#------------------------------------------------------------------------------
#$Date: 2022-10-05 00:56:31 +0300 (Wed, 05 Oct 2022) $
#$Revision: 278335 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/07/7130798.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_7130798
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 Pr S3'
_chemical_formula_sum            'C15 H14 N3 O4 Pr S3'
_chemical_formula_weight         537.38
_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             2021-10-25
_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                 95.0440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1531(2)
_cell_length_b                   10.0034(2)
_cell_length_c                   19.5478(5)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      33.39
_cell_measurement_theta_min      2.77
_cell_volume                     1977.69(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0640
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            107132
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.240
_diffrn_reflns_theta_min         2.014
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.804
_exptl_absorpt_correction_T_max  0.7473
_exptl_absorpt_correction_T_min  0.5662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1298 before and 0.0702 after correction.
The Ratio of minimum to maximum transmission is 0.7577.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.193
_refine_diff_density_max         0.810
_refine_diff_density_min         -1.237
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         10213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0189P)²+2.0480P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7641
_reflns_number_total             10213
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc03352f2.cif
_cod_data_source_block           a_CCDC3
_cod_database_code               7130798
_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   0.614
_shelx_estimated_absorpt_t_min   0.386
_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), C5(H5), C14(H14), C2(H2), C12(H12), C4(H4), C3(H3), C13(H13),
 C10(H10), 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
Pr1 Pr 0.34325(2) 0.58724(2) 0.55192(2) 0.02774(3) Uani 1 1 d . . . . .
S1 S 0.07456(6) 0.59113(7) 0.59970(4) 0.04249(14) Uani 1 1 d . . . . .
S3 S 0.58648(7) 0.60672(8) 0.65012(3) 0.04700(15) Uani 1 1 d . . . . .
S2 S 0.37340(9) 0.87083(8) 0.57961(6) 0.0681(2) Uani 1 1 d . . . . .
O3 O 0.51317(14) 0.40505(15) 0.54645(7) 0.0300(3) Uani 1 1 d . . . . .
O4 O 0.22833(18) 0.42835(19) 0.47065(11) 0.0483(4) Uani 1 1 d . . . . .
H4A H 0.269567 0.422886 0.434724 0.073 Uiso 1 1 d R U . . .
H4B H 0.152987 0.459942 0.456541 0.073 Uiso 1 1 d R U . . .
O2 O 0.21740(19) 0.72314(19) 0.47363(9) 0.0483(4) Uani 1 1 d . . . . .
N3 N 0.55689(17) 0.3522(2) 0.60832(9) 0.0323(4) Uani 1 1 d . . . . .
O1 O 0.30841(18) 0.4486(3) 0.64592(12) 0.0694(7) Uani 1 1 d . . . . .
N1 N 0.20324(19) 0.4075(2) 0.67600(11) 0.0439(5) Uani 1 1 d . . . . .
N2 N 0.1934(3) 0.8532(3) 0.47215(15) 0.0588(7) Uani 1 1 d . . . . .
C15 C 0.5554(3) 0.2181(3) 0.61349(15) 0.0472(6) Uani 1 1 d . . . . .
H15 H 0.527049 0.166267 0.575510 0.057 Uiso 1 1 calc R U . . .
C1 C 0.0839(2) 0.4652(2) 0.65896(12) 0.0347(4) Uani 1 1 d . . . . .
C11 C 0.5943(2) 0.4363(3) 0.66114(11) 0.0395(5) Uani 1 1 d . . . . .
C5 C 0.2219(3) 0.3109(4) 0.72418(17) 0.0651(10) Uani 1 1 d . . . . .
H5 H 0.305930 0.275156 0.734368 0.078 Uiso 1 1 calc R U . . .
C14 C 0.5957(3) 0.1578(4) 0.67484(19) 0.0662(10) Uani 1 1 d . . . . .
H14 H 0.594993 0.065216 0.678966 0.079 Uiso 1 1 calc R U . . .
C2 C -0.0212(3) 0.4159(3) 0.69265(17) 0.0546(7) Uani 1 1 d . . . . .
H2 H -0.105296 0.450828 0.681622 0.065 Uiso 1 1 calc R U . . .
C12 C 0.6361(3) 0.3730(4) 0.72368(13) 0.0574(8) Uani 1 1 d . . . . .
H12 H 0.663817 0.425218 0.761591 0.069 Uiso 1 1 calc R U . . .
C4 C 0.1199(3) 0.2657(4) 0.75777(18) 0.0703(10) Uani 1 1 d . . . . .
H4 H 0.133583 0.200327 0.791454 0.084 Uiso 1 1 calc R U . . .
C3 C -0.0049(3) 0.3178(4) 0.74145(19) 0.0676(10) Uani 1 1 d . . . . .
H3 H -0.076640 0.286723 0.763281 0.081 Uiso 1 1 calc R U . . .
C13 C 0.6372(3) 0.2371(4) 0.73023(17) 0.0711(11) Uani 1 1 d . . . . .
H13 H 0.665856 0.198040 0.772082 0.085 Uiso 1 1 calc R U . . .
C6 C 0.2593(3) 0.9347(3) 0.5188(2) 0.0706(11) Uani 1 1 d . . . . .
C10 C 0.1021(4) 0.8964(5) 0.4219(3) 0.0955(16) Uani 1 1 d . . . . .
H10 H 0.060705 0.836682 0.390551 0.115 Uiso 1 1 calc R U . . .
C7 C 0.2270(5) 1.0712(4) 0.5129(4) 0.138(3) Uani 1 1 d . . . . .
H7 H 0.269560 1.132055 0.543275 0.165 Uiso 1 1 calc R U . . .
C9 C 0.0728(6) 1.0297(7) 0.4187(5) 0.159(3) Uani 1 1 d . . . . .
H9 H 0.009639 1.061347 0.385295 0.191 Uiso 1 1 calc R U . . .
C8 C 0.1349(6) 1.1155(5) 0.4638(5) 0.181(4) Uani 1 1 d . . . . .
H8 H 0.114415 1.206102 0.461235 0.217 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'
Pr Pr -0.2180 2.8214 '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'
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 Pr1 S3 121.82(2) . . ?
S2 Pr1 S1 90.76(2) . . ?
S2 Pr1 S3 75.48(2) . . ?
O3 Pr1 S1 148.56(3) 3_666 . ?
O3 Pr1 S1 132.58(4) . . ?
O3 Pr1 S3 89.27(4) 3_666 . ?
O3 Pr1 S3 62.96(4) . . ?
O3 Pr1 S2 93.09(4) 3_666 . ?
O3 Pr1 S2 130.89(4) . . ?
O3 Pr1 O3 62.89(5) 3_666 . ?
O4 Pr1 S1 79.33(5) . . ?
O4 Pr1 S3 140.41(5) . . ?
O4 Pr1 S2 141.90(5) . . ?
O4 Pr1 O3 78.49(6) . 3_666 ?
O4 Pr1 O3 78.08(6) . . ?
O2 Pr1 S1 74.54(5) . . ?
O2 Pr1 S3 138.80(5) . . ?
O2 Pr1 S2 66.19(5) . . ?
O2 Pr1 O3 136.82(6) . . ?
O2 Pr1 O3 78.58(6) . 3_666 ?
O2 Pr1 O4 75.71(7) . . ?
O2 Pr1 O1 137.89(7) . . ?
O1 Pr1 S1 63.61(4) . . ?
O1 Pr1 S3 73.16(6) . . ?
O1 Pr1 S2 116.84(8) . . ?
O1 Pr1 O3 138.78(6) . 3_666 ?
O1 Pr1 O3 75.95(6) . . ?
O1 Pr1 O4 91.60(9) . . ?
C1 S1 Pr1 101.92(7) . . ?
C11 S3 Pr1 92.42(8) . . ?
C6 S2 Pr1 100.48(12) . . ?
Pr1 O3 Pr1 117.11(5) 3_666 . ?
N3 O3 Pr1 121.80(11) . 3_666 ?
N3 O3 Pr1 114.53(11) . . ?
Pr1 O4 H4A 109.5 . . ?
Pr1 O4 H4B 109.3 . . ?
H4A O4 H4B 104.5 . . ?
N2 O2 Pr1 132.39(18) . . ?
O3 N3 C11 118.90(19) . . ?
C15 N3 O3 116.7(2) . . ?
C15 N3 C11 124.3(2) . . ?
N1 O1 Pr1 135.20(14) . . ?
O1 N1 C1 119.65(19) . . ?
O1 N1 C5 117.4(2) . . ?
C5 N1 C1 122.9(2) . . ?
O2 N2 C6 119.8(2) . . ?
O2 N2 C10 116.1(4) . . ?
C6 N2 C10 124.0(3) . . ?
N3 C15 H15 120.0 . . ?
N3 C15 C14 119.9(3) . . ?
C14 C15 H15 120.0 . . ?
N1 C1 S1 118.38(17) . . ?
N1 C1 C2 116.0(2) . . ?
C2 C1 S1 125.63(19) . . ?
N3 C11 S3 120.75(16) . . ?
N3 C11 C12 115.1(3) . . ?
C12 C11 S3 124.2(2) . . ?
N1 C5 H5 119.6 . . ?
N1 C5 C4 120.7(3) . . ?
C4 C5 H5 119.6 . . ?
C15 C14 H14 120.6 . . ?
C15 C14 C13 118.8(3) . . ?
C13 C14 H14 120.6 . . ?
C1 C2 H2 118.9 . . ?
C3 C2 C1 122.2(3) . . ?
C3 C2 H2 118.9 . . ?
C11 C12 H12 119.0 . . ?
C13 C12 C11 121.9(3) . . ?
C13 C12 H12 119.0 . . ?
C5 C4 H4 120.4 . . ?
C5 C4 C3 119.2(3) . . ?
C3 C4 H4 120.4 . . ?
C2 C3 C4 119.0(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0(3) . . ?
C12 C13 H13 120.0 . . ?
N2 C6 S2 120.5(2) . . ?
N2 C6 C7 115.5(4) . . ?
C7 C6 S2 124.0(4) . . ?
N2 C10 H10 120.8 . . ?
N2 C10 C9 118.3(6) . . ?
C9 C10 H10 120.8 . . ?
C6 C7 H7 119.4 . . ?
C8 C7 C6 121.2(6) . . ?
C8 C7 H7 119.4 . . ?
C10 C9 H9 119.9 . . ?
C8 C9 C10 120.3(5) . . ?
C8 C9 H9 119.9 . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.6(5) . . ?
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
Pr1 S1 2.9604(6) . ?
Pr1 S3 2.9979(6) . ?
Pr1 S2 2.8993(8) . ?
Pr1 O3 2.5143(15) 3_666 ?
Pr1 O3 2.5183(14) . ?
Pr1 O4 2.4669(18) . ?
Pr1 O2 2.3407(16) . ?
Pr1 O1 2.3538(18) . ?
S1 C1 1.708(2) . ?
S3 C11 1.719(3) . ?
S2 C6 1.710(4) . ?
O3 N3 1.358(2) . ?
O4 H4A 0.8505 . ?
O4 H4B 0.8509 . ?
O2 N2 1.324(3) . ?
N3 C15 1.346(3) . ?
N3 C11 1.360(3) . ?
O1 N1 1.329(3) . ?
N1 C1 1.357(3) . ?
N1 C5 1.351(3) . ?
N2 C6 1.355(5) . ?
N2 C10 1.360(5) . ?
C15 H15 0.9300 . ?
C15 C14 1.372(4) . ?
C1 C2 1.393(3) . ?
C11 C12 1.409(3) . ?
C5 H5 0.9300 . ?
C5 C4 1.352(4) . ?
C14 H14 0.9300 . ?
C14 C13 1.378(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.368(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.365(5) . ?
C4 H4 0.9300 . ?
C4 C3 1.381(4) . ?
C3 H3 0.9300 . ?
C13 H13 0.9300 . ?
C6 C7 1.407(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.367(7) . ?
C7 H7 0.9300 . ?
C7 C8 1.354(9) . ?
C9 H9 0.9300 . ?
C9 C8 1.347(11) . ?
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
Pr1 S1 C1 N1 7.2(2) . . . . ?
Pr1 S1 C1 C2 -173.4(2) . . . . ?
Pr1 S3 C11 N3 34.52(18) . . . . ?
Pr1 S3 C11 C12 -144.3(2) . . . . ?
Pr1 S2 C6 N2 -4.7(3) . . . . ?
Pr1 S2 C6 C7 175.4(4) . . . . ?
Pr1 O3 N3 C15 129.73(17) . . . . ?
Pr1 O3 N3 C15 -79.5(2) 3_666 . . . ?
Pr1 O3 N3 C11 -47.9(2) . . . . ?
Pr1 O3 N3 C11 102.82(18) 3_666 . . . ?
Pr1 O2 N2 C6 7.8(4) . . . . ?
Pr1 O2 N2 C10 -172.7(3) . . . . ?
Pr1 O1 N1 C1 -10.9(4) . . . . ?
Pr1 O1 N1 C5 170.8(3) . . . . ?
S1 C1 C2 C3 -177.6(3) . . . . ?
S3 C11 C12 C13 178.2(2) . . . . ?
S2 C6 C7 C8 -179.6(6) . . . . ?
O3 N3 C15 C14 -178.7(2) . . . . ?
O3 N3 C11 S3 0.1(3) . . . . ?
O3 N3 C11 C12 178.96(19) . . . . ?
O2 N2 C6 S2 0.0(4) . . . . ?
O2 N2 C6 C7 179.9(4) . . . . ?
O2 N2 C10 C9 179.3(5) . . . . ?
N3 C15 C14 C13 0.0(4) . . . . ?
N3 C11 C12 C13 -0.7(4) . . . . ?
O1 N1 C1 S1 -0.9(4) . . . . ?
O1 N1 C1 C2 179.7(3) . . . . ?
O1 N1 C5 C4 178.9(4) . . . . ?
N1 C1 C2 C3 1.8(5) . . . . ?
N1 C5 C4 C3 1.1(7) . . . . ?
N2 C6 C7 C8 0.5(9) . . . . ?
N2 C10 C9 C8 1.0(10) . . . . ?
C15 N3 C11 S3 -177.39(18) . . . . ?
C15 N3 C11 C12 1.5(3) . . . . ?
C15 C14 C13 C12 0.8(5) . . . . ?
C1 N1 C5 C4 0.7(6) . . . . ?
C1 C2 C3 C4 -0.1(6) . . . . ?
C11 N3 C15 C14 -1.2(4) . . . . ?
C11 C12 C13 C14 -0.4(5) . . . . ?
C5 N1 C1 S1 177.3(3) . . . . ?
C5 N1 C1 C2 -2.1(4) . . . . ?
C5 C4 C3 C2 -1.3(7) . . . . ?
C6 N2 C10 C9 -1.2(7) . . . . ?
C6 C7 C8 C9 -0.7(12) . . . . ?
C10 N2 C6 S2 -179.5(3) . . . . ?
C10 N2 C6 C7 0.4(6) . . . . ?
C10 C9 C8 C7 -0.1(13) . . . . ?
