Uranium oxide hydrate frameworks with Er(iii) or Y(iii) ions: revealing structural insights leading to the low symmetry
Ablott, Timothy A.; Lu, Kimbal T.; Aughterson, Robert D.; Zhang, Yingjie; Dalton Transactions  (2022) –; doi:10.1039/D2DT02763A

data_7711439
_publ_section_title
;
 Uranium oxide hydrate frameworks with Er(iii) or Y(iii) ions: revealing
 structural insights leading to the low symmetry
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02763A
_journal_year                    2022
_chemical_formula_moiety         'Er O22.5 U5.5'
_chemical_formula_sum            'Er O22.5 U5.5'
_chemical_formula_weight         1836.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_audit_creation_date             2022-08-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-08-07 deposited with the CCDC.	2022-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                111.33(3)
_cell_angle_beta                 102.97(3)
_cell_angle_gamma                106.48(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1060(16)
_cell_length_b                   11.435(2)
_cell_length_c                   11.582(2)
_cell_measurement_reflns_used    16000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      2.030
_cell_volume                     892.1(5)
_computing_cell_refinement       'BlueIce (McPhillips, et al., 2002)'
_computing_data_collection       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Eiger Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.71095
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_unetI/netI     0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.934
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9898
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.030
_diffrn_source                   'Australian Synchrotron MX2'
_exptl_absorpt_coefficient_mu    54.500
_exptl_absorpt_correction_T_max  0.4344
_exptl_absorpt_correction_T_min  0.1810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.2142 before and 0.0882 after correction.
The Ratio of minimum to maximum transmission is 0.4167.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    6.837
_exptl_crystal_description       plate
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.004
_refine_diff_density_max         7.593
_refine_diff_density_min         -7.009
_refine_diff_density_rms         1.374
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         2934
_refine_ls_number_restraints     409
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0914
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1840P)^2^+198.1085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2623
_refine_ls_wR_factor_ref         0.2870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2456
_reflns_number_total             2934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02763a2.cif
_cod_data_source_block           p-1_CCDC1
_cod_original_cell_volume        892.0(4)
_cod_original_formula_sum        'Er O22.50 U5.50'
_cod_database_code               7711439
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O7) = Uanis(O17) = Uanis(O18) = Uanis(O12) = Uanis(O17) =
Uanis(O20) = Uanis(O23)
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O17(0.5)
;
_shelx_res_checksum              93681
_shelx_hkl_checksum              90701
_olex2_submission_special_instructions 'No special instructions were received'