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_1513623
_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 Cl2 N2 Th'
_chemical_formula_sum            'C32 H36 Cl2 N2 Th'
_chemical_formula_weight         751.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 91.134(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1650(2)
_cell_length_b                   15.5150(4)
_cell_length_c                   18.2424(4)
_cell_measurement_reflns_used    10980
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.4241
_cell_measurement_theta_min      3.2423
_cell_volume                     2876.44(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    ORTEP
_computing_publication_material  MERCURY
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 16.1042
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34644
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    5.394
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
                                                model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.4563
_exptl_crystal_size_mid          0.2770
_exptl_crystal_size_min          0.2067
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    RIDING
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         6582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0075P)^2^+3.4266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0374
_refine_ls_wR_factor_ref         0.0389
_reflns_number_gt                5907
_reflns_number_total             6582
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3sc52072b.txt
_cod_data_source_block           p12014c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'ANALYTICAL' changed to
'analytical' according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2876.45(11)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               1513623