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

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

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1539850'
_audit_update_record             
;
2017-03-23 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C34 H26 Gd2 N2 O16, H2 O'
_chemical_formula_sum            'C34 H27 Gd2 N2 O17'
_chemical_formula_weight         1050.08
_chemical_melting_point          ?
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'
Gd Gd -0.1653 3.9035 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   6.9800(14)
_cell_length_b                   13.540(3)
_cell_length_c                   17.990(4)
_cell_angle_alpha                91.02(3)
_cell_angle_beta                 98.04(3)
_cell_angle_gamma                102.72(3)
_cell_volume                     1640.1(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4064
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_exptl_absorpt_coefficient_mu    4.097
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1018
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17085
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         3.02
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 17.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1390
	          2theta: 29.8560
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 17.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1390
	          2theta: 29.8560
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 17.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1390
	          2theta: 29.8560
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.017085
_diffrn_orient_matrix_UB_12      0.147264
_diffrn_orient_matrix_UB_13      0.005734
_diffrn_orient_matrix_UB_21      -0.057307
_diffrn_orient_matrix_UB_22      0.022093
_diffrn_orient_matrix_UB_23      0.044394
_diffrn_orient_matrix_UB_31      0.032676
_diffrn_orient_matrix_UB_32      0.002785
_diffrn_orient_matrix_UB_33      0.045628
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                6084
_reflns_number_total             7524
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.884
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         7524
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0432
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0387P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1056
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 H32B-O32
 0.85 with sigma of 0.001
 O32-H32A
 0.85 with sigma of 0.001
 H32B-H32A
 1.39 with sigma of 0.001
 H24B-O24
 0.85 with sigma of 0.01
 O24-H24A
 0.85 with sigma of 0.01
 H24A-H24B
 1.39 with sigma of 0.01
 H17B-O17
 0.85 with sigma of 0.01
 O17-H17A
 0.85 with sigma of 0.01
 H17A-H17B
 1.39 with sigma of 0.01
 H4A-O4
 0.85 with sigma of 0.01
 O4-H4B
 0.85 with sigma of 0.01
 H4B-H4A
 1.39 with sigma of 0.01
3.a Fixed occupancy and ADP/Uiso:
 H24B, H32A, H32B
3.b Riding coordinates:
 O17(H17A), O24(H24A)
3.c Rotating group:
 O3(H3A,H3B)
3.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C11(H11), C15(H15), C20(H20), C21(H21), C33(H33), C37(H37), C39(H39),
 C40(H40), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49),
  C52(H52), C53(H53)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Gd1 Gd 0.69576(3) 0.360751(16) 0.447293(11) 0.01596(5) Uani 1 d . . .
Gd2 Gd 0.75231(3) 0.360660(16) 0.060970(12) 0.01630(6) Uani 1 d . . .
O1 O 0.9271(5) 0.4501(2) 0.37037(17) 0.0244(8) Uani 1 d . . .
O2 O 0.6935(5) 0.5330(2) 0.08637(18) 0.0257(8) Uani 1 d . . .
O3 O 0.4042(5) 0.3363(3) 0.01113(19) 0.0265(8) Uani 1 d . . .
H3A H 0.3336 0.3138 0.0452 0.040 Uiso 1 d . . GR
H3B H 0.3744 0.2932 -0.0266 0.040 Uiso 1 d . . GR
C4 C 1.0903(6) 0.5494(3) 0.2468(2) 0.0188(10) Uani 1 d . . .
H4 H 1.0528 0.4790 0.2414 0.023 Uiso 1 calc . . R
O5 O 0.9661(5) 0.2598(3) 0.4490(2) 0.0314(9) Uani 1 d . . .
C6 C 0.6424(7) 0.5095(4) 0.1499(3) 0.0226(11) Uani 1 d . . .
O7 O 0.6063(5) 0.4166(2) 0.16635(18) 0.0276(8) Uani 1 d . . .
O8 O 0.6788(5) 0.1839(2) 0.48064(19) 0.0249(8) Uani 1 d . . .
O9 O 1.0590(5) 0.4617(2) 0.10033(18) 0.0253(8) Uani 1 d . . .
O10 O 0.9990(5) 0.2685(2) 0.0293(2) 0.0322(9) Uani 1 d . . .
C11 C 0.6014(6) 0.5592(4) 0.2796(3) 0.0203(10) Uani 1 d . . .
H11 H 0.5729 0.4906 0.2890 0.024 Uiso 1 calc . . R
C12 C 0.6049(7) 0.6290(3) 0.3370(2) 0.0181(10) Uani 1 d . . .
O13 O 0.6884(5) 0.1827(3) 0.0164(2) 0.0318(9) Uani 1 d . . .
O14 O 1.0845(5) 0.5834(3) 0.44682(17) 0.0283(9) Uani 1 d . . .
C15 C 0.6819(7) 0.6910(3) 0.1942(3) 0.0208(10) Uani 1 d . . .
H15 H 0.7067 0.7115 0.1467 0.025 Uiso 1 calc . . R
C16 C 1.0298(6) 0.5398(4) 0.3820(2) 0.0192(10) Uani 1 d . . .
O17 O 0.6495(5) 0.2786(3) 0.32030(19) 0.0327(9) Uani 1 d . . D
H17A H 0.5717 0.2193 0.3191 0.049 Uiso 1 d . . DR
O18 O 0.5888(6) 0.5084(3) 0.42933(19) 0.0334(9) Uani 1 d . . .
C19 C 1.1499(7) 0.5541(3) 0.1117(2) 0.0186(10) Uani 1 d . . .
C20 C 1.1400(7) 0.7043(3) 0.3226(2) 0.0201(10) Uani 1 d . . .
H20 H 1.1392 0.7368 0.3686 0.024 Uiso 1 calc . . R
C21 C 1.1948(7) 0.7114(3) 0.1931(3) 0.0196(10) Uani 1 d . . .
H21 H 1.2289 0.7484 0.1520 0.024 Uiso 1 calc . . R
O22 O 1.2409(5) 0.6038(3) 0.06386(18) 0.0271(8) Uani 1 d . . .
O23 O 0.4909(5) 0.3458(2) 0.54422(17) 0.0235(8) Uani 1 d . . .
O24 O 0.8534(5) 0.2779(3) 0.1744(2) 0.0376(10) Uani 1 d . . D
H24A H 0.7898 0.2177 0.1800 0.056 Uiso 1 d . . DR
H24B H 0.9763(13) 0.2831(15) 0.191(3) 0.056 Uiso 1 d . . D
N25 N 0.7830(7) 1.0802(3) 0.2095(3) 0.0365(12) Uani 1 d . . .
C26 C 1.1471(6) 0.6060(3) 0.1864(2) 0.0173(10) Uani 1 d . . .
C27 C 0.8547(7) 0.1836(3) 0.4711(2) 0.0208(10) Uani 1 d . . .
C28 C 0.5665(7) 0.5956(4) 0.4134(3) 0.0207(10) Uani 1 d . . .
C29 C 0.6878(7) 0.7636(4) 0.2514(3) 0.0214(10) Uani 1 d . . .
C30 C 0.9379(7) 0.0906(4) 0.0061(3) 0.0253(11) Uani 1 d . . .
C31 C 0.9306(7) 0.0882(4) 0.4867(3) 0.0212(10) Uani 1 d . . .
O32 O 0.3376(3) 0.30275(12) 0.39181(10) 0.0441(12) Uani 1 d . . D
H32A H 0.3354(7) 0.33823(18) 0.35333(15) 0.066 Uiso 1 d . . D
H32B H 0.2480(6) 0.2484(2) 0.3834(3) 0.066 Uiso 1 d . . D
C33 C 1.1350(7) 0.0922(4) 0.4945(3) 0.0270(12) Uani 1 d . . .
H33 H 1.2247 0.1532 0.4906 0.032 Uiso 1 calc . . R
C34 C 0.6389(7) 0.5879(3) 0.2083(2) 0.0189(10) Uani 1 d . . .
C35 C 0.8707(7) 0.1867(4) 0.0174(3) 0.0252(11) Uani 1 d . . .
C36 C 1.1919(7) 0.7629(4) 0.2620(3) 0.0220(11) Uani 1 d . . .
C37 C 1.1380(8) 0.0906(4) 0.0208(3) 0.0305(13) Uani 1 d . . .
H37 H 1.2316 0.1507 0.0347 0.037 Uiso 1 calc . . R
C38 C 0.7255(7) 0.8735(4) 0.2361(3) 0.0251(11) Uani 1 d . . .
C39 C 0.7979(7) -0.0035(4) 0.4918(3) 0.0293(12) Uani 1 d . . .
H39 H 0.6625 -0.0059 0.4861 0.035 Uiso 1 calc . . R
C40 C 0.8019(8) 0.0009(4) -0.0144(3) 0.0327(13) Uani 1 d . . .
H40 H 0.6676 0.0011 -0.0243 0.039 Uiso 1 calc . . R
C41 C 1.0899(6) 0.5993(3) 0.3160(2) 0.0165(10) Uani 1 d . . .
C42 C 1.2699(10) 1.0391(4) 0.2176(4) 0.0475(17) Uani 1 d . . .
H42 H 1.2450 1.0773 0.1764 0.057 Uiso 1 calc . . R
C43 C 1.2434(7) 0.8748(4) 0.2690(3) 0.0228(11) Uani 1 d . . .
C44 C 0.6664(8) 0.9074(4) 0.1656(3) 0.0295(12) Uani 1 d . . .
H44 H 0.6090 0.8617 0.1252 0.035 Uiso 1 calc . . R
C45 C 1.3294(8) 0.9268(4) 0.3380(3) 0.0322(13) Uani 1 d . . .
H45 H 1.3505 0.8912 0.3810 0.039 Uiso 1 calc . . R
C46 C 0.6950(9) 1.0098(4) 0.1573(3) 0.0358(14) Uani 1 d . . .
H46 H 0.6479 1.0311 0.1108 0.043 Uiso 1 calc . . R
C47 C 0.6479(7) 0.7311(4) 0.3223(3) 0.0218(10) Uani 1 d . . .
H47 H 0.6503 0.7789 0.3603 0.026 Uiso 1 calc . . R
C48 C 1.2129(9) 0.9347(4) 0.2081(3) 0.0356(14) Uani 1 d . . .
H48 H 1.1544 0.9044 0.1612 0.043 Uiso 1 calc . . R
C49 C 0.8456(9) 1.0488(4) 0.2776(3) 0.0342(13) Uani 1 d . . .
H49 H 0.9088 1.0971 0.3158 0.041 Uiso 1 calc . . R
N50 N 1.3590(8) 1.0883(3) 0.2828(3) 0.0467(14) Uani 1 d . . .
C52 C 0.8193(8) 0.9475(4) 0.2927(3) 0.0294(12) Uani 1 d . . .
H52 H 0.8636 0.9284 0.3403 0.035 Uiso 1 calc . . R
C53 C 1.3832(9) 1.0331(4) 0.3411(4) 0.0419(16) Uani 1 d . . .
H53 H 1.4393 1.0664 0.3873 0.050 Uiso 1 calc . . R
O4 O 1.2567(7) 0.3033(4) 0.2236(3) 0.0665(16) Uani 1 d . . D
H4A H 1.334(3) 0.3396(11) 0.1973(13) 0.100 Uiso 1 d . . DR
H4B H 1.292(4) 0.2476(10) 0.231(2) 0.100 Uiso 1 d . . DR
H17B H 0.7341(18) 0.2778(15) 0.2911(10) 0.12(4) Uiso 1 d . . D


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.410(3) . ?
Gd1 O5 2.560(4) . ?
Gd1 O8 2.460(3) . ?
Gd1 O14 2.275(3) 2_766 ?
Gd1 O17 2.471(3) . ?
Gd1 O18 2.296(3) . ?
Gd1 O23 2.389(3) . ?
Gd1 C27 2.872(5) . ?
Gd1 O32 2.505(2) . ?
Gd2 O2 2.501(3) . ?
Gd2 O3 2.417(3) . ?
Gd2 C6 2.850(5) . ?
Gd2 O7 2.457(3) . ?
Gd2 O9 2.282(3) . ?
Gd2 O10 2.458(4) . ?
Gd2 O13 2.450(3) . ?
Gd2 O22 2.310(3) 2_765 ?
Gd2 O24 2.438(4) . ?
Gd2 C35 2.796(5) . ?
O1 C16 1.265(5) . ?
O2 C6 1.270(6) . ?
O3 H3A 0.8587 . ?
O3 H3B 0.8598 . ?
C4 H4 0.9300 . ?
C4 C26 1.395(6) . ?
C4 C41 1.407(6) . ?
O5 C27 1.256(6) . ?
C6 O7 1.275(6) . ?
C6 C34 1.487(6) . ?
O8 C27 1.264(6) . ?
O9 C19 1.271(5) . ?
O10 C35 1.255(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.381(6) . ?
C11 C34 1.390(6) . ?
C12 C28 1.496(6) . ?
C12 C47 1.386(6) . ?
O13 C35 1.260(6) . ?
O14 Gd1 2.275(3) 2_766 ?
O14 C16 1.268(5) . ?
C15 H15 0.9300 . ?
C15 C29 1.401(6) . ?
C15 C34 1.398(6) . ?
C16 C41 1.502(6) . ?
O17 H17A 0.8634 . ?
O17 H17B 0.846(9) . ?
O18 C28 1.257(6) . ?
C19 O22 1.258(5) . ?
C19 C26 1.509(6) . ?
C20 H20 0.9300 . ?
C20 C36 1.403(6) . ?
C20 C41 1.386(6) . ?
C21 H21 0.9300 . ?
C21 C26 1.391(6) . ?
C21 C36 1.415(6) . ?
O22 Gd2 2.310(3) 2_765 ?
O23 C28 1.255(6) 2_666 ?
O24 H24A 0.8524 . ?
O24 H24B 0.854(9) . ?
N25 C46 1.311(7) . ?
N25 C49 1.351(7) . ?
C27 C31 1.516(6) . ?
C28 O23 1.255(6) 2_666 ?
C29 C38 1.490(7) . ?
C29 C47 1.402(6) . ?
C30 C35 1.498(7) . ?
C30 C37 1.385(7) . ?
C30 C40 1.375(7) . ?
C31 C33 1.403(7) . ?
C31 C39 1.389(7) . ?
O32 H32A 0.8499(10) . ?
O32 H32B 0.8499(11) . ?
C33 H33 0.9300 . ?
C33 C39 1.396(7) 2_756 ?
C36 C43 1.476(7) . ?
C37 H37 0.9300 . ?
C37 C40 1.401(7) 2_755 ?
C38 C44 1.395(7) . ?
C38 C52 1.399(7) . ?
C39 C33 1.396(7) 2_756 ?
C39 H39 0.9300 . ?
C40 C37 1.401(7) 2_755 ?
C40 H40 0.9300 . ?
C42 H42 0.9300 . ?
C42 C48 1.382(8) . ?
C42 N50 1.339(8) . ?
C43 C45 1.404(7) . ?
C43 C48 1.395(7) . ?
C44 H44 0.9300 . ?
C44 C46 1.370(7) . ?
C45 H45 0.9300 . ?
C45 C53 1.403(7) . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
C49 C52 1.380(7) . ?
N50 C53 1.313(8) . ?
C52 H52 0.9300 . ?
C53 H53 0.9300 . ?
O4 H4A 0.849(10) . ?
O4 H4B 0.851(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 O5 74.41(12) . . ?
O1 Gd1 O8 123.41(11) . . ?
O1 Gd1 O17 67.78(11) . . ?
O1 Gd1 C27 99.13(13) . . ?
O1 Gd1 O32 118.89(9) . . ?
O5 Gd1 C27 25.93(12) . . ?
O8 Gd1 O5 51.90(11) . . ?
O8 Gd1 O17 80.20(12) . . ?
O8 Gd1 C27 25.99(12) . . ?
O8 Gd1 O32 86.29(9) . . ?
O14 Gd1 O1 90.82(12) 2_766 . ?
O14 Gd1 O5 74.01(13) 2_766 . ?
O14 Gd1 O8 90.44(12) 2_766 . ?
O14 Gd1 O17 145.18(13) 2_766 . ?
O14 Gd1 O18 96.56(13) 2_766 . ?
O14 Gd1 O23 76.46(12) 2_766 . ?
O14 Gd1 C27 81.02(13) 2_766 . ?
O14 Gd1 O32 146.10(10) 2_766 . ?
O17 Gd1 O5 73.88(12) . . ?
O17 Gd1 C27 76.01(12) . . ?
O17 Gd1 O32 67.21(10) . . ?
O18 Gd1 O1 78.18(12) . . ?
O18 Gd1 O5 150.75(12) . . ?
O18 Gd1 O8 157.31(12) . . ?
O18 Gd1 O17 104.94(12) . . ?
O18 Gd1 O23 82.13(12) . . ?
O18 Gd1 C27 176.40(14) . . ?
O18 Gd1 O32 75.87(11) . . ?
O23 Gd1 O1 155.16(11) . . ?
O23 Gd1 O5 120.75(11) . . ?
O23 Gd1 O8 78.57(11) . . ?
O23 Gd1 O17 132.84(12) . . ?
O23 Gd1 C27 99.81(12) . . ?
O23 Gd1 O32 69.81(9) . . ?
O32 Gd1 O5 126.91(9) . . ?
O32 Gd1 C27 107.62(11) . . ?
O2 Gd2 C6 26.44(12) . . ?
O2 Gd2 C35 169.47(13) . . ?
O3 Gd2 O2 78.73(12) . . ?
O3 Gd2 C6 79.31(13) . . ?
O3 Gd2 O7 76.39(12) . . ?
O3 Gd2 O10 129.82(12) . . ?
O3 Gd2 O13 81.22(12) . . ?
O3 Gd2 O24 120.00(12) . . ?
O3 Gd2 C35 106.63(13) . . ?
O7 Gd2 O2 52.58(11) . . ?
O7 Gd2 C6 26.51(12) . . ?
O7 Gd2 O10 143.22(12) . . ?
O7 Gd2 C35 136.97(13) . . ?
O9 Gd2 O2 74.51(12) . . ?
O9 Gd2 O3 151.86(12) . . ?
O9 Gd2 C6 80.60(13) . . ?
O9 Gd2 O7 93.83(12) . . ?
O9 Gd2 O10 72.63(12) . . ?
O9 Gd2 O13 125.11(12) . . ?
O9 Gd2 O22 93.86(12) . 2_765 ?
O9 Gd2 O24 79.43(12) . . ?
O9 Gd2 C35 98.53(13) . . ?
O10 Gd2 O2 144.16(11) . . ?
O10 Gd2 C6 150.79(12) . . ?
O10 Gd2 C35 26.66(12) . . ?
O13 Gd2 O2 159.94(11) . . ?
O13 Gd2 C6 147.55(13) . . ?
O13 Gd2 O7 122.79(12) . . ?
O13 Gd2 O10 53.30(11) . . ?
O13 Gd2 C35 26.76(13) . . ?
O22 Gd2 O2 89.47(12) 2_765 . ?
O22 Gd2 O3 77.19(12) 2_765 . ?
O22 Gd2 C6 115.03(13) 2_765 . ?
O22 Gd2 O7 137.14(12) 2_765 . ?
O22 Gd2 O10 78.90(13) 2_765 . ?
O22 Gd2 O13 85.27(13) 2_765 . ?
O22 Gd2 O24 152.72(13) 2_765 . ?
O22 Gd2 C35 83.05(14) 2_765 . ?
O24 Gd2 O2 113.58(12) . . ?
O24 Gd2 C6 90.15(13) . . ?
O24 Gd2 O7 70.05(12) . . ?
O24 Gd2 O10 73.85(13) . . ?
O24 Gd2 O13 77.50(13) . . ?
O24 Gd2 C35 72.02(14) . . ?
C35 Gd2 C6 161.92(14) . . ?
C16 O1 Gd1 127.0(3) . . ?
C6 O2 Gd2 92.3(3) . . ?
Gd2 O3 H3A 109.5 . . ?
Gd2 O3 H3B 110.0 . . ?
H3A O3 H3B 108.9 . . ?
C26 C4 H4 120.2 . . ?
C26 C4 C41 119.6(4) . . ?
C41 C4 H4 120.2 . . ?
C27 O5 Gd1 91.0(3) . . ?
O2 C6 Gd2 61.3(2) . . ?
O2 C6 O7 119.3(4) . . ?
O2 C6 C34 121.8(4) . . ?
O7 C6 Gd2 59.3(2) . . ?
O7 C6 C34 118.7(4) . . ?
C34 C6 Gd2 164.3(3) . . ?
C6 O7 Gd2 94.2(3) . . ?
C27 O8 Gd1 95.5(3) . . ?
C19 O9 Gd2 142.2(3) . . ?
C35 O10 Gd2 91.8(3) . . ?
C12 C11 H11 118.9 . . ?
C12 C11 C34 122.3(4) . . ?
C34 C11 H11 118.9 . . ?
C11 C12 C28 120.9(4) . . ?
C11 C12 C47 118.3(4) . . ?
C47 C12 C28 120.8(4) . . ?
C35 O13 Gd2 92.1(3) . . ?
C16 O14 Gd1 154.5(3) . 2_766 ?
C29 C15 H15 120.0 . . ?
C34 C15 H15 120.0 . . ?
C34 C15 C29 120.1(4) . . ?
O1 C16 O14 123.5(4) . . ?
O1 C16 C41 119.0(4) . . ?
O14 C16 C41 117.5(4) . . ?
Gd1 O17 H17A 109.8 . . ?
Gd1 O17 H17B 129.2(12) . . ?
H17A O17 H17B 109.4 . . ?
C28 O18 Gd1 166.9(3) . . ?
O9 C19 C26 117.9(4) . . ?
O22 C19 O9 123.1(4) . . ?
O22 C19 C26 118.9(4) . . ?
C36 C20 H20 119.1 . . ?
C41 C20 H20 119.1 . . ?
C41 C20 C36 121.8(4) . . ?
C26 C21 H21 119.7 . . ?
C26 C21 C36 120.6(4) . . ?
C36 C21 H21 119.7 . . ?
C19 O22 Gd2 147.6(3) . 2_765 ?
C28 O23 Gd1 137.3(3) 2_666 . ?
Gd2 O24 H24A 117.9 . . ?
Gd2 O24 H24B 120(2) . . ?
H24A O24 H24B 109.1 . . ?
C46 N25 C49 117.0(5) . . ?
C4 C26 C19 120.5(4) . . ?
C21 C26 C4 120.5(4) . . ?
C21 C26 C19 118.9(4) . . ?
O5 C27 Gd1 63.1(2) . . ?
O5 C27 O8 121.5(4) . . ?
O5 C27 C31 119.8(4) . . ?
O8 C27 Gd1 58.5(2) . . ?
O8 C27 C31 118.7(4) . . ?
C31 C27 Gd1 176.9(3) . . ?
O18 C28 C12 116.7(4) . . ?
O23 C28 C12 118.5(4) 2_666 . ?
O23 C28 O18 124.7(4) 2_666 . ?
C15 C29 C38 120.5(4) . . ?
C15 C29 C47 119.0(4) . . ?
C47 C29 C38 120.4(4) . . ?
C37 C30 C35 119.8(5) . . ?
C40 C30 C35 120.6(5) . . ?
C40 C30 C37 119.5(5) . . ?
C33 C31 C27 119.9(4) . . ?
C39 C31 C27 120.2(4) . . ?
C39 C31 C33 119.9(4) . . ?
Gd1 O32 H32A 100.0(3) . . ?
Gd1 O32 H32B 139.7(3) . . ?
H32A O32 H32B 109.71(18) . . ?
C31 C33 H33 120.4 . . ?
C39 C33 C31 119.1(5) 2_756 . ?
C39 C33 H33 120.4 2_756 . ?
C11 C34 C6 119.8(4) . . ?
C11 C34 C15 118.9(4) . . ?
C15 C34 C6 121.2(4) . . ?
O10 C35 Gd2 61.5(3) . . ?
O10 C35 O13 122.2(5) . . ?
O10 C35 C30 118.7(4) . . ?
O13 C35 Gd2 61.1(3) . . ?
O13 C35 C30 119.1(4) . . ?
C30 C35 Gd2 171.5(3) . . ?
C20 C36 C21 117.9(4) . . ?
C20 C36 C43 121.7(4) . . ?
C21 C36 C43 120.5(4) . . ?
C30 C37 H37 120.3 . . ?
C30 C37 C40 119.3(5) . 2_755 ?
C40 C37 H37 120.3 2_755 . ?
C44 C38 C29 121.9(4) . . ?
C44 C38 C52 117.1(5) . . ?
C52 C38 C29 121.0(4) . . ?
C31 C39 C33 121.0(5) . 2_756 ?
C31 C39 H39 119.5 . . ?
C33 C39 H39 119.5 2_756 . ?
C30 C40 C37 121.2(5) . 2_755 ?
C30 C40 H40 119.4 . . ?
C37 C40 H40 119.4 2_755 . ?
C4 C41 C16 120.5(4) . . ?
C20 C41 C4 119.6(4) . . ?
C20 C41 C16 119.9(4) . . ?
C48 C42 H42 118.2 . . ?
N50 C42 H42 118.2 . . ?
N50 C42 C48 123.7(6) . . ?
C45 C43 C36 121.2(4) . . ?
C48 C43 C36 122.5(4) . . ?
C48 C43 C45 116.3(5) . . ?
C38 C44 H44 120.8 . . ?
C46 C44 C38 118.3(5) . . ?
C46 C44 H44 120.8 . . ?
C43 C45 H45 120.4 . . ?
C53 C45 C43 119.1(5) . . ?
C53 C45 H45 120.4 . . ?
N25 C46 C44 125.5(5) . . ?
N25 C46 H46 117.3 . . ?
C44 C46 H46 117.3 . . ?
C12 C47 C29 121.4(4) . . ?
C12 C47 H47 119.3 . . ?
C29 C47 H47 119.3 . . ?
C42 C48 C43 119.9(5) . . ?
C42 C48 H48 120.0 . . ?
C43 C48 H48 120.0 . . ?
N25 C49 H49 118.8 . . ?
N25 C49 C52 122.4(5) . . ?
C52 C49 H49 118.8 . . ?
C53 N50 C42 117.0(5) . . ?
C38 C52 H52 120.1 . . ?
C49 C52 C38 119.7(5) . . ?
C49 C52 H52 120.1 . . ?
C45 C53 H53 118.0 . . ?
N50 C53 C45 123.9(5) . . ?
N50 C53 H53 118.0 . . ?
H4A O4 H4B 109.6(16) . . ?

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
Gd1 O1 C16 O14 27.4(6) . . . . ?
Gd1 O1 C16 C41 -152.0(3) . . . . ?
Gd1 O5 C27 O8 1.8(4) . . . . ?
Gd1 O5 C27 C31 -178.5(4) . . . . ?
Gd1 O8 C27 O5 -1.9(5) . . . . ?
Gd1 O8 C27 C31 178.5(3) . . . . ?
Gd1 O14 C16 O1 99.7(8) 2_766 . . . ?
Gd1 O14 C16 C41 -80.9(8) 2_766 . . . ?
Gd1 O18 C28 C12 46.5(16) . . . . ?
Gd1 O18 C28 O23 -135.8(12) . . . 2_666 ?
Gd1 C27 C31 C33 -140(6) . . . . ?
Gd1 C27 C31 C39 41(6) . . . . ?
Gd2 O2 C6 O7 -12.8(4) . . . . ?
Gd2 O2 C6 C34 162.2(4) . . . . ?
Gd2 C6 C34 C11 -76.7(13) . . . . ?
Gd2 C6 C34 C15 100.3(12) . . . . ?
Gd2 O9 C19 O22 -95.1(6) . . . . ?
Gd2 O9 C19 C26 84.7(6) . . . . ?
Gd2 O10 C35 O13 7.9(5) . . . . ?
Gd2 O10 C35 C30 -170.4(4) . . . . ?
Gd2 O13 C35 O10 -7.9(5) . . . . ?
Gd2 O13 C35 C30 170.3(4) . . . . ?
O1 Gd1 O5 C27 -161.9(3) . . . . ?
O1 Gd1 O8 C27 23.1(3) . . . . ?
O1 Gd1 O18 C28 -10.0(14) . . . . ?
O1 Gd1 O23 C28 8.8(6) . . . 2_666 ?
O1 Gd1 C27 O5 17.6(3) . . . . ?
O1 Gd1 C27 O8 -160.6(3) . . . . ?
O1 Gd1 C27 C31 174(6) . . . . ?
O1 C16 C41 C4 -20.3(6) . . . . ?
O1 C16 C41 C20 157.9(4) . . . . ?
O2 Gd2 C6 O7 167.1(4) . . . . ?
O2 Gd2 C6 C34 -105.8(13) . . . . ?
O2 Gd2 O7 C6 -7.2(2) . . . . ?
O2 Gd2 O9 C19 -14.3(5) . . . . ?
O2 Gd2 O10 C35 -169.9(3) . . . . ?
O2 Gd2 O13 C35 159.2(3) . . . . ?
O2 Gd2 C35 O10 34.1(8) . . . . ?
O2 Gd2 C35 O13 -138.3(6) . . . . ?
O2 Gd2 C35 C30 128(2) . . . . ?
O2 C6 O7 Gd2 13.0(4) . . . . ?
O2 C6 C34 C11 -173.6(4) . . . . ?
O2 C6 C34 C15 3.4(7) . . . . ?
O3 Gd2 O2 C6 88.6(3) . . . . ?
O3 Gd2 C6 O2 -86.2(3) . . . . ?
O3 Gd2 C6 O7 80.9(3) . . . . ?
O3 Gd2 C6 C34 168.0(13) . . . . ?
O3 Gd2 O7 C6 -93.3(3) . . . . ?
O3 Gd2 O9 C19 4.3(6) . . . . ?
O3 Gd2 O10 C35 -33.9(4) . . . . ?
O3 Gd2 O13 C35 161.7(3) . . . . ?
O3 Gd2 C35 O10 153.5(3) . . . . ?
O3 Gd2 C35 O13 -18.9(3) . . . . ?
O3 Gd2 C35 C30 -113(2) . . . . ?
O5 Gd1 O1 C16 -117.9(4) . . . . ?
O5 Gd1 O8 C27 1.0(2) . . . . ?
O5 Gd1 O18 C28 10.7(16) . . . . ?
O5 Gd1 O23 C28 131.5(4) . . . 2_666 ?
O5 Gd1 C27 O8 -178.2(4) . . . . ?
O5 Gd1 C27 C31 156(6) . . . . ?
O5 C27 C31 C33 15.8(7) . . . . ?
O5 C27 C31 C39 -163.1(5) . . . . ?
C6 Gd2 O9 C19 -40.7(5) . . . . ?
C6 Gd2 O10 C35 141.2(3) . . . . ?
C6 Gd2 O13 C35 -144.7(3) . . . . ?
C6 Gd2 C35 O10 -99.6(5) . . . . ?
C6 Gd2 C35 O13 88.0(5) . . . . ?
C6 Gd2 C35 C30 -6(3) . . . . ?
O7 Gd2 O2 C6 7.2(3) . . . . ?
O7 Gd2 C6 O2 -167.1(4) . . . . ?
O7 Gd2 C6 C34 87.1(13) . . . . ?
O7 Gd2 O9 C19 -63.7(5) . . . . ?
O7 Gd2 O10 C35 93.2(3) . . . . ?
O7 Gd2 O13 C35 -130.8(3) . . . . ?
O7 Gd2 C35 O10 -118.8(3) . . . . ?
O7 Gd2 C35 O13 68.8(3) . . . . ?
O7 Gd2 C35 C30 -25(2) . . . . ?
O7 C6 C34 C11 1.4(7) . . . . ?
O7 C6 C34 C15 178.4(4) . . . . ?
O8 Gd1 O1 C16 -135.9(3) . . . . ?
O8 Gd1 O5 C27 -1.0(2) . . . . ?
O8 Gd1 O18 C28 -173.4(13) . . . . ?
O8 Gd1 O23 C28 163.0(5) . . . 2_666 ?
O8 Gd1 C27 O5 178.2(4) . . . . ?
O8 Gd1 C27 C31 -26(6) . . . . ?
O8 C27 C31 C33 -164.6(4) . . . . ?
O8 C27 C31 C39 16.6(7) . . . . ?
O9 Gd2 O2 C6 -100.2(3) . . . . ?
O9 Gd2 C6 O2 74.0(3) . . . . ?
O9 Gd2 C6 O7 -118.9(3) . . . . ?
O9 Gd2 C6 C34 -31.8(12) . . . . ?
O9 Gd2 O7 C6 59.9(3) . . . . ?
O9 Gd2 O10 C35 165.7(3) . . . . ?
O9 Gd2 O13 C35 -7.5(4) . . . . ?
O9 Gd2 C35 O10 -13.8(3) . . . . ?
O9 Gd2 C35 O13 173.8(3) . . . . ?
O9 Gd2 C35 C30 80(2) . . . . ?
O9 C19 O22 Gd2 39.5(9) . . . 2_765 ?
O9 C19 C26 C4 15.4(6) . . . . ?
O9 C19 C26 C21 -162.2(4) . . . . ?
O10 Gd2 O2 C6 -124.3(3) . . . . ?
O10 Gd2 C6 O2 97.7(3) . . . . ?
O10 Gd2 C6 O7 -95.2(4) . . . . ?
O10 Gd2 C6 C34 -8.1(14) . . . . ?
O10 Gd2 O7 C6 125.7(3) . . . . ?
O10 Gd2 O9 C19 151.2(5) . . . . ?
O10 Gd2 O13 C35 4.3(3) . . . . ?
O10 Gd2 C35 O13 -172.4(5) . . . . ?
O10 Gd2 C35 C30 93(2) . . . . ?
C11 C12 C28 O18 20.2(6) . . . . ?
C11 C12 C28 O23 -157.7(4) . . . 2_666 ?
C11 C12 C47 C29 -0.2(7) . . . . ?
C12 C11 C34 C6 177.1(4) . . . . ?
C12 C11 C34 C15 0.1(7) . . . . ?
O13 Gd2 O2 C6 91.1(4) . . . . ?
O13 Gd2 C6 O2 -140.3(3) . . . . ?
O13 Gd2 C6 O7 26.8(4) . . . . ?
O13 Gd2 C6 C34 113.9(12) . . . . ?
O13 Gd2 O7 C6 -163.3(3) . . . . ?
O13 Gd2 O9 C19 161.0(5) . . . . ?
O13 Gd2 O10 C35 -4.3(3) . . . . ?
O13 Gd2 C35 O10 172.4(5) . . . . ?
O13 Gd2 C35 C30 -94(2) . . . . ?
O14 Gd1 O1 C16 -44.8(4) 2_766 . . . ?
O14 Gd1 O5 C27 102.6(3) 2_766 . . . ?
O14 Gd1 O8 C27 -68.2(3) 2_766 . . . ?
O14 Gd1 O18 C28 79.5(14) 2_766 . . . ?
O14 Gd1 O23 C28 69.7(4) 2_766 . . 2_666 ?
O14 Gd1 C27 O5 -71.8(3) 2_766 . . . ?
O14 Gd1 C27 O8 110.0(3) 2_766 . . . ?
O14 Gd1 C27 C31 84(6) 2_766 . . . ?
O14 C16 C41 C4 160.3(4) . . . . ?
O14 C16 C41 C20 -21.5(6) . . . . ?
C15 C29 C38 C44 30.6(7) . . . . ?
C15 C29 C38 C52 -150.6(5) . . . . ?
C15 C29 C47 C12 0.6(7) . . . . ?
O17 Gd1 O1 C16 163.5(4) . . . . ?
O17 Gd1 O5 C27 -91.1(3) . . . . ?
O17 Gd1 O8 C27 78.1(3) . . . . ?
O17 Gd1 O18 C28 -72.9(14) . . . . ?
O17 Gd1 O23 C28 -132.1(4) . . . 2_666 ?
O17 Gd1 C27 O5 81.8(3) . . . . ?
O17 Gd1 C27 O8 -96.4(3) . . . . ?
O17 Gd1 C27 C31 -122(6) . . . . ?
O18 Gd1 O1 C16 51.7(4) . . . . ?
O18 Gd1 O5 C27 177.0(3) . . . . ?
O18 Gd1 O8 C27 -176.5(3) . . . . ?
O18 Gd1 O23 C28 -29.0(4) . . . 2_666 ?
O18 Gd1 C27 O5 -24(2) . . . . ?
O18 Gd1 C27 O8 157.9(18) . . . . ?
O18 Gd1 C27 C31 132(5) . . . . ?
C20 C36 C43 C45 29.2(7) . . . . ?
C20 C36 C43 C48 -151.8(5) . . . . ?
C21 C36 C43 C45 -150.4(5) . . . . ?
C21 C36 C43 C48 28.6(7) . . . . ?
O22 Gd2 O2 C6 165.7(3) 2_765 . . . ?
O22 Gd2 C6 O2 -15.9(3) 2_765 . . . ?
O22 Gd2 C6 O7 151.2(3) 2_765 . . . ?
O22 Gd2 C6 C34 -121.7(12) 2_765 . . . ?
O22 Gd2 O7 C6 -39.9(3) 2_765 . . . ?
O22 Gd2 O9 C19 74.1(5) 2_765 . . . ?
O22 Gd2 O10 C35 -96.6(3) 2_765 . . . ?
O22 Gd2 O13 C35 83.9(3) 2_765 . . . ?
O22 Gd2 C35 O10 79.1(3) 2_765 . . . ?
O22 Gd2 C35 O13 -93.3(3) 2_765 . . . ?
O22 Gd2 C35 C30 173(2) 2_765 . . . ?
O22 C19 C26 C4 -164.8(4) . . . . ?
O22 C19 C26 C21 17.6(7) . . . . ?
O23 Gd1 O1 C16 13.4(5) . . . . ?
O23 Gd1 O5 C27 39.6(3) . . . . ?
O23 Gd1 O8 C27 -144.2(3) . . . . ?
O23 Gd1 O18 C28 154.8(14) . . . . ?
O23 Gd1 C27 O5 -146.2(3) . . . . ?
O23 Gd1 C27 O8 35.5(3) . . . . ?
O23 Gd1 C27 C31 10(6) . . . . ?
O24 Gd2 O2 C6 -29.4(3) . . . . ?
O24 Gd2 C6 O2 153.3(3) . . . . ?
O24 Gd2 C6 O7 -39.7(3) . . . . ?
O24 Gd2 C6 C34 47.5(12) . . . . ?
O24 Gd2 O7 C6 137.2(3) . . . . ?
O24 Gd2 O9 C19 -132.6(5) . . . . ?
O24 Gd2 O10 C35 82.0(3) . . . . ?
O24 Gd2 O13 C35 -74.8(3) . . . . ?
O24 Gd2 C35 O10 -89.7(3) . . . . ?
O24 Gd2 C35 O13 97.9(3) . . . . ?
O24 Gd2 C35 C30 4(2) . . . . ?
N25 C49 C52 C38 0.3(9) . . . . ?
C26 C4 C41 C16 -179.8(4) . . . . ?
C26 C4 C41 C20 2.0(7) . . . . ?
C26 C19 O22 Gd2 -140.3(5) . . . 2_765 ?
C26 C21 C36 C20 0.1(7) . . . . ?
C26 C21 C36 C43 179.7(4) . . . . ?
C27 Gd1 O1 C16 -125.8(4) . . . . ?
C27 Gd1 O18 C28 32(3) . . . . ?
C27 Gd1 O23 C28 147.9(4) . . . 2_666 ?
C27 C31 C33 C39 -179.5(4) . . . 2_756 ?
C27 C31 C39 C33 179.5(4) . . . 2_756 ?
C28 C12 C47 C29 178.8(4) . . . . ?
C29 C15 C34 C6 -176.7(4) . . . . ?
C29 C15 C34 C11 0.4(7) . . . . ?
C29 C38 C44 C46 175.8(5) . . . . ?
C29 C38 C52 C49 -177.6(5) . . . . ?
O32 Gd1 O1 C16 118.1(3) . . . . ?
O32 Gd1 O5 C27 -47.2(3) . . . . ?
O32 Gd1 O8 C27 145.6(3) . . . . ?
O32 Gd1 O18 C28 -134.2(14) . . . . ?
O32 Gd1 O23 C28 -106.8(5) . . . 2_666 ?
O32 Gd1 C27 O5 142.0(3) . . . . ?
O32 Gd1 C27 O8 -36.2(3) . . . . ?
O32 Gd1 C27 C31 -62(6) . . . . ?
C33 C31 C39 C33 0.6(8) . . . 2_756 ?
C34 C6 O7 Gd2 -162.1(4) . . . . ?
C34 C11 C12 C28 -179.2(4) . . . . ?
C34 C11 C12 C47 -0.1(7) . . . . ?
C34 C15 C29 C38 -177.6(4) . . . . ?
C34 C15 C29 C47 -0.7(7) . . . . ?
C35 Gd2 O2 C6 -149.7(6) . . . . ?
C35 Gd2 C6 O2 162.7(4) . . . . ?
C35 Gd2 C6 O7 -30.2(6) . . . . ?
C35 Gd2 C6 C34 56.9(14) . . . . ?
C35 Gd2 O7 C6 166.8(3) . . . . ?
C35 Gd2 O9 C19 157.6(5) . . . . ?
C35 C30 C37 C40 176.1(5) . . . 2_755 ?
C35 C30 C40 C37 -176.1(5) . . . 2_755 ?
C36 C20 C41 C4 -0.1(7) . . . . ?
C36 C20 C41 C16 -178.3(4) . . . . ?
C36 C21 C26 C4 1.8(7) . . . . ?
C36 C21 C26 C19 179.4(4) . . . . ?
C36 C43 C45 C53 177.4(5) . . . . ?
C36 C43 C48 C42 -178.0(6) . . . . ?
C37 C30 C35 Gd2 -79(2) . . . . ?
C37 C30 C35 O10 10.3(7) . . . . ?
C37 C30 C35 O13 -168.0(5) . . . . ?
C37 C30 C40 C37 0.1(9) . . . 2_755 ?
C38 C29 C47 C12 177.5(4) . . . . ?
C38 C44 C46 N25 3.6(9) . . . . ?
C39 C31 C33 C39 -0.6(8) . . . 2_756 ?
C40 C30 C35 Gd2 98(2) . . . . ?
C40 C30 C35 O10 -173.5(5) . . . . ?
C40 C30 C35 O13 8.2(7) . . . . ?
C40 C30 C37 C40 -0.1(9) . . . 2_755 ?
C41 C4 C26 C19 179.6(4) . . . . ?
C41 C4 C26 C21 -2.8(7) . . . . ?
C41 C20 C36 C21 -1.0(7) . . . . ?
C41 C20 C36 C43 179.4(4) . . . . ?
C42 N50 C53 C45 2.9(10) . . . . ?
C43 C45 C53 N50 -0.4(9) . . . . ?
C44 C38 C52 C49 1.3(8) . . . . ?
C45 C43 C48 C42 1.1(8) . . . . ?
C46 N25 C49 C52 -0.1(9) . . . . ?
C47 C12 C28 O18 -158.9(4) . . . . ?
C47 C12 C28 O23 23.3(7) . . . 2_666 ?
C47 C29 C38 C44 -146.2(5) . . . . ?
C47 C29 C38 C52 32.6(7) . . . . ?
C48 C42 N50 C53 -3.5(10) . . . . ?
C48 C43 C45 C53 -1.6(8) . . . . ?
C49 N25 C46 C44 -1.9(9) . . . . ?
N50 C42 C48 C43 1.5(10) . . . . ?
C52 C38 C44 C46 -3.0(8) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_777
_audit_block_doi                 10.5517/cc1j7mft
_database_code_depnum_ccdc_archive 'CCDC 1407506'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H19 N2 O10 Pr'
_chemical_formula_sum            'C26 H19 N2 O10 Pr'
_chemical_formula_weight         660.34
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.686(3)
_cell_length_b                   16.758(3)
_cell_length_c                   10.336(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.78(3)
_cell_angle_gamma                90
_cell_volume                     2459.6(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6465
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.045
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0873
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24913
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.518
_diffrn_reflns_theta_min         3.030
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1494
	          2theta: 29.8651
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1494
	          2theta: 29.8651
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1494
	          2theta: 29.8651
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.072701
_diffrn_orient_matrix_UB_12      -0.026879
_diffrn_orient_matrix_UB_13      0.063268
_diffrn_orient_matrix_UB_21      -0.036269
_diffrn_orient_matrix_UB_22      -0.040607
_diffrn_orient_matrix_UB_23      0.024425
_diffrn_orient_matrix_UB_31      0.034865
_diffrn_orient_matrix_UB_32      -0.051248
_diffrn_orient_matrix_UB_33      -0.033428
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5004
_reflns_number_total             5632
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.730
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5632
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0416
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0486P)²+4.1245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1107
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 C32, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C39 \\sim C32 \\sim N2 \\sim C41 \\sim C29: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
4.a Riding coordinates:
 O6(H6A,H6B), O2(H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C17(H17), C19(H19), C29(H29), C30(H30),
 C32(H32), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C41(H41)
4.c Idealised tetrahedral OH refined as rotating group:
 O8(H8)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.20233(2) 0.31450(2) 0.13525(2) 0.01889(9) Uani 1 1 d . . . . .
O10 O 0.3283(2) 0.2751(2) 0.0360(3) 0.0421(8) Uani 1 1 d . . . . .
O7 O 0.0878(2) 0.26148(17) 0.2428(3) 0.0303(7) Uani 1 1 d . . . . .
O3 O 0.1055(2) 0.43885(18) 0.1340(3) 0.0343(7) Uani 1 1 d . . . . .
O4 O 0.2036(2) 0.41197(16) 0.3294(3) 0.0294(6) Uani 1 1 d . . . . .
O1 O 0.0911(3) 0.31461(19) -0.0803(3) 0.0422(9) Uani 1 1 d . . . . .
O5 O 0.3102(2) 0.25750(17) 0.3227(3) 0.0280(6) Uani 1 1 d . . . . .
O6 O 0.1775(3) 0.16484(19) 0.0616(4) 0.0411(8) Uani 1 1 d . . . . .
H6A H 0.130555 0.139173 0.073964 0.049 Uiso 1 1 d R . . . .
H6B H 0.216425 0.141943 0.025394 0.049 Uiso 1 1 d R . . . .
O2 O 0.3037(3) 0.4295(2) 0.1129(4) 0.0440(8) Uani 1 1 d . . . . .
H2A H 0.293976 0.475017 0.143219 0.053 Uiso 1 1 d R . . . .
H2B H 0.348186 0.423407 0.074889 0.053 Uiso 1 1 d R . . . .
C10 C 0.4449(3) 0.1927(2) -0.0178(4) 0.0235(8) Uani 1 1 d . . . . .
C11 C 0.3540(3) 0.2400(2) -0.0558(4) 0.0229(8) Uani 1 1 d . . . . .
C12 C 0.1396(3) 0.4553(2) 0.2547(4) 0.0256(8) Uani 1 1 d . . . . .
C13 C 0.5009(3) 0.1919(2) 0.1130(4) 0.0275(9) Uani 1 1 d . . . . .
H13 H 0.483235 0.221484 0.178745 0.033 Uiso 1 1 calc R . . . .
C14 C -0.0435(3) 0.0808(2) 0.2684(4) 0.0253(8) Uani 1 1 d . . . . .
H14 H -0.022611 0.070834 0.359664 0.030 Uiso 1 1 calc R . . . .
C15 C 0.1354(3) 0.5422(2) 0.4506(4) 0.0252(8) Uani 1 1 d . . . . .
H15 H 0.175282 0.505720 0.505179 0.030 Uiso 1 1 calc R . . . .
C16 C -0.0121(3) 0.1486(2) 0.2130(4) 0.0240(8) Uani 1 1 d . . . . .
C17 C 0.6083(3) 0.1006(3) 0.0476(5) 0.0332(10) Uani 1 1 d . . . . .
H17 H 0.662043 0.068902 0.070483 0.040 Uiso 1 1 calc R . . . .
C18 C 0.0612(3) 0.2024(2) 0.2982(4) 0.0248(8) Uani 1 1 d . . . . .
C19 C 0.4722(3) 0.1483(2) -0.1154(4) 0.0254(8) Uani 1 1 d . . . . .
H19 H 0.435447 0.149540 -0.203165 0.031 Uiso 1 1 calc R . . . .
C20 C 0.1064(3) 0.5285(2) 0.3140(4) 0.0246(8) Uani 1 1 d . . . . .
C21 C 0.1057(3) 0.6099(2) 0.5078(4) 0.0251(8) Uani 1 1 d . . . . .
O8 O 0.7147(3) 0.1010(3) 0.3142(4) 0.0633(12) Uani 1 1 d . . . . .
H8 H 0.742991 0.106182 0.393070 0.095 Uiso 1 1 calc GR . . . .
O9 O 0.6315(4) 0.2012(3) 0.3655(4) 0.0738(15) Uani 1 1 d . . . . .
C25 C 0.6449(4) 0.1508(4) 0.2852(6) 0.0506(14) Uani 1 1 d . . . . .
C26 C 0.5830(3) 0.1468(3) 0.1457(4) 0.0323(9) Uani 1 1 d . . . . .
C27 C 0.5537(3) 0.1018(3) -0.0836(4) 0.0302(9) Uani 1 1 d . . . . .
C28 C 0.5821(3) 0.0564(3) -0.1911(5) 0.0309(9) Uani 1 1 d . . . . .
C29 C 0.1271(5) 0.5596(5) 0.7417(6) 0.0647(15) Uani 1 1 d . U . . .
H29 H 0.103250 0.510956 0.704756 0.078 Uiso 1 1 calc R . . . .
C30 C 0.6212(4) -0.0197(3) -0.1699(5) 0.0402(11) Uani 1 1 d . . . . .
H30 H 0.631927 -0.043647 -0.086189 0.048 Uiso 1 1 calc R . . . .
N2 N 0.1911(4) 0.6296(4) 0.9301(6) 0.0740(15) Uani 1 1 d . U . . .
C32 C 0.2051(6) 0.6940(5) 0.8615(8) 0.0729(17) Uani 1 1 d . U . . .
H32 H 0.234912 0.738651 0.906547 0.087 Uiso 1 1 calc R . . . .
N1 N 0.6330(3) -0.0290(3) -0.3965(5) 0.0481(11) Uani 1 1 d . . . . .
C34 C 0.5963(4) 0.0444(4) -0.4159(6) 0.0516(14) Uani 1 1 d . . . . .
H34 H 0.587906 0.067218 -0.500166 0.062 Uiso 1 1 calc R . . . .
C35 C 0.0452(3) 0.6636(2) 0.4247(4) 0.0258(8) Uani 1 1 d . . . . .
H35 H 0.026605 0.709812 0.460914 0.031 Uiso 1 1 calc R . . . .
C36 C 0.1358(3) 0.6225(3) 0.6549(5) 0.0368(11) Uani 1 1 d . . . . .
C37 C 0.5699(4) 0.0885(3) -0.3179(5) 0.0455(13) Uani 1 1 d . . . . .
H37 H 0.544302 0.139243 -0.337086 0.055 Uiso 1 1 calc R . . . .
C38 C 0.6442(4) -0.0597(3) -0.2756(6) 0.0481(13) Uani 1 1 d . . . . .
H38 H 0.668921 -0.110887 -0.260116 0.058 Uiso 1 1 calc R . . . .
C39 C 0.1727(5) 0.6942(4) 0.7120(7) 0.0610(15) Uani 1 1 d . U . . .
H39 H 0.176925 0.739174 0.661053 0.073 Uiso 1 1 calc R . . . .
C41 C 0.1518(6) 0.5672(5) 0.8760(7) 0.0761(17) Uani 1 1 d . U . . .
H41 H 0.139718 0.525701 0.929071 0.091 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O10 2.424(3) . ?
Pr1 O7 2.411(3) . ?
Pr1 O3 2.521(3) . ?
Pr1 O4 2.584(3) . ?
Pr1 O1 2.403(3) . ?
Pr1 O5 2.368(3) . ?
Pr1 O6 2.619(3) . ?
Pr1 O2 2.482(3) . ?
O10 C11 1.254(5) . ?
O7 C18 1.255(5) . ?
O3 C12 1.251(5) . ?
O4 C12 1.279(5) . ?
O1 C18 1.253(5) 4_565 ?
O5 C11 1.257(5) 4_566 ?
C10 C11 1.516(6) . ?
C10 C13 1.392(6) . ?
C10 C19 1.392(6) . ?
C12 C20 1.508(5) . ?
C13 C26 1.389(6) . ?
C14 C16 1.402(5) . ?
C14 C20 1.395(5) 2_545 ?
C15 C20 1.386(6) . ?
C15 C21 1.400(5) . ?
C16 C18 1.504(5) . ?
C16 C35 1.405(6) 2_545 ?
C17 C26 1.399(6) . ?
C17 C27 1.389(6) . ?
C19 C27 1.396(6) . ?
C21 C35 1.396(5) . ?
C21 C36 1.487(6) . ?
O8 C25 1.295(7) . ?
O9 C25 1.235(8) . ?
C25 C26 1.497(7) . ?
C27 C28 1.491(6) . ?
C28 C30 1.393(6) . ?
C28 C37 1.386(7) . ?
C29 C36 1.410(8) . ?
C29 C41 1.348(9) . ?
C30 C38 1.393(7) . ?
N2 C32 1.336(10) . ?
N2 C41 1.255(10) . ?
C32 C39 1.496(10) . ?
N1 C34 1.338(7) . ?
N1 C38 1.321(7) . ?
C34 C37 1.386(7) . ?
C36 C39 1.387(8) . ?

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
O10 Pr1 O3 135.50(12) . . ?
O10 Pr1 O4 130.22(11) . . ?
O10 Pr1 O6 71.37(12) . . ?
O10 Pr1 O2 68.39(12) . . ?
O7 Pr1 O10 142.40(12) . . ?
O7 Pr1 O3 81.25(11) . . ?
O7 Pr1 O4 75.07(10) . . ?
O7 Pr1 O6 73.70(11) . . ?
O7 Pr1 O2 146.62(11) . . ?
O3 Pr1 O4 51.23(9) . . ?
O3 Pr1 O6 138.90(11) . . ?
O4 Pr1 O6 143.50(10) . . ?
O1 Pr1 O10 91.11(12) . . ?
O1 Pr1 O7 92.21(13) . . ?
O1 Pr1 O3 75.26(10) . . ?
O1 Pr1 O4 126.03(10) . . ?
O1 Pr1 O6 73.75(11) . . ?
O1 Pr1 O2 101.24(13) . . ?
O5 Pr1 O10 79.22(11) . . ?
O5 Pr1 O7 82.75(11) . . ?
O5 Pr1 O3 126.60(10) . . ?
O5 Pr1 O4 75.45(10) . . ?
O5 Pr1 O1 155.96(10) . . ?
O5 Pr1 O6 82.29(11) . . ?
O5 Pr1 O2 95.61(12) . . ?
O2 Pr1 O3 73.05(12) . . ?
O2 Pr1 O4 72.29(11) . . ?
O2 Pr1 O6 139.35(12) . . ?
C11 O10 Pr1 149.1(3) . . ?
C18 O7 Pr1 146.7(3) . . ?
C12 O3 Pr1 95.4(2) . . ?
C12 O4 Pr1 91.8(2) . . ?
C18 O1 Pr1 155.6(3) 4_565 . ?
C11 O5 Pr1 150.4(3) 4_566 . ?
C13 C10 C11 121.3(4) . . ?
C13 C10 C19 119.4(4) . . ?
C19 C10 C11 119.3(4) . . ?
O10 C11 O5 124.3(4) . 4_565 ?
O10 C11 C10 117.7(4) . . ?
O5 C11 C10 118.0(3) 4_565 . ?
O3 C12 O4 121.5(4) . . ?
O3 C12 C20 119.7(4) . . ?
O4 C12 C20 118.8(4) . . ?
C26 C13 C10 120.2(4) . . ?
C20 C14 C16 119.7(4) 2_545 . ?
C20 C15 C21 121.0(4) . . ?
C14 C16 C18 120.5(4) . . ?
C14 C16 C35 119.6(4) . 2_545 ?
C35 C16 C18 119.8(3) 2_545 . ?
C27 C17 C26 120.4(4) . . ?
O7 C18 C16 117.7(4) . . ?
O1 C18 O7 124.5(4) 4_566 . ?
O1 C18 C16 117.8(4) 4_566 . ?
C10 C19 C27 121.1(4) . . ?
C14 C20 C12 119.8(4) 2 . ?
C15 C20 C12 120.1(3) . . ?
C15 C20 C14 120.2(4) . 2 ?
C15 C21 C36 120.3(4) . . ?
C35 C21 C15 118.8(4) . . ?
C35 C21 C36 120.9(4) . . ?
O8 C25 C26 116.4(5) . . ?
O9 C25 O8 122.5(5) . . ?
O9 C25 C26 121.1(5) . . ?
C13 C26 C17 120.0(4) . . ?
C13 C26 C25 119.1(4) . . ?
C17 C26 C25 120.9(4) . . ?
C17 C27 C19 119.0(4) . . ?
C17 C27 C28 121.3(4) . . ?
C19 C27 C28 119.7(4) . . ?
C30 C28 C27 122.2(4) . . ?
C37 C28 C27 120.8(4) . . ?
C37 C28 C30 116.9(4) . . ?
C41 C29 C36 122.7(7) . . ?
C28 C30 C38 119.3(5) . . ?
C41 N2 C32 123.5(7) . . ?
N2 C32 C39 119.9(6) . . ?
C38 N1 C34 116.6(5) . . ?
N1 C34 C37 123.9(5) . . ?
C21 C35 C16 120.6(4) . 2 ?
C29 C36 C21 119.5(5) . . ?
C39 C36 C21 122.7(5) . . ?
C39 C36 C29 117.8(6) . . ?
C28 C37 C34 119.4(5) . . ?
N1 C38 C30 123.9(5) . . ?
C36 C39 C32 115.1(7) . . ?
N2 C41 C29 120.6(8) . . ?

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
Pr1 O10 C11 O5 40.5(9) . . . 4_565 ?
Pr1 O10 C11 C10 -140.5(5) . . . . ?
Pr1 O7 C18 O1 85.5(7) . . . 4_566 ?
Pr1 O7 C18 C16 -94.9(5) . . . . ?
Pr1 O3 C12 O4 0.9(4) . . . . ?
Pr1 O3 C12 C20 179.7(3) . . . . ?
Pr1 O4 C12 O3 -0.9(4) . . . . ?
Pr1 O4 C12 C20 -179.7(3) . . . . ?
O3 C12 C20 C14 -5.2(6) . . . 2 ?
O3 C12 C20 C15 172.5(4) . . . . ?
O4 C12 C20 C14 173.7(4) . . . 2 ?
O4 C12 C20 C15 -8.7(6) . . . . ?
C10 C13 C26 C17 -1.7(7) . . . . ?
C10 C13 C26 C25 176.3(4) . . . . ?
C10 C19 C27 C17 -0.3(7) . . . . ?
C10 C19 C27 C28 -178.6(4) . . . . ?
C11 C10 C13 C26 178.8(4) . . . . ?
C11 C10 C19 C27 -177.9(4) . . . . ?
C13 C10 C11 O10 -3.7(6) . . . . ?
C13 C10 C11 O5 175.4(4) . . . 4_565 ?
C13 C10 C19 C27 1.1(6) . . . . ?
C14 C16 C18 O7 178.9(4) . . . . ?
C14 C16 C18 O1 -1.5(6) . . . 4_566 ?
C15 C21 C35 C16 2.2(6) . . . 2 ?
C15 C21 C36 C29 -48.5(7) . . . . ?
C15 C21 C36 C39 131.4(5) . . . . ?
C17 C27 C28 C30 39.8(7) . . . . ?
C17 C27 C28 C37 -140.5(5) . . . . ?
C19 C10 C11 O10 175.3(4) . . . . ?
C19 C10 C11 O5 -5.7(6) . . . 4_565 ?
C19 C10 C13 C26 -0.1(6) . . . . ?
C19 C27 C28 C30 -141.9(5) . . . . ?
C19 C27 C28 C37 37.7(7) . . . . ?
C20 C14 C16 C18 -175.4(4) 2_545 . . . ?
C20 C14 C16 C35 0.8(6) 2_545 . . 2_545 ?
C20 C15 C21 C35 0.6(6) . . . . ?
C20 C15 C21 C36 178.5(4) . . . . ?
C21 C15 C20 C12 179.7(4) . . . . ?
C21 C15 C20 C14 -2.7(6) . . . 2 ?
C21 C36 C39 C32 -176.0(5) . . . . ?
O8 C25 C26 C13 172.4(5) . . . . ?
O8 C25 C26 C17 -9.6(8) . . . . ?
O9 C25 C26 C13 -10.2(8) . . . . ?
O9 C25 C26 C17 167.7(6) . . . . ?
C26 C17 C27 C19 -1.5(7) . . . . ?
C26 C17 C27 C28 176.8(4) . . . . ?
C27 C17 C26 C13 2.5(7) . . . . ?
C27 C17 C26 C25 -175.4(5) . . . . ?
C27 C28 C30 C38 178.5(5) . . . . ?
C27 C28 C37 C34 -179.4(5) . . . . ?
C28 C30 C38 N1 1.5(9) . . . . ?
C29 C36 C39 C32 3.9(8) . . . . ?
C30 C28 C37 C34 0.3(8) . . . . ?
N2 C32 C39 C36 -4.8(10) . . . . ?
C32 N2 C41 C29 4.9(13) . . . . ?
N1 C34 C37 C28 0.4(10) . . . . ?
C34 N1 C38 C30 -0.8(9) . . . . ?
C35 C16 C18 O7 2.7(6) 2_545 . . . ?
C35 C16 C18 O1 -177.7(4) 2_545 . . 4_566 ?
C35 C21 C36 C29 129.3(5) . . . . ?
C35 C21 C36 C39 -50.8(7) . . . . ?
C36 C21 C35 C16 -175.7(4) . . . 2 ?
C36 C29 C41 N2 -5.7(12) . . . . ?
C37 C28 C30 C38 -1.1(7) . . . . ?
C38 N1 C34 C37 -0.2(9) . . . . ?
C41 C29 C36 C21 -179.2(6) . . . . ?
C41 C29 C36 C39 0.9(10) . . . . ?
C41 N2 C32 C39 0.4(12) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelxl_CCDC1
_audit_block_doi                 10.5517/cc1j7mm0
_database_code_depnum_ccdc_archive 'CCDC 1407512'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H39 N O29 Sm4, C3 H7 N O, H2 O'
_chemical_formula_sum            'C54 H48 N2 O31 Sm4'
_chemical_formula_weight         1822.34
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.860(2)
_cell_length_b                   14.230(3)
_cell_length_c                   20.180(4)
_cell_angle_alpha                86.18(3)
_cell_angle_beta                 83.88(3)
_cell_angle_gamma                78.24(3)
_cell_volume                     3032.5(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7798
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.911
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.996
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_unetI/netI     0.0923
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31561
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.569
_diffrn_reflns_theta_min         3.049
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1547
	          2theta: 29.8697
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1547
	          2theta: 29.8697
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1547
	          2theta: 29.8697
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.092379
_diffrn_orient_matrix_UB_12      0.018883
_diffrn_orient_matrix_UB_13      -0.006104
_diffrn_orient_matrix_UB_21      -0.001376
_diffrn_orient_matrix_UB_22      -0.069896
_diffrn_orient_matrix_UB_23      -0.016611
_diffrn_orient_matrix_UB_31      -0.010742
_diffrn_orient_matrix_UB_32      0.013679
_diffrn_orient_matrix_UB_33      -0.046743
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11233
_reflns_number_total             13925
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.402
_refine_diff_density_min         -1.972
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         13925
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0466
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0354P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1173
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 O25(H25A,H25B), O26(H26A,H26B), O27(H27A,H27B), O28(H28A,H28B), O31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C14(H14), C15(H15), C16(H16),
 C19(H19), C20(H20), C21(H21), C24(H24), C27(H27), C28(H28), C29(H29), C32(H32),
  C35(H35), C36(H36), C37(H37), C40(H40), C43(H43), C44(H44), C45(H45),
 C48(H48), C49(H49), C52(H52)
2.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.71437(3) 0.55198(2) 0.32684(2) 0.02001(8) Uani 1 1 d . . . . .
Sm2 Sm 1.08815(3) 0.76433(2) 0.30318(2) 0.02146(8) Uani 1 1 d . . . . .
Sm3 Sm 0.72972(3) 0.30843(2) 0.19118(2) 0.01986(8) Uani 1 1 d . . . . .
Sm4 Sm 1.04480(3) 1.01355(2) 0.14848(2) 0.02524(9) Uani 1 1 d . . . . .
O1 O 1.0062(5) 0.8800(3) 0.0953(3) 0.0387(12) Uani 1 1 d . . . . .
O2 O 0.9945(4) 0.8124(4) 0.1979(2) 0.0343(11) Uani 1 1 d . . . . .
O3 O 0.8036(5) 0.4349(4) 0.1310(3) 0.0490(14) Uani 1 1 d . . . . .
O4 O 0.7348(5) 0.5359(5) 0.2108(2) 0.0502(15) Uani 1 1 d . . . . .
O5 O 1.2364(4) 0.9009(3) 0.1534(2) 0.0315(10) Uani 1 1 d . . . . .
O6 O 1.2618(4) 0.7802(4) 0.2304(2) 0.0338(11) Uani 1 1 d . . . . .
O7 O 1.2559(5) 0.7619(4) -0.0800(2) 0.0397(13) Uani 1 1 d . . . . .
O8 O 1.4158(4) 0.6479(4) -0.1049(2) 0.0447(14) Uani 1 1 d . . . . .
O9 O 1.0466(6) 0.0028(5) 0.2631(3) 0.0602(18) Uani 1 1 d . . . . .
O10 O 1.0931(5) -0.0890(3) 0.3531(3) 0.0367(11) Uani 1 1 d . . . . .
O11 O 0.7918(4) 0.3376(3) 0.2952(2) 0.0313(10) Uani 1 1 d . . . . .
O12 O 0.7885(5) 0.4024(3) 0.3917(2) 0.0358(11) Uani 1 1 d . . . . .
O13 O 0.6970(5) 1.1572(3) 0.2255(3) 0.0442(13) Uani 1 1 d . . . . .
O14 O 0.8287(4) 1.0256(3) 0.1899(3) 0.0409(13) Uani 1 1 d . . . . .
O15 O 0.7278(4) 0.7196(3) 0.2943(3) 0.0342(11) Uani 1 1 d . . . . .
O16 O 0.5328(4) 0.6977(3) 0.3067(3) 0.0342(11) Uani 1 1 d . . . . .
O17 O 0.5367(4) 0.3664(4) 0.2514(2) 0.0331(11) Uani 1 1 d . . . . .
O18 O 0.5415(4) 0.4821(3) 0.3203(2) 0.0308(10) Uani 1 1 d . . . . .
O19 O 0.6115(4) 0.5775(4) 0.4424(2) 0.0335(11) Uani 1 1 d . . . . .
O20 O 0.7979(5) 0.6174(4) 0.4227(2) 0.0464(14) Uani 1 1 d . . . . .
O21 O 1.1432(5) 0.1469(4) 0.1525(4) 0.0604(18) Uani 1 1 d . . . . .
O22 O 0.9497(4) 0.2271(3) 0.1762(2) 0.0324(11) Uani 1 1 d . . . . .
O23 O 1.0811(5) 0.6165(3) 0.2675(2) 0.0364(11) Uani 1 1 d . . . . .
O24 O 0.9330(4) 0.5313(3) 0.2980(2) 0.0326(11) Uani 1 1 d . . . . .
O25 O 0.8756(4) 0.8188(4) 0.3449(3) 0.0416(13) Uani 1 1 d . . . . .
H25A H 0.845287 0.792291 0.380206 0.050 Uiso 1 1 d R . . . .
H25B H 0.829377 0.864851 0.324636 0.050 Uiso 1 1 d R . . . .
O26 O 1.0395(5) 0.6654(4) 0.4081(2) 0.0476(14) Uani 1 1 d . . . . .
H26A H 0.975200 0.639231 0.412020 0.057 Uiso 1 1 d R . . . .
H26B H 1.087520 0.658281 0.439490 0.057 Uiso 1 1 d R . . . .
O27 O 1.2779(4) 0.7032(4) 0.3561(2) 0.0390(12) Uani 1 1 d . . . . .
H27A H 1.275239 0.668613 0.391996 0.047 Uiso 1 1 d R . . . .
H27B H 1.347779 0.716183 0.338906 0.047 Uiso 1 1 d R . . . .
O28 O 0.9273(5) 1.0886(4) 0.0572(2) 0.0383(12) Uani 1 1 d . . . . .
H28A H 0.965173 1.094216 0.018507 0.046 Uiso 1 1 d R . . . .
H28B H 0.848133 1.109476 0.063897 0.046 Uiso 1 1 d R . . . .
O29 O 1.1868(5) 1.0184(4) 0.0398(3) 0.0512(14) Uani 1 1 d . . . . .
N2 N 1.3297(7) 1.0766(6) -0.0325(5) 0.070(3) Uani 1 1 d . . . . .
C1 C 0.9884(6) 0.8101(5) 0.1357(3) 0.0280(14) Uani 1 1 d . . . . .
C2 C 0.9525(6) 0.7273(4) 0.1063(3) 0.0261(13) Uani 1 1 d . . . . .
C3 C 0.9831(7) 0.7134(5) 0.0380(3) 0.0391(18) Uani 1 1 d . . . . .
H3 H 1.028358 0.754142 0.012582 0.047 Uiso 1 1 calc R . . . .
C4 C 0.9480(9) 0.6413(6) 0.0082(4) 0.051(2) Uani 1 1 d . . . . .
H4 H 0.966440 0.634757 -0.037506 0.061 Uiso 1 1 calc R . . . .
C5 C 0.8846(7) 0.5776(5) 0.0460(3) 0.0377(17) Uani 1 1 d . . . . .
H5 H 0.861892 0.527599 0.025791 0.045 Uiso 1 1 calc R . . . .
C6 C 0.8553(6) 0.5888(4) 0.1138(3) 0.0240(13) Uani 1 1 d . . . . .
C7 C 0.7946(7) 0.5163(5) 0.1546(3) 0.0334(16) Uani 1 1 d . . . . .
C8 C 0.8883(6) 0.6648(5) 0.1437(3) 0.0261(13) Uani 1 1 d . . . . .
H8 H 0.866913 0.673172 0.189060 0.031 Uiso 1 1 calc R . . . .
C9 C 1.2776(5) 0.8152(5) 0.1714(3) 0.0253(13) Uani 1 1 d . . . . .
C10 C 1.3494(5) 0.7466(5) 0.1204(3) 0.0244(13) Uani 1 1 d . . . . .
C11 C 1.3228(6) 0.7607(5) 0.0544(3) 0.0278(14) Uani 1 1 d . . . . .
H11 H 1.263201 0.813627 0.041527 0.033 Uiso 1 1 calc R . . . .
C12 C 1.3851(6) 0.6959(5) 0.0075(3) 0.0287(14) Uani 1 1 d . . . . .
C13 C 1.3508(6) 0.7032(5) -0.0626(3) 0.0288(14) Uani 1 1 d . . . . .
C14 C 1.4778(6) 0.6209(5) 0.0267(4) 0.0389(18) Uani 1 1 d . . . . .
H14 H 1.522986 0.579716 -0.005213 0.047 Uiso 1 1 calc R . . . .
C15 C 1.5055(7) 0.6052(5) 0.0926(4) 0.0388(17) Uani 1 1 d . . . . .
H15 H 1.567105 0.553475 0.105097 0.047 Uiso 1 1 calc R . . . .
C16 C 1.4388(6) 0.6688(5) 0.1395(3) 0.0317(15) Uani 1 1 d . . . . .
H16 H 1.454760 0.658771 0.184033 0.038 Uiso 1 1 calc R . . . .
C17 C 0.8191(6) 0.3320(4) 0.3551(3) 0.0250(13) Uani 1 1 d . . . . .
C18 C 0.8962(6) 0.2396(4) 0.3814(3) 0.0233(12) Uani 1 1 d . . . . .
C19 C 0.9273(6) 0.2322(5) 0.4473(3) 0.0282(14) Uani 1 1 d . . . . .
H19 H 0.900137 0.284295 0.474309 0.034 Uiso 1 1 calc R . . . .
C20 C 0.9980(7) 0.1481(5) 0.4726(3) 0.0329(15) Uani 1 1 d . . . . .
H20 H 1.017469 0.143738 0.516626 0.039 Uiso 1 1 calc R . . . .
C21 C 1.0396(6) 0.0711(4) 0.4330(3) 0.0294(14) Uani 1 1 d . . . . .
H21 H 1.087241 0.014701 0.450162 0.035 Uiso 1 1 calc R . . . .
C22 C 1.0105(6) 0.0773(4) 0.3672(3) 0.0244(13) Uani 1 1 d . . . . .
C23 C 1.0541(6) -0.0095(5) 0.3251(3) 0.0304(15) Uani 1 1 d . . . . .
C24 C 0.9389(6) 0.1612(5) 0.3411(3) 0.0262(13) Uani 1 1 d . . . . .
H24 H 0.919616 0.165133 0.297024 0.031 Uiso 1 1 calc R . . . .
C25 C 0.7254(7) 1.0670(5) 0.2167(3) 0.0282(14) Uani 1 1 d . . . . .
C26 C 0.6257(6) 1.0108(5) 0.2398(3) 0.0271(13) Uani 1 1 d . . . . .
C27 C 0.4997(7) 1.0566(5) 0.2538(4) 0.046(2) Uani 1 1 d . . . . .
H27 H 0.476471 1.122973 0.247713 0.055 Uiso 1 1 calc R . . . .
C28 C 0.4093(7) 1.0028(6) 0.2768(5) 0.055(2) Uani 1 1 d . . . . .
H28 H 0.325216 1.033497 0.284304 0.066 Uiso 1 1 calc R . . . .
C29 C 0.4420(6) 0.9040(5) 0.2888(4) 0.0418(19) Uani 1 1 d . . . . .
H29 H 0.380756 0.868849 0.304715 0.050 Uiso 1 1 calc R . . . .
C30 C 0.5692(6) 0.8581(5) 0.2766(3) 0.0260(13) Uani 1 1 d . . . . .
C31 C 0.6089(6) 0.7531(4) 0.2928(3) 0.0256(13) Uani 1 1 d . . . . .
C32 C 0.6581(6) 0.9116(4) 0.2511(3) 0.0262(13) Uani 1 1 d . . . . .
H32 H 0.741405 0.880472 0.241164 0.031 Uiso 1 1 calc R . . . .
C33 C 0.4996(6) 0.4118(5) 0.3039(3) 0.0240(13) Uani 1 1 d . . . . .
C34 C 0.4005(6) 0.3774(5) 0.3522(3) 0.0267(14) Uani 1 1 d . . . . .
C35 C 0.3233(6) 0.3181(5) 0.3331(3) 0.0361(17) Uani 1 1 d . . . . .
H35 H 0.330198 0.300670 0.289044 0.043 Uiso 1 1 calc R . . . .
C36 C 0.2378(8) 0.2858(7) 0.3792(4) 0.059(3) Uani 1 1 d . . . . .
H36 H 0.186346 0.246927 0.366174 0.071 Uiso 1 1 calc R . . . .
C37 C 0.2268(8) 0.3107(7) 0.4458(4) 0.059(3) Uani 1 1 d . . . . .
H37 H 0.167062 0.289643 0.476586 0.071 Uiso 1 1 calc R . . . .
C38 C 0.3054(7) 0.3669(6) 0.4658(3) 0.0345(16) Uani 1 1 d . . . . .
C39 C 0.7015(6) 0.6086(5) 0.4626(3) 0.0287(14) Uani 1 1 d . . . . .
C40 C 0.3904(6) 0.4015(5) 0.4187(3) 0.0248(13) Uani 1 1 d . . . . .
H40 H 0.441071 0.441084 0.431740 0.030 Uiso 1 1 calc R . . . .
C41 C 1.0678(7) 0.2230(5) 0.1691(4) 0.0351(16) Uani 1 1 d . . . . .
C42 C 1.1219(6) 0.3098(5) 0.1764(3) 0.0291(14) Uani 1 1 d . . . . .
C43 C 1.2404(7) 0.3179(6) 0.1437(4) 0.046(2) Uani 1 1 d . . . . .
H43 H 1.286734 0.268028 0.118444 0.055 Uiso 1 1 calc R . . . .
C44 C 1.2886(7) 0.3999(6) 0.1489(4) 0.049(2) Uani 1 1 d . . . . .
H44 H 1.366380 0.405164 0.126407 0.059 Uiso 1 1 calc R . . . .
C45 C 1.2215(6) 0.4738(5) 0.1873(4) 0.0381(18) Uani 1 1 d . . . . .
H45 H 1.253858 0.528950 0.190044 0.046 Uiso 1 1 calc R . . . .
C46 C 1.1049(5) 0.4660(4) 0.2221(3) 0.0217(12) Uani 1 1 d . . . . .
C47 C 1.0333(6) 0.5430(5) 0.2659(3) 0.0254(13) Uani 1 1 d . . . . .
C48 C 1.0554(6) 0.3836(4) 0.2159(3) 0.0257(13) Uani 1 1 d . . . . .
H48 H 0.977720 0.378279 0.238476 0.031 Uiso 1 1 calc R . . . .
C49 C 1.2350(10) 1.0781(8) 0.0093(6) 0.075(3) Uani 1 1 d . . . . .
H49 H 1.192874 1.140205 0.018690 0.090 Uiso 1 1 calc R . . . .
C50 C 1.3883(12) 0.9777(10) -0.0616(6) 0.100(4) Uani 1 1 d . . . . .
H50A H 1.322524 0.943271 -0.066154 0.150 Uiso 1 1 calc GR . . . .
H50B H 1.446316 0.941437 -0.032189 0.150 Uiso 1 1 calc GR . . . .
H50C H 1.432548 0.987012 -0.104576 0.150 Uiso 1 1 calc GR . . . .
C51 C 1.3760(12) 1.1547(10) -0.0677(7) 0.110(5) Uani 1 1 d . . . . .
H51A H 1.324304 1.179157 -0.103218 0.166 Uiso 1 1 calc GR . . . .
H51B H 1.461552 1.132691 -0.086001 0.166 Uiso 1 1 calc GR . . . .
H51C H 1.373183 1.204804 -0.037671 0.166 Uiso 1 1 calc GR . . . .
O30 O 0.7548(8) -0.0630(7) 0.4385(4) 0.094(3) Uani 1 1 d . . . . .
N1 N 0.6373(8) 0.0838(7) 0.4572(5) 0.078(3) Uani 1 1 d . . . . .
C52 C 0.7090(10) 0.0132(9) 0.4179(7) 0.081(4) Uani 1 1 d . . . . .
H52 H 0.721547 0.027208 0.372339 0.098 Uiso 1 1 calc R . . . .
C53 C 0.5800(13) 0.1739(9) 0.4219(8) 0.119(5) Uani 1 1 d . . . . .
H53A H 0.608563 0.171178 0.375278 0.179 Uiso 1 1 calc GR . . . .
H53B H 0.604538 0.227307 0.439986 0.179 Uiso 1 1 calc GR . . . .
H53C H 0.489637 0.181736 0.427623 0.179 Uiso 1 1 calc GR . . . .
C54 C 0.6232(13) 0.0716(13) 0.5275(7) 0.130(6) Uani 1 1 d . . . . .
H54A H 0.667588 0.008851 0.540802 0.196 Uiso 1 1 calc GR . . . .
H54B H 0.535123 0.078111 0.542731 0.196 Uiso 1 1 calc GR . . . .
H54C H 0.657116 0.119522 0.546848 0.196 Uiso 1 1 calc GR . . . .
O31 O 0.3509(5) 0.6371(4) 0.4775(3) 0.0542(16) Uani 1 1 d . . . . .
H31A H 0.306635 0.693610 0.475506 0.065 Uiso 1 1 d R . . . .
H31B H 0.329675 0.595830 0.506586 0.065 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
Sm1 O4 2.351(5) . ?
Sm1 O12 2.458(4) . ?
Sm1 O15 2.460(5) . ?
Sm1 O16 2.597(5) . ?
Sm1 O18 2.316(4) . ?
Sm1 O19 2.493(4) . ?
Sm1 O20 2.528(5) . ?
Sm1 O24 2.347(4) . ?
Sm2 O2 2.448(5) . ?
Sm2 O6 2.303(4) . ?
Sm2 O10 2.390(5) 1_565 ?
Sm2 O23 2.286(4) . ?
Sm2 O25 2.363(4) . ?
Sm2 O26 2.533(5) . ?
Sm2 O27 2.399(4) . ?
Sm3 O3 2.334(5) . ?
Sm3 O7 2.494(5) 2_765 ?
Sm3 O8 2.441(5) 2_765 ?
Sm3 O11 2.359(4) . ?
Sm3 O13 2.302(5) 1_545 ?
Sm3 O17 2.332(4) . ?
Sm3 O22 2.430(5) . ?
Sm3 C13 2.851(6) 2_765 ?
Sm4 O1 2.374(5) . ?
Sm4 O5 2.361(4) . ?
Sm4 O9 2.310(5) 1_565 ?
Sm4 O14 2.382(5) . ?
Sm4 O21 2.370(5) 1_565 ?
Sm4 O28 2.417(5) . ?
Sm4 O29 2.549(5) . ?
O1 C1 1.276(8) . ?
O2 C1 1.268(8) . ?
O3 C7 1.262(8) . ?
O4 C7 1.264(8) . ?
O5 C9 1.254(8) . ?
O6 C9 1.268(7) . ?
O7 C13 1.253(7) . ?
O8 C13 1.258(8) . ?
O9 C23 1.260(8) . ?
O10 C23 1.245(8) . ?
O11 C17 1.268(7) . ?
O12 C17 1.253(7) . ?
O13 C25 1.277(8) . ?
O14 C25 1.241(8) . ?
O15 C31 1.285(7) . ?
O16 C31 1.253(7) . ?
O17 C33 1.264(7) . ?
O18 C33 1.256(7) . ?
O19 C39 1.267(8) . ?
O20 C39 1.272(8) . ?
O21 C41 1.258(8) . ?
O22 C41 1.265(8) . ?
O23 C47 1.263(7) . ?
O24 C47 1.241(7) . ?
O25 H25A 0.8502 . ?
O25 H25B 0.8500 . ?
O26 H26A 0.8499 . ?
O26 H26B 0.8502 . ?
O27 H27A 0.8500 . ?
O27 H27B 0.8500 . ?
O28 H28A 0.8500 . ?
O28 H28B 0.8500 . ?
O29 C49 1.190(11) . ?
N2 C49 1.256(12) . ?
N2 C50 1.549(14) . ?
N2 C51 1.429(13) . ?
C1 C2 1.491(8) . ?
C2 C3 1.399(9) . ?
C2 C8 1.378(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.359(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.389(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.383(9) . ?
C6 C7 1.492(9) . ?
C6 C8 1.397(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.507(8) . ?
C10 C11 1.385(9) . ?
C10 C16 1.379(9) . ?
C11 H11 0.9300 . ?
C11 C12 1.390(8) . ?
C12 C13 1.491(9) . ?
C12 C14 1.376(9) . ?
C14 H14 0.9300 . ?
C14 C15 1.387(10) . ?
C15 H15 0.9300 . ?
C15 C16 1.393(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.505(8) . ?
C18 C19 1.398(8) . ?
C18 C24 1.397(8) . ?
C19 H19 0.9300 . ?
C19 C20 1.382(9) . ?
C20 H20 0.9300 . ?
C20 C21 1.372(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.389(9) . ?
C22 C23 1.514(8) . ?
C22 C24 1.391(9) . ?
C24 H24 0.9300 . ?
C25 C26 1.492(9) . ?
C26 C27 1.398(9) . ?
C26 C32 1.394(8) . ?
C27 H27 0.9300 . ?
C27 C28 1.388(10) . ?
C28 H28 0.9300 . ?
C28 C29 1.390(10) . ?
C29 H29 0.9300 . ?
C29 C30 1.406(9) . ?
C30 C31 1.492(8) . ?
C30 C32 1.385(8) . ?
C32 H32 0.9300 . ?
C33 C34 1.509(9) . ?
C34 C35 1.402(9) . ?
C34 C40 1.395(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.369(10) . ?
C36 H36 0.9300 . ?
C36 C37 1.399(10) . ?
C37 H37 0.9300 . ?
C37 C38 1.388(10) . ?
C38 C39 1.499(9) 2_666 ?
C38 C40 1.390(9) . ?
C40 H40 0.9300 . ?
C41 C42 1.492(9) . ?
C42 C43 1.405(9) . ?
C42 C48 1.394(8) . ?
C43 H43 0.9300 . ?
C43 C44 1.386(11) . ?
C44 H44 0.9300 . ?
C44 C45 1.384(9) . ?
C45 H45 0.9300 . ?
C45 C46 1.402(8) . ?
C46 C47 1.492(8) . ?
C46 C48 1.402(8) . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
O30 C52 1.167(12) . ?
N1 C52 1.377(14) . ?
N1 C53 1.478(15) . ?
N1 C54 1.415(16) . ?
C52 H52 0.9300 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
O31 H31A 0.8499 . ?
O31 H31B 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
O4 Sm1 O12 114.45(19) . . ?
O4 Sm1 O15 82.9(2) . . ?
O4 Sm1 O16 86.29(19) . . ?
O4 Sm1 O19 159.35(17) . . ?
O4 Sm1 O20 145.53(17) . . ?
O12 Sm1 O15 149.74(16) . . ?
O12 Sm1 O16 147.90(16) . . ?
O12 Sm1 O19 74.18(16) . . ?
O12 Sm1 O20 79.43(18) . . ?
O15 Sm1 O16 51.18(14) . . ?
O15 Sm1 O19 98.37(17) . . ?
O15 Sm1 O20 73.35(18) . . ?
O18 Sm1 O4 81.72(17) . . ?
O18 Sm1 O12 82.49(17) . . ?
O18 Sm1 O15 126.02(16) . . ?
O18 Sm1 O16 76.39(15) . . ?
O18 Sm1 O19 80.95(15) . . ?
O18 Sm1 O20 132.55(15) . . ?
O18 Sm1 O24 142.86(16) . . ?
O19 Sm1 O16 78.80(16) . . ?
O19 Sm1 O20 51.99(14) . . ?
O20 Sm1 O16 97.36(18) . . ?
O24 Sm1 O4 76.55(17) . . ?
O24 Sm1 O12 79.66(17) . . ?
O24 Sm1 O15 80.86(16) . . ?
O24 Sm1 O16 130.84(16) . . ?
O24 Sm1 O19 124.07(16) . . ?
O24 Sm1 O20 75.29(16) . . ?
O2 Sm2 O26 136.79(16) . . ?
O6 Sm2 O2 77.66(16) . . ?
O6 Sm2 O10 91.02(17) . 1_565 ?
O6 Sm2 O25 150.95(19) . . ?
O6 Sm2 O26 137.66(18) . . ?
O6 Sm2 O27 70.15(16) . . ?
O10 Sm2 O2 105.49(17) 1_565 . ?
O10 Sm2 O26 98.73(17) 1_565 . ?
O10 Sm2 O27 84.44(18) 1_565 . ?
O23 Sm2 O2 80.17(17) . . ?
O23 Sm2 O6 93.39(18) . . ?
O23 Sm2 O10 173.49(18) . 1_565 ?
O23 Sm2 O25 101.38(17) . . ?
O23 Sm2 O26 74.80(18) . . ?
O23 Sm2 O27 92.54(18) . . ?
O25 Sm2 O2 80.38(17) . . ?
O25 Sm2 O10 76.75(17) . 1_565 ?
O25 Sm2 O26 70.96(19) . . ?
O25 Sm2 O27 133.04(18) . . ?
O27 Sm2 O2 146.52(16) . . ?
O27 Sm2 O26 69.97(16) . . ?
O3 Sm3 O7 84.64(19) . 2_765 ?
O3 Sm3 O8 77.0(2) . 2_765 ?
O3 Sm3 O11 96.60(18) . . ?
O3 Sm3 O22 83.81(19) . . ?
O3 Sm3 C13 77.9(2) . 2_765 ?
O7 Sm3 C13 26.03(16) 2_765 2_765 ?
O8 Sm3 O7 51.94(15) 2_765 2_765 ?
O8 Sm3 C13 26.05(16) 2_765 2_765 ?
O11 Sm3 O7 158.45(15) . 2_765 ?
O11 Sm3 O8 149.30(16) . 2_765 ?
O11 Sm3 O22 81.15(15) . . ?
O11 Sm3 C13 173.33(18) . 2_765 ?
O13 Sm3 O3 162.4(2) 1_545 . ?
O13 Sm3 O7 80.81(19) 1_545 2_765 ?
O13 Sm3 O8 101.4(2) 1_545 2_765 ?
O13 Sm3 O11 93.34(19) 1_545 . ?
O13 Sm3 O17 86.44(18) 1_545 . ?
O13 Sm3 O22 83.37(17) 1_545 . ?
O13 Sm3 C13 93.0(2) 1_545 2_765 ?
O17 Sm3 O3 109.9(2) . . ?
O17 Sm3 O7 122.31(16) . 2_765 ?
O17 Sm3 O8 76.61(16) . 2_765 ?
O17 Sm3 O11 77.59(15) . . ?
O17 Sm3 O22 155.80(16) . . ?
O17 Sm3 C13 100.60(17) . 2_765 ?
O22 Sm3 O7 77.59(15) . 2_765 ?
O22 Sm3 O8 126.93(15) . 2_765 ?
O22 Sm3 C13 101.80(17) . 2_765 ?
O1 Sm4 O14 82.19(18) . . ?
O1 Sm4 O28 77.23(17) . . ?
O1 Sm4 O29 78.87(19) . . ?
O5 Sm4 O1 77.01(17) . . ?
O5 Sm4 O14 137.77(17) . . ?
O5 Sm4 O21 93.31(17) . 1_565 ?
O5 Sm4 O28 133.08(16) . . ?
O5 Sm4 O29 68.86(17) . . ?
O9 Sm4 O1 118.1(2) 1_565 . ?
O9 Sm4 O5 82.53(18) 1_565 . ?
O9 Sm4 O14 75.5(2) 1_565 . ?
O9 Sm4 O21 85.3(3) 1_565 1_565 ?
O9 Sm4 O28 144.39(18) 1_565 . ?
O9 Sm4 O29 142.9(2) 1_565 . ?
O14 Sm4 O28 75.24(18) . . ?
O14 Sm4 O29 141.56(19) . . ?
O21 Sm4 O1 152.5(2) 1_565 . ?
O21 Sm4 O14 119.78(18) 1_565 . ?
O21 Sm4 O28 91.9(2) 1_565 . ?
O21 Sm4 O29 73.7(2) 1_565 . ?
O28 Sm4 O29 68.13(18) . . ?
C1 O1 Sm4 113.5(4) . . ?
C1 O2 Sm2 154.8(4) . . ?
C7 O3 Sm3 122.9(5) . . ?
C7 O4 Sm1 155.0(5) . . ?
C9 O5 Sm4 140.9(4) . . ?
C9 O6 Sm2 134.6(4) . . ?
C13 O7 Sm3 93.1(4) . 2_765 ?
C13 O8 Sm3 95.5(4) . 2_765 ?
C23 O9 Sm4 175.3(5) . 1_545 ?
C23 O10 Sm2 121.4(4) . 1_545 ?
C17 O11 Sm3 165.2(4) . . ?
C17 O12 Sm1 111.4(4) . . ?
C25 O13 Sm3 147.6(5) . 1_565 ?
C25 O14 Sm4 154.4(5) . . ?
C31 O15 Sm1 97.7(4) . . ?
C31 O16 Sm1 92.0(4) . . ?
C33 O17 Sm3 136.6(4) . . ?
C33 O18 Sm1 148.1(4) . . ?
C39 O19 Sm1 94.8(4) . . ?
C39 O20 Sm1 93.0(4) . . ?
C41 O21 Sm4 113.8(5) . 1_545 ?
C41 O22 Sm3 154.7(5) . . ?
C47 O23 Sm2 154.1(4) . . ?
C47 O24 Sm1 158.1(5) . . ?
Sm2 O25 H25A 120.0 . . ?
Sm2 O25 H25B 120.0 . . ?
H25A O25 H25B 120.0 . . ?
Sm2 O26 H26A 120.0 . . ?
Sm2 O26 H26B 120.0 . . ?
H26A O26 H26B 120.0 . . ?
Sm2 O27 H27A 120.0 . . ?
Sm2 O27 H27B 120.0 . . ?
H27A O27 H27B 120.0 . . ?
Sm4 O28 H28A 120.0 . . ?
Sm4 O28 H28B 120.0 . . ?
H28A O28 H28B 120.0 . . ?
C49 O29 Sm4 134.8(7) . . ?
C49 N2 C50 115.6(9) . . ?
C49 N2 C51 129.5(10) . . ?
C51 N2 C50 113.5(9) . . ?
O1 C1 C2 116.2(6) . . ?
O2 C1 O1 122.2(6) . . ?
O2 C1 C2 121.5(6) . . ?
C3 C2 C1 119.0(6) . . ?
C8 C2 C1 122.3(6) . . ?
C8 C2 C3 118.7(6) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 C2 121.3(6) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.1(7) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.7(6) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 C7 119.2(6) . . ?
C5 C6 C8 119.8(6) . . ?
C8 C6 C7 120.9(6) . . ?
O3 C7 O4 120.9(7) . . ?
O3 C7 C6 118.0(6) . . ?
O4 C7 C6 121.0(7) . . ?
C2 C8 C6 120.3(6) . . ?
C2 C8 H8 119.8 . . ?
C6 C8 H8 119.8 . . ?
O5 C9 O6 124.5(6) . . ?
O5 C9 C10 119.3(6) . . ?
O6 C9 C10 116.2(6) . . ?
C11 C10 C9 119.6(6) . . ?
C16 C10 C9 120.3(6) . . ?
C16 C10 C11 120.1(6) . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.1(6) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C13 121.8(6) . . ?
C14 C12 C11 119.1(6) . . ?
C14 C12 C13 119.1(6) . . ?
O7 C13 Sm3 60.8(3) . 2_765 ?
O7 C13 O8 118.8(6) . . ?
O7 C13 C12 121.3(6) . . ?
O8 C13 Sm3 58.5(3) . 2_765 ?
O8 C13 C12 119.8(6) . . ?
C12 C13 Sm3 171.3(5) . 2_765 ?
C12 C14 H14 119.2 . . ?
C12 C14 C15 121.6(7) . . ?
C15 C14 H14 119.2 . . ?
C14 C15 H15 120.8 . . ?
C14 C15 C16 118.5(6) . . ?
C16 C15 H15 120.8 . . ?
C10 C16 C15 120.5(6) . . ?
C10 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
O11 C17 C18 118.7(6) . . ?
O12 C17 O11 121.8(6) . . ?
O12 C17 C18 119.4(6) . . ?
C19 C18 C17 119.5(6) . . ?
C24 C18 C17 121.3(6) . . ?
C24 C18 C19 119.1(6) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.6(6) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.2(6) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 119.9 . . ?
C20 C21 C22 120.1(6) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 C23 119.2(6) . . ?
C21 C22 C24 120.5(6) . . ?
C24 C22 C23 120.4(6) . . ?
O9 C23 C22 117.6(6) . . ?
O10 C23 O9 123.6(6) . . ?
O10 C23 C22 118.8(6) . . ?
C18 C24 H24 120.2 . . ?
C22 C24 C18 119.5(6) . . ?
C22 C24 H24 120.2 . . ?
O13 C25 C26 116.4(6) . . ?
O14 C25 O13 123.9(6) . . ?
O14 C25 C26 119.8(6) . . ?
C27 C26 C25 121.1(6) . . ?
C32 C26 C25 120.1(6) . . ?
C32 C26 C27 118.7(6) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 C26 119.9(7) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 119.3 . . ?
C27 C28 C29 121.3(7) . . ?
C29 C28 H28 119.3 . . ?
C28 C29 H29 120.5 . . ?
C28 C29 C30 119.0(7) . . ?
C30 C29 H29 120.5 . . ?
C29 C30 C31 120.4(6) . . ?
C32 C30 C29 119.4(6) . . ?
C32 C30 C31 120.2(6) . . ?
O15 C31 C30 117.3(5) . . ?
O16 C31 O15 119.1(6) . . ?
O16 C31 C30 123.6(6) . . ?
C26 C32 H32 119.2 . . ?
C30 C32 C26 121.6(6) . . ?
C30 C32 H32 119.2 . . ?
O17 C33 C34 118.0(5) . . ?
O18 C33 O17 125.1(6) . . ?
O18 C33 C34 116.9(5) . . ?
C35 C34 C33 122.1(6) . . ?
C40 C34 C33 118.6(5) . . ?
C40 C34 C35 119.2(6) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 C34 120.0(6) . . ?
C36 C35 H35 120.0 . . ?
C35 C36 H36 119.6 . . ?
C35 C36 C37 120.8(7) . . ?
C37 C36 H36 119.6 . . ?
C36 C37 H37 120.1 . . ?
C38 C37 C36 119.7(7) . . ?
C38 C37 H37 120.1 . . ?
C37 C38 C39 120.6(6) . 2_666 ?
C37 C38 C40 119.6(6) . . ?
C40 C38 C39 119.8(6) . 2_666 ?
O19 C39 O20 120.2(6) . . ?
O19 C39 C38 119.4(6) . 2_666 ?
O20 C39 C38 120.4(6) . 2_666 ?
C34 C40 H40 119.7 . . ?
C38 C40 C34 120.6(6) . . ?
C38 C40 H40 119.7 . . ?
O21 C41 O22 121.1(6) . . ?
O21 C41 C42 117.7(6) . . ?
O22 C41 C42 121.1(6) . . ?
C43 C42 C41 120.5(6) . . ?
C48 C42 C41 120.3(6) . . ?
C48 C42 C43 119.1(6) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 C42 120.4(6) . . ?
C44 C43 H43 119.8 . . ?
C43 C44 H44 119.8 . . ?
C45 C44 C43 120.3(7) . . ?
C45 C44 H44 119.8 . . ?
C44 C45 H45 119.9 . . ?
C44 C45 C46 120.3(6) . . ?
C46 C45 H45 119.9 . . ?
C45 C46 C47 121.3(5) . . ?
C45 C46 C48 119.3(5) . . ?
C48 C46 C47 119.5(5) . . ?
O23 C47 C46 116.2(6) . . ?
O24 C47 O23 124.7(6) . . ?
O24 C47 C46 119.1(5) . . ?
C42 C48 C46 120.5(6) . . ?
C42 C48 H48 119.7 . . ?
C46 C48 H48 119.7 . . ?
O29 C49 N2 134.8(11) . . ?
O29 C49 H49 112.6 . . ?
N2 C49 H49 112.6 . . ?
N2 C50 H50A 109.5 . . ?
N2 C50 H50B 109.5 . . ?
N2 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N2 C51 H51A 109.5 . . ?
N2 C51 H51B 109.5 . . ?
N2 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C52 N1 C53 116.4(11) . . ?
C52 N1 C54 121.6(12) . . ?
C54 N1 C53 122.0(12) . . ?
O30 C52 N1 123.9(13) . . ?
O30 C52 H52 118.0 . . ?
N1 C52 H52 118.0 . . ?
N1 C53 H53A 109.5 . . ?
N1 C53 H53B 109.5 . . ?
N1 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N1 C54 H54A 109.5 . . ?
N1 C54 H54B 109.5 . . ?
N1 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
H31A O31 H31B 120.0 . . ?

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
Sm1 O4 C7 O3 96.1(12) . . . . ?
Sm1 O4 C7 C6 -84.7(14) . . . . ?
Sm1 O12 C17 O11 -11.8(8) . . . . ?
Sm1 O12 C17 C18 164.9(4) . . . . ?
Sm1 O15 C31 O16 0.1(7) . . . . ?
Sm1 O15 C31 C30 178.1(5) . . . . ?
Sm1 O16 C31 O15 -0.1(6) . . . . ?
Sm1 O16 C31 C30 -178.0(6) . . . . ?
Sm1 O18 C33 O17 -40.9(12) . . . . ?
Sm1 O18 C33 C34 137.0(6) . . . . ?
Sm1 O19 C39 O20 1.6(7) . . . . ?
Sm1 O19 C39 C38 -177.1(6) . . . 2_666 ?
Sm1 O20 C39 O19 -1.5(7) . . . . ?
Sm1 O20 C39 C38 177.2(6) . . . 2_666 ?
Sm1 O24 C47 O23 74.0(13) . . . . ?
Sm1 O24 C47 C46 -106.1(11) . . . . ?
Sm2 O2 C1 O1 -110.6(10) . . . . ?
Sm2 O2 C1 C2 72.9(12) . . . . ?
Sm2 O6 C9 O5 59.3(9) . . . . ?
Sm2 O6 C9 C10 -119.7(6) . . . . ?
Sm2 O10 C23 O9 -22.7(9) 1_545 . . . ?
Sm2 O10 C23 C22 155.9(4) 1_545 . . . ?
Sm2 O23 C47 O24 1.5(15) . . . . ?
Sm2 O23 C47 C46 -178.4(8) . . . . ?
Sm3 O3 C7 O4 -6.0(9) . . . . ?
Sm3 O3 C7 C6 174.7(4) . . . . ?
Sm3 O7 C13 O8 7.7(7) 2_765 . . . ?
Sm3 O7 C13 C12 -170.2(6) 2_765 . . . ?
Sm3 O8 C13 O7 -7.9(7) 2_765 . . . ?
Sm3 O8 C13 C12 170.1(6) 2_765 . . . ?
Sm3 O11 C17 O12 -139.1(14) . . . . ?
Sm3 O11 C17 C18 44.2(19) . . . . ?
Sm3 O13 C25 O14 26.1(14) 1_565 . . . ?
Sm3 O13 C25 C26 -153.2(7) 1_565 . . . ?
Sm3 O17 C33 O18 42.3(10) . . . . ?
Sm3 O17 C33 C34 -135.6(5) . . . . ?
Sm3 O22 C41 O21 -168.9(7) . . . . ?
Sm3 O22 C41 C42 7.8(16) . . . . ?
Sm4 O1 C1 O2 -1.8(8) . . . . ?
Sm4 O1 C1 C2 174.8(4) . . . . ?
Sm4 O5 C9 O6 -59.9(10) . . . . ?
Sm4 O5 C9 C10 119.1(6) . . . . ?
Sm4 O14 C25 O13 13.9(16) . . . . ?
Sm4 O14 C25 C26 -166.9(8) . . . . ?
Sm4 O21 C41 O22 -6.3(10) 1_545 . . . ?
Sm4 O21 C41 C42 176.9(5) 1_545 . . . ?
Sm4 O29 C49 N2 156.0(11) . . . . ?
O1 C1 C2 C3 22.5(9) . . . . ?
O1 C1 C2 C8 -156.4(6) . . . . ?
O2 C1 C2 C3 -160.9(7) . . . . ?
O2 C1 C2 C8 20.2(10) . . . . ?
O5 C9 C10 C11 -29.4(9) . . . . ?
O5 C9 C10 C16 152.3(6) . . . . ?
O6 C9 C10 C11 149.7(6) . . . . ?
O6 C9 C10 C16 -28.7(9) . . . . ?
O11 C17 C18 C19 179.9(6) . . . . ?
O11 C17 C18 C24 0.7(9) . . . . ?
O12 C17 C18 C19 3.1(9) . . . . ?
O12 C17 C18 C24 -176.1(6) . . . . ?
O13 C25 C26 C27 16.2(10) . . . . ?
O13 C25 C26 C32 -160.6(6) . . . . ?
O14 C25 C26 C27 -163.1(7) . . . . ?
O14 C25 C26 C32 20.1(10) . . . . ?
O17 C33 C34 C35 -19.1(10) . . . . ?
O17 C33 C34 C40 157.4(6) . . . . ?
O18 C33 C34 C35 162.9(7) . . . . ?
O18 C33 C34 C40 -20.6(9) . . . . ?
O21 C41 C42 C43 22.7(11) . . . . ?
O21 C41 C42 C48 -157.1(7) . . . . ?
O22 C41 C42 C43 -154.1(7) . . . . ?
O22 C41 C42 C48 26.1(11) . . . . ?
C1 C2 C3 C4 -177.3(7) . . . . ?
C1 C2 C8 C6 179.2(6) . . . . ?
C2 C3 C4 C5 -2.4(13) . . . . ?
C3 C2 C8 C6 0.3(10) . . . . ?
C3 C4 C5 C6 1.2(13) . . . . ?
C4 C5 C6 C7 -176.1(7) . . . . ?
C4 C5 C6 C8 0.8(11) . . . . ?
C5 C6 C7 O3 19.4(10) . . . . ?
C5 C6 C7 O4 -159.9(7) . . . . ?
C5 C6 C8 C2 -1.5(10) . . . . ?
C7 C6 C8 C2 175.3(6) . . . . ?
C8 C2 C3 C4 1.7(12) . . . . ?
C8 C6 C7 O3 -157.4(6) . . . . ?
C8 C6 C7 O4 23.3(10) . . . . ?
C9 C10 C11 C12 -177.6(6) . . . . ?
C9 C10 C16 C15 -180.0(6) . . . . ?
C10 C11 C12 C13 174.2(6) . . . . ?
C10 C11 C12 C14 -3.5(10) . . . . ?
C11 C10 C16 C15 1.6(10) . . . . ?
C11 C12 C13 O7 -7.7(11) . . . . ?
C11 C12 C13 O8 174.4(7) . . . . ?
C11 C12 C14 C15 3.8(11) . . . . ?
C12 C14 C15 C16 -1.4(12) . . . . ?
C13 C12 C14 C15 -173.9(7) . . . . ?
C14 C12 C13 O7 170.0(7) . . . . ?
C14 C12 C13 O8 -7.9(10) . . . . ?
C14 C15 C16 C10 -1.4(11) . . . . ?
C16 C10 C11 C12 0.8(10) . . . . ?
C17 C18 C19 C20 -180.0(6) . . . . ?
C17 C18 C24 C22 179.6(6) . . . . ?
C18 C19 C20 C21 0.6(11) . . . . ?
C19 C18 C24 C22 0.5(9) . . . . ?
C19 C20 C21 C22 -0.1(11) . . . . ?
C20 C21 C22 C23 -178.2(6) . . . . ?
C20 C21 C22 C24 -0.2(10) . . . . ?
C21 C22 C23 O9 -167.6(7) . . . . ?
C21 C22 C23 O10 13.6(9) . . . . ?
C21 C22 C24 C18 0.0(9) . . . . ?
C23 C22 C24 C18 178.0(6) . . . . ?
C24 C18 C19 C20 -0.8(10) . . . . ?
C24 C22 C23 O9 14.4(9) . . . . ?
C24 C22 C23 O10 -164.4(6) . . . . ?
C25 C26 C27 C28 -178.4(7) . . . . ?
C25 C26 C32 C30 175.8(6) . . . . ?
C26 C27 C28 C29 2.5(14) . . . . ?
C27 C26 C32 C30 -1.1(10) . . . . ?
C27 C28 C29 C30 -0.7(14) . . . . ?
C28 C29 C30 C31 176.3(8) . . . . ?
C28 C29 C30 C32 -1.9(12) . . . . ?
C29 C30 C31 O15 -165.3(7) . . . . ?
C29 C30 C31 O16 12.6(10) . . . . ?
C29 C30 C32 C26 2.9(10) . . . . ?
C31 C30 C32 C26 -175.4(6) . . . . ?
C32 C26 C27 C28 -1.6(12) . . . . ?
C32 C30 C31 O15 12.9(9) . . . . ?
C32 C30 C31 O16 -169.1(6) . . . . ?
C33 C34 C35 C36 177.6(8) . . . . ?
C33 C34 C40 C38 -176.3(6) . . . . ?
C34 C35 C36 C37 -0.5(15) . . . . ?
C35 C34 C40 C38 0.3(10) . . . . ?
C35 C36 C37 C38 -1.5(16) . . . . ?
C36 C37 C38 C39 -177.7(9) . . . 2_666 ?
C36 C37 C38 C40 2.9(14) . . . . ?
C37 C38 C40 C34 -2.3(12) . . . . ?
C39 C38 C40 C34 178.3(6) 2_666 . . . ?
C40 C34 C35 C36 1.1(12) . . . . ?
C41 C42 C43 C44 177.9(8) . . . . ?
C41 C42 C48 C46 -178.9(6) . . . . ?
C42 C43 C44 C45 1.2(14) . . . . ?
C43 C42 C48 C46 1.3(10) . . . . ?
C43 C44 C45 C46 0.9(13) . . . . ?
C44 C45 C46 C47 177.5(7) . . . . ?
C44 C45 C46 C48 -1.8(11) . . . . ?
C45 C46 C47 O23 2.9(9) . . . . ?
C45 C46 C47 O24 -177.0(6) . . . . ?
C45 C46 C48 C42 0.7(10) . . . . ?
C47 C46 C48 C42 -178.6(6) . . . . ?
C48 C42 C43 C44 -2.2(12) . . . . ?
C48 C46 C47 O23 -177.8(6) . . . . ?
C48 C46 C47 O24 2.3(9) . . . . ?
C50 N2 C49 O29 12(2) . . . . ?
C51 N2 C49 O29 177.5(13) . . . . ?
C53 N1 C52 O30 -176.2(12) . . . . ?
C54 N1 C52 O30 5.8(19) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_333
_audit_block_doi                 10.5517/cc1j7mhw
_database_code_depnum_ccdc_archive 'CCDC 1407508'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H19 Eu N2 O10'
_chemical_formula_sum            'C26 H19 Eu N2 O10'
_chemical_formula_weight         671.40
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.672(3)
_cell_length_b                   16.543(3)
_cell_length_c                   10.243(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.53(3)
_cell_angle_gamma                90
_cell_volume                     2406.6(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6696
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.672
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1285
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19696
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.045
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1147
	          2theta: 29.9289
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1147
	          2theta: 29.9289
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1147
	          2theta: 29.9289
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.031422
_diffrn_orient_matrix_UB_12      -0.040423
_diffrn_orient_matrix_UB_13      0.086891
_diffrn_orient_matrix_UB_21      -0.053086
_diffrn_orient_matrix_UB_22      -0.028283
_diffrn_orient_matrix_UB_23      0.006040
_diffrn_orient_matrix_UB_31      0.030250
_diffrn_orient_matrix_UB_32      -0.060773
_diffrn_orient_matrix_UB_33      -0.018704
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3806
_reflns_number_total             4235
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.724
_refine_diff_density_min         -2.071
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         4235
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0429
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0503P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1073
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H5A-H5B
 1.39 with sigma of 0.01
 O5-H5B
 0.85 with sigma of 0.01
 O5-H5A
 0.85 with sigma of 0.01
 H5B-Eu1
 2.9 with sigma of 0.01
 H6B-H6A
 1.39 with sigma of 0.01
 H6B-O6
 0.85 with sigma of 0.01
 O6-H6A
 0.85 with sigma of 0.01
 H6B-Eu1
 2.9 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N2 \\sim C12 \\sim C13 \\sim C10 \\sim C11: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
4.a Riding coordinates:
 O6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C20(H20), C16(H16), C18(H18), C5(H5), C25(H25), C24(H24),
 C23(H23), C26(H26), C10(H10), C13(H13), C12(H12), C11(H11)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O9 O 0.2966(2) 0.58972(18) 0.6725(3) 0.0264(8) Uani 1 1 d . . . . .
C1 C 0.3611(3) 0.5466(3) 0.7477(5) 0.0244(11) Uani 1 1 d . . . . .
O3 O 0.8073(2) 0.25772(18) 0.3172(3) 0.0250(7) Uani 1 1 d . . . . .
O8 O 0.5942(3) 0.31501(19) 0.9217(4) 0.0385(10) Uani 1 1 d . . . . .
C4 C 0.3940(3) 0.3893(3) 0.4932(5) 0.0231(10) Uani 1 1 d . . . . .
C2 C 0.3947(3) 0.4731(2) 0.6885(5) 0.0215(10) Uani 1 1 d . . . . .
C3 C 0.3642(3) 0.4581(3) 0.5513(5) 0.0248(11) Uani 1 1 d . . . . .
H3 H 0.323301 0.494383 0.496607 0.030 Uiso 1 1 calc R . . . .
C9 C 0.3634(4) 0.3769(3) 0.3455(6) 0.0337(13) Uani 1 1 d . . . . .
Eu1 Eu 0.70110(2) 0.18630(2) 0.63404(2) 0.01703(12) Uani 1 1 d D . . . .
O7 O 0.5901(2) 0.23837(18) 0.7422(3) 0.0250(7) Uani 1 1 d . . . . .
O4 O 0.8215(3) 0.2269(2) 0.5322(4) 0.0380(9) Uani 1 1 d . . . . .
O5 O 0.6767(3) 0.3344(2) 0.5631(4) 0.0375(9) Uani 1 1 d D . . . .
C15 C 0.9407(4) 0.3075(2) 0.4793(5) 0.0225(11) Uani 1 1 d . . . . .
C8 C 0.5635(3) 0.2973(3) 0.7986(5) 0.0208(10) Uani 1 1 d . . . . .
C6 C 0.4891(3) 0.3520(3) 0.7144(5) 0.0212(10) Uani 1 1 d . . . . .
C14 C 0.8494(3) 0.2608(2) 0.4394(5) 0.0200(10) Uani 1 1 d . . . . .
C7 C 0.4582(3) 0.4198(3) 0.7706(5) 0.0243(11) Uani 1 1 d . . . . .
H7 H 0.479584 0.429752 0.862563 0.029 Uiso 1 1 calc R . . . .
C20 C 0.9693(3) 0.3520(3) 0.3813(5) 0.0241(10) Uani 1 1 d . . . . .
H20 H 0.933148 0.351151 0.292614 0.029 Uiso 1 1 calc R . . . .
C16 C 0.9967(4) 0.3074(3) 0.6107(6) 0.0250(11) Uani 1 1 d . . . . .
H16 H 0.978654 0.277072 0.676447 0.030 Uiso 1 1 calc R . . . .
C18 C 1.1050(4) 0.3979(3) 0.5459(6) 0.0320(12) Uani 1 1 d . . . . .
H18 H 1.159488 0.429060 0.569082 0.038 Uiso 1 1 calc R . . . .
C5 C 0.4553(3) 0.3364(3) 0.5764(5) 0.0230(10) Uani 1 1 d . . . . .
H5 H 0.474237 0.289667 0.540090 0.028 Uiso 1 1 calc R . . . .
C22 C 1.0809(4) 0.4443(3) 0.3070(6) 0.0298(12) Uani 1 1 d . . . . .
N1 N 1.1347(4) 0.5298(3) 0.1030(6) 0.0477(13) Uani 1 1 d . . . . .
C25 C 1.0964(5) 0.4565(4) 0.0808(7) 0.0536(18) Uani 1 1 d . . . . .
H25 H 1.088182 0.433865 -0.004538 0.064 Uiso 1 1 calc R . . . .
C17 C 1.0794(4) 0.3522(3) 0.6445(6) 0.0329(12) Uani 1 1 d . . . . .
C19 C 1.0520(4) 0.3982(3) 0.4152(5) 0.0282(11) Uani 1 1 d . . . . .
C24 C 1.1467(5) 0.5601(3) 0.2249(7) 0.0452(15) Uani 1 1 d . . . . .
H24 H 1.172686 0.611573 0.241186 0.054 Uiso 1 1 calc R . . . .
C23 C 1.1230(4) 0.5199(3) 0.3306(6) 0.0373(13) Uani 1 1 d . . . . .
H23 H 1.135029 0.543164 0.415885 0.045 Uiso 1 1 calc R . . . .
C26 C 1.0682(5) 0.4123(3) 0.1787(7) 0.0442(16) Uani 1 1 d . . . . .
H26 H 1.040990 0.361543 0.158463 0.053 Uiso 1 1 calc R . . . .
O10 O 0.3958(3) 0.56417(19) 0.8689(4) 0.0310(8) Uani 1 1 d . . . . .
O6 O 0.8003(3) 0.0732(2) 0.6114(5) 0.0429(10) Uani 1 1 d D . . . .
H6A H 0.807799 0.066077 0.532504 0.064 Uiso 1 1 d DR . . . .
H6B H 0.789319 0.028537 0.644444 0.064 Uiso 1 1 d DR . . . .
O1 O 1.2111(3) 0.3971(3) 0.8130(5) 0.0636(14) Uani 1 1 d . . . . .
H1 H 1.239499 0.391424 0.892266 0.095 Uiso 1 1 calc GR . . . .
O2 O 1.1268(5) 0.2980(3) 0.8666(6) 0.0770(18) Uani 1 1 d . . . . .
C21 C 1.1408(5) 0.3478(4) 0.7841(7) 0.0504(16) Uani 1 1 d . . . . .
C10 C 0.3722(6) 0.4399(5) 0.2586(7) 0.0612(16) Uani 1 1 d . U . . .
H10 H 0.395739 0.489293 0.295611 0.073 Uiso 1 1 calc R . . . .
N2 N 0.3066(5) 0.3681(4) 0.0668(7) 0.0716(16) Uani 1 1 d . U . . .
C13 C 0.3269(6) 0.3053(4) 0.2877(8) 0.0595(17) Uani 1 1 d . U . . .
H13 H 0.322980 0.259704 0.339131 0.071 Uiso 1 1 calc R . . . .
C12 C 0.2943(6) 0.3047(5) 0.1393(9) 0.0697(19) Uani 1 1 d . U . . .
H12 H 0.264544 0.258887 0.095878 0.084 Uiso 1 1 calc R . . . .
C11 C 0.3476(6) 0.4319(5) 0.1225(9) 0.0743(19) Uani 1 1 d . U . . .
H11 H 0.360836 0.473501 0.069004 0.089 Uiso 1 1 calc R . . . .
H5A H 0.690(5) 0.354(5) 0.493(5) 0.112 Uiso 1 1 d DR . . . .
H5B H 0.6190(18) 0.3441(17) 0.559(8) 0.112 Uiso 1 1 d DR . . . .


_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
O9 C1 1.277(6) . ?
O9 Eu1 2.539(3) 2_656 ?
C1 C2 1.497(6) . ?
C1 Eu1 2.862(5) 2_656 ?
C1 O10 1.252(6) . ?
O3 Eu1 2.310(3) 4_565 ?
O3 C14 1.251(6) . ?
O8 Eu1 2.341(4) 4_566 ?
O8 C8 1.263(7) . ?
C4 C3 1.404(6) . ?
C4 C9 1.480(7) . ?
C4 C5 1.384(7) . ?
C2 C3 1.386(7) . ?
C2 C7 1.400(6) . ?
C9 C10 1.398(9) . ?
C9 C13 1.371(8) . ?
Eu1 O7 2.351(3) . ?
Eu1 O4 2.362(4) . ?
Eu1 O5 2.554(4) . ?
Eu1 O10 2.466(3) 2_646 ?
Eu1 O6 2.418(3) . ?
O7 C8 1.244(6) . ?
O4 C14 1.258(6) . ?
C15 C14 1.511(7) . ?
C15 C20 1.391(7) . ?
C15 C16 1.389(8) . ?
C8 C6 1.512(6) . ?
C6 C7 1.388(6) . ?
C6 C5 1.399(7) . ?
C20 C19 1.402(7) . ?
C16 C17 1.389(7) . ?
C18 C17 1.388(8) . ?
C18 C19 1.369(8) . ?
C22 C19 1.492(7) . ?
C22 C23 1.388(7) . ?
C22 C26 1.386(8) . ?
N1 C25 1.333(7) . ?
N1 C24 1.315(8) . ?
C25 C26 1.385(8) . ?
C17 C21 1.489(9) . ?
C24 C23 1.388(8) . ?
O1 C21 1.289(8) . ?
O2 C21 1.233(9) . ?
C10 C11 1.356(10) . ?
N2 C12 1.323(10) . ?
N2 C11 1.277(10) . ?
C13 C12 1.475(12) . ?

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
C1 O9 Eu1 91.0(3) . 2_656 ?
O9 C1 C2 118.6(4) . . ?
O9 C1 Eu1 62.5(2) . 2_656 ?
C2 C1 Eu1 178.9(4) . 2_656 ?
O10 C1 O9 121.6(4) . . ?
O10 C1 C2 119.8(4) . . ?
O10 C1 Eu1 59.1(2) . 2_656 ?
C14 O3 Eu1 149.3(3) . 4_565 ?
C8 O8 Eu1 156.0(3) . 4_566 ?
C3 C4 C9 119.9(4) . . ?
C5 C4 C3 118.4(4) . . ?
C5 C4 C9 121.7(4) . . ?
C3 C2 C1 120.1(4) . . ?
C3 C2 C7 119.6(4) . . ?
C7 C2 C1 120.3(4) . . ?
C2 C3 C4 121.3(4) . . ?
C10 C9 C4 119.6(5) . . ?
C13 C9 C4 123.2(6) . . ?
C13 C9 C10 117.2(6) . . ?
O9 Eu1 C1 26.49(13) 2_646 2_646 ?
O9 Eu1 O5 143.02(12) 2_646 . ?
O3 Eu1 O9 75.19(11) 4_566 2_646 ?
O3 Eu1 C1 101.63(13) 4_566 2_646 ?
O3 Eu1 O8 156.39(11) 4_566 4_565 ?
O3 Eu1 O7 82.89(12) 4_566 . ?
O3 Eu1 O4 79.52(13) 4_566 . ?
O3 Eu1 O5 82.20(13) 4_566 . ?
O3 Eu1 O10 127.41(12) 4_566 2_646 ?
O3 Eu1 O6 95.09(13) 4_566 . ?
O8 Eu1 O9 126.45(11) 4_565 2_646 ?
O8 Eu1 C1 100.11(13) 4_565 2_646 ?
O8 Eu1 O7 93.42(14) 4_565 . ?
O8 Eu1 O4 89.60(14) 4_565 . ?
O8 Eu1 O5 74.41(12) 4_565 . ?
O8 Eu1 O10 74.42(12) 4_565 2_646 ?
O8 Eu1 O6 100.52(15) 4_565 . ?
O7 Eu1 O9 74.81(11) . 2_646 ?
O7 Eu1 C1 76.37(12) . 2_646 ?
O7 Eu1 O4 141.90(14) . . ?
O7 Eu1 O5 73.65(12) . . ?
O7 Eu1 O10 80.82(12) . 2_646 ?
O7 Eu1 O6 146.51(13) . . ?
O4 Eu1 O9 131.17(12) . 2_646 ?
O4 Eu1 C1 140.27(14) . 2_646 ?
O4 Eu1 O5 70.66(13) . . ?
O4 Eu1 O10 136.04(13) . 2_646 ?
O4 Eu1 O6 69.05(13) . . ?
O5 Eu1 C1 149.06(13) . 2_646 ?
O10 Eu1 O9 52.32(11) 2_646 2_646 ?
O10 Eu1 C1 25.83(13) 2_646 2_646 ?
O10 Eu1 O5 137.98(13) 2_646 . ?
O6 Eu1 O9 72.40(13) . 2_646 ?
O6 Eu1 C1 71.31(14) . 2_646 ?
O6 Eu1 O5 139.42(13) . . ?
O6 Eu1 O10 73.98(14) . 2_646 ?
C8 O7 Eu1 147.2(3) . . ?
C14 O4 Eu1 151.9(4) . . ?
C20 C15 C14 118.8(5) . . ?
C20 C15 C16 119.2(5) . . ?
C16 C15 C14 121.9(4) . . ?
O8 C8 C6 117.1(4) . . ?
O7 C8 O8 124.8(4) . . ?
O7 C8 C6 118.0(4) . . ?
C7 C6 C8 120.8(4) . . ?
C7 C6 C5 119.9(4) . . ?
C5 C6 C8 119.2(4) . . ?
O3 C14 C15 118.3(4) . . ?
O4 C14 O3 124.4(4) . . ?
O4 C14 C15 117.3(4) . . ?
C6 C7 C2 119.8(4) . . ?
C15 C20 C19 120.5(5) . . ?
C17 C16 C15 120.5(5) . . ?
C19 C18 C17 121.5(5) . . ?
C4 C5 C6 121.1(4) . . ?
C23 C22 C19 121.8(5) . . ?
C26 C22 C19 120.9(4) . . ?
C26 C22 C23 117.3(5) . . ?
C24 N1 C25 117.3(5) . . ?
N1 C25 C26 123.1(6) . . ?
C16 C17 C18 119.3(5) . . ?
C16 C17 C21 119.6(5) . . ?
C18 C17 C21 121.1(5) . . ?
C20 C19 C22 119.0(5) . . ?
C18 C19 C20 119.0(5) . . ?
C18 C19 C22 122.0(5) . . ?
N1 C24 C23 123.9(5) . . ?
C22 C23 C24 118.9(5) . . ?
C22 C26 C25 119.4(5) . . ?
C1 O10 Eu1 95.0(3) . 2_656 ?
O1 C21 C17 116.5(6) . . ?
O2 C21 C17 121.7(6) . . ?
O2 C21 O1 121.7(7) . . ?
C11 C10 C9 122.6(7) . . ?
C11 N2 C12 121.3(8) . . ?
C9 C13 C12 116.2(7) . . ?
N2 C12 C13 121.2(7) . . ?
N2 C11 C10 120.9(8) . . ?

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
O9 C1 C2 C3 7.6(7) . . . . ?
O9 C1 C2 C7 -173.5(4) . . . . ?
O9 C1 O10 Eu1 -0.4(5) . . . 2_656 ?
C1 C2 C3 C4 -179.5(4) . . . . ?
C1 C2 C7 C6 -179.7(4) . . . . ?
O8 C8 C6 C7 1.6(7) . . . . ?
O8 C8 C6 C5 177.8(5) . . . . ?
C4 C9 C10 C11 178.3(7) . . . . ?
C4 C9 C13 C12 176.3(6) . . . . ?
C2 C1 O10 Eu1 -179.8(4) . . . 2_656 ?
C3 C4 C9 C10 49.1(8) . . . . ?
C3 C4 C9 C13 -131.5(6) . . . . ?
C3 C4 C5 C6 -1.9(7) . . . . ?
C3 C2 C7 C6 -0.9(7) . . . . ?
C9 C4 C3 C2 -177.4(5) . . . . ?
C9 C4 C5 C6 175.3(5) . . . . ?
C9 C10 C11 N2 6.8(13) . . . . ?
C9 C13 C12 N2 5.0(12) . . . . ?
Eu1 O9 C1 C2 179.8(4) 2_656 . . . ?
Eu1 O9 C1 O10 0.4(5) 2_656 . . . ?
Eu1 O3 C14 O4 93.5(7) 4_565 . . . ?
Eu1 O3 C14 C15 -87.3(7) 4_565 . . . ?
Eu1 O8 C8 O7 20.3(12) 4_566 . . . ?
Eu1 O8 C8 C6 -159.6(6) 4_566 . . . ?
Eu1 O7 C8 O8 -84.8(8) . . . . ?
Eu1 O7 C8 C6 95.1(6) . . . . ?
Eu1 O4 C14 O3 -38.5(10) . . . . ?
Eu1 O4 C14 C15 142.3(6) . . . . ?
O7 C8 C6 C7 -178.4(4) . . . . ?
O7 C8 C6 C5 -2.2(7) . . . . ?
C15 C20 C19 C18 0.9(7) . . . . ?
C15 C20 C19 C22 179.2(4) . . . . ?
C15 C16 C17 C18 0.7(8) . . . . ?
C15 C16 C17 C21 -176.8(5) . . . . ?
C8 C6 C7 C2 175.0(4) . . . . ?
C8 C6 C5 C4 -173.6(4) . . . . ?
C14 C15 C20 C19 178.0(4) . . . . ?
C14 C15 C16 C17 -178.8(5) . . . . ?
C7 C2 C3 C4 1.6(7) . . . . ?
C7 C6 C5 C4 2.6(7) . . . . ?
C20 C15 C14 O3 6.7(6) . . . . ?
C20 C15 C14 O4 -174.1(4) . . . . ?
C20 C15 C16 C17 1.1(7) . . . . ?
C16 C15 C14 O3 -173.5(4) . . . . ?
C16 C15 C14 O4 5.8(7) . . . . ?
C16 C15 C20 C19 -1.9(7) . . . . ?
C16 C17 C21 O1 -172.9(6) . . . . ?
C16 C17 C21 O2 9.2(10) . . . . ?
C18 C17 C21 O1 9.6(9) . . . . ?
C18 C17 C21 O2 -168.3(7) . . . . ?
C5 C4 C3 C2 -0.3(7) . . . . ?
C5 C4 C9 C10 -128.0(6) . . . . ?
C5 C4 C9 C13 51.4(8) . . . . ?
C5 C6 C7 C2 -1.2(7) . . . . ?
N1 C25 C26 C22 -0.8(11) . . . . ?
N1 C24 C23 C22 -2.4(10) . . . . ?
C25 N1 C24 C23 0.8(10) . . . . ?
C17 C18 C19 C20 0.9(8) . . . . ?
C17 C18 C19 C22 -177.4(5) . . . . ?
C19 C18 C17 C16 -1.7(8) . . . . ?
C19 C18 C17 C21 175.8(5) . . . . ?
C19 C22 C23 C24 -179.0(5) . . . . ?
C19 C22 C26 C25 -179.6(6) . . . . ?
C24 N1 C25 C26 0.8(10) . . . . ?
C23 C22 C19 C20 143.5(5) . . . . ?
C23 C22 C19 C18 -38.2(8) . . . . ?
C23 C22 C26 C25 -0.8(9) . . . . ?
C26 C22 C19 C20 -37.7(7) . . . . ?
C26 C22 C19 C18 140.6(6) . . . . ?
C26 C22 C23 C24 2.2(8) . . . . ?
O10 C1 C2 C3 -172.9(5) . . . . ?
O10 C1 C2 C7 6.0(7) . . . . ?
C10 C9 C13 C12 -4.4(10) . . . . ?
C13 C9 C10 C11 -1.1(11) . . . . ?
C12 N2 C11 C10 -6.3(14) . . . . ?
C11 N2 C12 C13 0.4(13) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelxl_CCDC2
_audit_block_doi                 10.5517/cc1j7myb
_database_code_depnum_ccdc_archive 'CCDC 1407522'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H26 N2 O16 Sm2, H2 O'
_chemical_formula_sum            'C34 H28 N2 O17 Sm2'
_chemical_formula_weight         1037.28
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8700(14)
_cell_length_b                   13.860(3)
_cell_length_c                   17.710(3)
_cell_angle_alpha                88.64(3)
_cell_angle_beta                 79.67(3)
_cell_angle_gamma                84.36(3)
_cell_volume                     1650.9(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4056
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.610
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.992
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.087
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_unetI/netI     0.0892
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13450
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.028
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 18.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.2087
	          2theta: 29.8071
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 18.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.2087
	          2theta: 29.8071
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 18.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.2087
	          2theta: 29.8071
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.028108
_diffrn_orient_matrix_UB_12      0.142788
_diffrn_orient_matrix_UB_13      0.029536
_diffrn_orient_matrix_UB_21      0.052221
_diffrn_orient_matrix_UB_22      -0.007213
_diffrn_orient_matrix_UB_23      0.049737
_diffrn_orient_matrix_UB_31      0.039522
_diffrn_orient_matrix_UB_32      0.005692
_diffrn_orient_matrix_UB_33      -0.041186
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4999
_reflns_number_total             5723
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         3.847
_refine_diff_density_min         -1.993
_refine_diff_density_rms         0.237
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.302
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         5723
_refine_ls_number_restraints     193
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0804
_refine_ls_restrained_S_all      1.279
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+51.6027P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1872
_refine_ls_wR_factor_ref         0.1901
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H17B-H14A
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C35 \\sim C13 \\sim C21 \\sim C28 \\sim C25 \\sim C48: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.01
C36 \\sim N1 \\sim C51 \\sim C32 \\sim C33 \\sim C30: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(O9A) \\sim Ueq, Uanis(O9B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O9A) = Uanis(O9B)
4. Others
 Sof(O9B)=1-FVAR(1)
 Sof(O9A)=FVAR(1)
5.a Free rotating group:
 O17(H17A,H17B)
5.b Rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C19(H19), C22(H22), C23(H23), C28(H28), C30(H30), C32(H32),
 C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C43(H43), C46(H46), C48(H48),
  C49(H49), C51(H51), C52(H52)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.70390(11) 0.63421(5) 0.45204(4) 0.0183(2) Uani 1 1 d . . . . .
Sm2 Sm 0.33133(11) 0.36795(5) 0.94717(4) 0.0185(2) Uani 1 1 d . . . . .
O1 O 0.0603(19) 0.2586(9) 0.9627(9) 0.049(4) Uani 1 1 d . . . . .
O2 O 0.353(2) 0.1884(8) 0.9710(8) 0.043(3) Uani 1 1 d . . . . .
O3 O 0.9704(18) 0.7402(8) 0.4685(8) 0.038(3) Uani 1 1 d . . . . .
O4 O 0.6630(16) 0.8084(8) 0.4917(7) 0.028(3) Uani 1 1 d . . . . .
O5 O 0.4199(16) 0.6154(8) 0.5501(6) 0.024(2) Uani 1 1 d . . . . .
O6 O 0.3896(18) 0.4867(8) 0.6250(6) 0.031(3) Uani 1 1 d . . . . .
O7 O 0.456(2) 0.5147(8) 0.9037(7) 0.040(3) Uani 1 1 d . . . . .
O8 O 0.4904(16) 0.6582(8) 0.9467(6) 0.024(2) Uani 1 1 d . . . . .
O9B O 0.871(5) 0.551(3) 0.9540(16) 0.022(5) Uani 0.57(7) 1 d . U P A 2
O10 O 0.0733(17) 0.4445(8) 0.8813(6) 0.028(3) Uani 1 1 d . . . . .
O11 O 0.9853(18) 0.4473(8) 0.6035(7) 0.034(3) Uani 1 1 d . . . . .
O12 O 0.8162(17) 0.5777(8) 0.5619(6) 0.030(3) Uani 1 1 d . . . . .
O13 O 0.380(2) 0.3108(10) 0.8129(7) 0.049(4) Uani 1 1 d . . . . .
H13A H 0.509218 0.301410 0.792343 0.074 Uiso 1 1 d GR . . . .
H13B H 0.323382 0.354111 0.783470 0.074 Uiso 1 1 d GR . . . .
O14 O 0.7015(18) 0.3225(10) 0.8979(8) 0.040(3) Uani 1 1 d . . . . .
H14A H 0.737006 0.318016 0.848786 0.061 Uiso 1 1 d DGR . . . .
H14B H 0.710038 0.264886 0.916923 0.061 Uiso 1 1 d GR . . . .
O15 O 0.3790(17) 0.6927(9) 0.4055(7) 0.034(3) Uani 1 1 d . . . . .
H15A H 0.346529 0.647406 0.377876 0.051 Uiso 1 1 d GR . . . .
H15B H 0.392540 0.744844 0.376761 0.051 Uiso 1 1 d GR . . . .
O16 O 0.8002(18) 0.7107(8) 0.3237(6) 0.028(3) Uani 1 1 d . . . . .
H16A H 0.771639 0.675217 0.284636 0.042 Uiso 1 1 d GR . . . .
H16B H 0.934308 0.717718 0.311766 0.042 Uiso 1 1 d GR . . . .
N1 N 0.327(2) 1.1077(9) 0.7160(8) 0.026(2) Uani 1 1 d . U . . .
N2 N 0.800(2) 1.0477(10) 0.7586(8) 0.028(3) Uani 1 1 d . . . . .
C7 C 0.404(2) 0.5755(12) 0.6153(9) 0.025(3) Uani 1 1 d . . . . .
C11 C 0.457(2) 0.6035(11) 0.8959(8) 0.021(3) Uani 1 1 d . . . . .
C13 C 0.389(2) 0.7385(10) 0.6790(9) 0.019(2) Uani 1 1 d . U . . .
H13 H 0.382767 0.767838 0.631611 0.022 Uiso 1 1 calc R . . . .
C14 C 0.083(2) 0.0883(11) 0.9878(10) 0.027(4) Uani 1 1 d . . . . .
C19 C 0.871(2) 1.0848(11) 0.5032(8) 0.021(3) Uani 1 1 d . . . . .
H19 H 0.785049 1.141225 0.504586 0.025 Uiso 1 1 calc R . . . .
C20 C 0.884(2) 0.7361(11) 0.7559(8) 0.020(3) Uani 1 1 d . . . . .
C21 C 0.380(2) 0.7956(10) 0.7425(8) 0.016(2) Uani 1 1 d . U . . .
C22 C 0.802(2) 0.9946(11) 0.4980(8) 0.020(3) Uani 1 1 d . . . . .
H22 H 0.667976 0.991051 0.497427 0.024 Uiso 1 1 calc R . . . .
C23 C 0.909(2) 0.6819(11) 0.8203(9) 0.021(3) Uani 1 1 d . . . . .
H23 H 0.906815 0.713528 0.866282 0.025 Uiso 1 1 calc R . . . .
C24 C 0.968(2) 0.5232(14) 0.8883(9) 0.029(4) Uani 1 1 d . . . . .
C25 C 0.422(2) 0.6480(10) 0.8193(8) 0.016(2) Uani 1 1 d . U . . .
C26 C 0.859(2) 0.8429(10) 0.7585(8) 0.017(3) Uani 1 1 d . . . . .
C27 C 0.926(2) 0.9112(11) 0.4939(8) 0.020(3) Uani 1 1 d . . . . .
C28 C 0.398(2) 0.7513(10) 0.8133(8) 0.016(2) Uani 1 1 d . U . . .
H28 H 0.394412 0.789108 0.856254 0.020 Uiso 1 1 calc R . . . .
C29 C 0.910(2) 0.5851(10) 0.6849(8) 0.018(3) Uani 1 1 d . . . . .
C30 C 0.442(2) 0.9476(11) 0.6655(9) 0.024(2) Uani 1 1 d . U . . .
H30 H 0.506726 0.910015 0.624034 0.028 Uiso 1 1 calc R . . . .
C32 C 0.273(2) 0.9618(11) 0.7924(9) 0.025(2) Uani 1 1 d . U . . .
H32 H 0.220177 0.934854 0.839390 0.030 Uiso 1 1 calc R . . . .
C33 C 0.366(2) 0.9023(11) 0.7349(9) 0.023(2) Uani 1 1 d . U . . .
C35 C 0.406(2) 0.6362(10) 0.6847(8) 0.015(2) Uani 1 1 d . U . . .
C36 C 0.421(2) 1.0461(11) 0.6583(9) 0.025(2) Uani 1 1 d . U . . .
H36 H 0.473301 1.073184 0.611445 0.030 Uiso 1 1 calc R . . . .
C37 C 0.884(2) 0.6868(11) 0.6863(9) 0.025(4) Uani 1 1 d . . . . .
H37 H 0.867726 0.721757 0.642073 0.030 Uiso 1 1 calc R . . . .
C38 C 0.907(2) 0.5331(11) 0.6099(9) 0.020(3) Uani 1 1 d . . . . .
C39 C 0.948(2) 0.5317(11) 0.7482(8) 0.019(3) Uani 1 1 d . . . . .
H39 H 0.977982 0.464845 0.744890 0.023 Uiso 1 1 calc R . . . .
C40 C 0.763(3) 0.8932(12) 0.8246(10) 0.031(4) Uani 1 1 d . . . . .
H40 H 0.719603 0.859932 0.869696 0.038 Uiso 1 1 calc R . . . .
C41 C -0.124(3) 0.0858(12) 0.9963(9) 0.026(4) Uani 1 1 d . . . . .
H41 H -0.207918 0.142149 0.993374 0.031 Uiso 1 1 calc R . . . .
C42 C 0.170(3) 0.1852(12) 0.9717(9) 0.028(4) Uani 1 1 d . . . . .
C43 C 0.200(3) 0.0044(13) 0.9908(10) 0.032(4) Uani 1 1 d . . . . .
H43 H 0.336577 0.006668 0.983989 0.039 Uiso 1 1 calc R . . . .
C44 C 0.939(2) 0.5801(10) 0.8185(9) 0.018(3) Uani 1 1 d . . . . .
C45 C 0.847(2) 0.8140(11) 0.4835(8) 0.020(3) Uani 1 1 d . . . . .
C46 C 0.893(3) 0.9995(13) 0.6979(10) 0.034(4) Uani 1 1 d . . . . .
H46 H 0.942007 1.034846 0.654571 0.040 Uiso 1 1 calc R . . . .
C48 C 0.422(2) 0.5921(10) 0.7562(8) 0.017(2) Uani 1 1 d . U . . .
H48 H 0.432078 0.524853 0.760693 0.020 Uiso 1 1 calc R . . . .
C49 C 0.923(2) 0.8980(11) 0.6940(9) 0.024(3) Uani 1 1 d . . . . .
H49 H 0.985897 0.867879 0.648501 0.029 Uiso 1 1 calc R . . . .
C51 C 0.252(2) 1.0657(11) 0.7830(9) 0.026(2) Uani 1 1 d . U . . .
H51 H 0.185526 1.104246 0.823754 0.031 Uiso 1 1 calc R . . . .
C52 C 0.735(2) 0.9935(11) 0.8216(10) 0.029(4) Uani 1 1 d . . . . .
H52 H 0.667491 1.025815 0.865411 0.035 Uiso 1 1 calc R . . . .
O17 O 0.779(2) 0.2484(10) 0.7373(8) 0.049(4) Uani 1 1 d . . . . .
H17A H 0.754436 0.224482 0.696633 0.073 Uiso 1 1 d G . . . .
H17B H 0.837370 0.204593 0.761880 0.073 Uiso 1 1 d DG . . . .
O9A O 0.917(6) 0.578(3) 0.949(2) 0.022(5) Uani 0.43(7) 1 d . U P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O3 2.518(11) . ?
Sm1 O4 2.506(11) . ?
Sm1 O5 2.399(11) . ?
Sm1 O6 2.391(10) 2_666 ?
Sm1 O11 2.373(12) 2_766 ?
Sm1 O12 2.312(11) . ?
Sm1 O15 2.567(11) . ?
Sm1 O16 2.492(11) . ?
Sm1 C45 2.868(14) . ?
Sm2 O1 2.488(12) . ?
Sm2 O2 2.509(11) . ?
Sm2 O7 2.345(11) . ?
Sm2 O8 2.422(10) 2_667 ?
Sm2 O9B 2.27(2) 2_667 ?
Sm2 O10 2.438(11) . ?
Sm2 O13 2.478(12) . ?
Sm2 O14 2.558(12) . ?
Sm2 C42 2.857(16) . ?
Sm2 O9A 2.35(4) 2_667 ?
O1 C42 1.23(2) . ?
O2 C42 1.26(2) . ?
O3 C45 1.265(19) . ?
O4 C45 1.254(18) . ?
O5 C7 1.259(19) . ?
O6 C7 1.251(19) . ?
O7 C11 1.237(19) . ?
O8 C11 1.255(18) . ?
O9B C24 1.28(3) . ?
O10 C24 1.24(2) 1_455 ?
O11 C38 1.256(19) . ?
O12 C38 1.257(18) . ?
O13 H13A 0.8931 . ?
O13 H13B 0.8929 . ?
O14 H14A 0.8625 . ?
O14 H14B 0.8599 . ?
O15 H15A 0.8743 . ?
O15 H15B 0.8763 . ?
O16 H16A 0.9187 . ?
O16 H16B 0.9218 . ?
N1 C36 1.37(2) . ?
N1 C51 1.35(2) . ?
N2 C46 1.31(2) . ?
N2 C52 1.36(2) . ?
C7 C35 1.51(2) . ?
C11 C25 1.526(19) . ?
C13 H13 0.9300 . ?
C13 C21 1.38(2) . ?
C13 C35 1.414(19) . ?
C14 C41 1.41(2) . ?
C14 C42 1.52(2) . ?
C14 C43 1.35(2) . ?
C19 H19 0.9300 . ?
C19 C22 1.39(2) . ?
C19 C27 1.41(2) 2_776 ?
C20 C23 1.38(2) . ?
C20 C26 1.47(2) . ?
C20 C37 1.42(2) . ?
C21 C28 1.40(2) . ?
C21 C33 1.48(2) . ?
C22 H22 0.9300 . ?
C22 C27 1.36(2) . ?
C23 H23 0.9300 . ?
C23 C44 1.40(2) . ?
C24 C44 1.48(2) . ?
C24 O9A 1.31(4) . ?
C25 C28 1.427(19) . ?
C25 C48 1.376(19) . ?
C26 C40 1.40(2) . ?
C26 C49 1.39(2) . ?
C27 C45 1.528(19) . ?
C28 H28 0.9300 . ?
C29 C37 1.40(2) . ?
C29 C38 1.53(2) . ?
C29 C39 1.38(2) . ?
C30 H30 0.9300 . ?
C30 C33 1.40(2) . ?
C30 C36 1.36(2) . ?
C32 H32 0.9300 . ?
C32 C33 1.35(2) . ?
C32 C51 1.44(2) . ?
C35 C48 1.41(2) . ?
C36 H36 0.9300 . ?
C37 H37 0.9300 . ?
C39 H39 0.9300 . ?
C39 C44 1.42(2) . ?
C40 H40 0.9300 . ?
C40 C52 1.38(2) . ?
C41 H41 0.9300 . ?
C41 C43 1.40(2) 2_557 ?
C43 H43 0.9300 . ?
C46 H46 0.9300 . ?
C46 C49 1.40(2) . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?
O17 H17A 0.8499 . ?
O17 H17B 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
O3 Sm1 O15 125.2(4) . . ?
O3 Sm1 C45 26.1(4) . . ?
O4 Sm1 O3 51.9(4) . . ?
O4 Sm1 O15 79.4(4) . . ?
O4 Sm1 C45 25.9(4) . . ?
O5 Sm1 O3 122.5(4) . . ?
O5 Sm1 O4 85.7(4) . . ?
O5 Sm1 O15 68.6(4) . . ?
O5 Sm1 O16 141.5(4) . . ?
O5 Sm1 C45 105.9(4) . . ?
O6 Sm1 O3 145.7(4) 2_666 . ?
O6 Sm1 O4 147.4(4) 2_666 . ?
O6 Sm1 O5 91.3(4) 2_666 . ?
O6 Sm1 O15 69.4(4) 2_666 . ?
O6 Sm1 O16 81.5(4) 2_666 . ?
O6 Sm1 C45 156.6(4) 2_666 . ?
O11 Sm1 O3 72.3(4) 2_766 . ?
O11 Sm1 O4 123.0(4) 2_766 . ?
O11 Sm1 O5 141.4(4) 2_766 . ?
O11 Sm1 O6 77.3(4) 2_766 2_666 ?
O11 Sm1 O15 135.8(4) 2_766 . ?
O11 Sm1 O16 73.8(4) 2_766 . ?
O11 Sm1 C45 97.5(4) 2_766 . ?
O12 Sm1 O3 74.6(4) . . ?
O12 Sm1 O4 94.4(4) . . ?
O12 Sm1 O5 71.9(4) . . ?
O12 Sm1 O6 115.5(4) . 2_666 ?
O12 Sm1 O11 80.1(4) . 2_766 ?
O12 Sm1 O15 140.3(4) . . ?
O12 Sm1 O16 144.8(4) . . ?
O12 Sm1 C45 85.5(4) . . ?
O15 Sm1 C45 101.8(4) . . ?
O16 Sm1 O3 75.1(4) . . ?
O16 Sm1 O4 80.9(4) . . ?
O16 Sm1 O15 73.4(4) . . ?
O16 Sm1 C45 75.1(4) . . ?
O1 Sm2 O2 51.6(4) . . ?
O1 Sm2 O14 127.1(4) . . ?
O1 Sm2 C42 25.4(4) . . ?
O2 Sm2 O14 79.6(4) . . ?
O2 Sm2 C42 26.1(5) . . ?
O7 Sm2 O1 150.0(4) . . ?
O7 Sm2 O2 154.9(5) . . ?
O7 Sm2 O8 97.1(4) . 2_667 ?
O7 Sm2 O10 77.3(4) . . ?
O7 Sm2 O13 90.0(5) . . ?
O7 Sm2 O14 75.4(5) . . ?
O7 Sm2 C42 169.5(4) . . ?
O7 Sm2 O9A 100.9(14) . 2_667 ?
O8 Sm2 O1 109.1(4) 2_667 . ?
O8 Sm2 O2 74.8(4) 2_667 . ?
O8 Sm2 O10 155.0(4) 2_667 . ?
O8 Sm2 O13 135.7(4) 2_667 . ?
O8 Sm2 O14 69.4(4) 2_667 . ?
O8 Sm2 C42 92.3(4) 2_667 . ?
O9B Sm2 O1 83.2(12) 2_667 . ?
O9B Sm2 O2 111.1(11) 2_667 . ?
O9B Sm2 O7 89.1(12) 2_667 . ?
O9B Sm2 O10 79.3(7) 2_667 . ?
O9B Sm2 O13 147.8(8) 2_667 . ?
O9B Sm2 O14 139.8(10) 2_667 . ?
O9B Sm2 C42 97.7(12) 2_667 . ?
O9B Sm2 O9A 12.5(9) 2_667 2_667 ?
O10 Sm2 O1 72.8(4) . . ?
O10 Sm2 O2 119.7(4) . . ?
O10 Sm2 O13 69.1(4) . . ?
O10 Sm2 O14 130.4(4) . . ?
O10 Sm2 C42 96.0(4) . . ?
O13 Sm2 O1 81.6(5) . . ?
O13 Sm2 O2 80.6(5) . . ?
O13 Sm2 O14 70.4(4) . . ?
O13 Sm2 C42 80.0(5) . . ?
O14 Sm2 C42 103.9(5) . . ?
O9A Sm2 O1 71.0(14) 2_667 . ?
O9A Sm2 O2 100.6(13) 2_667 . ?
O9A Sm2 O8 78.9(9) 2_667 2_667 ?
O9A Sm2 O10 78.4(9) 2_667 . ?
O9A Sm2 O13 142.4(11) 2_667 . ?
O9A Sm2 O14 147.1(11) 2_667 . ?
O9A Sm2 C42 85.4(14) 2_667 . ?
C42 O1 Sm2 94.3(10) . . ?
C42 O2 Sm2 92.6(10) . . ?
C45 O3 Sm1 92.6(9) . . ?
C45 O4 Sm1 93.4(9) . . ?
C7 O5 Sm1 131.4(10) . . ?
C7 O6 Sm1 132.6(11) . 2_666 ?
C11 O7 Sm2 157.0(13) . . ?
C11 O8 Sm2 133.1(10) . 2_667 ?
C24 O9B Sm2 165(2) . 2_667 ?
C24 O10 Sm2 134.2(10) 1_455 . ?
C38 O11 Sm1 137.3(11) . 2_766 ?
C38 O12 Sm1 165.5(11) . . ?
Sm2 O13 H13A 111.5 . . ?
Sm2 O13 H13B 111.1 . . ?
H13A O13 H13B 107.4 . . ?
Sm2 O14 H14A 116.0 . . ?
Sm2 O14 H14B 98.1 . . ?
H14A O14 H14B 107.8 . . ?
Sm1 O15 H15A 109.3 . . ?
Sm1 O15 H15B 111.2 . . ?
H15A O15 H15B 107.9 . . ?
Sm1 O16 H16A 112.5 . . ?
Sm1 O16 H16B 112.7 . . ?
H16A O16 H16B 106.1 . . ?
C51 N1 C36 116.2(13) . . ?
C46 N2 C52 116.1(14) . . ?
O5 C7 C35 119.3(14) . . ?
O6 C7 O5 122.6(14) . . ?
O6 C7 C35 118.1(14) . . ?
O7 C11 O8 123.5(14) . . ?
O7 C11 C25 117.8(13) . . ?
O8 C11 C25 118.7(13) . . ?
C21 C13 H13 119.4 . . ?
C21 C13 C35 121.2(14) . . ?
C35 C13 H13 119.4 . . ?
C41 C14 C42 118.8(15) . . ?
C43 C14 C41 119.1(14) . . ?
C43 C14 C42 122.1(15) . . ?
C22 C19 H19 120.8 . . ?
C22 C19 C27 118.5(14) . 2_776 ?
C27 C19 H19 120.8 2_776 . ?
C23 C20 C26 121.0(13) . . ?
C23 C20 C37 118.6(14) . . ?
C37 C20 C26 120.4(13) . . ?
C13 C21 C28 119.3(13) . . ?
C13 C21 C33 120.3(13) . . ?
C28 C21 C33 120.2(13) . . ?
C19 C22 H22 119.1 . . ?
C27 C22 C19 121.8(14) . . ?
C27 C22 H22 119.1 . . ?
C20 C23 H23 119.1 . . ?
C20 C23 C44 121.9(14) . . ?
C44 C23 H23 119.1 . . ?
O9B C24 C44 119.9(19) . . ?
O10 C24 O9B 121(2) 1_655 . ?
O10 C24 C44 119.2(14) 1_655 . ?
O10 C24 O9A 128(2) 1_655 . ?
O9A C24 C44 110(2) . . ?
C28 C25 C11 117.9(12) . . ?
C48 C25 C11 122.0(13) . . ?
C48 C25 C28 120.0(13) . . ?
C40 C26 C20 121.9(14) . . ?
C49 C26 C20 121.0(13) . . ?
C49 C26 C40 117.1(14) . . ?
C19 C27 C45 120.2(14) 2_776 . ?
C22 C27 C19 119.7(14) . 2_776 ?
C22 C27 C45 120.1(14) . . ?
C21 C28 C25 120.0(13) . . ?
C21 C28 H28 120.0 . . ?
C25 C28 H28 120.0 . . ?
C37 C29 C38 118.9(13) . . ?
C39 C29 C37 121.4(14) . . ?
C39 C29 C38 119.5(13) . . ?
C33 C30 H30 119.7 . . ?
C36 C30 H30 119.7 . . ?
C36 C30 C33 120.7(15) . . ?
C33 C32 H32 119.0 . . ?
C33 C32 C51 121.9(15) . . ?
C51 C32 H32 119.0 . . ?
C30 C33 C21 121.3(14) . . ?
C32 C33 C21 122.5(14) . . ?
C32 C33 C30 116.2(14) . . ?
C13 C35 C7 120.1(13) . . ?
C48 C35 C7 120.7(13) . . ?
C48 C35 C13 119.2(13) . . ?
N1 C36 H36 118.0 . . ?
C30 C36 N1 124.1(15) . . ?
C30 C36 H36 118.0 . . ?
C20 C37 H37 120.2 . . ?
C29 C37 C20 119.6(15) . . ?
C29 C37 H37 120.2 . . ?
O11 C38 O12 125.5(15) . . ?
O11 C38 C29 116.9(13) . . ?
O12 C38 C29 117.4(13) . . ?
C29 C39 H39 120.5 . . ?
C29 C39 C44 119.0(14) . . ?
C44 C39 H39 120.5 . . ?
C26 C40 H40 120.6 . . ?
C52 C40 C26 118.8(16) . . ?
C52 C40 H40 120.6 . . ?
C14 C41 H41 121.1 . . ?
C43 C41 C14 117.7(16) 2_557 . ?
C43 C41 H41 121.1 2_557 . ?
O1 C42 Sm2 60.3(9) . . ?
O1 C42 O2 121.6(15) . . ?
O1 C42 C14 120.0(15) . . ?
O2 C42 Sm2 61.3(8) . . ?
O2 C42 C14 118.4(16) . . ?
C14 C42 Sm2 178.0(11) . . ?
C14 C43 C41 123.1(16) . 2_557 ?
C14 C43 H43 118.4 . . ?
C41 C43 H43 118.4 2_557 . ?
C23 C44 C24 121.0(14) . . ?
C23 C44 C39 119.3(14) . . ?
C39 C44 C24 119.7(14) . . ?
O3 C45 Sm1 61.3(8) . . ?
O3 C45 C27 118.3(13) . . ?
O4 C45 Sm1 60.7(8) . . ?
O4 C45 O3 121.6(14) . . ?
O4 C45 C27 120.1(14) . . ?
C27 C45 Sm1 175.8(10) . . ?
N2 C46 H46 117.9 . . ?
N2 C46 C49 124.3(16) . . ?
C49 C46 H46 117.9 . . ?
C25 C48 C35 120.3(13) . . ?
C25 C48 H48 119.9 . . ?
C35 C48 H48 119.9 . . ?
C26 C49 C46 119.5(15) . . ?
C26 C49 H49 120.2 . . ?
C46 C49 H49 120.2 . . ?
N1 C51 C32 120.9(14) . . ?
N1 C51 H51 119.5 . . ?
C32 C51 H51 119.5 . . ?
N2 C52 C40 124.2(15) . . ?
N2 C52 H52 117.9 . . ?
C40 C52 H52 117.9 . . ?
H17A O17 H17B 109.4 . . ?
C24 O9A Sm2 148(4) . 2_667 ?

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
Sm1 O3 C45 O4 6.6(16) . . . . ?
Sm1 O3 C45 C27 -175.3(11) . . . . ?
Sm1 O4 C45 O3 -6.6(16) . . . . ?
Sm1 O4 C45 C27 175.3(12) . . . . ?
Sm1 O5 C7 O6 -85.2(18) . . . . ?
Sm1 O5 C7 C35 93.8(16) . . . . ?
Sm1 O6 C7 O5 -19(2) 2_666 . . . ?
Sm1 O6 C7 C35 161.6(10) 2_666 . . . ?
Sm1 O11 C38 O12 87(2) 2_766 . . . ?
Sm1 O11 C38 C29 -97.0(16) 2_766 . . . ?
Sm1 O12 C38 O11 -30(5) . . . . ?
Sm1 O12 C38 C29 155(4) . . . . ?
Sm2 O1 C42 O2 0.5(19) . . . . ?
Sm2 O1 C42 C14 177.7(13) . . . . ?
Sm2 O2 C42 O1 -0.5(18) . . . . ?
Sm2 O2 C42 C14 -177.7(13) . . . . ?
Sm2 O7 C11 O8 77(3) . . . . ?
Sm2 O7 C11 C25 -104(3) . . . . ?
Sm2 O8 C11 O7 25(2) 2_667 . . . ?
Sm2 O8 C11 C25 -153.4(10) 2_667 . . . ?
Sm2 O9B C24 O10 -175(11) 2_667 . . 1_655 ?
Sm2 O9B C24 C44 -1(14) 2_667 . . . ?
O5 C7 C35 C13 12(2) . . . . ?
O5 C7 C35 C48 -169.6(14) . . . . ?
O6 C7 C35 C13 -169.3(14) . . . . ?
O6 C7 C35 C48 9(2) . . . . ?
O7 C11 C25 C28 172.4(15) . . . . ?
O7 C11 C25 C48 -11(2) . . . . ?
O8 C11 C25 C28 -9(2) . . . . ?
O8 C11 C25 C48 167.5(14) . . . . ?
O9B C24 C44 C23 37(3) . . . . ?
O9B C24 C44 C39 -145(3) . . . . ?
O10 C24 C44 C23 -149.3(15) 1_655 . . . ?
O10 C24 C44 C39 29(2) 1_655 . . . ?
O10 C24 O9A Sm2 -103(4) 1_655 . . 2_667 ?
N2 C46 C49 C26 -3(3) . . . . ?
C7 C35 C48 C25 -179.4(14) . . . . ?
C11 C25 C28 C21 175.1(13) . . . . ?
C11 C25 C48 C35 -174.2(13) . . . . ?
C13 C21 C28 C25 -1(2) . . . . ?
C13 C21 C33 C30 -27(2) . . . . ?
C13 C21 C33 C32 149.8(16) . . . . ?
C13 C35 C48 C25 -1(2) . . . . ?
C19 C22 C27 C19 2(2) . . . 2_776 ?
C19 C22 C27 C45 -176.3(13) . . . . ?
C19 C27 C45 O3 -8(2) 2_776 . . . ?
C19 C27 C45 O4 169.9(14) 2_776 . . . ?
C20 C23 C44 C24 179.4(14) . . . . ?
C20 C23 C44 C39 1(2) . . . . ?
C20 C26 C40 C52 -176.3(14) . . . . ?
C20 C26 C49 C46 178.4(14) . . . . ?
C21 C13 C35 C7 176.7(14) . . . . ?
C21 C13 C35 C48 -2(2) . . . . ?
C22 C27 C45 O3 169.8(15) . . . . ?
C22 C27 C45 O4 -12(2) . . . . ?
C23 C20 C26 C40 -33(2) . . . . ?
C23 C20 C26 C49 149.9(15) . . . . ?
C23 C20 C37 C29 0(2) . . . . ?
C26 C20 C23 C44 -178.1(14) . . . . ?
C26 C20 C37 C29 179.5(14) . . . . ?
C26 C40 C52 N2 -2(3) . . . . ?
C27 C19 C22 C27 -2(2) 2_776 . . . ?
C28 C21 C33 C30 148.9(15) . . . . ?
C28 C21 C33 C32 -34(2) . . . . ?
C28 C25 C48 C35 2(2) . . . . ?
C29 C39 C44 C23 -5(2) . . . . ?
C29 C39 C44 C24 176.5(14) . . . . ?
C33 C21 C28 C25 -176.8(14) . . . . ?
C33 C30 C36 N1 0(3) . . . . ?
C33 C32 C51 N1 0(3) . . . . ?
C35 C13 C21 C28 3(2) . . . . ?
C35 C13 C21 C33 178.6(14) . . . . ?
C36 N1 C51 C32 1(2) . . . . ?
C36 C30 C33 C21 177.2(15) . . . . ?
C36 C30 C33 C32 0(2) . . . . ?
C37 C20 C23 C44 1(2) . . . . ?
C37 C20 C26 C40 147.9(16) . . . . ?
C37 C20 C26 C49 -29(2) . . . . ?
C37 C29 C38 O11 159.9(15) . . . . ?
C37 C29 C38 O12 -24(2) . . . . ?
C37 C29 C39 C44 7(2) . . . . ?
C38 C29 C37 C20 179.2(14) . . . . ?
C38 C29 C39 C44 -176.6(13) . . . . ?
C39 C29 C37 C20 -4(2) . . . . ?
C39 C29 C38 O11 -17(2) . . . . ?
C39 C29 C38 O12 159.1(14) . . . . ?
C40 C26 C49 C46 1(2) . . . . ?
C41 C14 C42 O1 -3(2) . . . . ?
C41 C14 C42 O2 173.9(16) . . . . ?
C41 C14 C43 C41 -1(3) . . . 2_557 ?
C42 C14 C41 C43 178.5(15) . . . 2_557 ?
C42 C14 C43 C41 -178.5(15) . . . 2_557 ?
C43 C14 C41 C43 1(3) . . . 2_557 ?
C43 C14 C42 O1 173.5(17) . . . . ?
C43 C14 C42 O2 -9(3) . . . . ?
C44 C24 O9A Sm2 95(5) . . . 2_667 ?
C46 N2 C52 C40 1(2) . . . . ?
C48 C25 C28 C21 -2(2) . . . . ?
C49 C26 C40 C52 1(2) . . . . ?
C51 N1 C36 C30 0(2) . . . . ?
C51 C32 C33 C21 -176.9(14) . . . . ?
C51 C32 C33 C30 0(2) . . . . ?
C52 N2 C46 C49 2(2) . . . . ?
O9A C24 C44 C23 14(3) . . . . ?
O9A C24 C44 C39 -168(3) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_909090
_audit_block_doi                 10.5517/cc1j7mjx
_database_code_depnum_ccdc_archive 'CCDC 1407509'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H19 Gd N2 O10'
_chemical_formula_sum            'C26 H19 Gd N2 O10'
_chemical_formula_weight         676.68
_chemical_melting_point          ?
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'
Gd Gd -0.1653 3.9035 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.684(3)
_cell_length_b                   16.513(3)
_cell_length_c                   10.239(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.63(3)
_cell_angle_gamma                90
_cell_volume                     2402.2(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5636
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   0.602
_shelx_estimated_absorpt_T_min   0.602
_exptl_absorpt_coefficient_mu    2.827
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23758
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.567
_diffrn_reflns_theta_min         3.049
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.0914
	          2theta: 29.8782
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.0914
	          2theta: 29.8782
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.0914
	          2theta: 29.8782
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  
;
Rigaku Mercury375R (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.074767
_diffrn_orient_matrix_UB_12      0.060661
_diffrn_orient_matrix_UB_13      -0.030329
_diffrn_orient_matrix_UB_21      -0.029592
_diffrn_orient_matrix_UB_22      0.010593
_diffrn_orient_matrix_UB_23      -0.051763
_diffrn_orient_matrix_UB_31      -0.018240
_diffrn_orient_matrix_UB_32      0.063794
_diffrn_orient_matrix_UB_33      0.023482
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4664
_reflns_number_total             5529
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.746
_refine_diff_density_min         -2.073
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5529
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0512
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0451P)²+5.7660P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1226
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O12-H12A
 0.85 with sigma of 0.01
 O12-H12B
 0.85 with sigma of 0.01
 H12B-H12A
 1.39 with sigma of 0.01
 O8-H8B
 0.85 with sigma of 0.01
 O8-H8A
 0.85 with sigma of 0.01
 H8B-H8A
 1.39 with sigma of 0.01
 O30-H30
 0.92 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C26 \\sim N34 \\sim C35 \\sim C36 \\sim C37: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
4.a Riding coordinates:
 O30(H30)
4.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C35(H35), C36(H36), C37(H37)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4561(4) -0.1641(4) 0.5773(6) 0.0262(12) Uani 1 1 d . . . . .
H1 H 0.480(4) -0.214(4) 0.538(6) 0.031 Uiso 1 1 d R . . . .
C2 C 0.4903(4) -0.1480(3) 0.7152(5) 0.0235(11) Uani 1 1 d . . . . .
C3 C 0.4585(4) -0.0802(4) 0.7710(6) 0.0254(12) Uani 1 1 d . . . . .
H3 H 0.483(4) -0.072(4) 0.856(7) 0.030 Uiso 1 1 d R . . . .
Gd1 Gd 0.29841(2) 0.18636(2) 0.86567(2) 0.02053(10) Uani 1 1 d . . . . .
O4 O 0.3964(3) 0.0658(3) 0.8694(4) 0.0355(10) Uani 1 1 d . . . . .
O5 O 0.4086(3) 0.2383(3) 0.7585(4) 0.0299(9) Uani 1 1 d . . . . .
O6 O 0.2961(3) 0.0896(2) 0.6740(4) 0.0283(9) Uani 1 1 d . . . . .
O7 O 0.4051(3) 0.1851(3) 1.0775(4) 0.0395(12) Uani 1 1 d . . . . .
O8 O 0.2005(4) 0.0737(3) 0.8882(5) 0.0408(11) Uani 1 1 d D . . . .
H8A H 0.206(6) 0.0270(18) 0.857(6) 0.061 Uiso 1 1 d DR . . . .
H8B H 0.186(6) 0.069(4) 0.963(4) 0.061 Uiso 1 1 d DR . . . .
O9 O 0.1787(3) 0.2270(3) 0.9675(4) 0.0402(11) Uani 1 1 d . . . . .
C10 C 0.0598(4) 0.3078(3) 1.0218(6) 0.0249(12) Uani 1 1 d . . . . .
C11 C 0.3611(4) 0.0473(4) 0.7485(6) 0.0263(12) Uani 1 1 d . . . . .
O12 O 0.3223(4) 0.3337(3) 0.9352(5) 0.0400(11) Uani 1 1 d D . . . .
H12A H 0.379(2) 0.345(5) 0.940(7) 0.060 Uiso 1 1 d DR . . . .
H12B H 0.309(4) 0.347(5) 1.008(4) 0.060 Uiso 1 1 d DR . . . .
C13 C 0.0040(4) 0.3069(4) 0.8890(6) 0.0275(13) Uani 1 1 d . . . . .
H13 H 0.035(5) 0.282(4) 0.823(7) 0.033 Uiso 1 1 d R . . . .
C14 C 0.3654(4) -0.0423(4) 0.5511(6) 0.0285(13) Uani 1 1 d . . . . .
H14 H 0.318(5) -0.011(4) 0.509(7) 0.034 Uiso 1 1 d R . . . .
C15 C 0.1508(4) 0.2614(4) 1.0602(5) 0.0256(12) Uani 1 1 d . . . . .
C16 C 0.3953(4) -0.0270(3) 0.6896(5) 0.0248(12) Uani 1 1 d . . . . .
C17 C 0.0308(4) 0.3519(4) 1.1194(6) 0.0287(13) Uani 1 1 d . . . . .
H17 H 0.067(5) 0.356(4) 1.210(7) 0.034 Uiso 1 1 d R . . . .
C18 C -0.0961(6) 0.4571(5) 1.4194(8) 0.052(2) Uani 1 1 d . . . . .
H18 H -0.087(6) 0.434(5) 1.512(8) 0.063 Uiso 1 1 d R . . . .
C19 C -0.1056(5) 0.3980(4) 0.9544(6) 0.0348(14) Uani 1 1 d . . . . .
H19 H -0.166(5) 0.426(4) 0.922(7) 0.042 Uiso 1 1 d R . . . .
C20 C 0.3949(4) -0.1103(4) 0.4945(5) 0.0273(12) Uani 1 1 d . . . . .
C21 C -0.0809(4) 0.4447(4) 1.1936(6) 0.0317(13) Uani 1 1 d . . . . .
C22 C 0.3636(5) -0.1230(4) 0.3451(6) 0.0357(15) Uani 1 1 d . . . . .
C23 C -0.0795(4) 0.3526(4) 0.8555(6) 0.0331(14) Uani 1 1 d . . . . .
N24 N -0.1352(5) 0.5296(4) 1.3990(6) 0.0485(16) Uani 1 1 d . . . . .
C25 C -0.0519(4) 0.3979(4) 1.0854(6) 0.0282(12) Uani 1 1 d . . . . .
C26 C 0.3705(7) -0.0593(7) 0.2597(8) 0.068(2) Uani 1 1 d . U . . .
H26 H 0.392515 -0.009348 0.296594 0.081 Uiso 1 1 calc R . . . .
C27 C -0.1230(5) 0.5199(4) 1.1707(7) 0.0404(16) Uani 1 1 d . . . . .
H27 H -0.145(5) 0.535(5) 1.095(8) 0.048 Uiso 1 1 d R . . . .
C28 C -0.0670(6) 0.4126(5) 1.3228(8) 0.050(2) Uani 1 1 d . . . . .
H28 H -0.043(6) 0.359(5) 1.353(8) 0.060 Uiso 1 1 d R . . . .
O31 O -0.1266(5) 0.2974(4) 0.6353(6) 0.078(2) Uani 1 1 d . . . . .
C32 C -0.1481(6) 0.5614(5) 1.2753(8) 0.0469(18) Uani 1 1 d . . . . .
H32 H -0.180(5) 0.615(5) 1.276(8) 0.056 Uiso 1 1 d R . . . .
C33 C -0.1411(6) 0.3478(5) 0.7151(7) 0.051(2) Uani 1 1 d . . . . .
N34 N 0.3051(6) -0.1332(6) 0.0678(8) 0.076(2) Uani 1 1 d . U . . .
C35 C 0.3271(7) -0.1954(6) 0.2885(9) 0.066(2) Uani 1 1 d . U . . .
H35 H 0.324348 -0.240947 0.340873 0.080 Uiso 1 1 calc R . . . .
C36 C 0.2927(8) -0.1969(7) 0.1410(9) 0.073(2) Uani 1 1 d . U . . .
H36 H 0.262063 -0.242699 0.098389 0.088 Uiso 1 1 calc R . . . .
C37 C 0.3455(8) -0.0683(7) 0.1213(9) 0.077(2) Uani 1 1 d . U . . .
H37 H 0.358136 -0.027075 0.066616 0.092 Uiso 1 1 calc R . . . .
C38 C 0.4349(4) 0.2024(4) 1.2009(6) 0.0258(12) Uani 1 1 d . . . . .
O29 O 0.1929(3) 0.2577(3) 1.1836(4) 0.0278(9) Uani 1 1 d . . . . .
O30 O -0.2109(4) 0.3971(4) 0.6873(5) 0.0613(16) Uani 1 1 d D . . . .
H30 H -0.236273 0.383148 0.598411 0.092 Uiso 1 1 d DR . . . .


_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
C1 C2 1.399(7) . ?
C1 C20 1.390(8) . ?
C2 C3 1.389(8) . ?
C2 C38 1.508(8) 3_657 ?
C3 C16 1.392(8) . ?
Gd1 O4 2.450(4) . ?
Gd1 O5 2.336(4) . ?
Gd1 O6 2.524(4) . ?
Gd1 O7 2.333(4) . ?
Gd1 O8 2.397(5) . ?
Gd1 O9 2.357(4) . ?
Gd1 O12 2.534(5) . ?
Gd1 O29 2.296(4) 4_565 ?
O4 C11 1.253(7) . ?
O5 C38 1.253(7) 4_565 ?
O6 C11 1.269(7) . ?
O7 C38 1.261(7) . ?
O9 C15 1.259(7) . ?
C10 C13 1.399(8) . ?
C10 C15 1.505(8) . ?
C10 C17 1.387(8) . ?
C11 C16 1.508(8) . ?
C13 C23 1.406(9) . ?
C14 C16 1.398(8) . ?
C14 C20 1.382(8) . ?
C15 O29 1.260(6) . ?
C17 C25 1.400(8) . ?
C18 N24 1.321(10) . ?
C18 C28 1.384(10) . ?
C19 C23 1.389(9) . ?
C19 C25 1.374(8) . ?
C20 C22 1.497(8) . ?
C21 C25 1.498(8) . ?
C21 C27 1.380(9) . ?
C21 C28 1.392(9) . ?
C22 C26 1.389(11) . ?
C22 C35 1.378(11) . ?
C23 C33 1.494(9) . ?
N24 C32 1.340(10) . ?
C26 C37 1.379(11) . ?
C27 C32 1.397(10) . ?
O31 C33 1.222(10) . ?
C33 O30 1.284(9) . ?
N34 C36 1.331(13) . ?
N34 C37 1.279(13) . ?
C35 C36 1.466(12) . ?

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
C20 C1 C2 120.3(5) . . ?
C1 C2 C38 119.0(5) . 3_657 ?
C3 C2 C1 119.7(5) . . ?
C3 C2 C38 121.1(5) . 3_657 ?
C2 C3 C16 120.3(5) . . ?
O4 Gd1 O6 52.45(13) . . ?
O4 Gd1 O12 137.42(16) . . ?
O5 Gd1 O4 80.35(16) . . ?
O5 Gd1 O6 75.07(14) . . ?
O5 Gd1 O8 146.47(16) . . ?
O5 Gd1 O9 141.79(18) . . ?
O5 Gd1 O12 73.50(16) . . ?
O6 Gd1 O12 143.12(15) . . ?
O7 Gd1 O4 74.01(14) . . ?
O7 Gd1 O5 93.33(17) . . ?
O7 Gd1 O6 126.24(14) . . ?
O7 Gd1 O8 100.46(18) . . ?
O7 Gd1 O9 89.52(16) . . ?
O7 Gd1 O12 74.61(16) . . ?
O8 Gd1 O4 74.44(18) . . ?
O8 Gd1 O6 72.10(15) . . ?
O8 Gd1 O12 139.62(17) . . ?
O9 Gd1 O4 136.47(17) . . ?
O9 Gd1 O6 131.24(15) . . ?
O9 Gd1 O8 69.29(18) . . ?
O9 Gd1 O12 70.60(17) . . ?
O29 Gd1 O4 127.80(14) 4_565 . ?
O29 Gd1 O5 82.90(15) 4_565 . ?
O29 Gd1 O6 75.52(14) 4_565 . ?
O29 Gd1 O7 156.27(15) 4_565 . ?
O29 Gd1 O8 95.30(17) 4_565 . ?
O29 Gd1 O9 79.55(15) 4_565 . ?
O29 Gd1 O12 81.89(16) 4_565 . ?
C11 O4 Gd1 95.0(3) . . ?
C38 O5 Gd1 147.2(4) 4_565 . ?
C11 O6 Gd1 91.2(3) . . ?
C38 O7 Gd1 155.7(4) . . ?
C15 O9 Gd1 151.9(4) . . ?
C13 C10 C15 120.8(5) . . ?
C17 C10 C13 119.7(5) . . ?
C17 C10 C15 119.5(5) . . ?
O4 C11 O6 121.4(5) . . ?
O4 C11 C16 119.8(5) . . ?
O6 C11 C16 118.8(5) . . ?
C10 C13 C23 119.4(5) . . ?
C20 C14 C16 121.4(5) . . ?
O9 C15 C10 117.9(5) . . ?
O9 C15 O29 124.3(6) . . ?
O29 C15 C10 117.7(5) . . ?
C3 C16 C11 120.9(5) . . ?
C3 C16 C14 118.9(5) . . ?
C14 C16 C11 120.1(5) . . ?
C10 C17 C25 120.7(5) . . ?
N24 C18 C28 124.6(7) . . ?
C25 C19 C23 121.0(6) . . ?
C1 C20 C22 121.2(5) . . ?
C14 C20 C1 119.2(5) . . ?
C14 C20 C22 119.6(5) . . ?
C27 C21 C25 122.5(6) . . ?
C27 C21 C28 117.1(6) . . ?
C28 C21 C25 120.4(6) . . ?
C26 C22 C20 119.0(7) . . ?
C35 C22 C20 122.6(7) . . ?
C35 C22 C26 118.4(7) . . ?
C13 C23 C33 119.0(6) . . ?
C19 C23 C13 119.8(5) . . ?
C19 C23 C33 121.2(6) . . ?
C18 N24 C32 117.2(6) . . ?
C17 C25 C21 119.1(5) . . ?
C19 C25 C17 119.4(5) . . ?
C19 C25 C21 121.4(6) . . ?
C37 C26 C22 121.5(10) . . ?
C21 C27 C32 120.3(7) . . ?
C18 C28 C21 118.6(7) . . ?
N24 C32 C27 122.1(7) . . ?
O31 C33 C23 121.0(7) . . ?
O31 C33 O30 123.2(7) . . ?
O30 C33 C23 115.8(7) . . ?
C37 N34 C36 122.4(9) . . ?
C22 C35 C36 116.4(9) . . ?
N34 C36 C35 120.4(9) . . ?
N34 C37 C26 120.4(10) . . ?
O5 C38 C2 117.6(5) 4_566 3_657 ?
O5 C38 O7 125.3(5) 4_566 . ?
O7 C38 C2 117.0(5) . 3_657 ?
C15 O29 Gd1 148.7(4) . 4_566 ?

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
C1 C2 C3 C16 -2.1(9) . . . . ?
C1 C20 C22 C26 -129.8(8) . . . . ?
C1 C20 C22 C35 50.9(10) . . . . ?
C2 C1 C20 C14 -2.5(9) . . . . ?
C2 C1 C20 C22 175.1(6) . . . . ?
C2 C3 C16 C11 -179.3(6) . . . . ?
C2 C3 C16 C14 -0.8(9) . . . . ?
Gd1 O4 C11 O6 -0.2(6) . . . . ?
Gd1 O4 C11 C16 -179.6(5) . . . . ?
Gd1 O6 C11 O4 0.2(6) . . . . ?
Gd1 O6 C11 C16 179.6(5) . . . . ?
Gd1 O7 C38 C2 158.9(8) . . . 3_657 ?
Gd1 O7 C38 O5 -22.3(15) . . . 4_566 ?
Gd1 O9 C15 C10 142.3(7) . . . . ?
Gd1 O9 C15 O29 -39.7(13) . . . . ?
O4 C11 C16 C3 6.8(9) . . . . ?
O4 C11 C16 C14 -171.7(6) . . . . ?
O6 C11 C16 C3 -172.6(6) . . . . ?
O6 C11 C16 C14 9.0(9) . . . . ?
O9 C15 O29 Gd1 94.1(9) . . . 4_566 ?
C10 C13 C23 C19 0.0(10) . . . . ?
C10 C13 C23 C33 -176.8(6) . . . . ?
C10 C15 O29 Gd1 -87.9(8) . . . 4_566 ?
C10 C17 C25 C19 1.2(10) . . . . ?
C10 C17 C25 C21 180.0(6) . . . . ?
C13 C10 C15 O9 5.4(8) . . . . ?
C13 C10 C15 O29 -172.8(5) . . . . ?
C13 C10 C17 C25 -2.4(9) . . . . ?
C13 C23 C33 O31 9.7(12) . . . . ?
C13 C23 C33 O30 -173.1(7) . . . . ?
C14 C20 C22 C26 47.8(10) . . . . ?
C14 C20 C22 C35 -131.5(8) . . . . ?
C15 C10 C13 C23 -178.3(6) . . . . ?
C15 C10 C17 C25 177.7(6) . . . . ?
C16 C14 C20 C1 -0.5(10) . . . . ?
C16 C14 C20 C22 -178.1(6) . . . . ?
C17 C10 C13 C23 1.8(9) . . . . ?
C17 C10 C15 O9 -174.7(6) . . . . ?
C17 C10 C15 O29 7.1(8) . . . . ?
C18 N24 C32 C27 1.0(12) . . . . ?
C19 C23 C33 O31 -167.1(8) . . . . ?
C19 C23 C33 O30 10.1(11) . . . . ?
C20 C1 C2 C3 3.8(9) . . . . ?
C20 C1 C2 C38 -173.0(6) . . . 3_657 ?
C20 C14 C16 C3 2.2(10) . . . . ?
C20 C14 C16 C11 -179.4(6) . . . . ?
C20 C22 C26 C37 177.9(8) . . . . ?
C20 C22 C35 C36 175.4(7) . . . . ?
C21 C27 C32 N24 -2.0(12) . . . . ?
C22 C26 C37 N34 8.1(16) . . . . ?
C22 C35 C36 N34 6.0(14) . . . . ?
C23 C19 C25 C17 0.6(10) . . . . ?
C23 C19 C25 C21 -178.2(6) . . . . ?
N24 C18 C28 C21 -1.4(14) . . . . ?
C25 C19 C23 C13 -1.2(11) . . . . ?
C25 C19 C23 C33 175.6(7) . . . . ?
C25 C21 C27 C32 -179.5(7) . . . . ?
C25 C21 C28 C18 -179.0(7) . . . . ?
C26 C22 C35 C36 -3.9(12) . . . . ?
C27 C21 C25 C17 143.5(7) . . . . ?
C27 C21 C25 C19 -37.8(10) . . . . ?
C27 C21 C28 C18 0.3(12) . . . . ?
C28 C18 N24 C32 0.7(13) . . . . ?
C28 C21 C25 C17 -37.3(10) . . . . ?
C28 C21 C25 C19 141.4(8) . . . . ?
C28 C21 C27 C32 1.2(11) . . . . ?
C35 C22 C26 C37 -2.7(13) . . . . ?
C36 N34 C37 C26 -6.0(17) . . . . ?
C37 N34 C36 C35 -1.0(16) . . . . ?
C38 C2 C3 C16 174.6(6) 3_657 . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_787878
_audit_block_doi                 10.5517/cc1j7mx9
_database_code_depnum_ccdc_archive 'CCDC 1407521'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H26 Dy2 N2 O16, H2 O'
_chemical_formula_sum            'C34 H28 Dy2 N2 O17'
_chemical_formula_weight         1061.58
_chemical_melting_point          ?
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'
Dy Dy -0.1892 4.4098 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.9610(14)
_cell_length_b                   26.303(5)
_cell_length_c                   17.797(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.86(3)
_cell_angle_gamma                90
_cell_volume                     3227.9(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5756
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.684
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.184
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1437
_diffrn_reflns_av_unetI/netI     0.0884
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22508
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.054
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 49.9199
	          2theta: 29.8955
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 49.9199
	          2theta: 29.8955
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 49.9199
	          2theta: 29.8955
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.089739
_diffrn_orient_matrix_UB_12      0.052777
_diffrn_orient_matrix_UB_13      -0.100959
_diffrn_orient_matrix_UB_21      0.008329
_diffrn_orient_matrix_UB_22      -0.035395
_diffrn_orient_matrix_UB_23      -0.011099
_diffrn_orient_matrix_UB_31      -0.037587
_diffrn_orient_matrix_UB_32      0.004405
_diffrn_orient_matrix_UB_33      -0.042254
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4259
_reflns_number_total             5612
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.587
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         5612
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0544
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0511P)²+4.3261P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1425
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H17B-O17
 0.85 with sigma of 0.01
 O17-H17A
 0.85 with sigma of 0.01
 H17A-H17B
 1.39 with sigma of 0.01
 H11B_$1-H17B
 2.2 with sigma of 0.01
3.a Rotating group:
 O10(H10A,H10B), O9(H9A,H9B), O11(H11A,H11B), O12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C21(H21), C29(H29), C94(H94), C7(H7), C15(H15), C11(H11), C13(H13),
 C27(H27), C24(H24), C22(H22), C3(H3), C5(H5), C17(H17), C4(H4), C20(H20),
 C19(H19), C18(H18)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O16 O 0.6062(11) 0.1182(2) 0.5398(4) 0.0654(18) Uani 1 1 d . . . . .
O15 O 0.3270(10) 0.1572(2) 0.5273(4) 0.0576(16) Uani 1 1 d . . . . .
C1 C 0.5073(16) 0.1581(3) 0.5286(5) 0.052(2) Uani 1 1 d . . . . .
O8 O -0.0458(10) 0.5797(2) 0.4501(4) 0.0576(16) Uani 1 1 d . . . . .
C9 C 0.0240(14) 0.5489(4) 0.4079(5) 0.048(2) Uani 1 1 d . . . . .
O1 O 0.5764(12) 0.5376(3) 0.4462(4) 0.0639(18) Uani 1 1 d . . . . .
C25 C 0.6555(17) 0.7615(4) 0.3288(6) 0.064(3) Uani 1 1 d . . . . .
H25 H 0.700317 0.776884 0.374920 0.076 Uiso 1 1 calc R . . . .
N2 N 0.5957(15) 0.7914(3) 0.2696(5) 0.068(2) Uani 1 1 d . . . . .
C21 C 0.5313(18) 0.7679(4) 0.2048(7) 0.067(3) Uani 1 1 d . . . . .
H21 H 0.488173 0.787594 0.162495 0.081 Uiso 1 1 calc R . . . .
O4 O 0.6929(10) 0.5513(2) 0.0591(3) 0.0529(15) Uani 1 1 d . . . . .
C2 C 0.6087(15) 0.2078(3) 0.5202(5) 0.053(2) Uani 1 1 d . . . . .
Dy1 Dy 0.31802(6) 0.43003(2) 0.06620(2) 0.04379(16) Uani 1 1 d . . . . .
Dy2 Dy 0.23660(6) 0.43175(2) 0.45086(2) 0.04557(16) Uani 1 1 d . . . . .
O2 O 0.4327(10) 0.4760(2) 0.3753(3) 0.0522(15) Uani 1 1 d . . . . .
O14 O 0.2946(10) 0.3438(2) 0.4858(4) 0.0560(16) Uani 1 1 d . . . . .
O5 O 0.1838(10) 0.5177(3) 0.0801(3) 0.0536(15) Uani 1 1 d . . . . .
O6 O 0.1544(10) 0.4610(2) 0.1681(3) 0.0545(16) Uani 1 1 d . . . . .
O13 O 0.5501(11) 0.3840(2) 0.4586(4) 0.0634(18) Uani 1 1 d . . . . .
C29 C 0.5734(13) 0.5236(3) 0.2459(5) 0.049(2) Uani 1 1 d . . . . .
H29 H 0.564792 0.488408 0.242759 0.059 Uiso 1 1 calc R . . . .
C10 C 0.0533(13) 0.5671(3) 0.3284(5) 0.0458(19) Uani 1 1 d . . . . .
C28 C 0.6037(13) 0.5509(3) 0.1833(5) 0.048(2) Uani 1 1 d . . . . .
C94 C 0.5598(13) 0.5996(3) 0.3163(5) 0.0458(19) Uani 1 1 d . . . . .
H94 H 0.547227 0.615697 0.361885 0.055 Uiso 1 1 calc R . . . .
C7 C 0.5023(14) 0.2515(3) 0.5045(5) 0.048(2) Uani 1 1 d . . . . .
H7 H 0.367579 0.249929 0.496821 0.058 Uiso 1 1 calc R . . . .
C8 C 0.4706(14) 0.3442(3) 0.4803(5) 0.050(2) Uani 1 1 d . . . . .
C30 C 0.1478(12) 0.5077(3) 0.1459(5) 0.0466(19) Uani 1 1 d . . . . .
C32 C 0.5217(13) 0.5176(3) 0.3838(5) 0.049(2) Uani 1 1 d . . . . .
C15 C 0.0509(13) 0.6189(3) 0.3114(5) 0.048(2) Uani 1 1 d . . . . .
H15 H 0.033393 0.642612 0.348590 0.058 Uiso 1 1 calc R . . . .
C11 C 0.0807(13) 0.5326(3) 0.2731(5) 0.0450(19) Uani 1 1 d . . . . .
H11 H 0.082303 0.498152 0.284942 0.054 Uiso 1 1 calc R . . . .
C26 C 0.5824(13) 0.6291(3) 0.2534(5) 0.0476(19) Uani 1 1 d . . . . .
C31 C 0.5553(13) 0.5473(3) 0.3133(5) 0.0471(19) Uani 1 1 d . . . . .
C6 C 0.5955(14) 0.2981(3) 0.4999(5) 0.051(2) Uani 1 1 d . . . . .
C13 C 0.1029(14) 0.5994(4) 0.1835(5) 0.053(2) Uani 1 1 d . . . . .
H13 H 0.119770 0.609904 0.134882 0.063 Uiso 1 1 calc R . . . .
C12 C 0.1058(13) 0.5470(3) 0.2010(5) 0.048(2) Uani 1 1 d . . . . .
C27 C 0.6068(13) 0.6043(3) 0.1860(5) 0.048(2) Uani 1 1 d . . . . .
H27 H 0.625030 0.623053 0.143205 0.057 Uiso 1 1 calc R . . . .
C24 C 0.6547(15) 0.7100(4) 0.3259(6) 0.057(2) Uani 1 1 d . . . . .
H24 H 0.698648 0.691060 0.368968 0.068 Uiso 1 1 calc R . . . .
C33 C 0.6232(12) 0.5258(3) 0.1087(5) 0.0444(19) Uani 1 1 d . . . . .
C14 C 0.0751(14) 0.6354(4) 0.2380(5) 0.051(2) Uani 1 1 d . . . . .
C23 C 0.5877(14) 0.6856(4) 0.2578(5) 0.050(2) Uani 1 1 d . . . . .
C22 C 0.5256(18) 0.7155(4) 0.1975(6) 0.064(3) Uani 1 1 d . . . . .
H22 H 0.478966 0.700799 0.151037 0.077 Uiso 1 1 calc R . . . .
C3 C 0.8100(17) 0.2113(4) 0.5330(7) 0.066(3) Uani 1 1 d . . . . .
H3 H 0.884076 0.182170 0.544146 0.079 Uiso 1 1 calc R . . . .
C16 C 0.0639(15) 0.6904(4) 0.2199(6) 0.059(2) Uani 1 1 d . . . . .
C5 C 0.7918(16) 0.3016(4) 0.5123(6) 0.062(3) Uani 1 1 d . . . . .
H5 H 0.852437 0.332872 0.509561 0.074 Uiso 1 1 calc R . . . .
C17 C -0.0173(16) 0.7088(4) 0.1491(6) 0.065(3) Uani 1 1 d . . . . .
H17 H -0.061459 0.686657 0.109825 0.078 Uiso 1 1 calc R . . . .
C4 C 0.9011(16) 0.2579(4) 0.5291(7) 0.066(3) Uani 1 1 d . . . . .
H4 H 1.035671 0.259874 0.537850 0.079 Uiso 1 1 calc R . . . .
C20 C 0.1258(17) 0.7273(4) 0.2753(7) 0.065(3) Uani 1 1 d . . . . .
H20 H 0.182945 0.717566 0.323504 0.078 Uiso 1 1 calc R . . . .
N1 N 0.0197(19) 0.7958(4) 0.1899(7) 0.091(3) Uani 1 1 d . . . . .
C19 C 0.100(2) 0.7784(5) 0.2569(8) 0.082(4) Uani 1 1 d . . . . .
H19 H 0.142165 0.802177 0.294250 0.099 Uiso 1 1 calc R . . . .
C18 C -0.031(2) 0.7615(4) 0.1386(7) 0.077(3) Uani 1 1 d . . . . .
H18 H -0.080464 0.772994 0.090464 0.093 Uiso 1 1 calc R . . . .
O3 O 0.5789(10) 0.4794(2) 0.1011(3) 0.0516(15) Uani 1 1 d . . . . .
O7 O 0.0615(12) 0.5032(2) 0.4224(4) 0.0647(19) Uani 1 1 d . . . . .
O10 O -0.0172(10) 0.4164(3) 0.0212(4) 0.0560(15) Uani 1 1 d . . . . .
H10A H -0.040467 0.384193 0.013022 0.084 Uiso 1 1 d GR . . . .
H10B H -0.050306 0.432771 -0.021222 0.084 Uiso 1 1 d GR . . . .
O9 O 0.4500(11) 0.3890(3) 0.1841(4) 0.0641(18) Uani 1 1 d . . . . .
H9A H 0.581102 0.387071 0.189654 0.096 Uiso 1 1 d GR . . . .
H9B H 0.405956 0.356749 0.186752 0.096 Uiso 1 1 d GR . . . .
O11 O 0.2306(11) 0.3917(3) 0.3262(4) 0.0638(18) Uani 1 1 d . . . . .
H11A H 0.281360 0.412193 0.293213 0.096 Uiso 1 1 d GR . . . .
H11B H 0.108674 0.384107 0.304929 0.096 Uiso 1 1 d DGR . . . .
O12 O -0.0905(12) 0.3987(4) 0.3959(4) 0.078(2) Uani 1 1 d . . . . .
H12A H -0.077034 0.375569 0.363069 0.117 Uiso 1 1 d GR . . . .
H12B H -0.159068 0.423028 0.374097 0.117 Uiso 1 1 d GR . . . .
O17 O 0.8360(15) 0.4071(4) 0.2249(6) 0.092(3) Uani 1 1 d D . . . .
H17A H 0.85(2) 0.403(5) 0.179(3) 0.138 Uiso 1 1 d DR . . . .
H17B H 0.892(13) 0.4344(15) 0.241(6) 0.138 Uiso 1 1 d DR . . . .


_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
O16 C1 1.257(11) . ?
O16 Dy1 2.472(7) 4_566 ?
O15 C1 1.252(12) . ?
O15 Dy1 2.400(6) 4_566 ?
C1 C2 1.502(13) . ?
C1 Dy1 2.793(9) 4_566 ?
O8 C9 1.247(11) . ?
O8 Dy2 2.367(6) 3_566 ?
C9 C10 1.532(11) . ?
C9 O7 1.250(11) . ?
O1 Dy2 2.247(7) 3_666 ?
O1 C32 1.240(11) . ?
C25 H25 0.9300 . ?
C25 N2 1.335(13) . ?
C25 C24 1.355(14) . ?
N2 C21 1.330(14) . ?
C21 H21 0.9300 . ?
C21 C22 1.385(14) . ?
O4 Dy1 2.274(6) 3_665 ?
O4 C33 1.259(10) . ?
C2 C7 1.375(13) . ?
C2 C3 1.392(15) . ?
Dy1 O5 2.513(6) . ?
Dy1 O6 2.411(6) . ?
Dy1 O3 2.250(6) . ?
Dy1 O10 2.388(7) . ?
Dy1 O9 2.426(7) . ?
Dy2 O2 2.351(6) . ?
Dy2 O14 2.416(6) . ?
Dy2 O13 2.505(7) . ?
Dy2 O7 2.260(7) . ?
Dy2 O11 2.451(7) . ?
Dy2 O12 2.508(8) . ?
O2 C32 1.257(11) . ?
O14 C8 1.242(11) . ?
O5 C30 1.257(10) . ?
O6 C30 1.291(10) . ?
O13 C8 1.270(11) . ?
C29 H29 0.9300 . ?
C29 C28 1.365(12) . ?
C29 C31 1.374(12) . ?
C10 C15 1.396(12) . ?
C10 C11 1.371(11) . ?
C28 C27 1.407(13) . ?
C28 C33 1.505(11) . ?
C94 H94 0.9300 . ?
C94 C26 1.388(12) . ?
C94 C31 1.376(13) . ?
C7 H7 0.9300 . ?
C7 C6 1.395(13) . ?
C8 C6 1.505(13) . ?
C30 C12 1.482(12) . ?
C32 C31 1.522(12) . ?
C15 H15 0.9300 . ?
C15 C14 1.407(12) . ?
C11 H11 0.9300 . ?
C11 C12 1.372(12) . ?
C26 C27 1.396(12) . ?
C26 C23 1.487(12) . ?
C6 C5 1.357(14) . ?
C13 H13 0.9300 . ?
C13 C12 1.413(13) . ?
C13 C14 1.388(13) . ?
C27 H27 0.9300 . ?
C24 H24 0.9300 . ?
C24 C23 1.394(13) . ?
C33 O3 1.261(10) . ?
C14 C16 1.483(13) . ?
C23 C22 1.353(13) . ?
C22 H22 0.9300 . ?
C3 H3 0.9300 . ?
C3 C4 1.385(15) . ?
C16 C17 1.396(14) . ?
C16 C20 1.408(15) . ?
C5 H5 0.9300 . ?
C5 C4 1.388(15) . ?
C17 H17 0.9300 . ?
C17 C18 1.399(15) . ?
C4 H4 0.9300 . ?
C20 H20 0.9300 . ?
C20 C19 1.390(16) . ?
N1 C19 1.327(17) . ?
N1 C18 1.296(16) . ?
C19 H19 0.9300 . ?
C18 H18 0.9300 . ?
O10 H10A 0.8721 . ?
O10 H10B 0.8718 . ?
O9 H9A 0.9059 . ?
O9 H9B 0.9049 . ?
O11 H11A 0.9032 . ?
O11 H11B 0.9034 . ?
O12 H12A 0.8575 . ?
O12 H12B 0.8580 . ?
O17 H17A 0.851(10) . ?
O17 H17B 0.851(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O16 Dy1 91.0(6) . 4_566 ?
C1 O15 Dy1 94.5(5) . 4_566 ?
O16 C1 C2 119.2(9) . . ?
O16 C1 Dy1 62.2(5) . 4_566 ?
O15 C1 O16 120.9(9) . . ?
O15 C1 C2 119.9(8) . . ?
O15 C1 Dy1 59.0(5) . 4_566 ?
C2 C1 Dy1 171.6(6) . 4_566 ?
C9 O8 Dy2 132.2(6) . 3_566 ?
O8 C9 C10 117.8(8) . . ?
O8 C9 O7 125.9(8) . . ?
O7 C9 C10 116.2(7) . . ?
C32 O1 Dy2 162.7(7) . 3_666 ?
N2 C25 H25 118.0 . . ?
N2 C25 C24 124.0(10) . . ?
C24 C25 H25 118.0 . . ?
C21 N2 C25 116.2(9) . . ?
N2 C21 H21 118.5 . . ?
N2 C21 C22 123.1(10) . . ?
C22 C21 H21 118.5 . . ?
C33 O4 Dy1 147.0(6) . 3_665 ?
C7 C2 C1 120.0(9) . . ?
C7 C2 C3 118.6(9) . . ?
C3 C2 C1 121.2(8) . . ?
O16 Dy1 C1 26.7(3) 4_565 4_565 ?
O16 Dy1 O5 144.3(2) 4_565 . ?
O15 Dy1 O16 53.2(2) 4_565 4_565 ?
O15 Dy1 C1 26.5(2) 4_565 4_565 ?
O15 Dy1 O5 158.5(2) 4_565 . ?
O15 Dy1 O6 125.0(2) 4_565 . ?
O15 Dy1 O9 78.6(2) 4_565 . ?
O4 Dy1 O16 81.0(3) 3_665 4_565 ?
O4 Dy1 O15 85.5(2) 3_665 4_565 ?
O4 Dy1 C1 84.1(2) 3_665 4_565 ?
O4 Dy1 O5 86.3(2) 3_665 . ?
O4 Dy1 O6 135.1(2) 3_665 . ?
O4 Dy1 O10 78.7(2) 3_665 . ?
O4 Dy1 O9 154.4(3) 3_665 . ?
O5 Dy1 C1 168.3(2) . 4_565 ?
O6 Dy1 O16 142.7(2) . 4_565 ?
O6 Dy1 C1 138.4(2) . 4_565 ?
O6 Dy1 O5 52.8(2) . . ?
O6 Dy1 O9 70.2(2) . . ?
O3 Dy1 O16 72.8(2) . 4_565 ?
O3 Dy1 O15 125.4(2) . 4_565 ?
O3 Dy1 C1 99.0(3) . 4_565 ?
O3 Dy1 O4 93.6(2) . 3_665 ?
O3 Dy1 O5 74.9(2) . . ?
O3 Dy1 O6 92.5(2) . . ?
O3 Dy1 O10 153.3(2) . . ?
O3 Dy1 O9 79.8(2) . . ?
O10 Dy1 O16 129.8(2) . 4_565 ?
O10 Dy1 O15 79.8(2) . 4_565 ?
O10 Dy1 C1 105.5(3) . 4_565 ?
O10 Dy1 O5 79.1(2) . . ?
O10 Dy1 O6 76.2(2) . . ?
O10 Dy1 O9 117.4(2) . . ?
O9 Dy1 O16 73.5(3) . 4_565 ?
O9 Dy1 C1 72.7(2) . 4_565 ?
O9 Dy1 O5 115.2(2) . . ?
O8 Dy2 O14 77.2(2) 3_566 . ?
O8 Dy2 O13 118.0(2) 3_566 . ?
O8 Dy2 O11 132.7(2) 3_566 . ?
O8 Dy2 O12 71.0(2) 3_566 . ?
O1 Dy2 O8 76.1(3) 3_666 3_566 ?
O1 Dy2 O2 88.4(2) 3_666 . ?
O1 Dy2 O14 94.4(2) 3_666 . ?
O1 Dy2 O13 74.4(3) 3_666 . ?
O1 Dy2 O7 96.8(3) 3_666 . ?
O1 Dy2 O11 145.9(3) 3_666 . ?
O1 Dy2 O12 146.8(3) 3_666 . ?
O2 Dy2 O8 156.6(2) . 3_566 ?
O2 Dy2 O14 122.1(2) . . ?
O2 Dy2 O13 73.1(2) . . ?
O2 Dy2 O11 68.6(2) . . ?
O2 Dy2 O12 121.0(2) . . ?
O14 Dy2 O13 52.6(2) . . ?
O14 Dy2 O11 78.6(2) . . ?
O14 Dy2 O12 83.1(3) . . ?
O13 Dy2 O12 125.9(3) . . ?
O7 Dy2 O8 86.1(2) . 3_566 ?
O7 Dy2 O2 78.3(2) . . ?
O7 Dy2 O14 157.0(3) . . ?
O7 Dy2 O13 150.3(2) . . ?
O7 Dy2 O11 102.3(3) . . ?
O7 Dy2 O12 76.6(3) . . ?
O11 Dy2 O13 75.0(2) . . ?
O11 Dy2 O12 66.2(3) . . ?
C32 O2 Dy2 132.7(6) . . ?
C8 O14 Dy2 95.9(5) . . ?
C30 O5 Dy1 91.4(5) . . ?
C30 O6 Dy1 95.3(5) . . ?
C8 O13 Dy2 91.0(6) . . ?
C28 C29 H29 119.4 . . ?
C28 C29 C31 121.2(9) . . ?
C31 C29 H29 119.4 . . ?
C15 C10 C9 120.4(7) . . ?
C11 C10 C9 120.4(7) . . ?
C11 C10 C15 119.2(8) . . ?
C29 C28 C27 120.0(8) . . ?
C29 C28 C33 122.1(8) . . ?
C27 C28 C33 117.8(8) . . ?
C26 C94 H94 118.9 . . ?
C31 C94 H94 118.9 . . ?
C31 C94 C26 122.2(8) . . ?
C2 C7 H7 119.8 . . ?
C2 C7 C6 120.3(9) . . ?
C6 C7 H7 119.8 . . ?
O14 C8 O13 120.5(9) . . ?
O14 C8 C6 121.3(8) . . ?
O13 C8 C6 118.2(9) . . ?
O5 C30 O6 118.7(8) . . ?
O5 C30 C12 123.7(8) . . ?
O6 C30 C12 117.6(8) . . ?
O1 C32 O2 124.2(8) . . ?
O1 C32 C31 117.2(8) . . ?
O2 C32 C31 118.5(8) . . ?
C10 C15 H15 119.9 . . ?
C10 C15 C14 120.2(8) . . ?
C14 C15 H15 119.9 . . ?
C10 C11 H11 118.8 . . ?
C10 C11 C12 122.5(8) . . ?
C12 C11 H11 118.8 . . ?
C94 C26 C27 118.2(8) . . ?
C94 C26 C23 121.4(8) . . ?
C27 C26 C23 120.4(8) . . ?
C29 C31 C94 118.8(8) . . ?
C29 C31 C32 122.0(8) . . ?
C94 C31 C32 119.1(8) . . ?
C7 C6 C8 117.6(9) . . ?
C5 C6 C7 121.0(9) . . ?
C5 C6 C8 121.4(9) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C14 C13 C12 120.6(8) . . ?
C11 C12 C30 119.3(8) . . ?
C11 C12 C13 118.5(8) . . ?
C13 C12 C30 122.1(8) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 C28 119.5(8) . . ?
C26 C27 H27 120.3 . . ?
C25 C24 H24 120.2 . . ?
C25 C24 C23 119.6(10) . . ?
C23 C24 H24 120.2 . . ?
O4 C33 C28 118.4(8) . . ?
O4 C33 O3 123.5(8) . . ?
O3 C33 C28 118.0(8) . . ?
C15 C14 C16 119.5(8) . . ?
C13 C14 C15 119.0(8) . . ?
C13 C14 C16 121.4(8) . . ?
C24 C23 C26 120.6(8) . . ?
C22 C23 C26 122.4(9) . . ?
C22 C23 C24 117.0(9) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.1(10) . . ?
C23 C22 H22 119.9 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.6(9) . . ?
C4 C3 H3 119.7 . . ?
C17 C16 C14 122.5(10) . . ?
C17 C16 C20 116.2(10) . . ?
C20 C16 C14 121.2(10) . . ?
C6 C5 H5 120.3 . . ?
C6 C5 C4 119.3(10) . . ?
C4 C5 H5 120.3 . . ?
C16 C17 H17 120.8 . . ?
C16 C17 C18 118.4(11) . . ?
C18 C17 H17 120.8 . . ?
C3 C4 C5 120.1(10) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C16 C20 H20 120.5 . . ?
C19 C20 C16 118.9(12) . . ?
C19 C20 H20 120.5 . . ?
C18 N1 C19 115.7(11) . . ?
C20 C19 H19 117.6 . . ?
N1 C19 C20 124.7(13) . . ?
N1 C19 H19 117.6 . . ?
C17 C18 H18 117.0 . . ?
N1 C18 C17 126.0(12) . . ?
N1 C18 H18 117.0 . . ?
C33 O3 Dy1 139.9(6) . . ?
C9 O7 Dy2 159.6(7) . . ?
Dy1 O10 H10A 110.6 . . ?
Dy1 O10 H10B 110.3 . . ?
H10A O10 H10B 108.3 . . ?
Dy1 O9 H9A 112.1 . . ?
Dy1 O9 H9B 111.8 . . ?
H9A O9 H9B 106.6 . . ?
Dy2 O11 H11A 111.9 . . ?
Dy2 O11 H11B 111.9 . . ?
H11A O11 H11B 106.8 . . ?
Dy2 O12 H12A 109.5 . . ?
Dy2 O12 H12B 109.7 . . ?
H12A O12 H12B 109.1 . . ?
H17A O17 H17B 109.4(19) . . ?

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
O16 C1 C2 C7 177.0(9) . . . . ?
O16 C1 C2 C3 -7.3(14) . . . . ?
O15 C1 C2 C7 -5.8(13) . . . . ?
O15 C1 C2 C3 170.0(10) . . . . ?
C1 C2 C7 C6 177.2(8) . . . . ?
C1 C2 C3 C4 -176.4(10) . . . . ?
O8 C9 C10 C15 16.5(14) . . . . ?
O8 C9 C10 C11 -163.1(9) . . . . ?
O8 C9 O7 Dy2 -110.2(17) . . . . ?
C9 C10 C15 C14 -179.1(9) . . . . ?
C9 C10 C11 C12 179.4(9) . . . . ?
O1 C32 C31 C29 154.2(9) . . . . ?
O1 C32 C31 C94 -28.5(13) . . . . ?
C25 N2 C21 C22 -0.2(18) . . . . ?
C25 C24 C23 C26 -179.0(10) . . . . ?
C25 C24 C23 C22 -0.2(15) . . . . ?
N2 C25 C24 C23 -0.3(17) . . . . ?
N2 C21 C22 C23 -0.2(19) . . . . ?
O4 C33 O3 Dy1 -97.1(11) . . . . ?
C2 C7 C6 C8 178.3(8) . . . . ?
C2 C7 C6 C5 -1.3(14) . . . . ?
C2 C3 C4 C5 -0.1(18) . . . . ?
Dy1 O16 C1 O15 -6.6(9) 4_566 . . . ?
Dy1 O16 C1 C2 170.6(7) 4_566 . . . ?
Dy1 O15 C1 O16 6.8(9) 4_566 . . . ?
Dy1 O15 C1 C2 -170.4(7) 4_566 . . . ?
Dy1 O4 C33 C28 -141.8(9) 3_665 . . . ?
Dy1 O4 C33 O3 42.4(17) 3_665 . . . ?
Dy1 O5 C30 O6 -13.0(8) . . . . ?
Dy1 O5 C30 C12 164.3(8) . . . . ?
Dy1 O6 C30 O5 13.7(9) . . . . ?
Dy1 O6 C30 C12 -163.8(7) . . . . ?
Dy2 O8 C9 C10 150.9(7) 3_566 . . . ?
Dy2 O8 C9 O7 -24.3(15) 3_566 . . . ?
Dy2 O1 C32 O2 113(2) 3_666 . . . ?
Dy2 O1 C32 C31 -71(2) 3_666 . . . ?
Dy2 O2 C32 O1 24.7(14) . . . . ?
Dy2 O2 C32 C31 -151.6(6) . . . . ?
Dy2 O14 C8 O13 -2.4(9) . . . . ?
Dy2 O14 C8 C6 176.9(7) . . . . ?
Dy2 O13 C8 O14 2.3(9) . . . . ?
Dy2 O13 C8 C6 -177.0(7) . . . . ?
O2 C32 C31 C29 -29.3(13) . . . . ?
O2 C32 C31 C94 148.0(9) . . . . ?
O14 C8 C6 C7 16.9(13) . . . . ?
O14 C8 C6 C5 -163.5(9) . . . . ?
O5 C30 C12 C11 -175.8(9) . . . . ?
O5 C30 C12 C13 0.1(14) . . . . ?
O6 C30 C12 C11 1.6(12) . . . . ?
O6 C30 C12 C13 177.4(9) . . . . ?
O13 C8 C6 C7 -163.8(9) . . . . ?
O13 C8 C6 C5 15.8(14) . . . . ?
C29 C28 C27 C26 1.2(14) . . . . ?
C29 C28 C33 O4 -164.4(9) . . . . ?
C29 C28 C33 O3 11.7(13) . . . . ?
C10 C9 O7 Dy2 75(2) . . . . ?
C10 C15 C14 C13 -0.6(14) . . . . ?
C10 C15 C14 C16 177.4(9) . . . . ?
C10 C11 C12 C30 175.9(8) . . . . ?
C10 C11 C12 C13 -0.1(14) . . . . ?
C28 C29 C31 C94 2.8(14) . . . . ?
C28 C29 C31 C32 -179.9(9) . . . . ?
C28 C33 O3 Dy1 87.1(11) . . . . ?
C94 C26 C27 C28 1.3(13) . . . . ?
C94 C26 C23 C24 28.5(14) . . . . ?
C94 C26 C23 C22 -150.3(10) . . . . ?
C7 C2 C3 C4 -0.6(16) . . . . ?
C7 C6 C5 C4 0.6(16) . . . . ?
C8 C6 C5 C4 -179.1(9) . . . . ?
C15 C10 C11 C12 -0.1(14) . . . . ?
C15 C14 C16 C17 -144.1(10) . . . . ?
C15 C14 C16 C20 32.2(15) . . . . ?
C11 C10 C15 C14 0.5(14) . . . . ?
C26 C94 C31 C29 -0.2(14) . . . . ?
C26 C94 C31 C32 -177.5(8) . . . . ?
C26 C23 C22 C21 179.2(10) . . . . ?
C31 C29 C28 C27 -3.3(14) . . . . ?
C31 C29 C28 C33 -179.8(8) . . . . ?
C31 C94 C26 C27 -1.9(14) . . . . ?
C31 C94 C26 C23 -179.7(9) . . . . ?
C6 C5 C4 C3 0.2(17) . . . . ?
C13 C14 C16 C17 33.9(16) . . . . ?
C13 C14 C16 C20 -149.8(10) . . . . ?
C12 C13 C14 C15 0.4(15) . . . . ?
C12 C13 C14 C16 -177.6(9) . . . . ?
C27 C28 C33 O4 19.1(13) . . . . ?
C27 C28 C33 O3 -164.8(8) . . . . ?
C27 C26 C23 C24 -149.4(9) . . . . ?
C27 C26 C23 C22 31.9(15) . . . . ?
C24 C25 N2 C21 0.4(17) . . . . ?
C24 C23 C22 C21 0.4(16) . . . . ?
C33 C28 C27 C26 177.8(8) . . . . ?
C14 C13 C12 C30 -176.0(9) . . . . ?
C14 C13 C12 C11 0.0(14) . . . . ?
C14 C16 C17 C18 176.6(10) . . . . ?
C14 C16 C20 C19 -175.6(10) . . . . ?
C23 C26 C27 C28 179.2(9) . . . . ?
C3 C2 C7 C6 1.3(14) . . . . ?
C16 C17 C18 N1 -3(2) . . . . ?
C16 C20 C19 N1 0(2) . . . . ?
C17 C16 C20 C19 0.9(15) . . . . ?
C20 C16 C17 C18 0.1(16) . . . . ?
C19 N1 C18 C17 4(2) . . . . ?
C18 N1 C19 C20 -2(2) . . . . ?
O7 C9 C10 C15 -167.9(9) . . . . ?
O7 C9 C10 C11 12.5(13) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_2222222
_audit_block_doi                 10.5517/cc1j7mgv
_database_code_depnum_ccdc_archive 'CCDC 1407507'
_audit_update_record             
;
2018-01-10 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C26 H20 N2 O10 Sm'
_chemical_formula_sum            'C26 H20 N2 O10 Sm'
_chemical_formula_weight         670.80
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.640(3)
_cell_length_b                   16.580(3)
_cell_length_c                   10.250(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.63(3)
_cell_angle_gamma                90
_cell_volume                     2407.3(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4435
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.505
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1013
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.913
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15251
_diffrn_reflns_point_group_measured_fraction_full 0.913
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.008
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         3.048
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.0789
	          2theta: 29.9086
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.0789
	          2theta: 29.9086
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.0789
	          2theta: 29.9086
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.006716
_diffrn_orient_matrix_UB_12      -0.099733
_diffrn_orient_matrix_UB_13      -0.013176
_diffrn_orient_matrix_UB_21      0.038201
_diffrn_orient_matrix_UB_22      -0.003573
_diffrn_orient_matrix_UB_23      0.046516
_diffrn_orient_matrix_UB_31      -0.051433
_diffrn_orient_matrix_UB_32      -0.026794
_diffrn_orient_matrix_UB_33      0.040182
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2781
_reflns_number_total             3873
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         2.648
_refine_diff_density_min         -3.774
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.705
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3873
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2030
_refine_ls_R_factor_gt           0.1739
_refine_ls_restrained_S_all      2.705
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5265
_refine_ls_wR_factor_ref         0.5976
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Rotating group:
 O7BA(H7BA,H7BB), O1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C8AA(H8AA), C9AA(H9AA), C2BA(H2BA), C0DA(H0DA), C1DA(H1DA), C4DA(H4DA),
 C6DA(H6DA), C3CA(H3CA), C4CA(H4CA), C8CA(H8CA), C19(H19), C4(H4), N6(H6),
 C2(H2), C10(H10)
2.c Fitted hexagon refined as free rotating group:
 C4CA(C8CA,C18,C19,C4,N6)
2.d Idealised tetrahedral OH refined as rotating group:
 O9BA(H9BA)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.79865(10) 0.18607(5) 0.36556(10) 0.1165(10) Uani 1 1 d . . . . .
O0AA O 0.6949(12) 0.2425(7) 0.1801(12) 0.121(4) Uani 1 1 d . . . . .
O3BA O 0.9100(14) 0.1837(6) 0.5830(12) 0.144(7) Uani 1 1 d . . . . .
O4BA O 0.6737(14) 0.2232(12) 0.4652(17) 0.145(5) Uani 1 1 d . . . . .
O5BA O 0.8979(14) 0.0620(8) 0.3706(15) 0.123(4) Uani 1 1 d . . . . .
O6BA O 0.9095(13) 0.2374(9) 0.2557(18) 0.134(5) Uani 1 1 d . . . . .
O7BA O 0.8221(14) 0.3351(9) 0.4389(16) 0.131(4) Uani 1 1 d . . . . .
H7BA H 0.886187 0.349788 0.475337 0.196 Uiso 1 1 d GR . . . .
H7BB H 0.790971 0.349655 0.506303 0.196 Uiso 1 1 d GR . . . .
C8BA C 0.6536(14) 0.2383(10) 0.0624(18) 0.106(4) Uani 1 1 d . . . . .
O9BA O 0.3650(19) 0.1997(13) -0.370(2) 0.152(7) Uani 1 1 d . . . . .
H9BA H 0.415550 0.188537 -0.386120 0.227 Uiso 1 1 calc GR . . . .
C2AA C 0.5566(16) 0.1935(10) 0.0161(18) 0.103(5) Uani 1 1 d . . . . .
O3AA O 0.7952(11) 0.0892(7) 0.1683(14) 0.125(4) Uani 1 1 d . . . . .
C4AA C 0.8938(17) -0.0280(11) 0.185(2) 0.121(5) Uani 1 1 d . . . . .
O5AA O 0.2869(17) 0.0996(15) -0.320(2) 0.171(8) Uani 1 1 d . . . . .
N6AA N 0.3620(14) -0.0277(11) 0.3940(19) 0.125(5) Uani 1 1 d . . . . .
C7AA C 1.0148(18) 0.1461(10) 0.7858(19) 0.122(6) Uani 1 1 d . . . . .
C8AA C 1.0415(15) 0.1636(11) 0.922(2) 0.114(5) Uani 1 1 d . . . . .
H8AA H 1.018743 0.208978 0.957301 0.137 Uiso 1 1 calc R . . . .
C9AA C 0.406(2) 0.0418(17) 0.418(2) 0.151(9) Uani 1 1 d . . . . .
H9AA H 0.423983 0.060819 0.505731 0.181 Uiso 1 1 calc R . . . .
C0BA C 0.9391(17) 0.2016(13) 0.701(2) 0.111(5) Uani 1 1 d . . . . .
C2BA C 0.393(2) 0.1010(18) -0.045(2) 0.144(7) Uani 1 1 d . . . . .
H2BA H 0.338165 0.070135 -0.066473 0.172 Uiso 1 1 calc R . . . .
C0CA C 0.8567(14) 0.0469(10) 0.2422(19) 0.106(4) Uani 1 1 d . . . . .
C0DA C 0.8622(16) -0.0418(11) 0.0433(15) 0.115(5) Uani 1 1 d . . . . .
H0DA H 0.821106 -0.006416 -0.013069 0.138 Uiso 1 1 calc R . . . .
C1DA C 0.531(2) 0.1477(13) 0.121(2) 0.132(7) Uani 1 1 d . . . . .
H1DA H 0.567944 0.147964 0.209494 0.159 Uiso 1 1 calc R . . . .
C2DA C 0.416(2) 0.0559(12) 0.191(3) 0.135(7) Uani 1 1 d . . . . .
C3DA C 1.1047(16) 0.1097(12) 1.006(2) 0.120(5) Uani 1 1 d . . . . .
C4DA C 0.374(2) -0.0211(15) 0.1685(19) 0.142(8) Uani 1 1 d . . . . .
H4DA H 0.359924 -0.045145 0.083726 0.170 Uiso 1 1 calc R . . . .
C6DA C 1.043(2) 0.0828(11) 0.731(3) 0.133(7) Uani 1 1 d . . . . .
H6DA H 1.021688 0.073702 0.638790 0.160 Uiso 1 1 calc R . . . .
C1CA C 0.420(2) 0.1480(14) -0.150(3) 0.138(7) Uani 1 1 d . . . . .
C3CA C 0.426(2) 0.0882(14) 0.315(3) 0.145(8) Uani 1 1 d . . . . .
H3CA H 0.447017 0.141133 0.331362 0.174 Uiso 1 1 calc R . . . .
C4CA C 1.2082(18) 0.2017(15) 1.357(2) 0.26(3) Uani 1 1 d . . . . .
H4CA H 1.236138 0.249068 1.396594 0.312 Uiso 1 1 calc R . . . .
C8CA C 1.1780(19) 0.1957(10) 1.2174(19) 0.182(17) Uani 1 1 d G . . . .
H8CA H 1.185686 0.239092 1.163665 0.219 Uiso 1 1 calc R . . . .
C18 C 1.1362(14) 0.1249(10) 1.1582(11) 0.128(6) Uani 1 1 d G . . . .
C19 C 1.1247(14) 0.0601(10) 1.2386(16) 0.150(10) Uani 1 1 d G . . . .
H19 H 1.096704 0.012771 1.199002 0.180 Uiso 1 1 calc R . . . .
C4 C 1.1549(17) 0.0661(14) 1.3782(15) 0.21(2) Uani 1 1 d G . . . .
H4 H 1.147155 0.022745 1.431931 0.257 Uiso 1 1 calc R . . . .
N6 N 1.1966(16) 0.1369(18) 1.4374(12) 0.172(10) Uani 1 1 d G . . . .
H6 H 1.215349 0.140592 1.523701 0.206 Uiso 1 1 calc R . . . .
C5CA C 0.4458(18) 0.1019(13) 0.083(2) 0.130(6) Uani 1 1 d . . . . .
C2 C 0.357(3) -0.0577(16) 0.276(4) 0.180(14) Uani 1 1 d . . . . .
H2 H 0.338184 -0.111477 0.264062 0.216 Uiso 1 1 calc R . . . .
C3 C 0.346(3) 0.146(2) -0.2857(17) 0.175(15) Uani 1 1 d . . . . .
C10 C 0.516(4) 0.1921(11) -0.114(3) 0.169(17) Uani 1 1 d . . . . .
H10 H 0.542225 0.215780 -0.177772 0.203 Uiso 1 1 calc R . . . .
O1 O 0.6997(16) 0.0711(9) 0.386(2) 0.139(5) Uani 1 1 d . . . . .
H1A H 0.724669 0.023473 0.368740 0.208 Uiso 1 1 d GR . . . .
H1B H 0.641707 0.074672 0.328132 0.208 Uiso 1 1 d GR . . . .


_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 O0AA 2.310(14) . ?
Sm1 O3BA 2.406(7) . ?
Sm1 O4BA 2.390(14) . ?
Sm1 O5BA 2.512(14) . ?
Sm1 O6BA 2.356(13) . ?
Sm1 O7BA 2.580(16) . ?
Sm1 O3AA 2.573(14) . ?
Sm1 C0CA 2.862(18) . ?
Sm1 O1 2.436(16) . ?
O0AA C8BA 1.21(2) . ?
O3BA C0BA 1.21(2) . ?
O4BA C8BA 1.28(2) 4_566 ?
O5BA C0CA 1.33(2) . ?
O6BA C0BA 1.29(3) 4_565 ?
O7BA H7BA 0.9501 . ?
O7BA H7BB 0.9492 . ?
C8BA C2AA 1.57(3) . ?
O9BA H9BA 0.8200 . ?
O9BA C3 1.32(5) . ?
C2AA C1DA 1.44(2) . ?
C2AA C10 1.31(3) . ?
O3AA C0CA 1.24(2) . ?
C4AA C0CA 1.53(2) . ?
C4AA C0DA 1.43(3) . ?
C4AA C6DA 1.42(3) 3_756 ?
O5AA C3 1.15(5) . ?
N6AA C9AA 1.31(3) . ?
N6AA C2 1.29(4) . ?
C7AA C8AA 1.38(3) . ?
C7AA C0BA 1.53(3) . ?
C7AA C6DA 1.30(3) . ?
C8AA H8AA 0.9300 . ?
C8AA C3DA 1.41(3) . ?
C9AA H9AA 0.9300 . ?
C9AA C3CA 1.40(4) . ?
C2BA H2BA 0.9300 . ?
C2BA C1CA 1.47(3) . ?
C2BA C5CA 1.34(3) . ?
C0DA H0DA 0.9300 . ?
C0DA C3DA 1.37(3) 3_756 ?
C1DA H1DA 0.9300 . ?
C1DA C5CA 1.43(3) . ?
C2DA C4DA 1.41(3) . ?
C2DA C3CA 1.35(4) . ?
C2DA C5CA 1.50(3) . ?
C3DA C18 1.53(2) . ?
C4DA H4DA 0.9300 . ?
C4DA C2 1.34(4) . ?
C6DA H6DA 0.9300 . ?
C1CA C3 1.53(4) . ?
C1CA C10 1.54(5) . ?
C3CA H3CA 0.9300 . ?
C4CA H4CA 0.9300 . ?
C4CA C8CA 1.3900 . ?
C4CA N6 1.3900 . ?
C8CA H8CA 0.9300 . ?
C8CA C18 1.3900 . ?
C18 C19 1.3900 . ?
C19 H19 0.9300 . ?
C19 C4 1.3900 . ?
C4 H4 0.9300 . ?
C4 N6 1.3900 . ?
N6 H6 0.8600 . ?
C2 H2 0.9300 . ?
C10 H10 0.9300 . ?
O1 H1A 0.9069 . ?
O1 H1B 0.9067 . ?

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
O0AA Sm1 O3BA 156.8(4) . . ?
O0AA Sm1 O4BA 80.3(6) . . ?
O0AA Sm1 O5BA 127.3(5) . . ?
O0AA Sm1 O6BA 81.4(6) . . ?
O0AA Sm1 O7BA 82.1(5) . . ?
O0AA Sm1 O3AA 74.2(4) . . ?
O0AA Sm1 C0CA 99.8(5) . . ?
O0AA Sm1 O1 96.1(6) . . ?
O3BA Sm1 O5BA 73.4(5) . . ?
O3BA Sm1 O7BA 74.7(5) . . ?
O3BA Sm1 O3AA 126.3(5) . . ?
O3BA Sm1 C0CA 100.9(5) . . ?
O3BA Sm1 O1 100.7(7) . . ?
O4BA Sm1 O3BA 91.2(7) . . ?
O4BA Sm1 O5BA 134.7(6) . . ?
O4BA Sm1 O7BA 71.8(6) . . ?
O4BA Sm1 O3AA 129.2(6) . . ?
O4BA Sm1 C0CA 137.9(6) . . ?
O4BA Sm1 O1 68.2(7) . . ?
O5BA Sm1 O7BA 138.1(6) . . ?
O5BA Sm1 O3AA 53.2(4) . . ?
O5BA Sm1 C0CA 27.6(5) . . ?
O6BA Sm1 O3BA 93.5(7) . . ?
O6BA Sm1 O4BA 143.7(7) . . ?
O6BA Sm1 O5BA 80.8(6) . . ?
O6BA Sm1 O7BA 74.7(5) . . ?
O6BA Sm1 O3AA 74.3(5) . . ?
O6BA Sm1 C0CA 76.3(5) . . ?
O6BA Sm1 O1 145.2(6) . . ?
O7BA Sm1 C0CA 150.3(6) . . ?
O3AA Sm1 O7BA 143.3(4) . . ?
O3AA Sm1 C0CA 25.6(5) . . ?
O1 Sm1 O5BA 73.2(8) . . ?
O1 Sm1 O7BA 139.7(6) . . ?
O1 Sm1 O3AA 71.7(6) . . ?
O1 Sm1 C0CA 69.9(6) . . ?
C8BA O0AA Sm1 149.1(12) . . ?
C0BA O3BA Sm1 154.8(17) . . ?
C8BA O4BA Sm1 144.5(16) 4_566 . ?
C0CA O5BA Sm1 91.1(11) . . ?
C0BA O6BA Sm1 147.4(15) 4_565 . ?
Sm1 O7BA H7BA 113.9 . . ?
Sm1 O7BA H7BB 113.7 . . ?
H7BA O7BA H7BB 104.9 . . ?
O0AA C8BA O4BA 126.4(18) . 4_565 ?
O0AA C8BA C2AA 121.1(15) . . ?
O4BA C8BA C2AA 111.8(17) 4_565 . ?
C3 O9BA H9BA 109.5 . . ?
C1DA C2AA C8BA 114.3(19) . . ?
C10 C2AA C8BA 117(2) . . ?
C10 C2AA C1DA 127(2) . . ?
C0CA O3AA Sm1 90.3(11) . . ?
C0DA C4AA C0CA 117.7(19) . . ?
C6DA C4AA C0CA 122.0(18) 3_756 . ?
C6DA C4AA C0DA 120.4(17) 3_756 . ?
C2 N6AA C9AA 115(2) . . ?
C8AA C7AA C0BA 115.4(16) . . ?
C6DA C7AA C8AA 124(2) . . ?
C6DA C7AA C0BA 120(2) . . ?
C7AA C8AA H8AA 121.5 . . ?
C7AA C8AA C3DA 117.0(17) . . ?
C3DA C8AA H8AA 121.5 . . ?
N6AA C9AA H9AA 118.9 . . ?
N6AA C9AA C3CA 122(2) . . ?
C3CA C9AA H9AA 118.9 . . ?
O3BA C0BA O6BA 124(2) . 4_566 ?
O3BA C0BA C7AA 116.3(17) . . ?
O6BA C0BA C7AA 119.8(18) 4_566 . ?
C1CA C2BA H2BA 119.5 . . ?
C5CA C2BA H2BA 119.5 . . ?
C5CA C2BA C1CA 121(3) . . ?
O5BA C0CA Sm1 61.3(9) . . ?
O5BA C0CA C4AA 114.6(17) . . ?
O3AA C0CA Sm1 64.1(10) . . ?
O3AA C0CA O5BA 125.4(17) . . ?
O3AA C0CA C4AA 120.0(18) . . ?
C4AA C0CA Sm1 175.9(14) . . ?
C4AA C0DA H0DA 121.6 . . ?
C3DA C0DA C4AA 116.9(17) 3_756 . ?
C3DA C0DA H0DA 121.6 3_756 . ?
C2AA C1DA H1DA 121.7 . . ?
C5CA C1DA C2AA 117(2) . . ?
C5CA C1DA H1DA 121.7 . . ?
C4DA C2DA C5CA 122(2) . . ?
C3CA C2DA C4DA 117(2) . . ?
C3CA C2DA C5CA 121(2) . . ?
C8AA C3DA C18 119.8(16) . . ?
C0DA C3DA C8AA 122.4(17) 3_756 . ?
C0DA C3DA C18 117.8(16) 3_756 . ?
C2DA C4DA H4DA 121.9 . . ?
C2 C4DA C2DA 116(2) . . ?
C2 C4DA H4DA 121.9 . . ?
C4AA C6DA H6DA 120.6 3_756 . ?
C7AA C6DA C4AA 119(2) . 3_756 ?
C7AA C6DA H6DA 120.6 . . ?
C2BA C1CA C3 113(3) . . ?
C2BA C1CA C10 118(2) . . ?
C3 C1CA C10 129(3) . . ?
C9AA C3CA H3CA 120.1 . . ?
C2DA C3CA C9AA 120(2) . . ?
C2DA C3CA H3CA 120.1 . . ?
C8CA C4CA H4CA 120.0 . . ?
C8CA C4CA N6 120.0 . . ?
N6 C4CA H4CA 120.0 . . ?
C4CA C8CA H8CA 120.0 . . ?
C18 C8CA C4CA 120.0 . . ?
C18 C8CA H8CA 120.0 . . ?
C8CA C18 C3DA 124.7(13) . . ?
C8CA C18 C19 120.0 . . ?
C19 C18 C3DA 115.2(13) . . ?
C18 C19 H19 120.0 . . ?
C4 C19 C18 120.0 . . ?
C4 C19 H19 120.0 . . ?
C19 C4 H4 120.0 . . ?
N6 C4 C19 120.0 . . ?
N6 C4 H4 120.0 . . ?
C4CA N6 H6 120.0 . . ?
C4 N6 C4CA 120.0 . . ?
C4 N6 H6 120.0 . . ?
C2BA C5CA C1DA 122(2) . . ?
C2BA C5CA C2DA 121(2) . . ?
C1DA C5CA C2DA 118(2) . . ?
N6AA C2 C4DA 128(3) . . ?
N6AA C2 H2 116.0 . . ?
C4DA C2 H2 116.0 . . ?
O9BA C3 C1CA 111(4) . . ?
O5AA C3 O9BA 122(2) . . ?
O5AA C3 C1CA 127(3) . . ?
C2AA C10 C1CA 114(3) . . ?
C2AA C10 H10 122.9 . . ?
C1CA C10 H10 122.9 . . ?
Sm1 O1 H1A 112.7 . . ?
Sm1 O1 H1B 111.8 . . ?
H1A O1 H1B 106.6 . . ?

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
Sm1 O0AA C8BA O4BA -104(3) . . . 4_565 ?
Sm1 O0AA C8BA C2AA 86(3) . . . . ?
Sm1 O3BA C0BA O6BA -19(5) . . . 4_566 ?
Sm1 O3BA C0BA C7AA 160(3) . . . . ?
Sm1 O5BA C0CA O3AA 1(2) . . . . ?
Sm1 O5BA C0CA C4AA 179.1(15) . . . . ?
Sm1 O3AA C0CA O5BA -1(2) . . . . ?
Sm1 O3AA C0CA C4AA -178.9(17) . . . . ?
O0AA C8BA C2AA C1DA -10(3) . . . . ?
O0AA C8BA C2AA C10 179(2) . . . . ?
O4BA C8BA C2AA C1DA 178.9(19) 4_565 . . . ?
O4BA C8BA C2AA C10 8(3) 4_565 . . . ?
C8BA C2AA C1DA C5CA -176.5(18) . . . . ?
C8BA C2AA C10 C1CA -179(2) . . . . ?
C2AA C1DA C5CA C2BA 1(4) . . . . ?
C2AA C1DA C5CA C2DA -178(2) . . . . ?
N6AA C9AA C3CA C2DA -12(5) . . . . ?
C7AA C8AA C3DA C0DA -1(3) . . . 3_756 ?
C7AA C8AA C3DA C18 -179.2(19) . . . . ?
C8AA C7AA C0BA O3BA -175(2) . . . . ?
C8AA C7AA C0BA O6BA 4(3) . . . 4_566 ?
C8AA C7AA C6DA C4AA -1(4) . . . 3_756 ?
C8AA C3DA C18 C8CA -55(3) . . . . ?
C8AA C3DA C18 C19 127.6(19) . . . . ?
C9AA N6AA C2 C4DA -13(6) . . . . ?
C0BA C7AA C8AA C3DA 174.5(18) . . . . ?
C0BA C7AA C6DA C4AA -174.0(19) . . . 3_756 ?
C2BA C1CA C3 O9BA 169(2) . . . . ?
C2BA C1CA C3 O5AA -20(4) . . . . ?
C2BA C1CA C10 C2AA -10(4) . . . . ?
C0CA C4AA C0DA C3DA -179.3(19) . . . 3_756 ?
C0DA C4AA C0CA O5BA -171.6(18) . . . . ?
C0DA C4AA C0CA O3AA 6(3) . . . . ?
C0DA C3DA C18 C8CA 126.3(19) 3_756 . . . ?
C0DA C3DA C18 C19 -51(2) 3_756 . . . ?
C1DA C2AA C10 C1CA 12(5) . . . . ?
C2DA C4DA C2 N6AA 9(6) . . . . ?
C3DA C18 C19 C4 177.1(16) . . . . ?
C4DA C2DA C3CA C9AA 7(4) . . . . ?
C4DA C2DA C5CA C2BA 39(4) . . . . ?
C4DA C2DA C5CA C1DA -142(3) . . . . ?
C6DA C4AA C0CA O5BA 9(3) 3_756 . . . ?
C6DA C4AA C0CA O3AA -174(2) 3_756 . . . ?
C6DA C4AA C0DA C3DA 0(3) 3_756 . . 3_756 ?
C6DA C7AA C8AA C3DA 1(3) . . . . ?
C6DA C7AA C0BA O3BA -1(3) . . . . ?
C6DA C7AA C0BA O6BA 178(2) . . . 4_566 ?
C1CA C2BA C5CA C1DA -1(4) . . . . ?
C1CA C2BA C5CA C2DA 178(2) . . . . ?
C3CA C2DA C4DA C2 -6(4) . . . . ?
C3CA C2DA C5CA C2BA -139(3) . . . . ?
C3CA C2DA C5CA C1DA 40(4) . . . . ?
C4CA C8CA C18 C3DA -176.8(18) . . . . ?
C4CA C8CA C18 C19 0.0 . . . . ?
C8CA C4CA N6 C4 0.0 . . . . ?
C8CA C18 C19 C4 0.0 . . . . ?
C18 C19 C4 N6 0.0 . . . . ?
C19 C4 N6 C4CA 0.0 . . . . ?
N6 C4CA C8CA C18 0.0 . . . . ?
C5CA C2BA C1CA C3 -174(2) . . . . ?
C5CA C2BA C1CA C10 5(4) . . . . ?
C5CA C2DA C4DA C2 176(3) . . . . ?
C5CA C2DA C3CA C9AA -175(3) . . . . ?
C2 N6AA C9AA C3CA 14(5) . . . . ?
C3 C1CA C10 C2AA 169(2) . . . . ?
C10 C2AA C1DA C5CA -7(4) . . . . ?
C10 C1CA C3 O9BA -10(4) . . . . ?
C10 C1CA C3 O5AA 161(3) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_787878_CCDC1
_audit_block_doi                 10.5517/cc1j7mky
_database_code_depnum_ccdc_archive 'CCDC 1407510'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H19 N2 O10 Tb'
_chemical_formula_sum            'C26 H19 N2 O10 Tb'
_chemical_formula_weight         678.35
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.726(3)
_cell_length_b                   16.484(3)
_cell_length_c                   10.208(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.47(3)
_cell_angle_gamma                90
_cell_volume                     2399.2(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6075
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.013
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1161
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24320
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.557
_diffrn_reflns_theta_min         3.047
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1492
	          2theta: 29.8723
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1492
	          2theta: 29.8723
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1492
	          2theta: 29.8723
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.024084
_diffrn_orient_matrix_UB_12      -0.094062
_diffrn_orient_matrix_UB_13      0.028462
_diffrn_orient_matrix_UB_21      0.035422
_diffrn_orient_matrix_UB_22      0.022350
_diffrn_orient_matrix_UB_23      0.043890
_diffrn_orient_matrix_UB_31      -0.048540
_diffrn_orient_matrix_UB_32      -0.016827
_diffrn_orient_matrix_UB_33      0.047743
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4688
_reflns_number_total             5530
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.417
_refine_diff_density_min         -1.779
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5530
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0456
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0352P)²+3.4900P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1152
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H,H) groups
2. Restrained distances
 H9A-H9B
 1.39 with sigma of 0.01
 H10A-O10
 0.85 with sigma of 0.01
 H9A-O9
 0.85 with sigma of 0.01
 H9B-O9
 0.85 with sigma of 0.01
 H10B-O10
 0.85 with sigma of 0.01
 H10B-H10A
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N2 \\sim C24 \\sim C23 \\sim C25 \\sim C26: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
4.a Rotating group:
 O9(H9A)
4.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C16(H16), C10(H10), C21(H21), C12(H12), C7(H7), C4(H4), C2(H2),
 C1(H1A), C23(H23), C5(H5), C26(H26), C25(H25), C24(H24)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N2 N 0.3060(5) -0.1323(5) -0.4329(7) 0.0656(17) Uani 1 1 d . U . . .
C18 C 0.5646(4) -0.2032(3) 0.3000(6) 0.0240(11) Uani 1 1 d . . . . .
C19 C 0.4561(4) -0.1642(3) 0.0772(6) 0.0258(11) Uani 1 1 d . . . . .
H19 H 0.475020 -0.210810 0.040084 0.031 Uiso 1 1 calc R . . . .
C17 C 0.4899(4) -0.1486(3) 0.2157(5) 0.0221(10) Uani 1 1 d . . . . .
C16 C 0.4588(4) -0.0803(3) 0.2725(5) 0.0254(11) Uani 1 1 d . . . . .
H16 H 0.480291 -0.070243 0.364695 0.030 Uiso 1 1 calc R . . . .
Tb1 Tb 0.29929(2) 0.18665(2) 0.36640(2) 0.01890(9) Uani 1 1 d . . . . .
O4 O 0.1815(3) 0.2277(3) 0.4696(4) 0.0376(10) Uani 1 1 d . . . . .
O5 O 0.3960(3) 0.0657(2) 0.3701(4) 0.0317(9) Uani 1 1 d . . . . .
O6 O 0.2965(3) 0.0904(2) 0.1746(4) 0.0264(8) Uani 1 1 d . . . . .
C14 C 0.3617(4) 0.0473(3) 0.2486(6) 0.0260(11) Uani 1 1 d . . . . .
C11 C 0.0613(4) 0.3081(3) 0.5220(6) 0.0241(11) Uani 1 1 d . . . . .
C13 C 0.1526(4) 0.2613(3) 0.5615(5) 0.0226(11) Uani 1 1 d . . . . .
C10 C 0.0060(4) 0.3064(3) 0.3902(6) 0.0298(12) Uani 1 1 d . . . . .
H10 H 0.024151 0.275626 0.324657 0.036 Uiso 1 1 calc R . . . .
C21 C 0.3643(4) -0.0420(3) 0.0511(5) 0.0266(11) Uani 1 1 d . . . . .
H21 H 0.323140 -0.005979 -0.003852 0.032 Uiso 1 1 calc R . . . .
O1 O -0.2100(4) 0.3960(4) 0.1876(5) 0.0618(16) Uani 1 1 d . . . . .
H1 H -0.245857 0.383801 0.114983 0.093 Uiso 1 1 calc GR . . . .
C12 C 0.0321(4) 0.3519(3) 0.6204(6) 0.0264(11) Uani 1 1 d . . . . .
H12 H 0.067786 0.350671 0.709508 0.032 Uiso 1 1 calc R . . . .
C15 C 0.3954(4) -0.0268(3) 0.1906(6) 0.0230(11) Uani 1 1 d . . . . .
C8 C -0.0774(4) 0.3511(4) 0.3566(6) 0.0311(13) Uani 1 1 d . . . . .
C20 C 0.3944(4) -0.1105(3) -0.0055(5) 0.0256(11) Uani 1 1 d . . . . .
C3 C -0.0807(4) 0.4437(4) 0.6946(6) 0.0291(12) Uani 1 1 d . . . . .
C22 C 0.3637(4) -0.1232(4) -0.1543(6) 0.0317(13) Uani 1 1 d . . . . .
C7 C -0.1046(4) 0.3978(4) 0.4539(6) 0.0352(14) Uani 1 1 d . . . . .
H7 H -0.158789 0.429008 0.429845 0.042 Uiso 1 1 calc R . . . .
C6 C -0.0508(4) 0.3979(3) 0.5870(6) 0.0270(11) Uani 1 1 d . . . . .
C9 C -0.1390(5) 0.3457(5) 0.2143(7) 0.0459(17) Uani 1 1 d . . . . .
C4 C -0.1239(5) 0.5200(4) 0.6697(7) 0.0373(14) Uani 1 1 d . . . . .
H4 H -0.135779 0.543124 0.583983 0.045 Uiso 1 1 calc R . . . .
O7 O 0.5954(3) -0.1850(3) 0.4218(4) 0.0384(11) Uani 1 1 d . . . . .
O3 O 0.1945(3) 0.2577(2) 0.6850(4) 0.0266(8) Uani 1 1 d . . . . .
O8 O 0.5920(3) -0.2619(2) 0.2410(4) 0.0286(9) Uani 1 1 d . . . . .
O9 O 0.2017(4) 0.0745(3) 0.3891(5) 0.0409(11) Uani 1 1 d D . . . .
H9A H 0.190258 0.075348 0.468311 0.061 Uiso 1 1 d DGR . . . .
O10 O 0.3249(4) 0.3331(3) 0.4360(5) 0.0383(10) Uani 1 1 d D . . . .
N1 N -0.1358(4) 0.5307(4) 0.8975(6) 0.0479(15) Uani 1 1 d . . . . .
C2 C -0.0677(5) 0.4127(4) 0.8228(7) 0.0448(17) Uani 1 1 d . . . . .
H2 H -0.040756 0.361862 0.843979 0.054 Uiso 1 1 calc R . . . .
C1 C -0.0953(6) 0.4584(5) 0.9206(7) 0.0506(19) Uani 1 1 d . . . . .
H1A H -0.084808 0.437000 1.007442 0.061 Uiso 1 1 calc R . . . .
C23 C 0.3253(6) -0.1949(5) -0.2122(8) 0.0569(17) Uani 1 1 d . U . . .
H23 H 0.320766 -0.240080 -0.159734 0.068 Uiso 1 1 calc R . . . .
C5 C -0.1485(5) 0.5601(4) 0.7742(7) 0.0422(16) Uani 1 1 d . . . . .
H5 H -0.175784 0.611128 0.756653 0.051 Uiso 1 1 calc R . . . .
C26 C 0.3470(6) -0.0682(6) -0.3780(8) 0.0659(19) Uani 1 1 d . U . . .
H26 H 0.359900 -0.026672 -0.432381 0.079 Uiso 1 1 calc R . . . .
C25 C 0.3722(6) -0.0596(6) -0.2418(7) 0.0576(17) Uani 1 1 d . U . . .
H25 H 0.395804 -0.010021 -0.205085 0.069 Uiso 1 1 calc R . . . .
C24 C 0.2924(6) -0.1969(6) -0.3584(9) 0.0635(19) Uani 1 1 d . U . . .
H24 H 0.261802 -0.242682 -0.401057 0.076 Uiso 1 1 calc R . . . .
O2 O -0.1247(5) 0.2968(4) 0.1345(6) 0.0741(19) Uani 1 1 d . . . . .
H10A H 0.309(8) 0.345(5) 0.508(6) 0.111 Uiso 1 1 d DR . . . .
H9B H 0.204(8) 0.0258(12) 0.364(6) 0.111 Uiso 1 1 d DR . . . .
H10B H 0.324(8) 0.376(3) 0.388(8) 0.111 Uiso 1 1 d DR . . . .


_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
N2 C26 1.275(11) . ?
N2 C24 1.352(11) . ?
C18 C17 1.512(7) . ?
C18 O7 1.249(7) . ?
C18 O8 1.258(6) . ?
C19 C17 1.400(7) . ?
C19 C20 1.392(8) . ?
C17 C16 1.396(7) . ?
C16 C15 1.400(7) . ?
Tb1 O4 2.343(4) . ?
Tb1 O5 2.445(4) . ?
Tb1 O6 2.512(4) . ?
Tb1 O7 2.325(4) 3_656 ?
Tb1 O3 2.285(4) 4_565 ?
Tb1 O8 2.316(4) 2_655 ?
Tb1 O9 2.388(4) . ?
Tb1 O10 2.518(4) . ?
O4 C13 1.252(6) . ?
O5 C14 1.254(7) . ?
O6 C14 1.279(6) . ?
C14 C15 1.495(7) . ?
C11 C13 1.516(8) . ?
C11 C10 1.388(8) . ?
C11 C12 1.390(7) . ?
C13 O3 1.258(7) . ?
C10 C8 1.400(8) . ?
C21 C15 1.405(7) . ?
C21 C20 1.389(7) . ?
O1 C9 1.309(9) . ?
C12 C6 1.404(7) . ?
C8 C7 1.391(8) . ?
C8 C9 1.510(9) . ?
C20 C22 1.488(7) . ?
C3 C6 1.489(8) . ?
C3 C4 1.403(8) . ?
C3 C2 1.373(9) . ?
C22 C23 1.378(10) . ?
C22 C25 1.402(10) . ?
C7 C6 1.391(8) . ?
C9 O2 1.202(9) . ?
C4 C5 1.379(9) . ?
N1 C1 1.327(9) . ?
N1 C5 1.318(9) . ?
C2 C1 1.389(9) . ?
C23 C24 1.449(11) . ?
C26 C25 1.354(10) . ?

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
C26 N2 C24 121.7(8) . . ?
O7 C18 C17 117.1(5) . . ?
O7 C18 O8 125.5(5) . . ?
O8 C18 C17 117.4(5) . . ?
C20 C19 C17 120.6(5) . . ?
C19 C17 C18 119.4(5) . . ?
C16 C17 C18 120.7(5) . . ?
C16 C17 C19 119.8(5) . . ?
C17 C16 C15 120.0(5) . . ?
O4 Tb1 O5 136.25(15) . . ?
O4 Tb1 O6 131.53(14) . . ?
O4 Tb1 O9 69.43(16) . . ?
O4 Tb1 O10 70.83(16) . . ?
O5 Tb1 O6 52.63(13) . . ?
O5 Tb1 O10 137.05(15) . . ?
O6 Tb1 O10 142.89(14) . . ?
O7 Tb1 O4 88.95(15) 3_656 . ?
O7 Tb1 O5 74.08(13) 3_656 . ?
O7 Tb1 O6 126.49(13) 3_656 . ?
O7 Tb1 O9 100.29(17) 3_656 . ?
O7 Tb1 O10 74.38(15) 3_656 . ?
O3 Tb1 O4 79.81(14) 4_565 . ?
O3 Tb1 O5 127.75(14) 4_565 . ?
O3 Tb1 O6 75.26(13) 4_565 . ?
O3 Tb1 O7 156.44(14) 4_565 3_656 ?
O3 Tb1 O8 82.87(14) 4_565 2_655 ?
O3 Tb1 O9 95.07(16) 4_565 . ?
O3 Tb1 O10 82.36(15) 4_565 . ?
O8 Tb1 O4 141.64(17) 2_655 . ?
O8 Tb1 O5 80.63(14) 2_655 . ?
O8 Tb1 O6 75.01(13) 2_655 . ?
O8 Tb1 O7 93.73(16) 2_655 3_656 ?
O8 Tb1 O9 146.50(15) 2_655 . ?
O8 Tb1 O10 73.12(15) 2_655 . ?
O9 Tb1 O5 74.33(16) . . ?
O9 Tb1 O6 72.17(14) . . ?
O9 Tb1 O10 139.98(15) . . ?
C13 O4 Tb1 153.3(4) . . ?
C14 O5 Tb1 95.4(3) . . ?
C14 O6 Tb1 91.5(3) . . ?
O5 C14 O6 120.4(5) . . ?
O5 C14 C15 119.9(5) . . ?
O6 C14 C15 119.6(5) . . ?
C10 C11 C13 121.0(5) . . ?
C10 C11 C12 119.9(5) . . ?
C12 C11 C13 119.1(5) . . ?
O4 C13 C11 118.1(5) . . ?
O4 C13 O3 123.8(5) . . ?
O3 C13 C11 118.1(5) . . ?
C11 C10 C8 119.5(5) . . ?
C20 C21 C15 120.6(5) . . ?
C11 C12 C6 120.8(5) . . ?
C16 C15 C14 121.0(5) . . ?
C16 C15 C21 119.5(5) . . ?
C21 C15 C14 119.4(5) . . ?
C10 C8 C9 118.9(6) . . ?
C7 C8 C10 120.5(6) . . ?
C7 C8 C9 120.6(6) . . ?
C19 C20 C22 121.0(5) . . ?
C21 C20 C19 119.5(5) . . ?
C21 C20 C22 119.4(5) . . ?
C4 C3 C6 121.7(5) . . ?
C2 C3 C6 121.2(5) . . ?
C2 C3 C4 117.1(5) . . ?
C23 C22 C20 123.1(6) . . ?
C23 C22 C25 117.4(6) . . ?
C25 C22 C20 119.5(6) . . ?
C8 C7 C6 120.2(5) . . ?
C12 C6 C3 119.6(5) . . ?
C7 C6 C12 119.0(5) . . ?
C7 C6 C3 121.3(5) . . ?
O1 C9 C8 114.8(6) . . ?
O2 C9 O1 123.3(7) . . ?
O2 C9 C8 121.8(7) . . ?
C5 C4 C3 119.0(6) . . ?
C18 O7 Tb1 156.2(4) . 3_656 ?
C13 O3 Tb1 148.8(4) . 4_566 ?
C18 O8 Tb1 148.3(4) . 2_645 ?
C5 N1 C1 116.8(6) . . ?
C3 C2 C1 119.2(6) . . ?
N1 C1 C2 123.9(7) . . ?
C22 C23 C24 117.2(8) . . ?
N1 C5 C4 124.1(6) . . ?
N2 C26 C25 121.0(9) . . ?
C26 C25 C22 122.1(8) . . ?
N2 C24 C23 120.2(8) . . ?

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
N2 C26 C25 C22 6.8(14) . . . . ?
C18 C17 C16 C15 174.7(5) . . . . ?
C19 C17 C16 C15 -1.2(8) . . . . ?
C19 C20 C22 C23 53.1(9) . . . . ?
C19 C20 C22 C25 -127.9(7) . . . . ?
C17 C18 O7 Tb1 -161.6(8) . . . 3_656 ?
C17 C18 O8 Tb1 95.9(7) . . . 2_645 ?
C17 C19 C20 C21 -1.8(9) . . . . ?
C17 C19 C20 C22 175.3(5) . . . . ?
C17 C16 C15 C14 -179.4(5) . . . . ?
C17 C16 C15 C21 -0.7(8) . . . . ?
Tb1 O4 C13 C11 142.3(7) . . . . ?
Tb1 O4 C13 O3 -38.3(12) . . . . ?
Tb1 O5 C14 O6 -0.9(6) . . . . ?
Tb1 O5 C14 C15 -179.3(4) . . . . ?
Tb1 O6 C14 O5 0.9(5) . . . . ?
Tb1 O6 C14 C15 179.3(4) . . . . ?
O4 C13 O3 Tb1 92.9(8) . . . 4_566 ?
O5 C14 C15 C16 5.7(8) . . . . ?
O5 C14 C15 C21 -173.0(5) . . . . ?
O6 C14 C15 C16 -172.7(5) . . . . ?
O6 C14 C15 C21 8.6(8) . . . . ?
C11 C13 O3 Tb1 -87.8(7) . . . 4_566 ?
C11 C10 C8 C7 0.6(9) . . . . ?
C11 C10 C8 C9 -177.3(6) . . . . ?
C11 C12 C6 C3 179.6(5) . . . . ?
C11 C12 C6 C7 1.3(9) . . . . ?
C13 C11 C10 C8 -179.2(5) . . . . ?
C13 C11 C12 C6 178.2(5) . . . . ?
C10 C11 C13 O4 7.2(8) . . . . ?
C10 C11 C13 O3 -172.2(5) . . . . ?
C10 C11 C12 C6 -3.2(8) . . . . ?
C10 C8 C7 C6 -2.5(9) . . . . ?
C10 C8 C9 O1 -172.9(6) . . . . ?
C10 C8 C9 O2 9.4(11) . . . . ?
C21 C20 C22 C23 -129.8(7) . . . . ?
C21 C20 C22 C25 49.2(8) . . . . ?
C12 C11 C13 O4 -174.3(5) . . . . ?
C12 C11 C13 O3 6.3(7) . . . . ?
C12 C11 C10 C8 2.3(8) . . . . ?
C15 C21 C20 C19 -0.1(9) . . . . ?
C15 C21 C20 C22 -177.3(5) . . . . ?
C8 C7 C6 C12 1.5(9) . . . . ?
C8 C7 C6 C3 -176.7(6) . . . . ?
C20 C19 C17 C18 -173.5(5) . . . . ?
C20 C19 C17 C16 2.4(8) . . . . ?
C20 C21 C15 C16 1.4(8) . . . . ?
C20 C21 C15 C14 -179.9(5) . . . . ?
C20 C22 C23 C24 175.7(6) . . . . ?
C20 C22 C25 C26 178.7(7) . . . . ?
C3 C4 C5 N1 -1.4(11) . . . . ?
C3 C2 C1 N1 1.3(13) . . . . ?
C22 C23 C24 N2 4.8(12) . . . . ?
C7 C8 C9 O1 9.1(10) . . . . ?
C7 C8 C9 O2 -168.5(8) . . . . ?
C6 C3 C4 C5 -178.8(6) . . . . ?
C6 C3 C2 C1 178.9(6) . . . . ?
C9 C8 C7 C6 175.4(6) . . . . ?
C4 C3 C6 C12 143.5(6) . . . . ?
C4 C3 C6 C7 -38.2(9) . . . . ?
C4 C3 C2 C1 -1.5(10) . . . . ?
O7 C18 C17 C19 177.2(5) . . . . ?
O7 C18 C17 C16 1.2(8) . . . . ?
O7 C18 O8 Tb1 -82.4(9) . . . 2_645 ?
O8 C18 C17 C19 -1.3(8) . . . . ?
O8 C18 C17 C16 -177.2(5) . . . . ?
O8 C18 O7 Tb1 16.8(15) . . . 3_656 ?
C2 C3 C6 C12 -36.9(9) . . . . ?
C2 C3 C6 C7 141.4(7) . . . . ?
C2 C3 C4 C5 1.6(10) . . . . ?
C1 N1 C5 C4 1.1(11) . . . . ?
C23 C22 C25 C26 -2.2(12) . . . . ?
C5 N1 C1 C2 -1.0(12) . . . . ?
C26 N2 C24 C23 -0.5(14) . . . . ?
C25 C22 C23 C24 -3.3(11) . . . . ?
C24 N2 C26 C25 -5.3(15) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_434343
_audit_block_doi                 10.5517/cc1j7mlz
_database_code_depnum_ccdc_archive 'CCDC 1407511'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H19 Dy N2 O10'
_chemical_formula_sum            'C26 H19 Dy N2 O10'
_chemical_formula_weight         681.93
_chemical_melting_point          ?
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'
Dy Dy -0.1892 4.4098 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.708(3)
_cell_length_b                   16.437(3)
_cell_length_c                   10.219(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.47(3)
_cell_angle_gamma                90
_cell_volume                     2392.1(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5790
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.190
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.893
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24280
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         3.048
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1657
	          2theta: 29.8527
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1657
	          2theta: 29.8527
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1657
	          2theta: 29.8527
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.044652
_diffrn_orient_matrix_UB_12      0.037262
_diffrn_orient_matrix_UB_13      0.082654
_diffrn_orient_matrix_UB_21      0.027506
_diffrn_orient_matrix_UB_22      0.042342
_diffrn_orient_matrix_UB_23      -0.033948
_diffrn_orient_matrix_UB_31      -0.044935
_diffrn_orient_matrix_UB_32      0.048369
_diffrn_orient_matrix_UB_33      0.023921
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4595
_reflns_number_total             5480
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.781
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5480
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0435
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²+2.1087P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1018
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H,H,H) groups
2. Restrained distances
 O9-H9A
 0.85 with sigma of 0.01
 H10B-O10
 0.85 with sigma of 0.01
 H10A-O10
 0.85 with sigma of 0.01
 H10B-H10A
 1.39 with sigma of 0.01
 H9B-H9A
 1.39 with sigma of 0.01
 O9-H9B
 0.85 with sigma of 0.01
3. Rigid bond restraints
 N2, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Rotating group:
 O10(H10A)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C16(H16), C20(H20), C11(H11), C18(H18), C25(H25), C24(H24),
 C26(H26), C23(H23), C2(H2), C4(H4), C1(H1), C5(H5)
4.c Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C7 C 0.3637(4) 0.4585(3) 0.5522(5) 0.0248(11) Uani 1 1 d . . . . .
H7 H 0.322286 0.494744 0.497969 0.030 Uiso 1 1 calc R . . . .
C8 C 0.3956(4) 0.4730(3) 0.6911(5) 0.0220(11) Uani 1 1 d . . . . .
O7 O 0.8050(2) 0.2577(2) 0.3126(4) 0.0241(8) Uani 1 1 d . . . . .
Dy1 Dy 0.70032(2) 0.18689(2) 0.63314(2) 0.01789(8) Uani 1 1 d . . . . .
O4 O 0.5918(3) 0.2380(2) 0.7410(4) 0.0267(8) Uani 1 1 d . . . . .
O8 O 0.8164(3) 0.2281(3) 0.5292(4) 0.0359(10) Uani 1 1 d . . . . .
C15 C 0.9374(4) 0.3076(3) 0.4766(5) 0.0226(11) Uani 1 1 d . . . . .
C10 C 0.4896(4) 0.3520(3) 0.7162(5) 0.0208(10) Uani 1 1 d . . . . .
C13 C 0.5649(4) 0.2966(3) 0.8000(5) 0.0223(11) Uani 1 1 d . . . . .
C14 C 0.8458(4) 0.2615(3) 0.4369(5) 0.0204(10) Uani 1 1 d . . . . .
C9 C 0.4585(4) 0.4199(3) 0.7728(5) 0.0242(11) Uani 1 1 d . . . . .
H9 H 0.479737 0.429841 0.865009 0.029 Uiso 1 1 calc R . . . .
C16 C 0.9928(4) 0.3062(3) 0.6093(5) 0.0246(11) Uani 1 1 d . . . . .
H16 H 0.974301 0.275769 0.674895 0.030 Uiso 1 1 calc R . . . .
C20 C 0.9671(4) 0.3522(3) 0.3788(5) 0.0243(11) Uani 1 1 d . . . . .
H20 H 0.931269 0.351458 0.289867 0.029 Uiso 1 1 calc R . . . .
C11 C 0.4555(4) 0.3361(3) 0.5775(5) 0.0250(11) Uani 1 1 d . . . . .
H11 H 0.474573 0.289287 0.540712 0.030 Uiso 1 1 calc R . . . .
C22 C 1.0812(4) 0.4442(3) 0.3059(6) 0.0273(11) Uani 1 1 d . . . . .
C3 C 0.3631(4) 0.3769(4) 0.3450(6) 0.0309(13) Uani 1 1 d . . . . .
C18 C 1.1042(4) 0.3967(4) 0.5458(6) 0.0309(13) Uani 1 1 d . . . . .
H18 H 1.159276 0.426961 0.569601 0.037 Uiso 1 1 calc R . . . .
O6 O 1.1231(4) 0.2957(3) 0.8656(5) 0.0715(18) Uani 1 1 d . . . . .
C17 C 1.0763(4) 0.3509(3) 0.6426(5) 0.0287(12) Uani 1 1 d . . . . .
N1 N 1.1360(4) 0.5308(3) 0.1020(6) 0.0428(13) Uani 1 1 d . . . . .
C6 C 0.3940(4) 0.3893(3) 0.4948(5) 0.0247(11) Uani 1 1 d . . . . .
C19 C 1.0496(4) 0.3977(3) 0.4121(5) 0.0248(11) Uani 1 1 d . . . . .
C25 C 1.0964(5) 0.4578(4) 0.0791(7) 0.0488(18) Uani 1 1 d . . . . .
H25 H 1.087866 0.435552 -0.006790 0.059 Uiso 1 1 calc R . . . .
C21 C 1.1380(5) 0.3450(4) 0.7839(6) 0.0436(16) Uani 1 1 d . . . . .
C24 C 1.1488(5) 0.5605(4) 0.2261(7) 0.0451(16) Uani 1 1 d . . . . .
H24 H 1.176022 0.611736 0.243782 0.054 Uiso 1 1 calc R . . . .
C26 C 1.0673(5) 0.4132(4) 0.1752(6) 0.0430(16) Uani 1 1 d . . . . .
H26 H 1.038730 0.362842 0.153237 0.052 Uiso 1 1 calc R . . . .
C23 C 1.1239(4) 0.5199(4) 0.3304(6) 0.0368(14) Uani 1 1 d . . . . .
H23 H 1.135685 0.543016 0.416074 0.044 Uiso 1 1 calc R . . . .
O2 O 0.3966(3) 0.5662(2) 0.8713(4) 0.0298(9) Uani 1 1 d . . . . .
O3 O 0.5954(3) 0.3143(2) 0.9231(4) 0.0353(10) Uani 1 1 d . . . . .
O1 O 0.2964(3) 0.5906(2) 0.6751(4) 0.0254(8) Uani 1 1 d . . . . .
O10 O 0.7978(3) 0.0748(2) 0.6111(4) 0.0374(10) Uani 1 1 d D . . . .
H10A H 0.809613 0.075118 0.531377 0.056 Uiso 1 1 d DGR . . . .
O9 O 0.6758(3) 0.3342(3) 0.5648(4) 0.0363(10) Uani 1 1 d D . . . .
C12 C 0.3614(4) 0.5476(3) 0.7492(5) 0.0232(11) Uani 1 1 d . . . . .
C2 C 0.3255(5) 0.3044(5) 0.2882(7) 0.0513(19) Uani 1 1 d . . . . .
H2 H 0.321266 0.258978 0.340538 0.062 Uiso 1 1 calc R . . . .
N2 N 0.3058(5) 0.3664(5) 0.0655(6) 0.0644(19) Uani 1 1 d . U . . .
C4 C 0.3725(5) 0.4402(5) 0.2580(6) 0.0540(19) Uani 1 1 d . . . . .
H4 H 0.397092 0.489693 0.294678 0.065 Uiso 1 1 calc R . . . .
C1 C 0.2928(6) 0.3031(5) 0.1416(8) 0.062(2) Uani 1 1 d . U . . .
H1 H 0.262035 0.257070 0.099454 0.075 Uiso 1 1 calc R . . . .
C5 C 0.3470(7) 0.4317(6) 0.1222(8) 0.071(2) Uani 1 1 d . . . . .
H5 H 0.359323 0.473661 0.068137 0.086 Uiso 1 1 calc R . . . .
O5 O 1.2088(3) 0.3949(3) 0.8118(5) 0.0570(14) Uani 1 1 d . . . . .
H5A H 1.238258 0.388634 0.890608 0.086 Uiso 1 1 calc GR . . . .
H9A H 0.689(5) 0.353(5) 0.494(4) 0.086 Uiso 1 1 d DR . . . .
H10B H 0.794(6) 0.0258(11) 0.634(5) 0.086 Uiso 1 1 d DR . . . .
H9B H 0.6166(11) 0.330(5) 0.551(7) 0.086 Uiso 1 1 d DR . . . .


_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
C7 C8 1.399(7) . ?
C7 C6 1.402(7) . ?
C8 C9 1.389(7) . ?
C8 C12 1.503(7) . ?
O7 Dy1 2.269(3) 4_565 ?
O7 C14 1.264(6) . ?
Dy1 O4 2.312(4) . ?
Dy1 O8 2.326(4) . ?
Dy1 O2 2.436(4) 2_646 ?
Dy1 O3 2.310(4) 4_565 ?
Dy1 O1 2.510(4) 2_646 ?
Dy1 O10 2.379(4) . ?
Dy1 O9 2.520(4) . ?
Dy1 C12 2.838(5) 2_646 ?
O4 C13 1.251(6) . ?
O8 C14 1.258(6) . ?
C15 C14 1.510(7) . ?
C15 C16 1.397(7) . ?
C15 C20 1.394(7) . ?
C10 C13 1.522(7) . ?
C10 C9 1.386(7) . ?
C10 C11 1.405(7) . ?
C13 O3 1.260(6) . ?
C16 C17 1.399(7) . ?
C20 C19 1.393(7) . ?
C11 C6 1.384(7) . ?
C22 C19 1.493(7) . ?
C22 C26 1.396(8) . ?
C22 C23 1.388(8) . ?
C3 C6 1.498(7) . ?
C3 C2 1.379(9) . ?
C3 C4 1.399(9) . ?
C18 C17 1.384(8) . ?
C18 C19 1.401(7) . ?
O6 C21 1.222(8) . ?
C17 C21 1.504(8) . ?
N1 C25 1.328(8) . ?
N1 C24 1.328(8) . ?
C25 C26 1.376(8) . ?
C21 O5 1.300(8) . ?
C24 C23 1.383(8) . ?
O2 C12 1.263(6) . ?
O1 C12 1.274(6) . ?
C2 C1 1.454(10) . ?
N2 C1 1.341(10) . ?
N2 C5 1.295(11) . ?
C4 C5 1.351(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 C7 C6 120.1(5) . . ?
C7 C8 C12 118.6(4) . . ?
C9 C8 C7 120.4(5) . . ?
C9 C8 C12 120.9(5) . . ?
C14 O7 Dy1 148.0(3) . 4_565 ?
O7 Dy1 O4 83.02(13) 4_566 . ?
O7 Dy1 O8 79.93(14) 4_566 . ?
O7 Dy1 O2 128.11(13) 4_566 2_646 ?
O7 Dy1 O3 156.23(13) 4_566 4_565 ?
O7 Dy1 O1 75.26(12) 4_566 2_646 ?
O7 Dy1 O10 94.83(15) 4_566 . ?
O7 Dy1 O9 81.94(14) 4_566 . ?
O7 Dy1 C12 101.86(14) 4_566 2_646 ?
O4 Dy1 O8 141.73(15) . . ?
O4 Dy1 O2 80.47(13) . 2_646 ?
O4 Dy1 O1 74.78(12) . 2_646 ?
O4 Dy1 O10 146.11(14) . . ?
O4 Dy1 O9 73.46(14) . . ?
O4 Dy1 C12 76.07(14) . 2_646 ?
O8 Dy1 O2 136.15(14) . 2_646 ?
O8 Dy1 O1 131.85(14) . 2_646 ?
O8 Dy1 O10 69.74(15) . . ?
O8 Dy1 O9 70.40(15) . . ?
O8 Dy1 C12 141.00(15) . 2_646 ?
O2 Dy1 O1 52.99(12) 2_646 2_646 ?
O2 Dy1 O9 137.24(14) 2_646 . ?
O2 Dy1 C12 26.32(13) 2_646 2_646 ?
O3 Dy1 O4 93.77(15) 4_565 . ?
O3 Dy1 O8 88.53(14) 4_565 . ?
O3 Dy1 O2 73.96(13) 4_565 2_646 ?
O3 Dy1 O1 126.73(12) 4_565 2_646 ?
O3 Dy1 O10 100.59(16) 4_565 . ?
O3 Dy1 O9 74.60(14) 4_565 . ?
O3 Dy1 C12 100.17(14) 4_565 2_646 ?
O1 Dy1 O9 142.71(13) 2_646 . ?
O1 Dy1 C12 26.67(13) 2_646 2_646 ?
O10 Dy1 O2 74.40(15) . 2_646 ?
O10 Dy1 O1 72.01(13) . 2_646 ?
O10 Dy1 O9 139.96(15) . . ?
O10 Dy1 C12 71.29(15) . 2_646 ?
O9 Dy1 C12 148.58(15) . 2_646 ?
C13 O4 Dy1 148.0(4) . . ?
C14 O8 Dy1 154.0(4) . . ?
C16 C15 C14 121.1(5) . . ?
C20 C15 C14 119.3(5) . . ?
C20 C15 C16 119.6(5) . . ?
C9 C10 C13 121.1(4) . . ?
C9 C10 C11 120.0(5) . . ?
C11 C10 C13 118.8(4) . . ?
O4 C13 C10 117.6(4) . . ?
O4 C13 O3 125.6(5) . . ?
O3 C13 C10 116.8(5) . . ?
O7 C14 C15 117.6(4) . . ?
O8 C14 O7 124.4(5) . . ?
O8 C14 C15 118.0(5) . . ?
C10 C9 C8 119.6(5) . . ?
C15 C16 C17 119.4(5) . . ?
C19 C20 C15 121.1(5) . . ?
C6 C11 C10 120.8(5) . . ?
C26 C22 C19 120.8(5) . . ?
C23 C22 C19 122.4(5) . . ?
C23 C22 C26 116.8(5) . . ?
C2 C3 C6 122.4(6) . . ?
C2 C3 C4 117.9(6) . . ?
C4 C3 C6 119.7(6) . . ?
C17 C18 C19 120.2(5) . . ?
C16 C17 C21 118.8(5) . . ?
C18 C17 C16 120.7(5) . . ?
C18 C17 C21 120.4(5) . . ?
C24 N1 C25 116.9(5) . . ?
C7 C6 C3 119.4(5) . . ?
C11 C6 C7 119.0(5) . . ?
C11 C6 C3 121.5(5) . . ?
C20 C19 C22 120.5(5) . . ?
C20 C19 C18 118.9(5) . . ?
C18 C19 C22 120.5(5) . . ?
N1 C25 C26 123.8(6) . . ?
O6 C21 C17 122.0(6) . . ?
O6 C21 O5 122.7(6) . . ?
O5 C21 C17 115.3(6) . . ?
N1 C24 C23 123.8(6) . . ?
C25 C26 C22 119.4(6) . . ?
C24 C23 C22 119.3(6) . . ?
C12 O2 Dy1 94.9(3) . 2_656 ?
C13 O3 Dy1 156.1(4) . 4_566 ?
C12 O1 Dy1 91.2(3) . 2_656 ?
C8 C12 Dy1 178.3(4) . 2_656 ?
O2 C12 C8 119.5(5) . . ?
O2 C12 Dy1 58.8(3) . 2_656 ?
O2 C12 O1 120.9(5) . . ?
O1 C12 C8 119.5(4) . . ?
O1 C12 Dy1 62.1(3) . 2_656 ?
C3 C2 C1 116.2(7) . . ?
C5 N2 C1 120.1(7) . . ?
C5 C4 C3 122.0(8) . . ?
N2 C1 C2 121.8(7) . . ?
N2 C5 C4 121.6(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 C8 C9 C10 -0.2(8) . . . . ?
C7 C8 C12 O2 -172.8(5) . . . . ?
C7 C8 C12 O1 8.1(7) . . . . ?
C8 C7 C6 C11 0.1(8) . . . . ?
C8 C7 C6 C3 -176.9(5) . . . . ?
Dy1 O7 C14 O8 91.4(8) 4_565 . . . ?
Dy1 O7 C14 C15 -90.3(7) 4_565 . . . ?
Dy1 O4 C13 C10 95.9(7) . . . . ?
Dy1 O4 C13 O3 -83.4(8) . . . . ?
Dy1 O8 C14 O7 -38.7(12) . . . . ?
Dy1 O8 C14 C15 143.1(7) . . . . ?
Dy1 O2 C12 C8 -179.6(4) 2_656 . . . ?
Dy1 O2 C12 O1 -0.5(5) 2_656 . . . ?
Dy1 O1 C12 C8 179.6(4) 2_656 . . . ?
Dy1 O1 C12 O2 0.5(5) 2_656 . . . ?
O4 C13 O3 Dy1 19.3(13) . . . 4_566 ?
C15 C16 C17 C18 0.4(9) . . . . ?
C15 C16 C17 C21 -176.5(5) . . . . ?
C15 C20 C19 C22 179.1(5) . . . . ?
C15 C20 C19 C18 1.6(8) . . . . ?
C10 C13 O3 Dy1 -160.0(7) . . . 4_566 ?
C10 C11 C6 C7 -1.9(8) . . . . ?
C10 C11 C6 C3 175.0(5) . . . . ?
C13 C10 C9 C8 174.6(5) . . . . ?
C13 C10 C11 C6 -173.6(5) . . . . ?
C14 C15 C16 C17 -178.8(5) . . . . ?
C14 C15 C20 C19 177.8(5) . . . . ?
C9 C8 C12 O2 6.4(8) . . . . ?
C9 C8 C12 O1 -172.7(5) . . . . ?
C9 C10 C13 O4 -177.6(5) . . . . ?
C9 C10 C13 O3 1.8(8) . . . . ?
C9 C10 C11 C6 2.7(8) . . . . ?
C16 C15 C14 O7 -171.9(5) . . . . ?
C16 C15 C14 O8 6.5(8) . . . . ?
C16 C15 C20 C19 -2.3(8) . . . . ?
C16 C17 C21 O6 8.5(10) . . . . ?
C16 C17 C21 O5 -172.6(6) . . . . ?
C20 C15 C14 O7 8.1(7) . . . . ?
C20 C15 C14 O8 -173.6(5) . . . . ?
C20 C15 C16 C17 1.3(8) . . . . ?
C11 C10 C13 O4 -1.3(8) . . . . ?
C11 C10 C13 O3 178.0(5) . . . . ?
C11 C10 C9 C8 -1.6(8) . . . . ?
C3 C2 C1 N2 5.5(12) . . . . ?
C3 C4 C5 N2 5.4(14) . . . . ?
C18 C17 C21 O6 -168.5(7) . . . . ?
C18 C17 C21 O5 10.4(9) . . . . ?
C17 C18 C19 C20 0.2(9) . . . . ?
C17 C18 C19 C22 -177.4(5) . . . . ?
N1 C25 C26 C22 -1.4(12) . . . . ?
N1 C24 C23 C22 -1.4(11) . . . . ?
C6 C7 C8 C9 1.0(8) . . . . ?
C6 C7 C8 C12 -179.8(5) . . . . ?
C6 C3 C2 C1 176.0(6) . . . . ?
C6 C3 C4 C5 179.0(7) . . . . ?
C19 C22 C26 C25 179.3(6) . . . . ?
C19 C22 C23 C24 -178.0(6) . . . . ?
C19 C18 C17 C16 -1.1(9) . . . . ?
C19 C18 C17 C21 175.8(6) . . . . ?
C25 N1 C24 C23 0.4(11) . . . . ?
C24 N1 C25 C26 1.0(11) . . . . ?
C26 C22 C19 C20 -35.9(8) . . . . ?
C26 C22 C19 C18 141.6(6) . . . . ?
C26 C22 C23 C24 1.0(9) . . . . ?
C23 C22 C19 C20 143.0(6) . . . . ?
C23 C22 C19 C18 -39.5(8) . . . . ?
C23 C22 C26 C25 0.3(10) . . . . ?
C12 C8 C9 C10 -179.4(5) . . . . ?
C2 C3 C6 C7 -130.5(6) . . . . ?
C2 C3 C6 C11 52.6(8) . . . . ?
C2 C3 C4 C5 -0.7(11) . . . . ?
C4 C3 C6 C7 49.9(8) . . . . ?
C4 C3 C6 C11 -127.0(7) . . . . ?
C4 C3 C2 C1 -4.3(10) . . . . ?
C1 N2 C5 C4 -4.3(14) . . . . ?
C5 N2 C1 C2 -1.2(13) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelxl_CCDC3
_audit_block_doi                 10.5517/cc1j7mp2
_database_code_depnum_ccdc_archive 'CCDC 1407514'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H39 Gd4 N O29, C3 H7 N O, 1.5(H2 O)'
_chemical_formula_sum            'C54 H49 Gd4 N2 O31.50'
_chemical_formula_weight         1858.95
_chemical_melting_point          ?
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'
Gd Gd -0.1653 3.9035 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.850(2)
_cell_length_b                   14.180(3)
_cell_length_c                   20.180(4)
_cell_angle_alpha                86.61(3)
_cell_angle_beta                 83.77(3)
_cell_angle_gamma                78.89(3)
_cell_volume                     3026.3(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8612
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.422
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1790
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1161
_diffrn_reflns_av_unetI/netI     0.1074
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31061
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         3.049
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1500
	          2theta: 29.8760
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1500
	          2theta: 29.8760
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1500
	          2theta: 29.8760
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.056897
_diffrn_orient_matrix_UB_12      0.028318
_diffrn_orient_matrix_UB_13      0.069706
_diffrn_orient_matrix_UB_21      -0.009324
_diffrn_orient_matrix_UB_22      0.061682
_diffrn_orient_matrix_UB_23      -0.035708
_diffrn_orient_matrix_UB_31      -0.042438
_diffrn_orient_matrix_UB_32      0.006069
_diffrn_orient_matrix_UB_33      0.025489
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12220
_reflns_number_total             13814
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.764
_refine_diff_density_min         -1.530
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         13814
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0424
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0272P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1112
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H31A,H31B} of O31, {H28A,H28B} of O28, {H25A,H25B} of O25,
   {H26A,H26B} of O26, {H27A,H27B} of O27
 At 1.5 times of:
  All C(H,H,H) groups, {H1AA,H1AB} of O1A
2. Restrained distances
 H27B-H1AA
 2.2 with sigma of 0.01
 H1AA-H27A
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C51 \\sim N2 \\sim C52 \\sim C50 \\sim O30: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: O1A(0.5) H1AA(0.5) H1AB(0.5)
5.a Riding coordinates:
 O25(H25A,H25B), O26(H26A,H26B), O27(H27A,H27B), O28(H28A,H28B), O31(H31A,H31B)
5.b Free rotating group:
 O1A(H1AA,H1AB)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13), C15(H15),
 C19(H19), C20(H20), C21(H21), C23(H23), C27(H27), C28(H28), C29(H29), C31(H31),
  C34(H34), C35(H35), C37(H37), C41(H41), C43(H43), C44(H44), C45(H45),
 C47(H47), C110(H110), C50(H50)
5.d Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.41396(2) 0.73305(2) 0.19791(2) 0.01864(7) Uani 1 1 d . . . . .
Gd2 Gd 0.78885(2) 0.94529(2) 0.17389(2) 0.01754(7) Uani 1 1 d . . . . .
Gd3 Gd 0.22915(2) 0.80716(2) 0.69112(2) 0.01758(7) Uani 1 1 d . . . . .
Gd4 Gd 0.45494(2) 0.48765(2) 0.35235(2) 0.02180(7) Uani 1 1 d . . . . .
O1 O 0.0830(4) 0.8485(4) 0.60672(19) 0.0425(11) Uani 1 1 d . . . . .
O2 O 0.2465(4) 0.7379(3) 0.58083(19) 0.0379(10) Uani 1 1 d . . . . .
O3 O 0.2665(4) 0.5986(3) 0.34599(19) 0.0306(8) Uani 1 1 d . . . . .
O4 O 0.2402(3) 0.7192(3) 0.27022(18) 0.0289(8) Uani 1 1 d . . . . .
O5 O 0.3621(4) 1.3514(3) 0.3484(3) 0.0503(12) Uani 1 1 d . . . . .
O6 O 0.5543(4) 1.2692(3) 0.3235(2) 0.0314(9) Uani 1 1 d . . . . .
O7 O 0.5722(4) 0.9660(3) 0.2031(2) 0.0338(9) Uani 1 1 d . . . . .
O8 O 0.4236(4) 0.8799(3) 0.2328(2) 0.0342(9) Uani 1 1 d . . . . .
O9 O 0.7019(5) 1.0643(3) 0.3678(2) 0.0450(12) Uani 1 1 d . . . . .
O10 O 0.7707(4) 0.9591(4) 0.2883(2) 0.0460(12) Uani 1 1 d . . . . .
O11 O 0.5033(4) 0.6873(3) 0.3038(2) 0.0324(9) Uani 1 1 d . . . . .
O12 O 0.4931(4) 0.6201(2) 0.4063(2) 0.0314(9) Uani 1 1 d . . . . .
O13 O 0.7099(4) 0.1614(3) 0.20597(18) 0.0292(8) Uani 1 1 d . . . . .
O14 O 0.7077(4) 0.0920(3) 0.11085(19) 0.0342(9) Uani 1 1 d . . . . .
O15 O 0.4112(4) 0.5869(3) 0.1480(2) 0.0355(9) Uani 1 1 d . . . . .
O16 O 0.4542(5) 0.4944(4) 0.2389(2) 0.0514(13) Uani 1 1 d . . . . .
O17 O 0.9604(4) 1.1353(3) 0.24815(18) 0.0310(9) Uani 1 1 d . . . . .
O18 O 0.9586(4) 1.0197(3) 0.17861(19) 0.0293(8) Uani 1 1 d . . . . .
O19 O 0.8933(4) 0.9211(3) 0.05929(19) 0.0318(9) Uani 1 1 d . . . . .
O20 O 0.7128(4) 0.8728(4) 0.07962(19) 0.0418(11) Uani 1 1 d . . . . .
O21 O 0.6706(4) 0.4745(3) 0.3118(2) 0.0366(9) Uani 1 1 d . . . . .
O22 O 0.8011(4) 0.3440(3) 0.2759(2) 0.0421(11) Uani 1 1 d . . . . .
O23 O 0.9707(3) 0.8015(3) 0.1933(2) 0.0307(9) Uani 1 1 d . . . . .
O24 O 0.7755(4) 0.7800(3) 0.2077(2) 0.0317(9) Uani 1 1 d . . . . .
O25 O 0.5693(4) 0.4104(3) 0.4420(2) 0.0339(9) Uani 1 1 d . . . . .
H25A H 0.607688 0.442444 0.464376 0.041 Uiso 1 1 d R . . . .
H25B H 0.571548 0.350884 0.451356 0.041 Uiso 1 1 d R . . . .
O26 O 0.2272(4) 0.7939(3) 0.1447(2) 0.0380(10) Uani 1 1 d . . . . .
H26A H 0.231634 0.826156 0.107873 0.046 Uiso 1 1 d R . . . .
H26B H 0.156324 0.783246 0.162443 0.046 Uiso 1 1 d R . . . .
O27 O 0.4680(4) 0.8224(3) 0.09327(19) 0.0411(11) Uani 1 1 d . . . . .
H27A H 0.534917 0.845973 0.088445 0.049 Uiso 1 1 d DR . . . .
H27B H 0.419937 0.829333 0.062075 0.049 Uiso 1 1 d DR . . . .
O28 O 0.6264(4) 0.6776(3) 0.1607(2) 0.0387(10) Uani 1 1 d . . . . .
H28A H 0.659085 0.701517 0.124990 0.046 Uiso 1 1 d R . . . .
H28B H 0.670745 0.633437 0.182960 0.046 Uiso 1 1 d R . . . .
O29 O 0.3144(4) 0.4829(3) 0.4582(2) 0.0420(10) Uani 1 1 d . . . . .
N1 N 0.1731(6) 0.4230(5) 0.5325(4) 0.064(2) Uani 1 1 d . . . . .
C1 C 0.1489(5) 0.7950(4) 0.5642(3) 0.0265(11) Uani 1 1 d . . . . .
C2 C 0.1170(5) 0.8015(4) 0.4934(3) 0.0234(10) Uani 1 1 d . . . . .
C3 C 0.0221(5) 0.8779(4) 0.4747(3) 0.0326(12) Uani 1 1 d . . . . .
H3 H -0.024595 0.918159 0.506879 0.039 Uiso 1 1 calc R . . . .
C4 C -0.0018(6) 0.8934(5) 0.4084(3) 0.0383(14) Uani 1 1 d . . . . .
H4 H -0.061355 0.945918 0.395775 0.046 Uiso 1 1 calc R . . . .
C5 C 0.0627(5) 0.8307(4) 0.3610(3) 0.0309(12) Uani 1 1 d . . . . .
H5 H 0.046846 0.841212 0.316576 0.037 Uiso 1 1 calc R . . . .
C6 C 0.1521(5) 0.7513(4) 0.3799(2) 0.0221(10) Uani 1 1 d . . . . .
C7 C 0.1798(5) 0.7374(4) 0.4462(3) 0.0240(10) Uani 1 1 d . . . . .
H7 H 0.240279 0.685372 0.458678 0.029 Uiso 1 1 calc R . . . .
C8 C 0.2241(4) 0.6840(4) 0.3287(2) 0.0213(10) Uani 1 1 d . . . . .
C9 C 0.4368(5) 1.2757(4) 0.3322(3) 0.0273(11) Uani 1 1 d . . . . .
C10 C 0.3797(5) 1.1889(4) 0.3227(3) 0.0266(11) Uani 1 1 d . . . . .
C11 C 0.2598(6) 1.1821(5) 0.3532(3) 0.0402(15) Uani 1 1 d . . . . .
H11 H 0.213057 1.232467 0.377928 0.048 Uiso 1 1 calc R . . . .
C12 C 0.2105(6) 1.1008(5) 0.3467(4) 0.0442(16) Uani 1 1 d . . . . .
H12 H 0.131596 1.095899 0.368300 0.053 Uiso 1 1 calc R . . . .
C13 C 0.2782(6) 1.0257(4) 0.3080(3) 0.0381(14) Uani 1 1 d . . . . .
H13 H 0.243953 0.971523 0.303056 0.046 Uiso 1 1 calc R . . . .
C14 C 0.3968(5) 1.0326(4) 0.2769(3) 0.0232(10) Uani 1 1 d . . . . .
C15 C 0.4476(5) 1.1143(3) 0.2840(3) 0.0234(10) Uani 1 1 d . . . . .
H15 H 0.526896 1.118950 0.262825 0.028 Uiso 1 1 calc R . . . .
C16 C 0.4686(5) 0.9552(4) 0.2347(2) 0.0230(10) Uani 1 1 d . . . . .
C17 C 0.7115(5) 0.9833(4) 0.3439(3) 0.0272(12) Uani 1 1 d . . . . .
C18 C 0.6486(5) 0.9119(3) 0.3852(2) 0.0217(10) Uani 1 1 d . . . . .
C19 C 0.6193(6) 0.9246(4) 0.4539(3) 0.0338(13) Uani 1 1 d . . . . .
H19 H 0.644148 0.974483 0.473795 0.041 Uiso 1 1 calc R . . . .
C20 C 0.5528(7) 0.8623(4) 0.4923(3) 0.0419(16) Uani 1 1 d . . . . .
H20 H 0.531709 0.871607 0.537673 0.050 Uiso 1 1 calc R . . . .
C21 C 0.5178(6) 0.7865(4) 0.4630(3) 0.0348(14) Uani 1 1 d . . . . .
H21 H 0.474187 0.744675 0.488763 0.042 Uiso 1 1 calc R . . . .
C22 C 0.5487(5) 0.7734(4) 0.3944(3) 0.0225(10) Uani 1 1 d . . . . .
C23 C 0.6133(5) 0.8351(4) 0.3564(2) 0.0215(10) Uani 1 1 d . . . . .
H23 H 0.633925 0.825617 0.311015 0.026 Uiso 1 1 calc R . . . .
C24 C 0.5113(5) 0.6886(3) 0.3651(3) 0.0228(10) Uani 1 1 d . . . . .
C25 C 0.4500(5) 0.5064(4) 0.1769(3) 0.0293(12) Uani 1 1 d . . . . .
C26 C 0.4930(5) 0.4202(3) 0.1346(2) 0.0205(10) Uani 1 1 d . . . . .
C27 C 0.4653(5) 0.4268(4) 0.0680(3) 0.0277(11) Uani 1 1 d . . . . .
H27 H 0.419651 0.483625 0.050727 0.033 Uiso 1 1 calc R . . . .
C28 C 0.5061(6) 0.3483(4) 0.0278(3) 0.0296(12) Uani 1 1 d . . . . .
H28 H 0.487204 0.352251 -0.016281 0.036 Uiso 1 1 calc R . . . .
C29 C 0.5760(5) 0.2632(4) 0.0538(3) 0.0255(11) Uani 1 1 d . . . . .
H29 H 0.603113 0.210547 0.027068 0.031 Uiso 1 1 calc R . . . .
C30 C 0.6049(5) 0.2574(3) 0.1197(2) 0.0213(10) Uani 1 1 d . . . . .
C31 C 0.5620(5) 0.3351(3) 0.1601(2) 0.0222(10) Uani 1 1 d . . . . .
H31 H 0.579427 0.330453 0.204431 0.027 Uiso 1 1 calc R . . . .
C32 C 0.9968(5) 1.0920(4) 0.1946(2) 0.0240(10) Uani 1 1 d . . . . .
C33 C 1.0932(5) 1.1294(4) 0.1459(3) 0.0249(11) Uani 1 1 d . . . . .
C34 C 1.1664(6) 1.1916(4) 0.1649(3) 0.0341(13) Uani 1 1 d . . . . .
H34 H 1.159282 1.209504 0.208936 0.041 Uiso 1 1 calc R . . . .
C35 C 1.2499(7) 1.2263(6) 0.1176(3) 0.052(2) Uani 1 1 d . . . . .
H35 H 1.301705 1.265491 0.130692 0.063 Uiso 1 1 calc R . . . .
C36 C 1.1842(6) 1.1426(4) 0.0319(3) 0.0302(12) Uani 1 1 d . . . . .
C37 C 1.1025(5) 1.1045(4) 0.0798(2) 0.0234(10) Uani 1 1 d . . . . .
H37 H 1.054076 1.062263 0.067356 0.028 Uiso 1 1 calc R . . . .
C38 C 0.8055(5) 0.8842(4) 0.0392(3) 0.0263(11) Uani 1 1 d . . . . .
C39 C 0.7729(5) 0.4326(4) 0.2858(3) 0.0267(11) Uani 1 1 d . . . . .
C40 C 0.8750(5) 0.4896(4) 0.2619(3) 0.0282(11) Uani 1 1 d . . . . .
C41 C 0.8427(5) 0.5889(3) 0.2516(3) 0.0231(10) Uani 1 1 d . . . . .
H41 H 0.759914 0.620003 0.262453 0.028 Uiso 1 1 calc R . . . .
C42 C 0.9338(5) 0.6423(3) 0.2251(3) 0.0240(10) Uani 1 1 d . . . . .
C43 C 1.0578(6) 0.5952(4) 0.2125(4) 0.0400(15) Uani 1 1 d . . . . .
H43 H 1.119655 0.630059 0.196187 0.048 Uiso 1 1 calc R . . . .
C44 C 1.0905(6) 0.4969(5) 0.2240(4) 0.0506(19) Uani 1 1 d . . . . .
H44 H 1.174276 0.466322 0.216067 0.061 Uiso 1 1 calc R . . . .
C45 C 0.9991(6) 0.4438(4) 0.2473(4) 0.0458(17) Uani 1 1 d . . . . .
H45 H 1.020954 0.377320 0.253171 0.055 Uiso 1 1 calc R . . . .
C46 C 0.8936(5) 0.7467(4) 0.2081(3) 0.0227(10) Uani 1 1 d . . . . .
C47 C 0.2666(8) 0.4223(7) 0.4893(4) 0.062(2) Uani 1 1 d . . . . .
H47 H 0.308050 0.360319 0.479261 0.075 Uiso 1 1 calc R . . . .
C48 C 0.1145(11) 0.5210(9) 0.5603(6) 0.096(3) Uani 1 1 d . . . . .
H48A H 0.174418 0.563176 0.552572 0.143 Uiso 1 1 calc GR . . . .
H48B H 0.091550 0.513791 0.607387 0.143 Uiso 1 1 calc GR . . . .
H48C H 0.040516 0.547832 0.538486 0.143 Uiso 1 1 calc GR . . . .
C49 C 0.1257(11) 0.3473(9) 0.5690(6) 0.106(4) Uani 1 1 d . . . . .
H49A H 0.153199 0.288874 0.545503 0.160 Uiso 1 1 calc GR . . . .
H49B H 0.035119 0.362421 0.574087 0.160 Uiso 1 1 calc GR . . . .
H49C H 0.156531 0.339289 0.612189 0.160 Uiso 1 1 calc GR . . . .
C54 C 0.6799(5) 0.1649(4) 0.1465(3) 0.0227(10) Uani 1 1 d . . . . .
C110 C 1.2583(7) 1.2044(6) 0.0516(3) 0.0467(18) Uani 1 1 d . . . . .
H110 H 1.312919 1.230541 0.020290 0.056 Uiso 1 1 calc R . . . .
O30 O 0.7433(7) 0.5690(6) 0.0619(4) 0.0941(19) Uani 1 1 d . U . . .
N2 N 0.8549(8) 0.4213(7) 0.0409(5) 0.0824(19) Uani 1 1 d . U . . .
C50 C 0.7886(10) 0.4924(8) 0.0806(6) 0.085(2) Uani 1 1 d . U . . .
H50 H 0.778826 0.478311 0.126293 0.102 Uiso 1 1 calc R . . . .
C51 C 0.8661(11) 0.4283(9) -0.0277(6) 0.104(3) Uani 1 1 d . U . . .
H51A H 0.805465 0.396711 -0.044075 0.155 Uiso 1 1 calc GR . . . .
H51B H 0.949670 0.398162 -0.044570 0.155 Uiso 1 1 calc GR . . . .
H51C H 0.851057 0.494834 -0.042209 0.155 Uiso 1 1 calc GR . . . .
C52 C 0.9082(11) 0.3321(9) 0.0745(6) 0.101(2) Uani 1 1 d . U . . .
H52A H 0.998270 0.325654 0.071700 0.152 Uiso 1 1 calc GR . . . .
H52B H 0.887074 0.279069 0.053559 0.152 Uiso 1 1 calc GR . . . .
H52C H 0.874472 0.332451 0.120502 0.152 Uiso 1 1 calc GR . . . .
O31 O 0.1557(4) 0.8667(4) 0.0247(2) 0.0533(13) Uani 1 1 d . . . . .
H31A H 0.187015 0.895940 -0.009070 0.064 Uiso 1 1 d R . . . .
H31B H 0.078665 0.861280 0.027810 0.064 Uiso 1 1 d R . . . .
O1A O 0.4521(13) 1.0144(9) 0.0669(8) 0.089(5) Uani 0.5 1 d . . P . .
H1AA H 0.397500 0.981991 0.084076 0.133 Uiso 0.5 1 d DG . P . .
H1AB H 0.452728 1.016685 0.024650 0.133 Uiso 0.5 1 d G . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O4 2.287(4) . ?
Gd1 O8 2.262(4) . ?
Gd1 O11 2.443(4) . ?
Gd1 O15 2.363(4) . ?
Gd1 O26 2.386(4) . ?
Gd1 O27 2.472(4) . ?
Gd1 O28 2.343(4) . ?
Gd2 O7 2.327(4) . ?
Gd2 O10 2.312(4) . ?
Gd2 O14 2.439(4) 1_565 ?
Gd2 O18 2.305(4) . ?
Gd2 O19 2.475(4) . ?
Gd2 O20 2.501(4) . ?
Gd2 O23 2.594(4) . ?
Gd2 O24 2.429(4) . ?
Gd3 O1 2.422(4) . ?
Gd3 O2 2.460(4) . ?
Gd3 O6 2.385(4) 2_676 ?
Gd3 O9 2.318(4) 2_676 ?
Gd3 O13 2.339(3) 2_666 ?
Gd3 O17 2.307(4) 2_676 ?
Gd3 O22 2.281(4) 2_666 ?
Gd4 O3 2.338(4) . ?
Gd4 O5 2.354(4) 1_545 ?
Gd4 O12 2.350(4) . ?
Gd4 O16 2.286(4) . ?
Gd4 O21 2.369(4) . ?
Gd4 O25 2.396(4) . ?
Gd4 O29 2.492(5) . ?
O1 C1 1.248(7) . ?
O2 C1 1.267(6) . ?
O3 C8 1.252(6) . ?
O4 C8 1.262(6) . ?
O5 C9 1.250(7) . ?
O6 C9 1.254(7) . ?
O7 C16 1.263(7) . ?
O8 C16 1.260(6) . ?
O9 C17 1.254(7) . ?
O10 C17 1.263(7) . ?
O11 C24 1.250(6) . ?
O12 C24 1.272(6) . ?
O13 C54 1.273(6) . ?
O14 C54 1.264(6) . ?
O15 C25 1.269(7) . ?
O16 C25 1.258(7) . ?
O17 C32 1.262(6) . ?
O18 C32 1.250(6) . ?
O19 C38 1.282(6) . ?
O20 C38 1.253(7) . ?
O21 C39 1.233(7) . ?
O22 C39 1.256(7) . ?
O23 C46 1.250(6) . ?
O24 C46 1.278(6) . ?
O25 H25A 0.8499 . ?
O25 H25B 0.8501 . ?
O26 H26A 0.8501 . ?
O26 H26B 0.8499 . ?
O27 H27A 0.8499 . ?
O27 H27B 0.8501 . ?
O28 H28A 0.8502 . ?
O28 H28B 0.8500 . ?
O29 C47 1.200(8) . ?
N1 C47 1.263(10) . ?
N1 C48 1.525(13) . ?
N1 C49 1.412(10) . ?
C1 C2 1.501(7) . ?
C2 C3 1.408(7) . ?
C2 C7 1.384(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.388(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.382(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.400(7) . ?
C6 C7 1.399(7) . ?
C6 C8 1.497(7) . ?
C7 H7 0.9300 . ?
C9 C10 1.510(7) . ?
C10 C11 1.395(8) . ?
C10 C15 1.395(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.379(9) . ?
C12 H12 0.9300 . ?
C12 C13 1.400(9) . ?
C13 H13 0.9300 . ?
C13 C14 1.388(8) . ?
C14 C15 1.395(7) . ?
C14 C16 1.475(7) . ?
C15 H15 0.9300 . ?
C17 C18 1.492(7) . ?
C18 C19 1.402(7) . ?
C18 C23 1.398(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.394(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.389(7) . ?
C21 H21 0.9300 . ?
C21 C22 1.403(7) . ?
C22 C23 1.373(7) . ?
C22 C24 1.512(7) . ?
C23 H23 0.9300 . ?
C25 C26 1.502(7) . ?
C26 C27 1.404(7) . ?
C26 C31 1.394(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.390(8) . ?
C28 H28 0.9300 . ?
C28 C29 1.402(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.393(7) . ?
C30 C31 1.386(7) . ?
C30 C54 1.508(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.506(7) . ?
C33 C34 1.390(7) . ?
C33 C37 1.389(7) . ?
C34 H34 0.9300 . ?
C34 C35 1.379(8) . ?
C35 H35 0.9300 . ?
C35 C110 1.375(8) . ?
C36 C37 1.396(7) . ?
C36 C38 1.493(7) 2_775 ?
C36 C110 1.398(8) . ?
C37 H37 0.9300 . ?
C39 C40 1.515(7) . ?
C40 C41 1.393(7) . ?
C40 C45 1.386(8) . ?
C41 H41 0.9300 . ?
C41 C42 1.402(7) . ?
C42 C43 1.385(8) . ?
C42 C46 1.491(6) . ?
C43 H43 0.9300 . ?
C43 C44 1.382(8) . ?
C44 H44 0.9300 . ?
C44 C45 1.385(9) . ?
C45 H45 0.9300 . ?
C47 H47 0.9300 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C110 H110 0.9300 . ?
O30 C50 1.162(12) . ?
N2 C50 1.366(14) . ?
N2 C51 1.376(14) . ?
N2 C52 1.448(13) . ?
C50 H50 0.9300 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
O31 H31A 0.8500 . ?
O31 H31B 0.8499 . ?
O1A H1AA 0.8500 . ?
O1A H1AB 0.8504 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Gd1 O11 77.05(13) . . ?
O4 Gd1 O15 92.31(15) . . ?
O4 Gd1 O26 70.41(13) . . ?
O4 Gd1 O27 138.89(14) . . ?
O4 Gd1 O28 149.70(15) . . ?
O8 Gd1 O4 93.28(15) . . ?
O8 Gd1 O11 79.94(14) . . ?
O8 Gd1 O15 172.90(15) . . ?
O8 Gd1 O26 92.45(16) . . ?
O8 Gd1 O27 76.68(15) . . ?
O8 Gd1 O28 100.57(15) . . ?
O11 Gd1 O27 137.42(13) . . ?
O15 Gd1 O11 105.62(14) . . ?
O15 Gd1 O26 85.30(15) . . ?
O15 Gd1 O27 96.22(15) . . ?
O26 Gd1 O11 146.09(15) . . ?
O26 Gd1 O27 70.34(14) . . ?
O28 Gd1 O11 79.01(15) . . ?
O28 Gd1 O15 76.53(15) . . ?
O28 Gd1 O26 134.86(15) . . ?
O28 Gd1 O27 71.05(16) . . ?
O7 Gd2 O14 77.19(15) . 1_565 ?
O7 Gd2 O19 124.91(13) . . ?
O7 Gd2 O20 77.08(14) . . ?
O7 Gd2 O23 131.62(13) . . ?
O7 Gd2 O24 81.29(14) . . ?
O10 Gd2 O7 76.84(15) . . ?
O10 Gd2 O14 115.10(17) . 1_565 ?
O10 Gd2 O19 158.21(14) . . ?
O10 Gd2 O20 145.25(14) . . ?
O10 Gd2 O23 85.39(17) . . ?
O10 Gd2 O24 81.13(17) . . ?
O14 Gd2 O19 75.14(14) 1_565 . ?
O14 Gd2 O20 80.64(15) 1_565 . ?
O14 Gd2 O23 149.51(14) 1_565 . ?
O18 Gd2 O7 141.66(14) . . ?
O18 Gd2 O10 82.47(14) . . ?
O18 Gd2 O14 83.06(14) . 1_565 ?
O18 Gd2 O19 79.75(13) . . ?
O18 Gd2 O20 131.65(13) . . ?
O18 Gd2 O23 77.34(13) . . ?
O18 Gd2 O24 127.01(13) . . ?
O19 Gd2 O20 52.12(12) . . ?
O19 Gd2 O23 78.53(14) . . ?
O20 Gd2 O23 95.16(15) . . ?
O24 Gd2 O14 148.72(13) . 1_565 ?
O24 Gd2 O19 99.71(15) . . ?
O24 Gd2 O20 72.56(15) . . ?
O24 Gd2 O23 51.41(12) . . ?
O1 Gd3 O2 52.74(14) . . ?
O6 Gd3 O1 127.85(13) 2_676 . ?
O6 Gd3 O2 77.53(13) 2_676 . ?
O9 Gd3 O1 76.85(17) 2_676 . ?
O9 Gd3 O2 84.50(16) 2_676 . ?
O9 Gd3 O6 84.58(16) 2_676 2_676 ?
O9 Gd3 O13 96.27(15) 2_676 2_666 ?
O13 Gd3 O1 148.64(14) 2_666 . ?
O13 Gd3 O2 158.20(13) 2_666 . ?
O13 Gd3 O6 80.85(14) 2_666 2_676 ?
O17 Gd3 O1 76.55(13) 2_676 . ?
O17 Gd3 O2 123.75(14) 2_676 . ?
O17 Gd3 O6 155.20(13) 2_676 2_676 ?
O17 Gd3 O9 108.27(17) 2_676 2_676 ?
O17 Gd3 O13 76.79(13) 2_676 2_666 ?
O22 Gd3 O1 101.15(17) 2_666 . ?
O22 Gd3 O2 80.95(16) 2_666 . ?
O22 Gd3 O6 83.38(15) 2_666 2_676 ?
O22 Gd3 O9 162.81(18) 2_666 2_676 ?
O22 Gd3 O13 93.89(15) 2_666 2_666 ?
O22 Gd3 O17 87.53(16) 2_666 2_676 ?
O3 Gd4 O5 94.96(15) . 1_545 ?
O3 Gd4 O12 77.45(14) . . ?
O3 Gd4 O21 137.98(14) . . ?
O3 Gd4 O25 134.53(14) . . ?
O3 Gd4 O29 69.42(14) . . ?
O5 Gd4 O21 117.82(16) 1_545 . ?
O5 Gd4 O25 89.37(16) 1_545 . ?
O5 Gd4 O29 74.07(17) 1_545 . ?
O12 Gd4 O5 152.54(17) . 1_545 ?
O12 Gd4 O21 82.79(15) . . ?
O12 Gd4 O25 78.27(13) . . ?
O12 Gd4 O29 78.58(15) . . ?
O16 Gd4 O3 82.32(16) . . ?
O16 Gd4 O5 84.6(2) . 1_545 ?
O16 Gd4 O12 119.71(17) . . ?
O16 Gd4 O21 75.91(17) . . ?
O16 Gd4 O25 143.11(16) . . ?
O16 Gd4 O29 142.42(16) . . ?
O21 Gd4 O25 74.96(15) . . ?
O21 Gd4 O29 141.50(15) . . ?
O25 Gd4 O29 68.44(15) . . ?
C1 O1 Gd3 94.9(3) . . ?
C1 O2 Gd3 92.6(3) . . ?
C8 O3 Gd4 142.2(4) . . ?
C8 O4 Gd1 134.2(3) . . ?
C9 O5 Gd4 115.4(4) . 1_565 ?
C9 O6 Gd3 157.6(4) . 2_676 ?
C16 O7 Gd2 159.5(4) . . ?
C16 O8 Gd1 156.1(4) . . ?
C17 O9 Gd3 123.3(4) . 2_676 ?
C17 O10 Gd2 153.9(4) . . ?
C24 O11 Gd1 157.0(4) . . ?
C24 O12 Gd4 111.7(3) . . ?
C54 O13 Gd3 166.3(3) . 2_666 ?
C54 O14 Gd2 112.7(3) . 1_545 ?
C25 O15 Gd1 121.2(3) . . ?
C25 O16 Gd4 174.6(4) . . ?
C32 O17 Gd3 137.2(3) . 2_676 ?
C32 O18 Gd2 147.2(4) . . ?
C38 O19 Gd2 94.6(3) . . ?
C38 O20 Gd2 94.2(3) . . ?
C39 O21 Gd4 154.4(4) . . ?
C39 O22 Gd3 147.4(4) . 2_666 ?
C46 O23 Gd2 91.0(3) . . ?
C46 O24 Gd2 98.1(3) . . ?
Gd4 O25 H25A 120.0 . . ?
Gd4 O25 H25B 120.0 . . ?
H25A O25 H25B 120.0 . . ?
Gd1 O26 H26A 120.0 . . ?
Gd1 O26 H26B 119.9 . . ?
H26A O26 H26B 120.0 . . ?
Gd1 O27 H27A 120.0 . . ?
Gd1 O27 H27B 120.0 . . ?
H27A O27 H27B 120.0 . . ?
Gd1 O28 H28A 120.1 . . ?
Gd1 O28 H28B 119.9 . . ?
H28A O28 H28B 120.0 . . ?
C47 O29 Gd4 135.0(6) . . ?
C47 N1 C48 115.4(8) . . ?
C47 N1 C49 131.3(10) . . ?
C49 N1 C48 112.3(9) . . ?
O1 C1 O2 119.2(5) . . ?
O1 C1 C2 120.6(5) . . ?
O2 C1 C2 120.1(5) . . ?
C3 C2 C1 117.8(5) . . ?
C7 C2 C1 122.4(5) . . ?
C7 C2 C3 119.8(5) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.1(6) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0(5) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.1(5) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C8 120.4(4) . . ?
C7 C6 C5 120.0(5) . . ?
C7 C6 C8 119.4(4) . . ?
C2 C7 C6 119.8(5) . . ?
C2 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
O3 C8 O4 124.3(5) . . ?
O3 C8 C6 119.4(4) . . ?
O4 C8 C6 116.4(5) . . ?
O5 C9 O6 123.3(5) . . ?
O5 C9 C10 117.0(5) . . ?
O6 C9 C10 119.6(5) . . ?
C11 C10 C9 120.5(5) . . ?
C15 C10 C9 120.0(5) . . ?
C15 C10 C11 119.6(5) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 C10 120.2(6) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.5(6) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.5(5) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 C15 120.1(5) . . ?
C13 C14 C16 120.3(5) . . ?
C15 C14 C16 119.5(5) . . ?
C10 C15 C14 120.1(5) . . ?
C10 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
O7 C16 C14 119.3(5) . . ?
O8 C16 O7 122.9(5) . . ?
O8 C16 C14 117.8(5) . . ?
O9 C17 O10 124.3(5) . . ?
O9 C17 C18 116.6(5) . . ?
O10 C17 C18 119.1(5) . . ?
C19 C18 C17 119.3(4) . . ?
C23 C18 C17 121.4(4) . . ?
C23 C18 C19 119.3(4) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.9(5) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 119.9 . . ?
C21 C20 C19 120.2(5) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 120.2 . . ?
C20 C21 C22 119.7(5) . . ?
C22 C21 H21 120.2 . . ?
C21 C22 C24 117.8(5) . . ?
C23 C22 C21 120.2(5) . . ?
C23 C22 C24 122.0(5) . . ?
C18 C23 H23 119.7 . . ?
C22 C23 C18 120.7(5) . . ?
C22 C23 H23 119.7 . . ?
O11 C24 O12 124.0(5) . . ?
O11 C24 C22 120.5(5) . . ?
O12 C24 C22 115.5(4) . . ?
O15 C25 C26 118.1(5) . . ?
O16 C25 O15 123.9(5) . . ?
O16 C25 C26 118.0(5) . . ?
C27 C26 C25 119.1(4) . . ?
C31 C26 C25 121.1(4) . . ?
C31 C26 C27 119.8(5) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 C26 119.9(4) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 120.1 . . ?
C27 C28 C29 119.8(5) . . ?
C29 C28 H28 120.1 . . ?
C28 C29 H29 119.9 . . ?
C30 C29 C28 120.2(5) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 C54 119.0(4) . . ?
C31 C30 C29 120.0(4) . . ?
C31 C30 C54 121.0(4) . . ?
C26 C31 H31 119.8 . . ?
C30 C31 C26 120.3(4) . . ?
C30 C31 H31 119.8 . . ?
O17 C32 C33 118.4(5) . . ?
O18 C32 O17 124.7(5) . . ?
O18 C32 C33 116.9(5) . . ?
C34 C33 C32 121.7(5) . . ?
C37 C33 C32 118.1(4) . . ?
C37 C33 C34 120.1(5) . . ?
C33 C34 H34 120.4 . . ?
C35 C34 C33 119.2(5) . . ?
C35 C34 H34 120.4 . . ?
C34 C35 H35 119.2 . . ?
C110 C35 C34 121.6(5) . . ?
C110 C35 H35 119.2 . . ?
C37 C36 C38 120.4(5) . 2_775 ?
C37 C36 C110 119.2(5) . . ?
C110 C36 C38 120.4(5) . 2_775 ?
C33 C37 C36 120.3(5) . . ?
C33 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
O19 C38 C36 119.0(5) . 2_775 ?
O20 C38 O19 119.1(5) . . ?
O20 C38 C36 121.9(5) . 2_775 ?
O21 C39 O22 125.2(5) . . ?
O21 C39 C40 119.5(5) . . ?
O22 C39 C40 115.3(5) . . ?
C41 C40 C39 119.5(5) . . ?
C45 C40 C39 120.9(5) . . ?
C45 C40 C41 119.5(5) . . ?
C40 C41 H41 119.7 . . ?
C40 C41 C42 120.6(5) . . ?
C42 C41 H41 119.7 . . ?
C41 C42 C46 119.2(5) . . ?
C43 C42 C41 118.7(5) . . ?
C43 C42 C46 122.0(5) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 C42 120.7(5) . . ?
C44 C43 H43 119.6 . . ?
C43 C44 H44 119.9 . . ?
C43 C44 C45 120.3(6) . . ?
C45 C44 H44 119.9 . . ?
C40 C45 H45 120.0 . . ?
C44 C45 C40 120.0(5) . . ?
C44 C45 H45 120.0 . . ?
O23 C46 O24 119.5(4) . . ?
O23 C46 C42 122.5(5) . . ?
O24 C46 C42 118.0(4) . . ?
O29 C47 N1 134.9(10) . . ?
O29 C47 H47 112.5 . . ?
N1 C47 H47 112.5 . . ?
N1 C48 H48A 109.5 . . ?
N1 C48 H48B 109.5 . . ?
N1 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N1 C49 H49A 109.5 . . ?
N1 C49 H49B 109.5 . . ?
N1 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O13 C54 C30 118.6(5) . . ?
O14 C54 O13 121.4(4) . . ?
O14 C54 C30 119.9(4) . . ?
C35 C110 C36 119.6(5) . . ?
C35 C110 H110 120.2 . . ?
C36 C110 H110 120.2 . . ?
C50 N2 C51 123.9(10) . . ?
C50 N2 C52 116.5(10) . . ?
C51 N2 C52 119.5(10) . . ?
O30 C50 N2 125.2(12) . . ?
O30 C50 H50 117.4 . . ?
N2 C50 H50 117.4 . . ?
N2 C51 H51A 109.5 . . ?
N2 C51 H51B 109.5 . . ?
N2 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N2 C52 H52A 109.5 . . ?
N2 C52 H52B 109.5 . . ?
N2 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
H31A O31 H31B 120.0 . . ?
H1AA O1A H1AB 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Gd1 O4 C8 O3 -56.8(7) . . . . ?
Gd1 O4 C8 C6 121.5(5) . . . . ?
Gd1 O8 C16 O7 -5.7(13) . . . . ?
Gd1 O8 C16 C14 175.4(7) . . . . ?
Gd1 O11 C24 O12 110.2(9) . . . . ?
Gd1 O11 C24 C22 -71.9(11) . . . . ?
Gd1 O15 C25 O16 23.5(8) . . . . ?
Gd1 O15 C25 C26 -156.7(4) . . . . ?
Gd2 O7 C16 O8 -70.9(12) . . . . ?
Gd2 O7 C16 C14 108.0(10) . . . . ?
Gd2 O10 C17 O9 -88.4(10) . . . . ?
Gd2 O10 C17 C18 92.0(10) . . . . ?
Gd2 O14 C54 O13 9.6(6) 1_545 . . . ?
Gd2 O14 C54 C30 -167.9(4) 1_545 . . . ?
Gd2 O18 C32 O17 42.9(9) . . . . ?
Gd2 O18 C32 C33 -137.0(5) . . . . ?
Gd2 O19 C38 O20 -1.6(6) . . . . ?
Gd2 O19 C38 C36 177.4(4) . . . 2_775 ?
Gd2 O20 C38 O19 1.6(6) . . . . ?
Gd2 O20 C38 C36 -177.4(5) . . . 2_775 ?
Gd2 O23 C46 O24 -0.4(5) . . . . ?
Gd2 O23 C46 C42 178.5(5) . . . . ?
Gd2 O24 C46 O23 0.4(6) . . . . ?
Gd2 O24 C46 C42 -178.6(4) . . . . ?
Gd3 O1 C1 O2 7.5(6) . . . . ?
Gd3 O1 C1 C2 -169.3(4) . . . . ?
Gd3 O2 C1 O1 -7.4(6) . . . . ?
Gd3 O2 C1 C2 169.5(4) . . . . ?
Gd3 O6 C9 O5 166.5(7) 2_676 . . . ?
Gd3 O6 C9 C10 -14.0(13) 2_676 . . . ?
Gd3 O9 C17 O10 7.6(8) 2_676 . . . ?
Gd3 O9 C17 C18 -172.8(3) 2_676 . . . ?
Gd3 O13 C54 O14 145.7(13) 2_666 . . . ?
Gd3 O13 C54 C30 -36.8(18) 2_666 . . . ?
Gd3 O17 C32 O18 -47.2(8) 2_676 . . . ?
Gd3 O17 C32 C33 132.6(4) 2_676 . . . ?
Gd3 O22 C39 O21 -28.6(11) 2_666 . . . ?
Gd3 O22 C39 C40 152.6(6) 2_666 . . . ?
Gd4 O3 C8 O4 60.6(8) . . . . ?
Gd4 O3 C8 C6 -117.7(5) . . . . ?
Gd4 O5 C9 O6 5.2(8) 1_565 . . . ?
Gd4 O5 C9 C10 -174.3(4) 1_565 . . . ?
Gd4 O12 C24 O11 3.5(7) . . . . ?
Gd4 O12 C24 C22 -174.5(3) . . . . ?
Gd4 O21 C39 O22 -12.4(13) . . . . ?
Gd4 O21 C39 C40 166.4(6) . . . . ?
Gd4 O29 C47 N1 -158.5(8) . . . . ?
O1 C1 C2 C3 8.4(8) . . . . ?
O1 C1 C2 C7 -173.6(5) . . . . ?
O2 C1 C2 C3 -168.4(5) . . . . ?
O2 C1 C2 C7 9.7(8) . . . . ?
O5 C9 C10 C11 -22.9(8) . . . . ?
O5 C9 C10 C15 158.1(5) . . . . ?
O6 C9 C10 C11 157.6(6) . . . . ?
O6 C9 C10 C15 -21.5(8) . . . . ?
O9 C17 C18 C19 -20.3(8) . . . . ?
O9 C17 C18 C23 156.9(5) . . . . ?
O10 C17 C18 C19 159.3(5) . . . . ?
O10 C17 C18 C23 -23.5(8) . . . . ?
O15 C25 C26 C27 -12.9(8) . . . . ?
O15 C25 C26 C31 165.6(5) . . . . ?
O16 C25 C26 C27 166.9(5) . . . . ?
O16 C25 C26 C31 -14.6(8) . . . . ?
O17 C32 C33 C34 17.5(8) . . . . ?
O17 C32 C33 C37 -158.9(5) . . . . ?
O18 C32 C33 C34 -162.7(5) . . . . ?
O18 C32 C33 C37 21.0(7) . . . . ?
O21 C39 C40 C41 -18.4(8) . . . . ?
O21 C39 C40 C45 164.5(6) . . . . ?
O22 C39 C40 C41 160.5(5) . . . . ?
O22 C39 C40 C45 -16.6(8) . . . . ?
C1 C2 C3 C4 173.2(5) . . . . ?
C1 C2 C7 C6 -175.4(5) . . . . ?
C2 C3 C4 C5 3.5(10) . . . . ?
C3 C2 C7 C6 2.5(8) . . . . ?
C3 C4 C5 C6 0.2(10) . . . . ?
C4 C5 C6 C7 -2.6(9) . . . . ?
C4 C5 C6 C8 -178.9(5) . . . . ?
C5 C6 C7 C2 1.2(8) . . . . ?
C5 C6 C8 O3 -154.0(5) . . . . ?
C5 C6 C8 O4 27.5(7) . . . . ?
C7 C2 C3 C4 -4.9(9) . . . . ?
C7 C6 C8 O3 29.6(7) . . . . ?
C7 C6 C8 O4 -148.8(5) . . . . ?
C8 C6 C7 C2 177.5(5) . . . . ?
C9 C10 C11 C12 -177.1(6) . . . . ?
C9 C10 C15 C14 177.8(5) . . . . ?
C10 C11 C12 C13 -1.9(11) . . . . ?
C11 C10 C15 C14 -1.2(8) . . . . ?
C11 C12 C13 C14 1.2(11) . . . . ?
C12 C13 C14 C15 -0.4(9) . . . . ?
C12 C13 C14 C16 -178.7(6) . . . . ?
C13 C14 C15 C10 0.5(8) . . . . ?
C13 C14 C16 O7 174.9(5) . . . . ?
C13 C14 C16 O8 -6.1(8) . . . . ?
C15 C10 C11 C12 1.9(10) . . . . ?
C15 C14 C16 O7 -3.4(7) . . . . ?
C15 C14 C16 O8 175.6(5) . . . . ?
C16 C14 C15 C10 178.8(5) . . . . ?
C17 C18 C19 C20 175.6(6) . . . . ?
C17 C18 C23 C22 -176.0(5) . . . . ?
C18 C19 C20 C21 1.4(11) . . . . ?
C19 C18 C23 C22 1.2(8) . . . . ?
C19 C20 C21 C22 -0.6(11) . . . . ?
C20 C21 C22 C23 0.1(9) . . . . ?
C20 C21 C22 C24 178.6(6) . . . . ?
C21 C22 C23 C18 -0.4(8) . . . . ?
C21 C22 C24 O11 159.9(5) . . . . ?
C21 C22 C24 O12 -22.0(7) . . . . ?
C23 C18 C19 C20 -1.7(9) . . . . ?
C23 C22 C24 O11 -21.6(8) . . . . ?
C23 C22 C24 O12 156.5(5) . . . . ?
C24 C22 C23 C18 -178.9(5) . . . . ?
C25 C26 C27 C28 178.9(5) . . . . ?
C25 C26 C31 C30 -177.7(5) . . . . ?
C26 C27 C28 C29 -0.7(9) . . . . ?
C27 C26 C31 C30 0.9(8) . . . . ?
C27 C28 C29 C30 -0.3(9) . . . . ?
C28 C29 C30 C31 1.5(8) . . . . ?
C28 C29 C30 C54 179.8(5) . . . . ?
C29 C30 C31 C26 -1.8(8) . . . . ?
C29 C30 C54 O13 177.4(5) . . . . ?
C29 C30 C54 O14 -5.1(8) . . . . ?
C31 C26 C27 C28 0.4(8) . . . . ?
C31 C30 C54 O13 -4.3(8) . . . . ?
C31 C30 C54 O14 173.2(5) . . . . ?
C32 C33 C34 C35 -177.6(6) . . . . ?
C32 C33 C37 C36 175.7(5) . . . . ?
C33 C34 C35 C110 3.0(12) . . . . ?
C34 C33 C37 C36 -0.8(9) . . . . ?
C34 C35 C110 C36 -2.4(13) . . . . ?
C37 C33 C34 C35 -1.3(10) . . . . ?
C37 C36 C110 C35 0.3(11) . . . . ?
C38 C36 C37 C33 179.9(5) 2_775 . . . ?
C38 C36 C110 C35 -178.4(7) 2_775 . . . ?
C39 C40 C41 C42 -175.5(5) . . . . ?
C39 C40 C45 C44 178.5(6) . . . . ?
C40 C41 C42 C43 -3.2(8) . . . . ?
C40 C41 C42 C46 173.6(5) . . . . ?
C41 C40 C45 C44 1.3(10) . . . . ?
C41 C42 C43 C44 1.9(10) . . . . ?
C41 C42 C46 O23 169.6(5) . . . . ?
C41 C42 C46 O24 -11.5(7) . . . . ?
C42 C43 C44 C45 1.1(12) . . . . ?
C43 C42 C46 O23 -13.7(8) . . . . ?
C43 C42 C46 O24 165.2(6) . . . . ?
C43 C44 C45 C40 -2.7(12) . . . . ?
C45 C40 C41 C42 1.6(8) . . . . ?
C46 C42 C43 C44 -174.8(6) . . . . ?
C48 N1 C47 O29 -10.2(15) . . . . ?
C49 N1 C47 O29 -177.1(10) . . . . ?
C54 C30 C31 C26 179.9(5) . . . . ?
C110 C36 C37 C33 1.3(9) . . . . ?
C51 N2 C50 O30 -6.8(18) . . . . ?
C52 N2 C50 O30 177.5(10) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelxl_CCDC4
_audit_block_doi                 10.5517/cc1j7ms5
_database_code_depnum_ccdc_archive 'CCDC 1407517'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H39 Ho4 N O29, C3 H7 N O, 1.5(H2 O)'
_chemical_formula_sum            'C54 H49 Ho4 N2 O31.50'
_chemical_formula_weight         1880.66
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.840(2)
_cell_length_b                   14.120(3)
_cell_length_c                   20.070(4)
_cell_angle_alpha                86.59(3)
_cell_angle_beta                 83.70(3)
_cell_angle_gamma                78.88(3)
_cell_volume                     2993.7(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8876
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.325
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.096
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1814
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1017
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30651
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.553
_diffrn_reflns_theta_min         3.066
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.0714
	          2theta: 29.9126
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.0714
	          2theta: 29.9126
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.0714
	          2theta: 29.9126
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.092488
_diffrn_orient_matrix_UB_12      -0.013677
_diffrn_orient_matrix_UB_13      -0.013249
_diffrn_orient_matrix_UB_21      0.025992
_diffrn_orient_matrix_UB_22      -0.064977
_diffrn_orient_matrix_UB_23      -0.017766
_diffrn_orient_matrix_UB_31      -0.000201
_diffrn_orient_matrix_UB_32      -0.011264
_diffrn_orient_matrix_UB_33      0.048884
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12319
_reflns_number_total             13703
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.534
_refine_diff_density_min         -1.969
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     839
_refine_ls_number_reflns         13703
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0398
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0235P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1024
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H26A,H26B} of O26, {H27A,H27B} of O27, {H25A,H25B} of O25,
   {H31A,H31B} of O31
 At 1.5 times of:
  All C(H,H,H) groups, {H28A,H28B} of O28, {H1AA,H1AB} of O1A
2. Restrained distances
 H31B-H25A_$1
 2.2 with sigma of 0.01
 O25-H25A
 0.85 with sigma of 0.01
 H25B-O25
 0.85 with sigma of 0.01
 H25A-H25B
 1.39 with sigma of 0.01
 H25A-Ho1
 2.9 with sigma of 0.01
 H1AA-H26A
 2.2 with sigma of 0.01
 H1AA-H26B
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
4. Others
 Fixed Sof: O1A(0.5) H1AA(0.5) H1AB(0.5)
5.a Riding coordinates:
 O26(H26A,H26B), O27(H27A,H27B), O28(H28A,H28B), O31(H31A,H31B), O1A(H1AA,H1AB)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13), C15(H15),
 C19(H19), C20(H20), C21(H21), C23(H23), C27(H27), C28(H28), C29(H29), C31(H31),
  C35(H35), C37(H37), C38(H38), C39(H39), C43(H43), C44(H44), C45(H45),
 C47(H47), C49(H49), C52(H52)
5.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 1.08558(2) 0.76691(2) 0.30233(2) 0.01711(6) Uani 1 1 d D . . . .
Ho2 Ho 0.72825(2) 0.30685(2) 0.19069(2) 0.01616(6) Uani 1 1 d . . . . .
Ho3 Ho 0.71028(2) 0.55621(2) 0.32649(2) 0.01613(6) Uani 1 1 d . . . . .
Ho4 Ho 1.04551(2) 0.01177(2) 0.14696(2) 0.02057(7) Uani 1 1 d . . . . .
O1 O 1.0751(4) 0.6219(2) 0.2676(2) 0.0300(9) Uani 1 1 d . . . . .
O2 O 0.9245(4) 0.5371(3) 0.2959(2) 0.0280(8) Uani 1 1 d . . . . .
O3 O 0.9418(4) 0.2344(3) 0.17536(19) 0.0278(9) Uani 1 1 d . . . . .
O4 O 1.1325(4) 0.1493(3) 0.1518(3) 0.0418(11) Uani 1 1 d . . . . .
O5 O 1.0866(4) 0.9138(3) 0.3495(2) 0.0294(9) Uani 1 1 d . . . . .
O6 O 1.0462(5) 1.0074(3) 0.2590(2) 0.0418(11) Uani 1 1 d . . . . .
O7 O 0.7886(4) 1.3379(3) 0.29262(17) 0.0256(8) Uani 1 1 d . . . . .
O8 O 0.7932(4) 1.4092(3) 0.38691(19) 0.0315(9) Uani 1 1 d . . . . .
O9 O 1.2511(4) 0.7619(3) -0.08063(19) 0.0364(10) Uani 1 1 d . . . . .
O10 O 1.4176(4) 0.6536(3) -0.10782(19) 0.0388(11) Uani 1 1 d . . . . .
O11 O 1.2323(4) 0.9027(3) 0.15426(18) 0.0259(8) Uani 1 1 d . . . . .
O12 O 1.2564(4) 0.7815(3) 0.23102(18) 0.0263(8) Uani 1 1 d . . . . .
O13 O 0.7918(4) 0.4375(3) 0.1356(2) 0.0345(10) Uani 1 1 d . . . . .
O14 O 0.7249(4) 0.5447(3) 0.21325(19) 0.0372(11) Uani 1 1 d . . . . .
O15 O 0.9966(4) 0.8140(3) 0.1967(2) 0.0283(9) Uani 1 1 d . . . . .
O16 O 1.0070(4) 0.8802(3) 0.0943(2) 0.0289(9) Uani 1 1 d . . . . .
O17 O 0.5278(4) -0.3014(3) 0.3074(2) 0.0278(8) Uani 1 1 d . . . . .
O18 O 0.7236(3) -0.2800(3) 0.2933(2) 0.0269(8) Uani 1 1 d . . . . .
O19 O 0.8323(4) 0.0259(3) 0.1880(2) 0.0329(9) Uani 1 1 d . . . . .
O20 O 0.6994(4) 0.1577(3) 0.2235(2) 0.0371(10) Uani 1 1 d . . . . .
O21 O 0.2126(4) 0.3731(3) 0.57955(19) 0.0360(10) Uani 1 1 d . . . . .
O22 O 0.3940(4) 0.4207(3) 0.55968(18) 0.0276(8) Uani 1 1 d . . . . .
O23 O 0.5405(4) 0.3662(3) 0.25134(18) 0.0270(8) Uani 1 1 d . . . . .
O24 O 0.5445(3) 0.4810(3) 0.32191(18) 0.0255(8) Uani 1 1 d . . . . .
O25 O 1.2698(4) 0.7076(3) 0.3555(2) 0.0348(10) Uani 1 1 d D . . . .
H25A H 1.3152(16) 0.6518(12) 0.3457(5) 0.042 Uiso 1 1 d DR . . . .
H25B H 1.315(4) 0.7496(18) 0.340(3) 0.042 Uiso 1 1 d DR . . . .
O26 O 1.0313(4) 0.6804(3) 0.40637(18) 0.0361(10) Uani 1 1 d . . . . .
H26A H 0.963499 0.657870 0.411621 0.043 Uiso 1 1 d DR . . . .
H26B H 1.079969 0.672710 0.437541 0.043 Uiso 1 1 d DR . . . .
O27 O 0.8758(4) 0.8209(3) 0.3381(2) 0.0354(10) Uani 1 1 d . . . . .
H27A H 0.843059 0.797119 0.374154 0.042 Uiso 1 1 d R . . . .
H27B H 0.831269 0.864719 0.315454 0.042 Uiso 1 1 d R . . . .
O28 O 0.9335(4) 0.0888(3) 0.05863(19) 0.0297(9) Uani 1 1 d . . . . .
H28A H 0.971744 0.094886 0.019750 0.045 Uiso 1 1 d R . . . .
H28B H 0.854654 0.110526 0.065640 0.045 Uiso 1 1 d R . . . .
O29 O 1.1850(4) 0.0165(3) 0.0422(2) 0.0356(10) Uani 1 1 d . . . . .
N1 N 1.3264(6) 0.0758(5) -0.0323(3) 0.0560(17) Uani 1 1 d . . . . .
C1 C 1.0280(5) 0.5475(4) 0.2654(2) 0.0194(10) Uani 1 1 d . . . . .
C2 C 1.1023(5) 0.4681(3) 0.2235(2) 0.0200(10) Uani 1 1 d . . . . .
C3 C 1.2207(6) 0.4751(4) 0.1927(3) 0.0336(14) Uani 1 1 d . . . . .
H3 H 1.254635 0.529695 0.197461 0.040 Uiso 1 1 calc R . . . .
C4 C 1.2893(6) 0.3991(5) 0.1540(4) 0.0422(16) Uani 1 1 d . . . . .
H4 H 1.368199 0.404062 0.132160 0.051 Uiso 1 1 calc R . . . .
C5 C 1.2404(5) 0.3176(4) 0.1483(3) 0.0333(14) Uani 1 1 d . . . . .
H5 H 1.288883 0.265728 0.125324 0.040 Uiso 1 1 calc R . . . .
C6 C 1.1176(5) 0.3120(4) 0.1770(3) 0.0217(11) Uani 1 1 d . . . . .
C7 C 1.0503(5) 0.3876(3) 0.2149(3) 0.0210(10) Uani 1 1 d . . . . .
H7 H 0.969476 0.384384 0.234767 0.025 Uiso 1 1 calc R . . . .
C8 C 1.0599(5) 0.2270(4) 0.1675(3) 0.0232(11) Uani 1 1 d . . . . .
C9 C 1.0499(5) 0.9939(4) 0.3212(3) 0.0233(11) Uani 1 1 d . . . . .
C10 C 1.0067(5) 1.0798(3) 0.3646(2) 0.0182(10) Uani 1 1 d . . . . .
C11 C 1.0312(5) 1.0744(3) 0.4312(2) 0.0235(11) Uani 1 1 d . . . . .
H11 H 1.075372 1.017130 0.448991 0.028 Uiso 1 1 calc R . . . .
C12 C 0.9910(6) 1.1526(4) 0.4716(3) 0.0265(12) Uani 1 1 d . . . . .
H12 H 1.009413 1.148203 0.515976 0.032 Uiso 1 1 calc R . . . .
C13 C 0.9233(5) 1.2373(4) 0.4457(3) 0.0237(11) Uani 1 1 d . . . . .
H13 H 0.896370 1.289920 0.472880 0.028 Uiso 1 1 calc R . . . .
C14 C 0.8945(5) 1.2448(3) 0.3786(2) 0.0185(10) Uani 1 1 d . . . . .
C15 C 0.9388(5) 1.1649(3) 0.3387(2) 0.0201(10) Uani 1 1 d . . . . .
H15 H 0.922257 1.168914 0.294036 0.024 Uiso 1 1 calc R . . . .
C16 C 0.8200(5) 1.3357(3) 0.3513(2) 0.0188(10) Uani 1 1 d . . . . .
C17 C 0.6056(5) -0.2464(4) 0.2928(2) 0.0199(10) Uani 1 1 d . . . . .
C18 C 0.5668(5) -0.1417(4) 0.2744(3) 0.0226(11) Uani 1 1 d . . . . .
C19 C 0.4418(5) -0.0948(4) 0.2861(3) 0.0312(13) Uani 1 1 d . . . . .
H19 H 0.379592 -0.130043 0.301816 0.037 Uiso 1 1 calc R . . . .
C20 C 0.4094(6) 0.0038(5) 0.2744(4) 0.052(2) Uani 1 1 d . . . . .
H20 H 0.325811 0.035026 0.282585 0.062 Uiso 1 1 calc R . . . .
C21 C 0.5014(6) 0.0557(4) 0.2505(4) 0.0385(15) Uani 1 1 d . . . . .
H21 H 0.479103 0.122147 0.243220 0.046 Uiso 1 1 calc R . . . .
C22 C 0.6265(5) 0.0111(4) 0.2372(3) 0.0246(11) Uani 1 1 d . . . . .
C23 C 0.6588(5) -0.0887(3) 0.2486(3) 0.0201(10) Uani 1 1 d . . . . .
H23 H 0.742062 -0.120118 0.239056 0.024 Uiso 1 1 calc R . . . .
C24 C 0.7282(5) 0.0678(4) 0.2141(3) 0.0234(11) Uani 1 1 d . . . . .
C25 C 0.7844(5) 0.5198(4) 0.1578(2) 0.0226(11) Uani 1 1 d . . . . .
C26 C 0.8490(5) 0.5903(3) 0.1154(2) 0.0193(10) Uani 1 1 d . . . . .
C27 C 0.8782(6) 0.5764(4) 0.0469(3) 0.0286(13) Uani 1 1 d . . . . .
H27 H 0.853045 0.526113 0.027307 0.034 Uiso 1 1 calc R . . . .
C28 C 0.9449(7) 0.6378(4) 0.0082(3) 0.0390(16) Uani 1 1 d . . . . .
H28 H 0.964547 0.628471 -0.037462 0.047 Uiso 1 1 calc R . . . .
C29 C 0.9823(6) 0.7127(4) 0.0369(3) 0.0310(13) Uani 1 1 d . . . . .
H29 H 1.027619 0.753473 0.010722 0.037 Uiso 1 1 calc R . . . .
C30 C 0.9518(5) 0.7269(3) 0.1056(2) 0.0196(10) Uani 1 1 d . . . . .
C31 C 0.8837(5) 0.6662(3) 0.1443(3) 0.0204(10) Uani 1 1 d . . . . .
H31 H 0.861325 0.676611 0.189712 0.025 Uiso 1 1 calc R . . . .
C32 C 0.9881(5) 0.8121(3) 0.1345(3) 0.0212(10) Uani 1 1 d . . . . .
C33 C 1.3511(5) 0.7064(4) -0.0644(3) 0.0236(11) Uani 1 1 d . . . . .
C34 C 1.3828(5) 0.6982(4) 0.0064(3) 0.0228(11) Uani 1 1 d . . . . .
C35 C 1.3199(5) 0.7625(4) 0.0543(2) 0.0213(10) Uani 1 1 d . . . . .
H35 H 1.259651 0.814865 0.041681 0.026 Uiso 1 1 calc R . . . .
C36 C 1.3461(5) 0.7496(4) 0.1204(2) 0.0204(10) Uani 1 1 d . . . . .
C37 C 1.4353(6) 0.6709(4) 0.1392(3) 0.0277(12) Uani 1 1 d . . . . .
H37 H 1.451288 0.660394 0.183905 0.033 Uiso 1 1 calc R . . . .
C38 C 1.5007(6) 0.6078(4) 0.0911(3) 0.0372(15) Uani 1 1 d . . . . .
H38 H 1.561474 0.555824 0.103618 0.045 Uiso 1 1 calc R . . . .
C39 C 1.4759(6) 0.6220(4) 0.0252(3) 0.0318(13) Uani 1 1 d . . . . .
H39 H 1.521509 0.580564 -0.006884 0.038 Uiso 1 1 calc R . . . .
C40 C 1.2729(5) 0.8171(4) 0.1722(2) 0.0199(10) Uani 1 1 d . . . . .
C41 C 0.3066(5) 0.3847(4) 0.5395(2) 0.0215(10) Uani 1 1 d . . . . .
C42 C 0.3173(6) 0.3567(4) 0.4683(3) 0.0249(11) Uani 1 1 d . . . . .
C43 C 0.2441(7) 0.2938(5) 0.4479(3) 0.0406(16) Uani 1 1 d . . . . .
H43 H 0.190150 0.266877 0.479456 0.049 Uiso 1 1 calc R . . . .
C44 C 0.2517(7) 0.2720(5) 0.3820(3) 0.0455(18) Uani 1 1 d . . . . .
H44 H 0.200898 0.231830 0.368925 0.055 Uiso 1 1 calc R . . . .
C45 C 0.3351(6) 0.3095(5) 0.3341(3) 0.0341(14) Uani 1 1 d . . . . .
H45 H 0.340869 0.293281 0.289453 0.041 Uiso 1 1 calc R . . . .
C46 C 0.4093(5) 0.3710(4) 0.3535(3) 0.0212(10) Uani 1 1 d . . . . .
C47 C 0.3983(5) 0.3953(4) 0.4200(2) 0.0193(10) Uani 1 1 d . . . . .
H47 H 0.445824 0.438186 0.432720 0.023 Uiso 1 1 calc R . . . .
C48 C 0.5060(5) 0.4087(4) 0.3050(2) 0.0209(10) Uani 1 1 d . . . . .
C49 C 1.2317(8) 0.0801(6) 0.0125(4) 0.054(2) Uani 1 1 d . . . . .
H49 H 1.192613 0.142323 0.024119 0.065 Uiso 1 1 calc R . . . .
C50 C 1.3693(10) 0.1559(7) -0.0678(5) 0.082(3) Uani 1 1 d . . . . .
H50A H 1.394252 0.140538 -0.113840 0.124 Uiso 1 1 calc GR . . . .
H50B H 1.440138 0.169636 -0.047865 0.124 Uiso 1 1 calc GR . . . .
H50C H 1.302235 0.211391 -0.065436 0.124 Uiso 1 1 calc GR . . . .
C51 C 1.3869(10) -0.0223(7) -0.0598(4) 0.074(3) Uani 1 1 d . . . . .
H51A H 1.436604 -0.059477 -0.027226 0.111 Uiso 1 1 calc GR . . . .
H51B H 1.440116 -0.013561 -0.100313 0.111 Uiso 1 1 calc GR . . . .
H51C H 1.322017 -0.055783 -0.069274 0.111 Uiso 1 1 calc GR . . . .
O30 O 0.7600(7) -0.0704(5) 0.4379(3) 0.083(2) Uani 1 1 d . . . . .
N2 N 0.6454(8) 0.0759(6) 0.4609(5) 0.079(3) Uani 1 1 d . . . . .
C52 C 0.7120(9) 0.0072(7) 0.4203(6) 0.076(3) Uani 1 1 d . . . . .
H52 H 0.720438 0.022852 0.374553 0.092 Uiso 1 1 calc R . . . .
C53 C 0.5913(13) 0.1669(9) 0.4266(9) 0.149(7) Uani 1 1 d . . . . .
H53A H 0.500793 0.176473 0.433119 0.223 Uiso 1 1 calc GR . . . .
H53B H 0.618674 0.163952 0.379455 0.223 Uiso 1 1 calc GR . . . .
H53C H 0.619247 0.219614 0.444682 0.223 Uiso 1 1 calc GR . . . .
C54 C 0.6317(14) 0.0676(12) 0.5269(7) 0.138(6) Uani 1 1 d . . . . .
H54A H 0.643907 0.000420 0.540738 0.207 Uiso 1 1 calc GR . . . .
H54B H 0.548166 0.099023 0.543275 0.207 Uiso 1 1 calc GR . . . .
H54C H 0.692895 0.097174 0.544800 0.207 Uiso 1 1 calc GR . . . .
O31 O 0.3439(4) 0.6320(4) 0.4762(2) 0.0495(13) Uani 1 1 d . . . . .
H31A H 0.338262 0.600838 0.513648 0.059 Uiso 1 1 d R . . . .
H31B H 0.278682 0.650368 0.455398 0.059 Uiso 1 1 d DR . . . .
O1A O 1.0473(10) 0.4854(5) 0.4314(5) 0.060(3) Uani 0.5 1 d . U P . .
H1AA H 1.099677 0.520131 0.414744 0.089 Uiso 0.5 1 d DR . P . .
H1AB H 1.032657 0.493100 0.473444 0.089 Uiso 0.5 1 d R . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O1 2.229(3) . ?
Ho1 O5 2.334(3) . ?
Ho1 O12 2.247(4) . ?
Ho1 O15 2.429(4) . ?
Ho1 O25 2.355(4) . ?
Ho1 O26 2.430(4) . ?
Ho1 O27 2.304(4) . ?
Ho2 O3 2.339(4) . ?
Ho2 O7 2.306(3) 1_545 ?
Ho2 O9 2.436(4) 2_765 ?
Ho2 O10 2.389(4) 2_765 ?
Ho2 O13 2.276(4) . ?
Ho2 O20 2.239(4) . ?
Ho2 O23 2.290(4) . ?
Ho2 C33 2.793(5) 2_765 ?
Ho3 O2 2.304(4) . ?
Ho3 O8 2.410(4) 1_545 ?
Ho3 O14 2.274(4) . ?
Ho3 O17 2.577(4) 1_565 ?
Ho3 O18 2.395(4) 1_565 ?
Ho3 O21 2.479(4) 2_666 ?
Ho3 O22 2.446(4) 2_666 ?
Ho3 O24 2.270(4) . ?
Ho3 C17 2.870(5) 1_565 ?
Ho3 C41 2.839(5) 2_666 ?
Ho4 O4 2.328(4) . ?
Ho4 O6 2.247(4) 1_545 ?
Ho4 O11 2.308(4) 1_545 ?
Ho4 O16 2.317(3) 1_545 ?
Ho4 O19 2.342(4) . ?
Ho4 O28 2.352(4) . ?
Ho4 O29 2.456(4) . ?
O1 C1 1.259(6) . ?
O2 C1 1.247(6) . ?
O3 C8 1.256(7) . ?
O4 C8 1.256(6) . ?
O5 C9 1.249(6) . ?
O6 C9 1.254(6) . ?
O7 C16 1.257(6) . ?
O8 C16 1.265(6) . ?
O9 C33 1.271(6) . ?
O10 C33 1.253(6) . ?
O11 C40 1.250(6) . ?
O12 C40 1.264(6) . ?
O13 C25 1.254(6) . ?
O14 C25 1.256(7) . ?
O15 C32 1.264(6) . ?
O16 C32 1.251(6) . ?
O17 C17 1.253(6) . ?
O18 C17 1.277(6) . ?
O19 C24 1.244(7) . ?
O20 C24 1.267(6) . ?
O21 C41 1.257(6) . ?
O22 C41 1.270(6) . ?
O23 C48 1.249(6) . ?
O24 C48 1.252(6) . ?
O25 H25A 0.866(9) . ?
O25 H25B 0.858(10) . ?
O26 H26A 0.8498 . ?
O26 H26B 0.8504 . ?
O27 H27A 0.8500 . ?
O27 H27B 0.8499 . ?
O28 H28A 0.8502 . ?
O28 H28B 0.8500 . ?
O29 C49 1.210(8) . ?
N1 C49 1.284(9) . ?
N1 C50 1.427(10) . ?
N1 C51 1.521(11) . ?
C1 C2 1.493(7) . ?
C2 C3 1.381(8) . ?
C2 C7 1.390(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.404(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.372(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.407(8) . ?
C6 C7 1.388(7) . ?
C6 C8 1.487(7) . ?
C7 H7 0.9300 . ?
C9 C10 1.505(7) . ?
C10 C11 1.386(7) . ?
C10 C15 1.387(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.382(7) . ?
C12 H12 0.9300 . ?
C12 C13 1.383(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.408(7) . ?
C14 C15 1.400(7) . ?
C14 C16 1.488(6) . ?
C15 H15 0.9300 . ?
C17 C18 1.493(7) . ?
C18 C19 1.390(7) . ?
C18 C23 1.397(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.381(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.377(9) . ?
C21 H21 0.9300 . ?
C21 C22 1.385(8) . ?
C22 C23 1.397(6) . ?
C22 C24 1.502(7) . ?
C23 H23 0.9300 . ?
C25 C26 1.497(7) . ?
C26 C27 1.393(7) . ?
C26 C31 1.380(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.384(8) . ?
C28 H28 0.9300 . ?
C28 C29 1.380(8) . ?
C29 H29 0.9300 . ?
C29 C30 1.400(7) . ?
C30 C31 1.387(7) . ?
C30 C32 1.501(6) . ?
C31 H31 0.9300 . ?
C33 C34 1.491(7) . ?
C34 C35 1.391(7) . ?
C34 C39 1.391(7) . ?
C35 H35 0.9300 . ?
C35 C36 1.381(7) . ?
C36 C37 1.388(7) . ?
C36 C40 1.505(7) . ?
C37 H37 0.9300 . ?
C37 C38 1.392(8) . ?
C38 H38 0.9300 . ?
C38 C39 1.373(8) . ?
C39 H39 0.9300 . ?
C41 C42 1.493(7) . ?
C42 C43 1.404(8) . ?
C42 C47 1.392(7) . ?
C43 H43 0.9300 . ?
C43 C44 1.365(8) . ?
C44 H44 0.9300 . ?
C44 C45 1.398(8) . ?
C45 H45 0.9300 . ?
C45 C46 1.391(7) . ?
C46 C47 1.385(7) . ?
C46 C48 1.503(7) . ?
C47 H47 0.9300 . ?
C49 H49 0.9300 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
O30 C52 1.171(10) . ?
N2 C52 1.348(12) . ?
N2 C53 1.471(14) . ?
N2 C54 1.318(14) . ?
C52 H52 0.9300 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
O31 H31A 0.8500 . ?
O31 H31B 0.8500 . ?
O1A H1AA 0.8499 . ?
O1A H1AB 0.8504 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ho1 O5 174.03(15) . . ?
O1 Ho1 O12 93.75(15) . . ?
O1 Ho1 O15 80.18(14) . . ?
O1 Ho1 O25 93.14(16) . . ?
O1 Ho1 O26 77.35(14) . . ?
O1 Ho1 O27 99.85(15) . . ?
O5 Ho1 O15 103.77(13) . . ?
O5 Ho1 O25 85.97(15) . . ?
O5 Ho1 O26 96.81(14) . . ?
O12 Ho1 O5 91.52(15) . . ?
O12 Ho1 O15 77.07(14) . . ?
O12 Ho1 O25 70.52(14) . . ?
O12 Ho1 O26 139.35(14) . . ?
O12 Ho1 O27 149.34(15) . . ?
O15 Ho1 O26 137.74(14) . . ?
O25 Ho1 O15 146.42(14) . . ?
O25 Ho1 O26 70.49(14) . . ?
O27 Ho1 O5 76.82(15) . . ?
O27 Ho1 O15 78.35(15) . . ?
O27 Ho1 O25 135.17(15) . . ?
O27 Ho1 O26 70.92(16) . . ?
O3 Ho2 O9 76.85(14) . 2_765 ?
O3 Ho2 O10 127.98(13) . 2_765 ?
O3 Ho2 C33 102.29(14) . 2_765 ?
O7 Ho2 O3 80.72(14) 1_545 . ?
O7 Ho2 O9 157.39(14) 1_545 2_765 ?
O7 Ho2 O10 148.69(13) 1_545 2_765 ?
O7 Ho2 C33 173.01(14) 1_545 2_765 ?
O9 Ho2 C33 27.04(14) 2_765 2_765 ?
O10 Ho2 O9 53.48(13) 2_765 2_765 ?
O10 Ho2 C33 26.54(14) 2_765 2_765 ?
O13 Ho2 O3 84.97(15) . . ?
O13 Ho2 O7 94.80(14) . 1_545 ?
O13 Ho2 O9 86.03(15) . 2_765 ?
O13 Ho2 O10 77.92(16) . 2_765 ?
O13 Ho2 O23 105.56(16) . . ?
O13 Ho2 C33 79.29(15) . 2_765 ?
O20 Ho2 O3 84.25(15) . . ?
O20 Ho2 O7 93.70(15) . 1_545 ?
O20 Ho2 O9 81.40(15) . 2_765 ?
O20 Ho2 O10 100.75(17) . 2_765 ?
O20 Ho2 O13 165.01(16) . . ?
O20 Ho2 O23 88.41(16) . . ?
O20 Ho2 C33 92.87(16) . 2_765 ?
O23 Ho2 O3 155.65(13) . . ?
O23 Ho2 O7 76.61(13) . 1_545 ?
O23 Ho2 O9 124.96(14) . 2_765 ?
O23 Ho2 O10 76.20(13) . 2_765 ?
O23 Ho2 C33 101.24(15) . 2_765 ?
O2 Ho3 O8 77.22(15) . 1_545 ?
O2 Ho3 O17 131.42(13) . 1_565 ?
O2 Ho3 O18 80.66(14) . 1_565 ?
O2 Ho3 O21 77.10(14) . 2_666 ?
O2 Ho3 O22 125.87(13) . 2_666 ?
O2 Ho3 C17 106.25(14) . 1_565 ?
O2 Ho3 C41 101.42(15) . 2_666 ?
O8 Ho3 O17 150.09(14) 1_545 1_565 ?
O8 Ho3 O21 80.96(14) 1_545 2_666 ?
O8 Ho3 O22 76.23(14) 1_545 2_666 ?
O8 Ho3 C17 163.21(13) 1_545 1_565 ?
O8 Ho3 C41 76.90(14) 1_545 2_666 ?
O14 Ho3 O2 76.97(15) . . ?
O14 Ho3 O8 114.84(15) . 1_545 ?
O14 Ho3 O17 84.40(16) . 1_565 ?
O14 Ho3 O18 80.78(15) . 1_565 ?
O14 Ho3 O21 145.38(14) . 2_666 ?
O14 Ho3 O22 157.10(15) . 2_666 ?
O14 Ho3 C17 81.84(16) . 1_565 ?
O14 Ho3 C41 167.00(15) . 2_666 ?
O17 Ho3 C17 25.89(13) 1_565 1_565 ?
O17 Ho3 C41 87.29(14) 1_565 2_666 ?
O18 Ho3 O8 148.72(14) 1_565 1_545 ?
O18 Ho3 O17 52.02(12) 1_565 1_565 ?
O18 Ho3 O21 72.71(14) 1_565 2_666 ?
O18 Ho3 O22 99.87(14) 1_565 2_666 ?
O18 Ho3 C17 26.12(13) 1_565 1_565 ?
O18 Ho3 C41 86.22(14) 1_565 2_666 ?
O21 Ho3 O17 95.99(14) 2_666 1_565 ?
O21 Ho3 C17 83.83(15) 2_666 1_565 ?
O21 Ho3 C41 26.24(14) 2_666 2_666 ?
O22 Ho3 O17 78.37(13) 2_666 1_565 ?
O22 Ho3 O21 52.73(13) 2_666 2_666 ?
O22 Ho3 C17 88.92(14) 2_666 1_565 ?
O22 Ho3 C41 26.50(14) 2_666 2_666 ?
O24 Ho3 O2 141.19(13) . . ?
O24 Ho3 O8 82.63(15) . 1_545 ?
O24 Ho3 O14 82.09(14) . . ?
O24 Ho3 O17 77.44(13) . 1_565 ?
O24 Ho3 O18 127.73(13) . 1_565 ?
O24 Ho3 O21 131.93(13) . 2_666 ?
O24 Ho3 O22 79.54(13) . 2_666 ?
O24 Ho3 C17 102.59(14) . 1_565 ?
O24 Ho3 C41 105.85(14) . 2_666 ?
C41 Ho3 C17 86.31(15) 2_666 1_565 ?
O4 Ho4 O19 115.95(15) . . ?
O4 Ho4 O28 88.50(16) . . ?
O4 Ho4 O29 74.94(16) . . ?
O6 Ho4 O4 83.52(18) 1_545 . ?
O6 Ho4 O11 82.18(15) 1_545 1_545 ?
O6 Ho4 O16 120.11(16) 1_545 1_545 ?
O6 Ho4 O19 75.62(17) 1_545 . ?
O6 Ho4 O28 142.54(15) 1_545 . ?
O6 Ho4 O29 142.00(17) 1_545 . ?
O11 Ho4 O4 95.80(14) 1_545 . ?
O11 Ho4 O16 78.17(14) 1_545 1_545 ?
O11 Ho4 O19 138.18(14) 1_545 . ?
O11 Ho4 O28 135.14(13) 1_545 . ?
O11 Ho4 O29 69.57(14) 1_545 . ?
O16 Ho4 O4 153.90(16) 1_545 . ?
O16 Ho4 O19 82.98(15) 1_545 . ?
O16 Ho4 O28 78.82(13) 1_545 . ?
O16 Ho4 O29 79.19(15) 1_545 . ?
O19 Ho4 O28 75.26(15) . . ?
O19 Ho4 O29 142.08(15) . . ?
O28 Ho4 O29 68.62(14) . . ?
C1 O1 Ho1 155.5(4) . . ?
C1 O2 Ho3 161.3(4) . . ?
C8 O3 Ho2 159.2(4) . . ?
C8 O4 Ho4 118.4(4) . . ?
C9 O5 Ho1 123.2(3) . . ?
C9 O6 Ho4 172.9(4) . 1_565 ?
C16 O7 Ho2 167.3(3) . 1_565 ?
C16 O8 Ho3 113.9(3) . 1_565 ?
C33 O9 Ho2 92.3(3) . 2_765 ?
C33 O10 Ho2 95.0(3) . 2_765 ?
C40 O11 Ho4 141.1(4) . 1_565 ?
C40 O12 Ho1 134.4(3) . . ?
C25 O13 Ho2 127.5(4) . . ?
C25 O14 Ho3 152.5(4) . . ?
C32 O15 Ho1 156.6(4) . . ?
C32 O16 Ho4 112.9(3) . 1_565 ?
C17 O17 Ho3 90.2(3) . 1_545 ?
C17 O18 Ho3 98.2(3) . 1_545 ?
C24 O19 Ho4 155.4(4) . . ?
C24 O20 Ho2 147.9(4) . . ?
C41 O21 Ho3 93.1(3) . 2_666 ?
C41 O22 Ho3 94.3(3) . 2_666 ?
C48 O23 Ho2 136.8(3) . . ?
C48 O24 Ho3 147.7(3) . . ?
Ho1 O25 H25A 120.1(11) . . ?
Ho1 O25 H25B 100(4) . . ?
H25A O25 H25B 106.0(16) . . ?
Ho1 O26 H26A 119.8 . . ?
Ho1 O26 H26B 120.2 . . ?
H26A O26 H26B 120.0 . . ?
Ho1 O27 H27A 119.9 . . ?
Ho1 O27 H27B 120.1 . . ?
H27A O27 H27B 120.0 . . ?
Ho4 O28 H28A 120.2 . . ?
Ho4 O28 H28B 119.9 . . ?
H28A O28 H28B 120.0 . . ?
C49 O29 Ho4 132.7(5) . . ?
C49 N1 C50 126.2(8) . . ?
C49 N1 C51 118.2(7) . . ?
C50 N1 C51 114.8(7) . . ?
O1 C1 C2 116.9(5) . . ?
O2 C1 O1 123.9(5) . . ?
O2 C1 C2 119.2(5) . . ?
C3 C2 C1 120.4(5) . . ?
C3 C2 C7 120.2(5) . . ?
C7 C2 C1 119.3(5) . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.4(5) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.6(5) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C8 121.3(5) . . ?
C7 C6 C5 118.7(5) . . ?
C7 C6 C8 120.1(5) . . ?
C2 C7 H7 119.6 . . ?
C6 C7 C2 120.8(5) . . ?
C6 C7 H7 119.6 . . ?
O3 C8 C6 119.9(5) . . ?
O4 C8 O3 122.2(5) . . ?
O4 C8 C6 117.9(5) . . ?
O5 C9 O6 124.4(5) . . ?
O5 C9 C10 117.7(5) . . ?
O6 C9 C10 117.8(5) . . ?
C11 C10 C9 120.7(4) . . ?
C11 C10 C15 119.0(4) . . ?
C15 C10 C9 120.2(4) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 C10 121.2(5) . . ?
C12 C11 H11 119.4 . . ?
C11 C12 H12 120.2 . . ?
C11 C12 C13 119.6(5) . . ?
C13 C12 H12 120.2 . . ?
C12 C13 H13 119.6 . . ?
C12 C13 C14 120.8(5) . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C16 120.6(4) . . ?
C15 C14 C13 118.1(4) . . ?
C15 C14 C16 121.4(4) . . ?
C10 C15 C14 121.3(4) . . ?
C10 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
O7 C16 O8 121.9(4) . . ?
O7 C16 C14 119.0(4) . . ?
O8 C16 C14 119.1(4) . . ?
O17 C17 Ho3 63.9(3) . 1_545 ?
O17 C17 O18 119.6(5) . . ?
O17 C17 C18 122.9(5) . . ?
O18 C17 Ho3 55.7(2) . 1_545 ?
O18 C17 C18 117.5(5) . . ?
C18 C17 Ho3 173.2(4) . 1_545 ?
C19 C18 C17 121.1(5) . . ?
C19 C18 C23 119.5(5) . . ?
C23 C18 C17 119.3(5) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.3(6) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.8(6) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 119.3 . . ?
C20 C21 C22 121.5(5) . . ?
C22 C21 H21 119.3 . . ?
C21 C22 C23 118.7(5) . . ?
C21 C22 C24 121.7(5) . . ?
C23 C22 C24 119.6(5) . . ?
C18 C23 H23 119.8 . . ?
C22 C23 C18 120.3(5) . . ?
C22 C23 H23 119.8 . . ?
O19 C24 O20 124.7(5) . . ?
O19 C24 C22 119.8(5) . . ?
O20 C24 C22 115.5(5) . . ?
O13 C25 O14 122.7(5) . . ?
O13 C25 C26 117.6(5) . . ?
O14 C25 C26 119.6(5) . . ?
C27 C26 C25 119.4(4) . . ?
C31 C26 C25 120.3(4) . . ?
C31 C26 C27 120.2(5) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 C26 119.7(5) . . ?
C28 C27 H27 120.2 . . ?
C27 C28 H28 119.7 . . ?
C29 C28 C27 120.6(5) . . ?
C29 C28 H28 119.7 . . ?
C28 C29 H29 120.2 . . ?
C28 C29 C30 119.6(5) . . ?
C30 C29 H29 120.2 . . ?
C29 C30 C32 118.2(5) . . ?
C31 C30 C29 119.9(5) . . ?
C31 C30 C32 121.8(5) . . ?
C26 C31 C30 120.0(5) . . ?
C26 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
O15 C32 C30 120.6(5) . . ?
O16 C32 O15 122.7(5) . . ?
O16 C32 C30 116.7(5) . . ?
O9 C33 Ho2 60.6(3) . 2_765 ?
O9 C33 C34 120.6(5) . . ?
O10 C33 Ho2 58.4(3) . 2_765 ?
O10 C33 O9 118.7(5) . . ?
O10 C33 C34 120.5(5) . . ?
C34 C33 Ho2 169.8(4) . 2_765 ?
C35 C34 C33 122.1(5) . . ?
C39 C34 C33 118.6(5) . . ?
C39 C34 C35 119.3(5) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 C34 120.7(5) . . ?
C36 C35 H35 119.6 . . ?
C35 C36 C37 119.5(5) . . ?
C35 C36 C40 120.0(4) . . ?
C37 C36 C40 120.4(5) . . ?
C36 C37 H37 120.1 . . ?
C36 C37 C38 119.9(5) . . ?
C38 C37 H37 120.1 . . ?
C37 C38 H38 119.8 . . ?
C39 C38 C37 120.4(5) . . ?
C39 C38 H38 119.8 . . ?
C34 C39 H39 119.9 . . ?
C38 C39 C34 120.1(5) . . ?
C38 C39 H39 119.9 . . ?
O11 C40 O12 125.1(5) . . ?
O11 C40 C36 118.5(4) . . ?
O12 C40 C36 116.4(5) . . ?
O21 C41 Ho3 60.7(3) . 2_666 ?
O21 C41 O22 119.9(5) . . ?
O21 C41 C42 120.9(5) . . ?
O22 C41 Ho3 59.2(3) . 2_666 ?
O22 C41 C42 119.2(5) . . ?
C42 C41 Ho3 178.0(4) . 2_666 ?
C43 C42 C41 121.3(5) . . ?
C47 C42 C41 120.1(5) . . ?
C47 C42 C43 118.6(5) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 C42 120.4(6) . . ?
C44 C43 H43 119.8 . . ?
C43 C44 H44 119.7 . . ?
C43 C44 C45 120.7(6) . . ?
C45 C44 H44 119.7 . . ?
C44 C45 H45 120.2 . . ?
C46 C45 C44 119.6(5) . . ?
C46 C45 H45 120.2 . . ?
C45 C46 C48 121.9(5) . . ?
C47 C46 C45 119.4(5) . . ?
C47 C46 C48 118.7(4) . . ?
C42 C47 H47 119.4 . . ?
C46 C47 C42 121.2(5) . . ?
C46 C47 H47 119.4 . . ?
O23 C48 O24 125.6(5) . . ?
O23 C48 C46 117.8(4) . . ?
O24 C48 C46 116.6(4) . . ?
O29 C49 N1 130.6(8) . . ?
O29 C49 H49 114.7 . . ?
N1 C49 H49 114.7 . . ?
N1 C50 H50A 109.5 . . ?
N1 C50 H50B 109.5 . . ?
N1 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N1 C51 H51A 109.5 . . ?
N1 C51 H51B 109.5 . . ?
N1 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C52 N2 C53 115.2(11) . . ?
C54 N2 C52 124.8(11) . . ?
C54 N2 C53 120.0(11) . . ?
O30 C52 N2 125.4(11) . . ?
O30 C52 H52 117.3 . . ?
N2 C52 H52 117.3 . . ?
N2 C53 H53A 109.5 . . ?
N2 C53 H53B 109.5 . . ?
N2 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N2 C54 H54A 109.5 . . ?
N2 C54 H54B 109.5 . . ?
N2 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
H31A O31 H31B 120.0 . . ?
H1AA O1A H1AB 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ho1 O1 C1 O2 4.8(12) . . . . ?
Ho1 O1 C1 C2 -175.2(6) . . . . ?
Ho1 O5 C9 O6 -23.3(8) . . . . ?
Ho1 O5 C9 C10 156.4(3) . . . . ?
Ho1 O12 C40 O11 57.8(8) . . . . ?
Ho1 O12 C40 C36 -121.5(5) . . . . ?
Ho1 O15 C32 O16 -111.9(8) . . . . ?
Ho1 O15 C32 C30 69.4(11) . . . . ?
Ho2 O3 C8 O4 -169.7(7) . . . . ?
Ho2 O3 C8 C6 10.4(14) . . . . ?
Ho2 O7 C16 O8 -148.3(14) 1_565 . . . ?
Ho2 O7 C16 C14 33.7(19) 1_565 . . . ?
Ho2 O9 C33 O10 6.6(6) 2_765 . . . ?
Ho2 O9 C33 C34 -168.3(4) 2_765 . . . ?
Ho2 O10 C33 O9 -6.8(6) 2_765 . . . ?
Ho2 O10 C33 C34 168.1(4) 2_765 . . . ?
Ho2 O13 C25 O14 -8.9(8) . . . . ?
Ho2 O13 C25 C26 171.6(3) . . . . ?
Ho2 O20 C24 O19 28.4(11) . . . . ?
Ho2 O20 C24 C22 -151.8(6) . . . . ?
Ho2 O23 C48 O24 48.5(8) . . . . ?
Ho2 O23 C48 C46 -132.0(4) . . . . ?
Ho2 C33 C34 C35 -106(2) 2_765 . . . ?
Ho2 C33 C34 C39 72(2) 2_765 . . . ?
Ho3 O2 C1 O1 69.2(13) . . . . ?
Ho3 O2 C1 C2 -110.8(11) . . . . ?
Ho3 O8 C16 O7 -9.7(7) 1_565 . . . ?
Ho3 O8 C16 C14 168.2(3) 1_565 . . . ?
Ho3 O14 C25 O13 87.0(9) . . . . ?
Ho3 O14 C25 C26 -93.5(9) . . . . ?
Ho3 O17 C17 O18 0.3(5) 1_545 . . . ?
Ho3 O17 C17 C18 -179.7(4) 1_545 . . . ?
Ho3 O18 C17 O17 -0.3(5) 1_545 . . . ?
Ho3 O18 C17 C18 179.7(4) 1_545 . . . ?
Ho3 O21 C41 O22 1.5(5) 2_666 . . . ?
Ho3 O21 C41 C42 -178.5(4) 2_666 . . . ?
Ho3 O22 C41 O21 -1.5(5) 2_666 . . . ?
Ho3 O22 C41 C42 178.5(4) 2_666 . . . ?
Ho3 O24 C48 O23 -41.8(10) . . . . ?
Ho3 O24 C48 C46 138.8(5) . . . . ?
Ho4 O4 C8 O3 -5.8(8) . . . . ?
Ho4 O4 C8 C6 174.1(4) . . . . ?
Ho4 O11 C40 O12 -61.5(8) 1_565 . . . ?
Ho4 O11 C40 C36 117.8(5) 1_565 . . . ?
Ho4 O16 C32 O15 -3.6(7) 1_565 . . . ?
Ho4 O16 C32 C30 175.1(3) 1_565 . . . ?
Ho4 O19 C24 O20 11.6(13) . . . . ?
Ho4 O19 C24 C22 -168.2(7) . . . . ?
Ho4 O29 C49 N1 160.9(7) . . . . ?
O1 C1 C2 C3 4.0(7) . . . . ?
O1 C1 C2 C7 -174.8(5) . . . . ?
O2 C1 C2 C3 -175.9(5) . . . . ?
O2 C1 C2 C7 5.2(7) . . . . ?
O5 C9 C10 C11 13.0(8) . . . . ?
O5 C9 C10 C15 -165.2(5) . . . . ?
O6 C9 C10 C11 -167.2(5) . . . . ?
O6 C9 C10 C15 14.5(8) . . . . ?
O9 C33 C34 C35 -12.5(8) . . . . ?
O9 C33 C34 C39 165.7(5) . . . . ?
O10 C33 C34 C35 172.7(5) . . . . ?
O10 C33 C34 C39 -9.1(8) . . . . ?
O13 C25 C26 C27 20.6(8) . . . . ?
O13 C25 C26 C31 -157.0(5) . . . . ?
O14 C25 C26 C27 -159.0(5) . . . . ?
O14 C25 C26 C31 23.5(8) . . . . ?
O17 C17 C18 C19 13.7(8) . . . . ?
O17 C17 C18 C23 -170.0(5) . . . . ?
O18 C17 C18 C19 -166.3(5) . . . . ?
O18 C17 C18 C23 10.1(7) . . . . ?
O21 C41 C42 C43 -17.6(9) . . . . ?
O21 C41 C42 C47 160.4(5) . . . . ?
O22 C41 C42 C43 162.3(6) . . . . ?
O22 C41 C42 C47 -19.6(8) . . . . ?
C1 C2 C3 C4 179.5(6) . . . . ?
C1 C2 C7 C6 -179.2(5) . . . . ?
C2 C3 C4 C5 -1.6(11) . . . . ?
C3 C2 C7 C6 2.0(8) . . . . ?
C3 C4 C5 C6 4.6(11) . . . . ?
C4 C5 C6 C7 -4.3(9) . . . . ?
C4 C5 C6 C8 175.9(6) . . . . ?
C5 C6 C7 C2 1.0(8) . . . . ?
C5 C6 C8 O3 -158.8(6) . . . . ?
C5 C6 C8 O4 21.4(8) . . . . ?
C7 C2 C3 C4 -1.7(9) . . . . ?
C7 C6 C8 O3 21.4(8) . . . . ?
C7 C6 C8 O4 -158.4(5) . . . . ?
C8 C6 C7 C2 -179.2(5) . . . . ?
C9 C10 C11 C12 -179.4(5) . . . . ?
C9 C10 C15 C14 178.2(5) . . . . ?
C10 C11 C12 C13 1.2(9) . . . . ?
C11 C10 C15 C14 -0.1(8) . . . . ?
C11 C12 C13 C14 0.1(9) . . . . ?
C12 C13 C14 C15 -1.3(8) . . . . ?
C12 C13 C14 C16 179.1(5) . . . . ?
C13 C14 C15 C10 1.3(8) . . . . ?
C13 C14 C16 O7 -175.2(5) . . . . ?
C13 C14 C16 O8 6.7(8) . . . . ?
C15 C10 C11 C12 -1.1(8) . . . . ?
C15 C14 C16 O7 5.2(8) . . . . ?
C15 C14 C16 O8 -172.8(5) . . . . ?
C16 C14 C15 C10 -179.1(5) . . . . ?
C17 C18 C19 C20 174.2(6) . . . . ?
C17 C18 C23 C22 -173.8(5) . . . . ?
C18 C19 C20 C21 0.6(11) . . . . ?
C19 C18 C23 C22 2.6(8) . . . . ?
C19 C20 C21 C22 0.7(11) . . . . ?
C20 C21 C22 C23 -0.2(10) . . . . ?
C20 C21 C22 C24 -177.2(6) . . . . ?
C21 C22 C23 C18 -1.4(8) . . . . ?
C21 C22 C24 O19 -163.4(6) . . . . ?
C21 C22 C24 O20 16.8(8) . . . . ?
C23 C18 C19 C20 -2.2(9) . . . . ?
C23 C22 C24 O19 19.7(8) . . . . ?
C23 C22 C24 O20 -160.1(5) . . . . ?
C24 C22 C23 C18 175.6(5) . . . . ?
C25 C26 C27 C28 -176.0(6) . . . . ?
C25 C26 C31 C30 175.2(5) . . . . ?
C26 C27 C28 C29 -0.1(10) . . . . ?
C27 C26 C31 C30 -2.3(8) . . . . ?
C27 C28 C29 C30 -0.4(10) . . . . ?
C28 C29 C30 C31 -0.4(9) . . . . ?
C28 C29 C30 C32 -176.9(6) . . . . ?
C29 C30 C31 C26 1.7(8) . . . . ?
C29 C30 C32 O15 -159.7(5) . . . . ?
C29 C30 C32 O16 21.5(7) . . . . ?
C31 C26 C27 C28 1.5(9) . . . . ?
C31 C30 C32 O15 23.8(8) . . . . ?
C31 C30 C32 O16 -155.0(5) . . . . ?
C32 C30 C31 C26 178.2(5) . . . . ?
C33 C34 C35 C36 176.0(5) . . . . ?
C33 C34 C39 C38 -174.9(6) . . . . ?
C34 C35 C36 C37 -0.6(8) . . . . ?
C34 C35 C36 C40 -177.1(5) . . . . ?
C35 C34 C39 C38 3.4(9) . . . . ?
C35 C36 C37 C38 2.3(9) . . . . ?
C35 C36 C40 O11 -30.6(7) . . . . ?
C35 C36 C40 O12 148.7(5) . . . . ?
C36 C37 C38 C39 -1.1(10) . . . . ?
C37 C36 C40 O11 152.9(5) . . . . ?
C37 C36 C40 O12 -27.7(7) . . . . ?
C37 C38 C39 C34 -1.7(10) . . . . ?
C39 C34 C35 C36 -2.2(8) . . . . ?
C40 C36 C37 C38 178.7(6) . . . . ?
C41 C42 C43 C44 177.5(7) . . . . ?
C41 C42 C47 C46 -179.5(5) . . . . ?
C42 C43 C44 C45 1.9(12) . . . . ?
C43 C42 C47 C46 -1.4(9) . . . . ?
C43 C44 C45 C46 -1.2(11) . . . . ?
C44 C45 C46 C47 -0.8(10) . . . . ?
C44 C45 C46 C48 176.3(6) . . . . ?
C45 C46 C47 C42 2.1(8) . . . . ?
C45 C46 C48 O23 -17.0(8) . . . . ?
C45 C46 C48 O24 162.5(5) . . . . ?
C47 C42 C43 C44 -0.6(10) . . . . ?
C47 C46 C48 O23 160.1(5) . . . . ?
C47 C46 C48 O24 -20.4(7) . . . . ?
C48 C46 C47 C42 -175.0(5) . . . . ?
C50 N1 C49 O29 175.5(9) . . . . ?
C51 N1 C49 O29 6.6(14) . . . . ?
C53 N2 C52 O30 -178.4(11) . . . . ?
C54 N2 C52 O30 4.6(18) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelxl_CCDC5
_audit_block_doi                 10.5517/cc1j7mr4
_database_code_depnum_ccdc_archive 'CCDC 1407516'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H39 Dy4 N O29, C3 H7 N O, H2 O'
_chemical_formula_sum            'C54 H48 Dy4 N2 O31'
_chemical_formula_weight         1870.94
_chemical_melting_point          ?
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'
Dy Dy -0.1892 4.4098 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.830(2)
_cell_length_b                   14.130(3)
_cell_length_c                   20.070(4)
_cell_angle_alpha                86.10(3)
_cell_angle_beta                 83.59(3)
_cell_angle_gamma                78.31(3)
_cell_volume                     2985.5(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8861
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.044
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.993
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1141
_diffrn_reflns_av_unetI/netI     0.1129
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30302
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         3.067
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 18.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.0801
	          2theta: 29.9072
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 18.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.0801
	          2theta: 29.9072
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 18.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.0801
	          2theta: 29.9072
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.091292
_diffrn_orient_matrix_UB_12      -0.007655
_diffrn_orient_matrix_UB_13      0.024061
_diffrn_orient_matrix_UB_21      0.012949
_diffrn_orient_matrix_UB_22      -0.065545
_diffrn_orient_matrix_UB_23      -0.027741
_diffrn_orient_matrix_UB_31      0.018146
_diffrn_orient_matrix_UB_32      -0.012874
_diffrn_orient_matrix_UB_33      0.044993
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12051
_reflns_number_total             13572
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.427
_refine_diff_density_min         -2.138
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         13572
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0424
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0172P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1092
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Riding coordinates:
 O25(H25A,H25B), O26(H26A,H26B), O27(H27A,H27B), O28(H28A,H28B), O31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13), C15(H15),
 C19(H19), C20(H20), C21(H21), C23(H23), C27(H27), C28(H28), C29(H29), C31(H31),
  C35(H35), C36(H36), C37(H37), C39(H39), C43(H43), C44(H44), C45(H45),
 C47(H47), C49(H49), C52(H52)
2.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.28674(2) 0.44567(2) 0.17242(2) 0.01551(7) Uani 1 1 d . . . . .
Dy2 Dy -0.08813(2) 0.23688(2) 0.19652(2) 0.01659(7) Uani 1 1 d . . . . .
Dy3 Dy 0.27177(2) 0.69266(2) 0.30936(2) 0.01531(7) Uani 1 1 d . . . . .
Dy4 Dy -0.04623(2) 0.98823(2) 0.35254(2) 0.02034(8) Uani 1 1 d . . . . .
O1 O -0.1347(4) 0.8523(3) 0.3498(3) 0.0423(12) Uani 1 1 d . . . . .
O2 O 0.0574(4) 0.7677(3) 0.3248(2) 0.0284(9) Uani 1 1 d . . . . .
O3 O 0.0716(4) 0.4658(3) 0.2033(2) 0.0276(9) Uani 1 1 d . . . . .
O4 O -0.0786(4) 0.3816(3) 0.2323(2) 0.0293(9) Uani 1 1 d . . . . .
O5 O 0.1673(4) -0.0260(3) 0.3104(2) 0.0351(11) Uani 1 1 d . . . . .
O6 O 0.3018(4) -0.1580(3) 0.2766(2) 0.0365(11) Uani 1 1 d . . . . .
O7 O 0.2752(4) 0.2807(3) 0.2032(2) 0.0304(10) Uani 1 1 d . . . . .
O8 O 0.4700(4) 0.3016(3) 0.1922(2) 0.0281(9) Uani 1 1 d . . . . .
O9 O 0.2032(4) 0.3822(4) 0.0780(2) 0.0388(12) Uani 1 1 d . . . . .
O10 O 0.3895(4) 0.4204(3) 0.0586(2) 0.0277(9) Uani 1 1 d . . . . .
O11 O 0.4547(3) 0.5173(3) 0.1786(2) 0.0239(9) Uani 1 1 d . . . . .
O12 O 0.4592(3) 0.6320(3) 0.2495(2) 0.0267(9) Uani 1 1 d . . . . .
O13 O 0.2097(4) 0.5944(3) 0.1124(2) 0.0294(10) Uani 1 1 d . . . . .
O14 O 0.2098(4) 0.6641(3) 0.2075(2) 0.0271(9) Uani 1 1 d . . . . .
O15 O -0.0493(5) 0.9934(4) 0.2405(2) 0.0455(13) Uani 1 1 d . . . . .
O16 O -0.0906(4) 1.0904(3) 0.1502(2) 0.0311(10) Uani 1 1 d . . . . .
O17 O 0.2067(4) 0.5622(3) 0.3644(2) 0.0352(11) Uani 1 1 d . . . . .
O18 O 0.2719(4) 0.4555(4) 0.2859(2) 0.0336(11) Uani 1 1 d . . . . .
O19 O 0.0030(4) 0.1880(3) 0.3011(2) 0.0307(10) Uani 1 1 d . . . . .
O20 O -0.0065(4) 0.1194(3) 0.4035(2) 0.0321(10) Uani 1 1 d . . . . .
O21 O -0.2517(4) 0.2404(4) 0.5804(2) 0.0366(12) Uani 1 1 d . . . . .
O22 O -0.4177(4) 0.3482(4) 0.6068(2) 0.0392(12) Uani 1 1 d . . . . .
O23 O -0.2336(4) 0.0984(3) 0.3453(2) 0.0269(9) Uani 1 1 d . . . . .
O24 O -0.2580(4) 0.2200(3) 0.26820(19) 0.0269(9) Uani 1 1 d . . . . .
O25 O 0.1219(4) 0.1827(3) 0.1577(2) 0.0353(11) Uani 1 1 d . . . . .
H25A H 0.153350 0.207975 0.121807 0.053 Uiso 1 1 d R . . . .
H25B H 0.167740 0.137675 0.179387 0.053 Uiso 1 1 d R . . . .
O26 O -0.0393(4) 0.3305(4) 0.0913(2) 0.0404(12) Uani 1 1 d . . . . .
H26A H 0.026613 0.355238 0.086122 0.061 Uiso 1 1 d R . . . .
H26B H -0.088547 0.337929 0.060352 0.061 Uiso 1 1 d R . . . .
O27 O -0.2738(4) 0.2951(4) 0.1439(2) 0.0373(12) Uani 1 1 d . . . . .
H27A H -0.270629 0.328549 0.107163 0.056 Uiso 1 1 d R . . . .
H27B H -0.344179 0.282639 0.161583 0.056 Uiso 1 1 d R . . . .
O28 O 0.0679(4) 0.9112(3) 0.4409(2) 0.0302(10) Uani 1 1 d . . . . .
H28A H 0.030049 0.905693 0.479972 0.045 Uiso 1 1 d R . . . .
H28B H 0.146939 0.889003 0.433692 0.045 Uiso 1 1 d R . . . .
O29 O -0.1859(4) 0.9854(3) 0.4587(2) 0.0380(11) Uani 1 1 d . . . . .
N1 N -0.3268(6) 0.9264(6) 0.5340(4) 0.0536(18) Uani 1 1 d . . . . .
C1 C -0.0610(6) 0.7744(4) 0.3335(3) 0.0260(13) Uani 1 1 d . . . . .
C2 C -0.1185(5) 0.6890(4) 0.3250(3) 0.0232(12) Uani 1 1 d . . . . .
C3 C -0.2394(6) 0.6823(5) 0.3555(4) 0.0351(16) Uani 1 1 d . . . . .
H3 H -0.287153 0.733465 0.379656 0.042 Uiso 1 1 calc R . . . .
C4 C -0.2880(6) 0.6014(6) 0.3502(4) 0.0440(19) Uani 1 1 d . . . . .
H4 H -0.366462 0.596464 0.372712 0.053 Uiso 1 1 calc R . . . .
C5 C -0.2206(6) 0.5263(5) 0.3112(3) 0.0327(15) Uani 1 1 d . . . . .
H5 H -0.254232 0.471544 0.307558 0.039 Uiso 1 1 calc R . . . .
C6 C -0.1025(5) 0.5333(4) 0.2776(3) 0.0207(11) Uani 1 1 d . . . . .
C7 C -0.0523(5) 0.6132(4) 0.2856(3) 0.0203(11) Uani 1 1 d . . . . .
H7 H 0.027525 0.617051 0.264344 0.024 Uiso 1 1 calc R . . . .
C8 C -0.0315(5) 0.4556(4) 0.2347(3) 0.0199(11) Uani 1 1 d . . . . .
C9 C 0.2725(6) -0.0682(4) 0.2847(3) 0.0243(12) Uani 1 1 d . . . . .
C10 C 0.3725(5) -0.0108(4) 0.2609(3) 0.0229(12) Uani 1 1 d . . . . .
C11 C 0.4981(6) -0.0572(5) 0.2480(4) 0.0353(15) Uani 1 1 d . . . . .
H11 H 0.520561 -0.123904 0.255222 0.042 Uiso 1 1 calc R . . . .
C12 C 0.5907(6) -0.0040(5) 0.2243(5) 0.054(2) Uani 1 1 d . . . . .
H12 H 0.674777 -0.035199 0.216136 0.065 Uiso 1 1 calc R . . . .
C13 C 0.5576(6) 0.0946(5) 0.2129(4) 0.0353(16) Uani 1 1 d . . . . .
H13 H 0.620041 0.129688 0.197850 0.042 Uiso 1 1 calc R . . . .
C14 C 0.4314(5) 0.1426(4) 0.2238(3) 0.0219(12) Uani 1 1 d . . . . .
C15 C 0.3412(5) 0.0883(4) 0.2495(3) 0.0221(12) Uani 1 1 d . . . . .
H15 H 0.257529 0.119697 0.259142 0.027 Uiso 1 1 calc R . . . .
C16 C 0.3922(5) 0.2473(4) 0.2058(3) 0.0204(11) Uani 1 1 d . . . . .
C17 C 0.2997(5) 0.3913(4) 0.0380(3) 0.0243(12) Uani 1 1 d . . . . .
C18 C 0.3062(6) 0.3664(5) -0.0340(3) 0.0296(14) Uani 1 1 d . . . . .
C19 C 0.2320(7) 0.3061(7) -0.0539(4) 0.054(2) Uani 1 1 d . . . . .
H19 H 0.177878 0.279586 -0.022056 0.065 Uiso 1 1 calc R . . . .
C20 C 0.2382(8) 0.2848(7) -0.1220(4) 0.057(2) Uani 1 1 d . . . . .
H20 H 0.182532 0.249854 -0.136153 0.068 Uiso 1 1 calc R . . . .
C21 C 0.3291(6) 0.3171(5) -0.1677(3) 0.0373(16) Uani 1 1 d . . . . .
H21 H 0.339496 0.298103 -0.211808 0.045 Uiso 1 1 calc R . . . .
C22 C 0.4045(5) 0.3772(4) -0.1485(3) 0.0215(12) Uani 1 1 d . . . . .
C23 C 0.3927(5) 0.4021(4) -0.0813(3) 0.0208(11) Uani 1 1 d . . . . .
H23 H 0.442487 0.442542 -0.068108 0.025 Uiso 1 1 calc R . . . .
C24 C 0.4964(5) 0.5881(4) 0.1955(3) 0.0181(11) Uani 1 1 d . . . . .
C25 C 0.1815(5) 0.6665(4) 0.1487(3) 0.0205(11) Uani 1 1 d . . . . .
C26 C 0.1047(5) 0.7599(4) 0.1206(3) 0.0180(11) Uani 1 1 d . . . . .
C27 C 0.0754(5) 0.7673(4) 0.0540(3) 0.0235(12) Uani 1 1 d . . . . .
H27 H 0.104295 0.714916 0.026849 0.028 Uiso 1 1 calc R . . . .
C28 C 0.0055(6) 0.8499(5) 0.0283(3) 0.0310(14) Uani 1 1 d . . . . .
H28 H -0.013477 0.853104 -0.015971 0.037 Uiso 1 1 calc R . . . .
C29 C -0.0380(6) 0.9299(4) 0.0676(3) 0.0249(12) Uani 1 1 d . . . . .
H29 H -0.084495 0.986678 0.049682 0.030 Uiso 1 1 calc R . . . .
C30 C -0.0104(5) 0.9233(4) 0.1348(3) 0.0216(12) Uani 1 1 d . . . . .
C31 C 0.0607(5) 0.8383(4) 0.1612(3) 0.0191(11) Uani 1 1 d . . . . .
H31 H 0.078609 0.833971 0.205707 0.023 Uiso 1 1 calc R . . . .
C32 C -0.0524(5) 1.0087(5) 0.1781(3) 0.0259(13) Uani 1 1 d . . . . .
C33 C 0.0117(5) 0.1888(4) 0.3632(3) 0.0221(12) Uani 1 1 d . . . . .
C34 C 0.0465(5) 0.2723(4) 0.3929(3) 0.0209(11) Uani 1 1 d . . . . .
C35 C 0.0152(6) 0.2870(5) 0.4611(3) 0.0340(15) Uani 1 1 d . . . . .
H35 H -0.030494 0.246116 0.486896 0.041 Uiso 1 1 calc R . . . .
C36 C 0.0505(7) 0.3608(5) 0.4911(3) 0.0365(16) Uani 1 1 d . . . . .
H36 H 0.029729 0.368965 0.536815 0.044 Uiso 1 1 calc R . . . .
C37 C 0.1176(6) 0.4232(5) 0.4524(3) 0.0314(14) Uani 1 1 d . . . . .
H37 H 0.141343 0.473445 0.472331 0.038 Uiso 1 1 calc R . . . .
C38 C 0.1486(5) 0.4101(4) 0.3844(3) 0.0204(11) Uani 1 1 d . . . . .
C39 C 0.1150(5) 0.3342(4) 0.3543(3) 0.0196(11) Uani 1 1 d . . . . .
H39 H 0.138074 0.324685 0.308887 0.024 Uiso 1 1 calc R . . . .
C40 C 0.2149(5) 0.4792(4) 0.3417(3) 0.0236(12) Uani 1 1 d . . . . .
C41 C -0.3499(5) 0.2957(4) 0.5638(3) 0.0233(12) Uani 1 1 d . . . . .
C42 C -0.3842(5) 0.3028(4) 0.4931(3) 0.0227(12) Uani 1 1 d . . . . .
C43 C -0.4776(6) 0.3781(5) 0.4744(3) 0.0312(14) Uani 1 1 d . . . . .
H43 H -0.524076 0.419045 0.506601 0.037 Uiso 1 1 calc R . . . .
C44 C -0.5032(6) 0.3937(5) 0.4072(4) 0.0382(17) Uani 1 1 d . . . . .
H44 H -0.564692 0.445922 0.394617 0.046 Uiso 1 1 calc R . . . .
C45 C -0.4372(5) 0.3315(5) 0.3597(3) 0.0280(13) Uani 1 1 d . . . . .
H45 H -0.452153 0.342659 0.314876 0.034 Uiso 1 1 calc R . . . .
C46 C -0.3484(5) 0.2525(4) 0.3792(3) 0.0200(11) Uani 1 1 d . . . . .
C47 C -0.3200(5) 0.2378(4) 0.4458(3) 0.0213(11) Uani 1 1 d . . . . .
H47 H -0.258961 0.185208 0.458350 0.026 Uiso 1 1 calc R . . . .
C48 C -0.2747(5) 0.1846(4) 0.3279(3) 0.0203(11) Uani 1 1 d . . . . .
C49 C -0.2313(7) 0.9198(6) 0.4892(4) 0.052(2) Uani 1 1 d . . . . .
H49 H -0.191278 0.857316 0.478435 0.062 Uiso 1 1 calc R . . . .
C50 C -0.3838(9) 1.0213(8) 0.5611(5) 0.074(3) Uani 1 1 d . . . . .
H50A H -0.382997 1.070613 0.525761 0.110 Uiso 1 1 calc GR . . . .
H50B H -0.335978 1.033947 0.595801 0.110 Uiso 1 1 calc GR . . . .
H50C H -0.469610 1.021248 0.579257 0.110 Uiso 1 1 calc GR . . . .
C51 C -0.3724(10) 0.8478(8) 0.5695(6) 0.087(4) Uani 1 1 d . . . . .
H51A H -0.365684 0.850694 0.616544 0.131 Uiso 1 1 calc GR . . . .
H51B H -0.322770 0.787887 0.553525 0.131 Uiso 1 1 calc GR . . . .
H51C H -0.459454 0.851694 0.562260 0.131 Uiso 1 1 calc GR . . . .
O30 O 0.2424(7) 1.0652(6) 0.0618(4) 0.087(2) Uani 1 1 d . . . . .
N2 N 0.3599(7) 0.9186(6) 0.0427(5) 0.073(3) Uani 1 1 d . . . . .
C52 C 0.2905(9) 0.9901(8) 0.0828(7) 0.079(3) Uani 1 1 d . . . . .
H52 H 0.282041 0.977400 0.129029 0.094 Uiso 1 1 calc R . . . .
C53 C 0.4183(13) 0.8296(9) 0.0766(8) 0.127(6) Uani 1 1 d . . . . .
H53A H 0.502396 0.833852 0.085284 0.190 Uiso 1 1 calc GR . . . .
H53B H 0.422543 0.776303 0.048662 0.190 Uiso 1 1 calc GR . . . .
H53C H 0.368771 0.819727 0.118272 0.190 Uiso 1 1 calc GR . . . .
C54 C 0.3769(13) 0.9245(12) -0.0279(7) 0.127(6) Uani 1 1 d . . . . .
H54A H 0.321343 0.889489 -0.045377 0.190 Uiso 1 1 calc GR . . . .
H54B H 0.463236 0.896902 -0.042930 0.190 Uiso 1 1 calc GR . . . .
H54C H 0.357877 0.991048 -0.043559 0.190 Uiso 1 1 calc GR . . . .
O31 O 0.6536(5) 0.3649(4) 0.0228(2) 0.0508(15) Uani 1 1 d . . . . .
H31A H 0.625135 0.411688 -0.003712 0.076 Uiso 1 1 d R . . . .
H31B H 0.678995 0.308398 0.008328 0.076 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
Dy1 O3 2.308(4) . ?
Dy1 O7 2.395(4) . ?
Dy1 O8 2.583(4) . ?
Dy1 O9 2.482(4) . ?
Dy1 O10 2.444(4) . ?
Dy1 O11 2.272(4) . ?
Dy1 O13 2.394(4) . ?
Dy1 O18 2.277(4) . ?
Dy2 O4 2.238(4) . ?
Dy2 O16 2.332(4) 1_545 ?
Dy2 O19 2.417(4) . ?
Dy2 O24 2.248(4) . ?
Dy2 O25 2.312(4) . ?
Dy2 O26 2.479(5) . ?
Dy2 O27 2.350(4) . ?
Dy3 O2 2.345(4) . ?
Dy3 O6 2.244(4) 1_565 ?
Dy3 O12 2.278(4) . ?
Dy3 O14 2.306(4) . ?
Dy3 O17 2.279(4) . ?
Dy3 O21 2.435(4) 2_566 ?
Dy3 O22 2.398(4) 2_566 ?
Dy3 C41 2.796(6) 2_566 ?
Dy4 O1 2.320(5) . ?
Dy4 O5 2.345(4) 1_565 ?
Dy4 O15 2.249(5) . ?
Dy4 O20 2.312(4) 1_565 ?
Dy4 O23 2.306(4) 1_565 ?
Dy4 O28 2.353(4) . ?
Dy4 O29 2.475(4) . ?
O1 C1 1.260(7) . ?
O2 C1 1.259(7) . ?
O3 C8 1.249(7) . ?
O4 C8 1.259(7) . ?
O5 C9 1.247(7) . ?
O6 C9 1.260(7) . ?
O7 C16 1.266(6) . ?
O8 C16 1.247(7) . ?
O9 C17 1.267(7) . ?
O10 C17 1.248(7) . ?
O11 C24 1.259(7) . ?
O12 C24 1.269(6) . ?
O13 C25 1.260(7) . ?
O14 C25 1.249(7) . ?
O15 C32 1.258(7) . ?
O16 C32 1.260(7) . ?
O17 C40 1.269(8) . ?
O18 C40 1.250(7) . ?
O19 C33 1.262(7) . ?
O20 C33 1.261(7) . ?
O21 C41 1.249(7) . ?
O22 C41 1.250(7) . ?
O23 C48 1.250(7) . ?
O24 C48 1.274(7) . ?
O25 H25A 0.8502 . ?
O25 H25B 0.8499 . ?
O26 H26A 0.8498 . ?
O26 H26B 0.8501 . ?
O27 H27A 0.8499 . ?
O27 H27B 0.8499 . ?
O28 H28A 0.8500 . ?
O28 H28B 0.8500 . ?
O29 C49 1.231(9) . ?
N1 C49 1.285(9) . ?
N1 C50 1.470(12) . ?
N1 C51 1.421(11) . ?
C1 C2 1.493(8) . ?
C2 C3 1.401(8) . ?
C2 C7 1.402(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.366(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.394(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.396(8) . ?
C6 C7 1.375(8) . ?
C6 C8 1.476(8) . ?
C7 H7 0.9300 . ?
C9 C10 1.500(8) . ?
C10 C11 1.389(8) . ?
C10 C15 1.382(8) . ?
C11 H11 0.9300 . ?
C11 C12 1.395(10) . ?
C12 H12 0.9300 . ?
C12 C13 1.376(10) . ?
C13 H13 0.9300 . ?
C13 C14 1.398(8) . ?
C14 C15 1.395(8) . ?
C14 C16 1.485(8) . ?
C15 H15 0.9300 . ?
C17 C18 1.502(8) . ?
C18 C19 1.388(9) . ?
C18 C23 1.400(8) . ?
C19 H19 0.9300 . ?
C19 C20 1.412(10) . ?
C20 H20 0.9300 . ?
C20 C21 1.394(9) . ?
C21 H21 0.9300 . ?
C21 C22 1.391(8) . ?
C22 C23 1.403(8) . ?
C22 C24 1.485(7) 2_665 ?
C23 H23 0.9300 . ?
C25 C26 1.520(7) . ?
C26 C27 1.401(7) . ?
C26 C31 1.393(7) . ?
C27 H27 0.9300 . ?
C27 C28 1.359(8) . ?
C28 H28 0.9300 . ?
C28 C29 1.394(8) . ?
C29 H29 0.9300 . ?
C29 C30 1.407(8) . ?
C30 C31 1.395(8) . ?
C30 C32 1.500(8) . ?
C31 H31 0.9300 . ?
C33 C34 1.490(8) . ?
C34 C35 1.391(8) . ?
C34 C39 1.399(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.375(9) . ?
C36 H36 0.9300 . ?
C36 C37 1.396(9) . ?
C37 H37 0.9300 . ?
C37 C38 1.386(8) . ?
C38 C39 1.393(8) . ?
C38 C40 1.495(8) . ?
C39 H39 0.9300 . ?
C41 C42 1.498(8) . ?
C42 C43 1.375(8) . ?
C42 C47 1.394(8) . ?
C43 H43 0.9300 . ?
C43 C44 1.402(9) . ?
C44 H44 0.9300 . ?
C44 C45 1.377(9) . ?
C45 H45 0.9300 . ?
C45 C46 1.383(8) . ?
C46 C47 1.397(8) . ?
C46 C48 1.502(8) . ?
C47 H47 0.9300 . ?
C49 H49 0.9300 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
O30 C52 1.157(12) . ?
N2 C52 1.379(13) . ?
N2 C53 1.450(15) . ?
N2 C54 1.408(15) . ?
C52 H52 0.9300 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
O31 H31A 0.8501 . ?
O31 H31B 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
O3 Dy1 O7 81.17(15) . . ?
O3 Dy1 O8 131.22(14) . . ?
O3 Dy1 O9 75.79(15) . . ?
O3 Dy1 O10 125.38(14) . . ?
O3 Dy1 O13 78.76(15) . . ?
O7 Dy1 O8 51.64(13) . . ?
O7 Dy1 O9 73.27(16) . . ?
O7 Dy1 O10 97.65(16) . . ?
O9 Dy1 O8 98.34(16) . . ?
O10 Dy1 O8 78.32(14) . . ?
O10 Dy1 O9 52.54(13) . . ?
O11 Dy1 O3 141.59(14) . . ?
O11 Dy1 O7 126.64(14) . . ?
O11 Dy1 O8 76.44(14) . . ?
O11 Dy1 O9 132.92(14) . . ?
O11 Dy1 O10 81.00(14) . . ?
O11 Dy1 O13 82.18(15) . . ?
O11 Dy1 O18 81.46(15) . . ?
O13 Dy1 O7 149.84(15) . . ?
O13 Dy1 O8 149.04(14) . . ?
O13 Dy1 O9 80.11(16) . . ?
O13 Dy1 O10 76.41(15) . . ?
O18 Dy1 O3 76.85(15) . . ?
O18 Dy1 O7 81.82(17) . . ?
O18 Dy1 O8 84.06(16) . . ?
O18 Dy1 O9 145.30(15) . . ?
O18 Dy1 O10 157.57(14) . . ?
O18 Dy1 O13 114.79(16) . . ?
O4 Dy2 O16 175.09(16) . 1_545 ?
O4 Dy2 O19 79.85(16) . . ?
O4 Dy2 O24 94.03(16) . . ?
O4 Dy2 O25 100.41(16) . . ?
O4 Dy2 O26 76.69(16) . . ?
O4 Dy2 O27 94.16(17) . . ?
O16 Dy2 O19 103.51(15) 1_545 . ?
O16 Dy2 O26 98.49(17) 1_545 . ?
O16 Dy2 O27 84.98(17) 1_545 . ?
O19 Dy2 O26 138.01(15) . . ?
O24 Dy2 O16 90.24(17) . 1_545 ?
O24 Dy2 O19 77.21(14) . . ?
O24 Dy2 O25 149.63(17) . . ?
O24 Dy2 O26 138.35(15) . . ?
O24 Dy2 O27 70.45(15) . . ?
O25 Dy2 O16 76.91(16) . 1_545 ?
O25 Dy2 O19 79.23(16) . . ?
O25 Dy2 O26 71.50(17) . . ?
O25 Dy2 O27 134.00(16) . . ?
O27 Dy2 O19 146.62(15) . . ?
O27 Dy2 O26 69.89(15) . . ?
O2 Dy3 O21 76.83(14) . 2_566 ?
O2 Dy3 O22 127.47(14) . 2_566 ?
O2 Dy3 C41 101.78(15) . 2_566 ?
O6 Dy3 O2 84.17(16) 1_565 . ?
O6 Dy3 O12 88.60(17) 1_565 . ?
O6 Dy3 O14 93.78(17) 1_565 . ?
O6 Dy3 O17 164.94(17) 1_565 . ?
O6 Dy3 O21 81.45(18) 1_565 2_566 ?
O6 Dy3 O22 100.28(19) 1_565 2_566 ?
O6 Dy3 C41 92.64(18) 1_565 2_566 ?
O12 Dy3 O2 155.95(15) . . ?
O12 Dy3 O14 77.12(14) . . ?
O12 Dy3 O17 105.43(17) . . ?
O12 Dy3 O21 124.74(14) . 2_566 ?
O12 Dy3 O22 76.38(14) . 2_566 ?
O12 Dy3 C41 101.43(15) . 2_566 ?
O14 Dy3 O2 80.50(14) . . ?
O14 Dy3 O21 157.18(13) . 2_566 ?
O14 Dy3 O22 149.55(14) . 2_566 ?
O14 Dy3 C41 173.37(16) . 2_566 ?
O17 Dy3 O2 84.96(17) . . ?
O17 Dy3 O14 94.68(16) . . ?
O17 Dy3 O21 85.95(18) . 2_566 ?
O17 Dy3 O22 78.27(18) . 2_566 ?
O17 Dy3 C41 79.41(17) . 2_566 ?
O21 Dy3 C41 26.49(14) 2_566 2_566 ?
O22 Dy3 O21 52.81(14) 2_566 2_566 ?
O22 Dy3 C41 26.44(15) 2_566 2_566 ?
O1 Dy4 O5 116.80(16) . 1_565 ?
O1 Dy4 O28 88.81(18) . . ?
O1 Dy4 O29 74.78(18) . . ?
O5 Dy4 O28 75.34(16) 1_565 . ?
O5 Dy4 O29 142.15(17) 1_565 . ?
O15 Dy4 O1 83.9(2) . . ?
O15 Dy4 O5 75.79(18) . 1_565 ?
O15 Dy4 O20 119.71(19) . 1_565 ?
O15 Dy4 O23 81.81(16) . 1_565 ?
O15 Dy4 O28 142.96(16) . . ?
O15 Dy4 O29 141.88(18) . . ?
O20 Dy4 O1 153.69(18) 1_565 . ?
O20 Dy4 O5 82.49(16) 1_565 1_565 ?
O20 Dy4 O28 78.63(15) 1_565 . ?
O20 Dy4 O29 79.13(16) 1_565 . ?
O23 Dy4 O1 95.47(16) 1_565 . ?
O23 Dy4 O5 137.78(16) 1_565 1_565 ?
O23 Dy4 O20 78.22(15) 1_565 1_565 ?
O23 Dy4 O28 135.13(15) 1_565 . ?
O23 Dy4 O29 69.44(15) 1_565 . ?
O28 Dy4 O29 68.77(15) . . ?
C1 O1 Dy4 117.4(4) . . ?
C1 O2 Dy3 157.9(4) . . ?
C8 O3 Dy1 160.6(4) . . ?
C8 O4 Dy2 155.2(4) . . ?
C9 O5 Dy4 155.7(4) . 1_545 ?
C9 O6 Dy3 148.4(4) . 1_545 ?
C16 O7 Dy1 98.4(3) . . ?
C16 O8 Dy1 90.0(3) . . ?
C17 O9 Dy1 92.5(4) . . ?
C17 O10 Dy1 94.8(3) . . ?
C24 O11 Dy1 148.7(3) . . ?
C24 O12 Dy3 137.8(3) . . ?
C25 O13 Dy1 113.6(4) . . ?
C25 O14 Dy3 167.4(4) . . ?
C32 O15 Dy4 172.1(5) . . ?
C32 O16 Dy2 123.9(4) . 1_565 ?
C40 O17 Dy3 127.1(4) . . ?
C40 O18 Dy1 153.9(4) . . ?
C33 O19 Dy2 156.3(4) . . ?
C33 O20 Dy4 113.9(4) . 1_545 ?
C41 O21 Dy3 93.1(3) . 2_566 ?
C41 O22 Dy3 94.8(3) . 2_566 ?
C48 O23 Dy4 141.2(4) . 1_545 ?
C48 O24 Dy2 135.0(3) . . ?
Dy2 O25 H25A 119.9 . . ?
Dy2 O25 H25B 120.1 . . ?
H25A O25 H25B 120.0 . . ?
Dy2 O26 H26A 120.0 . . ?
Dy2 O26 H26B 120.0 . . ?
H26A O26 H26B 120.0 . . ?
Dy2 O27 H27A 119.9 . . ?
Dy2 O27 H27B 120.1 . . ?
H27A O27 H27B 120.0 . . ?
Dy4 O28 H28A 120.0 . . ?
Dy4 O28 H28B 120.0 . . ?
H28A O28 H28B 120.0 . . ?
C49 O29 Dy4 131.5(5) . . ?
C49 N1 C50 119.1(8) . . ?
C49 N1 C51 126.1(9) . . ?
C51 N1 C50 114.0(7) . . ?
O1 C1 C2 117.8(5) . . ?
O2 C1 O1 121.8(6) . . ?
O2 C1 C2 120.5(5) . . ?
C3 C2 C1 121.5(5) . . ?
C3 C2 C7 118.1(5) . . ?
C7 C2 C1 120.4(5) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.7(5) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.3(6) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0(6) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C8 120.7(5) . . ?
C7 C6 C5 119.2(5) . . ?
C7 C6 C8 120.2(5) . . ?
C2 C7 H7 119.2 . . ?
C6 C7 C2 121.5(5) . . ?
C6 C7 H7 119.2 . . ?
O3 C8 O4 123.5(5) . . ?
O3 C8 C6 119.1(5) . . ?
O4 C8 C6 117.5(5) . . ?
O5 C9 O6 124.2(6) . . ?
O5 C9 C10 119.5(5) . . ?
O6 C9 C10 116.3(6) . . ?
C11 C10 C9 120.2(5) . . ?
C15 C10 C9 120.8(5) . . ?
C15 C10 C11 118.9(6) . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.2(6) . . ?
C12 C11 H11 119.9 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 120.1(6) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 119.6 . . ?
C12 C13 C14 120.8(6) . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C16 121.6(5) . . ?
C15 C14 C13 118.0(6) . . ?
C15 C14 C16 120.4(5) . . ?
C10 C15 C14 121.9(5) . . ?
C10 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
O7 C16 C14 117.6(5) . . ?
O8 C16 O7 119.9(5) . . ?
O8 C16 C14 122.5(5) . . ?
O9 C17 C18 119.8(5) . . ?
O10 C17 O9 120.2(6) . . ?
O10 C17 C18 120.0(5) . . ?
C19 C18 C17 121.4(5) . . ?
C19 C18 C23 119.7(6) . . ?
C23 C18 C17 118.9(5) . . ?
C18 C19 H19 119.8 . . ?
C18 C19 C20 120.5(6) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 120.6 . . ?
C21 C20 C19 118.8(6) . . ?
C21 C20 H20 120.6 . . ?
C20 C21 H21 119.4 . . ?
C22 C21 C20 121.1(6) . . ?
C22 C21 H21 119.4 . . ?
C21 C22 C23 119.3(5) . . ?
C21 C22 C24 122.6(5) . 2_665 ?
C23 C22 C24 117.9(5) . 2_665 ?
C18 C23 C22 120.3(5) . . ?
C18 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
O11 C24 O12 124.6(5) . . ?
O11 C24 C22 117.3(5) . 2_665 ?
O12 C24 C22 118.1(5) . 2_665 ?
O13 C25 C26 118.4(5) . . ?
O14 C25 O13 123.3(5) . . ?
O14 C25 C26 118.3(5) . . ?
C27 C26 C25 120.3(5) . . ?
C31 C26 C25 120.3(5) . . ?
C31 C26 C27 119.3(5) . . ?
C26 C27 H27 119.5 . . ?
C28 C27 C26 121.1(5) . . ?
C28 C27 H27 119.5 . . ?
C27 C28 H28 119.7 . . ?
C27 C28 C29 120.7(5) . . ?
C29 C28 H28 119.7 . . ?
C28 C29 H29 120.5 . . ?
C28 C29 C30 119.0(5) . . ?
C30 C29 H29 120.5 . . ?
C29 C30 C32 120.5(5) . . ?
C31 C30 C29 120.3(5) . . ?
C31 C30 C32 119.2(5) . . ?
C26 C31 C30 119.7(5) . . ?
C26 C31 H31 120.2 . . ?
C30 C31 H31 120.2 . . ?
O15 C32 O16 124.3(6) . . ?
O15 C32 C30 117.4(6) . . ?
O16 C32 C30 118.3(5) . . ?
O19 C33 C34 121.3(5) . . ?
O20 C33 O19 122.7(5) . . ?
O20 C33 C34 116.0(5) . . ?
C35 C34 C33 119.5(5) . . ?
C35 C34 C39 119.1(5) . . ?
C39 C34 C33 121.3(5) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 C34 121.3(6) . . ?
C36 C35 H35 119.3 . . ?
C35 C36 H36 120.2 . . ?
C35 C36 C37 119.6(6) . . ?
C37 C36 H36 120.2 . . ?
C36 C37 H37 120.1 . . ?
C38 C37 C36 119.8(6) . . ?
C38 C37 H37 120.1 . . ?
C37 C38 C39 120.5(5) . . ?
C37 C38 C40 120.4(5) . . ?
C39 C38 C40 119.1(5) . . ?
C34 C39 H39 120.2 . . ?
C38 C39 C34 119.6(5) . . ?
C38 C39 H39 120.2 . . ?
O17 C40 C38 116.7(5) . . ?
O18 C40 O17 122.9(6) . . ?
O18 C40 C38 120.4(5) . . ?
O21 C41 Dy3 60.4(3) . 2_566 ?
O21 C41 O22 118.8(5) . . ?
O21 C41 C42 121.3(5) . . ?
O22 C41 Dy3 58.7(3) . 2_566 ?
O22 C41 C42 119.9(5) . . ?
C42 C41 Dy3 171.5(4) . 2_566 ?
C43 C42 C41 118.6(5) . . ?
C43 C42 C47 119.8(5) . . ?
C47 C42 C41 121.5(5) . . ?
C42 C43 H43 119.8 . . ?
C42 C43 C44 120.5(6) . . ?
C44 C43 H43 119.8 . . ?
C43 C44 H44 120.0 . . ?
C45 C44 C43 119.9(6) . . ?
C45 C44 H44 120.0 . . ?
C44 C45 H45 120.2 . . ?
C44 C45 C46 119.6(6) . . ?
C46 C45 H45 120.2 . . ?
C45 C46 C47 120.8(5) . . ?
C45 C46 C48 120.2(5) . . ?
C47 C46 C48 118.9(5) . . ?
C42 C47 C46 119.2(5) . . ?
C42 C47 H47 120.4 . . ?
C46 C47 H47 120.4 . . ?
O23 C48 O24 123.9(5) . . ?
O23 C48 C46 119.4(5) . . ?
O24 C48 C46 116.7(5) . . ?
O29 C49 N1 128.5(8) . . ?
O29 C49 H49 115.7 . . ?
N1 C49 H49 115.7 . . ?
N1 C50 H50A 109.5 . . ?
N1 C50 H50B 109.5 . . ?
N1 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N1 C51 H51A 109.5 . . ?
N1 C51 H51B 109.5 . . ?
N1 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C52 N2 C53 116.7(11) . . ?
C52 N2 C54 125.6(11) . . ?
C54 N2 C53 117.7(11) . . ?
O30 C52 N2 123.2(12) . . ?
O30 C52 H52 118.4 . . ?
N2 C52 H52 118.4 . . ?
N2 C53 H53A 109.5 . . ?
N2 C53 H53B 109.5 . . ?
N2 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N2 C54 H54A 109.5 . . ?
N2 C54 H54B 109.5 . . ?
N2 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
H31A O31 H31B 120.0 . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelxl_CCDC6
_audit_block_doi                 10.5517/cc1j7mv7
_database_code_depnum_ccdc_archive 'CCDC 1407519'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H26 Eu2 N2 O16, H2 O'
_chemical_formula_sum            'C34 H28 Eu2 N2 O17'
_chemical_formula_weight         1040.52
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.9810(14)
_cell_length_b                   26.527(5)
_cell_length_c                   17.919(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.89(3)
_cell_angle_gamma                90
_cell_volume                     3286.9(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8620
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   0.512
_shelx_estimated_absorpt_T_min   0.390
_exptl_absorpt_coefficient_mu    3.870
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.997
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32985
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.571
_diffrn_reflns_theta_min         3.044
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1269
	          2theta: 29.8518
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1269
	          2theta: 29.8518
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1269
	          2theta: 29.8518
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.085172
_diffrn_orient_matrix_UB_12      -0.116783
_diffrn_orient_matrix_UB_13      0.004243
_diffrn_orient_matrix_UB_21      -0.011368
_diffrn_orient_matrix_UB_22      -0.007010
_diffrn_orient_matrix_UB_23      0.035253
_diffrn_orient_matrix_UB_31      -0.037286
_diffrn_orient_matrix_UB_32      -0.037477
_diffrn_orient_matrix_UB_33      -0.019476
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6815
_reflns_number_total             7540
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.711
_refine_diff_density_min         -1.588
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         7540
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0309
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0283P)²+4.6930P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0737
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H,H,H) groups, All O(H) groups
2. Restrained distances
 H13A-H13B
 1.35 with sigma of 0.01
 H13A-O13 = H13B-O13
 0.85 with sigma of 0.01
 H16A-H16B
 1.35 with sigma of 0.01
 H16A-O16 = H16B-O16
 0.85 with sigma of 0.01
 H15A-H15B
 1.35 with sigma of 0.01
 H15A-O15 = H15B-O15
 0.85 with sigma of 0.01
 H14A-H14B
 1.35 with sigma of 0.01
 H14A-O14 = H14B-O14
 0.85 with sigma of 0.01
 H17B-O17 = H17A-O17
 0.85 with sigma of 0.01
 H17B-H17A
 1.38 with sigma of 0.01
3.a Riding coordinates:
 O17(H17A)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
H14A H 0.325(9) 0.1370(13) 0.188(3) 0.09(2) Uiso 1 1 d D . . . .
H16A H -0.072(2) 0.1083(19) 0.301(4) 0.09(2) Uiso 1 1 d D . . . .
H16B H 0.075(7) 0.1416(9) 0.301(3) 0.062(18) Uiso 1 1 d D . . . .
Eu2 Eu 0.26304(2) 0.06812(2) 0.04918(2) 0.01662(6) Uani 1 1 d . . . . .
H27 H -0.548(7) 0.2606(18) 0.456(3) 0.047(14) Uiso 1 1 d . . . . .
H32 H -0.393(7) 0.1780(18) 0.455(3) 0.045(13) Uiso 1 1 d . . . . .
H28 H -0.354(6) 0.3322(16) 0.491(2) 0.024(10) Uiso 1 1 d . . . . .
H30 H 0.128(6) 0.2496(15) 0.506(2) 0.021(10) Uiso 1 1 d . . . . .
O17 O 0.6636(5) 0.40717(16) 0.7758(2) 0.0661(12) Uani 1 1 d D . . . .
H17A H 0.581121 0.425191 0.794304 0.079 Uiso 1 1 d DR . . . .
O8 O 0.0823(4) -0.01994(9) 0.60184(14) 0.0237(5) Uani 1 1 d . . . . .
Eu1 Eu 0.18276(2) 0.07031(2) 0.43306(2) 0.01562(6) Uani 1 1 d . . . . .
O1 O 0.4401(4) -0.00445(10) 0.07921(15) 0.0344(7) Uani 1 1 d . . . . .
O2 O 0.5440(4) -0.08066(10) 0.05107(14) 0.0263(6) Uani 1 1 d . . . . .
O3 O 0.3156(4) -0.01872(10) 0.41829(13) 0.0244(5) Uani 1 1 d . . . . .
O4 O 0.3477(4) 0.03764(10) 0.33133(14) 0.0288(6) Uani 1 1 d . . . . .
O5 O 0.0714(4) 0.03786(11) 0.94445(14) 0.0349(7) Uani 1 1 d . . . . .
O6 O -0.0642(4) -0.02427(10) 0.87265(14) 0.0259(6) Uani 1 1 d . . . . .
O7 O 0.1913(4) 0.05163(10) 0.55939(13) 0.0258(6) Uani 1 1 d . . . . .
O9 O -0.1103(4) 0.11869(10) 0.45886(17) 0.0321(6) Uani 1 1 d . . . . .
O10 O 0.1696(4) 0.15840(10) 0.47305(16) 0.0276(6) Uani 1 1 d . . . . .
O11 O 0.2039(4) 0.34306(10) 0.51405(15) 0.0282(6) Uani 1 1 d . . . . .
O12 O -0.0523(4) 0.38351(10) 0.54169(17) 0.0336(7) Uani 1 1 d . . . . .
O13 O 0.5937(5) 0.10240(16) 0.1055(2) 0.0555(10) Uani 1 1 d D . . . .
O14 O 0.2730(5) 0.10887(13) 0.17483(17) 0.0403(7) Uani 1 1 d D . . . .
O15 O 0.5208(4) 0.08442(11) 0.47997(16) 0.0277(6) Uani 1 1 d D . . . .
O16 O 0.0492(5) 0.11177(11) 0.31386(17) 0.0350(7) Uani 1 1 d D . . . .
N1 N 0.4806(7) -0.29513(15) 0.3103(3) 0.0537(11) Uani 1 1 d . . . . .
N2 N 0.0919(6) 0.29061(13) 0.7696(2) 0.0369(8) Uani 1 1 d . . . . .
C1 C 0.4019(8) -0.27793(18) 0.2423(3) 0.0456(12) Uani 1 1 d . . . . .
C2 C 0.3793(7) -0.22688(16) 0.2253(3) 0.0362(10) Uani 1 1 d . . . . .
C3 C 0.4377(6) -0.19050(14) 0.2798(2) 0.0281(8) Uani 1 1 d . . . . .
C4 C 0.5160(7) -0.20884(17) 0.3509(3) 0.0364(10) Uani 1 1 d . . . . .
C5 C 0.5338(8) -0.26047(19) 0.3626(3) 0.0479(12) Uani 1 1 d . . . . .
C6 C 0.4260(5) -0.13550(13) 0.26237(19) 0.0211(7) Uani 1 1 d . . . . .
C7 C 0.4518(5) -0.11924(14) 0.1899(2) 0.0210(7) Uani 1 1 d . . . . .
C8 C 0.4482(5) -0.06817(12) 0.17202(18) 0.0179(7) Uani 1 1 d . . . . .
C9 C 0.4202(5) -0.03294(13) 0.22667(19) 0.0191(7) Uani 1 1 d . . . . .
C10 C 0.3939(5) -0.04835(13) 0.29880(19) 0.0196(7) Uani 1 1 d . . . . .
C11 C 0.3966(5) -0.09931(14) 0.3167(2) 0.0213(7) Uani 1 1 d . . . . .
C12 C 0.4787(5) -0.05011(13) 0.09439(19) 0.0202(7) Uani 1 1 d . . . . .
C13 C 0.3531(5) -0.00790(13) 0.35313(19) 0.0199(7) Uani 1 1 d . . . . .
C14 C 0.1517(6) 0.26131(16) 0.8287(2) 0.0334(9) Uani 1 1 d . . . . .
C15 C 0.1503(6) 0.20903(14) 0.8261(2) 0.0265(8) Uani 1 1 d . . . . .
C16 C 0.0846(5) 0.18453(14) 0.75817(19) 0.0228(7) Uani 1 1 d . . . . .
C17 C 0.0252(7) 0.21565(15) 0.6964(2) 0.0325(9) Uani 1 1 d . . . . .
C18 C 0.0293(7) 0.26723(17) 0.7043(3) 0.0396(10) Uani 1 1 d . . . . .
C19 C 0.0818(5) 0.12879(13) 0.75332(18) 0.0184(7) Uani 1 1 d . . . . .
C20 C 0.0573(5) 0.09966(14) 0.81617(18) 0.0196(7) Uani 1 1 d . . . . .
C21 C 0.0516(5) 0.04752(13) 0.81280(18) 0.0184(7) Uani 1 1 d . . . . .
C22 C 0.0721(5) 0.02309(13) 0.74524(18) 0.0179(6) Uani 1 1 d . . . . .
C23 C 0.1038(5) 0.05138(13) 0.68242(17) 0.0164(6) Uani 1 1 d . . . . .
C24 C 0.1069(5) 0.10390(13) 0.68643(19) 0.0186(7) Uani 1 1 d . . . . .
C25 C 0.1278(5) 0.02602(12) 0.60954(18) 0.0170(6) Uani 1 1 d . . . . .
C26 C 0.0180(5) 0.01788(13) 0.88156(19) 0.0187(7) Uani 1 1 d . . . . .
C27 C -0.4061(6) 0.25794(17) 0.4693(3) 0.0355(10) Uani 1 1 d . . . . .
C28 C -0.2965(6) 0.30117(15) 0.4867(2) 0.0291(8) Uani 1 1 d . . . . .
C29 C -0.0958(5) 0.29820(13) 0.50053(19) 0.0223(7) Uani 1 1 d . . . . .
C30 C -0.0057(6) 0.25171(14) 0.4953(2) 0.0226(7) Uani 1 1 d . . . . .
C31 C -0.1146(5) 0.20807(13) 0.4783(2) 0.0225(7) Uani 1 1 d . . . . .
C32 C -0.3156(6) 0.21138(16) 0.4656(2) 0.0314(9) Uani 1 1 d . . . . .
C33 C -0.0128(5) 0.15876(13) 0.4704(2) 0.0219(7) Uani 1 1 d . . . . .
C34 C 0.0249(5) 0.34442(13) 0.51989(19) 0.0218(7) Uani 1 1 d . . . . .
H20 H 0.042(5) 0.1149(14) 0.863(2) 0.015(9) Uiso 1 1 d . . . . .
H22 H 0.066(5) -0.0134(15) 0.741(2) 0.017(9) Uiso 1 1 d . . . . .
H15A H 0.565(5) 0.0636(11) 0.5139(16) 0.016(10) Uiso 1 1 d D . . . .
H24 H 0.134(6) 0.1213(16) 0.644(2) 0.033(12) Uiso 1 1 d . . . . .
H11 H 0.375(6) -0.1097(15) 0.364(2) 0.021(10) Uiso 1 1 d . . . . .
H15 H 0.192(5) 0.1908(14) 0.870(2) 0.017(9) Uiso 1 1 d . . . . .
H14 H 0.205(6) 0.2794(16) 0.873(2) 0.029(11) Uiso 1 1 d . . . . .
H9 H 0.415(6) 0.0008(15) 0.214(2) 0.019(10) Uiso 1 1 d . . . . .
H7 H 0.472(6) -0.1428(15) 0.152(2) 0.021(10) Uiso 1 1 d . . . . .
H15B H 0.618(4) 0.0976(16) 0.465(2) 0.049(15) Uiso 1 1 d D . . . .
H17 H -0.041(7) 0.2009(19) 0.651(3) 0.048(14) Uiso 1 1 d . . . . .
H18 H -0.008(7) 0.2877(18) 0.659(3) 0.043(13) Uiso 1 1 d . . . . .
H4 H 0.552(7) -0.1848(19) 0.399(3) 0.048(14) Uiso 1 1 d . . . . .
H5 H 0.599(8) -0.278(2) 0.412(3) 0.060(16) Uiso 1 1 d . . . . .
H14B H 0.212(8) 0.100(2) 0.211(2) 0.09(2) Uiso 1 1 d D . . . .
H1 H 0.355(8) -0.304(2) 0.206(3) 0.056(16) Uiso 1 1 d . . . . .
H2 H 0.318(8) -0.217(2) 0.173(3) 0.067(18) Uiso 1 1 d . . . . .
H17B H 0.606(4) 0.392(2) 0.737(2) 0.081 Uiso 1 1 d DR . . . .
H13A H 0.609(8) 0.0714(8) 0.117(4) 0.081 Uiso 1 1 d DR . . . .
H13B H 0.695(5) 0.1102(19) 0.087(3) 0.081 Uiso 1 1 d DR . . . .


_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
Eu2 O1 2.311(3) . ?
Eu2 O2 2.412(2) 3_655 ?
Eu2 O5 2.295(3) 1_554 ?
Eu2 O6 2.403(2) 3_556 ?
Eu2 O11 2.459(3) 4_565 ?
Eu2 O12 2.535(3) 4_565 ?
Eu2 O13 2.557(4) . ?
Eu2 O14 2.490(3) . ?
Eu2 C34 2.860(4) 4_565 ?
Eu2 H13A 2.55(6) . ?
O17 H17A 0.8499 . ?
O17 H17B 0.851(10) . ?
O8 Eu1 2.299(2) 3_556 ?
O8 C25 1.263(4) . ?
Eu1 O3 2.564(3) . ?
Eu1 O4 2.445(3) . ?
Eu1 O7 2.310(2) . ?
Eu1 O9 2.511(3) . ?
Eu1 O10 2.450(3) . ?
Eu1 O15 2.423(3) . ?
Eu1 O16 2.469(3) . ?
O1 C12 1.262(4) . ?
O2 C12 1.251(4) . ?
O3 C13 1.264(4) . ?
O4 C13 1.269(4) . ?
O5 C26 1.255(4) . ?
O6 C26 1.257(4) . ?
O7 C25 1.255(4) . ?
O9 C33 1.264(4) . ?
O10 C33 1.268(4) . ?
O11 C34 1.268(4) . ?
O12 C34 1.255(4) . ?
O13 H13A 0.849(10) . ?
O13 H13B 0.853(10) . ?
O14 H14A 0.848(10) . ?
O14 H14B 0.848(10) . ?
O15 H15A 0.848(10) . ?
O15 H15B 0.845(10) . ?
O16 H16A 0.849(10) . ?
O16 H16B 0.849(10) . ?
N1 C1 1.346(7) . ?
N1 C5 1.329(7) . ?
N2 C14 1.333(5) . ?
N2 C18 1.343(6) . ?
C1 C2 1.392(6) . ?
C1 H1 0.98(5) . ?
C2 C3 1.394(6) . ?
C2 H2 1.00(6) . ?
C3 C4 1.403(6) . ?
C3 C6 1.492(5) . ?
C4 C5 1.388(6) . ?
C4 H4 1.07(5) . ?
C5 H5 1.04(5) . ?
C6 C7 1.404(5) . ?
C6 C11 1.402(5) . ?
C7 C8 1.391(5) . ?
C7 H7 0.94(4) . ?
C8 C9 1.387(5) . ?
C8 C12 1.514(4) . ?
C9 C10 1.391(5) . ?
C9 H9 0.92(4) . ?
C10 C11 1.389(5) . ?
C10 C13 1.502(5) . ?
C11 H11 0.92(4) . ?
C14 C15 1.388(5) . ?
C14 H14 0.96(4) . ?
C15 C16 1.400(5) . ?
C15 H15 0.94(4) . ?
C16 C17 1.397(5) . ?
C16 C19 1.481(5) . ?
C17 C18 1.375(6) . ?
C17 H17 0.96(5) . ?
C18 H18 0.99(5) . ?
C19 C20 1.396(5) . ?
C19 C24 1.400(5) . ?
C20 C21 1.385(5) . ?
C20 H20 0.95(4) . ?
C21 C22 1.398(5) . ?
C21 C26 1.507(4) . ?
C22 C23 1.396(4) . ?
C22 H22 0.97(4) . ?
C23 C24 1.395(5) . ?
C23 C25 1.499(4) . ?
C24 H24 0.94(4) . ?
C27 H27 0.99(5) . ?
C27 C28 1.390(6) . ?
C27 C32 1.393(6) . ?
C28 H28 0.92(4) . ?
C28 C29 1.391(5) . ?
C29 C30 1.394(5) . ?
C29 C34 1.502(5) . ?
C30 H30 0.93(4) . ?
C30 C31 1.396(5) . ?
C31 C32 1.393(5) . ?
C31 C33 1.505(5) . ?
C32 H32 1.04(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu2 O2 87.28(9) . 3_655 ?
O1 Eu2 O6 78.14(10) . 3_556 ?
O1 Eu2 O11 157.42(10) . 4_565 ?
O1 Eu2 O12 150.07(9) . 4_565 ?
O1 Eu2 O13 77.24(13) . . ?
O1 Eu2 O14 101.73(11) . . ?
O1 Eu2 C34 175.68(10) . 4_565 ?
O1 Eu2 H13A 58.4(5) . . ?
O2 Eu2 O11 76.62(9) 3_655 4_565 ?
O2 Eu2 O12 117.42(9) 3_655 4_565 ?
O2 Eu2 O13 71.25(11) 3_655 . ?
O2 Eu2 O14 131.64(10) 3_655 . ?
O2 Eu2 C34 96.98(9) 3_655 4_565 ?
O2 Eu2 H13A 76.1(13) 3_655 . ?
O5 Eu2 O1 97.59(11) 1_554 . ?
O5 Eu2 O2 76.21(10) 1_554 3_655 ?
O5 Eu2 O6 89.36(9) 1_554 3_556 ?
O5 Eu2 O11 93.86(10) 1_554 4_565 ?
O5 Eu2 O12 74.30(11) 1_554 4_565 ?
O5 Eu2 O13 147.22(11) 1_554 . ?
O5 Eu2 O14 146.32(11) 1_554 . ?
O5 Eu2 C34 82.81(11) 1_554 4_565 ?
O5 Eu2 H13A 144.0(13) 1_554 . ?
O6 Eu2 O2 158.00(9) 3_556 3_655 ?
O6 Eu2 O11 121.52(9) 3_556 4_565 ?
O6 Eu2 O12 73.09(9) 3_556 4_565 ?
O6 Eu2 O13 120.30(10) 3_556 . ?
O6 Eu2 O14 68.27(10) 3_556 . ?
O6 Eu2 C34 97.58(10) 3_556 4_565 ?
O6 Eu2 H13A 108.9(10) 3_556 . ?
O11 Eu2 O12 52.23(8) 4_565 4_565 ?
O11 Eu2 O13 82.59(11) 4_565 . ?
O11 Eu2 O14 78.37(11) 4_565 . ?
O11 Eu2 C34 26.23(9) 4_565 4_565 ?
O11 Eu2 H13A 101.7(3) 4_565 . ?
O12 Eu2 O13 124.84(12) 4_565 . ?
O12 Eu2 C34 26.02(9) 4_565 4_565 ?
O12 Eu2 H13A 140.0(11) 4_565 . ?
O13 Eu2 C34 104.75(12) . 4_565 ?
O13 Eu2 H13A 19.1(3) . . ?
O14 Eu2 O12 75.20(11) . 4_565 ?
O14 Eu2 O13 64.97(12) . . ?
O14 Eu2 C34 75.95(11) . 4_565 ?
O14 Eu2 H13A 69.4(14) . . ?
C34 Eu2 H13A 123.2(6) 4_565 . ?
H17A O17 H17B 108.2 . . ?
C25 O8 Eu1 140.5(2) . 3_556 ?
O8 Eu1 O3 74.07(9) 3_556 . ?
O8 Eu1 O4 92.01(9) 3_556 . ?
O8 Eu1 O7 93.06(9) 3_556 . ?
O8 Eu1 O9 72.62(9) 3_556 . ?
O8 Eu1 O10 124.95(9) 3_556 . ?
O8 Eu1 O15 153.33(9) 3_556 . ?
O8 Eu1 O16 80.17(10) 3_556 . ?
O4 Eu1 O3 51.86(8) . . ?
O4 Eu1 O9 142.89(10) . . ?
O4 Eu1 O10 126.64(9) . . ?
O4 Eu1 O16 70.93(10) . . ?
O7 Eu1 O3 86.71(9) . . ?
O7 Eu1 O4 134.69(9) . . ?
O7 Eu1 O9 80.87(10) . . ?
O7 Eu1 O10 85.12(9) . . ?
O7 Eu1 O15 78.48(10) . . ?
O7 Eu1 O16 154.07(10) . . ?
O9 Eu1 O3 143.61(8) . . ?
O10 Eu1 O3 159.63(9) . . ?
O10 Eu1 O9 52.72(8) . . ?
O10 Eu1 O16 78.65(10) . . ?
O15 Eu1 O3 80.17(9) . . ?
O15 Eu1 O4 77.14(10) . . ?
O15 Eu1 O9 129.53(10) . . ?
O15 Eu1 O10 79.93(9) . . ?
O15 Eu1 O16 117.74(10) . . ?
O16 Eu1 O3 114.83(9) . . ?
O16 Eu1 O9 73.22(11) . . ?
C12 O1 Eu2 160.2(3) . . ?
C12 O2 Eu2 131.4(2) . 3_655 ?
C13 O3 Eu1 90.6(2) . . ?
C13 O4 Eu1 96.0(2) . . ?
C26 O5 Eu2 161.8(3) . 1_556 ?
C26 O6 Eu2 130.3(2) . 3_556 ?
C25 O7 Eu1 148.6(2) . . ?
C33 O9 Eu1 91.5(2) . . ?
C33 O10 Eu1 94.3(2) . . ?
C34 O11 Eu2 94.8(2) . 4_566 ?
C34 O12 Eu2 91.6(2) . 4_566 ?
Eu2 O13 H13A 80(4) . . ?
Eu2 O13 H13B 133(4) . . ?
H13A O13 H13B 104.3(17) . . ?
H14A O14 H14B 105.6(17) . . ?
Eu2 O14 H14A 126(4) . . ?
Eu2 O14 H14B 128(4) . . ?
Eu1 O15 H15A 113(2) . . ?
Eu1 O15 H15B 138(3) . . ?
H15A O15 H15B 106.0(16) . . ?
H16A O16 H16B 105.5(17) . . ?
Eu1 O16 H16A 116(4) . . ?
Eu1 O16 H16B 125(4) . . ?
C5 N1 C1 116.4(4) . . ?
C14 N2 C18 116.8(4) . . ?
N1 C1 C2 123.2(5) . . ?
N1 C1 H1 115(3) . . ?
C2 C1 H1 122(3) . . ?
C1 C2 C3 120.4(4) . . ?
C1 C2 H2 118(3) . . ?
C3 C2 H2 121(3) . . ?
C2 C3 C4 115.9(4) . . ?
C2 C3 C6 121.9(4) . . ?
C4 C3 C6 122.2(4) . . ?
C3 C4 H4 123(3) . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 H4 117(3) . . ?
N1 C5 C4 124.4(5) . . ?
N1 C5 H5 110(3) . . ?
C4 C5 H5 126(3) . . ?
C7 C6 C3 118.9(3) . . ?
C11 C6 C3 122.2(3) . . ?
C11 C6 C7 118.8(3) . . ?
C6 C7 H7 121(2) . . ?
C8 C7 C6 120.7(3) . . ?
C8 C7 H7 119(2) . . ?
C7 C8 C12 121.3(3) . . ?
C9 C8 C7 119.6(3) . . ?
C9 C8 C12 119.1(3) . . ?
C8 C9 C10 120.5(3) . . ?
C8 C9 H9 118(2) . . ?
C10 C9 H9 121(2) . . ?
C9 C10 C13 116.9(3) . . ?
C11 C10 C9 120.1(3) . . ?
C11 C10 C13 122.9(3) . . ?
C6 C11 H11 119(2) . . ?
C10 C11 C6 120.3(3) . . ?
C10 C11 H11 120(2) . . ?
O1 C12 C8 116.7(3) . . ?
O2 C12 O1 125.0(3) . . ?
O2 C12 C8 118.3(3) . . ?
O3 C13 O4 120.0(3) . . ?
O3 C13 C10 121.2(3) . . ?
O4 C13 C10 118.7(3) . . ?
N2 C14 C15 123.8(4) . . ?
N2 C14 H14 114(3) . . ?
C15 C14 H14 122(3) . . ?
C14 C15 C16 119.5(4) . . ?
C14 C15 H15 119(2) . . ?
C16 C15 H15 121(2) . . ?
C15 C16 C19 121.0(3) . . ?
C17 C16 C15 116.1(3) . . ?
C17 C16 C19 122.9(3) . . ?
C16 C17 H17 119(3) . . ?
C18 C17 C16 120.5(4) . . ?
C18 C17 H17 120(3) . . ?
N2 C18 C17 123.3(4) . . ?
N2 C18 H18 119(3) . . ?
C17 C18 H18 118(3) . . ?
C20 C19 C16 120.5(3) . . ?
C20 C19 C24 118.3(3) . . ?
C24 C19 C16 121.2(3) . . ?
C19 C20 H20 121(2) . . ?
C21 C20 C19 121.6(3) . . ?
C21 C20 H20 117(2) . . ?
C20 C21 C22 119.7(3) . . ?
C20 C21 C26 119.5(3) . . ?
C22 C21 C26 120.8(3) . . ?
C21 C22 H22 122(2) . . ?
C23 C22 C21 119.7(3) . . ?
C23 C22 H22 119(2) . . ?
C22 C23 C25 120.7(3) . . ?
C24 C23 C22 119.9(3) . . ?
C24 C23 C25 119.4(3) . . ?
C19 C24 H24 122(3) . . ?
C23 C24 C19 120.8(3) . . ?
C23 C24 H24 117(3) . . ?
O8 C25 C23 118.2(3) . . ?
O7 C25 O8 123.5(3) . . ?
O7 C25 C23 118.3(3) . . ?
O5 C26 O6 124.3(3) . . ?
O5 C26 C21 117.0(3) . . ?
O6 C26 C21 118.7(3) . . ?
C28 C27 H27 120(3) . . ?
C28 C27 C32 120.2(4) . . ?
C32 C27 H27 120(3) . . ?
C27 C28 H28 121(3) . . ?
C27 C28 C29 120.2(4) . . ?
C29 C28 H28 118(3) . . ?
C28 C29 C30 119.4(3) . . ?
C28 C29 C34 121.0(3) . . ?
C30 C29 C34 119.6(3) . . ?
C29 C30 H30 119(2) . . ?
C29 C30 C31 120.7(3) . . ?
C31 C30 H30 120(2) . . ?
C30 C31 C33 119.4(3) . . ?
C32 C31 C30 119.3(3) . . ?
C32 C31 C33 121.2(3) . . ?
C27 C32 H32 122(3) . . ?
C27 C32 C31 120.1(4) . . ?
C31 C32 H32 118(3) . . ?
O9 C33 O10 121.0(3) . . ?
O9 C33 C31 119.7(3) . . ?
O10 C33 C31 119.2(3) . . ?
O11 C34 Eu2 58.94(18) . 4_566 ?
O11 C34 C29 119.1(3) . . ?
O12 C34 Eu2 62.38(19) . 4_566 ?
O12 C34 O11 121.3(3) . . ?
O12 C34 C29 119.7(3) . . ?
C29 C34 Eu2 176.9(2) . 4_566 ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelxl_CCDC7
_audit_block_doi                 10.5517/cc1j7mt6
_database_code_depnum_ccdc_archive 'CCDC 1407518'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H26 N2 O16 Sm2, H2 O'
_chemical_formula_sum            'C34 H28 N2 O17 Sm2'
_chemical_formula_weight         1037.28
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.0170(14)
_cell_length_b                   26.637(5)
_cell_length_c                   18.062(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.27(3)
_cell_angle_gamma                90
_cell_volume                     3340.9(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7711
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   0.536
_shelx_estimated_absorpt_T_min   0.414
_exptl_absorpt_coefficient_mu    3.568
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.995
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25372
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.100
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         3.032
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.3639
	          2theta: 29.7522
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.3639
	          2theta: 29.7522
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 20.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.3639
	          2theta: 29.7522
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.002158
_diffrn_orient_matrix_UB_12      -0.030371
_diffrn_orient_matrix_UB_13      0.140745
_diffrn_orient_matrix_UB_21      -0.030312
_diffrn_orient_matrix_UB_22      0.021550
_diffrn_orient_matrix_UB_23      0.005115
_diffrn_orient_matrix_UB_31      -0.032532
_diffrn_orient_matrix_UB_32      -0.045502
_diffrn_orient_matrix_UB_33      -0.001087
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5235
_reflns_number_total             5863
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.868
_refine_diff_density_min         -1.542
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         5863
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0679
_refine_ls_restrained_S_all      1.234
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+100.7120P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1540
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1(10) 0(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H14A,H14B} of O14, All O(H,H,H,H,H,H) groups
 At 1.5 times of:
  {H15A,H15B} of O15
3. Restrained distances
 H13B-H13A
 1.35 with sigma of 0.01
 H13B-O13 = H13A-O13
 0.85 with sigma of 0.01
 H16A-H16B
 1.35 with sigma of 0.01
 H16A-O16 = H16B-O16
 0.85 with sigma of 0.01
 H17B-H17A
 1.39 with sigma of 0.01
 H17B-O17
 0.85 with sigma of 0.01
 H17A-O17
 0.85 with sigma of 0.01
 H15A-H17B
 2.2 with sigma of 0.01
 H13A_$1-H17B
 2.2 with sigma of 0.01
 H14B-O9_$2
 2.3 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) = Uanis(C7) = Uanis(C9)
5.a Riding coordinates:
 O14(H14A,H14B), O17(H17A)
5.b Rotating group:
 O15(H15A,H15B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C9(H9), C11(H11), C14(H14), C15(H15),
 C17(H17), C18(H18), C20(H20), C22(H22), C24(H24), C29(H29), C30(H30), C31(H31),
  C34(H34)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm2 Sm 0.68337(8) 0.42946(2) 0.93295(3) 0.01653(17) Uani 1 1 d . . . . .
O6 O 1.0589(14) 0.0049(3) 0.9207(5) 0.031(2) Uani 1 1 d . . . . .
Sm1 Sm 0.76281(9) 0.06791(2) 1.04918(3) 0.01741(17) Uani 1 1 d . . . . .
O1 O 0.5702(14) 0.0377(3) 0.9447(4) 0.030(2) Uani 1 1 d . U . . .
O2 O 0.4365(13) -0.0242(3) 0.8717(5) 0.0251(19) Uani 1 1 d . . . . .
O3 O 0.6907(13) 0.0515(3) 0.5597(5) 0.0254(19) Uani 1 1 d . . . . .
O4 O 0.5840(12) -0.0204(3) 0.6027(5) 0.0239(19) Uani 1 1 d . . . . .
O5 O 0.9546(13) 0.0812(3) 0.9486(5) 0.0256(19) Uani 1 1 d . . . . .
O7 O 1.1500(14) -0.0369(3) 0.6691(5) 0.030(2) Uani 1 1 d . . . . .
O8 O 1.1847(13) 0.0193(3) 0.5819(4) 0.0252(19) Uani 1 1 d . . . . .
O9 O 0.4374(13) 0.1155(3) 1.0450(6) 0.038(2) Uani 1 1 d D . . . .
O10 O 0.7028(12) 0.1571(3) 1.0145(5) 0.027(2) Uani 1 1 d . . . . .
O11 O 0.6681(12) 0.3411(3) 0.9741(5) 0.026(2) Uani 1 1 d . . . . .
O12 O 0.3905(13) 0.3810(3) 0.9589(6) 0.035(2) Uani 1 1 d . . . . .
O13 O 0.7743(16) 0.1088(4) 1.1762(5) 0.039(2) Uani 1 1 d D . . . .
O14 O 1.1057(15) 0.1033(5) 1.1016(5) 0.059(3) Uani 1 1 d . . . . .
H14A H 1.123103 0.134737 1.107319 0.070 Uiso 1 1 d R . . . .
H14B H 1.198273 0.083097 1.114399 0.070 Uiso 1 1 d DR . . . .
O15 O 0.5514(15) 0.3884(3) 0.8126(5) 0.036(2) Uani 1 1 d . . . . .
H15A H 0.420536 0.390651 0.803137 0.055 Uiso 1 1 d DGR . . . .
H15B H 0.580655 0.355070 0.812367 0.055 Uiso 1 1 d GR . . . .
O16 O 1.0249(13) 0.4156(3) 0.9798(5) 0.029(2) Uani 1 1 d D . . . .
N1 N 0.5890(19) 0.2904(4) 0.7695(6) 0.035(3) Uani 1 1 d . . . . .
N2 N 1.021(2) 0.2952(5) 0.6915(9) 0.062(4) Uani 1 1 d . . . . .
C1 C 1.096(3) 0.2777(6) 0.7574(9) 0.048(4) Uani 1 1 d . . . . .
H1 H 1.133802 0.300794 0.795227 0.057 Uiso 1 1 calc R . . . .
C2 C 1.123(2) 0.2270(5) 0.7746(8) 0.037(3) Uani 1 1 d . . . . .
H2 H 1.182213 0.217388 0.821831 0.045 Uiso 1 1 calc R . . . .
C3 C 1.0610(19) 0.1904(4) 0.7204(7) 0.027(3) Uani 1 1 d . . . . .
C4 C 0.986(2) 0.2091(5) 0.6491(7) 0.033(3) Uani 1 1 d . . . . .
H4 H 0.951056 0.187023 0.609654 0.040 Uiso 1 1 calc R . . . .
C5 C 0.965(3) 0.2613(6) 0.6377(9) 0.048(4) Uani 1 1 d . . . . .
H5 H 0.908652 0.272755 0.590920 0.058 Uiso 1 1 calc R . . . .
C6 C 1.0740(18) 0.1358(4) 0.7382(7) 0.023(3) Uani 1 1 d . . . . .
C7 C 1.0470(16) 0.1198(4) 0.8103(6) 0.0146(13) Uani 1 1 d . . . . .
H7 H 1.024925 0.143242 0.846239 0.018 Uiso 1 1 calc R . . . .
C8 C 1.0533(16) 0.0690(4) 0.8276(6) 0.0146(13) Uani 1 1 d . . . . .
C9 C 1.0816(16) 0.0330(4) 0.7736(6) 0.0146(13) Uani 1 1 d . . . . .
H9 H 1.082945 -0.000975 0.785383 0.018 Uiso 1 1 calc R . . . .
C10 C 1.1082(16) 0.0490(5) 0.7007(6) 0.019(2) Uani 1 1 d . . . . .
C11 C 1.1021(17) 0.0998(4) 0.6836(6) 0.020(2) Uani 1 1 d . . . . .
H11 H 1.116615 0.110243 0.635612 0.023 Uiso 1 1 calc R . . . .
C12 C 1.1464(17) 0.0083(4) 0.6473(6) 0.018(2) Uani 1 1 d . . . . .
C13 C 1.0211(17) 0.0500(4) 0.9052(6) 0.020(2) Uani 1 1 d . . . . .
C14 C 0.652(2) 0.2605(5) 0.8289(8) 0.032(3) Uani 1 1 d . . . . .
H14 H 0.699773 0.275659 0.874063 0.038 Uiso 1 1 calc R . . . .
C15 C 0.6474(19) 0.2084(5) 0.8257(7) 0.027(3) Uani 1 1 d . . . . .
H15 H 0.686775 0.189707 0.868659 0.033 Uiso 1 1 calc R . . . .
C16 C 0.5844(18) 0.1843(4) 0.7586(6) 0.022(3) Uani 1 1 d . . . . .
C17 C 0.523(2) 0.2153(5) 0.6971(7) 0.034(3) Uani 1 1 d . . . . .
H17 H 0.479655 0.200958 0.650853 0.041 Uiso 1 1 calc R . . . .
C18 C 0.527(2) 0.2673(5) 0.7044(8) 0.040(4) Uani 1 1 d . . . . .
H18 H 0.485212 0.286787 0.662529 0.048 Uiso 1 1 calc R . . . .
C19 C 0.5828(17) 0.1285(4) 0.7532(7) 0.021(2) Uani 1 1 d . . . . .
C20 C 0.5566(18) 0.1003(4) 0.8156(7) 0.021(3) Uani 1 1 d . . . . .
H20 H 0.542603 0.116629 0.860080 0.025 Uiso 1 1 calc R . . . .
C21 C 0.5508(15) 0.0474(4) 0.8127(6) 0.014(2) Uani 1 1 d . . . . .
C22 C 0.5718(16) 0.0235(4) 0.7450(6) 0.017(2) Uani 1 1 d . . . . .
H22 H 0.563300 -0.011243 0.741639 0.021 Uiso 1 1 calc R . . . .
C23 C 0.6052(16) 0.0514(4) 0.6829(6) 0.016(2) Uani 1 1 d . . . . .
C24 C 0.6068(16) 0.1040(4) 0.6860(6) 0.017(2) Uani 1 1 d . . . . .
H24 H 0.623705 0.122652 0.643909 0.021 Uiso 1 1 calc R . . . .
C25 C 0.5197(16) 0.0175(4) 0.8809(6) 0.019(2) Uani 1 1 d . . . . .
C26 C 0.6284(16) 0.0262(4) 0.6101(6) 0.016(2) Uani 1 1 d . . . . .
C27 C 0.5230(19) 0.1550(4) 1.0195(6) 0.023(3) Uani 1 1 d . . . . .
C28 C 0.4025(17) 0.2017(4) 1.0010(6) 0.020(2) Uani 1 1 d . . . . .
C29 C 0.2008(19) 0.1985(5) 0.9875(7) 0.027(3) Uani 1 1 d . . . . .
H29 H 0.139453 0.167756 0.990605 0.033 Uiso 1 1 calc R . . . .
C30 C 0.0939(18) 0.2420(5) 0.9695(8) 0.032(3) Uani 1 1 d . . . . .
H30 H -0.039667 0.239817 0.960138 0.038 Uiso 1 1 calc R . . . .
C31 C 0.1811(19) 0.2888(5) 0.9652(7) 0.029(3) Uani 1 1 d . . . . .
H31 H 0.107095 0.317427 0.953419 0.034 Uiso 1 1 calc R . . . .
C32 C 0.3832(18) 0.2917(4) 0.9791(7) 0.022(3) Uani 1 1 d . . . . .
C33 C 0.4874(18) 0.3409(4) 0.9707(7) 0.023(3) Uani 1 1 d . . . . .
C34 C 0.4908(18) 0.2484(4) 0.9952(6) 0.019(2) Uani 1 1 d . . . . .
H34 H 0.624476 0.250357 1.002359 0.023 Uiso 1 1 calc R . . . .
O17 O 0.1667(19) 0.4081(5) 0.7748(8) 0.070(4) Uani 1 1 d D . . . .
H17A H 0.076743 0.423733 0.791940 0.084 Uiso 1 1 d DR . . . .
H16A H 1.08(2) 0.425(7) 0.944(5) 0.084 Uiso 1 1 d DR . . . .
H16B H 1.07(2) 0.433(6) 1.017(5) 0.084 Uiso 1 1 d DR . . . .
H13A H 0.833(9) 0.1359(6) 1.190(8) 0.084 Uiso 1 1 d DR . . . .
H13B H 0.686(18) 0.106(6) 1.204(8) 0.084 Uiso 1 1 d DR . . . .
H17B H 0.120(2) 0.3832(18) 0.749(4) 0.084 Uiso 1 1 d DR . . . .


_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
Sm2 O3 2.339(8) 4_566 ?
Sm2 O4 2.318(8) 2_656 ?
Sm2 O7 2.488(8) 2_756 ?
Sm2 O8 2.595(8) 2_756 ?
Sm2 O11 2.476(8) . ?
Sm2 O12 2.527(9) . ?
Sm2 O15 2.490(9) . ?
Sm2 O16 2.452(9) . ?
Sm2 C12 2.904(11) 2_756 ?
O6 Sm1 2.329(8) 3_757 ?
O6 C13 1.254(14) . ?
Sm1 O1 2.302(8) . ?
Sm1 O2 2.435(8) 3_657 ?
Sm1 O5 2.437(8) . ?
Sm1 O9 2.603(9) . ?
Sm1 O10 2.478(8) . ?
Sm1 O13 2.531(9) . ?
Sm1 O14 2.630(10) . ?
O1 C25 1.275(14) . ?
O2 C25 1.255(14) . ?
O3 C26 1.259(13) . ?
O4 C26 1.280(14) . ?
O5 C13 1.276(14) . ?
O7 C12 1.265(14) . ?
O8 C12 1.282(14) . ?
O9 C27 1.327(15) . ?
O10 C27 1.279(16) . ?
O11 C33 1.260(15) . ?
O12 C33 1.267(14) . ?
O13 H13A 0.850(11) . ?
O13 H13B 0.850(11) . ?
O14 H14A 0.8499 . ?
O14 H14B 0.8500 . ?
O15 H15A 0.9115 . ?
O15 H15B 0.9119 . ?
O16 H16A 0.851(11) . ?
O16 H16B 0.850(11) . ?
N1 C14 1.358(17) . ?
N1 C18 1.343(18) . ?
N2 C1 1.31(2) . ?
N2 C5 1.34(2) . ?
C1 H1 0.9300 . ?
C1 C2 1.39(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.405(19) . ?
C3 C4 1.409(18) . ?
C3 C6 1.490(16) . ?
C4 H4 0.9300 . ?
C4 C5 1.41(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.408(16) . ?
C6 C11 1.409(16) . ?
C7 H7 0.9300 . ?
C7 C8 1.388(15) . ?
C8 C9 1.401(15) . ?
C8 C13 1.538(15) . ?
C9 H9 0.9300 . ?
C9 C10 1.422(15) . ?
C10 C11 1.387(17) . ?
C10 C12 1.502(15) . ?
C11 H11 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.388(17) . ?
C15 H15 0.9300 . ?
C15 C16 1.388(17) . ?
C16 C17 1.401(17) . ?
C16 C19 1.490(16) . ?
C17 H17 0.9300 . ?
C17 C18 1.390(18) . ?
C18 H18 0.9300 . ?
C19 C20 1.389(16) . ?
C19 C24 1.408(16) . ?
C20 H20 0.9300 . ?
C20 C21 1.412(14) . ?
C21 C22 1.405(15) . ?
C21 C25 1.509(15) . ?
C22 H22 0.9300 . ?
C22 C23 1.393(16) . ?
C23 C24 1.403(16) . ?
C23 C26 1.506(15) . ?
C24 H24 0.9300 . ?
C27 C28 1.514(16) . ?
C28 C29 1.404(18) . ?
C28 C34 1.399(16) . ?
C29 H29 0.9300 . ?
C29 C30 1.394(18) . ?
C30 H30 0.9300 . ?
C30 C31 1.395(18) . ?
C31 H31 0.9300 . ?
C31 C32 1.407(18) . ?
C32 C33 1.518(17) . ?
C32 C34 1.388(16) . ?
C34 H34 0.9300 . ?
O17 H17A 0.8503 . ?
O17 H17B 0.849(10) . ?

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 Sm2 O7 134.5(3) 4_566 2_756 ?
O3 Sm2 O8 86.7(3) 4_566 2_756 ?
O3 Sm2 O11 84.8(3) 4_566 . ?
O3 Sm2 O12 80.4(3) 4_566 . ?
O3 Sm2 O15 154.6(3) 4_566 . ?
O3 Sm2 O16 79.2(3) 4_566 . ?
O3 Sm2 C12 112.2(3) 4_566 2_756 ?
O4 Sm2 O3 92.8(3) 2_656 4_566 ?
O4 Sm2 O7 92.0(3) 2_656 2_756 ?
O4 Sm2 O8 74.1(3) 2_656 2_756 ?
O4 Sm2 O11 124.3(3) 2_656 . ?
O4 Sm2 O12 72.5(3) 2_656 . ?
O4 Sm2 O15 80.0(3) 2_656 . ?
O4 Sm2 O16 153.5(3) 2_656 . ?
O4 Sm2 C12 79.6(3) 2_656 2_756 ?
O7 Sm2 O8 51.6(3) 2_756 2_756 ?
O7 Sm2 O12 143.4(3) 2_756 . ?
O7 Sm2 O15 70.5(3) 2_756 . ?
O7 Sm2 C12 25.7(3) 2_756 2_756 ?
O8 Sm2 C12 26.2(3) 2_756 2_756 ?
O11 Sm2 O7 127.6(3) . 2_756 ?
O11 Sm2 O8 160.1(3) . 2_756 ?
O11 Sm2 O12 52.2(3) . . ?
O11 Sm2 O15 79.5(3) . . ?
O11 Sm2 C12 151.2(3) . 2_756 ?
O12 Sm2 O8 143.3(3) . 2_756 ?
O12 Sm2 C12 150.0(3) . 2_756 ?
O15 Sm2 O8 114.1(3) . 2_756 ?
O15 Sm2 O12 74.2(3) . . ?
O15 Sm2 C12 90.6(3) . 2_756 ?
O16 Sm2 O7 76.7(3) . 2_756 ?
O16 Sm2 O8 80.2(3) . 2_756 ?
O16 Sm2 O11 80.5(3) . . ?
O16 Sm2 O12 129.8(3) . . ?
O16 Sm2 O15 117.2(3) . . ?
O16 Sm2 C12 80.2(3) . 2_756 ?
C13 O6 Sm1 160.0(9) . 3_757 ?
O6 Sm1 O2 78.5(3) 3_757 3_657 ?
O6 Sm1 O5 87.7(3) 3_757 . ?
O6 Sm1 O9 148.4(3) 3_757 . ?
O6 Sm1 O10 157.4(3) 3_757 . ?
O6 Sm1 O13 101.6(3) 3_757 . ?
O6 Sm1 O14 77.4(4) 3_757 . ?
O1 Sm1 O6 97.6(3) . 3_757 ?
O1 Sm1 O2 89.7(3) . 3_657 ?
O1 Sm1 O5 76.2(3) . . ?
O1 Sm1 O9 74.8(4) . . ?
O1 Sm1 O10 94.0(3) . . ?
O1 Sm1 O13 146.3(4) . . ?
O1 Sm1 O14 145.0(3) . . ?
O2 Sm1 O5 158.8(3) 3_657 . ?
O2 Sm1 O9 71.0(3) 3_657 . ?
O2 Sm1 O10 121.0(3) 3_657 . ?
O2 Sm1 O13 67.6(3) 3_657 . ?
O2 Sm1 O14 122.2(3) 3_657 . ?
O5 Sm1 O9 118.9(3) . . ?
O5 Sm1 O10 76.4(3) . . ?
O5 Sm1 O13 131.6(3) . . ?
O5 Sm1 O14 69.0(3) . . ?
O9 Sm1 O14 126.1(4) . . ?
O10 Sm1 O9 53.8(3) . . ?
O10 Sm1 O13 78.4(3) . . ?
O10 Sm1 O14 82.0(4) . . ?
O13 Sm1 O9 74.3(3) . . ?
O13 Sm1 O14 67.1(3) . . ?
C25 O1 Sm1 160.4(9) . . ?
C25 O2 Sm1 129.8(7) . 3_657 ?
C26 O3 Sm2 149.5(8) . 4_565 ?
C26 O4 Sm2 139.7(8) . 2_646 ?
C13 O5 Sm1 130.8(7) . . ?
C12 O7 Sm2 95.8(7) . 2_746 ?
C12 O8 Sm2 90.5(7) . 2_746 ?
C27 O9 Sm1 87.6(7) . . ?
C27 O10 Sm1 94.2(7) . . ?
C33 O11 Sm2 94.3(7) . . ?
C33 O12 Sm2 91.8(8) . . ?
Sm1 O13 H13A 125(10) . . ?
Sm1 O13 H13B 124(10) . . ?
H13A O13 H13B 105.1(17) . . ?
Sm1 O14 H14A 120.3 . . ?
Sm1 O14 H14B 119.6 . . ?
H14A O14 H14B 120.0 . . ?
Sm2 O15 H15A 111.9 . . ?
Sm2 O15 H15B 112.1 . . ?
H15A O15 H15B 106.5 . . ?
Sm2 O16 H16A 103(10) . . ?
Sm2 O16 H16B 117(10) . . ?
H16A O16 H16B 104.9(18) . . ?
C18 N1 C14 116.7(11) . . ?
C1 N2 C5 117.0(14) . . ?
N2 C1 H1 117.6 . . ?
N2 C1 C2 124.8(15) . . ?
C2 C1 H1 117.6 . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 119.9(14) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 115.4(12) . . ?
C2 C3 C6 121.6(12) . . ?
C4 C3 C6 123.0(12) . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0(13) . . ?
C5 C4 H4 120.0 . . ?
N2 C5 C4 122.8(14) . . ?
N2 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?
C7 C6 C3 118.9(11) . . ?
C7 C6 C11 119.4(11) . . ?
C11 C6 C3 121.5(11) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0(10) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 120.9(10) . . ?
C7 C8 C13 121.5(10) . . ?
C9 C8 C13 117.6(10) . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.3(10) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 C12 116.0(10) . . ?
C11 C10 C9 119.6(10) . . ?
C11 C10 C12 124.3(10) . . ?
C6 C11 H11 119.6 . . ?
C10 C11 C6 120.7(10) . . ?
C10 C11 H11 119.6 . . ?
O7 C12 Sm2 58.5(6) . 2_746 ?
O7 C12 O8 120.6(10) . . ?
O7 C12 C10 118.9(10) . . ?
O8 C12 Sm2 63.3(6) . 2_746 ?
O8 C12 C10 120.4(10) . . ?
C10 C12 Sm2 165.3(8) . 2_746 ?
O6 C13 O5 124.8(10) . . ?
O6 C13 C8 117.7(10) . . ?
O5 C13 C8 117.4(10) . . ?
N1 C14 H14 118.3 . . ?
N1 C14 C15 123.5(12) . . ?
C15 C14 H14 118.3 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 120.1(12) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 116.2(11) . . ?
C15 C16 C19 121.2(11) . . ?
C17 C16 C19 122.6(11) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 C16 120.9(12) . . ?
C18 C17 H17 119.6 . . ?
N1 C18 C17 122.6(13) . . ?
N1 C18 H18 118.7 . . ?
C17 C18 H18 118.7 . . ?
C20 C19 C16 119.0(10) . . ?
C20 C19 C24 119.8(10) . . ?
C24 C19 C16 121.2(10) . . ?
C19 C20 H20 119.5 . . ?
C19 C20 C21 121.0(11) . . ?
C21 C20 H20 119.5 . . ?
C20 C21 C25 120.3(10) . . ?
C22 C21 C20 118.6(10) . . ?
C22 C21 C25 121.2(10) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.8(10) . . ?
C23 C22 H22 119.6 . . ?
C22 C23 C24 120.0(10) . . ?
C22 C23 C26 121.2(10) . . ?
C24 C23 C26 118.7(10) . . ?
C19 C24 H24 120.1 . . ?
C23 C24 C19 119.7(10) . . ?
C23 C24 H24 120.1 . . ?
O1 C25 C21 117.4(10) . . ?
O2 C25 O1 123.9(11) . . ?
O2 C25 C21 118.6(10) . . ?
O3 C26 O4 123.2(10) . . ?
O3 C26 C23 118.9(10) . . ?
O4 C26 C23 117.9(9) . . ?
O9 C27 C28 117.5(11) . . ?
O10 C27 O9 124.0(11) . . ?
O10 C27 C28 118.3(10) . . ?
C29 C28 C27 120.3(11) . . ?
C34 C28 C27 120.5(11) . . ?
C34 C28 C29 119.2(11) . . ?
C28 C29 H29 120.5 . . ?
C30 C29 C28 119.0(11) . . ?
C30 C29 H29 120.5 . . ?
C29 C30 H30 119.0 . . ?
C29 C30 C31 122.0(12) . . ?
C31 C30 H30 119.0 . . ?
C30 C31 H31 120.7 . . ?
C30 C31 C32 118.6(12) . . ?
C32 C31 H31 120.7 . . ?
C31 C32 C33 121.2(11) . . ?
C34 C32 C31 119.7(11) . . ?
C34 C32 C33 119.0(11) . . ?
O11 C33 O12 121.1(11) . . ?
O11 C33 C32 119.6(10) . . ?
O12 C33 C32 119.3(11) . . ?
C28 C34 H34 119.3 . . ?
C32 C34 C28 121.5(12) . . ?
C32 C34 H34 119.3 . . ?
H17A O17 H17B 109.6 . . ?

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
Sm2 O3 C26 O4 38(2) 4_565 . . . ?
Sm2 O3 C26 C23 -142.2(12) 4_565 . . . ?
Sm2 O4 C26 O3 -94.4(14) 2_646 . . . ?
Sm2 O4 C26 C23 85.9(13) 2_646 . . . ?
Sm2 O7 C12 O8 13.1(12) 2_746 . . . ?
Sm2 O7 C12 C10 -163.3(9) 2_746 . . . ?
Sm2 O8 C12 O7 -12.5(12) 2_746 . . . ?
Sm2 O8 C12 C10 163.8(10) 2_746 . . . ?
Sm2 O11 C33 O12 -8.0(13) . . . . ?
Sm2 O11 C33 C32 170.5(10) . . . . ?
Sm2 O12 C33 O11 7.8(13) . . . . ?
Sm2 O12 C33 C32 -170.7(10) . . . . ?
Sm1 O6 C13 O5 -109(2) 3_757 . . . ?
Sm1 O6 C13 C8 72(3) 3_757 . . . ?
Sm1 O1 C25 O2 111(2) . . . . ?
Sm1 O1 C25 C21 -73(3) . . . . ?
Sm1 O2 C25 O1 25.1(17) 3_657 . . . ?
Sm1 O2 C25 C21 -150.7(8) 3_657 . . . ?
Sm1 O5 C13 O6 -26.3(19) . . . . ?
Sm1 O5 C13 C8 152.5(8) . . . . ?
Sm1 O9 C27 O10 -6.4(12) . . . . ?
Sm1 O9 C27 C28 178.5(9) . . . . ?
Sm1 O10 C27 O9 6.7(13) . . . . ?
Sm1 O10 C27 C28 -178.2(9) . . . . ?
O9 C27 C28 C29 -20.4(17) . . . . ?
O9 C27 C28 C34 161.2(11) . . . . ?
O10 C27 C28 C29 164.2(11) . . . . ?
O10 C27 C28 C34 -14.3(17) . . . . ?
N1 C14 C15 C16 3(2) . . . . ?
N2 C1 C2 C3 -3(3) . . . . ?
C1 N2 C5 C4 -1(3) . . . . ?
C1 C2 C3 C4 4(2) . . . . ?
C1 C2 C3 C6 -175.4(14) . . . . ?
C2 C3 C4 C5 -5(2) . . . . ?
C2 C3 C6 C7 34.2(19) . . . . ?
C2 C3 C6 C11 -149.3(14) . . . . ?
C3 C4 C5 N2 3(3) . . . . ?
C3 C6 C7 C8 178.3(11) . . . . ?
C3 C6 C11 C10 -178.2(12) . . . . ?
C4 C3 C6 C7 -145.6(13) . . . . ?
C4 C3 C6 C11 31(2) . . . . ?
C5 N2 C1 C2 1(3) . . . . ?
C6 C3 C4 C5 175.1(14) . . . . ?
C6 C7 C8 C9 -1.6(17) . . . . ?
C6 C7 C8 C13 -178.9(11) . . . . ?
C7 C6 C11 C10 -1.7(18) . . . . ?
C7 C8 C9 C10 1.4(17) . . . . ?
C7 C8 C13 O6 -168.9(11) . . . . ?
C7 C8 C13 O5 12.3(17) . . . . ?
C8 C9 C10 C11 -1.3(17) . . . . ?
C8 C9 C10 C12 177.4(10) . . . . ?
C9 C8 C13 O6 13.7(16) . . . . ?
C9 C8 C13 O5 -165.2(11) . . . . ?
C9 C10 C11 C6 1.4(18) . . . . ?
C9 C10 C12 Sm2 -75(3) . . . 2_746 ?
C9 C10 C12 O7 1.0(16) . . . . ?
C9 C10 C12 O8 -175.4(10) . . . . ?
C11 C6 C7 C8 1.7(17) . . . . ?
C11 C10 C12 Sm2 104(3) . . . 2_746 ?
C11 C10 C12 O7 179.5(12) . . . . ?
C11 C10 C12 O8 3.1(18) . . . . ?
C12 C10 C11 C6 -177.1(11) . . . . ?
C13 C8 C9 C10 178.8(10) . . . . ?
C14 N1 C18 C17 1(2) . . . . ?
C14 C15 C16 C17 -1(2) . . . . ?
C14 C15 C16 C19 178.5(13) . . . . ?
C15 C16 C17 C18 0(2) . . . . ?
C15 C16 C19 C20 29.7(19) . . . . ?
C15 C16 C19 C24 -150.4(12) . . . . ?
C16 C17 C18 N1 0(3) . . . . ?
C16 C19 C20 C21 178.9(11) . . . . ?
C16 C19 C24 C23 179.8(11) . . . . ?
C17 C16 C19 C20 -150.3(13) . . . . ?
C17 C16 C19 C24 29.6(19) . . . . ?
C18 N1 C14 C15 -2(2) . . . . ?
C19 C16 C17 C18 -179.9(14) . . . . ?
C19 C20 C21 C22 -0.1(18) . . . . ?
C19 C20 C21 C25 -179.2(11) . . . . ?
C20 C19 C24 C23 -0.4(18) . . . . ?
C20 C21 C22 C23 2.5(17) . . . . ?
C20 C21 C25 O1 -25.8(17) . . . . ?
C20 C21 C25 O2 150.3(11) . . . . ?
C21 C22 C23 C24 -3.8(17) . . . . ?
C21 C22 C23 C26 179.9(10) . . . . ?
C22 C21 C25 O1 155.1(11) . . . . ?
C22 C21 C25 O2 -28.8(16) . . . . ?
C22 C23 C24 C19 2.7(17) . . . . ?
C22 C23 C26 O3 -167.9(11) . . . . ?
C22 C23 C26 O4 11.8(16) . . . . ?
C24 C19 C20 C21 -0.9(19) . . . . ?
C24 C23 C26 O3 15.7(16) . . . . ?
C24 C23 C26 O4 -164.6(11) . . . . ?
C25 C21 C22 C23 -178.4(10) . . . . ?
C26 C23 C24 C19 179.1(10) . . . . ?
C27 C28 C29 C30 -179.1(12) . . . . ?
C27 C28 C34 C32 -179.3(11) . . . . ?
C28 C29 C30 C31 -1(2) . . . . ?
C29 C28 C34 C32 2.2(18) . . . . ?
C29 C30 C31 C32 0(2) . . . . ?
C30 C31 C32 C33 176.3(12) . . . . ?
C30 C31 C32 C34 1.2(19) . . . . ?
C31 C32 C33 O11 -170.9(12) . . . . ?
C31 C32 C33 O12 7.6(19) . . . . ?
C31 C32 C34 C28 -2.5(18) . . . . ?
C33 C32 C34 C28 -177.8(11) . . . . ?
C34 C28 C29 C30 -0.6(19) . . . . ?
C34 C32 C33 O11 4.2(18) . . . . ?
C34 C32 C33 O12 -177.2(11) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1(10)
2 0(10)

####################################################################### 
# 
# 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_shelxl_CCDC8
_audit_block_doi                 10.5517/cc1j7mq3
_database_code_depnum_ccdc_archive 'CCDC 1407515'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C51 H39 N O29 Tb4, C3 H7 N O, 0.5(O2), 0.5(H2 O)'
_chemical_formula_sum            'C54 H49 N2 O31.50 Tb4'
_chemical_formula_weight         1865.63
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.860(2)
_cell_length_b                   14.210(3)
_cell_length_c                   20.130(4)
_cell_angle_alpha                86.63(3)
_cell_angle_beta                 83.76(3)
_cell_angle_gamma                78.72(3)
_cell_volume                     3026.2(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8991
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.713
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.992
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1798
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1304
_diffrn_reflns_av_unetI/netI     0.1219
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25032
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.150
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.2259
	          2theta: 29.8061
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.2259
	          2theta: 29.8061
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.2259
	          2theta: 29.8061
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.083955
_diffrn_orient_matrix_UB_12      -0.009393
_diffrn_orient_matrix_UB_13      0.042009
_diffrn_orient_matrix_UB_21      -0.030705
_diffrn_orient_matrix_UB_22      -0.062737
_diffrn_orient_matrix_UB_23      0.016605
_diffrn_orient_matrix_UB_31      0.014872
_diffrn_orient_matrix_UB_32      -0.016890
_diffrn_orient_matrix_UB_33      -0.044640
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9388
_reflns_number_total             10586
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.544
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         10586
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0404
_refine_ls_restrained_S_all      0.935
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0129P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0922
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H25A,H25B} of O25, {H27A,H27B} of O27, {H26A,H26B} of O26,
   {H28A,H28B} of O28
 At 1.5 times of:
  All C(H,H,H) groups, {H1AA,H1AB} of O1A
2. Restrained distances
 H27B-H27A
 1.39 with sigma of 0.01
 H27B-O27
 0.85 with sigma of 0.01
 O27-H27A
 0.85 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C44 \\sim O29 \\sim N2 \\sim C45 \\sim C46: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq, Uanis(O31) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O1B) = Uanis(O31)
4. Others
 Fixed Sof: O31(0.5) O1A(0.5) H1AA(0.5) H1AB(0.5) O1B(0.5)
5.a Fixed occupancy and ADP/Uiso:
 H27A, H27B
5.b Riding coordinates:
 O25(H25A,H25B), O26(H26A,H26B), O28(H28A,H28B)
5.c Free rotating group:
 O1A(H1AA,H1AB)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13), C16(H16),
 C19(H19), C20(H20), C21(H21), C23(H23), C27(H27), C28(H28), C29(H29), C32(H32),
  C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C49(H49), C50(H50),
 C51(H51), C53(H53), C44(H44)
5.e Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O11 O 0.5429(5) 0.4813(3) -0.1787(2) 0.0242(10) Uani 1 1 d . . . . .
C24 C 0.5037(7) 0.4091(4) -0.1949(3) 0.0207(14) Uani 1 1 d . . . . .
Tb1 Tb -0.08644(3) 1.23338(2) 0.19763(2) 0.01743(9) Uani 1 1 d . . . . .
Tb2 Tb 0.28915(3) 0.44449(2) 0.17358(2) 0.01628(9) Uani 1 1 d . . . . .
Tb3 Tb -0.27140(3) 1.30712(2) 0.69080(2) 0.01629(9) Uani 1 1 d . . . . .
Tb4 Tb -0.04557(3) 0.98793(2) 0.35276(2) 0.02062(9) Uani 1 1 d . . . . .
O1 O -0.2332(5) 1.0973(3) 0.3460(2) 0.0257(11) Uani 1 1 d . . . . .
O2 O -0.2585(5) 1.2186(3) 0.2691(2) 0.0293(11) Uani 1 1 d . . . . .
O3 O -0.2525(6) 1.2379(3) 0.5801(2) 0.0375(13) Uani 1 1 d . . . . .
O4 O -0.4170(5) 1.3476(4) 0.6073(2) 0.0405(14) Uani 1 1 d . . . . .
O5 O -0.0892(5) 1.0872(3) 0.1495(2) 0.0290(11) Uani 1 1 d . . . . .
O6 O -0.0470(6) 0.9922(4) 0.2403(2) 0.0457(15) Uani 1 1 d . . . . .
O7 O 0.2106(5) 0.6622(3) 0.2068(2) 0.0261(11) Uani 1 1 d . . . . .
O8 O 0.2077(5) 0.5917(3) 0.1118(2) 0.0333(13) Uani 1 1 d . . . . .
O9 O 0.3944(5) 0.4212(3) 0.0592(2) 0.0283(11) Uani 1 1 d . . . . .
O10 O 0.2123(5) 0.3737(4) 0.0798(2) 0.0365(13) Uani 1 1 d . . . . .
O12 O 0.5406(5) 0.3661(3) -0.2487(2) 0.0279(11) Uani 1 1 d . . . . .
O13 O 0.2719(6) 1.4564(4) 0.2872(2) 0.0396(14) Uani 1 1 d . . . . .
O14 O 0.2055(6) 1.5627(3) 0.3662(2) 0.0403(15) Uani 1 1 d . . . . .
O15 O 0.0034(5) 1.1857(3) 0.3030(2) 0.0328(12) Uani 1 1 d . . . . .
O16 O -0.0060(5) 1.1194(3) 0.4062(2) 0.0308(12) Uani 1 1 d . . . . .
O17 O 0.0732(5) 1.4648(3) 0.2039(2) 0.0303(11) Uani 1 1 d . . . . .
O18 O -0.0757(5) 1.3784(3) 0.2331(2) 0.0329(13) Uani 1 1 d . . . . .
O19 O 0.0570(5) 1.7674(3) 0.3245(2) 0.0286(11) Uani 1 1 d . . . . .
O20 O -0.1355(6) 1.8509(3) 0.3488(3) 0.0468(15) Uani 1 1 d . . . . .
O21 O 0.1705(5) -0.0262(3) 0.3115(3) 0.0356(12) Uani 1 1 d . . . . .
O22 O 0.2993(6) -0.1564(3) 0.2756(3) 0.0412(14) Uani 1 1 d . . . . .
O23 O 0.2765(5) 0.2802(3) 0.2077(2) 0.0289(11) Uani 1 1 d . . . . .
O24 O 0.4728(5) 0.3016(3) 0.1923(2) 0.0305(11) Uani 1 1 d . . . . .
O25 O 0.1242(5) 1.1788(3) 0.1611(3) 0.0406(13) Uani 1 1 d . . . . .
H25A H 0.156974 1.202664 0.125290 0.049 Uiso 1 1 d R . . . .
H25B H 0.168624 1.134874 0.183460 0.049 Uiso 1 1 d R . . . .
O26 O -0.0329(6) 1.3222(4) 0.0930(2) 0.0396(14) Uani 1 1 d . . . . .
H26A H 0.034624 1.344767 0.087999 0.048 Uiso 1 1 d R . . . .
H26B H -0.081526 1.330047 0.062009 0.048 Uiso 1 1 d R . . . .
O27 O -0.2709(5) 1.2937(4) 0.1444(2) 0.0349(12) Uani 1 1 d D . . . .
H27A H -0.277(6) 1.304(5) 0.1027(8) 0.042 Uiso 1 1 d D . . . .
H27B H -0.344(3) 1.296(5) 0.165(3) 0.042 Uiso 1 1 d D . . . .
O28 O 0.0666(5) 0.9104(3) 0.4414(2) 0.0321(12) Uani 1 1 d . . . . .
H28A H 0.028206 0.904149 0.480022 0.039 Uiso 1 1 d R . . . .
H28B H 0.145446 0.889019 0.434562 0.039 Uiso 1 1 d R . . . .
O30 O -0.1859(6) 0.9835(3) 0.4575(2) 0.0394(13) Uani 1 1 d . . . . .
N1 N -0.3272(8) 0.9248(5) 0.5338(4) 0.055(2) Uani 1 1 d . . . . .
C1 C -0.2748(6) 1.1835(5) 0.3284(3) 0.0198(14) Uani 1 1 d . . . . .
C2 C -0.3469(7) 1.2513(4) 0.3793(3) 0.0234(15) Uani 1 1 d . . . . .
C3 C -0.4364(7) 1.3294(5) 0.3613(3) 0.0269(16) Uani 1 1 d . . . . .
H3 H -0.453334 1.339218 0.316822 0.032 Uiso 1 1 calc R . . . .
C4 C -0.4998(8) 1.3918(5) 0.4074(4) 0.0365(18) Uani 1 1 d . . . . .
H4 H -0.558451 1.444721 0.394316 0.044 Uiso 1 1 calc R . . . .
C5 C -0.4767(7) 1.3765(5) 0.4748(3) 0.0319(17) Uani 1 1 d . . . . .
H5 H -0.525069 1.416111 0.506903 0.038 Uiso 1 1 calc R . . . .
C6 C -0.3819(7) 1.3021(5) 0.4937(3) 0.0259(15) Uani 1 1 d . . . . .
C7 C -0.3193(7) 1.2378(4) 0.4457(3) 0.0240(15) Uani 1 1 d . . . . .
H7 H -0.258823 1.185710 0.458089 0.029 Uiso 1 1 calc R . . . .
C8 C -0.3497(7) 1.2937(5) 0.5640(3) 0.0257(15) Uani 1 1 d . . . . .
C9 C -0.0509(7) 1.0051(5) 0.1780(3) 0.0256(15) Uani 1 1 d . . . . .
C10 C -0.0082(7) 0.9199(4) 0.1355(3) 0.0186(14) Uani 1 1 d . . . . .
C11 C -0.0335(7) 0.9267(4) 0.0685(3) 0.0248(15) Uani 1 1 d . . . . .
H11 H -0.078116 0.983558 0.050765 0.030 Uiso 1 1 calc R . . . .
C12 C 0.0088(8) 0.8477(5) 0.0285(3) 0.0287(17) Uani 1 1 d . . . . .
H12 H -0.008526 0.851801 -0.015892 0.034 Uiso 1 1 calc R . . . .
C13 C 0.0758(7) 0.7637(4) 0.0542(3) 0.0244(15) Uani 1 1 d . . . . .
H13 H 0.102142 0.711208 0.027084 0.029 Uiso 1 1 calc R . . . .
C14 C 0.1049(7) 0.7562(4) 0.1204(3) 0.0202(14) Uani 1 1 d . . . . .
C15 C 0.1800(7) 0.6652(4) 0.1481(3) 0.0223(15) Uani 1 1 d . . . . .
C16 C 0.0609(7) 0.8358(4) 0.1603(3) 0.0215(15) Uani 1 1 d . . . . .
H16 H 0.078792 0.831763 0.204678 0.026 Uiso 1 1 calc R . . . .
C17 C 0.3059(7) 0.3855(4) 0.0392(3) 0.0243(16) Uani 1 1 d . . . . .
C18 C 0.3150(7) 0.3578(5) -0.0321(3) 0.0281(16) Uani 1 1 d . . . . .
C19 C 0.2422(9) 0.2954(6) -0.0522(3) 0.044(2) Uani 1 1 d . . . . .
H19 H 0.187711 0.269221 -0.020823 0.053 Uiso 1 1 calc R . . . .
C20 C 0.2512(9) 0.2727(6) -0.1184(4) 0.047(2) Uani 1 1 d . . . . .
H20 H 0.200594 0.232882 -0.131668 0.056 Uiso 1 1 calc R . . . .
C21 C 0.3340(8) 0.3082(5) -0.1646(3) 0.039(2) Uani 1 1 d . . . . .
H21 H 0.341413 0.290531 -0.208853 0.047 Uiso 1 1 calc R . . . .
C22 C 0.4081(7) 0.3710(5) -0.1459(3) 0.0234(15) Uani 1 1 d . . . . .
C23 C 0.3960(7) 0.3961(4) -0.0800(3) 0.0210(14) Uani 1 1 d . . . . .
H23 H 0.442606 0.439238 -0.067378 0.025 Uiso 1 1 calc R . . . .
C25 C 0.2137(7) 1.4806(5) 0.3432(3) 0.0256(16) Uani 1 1 d . . . . .
C26 C 0.1505(7) 1.4105(4) 0.3852(3) 0.0225(15) Uani 1 1 d . . . . .
C27 C 0.1203(8) 1.4237(5) 0.4536(3) 0.0340(19) Uani 1 1 d . . . . .
H27 H 0.144114 1.474103 0.473309 0.041 Uiso 1 1 calc R . . . .
C28 C 0.0547(9) 1.3619(5) 0.4926(3) 0.039(2) Uani 1 1 d . . . . .
H28 H 0.036790 1.369939 0.538339 0.047 Uiso 1 1 calc R . . . .
C29 C 0.0159(8) 1.2877(5) 0.4627(3) 0.0312(18) Uani 1 1 d . . . . .
H29 H -0.031310 1.248153 0.488275 0.037 Uiso 1 1 calc R . . . .
C30 C 0.0482(7) 1.2730(4) 0.3944(3) 0.0223(15) Uani 1 1 d . . . . .
C31 C 0.0125(7) 1.1881(4) 0.3653(3) 0.0238(15) Uani 1 1 d . . . . .
C32 C 0.1158(7) 1.3339(4) 0.3557(3) 0.0203(14) Uani 1 1 d . . . . .
H32 H 0.137906 1.323782 0.310415 0.024 Uiso 1 1 calc R . . . .
C33 C -0.0284(7) 1.4530(4) 0.2341(3) 0.0201(14) Uani 1 1 d . . . . .
C34 C -0.1042(7) 1.5330(4) 0.2771(3) 0.0224(15) Uani 1 1 d . . . . .
C35 C -0.2202(8) 1.5258(5) 0.3090(4) 0.0347(18) Uani 1 1 d . . . . .
H35 H -0.252605 1.470688 0.305060 0.042 Uiso 1 1 calc R . . . .
C36 C -0.2905(8) 1.6004(6) 0.3474(4) 0.047(2) Uani 1 1 d . . . . .
H36 H -0.369669 1.595733 0.368486 0.056 Uiso 1 1 calc R . . . .
C37 C -0.2396(8) 1.6819(5) 0.3533(4) 0.0387(19) Uani 1 1 d . . . . .
H37 H -0.286011 1.732719 0.377854 0.046 Uiso 1 1 calc R . . . .
C38 C -0.1196(7) 1.6878(4) 0.3228(3) 0.0226(15) Uani 1 1 d . . . . .
C39 C -0.0605(8) 1.7741(5) 0.3316(3) 0.0268(16) Uani 1 1 d . . . . .
C40 C -0.0528(7) 1.6139(4) 0.2847(3) 0.0229(15) Uani 1 1 d . . . . .
H40 H 0.026854 1.617907 0.263949 0.027 Uiso 1 1 calc R . . . .
C41 C -0.2320(10) 0.9206(7) 0.4878(5) 0.059(3) Uani 1 1 d . . . . .
H41 H -0.192847 0.858636 0.476242 0.071 Uiso 1 1 calc R . . . .
C42 C -0.3773(14) 0.8477(9) 0.5684(5) 0.096(5) Uani 1 1 d . . . . .
H42A H -0.310914 0.792583 0.571796 0.143 Uiso 1 1 calc GR . . . .
H42B H -0.441617 0.831999 0.544321 0.143 Uiso 1 1 calc GR . . . .
H42C H -0.412883 0.866856 0.612462 0.143 Uiso 1 1 calc GR . . . .
C43 C -0.3868(13) 1.0215(8) 0.5580(5) 0.085(4) Uani 1 1 d . . . . .
H43A H -0.353804 1.031558 0.598792 0.128 Uiso 1 1 calc GR . . . .
H43B H -0.476460 1.025797 0.565980 0.128 Uiso 1 1 calc GR . . . .
H43C H -0.368632 1.069564 0.524834 0.128 Uiso 1 1 calc GR . . . .
C47 C 0.2714(8) -0.0672(4) 0.2853(3) 0.0246(16) Uani 1 1 d . . . . .
C48 C 0.3727(7) -0.0107(4) 0.2625(3) 0.0237(15) Uani 1 1 d . . . . .
C49 C 0.4970(9) -0.0565(5) 0.2480(4) 0.043(2) Uani 1 1 d . . . . .
H49 H 0.518694 -0.122705 0.254987 0.052 Uiso 1 1 calc R . . . .
C50 C 0.5916(9) -0.0040(5) 0.2229(5) 0.054(2) Uani 1 1 d . . . . .
H50 H 0.675123 -0.034843 0.214099 0.065 Uiso 1 1 calc R . . . .
C51 C 0.5569(8) 0.0946(5) 0.2116(4) 0.0332(17) Uani 1 1 d . . . . .
H51 H 0.618015 0.129794 0.194870 0.040 Uiso 1 1 calc R . . . .
C52 C 0.4343(7) 0.1408(4) 0.2246(3) 0.0233(15) Uani 1 1 d . . . . .
C53 C 0.3413(7) 0.0892(4) 0.2510(3) 0.0222(14) Uani 1 1 d . . . . .
H53 H 0.258677 0.121267 0.260956 0.027 Uiso 1 1 calc R . . . .
C54 C 0.3931(7) 0.2462(4) 0.2072(3) 0.0226(15) Uani 1 1 d . . . . .
O29 O 0.2400(9) 1.0698(6) 0.0625(4) 0.090(2) Uani 1 1 d . U . . .
N2 N 0.3568(10) 0.9234(7) 0.0409(5) 0.082(2) Uani 1 1 d . U . . .
C44 C 0.2908(13) 0.9935(9) 0.0811(7) 0.087(3) Uani 1 1 d . U . . .
H44 H 0.285364 0.979968 0.126996 0.104 Uiso 1 1 calc R . . . .
C45 C 0.4065(14) 0.8318(9) 0.0777(7) 0.102(3) Uani 1 1 d . U . . .
H45A H 0.494765 0.827511 0.081581 0.153 Uiso 1 1 calc GR . . . .
H45B H 0.394902 0.778349 0.053577 0.153 Uiso 1 1 calc GR . . . .
H45C H 0.361841 0.830657 0.121470 0.153 Uiso 1 1 calc GR . . . .
C46 C 0.3704(14) 0.9304(9) -0.0272(6) 0.100(3) Uani 1 1 d . U . . .
H46A H 0.322578 0.889120 -0.044704 0.150 Uiso 1 1 calc GR . . . .
H46B H 0.457919 0.911542 -0.043101 0.150 Uiso 1 1 calc GR . . . .
H46C H 0.340362 0.995614 -0.041843 0.150 Uiso 1 1 calc GR . . . .
O31 O 0.650(2) 0.3546(13) 0.0197(12) 0.031(3) Uani 0.5 1 d . U P . .
O1A O 0.9505(15) 0.5145(9) 0.0700(9) 0.077(5) Uani 0.5 1 d . . P . .
H1AA H 0.926775 0.565022 0.092261 0.115 Uiso 0.5 1 d G . P . .
H1AB H 0.886589 0.490886 0.064091 0.115 Uiso 0.5 1 d G . P . .
O1B O 0.663(2) 0.3774(13) 0.0278(12) 0.031(3) Uani 0.5 1 d . U P . .


_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
O11 C24 1.257(7) . ?
O11 Tb2 2.292(4) 2_665 ?
C24 O12 1.262(7) . ?
C24 C22 1.510(8) . ?
Tb1 O2 2.267(5) . ?
Tb1 O5 2.350(4) . ?
Tb1 O15 2.436(5) . ?
Tb1 O18 2.249(4) . ?
Tb1 O25 2.320(5) . ?
Tb1 O26 2.464(5) . ?
Tb1 O27 2.363(5) . ?
Tb2 O8 2.433(5) . ?
Tb2 O9 2.468(4) . ?
Tb2 O10 2.484(4) . ?
Tb2 O13 2.288(4) 1_545 ?
Tb2 O17 2.324(5) 1_545 ?
Tb2 O23 2.420(4) . ?
Tb2 O24 2.595(5) . ?
Tb3 O3 2.462(4) . ?
Tb3 O4 2.401(5) . ?
Tb3 O7 2.322(4) 2_576 ?
Tb3 O12 2.294(5) 1_466 ?
Tb3 O14 2.311(4) 2_586 ?
Tb3 O19 2.357(5) 2_586 ?
Tb3 O22 2.275(4) 2_566 ?
Tb4 O1 2.320(5) . ?
Tb4 O6 2.264(5) . ?
Tb4 O16 2.341(4) . ?
Tb4 O20 2.352(5) 1_545 ?
Tb4 O21 2.376(5) 1_565 ?
Tb4 O28 2.365(5) . ?
Tb4 O30 2.470(5) . ?
O1 C1 1.264(7) . ?
O2 C1 1.275(7) . ?
O3 C8 1.250(9) . ?
O4 C8 1.266(8) . ?
O5 C9 1.284(8) . ?
O6 C9 1.259(8) . ?
O7 C15 1.258(7) . ?
O8 C15 1.278(7) . ?
O9 C17 1.281(8) . ?
O10 C17 1.265(8) . ?
O13 C25 1.263(8) . ?
O14 C25 1.264(7) . ?
O15 C31 1.270(7) . ?
O16 C31 1.273(7) . ?
O17 C33 1.236(8) . ?
O18 C33 1.267(7) . ?
O19 C39 1.254(9) . ?
O20 C39 1.270(9) . ?
O21 C47 1.217(9) . ?
O22 C47 1.266(8) . ?
O23 C54 1.263(9) . ?
O24 C54 1.281(8) . ?
O25 H25A 0.8501 . ?
O25 H25B 0.8497 . ?
O26 H26A 0.8502 . ?
O26 H26B 0.8499 . ?
O27 H27A 0.851(10) . ?
O27 H27B 0.853(10) . ?
O28 H28A 0.8502 . ?
O28 H28B 0.8501 . ?
O30 C41 1.210(9) . ?
N1 C41 1.306(12) . ?
N1 C42 1.429(10) . ?
N1 C43 1.485(12) . ?
C1 C2 1.496(9) . ?
C2 C3 1.385(10) . ?
C2 C7 1.395(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.357(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.403(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.391(10) . ?
C6 C7 1.395(9) . ?
C6 C8 1.488(9) . ?
C7 H7 0.9300 . ?
C9 C10 1.493(8) . ?
C10 C11 1.399(8) . ?
C10 C16 1.379(9) . ?
C11 H11 0.9300 . ?
C11 C12 1.394(9) . ?
C12 H12 0.9300 . ?
C12 C13 1.375(9) . ?
C13 H13 0.9300 . ?
C13 C14 1.397(9) . ?
C14 C15 1.500(9) . ?
C14 C16 1.401(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.499(8) . ?
C18 C19 1.400(9) . ?
C18 C23 1.393(9) . ?
C19 H19 0.9300 . ?
C19 C20 1.377(10) . ?
C20 H20 0.9300 . ?
C20 C21 1.368(10) . ?
C21 H21 0.9300 . ?
C21 C22 1.405(9) . ?
C22 C23 1.378(8) . ?
C23 H23 0.9300 . ?
C25 C26 1.489(8) . ?
C26 C27 1.396(9) . ?
C26 C32 1.401(8) . ?
C27 H27 0.9300 . ?
C27 C28 1.391(9) . ?
C28 H28 0.9300 . ?
C28 C29 1.397(9) . ?
C29 H29 0.9300 . ?
C29 C30 1.401(9) . ?
C30 C31 1.505(8) . ?
C30 C32 1.392(8) . ?
C32 H32 0.9300 . ?
C33 C34 1.521(8) . ?
C34 C35 1.369(10) . ?
C34 C40 1.396(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.398(10) . ?
C36 H36 0.9300 . ?
C36 C37 1.393(9) . ?
C37 H37 0.9300 . ?
C37 C38 1.394(10) . ?
C38 C39 1.518(8) . ?
C38 C40 1.376(9) . ?
C40 H40 0.9300 . ?
C41 H41 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C47 C48 1.503(9) . ?
C48 C49 1.388(11) . ?
C48 C53 1.405(8) . ?
C49 H49 0.9300 . ?
C49 C50 1.418(11) . ?
C50 H50 0.9300 . ?
C50 C51 1.389(10) . ?
C51 H51 0.9300 . ?
C51 C52 1.370(11) . ?
C52 C53 1.402(9) . ?
C52 C54 1.509(9) . ?
C53 H53 0.9300 . ?
O29 C44 1.176(13) . ?
N2 C44 1.361(14) . ?
N2 C45 1.494(14) . ?
N2 C46 1.363(14) . ?
C44 H44 0.9300 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
O1A H1AA 0.8501 . ?
O1A H1AB 0.8498 . ?

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
C24 O11 Tb2 148.0(4) . 2_665 ?
O11 C24 O12 124.2(6) . . ?
O11 C24 C22 117.3(5) . . ?
O12 C24 C22 118.5(5) . . ?
O2 Tb1 O5 91.22(16) . . ?
O2 Tb1 O15 77.25(17) . . ?
O2 Tb1 O25 149.46(18) . . ?
O2 Tb1 O26 138.99(19) . . ?
O2 Tb1 O27 70.60(17) . . ?
O5 Tb1 O15 104.18(16) . . ?
O5 Tb1 O26 97.05(15) . . ?
O5 Tb1 O27 85.62(19) . . ?
O15 Tb1 O26 137.68(17) . . ?
O18 Tb1 O2 93.83(17) . . ?
O18 Tb1 O5 174.03(16) . . ?
O18 Tb1 O15 80.08(17) . . ?
O18 Tb1 O25 100.01(19) . . ?
O18 Tb1 O26 77.04(16) . . ?
O18 Tb1 O27 93.1(2) . . ?
O25 Tb1 O5 77.00(17) . . ?
O25 Tb1 O15 78.51(19) . . ?
O25 Tb1 O26 71.1(2) . . ?
O25 Tb1 O27 134.83(18) . . ?
O27 Tb1 O15 146.60(18) . . ?
O27 Tb1 O26 70.10(18) . . ?
O11 Tb2 O8 82.71(17) 2_665 . ?
O11 Tb2 O9 79.53(15) 2_665 . ?
O11 Tb2 O10 132.09(15) 2_665 . ?
O11 Tb2 O17 141.27(15) 2_665 1_545 ?
O11 Tb2 O23 127.01(17) 2_665 . ?
O11 Tb2 O24 77.08(15) 2_665 . ?
O8 Tb2 O9 75.58(16) . . ?
O8 Tb2 O10 80.95(16) . . ?
O8 Tb2 O24 149.28(16) . . ?
O9 Tb2 O10 52.83(16) . . ?
O9 Tb2 O24 78.16(16) . . ?
O10 Tb2 O24 95.66(17) . . ?
O13 Tb2 O11 82.46(17) 1_545 2_665 ?
O13 Tb2 O8 115.05(17) 1_545 . ?
O13 Tb2 O9 157.7(2) 1_545 . ?
O13 Tb2 O10 144.84(16) 1_545 . ?
O13 Tb2 O17 76.46(19) 1_545 1_545 ?
O13 Tb2 O23 80.34(16) 1_545 . ?
O13 Tb2 O24 85.12(19) 1_545 . ?
O17 Tb2 O8 77.50(18) 1_545 . ?
O17 Tb2 O9 125.78(17) 1_545 . ?
O17 Tb2 O10 77.11(17) 1_545 . ?
O17 Tb2 O23 81.07(17) 1_545 . ?
O17 Tb2 O24 131.82(15) 1_545 . ?
O23 Tb2 O8 149.31(17) . . ?
O23 Tb2 O9 100.21(15) . . ?
O23 Tb2 O10 72.99(16) . . ?
O23 Tb2 O24 51.85(15) . . ?
O4 Tb3 O3 53.08(17) . . ?
O7 Tb3 O3 157.75(18) 2_576 . ?
O7 Tb3 O4 148.77(16) 2_576 . ?
O7 Tb3 O19 80.90(16) 2_576 2_586 ?
O12 Tb3 O3 124.42(17) 1_466 . ?
O12 Tb3 O4 76.39(17) 1_466 . ?
O12 Tb3 O7 76.68(17) 1_466 2_576 ?
O12 Tb3 O14 106.49(19) 1_466 2_586 ?
O12 Tb3 O19 155.61(16) 1_466 2_586 ?
O14 Tb3 O3 85.51(17) 2_586 . ?
O14 Tb3 O4 77.38(19) 2_586 . ?
O14 Tb3 O7 95.48(16) 2_586 2_576 ?
O14 Tb3 O19 85.0(2) 2_586 2_586 ?
O19 Tb3 O3 77.04(17) 2_586 . ?
O19 Tb3 O4 127.73(16) 2_586 . ?
O22 Tb3 O3 81.39(17) 2_566 . ?
O22 Tb3 O4 101.5(2) 2_566 . ?
O22 Tb3 O7 93.28(17) 2_566 2_576 ?
O22 Tb3 O12 88.43(19) 2_566 1_466 ?
O22 Tb3 O14 164.1(2) 2_566 2_586 ?
O22 Tb3 O19 83.36(19) 2_566 2_586 ?
O1 Tb4 O16 78.24(17) . . ?
O1 Tb4 O20 95.31(18) . 1_545 ?
O1 Tb4 O21 138.26(16) . 1_565 ?
O1 Tb4 O28 134.80(16) . . ?
O1 Tb4 O30 69.21(17) . . ?
O6 Tb4 O1 82.36(18) . . ?
O6 Tb4 O16 120.41(18) . . ?
O6 Tb4 O20 83.9(2) . 1_545 ?
O6 Tb4 O21 75.9(2) . 1_565 ?
O6 Tb4 O28 142.68(19) . . ?
O6 Tb4 O30 141.7(2) . . ?
O16 Tb4 O20 153.14(18) . 1_545 ?
O16 Tb4 O21 82.65(18) . 1_565 ?
O16 Tb4 O28 78.66(16) . . ?
O16 Tb4 O30 79.21(17) . . ?
O20 Tb4 O21 116.88(18) 1_545 1_565 ?
O20 Tb4 O28 88.34(19) 1_545 . ?
O20 Tb4 O30 74.16(18) 1_545 . ?
O21 Tb4 O30 142.08(19) 1_565 . ?
O28 Tb4 O21 75.33(18) . 1_565 ?
O28 Tb4 O30 68.62(18) . . ?
C1 O1 Tb4 141.3(4) . . ?
C1 O2 Tb1 134.2(5) . . ?
C8 O3 Tb3 92.2(4) . . ?
C8 O4 Tb3 94.7(4) . . ?
C9 O5 Tb1 123.0(4) . . ?
C9 O6 Tb4 173.3(5) . . ?
C15 O7 Tb3 166.9(4) . 2_576 ?
C15 O8 Tb2 113.1(4) . . ?
C17 O9 Tb2 93.8(4) . . ?
C17 O10 Tb2 93.5(4) . . ?
C24 O12 Tb3 137.8(4) . 1_644 ?
C25 O13 Tb2 154.1(5) . 1_565 ?
C25 O14 Tb3 125.9(4) . 2_586 ?
C31 O15 Tb1 156.4(5) . . ?
C31 O16 Tb4 112.4(4) . . ?
C33 O17 Tb2 160.0(5) . 1_565 ?
C33 O18 Tb1 154.7(5) . . ?
C39 O19 Tb3 158.0(4) . 2_586 ?
C39 O20 Tb4 116.5(5) . 1_565 ?
C47 O21 Tb4 154.9(5) . 1_545 ?
C47 O22 Tb3 148.0(5) . 2_566 ?
C54 O23 Tb2 98.7(4) . . ?
C54 O24 Tb2 90.0(4) . . ?
Tb1 O25 H25A 120.1 . . ?
Tb1 O25 H25B 119.9 . . ?
H25A O25 H25B 120.0 . . ?
Tb1 O26 H26A 119.8 . . ?
Tb1 O26 H26B 120.2 . . ?
H26A O26 H26B 120.0 . . ?
Tb1 O27 H27A 128(4) . . ?
Tb1 O27 H27B 122(4) . . ?
H27A O27 H27B 109.3(18) . . ?
Tb4 O28 H28A 120.1 . . ?
Tb4 O28 H28B 119.9 . . ?
H28A O28 H28B 120.0 . . ?
C41 O30 Tb4 133.2(6) . . ?
C41 N1 C42 128.7(10) . . ?
C41 N1 C43 116.8(8) . . ?
C42 N1 C43 114.3(9) . . ?
O1 C1 O2 124.3(6) . . ?
O1 C1 C2 119.5(5) . . ?
O2 C1 C2 116.2(6) . . ?
C3 C2 C1 121.2(6) . . ?
C3 C2 C7 119.5(6) . . ?
C7 C2 C1 119.3(6) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.1(6) . . ?
C4 C3 H3 119.5 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.8(7) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.2(7) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C7 118.7(6) . . ?
C5 C6 C8 119.3(6) . . ?
C7 C6 C8 122.0(7) . . ?
C2 C7 C6 120.4(7) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
O3 C8 O4 119.5(6) . . ?
O3 C8 C6 120.6(6) . . ?
O4 C8 C6 119.7(7) . . ?
O5 C9 C10 118.5(6) . . ?
O6 C9 O5 123.6(6) . . ?
O6 C9 C10 117.9(6) . . ?
C11 C10 C9 119.6(6) . . ?
C16 C10 C9 121.0(5) . . ?
C16 C10 C11 119.3(5) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.5(6) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 119.7 . . ?
C13 C12 C11 120.7(6) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 H13 119.6 . . ?
C12 C13 C14 120.7(6) . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C15 120.8(5) . . ?
C13 C14 C16 118.1(6) . . ?
C16 C14 C15 121.1(6) . . ?
O7 C15 O8 121.8(6) . . ?
O7 C15 C14 119.4(5) . . ?
O8 C15 C14 118.7(5) . . ?
C10 C16 C14 121.6(6) . . ?
C10 C16 H16 119.2 . . ?
C14 C16 H16 119.2 . . ?
O9 C17 C18 119.4(6) . . ?
O10 C17 O9 119.8(6) . . ?
O10 C17 C18 120.7(6) . . ?
C19 C18 C17 121.6(6) . . ?
C23 C18 C17 119.5(6) . . ?
C23 C18 C19 118.9(6) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.1(6) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.8 . . ?
C21 C20 C19 120.5(7) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 119.7 . . ?
C20 C21 C22 120.5(6) . . ?
C22 C21 H21 119.7 . . ?
C21 C22 C24 122.1(5) . . ?
C23 C22 C24 119.0(5) . . ?
C23 C22 C21 118.8(6) . . ?
C18 C23 H23 119.5 . . ?
C22 C23 C18 121.0(6) . . ?
C22 C23 H23 119.5 . . ?
O13 C25 O14 123.1(6) . . ?
O13 C25 C26 119.7(6) . . ?
O14 C25 C26 117.2(6) . . ?
C27 C26 C25 119.9(5) . . ?
C27 C26 C32 119.8(6) . . ?
C32 C26 C25 120.2(5) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 C26 120.4(6) . . ?
C28 C27 H27 119.8 . . ?
C27 C28 H28 120.1 . . ?
C27 C28 C29 119.9(6) . . ?
C29 C28 H28 120.1 . . ?
C28 C29 H29 120.0 . . ?
C28 C29 C30 119.9(6) . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C31 118.2(6) . . ?
C32 C30 C29 120.0(5) . . ?
C32 C30 C31 121.7(6) . . ?
O15 C31 O16 122.6(5) . . ?
O15 C31 C30 121.1(6) . . ?
O16 C31 C30 116.3(5) . . ?
C26 C32 H32 120.0 . . ?
C30 C32 C26 120.0(5) . . ?
C30 C32 H32 120.0 . . ?
O17 C33 O18 125.5(6) . . ?
O17 C33 C34 118.6(5) . . ?
O18 C33 C34 115.9(6) . . ?
C35 C34 C33 121.1(5) . . ?
C35 C34 C40 120.0(6) . . ?
C40 C34 C33 118.9(6) . . ?
C34 C35 H35 119.6 . . ?
C34 C35 C36 120.8(6) . . ?
C36 C35 H35 119.6 . . ?
C35 C36 H36 120.6 . . ?
C37 C36 C35 118.8(7) . . ?
C37 C36 H36 120.6 . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.5(6) . . ?
C38 C37 H37 119.7 . . ?
C37 C38 C39 121.1(6) . . ?
C40 C38 C37 119.6(6) . . ?
C40 C38 C39 119.3(6) . . ?
O19 C39 O20 122.5(6) . . ?
O19 C39 C38 120.8(6) . . ?
O20 C39 C38 116.6(7) . . ?
C34 C40 H40 119.9 . . ?
C38 C40 C34 120.3(6) . . ?
C38 C40 H40 119.9 . . ?
O30 C41 N1 130.9(10) . . ?
O30 C41 H41 114.5 . . ?
N1 C41 H41 114.5 . . ?
N1 C42 H42A 109.5 . . ?
N1 C42 H42B 109.5 . . ?
N1 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N1 C43 H43A 109.5 . . ?
N1 C43 H43B 109.5 . . ?
N1 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O21 C47 O22 124.5(7) . . ?
O21 C47 C48 119.5(6) . . ?
O22 C47 C48 116.0(7) . . ?
C49 C48 C47 120.8(6) . . ?
C49 C48 C53 118.8(6) . . ?
C53 C48 C47 120.3(6) . . ?
C48 C49 H49 119.5 . . ?
C48 C49 C50 121.0(7) . . ?
C50 C49 H49 119.5 . . ?
C49 C50 H50 120.7 . . ?
C51 C50 C49 118.6(8) . . ?
C51 C50 H50 120.7 . . ?
C50 C51 H51 119.4 . . ?
C52 C51 C50 121.1(7) . . ?
C52 C51 H51 119.4 . . ?
C51 C52 C53 120.3(6) . . ?
C51 C52 C54 121.8(6) . . ?
C53 C52 C54 117.9(6) . . ?
C48 C53 H53 119.9 . . ?
C52 C53 C48 120.2(7) . . ?
C52 C53 H53 119.9 . . ?
O23 C54 O24 119.5(6) . . ?
O23 C54 C52 118.6(6) . . ?
O24 C54 C52 121.9(6) . . ?
C44 N2 C45 113.9(11) . . ?
C44 N2 C46 124.8(11) . . ?
C46 N2 C45 121.1(10) . . ?
O29 C44 N2 125.2(13) . . ?
O29 C44 H44 117.4 . . ?
N2 C44 H44 117.4 . . ?
N2 C45 H45A 109.5 . . ?
N2 C45 H45B 109.5 . . ?
N2 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N2 C46 H46A 109.5 . . ?
N2 C46 H46B 109.5 . . ?
N2 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
H1AA O1A H1AB 109.4 . . ?

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
O11 C24 O12 Tb3 47.7(10) . . . 1_644 ?
O11 C24 C22 C21 163.3(7) . . . . ?
O11 C24 C22 C23 -18.9(10) . . . . ?
C24 C22 C23 C18 -175.8(7) . . . . ?
Tb1 O2 C1 O1 -58.6(8) . . . . ?
Tb1 O2 C1 C2 120.6(6) . . . . ?
Tb1 O5 C9 O6 23.8(10) . . . . ?
Tb1 O5 C9 C10 -156.1(5) . . . . ?
Tb1 O15 C31 O16 113.1(10) . . . . ?
Tb1 O15 C31 C30 -67.8(14) . . . . ?
Tb1 O18 C33 O17 -7.4(16) . . . . ?
Tb1 O18 C33 C34 173.4(8) . . . . ?
Tb2 O11 C24 O12 -42.4(12) 2_665 . . . ?
Tb2 O11 C24 C22 136.4(6) 2_665 . . . ?
Tb2 O8 C15 O7 10.1(8) . . . . ?
Tb2 O8 C15 C14 -167.7(4) . . . . ?
Tb2 O9 C17 O10 -2.1(7) . . . . ?
Tb2 O9 C17 C18 178.2(5) . . . . ?
Tb2 O10 C17 O9 2.1(7) . . . . ?
Tb2 O10 C17 C18 -178.2(6) . . . . ?
Tb2 O13 C25 O14 -86.5(12) 1_565 . . . ?
Tb2 O13 C25 C26 93.4(11) 1_565 . . . ?
Tb2 O17 C33 O18 -66.4(15) 1_565 . . . ?
Tb2 O17 C33 C34 112.7(11) 1_565 . . . ?
Tb2 O23 C54 O24 1.4(6) . . . . ?
Tb2 O23 C54 C52 -178.8(4) . . . . ?
Tb2 O24 C54 O23 -1.3(6) . . . . ?
Tb2 O24 C54 C52 178.9(5) . . . . ?
Tb3 O3 C8 O4 -7.2(7) . . . . ?
Tb3 O3 C8 C6 168.6(6) . . . . ?
Tb3 O4 C8 O3 7.4(7) . . . . ?
Tb3 O4 C8 C6 -168.4(5) . . . . ?
Tb3 O7 C15 O8 146.7(17) 2_576 . . . ?
Tb3 O7 C15 C14 -36(2) 2_576 . . . ?
Tb3 O14 C25 O13 7.6(11) 2_586 . . . ?
Tb3 O14 C25 C26 -172.3(5) 2_586 . . . ?
Tb3 O19 C39 O20 169.2(8) 2_586 . . . ?
Tb3 O19 C39 C38 -8.1(16) 2_586 . . . ?
Tb3 O22 C47 O21 -29.3(15) 2_566 . . . ?
Tb3 O22 C47 C48 150.3(7) 2_566 . . . ?
Tb4 O1 C1 O2 61.8(9) . . . . ?
Tb4 O1 C1 C2 -117.4(6) . . . . ?
Tb4 O16 C31 O15 3.5(9) . . . . ?
Tb4 O16 C31 C30 -175.7(5) . . . . ?
Tb4 O20 C39 O19 8.1(9) 1_565 . . . ?
Tb4 O20 C39 C38 -174.5(4) 1_565 . . . ?
Tb4 O21 C47 O22 -13.6(17) 1_545 . . . ?
Tb4 O21 C47 C48 166.8(8) 1_545 . . . ?
Tb4 O30 C41 N1 -161.9(8) . . . . ?
O1 C1 C2 C3 -152.6(6) . . . . ?
O1 C1 C2 C7 30.3(9) . . . . ?
O2 C1 C2 C3 28.2(9) . . . . ?
O2 C1 C2 C7 -148.9(6) . . . . ?
O5 C9 C10 C11 -12.5(10) . . . . ?
O5 C9 C10 C16 164.5(6) . . . . ?
O6 C9 C10 C11 167.6(7) . . . . ?
O6 C9 C10 C16 -15.4(10) . . . . ?
O9 C17 C18 C19 161.9(7) . . . . ?
O9 C17 C18 C23 -19.2(10) . . . . ?
O10 C17 C18 C19 -17.7(11) . . . . ?
O10 C17 C18 C23 161.1(7) . . . . ?
O12 C24 C22 C21 -17.9(11) . . . . ?
O12 C24 C22 C23 159.9(6) . . . . ?
O13 C25 C26 C27 160.3(7) . . . . ?
O13 C25 C26 C32 -22.8(11) . . . . ?
O14 C25 C26 C27 -19.8(11) . . . . ?
O14 C25 C26 C32 157.1(7) . . . . ?
O17 C33 C34 C35 176.7(7) . . . . ?
O17 C33 C34 C40 -4.3(9) . . . . ?
O18 C33 C34 C35 -4.1(10) . . . . ?
O18 C33 C34 C40 174.9(6) . . . . ?
O21 C47 C48 C49 163.8(7) . . . . ?
O21 C47 C48 C53 -20.6(10) . . . . ?
O22 C47 C48 C49 -15.9(10) . . . . ?
O22 C47 C48 C53 159.7(6) . . . . ?
C1 C2 C3 C4 -178.7(6) . . . . ?
C1 C2 C7 C6 177.6(6) . . . . ?
C2 C3 C4 C5 -1.3(12) . . . . ?
C3 C2 C7 C6 0.4(10) . . . . ?
C3 C4 C5 C6 5.3(12) . . . . ?
C4 C5 C6 C7 -6.4(11) . . . . ?
C4 C5 C6 C8 173.4(7) . . . . ?
C5 C6 C7 C2 3.5(10) . . . . ?
C5 C6 C8 O3 -168.4(7) . . . . ?
C5 C6 C8 O4 7.3(10) . . . . ?
C7 C2 C3 C4 -1.5(11) . . . . ?
C7 C6 C8 O3 11.3(10) . . . . ?
C7 C6 C8 O4 -173.0(6) . . . . ?
C8 C6 C7 C2 -176.2(6) . . . . ?
C9 C10 C11 C12 178.7(6) . . . . ?
C9 C10 C16 C14 -178.1(6) . . . . ?
C10 C11 C12 C13 -0.6(11) . . . . ?
C11 C10 C16 C14 -1.0(10) . . . . ?
C11 C12 C13 C14 -1.1(11) . . . . ?
C12 C13 C14 C15 -178.9(6) . . . . ?
C12 C13 C14 C16 1.6(10) . . . . ?
C13 C14 C15 O7 176.2(6) . . . . ?
C13 C14 C15 O8 -6.0(10) . . . . ?
C13 C14 C16 C10 -0.6(10) . . . . ?
C15 C14 C16 C10 179.9(6) . . . . ?
C16 C10 C11 C12 1.6(10) . . . . ?
C16 C14 C15 O7 -4.4(10) . . . . ?
C16 C14 C15 O8 173.4(6) . . . . ?
C17 C18 C19 C20 178.9(8) . . . . ?
C17 C18 C23 C22 179.0(7) . . . . ?
C18 C19 C20 C21 2.1(15) . . . . ?
C19 C18 C23 C22 -2.1(11) . . . . ?
C19 C20 C21 C22 -2.2(15) . . . . ?
C20 C21 C22 C24 177.9(8) . . . . ?
C20 C21 C22 C23 0.1(13) . . . . ?
C21 C22 C23 C18 2.0(11) . . . . ?
C22 C24 O12 Tb3 -131.1(6) . . . 1_644 ?
C23 C18 C19 C20 0.0(13) . . . . ?
C25 C26 C27 C28 176.2(8) . . . . ?
C25 C26 C32 C30 -175.0(7) . . . . ?
C26 C27 C28 C29 -1.7(14) . . . . ?
C27 C26 C32 C30 1.9(11) . . . . ?
C27 C28 C29 C30 3.0(13) . . . . ?
C28 C29 C30 C31 175.7(7) . . . . ?
C28 C29 C30 C32 -1.8(12) . . . . ?
C29 C30 C31 O15 158.5(7) . . . . ?
C29 C30 C31 O16 -22.3(10) . . . . ?
C29 C30 C32 C26 -0.6(11) . . . . ?
C31 C30 C32 C26 -178.0(6) . . . . ?
C32 C26 C27 C28 -0.7(12) . . . . ?
C32 C30 C31 O15 -24.0(11) . . . . ?
C32 C30 C31 O16 155.1(7) . . . . ?
C33 C34 C35 C36 -178.7(7) . . . . ?
C33 C34 C40 C38 179.4(6) . . . . ?
C34 C35 C36 C37 -0.8(14) . . . . ?
C35 C34 C40 C38 -1.6(11) . . . . ?
C35 C36 C37 C38 -1.4(14) . . . . ?
C36 C37 C38 C39 -177.1(7) . . . . ?
C36 C37 C38 C40 2.2(12) . . . . ?
C37 C38 C39 O19 156.0(7) . . . . ?
C37 C38 C39 O20 -21.5(10) . . . . ?
C37 C38 C40 C34 -0.6(11) . . . . ?
C39 C38 C40 C34 178.6(6) . . . . ?
C40 C34 C35 C36 2.3(12) . . . . ?
C40 C38 C39 O19 -23.3(10) . . . . ?
C40 C38 C39 O20 159.3(7) . . . . ?
C42 N1 C41 O30 -179.4(11) . . . . ?
C43 N1 C41 O30 -4.7(17) . . . . ?
C47 C48 C49 C50 176.4(7) . . . . ?
C47 C48 C53 C52 -174.8(6) . . . . ?
C48 C49 C50 C51 -1.3(13) . . . . ?
C49 C48 C53 C52 0.9(10) . . . . ?
C49 C50 C51 C52 0.3(12) . . . . ?
C50 C51 C52 C53 1.3(11) . . . . ?
C50 C51 C52 C54 -174.8(7) . . . . ?
C51 C52 C53 C48 -1.9(10) . . . . ?
C51 C52 C54 O23 165.9(7) . . . . ?
C51 C52 C54 O24 -14.3(10) . . . . ?
C53 C48 C49 C50 0.7(12) . . . . ?
C53 C52 C54 O23 -10.3(9) . . . . ?
C53 C52 C54 O24 169.5(6) . . . . ?
C54 C52 C53 C48 174.4(5) . . . . ?
C45 N2 C44 O29 -177.4(13) . . . . ?
C46 N2 C44 O29 -2(2) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelxl_CCDC9
_audit_block_doi                 10.5517/cc1j7mw8
_database_code_depnum_ccdc_archive 'CCDC 1407520'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H26 N2 O16 Tb2, H2 O'
_chemical_formula_sum            'C34 H28 N2 O17 Tb2'
_chemical_formula_weight         1054.42
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.9650(14)
_cell_length_b                   26.433(5)
_cell_length_c                   17.879(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.90(3)
_cell_angle_gamma                90
_cell_volume                     3260.4(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7740
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.392
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.148
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32602
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.525
_diffrn_reflns_theta_min         3.052
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1407
	          2theta: 29.8659
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1407
	          2theta: 29.8659
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 30.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1407
	          2theta: 29.8659
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.048042
_diffrn_orient_matrix_UB_12      -0.009369
_diffrn_orient_matrix_UB_13      0.136426
_diffrn_orient_matrix_UB_21      -0.034893
_diffrn_orient_matrix_UB_22      -0.008785
_diffrn_orient_matrix_UB_23      0.011684
_diffrn_orient_matrix_UB_31      0.013681
_diffrn_orient_matrix_UB_32      -0.054785
_diffrn_orient_matrix_UB_33      -0.000332
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6400
_reflns_number_total             7476
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.493
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7476
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0352
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0333P)²+6.6295P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0849
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H7A of O7, H8A of O8, {H1A,H1B} of O1
 At 1.5 times of:
  All H(H) groups, H17A of O17, H7B of O7, {H2A,H2B} of O2
2. Restrained distances
 H7B-H7A
 1.39 with sigma of 0.01
 H7A-H7B
 1.39 with sigma of 0.01
 O7-H7B
 0.85 with sigma of 0.01
 H7A-O7
 0.85 with sigma of 0.01
 H17A-H2A_$1
 2.2 with sigma of 0.01
 H31_$2-H2B
 2.2 with sigma of 0.01
 H2B-O2
 0.85 with sigma of 0.01
 H2A-H2B
 1.39 with sigma of 0.01
 H2A-Tb2
 2.9 with sigma of 0.01
 H7B-H29_$3
 2.2 with sigma of 0.01
3.a Riding coordinates:
 O7(H7A), O1(H1A,H1B), O8(H8A), O17(H17A)
3.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C7(H7), C16(H16), C10(H10), C34(H34), C4(H4), C29(H29), C30(H30),
 C24(H24), C25(H25), C12(H12), C23(H23), C26(H26), C19(H19), C1(H1), C3(H3),
 C2(H2), C31(H31)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O7 O 1.0175(5) 0.08410(13) 0.97934(19) 0.0279(7) Uani 1 1 d D . . . .
H7A H 1.104220 0.065595 0.964171 0.034 Uiso 1 1 d DR . . . .
H7B H 1.070(3) 0.1081(3) 1.0059(8) 0.042 Uiso 1 1 d DR . . . .
O10 O 0.5799(5) -0.01989(11) 1.10114(17) 0.0236(6) Uani 1 1 d . . . . .
Tb1 Tb 0.68186(3) 0.07002(2) 0.93359(2) 0.01573(7) Uani 1 1 d . . . . .
Tb2 Tb 1.23679(3) -0.06827(2) 0.45074(2) 0.01699(7) Uani 1 1 d D . . . .
O6 O 0.8164(5) -0.01833(12) 0.91948(16) 0.0250(7) Uani 1 1 d . . . . .
O13 O 0.7069(5) 0.34360(12) 1.01452(19) 0.0278(7) Uani 1 1 d . . . . .
O9 O 0.6921(5) 0.05160(12) 1.05906(16) 0.0256(7) Uani 1 1 d . . . . .
O1 O 1.2302(6) -0.10837(14) 0.32585(19) 0.0380(9) Uani 1 1 d . . . . .
H1A H 1.125144 -0.120543 0.303123 0.046 Uiso 1 1 d R . . . .
H1B H 1.333513 -0.110043 0.305593 0.046 Uiso 1 1 d R . . . .
C21 C 0.6068(6) 0.10432(15) 1.1864(2) 0.0189(8) Uani 1 1 d . . . . .
H21 H 0.627014 0.123128 1.144244 0.023 Uiso 1 1 calc R . . . .
C11 C 0.9489(6) -0.06764(15) 0.6713(2) 0.0181(8) Uani 1 1 d . . . . .
O2 O 0.9085(6) -0.10192(18) 0.3945(2) 0.0510(11) Uani 1 1 d D . . . .
H2A H 0.8327(16) -0.0673(14) 0.3855(6) 0.077 Uiso 1 1 d DR . . . .
H2B H 0.815(2) -0.116(2) 0.413(2) 0.077 Uiso 1 1 d DR . . . .
C7 C 0.8970(6) -0.09933(17) 0.8168(2) 0.0220(9) Uani 1 1 d . . . . .
H7 H 0.878807 -0.109758 0.864962 0.026 Uiso 1 1 calc R . . . .
C18 C 0.5187(6) 0.01812(16) 1.3827(2) 0.0190(8) Uani 1 1 d . . . . .
C16 C 0.5727(6) 0.02311(16) 1.2456(2) 0.0182(8) Uani 1 1 d . . . . .
H16 H 0.566324 -0.011997 1.242730 0.022 Uiso 1 1 calc R . . . .
O16 O 0.3917(5) 0.11827(12) 0.9598(2) 0.0338(8) Uani 1 1 d . . . . .
C20 C 0.5810(6) 0.12921(16) 1.2535(2) 0.0207(9) Uani 1 1 d . . . . .
O5 O 0.8467(5) 0.03839(12) 0.83212(17) 0.0291(7) Uani 1 1 d . . . . .
O14 O 0.4500(5) 0.38381(12) 1.0420(2) 0.0336(8) Uani 1 1 d . . . . .
C15 C 0.6023(6) 0.05142(15) 1.1822(2) 0.0163(8) Uani 1 1 d . . . . .
C8 C 0.8946(6) -0.04771(16) 0.7994(2) 0.0194(8) Uani 1 1 d . . . . .
C9 C 0.8528(6) -0.00742(16) 0.8539(2) 0.0192(8) Uani 1 1 d . . . . .
O3 O 1.0436(5) -0.07994(12) 0.54993(17) 0.0259(7) Uani 1 1 d . . . . .
C10 C 0.9191(6) -0.03245(16) 0.7264(2) 0.0200(8) Uani 1 1 d . . . . .
H10 H 0.915413 0.001814 0.714435 0.024 Uiso 1 1 calc R . . . .
O8 O 0.5508(6) 0.11114(13) 0.81556(19) 0.0339(8) Uani 1 1 d . . . . .
H8A H 0.431358 0.107787 0.798557 0.041 Uiso 1 1 d R . . . .
C27 C 0.4884(7) 0.15826(16) 0.9714(2) 0.0232(9) Uani 1 1 d . . . . .
O11 O 0.4339(5) -0.02393(11) 1.37413(16) 0.0251(7) Uani 1 1 d . . . . .
O4 O 0.9390(6) -0.00362(13) 0.57851(19) 0.0352(9) Uani 1 1 d . . . . .
C34 C 0.4963(7) 0.25140(16) 0.9959(2) 0.0214(9) Uani 1 1 d . . . . .
H34 H 0.630867 0.249509 1.004027 0.026 Uiso 1 1 calc R . . . .
C6 C 0.9263(7) -0.13526(16) 0.7624(2) 0.0219(9) Uani 1 1 d . . . . .
C4 C 1.0134(9) -0.2091(2) 0.8506(3) 0.0406(13) Uani 1 1 d . . . . .
H4 H 1.051827 -0.186910 0.890211 0.049 Uiso 1 1 calc R . . . .
C29 C 0.1861(7) 0.21111(18) 0.9660(3) 0.0320(11) Uani 1 1 d . . . . .
H29 H 0.111265 0.182246 0.954815 0.038 Uiso 1 1 calc DR . . . .
C13 C 0.9780(6) -0.04890(16) 0.5937(2) 0.0202(8) Uani 1 1 d . . . . .
O12 O 0.5746(6) 0.03769(13) 1.44595(16) 0.0338(8) Uani 1 1 d . . . . .
C28 C 0.3889(7) 0.20746(16) 0.9790(2) 0.0235(9) Uani 1 1 d . . . . .
C30 C 0.0969(8) 0.25805(19) 0.9698(3) 0.0373(12) Uani 1 1 d . . . . .
H30 H -0.037532 0.260351 0.960683 0.045 Uiso 1 1 calc R . . . .
C5 C 0.9361(7) -0.19034(18) 0.7796(3) 0.0296(10) Uani 1 1 d . . . . .
N2 N 0.5925(7) 0.29116(16) 1.2696(2) 0.0393(11) Uani 1 1 d . . . . .
C24 C 0.6547(8) 0.26176(19) 1.3283(3) 0.0341(11) Uani 1 1 d . . . . .
H24 H 0.702823 0.277293 1.373740 0.041 Uiso 1 1 calc R . . . .
C25 C 0.5297(10) 0.2680(2) 1.2045(3) 0.0436(14) Uani 1 1 d . . . . .
H25 H 0.487681 0.287844 1.162452 0.052 Uiso 1 1 calc R . . . .
C14 C 0.6259(6) 0.02607(15) 1.1087(2) 0.0177(8) Uani 1 1 d . . . . .
C33 C 0.5271(7) 0.34467(16) 1.0203(2) 0.0221(9) Uani 1 1 d . . . . .
C32 C 0.4066(7) 0.29812(17) 1.0009(2) 0.0231(9) Uani 1 1 d . . . . .
C12 C 0.9516(6) -0.11867(16) 0.6892(2) 0.0210(9) Uani 1 1 d . . . . .
H12 H 0.970426 -0.142382 0.652471 0.025 Uiso 1 1 calc R . . . .
C23 C 0.6523(7) 0.20955(17) 1.3259(3) 0.0275(10) Uani 1 1 d . . . . .
H23 H 0.694340 0.190873 1.369135 0.033 Uiso 1 1 calc R . . . .
C22 C 0.5863(7) 0.18503(17) 1.2582(2) 0.0256(9) Uani 1 1 d . . . . .
C26 C 0.5241(9) 0.21573(18) 1.1965(3) 0.0344(12) Uani 1 1 d . . . . .
H26 H 0.478906 0.201307 1.149980 0.041 Uiso 1 1 calc R . . . .
C19 C 0.5570(6) 0.09970(16) 1.3169(2) 0.0208(9) Uani 1 1 d . . . . .
H19 H 0.543877 0.115703 1.362195 0.025 Uiso 1 1 calc R . . . .
C1 C 0.8773(9) -0.2271(2) 0.7247(3) 0.0387(12) Uani 1 1 d . . . . .
H1 H 0.822576 -0.217268 0.676511 0.046 Uiso 1 1 calc R . . . .
N1 N 0.9785(9) -0.29558(19) 0.8099(3) 0.0584(15) Uani 1 1 d . . . . .
C3 C 1.0326(10) -0.2608(2) 0.8618(4) 0.0507(15) Uani 1 1 d . . . . .
H3 H 1.087520 -0.271894 0.909348 0.061 Uiso 1 1 calc R . . . .
C2 C 0.9008(10) -0.2784(2) 0.7423(4) 0.0509(16) Uani 1 1 d . . . . .
H2 H 0.859841 -0.301924 0.704776 0.061 Uiso 1 1 calc R . . . .
C17 C 0.5526(6) 0.04786(17) 1.3136(2) 0.0183(8) Uani 1 1 d . . . . .
C31 C 0.2064(7) 0.30139(18) 0.9872(3) 0.0318(11) Uani 1 1 d . . . . .
H31 H 0.145571 0.332549 0.989504 0.038 Uiso 1 1 calc DR . . . .
O15 O 0.6721(5) 0.15759(12) 0.97298(18) 0.0265(7) Uani 1 1 d . . . . .
O17 O 0.1620(7) 0.0936(2) 0.7754(3) 0.0635(14) Uani 1 1 d . . . . .
H17A H 0.142366 0.076265 0.735082 0.095 Uiso 1 1 d DR . . . .
H8B H 0.591(10) 0.141(3) 0.801(4) 0.06(2) Uiso 1 1 d . . . . .
H17B H 0.101(13) 0.082(3) 0.814(5) 0.092 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
O7 H7A 0.8499 . ?
O7 H7B 0.846(10) . ?
O7 Tb1 2.398(3) . ?
O10 Tb1 2.270(3) 3_657 ?
O10 C14 1.259(5) . ?
Tb1 O6 2.542(3) . ?
Tb1 O9 2.287(3) . ?
Tb1 O16 2.488(3) . ?
Tb1 O5 2.425(3) . ?
Tb1 O8 2.437(3) . ?
Tb1 O15 2.423(3) . ?
Tb2 O13 2.429(3) 2_746 ?
Tb2 O1 2.466(3) . ?
Tb2 O2 2.530(4) . ?
Tb2 O14 2.510(3) 2_746 ?
Tb2 O3 2.389(3) . ?
Tb2 O11 2.377(3) 1_654 ?
Tb2 O4 2.282(3) 3_756 ?
Tb2 O12 2.263(3) 3_757 ?
Tb2 C33 2.834(4) 2_746 ?
O6 C9 1.266(5) . ?
O13 C33 1.271(6) . ?
O9 C14 1.253(5) . ?
O1 H1A 0.8500 . ?
O1 H1B 0.8500 . ?
C21 H21 0.9300 . ?
C21 C20 1.401(6) . ?
C21 C15 1.400(6) . ?
C11 C10 1.390(5) . ?
C11 C13 1.514(5) . ?
C11 C12 1.386(6) . ?
O2 H2A 1.06(3) . ?
O2 H2B 0.850(10) . ?
C7 H7 0.9300 . ?
C7 C8 1.399(6) . ?
C7 C6 1.394(6) . ?
C18 O11 1.258(5) . ?
C18 O12 1.255(5) . ?
C18 C17 1.511(5) . ?
C16 H16 0.9300 . ?
C16 C15 1.396(5) . ?
C16 C17 1.405(5) . ?
O16 C27 1.255(5) . ?
C20 C22 1.478(6) . ?
C20 C19 1.404(6) . ?
O5 C9 1.271(5) . ?
O14 C33 1.252(5) . ?
C15 C14 1.504(5) . ?
C8 C9 1.500(5) . ?
C8 C10 1.399(6) . ?
O3 C13 1.261(5) . ?
C10 H10 0.9300 . ?
O8 H8A 0.8501 . ?
O8 H8B 0.89(7) . ?
C27 C28 1.489(6) . ?
C27 O15 1.276(5) . ?
O4 C13 1.249(5) . ?
C34 H34 0.9300 . ?
C34 C28 1.392(6) . ?
C34 C32 1.393(6) . ?
C6 C5 1.488(6) . ?
C6 C12 1.413(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.401(7) . ?
C4 C3 1.384(8) . ?
C29 H29 0.9300 . ?
C29 C28 1.403(7) . ?
C29 C30 1.393(7) . ?
C30 H30 0.9300 . ?
C30 C31 1.388(7) . ?
C5 C1 1.401(7) . ?
N2 C24 1.330(7) . ?
N2 C25 1.335(7) . ?
C24 H24 0.9300 . ?
C24 C23 1.381(7) . ?
C25 H25 0.9300 . ?
C25 C26 1.389(7) . ?
C33 C32 1.503(6) . ?
C32 C31 1.384(7) . ?
C12 H12 0.9300 . ?
C23 H23 0.9300 . ?
C23 C22 1.394(6) . ?
C22 C26 1.390(6) . ?
C26 H26 0.9300 . ?
C19 H19 0.9300 . ?
C19 C17 1.372(6) . ?
C1 H1 0.9300 . ?
C1 C2 1.398(8) . ?
N1 C3 1.325(8) . ?
N1 C2 1.334(8) . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C31 H31 0.9300 . ?
O17 H17A 0.8499 . ?
O17 H17B 0.92(8) . ?

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
H7A O7 H7B 109.7 . . ?
Tb1 O7 H7A 120.3 . . ?
Tb1 O7 H7B 129.6(13) . . ?
C14 O10 Tb1 140.8(3) . 3_657 ?
O7 Tb1 O6 79.69(11) . . ?
O7 Tb1 O16 129.44(12) . . ?
O7 Tb1 O5 76.65(12) . . ?
O7 Tb1 O8 117.25(12) . . ?
O7 Tb1 O15 79.48(11) . . ?
O10 Tb1 O7 153.23(11) 3_657 . ?
O10 Tb1 O6 74.33(11) 3_657 . ?
O10 Tb1 O9 93.42(11) 3_657 . ?
O10 Tb1 O16 73.03(11) 3_657 . ?
O10 Tb1 O5 92.24(11) 3_657 . ?
O10 Tb1 O8 80.34(12) 3_657 . ?
O10 Tb1 O15 125.69(11) 3_657 . ?
O9 Tb1 O7 78.52(12) . . ?
O9 Tb1 O6 86.54(11) . . ?
O9 Tb1 O16 80.84(13) . . ?
O9 Tb1 O5 134.94(12) . . ?
O9 Tb1 O8 154.40(12) . . ?
O9 Tb1 O15 85.22(11) . . ?
O16 Tb1 O6 144.08(11) . . ?
O5 Tb1 O6 52.42(10) . . ?
O5 Tb1 O16 142.94(12) . . ?
O5 Tb1 O8 70.45(12) . . ?
O8 Tb1 O6 115.04(11) . . ?
O8 Tb1 O16 73.58(13) . . ?
O15 Tb1 O6 158.74(11) . . ?
O15 Tb1 O16 53.11(10) . . ?
O15 Tb1 O5 125.57(11) . . ?
O15 Tb1 O8 78.66(11) . . ?
O13 Tb2 O1 78.56(12) 2_746 . ?
O13 Tb2 O2 82.52(14) 2_746 . ?
O13 Tb2 O14 52.72(10) 2_746 2_746 ?
O13 Tb2 C33 26.54(11) 2_746 2_746 ?
O1 Tb2 O2 65.52(13) . . ?
O1 Tb2 O14 74.81(13) . 2_746 ?
O1 Tb2 C33 75.79(13) . 2_746 ?
O2 Tb2 C33 104.90(14) . 2_746 ?
O14 Tb2 O2 125.08(14) 2_746 . ?
O14 Tb2 C33 26.19(11) 2_746 2_746 ?
O3 Tb2 O13 76.93(10) . 2_746 ?
O3 Tb2 O1 132.40(12) . . ?
O3 Tb2 O2 71.29(12) . . ?
O3 Tb2 O14 118.07(11) . 2_746 ?
O3 Tb2 C33 97.55(12) . 2_746 ?
O11 Tb2 O13 122.31(11) 1_654 2_746 ?
O11 Tb2 O1 68.32(11) 1_654 . ?
O11 Tb2 O2 120.42(12) 1_654 . ?
O11 Tb2 O14 73.26(11) 1_654 2_746 ?
O11 Tb2 O3 156.96(11) 1_654 . ?
O11 Tb2 C33 97.99(12) 1_654 2_746 ?
O4 Tb2 O13 156.91(12) 3_756 2_746 ?
O4 Tb2 O1 101.99(13) 3_756 . ?
O4 Tb2 O2 76.96(15) 3_756 . ?
O4 Tb2 O14 150.12(12) 3_756 2_746 ?
O4 Tb2 O3 86.46(11) 3_756 . ?
O4 Tb2 O11 77.98(12) 3_756 1_654 ?
O4 Tb2 C33 175.93(12) 3_756 2_746 ?
O12 Tb2 O13 94.51(12) 3_757 2_746 ?
O12 Tb2 O1 145.97(13) 3_757 . ?
O12 Tb2 O2 147.30(13) 3_757 . ?
O12 Tb2 O14 74.65(13) 3_757 2_746 ?
O12 Tb2 O3 76.30(12) 3_757 . ?
O12 Tb2 O11 88.73(11) 3_757 1_654 ?
O12 Tb2 O4 97.04(14) 3_757 3_756 ?
O12 Tb2 C33 83.34(13) 3_757 2_746 ?
C9 O6 Tb1 90.4(2) . . ?
C33 O13 Tb2 94.8(3) . 2_756 ?
C14 O9 Tb1 147.7(3) . . ?
Tb2 O1 H1A 120.2 . . ?
Tb2 O1 H1B 119.8 . . ?
H1A O1 H1B 120.0 . . ?
C20 C21 H21 119.7 . . ?
C15 C21 H21 119.7 . . ?
C15 C21 C20 120.7(4) . . ?
C10 C11 C13 118.8(4) . . ?
C12 C11 C10 119.1(4) . . ?
C12 C11 C13 122.1(4) . . ?
Tb2 O2 H2A 99.3(12) . . ?
Tb2 O2 H2B 134(3) . . ?
H2A O2 H2B 92(2) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C6 C7 C8 120.5(4) . . ?
O11 C18 C17 118.9(4) . . ?
O12 C18 O11 123.8(4) . . ?
O12 C18 C17 117.3(4) . . ?
C15 C16 H16 120.1 . . ?
C15 C16 C17 119.7(4) . . ?
C17 C16 H16 120.1 . . ?
C27 O16 Tb1 91.8(3) . . ?
C21 C20 C22 120.8(4) . . ?
C21 C20 C19 118.2(4) . . ?
C19 C20 C22 120.9(4) . . ?
C9 O5 Tb1 95.6(2) . . ?
C33 O14 Tb2 91.5(3) . 2_756 ?
C21 C15 C14 119.2(3) . . ?
C16 C15 C21 119.8(4) . . ?
C16 C15 C14 121.0(4) . . ?
C7 C8 C9 123.1(4) . . ?
C7 C8 C10 119.3(4) . . ?
C10 C8 C9 117.5(4) . . ?
O6 C9 O5 119.9(4) . . ?
O6 C9 C8 121.5(4) . . ?
O5 C9 C8 118.6(4) . . ?
C13 O3 Tb2 131.7(3) . . ?
C11 C10 C8 121.1(4) . . ?
C11 C10 H10 119.4 . . ?
C8 C10 H10 119.4 . . ?
Tb1 O8 H8A 119.7 . . ?
Tb1 O8 H8B 124(5) . . ?
H8A O8 H8B 108.6 . . ?
O16 C27 C28 120.3(4) . . ?
O16 C27 O15 120.4(4) . . ?
O15 C27 C28 119.2(4) . . ?
C18 O11 Tb2 131.6(3) . 1_456 ?
C13 O4 Tb2 160.3(3) . 3_756 ?
C28 C34 H34 119.3 . . ?
C28 C34 C32 121.4(4) . . ?
C32 C34 H34 119.3 . . ?
C7 C6 C5 122.0(4) . . ?
C7 C6 C12 118.9(4) . . ?
C12 C6 C5 119.1(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.9(6) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C30 C29 C28 119.9(5) . . ?
O3 C13 C11 117.5(4) . . ?
O4 C13 C11 117.4(4) . . ?
O4 C13 O3 125.1(4) . . ?
C18 O12 Tb2 162.8(3) . 3_757 ?
C34 C28 C27 120.4(4) . . ?
C34 C28 C29 118.5(4) . . ?
C29 C28 C27 121.0(4) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 C29 120.7(5) . . ?
C31 C30 H30 119.6 . . ?
C4 C5 C6 122.4(5) . . ?
C1 C5 C6 122.2(5) . . ?
C1 C5 C4 115.4(5) . . ?
C24 N2 C25 116.9(4) . . ?
N2 C24 H24 118.0 . . ?
N2 C24 C23 123.9(5) . . ?
C23 C24 H24 118.0 . . ?
N2 C25 H25 118.4 . . ?
N2 C25 C26 123.1(5) . . ?
C26 C25 H25 118.4 . . ?
O10 C14 C15 117.9(4) . . ?
O9 C14 O10 123.8(4) . . ?
O9 C14 C15 118.3(4) . . ?
O13 C33 Tb2 58.6(2) . 2_756 ?
O13 C33 C32 119.2(4) . . ?
O14 C33 Tb2 62.3(2) . 2_756 ?
O14 C33 O13 120.9(4) . . ?
O14 C33 C32 119.9(4) . . ?
C32 C33 Tb2 176.8(3) . 2_756 ?
C34 C32 C33 120.0(4) . . ?
C31 C32 C34 119.6(4) . . ?
C31 C32 C33 120.5(4) . . ?
C11 C12 C6 121.1(4) . . ?
C11 C12 H12 119.5 . . ?
C6 C12 H12 119.5 . . ?
C24 C23 H23 120.2 . . ?
C24 C23 C22 119.6(4) . . ?
C22 C23 H23 120.2 . . ?
C23 C22 C20 121.1(4) . . ?
C26 C22 C20 122.3(4) . . ?
C26 C22 C23 116.6(4) . . ?
C25 C26 C22 119.9(5) . . ?
C25 C26 H26 120.1 . . ?
C22 C26 H26 120.1 . . ?
C20 C19 H19 119.2 . . ?
C17 C19 C20 121.7(4) . . ?
C17 C19 H19 119.2 . . ?
C5 C1 H1 119.9 . . ?
C2 C1 C5 120.1(6) . . ?
C2 C1 H1 119.9 . . ?
C3 N1 C2 116.1(5) . . ?
C4 C3 H3 117.6 . . ?
N1 C3 C4 124.8(6) . . ?
N1 C3 H3 117.6 . . ?
C1 C2 H2 118.2 . . ?
N1 C2 C1 123.7(6) . . ?
N1 C2 H2 118.2 . . ?
C16 C17 C18 120.8(4) . . ?
C19 C17 C18 119.3(3) . . ?
C19 C17 C16 119.9(4) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 C30 119.8(4) . . ?
C32 C31 H31 120.1 . . ?
C27 O15 Tb1 94.3(3) . . ?
H17A O17 H17B 115.3 . . ?

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
Tb1 O10 C14 O9 -95.4(5) 3_657 . . . ?
Tb1 O10 C14 C15 85.5(5) 3_657 . . . ?
Tb1 O6 C9 O5 12.8(4) . . . . ?
Tb1 O6 C9 C8 -164.3(4) . . . . ?
Tb1 O9 C14 O10 39.3(8) . . . . ?
Tb1 O9 C14 C15 -141.6(4) . . . . ?
Tb1 O16 C27 C28 170.0(4) . . . . ?
Tb1 O16 C27 O15 -6.6(5) . . . . ?
Tb1 O5 C9 O6 -13.5(4) . . . . ?
Tb1 O5 C9 C8 163.7(3) . . . . ?
Tb2 O13 C33 O14 -2.9(5) 2_756 . . . ?
Tb2 O13 C33 C32 177.2(3) 2_756 . . . ?
Tb2 O14 C33 O13 2.8(4) 2_756 . . . ?
Tb2 O14 C33 C32 -177.4(3) 2_756 . . . ?
Tb2 O3 C13 C11 -150.5(3) . . . . ?
Tb2 O3 C13 O4 27.9(7) . . . . ?
Tb2 O4 C13 C11 -73.3(10) 3_756 . . . ?
Tb2 O4 C13 O3 108.3(8) 3_756 . . . ?
O13 C33 C32 C34 16.5(6) . . . . ?
O13 C33 C32 C31 -162.8(4) . . . . ?
C21 C20 C22 C23 -149.1(5) . . . . ?
C21 C20 C22 C26 31.7(7) . . . . ?
C21 C20 C19 C17 -2.0(7) . . . . ?
C21 C15 C14 O10 -164.8(4) . . . . ?
C21 C15 C14 O9 16.0(6) . . . . ?
C7 C8 C9 O6 -0.2(7) . . . . ?
C7 C8 C9 O5 -177.4(4) . . . . ?
C7 C8 C10 C11 -1.1(7) . . . . ?
C7 C6 C5 C4 -33.2(7) . . . . ?
C7 C6 C5 C1 150.0(5) . . . . ?
C7 C6 C12 C11 0.4(7) . . . . ?
C16 C15 C14 O10 14.0(6) . . . . ?
C16 C15 C14 O9 -165.1(4) . . . . ?
O16 C27 C28 C34 176.5(4) . . . . ?
O16 C27 C28 C29 -6.5(7) . . . . ?
O16 C27 O15 Tb1 6.8(5) . . . . ?
C20 C21 C15 C16 -0.3(6) . . . . ?
C20 C21 C15 C14 178.6(4) . . . . ?
C20 C22 C26 C25 179.1(5) . . . . ?
C20 C19 C17 C18 -177.7(4) . . . . ?
C20 C19 C17 C16 0.1(7) . . . . ?
O14 C33 C32 C34 -163.4(4) . . . . ?
O14 C33 C32 C31 17.4(7) . . . . ?
C15 C21 C20 C22 179.8(4) . . . . ?
C15 C21 C20 C19 2.0(7) . . . . ?
C15 C16 C17 C18 179.5(4) . . . . ?
C15 C16 C17 C19 1.7(6) . . . . ?
C8 C7 C6 C5 177.9(4) . . . . ?
C8 C7 C6 C12 -0.7(7) . . . . ?
C9 C8 C10 C11 -176.8(4) . . . . ?
C10 C11 C13 O3 165.8(4) . . . . ?
C10 C11 C13 O4 -12.8(6) . . . . ?
C10 C11 C12 C6 -0.5(7) . . . . ?
C10 C8 C9 O6 175.4(4) . . . . ?
C10 C8 C9 O5 -1.8(6) . . . . ?
O11 C18 O12 Tb2 112.4(9) . . . 3_757 ?
O11 C18 C17 C16 -28.2(6) . . . . ?
O11 C18 C17 C19 149.6(4) . . . . ?
C34 C32 C31 C30 1.2(7) . . . . ?
C6 C7 C8 C9 176.5(4) . . . . ?
C6 C7 C8 C10 1.0(7) . . . . ?
C6 C5 C1 C2 175.9(5) . . . . ?
C4 C5 C1 C2 -1.1(8) . . . . ?
C29 C30 C31 C32 -0.1(8) . . . . ?
C13 C11 C10 C8 -178.9(4) . . . . ?
C13 C11 C12 C6 179.3(4) . . . . ?
O12 C18 O11 Tb2 27.2(7) . . . 1_456 ?
O12 C18 C17 C16 153.2(4) . . . . ?
O12 C18 C17 C19 -29.1(6) . . . . ?
C28 C27 O15 Tb1 -169.8(4) . . . . ?
C28 C34 C32 C33 179.2(4) . . . . ?
C28 C34 C32 C31 -1.5(7) . . . . ?
C28 C29 C30 C31 -0.6(8) . . . . ?
C30 C29 C28 C27 -176.8(5) . . . . ?
C30 C29 C28 C34 0.3(7) . . . . ?
C5 C6 C12 C11 -178.2(4) . . . . ?
C5 C4 C3 N1 -1.6(10) . . . . ?
C5 C1 C2 N1 -0.3(10) . . . . ?
N2 C24 C23 C22 1.8(8) . . . . ?
N2 C25 C26 C22 -0.1(10) . . . . ?
C24 N2 C25 C26 1.1(9) . . . . ?
C24 C23 C22 C20 -179.8(5) . . . . ?
C24 C23 C22 C26 -0.6(7) . . . . ?
C25 N2 C24 C23 -2.0(8) . . . . ?
C33 C32 C31 C30 -179.6(5) . . . . ?
C32 C34 C28 C27 177.9(4) . . . . ?
C32 C34 C28 C29 0.8(7) . . . . ?
C12 C11 C10 C8 0.9(7) . . . . ?
C12 C11 C13 O3 -14.0(6) . . . . ?
C12 C11 C13 O4 167.5(4) . . . . ?
C12 C6 C5 C4 145.4(5) . . . . ?
C12 C6 C5 C1 -31.4(7) . . . . ?
C23 C22 C26 C25 -0.1(8) . . . . ?
C22 C20 C19 C17 -179.7(4) . . . . ?
C19 C20 C22 C23 28.6(7) . . . . ?
C19 C20 C22 C26 -150.6(5) . . . . ?
C3 C4 C5 C6 -175.1(5) . . . . ?
C3 C4 C5 C1 2.0(8) . . . . ?
C3 N1 C2 C1 0.8(10) . . . . ?
C2 N1 C3 C4 0.2(10) . . . . ?
C17 C18 O11 Tb2 -151.4(3) . . . 1_456 ?
C17 C18 O12 Tb2 -69.0(12) . . . 3_757 ?
C17 C16 C15 C21 -1.6(6) . . . . ?
C17 C16 C15 C14 179.5(4) . . . . ?
O15 C27 C28 C34 -7.0(6) . . . . ?
O15 C27 C28 C29 170.1(4) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_shelxl_CCDC10
_audit_block_doi                 10.5517/cc1j7mn1
_database_code_depnum_ccdc_archive 'CCDC 1407513'
_audit_update_record             
;
2015-06-18 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;
_audit_creation_date             2017-12-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C51 H39 Eu4 N O29, C3 H7 N O, 1.5(H2 O)'
_chemical_formula_sum            'C54 H49 Eu4 N2 O31.50'
_chemical_formula_weight         1822.76
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.850(2)
_cell_length_b                   14.040(3)
_cell_length_c                   19.950(4)
_cell_angle_alpha                86.50(3)
_cell_angle_beta                 83.40(3)
_cell_angle_gamma                78.89(3)
_cell_volume                     2960.0(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8265
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.278
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.992
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.062
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1782
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1636
_diffrn_reflns_av_unetI/netI     0.1440
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24829
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.172
_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1253
	          2theta: 29.8765
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1253
	          2theta: 29.8765
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 16.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1253
	          2theta: 29.8765
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.088923
_diffrn_orient_matrix_UB_12      0.030738
_diffrn_orient_matrix_UB_13      0.007862
_diffrn_orient_matrix_UB_21      -0.008168
_diffrn_orient_matrix_UB_22      -0.052834
_diffrn_orient_matrix_UB_23      -0.049143
_diffrn_orient_matrix_UB_31      -0.002244
_diffrn_orient_matrix_UB_32      -0.032653
_diffrn_orient_matrix_UB_33      0.038428
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9391
_reflns_number_total             10353
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.307
_refine_diff_density_min         -2.743
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         10353
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0499
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0278P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1248
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H27_$1-H27B
 2.2 with sigma of 0.01
 H28A-H1AA
 2.2 with sigma of 0.01
 H1AA-H28B
 2.2 with sigma of 0.01
 H28B-H29A
 2.2 with sigma of 0.01
 H5_$2-H26A
 2.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O30 \\sim C56 \\sim N2 \\sim C57 \\sim C58: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: O1A(0.5) H1AA(0.5) H1AB(0.5)
5.a Riding coordinates:
 O26(H26A,H26B), O27(H27A,H27B), O28(H28A,H28B), O29(H29A,H29B), O31(H31A,H31B)
5.b Free rotating group:
 O1A(H1AA,H1AB)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13), C15(H15),
 C19(H19), C20(H20), C21(H21), C23(H23), C27(H27), C29(H29), C30(H30), C31(H31),
  C35(H35), C37(H37), C38(H38), C39(H39), C43(H43), C44(H44), C45(H45),
 C47(H47), C49(H49), C56(H56)
5.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.77307(3) 0.69368(2) 0.30966(2) 0.01345(10) Uani 1 1 d . . . . .
Eu2 Eu 0.41569(3) 0.23425(2) 0.19742(2) 0.01514(10) Uani 1 1 d . . . . .
Eu3 Eu 0.78940(3) 0.44245(2) 0.17304(2) 0.01385(10) Uani 1 1 d . . . . .
Eu4 Eu 0.45556(3) -0.01059(2) 0.35326(2) 0.01898(11) Uani 1 1 d . . . . .
O1 O 0.9548(5) 0.6329(4) 0.2495(3) 0.0379(13) Uani 1 1 d . . . . .
O2 O 0.9492(5) 0.5198(4) 0.1768(3) 0.0369(12) Uani 1 1 d . . . . .
O3 O 0.8929(5) 0.4190(4) 0.0613(3) 0.0401(13) Uani 1 1 d . . . . .
O4 O 0.7089(6) 0.3757(4) 0.0805(3) 0.0479(15) Uani 1 1 d . . . . .
O5 O 0.7042(6) 0.5890(4) 0.1168(3) 0.0400(14) Uani 1 1 d . . . . .
O6 O 0.7133(5) 0.6656(4) 0.2100(3) 0.0351(13) Uani 1 1 d . . . . .
O7 O 0.4163(5) 1.0896(4) 0.1530(3) 0.0408(14) Uani 1 1 d . . . . .
O8 O 0.4535(6) 0.9936(5) 0.2436(3) 0.0532(17) Uani 1 1 d . . . . .
O9 O 0.7783(6) 0.4517(4) 0.2841(3) 0.0424(14) Uani 1 1 d . . . . .
O10 O 0.7165(6) 0.5619(4) 0.3615(3) 0.0398(14) Uani 1 1 d . . . . .
O11 O 0.4955(6) 0.1172(4) 0.4043(3) 0.0405(13) Uani 1 1 d . . . . .
O12 O 0.5043(5) 0.1872(4) 0.3002(3) 0.0383(13) Uani 1 1 d . . . . .
O13 O 0.3761(6) 0.8523(4) 0.3492(3) 0.0502(16) Uani 1 1 d . . . . .
O14 O 0.5634(5) 0.7625(4) 0.3259(3) 0.0370(13) Uani 1 1 d . . . . .
O15 O 0.4263(6) 0.3761(4) 0.2318(3) 0.0435(14) Uani 1 1 d . . . . .
O16 O 0.5799(5) 0.4607(4) 0.2052(3) 0.0391(13) Uani 1 1 d . . . . .
O17 O 0.6660(6) 0.9733(4) 0.3115(3) 0.0447(15) Uani 1 1 d . . . . .
O18 O 0.8005(6) 0.8414(4) 0.2778(3) 0.0494(16) Uani 1 1 d . . . . .
O19 O 0.7796(5) 1.2806(4) 0.2044(3) 0.0386(13) Uani 1 1 d . . . . .
O20 O 0.9737(5) 1.3019(4) 0.1925(3) 0.0398(13) Uani 1 1 d . . . . .
O21 O 0.9182(5) 0.6563(4) 0.3900(3) 0.0446(14) Uani 1 1 d . . . . .
O22 O 0.7469(6) 0.7595(4) 0.4193(3) 0.0469(16) Uani 1 1 d . . . . .
O23 O 0.2723(5) 0.0968(4) 0.3451(3) 0.0379(13) Uani 1 1 d . . . . .
O24 O 0.2501(5) 0.2181(4) 0.2687(3) 0.0379(13) Uani 1 1 d . . . . .
O25 O 0.3172(6) -0.0148(4) 0.4564(3) 0.0516(16) Uani 1 1 d . . . . .
O26 O 0.5685(5) -0.0857(4) 0.4377(3) 0.0408(14) Uani 1 1 d . . . . .
H26A H 0.579903 -0.147235 0.442816 0.061 Uiso 1 1 d DR . . . .
H26B H 0.598053 -0.052845 0.464246 0.061 Uiso 1 1 d R . . . .
O27 O 0.6218(5) 0.1816(4) 0.1606(3) 0.0462(15) Uani 1 1 d . . . . .
H27A H 0.655174 0.204834 0.124127 0.069 Uiso 1 1 d R . . . .
H27B H 0.666054 0.138614 0.184167 0.069 Uiso 1 1 d DR . . . .
O28 O 0.4716(5) 0.3181(4) 0.0933(3) 0.0467(15) Uani 1 1 d . . . . .
H28A H 0.540709 0.339078 0.087166 0.070 Uiso 1 1 d DR . . . .
H28B H 0.422179 0.326758 0.062496 0.070 Uiso 1 1 d DR . . . .
O29 O 0.2336(5) 0.2922(4) 0.1471(3) 0.0470(15) Uani 1 1 d . . . . .
H29A H 0.238166 0.323629 0.109409 0.070 Uiso 1 1 d DR . . . .
H29B H 0.162516 0.282109 0.165699 0.070 Uiso 1 1 d R . . . .
N1 N 0.1753(9) -0.0759(6) 0.5329(5) 0.068(3) Uani 1 1 d . . . . .
C1 C 0.7221(7) 0.4782(5) 0.3394(4) 0.0275(16) Uani 1 1 d . . . . .
C2 C 0.6547(8) 0.4096(5) 0.3830(4) 0.0325(17) Uani 1 1 d . . . . .
C3 C 0.6234(9) 0.4246(6) 0.4520(4) 0.041(2) Uani 1 1 d . . . . .
H3 H 0.647300 0.475732 0.471591 0.049 Uiso 1 1 calc R . . . .
C4 C 0.5562(10) 0.3623(7) 0.4910(4) 0.049(2) Uani 1 1 d . . . . .
H4 H 0.536950 0.368267 0.537408 0.059 Uiso 1 1 calc R . . . .
C5 C 0.5203(10) 0.2929(6) 0.4580(4) 0.050(2) Uani 1 1 d . . . . .
H5 H 0.469041 0.255032 0.483296 0.060 Uiso 1 1 calc DR . . . .
C6 C 0.5504(7) 0.2724(5) 0.3926(4) 0.0291(16) Uani 1 1 d . . . . .
C7 C 0.6199(7) 0.3334(5) 0.3537(4) 0.0317(17) Uani 1 1 d . . . . .
H7 H 0.642949 0.322826 0.307974 0.038 Uiso 1 1 calc R . . . .
C8 C 0.5154(7) 0.1890(5) 0.3623(4) 0.0331(17) Uani 1 1 d . . . . .
C9 C 0.4736(7) 0.4511(5) 0.2354(4) 0.0288(16) Uani 1 1 d . . . . .
C10 C 0.4004(7) 0.5307(5) 0.2767(4) 0.0339(18) Uani 1 1 d . . . . .
C11 C 0.2793(8) 0.5263(6) 0.3065(5) 0.044(2) Uani 1 1 d . . . . .
H11 H 0.243425 0.472514 0.301264 0.052 Uiso 1 1 calc R . . . .
C12 C 0.2122(9) 0.6035(7) 0.3442(5) 0.057(3) Uani 1 1 d . . . . .
H12 H 0.131531 0.600237 0.364595 0.069 Uiso 1 1 calc R . . . .
C13 C 0.2622(8) 0.6842(6) 0.3518(5) 0.047(2) Uani 1 1 d . . . . .
H13 H 0.215031 0.735449 0.376458 0.057 Uiso 1 1 calc R . . . .
C14 C 0.3855(8) 0.6894(5) 0.3222(4) 0.0342(18) Uani 1 1 d . . . . .
C15 C 0.4529(7) 0.6105(5) 0.2859(4) 0.0288(16) Uani 1 1 d . . . . .
H15 H 0.535270 0.611741 0.267373 0.035 Uiso 1 1 calc R . . . .
C16 C 0.4475(7) 0.7722(5) 0.3320(4) 0.0316(17) Uani 1 1 d . . . . .
C17 C 0.6788(7) 0.6647(5) 0.1514(4) 0.0288(16) Uani 1 1 d . . . . .
C18 C 0.6065(7) 0.7554(5) 0.1231(4) 0.0272(16) Uani 1 1 d . . . . .
C19 C 0.5769(7) 0.7621(5) 0.0567(4) 0.0339(18) Uani 1 1 d . . . . .
H19 H 0.602807 0.708264 0.030131 0.041 Uiso 1 1 calc R . . . .
C20 C 0.5103(9) 0.8464(6) 0.0292(4) 0.042(2) Uani 1 1 d . . . . .
H20 H 0.493400 0.849945 -0.015686 0.050 Uiso 1 1 calc R . . . .
C21 C 0.4688(8) 0.9259(5) 0.0699(4) 0.0323(18) Uani 1 1 d . . . . .
H21 H 0.423590 0.982937 0.051833 0.039 Uiso 1 1 calc R . . . .
C22 C 0.4935(7) 0.9215(5) 0.1366(4) 0.0266(15) Uani 1 1 d . . . . .
C23 C 0.5631(7) 0.8362(5) 0.1625(4) 0.0286(16) Uani 1 1 d . . . . .
H23 H 0.581130 0.833011 0.207174 0.034 Uiso 1 1 calc R . . . .
C24 C 0.4511(7) 1.0082(5) 0.1813(4) 0.0292(17) Uani 1 1 d . . . . .
C25 C 0.7716(8) 0.9307(5) 0.2862(4) 0.0330(18) Uani 1 1 d . . . . .
C26 C 0.8729(8) 0.9883(5) 0.2634(4) 0.0345(18) Uani 1 1 d . . . . .
C27 C 0.8461(7) 1.0887(5) 0.2534(4) 0.0337(18) Uani 1 1 d . . . . .
H27 H 0.764982 1.121741 0.266772 0.040 Uiso 1 1 calc DR . . . .
C28 C 0.9338(8) 1.1408(5) 0.2249(4) 0.0320(17) Uani 1 1 d . . . . .
C29 C 1.0618(8) 1.0941(6) 0.2139(5) 0.046(2) Uani 1 1 d . . . . .
H29 H 1.124488 1.128981 0.197724 0.055 Uiso 1 1 calc R . . . .
C30 C 1.0914(9) 0.9943(6) 0.2281(6) 0.070(3) Uani 1 1 d . . . . .
H30 H 1.175248 0.962724 0.222281 0.084 Uiso 1 1 calc R . . . .
C31 C 0.9982(9) 0.9411(6) 0.2507(5) 0.049(2) Uani 1 1 d . . . . .
H31 H 1.019266 0.874023 0.257335 0.059 Uiso 1 1 calc R . . . .
C32 C 0.8968(7) 1.2470(5) 0.2067(4) 0.0295(16) Uani 1 1 d . . . . .
C33 C 0.8491(7) 0.7056(5) 0.4350(4) 0.0311(17) Uani 1 1 d . . . . .
C34 C 0.8831(8) 0.6980(5) 0.5055(4) 0.0344(18) Uani 1 1 d . . . . .
C35 C 0.8164(7) 0.7640(5) 0.5542(4) 0.0293(16) Uani 1 1 d . . . . .
H35 H 0.755222 0.815884 0.541575 0.035 Uiso 1 1 calc R . . . .
C36 C 0.8432(7) 0.7504(5) 0.6201(4) 0.0312(16) Uani 1 1 d . . . . .
C37 C 0.9305(8) 0.6704(6) 0.6399(4) 0.0367(19) Uani 1 1 d . . . . .
H37 H 0.942888 0.658323 0.685197 0.044 Uiso 1 1 calc R . . . .
C38 C 0.9999(9) 0.6079(6) 0.5906(4) 0.047(2) Uani 1 1 d . . . . .
H38 H 1.061903 0.556405 0.602958 0.056 Uiso 1 1 calc R . . . .
C39 C 0.9754(8) 0.6234(6) 0.5237(4) 0.042(2) Uani 1 1 d . . . . .
H39 H 1.022122 0.582730 0.491055 0.050 Uiso 1 1 calc R . . . .
C40 C 0.2326(7) 0.1813(5) 0.3281(4) 0.0293(16) Uani 1 1 d . . . . .
C41 C 0.9900(7) 0.5907(5) 0.1941(4) 0.0268(15) Uani 1 1 d . . . . .
C42 C 1.0845(7) 0.6300(5) 0.1457(3) 0.0271(15) Uani 1 1 d . . . . .
C43 C 1.1579(8) 0.6935(6) 0.1656(4) 0.041(2) Uani 1 1 d . . . . .
H43 H 1.149560 0.711265 0.210327 0.049 Uiso 1 1 calc R . . . .
C44 C 1.2434(9) 0.7297(7) 0.1178(5) 0.053(2) Uani 1 1 d . . . . .
H44 H 1.293678 0.770445 0.131064 0.064 Uiso 1 1 calc R . . . .
C45 C 1.2539(9) 0.7060(6) 0.0521(5) 0.049(2) Uani 1 1 d . . . . .
H45 H 1.310042 0.731352 0.020408 0.059 Uiso 1 1 calc R . . . .
C46 C 1.1803(7) 0.6436(5) 0.0320(4) 0.0292(16) Uani 1 1 d . . . . .
C47 C 1.0976(7) 0.6054(5) 0.0788(4) 0.0328(17) Uani 1 1 d . . . . .
H47 H 1.050193 0.562793 0.065301 0.039 Uiso 1 1 calc R . . . .
C48 C 0.8071(7) 0.3843(5) 0.0404(4) 0.0306(17) Uani 1 1 d . . . . .
C49 C 0.2672(11) -0.0811(7) 0.4877(6) 0.066(3) Uani 1 1 d . . . . .
H49 H 0.304202 -0.143869 0.475392 0.079 Uiso 1 1 calc R . . . .
C51 C 0.1127(13) 0.0210(9) 0.5595(6) 0.086(4) Uani 1 1 d . . . . .
H51A H 0.094527 0.015121 0.607625 0.129 Uiso 1 1 calc GR . . . .
H51B H 0.035455 0.043295 0.539388 0.129 Uiso 1 1 calc GR . . . .
H51C H 0.167985 0.066739 0.548411 0.129 Uiso 1 1 calc GR . . . .
C53 C 0.1259(15) -0.1547(10) 0.5660(7) 0.100(5) Uani 1 1 d . . . . .
H53A H 0.147757 -0.210068 0.538099 0.150 Uiso 1 1 calc GR . . . .
H53B H 0.035697 -0.136969 0.574171 0.150 Uiso 1 1 calc GR . . . .
H53C H 0.160917 -0.170624 0.608265 0.150 Uiso 1 1 calc GR . . . .
O30 O 0.7397(10) 1.0745(7) 0.0623(5) 0.105(2) Uani 1 1 d . U . . .
N2 N 0.8532(11) 0.9237(8) 0.0396(7) 0.095(3) Uani 1 1 d . U . . .
C56 C 0.7845(14) 0.9938(11) 0.0814(9) 0.098(3) Uani 1 1 d . U . . .
H56 H 0.772017 0.977754 0.127303 0.118 Uiso 1 1 calc R . . . .
C57 C 0.9049(16) 0.8392(11) 0.0715(9) 0.118(3) Uani 1 1 d . U . . .
H57A H 0.989585 0.841982 0.079795 0.177 Uiso 1 1 calc GR . . . .
H57B H 0.906392 0.785653 0.043563 0.177 Uiso 1 1 calc GR . . . .
H57C H 0.855239 0.830589 0.113688 0.177 Uiso 1 1 calc GR . . . .
C58 C 0.8712(16) 0.9315(11) -0.0309(9) 0.116(3) Uani 1 1 d . U . . .
H58A H 0.842633 0.879079 -0.049447 0.173 Uiso 1 1 calc GR . . . .
H58B H 0.959383 0.928332 -0.045370 0.173 Uiso 1 1 calc GR . . . .
H58C H 0.824112 0.992308 -0.046332 0.173 Uiso 1 1 calc GR . . . .
O31 O 0.1592(7) 0.3670(5) 0.0255(3) 0.0632(19) Uani 1 1 d . . . . .
H31A H 0.190544 0.395350 -0.009368 0.095 Uiso 1 1 d R . . . .
H31B H 0.081774 0.362270 0.029532 0.095 Uiso 1 1 d R . . . .
O1A O 0.4531(14) 0.5144(10) 0.0683(7) 0.064(4) Uani 0.5 1 d . . P . .
H1AA H 0.406090 0.478271 0.089734 0.095 Uiso 0.5 1 d DG . P . .
H1AB H 0.523864 0.504601 0.084390 0.095 Uiso 0.5 1 d G . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.233(6) . ?
Eu1 O6 2.241(5) . ?
Eu1 O10 2.220(5) . ?
Eu1 O14 2.288(6) . ?
Eu1 O18 2.198(5) . ?
Eu1 O21 2.341(5) . ?
Eu1 O22 2.392(6) . ?
Eu1 C1 3.187(7) . ?
Eu2 Eu4 4.4835(15) . ?
Eu2 O7 2.265(5) 1_545 ?
Eu2 O12 2.368(5) . ?
Eu2 O15 2.174(5) . ?
Eu2 O24 2.198(6) . ?
Eu2 O27 2.267(6) . ?
Eu2 H27A 2.8013 . ?
Eu2 H27B 2.7793 . ?
Eu2 O28 2.399(5) . ?
Eu2 O29 2.304(5) . ?
Eu2 H29A 2.8187 . ?
Eu2 C24 3.154(7) 1_545 ?
Eu2 C40 3.230(8) . ?
Eu3 O2 2.227(5) . ?
Eu3 O3 2.390(6) . ?
Eu3 O4 2.439(6) . ?
Eu3 O5 2.360(5) . ?
Eu3 O9 2.215(6) . ?
Eu3 O16 2.260(6) . ?
Eu3 O19 2.339(5) 1_545 ?
Eu3 O20 2.571(6) 1_545 ?
Eu3 C32 2.839(7) 1_545 ?
Eu4 O8 2.187(6) 1_545 ?
Eu4 O11 2.251(5) . ?
Eu4 O13 2.265(5) 1_545 ?
Eu4 O17 2.312(6) 1_545 ?
Eu4 O23 2.268(5) . ?
Eu4 O25 2.408(6) . ?
Eu4 O26 2.283(5) . ?
Eu4 H26A 2.7983 . ?
Eu4 H26B 2.8138 . ?
Eu4 C16 3.123(7) 1_545 ?
O1 C41 1.271(9) . ?
O2 C41 1.246(8) . ?
O3 C48 1.251(9) . ?
O4 C48 1.277(10) . ?
O5 C17 1.272(9) . ?
O6 C17 1.269(8) . ?
O7 C24 1.253(8) . ?
O8 C24 1.251(9) . ?
O9 C1 1.240(10) . ?
O10 C1 1.268(9) . ?
O11 C8 1.305(9) . ?
O12 C8 1.262(9) . ?
O13 C16 1.278(9) . ?
O14 C16 1.231(9) . ?
O15 C9 1.265(9) . ?
O16 C9 1.265(9) . ?
O17 C25 1.251(10) . ?
O18 C25 1.248(9) . ?
O19 C32 1.273(9) . ?
O20 C32 1.240(9) . ?
O21 C33 1.254(9) . ?
O22 C33 1.276(9) . ?
O23 C40 1.223(8) . ?
O24 C40 1.271(9) . ?
O25 C49 1.264(11) . ?
O26 H26A 0.8501 . ?
O26 H26B 0.8499 . ?
O27 H27A 0.8501 . ?
O27 H27B 0.8499 . ?
O28 H28A 0.8499 . ?
O28 H28B 0.8500 . ?
O29 H29A 0.8496 . ?
O29 H29B 0.8502 . ?
N1 C49 1.260(14) . ?
N1 C51 1.498(14) . ?
N1 C53 1.416(13) . ?
C1 C2 1.497(10) . ?
C2 C3 1.398(11) . ?
C2 C7 1.384(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.391(11) . ?
C4 H4 0.9300 . ?
C4 C5 1.349(11) . ?
C5 H5 0.9300 . ?
C5 C6 1.342(11) . ?
C6 C7 1.392(10) . ?
C6 C8 1.481(10) . ?
C7 H7 0.9300 . ?
C9 C10 1.477(10) . ?
C10 C11 1.390(11) . ?
C10 C15 1.381(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.393(12) . ?
C12 H12 0.9300 . ?
C12 C13 1.371(12) . ?
C13 H13 0.9300 . ?
C13 C14 1.412(12) . ?
C14 C15 1.397(10) . ?
C14 C16 1.485(10) . ?
C15 H15 0.9300 . ?
C17 C18 1.478(9) . ?
C18 C19 1.392(10) . ?
C18 C23 1.395(10) . ?
C19 H19 0.9300 . ?
C19 C20 1.381(10) . ?
C20 H20 0.9300 . ?
C20 C21 1.394(11) . ?
C21 H21 0.9300 . ?
C21 C22 1.384(10) . ?
C22 C23 1.392(9) . ?
C22 C24 1.519(10) . ?
C23 H23 0.9300 . ?
C25 C26 1.501(10) . ?
C26 C27 1.390(10) . ?
C26 C31 1.395(12) . ?
C27 H27 0.9300 . ?
C27 C28 1.363(11) . ?
C28 C29 1.415(12) . ?
C28 C32 1.501(9) . ?
C29 H29 0.9300 . ?
C29 C30 1.395(11) . ?
C30 H30 0.9300 . ?
C30 C31 1.389(13) . ?
C31 H31 0.9300 . ?
C33 C34 1.486(10) . ?
C34 C35 1.420(11) . ?
C34 C39 1.366(10) . ?
C35 H35 0.9300 . ?
C35 C36 1.374(10) . ?
C36 C37 1.391(10) . ?
C36 C40 1.512(11) 2_666 ?
C37 H37 0.9300 . ?
C37 C38 1.408(12) . ?
C38 H38 0.9300 . ?
C38 C39 1.388(11) . ?
C39 H39 0.9300 . ?
C41 C42 1.487(10) . ?
C42 C43 1.406(10) . ?
C42 C47 1.385(10) . ?
C43 H43 0.9300 . ?
C43 C44 1.396(12) . ?
C44 H44 0.9300 . ?
C44 C45 1.361(12) . ?
C45 H45 0.9300 . ?
C45 C46 1.397(11) . ?
C46 C47 1.376(11) . ?
C46 C48 1.504(10) 2_765 ?
C47 H47 0.9300 . ?
C49 H49 0.9300 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
O30 C56 1.202(14) . ?
N2 C56 1.377(18) . ?
N2 C57 1.365(16) . ?
N2 C58 1.398(18) . ?
C56 H56 0.9300 . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
O31 H31A 0.8500 . ?
O31 H31B 0.8500 . ?
O1A H1AA 0.8503 . ?
O1A H1AB 0.8498 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 O6 76.5(2) . . ?
O1 Eu1 O14 155.72(19) . . ?
O1 Eu1 O21 75.9(2) . . ?
O1 Eu1 O22 127.1(2) . . ?
O1 Eu1 C1 89.0(2) . . ?
O6 Eu1 O14 80.2(2) . . ?
O6 Eu1 O21 149.2(2) . . ?
O6 Eu1 O22 155.8(2) . . ?
O6 Eu1 C1 80.10(18) . . ?
O10 Eu1 O1 102.5(2) . . ?
O10 Eu1 O6 94.5(2) . . ?
O10 Eu1 O14 85.8(2) . . ?
O10 Eu1 O21 78.6(2) . . ?
O10 Eu1 O22 86.3(2) . . ?
O10 Eu1 C1 17.7(2) . . ?
O14 Eu1 O21 128.4(2) . . ?
O14 Eu1 O22 75.7(2) . . ?
O14 Eu1 C1 93.55(19) . . ?
O18 Eu1 O1 89.8(2) . . ?
O18 Eu1 O6 93.4(2) . . ?
O18 Eu1 O10 166.7(2) . . ?
O18 Eu1 O14 84.9(2) . . ?
O18 Eu1 O21 99.8(2) . . ?
O18 Eu1 O22 82.1(2) . . ?
O18 Eu1 C1 173.5(2) . . ?
O21 Eu1 O22 54.58(19) . . ?
O21 Eu1 C1 86.17(19) . . ?
O22 Eu1 C1 103.7(2) . . ?
Eu4 Eu2 H27A 102.3 . . ?
Eu4 Eu2 H27B 72.2 . . ?
Eu4 Eu2 H29A 138.0 . . ?
O7 Eu2 Eu4 67.94(14) 1_545 . ?
O7 Eu2 O12 102.52(19) 1_545 . ?
O7 Eu2 O27 76.5(2) 1_545 . ?
O7 Eu2 H27A 80.3 1_545 . ?
O7 Eu2 H27B 73.9 1_545 . ?
O7 Eu2 O28 96.9(2) 1_545 . ?
O7 Eu2 O29 86.9(2) 1_545 . ?
O7 Eu2 H29A 89.1 1_545 . ?
O7 Eu2 C24 19.00(18) 1_545 1_545 ?
O7 Eu2 C40 90.9(2) 1_545 . ?
O12 Eu2 Eu4 38.92(13) . . ?
O12 Eu2 H27A 91.5 . . ?
O12 Eu2 H27B 64.7 . . ?
O12 Eu2 O28 137.19(19) . . ?
O12 Eu2 H29A 158.8 . . ?
O12 Eu2 C24 83.55(18) . 1_545 ?
O12 Eu2 C40 61.39(19) . . ?
O15 Eu2 Eu4 115.94(15) . . ?
O15 Eu2 O7 174.7(2) . 1_545 ?
O15 Eu2 O12 80.2(2) . . ?
O15 Eu2 O24 94.1(2) . . ?
O15 Eu2 O27 99.7(2) . . ?
O15 Eu2 H27A 95.2 . . ?
O15 Eu2 H27B 103.5 . . ?
O15 Eu2 O28 78.2(2) . . ?
O15 Eu2 O29 93.4(2) . . ?
O15 Eu2 H29A 89.8 . . ?
O15 Eu2 C24 163.29(19) . 1_545 ?
O15 Eu2 C40 94.4(2) . . ?
O24 Eu2 Eu4 61.62(13) . . ?
O24 Eu2 O7 91.0(2) . 1_545 ?
O24 Eu2 O12 77.0(2) . . ?
O24 Eu2 O27 149.04(19) . . ?
O24 Eu2 H27A 163.8 . . ?
O24 Eu2 H27B 133.7 . . ?
O24 Eu2 O28 140.81(19) . . ?
O24 Eu2 O29 70.27(19) . . ?
O24 Eu2 H29A 85.3 . . ?
O24 Eu2 C24 85.8(2) . 1_545 ?
O24 Eu2 C40 16.01(17) . . ?
O27 Eu2 Eu4 87.42(14) . . ?
O27 Eu2 O12 78.3(2) . . ?
O27 Eu2 H27A 15.1 . . ?
O27 Eu2 H27B 15.5 . . ?
O27 Eu2 O28 69.7(2) . . ?
O27 Eu2 O29 135.6(2) . . ?
O27 Eu2 H29A 122.1 . . ?
O27 Eu2 C24 73.2(2) . 1_545 ?
O27 Eu2 C40 134.06(19) . . ?
H27A Eu2 H27B 30.6 . . ?
H27A Eu2 H29A 108.0 . . ?
H27B Eu2 H29A 136.3 . . ?
O28 Eu2 Eu4 155.32(14) . . ?
O28 Eu2 H27A 54.6 . . ?
O28 Eu2 H27B 85.2 . . ?
O28 Eu2 H29A 56.7 . . ?
O28 Eu2 C24 112.2(2) . 1_545 ?
O28 Eu2 C40 156.27(19) . . ?
O29 Eu2 Eu4 124.07(13) . . ?
O29 Eu2 O12 146.1(2) . . ?
O29 Eu2 H27A 122.3 . . ?
O29 Eu2 H27B 148.2 . . ?
O29 Eu2 O28 71.91(17) . . ?
O29 Eu2 H29A 15.2 . . ?
O29 Eu2 C24 102.2(2) . 1_545 ?
O29 Eu2 C40 86.25(19) . . ?
C24 Eu2 Eu4 49.73(14) 1_545 . ?
C24 Eu2 H27A 81.6 1_545 . ?
C24 Eu2 H27B 65.8 1_545 . ?
C24 Eu2 H29A 106.8 1_545 . ?
C24 Eu2 C40 80.9(2) 1_545 . ?
C40 Eu2 Eu4 47.49(13) . . ?
C40 Eu2 H27A 149.1 . . ?
C40 Eu2 H27B 118.5 . . ?
C40 Eu2 H29A 101.3 . . ?
O2 Eu3 O3 79.59(19) . . ?
O2 Eu3 O4 132.5(2) . . ?
O2 Eu3 O5 81.88(19) . . ?
O2 Eu3 O16 140.0(2) . . ?
O2 Eu3 O19 128.36(19) . 1_545 ?
O2 Eu3 O20 77.65(18) . 1_545 ?
O2 Eu3 C32 102.9(2) . 1_545 ?
O3 Eu3 O4 53.73(19) . . ?
O3 Eu3 O20 78.02(19) . 1_545 ?
O3 Eu3 C32 88.4(2) . 1_545 ?
O4 Eu3 O20 98.3(2) . 1_545 ?
O4 Eu3 C32 85.7(2) . 1_545 ?
O5 Eu3 O3 78.5(2) . . ?
O5 Eu3 O4 80.9(2) . . ?
O5 Eu3 O20 151.2(2) . 1_545 ?
O5 Eu3 C32 165.1(2) . 1_545 ?
O9 Eu3 O2 81.8(2) . . ?
O9 Eu3 O3 155.7(2) . . ?
O9 Eu3 O4 145.39(19) . . ?
O9 Eu3 O5 114.0(2) . . ?
O9 Eu3 O16 77.1(2) . . ?
O9 Eu3 O19 81.0(2) . 1_545 ?
O9 Eu3 O20 82.9(2) . 1_545 ?
O9 Eu3 C32 80.8(2) . 1_545 ?
O16 Eu3 O3 127.02(19) . . ?
O16 Eu3 O4 76.6(2) . . ?
O16 Eu3 O5 76.4(2) . . ?
O16 Eu3 O19 81.3(2) . 1_545 ?
O16 Eu3 O20 131.70(18) . 1_545 ?
O16 Eu3 C32 106.7(2) . 1_545 ?
O19 Eu3 O3 98.7(2) 1_545 . ?
O19 Eu3 O4 73.20(19) 1_545 . ?
O19 Eu3 O5 149.04(18) 1_545 . ?
O19 Eu3 O20 52.15(18) 1_545 1_545 ?
O19 Eu3 C32 26.3(2) 1_545 1_545 ?
O20 Eu3 C32 25.90(19) 1_545 1_545 ?
Eu2 Eu4 H26A 156.6 . . ?
Eu2 Eu4 H26B 133.0 . . ?
O8 Eu4 Eu2 47.40(17) 1_545 . ?
O8 Eu4 O11 120.3(2) 1_545 . ?
O8 Eu4 O13 83.5(3) 1_545 1_545 ?
O8 Eu4 O17 75.8(2) 1_545 1_545 ?
O8 Eu4 O23 81.2(2) 1_545 . ?
O8 Eu4 O25 141.1(2) 1_545 . ?
O8 Eu4 O26 141.8(2) 1_545 . ?
O8 Eu4 H26A 132.2 1_545 . ?
O8 Eu4 H26B 147.7 1_545 . ?
O8 Eu4 C16 80.0(2) 1_545 1_545 ?
O11 Eu4 Eu2 74.96(13) . . ?
O11 Eu4 O13 154.5(2) . 1_545 ?
O11 Eu4 O17 83.1(2) . 1_545 ?
O11 Eu4 O23 79.3(2) . . ?
O11 Eu4 O25 79.8(2) . . ?
O11 Eu4 O26 78.37(19) . . ?
O11 Eu4 H26A 93.7 . . ?
O11 Eu4 H26B 63.3 . . ?
O11 Eu4 C16 157.42(19) . 1_545 ?
O13 Eu4 Eu2 124.43(16) 1_545 . ?
O13 Eu4 O17 113.8(2) 1_545 1_545 ?
O13 Eu4 O23 97.1(2) 1_545 . ?
O13 Eu4 O25 75.4(2) 1_545 . ?
O13 Eu4 O26 87.9(2) 1_545 . ?
O13 Eu4 H26A 73.4 1_545 . ?
O13 Eu4 H26B 102.1 1_545 . ?
O13 Eu4 C16 20.5(2) 1_545 1_545 ?
O17 Eu4 Eu2 81.96(13) 1_545 . ?
O17 Eu4 O25 142.7(2) 1_545 . ?
O17 Eu4 H26A 76.3 1_545 . ?
O17 Eu4 H26B 72.8 1_545 . ?
O17 Eu4 C16 93.5(2) 1_545 1_545 ?
O23 Eu4 Eu2 57.22(14) . . ?
O23 Eu4 O17 138.44(19) . 1_545 ?
O23 Eu4 O25 69.7(2) . . ?
O23 Eu4 O26 136.9(2) . . ?
O23 Eu4 H26A 141.8 . . ?
O23 Eu4 H26B 128.6 . . ?
O23 Eu4 C16 116.1(2) . 1_545 ?
O25 Eu4 Eu2 124.16(14) . . ?
O25 Eu4 H26A 72.1 . . ?
O25 Eu4 H26B 69.9 . . ?
O25 Eu4 C16 90.0(2) . 1_545 ?
O26 Eu4 Eu2 145.77(14) . . ?
O26 Eu4 O17 73.8(2) . 1_545 ?
O26 Eu4 O25 70.4(2) . . ?
O26 Eu4 H26A 15.4 . . ?
O26 Eu4 H26B 15.0 . . ?
O26 Eu4 C16 79.24(19) . 1_545 ?
H26A Eu4 H26B 30.4 . . ?
C16 Eu4 Eu2 126.81(14) 1_545 . ?
C16 Eu4 H26A 63.9 1_545 . ?
C16 Eu4 H26B 94.3 1_545 . ?
C41 O1 Eu1 137.6(5) . . ?
C41 O2 Eu3 149.9(6) . . ?
C48 O3 Eu3 95.0(5) . . ?
C48 O4 Eu3 92.0(4) . . ?
C17 O5 Eu3 116.6(5) . . ?
C17 O6 Eu1 170.4(5) . . ?
C24 O7 Eu2 125.0(5) . 1_565 ?
C24 O8 Eu4 172.2(6) . 1_565 ?
C1 O9 Eu3 152.3(6) . . ?
C1 O10 Eu1 130.1(5) . . ?
C8 O11 Eu4 113.3(5) . . ?
C8 O12 Eu2 157.0(5) . . ?
C16 O13 Eu4 121.1(5) . 1_565 ?
C16 O14 Eu1 161.4(5) . . ?
C9 O15 Eu2 156.3(6) . . ?
C9 O16 Eu3 163.3(5) . . ?
C25 O17 Eu4 156.6(5) . 1_565 ?
C25 O18 Eu1 148.8(6) . . ?
C32 O19 Eu3 99.4(4) . 1_565 ?
C32 O20 Eu3 89.2(5) . 1_565 ?
C33 O21 Eu1 94.8(4) . . ?
C33 O22 Eu1 91.8(5) . . ?
C40 O23 Eu4 141.2(5) . . ?
C40 O24 Eu2 135.5(5) . . ?
C49 O25 Eu4 133.0(7) . . ?
Eu4 O26 H26A 119.3 . . ?
Eu4 O26 H26B 120.8 . . ?
H26A O26 H26B 120.0 . . ?
Eu2 O27 H27A 121.0 . . ?
Eu2 O27 H27B 119.0 . . ?
H27A O27 H27B 120.0 . . ?
Eu2 O28 H28A 120.2 . . ?
Eu2 O28 H28B 119.7 . . ?
H28A O28 H28B 120.0 . . ?
Eu2 O29 H29A 119.3 . . ?
Eu2 O29 H29B 120.7 . . ?
H29A O29 H29B 120.0 . . ?
C49 N1 C51 119.5(9) . . ?
C49 N1 C53 126.6(11) . . ?
C53 N1 C51 113.7(11) . . ?
O9 C1 Eu1 91.7(4) . . ?
O9 C1 O10 123.5(6) . . ?
O9 C1 C2 119.4(7) . . ?
O10 C1 Eu1 32.2(3) . . ?
O10 C1 C2 117.1(7) . . ?
C2 C1 Eu1 148.3(5) . . ?
C3 C2 C1 120.3(6) . . ?
C7 C2 C1 119.1(7) . . ?
C7 C2 C3 120.5(7) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 C2 119.4(7) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 121.8 . . ?
C5 C4 C3 116.4(8) . . ?
C5 C4 H4 121.8 . . ?
C4 C5 H5 116.4 . . ?
C6 C5 C4 127.3(8) . . ?
C6 C5 H5 116.4 . . ?
C5 C6 C7 116.3(7) . . ?
C5 C6 C8 123.1(7) . . ?
C7 C6 C8 120.5(7) . . ?
C2 C7 C6 119.9(8) . . ?
C2 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
O11 C8 C6 115.6(7) . . ?
O12 C8 O11 121.8(7) . . ?
O12 C8 C6 122.6(7) . . ?
O15 C9 C10 118.0(7) . . ?
O16 C9 O15 123.1(7) . . ?
O16 C9 C10 118.9(6) . . ?
C11 C10 C9 120.7(7) . . ?
C15 C10 C9 119.7(7) . . ?
C15 C10 C11 119.6(7) . . ?
C10 C11 H11 120.4 . . ?
C10 C11 C12 119.2(8) . . ?
C12 C11 H11 120.4 . . ?
C11 C12 H12 119.2 . . ?
C13 C12 C11 121.5(9) . . ?
C13 C12 H12 119.2 . . ?
C12 C13 H13 120.1 . . ?
C12 C13 C14 119.9(8) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 C16 122.4(7) . . ?
C15 C14 C13 118.0(7) . . ?
C15 C14 C16 119.5(7) . . ?
C10 C15 C14 121.7(7) . . ?
C10 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
O13 C16 Eu4 38.4(4) . 1_565 ?
O13 C16 C14 117.4(7) . . ?
O14 C16 Eu4 83.9(4) . 1_565 ?
O14 C16 O13 121.8(7) . . ?
O14 C16 C14 120.8(7) . . ?
C14 C16 Eu4 155.1(5) . 1_565 ?
O5 C17 C18 119.4(7) . . ?
O6 C17 O5 122.3(6) . . ?
O6 C17 C18 118.3(6) . . ?
C19 C18 C17 121.0(7) . . ?
C19 C18 C23 117.9(6) . . ?
C23 C18 C17 121.1(6) . . ?
C18 C19 H19 119.0 . . ?
C20 C19 C18 122.0(7) . . ?
C20 C19 H19 119.0 . . ?
C19 C20 H20 120.7 . . ?
C19 C20 C21 118.7(7) . . ?
C21 C20 H20 120.7 . . ?
C20 C21 H21 119.4 . . ?
C22 C21 C20 121.2(6) . . ?
C22 C21 H21 119.4 . . ?
C21 C22 C23 118.7(7) . . ?
C21 C22 C24 121.8(6) . . ?
C23 C22 C24 119.4(6) . . ?
C18 C23 H23 119.2 . . ?
C22 C23 C18 121.5(7) . . ?
C22 C23 H23 119.2 . . ?
O7 C24 Eu2 36.0(3) . 1_565 ?
O7 C24 C22 117.6(7) . . ?
O8 C24 Eu2 90.7(5) . 1_565 ?
O8 C24 O7 124.6(7) . . ?
O8 C24 C22 117.8(6) . . ?
C22 C24 Eu2 148.7(5) . 1_565 ?
O17 C25 C26 119.5(7) . . ?
O18 C25 O17 124.5(7) . . ?
O18 C25 C26 115.9(8) . . ?
C27 C26 C25 122.0(7) . . ?
C27 C26 C31 117.9(7) . . ?
C31 C26 C25 120.0(7) . . ?
C26 C27 H27 118.6 . . ?
C28 C27 C26 122.8(7) . . ?
C28 C27 H27 118.6 . . ?
C27 C28 C29 119.2(7) . . ?
C27 C28 C32 120.9(7) . . ?
C29 C28 C32 119.9(7) . . ?
C28 C29 H29 120.9 . . ?
C30 C29 C28 118.1(8) . . ?
C30 C29 H29 120.9 . . ?
C29 C30 H30 119.3 . . ?
C31 C30 C29 121.4(9) . . ?
C31 C30 H30 119.3 . . ?
C26 C31 H31 120.0 . . ?
C30 C31 C26 119.9(8) . . ?
C30 C31 H31 120.0 . . ?
O19 C32 Eu3 54.4(3) . 1_565 ?
O19 C32 C28 117.1(6) . . ?
O20 C32 Eu3 64.9(4) . 1_565 ?
O20 C32 O19 119.3(7) . . ?
O20 C32 C28 123.6(7) . . ?
C28 C32 Eu3 171.4(5) . 1_565 ?
O21 C33 O22 118.2(7) . . ?
O21 C33 C34 120.6(7) . . ?
O22 C33 C34 121.1(7) . . ?
C35 C34 C33 120.7(6) . . ?
C39 C34 C33 118.9(7) . . ?
C39 C34 C35 120.2(7) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 C34 119.4(7) . . ?
C36 C35 H35 120.3 . . ?
C35 C36 C37 120.6(7) . . ?
C35 C36 C40 118.7(7) . 2_666 ?
C37 C36 C40 120.5(7) . 2_666 ?
C36 C37 H37 120.3 . . ?
C36 C37 C38 119.4(7) . . ?
C38 C37 H37 120.3 . . ?
C37 C38 H38 120.1 . . ?
C39 C38 C37 119.8(7) . . ?
C39 C38 H38 120.1 . . ?
C34 C39 C38 120.4(8) . . ?
C34 C39 H39 119.8 . . ?
C38 C39 H39 119.8 . . ?
O23 C40 Eu2 107.0(5) . . ?
O23 C40 O24 124.8(7) . . ?
O23 C40 C36 119.4(7) . 2_666 ?
O24 C40 Eu2 28.5(3) . . ?
O24 C40 C36 115.7(6) . 2_666 ?
C36 C40 Eu2 127.7(5) 2_666 . ?
O1 C41 C42 117.8(6) . . ?
O2 C41 O1 124.6(7) . . ?
O2 C41 C42 117.6(7) . . ?
C43 C42 C41 121.9(7) . . ?
C47 C42 C41 118.8(6) . . ?
C47 C42 C43 119.3(7) . . ?
C42 C43 H43 120.3 . . ?
C44 C43 C42 119.5(8) . . ?
C44 C43 H43 120.3 . . ?
C43 C44 H44 119.7 . . ?
C45 C44 C43 120.5(8) . . ?
C45 C44 H44 119.7 . . ?
C44 C45 H45 120.0 . . ?
C44 C45 C46 120.1(8) . . ?
C46 C45 H45 120.0 . . ?
C45 C46 C48 120.4(7) . 2_765 ?
C47 C46 C45 120.1(7) . . ?
C47 C46 C48 119.5(7) . 2_765 ?
C42 C47 H47 119.8 . . ?
C46 C47 C42 120.5(7) . . ?
C46 C47 H47 119.8 . . ?
O3 C48 O4 119.3(7) . . ?
O3 C48 C46 119.4(7) . 2_765 ?
O4 C48 C46 121.2(7) . 2_765 ?
O25 C49 H49 114.8 . . ?
N1 C49 O25 130.4(11) . . ?
N1 C49 H49 114.8 . . ?
N1 C51 H51A 109.5 . . ?
N1 C51 H51B 109.5 . . ?
N1 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N1 C53 H53A 109.5 . . ?
N1 C53 H53B 109.5 . . ?
N1 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C56 N2 C58 126.0(13) . . ?
C57 N2 C56 115.2(15) . . ?
C57 N2 C58 118.8(13) . . ?
O30 C56 N2 123.9(16) . . ?
O30 C56 H56 118.0 . . ?
N2 C56 H56 118.0 . . ?
N2 C57 H57A 109.5 . . ?
N2 C57 H57B 109.5 . . ?
N2 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
N2 C58 H58A 109.5 . . ?
N2 C58 H58B 109.5 . . ?
N2 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
H31A O31 H31B 120.0 . . ?
H1AA O1A H1AB 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Eu1 O1 C41 O2 -49.3(11) . . . . ?
Eu1 O1 C41 C42 129.3(6) . . . . ?
Eu1 O10 C1 O9 9.9(11) . . . . ?
Eu1 O10 C1 C2 -169.0(5) . . . . ?
Eu1 O14 C16 Eu4 -179.8(16) . . . 1_565 ?
Eu1 O14 C16 O13 173.8(12) . . . . ?
Eu1 O14 C16 C14 -4(2) . . . . ?
Eu1 O18 C25 O17 -28.0(15) . . . . ?
Eu1 O18 C25 C26 152.4(8) . . . . ?
Eu1 O21 C33 O22 -7.5(8) . . . . ?
Eu1 O21 C33 C34 169.9(6) . . . . ?
Eu1 O22 C33 O21 7.4(8) . . . . ?
Eu1 O22 C33 C34 -170.0(6) . . . . ?
Eu1 C1 C2 C3 -31.1(13) . . . . ?
Eu1 C1 C2 C7 146.6(7) . . . . ?
Eu2 O7 C24 O8 23.0(11) 1_565 . . . ?
Eu2 O7 C24 C22 -156.9(5) 1_565 . . . ?
Eu2 O12 C8 O11 112.8(12) . . . . ?
Eu2 O12 C8 C6 -66.6(16) . . . . ?
Eu2 O15 C9 O16 -4.0(18) . . . . ?
Eu2 O15 C9 C10 176.0(9) . . . . ?
Eu2 O24 C40 O23 -57.5(11) . . . . ?
Eu2 O24 C40 C36 122.5(7) . . . 2_666 ?
Eu3 O2 C41 O1 38.5(14) . . . . ?
Eu3 O2 C41 C42 -140.1(8) . . . . ?
Eu3 O3 C48 O4 0.3(7) . . . . ?
Eu3 O3 C48 C46 178.5(5) . . . 2_765 ?
Eu3 O4 C48 O3 -0.3(7) . . . . ?
Eu3 O4 C48 C46 -178.5(6) . . . 2_765 ?
Eu3 O5 C17 O6 9.8(10) . . . . ?
Eu3 O5 C17 C18 -170.1(5) . . . . ?
Eu3 O9 C1 Eu1 -78.1(10) . . . . ?
Eu3 O9 C1 O10 -83.3(13) . . . . ?
Eu3 O9 C1 C2 95.6(11) . . . . ?
Eu3 O16 C9 O15 -67(2) . . . . ?
Eu3 O16 C9 C10 113.0(17) . . . . ?
Eu3 O19 C32 O20 -1.0(8) 1_565 . . . ?
Eu3 O19 C32 C28 -179.2(5) 1_565 . . . ?
Eu3 O20 C32 O19 0.9(7) 1_565 . . . ?
Eu3 O20 C32 C28 179.0(7) 1_565 . . . ?
Eu4 O11 C8 O12 4.4(9) . . . . ?
Eu4 O11 C8 C6 -176.1(5) . . . . ?
Eu4 O13 C16 O14 10.0(11) 1_565 . . . ?
Eu4 O13 C16 C14 -172.3(5) 1_565 . . . ?
Eu4 O17 C25 O18 -8.5(19) 1_565 . . . ?
Eu4 O17 C25 C26 171.1(9) 1_565 . . . ?
Eu4 O23 C40 Eu2 37.8(9) . . . . ?
Eu4 O23 C40 O24 62.7(11) . . . . ?
Eu4 O23 C40 C36 -117.3(8) . . . 2_666 ?
Eu4 O25 C49 N1 -162.6(10) . . . . ?
O1 C41 C42 C43 16.6(11) . . . . ?
O1 C41 C42 C47 -161.5(7) . . . . ?
O2 C41 C42 C43 -164.7(7) . . . . ?
O2 C41 C42 C47 17.2(10) . . . . ?
O5 C17 C18 C19 -6.7(11) . . . . ?
O5 C17 C18 C23 171.8(7) . . . . ?
O6 C17 C18 C19 173.5(7) . . . . ?
O6 C17 C18 C23 -8.1(11) . . . . ?
O9 C1 C2 C3 161.0(8) . . . . ?
O9 C1 C2 C7 -21.3(11) . . . . ?
O10 C1 C2 C3 -20.0(11) . . . . ?
O10 C1 C2 C7 157.7(7) . . . . ?
O15 C9 C10 C11 -4.9(11) . . . . ?
O15 C9 C10 C15 175.2(7) . . . . ?
O16 C9 C10 C11 175.1(7) . . . . ?
O16 C9 C10 C15 -4.8(11) . . . . ?
O17 C25 C26 C27 -16.4(11) . . . . ?
O17 C25 C26 C31 164.5(8) . . . . ?
O18 C25 C26 C27 163.2(7) . . . . ?
O18 C25 C26 C31 -15.9(11) . . . . ?
O21 C33 C34 C35 170.3(7) . . . . ?
O21 C33 C34 C39 -13.0(12) . . . . ?
O22 C33 C34 C35 -12.4(12) . . . . ?
O22 C33 C34 C39 164.3(8) . . . . ?
C1 C2 C3 C4 177.3(8) . . . . ?
C1 C2 C7 C6 -176.1(7) . . . . ?
C2 C3 C4 C5 -2.9(14) . . . . ?
C3 C2 C7 C6 1.6(12) . . . . ?
C3 C4 C5 C6 5.5(17) . . . . ?
C4 C5 C6 C7 -4.3(15) . . . . ?
C4 C5 C6 C8 174.5(9) . . . . ?
C5 C6 C7 C2 0.4(12) . . . . ?
C5 C6 C8 O11 -24.0(12) . . . . ?
C5 C6 C8 O12 155.4(8) . . . . ?
C7 C2 C3 C4 -0.3(13) . . . . ?
C7 C6 C8 O11 154.7(7) . . . . ?
C7 C6 C8 O12 -25.9(12) . . . . ?
C8 C6 C7 C2 -178.4(7) . . . . ?
C9 C10 C11 C12 -178.8(8) . . . . ?
C9 C10 C15 C14 177.3(7) . . . . ?
C10 C11 C12 C13 0.9(16) . . . . ?
C11 C10 C15 C14 -2.6(12) . . . . ?
C11 C12 C13 C14 -1.3(16) . . . . ?
C12 C13 C14 C15 -0.2(13) . . . . ?
C12 C13 C14 C16 -176.4(9) . . . . ?
C13 C14 C15 C10 2.2(12) . . . . ?
C13 C14 C16 Eu4 -33.2(17) . . . 1_565 ?
C13 C14 C16 O13 -21.9(12) . . . . ?
C13 C14 C16 O14 155.8(8) . . . . ?
C15 C10 C11 C12 1.0(13) . . . . ?
C15 C14 C16 Eu4 150.7(10) . . . 1_565 ?
C15 C14 C16 O13 162.0(7) . . . . ?
C15 C14 C16 O14 -20.3(12) . . . . ?
C16 C14 C15 C10 178.4(7) . . . . ?
C17 C18 C19 C20 -179.5(8) . . . . ?
C17 C18 C23 C22 -179.2(7) . . . . ?
C18 C19 C20 C21 -1.7(13) . . . . ?
C19 C18 C23 C22 -0.6(11) . . . . ?
C19 C20 C21 C22 0.2(13) . . . . ?
C20 C21 C22 C23 1.1(12) . . . . ?
C20 C21 C22 C24 178.8(8) . . . . ?
C21 C22 C23 C18 -0.9(11) . . . . ?
C21 C22 C24 Eu2 -40.8(13) . . . 1_565 ?
C21 C22 C24 O7 -14.5(11) . . . . ?
C21 C22 C24 O8 165.6(8) . . . . ?
C23 C18 C19 C20 2.0(12) . . . . ?
C23 C22 C24 Eu2 136.9(8) . . . 1_565 ?
C23 C22 C24 O7 163.2(7) . . . . ?
C23 C22 C24 O8 -16.7(11) . . . . ?
C24 C22 C23 C18 -178.6(7) . . . . ?
C25 C26 C27 C28 -171.6(7) . . . . ?
C25 C26 C31 C30 178.5(9) . . . . ?
C26 C27 C28 C29 -9.7(11) . . . . ?
C26 C27 C28 C32 171.9(7) . . . . ?
C27 C26 C31 C30 -0.6(14) . . . . ?
C27 C28 C29 C30 4.9(13) . . . . ?
C27 C28 C32 O19 -15.7(11) . . . . ?
C27 C28 C32 O20 166.2(7) . . . . ?
C28 C29 C30 C31 1.6(16) . . . . ?
C29 C28 C32 O19 165.9(8) . . . . ?
C29 C28 C32 O20 -12.2(12) . . . . ?
C29 C30 C31 C26 -3.8(17) . . . . ?
C31 C26 C27 C28 7.5(11) . . . . ?
C32 C28 C29 C30 -176.7(8) . . . . ?
C33 C34 C35 C36 174.8(7) . . . . ?
C33 C34 C39 C38 -172.9(8) . . . . ?
C34 C35 C36 C37 -3.0(12) . . . . ?
C34 C35 C36 C40 -177.3(7) . . . 2_666 ?
C35 C34 C39 C38 3.8(13) . . . . ?
C35 C36 C37 C38 5.7(13) . . . . ?
C36 C37 C38 C39 -3.7(14) . . . . ?
C37 C38 C39 C34 -1.0(14) . . . . ?
C39 C34 C35 C36 -1.8(12) . . . . ?
C40 C36 C37 C38 180.0(8) 2_666 . . . ?
C41 C42 C43 C44 -178.7(8) . . . . ?
C41 C42 C47 C46 177.3(7) . . . . ?
C42 C43 C44 C45 1.6(15) . . . . ?
C43 C42 C47 C46 -0.8(11) . . . . ?
C43 C44 C45 C46 -1.1(15) . . . . ?
C44 C45 C46 C47 -0.4(14) . . . . ?
C44 C45 C46 C48 -179.0(8) . . . 2_765 ?
C45 C46 C47 C42 1.4(12) . . . . ?
C47 C42 C43 C44 -0.7(13) . . . . ?
C48 C46 C47 C42 180.0(7) 2_765 . . . ?
C51 N1 C49 O25 -3.3(19) . . . . ?
C53 N1 C49 O25 -179.3(11) . . . . ?
C57 N2 C56 O30 174.8(15) . . . . ?
C58 N2 C56 O30 -7(2) . . . . ?

_shelx_SHELXL_version_number     2016/6

_olex2_submission_special_instructions 'No special instructions were received'
