
data_mlc03
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C19 H25 N5 O8 Tb, C16 H36 N, 0.47(C3 H8 O), 0.53(C3 H6 O), 3(H2 O)'
_chemical_formula_sum
 'C38 H73 N6 O12 Tb'
_chemical_formula_weight          964.94
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Tb'  'Tb'  -0.1723   4.1537
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    P2(1)/c
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    13.1047(5)
_cell_length_b                    13.3397(5)
_cell_length_c                    26.0901(9)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.0130(10)
_cell_angle_gamma                 90.00
_cell_volume                      4560.9(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     24638
_cell_measurement_theta_min       2.18
_cell_measurement_theta_max       37.67
 
_exptl_crystal_description        Square
_exptl_crystal_colour             Colorless
_exptl_crystal_size_max           0.35
_exptl_crystal_size_mid           0.31
_exptl_crystal_size_min           0.11
_exptl_crystal_density_meas       0
_exptl_crystal_density_diffrn     1.405
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2016
_exptl_absorpt_coefficient_mu     1.613
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   0.6022
_exptl_absorpt_correction_T_max   0.8425
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker SMART 1000'
_diffrn_measurement_method        'ω scans at 5 φ settings'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             78733
_diffrn_reflns_av_R_equivalents   0.0879
_diffrn_reflns_av_sigmaI/netI     0.0790
_diffrn_reflns_limit_h_min        -22
_diffrn_reflns_limit_h_max        22
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -40
_diffrn_reflns_limit_l_max        44
_diffrn_reflns_theta_min          1.56
_diffrn_reflns_theta_max          37.67
_reflns_number_total              20316
_reflns_number_gt                 11252
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'Bruker SMART v5.630'
_computing_cell_refinement        'Bruker SAINT v6.45A'
_computing_data_reduction         'Bruker SAINT v6.45A'
_computing_structure_solution     'Bruker XS v6.12'
_computing_structure_refinement   'Bruker XL v6.12'
_computing_molecular_graphics     'Bruker XP v5.1'
_computing_publication_material   'Bruker XCIF v6.12'
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            'Full matrix'
_refine_ls_weighting_scheme       Sigma
_refine_ls_weighting_details      'w=1/s²(Fo²)'
_atom_sites_solution_primary      'Direct methods'
_atom_sites_solution_secondary    'Difference Fourier map'
_atom_sites_solution_hydrogens    'Geometric positions'
_refine_ls_hydrogen_treatment     Riding
_chemical_absolute_configuration  ?
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          20316
_refine_ls_number_parameters      577
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0900
_refine_ls_R_factor_gt            0.0384
_refine_ls_wR_factor_ref          0.0717
_refine_ls_wR_factor_gt           0.0639
_refine_ls_goodness_of_fit_ref    1.077
_refine_ls_restrained_S_all       1.077
_refine_ls_shift/su_max           0.005
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Tb Tb 0.248793(9) 0.007650(7) 0.499532(4) 0.01424(3) Uani 1 1 d . . .
O1 O 0.17019(11) -0.08704(12) 0.56642(6) 0.0186(3) Uani 1 1 d . . .
O2 O 0.14198(13) -0.23222(13) 0.60743(6) 0.0291(4) Uani 1 1 d . . .
O3 O 0.33036(11) -0.04999(12) 0.42269(5) 0.0185(3) Uani 1 1 d . . .
O4 O 0.36419(16) -0.17090(14) 0.36576(6) 0.0362(5) Uani 1 1 d . . .
O5 O 0.39468(11) -0.05726(12) 0.54070(5) 0.0179(3) Uani 1 1 d . . .
O6 O 0.46724(11) -0.10652(12) 0.61366(6) 0.0186(3) Uani 1 1 d . . .
O7 O 0.10577(11) -0.03364(12) 0.44968(5) 0.0179(3) Uani 1 1 d . . .
O8 O 0.03028(12) -0.03909(13) 0.37334(6) 0.0235(3) Uani 1 1 d . . .
N1 N 0.25043(13) -0.17768(14) 0.48762(6) 0.0165(4) Uani 1 1 d . . .
N2 N 0.29506(13) 0.10109(14) 0.58583(7) 0.0173(4) Uani 1 1 d . . .
N3 N 0.39144(13) 0.13675(14) 0.48613(7) 0.0177(4) Uani 1 1 d . . .
H3 H 0.4412 0.1029 0.4675 0.021 Uiso 1 1 calc R . .
N4 N 0.20267(13) 0.14462(15) 0.42942(7) 0.0182(4) Uani 1 1 d . . .
N5 N 0.10483(14) 0.12221(14) 0.53019(7) 0.0175(4) Uani 1 1 d . . .
H5 H 0.0553 0.0792 0.5431 0.021 Uiso 1 1 calc R . .
C1 C 0.28925(16) -0.21672(18) 0.44489(8) 0.0192(4) Uani 1 1 d . . .
C2 C 0.29104(18) -0.31953(19) 0.43646(10) 0.0282(5) Uani 1 1 d . . .
H2 H 0.3173 -0.3464 0.4054 0.034 Uiso 1 1 calc R . .
C3 C 0.2534(2) -0.3821(2) 0.47463(12) 0.0381(7) Uani 1 1 d . . .
H3A H 0.2550 -0.4528 0.4703 0.046 Uiso 1 1 calc R . .
C4 C 0.2134(2) -0.3404(2) 0.51910(11) 0.0330(6) Uani 1 1 d . . .
H4 H 0.1867 -0.3819 0.5455 0.040 Uiso 1 1 calc R . .
C5 C 0.21346(16) -0.23718(17) 0.52417(9) 0.0202(5) Uani 1 1 d . . .
C6 C 0.33125(17) -0.13945(19) 0.40734(8) 0.0205(5) Uani 1 1 d . . .
C7 C 0.17127(17) -0.18167(19) 0.57066(9) 0.0207(5) Uani 1 1 d . . .
C8 C 0.36370(17) 0.18656(18) 0.57593(9) 0.0214(5) Uani 1 1 d . . .
H8A H 0.3991 0.2046 0.6082 0.026 Uiso 1 1 calc R . .
H8B H 0.3224 0.2450 0.5652 0.026 Uiso 1 1 calc R . .
C9 C 0.44248(17) 0.16484(18) 0.53505(9) 0.0215(5) Uani 1 1 d . . .
H9A H 0.4855 0.2249 0.5296 0.026 Uiso 1 1 calc R . .
H9B H 0.4872 0.1094 0.5465 0.026 Uiso 1 1 calc R . .
C10 C 0.36635(18) 0.22477(18) 0.45492(9) 0.0237(5) Uani 1 1 d . . .
H10A H 0.4297 0.2550 0.4412 0.028 Uiso 1 1 calc R . .
H10B H 0.3314 0.2756 0.4763 0.028 Uiso 1 1 calc R . .
C11 C 0.29702(17) 0.19312(19) 0.41082(9) 0.0234(5) Uani 1 1 d . . .
H11A H 0.2789 0.2528 0.3902 0.028 Uiso 1 1 calc R . .
H11B H 0.3343 0.1459 0.3883 0.028 Uiso 1 1 calc R . .
C12 C 0.13242(17) 0.22047(18) 0.45128(9) 0.0235(5) Uani 1 1 d . . .
H12A H 0.0964 0.2549 0.4229 0.028 Uiso 1 1 calc R . .
H12B H 0.1729 0.2714 0.4700 0.028 Uiso 1 1 calc R . .
C13 C 0.05420(17) 0.17595(18) 0.48744(9) 0.0214(5) Uani 1 1 d . . .
H13A H 0.0107 0.2301 0.5014 0.026 Uiso 1 1 calc R . .
H13B H 0.0098 0.1288 0.4684 0.026 Uiso 1 1 calc R . .
C14 C 0.13005(17) 0.18997(18) 0.57305(9) 0.0220(5) Uani 1 1 d . . .
H14A H 0.0667 0.2112 0.5906 0.026 Uiso 1 1 calc R . .
H14B H 0.1646 0.2506 0.5598 0.026 Uiso 1 1 calc R . .
C15 C 0.19911(16) 0.13668(18) 0.61055(8) 0.0204(5) Uani 1 1 d . . .
H15A H 0.2164 0.1829 0.6389 0.024 Uiso 1 1 calc R . .
H15B H 0.1624 0.0786 0.6253 0.024 Uiso 1 1 calc R . .
C16 C 0.34549(16) 0.02554(18) 0.61839(8) 0.0197(4) Uani 1 1 d . . .
H16A H 0.2927 -0.0102 0.6385 0.024 Uiso 1 1 calc R . .
H16B H 0.3908 0.0604 0.6430 0.024 Uiso 1 1 calc R . .
C17 C 0.40811(15) -0.05124(17) 0.58888(8) 0.0160(4) Uani 1 1 d . . .
C18 C 0.15250(17) 0.08943(18) 0.38702(8) 0.0217(5) Uani 1 1 d . . .
H18A H 0.2055 0.0662 0.3627 0.026 Uiso 1 1 calc R . .
H18B H 0.1071 0.1361 0.3683 0.026 Uiso 1 1 calc R . .
C19 C 0.09038(15) -0.00018(17) 0.40452(7) 0.0181(4) Uani 1 1 d . . .
N6 N 0.63769(14) 0.28388(14) 0.27996(7) 0.0197(4) Uani 1 1 d . . .
C20 C 0.71915(16) 0.34706(19) 0.25415(9) 0.0236(5) Uani 1 1 d . . .
H20A H 0.7005 0.4186 0.2580 0.028 Uiso 1 1 calc R . .
H20B H 0.7190 0.3315 0.2170 0.028 Uiso 1 1 calc R . .
C21 C 0.82709(17) 0.3325(2) 0.27457(10) 0.0293(6) Uani 1 1 d . . .
H21A H 0.8493 0.2626 0.2684 0.035 Uiso 1 1 calc R . .
H21B H 0.8281 0.3448 0.3120 0.035 Uiso 1 1 calc R . .
C22 C 0.8999(2) 0.4044(3) 0.24810(14) 0.0545(10) Uani 1 1 d . . .
H22A H 0.8918 0.3984 0.2105 0.065 Uiso 1 1 calc R . .
H22B H 0.8829 0.4741 0.2580 0.065 Uiso 1 1 calc R . .
C23 C 1.0110(2) 0.3815(3) 0.26291(14) 0.0571(10) Uani 1 1 d . . .
H23A H 1.0185 0.3856 0.3002 0.086 Uiso 1 1 calc R . .
H23B H 1.0564 0.4303 0.2466 0.086 Uiso 1 1 calc R . .
H23C H 1.0290 0.3138 0.2514 0.086 Uiso 1 1 calc R . .
C24 C 0.66727(17) 0.17328(17) 0.27939(8) 0.0215(5) Uani 1 1 d . . .
H24A H 0.7311 0.1651 0.2993 0.026 Uiso 1 1 calc R . .
H24B H 0.6133 0.1347 0.2971 0.026 Uiso 1 1 calc R . .
C25 C 0.6831(2) 0.1282(2) 0.22651(9) 0.0296(6) Uani 1 1 d . . .
H25A H 0.6206 0.1375 0.2057 0.036 Uiso 1 1 calc R . .
H25B H 0.7400 0.1630 0.2090 0.036 Uiso 1 1 calc R . .
C26 C 0.7071(2) 0.01755(19) 0.23077(9) 0.0306(5) Uani 1 1 d . . .
H26A H 0.6489 -0.0172 0.2471 0.037 Uiso 1 1 calc R . .
H26B H 0.7676 0.0085 0.2531 0.037 Uiso 1 1 calc R . .
C27 C 0.7281(2) -0.0300(2) 0.17879(10) 0.0389(7) Uani 1 1 d . . .
H27A H 0.6681 -0.0222 0.1568 0.058 Uiso 1 1 calc R . .
H27B H 0.7429 -0.1015 0.1833 0.058 Uiso 1 1 calc R . .
H27C H 0.7868 0.0030 0.1628 0.058 Uiso 1 1 calc R . .
C28 C 0.53833(17) 0.30036(19) 0.25045(9) 0.0235(5) Uani 1 1 d . . .
H28A H 0.5493 0.2799 0.2144 0.028 Uiso 1 1 calc R . .
H28B H 0.5230 0.3730 0.2504 0.028 Uiso 1 1 calc R . .
C29 C 0.44577(17) 0.2451(2) 0.27074(9) 0.0267(5) Uani 1 1 d . . .
H29A H 0.4652 0.1755 0.2797 0.032 Uiso 1 1 calc R . .
H29B H 0.4211 0.2785 0.3023 0.032 Uiso 1 1 calc R . .
C30 C 0.36064(19) 0.2431(2) 0.23107(9) 0.0282(5) Uani 1 1 d . . .
H30A H 0.3855 0.2086 0.1999 0.034 Uiso 1 1 calc R . .
H30B H 0.3432 0.3129 0.2215 0.034 Uiso 1 1 calc R . .
C31 C 0.2648(2) 0.1905(2) 0.25007(11) 0.0374(7) Uani 1 1 d . . .
H31A H 0.2822 0.1228 0.2617 0.056 Uiso 1 1 calc R . .
H31B H 0.2149 0.1865 0.2221 0.056 Uiso 1 1 calc R . .
H31C H 0.2355 0.2285 0.2787 0.056 Uiso 1 1 calc R . .
C32 C 0.62434(17) 0.31335(17) 0.33590(8) 0.0212(5) Uani 1 1 d . . .
H32A H 0.5692 0.2718 0.3508 0.025 Uiso 1 1 calc R . .
H32B H 0.6881 0.2972 0.3545 0.025 Uiso 1 1 calc R . .
C33 C 0.5990(2) 0.4229(2) 0.34513(10) 0.0319(6) Uani 1 1 d . . .
H33A H 0.6594 0.4646 0.3371 0.038 Uiso 1 1 calc R . .
H33B H 0.5428 0.4434 0.3220 0.038 Uiso 1 1 calc R . .
C34 C 0.5677(2) 0.4402(2) 0.39990(11) 0.0371(7) Uani 1 1 d . . .
H34A H 0.6192 0.4089 0.4226 0.044 Uiso 1 1 calc R . .
H34B H 0.5020 0.4055 0.4060 0.044 Uiso 1 1 calc R . .
C35 C 0.5560(3) 0.5486(3) 0.41505(14) 0.0576(9) Uani 1 1 d . . .
H35A H 0.6223 0.5823 0.4127 0.086 Uiso 1 1 calc R . .
H35B H 0.5308 0.5526 0.4504 0.086 Uiso 1 1 calc R . .
H35C H 0.5074 0.5814 0.3920 0.086 Uiso 1 1 calc R . .
O11 O 0.57538(13) 0.50550(12) 0.18920(6) 0.0269(4) Uani 1 1 d G . .
H11A H 0.6027 0.4468 0.1698 0.040 Uiso 1 1 d G . .
H11B H 0.5354 0.5544 0.1683 0.040 Uiso 1 1 d G . .
O12 O 0.91747(15) 0.09753(15) 0.31226(6) 0.0349(4) Uani 1 1 d G . .
H12A H 0.8917 0.1478 0.3375 0.052 Uiso 1 1 d G . .
H12B H 0.9665 0.0469 0.3261 0.052 Uiso 1 1 d G . .
O51A O 0.1484(7) 0.4416(5) 0.6143(5) 0.065(3) Uani 0.476(4) 1 d P A 1
H51C H 0.1742 0.3943 0.6311 0.097 Uiso 0.476(4) 1 calc PR A 1
C52A C 0.0544(6) 0.4415(7) 0.6202(4) 0.064(3) Uani 0.476(4) 1 d P A 1
H52A H 0.0496 0.5036 0.6415 0.077 Uiso 0.476(4) 1 calc PR A 1
C53A C 0.0002(6) 0.3743(6) 0.6551(3) 0.058(2) Uani 0.476(4) 1 d P A 1
H53A H 0.0489 0.3279 0.6710 0.086 Uiso 0.476(4) 1 calc PR A 1
H53B H -0.0511 0.3361 0.6359 0.086 Uiso 0.476(4) 1 calc PR A 1
H53C H -0.0336 0.4138 0.6818 0.086 Uiso 0.476(4) 1 calc PR A 1
C54A C -0.0223(9) 0.4727(10) 0.5781(5) 0.092(4) Uani 0.476(4) 1 d P A 1
H54A H 0.0079 0.5253 0.5568 0.138 Uiso 0.476(4) 1 calc PR A 1
H54B H -0.0848 0.4981 0.5942 0.138 Uiso 0.476(4) 1 calc PR A 1
H54C H -0.0388 0.4144 0.5568 0.138 Uiso 0.476(4) 1 calc PR A 1
O50A O 0.8868(4) 0.2675(4) 0.14694(19) 0.0619(16) Uani 0.476(4) 1 d P A 1
O51B O 0.1315(5) 0.4316(3) 0.5364(2) 0.0745(18) Uani 0.524(4) 1 d P A 2
C52B C 0.0899(7) 0.4533(5) 0.5758(3) 0.0529(19) Uani 0.524(4) 1 d P A 2
C53B C -0.0022(8) 0.5292(7) 0.5909(5) 0.068(3) Uani 0.524(4) 1 d P A 2
H53D H -0.0373 0.5042 0.6215 0.102 Uiso 0.524(4) 1 calc PR A 2
H53E H -0.0508 0.5333 0.5623 0.102 Uiso 0.524(4) 1 calc PR A 2
H53F H 0.0258 0.5960 0.5978 0.102 Uiso 0.524(4) 1 calc PR A 2
C54B C 0.1385(15) 0.4504(15) 0.6255(7) 0.149(10) Uani 0.524(4) 1 d P A 2
H54D H 0.2064 0.4202 0.6222 0.223 Uiso 0.524(4) 1 calc PR A 2
H54E H 0.0970 0.4103 0.6491 0.223 Uiso 0.524(4) 1 calc PR A 2
H54F H 0.1451 0.5187 0.6389 0.223 Uiso 0.524(4) 1 calc PR A 2
O50B O -0.0123(5) 0.3726(6) 0.7096(2) 0.096(2) Uani 0.524(4) 1 d PG A 2
H50C H -0.0159 0.3218 0.6815 0.144 Uiso 0.524(4) 1 d PG A 2
H50D H -0.0577 0.4027 0.7362 0.144 Uiso 0.524(4) 1 d PG A 2
 
 
_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 O7 2.3467(14) . ?
Tb O5 2.3573(15) . ?
Tb O1 2.3879(15) . ?
Tb O3 2.3987(15) . ?
Tb N1 2.4918(19) . ?
Tb N5 2.5564(18) . ?
Tb N3 2.5657(18) . ?
Tb N2 2.6437(17) . ?
Tb N4 2.6550(18) . ?
O1 C7 1.267(3) . ?
O2 C7 1.234(3) . ?
O3 C6 1.259(3) . ?
O4 C6 1.241(3) . ?
O5 C17 1.272(2) . ?
O6 C17 1.250(2) . ?
O7 C19 1.276(2) . ?
O8 C19 1.245(2) . ?
N1 C5 1.332(3) . ?
N1 C1 1.332(3) . ?
N2 C8 1.475(3) . ?
N2 C16 1.475(3) . ?
N2 C15 1.491(3) . ?
N3 C10 1.466(3) . ?
N3 C9 1.489(3) . ?
N4 C18 1.483(3) . ?
N4 C12 1.482(3) . ?
N4 C11 1.478(3) . ?
N5 C13 1.482(3) . ?
N5 C14 1.475(3) . ?
C1 C2 1.389(3) . ?
C1 C6 1.525(3) . ?
C2 C3 1.390(4) . ?
C3 C4 1.389(4) . ?
C4 C5 1.384(3) . ?
C5 C7 1.525(3) . ?
C8 C9 1.513(3) . ?
C10 C11 1.526(3) . ?
C12 C13 1.515(3) . ?
C14 C15 1.510(3) . ?
C16 C17 1.522(3) . ?
C18 C19 1.517(3) . ?
N6 C20 1.518(3) . ?
N6 C28 1.528(3) . ?
N6 C32 1.522(3) . ?
N6 C24 1.526(3) . ?
C20 C21 1.524(3) . ?
C21 C22 1.518(4) . ?
C22 C23 1.538(4) . ?
C24 C25 1.519(3) . ?
C25 C26 1.513(4) . ?
C26 C27 1.522(4) . ?
C28 C29 1.515(3) . ?
C29 C30 1.522(3) . ?
C30 C31 1.522(4) . ?
C32 C33 1.517(3) . ?
C33 C34 1.505(4) . ?
C34 C35 1.507(4) . ?
O51A C52A 1.241(12) . ?
C52A C53A 1.463(12) . ?
C52A C54A 1.545(15) . ?
O51B C52B 1.199(8) . ?
C52B C54B 1.445(19) . ?
C52B C53B 1.625(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
O7 Tb O5 144.47(6) . . ?
O7 Tb O1 86.35(5) . . ?
O5 Tb O1 79.79(5) . . ?
O7 Tb O3 79.49(5) . . ?
O5 Tb O3 84.35(5) . . ?
O1 Tb O3 129.31(6) . . ?
O7 Tb N1 72.84(5) . . ?
O5 Tb N1 71.66(5) . . ?
O1 Tb N1 64.54(5) . . ?
O3 Tb N1 64.78(6) . . ?
O7 Tb N5 74.00(5) . . ?
O5 Tb N5 132.49(5) . . ?
O1 Tb N5 76.65(6) . . ?
O3 Tb N5 141.46(5) . . ?
N1 Tb N5 129.68(6) . . ?
O7 Tb N3 131.59(5) . . ?
O5 Tb N3 73.61(6) . . ?
O1 Tb N3 140.27(5) . . ?
O3 Tb N3 77.08(6) . . ?
N1 Tb N3 129.99(6) . . ?
N5 Tb N3 100.32(6) . . ?
O7 Tb N2 139.96(5) . . ?
O5 Tb N2 66.38(5) . . ?
O1 Tb N2 74.10(5) . . ?
O3 Tb N2 139.53(5) . . ?
N1 Tb N2 124.89(5) . . ?
N5 Tb N2 67.71(5) . . ?
N3 Tb N2 68.45(6) . . ?
O7 Tb N4 66.30(5) . . ?
O5 Tb N4 138.69(5) . . ?
O1 Tb N4 140.29(5) . . ?
O3 Tb N4 75.30(6) . . ?
N1 Tb N4 126.78(5) . . ?
N5 Tb N4 68.67(6) . . ?
N3 Tb N4 67.04(5) . . ?
N2 Tb N4 108.32(6) . . ?
C7 O1 Tb 125.87(15) . . ?
C6 O3 Tb 125.03(14) . . ?
C17 O5 Tb 122.63(14) . . ?
C19 O7 Tb 123.76(14) . . ?
C5 N1 C1 120.4(2) . . ?
C5 N1 Tb 119.92(14) . . ?
C1 N1 Tb 119.72(15) . . ?
C8 N2 C16 110.85(17) . . ?
C8 N2 C15 110.12(18) . . ?
C16 N2 C15 110.26(17) . . ?
C8 N2 Tb 110.80(13) . . ?
C16 N2 Tb 105.73(13) . . ?
C15 N2 Tb 108.99(12) . . ?
C10 N3 C9 112.04(18) . . ?
C10 N3 Tb 116.74(13) . . ?
C9 N3 Tb 112.29(13) . . ?
C18 N4 C12 110.54(17) . . ?
C18 N4 C11 110.08(17) . . ?
C12 N4 C11 110.32(19) . . ?
C18 N4 Tb 105.86(13) . . ?
C12 N4 Tb 110.24(12) . . ?
C11 N4 Tb 109.71(12) . . ?
C13 N5 C14 111.97(18) . . ?
C13 N5 Tb 112.57(13) . . ?
C14 N5 Tb 115.99(13) . . ?
N1 C1 C2 121.7(2) . . ?
N1 C1 C6 114.3(2) . . ?
C2 C1 C6 124.0(2) . . ?
C1 C2 C3 118.2(2) . . ?
C2 C3 C4 119.5(2) . . ?
C5 C4 C3 118.5(2) . . ?
N1 C5 C4 121.7(2) . . ?
N1 C5 C7 114.3(2) . . ?
C4 C5 C7 124.0(2) . . ?
O4 C6 O3 127.0(2) . . ?
O4 C6 C1 117.3(2) . . ?
O3 C6 C1 115.66(19) . . ?
O2 C7 O1 127.5(2) . . ?
O2 C7 C5 117.8(2) . . ?
O1 C7 C5 114.7(2) . . ?
N2 C8 C9 113.07(19) . . ?
N3 C9 C8 110.25(17) . . ?
N3 C10 C11 109.31(19) . . ?
N4 C11 C10 111.82(18) . . ?
N4 C12 C13 113.11(19) . . ?
N5 C13 C12 110.81(17) . . ?
N5 C14 C15 109.68(18) . . ?
N2 C15 C14 112.02(18) . . ?
N2 C16 C17 114.21(17) . . ?
O6 C17 O5 124.0(2) . . ?
O6 C17 C16 118.02(18) . . ?
O5 C17 C16 117.91(18) . . ?
N4 C18 C19 113.87(17) . . ?
O8 C19 O7 123.9(2) . . ?
O8 C19 C18 118.11(19) . . ?
O7 C19 C18 117.97(18) . . ?
C20 N6 C28 107.20(16) . . ?
C20 N6 C32 111.30(18) . . ?
C28 N6 C32 110.36(17) . . ?
C20 N6 C24 110.72(17) . . ?
C28 N6 C24 110.53(18) . . ?
C32 N6 C24 106.77(16) . . ?
N6 C20 C21 115.28(18) . . ?
C20 C21 C22 110.1(2) . . ?
C23 C22 C21 110.8(2) . . ?
C25 C24 N6 115.25(18) . . ?
C26 C25 C24 110.4(2) . . ?
C25 C26 C27 112.2(2) . . ?
N6 C28 C29 115.84(18) . . ?
C30 C29 C28 110.94(19) . . ?
C29 C30 C31 113.0(2) . . ?
C33 C32 N6 115.22(18) . . ?
C34 C33 C32 111.0(2) . . ?
C33 C34 C35 115.1(3) . . ?
O51A C52A C53A 124.1(10) . . ?
O51A C52A C54A 123.9(11) . . ?
C53A C52A C54A 106.9(8) . . ?
O51B C52B C54B 124.3(12) . . ?
O51B C52B C53B 134.0(8) . . ?
C54B C52B C53B 97.3(10) . . ?
 
loop_
 _geom_hbond_atom_site_label_D
 _geom_hbond_atom_site_label_H
 _geom_hbond_atom_site_label_A
 _geom_hbond_distance_DH
 _geom_hbond_distance_HA
 _geom_hbond_distance_DA
 _geom_hbond_angle_DHA
 _geom_hbond_site_symmetry_A
N3 H3 O5  0.93 2.25 3.078(2) 148.5 3_656
N3 H3 O6  0.93 2.43 3.221(2) 142.2 3_656
N5 H5 O7  0.93 2.20 3.048(2) 150.4 3_556
N5 H5 O8  0.93 2.51 3.271(3) 139.4 3_556
O11 H11A O4  1.00 1.87 2.867(2) 172.1 2_655
O11 H11B O6  1.00 1.82 2.776(2) 159.2 4_565
O12 H12A O2  1.00 1.88 2.868(3) 170.6 3_656
O12 H12B O8  1.00 1.88 2.836(2) 159.2 1_655
N3 H3 O3  0.93 2.76 3.096(2) 102.2 .
N5 H5 O1  0.93 2.75 3.069(2) 101.3 .
 
_diffrn_measured_fraction_theta_max    0.836
_diffrn_reflns_theta_full              37.67
_diffrn_measured_fraction_theta_full   0.836
_refine_diff_density_max    3.035
_refine_diff_density_min   -2.004
_refine_diff_density_rms    0.128

