# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010


data_global

_journal_coden_Cambridge         222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Jan Reedijk'
'Wen-Tian Fu'
'Patrick Gamez'
'Marta Kasunic'
'Bojan Kozlevcar'
'Tiddo Jonathan Mooibroek'
'Andrej Pevec'

_publ_contact_author_name        'Jan Reedijk'
_publ_contact_author_email       REEDIJK@CHEM.LEIDENUNIV.NL

_publ_section_title              
;
Efficient, stable, tunable, and easy to synthesize,
handle and recycle luminescent materials:
[H2NMe2]3[Ln(III)(2,6-dipicolinolate)3]
(Ln = Eu, Tb, or its solid solutions)
;

# Attachment 'k982zakEU.cif'

data_k982
_database_code_depnum_ccdc_archive 'CCDC 761087'
#TrackingRef 'k982zakEU.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H33 Eu N6 O12'
_chemical_formula_weight         785.55

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'

_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                   12.0026(2)
_cell_length_b                   12.0692(2)
_cell_length_c                   12.4073(2)
_cell_angle_alpha                78.6380(7)
_cell_angle_beta                 69.8886(7)
_cell_angle_gamma                72.6756(8)
_cell_volume                     1602.19(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6135
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_absorpt_coefficient_mu    2.027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7508
_exptl_absorpt_correction_T_max  0.8880
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'

_exptl_special_details           
;
203 frames in 4 sets of \w scans. Rotation/frame = 2 \%.
Crystal-detector distance = 30 mm. Measuring time = 600 s/\%.
;

_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  
;
Nonius KappaCCD area-detector diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11707
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.44
_diffrn_reflns_theta_max         27.00
_reflns_number_total             6922
_reflns_number_gt                6214
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'KappaCCD Reference Manual (Nonius, 1998)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0122P)^2^+1.4003P] where P=(Fo^2^+2Fc^2^)/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         6922
_refine_ls_number_parameters     439
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0649
_refine_ls_wR_factor_gt          0.0616
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.0001

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
Eu1 Eu 0.227509(12) 0.263099(12) 0.231053(12) 0.03033(6) Uani 1 1 d . . .
O1 O 0.1416(2) 0.47107(18) 0.22304(19) 0.0418(5) Uani 1 1 d . . .
O2 O 0.2744(2) 0.13258(18) 0.39920(19) 0.0445(5) Uani 1 1 d . . .
O3 O 0.0906(3) 0.6442(2) 0.2880(2) 0.0637(7) Uani 1 1 d . . .
O4 O 0.2826(3) 0.1001(2) 0.5796(2) 0.0672(8) Uani 1 1 d . . .
O5 O 0.29824(18) 0.3168(2) 0.02270(18) 0.0408(5) Uani 1 1 d . . .
O6 O 0.02431(19) 0.24369(19) 0.34852(18) 0.0403(5) Uani 1 1 d . . .
O7 O 0.2694(2) 0.3717(2) -0.14984(19) 0.0533(6) Uani 1 1 d . . .
O8 O -0.1665(2) 0.2395(3) 0.3695(2) 0.0621(7) Uani 1 1 d . . .
O9 O 0.41097(18) 0.32958(18) 0.20296(19) 0.0418(5) Uani 1 1 d . . .
O10 O 0.22459(19) 0.07093(18) 0.19362(19) 0.0412(5) Uani 1 1 d . . .
O11 O 0.6114(2) 0.3137(2) 0.1271(3) 0.0661(8) Uani 1 1 d . . .
O12 O 0.3122(2) -0.1191(2) 0.1825(2) 0.0588(7) Uani 1 1 d . . .
N1 N 0.1938(2) 0.3592(2) 0.4093(2) 0.0337(5) Uani 1 1 d . . .
N2 N 0.0727(2) 0.3014(2) 0.1244(2) 0.0319(5) Uani 1 1 d . . .
N3 N 0.4348(2) 0.1176(2) 0.1597(2) 0.0344(5) Uani 1 1 d . . .
C1 C 0.1273(3) 0.5366(3) 0.2967(3) 0.0385(7) Uani 1 1 d . . .
C2 C 0.1568(3) 0.4754(3) 0.4063(3) 0.0358(6) Uani 1 1 d . . .
C3 C 0.1483(3) 0.5323(3) 0.4966(3) 0.0480(8) Uani 1 1 d . . .
H3 H 0.1224 0.6133 0.4934 0.058 Uiso 1 1 calc R . .
C4 C 0.1788(3) 0.4666(3) 0.5915(3) 0.0543(9) Uani 1 1 d . . .
H4 H 0.1744 0.5031 0.6527 0.065 Uiso 1 1 calc R . .
C5 C 0.2157(3) 0.3464(3) 0.5951(3) 0.0504(8) Uani 1 1 d . . .
H5 H 0.2358 0.3009 0.6588 0.060 Uiso 1 1 calc R . .
C6 C 0.2223(3) 0.2953(3) 0.5015(3) 0.0384(7) Uani 1 1 d . . .
C7 C 0.2622(3) 0.1657(3) 0.4939(3) 0.0431(7) Uani 1 1 d . . .
C8 C 0.2335(3) 0.3418(3) -0.0432(3) 0.0374(7) Uani 1 1 d . . .
C9 C 0.1023(3) 0.3333(3) 0.0109(3) 0.0362(6) Uani 1 1 d . . .
C10 C 0.0184(3) 0.3563(3) -0.0495(3) 0.0504(8) Uani 1 1 d . . .
H10 H 0.0407 0.3787 -0.1285 0.060 Uiso 1 1 calc R . .
C11 C -0.0990(3) 0.3451(4) 0.0104(3) 0.0588(10) Uani 1 1 d . . .
H11 H -0.1573 0.3606 -0.0278 0.071 Uiso 1 1 calc R . .
C12 C -0.1289(3) 0.3110(3) 0.1271(3) 0.0521(9) Uani 1 1 d . . .
H12 H -0.2070 0.3017 0.1684 0.063 Uiso 1 1 calc R . .
C13 C -0.0408(3) 0.2905(3) 0.1825(3) 0.0356(6) Uani 1 1 d . . .
C14 C -0.0637(3) 0.2545(3) 0.3108(3) 0.0384(7) Uani 1 1 d . . .
C15 C 0.5193(3) 0.2743(3) 0.1566(3) 0.0424(7) Uani 1 1 d . . .
C16 C 0.5381(3) 0.1495(3) 0.1382(3) 0.0395(7) Uani 1 1 d . . .
C17 C 0.6515(3) 0.0708(3) 0.1061(3) 0.0533(9) Uani 1 1 d . . .
H17 H 0.7230 0.0947 0.0891 0.064 Uiso 1 1 calc R . .
C18 C 0.6570(3) -0.0426(3) 0.0995(3) 0.0543(9) Uani 1 1 d . . .
H18 H 0.7322 -0.0969 0.0795 0.065 Uiso 1 1 calc R . .
C19 C 0.5497(3) -0.0757(3) 0.1229(3) 0.0466(8) Uani 1 1 d . . .
H19 H 0.5513 -0.1525 0.1196 0.056 Uiso 1 1 calc R . .
C20 C 0.4396(3) 0.0080(3) 0.1514(2) 0.0365(6) Uani 1 1 d . . .
C21 C 0.3158(3) -0.0159(3) 0.1773(3) 0.0380(7) Uani 1 1 d . . .
N4 N 0.0730(3) -0.1262(3) 0.2706(3) 0.0583(8) Uani 1 1 d D . .
H1N H 0.151(2) -0.122(4) 0.235(3) 0.070 Uiso 1 1 d D . .
H2N H 0.071(4) -0.2006(19) 0.283(3) 0.070 Uiso 1 1 d D . .
N5 N 0.5324(3) 0.5368(3) 0.1901(4) 0.0731(11) Uani 1 1 d D . .
H3N H 0.595(3) 0.571(4) 0.168(4) 0.088 Uiso 1 1 d D . .
H4N H 0.565(4) 0.468(2) 0.161(4) 0.088 Uiso 1 1 d D . .
N6 N -0.3476(3) 0.1275(3) 0.4688(3) 0.0497(7) Uani 1 1 d D . .
H5N H -0.280(2) 0.153(3) 0.439(3) 0.060 Uiso 1 1 d D . .
H6N H -0.321(3) 0.0500(17) 0.470(3) 0.060 Uiso 1 1 d D . .
C22 C 0.0297(4) -0.0792(4) 0.3833(4) 0.0745(12) Uani 1 1 d . . .
H22A H 0.0300 0.0017 0.3711 0.112 Uiso 1 1 calc R . .
H22B H 0.0831 -0.1217 0.4282 0.112 Uiso 1 1 calc R . .
H22C H -0.0520 -0.0872 0.4236 0.112 Uiso 1 1 calc R . .
C23 C 0.0013(5) -0.0612(5) 0.1937(5) 0.0917(15) Uani 1 1 d . . .
H23A H -0.0833 -0.0616 0.2304 0.138 Uiso 1 1 calc R . .
H23B H 0.0312 -0.0971 0.1232 0.138 Uiso 1 1 calc R . .
H23C H 0.0089 0.0178 0.1768 0.138 Uiso 1 1 calc R . .
C24 C 0.4857(8) 0.5229(7) 0.3165(5) 0.139(3) Uani 1 1 d . . .
H24A H 0.4342 0.5960 0.3434 0.208 Uiso 1 1 calc R . .
H24B H 0.5532 0.4983 0.3476 0.208 Uiso 1 1 calc R . .
H24C H 0.4391 0.4652 0.3411 0.208 Uiso 1 1 calc R . .
C25 C 0.4404(5) 0.6014(4) 0.1325(6) 0.109(2) Uani 1 1 d . . .
H25A H 0.3735 0.5649 0.1575 0.164 Uiso 1 1 calc R . .
H25B H 0.4768 0.6013 0.0504 0.164 Uiso 1 1 calc R . .
H25C H 0.4107 0.6804 0.1518 0.164 Uiso 1 1 calc R . .
C26 C -0.4193(8) 0.1599(6) 0.5827(5) 0.139(3) Uani 1 1 d . . .
H26A H -0.4680 0.2387 0.5770 0.208 Uiso 1 1 calc R . .
H26B H -0.3657 0.1542 0.6269 0.208 Uiso 1 1 calc R . .
H26C H -0.4721 0.1085 0.6200 0.208 Uiso 1 1 calc R . .
C27 C -0.4188(6) 0.1649(6) 0.3901(6) 0.119(2) Uani 1 1 d . . .
H27A H -0.4924 0.1381 0.4223 0.179 Uiso 1 1 calc R . .
H27B H -0.3720 0.1331 0.3182 0.179 Uiso 1 1 calc R . .
H27C H -0.4397 0.2486 0.3772 0.179 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Eu1 0.02770(8) 0.02669(8) 0.03815(9) -0.00627(5) -0.01038(6) -0.00678(5)
O1 0.0499(13) 0.0297(11) 0.0480(12) -0.0043(9) -0.0219(10) -0.0046(9)
O2 0.0552(14) 0.0310(11) 0.0476(13) -0.0053(9) -0.0198(10) -0.0058(10)
O3 0.086(2) 0.0266(12) 0.0806(18) -0.0063(12) -0.0343(15) -0.0065(12)
O4 0.101(2) 0.0486(15) 0.0556(16) 0.0083(12) -0.0412(15) -0.0131(15)
O5 0.0320(11) 0.0489(13) 0.0428(12) -0.0061(10) -0.0103(9) -0.0124(9)
O6 0.0377(12) 0.0436(12) 0.0390(11) -0.0049(9) -0.0091(9) -0.0122(9)
O7 0.0540(14) 0.0668(17) 0.0404(13) 0.0021(11) -0.0104(11) -0.0267(13)
O8 0.0393(13) 0.082(2) 0.0632(16) -0.0009(14) -0.0022(11) -0.0332(13)
O9 0.0322(11) 0.0347(11) 0.0621(14) -0.0141(10) -0.0135(10) -0.0088(9)
O10 0.0369(11) 0.0318(11) 0.0569(13) -0.0109(10) -0.0126(10) -0.0094(9)
O11 0.0336(13) 0.0538(16) 0.116(2) -0.0183(15) -0.0190(13) -0.0161(11)
O12 0.0576(15) 0.0321(12) 0.0867(18) -0.0179(12) -0.0127(13) -0.0144(11)
N1 0.0291(12) 0.0310(13) 0.0408(13) -0.0072(10) -0.0096(10) -0.0065(10)
N2 0.0301(12) 0.0276(12) 0.0388(13) -0.0050(10) -0.0100(10) -0.0077(9)
N3 0.0323(12) 0.0336(13) 0.0374(13) -0.0062(10) -0.0093(10) -0.0081(10)
C1 0.0333(15) 0.0267(15) 0.0533(19) -0.0034(13) -0.0127(13) -0.0053(12)
C2 0.0309(15) 0.0307(15) 0.0452(17) -0.0088(13) -0.0073(12) -0.0086(12)
C3 0.051(2) 0.0384(18) 0.055(2) -0.0195(15) -0.0100(15) -0.0088(15)
C4 0.061(2) 0.059(2) 0.047(2) -0.0237(17) -0.0136(16) -0.0124(18)
C5 0.055(2) 0.055(2) 0.0411(18) -0.0093(15) -0.0162(15) -0.0099(17)
C6 0.0363(16) 0.0405(17) 0.0391(16) -0.0061(13) -0.0113(12) -0.0095(13)
C7 0.0464(18) 0.0365(17) 0.0482(19) 0.0013(14) -0.0195(15) -0.0107(14)
C8 0.0393(16) 0.0323(15) 0.0405(17) -0.0043(13) -0.0092(13) -0.0118(13)
C9 0.0363(16) 0.0308(15) 0.0450(17) -0.0051(13) -0.0154(13) -0.0090(12)
C10 0.051(2) 0.056(2) 0.0489(19) 0.0008(16) -0.0263(16) -0.0125(16)
C11 0.045(2) 0.074(3) 0.069(2) -0.003(2) -0.0337(18) -0.0160(18)
C12 0.0342(17) 0.063(2) 0.063(2) -0.0040(18) -0.0185(15) -0.0152(16)
C13 0.0295(14) 0.0319(15) 0.0478(17) -0.0050(13) -0.0127(12) -0.0094(12)
C14 0.0341(16) 0.0321(15) 0.0477(18) -0.0083(13) -0.0069(13) -0.0103(12)
C15 0.0329(16) 0.0398(17) 0.059(2) -0.0073(15) -0.0163(14) -0.0110(13)
C16 0.0316(15) 0.0376(17) 0.0486(18) -0.0089(14) -0.0099(13) -0.0077(12)
C17 0.0329(17) 0.053(2) 0.070(2) -0.0139(18) -0.0094(15) -0.0072(15)
C18 0.0379(18) 0.046(2) 0.069(2) -0.0188(17) -0.0080(16) 0.0030(15)
C19 0.0476(19) 0.0342(17) 0.0507(19) -0.0114(14) -0.0106(15) -0.0003(14)
C20 0.0408(16) 0.0304(15) 0.0361(15) -0.0070(12) -0.0082(12) -0.0078(12)
C21 0.0448(17) 0.0326(16) 0.0388(16) -0.0094(13) -0.0106(13) -0.0119(13)
N4 0.0539(19) 0.0336(16) 0.086(2) -0.0026(16) -0.0170(17) -0.0162(14)
N5 0.058(2) 0.052(2) 0.106(3) -0.025(2) 0.001(2) -0.0288(18)
N6 0.0446(17) 0.0435(16) 0.0610(19) 0.0021(14) -0.0152(14) -0.0168(14)
C22 0.078(3) 0.066(3) 0.072(3) -0.007(2) -0.006(2) -0.027(2)
C23 0.095(4) 0.078(3) 0.109(4) -0.002(3) -0.047(3) -0.018(3)
C24 0.171(7) 0.151(6) 0.101(5) -0.052(4) 0.024(5) -0.101(6)
C25 0.080(4) 0.047(3) 0.195(7) 0.001(3) -0.042(4) -0.017(2)
C26 0.220(9) 0.121(6) 0.056(3) -0.015(3) -0.014(4) -0.043(6)
C27 0.125(5) 0.132(6) 0.139(5) 0.009(4) -0.094(5) -0.039(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.409(2) . ?
Eu1 O6 2.427(2) . ?
Eu1 O5 2.446(2) . ?
Eu1 O9 2.455(2) . ?
Eu1 O10 2.466(2) . ?
Eu1 O2 2.477(2) . ?
Eu1 N2 2.521(2) . ?
Eu1 N1 2.552(2) . ?
Eu1 N3 2.559(2) . ?
O1 C1 1.260(4) . ?
O2 C7 1.262(4) . ?
O3 C1 1.237(4) . ?
O4 C7 1.244(4) . ?
O5 C8 1.251(4) . ?
O6 C14 1.259(4) . ?
O7 C8 1.256(4) . ?
O8 C14 1.245(4) . ?
O9 C15 1.259(4) . ?
O10 C21 1.259(4) . ?
O11 C15 1.245(4) . ?
O12 C21 1.248(4) . ?
N1 C2 1.336(4) . ?
N1 C6 1.336(4) . ?
N2 C9 1.334(4) . ?
N2 C13 1.337(4) . ?
N3 C20 1.329(4) . ?
N3 C16 1.332(4) . ?
C1 C2 1.516(5) . ?
C2 C3 1.387(4) . ?
C3 C4 1.379(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.388(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.505(4) . ?
C8 C9 1.511(4) . ?
C9 C10 1.386(4) . ?
C10 C11 1.382(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.374(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.389(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.515(4) . ?
C15 C16 1.506(4) . ?
C16 C17 1.386(5) . ?
C17 C18 1.368(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.381(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.384(4) . ?
C19 H19 0.9300 . ?
C20 C21 1.511(4) . ?
N4 C23 1.461(6) . ?
N4 C22 1.477(6) . ?
N4 H1N 0.900(19) . ?
N4 H2N 0.887(19) . ?
N5 C25 1.466(7) . ?
N5 C24 1.466(7) . ?
N5 H3N 0.905(19) . ?
N5 H4N 0.898(19) . ?
N6 C27 1.435(6) . ?
N6 C26 1.439(6) . ?
N6 H5N 0.891(18) . ?
N6 H6N 0.893(19) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 O6 86.82(8) . . ?
O1 Eu1 O5 79.82(7) . . ?
O6 Eu1 O5 127.60(7) . . ?
O1 Eu1 O9 79.91(8) . . ?
O6 Eu1 O9 150.01(7) . . ?
O5 Eu1 O9 76.46(7) . . ?
O1 Eu1 O10 148.61(8) . . ?
O6 Eu1 O10 76.80(7) . . ?
O5 Eu1 O10 89.13(7) . . ?
O9 Eu1 O10 126.10(7) . . ?
O1 Eu1 O2 126.31(7) . . ?
O6 Eu1 O2 79.21(8) . . ?
O5 Eu1 O2 146.45(8) . . ?
O9 Eu1 O2 87.17(8) . . ?
O10 Eu1 O2 77.06(8) . . ?
O1 Eu1 N2 75.25(7) . . ?
O6 Eu1 N2 64.23(8) . . ?
O5 Eu1 N2 63.38(7) . . ?
O9 Eu1 N2 135.57(8) . . ?
O10 Eu1 N2 73.54(7) . . ?
O2 Eu1 N2 137.10(8) . . ?
O1 Eu1 N1 63.44(8) . . ?
O6 Eu1 N1 77.92(7) . . ?
O5 Eu1 N1 134.76(8) . . ?
O9 Eu1 N1 72.10(7) . . ?
O10 Eu1 N1 135.83(8) . . ?
O2 Eu1 N1 62.99(8) . . ?
N2 Eu1 N1 124.75(7) . . ?
O1 Eu1 N3 139.10(8) . . ?
O6 Eu1 N3 134.05(8) . . ?
O5 Eu1 N3 75.10(8) . . ?
O9 Eu1 N3 63.20(8) . . ?
O10 Eu1 N3 62.91(7) . . ?
O2 Eu1 N3 71.38(8) . . ?
N2 Eu1 N3 119.09(8) . . ?
N1 Eu1 N3 116.17(8) . . ?
C1 O1 Eu1 126.8(2) . . ?
C7 O2 Eu1 125.1(2) . . ?
C8 O5 Eu1 125.36(18) . . ?
C14 O6 Eu1 125.28(19) . . ?
C15 O9 Eu1 124.78(19) . . ?
C21 O10 Eu1 124.44(19) . . ?
C2 N1 C6 119.9(3) . . ?
C2 N1 Eu1 119.3(2) . . ?
C6 N1 Eu1 120.58(19) . . ?
C9 N2 C13 119.6(3) . . ?
C9 N2 Eu1 120.92(18) . . ?
C13 N2 Eu1 119.51(19) . . ?
C20 N3 C16 119.8(3) . . ?
C20 N3 Eu1 120.13(19) . . ?
C16 N3 Eu1 119.97(19) . . ?
O3 C1 O1 126.1(3) . . ?
O3 C1 C2 118.1(3) . . ?
O1 C1 C2 115.7(3) . . ?
N1 C2 C3 121.5(3) . . ?
N1 C2 C1 114.2(2) . . ?
C3 C2 C1 124.3(3) . . ?
C4 C3 C2 118.7(3) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 119.8(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C4 C5 C6 118.4(3) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
N1 C6 C5 121.7(3) . . ?
N1 C6 C7 114.4(3) . . ?
C5 C6 C7 123.8(3) . . ?
O4 C7 O2 125.3(3) . . ?
O4 C7 C6 118.1(3) . . ?
O2 C7 C6 116.6(3) . . ?
O5 C8 O7 125.2(3) . . ?
O5 C8 C9 116.6(3) . . ?
O7 C8 C9 118.2(3) . . ?
N2 C9 C10 122.0(3) . . ?
N2 C9 C8 113.7(3) . . ?
C10 C9 C8 124.3(3) . . ?
C11 C10 C9 118.5(3) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C12 C11 C10 119.4(3) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 119.2(3) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
N2 C13 C12 121.3(3) . . ?
N2 C13 C14 114.8(3) . . ?
C12 C13 C14 123.9(3) . . ?
O8 C14 O6 125.8(3) . . ?
O8 C14 C13 118.1(3) . . ?
O6 C14 C13 116.1(2) . . ?
O11 C15 O9 125.4(3) . . ?
O11 C15 C16 117.8(3) . . ?
O9 C15 C16 116.8(3) . . ?
N3 C16 C17 121.3(3) . . ?
N3 C16 C15 114.3(3) . . ?
C17 C16 C15 124.4(3) . . ?
C18 C17 C16 119.2(3) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 119.4(3) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C18 C19 C20 118.5(3) . . ?
C18 C19 H19 120.8 . . ?
C20 C19 H19 120.8 . . ?
N3 C20 C19 121.8(3) . . ?
N3 C20 C21 114.2(3) . . ?
C19 C20 C21 123.9(3) . . ?
O12 C21 O10 125.6(3) . . ?
O12 C21 C20 117.8(3) . . ?
O10 C21 C20 116.5(3) . . ?
C23 N4 C22 113.0(4) . . ?
C23 N4 H1N 107(3) . . ?
C22 N4 H1N 109(3) . . ?
C23 N4 H2N 110(3) . . ?
C22 N4 H2N 108(3) . . ?
H1N N4 H2N 109(4) . . ?
C25 N5 C24 114.8(5) . . ?
C25 N5 H3N 110(3) . . ?
C24 N5 H3N 109(3) . . ?
C25 N5 H4N 106(3) . . ?
C24 N5 H4N 112(3) . . ?
H3N N5 H4N 105(4) . . ?
C27 N6 C26 111.6(5) . . ?
C27 N6 H5N 110(3) . . ?
C26 N6 H5N 114(2) . . ?
C27 N6 H6N 107(3) . . ?
C26 N6 H6N 110(2) . . ?
H5N N6 H6N 104(4) . . ?
N4 C22 H22A 109.5 . . ?
N4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 H23A 109.5 . . ?
N4 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N4 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N5 C24 H24A 109.5 . . ?
N5 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N5 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N5 C25 H25A 109.5 . . ?
N5 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N5 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N6 C26 H26A 109.5 . . ?
N6 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N6 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N6 C27 H27A 109.5 . . ?
N6 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N6 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 Eu1 O1 C1 84.5(2) . . . . ?
O5 Eu1 O1 C1 -146.4(2) . . . . ?
O9 Eu1 O1 C1 -68.5(2) . . . . ?
O10 Eu1 O1 C1 142.5(2) . . . . ?
O2 Eu1 O1 C1 10.4(3) . . . . ?
N2 Eu1 O1 C1 148.7(2) . . . . ?
N1 Eu1 O1 C1 6.4(2) . . . . ?
N3 Eu1 O1 C1 -93.7(3) . . . . ?
O1 Eu1 O2 C7 -3.5(3) . . . . ?
O6 Eu1 O2 C7 -81.4(2) . . . . ?
O5 Eu1 O2 C7 131.8(2) . . . . ?
O9 Eu1 O2 C7 71.8(2) . . . . ?
O10 Eu1 O2 C7 -160.2(3) . . . . ?
N2 Eu1 O2 C7 -112.6(2) . . . . ?
N1 Eu1 O2 C7 0.4(2) . . . . ?
N3 Eu1 O2 C7 134.4(3) . . . . ?
O1 Eu1 O5 C8 -76.5(2) . . . . ?
O6 Eu1 O5 C8 1.4(3) . . . . ?
O9 Eu1 O5 C8 -158.5(2) . . . . ?
O10 Eu1 O5 C8 73.9(2) . . . . ?
O2 Eu1 O5 C8 138.6(2) . . . . ?
N2 Eu1 O5 C8 2.0(2) . . . . ?
N1 Eu1 O5 C8 -111.7(2) . . . . ?
N3 Eu1 O5 C8 136.1(2) . . . . ?
O1 Eu1 O6 C14 78.2(2) . . . . ?
O5 Eu1 O6 C14 3.7(3) . . . . ?
O9 Eu1 O6 C14 141.7(2) . . . . ?
O10 Eu1 O6 C14 -74.8(2) . . . . ?
O2 Eu1 O6 C14 -153.9(2) . . . . ?
N2 Eu1 O6 C14 3.1(2) . . . . ?
N1 Eu1 O6 C14 141.7(2) . . . . ?
N3 Eu1 O6 C14 -103.4(2) . . . . ?
O1 Eu1 O9 C15 -153.6(3) . . . . ?
O6 Eu1 O9 C15 141.3(2) . . . . ?
O5 Eu1 O9 C15 -71.7(3) . . . . ?
O10 Eu1 O9 C15 7.0(3) . . . . ?
O2 Eu1 O9 C15 78.8(3) . . . . ?
N2 Eu1 O9 C15 -97.0(3) . . . . ?
N1 Eu1 O9 C15 141.3(3) . . . . ?
N3 Eu1 O9 C15 8.2(2) . . . . ?
O1 Eu1 O10 C21 154.8(2) . . . . ?
O6 Eu1 O10 C21 -144.7(2) . . . . ?
O5 Eu1 O10 C21 86.2(2) . . . . ?
O9 Eu1 O10 C21 13.7(3) . . . . ?
O2 Eu1 O10 C21 -63.0(2) . . . . ?
N2 Eu1 O10 C21 148.6(2) . . . . ?
N1 Eu1 O10 C21 -88.1(2) . . . . ?
N3 Eu1 O10 C21 12.5(2) . . . . ?
O1 Eu1 N1 C2 -5.94(19) . . . . ?
O6 Eu1 N1 C2 -98.4(2) . . . . ?
O5 Eu1 N1 C2 33.3(2) . . . . ?
O9 Eu1 N1 C2 81.5(2) . . . . ?
O10 Eu1 N1 C2 -154.70(18) . . . . ?
O2 Eu1 N1 C2 177.6(2) . . . . ?
N2 Eu1 N1 C2 -52.1(2) . . . . ?
N3 Eu1 N1 C2 128.15(19) . . . . ?
O1 Eu1 N1 C6 179.5(2) . . . . ?
O6 Eu1 N1 C6 87.0(2) . . . . ?
O5 Eu1 N1 C6 -141.2(2) . . . . ?
O9 Eu1 N1 C6 -93.1(2) . . . . ?
O10 Eu1 N1 C6 30.7(3) . . . . ?
O2 Eu1 N1 C6 3.0(2) . . . . ?
N2 Eu1 N1 C6 133.4(2) . . . . ?
N3 Eu1 N1 C6 -46.4(2) . . . . ?
O1 Eu1 N2 C9 84.6(2) . . . . ?
O6 Eu1 N2 C9 178.2(2) . . . . ?
O5 Eu1 N2 C9 -1.26(19) . . . . ?
O9 Eu1 N2 C9 26.4(2) . . . . ?
O10 Eu1 N2 C9 -98.8(2) . . . . ?
O2 Eu1 N2 C9 -147.37(19) . . . . ?
N1 Eu1 N2 C9 126.4(2) . . . . ?
N3 Eu1 N2 C9 -53.8(2) . . . . ?
O1 Eu1 N2 C13 -94.8(2) . . . . ?
O6 Eu1 N2 C13 -1.16(19) . . . . ?
O5 Eu1 N2 C13 179.3(2) . . . . ?
O9 Eu1 N2 C13 -152.97(19) . . . . ?
O10 Eu1 N2 C13 81.9(2) . . . . ?
O2 Eu1 N2 C13 33.2(2) . . . . ?
N1 Eu1 N2 C13 -53.0(2) . . . . ?
N3 Eu1 N2 C13 126.8(2) . . . . ?
O1 Eu1 N3 C20 -159.1(2) . . . . ?
O6 Eu1 N3 C20 23.4(3) . . . . ?
O5 Eu1 N3 C20 -105.0(2) . . . . ?
O9 Eu1 N3 C20 172.8(2) . . . . ?
O10 Eu1 N3 C20 -8.2(2) . . . . ?
O2 Eu1 N3 C20 76.4(2) . . . . ?
N2 Eu1 N3 C20 -57.8(2) . . . . ?
N1 Eu1 N3 C20 122.0(2) . . . . ?
O1 Eu1 N3 C16 25.3(3) . . . . ?
O6 Eu1 N3 C16 -152.2(2) . . . . ?
O5 Eu1 N3 C16 79.4(2) . . . . ?
O9 Eu1 N3 C16 -2.7(2) . . . . ?
O10 Eu1 N3 C16 176.2(2) . . . . ?
O2 Eu1 N3 C16 -99.1(2) . . . . ?
N2 Eu1 N3 C16 126.7(2) . . . . ?
N1 Eu1 N3 C16 -53.5(2) . . . . ?
Eu1 O1 C1 O3 174.8(2) . . . . ?
Eu1 O1 C1 C2 -6.0(4) . . . . ?
C6 N1 C2 C3 0.8(4) . . . . ?
Eu1 N1 C2 C3 -173.9(2) . . . . ?
C6 N1 C2 C1 -179.8(3) . . . . ?
Eu1 N1 C2 C1 5.6(3) . . . . ?
O3 C1 C2 N1 179.0(3) . . . . ?
O1 C1 C2 N1 -0.2(4) . . . . ?
O3 C1 C2 C3 -1.6(5) . . . . ?
O1 C1 C2 C3 179.2(3) . . . . ?
N1 C2 C3 C4 -0.1(5) . . . . ?
C1 C2 C3 C4 -179.5(3) . . . . ?
C2 C3 C4 C5 -0.6(5) . . . . ?
C3 C4 C5 C6 0.7(5) . . . . ?
C2 N1 C6 C5 -0.7(4) . . . . ?
Eu1 N1 C6 C5 173.9(2) . . . . ?
C2 N1 C6 C7 179.8(2) . . . . ?
Eu1 N1 C6 C7 -5.6(3) . . . . ?
C4 C5 C6 N1 0.0(5) . . . . ?
C4 C5 C6 C7 179.4(3) . . . . ?
Eu1 O2 C7 O4 178.0(3) . . . . ?
Eu1 O2 C7 C6 -3.3(4) . . . . ?
N1 C6 C7 O4 -175.4(3) . . . . ?
C5 C6 C7 O4 5.1(5) . . . . ?
N1 C6 C7 O2 5.8(4) . . . . ?
C5 C6 C7 O2 -173.7(3) . . . . ?
Eu1 O5 C8 O7 178.4(2) . . . . ?
Eu1 O5 C8 C9 -2.3(4) . . . . ?
C13 N2 C9 C10 0.2(4) . . . . ?
Eu1 N2 C9 C10 -179.2(2) . . . . ?
C13 N2 C9 C8 -179.9(2) . . . . ?
Eu1 N2 C9 C8 0.7(3) . . . . ?
O5 C8 C9 N2 1.0(4) . . . . ?
O7 C8 C9 N2 -179.8(3) . . . . ?
O5 C8 C9 C10 -179.2(3) . . . . ?
O7 C8 C9 C10 0.1(5) . . . . ?
N2 C9 C10 C11 -0.2(5) . . . . ?
C8 C9 C10 C11 179.9(3) . . . . ?
C9 C10 C11 C12 -0.5(6) . . . . ?
C10 C11 C12 C13 1.2(6) . . . . ?
C9 N2 C13 C12 0.5(4) . . . . ?
Eu1 N2 C13 C12 179.9(2) . . . . ?
C9 N2 C13 C14 -179.7(2) . . . . ?
Eu1 N2 C13 C14 -0.3(3) . . . . ?
C11 C12 C13 N2 -1.2(5) . . . . ?
C11 C12 C13 C14 179.0(3) . . . . ?
Eu1 O6 C14 O8 176.5(2) . . . . ?
Eu1 O6 C14 C13 -4.3(4) . . . . ?
N2 C13 C14 O8 -178.0(3) . . . . ?
C12 C13 C14 O8 1.9(5) . . . . ?
N2 C13 C14 O6 2.8(4) . . . . ?
C12 C13 C14 O6 -177.3(3) . . . . ?
Eu1 O9 C15 O11 169.3(3) . . . . ?
Eu1 O9 C15 C16 -12.2(4) . . . . ?
C20 N3 C16 C17 0.6(5) . . . . ?
Eu1 N3 C16 C17 176.1(3) . . . . ?
C20 N3 C16 C15 -177.1(3) . . . . ?
Eu1 N3 C16 C15 -1.5(4) . . . . ?
O11 C15 C16 N3 -172.9(3) . . . . ?
O9 C15 C16 N3 8.5(4) . . . . ?
O11 C15 C16 C17 9.5(5) . . . . ?
O9 C15 C16 C17 -169.1(3) . . . . ?
N3 C16 C17 C18 -1.8(5) . . . . ?
C15 C16 C17 C18 175.6(3) . . . . ?
C16 C17 C18 C19 1.2(6) . . . . ?
C17 C18 C19 C20 0.6(5) . . . . ?
C16 N3 C20 C19 1.3(5) . . . . ?
Eu1 N3 C20 C19 -174.3(2) . . . . ?
C16 N3 C20 C21 -179.6(3) . . . . ?
Eu1 N3 C20 C21 4.9(3) . . . . ?
C18 C19 C20 N3 -1.9(5) . . . . ?
C18 C19 C20 C21 179.1(3) . . . . ?
Eu1 O10 C21 O12 163.9(2) . . . . ?
Eu1 O10 C21 C20 -15.0(4) . . . . ?
N3 C20 C21 O12 -173.0(3) . . . . ?
C19 C20 C21 O12 6.1(5) . . . . ?
N3 C20 C21 O10 5.9(4) . . . . ?
C19 C20 C21 O10 -175.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.076

# Attachment 'k1649Tb.cif'

data_K1649
_database_code_depnum_ccdc_archive 'CCDC 761088'
#TrackingRef 'k1649Tb.cif'

_audit_creation_method           Xtal3.6
_audit_creation_date             09-09-29

_chemical_formula_sum            'C27 H33 N6 O14 Tb1'
_chemical_formula_moiety         'C21 H9 N3 O12 Tb, 3(C2 H8 N), 2(O)'
_chemical_formula_weight         824.52
_chemical_melting_point          ?

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P_c_21_n
_symmetry_space_group_name_Hall  p_-2n_-2ac

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

_cell_length_a                   10.67920(10)
_cell_length_b                   17.0739(3)
_cell_length_c                   18.7096(3)
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                90.00000
_cell_volume                     3411.43(9)
_cell_formula_units_Z            4

_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71072

_cell_measurement_reflns_used    4376
_cell_measurement_theta_min      1.00
_cell_measurement_theta_max      27.48
_cell_measurement_temperature    293

_exptl_absorpt_coefficient_mu    2.146
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            colourless

_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinovski & Minor, 1997)'
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_diffrn_reflns_number            63289 #total no. of integrated reflns
_reflns_number_total             4033
_reflns_Friedel_coverage         0
_reflns_number_gt                3530
_reflns_threshold_expression     'F2 > 3.00 sig(F2)'

_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measured_fraction_theta_full 1.00
_diffrn_reflns_av_R_equivalents  .056
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ? #<< do not append units
_diffrn_standards_decay_%        ? #<< do not append %

_refine_ls_structure_factor_coef F
_refine_ls_R_factor_gt           .030
_refine_ls_wR_factor_ref         .024
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_number_reflns         3899
_refine_ls_number_parameters     433
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    noref
_refine_ls_shift/su_max          .017
_refine_diff_density_min         -2.211
_refine_diff_density_max         1.044

_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .00000
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   ?

# 3. Information for the "methods" section
#-----------------------------------------

_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_cell_refinement       'DENZO-SMN (Otwinovski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinovski & Minor, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'

# 4. Supplementary data for validation and tables
#------------------------------------------------

loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 108 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 148 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N ? 0 24 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 56 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Tb ? 0 4 -.591 4.151 'Int Tables Vol IV Tables 2.2B and 2.3.1'

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 .618937(18) .516(3) .259932(12) .0283(2) Uani ? ? 1.00000 ? ?
O2 .7203(9) .605(3) .3438(5) .045(4) Uani ? ? 1.00000 ? ?
N3 .5061(12) .389(3) .2644(5) .029(4) Uani ? ? 1.00000 ? ?
O4 .4484(5) .499(3) .1763(3) .041(3) Uani ? ? 1.00000 ? ?
N5 .4934(15) .642(3) .2567(5) .040(5) Uani ? ? 1.00000 ? ?
C7 1.1116(7) .514(3) .2564(5) .072(7) Uani ? ? 1.00000 ? ?
O8 .7170(7) .434(3) .1682(5) .043(4) Uani ? ? 1.00000 ? ?
C9 .4141(7) .373(3) .2187(4) .035(4) Uani ? ? 1.00000 ? ?
C10 .3862(6) .438(3) .1665(4) .035(3) Uani ? ? 1.00000 ? ?
O11 .6758(7) .609(3) .1662(4) .042(4) Uani ? ? 1.00000 ? ?
C12 .6201(8) .674(3) .1532(4) .043(4) Uani ? ? 1.00000 ? ?
O15 .8912(6) .642(3) .4039(4) .058(4) Uani ? ? 1.00000 ? ?
O16 .6928(9) .425(3) .3515(5) .047(4) Uani ? ? 1.00000 ? ?
O17 .8770(6) .405(3) .1000(5) .066(4) Uani ? ? 1.00000 ? ?
C18 .8293(8) .436(3) .1533(4) .041(4) Uani ? ? 1.00000 ? ?
C20 .4778(10) .263(3) .3188(5) .050(5) Uani ? ? 1.00000 ? ?
C21 .6431(8) .360(3) .3641(4) .041(4) Uani ? ? 1.00000 ? ?
C22 .9149(7) .477(3) .2053(4) .039(4) Uani ? ? 1.00000 ? ?
C23 .8399(8) .605(3) .3557(4) .038(4) Uani ? ? 1.00000 ? ?
O24 .4621(5) .532(3) .3537(3) .050(4) Uani ? ? 1.00000 ? ?
C25 .9180(7) .559(3) .3051(4) .039(4) Uani ? ? 1.00000 ? ?
O26 .3081(6) .425(3) .1200(4) .052(3) Uani ? ? 1.00000 ? ?
C27 .4049(7) .655(3) .3038(4) .038(4) Uani ? ? 1.00000 ? ?
N28 .8540(5) .520(3) .2556(3) .033(2) Uani ? ? 1.00000 ? ?
O29 .3138(7) .603(3) .4084(4) .066(4) Uani ? ? 1.00000 ? ?
C31 .3857(14) .245(3) .2714(10) .053(7) Uani ? ? 1.00000 ? ?
C32 .3912(6) .594(3) .3606(4) .040(4) Uani ? ? 1.00000 ? ?
C33 .349(2) .775(3) .2493(9) .061(9) Uani ? ? 1.00000 ? ?
O34 .6761(8) .312(3) .4108(4) .064(4) Uani ? ? 1.00000 ? ?
C35 .5154(7) .694(3) .2039(4) .039(4) Uani ? ? 1.00000 ? ?
O36 .6420(9) .720(3) .1046(4) .072(5) Uani ? ? 1.00000 ? ?
C37 .3513(8) .301(3) .2200(6) .045(5) Uani ? ? 1.00000 ? ?
C40 .5370(7) .336(3) .3147(4) .038(4) Uani ? ? 1.00000 ? ?
C41 .3294(9) .721(3) .3007(5) .057(5) Uani ? ? 1.00000 ? ?
C44 1.0431(9) .473(3) .2052(6) .059(5) Uani ? ? 1.00000 ? ?
C45 .4422(10) .761(3) .1983(5) .054(5) Uani ? ? 1.00000 ? ?
N1 .8264(8) .363(3) .5168(4) .062(5) Uani ? ? 1.00000 ? ?
N2 .2984(8) .195(3) .5089(5) .066(5) Uani ? ? 1.00000 ? ?
N4 .2228(7) .560(3) .5418(4) .054(4) Uani ? ? 1.00000 ? ?
C6 .0967(10) .588(3) .5204(8) .082(8) Uani ? ? 1.00000 ? ?
C15 .8919(19) .436(3) .4964(10) .101(11) Uani ? ? 1.00000 ? ?
C16 .3694(15) .123(3) .4874(8) .095(10) Uani ? ? 1.00000 ? ?
C11 .2836(15) .615(3) .5932(8) .085(8) Uani ? ? 1.00000 ? ?
C13 .9149(16) .301(3) .5427(9) .097(10) Uani ? ? 1.00000 ? ?
C14 .3754(19) .256(3) .5433(12) .113(14) Uani ? ? 1.00000 ? ?
C8 1.0500(8) .557(3) .3056(5) .058(5) Uani ? ? 1.00000 ? ?
O3w .4344(10) .458(3) .4933(7) .097(7) Uani ? ? 1.00000 ? ?
O2w .696(3) .898(3) .085(3) .22(3) Uani ? ? 1.00000 ? ?
H41 .26627 .72919 .33381 .07006 Uiso ? ? 1.00000 ? ?
H33 .30030 .82036 .24768 .07494 Uiso ? ? 1.00000 ? ?
H45 .47122 .78775 .15844 .06757 Uiso ? ? 1.00000 ? ?
H8 1.09464 .58529 .33902 .07194 Uiso ? ? 1.00000 ? ?
H7 1.19865 .50996 .25741 .08429 Uiso ? ? 1.00000 ? ?
H44 1.08442 .44425 .17080 .07252 Uiso ? ? 1.00000 ? ?
H20 .50060 .22733 .35354 .06212 Uiso ? ? 1.00000 ? ?
H31 .34642 .19739 .27237 .06520 Uiso ? ? 1.00000 ? ?
H37 .28732 .29135 .18783 .05573 Uiso ? ? 1.00000 ? ?
H1a .78315 .34284 .47536 .07698 Uiso ? ? 1.00000 ? ?
H1b .76768 .37468 .55438 .07698 Uiso ? ? 1.00000 ? ?
H4a .27490 .55616 .50000 .06786 Uiso ? ? 1.00000 ? ?
H4b .21409 .50950 .56443 .06786 Uiso ? ? 1.00000 ? ?
H2a .23405 .17949 .54209 .08182 Uiso ? ? 1.00000 ? ?
H2b .26129 .21715 .46630 .08182 Uiso ? ? 1.00000 ? ?
H14a .41286 .23388 .58604 .17678 Uiso ? ? 1.00000 ? ?
H14b .44038 .27193 .50947 .17678 Uiso ? ? 1.00000 ? ?
H14c .32869 .30352 .55723 .17678 Uiso ? ? 1.00000 ? ?
H16a .43461 .13895 .45376 .14624 Uiso ? ? 1.00000 ? ?
H16b .40709 .10090 .53033 .14624 Uiso ? ? 1.00000 ? ?
H16c .31847 .08236 .46451 .14624 Uiso ? ? 1.00000 ? ?
H15a .93513 .45663 .53803 .15347 Uiso ? ? 1.00000 ? ?
H15b .95075 .42447 .45819 .15347 Uiso ? ? 1.00000 ? ?
H15c .83346 .47707 .47888 .15347 Uiso ? ? 1.00000 ? ?
H13a .97406 .28931 .50502 .15083 Uiso ? ? 1.00000 ? ?
H13b .95844 .32147 .58486 .15083 Uiso ? ? 1.00000 ? ?
H13c .87180 .25237 .55671 .15083 Uiso ? ? 1.00000 ? ?
H11a .29156 .66619 .57090 .13341 Uiso ? ? 1.00000 ? ?
H11b .23012 .61907 .63599 .13341 Uiso ? ? 1.00000 ? ?
H11c .36617 .59617 .60782 .13341 Uiso ? ? 1.00000 ? ?
H6a .04469 .59272 .56308 .12812 Uiso ? ? 1.00000 ? ?
H6b .10613 .63984 .49799 .12812 Uiso ? ? 1.00000 ? ?
H6c .05752 .55245 .48655 .12812 Uiso ? ? 1.00000 ? ?

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Tb1 .02478(19) .0282(2) .0320(2) -.0005(3) .00035(8) -.0002(5)
O2 .045(4) .048(4) .043(3) .005(3) -.003(3) -.017(3)
N3 .023(4) .029(5) .036(4) .001(3) .000(3) -.004(3)
O4 .036(2) .041(5) .047(3) -.006(2) -.0125(17) .005(2)
N5 .038(5) .043(6) .039(5) .001(5) -.000(4) -.004(4)
C7 .035(3) .127(13) .054(4) .037(11) .005(3) -.016(12)
O8 .033(4) .041(4) .054(4) .001(3) .001(3) -.012(3)
C9 .028(4) .043(4) .034(3) -.003(3) .005(3) -.002(3)
C10 .022(3) .050(4) .033(3) .001(3) -.002(3) -.005(3)
O11 .039(4) .045(4) .043(3) -.002(3) .015(3) -.001(3)
C12 .055(4) .040(4) .033(4) -.004(4) -.001(3) .007(3)
O15 .052(3) .075(4) .047(3) -.006(3) -.006(2) -.020(3)
O16 .056(5) .035(4) .051(4) .002(3) -.018(3) .001(3)
O17 .052(3) .082(5) .063(5) -.001(3) .010(3) -.036(4)
C18 .043(4) .041(4) .039(4) .004(3) .005(3) -.015(3)
C20 .065(5) .031(4) .055(5) .002(4) .007(4) .010(3)
C21 .049(4) .041(4) .035(4) .007(3) -.003(3) .003(3)
C22 .034(4) .047(4) .035(4) .005(3) .006(3) -.007(4)
C23 .039(4) .036(4) .039(4) -.007(3) -.006(3) -.005(3)
O24 .042(2) .061(6) .048(3) .003(3) .0180(18) .008(3)
C25 .037(4) .044(4) .035(4) -.002(3) -.003(3) -.002(3)
O26 .045(3) .049(3) .061(4) -.003(2) -.014(3) .002(3)
C27 .037(3) .043(4) .035(4) .005(3) -.001(3) -.009(3)
N28 .0249(18) .035(3) .040(2) .008(6) .0014(15) -.006(5)
O29 .060(4) .082(5) .055(4) .020(3) .021(3) .008(3)
C31 .059(7) .032(6) .068(9) -.016(5) .004(5) .005(5)
C32 .027(3) .050(5) .043(4) .001(4) .010(3) -.007(3)
C33 .067(9) .056(9) .060(8) .022(7) -.008(6) -.008(6)
O34 .084(5) .053(4) .053(4) .004(4) -.022(3) .009(3)
C35 .042(4) .035(4) .039(4) .003(3) -.010(3) -.003(3)
O36 .087(5) .080(5) .050(4) .016(4) .016(3) .022(4)
C37 .042(4) .047(5) .046(4) -.005(4) -.002(4) -.008(5)
C40 .045(4) .037(4) .034(3) .000(3) -.000(3) -.001(3)
C41 .054(4) .069(6) .049(5) .024(5) .001(3) -.002(4)
C44 .047(5) .073(6) .057(5) .006(4) .017(4) -.019(5)
C45 .068(6) .051(5) .043(5) .015(5) -.008(4) .004(4)
N1 .065(5) .080(6) .042(4) -.003(4) .000(3) -.013(4)
N2 .055(4) .094(7) .050(4) .006(5) .004(3) .024(4)
N4 .055(4) .052(4) .055(4) -.002(3) .013(3) .006(3)
C6 .062(6) .099(9) .084(8) -.004(6) .001(5) .036(7)
C15 .120(12) .103(12) .081(9) -.040(10) -.001(8) -.003(8)
C16 .101(10) .121(13) .062(7) .019(9) .015(6) .018(7)
C11 .084(8) .087(9) .083(8) -.010(7) .012(7) -.006(7)
C13 .104(9) .111(13) .076(9) .042(9) -.020(7) -.011(8)
C14 .125(15) .088(11) .125(15) -.007(10) .025(10) .029(11)
C8 .034(4) .084(6) .058(5) -.015(4) -.009(4) -.015(5)
O3w .082(5) .099(8) .110(7) .013(5) .012(5) .042(6)
O2w .17(2) .106(13) .38(6) .030(13) .08(3) .01(2)

# 5. Molecular Geometry
#----------------------

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O2 2.44(5) . . no
Tb1 O4 2.419(10) . . no
Tb1 O8 2.45(4) . . no
Tb1 O11 2.44(5) . . no
Tb1 O16 2.44(5) . . no
Tb1 O24 2.441(10) . . no
Tb1 N3 2.48(6) . . no
Tb1 N5 2.54(6) . . no
Tb1 N28 2.513(6) . . no
O2 C23 1.297(13) . . no
O4 C10 1.25(6) . . no
O8 C18 1.232(12) . . no
O11 C12 1.28(6) . . no
O15 C23 1.23(4) . . no
O16 C21 1.25(6) . . no
O17 C18 1.24(3) . . no
O24 C32 1.31(6) . . no
O26 C10 1.226(16) . . no
O29 C32 1.228(14) . . no
O34 C21 1.25(5) . . no
O36 C12 1.22(5) . . no
N3 C9 1.33(2) . . no
N3 C40 1.35(5) . . no
N5 C27 1.31(2) . . no
N5 C35 1.35(5) . . no
N28 C22 1.36(4) . . no
N28 C25 1.33(4) . . no
N1 C15 1.48(6) . . no
N1 C13 1.50(5) . . no
N1 H1A 0.9700 . . no
N1 H1B 0.9600 . . no
N2 C14 1.48(5) . . no
N2 C16 1.50(6) . . no
N2 H2A 0.9600 . . no
N2 H2B 0.9700 . . no
N4 C11 1.49(5) . . no
N4 C6 1.48(3) . . no
N4 H4A 0.9600 . . no
N4 H4B 0.9700 . . no
C7 C8 1.35(4) . . no
C7 C44 1.39(4) . . no
C8 C25 1.410(12) . . no
C9 C10 1.51(5) . . no
C9 C37 1.40(6) . . no
C12 C35 1.51(2) . . no
C18 C22 1.51(4) . . no
C20 C40 1.40(6) . . no
C20 C31 1.36(3) . . no
C21 C40 1.52(2) . . no
C22 C44 1.371(13) . . no
C23 C25 1.49(4) . . no
C27 C32 1.50(5) . . no
C27 C41 1.39(6) . . no
C31 C37 1.41(5) . . no
C33 C41 1.35(5) . . no
C33 C45 1.40(2) . . no
C35 C45 1.39(6) . . no
C7 H7 0.9300 . . no
C8 H8 0.9200 . . no
C20 H20 0.9200 . . no
C31 H31 0.9100 . . no
C33 H33 0.9300 . . no
C37 H37 0.9300 . . no
C41 H41 0.9300 . . no
C44 H44 0.9200 . . no
C45 H45 0.9300 . . no
C13 H13A 0.9700 . . no
C13 H13C 0.9800 . . no
C13 H13B 0.9800 . . no
C15 H15C 0.9900 . . no
C15 H15A 0.9700 . . no
C15 H15B 0.9700 . . no
C14 H14A 0.9700 . . no
C14 H14B 0.9800 . . no
C14 H14C 0.9900 . . no
C16 H16B 0.9700 . . no
C16 H16C 0.9800 . . no
C16 H16A 0.9800 . . no
C6 H6A 0.9800 . . no
C6 H6B 0.9800 . . no
C6 H6C 0.9700 . . no
C11 H11A 0.9700 . . no
C11 H11B 0.9900 . . no
C11 H11C 0.9800 . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Tb1 O4 146(2) . . . no
O2 Tb1 O8 128.1(6) . . . no
O2 Tb1 O11 86.9(18) . . . no
O2 Tb1 O16 78.6(13) . . . no
O2 Tb1 O24 76.8(10) . . . no
O2 Tb1 N3 137.6(11) . . . no
O2 Tb1 N5 73.8(17) . . . no
O2 Tb1 N28 63.9(10) . . . no
O4 Tb1 O8 78.5(10) . . . no
O4 Tb1 O11 78.5(10) . . . no
O4 Tb1 O16 128(2) . . . no
O4 Tb1 O24 87.8(3) . . . no
O4 Tb1 N3 63.3(14) . . . no
O4 Tb1 N5 71.8(14) . . . no
O4 Tb1 N28 137.3(4) . . . no
O8 Tb1 O11 76.3(13) . . . no
O8 Tb1 O16 89.4(18) . . . no
O8 Tb1 O24 149(2) . . . no
O8 Tb1 N3 74.5(17) . . . no
O8 Tb1 N5 134.0(11) . . . no
O8 Tb1 N28 64.3(10) . . . no
O11 Tb1 O16 146.8(4) . . . no
O11 Tb1 O24 128(2) . . . no
O11 Tb1 N3 135.5(10) . . . no
O11 Tb1 N5 64.1(14) . . . no
O11 Tb1 N28 73.2(10) . . . no
O16 Tb1 O24 77.8(10) . . . no
O16 Tb1 N3 65.0(15) . . . no
O16 Tb1 N5 136.6(10) . . . no
O16 Tb1 N28 73.6(10) . . . no
O24 Tb1 N3 75.0(14) . . . no
O24 Tb1 N5 63.9(14) . . . no
O24 Tb1 N28 134.9(5) . . . no
N3 Tb1 N5 119.0(9) . . . no
N3 Tb1 N28 121(2) . . . no
N5 Tb1 N28 120(2) . . . no
Tb1 O2 C23 123(3) . . . no
Tb1 O4 C10 127(3) . . . no
Tb1 O8 C18 124(3) . . . no
Tb1 O11 C12 125.7(10) . . . no
Tb1 O16 C21 124.0(12) . . . no
Tb1 O24 C32 124(2) . . . no
Tb1 N3 C9 121(3) . . . no
Tb1 N3 C40 119.5(19) . . . no
C9 N3 C40 120(4) . . . no
Tb1 N5 C27 121(3) . . . no
Tb1 N5 C35 118.9(19) . . . no
C27 N5 C35 120(4) . . . no
Tb1 N28 C22 119.1(18) . . . no
Tb1 N28 C25 120.3(15) . . . no
C22 N28 C25 120.5(11) . . . no
C13 N1 C15 112.3(18) . . . no
C13 N1 H1A 108.00 . . . no
C13 N1 H1B 109.00 . . . no
C15 N1 H1A 109.00 . . . no
C15 N1 H1B 109.00 . . . no
H1A N1 H1B 110.00 . . . no
C14 N2 C16 114.5(18) . . . no
C16 N2 H2A 108.00 . . . no
C16 N2 H2B 108.00 . . . no
C14 N2 H2A 108.00 . . . no
C14 N2 H2B 108.00 . . . no
H2A N2 H2B 110.00 . . . no
C6 N4 C11 112(3) . . . no
C11 N4 H4B 109.00 . . . no
H4A N4 H4B 111.00 . . . no
C6 N4 H4B 109.00 . . . no
C11 N4 H4A 108.00 . . . no
C6 N4 H4A 109.00 . . . no
C8 C7 C44 119.1(12) . . . no
C7 C8 C25 120(3) . . . no
N3 C9 C37 122(3) . . . no
N3 C9 C10 114(4) . . . no
C10 C9 C37 124.2(15) . . . no
O4 C10 O26 128(4) . . . no
O26 C10 C9 117(4) . . . no
O4 C10 C9 114.4(16) . . . no
O11 C12 C35 115(3) . . . no
O36 C12 C35 118(4) . . . no
O11 C12 O36 127(2) . . . no
O17 C18 C22 118.0(11) . . . no
O8 C18 O17 125(3) . . . no
O8 C18 C22 117(2) . . . no
C31 C20 C40 120(3) . . . no
O16 C21 C40 116(3) . . . no
O16 C21 O34 126(2) . . . no
O34 C21 C40 117(4) . . . no
N28 C22 C44 120(2) . . . no
C18 C22 C44 126(3) . . . no
N28 C22 C18 114.1(11) . . . no
O2 C23 O15 124(3) . . . no
O2 C23 C25 116(2) . . . no
O15 C23 C25 119.3(12) . . . no
N28 C25 C23 114.8(12) . . . no
C8 C25 C23 125(2) . . . no
N28 C25 C8 120(3) . . . no
N5 C27 C32 116(4) . . . no
C32 C27 C41 122.6(14) . . . no
N5 C27 C41 122(3) . . . no
C20 C31 C37 119(4) . . . no
O29 C32 C27 120(4) . . . no
O24 C32 C27 115.9(15) . . . no
O24 C32 O29 124(4) . . . no
C41 C33 C45 119(4) . . . no
N5 C35 C45 119.9(17) . . . no
C12 C35 C45 124(3) . . . no
N5 C35 C12 116(4) . . . no
C9 C37 C31 119.0(18) . . . no
C20 C40 C21 123(3) . . . no
N3 C40 C20 121.7(19) . . . no
N3 C40 C21 115(4) . . . no
C27 C41 C33 119.7(18) . . . no
C7 C44 C22 120(3) . . . no
C33 C45 C35 119(3) . . . no
C44 C7 H7 120.00 . . . no
C8 C7 H7 121.00 . . . no
C7 C8 H8 120.00 . . . no
C25 C8 H8 121.00 . . . no
C31 C20 H20 120.00 . . . no
C40 C20 H20 120.00 . . . no
C37 C31 H31 120.00 . . . no
C20 C31 H31 121.00 . . . no
C41 C33 H33 120.00 . . . no
C45 C33 H33 121.00 . . . no
C9 C37 H37 120.00 . . . no
C31 C37 H37 121.00 . . . no
C33 C41 H41 119.00 . . . no
C27 C41 H41 121.00 . . . no
C22 C44 H44 120.00 . . . no
C7 C44 H44 120.00 . . . no
C33 C45 H45 135.00 . . . no
C35 C45 H45 106.00 . . . no
N1 C13 H13C 113.00 . . . no
H13B C13 H13C 108.00 . . . no
N1 C13 H13A 109.00 . . . no
N1 C13 H13B 108.00 . . . no
H13A C13 H13C 109.00 . . . no
H13A C13 H13B 111.00 . . . no
N1 C15 H15B 109.00 . . . no
N1 C15 H15C 112.00 . . . no
N1 C15 H15A 109.00 . . . no
H15A C15 H15C 108.00 . . . no
H15B C15 H15C 108.00 . . . no
H15A C15 H15B 111.00 . . . no
H14A C14 H14B 110.00 . . . no
H14A C14 H14C 108.00 . . . no
N2 C14 H14A 108.00 . . . no
N2 C14 H14B 108.00 . . . no
N2 C14 H14C 114.00 . . . no
H14B C14 H14C 108.00 . . . no
H16B C16 H16C 108.00 . . . no
N2 C16 H16A 108.00 . . . no
N2 C16 H16B 108.00 . . . no
N2 C16 H16C 115.00 . . . no
H16A C16 H16B 110.00 . . . no
H16A C16 H16C 108.00 . . . no
N4 C6 H6A 109.00 . . . no
N4 C6 H6B 108.00 . . . no
N4 C6 H6C 111.00 . . . no
H6A C6 H6B 109.00 . . . no
H6A C6 H6C 110.00 . . . no
H6B C6 H6C 109.00 . . . no
N4 C11 H11A 109.00 . . . no
N4 C11 H11B 108.00 . . . no
N4 C11 H11C 111.00 . . . no
H11A C11 H11B 110.00 . . . no
H11A C11 H11C 110.00 . . . no
H11B C11 H11C 109.00 . . . no

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

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
#
#D H A D - H H...A D...A D - H...A symm(A)
#
N1 H1A O34 0.9700 1.7400 2.70(3) 168.00 . no
N1 H1B O8 0.9600 2.3600 3.12(3) 135.00 4_655 no
N1 H1B O17 0.9600 1.8400 2.77(2) 161.00 4_655 no
N2 H2A O2 0.9600 2.5300 3.16(4) 123.00 2_646 no
N2 H2A O15 0.9600 1.7900 2.75(3) 173.00 2_646 no
N2 H2B O36 0.9700 1.8400 2.735(17) 153.00 3_445 no
N4 H4A O3W 0.9600 2.3900 2.99(4) 120.00 . no
N4 H4A O29 0.9600 1.9400 2.78(2) 145.00 . no
N4 H4B O26 0.9700 1.7900 2.75(6) 170.00 4_555 no
C11 H11A O34 0.9700 2.5400 3.39(7) 147.00 2_656 no
C44 H44 O26 0.9200 2.5900 3.35(2) 140.00 1_655 no
C45 H45 O36 0.9300 2.3800 2.85(2) 111.00 . no

#--------------------------------------------------------------------------
# Special items requested by author for inclusion in paper
#--------------------------------------------------------------------------

loop_
_publ_manuscript_incl_extra_item
_publ_manuscript_incl_extra_defn
? ?

#--------------------------------------------------------------------------
# Items which are non-mandatory for Acta C submissions
#--------------------------------------------------------------------------

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Tb1 H33 3.8600 . 3_545 no
O2 O16 3.09(7) . . no
O2 O24 3.03(3) . . no
O2 N5 2.99(2) . . no
O2 N28 2.62(4) . . no
O2 C25 2.37(3) . . no
O2 N2 3.16(4) . 2_656 no
O2 C16 3.315(19) . 2_656 no
O2W O3W 3.11(5) . 3_555 no
O2W O36 3.12(7) . . no
O3W O29 3.21(6) . . no
O3W O24 2.92(3) . . no
O3W O17 2.98(3) . 4_655 no
O3W N4 2.99(4) . . no
O3W O2W 3.11(5) . 3_445 no
O4 N3 2.57(5) . . no
O4 C9 2.32(7) . . no
O4 O11 3.08(4) . . no
O4 C6 3.32(4) . 4_554 no
O4 N5 2.91(6) . . no
O4 O8 3.08(3) . . no
O8 C22 2.34(2) . . no
O8 N3 2.98(2) . . no
O8 C15 3.42(2) . 4_654 no
O8 N1 3.12(3) . 4_654 no
O8 O4 3.08(3) . . no
O8 N28 2.64(4) . . no
O8 O11 3.02(7) . . no
O11 C35 2.35(5) . . no
O11 N28 2.95(4) . . no
O11 C18 3.39(6) . . no
O11 O8 3.02(7) . . no
O11 N5 2.64(2) . . no
O11 O4 3.08(4) . . no
O15 N2 2.75(3) . 2_656 no
O15 C6 3.23(3) . 1_655 no
O16 N28 2.97(4) . . no
O16 O2 3.09(7) . . no
O16 C40 2.36(5) . . no
O16 N3 2.65(2) . . no
O16 O24 3.07(4) . . no
O17 O3W 2.98(3) . 4_654 no
O17 N1 2.77(2) . 4_654 no
O24 O2 3.03(3) . . no
O24 N5 2.63(5) . . no
O24 O3W 2.92(3) . . no
O24 N3 3.00(6) . . no
O24 O16 3.07(4) . . no
O24 C27 2.38(6) . . no
O26 N4 2.75(6) . 4_554 no
O26 C44 3.35(2) . 1_455 no
O29 N4 2.78(2) . . no
O29 O3W 3.21(6) . . no
O29 C6 3.136(16) . . no
O34 N1 2.70(3) . . no
O34 C11 3.39(7) . 2_646 no
O36 O2W 3.12(7) . . no
O36 C16 3.41(4) . 3_555 no
O36 N2 2.735(17) . 3_555 no
O2 H16B 2.7200 . 2_656 no
O2 H2A 2.5300 . 2_656 no
O2W H15B 2.7800 . 3_455 no
O3W H4A 2.3900 . . no
O3W H4B 2.8400 . . no
O4 H4B 2.7200 . 4_554 no
O4 H6A 2.6600 . 4_554 no
O4 H11B 2.9000 . 4_554 no
O8 H1B 2.3600 . 4_654 no
O8 H33 2.6500 . 3_545 no
O11 H16C 2.9200 . 3_555 no
O11 H31 2.6300 . 3_555 no
O15 H8 2.6700 . . no
O15 H6B 2.8900 . 1_655 no
O15 H2A 1.7900 . 2_656 no
O15 H6C 2.8100 . 1_655 no
O16 H1A 2.8800 . . no
O16 H33 2.8200 . 3_545 no
O17 H44 2.6700 . . no
O17 H1B 1.8400 . 4_654 no
O24 H16B 2.8400 . 2_656 no
O26 H14C 2.8000 . 4_554 no
O26 H4B 1.7900 . 4_554 no
O26 H44 2.5900 . 1_455 no
O26 H37 2.6200 . . no
O29 H8 2.6900 . 1_455 no
O29 H6B 2.8500 . . no
O29 H41 2.6200 . . no
O29 H4A 1.9400 . . no
O34 H11A 2.5400 . 2_646 no
O34 H20 2.6000 . . no
O34 H1A 1.7400 . . no
O36 H45 2.3800 . . no
O36 H2B 1.8400 . 3_555 no
N1 O17 2.77(2) . 4_655 no
N1 O34 2.70(3) . . no
N1 O8 3.12(3) . 4_655 no
N1 C18 3.29(3) . 4_655 no
N2 O36 2.735(17) . 3_445 no
N2 O15 2.75(3) . 2_646 no
N2 C23 3.31(4) . 2_646 no
N2 O2 3.16(4) . 2_646 no
N3 C21 2.42(2) . . no
N3 O4 2.57(5) . . no
N3 C10 2.39(3) . . no
N3 O8 2.98(2) . . no
N3 O16 2.65(2) . . no
N3 O24 3.00(6) . . no
N4 O29 2.78(2) . . no
N4 O3W 2.99(4) . . no
N4 O26 2.75(6) . 4_555 no
N4 C10 3.34(5) . 4_555 no
N5 C32 2.38(3) . . no
N5 O4 2.91(6) . . no
N5 C12 2.43(2) . . no
N5 O24 2.63(5) . . no
N5 O2 2.99(2) . . no
N5 O11 2.64(2) . . no
N28 O16 2.97(4) . . no
N28 O8 2.64(4) . . no
N28 O11 2.95(4) . . no
N28 C18 2.41(4) . . no
N28 C23 2.37(4) . . no
N28 O2 2.62(4) . . no
C6 C15 3.42(6) . 1_455 no
C6 O29 3.136(16) . . no
C6 O4 3.32(4) . 4_555 no
C6 O15 3.23(3) . 1_455 no
C10 N4 3.34(5) . 4_554 no
C11 O34 3.39(7) . 2_656 no
C12 C31 3.39(3) . 3_555 no
C15 C6 3.42(6) . 1_655 no
C15 O8 3.42(2) . 4_655 no
C16 O2 3.315(19) . 2_646 no
C16 O36 3.41(4) . 3_445 no
C18 C33 3.31(6) . 3_545 no
C18 N1 3.29(3) . 4_654 no
C21 C33 3.38(4) . 3_545 no
C23 C31 3.41(5) . 3_555 no
C23 N2 3.31(4) . 2_656 no
C25 C31 3.50(7) . 3_555 no
C31 C25 3.50(7) . 3_445 no
C31 C23 3.41(5) . 3_445 no
C31 C12 3.39(3) . 3_445 no
C33 C18 3.31(6) . 3_455 no
C33 C21 3.38(4) . 3_455 no
C44 O26 3.35(2) . 1_655 no
C6 H15A 2.8500 . 1_455 no
C9 H13B 2.9800 . 4_654 no
C10 H13B 3.0100 . 4_654 no
C10 H15A 3.0900 . 4_654 no
C10 H7 2.9000 . 1_455 no
C10 H4B 2.5100 . 4_554 no
C12 H31 2.8200 . 3_555 no
C12 H6A 2.8000 . 4_554 no
C12 H2B 2.8000 . 3_555 no
C13 H6B 2.8600 . 2_646 no
C15 H6C 2.6700 . 1_655 no
C18 H1B 2.3700 . 4_654 no
C18 H33 2.7300 . 3_545 no
C21 H33 2.7700 . 3_545 no
C21 H1A 2.5800 . . no
C22 H33 3.0700 . 3_545 no
C23 H31 2.8700 . 3_555 no
C23 H2A 2.4300 . 2_656 no
C25 H31 2.8800 . 3_555 no
C32 H4A 2.9600 . . no
C32 H16B 2.9700 . 2_656 no
C40 H33 3.0600 . 3_545 no
C44 H11C 2.9500 . 4_654 no
H1A O34 1.7400 . . no
H1A C21 2.5800 . . no
H1A O16 2.8800 . . no
H1B O17 1.8400 . 4_655 no
H1B C18 2.3700 . 4_655 no
H1B O8 2.3600 . 4_655 no
H2A C23 2.4300 . 2_646 no
H2A O15 1.7900 . 2_646 no
H2A O2 2.5300 . 2_646 no
H2B C12 2.8000 . 3_445 no
H2B O36 1.8400 . 3_445 no
H4A C32 2.9600 . . no
H4A O29 1.9400 . . no
H4A O3W 2.3900 . . no
H4B O26 1.7900 . 4_555 no
H4B O3W 2.8400 . . no
H4B C10 2.5100 . 4_555 no
H4B O4 2.7200 . 4_555 no
H6A C12 2.8000 . 4_555 no
H6A O4 2.6600 . 4_555 no
H6A H11B 2.4500 . . no
H6B H13C 2.1900 . 2_656 no
H6B O29 2.8500 . . no
H6B C13 2.8600 . 2_656 no
H6B H11A 2.4500 . . no
H6B O15 2.8900 . 1_455 no
H6C C15 2.6700 . 1_455 no
H6C H15B 2.5200 . 1_455 no
H6C O15 2.8100 . 1_455 no
H6C H15A 2.3000 . 1_455 no
H7 C10 2.9000 . 1_655 no
H8 O15 2.6700 . . no
H8 O29 2.6900 . 1_655 no
H11A O34 2.5400 . 2_656 no
H11A H6B 2.4500 . . no
H11B H6A 2.4500 . . no
H11B O4 2.9000 . 4_555 no
H11C C44 2.9500 . 4_655 no
H11C H16A 2.5300 . 2_656 no
H13A H15B 2.4800 . . no
H13B C10 3.0100 . 4_655 no
H13B H15A 2.4800 . . no
H13B C9 2.9800 . 4_655 no
H13C H6B 2.1900 . 2_646 no
H13C H41 2.5500 . 2_646 no
H14A H16B 2.5000 . . no
H14B H16A 2.5000 . . no
H14C O26 2.8000 . 4_555 no
H15A C6 2.8500 . 1_655 no
H15A H6C 2.3000 . 1_655 no
H15A H13B 2.4800 . . no
H15A C10 3.0900 . 4_655 no
H15B O2W 2.7800 . 3_545 no
H15B H6C 2.5200 . 1_655 no
H15B H13A 2.4800 . . no
H16A H20 2.5100 . . no
H16A H11C 2.5300 . 2_646 no
H16A H14B 2.5000 . . no
H16B O24 2.8400 . 2_646 no
H16B C32 2.9700 . 2_646 no
H16B O2 2.7200 . 2_646 no
H16B H14A 2.5000 . . no
H16C O11 2.9200 . 3_445 no
H20 O34 2.6000 . . no
H20 H16A 2.5100 . . no
H31 O11 2.6300 . 3_445 no
H31 C12 2.8200 . 3_445 no
H31 C23 2.8700 . 3_445 no
H31 C25 2.8800 . 3_445 no
H33 Tb1 3.8600 . 3_455 no
H33 O8 2.6500 . 3_455 no
H33 O16 2.8200 . 3_455 no
H33 C18 2.7300 . 3_455 no
H33 C21 2.7700 . 3_455 no
H33 C22 3.0700 . 3_455 no
H33 C40 3.0600 . 3_455 no
H37 O26 2.6200 . . no
H41 O29 2.6200 . . no
H41 H13C 2.5500 . 2_656 no
H44 O17 2.6700 . . no
H44 O26 2.5900 . 1_655 no
H45 O36 2.3800 . . no

_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   ?

_geom_special_details            ?

_cell_special_details            
; ?
;

_exptl_special_details           
; ?
;

_diffrn_special_details          
; ?
;

_chemical_compound_source        ?
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_analytical     ?
_chemical_formula_structural     ?

_exptl_crystal_F_000             1672

loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
? ?

_reflns_limit_h_min              0
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              24
_reflns_number_observed          ?
_reflns_d_resolution_high        .77
_reflns_d_resolution_low         9.355

_diffrn_reflns_av_sigmaI/netI    .023
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_reduction_process ?

_diffrn_ambient_temperature      293
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_detector       'CCD plate'

_refine_ls_extinction_expression ?
_refine_ls_matrix_type           full
_refine_ls_number_restraints     7
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          .045
_refine_ls_wR_factor_all         .041
_refine_ls_goodness_of_fit_all   1.752
_refine_ls_shift/su_mean         .002

#==========================================================================
# Structure Factor lists should be submitted as separate files
#==========================================================================

#data_<structure> # but for xtal use the refln data is needed in same block

loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_meas
_refln_F_calc
_refln_F_sigma
_refln_F_squared_meas
_refln_F_squared_calc
_refln_F_squared_sigma
_refln_observed_status
_refln_F_meas_friedel
_refln_F_sigma_friedel
_refln_F_squared_meas_friedel
_refln_F_squared_sigma_friedel
? ? ? ? ? ? ? ? ? ? ? ? ? ?

#-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end-end