# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

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

data_La
_database_code_depnum_ccdc_archive 'CCDC 1472125'
_audit_update_record             
;
2016-04-04 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H28 La2 N4 O19'
_chemical_formula_weight         954.32

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   8.9602(13)
_cell_length_b                   10.7764(16)
_cell_length_c                   19.041(3)
_cell_angle_alpha                75.382(2)
_cell_angle_beta                 83.782(2)
_cell_angle_gamma                69.363(2)
_cell_volume                     1664.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5538
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      27.92

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             932
_exptl_absorpt_coefficient_mu    2.618
_exptl_absorpt_correction_type   'multi-scan '
_exptl_absorpt_correction_T_min  0.6225
_exptl_absorpt_correction_T_max  0.7797
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8526
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         25.20
_reflns_number_total             5863
_reflns_number_gt                5262
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0453P)²+10.9923P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5863
_refine_ls_number_parameters     424
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.1004
_refine_ls_wR_factor_gt          0.0980
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La -0.39654(9) 0.46842(5) 0.77683(4) 0.01311(13) Uani 0.90 1 d P . 1
La2 La -0.00151(8) 0.58977(5) 0.71255(4) 0.01246(12) Uani 0.90 1 d P . 1
La1' La -0.3792(9) 0.4164(9) 0.7842(4) 0.0400(19) Uani 0.10 1 d PU . 2
La2' La 0.0168(10) 0.5392(11) 0.7178(5) 0.054(2) Uani 0.10 1 d PU . 2
C1 C -0.1023(8) 0.6921(8) 0.9150(3) 0.0363(16) Uani 1 1 d . . .
H1A H -0.0673 0.7132 0.8671 0.044 Uiso 1 1 calc R . .
C2 C -0.2302(7) 0.6452(7) 0.9288(3) 0.0271(13) Uani 1 1 d . . .
C3 C -0.2878(7) 0.6180(7) 1.0000(3) 0.0271(13) Uani 1 1 d . . .
H3A H -0.3771 0.5910 1.0105 0.032 Uiso 1 1 calc R . .
C4 C -0.2081(7) 0.6322(7) 1.0550(3) 0.0264(13) Uani 1 1 d . . .
C5 C -0.0783(8) 0.6765(8) 1.0356(3) 0.0335(16) Uani 1 1 d . . .
H5A H -0.0245 0.6842 1.0725 0.040 Uiso 1 1 calc R . .
C6 C -0.3003(7) 0.6149(7) 0.8699(3) 0.0267(13) Uani 1 1 d . . .
C7 C -0.2562(7) 0.5955(6) 1.1338(3) 0.0240(13) Uani 1 1 d . . .
C8 C 0.3665(8) 0.9302(7) 0.7546(4) 0.0364(16) Uani 1 1 d . . .
H8A H 0.4643 0.8607 0.7549 0.044 Uiso 1 1 calc R . .
C9 C 0.2281(7) 0.8990(6) 0.7529(3) 0.0246(13) Uani 1 1 d . . .
C10 C 0.0830(7) 1.0055(6) 0.7512(3) 0.0260(13) Uani 1 1 d . . .
H10A H -0.0121 0.9893 0.7507 0.031 Uiso 1 1 calc R . .
C11 C 0.0802(7) 1.1345(6) 0.7503(3) 0.0249(13) Uani 1 1 d . . .
C12 C 0.2261(8) 1.1536(7) 0.7531(4) 0.0361(16) Uani 1 1 d . . .
H12A H 0.2253 1.2402 0.7532 0.043 Uiso 1 1 calc R . .
C13 C 0.2392(7) 0.7572(6) 0.7515(3) 0.0221(12) Uani 1 1 d . . .
C14 C -0.0716(7) 1.2529(6) 0.7479(3) 0.0254(13) Uani 1 1 d . . .
C15 C 0.5905(7) 0.3206(6) 0.5512(3) 0.0252(13) Uani 1 1 d . . .
H15A H 0.6683 0.3028 0.5845 0.030 Uiso 1 1 calc R . .
C16 C 0.4315(7) 0.3752(6) 0.5715(3) 0.0204(12) Uani 1 1 d . . .
C17 C 0.3152(7) 0.3991(6) 0.5223(3) 0.0250(13) Uani 1 1 d . . .
H17A H 0.2077 0.4335 0.5349 0.030 Uiso 1 1 calc R . .
C18 C 0.3606(7) 0.3713(6) 0.4545(3) 0.0227(12) Uani 1 1 d . . .
C19 C 0.5226(7) 0.3171(6) 0.4389(3) 0.0242(13) Uani 1 1 d . . .
H19A H 0.5534 0.2971 0.3937 0.029 Uiso 1 1 calc R . .
C20 C 0.3865(7) 0.4148(6) 0.6431(3) 0.0220(12) Uani 1 1 d . . .
C21 C 0.2424(7) 0.4010(6) 0.3974(3) 0.0229(12) Uani 1 1 d . . .
C22 C -0.2744(12) 0.2673(12) 0.9502(8) 0.083(4) Uani 1 1 d . . .
H22A H -0.2899 0.3308 0.9779 0.099 Uiso 1 1 calc R . .
C23 C -0.295(3) 0.117(2) 1.0677(11) 0.172(6) Uani 1 1 d U . .
H23A H -0.3034 0.1964 1.0845 0.258 Uiso 1 1 calc R . .
H23B H -0.2037 0.0426 1.0885 0.258 Uiso 1 1 calc R . .
H23C H -0.3897 0.0938 1.0822 0.258 Uiso 1 1 calc R . .
C24 C -0.310(3) 0.044(2) 0.9444(12) 0.190(6) Uani 1 1 d U . .
H24A H -0.3077 0.0801 0.8929 0.286 Uiso 1 1 calc R . .
H24B H -0.4122 0.0346 0.9590 0.286 Uiso 1 1 calc R . .
H24C H -0.2282 -0.0440 0.9564 0.286 Uiso 1 1 calc R . .
N1 N -0.0254(7) 0.7088(7) 0.9672(3) 0.0443(16) Uani 1 1 d . . .
N2 N 0.3669(7) 1.0524(6) 0.7557(4) 0.0456(16) Uani 1 1 d . . .
N3 N 0.6373(6) 0.2921(6) 0.4860(3) 0.0288(12) Uani 1 1 d . . .
N4 N -0.278(2) 0.1473(18) 0.9868(9) 0.159(5) Uani 1 1 d U . .
O1W O 0.0871(6) 0.7483(5) 0.6035(3) 0.0458(13) Uani 1 1 d . . .
O1 O -0.4306(5) 0.5933(6) 0.8812(3) 0.0400(12) Uani 1 1 d . . .
O2W O -0.1980(6) 0.8343(5) 0.6879(3) 0.0487(13) Uani 1 1 d . . .
O2 O -0.2219(5) 0.6059(5) 0.8108(2) 0.0311(10) Uani 1 1 d . . .
O3 O -0.1501(6) 0.5626(5) 1.1794(2) 0.0344(11) Uani 1 1 d . . .
O4 O -0.3988(6) 0.6032(6) 1.1478(2) 0.0393(12) Uani 1 1 d . . .
O5 O 0.1114(5) 0.7315(4) 0.7602(3) 0.0315(10) Uani 1 1 d . . .
O6 O 0.3760(5) 0.6745(4) 0.7420(3) 0.0324(10) Uani 1 1 d . . .
O7 O -0.2037(5) 1.2332(5) 0.7503(3) 0.0445(13) Uani 1 1 d . . .
O8 O -0.0669(5) 1.3691(4) 0.7447(3) 0.0322(10) Uani 1 1 d . . .
O9 O 0.4976(5) 0.4062(5) 0.6813(2) 0.0312(10) Uani 1 1 d . . .
O10 O 0.2404(5) 0.4552(5) 0.6595(2) 0.0315(10) Uani 1 1 d . . .
O11 O 0.0968(5) 0.4281(6) 0.4135(2) 0.0418(13) Uani 1 1 d . . .
O12 O 0.2947(5) 0.3927(4) 0.3338(2) 0.0257(9) Uani 1 1 d . . .
O13 O -0.2544(6) 0.3051(6) 0.8886(3) 0.0527(15) 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
La1 O6 2.426(4) 1_455 ?
La1 O4 2.426(4) 2_467 ?
La1 O9 2.468(4) 1_455 ?
La1 O13 2.524(5) . ?
La1 O12 2.543(4) 2_566 ?
La1 O1 2.605(5) . ?
La1 O7 2.653(5) 1_545 ?
La1 O2 2.719(4) . ?
La1 O8 2.821(4) 1_545 ?
La1 C6 3.014(6) . ?
La1 C14 3.116(6) 1_545 ?
La1 La2 4.1536(11) . ?
La2 O10 2.423(4) . ?
La2 O3 2.471(4) 2_567 ?
La2 O5 2.484(4) . ?
La2 O8 2.558(4) 1_545 ?
La2 O2W 2.559(5) . ?
La2 O2 2.560(4) . ?
La2 O1W 2.583(5) . ?
La2 O11 2.705(4) 2_566 ?
La2 O12 2.791(4) 2_566 ?
La2 C21 3.126(6) 2_566 ?
La1' O13 2.231(10) . ?
La1' O7 2.241(10) 1_545 ?
La1' O4 2.297(9) 2_467 ?
La1' O9 2.393(9) 1_455 ?
La1' O8 2.718(9) 1_545 ?
La1' C14 2.821(10) 1_545 ?
La1' O6 2.854(10) 1_455 ?
La1' O1 2.870(9) . ?
La1' O12 2.873(9) 2_566 ?
La1' O2 3.020(9) . ?
La1' La2' 4.176(11) . ?
La2' O8 2.145(11) 1_545 ?
La2' O10 2.194(10) . ?
La2' O3 2.227(10) 2_567 ?
La2' O2 2.639(10) . ?
La2' O11 2.695(10) 2_566 ?
La2' O5 2.810(11) . ?
La2' O12 2.844(9) 2_566 ?
La2' O1W 2.905(11) . ?
La2' O2W 3.025(11) . ?
C1 N1 1.350(9) . ?
C1 C2 1.384(9) . ?
C2 C3 1.393(9) . ?
C2 C6 1.496(8) . ?
C3 C4 1.396(8) . ?
C4 C5 1.388(9) . ?
C4 C7 1.508(8) . ?
C5 N1 1.340(9) . ?
C6 O1 1.255(8) . ?
C6 O2 1.267(7) . ?
C7 O3 1.253(7) . ?
C7 O4 1.254(7) . ?
C8 N2 1.324(9) . ?
C8 C9 1.400(9) . ?
C9 C10 1.395(8) . ?
C9 C13 1.503(8) . ?
C10 C11 1.377(9) . ?
C11 C12 1.402(9) . ?
C11 C14 1.497(8) . ?
C12 N2 1.342(9) . ?
C13 O5 1.254(7) . ?
C13 O6 1.263(7) . ?
C14 O8 1.253(7) . ?
C14 O7 1.269(8) . ?
C14 La1' 2.821(10) 1_565 ?
C14 La1 3.116(6) 1_565 ?
C15 N3 1.341(8) . ?
C15 C16 1.389(8) . ?
C16 C17 1.388(8) . ?
C16 C20 1.503(8) . ?
C17 C18 1.386(8) . ?
C18 C19 1.390(8) . ?
C18 C21 1.497(8) . ?
C19 N3 1.347(8) . ?
C20 O10 1.257(7) . ?
C20 O9 1.261(7) . ?
C21 O11 1.254(8) . ?
C21 O12 1.263(7) . ?
C21 La2 3.126(6) 2_566 ?
C22 O13 1.157(13) . ?
C22 N4 1.315(18) . ?
C23 N4 1.49(2) . ?
C24 N4 1.64(3) . ?
O3 La2' 2.227(10) 2_567 ?
O3 La2 2.471(4) 2_567 ?
O4 La1' 2.297(9) 2_467 ?
O4 La1 2.426(4) 2_467 ?
O6 La1 2.426(4) 1_655 ?
O6 La1' 2.854(10) 1_655 ?
O7 La1' 2.240(10) 1_565 ?
O7 La1 2.653(5) 1_565 ?
O8 La2' 2.145(11) 1_565 ?
O8 La2 2.558(4) 1_565 ?
O8 La1' 2.718(9) 1_565 ?
O8 La1 2.821(4) 1_565 ?
O9 La1' 2.393(9) 1_655 ?
O9 La1 2.468(4) 1_655 ?
O11 La2' 2.695(10) 2_566 ?
O11 La2 2.705(4) 2_566 ?
O12 La1 2.543(4) 2_566 ?
O12 La2 2.791(4) 2_566 ?
O12 La2' 2.844(9) 2_566 ?
O12 La1' 2.873(9) 2_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 La1 O4 80.83(17) 1_455 2_467 ?
O6 La1 O9 80.86(15) 1_455 1_455 ?
O4 La1 O9 83.64(15) 2_467 1_455 ?
O6 La1 O13 140.60(18) 1_455 . ?
O4 La1 O13 74.93(17) 2_467 . ?
O9 La1 O13 125.67(19) 1_455 . ?
O6 La1 O12 76.20(15) 1_455 2_566 ?
O4 La1 O12 154.19(15) 2_467 2_566 ?
O9 La1 O12 81.27(14) 1_455 2_566 ?
O13 La1 O12 130.80(16) . 2_566 ?
O6 La1 O1 75.73(16) 1_455 . ?
O4 La1 O1 78.64(16) 2_467 . ?
O9 La1 O1 152.51(15) 1_455 . ?
O13 La1 O1 69.42(19) . . ?
O12 La1 O1 106.49(15) 2_566 . ?
O6 La1 O7 148.96(16) 1_455 1_545 ?
O4 La1 O7 100.92(18) 2_467 1_545 ?
O9 La1 O7 68.68(15) 1_455 1_545 ?
O13 La1 O7 67.43(19) . 1_545 ?
O12 La1 O7 92.93(16) 2_566 1_545 ?
O1 La1 O7 135.23(17) . 1_545 ?
O6 La1 O2 92.68(15) 1_455 . ?
O4 La1 O2 126.68(14) 2_467 . ?
O9 La1 O2 147.83(14) 1_455 . ?
O13 La1 O2 78.10(18) . . ?
O12 La1 O2 66.60(13) 2_566 . ?
O1 La1 O2 48.84(13) . . ?
O7 La1 O2 109.79(14) 1_545 . ?
O6 La1 O8 138.84(15) 1_455 1_545 ?
O4 La1 O8 140.33(16) 2_467 1_545 ?
O9 La1 O8 100.21(14) 1_455 1_545 ?
O13 La1 O8 70.93(16) . 1_545 ?
O12 La1 O8 63.52(14) 2_566 1_545 ?
O1 La1 O8 106.86(14) . 1_545 ?
O7 La1 O8 47.17(13) 1_545 1_545 ?
O2 La1 O8 64.60(13) . 1_545 ?
O6 La1 C6 86.95(16) 1_455 . ?
O4 La1 C6 101.85(16) 2_467 . ?
O9 La1 C6 165.70(17) 1_455 . ?
O13 La1 C6 68.6(2) . . ?
O12 La1 C6 88.62(15) 2_566 . ?
O1 La1 C6 24.45(15) . . ?
O7 La1 C6 122.27(16) 1_545 . ?
O2 La1 C6 24.87(15) . . ?
O8 La1 C6 84.08(15) 1_545 . ?
O6 La1 C14 153.89(16) 1_455 1_545 ?
O4 La1 C14 120.17(18) 2_467 1_545 ?
O9 La1 C14 86.06(15) 1_455 1_545 ?
O13 La1 C14 64.63(17) . 1_545 ?
O12 La1 C14 79.56(15) 2_566 1_545 ?
O1 La1 C14 121.04(16) . 1_545 ?
O7 La1 C14 23.71(15) 1_545 1_545 ?
O2 La1 C14 86.46(15) . 1_545 ?
O8 La1 C14 23.72(14) 1_545 1_545 ?
C6 La1 C14 102.11(16) . 1_545 ?
O6 La1 La2 104.69(11) 1_455 . ?
O4 La1 La2 161.54(11) 2_467 . ?
O9 La1 La2 114.47(11) 1_455 . ?
O13 La1 La2 90.62(14) . . ?
O12 La1 La2 41.05(9) 2_566 . ?
O1 La1 La2 85.61(10) . . ?
O7 La1 La2 83.51(11) 1_545 . ?
O2 La1 La2 36.78(9) . . ?
O8 La1 La2 37.20(9) 1_545 . ?
C6 La1 La2 61.48(12) . . ?
C14 La1 La2 60.74(11) 1_545 . ?
O10 La2 O3 77.47(15) . 2_567 ?
O10 La2 O5 98.67(15) . . ?
O3 La2 O5 74.35(16) 2_567 . ?
O10 La2 O8 84.14(15) . 1_545 ?
O3 La2 O8 71.16(15) 2_567 1_545 ?
O5 La2 O8 143.89(16) . 1_545 ?
O10 La2 O2W 138.83(18) . . ?
O3 La2 O2W 132.87(17) 2_567 . ?
O5 La2 O2W 71.56(17) . . ?
O8 La2 O2W 127.57(17) 1_545 . ?
O10 La2 O2 149.68(16) . . ?
O3 La2 O2 78.53(15) 2_567 . ?
O5 La2 O2 92.39(15) . . ?
O8 La2 O2 70.71(15) 1_545 . ?
O2W La2 O2 71.47(17) . . ?
O10 La2 O1W 71.45(16) . . ?
O3 La2 O1W 129.09(17) 2_567 . ?
O5 La2 O1W 71.78(17) . . ?
O8 La2 O1W 140.84(17) 1_545 . ?
O2W La2 O1W 67.51(17) . . ?
O2 La2 O1W 138.83(16) . . ?
O10 La2 O11 75.88(15) . 2_566 ?
O3 La2 O11 138.80(17) 2_567 2_566 ?
O5 La2 O11 140.44(16) . 2_566 ?
O8 La2 O11 75.35(16) 1_545 2_566 ?
O2W La2 O11 86.90(18) . 2_566 ?
O2 La2 O11 112.15(14) . 2_566 ?
O1W La2 O11 69.37(17) . 2_566 ?
O10 La2 O12 118.59(14) . 2_566 ?
O3 La2 O12 128.99(14) 2_567 2_566 ?
O5 La2 O12 138.24(14) . 2_566 ?
O8 La2 O12 63.80(14) 1_545 2_566 ?
O2W La2 O12 68.03(16) . 2_566 ?
O2 La2 O12 65.30(13) . 2_566 ?
O1W La2 O12 101.38(16) . 2_566 ?
O11 La2 O12 47.08(13) 2_566 2_566 ?
O10 La2 C21 97.93(15) . 2_566 ?
O3 La2 C21 140.70(16) 2_567 2_566 ?
O5 La2 C21 144.02(15) . 2_566 ?
O8 La2 C21 69.54(15) 1_545 2_566 ?
O2W La2 C21 74.92(17) . 2_566 ?
O2 La2 C21 89.08(15) . 2_566 ?
O1W La2 C21 83.72(17) . 2_566 ?
O11 La2 C21 23.43(15) 2_566 2_566 ?
O12 La2 C21 23.78(14) 2_566 2_566 ?
O10 La2 La1 124.11(11) . . ?
O3 La2 La1 92.87(11) 2_567 . ?
O5 La2 La1 131.83(11) . . ?
O8 La2 La1 41.80(10) 1_545 . ?
O2W La2 La1 86.50(13) . . ?
O2 La2 La1 39.50(10) . . ?
O1W La2 La1 137.97(13) . . ?
O11 La2 La1 77.10(10) 2_566 . ?
O12 La2 La1 36.76(8) 2_566 . ?
C21 La2 La1 57.09(11) 2_566 . ?
O13 La1' O7 80.0(4) . 1_545 ?
O13 La1' O4 83.4(3) . 2_467 ?
O7 La1' O4 119.5(4) 1_545 2_467 ?
O13 La1' O9 147.7(5) . 1_455 ?
O7 La1' O9 77.2(3) 1_545 1_455 ?
O4 La1' O9 88.2(3) 2_467 1_455 ?
O13 La1' O8 77.2(3) . 1_545 ?
O7 La1' O8 51.4(2) 1_545 1_545 ?
O4 La1' O8 159.6(4) 2_467 1_545 ?
O9 La1' O8 105.2(3) 1_455 1_545 ?
O13 La1' C14 73.4(3) . 1_545 ?
O7 La1' C14 25.94(19) 1_545 1_545 ?
O4 La1' C14 140.2(4) 2_467 1_545 ?
O9 La1' C14 94.5(3) 1_455 1_545 ?
O8 La1' C14 26.07(17) 1_545 1_545 ?
O13 La1' O6 132.4(4) . 1_455 ?
O7 La1' O6 147.5(4) 1_545 1_455 ?
O4 La1' O6 74.4(3) 2_467 1_455 ?
O9 La1' O6 73.9(3) 1_455 1_455 ?
O8 La1' O6 123.7(3) 1_545 1_455 ?
C14 La1' O6 144.2(4) 1_545 1_455 ?
O13 La1' O1 68.5(3) . . ?
O7 La1' O1 143.8(4) 1_545 . ?
O4 La1' O1 75.3(3) 2_467 . ?
O9 La1' O1 138.7(4) 1_455 . ?
O8 La1' O1 102.5(3) 1_545 . ?
C14 La1' O1 122.3(3) 1_545 . ?
O6 La1' O1 65.4(2) 1_455 . ?
O13 La1' O12 128.6(4) . 2_566 ?
O7 La1' O12 94.1(3) 1_545 2_566 ?
O4 La1' O12 138.8(4) 2_467 2_566 ?
O9 La1' O12 76.0(3) 1_455 2_566 ?
O8 La1' O12 60.8(2) 1_545 2_566 ?
C14 La1' O12 79.7(3) 1_545 2_566 ?
O6 La1' O12 64.8(2) 1_455 2_566 ?
O1 La1' O12 91.8(3) . 2_566 ?
O13 La1' O2 76.4(3) . . ?
O7 La1' O2 112.5(3) 1_545 . ?
O4 La1' O2 119.2(3) 2_467 . ?
O9 La1' O2 133.8(4) 1_455 . ?
O8 La1' O2 61.9(2) 1_545 . ?
C14 La1' O2 86.6(3) 1_545 . ?
O6 La1' O2 78.7(3) 1_455 . ?
O1 La1' O2 43.84(17) . . ?
O12 La1' O2 58.7(2) 2_566 . ?
O13 La1' La2' 86.6(3) . . ?
O7 La1' La2' 77.7(3) 1_545 . ?
O4 La1' La2' 158.0(3) 2_467 . ?
O9 La1' La2' 110.3(3) 1_455 . ?
O8 La1' La2' 27.0(2) 1_545 . ?
C14 La1' La2' 53.0(2) 1_545 . ?
O6 La1' La2' 98.6(3) 1_455 . ?
O1 La1' La2' 82.8(2) . . ?
O12 La1' La2' 42.80(18) 2_566 . ?
O2 La1' La2' 39.02(18) . . ?
O8 La2' O10 100.6(5) 1_545 . ?
O8 La2' O3 84.0(4) 1_545 2_567 ?
O10 La2' O3 87.7(4) . 2_567 ?
O8 La2' O2 75.7(3) 1_545 . ?
O10 La2' O2 168.6(5) . . ?
O3 La2' O2 81.3(3) 2_567 . ?
O8 La2' O11 82.5(3) 1_545 2_566 ?
O10 La2' O11 79.8(3) . 2_566 ?
O3 La2' O11 159.6(5) 2_567 2_566 ?
O2 La2' O11 110.0(3) . 2_566 ?
O8 La2' O5 150.5(4) 1_545 . ?
O10 La2' O5 95.3(3) . . ?
O3 La2' O5 71.9(3) 2_567 . ?
O2 La2' O5 83.8(3) . . ?
O11 La2' O5 125.0(4) 2_566 . ?
O8 La2' O12 67.5(3) 1_545 2_566 ?
O10 La2' O12 125.4(4) . 2_566 ?
O3 La2' O12 138.7(4) 2_567 2_566 ?
O2 La2' O12 63.6(2) . 2_566 ?
O11 La2' O12 46.63(19) 2_566 2_566 ?
O5 La2' O12 121.4(4) . 2_566 ?
O8 La2' O1W 146.7(4) 1_545 . ?
O10 La2' O1W 68.4(3) . . ?
O3 La2' O1W 125.0(4) 2_567 . ?
O2 La2' O1W 120.5(4) . . ?
O11 La2' O1W 64.9(3) 2_566 . ?
O5 La2' O1W 62.6(3) . . ?
O12 La2' O1W 92.7(3) 2_566 . ?
O8 La2' O2W 124.4(4) 1_545 . ?
O10 La2' O2W 125.9(4) . . ?
O3 La2' O2W 122.0(4) 2_567 . ?
O2 La2' O2W 63.3(3) . . ?
O11 La2' O2W 78.3(3) 2_566 . ?
O5 La2' O2W 60.6(3) . . ?
O12 La2' O2W 61.4(2) 2_566 . ?
O1W La2' O2W 57.6(2) . . ?
O8 La2' La1' 35.1(2) 1_545 . ?
O10 La2' La1' 133.7(4) . . ?
O3 La2' La1' 96.7(3) 2_567 . ?
O2 La2' La1' 46.1(2) . . ?
O11 La2' La1' 80.8(3) 2_566 . ?
O5 La2' La1' 129.9(3) . . ?
O12 La2' La1' 43.35(19) 2_566 . ?
O1W La2' La1' 135.9(3) . . ?
O2W La2' La1' 90.1(2) . . ?
N1 C1 C2 123.6(6) . . ?
C1 C2 C3 118.9(6) . . ?
C1 C2 C6 121.3(6) . . ?
C3 C2 C6 119.7(6) . . ?
C2 C3 C4 118.4(6) . . ?
C5 C4 C3 118.2(6) . . ?
C5 C4 C7 120.2(5) . . ?
C3 C4 C7 121.6(5) . . ?
N1 C5 C4 124.3(6) . . ?
O1 C6 O2 121.7(5) . . ?
O1 C6 C2 119.6(5) . . ?
O2 C6 C2 118.5(5) . . ?
O1 C6 La1 59.2(3) . . ?
O2 C6 La1 64.5(3) . . ?
C2 C6 La1 162.9(5) . . ?
O3 C7 O4 126.0(6) . . ?
O3 C7 C4 116.7(5) . . ?
O4 C7 C4 117.3(5) . . ?
N2 C8 C9 124.1(6) . . ?
C10 C9 C8 116.8(6) . . ?
C10 C9 C13 122.8(5) . . ?
C8 C9 C13 120.4(6) . . ?
C11 C10 C9 120.3(5) . . ?
C10 C11 C12 118.0(6) . . ?
C10 C11 C14 122.7(5) . . ?
C12 C11 C14 119.3(5) . . ?
N2 C12 C11 122.8(6) . . ?
O5 C13 O6 125.8(6) . . ?
O5 C13 C9 117.0(5) . . ?
O6 C13 C9 117.2(5) . . ?
O8 C14 O7 121.0(6) . . ?
O8 C14 C11 119.9(5) . . ?
O7 C14 C11 119.1(5) . . ?
O8 C14 La1' 72.4(4) . 1_565 ?
O7 C14 La1' 50.6(4) . 1_565 ?
C11 C14 La1' 161.1(5) . 1_565 ?
O8 C14 La1 64.8(3) . 1_565 ?
O7 C14 La1 57.2(3) . 1_565 ?
C11 C14 La1 167.9(4) . 1_565 ?
La1' C14 La1 8.10(18) 1_565 1_565 ?
N3 C15 C16 123.3(5) . . ?
C17 C16 C15 118.4(5) . . ?
C17 C16 C20 120.6(5) . . ?
C15 C16 C20 120.9(5) . . ?
C18 C17 C16 119.4(5) . . ?
C17 C18 C19 118.1(5) . . ?
C17 C18 C21 122.5(5) . . ?
C19 C18 C21 119.4(5) . . ?
N3 C19 C18 123.4(5) . . ?
O10 C20 O9 125.4(5) . . ?
O10 C20 C16 117.1(5) . . ?
O9 C20 C16 117.6(5) . . ?
O11 C21 O12 121.6(5) . . ?
O11 C21 C18 120.4(5) . . ?
O12 C21 C18 118.0(5) . . ?
O11 C21 La2 59.1(3) . 2_566 ?
O12 C21 La2 63.0(3) . 2_566 ?
C18 C21 La2 170.2(4) . 2_566 ?
O13 C22 N4 129.3(15) . . ?
C5 N1 C1 116.5(6) . . ?
C8 N2 C12 118.0(6) . . ?
C15 N3 C19 117.4(5) . . ?
C22 N4 C23 120.3(17) . . ?
C22 N4 C24 120.0(16) . . ?
C23 N4 C24 117.9(17) . . ?
La2 O1W La2' 7.90(19) . . ?
C6 O1 La1 96.3(4) . . ?
C6 O1 La1' 98.1(4) . . ?
La1 O1 La1' 9.18(18) . . ?
La2 O2W La2' 3.54(18) . . ?
C6 O2 La2 163.6(4) . . ?
C6 O2 La2' 161.2(5) . . ?
La2 O2 La2' 10.8(2) . . ?
C6 O2 La1 90.7(4) . . ?
La2 O2 La1 103.73(14) . . ?
La2' O2 La1 97.4(2) . . ?
C6 O2 La1' 90.7(4) . . ?
La2 O2 La1' 102.3(2) . . ?
La2' O2 La1' 94.9(3) . . ?
La1 O2 La1' 8.29(16) . . ?
C7 O3 La2' 159.0(5) . 2_567 ?
C7 O3 La2 152.1(4) . 2_567 ?
La2' O3 La2 10.6(3) 2_567 2_567 ?
C7 O4 La1' 158.6(5) . 2_467 ?
C7 O4 La1 151.8(4) . 2_467 ?
La1' O4 La1 12.0(2) 2_467 2_467 ?
C13 O5 La2 135.9(4) . . ?
C13 O5 La2' 132.5(4) . . ?
La2 O5 La2' 8.13(19) . . ?
C13 O6 La1 154.3(4) . 1_655 ?
C13 O6 La1' 150.7(4) . 1_655 ?
La1 O6 La1' 6.11(17) 1_655 1_655 ?
C14 O7 La1' 103.5(4) . 1_565 ?
C14 O7 La1 99.1(4) . 1_565 ?
La1' O7 La1 7.1(2) 1_565 1_565 ?
C14 O8 La2' 159.6(5) . 1_565 ?
C14 O8 La2 165.0(4) . 1_565 ?
La2' O8 La2 6.7(3) 1_565 1_565 ?
C14 O8 La1' 81.5(4) . 1_565 ?
La2' O8 La1' 117.9(4) 1_565 1_565 ?
La2 O8 La1' 111.3(2) 1_565 1_565 ?
C14 O8 La1 91.5(4) . 1_565 ?
La2' O8 La1 107.6(3) 1_565 1_565 ?
La2 O8 La1 101.00(14) 1_565 1_565 ?
La1' O8 La1 10.40(18) 1_565 1_565 ?
C20 O9 La1' 157.7(4) . 1_655 ?
C20 O9 La1 152.6(4) . 1_655 ?
La1' O9 La1 12.0(2) 1_655 1_655 ?
C20 O10 La2' 161.0(5) . . ?
C20 O10 La2 156.5(4) . . ?
La2' O10 La2 11.0(3) . . ?
C21 O11 La2' 99.6(4) . 2_566 ?
C21 O11 La2 97.5(4) . 2_566 ?
La2' O11 La2 10.5(2) 2_566 2_566 ?
C21 O12 La1 139.1(4) . 2_566 ?
C21 O12 La2 93.2(3) . 2_566 ?
La1 O12 La2 102.19(13) 2_566 2_566 ?
C21 O12 La2' 92.2(4) . 2_566 ?
La1 O12 La2' 96.6(2) 2_566 2_566 ?
La2 O12 La2' 10.1(2) 2_566 2_566 ?
C21 O12 La1' 131.7(4) . 2_566 ?
La1 O12 La1' 8.31(17) 2_566 2_566 ?
La2 O12 La1' 100.6(2) 2_566 2_566 ?
La2' O12 La1' 93.9(3) 2_566 2_566 ?
C22 O13 La1' 143.7(7) . . ?
C22 O13 La1 141.8(7) . . ?
La1' O13 La1 10.2(2) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         2.576
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.145
# 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 -0.026 0.000 0.500 231 63 ' '
2 0.314 0.061 0.184 12 6 ' '
3 0.351 0.894 0.309 6 2 ' '
4 0.649 0.106 0.691 7 2 ' '
5 0.686 0.939 0.816 12 6 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Pr
_database_code_depnum_ccdc_archive 'CCDC 1472126'
_audit_update_record             
;
2016-04-04 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H28 N4 O19 Pr2'
_chemical_formula_weight         958.32

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   8.8723(12)
_cell_length_b                   10.7152(15)
_cell_length_c                   18.920(3)
_cell_angle_alpha                75.496(2)
_cell_angle_beta                 83.797(2)
_cell_angle_gamma                69.336(2)
_cell_volume                     1629.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4318
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      28.01

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             940
_exptl_absorpt_coefficient_mu    3.044
_exptl_absorpt_correction_type   ' multi-scan '
_exptl_absorpt_correction_T_min  0.5812
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8456
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         25.20
_reflns_number_total             5760
_reflns_number_gt                4925
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0398P)²+3.0893P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5760
_refine_ls_number_parameters     411
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0791
_refine_ls_wR_factor_gt          0.0757
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.49816(3) 0.58858(3) 0.213001(13) 0.01675(9) Uani 1 1 d . . .
Pr2 Pr 0.10400(3) 0.46808(3) 0.276277(13) 0.01684(9) Uani 1 1 d . . .
C1 C 0.3985(7) 0.6927(6) 0.4168(3) 0.0320(13) Uani 1 1 d . . .
H1A H 0.4338 0.7156 0.3688 0.038 Uiso 1 1 calc R . .
C2 C 0.2699(6) 0.6435(5) 0.4296(3) 0.0245(11) Uani 1 1 d . . .
C3 C 0.2129(6) 0.6162(5) 0.5013(3) 0.0220(11) Uani 1 1 d . . .
H3A H 0.1234 0.5881 0.5118 0.026 Uiso 1 1 calc R . .
C4 C 0.2900(6) 0.6312(5) 0.5564(3) 0.0212(10) Uani 1 1 d . . .
C5 C 0.4212(7) 0.6760(6) 0.5370(3) 0.0310(13) Uani 1 1 d . . .
H5A H 0.4757 0.6832 0.5743 0.037 Uiso 1 1 calc R . .
C6 C 0.2009(6) 0.6133(5) 0.3703(3) 0.0250(11) Uani 1 1 d . . .
C7 C 0.2414(6) 0.5937(5) 0.6354(3) 0.0195(10) Uani 1 1 d . . .
C8 C -0.0239(6) 0.6843(5) 0.0604(3) 0.0217(11) Uani 1 1 d . . .
H8A H -0.0554 0.7041 0.1060 0.026 Uiso 1 1 calc R . .
C9 C 0.1385(6) 0.6297(5) 0.0457(3) 0.0219(11) Uani 1 1 d . . .
C10 C 0.1868(6) 0.5991(5) -0.0220(3) 0.0219(11) Uani 1 1 d . . .
H10A H 0.2955 0.5625 -0.0338 0.026 Uiso 1 1 calc R . .
C11 C 0.0689(6) 0.6244(5) -0.0720(3) 0.0210(10) Uani 1 1 d . . .
C12 C -0.0920(6) 0.6806(5) -0.0526(3) 0.0246(11) Uani 1 1 d . . .
H12A H -0.1701 0.6981 -0.0862 0.029 Uiso 1 1 calc R . .
C13 C 0.2565(6) 0.5993(5) 0.1036(3) 0.0241(11) Uani 1 1 d . . .
C14 C 0.1150(6) 0.5831(5) -0.1438(3) 0.0212(11) Uani 1 1 d . . .
C15 C 0.7279(7) 0.1527(5) 0.2539(3) 0.0329(13) Uani 1 1 d . . .
H15A H 0.7274 0.2393 0.2546 0.039 Uiso 1 1 calc R . .
C16 C 0.5813(6) 0.1356(5) 0.2498(3) 0.0237(11) Uani 1 1 d . . .
C17 C 0.5819(6) 0.0064(5) 0.2496(3) 0.0256(11) Uani 1 1 d . . .
H17A H 0.4855 -0.0086 0.2477 0.031 Uiso 1 1 calc R . .
C18 C 0.7270(6) -0.1004(5) 0.2523(3) 0.0209(10) Uani 1 1 d . . .
C19 C 0.8683(7) -0.0721(6) 0.2553(3) 0.0350(14) Uani 1 1 d . . .
H19A H 0.9662 -0.1432 0.2562 0.042 Uiso 1 1 calc R . .
C20 C 0.4267(6) 0.2562(5) 0.2459(3) 0.0248(11) Uani 1 1 d . . .
C21 C 0.7384(6) -0.2438(5) 0.2520(3) 0.0243(11) Uani 1 1 d . . .
C22 C 0.2234(9) 0.2628(10) 0.4502(5) 0.068(2) Uani 1 1 d . . .
H22 H 0.2072 0.3273 0.4777 0.082 Uiso 1 1 calc R A 1
C23 C 0.2257(19) 0.0565(13) 0.4489(8) 0.167(5) Uani 1 1 d U . .
H23A H 0.2392 0.0908 0.3975 0.200 Uiso 1 1 d R C .
H23B H 0.1310 0.0306 0.4574 0.200 Uiso 1 1 d R . .
H23C H 0.3182 -0.0220 0.4663 0.200 Uiso 1 1 d R . .
C24 C 0.1990(16) 0.1119(12) 0.5637(6) 0.124(4) Uani 1 1 d U . .
H24A H 0.1966 0.1853 0.5848 0.186 Uiso 1 1 calc R B 1
H24B H 0.2874 0.0312 0.5831 0.186 Uiso 1 1 calc R B 1
H24C H 0.0998 0.0934 0.5753 0.186 Uiso 1 1 calc R B 1
N1 N 0.4740(6) 0.7089(6) 0.4693(3) 0.0376(12) Uani 1 1 d . . .
N2 N -0.1397(5) 0.7109(5) 0.0131(2) 0.0271(10) Uani 1 1 d . . .
N3 N 0.8705(5) 0.0507(5) 0.2570(3) 0.0405(13) Uani 1 1 d . . .
N4 N 0.2188(18) 0.1503(11) 0.4859(6) 0.059(3) Uani 0.50 1 d PU C 1
N4' N 0.216(6) 0.271(5) 0.543(3) 0.33(2) Uiso 0.50 1 d P C 2
O1 O 0.0702(5) 0.5910(4) 0.3807(2) 0.0373(10) Uani 1 1 d . . .
O1W O 0.3016(5) 0.8296(4) 0.1893(2) 0.0465(11) Uani 1 1 d . . .
H1WA H 0.2500 0.8450 0.2285 0.056 Uiso 1 1 d R . .
H1WB H 0.2344 0.8394 0.1579 0.056 Uiso 1 1 d R . .
O2 O 0.2802(4) 0.6035(4) 0.31043(19) 0.0302(9) Uani 1 1 d . . .
O2W O 0.5855(5) 0.7473(4) 0.1045(2) 0.0469(11) Uani 1 1 d . . .
H2WA H 0.5193 0.8285 0.0998 0.056 Uiso 1 1 d R . .
H2WB H 0.5852 0.7213 0.0656 0.056 Uiso 1 1 d R . .
O3 O 0.0976(5) 0.6024(4) 0.6489(2) 0.0350(9) Uani 1 1 d . . .
O4 O 0.3494(5) 0.5575(4) 0.68108(19) 0.0306(9) Uani 1 1 d . . .
O5 O 0.2024(4) 0.6079(4) 0.16790(17) 0.0243(8) Uani 1 1 d . . .
O6 O 0.4034(4) 0.5719(5) 0.0881(2) 0.0378(10) Uani 1 1 d . . .
O7 O 0.2634(4) 0.5416(4) -0.15957(19) 0.0296(9) Uani 1 1 d . . .
O8 O 0.0052(4) 0.5903(4) -0.18211(19) 0.0299(9) Uani 1 1 d . . .
O9 O 0.2952(4) 0.2387(4) 0.2461(3) 0.0410(10) Uani 1 1 d . . .
O10 O 0.4348(5) 0.3718(4) 0.2443(2) 0.0322(9) Uani 1 1 d . . .
O11 O 0.6095(4) -0.2689(4) 0.2588(2) 0.0307(9) Uani 1 1 d . . .
O12 O 0.8760(4) -0.3263(4) 0.2435(2) 0.0314(9) Uani 1 1 d . . .
O13 O 0.2456(5) 0.3035(5) 0.3850(2) 0.0479(12) Uani 1 1 d . C .


_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 O7 2.367(3) 2_665 ?
Pr1 O4 2.411(4) 2_666 ?
Pr1 O11 2.444(4) 1_565 ?
Pr1 O10 2.495(3) . ?
Pr1 O2 2.514(3) . ?
Pr1 O1W 2.514(4) . ?
Pr1 O2W 2.558(4) . ?
Pr1 O6 2.659(4) . ?
Pr1 O5 2.769(4) . ?
Pr1 Pr2 4.1034(6) . ?
Pr2 O3 2.376(4) 2_566 ?
Pr2 O12 2.403(4) 1_465 ?
Pr2 O8 2.422(3) 2_565 ?
Pr2 O13 2.470(4) . ?
Pr2 O5 2.492(3) . ?
Pr2 O1 2.574(4) . ?
Pr2 O9 2.607(4) . ?
Pr2 O2 2.694(4) . ?
Pr2 O10 2.799(4) . ?
C1 N1 1.333(7) . ?
C1 C2 1.393(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.391(7) . ?
C2 C6 1.486(7) . ?
C3 C4 1.378(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.391(7) . ?
C4 C7 1.504(6) . ?
C5 N1 1.321(7) . ?
C5 H5A 0.9300 . ?
C6 O1 1.249(6) . ?
C6 O2 1.275(6) . ?
C7 O3 1.248(6) . ?
C7 O4 1.251(6) . ?
C8 N2 1.343(6) . ?
C8 C9 1.377(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.388(7) . ?
C9 C13 1.494(7) . ?
C10 C11 1.396(7) . ?
C10 H10A 0.9300 . ?
C11 C12 1.388(7) . ?
C11 C14 1.503(6) . ?
C12 N2 1.349(6) . ?
C12 H12A 0.9300 . ?
C13 O6 1.250(6) . ?
C13 O5 1.271(6) . ?
C14 O8 1.246(6) . ?
C14 O7 1.261(6) . ?
C15 N3 1.344(7) . ?
C15 C16 1.389(7) . ?
C15 H15A 0.9300 . ?
C16 C17 1.383(7) . ?
C16 C20 1.510(7) . ?
C17 C18 1.384(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.399(7) . ?
C18 C21 1.505(7) . ?
C19 N3 1.331(7) . ?
C19 H19A 0.9300 . ?
C20 O9 1.245(6) . ?
C20 O10 1.259(6) . ?
C21 O11 1.251(6) . ?
C21 O12 1.251(6) . ?
C22 O13 1.220(9) . ?
C22 N4 1.238(13) . ?
C22 N4' 1.76(5) . ?
C22 H22 0.9300 . ?
C23 N4 1.344(16) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9601 . ?
C23 H23C 0.9600 . ?
C24 N4 1.434(13) . ?
C24 N4' 1.71(5) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8501 . ?
O2W H2WB 0.8501 . ?
O3 Pr2 2.376(4) 2_566 ?
O4 Pr1 2.411(4) 2_666 ?
O7 Pr1 2.367(3) 2_665 ?
O8 Pr2 2.422(3) 2_565 ?
O11 Pr1 2.444(3) 1_545 ?
O12 Pr2 2.403(4) 1_645 ?

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
O7 Pr1 O4 77.97(13) 2_665 2_666 ?
O7 Pr1 O11 98.58(13) 2_665 1_565 ?
O4 Pr1 O11 73.92(13) 2_666 1_565 ?
O7 Pr1 O10 84.44(13) 2_665 . ?
O4 Pr1 O10 72.28(13) 2_666 . ?
O11 Pr1 O10 144.60(13) 1_565 . ?
O7 Pr1 O2 150.06(13) 2_665 . ?
O4 Pr1 O2 78.76(13) 2_666 . ?
O11 Pr1 O2 92.79(12) 1_565 . ?
O10 Pr1 O2 70.65(12) . . ?
O7 Pr1 O1W 138.55(14) 2_665 . ?
O4 Pr1 O1W 132.21(14) 2_666 . ?
O11 Pr1 O1W 71.27(14) 1_565 . ?
O10 Pr1 O1W 127.37(13) . . ?
O2 Pr1 O1W 71.38(13) . . ?
O7 Pr1 O2W 71.08(13) 2_665 . ?
O4 Pr1 O2W 128.24(14) 2_666 . ?
O11 Pr1 O2W 71.05(14) 1_565 . ?
O10 Pr1 O2W 140.91(13) . . ?
O2 Pr1 O2W 138.83(13) . . ?
O1W Pr1 O2W 67.61(14) . . ?
O7 Pr1 O6 75.62(12) 2_665 . ?
O4 Pr1 O6 139.90(13) 2_666 . ?
O11 Pr1 O6 139.49(13) 1_565 . ?
O10 Pr1 O6 75.60(13) . . ?
O2 Pr1 O6 112.29(12) . . ?
O1W Pr1 O6 86.71(14) . . ?
O2W Pr1 O6 69.18(14) . . ?
O7 Pr1 O5 119.15(11) 2_665 . ?
O4 Pr1 O5 129.96(11) 2_666 . ?
O11 Pr1 O5 137.32(11) 1_565 . ?
O10 Pr1 O5 64.17(12) . . ?
O2 Pr1 O5 64.83(11) . . ?
O1W Pr1 O5 67.30(13) . . ?
O2W Pr1 O5 101.44(13) . . ?
O6 Pr1 O5 47.73(10) . . ?
O7 Pr1 Pr2 124.38(9) 2_665 . ?
O4 Pr1 Pr2 94.02(9) 2_666 . ?
O11 Pr1 Pr2 132.28(9) 1_565 . ?
O10 Pr1 Pr2 41.95(9) . . ?
O2 Pr1 Pr2 39.58(8) . . ?
O1W Pr1 Pr2 86.12(10) . . ?
O2W Pr1 Pr2 137.70(11) . . ?
O6 Pr1 Pr2 77.08(8) . . ?
O5 Pr1 Pr2 36.38(7) . . ?
O3 Pr2 O12 80.59(13) 2_566 1_465 ?
O3 Pr2 O8 83.55(13) 2_566 2_565 ?
O12 Pr2 O8 80.65(13) 1_465 2_565 ?
O3 Pr2 O13 74.61(14) 2_566 . ?
O12 Pr2 O13 140.69(14) 1_465 . ?
O8 Pr2 O13 125.18(15) 2_565 . ?
O3 Pr2 O5 154.12(13) 2_566 . ?
O12 Pr2 O5 76.08(12) 1_465 . ?
O8 Pr2 O5 81.77(12) 2_565 . ?
O13 Pr2 O5 131.15(13) . . ?
O3 Pr2 O1 78.18(13) 2_566 . ?
O12 Pr2 O1 75.13(13) 1_465 . ?
O8 Pr2 O1 151.64(12) 2_565 . ?
O13 Pr2 O1 70.31(15) . . ?
O5 Pr2 O1 106.05(12) . . ?
O3 Pr2 O9 101.93(14) 2_566 . ?
O12 Pr2 O9 148.54(13) 1_465 . ?
O8 Pr2 O9 68.65(13) 2_565 . ?
O13 Pr2 O9 67.81(15) . . ?
O5 Pr2 O9 92.41(13) . . ?
O1 Pr2 O9 136.29(14) . . ?
O3 Pr2 O2 126.45(12) 2_566 . ?
O12 Pr2 O2 92.66(12) 1_465 . ?
O8 Pr2 O2 148.01(12) 2_565 . ?
O13 Pr2 O2 78.71(14) . . ?
O5 Pr2 O2 66.28(11) . . ?
O1 Pr2 O2 49.13(11) . . ?
O9 Pr2 O2 109.58(12) . . ?
O3 Pr2 O10 140.65(12) 2_566 . ?
O12 Pr2 O10 138.74(12) 1_465 . ?
O8 Pr2 O10 101.59(12) 2_565 . ?
O13 Pr2 O10 70.70(13) . . ?
O5 Pr2 O10 63.74(11) . . ?
O1 Pr2 O10 106.31(12) . . ?
O9 Pr2 O10 47.56(11) . . ?
O2 Pr2 O10 63.61(11) . . ?
O3 Pr2 Pr1 161.05(9) 2_566 . ?
O12 Pr2 Pr1 104.84(9) 1_465 . ?
O8 Pr2 Pr1 115.08(9) 2_565 . ?
O13 Pr2 Pr1 90.80(10) . . ?
O5 Pr2 Pr1 41.23(8) . . ?
O1 Pr2 Pr1 85.62(8) . . ?
O9 Pr2 Pr1 83.02(9) . . ?
O2 Pr2 Pr1 36.49(7) . . ?
O10 Pr2 Pr1 36.57(7) . . ?
N1 C1 C2 123.9(5) . . ?
N1 C1 H1A 118.1 . . ?
C2 C1 H1A 118.1 . . ?
C3 C2 C1 117.5(5) . . ?
C3 C2 C6 120.6(5) . . ?
C1 C2 C6 121.8(5) . . ?
C4 C3 C2 119.5(5) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C3 C4 C5 117.6(5) . . ?
C3 C4 C7 121.9(4) . . ?
C5 C4 C7 120.4(4) . . ?
N1 C5 C4 124.6(5) . . ?
N1 C5 H5A 117.7 . . ?
C4 C5 H5A 117.7 . . ?
O1 C6 O2 120.5(5) . . ?
O1 C6 C2 120.0(4) . . ?
O2 C6 C2 119.3(5) . . ?
O3 C7 O4 126.5(5) . . ?
O3 C7 C4 116.9(4) . . ?
O4 C7 C4 116.5(4) . . ?
N2 C8 C9 124.2(4) . . ?
N2 C8 H8A 117.9 . . ?
C9 C8 H8A 117.9 . . ?
C8 C9 C10 118.4(5) . . ?
C8 C9 C13 119.5(4) . . ?
C10 C9 C13 122.0(4) . . ?
C9 C10 C11 118.7(4) . . ?
C9 C10 H10A 120.7 . . ?
C11 C10 H10A 120.7 . . ?
C12 C11 C10 118.9(4) . . ?
C12 C11 C14 120.6(4) . . ?
C10 C11 C14 120.5(4) . . ?
N2 C12 C11 122.8(5) . . ?
N2 C12 H12A 118.6 . . ?
C11 C12 H12A 118.6 . . ?
O6 C13 O5 121.4(5) . . ?
O6 C13 C9 120.4(4) . . ?
O5 C13 C9 118.2(4) . . ?
O8 C14 O7 125.3(5) . . ?
O8 C14 C11 118.0(4) . . ?
O7 C14 C11 116.6(4) . . ?
N3 C15 C16 123.5(5) . . ?
N3 C15 H15A 118.3 . . ?
C16 C15 H15A 118.3 . . ?
C17 C16 C15 118.3(5) . . ?
C17 C16 C20 121.7(5) . . ?
C15 C16 C20 120.0(5) . . ?
C16 C17 C18 119.5(5) . . ?
C16 C17 H17A 120.2 . . ?
C18 C17 H17A 120.2 . . ?
C17 C18 C19 117.8(5) . . ?
C17 C18 C21 122.9(4) . . ?
C19 C18 C21 119.3(5) . . ?
N3 C19 C18 123.8(5) . . ?
N3 C19 H19A 118.1 . . ?
C18 C19 H19A 118.1 . . ?
O9 C20 O10 121.7(5) . . ?
O9 C20 C16 119.6(5) . . ?
O10 C20 C16 118.6(5) . . ?
O11 C21 O12 126.0(5) . . ?
O11 C21 C18 117.2(4) . . ?
O12 C21 C18 116.8(5) . . ?
O13 C22 N4 131.1(10) . . ?
O13 C22 N4' 153.4(19) . . ?
N4 C22 N4' 74.5(18) . . ?
O13 C22 H22 114.5 . . ?
N4 C22 H22 114.5 . . ?
N4' C22 H22 40.8 . . ?
N4 C23 H23A 110.4 . . ?
N4 C23 H23B 111.7 . . ?
H23A C23 H23B 109.5 . . ?
N4 C23 H23C 106.2 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N4 C24 N4' 72.3(18) . . ?
N4 C24 H24A 109.5 . . ?
N4' C24 H24A 37.2 . . ?
N4 C24 H24B 109.5 . . ?
N4' C24 H24B 121.6 . . ?
H24A C24 H24B 109.5 . . ?
N4 C24 H24C 109.5 . . ?
N4' C24 H24C 125.2 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C5 N1 C1 116.9(5) . . ?
C8 N2 C12 117.1(4) . . ?
C19 N3 C15 117.2(5) . . ?
C22 N4 C23 117.7(11) . . ?
C22 N4 C24 126.1(11) . . ?
C23 N4 C24 116.2(11) . . ?
C22 N4' C24 87(2) . . ?
C6 O1 Pr2 97.2(3) . . ?
Pr1 O1W H1WA 109.6 . . ?
Pr1 O1W H1WB 109.5 . . ?
H1WA O1W H1WB 108.2 . . ?
C6 O2 Pr1 163.4(3) . . ?
C6 O2 Pr2 90.9(3) . . ?
Pr1 O2 Pr2 103.92(12) . . ?
Pr1 O2W H2WA 109.6 . . ?
Pr1 O2W H2WB 109.5 . . ?
H2WA O2W H2WB 108.2 . . ?
C7 O3 Pr2 151.0(3) . 2_566 ?
C7 O4 Pr1 154.5(3) . 2_666 ?
C13 O5 Pr2 138.4(3) . . ?
C13 O5 Pr1 92.2(3) . . ?
Pr2 O5 Pr1 102.39(12) . . ?
C13 O6 Pr1 98.0(3) . . ?
C14 O7 Pr1 156.3(3) . 2_665 ?
C14 O8 Pr2 154.3(3) . 2_565 ?
C20 O9 Pr2 99.3(3) . . ?
C20 O10 Pr1 165.0(3) . . ?
C20 O10 Pr2 89.8(3) . . ?
Pr1 O10 Pr2 101.49(12) . . ?
C21 O11 Pr1 137.1(3) . 1_545 ?
C21 O12 Pr2 155.6(4) . 1_645 ?
C22 O13 Pr2 141.0(5) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         1.135
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.120
# 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 -0.018 0.000 0.000 223 62 ' '
2 0.148 0.107 0.191 7 2 ' '
3 0.193 0.970 0.306 13 7 ' '
4 0.808 0.025 0.697 13 8 ' '
5 0.854 0.888 0.814 5 2 ' '
_platon_squeeze_details          ?
####################################################################### 
# 
# 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_Sm
_database_code_depnum_ccdc_archive 'CCDC 1472127'
_audit_update_record             
;
2016-04-04 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H28 N4 O19 Sm2'
_chemical_formula_weight         977.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   8.8475(18)
_cell_length_b                   10.716(2)
_cell_length_c                   18.895(4)
_cell_angle_alpha                75.521(2)
_cell_angle_beta                 83.777(2)
_cell_angle_gamma                69.306(2)
_cell_volume                     1622.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4501
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      28.17

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    3.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5270
_exptl_absorpt_correction_T_max  0.7102
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8394
_diffrn_reflns_av_R_equivalents  0.1231
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         25.20
_reflns_number_total             5733
_reflns_number_gt                4712
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0989P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0009(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5733
_refine_ls_number_parameters     387
_refine_ls_number_restraints     365
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0564
_refine_ls_wR_factor_ref         0.1605
_refine_ls_wR_factor_gt          0.1547
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.00220(5) 0.41200(4) 0.28695(2) 0.01633(18) Uani 1 1 d . . .
Sm2 Sm 0.39655(5) 0.53203(4) 0.22375(2) 0.01615(18) Uani 1 1 d . . .
C1 C 0.5260(9) 0.3142(8) 0.4395(4) 0.0180(15) Uani 1 1 d U . .
H1A H 0.5574 0.2924 0.3943 0.022 Uiso 1 1 calc RU . .
C2 C 0.3614(10) 0.3714(9) 0.4544(4) 0.0200(15) Uani 1 1 d U . .
C3 C 0.3120(10) 0.4034(8) 0.5214(4) 0.0191(14) Uani 1 1 d U . .
H3A H 0.2029 0.4414 0.5329 0.023 Uiso 1 1 calc R . .
C4 C 0.4316(10) 0.3770(8) 0.5721(4) 0.0171(14) Uani 1 1 d U . .
C5 C 0.5915(10) 0.3192(9) 0.5528(5) 0.0223(16) Uani 1 1 d U . .
H5A H 0.6694 0.2999 0.5870 0.027 Uiso 1 1 calc R . .
C6 C 0.2443(10) 0.4001(8) 0.3961(4) 0.0184(15) Uani 1 1 d U . .
C7 C 0.3857(10) 0.4163(8) 0.6439(4) 0.0186(16) Uani 1 1 d U . .
C8 C -0.0995(11) 0.6914(9) -0.0838(5) 0.0282(17) Uani 1 1 d U . .
H8A H -0.0632 0.7135 -0.1318 0.034 Uiso 1 1 calc RU . .
C9 C -0.2305(10) 0.6431(9) -0.0703(5) 0.0226(15) Uani 1 1 d U . .
C10 C -0.2895(10) 0.6154(8) 0.0010(4) 0.0199(15) Uani 1 1 d U . .
H10A H -0.3795 0.5877 0.0112 0.024 Uiso 1 1 calc R . .
C11 C -0.2107(10) 0.6301(9) 0.0569(5) 0.0196(15) Uani 1 1 d U . .
C12 C -0.0779(11) 0.6763(10) 0.0371(5) 0.0295(16) Uani 1 1 d U . .
H12A H -0.0244 0.6856 0.0741 0.035 Uiso 1 1 calc RU . .
C13 C -0.2552(10) 0.5922(8) 0.1360(4) 0.0192(15) Uani 1 1 d U . .
C14 C -0.2992(11) 0.6120(9) -0.1298(5) 0.0243(17) Uani 1 1 d U . .
C15 C -0.3679(11) 0.0723(9) 0.2439(5) 0.0271(17) Uani 1 1 d U . .
H15A H -0.4658 0.1440 0.2420 0.033 Uiso 1 1 calc R . .
C16 C -0.2272(10) -0.1524(9) 0.2457(5) 0.0271(17) Uani 1 1 d U . .
H16A H -0.2267 -0.2390 0.2449 0.033 Uiso 1 1 calc R . .
C17 C -0.0818(10) -0.1356(8) 0.2498(5) 0.0216(15) Uani 1 1 d U . .
C18 C -0.0819(10) -0.0058(8) 0.2489(5) 0.0221(15) Uani 1 1 d U . .
H18A H 0.0152 0.0095 0.2492 0.026 Uiso 1 1 calc RU . .
C19 C -0.2275(10) 0.1011(8) 0.2475(5) 0.0200(15) Uani 1 1 d U . .
C20 C -0.2371(10) 0.2441(8) 0.2479(5) 0.0198(15) Uani 1 1 d U . .
C21 C 0.0724(10) -0.2577(8) 0.2540(5) 0.0201(16) Uani 1 1 d U . .
N1 N 0.6418(9) 0.2887(8) 0.4870(4) 0.0273(17) Uani 1 1 d . . .
N2 N -0.0249(11) 0.7071(9) -0.0307(4) 0.038(2) Uani 1 1 d . . .
N3 N -0.3723(9) -0.0489(8) 0.2429(6) 0.043(2) Uani 1 1 d . . .
O1 O 0.0946(8) 0.4293(8) 0.4113(4) 0.0354(17) Uani 1 1 d . . .
O1W O -0.0837(9) 0.2538(7) 0.3951(4) 0.0441(19) Uani 1 1 d . . .
H1WA H -0.0831 0.2795 0.4341 0.053 Uiso 1 1 d RU . .
H1WB H -0.0173 0.1726 0.3996 0.053 Uiso 1 1 d RU . .
O2 O 0.2968(7) 0.3937(6) 0.3315(3) 0.0193(12) Uani 1 1 d . . .
O2W O 0.2018(9) 0.1726(7) 0.3102(4) 0.0419(18) Uani 1 1 d . . .
H2WA H 0.2692 0.1632 0.3416 0.050 Uiso 1 1 d RU . .
H2WB H 0.2535 0.1577 0.2708 0.050 Uiso 1 1 d RU . .
O3 O 0.2341(7) 0.4605(7) 0.6601(4) 0.0293(15) Uani 1 1 d . . .
O4 O 0.4947(7) 0.4104(7) 0.6826(3) 0.0276(14) Uani 1 1 d . . .
O5 O -0.1485(7) 0.5557(6) 0.1805(3) 0.0246(14) Uani 1 1 d . . .
O6 O -0.4021(7) 0.6020(7) 0.1504(4) 0.0328(15) Uani 1 1 d . . .
O7 O -0.4324(7) 0.5893(7) -0.1188(4) 0.0318(15) Uani 1 1 d . . .
O8 O -0.2198(7) 0.6016(6) -0.1895(3) 0.0264(14) Uani 1 1 d . . .
O9 O -0.3758(7) 0.3269(6) 0.2565(4) 0.0263(14) Uani 1 1 d . . .
O10 O -0.1075(7) 0.2678(6) 0.2413(4) 0.0284(15) Uani 1 1 d . . .
O11 O 0.2043(7) -0.2408(6) 0.2535(4) 0.0354(17) Uani 1 1 d . . .
O12 O 0.0627(8) -0.3708(6) 0.2556(4) 0.0308(15) Uani 1 1 d . . .
O13 O 0.2557(9) 0.6949(8) 0.1153(4) 0.046(2) Uani 1 1 d . . .
C22 C 0.2783(18) 0.7297(17) 0.0512(9) 0.076(3) Uiso 1 1 d U . .
H22A H 0.2973 0.6646 0.0237 0.091 Uiso 1 1 calc RU . .
N4 N 0.279(3) 0.854(2) 0.0152(13) 0.142(6) Uiso 1 1 d U . .
C23 C 0.282(3) 0.877(2) -0.0683(13) 0.145(6) Uiso 1 1 d U . .
H23C H 0.3918 0.8650 -0.0853 0.174 Uiso 1 1 d RU . .
H23A H 0.2493 0.8065 -0.0778 0.174 Uiso 1 1 d RU . .
H23B H 0.2114 0.9650 -0.0924 0.174 Uiso 1 1 d RU . .
C24 C 0.314(3) 0.951(2) 0.0514(14) 0.149(6) Uiso 1 1 d U . .
H24A H 0.2959 0.9258 0.1033 0.179 Uiso 1 1 calc RU . .
H24B H 0.2439 1.0427 0.0325 0.179 Uiso 1 1 calc RU . .
H24C H 0.4245 0.9458 0.0416 0.179 Uiso 1 1 calc RU . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O3 2.334(6) 2_566 ?
Sm1 O5 2.404(6) . ?
Sm1 O10 2.445(6) . ?
Sm1 O12 2.485(6) 1_565 ?
Sm1 O8 2.507(6) 2_565 ?
Sm1 O2W 2.509(6) . ?
Sm1 O1W 2.543(7) . ?
Sm1 O1 2.638(6) . ?
Sm1 O2 2.752(6) . ?
Sm1 Sm2 4.0932(9) . ?
Sm2 O6 2.355(6) 1_655 ?
Sm2 O9 2.394(6) 1_655 ?
Sm2 O4 2.402(6) 2_666 ?
Sm2 O13 2.454(7) . ?
Sm2 O2 2.480(6) . ?
Sm2 O7 2.566(6) 2_565 ?
Sm2 O11 2.586(6) 1_565 ?
Sm2 O8 2.680(6) 2_565 ?
Sm2 O12 2.815(6) 1_565 ?
Sm2 C14 2.986(8) 2_565 ?
Sm2 C21 3.058(8) 1_565 ?
C1 N1 1.345(11) . ?
C1 C2 1.393(12) . ?
C1 H1A 0.9300 . ?
C2 C3 1.380(11) . ?
C2 C6 1.494(11) . ?
C3 C4 1.411(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.379(12) . ?
C4 C7 1.493(11) . ?
C5 N1 1.353(11) . ?
C5 H5A 0.9300 . ?
C6 O2 1.268(10) . ?
C6 O1 1.267(10) . ?
C7 O4 1.247(10) . ?
C7 O3 1.285(10) . ?
C8 N2 1.333(12) . ?
C8 C9 1.404(12) . ?
C8 H8A 0.9300 . ?
C9 C10 1.390(12) . ?
C9 C14 1.491(11) . ?
C10 C11 1.396(11) . ?
C10 H10A 0.9300 . ?
C11 C12 1.410(12) . ?
C11 C13 1.495(11) . ?
C12 N2 1.317(12) . ?
C12 H12A 0.9300 . ?
C13 O5 1.224(10) . ?
C13 O6 1.271(10) . ?
C14 O8 1.270(11) . ?
C14 O7 1.271(11) . ?
C14 Sm2 2.985(8) 2_565 ?
C15 N3 1.318(12) . ?
C15 C19 1.394(12) . ?
C15 H15A 0.9300 . ?
C16 N3 1.364(11) . ?
C16 C17 1.374(12) . ?
C16 H16A 0.9300 . ?
C17 C18 1.386(11) . ?
C17 C21 1.513(11) . ?
C18 C19 1.386(11) . ?
C18 H18A 0.9300 . ?
C19 C20 1.506(11) . ?
C20 O10 1.247(10) . ?
C20 O9 1.257(10) . ?
C21 O12 1.238(10) . ?
C21 O11 1.241(10) . ?
C21 Sm2 3.058(8) 1_545 ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8500 . ?
O2W H2WA 0.8499 . ?
O2W H2WB 0.8498 . ?
O3 Sm1 2.334(6) 2_566 ?
O4 Sm2 2.402(6) 2_666 ?
O6 Sm2 2.355(6) 1_455 ?
O7 Sm2 2.566(6) 2_565 ?
O8 Sm1 2.507(6) 2_565 ?
O8 Sm2 2.680(6) 2_565 ?
O9 Sm2 2.394(6) 1_455 ?
O11 Sm2 2.586(6) 1_545 ?
O12 Sm1 2.485(6) 1_545 ?
O12 Sm2 2.815(6) 1_545 ?
O13 C22 1.193(17) . ?
C22 N4 1.34(2) . ?
C22 H22A 0.9300 . ?
N4 C23 1.53(3) . ?
N4 C24 1.51(3) . ?
C23 H23C 0.9600 . ?
C23 H23A 0.9599 . ?
C23 H23B 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 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
O3 Sm1 O5 78.6(2) 2_566 . ?
O3 Sm1 O10 98.7(2) 2_566 . ?
O5 Sm1 O10 73.9(2) . . ?
O3 Sm1 O12 84.3(2) 2_566 1_565 ?
O5 Sm1 O12 72.2(2) . 1_565 ?
O10 Sm1 O12 144.6(2) . 1_565 ?
O3 Sm1 O8 150.0(2) 2_566 2_565 ?
O5 Sm1 O8 78.1(2) . 2_565 ?
O10 Sm1 O8 92.8(2) . 2_565 ?
O12 Sm1 O8 70.7(2) 1_565 2_565 ?
O3 Sm1 O2W 138.9(3) 2_566 . ?
O5 Sm1 O2W 131.6(2) . . ?
O10 Sm1 O2W 71.4(2) . . ?
O12 Sm1 O2W 127.2(2) 1_565 . ?
O8 Sm1 O2W 71.1(2) 2_565 . ?
O3 Sm1 O1W 71.0(2) 2_566 . ?
O5 Sm1 O1W 128.6(2) . . ?
O10 Sm1 O1W 71.0(2) . . ?
O12 Sm1 O1W 140.9(2) 1_565 . ?
O8 Sm1 O1W 138.9(2) 2_565 . ?
O2W Sm1 O1W 68.0(2) . . ?
O3 Sm1 O1 75.4(2) 2_566 . ?
O5 Sm1 O1 140.3(2) . . ?
O10 Sm1 O1 139.2(2) . . ?
O12 Sm1 O1 75.8(2) 1_565 . ?
O8 Sm1 O1 112.57(19) 2_565 . ?
O2W Sm1 O1 86.8(2) . . ?
O1W Sm1 O1 69.0(2) . . ?
O3 Sm1 O2 119.27(19) 2_566 . ?
O5 Sm1 O2 129.72(19) . . ?
O10 Sm1 O2 137.04(18) . . ?
O12 Sm1 O2 64.47(19) 1_565 . ?
O8 Sm1 O2 64.75(18) 2_565 . ?
O2W Sm1 O2 66.9(2) . . ?
O1W Sm1 O2 101.4(2) . . ?
O1 Sm1 O2 48.10(18) . . ?
O3 Sm1 Sm2 124.66(17) 2_566 . ?
O5 Sm1 Sm2 93.91(15) . . ?
O10 Sm1 Sm2 132.08(15) . . ?
O12 Sm1 Sm2 42.48(14) 1_565 . ?
O8 Sm1 Sm2 39.40(13) 2_565 . ?
O2W Sm1 Sm2 85.41(18) . . ?
O1W Sm1 Sm2 137.50(18) . . ?
O1 Sm1 Sm2 77.34(14) . . ?
O2 Sm1 Sm2 36.20(12) . . ?
O6 Sm2 O9 80.5(2) 1_655 1_655 ?
O6 Sm2 O4 83.1(2) 1_655 2_666 ?
O9 Sm2 O4 80.6(2) 1_655 2_666 ?
O6 Sm2 O13 75.0(2) 1_655 . ?
O9 Sm2 O13 140.6(2) 1_655 . ?
O4 Sm2 O13 125.5(3) 2_666 . ?
O6 Sm2 O2 154.1(2) 1_655 . ?
O9 Sm2 O2 76.3(2) 1_655 . ?
O4 Sm2 O2 81.8(2) 2_666 . ?
O13 Sm2 O2 130.9(2) . . ?
O6 Sm2 O7 78.0(2) 1_655 2_565 ?
O9 Sm2 O7 75.2(2) 1_655 2_565 ?
O4 Sm2 O7 151.3(2) 2_666 2_565 ?
O13 Sm2 O7 69.9(3) . 2_565 ?
O2 Sm2 O7 106.6(2) . 2_565 ?
O6 Sm2 O11 102.1(2) 1_655 1_565 ?
O9 Sm2 O11 148.8(2) 1_655 1_565 ?
O4 Sm2 O11 69.1(2) 2_666 1_565 ?
O13 Sm2 O11 67.9(3) . 1_565 ?
O2 Sm2 O11 92.0(2) . 1_565 ?
O7 Sm2 O11 136.0(2) 2_565 1_565 ?
O6 Sm2 O8 126.9(2) 1_655 2_565 ?
O9 Sm2 O8 92.9(2) 1_655 2_565 ?
O4 Sm2 O8 148.0(2) 2_666 2_565 ?
O13 Sm2 O8 78.4(2) . 2_565 ?
O2 Sm2 O8 66.23(18) . 2_565 ?
O7 Sm2 O8 49.76(19) 2_565 2_565 ?
O11 Sm2 O8 108.92(19) 1_565 2_565 ?
O6 Sm2 O12 140.7(2) 1_655 1_565 ?
O9 Sm2 O12 138.7(2) 1_655 1_565 ?
O4 Sm2 O12 101.7(2) 2_666 1_565 ?
O13 Sm2 O12 70.7(2) . 1_565 ?
O2 Sm2 O12 63.54(19) . 1_565 ?
O7 Sm2 O12 106.62(19) 2_565 1_565 ?
O11 Sm2 O12 47.14(19) 1_565 1_565 ?
O8 Sm2 O12 63.39(18) 2_565 1_565 ?
O6 Sm2 C14 101.8(2) 1_655 2_565 ?
O9 Sm2 C14 86.6(2) 1_655 2_565 ?
O4 Sm2 C14 165.4(2) 2_666 2_565 ?
O13 Sm2 C14 69.1(3) . 2_565 ?
O2 Sm2 C14 88.3(2) . 2_565 ?
O7 Sm2 C14 25.0(2) 2_565 2_565 ?
O11 Sm2 C14 122.3(2) 1_565 2_565 ?
O8 Sm2 C14 25.2(2) 2_565 2_565 ?
O12 Sm2 C14 83.3(2) 1_565 2_565 ?
O6 Sm2 C21 120.8(2) 1_655 1_565 ?
O9 Sm2 C21 153.9(2) 1_655 1_565 ?
O4 Sm2 C21 87.0(2) 2_666 1_565 ?
O13 Sm2 C21 64.5(2) . 1_565 ?
O2 Sm2 C21 79.3(2) . 1_565 ?
O7 Sm2 C21 121.3(2) 2_565 1_565 ?
O11 Sm2 C21 23.6(2) 1_565 1_565 ?
O8 Sm2 C21 85.6(2) 2_565 1_565 ?
O12 Sm2 C21 23.9(2) 1_565 1_565 ?
C14 Sm2 C21 101.8(2) 2_565 1_565 ?
O6 Sm2 Sm1 161.55(16) 1_655 . ?
O9 Sm2 Sm1 104.74(15) 1_655 . ?
O4 Sm2 Sm1 115.05(16) 2_666 . ?
O13 Sm2 Sm1 90.78(18) . . ?
O2 Sm2 Sm1 40.96(13) . . ?
O7 Sm2 Sm1 86.20(14) 2_565 . ?
O11 Sm2 Sm1 82.62(15) 1_565 . ?
O8 Sm2 Sm1 36.43(13) 2_565 . ?
O12 Sm2 Sm1 36.59(12) 1_565 . ?
C14 Sm2 Sm1 61.49(18) 2_565 . ?
C21 Sm2 Sm1 60.21(16) 1_565 . ?
N1 C1 C2 123.6(8) . . ?
N1 C1 H1A 118.2 . . ?
C2 C1 H1A 118.2 . . ?
C3 C2 C1 119.2(7) . . ?
C3 C2 C6 122.1(8) . . ?
C1 C2 C6 118.7(7) . . ?
C2 C3 C4 118.1(8) . . ?
C2 C3 H3A 120.9 . . ?
C4 C3 H3A 120.9 . . ?
C5 C4 C3 118.6(7) . . ?
C5 C4 C7 120.9(7) . . ?
C3 C4 C7 120.4(7) . . ?
N1 C5 C4 123.9(8) . . ?
N1 C5 H5A 118.0 . . ?
C4 C5 H5A 118.0 . . ?
O2 C6 O1 120.4(7) . . ?
O2 C6 C2 119.2(7) . . ?
O1 C6 C2 120.4(7) . . ?
O4 C7 O3 124.3(8) . . ?
O4 C7 C4 118.5(7) . . ?
O3 C7 C4 117.1(7) . . ?
N2 C8 C9 122.8(9) . . ?
N2 C8 H8A 118.6 . . ?
C9 C8 H8A 118.6 . . ?
C10 C9 C8 118.8(8) . . ?
C10 C9 C14 119.7(8) . . ?
C8 C9 C14 121.4(8) . . ?
C9 C10 C11 118.5(8) . . ?
C9 C10 H10A 120.7 . . ?
C11 C10 H10A 120.7 . . ?
C10 C11 C12 117.6(8) . . ?
C10 C11 C13 123.0(7) . . ?
C12 C11 C13 119.3(8) . . ?
N2 C12 C11 124.1(8) . . ?
N2 C12 H12A 117.9 . . ?
C11 C12 H12A 117.9 . . ?
O5 C13 O6 126.2(8) . . ?
O5 C13 C11 117.6(7) . . ?
O6 C13 C11 116.1(7) . . ?
O8 C14 O7 120.8(8) . . ?
O8 C14 C9 119.5(8) . . ?
O7 C14 C9 119.6(8) . . ?
O8 C14 Sm2 63.8(4) . 2_565 ?
O7 C14 Sm2 58.7(4) . 2_565 ?
C9 C14 Sm2 163.6(6) . 2_565 ?
N3 C15 C19 124.9(8) . . ?
N3 C15 H15A 117.5 . . ?
C19 C15 H15A 117.5 . . ?
N3 C16 C17 123.5(8) . . ?
N3 C16 H16A 118.3 . . ?
C17 C16 H16A 118.3 . . ?
C16 C17 C18 118.4(8) . . ?
C16 C17 C21 119.3(7) . . ?
C18 C17 C21 122.3(7) . . ?
C19 C18 C17 119.6(8) . . ?
C19 C18 H18A 120.2 . . ?
C17 C18 H18A 120.2 . . ?
C18 C19 C15 117.2(7) . . ?
C18 C19 C20 122.6(7) . . ?
C15 C19 C20 120.3(7) . . ?
O10 C20 O9 126.5(8) . . ?
O10 C20 C19 117.3(7) . . ?
O9 C20 C19 116.2(7) . . ?
O12 C21 O11 122.2(8) . . ?
O12 C21 C17 118.6(7) . . ?
O11 C21 C17 119.2(7) . . ?
O12 C21 Sm2 67.0(5) . 1_545 ?
O11 C21 Sm2 56.4(4) . 1_545 ?
C17 C21 Sm2 165.8(6) . 1_545 ?
C1 N1 C5 116.6(7) . . ?
C12 N2 C8 118.0(8) . . ?
C15 N3 C16 116.4(8) . . ?
C6 O1 Sm1 98.0(5) . . ?
Sm1 O1W H1WA 109.6 . . ?
Sm1 O1W H1WB 109.6 . . ?
H1WA O1W H1WB 108.2 . . ?
C6 O2 Sm2 139.2(5) . . ?
C6 O2 Sm1 92.6(5) . . ?
Sm2 O2 Sm1 102.84(19) . . ?
Sm1 O2W H2WA 109.7 . . ?
Sm1 O2W H2WB 109.6 . . ?
H2WA O2W H2WB 108.2 . . ?
C7 O3 Sm1 157.3(6) . 2_566 ?
C7 O4 Sm2 155.0(5) . 2_666 ?
C13 O5 Sm1 154.8(6) . . ?
C13 O6 Sm2 151.5(6) . 1_455 ?
C14 O7 Sm2 96.3(5) . 2_565 ?
C14 O8 Sm1 163.3(6) . 2_565 ?
C14 O8 Sm2 91.0(5) . 2_565 ?
Sm1 O8 Sm2 104.2(2) 2_565 2_565 ?
C20 O9 Sm2 155.4(6) . 1_455 ?
C20 O10 Sm1 136.6(6) . . ?
C21 O11 Sm2 100.1(5) . 1_545 ?
C21 O12 Sm1 165.6(6) . 1_545 ?
C21 O12 Sm2 89.1(5) . 1_545 ?
Sm1 O12 Sm2 100.93(19) 1_545 1_545 ?
C22 O13 Sm2 140.1(9) . . ?
O13 C22 N4 125.9(18) . . ?
O13 C22 H22A 117.1 . . ?
N4 C22 H22A 117.1 . . ?
C22 N4 C23 114(2) . . ?
C22 N4 C24 123(2) . . ?
C23 N4 C24 121(2) . . ?
N4 C23 H23C 107.9 . . ?
N4 C23 H23A 105.3 . . ?
H23C C23 H23A 110.2 . . ?
N4 C23 H23B 113.7 . . ?
H23C C23 H23B 110.2 . . ?
H23A C23 H23B 109.5 . . ?
N4 C24 H24A 109.5 . . ?
N4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N4 C24 H24C 109.4 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         3.185
_refine_diff_density_min         -2.779
_refine_diff_density_rms         0.258


# 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 -0.028 0.000 0.500 223 74 ' '
2 0.314 0.029 0.188 15 8 ' '
3 0.355 0.888 0.313 5 2 ' '
4 0.647 0.107 0.692 6 3 ' '
5 0.686 0.966 0.815 15 8 ' '
_platon_squeeze_details          ?
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Tb
_database_code_depnum_ccdc_archive 'CCDC 1472128'
_audit_update_record             
;
2016-04-04 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H28 N4 O19 Tb2'
_chemical_formula_weight         994.34

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   10.0739(19)
_cell_length_b                   20.130(4)
_cell_length_c                   17.349(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.934(8)
_cell_angle_gamma                90.00
_cell_volume                     3215.6(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5165
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      28.39

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    4.452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4696
_exptl_absorpt_correction_T_max  0.7171
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12854
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         25.20
_reflns_number_total             5747
_reflns_number_gt                4950
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0263P)²+0.4398P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    contr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5747
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0580
_refine_ls_wR_factor_gt          0.0555
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.11373(2) -0.045579(10) -0.318878(11) 0.01506(6) Uani 1 1 d . . .
Tb2 Tb -0.06726(2) -0.132491(10) -0.172895(12) 0.01636(6) Uani 1 1 d . . .
O1 O 0.0397(3) -0.21080(15) -0.23062(19) 0.0314(8) Uani 1 1 d . . .
O1W O 0.0885(4) 0.05166(15) -0.39964(18) 0.0345(8) Uani 1 1 d . . .
H1 H 0.0051 0.0522 -0.4403 0.052 Uiso 1 1 d R . .
H2 H 0.1522 0.0519 -0.4201 0.052 Uiso 1 1 d R . .
O2 O 0.0973(3) -0.16329(14) -0.32997(18) 0.0276(8) Uani 1 1 d . . .
O2W O 0.3072(3) 0.02983(16) -0.24020(18) 0.0312(8) Uani 1 1 d . . .
H3 H 0.3353 0.0223 -0.1877 0.047 Uiso 1 1 d R . .
H4 H 0.2762 0.0696 -0.2497 0.047 Uiso 1 1 d R . .
O3 O -0.0036(3) -0.46440(15) -0.23809(19) 0.0275(7) Uani 1 1 d . . .
O3W O -0.2488(4) -0.21521(16) -0.2381(2) 0.0465(9) Uani 1 1 d . . .
H5 H -0.2227 -0.2396 -0.2695 0.070 Uiso 1 1 d R . .
H6 H -0.2586 -0.2389 -0.2002 0.070 Uiso 1 1 d R . .
O4 O 0.0545(3) -0.51506(15) -0.33547(18) 0.0276(7) Uani 1 1 d . . .
O5 O 0.1555(3) -0.07550(15) -0.44756(17) 0.0252(7) Uani 1 1 d . . .
O6 O 0.3400(3) -0.08305(16) -0.32511(17) 0.0267(7) Uani 1 1 d . . .
O7 O -0.1489(3) -0.09446(15) -0.31067(17) 0.0264(7) Uani 1 1 d . . .
O8 O -0.1260(3) -0.05813(15) -0.42412(17) 0.0261(7) Uani 1 1 d . . .
O9 O 0.6953(3) -0.09063(17) -0.17836(17) 0.0303(8) Uani 1 1 d . . .
O10 O 0.8749(3) -0.10472(17) -0.05419(18) 0.0313(8) Uani 1 1 d . . .
O11 O 0.1849(3) -0.08543(15) -0.18111(16) 0.0223(7) Uani 1 1 d . . .
O12 O 0.1715(3) -0.10827(16) -0.06084(17) 0.0239(7) Uani 1 1 d . . .
O13 O -0.1033(4) -0.31883(17) -0.1437(2) 0.0460(9) Uani 1 1 d . . .
O14 O 0.0047(4) -0.22546(15) -0.07933(18) 0.0390(9) Uani 1 1 d . . .
N1 N 0.1583(4) -0.34303(17) -0.4175(2) 0.0205(8) Uani 1 1 d . . .
N2 N 0.4356(4) -0.07788(19) -0.5727(2) 0.0264(9) Uani 1 1 d . . .
N3 N 0.6126(4) -0.0761(2) 0.0737(2) 0.0286(9) Uani 1 1 d . . .
C1 C 0.1436(4) -0.2840(2) -0.3861(2) 0.0209(9) Uani 1 1 d . . .
H1A H 0.1667 -0.2454 -0.4073 0.025 Uiso 1 1 calc R . .
C2 C 0.0947(4) -0.2798(2) -0.3227(2) 0.0197(9) Uani 1 1 d . . .
C3 C 0.0615(4) -0.3387(2) -0.2916(3) 0.0185(9) Uani 1 1 d . . .
H3A H 0.0280 -0.3372 -0.2490 0.022 Uiso 1 1 calc R . .
C4 C 0.0783(4) -0.3991(2) -0.3241(2) 0.0198(9) Uani 1 1 d . . .
C5 C 0.1261(4) -0.3998(2) -0.3889(2) 0.0209(9) Uani 1 1 d . . .
H5A H 0.1358 -0.4400 -0.4125 0.025 Uiso 1 1 calc R . .
C6 C 0.0753(4) -0.2121(2) -0.2916(3) 0.0217(10) Uani 1 1 d . . .
C7 C 0.0407(4) -0.4651(2) -0.2963(3) 0.0207(10) Uani 1 1 d . . .
C8 C 0.3455(4) -0.0819(2) -0.5332(3) 0.0230(10) Uani 1 1 d . . .
H8A H 0.2460 -0.0814 -0.5658 0.028 Uiso 1 1 calc R . .
C9 C 0.3927(4) -0.0866(2) -0.4465(2) 0.0198(9) Uani 1 1 d . . .
C10 C 0.5420(4) -0.0889(2) -0.3976(3) 0.0196(9) Uani 1 1 d . . .
H10A H 0.5774 -0.0940 -0.3394 0.024 Uiso 1 1 calc R . .
C11 C 0.6364(4) -0.0835(2) -0.4370(2) 0.0179(9) Uani 1 1 d . . .
C12 C 0.5781(4) -0.0772(2) -0.5242(3) 0.0223(10) Uani 1 1 d . . .
H12A H 0.6418 -0.0723 -0.5504 0.027 Uiso 1 1 calc R . .
C13 C 0.2890(4) -0.0826(2) -0.4041(2) 0.0180(9) Uani 1 1 d . . .
C14 C -0.2031(4) -0.0793(2) -0.3883(3) 0.0208(10) Uani 1 1 d . . .
C15 C 0.6958(5) -0.0789(2) 0.0300(3) 0.0290(11) Uani 1 1 d . . .
H15A H 0.7960 -0.0768 0.0599 0.035 Uiso 1 1 calc R . .
C16 C 0.6420(4) -0.0847(2) -0.0567(3) 0.0215(10) Uani 1 1 d . . .
C17 C 0.4936(4) -0.0866(2) -0.1016(2) 0.0211(9) Uani 1 1 d . . .
H17A H 0.4537 -0.0885 -0.1602 0.025 Uiso 1 1 calc R . .
C18 C 0.4045(4) -0.0857(2) -0.0579(2) 0.0185(9) Uani 1 1 d . . .
C19 C 0.4704(4) -0.0802(2) 0.0296(2) 0.0245(10) Uani 1 1 d . . .
H19A H 0.4109 -0.0793 0.0589 0.029 Uiso 1 1 calc R . .
C20 C 0.7436(4) -0.0929(2) -0.0996(3) 0.0208(9) Uani 1 1 d . . .
C21 C 0.2446(4) -0.0926(2) -0.1022(2) 0.0191(9) Uani 1 1 d . . .
C22 C -0.0133(6) -0.2865(3) -0.0853(3) 0.0462(14) Uani 1 1 d . . .
H22 H 0.0492 -0.3113 -0.0398 0.055 Uiso 1 1 calc R . .
O4W O 0.4250(4) -0.45903(19) -0.2447(2) 0.0505(10) Uani 1 1 d . . .
H7 H 0.3758 -0.4292 -0.2792 0.076 Uiso 1 1 d R . .
H8 H 0.5112 -0.4566 -0.2416 0.076 Uiso 1 1 d R . .
O5W O 0.4634(4) -0.21695(19) -0.2847(2) 0.0540(10) Uani 1 1 d . . .
H9 H 0.4291 -0.1786 -0.2834 0.081 Uiso 1 1 d R . .
H10 H 0.4370 -0.2444 -0.2564 0.081 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O11 2.341(3) . ?
Tb1 O1W 2.360(3) . ?
Tb1 O2 2.378(3) . ?
Tb1 O8 2.378(3) . ?
Tb1 O3 2.402(3) 2_554 ?
Tb1 O2W 2.410(3) . ?
Tb1 O6 2.444(3) . ?
Tb1 O5 2.507(3) . ?
Tb1 C13 2.824(4) . ?
Tb1 O7 2.880(3) . ?
Tb1 C14 2.996(4) . ?
Tb2 O7 2.320(3) . ?
Tb2 O1 2.350(3) . ?
Tb2 O4 2.369(3) 2_554 ?
Tb2 O14 2.389(3) . ?
Tb2 O3W 2.391(3) . ?
Tb2 O10 2.422(3) 1_455 ?
Tb2 O12 2.451(3) . ?
Tb2 O9 2.502(3) 1_455 ?
Tb2 O11 2.768(3) . ?
Tb2 C20 2.802(4) 1_455 ?
Tb2 C21 2.982(4) . ?
O1 C6 1.248(5) . ?
O1W H1 0.8499 . ?
O1W H2 0.8500 . ?
O2 C6 1.256(5) . ?
O2W H3 0.8501 . ?
O2W H4 0.8501 . ?
O3 C7 1.260(5) . ?
O3 Tb1 2.402(3) 2_544 ?
O3W H5 0.8500 . ?
O3W H6 0.8499 . ?
O4 C7 1.253(5) . ?
O4 Tb2 2.369(3) 2_544 ?
O5 C13 1.255(5) . ?
O6 C13 1.254(5) . ?
O7 C14 1.267(5) . ?
O8 C14 1.250(5) . ?
O9 C20 1.252(5) . ?
O9 Tb2 2.502(3) 1_655 ?
O10 C20 1.257(5) . ?
O10 Tb2 2.422(3) 1_655 ?
O11 C21 1.260(5) . ?
O12 C21 1.259(5) . ?
O13 C22 1.236(6) . ?
O14 C22 1.241(6) . ?
N1 C5 1.337(5) . ?
N1 C1 1.340(5) . ?
N2 C8 1.345(5) . ?
N2 C12 1.337(5) . ?
N3 C19 1.324(5) . ?
N3 C15 1.340(5) . ?
C1 C2 1.378(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.398(6) . ?
C2 C6 1.508(6) . ?
C3 C4 1.379(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.391(5) . ?
C4 C7 1.512(6) . ?
C5 H5A 0.9300 . ?
C8 C9 1.384(5) . ?
C8 H8A 0.9300 . ?
C9 C10 1.396(5) . ?
C9 C13 1.504(5) . ?
C10 C11 1.383(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.388(5) . ?
C11 C14 1.492(5) 1_655 ?
C12 H12A 0.9300 . ?
C14 C11 1.492(5) 1_455 ?
C15 C16 1.382(6) . ?
C15 H15A 0.9300 . ?
C16 C17 1.378(6) . ?
C16 C20 1.498(6) . ?
C17 C18 1.391(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.392(5) . ?
C18 C21 1.483(5) . ?
C19 H19A 0.9300 . ?
C20 Tb2 2.802(4) 1_655 ?
C22 H22 0.9300 . ?
O4W H7 0.8499 . ?
O4W H8 0.8500 . ?
O5W H9 0.8500 . ?
O5W H10 0.8499 . ?

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
O11 Tb1 O1W 143.61(10) . . ?
O11 Tb1 O2 73.95(10) . . ?
O1W Tb1 O2 142.31(10) . . ?
O11 Tb1 O8 122.85(10) . . ?
O1W Tb1 O8 78.52(11) . . ?
O2 Tb1 O8 79.42(10) . . ?
O11 Tb1 O3 79.29(10) . 2_554 ?
O1W Tb1 O3 73.94(11) . 2_554 ?
O2 Tb1 O3 133.07(10) . 2_554 ?
O8 Tb1 O3 83.87(11) . 2_554 ?
O11 Tb1 O2W 78.19(10) . . ?
O1W Tb1 O2W 71.43(11) . . ?
O2 Tb1 O2W 133.42(11) . . ?
O8 Tb1 O2W 146.93(11) . . ?
O3 Tb1 O2W 74.97(10) 2_554 . ?
O11 Tb1 O6 91.99(9) . . ?
O1W Tb1 O6 96.18(11) . . ?
O2 Tb1 O6 74.00(10) . . ?
O8 Tb1 O6 127.46(10) . . ?
O3 Tb1 O6 145.38(10) 2_554 . ?
O2W Tb1 O6 70.44(10) . . ?
O11 Tb1 O5 137.26(10) . . ?
O1W Tb1 O5 71.77(10) . . ?
O2 Tb1 O5 73.73(10) . . ?
O8 Tb1 O5 77.04(9) . . ?
O3 Tb1 O5 143.35(10) 2_554 . ?
O2W Tb1 O5 105.46(10) . . ?
O6 Tb1 O5 52.43(9) . . ?
O11 Tb1 C13 116.53(11) . . ?
O1W Tb1 C13 81.25(12) . . ?
O2 Tb1 C13 74.47(11) . . ?
O8 Tb1 C13 103.06(11) . . ?
O3 Tb1 C13 152.41(11) 2_554 . ?
O2W Tb1 C13 85.94(11) . . ?
O6 Tb1 C13 26.28(10) . . ?
O5 Tb1 C13 26.37(10) . . ?
O11 Tb1 O7 74.88(9) . . ?
O1W Tb1 O7 115.65(10) . . ?
O2 Tb1 O7 68.19(9) . . ?
O8 Tb1 O7 48.26(9) . . ?
O3 Tb1 O7 67.98(9) 2_554 . ?
O2W Tb1 O7 137.33(9) . . ?
O6 Tb1 O7 142.04(10) . . ?
O5 Tb1 O7 116.83(9) . . ?
C13 Tb1 O7 135.86(10) . . ?
O11 Tb1 C14 99.64(11) . . ?
O1W Tb1 C14 96.25(11) . . ?
O2 Tb1 C14 73.37(11) . . ?
O8 Tb1 C14 23.49(10) . . ?
O3 Tb1 C14 74.04(11) 2_554 . ?
O2W Tb1 C14 148.77(11) . . ?
O6 Tb1 C14 140.58(10) . . ?
O5 Tb1 C14 97.12(10) . . ?
C13 Tb1 C14 121.33(11) . . ?
O7 Tb1 C14 24.81(9) . . ?
O7 Tb2 O1 79.30(10) . . ?
O7 Tb2 O4 73.83(10) . 2_554 ?
O1 Tb2 O4 132.26(10) . 2_554 ?
O7 Tb2 O14 147.31(10) . . ?
O1 Tb2 O14 72.48(11) . . ?
O4 Tb2 O14 138.26(10) 2_554 . ?
O7 Tb2 O3W 81.89(11) . . ?
O1 Tb2 O3W 74.10(12) . . ?
O4 Tb2 O3W 137.40(11) 2_554 . ?
O14 Tb2 O3W 74.87(11) . . ?
O7 Tb2 O10 133.87(10) . 1_455 ?
O1 Tb2 O10 145.80(11) . 1_455 ?
O4 Tb2 O10 75.14(11) 2_554 1_455 ?
O14 Tb2 O10 73.40(11) . 1_455 ?
O3W Tb2 O10 99.29(12) . 1_455 ?
O7 Tb2 O12 125.11(10) . . ?
O1 Tb2 O12 89.97(11) . . ?
O4 Tb2 O12 75.02(10) 2_554 . ?
O14 Tb2 O12 71.79(11) . . ?
O3W Tb2 O12 146.08(11) . . ?
O10 Tb2 O12 77.11(9) 1_455 . ?
O7 Tb2 O9 85.19(10) . 1_455 ?
O1 Tb2 O9 143.74(11) . 1_455 ?
O4 Tb2 O9 72.16(10) 2_554 1_455 ?
O14 Tb2 O9 108.14(11) . 1_455 ?
O3W Tb2 O9 71.37(11) . 1_455 ?
O10 Tb2 O9 53.01(9) 1_455 1_455 ?
O12 Tb2 O9 125.36(10) . 1_455 ?
O7 Tb2 O11 77.47(9) . . ?
O1 Tb2 O11 67.60(10) . . ?
O4 Tb2 O11 68.49(9) 2_554 . ?
O14 Tb2 O11 105.75(11) . . ?
O3W Tb2 O11 139.07(11) . . ?
O10 Tb2 O11 120.47(9) 1_455 . ?
O12 Tb2 O11 49.24(8) . . ?
O9 Tb2 O11 140.01(10) 1_455 . ?
O7 Tb2 C20 110.60(11) . 1_455 ?
O1 Tb2 C20 153.91(11) . 1_455 ?
O4 Tb2 C20 73.62(11) 2_554 1_455 ?
O14 Tb2 C20 89.39(12) . 1_455 ?
O3W Tb2 C20 83.27(12) . 1_455 ?
O10 Tb2 C20 26.60(10) 1_455 1_455 ?
O12 Tb2 C20 102.27(11) . 1_455 ?
O9 Tb2 C20 26.54(10) 1_455 1_455 ?
O11 Tb2 C20 137.14(10) . 1_455 ?
O7 Tb2 C21 102.05(11) . . ?
O1 Tb2 C21 76.56(11) . . ?
O4 Tb2 C21 71.57(11) 2_554 . ?
O14 Tb2 C21 87.32(12) . . ?
O3W Tb2 C21 149.10(12) . . ?
O10 Tb2 C21 99.48(11) 1_455 . ?
O12 Tb2 C21 24.38(9) . . ?
O9 Tb2 C21 139.15(11) 1_455 . ?
O11 Tb2 C21 24.97(9) . . ?
C20 Tb2 C21 122.23(11) 1_455 . ?
C6 O1 Tb2 135.6(3) . . ?
Tb1 O1W H1 109.6 . . ?
Tb1 O1W H2 109.6 . . ?
H1 O1W H2 108.2 . . ?
C6 O2 Tb1 139.3(3) . . ?
Tb1 O2W H3 109.6 . . ?
Tb1 O2W H4 109.5 . . ?
H3 O2W H4 108.2 . . ?
C7 O3 Tb1 134.1(3) . 2_544 ?
Tb2 O3W H5 109.3 . . ?
Tb2 O3W H6 109.4 . . ?
H5 O3W H6 109.5 . . ?
C7 O4 Tb2 141.6(3) . 2_544 ?
C13 O5 Tb1 91.1(2) . . ?
C13 O6 Tb1 94.0(2) . . ?
C14 O7 Tb2 173.5(3) . . ?
C14 O7 Tb1 82.8(2) . . ?
Tb2 O7 Tb1 102.42(10) . . ?
C14 O8 Tb1 107.2(3) . . ?
C20 O9 Tb2 90.2(2) . 1_655 ?
C20 O10 Tb2 93.8(2) . 1_655 ?
C21 O11 Tb1 164.1(3) . . ?
C21 O11 Tb2 87.1(2) . . ?
Tb1 O11 Tb2 105.23(10) . . ?
C21 O12 Tb2 102.2(2) . . ?
C22 O14 Tb2 136.5(3) . . ?
C5 N1 C1 121.5(4) . . ?
C8 N2 C12 116.9(4) . . ?
C19 N3 C15 116.6(4) . . ?
N1 C1 C2 120.9(4) . . ?
N1 C1 H1A 119.5 . . ?
C2 C1 H1A 119.5 . . ?
C1 C2 C3 118.3(4) . . ?
C1 C2 C6 118.7(4) . . ?
C3 C2 C6 122.9(4) . . ?
C4 C3 C2 120.2(4) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C3 C4 C5 118.6(4) . . ?
C3 C4 C7 123.8(4) . . ?
C5 C4 C7 117.6(4) . . ?
N1 C5 C4 120.5(4) . . ?
N1 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
O1 C6 O2 127.3(4) . . ?
O1 C6 C2 116.4(4) . . ?
O2 C6 C2 116.2(4) . . ?
O4 C7 O3 126.6(4) . . ?
O4 C7 C4 115.8(4) . . ?
O3 C7 C4 117.5(4) . . ?
N2 C8 C9 123.6(4) . . ?
N2 C8 H8A 118.2 . . ?
C9 C8 H8A 118.2 . . ?
C8 C9 C10 118.2(4) . . ?
C8 C9 C13 121.7(4) . . ?
C10 C9 C13 119.7(4) . . ?
C11 C10 C9 119.0(4) . . ?
C11 C10 H10A 120.5 . . ?
C9 C10 H10A 120.5 . . ?
C12 C11 C10 118.3(4) . . ?
C12 C11 C14 119.7(4) . 1_655 ?
C10 C11 C14 121.9(4) . 1_655 ?
N2 C12 C11 123.9(4) . . ?
N2 C12 H12A 118.1 . . ?
C11 C12 H12A 118.1 . . ?
O5 C13 O6 121.4(4) . . ?
O5 C13 C9 120.0(4) . . ?
O6 C13 C9 118.4(4) . . ?
O5 C13 Tb1 62.6(2) . . ?
O6 C13 Tb1 59.7(2) . . ?
C9 C13 Tb1 167.4(3) . . ?
O8 C14 O7 121.6(4) . . ?
O8 C14 C11 119.0(4) . 1_455 ?
O7 C14 C11 119.3(4) . 1_455 ?
O8 C14 Tb1 49.3(2) . . ?
O7 C14 Tb1 72.4(2) . . ?
C11 C14 Tb1 166.6(3) 1_455 . ?
N3 C15 C16 124.1(4) . . ?
N3 C15 H15A 118.0 . . ?
C16 C15 H15A 118.0 . . ?
C15 C16 C17 118.3(4) . . ?
C15 C16 C20 120.3(4) . . ?
C17 C16 C20 121.3(4) . . ?
C16 C17 C18 118.9(4) . . ?
C16 C17 H17A 120.5 . . ?
C18 C17 H17A 120.5 . . ?
C19 C18 C17 117.9(4) . . ?
C19 C18 C21 120.7(4) . . ?
C17 C18 C21 121.4(4) . . ?
N3 C19 C18 124.1(4) . . ?
N3 C19 H19A 118.0 . . ?
C18 C19 H19A 118.0 . . ?
O10 C20 O9 122.4(4) . . ?
O10 C20 C16 117.8(4) . . ?
O9 C20 C16 119.7(4) . . ?
O10 C20 Tb2 59.6(2) . 1_655 ?
O9 C20 Tb2 63.2(2) . 1_655 ?
C16 C20 Tb2 169.6(3) . 1_655 ?
O12 C21 O11 121.0(4) . . ?
O12 C21 C18 119.4(3) . . ?
O11 C21 C18 119.5(4) . . ?
O12 C21 Tb2 53.5(2) . . ?
O11 C21 Tb2 68.0(2) . . ?
C18 C21 Tb2 168.4(3) . . ?
O13 C22 O14 128.5(5) . . ?
O13 C22 H22 115.7 . . ?
O14 C22 H22 115.7 . . ?
H7 O4W H8 107.0 . . ?
H9 O5W H10 110.4 . . ?

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
O7 Tb2 O1 C6 23.5(4) . . . . ?
O4 Tb2 O1 C6 -32.9(5) 2_554 . . . ?
O14 Tb2 O1 C6 -173.3(4) . . . . ?
O3W Tb2 O1 C6 108.0(4) . . . . ?
O10 Tb2 O1 C6 -168.9(4) 1_455 . . . ?
O12 Tb2 O1 C6 -102.4(4) . . . . ?
O9 Tb2 O1 C6 89.8(4) 1_455 . . . ?
O11 Tb2 O1 C6 -57.3(4) . . . . ?
C20 Tb2 O1 C6 138.8(4) 1_455 . . . ?
C21 Tb2 O1 C6 -81.8(4) . . . . ?
O11 Tb1 O2 C6 28.1(4) . . . . ?
O1W Tb1 O2 C6 -155.8(4) . . . . ?
O8 Tb1 O2 C6 -100.8(4) . . . . ?
O3 Tb1 O2 C6 -29.6(5) 2_554 . . . ?
O2W Tb1 O2 C6 83.7(4) . . . . ?
O6 Tb1 O2 C6 125.0(4) . . . . ?
O5 Tb1 O2 C6 179.8(4) . . . . ?
C13 Tb1 O2 C6 152.3(4) . . . . ?
O7 Tb1 O2 C6 -51.7(4) . . . . ?
C14 Tb1 O2 C6 -77.4(4) . . . . ?
O11 Tb1 O5 C13 -45.5(3) . . . . ?
O1W Tb1 O5 C13 107.7(3) . . . . ?
O2 Tb1 O5 C13 -87.8(2) . . . . ?
O8 Tb1 O5 C13 -170.3(3) . . . . ?
O3 Tb1 O5 C13 129.2(2) 2_554 . . . ?
O2W Tb1 O5 C13 43.7(3) . . . . ?
O6 Tb1 O5 C13 -5.7(2) . . . . ?
O7 Tb1 O5 C13 -142.2(2) . . . . ?
C14 Tb1 O5 C13 -158.1(2) . . . . ?
O11 Tb1 O6 C13 159.9(3) . . . . ?
O1W Tb1 O6 C13 -55.6(3) . . . . ?
O2 Tb1 O6 C13 87.2(3) . . . . ?
O8 Tb1 O6 C13 24.6(3) . . . . ?
O3 Tb1 O6 C13 -126.2(3) 2_554 . . . ?
O2W Tb1 O6 C13 -123.4(3) . . . . ?
O5 Tb1 O6 C13 5.7(2) . . . . ?
O7 Tb1 O6 C13 92.2(3) . . . . ?
C14 Tb1 O6 C13 52.1(3) . . . . ?
O1 Tb2 O7 C14 73(3) . . . . ?
O4 Tb2 O7 C14 -147(3) 2_554 . . . ?
O14 Tb2 O7 C14 43(3) . . . . ?
O3W Tb2 O7 C14 -2(3) . . . . ?
O10 Tb2 O7 C14 -97(3) 1_455 . . . ?
O12 Tb2 O7 C14 155(2) . . . . ?
O9 Tb2 O7 C14 -74(3) 1_455 . . . ?
O11 Tb2 O7 C14 142(3) . . . . ?
C20 Tb2 O7 C14 -82(3) 1_455 . . . ?
C21 Tb2 O7 C14 147(3) . . . . ?
O1 Tb2 O7 Tb1 -69.18(11) . . . . ?
O4 Tb2 O7 Tb1 70.94(10) 2_554 . . . ?
O14 Tb2 O7 Tb1 -99.7(2) . . . . ?
O3W Tb2 O7 Tb1 -144.43(12) . . . . ?
O10 Tb2 O7 Tb1 120.46(13) 1_455 . . . ?
O12 Tb2 O7 Tb1 13.14(16) . . . . ?
O9 Tb2 O7 Tb1 143.74(12) 1_455 . . . ?
O11 Tb2 O7 Tb1 0.00(8) . . . . ?
C20 Tb2 O7 Tb1 135.94(11) 1_455 . . . ?
C21 Tb2 O7 Tb1 4.42(12) . . . . ?
O11 Tb1 O7 C14 -176.0(3) . . . . ?
O1W Tb1 O7 C14 41.3(3) . . . . ?
O2 Tb1 O7 C14 -97.5(2) . . . . ?
O8 Tb1 O7 C14 -2.3(2) . . . . ?
O3 Tb1 O7 C14 99.7(2) 2_554 . . . ?
O2W Tb1 O7 C14 131.3(2) . . . . ?
O6 Tb1 O7 C14 -102.7(3) . . . . ?
O5 Tb1 O7 C14 -40.3(3) . . . . ?
C13 Tb1 O7 C14 -63.3(3) . . . . ?
O11 Tb1 O7 Tb2 0.00(10) . . . . ?
O1W Tb1 O7 Tb2 -142.68(11) . . . . ?
O2 Tb1 O7 Tb2 78.44(12) . . . . ?
O8 Tb1 O7 Tb2 173.73(17) . . . . ?
O3 Tb1 O7 Tb2 -84.35(12) 2_554 . . . ?
O2W Tb1 O7 Tb2 -52.71(18) . . . . ?
O6 Tb1 O7 Tb2 73.27(16) . . . . ?
O5 Tb1 O7 Tb2 135.72(10) . . . . ?
C13 Tb1 O7 Tb2 112.71(14) . . . . ?
C14 Tb1 O7 Tb2 176.0(3) . . . . ?
O11 Tb1 O8 C14 9.6(3) . . . . ?
O1W Tb1 O8 C14 -138.3(3) . . . . ?
O2 Tb1 O8 C14 72.5(3) . . . . ?
O3 Tb1 O8 C14 -63.5(3) 2_554 . . . ?
O2W Tb1 O8 C14 -113.4(3) . . . . ?
O6 Tb1 O8 C14 132.7(3) . . . . ?
O5 Tb1 O8 C14 148.0(3) . . . . ?
C13 Tb1 O8 C14 143.7(3) . . . . ?
O7 Tb1 O8 C14 2.4(2) . . . . ?
O1W Tb1 O11 C21 -26.5(11) . . . . ?
O2 Tb1 O11 C21 149.4(10) . . . . ?
O8 Tb1 O11 C21 -145.0(10) . . . . ?
O3 Tb1 O11 C21 -69.6(10) 2_554 . . . ?
O2W Tb1 O11 C21 7.1(10) . . . . ?
O6 Tb1 O11 C21 76.7(10) . . . . ?
O5 Tb1 O11 C21 107.2(10) . . . . ?
C13 Tb1 O11 C21 86.5(10) . . . . ?
O7 Tb1 O11 C21 -139.4(10) . . . . ?
C14 Tb1 O11 C21 -141.2(10) . . . . ?
O1W Tb1 O11 Tb2 112.90(17) . . . . ?
O2 Tb1 O11 Tb2 -71.17(11) . . . . ?
O8 Tb1 O11 Tb2 -5.57(15) . . . . ?
O3 Tb1 O11 Tb2 69.87(11) 2_554 . . . ?
O2W Tb1 O11 Tb2 146.57(12) . . . . ?
O6 Tb1 O11 Tb2 -143.88(11) . . . . ?
O5 Tb1 O11 Tb2 -113.36(13) . . . . ?
C13 Tb1 O11 Tb2 -134.10(11) . . . . ?
O7 Tb1 O11 Tb2 0.00(8) . . . . ?
C14 Tb1 O11 Tb2 -1.71(12) . . . . ?
O7 Tb2 O11 C21 169.7(3) . . . . ?
O1 Tb2 O11 C21 -106.8(2) . . . . ?
O4 Tb2 O11 C21 92.4(2) 2_554 . . . ?
O14 Tb2 O11 C21 -43.9(2) . . . . ?
O3W Tb2 O11 C21 -128.8(2) . . . . ?
O10 Tb2 O11 C21 35.8(3) 1_455 . . . ?
O12 Tb2 O11 C21 3.9(2) . . . . ?
O9 Tb2 O11 C21 103.2(2) 1_455 . . . ?
C20 Tb2 O11 C21 62.8(3) 1_455 . . . ?
O7 Tb2 O11 Tb1 0.00(10) . . . . ?
O1 Tb2 O11 Tb1 83.45(12) . . . . ?
O4 Tb2 O11 Tb1 -77.35(12) 2_554 . . . ?
O14 Tb2 O11 Tb1 146.42(11) . . . . ?
O3W Tb2 O11 Tb1 61.52(18) . . . . ?
O10 Tb2 O11 Tb1 -133.86(11) 1_455 . . . ?
O12 Tb2 O11 Tb1 -165.79(17) . . . . ?
O9 Tb2 O11 Tb1 -66.50(16) 1_455 . . . ?
C20 Tb2 O11 Tb1 -106.88(15) 1_455 . . . ?
C21 Tb2 O11 Tb1 -169.7(3) . . . . ?
O7 Tb2 O12 C21 -21.0(3) . . . . ?
O1 Tb2 O12 C21 55.8(3) . . . . ?
O4 Tb2 O12 C21 -78.3(3) 2_554 . . . ?
O14 Tb2 O12 C21 127.4(3) . . . . ?
O3W Tb2 O12 C21 116.4(3) . . . . ?
O10 Tb2 O12 C21 -156.1(3) 1_455 . . . ?
O9 Tb2 O12 C21 -133.0(3) 1_455 . . . ?
O11 Tb2 O12 C21 -4.0(2) . . . . ?
C20 Tb2 O12 C21 -147.4(3) 1_455 . . . ?
O7 Tb2 O14 C22 -20.3(7) . . . . ?
O1 Tb2 O14 C22 -51.9(5) . . . . ?
O4 Tb2 O14 C22 173.2(5) 2_554 . . . ?
O3W Tb2 O14 C22 25.9(5) . . . . ?
O10 Tb2 O14 C22 130.6(6) 1_455 . . . ?
O12 Tb2 O14 C22 -147.8(6) . . . . ?
O9 Tb2 O14 C22 90.0(5) 1_455 . . . ?
O11 Tb2 O14 C22 -111.6(5) . . . . ?
C20 Tb2 O14 C22 109.1(5) 1_455 . . . ?
C21 Tb2 O14 C22 -128.6(5) . . . . ?
C5 N1 C1 C2 0.1(6) . . . . ?
N1 C1 C2 C3 0.3(6) . . . . ?
N1 C1 C2 C6 -178.0(4) . . . . ?
C1 C2 C3 C4 0.2(6) . . . . ?
C6 C2 C3 C4 178.4(4) . . . . ?
C2 C3 C4 C5 -1.1(6) . . . . ?
C2 C3 C4 C7 -178.0(4) . . . . ?
C1 N1 C5 C4 -1.0(6) . . . . ?
C3 C4 C5 N1 1.6(6) . . . . ?
C7 C4 C5 N1 178.6(4) . . . . ?
Tb2 O1 C6 O2 20.2(7) . . . . ?
Tb2 O1 C6 C2 -160.1(3) . . . . ?
Tb1 O2 C6 O1 6.8(7) . . . . ?
Tb1 O2 C6 C2 -172.9(3) . . . . ?
C1 C2 C6 O1 -175.6(4) . . . . ?
C3 C2 C6 O1 6.2(6) . . . . ?
C1 C2 C6 O2 4.2(6) . . . . ?
C3 C2 C6 O2 -174.1(4) . . . . ?
Tb2 O4 C7 O3 -16.5(7) 2_544 . . . ?
Tb2 O4 C7 C4 165.0(3) 2_544 . . . ?
Tb1 O3 C7 O4 -9.9(7) 2_544 . . . ?
Tb1 O3 C7 C4 168.6(3) 2_544 . . . ?
C3 C4 C7 O4 176.0(4) . . . . ?
C5 C4 C7 O4 -0.9(6) . . . . ?
C3 C4 C7 O3 -2.6(6) . . . . ?
C5 C4 C7 O3 -179.5(4) . . . . ?
C12 N2 C8 C9 -1.4(7) . . . . ?
N2 C8 C9 C10 -1.5(7) . . . . ?
N2 C8 C9 C13 172.4(4) . . . . ?
C8 C9 C10 C11 2.7(6) . . . . ?
C13 C9 C10 C11 -171.3(4) . . . . ?
C9 C10 C11 C12 -1.2(6) . . . . ?
C9 C10 C11 C14 174.3(4) . . . 1_655 ?
C8 N2 C12 C11 3.1(6) . . . . ?
C10 C11 C12 N2 -1.8(7) . . . . ?
C14 C11 C12 N2 -177.5(4) 1_655 . . . ?
Tb1 O5 C13 O6 10.3(4) . . . . ?
Tb1 O5 C13 C9 -165.9(3) . . . . ?
Tb1 O6 C13 O5 -10.6(4) . . . . ?
Tb1 O6 C13 C9 165.7(3) . . . . ?
C8 C9 C13 O5 0.8(6) . . . . ?
C10 C9 C13 O5 174.6(4) . . . . ?
C8 C9 C13 O6 -175.5(4) . . . . ?
C10 C9 C13 O6 -1.7(6) . . . . ?
C8 C9 C13 Tb1 -97.6(13) . . . . ?
C10 C9 C13 Tb1 76.3(14) . . . . ?
O11 Tb1 C13 O5 147.2(2) . . . . ?
O1W Tb1 C13 O5 -66.3(2) . . . . ?
O2 Tb1 C13 O5 84.6(2) . . . . ?
O8 Tb1 C13 O5 9.7(3) . . . . ?
O3 Tb1 C13 O5 -92.3(3) 2_554 . . . ?
O2W Tb1 C13 O5 -138.1(2) . . . . ?
O6 Tb1 C13 O5 169.8(4) . . . . ?
O7 Tb1 C13 O5 51.7(3) . . . . ?
C14 Tb1 C13 O5 25.7(3) . . . . ?
O11 Tb1 C13 O6 -22.6(3) . . . . ?
O1W Tb1 C13 O6 123.9(3) . . . . ?
O2 Tb1 C13 O6 -85.2(2) . . . . ?
O8 Tb1 C13 O6 -160.1(2) . . . . ?
O3 Tb1 C13 O6 97.9(3) 2_554 . . . ?
O2W Tb1 C13 O6 52.1(2) . . . . ?
O5 Tb1 C13 O6 -169.8(4) . . . . ?
O7 Tb1 C13 O6 -118.1(2) . . . . ?
C14 Tb1 C13 O6 -144.1(2) . . . . ?
O11 Tb1 C13 C9 -107.6(13) . . . . ?
O1W Tb1 C13 C9 38.9(13) . . . . ?
O2 Tb1 C13 C9 -170.2(13) . . . . ?
O8 Tb1 C13 C9 114.8(13) . . . . ?
O3 Tb1 C13 C9 12.9(14) 2_554 . . . ?
O2W Tb1 C13 C9 -33.0(13) . . . . ?
O6 Tb1 C13 C9 -85.0(13) . . . . ?
O5 Tb1 C13 C9 105.2(13) . . . . ?
O7 Tb1 C13 C9 156.9(12) . . . . ?
C14 Tb1 C13 C9 130.9(13) . . . . ?
Tb1 O8 C14 O7 -4.7(5) . . . . ?
Tb1 O8 C14 C11 172.0(3) . . . 1_455 ?
Tb2 O7 C14 O8 -139(2) . . . . ?
Tb1 O7 C14 O8 3.8(4) . . . . ?
Tb2 O7 C14 C11 44(3) . . . 1_455 ?
Tb1 O7 C14 C11 -173.0(4) . . . 1_455 ?
Tb2 O7 C14 Tb1 -143(3) . . . . ?
O11 Tb1 C14 O8 -171.8(3) . . . . ?
O1W Tb1 C14 O8 41.0(3) . . . . ?
O2 Tb1 C14 O8 -101.9(3) . . . . ?
O3 Tb1 C14 O8 112.3(3) 2_554 . . . ?
O2W Tb1 C14 O8 105.1(3) . . . . ?
O6 Tb1 C14 O8 -66.7(3) . . . . ?
O5 Tb1 C14 O8 -31.3(3) . . . . ?
C13 Tb1 C14 O8 -42.5(3) . . . . ?
O7 Tb1 C14 O8 -175.8(4) . . . . ?
O11 Tb1 C14 O7 3.9(2) . . . . ?
O1W Tb1 C14 O7 -143.2(2) . . . . ?
O2 Tb1 C14 O7 73.9(2) . . . . ?
O8 Tb1 C14 O7 175.8(4) . . . . ?
O3 Tb1 C14 O7 -71.9(2) 2_554 . . . ?
O2W Tb1 C14 O7 -79.1(3) . . . . ?
O6 Tb1 C14 O7 109.1(2) . . . . ?
O5 Tb1 C14 O7 144.5(2) . . . . ?
C13 Tb1 C14 O7 133.3(2) . . . . ?
O11 Tb1 C14 C11 156.5(12) . . . 1_455 ?
O1W Tb1 C14 C11 9.4(12) . . . 1_455 ?
O2 Tb1 C14 C11 -133.6(13) . . . 1_455 ?
O8 Tb1 C14 C11 -31.7(11) . . . 1_455 ?
O3 Tb1 C14 C11 80.7(12) 2_554 . . 1_455 ?
O2W Tb1 C14 C11 73.4(13) . . . 1_455 ?
O6 Tb1 C14 C11 -98.3(12) . . . 1_455 ?
O5 Tb1 C14 C11 -63.0(12) . . . 1_455 ?
C13 Tb1 C14 C11 -74.2(13) . . . 1_455 ?
O7 Tb1 C14 C11 152.6(14) . . . 1_455 ?
C19 N3 C15 C16 0.9(7) . . . . ?
N3 C15 C16 C17 1.2(7) . . . . ?
N3 C15 C16 C20 -175.1(4) . . . . ?
C15 C16 C17 C18 -2.9(6) . . . . ?
C20 C16 C17 C18 173.4(4) . . . . ?
C16 C17 C18 C19 2.5(6) . . . . ?
C16 C17 C18 C21 -175.5(4) . . . . ?
C15 N3 C19 C18 -1.3(7) . . . . ?
C17 C18 C19 N3 -0.3(7) . . . . ?
C21 C18 C19 N3 177.7(4) . . . . ?
Tb2 O10 C20 O9 -8.3(5) 1_655 . . . ?
Tb2 O10 C20 C16 168.5(3) 1_655 . . . ?
Tb2 O9 C20 O10 8.0(4) 1_655 . . . ?
Tb2 O9 C20 C16 -168.7(4) 1_655 . . . ?
C15 C16 C20 O10 11.1(6) . . . . ?
C17 C16 C20 O10 -165.1(4) . . . . ?
C15 C16 C20 O9 -172.0(4) . . . . ?
C17 C16 C20 O9 11.7(7) . . . . ?
C15 C16 C20 Tb2 84.0(17) . . . 1_655 ?
C17 C16 C20 Tb2 -92.2(16) . . . 1_655 ?
Tb2 O12 C21 O11 7.8(5) . . . . ?
Tb2 O12 C21 C18 -169.1(3) . . . . ?
Tb1 O11 C21 O12 134.3(8) . . . . ?
Tb2 O11 C21 O12 -6.8(4) . . . . ?
Tb1 O11 C21 C18 -48.8(12) . . . . ?
Tb2 O11 C21 C18 170.1(4) . . . . ?
Tb1 O11 C21 Tb2 141.1(10) . . . . ?
C19 C18 C21 O12 -15.9(6) . . . . ?
C17 C18 C21 O12 162.1(4) . . . . ?
C19 C18 C21 O11 167.2(4) . . . . ?
C17 C18 C21 O11 -14.8(6) . . . . ?
C19 C18 C21 Tb2 -65.2(16) . . . . ?
C17 C18 C21 Tb2 112.8(13) . . . . ?
O7 Tb2 C21 O12 162.5(3) . . . . ?
O1 Tb2 C21 O12 -121.7(3) . . . . ?
O4 Tb2 C21 O12 94.3(3) 2_554 . . . ?
O14 Tb2 C21 O12 -49.1(3) . . . . ?
O3W Tb2 C21 O12 -103.1(3) . . . . ?
O10 Tb2 C21 O12 23.6(3) 1_455 . . . ?
O9 Tb2 C21 O12 65.9(3) 1_455 . . . ?
O11 Tb2 C21 O12 172.8(4) . . . . ?
C20 Tb2 C21 O12 38.5(3) 1_455 . . . ?
O7 Tb2 C21 O11 -10.3(3) . . . . ?
O1 Tb2 C21 O11 65.5(2) . . . . ?
O4 Tb2 C21 O11 -78.5(2) 2_554 . . . ?
O14 Tb2 C21 O11 138.1(2) . . . . ?
O3W Tb2 C21 O11 84.1(3) . . . . ?
O10 Tb2 C21 O11 -149.2(2) 1_455 . . . ?
O12 Tb2 C21 O11 -172.8(4) . . . . ?
O9 Tb2 C21 O11 -106.9(2) 1_455 . . . ?
C20 Tb2 C21 O11 -134.3(2) 1_455 . . . ?
O7 Tb2 C21 C18 -142.2(14) . . . . ?
O1 Tb2 C21 C18 -66.4(14) . . . . ?
O4 Tb2 C21 C18 149.6(14) 2_554 . . . ?
O14 Tb2 C21 C18 6.2(14) . . . . ?
O3W Tb2 C21 C18 -47.8(15) . . . . ?
O10 Tb2 C21 C18 78.9(14) 1_455 . . . ?
O12 Tb2 C21 C18 55.3(14) . . . . ?
O9 Tb2 C21 C18 121.2(14) 1_455 . . . ?
O11 Tb2 C21 C18 -131.9(15) . . . . ?
C20 Tb2 C21 C18 93.8(14) 1_455 . . . ?
Tb2 O14 C22 O13 -16.0(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.113
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ho
_database_code_depnum_ccdc_archive 'CCDC 1472129'
_audit_update_record             
;
2016-04-04 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H28 Ho2 N4 O19'
_chemical_formula_weight         1006.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c '

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

_cell_length_a                   10.0690(9)
_cell_length_b                   20.0854(19)
_cell_length_c                   17.3482(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.898(4)
_cell_angle_gamma                90.00
_cell_volume                     3207.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7749
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      27.97

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.084
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1944
_exptl_absorpt_coefficient_mu    4.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4354
_exptl_absorpt_correction_T_max  0.6911
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16272
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.64
_diffrn_reflns_theta_max         25.20
_reflns_number_total             5763
_reflns_number_gt                5095
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0323P)²+0.2064P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    contr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5763
_refine_ls_number_parameters     405
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0645
_refine_ls_wR_factor_gt          0.0630
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.06756(2) -0.367455(9) -0.327150(11) 0.01520(7) Uani 1 1 d . . .
Ho2 Ho -0.11382(2) -0.454620(9) -0.181197(11) 0.01400(7) Uani 1 1 d . . .
O1 O 0.0539(4) -0.48467(14) -0.33593(18) 0.0240(7) Uani 1 1 d . . .
O1W O 0.2454(4) -0.28422(17) -0.2631(2) 0.0469(10) Uani 1 1 d . . .
H1 H 0.2267 -0.2440 -0.2562 0.070 Uiso 1 1 d R . .
H2 H 0.3257 -0.2983 -0.2566 0.070 Uiso 1 1 d R . .
O2 O -0.0028(4) -0.53517(14) -0.23774(19) 0.0252(7) Uani 1 1 d . . .
O2W O -0.3059(3) -0.53013(15) -0.25964(19) 0.0281(7) Uani 1 1 d . . .
H3 H -0.3335 -0.5225 -0.3121 0.042 Uiso 1 1 d R . .
H4 H -0.2745 -0.5699 -0.2500 0.042 Uiso 1 1 d R . .
O3 O 0.0968(4) -0.83707(13) -0.32998(19) 0.0252(8) Uani 1 1 d . . .
O3W O -0.0893(4) -0.55087(14) -0.10013(19) 0.0298(8) Uani 1 1 d . . .
H5 H -0.0061 -0.5511 -0.0593 0.045 Uiso 1 1 d R . .
H6 H -0.1534 -0.5509 -0.0799 0.045 Uiso 1 1 d R . .
O4 O 0.0390(4) -0.78932(14) -0.2306(2) 0.0283(8) Uani 1 1 d . . .
O5 O 0.8457(3) -0.42429(15) -0.05217(18) 0.0229(7) Uani 1 1 d . . .
O6 O 0.6620(3) -0.41752(16) -0.17483(18) 0.0251(7) Uani 1 1 d . . .
O7 O 0.1496(3) -0.40515(15) -0.19016(18) 0.0248(7) Uani 1 1 d . . .
O8 O 0.1252(3) -0.44254(15) -0.07702(18) 0.0247(7) Uani 1 1 d . . .
O9 O -0.1834(3) -0.41477(14) -0.31804(17) 0.0205(7) Uani 1 1 d . . .
O10 O -0.1705(3) -0.39173(15) -0.43811(17) 0.0233(7) Uani 1 1 d . . .
O11 O 0.3035(3) -0.40921(16) -0.32150(18) 0.0279(8) Uani 1 1 d . . .
O12 O 0.1245(3) -0.39440(16) -0.44582(18) 0.0274(7) Uani 1 1 d . . .
O13 O -0.0041(4) -0.27498(15) -0.42021(19) 0.0370(9) Uani 1 1 d . . .
O14 O 0.1040(5) -0.18091(16) -0.3553(2) 0.0430(10) Uani 1 1 d . . .
N1 N 0.1579(4) -0.65700(16) -0.4176(2) 0.0185(8) Uani 1 1 d . . .
N2 N 0.5646(4) -0.42223(19) 0.0731(2) 0.0238(8) Uani 1 1 d . . .
N3 N -0.6122(4) -0.4239(2) -0.5733(2) 0.0286(9) Uani 1 1 d . . .
C1 C 0.1262(5) -0.6006(2) -0.3891(3) 0.0193(9) Uani 1 1 d . . .
H1A H 0.1363 -0.5604 -0.4127 0.023 Uiso 1 1 calc R . .
C2 C 0.0776(5) -0.6008(2) -0.3240(2) 0.0160(9) Uani 1 1 d . . .
C3 C 0.0622(5) -0.6612(2) -0.2915(3) 0.0201(10) Uani 1 1 d . . .
H3A H 0.0302 -0.6627 -0.2482 0.024 Uiso 1 1 calc R . .
C4 C 0.0938(5) -0.7202(2) -0.3224(2) 0.0185(9) Uani 1 1 d . . .
C5 C 0.1429(5) -0.7164(2) -0.3865(3) 0.0195(9) Uani 1 1 d . . .
H5A H 0.1654 -0.7551 -0.4080 0.023 Uiso 1 1 calc R . .
C6 C 0.0403(5) -0.5345(2) -0.2965(3) 0.0191(9) Uani 1 1 d . . .
C7 C 0.0751(5) -0.7880(2) -0.2910(3) 0.0212(10) Uani 1 1 d . . .
C8 C 0.6547(5) -0.4182(2) 0.0334(3) 0.0197(9) Uani 1 1 d . . .
H8A H 0.7542 -0.4186 0.0659 0.024 Uiso 1 1 calc R . .
C9 C 0.6071(5) -0.4135(2) -0.0537(3) 0.0181(9) Uani 1 1 d . . .
C10 C 0.4596(5) -0.4111(2) -0.1023(3) 0.0189(9) Uani 1 1 d . . .
H10A H 0.4249 -0.4060 -0.1605 0.023 Uiso 1 1 calc R . .
C11 C 0.3628(5) -0.4164(2) -0.0632(2) 0.0169(9) Uani 1 1 d . . .
C12 C 0.4217(5) -0.4229(2) 0.0239(3) 0.0211(10) Uani 1 1 d . . .
H12A H 0.3579 -0.4280 0.0500 0.025 Uiso 1 1 calc R . .
C13 C 0.7120(5) -0.4178(2) -0.0956(3) 0.0178(9) Uani 1 1 d . . .
C14 C 0.2025(5) -0.4205(2) -0.1126(2) 0.0169(9) Uani 1 1 d . . .
C15 C -0.4697(5) -0.4193(2) -0.5292(3) 0.0221(10) Uani 1 1 d . . .
H15A H -0.4103 -0.4195 -0.5586 0.026 Uiso 1 1 calc R . .
C16 C -0.4035(5) -0.4143(2) -0.4414(3) 0.0180(9) Uani 1 1 d . . .
C17 C -0.4935(5) -0.4132(2) -0.3976(3) 0.0172(9) Uani 1 1 d . . .
H17A H -0.4540 -0.4112 -0.3390 0.021 Uiso 1 1 calc R . .
C18 C -0.6418(5) -0.4153(2) -0.4430(3) 0.0177(9) Uani 1 1 d . . .
C19 C -0.6960(5) -0.4211(2) -0.5301(3) 0.0273(11) Uani 1 1 d . . .
H19A H -0.7962 -0.4232 -0.5602 0.033 Uiso 1 1 calc R . .
C20 C -0.2439(5) -0.40737(19) -0.3969(2) 0.0150(9) Uani 1 1 d . . .
C21 C 0.2556(5) -0.4070(2) -0.4002(3) 0.0186(9) Uani 1 1 d . . .
C22 C 0.0133(7) -0.2128(3) -0.4136(3) 0.0434(14) Uani 1 1 d . . .
H22 H -0.0504 -0.1877 -0.4584 0.052 Uiso 1 1 calc R . .
O4W O 0.5746(4) -0.04196(18) -0.2548(2) 0.0472(10) Uiso 1 1 d . . .
H7 H 0.5147 -0.0113 -0.2575 0.071 Uiso 1 1 d R . .
H8 H 0.5613 -0.0755 -0.2290 0.071 Uiso 1 1 d R . .
O5W O 0.5372(5) -0.28422(19) -0.2164(2) 0.0535(10) Uiso 1 1 d . . .
H9 H 0.5767 -0.2590 -0.1739 0.080 Uiso 1 1 d R . .
H10 H 0.5559 -0.2685 -0.2564 0.080 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O7 2.305(3) . ?
Ho1 O4 2.343(3) 2_554 ?
Ho1 O1 2.360(3) . ?
Ho1 O1W 2.372(3) . ?
Ho1 O13 2.373(3) . ?
Ho1 O12 2.412(3) . ?
Ho1 O10 2.439(3) . ?
Ho1 O11 2.484(3) . ?
Ho1 O9 2.764(3) . ?
Ho1 C21 2.787(4) . ?
Ho1 C20 2.977(4) . ?
Ho2 O9 2.328(3) . ?
Ho2 O3W 2.344(3) . ?
Ho2 O8 2.365(3) . ?
Ho2 O3 2.369(3) 2_554 ?
Ho2 O2 2.391(3) . ?
Ho2 O2W 2.400(3) . ?
Ho2 O6 2.422(3) 1_455 ?
Ho2 O5 2.507(3) 1_455 ?
Ho2 C13 2.817(4) 1_455 ?
Ho2 O7 2.895(3) . ?
Ho2 C14 2.993(4) . ?
O1 C6 1.251(5) . ?
O1W H1 0.8499 . ?
O1W H2 0.8200 . ?
O2 C6 1.260(5) . ?
O2W H3 0.8501 . ?
O2W H4 0.8499 . ?
O3 C7 1.263(5) . ?
O3 Ho2 2.369(3) 2_544 ?
O3W H5 0.8500 . ?
O3W H6 0.8501 . ?
O4 C7 1.240(5) . ?
O4 Ho1 2.343(3) 2_544 ?
O5 C13 1.255(5) . ?
O5 Ho2 2.507(3) 1_655 ?
O6 C13 1.258(5) . ?
O6 Ho2 2.422(3) 1_655 ?
O7 C14 1.268(5) . ?
O8 C14 1.254(5) . ?
O9 C20 1.261(5) . ?
O10 C20 1.258(5) . ?
O11 C21 1.252(5) . ?
O12 C21 1.259(5) . ?
O13 C22 1.260(6) . ?
O14 C22 1.232(7) . ?
N1 C1 1.325(5) . ?
N1 C5 1.342(5) . ?
N2 C8 1.346(5) . ?
N2 C12 1.343(6) . ?
N3 C15 1.327(6) . ?
N3 C19 1.337(5) . ?
C1 C2 1.401(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.374(6) . ?
C2 C6 1.511(6) . ?
C3 C4 1.389(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.390(5) . ?
C4 C7 1.508(6) . ?
C5 H5A 0.9300 . ?
C8 C9 1.390(6) . ?
C8 H8A 0.9300 . ?
C9 C10 1.380(6) . ?
C9 C13 1.509(5) . ?
C10 C11 1.399(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.388(6) . ?
C11 C14 1.492(6) . ?
C12 H12A 0.9300 . ?
C13 Ho2 2.817(4) 1_655 ?
C15 C16 1.397(6) . ?
C15 H15A 0.9300 . ?
C16 C17 1.399(5) . ?
C16 C20 1.481(6) . ?
C17 C18 1.379(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.388(6) . ?
C18 C21 1.505(6) 1_455 ?
C19 H19A 0.9300 . ?
C21 C18 1.505(6) 1_655 ?
C22 H22 0.9300 . ?
O4W H7 0.8499 . ?
O4W H8 0.8499 . ?
O5W H9 0.8499 . ?
O5W H10 0.8500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Ho1 O4 79.29(11) . 2_554 ?
O7 Ho1 O1 74.10(10) . . ?
O4 Ho1 O1 132.15(10) 2_554 . ?
O7 Ho1 O1W 82.04(12) . . ?
O4 Ho1 O1W 73.58(12) 2_554 . ?
O1 Ho1 O1W 138.31(12) . . ?
O7 Ho1 O13 147.32(10) . . ?
O4 Ho1 O13 72.61(11) 2_554 . ?
O1 Ho1 O13 138.00(10) . . ?
O1W Ho1 O13 74.37(12) . . ?
O7 Ho1 O12 134.15(11) . . ?
O4 Ho1 O12 145.47(11) 2_554 . ?
O1 Ho1 O12 75.45(10) . . ?
O1W Ho1 O12 99.34(12) . . ?
O13 Ho1 O12 72.95(11) . . ?
O7 Ho1 O10 125.12(10) . . ?
O4 Ho1 O10 89.86(11) 2_554 . ?
O1 Ho1 O10 74.73(11) . . ?
O1W Ho1 O10 145.55(11) . . ?
O13 Ho1 O10 71.88(11) . . ?
O12 Ho1 O10 77.22(10) . . ?
O7 Ho1 O11 84.87(10) . . ?
O4 Ho1 O11 143.68(11) 2_554 . ?
O1 Ho1 O11 72.27(11) . . ?
O1W Ho1 O11 71.98(12) . . ?
O13 Ho1 O11 108.26(11) . . ?
O12 Ho1 O11 53.38(10) . . ?
O10 Ho1 O11 125.59(10) . . ?
O7 Ho1 O9 77.43(10) . . ?
O4 Ho1 O9 67.55(10) 2_554 . ?
O1 Ho1 O9 68.27(9) . . ?
O1W Ho1 O9 138.61(11) . . ?
O13 Ho1 O9 105.97(11) . . ?
O12 Ho1 O9 120.71(10) . . ?
O10 Ho1 O9 49.27(8) . . ?
O11 Ho1 O9 139.80(10) . . ?
O7 Ho1 C21 110.45(12) . . ?
O4 Ho1 C21 153.99(11) 2_554 . ?
O1 Ho1 C21 73.66(11) . . ?
O1W Ho1 C21 83.73(13) . . ?
O13 Ho1 C21 89.36(12) . . ?
O12 Ho1 C21 26.81(11) . . ?
O10 Ho1 C21 102.43(11) . . ?
O11 Ho1 C21 26.69(11) . . ?
O9 Ho1 C21 137.16(10) . . ?
O7 Ho1 C20 102.08(11) . . ?
O4 Ho1 C20 76.40(11) 2_554 . ?
O1 Ho1 C20 71.39(11) . . ?
O1W Ho1 C20 148.36(12) . . ?
O13 Ho1 C20 87.39(12) . . ?
O12 Ho1 C20 99.67(11) . . ?
O10 Ho1 C20 24.37(9) . . ?
O11 Ho1 C20 139.30(11) . . ?
O9 Ho1 C20 25.02(9) . . ?
C21 Ho1 C20 122.40(12) . . ?
O9 Ho2 O3W 144.13(10) . . ?
O9 Ho2 O8 122.46(10) . . ?
O3W Ho2 O8 78.40(11) . . ?
O9 Ho2 O3 73.91(10) . 2_554 ?
O3W Ho2 O3 141.82(10) . 2_554 ?
O8 Ho2 O3 79.50(11) . 2_554 ?
O9 Ho2 O2 79.16(10) . . ?
O3W Ho2 O2 74.63(10) . . ?
O8 Ho2 O2 83.27(11) . . ?
O3 Ho2 O2 132.65(10) 2_554 . ?
O9 Ho2 O2W 78.37(10) . . ?
O3W Ho2 O2W 71.57(11) . . ?
O8 Ho2 O2W 146.61(11) . . ?
O3 Ho2 O2W 133.71(11) 2_554 . ?
O2 Ho2 O2W 75.10(11) . . ?
O9 Ho2 O6 92.27(10) . 1_455 ?
O3W Ho2 O6 95.73(11) . 1_455 ?
O8 Ho2 O6 127.76(10) . 1_455 ?
O3 Ho2 O6 74.19(11) 2_554 1_455 ?
O2 Ho2 O6 145.70(11) . 1_455 ?
O2W Ho2 O6 70.64(11) . 1_455 ?
O9 Ho2 O5 137.41(10) . 1_455 ?
O3W Ho2 O5 71.36(10) . 1_455 ?
O8 Ho2 O5 77.05(10) . 1_455 ?
O3 Ho2 O5 73.58(10) 2_554 1_455 ?
O2 Ho2 O5 143.38(10) . 1_455 ?
O2W Ho2 O5 105.95(10) . 1_455 ?
O6 Ho2 O5 52.63(10) 1_455 1_455 ?
O9 Ho2 C13 116.93(11) . 1_455 ?
O3W Ho2 C13 80.61(12) . 1_455 ?
O8 Ho2 C13 103.19(11) . 1_455 ?
O3 Ho2 C13 74.64(11) 2_554 1_455 ?
O2 Ho2 C13 152.62(11) . 1_455 ?
O2W Ho2 C13 86.23(11) . 1_455 ?
O6 Ho2 C13 26.43(11) 1_455 1_455 ?
O5 Ho2 C13 26.45(11) 1_455 1_455 ?
O9 Ho2 O7 74.40(9) . . ?
O3W Ho2 O7 116.05(11) . . ?
O8 Ho2 O7 48.32(9) . . ?
O3 Ho2 O7 67.98(9) 2_554 . ?
O2 Ho2 O7 67.63(9) . . ?
O2W Ho2 O7 137.03(9) . . ?
O6 Ho2 O7 142.01(10) 1_455 . ?
O5 Ho2 O7 116.64(9) 1_455 . ?
C13 Ho2 O7 135.87(10) 1_455 . ?
O9 Ho2 C14 99.14(10) . . ?
O3W Ho2 C14 96.54(12) . . ?
O8 Ho2 C14 23.54(10) . . ?
O3 Ho2 C14 73.10(11) 2_554 . ?
O2 Ho2 C14 73.68(11) . . ?
O2W Ho2 C14 148.58(11) . . ?
O6 Ho2 C14 140.61(10) 1_455 . ?
O5 Ho2 C14 96.95(10) 1_455 . ?
C13 Ho2 C14 121.31(12) 1_455 . ?
O7 Ho2 C14 24.80(9) . . ?
C6 O1 Ho1 141.3(3) . . ?
Ho1 O1W H1 124.6 . . ?
Ho1 O1W H2 109.7 . . ?
H1 O1W H2 124.9 . . ?
C6 O2 Ho2 134.2(3) . . ?
Ho2 O2W H3 109.4 . . ?
Ho2 O2W H4 109.4 . . ?
H3 O2W H4 108.2 . . ?
C7 O3 Ho2 139.1(3) . 2_544 ?
Ho2 O3W H5 109.4 . . ?
Ho2 O3W H6 109.6 . . ?
H5 O3W H6 108.2 . . ?
C7 O4 Ho1 135.8(3) . 2_544 ?
C13 O5 Ho2 90.7(2) . 1_655 ?
C13 O6 Ho2 94.6(3) . 1_655 ?
C14 O7 Ho1 174.1(3) . . ?
C14 O7 Ho2 81.9(2) . . ?
Ho1 O7 Ho2 102.38(11) . . ?
C14 O8 Ho2 107.6(3) . . ?
C20 O9 Ho2 163.9(3) . . ?
C20 O9 Ho1 87.0(2) . . ?
Ho2 O9 Ho1 105.79(11) . . ?
C20 O10 Ho1 102.5(2) . . ?
C21 O11 Ho1 90.3(3) . . ?
C21 O12 Ho1 93.5(2) . . ?
C22 O13 Ho1 136.1(3) . . ?
C1 N1 C5 121.8(4) . . ?
C8 N2 C12 116.5(4) . . ?
C15 N3 C19 117.0(4) . . ?
N1 C1 C2 120.9(4) . . ?
N1 C1 H1A 119.5 . . ?
C2 C1 H1A 119.5 . . ?
C3 C2 C1 117.9(4) . . ?
C3 C2 C6 124.3(3) . . ?
C1 C2 C6 117.7(4) . . ?
C2 C3 C4 120.9(4) . . ?
C2 C3 H3A 119.6 . . ?
C4 C3 H3A 119.6 . . ?
C5 C4 C3 118.2(4) . . ?
C5 C4 C7 118.4(4) . . ?
C3 C4 C7 123.3(3) . . ?
N1 C5 C4 120.3(4) . . ?
N1 C5 H5A 119.8 . . ?
C4 C5 H5A 119.8 . . ?
O1 C6 O2 126.9(4) . . ?
O1 C6 C2 115.8(3) . . ?
O2 C6 C2 117.3(4) . . ?
O4 C7 O3 127.6(4) . . ?
O4 C7 C4 116.5(4) . . ?
O3 C7 C4 115.9(3) . . ?
N2 C8 C9 123.6(4) . . ?
N2 C8 H8A 118.2 . . ?
C9 C8 H8A 118.2 . . ?
C10 C9 C8 118.6(4) . . ?
C10 C9 C13 119.9(4) . . ?
C8 C9 C13 121.2(4) . . ?
C9 C10 C11 119.3(4) . . ?
C9 C10 H10A 120.4 . . ?
C11 C10 H10A 120.4 . . ?
C12 C11 C10 117.4(4) . . ?
C12 C11 C14 120.4(4) . . ?
C10 C11 C14 122.0(4) . . ?
N2 C12 C11 124.5(4) . . ?
N2 C12 H12A 117.8 . . ?
C11 C12 H12A 117.8 . . ?
O5 C13 O6 120.9(4) . . ?
O5 C13 C9 120.5(4) . . ?
O6 C13 C9 118.5(4) . . ?
O5 C13 Ho2 62.9(2) . 1_655 ?
O6 C13 Ho2 59.0(2) . 1_655 ?
C9 C13 Ho2 167.5(3) . 1_655 ?
O8 C14 O7 122.1(4) . . ?
O8 C14 C11 118.7(4) . . ?
O7 C14 C11 119.2(4) . . ?
O8 C14 Ho2 48.9(2) . . ?
O7 C14 Ho2 73.3(2) . . ?
C11 C14 Ho2 166.0(3) . . ?
N3 C15 C16 124.1(4) . . ?
N3 C15 H15A 117.9 . . ?
C16 C15 H15A 117.9 . . ?
C17 C16 C15 117.7(4) . . ?
C17 C16 C20 121.4(4) . . ?
C15 C16 C20 120.8(4) . . ?
C18 C17 C16 118.7(4) . . ?
C18 C17 H17A 120.7 . . ?
C16 C17 H17A 120.7 . . ?
C19 C18 C17 118.8(4) . . ?
C19 C18 C21 120.0(4) . 1_455 ?
C17 C18 C21 121.1(4) . 1_455 ?
N3 C19 C18 123.6(4) . . ?
N3 C19 H19A 118.2 . . ?
C18 C19 H19A 118.2 . . ?
O10 C20 O9 120.6(4) . . ?
O10 C20 C16 119.4(3) . . ?
O9 C20 C16 119.9(4) . . ?
O10 C20 Ho1 53.1(2) . . ?
O9 C20 Ho1 68.0(2) . . ?
C16 C20 Ho1 168.3(3) . . ?
O12 C21 O11 122.3(4) . . ?
O12 C21 C18 117.8(4) . 1_655 ?
O11 C21 C18 119.7(4) . 1_655 ?
O12 C21 Ho1 59.7(2) . . ?
O11 C21 Ho1 63.0(2) . . ?
C18 C21 Ho1 169.7(3) 1_655 . ?
O14 C22 O13 128.3(5) . . ?
O14 C22 H22 115.9 . . ?
O13 C22 H22 115.9 . . ?
H7 O4W H8 110.0 . . ?
H9 O5W H10 107.9 . . ?

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
O7 Ho1 O1 C6 26.3(5) . . . . ?
O4 Ho1 O1 C6 -32.5(5) 2_554 . . . ?
O1W Ho1 O1 C6 83.8(5) . . . . ?
O13 Ho1 O1 C6 -146.2(5) . . . . ?
O12 Ho1 O1 C6 171.6(5) . . . . ?
O10 Ho1 O1 C6 -108.0(5) . . . . ?
O11 Ho1 O1 C6 115.9(5) . . . . ?
O9 Ho1 O1 C6 -56.2(5) . . . . ?
C21 Ho1 O1 C6 143.8(5) . . . . ?
C20 Ho1 O1 C6 -82.7(5) . . . . ?
O9 Ho2 O2 C6 25.1(4) . . . . ?
O3W Ho2 O2 C6 -179.6(4) . . . . ?
O8 Ho2 O2 C6 -99.8(4) . . . . ?
O3 Ho2 O2 C6 -30.8(5) 2_554 . . . ?
O2W Ho2 O2 C6 105.8(4) . . . . ?
O6 Ho2 O2 C6 103.0(4) 1_455 . . . ?
O5 Ho2 O2 C6 -157.4(4) 1_455 . . . ?
C13 Ho2 O2 C6 154.4(4) 1_455 . . . ?
O7 Ho2 O2 C6 -52.3(4) . . . . ?
C14 Ho2 O2 C6 -77.9(4) . . . . ?
O4 Ho1 O7 C14 -68(3) 2_554 . . . ?
O1 Ho1 O7 C14 152(3) . . . . ?
O1W Ho1 O7 C14 7(3) . . . . ?
O13 Ho1 O7 C14 -37(3) . . . . ?
O12 Ho1 O7 C14 102(3) . . . . ?
O10 Ho1 O7 C14 -150(3) . . . . ?
O11 Ho1 O7 C14 79(3) . . . . ?
O9 Ho1 O7 C14 -137(3) . . . . ?
C21 Ho1 O7 C14 87(3) . . . . ?
C20 Ho1 O7 C14 -141(3) . . . . ?
O4 Ho1 O7 Ho2 69.15(11) 2_554 . . . ?
O1 Ho1 O7 Ho2 -70.67(11) . . . . ?
O1W Ho1 O7 Ho2 143.84(12) . . . . ?
O13 Ho1 O7 Ho2 100.1(2) . . . . ?
O12 Ho1 O7 Ho2 -120.84(13) . . . . ?
O10 Ho1 O7 Ho2 -13.03(15) . . . . ?
O11 Ho1 O7 Ho2 -143.68(11) . . . . ?
O9 Ho1 O7 Ho2 0.01(8) . . . . ?
C21 Ho1 O7 Ho2 -135.94(11) . . . . ?
C20 Ho1 O7 Ho2 -4.28(12) . . . . ?
O9 Ho2 O7 C14 175.9(2) . . . . ?
O3W Ho2 O7 C14 -40.9(2) . . . . ?
O8 Ho2 O7 C14 1.8(2) . . . . ?
O3 Ho2 O7 C14 97.3(2) 2_554 . . . ?
O2 Ho2 O7 C14 -99.6(2) . . . . ?
O2W Ho2 O7 C14 -131.4(2) . . . . ?
O6 Ho2 O7 C14 102.8(2) 1_455 . . . ?
O5 Ho2 O7 C14 40.3(2) 1_455 . . . ?
C13 Ho2 O7 C14 63.2(3) 1_455 . . . ?
O9 Ho2 O7 Ho1 -0.01(10) . . . . ?
O3W Ho2 O7 Ho1 143.12(10) . . . . ?
O8 Ho2 O7 Ho1 -174.18(17) . . . . ?
O3 Ho2 O7 Ho1 -78.62(12) 2_554 . . . ?
O2 Ho2 O7 Ho1 84.47(12) . . . . ?
O2W Ho2 O7 Ho1 52.64(18) . . . . ?
O6 Ho2 O7 Ho1 -73.11(16) 1_455 . . . ?
O5 Ho2 O7 Ho1 -135.66(10) 1_455 . . . ?
C13 Ho2 O7 Ho1 -112.81(15) 1_455 . . . ?
C14 Ho2 O7 Ho1 -176.0(3) . . . . ?
O9 Ho2 O8 C14 -8.5(3) . . . . ?
O3W Ho2 O8 C14 139.7(3) . . . . ?
O3 Ho2 O8 C14 -71.6(3) 2_554 . . . ?
O2 Ho2 O8 C14 64.0(3) . . . . ?
O2W Ho2 O8 C14 113.6(3) . . . . ?
O6 Ho2 O8 C14 -132.0(3) 1_455 . . . ?
O5 Ho2 O8 C14 -147.0(3) 1_455 . . . ?
C13 Ho2 O8 C14 -143.0(3) 1_455 . . . ?
O7 Ho2 O8 C14 -1.9(2) . . . . ?
O3W Ho2 O9 C20 28.5(11) . . . . ?
O8 Ho2 O9 C20 146.7(10) . . . . ?
O3 Ho2 O9 C20 -147.4(10) 2_554 . . . ?
O2 Ho2 O9 C20 72.0(10) . . . . ?
O2W Ho2 O9 C20 -4.8(10) . . . . ?
O6 Ho2 O9 C20 -74.5(10) 1_455 . . . ?
O5 Ho2 O9 C20 -105.8(10) 1_455 . . . ?
C13 Ho2 O9 C20 -84.5(10) 1_455 . . . ?
O7 Ho2 O9 C20 141.6(10) . . . . ?
C14 Ho2 O9 C20 143.3(10) . . . . ?
O3W Ho2 O9 Ho1 -113.07(18) . . . . ?
O8 Ho2 O9 Ho1 5.16(15) . . . . ?
O3 Ho2 O9 Ho1 71.07(11) 2_554 . . . ?
O2 Ho2 O9 Ho1 -69.58(11) . . . . ?
O2W Ho2 O9 Ho1 -146.41(12) . . . . ?
O6 Ho2 O9 Ho1 143.89(11) 1_455 . . . ?
O5 Ho2 O9 Ho1 112.60(14) 1_455 . . . ?
C13 Ho2 O9 Ho1 133.95(11) 1_455 . . . ?
O7 Ho2 O9 Ho1 0.01(8) . . . . ?
C14 Ho2 O9 Ho1 1.73(12) . . . . ?
O7 Ho1 O9 C20 -170.1(2) . . . . ?
O4 Ho1 O9 C20 106.5(2) 2_554 . . . ?
O1 Ho1 O9 C20 -92.4(2) . . . . ?
O1W Ho1 O9 C20 127.8(2) . . . . ?
O13 Ho1 O9 C20 43.5(2) . . . . ?
O12 Ho1 O9 C20 -35.8(3) . . . . ?
O10 Ho1 O9 C20 -4.2(2) . . . . ?
O11 Ho1 O9 C20 -104.0(2) . . . . ?
C21 Ho1 O9 C20 -63.4(3) . . . . ?
O7 Ho1 O9 Ho2 -0.01(10) . . . . ?
O4 Ho1 O9 Ho2 -83.47(12) 2_554 . . . ?
O1 Ho1 O9 Ho2 77.67(12) . . . . ?
O1W Ho1 O9 Ho2 -62.12(19) . . . . ?
O13 Ho1 O9 Ho2 -146.43(11) . . . . ?
O12 Ho1 O9 Ho2 134.22(11) . . . . ?
O10 Ho1 O9 Ho2 165.90(17) . . . . ?
O11 Ho1 O9 Ho2 66.05(16) . . . . ?
C21 Ho1 O9 Ho2 106.61(16) . . . . ?
C20 Ho1 O9 Ho2 170.0(3) . . . . ?
O7 Ho1 O10 C20 21.1(3) . . . . ?
O4 Ho1 O10 C20 -55.6(2) 2_554 . . . ?
O1 Ho1 O10 C20 78.5(2) . . . . ?
O1W Ho1 O10 C20 -115.4(3) . . . . ?
O13 Ho1 O10 C20 -127.3(3) . . . . ?
O12 Ho1 O10 C20 156.7(3) . . . . ?
O11 Ho1 O10 C20 132.8(2) . . . . ?
O9 Ho1 O10 C20 4.3(2) . . . . ?
C21 Ho1 O10 C20 147.5(2) . . . . ?
O7 Ho1 O11 C21 163.7(3) . . . . ?
O4 Ho1 O11 C21 -132.2(2) 2_554 . . . ?
O1 Ho1 O11 C21 88.8(3) . . . . ?
O1W Ho1 O11 C21 -113.0(3) . . . . ?
O13 Ho1 O11 C21 -47.0(3) . . . . ?
O12 Ho1 O11 C21 4.0(2) . . . . ?
O10 Ho1 O11 C21 33.4(3) . . . . ?
O9 Ho1 O11 C21 100.1(3) . . . . ?
C20 Ho1 O11 C21 61.1(3) . . . . ?
O7 Ho1 O12 C21 -32.8(3) . . . . ?
O4 Ho1 O12 C21 129.7(3) 2_554 . . . ?
O1 Ho1 O12 C21 -82.5(3) . . . . ?
O1W Ho1 O12 C21 55.2(3) . . . . ?
O13 Ho1 O12 C21 125.5(3) . . . . ?
O10 Ho1 O12 C21 -159.8(3) . . . . ?
O11 Ho1 O12 C21 -4.0(2) . . . . ?
O9 Ho1 O12 C21 -135.7(2) . . . . ?
C20 Ho1 O12 C21 -150.2(3) . . . . ?
O7 Ho1 O13 C22 19.0(6) . . . . ?
O4 Ho1 O13 C22 50.9(5) 2_554 . . . ?
O1 Ho1 O13 C22 -174.4(5) . . . . ?
O1W Ho1 O13 C22 -26.4(5) . . . . ?
O12 Ho1 O13 C22 -131.6(5) . . . . ?
O10 Ho1 O13 C22 146.7(5) . . . . ?
O11 Ho1 O13 C22 -90.9(5) . . . . ?
O9 Ho1 O13 C22 110.5(5) . . . . ?
C21 Ho1 O13 C22 -110.0(5) . . . . ?
C20 Ho1 O13 C22 127.5(5) . . . . ?
C5 N1 C1 C2 1.1(7) . . . . ?
N1 C1 C2 C3 -0.8(7) . . . . ?
N1 C1 C2 C6 -178.6(4) . . . . ?
C1 C2 C3 C4 0.0(7) . . . . ?
C6 C2 C3 C4 177.5(4) . . . . ?
C2 C3 C4 C5 0.6(7) . . . . ?
C2 C3 C4 C7 -178.2(4) . . . . ?
C1 N1 C5 C4 -0.4(7) . . . . ?
C3 C4 C5 N1 -0.4(7) . . . . ?
C7 C4 C5 N1 178.5(4) . . . . ?
Ho1 O1 C6 O2 16.4(8) . . . . ?
Ho1 O1 C6 C2 -164.7(3) . . . . ?
Ho2 O2 C6 O1 11.1(7) . . . . ?
Ho2 O2 C6 C2 -167.9(3) . . . . ?
C3 C2 C6 O1 -176.4(4) . . . . ?
C1 C2 C6 O1 1.2(6) . . . . ?
C3 C2 C6 O2 2.7(7) . . . . ?
C1 C2 C6 O2 -179.8(4) . . . . ?
Ho1 O4 C7 O3 -19.4(8) 2_544 . . . ?
Ho1 O4 C7 C4 159.9(3) 2_544 . . . ?
Ho2 O3 C7 O4 -7.9(8) 2_544 . . . ?
Ho2 O3 C7 C4 172.8(3) 2_544 . . . ?
C5 C4 C7 O4 176.1(4) . . . . ?
C3 C4 C7 O4 -5.1(7) . . . . ?
C5 C4 C7 O3 -4.5(6) . . . . ?
C3 C4 C7 O3 174.3(4) . . . . ?
C12 N2 C8 C9 1.3(6) . . . . ?
N2 C8 C9 C10 1.7(6) . . . . ?
N2 C8 C9 C13 -172.3(4) . . . . ?
C8 C9 C10 C11 -2.8(6) . . . . ?
C13 C9 C10 C11 171.2(4) . . . . ?
C9 C10 C11 C12 1.0(6) . . . . ?
C9 C10 C11 C14 -174.3(4) . . . . ?
C8 N2 C12 C11 -3.3(6) . . . . ?
C10 C11 C12 N2 2.2(6) . . . . ?
C14 C11 C12 N2 177.6(4) . . . . ?
Ho2 O5 C13 O6 -10.8(4) 1_655 . . . ?
Ho2 O5 C13 C9 166.2(3) 1_655 . . . ?
Ho2 O6 C13 O5 11.2(4) 1_655 . . . ?
Ho2 O6 C13 C9 -165.9(3) 1_655 . . . ?
C10 C9 C13 O5 -175.5(4) . . . . ?
C8 C9 C13 O5 -1.6(6) . . . . ?
C10 C9 C13 O6 1.7(6) . . . . ?
C8 C9 C13 O6 175.5(4) . . . . ?
C10 C9 C13 Ho2 -73.3(15) . . . 1_655 ?
C8 C9 C13 Ho2 100.6(14) . . . 1_655 ?
Ho2 O8 C14 O7 3.8(5) . . . . ?
Ho2 O8 C14 C11 -172.2(3) . . . . ?
Ho1 O7 C14 O8 135(3) . . . . ?
Ho2 O7 C14 O8 -3.0(4) . . . . ?
Ho1 O7 C14 C11 -49(3) . . . . ?
Ho2 O7 C14 C11 173.0(3) . . . . ?
Ho1 O7 C14 Ho2 138(3) . . . . ?
C12 C11 C14 O8 -13.8(6) . . . . ?
C10 C11 C14 O8 161.3(4) . . . . ?
C12 C11 C14 O7 170.0(4) . . . . ?
C10 C11 C14 O7 -14.8(6) . . . . ?
C12 C11 C14 Ho2 -38.7(13) . . . . ?
C10 C11 C14 Ho2 136.4(10) . . . . ?
O9 Ho2 C14 O8 172.7(3) . . . . ?
O3W Ho2 C14 O8 -39.6(3) . . . . ?
O3 Ho2 C14 O8 102.7(3) 2_554 . . . ?
O2 Ho2 C14 O8 -111.5(3) . . . . ?
O2W Ho2 C14 O8 -104.6(3) . . . . ?
O6 Ho2 C14 O8 67.7(3) 1_455 . . . ?
O5 Ho2 C14 O8 32.3(3) 1_455 . . . ?
C13 Ho2 C14 O8 43.3(3) 1_455 . . . ?
O7 Ho2 C14 O8 176.7(4) . . . . ?
O9 Ho2 C14 O7 -4.0(2) . . . . ?
O3W Ho2 C14 O7 143.7(2) . . . . ?
O8 Ho2 C14 O7 -176.7(4) . . . . ?
O3 Ho2 C14 O7 -73.9(2) 2_554 . . . ?
O2 Ho2 C14 O7 71.8(2) . . . . ?
O2W Ho2 C14 O7 78.7(3) . . . . ?
O6 Ho2 C14 O7 -109.0(2) 1_455 . . . ?
O5 Ho2 C14 O7 -144.4(2) 1_455 . . . ?
C13 Ho2 C14 O7 -133.4(2) 1_455 . . . ?
O9 Ho2 C14 C11 -158.0(11) . . . . ?
O3W Ho2 C14 C11 -10.3(11) . . . . ?
O8 Ho2 C14 C11 29.3(10) . . . . ?
O3 Ho2 C14 C11 132.1(11) 2_554 . . . ?
O2 Ho2 C14 C11 -82.2(11) . . . . ?
O2W Ho2 C14 C11 -75.3(12) . . . . ?
O6 Ho2 C14 C11 97.0(11) 1_455 . . . ?
O5 Ho2 C14 C11 61.6(11) 1_455 . . . ?
C13 Ho2 C14 C11 72.6(11) 1_455 . . . ?
O7 Ho2 C14 C11 -154.0(13) . . . . ?
C19 N3 C15 C16 2.4(7) . . . . ?
N3 C15 C16 C17 -0.9(7) . . . . ?
N3 C15 C16 C20 -178.1(4) . . . . ?
C15 C16 C17 C18 -1.8(6) . . . . ?
C20 C16 C17 C18 175.5(4) . . . . ?
C16 C17 C18 C19 2.6(6) . . . . ?
C16 C17 C18 C21 -173.5(4) . . . 1_455 ?
C15 N3 C19 C18 -1.5(7) . . . . ?
C17 C18 C19 N3 -1.1(7) . . . . ?
C21 C18 C19 N3 175.2(4) 1_455 . . . ?
Ho1 O10 C20 O9 -8.2(4) . . . . ?
Ho1 O10 C20 C16 169.2(3) . . . . ?
Ho2 O9 C20 O10 -136.1(8) . . . . ?
Ho1 O9 C20 O10 7.1(4) . . . . ?
Ho2 O9 C20 C16 46.4(12) . . . . ?
Ho1 O9 C20 C16 -170.4(3) . . . . ?
Ho2 O9 C20 Ho1 -143.2(10) . . . . ?
C17 C16 C20 O10 -162.1(4) . . . . ?
C15 C16 C20 O10 15.1(6) . . . . ?
C17 C16 C20 O9 15.4(6) . . . . ?
C15 C16 C20 O9 -167.4(4) . . . . ?
C17 C16 C20 Ho1 -114.6(13) . . . . ?
C15 C16 C20 Ho1 62.5(15) . . . . ?
O7 Ho1 C20 O10 -162.4(2) . . . . ?
O4 Ho1 C20 O10 121.9(3) 2_554 . . . ?
O1 Ho1 C20 O10 -94.0(3) . . . . ?
O1W Ho1 C20 O10 103.1(3) . . . . ?
O13 Ho1 C20 O10 49.2(3) . . . . ?
O12 Ho1 C20 O10 -23.1(3) . . . . ?
O11 Ho1 C20 O10 -66.2(3) . . . . ?
O9 Ho1 C20 O10 -172.4(4) . . . . ?
C21 Ho1 C20 O10 -38.4(3) . . . . ?
O7 Ho1 C20 O9 9.9(2) . . . . ?
O4 Ho1 C20 O9 -65.8(2) 2_554 . . . ?
O1 Ho1 C20 O9 78.3(2) . . . . ?
O1W Ho1 C20 O9 -84.5(3) . . . . ?
O13 Ho1 C20 O9 -138.5(2) . . . . ?
O12 Ho1 C20 O9 149.3(2) . . . . ?
O10 Ho1 C20 O9 172.4(4) . . . . ?
O11 Ho1 C20 O9 106.2(2) . . . . ?
C21 Ho1 C20 O9 133.9(2) . . . . ?
O7 Ho1 C20 C16 144.2(13) . . . . ?
O4 Ho1 C20 C16 68.5(13) 2_554 . . . ?
O1 Ho1 C20 C16 -147.4(13) . . . . ?
O1W Ho1 C20 C16 49.8(14) . . . . ?
O13 Ho1 C20 C16 -4.2(13) . . . . ?
O12 Ho1 C20 C16 -76.4(13) . . . . ?
O10 Ho1 C20 C16 -53.3(13) . . . . ?
O11 Ho1 C20 C16 -119.5(13) . . . . ?
O9 Ho1 C20 C16 134.3(14) . . . . ?
C21 Ho1 C20 C16 -91.8(13) . . . . ?
Ho1 O12 C21 O11 7.5(4) . . . . ?
Ho1 O12 C21 C18 -168.5(3) . . . 1_655 ?
Ho1 O11 C21 O12 -7.3(4) . . . . ?
Ho1 O11 C21 C18 168.7(3) . . . 1_655 ?
O7 Ho1 C21 O12 155.5(2) . . . . ?
O4 Ho1 C21 O12 -96.3(4) 2_554 . . . ?
O1 Ho1 C21 O12 90.0(3) . . . . ?
O1W Ho1 C21 O12 -125.4(3) . . . . ?
O13 Ho1 C21 O12 -51.1(3) . . . . ?
O10 Ho1 C21 O12 20.2(3) . . . . ?
O11 Ho1 C21 O12 172.9(4) . . . . ?
O9 Ho1 C21 O12 62.0(3) . . . . ?
C20 Ho1 C21 O12 35.4(3) . . . . ?
O7 Ho1 C21 O11 -17.4(3) . . . . ?
O4 Ho1 C21 O11 90.8(4) 2_554 . . . ?
O1 Ho1 C21 O11 -82.9(3) . . . . ?
O1W Ho1 C21 O11 61.7(3) . . . . ?
O13 Ho1 C21 O11 136.0(3) . . . . ?
O12 Ho1 C21 O11 -172.9(4) . . . . ?
O10 Ho1 C21 O11 -152.7(2) . . . . ?
O9 Ho1 C21 O11 -110.8(3) . . . . ?
C20 Ho1 C21 O11 -137.5(2) . . . . ?
O7 Ho1 C21 C18 -125.4(17) . . . 1_655 ?
O4 Ho1 C21 C18 -17.2(19) 2_554 . . 1_655 ?
O1 Ho1 C21 C18 169.1(17) . . . 1_655 ?
O1W Ho1 C21 C18 -46.3(17) . . . 1_655 ?
O13 Ho1 C21 C18 28.0(17) . . . 1_655 ?
O12 Ho1 C21 C18 79.1(17) . . . 1_655 ?
O10 Ho1 C21 C18 99.3(17) . . . 1_655 ?
O11 Ho1 C21 C18 -108.0(18) . . . 1_655 ?
O9 Ho1 C21 C18 141.1(17) . . . 1_655 ?
C20 Ho1 C21 C18 114.5(17) . . . 1_655 ?
Ho1 O13 C22 O14 17.8(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.20
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.138
####################################################################### 
# 
# 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_Er
_database_code_depnum_ccdc_archive 'CCDC 1472130'
_audit_update_record             
;
2016-04-04 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H18 Er N3 O15'
_chemical_formula_weight         719.64

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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'Cc   '

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

_cell_length_a                   21.091(5)
_cell_length_b                   11.959(2)
_cell_length_c                   9.6220(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.456(4)
_cell_angle_gamma                90.00
_cell_volume                     2386.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4779
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      28.30

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1412
_exptl_absorpt_coefficient_mu    3.603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5327
_exptl_absorpt_correction_T_max  0.7146
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6043
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.19
_reflns_number_total             3242
_reflns_number_gt                3171
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0379P)²+19.8190P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00156(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.65(2)
_refine_ls_number_reflns         3242
_refine_ls_number_parameters     366
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0796
_refine_ls_wR_factor_gt          0.0790
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.16749(7) 0.51152(2) 0.15806(12) 0.01537(13) Uani 1 1 d . . .
C1 C 0.1995(7) 0.0905(15) 0.0634(14) 0.026(3) Uani 1 1 d . . .
H1A H 0.2256 0.1284 0.0108 0.031 Uiso 1 1 calc R . .
N1 N 0.1946(6) -0.0203(9) 0.0489(13) 0.033(3) Uani 1 1 d . . .
O1 O 0.2050(4) 0.3266(8) 0.0757(8) 0.0227(19) Uani 1 1 d . . .
O1W O 0.2043(5) 0.6770(10) 0.2896(9) 0.033(2) Uani 1 1 d . . .
H1WA H 0.1701 0.7239 0.3028 0.049 Uiso 1 1 d R . .
H1WB H 0.2317 0.7251 0.2468 0.049 Uiso 1 1 d R . .
C2 C 0.1684(10) 0.1523(5) 0.1514(19) 0.0230(16) Uani 1 1 d . . .
N2 N -0.0888(5) 0.6875(12) 0.1612(10) 0.029(3) Uani 1 1 d . . .
O2 O 0.1509(4) 0.3300(9) 0.2496(8) 0.024(2) Uani 1 1 d . . .
O2W O 0.1193(4) 0.6703(10) 0.0156(9) 0.028(2) Uani 1 1 d . . .
H2WA H 0.0738 0.6679 -0.0050 0.042 Uiso 1 1 d R . .
H2WB H 0.1320 0.6745 -0.0731 0.042 Uiso 1 1 d R . .
C3 C 0.1264(6) 0.0961(13) 0.2257(14) 0.021(3) Uani 1 1 d . . .
H3A H 0.1030 0.1359 0.2824 0.025 Uiso 1 1 calc R . .
N3 N 0.4546(5) 0.6170(12) -0.0193(12) 0.031(3) Uani 1 1 d . . .
O3 O 0.0394(4) -0.0259(6) 0.3450(10) 0.047(2) Uani 1 1 d . . .
H11A H 0.0213 -0.0655 0.3954 0.070 Uiso 1 1 calc R . .
O3W O 0.2892(11) 0.865(2) 0.306(2) 0.204(10) Uani 1 1 d . . .
H3WA H 0.2708 0.8657 0.2197 0.245 Uiso 1 1 d R . .
H3WB H 0.3293 0.8593 0.3043 0.245 Uiso 1 1 d R . .
C4 C 0.1202(7) -0.0185(10) 0.2140(16) 0.028(3) Uani 1 1 d . . .
O4 O 0.0849(5) -0.1873(6) 0.3008(10) 0.056(2) Uani 1 1 d . . .
C5 C 0.1559(5) -0.0732(7) 0.1218(9) 0.030(3) Uani 1 1 d . . .
H5A H 0.1521 -0.1504 0.1122 0.036 Uiso 1 1 calc R . .
O5 O 0.0935(5) 0.5525(12) 0.2913(11) 0.030(2) Uani 1 1 d . . .
C6 C 0.1732(9) 0.2769(6) 0.1591(17) 0.025(2) Uani 1 1 d . . .
O6 O 0.0772(6) 0.5500(15) 0.5105(11) 0.038(3) Uani 1 1 d . . .
C7 C 0.0789(5) -0.0856(7) 0.2887(10) 0.029(2) Uani 1 1 d . . .
O7 O -0.1515(4) 0.5537(8) 0.5784(8) 0.054(2) Uani 1 1 d . . .
C8 C -0.0285(6) 0.6511(14) 0.2034(13) 0.028(3) Uani 1 1 d . . .
H8A H 0.0018 0.6619 0.1454 0.033 Uiso 1 1 calc R . .
O8 O -0.2253(4) 0.6237(7) 0.4043(8) 0.0431(18) Uani 1 1 d . . .
H8 H -0.2500 0.6076 0.4580 0.065 Uiso 1 1 calc R . .
C9 C -0.0101(6) 0.5965(11) 0.3346(11) 0.014(2) Uani 1 1 d . . .
O9 O 0.4888(4) 0.7699(8) 0.3813(8) 0.058(2) Uani 1 1 d . . .
C10 C -0.0539(6) 0.5851(12) 0.4169(13) 0.019(3) Uani 1 1 d . . .
H10A H -0.0423 0.5531 0.5060 0.023 Uiso 1 1 calc R . .
O10 O 0.3884(4) 0.7271(8) 0.4065(9) 0.055(2) Uani 1 1 d . . .
H10 H 0.3927 0.7771 0.4658 0.082 Uiso 1 1 calc R . .
C11 C -0.1188(7) 0.6216(13) 0.3690(14) 0.026(3) Uani 1 1 d . . .
O11 O 0.2667(7) 0.5373(15) -0.1931(13) 0.040(3) Uani 1 1 d . . .
C12 C -0.1319(6) 0.6716(14) 0.2402(13) 0.029(3) Uani 1 1 d . . .
H12A H -0.1738 0.6956 0.2069 0.034 Uiso 1 1 calc R . .
O12 O 0.2345(5) 0.5593(13) 0.0122(10) 0.029(2) Uani 1 1 d . . .
C13 C 0.0609(6) 0.5613(14) 0.3818(13) 0.015(3) Uani 1 1 d . . .
C14 C -0.1663(5) 0.5939(8) 0.4615(10) 0.032(2) Uani 1 1 d . . .
C15 C 0.4664(6) 0.6693(14) 0.1096(13) 0.030(3) Uani 1 1 d . . .
H15A H 0.5074 0.6971 0.1441 0.035 Uiso 1 1 calc R . .
C16 C 0.4182(6) 0.6815(12) 0.1896(12) 0.023(3) Uani 1 1 d . . .
C17 C 0.3570(6) 0.6437(14) 0.1361(13) 0.025(3) Uani 1 1 d U . .
H17A H 0.3253 0.6467 0.1917 0.031 Uiso 1 1 calc R . .
C18 C 0.3426(6) 0.6023(13) 0.0033(13) 0.020(3) Uani 1 1 d U . .
C19 C 0.3947(7) 0.5875(13) -0.0698(15) 0.030(3) Uani 1 1 d . . .
H19A H 0.3860 0.5549 -0.1590 0.037 Uiso 1 1 calc R . .
C20 C 0.4355(6) 0.7319(10) 0.3351(12) 0.040(3) Uani 1 1 d . . .
C21 C 0.2781(7) 0.5651(14) -0.0631(14) 0.022(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
Er1 O12 2.240(11) . ?
Er1 O5 2.246(11) . ?
Er1 O6 2.281(11) 2_564 ?
Er1 O11 2.384(13) 2_565 ?
Er1 O2 2.392(10) . ?
Er1 O1W 2.401(10) . ?
Er1 O2W 2.452(11) . ?
Er1 O1 2.524(10) . ?
Er1 C6 2.809(7) . ?
C1 N1 1.335(18) . ?
C1 C2 1.38(2) . ?
C1 H1A 0.9300 . ?
N1 C5 1.328(17) . ?
O1 C6 1.28(2) . ?
O1W H1WA 0.9405 . ?
O1W H1WB 0.9592 . ?
C2 C3 1.41(2) . ?
C2 C6 1.494(9) . ?
N2 C12 1.301(17) . ?
N2 C8 1.336(17) . ?
O2 C6 1.239(18) . ?
O2W H2WA 0.9448 . ?
O2W H2WB 0.9414 . ?
C3 C4 1.379(16) . ?
C3 H3A 0.9300 . ?
N3 C19 1.316(18) . ?
N3 C15 1.371(18) . ?
O3 C7 1.289(12) . ?
O3 H11A 0.8200 . ?
O3W H3WA 0.8499 . ?
O3W H3WB 0.8500 . ?
C4 C5 1.424(18) . ?
C4 C7 1.465(17) . ?
O4 C7 1.225(11) . ?
C5 H5A 0.9300 . ?
O5 C13 1.208(18) . ?
O6 C13 1.231(16) . ?
O6 Er1 2.281(11) 2_565 ?
O7 C14 1.211(12) . ?
C8 C9 1.412(16) . ?
C8 H8A 0.9300 . ?
O8 C14 1.316(12) . ?
O8 H8 0.8200 . ?
C9 C10 1.329(18) . ?
C9 C13 1.542(17) . ?
O9 C20 1.218(14) . ?
C10 C11 1.431(18) . ?
C10 H10A 0.9300 . ?
O10 C20 1.309(14) . ?
O10 H10 0.8200 . ?
C11 C12 1.358(19) . ?
C11 C14 1.493(17) . ?
O11 C21 1.274(18) . ?
O11 Er1 2.384(13) 2_564 ?
C12 H12A 0.9300 . ?
O12 C21 1.27(2) . ?
C15 C16 1.391(18) . ?
C15 H15A 0.9300 . ?
C16 C17 1.376(18) . ?
C16 C20 1.507(15) . ?
C17 C18 1.352(18) . ?
C17 H17A 0.9300 . ?
C18 C19 1.420(19) . ?
C18 C21 1.46(2) . ?
C19 H19A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O12 Er1 O5 152.3(2) . . ?
O12 Er1 O6 104.1(4) . 2_564 ?
O5 Er1 O6 80.7(5) . 2_564 ?
O12 Er1 O11 81.6(4) . 2_565 ?
O5 Er1 O11 109.6(4) . 2_565 ?
O6 Er1 O11 146.9(3) 2_564 2_565 ?
O12 Er1 O2 127.9(4) . . ?
O5 Er1 O2 79.9(4) . . ?
O6 Er1 O2 77.0(4) 2_564 . ?
O11 Er1 O2 74.2(5) 2_565 . ?
O12 Er1 O1W 86.5(4) . . ?
O5 Er1 O1W 73.2(4) . . ?
O6 Er1 O1W 138.4(5) 2_564 . ?
O11 Er1 O1W 73.7(5) 2_565 . ?
O2 Er1 O1W 127.5(3) . . ?
O12 Er1 O2W 72.3(4) . . ?
O5 Er1 O2W 83.7(4) . . ?
O6 Er1 O2W 71.8(5) 2_564 . ?
O11 Er1 O2W 139.0(5) 2_565 . ?
O2 Er1 O2W 146.6(3) . . ?
O1W Er1 O2W 73.6(2) . . ?
O12 Er1 O1 76.0(4) . . ?
O5 Er1 O1 131.3(4) . . ?
O6 Er1 O1 78.2(5) 2_564 . ?
O11 Er1 O1 71.5(5) 2_565 . ?
O2 Er1 O1 52.82(18) . . ?
O1W Er1 O1 142.9(3) . . ?
O2W Er1 O1 128.7(3) . . ?
O12 Er1 C6 103.0(6) . . ?
O5 Er1 C6 104.5(6) . . ?
O6 Er1 C6 73.2(6) 2_564 . ?
O11 Er1 C6 73.8(6) 2_565 . ?
O2 Er1 C6 26.0(4) . . ?
O1W Er1 C6 144.3(4) . . ?
O2W Er1 C6 142.1(4) . . ?
O1 Er1 C6 27.1(4) . . ?
N1 C1 C2 124.1(13) . . ?
N1 C1 H1A 117.9 . . ?
C2 C1 H1A 117.9 . . ?
C5 N1 C1 117.5(11) . . ?
C6 O1 Er1 88.9(6) . . ?
Er1 O1W H1WA 112.3 . . ?
Er1 O1W H1WB 115.5 . . ?
H1WA O1W H1WB 103.6 . . ?
C1 C2 C3 118.1(7) . . ?
C1 C2 C6 122.0(17) . . ?
C3 C2 C6 119.6(16) . . ?
C12 N2 C8 120.2(11) . . ?
C6 O2 Er1 96.1(8) . . ?
Er1 O2W H2WA 113.3 . . ?
Er1 O2W H2WB 113.0 . . ?
H2WA O2W H2WB 104.9 . . ?
C4 C3 C2 119.5(12) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C19 N3 C15 117.5(12) . . ?
C7 O3 H11A 109.5 . . ?
H3WA O3W H3WB 105.1 . . ?
C3 C4 C5 117.0(12) . . ?
C3 C4 C7 124.1(11) . . ?
C5 C4 C7 118.9(10) . . ?
N1 C5 C4 123.7(8) . . ?
N1 C5 H5A 118.1 . . ?
C4 C5 H5A 118.1 . . ?
C13 O5 Er1 167.3(11) . . ?
O2 C6 O1 120.7(7) . . ?
O2 C6 C2 121.0(16) . . ?
O1 C6 C2 118.1(15) . . ?
O2 C6 Er1 57.9(6) . . ?
O1 C6 Er1 63.9(5) . . ?
C2 C6 Er1 173.5(14) . . ?
C13 O6 Er1 135.3(10) . 2_565 ?
O4 C7 O3 125.0(10) . . ?
O4 C7 C4 122.0(10) . . ?
O3 C7 C4 112.9(8) . . ?
N2 C8 C9 121.0(12) . . ?
N2 C8 H8A 119.5 . . ?
C9 C8 H8A 119.5 . . ?
C14 O8 H8 109.5 . . ?
C10 C9 C8 118.2(12) . . ?
C10 C9 C13 122.7(11) . . ?
C8 C9 C13 119.0(11) . . ?
C9 C10 C11 120.4(12) . . ?
C9 C10 H10A 119.8 . . ?
C11 C10 H10A 119.8 . . ?
C20 O10 H10 109.5 . . ?
C12 C11 C10 116.9(13) . . ?
C12 C11 C14 126.5(12) . . ?
C10 C11 C14 116.5(11) . . ?
C21 O11 Er1 129.9(13) . 2_564 ?
N2 C12 C11 123.3(13) . . ?
N2 C12 H12A 118.3 . . ?
C11 C12 H12A 118.3 . . ?
C21 O12 Er1 167.1(13) . . ?
O5 C13 O6 128.6(14) . . ?
O5 C13 C9 117.4(12) . . ?
O6 C13 C9 113.9(12) . . ?
O7 C14 O8 124.1(9) . . ?
O7 C14 C11 123.7(10) . . ?
O8 C14 C11 112.1(9) . . ?
N3 C15 C16 121.1(12) . . ?
N3 C15 H15A 119.4 . . ?
C16 C15 H15A 119.4 . . ?
C17 C16 C15 119.3(12) . . ?
C17 C16 C20 122.2(11) . . ?
C15 C16 C20 118.5(12) . . ?
C18 C17 C16 120.6(12) . . ?
C18 C17 H17A 119.7 . . ?
C16 C17 H17A 119.7 . . ?
C17 C18 C19 116.9(13) . . ?
C17 C18 C21 123.8(12) . . ?
C19 C18 C21 119.2(12) . . ?
N3 C19 C18 124.1(13) . . ?
N3 C19 H19A 117.9 . . ?
C18 C19 H19A 117.9 . . ?
O9 C20 O10 124.2(12) . . ?
O9 C20 C16 122.8(11) . . ?
O10 C20 C16 113.0(10) . . ?
O11 C21 O12 121.3(16) . . ?
O11 C21 C18 120.1(15) . . ?
O12 C21 C18 118.6(12) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.19
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.107
####################################################################### 
# 
# 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_Lu
_database_code_depnum_ccdc_archive 'CCDC 1472131'
_audit_update_record             
;
2016-04-04 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H18 Lu N3 O15'
_chemical_formula_weight         727.35

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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'Cc   '

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

_cell_length_a                   20.994(14)
_cell_length_b                   11.889(8)
_cell_length_c                   9.577(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.552(7)
_cell_angle_gamma                90.00
_cell_volume                     2350(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1935
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      23.60

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    4.289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4808
_exptl_absorpt_correction_T_max  0.6737
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5934
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         25.19
_reflns_number_total             4000
_reflns_number_gt                3699
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0375P)²+24.7431P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.59(2)
_refine_ls_number_reflns         4000
_refine_ls_number_parameters     361
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0412
_refine_ls_wR_factor_ref         0.0939
_refine_ls_wR_factor_gt          0.0907
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu 0.16625(10) 1.01192(3) 0.1864(2) 0.01837(11) Uani 1 1 d . . .
C1 C 0.1528(6) 0.4286(8) 0.1499(14) 0.032(3) Uani 1 1 d . . .
H1A H 0.1472 0.3513 0.1390 0.038 Uiso 1 1 calc R . .
C2 C 0.1190(9) 0.4831(13) 0.2383(17) 0.030(4) Uani 1 1 d . . .
C3 C 0.1239(8) 0.5971(17) 0.2507(17) 0.023(4) Uani 1 1 d . . .
H3B H 0.0993 0.6362 0.3060 0.027 Uiso 1 1 calc R . .
C4 C 0.1654(11) 0.6532(7) 0.181(2) 0.023(2) Uani 1 1 d . . .
C5 C 0.1975(8) 0.5919(16) 0.0908(17) 0.025(4) Uani 1 1 d . . .
H5A H 0.2229 0.6310 0.0370 0.030 Uiso 1 1 calc R . .
C6 C 0.1691(11) 0.7787(7) 0.189(2) 0.024(2) Uani 1 1 d . . .
C7 C 0.0769(5) 0.4147(9) 0.3183(12) 0.029(3) Uani 1 1 d . . .
C8 C -0.0294(8) 0.8521(19) -0.2703(18) 0.033(5) Uani 1 1 d . . .
H8B H 0.0008 0.8423 -0.3292 0.040 Uiso 1 1 calc R . .
C9 C -0.0119(7) 0.9039(15) -0.1394(16) 0.017(3) Uani 1 1 d U . .
C10 C -0.0577(8) 0.9150(18) -0.061(2) 0.029(5) Uani 1 1 d . . .
H10A H -0.0468 0.9481 0.0281 0.035 Uiso 1 1 calc R . .
C11 C -0.1206(8) 0.8795(16) -0.1066(19) 0.024(4) Uani 1 1 d . . .
C12 C -0.1341(8) 0.8312(18) -0.2279(19) 0.033(4) Uani 1 1 d . . .
H12A H -0.1762 0.8056 -0.2588 0.039 Uiso 1 1 calc R . .
C13 C 0.0581(8) 0.9372(17) -0.0910(19) 0.020(4) Uani 1 1 d U . .
C14 C -0.1693(6) 0.9033(10) -0.0082(14) 0.037(3) Uani 1 1 d . . .
C15 C 0.4630(8) 1.1708(18) 0.1347(17) 0.032(4) Uani 1 1 d . . .
H15A H 0.5042 1.1997 0.1671 0.038 Uiso 1 1 calc R . .
C16 C 0.4164(8) 1.1851(18) 0.2188(17) 0.030(4) Uani 1 1 d . . .
C17 C 0.3543(8) 1.1465(17) 0.1598(17) 0.027(4) Uani 1 1 d . . .
H17A H 0.3218 1.1520 0.2135 0.033 Uiso 1 1 calc R . .
C18 C 0.3398(8) 1.1022(16) 0.0301(17) 0.020(3) Uani 1 1 d U . .
C19 C 0.3896(8) 1.0859(18) -0.051(2) 0.032(5) Uani 1 1 d . . .
H19A H 0.3800 1.0549 -0.1413 0.038 Uiso 1 1 calc R . .
C20 C 0.2747(8) 1.0628(17) -0.0368(17) 0.016(3) Uani 1 1 d U . .
C21 C 0.4327(6) 1.2320(14) 0.3638(15) 0.038(3) Uani 1 1 d . . .
N1 N 0.1938(7) 0.4804(12) 0.0774(15) 0.036(4) Uani 1 1 d . . .
N2 N -0.0913(7) 0.8159(14) -0.3112(13) 0.030(3) Uani 1 1 d . . .
N3 N 0.4518(6) 1.1163(16) 0.0066(16) 0.036(4) Uani 1 1 d . . .
O1W O 0.2009(5) 1.1804(12) 0.3148(11) 0.030(3) Uani 1 1 d . . .
H2A H 0.1706 1.2348 0.2970 0.045 Uiso 1 1 d R . .
H2B H 0.2374 1.2086 0.2912 0.045 Uiso 1 1 d R . .
O1 O 0.1465(5) 0.8308(11) 0.2763(11) 0.024(3) Uani 1 1 d . . .
O2 O 0.2008(5) 0.8283(11) 0.1018(11) 0.026(3) Uani 1 1 d . . .
O2W O 0.1166(5) 1.1677(11) 0.0414(11) 0.025(3) Uani 1 1 d . . .
H14A H 0.0714 1.1603 0.0101 0.038 Uiso 1 1 d R . .
H14B H 0.1335 1.1775 -0.0422 0.038 Uiso 1 1 d R . .
O3 O 0.0350(5) 0.4749(7) 0.3691(12) 0.048(2) Uani 1 1 d . . .
H3A H 0.0147 0.4345 0.4149 0.072 Uiso 1 1 calc R . .
O3W O 0.2904(15) 1.361(3) 0.330(4) 0.292(16) Uiso 1 1 d . . .
H3WA H 0.3040 1.3631 0.2514 0.351 Uiso 1 1 d R . .
H3WB H 0.3170 1.3231 0.3893 0.351 Uiso 1 1 d R . .
O4 O 0.0819(5) 0.3148(8) 0.3278(12) 0.059(3) Uani 1 1 d . . .
O5 O 0.0921(6) 0.9486(15) -0.1847(14) 0.036(4) Uani 1 1 d . . .
O6 O 0.0753(7) 0.9523(16) 0.0398(13) 0.033(3) Uani 1 1 d . . .
O7 O -0.1548(4) 0.9474(10) 0.1059(11) 0.059(3) Uani 1 1 d . . .
O8 O -0.2284(4) 0.8770(8) -0.0664(10) 0.042(2) Uani 1 1 d . . .
H8A H -0.2502 0.9344 -0.0817 0.063 Uiso 1 1 calc R . .
O9 O 0.2324(5) 1.0600(13) 0.0385(12) 0.023(3) Uani 1 1 d . . .
O10 O 0.2631(7) 1.0370(17) -0.1617(17) 0.039(4) Uani 1 1 d . . .
O11 O 0.3852(5) 1.2271(12) 0.4322(11) 0.062(3) Uani 1 1 d . . .
H11 H 0.3960 1.2566 0.5103 0.094 Uiso 1 1 calc R . .
O12 O 0.4855(5) 1.2707(10) 0.4079(11) 0.058(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Lu1 O5 2.206(13) 2_575 ?
Lu1 O9 2.233(12) . ?
Lu1 O6 2.267(13) . ?
Lu1 O10 2.346(14) 2_575 ?
Lu1 O1 2.384(13) . ?
Lu1 O1W 2.393(13) . ?
Lu1 O2W 2.432(12) . ?
Lu1 O2 2.483(13) . ?
Lu1 C6 2.773(8) . ?
C1 N1 1.35(2) . ?
C1 C2 1.36(2) . ?
C1 H1A 0.9300 . ?
C2 C3 1.36(2) . ?
C2 C7 1.51(2) . ?
C3 C4 1.36(3) . ?
C3 H3B 0.9300 . ?
C4 C5 1.40(3) . ?
C4 C6 1.495(11) . ?
C5 N1 1.33(2) . ?
C5 H5A 0.9300 . ?
C6 O1 1.20(2) . ?
C6 O2 1.30(2) . ?
C7 O4 1.194(14) . ?
C7 O3 1.296(13) . ?
C8 N2 1.36(2) . ?
C8 C9 1.38(2) . ?
C8 H8B 0.9300 . ?
C9 C10 1.33(2) . ?
C9 C13 1.51(2) . ?
C10 C11 1.38(2) . ?
C10 H10A 0.9300 . ?
C11 C12 1.28(2) . ?
C11 C14 1.54(2) . ?
C12 N2 1.32(2) . ?
C12 H12A 0.9300 . ?
C13 O6 1.25(2) . ?
C13 O5 1.25(2) . ?
C14 O7 1.200(15) . ?
C14 O8 1.301(14) . ?
C15 N3 1.37(2) . ?
C15 C16 1.39(2) . ?
C15 H15A 0.9300 . ?
C16 C17 1.40(2) . ?
C16 C21 1.48(2) . ?
C17 C18 1.33(2) . ?
C17 H17A 0.9300 . ?
C18 C19 1.42(2) . ?
C18 C20 1.47(2) . ?
C19 N3 1.37(2) . ?
C19 H19A 0.9300 . ?
C20 O10 1.22(2) . ?
C20 O9 1.24(2) . ?
C21 O12 1.202(15) . ?
C21 O11 1.292(14) . ?
O1W H2A 0.9001 . ?
O1W H2B 0.9020 . ?
O2W H14A 0.9460 . ?
O2W H14B 0.9401 . ?
O3 H3A 0.8200 . ?
O3W H3WA 0.8501 . ?
O3W H3WB 0.8501 . ?
O5 Lu1 2.206(13) 2_574 ?
O8 H8A 0.8200 . ?
O10 Lu1 2.346(14) 2_574 ?
O11 H11 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Lu1 O9 152.3(3) 2_575 . ?
O5 Lu1 O6 79.2(5) 2_575 . ?
O9 Lu1 O6 103.8(5) . . ?
O5 Lu1 O10 109.0(5) 2_575 2_575 ?
O9 Lu1 O10 83.6(5) . 2_575 ?
O6 Lu1 O10 147.4(3) . 2_575 ?
O5 Lu1 O1 78.6(5) 2_575 . ?
O9 Lu1 O1 129.1(5) . . ?
O6 Lu1 O1 76.0(5) . . ?
O10 Lu1 O1 75.0(5) 2_575 . ?
O5 Lu1 O1W 73.4(5) 2_575 . ?
O9 Lu1 O1W 86.9(5) . . ?
O6 Lu1 O1W 136.2(6) . . ?
O10 Lu1 O1W 75.0(6) 2_575 . ?
O1 Lu1 O1W 128.9(4) . . ?
O5 Lu1 O2W 83.4(5) 2_575 . ?
O9 Lu1 O2W 72.2(5) . . ?
O6 Lu1 O2W 70.1(6) . . ?
O10 Lu1 O2W 140.8(6) 2_575 . ?
O1 Lu1 O2W 144.0(4) . . ?
O1W Lu1 O2W 73.4(3) . . ?
O5 Lu1 O2 130.4(5) 2_575 . ?
O9 Lu1 O2 76.4(5) . . ?
O6 Lu1 O2 77.7(6) . . ?
O10 Lu1 O2 73.3(6) 2_575 . ?
O1 Lu1 O2 53.4(2) . . ?
O1W Lu1 O2 145.5(4) . . ?
O2W Lu1 O2 127.1(4) . . ?
O5 Lu1 C6 102.9(7) 2_575 . ?
O9 Lu1 C6 104.3(6) . . ?
O6 Lu1 C6 73.0(7) . . ?
O10 Lu1 C6 74.4(7) 2_575 . ?
O1 Lu1 C6 25.6(5) . . ?
O1W Lu1 C6 145.9(5) . . ?
O2W Lu1 C6 140.6(5) . . ?
O2 Lu1 C6 28.0(5) . . ?
N1 C1 C2 123.8(9) . . ?
N1 C1 H1A 118.1 . . ?
C2 C1 H1A 118.1 . . ?
C3 C2 C1 119.1(15) . . ?
C3 C2 C7 122.3(13) . . ?
C1 C2 C7 118.5(13) . . ?
C2 C3 C4 119.3(15) . . ?
C2 C3 H3B 120.3 . . ?
C4 C3 H3B 120.3 . . ?
C3 C4 C5 118.1(8) . . ?
C3 C4 C6 120(2) . . ?
C5 C4 C6 121.7(19) . . ?
N1 C5 C4 123.5(15) . . ?
N1 C5 H5A 118.2 . . ?
C4 C5 H5A 118.2 . . ?
O1 C6 O2 121.7(8) . . ?
O1 C6 C4 122(2) . . ?
O2 C6 C4 116.6(18) . . ?
O1 C6 Lu1 58.8(7) . . ?
O2 C6 Lu1 63.5(6) . . ?
C4 C6 Lu1 175.1(17) . . ?
O4 C7 O3 125.2(11) . . ?
O4 C7 C2 121.6(11) . . ?
O3 C7 C2 113.2(10) . . ?
N2 C8 C9 118.9(16) . . ?
N2 C8 H8B 120.6 . . ?
C9 C8 H8B 120.6 . . ?
C10 C9 C8 117.2(16) . . ?
C10 C9 C13 124.4(16) . . ?
C8 C9 C13 118.3(15) . . ?
C9 C10 C11 122.8(19) . . ?
C9 C10 H10A 118.6 . . ?
C11 C10 H10A 118.6 . . ?
C12 C11 C10 117.6(18) . . ?
C12 C11 C14 125.3(15) . . ?
C10 C11 C14 117.1(16) . . ?
C11 C12 N2 123.3(17) . . ?
C11 C12 H12A 118.3 . . ?
N2 C12 H12A 118.3 . . ?
O6 C13 O5 127.2(17) . . ?
O6 C13 C9 115.4(16) . . ?
O5 C13 C9 117.4(16) . . ?
O7 C14 O8 124.0(11) . . ?
O7 C14 C11 123.5(12) . . ?
O8 C14 C11 112.4(11) . . ?
N3 C15 C16 123.6(15) . . ?
N3 C15 H15A 118.2 . . ?
C16 C15 H15A 118.2 . . ?
C15 C16 C17 115.4(16) . . ?
C15 C16 C21 121.7(15) . . ?
C17 C16 C21 122.8(14) . . ?
C18 C17 C16 122.9(17) . . ?
C18 C17 H17A 118.5 . . ?
C16 C17 H17A 118.5 . . ?
C17 C18 C19 119.7(17) . . ?
C17 C18 C20 124.5(16) . . ?
C19 C18 C20 115.7(16) . . ?
N3 C19 C18 119.1(18) . . ?
N3 C19 H19A 120.4 . . ?
C18 C19 H19A 120.4 . . ?
O10 C20 O9 121.8(18) . . ?
O10 C20 C18 120.8(16) . . ?
O9 C20 C18 117.4(16) . . ?
O12 C21 O11 125.9(15) . . ?
O12 C21 C16 121.0(13) . . ?
O11 C21 C16 113.1(13) . . ?
C5 N1 C1 115.8(13) . . ?
C12 N2 C8 120.2(15) . . ?
C15 N3 C19 118.7(16) . . ?
Lu1 O1W H2A 111.5 . . ?
Lu1 O1W H2B 112.0 . . ?
H2A O1W H2B 106.7 . . ?
C6 O1 Lu1 95.6(9) . . ?
C6 O2 Lu1 88.5(7) . . ?
Lu1 O2W H14A 114.2 . . ?
Lu1 O2W H14B 113.0 . . ?
H14A O2W H14B 104.7 . . ?
C7 O3 H3A 109.5 . . ?
H3WA O3W H3WB 108.8 . . ?
C13 O5 Lu1 167.7(13) . 2_574 ?
C13 O6 Lu1 136.0(12) . . ?
C14 O8 H8A 109.5 . . ?
C20 O9 Lu1 165.7(14) . . ?
C20 O10 Lu1 132.0(14) . 2_574 ?
C21 O11 H11 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.19
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.136
