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_1513629
_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         'C32 H36 I4 N2 U2'
_chemical_formula_sum            'C32 H36 I4 N2 U2'
_chemical_formula_weight         1432.29
_chemical_name_common            U2I4L
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.0498(7)
_cell_length_b                   11.5475(2)
_cell_length_c                   10.1812(2)
_cell_measurement_reflns_used    10731
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.4235
_cell_measurement_theta_min      2.9667
_cell_volume                     3650.44(13)
_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      170(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            38038
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.606
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.3613
_exptl_crystal_size_mid          0.2657
_exptl_crystal_size_min          0.1180
_refine_diff_density_max         2.867
_refine_diff_density_min         -1.611
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         4380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+35.6295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                3924
_reflns_number_total             4380
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3sc52072b.txt
_cod_data_source_block           p12140
_cod_database_code               1513629