Isolation of Uranyl Dicyanamide Complexes from N-Donor Ionic Liquids.
Kelley, Steven P.; Rogers, Robin D.; Inorganic chemistry 54 (2015) 10323–10334; doi:10.1021/acs.inorgchem.5b01699

data_4346575
_publ_section_title
;
 Isolation of Uranyl Dicyanamide Complexes from N-Donor Ionic Liquids.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10323
_journal_page_last               10334
_journal_paper_doi               10.1021/acs.inorgchem.5b01699
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C4 H14 N6 O18 S2 U2'
_chemical_formula_weight         974.39
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.0370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9627(2)
_cell_length_b                   10.9246(3)
_cell_length_c                   10.9120(3)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      34.53
_cell_measurement_theta_min      2.64
_cell_volume                     949.23(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 1.000
_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       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46293
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.717
_diffrn_reflns_theta_min         2.638
_exptl_absorpt_coefficient_mu    17.366
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.3833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.584
_refine_diff_density_min         -2.671
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0202
_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^)+(0.0087P)^2^+3.8618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3735
_reflns_number_total             4081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01699_si_002.cif
_cod_data_source_block           (UO2(SO4)(biuret)(OH2))2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4346575
_shelx_estimated_absorpt_t_min   0.211
_shelx_estimated_absorpt_t_max   0.543
_shelxl_version_number           2013-4
_shelx_res_checksum              49250
_shelx_hkl_checksum              46569