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_7130789
_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 Am N3 O4 S3, 3(H2O)'
_chemical_formula_sum            'C15 H20 Am N3 O7 S3'
_chemical_formula_weight         693.52
_chemical_name_systematic        '[Am(mpo)2(u-O-mpo)(H2O)]2?3H2O'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-21
_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                92.332(5)
_cell_angle_beta                 107.744(4)
_cell_angle_gamma                92.932(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3942(10)
_cell_length_b                   9.6982(10)
_cell_length_c                   13.6896(18)
_cell_measurement_reflns_used    9510
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.55
_cell_volume                     1058.2(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      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-III CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54347
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.353
_diffrn_reflns_theta_min         2.552
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.963
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1681 before and 0.1088 after correction.
The Ratio of minimum to maximum transmission is 0.5773.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_description       irregular
_exptl_crystal_F_000             660
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.536
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.870
_refine_diff_density_min         -4.895
_refine_diff_density_rms         0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5265
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0392
_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/[\s^2^(Fo^2^)+(0.0198P)^2^+19.3672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5084
_reflns_number_total             5265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03352f2.cif
_cod_data_source_block           e
_cod_database_code               7130789
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.520
_shelx_estimated_absorpt_t_min   0.225
_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. Restrained distances
 Am1-H4A \\sim Am1-H4B
 with sigma of 0.02
3.a Free rotating group:
 O4(H4A,H4B), O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C15(H15), C8(H8), C4(H4), C9(H9), C10(H10), C14(H14),
 C12(H12), C13(H13), C2(H2), C3(H3)
;
_shelx_res_checksum              15600
_shelx_hkl_checksum              8197
_olex2_submission_special_instructions 'No special instructions were received'