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_4347955
_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            'C16 H16 F6 N4 O8 S2 U'
_chemical_formula_weight         808.48
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7508(5)
_cell_length_b                   18.8073(10)
_cell_length_c                   10.7623(4)
_cell_measurement_reflns_used    3982
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.3
_cell_measurement_theta_min      31.0
_cell_volume                     2378.48(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       omega-scan
_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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13794
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    7.098
_exptl_absorpt_correction_T_max  0.701
_exptl_absorpt_correction_T_min  0.533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.771
_refine_diff_density_min         -2.114
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4744
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                3857
_reflns_number_total             4744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00799_si_001.cif
_cod_data_source_block           complex_3
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               4347955