#------------------------------------------------------------------------------
#$Date: 2022-10-05 00:56:31 +0300 (Wed, 05 Oct 2022) $
#$Revision: 278335 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/07/7130797.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_7130797
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 Nd O4 S3'
_chemical_formula_sum            'C15 H14 N3 Nd O4 S3'
_chemical_formula_weight         540.71
_chemical_name_systematic        '[Nd(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                 95.0050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1252(2)
_cell_length_b                   9.9839(2)
_cell_length_c                   19.5248(5)
_cell_measurement_reflns_used    9572
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      40.35
_cell_measurement_theta_min      2.78
_cell_volume                     1966.22(7)
_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 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  0.0411
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            112293
_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         41.127
_diffrn_reflns_theta_min         2.019
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.984
_exptl_absorpt_correction_T_max  0.7481
_exptl_absorpt_correction_T_min  0.5886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0852 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.7868.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.158
_refine_diff_density_max         1.453
_refine_diff_density_min         -2.036
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         13041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0225P)²+2.0145P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11293
_reflns_number_total             13041
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc03352f2.cif
_cod_data_source_block           a_CCDC2
_cod_database_code               7130797
_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   0.650
_shelx_estimated_absorpt_t_min   0.492
_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), C3(H3), C13(H13), C4(H4),
 C10(H10), C9(H9), 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
Nd1 Nd 0.34362(2) 0.58683(2) 0.55187(2) 0.02561(3) Uani 1 1 d . . . . .
S1 S 0.07521(5) 0.59163(6) 0.59902(3) 0.03981(12) Uani 1 1 d . . . . .
S3 S 0.58607(6) 0.60762(7) 0.64940(3) 0.04415(13) Uani 1 1 d . . . . .
S2 S 0.37359(10) 0.86898(8) 0.57941(6) 0.0643(2) Uani 1 1 d . . . . .
O3 O 0.51279(14) 0.40538(14) 0.54601(7) 0.0279(2) Uani 1 1 d . . . . .
O4 O 0.22893(17) 0.42795(19) 0.47185(11) 0.0452(4) Uani 1 1 d . . . . .
H4A H 0.274132 0.416329 0.437502 0.068 Uiso 1 1 d R U . . .
H4B H 0.156502 0.462542 0.454678 0.068 Uiso 1 1 d R U . . .
O2 O 0.21693(19) 0.72074(19) 0.47326(9) 0.0452(4) Uani 1 1 d . . . . .
N3 N 0.55652(15) 0.35269(19) 0.60776(8) 0.0303(3) Uani 1 1 d . . . . .
O1 O 0.30934(17) 0.4494(3) 0.64602(12) 0.0674(8) Uani 1 1 d . . . . .
N1 N 0.20427(18) 0.4089(2) 0.67608(11) 0.0417(5) Uani 1 1 d . . . . .
N2 N 0.1932(2) 0.8511(3) 0.47195(15) 0.0549(6) Uani 1 1 d . . . . .
C15 C 0.5547(3) 0.2179(3) 0.61308(15) 0.0449(5) Uani 1 1 d . . . . .
H15 H 0.525850 0.165631 0.575258 0.054 Uiso 1 1 calc R U . . .
C1 C 0.08435(18) 0.4662(2) 0.65877(11) 0.0326(4) Uani 1 1 d . . . . .
C11 C 0.59408(19) 0.4371(3) 0.66090(10) 0.0367(4) Uani 1 1 d . . . . .
C14 C 0.5958(3) 0.1582(4) 0.67506(19) 0.0633(10) Uani 1 1 d . . . . .
H14 H 0.595565 0.065450 0.679386 0.076 Uiso 1 1 calc R U . . .
C12 C 0.6362(3) 0.3735(4) 0.72345(12) 0.0557(8) Uani 1 1 d . . . . .
H12 H 0.664391 0.425923 0.761315 0.067 Uiso 1 1 calc R U . . .
C2 C -0.0219(2) 0.4173(3) 0.69278(17) 0.0510(7) Uani 1 1 d . . . . .
H2 H -0.106151 0.452427 0.681868 0.061 Uiso 1 1 calc R U . . .
C5 C 0.2227(3) 0.3123(4) 0.72459(17) 0.0613(9) Uani 1 1 d . . . . .
H5 H 0.306896 0.276502 0.734924 0.074 Uiso 1 1 calc R U . . .
C3 C -0.0047(3) 0.3191(4) 0.74173(19) 0.0633(9) Uani 1 1 d . . . . .
H3 H -0.076664 0.287893 0.763612 0.076 Uiso 1 1 calc R U . . .
C13 C 0.6371(3) 0.2375(4) 0.73022(16) 0.0672(11) Uani 1 1 d . . . . .
H13 H 0.665617 0.198601 0.772193 0.081 Uiso 1 1 calc R U . . .
C4 C 0.1201(3) 0.2669(4) 0.75831(19) 0.0670(10) Uani 1 1 d . . . . .
H4 H 0.133657 0.201578 0.792135 0.080 Uiso 1 1 calc R U . . .
C6 C 0.2594(3) 0.9331(3) 0.5187(3) 0.0676(11) Uani 1 1 d . . . . .
C10 C 0.1022(5) 0.8947(5) 0.4217(3) 0.0920(16) Uani 1 1 d . . . . .
H10 H 0.061164 0.834941 0.390117 0.110 Uiso 1 1 calc R U . . .
C9 C 0.0719(6) 1.0279(7) 0.4184(5) 0.155(4) Uani 1 1 d . . . . .
H9 H 0.007805 1.059042 0.385205 0.186 Uiso 1 1 calc R U . . .
C7 C 0.2271(5) 1.0697(4) 0.5126(5) 0.132(3) Uani 1 1 d . . . . .
H7 H 0.269482 1.130978 0.542942 0.159 Uiso 1 1 calc R U . . .
C8 C 0.1342(6) 1.1137(5) 0.4628(6) 0.172(5) Uani 1 1 d . . . . .
H8 H 0.114108 1.204449 0.459614 0.206 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'
Nd Nd -0.1943 3.0179 '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'
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 Nd1 S3 122.025(19) . . ?
S2 Nd1 S1 90.62(2) . . ?
S2 Nd1 S3 75.22(2) . . ?
O3 Nd1 S1 148.44(3) 3_666 . ?
O3 Nd1 S1 132.85(4) . . ?
O3 Nd1 S3 89.13(3) 3_666 . ?
O3 Nd1 S3 63.30(3) . . ?
O3 Nd1 S2 93.06(4) 3_666 . ?
O3 Nd1 S2 130.95(4) . . ?
O3 Nd1 O3 62.73(5) 3_666 . ?
O4 Nd1 S1 79.09(5) . . ?
O4 Nd1 S3 140.51(5) . . ?
O4 Nd1 S2 142.18(5) . . ?
O4 Nd1 O3 78.90(6) . 3_666 ?
O4 Nd1 O3 77.89(5) . . ?
O2 Nd1 S1 74.15(5) . . ?
O2 Nd1 S3 139.06(6) . . ?
O2 Nd1 S2 66.74(6) . . ?
O2 Nd1 O3 136.38(5) . . ?
O2 Nd1 O3 78.61(6) . 3_666 ?
O2 Nd1 O4 75.43(7) . . ?
O2 Nd1 O1 137.79(7) . . ?
O1 Nd1 S1 63.93(4) . . ?
O1 Nd1 S3 73.13(6) . . ?
O1 Nd1 S2 116.54(8) . . ?
O1 Nd1 O3 138.86(6) . 3_666 ?
O1 Nd1 O3 76.16(6) . . ?
O1 Nd1 O4 91.53(9) . . ?
C1 S1 Nd1 101.83(7) . . ?
C11 S3 Nd1 92.37(7) . . ?
C6 S2 Nd1 100.58(12) . . ?
Nd1 O3 Nd1 117.27(5) 3_666 . ?
N3 O3 Nd1 121.72(10) . 3_666 ?
N3 O3 Nd1 114.36(10) . . ?
Nd1 O4 H4A 109.5 . . ?
Nd1 O4 H4B 109.4 . . ?
H4A O4 H4B 104.4 . . ?
N2 O2 Nd1 131.65(19) . . ?
O3 N3 C11 119.00(18) . . ?
C15 N3 O3 116.7(2) . . ?
C15 N3 C11 124.2(2) . . ?
N1 O1 Nd1 134.99(14) . . ?
O1 N1 C1 119.81(18) . . ?
O1 N1 C5 117.47(19) . . ?
C5 N1 C1 122.7(2) . . ?
O2 N2 C6 120.1(2) . . ?
O2 N2 C10 116.1(4) . . ?
C10 N2 C6 123.7(3) . . ?
N3 C15 H15 120.2 . . ?
N3 C15 C14 119.5(3) . . ?
C14 C15 H15 120.2 . . ?
N1 C1 S1 118.22(15) . . ?
N1 C1 C2 116.2(2) . . ?
C2 C1 S1 125.54(17) . . ?
N3 C11 S3 120.38(15) . . ?
N3 C11 C12 115.1(3) . . ?
C12 C11 S3 124.5(2) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 C15 119.1(3) . . ?
C13 C14 H14 120.4 . . ?
C11 C12 H12 118.9 . . ?
C13 C12 C11 122.1(3) . . ?
C13 C12 H12 118.9 . . ?
C1 C2 H2 119.2 . . ?
C3 C2 C1 121.6(2) . . ?
C3 C2 H2 119.2 . . ?
N1 C5 H5 119.6 . . ?
N1 C5 C4 120.9(2) . . ?
C4 C5 H5 119.6 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.5(3) . . ?
C4 C3 H3 120.3 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0(2) . . ?
C12 C13 H13 120.0 . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
N2 C6 S2 120.3(2) . . ?
N2 C6 C7 115.5(4) . . ?
C7 C6 S2 124.2(4) . . ?
N2 C10 H10 120.6 . . ?
N2 C10 C9 118.9(6) . . ?
C9 C10 H10 120.6 . . ?
C10 C9 H9 119.9 . . ?
C8 C9 C10 120.1(6) . . ?
C8 C9 H9 119.9 . . ?
C6 C7 H7 119.6 . . ?
C8 C7 C6 120.9(6) . . ?
C8 C7 H7 119.6 . . ?
C9 C8 C7 120.9(5) . . ?
C9 C8 H8 119.6 . . ?
C7 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
Nd1 S1 2.9450(5) . ?
Nd1 S3 2.9800(6) . ?
Nd1 S2 2.8790(8) . ?
Nd1 O3 2.5013(13) 3_666 ?
Nd1 O3 2.5026(13) . ?
Nd1 O4 2.4472(18) . ?
Nd1 O2 2.3335(16) . ?
Nd1 O1 2.3441(18) . ?
S1 C1 1.708(2) . ?
S3 C11 1.718(3) . ?
S2 C6 1.707(4) . ?
O3 N3 1.3540(19) . ?
O4 H4A 0.8522 . ?
O4 H4B 0.8525 . ?
O2 N2 1.323(3) . ?
N3 C15 1.350(3) . ?
N3 C11 1.365(3) . ?
O1 N1 1.322(2) . ?
N1 C1 1.358(3) . ?
N1 C5 1.353(3) . ?
N2 C6 1.359(5) . ?
N2 C10 1.358(5) . ?
C15 H15 0.9300 . ?
C15 C14 1.380(4) . ?
C1 C2 1.400(3) . ?
C11 C12 1.409(3) . ?
C14 H14 0.9300 . ?
C14 C13 1.372(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.364(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.370(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.355(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.379(4) . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C6 C7 1.405(4) . ?
C10 H10 0.9300 . ?
C10 C9 1.365(7) . ?
C9 H9 0.9300 . ?
C9 C8 1.336(12) . ?
C7 H7 0.9300 . ?
C7 C8 1.365(10) . ?
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
Nd1 S1 C1 N1 7.3(2) . . . . ?
Nd1 S1 C1 C2 -173.6(2) . . . . ?
Nd1 S3 C11 N3 34.64(16) . . . . ?
Nd1 S3 C11 C12 -144.42(19) . . . . ?
Nd1 S2 C6 N2 -4.7(3) . . . . ?
Nd1 S2 C6 C7 175.6(5) . . . . ?
Nd1 O3 N3 C15 129.57(16) . . . . ?
Nd1 O3 N3 C15 -79.9(2) 3_666 . . . ?
Nd1 O3 N3 C11 102.79(16) 3_666 . . . ?
Nd1 O3 N3 C11 -47.79(19) . . . . ?
Nd1 O2 N2 C6 7.6(4) . . . . ?
Nd1 O2 N2 C10 -173.1(3) . . . . ?
Nd1 O1 N1 C1 -10.7(5) . . . . ?
Nd1 O1 N1 C5 170.7(3) . . . . ?
S1 C1 C2 C3 -177.8(3) . . . . ?
S3 C11 C12 C13 178.1(2) . . . . ?
S2 C6 C7 C8 -179.8(6) . . . . ?
O3 N3 C15 C14 -178.9(2) . . . . ?
O3 N3 C11 S3 -0.1(2) . . . . ?
O3 N3 C11 C12 179.07(17) . . . . ?
O2 N2 C6 S2 0.1(4) . . . . ?
O2 N2 C6 C7 179.8(4) . . . . ?
O2 N2 C10 C9 179.0(5) . . . . ?
N3 C15 C14 C13 0.4(4) . . . . ?
N3 C11 C12 C13 -1.0(4) . . . . ?
O1 N1 C1 S1 -1.0(4) . . . . ?
O1 N1 C1 C2 179.8(3) . . . . ?
O1 N1 C5 C4 179.1(4) . . . . ?
N1 C1 C2 C3 1.3(5) . . . . ?
N1 C5 C4 C3 1.1(7) . . . . ?
N2 C6 C7 C8 0.5(9) . . . . ?
N2 C10 C9 C8 2.0(11) . . . . ?
C15 N3 C11 S3 -177.23(17) . . . . ?
C15 N3 C11 C12 1.9(3) . . . . ?
C15 C14 C13 C12 0.4(5) . . . . ?
C1 N1 C5 C4 0.5(6) . . . . ?
C1 C2 C3 C4 0.2(6) . . . . ?
C11 N3 C15 C14 -1.7(4) . . . . ?
C11 C12 C13 C14 -0.1(4) . . . . ?
C2 C3 C4 C5 -1.4(7) . . . . ?
C5 N1 C1 S1 177.6(3) . . . . ?
C5 N1 C1 C2 -1.6(4) . . . . ?
C6 N2 C10 C9 -1.7(7) . . . . ?
C6 C7 C8 C9 -0.1(13) . . . . ?
C10 N2 C6 S2 -179.2(3) . . . . ?
C10 N2 C6 C7 0.5(6) . . . . ?
C10 C9 C8 C7 -1.1(13) . . . . ?
