#------------------------------------------------------------------------------
#$Date: 2022-10-05 00:56:31 +0300 (Wed, 05 Oct 2022) $
#$Revision: 278335 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/07/7130795.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_7130795
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 Sm'
_chemical_formula_sum            'C15 H14 N3 O4 S3 Sm'
_chemical_formula_weight         546.82
_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             2021-10-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-14 deposited with the CCDC.	2022-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.919(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0701(15)
_cell_length_b                   9.9650(14)
_cell_length_c                   19.421(3)
_cell_measurement_reflns_used    9037
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.94
_cell_measurement_theta_min      2.30
_cell_volume                     1941.7(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0582
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            88915
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.004
_diffrn_reflns_theta_min         2.299
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.372
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1110 before and 0.0707 after correction.
The Ratio of minimum to maximum transmission is 0.8466.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull gray'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.487
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0296
_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)+(0.0300P)²+3.5211P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4446
_reflns_number_total             5167
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc03352f2.cif
_cod_data_source_block           a_CCDC1
_cod_database_code               7130795
_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   0.635
_shelx_estimated_absorpt_t_min   0.291
_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), C14(H14), C12(H12), C2(H2), C5(H5), C13(H13), C10(H10), C3(H3),
 C4(H4), C7(H7), C9(H9), 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
Sm1 Sm 0.65541(2) 0.58615(2) 0.44846(2) 0.02500(6) Uani 1 1 d . . . . .
S1 S 0.92336(9) 0.59445(9) 0.40172(5) 0.0378(2) Uani 1 1 d . . . . .
S3 S 0.41366(10) 0.60920(11) 0.35181(5) 0.0423(2) Uani 1 1 d . . . . .
S2 S 0.62529(13) 0.86646(11) 0.42245(7) 0.0583(3) Uani 1 1 d . . . . .
O3 O 0.4877(2) 0.4063(2) 0.45446(11) 0.0268(4) Uani 1 1 d . . . . .
O4 O 0.7701(3) 0.4249(3) 0.52502(14) 0.0418(6) Uani 1 1 d . . . . .
H4A H 0.725588 0.411954 0.559676 0.063 Uiso 1 1 d R U . . .
H4B H 0.843358 0.458364 0.542064 0.063 Uiso 1 1 d R U . . .
O2 O 0.7824(3) 0.7152(3) 0.52764(13) 0.0399(6) Uani 1 1 d . . . . .
N3 N 0.4440(2) 0.3536(3) 0.39209(13) 0.0292(6) Uani 1 1 d . . . . .
N1 N 0.7944(3) 0.4118(3) 0.32391(16) 0.0397(7) Uani 1 1 d . . . . .
O1 O 0.6888(3) 0.4522(4) 0.35421(16) 0.0621(10) Uani 1 1 d . . . . .
N2 N 0.8068(3) 0.8457(3) 0.5295(2) 0.0482(8) Uani 1 1 d . . . . .
C15 C 0.4458(4) 0.2190(4) 0.3863(2) 0.0433(9) Uani 1 1 d . . . . .
H15 H 0.474256 0.166253 0.424203 0.052 Uiso 1 1 calc R U . . .
C14 C 0.4055(5) 0.1601(5) 0.3242(3) 0.0617(14) Uani 1 1 d . . . . .
H14 H 0.406442 0.067233 0.319560 0.074 Uiso 1 1 calc R U . . .
C11 C 0.4061(3) 0.4387(4) 0.33960(17) 0.0364(8) Uani 1 1 d . . . . .
C1 C 0.9144(3) 0.4694(4) 0.34156(17) 0.0318(7) Uani 1 1 d . . . . .
C12 C 0.3635(4) 0.3764(6) 0.2763(2) 0.0526(11) Uani 1 1 d . . . . .
H12 H 0.334443 0.429388 0.238600 0.063 Uiso 1 1 calc R U . . .
C6 C 0.7402(5) 0.9292(4) 0.4837(3) 0.0605(13) Uani 1 1 d . . . . .
C2 C 1.0223(4) 0.4201(4) 0.3074(2) 0.0470(10) Uani 1 1 d . . . . .
H2 H 1.107255 0.454290 0.318945 0.056 Uiso 1 1 calc R U . . .
C5 C 0.7765(4) 0.3153(5) 0.2749(2) 0.0584(13) Uani 1 1 d . . . . .
H5 H 0.691838 0.280093 0.263853 0.070 Uiso 1 1 calc R U . . .
C13 C 0.3638(4) 0.2398(6) 0.2691(2) 0.0638(14) Uani 1 1 d . . . . .
H13 H 0.335620 0.201036 0.226805 0.077 Uiso 1 1 calc R U . . .
C10 C 0.8995(6) 0.8884(6) 0.5791(3) 0.0763(17) Uani 1 1 d . . . . .
H10 H 0.942075 0.827095 0.609637 0.092 Uiso 1 1 calc R U . . .
C3 C 1.0050(4) 0.3235(5) 0.2579(3) 0.0583(12) Uani 1 1 d . . . . .
H3 H 1.077108 0.293918 0.235171 0.070 Uiso 1 1 calc R U . . .
C4 C 0.8802(4) 0.2697(5) 0.2417(3) 0.0640(14) Uani 1 1 d . . . . .
H4 H 0.867530 0.202816 0.208348 0.077 Uiso 1 1 calc R U . . .
C7 C 0.7729(7) 1.0661(5) 0.4904(5) 0.112(3) Uani 1 1 d . . . . .
H7 H 0.730765 1.128411 0.460292 0.134 Uiso 1 1 calc R U . . .
C9 C 0.9302(8) 1.0198(8) 0.5843(5) 0.130(4) Uani 1 1 d . . . . .
H9 H 0.995393 1.049075 0.617816 0.156 Uiso 1 1 calc R U . . .
C8 C 0.8668(8) 1.1081(7) 0.5413(6) 0.145(5) Uani 1 1 d . . . . .
H8 H 0.886609 1.199010 0.545873 0.174 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 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'
Sm Sm -0.1638 3.4418 '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 Sm1 S3 122.24(3) . . ?
S2 Sm1 S1 90.25(3) . . ?
S2 Sm1 S3 75.03(3) . . ?
O3 Sm1 S1 148.33(5) 3_666 . ?
O3 Sm1 S1 133.50(5) . . ?
O3 Sm1 S3 88.84(5) 3_666 . ?
O3 Sm1 S3 63.70(5) . . ?
O3 Sm1 S2 92.60(6) 3_666 . ?
O3 Sm1 S2 130.99(6) . . ?
O3 Sm1 O3 62.64(8) 3_666 . ?
O4 Sm1 S1 78.71(7) . . ?
O4 Sm1 S3 140.16(7) . . ?
O4 Sm1 S2 143.06(7) . . ?
O4 Sm1 O3 80.21(8) . 3_666 ?
O4 Sm1 O3 77.37(8) . . ?
O2 Sm1 S1 73.57(7) . . ?
O2 Sm1 S3 139.50(7) . . ?
O2 Sm1 S2 67.42(7) . . ?
O2 Sm1 O3 135.64(8) . . ?
O2 Sm1 O3 78.49(8) . 3_666 ?
O2 Sm1 O4 75.64(9) . . ?
O2 Sm1 O1 137.72(9) . . ?
O1 Sm1 S1 64.52(7) . . ?
O1 Sm1 S3 73.12(8) . . ?
O1 Sm1 S2 116.48(11) . . ?
O1 Sm1 O3 139.04(9) . 3_666 ?
O1 Sm1 O3 76.41(9) . . ?
O1 Sm1 O4 90.50(12) . . ?
C1 S1 Sm1 101.32(11) . . ?
C11 S3 Sm1 92.01(11) . . ?
C6 S2 Sm1 100.37(16) . . ?
Sm1 O3 Sm1 117.36(8) 3_666 . ?
N3 O3 Sm1 121.79(16) . 3_666 ?
N3 O3 Sm1 114.12(17) . . ?
Sm1 O4 H4A 109.3 . . ?
Sm1 O4 H4B 109.3 . . ?
H4A O4 H4B 104.5 . . ?
N2 O2 Sm1 131.1(2) . . ?
C15 N3 O3 117.0(3) . . ?
C15 N3 C11 124.4(3) . . ?
C11 N3 O3 118.5(3) . . ?
O1 N1 C1 119.5(3) . . ?
O1 N1 C5 117.7(3) . . ?
C5 N1 C1 122.7(3) . . ?
N1 O1 Sm1 134.8(2) . . ?
O2 N2 C6 120.4(3) . . ?
O2 N2 C10 116.4(4) . . ?
C10 N2 C6 123.3(4) . . ?
N3 C15 H15 120.2 . . ?
N3 C15 C14 119.7(4) . . ?
C14 C15 H15 120.2 . . ?
C15 C14 H14 120.4 . . ?
C13 C14 C15 119.1(5) . . ?
C13 C14 H14 120.4 . . ?
N3 C11 S3 120.6(2) . . ?
N3 C11 C12 115.1(4) . . ?
C12 C11 S3 124.2(3) . . ?
N1 C1 S1 118.4(3) . . ?
N1 C1 C2 116.1(3) . . ?
C2 C1 S1 125.4(3) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 C11 121.6(4) . . ?
C13 C12 H12 119.2 . . ?
N2 C6 S2 120.1(3) . . ?
N2 C6 C7 115.9(5) . . ?
C7 C6 S2 124.0(5) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 C1 121.4(4) . . ?
C3 C2 H2 119.3 . . ?
N1 C5 H5 119.6 . . ?
C4 C5 N1 120.8(4) . . ?
C4 C5 H5 119.6 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0(4) . . ?
C12 C13 H13 120.0 . . ?
N2 C10 H10 120.0 . . ?
C9 C10 N2 120.0(7) . . ?
C9 C10 H10 120.0 . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.8(4) . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 119.1(4) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C6 C7 H7 119.9 . . ?
C8 C7 C6 120.2(7) . . ?
C8 C7 H7 119.9 . . ?
C10 C9 H9 120.1 . . ?
C8 C9 C10 119.9(7) . . ?
C8 C9 H9 120.1 . . ?
C7 C8 H8 119.6 . . ?
C9 C8 C7 120.8(6) . . ?
C9 C8 H8 119.6 . . ?
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
Sm1 S1 2.9209(9) . ?
Sm1 S3 2.9527(10) . ?
Sm1 S2 2.8502(12) . ?
Sm1 O3 2.470(2) 3_666 ?
Sm1 O3 2.472(2) . ?
Sm1 O4 2.415(2) . ?
Sm1 O2 2.306(2) . ?
Sm1 O1 2.313(3) . ?
S1 C1 1.705(4) . ?
S3 C11 1.717(4) . ?
S2 C6 1.706(6) . ?
O3 N3 1.359(3) . ?
O4 H4A 0.8501 . ?
O4 H4B 0.8501 . ?
O2 N2 1.324(4) . ?
N3 C15 1.346(5) . ?
N3 C11 1.355(5) . ?
N1 O1 1.322(4) . ?
N1 C1 1.355(4) . ?
N1 C5 1.355(5) . ?
N2 C6 1.353(7) . ?
N2 C10 1.351(6) . ?
C15 H15 0.9300 . ?
C15 C14 1.371(6) . ?
C14 H14 0.9300 . ?
C14 C13 1.369(8) . ?
C11 C12 1.410(5) . ?
C1 C2 1.409(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.368(7) . ?
C6 C7 1.407(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.361(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.352(6) . ?
C13 H13 0.9300 . ?
C10 H10 0.9300 . ?
C10 C9 1.347(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.377(6) . ?
C4 H4 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.373(11) . ?
C9 H9 0.9300 . ?
C9 C8 1.338(13) . ?
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
Sm1 S1 C1 N1 7.7(3) . . . . ?
Sm1 S1 C1 C2 -172.9(3) . . . . ?
Sm1 S3 C11 N3 34.6(3) . . . . ?
Sm1 S3 C11 C12 -144.5(3) . . . . ?
Sm1 S2 C6 N2 -4.3(4) . . . . ?
Sm1 S2 C6 C7 175.4(5) . . . . ?
Sm1 O3 N3 C15 129.6(3) . . . . ?
Sm1 O3 N3 C15 -79.9(3) 3_666 . . . ?
Sm1 O3 N3 C11 102.3(3) 3_666 . . . ?
Sm1 O3 N3 C11 -48.2(3) . . . . ?
Sm1 O2 N2 C6 8.2(5) . . . . ?
Sm1 O2 N2 C10 -172.1(3) . . . . ?
S1 C1 C2 C3 -177.3(4) . . . . ?
S3 C11 C12 C13 177.8(3) . . . . ?
S2 C6 C7 C8 -180.0(7) . . . . ?
O3 N3 C15 C14 -178.7(3) . . . . ?
O3 N3 C11 S3 0.1(4) . . . . ?
O3 N3 C11 C12 179.3(3) . . . . ?
O2 N2 C6 S2 -0.6(6) . . . . ?
O2 N2 C6 C7 179.6(5) . . . . ?
O2 N2 C10 C9 179.8(6) . . . . ?
N3 C15 C14 C13 -0.1(6) . . . . ?
N3 C11 C12 C13 -1.4(5) . . . . ?
N1 C1 C2 C3 2.2(6) . . . . ?
N1 C5 C4 C3 -0.6(9) . . . . ?
O1 N1 C1 S1 -1.0(5) . . . . ?
O1 N1 C1 C2 179.5(4) . . . . ?
O1 N1 C5 C4 179.8(5) . . . . ?
N2 C6 C7 C8 -0.2(11) . . . . ?
N2 C10 C9 C8 1.4(13) . . . . ?
C15 N3 C11 S3 -177.5(3) . . . . ?
C15 N3 C11 C12 1.7(5) . . . . ?
C15 C14 C13 C12 0.4(7) . . . . ?
C11 N3 C15 C14 -1.0(5) . . . . ?
C11 C12 C13 C14 0.4(7) . . . . ?
C1 N1 O1 Sm1 -11.3(6) . . . . ?
C1 N1 C5 C4 1.3(8) . . . . ?
C1 C2 C3 C4 -1.6(8) . . . . ?
C6 N2 C10 C9 -0.5(9) . . . . ?
C6 C7 C8 C9 1.2(15) . . . . ?
C2 C3 C4 C5 0.8(9) . . . . ?
C5 N1 O1 Sm1 170.1(4) . . . . ?
C5 N1 C1 S1 177.5(4) . . . . ?
C5 N1 C1 C2 -2.0(6) . . . . ?
C10 N2 C6 S2 179.6(4) . . . . ?
C10 N2 C6 C7 -0.1(8) . . . . ?
C10 C9 C8 C7 -1.7(15) . . . . ?
