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_4512378
_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         'C5 N5 O2 S5 U, 3(C8 H15 N2)'
_chemical_formula_sum            'C29 H45 N11 O2 S5 U'
_chemical_formula_weight         978.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.211(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7336(7)
_cell_length_b                   17.8778(7)
_cell_length_c                   14.9349(8)
_cell_measurement_reflns_used    9743
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      26.4400
_cell_measurement_theta_min      3.3640
_cell_volume                     4192.8(4)
_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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 10.4713
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.8971
_diffrn_measurement_details
;
  1 omega  -15.00   81.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2066   57.0000  -90.0000 96

  2 omega  -58.00   31.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2066  -57.0000  120.0000 89

  3 omega   62.00   88.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2066  178.0000 -180.0000 26

  4 omega  -17.00   60.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2066   57.0000   90.0000 77

  5 omega -101.00  -32.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.4410  178.0000 -180.0000 69
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0072843000
_diffrn_orient_matrix_UB_12      -0.0311767000
_diffrn_orient_matrix_UB_13      0.0255082000
_diffrn_orient_matrix_UB_21      -0.0301911000
_diffrn_orient_matrix_UB_22      0.0211153000
_diffrn_orient_matrix_UB_23      0.0130070000
_diffrn_orient_matrix_UB_31      -0.0328123000
_diffrn_orient_matrix_UB_32      -0.0124726000
_diffrn_orient_matrix_UB_33      -0.0417385000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34723
_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         26.372
_diffrn_reflns_theta_min         3.122
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41603
_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    1.549
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.185
_refine_diff_density_min         -1.578
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8566
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+4.7935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5879
_reflns_number_total             8566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501277d_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4512377--4512386.cif.'
_cod_original_cell_volume        4192.8(3)
_cod_database_code               4512378
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C1 H1 N1 O1 S1'
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.490
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H6(0.15) H7(0.119) H8(0.121) H9A(0.314) H9B(0.314) H9C(0.314)
 H10A(0.243) H10B(0.243) H11A(0.306) H11B(0.306) H12A(0.318) H12B(0.318)
 H13A(0.326) H13B(0.326) H13C(0.326) H14(0.148) H15(0.131) H16(0.114)
 H17A(0.213) H17B(0.213) H17C(0.213) H18A(0.247) H18B(0.247) H19A(0.195)
 H19B(0.195) H20A(0.279) H20B(0.279) H21A(0.185) H21B(0.185) H21C(0.185)
 H22(0.091) H23(0.101) H24(0.108) H25A(0.185) H25B(0.185) H25C(0.185)
 H26A(0.12) H26B(0.12) H27A(0.12) H27B(0.12) H28A(0.171) H28B(0.171) H29A(0.39)
 H29B(0.39) H29C(0.39)
 Fixed X: H6(0.8412) H7(1.0871) H8(1.0661) H9A(0.9299) H9B(0.9815) H9C(0.8821)
 H10A(0.8329) H10B(0.9193) H11A(0.862) H11B(0.9507) H12A(0.8395) H12B(0.8804)
 H13A(0.7333) H13B(0.7282) H13C(0.7733) H14(0.6657) H15(0.4535) H16(0.4346)
 H17A(0.5956) H17B(0.5199) H17C(0.6145) H18A(0.577) H18B(0.6516) H19A(0.6409)
 H19B(0.7087) H20A(0.789) H20B(0.7678) H21A(0.6824) H21B(0.6381) H21C(0.7251)
 H22(0.28) H23(0.4753) H24(0.3561) H25A(0.3994) H25B(0.4796) H25C(0.4713)
 H26A(0.214) H26B(0.1697) H27A(0.1998) H27B(0.1507) H28A(0.0914) H28B(0.0394)
 H29A(-0.0203) H29B(0.0688) H29C(0.0437)
 Fixed Y: H6(0.7744) H7(0.8079) H8(0.6768) H9A(0.8988) H9B(0.9259) H9C(0.9072)
 H10A(0.6507) H10B(0.6161) H11A(0.5978) H11B(0.5658) H12A(0.5037) H12B(0.4616)
 H13A(0.557) H13B(0.4677) H13C(0.5138) H14(0.7787) H15(0.6755) H16(0.8072)
 H17A(0.9091) H17B(0.9268) H17C(0.9138) H18A(0.5981) H18B(0.6508) H19A(0.5825)
 H19B(0.6462) H20A(0.5652) H20B(0.5161) H21A(0.5102) H21B(0.4772) H21C(0.4416)
 H22(0.8545) H23(0.7301) H24(0.647) H25A(0.9239) H25B(0.8756) H25C(0.9006)
 H26A(0.6882) H26B(0.7592) H27A(0.6243) H27B(0.6951) H28A(0.624) H28B(0.6819)
 H29A(0.5739) H29B(0.5304) H29C(0.5854)
 Fixed Z: H6(0.4093) H7(0.4782) H8(0.506) H9A(0.3372) H9B(0.4437) H9C(0.4128)
 H10A(0.4643) H10B(0.5371) H11A(0.3345) H11B(0.405) H12A(0.4723) H12B(0.4028)
 H13A(0.3359) H13B(0.3288) H13C(0.2675) H14(0.5946) H15(0.5834) H16(0.6042)
 H17A(0.6847) H17B(0.5869) H17C(0.5869) H18A(0.5298) H18B(0.5223) H19A(0.683)
 H19B(0.6876) H20A(0.6239) H20B(0.7032) H21A(0.5021) H21B(0.5729) H21C(0.5707)
 H22(0.3301) H23(0.325) H24(0.3178) H25A(0.2948) H25B(0.2939) H25C(0.3932)
 H26A(0.38) H26B(0.3179) H27A(0.2414) H27B(0.1814) H28A(0.3176) H28B(0.2372)
 H29A(0.1819) H29B(0.2145) H29C(0.1245)
;