UO22±Mediated Ring Contraction of Pyrihexaphyrin: Synthesis of a Contracted Expanded Porphyrin-Uranyl Complex
Brewster II, James T.; Root, Harrison Duane; Mangel, Daniel; Zafar, Hadiqa; Samia, Adam; Sedgwick, Adam C.; Lynch, Vincent; Sessler, Jonathan L.; Chemical Science  (2019) –; doi:10.1039/C9SC01593K

data_1550957
_publ_section_title
;
 UO22+-Mediated Ring Contraction of Pyrihexaphyrin: Synthesis of a
 Contracted Expanded Porphyrin-Uranyl Complex
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01593K
_journal_year                    2019
_chemical_formula_moiety         'C42 H46 N6, U O2, 2 C H Cl3'
_chemical_formula_sum            'C44 H48 Cl6 N6 O2 U'
_chemical_formula_weight         1143.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2019-01-28 deposited with the CCDC.    2019-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.580(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4660(3)
_cell_length_b                   14.7143(4)
_cell_length_c                   27.0626(5)
_cell_measurement_reflns_used    10669
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.30
_cell_volume                     4488.22(19)
_computing_cell_refinement
'CrysAlisPro V 1.171.39.46, Agilent Technologies'
_computing_data_collection
'CrysAlisPro V 1.171.39.46, Agilent Technologies'
_computing_data_reduction
'CrysAlisPro V 1.171.39.46, Agilent Technologies'
_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 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Agilent SuperNova with Atlas S2 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            25019
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.501
_diffrn_reflns_theta_min         3.323
_diffrn_source                   'micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    13.820
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.243
_exptl_absorpt_correction_type   'Gaussian and multi-scan'
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'dark red'
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_description       needle
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.066
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         8194
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0575P)^2^+8.1029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6846
_reflns_number_total             8194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01593k2.cif
_cod_data_source_block           shelx
_cod_database_code               1550957
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.216
_shelx_estimated_absorpt_t_max   0.682
_shelx_res_checksum              47743