In-Plane Thorium(IV), Uranium(IV), and Neptunium(IV) Expanded Porphyrin Complexes.
Brewster, 2nd, James T; Mangel, Daniel N.; Gaunt, Andrew J.; Saunders, Douglas P.; Zafar, Hadiqa; Lynch, Vincent M.; Boreen, Michael A.; Garner, Mary E.; Goodwin, Conrad A. P.; Settineri, Nicholas S.; Arnold, John; Sessler, Jonathan L.; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b09123

data_4127304
_publ_section_title
;
 In-Plane Thorium(IV), Uranium(IV), and Neptunium(IV) Expanded Porphyrin
 Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b09123
_journal_year                    2019
_chemical_formula_moiety
'C56 H56 N6, 2 C3 H9 Si O, Np, C7 H8, 1/2 C6 H14'
_chemical_formula_sum            'C72 H89 N6 Np O2 Si2'
_chemical_formula_weight         1363.67
_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-2016/6
_cell_angle_alpha                87.590(4)
_cell_angle_beta                 81.979(5)
_cell_angle_gamma                75.384(5)
_cell_formula_units_Z            2
_cell_length_a                   11.3443(8)
_cell_length_b                   16.9737(7)
_cell_length_c                   17.8448(12)
_cell_measurement_reflns_used    3201
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      1.83
_cell_volume                     3292.3(4)
_computing_cell_refinement
'CrysAlisPro V 1.171.40.37a, Rigaku Oxford Diffraction'
_computing_data_reduction
'CrysAlisPro V 1.171.40.37a, Rigaku Oxford Diffraction'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution
'SHELXT. Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8.'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'SAXI-CrysAlisPro-abstract goniometer'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1559
_diffrn_reflns_av_unetI/netI     0.2314
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32793
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.149
_diffrn_source                   'sealed fine focus tube'
_exptl_absorpt_coefficient_mu    1.664
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   'analytical and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       needle
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.599
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         11804
_refine_ls_number_restraints     1708
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.1517
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6629
_reflns_number_total             11804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09123_si_007.cif
_cod_data_source_block           shelx
_cod_database_code               4127304
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.445
_shelx_estimated_absorpt_t_max   0.933
_shelx_res_checksum              76925
_shelx_hkl_checksum              95017