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_1513626
_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_sum            'C38 H52 K N3 Si2 Th'
_chemical_formula_weight         878.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   12.232(5)
_cell_length_b                   12.893(5)
_cell_length_c                   23.252(5)
_cell_measurement_reflns_used    15916
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.5010
_cell_measurement_theta_min      3.7730
_cell_volume                     3667(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    ORTEP
_computing_publication_material  MERCURY
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    sir-92
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            28994
_diffrn_reflns_theta_full        73.45
_diffrn_reflns_theta_max         73.45
_diffrn_reflns_theta_min         3.80
_exptl_absorpt_coefficient_mu    14.978
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Numerical absorption correction based on gaussian integration over
                                                a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.1305
_exptl_crystal_size_mid          0.1069
_exptl_crystal_size_min          0.0426
_refine_diff_density_max         1.973
_refine_diff_density_min         -1.403
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1.055(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    RIDING
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         7189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+66.3051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1645
_reflns_number_gt                6871
_reflns_number_total             7189
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3sc52072b.txt
_cod_data_source_block           po3003_refinalized
_cod_database_code               1513626