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_7130799
_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 Er N3 O5 S3, H2 O'
_chemical_formula_sum            'C15 H18 Er N3 O6 S3'
_chemical_formula_weight         599.76
_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             2021-10-26
_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                111.4100(10)
_cell_angle_beta                 94.0230(10)
_cell_angle_gamma                91.0700(10)
_cell_formula_units_Z            2
_cell_length_a                   7.44370(10)
_cell_length_b                   11.0980(2)
_cell_length_c                   13.1205(2)
_cell_measurement_reflns_used    9086
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      38.65
_cell_measurement_theta_min      2.75
_cell_volume                     1005.46(3)
_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       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            178231
_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         46.476
_diffrn_reflns_theta_min         1.973
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.522
_exptl_absorpt_correction_T_max  0.7491
_exptl_absorpt_correction_T_min  0.6355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0776 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.8484.
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    1.981
_exptl_crystal_description       plate
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.563
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.258
_refine_diff_density_max         1.085
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         17847
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+0.5382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14492
_reflns_number_total             17847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03352f2.cif
_cod_data_source_block           a_CCDC4
_cod_depositor_comments
;

2025-03-31
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C30 H36 Er2 N6 O12 S6'
_cod_original_formula_weight         1199.53
_cod_original_formula_moiety         '2(C15 H16 Er N3 O5 S3), 2(H2 O)'
_cod_original_formula_units_Z            1
_cod_database_code               7130799
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.388
_shelx_estimated_absorpt_t_min   0.185
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Er1-H5A \\sim Er1-H5B
 with sigma of 0.02
3.a Free rotating group:
 O5(H5A,H5B), O6(H6A)
3.b Rotating group:
 O4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C5(H5), C10(H10), C2(H2), C4(H4), C12(H12), C3(H3), C14(H14),
 C9(H9), C7(H7), C8(H8), C13(H13)
;
_shelx_res_checksum              40917
_shelx_hkl_checksum              37354
_olex2_submission_special_instructions 'No special instructions were received'