#------------------------------------------------------------------------------
#$Date: 2024-03-04 22:08:59 +0200 (Mon, 04 Mar 2024) $
#$Revision: 290151 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/79/7247997.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_7247997
loop_
_publ_author_name
'Takahara, Kazuma'
'Horino, Yuki'
'Wada, Koki'
'Sakata, Hiromu'
'Tomita, Daichi'
'Sunatsuki, Yukinari'
'Isobe, Hiroshi'
'Kojima, Masaaki'
'Suzuki, Takayoshi'
_publ_section_title
;
 The effect of solvent molecules on crystallisation of heterotrinuclear
 MII--TbIII--MII complexes with tripodal nonadentate ligands
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1004
_journal_page_last               1014
_journal_paper_doi               10.1039/D3CE01192E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C66 H84 Mn2 N7 O19 Tb'
_chemical_formula_sum            'C66 H84 Mn2 N7 O19 Tb'
_chemical_formula_weight         1548.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2023-10-25 deposited with the CCDC.	2024-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                104.939(4)
_cell_angle_beta                 90.305(4)
_cell_angle_gamma                117.451(4)
_cell_formula_units_Z            1
_cell_length_a                   11.8404(17)
_cell_length_b                   11.8606(14)
_cell_length_c                   14.328(2)
_cell_measurement_reflns_used    12880
_cell_measurement_temperature    188
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.07
_cell_volume                     1707.0(4)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2014 (Burla, et al., 2014)'
_diffrn_ambient_temperature      188
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16846
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.068
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.463
_exptl_absorpt_correction_T_max  0.447
_exptl_absorpt_correction_T_min  0.232
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             796.00
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.550
_exptl_crystal_size_min          0.550
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.74
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7757
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0369P)²+0.8122P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7443
_reflns_number_total             7757
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            d3ce01192e2.cif
_cod_data_source_block           190314_aoff
_cod_depositor_comments
'Adding full bibliography for 7247989--7247998.cif.'
_cod_original_cell_volume        1707.1(4)
_cod_database_code               7247997
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.0000 1.0000 0.5000 0.02216(5) Uani 1 2 d S . P . .
Mn1 Mn 0.01372(3) 0.89961(3) 0.26372(2) 0.02114(7) Uani 1 1 d . . . . .
O1 O -0.20536(15) 1.07024(16) 0.48203(11) 0.0300(3) Uani 1 1 d . . . . .
O2 O -0.10265(13) 0.97349(14) 0.34497(10) 0.0233(3) Uani 1 1 d . . . . .
O3 O -0.06603(15) 0.75099(15) 0.54288(11) 0.0280(3) Uani 1 1 d . . . . .
O4 O -0.02091(14) 0.80788(14) 0.37855(10) 0.0232(3) Uani 1 1 d . . . . .
O5 O 0.26293(14) 1.21461(15) 0.56067(11) 0.0287(3) Uani 1 1 d . . . . .
O6 O 0.14818(13) 1.05469(14) 0.38691(10) 0.0233(3) Uani 1 1 d . . . . .
O10 O 0.3085(3) 0.6428(3) -0.0508(2) 0.0899(9) Uani 1 1 d . . . . .
O11 O 0.2296(3) 0.5521(2) 0.10698(18) 0.0676(6) Uani 1 1 d . . . . .
N1 N -0.12758(18) 0.84550(18) 0.13778(13) 0.0282(4) Uani 1 1 d . . . . .
N2 N 0.0244(2) 0.72151(19) 0.18037(13) 0.0298(4) Uani 1 1 d . . . . .
N3 N 0.15896(18) 1.00384(18) 0.17968(13) 0.0274(4) Uani 1 1 d . . . . .
N4 N -0.4763(7) 1.0039(14) -0.0119(6) 0.049(3) Uani 0.5 1 d . . P A -1
O7 O -0.4926(7) 0.8895(7) -0.0517(5) 0.0724(17) Uani 0.5 1 d . . P A -1
O8 O -0.5568(12) 1.0187(15) 0.0381(6) 0.074(3) Uani 0.5 1 d . . P A -1
O9 O -0.3829(5) 1.0978(6) -0.0261(5) 0.0753(16) Uani 0.5 1 d . . P A -1
C1 C 0.0381(3) 0.7598(3) -0.07513(17) 0.0421(6) Uani 1 1 d . . . . .
H1A H 0.1231 0.7668 -0.0827 0.051 Uiso 1 1 calc R U . . .
H1B H 0.0258 0.8175 -0.1075 0.051 Uiso 1 1 calc R U . . .
H1C H -0.0285 0.6675 -0.1047 0.051 Uiso 1 1 calc R U . . .
C2 C 0.0284(2) 0.8031(2) 0.03415(16) 0.0318(5) Uani 1 1 d . . . . .
C3 C -0.1112(2) 0.7730(2) 0.04295(16) 0.0336(5) Uani 1 1 d . . . . .
H3A H -0.1429 0.7961 -0.0096 0.040 Uiso 1 1 calc R U . . .
H3B H -0.1651 0.6764 0.0328 0.040 Uiso 1 1 calc R U . . .
C4 C -0.2134(2) 0.8818(2) 0.13669(17) 0.0311(5) Uani 1 1 d . . . . .
H4 H -0.2556 0.8641 0.0740 0.037 Uiso 1 1 calc R U . . .
C5 C -0.2550(2) 0.9466(2) 0.21883(17) 0.0293(4) Uani 1 1 d . . . . .
C6 C -0.3605(3) 0.9645(3) 0.1945(2) 0.0432(6) Uani 1 1 d . . . . .
H6 H -0.3954 0.9386 0.1280 0.052 Uiso 1 1 calc R U . . .
C7 C -0.4127(3) 1.0186(3) 0.2659(2) 0.0468(7) Uani 1 1 d . . . . .
H7 H -0.4831 1.0307 0.2487 0.056 Uiso 1 1 calc R U . . .
C8 C -0.3629(2) 1.0556(2) 0.36344(19) 0.0357(5) Uani 1 1 d . . . . .
H8 H -0.3998 1.0924 0.4129 0.043 Uiso 1 1 calc R U . . .
C9 C -0.2600(2) 1.0391(2) 0.38863(16) 0.0261(4) Uani 1 1 d . . . . .
C10 C -0.2605(2) 1.1225(3) 0.55804(18) 0.0376(5) Uani 1 1 d . . . . .
H10A H -0.2157 1.1382 0.6215 0.045 Uiso 1 1 calc R U . . .
H10B H -0.3518 1.0588 0.5527 0.045 Uiso 1 1 calc R U . . .
H10C H -0.2522 1.2064 0.5522 0.045 Uiso 1 1 calc R U . . .
C11 C -0.20153(19) 0.98546(19) 0.31682(15) 0.0231(4) Uani 1 1 d . . . . .
C12 C 0.0655(3) 0.7213(2) 0.08376(17) 0.0359(5) Uani 1 1 d . . . . .
H12A H 0.0261 0.6284 0.0411 0.043 Uiso 1 1 calc R U . . .
H12B H 0.1601 0.7579 0.0907 0.043 Uiso 1 1 calc R U . . .
C13 C -0.0226(2) 0.6116(2) 0.20064(16) 0.0306(5) Uani 1 1 d . . . . .
H13 H -0.0329 0.5368 0.1496 0.037 Uiso 1 1 calc R U . . .
C14 C -0.0627(2) 0.5863(2) 0.29231(15) 0.0256(4) Uani 1 1 d . . . . .
C15 C -0.1082(2) 0.4548(2) 0.29552(17) 0.0322(5) Uani 1 1 d . . . . .
H15 H -0.1167 0.3882 0.2380 0.039 Uiso 1 1 calc R U . . .
C16 C -0.1405(2) 0.4210(2) 0.37946(18) 0.0320(5) Uani 1 1 d . . . . .
H16 H -0.1722 0.3315 0.3799 0.038 Uiso 1 1 calc R U . . .
C17 C -0.1266(2) 0.5186(2) 0.46489(16) 0.0270(4) Uani 1 1 d . . . . .
H17 H -0.1464 0.4961 0.5239 0.032 Uiso 1 1 calc R U . . .
C18 C -0.08424(19) 0.6474(2) 0.46343(15) 0.0228(4) Uani 1 1 d . . . . .
C19 C -0.0925(2) 0.7213(2) 0.63284(16) 0.0328(5) Uani 1 1 d . . . . .
H19A H -0.1834 0.6561 0.6266 0.039 Uiso 1 1 calc R U . . .
H19B H -0.0738 0.8028 0.6844 0.039 Uiso 1 1 calc R U . . .
H19C H -0.0387 0.6847 0.6496 0.039 Uiso 1 1 calc R U . . .
C20 C -0.05445(19) 0.68469(19) 0.37659(15) 0.0219(4) Uani 1 1 d . . . . .
C21 C 0.1242(2) 0.9526(2) 0.07299(16) 0.0326(5) Uani 1 1 d . . . . .
H21A H 0.2036 0.9703 0.0432 0.039 Uiso 1 1 calc R U . . .
H21B H 0.0864 1.0025 0.0515 0.039 Uiso 1 1 calc R U . . .
C22 C 0.2761(2) 1.0879(2) 0.21142(17) 0.0294(5) Uani 1 1 d . . . . .
H22 H 0.3322 1.1047 0.1636 0.035 Uiso 1 1 calc R U . . .
C23 C 0.3347(2) 1.1617(2) 0.31216(17) 0.0275(4) Uani 1 1 d . . . . .
C24 C 0.4649(2) 1.2595(2) 0.3266(2) 0.0362(5) Uani 1 1 d . . . . .
H24 H 0.5098 1.2679 0.2719 0.043 Uiso 1 1 calc R U . . .
C25 C 0.5279(2) 1.3425(3) 0.4172(2) 0.0402(6) Uani 1 1 d . . . . .
H25 H 0.6156 1.4079 0.4251 0.048 Uiso 1 1 calc R U . . .
C26 C 0.4628(2) 1.3307(2) 0.49833(19) 0.0340(5) Uani 1 1 d . . . . .
H26 H 0.5057 1.3891 0.5614 0.041 Uiso 1 1 calc R U . . .
C27 C 0.33610(19) 1.2341(2) 0.48655(16) 0.0258(4) Uani 1 1 d . . . . .
C28 C 0.3237(2) 1.3048(2) 0.65562(16) 0.0325(5) Uani 1 1 d . . . . .
H28A H 0.2620 1.2846 0.7021 0.039 Uiso 1 1 calc R U . . .
H28B H 0.3534 1.3961 0.6537 0.039 Uiso 1 1 calc R U . . .
H28C H 0.3973 1.2956 0.6762 0.039 Uiso 1 1 calc R U . . .
C29 C 0.26849(19) 1.14560(19) 0.39355(15) 0.0224(4) Uani 1 1 d . . . . .
C30 C 0.4908(6) 0.6112(7) -0.0809(5) 0.132(2) Uani 1 1 d . . . . .
H30A H 0.4937 0.5915 -0.0189 0.158 Uiso 1 1 calc R U . . .
H30B H 0.5448 0.7068 -0.0710 0.158 Uiso 1 1 calc R U . . .
H30C H 0.5230 0.5619 -0.1289 0.158 Uiso 1 1 calc R U . . .
C31 C 0.3606(5) 0.5725(5) -0.1161(3) 0.0934(15) Uani 1 1 d . . . . .
H31A H 0.3578 0.5888 -0.1802 0.112 Uiso 1 1 calc R U . . .
H31B H 0.3066 0.4760 -0.1258 0.112 Uiso 1 1 calc R U . . .
C32 C 0.2865(5) 0.5821(5) 0.2741(3) 0.0889(13) Uani 1 1 d . . . . .
H32A H 0.3031 0.5061 0.2580 0.107 Uiso 1 1 calc R U . . .
H32B H 0.1962 0.5517 0.2831 0.107 Uiso 1 1 calc R U . . .
H32C H 0.3420 0.6476 0.3345 0.107 Uiso 1 1 calc R U . . .
C33 C 0.3137(4) 0.6434(4) 0.1942(3) 0.0714(10) Uani 1 1 d . . . . .
H33A H 0.3025 0.7237 0.2122 0.086 Uiso 1 1 calc R U . . .
H33B H 0.4040 0.6710 0.1832 0.086 Uiso 1 1 calc R U . . .
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 for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Mn Mn 0.3368 0.7283
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Tb Tb -0.1723 4.1537
;
International Tables for Crystallography
(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
_geom_angle_publ_flag
O6 Tb1 O6 180.0 . 2_576 ?
O6 Tb1 O4 112.54(5) . 2_576 ?
O6 Tb1 O4 67.46(5) 2_576 2_576 ?
O6 Tb1 O4 67.46(5) . . ?
O6 Tb1 O4 112.54(5) 2_576 . ?
O4 Tb1 O4 180.0 2_576 . ?
O6 Tb1 O2 68.08(5) . . ?
O6 Tb1 O2 111.92(5) 2_576 . ?
O4 Tb1 O2 111.56(5) 2_576 . ?
O4 Tb1 O2 68.43(5) . . ?
O6 Tb1 O2 111.92(5) . 2_576 ?
O6 Tb1 O2 68.08(5) 2_576 2_576 ?
O4 Tb1 O2 68.44(5) 2_576 2_576 ?
O4 Tb1 O2 111.56(5) . 2_576 ?
O2 Tb1 O2 180.00(3) . 2_576 ?
O6 Tb1 O5 121.91(5) . 2_576 ?
O6 Tb1 O5 58.09(5) 2_576 2_576 ?
O4 Tb1 O5 114.13(5) 2_576 2_576 ?
O4 Tb1 O5 65.87(5) . 2_576 ?
O2 Tb1 O5 63.94(5) . 2_576 ?
O2 Tb1 O5 116.06(5) 2_576 2_576 ?
O6 Tb1 O5 58.09(5) . . ?
O6 Tb1 O5 121.91(5) 2_576 . ?
O4 Tb1 O5 65.87(5) 2_576 . ?
O4 Tb1 O5 114.13(5) . . ?
O2 Tb1 O5 116.06(5) . . ?
O2 Tb1 O5 63.94(5) 2_576 . ?
O5 Tb1 O5 180.0 2_576 . ?
O6 Tb1 O3 115.71(5) . . ?
O6 Tb1 O3 64.29(5) 2_576 . ?
O4 Tb1 O3 122.27(5) 2_576 . ?
O4 Tb1 O3 57.73(5) . . ?
O2 Tb1 O3 114.44(5) . . ?
O2 Tb1 O3 65.56(5) 2_576 . ?
O5 Tb1 O3 61.81(5) 2_576 . ?
O5 Tb1 O3 118.19(5) . . ?
O6 Tb1 O3 64.29(5) . 2_576 ?
O6 Tb1 O3 115.71(5) 2_576 2_576 ?
O4 Tb1 O3 57.73(5) 2_576 2_576 ?
O4 Tb1 O3 122.27(5) . 2_576 ?
O2 Tb1 O3 65.56(5) . 2_576 ?
O2 Tb1 O3 114.44(5) 2_576 2_576 ?
O5 Tb1 O3 118.19(5) 2_576 2_576 ?
O5 Tb1 O3 61.81(5) . 2_576 ?
O3 Tb1 O3 180.0 . 2_576 ?
O6 Tb1 Mn1 40.30(3) . . ?
O6 Tb1 Mn1 139.70(4) 2_576 . ?
O4 Tb1 Mn1 139.97(3) 2_576 . ?
O4 Tb1 Mn1 40.03(3) . . ?
O2 Tb1 Mn1 40.32(3) . . ?
O2 Tb1 Mn1 139.68(3) 2_576 . ?
O5 Tb1 Mn1 81.62(3) 2_576 . ?
O5 Tb1 Mn1 98.38(3) . . ?
O3 Tb1 Mn1 97.72(3) . . ?
O3 Tb1 Mn1 82.28(3) 2_576 . ?
O6 Tb1 Mn1 139.70(3) . 2_576 ?
O6 Tb1 Mn1 40.30(3) 2_576 2_576 ?
O4 Tb1 Mn1 40.03(3) 2_576 2_576 ?
O4 Tb1 Mn1 139.97(3) . 2_576 ?
O2 Tb1 Mn1 139.68(3) . 2_576 ?
O2 Tb1 Mn1 40.32(3) 2_576 2_576 ?
O5 Tb1 Mn1 98.38(3) 2_576 2_576 ?
O5 Tb1 Mn1 81.62(3) . 2_576 ?
O3 Tb1 Mn1 82.28(3) . 2_576 ?
O3 Tb1 Mn1 97.72(3) 2_576 2_576 ?
Mn1 Tb1 Mn1 180.0 . 2_576 ?
O4 Mn1 O2 77.82(5) . . ?
O4 Mn1 O6 76.16(6) . . ?
O2 Mn1 O6 76.88(5) . . ?
O4 Mn1 N3 144.77(7) . . ?
O2 Mn1 N3 125.34(6) . . ?
O6 Mn1 N3 83.60(6) . . ?
O4 Mn1 N1 125.99(7) . . ?
O2 Mn1 N1 83.84(6) . . ?
O6 Mn1 N1 146.72(6) . . ?
N3 Mn1 N1 85.87(7) . . ?
O4 Mn1 N2 83.87(6) . . ?
O2 Mn1 N2 145.71(7) . . ?
O6 Mn1 N2 126.40(7) . . ?
N3 Mn1 N2 85.43(7) . . ?
N1 Mn1 N2 83.87(7) . . ?
O4 Mn1 Tb1 45.93(4) . . ?
O2 Mn1 Tb1 46.27(4) . . ?
O6 Mn1 Tb1 45.59(4) . . ?
N3 Mn1 Tb1 128.17(5) . . ?
N1 Mn1 Tb1 128.90(5) . . ?
N2 Mn1 Tb1 129.00(5) . . ?
C9 O1 C10 116.69(17) . . ?
C11 O2 Mn1 131.74(13) . . ?
C11 O2 Tb1 134.53(13) . . ?
Mn1 O2 Tb1 93.42(5) . . ?
C18 O3 C19 116.67(17) . . ?
C18 O3 Tb1 114.88(12) . . ?
C19 O3 Tb1 128.19(12) . . ?
C20 O4 Mn1 130.90(13) . . ?
C20 O4 Tb1 134.73(13) . . ?
Mn1 O4 Tb1 94.04(5) . . ?
C27 O5 C28 116.27(17) . . ?
C27 O5 Tb1 114.79(12) . . ?
C28 O5 Tb1 128.88(13) . . ?
C29 O6 Mn1 131.35(13) . . ?
C29 O6 Tb1 134.53(13) . . ?
Mn1 O6 Tb1 94.12(5) . . ?
C4 N1 C3 116.76(19) . . ?
C4 N1 Mn1 126.55(15) . . ?
C3 N1 Mn1 116.29(14) . . ?
C13 N2 C12 116.94(18) . . ?
C13 N2 Mn1 125.37(15) . . ?
C12 N2 Mn1 116.48(14) . . ?
C22 N3 C21 116.01(19) . . ?
C22 N3 Mn1 126.81(16) . . ?
C21 N3 Mn1 116.04(14) . . ?
O9 N4 O8 122.0(13) . . ?
O9 N4 O7 118.2(7) . . ?
O8 N4 O7 119.7(11) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 C1 107.6(2) . . ?
C3 C2 C21 112.36(19) . . ?
C1 C2 C21 106.63(19) . . ?
C3 C2 C12 111.1(2) . . ?
C1 C2 C12 107.25(19) . . ?
C21 C2 C12 111.5(2) . . ?
N1 C3 C2 113.89(19) . . ?
N1 C3 H3A 108.8 . . ?
C2 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
N1 C4 C5 128.5(2) . . ?
N1 C4 H4 115.8 . . ?
C5 C4 H4 115.8 . . ?
C11 C5 C6 120.3(2) . . ?
C11 C5 C4 124.5(2) . . ?
C6 C5 C4 115.1(2) . . ?
C7 C6 C5 120.7(2) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 H6 119.7 . . ?
C6 C7 C8 120.0(2) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 120.1(2) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
O1 C9 C8 124.8(2) . . ?
O1 C9 C11 113.59(17) . . ?
C8 C9 C11 121.7(2) . . ?
O1 C10 H10A 109.5 . . ?
O1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O2 C11 C5 123.83(19) . . ?
O2 C11 C9 119.06(19) . . ?
C5 C11 C9 117.10(19) . . ?
N2 C12 C2 113.21(18) . . ?
N2 C12 H12A 108.9 . . ?
C2 C12 H12A 108.9 . . ?
N2 C12 H12B 108.9 . . ?
C2 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
N2 C13 C14 128.06(19) . . ?
N2 C13 H13 116.0 . . ?
C14 C13 H13 116.0 . . ?
C15 C14 C20 119.5(2) . . ?
C15 C14 C13 116.12(19) . . ?
C20 C14 C13 124.32(19) . . ?
C16 C15 C14 121.4(2) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C17 119.7(2) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C18 C17 C16 120.0(2) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
O3 C18 C17 124.88(19) . . ?
O3 C18 C20 113.51(17) . . ?
C17 C18 C20 121.61(19) . . ?
O3 C19 H19A 109.5 . . ?
O3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O4 C20 C14 123.66(19) . . ?
O4 C20 C18 118.81(17) . . ?
C14 C20 C18 117.53(18) . . ?
N3 C21 C2 114.65(18) . . ?
N3 C21 H21A 108.6 . . ?
C2 C21 H21A 108.6 . . ?
N3 C21 H21B 108.6 . . ?
C2 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
N3 C22 C23 127.7(2) . . ?
N3 C22 H22 116.2 . . ?
C23 C22 H22 116.2 . . ?
C24 C23 C29 119.5(2) . . ?
C24 C23 C22 116.0(2) . . ?
C29 C23 C22 124.4(2) . . ?
C25 C24 C23 121.6(2) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C24 C25 C26 119.7(2) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C27 C26 C25 119.9(2) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
O5 C27 C26 124.7(2) . . ?
O5 C27 C29 113.53(18) . . ?
C26 C27 C29 121.7(2) . . ?
O5 C28 H28A 109.5 . . ?
O5 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O5 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O6 C29 C23 123.44(19) . . ?
O6 C29 C27 119.03(18) . . ?
C23 C29 C27 117.52(19) . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C31 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O10 C31 C30 112.5(5) . . ?
O10 C31 H31A 109.1 . . ?
C30 C31 H31A 109.1 . . ?
O10 C31 H31B 109.1 . . ?
C30 C31 H31B 109.1 . . ?
H31A C31 H31B 107.8 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O11 C33 C32 110.4(4) . . ?
O11 C33 H33A 109.6 . . ?
C32 C33 H33A 109.6 . . ?
O11 C33 H33B 109.6 . . ?
C32 C33 H33B 109.6 . . ?
H33A C33 H33B 108.1 . . ?
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 O6 2.3764(14) . ?
Tb1 O6 2.3764(14) 2_576 ?
Tb1 O4 2.3901(14) 2_576 ?
Tb1 O4 2.3901(14) . ?
Tb1 O2 2.4019(14) . ?
Tb1 O2 2.4020(15) 2_576 ?
Tb1 O5 2.9070(15) 2_576 ?
Tb1 O5 2.9071(15) . ?
Tb1 O3 2.9195(15) . ?
Tb1 O3 2.9195(15) 2_576 ?
Tb1 Mn1 3.3183(6) . ?
Tb1 Mn1 3.3183(6) 2_576 ?
Mn1 O4 2.1395(15) . ?
Mn1 O2 2.1509(14) . ?
Mn1 O6 2.1517(15) . ?
Mn1 N3 2.1828(19) . ?
Mn1 N1 2.2018(19) . ?
Mn1 N2 2.2026(18) . ?
O1 C9 1.364(3) . ?
O1 C10 1.425(3) . ?
O2 C11 1.316(2) . ?
O3 C18 1.373(2) . ?
O3 C19 1.421(3) . ?
O4 C20 1.318(2) . ?
O5 C27 1.373(3) . ?
O5 C28 1.429(3) . ?
O6 C29 1.315(2) . ?
O10 C31 1.424(6) . ?
O11 C33 1.421(4) . ?
N1 C4 1.274(3) . ?
N1 C3 1.475(3) . ?
N2 C13 1.274(3) . ?
N2 C12 1.470(3) . ?
N3 C22 1.269(3) . ?
N3 C21 1.469(3) . ?
N4 O9 1.220(13) . ?
N4 O8 1.245(11) . ?
N4 O7 1.250(15) . ?
C1 C2 1.539(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.536(3) . ?
C2 C21 1.540(3) . ?
C2 C12 1.544(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.452(3) . ?
C4 H4 0.9500 . ?
C5 C11 1.405(3) . ?
C5 C6 1.415(3) . ?
C6 C7 1.369(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.389(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.380(3) . ?
C8 H8 0.9500 . ?
C9 C11 1.421(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.455(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.410(3) . ?
C14 C20 1.413(3) . ?
C15 C16 1.366(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.399(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.376(3) . ?
C17 H17 0.9500 . ?
C18 C20 1.419(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.452(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.410(3) . ?
C23 C29 1.413(3) . ?
C24 C25 1.365(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.400(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.380(3) . ?
C26 H26 0.9500 . ?
C27 C29 1.418(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C30 C31 1.436(7) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.470(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
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
C4 N1 C3 C2 145.3(2) . . . . ?
Mn1 N1 C3 C2 -27.9(2) . . . . ?
C1 C2 C3 N1 -161.7(2) . . . . ?
C21 C2 C3 N1 -44.6(3) . . . . ?
C12 C2 C3 N1 81.1(2) . . . . ?
C3 N1 C4 C5 175.9(2) . . . . ?
Mn1 N1 C4 C5 -11.7(4) . . . . ?
N1 C4 C5 C11 2.4(4) . . . . ?
N1 C4 C5 C6 -174.9(3) . . . . ?
C11 C5 C6 C7 -0.6(4) . . . . ?
C4 C5 C6 C7 176.8(3) . . . . ?
C5 C6 C7 C8 -0.5(5) . . . . ?
C6 C7 C8 C9 0.5(4) . . . . ?
C10 O1 C9 C8 0.5(3) . . . . ?
C10 O1 C9 C11 -179.0(2) . . . . ?
C7 C8 C9 O1 -178.9(2) . . . . ?
C7 C8 C9 C11 0.5(4) . . . . ?
Mn1 O2 C11 C5 0.9(3) . . . . ?
Tb1 O2 C11 C5 -170.85(15) . . . . ?
Mn1 O2 C11 C9 -179.88(14) . . . . ?
Tb1 O2 C11 C9 8.4(3) . . . . ?
C6 C5 C11 O2 -179.2(2) . . . . ?
C4 C5 C11 O2 3.7(4) . . . . ?
C6 C5 C11 C9 1.6(3) . . . . ?
C4 C5 C11 C9 -175.6(2) . . . . ?
O1 C9 C11 O2 -1.3(3) . . . . ?
C8 C9 C11 O2 179.1(2) . . . . ?
O1 C9 C11 C5 177.94(19) . . . . ?
C8 C9 C11 C5 -1.6(3) . . . . ?
C13 N2 C12 C2 138.3(2) . . . . ?
Mn1 N2 C12 C2 -29.8(3) . . . . ?
C3 C2 C12 N2 -45.3(3) . . . . ?
C1 C2 C12 N2 -162.7(2) . . . . ?
C21 C2 C12 N2 80.9(3) . . . . ?
C12 N2 C13 C14 175.7(2) . . . . ?
Mn1 N2 C13 C14 -17.3(4) . . . . ?
N2 C13 C14 C15 -178.1(2) . . . . ?
N2 C13 C14 C20 -0.3(4) . . . . ?
C20 C14 C15 C16 -2.3(3) . . . . ?
C13 C14 C15 C16 175.6(2) . . . . ?
C14 C15 C16 C17 -1.0(4) . . . . ?
C15 C16 C17 C18 1.9(3) . . . . ?
C19 O3 C18 C17 0.5(3) . . . . ?
Tb1 O3 C18 C17 -174.11(16) . . . . ?
C19 O3 C18 C20 -179.29(18) . . . . ?
Tb1 O3 C18 C20 6.1(2) . . . . ?
C16 C17 C18 O3 -179.4(2) . . . . ?
C16 C17 C18 C20 0.4(3) . . . . ?
Mn1 O4 C20 C14 6.5(3) . . . . ?
Tb1 O4 C20 C14 178.17(14) . . . . ?
Mn1 O4 C20 C18 -173.45(13) . . . . ?
Tb1 O4 C20 C18 -1.8(3) . . . . ?
C15 C14 C20 O4 -175.5(2) . . . . ?
C13 C14 C20 O4 6.7(3) . . . . ?
C15 C14 C20 C18 4.5(3) . . . . ?
C13 C14 C20 C18 -173.3(2) . . . . ?
O3 C18 C20 O4 -3.8(3) . . . . ?
C17 C18 C20 O4 176.42(19) . . . . ?
O3 C18 C20 C14 176.19(18) . . . . ?
C17 C18 C20 C14 -3.6(3) . . . . ?
C22 N3 C21 C2 140.1(2) . . . . ?
Mn1 N3 C21 C2 -28.6(2) . . . . ?
C3 C2 C21 N3 80.4(2) . . . . ?
C1 C2 C21 N3 -161.9(2) . . . . ?
C12 C2 C21 N3 -45.2(3) . . . . ?
C21 N3 C22 C23 174.9(2) . . . . ?
Mn1 N3 C22 C23 -17.9(3) . . . . ?
N3 C22 C23 C24 -173.6(2) . . . . ?
N3 C22 C23 C29 3.2(4) . . . . ?
C29 C23 C24 C25 -2.2(4) . . . . ?
C22 C23 C24 C25 174.8(2) . . . . ?
C23 C24 C25 C26 0.2(4) . . . . ?
C24 C25 C26 C27 1.0(4) . . . . ?
C28 O5 C27 C26 2.0(3) . . . . ?
Tb1 O5 C27 C26 179.49(18) . . . . ?
C28 O5 C27 C29 -177.13(18) . . . . ?
Tb1 O5 C27 C29 0.4(2) . . . . ?
C25 C26 C27 O5 -179.4(2) . . . . ?
C25 C26 C27 C29 -0.4(4) . . . . ?
Mn1 O6 C29 C23 2.9(3) . . . . ?
Tb1 O6 C29 C23 -176.63(14) . . . . ?
Mn1 O6 C29 C27 -178.04(13) . . . . ?
Tb1 O6 C29 C27 2.4(3) . . . . ?
C24 C23 C29 O6 -178.2(2) . . . . ?
C22 C23 C29 O6 5.1(3) . . . . ?
C24 C23 C29 C27 2.7(3) . . . . ?
C22 C23 C29 C27 -173.96(19) . . . . ?
O5 C27 C29 O6 -1.5(3) . . . . ?
C26 C27 C29 O6 179.4(2) . . . . ?
O5 C27 C29 C23 177.60(18) . . . . ?
C26 C27 C29 C23 -1.5(3) . . . . ?
