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_4127301
_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, Th 2+, 2 Cl 1-, 2 C4 H8 O'
_chemical_formula_sum            'C64 H72 Cl2 N6 O2 Th'
_chemical_formula_weight         1260.21
_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                106.776(2)
_cell_angle_beta                 95.603(2)
_cell_angle_gamma                105.556(2)
_cell_formula_units_Z            2
_cell_length_a                   13.6652(3)
_cell_length_b                   13.9046(4)
_cell_length_c                   18.5599(4)
_cell_measurement_reflns_used    19623
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.2
_cell_measurement_theta_min      3.38
_cell_volume                     3193.67(15)
_computing_cell_refinement
'CrysAlisPro V 1.171.40_64.37a, Rigaku Oxford Diffraction'
_computing_data_collection
'CrysAlisPro V 1.171.40_64.37a, Rigaku Oxford Diffraction'
_computing_data_reduction
'CrysAlisPro V 1.171.40_64.37a, Rigaku Oxford Diffraction'
_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). Acta Cryst. A71, 3-8. SHELXT.  An Integrated Space Group 
and Crystal Structure Determination Program.  

;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Agilent SuperNova with an Atlas S2 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36500
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.561
_diffrn_reflns_theta_min         2.533
_diffrn_source                   'sealed micro-focus tube'
_exptl_absorpt_coefficient_mu    8.638
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.182
_exptl_absorpt_correction_type   'gaussian and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_description       plate
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.031
_refine_diff_density_max         2.946
_refine_diff_density_min         -1.751
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         12105
_refine_ls_number_restraints     576
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0892P)^2^+1.5676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1217
_refine_ls_wR_factor_ref         0.1272
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10948
_reflns_number_total             12105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09123_si_004.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        3193.67(14)
_cod_database_code               4127301
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.204
_shelx_estimated_absorpt_t_max   0.776
_shelx_res_checksum              84320
_shelx_hkl_checksum              74795
_shelx_fab_checksum              2381