# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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. 
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data_1
_database_code_depnum_ccdc_archive 'CCDC 2255509'
_audit_update_record             
;
2023-04-11 deposited with the CCDC.	2023-11-21 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H22 N4 O20 Tb2), 4(H O0.50)'
_chemical_formula_sum            'C32 H50 N8 O43 Tb4'
_chemical_formula_weight         1870.48

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

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

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

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

_cell_length_a                   8.0598(9)
_cell_length_b                   11.6244(12)
_cell_length_c                   15.0918(16)
_cell_angle_alpha                78.2750(19)
_cell_angle_beta                 79.5600(17)
_cell_angle_gamma                72.4270(19)
_cell_volume                     1308.9(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5480
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      27.52

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.373
_exptl_crystal_F_000             902
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    5.467
_shelx_estimated_absorpt_T_min   0.611
_shelx_estimated_absorpt_T_max   0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.728
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7630
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.390
_diffrn_reflns_theta_max         25.496
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             4771
_reflns_number_gt                4242
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0405P)²+2.6400P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4771
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0753
_refine_ls_wR_factor_gt          0.0685
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.72109(3) 0.05800(2) 0.22404(2) 0.01401(8) Uani 1 1 d . . . . .
Tb2 Tb 0.00576(3) 0.49691(2) 0.28379(2) 0.01407(8) Uani 1 1 d . . . . .
O1 O 0.5922(5) 0.1373(3) 0.3825(2) 0.0244(8) Uani 1 1 d . . . . .
O1W O 0.9929(5) -0.0301(4) 0.1414(3) 0.0325(10) Uani 1 1 d . . . . .
H1WA H 1.077998 0.000151 0.119979 0.049 Uiso 1 1 d R U . . .
H1WB H 1.035035 -0.106509 0.156119 0.049 Uiso 1 1 d R U . . .
O2 O 0.3036(5) 0.3983(3) 0.2707(3) 0.0267(8) Uani 1 1 d . . . . .
O2W O 0.7086(5) -0.1290(3) 0.1746(3) 0.0273(8) Uani 1 1 d . . . . .
H2WA H 0.620937 -0.150092 0.205714 0.041 Uiso 1 1 d R U . . .
H2WB H 0.794526 -0.192662 0.173204 0.041 Uiso 1 1 d R U . . .
O3 O 0.5458(5) 0.2644(3) 0.2207(2) 0.0253(8) Uani 1 1 d . . . . .
O3W O 0.6817(5) 0.1252(4) 0.0704(2) 0.0301(9) Uani 1 1 d . . . . .
H3WA H 0.582449 0.177763 0.074046 0.045 Uiso 1 1 d R U . . .
H3WB H 0.745682 0.151633 0.024636 0.045 Uiso 1 1 d R U . . .
O4 O 0.8150(5) -0.0947(3) 0.3379(3) 0.0271(8) Uani 1 1 d . . . . .
O4W O -0.0369(9) 0.4268(4) 0.4421(3) 0.0641(17) Uani 1 1 d . . . . .
H4WA H -0.118978 0.470021 0.475069 0.096 Uiso 1 1 d R U . . .
H4WB H -0.044528 0.354051 0.455449 0.096 Uiso 1 1 d R U . . .
O5W O 0.1428(5) 0.6183(4) 0.3380(3) 0.0328(10) Uani 1 1 d . . . . .
H5WA H 0.081898 0.691252 0.340962 0.049 Uiso 1 1 d R U . . .
H5WB H 0.249797 0.618022 0.326693 0.049 Uiso 1 1 d R U . . .
O5 O 0.9665(6) -0.2152(4) 0.4469(3) 0.0379(10) Uani 1 1 d . . . . .
O6W O -0.2194(5) 0.6578(4) 0.3493(3) 0.0316(9) Uani 1 1 d . . . . .
H6WA H -0.229590 0.724362 0.367352 0.047 Uiso 1 1 d R U . . .
H6WB H -0.321179 0.648206 0.355242 0.047 Uiso 1 1 d R U . . .
O6 O 0.5638(5) -0.0509(4) 0.7497(3) 0.0272(9) Uani 1 1 d . . . . .
O7 O 0.6911(5) 0.0153(4) 0.8407(3) 0.0282(9) Uani 1 1 d . . . . .
O7W O 0.3983(5) 0.1246(4) 0.9930(3) 0.0317(9) Uani 1 1 d . . . . .
H7WA H 0.316751 0.190497 0.985609 0.048 Uiso 1 1 d R U . . .
H7WB H 0.367021 0.069517 0.976649 0.048 Uiso 1 1 d R U . . .
O8 O 0.0852(5) 0.4019(3) 0.1358(2) 0.0207(7) Uani 1 1 d . . . . .
O8W O 0.576(2) 0.483(3) 0.4937(11) 0.161(11) Uani 0.5 1 d . . P . .
H8WA H 0.621341 0.461960 0.543180 0.241 Uiso 0.5 1 d R U P . .
H8WB H 0.638173 0.428492 0.461999 0.241 Uiso 0.5 1 d R U P . .
O9 O -0.0756(5) 0.1534(3) 0.2460(3) 0.0252(8) Uani 1 1 d . . . . .
O10 O -0.0104(5) 0.2950(3) 0.3006(2) 0.0256(8) Uani 1 1 d . . . . .
O11 O 0.0091(5) 0.6507(3) 0.1609(2) 0.0262(8) Uani 1 1 d . . . . .
O12 O 0.0846(5) 0.7784(3) 0.0432(3) 0.0303(9) Uani 1 1 d . . . . .
O13 O 0.2493(5) 0.4920(4) -0.2304(3) 0.0328(9) Uani 1 1 d . . . . .
O14 O 0.5049(5) 0.3867(4) -0.2931(3) 0.0355(10) Uani 1 1 d . . . . .
C1 C 0.6606(6) 0.0893(5) 0.4619(3) 0.0198(10) Uani 1 1 d . . . . .
C2 C 0.7804(6) -0.0252(5) 0.4772(3) 0.0202(10) Uani 1 1 d . . . . .
C3 C 0.8137(7) -0.0319(5) 0.5648(4) 0.0224(11) Uani 1 1 d . . . . .
H3A H 0.890358 -0.097314 0.596500 0.027 Uiso 1 1 calc R U . . .
C4 C 0.4575(8) 0.2529(5) 0.3805(4) 0.0311(13) Uani 1 1 d . . . . .
H4A H 0.491757 0.307976 0.409401 0.037 Uiso 1 1 calc R U . . .
H4B H 0.348118 0.240018 0.413812 0.037 Uiso 1 1 calc R U . . .
C5 C 0.4329(6) 0.3078(4) 0.2836(3) 0.0181(10) Uani 1 1 d . . . . .
C6 C 0.8582(7) -0.1175(5) 0.4185(3) 0.0231(11) Uani 1 1 d . . . . .
C7 C 0.7159(7) 0.0995(5) 0.6846(3) 0.0230(11) Uani 1 1 d . . . . .
H7A H 0.639243 0.181540 0.686791 0.028 Uiso 1 1 calc R U . . .
H7B H 0.832762 0.100521 0.691470 0.028 Uiso 1 1 calc R U . . .
C8 C 0.6530(6) 0.0135(5) 0.7647(3) 0.0189(10) Uani 1 1 d . . . . .
C9 C 0.1826(6) 0.4450(4) 0.0594(3) 0.0169(10) Uani 1 1 d . . . . .
C10 C 0.1871(6) 0.5674(5) 0.0352(3) 0.0188(10) Uani 1 1 d . . . . .
C11 C 0.3030(7) 0.5663(5) -0.0452(4) 0.0224(11) Uani 1 1 d . . . . .
H11A H 0.336721 0.632944 -0.080549 0.027 Uiso 1 1 calc R U . . .
C12 C 0.0871(7) 0.2752(4) 0.1453(3) 0.0192(10) Uani 1 1 d . . . . .
H12A H 0.207018 0.223628 0.141195 0.023 Uiso 1 1 calc R U . . .
H12B H 0.031608 0.263793 0.097041 0.023 Uiso 1 1 calc R U . . .
C13 C -0.0126(6) 0.2414(4) 0.2379(3) 0.0163(10) Uani 1 1 d . . . . .
C14 C 0.0896(7) 0.6718(5) 0.0828(3) 0.0193(10) Uani 1 1 d . . . . .
C15 C 0.4817(6) 0.4055(5) -0.1388(3) 0.0229(11) Uani 1 1 d . . . . .
H15A H 0.530358 0.318101 -0.121908 0.028 Uiso 1 1 calc R U . . .
H15B H 0.577557 0.442798 -0.149032 0.028 Uiso 1 1 calc R U . . .
C16 C 0.4056(7) 0.4284(5) -0.2272(4) 0.0218(11) Uani 1 1 d . . . . .
N1 N 0.7206(6) 0.0680(4) 0.5962(3) 0.0230(9) Uani 1 1 d . . . . .
N2 N 0.6166(6) 0.1487(4) 0.5337(3) 0.0251(10) Uani 1 1 d . . . . .
N3 N 0.3564(6) 0.4522(4) -0.0620(3) 0.0223(9) Uani 1 1 d . . . . .
N4 N 0.2800(5) 0.3747(4) 0.0015(3) 0.0195(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O4 2.257(4) . ?
Tb1 O6 2.282(3) 2_656 ?
Tb1 O9 2.338(3) 1_655 ?
Tb1 O3W 2.338(4) . ?
Tb1 O1W 2.362(4) . ?
Tb1 O3 2.385(4) . ?
Tb1 O2W 2.472(4) . ?
Tb1 O1 2.658(3) . ?
Tb2 O11 2.302(4) . ?
Tb2 O13 2.300(4) 2_565 ?
Tb2 O2 2.318(4) . ?
Tb2 O10 2.349(3) . ?
Tb2 O4W 2.360(4) . ?
Tb2 O5W 2.370(4) . ?
Tb2 O6W 2.413(4) . ?
Tb2 O8 2.584(3) . ?
O1 C1 1.354(6) . ?
O1 C4 1.449(6) . ?
O1W H1WA 0.8469 . ?
O1W H1WB 0.8476 . ?
O2 C5 1.248(6) . ?
O2W H2WA 0.8472 . ?
O2W H2WB 0.8480 . ?
O3 C5 1.260(6) . ?
O3W H3WA 0.8480 . ?
O3W H3WB 0.8473 . ?
O4 C6 1.280(6) . ?
O4W H4WA 0.8482 . ?
O4W H4WB 0.8470 . ?
O5W H5WA 0.8478 . ?
O5W H5WB 0.8475 . ?
O5 C6 1.255(6) . ?
O6W H6WA 0.8474 . ?
O6W H6WB 0.8474 . ?
O6 C8 1.257(6) . ?
O7 C8 1.247(6) . ?
O7W H7WA 0.8479 . ?
O7W H7WB 0.8474 . ?
O8 C9 1.367(6) . ?
O8 C12 1.446(6) . ?
O8W O8W 1.17(4) 2_666 ?
O8W H8WA 0.8482 . ?
O8W H8WB 0.8482 . ?
O9 C13 1.249(6) . ?
O10 C13 1.240(6) . ?
O11 C14 1.253(6) . ?
O12 C14 1.254(6) . ?
O13 C16 1.257(6) . ?
O14 C16 1.240(6) . ?
C1 N2 1.339(7) . ?
C1 C2 1.392(7) . ?
C2 C3 1.378(7) . ?
C2 C6 1.452(7) . ?
C3 N1 1.306(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.495(7) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C7 N1 1.445(6) . ?
C7 C8 1.519(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C9 N4 1.305(6) . ?
C9 C10 1.405(7) . ?
C10 C11 1.391(7) . ?
C10 C14 1.476(7) . ?
C11 N3 1.327(7) . ?
C11 H11A 0.9300 . ?
C12 C13 1.522(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C15 N3 1.470(6) . ?
C15 C16 1.511(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
N1 N2 1.387(6) . ?
N3 N4 1.371(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Tb1 O6 95.90(14) . 2_656 ?
O4 Tb1 O9 89.57(14) . 1_655 ?
O6 Tb1 O9 146.87(13) 2_656 1_655 ?
O4 Tb1 O3W 149.96(14) . . ?
O6 Tb1 O3W 87.27(14) 2_656 . ?
O9 Tb1 O3W 103.96(13) 1_655 . ?
O4 Tb1 O1W 84.31(15) . . ?
O6 Tb1 O1W 140.70(13) 2_656 . ?
O9 Tb1 O1W 72.30(13) 1_655 . ?
O3W Tb1 O1W 74.81(14) . . ?
O4 Tb1 O3 133.43(13) . . ?
O6 Tb1 O3 73.88(13) 2_656 . ?
O9 Tb1 O3 78.69(13) 1_655 . ?
O3W Tb1 O3 76.15(13) . . ?
O1W Tb1 O3 131.94(14) . . ?
O4 Tb1 O2W 75.10(13) . . ?
O6 Tb1 O2W 71.77(13) 2_656 . ?
O9 Tb1 O2W 140.71(13) 1_655 . ?
O3W Tb1 O2W 77.62(14) . . ?
O1W Tb1 O2W 70.36(13) . . ?
O3 Tb1 O2W 137.30(13) . . ?
O4 Tb1 O1 71.37(12) . . ?
O6 Tb1 O1 74.63(13) 2_656 . ?
O9 Tb1 O1 76.31(12) 1_655 . ?
O3W Tb1 O1 137.52(13) . . ?
O1W Tb1 O1 140.12(13) . . ?
O3 Tb1 O1 62.08(11) . . ?
O2W Tb1 O1 128.95(12) . . ?
O11 Tb2 O13 80.12(15) . 2_565 ?
O11 Tb2 O2 98.41(14) . . ?
O13 Tb2 O2 142.19(14) 2_565 . ?
O11 Tb2 O10 133.70(13) . . ?
O13 Tb2 O10 73.58(15) 2_565 . ?
O2 Tb2 O10 81.32(13) . . ?
O11 Tb2 O4W 151.79(14) . . ?
O13 Tb2 O4W 105.8(2) 2_565 . ?
O2 Tb2 O4W 93.21(19) . . ?
O10 Tb2 O4W 73.37(14) . . ?
O11 Tb2 O5W 79.04(15) . . ?
O13 Tb2 O5W 141.34(14) 2_565 . ?
O2 Tb2 O5W 73.26(13) . . ?
O10 Tb2 O5W 141.71(14) . . ?
O4W Tb2 O5W 79.87(17) . . ?
O11 Tb2 O6W 82.10(14) . . ?
O13 Tb2 O6W 73.69(13) 2_565 . ?
O2 Tb2 O6W 143.94(13) . . ?
O10 Tb2 O6W 124.02(13) . . ?
O4W Tb2 O6W 73.55(17) . . ?
O5W Tb2 O6W 71.46(13) . . ?
O11 Tb2 O8 71.34(12) . . ?
O13 Tb2 O8 71.21(13) 2_565 . ?
O2 Tb2 O8 72.61(13) . . ?
O10 Tb2 O8 64.42(11) . . ?
O4W Tb2 O8 136.85(13) . . ?
O5W Tb2 O8 130.18(12) . . ?
O6W Tb2 O8 138.82(13) . . ?
C1 O1 C4 116.9(4) . . ?
C1 O1 Tb1 125.2(3) . . ?
C4 O1 Tb1 117.1(3) . . ?
Tb1 O1W H1WA 129.1 . . ?
Tb1 O1W H1WB 115.9 . . ?
H1WA O1W H1WB 107.6 . . ?
C5 O2 Tb2 153.5(3) . . ?
Tb1 O2W H2WA 107.8 . . ?
Tb1 O2W H2WB 123.3 . . ?
H2WA O2W H2WB 107.7 . . ?
C5 O3 Tb1 126.7(3) . . ?
Tb1 O3W H3WA 102.0 . . ?
Tb1 O3W H3WB 132.6 . . ?
H3WA O3W H3WB 107.7 . . ?
C6 O4 Tb1 143.4(3) . . ?
Tb2 O4W H4WA 118.8 . . ?
Tb2 O4W H4WB 114.0 . . ?
H4WA O4W H4WB 107.7 . . ?
Tb2 O5W H5WA 115.2 . . ?
Tb2 O5W H5WB 127.4 . . ?
H5WA O5W H5WB 107.8 . . ?
Tb2 O6W H6WA 139.3 . . ?
Tb2 O6W H6WB 113.1 . . ?
H6WA O6W H6WB 107.6 . . ?
C8 O6 Tb1 138.4(3) . 2_656 ?
H7WA O7W H7WB 107.7 . . ?
C9 O8 C12 115.9(4) . . ?
C9 O8 Tb2 123.2(3) . . ?
C12 O8 Tb2 116.6(3) . . ?
O8W O8W H8WA 111.9 2_666 . ?
O8W O8W H8WB 127.6 2_666 . ?
H8WA O8W H8WB 103.4 . . ?
C13 O9 Tb1 154.6(3) . 1_455 ?
C13 O10 Tb2 125.8(3) . . ?
C14 O11 Tb2 141.3(3) . . ?
C16 O13 Tb2 142.5(3) . 2_565 ?
N2 C1 O1 122.2(4) . . ?
N2 C1 C2 113.9(5) . . ?
O1 C1 C2 123.8(4) . . ?
C3 C2 C1 102.6(5) . . ?
C3 C2 C6 126.4(5) . . ?
C1 C2 C6 131.0(5) . . ?
N1 C3 C2 109.3(5) . . ?
N1 C3 H3A 125.4 . . ?
C2 C3 H3A 125.4 . . ?
O1 C4 C5 109.2(4) . . ?
O1 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
O1 C4 H4B 109.8 . . ?
C5 C4 H4B 109.8 . . ?
H4A C4 H4B 108.3 . . ?
O2 C5 O3 124.2(5) . . ?
O2 C5 C4 116.8(5) . . ?
O3 C5 C4 118.9(4) . . ?
O5 C6 O4 122.1(5) . . ?
O5 C6 C2 119.8(5) . . ?
O4 C6 C2 118.1(5) . . ?
N1 C7 C8 114.4(4) . . ?
N1 C7 H7A 108.7 . . ?
C8 C7 H7A 108.7 . . ?
N1 C7 H7B 108.7 . . ?
C8 C7 H7B 108.7 . . ?
H7A C7 H7B 107.6 . . ?
O7 C8 O6 125.4(5) . . ?
O7 C8 C7 116.6(4) . . ?
O6 C8 C7 118.0(4) . . ?
N4 C9 O8 122.3(4) . . ?
N4 C9 C10 113.7(4) . . ?
O8 C9 C10 124.0(4) . . ?
C11 C10 C9 103.0(4) . . ?
C11 C10 C14 128.7(5) . . ?
C9 C10 C14 128.3(4) . . ?
N3 C11 C10 107.0(4) . . ?
N3 C11 H11A 126.5 . . ?
C10 C11 H11A 126.5 . . ?
O8 C12 C13 107.9(4) . . ?
O8 C12 H12A 110.1 . . ?
C13 C12 H12A 110.1 . . ?
O8 C12 H12B 110.1 . . ?
C13 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
O10 C13 O9 125.6(5) . . ?
O10 C13 C12 117.8(4) . . ?
O9 C13 C12 116.3(4) . . ?
O11 C14 O12 122.1(5) . . ?
O11 C14 C10 118.4(4) . . ?
O12 C14 C10 119.5(4) . . ?
N3 C15 C16 114.9(4) . . ?
N3 C15 H15A 108.5 . . ?
C16 C15 H15A 108.5 . . ?
N3 C15 H15B 108.5 . . ?
C16 C15 H15B 108.5 . . ?
H15A C15 H15B 107.5 . . ?
O14 C16 O13 124.4(5) . . ?
O14 C16 C15 117.2(5) . . ?
O13 C16 C15 118.3(5) . . ?
C3 N1 N2 112.3(4) . . ?
C3 N1 C7 127.8(5) . . ?
N2 N1 C7 119.9(4) . . ?
C1 N2 N1 101.8(4) . . ?
C11 N3 N4 112.9(4) . . ?
C11 N3 C15 127.1(4) . . ?
N4 N3 C15 120.0(4) . . ?
C9 N4 N3 103.3(4) . . ?

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
_geom_hbond_publ_flag
O1W H1WA O7 0.85 2.00 2.668(5) 135.1 2_756 yes
O1W H1WB O12 0.85 2.28 2.766(5) 116.4 1_645 yes
O2W H2WB O11 0.85 2.11 2.959(5) 176.4 1_645 yes
O3W H3WB O12 0.85 1.85 2.658(5) 160.1 2_665 yes
O4W H4WA O8W 0.85 2.38 2.974(18) 127.3 1_455 yes
O4W H4WB O5 0.85 1.98 2.647(6) 134.7 2_656 yes
O5W H5WA O5 0.85 2.04 2.693(5) 133.3 1_465 yes
O5W H5WB O14 0.85 1.94 2.783(5) 176.1 2_665 yes
O6W H6WA O4 0.85 2.18 2.940(5) 148.6 1_465 yes
O6W H6WA O5 0.85 2.48 3.100(6) 131.1 1_465 yes
O6W H6WB O14 0.85 2.06 2.808(6) 146.4 2_565 yes
O7W H7WA N4 0.85 2.13 2.795(6) 135.2 1_556 yes
O7W H7WB O2W 0.85 2.38 2.802(6) 111.3 2_656 yes
O7W H7WB O3W 0.85 2.66 3.500(6) 171.2 2_656 yes
O8W H8WA O14 0.85 2.56 3.192(16) 132.7 1_556 yes
C3 H3A O10 0.93 2.53 3.422(6) 161.8 2_656 yes
C7 H7A O14 0.97 2.36 3.312(7) 167.0 1_556 yes
C11 H11A O3 0.93 2.39 3.245(6) 152.4 2_665 yes
C12 H12A O7 0.97 2.62 3.294(6) 126.8 2_656 yes
C12 H12B O12 0.97 2.65 3.614(7) 173.7 2_565 yes
C15 H15B O2 0.97 2.60 3.384(7) 138.1 2_665 yes

_refine_diff_density_max         0.946
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.156



