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_4345903
_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            'C32 H49 N5 O3 Si2 U'
_chemical_formula_weight         845.97
_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                93.119(4)
_cell_angle_beta                 103.060(4)
_cell_angle_gamma                106.749(4)
_cell_formula_units_Z            4
_cell_length_a                   12.614(4)
_cell_length_b                   17.491(5)
_cell_length_c                   17.517(5)
_cell_measurement_reflns_used    757
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.125
_cell_measurement_theta_min      21.125
_cell_volume                     3575.4(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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0942
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            34368
_diffrn_reflns_theta_full        28.43
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    4.644
_exptl_absorpt_correction_T_max  0.493
_exptl_absorpt_correction_T_min  0.303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.014
_refine_diff_density_min         -2.262
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         17762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0616P)^2^+5.3269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                11513
_reflns_number_total             17762
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7b00700_si_001.cif
_cod_data_source_block           complex_1
_cod_original_cell_volume        3575.5(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4345903