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_4127302
_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, 2 Cl'
_chemical_formula_sum            'C56 H56 Cl2 N6 U'
_chemical_formula_weight         1121.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 103.6230(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.26444(13)
_cell_length_b                   28.6778(2)
_cell_length_c                   27.8019(2)
_cell_measurement_reflns_used    74123
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.1
_cell_measurement_theta_min      3.43
_cell_volume                     11053.04(16)
_computing_cell_refinement
'CrysAlisPro V 1.171.40.37a, Rigaku Oxford Diffraction'
_computing_data_collection
'CrysAlisPro V 1.171.40.37a, Rigaku Oxford Diffraction'
_computing_data_reduction
'CrysAlisPro V 1.171.40.37a, 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
;

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 0.999
_diffrn_measurement_device_type  'ROD, Synergy Custon DW system, Pilatus 200K'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            111149
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         3.082
_diffrn_source                   'sealed microfocus tube'
_exptl_absorpt_coefficient_mu    9.452
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.334
_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            black
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       needle
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.034
_refine_diff_density_max         3.345
_refine_diff_density_min         -1.642
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         20220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+135.1412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19479
_reflns_number_total             20220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09123_si_006.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        11053.06(17)
_cod_database_code               4127302
_shelx_shelxl_version_number     2016/6
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              96191
_shelx_hkl_checksum              26400
_shelx_fab_checksum              91444