#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/96/7219694.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7219694
loop_
_publ_author_name
'Zhang, Lina'
'Zhang, Chao'
'Zhang, Bin'
'Du, Chenxia'
'Hou, Hongwei'
_publ_section_title
;
 Two series of pH-dependent lanthanide complexes showing solvent-induced
 single crystal to single crystal transformation, sorption and
 luminescence properties
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2837
_journal_paper_doi               10.1039/C5CE00263J
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety
'C73.5 H53 N1.5 O22 Tb2, C3 H6 N O, C3 H7 N O'
_chemical_formula_sum            'C79.5 H71.5 N3.5 O24 Tb2'
_chemical_formula_weight         1777.19
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2012.05.09 svn.r2324, GUI svn.r4862)
;
_audit_update_record
;
2015-01-16 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.034(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0878(3)
_cell_length_b                   29.4702(7)
_cell_length_c                   18.4237(4)
_cell_measurement_reflns_used    10302
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      29.2273
_cell_measurement_theta_min      2.8986
_cell_volume                     7313.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -24.00    5.00   1.0000   54.8200
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000   30.0000 29

  2 omega  -13.00   25.00   1.0000   54.8200
omega____ theta____ kappa____ phi______ frames
    -      -17.1323  -99.0000 -150.0000 38

  3 omega   32.00   80.00   1.0000   54.8200
omega____ theta____ kappa____ phi______ frames
    -       19.7104 -178.0000   90.0000 48

  4 omega  -38.00   79.00   1.0000   54.8200
omega____ theta____ kappa____ phi______ frames
    -       19.7104    0.0000    0.0000 117
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0320665000
_diffrn_orient_matrix_UB_12      -0.0173461000
_diffrn_orient_matrix_UB_13      -0.0199735000
_diffrn_orient_matrix_UB_21      -0.0411708000
_diffrn_orient_matrix_UB_22      0.0148196000
_diffrn_orient_matrix_UB_23      -0.0054474000
_diffrn_orient_matrix_UB_31      0.0070450000
_diffrn_orient_matrix_UB_32      0.0076850000
_diffrn_orient_matrix_UB_33      -0.0345276000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31944
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    2.002
_exptl_absorpt_correction_T_max  0.74580
_exptl_absorpt_correction_T_min  0.67933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3558
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         15387
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0356P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                11260
_reflns_number_total             15387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00263j2.cif
_cod_data_source_block           Tb-p21c
_cod_depositor_comments
'Adding full bibliography for 7219688--7219700.cif.'
_cod_original_formula_sum        'C79.50 H71.5 N3.50 O24 Tb2'
_cod_database_code               7219694
#BEGIN Tags that were not found in dictionaries:
_chemical_oxdiff_formula         C30H30O6N2Tb2
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_submission_special_instructions 'No special instructions were received'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'
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 0.313139(9) 0.743645(5) 0.678142(7) 0.02092(4) Uani 1 1 d U . .
Tb2 Tb 0.173202(9) 0.670476(5) 0.826499(8) 0.02284(4) Uani 1 1 d U . .
O1 O 0.29875(15) 0.81640(7) 0.61125(11) 0.0360(6) Uani 1 1 d . . .
O24 O 0.2089(4) 0.63549(18) 0.4974(4) 0.179(3) Uiso 0.734(5) 1 d PD A 1
O2 O 0.41288(15) 0.81322(7) 0.72161(11) 0.0333(6) Uani 1 1 d . . .
O3 O 0.54219(16) 0.87624(8) 0.76377(11) 0.0397(6) Uani 1 1 d . . .
H3 H 0.5124 0.8527 0.7663 0.060 Uiso 1 1 calc R . .
O4 O 0.31008(16) 0.66474(7) 0.67741(11) 0.0379(6) Uani 1 1 d . . .
O5 O 0.25140(15) 0.62426(7) 0.75682(11) 0.0378(6) Uani 1 1 d . . .
O6 O 0.27303(16) 0.53831(8) 0.76491(14) 0.0571(7) Uani 1 1 d . . .
H6 H 0.2552 0.5635 0.7748 0.086 Uiso 1 1 calc R . .
O7 O 0.34482(14) 0.68224(8) 0.87700(12) 0.0409(7) Uani 1 1 d . . .
O8 O 0.40708(15) 0.72299(8) 0.80017(11) 0.0380(6) Uani 1 1 d U . .
O9 O 0.59118(15) 0.74164(9) 0.83572(11) 0.0497(7) Uani 1 1 d . . .
H9 H 0.5344 0.7388 0.8076 0.074 Uiso 1 1 calc R . .
O10 O 0.11492(17) 0.69551(9) 0.70318(12) 0.0492(7) Uani 1 1 d . . .
O11 O 0.14057(14) 0.74126(8) 0.61619(12) 0.0421(7) Uani 1 1 d . . .
O12 O -0.01258(14) 0.77173(8) 0.51053(12) 0.0381(6) Uani 1 1 d . . .
H12 H 0.0423 0.7736 0.5418 0.057 Uiso 1 1 calc R . .
O13 O 0.17471(16) 0.74842(7) 0.83614(11) 0.0375(6) Uani 1 1 d . . .
O14 O 0.24125(14) 0.78559(7) 0.75778(11) 0.0357(6) Uani 1 1 d U . .
O15 O 0.24668(15) 0.87394(8) 0.77308(13) 0.0450(6) Uani 1 1 d . . .
H15 H 0.2610 0.8496 0.7573 0.068 Uiso 1 1 calc R . .
O16 O 0.16273(15) 0.60031(7) 0.89095(11) 0.0379(6) Uani 1 1 d . . .
O17 O 0.06149(15) 0.60498(8) 0.77554(11) 0.0372(6) Uani 1 1 d . . .
O18 O -0.05028(16) 0.53807(8) 0.71584(11) 0.0395(6) Uani 1 1 d . . .
H18 H -0.0253 0.5634 0.7196 0.059 Uiso 1 1 calc R . .
O19 O 0.28530(17) 0.72423(8) 0.54294(11) 0.0448(7) Uani 1 1 d DU . .
O20 O 0.01159(15) 0.68706(9) 0.84293(13) 0.0498(7) Uani 1 1 d U . .
H20A H 0.0176 0.6972 0.8890 0.075 Uiso 1 1 d R . .
H20B H -0.0254 0.6625 0.8359 0.075 Uiso 1 1 d R . .
O21 O 0.19421(15) 0.69325(8) 0.95869(10) 0.0393(6) Uani 1 1 d . . .
H21A H 0.2001 0.7223 0.9630 0.059 Uiso 1 1 d R . .
H21B H 0.2469 0.6808 0.9879 0.059 Uiso 1 1 d R . .
O22 O 0.46963(15) 0.73228(9) 0.65847(12) 0.0474(7) Uani 1 1 d . . .
O23 O 0.1674(2) 0.35371(12) 0.19604(17) 0.0830(11) Uani 1 1 d . . .
N1 N 0.6322(2) 0.72811(12) 0.66573(16) 0.0517(8) Uani 1 1 d U . .
N2 N 0.3742(5) 0.6817(3) 0.4766(4) 0.103(2) Uani 0.50 1 d PDU . .
N3 N 0.2686(2) 0.41221(12) 0.19215(18) 0.0631(10) Uani 1 1 d . . .
N4 N 0.1393(3) 0.57372(14) 0.5242(2) 0.1152(16) Uiso 1 1 d D A .
C1 C 0.3712(2) 0.83486(10) 0.66159(16) 0.0268(8) Uani 1 1 d . . .
C1B C 0.5490(5) 0.4751(3) 0.5930(4) 0.0467(14) Uani 0.490(3) 1 d PU B 1
H1B H 0.5743 0.4492 0.5765 0.056 Uiso 0.490(3) 1 calc PR B 1
C2 C 0.4060(2) 0.88112(10) 0.64866(15) 0.0269(8) Uani 1 1 d . . .
C3 C 0.3564(2) 0.90567(11) 0.58538(16) 0.0323(9) Uani 1 1 d . . .
H3A H 0.3012 0.8930 0.5506 0.039 Uiso 1 1 calc R . .
C4 C 0.3869(2) 0.94911(11) 0.57210(17) 0.0352(9) Uani 1 1 d . . .
C5 C 0.3354(2) 0.97386(11) 0.50697(19) 0.0460(10) Uani 1 1 d D . .
H5 H 0.2831 0.9602 0.4706 0.055 Uiso 1 1 calc R . .
C6 C 0.3608(3) 1.01744(12) 0.4962(2) 0.0522(11) Uani 1 1 d D . .
H6A H 0.3234 1.0342 0.4549 0.063 Uiso 1 1 calc R . .
C7 C 0.4435(3) 1.03644(12) 0.54810(19) 0.0508(11) Uani 1 1 d U . .
H7 H 0.4622 1.0658 0.5402 0.061 Uiso 1 1 calc R . .
C8 C 0.4975(2) 1.01323(12) 0.60994(17) 0.0409(9) Uani 1 1 d U . .
H8 H 0.5533 1.0268 0.6427 0.049 Uiso 1 1 calc R . .
C9 C 0.4712(2) 0.96891(11) 0.62577(16) 0.0303(8) Uani 1 1 d . . .
C10 C 0.5240(2) 0.94329(10) 0.69094(16) 0.0278(8) Uani 1 1 d . . .
C11 C 0.4905(2) 0.90042(11) 0.70187(16) 0.0276(8) Uani 1 1 d . . .
C12 C 0.3004(2) 0.62813(11) 0.70917(16) 0.0293(8) Uani 1 1 d . . .
C13 C 0.3498(2) 0.58619(11) 0.69199(15) 0.0282(8) Uani 1 1 d U B .
C14 C 0.3374(2) 0.54300(11) 0.72240(17) 0.0324(8) Uani 1 1 d . . .
C15 C 0.3904(2) 0.50557(11) 0.71315(16) 0.0294(8) Uani 1 1 d . . .
C16 C 0.4540(2) 0.50913(12) 0.66739(17) 0.0365(9) Uani 1 1 d . . .
C17 C 0.5088(3) 0.47068(13) 0.65301(19) 0.0496(10) Uani 1 1 d U B .
H17A H 0.4887 0.4416 0.6612 0.059 Uiso 0.510(3) 1 calc PR B 2
H17 H 0.5169 0.4444 0.6822 0.059 Uiso 0.490(3) 1 calc PR B 1
C18A C 0.5940(5) 0.4765(3) 0.6262(4) 0.0467(14) Uani 0.510(3) 1 d PU B 2
H18A H 0.6350 0.4520 0.6247 0.056 Uiso 0.510(3) 1 calc PR B 2
C19 C 0.5539(5) 0.5145(3) 0.5570(4) 0.0513(9) Uani 0.490(3) 1 d PU B 1
H19 H 0.5904 0.5159 0.5223 0.062 Uiso 0.490(3) 1 calc PR B 1
C19A C 0.6144(5) 0.5195(3) 0.6025(4) 0.0513(9) Uani 0.510(3) 1 d PU B 2
H19A H 0.6661 0.5231 0.5811 0.062 Uiso 0.510(3) 1 calc PR B 2
C20 C 0.5062(5) 0.5520(3) 0.5708(4) 0.0509(7) Uani 0.490(3) 1 d PU B 1
H20 H 0.5076 0.5786 0.5440 0.061 Uiso 0.490(3) 1 calc PR B 1
C20A C 0.5590(5) 0.5563(3) 0.6106(4) 0.0509(7) Uani 0.510(3) 1 d PU B 2
H20C H 0.5735 0.5845 0.5937 0.061 Uiso 0.510(3) 1 calc PR B 2
C21 C 0.4534(6) 0.5507(3) 0.6271(4) 0.0474(8) Uani 0.490(3) 1 d PU B 1
C21A C 0.4787(6) 0.5528(3) 0.6444(4) 0.0474(8) Uani 0.510(3) 1 d PU B 2
C22 C 0.4150(3) 0.58929(12) 0.64988(19) 0.0466(10) Uani 1 1 d U . .
H22 H 0.4336 0.6177 0.6366 0.056 Uiso 0.490(3) 1 calc PR B 1
H22A H 0.4178 0.6161 0.6240 0.056 Uiso 0.510(3) 1 calc PR B 2
C23 C 0.6191(2) 0.96121(11) 0.74698(17) 0.0314(8) Uani 1 1 d . . .
H23A H 0.6444 0.9382 0.7854 0.038 Uiso 1 1 calc R . .
H23B H 0.6681 0.9654 0.7200 0.038 Uiso 1 1 calc R . .
C24 C 0.4160(2) 0.70008(11) 0.86027(17) 0.0322(9) Uani 1 1 d U . .
C25 C 0.5196(2) 0.69500(11) 0.91444(16) 0.0290(8) Uani 1 1 d . . .
C26 C 0.5334(2) 0.66923(11) 0.97819(16) 0.0293(8) Uani 1 1 d . . .
H26 H 0.4786 0.6564 0.9889 0.035 Uiso 1 1 calc R . .
C27 C 0.6294(2) 0.66164(11) 1.02839(16) 0.0298(8) Uani 1 1 d . . .
C28 C 0.6450(2) 0.63340(12) 1.09213(17) 0.0395(10) Uani 1 1 d . . .
H28 H 0.5904 0.6206 1.1031 0.047 Uiso 1 1 calc R . .
C29 C 0.7373(3) 0.62418(13) 1.13812(18) 0.0470(11) Uani 1 1 d . . .
H29 H 0.7455 0.6056 1.1803 0.056 Uiso 1 1 calc R . .
C30 C 0.8202(2) 0.64279(13) 1.12166(17) 0.0436(10) Uani 1 1 d . . .
H30 H 0.8837 0.6360 1.1525 0.052 Uiso 1 1 calc R . .
C31 C 0.8084(2) 0.67078(11) 1.06058(17) 0.0334(9) Uani 1 1 d . . .
H31 H 0.8644 0.6829 1.0508 0.040 Uiso 1 1 calc R . .
C32 C 0.7132(2) 0.68194(11) 1.01157(15) 0.0267(8) Uani 1 1 d . . .
C33 C 0.69821(19) 0.71089(11) 0.94788(15) 0.0251(8) Uani 1 1 d . . .
C34 C 0.6027(2) 0.71585(11) 0.89904(15) 0.0293(8) Uani 1 1 d . . .
C35 C 0.0846(2) 0.71495(11) 0.64030(17) 0.0324(9) Uani 1 1 d . . .
C36 C -0.0171(2) 0.70680(11) 0.59087(15) 0.0287(8) Uani 1 1 d . . .
C37 C -0.0677(2) 0.66956(12) 0.60318(17) 0.0362(9) Uani 1 1 d . . .
H37 H -0.0389 0.6511 0.6447 0.043 Uiso 1 1 calc R . .
C38 C -0.1618(2) 0.65830(12) 0.55519(17) 0.0359(9) Uani 1 1 d . . .
C39 C -0.2074(2) 0.61595(13) 0.5607(2) 0.0522(11) Uani 1 1 d . . .
H39 H -0.1761 0.5955 0.5985 0.063 Uiso 1 1 calc R . .
C40 C -0.2965(3) 0.60523(15) 0.5110(2) 0.0652(12) Uani 1 1 d . . .
H40 H -0.3248 0.5770 0.5135 0.078 Uiso 1 1 calc R . .
C41 C -0.3451(3) 0.63623(14) 0.4567(2) 0.0582(12) Uani 1 1 d . . .
H41 H -0.4070 0.6288 0.4240 0.070 Uiso 1 1 calc R . .
C42 C -0.3054(2) 0.67719(13) 0.44974(19) 0.0432(10) Uani 1 1 d . . .
H42 H -0.3406 0.6974 0.4129 0.052 Uiso 1 1 calc R . .
C43 C -0.2103(2) 0.68971(11) 0.49804(16) 0.0283(8) Uani 1 1 d . . .
C44 C -0.16190(19) 0.73030(11) 0.48767(15) 0.0253(8) Uani 1 1 d . . .
C45 C -0.06331(19) 0.73616(11) 0.52893(15) 0.0258(8) Uani 1 1 d . . .
C46 C 0.7852(2) 0.73388(11) 0.92979(15) 0.0288(8) Uani 1 1 d . . .
H46A H 0.7614 0.7481 0.8803 0.035 Uiso 1 1 calc R . .
H46B H 0.8330 0.7108 0.9266 0.035 Uiso 1 1 calc R . .
C47 C 0.1859(2) 0.78369(11) 0.80074(16) 0.0267(7) Uani 1 1 d U . .
C48 C 0.1317(2) 0.82492(10) 0.80993(16) 0.0285(8) Uani 1 1 d . . .
C49 C 0.0455(2) 0.82139(12) 0.83078(17) 0.0365(9) Uani 1 1 d . . .
H49 H 0.0254 0.7928 0.8417 0.044 Uiso 1 1 calc R . .
C50 C -0.0126(2) 0.85877(12) 0.83626(17) 0.0366(9) Uani 1 1 d . . .
C51 C -0.1018(2) 0.85461(14) 0.8576(2) 0.0558(11) Uani 1 1 d . . .
H51 H -0.1222 0.8260 0.8685 0.067 Uiso 1 1 calc R . .
C52 C -0.1570(3) 0.89114(15) 0.8624(2) 0.0637(12) Uani 1 1 d . . .
H52 H -0.2153 0.8876 0.8758 0.076 Uiso 1 1 calc R . .
C53 C -0.1267(3) 0.93402(14) 0.84739(19) 0.0535(11) Uani 1 1 d . . .
H53 H -0.1652 0.9591 0.8509 0.064 Uiso 1 1 calc R . .
C54 C -0.0412(2) 0.94004(12) 0.82744(18) 0.0423(10) Uani 1 1 d . . .
H54 H -0.0217 0.9692 0.8189 0.051 Uiso 1 1 calc R . .
C55 C 0.0180(2) 0.90264(11) 0.81963(16) 0.0316(8) Uani 1 1 d . . .
C56 C 0.1055(2) 0.90749(11) 0.79648(16) 0.0295(8) Uani 1 1 d . . .
C57 C 0.1594(2) 0.86915(11) 0.79302(17) 0.0304(8) Uani 1 1 d . . .
C58 C 0.0948(2) 0.58322(11) 0.83812(17) 0.0313(8) Uani 1 1 d . . .
C59 C 0.0523(2) 0.53790(11) 0.84597(16) 0.0287(8) Uani 1 1 d . . .
C60 C 0.0833(2) 0.51525(11) 0.91389(17) 0.0361(9) Uani 1 1 d . . .
H60 H 0.1317 0.5284 0.9539 0.043 Uiso 1 1 calc R . .
C61 C 0.0442(2) 0.47279(12) 0.92511(17) 0.0376(9) Uani 1 1 d . . .
C62 C 0.0784(3) 0.44941(13) 0.99554(19) 0.0499(11) Uani 1 1 d . . .
H62 H 0.1297 0.4617 1.0345 0.060 Uiso 1 1 calc R . .
C63 C 0.0369(3) 0.40910(14) 1.0066(2) 0.0580(12) Uani 1 1 d . . .
H63 H 0.0615 0.3933 1.0519 0.070 Uiso 1 1 calc R . .
C64 C -0.0426(3) 0.39198(13) 0.9491(2) 0.0547(11) Uani 1 1 d . . .
H64 H -0.0731 0.3654 0.9578 0.066 Uiso 1 1 calc R . .
C65 C -0.0772(2) 0.41284(12) 0.88063(18) 0.0396(9) Uani 1 1 d . . .
H65 H -0.1307 0.4004 0.8437 0.048 Uiso 1 1 calc R . .
C66 C -0.0327(2) 0.45349(11) 0.86476(17) 0.0308(8) Uani 1 1 d . . .
C67 C -0.0629(2) 0.47572(11) 0.79276(16) 0.0292(8) Uani 1 1 d . . .
C68 C -0.0203(2) 0.51655(11) 0.78546(16) 0.0299(8) Uani 1 1 d . . .
C69 C 0.1370(2) 0.95330(11) 0.77413(17) 0.0330(8) Uani 1 1 d . . .
H69A H 0.1492 0.9735 0.8175 0.040 Uiso 1 1 calc R . .
H69B H 0.1992 0.9496 0.7622 0.040 Uiso 1 1 calc R . .
C70 C 0.5539(2) 0.74929(14) 0.67037(19) 0.0455(10) Uani 1 1 d . . .
H70 H 0.5610 0.7798 0.6837 0.055 Uiso 1 1 calc R . .
C71 C 0.6266(3) 0.68071(16) 0.6458(3) 0.0837(13) Uani 1 1 d U . .
H71A H 0.6022 0.6776 0.5916 0.126 Uiso 1 1 calc R . .
H71B H 0.5824 0.6655 0.6687 0.126 Uiso 1 1 calc R . .
H71C H 0.6915 0.6674 0.6636 0.126 Uiso 1 1 calc R . .
C72 C 0.7288(3) 0.74876(16) 0.6838(2) 0.0732(14) Uani 1 1 d U . .
H72A H 0.7756 0.7305 0.7206 0.110 Uiso 1 1 calc R . .
H72B H 0.7260 0.7785 0.7044 0.110 Uiso 1 1 calc R . .
H72C H 0.7492 0.7511 0.6387 0.110 Uiso 1 1 calc R . .
C73 C 0.3119(6) 0.6918(3) 0.5177(5) 0.108(3) Uani 0.50 1 d PDU . .
C74 C 0.4263(6) 0.7132(3) 0.4636(5) 0.076(2) Uani 0.50 1 d PU . .
C75 C 0.3817(7) 0.6387(4) 0.4458(6) 0.100(3) Uani 0.50 1 d PU . .
C76 C 0.1914(3) 0.39310(18) 0.2055(2) 0.0713(15) Uani 1 1 d . . .
H76 H 0.1509 0.4118 0.2243 0.086 Uiso 1 1 calc R . .
C77 C 0.2888(4) 0.46028(18) 0.2013(3) 0.1020(19) Uani 1 1 d U . .
H77A H 0.2667 0.4749 0.1527 0.153 Uiso 1 1 calc R . .
H77B H 0.3589 0.4650 0.2228 0.153 Uiso 1 1 calc R . .
H77C H 0.2543 0.4729 0.2344 0.153 Uiso 1 1 calc R . .
C78 C 0.3361(4) 0.3863(2) 0.1631(3) 0.126(2) Uani 1 1 d U . .
H78A H 0.3277 0.3546 0.1713 0.189 Uiso 1 1 calc R . .
H78B H 0.4031 0.3951 0.1889 0.189 Uiso 1 1 calc R . .
H78C H 0.3225 0.3920 0.1097 0.189 Uiso 1 1 calc R . .
C79 C 0.1437(5) 0.61860(19) 0.5153(4) 0.194(4) Uiso 1 1 d D . .
C80 C 0.1982(4) 0.54004(17) 0.5002(3) 0.143(3) Uiso 1 1 d D . .
H80A H 0.2440 0.5265 0.5440 0.215 Uiso 1 1 calc R A .
H80B H 0.2344 0.5542 0.4695 0.215 Uiso 1 1 calc R . .
H80C H 0.1554 0.5170 0.4711 0.215 Uiso 1 1 calc R . .
C81 C 0.0666(4) 0.5640(2) 0.5630(3) 0.178(3) Uiso 1 1 d D . .
H81A H 0.0238 0.5898 0.5594 0.267 Uiso 1 1 calc R A .
H81B H 0.0997 0.5577 0.6154 0.267 Uiso 1 1 calc R . .
H81C H 0.0280 0.5381 0.5401 0.267 Uiso 1 1 calc R . .
O24A O 0.1200(10) 0.6527(2) 0.5363(8) 0.179(3) Uiso 0.266(5) 1 d PD A 2
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'
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
O1 Tb1 O2 52.80(6) . .
O1 Tb1 O19 74.37(7) . .
O1 Tb1 C1 26.62(7) . .
O2 Tb1 C1 26.22(7) . .
O4 Tb1 O1 150.79(7) . .
O4 Tb1 O2 146.68(7) . .
O4 Tb1 O8 75.45(7) . .
O4 Tb1 O11 87.29(8) . .
O4 Tb1 O14 121.09(8) . .
O4 Tb1 O19 76.44(7) . .
O4 Tb1 O22 82.75(8) . .
O4 Tb1 C1 161.29(8) . .
O8 Tb1 O1 130.78(7) . .
O8 Tb1 O2 78.27(7) . .
O8 Tb1 O11 132.12(8) . .
O8 Tb1 O14 76.30(7) . .
O8 Tb1 O19 142.09(8) . .
O8 Tb1 O22 79.58(8) . .
O8 Tb1 C1 104.46(8) . .
O11 Tb1 O1 82.04(8) . .
O11 Tb1 O2 125.81(8) . .
O11 Tb1 O19 70.71(8) . .
O11 Tb1 C1 105.24(8) . .
O14 Tb1 O1 82.37(7) . .
O14 Tb1 O2 70.88(7) . .
O14 Tb1 O11 75.41(7) . .
O14 Tb1 O19 140.96(7) . .
O14 Tb1 C1 76.21(8) . .
O19 Tb1 O2 115.08(7) . .
O19 Tb1 C1 94.37(8) . .
O22 Tb1 O1 89.44(8) . .
O22 Tb1 O2 72.59(8) . .
O22 Tb1 O11 142.75(8) . .
O22 Tb1 O14 139.42(7) . .
O22 Tb1 O19 72.07(7) . .
O22 Tb1 C1 78.89(9) . .
O5 Tb2 O16 83.01(8) . .
O5 Tb2 O17 72.03(7) . .
O5 Tb2 O20 142.03(8) . .
O5 Tb2 O21 139.28(7) . .
O5 Tb2 C58 76.76(8) . .
O7 Tb2 O5 73.12(8) . .
O7 Tb2 O16 97.81(7) . .
O7 Tb2 O17 136.59(8) . .
O7 Tb2 O20 144.45(8) . .
O7 Tb2 O21 75.88(7) . .
O7 Tb2 C58 118.89(8) . .
O10 Tb2 O5 74.67(8) . .
O10 Tb2 O7 111.86(8) . .
O10 Tb2 O13 75.45(8) . .
O10 Tb2 O16 134.93(8) . .
O10 Tb2 O17 82.71(8) . .
O10 Tb2 O20 88.98(8) . .
O10 Tb2 O21 142.71(8) . .
O10 Tb2 C58 109.38(9) . .
O13 Tb2 O5 128.58(8) . .
O13 Tb2 O7 80.62(8) . .
O13 Tb2 O16 144.88(7) . .
O13 Tb2 O17 142.32(7) . .
O13 Tb2 O20 77.17(8) . .
O13 Tb2 O21 69.87(7) . .
O13 Tb2 C58 153.50(9) . .
O16 Tb2 O17 53.02(6) . .
O16 Tb2 O20 85.21(8) . .
O16 Tb2 O21 75.71(7) . .
O16 Tb2 C58 26.11(7) . .
O17 Tb2 C58 26.92(7) . .
O20 Tb2 O17 72.06(8) . .
O20 Tb2 O21 70.58(7) . .
O20 Tb2 C58 76.89(9) . .
O21 Tb2 O17 117.62(7) . .
O21 Tb2 C58 96.28(8) . .
C1 O1 Tb1 94.39(17) . .
C1 O2 Tb1 93.48(17) . .
C12 O4 Tb1 149.5(2) . .
C12 O5 Tb2 139.5(2) . .
C24 O7 Tb2 140.59(19) . .
C24 O8 Tb1 149.55(19) . .
C35 O10 Tb2 171.4(2) . .
C35 O11 Tb1 120.22(18) . .
C47 O13 Tb2 141.4(2) . .
C47 O14 Tb1 145.2(2) . .
C58 O16 Tb2 96.04(19) . .
C58 O17 Tb2 91.38(17) . .
C73 O19 Tb1 127.9(5) . .
C70 O22 Tb1 143.1(2) . .
C70 N1 C71 120.1(3) . .
C70 N1 C72 123.3(4) . .
C72 N1 C71 116.6(3) . .
C73 N2 C75 124.3(9) . .
C74 N2 C73 117.3(9) . .
C74 N2 C75 118.4(9) . .
C76 N3 C77 123.1(4) . .
C76 N3 C78 121.2(4) . .
C78 N3 C77 115.7(4) . .
C79 N4 C80 126.3(5) . .
C79 N4 C81 108.8(5) . .
C81 N4 C80 124.9(5) . .
O1 C1 Tb1 58.99(15) . .
O1 C1 C2 120.1(2) . .
O2 C1 Tb1 60.30(15) . .
O2 C1 O1 119.1(3) . .
O2 C1 C2 120.8(2) . .
C2 C1 Tb1 175.3(2) . .
C19 C1B C17 124.3(7) . .
C3 C2 C1 120.4(3) . .
C3 C2 C11 119.3(3) . .
C11 C2 C1 120.3(3) . .
C2 C3 C4 121.7(3) . .
C3 C4 C5 121.1(3) . .
C3 C4 C9 119.3(3) . .
C5 C4 C9 119.6(3) . .
C6 C5 C4 121.3(3) . .
C5 C6 C7 118.8(3) . .
C8 C7 C6 121.7(3) . .
C7 C8 C9 121.6(3) . .
C8 C9 C4 116.8(3) . .
C8 C9 C10 124.0(3) . .
C10 C9 C4 119.2(3) . .
C9 C10 C23 121.5(3) . .
C11 C10 C9 119.3(3) . .
C11 C10 C23 119.1(3) . .
O3 C11 C2 120.2(3) . .
O3 C11 C10 118.6(2) . .
C10 C11 C2 121.2(3) . .
O4 C12 O5 123.7(3) . .
O4 C12 C13 119.4(3) . .
O5 C12 C13 116.9(3) . .
C14 C13 C12 122.5(3) . .
C22 C13 C12 119.7(3) . .
C22 C13 C14 117.6(3) . .
O6 C14 C13 119.6(3) . .
O6 C14 C15 117.8(3) . .
C15 C14 C13 122.5(3) . .
C14 C15 C16 118.8(3) . .
C14 C15 C23 120.2(3) . 2_646
C16 C15 C23 121.0(3) . 2_646
C15 C16 C17 121.6(3) . .
C15 C16 C21 117.9(4) . .
C15 C16 C21A 120.0(4) . .
C21 C16 C17 120.0(4) . .
C21A C16 C17 117.6(4) . .
C1B C17 C16 116.0(4) . .
C18A C17 C16 121.2(4) . .
C19A C18A C17 119.0(6) . .
C1B C19 C20 120.7(7) . .
C20A C19A C18A 120.6(7) . .
C19 C20 C21 120.1(7) . .
C19A C20A C21A 122.1(7) . .
C16 C21 C20 118.1(7) . .
C22 C21 C16 119.5(6) . .
C22 C21 C20 121.9(7) . .
C16 C21A C20A 118.8(7) . .
C22 C21A C16 116.5(6) . .
C22 C21A C20A 124.4(7) . .
C13 C22 C21 120.4(5) . .
C13 C22 C21A 122.2(4) . .
C15 C23 C10 116.1(2) 2_656 .
O7 C24 O8 123.9(3) . .
O7 C24 C25 119.0(3) . .
O8 C24 C25 117.2(3) . .
C26 C25 C24 119.3(3) . .
C26 C25 C34 119.6(2) . .
C34 C25 C24 121.1(3) . .
C25 C26 C27 121.2(3) . .
C26 C27 C32 118.8(3) . .
C28 C27 C26 121.8(3) . .
C28 C27 C32 119.3(3) . .
C29 C28 C27 121.9(3) . .
C28 C29 C30 119.6(3) . .
C31 C30 C29 120.4(3) . .
C30 C31 C32 121.9(3) . .
C31 C32 C27 116.7(3) . .
C33 C32 C27 119.8(2) . .
C33 C32 C31 123.4(3) . .
C32 C33 C46 121.1(2) . .
C34 C33 C32 118.7(3) . .
C34 C33 C46 120.1(3) . .
O9 C34 C25 120.9(2) . .
O9 C34 C33 117.5(3) . .
C33 C34 C25 121.5(3) . .
O10 C35 O11 121.5(3) . .
O10 C35 C36 120.3(3) . .
O11 C35 C36 118.2(3) . .
C37 C36 C35 119.3(3) . .
C37 C36 C45 118.9(3) . .
C45 C36 C35 121.8(3) . .
C36 C37 C38 122.0(3) . .
C37 C38 C39 121.8(3) . .
C37 C38 C43 118.4(3) . .
C43 C38 C39 119.8(3) . .
C40 C39 C38 120.3(4) . .
C39 C40 C41 120.0(4) . .
C42 C41 C40 121.9(3) . .
C41 C42 C43 120.8(3) . .
C38 C43 C42 117.1(3) . .
C44 C43 C38 120.3(2) . .
C44 C43 C42 122.4(3) . .
C43 C44 C46 121.4(2) . 4_475
C45 C44 C43 118.4(3) . .
C45 C44 C46 120.1(3) . 4_475
O12 C45 C36 120.9(2) . .
O12 C45 C44 118.2(3) . .
C44 C45 C36 120.8(3) . .
C33 C46 C44 114.4(2) . 4_676
O13 C47 O14 123.6(3) . .
O13 C47 C48 118.2(3) . .
O14 C47 C48 118.2(3) . .
C49 C48 C47 119.9(3) . .
C49 C48 C57 116.8(3) . .
C57 C48 C47 123.1(3) . .
C48 C49 C50 122.9(3) . .
C49 C50 C51 122.4(3) . .
C49 C50 C55 118.7(3) . .
C55 C50 C51 118.9(3) . .
C52 C51 C50 121.4(4) . .
C51 C52 C53 119.9(3) . .
C54 C53 C52 121.1(4) . .
C53 C54 C55 121.2(3) . .
C50 C55 C56 119.9(3) . .
C54 C55 C50 117.4(3) . .
C54 C55 C56 122.7(3) . .
C55 C56 C69 121.2(3) . .
C57 C56 C55 118.0(3) . .
C57 C56 C69 120.7(3) . .
O15 C57 C48 118.2(3) . .
C56 C57 O15 118.2(3) . .
C56 C57 C48 123.6(3) . .
O16 C58 Tb2 57.85(16) . .
O16 C58 O17 119.5(3) . .
O16 C58 C59 121.5(3) . .
O17 C58 Tb2 61.70(16) . .
O17 C58 C59 119.0(3) . .
C59 C58 Tb2 178.3(2) . .
C60 C59 C58 119.7(3) . .
C60 C59 C68 117.6(3) . .
C68 C59 C58 122.6(3) . .
C59 C60 C61 122.3(3) . .
C60 C61 C62 121.5(3) . .
C60 C61 C66 118.8(3) . .
C62 C61 C66 119.7(3) . .
C63 C62 C61 120.8(3) . .
C62 C63 C64 119.1(3) . .
C65 C64 C63 122.2(4) . .
C64 C65 C66 120.8(3) . .
C61 C66 C67 119.5(3) . .
C65 C66 C61 117.2(3) . .
C65 C66 C67 123.3(3) . .
C66 C67 C69 120.2(3) . 2_546
C68 C67 C66 118.4(3) . .
C68 C67 C69 121.4(3) . 2_546
O18 C68 C59 118.7(3) . .
C67 C68 O18 118.1(3) . .
C67 C68 C59 123.2(3) . .
C67 C69 C56 115.1(2) 2_556 .
O22 C70 N1 125.6(4) . .
O19 C73 N2 137.7(9) . .
O23 C76 N3 126.7(5) . .
O24 C79 N4 121.5(6) . .
O24A C79 O24 92.9(8) . .
O24A C79 N4 142.1(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O1 2.452(2) .
Tb1 O2 2.482(2) .
Tb1 O4 2.326(2) .
Tb1 O8 2.3309(19) .
Tb1 O11 2.3649(19) .
Tb1 O14 2.362(2) .
Tb1 O19 2.473(2) .
Tb1 O22 2.360(2) .
Tb1 C1 2.852(3) .
Tb2 O5 2.355(2) .
Tb2 O7 2.3480(19) .
Tb2 O10 2.299(2) .
Tb2 O13 2.303(2) .
Tb2 O16 2.410(2) .
Tb2 O17 2.494(2) .
Tb2 O20 2.433(2) .
Tb2 O21 2.4591(19) .
Tb2 C58 2.831(3) .
O1 C1 1.282(3) .
O24 C79 1.174(7) .
O2 C1 1.263(3) .
O3 C11 1.361(3) .
O4 C12 1.254(4) .
O5 C12 1.271(4) .
O6 C14 1.368(4) .
O7 C24 1.248(4) .
O8 C24 1.271(4) .
O9 C34 1.362(3) .
O10 C35 1.250(4) .
O11 C35 1.275(4) .
O12 C45 1.366(4) .
O13 C47 1.262(4) .
O14 C47 1.264(4) .
O15 C57 1.389(4) .
O16 C58 1.253(3) .
O17 C58 1.282(3) .
O18 C68 1.381(3) .
O19 C73 1.170(7) .
O22 C70 1.248(4) .
O23 C76 1.207(6) .
N1 C70 1.292(4) .
N1 C71 1.441(5) .
N1 C72 1.438(5) .
N2 C73 1.350(8) .
N2 C74 1.249(11) .
N2 C75 1.405(13) .
N3 C76 1.311(5) .
N3 C77 1.445(6) .
N3 C78 1.439(6) .
N4 C79 1.336(6) .
N4 C80 1.443(6) .
N4 C81 1.440(4) .
C1 C2 1.491(4) .
C1B C17 1.389(8) .
C1B C19 1.348(11) .
C2 C3 1.376(4) .
C2 C11 1.420(4) .
C3 C4 1.394(4) .
C4 C5 1.410(4) .
C4 C9 1.429(4) .
C5 C6 1.363(4) .
C6 C7 1.390(5) .
C7 C8 1.355(4) .
C8 C9 1.411(4) .
C9 C10 1.428(4) .
C10 C11 1.384(4) .
C10 C23 1.527(4) .
C12 C13 1.497(4) .
C13 C14 1.422(4) .
C13 C22 1.369(4) .
C14 C15 1.370(4) .
C15 C16 1.403(4) .
C15 C23 1.524(4) 2_646
C16 C17 1.439(5) .
C16 C21 1.431(9) .
C16 C21A 1.430(9) .
C17 C18A 1.435(8) .
C18A C19A 1.397(11) .
C19 C20 1.357(11) .
C19A C20A 1.372(10) .
C20 C21 1.442(11) .
C20A C21A 1.445(11) .
C21 C22 1.377(9) .
C21A C22 1.423(9) .
C23 C15 1.524(4) 2_656
C24 C25 1.515(4) .
C25 C26 1.364(4) .
C25 C34 1.422(4) .
C26 C27 1.415(4) .
C27 C28 1.403(4) .
C27 C32 1.437(4) .
C28 C29 1.355(4) .
C29 C30 1.402(5) .
C30 C31 1.366(4) .
C31 C32 1.418(4) .
C32 C33 1.416(4) .
C33 C34 1.390(4) .
C33 C46 1.521(4) .
C35 C36 1.475(4) .
C36 C37 1.363(4) .
C36 C45 1.428(4) .
C37 C38 1.401(4) .
C38 C39 1.421(5) .
C38 C43 1.418(4) .
C39 C40 1.357(5) .
C40 C41 1.379(5) .
C41 C42 1.353(5) .
C42 C43 1.422(4) .
C43 C44 1.418(4) .
C44 C45 1.385(4) .
C44 C46 1.530(4) 4_475
C46 C44 1.530(4) 4_676
C47 C48 1.472(4) .
C48 C49 1.380(4) .
C48 C57 1.421(4) .
C49 C50 1.394(5) .
C50 C51 1.428(5) .
C50 C55 1.424(5) .
C51 C52 1.346(5) .
C52 C53 1.387(6) .
C53 C54 1.371(5) .
C54 C55 1.415(5) .
C55 C56 1.425(4) .
C56 C57 1.373(4) .
C56 C69 1.515(4) .
C58 C59 1.488(4) .
C59 C60 1.372(4) .
C59 C68 1.420(4) .
C60 C61 1.406(5) .
C61 C62 1.423(4) .
C61 C66 1.424(4) .
C62 C63 1.365(5) .
C63 C64 1.392(5) .
C64 C65 1.358(5) .
C65 C66 1.422(4) .
C66 C67 1.428(4) .
C67 C68 1.369(4) .
C67 C69 1.514(4) 2_546
C69 C67 1.514(4) 2_556
C79 O24A 1.161(8) .
