# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_MIL-164(La)
_database_code_depnum_ccdc_archive 'CCDC 1833257'
_audit_update_record             
;
2018-05-31 deposited with the CCDC.
2018-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            LaCl(Tz(OCH2CO2)2)(DMF)2
_chemical_melting_point          ?
_chemical_formula_moiety         LaCl(C6H4N4O6)(C3H7NO)2
_chemical_formula_sum            'C12 H18 Cl La N6 O8'
_chemical_formula_weight         548.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2870 2.4520 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.5822(5)
_cell_length_b                   18.3349(6)
_cell_length_c                   8.7335(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.582(2)
_cell_angle_gamma                90
_cell_volume                     1949.86(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11757
_cell_measurement_theta_min      2.008
_cell_measurement_theta_max      30.532

_exptl_crystal_description       platelet
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_F_000             1080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    2.381
_shelx_estimated_absorpt_T_min   0.832
_shelx_estimated_absorpt_T_max   0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6730
_exptl_absorpt_correction_T_max  0.7461
_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                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29902
_diffrn_reflns_av_unetI/netI     0.1284
_diffrn_reflns_av_R_equivalents  0.1484
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.008
_diffrn_reflns_theta_max         30.532
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5967
_reflns_number_gt                3246
_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       SAINT
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXS-86
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_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)+(0.0300P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5967
_refine_ls_number_parameters     257
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.0594
_refine_ls_wR_factor_ref         0.1129
_refine_ls_wR_factor_gt          0.0887
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
La1 La 0.80543(3) 0.75487(2) 0.18359(4) 0.01934(10) Uani 1 1 d . . . . .
Cl1 Cl 0.79890(18) 0.60192(9) 0.2030(2) 0.0466(5) Uani 1 1 d . . . . .
O1 O 0.7035(3) 0.7843(2) 0.3903(5) 0.0248(10) Uani 1 1 d . . . . .
O2 O 0.5985(4) 0.7891(2) 0.5581(5) 0.0277(10) Uani 1 1 d . . . . .
C1 C 0.6136(5) 0.8008(3) 0.4258(7) 0.0215(14) Uani 1 1 d . . . . .
C2 C 0.5260(5) 0.8344(4) 0.2946(8) 0.0319(17) Uani 1 1 d . . . . .
H2A H 0.5569 0.8759 0.2519 0.038 Uiso 1 1 calc R U . . .
H2B H 0.5029 0.7990 0.2102 0.038 Uiso 1 1 calc R U . . .
O3 O 0.4322(4) 0.8580(2) 0.3455(6) 0.0360(12) Uani 1 1 d . . . . .
C3 C 0.3689(5) 0.8069(4) 0.3877(8) 0.0264(15) Uani 1 1 d . . . . .
N1 N 0.2927(5) 0.8342(3) 0.4534(8) 0.0399(16) Uani 1 1 d . . . . .
N2 N 0.2274(5) 0.7861(3) 0.4996(8) 0.0368(16) Uani 1 1 d . . . . .
N3 N 0.3196(5) 0.6891(3) 0.4062(7) 0.0316(14) Uani 1 1 d . . . . .
N4 N 0.3839(4) 0.7364(3) 0.3589(6) 0.0312(13) Uani 1 1 d . . . . .
C4 C 0.2466(5) 0.7156(4) 0.4761(8) 0.0249(15) Uani 1 1 d . . . . .
O4 O 0.1881(4) 0.6645(2) 0.5287(6) 0.0348(12) Uani 1 1 d . . . . .
C5 C 0.0952(5) 0.6884(4) 0.5830(8) 0.0339(17) Uani 1 1 d . . . . .
H5A H 0.1174 0.7286 0.6562 0.041 Uiso 1 1 calc R U . . .
H5B H 0.0711 0.6488 0.6399 0.041 Uiso 1 1 calc R U . . .
C6 C -0.0003(5) 0.7127(3) 0.4484(7) 0.0233(14) Uani 1 1 d . . . . .
O5 O -0.0895(3) 0.7276(2) 0.4834(5) 0.0287(11) Uani 1 1 d . . . . .
O6 O 0.0106(4) 0.7145(2) 0.3127(5) 0.0308(11) Uani 1 1 d . . . . .
O7 O 0.6915(4) 0.8644(2) 0.0562(6) 0.0383(12) Uani 1 1 d . . . . .
C7 C 0.6214(6) 0.8777(4) -0.0665(9) 0.0390(19) Uani 1 1 d . . . . .
H7 H 0.5862 0.8380 -0.1237 0.047 Uiso 1 1 calc R U . . .
N5 N 0.5915(5) 0.9430(3) -0.1248(7) 0.0385(16) Uani 1 1 d . . . . .
C8 C 0.5183(8) 0.9527(4) -0.2791(10) 0.069(3) Uani 1 1 d . . . . .
H8A H 0.5576 0.9742 -0.3488 0.104 Uiso 1 1 calc R U . . .
H8B H 0.4589 0.9842 -0.2712 0.104 Uiso 1 1 calc R U . . .
H8C H 0.4894 0.9062 -0.3203 0.104 Uiso 1 1 calc R U . . .
C9 C 0.6479(8) 1.0080(4) -0.0494(11) 0.076(3) Uani 1 1 d . . . . .
H9A H 0.6908 0.9959 0.0548 0.114 Uiso 1 1 calc R U . . .
H9B H 0.5947 1.0446 -0.0422 0.114 Uiso 1 1 calc R U . . .
H9C H 0.6952 1.0264 -0.1113 0.114 Uiso 1 1 calc R U . . .
O8 O 0.9027(4) 0.8694(2) 0.2823(6) 0.0385(12) Uani 1 1 d . . . . .
C10 C 0.8745(6) 0.9253(4) 0.3419(9) 0.0420(19) Uani 1 1 d . . . . .
H10 H 0.8389 0.9199 0.4226 0.050 Uiso 1 1 calc R U . . .
N6 N 0.8922(5) 0.9924(3) 0.2966(8) 0.0413(16) Uani 1 1 d . . . . .
C11 C 0.9453(8) 1.0027(5) 0.1672(13) 0.083(4) Uani 1 1 d . . . . .
H11A H 1.0218 1.0130 0.2099 0.125 Uiso 1 1 calc R U . . .
H11B H 0.9113 1.0428 0.1023 0.125 Uiso 1 1 calc R U . . .
H11C H 0.9375 0.9591 0.1044 0.125 Uiso 1 1 calc R U . . .
C12 C 0.8595(9) 1.0568(4) 0.3681(12) 0.088(4) Uani 1 1 d . . . . .
H12A H 0.8053 1.0830 0.2905 0.132 Uiso 1 1 calc R U . . .
H12B H 0.9223 1.0874 0.4072 0.132 Uiso 1 1 calc R U . . .
H12C H 0.8290 1.0428 0.4541 0.132 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O5 2.464(4) 4_675 ?
La1 O8 2.474(4) . ?
La1 O1 2.522(4) . ?
La1 O7 2.554(4) . ?
La1 O6 2.649(4) 1_655 ?
La1 O1 2.658(4) 4_575 ?
La1 O5 2.667(4) 1_655 ?
La1 O2 2.682(4) 4_575 ?
La1 Cl1 2.8119(18) . ?
La1 C6 3.012(6) 1_655 ?
La1 C1 3.033(6) 4_575 ?
O1 C1 1.283(7) . ?
O1 La1 2.658(4) 4_576 ?
O2 C1 1.236(7) . ?
O2 La1 2.682(4) 4_576 ?
C1 C2 1.507(8) . ?
C1 La1 3.033(6) 4_576 ?
C2 O3 1.429(8) . ?
O3 C3 1.340(8) . ?
C3 N1 1.334(8) . ?
C3 N4 1.338(8) . ?
N1 N2 1.335(8) . ?
N2 C4 1.339(8) . ?
N3 C4 1.317(8) . ?
N3 N4 1.322(7) . ?
C4 O4 1.342(8) . ?
O4 C5 1.436(8) . ?
C5 C6 1.521(8) . ?
C6 O6 1.228(7) . ?
C6 O5 1.265(7) . ?
C6 La1 3.012(6) 1_455 ?
O5 La1 2.464(4) 4_476 ?
O5 La1 2.667(4) 1_455 ?
O6 La1 2.649(4) 1_455 ?
O7 C7 1.229(8) . ?
C7 N5 1.318(8) . ?
N5 C8 1.439(9) . ?
N5 C9 1.457(9) . ?
O8 C10 1.241(8) . ?
C10 N6 1.328(9) . ?
N6 C12 1.444(9) . ?
N6 C11 1.462(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 La1 O8 80.18(16) 4_675 . ?
O5 La1 O1 160.11(13) 4_675 . ?
O8 La1 O1 82.26(16) . . ?
O5 La1 O7 86.04(15) 4_675 . ?
O8 La1 O7 70.03(15) . . ?
O1 La1 O7 79.21(15) . . ?
O5 La1 O6 72.49(14) 4_675 1_655 ?
O8 La1 O6 75.24(15) . 1_655 ?
O1 La1 O6 111.82(13) . 1_655 ?
O7 La1 O6 141.73(15) . 1_655 ?
O5 La1 O1 64.31(13) 4_675 4_575 ?
O8 La1 O1 129.88(15) . 4_575 ?
O1 La1 O1 122.58(17) . 4_575 ?
O7 La1 O1 73.19(14) . 4_575 ?
O6 La1 O1 121.12(14) 1_655 4_575 ?
O5 La1 O5 119.96(16) 4_675 1_655 ?
O8 La1 O5 74.80(15) . 1_655 ?
O1 La1 O5 63.44(13) . 1_655 ?
O7 La1 O5 131.33(14) . 1_655 ?
O6 La1 O5 48.74(13) 1_655 1_655 ?
O1 La1 O5 153.52(12) 4_575 1_655 ?
O5 La1 O2 112.85(13) 4_675 4_575 ?
O8 La1 O2 137.87(15) . 4_575 ?
O1 La1 O2 74.96(13) . 4_575 ?
O7 La1 O2 71.18(14) . 4_575 ?
O6 La1 O2 146.29(13) 1_655 4_575 ?
O1 La1 O2 48.84(13) 4_575 4_575 ?
O5 La1 O2 122.36(13) 1_655 4_575 ?
O5 La1 Cl1 101.66(11) 4_675 . ?
O8 La1 Cl1 147.68(12) . . ?
O1 La1 Cl1 98.17(10) . . ?
O7 La1 Cl1 142.06(12) . . ?
O6 La1 Cl1 74.69(11) 1_655 . ?
O1 La1 Cl1 76.97(10) 4_575 . ?
O5 La1 Cl1 76.61(10) 1_655 . ?
O2 La1 Cl1 71.64(10) 4_575 . ?
O5 La1 C6 95.85(17) 4_675 1_655 ?
O8 La1 C6 73.49(16) . 1_655 ?
O1 La1 C6 88.04(16) . 1_655 ?
O7 La1 C6 142.58(16) . 1_655 ?
O6 La1 C6 23.96(15) 1_655 1_655 ?
O1 La1 C6 140.53(15) 4_575 1_655 ?
O5 La1 C6 24.79(15) 1_655 1_655 ?
O2 La1 C6 138.87(15) 4_575 1_655 ?
Cl1 La1 C6 74.22(12) . 1_655 ?
O5 La1 C1 89.21(16) 4_675 4_575 ?
O8 La1 C1 140.88(16) . 4_575 ?
O1 La1 C1 98.64(17) . 4_575 ?
O7 La1 C1 71.75(15) . 4_575 ?
O6 La1 C1 136.89(16) 1_655 4_575 ?
O1 La1 C1 24.94(15) 4_575 4_575 ?
O5 La1 C1 140.41(15) 1_655 4_575 ?
O2 La1 C1 23.98(14) 4_575 4_575 ?
Cl1 La1 C1 71.28(11) . 4_575 ?
C6 La1 C1 145.45(15) 1_655 4_575 ?
C1 O1 La1 149.6(4) . . ?
C1 O1 La1 94.1(4) . 4_576 ?
La1 O1 La1 115.03(16) . 4_576 ?
C1 O2 La1 94.2(4) . 4_576 ?
O2 C1 O1 122.5(6) . . ?
O2 C1 C2 121.8(6) . . ?
O1 C1 C2 115.7(6) . . ?
O2 C1 La1 61.9(3) . 4_576 ?
O1 C1 La1 60.9(3) . 4_576 ?
C2 C1 La1 174.2(4) . 4_576 ?
O3 C2 C1 112.9(6) . . ?
C3 O3 C2 118.0(5) . . ?
N1 C3 N4 126.5(7) . . ?
N1 C3 O3 113.4(6) . . ?
N4 C3 O3 120.1(6) . . ?
C3 N1 N2 116.5(6) . . ?
N1 N2 C4 116.3(6) . . ?
C4 N3 N4 117.1(6) . . ?
N3 N4 C3 116.6(6) . . ?
N3 C4 N2 126.9(7) . . ?
N3 C4 O4 114.0(6) . . ?
N2 C4 O4 119.0(6) . . ?
C4 O4 C5 117.5(5) . . ?
O4 C5 C6 112.6(6) . . ?
O6 C6 O5 123.3(6) . . ?
O6 C6 C5 119.7(6) . . ?
O5 C6 C5 116.9(6) . . ?
O6 C6 La1 61.2(3) . 1_455 ?
O5 C6 La1 62.1(3) . 1_455 ?
C5 C6 La1 177.5(4) . 1_455 ?
C6 O5 La1 150.1(4) . 4_476 ?
C6 O5 La1 93.1(4) . 1_455 ?
La1 O5 La1 116.76(16) 4_476 1_455 ?
C6 O6 La1 94.9(4) . 1_455 ?
C7 O7 La1 137.5(5) . . ?
O7 C7 N5 126.1(7) . . ?
C7 N5 C8 121.8(6) . . ?
C7 N5 C9 120.6(6) . . ?
C8 N5 C9 116.5(6) . . ?
C10 O8 La1 132.7(5) . . ?
O8 C10 N6 123.5(8) . . ?
C10 N6 C12 122.8(8) . . ?
C10 N6 C11 119.6(7) . . ?
C12 N6 C11 117.6(7) . . ?

_refine_diff_density_max         1.024
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.199


_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_MIL-165(Tb)
_database_code_depnum_ccdc_archive 'CCDC 1833258'
_audit_update_record             
;
2018-05-31 deposited with the CCDC.
2018-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            TbCl(Tz(OCH2CO2)2)(C3H7NO)2
_chemical_melting_point          ?
_chemical_formula_moiety         TbCl(C6H4N4O6)(C3H7NO)2
_chemical_formula_sum            'C12 H18 Cl N6 O8 Tb'
_chemical_formula_weight         568.69

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'
Cl Cl 0.1484 0.1585 '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                   8.443(5)
_cell_length_b                   10.802(6)
_cell_length_c                   11.764(8)
_cell_angle_alpha                64.44(2)
_cell_angle_beta                 84.15(3)
_cell_angle_gamma                89.13(4)
_cell_volume                     962.2(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    149(2)
_cell_measurement_reflns_used    6046
_cell_measurement_theta_min      2.091
_cell_measurement_theta_max      25.118

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.963
_exptl_crystal_F_000             556
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    3.867
_shelx_estimated_absorpt_T_min   0.512
_shelx_estimated_absorpt_T_max   0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3806
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   SADABDS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      149(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17158
_diffrn_reflns_av_unetI/netI     0.3552
_diffrn_reflns_av_R_equivalents  0.3562
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.091
_diffrn_reflns_theta_max         25.118
_diffrn_reflns_theta_full        25.118
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.966
_reflns_number_total             3317
_reflns_number_gt                1486
_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       SAINT
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
The poor quality of the diffraction dataset is associated with the very weak diffracting power
 of the crystal and the limited number of intense reflections.Data collection at low temperature
 (here 149 K) leads only to a very limited improvement. Utimately, few non -H atoms (mainly
 belonging to solvent molecules) had to be refined isotropically ; and the resulting precision
on bond lengths is low.  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0917P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3317
_refine_ls_number_parameters     207
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.2253
_refine_ls_R_factor_gt           0.1032
_refine_ls_wR_factor_ref         0.2674
_refine_ls_wR_factor_gt          0.2093
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_restrained_S_all      0.948
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.42262(15) 0.45488(13) 0.17903(11) 0.0339(5) Uani 1 1 d . . . . .
Cl2 Cl 0.4023(8) 0.6571(6) 0.2528(5) 0.0429(16) Uani 1 1 d . . . . .
O1 O 0.3297(17) 0.2353(16) 0.1939(12) 0.034(4) Uani 1 1 d . U . . .
O2 O 0.4593(17) 0.3622(15) 0.0084(13) 0.031(4) Uiso 1 1 d . U . . .
C1 C 0.379(3) 0.258(3) 0.082(2) 0.039(6) Uiso 1 1 d . . . . .
C2 C 0.348(3) 0.147(3) 0.035(2) 0.041(6) Uani 1 1 d . . . . .
H2A H 0.304560 0.189545 -0.048333 0.050 Uiso 1 1 calc R U . . .
H2B H 0.448002 0.101826 0.025119 0.050 Uiso 1 1 calc R U . . .
O3 O 0.2388(18) 0.0513(15) 0.1242(12) 0.032(4) Uani 1 1 d . . . . .
C3 C 0.183(3) -0.040(2) 0.089(2) 0.037(6) Uani 1 1 d . . . . .
N1 N 0.259(2) -0.058(2) -0.0073(18) 0.041(5) Uani 1 1 d . . . . .
N2 N 0.198(2) -0.148(2) -0.0394(16) 0.038(5) Uani 1 1 d . . . . .
N3 N -0.010(2) -0.197(2) 0.1281(17) 0.032(5) Uani 1 1 d . . . . .
N4 N 0.055(2) -0.111(2) 0.1601(16) 0.032(5) Uani 1 1 d . . . . .
C4 C 0.061(3) -0.209(2) 0.0266(19) 0.029(6) Uani 1 1 d . . . . .
O4 O -0.0162(18) -0.2922(17) -0.0084(14) 0.040(4) Uani 1 1 d . . . . .
C5 C 0.063(3) -0.315(3) -0.113(2) 0.051(8) Uani 1 1 d . . . . .
H5A H 0.091604 -0.225768 -0.186697 0.061 Uiso 1 1 calc R U . . .
H5B H -0.010746 -0.366253 -0.139578 0.061 Uiso 1 1 calc R U . . .
C6 C 0.213(3) -0.397(3) -0.073(2) 0.038(6) Uani 1 1 d . . . . .
O5 O 0.3074(19) -0.3964(17) -0.1629(13) 0.047(5) Uani 1 1 d . . . . .
O6 O 0.2274(17) -0.4570(17) 0.0425(14) 0.035(4) Uani 1 1 d . . . . .
O7 O 0.1749(19) 0.3951(16) 0.3141(14) 0.037(4) Uani 1 1 d . . . . .
C7 C 0.068(3) 0.462(3) 0.323(2) 0.037(6) Uiso 1 1 d . . . . .
H7 H 0.083168 0.557665 0.271251 0.045 Uiso 1 1 calc R U . . .
N5 N -0.072(2) 0.425(2) 0.3933(17) 0.043(5) Uiso 1 1 d . . . . .
C8 C -0.108(4) 0.276(4) 0.455(3) 0.089(11) Uiso 1 1 d . . . . .
H8A H -0.222849 0.259370 0.460171 0.133 Uiso 1 1 calc R U . . .
H8B H -0.074474 0.236639 0.540808 0.133 Uiso 1 1 calc R U . . .
H8C H -0.050795 0.232590 0.405750 0.133 Uiso 1 1 calc R U . . .
C9 C -0.198(3) 0.515(3) 0.395(2) 0.049(7) Uiso 1 1 d . . . . .
H9A H -0.153287 0.608032 0.368580 0.074 Uiso 1 1 calc R U . . .
H9B H -0.253212 0.482000 0.480563 0.074 Uiso 1 1 calc R U . . .
H9C H -0.274024 0.518068 0.336016 0.074 Uiso 1 1 calc R U . . .
O8 O 0.4824(16) 0.3108(14) 0.3790(12) 0.027(4) Uani 1 1 d D . . . .
C10 C 0.453(3) 0.257(2) 0.4931(17) 0.041(6) Uiso 1 1 d D . . . .
H10 H 0.495533 0.303667 0.536196 0.049 Uiso 1 1 calc R U . . .
N6 N 0.373(2) 0.1434(19) 0.5648(15) 0.045(5) Uiso 1 1 d D . . . .
C11 C 0.347(3) 0.087(3) 0.7017(17) 0.052(7) Uiso 1 1 d D . . . .
H11A H 0.393882 -0.003642 0.738726 0.078 Uiso 1 1 calc R U . . .
H11B H 0.232340 0.078163 0.728736 0.078 Uiso 1 1 calc R U . . .
H11C H 0.397297 0.148221 0.730236 0.078 Uiso 1 1 calc R U . . .
C12 C 0.306(3) 0.063(3) 0.510(2) 0.053(7) Uiso 1 1 d D . . . .
H12A H 0.324340 0.111203 0.417105 0.079 Uiso 1 1 calc R U . . .
H12B H 0.190725 0.048855 0.535578 0.079 Uiso 1 1 calc R U . . .
H12C H 0.356120 -0.026375 0.538862 0.079 Uiso 1 1 calc R U . . .


_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 O8 2.295(13) . ?
Tb1 O6 2.318(15) 1_565 ?
Tb1 O5 2.367(14) 2_655 ?
Tb1 O2 2.369(15) 2_665 ?
Tb1 O7 2.407(16) . ?
Tb1 O1 2.437(16) . ?
Tb1 O2 2.593(14) . ?
Tb1 Cl2 2.674(6) . ?
Tb1 C1 2.86(3) . ?
Tb1 Tb1 3.972(3) 2_665 ?
O1 C1 1.26(3) . ?
O2 C1 1.24(3) . ?
C1 C2 1.56(4) . ?
C2 O3 1.38(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O3 C3 1.33(3) . ?
C3 N4 1.32(3) . ?
C3 N1 1.33(3) . ?
N1 N2 1.31(3) . ?
N2 C4 1.33(3) . ?
N3 N4 1.30(3) . ?
N3 C4 1.33(3) . ?
C4 O4 1.34(3) . ?
O4 C5 1.46(2) . ?
C5 C6 1.53(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O6 1.24(3) . ?
C6 O5 1.26(3) . ?
O7 C7 1.17(3) . ?
C7 N5 1.33(3) . ?
C7 H7 0.9500 . ?
N5 C9 1.44(3) . ?
N5 C8 1.47(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O8 C10 1.210(16) . ?
C10 N6 1.302(17) . ?
C10 H10 0.9500 . ?
N6 C12 1.440(17) . ?
N6 C11 1.448(17) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

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
O8 Tb1 O6 147.3(5) . 1_565 ?
O8 Tb1 O5 72.3(5) . 2_655 ?
O6 Tb1 O5 136.6(5) 1_565 2_655 ?
O8 Tb1 O2 139.8(5) . 2_665 ?
O6 Tb1 O2 72.2(5) 1_565 2_665 ?
O5 Tb1 O2 75.4(5) 2_655 2_665 ?
O8 Tb1 O7 73.3(5) . . ?
O6 Tb1 O7 75.0(5) 1_565 . ?
O5 Tb1 O7 144.4(5) 2_655 . ?
O2 Tb1 O7 139.5(5) 2_665 . ?
O8 Tb1 O1 79.7(5) . . ?
O6 Tb1 O1 83.7(5) 1_565 . ?
O5 Tb1 O1 91.9(6) 2_655 . ?
O2 Tb1 O1 125.0(5) 2_665 . ?
O7 Tb1 O1 73.2(5) . . ?
O8 Tb1 O2 117.2(5) . . ?
O6 Tb1 O2 71.1(5) 1_565 . ?
O5 Tb1 O2 72.6(5) 2_655 . ?
O2 Tb1 O2 73.7(6) 2_665 . ?
O7 Tb1 O2 116.8(5) . . ?
O1 Tb1 O2 51.6(4) . . ?
O8 Tb1 Cl2 88.0(4) . . ?
O6 Tb1 Cl2 93.3(4) 1_565 . ?
O5 Tb1 Cl2 109.1(5) 2_655 . ?
O2 Tb1 Cl2 80.5(4) 2_665 . ?
O7 Tb1 Cl2 78.3(4) . . ?
O1 Tb1 Cl2 151.2(3) . . ?
O2 Tb1 Cl2 152.9(4) . . ?
O8 Tb1 C1 99.6(6) . . ?
O6 Tb1 C1 75.1(6) 1_565 . ?
O5 Tb1 C1 82.5(7) 2_655 . ?
O2 Tb1 C1 99.2(6) 2_665 . ?
O7 Tb1 C1 94.7(6) . . ?
O1 Tb1 C1 25.9(6) . . ?
O2 Tb1 C1 25.7(5) . . ?
Cl2 Tb1 C1 167.8(5) . . ?
O8 Tb1 Tb1 138.9(3) . 2_665 ?
O6 Tb1 Tb1 66.8(3) 1_565 2_665 ?
O5 Tb1 Tb1 69.8(3) 2_655 2_665 ?
O2 Tb1 Tb1 38.8(3) 2_665 2_665 ?
O7 Tb1 Tb1 138.4(4) . 2_665 ?
O1 Tb1 Tb1 86.4(3) . 2_665 ?
O2 Tb1 Tb1 34.9(3) . 2_665 ?
Cl2 Tb1 Tb1 118.85(14) . 2_665 ?
C1 Tb1 Tb1 60.5(5) . 2_665 ?
C1 O1 Tb1 96.1(14) . . ?
C1 O2 Tb1 162.2(16) . 2_665 ?
C1 O2 Tb1 89.2(13) . . ?
Tb1 O2 Tb1 106.3(6) 2_665 . ?
O2 C1 O1 123(2) . . ?
O2 C1 C2 118(2) . . ?
O1 C1 C2 119(2) . . ?
O2 C1 Tb1 65.1(13) . . ?
O1 C1 Tb1 58.0(12) . . ?
C2 C1 Tb1 176.9(17) . . ?
O3 C2 C1 107.4(18) . . ?
O3 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
O3 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
C3 O3 C2 114.3(18) . . ?
N4 C3 N1 126(2) . . ?
N4 C3 O3 114.0(19) . . ?
N1 C3 O3 120(2) . . ?
N2 N1 C3 118(2) . . ?
N1 N2 C4 115(2) . . ?
N4 N3 C4 116(2) . . ?
N3 N4 C3 117.4(19) . . ?
N2 C4 N3 127(2) . . ?
N2 C4 O4 119(2) . . ?
N3 C4 O4 114(2) . . ?
C4 O4 C5 116.3(19) . . ?
O4 C5 C6 109.6(19) . . ?
O4 C5 H5A 109.7 . . ?
C6 C5 H5A 109.7 . . ?
O4 C5 H5B 109.7 . . ?
C6 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
O6 C6 O5 128(2) . . ?
O6 C6 C5 118(2) . . ?
O5 C6 C5 114(2) . . ?
C6 O5 Tb1 133.1(15) . 2_655 ?
C6 O6 Tb1 140.4(14) . 1_545 ?
C7 O7 Tb1 131.6(16) . . ?
O7 C7 N5 130(3) . . ?
O7 C7 H7 114.9 . . ?
N5 C7 H7 114.9 . . ?
C7 N5 C9 126(2) . . ?
C7 N5 C8 115(2) . . ?
C9 N5 C8 118(2) . . ?
N5 C8 H8A 109.5 . . ?
N5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N5 C9 H9A 109.5 . . ?
N5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10 O8 Tb1 152.3(14) . . ?
O8 C10 N6 129(2) . . ?
O8 C10 H10 115.6 . . ?
N6 C10 H10 115.6 . . ?
C10 N6 C12 120.3(19) . . ?
C10 N6 C11 124(2) . . ?
C12 N6 C11 115(2) . . ?
N6 C11 H11A 109.5 . . ?
N6 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N6 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N6 C12 H12A 109.5 . . ?
N6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_refine_diff_density_max         2.967
_refine_diff_density_min         -3.058
_refine_diff_density_rms         0.322


_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_H2OTz
_database_code_depnum_ccdc_archive 'CCDC 1833260'
_audit_update_record             
;
2018-05-31 deposited with the CCDC.
2018-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            H2OTz
_chemical_melting_point          ?
_chemical_formula_moiety         C6H6N4O6
_chemical_formula_sum            'C6 H6 N4 O6'
_chemical_formula_weight         230.15

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   4.6883(2)
_cell_length_b                   10.7516(5)
_cell_length_c                   8.7635(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.497(3)
_cell_angle_gamma                90
_cell_volume                     439.71(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5154
_cell_measurement_theta_min      3.007
_cell_measurement_theta_max      38.602

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_F_000             236
_exptl_transmission_factor_min   0.6975
_exptl_transmission_factor_max   0.7476
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.157
_shelx_estimated_absorpt_T_min   0.962
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7504
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.007
_diffrn_reflns_theta_max         38.602
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2491
_reflns_number_gt                1784
_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       SAINT
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0773P)²+0.0252P] 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         2491
_refine_ls_number_parameters     76
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1479
_refine_ls_wR_factor_gt          0.1337
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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
O1 O 0.74253(15) 0.04851(7) 1.12587(9) 0.04166(18) Uani 1 1 d . . . . .
H1 H 0.787(3) -0.0117(14) 1.0537(16) 0.050 Uiso 1 1 d . U . . .
O2 O 1.11885(16) 0.14589(6) 1.03864(8) 0.04040(17) Uani 1 1 d . . . . .
C1 C 0.92191(17) 0.14078(8) 1.12005(9) 0.03142(17) Uani 1 1 d . . . . .
C2 C 0.8620(2) 0.24293(8) 1.22998(10) 0.03777(19) Uani 1 1 d . . . . .
H2A H 0.669843 0.274629 1.203694 0.045 Uiso 1 1 calc R U . . .
H2B H 0.870937 0.209355 1.333063 0.045 Uiso 1 1 calc R U . . .
O3 O 1.06298(17) 0.34255(7) 1.22622(7) 0.03985(17) Uani 1 1 d . . . . .
C3 C 1.02609(17) 0.42150(8) 1.10845(9) 0.03160(16) Uani 1 1 d . . . . .
N1 N 0.80968(17) 0.40499(8) 0.99990(9) 0.03703(17) Uani 1 1 d . . . . .
N2 N 0.78261(17) 0.48672(8) 0.88680(8) 0.03803(18) 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
O1 C1 1.3047(11) . ?
O2 C1 1.2210(10) . ?
C1 C2 1.5049(12) . ?
C2 O3 1.4291(12) . ?
O3 C3 1.3347(10) . ?
C3 N2 1.3315(12) 3_767 ?
C3 N1 1.3345(11) . ?
N1 N2 1.3215(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 125.69(8) . . ?
O2 C1 C2 122.63(8) . . ?
O1 C1 C2 111.67(7) . . ?
O3 C2 C1 111.61(7) . . ?
C3 O3 C2 117.23(7) . . ?
N2 C3 N1 125.78(8) 3_767 . ?
N2 C3 O3 114.21(7) 3_767 . ?
N1 C3 O3 120.00(8) . . ?
N2 N1 C3 117.26(8) . . ?
N1 N2 C3 116.96(7) . 3_767 ?

_refine_diff_density_max         0.409
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.052


_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_MIL-166(Tb)
_database_code_depnum_ccdc_archive 'CCDC 1833259'
_audit_update_record             
;
2018-05-31 deposited with the CCDC.
2018-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            Tb(Tz(OCH2CO2)2)1.5(DMF)2
_chemical_melting_point          ?
_chemical_formula_moiety         C15H20N8O11Tb
_chemical_formula_sum            'C15 H20 N8 O11 Tb'
_chemical_formula_weight         647.31

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.177(3)
_cell_length_b                   11.787(4)
_cell_length_c                   12.028(3)
_cell_angle_alpha                113.632(13)
_cell_angle_beta                 92.422(17)
_cell_angle_gamma                102.029(14)
_cell_volume                     1280.0(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8481
_cell_measurement_theta_min      1.946
_cell_measurement_theta_max      26.695

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_F_000             638
_exptl_transmission_factor_min   0.6045
_exptl_transmission_factor_max   0.7454
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    2.828
_shelx_estimated_absorpt_T_min   0.602
_shelx_estimated_absorpt_T_max   0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6045
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9787
_diffrn_reflns_av_unetI/netI     0.3080
_diffrn_reflns_av_R_equivalents  0.1327
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.946
_diffrn_reflns_theta_max         26.695
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measured_fraction_theta_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_point_group_measured_fraction_full 0.956
_reflns_number_total             4966
_reflns_number_gt                2103
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       SAINT
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;The title compound was produced in a two step processes, and only 
small size crystals were obtained. As a consequence, a diffraction dataset
of poor quality was obtained, although sufficient to solve and refine the 
structure reasonnably.,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0384P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4966
_refine_ls_number_parameters     320
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1786
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1403
_refine_ls_wR_factor_gt          0.1053
_refine_ls_goodness_of_fit_ref   0.845
_refine_ls_restrained_S_all      0.845
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb Tb 0.08404(7) 0.09861(6) 0.17631(6) 0.0337(2) Uani 1 1 d . . . . .
O1 O -1.0769(9) -0.2309(7) -0.0706(7) 0.051(3) Uani 1 1 d . . . . .
O2 O -0.9746(8) -0.1231(7) 0.1227(7) 0.039(2) Uani 1 1 d . . . . .
C1 C -1.0179(13) -0.2215(12) 0.0257(11) 0.034(3) Uani 1 1 d . . . . .
C2 C -1.0006(12) -0.3465(11) 0.0244(11) 0.046(4) Uani 1 1 d . . . . .
H2A H -1.087669 -0.395954 0.028786 0.055 Uiso 1 1 calc R U . . .
H2B H -0.971446 -0.395013 -0.052522 0.055 Uiso 1 1 calc R U . . .
O3 O -0.9039(9) -0.3292(7) 0.1238(7) 0.042(2) Uani 1 1 d . . . . .
C3 C -0.7767(14) -0.2719(12) 0.1258(13) 0.044(4) Uani 1 1 d . . . . .
N1 N -0.6080(11) -0.1975(10) 0.0356(8) 0.045(3) Uani 1 1 d . . . . .
N2 N -0.6944(11) -0.2411(10) 0.2290(9) 0.047(3) Uani 1 1 d . . . . .
N3 N -0.5699(11) -0.1804(10) 0.2389(9) 0.051(3) Uani 1 1 d . . . . .
N4 N -0.7361(11) -0.2574(9) 0.0268(9) 0.047(3) Uani 1 1 d . . . . .
C4 C -0.5308(14) -0.1601(12) 0.1412(11) 0.042(4) Uani 1 1 d . . . . .
O4 O -0.4042(9) -0.0924(8) 0.1629(7) 0.054(3) Uani 1 1 d . . . . .
C5 C -0.3493(12) -0.0806(12) 0.0592(10) 0.047(4) Uani 1 1 d . . . . .
H5A H -0.402845 -0.040706 0.024256 0.056 Uiso 1 1 calc R U . . .
H5B H -0.349165 -0.164079 -0.003338 0.056 Uiso 1 1 calc R U . . .
C6 C -0.2069(13) 0.0008(11) 0.1052(12) 0.039(3) Uani 1 1 d . . . . .
O5 O -0.1348(7) 0.0069(7) 0.0223(6) 0.031(2) Uani 1 1 d . . . . .
O6 O -0.1552(9) 0.0522(9) 0.2157(8) 0.061(3) Uani 1 1 d . . . . .
O7 O 0.3136(10) 0.0475(8) 0.2112(8) 0.060(3) Uani 1 1 d . . . . .
O8 O 0.3102(9) 0.2408(8) 0.2369(8) 0.051(3) Uani 1 1 d . . . . .
C7 C 0.3699(15) 0.1613(14) 0.2404(11) 0.044(4) Uani 1 1 d . . . . .
C8 C 0.5236(14) 0.2045(13) 0.2847(13) 0.078(5) Uani 1 1 d . . . . .
H8A H 0.541218 0.188766 0.356455 0.094 Uiso 1 1 calc R U . . .
H8B H 0.569640 0.153945 0.221022 0.094 Uiso 1 1 calc R U . . .
O9 O 0.5775(10) 0.3366(10) 0.3143(10) 0.081(4) Uani 1 1 d . . . . .
C9 C 0.5343(15) 0.4185(17) 0.4102(14) 0.055(4) Uani 1 1 d . . . . .
N5 N 0.4731(14) 0.3788(11) 0.4878(14) 0.068(4) Uani 1 1 d . . . . .
N6 N 0.4376(14) 0.4646(15) 0.5842(13) 0.078(4) Uani 1 1 d . . . . .
O10 O 0.1064(10) 0.0947(8) 0.3691(7) 0.056(3) Uani 1 1 d . . . . .
N7 N 0.2020(13) 0.0341(11) 0.5022(9) 0.064(4) Uani 1 1 d D . . . .
C10 C 0.1442(16) 0.0156(14) 0.3948(11) 0.058(5) Uani 1 1 d . . . . .
H10 H 0.130818 -0.065784 0.332103 0.070 Uiso 1 1 calc R U . . .
C11 C 0.2452(19) -0.0647(15) 0.5265(13) 0.102(7) Uani 1 1 d . . . . .
H11A H 0.216692 -0.063979 0.601793 0.153 Uiso 1 1 calc R U . . .
H11B H 0.342260 -0.048785 0.533214 0.153 Uiso 1 1 calc R U . . .
H11C H 0.205166 -0.146533 0.460534 0.153 Uiso 1 1 calc R U . . .
C12 C 0.230(2) 0.1611(13) 0.6039(13) 0.124(8) Uani 1 1 d D . . . .
H12A H 0.195940 0.217799 0.577498 0.186 Uiso 1 1 calc R U . . .
H12B H 0.325614 0.193183 0.629824 0.186 Uiso 1 1 calc R U . . .
H12C H 0.185185 0.155462 0.671043 0.186 Uiso 1 1 calc R U . . .
O11 O 0.0475(11) 0.2916(10) 0.3166(9) 0.065(3) Uani 1 1 d . . . . .
C13 C -0.0201(18) 0.3608(18) 0.3087(13) 0.073(5) Uani 1 1 d . . . . .
H13 H -0.109596 0.321118 0.272331 0.087 Uiso 1 1 calc R U . . .
N8 N 0.0165(15) 0.4883(12) 0.3455(11) 0.062(4) Uani 1 1 d D . . . .
C15 C -0.075(2) 0.5640(17) 0.3357(16) 0.130(9) Uani 1 1 d D . . . .
H15A H -0.160645 0.508343 0.289770 0.195 Uiso 1 1 calc R U . . .
H15B H -0.036714 0.615447 0.294729 0.195 Uiso 1 1 calc R U . . .
H15C H -0.089315 0.618468 0.416276 0.195 Uiso 1 1 calc R U . . .
C14 C 0.160(2) 0.547(2) 0.384(2) 0.157(10) Uani 1 1 d . . . . .
H14A H 0.207908 0.483170 0.376300 0.235 Uiso 1 1 calc R U . . .
H14B H 0.174674 0.609195 0.467411 0.235 Uiso 1 1 calc R U . . .
H14C H 0.192882 0.589053 0.332534 0.235 Uiso 1 1 calc R U . . .


_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
Tb O10 2.340(8) . ?
Tb O11 2.342(11) . ?
Tb O5 2.348(7) 2 ?
Tb O2 2.360(7) 1_655 ?
Tb O1 2.384(8) 2_455 ?
Tb O8 2.431(8) . ?
Tb O6 2.490(9) . ?
Tb O5 2.569(7) . ?
Tb O7 2.589(10) . ?
Tb C7 2.840(15) . ?
Tb C6 2.898(13) . ?
Tb Tb 4.0179(16) 2 ?
O1 C1 1.235(12) . ?
O2 C1 1.249(12) . ?
C1 C2 1.514(15) . ?
C2 O3 1.435(13) . ?
O3 C3 1.324(14) . ?
C3 N4 1.338(14) . ?
C3 N2 1.342(14) . ?
N1 C4 1.322(14) . ?
N1 N4 1.324(13) . ?
N2 N3 1.293(12) . ?
N3 C4 1.350(13) . ?
C4 O4 1.319(13) . ?
O4 C5 1.433(11) . ?
C5 C6 1.501(15) . ?
C6 O6 1.254(13) . ?
C6 O5 1.278(13) . ?
O7 C7 1.239(14) . ?
O8 C7 1.232(15) . ?
C7 C8 1.539(18) . ?
C8 O9 1.427(15) . ?
O9 C9 1.335(15) . ?
C9 N6 1.321(18) 2_666 ?
C9 N5 1.326(17) . ?
N5 N6 1.320(16) . ?
O10 C10 1.218(15) . ?
N7 C10 1.312(15) . ?
N7 C11 1.452(16) . ?
N7 C12 1.464(13) . ?
O11 C13 1.199(18) . ?
C13 N8 1.346(17) . ?
N8 C14 1.45(2) . ?
N8 C15 1.452(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Tb O11 73.6(3) . . ?
O10 Tb O5 140.1(3) . 2 ?
O11 Tb O5 144.0(3) . 2 ?
O10 Tb O2 78.6(3) . 1_655 ?
O11 Tb O2 141.8(3) . 1_655 ?
O5 Tb O2 71.7(3) 2 1_655 ?
O10 Tb O1 144.9(3) . 2_455 ?
O11 Tb O1 72.6(3) . 2_455 ?
O5 Tb O1 71.7(3) 2 2_455 ?
O2 Tb O1 135.6(3) 1_655 2_455 ?
O10 Tb O8 87.0(3) . . ?
O11 Tb O8 77.1(3) . . ?
O5 Tb O8 90.3(3) 2 . ?
O2 Tb O8 127.4(3) 1_655 . ?
O1 Tb O8 76.8(3) 2_455 . ?
O10 Tb O6 76.9(3) . . ?
O11 Tb O6 73.2(3) . . ?
O5 Tb O6 118.9(3) 2 . ?
O2 Tb O6 75.4(3) 1_655 . ?
O1 Tb O6 101.7(3) 2_455 . ?
O8 Tb O6 149.1(3) . . ?
O10 Tb O5 125.8(3) . . ?
O11 Tb O5 101.8(3) . . ?
O5 Tb O5 70.5(3) 2 . ?
O2 Tb O5 74.0(3) 1_655 . ?
O1 Tb O5 70.7(2) 2_455 . ?
O8 Tb O5 146.1(3) . . ?
O6 Tb O5 51.5(2) . . ?
O10 Tb O7 71.5(3) . . ?
O11 Tb O7 117.7(3) . . ?
O5 Tb O7 75.9(3) 2 . ?
O2 Tb O7 76.1(3) 1_655 . ?
O1 Tb O7 117.5(3) 2_455 . ?
O8 Tb O7 51.4(3) . . ?
O6 Tb O7 140.8(3) . . ?
O5 Tb O7 140.4(3) . . ?
O10 Tb C7 77.5(4) . . ?
O11 Tb C7 97.1(4) . . ?
O5 Tb C7 83.2(3) 2 . ?
O2 Tb C7 102.0(4) 1_655 . ?
O1 Tb C7 97.8(4) 2_455 . ?
O8 Tb C7 25.6(3) . . ?
O6 Tb C7 154.2(3) . . ?
O5 Tb C7 153.4(3) . . ?
O7 Tb C7 25.9(3) . . ?
O10 Tb C6 100.4(3) . . ?
O11 Tb C6 89.1(4) . . ?
O5 Tb C6 94.3(3) 2 . ?
O2 Tb C6 70.5(3) 1_655 . ?
O1 Tb C6 88.0(3) 2_455 . ?
O8 Tb C6 161.9(3) . . ?
O6 Tb C6 25.5(3) . . ?
O5 Tb C6 26.2(3) . . ?
O7 Tb C6 146.6(3) . . ?
C7 Tb C6 172.5(4) . . ?
O10 Tb Tb 145.3(2) . 2 ?
O11 Tb Tb 127.1(3) . 2 ?
O5 Tb Tb 37.07(18) 2 2 ?
O2 Tb Tb 68.91(18) 1_655 2 ?
O1 Tb Tb 66.78(18) 2_455 2 ?
O8 Tb Tb 122.3(2) . 2 ?
O6 Tb Tb 83.33(19) . 2 ?
O5 Tb Tb 33.42(16) . 2 ?
O7 Tb Tb 110.50(19) . 2 ?
C7 Tb Tb 120.2(2) . 2 ?
C6 Tb Tb 58.0(3) . 2 ?
C1 O1 Tb 137.5(8) . 2_455 ?
C1 O2 Tb 135.4(7) . 1_455 ?
O1 C1 O2 127.9(12) . . ?
O1 C1 C2 114.7(11) . . ?
O2 C1 C2 117.3(10) . . ?
O3 C2 C1 113.0(9) . . ?
C3 O3 C2 116.8(9) . . ?
O3 C3 N4 120.6(12) . . ?
O3 C3 N2 114.5(11) . . ?
N4 C3 N2 124.7(12) . . ?
C4 N1 N4 116.5(10) . . ?
N3 N2 C3 117.6(10) . . ?
N2 N3 C4 117.3(10) . . ?
N1 N4 C3 117.6(11) . . ?
O4 C4 N1 121.7(11) . . ?
O4 C4 N3 112.3(11) . . ?
N1 C4 N3 125.9(12) . . ?
C4 O4 C5 115.8(9) . . ?
O4 C5 C6 106.5(9) . . ?
O6 C6 O5 120.4(11) . . ?
O6 C6 C5 123.9(12) . . ?
O5 C6 C5 115.4(10) . . ?
O6 C6 Tb 58.8(7) . . ?
O5 C6 Tb 62.4(6) . . ?
C5 C6 Tb 166.1(9) . . ?
C6 O5 Tb 147.2(7) . 2 ?
C6 O5 Tb 91.4(6) . . ?
Tb O5 Tb 109.5(3) 2 . ?
C6 O6 Tb 95.7(8) . . ?
C7 O7 Tb 88.4(9) . . ?
C7 O8 Tb 96.1(8) . . ?
O8 C7 O7 123.9(14) . . ?
O8 C7 C8 118.8(13) . . ?
O7 C7 C8 117.3(14) . . ?
O8 C7 Tb 58.3(7) . . ?
O7 C7 Tb 65.7(8) . . ?
C8 C7 Tb 175.3(9) . . ?
O9 C8 C7 112.3(13) . . ?
C9 O9 C8 115.8(13) . . ?
N6 C9 N5 127.5(15) 2_666 . ?
N6 C9 O9 112.5(18) 2_666 . ?
N5 C9 O9 120.0(19) . . ?
N6 N5 C9 117.7(13) . . ?
N5 N6 C9 114.8(13) . 2_666 ?
C10 O10 Tb 127.3(8) . . ?
C10 N7 C11 123.5(12) . . ?
C10 N7 C12 119.5(12) . . ?
C11 N7 C12 116.9(11) . . ?
O10 C10 N7 126.4(13) . . ?
C13 O11 Tb 133.2(10) . . ?
O11 C13 N8 128.6(17) . . ?
C13 N8 C14 115.8(16) . . ?
C13 N8 C15 124.2(16) . . ?
C14 N8 C15 119.6(14) . . ?

_refine_diff_density_max         1.390
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.203



_exptl_crystal_preparation       Luminescent
