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_4512386
_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(C9 H17 N2), Cl4 O2 U'
_chemical_formula_sum            'C18 H34 Cl4 N4 O2 U'
_chemical_formula_weight         718.32
_chemical_name_systematic
;
 ?
;
_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             2014-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.879(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3975(2)
_cell_length_b                   13.52281(19)
_cell_length_c                   10.3966(2)
_cell_measurement_reflns_used    7839
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      29.4540
_cell_measurement_theta_min      3.7300
_cell_volume                     1303.87(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4674
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0555792000
_diffrn_orient_matrix_UB_12      0.0357955000
_diffrn_orient_matrix_UB_13      0.0195850000
_diffrn_orient_matrix_UB_21      0.0459592000
_diffrn_orient_matrix_UB_22      -0.0300812000
_diffrn_orient_matrix_UB_23      0.0587333000
_diffrn_orient_matrix_UB_31      0.0254870000
_diffrn_orient_matrix_UB_32      -0.0237615000
_diffrn_orient_matrix_UB_33      -0.0448929000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13309
_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         25.994
_diffrn_reflns_theta_min         3.729
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0174
_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^)+(0.0144P)^2^+1.3139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0376
_refine_ls_wR_factor_ref         0.0394
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2198
_reflns_number_total             2567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501277d_si_002.cif
_cod_data_source_block           6-180k
_cod_depositor_comments
'Adding full bibliography for 4512377--4512386.cif.'
_cod_database_code               4512386
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C1 H1 O1 N1 U1 Cl2'
_shelx_estimated_absorpt_t_max   0.556
_shelx_estimated_absorpt_t_min   0.350
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.034) H3(0.033) H4B(0.049) H4C(0.049) H4A(0.049) H5A(0.052)
 H5B(0.052) H5C(0.052) H6A(0.031) H6B(0.031) H7A(0.032) H7B(0.032) H8A(0.04)
 H8B(0.04) H9A(0.067) H9B(0.067) H9C(0.067)
 Fixed X: H2(0.0692) H3(0.0756) H4B(0.1766) H4C(0.2256) H4A(0.3406)
 H5A(0.4467) H5B(0.35) H5C(0.3133) H6A(0.2516) H6B(0.1413) H7A(0.4443)
 H7B(0.3375) H8A(0.3966) H8B(0.2784) H9A(0.4596) H9B(0.579) H9C(0.5003) U1(0)
 Fixed Y: H2(0.433) H3(0.2875) H4B(0.2499) H4C(0.3425) H4A(0.2866) H5A(0.5226)
 H5B(0.4871) H5C(0.5885) H6A(0.6471) H6B(0.6221) H7A(0.5799) H7B(0.5394)
 H8A(0.7442) H8B(0.7078) H9A(0.632) H9B(0.6622) H9C(0.7459) U1(0.5)
 Fixed Z: H2(0.3555) H3(0.502) H4B(0.7702) H4C(0.8775) H4A(0.8408) H5A(0.8289)
 H5B(0.9041) H5C(0.8151) H6A(0.5861) H6B(0.4222) H7A(0.5573) H7B(0.4001)
 H8A(0.4751) H8B(0.3197) H9A(0.2769) H9B(0.4349) H9C(0.3161) U1(0)
;