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_4127307
_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, U O2, C H2 Cl2'
_chemical_formula_sum            'C57 H58 Cl2 N6 O2 U'
_chemical_formula_weight         1168.02
_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                84.014(5)
_cell_angle_beta                 79.109(5)
_cell_angle_gamma                77.062(4)
_cell_formula_units_Z            2
_cell_length_a                   13.264(2)
_cell_length_b                   13.7607(16)
_cell_length_c                   15.981(2)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      2.23
_cell_volume                     2785.8(6)
_computing_cell_refinement       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_collection       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_reduction        'Apex II release 2010, Bruker AXS, Inc.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'SHELXL-2016/6, Sheldrick, G. M.'
_computing_structure_refinement  'Shelxl-2016/6, Sheldrick, G. M.'
_computing_structure_solution
;

Sheldrick, G. M. (2015).  SHELXT.  Acta Cryst. A71, 3-8.

;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'Nonius Kappa CCD with Bruker Apex II detector'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0788
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46392
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.690
_diffrn_reflns_theta_min         2.140
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    3.053
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS. G. M. Sheldrick. Apex II release 2010, Bruker AXS, Inc.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.670
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         17103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14510
_reflns_number_total             17103
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09123_si_008.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        2785.9(7)
_cod_database_code               4127307
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.493
_shelx_estimated_absorpt_t_max   0.711
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              33281
_shelx_hkl_checksum              54500
_shelx_fab_checksum              17149