Layer-structured uranyl-oxide hydroxy-hydrates with Pr(iii) and Tb(iii) ions: hydroxyl to oxo transition driven by interlayer cations.
Lu, Kimbal Thane; Zhang, Yingjie; Wei, Tao; Čejka, Jiří; Zheng, Rongkun; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5832–5841; doi:10.1039/d0dt00526f

data_7703937
_publ_section_title
;
 Layer-structured uranyl-oxide hydroxy-hydrates with Pr(iii) and Tb(iii)
 ions: hydroxyl to oxo transition driven by interlayer cations.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5832
_journal_page_last               5841
_journal_paper_doi               10.1039/d0dt00526f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'O27 Tb U6, 0.5(O)'
_chemical_formula_sum            'O27.5 Tb U6'
_chemical_formula_weight         2027.10
_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'
_audit_creation_date             2019-12-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-01-30 deposited with the CCDC.	2020-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.66(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.772(3)
_cell_length_b                   14.798(3)
_cell_length_c                   13.743(3)
_cell_measurement_reflns_used    15000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.997
_cell_measurement_theta_min      1.704
_cell_volume                     2433.8(12)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Eiga Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.71077
_diffrn_reflns_av_R_equivalents  0.1338
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28776
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.702
_diffrn_source                   'Australian Synchrotron MX2'
_exptl_absorpt_coefficient_mu    42.748
_exptl_absorpt_correction_T_max  0.4347
_exptl_absorpt_correction_T_min  0.1940
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.2176 before and 0.0814 after correction.
The Ratio of minimum to maximum transmission is 0.4463.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    5.532
_exptl_crystal_description       plate
_exptl_crystal_F_000             3348
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.005
_refine_diff_density_max         8.788
_refine_diff_density_min         -3.424
_refine_diff_density_rms         0.797
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4287
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0880P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3372
_reflns_number_total             4287
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00526f2.cif
_cod_data_source_block           p21byc_a
_cod_depositor_comments
'Adding full bibliography for 7703936--7703937.cif.'
_cod_original_cell_volume        2433.8(11)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'O27.50 Tb U6'
_cod_database_code               7703937
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Restrained distances
 U6-O20 = U6-O21
 1.75 with sigma of 0.02
2. Others
 Fixed Sof: O6W(0.5)
;
_shelx_res_checksum              18488
_olex2_submission_special_instructions 'No special instructions were received'