#------------------------------------------------------------------------------
#$Date: 2019-11-10 19:27:51 +0200 (Sun, 10 Nov 2019) $
#$Revision: 226039 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/59/4515994.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_4515994
loop_
_publ_author_name
'Kalita, Pankaj'
'Goura, Joydeb'
'Herrera, Juan Manuel'
'Colacio, Enrique'
'Chandrasekhar, Vadapalli'
_publ_section_title
;
 Heterometallic Octanuclear
 NiII₄LnIII₄ (Ln = Y, Gd, Tb,
 Dy, Ho, Er) Complexes Containing
 NiII₂LnIII₂O₄
 Distorted Cubane Motifs: Synthesis, Structure, and Magnetic Properties.
;
_journal_issue                   5
_journal_name_full               'ACS omega'
_journal_page_first              5202
_journal_page_last               5211
_journal_paper_doi               10.1021/acsomega.8b00292
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C64 H98 N8 Ni4 O34 Tb4, 2(H O)'
_chemical_formula_sum            'C64 H100 N8 Ni4 O36 Tb4'
_chemical_formula_weight         2428.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-22
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.576(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9219(8)
_cell_length_b                   15.5160(10)
_cell_length_c                   23.5346(13)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.20
_cell_measurement_theta_min      2.58
_cell_volume                     4687.6(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            71751
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.295
_diffrn_reflns_theta_min         2.059
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.840
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0981 before and 0.0586 after correction. The Ratio of minimum to maximum transmission is 0.8023. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.007
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         11609
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0713P)²+19.6597P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7993
_reflns_number_total             11609
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ao8b00292_si_001.cif
_cod_data_source_block           vc_pk_ni4tb4
_cod_database_code               4515994
_shelx_shelxl_version_number     2016/4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.677
_shelx_estimated_absorpt_t_min   0.579
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H1-O1 = O3-H3 = O2-H2
 0.85 with sigma of 0.002
 O3A-C11A \\sim O3B-C11B
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C1A) = Uanis(C2A) = Uanis(C3A) = Uanis(C4A) = Uanis(C5A) = Uanis(C6A)
Uanis(O3A) = Uanis(O3B)
4.a Riding coordinates:
 O3A(H3A), O3B(H3B), C2E(H2EA,H2EB,H2EC), O4(H4)
4.b Ternary CH refined with riding coordinates:
 N2A(H2A), N2B(H2B)
4.c Secondary CH2 refined with riding coordinates:
 C8A(H8AA,H8AB), C8B(H8BA,H8BB), C9A(H9AA,H9AB), C9B(H9BA,H9BB), C10A(H10A,
 H10B), C10B(H10C,H10D), C11A(H11A,H11B), C11B(H11C,H11D)
4.d Aromatic/amide H refined with riding coordinates:
 C3A(H3AA), C3B(H3BA), C4A(H4A), C4B(H4B), C5A(H5A), C5B(H5B), C7A(H7A),
 C7B(H7B)
4.e Idealised Me refined as rotating group:
 C2C(H2CA,H2CB,H2CC), C2D(H2DA,H2DB,H2DC), C2F(H2FA,H2FB,H2FC), C12A(H12A,H12B,
 H12C), C12B(H12D,H12E,H12F)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Tb01 Tb 0.51792(3) 0.31663(2) 0.50294(2) 0.03386(11) Uani 1 1 d .
Tb02 Tb 0.47217(3) 0.50598(2) 0.37969(2) 0.03592(11) Uani 1 1 d .
Ni1 Ni 0.42114(8) 0.28430(6) 0.63275(4) 0.0367(2) Uani 1 1 d .
Ni2 Ni 0.67244(8) 0.30687(6) 0.63686(4) 0.0382(2) Uani 1 1 d .
O1 O 0.4450(5) 0.4361(3) 0.4606(2) 0.0451(13) Uani 1 1 d D
H1 H 0.3790(9) 0.435(8) 0.459(5) 0.10(4) Uiso 1 1 d D
O1A O 0.4576(5) 0.4898(3) 0.7181(2) 0.0484(14) Uani 1 1 d .
O1B O 0.6192(4) 0.1725(3) 0.5038(2) 0.0443(13) Uani 1 1 d .
O1C O 0.4592(5) 0.3641(3) 0.3422(2) 0.0532(15) Uani 1 1 d .
O1D O 0.6416(5) 0.4533(4) 0.3957(3) 0.0549(15) Uani 1 1 d .
O1E O 0.3086(5) 0.2148(4) 0.5815(2) 0.0481(14) Uani 1 1 d .
O1F O 0.7836(4) 0.3875(4) 0.6756(2) 0.0512(14) Uani 1 1 d .
O2 O 0.6294(4) 0.3914(3) 0.5730(2) 0.0356(11) Uani 1 1 d D
H2 H 0.691(2) 0.401(6) 0.565(3) 0.06(3) Uiso 1 1 d D
O2A O 0.5515(4) 0.3599(3) 0.6772(2) 0.0397(12) Uani 1 1 d .
O2B O 0.5412(4) 0.2323(3) 0.5926(2) 0.0365(11) Uani 1 1 d .
O2C O 0.4858(5) 0.2628(4) 0.4086(2) 0.0511(15) Uani 1 1 d .
O2D O 0.6686(5) 0.3515(4) 0.4613(3) 0.0533(15) Uani 1 1 d .
O2E O 0.3642(5) 0.2374(4) 0.4965(2) 0.0520(15) Uani 1 1 d .
O2F O 0.6978(5) 0.5132(4) 0.6663(3) 0.0528(15) Uani 1 1 d .
O3 O 0.4240(4) 0.3816(3) 0.5758(2) 0.0369(11) Uani 1 1 d D
H3 H 0.3622(19) 0.396(4) 0.563(3) 0.03(2) Uiso 1 1 d D
O3A O 0.9154(9) 0.1777(8) 0.5173(6) 0.143(3) Uani 1 1 d D
H3A H 0.926134 0.133969 0.536592 0.215 Uiso 1 1 d R
O3B O 0.1579(9) 0.4610(8) 0.7233(6) 0.143(3) Uani 1 1 d D
H3B H 0.199211 0.440116 0.748676 0.215 Uiso 1 1 d R
N1A N 0.7056(6) 0.2261(4) 0.7036(3) 0.0522(18) Uani 1 1 d .
N1B N 0.4334(6) 0.1872(4) 0.6891(3) 0.0436(15) Uani 1 1 d .
N2A N 0.7954(5) 0.2395(5) 0.6039(3) 0.0496(17) Uani 1 1 d .
H2A H 0.763383 0.193718 0.577634 0.060 Uiso 1 1 calc R
N2B N 0.3049(6) 0.3282(4) 0.6832(3) 0.0477(16) Uani 1 1 d .
H2B H 0.337469 0.371632 0.711122 0.057 Uiso 1 1 calc R
C1A C 0.5683(9) 0.3723(7) 0.7351(4) 0.0674(12) Uani 1 1 d .
C1B C 0.5501(6) 0.1456(5) 0.5898(3) 0.0404(18) Uani 1 1 d .
C1C C 0.4772(7) 0.2887(5) 0.3582(3) 0.0442(19) Uani 1 1 d .
C1D C 0.6970(7) 0.3967(6) 0.4227(4) 0.051(2) Uani 1 1 d .
C1E C 0.2981(7) 0.2121(5) 0.5273(4) 0.0456(19) Uani 1 1 d .
C1F C 0.7758(6) 0.4675(6) 0.6817(4) 0.048(2) Uani 1 1 d .
C2A C 0.5195(9) 0.4426(7) 0.7577(4) 0.0674(12) Uani 1 1 d .
C2B C 0.5970(6) 0.1121(5) 0.5434(3) 0.0424(18) Uani 1 1 d .
C2C C 0.4859(11) 0.2228(6) 0.3122(4) 0.078(4) Uani 1 1 d .
H2CA H 0.552640 0.192526 0.319655 0.117 Uiso 1 1 calc GR
H2CB H 0.482009 0.251642 0.274956 0.117 Uiso 1 1 calc GR
H2CC H 0.428719 0.181260 0.311927 0.117 Uiso 1 1 calc GR
C2D C 0.8075(9) 0.3835(9) 0.4075(6) 0.093(4) Uani 1 1 d .
H2DA H 0.853050 0.366565 0.441812 0.140 Uiso 1 1 calc GR
H2DB H 0.832911 0.437431 0.392376 0.140 Uiso 1 1 calc GR
H2DC H 0.807422 0.338204 0.378488 0.140 Uiso 1 1 calc GR
C2E C 0.1987(8) 0.1743(8) 0.4980(4) 0.079(3) Uani 1 1 d .
H2EA H 0.212491 0.119927 0.481058 0.118 Uiso 1 1 d R
H2EB H 0.170671 0.213647 0.468708 0.118 Uiso 1 1 d R
H2EC H 0.149441 0.166517 0.525118 0.118 Uiso 1 1 d R
C2F C 0.8713(9) 0.5119(7) 0.7092(6) 0.086(4) Uani 1 1 d .
H2FA H 0.909841 0.536441 0.679561 0.129 Uiso 1 1 calc GR
H2FB H 0.915451 0.470288 0.731995 0.129 Uiso 1 1 calc GR
H2FC H 0.851082 0.558121 0.734111 0.129 Uiso 1 1 calc GR
C3A C 0.5370(9) 0.4630(7) 0.8144(4) 0.0674(12) Uani 1 1 d .
H3AA H 0.502449 0.510958 0.828845 0.081 Uiso 1 1 calc R
C3B C 0.6165(8) 0.0247(6) 0.5390(4) 0.057(2) Uani 1 1 d .
H3BA H 0.649283 0.003439 0.507700 0.068 Uiso 1 1 calc R
C4A C 0.6046(9) 0.4141(7) 0.8509(4) 0.0674(12) Uani 1 1 d .
H4A H 0.617978 0.429238 0.890167 0.081 Uiso 1 1 calc R
C4B C 0.5883(9) -0.0322(6) 0.5804(4) 0.063(3) Uani 1 1 d .
H4B H 0.601849 -0.092086 0.577611 0.075 Uiso 1 1 calc R
C5A C 0.6518(9) 0.3443(7) 0.8305(4) 0.0674(12) Uani 1 1 d .
H5A H 0.698280 0.311068 0.855922 0.081 Uiso 1 1 calc R
C5B C 0.5406(8) -0.0007(5) 0.6253(4) 0.059(3) Uani 1 1 d .
H5B H 0.521051 -0.039574 0.653435 0.071 Uiso 1 1 calc R
C6A C 0.6336(9) 0.3199(7) 0.7721(4) 0.0674(12) Uani 1 1 d .
C6B C 0.5204(6) 0.0867(5) 0.6306(3) 0.0439(19) Uani 1 1 d .
C7A C 0.6921(8) 0.2468(6) 0.7542(4) 0.063(3) Uani 1 1 d .
H7A H 0.723683 0.210522 0.783716 0.075 Uiso 1 1 calc R
C7B C 0.4670(7) 0.1127(5) 0.6795(4) 0.048(2) Uani 1 1 d .
H7B H 0.456542 0.069246 0.706715 0.058 Uiso 1 1 calc R
C8A C 0.7792(8) 0.1576(6) 0.6912(4) 0.060(3) Uani 1 1 d .
H8AA H 0.740962 0.109001 0.671187 0.072 Uiso 1 1 calc R
H8AB H 0.817247 0.135652 0.727171 0.072 Uiso 1 1 calc R
C8B C 0.3750(8) 0.2036(7) 0.7380(4) 0.062(3) Uani 1 1 d .
H8BA H 0.417327 0.238754 0.767078 0.075 Uiso 1 1 calc R
H8BB H 0.357509 0.148512 0.755815 0.075 Uiso 1 1 calc R
C9A C 0.8535(7) 0.1955(6) 0.6543(4) 0.061(3) Uani 1 1 d .
H9AA H 0.897982 0.149466 0.641019 0.073 Uiso 1 1 calc R
H9AB H 0.899148 0.237562 0.676693 0.073 Uiso 1 1 calc R
C9B C 0.2765(8) 0.2513(6) 0.7158(4) 0.057(2) Uani 1 1 d .
H9BA H 0.230044 0.213115 0.690742 0.068 Uiso 1 1 calc R
H9BB H 0.239056 0.269553 0.748257 0.068 Uiso 1 1 calc R
C10A C 0.8616(8) 0.2939(8) 0.5709(5) 0.078(3) Uani 1 1 d .
H10A H 0.817352 0.317106 0.537210 0.094 Uiso 1 1 calc R
H10B H 0.886788 0.343487 0.595027 0.094 Uiso 1 1 calc R
C10B C 0.2122(7) 0.3690(7) 0.6496(4) 0.062(2) Uani 1 1 d .
H10C H 0.236693 0.420330 0.630005 0.074 Uiso 1 1 calc R
H10D H 0.184270 0.327850 0.619597 0.074 Uiso 1 1 calc R
C11A C 0.9507(11) 0.2523(9) 0.5509(7) 0.110(5) Uani 1 1 d D
H11A H 1.000505 0.234340 0.583948 0.132 Uiso 1 1 calc R
H11B H 0.986718 0.292823 0.527324 0.132 Uiso 1 1 calc R
C11B C 0.1263(8) 0.3959(8) 0.6809(5) 0.084(4) Uani 1 1 d D
H11C H 0.069021 0.418895 0.653563 0.101 Uiso 1 1 calc R
H11D H 0.099331 0.345120 0.700051 0.101 Uiso 1 1 calc R
C12A C 0.3979(9) 0.5615(6) 0.7406(4) 0.066(3) Uani 1 1 d .
H12A H 0.446012 0.607053 0.755576 0.099 Uiso 1 1 calc GR
H12B H 0.359739 0.539947 0.771414 0.099 Uiso 1 1 calc GR
H12C H 0.348393 0.584781 0.709775 0.099 Uiso 1 1 calc GR
C12B C 0.6691(7) 0.1431(6) 0.4566(4) 0.057(2) Uani 1 1 d .
H12D H 0.621674 0.105310 0.432576 0.085 Uiso 1 1 calc GR
H12E H 0.732257 0.111077 0.470695 0.085 Uiso 1 1 calc GR
H12F H 0.687814 0.192645 0.434072 0.085 Uiso 1 1 calc GR
O4 O 0.2447(11) 0.4058(8) 0.8290(4) 0.149(5) Uani 1 1 d .
H4 H 0.302161 0.378778 0.830310 0.224 Uiso 1 1 d R
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'
Ni Ni 0.3393 1.1124 '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
Ni1 Tb01 Tb02 57.506(18) . 3_666
O1 Tb01 Tb02 73.21(15) . 3_666
O1 Tb01 Ni1 109.47(16) . .
O1 Tb01 O1B 153.72(19) . .
O1 Tb01 O2 95.46(19) . .
O1 Tb01 O2B 144.58(19) . .
O1 Tb01 O2C 81.7(2) . .
O1 Tb01 O2D 87.2(2) . .
O1 Tb01 O2E 95.4(2) . .
O1 Tb01 O3 75.76(19) . .
O1B Tb01 Tb02 129.04(12) . 3_666
O1B Tb01 Ni1 95.82(12) . .
O2 Tb01 Tb02 35.95(13) . 3_666
O2 Tb01 Ni1 73.12(13) . .
O2 Tb01 O1B 98.71(17) . .
O2 Tb01 O2B 70.14(16) . .
O2 Tb01 O3 67.58(18) . .
O2B Tb01 Tb02 77.14(11) . 3_666
O2B Tb01 Ni1 36.10(12) . .
O2B Tb01 O1B 61.63(17) . .
O2C Tb01 Tb02 154.77(13) . 3_666
O2C Tb01 Ni1 137.24(15) . .
O2C Tb01 O1B 74.71(18) . .
O2C Tb01 O2 148.8(2) . .
O2C Tb01 O2B 127.30(17) . .
O2C Tb01 O3 139.56(19) . .
O2D Tb01 Tb02 99.94(15) . 3_666
O2D Tb01 Ni1 143.45(15) . .
O2D Tb01 O1B 76.02(19) . .
O2D Tb01 O2 73.1(2) . .
O2D Tb01 O2B 117.00(19) . .
O2D Tb01 O2C 75.7(2) . .
O2D Tb01 O3 134.9(2) . .
O2E Tb01 Tb02 112.25(15) . 3_666
O2E Tb01 Ni1 65.78(14) . .
O2E Tb01 O1B 88.4(2) . .
O2E Tb01 O2 138.80(19) . .
O2E Tb01 O2B 78.20(18) . .
O2E Tb01 O2C 72.3(2) . .
O2E Tb01 O2D 147.1(2) . .
O2E Tb01 O3 76.92(19) . .
O3 Tb01 Tb02 35.33(12) . 3_666
O3 Tb01 Ni1 34.81(12) . .
O3 Tb01 O1B 130.23(17) . .
O3 Tb01 O2B 68.84(16) . .
Ni2 Tb02 Tb01 57.200(17) 3_666 3_666
O1 Tb02 Tb01 74.72(15) . 3_666
O1 Tb02 Ni2 111.44(15) . 3_666
O1 Tb02 O1A 150.97(19) . 3_666
O1 Tb02 O1C 81.8(2) . .
O1 Tb02 O1D 86.0(2) . .
O1 Tb02 O2 77.40(19) . 3_666
O1 Tb02 O2A 147.19(19) . 3_666
O1 Tb02 O2F 95.7(2) . 3_666
O1 Tb02 O3 96.64(19) . 3_666
O1A Tb02 Tb01 129.15(13) 3_666 3_666
O1A Tb02 Ni2 96.85(12) 3_666 3_666
O1C Tb02 Tb01 156.42(14) . 3_666
O1C Tb02 Ni2 136.48(15) . 3_666
O1C Tb02 O1A 72.98(19) . 3_666
O1C Tb02 O2 139.9(2) . 3_666
O1C Tb02 O2A 125.47(18) . 3_666
O1D Tb02 Tb01 100.36(16) . 3_666
O1D Tb02 Ni2 143.22(16) . 3_666
O1D Tb02 O1A 74.4(2) . 3_666
O1D Tb02 O1C 76.1(2) . .
O1D Tb02 O2 135.1(2) . 3_666
O1D Tb02 O2A 116.0(2) . 3_666
O1D Tb02 O2F 147.3(2) . 3_666
O1D Tb02 O3 73.3(2) . 3_666
O2 Tb02 Tb01 35.10(12) 3_666 3_666
O2 Tb02 Ni2 35.08(11) 3_666 3_666
O2 Tb02 O1A 131.49(17) 3_666 3_666
O2 Tb02 O2A 69.85(17) 3_666 3_666
O2A Tb02 Tb01 77.36(12) 3_666 3_666
O2A Tb02 Ni2 36.83(13) 3_666 3_666
O2A Tb02 O1A 61.83(17) 3_666 3_666
O2F Tb02 Tb01 111.65(15) 3_666 3_666
O2F Tb02 Ni2 65.78(14) 3_666 3_666
O2F Tb02 O1A 89.9(2) 3_666 3_666
O2F Tb02 O1C 71.9(2) 3_666 .
O2F Tb02 O2 76.56(19) 3_666 3_666
O2F Tb02 O2A 78.86(19) 3_666 3_666
O2F Tb02 O3 138.37(18) 3_666 3_666
O3 Tb02 Tb01 36.34(13) 3_666 3_666
O3 Tb02 Ni2 72.69(12) 3_666 3_666
O3 Tb02 O1A 97.90(18) 3_666 3_666
O3 Tb02 O1C 149.3(2) 3_666 .
O3 Tb02 O2 67.73(17) 3_666 3_666
O3 Tb02 O2A 69.46(16) 3_666 3_666
O1E Ni1 Tb01 82.15(16) . .
O1E Ni1 O2A 172.6(2) . .
O1E Ni1 N2B 89.9(3) . .
O2A Ni1 Tb01 90.46(14) . .
O2B Ni1 Tb01 44.75(13) . .
O2B Ni1 O1E 92.6(2) . .
O2B Ni1 O2A 81.5(2) . .
O2B Ni1 N2B 172.7(2) . .
O3 Ni1 Tb01 43.27(15) . .
O3 Ni1 O1E 93.9(2) . .
O3 Ni1 O2A 81.2(2) . .
O3 Ni1 O2B 85.2(2) . .
O3 Ni1 N2B 101.5(2) . .
N1B Ni1 Tb01 133.1(2) . .
N1B Ni1 O1E 89.5(2) . .
N1B Ni1 O2A 95.0(2) . .
N1B Ni1 O2B 90.1(2) . .
N1B Ni1 O3 174.4(3) . .
N1B Ni1 N2B 83.0(3) . .
N2B Ni1 Tb01 142.50(19) . .
N2B Ni1 O2A 96.5(2) . .
O1F Ni2 Tb02 83.04(16) . 3_666
O1F Ni2 O2A 94.6(2) . .
O1F Ni2 O2B 173.6(2) . .
O1F Ni2 N2A 87.0(3) . .
O2 Ni2 Tb02 43.28(15) . 3_666
O2 Ni2 O1F 93.1(2) . .
O2 Ni2 O2A 85.8(2) . .
O2 Ni2 O2B 81.90(19) . .
O2 Ni2 N2A 101.6(3) . .
O2A Ni2 Tb02 45.24(14) . 3_666
O2A Ni2 O2B 81.17(19) . .
O2A Ni2 N2A 172.4(2) . .
O2B Ni2 Tb02 90.62(12) . 3_666
N1A Ni2 Tb02 132.4(2) . 3_666
N1A Ni2 O1F 87.5(3) . .
N1A Ni2 O2 175.4(3) . .
N1A Ni2 O2A 89.7(3) . .
N1A Ni2 O2B 97.2(2) . .
N1A Ni2 N2A 83.0(3) . .
N2A Ni2 Tb02 142.4(2) . 3_666
N2A Ni2 O2B 97.8(2) . .
Tb01 O1 H1 112(8) . .
Tb02 O1 Tb01 132.1(3) . .
Tb02 O1 H1 103(8) . .
C2A O1A Tb02 112.7(6) . 3_666
C2A O1A C12A 116.4(7) . .
C12A O1A Tb02 123.4(5) . 3_666
C2B O1B Tb01 116.6(5) . .
C2B O1B C12B 117.4(6) . .
C12B O1B Tb01 123.0(5) . .
C1C O1C Tb02 139.3(5) . .
C1D O1D Tb02 142.8(6) . .
C1E O1E Ni1 126.0(5) . .
C1F O1F Ni2 126.6(5) . .
Tb01 O2 Tb02 109.0(2) . 3_666
Tb01 O2 H2 116(6) . .
Tb02 O2 H2 124(6) 3_666 .
Ni2 O2 Tb01 107.0(2) . .
Ni2 O2 Tb02 101.6(2) . 3_666
Ni2 O2 H2 96(6) . .
Ni1 O2A Tb02 98.63(17) . 3_666
Ni2 O2A Tb02 97.9(2) . 3_666
Ni2 O2A Ni1 98.3(2) . .
C1A O2A Tb02 114.6(5) . 3_666
C1A O2A Ni1 124.7(6) . .
C1A O2A Ni2 117.8(6) . .
Ni1 O2B Tb01 99.15(18) . .
Ni1 O2B Ni2 99.0(2) . .
Ni2 O2B Tb01 97.84(18) . .
C1B O2B Tb01 119.1(4) . .
C1B O2B Ni1 118.9(5) . .
C1B O2B Ni2 118.6(4) . .
C1C O2C Tb01 140.2(5) . .
C1D O2D Tb01 140.3(6) . .
C1E O2E Tb01 140.0(5) . .
C1F O2F Tb02 137.7(5) . 3_666
Tb01 O3 H3 112(5) . .
Tb02 O3 Tb01 108.3(2) 3_666 .
Tb02 O3 H3 115(5) 3_666 .
Ni1 O3 Tb01 101.9(2) . .
Ni1 O3 Tb02 108.0(2) . 3_666
Ni1 O3 H3 110(5) . .
C11A O3A H3A 109.7 . .
C11B O3B H3B 109.6 . .
C7A N1A Ni2 122.4(6) . .
C7A N1A C8A 122.1(8) . .
C8A N1A Ni2 112.1(6) . .
C7B N1B Ni1 125.0(6) . .
C7B N1B C8B 121.1(7) . .
C8B N1B Ni1 112.3(5) . .
Ni2 N2A H2A 107.6 . .
C9A N2A Ni2 105.3(6) . .
C9A N2A H2A 107.6 . .
C10A N2A Ni2 114.3(6) . .
C10A N2A H2A 107.6 . .
C10A N2A C9A 114.1(7) . .
Ni1 N2B H2B 108.2 . .
C9B N2B Ni1 105.3(5) . .
C9B N2B H2B 108.2 . .
C9B N2B C10B 112.5(7) . .
C10B N2B Ni1 114.4(5) . .
C10B N2B H2B 108.2 . .
O2A C1A C2A 117.5(8) . .
O2A C1A C6A 123.6(9) . .
C2A C1A C6A 118.8(9) . .
O2B C1B C2B 116.9(7) . .
O2B C1B C6B 125.4(7) . .
C2B C1B C6B 117.7(7) . .
O1C C1C O2C 125.8(7) . .
O1C C1C C2C 116.6(7) . .
O2C C1C C2C 117.5(7) . .
O1D C1D C2D 117.9(8) . .
O2D C1D O1D 124.6(8) . .
O2D C1D C2D 117.4(8) . .
O1E C1E C2E 117.5(8) . .
O2E C1E O1E 125.0(7) . .
O2E C1E C2E 117.5(8) . .
O1F C1F C2F 115.6(8) . .
O2F C1F O1F 126.9(8) . .
O2F C1F C2F 117.5(8) . .
O1A C2A C1A 114.3(8) . .
C3A C2A O1A 124.1(9) . .
C3A C2A C1A 121.5(9) . .
O1B C2B C1B 114.7(7) . .
O1B C2B C3B 124.2(8) . .
C3B C2B C1B 121.2(8) . .
C1C C2C H2CA 109.5 . .
C1C C2C H2CB 109.5 . .
C1C C2C H2CC 109.5 . .
H2CA C2C H2CB 109.5 . .
H2CA C2C H2CC 109.5 . .
H2CB C2C H2CC 109.5 . .
C1D C2D H2DA 109.5 . .
C1D C2D H2DB 109.5 . .
C1D C2D H2DC 109.5 . .
H2DA C2D H2DB 109.5 . .
H2DA C2D H2DC 109.5 . .
H2DB C2D H2DC 109.5 . .
C1E C2E H2EA 110.1 . .
C1E C2E H2EB 108.3 . .
C1E C2E H2EC 110.0 . .
H2EA C2E H2EB 109.5 . .
H2EA C2E H2EC 109.5 . .
H2EB C2E H2EC 109.5 . .
C1F C2F H2FA 109.5 . .
C1F C2F H2FB 109.5 . .
C1F C2F H2FC 109.5 . .
H2FA C2F H2FB 109.5 . .
H2FA C2F H2FC 109.5 . .
H2FB C2F H2FC 109.5 . .
C2A C3A H3AA 119.9 . .
C2A C3A C4A 120.2(10) . .
C4A C3A H3AA 119.9 . .
C2B C3B H3BA 119.9 . .
C2B C3B C4B 120.2(9) . .
C4B C3B H3BA 119.9 . .
C3A C4A H4A 120.1 . .
C5A C4A C3A 119.8(9) . .
C5A C4A H4A 120.1 . .
C3B C4B H4B 120.3 . .
C5B C4B C3B 119.4(8) . .
C5B C4B H4B 120.3 . .
C4A C5A H5A 119.2 . .
C4A C5A C6A 121.6(9) . .
C6A C5A H5A 119.2 . .
C4B C5B H5B 119.3 . .
C4B C5B C6B 121.4(9) . .
C6B C5B H5B 119.3 . .
C1A C6A C5A 118.0(10) . .
C1A C6A C7A 124.6(9) . .
C5A C6A C7A 117.1(8) . .
C1B C6B C7B 123.1(7) . .
C5B C6B C1B 120.2(9) . .
C5B C6B C7B 116.7(8) . .
N1A C7A C6A 127.2(8) . .
N1A C7A H7A 116.4 . .
C6A C7A H7A 116.4 . .
N1B C7B C6B 126.5(7) . .
N1B C7B H7B 116.8 . .
C6B C7B H7B 116.8 . .
N1A C8A H8AA 110.2 . .
N1A C8A H8AB 110.2 . .
N1A C8A C9A 107.7(7) . .
H8AA C8A H8AB 108.5 . .
C9A C8A H8AA 110.2 . .
C9A C8A H8AB 110.2 . .
N1B C8B H8BA 110.2 . .
N1B C8B H8BB 110.2 . .
N1B C8B C9B 107.7(7) . .
H8BA C8B H8BB 108.5 . .
C9B C8B H8BA 110.2 . .
C9B C8B H8BB 110.2 . .
N2A C9A H9AA 109.6 . .
N2A C9A H9AB 109.6 . .
C8A C9A N2A 110.2(7) . .
C8A C9A H9AA 109.6 . .
C8A C9A H9AB 109.6 . .
H9AA C9A H9AB 108.1 . .
N2B C9B C8B 108.8(7) . .
N2B C9B H9BA 109.9 . .
N2B C9B H9BB 109.9 . .
C8B C9B H9BA 109.9 . .
C8B C9B H9BB 109.9 . .
H9BA C9B H9BB 108.3 . .
N2A C10A H10A 108.2 . .
N2A C10A H10B 108.2 . .
H10A C10A H10B 107.3 . .
C11A C10A N2A 116.4(11) . .
C11A C10A H10A 108.2 . .
C11A C10A H10B 108.2 . .
N2B C10B H10C 107.9 . .
N2B C10B H10D 107.9 . .
H10C C10B H10D 107.2 . .
C11B C10B N2B 117.6(9) . .
C11B C10B H10C 107.9 . .
C11B C10B H10D 107.9 . .
O3A C11A H11A 109.9 . .
O3A C11A H11B 109.9 . .
C10A C11A O3A 108.7(11) . .
C10A C11A H11A 109.9 . .
C10A C11A H11B 109.9 . .
H11A C11A H11B 108.3 . .
O3B C11B C10B 112.1(10) . .
O3B C11B H11C 109.2 . .
O3B C11B H11D 109.2 . .
C10B C11B H11C 109.2 . .
C10B C11B H11D 109.2 . .
H11C C11B H11D 107.9 . .
O1A C12A H12A 109.5 . .
O1A C12A H12B 109.5 . .
O1A C12A H12C 109.5 . .
H12A C12A H12B 109.5 . .
H12A C12A H12C 109.5 . .
H12B C12A H12C 109.5 . .
O1B C12B H12D 109.5 . .
O1B C12B H12E 109.5 . .
O1B C12B H12F 109.5 . .
H12D C12B H12E 109.5 . .
H12D C12B H12F 109.5 . .
H12E C12B H12F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb01 Tb02 3.8910(5) 3_666
Tb01 Ni1 3.4675(10) .
Tb01 O1 2.259(5) .
Tb01 O1B 2.591(5) .
Tb01 O2 2.365(5) .
Tb01 O2B 2.473(5) .
Tb01 O2C 2.363(5) .
Tb01 O2D 2.341(6) .
Tb01 O2E 2.327(6) .
Tb01 O3 2.429(5) .
Tb02 Tb01 3.8911(5) 3_666
Tb02 Ni2 3.4509(10) 3_666
Tb02 O1 2.253(6) .
Tb02 O1A 2.570(6) 3_666
Tb02 O1C 2.371(5) .
Tb02 O1D 2.327(6) .
Tb02 O2 2.415(5) 3_666
Tb02 O2A 2.474(5) 3_666
Tb02 O2F 2.353(6) 3_666
Tb02 O3 2.370(5) 3_666
Ni1 O1E 2.081(6) .
Ni1 O2A 2.214(5) .
Ni1 O2B 2.070(5) .
Ni1 O3 2.023(5) .
Ni1 N1B 2.002(6) .
Ni1 N2B 2.130(7) .
Ni2 Tb02 3.4509(10) 3_666
Ni2 O1F 2.040(5) .
Ni2 O2 2.025(5) .
Ni2 O2A 2.089(5) .
Ni2 O2B 2.213(5) .
Ni2 N1A 2.017(7) .
Ni2 N2A 2.122(7) .
O1 H1 0.850(2) .
O1A Tb02 2.570(6) 3_666
O1A C2A 1.368(10) .
O1A C12A 1.487(10) .
O1B C2B 1.375(9) .
O1B C12B 1.420(10) .
O1C C1C 1.244(9) .
O1D C1D 1.259(10) .
O1E C1E 1.269(9) .
O1F C1F 1.254(10) .
O2 Tb02 2.415(5) 3_666
O2 H2 0.850(2) .
O2A Tb02 2.474(5) 3_666
O2A C1A 1.368(10) .
O2B C1B 1.353(8) .
O2C C1C 1.245(9) .
O2D C1D 1.237(10) .
O2E C1E 1.245(10) .
O2F Tb02 2.353(6) 3_666
O2F C1F 1.252(10) .
O3 Tb02 2.370(5) 3_666
O3 H3 0.850(2) .
O3A H3A 0.8193 .
O3A C11A 1.445(11) .
O3B H3B 0.8200 .
O3B C11B 1.445(11) .
N1A C7A 1.263(12) .
N1A C8A 1.478(11) .
N1B C7B 1.263(10) .
N1B C8B 1.469(11) .
N2A H2A 1.0000 .
N2A C9A 1.494(11) .
N2A C10A 1.484(13) .
N2B H2B 1.0000 .
N2B C9B 1.487(11) .
N2B C10B 1.498(11) .
C1A C2A 1.397(14) .
C1A C6A 1.401(13) .
C1B C2B 1.406(11) .
C1B C6B 1.410(11) .
C1C C2C 1.503(11) .
C1D C2D 1.525(13) .
C1E C2E 1.504(12) .
C1F C2F 1.494(13) .
C2A C3A 1.365(13) .
C2B C3B 1.386(11) .
C2C H2CA 0.9800 .
C2C H2CB 0.9800 .
C2C H2CC 0.9800 .
C2D H2DA 0.9800 .
C2D H2DB 0.9800 .
C2D H2DC 0.9800 .
C2E H2EA 0.9592 .
C2E H2EB 0.9600 .
C2E H2EC 0.9595 .
C2F H2FA 0.9800 .
C2F H2FB 0.9800 .
C2F H2FC 0.9800 .
C3A H3AA 0.9500 .
C3A C4A 1.379(13) .
C3B H3BA 0.9500 .
C3B C4B 1.394(14) .
C4A H4A 0.9500 .
C4A C5A 1.358(14) .
C4B H4B 0.9500 .
C4B C5B 1.372(14) .
C5A H5A 0.9500 .
C5A C6A 1.419(12) .
C5B H5B 0.9500 .
C5B C6B 1.390(11) .
C6A C7A 1.453(14) .
C6B C7B 1.465(12) .
C7A H7A 0.9500 .
C7B H7B 0.9500 .
C8A H8AA 0.9900 .
C8A H8AB 0.9900 .
C8A C9A 1.487(14) .
C8B H8BA 0.9900 .
C8B H8BB 0.9900 .
C8B C9B 1.513(13) .
C9A H9AA 0.9900 .
C9A H9AB 0.9900 .
C9B H9BA 0.9900 .
C9B H9BB 0.9900 .
C10A H10A 0.9900 .
C10A H10B 0.9900 .
C10A C11A 1.445(16) .
C10B H10C 0.9900 .
C10B H10D 0.9900 .
C10B C11B 1.462(14) .
C11A H11A 0.9900 .
C11A H11B 0.9900 .
C11B H11C 0.9900 .
C11B H11D 0.9900 .
C12A H12A 0.9800 .
C12A H12B 0.9800 .
C12A H12C 0.9800 .
C12B H12D 0.9800 .
C12B H12E 0.9800 .
C12B H12F 0.9800 .
O4 H4 0.8499 .
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
Tb01 O1B C2B C1B -20.3(8) .
Tb01 O1B C2B C3B 158.7(7) .
Tb01 O2B C1B C2B 31.2(8) .
Tb01 O2B C1B C6B -151.6(6) .
Tb01 O2C C1C O1C -19.1(16) .
Tb01 O2C C1C C2C 162.9(8) .
Tb01 O2D C1D O1D 10.7(15) .
Tb01 O2D C1D C2D -170.3(8) .
Tb01 O2E C1E O1E -12.1(15) .
Tb01 O2E C1E C2E 168.8(8) .
Tb02 O1A C2A C1A -33.5(11) 3_666
Tb02 O1A C2A C3A 144.0(10) 3_666
Tb02 O1C C1C O2C 20.7(15) .
Tb02 O1C C1C C2C -161.4(8) .
Tb02 O1D C1D O2D -11.5(16) .
Tb02 O1D C1D C2D 169.5(8) .
Tb02 O2A C1A C2A 32.9(12) 3_666
Tb02 O2A C1A C6A -145.2(10) 3_666
Tb02 O2F C1F O1F -0.1(16) 3_666
Tb02 O2F C1F C2F 178.3(8) 3_666
Ni1 O1E C1E O2E 13.9(12) .
Ni1 O1E C1E C2E -166.9(7) .
Ni1 O2A C1A C2A -88.3(11) .
Ni1 O2A C1A C6A 93.6(12) .
Ni1 O2B C1B C2B 152.2(5) .
Ni1 O2B C1B C6B -30.6(9) .
Ni1 N1B C7B C6B 11.8(12) .
Ni1 N1B C8B C9B 36.2(9) .
Ni1 N2B C9B C8B 42.9(8) .
Ni1 N2B C10B C11B 176.3(8) .
Ni2 O1F C1F O2F 1.4(14) .
Ni2 O1F C1F C2F -177.0(8) .
Ni2 O2A C1A C2A 147.3(9) .
Ni2 O2A C1A C6A -30.8(14) .
Ni2 O2B C1B C2B -87.5(7) .
Ni2 O2B C1B C6B 89.6(8) .
Ni2 N1A C7A C6A 13.5(16) .
Ni2 N1A C8A C9A 35.3(8) .
Ni2 N2A C9A C8A 42.3(8) .
Ni2 N2A C10A C11A 175.8(9) .
O1A C2A C3A C4A -176.9(10) .
O1B C2B C3B C4B -178.0(8) .
O2A C1A C2A O1A 1.7(15) .
O2A C1A C2A C3A -175.9(10) .
O2A C1A C6A C5A 174.3(10) .
O2A C1A C6A C7A 0.5(19) .
O2B C1B C2B O1B -5.7(10) .
O2B C1B C2B C3B 175.2(7) .
O2B C1B C6B C5B -175.1(7) .
O2B C1B C6B C7B 5.5(12) .
N1A C8A C9A N2A -51.9(10) .
N1B C8B C9B N2B -53.0(10) .
N2A C10A C11A O3A 55.9(16) .
N2B C10B C11B O3B 61.8(14) .
C1A C2A C3A C4A 0.4(19) .
C1A C6A C7A N1A 10.7(19) .
C1B C2B C3B C4B 1.0(14) .
C1B C6B C7B N1B 6.2(13) .
C2A C1A C6A C5A -3.8(17) .
C2A C1A C6A C7A -177.6(11) .
C2A C3A C4A C5A -1.6(18) .
C2B C1B C6B C5B 2.1(11) .
C2B C1B C6B C7B -177.4(7) .
C2B C3B C4B C5B 0.3(15) .
C3A C4A C5A C6A 0.0(18) .
C3B C4B C5B C6B -0.3(15) .
C4A C5A C6A C1A 2.7(18) .
C4A C5A C6A C7A 177.0(11) .
C4B C5B C6B C1B -0.9(14) .
C4B C5B C6B C7B 178.6(8) .
C5A C6A C7A N1A -163.2(11) .
C5B C6B C7B N1B -173.2(8) .
C6A C1A C2A O1A 179.9(10) .
C6A C1A C2A C3A 2.3(18) .
C6B C1B C2B O1B 176.9(6) .
C6B C1B C2B C3B -2.1(12) .
C7A N1A C8A C9A -124.3(10) .
C7B N1B C8B C9B -129.8(9) .
C8A N1A C7A C6A 171.0(10) .
C8B N1B C7B C6B 176.0(8) .
C9A N2A C10A C11A 54.4(13) .
C9B N2B C10B C11B 56.2(12) .
C10A N2A C9A C8A 168.5(8) .
C10B N2B C9B C8B 168.1(8) .
C12A O1A C2A C1A 175.7(10) .
C12A O1A C2A C3A -6.9(15) .
C12B O1B C2B C1B 178.4(7) .
C12B O1B C2B C3B -2.5(12) .
