Comparison of the structural, electrochemical, and spectroscopic properties of two cryptates of trivalent uranium.
Kulasekara, D. Nuwangi; Bailey, Matthew D.; Ward, Cassandra L.; Allen, Matthew J.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8657–8661; doi:10.1039/d4dt00521j

data_7715929
_publ_section_title
;
 Comparison of the structural, electrochemical, and spectroscopic
 properties of two cryptates of trivalent uranium.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8657
_journal_page_last               8661
_journal_paper_doi               10.1039/d4dt00521j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C20.174 H41.762 N3.013 O6.555 U0.885, 3(I), 0.115(C24 H50 N4 O8 U1), C1.073 H2.503 N0.528 O0.528'
_chemical_formula_sum            'C24 H50.01 I3 N4 O8 U'
_chemical_formula_weight         1141.44
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2023-03-15 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.769(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8644(12)
_cell_length_b                   10.3453(6)
_cell_length_c                   18.2109(10)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.024
_cell_measurement_theta_min      2.233
_cell_volume                     3436.6(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            134878
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.730
_diffrn_reflns_theta_min         2.233
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.465
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.4980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1320 before and 0.0937 after correction.
The Ratio of minimum to maximum transmission is 0.6677.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.206
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.626
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.235
_refine_diff_density_max         0.959
_refine_diff_density_min         -1.776
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         7296
_refine_ls_number_restraints     1818
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+29.3223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6465
_reflns_number_total             7296
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00521j2.cif
_cod_data_source_block           mb_nk_aza222_ui3_3
_cod_depositor_comments
'Adding full bibliography for 7715927--7715929.cif.'
_cod_database_code               7715929
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.273
_shelx_estimated_absorpt_t_min   0.089
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N3, N3C}
{O7, O7C}
3. Restrained distances
 O7-C19C \\sim O7-C19 \\sim O8-C22 \\sim O7B-C19B
 with sigma of 0.02
 C19C-C21C \\sim C19-C21 \\sim C22-C23 \\sim C21B-C20B
 with sigma of 0.02
 N3-C19C \\sim N3-C19 \\sim N4-C22 \\sim N3B-C19B
 with sigma of 0.02
 C19C-C20C \\sim C19-C20 \\sim C22-C24 \\sim C19B-C20B
 with sigma of 0.02
 N3-C21C \\sim N3-C20 \\sim N3-C20C \\sim N3-C21 \\sim N4-C24 \\sim N4-C23
\\sim N3B-C20B \\sim N3B-C21B
 with sigma of 0.02
 C21-C20 \\sim C23-C24 \\sim C20C-C21C
 with sigma of 0.02
 O2B-C4B \\sim O2B-C5B \\sim O1-C2 \\sim O1-C3 \\sim O3B-C8B \\sim O3B-C9B
\\sim O2-C4 \\sim O2-C5 \\sim O4B-
 C10B \\sim O4B-C11B \\sim O3-C8 \\sim O3-C9 \\sim O1B-C2B \\sim O1B-C3B \\sim
O4-C10 \\sim O4-C11 \\sim O5-C14
 \\sim O5-C15 \\sim O6-C16 \\sim O6-C17 \\sim O5B-C15B \\sim O5B-C14B \\sim
O6B-C16B \\sim O6B-C17B
 with sigma of 0.02
 N1-C12 \\sim N1-C13 \\sim N1-C1 \\sim N2B-C6B \\sim N2B-C7B \\sim N2B-C18B
\\sim N2-C7 \\sim N2-C18 \\sim N2-
 C6 \\sim N1B-C1B \\sim N1B-C13B \\sim N1B-C12B
 with sigma of 0.02
 C12-C11 \\sim C9-C10 \\sim C2B-C1B \\sim C14B-C13B \\sim C16B-C15B \\sim
C18B-C17B \\sim C14-C13 ~
 C16-C15 \\sim C8B-C7B \\sim C4-C3 \\sim C10B-C9B \\sim C6-C5 \\sim C3B-C4B
\\sim C6B-C5B \\sim C2-C1 \\sim C18-
 C17 \\sim C8-C7 \\sim C12B-C11B
 with sigma of 0.02
 U1-N2 \\sim U1B-N1B \\sim U1-N1 \\sim U1B-N2B
 with sigma of 0.02
 U1-O3 \\sim U1B-O4B \\sim U1-O2 \\sim U1B-O3B \\sim U1-O1 \\sim U1B-O2B \\sim
U1-O4 \\sim U1B-O1B \\sim U1-O5
 \\sim U1B-O6B \\sim U1B-O5B \\sim U1-O6
 with sigma of 0.02
 C4-C5 \\sim C2-C3 \\sim C10-C11 \\sim C8-C9 \\sim C17B-C16B \\sim C15B-C14B
\\sim C14-C15 \\sim C16-C17 ~
 C5B-C4B \\sim C3B-C2B \\sim C11B-C10B \\sim C9B-C8B
 with sigma of 0.02
 C1-C12 \\sim C6B-C7B \\sim C12B-C1B \\sim C7-C6
 with sigma of 0.02
 C23B-C25 \\sim C23-C24 \\sim C21-C20 \\sim C20C-C21C
 with sigma of 0.02
 N4B-C25 \\sim N4B-C23B \\sim N4-C23 \\sim N4-C24 \\sim N3-C21 \\sim N3-C20C
\\sim N3-C20 \\sim N3-C21C
 with sigma of 0.02
 C22B-C25 \\sim C22-C24 \\sim C19C-C20C \\sim C19-C20
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
U1 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8
\\sim N1 \\sim N2 \\sim N3 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14
\\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22
\\sim C23 \\sim C24 \\sim U1B \\sim O1B \\sim O2B \\sim O3B \\sim O4B \\sim O5B
\\sim O6B \\sim O7B \\sim O8B \\sim N1B \\sim N2B \\sim N3B \\sim C1B \\sim C2B
\\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim C9B \\sim
C10B \\sim C11B \\sim C12B \\sim C13B \\sim C14B \\sim C15B \\sim C16B \\sim
C17B \\sim C18B \\sim C19B \\sim C20B \\sim C21B \\sim C22B \\sim C19C \\sim
H19C \\sim C20C \\sim C21C: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
N4B \\sim C22B \\sim C23B \\sim C25: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
Uanis(N3) = Uanis(N3C)
Uanis(O7) = Uanis(O7C)
5. Others
 1*[Sof(O7)+Sof(N3)+Sof(C19C)+Sof(H19C)+Sof(C20C)+Sof(H20G)+Sof(H20H)+
 Sof(H20I)+Sof(C21C)+Sof(H21G)+Sof(H21H)+Sof(H21I)]+1*[Sof(C19)+Sof(H19)+
 Sof(C20)+Sof(H20A)+Sof(H20B)+Sof(H20C)+Sof(C21)+Sof(H21A)+Sof(H21B)+Sof(H21C)+
 Sof(O7C)+Sof(N3C)]=0.885 with esd of 0.001
 Sof(U1B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(O7B)=
 Sof(O8B)=Sof(N1B)=Sof(N2B)=Sof(N3B)=Sof(N4B)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=
 Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C4B)=Sof(H4BA)=
 Sof(H4BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C7B)=
 Sof(H7BB)=Sof(H7BA)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=
 Sof(C10B)=Sof(H10C)=Sof(H10D)=Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=
 Sof(H12D)=Sof(H12C)=Sof(C13B)=Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14C)=
 Sof(H14D)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C16B)=Sof(H16C)=Sof(H16D)=
 Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=Sof(H18D)=Sof(H18C)=Sof(C19B)=
 Sof(H19B)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21B)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=1-FVAR(1)
 Sof(U1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(O8)=Sof(N1)=
 Sof(N2)=Sof(N4)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=
 Sof(H6B)=Sof(H6A)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14B)=
 Sof(H14A)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=
 Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18B)=Sof(H18A)=Sof(C22)=Sof(H22)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
 Sof(O7)=Sof(N3)=Sof(C19C)=Sof(H19C)=Sof(C20C)=Sof(H20G)=Sof(H20H)=Sof(H20I)=
 Sof(C21C)=Sof(H21G)=Sof(H21H)=Sof(H21I)=FVAR(2)
 Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=Sof(O7C)=Sof(N3C)=FVAR(3)
 Sof(I1B)=1-FVAR(4)
 Sof(I1)=FVAR(4)
 Sof(I2B)=1-FVAR(5)
 Sof(I2)=FVAR(5)
 Sof(I3B)=1-FVAR(6)
 Sof(I3)=FVAR(6)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6B,H6A),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14B,H14A), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18B,H18A), C1B(H1BA,H1BB), C2B(H2BA,H2BB), C3B(H3BA,
 H3BB), C4B(H4BA,H4BB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C7B(H7BB,H7BA),
 C8B(H8BA,H8BB), C9B(H9BA,H9BB), C10B(H10C,H10D), C11B(H11C,H11D), C12B(H12D,
 H12C), C13B(H13C,H13D), C14B(H14C,H14D), C15B(H15C,H15D), C16B(H16C,H16D),
 C17B(H17C,H17D), C18B(H18D,H18C)
6.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C22(H22), C19B(H19B), C22B(H22B), C19C(H19C)
6.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C20B(H20D,H20E,H20F), C21B(H21D,H21E,H21F), C23B(H23D,H23E,H23F),
 C25(H25A,H25B,H25C), C20C(H20G,H20H,H20I), C21C(H21G,H21H,H21I)
;
_shelx_res_checksum              8777
_olex2_exptl_crystal_mounting_method
'MicroMount (MiTeGen) with paratone oil (Parabar 10312, Hampton Research)'
_olex2_submission_special_instructions 'No special instructions were received'