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_4512383
_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(C6 H11 N2)'
_chemical_formula_sum            'C12 H22 Cl4 N4 O2 U'
_chemical_formula_weight         634.17
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.009(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0580(4)
_cell_length_b                   9.7278(4)
_cell_length_c                   10.4943(4)
_cell_measurement_reflns_used    5047
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.2660
_cell_measurement_theta_min      4.0430
_cell_volume                     1024.27(7)
_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 0.9982
_diffrn_measured_fraction_theta_max 0.8851
_diffrn_measurement_details
;
  1 omega  -14.00   57.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5565   38.0000 -150.0000 71

  2 omega  -70.00   47.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5565  -19.0000    0.0000 117

  3 omega   20.00   52.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5565  -99.0000 -150.0000 32

  4 omega    4.00   31.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5565  -99.0000   90.0000 27

  5 omega    7.00   80.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -       11.5565   38.0000  -30.0000 73

  6 omega  -15.00   27.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.3378  -99.0000  -30.0000 42
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0220906000
_diffrn_orient_matrix_UB_12      -0.0460699000
_diffrn_orient_matrix_UB_13      -0.0494702000
_diffrn_orient_matrix_UB_21      0.0218203000
_diffrn_orient_matrix_UB_22      0.0465975000
_diffrn_orient_matrix_UB_23      -0.0461443000
_diffrn_orient_matrix_UB_31      0.0634992000
_diffrn_orient_matrix_UB_32      -0.0319817000
_diffrn_orient_matrix_UB_33      0.0040248000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7800
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08797
_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    2.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.643
_refine_diff_density_min         -3.144
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         2012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                1787
_reflns_number_total             2012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg501277d_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4512377--4512386.cif.'
_cod_original_cell_volume        1024.28(8)
_cod_database_code               4512383
_chemical_oxdiff_formula         'C1 H1 N1 O1 Cl1 U1'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.027) H5A(0.032) H5B(0.032) H3(0.038) H4A(0.06) H4B(0.06)
 H4C(0.06) H6A(0.057) H6B(0.057) H6C(0.057) H2(0.038)
 Fixed X: U1(1) H1(0.7187) H5A(0.6601) H5B(0.7803) H3(0.3327) H4A(0.6043)
 H4B(0.4465) H4C(0.5061) H6A(0.5953) H6B(0.7483) H6C(0.7107) H2(0.4156)
 Fixed Y: U1(0.5) H1(0.7062) H5A(0.8299) H5B(0.8035) H3(0.6297) H4A(0.5335)
 H4B(0.515) H4C(0.6516) H6A(1.0238) H6B(1.039) H6C(0.996) H2(0.7655)
 Fixed Z: U1(0.5) H1(0.6135) H5A(0.289) H5B(0.3946) H3(0.5322) H4A(0.7614)
 H4B(0.7372) H4C(0.8043) H6A(0.4) H6B(0.3696) H6C(0.5098) H2(0.3542)
;