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_7715928
_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         'C22 H46 N4 O7 U, 3(I)'
_chemical_formula_sum            'C22 H46 I3 N4 O7 U'
_chemical_formula_weight         1097.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_Hall           '-I 2b 2c'
_space_group_name_H-M_alt        'I b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-03-15 deposited with the CCDC.	2024-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.2159(5)
_cell_length_b                   14.8269(5)
_cell_length_c                   31.2033(11)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.477
_cell_measurement_theta_min      2.376
_cell_volume                     6577.0(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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Photon III'
_diffrn_detector_type            'CPAD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.8 mm pinhole collimator'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            38026
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         2.376
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\mS'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.794
_exptl_absorpt_correction_T_max  0.4935
_exptl_absorpt_correction_T_min  0.4108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1285 before and 0.0693 after correction.
The Ratio of minimum to maximum transmission is 0.8324.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_description       block
_exptl_crystal_F_000             4104
_exptl_crystal_recrystallization_method
'Vapour diffusion in dimethylformamide and ether'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.831
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0356P)^2^+37.2613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3040
_reflns_number_total             3240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00521j2.cif
_cod_data_source_block           mo_mja_nk_11052021_0m
_cod_depositor_comments
'Adding full bibliography for 7715927--7715929.cif.'
_cod_database_code               7715928
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.652
_shelx_estimated_absorpt_t_min   0.652
_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.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C2(H2A,H2B), C4(H4A,H4B), C7(H7A,H7B), C6(H6A,H6B), C3(H3A,H3B),
 C1(H1A,H1B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C1S(H1S)
2.c Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              38407
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MicroMount (MiTeGen) with paratone oil (Parabar 10312, Hampton Research).'
_olex2_submission_special_instructions 'No special instructions were received'