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_4512381
_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      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                73.820(4)
_cell_angle_beta                 66.506(5)
_cell_angle_gamma                71.928(4)
_cell_formula_units_Z            1
_cell_length_a                   8.8731(4)
_cell_length_b                   8.9844(4)
_cell_length_c                   9.2813(5)
_cell_measurement_reflns_used    5569
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      26.0270
_cell_measurement_theta_min      4.7190
_cell_volume                     634.81(6)
_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 0.9985
_diffrn_measured_fraction_theta_max 0.8213
_diffrn_measurement_details
;
  1 omega  -10.00   77.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0503   57.0000 -180.0000 87

  2 omega  -62.00   38.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0503  -57.0000   30.0000 100

  3 omega   -6.00   20.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0503   38.0000 -120.0000 26

  4 omega  -78.00   14.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2847  -77.0000  -90.0000 92

  5 omega   -4.00   54.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0503  -99.0000   90.0000 58

  6 omega  -18.00   86.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0503   57.0000    0.0000 104

  7 omega   57.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       12.0503  178.0000   90.0000 45

  8 omega  -39.00   64.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2847   38.0000  -90.0000 103

  9 omega -102.00  -35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.2847 -178.0000   60.0000 67
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0706122000
_diffrn_orient_matrix_UB_12      0.0202421000
_diffrn_orient_matrix_UB_13      -0.0252402000
_diffrn_orient_matrix_UB_21      0.0548548000
_diffrn_orient_matrix_UB_22      0.0000504000
_diffrn_orient_matrix_UB_23      -0.0803023000
_diffrn_orient_matrix_UB_31      0.0034255000
_diffrn_orient_matrix_UB_32      -0.0819248000
_diffrn_orient_matrix_UB_33      0.0092191000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0232
_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       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10162
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         25.991
_diffrn_reflns_theta_min         3.031
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.830
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49084
_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    1.806
_exptl_crystal_description
;
;
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.327
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2492
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0451P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2490
_reflns_number_total             2492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501277d_si_002.cif
_cod_data_source_block           3TG
_cod_depositor_comments
'Adding full bibliography for 4512377--4512386.cif.'
_cod_original_cell_volume        634.82(6)
_cod_database_code               4512381
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C1 H1 O1 N1 Cl1 U1'
_shelx_estimated_absorpt_t_max   0.548
_shelx_estimated_absorpt_t_min   0.342
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.095) H2(0.12) H3(0.111) H4A(0.205) H4B(0.205) H4C(0.205)
 H5A(0.252) H5B(0.252) H6A(0.212) H6B(0.212) H7A(0.184) H7B(0.184) H8A(0.284)
 H8B(0.284) H8C(0.284)
 Fixed X: U1(0.5) H1(0.1986) H2(0.2704) H3(0.2886) H4A(0.2583) H4B(0.3191)
 H4C(0.1259) H5A(0.3422) H5B(0.3444) H6A(0.0483) H6B(0.0475) H7A(0.1837)
 H7B(0.0325) H8A(0.2251) H8B(0.2113) H8C(0.359)
 Fixed Y: U1(0.5) H1(0.3355) H2(0.1723) H3(-0.0508) H4A(0.082) H4B(-0.0759)
 H4C(0.0011) H5A(0.5061) H5B(0.4444) H6A(0.5854) H6B(0.5191) H7A(0.7051)
 H7B(0.7991) H8A(0.8451) H8B(0.9304) H8C(0.7824)
 Fixed Z: U1(0) H1(0.9411) H2(0.561) H3(0.776) H4A(1.1252) H4B(1.0571)
 H4C(1.1236) H5A(0.6454) H5B(0.5006) H6A(0.7289) H6B(0.5889) H7A(0.3957)
 H7B(0.516) H8A(0.5919) H8B(0.424) H8C(0.4376)
;