Interaction of In(I) and Tl(I) Cations with 2,6-Diaryl Pyridine Ligands: Cation Encapsulation within a Very Weakly Interacting N/Arene Host Environment
Hassanatu B. Mansaray; Christina Y. Tang; Dragoslav Vidovic; Amber L. Thompson; Simon Aldridge; Inorganic Chemistry 51 (2012) 13017–13022; doi:10.1021/ic3021386

data_4331224
_publ_contact_author             'Simon Aldridge'
_publ_contact_author_email       simon.aldridge@chem.ox.ac.uk
_publ_section_title
;
 Interaction of In(I) and Tl(I) Cations with 2,6-Diaryl Pyridine Ligands:
 Cation Encapsulation within a Very Weakly Interacting N/Arene Host
 Environment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13017
_journal_page_last               13022
_journal_paper_doi               10.1021/ic3021386
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C32 H12 B F24, C23 H25 N Tl, 2(C6 H5 F)'
_chemical_formula_sum            'C67 H47 B F26 N Tl'
_chemical_formula_weight         1575.24
_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
_audit_creation_date             10-12-22
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                90
_cell_angle_beta                 91.5709(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8413(1)
_cell_length_b                   13.8219(1)
_cell_length_c                   35.7025(4)
_cell_measurement_reflns_used    14012
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     6334.50(10)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            53209
_diffrn_reflns_theta_full        26.929
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         5.108
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.669
_exptl_absorpt_correction_T_max  0.51
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.79
_refine_diff_density_min         -1.54
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9355
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1105
_refine_ls_number_reflns         14327
_refine_ls_number_restraints     1476
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.0298136
_refine_ls_shift/su_mean         0.0013679
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 18.1 26.4 12.6 3.16 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2159
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.2159
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              46
_reflns_limit_l_min              0
_reflns_number_gt                9924
_reflns_number_total             14330
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.07
_oxford_diffrn_Wilson_scale      81.47
_oxford_refine_ls_r_factor_ref   0.1062
_oxford_refine_ls_scale          0.13574(7)
_oxford_reflns_number_all        14327
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 020HMCT10
_cod_data_source_file            ic3021386_si_001_2.cif
_cod_data_source_block           1
_cod_original_cell_volume        6334.5(1)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C67 H47 B1 F26 N1 Tl1'
_cod_database_code               4331224