

data_mlc23

 

_audit_creation_method            SHELXL-97

_chemical_name_systematic

;

 ?

;

_chemical_name_common             ?

_chemical_melting_point           ?

_chemical_formula_moiety          
 'C19 H24 Cl0.63 F0.37 N5 O8 Tb, C16 H36 N, C3 H6 O, 2(H2 O)'

_chemical_formula_sum

 'C38 H70 Cl0.64 F0.36 N6 O11 Tb'

_chemical_formula_weight          975.45

 

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'

 'F'  'F'   0.0171   0.0103

 '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'

 

_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                    13.2324(6)

_cell_length_b                    12.9812(6)

_cell_length_c                    26.2126(11)

_cell_angle_alpha                 90.00

_cell_angle_beta                  90.528(2)

_cell_angle_gamma                 90.00

_cell_volume                      4502.4(3)

_cell_formula_units_Z             4

_cell_measurement_temperature     100(2)

_cell_measurement_reflns_used     9873

_cell_measurement_theta_min       2.33

_cell_measurement_theta_max       38.01

 

_exptl_crystal_description        Trapezoidal

_exptl_crystal_colour             Colorless

_exptl_crystal_size_max           0.15

_exptl_crystal_size_mid           0.15

_exptl_crystal_size_min           0.15

_exptl_crystal_density_meas       .

_exptl_crystal_density_diffrn     1.439

_exptl_crystal_density_method     'not measured'

_exptl_crystal_F_000              2028

_exptl_absorpt_coefficient_mu     1.671

_exptl_absorpt_correction_type    'multi-scan'

_exptl_absorpt_correction_T_min   0.6753

_exptl_absorpt_correction_T_max   0.7478

_exptl_absorpt_process_details    'SADABS v2008/1, Bruker-AXS, Madison, WI'

 

_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 KAPPA APEX II'

_diffrn_measurement_method        'ω scans; 16 settings'

_diffrn_detector_area_resol_mean  ?

_diffrn_reflns_number             172388

_diffrn_reflns_av_R_equivalents   0.0331

_diffrn_reflns_av_sigmaI/netI     0.0252

_diffrn_reflns_limit_h_min        -22

_diffrn_reflns_limit_h_max        23

_diffrn_reflns_limit_k_min        -23

_diffrn_reflns_limit_k_max        21

_diffrn_reflns_limit_l_min        -44

_diffrn_reflns_limit_l_max        46

_diffrn_reflns_theta_min          1.54

_diffrn_reflns_theta_max          39.88

_reflns_number_total              26652

_reflns_number_gt                 18685

_reflns_threshold_expression      >2sigma(I)

 

_computing_data_collection        'Bruker APEX2 v2009.7-0'

_computing_cell_refinement        'Bruker SAINT-Plus v7.66A'

_computing_data_reduction         'Bruker SAINT-Plus v7.66A'

_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)'

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'

_computing_molecular_graphics     'Bruker XP v5.1'

_computing_publication_material   'Bruker XCIF 2008'

 

_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          26652

_refine_ls_number_parameters      525

_refine_ls_number_restraints      0

_refine_ls_R_factor_all           0.0534

_refine_ls_R_factor_gt            0.0285

_refine_ls_wR_factor_ref          0.0518

_refine_ls_wR_factor_gt           0.0499

_refine_ls_goodness_of_fit_ref    2.025

_refine_ls_restrained_S_all       2.025

_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

Tb1 Tb 0.247197(3) 0.502442(4) 0.497427(2) 0.01641(1) Uani 1 1 d . . .

Cl1 Cl 0.26577(13) -0.02595(13) 0.48040(4) 0.0538(4) Uani 0.630(6) 1 d P . .

F1 F 0.2514(4) 0.0026(5) 0.47745(19) 0.0503(15) Uiso 0.370(6) 1 d P . .

O1 O 0.16965(6) 0.41199(6) 0.56584(3) 0.02131(15) Uani 1 1 d . . .

O2 O 0.13715(7) 0.26674(7) 0.60911(3) 0.0314(2) Uani 1 1 d . . .

O3 O 0.32900(6) 0.43543(6) 0.42365(3) 0.02214(16) Uani 1 1 d . . .

O4 O 0.36779(7) 0.30589(7) 0.37077(3) 0.0330(2) Uani 1 1 d . . .

O5 O 0.39110(6) 0.44028(6) 0.54061(3) 0.02011(15) Uani 1 1 d . . .

O6 O 0.46612(6) 0.40014(6) 0.61423(3) 0.02096(15) Uani 1 1 d . . .

O7 O 0.10477(6) 0.45484(6) 0.44944(3) 0.02125(15) Uani 1 1 d . . .

O8 O 0.02511(6) 0.44387(7) 0.37447(3) 0.02638(17) Uani 1 1 d . . .

N1 N 0.24953(7) 0.31101(7) 0.49024(3) 0.01929(17) Uani 1 1 d . . .

N2 N 0.29395(7) 0.60795(7) 0.58080(3) 0.02096(18) Uani 1 1 d . . .

N3 N 0.38949(7) 0.63200(7) 0.48113(3) 0.02154(18) Uani 1 1 d . . .

H3 H 0.4382 0.5951 0.4635 0.026 Uiso 1 1 calc R . .

N4 N 0.20109(7) 0.63404(7) 0.42399(3) 0.02246(19) Uani 1 1 d . . .

N5 N 0.10617(7) 0.62484(7) 0.52448(3) 0.02112(18) Uani 1 1 d . . .

H5 H 0.0572 0.5826 0.5388 0.025 Uiso 1 1 calc R . .

C1 C 0.28980(9) 0.26650(9) 0.44944(4) 0.0217(2) Uani 1 1 d . . .

C2 C 0.29378(10) 0.15995(9) 0.44407(5) 0.0284(3) Uani 1 1 d . . .

H2 H 0.3216 0.1284 0.4146 0.034 Uiso 1 1 calc R . .

C3 C 0.25550(11) 0.10258(9) 0.48349(5) 0.0315(3) Uani 1 1 d . . .

C4 C 0.21443(10) 0.14617(9) 0.52633(5) 0.0285(3) Uani 1 1 d . . .

H4 H 0.1889 0.1054 0.5534 0.034 Uiso 1 1 calc R . .

C5 C 0.21228(8) 0.25337(9) 0.52788(4) 0.0213(2) Uani 1 1 d . . .

C6 C 0.33219(9) 0.34148(10) 0.41079(4) 0.0232(2) Uani 1 1 d . . .

C7 C 0.16930(9) 0.31506(9) 0.57189(4) 0.0228(2) Uani 1 1 d . . .

C8 C 0.36352(9) 0.69387(9) 0.56872(4) 0.0253(2) Uani 1 1 d . . .

H8A H 0.3995 0.7150 0.6003 0.030 Uiso 1 1 calc R . .

H8B H 0.3234 0.7535 0.5565 0.030 Uiso 1 1 calc R . .

C9 C 0.44064(9) 0.66611(9) 0.52859(4) 0.0242(2) Uani 1 1 d . . .

H9A H 0.4835 0.7268 0.5213 0.029 Uiso 1 1 calc R . .

H9B H 0.4849 0.6103 0.5416 0.029 Uiso 1 1 calc R . .

C10 C 0.36294(9) 0.71872(9) 0.44739(5) 0.0267(2) Uani 1 1 d . . .

H10A H 0.4252 0.7491 0.4332 0.032 Uiso 1 1 calc R . .

H10B H 0.3278 0.7727 0.4672 0.032 Uiso 1 1 calc R . .

C11 C 0.29493(9) 0.68162(10) 0.40432(4) 0.0261(2) Uani 1 1 d . . .

H11A H 0.2771 0.7406 0.3820 0.031 Uiso 1 1 calc R . .

H11B H 0.3318 0.6305 0.3835 0.031 Uiso 1 1 calc R . .

C12 C 0.13187(9) 0.71483(9) 0.44294(5) 0.0273(2) Uani 1 1 d . . .

H12A H 0.0956 0.7460 0.4135 0.033 Uiso 1 1 calc R . .

H12B H 0.1722 0.7697 0.4596 0.033 Uiso 1 1 calc R . .

C13 C 0.05535(9) 0.67441(9) 0.48042(4) 0.0245(2) Uani 1 1 d . . .

H13A H 0.0128 0.7320 0.4926 0.029 Uiso 1 1 calc R . .

H13B H 0.0108 0.6238 0.4631 0.029 Uiso 1 1 calc R . .

C14 C 0.13230(9) 0.69932(9) 0.56487(4) 0.0253(2) Uani 1 1 d . . .

H14A H 0.0699 0.7242 0.5814 0.030 Uiso 1 1 calc R . .

H14B H 0.1672 0.7593 0.5498 0.030 Uiso 1 1 calc R . .

C15 C 0.20035(9) 0.64874(9) 0.60426(4) 0.0241(2) Uani 1 1 d . . .

H15A H 0.2186 0.6997 0.6309 0.029 Uiso 1 1 calc R . .

H15B H 0.1635 0.5916 0.6208 0.029 Uiso 1 1 calc R . .

C16 C 0.34323(9) 0.53336(9) 0.61548(4) 0.0229(2) Uani 1 1 d . . .

H16A H 0.2906 0.4984 0.6357 0.027 Uiso 1 1 calc R . .

H16B H 0.3877 0.5713 0.6395 0.027 Uiso 1 1 calc R . .

C17 C 0.40570(8) 0.45205(8) 0.58814(4) 0.0183(2) Uani 1 1 d . . .

C18 C 0.15130(9) 0.57236(10) 0.38341(4) 0.0254(2) Uani 1 1 d . . .

H18A H 0.2038 0.5439 0.3607 0.031 Uiso 1 1 calc R . .

H18B H 0.1076 0.6183 0.3627 0.031 Uiso 1 1 calc R . .

C19 C 0.08745(8) 0.48375(9) 0.40378(4) 0.0210(2) Uani 1 1 d . . .

N6 N 0.36113(7) 0.27189(7) 0.22323(3) 0.01890(18) Uani 1 1 d . . .

C20 C 0.33137(9) 0.15899(8) 0.22249(4) 0.0210(2) Uani 1 1 d . . .

H20A H 0.3842 0.1198 0.2043 0.025 Uiso 1 1 calc R . .

H20B H 0.2677 0.1518 0.2027 0.025 Uiso 1 1 calc R . .

C21 C 0.31678(11) 0.11070(9) 0.27471(5) 0.0298(3) Uani 1 1 d . . .

H21A H 0.3799 0.1173 0.2950 0.036 Uiso 1 1 calc R . .

H21B H 0.2626 0.1476 0.2930 0.036 Uiso 1 1 calc R . .

C22 C 0.28912(10) -0.00151(9) 0.26958(5) 0.0312(2) Uani 1 1 d . . .

H22A H 0.3445 -0.0384 0.2522 0.037 Uiso 1 1 calc R . .

H22B H 0.2276 -0.0078 0.2481 0.037 Uiso 1 1 calc R . .

C23 C 0.27019(12) -0.05206(11) 0.32085(5) 0.0382(3) Uani 1 1 d . . .

H23A H 0.3320 -0.0490 0.3417 0.057 Uiso 1 1 calc R . .

H23B H 0.2507 -0.1242 0.3156 0.057 Uiso 1 1 calc R . .

H23C H 0.2157 -0.0156 0.3383 0.057 Uiso 1 1 calc R . .

C24 C 0.45819(8) 0.28750(9) 0.25352(4) 0.0215(2) Uani 1 1 d . . .

H24A H 0.4464 0.2653 0.2891 0.026 Uiso 1 1 calc R . .

H24B H 0.4736 0.3621 0.2543 0.026 Uiso 1 1 calc R . .

C25 C 0.55021(9) 0.23088(10) 0.23371(4) 0.0260(2) Uani 1 1 d . . .

H25A H 0.5769 0.2674 0.2036 0.031 Uiso 1 1 calc R . .

H25B H 0.5306 0.1605 0.2230 0.031 Uiso 1 1 calc R . .

C26 C 0.63185(10) 0.22477(9) 0.27490(5) 0.0272(3) Uani 1 1 d . . .

H26A H 0.6489 0.2954 0.2864 0.033 Uiso 1 1 calc R . .

H26B H 0.6049 0.1868 0.3046 0.033 Uiso 1 1 calc R . .

C27 C 0.72713(10) 0.17206(11) 0.25704(5) 0.0364(3) Uani 1 1 d . . .

H27A H 0.7099 0.1049 0.2423 0.055 Uiso 1 1 calc R . .

H27B H 0.7733 0.1624 0.2861 0.055 Uiso 1 1 calc R . .

H27C H 0.7599 0.2148 0.2312 0.055 Uiso 1 1 calc R . .

C28 C 0.37443(9) 0.30422(8) 0.16811(4) 0.0208(2) Uani 1 1 d . . .

H28A H 0.3124 0.2854 0.1489 0.025 Uiso 1 1 calc R . .

H28B H 0.4308 0.2640 0.1536 0.025 Uiso 1 1 calc R . .

C29 C 0.39547(10) 0.41770(9) 0.15935(4) 0.0261(2) Uani 1 1 d . . .

H29A H 0.4457 0.4425 0.1847 0.031 Uiso 1 1 calc R . .

H29B H 0.3325 0.4578 0.1637 0.031 Uiso 1 1 calc R . .

C30 C 0.43582(10) 0.43382(9) 0.10573(5) 0.0293(3) Uani 1 1 d . . .

H30A H 0.3919 0.3967 0.0811 0.035 Uiso 1 1 calc R . .

H30B H 0.5045 0.4039 0.1036 0.035 Uiso 1 1 calc R . .

C31 C 0.44025(14) 0.54728(12) 0.09082(6) 0.0482(4) Uani 1 1 d . . .

H31A H 0.3718 0.5762 0.0906 0.072 Uiso 1 1 calc R . .

H31B H 0.4694 0.5538 0.0567 0.072 Uiso 1 1 calc R . .

H31C H 0.4824 0.5848 0.1155 0.072 Uiso 1 1 calc R . .

C32 C 0.27977(8) 0.33650(9) 0.24884(4) 0.0215(2) Uani 1 1 d . . .

H32A H 0.2779 0.3181 0.2855 0.026 Uiso 1 1 calc R . .

H32B H 0.2992 0.4100 0.2465 0.026 Uiso 1 1 calc R . .

C33 C 0.17460(9) 0.32396(10) 0.22652(5) 0.0261(2) Uani 1 1 d . . .

H33A H 0.1520 0.2518 0.2310 0.031 Uiso 1 1 calc R . .

H33B H 0.1759 0.3389 0.1895 0.031 Uiso 1 1 calc R . .

C34 C 0.10040(10) 0.39602(11) 0.25231(5) 0.0363(3) Uani 1 1 d . . .

H34A H 0.1194 0.4683 0.2450 0.044 Uiso 1 1 calc R . .

H34B H 0.1040 0.3857 0.2897 0.044 Uiso 1 1 calc R . .

C35 C -0.00718(11) 0.37672(13) 0.23364(6) 0.0466(4) Uani 1 1 d . . .

H35A H -0.0108 0.3868 0.1966 0.070 Uiso 1 1 calc R . .

H35B H -0.0532 0.4250 0.2504 0.070 Uiso 1 1 calc R . .

H35C H -0.0269 0.3059 0.2419 0.070 Uiso 1 1 calc R . .

O41 O 0.57662(7) 0.50828(6) 0.68541(3) 0.02834(18) Uani 1 1 d . . .

H41A H 0.5465 0.4709 0.6646 0.034 Uiso 1 1 d R . .

H41B H 0.5905 0.5642 0.6685 0.034 Uiso 1 1 d R . .

O42 O 0.91363(8) 0.58532(7) 0.31289(3) 0.0374(2) Uani 1 1 d . . .

H42A H 0.9429 0.5399 0.3285 0.045 Uiso 1 1 d R . .

H42B H 0.8968 0.6263 0.3367 0.045 Uiso 1 1 d R . .

O51 O 0.14220(9) 0.94565(10) 0.62466(5) 0.0567(3) Uani 1 1 d . . .

C51 C 0.00168(14) 0.86546(15) 0.66482(7) 0.0611(5) Uani 1 1 d . . .

H51A H 0.0520 0.8215 0.6817 0.092 Uiso 1 1 calc R . .

H51B H -0.0494 0.8222 0.6480 0.092 Uiso 1 1 calc R . .

H51C H -0.0309 0.9095 0.6902 0.092 Uiso 1 1 calc R . .

C52 C 0.05251(13) 0.93127(14) 0.62585(6) 0.0519(4) Uani 1 1 d . . .

C53 C -0.01485(19) 0.9784(3) 0.58586(10) 0.1211(12) Uani 1 1 d . . .

H53A H -0.0308 1.0495 0.5954 0.182 Uiso 1 1 calc R . .

H53B H -0.0775 0.9384 0.5831 0.182 Uiso 1 1 calc R . .

H53C H 0.0197 0.9779 0.5530 0.182 Uiso 1 1 calc R . .

 


 

_geom_special_details

;

 All esds (except the esd in the dihedral angle between two l.s. planes)

 are estimated using the full covariance matrix.  The cell esds are taken

 into account individually in the estimation of esds in distances, angles

 and torsion angles; correlations between esds in cell parameters are only

 used when they are defined by crystal symmetry.  An approximate (isotropic)

 treatment of cell esds is used for estimating esds involving l.s. planes.

;

 

loop_

 _geom_bond_atom_site_label_1

 _geom_bond_atom_site_label_2

 _geom_bond_distance

 _geom_bond_site_symmetry_2

 _geom_bond_publ_flag

Tb1 O7 2.3392(8) . yes

Tb1 O5 2.3492(7) . yes

Tb1 O1 2.3835(7) . yes

Tb1 O3 2.3889(8) . yes

Tb1 N1 2.4924(9) . yes

Tb1 N5 2.5562(9) . yes

Tb1 N3 2.5634(9) . yes

Tb1 N4 2.6409(9) . yes

Tb1 N2 2.6476(9) . yes

Cl1 C3 1.676(2) . ?

F1 C3 1.309(6) . ?

O1 C7 1.2683(14) . ?

O2 C7 1.2385(13) . ?

O3 C6 1.2662(14) . ?

O4 C6 1.2430(13) . ?

O5 C17 1.2681(12) . ?

O6 C17 1.2455(12) . ?

O7 C19 1.2731(12) . ?

O8 C19 1.2358(13) . ?

N1 C1 1.3312(14) . ?

N1 C5 1.3362(14) . ?

N2 C16 1.4759(14) . ?

N2 C8 1.4822(15) . ?

N2 C15 1.4854(15) . ?

N3 C10 1.4722(14) . ?

N3 C9 1.4788(14) . ?

N4 C18 1.4812(15) . ?

N4 C12 1.4812(15) . ?

N4 C11 1.4834(15) . ?

N5 C14 1.4726(15) . ?

N5 C13 1.4786(14) . ?

C1 C2 1.3913(16) . ?

C1 C6 1.5163(16) . ?

C2 C3 1.3741(18) . ?

C3 C4 1.3740(18) . ?

C4 C5 1.3924(16) . ?

C5 C7 1.5190(17) . ?

C8 C9 1.5157(17) . ?

C10 C11 1.5158(17) . ?

C12 C13 1.5114(17) . ?

C14 C15 1.5136(16) . ?

C16 C17 1.5237(16) . ?

C18 C19 1.5267(16) . ?

N6 C28 1.5163(14) . ?

N6 C24 1.5172(14) . ?

N6 C20 1.5176(14) . ?

N6 C32 1.5254(14) . ?

C20 C21 1.5195(16) . ?

C21 C22 1.5076(17) . ?

C22 C23 1.5185(18) . ?

C24 C25 1.5179(16) . ?

C25 C26 1.5223(17) . ?

C26 C27 1.5126(18) . ?

C28 C29 1.5171(16) . ?

C29 C30 1.5225(17) . ?

C30 C31 1.525(2) . ?

C32 C33 1.5135(16) . ?

C33 C34 1.5191(17) . ?

C34 C35 1.5219(19) . ?

O51 C52 1.202(2) . ?

C51 C52 1.496(3) . ?

C52 C53 1.500(3) . ?

 

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 Tb1 O5 144.47(3) . . yes

O7 Tb1 O1 85.65(3) . . yes

O5 Tb1 O1 79.68(3) . . yes

O7 Tb1 O3 80.64(3) . . yes

O5 Tb1 O3 83.90(3) . . yes

O1 Tb1 O3 129.13(3) . . yes

O7 Tb1 N1 72.93(3) . . yes

O5 Tb1 N1 71.54(3) . . yes

O1 Tb1 N1 64.62(3) . . yes

O3 Tb1 N1 64.52(3) . . yes

O7 Tb1 N5 74.14(3) . . yes

O5 Tb1 N5 132.09(3) . . yes

O1 Tb1 N5 77.12(3) . . yes

O3 Tb1 N5 142.03(3) . . yes

N1 Tb1 N5 130.57(3) . . yes

O7 Tb1 N3 132.31(3) . . yes

O5 Tb1 N3 73.28(3) . . yes

O1 Tb1 N3 140.40(3) . . yes

O3 Tb1 N3 76.41(3) . . yes

N1 Tb1 N3 129.19(3) . . yes

N5 Tb1 N3 100.23(3) . . yes

O7 Tb1 N4 66.38(3) . . yes

O5 Tb1 N4 138.96(3) . . yes

O1 Tb1 N4 140.26(3) . . yes

O3 Tb1 N4 75.45(3) . . yes

N1 Tb1 N4 126.36(3) . . yes

N5 Tb1 N4 68.64(3) . . yes

N3 Tb1 N4 67.62(3) . . yes

O7 Tb1 N2 139.59(3) . . yes

O5 Tb1 N2 66.28(3) . . yes

O1 Tb1 N2 74.50(3) . . yes

O3 Tb1 N2 138.80(3) . . yes

N1 Tb1 N2 125.11(3) . . yes

N5 Tb1 N2 67.36(3) . . yes

N3 Tb1 N2 68.39(3) . . yes

N4 Tb1 N2 108.52(3) . . yes

C7 O1 Tb1 125.80(7) . . ?

C6 O3 Tb1 125.65(7) . . ?

C17 O5 Tb1 123.19(7) . . ?

C19 O7 Tb1 124.39(7) . . ?

C1 N1 C5 120.22(10) . . ?

C1 N1 Tb1 119.92(7) . . ?

C5 N1 Tb1 119.84(7) . . ?

C16 N2 C8 110.70(9) . . ?

C16 N2 C15 110.13(9) . . ?

C8 N2 C15 110.00(9) . . ?

C16 N2 Tb1 105.52(6) . . ?

C8 N2 Tb1 110.72(6) . . ?

C15 N2 Tb1 109.68(6) . . ?

C10 N3 C9 112.41(9) . . ?

C10 N3 Tb1 115.48(7) . . ?

C9 N3 Tb1 112.80(7) . . ?

C18 N4 C12 110.56(9) . . ?

C18 N4 C11 110.10(9) . . ?

C12 N4 C11 110.11(9) . . ?

C18 N4 Tb1 105.79(6) . . ?

C12 N4 Tb1 110.67(6) . . ?

C11 N4 Tb1 109.52(7) . . ?

C14 N5 C13 112.21(9) . . ?

C14 N5 Tb1 116.13(7) . . ?

C13 N5 Tb1 112.44(7) . . ?

N1 C1 C2 121.91(11) . . ?

N1 C1 C6 114.30(10) . . ?

C2 C1 C6 123.78(10) . . ?

C3 C2 C1 116.63(11) . . ?

F1 C3 C4 119.4(3) . . ?

F1 C3 C2 117.5(2) . . ?

C4 C3 C2 122.86(11) . . ?

F1 C3 Cl1 8.1(2) . . ?

C4 C3 Cl1 118.84(11) . . ?

C2 C3 Cl1 118.20(11) . . ?

C3 C4 C5 116.35(11) . . ?

N1 C5 C4 122.02(11) . . ?

N1 C5 C7 114.13(10) . . ?

C4 C5 C7 123.85(10) . . ?

O4 C6 O3 126.63(11) . . ?

O4 C6 C1 118.09(11) . . ?

O3 C6 C1 115.27(9) . . ?

O2 C7 O1 127.06(11) . . ?

O2 C7 C5 117.71(10) . . ?

O1 C7 C5 115.23(9) . . ?

N2 C8 C9 113.13(9) . . ?

N3 C9 C8 110.43(9) . . ?

N3 C10 C11 109.95(9) . . ?

N4 C11 C10 111.51(9) . . ?

N4 C12 C13 113.09(9) . . ?

N5 C13 C12 110.87(9) . . ?

N5 C14 C15 109.87(9) . . ?

N2 C15 C14 111.42(9) . . ?

N2 C16 C17 113.78(9) . . ?

O6 C17 O5 124.44(10) . . ?

O6 C17 C16 117.70(9) . . ?

O5 C17 C16 117.85(9) . . ?

N4 C18 C19 113.58(9) . . ?

O8 C19 O7 125.07(11) . . ?

O8 C19 C18 117.80(9) . . ?

O7 C19 C18 117.10(9) . . ?

C28 N6 C24 110.89(8) . . ?

C28 N6 C20 106.70(8) . . ?

C24 N6 C20 110.73(8) . . ?

C28 N6 C32 110.84(8) . . ?

C24 N6 C32 107.08(8) . . ?

C20 N6 C32 110.64(8) . . ?

N6 C20 C21 114.96(9) . . ?

C22 C21 C20 110.55(10) . . ?

C21 C22 C23 112.37(11) . . ?

N6 C24 C25 115.73(9) . . ?

C24 C25 C26 110.42(9) . . ?

C27 C26 C25 113.09(10) . . ?

N6 C28 C29 115.86(9) . . ?

C28 C29 C30 109.86(9) . . ?

C29 C30 C31 112.58(11) . . ?

C33 C32 N6 114.90(9) . . ?

C32 C33 C34 110.95(9) . . ?

C33 C34 C35 111.23(11) . . ?

O51 C52 C51 123.83(17) . . ?

O51 C52 C53 119.93(18) . . ?

C51 C52 C53 116.22(17) . . ?

 

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 2.31 3.1089(12) 144.0 3_666

N3 H3 O6  0.93 2.41 3.1876(12) 141.2 3_666

N5 H5 O7  0.93 2.22 3.0600(12) 149.4 3_566

N5 H5 O8  0.93 2.55 3.3037(12) 137.9 3_566

O41 H41A O6  0.83 1.92 2.7457(11) 172.4 .

O41 H41B O4  0.87 2.05 2.9239(12) 176.6 3_666

O42 H42A O8  0.81 2.04 2.8477(12) 171.1 1_655

O42 H42B O2  0.85 2.04 2.8888(13) 175.5 3_666

 

_diffrn_measured_fraction_theta_max    0.962

_diffrn_reflns_theta_full              39.88

_diffrn_measured_fraction_theta_full   0.962

_refine_diff_density_max    2.226

_refine_diff_density_min   -1.457

_refine_diff_density_rms    0.091

