Flux versus Hydrothermal Growth: Polymorphism of A2(UO2)Si2O6 (A = Rb, Cs).
Morrison, Gregory; Smith, Mark D.; Zur Loye, Hans-Conrad; Inorganic chemistry 56 (2017) 1053–1056; doi:10.1021/acs.inorgchem.6b02931

data_4345401
_publ_section_title
;
 Flux versus Hydrothermal Growth: Polymorphism of A2(UO2)Si2O6 (A = Rb,
 Cs).
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1053
_journal_page_last               1056
_journal_paper_doi               10.1021/acs.inorgchem.6b02931
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'Cs2 O8 Si2 U'
_chemical_formula_weight         688.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 95.849(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.136(2)
_cell_length_b                   10.0426(17)
_cell_length_c                   7.7896(13)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      32.441
_cell_measurement_theta_min      2.629
_cell_volume                     944.4(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'ShelXle (Hubshcle, 2011)'
_computing_publication_material  'ShelXle (Hubshcle, 2011)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14274
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        32.555
_diffrn_reflns_theta_max         32.557
_diffrn_reflns_theta_min         2.628
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    25.048
_exptl_absorpt_correction_T_max  0.103386
_exptl_absorpt_correction_T_min  0.037927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1110 before and 0.0366 after correction for twin component 
1 and 0.1099 before and 0.0387 after correction for twin component 2.
The Ratio of minimum to maximum transmission is 0.36685.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.839
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.514
_refine_diff_density_min         -2.360
_refine_diff_density_rms         0.261
_refine_ls_abs_structure_details
;
 Flack x determined using 1392 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(3)
_refine_ls_extinction_coef       0.00062(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         14274
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0379P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0704
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                13452
_reflns_number_total             14274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02931_si_003.cif
_cod_data_source_block           twin5a
_cod_database_code               4345401
_shelx_estimated_absorpt_t_min   0.188
_shelx_estimated_absorpt_t_max   0.634
_shelxl_version_number           2014/6
_shelx_res_checksum              20165
_shelx_hkl_checksum              25856