Uranyl Coordination by the 14-Membered Macrocycle Dibenzotetramethyltetraaza[14]annulene.
Pedrick, Elizabeth A.; Assefa, Mikiyas K.; Wakefield, Megan E.; Wu, Guang; Hayton, Trevor W.; Inorganic chemistry 56 (2017) 6638–6644; doi:10.1021/acs.inorgchem.7b00700

data_4345905
_publ_section_title
;
 Uranyl Coordination by the 14-Membered Macrocycle
 Dibenzotetramethyltetraaza[14]annulene.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6638
_journal_page_last               6644
_journal_paper_doi               10.1021/acs.inorgchem.7b00700
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C54 H74 D12 Li2 N6 O4 Si4 U'
_chemical_formula_weight         1259.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.608(14)
_cell_length_b                   19.504(12)
_cell_length_c                   12.206(7)
_cell_measurement_reflns_used    572
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.75
_cell_measurement_theta_min      2.05
_cell_volume                     5858(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2992
_diffrn_reflns_av_unetI/netI     0.2117
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32934
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.113
_diffrn_reflns_theta_max         25.113
_diffrn_reflns_theta_min         1.655
_exptl_absorpt_coefficient_mu    2.899
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         6.122
_refine_diff_density_min         -1.948
_refine_diff_density_rms         0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5309
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.2212
_refine_ls_R_factor_gt           0.1290
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1716P)^2^+127.1699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3079
_refine_ls_wR_factor_ref         0.3594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2791
_reflns_number_total             5309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00700_si_001.cif
_cod_data_source_block           MERGED
_cod_original_cell_volume        5859(6)
_cod_database_code               4345905
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              69910
_shelx_hkl_checksum              92376