1C Gd1 165.0(4) . 2_656 ?
C3A C2A C8A 119.2(5) . 2_665 ?
C3A C2A C1A 121.2(5) . . ?
C8A C2A C1A 119.6(5) 2_665 . ?
C3B C2B C8B 120.9(5) . 2_646 ?
C3B C2B C1B 119.7(4) . . ?
C8B C2B C1B 119.3(5) 2_646 . ?
C8C C2C C3C 120.7(5) 2_556 . ?
C8C C2C C1C 119.8(5) 2_556 . ?
C3C C2C C1C 119.5(5) . . ?
O1D C2D N3D 125.9(8) . . ?
O1E C2E N3E 126.3(7) . . ?
C2A C3A C4A 122.5(5) . . ?
C2A C3A C8A 120.2(5) . . ?
C4A C3A C8A 117.3(5) . . ?
C2B C3B C4B 122.2(5) . . ?
C2B C3B C8B 119.4(5) . . ?
C4B C3B C8B 118.4(5) . . ?
C2C C3C C8C 119.5(5) . . ?
C2C C3C C4C 122.1(5) . . ?
C8C C3C C4C 118.4(5) . . ?
C5A C4A C3A 122.1(6) . . ?
C5B C4B C3B 121.3(6) . . ?
C5C C4C C3C 121.4(6) . . ?
C4A C5A C6A 120.5(6) . . ?
C4B C5B C6B 120.6(6) . . ?
C4C C5C C6C 119.8(6) . . ?
C7A C6A C5A 120.9(6) . . ?
C7B C6B C5B 120.9(6) . . ?
C7C C6C C5C 121.4(6) . . ?
C6A C7A C8A 120.4(6) . . ?
C6B C7B C8B 120.7(6) . . ?
C6C C7C C8C 120.9(6) . . ?
C2A C8A C7A 120.8(5) 2_665 . ?
C2A C8A C3A 120.4(5) 2_665 . ?
C7A C8A C3A 118.7(6) . . ?
C2B C8B C7B 122.3(5) 2_646 . ?
C2B C8B C3B 119.7(5) 2_646 . ?
C7B C8B C3B 118.0(5) . . ?
C2C C8C C3C 119.8(5) 2_556 . ?
C2C C8C C7C 122.1(6) 2_556 . ?
C3C C8C C7C 118.1(5) . . ?
C2D N3D C4D 119.2(8) . . ?
C2D N3D C5D 121.2(8) . . ?
C4D N3D C5D 119.5(7) . . ?
C2E N3E C4E 121.8(7) . . ?
C2E N3E C5E 121.6(7) . . ?
C4E N3E C5E 116.6(7) . . ?
C1A O1A Gd1 93.2(3) . . ?
C1B O1B Gd1 138.9(3) . . ?
C1C O1C Gd1 152.0(3) . . ?
C1C O1C Gd1 92.7(3) . 2_656 ?
Gd1 O1C Gd1 107.50(12) . 2_656 ?
C2D O1D Gd1 140.5(4) . . ?
C2E O1E Gd1 124.1(4) . . ?
C1A O2A Gd1 92.3(3) . . ?
C1B O2B Gd1 137.2(3) . 2_656 ?
C1C O2C Gd1 94.8(3) 2_656 . ?

_refine_diff_density_max         1.997
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.154

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 0.000 0.500 1.000 218 37 ' '
_platon_squeeze_details          
;
;

# start Validation Reply Form
_vrf_CHEMW03_Comp3_Gd            
;
PROBLEM: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
RESPONSE: The crystal structure contains a percentage of voids occupied by
disordered solvent molecules. We have used SQUEZZE routine to eliminate
one DMF molecule.
;
# end Validation Reply Form

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_Comp4_Tb
_database_code_depnum_ccdc_archive 'CCDC 1421045'
_audit_update_record             
;
2015-11-10 deposited with the CCDC.
2015-11-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H33 N3 O9 Tb'
_chemical_formula_weight         774.54

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.468(5)
_cell_length_b                   11.356(5)
_cell_length_c                   13.089(6)
_cell_angle_alpha                107.539(5)
_cell_angle_beta                 90.086(6)
_cell_angle_gamma                92.356(6)
_cell_volume                     1482.1(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1474
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      18.45

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_F_000             778
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    2.449
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'

_exptl_special_details           
;
Crystal structure have some disorder problems. The crystal structure contains a percentage of voids occupied by disordered solvent molecules. We have used SQUEEZE routine to eliminate one crystallization DMF molecule.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16407
_diffrn_reflns_av_unetI/netI     0.1336
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.632
_diffrn_reflns_theta_max         28.540
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6811
_reflns_number_gt                4580
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker ApexII'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        'Bruker Apex II'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ViewerLite 5.0 (Acccelrys)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0470P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6811
_refine_ls_number_parameters     374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_ref         0.1229
_refine_ls_wR_factor_gt          0.1121
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_restrained_S_all      0.911
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.48066(3) 0.45339(3) 0.33946(3) 0.02733(11) Uani 1 1 d . . . . .
C1A C 0.4989(8) 0.2333(6) 0.1704(5) 0.0369(18) Uani 1 1 d . . . . .
C1B C 0.5084(6) 0.7456(6) 0.5064(6) 0.0311(16) Uani 1 1 d . . . . .
C1C C 0.2671(7) 0.4913(6) 0.5606(6) 0.0330(16) Uani 1 1 d . . . . .
C2A C 0.5007(8) 0.1154(7) 0.0868(6) 0.044(2) Uani 1 1 d . . . . .
C2B C 0.5062(7) 0.8801(6) 0.5067(6) 0.0322(16) Uani 1 1 d . . . . .
C2C C 0.1295(6) 0.4962(7) 0.5281(6) 0.0351(17) Uani 1 1 d . . . . .
C2D C 0.5839(9) 0.6280(10) 0.1983(7) 0.064(3) Uani 1 1 d . . . . .
H2D H 0.5697 0.6903 0.2617 0.077 Uiso 1 1 calc R U . . .
C2E C 0.1916(12) 0.4844(11) 0.2373(9) 0.083(3) Uani 1 1 d . . . . .
H2E H 0.1922 0.4047 0.1900 0.099 Uiso 1 1 calc R U . . .
C3A C 0.4520(9) 0.0055(8) 0.1017(7) 0.062(2) Uani 1 1 d . . . . .
C3B C 0.3914(7) 0.9398(6) 0.5256(6) 0.0377(18) Uani 1 1 d . . . . .
C3C C 0.0768(7) 0.4028(7) 0.4412(6) 0.0371(17) Uani 1 1 d . . . . .
C4A C 0.4032(10) 0.0007(9) 0.2057(7) 0.073(3) Uani 1 1 d . . . . .
H4A H 0.4104 0.0716 0.2643 0.088 Uiso 1 1 calc R U . . .
C4B C 0.2763(8) 0.8845(8) 0.5527(8) 0.063(3) Uani 1 1 d . . . . .
H4B H 0.2784 0.8054 0.5596 0.076 Uiso 1 1 calc R U . . .
C4C C 0.1483(7) 0.3031(7) 0.3811(7) 0.050(2) Uani 1 1 d . . . . .
H4C H 0.2334 0.2990 0.4000 0.060 Uiso 1 1 calc R U . . .
C4D C 0.6800(11) 0.5674(12) 0.0258(9) 0.106(4) Uani 1 1 d . . . . .
H4D1 H 0.6634 0.4867 0.0332 0.158 Uiso 1 1 d R U . . .
H4D2 H 0.7676 0.5755 0.0062 0.158 Uiso 1 1 d R U . . .
H4D3 H 0.6248 0.5785 -0.0290 0.158 Uiso 1 1 d R U . . .
C4E C 0.0692(14) 0.6627(14) 0.3046(11) 0.130(5) Uani 1 1 d . . . . .
H4E1 H 0.1373 0.6844 0.3570 0.196 Uiso 1 1 d R U . . .
H4E2 H -0.0110 0.6616 0.3399 0.196 Uiso 1 1 d R U . . .
H4E3 H 0.0682 0.7224 0.2660 0.196 Uiso 1 1 d R U . . .
C5A C 0.3490(13) -0.1020(10) 0.2188(9) 0.107(5) Uani 1 1 d . . . . .
H5A H 0.3145 -0.0996 0.2848 0.128 Uiso 1 1 calc R U . . .
C5B C 0.1658(9) 0.9419(10) 0.5686(10) 0.094(4) Uani 1 1 d . . . . .
H5B H 0.0918 0.9014 0.5824 0.113 Uiso 1 1 calc R U . . .
C5C C 0.0956(8) 0.2130(8) 0.2963(7) 0.064(3) Uani 1 1 d . . . . .
H5C H 0.1442 0.1479 0.2581 0.077 Uiso 1 1 calc R U . . .
C5D C 0.7073(12) 0.7837(12) 0.1400(11) 0.126(6) Uani 1 1 d . . . . .
H5D1 H 0.6592 0.8413 0.1933 0.190 Uiso 1 1 d R U . . .
H5D2 H 0.7015 0.8024 0.0733 0.190 Uiso 1 1 d R U . . .
H5D3 H 0.7953 0.7900 0.1626 0.190 Uiso 1 1 d R U . . .
C5E C -0.0111(14) 0.4946(15) 0.1592(11) 0.144(6) Uani 1 1 d . . . . .
H5E1 H -0.0019 0.5246 0.0983 0.216 Uiso 1 1 d R U . . .
H5E2 H -0.0923 0.5171 0.1917 0.216 Uiso 1 1 d R U . . .
H5E3 H -0.0065 0.4063 0.1365 0.216 Uiso 1 1 d R U . . .
C6A C 0.3427(13) -0.2154(10) 0.1336(9) 0.108(5) Uani 1 1 d . . . . .
H6A H 0.3063 -0.2868 0.1443 0.129 Uiso 1 1 calc R U . . .
C6B C 0.1621(9) 1.0634(10) 0.5644(10) 0.096(4) Uani 1 1 d . . . . .
H6B H 0.0855 1.1037 0.5772 0.115 Uiso 1 1 calc R U . . .
C6C C -0.0330(8) 0.2184(8) 0.2666(7) 0.061(3) Uani 1 1 d . . . . .
H6C H -0.0682 0.1575 0.2076 0.073 Uiso 1 1 calc R U . . .
C7A C 0.3914(10) -0.2178(9) 0.0352(8) 0.080(3) Uani 1 1 d . . . . .
H7A H 0.3875 -0.2922 -0.0199 0.096 Uiso 1 1 calc R U . . .
C7B C 0.2671(8) 1.1231(8) 0.5423(7) 0.060(3) Uani 1 1 d . . . . .
H7B H 0.2620 1.2042 0.5408 0.072 Uiso 1 1 calc R U . . .
C7C C -0.1058(7) 0.3111(8) 0.3226(6) 0.049(2) Uani 1 1 d . . . . .
H7C H -0.1911 0.3119 0.3028 0.058 Uiso 1 1 calc R U . . .
C8A C 0.4477(9) -0.1101(8) 0.0142(7) 0.062(3) Uani 1 1 d . . . . .
C8B C 0.3858(7) 1.0642(6) 0.5211(6) 0.0351(17) Uani 1 1 d . . . . .
C8C C -0.0536(7) 0.4079(7) 0.4121(6) 0.0386(18) Uani 1 1 d . . . . .
N3D N 0.6563(8) 0.6599(8) 0.1258(7) 0.077(3) Uani 1 1 d . . . . .
N3E N 0.0878(8) 0.5477(11) 0.2346(9) 0.088(3) Uani 1 1 d . . . . .
O1A O 0.3911(5) 0.2814(4) 0.1952(4) 0.0414(13) Uani 1 1 d . . . . .
O1B O 0.4931(5) 0.6670(4) 0.4158(4) 0.0342(11) Uani 1 1 d . . . . .
O1C O 0.3570(4) 0.5052(4) 0.5018(4) 0.0375(12) Uani 1 1 d . . . . .
O1D O 0.5349(5) 0.5271(5) 0.1906(4) 0.0505(15) Uani 1 1 d . . . . .
O1E O 0.2828(6) 0.5186(6) 0.2930(5) 0.0574(17) Uani 1 1 d . . . . .
O2A O 0.5982(5) 0.2828(5) 0.2172(4) 0.0479(14) Uani 1 1 d . . . . .
O2B O 0.5274(5) 0.7244(4) 0.5925(4) 0.0382(12) Uani 1 1 d . . . . .
O2C O 0.7115(5) 0.5169(5) 0.3480(4) 0.0444(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 O1B 2.326(4) . ?
Tb1 O1E 2.367(6) . ?
Tb1 O1D 2.401(5) . ?
Tb1 O1C 2.420(5) . ?
Tb1 O1A 2.425(5) . ?
Tb1 O2B 2.438(5) 2_666 ?
Tb1 O2A 2.482(5) . ?
Tb1 O2C 2.486(5) . ?
Tb1 O1C 2.600(5) 2_666 ?
Tb1 C1A 2.808(7) . ?
Tb1 C1C 2.905(7) 2_666 ?
C1A O2A 1.230(8) . ?
C1A O1A 1.273(8) . ?
C1A C2A 1.452(9) . ?
C1B O2B 1.240(8) . ?
C1B O1B 1.257(7) . ?
C1B C2B 1.527(9) . ?
C1C O2C 1.249(8) 2_666 ?
C1C O1C 1.252(8) . ?
C1C C2C 1.509(9) . ?
C1C Tb1 2.905(7) 2_666 ?
C2A C3A 1.396(11) . ?
C2A C8A 1.415(11) 2_655 ?
C2B C8B 1.376(9) 2_676 ?
C2B C3B 1.390(10) . ?
C2C C3C 1.395(10) . ?
C2C C8C 1.411(10) 2_566 ?
C2D O1D 1.212(10) . ?
C2D N3D 1.338(10) . ?
C2E O1E 1.179(12) . ?
C2E N3E 1.333(12) . ?
C3A C8A 1.458(12) . ?
C3A C4A 1.471(12) . ?
C3B C4B 1.431(10) . ?
C3B C8B 1.435(9) . ?
C3C C4C 1.413(10) . ?
C3C C8C 1.424(10) . ?
C4A C5A 1.334(13) . ?
C4B C5B 1.337(12) . ?
C4C C5C 1.361(11) . ?
C4D N3D 1.440(13) . ?
C4E N3E 1.372(15) . ?
C5A C6A 1.426(14) . ?
C5B C6B 1.400(12) . ?
C5C C6C 1.409(11) . ?
C5D N3D 1.442(13) . ?
C5E N3E 1.413(15) . ?
C6A C7A 1.379(13) . ?
C6B C7B 1.345(12) . ?
C6C C7C 1.353(11) . ?
C7A C8A 1.436(12) . ?
C7B C8B 1.423(10) . ?
C7C C8C 1.432(10) . ?
C8A C2A 1.415(11) 2_655 ?
C8B C2B 1.376(9) 2_676 ?
C8C C2C 1.411(10) 2_566 ?
O1C Tb1 2.600(5) 2_666 ?
O2B Tb1 2.438(5) 2_666 ?
O2C C1C 1.249(8) 2_666 ?

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
O1B Tb1 O1E 75.84(19) . . ?
O1B Tb1 O1D 76.87(17) . . ?
O1E Tb1 O1D 77.1(2) . . ?
O1B Tb1 O1C 71.57(16) . . ?
O1E Tb1 O1C 74.28(18) . . ?
O1D Tb1 O1C 141.51(18) . . ?
O1B Tb1 O1A 145.92(17) . . ?
O1E Tb1 O1A 74.20(19) . . ?
O1D Tb1 O1A 80.94(18) . . ?
O1C Tb1 O1A 114.62(17) . . ?
O1B Tb1 O2B 135.46(15) . 2_666 ?
O1E Tb1 O2B 116.73(18) . 2_666 ?
O1D Tb1 O2B 145.65(17) . 2_666 ?
O1C Tb1 O2B 71.78(16) . 2_666 ?
O1A Tb1 O2B 73.95(16) . 2_666 ?
O1B Tb1 O2A 141.18(17) . . ?
O1E Tb1 O2A 123.15(19) . . ?
O1D Tb1 O2A 75.73(19) . . ?
O1C Tb1 O2A 142.25(17) . . ?
O1A Tb1 O2A 52.87(17) . . ?
O2B Tb1 O2A 70.49(17) 2_666 . ?
O1B Tb1 O2C 73.65(17) . . ?
O1E Tb1 O2C 139.00(19) . . ?
O1D Tb1 O2C 69.81(18) . . ?
O1C Tb1 O2C 119.65(16) . . ?
O1A Tb1 O2C 121.84(17) . . ?
O2B Tb1 O2C 104.22(17) 2_666 . ?
O2A Tb1 O2C 71.37(17) . . ?
O1B Tb1 O1C 74.65(16) . 2_666 ?
O1E Tb1 O1C 141.51(18) . 2_666 ?
O1D Tb1 O1C 118.76(17) . 2_666 ?
O1C Tb1 O1C 73.32(17) . 2_666 ?
O1A Tb1 O1C 139.31(16) . 2_666 ?
O2B Tb1 O1C 71.28(15) 2_666 2_666 ?
O2A Tb1 O1C 95.28(16) . 2_666 ?
O2C Tb1 O1C 50.58(15) . 2_666 ?
O1B Tb1 C1A 154.25(19) . . ?
O1E Tb1 C1A 99.4(2) . . ?
O1D Tb1 C1A 77.4(2) . . ?
O1C Tb1 C1A 132.26(19) . . ?
O1A Tb1 C1A 26.91(19) . . ?
O2B Tb1 C1A 69.56(19) 2_666 . ?
O2A Tb1 C1A 25.96(18) . . ?
O2C Tb1 C1A 96.4(2) . . ?
O1C Tb1 C1A 117.7(2) 2_666 . ?
O1B Tb1 C1C 74.93(18) . 2_666 ?
O1E Tb1 C1C 150.7(2) . 2_666 ?
O1D Tb1 C1C 94.8(2) . 2_666 ?
O1C Tb1 C1C 97.67(19) . 2_666 ?
O1A Tb1 C1C 132.96(18) . 2_666 ?
O2B Tb1 C1C 85.81(18) 2_666 2_666 ?
O2A Tb1 C1C 80.53(19) . 2_666 ?
O2C Tb1 C1C 25.29(17) . 2_666 ?
O1C Tb1 C1C 25.52(16) 2_666 2_666 ?
C1A Tb1 C1C 106.2(2) . 2_666 ?
O2A C1A O1A 121.6(6) . . ?
O2A C1A C2A 120.7(7) . . ?
O1A C1A C2A 117.7(7) . . ?
O2A C1A Tb1 62.1(4) . . ?
O1A C1A Tb1 59.5(3) . . ?
C2A C1A Tb1 175.6(6) . . ?
O2B C1B O1B 126.7(6) . . ?
O2B C1B C2B 118.4(6) . . ?
O1B C1B C2B 114.9(6) . . ?
O2C C1C O1C 120.9(7) 2_666 . ?
O2C C1C C2C 117.6(6) 2_666 . ?
O1C C1C C2C 121.3(7) . . ?
O2C C1C Tb1 58.2(4) 2_666 2_666 ?
O1C C1C Tb1 63.5(4) . 2_666 ?
C2C C1C Tb1 164.8(5) . 2_666 ?
C3A C2A C8A 117.9(7) . 2_655 ?
C3A C2A C1A 122.4(7) . . ?
C8A C2A C1A 119.6(7) 2_655 . ?
C8B C2B C3B 121.3(6) 2_676 . ?
C8B C2B C1B 119.5(6) 2_676 . ?
C3B C2B C1B 118.9(6) . . ?
C3C C2C C8C 120.3(7) . 2_566 ?
C3C C2C C1C 119.6(6) . . ?
C8C C2C C1C 120.1(6) 2_566 . ?
O1D C2D N3D 127.2(10) . . ?
O1E C2E N3E 127.0(12) . . ?
C2A C3A C8A 121.2(8) . . ?
C2A C3A C4A 121.8(8) . . ?
C8A C3A C4A 117.0(8) . . ?
C2B C3B C4B 123.1(7) . . ?
C2B C3B C8B 119.8(7) . . ?
C4B C3B C8B 117.0(7) . . ?
C2C C3C C4C 122.2(7) . . ?
C2C C3C C8C 119.0(7) . . ?
C4C C3C C8C 118.9(7) . . ?
C5A C4A C3A 122.1(9) . . ?
C5B C4B C3B 122.6(8) . . ?
C5C C4C C3C 121.4(8) . . ?
C4A C5A C6A 121.4(10) . . ?
C4B C5B C6B 119.6(9) . . ?
C4C C5C C6C 119.9(8) . . ?
C7A C6A C5A 119.1(10) . . ?
C7B C6B C5B 121.4(9) . . ?
C7C C6C C5C 120.8(8) . . ?
C6A C7A C8A 122.7(9) . . ?
C6B C7B C8B 121.0(8) . . ?
C6C C7C C8C 120.9(7) . . ?
C2A C8A C7A 121.6(8) 2_655 . ?
C2A C8A C3A 120.8(8) 2_655 . ?
C7A C8A C3A 117.6(9) . . ?
C2B C8B C7B 122.8(7) 2_676 . ?
C2B C8B C3B 118.8(6) 2_676 . ?
C7B C8B C3B 118.4(7) . . ?
C2C C8C C3C 120.7(7) 2_566 . ?
C2C C8C C7C 121.2(7) 2_566 . ?
C3C C8C C7C 118.1(7) . . ?
C2D N3D C4D 118.7(9) . . ?
C2D N3D C5D 123.6(10) . . ?
C4D N3D C5D 117.6(9) . . ?
C2E N3E C4E 123.1(12) . . ?
C2E N3E C5E 119.8(13) . . ?
C4E N3E C5E 117.1(10) . . ?
C1A O1A Tb1 93.6(4) . . ?
C1B O1B Tb1 139.3(4) . . ?
C1C O1C Tb1 155.0(5) . . ?
C1C O1C Tb1 91.0(4) . 2_666 ?
Tb1 O1C Tb1 106.68(17) . 2_666 ?
C2D O1D Tb1 124.7(6) . . ?
C2E O1E Tb1 142.6(7) . . ?
C1A O2A Tb1 92.0(4) . . ?
C1B O2B Tb1 137.8(4) . 2_666 ?
C1C O2C Tb1 96.5(4) 2_666 . ?

_refine_diff_density_max         1.630
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.167

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 0.000 0.000 0.000 277 37 ' '
_platon_squeeze_details          
;
;
# start Validation Reply Form
_vrf_CHEMW03_Comp4_Tb            
;
PROBLEM: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
RESPONSE: The crystal structure contains a percentage of voids occupied by
disordered solvent molecules. We have used SQUEZZE routine to eliminate
one DMF molecule.
;
# end Validation Reply Form



_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_Comp7_Yb
_database_code_depnum_ccdc_archive 'CCDC 1421046'
_audit_update_record             
;
2015-11-10 deposited with the CCDC.
2015-11-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C69 H73 N10 O28 Yb3'
_chemical_formula_weight         2009.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.5512(16)
_cell_length_b                   13.6376(16)
_cell_length_c                   21.667(2)
_cell_angle_alpha                106.851(4)
_cell_angle_beta                 97.131(4)
_cell_angle_gamma                91.457(4)
_cell_volume                     3794.7(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    100353
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      28.75

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_F_000             1982
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    3.755
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'

_exptl_special_details           
;
Crystal structure have some disorder problems. The crystal structure contains a percentage of voids occupied by disordered solvent molecules. We have used SQUEEZE routine to eliminate one crystallization DMF molecule.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            173864
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.326
_diffrn_reflns_theta_max         28.862
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             19714
_reflns_number_gt                17080
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker ApexII'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        'Bruker Apex II'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ViewerLite 5.0 (Acccelrys)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0156P)²+78.6054P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         19714
_refine_ls_number_parameters     1029
_refine_ls_number_restraints     138
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1294
_refine_ls_wR_factor_gt          0.1250
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.29797(2) 0.25302(2) 0.59196(2) 0.01623(6) Uani 1 1 d . U . . .
Yb2 Yb 0.03812(2) 0.39917(2) 0.73220(2) 0.02143(7) Uani 1 1 d . . . . .
Yb3 Yb 0.64170(2) -0.06593(2) 0.93952(2) 0.01854(7) Uani 1 1 d . . . . .
C1A C 0.2327(5) 0.2582(4) 0.7401(3) 0.0133(11) Uani 1 1 d . . . . .
C1B C 0.3139(5) 0.2256(5) 0.4636(3) 0.0194(12) Uani 1 1 d . . . . .
C1C C 0.0186(7) 0.4435(6) 0.8616(5) 0.037(2) Uani 1 1 d . . . . .
C2A C 0.4372(5) 0.0521(6) 0.9156(3) 0.0266(15) Uani 1 1 d . . . . .
C2B C 0.6725(5) -0.1135(5) 0.8138(3) 0.0208(13) Uani 1 1 d . . . . .
C2C C 0.0948(5) 0.3808(5) 0.5807(3) 0.0174(12) Uani 1 1 d . . . . .
C2D C 0.5306(8) 0.2271(8) 0.5883(5) 0.053(3) Uani 1 1 d . . . . .
H2D H 0.5384 0.2953 0.5888 0.063 Uiso 1 1 calc R U . . .
C2F C -0.1542(7) 0.4629(8) 0.6506(6) 0.049(2) Uani 1 1 d . . . . .
H2F H -0.1223 0.4327 0.6149 0.058 Uiso 1 1 calc R U . . .
C2G C 0.7157(13) 0.1714(10) 1.0294(7) 0.086(3) Uani 1 1 d . U . . .
H2G H 0.6896 0.1633 1.0655 0.103 Uiso 1 1 calc R U . . .
C2Z C 0.4079(7) 0.4700(8) 0.6914(5) 0.0488(15) Uani 1 1 d . U . . .
H2Z H 0.4067 0.4515 0.7293 0.059 Uiso 1 1 calc R U . . .
C3A C 0.2842(4) 0.2061(4) 0.7866(3) 0.0113(10) Uani 1 1 d . . . . .
C3B C 0.3175(5) 0.2010(5) 0.3920(3) 0.0186(12) Uani 1 1 d . . . . .
C3C C 0.0090(7) 0.4711(6) 0.9332(4) 0.039(2) Uani 1 1 d . . . . .
C4A C 0.2564(4) 0.1031(4) 0.7798(3) 0.0103(10) Uani 1 1 d . . . . .
C4B C 0.2328(5) 0.2105(5) 0.3504(3) 0.0188(12) Uani 1 1 d . . . . .
C4C C 0.0911(7) 0.4624(6) 0.9776(5) 0.040(2) Uani 1 1 d . . . . .
C4D C 0.6183(15) 0.0650(9) 0.5699(9) 0.104(6) Uani 1 1 d . . . . .
H4DA H 0.6553 0.0535 0.6077 0.156 Uiso 1 1 d R U . . .
H4DB H 0.6522 0.0375 0.5328 0.156 Uiso 1 1 d R U . . .
H4DC H 0.5528 0.0312 0.5621 0.156 Uiso 1 1 d R U . . .
C4F C -0.2900(8) 0.5532(9) 0.6981(8) 0.076(4) Uani 1 1 d . . . . .
H4FA H -0.2444 0.5655 0.7378 0.114 Uiso 1 1 d R U . . .
H4FB H -0.3460 0.5093 0.6995 0.114 Uiso 1 1 d R U . . .
H4FC H -0.3131 0.6175 0.6943 0.114 Uiso 1 1 d R U . . .
C4G C 0.7812(16) 0.2900(11) 0.9809(8) 0.111(3) Uani 1 1 d . U . . .
H4GA H 0.7583 0.2405 0.9388 0.167 Uiso 1 1 d R U . . .
H4GB H 0.8534 0.2969 0.9857 0.167 Uiso 1 1 d R U . . .
H4GC H 0.7550 0.3559 0.9807 0.167 Uiso 1 1 d R U . . .
C4Z C 0.4504(9) 0.5964(9) 0.6371(5) 0.061(2) Uani 1 1 d . U . . .
H4ZA H 0.5196 0.6115 0.6352 0.091 Uiso 1 1 d R U . . .
H4ZB H 0.4145 0.6572 0.6393 0.091 Uiso 1 1 d R U . . .
H4ZC H 0.4233 0.5429 0.5983 0.091 Uiso 1 1 d R U . . .
C5A C 0.1786(5) 0.0460(5) 0.7306(3) 0.0166(11) Uani 1 1 d . . . . .
H5A H 0.1445 0.0767 0.7020 0.020 Uiso 1 1 calc R U . . .
C5B C 0.1439(5) 0.2522(5) 0.3746(4) 0.0245(14) Uani 1 1 d . . . . .
H5B H 0.1409 0.2714 0.4191 0.029 Uiso 1 1 calc R U . . .
C5C C 0.1840(7) 0.4219(7) 0.9581(4) 0.041(2) Uani 1 1 d . . . . .
H5C H 0.1908 0.4023 0.9141 0.049 Uiso 1 1 calc R U . . .
C5D C 0.7013(11) 0.2296(12) 0.5814(10) 0.116(8) Uani 1 1 d . . . . .
H5DA H 0.6911 0.3014 0.5982 0.174 Uiso 1 1 d R U . . .
H5DB H 0.7188 0.2159 0.5382 0.174 Uiso 1 1 d R U . . .
H5DC H 0.7548 0.2119 0.6091 0.174 Uiso 1 1 d R U . . .
C5F C -0.2827(8) 0.5020(8) 0.5753(7) 0.063(3) Uani 1 1 d . . . . .
H5FA H -0.2375 0.4734 0.5449 0.094 Uiso 1 1 d R U . . .
H5FB H -0.2953 0.5706 0.5742 0.094 Uiso 1 1 d R U . . .
H5FC H -0.3443 0.4603 0.5633 0.094 Uiso 1 1 d R U . . .
C5G C 0.7193(16) 0.3577(11) 1.0830(8) 0.115(4) Uani 1 1 d . U . . .
H5GA H 0.6541 0.3456 1.0941 0.173 Uiso 1 1 d R U . . .
H5GB H 0.7165 0.4118 1.0622 0.173 Uiso 1 1 d R U . . .
H5GC H 0.7661 0.3802 1.1227 0.173 Uiso 1 1 d R U . . .
C5Z C 0.4578(12) 0.6501(10) 0.7541(6) 0.082(3) Uani 1 1 d . U . . .
H5ZA H 0.3979 0.6866 0.7688 0.123 Uiso 1 1 d R U . . .
H5ZB H 0.5085 0.7080 0.7551 0.123 Uiso 1 1 d R U . . .
H5ZC H 0.4850 0.6226 0.7899 0.123 Uiso 1 1 d R U . . .
C6A C 0.1550(6) -0.0541(5) 0.7262(3) 0.0275(15) Uani 1 1 d . . . . .
H6A H 0.1037 -0.0906 0.6947 0.033 Uiso 1 1 calc R U . . .
C6B C 0.0643(6) 0.2639(6) 0.3331(4) 0.0297(16) Uani 1 1 d . . . . .
H6B H 0.0083 0.2934 0.3496 0.036 Uiso 1 1 calc R U . . .
C6C C 0.2624(8) 0.4113(8) 1.0020(5) 0.048(2) Uani 1 1 d . . . . .
H6C H 0.3213 0.3859 0.9879 0.057 Uiso 1 1 calc R U . . .
C7B C 0.0661(6) 0.2320(6) 0.2659(4) 0.0343(17) Uani 1 1 d . . . . .
H7B H 0.0106 0.2393 0.2381 0.041 Uiso 1 1 calc R U . . .
C7C C 0.2011(5) 0.6904(6) 0.6033(3) 0.0253(14) Uani 1 1 d . . . . .
H7C H 0.2545 0.7205 0.6351 0.030 Uiso 1 1 calc R U . . .
C7AA C 0.2070(7) -0.1037(5) 0.7686(4) 0.0312(17) Uani 1 1 d . . . . .
H7AA H 0.1903 -0.1723 0.7638 0.037 Uiso 1 1 calc R U . . .
C8A C 0.2793(6) -0.0526(5) 0.8150(3) 0.0249(15) Uani 1 1 d . . . . .
H8A H 0.3122 -0.0858 0.8427 0.030 Uiso 1 1 calc R U . . .
C8B C 0.1486(6) 0.1900(6) 0.2405(4) 0.0284(15) Uani 1 1 d . . . . .
H8B H 0.1481 0.1684 0.1956 0.034 Uiso 1 1 calc R U . . .
C8C C 0.1697(5) 0.5900(6) 0.5939(3) 0.0228(14) Uani 1 1 d . . . . .
H8C H 0.2036 0.5523 0.6183 0.027 Uiso 1 1 calc R U . . .
C9A C 0.3070(4) 0.0529(4) 0.8230(3) 0.0130(11) Uani 1 1 d . . . . .
C9B C 0.2353(5) 0.1792(5) 0.2824(3) 0.0207(13) Uani 1 1 d . . . . .
C9C C 0.0852(4) 0.5424(5) 0.5469(3) 0.0171(12) Uani 1 1 d . . . . .
C10A C 0.3837(5) 0.1064(5) 0.8704(3) 0.0167(12) Uani 1 1 d . . . . .
C10B C 0.3230(5) 0.1412(5) 0.2582(3) 0.0188(12) Uani 1 1 d . . . . .
C10C C 0.0461(4) 0.4410(5) 0.5380(3) 0.0156(11) Uani 1 1 d . . . . .
C11A C 0.4121(5) 0.2086(5) 0.8773(3) 0.0194(12) Uani 1 1 d . . . . .
C11B C 0.4088(5) 0.1339(5) 0.3001(3) 0.0193(12) Uani 1 1 d . . . . .
C11C C -0.0377(4) 0.3971(5) 0.4917(3) 0.0168(12) Uani 1 1 d . . . . .
C12A C 0.4913(6) 0.2635(7) 0.9247(4) 0.036(2) Uani 1 1 d . . . . .
H12A H 0.5278 0.2302 0.9510 0.043 Uiso 1 1 calc R U . . .
C12B C 0.4983(5) 0.0939(6) 0.2765(3) 0.0230(13) Uani 1 1 d . . . . .
H12B H 0.5013 0.0730 0.2319 0.028 Uiso 1 1 calc R U . . .
C12C C -0.0752(5) 0.2936(5) 0.4809(3) 0.0198(12) Uani 1 1 d . . . . .
H12C H -0.0454 0.2548 0.5061 0.024 Uiso 1 1 calc R U . . .
C13A C 0.5145(8) 0.3642(8) 0.9322(4) 0.050(3) Uani 1 1 d . . . . .
H13A H 0.5664 0.3993 0.9638 0.060 Uiso 1 1 calc R U . . .
C13B C 0.5797(5) 0.0860(6) 0.3190(4) 0.0261(15) Uani 1 1 d . . . . .
H13B H 0.6372 0.0599 0.3029 0.031 Uiso 1 1 calc R U . . .
C13C C -0.1534(5) 0.2513(5) 0.4346(3) 0.0231(13) Uani 1 1 d . . . . .
H13C H -0.1760 0.1835 0.4277 0.028 Uiso 1 1 calc R U . . .
C14A C 0.4600(8) 0.4170(7) 0.8922(4) 0.044(2) Uani 1 1 d . . . . .
H14A H 0.4761 0.4861 0.8983 0.053 Uiso 1 1 calc R U . . .
C14B C 0.5771(6) 0.1170(6) 0.3870(3) 0.0259(14) Uani 1 1 d . . . . .
H14B H 0.6326 0.1113 0.4154 0.031 Uiso 1 1 calc R U . . .
C14C C -0.2522(8) 0.5598(8) 0.9299(5) 0.051(3) Uani 1 1 d . . . . .
H14C H -0.3047 0.5668 0.8998 0.061 Uiso 1 1 calc R U . . .
C15A C 0.3848(6) 0.3662(5) 0.8452(3) 0.0272(15) Uani 1 1 d . . . . .
H15A H 0.3500 0.4010 0.8193 0.033 Uiso 1 1 calc R U . . .
C15B C 0.4925(5) 0.1555(5) 0.4108(3) 0.0230(13) Uani 1 1 d . . . . .
H15B H 0.4914 0.1760 0.4555 0.028 Uiso 1 1 calc R U . . .
C15C C -0.1663(8) 0.5225(8) 0.9092(5) 0.051(3) Uani 1 1 d . . . . .
H15C H -0.1612 0.5050 0.8650 0.061 Uiso 1 1 calc R U . . .
C16A C 0.3586(5) 0.2599(5) 0.8353(3) 0.0157(11) Uani 1 1 d . . . . .
C16B C 0.4060(5) 0.1647(5) 0.3686(3) 0.0170(12) Uani 1 1 d . . . . .
C16C C -0.0832(7) 0.5090(6) 0.9531(5) 0.041(2) Uani 1 1 d . . . . .
C068 C -0.0466(5) 0.1661(6) 0.6420(3) 0.0271(15) Uani 1 1 d . . . . .
H068 H -0.0160 0.1728 0.6072 0.033 Uiso 1 1 calc R U . . .
C081 C -0.1154(10) 0.0551(10) 0.6963(6) 0.065(3) Uani 1 1 d . . . . .
H08A H -0.1090 0.1178 0.7316 0.098 Uiso 1 1 d R U . . .
H08B H -0.0791 0.0038 0.7100 0.098 Uiso 1 1 d R U . . .
H08C H -0.1845 0.0320 0.6839 0.098 Uiso 1 1 d R U . . .
C084 C -0.0593(11) -0.0197(8) 0.5883(5) 0.067(4) Uani 1 1 d . . . . .
H08D H -0.1220 -0.0568 0.5687 0.101 Uiso 1 1 d R U . . .
H08E H -0.0166 -0.0628 0.6061 0.101 Uiso 1 1 d R U . . .
H08F H -0.0284 0.0005 0.5560 0.101 Uiso 1 1 d R U . . .
N1N N 0.1980(9) 0.0605(6) 0.5726(4) 0.054(3) Uani 1 1 d . . . . .
N2J N -0.0750(5) 0.0732(5) 0.6415(3) 0.0354(16) Uani 1 1 d . . . . .
N2N N 0.1681(6) 0.5730(5) 0.7438(4) 0.0385(17) Uani 1 1 d . . . . .
N3D N 0.6120(5) 0.1688(6) 0.5796(4) 0.0387(17) Uani 1 1 d . . . . .
N3F N -0.2394(6) 0.5045(6) 0.6407(5) 0.053(2) Uani 1 1 d . . . . .
N3G N 0.7462(12) 0.2653(9) 1.0339(6) 0.1029(19) Uani 1 1 d . U . . .
N3NB N 0.5074(17) -0.2339(17) 0.9310(12) 0.0456(13) Uani 0.4 1 d . U P A 2
N3Z N 0.4398(7) 0.5646(7) 0.6972(4) 0.0567(14) Uani 1 1 d . U . . .
O1A O 0.1462(4) 0.2860(4) 0.7483(2) 0.0212(9) Uani 1 1 d . . . . .
O1B O 0.2690(5) 0.1582(4) 0.4826(2) 0.0387(15) Uani 1 1 d . . . . .
O1C O -0.0362(5) 0.3691(5) 0.8201(3) 0.0452(17) Uani 1 1 d . . . . .
O1D O 0.4532(4) 0.1974(6) 0.5950(3) 0.0467(17) Uani 1 1 d . . . . .
O1F O -0.1111(5) 0.4620(5) 0.7100(5) 0.061(2) Uani 1 1 d . . . . .
O1G O 0.7167(5) 0.0941(5) 0.9853(3) 0.0446(12) Uani 1 1 d . U . . .
O1J O -0.0577(4) 0.2467(4) 0.6861(3) 0.0268(11) Uani 1 1 d . . . . .
O1N O 0.1507(5) 0.1402(4) 0.5768(3) 0.0349(13) Uani 1 1 d . . . . .
O1XB O 0.8087(11) -0.1015(12) 0.9455(8) 0.0362(11) Uani 0.4 1 d . U P B 2
O1Z O 0.3796(4) 0.4043(5) 0.6391(3) 0.0440(12) Uani 1 1 d . U . . .
O2A O 0.2796(4) 0.2686(3) 0.6954(2) 0.0190(9) Uani 1 1 d . . . . .
O2B O 0.3549(4) 0.3060(4) 0.5033(2) 0.0209(9) Uani 1 1 d . . . . .
O2C O 0.0764(5) 0.4981(4) 0.8432(3) 0.0379(14) Uani 1 1 d . . . . .
O2N O 0.2889(7) 0.0745(5) 0.5880(3) 0.0469(18) Uani 1 1 d . . . . .
O3A O 0.5237(4) 0.0267(5) 0.9073(3) 0.0388(14) Uani 1 1 d . . . . .
O3B O 0.6260(5) -0.1741(4) 0.8339(3) 0.0381(14) Uani 1 1 d . . . . .
O3C O 0.0488(4) 0.3677(4) 0.6247(3) 0.0283(11) Uani 1 1 d . . . . .
O3N O 0.1564(10) -0.0260(6) 0.5520(5) 0.100(4) Uani 1 1 d . . . . .
O4A O 0.3893(4) 0.0353(5) 0.9585(3) 0.0394(15) Uani 1 1 d . . . . .
O4B O 0.7146(4) -0.0318(5) 0.8524(3) 0.0392(15) Uani 1 1 d . . . . .
O4C O 0.1768(4) 0.3469(4) 0.5681(2) 0.0240(10) Uani 1 1 d . . . . .
O4N O 0.1994(4) 0.4844(4) 0.7427(3) 0.0300(11) Uani 1 1 d . . . . .
O5N O 0.0740(4) 0.5727(4) 0.7315(3) 0.0396(15) Uani 1 1 d . . . . .
O6N O 0.2249(6) 0.6465(6) 0.7544(4) 0.062(2) Uani 1 1 d . . . . .
O7NB O 0.4798(14) -0.1476(13) 0.9277(9) 0.042(3) Uani 0.4 1 d . U P A 2
O8NB O 0.6019(13) -0.2381(11) 0.9477(6) 0.0261(18) Uani 0.4 1 d . U P A 2
O9NB O 0.4520(11) -0.3116(10) 0.9192(6) 0.0293(19) Uani 0.4 1 d . U P A 2
C1 C 0.8526(15) -0.1819(18) 0.9257(11) 0.037(3) Uani 0.4 1 d . U P B 2
H1 H 0.8158 -0.2446 0.9143 0.044 Uiso 0.4 1 calc R U P B 2
C0AA C 0.9937(16) -0.2826(18) 0.8947(14) 0.046(4) Uani 0.4 1 d . U P B 2
H0AA H 1.0168 -0.3086 0.9303 0.069 Uiso 0.4 1 calc R U P B 2
H0AB H 1.0488 -0.2725 0.8729 0.069 Uiso 0.4 1 calc R U P B 2
H0AC H 0.9447 -0.3310 0.8647 0.069 Uiso 0.4 1 calc R U P B 2
N4 N 0.9483(13) -0.1825(16) 0.9202(11) 0.044(2) Uani 0.4 1 d . U P B 2
C1AA C 1.0096(17) -0.0856(19) 0.9293(15) 0.050(4) Uani 0.4 1 d . U P B 2
H1AA H 0.9769 -0.0470 0.9030 0.075 Uiso 0.4 1 calc R U P B 2
H1AB H 1.0739 -0.1020 0.9164 0.075 Uiso 0.4 1 calc R U P B 2
H1AC H 1.0173 -0.0456 0.9742 0.075 Uiso 0.4 1 calc R U P B 2
N1 N 0.9117(10) -0.1578(13) 1.0417(7) 0.0520(17) Uani 0.6 1 d . U P B 1
C2 C 0.8287(10) -0.1203(10) 1.0291(7) 0.0329(16) Uani 0.6 1 d . U P B 1
H2 H 0.7907 -0.0990 1.0629 0.040 Uiso 0.6 1 calc R U P B 1
C3 C 0.9526(14) -0.148(2) 1.1060(9) 0.077(4) Uani 0.6 1 d . U P B 1
H3A H 0.9882 -0.0825 1.1248 0.116 Uiso 0.6 1 calc R U P B 1
H3B H 0.9976 -0.2015 1.1063 0.116 Uiso 0.6 1 calc R U P B 1
H3C H 0.9001 -0.1544 1.1308 0.116 Uiso 0.6 1 calc R U P B 1
C5 C 0.9693(13) -0.2024(17) 0.9891(8) 0.059(3) Uani 0.6 1 d . U P B 1
H5D H 0.9249 -0.2396 0.9509 0.089 Uiso 0.6 1 calc R U P B 1
H5E H 1.0144 -0.2483 1.0020 0.089 Uiso 0.6 1 calc R U P B 1
H5F H 1.0064 -0.1487 0.9799 0.089 Uiso 0.6 1 calc R U P B 1
O1XA O 0.7940(7) -0.1099(8) 0.9753(5) 0.0362(11) Uani 0.6 1 d . U P B 1
N3NA N 0.5504(12) -0.2573(10) 0.9268(8) 0.0456(13) Uani 0.6 1 d . U P B 1
O8NA O 0.6457(9) -0.2352(8) 0.9446(6) 0.041(2) Uani 0.6 1 d . U P B 1
O9NA O 0.5159(9) -0.3448(8) 0.9096(8) 0.062(3) Uani 0.6 1 d . U P B 1
O7NA O 0.4989(9) -0.1849(9) 0.9200(6) 0.0381(19) Uani 0.6 1 d . U P B 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O4C 2.209(4) . ?
Yb1 O1Z 2.215(6) . ?
Yb1 O2A 2.235(4) . ?
Yb1 O1D 2.254(5) . ?
Yb1 O1B 2.325(5) . ?
Yb1 O2N 2.410(6) . ?
Yb1 O1N 2.418(6) . ?
Yb1 O2B 2.439(5) . ?
Yb1 C1B 2.733(6) . ?
Yb1 N1N 2.818(7) . ?
Yb2 O1A 2.225(4) . ?
Yb2 O1F 2.267(6) . ?
Yb2 O3C 2.267(5) . ?
Yb2 O1J 2.311(5) . ?
Yb2 O2C 2.376(6) . ?
Yb2 O1C 2.391(6) . ?
Yb2 O4N 2.403(5) . ?
Yb2 O5N 2.408(5) . ?
Yb2 C1C 2.739(9) . ?
Yb2 N2N 2.850(7) . ?
Yb3 O4A 2.223(5) 2_657 ?
Yb3 O3A 2.231(5) . ?
Yb3 O1XA 2.271(9) . ?
Yb3 O1G 2.272(7) . ?
Yb3 O3B 2.316(5) . ?
Yb3 O1XB 2.322(14) . ?
Yb3 O8NA 2.345(10) . ?
Yb3 O7NB 2.386(17) . ?
Yb3 O4B 2.388(6) . ?
Yb3 O7NA 2.407(11) . ?
Yb3 O8NB 2.457(13) . ?
Yb3 C2B 2.699(7) . ?
C1A O1A 1.259(7) . ?
C1A O2A 1.260(7) . ?
C1A C3A 1.508(7) . ?
C1B O2B 1.247(8) . ?
C1B O1B 1.279(8) . ?
C1B C3B 1.497(8) . ?
C1C O2C 1.244(9) . ?
C1C O1C 1.286(11) . ?
C1C C3C 1.511(12) . ?
C2A O3A 1.250(8) . ?
C2A O4A 1.266(9) . ?
C2A C10A 1.517(8) . ?
C2B O3B 1.233(9) . ?
C2B O4B 1.255(8) . ?
C2B C10B 1.504(9) 2_656 ?
C2C O4C 1.245(8) . ?
C2C O3C 1.253(8) . ?
C2C C10C 1.512(8) . ?
C2D O1D 1.156(13) . ?
C2D N3D 1.375(13) . ?
C2D H2D 0.9300 . ?
C2F N3F 1.321(10) . ?
C2F O1F 1.348(14) . ?
C2F H2F 0.9300 . ?
C2G O1G 1.203(13) . ?
C2G N3G 1.307(17) . ?
C2G H2G 0.9300 . ?
C2Z O1Z 1.233(11) . ?
C2Z N3Z 1.316(13) . ?
C2Z H2Z 0.9300 . ?
C3A C16A 1.386(8) . ?
C3A C4A 1.405(8) . ?
C3B C4B 1.402(9) . ?
C3B C16B 1.406(9) . ?
C3C C4C 1.409(15) . ?
C3C C16C 1.432(12) . ?
C4A C9A 1.431(7) . ?
C4A C5A 1.433(8) . ?
C4B C9B 1.416(9) . ?
C4B C5B 1.438(9) . ?
C4C C5C 1.449(12) . ?
C4C C16C 1.456(12) 2_567 ?
C4D N3D 1.376(13) . ?
C4D H4DA 0.9611 . ?
C4D H4DB 0.9614 . ?
C4D H4DC 0.9612 . ?
C4F N3F 1.488(16) . ?
C4F H4FA 0.9629 . ?
C4F H4FB 0.9624 . ?
C4F H4FC 0.9624 . ?
C4G N3G 1.418(17) . ?
C4G H4GA 0.9731 . ?
C4G H4GB 0.9705 . ?
C4G H4GC 0.9751 . ?
C4Z N3Z 1.507(15) . ?
C4Z H4ZA 0.9636 . ?
C4Z H4ZB 0.9643 . ?
C4Z H4ZC 0.9636 . ?
C5A C6A 1.366(9) . ?
C5A H5A 0.9300 . ?
C5B C6B 1.359(11) . ?
C5B H5B 0.9300 . ?
C5C C6C 1.376(15) . ?
C5C H5C 0.9300 . ?
C5D N3D 1.440(14) . ?
C5D H5DA 0.9614 . ?
C5D H5DB 0.9614 . ?
C5D H5DC 0.9628 . ?
C5F N3F 1.456(15) . ?
C5F H5FA 0.9612 . ?
C5F H5FB 0.9621 . ?
C5F H5FC 0.9615 . ?
C5G N3G 1.481(16) . ?
C5G H5GA 0.9665 . ?
C5G H5GB 0.9682 . ?
C5G H5GC 0.9672 . ?
C5Z N3Z 1.420(13) . ?
C5Z H5ZA 1.0006 . ?
C5Z H5ZB 1.0280 . ?
C5Z H5ZC 0.9915 . ?
C6A C7AA 1.422(11) . ?
C6A H6A 0.9300 . ?
C6B C7B 1.397(11) . ?
C6B H6B 0.9300 . ?
C6C C14C 1.438(13) 2_567 ?
C6C H6C 0.9300 . ?
C7B C8B 1.373(10) . ?
C7B H7B 0.9300 . ?
C7C C8C 1.372(10) . ?
C7C C13C 1.414(9) 2_566 ?
C7C H7C 0.9300 . ?
C7AA C8A 1.331(11) . ?
C7AA H7AA 0.9300 . ?
C8A C9A 1.433(9) . ?
C8A H8A 0.9300 . ?
C8B C9B 1.431(9) . ?
C8B H8B 0.9300 . ?
C8C C9C 1.434(9) . ?
C8C H8C 0.9300 . ?
C9A C10A 1.389(9) . ?
C9B C10B 1.408(9) . ?
C9C C10C 1.419(9) . ?
C9C C11C 1.445(8) 2_566 ?
C10A C11A 1.398(9) . ?
C10B C11B 1.408(9) . ?
C10B C2B 1.504(9) 2_656 ?
C10C C11C 1.410(9) . ?
C11A C12A 1.416(9) . ?
C11A C16A 1.440(8) . ?
C11B C16B 1.427(8) . ?
C11B C12B 1.434(9) . ?
C11C C12C 1.432(9) . ?
C11C C9C 1.445(8) 2_566 ?
C12A C13A 1.360(13) . ?
C12A H12A 0.9300 . ?
C12B C13B 1.374(9) . ?
C12B H12B 0.9300 . ?
C12C C13C 1.353(10) . ?
C12C H12C 0.9300 . ?
C13A C14A 1.429(14) . ?
C13A H13A 0.9300 . ?
C13B C14B 1.416(10) . ?
C13B H13B 0.9300 . ?
C13C C7C 1.414(9) 2_566 ?
C13C H13C 0.9300 . ?
C14A C15A 1.361(10) . ?
C14A H14A 0.9300 . ?
C14B C15B 1.369(10) . ?
C14B H14B 0.9300 . ?
C14C C15C 1.358(13) . ?
C14C C6C 1.438(13) 2_567 ?
C14C H14C 0.9300 . ?
C15A C16A 1.430(9) . ?
C15A H15A 0.9300 . ?
C15B C16B 1.426(9) . ?
C15B H15B 0.9300 . ?
C15C C16C 1.432(15) . ?
C15C H15C 0.9300 . ?
C16C C4C 1.456(12) 2_567 ?
C068 O1J 1.258(9) . ?
C068 N2J 1.310(10) . ?
C068 H068 0.9300 . ?
C081 N2J 1.449(12) . ?
C081 H08A 0.9606 . ?
C081 H08B 0.9606 . ?
C081 H08C 0.9599 . ?
C084 N2J 1.485(12) . ?
C084 H08D 0.9602 . ?
C084 H08E 0.9602 . ?
C084 H08F 0.9601 . ?
N1N O3N 1.228(10) . ?
N1N O2N 1.231(12) . ?
N1N O1N 1.262(11) . ?
N2N O6N 1.197(9) . ?
N2N O5N 1.269(9) . ?
N2N O4N 1.286(8) . ?
N3NB O9NB 1.23(2) . ?
N3NB O7NB 1.26(3) . ?
N3NB O8NB 1.29(3) . ?
O1XB C1 1.25(3) . ?
O4A Yb3 2.223(5) 2_657 ?
C1 N4 1.32(3) . ?
C1 H1 0.9300 . ?
C0AA N4 1.49(3) . ?
C0AA H0AA 0.9600 . ?
C0AA H0AB 0.9600 . ?
C0AA H0AC 0.9600 . ?
N4 C1AA 1.49(3) . ?
C1AA H1AA 0.9600 . ?
C1AA H1AB 0.9600 . ?
C1AA H1AC 0.9600 . ?
N1 C2 1.280(16) . ?
N1 C3 1.40(2) . ?
N1 C5 1.45(2) . ?
C2 O1XA 1.249(17) . ?
C2 H2 0.9300 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C5 H5D 0.9600 . ?
C5 H5E 0.9600 . ?
C5 H5F 0.9600 . ?
N3NA O9NA 1.205(16) . ?
N3NA O7NA 1.255(18) . ?
N3NA O8NA 1.302(18) . ?

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
O4C Yb1 O1Z 83.5(2) . . ?
O4C Yb1 O2A 99.55(17) . . ?
O1Z Yb1 O2A 80.9(2) . . ?
O4C Yb1 O1D 156.0(2) . . ?
O1Z Yb1 O1D 82.5(3) . . ?
O2A Yb1 O1D 97.4(2) . . ?
O4C Yb1 O1B 86.1(2) . . ?
O1Z Yb1 O1B 129.7(2) . . ?
O2A Yb1 O1B 149.36(18) . . ?
O1D Yb1 O1B 88.0(3) . . ?
O4C Yb1 O2N 128.6(3) . . ?
O1Z Yb1 O2N 145.0(3) . . ?
O2A Yb1 O2N 80.12(19) . . ?
O1D Yb1 O2N 71.1(3) . . ?
O1B Yb1 O2N 73.1(2) . . ?
O4C Yb1 O1N 77.3(2) . . ?
O1Z Yb1 O1N 149.6(2) . . ?
O2A Yb1 O1N 79.36(18) . . ?
O1D Yb1 O1N 122.8(3) . . ?
O1B Yb1 O1N 72.5(2) . . ?
O2N Yb1 O1N 51.9(3) . . ?
O4C Yb1 O2B 77.86(17) . . ?
O1Z Yb1 O2B 74.7(2) . . ?
O2A Yb1 O2B 155.66(17) . . ?
O1D Yb1 O2B 79.70(19) . . ?
O1B Yb1 O2B 54.98(17) . . ?
O2N Yb1 O2B 120.65(18) . . ?
O1N Yb1 O2B 122.69(17) . . ?
O4C Yb1 C1B 80.45(19) . . ?
O1Z Yb1 C1B 101.9(2) . . ?
O2A Yb1 C1B 177.16(19) . . ?
O1D Yb1 C1B 83.5(2) . . ?
O1B Yb1 C1B 27.84(19) . . ?
O2N Yb1 C1B 97.6(2) . . ?
O1N Yb1 C1B 97.89(19) . . ?
O2B Yb1 C1B 27.15(18) . . ?
O4C Yb1 N1N 102.9(3) . . ?
O1Z Yb1 N1N 162.1(2) . . ?
O2A Yb1 N1N 81.6(2) . . ?
O1D Yb1 N1N 96.3(3) . . ?
O1B Yb1 N1N 67.8(2) . . ?
O2N Yb1 N1N 25.7(3) . . ?
O1N Yb1 N1N 26.5(3) . . ?
O2B Yb1 N1N 122.72(19) . . ?
C1B Yb1 N1N 95.7(2) . . ?
O1A Yb2 O1F 158.4(2) . . ?
O1A Yb2 O3C 95.65(18) . . ?
O1F Yb2 O3C 85.8(3) . . ?
O1A Yb2 O1J 78.94(18) . . ?
O1F Yb2 O1J 80.4(2) . . ?
O3C Yb2 O1J 77.47(19) . . ?
O1A Yb2 O2C 90.4(2) . . ?
O1F Yb2 O2C 98.2(3) . . ?
O3C Yb2 O2C 152.7(2) . . ?
O1J Yb2 O2C 129.80(19) . . ?
O1A Yb2 O1C 85.8(2) . . ?
O1F Yb2 O1C 83.0(3) . . ?
O3C Yb2 O1C 151.9(2) . . ?
O1J Yb2 O1C 75.29(19) . . ?
O2C Yb2 O1C 55.0(2) . . ?
O1A Yb2 O4N 75.07(18) . . ?
O1F Yb2 O4N 126.3(2) . . ?
O3C Yb2 O4N 82.09(19) . . ?
O1J Yb2 O4N 144.96(18) . . ?
O2C Yb2 O4N 73.8(2) . . ?
O1C Yb2 O4N 125.0(2) . . ?
O1A Yb2 O5N 127.71(19) . . ?
O1F Yb2 O5N 73.8(2) . . ?
O3C Yb2 O5N 81.3(2) . . ?
O1J Yb2 O5N 147.59(19) . . ?
O2C Yb2 O5N 74.0(2) . . ?
O1C Yb2 O5N 119.6(2) . . ?
O4N Yb2 O5N 52.72(18) . . ?
O1A Yb2 C1C 87.0(2) . . ?
O1F Yb2 C1C 91.7(3) . . ?
O3C Yb2 C1C 177.3(2) . . ?
O1J Yb2 C1C 103.0(2) . . ?
O2C Yb2 C1C 27.0(2) . . ?
O1C Yb2 C1C 28.0(2) . . ?
O4N Yb2 C1C 98.8(2) . . ?
O5N Yb2 C1C 97.2(2) . . ?
O1A Yb2 N2N 101.5(2) . . ?
O1F Yb2 N2N 100.1(2) . . ?
O3C Yb2 N2N 82.9(2) . . ?
O1J Yb2 N2N 160.3(2) . . ?
O2C Yb2 N2N 69.9(2) . . ?
O1C Yb2 N2N 124.4(2) . . ?
O4N Yb2 N2N 26.63(19) . . ?
O5N Yb2 N2N 26.25(19) . . ?
C1C Yb2 N2N 96.8(2) . . ?
O4A Yb3 O3A 97.3(2) 2_657 . ?
O4A Yb3 O1XA 86.2(3) 2_657 . ?
O3A Yb3 O1XA 160.1(3) . . ?
O4A Yb3 O1G 79.2(3) 2_657 . ?
O3A Yb3 O1G 80.2(2) . . ?
O1XA Yb3 O1G 81.2(3) . . ?
O4A Yb3 O3B 149.5(2) 2_657 . ?
O3A Yb3 O3B 89.1(2) . . ?
O1XA Yb3 O3B 97.8(3) . . ?
O1G Yb3 O3B 131.2(2) . . ?
O4A Yb3 O1XB 103.6(4) 2_657 . ?
O3A Yb3 O1XB 146.9(4) . . ?
O1G Yb3 O1XB 78.9(4) . . ?
O3B Yb3 O1XB 85.7(5) . . ?
O4A Yb3 O8NA 82.4(4) 2_657 . ?
O3A Yb3 O8NA 134.3(3) . . ?
O1XA Yb3 O8NA 65.5(4) . . ?
O1G Yb3 O8NA 142.9(3) . . ?
O3B Yb3 O8NA 72.1(3) . . ?
O4A Yb3 O7NB 76.5(5) 2_657 . ?
O3A Yb3 O7NB 68.7(4) . . ?
O1G Yb3 O7NB 137.3(5) . . ?
O3B Yb3 O7NB 78.2(5) . . ?
O1XB Yb3 O7NB 141.0(6) . . ?
O4A Yb3 O4B 155.7(2) 2_657 . ?
O3A Yb3 O4B 81.3(2) . . ?
O1XA Yb3 O4B 87.4(3) . . ?
O1G Yb3 O4B 76.6(2) . . ?
O3B Yb3 O4B 54.74(19) . . ?
O1XB Yb3 O4B 69.1(4) . . ?
O8NA Yb3 O4B 116.0(4) . . ?
O7NB Yb3 O4B 124.2(5) . . ?
O4A Yb3 O7NA 81.3(3) 2_657 . ?
O3A Yb3 O7NA 80.2(3) . . ?
O1XA Yb3 O7NA 119.7(4) . . ?
O1G Yb3 O7NA 150.3(3) . . ?
O3B Yb3 O7NA 70.4(3) . . ?
O8NA Yb3 O7NA 54.4(4) . . ?
O4B Yb3 O7NA 121.9(3) . . ?
O4A Yb3 O8NB 76.7(4) 2_657 . ?
O3A Yb3 O8NB 121.4(5) . . ?
O1G Yb3 O8NB 149.3(4) . . ?
O3B Yb3 O8NB 74.6(3) . . ?
O1XB Yb3 O8NB 88.6(6) . . ?
O7NB Yb3 O8NB 53.1(6) . . ?
O4B Yb3 O8NB 124.8(4) . . ?
O4A Yb3 C2B 176.6(2) 2_657 . ?
O3A Yb3 C2B 83.0(2) . . ?
O1XA Yb3 C2B 94.6(3) . . ?
O1G Yb3 C2B 104.1(2) . . ?
O3B Yb3 C2B 27.1(2) . . ?
O1XB Yb3 C2B 77.6(4) . . ?
O8NA Yb3 C2B 94.9(4) . . ?
O7NB Yb3 C2B 100.5(5) . . ?
O4B Yb3 C2B 27.71(19) . . ?
O7NA Yb3 C2B 95.4(3) . . ?
O8NB Yb3 C2B 100.2(4) . . ?
O1A C1A O2A 125.5(5) . . ?
O1A C1A C3A 117.6(5) . . ?
O2A C1A C3A 116.9(5) . . ?
O2B C1B O1B 121.2(6) . . ?
O2B C1B C3B 122.1(6) . . ?
O1B C1B C3B 116.6(6) . . ?
O2B C1B Yb1 63.2(3) . . ?
O1B C1B Yb1 58.0(3) . . ?
C3B C1B Yb1 174.7(5) . . ?
O2C C1C O1C 120.7(8) . . ?
O2C C1C C3C 118.4(8) . . ?
O1C C1C C3C 120.7(7) . . ?
O2C C1C Yb2 60.0(5) . . ?
O1C C1C Yb2 60.8(4) . . ?
C3C C1C Yb2 178.3(6) . . ?
O3A C2A O4A 125.3(6) . . ?
O3A C2A C10A 118.1(6) . . ?
O4A C2A C10A 116.6(6) . . ?
O3B C2B O4B 120.8(7) . . ?
O3B C2B C10B 117.7(6) . 2_656 ?
O4B C2B C10B 121.5(6) . 2_656 ?
O3B C2B Yb3 58.9(4) . . ?
O4B C2B Yb3 62.2(4) . . ?
C10B C2B Yb3 173.5(4) 2_656 . ?
O4C C2C O3C 125.7(6) . . ?
O4C C2C C10C 116.7(5) . . ?
O3C C2C C10C 117.5(5) . . ?
O1D C2D N3D 124.7(10) . . ?
O1D C2D H2D 117.7 . . ?
N3D C2D H2D 117.7 . . ?
N3F C2F O1F 123.4(10) . . ?
N3F C2F H2F 118.3 . . ?
O1F C2F H2F 118.3 . . ?
O1G C2G N3G 129.2(13) . . ?
O1G C2G H2G 115.4 . . ?
N3G C2G H2G 115.4 . . ?
O1Z C2Z N3Z 124.5(11) . . ?
O1Z C2Z H2Z 117.7 . . ?
N3Z C2Z H2Z 117.7 . . ?
C16A C3A C4A 120.7(5) . . ?
C16A C3A C1A 119.7(5) . . ?
C4A C3A C1A 119.6(5) . . ?
C4B C3B C16B 122.2(6) . . ?
C4B C3B C1B 119.9(6) . . ?
C16B C3B C1B 117.9(6) . . ?
C4C C3C C16C 122.8(8) . . ?
C4C C3C C1C 119.3(7) . . ?
C16C C3C C1C 117.8(9) . . ?
C3A C4A C9A 119.6(5) . . ?
C3A C4A C5A 121.9(5) . . ?
C9A C4A C5A 118.5(5) . . ?
C3B C4B C9B 118.9(6) . . ?
C3B C4B C5B 122.2(6) . . ?
C9B C4B C5B 118.9(6) . . ?
C3C C4C C5C 123.5(8) . . ?
C3C C4C C16C 119.7(8) . 2_567 ?
C5C C4C C16C 116.8(9) . 2_567 ?
N3D C4D H4DA 109.5 . . ?
N3D C4D H4DB 108.7 . . ?
H4DA C4D H4DB 109.3 . . ?
N3D C4D H4DC 110.5 . . ?
H4DA C4D H4DC 109.3 . . ?
H4DB C4D H4DC 109.4 . . ?
N3F C4F H4FA 110.5 . . ?
N3F C4F H4FB 110.1 . . ?
H4FA C4F H4FB 109.2 . . ?
N3F C4F H4FC 108.6 . . ?
H4FA C4F H4FC 109.2 . . ?
H4FB C4F H4FC 109.2 . . ?
N3G C4G H4GA 113.9 . . ?
N3G C4G H4GB 112.3 . . ?
H4GA C4G H4GB 107.5 . . ?
N3G C4G H4GC 106.0 . . ?
H4GA C4G H4GC 108.1 . . ?
H4GB C4G H4GC 108.9 . . ?
N3Z C4Z H4ZA 110.3 . . ?
N3Z C4Z H4ZB 108.4 . . ?
H4ZA C4Z H4ZB 109.2 . . ?
N3Z C4Z H4ZC 110.9 . . ?
H4ZA C4Z H4ZC 109.1 . . ?
H4ZB C4Z H4ZC 109.0 . . ?
C6A C5A C4A 119.4(6) . . ?
C6A C5A H5A 120.3 . . ?
C4A C5A H5A 120.3 . . ?
C6B C5B C4B 120.8(7) . . ?
C6B C5B H5B 119.6 . . ?
C4B C5B H5B 119.6 . . ?
C6C C5C C4C 122.7(8) . . ?
C6C C5C H5C 118.6 . . ?
C4C C5C H5C 118.6 . . ?
N3D C5D H5DA 110.2 . . ?
N3D C5D H5DB 109.5 . . ?
H5DA C5D H5DB 109.2 . . ?
N3D C5D H5DC 109.3 . . ?
H5DA C5D H5DC 109.3 . . ?
H5DB C5D H5DC 109.4 . . ?
N3F C5F H5FA 109.8 . . ?
N3F C5F H5FB 109.6 . . ?
H5FA C5F H5FB 109.4 . . ?
N3F C5F H5FC 109.5 . . ?
H5FA C5F H5FC 109.3 . . ?
H5FB C5F H5FC 109.4 . . ?
N3G C5G H5GA 109.8 . . ?
N3G C5G H5GB 105.9 . . ?
H5GA C5G H5GB 108.8 . . ?
N3G C5G H5GC 114.7 . . ?
H5GA C5G H5GC 108.7 . . ?
H5GB C5G H5GC 108.7 . . ?
N3Z C5Z H5ZA 116.1 . . ?
N3Z C5Z H5ZB 118.3 . . ?
H5ZA C5Z H5ZB 104.2 . . ?
N3Z C5Z H5ZC 106.2 . . ?
H5ZA C5Z H5ZC 105.6 . . ?
H5ZB C5Z H5ZC 105.3 . . ?
C5A C6A C7AA 121.6(7) . . ?
C5A C6A H6A 119.2 . . ?
C7AA C6A H6A 119.2 . . ?
C5B C6B C7B 120.4(7) . . ?
C5B C6B H6B 119.8 . . ?
C7B C6B H6B 119.8 . . ?
C5C C6C C14C 119.1(9) . 2_567 ?
C5C C6C H6C 120.4 . . ?
C14C C6C H6C 120.4 2_567 . ?
C8B C7B C6B 120.9(8) . . ?
C8B C7B H7B 119.6 . . ?
C6B C7B H7B 119.6 . . ?
C8C C7C C13C 121.0(6) . 2_566 ?
C8C C7C H7C 119.5 . . ?
C13C C7C H7C 119.5 2_566 . ?
C8A C7AA C6A 120.4(6) . . ?
C8A C7AA H7AA 119.8 . . ?
C6A C7AA H7AA 119.8 . . ?
C7AA C8A C9A 120.9(6) . . ?
C7AA C8A H8A 119.6 . . ?
C9A C8A H8A 119.6 . . ?
C7B C8B C9B 120.6(7) . . ?
C7B C8B H8B 119.7 . . ?
C9B C8B H8B 119.7 . . ?
C7C C8C C9C 120.9(6) . . ?
C7C C8C H8C 119.5 . . ?
C9C C8C H8C 119.5 . . ?
C10A C9A C4A 119.5(5) . . ?
C10A C9A C8A 121.4(6) . . ?
C4A C9A C8A 119.1(6) . . ?
C10B C9B C4B 119.5(6) . . ?
C10B C9B C8B 122.2(6) . . ?
C4B C9B C8B 118.3(6) . . ?
C10C C9C C8C 123.2(5) . . ?
C10C C9C C11C 119.4(6) . 2_566 ?
C8C C9C C11C 117.4(6) . 2_566 ?
C9A C10A C11A 121.4(5) . . ?
C9A C10A C2A 119.0(6) . . ?
C11A C10A C2A 119.7(6) . . ?
C11B C10B C9B 121.6(6) . . ?
C11B C10B C2B 118.9(6) . 2_656 ?
C9B C10B C2B 119.4(6) . 2_656 ?
C11C C10C C9C 121.6(5) . . ?
C11C C10C C2C 119.9(6) . . ?
C9C C10C C2C 118.4(5) . . ?
C10A C11A C12A 121.9(6) . . ?
C10A C11A C16A 119.0(5) . . ?
C12A C11A C16A 119.1(6) . . ?
C10B C11B C16B 119.0(6) . . ?
C10B C11B C12B 122.5(6) . . ?
C16B C11B C12B 118.5(6) . . ?
C10C C11C C12C 121.8(5) . . ?
C10C C11C C9C 119.0(6) . 2_566 ?
C12C C11C C9C 119.3(6) . 2_566 ?
C13A C12A C11A 120.7(8) . . ?
C13A C12A H12A 119.7 . . ?
C11A C12A H12A 119.7 . . ?
C13B C12B C11B 120.7(6) . . ?
C13B C12B H12B 119.7 . . ?
C11B C12B H12B 119.7 . . ?
C13C C12C C11C 121.0(6) . . ?
C13C C12C H12C 119.5 . . ?
C11C C12C H12C 119.5 . . ?
C12A C13A C14A 120.8(7) . . ?
C12A C13A H13A 119.6 . . ?
C14A C13A H13A 119.6 . . ?
C12B C13B C14B 120.9(6) . . ?
C12B C13B H13B 119.6 . . ?
C14B C13B H13B 119.6 . . ?
C12C C13C C7C 120.4(7) . 2_566 ?
C12C C13C H13C 119.8 . . ?
C7C C13C H13C 119.8 2_566 . ?
C15A C14A C13A 120.2(7) . . ?
C15A C14A H14A 119.9 . . ?
C13A C14A H14A 119.9 . . ?
C15B C14B C13B 119.6(7) . . ?
C15B C14B H14B 120.2 . . ?
C13B C14B H14B 120.2 . . ?
C15C C14C C6C 120.4(11) . 2_567 ?
C15C C14C H14C 119.8 . . ?
C6C C14C H14C 119.8 2_567 . ?
C14A C15A C16A 120.8(7) . . ?
C14A C15A H15A 119.6 . . ?
C16A C15A H15A 119.6 . . ?
C14B C15B C16B 121.6(6) . . ?
C14B C15B H15B 119.2 . . ?
C16B C15B H15B 119.2 . . ?
C14C C15C C16C 122.3(9) . . ?
C14C C15C H15C 118.8 . . ?
C16C C15C H15C 118.8 . . ?
C3A C16A C15A 121.7(6) . . ?
C3A C16A C11A 119.9(5) . . ?
C15A C16A C11A 118.4(6) . . ?
C3B C16B C15B 122.4(6) . . ?
C3B C16B C11B 118.8(6) . . ?
C15B C16B C11B 118.8(6) . . ?
C15C C16C C3C 123.9(8) . . ?
C15C C16C C4C 118.6(8) . 2_567 ?
C3C C16C C4C 117.5(9) . 2_567 ?
O1J C068 N2J 124.7(7) . . ?
O1J C068 H068 117.6 . . ?
N2J C068 H068 117.6 . . ?
N2J C081 H08A 109.4 . . ?
N2J C081 H08B 109.3 . . ?
H08A C081 H08B 109.4 . . ?
N2J C081 H08C 109.8 . . ?
H08A C081 H08C 109.5 . . ?
H08B C081 H08C 109.5 . . ?
N2J C084 H08D 110.1 . . ?
N2J C084 H08E 109.0 . . ?
H08D C084 H08E 109.5 . . ?
N2J C084 H08F 109.3 . . ?
H08D C084 H08F 109.4 . . ?
H08E C084 H08F 109.5 . . ?
O3N N1N O2N 121.9(11) . . ?
O3N N1N O1N 122.1(12) . . ?
O2N N1N O1N 116.0(7) . . ?
O3N N1N Yb1 167.9(7) . . ?
O2N N1N Yb1 58.3(4) . . ?
O1N N1N Yb1 58.7(4) . . ?
C068 N2J C081 121.1(8) . . ?
C068 N2J C084 122.6(8) . . ?
C081 N2J C084 116.0(8) . . ?
O6N N2N O5N 125.2(8) . . ?
O6N N2N O4N 121.3(8) . . ?
O5N N2N O4N 113.5(6) . . ?
O6N N2N Yb2 174.1(6) . . ?
O5N N2N Yb2 57.1(4) . . ?
O4N N2N Yb2 56.9(4) . . ?
C2D N3D C4D 129.6(11) . . ?
C2D N3D C5D 112.2(10) . . ?
C4D N3D C5D 118.3(12) . . ?
C2F N3F C5F 120.8(10) . . ?
C2F N3F C4F 118.1(10) . . ?
C5F N3F C4F 121.1(9) . . ?
C2G N3G C4G 121.4(11) . . ?
C2G N3G C5G 124.1(12) . . ?
C4G N3G C5G 111.8(12) . . ?
O9NB N3NB O7NB 125(2) . . ?
O9NB N3NB O8NB 119(2) . . ?
O7NB N3NB O8NB 115.7(18) . . ?
O9NB N3NB Yb3 171.7(19) . . ?
O7NB N3NB Yb3 56.5(11) . . ?
O8NB N3NB Yb3 59.8(9) . . ?
C2Z N3Z C5Z 128.7(10) . . ?
C2Z N3Z C4Z 119.8(9) . . ?
C5Z N3Z C4Z 111.1(9) . . ?
C1A O1A Yb2 143.2(4) . . ?
C1B O1B Yb1 94.1(4) . . ?
C1C O1C Yb2 91.2(5) . . ?
C2D O1D Yb1 136.1(7) . . ?
C2F O1F Yb2 125.8(6) . . ?
C2G O1G Yb3 143.0(8) . . ?
C068 O1J Yb2 133.1(5) . . ?
N1N O1N Yb1 94.7(6) . . ?
C1 O1XB Yb3 133.1(15) . . ?
C2Z O1Z Yb1 145.1(7) . . ?
C1A O2A Yb1 154.3(4) . . ?
C1B O2B Yb1 89.7(4) . . ?
C1C O2C Yb2 93.0(5) . . ?
N1N O2N Yb1 96.0(5) . . ?
C2A O3A Yb3 141.4(5) . . ?
C2B O3B Yb3 94.0(4) . . ?
C2C O3C Yb2 149.2(5) . . ?
C2A O4A Yb3 152.5(6) . 2_657 ?
C2B O4B Yb3 90.1(4) . . ?
C2C O4C Yb1 146.1(4) . . ?
N2N O4N Yb2 96.5(4) . . ?
N2N O5N Yb2 96.7(4) . . ?
N3NB O7NB Yb3 97.3(14) . . ?
N3NB O8NB Yb3 93.1(11) . . ?
O1XB C1 N4 123(2) . . ?
O1XB C1 H1 118.3 . . ?
N4 C1 H1 118.3 . . ?
N4 C0AA H0AA 109.5 . . ?
N4 C0AA H0AB 109.5 . . ?
H0AA C0AA H0AB 109.5 . . ?
N4 C0AA H0AC 109.5 . . ?
H0AA C0AA H0AC 109.5 . . ?
H0AB C0AA H0AC 109.5 . . ?
C1 N4 C1AA 121.5(19) . . ?
C1 N4 C0AA 120(2) . . ?
C1AA N4 C0AA 118.4(18) . . ?
N4 C1AA H1AA 109.5 . . ?
N4 C1AA H1AB 109.5 . . ?
H1AA C1AA H1AB 109.5 . . ?
N4 C1AA H1AC 109.5 . . ?
H1AA C1AA H1AC 109.5 . . ?
H1AB C1AA H1AC 109.5 . . ?
C2 N1 C3 121.0(14) . . ?
C2 N1 C5 119.5(14) . . ?
C3 N1 C5 119.2(13) . . ?
O1XA C2 N1 125.8(14) . . ?
O1XA C2 H2 117.1 . . ?
N1 C2 H2 117.1 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C5 H5D 109.5 . . ?
N1 C5 H5E 109.5 . . ?
H5D C5 H5E 109.5 . . ?
N1 C5 H5F 109.5 . . ?
H5D C5 H5F 109.5 . . ?
H5E C5 H5F 109.5 . . ?
C2 O1XA Yb3 131.0(9) . . ?
O9NA N3NA O7NA 121.6(15) . . ?
O9NA N3NA O8NA 121.3(14) . . ?
O7NA N3NA O8NA 116.4(12) . . ?
O9NA N3NA Yb3 167.6(14) . . ?
O7NA N3NA Yb3 59.6(7) . . ?
O8NA N3NA Yb3 57.0(6) . . ?
N3NA O8NA Yb3 95.2(8) . . ?
N3NA O7NA Yb3 93.6(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1A C1A C3A C16A -104.1(7) . . . . ?
O2A C1A C3A C16A 77.1(7) . . . . ?
O1A C1A C3A C4A 76.3(7) . . . . ?
O2A C1A C3A C4A -102.6(7) . . . . ?
O2B C1B C3B C4B -105.3(8) . . . . ?
O1B C1B C3B C4B 76.7(8) . . . . ?
O2B C1B C3B C16B 77.4(8) . . . . ?
O1B C1B C3B C16B -100.6(8) . . . . ?
O2C C1C C3C C4C -66.7(11) . . . . ?
O1C C1C C3C C4C 117.4(10) . . . . ?
O2C C1C C3C C16C 110.9(10) . . . . ?
O1C C1C C3C C16C -64.9(11) . . . . ?
C16A C3A C4A C9A -1.2(8) . . . . ?
C1A C3A C4A C9A 178.4(5) . . . . ?
C16A C3A C4A C5A 179.0(6) . . . . ?
C1A C3A C4A C5A -1.4(8) . . . . ?
C16B C3B C4B C9B 2.1(10) . . . . ?
C1B C3B C4B C9B -175.0(6) . . . . ?
C16B C3B C4B C5B -177.0(6) . . . . ?
C1B C3B C4B C5B 5.8(10) . . . . ?
C16C C3C C4C C5C 178.5(8) . . . . ?
C1C C3C C4C C5C -4.0(12) . . . . ?
C16C C3C C4C C16C 1.1(13) . . . 2_567 ?
C1C C3C C4C C16C 178.6(7) . . . 2_567 ?
C3A C4A C5A C6A 179.8(6) . . . . ?
C9A C4A C5A C6A 0.0(9) . . . . ?
C3B C4B C5B C6B 177.5(7) . . . . ?
C9B C4B C5B C6B -1.6(10) . . . . ?
C3C C4C C5C C6C -178.2(9) . . . . ?
C16C C4C C5C C6C -0.7(13) 2_567 . . . ?
C4A C5A C6A C7AA -1.1(10) . . . . ?
C4B C5B C6B C7B 2.4(11) . . . . ?
C4C C5C C6C C14C 0.8(15) . . . 2_567 ?
C5B C6B C7B C8B -1.2(13) . . . . ?
C5A C6A C7AA C8A 1.4(12) . . . . ?
C6A C7AA C8A C9A -0.6(11) . . . . ?
C6B C7B C8B C9B -0.8(13) . . . . ?
C13C C7C C8C C9C -2.3(11) 2_566 . . . ?
C3A C4A C9A C10A -0.7(8) . . . . ?
C5A C4A C9A C10A 179.1(5) . . . . ?
C3A C4A C9A C8A -179.0(5) . . . . ?
C5A C4A C9A C8A 0.8(8) . . . . ?
C7AA C8A C9A C10A -178.7(7) . . . . ?
C7AA C8A C9A C4A -0.5(9) . . . . ?
C3B C4B C9B C10B -1.1(10) . . . . ?
C5B C4B C9B C10B 178.1(6) . . . . ?
C3B C4B C9B C8B -179.5(6) . . . . ?
C5B C4B C9B C8B -0.4(10) . . . . ?
C7B C8B C9B C10B -176.8(7) . . . . ?
C7B C8B C9B C4B 1.6(11) . . . . ?
C7C C8C C9C C10C -176.1(6) . . . . ?
C7C C8C C9C C11C 2.5(10) . . . 2_566 ?
C4A C9A C10A C11A 0.4(9) . . . . ?
C8A C9A C10A C11A 178.7(6) . . . . ?
C4A C9A C10A C2A -179.6(5) . . . . ?
C8A C9A C10A C2A -1.4(9) . . . . ?
O3A C2A C10A C9A 106.7(9) . . . . ?
O4A C2A C10A C9A -72.5(9) . . . . ?
O3A C2A C10A C11A -73.3(10) . . . . ?
O4A C2A C10A C11A 107.5(9) . . . . ?
C4B C9B C10B C11B -0.4(10) . . . . ?
C8B C9B C10B C11B 178.0(7) . . . . ?
C4B C9B C10B C2B -176.6(6) . . . 2_656 ?
C8B C9B C10B C2B 1.8(10) . . . 2_656 ?
C8C C9C C10C C11C 179.4(6) . . . . ?
C11C C9C C10C C11C 0.7(10) 2_566 . . . ?
C8C C9C C10C C2C 0.9(9) . . . . ?
C11C C9C C10C C2C -177.7(5) 2_566 . . . ?
O4C C2C C10C C11C 106.9(7) . . . . ?
O3C C2C C10C C11C -71.9(8) . . . . ?
O4C C2C C10C C9C -74.6(8) . . . . ?
O3C C2C C10C C9C 106.6(7) . . . . ?
C9A C10A C11A C12A -178.8(7) . . . . ?
C2A C10A C11A C12A 1.2(10) . . . . ?
C9A C10A C11A C16A 1.7(9) . . . . ?
C2A C10A C11A C16A -178.2(6) . . . . ?
C9B C10B C11B C16B 0.9(10) . . . . ?
C2B C10B C11B C16B 177.1(6) 2_656 . . . ?
C9B C10B C11B C12B 178.9(7) . . . . ?
C2B C10B C11B C12B -4.8(10) 2_656 . . . ?
C9C C10C C11C C12C 177.8(6) . . . . ?
C2C C10C C11C C12C -3.8(9) . . . . ?
C9C C10C C11C C9C -0.7(10) . . . 2_566 ?
C2C C10C C11C C9C 177.7(5) . . . 2_566 ?
C10A C11A C12A C13A -177.1(8) . . . . ?
C16A C11A C12A C13A 2.4(12) . . . . ?
C10B C11B C12B C13B -178.5(7) . . . . ?
C16B C11B C12B C13B -0.5(11) . . . . ?
C10C C11C C12C C13C -177.5(6) . . . . ?
C9C C11C C12C C13C 1.0(9) 2_566 . . . ?
C11A C12A C13A C14A -0.5(15) . . . . ?
C11B C12B C13B C14B 0.1(12) . . . . ?
C11C C12C C13C C7C -1.3(10) . . . 2_566 ?
C12A C13A C14A C15A -0.9(15) . . . . ?
C12B C13B C14B C15B 0.0(12) . . . . ?
C13A C14A C15A C16A 0.3(14) . . . . ?
C13B C14B C15B C16B 0.3(11) . . . . ?
C6C C14C C15C C16C 0.7(17) 2_567 . . . ?
C4A C3A C16A C15A -176.8(6) . . . . ?
C1A C3A C16A C15A 3.5(9) . . . . ?
C4A C3A C16A C11A 3.4(9) . . . . ?
C1A C3A C16A C11A -176.2(5) . . . . ?
C14A C15A C16A C3A -178.1(7) . . . . ?
C14A C15A C16A C11A 1.6(11) . . . . ?
C10A C11A C16A C3A -3.7(9) . . . . ?
C12A C11A C16A C3A 176.9(7) . . . . ?
C10A C11A C16A C15A 176.6(6) . . . . ?
C12A C11A C16A C15A -2.9(10) . . . . ?
C4B C3B C16B C15B 179.7(6) . . . . ?
C1B C3B C16B C15B -3.1(10) . . . . ?
C4B C3B C16B C11B -1.6(10) . . . . ?
C1B C3B C16B C11B 175.6(6) . . . . ?
C14B C15B C16B C3B 178.0(7) . . . . ?
C14B C15B C16B C11B -0.7(10) . . . . ?
C10B C11B C16B C3B 0.1(10) . . . . ?
C12B C11B C16B C3B -178.1(6) . . . . ?
C10B C11B C16B C15B 178.9(6) . . . . ?
C12B C11B C16B C15B 0.7(10) . . . . ?
C14C C15C C16C C3C -179.2(9) . . . . ?
C14C C15C C16C C4C -0.8(15) . . . 2_567 ?
C4C C3C C16C C15C 177.4(9) . . . . ?
C1C C3C C16C C15C -0.2(13) . . . . ?
C4C C3C C16C C4C -1.1(13) . . . 2_567 ?
C1C C3C C16C C4C -178.6(7) . . . 2_567 ?
O1J C068 N2J C081 -5.3(13) . . . . ?
O1J C068 N2J C084 -179.5(9) . . . . ?
O1D C2D N3D C4D 7.9(19) . . . . ?
O1D C2D N3D C5D -172.2(12) . . . . ?
O1F C2F N3F C5F -179.3(9) . . . . ?
O1F C2F N3F C4F 0.3(15) . . . . ?
O1G C2G N3G C4G 4(3) . . . . ?
O1G C2G N3G C5G 164.3(19) . . . . ?
O1Z C2Z N3Z C5Z 168.2(13) . . . . ?
O1Z C2Z N3Z C4Z -4.4(16) . . . . ?
O2A C1A O1A Yb2 -28.1(11) . . . . ?
C3A C1A O1A Yb2 153.1(5) . . . . ?
O2B C1B O1B Yb1 1.9(7) . . . . ?
C3B C1B O1B Yb1 179.9(5) . . . . ?
O2C C1C O1C Yb2 3.5(9) . . . . ?
C3C C1C O1C Yb2 179.2(8) . . . . ?
N3D C2D O1D Yb1 -166.2(7) . . . . ?
N3F C2F O1F Yb2 -177.0(7) . . . . ?
N3G C2G O1G Yb3 -155.7(14) . . . . ?
N2J C068 O1J Yb2 144.5(6) . . . . ?
O3N N1N O1N Yb1 -165.8(8) . . . . ?
O2N N1N O1N Yb1 11.6(8) . . . . ?
N3Z C2Z O1Z Yb1 -164.7(8) . . . . ?
O1A C1A O2A Yb1 -51.5(12) . . . . ?
C3A C1A O2A Yb1 127.2(8) . . . . ?
O1B C1B O2B Yb1 -1.8(7) . . . . ?
C3B C1B O2B Yb1 -179.7(6) . . . . ?
O1C C1C O2C Yb2 -3.5(9) . . . . ?
C3C C1C O2C Yb2 -179.3(7) . . . . ?
O3N N1N O2N Yb1 165.7(8) . . . . ?
O1N N1N O2N Yb1 -11.6(8) . . . . ?
O4A C2A O3A Yb3 9.2(16) . . . . ?
C10A C2A O3A Yb3 -170.0(6) . . . . ?
O4B C2B O3B Yb3 6.5(8) . . . . ?
C10B C2B O3B Yb3 -173.6(5) 2_656 . . . ?
O4C C2C O3C Yb2 68.6(12) . . . . ?
C10C C2C O3C Yb2 -112.8(8) . . . . ?
O3A C2A O4A Yb3 74.0(15) . . . 2_657 ?
C10A C2A O4A Yb3 -106.8(10) . . . 2_657 ?
O3B C2B O4B Yb3 -6.3(7) . . . . ?
C10B C2B O4B Yb3 173.9(5) 2_656 . . . ?
O3C C2C O4C Yb1 2.9(14) . . . . ?
C10C C2C O4C Yb1 -175.8(6) . . . . ?
O6N N2N O4N Yb2 173.4(8) . . . . ?
O5N N2N O4N Yb2 -7.8(7) . . . . ?
O6N N2N O5N Yb2 -173.4(8) . . . . ?
O4N N2N O5N Yb2 7.8(7) . . . . ?
O9NB N3NB O7NB Yb3 -170(2) . . . . ?
O8NB N3NB O7NB Yb3 9(2) . . . . ?
O9NB N3NB O8NB Yb3 170(2) . . . . ?
O7NB N3NB O8NB Yb3 -9(2) . . . . ?
Yb3 O1XB C1 N4 163.2(17) . . . . ?
O1XB C1 N4 C1AA -8(4) . . . . ?
O1XB C1 N4 C0AA -179(2) . . . . ?
C3 N1 C2 O1XA 167.7(19) . . . . ?
C5 N1 C2 O1XA -6(3) . . . . ?
N1 C2 O1XA Yb3 170.8(13) . . . . ?
O9NA N3NA O8NA Yb3 165.5(16) . . . . ?
O7NA N3NA O8NA Yb3 -5.2(16) . . . . ?
O9NA N3NA O7NA Yb3 -165.6(17) . . . . ?
O8NA N3NA O7NA Yb3 5.1(16) . . . . ?

_refine_diff_density_max         2.695
_refine_diff_density_min         -4.807
_refine_diff_density_rms         0.232

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 0.090 0.910 0.875 9 2 ' '
2 0.345 0.755 0.224 138 16 ' '
3 0.201 0.311 0.155 11 1 ' '
4 0.655 0.245 0.776 138 16 ' '
5 0.500 0.500 0.500 14 2 ' '
6 0.799 0.689 0.845 11 1 ' '
7 0.910 0.090 0.125 9 2 ' '
_platon_squeeze_details          
;
;

# start Validation Reply Form
_vrf_PLAT213_Comp7_Yb            
;
PROBLEM: Atom O3N             has ADP max/min Ratio .....        4.4 prolat
RESPONSE: Crystal structure possesses some disorder problems in nitrate 
anions and DMF molecules. We have used RIGU in come atoms to model these
 molecules.
;
_vrf_PLAT220_Comp7_Yb            
;
PROBLEM: Large Non-Solvent  C     Ueq(max)/Ueq(min) Range        8.5 Ratio 
RESPONSE: Crystal structure possesses some disorder problems. Usually, too 
high Ueq's may be an indication for incorrectly  identified atomic species,
but we have correctly identified all the atomic species.
;
_vrf_PLAT230_Comp7_Yb            
;
PROBLEM: Hirshfeld Test Diff for    O1F    --  C2F     ..        7.1 su
RESPONSE: Large differences might indicate contamination of these parameters
with disorder in this F DMF molecule.
;
_vrf_PLAT242_Comp7_Yb            
;
PROBLEM: Low       Ueq as Compared to Neighbors for .....        N3D Check
RESPONSE: Large differences may indicate that the wrong atom type was 
assigned. In this case, false alarms may occur for terminal groups such as
this D DMF molecule.
;
_vrf_PLAT413_Comp7_Yb            
;
PROBLEM: Short Inter XH3 .. XHn     H5E    ..  H4GB    ..       1.94 Ang
RESPONSE: Crystal structure possesses some disorder problems in nitrate 
anions and DMF molecules, and this short distance is one of the consequences
of these problems.
;
# end Validation Reply Form


_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_Comp1_Pr
_database_code_depnum_ccdc_archive 'CCDC 1421047'
_audit_update_record             
;
2015-11-10 deposited with the CCDC.
2015-11-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H33 N3 O9 Pr'
_chemical_formula_weight         756.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4477(6)
_cell_length_b                   11.4945(7)
_cell_length_c                   12.9583(7)
_cell_angle_alpha                106.639(2)
_cell_angle_beta                 90.322(2)
_cell_angle_gamma                93.194(2)
_cell_volume                     1488.32(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6354
_cell_measurement_theta_min      2.564
_cell_measurement_theta_max      27.559

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_F_000             766
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    1.700
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'

_exptl_special_details           
;
Crystal structure have some disorder problems. The crystal structure contains a percentage of voids occupied by disordered solvent molecules. We have used SQUEEZE routine to eliminate one crystallization DMF molecule.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21270
_diffrn_reflns_av_unetI/netI     0.1108
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.522
_diffrn_reflns_theta_max         28.797
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             7493
_reflns_number_gt                5643
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker ApexII'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        'Bruker Apex II'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ViewerLite 5.0 (Acccelrys)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_refine_special_details          
;
Crystal structure have some disorder problems. The crystal structure 
contains a percentage of voids occupied by disordered solvent 
molecules. We have used SQUEZZE routine to eliminate one 
crystallization DMF molecule.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0437P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7493
_refine_ls_number_parameters     413
_refine_ls_number_restraints     102
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.1027
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.47424(2) 0.45386(2) 0.33549(2) 0.01057(8) Uani 1 1 d . . . . .
C1A C 0.4934(4) 0.2316(4) 0.1659(4) 0.0181(10) Uani 1 1 d . . . . .
C1B C 0.5125(4) 0.7480(4) 0.5046(4) 0.0140(9) Uani 1 1 d . U . . .
C1C C 0.2642(4) 0.4890(4) 0.5666(4) 0.0142(10) Uani 1 1 d . . . . .
C2A C 0.4982(5) 0.1133(4) 0.0821(4) 0.0226(11) Uani 1 1 d . . . . .
C2B C 0.5069(4) 0.8798(4) 0.5048(4) 0.0131(9) Uani 1 1 d . U . . .
C2C C 0.1287(4) 0.4932(5) 0.5319(4) 0.0212(11) Uani 1 1 d . . . . .
C2D C 0.5852(5) 0.6353(6) 0.1918(5) 0.0386(15) Uani 1 1 d . . . . .
H2D H 0.5726 0.6959 0.2554 0.046 Uiso 1 1 calc R U . . .
C3A C 0.4474(5) 0.0053(5) 0.1012(5) 0.0286(13) Uani 1 1 d . . . . .
C3B C 0.3913(4) 0.9362(4) 0.5263(4) 0.0198(11) Uani 1 1 d . U . . .
C3C C 0.0754(4) 0.4042(5) 0.4428(4) 0.0239(12) Uani 1 1 d . . . . .
C4A C 0.3963(5) 0.0036(5) 0.2044(5) 0.0334(14) Uani 1 1 d . . . . .
H4A H 0.3973 0.0757 0.2600 0.040 Uiso 1 1 calc R U . . .
C4B C 0.2776(5) 0.8760(6) 0.5509(7) 0.058(2) Uani 1 1 d . U . . .
H4B H 0.2797 0.7961 0.5536 0.070 Uiso 1 1 calc R U . . .
C4C C 0.1468(5) 0.3064(5) 0.3834(5) 0.0311(13) Uani 1 1 d . . . . .
H4C H 0.2311 0.3016 0.4046 0.037 Uiso 1 1 calc R U . . .
C4D C 0.6856(6) 0.5787(7) 0.0213(6) 0.060(2) Uani 1 1 d . . . . .
H4DA H 0.6569 0.4988 0.0242 0.091 Uiso 1 1 d R U . . .
H4DB H 0.7762 0.5809 0.0092 0.091 Uiso 1 1 d R U . . .
H4DC H 0.6415 0.5972 -0.0369 0.091 Uiso 1 1 d R U . . .
C5A C 0.3473(7) -0.0997(5) 0.2219(5) 0.0487(18) Uani 1 1 d . . . . .
H5A H 0.3147 -0.0975 0.2890 0.058 Uiso 1 1 calc R U . . .
C5B C 0.1676(6) 0.9325(7) 0.5702(9) 0.103(4) Uani 1 1 d . U . . .
H5B H 0.0942 0.8911 0.5850 0.124 Uiso 1 1 calc R U . . .
C5C C 0.0950(5) 0.2197(5) 0.2963(5) 0.0414(17) Uani 1 1 d . . . . .
H5C H 0.1439 0.1569 0.2582 0.050 Uiso 1 1 calc R U . . .
C5D C 0.7123(8) 0.7911(7) 0.1399(8) 0.087(3) Uani 1 1 d . . . . .
H5DA H 0.6844 0.8406 0.2083 0.131 Uiso 1 1 d R U . . .
H5DB H 0.6839 0.8240 0.0838 0.131 Uiso 1 1 d R U . . .
H5DC H 0.8046 0.7921 0.1406 0.131 Uiso 1 1 d R U . . .
C6A C 0.3449(6) -0.2115(5) 0.1395(5) 0.0473(17) Uani 1 1 d . . . . .
H6A H 0.3110 -0.2821 0.1530 0.057 Uiso 1 1 calc R U . . .
C6B C 0.1619(6) 1.0553(7) 0.5682(10) 0.110(4) Uani 1 1 d . U . . .
H6B H 0.0860 1.0946 0.5846 0.132 Uiso 1 1 calc R U . . .
C6C C -0.0353(5) 0.2251(5) 0.2633(5) 0.0432(17) Uani 1 1 d . . . . .
H6C H -0.0707 0.1656 0.2039 0.052 Uiso 1 1 calc R U . . .
C7A C 0.3921(6) -0.2164(5) 0.0400(5) 0.0388(15) Uani 1 1 d . . . . .
H7A H 0.3890 -0.2903 -0.0136 0.047 Uiso 1 1 calc R U . . .
C7B C 0.2660(5) 1.1148(5) 0.5427(7) 0.056(2) Uani 1 1 d . U . . .
H7B H 0.2600 1.1941 0.5394 0.067 Uiso 1 1 calc R U . . .
C7C C -0.1069(5) 0.3160(5) 0.3179(5) 0.0321(14) Uani 1 1 d . . . . .
H7C H -0.1913 0.3177 0.2956 0.038 Uiso 1 1 calc R U . . .
C8A C 0.4467(5) -0.1084(4) 0.0172(4) 0.0275(12) Uani 1 1 d . . . . .
C8B C 0.3854(4) 1.0590(4) 0.5205(4) 0.0208(11) Uani 1 1 d . U . . .
C8C C -0.0557(4) 0.4100(5) 0.4096(4) 0.0249(12) Uani 1 1 d . . . . .
N3D N 0.6586(5) 0.6651(5) 0.1203(5) 0.0489(15) Uani 1 1 d . . . . .
O1A O 0.3854(3) 0.2775(3) 0.1846(3) 0.0212(8) Uani 1 1 d . . . . .
O1B O 0.4897(3) 0.6716(3) 0.4144(3) 0.0194(7) Uani 1 1 d . U . . .
O1C O 0.3546(3) 0.5099(3) 0.5077(3) 0.0158(7) Uani 1 1 d . . . . .
O1D O 0.5309(3) 0.5334(3) 0.1822(3) 0.0246(8) Uani 1 1 d . . . . .
O1E O 0.2674(3) 0.5151(3) 0.2836(3) 0.0232(8) Uani 1 1 d . . . . .
O2A O 0.5951(3) 0.2838(3) 0.2138(3) 0.0216(8) Uani 1 1 d . . . . .
O2B O 0.5388(3) 0.7261(3) 0.5904(3) 0.0189(7) Uani 1 1 d . U . . .
O2C O 0.7153(3) 0.5257(3) 0.3440(3) 0.0223(8) Uani 1 1 d . . . . .
C2 C 0.1742(7) 0.4791(9) 0.2271(7) 0.0309(16) Uani 0.635(7) 1 d . U P A 1
H2 H 0.1735 0.4005 0.1810 0.037 Uiso 0.635(7) 1 calc R U P A 1
C5 C 0.2013(14) 0.5955(16) 0.3168(15) 0.039(3) Uani 0.365(7) 1 d . U P A 2
H5 H 0.2323 0.6539 0.3788 0.046 Uiso 0.365(7) 1 calc R U P A 2
C3AA C -0.0357(9) 0.4876(10) 0.1475(9) 0.050(2) Uani 0.635(7) 1 d . U P A 1
H3AA H -0.0429 0.5340 0.0969 0.074 Uiso 0.635(7) 1 calc R U P A 1
H3AB H -0.1140 0.4895 0.1862 0.074 Uiso 0.635(7) 1 calc R U P A 1
H3AC H -0.0202 0.4050 0.1095 0.074 Uiso 0.635(7) 1 calc R U P A 1
N2B N 0.0722(8) 0.5408(10) 0.2243(8) 0.0368(17) Uani 0.635(7) 1 d . U P A 1
C1AA C 0.0152(16) 0.7128(18) 0.3297(16) 0.049(3) Uani 0.365(7) 1 d . U P A 2
H1AA H -0.0678 0.6809 0.3435 0.074 Uiso 0.365(7) 1 calc R U P A 2
H1AB H 0.0059 0.7626 0.2823 0.074 Uiso 0.365(7) 1 calc R U P A 2
H1AC H 0.0551 0.7608 0.3963 0.074 Uiso 0.365(7) 1 calc R U P A 2
N2A N 0.0920(15) 0.6159(19) 0.2811(16) 0.046(2) Uani 0.365(7) 1 d . U P A 2
C0AA C 0.0616(11) 0.6583(11) 0.2945(9) 0.046(2) Uani 0.635(7) 1 d . U P A 1
H0AA H 0.1361 0.6807 0.3412 0.069 Uiso 0.635(7) 1 calc R U P A 1
H0AB H -0.0135 0.6593 0.3369 0.069 Uiso 0.635(7) 1 calc R U P A 1
H0AC H 0.0551 0.7152 0.2533 0.069 Uiso 0.635(7) 1 calc R U P A 1
C2AA C 0.0358(19) 0.532(2) 0.189(2) 0.056(4) Uani 0.365(7) 1 d . U P A 2
H2AA H 0.0758 0.5433 0.1261 0.084 Uiso 0.365(7) 1 calc R U P A 2
H2AB H -0.0541 0.5442 0.1862 0.084 Uiso 0.365(7) 1 calc R U P A 2
H2AC H 0.0472 0.4509 0.1928 0.084 Uiso 0.365(7) 1 calc R U P A 2


_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 O1B 2.413(3) . ?
Pr1 O1E 2.458(3) . ?
Pr1 O1D 2.475(3) . ?
Pr1 O1C 2.501(3) . ?
Pr1 O1A 2.509(3) . ?
Pr1 O2B 2.516(3) 2_666 ?
Pr1 O2A 2.537(3) . ?
Pr1 O2C 2.598(3) . ?
Pr1 O1C 2.625(3) 2_666 ?
Pr1 C1A 2.871(5) . ?
Pr1 C1C 2.965(4) 2_666 ?
Pr1 Pr1 4.1125(6) 2_666 ?
C1A O2A 1.259(6) . ?
C1A O1A 1.267(5) . ?
C1A C2A 1.481(6) . ?
C1B O2B 1.241(6) . ?
C1B O1B 1.257(5) . ?
C1B C2B 1.518(6) . ?
C1C O2C 1.237(6) 2_666 ?
C1C O1C 1.273(5) . ?
C1C C2C 1.491(6) . ?
C1C Pr1 2.965(4) 2_666 ?
C2A C8A 1.400(7) 2_655 ?
C2A C3A 1.409(7) . ?
C2B C8B 1.385(6) 2_676 ?
C2B C3B 1.394(6) . ?
C2C C3C 1.394(7) . ?
C2C C8C 1.418(7) 2_566 ?
C2D O1D 1.246(6) . ?
C2D N3D 1.313(7) . ?
C2D H2D 0.9300 . ?
C3A C8A 1.441(7) . ?
C3A C4A 1.448(8) . ?
C3B C4B 1.425(7) . ?
C3B C8B 1.440(6) . ?
C3C C4C 1.420(7) . ?
C3C C8C 1.444(7) . ?
C4A C5A 1.345(8) . ?
C4A H4A 0.9300 . ?
C4B C5B 1.341(8) . ?
C4B H4B 0.9300 . ?
C4C C5C 1.361(8) . ?
C4C H4C 0.9300 . ?
C4D N3D 1.420(9) . ?
C4D H4DA 0.9611 . ?
C4D H4DB 0.9609 . ?
C4D H4DC 0.9614 . ?
C5A C6A 1.415(8) . ?
C5A H5A 0.9300 . ?
C5B C6B 1.424(9) . ?
C5B H5B 0.9300 . ?
C5C C6C 1.435(7) . ?
C5C H5C 0.9300 . ?
C5D N3D 1.474(9) . ?
C5D H5DA 0.9630 . ?
C5D H5DB 0.9627 . ?
C5D H5DC 0.9634 . ?
C6A C7A 1.371(8) . ?
C6A H6A 0.9300 . ?
C6B C7B 1.345(8) . ?
C6B H6B 0.9300 . ?
C6C C7C 1.349(7) . ?
C6C H6C 0.9300 . ?
C7A C8A 1.445(7) . ?
C7A H7A 0.9300 . ?
C7B C8B 1.427(7) . ?
C7B H7B 0.9300 . ?
C7C C8C 1.435(7) . ?
C7C H7C 0.9300 . ?
C8A C2A 1.400(7) 2_655 ?
C8B C2B 1.385(6) 2_676 ?
C8C C2C 1.418(7) 2_566 ?
O1C Pr1 2.625(3) 2_666 ?
O1E C5 1.168(16) . ?
O1E C2 1.196(9) . ?
O2B Pr1 2.516(3) 2_666 ?
O2C C1C 1.237(6) 2_666 ?
C2 N2B 1.318(11) . ?
C2 H2 0.9300 . ?
C5 N2A 1.29(2) . ?
C5 H5 0.9300 . ?
C3AA N2B 1.482(13) . ?
C3AA H3AA 0.9600 . ?
C3AA H3AB 0.9600 . ?
C3AA H3AC 0.9600 . ?
N2B C0AA 1.407(15) . ?
C1AA N2A 1.41(2) . ?
C1AA H1AA 0.9600 . ?
C1AA H1AB 0.9600 . ?
C1AA H1AC 0.9600 . ?
N2A C2AA 1.40(3) . ?
C0AA H0AA 0.9600 . ?
C0AA H0AB 0.9600 . ?
C0AA H0AC 0.9600 . ?
C2AA H2AA 0.9600 . ?
C2AA H2AB 0.9600 . ?
C2AA H2AC 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1B Pr1 O1E 77.25(11) . . ?
O1B Pr1 O1D 76.29(11) . . ?
O1E Pr1 O1D 77.27(11) . . ?
O1B Pr1 O1C 69.87(10) . . ?
O1E Pr1 O1C 76.12(11) . . ?
O1D Pr1 O1C 140.59(10) . . ?
O1B Pr1 O1A 146.92(11) . . ?
O1E Pr1 O1A 74.36(11) . . ?
O1D Pr1 O1A 81.19(11) . . ?
O1C Pr1 O1A 118.19(10) . . ?
O1B Pr1 O2B 134.61(11) . 2_666 ?
O1E Pr1 O2B 115.20(11) . 2_666 ?
O1D Pr1 O2B 147.25(11) . 2_666 ?
O1C Pr1 O2B 71.51(10) . 2_666 ?
O1A Pr1 O2B 74.16(11) . 2_666 ?
O1B Pr1 O2A 141.09(11) . . ?
O1E Pr1 O2A 123.07(11) . . ?
O1D Pr1 O2A 76.98(11) . . ?
O1C Pr1 O2A 142.36(11) . . ?
O1A Pr1 O2A 52.07(10) . . ?
O2B Pr1 O2A 70.93(11) 2_666 . ?
O1B Pr1 O2C 72.45(11) . . ?
O1E Pr1 O2C 138.56(11) . . ?
O1D Pr1 O2C 68.64(11) . . ?
O1C Pr1 O2C 117.32(10) . . ?
O1A Pr1 O2C 120.86(11) . . ?
O2B Pr1 O2C 106.20(10) 2_666 . ?
O2A Pr1 O2C 71.73(10) . . ?
O1B Pr1 O1C 75.69(10) . 2_666 ?
O1E Pr1 O1C 144.54(10) . 2_666 ?
O1D Pr1 O1C 117.32(10) . 2_666 ?
O1C Pr1 O1C 73.32(10) . 2_666 ?
O1A Pr1 O1C 136.93(10) . 2_666 ?
O2B Pr1 O1C 71.13(10) 2_666 2_666 ?
O2A Pr1 O1C 92.30(10) . 2_666 ?
O2C Pr1 O1C 49.74(10) . 2_666 ?
O1B Pr1 C1A 155.22(13) . . ?
O1E Pr1 C1A 99.31(12) . . ?
O1D Pr1 C1A 79.02(12) . . ?
O1C Pr1 C1A 133.73(12) . . ?
O1A Pr1 C1A 26.14(11) . . ?
O2B Pr1 C1A 69.32(12) 2_666 . ?
O2A Pr1 C1A 25.98(11) . . ?
O2C Pr1 C1A 96.67(12) . . ?
O1C Pr1 C1A 114.74(11) 2_666 . ?
O1B Pr1 C1C 74.80(11) . 2_666 ?
O1E Pr1 C1C 151.88(11) . 2_666 ?
O1D Pr1 C1C 93.07(12) . 2_666 ?
O1C Pr1 C1C 96.92(12) . 2_666 ?
O1A Pr1 C1C 130.82(11) . 2_666 ?
O2B Pr1 C1C 87.19(11) 2_666 2_666 ?
O2A Pr1 C1C 78.95(11) . 2_666 ?
O2C Pr1 C1C 24.57(11) . 2_666 ?
O1C Pr1 C1C 25.40(11) 2_666 2_666 ?
C1A Pr1 C1C 104.72(13) . 2_666 ?
O1B Pr1 Pr1 68.47(8) . 2_666 ?
O1E Pr1 Pr1 111.96(8) . 2_666 ?
O1D Pr1 Pr1 139.72(8) . 2_666 ?
O1C Pr1 Pr1 37.69(7) . 2_666 ?
O1A Pr1 Pr1 138.90(8) . 2_666 ?
O2B Pr1 Pr1 66.47(7) 2_666 2_666 ?
O2A Pr1 Pr1 120.48(8) . 2_666 ?
O2C Pr1 Pr1 82.34(8) . 2_666 ?
O1C Pr1 Pr1 35.63(6) 2_666 2_666 ?
C1A Pr1 Pr1 133.43(10) . 2_666 ?
C1C Pr1 Pr1 59.78(9) 2_666 2_666 ?
O2A C1A O1A 122.6(4) . . ?
O2A C1A C2A 119.7(4) . . ?
O1A C1A C2A 117.7(4) . . ?
O2A C1A Pr1 62.0(2) . . ?
O1A C1A Pr1 60.8(2) . . ?
C2A C1A Pr1 176.6(4) . . ?
O2B C1B O1B 126.8(4) . . ?
O2B C1B C2B 118.5(4) . . ?
O1B C1B C2B 114.6(4) . . ?
O2C C1C O1C 122.1(4) 2_666 . ?
O2C C1C C2C 118.3(4) 2_666 . ?
O1C C1C C2C 119.3(4) . . ?
O2C C1C Pr1 60.8(2) 2_666 2_666 ?
O1C C1C Pr1 62.2(2) . 2_666 ?
C2C C1C Pr1 165.5(3) . 2_666 ?
C8A C2A C3A 119.5(4) 2_655 . ?
C8A C2A C1A 119.8(4) 2_655 . ?
C3A C2A C1A 120.6(5) . . ?
C8B C2B C3B 120.8(4) 2_676 . ?
C8B C2B C1B 119.9(4) 2_676 . ?
C3B C2B C1B 119.3(4) . . ?
C3C C2C C8C 120.7(4) . 2_566 ?
C3C C2C C1C 120.4(4) . . ?
C8C C2C C1C 118.8(4) 2_566 . ?
O1D C2D N3D 126.0(6) . . ?
O1D C2D H2D 117.0 . . ?
N3D C2D H2D 117.0 . . ?
C2A C3A C8A 120.1(5) . . ?
C2A C3A C4A 122.0(5) . . ?
C8A C3A C4A 117.8(5) . . ?
C2B C3B C4B 122.7(4) . . ?
C2B C3B C8B 118.8(4) . . ?
C4B C3B C8B 118.5(4) . . ?
C2C C3C C4C 121.6(4) . . ?
C2C C3C C8C 119.8(4) . . ?
C4C C3C C8C 118.6(5) . . ?
C5A C4A C3A 121.8(5) . . ?
C5A C4A H4A 119.1 . . ?
C3A C4A H4A 119.1 . . ?
C5B C4B C3B 121.1(5) . . ?
C5B C4B H4B 119.4 . . ?
C3B C4B H4B 119.4 . . ?
C5C C4C C3C 121.6(5) . . ?
C5C C4C H4C 119.2 . . ?
C3C C4C H4C 119.2 . . ?
N3D C4D H4DA 109.2 . . ?
N3D C4D H4DB 110.0 . . ?
H4DA C4D H4DB 109.4 . . ?
N3D C4D H4DC 109.6 . . ?
H4DA C4D H4DC 109.4 . . ?
H4DB C4D H4DC 109.3 . . ?
C4A C5A C6A 120.8(6) . . ?
C4A C5A H5A 119.6 . . ?
C6A C5A H5A 119.6 . . ?
C4B C5B C6B 120.7(6) . . ?
C4B C5B H5B 119.6 . . ?
C6B C5B H5B 119.6 . . ?
C4C C5C C6C 119.9(5) . . ?
C4C C5C H5C 120.1 . . ?
C6C C5C H5C 120.1 . . ?
N3D C5D H5DA 109.8 . . ?
N3D C5D H5DB 109.9 . . ?
H5DA C5D H5DB 109.1 . . ?
N3D C5D H5DC 109.6 . . ?
H5DA C5D H5DC 109.3 . . ?
H5DB C5D H5DC 109.1 . . ?
C7A C6A C5A 120.5(5) . . ?
C7A C6A H6A 119.8 . . ?
C5A C6A H6A 119.8 . . ?
C7B C6B C5B 120.2(6) . . ?
C7B C6B H6B 119.9 . . ?
C5B C6B H6B 119.9 . . ?
C7C C6C C5C 120.5(5) . . ?
C7C C6C H6C 119.8 . . ?
C5C C6C H6C 119.8 . . ?
C6A C7A C8A 121.0(5) . . ?
C6A C7A H7A 119.5 . . ?
C8A C7A H7A 119.5 . . ?
C6B C7B C8B 121.5(5) . . ?
C6B C7B H7B 119.2 . . ?
C8B C7B H7B 119.2 . . ?
C6C C7C C8C 121.5(5) . . ?
C6C C7C H7C 119.2 . . ?
C8C C7C H7C 119.2 . . ?
C2A C8A C3A 120.3(5) 2_655 . ?
C2A C8A C7A 121.6(5) 2_655 . ?
C3A C8A C7A 118.1(5) . . ?
C2B C8B C7B 121.8(4) 2_676 . ?
C2B C8B C3B 120.4(4) 2_676 . ?
C7B C8B C3B 117.8(4) . . ?
C2C C8C C7C 122.7(4) 2_566 . ?
C2C C8C C3C 119.4(5) 2_566 . ?
C7C C8C C3C 117.9(4) . . ?
C2D N3D C4D 121.4(6) . . ?
C2D N3D C5D 120.4(7) . . ?
C4D N3D C5D 118.2(6) . . ?
C1A O1A Pr1 93.1(3) . . ?
C1B O1B Pr1 139.1(3) . . ?
C1C O1C Pr1 150.7(3) . . ?
C1C O1C Pr1 92.4(3) . 2_666 ?
Pr1 O1C Pr1 106.68(10) . 2_666 ?
C2D O1D Pr1 124.2(4) . . ?
C5 O1E Pr1 136.6(9) . . ?
C2 O1E Pr1 143.1(5) . . ?
C1A O2A Pr1 92.0(3) . . ?
C1B O2B Pr1 137.7(3) . 2_666 ?
C1C O2C Pr1 94.6(3) 2_666 . ?
O1E C2 N2B 126.0(10) . . ?
O1E C2 H2 117.0 . . ?
N2B C2 H2 117.0 . . ?
O1E C5 N2A 130.1(19) . . ?
O1E C5 H5 114.9 . . ?
N2A C5 H5 114.9 . . ?
N2B C3AA H3AA 109.5 . . ?
N2B C3AA H3AB 109.5 . . ?
H3AA C3AA H3AB 109.5 . . ?
N2B C3AA H3AC 109.5 . . ?
H3AA C3AA H3AC 109.5 . . ?
H3AB C3AA H3AC 109.5 . . ?
C2 N2B C0AA 121.2(10) . . ?
C2 N2B C3AA 120.9(10) . . ?
C0AA N2B C3AA 117.9(8) . . ?
N2A C1AA H1AA 109.5 . . ?
N2A C1AA H1AB 109.5 . . ?
H1AA C1AA H1AB 109.5 . . ?
N2A C1AA H1AC 109.5 . . ?
H1AA C1AA H1AC 109.5 . . ?
H1AB C1AA H1AC 109.5 . . ?
C5 N2A C2AA 119(2) . . ?
C5 N2A C1AA 126(2) . . ?
C2AA N2A C1AA 114.2(15) . . ?
N2B C0AA H0AA 109.5 . . ?
N2B C0AA H0AB 109.5 . . ?
H0AA C0AA H0AB 109.5 . . ?
N2B C0AA H0AC 109.5 . . ?
H0AA C0AA H0AC 109.5 . . ?
H0AB C0AA H0AC 109.5 . . ?
N2A C2AA H2AA 109.5 . . ?
N2A C2AA H2AB 109.5 . . ?
H2AA C2AA H2AB 109.5 . . ?
N2A C2AA H2AC 109.5 . . ?
H2AA C2AA H2AC 109.5 . . ?
H2AB C2AA H2AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2A C1A C2A C8A -70.9(7) . . . 2_655 ?
O1A C1A C2A C8A 107.6(6) . . . 2_655 ?
O2A C1A C2A C3A 109.3(6) . . . . ?
O1A C1A C2A C3A -72.3(6) . . . . ?
O2B C1B C2B C8B 93.2(6) . . . 2_676 ?
O1B C1B C2B C8B -86.6(5) . . . 2_676 ?
O2B C1B C2B C3B -89.4(5) . . . . ?
O1B C1B C2B C3B 90.9(5) . . . . ?
O2C C1C C2C C3C -116.0(5) 2_666 . . . ?
O1C C1C C2C C3C 69.3(6) . . . . ?
Pr1 C1C C2C C3C 161.2(11) 2_666 . . . ?
O2C C1C C2C C8C 64.7(6) 2_666 . . 2_566 ?
O1C C1C C2C C8C -110.0(5) . . . 2_566 ?
Pr1 C1C C2C C8C -18.1(16) 2_666 . . 2_566 ?
C8A C2A C3A C8A -3.0(9) 2_655 . . . ?
C1A C2A C3A C8A 176.8(5) . . . . ?
C8A C2A C3A C4A 176.2(5) 2_655 . . . ?
C1A C2A C3A C4A -4.0(8) . . . . ?
C8B C2B C3B C4B 178.9(6) 2_676 . . . ?
C1B C2B C3B C4B 1.5(8) . . . . ?
C8B C2B C3B C8B 0.8(8) 2_676 . . . ?
C1B C2B C3B C8B -176.7(5) . . . . ?
C8C C2C C3C C4C -179.8(5) 2_566 . . . ?
C1C C2C C3C C4C 0.9(8) . . . . ?
C8C C2C C3C C8C -0.3(9) 2_566 . . . ?
C1C C2C C3C C8C -179.5(4) . . . . ?
C2A C3A C4A C5A 179.7(6) . . . . ?
C8A C3A C4A C5A -1.2(9) . . . . ?
C2B C3B C4B C5B -179.3(8) . . . . ?
C8B C3B C4B C5B -1.2(11) . . . . ?
C2C C3C C4C C5C -179.9(6) . . . . ?
C8C C3C C4C C5C 0.6(9) . . . . ?
C3A C4A C5A C6A 0.5(10) . . . . ?
C3B C4B C5B C6B -1.0(16) . . . . ?
C3C C4C C5C C6C -0.7(10) . . . . ?
C4A C5A C6A C7A -0.2(11) . . . . ?
C4B C5B C6B C7B 2.7(18) . . . . ?
C4C C5C C6C C7C 0.2(11) . . . . ?
C5A C6A C7A C8A 0.8(10) . . . . ?
C5B C6B C7B C8B -2.1(16) . . . . ?
C5C C6C C7C C8C 0.4(10) . . . . ?
C2A C3A C8A C2A 3.0(9) . . . 2_655 ?
C4A C3A C8A C2A -176.2(5) . . . 2_655 ?
C2A C3A C8A C7A -179.2(5) . . . . ?
C4A C3A C8A C7A 1.6(8) . . . . ?
C6A C7A C8A C2A 176.3(6) . . . 2_655 ?
C6A C7A C8A C3A -1.5(9) . . . . ?
C6B C7B C8B C2B -179.3(8) . . . 2_676 ?
C6B C7B C8B C3B 0.0(11) . . . . ?
C2B C3B C8B C2B -0.8(8) . . . 2_676 ?
C4B C3B C8B C2B -179.0(6) . . . 2_676 ?
C2B C3B C8B C7B 179.9(6) . . . . ?
C4B C3B C8B C7B 1.6(9) . . . . ?
C6C C7C C8C C2C 179.7(6) . . . 2_566 ?
C6C C7C C8C C3C -0.5(9) . . . . ?
C2C C3C C8C C2C 0.3(8) . . . 2_566 ?
C4C C3C C8C C2C 179.8(5) . . . 2_566 ?
C2C C3C C8C C7C -179.6(5) . . . . ?
C4C C3C C8C C7C 0.0(8) . . . . ?
O1D C2D N3D C4D -1.1(10) . . . . ?
O1D C2D N3D C5D 177.2(6) . . . . ?
O2A C1A O1A Pr1 -5.1(5) . . . . ?
C2A C1A O1A Pr1 176.5(4) . . . . ?
O2B C1B O1B Pr1 0.9(7) . . . . ?
C2B C1B O1B Pr1 -179.3(3) . . . . ?
O2C C1C O1C Pr1 120.7(6) 2_666 . . . ?
C2C C1C O1C Pr1 -64.9(7) . . . . ?
Pr1 C1C O1C Pr1 131.5(6) 2_666 . . . ?
O2C C1C O1C Pr1 -10.8(4) 2_666 . . 2_666 ?
C2C C1C O1C Pr1 163.6(4) . . . 2_666 ?
N3D C2D O1D Pr1 152.7(5) . . . . ?
O1A C1A O2A Pr1 5.0(5) . . . . ?
C2A C1A O2A Pr1 -176.6(4) . . . . ?
O1B C1B O2B Pr1 -15.1(7) . . . 2_666 ?
C2B C1B O2B Pr1 165.2(3) . . . 2_666 ?
C5 O1E C2 N2B 6.3(11) . . . . ?
Pr1 O1E C2 N2B 176.2(6) . . . . ?
C2 O1E C5 N2A -8.1(17) . . . . ?
Pr1 O1E C5 N2A -179.2(12) . . . . ?
O1E C2 N2B C0AA -3.0(15) . . . . ?
O1E C2 N2B C3AA 177.6(9) . . . . ?
O1E C5 N2A C2AA 1(3) . . . . ?
O1E C5 N2A C1AA 176.5(16) . . . . ?

_refine_diff_density_max         1.073
_refine_diff_density_min         -1.638
_refine_diff_density_rms         0.183

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 0.000 0.000 0.000 237 13 ' '
_platon_squeeze_details          
;
;
# start Validation Reply Form
_vrf_CHEMW03_Comp1_Pr            
;
PROBLEM: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
RESPONSE: The crystal structure contains a percentage of voids occupied by
disordered solvent molecules. We have used SQUEEZE routine to eliminate
one crystallization DMF molecule.
;
_vrf_PLAT213_Comp1_Pr            
;
PROBLEM: Atom C6B             has ADP max/min Ratio .....        4.2 prolat
RESPONSE: Crystal structure possesses some disorder problems. We have used 
RIGU in C5B and C6B to model B anthracene ligand.
;
_vrf_PLAT220_Comp1_Pr            
;
PROBLEM: Large Non-Solvent  C     Ueq(max)/Ueq(min) Range        8.5 Ratio 
RESPONSE: Crystal structure possesses some disorder problems. Usually, too 
high Ueq's may be an indication for incorrectly  identified atomic species,
but we have correctly identified all the atomic species.
;
# end Validation Reply Form

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_Comp2_Nd
_database_code_depnum_ccdc_archive 'CCDC 1421048'
_audit_update_record             
;
2015-11-10 deposited with the CCDC.
2015-11-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H33 N3 Nd O9'
_chemical_formula_weight         759.86

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.471(5)
_cell_length_b                   11.359(5)
_cell_length_c                   13.093(6)
_cell_angle_alpha                107.541(5)
_cell_angle_beta                 90.084(6)
_cell_angle_gamma                92.355(6)
_cell_volume                     1483.5(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1465
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      18.44

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            White
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_F_000             768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    1.813
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'

_exptl_special_details           
;
Crystal structure have some disorder problems. The crystal structure contains a percentage of voids occupied by disordered solvent molecules. We have used SQUEEZE routine to eliminate one crystallization DMF molecule.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11612
_diffrn_reflns_av_unetI/netI     0.0905
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.631
_diffrn_reflns_theta_max         23.295
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.792
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.792
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.792
_reflns_number_total             4249
_reflns_number_gt                3449
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker ApexII'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        'Bruker Apex II'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ViewerLite 5.0 (Acccelrys)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0490P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4249
_refine_ls_number_parameters     374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.1076
_refine_ls_wR_factor_gt          0.1023
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.978
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.48068(4) 0.45342(3) 0.33946(3) 0.02640(15) Uani 1 1 d . . . . .
C1A C 0.4987(9) 0.2335(7) 0.1706(6) 0.044(2) Uani 1 1 d . . . . .
C1B C 0.5089(7) 0.7462(7) 0.5072(7) 0.041(2) Uani 1 1 d . . . . .
C1C C 0.2668(8) 0.4913(7) 0.5612(7) 0.042(2) Uani 1 1 d . . . . .
C2A C 0.4998(9) 0.1154(8) 0.0861(7) 0.053(2) Uani 1 1 d . . . . .
C2B C 0.5064(8) 0.8799(7) 0.5069(6) 0.042(2) Uani 1 1 d . . . . .
C2C C 0.1288(7) 0.4966(8) 0.5284(6) 0.045(2) Uani 1 1 d . . . . .
C2D C 0.5841(10) 0.6298(11) 0.1998(8) 0.077(3) Uani 1 1 d . . . . .
H2D H 0.5708 0.6920 0.2633 0.092 Uiso 1 1 calc R U . . .
C2E C 0.1904(13) 0.4823(12) 0.2352(10) 0.095(4) Uani 1 1 d . . . . .
H2E H 0.1911 0.4028 0.1876 0.114 Uiso 1 1 calc R U . . .
C3A C 0.4514(10) 0.0060(10) 0.1010(8) 0.075(3) Uani 1 1 d . . . . .
C3B C 0.3912(8) 0.9397(7) 0.5257(7) 0.046(2) Uani 1 1 d . . . . .
C3C C 0.0764(7) 0.4029(8) 0.4409(7) 0.047(2) Uani 1 1 d . . . . .
C4A C 0.4033(11) 0.0005(10) 0.2051(8) 0.086(3) Uani 1 1 d . . . . .
H4A H 0.4110 0.0712 0.2637 0.104 Uiso 1 1 calc R U . . .
C4B C 0.2769(9) 0.8831(9) 0.5525(9) 0.076(3) Uani 1 1 d . . . . .
H4B H 0.2792 0.8040 0.5592 0.091 Uiso 1 1 calc R U . . .
C4C C 0.1495(8) 0.3028(8) 0.3813(7) 0.061(3) Uani 1 1 d . . . . .
H4C H 0.2346 0.2990 0.4001 0.073 Uiso 1 1 calc R U . . .
C4D C 0.6799(12) 0.5642(13) 0.0250(10) 0.124(5) Uani 1 1 d . . . . .
H4D1 H 0.6791 0.4850 0.0373 0.187 Uiso 1 1 d R U . . .
H4D2 H 0.7617 0.5809 -0.0018 0.187 Uiso 1 1 d R U . . .
H4D3 H 0.6144 0.5638 -0.0266 0.187 Uiso 1 1 d R U . . .
C4E C 0.0695(16) 0.6668(15) 0.3086(12) 0.159(7) Uani 1 1 d . . . . .
H4E1 H 0.1398 0.6881 0.3590 0.239 Uiso 1 1 d R U . . .
H4E2 H -0.0089 0.6655 0.3463 0.239 Uiso 1 1 d R U . . .
H4E3 H 0.0661 0.7269 0.2707 0.239 Uiso 1 1 d R U . . .
C5A C 0.3486(15) -0.1032(11) 0.2187(10) 0.125(6) Uani 1 1 d . . . . .
H5A H 0.3135 -0.1007 0.2845 0.150 Uiso 1 1 calc R U . . .
C5B C 0.1655(11) 0.9417(10) 0.5685(12) 0.110(5) Uani 1 1 d . . . . .
H5B H 0.0918 0.9014 0.5832 0.133 Uiso 1 1 calc R U . . .
C5C C 0.0954(9) 0.2122(9) 0.2965(8) 0.079(3) Uani 1 1 d . . . . .
H5C H 0.1436 0.1467 0.2582 0.095 Uiso 1 1 calc R U . . .
C5D C 0.7068(14) 0.7851(13) 0.1418(12) 0.148(7) Uani 1 1 d . . . . .
H5D1 H 0.7064 0.8028 0.0745 0.222 Uiso 1 1 d R U . . .
H5D2 H 0.7929 0.7929 0.1691 0.222 Uiso 1 1 d R U . . .
H5D3 H 0.6550 0.8424 0.1919 0.222 Uiso 1 1 d R U . . .
C5E C -0.0134(15) 0.4888(16) 0.1566(11) 0.161(7) Uani 1 1 d . . . . .
H5E1 H 0.0075 0.4054 0.1196 0.242 Uiso 1 1 d R U . . .
H5E2 H -0.0214 0.5342 0.1060 0.242 Uiso 1 1 d R U . . .
H5E3 H -0.0928 0.4885 0.1931 0.242 Uiso 1 1 d R U . . .
C6A C 0.3439(14) -0.2169(11) 0.1336(10) 0.125(6) Uani 1 1 d . . . . .
H6A H 0.3091 -0.2889 0.1440 0.150 Uiso 1 1 calc R U . . .
C6B C 0.1604(10) 1.0627(11) 0.5631(12) 0.112(5) Uani 1 1 d . . . . .
H6B H 0.0832 1.1020 0.5737 0.134 Uiso 1 1 calc R U . . .
C6C C -0.0335(9) 0.2181(9) 0.2671(8) 0.076(3) Uani 1 1 d . . . . .
H6C H -0.0687 0.1573 0.2082 0.092 Uiso 1 1 calc R U . . .
C7A C 0.3919(12) -0.2173(10) 0.0362(9) 0.094(4) Uani 1 1 d . . . . .
H7A H 0.3883 -0.2915 -0.0190 0.113 Uiso 1 1 calc R U . . .
C7B C 0.2674(10) 1.1235(9) 0.5427(9) 0.075(3) Uani 1 1 d . . . . .
H7B H 0.2631 1.2051 0.5427 0.090 Uiso 1 1 calc R U . . .
C7C C -0.1069(9) 0.3108(9) 0.3231(7) 0.061(3) Uani 1 1 d . . . . .
H7C H -0.1923 0.3114 0.3037 0.074 Uiso 1 1 calc R U . . .
C8A C 0.4475(10) -0.1095(9) 0.0145(8) 0.074(3) Uani 1 1 d . . . . .
C8B C 0.3863(7) 1.0640(7) 0.5213(7) 0.045(2) Uani 1 1 d . . . . .
C8C C -0.0539(8) 0.4077(8) 0.4119(7) 0.047(2) Uani 1 1 d . . . . .
N3D N 0.6559(9) 0.6601(9) 0.1261(8) 0.089(3) Uani 1 1 d . . . . .
N3E N 0.0870(9) 0.5473(13) 0.2343(10) 0.104(4) Uani 1 1 d . . . . .
O1A O 0.3909(5) 0.2810(5) 0.1951(4) 0.0536(15) Uani 1 1 d . . . . .
O1B O 0.4929(5) 0.6670(5) 0.4159(4) 0.0460(14) Uani 1 1 d . . . . .
O1C O 0.3574(5) 0.5053(5) 0.5021(4) 0.0485(14) Uani 1 1 d . . . . .
O1D O 0.5344(6) 0.5278(6) 0.1912(5) 0.0620(17) Uani 1 1 d . . . . .
O1E O 0.2831(6) 0.5188(6) 0.2930(5) 0.069(2) Uani 1 1 d . . . . .
O2A O 0.5985(6) 0.2833(5) 0.2172(5) 0.0585(16) Uani 1 1 d . . . . .
O2B O 0.5277(6) 0.7242(5) 0.5928(4) 0.0501(15) Uani 1 1 d . . . . .
O2C O 0.7113(5) 0.5162(5) 0.3476(5) 0.0564(16) 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 O1B 2.327(5) . ?
Nd1 O1E 2.366(7) . ?
Nd1 O1D 2.398(6) . ?
Nd1 O1C 2.421(6) . ?
Nd1 O1A 2.430(5) . ?
Nd1 O2B 2.436(5) 2_666 ?
Nd1 O2A 2.481(5) . ?
Nd1 O2C 2.482(6) . ?
Nd1 O1C 2.595(5) 2_666 ?
Nd1 C1A 2.806(8) . ?
Nd1 C1C 2.905(8) 2_666 ?
Nd1 Nd1 4.029(2) 2_666 ?
C1A O2A 1.235(9) . ?
C1A O1A 1.271(9) . ?
C1A C2A 1.460(11) . ?
C1B O2B 1.236(9) . ?
C1B O1B 1.268(8) . ?
C1B C2B 1.522(10) . ?
C1C O2C 1.244(9) 2_666 ?
C1C O1C 1.261(9) . ?
C1C C2C 1.516(11) . ?
C1C Nd1 2.905(8) 2_666 ?
C2A C3A 1.391(12) . ?
C2A C8A 1.413(12) 2_655 ?
C2B C8B 1.374(10) 2_676 ?
C2B C3B 1.394(11) . ?
C2C C3C 1.401(11) . ?
C2C C8C 1.402(11) 2_566 ?
C2D O1D 1.224(11) . ?
C2D N3D 1.340(11) . ?
C2E O1E 1.209(13) . ?
C2E N3E 1.337(13) . ?
C3A C8A 1.452(13) . ?
C3A C4A 1.471(13) . ?
C3B C4B 1.429(11) . ?
C3B C8B 1.434(10) . ?
C3C C8C 1.423(11) . ?
C3C C4C 1.424(11) . ?
C4A C5A 1.349(14) . ?
C4B C5B 1.352(13) . ?
C4C C5C 1.370(12) . ?
C4D N3D 1.469(14) . ?
C4E N3E 1.431(17) . ?
C5A C6A 1.428(15) . ?
C5B C6B 1.401(14) . ?
C5C C6C 1.413(12) . ?
C5D N3D 1.451(14) . ?
C5E N3E 1.454(16) . ?
C6A C7A 1.370(14) . ?
C6B C7B 1.361(13) . ?
C6C C7C 1.357(12) . ?
C7A C8A 1.439(13) . ?
C7B C8B 1.428(11) . ?
C7C C8C 1.430(12) . ?
C8A C2A 1.413(12) 2_655 ?
C8B C2B 1.374(10) 2_676 ?
C8C C2C 1.402(11) 2_566 ?
O1C Nd1 2.595(5) 2_666 ?
O2B Nd1 2.436(5) 2_666 ?
O2C C1C 1.245(9) 2_666 ?

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
O1B Nd1 O1E 75.8(2) . . ?
O1B Nd1 O1D 76.71(19) . . ?
O1E Nd1 O1D 76.9(2) . . ?
O1B Nd1 O1C 71.50(18) . . ?
O1E Nd1 O1C 74.4(2) . . ?
O1D Nd1 O1C 141.3(2) . . ?
O1B Nd1 O1A 145.96(19) . . ?
O1E Nd1 O1A 74.3(2) . . ?
O1D Nd1 O1A 81.2(2) . . ?
O1C Nd1 O1A 114.65(19) . . ?
O1B Nd1 O2B 135.47(17) . 2_666 ?
O1E Nd1 O2B 116.7(2) . 2_666 ?
O1D Nd1 O2B 145.9(2) . 2_666 ?
O1C Nd1 O2B 71.73(18) . 2_666 ?
O1A Nd1 O2B 73.82(19) . 2_666 ?
O1B Nd1 O2A 141.11(19) . . ?
O1E Nd1 O2A 123.2(2) . . ?
O1D Nd1 O2A 75.9(2) . . ?
O1C Nd1 O2A 142.33(19) . . ?
O1A Nd1 O2A 52.97(19) . . ?
O2B Nd1 O2A 70.60(19) 2_666 . ?
O1B Nd1 O2C 73.86(19) . . ?
O1E Nd1 O2C 139.0(2) . . ?
O1D Nd1 O2C 69.8(2) . . ?
O1C Nd1 O2C 119.67(18) . . ?
O1A Nd1 O2C 121.72(19) . . ?
O2B Nd1 O2C 104.22(19) 2_666 . ?
O2A Nd1 O2C 71.09(19) . . ?
O1B Nd1 O1C 74.66(18) . 2_666 ?
O1E Nd1 O1C 141.5(2) . 2_666 ?
O1D Nd1 O1C 118.79(19) . 2_666 ?
O1C Nd1 O1C 73.2(2) . 2_666 ?
O1A Nd1 O1C 139.27(18) . 2_666 ?
O2B Nd1 O1C 71.34(17) 2_666 2_666 ?
O2A Nd1 O1C 95.26(19) . 2_666 ?
O2C Nd1 O1C 50.67(17) . 2_666 ?
O1B Nd1 C1A 154.3(2) . . ?
O1E Nd1 C1A 99.4(2) . . ?
O1D Nd1 C1A 77.6(2) . . ?
O1C Nd1 C1A 132.3(2) . . ?
O1A Nd1 C1A 26.9(2) . . ?
O2B Nd1 C1A 69.5(2) 2_666 . ?
O2A Nd1 C1A 26.1(2) . . ?
O2C Nd1 C1A 96.2(2) . . ?
O1C Nd1 C1A 117.7(2) 2_666 . ?
O1B Nd1 C1C 75.0(2) . 2_666 ?
O1E Nd1 C1C 150.7(2) . 2_666 ?
O1D Nd1 C1C 94.7(2) . 2_666 ?
O1C Nd1 C1C 97.7(2) . 2_666 ?
O1A Nd1 C1C 132.9(2) . 2_666 ?
O2B Nd1 C1C 86.0(2) 2_666 2_666 ?
O2A Nd1 C1C 80.3(2) . 2_666 ?
O2C Nd1 C1C 25.18(19) . 2_666 ?
O1C Nd1 C1C 25.72(19) 2_666 2_666 ?
C1A Nd1 C1C 106.2(2) . 2_666 ?
O1B Nd1 Nd1 68.83(13) . 2_666 ?
O1E Nd1 Nd1 110.03(16) . 2_666 ?
O1D Nd1 Nd1 141.21(14) . 2_666 ?
O1C Nd1 Nd1 38.07(13) . 2_666 ?
O1A Nd1 Nd1 137.62(14) . 2_666 ?
O2B Nd1 Nd1 66.77(12) 2_666 2_666 ?
O2A Nd1 Nd1 122.32(14) . 2_666 ?
O2C Nd1 Nd1 83.64(13) . 2_666 ?
O1C Nd1 Nd1 35.11(12) 2_666 2_666 ?
C1A Nd1 Nd1 134.73(17) . 2_666 ?
C1C Nd1 Nd1 60.02(18) 2_666 2_666 ?
O2A C1A O1A 121.9(7) . . ?
O2A C1A C2A 121.0(8) . . ?
O1A C1A C2A 117.1(8) . . ?
O2A C1A Nd1 62.1(4) . . ?
O1A C1A Nd1 59.8(4) . . ?
C2A C1A Nd1 175.7(6) . . ?
O2B C1B O1B 126.3(7) . . ?
O2B C1B C2B 119.1(7) . . ?
O1B C1B C2B 114.5(7) . . ?
O2C C1C O1C 120.5(8) 2_666 . ?
O2C C1C C2C 118.0(7) 2_666 . ?
O1C C1C C2C 121.2(8) . . ?
O2C C1C Nd1 58.1(4) 2_666 2_666 ?
O1C C1C Nd1 63.3(4) . 2_666 ?
C2C C1C Nd1 164.8(6) . 2_666 ?
C3A C2A C8A 117.9(8) . 2_655 ?
C3A C2A C1A 122.2(8) . . ?
C8A C2A C1A 120.0(8) 2_655 . ?
C8B C2B C3B 121.0(7) 2_676 . ?
C8B C2B C1B 119.8(7) 2_676 . ?
C3B C2B C1B 118.9(7) . . ?
C3C C2C C8C 120.8(7) . 2_566 ?
C3C C2C C1C 119.3(7) . . ?
C8C C2C C1C 119.8(7) 2_566 . ?
O1D C2D N3D 126.0(11) . . ?
O1E C2E N3E 125.1(13) . . ?
C2A C3A C8A 121.4(9) . . ?
C2A C3A C4A 122.1(9) . . ?
C8A C3A C4A 116.4(10) . . ?
C2B C3B C4B 122.6(8) . . ?
C2B C3B C8B 119.5(7) . . ?
C4B C3B C8B 117.9(8) . . ?
C2C C3C C8C 118.9(7) . . ?
C2C C3C C4C 121.8(8) . . ?
C8C C3C C4C 119.4(8) . . ?
C5A C4A C3A 122.6(10) . . ?
C5B C4B C3B 121.7(9) . . ?
C5C C4C C3C 120.4(9) . . ?
C4A C5A C6A 120.9(11) . . ?
C4B C5B C6B 120.3(10) . . ?
C4C C5C C6C 120.0(9) . . ?
C7A C6A C5A 118.5(11) . . ?
C7B C6B C5B 120.7(10) . . ?
C7C C6C C5C 121.3(9) . . ?
C6A C7A C8A 123.8(11) . . ?
C6B C7B C8B 121.1(9) . . ?
C6C C7C C8C 120.5(9) . . ?
C2A C8A C7A 121.8(9) 2_655 . ?
C2A C8A C3A 120.6(9) 2_655 . ?
C7A C8A C3A 117.6(10) . . ?
C2B C8B C7B 122.4(8) 2_676 . ?
C2B C8B C3B 119.4(7) 2_676 . ?
C7B C8B C3B 118.2(8) . . ?
C2C C8C C3C 120.3(7) 2_566 . ?
C2C C8C C7C 121.3(8) 2_566 . ?
C3C C8C C7C 118.4(8) . . ?
C2D N3D C5D 122.1(11) . . ?
C2D N3D C4D 118.6(10) . . ?
C5D N3D C4D 119.2(10) . . ?
C2E N3E C4E 123.1(14) . . ?
C2E N3E C5E 117.1(14) . . ?
C4E N3E C5E 119.7(11) . . ?
C1A O1A Nd1 93.3(5) . . ?
C1B O1B Nd1 139.2(5) . . ?
C1C O1C Nd1 154.9(5) . . ?
C1C O1C Nd1 91.0(5) . 2_666 ?
Nd1 O1C Nd1 106.8(2) . 2_666 ?
C2D O1D Nd1 124.4(6) . . ?
C2E O1E Nd1 141.7(8) . . ?
C1A O2A Nd1 91.8(5) . . ?
C1B O2B Nd1 138.2(5) . 2_666 ?
C1C O2C Nd1 96.8(5) 2_666 . ?

_refine_diff_density_max         1.075
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.126

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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
_platon_squeeze_void_content
1 0.000 0.000 0.000 238 41 ' '
_platon_squeeze_details          
;
;

# start Validation Reply Form
_vrf_CHEMW03_Comp2_Nd            
;
PROBLEM: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
RESPONSE: The crystal structure contains a percentage of voids occupied by
disordered solvent molecules. We have used SQUEZZE routine to eliminate
one DMF molecule.
;
# end Validation Reply Form

_shelxl_version_number           2014-3

