Noncovalent Interactions of Metal Cations and Arenes Probed with Thallium(I) Complexes
Titel Jurca; Ilia Korobkov; Serge I. Gorelsky; Darrin S. Richeson; Inorganic Chemistry 52 (2013) 5749–5756; doi:10.1021/ic302552v

data_4334811
_publ_section_title
;
 Noncovalent Interactions of Metal Cations and Arenes Probed with
 Thallium(I) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5749
_journal_page_last               5756
_journal_paper_doi               10.1021/ic302552v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C56.75 H67 F3 N3 O3 S Tl'
_chemical_formula_weight         1132.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 106.2800(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.1041(7)
_cell_length_b                   20.6691(5)
_cell_length_c                   19.5116(5)
_cell_measurement_reflns_used    9345
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.47
_cell_volume                     12040.9(5)
_computing_cell_refinement       'APEX II, Bruker (2009)'
_computing_data_collection       'APEX II, Bruker (2009)'
_computing_data_reduction        'XPREP, Bruker (2009)'
_computing_molecular_graphics    'SHELXTL, Bruker (2004)'
_computing_publication_material  'SHELXTL, Bruker (2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            69336
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.766
_exptl_absorpt_correction_T_max  0.6817
_exptl_absorpt_correction_T_min  0.6506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             4612
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
 Initial solution suggested two toluene solvent molecule, partially occupied and
 disordered by an inversion center over two symmetry related position each.
 The data set was treated with the Squeeze routine of PLATON
 (Spek, A.L. (1990), Acta Cryst. A46, C-34) with a refined void
 space/cell = 3624.4 Ang^3 and an electron count/cell = 402 consistent with 
 eight toluene solvent molecules/cell.  
;
_refine_diff_density_max         1.932
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         14899
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0574P)^2^+19.6788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                11814
_reflns_number_total             14899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302552v_si_002_4.cif
_cod_data_source_block           dr019sqz
_cod_database_code               4334811