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_7240281
_publ_section_title
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 Targeted Crystal Growth of Uranium Gallophosphates Via the Systematic
 Exploration of the UF4-GaPO4-ACl (A = Cs, Rb) Phase Space
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00343C
_journal_year                    2020
_chemical_formula_moiety         '0.5(F0.8 O65.2 P4 Rb15.2 U16)'
_chemical_formula_sum            'F0.4 O32.6 P2 Rb7.6 U8'
_chemical_formula_weight         3144.95
_chemical_name_systematic        Rb7.5[(UO2)8O8.6F0.4(PO4)2]
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-04
_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                 101.343(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5935(5)
_cell_length_b                   13.7652(8)
_cell_length_c                   13.2983(8)
_cell_measurement_reflns_used    9562
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      35.67
_cell_measurement_theta_min      2.83
_cell_volume                     1721.82(17)
_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      302.88
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0674
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            109936
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         2.151
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    48.351
_exptl_absorpt_correction_T_max  0.1661
_exptl_absorpt_correction_T_min  0.0738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1673 before and 0.0776 after correction.
The Ratio of minimum to maximum transmission is 0.4443.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    6.066
_exptl_crystal_description       shard
_exptl_crystal_F_000             2623
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.573
_refine_diff_density_min         -2.114
_refine_diff_density_rms         0.382
_refine_ls_extinction_coef       0.000081(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.362
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3952
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.362
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0056P)^2^+99.4920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3757
_reflns_number_total             3952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00343c2.cif
_cod_data_source_block           Rb76U8P2O326F04
_cod_original_formula_sum        'F0.40 O32.60 P2 Rb7.60 U8'
_cod_database_code               7240281
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.643
_shelx_estimated_absorpt_t_min   0.325
_olex2_refinement_description
;
1. Shared sites
{F4, O4}
2. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(F4) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(F4) = Uanis(O4)
3. Others
 Sof(Rb3A)=1-FVAR(1)
 Sof(Rb3B)=FVAR(1)
 Sof(Rb4B)=1-FVAR(2)
 Sof(Rb4A)=FVAR(2)
 Fixed Sof: U4A(0.5) U4B(0.5) Rb5(0.3) F4(0.2) O4(0.8) O11(0.5)
;
_shelx_res_checksum              93247
_olex2_submission_special_instructions 'No special instructions were received'