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_4345904
_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            'C44 H46 N8 O2 U'
_chemical_formula_weight         956.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                91.799(15)
_cell_angle_beta                 94.571(15)
_cell_angle_gamma                90.844(15)
_cell_formula_units_Z            1
_cell_length_a                   8.538(7)
_cell_length_b                   9.684(7)
_cell_length_c                   11.786(9)
_cell_measurement_reflns_used    8057
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      1.5
_cell_volume                     970.8(13)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1286
_diffrn_reflns_av_unetI/netI     0.1923
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_number            12025
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.304
_diffrn_reflns_theta_min         1.734
_exptl_absorpt_coefficient_mu    4.229
_exptl_absorpt_correction_T_max  0.745369
_exptl_absorpt_correction_T_min  0.487483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   twinabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.938
_refine_diff_density_min         -3.120
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1083P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2960
_reflns_number_total             3860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00700_si_001.cif
_cod_data_source_block           twin4_a
_cod_database_code               4345904
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.364
_shelx_estimated_absorpt_t_max   0.485
_shelx_res_checksum              58555
_shelx_hkl_checksum              98749