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_4346574
_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            'C17 H21 N7 O9 U2'
_chemical_formula_weight         943.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                102.123(5)
_cell_angle_beta                 96.577(6)
_cell_angle_gamma                103.460(5)
_cell_formula_units_Z            2
_cell_length_a                   10.0087(8)
_cell_length_b                   10.6432(8)
_cell_length_c                   12.4241(10)
_cell_measurement_reflns_used    2921
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      2.31
_cell_volume                     1239.69(18)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.970
_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  0.0769
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16262
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.584
_diffrn_reflns_theta_min         2.029
_exptl_absorpt_coefficient_mu    13.106
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXScale'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.606
_refine_diff_density_min         -1.824
_refine_diff_density_rms         0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0214P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3060
_reflns_number_total             4509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01699_si_002.cif
_cod_data_source_block
'[(C2CN)(C4CN)Im]2n[{(UO2)4(O)2(OAc)4(N(CN)2)2}n]'
_cod_original_cell_volume        1239.69(17)
_cod_database_code               4346574
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.461
_shelx_estimated_absorpt_t_max   0.695
_shelx_res_checksum              99354
_shelx_hkl_checksum              82423