Uranyl and uranyl-3d block cation complexes with 1,3-adamantanedicarboxylate: crystal structures, luminescence, and magnetic properties.
Thuéry, Pierre; Rivière, Eric; Harrowfield, Jack; Inorganic chemistry 54 (2015) 2838–2850; doi:10.1021/ic503004j

data_4342522
_publ_section_title
;
 Uranyl and uranyl-3d block cation complexes with
 1,3-adamantanedicarboxylate: crystal structures, luminescence, and
 magnetic properties.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2838
_journal_page_last               2850
_journal_paper_doi               10.1021/ic503004j
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C66 H72 N6 Ni O25 U4'
_chemical_formula_weight         2360.13
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.9388(17)
_cell_angle_beta                 97.3018(15)
_cell_angle_gamma                114.3083(16)
_cell_formula_units_Z            2
_cell_length_a                   14.0975(5)
_cell_length_b                   14.5802(3)
_cell_length_c                   20.5052(7)
_cell_measurement_reflns_used    216111
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.92
_cell_volume                     3627.7(2)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'2 \f and 14 \w scans with 2\% steps (758 frames)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            216111
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.235
_exptl_absorpt_correction_T_max  0.524
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    2.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2212
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.804
_refine_diff_density_min         -1.657
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         18707
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                15588
_reflns_number_total             18707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic503004j_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 4342516--4342524.cif.'
_cod_database_code               4342522