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_7130790
_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 H16 Ho N3 O5 S3, H2 O'
_chemical_formula_sum            'C15 H18 Ho N3 O6 S3'
_chemical_formula_weight         597.43
_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             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                111.452(3)
_cell_angle_beta                 93.982(3)
_cell_angle_gamma                91.030(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4507(8)
_cell_length_b                   11.1249(13)
_cell_length_c                   13.1555(16)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      3.01
_cell_volume                     1011.3(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      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.889
_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  0.0586
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32658
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.232
_diffrn_reflns_theta_min         2.743
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.258
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1409 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.7846.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_description       plate
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4439
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0122P)^2^+0.5442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3834
_reflns_number_total             4439
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03352f2.cif
_cod_data_source_block           b
_cod_database_code               7130790
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.265
_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
 Ho01-H5A \\sim Ho01-H5B
 with sigma of 0.02
3.a Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
3.b Rotating group:
 O4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C15(H15), C5(H5), C14(H14), C12(H12), C7(H7), C9(H9), C13(H13),
 C8(H8), C2(H2), C4(H4), C3(H3)
;
_shelx_res_checksum              96768
_shelx_hkl_checksum              88911
_olex2_submission_special_instructions 'No special instructions were received'