Synthesis and structure of the new pentanary uranium(vi) silicate, K4CaUSi4O14, a member of a structural family related to fresnoite
Morrison, Gregory; Smith, Mark D.; Tran, T. Thao; Halasyamani, P. Shiv; zur Loye, Hans-Conrad; CrystEngComm 17 (2015) 4218–; doi:10.1039/C5CE00504C

data_7220451
_publ_section_title
;
 Synthesis and structure of the new pentanary uranium(vi) silicate,
 K4CaUSi4O14, a member of a structural family related to fresnoite
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4218
_journal_paper_doi               10.1039/C5CE00504C
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'Ca K4 O14 Si4 U'
_chemical_formula_sum            'Ca K4 O14 Si4 U'
_chemical_formula_weight         770.87
_space_group_crystal_system      tetragonal
_space_group_IT_number           118
_space_group_name_Hall           'P -4 -2n'
_space_group_name_H-M_alt        'P -4 n 2'
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 2'
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.2862(2)
_cell_length_b                   9.2862(2)
_cell_length_c                   8.3796(4)
_cell_measurement_reflns_used    7120
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      34.656
_cell_measurement_theta_min      3.102
_cell_volume                     722.60(4)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
_computing_publication_material  various
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16843
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        35.050
_diffrn_reflns_theta_max         35.050
_diffrn_reflns_theta_min         3.102
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    13.143
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.543
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.707
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.208
_refine_ls_abs_structure_details
; 
 Flack x determined using 564 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.006(5)
_refine_ls_extinction_coef       0.0248(14)
_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   1.066
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0300P)^2^+1.6364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.771
_reflns_friedel_fraction_full    0.990
_reflns_friedel_fraction_max     0.990
_reflns_number_gt                1407
_reflns_number_total             1601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00504c2.cif
_cod_data_source_block           p-4n2
_cod_depositor_comments          'Adding full bibliography for 7220451.cif.'
_cod_original_cell_volume        722.60(5)
_cod_database_code               7220451
_shelx_estimated_absorpt_t_min   0.302
_shelx_estimated_absorpt_t_max   0.506
_shelxl_version_number           2014/6
_shelx_res_checksum              97282
_shelx_hkl_checksum              63792