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_4512377
_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(N2 H O9 U), 2(C8 H15 N2)'
_chemical_formula_sum            'C16 H32 N8 O18 U2'
_chemical_formula_weight         1100.55
_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   mixed
_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                104.586(3)
_cell_angle_beta                 91.067(3)
_cell_angle_gamma                90.718(3)
_cell_formula_units_Z            2
_cell_length_a                   5.52386(17)
_cell_length_b                   15.9591(5)
_cell_length_c                   19.0897(7)
_cell_measurement_temperature    290(2)
_cell_volume                     1628.09(10)
_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_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.962
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14551
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.343
_diffrn_reflns_theta_min         3.306
_exptl_absorpt_coefficient_mu    10.017
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    2.245
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.621
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6379
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0280P)^2^+5.6195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4671
_reflns_number_total             6379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501277d_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4512377--4512386.cif.'
_cod_database_code               4512377
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.434
_shelx_estimated_absorpt_t_min   0.239
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.251) H2(0.251) H3(0.251) H4A(0.22) H4B(0.22) H4C(0.22)
 H5A(0.251) H5B(0.251) H6A(0.251) H6B(0.251) H7A(0.251) H7B(0.251) H8A(0.314)
 H8B(0.314) H8C(0.314) H9(0.087) H10(0.088) H11(0.101) H12A(0.174) H12B(0.174)
 H12C(0.174) H13A(0.118) H13B(0.118) H14A(0.211) H14B(0.211) H15A(0.179)
 H15B(0.179) H16A(0.272) H16B(0.272) H16C(0.272)
 Fixed X: H1(0.5096) H2(-0.0165) H3(0.1764) H4A(0.478) H4B(0.6179) H4C(0.6918)
 H5A(0.0124) H5B(0.2757) H6A(0.1804) H6B(-0.0873) H7A(0.2425) H7B(0.0798) H8A(-
 0.2548) H8B(-0.1656) H8C(-0.0723) H9(0.5653) H10(0.1311) H11(-0.0282)
 H12A(0.3993) H12B(0.1273) H12C(0.1951) H13A(0.6028) H13B(0.7049) H14A(0.5564)
 H14B(0.3) H15A(0.5306) H15B(0.3025) H16A(0.2934) H16B(0.1877) H16C(0.0649)
 Fixed Y: H1(0.3201) H2(0.2627) H3(0.1391) H4A(0.1228) H4B(0.1154) H4C(0.1875)
 H5A(0.4057) H5B(0.4415) H6A(0.4434) H6B(0.4427) H7A(0.5816) H7B(0.5747)
 H8A(0.5567) H8B(0.6504) H8C(0.6069) H9(0.8318) H10(0.6804) H11(0.6869)
 H12A(0.7807) H12B(0.7499) H12C(0.8468) H13A(0.7212) H13B(0.8062) H14A(0.8312)
 H14B(0.7987) H15A(0.9465) H15B(0.9122) H16A(0.9566) H16B(1.0149) H16C(0.9251)
 Fixed Z: H1(0.2106) H2(0.3359) H3(0.2793) H4A(0.15) H4B(0.2203) H4C(0.1818)
 H5A(0.2649) H5B(0.2811) H6A(0.4074) H6B(0.3791) H7A(0.408) H7B(0.3381)
 H8A(0.4207) H8B(0.4209) H8C(0.4811) H9(0.2626) H10(0.117) H11(0.2394)
 H12A(0.3762) H12B(0.3676) H12C(0.3722) H13A(0.0834) H13B(0.1366) H14A(0.0294)
 H14B(0.0447) H15A(0.1121) H15B(0.1443) H16A(0.0091) H16B(0.0802) H16C(0.0434)
;