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#$Date: 2022-10-05 00:56:31 +0300 (Wed, 05 Oct 2022) $
#$Revision: 278335 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/08/7130800.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_7130800
loop_
_publ_author_name
'Huffman, Zachary K.'
'Sperling, Joseph M.'
'Windorff, Cory J.'
'Long, Brian N.'
'Cordova, Lucas'
'Ramanantoanina, Harry'
'Celis-Barros, Cristian'
'Albrecht-Schönzart, Thomas E.'
_publ_section_title
;
 Synthesis and characterization of a bimetallic americium(iii)
 pyrithionate coordination complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03352F
_journal_year                    2022
_chemical_formula_moiety         'C15 H14 N3 O4 S3 Tb'
_chemical_formula_sum            'C15 H14 N3 O4 S3 Tb'
_chemical_formula_weight         555.39
_chemical_name_systematic        '[Tb(mpo)2(mu-O-mpo)(H2O)]2'
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2022-06-14 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.797(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.061(3)
_cell_length_b                   9.949(3)
_cell_length_c                   19.421(5)
_cell_measurement_reflns_used    9346
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.80
_cell_volume                     1937.2(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            101200
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.587
_diffrn_reflns_theta_min         2.801
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.999
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0847 before and 0.0518 after correction.
The Ratio of minimum to maximum transmission is 0.7682.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.203
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0183
_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)+(0.0167P)²+2.4056P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0442
_refine_ls_wR_factor_ref         0.0452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4286
_reflns_number_total             4455
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc03352f2.cif
_cod_data_source_block           b_CCDC3
_cod_original_cell_volume        1937.2(9)
_cod_database_code               7130800
_shelx_shelxl_version_number     2018/3
_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   0.497
_shelx_estimated_absorpt_t_min   0.283
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C2(H2), C12(H12), C14(H14), C3(H3), C5(H5), C13(H13), C4(H4),
 C10(H10), C7(H7), C8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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_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 0.65421(2) 0.41479(2) 0.44894(2) 0.02429(4) Uani 1 1 d . . . . .
S1 S 0.92180(6) 0.40250(7) 0.40304(4) 0.03744(14) Uani 1 1 d . . . . .
S3 S 0.41390(7) 0.38857(8) 0.35342(3) 0.04085(15) Uani 1 1 d . . . . .
S2 S 0.62372(8) 0.13734(8) 0.42336(5) 0.05365(19) Uani 1 1 d . . . . .
O3 O 0.48867(16) 0.59344(16) 0.45516(8) 0.0272(3) Uani 1 1 d . . . . .
O4 O 0.76841(18) 0.57717(18) 0.52187(10) 0.0392(4) Uani 1 1 d . . . . .
H4A H 0.844862 0.545901 0.539698 0.059 Uiso 1 1 d R U . . .
H4B H 0.724732 0.592811 0.558048 0.059 Uiso 1 1 d R U . . .
O2 O 0.78091(18) 0.29089(18) 0.52873(9) 0.0378(4) Uani 1 1 d . . . . .
N3 N 0.44441(18) 0.6458(2) 0.39264(10) 0.0289(4) Uani 1 1 d . . . . .
O1 O 0.68622(18) 0.5442(3) 0.35456(12) 0.0590(7) Uani 1 1 d . . . . .
N1 N 0.7930(2) 0.5844(2) 0.32418(11) 0.0372(5) Uani 1 1 d . . . . .
N2 N 0.8069(2) 0.1596(2) 0.53061(13) 0.0435(5) Uani 1 1 d . . . . .
C15 C 0.4472(3) 0.7807(3) 0.38628(15) 0.0421(6) Uani 1 1 d . . . . .
H15 H 0.476635 0.833879 0.423885 0.050 Uiso 1 1 calc R U . . .
C1 C 0.9132(2) 0.5262(2) 0.34202(12) 0.0302(5) Uani 1 1 d . . . . .
C2 C 1.0217(3) 0.5751(3) 0.30721(16) 0.0454(7) Uani 1 1 d . . . . .
H2 H 1.106402 0.539804 0.318259 0.054 Uiso 1 1 calc R U . . .
C11 C 0.4055(2) 0.5598(3) 0.33994(12) 0.0342(5) Uani 1 1 d . . . . .
C12 C 0.3633(3) 0.6214(4) 0.27653(14) 0.0501(8) Uani 1 1 d . . . . .
H12 H 0.334377 0.567745 0.239020 0.060 Uiso 1 1 calc R U . . .
C14 C 0.4062(3) 0.8396(4) 0.32368(19) 0.0597(9) Uani 1 1 d . . . . .
H14 H 0.407209 0.932526 0.318701 0.072 Uiso 1 1 calc R U . . .
C3 C 1.0048(3) 0.6730(4) 0.25767(18) 0.0553(8) Uani 1 1 d . . . . .
H3 H 1.077311 0.703702 0.235437 0.066 Uiso 1 1 calc R U . . .
C5 C 0.7751(3) 0.6811(4) 0.27500(17) 0.0538(8) Uani 1 1 d . . . . .
H5 H 0.690534 0.717171 0.264479 0.065 Uiso 1 1 calc R U . . .
C6 C 0.7403(3) 0.0749(3) 0.4849(2) 0.0545(8) Uani 1 1 d . . . . .
C13 C 0.3635(3) 0.7582(4) 0.26862(17) 0.0617(10) Uani 1 1 d . . . . .
H13 H 0.335052 0.796237 0.226195 0.074 Uiso 1 1 calc R U . . .
C4 C 0.8790(3) 0.7259(4) 0.24096(18) 0.0592(9) Uani 1 1 d . . . . .
H4 H 0.865839 0.791330 0.206858 0.071 Uiso 1 1 calc R U . . .
C10 C 0.9005(4) 0.1182(4) 0.5804(2) 0.0702(11) Uani 1 1 d . . . . .
H10 H 0.943407 0.180225 0.610462 0.084 Uiso 1 1 calc R U . . .
C7 C 0.7724(4) -0.0619(4) 0.4930(3) 0.0964(18) Uani 1 1 d . . . . .
H7 H 0.728277 -0.124844 0.464037 0.116 Uiso 1 1 calc R U . . .
C9 C 0.9313(6) -0.0152(6) 0.5862(4) 0.116(2) Uani 1 1 d . . . . .
C8 C 0.8673(5) -0.1042(5) 0.5428(4) 0.127(3) Uani 1 1 d . . . . .
H8 H 0.887824 -0.195201 0.546799 0.152 Uiso 1 1 calc R U . . .
H9 H 1.006(6) -0.034(7) 0.616(3) 0.14(2) Uiso 1 1 d . . . . .
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'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
S1 Tb1 S3 122.52(3) . . ?
S2 Tb1 S1 89.70(2) . . ?
S2 Tb1 S3 74.30(2) . . ?
O3 Tb1 S1 134.22(4) . . ?
O3 Tb1 S1 148.16(4) 3_666 . ?
O3 Tb1 S3 64.35(4) . . ?
O3 Tb1 S3 88.44(4) 3_666 . ?
O3 Tb1 S2 131.02(4) . . ?
O3 Tb1 S2 92.25(4) 3_666 . ?
O3 Tb1 O3 62.67(6) . 3_666 ?
O4 Tb1 S1 78.33(5) . . ?
O4 Tb1 S3 140.18(5) . . ?
O4 Tb1 S2 144.12(5) . . ?
O4 Tb1 O3 76.95(6) . . ?
O4 Tb1 O3 81.66(6) . 3_666 ?
O2 Tb1 S1 72.95(5) . . ?
O2 Tb1 S3 139.90(5) . . ?
O2 Tb1 S2 68.72(5) . . ?
O2 Tb1 O3 78.21(6) . 3_666 ?
O2 Tb1 O3 134.63(6) . . ?
O2 Tb1 O4 75.42(7) . . ?
O2 Tb1 O1 137.77(7) . . ?
O1 Tb1 S1 65.27(5) . . ?
O1 Tb1 S3 72.95(6) . . ?
O1 Tb1 S2 115.55(8) . . ?
O1 Tb1 O3 76.85(7) . . ?
O1 Tb1 O3 139.51(7) . 3_666 ?
O1 Tb1 O4 90.09(9) . . ?
C1 S1 Tb1 100.84(8) . . ?
C11 S3 Tb1 92.02(8) . . ?
C6 S2 Tb1 99.99(11) . . ?
Tb1 O3 Tb1 117.33(6) . 3_666 ?
N3 O3 Tb1 114.03(12) . . ?
N3 O3 Tb1 121.49(12) . 3_666 ?
Tb1 O4 H4A 111.1 . . ?
Tb1 O4 H4B 110.5 . . ?
H4A O4 H4B 103.3 . . ?
N2 O2 Tb1 130.18(16) . . ?
O3 N3 C11 118.7(2) . . ?
C15 N3 O3 117.1(2) . . ?
C15 N3 C11 124.2(2) . . ?
N1 O1 Tb1 134.31(15) . . ?
O1 N1 C1 119.6(2) . . ?
O1 N1 C5 117.4(2) . . ?
C5 N1 C1 123.0(2) . . ?
O2 N2 C6 120.3(2) . . ?
O2 N2 C10 116.1(3) . . ?
C10 N2 C6 123.6(3) . . ?
N3 C15 H15 120.1 . . ?
N3 C15 C14 119.7(3) . . ?
C14 C15 H15 120.1 . . ?
N1 C1 S1 118.48(18) . . ?
N1 C1 C2 115.9(2) . . ?
C2 C1 S1 125.64(19) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 C1 121.6(3) . . ?
C3 C2 H2 119.2 . . ?
N3 C11 S3 119.86(18) . . ?
N3 C11 C12 115.4(3) . . ?
C12 C11 S3 124.7(2) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 C11 121.8(3) . . ?
C13 C12 H12 119.1 . . ?
C15 C14 H14 120.5 . . ?
C13 C14 C15 118.9(3) . . ?
C13 C14 H14 120.5 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.5(3) . . ?
C4 C3 H3 120.2 . . ?
N1 C5 H5 119.6 . . ?
N1 C5 C4 120.8(3) . . ?
C4 C5 H5 119.6 . . ?
N2 C6 S2 120.0(2) . . ?
N2 C6 C7 115.5(4) . . ?
C7 C6 S2 124.4(3) . . ?
C12 C13 C14 120.0(3) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.1(3) . . ?
C5 C4 H4 120.4 . . ?
N2 C10 H10 120.2 . . ?
N2 C10 C9 119.5(5) . . ?
C9 C10 H10 120.2 . . ?
C6 C7 H7 119.4 . . ?
C8 C7 C6 121.2(5) . . ?
C8 C7 H7 119.4 . . ?
C10 C9 H9 115(4) . . ?
C8 C9 C10 119.6(5) . . ?
C8 C9 H9 125(4) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.5(4) . . ?
C9 C8 H8 119.7 . . ?
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 S1 2.9083(9) . ?
Tb1 S3 2.9334(9) . ?
Tb1 S2 2.8169(10) . ?
Tb1 O3 2.4457(16) . ?
Tb1 O3 2.4473(16) 3_666 ?
Tb1 O4 2.3799(18) . ?
Tb1 O2 2.2836(17) . ?
Tb1 O1 2.285(2) . ?
S1 C1 1.706(2) . ?
S3 C11 1.725(3) . ?
S2 C6 1.719(4) . ?
O3 N3 1.361(2) . ?
O4 H4A 0.8739 . ?
O4 H4B 0.8733 . ?
O2 N2 1.332(3) . ?
N3 C15 1.348(3) . ?
N3 C11 1.366(3) . ?
O1 N1 1.330(3) . ?
N1 C1 1.359(3) . ?
N1 C5 1.357(3) . ?
N2 C6 1.359(4) . ?
N2 C10 1.357(4) . ?
C15 H15 0.9300 . ?
C15 C14 1.381(4) . ?
C1 C2 1.417(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.370(4) . ?
C11 C12 1.409(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.369(5) . ?
C14 H14 0.9300 . ?
C14 C13 1.381(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.384(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.358(4) . ?
C6 C7 1.405(4) . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C10 H10 0.9300 . ?
C10 C9 1.366(6) . ?
C7 H7 0.9300 . ?
C7 C8 1.367(7) . ?
C9 C8 1.348(9) . ?
C9 H9 0.93(6) . ?
C8 H8 0.9300 . ?
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
Tb1 S1 C1 N1 -7.4(2) . . . . ?
Tb1 S1 C1 C2 172.7(2) . . . . ?
Tb1 S3 C11 N3 -34.26(18) . . . . ?
Tb1 S3 C11 C12 144.2(2) . . . . ?
Tb1 S2 C6 N2 4.5(3) . . . . ?
Tb1 S2 C6 C7 -176.6(4) . . . . ?
Tb1 O3 N3 C15 -129.21(18) . . . . ?
Tb1 O3 N3 C15 81.2(2) 3_666 . . . ?
Tb1 O3 N3 C11 48.1(2) . . . . ?
Tb1 O3 N3 C11 -101.47(19) 3_666 . . . ?
Tb1 O2 N2 C6 -9.2(4) . . . . ?
Tb1 O2 N2 C10 171.6(2) . . . . ?
Tb1 O1 N1 C1 12.6(4) . . . . ?
Tb1 O1 N1 C5 -168.8(3) . . . . ?
S1 C1 C2 C3 178.5(3) . . . . ?
S3 C11 C12 C13 -177.6(2) . . . . ?
S2 C6 C7 C8 179.4(5) . . . . ?
O3 N3 C15 C14 178.7(2) . . . . ?
O3 N3 C11 S3 -0.3(3) . . . . ?
O3 N3 C11 C12 -178.91(19) . . . . ?
O2 N2 C6 S2 1.0(4) . . . . ?
O2 N2 C6 C7 -177.9(3) . . . . ?
O2 N2 C10 C9 179.2(4) . . . . ?
N3 C15 C14 C13 -0.3(4) . . . . ?
N3 C11 C12 C13 1.0(4) . . . . ?
O1 N1 C1 S1 0.2(4) . . . . ?
O1 N1 C1 C2 -179.9(3) . . . . ?
O1 N1 C5 C4 -179.0(3) . . . . ?
N1 C1 C2 C3 -1.3(4) . . . . ?
N1 C5 C4 C3 -0.9(6) . . . . ?
N2 C6 C7 C8 -1.7(7) . . . . ?
N2 C10 C9 C8 -0.8(9) . . . . ?
C15 N3 C11 S3 176.88(19) . . . . ?
C15 N3 C11 C12 -1.8(3) . . . . ?
C15 C14 C13 C12 -0.4(5) . . . . ?
C1 N1 C5 C4 -0.5(5) . . . . ?
C1 C2 C3 C4 0.0(6) . . . . ?
C2 C3 C4 C5 1.1(6) . . . . ?
C11 N3 C15 C14 1.5(4) . . . . ?
C11 C12 C13 C14 0.0(5) . . . . ?
C5 N1 C1 S1 -178.3(3) . . . . ?
C5 N1 C1 C2 1.6(4) . . . . ?
C6 N2 C10 C9 -0.1(6) . . . . ?
C6 C7 C8 C9 1.0(10) . . . . ?
C10 N2 C6 S2 -179.8(3) . . . . ?
C10 N2 C6 C7 1.3(5) . . . . ?
C10 C9 C8 C7 0.3(11) . . . . ?
