Targeted Crystal Growth of Uranium Gallophosphates Via the Systematic Exploration of the UF4-GaPO4-ACl (A = Cs, Rb) Phase Space
Juillerat, Christian A.; Klepov, Vladislav; Smith, Mark D.; Zur Loye, Hans-Conrad; CrystEngComm  (2020) –; doi:10.1039/D0CE00343C

data_7240282
_publ_section_title
;
 Targeted Crystal Growth of Uranium Gallophosphates Via the Systematic
 Exploration of the UF4-GaPO4-ACl (A = Cs, Rb) Phase Space
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00343C
_journal_year                    2020
_chemical_formula_moiety         '0.25(O208 P36 Rb44 U32)'
_chemical_formula_sum            'O52 P9 Rb11.02 U8'
_chemical_formula_weight         3957.28
_chemical_name_systematic        Rb11[(UO2)8(PO4)9]
_space_group_crystal_system      tetragonal
_space_group_IT_number           135
_space_group_name_Hall           '-P 4c 2ab'
_space_group_name_H-M_alt        'P 42/m b c'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-31
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-18 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.7697(6)
_cell_length_b                   25.7697(6)
_cell_length_c                   9.3962(2)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      33.09
_cell_measurement_theta_min      2.50
_cell_volume                     6239.8(2)
_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      301.14
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            100392
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.499
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    29.564
_exptl_absorpt_correction_T_max  0.1605
_exptl_absorpt_correction_T_min  0.0668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1592 before and 0.0684 after correction.
The Ratio of minimum to maximum transmission is 0.4162.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.212
_exptl_crystal_description       needle
_exptl_crystal_F_000             6780
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.126
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.326
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         3807
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.328
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+153.3181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3640
_reflns_number_total             3807
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00343c2.cif
_cod_data_source_block           Rb11U8P9O52
_cod_original_cell_volume        6239.8(3)
_cod_database_code               7240282
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.589
_shelx_estimated_absorpt_t_min   0.156
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Rb4A) \\sim Ueq, Uanis(Rb4B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O12A) \\sim Ueq, Uanis(O9A) \\sim Ueq, Uanis(O11A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.01
2. Others
 1*[Sof(Rb5A)]+2*[Sof(Rb5B)]+1*[Sof(Rb5C)]=1 with esd of 0.0001
 2*[Sof(Rb4A)]+1*[Sof(Rb4B)]=0.5 with esd of 0.0001
 Sof(P2B)=Sof(O9B)=Sof(O10B)=Sof(O11B)=Sof(O12B)=1-FVAR(1)
 Sof(P2A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=FVAR(1)
 Sof(P3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=1-FVAR(2)
 Sof(P3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=FVAR(2)
 Fixed Sof: U4(0.5) O8(0.5) O15A(0.5) O15B(0.5) O16(0.5) O17(0.5)
;
_shelx_res_checksum              54238
_olex2_submission_special_instructions 'No special instructions were received'