#------------------------------------------------------------------------------
#$Date: 2022-01-07 01:08:26 +0200 (Fri, 07 Jan 2022) $
#$Revision: 271904 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243985.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243985
loop_
_publ_author_name
'Pavlishchuk, Anna V.'
'Vasylenko, Inna V.'
'Zeller, Matthias'
'Addison, Anthony W.'
_publ_section_title
;
 Crystal structure of a TbIII--CuII glycinehydroxamate
 15-metallacrown-5 sulfate complex
;
_journal_coeditor_code           YY2004
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1197
_journal_page_last               1202
_journal_paper_doi               10.1107/S2056989021011907
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac
'[Tb Cu5 (C2 H4 N2 O2)5 (S O4) (H2 O)6.5]2 (S O4), 6H2 O'
_chemical_formula_moiety
'2(C10 H33 Cu5 N10 O20.50 S Tb +), O4 S 2-, 6(H2 O)'
_chemical_formula_sum            'C20 H78 Cu10 N20 O51 S3 Tb2'
_chemical_formula_weight         2464.44
_chemical_name_systematic
'Bis[hexaaquahemiaquapentakis(μ₃-glycinehydroxamato)sulfatopentacopper(II)terbium(III)] sulfate hexahydrate'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                99.6716(13)
_cell_angle_beta                 91.3031(12)
_cell_angle_gamma                105.3123(12)
_cell_formula_units_Z            1
_cell_length_a                   9.6370(4)
_cell_length_b                   11.5888(5)
_cell_length_c                   16.2367(6)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      79.9275
_cell_measurement_theta_min      4.0210
_cell_volume                     1719.81(12)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015),
shelXle  (Hübschle et al.,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest CMOS diffractometer with PhotonII charge-integrating pixel
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16278
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.280
_diffrn_reflns_theta_min         2.768
_diffrn_source                   'I-mu-S microsource X-ray tube'
_diffrn_source_current           '1.0 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    15.108
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.4537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al.,  2015
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_description       plate
_exptl_crystal_F_000             1214
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.590
_refine_diff_density_min         -1.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7029
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0656P)²+1.8351P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                6786
_reflns_number_total             7029
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            yy2004sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1719.80(12)
_cod_database_code               2243985
_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_min   0.152
_shelx_estimated_absorpt_t_max   0.378
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.4433(5) 0.2625(4) 0.5042(3) 0.0167(8) Uani d 1 . .
C C2 0.3610(5) 0.2938(4) 0.5788(3) 0.0195(9) Uani d 1 . .
H H2C 0.320220 0.220082 0.602893 0.023 Uiso calc 1 . .
H H2D 0.427084 0.354919 0.622292 0.023 Uiso calc 1 . .
C C3 0.6783(5) 0.0423(4) 0.2493(3) 0.0158(8) Uani d 1 . .
C C4 0.6931(6) -0.0360(5) 0.3110(3) 0.0235(10) Uani d 1 . .
H H4C 0.794720 -0.038433 0.316648 0.028 Uiso calc 1 . .
H H4D 0.632740 -0.119964 0.290399 0.028 Uiso calc 1 . .
C C5 0.7890(5) 0.3483(4) 0.0317(3) 0.0175(9) Uani d 1 . .
C C6 0.8858(5) 0.2707(4) -0.0019(3) 0.0221(10) Uani d 1 . .
H H6C 0.874472 0.253424 -0.063895 0.027 Uiso calc 1 . .
H H6D 0.987712 0.315424 0.015213 0.027 Uiso calc 1 . .
C C7 0.5254(5) 0.6985(4) 0.1304(3) 0.0159(8) Uani d 1 . .
C C8 0.6022(5) 0.7507(4) 0.0594(3) 0.0179(9) Uani d 1 . .
H H8C 0.532673 0.736705 0.010561 0.022 Uiso calc 1 . .
H H8D 0.643978 0.839491 0.076935 0.022 Uiso calc 1 . .
C C9 0.2149(5) 0.5808(4) 0.3895(3) 0.0163(9) Uani d 1 . .
C C10 0.1644(5) 0.6898(4) 0.3802(3) 0.0222(10) Uani d 1 . .
H H10C 0.058903 0.664428 0.366493 0.027 Uiso calc 1 . .
H H10D 0.184336 0.748022 0.434014 0.027 Uiso calc 1 . .
Cu Cu1 0.57451(7) 0.15475(6) 0.38923(4) 0.01792(16) Uani d 1 . .
Cu Cu2 0.71639(7) 0.16393(6) 0.12404(4) 0.01884(16) Uani d 1 . .
Cu Cu3 0.68477(7) 0.53540(6) 0.08031(4) 0.01553(15) Uani d 1 . .
Cu Cu4 0.34975(7) 0.64627(6) 0.24858(4) 0.01548(15) Uani d 1 . .
Cu Cu5 0.28203(7) 0.39948(6) 0.44370(4) 0.01615(15) Uani d 1 . .
Tb Tb1 0.48345(2) 0.35681(2) 0.24306(2) 0.01322(9) Uani d 1 . .
N N1 0.4245(4) 0.3141(3) 0.4416(2) 0.0171(7) Uani d 1 . .
N N2 0.2431(4) 0.3430(4) 0.5530(2) 0.0195(8) Uani d 1 . .
H H2A 0.236548 0.406266 0.592889 0.023 Uiso calc 1 . .
H H2B 0.157731 0.284301 0.547628 0.023 Uiso calc 1 . .
N N3 0.6105(4) 0.1242(3) 0.2732(2) 0.0178(7) Uani d 1 . .
N N4 0.6482(5) 0.0108(4) 0.3943(3) 0.0215(8) Uani d 1 . .
H H4A 0.724750 0.031948 0.432837 0.026 Uiso calc 1 . .
H H4B 0.577960 -0.048780 0.410697 0.026 Uiso calc 1 . .
N N5 0.7027(4) 0.3075(3) 0.0865(2) 0.0166(7) Uani d 1 . .
N N6 0.8492(4) 0.1541(3) 0.0304(2) 0.0171(7) Uani d 1 . .
H H6A 0.931299 0.139490 0.049586 0.021 Uiso calc 1 . .
H H6B 0.805401 0.091646 -0.011692 0.021 Uiso calc 1 . .
N N7 0.5575(4) 0.6039(3) 0.1480(2) 0.0172(7) Uani d 1 . .
N N8 0.7190(4) 0.6918(3) 0.0356(2) 0.0159(7) Uani d 1 . .
H H8A 0.805912 0.742721 0.057077 0.019 Uiso calc 1 . .
H H8B 0.720395 0.676114 -0.021109 0.019 Uiso calc 1 . .
N N9 0.2929(4) 0.5471(3) 0.3302(2) 0.0173(7) Uani d 1 . .
N N10 0.2378(4) 0.7509(4) 0.3133(3) 0.0226(8) Uani d 1 . .
H H10A 0.298699 0.824200 0.336523 0.027 Uiso calc 1 . .
H H10B 0.171092 0.763954 0.278010 0.027 Uiso calc 1 . .
O O1 0.5000(3) 0.2882(3) 0.37163(19) 0.0166(6) Uani d 1 . .
O O2 0.5244(4) 0.1896(3) 0.5060(2) 0.0196(6) Uani d 1 . .
O O3 0.6029(4) 0.1998(3) 0.2163(2) 0.0199(7) Uani d 1 . .
O O4 0.7336(4) 0.0300(3) 0.1769(2) 0.0196(7) Uani d 1 . .
O O5 0.6158(3) 0.3809(3) 0.11866(19) 0.0157(6) Uani d 1 . .
O O6 0.7979(4) 0.4510(3) 0.0074(2) 0.0189(6) Uani d 1 . .
O O7 0.4861(3) 0.5537(3) 0.2123(2) 0.0166(6) Uani d 1 . .
O O8 0.4330(3) 0.7478(3) 0.1689(2) 0.0193(6) Uani d 1 . .
O O9 0.3463(3) 0.4493(3) 0.3393(2) 0.0170(6) Uani d 1 . .
O O10 0.1827(4) 0.5265(3) 0.4519(2) 0.0195(7) Uani d 1 . .
O O11 0.2853(4) 0.1696(3) 0.2229(2) 0.0238(7) Uani d 1 . .
O O12 0.2734(4) 0.3216(3) 0.1464(2) 0.0205(7) Uani d 1 . .
O O13 0.1448(4) 0.1123(3) 0.0876(2) 0.0253(7) Uani d 1 . .
O O14 0.0575(4) 0.2189(4) 0.2058(2) 0.0311(8) Uani d 1 . .
O O15 0.7222(3) 0.4609(3) 0.3006(2) 0.0184(6) Uani d 1 . .
H H15A 0.767(6) 0.430(5) 0.331(3) 0.028 Uiso d 1 . .
H H15B 0.782(5) 0.495(5) 0.269(3) 0.028 Uiso d 1 . .
O O16 0.8851(4) 0.5789(3) 0.1920(2) 0.0254(7) Uani d 1 . .
H H16A 0.960(5) 0.557(6) 0.184(4) 0.038 Uiso d 1 . .
H H16B 0.917(7) 0.653(2) 0.213(4) 0.038 Uiso d 1 . .
O O17 0.1408(4) 0.5205(3) 0.1525(2) 0.0220(7) Uani d 1 . .
H H17A 0.163(7) 0.457(4) 0.156(4) 0.033 Uiso d 1 . .
H H17B 0.155(7) 0.528(6) 0.1031(18) 0.033 Uiso d 1 . .
O O18 0.0716(4) 0.2521(3) 0.3767(2) 0.0241(7) Uani d 1 . .
H H18A 0.043(7) 0.185(3) 0.393(4) 0.036 Uiso d 1 . .
H H18B 0.070(7) 0.236(6) 0.3246(13) 0.036 Uiso d 1 . .
O O19 0.5200(11) 0.0381(11) 0.0275(6) 0.047(2) Uani d 0.5 A -1
H H19A 0.472(19) -0.003(15) 0.060(9) 0.071 Uiso d 0.5 B -1
H H19B 0.55(2) 0.02(2) -0.021(6) 0.071 Uiso d 0.5 C -1
O O20 0.3102(4) 0.0221(3) 0.3519(3) 0.0283(8) Uani d 1 . .
H H20A 0.236(5) 0.022(7) 0.377(4) 0.043 Uiso d 1 . .
H H20B 0.291(8) 0.063(6) 0.318(4) 0.043 Uiso d 1 . .
O O21 0.8274(4) 0.3337(4) 0.3966(2) 0.0308(8) Uani d 1 . .
H H21A 0.909(4) 0.320(7) 0.392(5) 0.046 Uiso d 1 . .
H H21B 0.841(8) 0.380(6) 0.443(3) 0.046 Uiso d 1 . .
O O22 0.9749(5) 0.8150(4) 0.2711(3) 0.0361(9) Uani d 1 . .
H H22A 0.972(9) 0.855(7) 0.319(2) 0.054 Uiso d 1 . .
H H22B 0.980(9) 0.857(6) 0.234(4) 0.054 Uiso d 1 . .
O O23 0.9394(4) 0.9116(3) 0.1345(2) 0.0243(7) Uani d 1 . .
H H23A 0.876(4) 0.947(5) 0.150(4) 0.036 Uiso d 1 . .
H H23B 1.011(4) 0.968(4) 0.126(4) 0.036 Uiso d 1 . .
O O24 0.3431(7) 0.9430(4) 0.1264(3) 0.0523(14) Uani d 1 . .
H H24A 0.328(11) 0.998(6) 0.163(4) 0.079 Uiso d 1 . .
H H24B 0.368(10) 0.893(6) 0.152(4) 0.079 Uiso d 1 . .
O O25 0.1618(8) 0.0365(9) 0.4920(5) 0.0357(19) Uani d 0.5 D -1
O O26 -0.0300(9) -0.0158(7) 0.5820(5) 0.0339(17) Uani d 0.5 D -1
O O27 -0.0484(9) 0.1032(7) 0.4781(5) 0.0333(17) Uani d 0.5 D -1
O O28 -0.0592(9) -0.1078(7) 0.4360(5) 0.0346(17) Uani d 0.5 D -1
S S1 0.18461(12) 0.20240(10) 0.16476(7) 0.0195(2) Uani d 1 . .
S S2 0.000000 0.000000 0.500000 0.0199(3) Uani d 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 C1 O2 . . 125.3(4) ?
N1 C1 C2 . . 114.2(4) ?
O2 C1 C2 . . 120.5(4) ?
N2 C2 C1 . . 110.0(4) ?
N2 C2 H2C . . 109.7 ?
C1 C2 H2C . . 109.7 ?
N2 C2 H2D . . 109.7 ?
C1 C2 H2D . . 109.7 ?
H2C C2 H2D . . 108.2 ?
N3 C3 O4 . . 123.0(4) ?
N3 C3 C4 . . 115.9(4) ?
O4 C3 C4 . . 121.1(4) ?
C3 C4 N4 . . 111.1(4) ?
C3 C4 H4C . . 109.4 ?
N4 C4 H4C . . 109.4 ?
C3 C4 H4D . . 109.4 ?
N4 C4 H4D . . 109.4 ?
H4C C4 H4D . . 108.0 ?
N5 C5 O6 . . 123.7(4) ?
N5 C5 C6 . . 116.0(4) ?
O6 C5 C6 . . 120.3(4) ?
N6 C6 C5 . . 110.5(4) ?
N6 C6 H6C . . 109.5 ?
C5 C6 H6C . . 109.5 ?
N6 C6 H6D . . 109.5 ?
C5 C6 H6D . . 109.5 ?
H6C C6 H6D . . 108.1 ?
N7 C7 O8 . . 124.1(4) ?
N7 C7 C8 . . 115.5(4) ?
O8 C7 C8 . . 120.4(4) ?
N8 C8 C7 . . 109.8(4) ?
N8 C8 H8C . . 109.7 ?
C7 C8 H8C . . 109.7 ?
N8 C8 H8D . . 109.7 ?
C7 C8 H8D . . 109.7 ?
H8C C8 H8D . . 108.2 ?
O10 C9 N9 . . 123.8(4) ?
O10 C9 C10 . . 121.2(4) ?
N9 C9 C10 . . 115.0(4) ?
N10 C10 C9 . . 111.3(4) ?
N10 C10 H10C . . 109.4 ?
C9 C10 H10C . . 109.4 ?
N10 C10 H10D . . 109.4 ?
C9 C10 H10D . . 109.4 ?
H10C C10 H10D . . 108.0 ?
N3 Cu1 O1 . . 90.36(14) ?
N3 Cu1 O2 . . 175.68(15) ?
O1 Cu1 O2 . . 86.12(13) ?
N3 Cu1 N4 . . 83.85(16) ?
O1 Cu1 N4 . . 173.91(15) ?
O2 Cu1 N4 . . 99.57(15) ?
N3 Cu1 O20 . . 89.10(15) ?
O1 Cu1 O20 . . 85.07(13) ?
O2 Cu1 O20 . . 88.10(14) ?
N4 Cu1 O20 . . 92.89(15) ?
N3 Cu1 O21 . . 82.42(14) ?
O1 Cu1 O21 . . 80.09(13) ?
O2 Cu1 O21 . . 99.41(13) ?
N4 Cu1 O21 . . 100.98(15) ?
O20 Cu1 O21 . . 162.82(12) ?
N5 Cu2 O3 . . 89.51(15) ?
N5 Cu2 O4 . . 172.53(15) ?
O3 Cu2 O4 . . 84.79(13) ?
N5 Cu2 N6 . . 83.61(16) ?
O3 Cu2 N6 . . 171.24(15) ?
O4 Cu2 N6 . . 101.58(15) ?
N5 Cu2 O19 . . 92.3(3) ?
O3 Cu2 O19 . . 97.4(3) ?
O4 Cu2 O19 . . 93.2(3) ?
N6 Cu2 O19 . . 88.3(3) ?
N7 Cu3 O6 . . 174.11(15) ?
N7 Cu3 O5 . . 91.24(15) ?
O6 Cu3 O5 . . 84.79(13) ?
N7 Cu3 N8 . . 82.67(16) ?
O6 Cu3 N8 . . 100.63(14) ?
O5 Cu3 N8 . . 169.87(14) ?
N7 Cu3 O16 . . 96.61(14) ?
O6 Cu3 O16 . . 87.37(13) ?
O5 Cu3 O16 . . 84.87(13) ?
N8 Cu3 O16 . . 103.81(14) ?
N9 Cu4 O8 . . 172.67(15) ?
N9 Cu4 O7 . . 89.19(15) ?
O8 Cu4 O7 . . 85.34(13) ?
N9 Cu4 N10 . . 83.73(17) ?
O8 Cu4 N10 . . 100.54(16) ?
O7 Cu4 N10 . . 165.82(17) ?
N9 Cu4 O17 . . 90.56(14) ?
O8 Cu4 O17 . . 94.98(13) ?
O7 Cu4 O17 . . 97.53(13) ?
N10 Cu4 O17 . . 94.81(15) ?
N1 Cu5 O9 . . 88.98(14) ?
N1 Cu5 O10 . . 163.89(16) ?
O9 Cu5 O10 . . 85.41(13) ?
N1 Cu5 N2 . . 83.21(16) ?
O9 Cu5 N2 . . 171.78(14) ?
O10 Cu5 N2 . . 101.44(14) ?
N1 Cu5 O18 . . 104.51(15) ?
O9 Cu5 O18 . . 93.14(13) ?
O10 Cu5 O18 . . 90.88(14) ?
N2 Cu5 O18 . . 91.31(15) ?
O9 Tb1 O1 . . 71.67(10) ?
O9 Tb1 O15 . . 100.80(11) ?
O1 Tb1 O15 . . 75.87(11) ?
O9 Tb1 O3 . . 144.63(11) ?
O1 Tb1 O3 . . 73.91(10) ?
O15 Tb1 O3 . . 78.22(11) ?
O9 Tb1 O7 . . 70.65(10) ?
O1 Tb1 O7 . . 131.81(10) ?
O15 Tb1 O7 . . 82.82(11) ?
O3 Tb1 O7 . . 142.47(10) ?
O9 Tb1 O5 . . 143.39(10) ?
O1 Tb1 O5 . . 139.79(10) ?
O15 Tb1 O5 . . 77.50(11) ?
O3 Tb1 O5 . . 71.55(10) ?
O7 Tb1 O5 . . 72.88(10) ?
O9 Tb1 O12 . . 83.74(11) ?
O1 Tb1 O12 . . 129.16(11) ?
O15 Tb1 O12 . . 153.99(11) ?
O3 Tb1 O12 . . 112.70(11) ?
O7 Tb1 O12 . . 74.50(11) ?
O5 Tb1 O12 . . 83.70(11) ?
O9 Tb1 O11 . . 88.43(11) ?
O1 Tb1 O11 . . 77.71(11) ?
O15 Tb1 O11 . . 147.49(12) ?
O3 Tb1 O11 . . 76.51(12) ?
O7 Tb1 O11 . . 129.39(11) ?
O5 Tb1 O11 . . 112.83(11) ?
O12 Tb1 O11 . . 57.34(11) ?
O9 Tb1 S1 . . 83.26(8) ?
O1 Tb1 S1 . . 102.84(8) ?
O15 Tb1 S1 . . 174.96(8) ?
O3 Tb1 S1 . . 96.74(9) ?
O7 Tb1 S1 . . 101.43(8) ?
O5 Tb1 S1 . . 101.06(8) ?
O12 Tb1 S1 . . 28.74(8) ?
O11 Tb1 S1 . . 28.77(8) ?
C1 N1 O1 . . 115.9(3) ?
C1 N1 Cu5 . . 119.5(3) ?
O1 N1 Cu5 . . 124.1(3) ?
C2 N2 Cu5 . . 109.8(3) ?
C2 N2 H2A . . 109.7 ?
Cu5 N2 H2A . . 109.7 ?
C2 N2 H2B . . 109.7 ?
Cu5 N2 H2B . . 109.7 ?
H2A N2 H2B . . 108.2 ?
C3 N3 O3 . . 115.1(4) ?
C3 N3 Cu1 . . 117.5(3) ?
O3 N3 Cu1 . . 125.5(3) ?
C4 N4 Cu1 . . 110.6(3) ?
C4 N4 H4A . . 109.5 ?
Cu1 N4 H4A . . 109.5 ?
C4 N4 H4B . . 109.5 ?
Cu1 N4 H4B . . 109.5 ?
H4A N4 H4B . . 108.1 ?
C5 N5 O5 . . 115.7(4) ?
C5 N5 Cu2 . . 118.6(3) ?
O5 N5 Cu2 . . 125.5(3) ?
C6 N6 Cu2 . . 109.6(3) ?
C6 N6 H6A . . 109.7 ?
Cu2 N6 H6A . . 109.7 ?
C6 N6 H6B . . 109.7 ?
Cu2 N6 H6B . . 109.7 ?
H6A N6 H6B . . 108.2 ?
C7 N7 O7 . . 116.2(4) ?
C7 N7 Cu3 . . 119.0(3) ?
O7 N7 Cu3 . . 124.6(3) ?
C8 N8 Cu3 . . 109.7(3) ?
C8 N8 H8A . . 109.7 ?
Cu3 N8 H8A . . 109.7 ?
C8 N8 H8B . . 109.7 ?
Cu3 N8 H8B . . 109.7 ?
H8A N8 H8B . . 108.2 ?
C9 N9 O9 . . 116.1(4) ?
C9 N9 Cu4 . . 119.1(3) ?
O9 N9 Cu4 . . 124.1(3) ?
C10 N10 Cu4 . . 109.9(3) ?
C10 N10 H10A . . 109.7 ?
Cu4 N10 H10A . . 109.7 ?
C10 N10 H10B . . 109.7 ?
Cu4 N10 H10B . . 109.7 ?
H10A N10 H10B . . 108.2 ?
N1 O1 Cu1 . . 106.2(2) ?
N1 O1 Tb1 . . 125.6(2) ?
Cu1 O1 Tb1 . . 126.24(14) ?
C1 O2 Cu1 . . 104.0(3) ?
N3 O3 Cu2 . . 108.6(2) ?
N3 O3 Tb1 . . 122.4(2) ?
Cu2 O3 Tb1 . . 128.77(15) ?
C3 O4 Cu2 . . 107.7(3) ?
N5 O5 Cu3 . . 107.1(2) ?
N5 O5 Tb1 . . 124.1(2) ?
Cu3 O5 Tb1 . . 123.88(13) ?
C5 O6 Cu3 . . 107.0(3) ?
N7 O7 Cu4 . . 107.2(2) ?
N7 O7 Tb1 . . 124.7(2) ?
Cu4 O7 Tb1 . . 125.89(14) ?
C7 O8 Cu4 . . 106.9(3) ?
N9 O9 Cu5 . . 107.2(2) ?
N9 O9 Tb1 . . 126.2(2) ?
Cu5 O9 Tb1 . . 126.55(14) ?
C9 O10 Cu5 . . 107.4(3) ?
S1 O11 Tb1 . . 99.41(17) ?
S1 O12 Tb1 . . 100.02(16) ?
Tb1 O15 H15A . . 121(4) ?
Tb1 O15 H15B . . 118(4) ?
H15A O15 H15B . . 107(6) ?
Cu3 O16 H16A . . 122(5) ?
Cu3 O16 H16B . . 114(5) ?
H16A O16 H16B . . 102(7) ?
Cu4 O17 H17A . . 92(5) ?
Cu4 O17 H17B . . 111(5) ?
H17A O17 H17B . . 103(6) ?
Cu5 O18 H18A . . 120(5) ?
Cu5 O18 H18B . . 115(5) ?
H18A O18 H18B . . 107(7) ?
Cu2 O19 H19A . . 99(10) ?
Cu2 O19 H19B . . 113(10) ?
H19A O19 H19B . . 135(10) ?
Cu1 O20 H20A . . 131(5) ?
Cu1 O20 H20B . . 95(5) ?
H20A O20 H20B . . 93(7) ?
Cu1 O21 H21A . . 124(5) ?
Cu1 O21 H21B . . 110(5) ?
H21A O21 H21B . . 101(7) ?
H22A O22 H22B . . 113(8) ?
H23A O23 H23B . . 105(3) ?
H24A O24 H24B . . 108(3) ?
O14 S1 O13 . . 110.9(2) ?
O14 S1 O11 . . 111.0(2) ?
O13 S1 O11 . . 111.6(2) ?
O14 S1 O12 . . 110.1(2) ?
O13 S1 O12 . . 110.3(2) ?
O11 S1 O12 . . 102.68(19) ?
O14 S1 Tb1 . . 118.92(16) ?
O13 S1 Tb1 . . 130.15(15) ?
O11 S1 Tb1 . . 51.82(13) ?
O12 S1 Tb1 . . 51.24(13) ?
O26 S2 O26 2_556 . 180.0 ?
O26 S2 O28 2_556 2_556 114.8(5) ?
O26 S2 O28 . 2_556 65.2(5) ?
O26 S2 O28 2_556 . 65.2(5) ?
O26 S2 O28 . . 114.8(5) ?
O28 S2 O28 2_556 . 180.0(5) ?
O26 S2 O27 2_556 . 68.7(5) ?
O26 S2 O27 . . 111.3(5) ?
O28 S2 O27 2_556 . 70.8(5) ?
O28 S2 O27 . . 109.2(5) ?
O26 S2 O25 2_556 . 69.6(5) ?
O26 S2 O25 . . 110.4(5) ?
O28 S2 O25 2_556 . 73.6(5) ?
O28 S2 O25 . . 106.4(5) ?
O27 S2 O25 . . 104.2(5) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N1 . 1.294(6) ?
C1 O2 . 1.298(5) ?
C1 C2 . 1.509(6) ?
C2 N2 . 1.480(6) ?
C2 H2C . 0.9900 ?
C2 H2D . 0.9900 ?
C3 N3 . 1.301(5) ?
C3 O4 . 1.304(6) ?
C3 C4 . 1.488(7) ?
C4 N4 . 1.488(6) ?
C4 H4C . 0.9900 ?
C4 H4D . 0.9900 ?
C5 N5 . 1.295(6) ?
C5 O6 . 1.298(6) ?
C5 C6 . 1.509(6) ?
C6 N6 . 1.491(6) ?
C6 H6C . 0.9900 ?
C6 H6D . 0.9900 ?
C7 N7 . 1.288(6) ?
C7 O8 . 1.298(5) ?
C7 C8 . 1.509(6) ?
C8 N8 . 1.489(5) ?
C8 H8C . 0.9900 ?
C8 H8D . 0.9900 ?
C9 O10 . 1.282(6) ?
C9 N9 . 1.306(6) ?
C9 C10 . 1.498(6) ?
C10 N10 . 1.487(7) ?
C10 H10C . 0.9900 ?
C10 H10D . 0.9900 ?
Cu1 N3 . 1.915(4) yes
Cu1 O1 . 1.928(3) yes
Cu1 O2 . 1.969(3) yes
Cu1 N4 . 1.991(4) yes
Cu1 O20 . 2.601(4) yes
Cu1 O21 . 2.736(4) yes
Cu2 N5 . 1.900(4) yes
Cu2 O3 . 1.928(3) yes
Cu2 O4 . 1.936(3) yes
Cu2 N6 . 2.018(4) yes
Cu2 O19 . 2.409(10) yes
Cu3 N7 . 1.904(4) yes
Cu3 O6 . 1.944(3) yes
Cu3 O5 . 1.949(3) yes
Cu3 N8 . 2.014(4) yes
Cu3 O16 . 2.508(4) yes
Cu4 N9 . 1.894(4) yes
Cu4 O8 . 1.940(3) yes
Cu4 O7 . 1.947(3) yes
Cu4 N10 . 2.012(4) yes
Cu4 O17 . 2.481(4) yes
Cu5 N1 . 1.890(4) yes
Cu5 O9 . 1.943(3) yes
Cu5 O10 . 1.946(3) yes
Cu5 N2 . 2.003(4) yes
Cu5 O18 . 2.379(4) yes
Tb1 O9 . 2.370(3) yes
Tb1 O1 . 2.372(3) yes
Tb1 O15 . 2.383(3) yes
Tb1 O3 . 2.386(3) yes
Tb1 O7 . 2.411(3) yes
Tb1 O5 . 2.430(3) yes
Tb1 O12 . 2.436(3) yes
Tb1 O11 . 2.451(3) yes
Tb1 S1 . 3.0756(11) ?
N1 O1 . 1.396(5) ?
N2 H2A . 0.9100 ?
N2 H2B . 0.9100 ?
N3 O3 . 1.389(5) ?
N4 H4A . 0.9100 ?
N4 H4B . 0.9100 ?
N5 O5 . 1.395(4) ?
N6 H6A . 0.9100 ?
N6 H6B . 0.9100 ?
N7 O7 . 1.388(5) ?
N8 H8A . 0.9100 ?
N8 H8B . 0.9100 ?
N9 O9 . 1.391(5) ?
N10 H10A . 0.9100 ?
N10 H10B . 0.9100 ?
O11 S1 . 1.500(4) ?
O12 S1 . 1.502(3) ?
O13 S1 . 1.461(3) ?
O14 S1 . 1.448(4) ?
O15 H15A . 0.84(2) ?
O15 H15B . 0.84(2) ?
O16 H16A . 0.84(2) ?
O16 H16B . 0.84(2) ?
O17 H17A . 0.83(2) ?
O17 H17B . 0.83(2) ?
O18 H18A . 0.84(2) ?
O18 H18B . 0.83(2) ?
O19 H19A . 0.84(2) ?
O19 H19B . 0.84(2) ?
O20 H20A . 0.83(2) ?
O20 H20B . 0.83(2) ?
O21 H21A . 0.84(2) ?
O21 H21B . 0.83(2) ?
O22 H22A . 0.84(2) ?
O22 H22B . 0.84(2) ?
O23 H23A . 0.84(2) ?
O23 H23B . 0.85(2) ?
O24 H24A . 0.84(2) ?
O24 H24B . 0.84(2) ?
O25 S2 . 1.519(7) ?
O26 S2 . 1.401(8) ?
O27 S2 . 1.485(7) ?
O28 S2 . 1.458(8) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O24 H24B O8 . 0.84(2) 2.01(3) 2.807(5) 159(7) yes
O24 H24A O11 1_565 0.84(2) 2.21(3) 3.015(5) 162(7) yes
O23 H23B O13 1_665 0.85(2) 2.02(3) 2.853(5) 166(6) yes
O23 H23A O4 1_565 0.84(2) 1.89(2) 2.734(5) 176(7) yes
O22 H22B O23 . 0.84(2) 1.89(3) 2.701(6) 162(8) yes
O22 H22A O26 2_666 0.84(2) 2.18(4) 2.968(9) 155(8) yes
O22 H22A O28 1_665 0.84(2) 1.92(3) 2.733(9) 161(8) yes
O21 H21B O10 2_666 0.83(2) 1.91(3) 2.728(5) 165(8) yes
O21 H21A O18 1_655 0.84(2) 1.94(3) 2.765(5) 167(7) yes
O20 H20B O11 . 0.83(2) 2.14(3) 2.960(5) 168(7) yes
O20 H20A O26 2_556 0.83(2) 2.09(3) 2.916(9) 170(7) yes
O20 H20A O25 . 0.83(2) 2.02(5) 2.719(9) 142(7) yes
O19 H19B O24 2_665 0.84(2) 2.07(9) 2.866(11) 16E1(2) yes
O19 H19A O24 1_545 0.84(2) 1.72(7) 2.535(12) 16E1(2) yes
O18 H18B O14 . 0.83(2) 1.90(2) 2.732(5) 173(7) yes
O18 H18A O26 2_556 0.84(2) 2.04(3) 2.857(9) 163(7) yes
O18 H18A O27 . 0.84(2) 1.91(4) 2.648(9) 146(6) yes
O17 H17B O6 2_665 0.83(2) 1.90(2) 2.730(5) 176(7) yes
O17 H17A O12 . 0.83(2) 2.10(3) 2.905(5) 163(6) yes
O16 H16B O22 . 0.84(2) 1.89(2) 2.721(6) 173(7) yes
O16 H16A O17 1_655 0.84(2) 1.95(2) 2.784(5) 172(7) yes
O15 H15B O16 . 0.84(2) 1.86(2) 2.692(5) 170(6) yes
O15 H15A O21 . 0.84(2) 1.85(3) 2.668(5) 166(6) yes
N10 H10B O22 1_455 0.91 2.13 2.920(6) 144.5 yes
N10 H10A O20 1_565 0.91 2.24 2.987(5) 139.3 yes
N8 H8B O12 2_665 0.91 2.04 2.937(5) 168.1 yes
N8 H8A O23 . 0.91 2.20 3.031(5) 151.8 yes
N6 H6B O13 2_655 0.91 2.64 3.363(5) 136.8 yes
N6 H6B O24 2_665 0.91 2.24 2.984(6) 139.1 yes
N6 H6A O13 1_655 0.91 2.25 3.158(5) 174.6 yes
N4 H4B O2 2_656 0.91 2.33 3.182(5) 156.3 yes
N4 H4A O27 1_655 0.91 2.18 3.037(9) 155.8 yes
N4 H4A O25 2_656 0.91 2.01 2.789(9) 142.8 yes
N2 H2B O27 . 0.91 2.55 3.418(9) 158.5 yes
N2 H2B O28 2_556 0.91 2.08 2.868(9) 144.3 yes
N2 H2A O15 2_666 0.91 2.07 2.946(5) 162.0 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C1 C2 N2 . . . . 18.5(6) ?
O2 C1 C2 N2 . . . . -161.5(4) ?
N3 C3 C4 N4 . . . . -9.9(6) ?
O4 C3 C4 N4 . . . . 168.5(4) ?
N5 C5 C6 N6 . . . . 5.8(6) ?
O6 C5 C6 N6 . . . . -176.2(4) ?
N7 C7 C8 N8 . . . . -10.1(5) ?
O8 C7 C8 N8 . . . . 170.5(4) ?
O10 C9 C10 N10 . . . . 168.9(4) ?
N9 C9 C10 N10 . . . . -10.9(6) ?
O2 C1 N1 O1 . . . . -0.6(6) ?
C2 C1 N1 O1 . . . . 179.4(4) ?
O2 C1 N1 Cu5 . . . . 171.2(3) ?
C2 C1 N1 Cu5 . . . . -8.8(5) ?
O9 Cu5 N1 C1 . . . . 175.3(4) ?
O10 Cu5 N1 C1 . . . . 105.8(6) ?
N2 Cu5 N1 C1 . . . . -2.1(4) ?
O18 Cu5 N1 C1 . . . . -91.7(4) ?
O9 Cu5 N1 O1 . . . . -13.6(3) ?
O10 Cu5 N1 O1 . . . . -83.1(6) ?
N2 Cu5 N1 O1 . . . . 169.0(3) ?
O18 Cu5 N1 O1 . . . . 79.4(3) ?
C1 C2 N2 Cu5 . . . . -19.1(5) ?
O4 C3 N3 O3 . . . . -1.0(6) ?
C4 C3 N3 O3 . . . . 177.4(4) ?
O4 C3 N3 Cu1 . . . . -166.2(3) ?
C4 C3 N3 Cu1 . . . . 12.2(5) ?
C3 C4 N4 Cu1 . . . . 3.3(5) ?
O6 C5 N5 O5 . . . . 0.7(6) ?
C6 C5 N5 O5 . . . . 178.6(4) ?
O6 C5 N5 Cu2 . . . . -173.6(3) ?
C6 C5 N5 Cu2 . . . . 4.4(5) ?
O3 Cu2 N5 C5 . . . . 165.2(4) ?
N6 Cu2 N5 C5 . . . . -9.4(3) ?
O19 Cu2 N5 C5 . . . . -97.4(4) ?
O3 Cu2 N5 O5 . . . . -8.4(3) ?
N6 Cu2 N5 O5 . . . . 177.0(3) ?
O19 Cu2 N5 O5 . . . . 88.9(4) ?
C5 C6 N6 Cu2 . . . . -12.1(5) ?
O8 C7 N7 O7 . . . . 0.3(6) ?
C8 C7 N7 O7 . . . . -179.1(4) ?
O8 C7 N7 Cu3 . . . . 175.5(3) ?
C8 C7 N7 Cu3 . . . . -3.9(5) ?
C7 C8 N8 Cu3 . . . . 18.0(4) ?
O10 C9 N9 O9 . . . . -2.5(6) ?
C10 C9 N9 O9 . . . . 177.3(4) ?
O10 C9 N9 Cu4 . . . . -173.1(3) ?
C10 C9 N9 Cu4 . . . . 6.7(5) ?
O7 Cu4 N9 C9 . . . . 167.0(4) ?
N10 Cu4 N9 C9 . . . . -0.7(4) ?
O17 Cu4 N9 C9 . . . . -95.5(3) ?
O7 Cu4 N9 O9 . . . . -2.8(3) ?
N10 Cu4 N9 O9 . . . . -170.5(3) ?
O17 Cu4 N9 O9 . . . . 94.8(3) ?
C9 C10 N10 Cu4 . . . . 9.8(5) ?
C1 N1 O1 Cu1 . . . . 11.7(4) ?
Cu5 N1 O1 Cu1 . . . . -159.6(2) ?
C1 N1 O1 Tb1 . . . . 176.5(3) ?
Cu5 N1 O1 Tb1 . . . . 5.2(5) ?
N1 C1 O2 Cu1 . . . . -10.6(5) ?
C2 C1 O2 Cu1 . . . . 169.4(3) ?
C3 N3 O3 Cu2 . . . . -5.7(4) ?
Cu1 N3 O3 Cu2 . . . . 158.1(2) ?
C3 N3 O3 Tb1 . . . . 179.5(3) ?
Cu1 N3 O3 Tb1 . . . . -16.7(5) ?
N3 C3 O4 Cu2 . . . . 7.1(5) ?
C4 C3 O4 Cu2 . . . . -171.2(4) ?
C5 N5 O5 Cu3 . . . . -9.7(4) ?
Cu2 N5 O5 Cu3 . . . . 164.1(2) ?
C5 N5 O5 Tb1 . . . . -165.6(3) ?
Cu2 N5 O5 Tb1 . . . . 8.2(4) ?
N5 C5 O6 Cu3 . . . . 8.8(5) ?
C6 C5 O6 Cu3 . . . . -169.1(3) ?
C7 N7 O7 Cu4 . . . . 3.2(4) ?
Cu3 N7 O7 Cu4 . . . . -171.6(2) ?
C7 N7 O7 Tb1 . . . . 167.2(3) ?
Cu3 N7 O7 Tb1 . . . . -7.7(5) ?
N7 C7 O8 Cu4 . . . . -3.7(5) ?
C8 C7 O8 Cu4 . . . . 175.7(3) ?
C9 N9 O9 Cu5 . . . . -0.7(4) ?
Cu4 N9 O9 Cu5 . . . . 169.3(2) ?
C9 N9 O9 Tb1 . . . . 177.4(3) ?
Cu4 N9 O9 Tb1 . . . . -12.5(5) ?
N9 C9 O10 Cu5 . . . . 4.2(5) ?
C10 C9 O10 Cu5 . . . . -175.6(4) ?
Tb1 O11 S1 O14 . . . . -110.9(2) ?
Tb1 O11 S1 O13 . . . . 124.81(18) ?
Tb1 O11 S1 O12 . . . . 6.7(2) ?
Tb1 O12 S1 O14 . . . . 111.5(2) ?
Tb1 O12 S1 O13 . . . . -125.78(18) ?
Tb1 O12 S1 O11 . . . . -6.7(2) ?

_cod_database_fobs_code 2243985
