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_4127303
_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 H58 N6, C4 H8 O'
_chemical_formula_sum            'C60 H66 N6 O'
_chemical_formula_weight         887.18
_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   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                92.950(5)
_cell_angle_beta                 113.741(6)
_cell_angle_gamma                93.357(4)
_cell_formula_units_Z            2
_cell_length_a                   13.5452(7)
_cell_length_b                   13.9827(6)
_cell_length_c                   14.4207(11)
_cell_measurement_reflns_used    12164
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6
_cell_measurement_theta_min      3.15
_cell_volume                     2487.4(3)
_computing_cell_refinement
'CrysAlisPro V 1.171.40.39a, Rigaku Oxford Diffraction'
_computing_data_collection
'CrysAlisPro V 1.171.40.39a, Rigaku Oxford Diffraction'
_computing_data_reduction
'CrysAlisPro V 1.171.40.39a, 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
;

SHELXT. Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8. 
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24448
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.610
_diffrn_reflns_theta_min         3.177
_diffrn_source                   'micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       lath
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         10107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0829P)^2^+0.9258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8801
_reflns_number_total             10107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09123_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4127303
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.904
_shelx_estimated_absorpt_t_max   0.976
_shelx_res_checksum              82590
_shelx_hkl_checksum              98418