#------------------------------------------------------------------------------
#$Date: 2022-10-05 00:56:31 +0300 (Wed, 05 Oct 2022) $
#$Revision: 278335 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/07/7130793.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_7130793
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 Gd N3 O4 S3'
_chemical_formula_sum            'C15 H14 Gd N3 O4 S3'
_chemical_formula_weight         553.72
_chemical_name_systematic        '[Gd(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             2021-10-05
_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                 94.848(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0345(7)
_cell_length_b                   9.9366(7)
_cell_length_c                   19.3797(13)
_cell_measurement_reflns_used    9632
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      32.66
_cell_measurement_theta_min      2.81
_cell_volume                     1925.4(2)
_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 0.968
_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  0.0512
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            96150
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.760
_diffrn_reflns_theta_min         2.806
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.795
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1207 before and 0.0615 after correction.
The Ratio of minimum to maximum transmission is 0.6876.
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    1.910
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.915
_exptl_crystal_size_mid          0.371
_exptl_crystal_size_min          0.218
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         6892
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0145P)²+4.1983P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5587
_reflns_number_total             6892
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc03352f2.cif
_cod_data_source_block           b_CCDC2
_cod_database_code               7130793
_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   0.492
_shelx_estimated_absorpt_t_min   0.129
_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. Uiso/Uaniso restraints and constraints
C9 \\sim C8 \\sim C7 \\sim C6 \\sim C10: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C6) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3.a Rotating group:
 O4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C12(H12), C5(H5), C10(H10), C2(H2), C13(H13), C4(H4),
 C3(H3), 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
Gd1 Gd 0.34521(2) 0.58545(2) 0.55133(2) 0.02409(4) Uani 1 1 d . . . . .
S1 S 0.07746(7) 0.59550(8) 0.59738(4) 0.03692(17) Uani 1 1 d . . . . .
S3 S 0.58597(8) 0.61000(9) 0.64728(4) 0.04089(19) Uani 1 1 d . . . . .
S2 S 0.37499(11) 0.86378(10) 0.57781(6) 0.0552(2) Uani 1 1 d . . . . .
O3 O 0.51174(18) 0.40643(19) 0.54487(9) 0.0253(4) Uani 1 1 d . . . . .
O2 O 0.2182(2) 0.7120(2) 0.47162(11) 0.0383(5) Uani 1 1 d . . . . .
O4 O 0.2312(2) 0.4244(2) 0.47649(12) 0.0391(5) Uani 1 1 d . . . . .
H4A H 0.273692 0.413637 0.440749 0.059 Uiso 1 1 d R U . . .
H4B H 0.155972 0.456351 0.460967 0.059 Uiso 1 1 d R U . . .
N3 N 0.5559(2) 0.3532(3) 0.60731(12) 0.0281(5) Uani 1 1 d . . . . .
O1 O 0.3125(2) 0.4536(3) 0.64571(14) 0.0600(8) Uani 1 1 d . . . . .
N2 N 0.1927(3) 0.8430(3) 0.47013(17) 0.0450(7) Uani 1 1 d . . . . .
N1 N 0.2061(2) 0.4137(3) 0.67600(13) 0.0365(6) Uani 1 1 d . . . . .
C15 C 0.5535(3) 0.2182(3) 0.61353(19) 0.0408(7) Uani 1 1 d . . . . .
H15 H 0.524141 0.165171 0.575729 0.049 Uiso 1 1 calc R U . . .
C14 C 0.5942(4) 0.1595(5) 0.6754(2) 0.0585(11) Uani 1 1 d . . . . .
H14 H 0.593670 0.066337 0.680006 0.070 Uiso 1 1 calc R U . . .
C12 C 0.6362(3) 0.3763(5) 0.72319(17) 0.0510(10) Uani 1 1 d . . . . .
H12 H 0.664733 0.429538 0.761056 0.061 Uiso 1 1 calc R U . . .
C11 C 0.5944(3) 0.4388(4) 0.65989(14) 0.0340(7) Uani 1 1 d . . . . .
C1 C 0.0854(3) 0.4705(3) 0.65811(15) 0.0302(6) Uani 1 1 d . . . . .
C5 C 0.2243(4) 0.3171(5) 0.7251(2) 0.0566(11) Uani 1 1 d . . . . .
H5 H 0.309094 0.281048 0.735643 0.068 Uiso 1 1 calc R U . . .
C10 C 0.1003(5) 0.8856(5) 0.4200(3) 0.0716(14) Uani 1 1 d . U . . .
H10 H 0.057763 0.823965 0.389476 0.086 Uiso 1 1 calc R U . . .
C6 C 0.2593(4) 0.9267(4) 0.5162(3) 0.0571(11) Uani 1 1 d . U . . .
C2 C -0.0218(3) 0.4226(4) 0.6926(2) 0.0464(8) Uani 1 1 d . . . . .
H2 H -0.106682 0.457898 0.681375 0.056 Uiso 1 1 calc R U . . .
C13 C 0.6361(4) 0.2398(5) 0.7306(2) 0.0620(13) Uani 1 1 d . . . . .
H13 H 0.664305 0.201129 0.773017 0.074 Uiso 1 1 calc R U . . .
C4 C 0.1203(4) 0.2724(5) 0.7590(2) 0.0594(11) Uani 1 1 d . . . . .
H4 H 0.133391 0.206734 0.793069 0.071 Uiso 1 1 calc R U . . .
C3 C -0.0052(4) 0.3255(4) 0.7424(2) 0.0559(10) Uani 1 1 d . . . . .
H3 H -0.077869 0.295449 0.764825 0.067 Uiso 1 1 calc R U . . .
C9 C 0.0699(6) 1.0177(7) 0.4145(4) 0.118(3) Uani 1 1 d . U . . .
H9 H 0.005871 1.047539 0.380433 0.142 Uiso 1 1 calc R U . . .
C7 C 0.2271(5) 1.0636(5) 0.5087(4) 0.105(2) Uani 1 1 d . U . . .
H7 H 0.270579 1.126187 0.538311 0.126 Uiso 1 1 calc R U . . .
C8 C 0.1335(6) 1.1062(5) 0.4588(5) 0.131(3) Uani 1 1 d . U . . .
H8 H 0.112886 1.197312 0.455141 0.158 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'
Gd Gd -0.1653 3.9035 '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'
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 Gd1 S3 122.45(2) . . ?
S2 Gd1 S1 89.82(3) . . ?
S2 Gd1 S3 74.60(3) . . ?
O3 Gd1 S1 133.89(5) . . ?
O3 Gd1 S1 148.23(4) 3_666 . ?
O3 Gd1 S3 64.15(5) . . ?
O3 Gd1 S3 88.60(5) 3_666 . ?
O3 Gd1 S2 131.14(5) . . ?
O3 Gd1 S2 92.65(5) 3_666 . ?
O3 Gd1 O3 62.55(7) 3_666 . ?
O2 Gd1 S1 73.28(6) . . ?
O2 Gd1 S3 139.72(6) . . ?
O2 Gd1 S2 68.27(6) . . ?
O2 Gd1 O3 134.91(7) . . ?
O2 Gd1 O3 78.29(7) . 3_666 ?
O2 Gd1 O4 75.38(8) . . ?
O2 Gd1 O1 137.80(8) . . ?
O4 Gd1 S1 78.54(6) . . ?
O4 Gd1 S3 140.22(6) . . ?
O4 Gd1 S2 143.63(6) . . ?
O4 Gd1 O3 77.07(7) . . ?
O4 Gd1 O3 80.85(7) . 3_666 ?
O1 Gd1 S1 64.93(6) . . ?
O1 Gd1 S3 73.02(7) . . ?
O1 Gd1 S2 115.73(9) . . ?
O1 Gd1 O3 139.29(8) . 3_666 ?
O1 Gd1 O3 76.74(8) . . ?
O1 Gd1 O4 90.46(11) . . ?
C1 S1 Gd1 101.33(10) . . ?
C11 S3 Gd1 92.06(10) . . ?
C6 S2 Gd1 100.13(14) . . ?
Gd1 O3 Gd1 117.45(7) 3_666 . ?
N3 O3 Gd1 121.49(14) . 3_666 ?
N3 O3 Gd1 114.14(14) . . ?
N2 O2 Gd1 130.4(2) . . ?
Gd1 O4 H4A 109.4 . . ?
Gd1 O4 H4B 109.3 . . ?
H4A O4 H4B 104.5 . . ?
C15 N3 O3 117.4(3) . . ?
C15 N3 C11 124.2(3) . . ?
C11 N3 O3 118.4(2) . . ?
N1 O1 Gd1 134.44(18) . . ?
O2 N2 C10 116.2(4) . . ?
O2 N2 C6 120.3(3) . . ?
C10 N2 C6 123.5(4) . . ?
O1 N1 C1 120.0(2) . . ?
O1 N1 C5 117.3(3) . . ?
C5 N1 C1 122.7(3) . . ?
N3 C15 H15 120.1 . . ?
N3 C15 C14 119.9(4) . . ?
C14 C15 H15 120.1 . . ?
C15 C14 H14 120.5 . . ?
C15 C14 C13 119.1(4) . . ?
C13 C14 H14 120.5 . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C13 C12 C11 121.8(4) . . ?
N3 C11 S3 120.3(2) . . ?
N3 C11 C12 115.0(3) . . ?
C12 C11 S3 124.6(3) . . ?
N1 C1 S1 117.9(2) . . ?
N1 C1 C2 116.3(3) . . ?
C2 C1 S1 125.8(2) . . ?
N1 C5 H5 119.7 . . ?
N1 C5 C4 120.7(3) . . ?
C4 C5 H5 119.7 . . ?
N2 C10 H10 120.1 . . ?
C9 C10 N2 119.8(6) . . ?
C9 C10 H10 120.1 . . ?
N2 C6 S2 120.2(3) . . ?
N2 C6 C7 115.4(4) . . ?
C7 C6 S2 124.3(4) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.8(3) . . ?
C3 C2 H2 119.1 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0(3) . . ?
C12 C13 H13 120.0 . . ?
C5 C4 H4 120.4 . . ?
C5 C4 C3 119.2(3) . . ?
C3 C4 H4 120.4 . . ?
C2 C3 C4 119.4(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C10 C9 H9 120.3 . . ?
C10 C9 C8 119.4(6) . . ?
C8 C9 H9 120.3 . . ?
C6 C7 H7 119.4 . . ?
C8 C7 C6 121.1(6) . . ?
C8 C7 H7 119.4 . . ?
C9 C8 C7 120.7(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
Gd1 S1 2.9034(8) . ?
Gd1 S3 2.9316(8) . ?
Gd1 S2 2.8241(10) . ?
Gd1 O3 2.4484(18) 3_666 ?
Gd1 O3 2.4511(18) . ?
Gd1 O2 2.293(2) . ?
Gd1 O4 2.386(2) . ?
Gd1 O1 2.296(2) . ?
S1 C1 1.708(3) . ?
S3 C11 1.720(4) . ?
S2 C6 1.711(5) . ?
O3 N3 1.360(3) . ?
O2 N2 1.327(4) . ?
O4 H4A 0.8501 . ?
O4 H4B 0.8502 . ?
N3 C15 1.347(4) . ?
N3 C11 1.358(4) . ?
O1 N1 1.321(3) . ?
N2 C10 1.352(5) . ?
N2 C6 1.355(6) . ?
N1 C1 1.355(4) . ?
N1 C5 1.353(4) . ?
C15 H15 0.9300 . ?
C15 C14 1.364(5) . ?
C14 H14 0.9300 . ?
C14 C13 1.372(7) . ?
C12 H12 0.9300 . ?
C12 C11 1.407(4) . ?
C12 C13 1.364(6) . ?
C1 C2 1.397(4) . ?
C5 H5 0.9300 . ?
C5 C4 1.354(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.350(7) . ?
C6 C7 1.403(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.364(5) . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C4 C3 1.378(5) . ?
C3 H3 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.352(10) . ?
C7 H7 0.9300 . ?
C7 C8 1.357(9) . ?
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
Gd1 S1 C1 N1 8.0(3) . . . . ?
Gd1 S1 C1 C2 -173.4(3) . . . . ?
Gd1 S3 C11 N3 34.2(2) . . . . ?
Gd1 S3 C11 C12 -143.9(3) . . . . ?
Gd1 S2 C6 N2 -4.3(4) . . . . ?
Gd1 S2 C6 C7 176.4(5) . . . . ?
Gd1 O3 N3 C15 129.2(2) . . . . ?
Gd1 O3 N3 C15 -80.6(3) 3_666 . . . ?
Gd1 O3 N3 C11 -48.2(3) . . . . ?
Gd1 O3 N3 C11 101.9(2) 3_666 . . . ?
Gd1 O2 N2 C10 -172.2(3) . . . . ?
Gd1 O2 N2 C6 9.0(5) . . . . ?
Gd1 O1 N1 C1 -11.3(5) . . . . ?
Gd1 O1 N1 C5 169.5(3) . . . . ?
S1 C1 C2 C3 -177.6(3) . . . . ?
S2 C6 C7 C8 -179.6(6) . . . . ?
O3 N3 C15 C14 -178.8(3) . . . . ?
O3 N3 C11 S3 0.4(3) . . . . ?
O3 N3 C11 C12 178.7(2) . . . . ?
O2 N2 C10 C9 -179.1(5) . . . . ?
O2 N2 C6 S2 -1.1(5) . . . . ?
O2 N2 C6 C7 178.3(4) . . . . ?
N3 C15 C14 C13 0.6(5) . . . . ?
O1 N1 C1 S1 -1.3(4) . . . . ?
O1 N1 C1 C2 -180.0(3) . . . . ?
O1 N1 C5 C4 179.1(4) . . . . ?
N2 C10 C9 C8 0.6(10) . . . . ?
N2 C6 C7 C8 1.0(9) . . . . ?
N1 C1 C2 C3 1.0(6) . . . . ?
N1 C5 C4 C3 0.7(8) . . . . ?
C15 N3 C11 S3 -176.9(2) . . . . ?
C15 N3 C11 C12 1.5(4) . . . . ?
C15 C14 C13 C12 0.1(6) . . . . ?
C11 N3 C15 C14 -1.4(5) . . . . ?
C11 C12 C13 C14 -0.1(6) . . . . ?
C1 N1 C5 C4 0.0(7) . . . . ?
C1 C2 C3 C4 -0.3(7) . . . . ?
C5 N1 C1 S1 177.8(3) . . . . ?
C5 N1 C1 C2 -0.9(5) . . . . ?
C5 C4 C3 C2 -0.6(7) . . . . ?
C10 N2 C6 S2 -179.9(4) . . . . ?
C10 N2 C6 C7 -0.4(7) . . . . ?
C10 C9 C8 C7 0.0(13) . . . . ?
C6 N2 C10 C9 -0.4(8) . . . . ?
C6 C7 C8 C9 -0.8(12) . . . . ?
C13 C12 C11 S3 177.5(3) . . . . ?
C13 C12 C11 N3 -0.7(5) . . . . ?
