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_4512382
_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         '2(C8 H15 N2), Cl4 O2 U'
_chemical_formula_sum            'C16 H30 Cl4 N4 O2 U'
_chemical_formula_weight         690.27
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                73.850(7)
_cell_angle_beta                 68.900(6)
_cell_angle_gamma                64.912(7)
_cell_formula_units_Z            1
_cell_length_a                   8.9048(6)
_cell_length_b                   8.9663(8)
_cell_length_c                   9.0618(6)
_cell_measurement_reflns_used    3180
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.9740
_cell_measurement_theta_min      4.6010
_cell_volume                     604.55(9)
_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      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.5542
_diffrn_measurement_details
;
  1 omega   34.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8579 -178.0000 -150.0000 64

  2 omega  -19.00    7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -99.0000 -180.0000 26

  3 omega  -81.00   18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -57.0000 -150.0000 99

  4 omega  -25.00    0.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6392  -77.0000    0.0000 25

  5 omega  -26.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.6392   77.0000  -30.0000 93
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0179359000
_diffrn_orient_matrix_UB_12      -0.0755181000
_diffrn_orient_matrix_UB_13      -0.0250330000
_diffrn_orient_matrix_UB_21      -0.0670707000
_diffrn_orient_matrix_UB_22      0.0412084000
_diffrn_orient_matrix_UB_23      -0.0381384000
_diffrn_orient_matrix_UB_31      0.0597024000
_diffrn_orient_matrix_UB_32      0.0200203000
_diffrn_orient_matrix_UB_33      -0.0715300000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4461
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.920
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.172
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23017
_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    1.896
_exptl_crystal_description
;
;
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.724
_refine_diff_density_min         -1.528
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0239P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2365
_reflns_number_total             2368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501277d_si_002.cif
_cod_data_source_block           3TG-180K
_cod_depositor_comments
'Adding full bibliography for 4512377--4512386.cif.'
_cod_database_code               4512382
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C16H30N4U1O2Cl4
_shelx_estimated_absorpt_t_max   0.413
_shelx_estimated_absorpt_t_min   0.328
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6A(0.036) H6B(0.036) H5A(0.035) H5B(0.035) H4(0.039) H3(0.04)
 H4A(0.055) H4B(0.055) H4C(0.055) H7A(0.039) H7B(0.039) H1(0.03) H8A(0.065)
 H8B(0.065) H8C(0.065)
 Fixed X: H6A(0.0265) H6B(0.0467) H5A(0.3436) H5B(0.3362) H4(0.2894)
 H3(0.2583) H4A(0.3173) H4B(0.2041) H4C(0.1128) H7A(-0.0158) H7B(0.1438)
 H1(0.236) H8A(0.3388) H8B(0.2045) H8C(0.1855) U1(0.5)
 Fixed Y: H6A(0.1186) H6B(0.2464) H5A(0.1374) H5B(-0.012) H4(0.0455) H3(0.287)
 H4A(0.5853) H4B(0.6594) H4C(0.6309) H7A(0.0345) H7B(-0.1053) H1(0.4377) H8A(-
 0.0278) H8B(-0.0591) H8C(0.127) U1(0.5)
 Fixed Z: H6A(0.5172) H6B(0.5949) H5A(0.4993) H5B(0.4415) H4(0.1585) H3(-
 0.0562) H4A(-0.0716) H4B(0.0921) H4C(-0.0154) H7A(0.7967) H7B(0.7003)
 H1(0.3275) H8A(0.7476) H8B(0.9155) H8C(0.8281) U1(0.5)
;