Crystallization in Ionic Liquids: Synthesis, Properties, and Polymorphs of Uranyl Salts
Qu, Feng; Zhu, Qian-Qian; Liu, Chun-Li; Crystal Growth & Design 14 (2014) 6421–; doi:10.1021/cg501277d

data_4512379
_publ_section_title
;
 Crystallization in Ionic Liquids: Synthesis, Properties, and Polymorphs
 of Uranyl Salts
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6421
_journal_paper_doi               10.1021/cg501277d
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'Cl4 O2 U, 2(C8 H15 N2)'
_chemical_formula_sum            'C16 H30 Cl4 N4 O2 U'
_chemical_formula_weight         690.27
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.449(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5341(5)
_cell_length_b                   17.5319(10)
_cell_length_c                   8.8715(6)
_cell_measurement_reflns_used    3545
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      26.6060
_cell_measurement_theta_min      4.0340
_cell_volume                     1273.02(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 10.4713
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.8863
_diffrn_measurement_details
;
  1 omega   -8.00   81.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2066   57.0000 -180.0000 89

  2 omega  -56.00   42.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2066  -57.0000   30.0000 98

  3 omega  -21.00   73.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2066   77.0000    0.0000 94

  4 omega  -74.00   -1.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.4410  132.0000  125.0000 73
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0291531000
_diffrn_orient_matrix_UB_12      0.0000451000
_diffrn_orient_matrix_UB_13      0.0832298000
_diffrn_orient_matrix_UB_21      0.0025323000
_diffrn_orient_matrix_UB_22      -0.0404263000
_diffrn_orient_matrix_UB_23      -0.0000656000
_diffrn_orient_matrix_UB_31      0.0816444000
_diffrn_orient_matrix_UB_32      0.0012276000
_diffrn_orient_matrix_UB_33      -0.0045413000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10281
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.013
_diffrn_reflns_theta_min         3.147
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_description
;
;
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.2749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1835
_reflns_number_total             2505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501277d_si_002.cif
_cod_data_source_block           3TT
_cod_depositor_comments
'Adding full bibliography for 4512377--4512386.cif.'
_cod_database_code               4512379
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cl1 U1'
_shelx_estimated_absorpt_t_max   0.549
_shelx_estimated_absorpt_t_min   0.343
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.079) H2(0.092) H3(0.099) H4A(0.157) H4B(0.157) H4C(0.157)
 H5A(0.103) H5B(0.103) H6A(0.103) H6B(0.103) H7A(0.166) H7B(0.166) H8A(0.273)
 H8B(0.273) H8C(0.273)
 Fixed X: U1(1) H1(0.645) H2(0.7446) H3(0.6429) H4A(0.8424) H4B(0.6657)
 H4C(0.7999) H5A(0.4912) H5B(0.4723) H6A(0.7286) H6B(0.7625) H7A(0.5523)
 H7B(0.5265) H8A(0.7709) H8B(0.6595) H8C(0.795)
 Fixed Y: U1(0.5) H1(0.4598) H2(0.3809) H3(0.2749) H4A(0.5192) H4B(0.5491)
 H4C(0.551) H5A(0.3472) H5B(0.2748) H6A(0.2336) H6B(0.3092) H7A(0.1892)
 H7B(0.2701) H8A(0.2647) H8B(0.1971) H8C(0.1832)
 Fixed Z: U1(1) H1(0.1623) H2(0.5937) H3(0.4109) H4A(0.5557) H4B(0.4733)
 H4C(0.3838) H5A(0.0076) H5B(0.105) H6A(0.111) H6B(0.0307) H7A(-0.115) H7B(-
 0.1921) H8A(-0.2255) H8B(-0.3087) H8C(-0.15)
;