Perturbation of the O-U-O Angle in Uranyl by Coordination to a 12-Membered Macrocycle.
Pedrick, Elizabeth A.; Schultz, Jason W.; Wu, Guang; Mirica, Liviu M.; Hayton, Trevor W.; Inorganic chemistry 55 (2016) 5693–5701; doi:10.1021/acs.inorgchem.6b00799

data_4347956
_publ_section_title
;
 Perturbation of the O-U-O Angle in Uranyl by Coordination to a
 12-Membered Macrocycle.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5693
_journal_page_last               5701
_journal_paper_doi               10.1021/acs.inorgchem.6b00799
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C24 H32 F6 N4 O9.5 S2 U'
_chemical_formula_weight         944.69
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                90.59(2)
_cell_angle_beta                 100.232(19)
_cell_angle_gamma                106.377(19)
_cell_formula_units_Z            4
_cell_length_a                   12.329(12)
_cell_length_b                   16.376(16)
_cell_length_c                   16.606(15)
_cell_measurement_reflns_used    218
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.49
_cell_measurement_theta_min      62.84
_cell_volume                     3159(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_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  0.1521
_diffrn_reflns_av_sigmaI/netI    0.3503
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21773
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    5.363
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             1825
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.344
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         10655
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.2134
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                3616
_reflns_number_total             10655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00799_si_001.cif
_cod_data_source_block           complex_4
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C24 H32 F6 N4 O9.50 S2 U'
_cod_database_code               4347956