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_4512384
_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(C7 H13 N2)'
_chemical_formula_sum            'C14 H26 Cl4 N4 O2 U'
_chemical_formula_weight         662.22
_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             2014-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.510(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6181(5)
_cell_length_b                   9.8110(5)
_cell_length_c                   12.0087(6)
_cell_measurement_reflns_used    2445
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.0550
_cell_measurement_theta_min      3.2720
_cell_volume                     1123.46(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      180.00(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.9859
_diffrn_measured_fraction_theta_max 0.8323
_diffrn_measurement_details
;
  1 omega  -34.00   30.00   1.0000    2.9800
omega____ theta____ kappa____ phi______ frames
    -       10.8579  -57.0000   30.0000 64

  2 omega  -12.00   80.00   1.0000    2.9800
omega____ theta____ kappa____ phi______ frames
    -       10.8579   77.0000 -150.0000 92
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0266479000
_diffrn_orient_matrix_UB_12      0.0674896000
_diffrn_orient_matrix_UB_13      -0.0044490000
_diffrn_orient_matrix_UB_21      -0.0630301000
_diffrn_orient_matrix_UB_22      -0.0244161000
_diffrn_orient_matrix_UB_23      -0.0308254000
_diffrn_orient_matrix_UB_31      -0.0290785000
_diffrn_orient_matrix_UB_32      -0.0088935000
_diffrn_orient_matrix_UB_33      0.0508049000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4036
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.906
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.958
_exptl_crystal_description
;
;
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0150P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1760
_reflns_number_total             2179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501277d_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 4512377--4512386.cif.'
_cod_database_code               4512384
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C1 H1 O1 N1 U1 Cl1'
_shelx_estimated_absorpt_t_max   0.513
_shelx_estimated_absorpt_t_min   0.391
_reflns_odcompleteness_completeness 98.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.043) H3(0.041) H4A(0.056) H4B(0.056) H4C(0.056) H5A(0.051)
 H5B(0.051) H5C(0.051) H6A(0.049) H6B(0.049) H7A(0.074) H7B(0.074) H7C(0.074)
 Fixed X: U1(0) H2(0.2546) H3(0.3282) H4A(0.355) H4B(0.4344) H4C(0.5148)
 H5A(0.318) H5B(0.4757) H5C(0.433) H6A(0.3522) H6B(0.2731) H7A(0.1431)
 H7B(0.1237) H7C(0.0648)
 Fixed Y: U1(1) H2(0.3715) H3(0.5164) H4A(0.8524) H4B(0.7527) H4C(0.8107)
 H5A(0.8261) H5B(0.8246) H5C(0.7305) H6A(0.5166) H6B(0.3877) H7A(0.6429)
 H7B(0.5111) H7C(0.511)
 Fixed Z: U1(0.5) H2(0.4153) H3(0.266) H4A(0.3306) H4B(0.2544) H4C(0.3697)
 H5A(0.5868) H5B(0.5576) H5C(0.6565) H6A(0.6916) H6B(0.6311) H7A(0.6575)
 H7B(0.7324) H7C(0.6015)
;