Supercritical synthesis and topological analysis of K5U5O17(OH)
Felder, Justin B.; Smith, Mark D.; zur Loye, Hans-Conrad; CrystEngComm  (2017) –; doi:10.1039/C7CE00746A

data_7228488
_publ_section_title
;
 Supercritical synthesis and topological analysis of K5U5O17(OH)
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00746A
_journal_year                    2017
_chemical_formula_moiety         'H K5 O18 U5'
_chemical_formula_sum            'H K5 O18 U5'
_chemical_formula_weight         1674.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-13 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.8270(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.9926(2)
_cell_length_b                   20.0065(5)
_cell_length_c                   7.0055(2)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    303(2)
_cell_measurement_theta_max      35.114
_cell_measurement_theta_min      3.091
_cell_volume                     921.96(4)
_computing_cell_refinement       'SAINT Version 8.34a (Bruker, 2014)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT Version 8.34a (Bruker, 2014)'
_computing_molecular_graphics    various
_computing_publication_material  various
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      303(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_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            33455
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        35.155
_diffrn_reflns_theta_max         35.157
_diffrn_reflns_theta_min         3.091
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    44.977
_exptl_absorpt_correction_T_max  0.0581
_exptl_absorpt_correction_T_min  0.0143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2014/4 (Bruker, 2014)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    6.032
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             1400
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method 'Supercritical Hydrothermal'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.616
_refine_diff_density_min         -1.465
_refine_diff_density_rms         0.309
_refine_ls_extinction_coef       0.00120(3)
_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   1.138
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         4195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+2.0314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0434
_reflns_number_gt                3815
_reflns_number_total             4195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00746a2.cif
_cod_data_source_block           jbf1201a
_cod_original_cell_volume        921.95(4)
_cod_database_code               7228488
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.094
_shelx_estimated_absorpt_t_max   0.266
_shelx_res_checksum              12314