# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_eu
_database_code_depnum_ccdc_archive 'CCDC 1558322'
_audit_update_record             
;
2017-09-03 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'[Eu (H2 O)4 (C16 H6 N2 O9)], (C10 H9 N2), (H2 O)'
_chemical_formula_sum            'C26 H25 Eu N4 O14'
_chemical_formula_weight         769.46

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'
Eu Eu -0.1578 3.6682 '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_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8823(12)
_cell_length_b                   11.4591(12)
_cell_length_c                   14.1152(15)
_cell_angle_alpha                102.027(2)
_cell_angle_beta                 110.939(2)
_cell_angle_gamma                113.321(2)
_cell_volume                     1378.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1857
_cell_measurement_theta_min      2.3376
_cell_measurement_theta_max      21.8113

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_F_000             768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    2.358
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.754504
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8558
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.105
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             6140
_reflns_number_gt                4836

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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
 H1WB-O1W
 0.84 with sigma of 0.02
 O1W-H1WB
 0.83 with sigma of 0.02
 H1WA-O1W
 0.83 with sigma of 0.02
3.a Free rotating group:
 O5W(H5WA,H5WB)
3.b Rotating group:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0388P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6140
_refine_ls_number_parameters     443
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0839
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_restrained_S_all      0.960
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.14996(3) 0.70096(3) 0.50709(2) 0.02280(9) Uani 1 1 d D . . . .
O1 O 0.0374(4) 0.4411(3) 0.4323(3) 0.0298(8) Uani 1 1 d . . . . .
O2 O 0.0354(4) 0.2584(4) 0.4565(3) 0.0347(9) Uani 1 1 d . . . . .
O3 O 0.1793(4) 0.6358(3) 0.3500(3) 0.0312(9) Uani 1 1 d . . . . .
O4 O -0.0012(5) 0.4423(4) 0.2001(3) 0.0541(13) Uani 1 1 d . . . . .
O5 O 0.4818(5) 0.8780(4) 0.3667(3) 0.0365(9) Uani 1 1 d . . . . .
O6 O 0.6782(5) 0.8471(4) 0.3958(3) 0.0426(10) Uani 1 1 d . . . . .
O7 O 0.7050(4) 1.0971(4) 0.3268(3) 0.0329(9) Uani 1 1 d . . . . .
O8 O 0.5500(5) 1.1134(4) 0.1845(3) 0.0503(12) Uani 1 1 d . . . . .
O9 O 0.4770(9) 0.4801(7) 0.1668(6) 0.066(2) Uani 0.730(7) 1 d D U P A 1
O9' O 0.2213(17) 0.5241(17) 0.1558(12) 0.066(2) Uani 0.270(7) 1 d D . P A 2
O1W O 0.1396(5) 0.8799(4) 0.4446(3) 0.0344(9) Uani 1 1 d D . . . .
H11 H 0.196(4) 0.9617(19) 0.494(3) 0.052 Uiso 1 1 d D U . . .
H12 H 0.0505(18) 0.866(3) 0.409(4) 0.052 Uiso 1 1 d D U . . .
O2W O 0.2979(5) 0.6485(4) 0.6433(3) 0.0351(9) Uani 1 1 d D . . . .
H21 H 0.359(5) 0.721(2) 0.7026(17) 0.053 Uiso 1 1 d D U . . .
H22 H 0.238(3) 0.587(4) 0.655(3) 0.053 Uiso 1 1 d D U . . .
O3W O 0.4108(5) 0.8457(4) 0.5388(3) 0.0335(9) Uani 1 1 d D . . . .
H31 H 0.416(5) 0.836(4) 0.4804(19) 0.050 Uiso 1 1 d D U . . .
H32 H 0.451(5) 0.9305(14) 0.577(3) 0.050 Uiso 1 1 d D U . . .
O4W O -0.1108(5) 0.5750(4) 0.3294(3) 0.0360(9) Uani 1 1 d D . . . .
H41 H -0.104(5) 0.537(5) 0.2757(19) 0.043 Uiso 1 1 d D U . . .
H42 H -0.136(5) 0.633(3) 0.318(3) 0.054 Uiso 1 1 d D U . . .
O5W O -0.1586(5) 0.7829(5) 0.3111(3) 0.0423(10) Uani 1 1 d D . . . .
H51 H -0.216(6) 0.803(6) 0.329(3) 0.063 Uiso 1 1 d D U . . .
H52 H -0.154(5) 0.807(6) 0.260(3) 0.063 Uiso 1 1 d D U . . .
N1 N 0.4309(6) 0.5612(5) 0.1927(4) 0.0436(13) Uani 1 1 d D . . . .
N2 N 0.3460(7) 0.5443(6) 0.2328(5) 0.0509(14) Uani 1 1 d D . . . .
N3 N -0.1612(6) 0.8880(5) 0.1504(4) 0.0450(13) Uani 1 1 d . . . . .
N4 N -0.1586(6) 1.2136(5) -0.2179(4) 0.0428(13) Uani 1 1 d D . . . .
H4 H -0.153(7) 1.257(5) -0.262(4) 0.051 Uiso 1 1 d D U . . .
C1 C 0.0839(6) 0.3555(5) 0.4280(4) 0.0270(12) Uani 1 1 d . . . . .
C2 C 0.1972(6) 0.3708(5) 0.3890(4) 0.0256(11) Uani 1 1 d . . . . .
C3 C 0.2878(6) 0.3127(5) 0.4222(4) 0.0308(12) Uani 1 1 d . . . . .
H3 H 0.2738 0.2625 0.4652 0.037 Uiso 1 1 calc R U . . .
C4 C 0.3992(7) 0.3304(6) 0.3906(5) 0.0376(14) Uani 1 1 d . . . . .
H4A H 0.4602 0.2925 0.4133 0.045 Uiso 1 1 calc R U . . .
C5 C 0.4197(7) 0.4033(6) 0.3263(5) 0.0390(14) Uani 1 1 d . . . . .
H5 H 0.4948 0.4154 0.3059 0.047 Uiso 1 1 calc R U . . .
C6 C 0.3278(7) 0.4587(6) 0.2919(4) 0.0335(13) Uani 1 1 d . . . . .
C7 C 0.2165(6) 0.4444(5) 0.3238(4) 0.0272(12) Uani 1 1 d . . . . .
C8 C 0.1214(7) 0.5094(6) 0.2863(4) 0.0288(12) Uani 1 1 d . . . . .
C9 C 0.4480(7) 0.6615(6) 0.1436(5) 0.0370(14) Uani 1 1 d . . . . .
C10 C 0.4041(8) 0.6168(6) 0.0322(5) 0.0482(17) Uani 1 1 d . . . . .
H10 H 0.3682 0.5247 -0.0099 0.058 Uiso 1 1 calc R U . . .
C11 C 0.4140(8) 0.7098(6) -0.0155(5) 0.0490(17) Uani 1 1 d . . . . .
H11A H 0.3814 0.6808 -0.0912 0.059 Uiso 1 1 calc R U . . .
C12 C 0.4722(7) 0.8459(6) 0.0484(4) 0.0428(16) Uani 1 1 d . . . . .
H12A H 0.4783 0.9084 0.0150 0.051 Uiso 1 1 calc R U . . .
C13 C 0.5226(6) 0.8936(5) 0.1616(4) 0.0305(12) Uani 1 1 d . . . . .
C14 C 0.5084(7) 0.7984(6) 0.2111(4) 0.0333(13) Uani 1 1 d . . . . .
C15 C 0.5609(7) 0.8455(5) 0.3356(4) 0.0317(13) Uani 1 1 d . . . . .
C16 C 0.5984(7) 1.0471(6) 0.2293(4) 0.0319(13) Uani 1 1 d . . . . .
C17 C -0.2122(9) 0.8191(7) 0.0441(5) 0.0557(19) Uani 1 1 d . . . . .
H17 H -0.2477 0.7243 0.0184 0.067 Uiso 1 1 calc R U . . .
C18 C -0.2159(8) 0.8790(6) -0.0304(5) 0.0516(18) Uani 1 1 d . . . . .
H18 H -0.2527 0.8253 -0.1042 0.062 Uiso 1 1 calc R U . . .
C19 C -0.1651(7) 1.0190(6) 0.0041(4) 0.0321(13) Uani 1 1 d . . . . .
C20 C -0.1156(8) 1.0893(6) 0.1137(5) 0.0454(16) Uani 1 1 d . . . . .
H20 H -0.0816 1.1838 0.1414 0.054 Uiso 1 1 calc R U . . .
C21 C -0.1161(8) 1.0212(7) 0.1830(5) 0.0515(18) Uani 1 1 d . . . . .
H21A H -0.0827 1.0717 0.2568 0.062 Uiso 1 1 calc R U . . .
C22 C -0.2125(8) 1.0818(7) -0.2541(5) 0.0498(17) Uani 1 1 d . . . . .
H22A H -0.2480 1.0311 -0.3284 0.060 Uiso 1 1 calc R U . . .
C23 C -0.2182(8) 1.0152(6) -0.1842(5) 0.0458(16) Uani 1 1 d . . . . .
H23 H -0.2592 0.9194 -0.2119 0.055 Uiso 1 1 calc R U . . .
C24 C -0.1643(7) 1.0878(6) -0.0746(4) 0.0345(13) Uani 1 1 d . . . . .
C25 C -0.1081(9) 1.2293(7) -0.0397(5) 0.061(2) Uani 1 1 d . . . . .
H25 H -0.0718 1.2834 0.0339 0.073 Uiso 1 1 calc R U . . .
C26 C -0.1058(10) 1.2892(7) -0.1135(6) 0.066(2) Uani 1 1 d . . . . .
H26 H -0.0665 1.3846 -0.0896 0.079 Uiso 1 1 calc R U . . .


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 O7 2.355(3) 2_676 ?
Eu1 O3 2.363(3) . ?
Eu1 O2W 2.384(4) . ?
Eu1 O1W 2.421(3) . ?
Eu1 O2 2.437(4) 2_566 ?
Eu1 O3W 2.462(4) . ?
Eu1 O1 2.521(3) . ?
Eu1 O4W 2.567(4) . ?
Eu1 O1 2.596(4) 2_566 ?
Eu1 Eu1 4.3763(7) 2_566 ?
O1 C1 1.270(5) . ?
O1 Eu1 2.596(4) 2_566 ?
O2 C1 1.246(6) . ?
O2 Eu1 2.437(4) 2_566 ?
O3 C8 1.278(6) . ?
O4 C8 1.220(6) . ?
O5 C15 1.237(6) . ?
O6 C15 1.246(7) . ?
O7 C16 1.254(6) . ?
O7 Eu1 2.355(3) 2_676 ?
O8 C16 1.239(6) . ?
O9 N1 1.269(7) . ?
O9' N2 1.292(11) . ?
N1 N2 1.220(7) . ?
N1 C9 1.446(7) . ?
N2 C6 1.415(7) . ?
N3 C21 1.317(7) . ?
N3 C17 1.321(8) . ?
N4 C22 1.284(7) . ?
N4 C26 1.312(8) . ?
C1 C2 1.486(7) . ?
C1 Eu1 2.889(5) 2_566 ?
C2 C7 1.387(7) . ?
C2 C3 1.398(7) . ?
C3 C4 1.393(8) . ?
C4 C5 1.373(7) . ?
C5 C6 1.387(7) . ?
C6 C7 1.400(7) . ?
C7 C8 1.513(7) . ?
C9 C10 1.378(8) . ?
C9 C14 1.383(7) . ?
C10 C11 1.364(8) . ?
C11 C12 1.368(7) . ?
C12 C13 1.387(7) . ?
C13 C14 1.402(7) . ?
C13 C16 1.508(7) . ?
C14 C15 1.532(7) . ?
C17 C18 1.368(8) . ?
C18 C19 1.377(7) . ?
C19 C20 1.370(7) . ?
C19 C24 1.490(7) . ?
C20 C21 1.373(8) . ?
C22 C23 1.371(8) . ?
C23 C24 1.363(7) . ?
C24 C25 1.383(8) . ?
C25 C26 1.364(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
O7 Eu1 O3 133.54(13) 2_676 . ?
O7 Eu1 O2W 74.60(12) 2_676 . ?
O3 Eu1 O2W 107.24(12) . . ?
O7 Eu1 O1W 76.44(12) 2_676 . ?
O3 Eu1 O1W 80.78(12) . . ?
O2W Eu1 O1W 146.09(13) . . ?
O7 Eu1 O2 73.99(13) 2_676 2_566 ?
O3 Eu1 O2 136.15(13) . 2_566 ?
O2W Eu1 O2 113.83(13) . 2_566 ?
O1W Eu1 O2 73.89(12) . 2_566 ?
O7 Eu1 O3W 69.05(13) 2_676 . ?
O3 Eu1 O3W 66.30(12) . . ?
O2W Eu1 O3W 77.85(13) . . ?
O1W Eu1 O3W 75.59(13) . . ?
O2 Eu1 O3W 136.36(12) 2_566 . ?
O7 Eu1 O1 142.81(11) 2_676 . ?
O3 Eu1 O1 72.43(11) . . ?
O2W Eu1 O1 71.54(12) . . ?
O1W Eu1 O1 140.34(12) . . ?
O2 Eu1 O1 106.32(12) 2_566 . ?
O3W Eu1 O1 117.10(12) . . ?
O7 Eu1 O4W 137.98(12) 2_676 . ?
O3 Eu1 O4W 70.18(13) . . ?
O2W Eu1 O4W 139.04(12) . . ?
O1W Eu1 O4W 74.87(12) . . ?
O2 Eu1 O4W 68.97(13) 2_566 . ?
O3W Eu1 O4W 130.29(12) . . ?
O1 Eu1 O4W 68.87(11) . . ?
O7 Eu1 O1 94.55(12) 2_676 2_566 ?
O3 Eu1 O1 131.47(11) . 2_566 ?
O2W Eu1 O1 75.39(12) . 2_566 ?
O1W Eu1 O1 124.44(12) . 2_566 ?
O2 Eu1 O1 51.31(11) 2_566 2_566 ?
O3W Eu1 O1 151.59(12) . 2_566 ?
O1 Eu1 O1 62.46(13) . 2_566 ?
O4W Eu1 O1 77.49(12) . 2_566 ?
O7 Eu1 Eu1 120.40(9) 2_676 2_566 ?
O3 Eu1 Eu1 102.65(8) . 2_566 ?
O2W Eu1 Eu1 70.60(9) . 2_566 ?
O1W Eu1 Eu1 141.18(10) . 2_566 ?
O2 Eu1 Eu1 77.94(8) 2_566 2_566 ?
O3W Eu1 Eu1 141.65(8) . 2_566 ?
O1 Eu1 Eu1 31.74(8) . 2_566 ?
O4W Eu1 Eu1 70.35(8) . 2_566 ?
O1 Eu1 Eu1 30.72(7) 2_566 2_566 ?
C1 O1 Eu1 138.5(3) . . ?
C1 O1 Eu1 90.0(3) . 2_566 ?
Eu1 O1 Eu1 117.54(13) . 2_566 ?
C1 O2 Eu1 98.1(3) . 2_566 ?
C8 O3 Eu1 123.5(3) . . ?
C16 O7 Eu1 140.3(3) . 2_676 ?
N2 N1 O9 126.4(5) . . ?
N2 N1 C9 116.4(5) . . ?
O9 N1 C9 115.2(5) . . ?
N1 N2 O9' 104.5(9) . . ?
N1 N2 C6 122.9(5) . . ?
O9' N2 C6 116.3(9) . . ?
C21 N3 C17 116.3(5) . . ?
C22 N4 C26 121.7(5) . . ?
O2 C1 O1 120.4(5) . . ?
O2 C1 C2 119.4(4) . . ?
O1 C1 C2 120.1(4) . . ?
O2 C1 Eu1 56.6(3) . 2_566 ?
O1 C1 Eu1 64.0(3) . 2_566 ?
C2 C1 Eu1 174.8(3) . 2_566 ?
C7 C2 C3 120.4(5) . . ?
C7 C2 C1 121.1(4) . . ?
C3 C2 C1 118.5(4) . . ?
C4 C3 C2 119.7(5) . . ?
C5 C4 C3 120.5(5) . . ?
C4 C5 C6 119.6(5) . . ?
C5 C6 C7 121.1(5) . . ?
C5 C6 N2 124.6(5) . . ?
C7 C6 N2 114.0(5) . . ?
C2 C7 C6 118.7(5) . . ?
C2 C7 C8 122.2(5) . . ?
C6 C7 C8 119.2(4) . . ?
O4 C8 O3 124.3(5) . . ?
O4 C8 C7 120.3(5) . . ?
O3 C8 C7 115.4(5) . . ?
C10 C9 C14 123.0(5) . . ?
C10 C9 N1 118.7(5) . . ?
C14 C9 N1 118.3(5) . . ?
C11 C10 C9 118.9(5) . . ?
C10 C11 C12 119.7(5) . . ?
C11 C12 C13 122.0(5) . . ?
C12 C13 C14 118.9(5) . . ?
C12 C13 C16 119.4(5) . . ?
C14 C13 C16 121.6(5) . . ?
C9 C14 C13 117.3(5) . . ?
C9 C14 C15 121.7(5) . . ?
C13 C14 C15 121.0(5) . . ?
O6 C15 O5 126.1(5) . . ?
O6 C15 C14 117.4(5) . . ?
O5 C15 C14 116.5(5) . . ?
O8 C16 O7 125.3(5) . . ?
O8 C16 C13 117.5(5) . . ?
O7 C16 C13 117.2(5) . . ?
N3 C17 C18 123.9(6) . . ?
C17 C18 C19 119.9(6) . . ?
C20 C19 C18 116.0(5) . . ?
C20 C19 C24 122.9(5) . . ?
C18 C19 C24 121.1(5) . . ?
C19 C20 C21 120.4(5) . . ?
N3 C21 C20 123.4(6) . . ?
N4 C22 C23 120.6(6) . . ?
C24 C23 C22 120.7(6) . . ?
C23 C24 C25 116.5(5) . . ?
C23 C24 C19 122.0(5) . . ?
C25 C24 C19 121.4(5) . . ?
C26 C25 C24 119.8(6) . . ?
N4 C26 C25 120.6(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11 O6 0.842(10) 1.943(11) 2.784(5) 178(3) 2_676
O1W H12 O5W 0.846(10) 1.866(14) 2.687(6) 163(3) .
O2W H21 O8 0.842(10) 1.799(17) 2.622(5) 165(5) 2_676
O2W H22 O4W 0.840(10) 1.942(13) 2.774(5) 171(5) 2_566
O3W H31 O5 0.836(10) 2.045(15) 2.851(5) 162(3) .
O3W H32 O5 0.840(10) 1.889(17) 2.714(5) 167(5) 2_676
O4W H41 O4 0.838(10) 2.209(18) 2.984(6) 154(3) .
O4W H42 O5W 0.839(10) 1.843(13) 2.675(5) 170(4) .
O5W H51 O6 0.843(10) 1.871(12) 2.703(6) 169(2) 1_455
O5W H52 N3 0.837(10) 1.954(14) 2.778(6) 167(3) .
N4 H4 O3 0.879(10) 1.95(2) 2.803(5) 164(6) 2_575

_refine_diff_density_max         1.181
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.144

_shelxl_version_number           2014/6

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

data_dy
_database_code_depnum_ccdc_archive 'CCDC 1558325'
_audit_update_record             
;
2017-09-03 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;

_vrf_PLAT029_dy                  
;
PROBLEM:  _diffrn_measured_fraction_theta_full Low .......      0.950 Note 
RESPONSE: The fraction is 100% full at a 2\q~max~ of 50 \%.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C10 H9 N2), [Dy (H2 O)4 (C16 H6 N2 O9), (H2 O)'
_chemical_formula_sum            'C26 H25 Dy N4 O14'
_chemical_formula_weight         780.00

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   10.8893(6)
_cell_length_b                   11.4543(7)
_cell_length_c                   14.1156(8)
_cell_angle_alpha                101.7907(10)
_cell_angle_beta                 110.9658(9)
_cell_angle_gamma                113.3613(8)
_cell_volume                     1380.72(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5009
_cell_measurement_theta_min      2.3346
_cell_measurement_theta_max      28.3854

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             774
_exptl_absorpt_coefficient_mu    2.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_T_max  0.640
_exptl_absorpt_process_details   SADABS

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8234
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6336
_reflns_number_gt                5332
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0823P)²+0.5197P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6022
_refine_ls_number_parameters     449
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.1240
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.15012(3) 0.70101(2) 0.507174(19) 0.02310(10) Uani 1 1 d . . .
O1 O 0.1794(4) 0.6348(4) 0.3481(3) 0.0249(7) Uani 1 1 d . . .
O2 O -0.0017(6) 0.4413(5) 0.2010(4) 0.0501(13) Uani 1 1 d . . .
O3 O 0.0391(4) 0.4412(4) 0.4324(3) 0.0236(7) Uani 1 1 d . . .
O4 O 0.0373(5) 0.2579(4) 0.4563(4) 0.0327(9) Uani 1 1 d . . .
O5 O 0.4824(5) 0.8777(4) 0.3672(4) 0.0331(9) Uani 1 1 d . A .
O6 O 0.6793(5) 0.8479(5) 0.3968(4) 0.0371(10) Uani 1 1 d . A .
O7 O 0.7048(4) 1.0962(4) 0.3256(3) 0.0262(8) Uani 1 1 d . . .
O8 O 0.5503(6) 1.1119(5) 0.1829(4) 0.0480(12) Uani 1 1 d . . .
O9 O 0.4790(10) 0.4821(7) 0.1691(7) 0.052(2) Uani 0.690(13) 1 d PU A 1
O9' O 0.212(2) 0.512(2) 0.1450(17) 0.065(6) Uani 0.310(13) 1 d PU A 2
O1w O 0.1387(4) 0.8824(4) 0.4444(3) 0.0266(8) Uani 1 1 d D . .
H11 H 0.184(6) 0.963(3) 0.492(4) 0.040 Uiso 1 1 d D . .
H12 H 0.051(3) 0.861(5) 0.399(4) 0.040 Uiso 1 1 d D . .
O2w O 0.4117(4) 0.8467(4) 0.5382(3) 0.0254(7) Uani 1 1 d D . .
H21 H 0.421(8) 0.834(5) 0.481(3) 0.038 Uiso 1 1 d D . .
H22 H 0.449(7) 0.9313(18) 0.573(4) 0.038 Uiso 1 1 d D . .
O3w O 0.2987(4) 0.6490(4) 0.6458(3) 0.0298(8) Uani 1 1 d D . .
H31 H 0.342(7) 0.723(3) 0.702(3) 0.045 Uiso 1 1 d D . .
H32 H 0.248(7) 0.581(4) 0.657(5) 0.045 Uiso 1 1 d D . .
O4w O -0.1119(4) 0.5749(4) 0.3276(3) 0.0296(8) Uani 1 1 d D . .
H41 H -0.082(8) 0.560(7) 0.282(5) 0.044 Uiso 1 1 d D . .
H42 H -0.126(8) 0.642(5) 0.329(5) 0.044 Uiso 1 1 d D . .
O5w O -0.1583(5) 0.7832(5) 0.3101(4) 0.0368(10) Uani 1 1 d D . .
H51 H -0.186(9) 0.818(7) 0.350(5) 0.055 Uiso 1 1 d D . .
H52 H -0.159(9) 0.816(7) 0.262(5) 0.055 Uiso 1 1 d D . .
N1 N 0.3444(7) 0.5422(6) 0.2303(5) 0.0449(14) Uani 1 1 d . . .
N2 N 0.4305(7) 0.5595(5) 0.1936(5) 0.0411(13) Uani 1 1 d . A .
N3 N 0.1583(6) 0.7835(6) 0.2164(5) 0.0404(12) Uani 1 1 d D . .
H3 H 0.171(8) 0.755(7) 0.270(4) 0.049 Uiso 1 1 d D . .
N4 N 0.1624(6) 1.1141(5) -0.1491(4) 0.0366(11) Uani 1 1 d . . .
C1 C 0.1211(6) 0.5089(5) 0.2867(4) 0.0249(11) Uani 1 1 d . A .
C2 C 0.2169(6) 0.4439(5) 0.3234(4) 0.0231(10) Uani 1 1 d . . .
C3 C 0.1988(6) 0.3710(5) 0.3892(4) 0.0225(10) Uani 1 1 d . A .
C4 C 0.2894(6) 0.3133(5) 0.4227(5) 0.0251(11) Uani 1 1 d . . .
H4 H 0.2758 0.2637 0.4663 0.030 Uiso 1 1 calc R A .
C5 C 0.3993(6) 0.3301(6) 0.3909(5) 0.0306(12) Uani 1 1 d . A .
H5 H 0.4600 0.2919 0.4135 0.037 Uiso 1 1 calc R . .
C6 C 0.4193(7) 0.4027(6) 0.3263(5) 0.0323(12) Uani 1 1 d . . .
H6 H 0.4940 0.4142 0.3055 0.039 Uiso 1 1 calc R A .
C7 C 0.3285(7) 0.4589(6) 0.2918(5) 0.0288(11) Uani 1 1 d . A .
C8 C 0.0859(6) 0.3554(5) 0.4284(4) 0.0227(10) Uani 1 1 d . . .
C9 C 0.4484(7) 0.6624(6) 0.1449(5) 0.0333(12) Uani 1 1 d . . .
C10 C 0.4047(9) 0.6160(7) 0.0340(6) 0.0447(16) Uani 1 1 d . A .
H10 H 0.3695 0.5241 -0.0072 0.054 Uiso 1 1 calc R . .
C11 C 0.4146(8) 0.7096(7) -0.0138(6) 0.0487(17) Uani 1 1 d . . .
H11A H 0.3816 0.6803 -0.0895 0.058 Uiso 1 1 calc R A .
C12 C 0.4722(7) 0.8451(6) 0.0483(5) 0.0375(14) Uani 1 1 d . A .
H12A H 0.4775 0.9069 0.0141 0.045 Uiso 1 1 calc R . .
C13 C 0.5237(6) 0.8937(5) 0.1624(5) 0.0272(11) Uani 1 1 d . . .
C14 C 0.5108(6) 0.7999(5) 0.2120(5) 0.0255(10) Uani 1 1 d . A .
C15 C 0.5607(6) 0.8448(5) 0.3350(5) 0.0256(11) Uani 1 1 d . . .
C16 C 0.5976(6) 1.0461(5) 0.2276(5) 0.0270(11) Uani 1 1 d . A .
C17 C 0.1075(11) 0.7110(8) 0.1137(7) 0.060(2) Uani 1 1 d . . .
H17 H 0.0694 0.6158 0.0897 0.072 Uiso 1 1 calc R . .
C18 C 0.1084(10) 0.7715(7) 0.0386(6) 0.053(2) Uani 1 1 d . . .
H18 H 0.0708 0.7175 -0.0351 0.064 Uiso 1 1 calc R . .
C19 C 0.1655(7) 0.9123(6) 0.0740(5) 0.0294(11) Uani 1 1 d . . .
C20 C 0.2184(8) 0.9842(7) 0.1840(5) 0.0429(15) Uani 1 1 d . . .
H20 H 0.2573 1.0796 0.2111 0.051 Uiso 1 1 calc R . .
C21 C 0.2149(8) 0.9185(8) 0.2543(5) 0.0454(16) Uani 1 1 d . . .
H21A H 0.2526 0.9692 0.3288 0.055 Uiso 1 1 calc R . .
C22 C 0.1149(9) 0.9787(8) -0.1825(6) 0.0482(17) Uani 1 1 d . . .
H22A H 0.0801 0.9283 -0.2565 0.058 Uiso 1 1 calc R . .
C23 C 0.1146(9) 0.9101(7) -0.1135(5) 0.0425(15) Uani 1 1 d . . .
H23 H 0.0800 0.8156 -0.1408 0.051 Uiso 1 1 calc R . .
C24 C 0.1654(7) 0.9816(6) -0.0042(5) 0.0304(12) Uani 1 1 d . . .
C25 C 0.2168(9) 1.1223(7) 0.0315(6) 0.0471(17) Uani 1 1 d . . .
H25A H 0.2545 1.1761 0.1053 0.057 Uiso 1 1 calc R . .
C26 C 0.2107(9) 1.1800(7) -0.0446(6) 0.0483(17) Uani 1 1 d . . .
H26 H 0.2439 1.2742 -0.0196 0.058 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
Dy1 O1 2.393(4) . ?
Dy1 O3 2.526(3) . ?
Dy1 O3 2.606(4) 2_566 ?
Dy1 O4 2.463(4) 2_566 ?
Dy1 O7 2.376(4) 2_676 ?
Dy1 O1w 2.448(3) . ?
Dy1 O2w 2.476(4) . ?
Dy1 O3w 2.403(4) . ?
Dy1 O4w 2.591(4) . ?
O1 C1 1.266(6) . ?
O2 C1 1.220(7) . ?
O3 C8 1.275(6) . ?
O3 Dy1 2.606(3) 2_566 ?
O4 C8 1.243(6) . ?
O4 Dy1 2.463(4) 2_566 ?
O5 C15 1.239(7) . ?
O6 C15 1.254(7) . ?
O7 C16 1.262(7) . ?
O7 Dy1 2.376(4) 2_676 ?
O8 C16 1.225(6) . ?
O9 N2 1.250(8) . ?
O9' N1 1.356(19) . ?
O1w H11 0.838(10) . ?
O1w H12 0.837(10) . ?
O2w H21 0.840(10) . ?
O2w H22 0.834(10) . ?
O3w H31 0.839(10) . ?
O3w H32 0.839(10) . ?
O4w H41 0.836(10) . ?
O4w H42 0.834(10) . ?
O5w H51 0.834(10) . ?
O5w H52 0.837(10) . ?
N1 N2 1.195(7) . ?
N1 C7 1.418(7) . ?
N2 C9 1.465(7) . ?
N3 C17 1.292(10) . ?
N3 C21 1.314(9) . ?
N3 H3 0.874(10) . ?
N4 C26 1.303(9) . ?
N4 C22 1.336(9) . ?
C1 C2 1.516(6) . ?
C2 C3 1.384(7) . ?
C2 C7 1.399(7) . ?
C3 C4 1.394(6) . ?
C3 C8 1.484(7) . ?
C4 C5 1.381(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.372(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.385(7) . ?
C6 H6 0.9300 . ?
C9 C10 1.373(9) . ?
C9 C14 1.385(8) . ?
C10 C11 1.369(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.360(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.399(8) . ?
C12 H12A 0.9300 . ?
C13 C14 1.387(7) . ?
C13 C16 1.497(7) . ?
C14 C15 1.521(8) . ?
C17 C18 1.380(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.375(9) . ?
C18 H18 0.9300 . ?
C19 C20 1.371(9) . ?
C19 C24 1.486(7) . ?
C20 C21 1.364(8) . ?
C20 H20 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.371(9) . ?
C22 H22A 0.9300 . ?
C23 C24 1.368(8) . ?
C23 H23 0.9300 . ?
C24 C25 1.383(8) . ?
C25 C26 1.367(9) . ?
C25 H25A 0.9300 . ?
C26 H26 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Dy1 O1 133.96(13) 2_676 . ?
O7 Dy1 O3w 74.14(12) 2_676 . ?
O1 Dy1 O3w 107.79(13) . . ?
O7 Dy1 O1w 76.32(12) 2_676 . ?
O1 Dy1 O1w 81.26(12) . . ?
O3w Dy1 O1w 145.90(13) . . ?
O7 Dy1 O4 73.80(14) 2_676 2_566 ?
O1 Dy1 O4 136.00(13) . 2_566 ?
O3w Dy1 O4 113.42(14) . 2_566 ?
O1w Dy1 O4 73.41(12) . 2_566 ?
O7 Dy1 O2w 69.34(13) 2_676 . ?
O1 Dy1 O2w 66.36(12) . . ?
O3w Dy1 O2w 78.25(13) . . ?
O1w Dy1 O2w 75.67(12) . . ?
O4 Dy1 O2w 136.25(12) 2_566 . ?
O7 Dy1 O3 142.84(12) 2_676 . ?
O1 Dy1 O3 71.92(11) . . ?
O3w Dy1 O3 71.83(13) . . ?
O1w Dy1 O3 140.44(13) . . ?
O4 Dy1 O3 106.77(12) 2_566 . ?
O2w Dy1 O3 116.79(11) . . ?
O7 Dy1 O4w 137.95(12) 2_676 . ?
O1 Dy1 O4w 69.77(13) . . ?
O3w Dy1 O4w 139.42(12) . . ?
O1w Dy1 O4w 74.68(12) . . ?
O4 Dy1 O4w 69.15(14) 2_566 . ?
O2w Dy1 O4w 129.78(12) . . ?
O3 Dy1 O4w 69.08(11) . . ?
O7 Dy1 O3 94.32(13) 2_676 2_566 ?
O1 Dy1 O3 131.34(12) . 2_566 ?
O3w Dy1 O3 75.50(12) . 2_566 ?
O1w Dy1 O3 123.68(12) . 2_566 ?
O4 Dy1 O3 51.03(11) 2_566 2_566 ?
O2w Dy1 O3 152.11(12) . 2_566 ?
O3 Dy1 O3 63.06(14) . 2_566 ?
O4w Dy1 O3 77.54(12) . 2_566 ?
C1 O1 Dy1 122.4(3) . . ?
C8 O3 Dy1 138.7(3) . . ?
C8 O3 Dy1 90.3(3) . 2_566 ?
Dy1 O3 Dy1 116.93(13) . 2_566 ?
C8 O4 Dy1 97.9(3) . 2_566 ?
C16 O7 Dy1 140.2(3) . 2_676 ?
Dy1 O1w H11 118(4) . . ?
Dy1 O1w H12 114(4) . . ?
H11 O1w H12 109.6(18) . . ?
Dy1 O2w H21 115(5) . . ?
Dy1 O2w H22 113(4) . . ?
H21 O2w H22 109.9(18) . . ?
Dy1 O3w H31 100(5) . . ?
Dy1 O3w H32 116(5) . . ?
H31 O3w H32 109.4(18) . . ?
Dy1 O4w H41 98(5) . . ?
Dy1 O4w H42 99(5) . . ?
H41 O4w H42 110.4(19) . . ?
H51 O5w H52 110.3(18) . . ?
N2 N1 O9' 104.5(10) . . ?
N2 N1 C7 121.7(5) . . ?
O9' N1 C7 115.8(9) . . ?
N1 N2 O9 128.1(6) . . ?
N1 N2 C9 114.9(5) . . ?
O9 N2 C9 114.9(6) . . ?
C17 N3 C21 121.4(6) . . ?
C17 N3 H3 127(5) . . ?
C21 N3 H3 112(5) . . ?
C26 N4 C22 115.8(5) . . ?
O2 C1 O1 124.3(4) . . ?
O2 C1 C2 119.9(5) . . ?
O1 C1 C2 115.7(5) . . ?
C3 C2 C7 118.5(4) . . ?
C3 C2 C1 121.8(5) . . ?
C7 C2 C1 119.7(4) . . ?
C2 C3 C4 120.7(5) . . ?
C2 C3 C8 121.1(4) . . ?
C4 C3 C8 118.3(4) . . ?
C5 C4 C3 119.8(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 120.1(5) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C2 120.6(5) . . ?
C6 C7 N1 125.1(5) . . ?
C2 C7 N1 114.1(4) . . ?
O4 C8 O3 120.7(5) . . ?
O4 C8 C3 119.5(4) . . ?
O3 C8 C3 119.9(4) . . ?
C10 C9 C14 123.6(5) . . ?
C10 C9 N2 117.1(5) . . ?
C14 C9 N2 119.3(5) . . ?
C11 C10 C9 117.8(6) . . ?
C11 C10 H10 121.1 . . ?
C9 C10 H10 121.1 . . ?
C12 C11 C10 120.5(6) . . ?
C12 C11 H11A 119.7 . . ?
C10 C11 H11A 119.7 . . ?
C11 C12 C13 121.6(5) . . ?
C11 C12 H12A 119.2 . . ?
C13 C12 H12A 119.2 . . ?
C14 C13 C12 118.8(5) . . ?
C14 C13 C16 122.2(5) . . ?
C12 C13 C16 118.9(5) . . ?
C9 C14 C13 117.5(5) . . ?
C9 C14 C15 120.9(5) . . ?
C13 C14 C15 121.6(5) . . ?
O5 C15 O6 124.8(5) . . ?
O5 C15 C14 117.5(5) . . ?
O6 C15 C14 117.7(5) . . ?
O8 C16 O7 125.3(5) . . ?
O8 C16 C13 118.3(5) . . ?
O7 C16 C13 116.3(4) . . ?
N3 C17 C18 121.5(6) . . ?
N3 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C19 C18 C17 119.3(7) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C18 116.7(5) . . ?
C20 C19 C24 122.0(5) . . ?
C18 C19 C24 121.3(5) . . ?
C21 C20 C19 121.2(6) . . ?
C21 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
N3 C21 C20 119.9(6) . . ?
N3 C21 H21A 120.1 . . ?
C20 C21 H21A 120.1 . . ?
N4 C22 C23 123.5(6) . . ?
N4 C22 H22A 118.3 . . ?
C23 C22 H22A 118.3 . . ?
C24 C23 C22 119.5(6) . . ?
C24 C23 H23 120.2 . . ?
C22 C23 H23 120.2 . . ?
C23 C24 C25 117.4(5) . . ?
C23 C24 C19 121.9(5) . . ?
C25 C24 C19 120.7(5) . . ?
C26 C25 C24 118.3(6) . . ?
C26 C25 H25A 120.9 . . ?
C24 C25 H25A 120.9 . . ?
N4 C26 C25 125.5(6) . . ?
N4 C26 H26 117.2 . . ?
C25 C26 H26 117.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 Dy1 O1 C1 155.2(3) 2_676 . . . ?
O3w Dy1 O1 C1 70.3(4) . . . . ?
O1w Dy1 O1 C1 -143.6(4) . . . . ?
O4 Dy1 O1 C1 -88.7(4) 2_566 . . . ?
O2w Dy1 O1 C1 138.3(4) . . . . ?
O3 Dy1 O1 C1 7.0(4) . . . . ?
O4w Dy1 O1 C1 -66.8(4) . . . . ?
O3 Dy1 O1 C1 -15.8(4) 2_566 . . . ?
O7 Dy1 O3 C8 -68.0(6) 2_676 . . . ?
O1 Dy1 O3 C8 73.1(5) . . . . ?
O3w Dy1 O3 C8 -43.4(5) . . . . ?
O1w Dy1 O3 C8 122.8(5) . . . . ?
O4 Dy1 O3 C8 -153.2(5) 2_566 . . . ?
O2w Dy1 O3 C8 22.6(5) . . . . ?
O4w Dy1 O3 C8 147.7(5) . . . . ?
O3 Dy1 O3 C8 -126.0(6) 2_566 . . . ?
O7 Dy1 O3 Dy1 58.0(3) 2_676 . . 2_566 ?
O1 Dy1 O3 Dy1 -160.94(18) . . . 2_566 ?
O3w Dy1 O3 Dy1 82.60(17) . . . 2_566 ?
O1w Dy1 O3 Dy1 -111.2(2) . . . 2_566 ?
O4 Dy1 O3 Dy1 -27.15(19) 2_566 . . 2_566 ?
O2w Dy1 O3 Dy1 148.66(14) . . . 2_566 ?
O4w Dy1 O3 Dy1 -86.28(16) . . . 2_566 ?
O3 Dy1 O3 Dy1 0.0 2_566 . . 2_566 ?
O9' N1 N2 O9 -108.3(12) . . . . ?
C7 N1 N2 O9 25.2(12) . . . . ?
O9' N1 N2 C9 54.2(12) . . . . ?
C7 N1 N2 C9 -172.3(6) . . . . ?
Dy1 O1 C1 O2 96.0(6) . . . . ?
Dy1 O1 C1 C2 -86.2(5) . . . . ?
O2 C1 C2 C3 -88.8(7) . . . . ?
O1 C1 C2 C3 93.2(6) . . . . ?
O2 C1 C2 C7 92.1(7) . . . . ?
O1 C1 C2 C7 -85.8(7) . . . . ?
C7 C2 C3 C4 -0.3(8) . . . . ?
C1 C2 C3 C4 -179.4(5) . . . . ?
C7 C2 C3 C8 178.0(5) . . . . ?
C1 C2 C3 C8 -1.1(8) . . . . ?
C2 C3 C4 C5 0.6(8) . . . . ?
C8 C3 C4 C5 -177.8(5) . . . . ?
C3 C4 C5 C6 -0.2(9) . . . . ?
C4 C5 C6 C7 -0.4(9) . . . . ?
C5 C6 C7 C2 0.8(9) . . . . ?
C5 C6 C7 N1 176.2(6) . . . . ?
C3 C2 C7 C6 -0.4(9) . . . . ?
C1 C2 C7 C6 178.7(5) . . . . ?
C3 C2 C7 N1 -176.3(5) . . . . ?
C1 C2 C7 N1 2.8(8) . . . . ?
N2 N1 C7 C6 7.5(11) . . . . ?
O9' N1 C7 C6 136.2(12) . . . . ?
N2 N1 C7 C2 -176.8(7) . . . . ?
O9' N1 C7 C2 -48.0(13) . . . . ?
Dy1 O4 C8 O3 3.8(5) 2_566 . . . ?
Dy1 O4 C8 C3 -175.8(4) 2_566 . . . ?
Dy1 O3 C8 O4 130.3(5) . . . . ?
Dy1 O3 C8 O4 -3.5(5) 2_566 . . . ?
Dy1 O3 C8 C3 -50.1(7) . . . . ?
Dy1 O3 C8 C3 176.0(4) 2_566 . . . ?
C2 C3 C8 O4 157.7(5) . . . . ?
C4 C3 C8 O4 -23.9(8) . . . . ?
C2 C3 C8 O3 -21.8(8) . . . . ?
C4 C3 C8 O3 156.6(5) . . . . ?
N1 N2 C9 C10 -118.0(8) . . . . ?
O9 N2 C9 C10 46.8(9) . . . . ?
N1 N2 C9 C14 63.4(8) . . . . ?
O9 N2 C9 C14 -131.7(7) . . . . ?
C14 C9 C10 C11 -4.3(11) . . . . ?
N2 C9 C10 C11 177.3(6) . . . . ?
C9 C10 C11 C12 2.8(11) . . . . ?
C10 C11 C12 C13 0.3(12) . . . . ?
C11 C12 C13 C14 -2.1(10) . . . . ?
C11 C12 C13 C16 175.1(6) . . . . ?
C10 C9 C14 C13 2.5(9) . . . . ?
N2 C9 C14 C13 -179.0(5) . . . . ?
C10 C9 C14 C15 -178.4(6) . . . . ?
N2 C9 C14 C15 0.1(8) . . . . ?
C12 C13 C14 C9 0.7(8) . . . . ?
C16 C13 C14 C9 -176.3(5) . . . . ?
C12 C13 C14 C15 -178.4(5) . . . . ?
C16 C13 C14 C15 4.6(8) . . . . ?
C9 C14 C15 O5 -109.1(6) . . . . ?
C13 C14 C15 O5 70.0(7) . . . . ?
C9 C14 C15 O6 72.0(7) . . . . ?
C13 C14 C15 O6 -108.9(6) . . . . ?
Dy1 O7 C16 O8 14.5(10) 2_676 . . . ?
Dy1 O7 C16 C13 -165.3(4) 2_676 . . . ?
C14 C13 C16 O8 -148.2(6) . . . . ?
C12 C13 C16 O8 34.8(9) . . . . ?
C14 C13 C16 O7 31.6(8) . . . . ?
C12 C13 C16 O7 -145.4(6) . . . . ?
C21 N3 C17 C18 -0.9(13) . . . . ?
N3 C17 C18 C19 0.4(14) . . . . ?
C17 C18 C19 C20 -0.1(11) . . . . ?
C17 C18 C19 C24 -178.5(7) . . . . ?
C18 C19 C20 C21 0.4(10) . . . . ?
C24 C19 C20 C21 178.7(6) . . . . ?
C17 N3 C21 C20 1.1(11) . . . . ?
C19 C20 C21 N3 -0.9(11) . . . . ?
C26 N4 C22 C23 0.4(11) . . . . ?
N4 C22 C23 C24 -0.2(12) . . . . ?
C22 C23 C24 C25 -0.7(11) . . . . ?
C22 C23 C24 C19 179.0(6) . . . . ?
C20 C19 C24 C23 179.1(7) . . . . ?
C18 C19 C24 C23 -2.6(10) . . . . ?
C20 C19 C24 C25 -1.2(9) . . . . ?
C18 C19 C24 C25 177.1(7) . . . . ?
C23 C24 C25 C26 1.3(11) . . . . ?
C19 C24 C25 C26 -178.4(6) . . . . ?
C22 N4 C26 C25 0.3(12) . . . . ?
C24 C25 C26 N4 -1.2(13) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1w H11 O6 0.84(1) 1.93(1) 2.763(6) 170(6) 2_676
O1w H12 O5w 0.84(1) 1.85(2) 2.677(6) 167(7) .
O2w H21 O5 0.84(1) 2.03(2) 2.831(5) 159(5) .
O2w H22 O5 0.83(1) 1.89(2) 2.714(5) 173(6) 2_676
O3w H31 O8 0.84(1) 1.80(1) 2.632(6) 174(6) 2_676
O3w H32 O4w 0.84(1) 1.93(1) 2.768(5) 174(7) 2_566
O4w H41 O2 0.84(1) 2.22(3) 2.975(7) 150(5) .
O4w H42 O5w 0.83(1) 1.84(2) 2.667(5) 171(6) .
O5w H51 O6 0.83(1) 1.92(3) 2.719(6) 159(8) 1_455
O5w H52 N4 0.84(1) 1.92(1) 2.760(6) 178(7) 2_575

_diffrn_measured_fraction_theta_max 0.950
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.950
_refine_diff_density_max         1.711
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.168
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_er
_database_code_depnum_ccdc_archive 'CCDC 1558326'
_audit_update_record             
;
2017-09-03 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;

_vrf_PLAT029_er                  
;
PROBLEM:  _diffrn_measured_fraction_theta_full Low .......      0.959 Note 
RESPONSE: The fraction is 100% full at a 2\q~max~ of 50 \%.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C10 H9 N2), [Er (H2 O)4 (C16 H6 N2 O9), (H2 O)'
_chemical_formula_sum            'C26 H25 Er N4 O14'
_chemical_formula_weight         784.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   10.8744(6)
_cell_length_b                   11.4722(6)
_cell_length_c                   14.0935(7)
_cell_angle_alpha                102.0191(8)
_cell_angle_beta                 110.9302(7)
_cell_angle_gamma                113.5225(8)
_cell_volume                     1373.61(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6064
_cell_measurement_theta_min      2.2008
_cell_measurement_theta_max      28.1954

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             778
_exptl_absorpt_coefficient_mu    3.137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5096
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8451
_diffrn_reflns_av_R_equivalents  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6087
_reflns_number_gt                5671
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0381P)²+0.6208P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6087
_refine_ls_number_parameters     449
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0235
_refine_ls_wR_factor_ref         0.0620
_refine_ls_wR_factor_gt          0.0604
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.149926(13) 0.701171(12) 0.506643(9) 0.02046(5) Uani 1 1 d . . .
O1 O 0.1777(3) 0.6356(2) 0.35145(17) 0.0281(4) Uani 1 1 d . . .
O2 O -0.0015(3) 0.4437(3) 0.2006(2) 0.0501(7) Uani 1 1 d . . .
O3 O 0.0347(2) 0.4419(2) 0.43131(18) 0.0280(4) Uani 1 1 d . . .
O4 O 0.0330(3) 0.2599(2) 0.4573(2) 0.0325(5) Uani 1 1 d . . .
O5 O 0.4823(3) 0.8789(2) 0.36829(19) 0.0337(5) Uani 1 1 d . A .
O6 O 0.6802(3) 0.8482(3) 0.39792(19) 0.0372(5) Uani 1 1 d . A .
O7 O 0.7093(2) 1.0996(2) 0.32972(17) 0.0278(4) Uani 1 1 d . . .
O8 O 0.5518(3) 1.1155(2) 0.1870(2) 0.0457(6) Uani 1 1 d . . .
O9 O 0.4787(5) 0.4808(4) 0.1684(3) 0.0504(13) Uani 0.709(7) 1 d PU A 1
O9' O 0.2093(15) 0.5220(15) 0.1497(11) 0.080(4) Uani 0.291(7) 1 d PU A 2
O1w O 0.1392(3) 0.8754(2) 0.44460(18) 0.0280(4) Uani 1 1 d D . .
H11 H 0.192(3) 0.9571(19) 0.495(2) 0.042 Uiso 1 1 d D . .
H12 H 0.0478(16) 0.855(3) 0.410(3) 0.042 Uiso 1 1 d D . .
O2w O 0.4082(3) 0.8443(2) 0.53922(18) 0.0299(5) Uani 1 1 d D . .
H21 H 0.423(4) 0.840(3) 0.484(2) 0.045 Uiso 1 1 d D . .
H22 H 0.443(4) 0.9277(16) 0.578(2) 0.045 Uiso 1 1 d D . .
O3w O 0.2948(3) 0.6482(2) 0.63778(18) 0.0290(4) Uani 1 1 d D . .
H31 H 0.353(4) 0.720(2) 0.6976(17) 0.044 Uiso 1 1 d D . .
H32 H 0.247(4) 0.580(2) 0.649(3) 0.044 Uiso 1 1 d D . .
O4w O -0.1092(3) 0.5749(2) 0.33159(19) 0.0318(5) Uani 1 1 d D . .
H41 H -0.092(5) 0.545(4) 0.281(2) 0.048 Uiso 1 1 d D . .
H42 H -0.145(4) 0.625(4) 0.316(3) 0.048 Uiso 1 1 d D . .
O5w O -0.1573(3) 0.7827(3) 0.3117(2) 0.0381(5) Uani 1 1 d D . .
H51 H -0.200(5) 0.804(5) 0.345(3) 0.057 Uiso 1 1 d D . .
H52 H -0.172(5) 0.806(4) 0.258(2) 0.057 Uiso 1 1 d D . .
N1 N 0.3460(4) 0.5462(3) 0.2333(3) 0.0425(7) Uani 1 1 d . . .
N2 N 0.4309(4) 0.5602(3) 0.1928(3) 0.0379(7) Uani 1 1 d . A .
N3 N 0.1570(4) 0.7864(3) 0.2188(3) 0.0423(7) Uani 1 1 d D . .
H3 H 0.163(5) 0.745(4) 0.264(3) 0.051 Uiso 1 1 d D . .
N4 N 0.1607(4) 1.1124(3) -0.1510(2) 0.0398(7) Uani 1 1 d . . .
C1 C 0.1206(4) 0.5103(3) 0.2874(2) 0.0270(6) Uani 1 1 d . A .
C2 C 0.2156(3) 0.4451(3) 0.3242(2) 0.0244(6) Uani 1 1 d . . .
C3 C 0.1960(3) 0.3715(3) 0.3898(2) 0.0229(5) Uani 1 1 d . A .
C4 C 0.2864(4) 0.3133(3) 0.4231(3) 0.0280(6) Uani 1 1 d . . .
H4 H 0.2718 0.2632 0.4661 0.034 Uiso 1 1 calc R A .
C5 C 0.3971(4) 0.3301(3) 0.3923(3) 0.0309(6) Uani 1 1 d . A .
H5 H 0.4583 0.2928 0.4159 0.037 Uiso 1 1 calc R . .
C6 C 0.4178(4) 0.4022(3) 0.3263(3) 0.0316(7) Uani 1 1 d . . .
H6 H 0.4915 0.4120 0.3046 0.038 Uiso 1 1 calc R A .
C7 C 0.3282(4) 0.4598(3) 0.2929(3) 0.0287(6) Uani 1 1 d . A .
C8 C 0.0820(3) 0.3568(3) 0.4286(2) 0.0227(5) Uani 1 1 d . . .
C9 C 0.4492(4) 0.6628(3) 0.1453(3) 0.0316(7) Uani 1 1 d . . .
C10 C 0.4047(5) 0.6173(4) 0.0330(3) 0.0427(8) Uani 1 1 d . A .
H10 H 0.3684 0.5251 -0.0090 0.051 Uiso 1 1 calc R . .
C11 C 0.4153(5) 0.7111(4) -0.0150(3) 0.0459(9) Uani 1 1 d . . .
H11A H 0.3826 0.6820 -0.0908 0.055 Uiso 1 1 calc R A .
C12 C 0.4744(4) 0.8481(3) 0.0496(3) 0.0364(7) Uani 1 1 d . A .
H12A H 0.4804 0.9108 0.0163 0.044 Uiso 1 1 calc R . .
C13 C 0.5254(4) 0.8956(3) 0.1636(2) 0.0271(6) Uani 1 1 d . . .
C14 C 0.5116(3) 0.8008(3) 0.2134(2) 0.0252(6) Uani 1 1 d . A .
C15 C 0.5621(4) 0.8458(3) 0.3366(2) 0.0270(6) Uani 1 1 d . . .
C16 C 0.5998(4) 1.0488(3) 0.2313(2) 0.0267(6) Uani 1 1 d . A .
C17 C 0.1033(6) 0.7106(4) 0.1141(4) 0.0606(12) Uani 1 1 d . . .
H17 H 0.0629 0.6150 0.0902 0.073 Uiso 1 1 calc R . .
C18 C 0.1057(6) 0.7704(4) 0.0391(3) 0.0564(12) Uani 1 1 d . . .
H18 H 0.0686 0.7158 -0.0348 0.068 Uiso 1 1 calc R . .
C19 C 0.1640(4) 0.9126(3) 0.0745(3) 0.0313(7) Uani 1 1 d . . .
C20 C 0.2194(4) 0.9868(4) 0.1853(3) 0.0414(8) Uani 1 1 d . . .
H20 H 0.2604 1.0826 0.2124 0.050 Uiso 1 1 calc R . .
C21 C 0.2152(4) 0.9215(4) 0.2561(3) 0.0440(9) Uani 1 1 d . . .
H21A H 0.2537 0.9732 0.3310 0.053 Uiso 1 1 calc R . .
C22 C 0.1151(5) 0.9781(4) -0.1838(3) 0.0445(9) Uani 1 1 d . . .
H22A H 0.0811 0.9277 -0.2580 0.053 Uiso 1 1 calc R . .
C23 C 0.1150(5) 0.9083(4) -0.1145(3) 0.0418(8) Uani 1 1 d . . .
H23 H 0.0818 0.8140 -0.1418 0.050 Uiso 1 1 calc R . .
C24 C 0.1655(4) 0.9819(3) -0.0036(3) 0.0305(6) Uani 1 1 d . . .
C25 C 0.2156(5) 1.1213(4) 0.0308(3) 0.0467(9) Uani 1 1 d . . .
H25A H 0.2528 1.1753 0.1048 0.056 Uiso 1 1 calc R . .
C26 C 0.2107(5) 1.1811(4) -0.0446(3) 0.0494(10) Uani 1 1 d . . .
H26 H 0.2446 1.2756 -0.0192 0.059 Uiso 1 1 calc R . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.325(2) . ?
Er1 O3 2.511(2) . ?
Er1 O3 2.590(2) 2_566 ?
Er1 O4 2.398(2) 2_566 ?
Er1 O7 2.318(2) 2_676 ?
Er1 O1w 2.369(2) . ?
Er1 O2w 2.424(2) . ?
Er1 O3w 2.328(2) . ?
Er1 O4w 2.532(2) . ?
O1 C1 1.271(4) . ?
O2 C1 1.218(4) . ?
O3 C8 1.271(3) . ?
O3 Er1 2.591(2) 2_566 ?
O4 C8 1.246(3) . ?
O4 Er1 2.398(2) 2_566 ?
O5 C15 1.252(4) . ?
O6 C15 1.252(4) . ?
O7 C16 1.270(4) . ?
O7 Er1 2.318(2) 2_676 ?
O8 C16 1.237(4) . ?
O9 N2 1.262(4) . ?
O9' N1 1.399(13) . ?
O1w H11 0.845(10) . ?
O1w H12 0.838(10) . ?
O2w H21 0.839(10) . ?
O2w H22 0.838(10) . ?
O3w H31 0.837(10) . ?
O3w H32 0.836(10) . ?
O4w H41 0.839(10) . ?
O4w H42 0.841(10) . ?
O5w H51 0.834(10) . ?
O5w H52 0.839(10) . ?
N1 N2 1.224(4) . ?
N1 C7 1.426(4) . ?
N2 C9 1.453(4) . ?
N3 C17 1.311(5) . ?
N3 C21 1.312(5) . ?
N3 H3 0.869(10) . ?
N4 C26 1.322(5) . ?
N4 C22 1.328(5) . ?
C1 C2 1.514(4) . ?
C2 C3 1.392(4) . ?
C2 C7 1.405(4) . ?
C3 C4 1.399(4) . ?
C3 C8 1.490(4) . ?
C4 C5 1.377(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.387(4) . ?
C6 H6 0.9300 . ?
C9 C10 1.385(5) . ?
C9 C14 1.390(4) . ?
C10 C11 1.374(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.376(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.394(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.400(4) . ?
C13 C16 1.507(4) . ?
C14 C15 1.517(4) . ?
C17 C18 1.378(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.386(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.375(5) . ?
C19 C24 1.487(4) . ?
C20 C21 1.370(5) . ?
C20 H20 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.386(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.387(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.373(5) . ?
C25 C26 1.376(5) . ?
C25 H25A 0.9300 . ?
C26 H26 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Er1 O1 134.33(8) 2_676 . ?
O7 Er1 O3w 75.81(7) 2_676 . ?
O1 Er1 O3w 106.30(8) . . ?
O7 Er1 O1w 76.43(7) 2_676 . ?
O1 Er1 O1w 80.87(7) . . ?
O3w Er1 O1w 146.71(8) . . ?
O7 Er1 O4 73.33(8) 2_676 2_566 ?
O1 Er1 O4 136.19(8) . 2_566 ?
O3w Er1 O4 114.43(8) . 2_566 ?
O1w Er1 O4 74.09(7) . 2_566 ?
O7 Er1 O2w 69.44(8) 2_676 . ?
O1 Er1 O2w 66.84(8) . . ?
O3w Er1 O2w 77.34(8) . . ?
O1w Er1 O2w 75.96(8) . . ?
O4 Er1 O2w 136.48(8) 2_566 . ?
O7 Er1 O3 143.14(7) 2_676 . ?
O1 Er1 O3 72.27(7) . . ?
O3w Er1 O3 71.31(7) . . ?
O1w Er1 O3 139.82(7) . . ?
O4 Er1 O3 105.68(7) 2_566 . ?
O2w Er1 O3 117.57(7) . . ?
O7 Er1 O4w 137.33(8) 2_676 . ?
O1 Er1 O4w 70.34(8) . . ?
O3w Er1 O4w 138.26(7) . . ?
O1w Er1 O4w 75.01(7) . . ?
O4 Er1 O4w 68.77(8) 2_566 . ?
O2w Er1 O4w 131.10(7) . . ?
O3 Er1 O4w 68.15(7) . . ?
O7 Er1 O3 94.06(7) 2_676 2_566 ?
O1 Er1 O3 131.13(7) . 2_566 ?
O3w Er1 O3 74.90(7) . 2_566 ?
O1w Er1 O3 125.20(7) . 2_566 ?
O4 Er1 O3 51.84(7) 2_566 2_566 ?
O2w Er1 O3 150.51(7) . 2_566 ?
O3 Er1 O3 61.81(8) . 2_566 ?
O4w Er1 O3 77.65(7) . 2_566 ?
C1 O1 Er1 124.49(18) . . ?
C8 O3 Er1 137.66(18) . . ?
C8 O3 Er1 88.83(16) . 2_566 ?
Er1 O3 Er1 118.19(8) . 2_566 ?
C8 O4 Er1 98.55(18) . 2_566 ?
C16 O7 Er1 139.31(19) . 2_676 ?
Er1 O1w H11 115(3) . . ?
Er1 O1w H12 110(3) . . ?
H11 O1w H12 108.7(17) . . ?
Er1 O2w H21 119(3) . . ?
Er1 O2w H22 109(3) . . ?
H21 O2w H22 109.1(17) . . ?
Er1 O3w H31 108(3) . . ?
Er1 O3w H32 117(3) . . ?
H31 O3w H32 110.1(17) . . ?
Er1 O4w H41 103(3) . . ?
Er1 O4w H42 115(3) . . ?
H41 O4w H42 109.2(17) . . ?
H51 O5w H52 109.8(17) . . ?
N2 N1 O9' 105.4(6) . . ?
N2 N1 C7 121.0(3) . . ?
O9' N1 C7 115.8(5) . . ?
N1 N2 O9 128.2(3) . . ?
N1 N2 C9 114.3(3) . . ?
O9 N2 C9 116.0(3) . . ?
C17 N3 C21 121.5(3) . . ?
C17 N3 H3 117(3) . . ?
C21 N3 H3 121(3) . . ?
C26 N4 C22 116.2(3) . . ?
O2 C1 O1 124.0(3) . . ?
O2 C1 C2 120.2(3) . . ?
O1 C1 C2 115.8(3) . . ?
C3 C2 C7 118.5(3) . . ?
C3 C2 C1 121.8(3) . . ?
C7 C2 C1 119.7(3) . . ?
C2 C3 C4 120.4(3) . . ?
C2 C3 C8 120.7(3) . . ?
C4 C3 C8 118.9(2) . . ?
C5 C4 C3 120.2(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.4(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C7 119.6(3) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C6 C7 C2 120.9(3) . . ?
C6 C7 N1 125.5(3) . . ?
C2 C7 N1 113.4(3) . . ?
O4 C8 O3 120.7(3) . . ?
O4 C8 C3 119.2(3) . . ?
O3 C8 C3 120.1(2) . . ?
C10 C9 C14 123.1(3) . . ?
C10 C9 N2 117.5(3) . . ?
C14 C9 N2 119.4(3) . . ?
C11 C10 C9 118.7(3) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 119.7(3) . . ?
C10 C11 H11A 120.1 . . ?
C12 C11 H11A 120.1 . . ?
C11 C12 C13 121.7(3) . . ?
C11 C12 H12A 119.2 . . ?
C13 C12 H12A 119.2 . . ?
C12 C13 C14 119.4(3) . . ?
C12 C13 C16 119.1(3) . . ?
C14 C13 C16 121.4(3) . . ?
C9 C14 C13 117.3(3) . . ?
C9 C14 C15 121.0(3) . . ?
C13 C14 C15 121.7(3) . . ?
O5 C15 O6 125.6(3) . . ?
O5 C15 C14 116.8(3) . . ?
O6 C15 C14 117.6(3) . . ?
O8 C16 O7 125.2(3) . . ?
O8 C16 C13 118.2(3) . . ?
O7 C16 C13 116.6(3) . . ?
N3 C17 C18 121.0(4) . . ?
N3 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 119.5(4) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C18 116.9(3) . . ?
C20 C19 C24 121.4(3) . . ?
C18 C19 C24 121.7(3) . . ?
C21 C20 C19 120.9(3) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
N3 C21 C20 120.2(3) . . ?
N3 C21 H21A 119.9 . . ?
C20 C21 H21A 119.9 . . ?
N4 C22 C23 124.1(3) . . ?
N4 C22 H22A 118.0 . . ?
C23 C22 H22A 118.0 . . ?
C22 C23 C24 118.8(3) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
C25 C24 C23 117.1(3) . . ?
C25 C24 C19 121.4(3) . . ?
C23 C24 C19 121.6(3) . . ?
C24 C25 C26 119.8(3) . . ?
C24 C25 H25A 120.1 . . ?
C26 C25 H25A 120.1 . . ?
N4 C26 C25 124.0(3) . . ?
N4 C26 H26 118.0 . . ?
C25 C26 H26 118.0 . . ?

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
O7 Er1 O1 C1 155.7(2) 2_676 . . . ?
O3w Er1 O1 C1 69.8(2) . . . . ?
O1w Er1 O1 C1 -143.6(2) . . . . ?
O4 Er1 O1 C1 -88.2(2) 2_566 . . . ?
O2w Er1 O1 C1 137.9(3) . . . . ?
O3 Er1 O1 C1 6.2(2) . . . . ?
O4w Er1 O1 C1 -66.3(2) . . . . ?
O3 Er1 O1 C1 -14.2(3) 2_566 . . . ?
O7 Er1 O3 C8 -69.2(3) 2_676 . . . ?
O1 Er1 O3 C8 73.7(3) . . . . ?
O3w Er1 O3 C8 -41.1(3) . . . . ?
O1w Er1 O3 C8 124.1(3) . . . . ?
O4 Er1 O3 C8 -152.1(3) 2_566 . . . ?
O2w Er1 O3 C8 22.9(3) . . . . ?
O4w Er1 O3 C8 149.0(3) . . . . ?
O3 Er1 O3 C8 -123.6(3) 2_566 . . . ?
O7 Er1 O3 Er1 54.47(16) 2_676 . . 2_566 ?
O1 Er1 O3 Er1 -162.72(11) . . . 2_566 ?
O3w Er1 O3 Er1 82.49(10) . . . 2_566 ?
O1w Er1 O3 Er1 -112.27(11) . . . 2_566 ?
O4 Er1 O3 Er1 -28.52(11) 2_566 . . 2_566 ?
O2w Er1 O3 Er1 146.54(8) . . . 2_566 ?
O4w Er1 O3 Er1 -87.34(10) . . . 2_566 ?
O3 Er1 O3 Er1 0.0 2_566 . . 2_566 ?
O9' N1 N2 O9 -112.6(8) . . . . ?
C7 N1 N2 O9 21.2(6) . . . . ?
O9' N1 N2 C9 52.5(7) . . . . ?
C7 N1 N2 C9 -173.7(3) . . . . ?
Er1 O1 C1 O2 95.9(3) . . . . ?
Er1 O1 C1 C2 -84.8(3) . . . . ?
O2 C1 C2 C3 -89.5(4) . . . . ?
O1 C1 C2 C3 91.2(3) . . . . ?
O2 C1 C2 C7 91.2(4) . . . . ?
O1 C1 C2 C7 -88.1(3) . . . . ?
C7 C2 C3 C4 -0.3(4) . . . . ?
C1 C2 C3 C4 -179.6(3) . . . . ?
C7 C2 C3 C8 177.9(3) . . . . ?
C1 C2 C3 C8 -1.4(4) . . . . ?
C2 C3 C4 C5 0.9(5) . . . . ?
C8 C3 C4 C5 -177.3(3) . . . . ?
C3 C4 C5 C6 -1.3(5) . . . . ?
C4 C5 C6 C7 1.1(5) . . . . ?
C5 C6 C7 C2 -0.5(5) . . . . ?
C5 C6 C7 N1 174.4(3) . . . . ?
C3 C2 C7 C6 0.1(5) . . . . ?
C1 C2 C7 C6 179.4(3) . . . . ?
C3 C2 C7 N1 -175.4(3) . . . . ?
C1 C2 C7 N1 4.0(4) . . . . ?
N2 N1 C7 C6 10.6(6) . . . . ?
O9' N1 C7 C6 140.0(8) . . . . ?
N2 N1 C7 C2 -174.2(3) . . . . ?
O9' N1 C7 C2 -44.8(8) . . . . ?
Er1 O4 C8 O3 3.2(3) 2_566 . . . ?
Er1 O4 C8 C3 -176.2(2) 2_566 . . . ?
Er1 O3 C8 O4 129.9(3) . . . . ?
Er1 O3 C8 O4 -2.9(3) 2_566 . . . ?
Er1 O3 C8 C3 -50.7(4) . . . . ?
Er1 O3 C8 C3 176.5(2) 2_566 . . . ?
C2 C3 C8 O4 158.7(3) . . . . ?
C4 C3 C8 O4 -23.1(4) . . . . ?
C2 C3 C8 O3 -20.7(4) . . . . ?
C4 C3 C8 O3 157.5(3) . . . . ?
N1 N2 C9 C10 -120.1(4) . . . . ?
O9 N2 C9 C10 46.9(5) . . . . ?
N1 N2 C9 C14 60.8(4) . . . . ?
O9 N2 C9 C14 -132.2(4) . . . . ?
C14 C9 C10 C11 -3.4(6) . . . . ?
N2 C9 C10 C11 177.5(3) . . . . ?
C9 C10 C11 C12 2.3(6) . . . . ?
C10 C11 C12 C13 0.4(6) . . . . ?
C11 C12 C13 C14 -2.2(6) . . . . ?
C11 C12 C13 C16 175.5(3) . . . . ?
C10 C9 C14 C13 1.6(5) . . . . ?
N2 C9 C14 C13 -179.3(3) . . . . ?
C10 C9 C14 C15 -178.5(3) . . . . ?
N2 C9 C14 C15 0.6(5) . . . . ?
C12 C13 C14 C9 1.2(5) . . . . ?
C16 C13 C14 C9 -176.5(3) . . . . ?
C12 C13 C14 C15 -178.7(3) . . . . ?
C16 C13 C14 C15 3.6(5) . . . . ?
C9 C14 C15 O5 -109.7(3) . . . . ?
C13 C14 C15 O5 70.2(4) . . . . ?
C9 C14 C15 O6 71.0(4) . . . . ?
C13 C14 C15 O6 -109.1(3) . . . . ?
Er1 O7 C16 O8 15.6(5) 2_676 . . . ?
Er1 O7 C16 C13 -165.5(2) 2_676 . . . ?
C12 C13 C16 O8 34.7(5) . . . . ?
C14 C13 C16 O8 -147.7(3) . . . . ?
C12 C13 C16 O7 -144.3(3) . . . . ?
C14 C13 C16 O7 33.4(4) . . . . ?
C21 N3 C17 C18 -0.1(7) . . . . ?
N3 C17 C18 C19 -0.9(8) . . . . ?
C17 C18 C19 C20 1.2(7) . . . . ?
C17 C18 C19 C24 -178.3(4) . . . . ?
C18 C19 C20 C21 -0.6(6) . . . . ?
C24 C19 C20 C21 178.9(4) . . . . ?
C17 N3 C21 C20 0.7(6) . . . . ?
C19 C20 C21 N3 -0.4(6) . . . . ?
C26 N4 C22 C23 1.1(6) . . . . ?
N4 C22 C23 C24 -0.1(7) . . . . ?
C22 C23 C24 C25 -1.3(6) . . . . ?
C22 C23 C24 C19 178.1(4) . . . . ?
C20 C19 C24 C25 -3.1(5) . . . . ?
C18 C19 C24 C25 176.4(4) . . . . ?
C20 C19 C24 C23 177.6(4) . . . . ?
C18 C19 C24 C23 -3.0(6) . . . . ?
C23 C24 C25 C26 1.5(6) . . . . ?
C19 C24 C25 C26 -177.9(4) . . . . ?
C22 N4 C26 C25 -0.9(6) . . . . ?
C24 C25 C26 N4 -0.5(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1w H11 O6 0.85(1) 1.96(1) 2.797(3) 175(4) 2_676
O1w H12 O5w 0.84(1) 1.85(1) 2.675(3) 168(3) .
O2w H21 O5 0.84(1) 2.03(1) 2.853(3) 166(3) .
O2w H22 O5 0.84(1) 1.89(1) 2.711(3) 165(3) 2_676
O3w H31 O8 0.84(1) 1.80(1) 2.625(3) 168(4) 2_676
O3w H32 O4w 0.84(1) 1.96(1) 2.788(3) 171(4) 2_566
O4w H41 O2 0.84(1) 2.18(2) 2.973(4) 157(3) .
O4w H42 O5w 0.84(1) 1.87(2) 2.683(3) 161(4) .
O5w H51 O6 0.83(1) 1.89(1) 2.715(3) 171(4) 1_455
O5w H52 N4 0.84(1) 1.95(1) 2.774(4) 168(4) 2_575

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         1.179
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.093
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_tb
_database_code_depnum_ccdc_archive 'CCDC 1558324'
_audit_update_record             
;
2017-09-03 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_audit_creation_date             2017-09-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C16 H14 N2 O13 Tb, H2 O, C10 H9 N2'
_chemical_formula_sum            'C26 H25 N4 O14 Tb'
_chemical_formula_weight         776.41
_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                   10.9023(3)
_cell_length_b                   11.4881(3)
_cell_length_c                   13.1686(4)
_cell_angle_alpha                108.622(2)
_cell_angle_beta                 95.609(2)
_cell_angle_gamma                113.432(2)
_cell_volume                     1385.36(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4865
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.730
_cell_measurement_theta_min      3.733
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.634
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             770
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14757
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.334
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Single source'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4627
_reflns_number_total             4865
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         2.296
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         4865
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0253
_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)+(0.0324P)²+1.7943P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0667
_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
 H1WB-O1W
 0.84 with sigma of 0.02
 O1W-H1WB
 0.83 with sigma of 0.02
 H1WA-O1W
 0.83 with sigma of 0.02
3.a Free rotating group:
 O5W(H5WA,H5WB)
3.b Rotating group:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C17(H17), C18(H18),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26)
;
_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
Tb1 Tb 0.14292(2) 0.19394(2) 0.49316(2) 0.01652(7) Uani 1 1 d . . . . .
O1 O 0.1199(3) 0.2292(2) 0.3278(2) 0.0254(6) Uani 1 1 d . . . . .
O1W O 0.3704(3) 0.3058(3) 0.4610(2) 0.0267(6) Uani 1 1 d D . . . .
H1WA H 0.442(3) 0.352(5) 0.511(3) 0.054(16) Uiso 1 1 d D . . . .
H1WB H 0.371(5) 0.360(4) 0.431(4) 0.051(16) Uiso 1 1 d D . . . .
O2 O 0.1345(4) 0.0710(3) 0.1855(2) 0.0430(8) Uani 1 1 d . . . . .
O2W O 0.1951(3) 0.4338(2) 0.5555(2) 0.0244(6) Uani 1 1 d . . . . .
H2WA H 0.1314 0.4547 0.5906 0.037 Uiso 1 1 d GR . . . .
H2WB H 0.1967 0.4648 0.4979 0.037 Uiso 1 1 d GR . . . .
O3 O 0.3850(3) 0.4886(3) 0.3670(2) 0.0301(6) Uani 1 1 d . . . . .
O3W O 0.0601(3) 0.2451(3) 0.6707(2) 0.0274(6) Uani 1 1 d . . . . .
H3WA H 0.0427 0.3176 0.6846 0.041 Uiso 1 1 d GR . . . .
H3WB H 0.1237 0.2640 0.7299 0.041 Uiso 1 1 d GR . . . .
O4 O 0.2174(3) 0.5494(3) 0.3965(2) 0.0349(7) Uani 1 1 d . . . . .
O4W O 0.1535(3) 0.0060(2) 0.3583(2) 0.0260(6) Uani 1 1 d . . . . .
H4WA H 0.2277 0.0008 0.3801 0.039 Uiso 1 1 d GR . . . .
H4WB H 0.1544 0.0173 0.2967 0.039 Uiso 1 1 d GR . . . .
O5 O 0.7019(4) 0.7580(3) 0.2009(2) 0.0472(9) Uani 1 1 d . . . . .
O5W O 0.0315(3) 0.4715(3) 0.6890(2) 0.0346(7) Uani 1 1 d . . . . .
H5WA H 0.0770 0.5511 0.7409 0.052 Uiso 1 1 d G . . . .
H5WB H -0.0488 0.4602 0.6630 0.052 Uiso 1 1 d G . . . .
O6 O 0.6716(3) 0.7148(2) 0.3507(2) 0.0241(6) Uani 1 1 d . . . . .
O7 O 0.8954(3) 0.9906(2) 0.4318(2) 0.0224(6) Uani 1 1 d . . . . .
O8 O 0.9219(3) 1.1984(2) 0.4567(2) 0.0280(6) Uani 1 1 d . . . . .
O9 O 0.1887(5) 0.6868(4) 0.1679(4) 0.0893(15) Uani 1 1 d . . . . .
N1 N 0.2621(4) 0.6318(3) 0.1928(3) 0.0349(9) Uani 1 1 d . . . . .
N2 N 0.3870(3) 0.6866(3) 0.2315(3) 0.0412(10) Uani 1 1 d . . . . .
N3 N 0.1880(4) 0.7365(3) 0.8494(3) 0.0364(9) Uani 1 1 d . . . . .
N4 N 0.5608(4) 1.4333(3) 1.2192(3) 0.0387(9) Uani 1 1 d . . . . .
C1 C 0.1303(4) 0.1820(4) 0.2297(3) 0.0247(8) Uani 1 1 d . . . . .
C2 C 0.1372(4) 0.2690(4) 0.1627(3) 0.0263(8) Uani 1 1 d . . . . .
C3 C 0.0751(4) 0.2019(4) 0.0485(3) 0.0344(10) Uani 1 1 d . . . . .
H3 H 0.0371 0.1063 0.0153 0.041 Uiso 1 1 calc R . . . .
C4 C 0.0690(5) 0.2743(5) -0.0154(4) 0.0429(12) Uani 1 1 d . . . . .
H4 H 0.0254 0.2277 -0.0908 0.051 Uiso 1 1 calc R . . . .
C5 C 0.1280(5) 0.4162(4) 0.0327(4) 0.0401(11) Uani 1 1 d . . . . .
H5 H 0.1226 0.4666 -0.0091 0.048 Uiso 1 1 calc R . . . .
C6 C 0.1953(4) 0.4822(4) 0.1446(3) 0.0282(9) Uani 1 1 d . . . . .
C7 C 0.2015(4) 0.4124(4) 0.2125(3) 0.0238(8) Uani 1 1 d . . . . .
C8 C 0.2737(4) 0.4904(3) 0.3356(3) 0.0236(8) Uani 1 1 d . . . . .
C9 C 0.4640(4) 0.8331(4) 0.2923(3) 0.0259(8) Uani 1 1 d . . . . .
C10 C 0.4076(4) 0.9240(4) 0.3264(3) 0.0290(9) Uani 1 1 d . . . . .
H10 H 0.3125 0.8923 0.3050 0.035 Uiso 1 1 calc R . . . .
C11 C 0.4928(4) 1.0610(4) 0.3918(3) 0.0275(9) Uani 1 1 d . . . . .
H11 H 0.4549 1.1213 0.4155 0.033 Uiso 1 1 calc R . . . .
C12 C 0.6347(4) 1.1092(4) 0.4223(3) 0.0244(8) Uani 1 1 d . . . . .
H12 H 0.6921 1.2023 0.4646 0.029 Uiso 1 1 calc R . . . .
C13 C 0.6916(4) 1.0179(3) 0.3893(3) 0.0198(8) Uani 1 1 d . . . . .
C14 C 0.6074(4) 0.8793(3) 0.3244(3) 0.0206(8) Uani 1 1 d . . . . .
C15 C 0.6649(4) 0.7769(4) 0.2865(3) 0.0232(8) Uani 1 1 d . . . . .
C16 C 0.8450(4) 1.0725(4) 0.4288(3) 0.0200(8) Uani 1 1 d . . . . .
C17 C 0.2009(5) 0.8373(4) 0.8167(4) 0.0418(11) Uani 1 1 d . . . . .
H17 H 0.1615 0.8139 0.7427 0.050 Uiso 1 1 calc R . . . .
C18 C 0.2698(5) 0.9762(4) 0.8864(4) 0.0427(12) Uani 1 1 d . . . . .
H18 H 0.2746 1.0429 0.8592 0.051 Uiso 1 1 calc R . . . .
C19 C 0.3312(4) 1.0146(4) 0.9965(3) 0.0274(9) Uani 1 1 d . . . . .
C20 C 0.3150(5) 0.9091(4) 1.0309(4) 0.0456(12) Uani 1 1 d . . . . .
H20 H 0.3516 0.9289 1.1046 0.055 Uiso 1 1 calc R . . . .
C21 C 0.2446(5) 0.7745(4) 0.9556(4) 0.0475(13) Uani 1 1 d . . . . .
H21 H 0.2360 0.7056 0.9810 0.057 Uiso 1 1 calc R . . . .
C22 C 0.4098(4) 1.1614(4) 1.0737(3) 0.0276(9) Uani 1 1 d . . . . .
C23 C 0.4321(6) 1.2680(4) 1.0398(4) 0.0502(14) Uani 1 1 d . . . . .
H23 H 0.3956 1.2487 0.9662 0.060 Uiso 1 1 calc R . . . .
C24 C 0.5076(6) 1.4026(5) 1.1134(4) 0.0560(15) Uani 1 1 d . . . . .
H24 H 0.5218 1.4733 1.0889 0.067 Uiso 1 1 calc R . . . .
C25 C 0.5399(5) 1.3344(4) 1.2553(4) 0.0419(11) Uani 1 1 d . . . . .
H25 H 0.5762 1.3572 1.3298 0.050 Uiso 1 1 calc R . . . .
C26 C 0.4654(5) 1.1978(4) 1.1848(3) 0.0394(11) Uani 1 1 d . . . . .
H26 H 0.4523 1.1294 1.2120 0.047 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
Tb1 O1 2.346(2) . ?
Tb1 O1W 2.450(3) . ?
Tb1 O2W 2.410(2) . ?
Tb1 O3W 2.566(3) . ?
Tb1 O4W 2.370(2) . ?
Tb1 O6 2.353(2) 2_666 ?
Tb1 O7 2.522(2) 2_666 ?
Tb1 O7 2.598(2) 1_445 ?
Tb1 O8 2.434(3) 1_445 ?
Tb1 C16 2.884(4) 1_445 ?
O1 C1 1.268(4) . ?
O1W H1WA 0.82(2) . ?
O1W H1WB 0.828(14) . ?
O2 C1 1.243(5) . ?
O2W H2WA 0.9368 . ?
O2W H2WB 0.9339 . ?
O3 C8 1.254(5) . ?
O3W H3WA 0.8939 . ?
O3W H3WB 0.8949 . ?
O4 C8 1.248(5) . ?
O4W H4WA 0.8622 . ?
O4W H4WB 0.8619 . ?
O5 C15 1.218(5) . ?
O5W H5WA 0.8502 . ?
O5W H5WB 0.8502 . ?
O6 Tb1 2.353(2) 2_666 ?
O6 C15 1.282(4) . ?
O7 Tb1 2.598(2) 1_665 ?
O7 Tb1 2.522(2) 2_666 ?
O7 C16 1.273(4) . ?
O8 Tb1 2.435(3) 1_665 ?
O8 C16 1.251(4) . ?
O9 N1 1.276(5) . ?
N1 N2 1.220(5) . ?
N1 C6 1.451(5) . ?
N2 C9 1.437(5) . ?
N3 C17 1.321(6) . ?
N3 C21 1.325(6) . ?
N4 C24 1.330(6) . ?
N4 C25 1.315(6) . ?
C1 C2 1.516(5) . ?
C2 C3 1.399(5) . ?
C2 C7 1.392(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.373(6) . ?
C4 H4 0.9300 . ?
C4 C5 1.379(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.385(6) . ?
C6 C7 1.391(5) . ?
C7 C8 1.521(5) . ?
C9 C10 1.390(5) . ?
C9 C14 1.405(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.377(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.384(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.399(5) . ?
C13 C14 1.387(5) . ?
C13 C16 1.499(5) . ?
C14 C15 1.515(5) . ?
C16 Tb1 2.884(4) 1_665 ?
C17 H17 0.9300 . ?
C17 C18 1.389(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.382(6) . ?
C19 C20 1.379(6) . ?
C19 C22 1.482(5) . ?
C20 H20 0.9300 . ?
C20 C21 1.375(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.376(6) . ?
C22 C26 1.384(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.372(6) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
C25 C26 1.376(6) . ?
C26 H26 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O1W 69.46(9) . . ?
O1 Tb1 O2W 76.50(9) . . ?
O1 Tb1 O3W 137.68(9) . . ?
O1 Tb1 O4W 75.01(9) . . ?
O1 Tb1 O6 134.00(9) . 2_666 ?
O1 Tb1 O7 142.86(8) . 2_666 ?
O1 Tb1 O7 93.98(8) . 1_445 ?
O1 Tb1 O8 73.36(9) . 1_445 ?
O1 Tb1 C16 82.30(10) . 1_445 ?
O1W Tb1 O3W 130.44(9) . . ?
O1W Tb1 O7 151.08(9) . 1_445 ?
O1W Tb1 O7 117.21(9) . 2_666 ?
O1W Tb1 C16 151.75(10) . 1_445 ?
O2W Tb1 O1W 75.71(9) . . ?
O2W Tb1 O3W 74.90(8) . . ?
O2W Tb1 O7 124.73(8) . 1_445 ?
O2W Tb1 O7 140.15(8) . 2_666 ?
O2W Tb1 O8 73.85(8) . 1_445 ?
O2W Tb1 C16 99.07(9) . 1_445 ?
O3W Tb1 O7 77.82(8) . 1_445 ?
O3W Tb1 C16 72.25(9) . 1_445 ?
O4W Tb1 O1W 78.01(9) . . ?
O4W Tb1 O2W 146.46(9) . . ?
O4W Tb1 O3W 138.64(8) . . ?
O4W Tb1 O7 71.39(9) . 2_666 ?
O4W Tb1 O7 74.77(8) . 1_445 ?
O4W Tb1 O8 113.72(9) . 1_445 ?
O4W Tb1 C16 94.29(9) . 1_445 ?
O6 Tb1 O1W 66.41(9) 2_666 . ?
O6 Tb1 O2W 80.73(8) 2_666 . ?
O6 Tb1 O3W 70.13(9) 2_666 . ?
O6 Tb1 O4W 107.24(9) 2_666 . ?
O6 Tb1 O7 131.58(8) 2_666 1_445 ?
O6 Tb1 O7 72.41(8) 2_666 2_666 ?
O6 Tb1 O8 136.22(9) 2_666 1_445 ?
O6 Tb1 C16 141.03(10) 2_666 1_445 ?
O7 Tb1 O3W 68.61(8) 2_666 . ?
O7 Tb1 O7 62.38(9) 2_666 1_445 ?
O7 Tb1 C16 26.19(9) 1_445 1_445 ?
O7 Tb1 C16 84.85(9) 2_666 1_445 ?
O8 Tb1 O1W 136.22(9) 1_445 . ?
O8 Tb1 O3W 69.15(9) 1_445 . ?
O8 Tb1 O7 51.63(8) 1_445 1_445 ?
O8 Tb1 O7 106.33(8) 1_445 2_666 ?
O8 Tb1 C16 25.45(9) 1_445 1_445 ?
C1 O1 Tb1 140.0(2) . . ?
Tb1 O1W H1WA 123(4) . . ?
Tb1 O1W H1WB 110(4) . . ?
H1WA O1W H1WB 103(5) . . ?
Tb1 O2W H2WA 113.8 . . ?
Tb1 O2W H2WB 113.1 . . ?
H2WA O2W H2WB 105.1 . . ?
Tb1 O3W H3WA 111.4 . . ?
Tb1 O3W H3WB 111.5 . . ?
H3WA O3W H3WB 107.4 . . ?
Tb1 O4W H4WA 110.4 . . ?
Tb1 O4W H4WB 109.7 . . ?
H4WA O4W H4WB 108.7 . . ?
H5WA O5W H5WB 109.4 . . ?
C15 O6 Tb1 124.0(2) . 2_666 ?
Tb1 O7 Tb1 117.62(9) 2_666 1_665 ?
C16 O7 Tb1 89.6(2) . 1_665 ?
C16 O7 Tb1 138.0(2) . 2_666 ?
C16 O8 Tb1 97.8(2) . 1_665 ?
O9 N1 C6 115.0(3) . . ?
N2 N1 O9 127.9(4) . . ?
N2 N1 C6 115.2(3) . . ?
N1 N2 C9 121.1(4) . . ?
C17 N3 C21 116.0(4) . . ?
C25 N4 C24 120.2(4) . . ?
O1 C1 C2 116.5(3) . . ?
O2 C1 O1 124.8(4) . . ?
O2 C1 C2 118.7(3) . . ?
C3 C2 C1 118.5(3) . . ?
C7 C2 C1 121.5(3) . . ?
C7 C2 C3 119.9(4) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 C2 121.4(4) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.7(4) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 120.7 . . ?
C4 C5 C6 118.5(4) . . ?
C6 C5 H5 120.7 . . ?
C5 C6 N1 117.8(4) . . ?
C5 C6 C7 123.4(4) . . ?
C7 C6 N1 118.8(3) . . ?
C2 C7 C8 122.0(3) . . ?
C6 C7 C2 116.9(3) . . ?
C6 C7 C8 121.0(3) . . ?
O3 C8 C7 116.5(3) . . ?
O4 C8 O3 125.7(4) . . ?
O4 C8 C7 117.8(3) . . ?
C10 C9 N2 125.7(4) . . ?
C10 C9 C14 120.7(3) . . ?
C14 C9 N2 113.3(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 119.9(4) . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.3(4) . . ?
C12 C11 H11 119.8 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 119.9(3) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C16 118.4(3) . . ?
C14 C13 C12 120.6(3) . . ?
C14 C13 C16 120.9(3) . . ?
C9 C14 C15 119.2(3) . . ?
C13 C14 C9 118.5(3) . . ?
C13 C14 C15 122.3(3) . . ?
O5 C15 O6 123.9(4) . . ?
O5 C15 C14 120.7(3) . . ?
O6 C15 C14 115.3(3) . . ?
O7 C16 Tb1 64.26(18) . 1_665 ?
O7 C16 C13 119.9(3) . . ?
O8 C16 Tb1 56.77(18) . 1_665 ?
O8 C16 O7 121.0(3) . . ?
O8 C16 C13 119.1(3) . . ?
C13 C16 Tb1 174.6(2) . 1_665 ?
N3 C17 H17 118.1 . . ?
N3 C17 C18 123.8(4) . . ?
C18 C17 H17 118.1 . . ?
C17 C18 H18 120.2 . . ?
C19 C18 C17 119.6(4) . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C22 121.9(4) . . ?
C20 C19 C18 116.5(4) . . ?
C20 C19 C22 121.7(4) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 C19 119.7(4) . . ?
C21 C20 H20 120.2 . . ?
N3 C21 C20 124.4(4) . . ?
N3 C21 H21 117.8 . . ?
C20 C21 H21 117.8 . . ?
C23 C22 C19 122.5(4) . . ?
C23 C22 C26 116.5(4) . . ?
C26 C22 C19 121.0(4) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.8(4) . . ?
C24 C23 H23 119.6 . . ?
N4 C24 C23 120.9(4) . . ?
N4 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
N4 C25 H25 119.4 . . ?
N4 C25 C26 121.2(4) . . ?
C26 C25 H25 119.4 . . ?
C22 C26 H26 119.8 . . ?
C25 C26 C22 120.4(4) . . ?
C25 C26 H26 119.8 . . ?

_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_gd
_database_code_depnum_ccdc_archive 'CCDC 1558323'
_audit_update_record             
;
2017-09-03 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;

_vrf_PLAT029_gd                  
;
PROBLEM:  _diffrn_measured_fraction_theta_full Low .......      0.957 Note 
RESPONSE: The fraction is 100% full at a 2\q~max~ of 50 \%.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C10 H9 N2), [Gd (H2 O)4 (C16 H6 N2 O9), (H2 O)'
_chemical_formula_sum            'C26 H25 Gd N4 O14'
_chemical_formula_weight         774.75

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

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   11.0590(6)
_cell_length_b                   11.6279(7)
_cell_length_c                   13.3101(8)
_cell_angle_alpha                108.6658(8)
_cell_angle_beta                 95.5856(10)
_cell_angle_gamma                113.4215(8)
_cell_volume                     1437.46(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6554
_cell_measurement_theta_min      2.3093
_cell_measurement_theta_max      28.3241

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             770
_exptl_absorpt_coefficient_mu    2.386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_process_details   SADABS

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8751
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6612
_reflns_number_gt                5778
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0696P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6330
_refine_ls_number_parameters     449
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.1044
_refine_ls_wR_factor_gt          0.1002
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.142966(17) 0.693812(16) 0.493090(13) 0.02165(8) Uani 1 1 d . . .
O1 O 0.3291(3) 0.7856(3) 0.6508(2) 0.0307(6) Uani 1 1 d . . .
O2 O 0.2982(5) 0.7423(4) 0.7996(3) 0.0548(10) Uani 1 1 d . . .
O3 O 0.1047(3) 0.5085(3) 0.5671(2) 0.0279(6) Uani 1 1 d . . .
O4 O 0.0795(3) 0.3022(3) 0.5438(3) 0.0364(7) Uani 1 1 d . . .
O5 O 0.6147(3) 1.0115(3) 0.6327(3) 0.0367(7) Uani 1 1 d . . .
O6 O 0.7826(4) 0.9506(3) 0.6041(3) 0.0433(8) Uani 1 1 d . . .
O7 O 0.8789(3) 1.2705(3) 0.6731(2) 0.0315(6) Uani 1 1 d . . .
O8 O 0.8671(5) 1.4300(4) 0.8158(3) 0.0527(10) Uani 1 1 d . . .
O9 O 0.8094(6) 0.8143(5) 0.8326(5) 0.058(2) Uani 0.694(11) 1 d PU . .
O9' O 0.5617(19) 0.8699(19) 0.8512(16) 0.087(6) Uani 0.306(11) 1 d PU . .
O1w O 0.0600(3) 0.7467(3) 0.6710(3) 0.0357(7) Uani 1 1 d D . .
H11 H 0.114(5) 0.761(5) 0.728(3) 0.054 Uiso 1 1 d D . .
H12 H 0.037(5) 0.811(4) 0.686(4) 0.054 Uiso 1 1 d D . .
O2w O 0.1945(3) 0.9352(3) 0.5550(3) 0.0317(6) Uani 1 1 d D . .
H21 H 0.192(5) 0.962(5) 0.503(3) 0.048 Uiso 1 1 d D . .
H22 H 0.146(5) 0.958(6) 0.595(3) 0.048 Uiso 1 1 d D . .
O3w O 0.3720(3) 0.8074(3) 0.4621(3) 0.0341(7) Uani 1 1 d D . .
H31 H 0.439(4) 0.851(4) 0.518(3) 0.051 Uiso 1 1 d D . .
H32 H 0.377(5) 0.855(4) 0.425(4) 0.051 Uiso 1 1 d D . .
O4w O 0.1551(3) 0.5054(3) 0.3572(3) 0.0339(7) Uani 1 1 d D . .
H41 H 0.159(5) 0.523(5) 0.301(2) 0.051 Uiso 1 1 d D . .
H42 H 0.090(4) 0.428(3) 0.341(4) 0.051 Uiso 1 1 d D . .
O5w O 0.0306(4) 0.9724(3) 0.6884(3) 0.0429(8) Uani 1 1 d D . .
H51 H -0.051(2) 0.955(5) 0.666(5) 0.064 Uiso 1 1 d D . .
H52 H 0.072(5) 1.051(3) 0.738(4) 0.064 Uiso 1 1 d D . .
N1 N 0.6128(4) 0.8125(4) 0.7675(4) 0.0516(12) Uani 1 1 d . . .
N2 N 0.7380(4) 0.8673(4) 0.8072(4) 0.0447(10) Uani 1 1 d . . .
N3 N 0.4396(5) 1.0672(4) 0.7825(4) 0.0481(10) Uani 1 1 d D . .
H3 H 0.399(5) 0.982(2) 0.735(4) 0.058 Uiso 1 1 d D . .
N4 N 0.8120(5) 1.7632(4) 1.1499(3) 0.0442(10) Uani 1 1 d . . .
C1 C 0.3347(4) 0.7230(4) 0.7135(3) 0.0292(8) Uani 1 1 d . . .
C2 C 0.3929(4) 0.6209(4) 0.6763(4) 0.0283(8) Uani 1 1 d . . .
C3 C 0.5362(4) 0.6669(5) 0.7077(4) 0.0335(9) Uani 1 1 d . . .
C4 C 0.5919(5) 0.5762(5) 0.6744(4) 0.0354(9) Uani 1 1 d . . .
H4 H 0.6855 0.6073 0.6963 0.043 Uiso 1 1 calc R . .
C5 C 0.5071(5) 0.4391(5) 0.6084(4) 0.0375(10) Uani 1 1 d . . .
H5A H 0.5450 0.3798 0.5850 0.045 Uiso 1 1 calc R . .
C6 C 0.3653(4) 0.3899(4) 0.5770(4) 0.0307(9) Uani 1 1 d . . .
H6 H 0.3091 0.2980 0.5348 0.037 Uiso 1 1 calc R . .
C7 C 0.3081(4) 0.4818(4) 0.6104(3) 0.0259(8) Uani 1 1 d . . .
C8 C 0.1557(4) 0.4272(4) 0.5710(3) 0.0255(8) Uani 1 1 d . . .
C9 C 0.8030(5) 1.0172(5) 0.8553(4) 0.0369(10) Uani 1 1 d . . .
C10 C 0.8703(6) 1.0846(6) 0.9673(4) 0.0489(13) Uani 1 1 d . . .
H10 H 0.8752 1.0354 1.0093 0.059 Uiso 1 1 calc R . .
C11 C 0.9294(6) 1.2252(6) 1.0144(4) 0.0525(14) Uani 1 1 d . . .
H11A H 0.9733 1.2713 1.0889 0.063 Uiso 1 1 calc R . .
C12 C 0.9235(5) 1.2978(5) 0.9509(4) 0.0426(11) Uani 1 1 d . . .
H12A H 0.9613 1.3922 0.9841 0.051 Uiso 1 1 calc R . .
C13 C 0.8620(5) 1.2319(4) 0.8377(4) 0.0312(9) Uani 1 1 d . . .
C14 C 0.7980(4) 1.0880(4) 0.7877(3) 0.0303(8) Uani 1 1 d . . .
C15 C 0.7251(4) 1.0100(4) 0.6646(4) 0.0299(9) Uani 1 1 d . . .
C16 C 0.8693(4) 1.3186(4) 0.7707(3) 0.0305(9) Uani 1 1 d . . .
C17 C 0.4937(8) 1.0979(6) 0.8867(5) 0.0687(19) Uani 1 1 d . . .
H17 H 0.4822 1.0280 0.9103 0.082 Uiso 1 1 calc R . .
C18 C 0.5671(7) 1.2324(6) 0.9610(5) 0.0610(17) Uani 1 1 d . . .
H18A H 0.6014 1.2518 1.0343 0.073 Uiso 1 1 calc R . .
C19 C 0.5895(5) 1.3384(4) 0.9261(4) 0.0334(9) Uani 1 1 d . . .
C20 C 0.5348(6) 1.3013(5) 0.8164(4) 0.0465(12) Uani 1 1 d . . .
H20 H 0.5485 1.3685 0.7891 0.056 Uiso 1 1 calc R . .
C21 C 0.4600(6) 1.1658(6) 0.7463(4) 0.0510(13) Uani 1 1 d . . .
H21A H 0.4233 1.1433 0.6728 0.061 Uiso 1 1 calc R . .
C22 C 0.7984(6) 1.6614(5) 1.1821(4) 0.0509(13) Uani 1 1 d . . .
H22A H 0.8381 1.6844 1.2551 0.061 Uiso 1 1 calc R . .
C23 C 0.7286(6) 1.5234(5) 1.1134(4) 0.0492(13) Uani 1 1 d . . .
H23A H 0.7218 1.4575 1.1408 0.059 Uiso 1 1 calc R . .
C24 C 0.6692(5) 1.4855(5) 1.0035(4) 0.0347(9) Uani 1 1 d . . .
C25 C 0.6856(6) 1.5898(5) 0.9689(4) 0.0527(14) Uani 1 1 d . . .
H25 H 0.6503 1.5701 0.8957 0.063 Uiso 1 1 calc R . .
C26 C 0.7558(7) 1.7250(5) 1.0446(5) 0.0553(14) Uani 1 1 d . . .
H26 H 0.7635 1.7930 1.0195 0.066 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
Gd1 O7 2.385(3) 2_676 ?
Gd1 O1 2.400(3) . ?
Gd1 O4w 2.416(3) . ?
Gd1 O2w 2.458(3) . ?
Gd1 O4 2.484(3) 2_566 ?
Gd1 O3w 2.494(3) . ?
Gd1 O3 2.552(3) . ?
Gd1 O1w 2.601(3) . ?
Gd1 O3 2.631(3) 2_566 ?
O1 C1 1.284(5) . ?
O2 C1 1.234(5) . ?
O3 C8 1.289(5) . ?
O3 Gd1 2.631(3) 2_566 ?
O4 C8 1.259(5) . ?
O4 Gd1 2.484(3) 2_566 ?
O5 C15 1.262(5) . ?
O6 C15 1.274(6) . ?
O7 C16 1.273(5) . ?
O7 Gd1 2.385(3) 2_676 ?
O8 C16 1.252(5) . ?
O9 N2 1.259(6) . ?
O9' N1 1.398(17) . ?
O1w H11 0.842(10) . ?
O1w H12 0.846(10) . ?
O2w H21 0.845(10) . ?
O2w H22 0.842(10) . ?
O3w H31 0.841(10) . ?
O3w H32 0.841(10) . ?
O4w H41 0.836(10) . ?
O4w H42 0.842(10) . ?
O5w H51 0.842(10) . ?
O5w H52 0.843(10) . ?
N1 N2 1.243(6) . ?
N1 C3 1.443(6) . ?
N2 C9 1.471(6) . ?
N3 C17 1.327(8) . ?
N3 C21 1.329(7) . ?
N3 H3 0.876(10) . ?
N4 C26 1.327(7) . ?
N4 C22 1.342(7) . ?
C1 C2 1.536(6) . ?
C2 C7 1.411(6) . ?
C2 C3 1.424(6) . ?
C3 C4 1.400(6) . ?
C4 C5 1.395(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.402(6) . ?
C5 H5A 0.9300 . ?
C6 C7 1.424(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.511(6) . ?
C8 Gd1 2.933(4) 2_566 ?
C9 C10 1.401(7) . ?
C9 C14 1.412(6) . ?
C10 C11 1.382(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.386(7) . ?
C11 H11A 0.9300 . ?
C12 C13 1.403(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.413(6) . ?
C13 C16 1.530(6) . ?
C14 C15 1.539(6) . ?
C17 C18 1.389(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.394(7) . ?
C18 H18A 0.9300 . ?
C19 C20 1.379(7) . ?
C19 C24 1.504(6) . ?
C20 C21 1.381(7) . ?
C20 H20 0.9300 . ?
C21 H21A 0.9300 . ?
C22 C23 1.395(7) . ?
C22 H22A 0.9300 . ?
C23 C24 1.391(7) . ?
C23 H23A 0.9300 . ?
C24 C25 1.385(7) . ?
C25 C26 1.397(7) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Gd1 O1 133.84(10) 2_676 . ?
O7 Gd1 O4w 74.88(10) 2_676 . ?
O1 Gd1 O4w 107.05(11) . . ?
O7 Gd1 O2w 76.17(10) 2_676 . ?
O1 Gd1 O2w 81.10(10) . . ?
O4w Gd1 O2w 146.06(10) . . ?
O7 Gd1 O4 73.63(11) 2_676 2_566 ?
O1 Gd1 O4 136.21(11) . 2_566 ?
O4w Gd1 O4 113.92(11) . 2_566 ?
O2w Gd1 O4 73.69(10) . 2_566 ?
O7 Gd1 O3w 69.51(11) 2_676 . ?
O1 Gd1 O3w 66.14(10) . . ?
O4w Gd1 O3w 77.98(11) . . ?
O2w Gd1 O3w 75.58(10) . . ?
O4 Gd1 O3w 136.40(10) 2_566 . ?
O7 Gd1 O3 142.60(9) 2_676 . ?
O1 Gd1 O3 72.53(9) . . ?
O4w Gd1 O3 71.22(10) . . ?
O2w Gd1 O3 140.76(10) . . ?
O4 Gd1 O3 106.34(10) 2_566 . ?
O3w Gd1 O3 117.04(10) . . ?
O7 Gd1 O1w 137.46(10) 2_676 . ?
O1 Gd1 O1w 70.19(11) . . ?
O4w Gd1 O1w 139.29(10) . . ?
O2w Gd1 O1w 74.64(10) . . ?
O4 Gd1 O1w 68.91(11) 2_566 . ?
O3w Gd1 O1w 129.93(11) . . ?
O3 Gd1 O1w 69.38(9) . . ?
O7 Gd1 O3 94.42(10) 2_676 2_566 ?
O1 Gd1 O3 131.35(9) . 2_566 ?
O4w Gd1 O3 75.61(10) . 2_566 ?
O2w Gd1 O3 124.14(9) . 2_566 ?
O4 Gd1 O3 51.21(9) 2_566 2_566 ?
O3w Gd1 O3 151.96(10) . 2_566 ?
O3 Gd1 O3 62.36(11) . 2_566 ?
O1w Gd1 O3 77.51(10) . 2_566 ?
C1 O1 Gd1 123.4(2) . . ?
C8 O3 Gd1 138.3(3) . . ?
C8 O3 Gd1 90.2(2) . 2_566 ?
Gd1 O3 Gd1 117.64(10) . 2_566 ?
C8 O4 Gd1 97.8(2) . 2_566 ?
C16 O7 Gd1 139.6(3) . 2_676 ?
Gd1 O1w H11 114(4) . . ?
Gd1 O1w H12 116(4) . . ?
H11 O1w H12 108.1(17) . . ?
Gd1 O2w H21 114(4) . . ?
Gd1 O2w H22 115(4) . . ?
H21 O2w H22 108.5(17) . . ?
Gd1 O3w H31 117(4) . . ?
Gd1 O3w H32 115(4) . . ?
H31 O3w H32 109.0(18) . . ?
Gd1 O4w H41 106(4) . . ?
Gd1 O4w H42 116(4) . . ?
H41 O4w H42 109.5(18) . . ?
H51 O5w H52 108.6(18) . . ?
N2 N1 O9' 105.1(9) . . ?
N2 N1 C3 121.1(4) . . ?
O9' N1 C3 115.6(9) . . ?
N1 N2 O9 128.2(5) . . ?
N1 N2 C9 114.4(4) . . ?
O9 N2 C9 115.4(4) . . ?
C17 N3 C21 120.1(5) . . ?
C17 N3 H3 121(4) . . ?
C21 N3 H3 119(4) . . ?
C26 N4 C22 115.4(4) . . ?
O2 C1 O1 123.7(4) . . ?
O2 C1 C2 120.5(4) . . ?
O1 C1 C2 115.8(4) . . ?
C7 C2 C3 118.5(4) . . ?
C7 C2 C1 121.8(4) . . ?
C3 C2 C1 119.7(4) . . ?
C4 C3 C2 120.8(4) . . ?
C4 C3 N1 125.7(4) . . ?
C2 C3 N1 113.3(4) . . ?
C5 C4 C3 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.6(4) . . ?
C4 C5 H5A 119.7 . . ?
C6 C5 H5A 119.7 . . ?
C5 C6 C7 119.5(4) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C2 C7 C6 120.4(4) . . ?
C2 C7 C8 121.2(3) . . ?
C6 C7 C8 118.3(4) . . ?
O4 C8 O3 120.7(4) . . ?
O4 C8 C7 119.1(3) . . ?
O3 C8 C7 120.2(3) . . ?
O4 C8 Gd1 57.0(2) . 2_566 ?
O3 C8 Gd1 63.8(2) . 2_566 ?
C7 C8 Gd1 174.7(3) . 2_566 ?
C10 C9 C14 122.3(4) . . ?
C10 C9 N2 118.2(4) . . ?
C14 C9 N2 119.5(4) . . ?
C11 C10 C9 119.0(5) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10 C11 C12 120.1(5) . . ?
C10 C11 H11A 119.9 . . ?
C12 C11 H11A 119.9 . . ?
C11 C12 C13 121.5(4) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C12 C13 C14 119.6(4) . . ?
C12 C13 C16 118.8(4) . . ?
C14 C13 C16 121.6(4) . . ?
C9 C14 C13 117.4(4) . . ?
C9 C14 C15 120.7(4) . . ?
C13 C14 C15 121.9(4) . . ?
O5 C15 O6 126.0(4) . . ?
O5 C15 C14 117.1(4) . . ?
O6 C15 C14 116.8(4) . . ?
O8 C16 O7 125.7(4) . . ?
O8 C16 C13 118.2(4) . . ?
O7 C16 C13 116.1(4) . . ?
N3 C17 C18 121.2(5) . . ?
N3 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C19 120.1(5) . . ?
C17 C18 H18A 119.9 . . ?
C19 C18 H18A 119.9 . . ?
C20 C19 C18 116.5(4) . . ?
C20 C19 C24 121.6(4) . . ?
C18 C19 C24 122.0(4) . . ?
C21 C20 C19 121.1(5) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
N3 C21 C20 120.9(5) . . ?
N3 C21 H21A 119.5 . . ?
C20 C21 H21A 119.5 . . ?
N4 C22 C23 124.3(5) . . ?
N4 C22 H22A 117.8 . . ?
C23 C22 H22A 117.8 . . ?
C24 C23 C22 119.3(5) . . ?
C24 C23 H23A 120.3 . . ?
C22 C23 H23A 120.3 . . ?
C25 C24 C23 116.8(4) . . ?
C25 C24 C19 121.4(4) . . ?
C23 C24 C19 121.8(4) . . ?
C24 C25 C26 119.5(5) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
N4 C26 C25 124.6(5) . . ?
N4 C26 H26 117.7 . . ?
C25 C26 H26 117.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 Gd1 O1 C1 -155.1(3) 2_676 . . . ?
O4w Gd1 O1 C1 -69.9(3) . . . . ?
O2w Gd1 O1 C1 144.0(3) . . . . ?
O4 Gd1 O1 C1 89.0(3) 2_566 . . . ?
O3w Gd1 O1 C1 -137.9(3) . . . . ?
O3 Gd1 O1 C1 -6.6(3) . . . . ?
O1w Gd1 O1 C1 67.2(3) . . . . ?
O3 Gd1 O1 C1 15.7(4) 2_566 . . . ?
O7 Gd1 O3 C8 69.2(4) 2_676 . . . ?
O1 Gd1 O3 C8 -72.4(4) . . . . ?
O4w Gd1 O3 C8 43.1(4) . . . . ?
O2w Gd1 O3 C8 -122.5(4) . . . . ?
O4 Gd1 O3 C8 153.4(4) 2_566 . . . ?
O3w Gd1 O3 C8 -22.0(4) . . . . ?
O1w Gd1 O3 C8 -147.3(4) . . . . ?
O3 Gd1 O3 C8 126.4(4) 2_566 . . . ?
O7 Gd1 O3 Gd1 -57.2(2) 2_676 . . 2_566 ?
O1 Gd1 O3 Gd1 161.20(15) . . . 2_566 ?
O4w Gd1 O3 Gd1 -83.22(13) . . . 2_566 ?
O2w Gd1 O3 Gd1 111.12(16) . . . 2_566 ?
O4 Gd1 O3 Gd1 27.07(15) 2_566 . . 2_566 ?
O3w Gd1 O3 Gd1 -148.35(12) . . . 2_566 ?
O1w Gd1 O3 Gd1 86.34(13) . . . 2_566 ?
O3 Gd1 O3 Gd1 0.0 2_566 . . 2_566 ?
O9' N1 N2 O9 110.3(11) . . . . ?
C3 N1 N2 O9 -23.1(9) . . . . ?
O9' N1 N2 C9 -52.8(10) . . . . ?
C3 N1 N2 C9 173.8(5) . . . . ?
Gd1 O1 C1 O2 -95.7(5) . . . . ?
Gd1 O1 C1 C2 85.1(4) . . . . ?
O2 C1 C2 C7 88.8(6) . . . . ?
O1 C1 C2 C7 -92.0(5) . . . . ?
O2 C1 C2 C3 -91.8(6) . . . . ?
O1 C1 C2 C3 87.3(5) . . . . ?
C7 C2 C3 C4 -0.3(7) . . . . ?
C1 C2 C3 C4 -179.7(4) . . . . ?
C7 C2 C3 N1 175.4(4) . . . . ?
C1 C2 C3 N1 -4.0(6) . . . . ?
N2 N1 C3 C4 -9.6(8) . . . . ?
O9' N1 C3 C4 -138.5(11) . . . . ?
N2 N1 C3 C2 175.0(5) . . . . ?
O9' N1 C3 C2 46.0(12) . . . . ?
C2 C3 C4 C5 0.9(7) . . . . ?
N1 C3 C4 C5 -174.2(5) . . . . ?
C3 C4 C5 C6 -1.7(7) . . . . ?
C4 C5 C6 C7 1.8(7) . . . . ?
C3 C2 C7 C6 0.5(6) . . . . ?
C1 C2 C7 C6 179.8(4) . . . . ?
C3 C2 C7 C8 -177.9(4) . . . . ?
C1 C2 C7 C8 1.4(6) . . . . ?
C5 C6 C7 C2 -1.2(6) . . . . ?
C5 C6 C7 C8 177.2(4) . . . . ?
Gd1 O4 C8 O3 -3.2(4) 2_566 . . . ?
Gd1 O4 C8 C7 175.8(3) 2_566 . . . ?
Gd1 O3 C8 O4 -131.5(4) . . . . ?
Gd1 O3 C8 O4 3.0(4) 2_566 . . . ?
Gd1 O3 C8 C7 49.5(6) . . . . ?
Gd1 O3 C8 C7 -176.0(3) 2_566 . . . ?
Gd1 O3 C8 Gd1 -134.5(4) . . . 2_566 ?
C2 C7 C8 O4 -157.6(4) . . . . ?
C6 C7 C8 O4 24.0(6) . . . . ?
C2 C7 C8 O3 21.3(6) . . . . ?
C6 C7 C8 O3 -157.1(4) . . . . ?
C2 C7 C8 Gd1 -115(3) . . . 2_566 ?
C6 C7 C8 Gd1 66(3) . . . 2_566 ?
N1 N2 C9 C10 119.3(6) . . . . ?
O9 N2 C9 C10 -46.1(7) . . . . ?
N1 N2 C9 C14 -61.9(6) . . . . ?
O9 N2 C9 C14 132.8(6) . . . . ?
C14 C9 C10 C11 2.6(9) . . . . ?
N2 C9 C10 C11 -178.6(5) . . . . ?
C9 C10 C11 C12 -1.0(9) . . . . ?
C10 C11 C12 C13 -2.0(9) . . . . ?
C11 C12 C13 C14 3.4(8) . . . . ?
C11 C12 C13 C16 -175.0(5) . . . . ?
C10 C9 C14 C13 -1.1(7) . . . . ?
N2 C9 C14 C13 -179.9(4) . . . . ?
C10 C9 C14 C15 178.9(5) . . . . ?
N2 C9 C14 C15 0.0(7) . . . . ?
C12 C13 C14 C9 -1.8(7) . . . . ?
C16 C13 C14 C9 176.6(4) . . . . ?
C12 C13 C14 C15 178.2(4) . . . . ?
C16 C13 C14 C15 -3.4(7) . . . . ?
C9 C14 C15 O5 109.6(5) . . . . ?
C13 C14 C15 O5 -70.4(6) . . . . ?
C9 C14 C15 O6 -70.8(6) . . . . ?
C13 C14 C15 O6 109.2(5) . . . . ?
Gd1 O7 C16 O8 -14.9(8) 2_676 . . . ?
Gd1 O7 C16 C13 166.0(3) 2_676 . . . ?
C12 C13 C16 O8 -33.7(7) . . . . ?
C14 C13 C16 O8 147.9(5) . . . . ?
C12 C13 C16 O7 145.4(5) . . . . ?
C14 C13 C16 O7 -33.0(6) . . . . ?
C21 N3 C17 C18 2.9(11) . . . . ?
N3 C17 C18 C19 -2.3(11) . . . . ?
C17 C18 C19 C20 0.3(9) . . . . ?
C17 C18 C19 C24 -179.6(6) . . . . ?
C18 C19 C20 C21 1.1(8) . . . . ?
C24 C19 C20 C21 -179.0(5) . . . . ?
C17 N3 C21 C20 -1.4(9) . . . . ?
C19 C20 C21 N3 -0.6(9) . . . . ?
C26 N4 C22 C23 -1.2(9) . . . . ?
N4 C22 C23 C24 0.7(10) . . . . ?
C22 C23 C24 C25 1.0(9) . . . . ?
C22 C23 C24 C19 -178.4(5) . . . . ?
C20 C19 C24 C25 3.0(8) . . . . ?
C18 C19 C24 C25 -177.1(6) . . . . ?
C20 C19 C24 C23 -177.7(5) . . . . ?
C18 C19 C24 C23 2.2(8) . . . . ?
C23 C24 C25 C26 -1.9(9) . . . . ?
C19 C24 C25 C26 177.4(5) . . . . ?
C22 N4 C26 C25 0.2(9) . . . . ?
C24 C25 C26 N4 1.4(10) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1w H11 O2 0.84(1) 2.28(3) 3.026(5) 147(5) .
O1w H12 O5w 0.85(1) 1.90(2) 2.711(4) 160(6) .
O2w H21 O6 0.85(1) 1.98(1) 2.819(5) 170(6) 2_676
O2w H22 O5w 0.84(1) 1.89(1) 2.716(5) 168(5) .
O3w H31 O5 0.84(1) 2.08(2) 2.880(5) 160(4) .
O3w H32 O5 0.84(1) 1.92(2) 2.746(4) 169(6) 2_676
O4w H41 O8 0.84(1) 1.84(2) 2.658(5) 167(6) 2_676
O4w H42 O1w 0.84(1) 1.99(1) 2.824(4) 171(5) 2_566
O5w H51 O6 0.84(1) 1.92(2) 2.741(5) 166(6) 1_455
O5w H52 N4 0.84(1) 1.97(1) 2.810(5) 173(5) 2_687
N3 H3 O1 0.88(1) 1.97(2) 2.831(5) 168(6) .

_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         1.786
_refine_diff_density_min         -2.454
_refine_diff_density_rms         0.167
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Sm
_database_code_depnum_ccdc_archive 'CCDC 1558321'
_audit_update_record             
;
2017-09-03 deposited with the CCDC.
2017-09-18 downloaded from the CCDC.
;
_audit_creation_date             2017-09-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C16 H16 N2 O13 Sm, O, C10 H9 N2'
_chemical_formula_sum            'C26 H25 N4 O14 Sm'
_chemical_formula_weight         767.82
_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                   10.889(4)
_cell_length_b                   11.454(5)
_cell_length_c                   13.192(9)
_cell_angle_alpha                108.803(9)
_cell_angle_beta                 95.641(8)
_cell_angle_gamma                113.361(6)
_cell_volume                     1380.6(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5009
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.386
_cell_measurement_theta_min      2.334
_shelx_estimated_absorpt_T_max   0.577
_shelx_estimated_absorpt_T_min   0.465
_exptl_absorpt_coefficient_mu    2.209
_exptl_absorpt_correction_T_max  0.5768
_exptl_absorpt_correction_T_min  0.4646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7172
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.495
_diffrn_reflns_theta_min         1.689
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4539
_reflns_number_total             5025
_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       'SAINT v7.60A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.60A (Bruker, 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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         2.632
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5025
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0388
_refine_ls_restrained_S_all      1.076
_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)+(0.0919P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1255
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C19(H19), C20(H20), C21(H21)
2.b Tetrahedral OH refined with riding coordinates:
 O1W(H1WA), O2W(H2WA), O4W(H4WA)
;
_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 0.35703(2) -0.19386(2) 0.00715(2) 0.02266(13) Uani 1 1 d . . . . .
O1W O 0.1268(4) -0.3079(4) 0.0383(3) 0.0308(8) Uani 1 1 d . . . . .
H1WA H 0.1272 -0.3615 0.0671 0.046 Uiso 1 1 calc R . . . .
O1 O 1.3109(9) 0.3137(7) 0.3309(8) 0.108(3) Uani 1 1 d . . . . .
O2W O 0.3473(4) -0.0033(4) 0.1457(4) 0.0342(9) Uani 1 1 d . . . . .
H2WA H 0.3527 -0.0120 0.2050 0.051 Uiso 1 1 calc R . . . .
O2 O 1.2829(5) 0.4511(4) 0.1033(4) 0.0434(11) Uani 1 1 d . . . . .
O3W O 0.4388(5) -0.2475(4) -0.1724(4) 0.0357(10) Uani 1 1 d . . . . .
H3WA H 0.371(9) -0.264(8) -0.229(7) 0.054 Uiso 1 1 d R . . . .
H3WB H 0.455(8) -0.303(8) -0.196(7) 0.054 Uiso 1 1 d R . . . .
O3 O 1.1156(4) 0.5111(4) 0.1330(4) 0.0381(10) Uani 1 1 d . . . . .
O4W O 0.3051(4) -0.4382(4) -0.0551(3) 0.0316(9) Uani 1 1 d . . . . .
H4WA H 0.3530 -0.4540 -0.0967 0.047 Uiso 1 1 calc R . . . .
O4 O 0.6063(4) 0.0084(4) 0.0676(3) 0.0279(8) Uani 1 1 d . . . . .
O5 O 0.5812(4) -0.1981(4) 0.0447(4) 0.0388(10) Uani 1 1 d . . . . .
O5W O 0.5308(5) 0.4744(4) 0.1897(4) 0.0418(10) Uani 1 1 d . . . . .
O6 O 0.2021(6) -0.2402(5) -0.2987(4) 0.0584(15) Uani 1 1 d . . . . .
O7 O 0.1687(4) -0.2864(4) -0.1519(3) 0.0306(9) Uani 1 1 d . . . . .
O8 O 0.3796(4) -0.2290(4) 0.1745(3) 0.0324(9) Uani 1 1 d . . . . .
O9 O 0.3682(6) -0.0703(5) 0.3171(4) 0.0547(13) Uani 1 1 d . . . . .
N1 N 1.2370(6) 0.3672(5) 0.3058(5) 0.0456(14) Uani 1 1 d . . . . .
N2 N 1.1131(6) 0.3123(5) 0.2704(6) 0.0516(16) Uani 1 1 d . . . . .
N3 N 0.3127(6) 1.2633(5) 0.6492(5) 0.0411(13) Uani 1 1 d . . . . .
N4 N -0.0579(6) 0.5663(5) 0.2828(5) 0.0461(13) Uani 1 1 d . . . . .
C1 C -0.0051(10) 0.5977(7) 0.3864(7) 0.065(2) Uani 1 1 d . . . . .
H1 H -0.0187 0.5267 0.4105 0.078 Uiso 1 1 calc R . . . .
C2 C 0.0707(9) 0.7334(7) 0.4617(6) 0.060(2) Uani 1 1 d . . . . .
H2 H 0.1069 0.7532 0.5354 0.072 Uiso 1 1 calc R . . . .
C3 C 0.0917(6) 0.8382(6) 0.4265(5) 0.0355(13) Uani 1 1 d . . . . .
C4 C 0.0357(7) 0.8013(7) 0.3159(6) 0.0479(16) Uani 1 1 d . . . . .
H4 H 0.0486 0.8698 0.2888 0.058 Uiso 1 1 calc R . . . .
C5 C -0.0389(8) 0.6646(7) 0.2456(6) 0.0499(17) Uani 1 1 d . . . . .
H5 H -0.0764 0.6409 0.1712 0.060 Uiso 1 1 calc R . . . .
C6 C 0.1695(6) 0.9863(6) 0.5040(5) 0.0349(13) Uani 1 1 d . . . . .
C7 C 0.2311(9) 1.0248(7) 0.6121(6) 0.058(2) Uani 1 1 d . . . . .
H7 H 0.2281 0.9577 0.6384 0.070 Uiso 1 1 calc R . . . .
C8 C 0.2975(8) 1.1617(7) 0.6824(6) 0.0526(18) Uani 1 1 d . . . . .
H8 H 0.3336 1.1847 0.7569 0.063 Uiso 1 1 calc R . . . .
C9 C 0.2541(8) 1.2244(6) 0.5440(6) 0.0530(18) Uani 1 1 d . . . . .
H9 H 0.2604 1.2933 0.5191 0.064 Uiso 1 1 calc R . . . .
C10 C 0.1849(8) 1.0904(7) 0.4688(6) 0.0531(19) Uani 1 1 d . . . . .
H10 H 0.1487 1.0700 0.3949 0.064 Uiso 1 1 calc R . . . .
C11 C 1.2985(6) 0.5878(6) 0.2884(5) 0.0313(12) Uani 1 1 d . . . . .
C12 C 1.3028(7) 0.5169(6) 0.3545(6) 0.0386(14) Uani 1 1 d . . . . .
C13 C 1.3695(8) 0.5818(7) 0.4663(6) 0.0499(17) Uani 1 1 d . . . . .
H13 H 1.3747 0.5311 0.5079 0.060 Uiso 1 1 calc R . . . .
C14 C 1.4278(8) 0.7238(7) 0.5139(6) 0.0533(18) Uani 1 1 d . . . . .
H14 H 1.4715 0.7704 0.5893 0.064 Uiso 1 1 calc R . . . .
C15 C 1.4224(7) 0.7965(6) 0.4521(5) 0.0430(15) Uani 1 1 d . . . . .
H15 H 1.4596 0.8924 0.4863 0.052 Uiso 1 1 calc R . . . .
C16 C 1.3618(7) 0.7299(6) 0.3374(5) 0.0364(13) Uani 1 1 d . . . . .
C17 C 1.2258(6) 0.5096(5) 0.1644(5) 0.0297(12) Uani 1 1 d . . . . .
C18 C 1.0363(6) 0.1668(6) 0.2085(5) 0.0343(13) Uani 1 1 d . . . . .
C19 C 1.0924(6) 0.0768(6) 0.1740(6) 0.0372(14) Uani 1 1 d . . . . .
H19 H 1.1878 0.1096 0.1948 0.045 Uiso 1 1 calc R . . . .
C20 C 1.0089(6) -0.0606(6) 0.1094(5) 0.0346(13) Uani 1 1 d . . . . .
H20 H 1.0475 -0.1210 0.0873 0.042 Uiso 1 1 calc R . . . .
C21 C 0.8668(6) -0.1094(5) 0.0770(5) 0.0295(12) Uani 1 1 d . . . . .
H21 H 0.8099 -0.2025 0.0328 0.035 Uiso 1 1 calc R . . . .
C22 C 0.8088(6) -0.0183(5) 0.1109(5) 0.0272(11) Uani 1 1 d . . . . .
C23 C 0.8938(6) 0.1204(5) 0.1767(5) 0.0268(11) Uani 1 1 d . . . . .
C24 C 0.6576(6) -0.0729(5) 0.0714(5) 0.0269(11) Uani 1 1 d . . . . .
C25 C 0.3700(6) -0.1812(5) 0.2722(5) 0.0321(12) Uani 1 1 d . . . . .
C26 C 0.1652(6) -0.2224(5) -0.2138(5) 0.0282(12) Uani 1 1 d . . . . .
H1WB H 0.061(7) -0.344(7) -0.021(6) 0.034 Uiso 1 1 d R . . . .
H2WB H 0.405(7) 0.074(7) 0.158(6) 0.034 Uiso 1 1 d R . . . .
H4WB H 0.300(6) -0.489(6) 0.003(5) 0.034 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 O1W 2.472(4) . ?
Sm1 O2W 2.401(4) . ?
Sm1 O3W 2.586(5) . ?
Sm1 O4W 2.449(4) . ?
Sm1 O4 2.529(4) 2_655 ?
Sm1 O4 2.601(4) . ?
Sm1 O5 2.465(4) . ?
Sm1 O7 2.393(4) . ?
Sm1 O8 2.375(4) . ?
Sm1 C24 2.907(6) . ?
O1W H1WA 0.8200 . ?
O1W H1WB 0.86(7) . ?
O1 N1 1.266(8) . ?
O2W H2WA 0.8200 . ?
O2W H2WB 0.80(7) . ?
O2 C17 1.252(7) . ?
O3W H3WA 0.91(9) . ?
O3W H3WB 0.71(7) . ?
O3 C17 1.238(7) . ?
O4W H4WA 0.8200 . ?
O4W H4WB 1.10(6) . ?
O4 Sm1 2.529(4) 2_655 ?
O4 C24 1.273(6) . ?
O5 C24 1.242(6) . ?
O6 C26 1.210(7) . ?
O7 C26 1.268(6) . ?
O8 C25 1.260(7) . ?
O9 C25 1.226(7) . ?
N1 N2 1.203(7) . ?
N1 C12 1.445(7) . ?
N2 C18 1.424(7) . ?
N3 C8 1.328(9) . ?
N3 C9 1.316(9) . ?
N4 C1 1.301(10) . ?
N4 C5 1.320(9) . ?
C1 H1 0.9300 . ?
C1 C2 1.381(10) . ?
C2 H2 0.9300 . ?
C2 C3 1.368(9) . ?
C3 C4 1.380(9) . ?
C3 C6 1.488(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.371(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.360(10) . ?
C6 C10 1.371(9) . ?
C7 H7 0.9300 . ?
C7 C8 1.369(10) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C9 C10 1.365(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.379(8) . ?
C11 C16 1.373(8) . ?
C11 C17 1.532(8) . ?
C12 C13 1.383(10) . ?
C13 H13 0.9300 . ?
C13 C14 1.374(9) . ?
C14 H14 0.9300 . ?
C14 C15 1.352(9) . ?
C15 H15 0.9300 . ?
C15 C16 1.403(9) . ?
C16 C25 1.515(8) 1_665 ?
C18 C19 1.376(8) . ?
C18 C23 1.393(8) . ?
C19 H19 0.9300 . ?
C19 C20 1.371(9) . ?
C20 H20 0.9300 . ?
C20 C21 1.385(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.401(7) . ?
C22 C23 1.386(7) . ?
C22 C24 1.476(8) . ?
C23 C26 1.518(7) 2_655 ?
C25 C16 1.515(8) 1_445 ?
C26 C23 1.518(7) 2_655 ?

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
O1W Sm1 O3W 129.73(14) . . ?
O1W Sm1 O4 116.81(12) . 2_655 ?
O1W Sm1 O4 152.01(13) . . ?
O1W Sm1 C24 151.97(15) . . ?
O2W Sm1 O1W 78.20(14) . . ?
O2W Sm1 O3W 139.41(14) . . ?
O2W Sm1 O4W 145.72(14) . . ?
O2W Sm1 O4 71.82(14) . 2_655 ?
O2W Sm1 O4 75.44(13) . . ?
O2W Sm1 O5 113.16(15) . . ?
O2W Sm1 C24 94.44(15) . . ?
O3W Sm1 O4 77.68(13) . . ?
O3W Sm1 C24 72.37(16) . . ?
O4W Sm1 O1W 75.58(13) . . ?
O4W Sm1 O3W 74.87(13) . . ?
O4W Sm1 O4 140.63(14) . 2_655 ?
O4W Sm1 O4 123.83(12) . . ?
O4W Sm1 O5 73.59(13) . . ?
O4W Sm1 C24 98.39(13) . . ?
O4 Sm1 O3W 69.04(13) 2_655 . ?
O4 Sm1 O4 62.98(14) 2_655 . ?
O4 Sm1 C24 25.97(12) . . ?
O4 Sm1 C24 85.45(13) 2_655 . ?
O5 Sm1 O1W 136.18(13) . . ?
O5 Sm1 O3W 69.55(16) . . ?
O5 Sm1 O4 51.00(12) . . ?
O5 Sm1 O4 106.79(13) . 2_655 ?
O5 Sm1 C24 25.05(13) . . ?
O7 Sm1 O1W 66.38(14) . . ?
O7 Sm1 O2W 107.77(14) . . ?
O7 Sm1 O3W 69.66(15) . . ?
O7 Sm1 O4W 81.34(13) . . ?
O7 Sm1 O4 71.95(12) . 2_655 ?
O7 Sm1 O4 131.32(13) . . ?
O7 Sm1 O5 136.31(14) . . ?
O7 Sm1 C24 140.69(14) . . ?
O8 Sm1 O1W 69.45(14) . . ?
O8 Sm1 O2W 74.10(14) . . ?
O8 Sm1 O3W 138.02(14) . . ?
O8 Sm1 O4W 76.24(13) . . ?
O8 Sm1 O4 142.72(12) . 2_655 ?
O8 Sm1 O4 94.19(13) . . ?
O8 Sm1 O5 73.48(15) . . ?
O8 Sm1 O7 134.10(14) . . ?
O8 Sm1 C24 82.52(15) . . ?
Sm1 O1W H1WA 109.5 . . ?
Sm1 O1W H1WB 111(5) . . ?
H1WA O1W H1WB 115.1 . . ?
Sm1 O2W H2WA 109.5 . . ?
Sm1 O2W H2WB 118(5) . . ?
H2WA O2W H2WB 106.5 . . ?
Sm1 O3W H3WA 107(5) . . ?
Sm1 O3W H3WB 125(7) . . ?
H3WA O3W H3WB 102(8) . . ?
Sm1 O4W H4WA 109.5 . . ?
Sm1 O4W H4WB 122(3) . . ?
H4WA O4W H4WB 111.4 . . ?
Sm1 O4 Sm1 117.02(14) 2_655 . ?
C24 O4 Sm1 90.6(3) . . ?
C24 O4 Sm1 138.3(3) . 2_655 ?
C24 O5 Sm1 97.8(3) . . ?
C26 O7 Sm1 122.7(3) . . ?
C25 O8 Sm1 140.1(4) . . ?
O1 N1 C12 114.7(6) . . ?
N2 N1 O1 127.4(6) . . ?
N2 N1 C12 115.3(5) . . ?
N1 N2 C18 121.5(5) . . ?
C9 N3 C8 115.8(6) . . ?
C1 N4 C5 120.5(6) . . ?
N4 C1 H1 119.0 . . ?
N4 C1 C2 122.0(7) . . ?
C2 C1 H1 119.0 . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.2(7) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 C4 117.3(6) . . ?
C2 C3 C6 121.8(6) . . ?
C4 C3 C6 120.9(5) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.4(6) . . ?
C5 C4 H4 119.8 . . ?
N4 C5 C4 120.5(7) . . ?
N4 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C7 C6 C3 121.7(6) . . ?
C7 C6 C10 117.0(6) . . ?
C10 C6 C3 121.3(6) . . ?
C6 C7 H7 119.8 . . ?
C6 C7 C8 120.3(7) . . ?
C8 C7 H7 119.8 . . ?
N3 C8 C7 123.1(7) . . ?
N3 C8 H8 118.5 . . ?
C7 C8 H8 118.5 . . ?
N3 C9 H9 117.6 . . ?
N3 C9 C10 124.8(6) . . ?
C10 C9 H9 117.6 . . ?
C6 C10 H10 120.5 . . ?
C9 C10 C6 118.9(7) . . ?
C9 C10 H10 120.5 . . ?
C12 C11 C17 120.6(5) . . ?
C16 C11 C12 117.9(6) . . ?
C16 C11 C17 121.5(5) . . ?
C11 C12 N1 119.4(6) . . ?
C11 C12 C13 123.2(6) . . ?
C13 C12 N1 117.4(6) . . ?
C12 C13 H13 121.2 . . ?
C14 C13 C12 117.6(6) . . ?
C14 C13 H13 121.2 . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.7(7) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 119.4 . . ?
C14 C15 C16 121.1(6) . . ?
C16 C15 H15 119.4 . . ?
C11 C16 C15 119.4(6) . . ?
C11 C16 C25 122.5(5) . 1_665 ?
C15 C16 C25 118.1(5) . 1_665 ?
O2 C17 C11 117.6(5) . . ?
O3 C17 O2 125.6(6) . . ?
O3 C17 C11 116.8(5) . . ?
C19 C18 N2 125.4(6) . . ?
C19 C18 C23 120.6(6) . . ?
C23 C18 N2 113.8(5) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.6(6) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 120.1 . . ?
C19 C20 C21 119.8(5) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 120.0 . . ?
C20 C21 C22 119.9(5) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C24 118.4(5) . . ?
C23 C22 C21 119.9(5) . . ?
C23 C22 C24 121.6(4) . . ?
C18 C23 C26 119.5(5) . 2_655 ?
C22 C23 C18 119.0(5) . . ?
C22 C23 C26 121.4(5) . 2_655 ?
O4 C24 Sm1 63.5(3) . . ?
O4 C24 C22 120.1(5) . . ?
O5 C24 Sm1 57.2(3) . . ?
O5 C24 O4 120.6(5) . . ?
O5 C24 C22 119.2(5) . . ?
C22 C24 Sm1 174.7(4) . . ?
O8 C25 C16 115.7(5) . 1_445 ?
O9 C25 O8 125.4(6) . . ?
O9 C25 C16 118.9(5) . 1_445 ?
O6 C26 O7 124.4(5) . . ?
O6 C26 C23 120.0(5) . 2_655 ?
O7 C26 C23 115.6(5) . 2_655 ?

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 C24 Sm1 -134.0(5) 2_655 . . . ?
Sm1 O4 C24 O5 -131.4(5) 2_655 . . . ?
Sm1 O4 C24 O5 2.5(5) . . . . ?
Sm1 O4 C24 C22 50.4(8) 2_655 . . . ?
Sm1 O4 C24 C22 -175.6(5) . . . . ?
Sm1 O5 C24 O4 -2.7(6) . . . . ?
Sm1 O5 C24 C22 175.5(4) . . . . ?
Sm1 O7 C26 O6 95.7(7) . . . . ?
Sm1 O7 C26 C23 -86.0(5) . . . 2_655 ?
Sm1 O8 C25 O9 -15.4(10) . . . . ?
Sm1 O8 C25 C16 165.3(4) . . . 1_445 ?
O1 N1 N2 C18 -27.0(13) . . . . ?
O1 N1 C12 C11 132.1(8) . . . . ?
O1 N1 C12 C13 -46.9(10) . . . . ?
N1 N2 C18 C19 -6.1(11) . . . . ?
N1 N2 C18 C23 178.3(7) . . . . ?
N1 C12 C13 C14 -177.6(6) . . . . ?
N2 N1 C12 C11 -64.7(9) . . . . ?
N2 N1 C12 C13 116.2(8) . . . . ?
N2 C18 C19 C20 -176.4(7) . . . . ?
N2 C18 C23 C22 176.5(6) . . . . ?
N2 C18 C23 C26 -2.8(8) . . . 2_655 ?
N3 C9 C10 C6 2.4(13) . . . . ?
N4 C1 C2 C3 -0.4(14) . . . . ?
C1 N4 C5 C4 -0.7(12) . . . . ?
C1 C2 C3 C4 -0.4(12) . . . . ?
C1 C2 C3 C6 178.6(8) . . . . ?
C2 C3 C4 C5 0.6(11) . . . . ?
C2 C3 C6 C7 4.3(11) . . . . ?
C2 C3 C6 C10 -177.2(8) . . . . ?
C3 C4 C5 N4 -0.1(11) . . . . ?
C3 C6 C7 C8 -177.5(7) . . . . ?
C3 C6 C10 C9 178.3(7) . . . . ?
C4 C3 C6 C7 -176.8(7) . . . . ?
C4 C3 C6 C10 1.7(10) . . . . ?
C5 N4 C1 C2 0.9(13) . . . . ?
C6 C3 C4 C5 -178.3(6) . . . . ?
C6 C7 C8 N3 -4.0(13) . . . . ?
C7 C6 C10 C9 -3.1(12) . . . . ?
C8 N3 C9 C10 -2.2(12) . . . . ?
C9 N3 C8 C7 2.9(11) . . . . ?
C10 C6 C7 C8 3.9(12) . . . . ?
C11 C12 C13 C14 3.3(11) . . . . ?
C12 N1 N2 C18 172.3(6) . . . . ?
C12 C11 C16 C15 -2.8(9) . . . . ?
C12 C11 C16 C25 176.8(6) . . . 1_665 ?
C12 C11 C17 O2 -71.3(8) . . . . ?
C12 C11 C17 O3 109.3(6) . . . . ?
C12 C13 C14 C15 -1.6(12) . . . . ?
C13 C14 C15 C16 -2.3(12) . . . . ?
C14 C15 C16 C11 4.5(11) . . . . ?
C14 C15 C16 C25 -175.1(6) . . . 1_665 ?
C16 C11 C12 N1 179.9(6) . . . . ?
C16 C11 C12 C13 -1.1(10) . . . . ?
C16 C11 C17 O2 108.3(6) . . . . ?
C16 C11 C17 O3 -71.1(7) . . . . ?
C17 C11 C12 N1 -0.5(9) . . . . ?
C17 C11 C12 C13 178.5(6) . . . . ?
C17 C11 C16 C15 177.6(6) . . . . ?
C17 C11 C16 C25 -2.8(9) . . . 1_665 ?
C18 C19 C20 C21 0.9(10) . . . . ?
C19 C18 C23 C22 0.7(9) . . . . ?
C19 C18 C23 C26 -178.7(6) . . . 2_655 ?
C19 C20 C21 C22 -0.3(9) . . . . ?
C20 C21 C22 C23 0.0(9) . . . . ?
C20 C21 C22 C24 177.8(5) . . . . ?
C21 C22 C23 C18 -0.1(8) . . . . ?
C21 C22 C23 C26 179.2(5) . . . 2_655 ?
C21 C22 C24 O4 -156.6(5) . . . . ?
C21 C22 C24 O5 25.2(8) . . . . ?
C23 C18 C19 C20 -1.1(10) . . . . ?
C23 C22 C24 O4 21.2(8) . . . . ?
C23 C22 C24 O5 -157.0(6) . . . . ?
C24 C22 C23 C18 -177.9(6) . . . . ?
C24 C22 C23 C26 1.5(8) . . . 2_655 ?

_olex2_submission_special_instructions 'No special instructions were received'
