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_7703936
_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         'O28 Pr3 U6'
_chemical_formula_sum            'O28 Pr3 U6'
_chemical_formula_weight         2298.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-06
_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                 90.08(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   6.8880(14)
_cell_length_b                   6.7750(14)
_cell_length_c                   11.928(2)
_cell_measurement_reflns_used    15000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.993
_cell_measurement_theta_min      3.414
_cell_volume                     556.63(19)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Eiga Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.71078
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6389
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         3.414
_diffrn_source                   'Australian Synchrotron MX2'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    50.017
_exptl_absorpt_correction_T_max  0.4345
_exptl_absorpt_correction_T_min  0.3655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0910 before and 0.0559 after correction.
The Ratio of minimum to maximum transmission is 0.8412.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    6.858
_exptl_crystal_description       plate
_exptl_crystal_F_000             953
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.003
_refine_diff_density_max         3.385
_refine_diff_density_min         -3.132
_refine_diff_density_rms         0.630
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.22(3)
_refine_ls_extinction_coef       0.00123(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         1915
_refine_ls_number_restraints     314
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0467
_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^)+108.6860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1074
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                1912
_reflns_number_total             1915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00526f2.cif
_cod_data_source_block           p21byn
_cod_depositor_comments
'Adding full bibliography for 7703936--7703937.cif.'
_cod_original_cell_volume        556.6(2)
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               7703936
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.78(3)
 0.22(3)
2. Uiso/Uaniso restraints and constraints
Uanis(O12) = Uanis(O14) = Uanis(O13)
Uanis(U2) = Uanis(U3) = Uanis(U1)
3. 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
4. Others
 Fixed Sof: Pr2(0.5)
;
_shelx_res_checksum              72022
_olex2_submission_special_instructions 'No special instructions were received'