Switchable π-coordination and C–H metallation in small-cavity macrocyclic uranium and thorium complexes
Arnold, Polly L.; Farnaby, Joy H.; White, Rebecca C.; Kaltsoyannis, Nikolas; Gardiner, Michael G.; Love, Jason B.; Chemical Science 5 (2014) 756–; doi:10.1039/c3sc52072b

data_1513627
_publ_section_title
;
 Switchable \p-coordination and C--H metallation in small-cavity
 macrocyclic uranium and thorium complexes
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              756
_journal_paper_doi               10.1039/c3sc52072b
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C36 H44 I N2 O U, C6 H12 O1.5'
_chemical_formula_sum            'C42 H56 I N2 O2.5 U'
_chemical_formula_weight         993.82
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.530(5)
_cell_angle_beta                 99.536(5)
_cell_angle_gamma                108.352(5)
_cell_formula_units_Z            2
_cell_length_a                   10.112(5)
_cell_length_b                   11.224(5)
_cell_length_c                   18.141(5)
_cell_measurement_reflns_used    27329
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.2931
_cell_measurement_theta_min      2.6788
_cell_volume                     1874.4(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies
 
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
 
(compiled Jul 11 2012,15:38:31)
 
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies
 
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
 
(compiled Jul 11 2012,15:38:31)
 
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies
 
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
 
(compiled Jul 11 2012,15:38:31)
 
;
_computing_molecular_graphics    'ORTEP (Farrugia, 1997)'
_computing_publication_material  Mercury
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            87370
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    5.193
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             974
_exptl_crystal_size_max          0.3004
_exptl_crystal_size_mid          0.1042
_exptl_crystal_size_min          0.0691
_refine_diff_density_max         2.953
_refine_diff_density_min         -2.637
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6851
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+25.3904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                6421
_reflns_number_total             6851
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3sc52072b.txt
_cod_data_source_block           po3006_refinalized2
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C42 H56 I N2 O2.50 U'
_cod_database_code               1513627