Synthesis and characterization of a bimetallic americium(iii) pyrithionate coordination complex
Huffman, Zachary K.; Sperling, Joseph M.; Windorff, Cory J.; Long, Brian N.; Cordova, Lucas; Ramanantoanina, Harry; Celis-Barros, Cristian; Albrecht-Schönzart, Thomas E.; Chemical Communications  (2022) –; doi:10.1039/D2CC03352F

data_7130793
_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       '\f and \w 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 \l/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/[\s^2^(Fo^2^)+(0.0145P)^2^+4.1983P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            d2cc03352f2.cif
_cod_data_source_block           b_CCDC2
_cod_database_code               7130793
_shelx_shelxl_version_number     2018/3
_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)
;
_shelx_res_checksum              89149
_shelx_hkl_checksum              21319
_olex2_submission_special_instructions 'No special instructions were received'