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_4334808
_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            'C41 H41.5 F3 N3 O3.25 S Tl'
_chemical_formula_weight         921.70
_chemical_name_systematic
; 
 ? 
;
_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                113.570(2)
_cell_angle_beta                 99.759(2)
_cell_angle_gamma                97.068(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5837(4)
_cell_length_b                   12.5411(4)
_cell_length_c                   15.4083(5)
_cell_measurement_reflns_used    9186
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.57
_cell_volume                     1976.33(12)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29982
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    4.194
_exptl_absorpt_correction_T_max  0.5189
_exptl_absorpt_correction_T_min  0.2540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       block
_exptl_crystal_F_000             917
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
 Initial solution suggested one cocrystallized diethyl ether solvent molecule,
 partially occupied and disordered  over two symmetry related position by an
 inversion center. 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 = 235.7 Ang^3 and an electron count/cell = 22 consistent with one
 half diethyl molecule/cell.  
;
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         9726
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0677
_reflns_number_gt                8636
_reflns_number_total             9726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302552v_si_002_1.cif
_cod_data_source_block           dr015sqz
_cod_original_cell_volume        1976.33(11)
_cod_original_formula_sum        'C41 H41.50 F3 N3 O3.25 S Tl'
_cod_database_code               4334808