Hydrothermal synthesis, structures and properties of two uranyl oxide hydroxyl hydrate phases with Co(ii) or Ni(ii) ions
Zhang, Yingjie; Čejka, Jiří; Lumpkin, Gregory R.; Tran, Toan Trong; Aharonovich, Igor; Karatchevtseva, Inna; Price, Jason R.; Scales, Nicholas; Lu, Kim; New J. Chem. 40 (2016) 5357–; doi:10.1039/C5NJ03055B

data_7055481
_publ_section_title
;
 Hydrothermal synthesis, structures and properties of two uranyl oxide
 hydroxyl hydrate phases with Co(ii) or Ni(ii) ions
;
_journal_issue                   6
_journal_name_full               'New J. Chem.'
_journal_page_first              5357
_journal_paper_doi               10.1039/C5NJ03055B
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'Co2 K7 O112 U24'
_chemical_formula_sum            'Co2 K7 O112 U24'
_chemical_formula_weight         7896.28
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_audit_creation_date             2016-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-22 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   14.054(2)
_cell_length_b                   14.054(2)
_cell_length_c                   14.669(3)
_cell_measurement_reflns_used    9000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      1.80
_cell_volume                     2509.2(7)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BLU-ICE (McPhillips et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            'ADSC Quantum 210r'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7294
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45862
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.971
_diffrn_reflns_theta_min         1.717
_diffrn_source                   'Synchrotron BM'
_exptl_absorpt_coefficient_mu    18.379
_exptl_absorpt_correction_T_max  0.4325
_exptl_absorpt_correction_T_min  0.3529
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    5.226
_exptl_crystal_description       prism
_exptl_crystal_F_000             3291
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.054
_refine_diff_density_min         -1.985
_refine_diff_density_rms         0.376
_refine_ls_abs_structure_details
;
 Flack x determined using 2133 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.098(9)
_refine_ls_extinction_coef       0.00063(6)
_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   1.130
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         4460
_refine_ls_number_restraints     460
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0265P)^2^+43.0179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                4411
_reflns_number_total             4460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03055b2.cif
_cod_data_source_block           p-31c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055481--7055482.cif.
;
_cod_original_cell_volume        2509.2(9)
_cod_database_code               7055481
_exptl_absorpt_special_details   'SADABS (Sheldrick, 2012)'
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(O1)
Uanis(O1W) = Uanis(O3W) = Uanis(O4W)
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: K2(0.16667)
;
_shelx_res_checksum              70827
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'