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_4331225
_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(C7 H8)'
_chemical_formula_sum            'C69 H53 B F24 N Tl'
_chemical_formula_weight         1567.32
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             11-07-11
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                90
_cell_angle_beta                 91.6851(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8041(1)
_cell_length_b                   13.8915(2)
_cell_length_c                   35.7688(4)
_cell_measurement_reflns_used    13652
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     6359.38(13)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.980
_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  0.053
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            94242
_diffrn_reflns_theta_full        25.036
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_min         5.123
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.654
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.56
_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    1.637
_exptl_crystal_description       block
_exptl_crystal_F_000             3103.999
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         3.49
_refine_diff_density_min         -2.52
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9592
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1177
_refine_ls_number_reflns         12642
_refine_ls_number_restraints     1678
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0.0044181
_refine_ls_shift/su_mean         0.0001486
_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: 
 25.4 36.1 16.7 3.90 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2429
_refine_ls_wR_factor_gt          0.1901
_refine_ls_wR_factor_ref         0.2428
_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                7865
_reflns_number_total             14328
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.90
_oxford_diffrn_Wilson_scale      76.50
_oxford_refine_ls_r_factor_ref   0.1303
_oxford_refine_ls_scale          0.13094(7)
_oxford_reflns_number_all        12643
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 013HMCT10/6369
_cod_data_source_file            ic3021386_si_001_3.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C69 H53 B1 F24 N1 Tl1'
_cod_database_code               4331225
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, TL(1,U'S) UNTIL C(79) 
CONT C(100,U'S) UNTIL C(116) 
CONT C(120,U'S) UNTIL C(136) 
CONT F(80,U'S) UNTIL F(87) 
CONT F(90,U'S) UNTIL F(97) 
CONT F(100,U'S) UNTIL F(107) 
CONT F(110,U'S) UNTIL F(117) 
CONT F(120,U'S) UNTIL F(127) 
CONT F(130,U'S) UNTIL F(137) 
CONT F(140,U'S) UNTIL F(147) 
EQUIV PART(1001,OCC) PART(1002,OCC) 
EQUIV PART(2001,OCC) PART(2002,OCC) 
EQUIV PART(3001,OCC) PART(3002,OCC) 
EQUIV PART(3003,OCC) PART(3004,OCC) 
EQUIV PART(4001,OCC) PART(4002,OCC) 
EQUIV PART(4003,OCC) PART(4004,OCC) 
EQUIV PART(5001,OCC) PART(5002,OCC) 
EQUIV PART(5003,OCC) PART(5004,OCC) 
EQUIV PART(6001,OCC) PART(6002,OCC) 
WEIGHT -1 PART(1002,OCC) 
WEIGHT -1 PART(2002,OCC) 
WEIGHT -1 PART(3002,OCC) 
WEIGHT -1 PART(3004,OCC) 
WEIGHT -1 PART(4002,OCC) 
WEIGHT -1 PART(4004,OCC) 
WEIGHT -1 PART(5002,OCC) 
WEIGHT -1 PART(5004,OCC) 
WEIGHT -1 PART(6002,OCC) 
RIDE C(27,U'S) C(79,U'S) 
RIDE C(51,U'S) C(61,U'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 143,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 153,X'S) H   ( 152,X'S) 
RIDE C   (  16,X'S) H   ( 162,X'S) H   ( 161,X'S) H   ( 163,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 242,X'S) H   ( 243,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 253,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   ( 100,X'S) H   (1001,X'S) 
RIDE C   ( 101,X'S) H   (1011,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) H   (1063,X'S) H   (1062,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) H   (1162,X'S) H   (1163,X'S) 
RIDE C   ( 121,X'S) H   (1211,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) 
RIDE C   ( 126,X'S) H   (1262,X'S) H   (1261,X'S) H   (1263,X'S) 
RIDE C   ( 131,X'S) H   (1311,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) 
RIDE C   ( 133,X'S) H   (1331,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) 
RIDE C   ( 135,X'S) H   (1351,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) H   (1362,X'S) H   (1363,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM :CF3 
SAME C(79) F(80) F(81) F(82) AND 
CONT C(79) F(82) F(80) F(81) AND 
CONT C(79) F(81) F(82) F(80) AND 
CONT C(79) F(85) F(86) F(87) AND 
CONT C(79) F(87) F(85) F(86) AND 
CONT C(79) F(86) F(87) F(85) AND 
CONT C(51) F(90) F(91) F(92) AND 
CONT C(51) F(92) F(90) F(91) AND 
CONT C(51) F(91) F(92) F(90) AND 
CONT C(51) F(95) F(96) F(97) AND 
CONT C(51) F(97) F(95) F(96) AND 
CONT C(51) F(96) F(97) F(95) AND 
CONT C(36) F(100) F(101) F(102) AND 
CONT C(36) F(102) F(100) F(101) AND 
CONT C(36) F(101) F(102) F(100) AND 
CONT C(36) F(105) F(106) F(107) AND 
CONT C(36) F(107) F(105) F(106) AND 
CONT C(36) F(106) F(107) F(105) AND 
CONT C(75) F(110) F(111) F(112) AND 
CONT C(75) F(112) F(110) F(111) AND 
CONT C(75) F(111) F(112) F(110) AND 
CONT C(75) F(115) F(116) F(117) AND 
CONT C(75) F(117) F(115) F(116) AND 
CONT C(75) F(116) F(117) F(115) AND 
CONT C(47) F(120) F(121) F(122) AND 
CONT C(47) F(122) F(120) F(121) AND 
CONT C(47) F(121) F(122) F(120) AND 
CONT C(47) F(125) F(126) F(127) AND 
CONT C(47) F(127) F(125) F(126) AND 
CONT C(47) F(126) F(127) F(125) AND 
CONT C(61) F(130) F(131) F(132) AND 
CONT C(61) F(132) F(130) F(131) AND 
CONT C(61) F(131) F(132) F(130) AND 
CONT C(61) F(135) F(136) F(137) AND 
CONT C(61) F(137) F(135) F(136) AND 
CONT C(61) F(136) F(137) F(135) AND 
CONT C(65) F(140) F(141) F(142) AND 
CONT C(65) F(142) F(140) F(141) AND 
CONT C(65) F(141) F(142) F(140) AND 
CONT C(65) F(145) F(146) F(147) AND 
CONT C(65) F(147) F(145) F(146) AND 
CONT C(65) F(146) F(147) F(145) 
SIMU 0.01 C(79) F(80) F(81) F(82) AND 
CONT C(79) F(82) F(80) F(81) AND 
CONT C(79) F(81) F(82) F(80) AND 
CONT C(79) F(85) F(86) F(87) AND 
CONT C(79) F(87) F(85) F(86) AND 
CONT C(79) F(86) F(87) F(85) AND 
CONT C(51) F(90) F(91) F(92) AND 
CONT C(51) F(92) F(90) F(91) AND 
CONT C(51) F(91) F(92) F(90) AND 
CONT C(51) F(95) F(96) F(97) AND 
CONT C(51) F(97) F(95) F(96) AND 
CONT C(51) F(96) F(97) F(95) AND 
CONT C(36) F(100) F(101) F(102) AND 
CONT C(36) F(102) F(100) F(101) AND 
CONT C(36) F(101) F(102) F(100) AND 
CONT C(36) F(105) F(106) F(107) AND 
CONT C(36) F(107) F(105) F(106) AND 
CONT C(36) F(106) F(107) F(105) AND 
CONT C(75) F(110) F(111) F(112) AND 
CONT C(75) F(112) F(110) F(111) AND 
CONT C(75) F(111) F(112) F(110) AND 
CONT C(75) F(115) F(116) F(117) AND 
CONT C(75) F(117) F(115) F(116) AND 
CONT C(75) F(116) F(117) F(115) AND 
CONT C(47) F(120) F(121) F(122) AND 
CONT C(47) F(122) F(120) F(121) AND 
CONT C(47) F(121) F(122) F(120) AND 
CONT C(47) F(125) F(126) F(127) AND 
CONT C(47) F(127) F(125) F(126) AND 
CONT C(47) F(126) F(127) F(125) AND 
CONT C(61) F(130) F(131) F(132) AND 
CONT C(61) F(132) F(130) F(131) AND 
CONT C(61) F(131) F(132) F(130) AND 
CONT C(61) F(135) F(136) F(137) AND 
CONT C(61) F(137) F(135) F(136) AND 
CONT C(61) F(136) F(137) F(135) AND 
CONT C(65) F(140) F(141) F(142) AND 
CONT C(65) F(142) F(140) F(141) AND 
CONT C(65) F(141) F(142) F(140) AND 
CONT C(65) F(145) F(146) F(147) AND 
CONT C(65) F(147) F(145) F(146) AND 
CONT C(65) F(146) F(147) F(145) 
DELU 0.01 C(79) F(80) F(81) F(82) AND 
CONT C(79) F(82) F(80) F(81) AND 
CONT C(79) F(81) F(82) F(80) AND 
CONT C(79) F(85) F(86) F(87) AND 
CONT C(79) F(87) F(85) F(86) AND 
CONT C(79) F(86) F(87) F(85) AND 
CONT C(51) F(90) F(91) F(92) AND 
CONT C(51) F(92) F(90) F(91) AND 
CONT C(51) F(91) F(92) F(90) AND 
CONT C(51) F(95) F(96) F(97) AND 
CONT C(51) F(97) F(95) F(96) AND 
CONT C(51) F(96) F(97) F(95) AND 
CONT C(36) F(100) F(101) F(102) AND 
CONT C(36) F(102) F(100) F(101) AND 
CONT C(36) F(101) F(102) F(100) AND 
CONT C(36) F(105) F(106) F(107) AND 
CONT C(36) F(107) F(105) F(106) AND 
CONT C(36) F(106) F(107) F(105) AND 
CONT C(75) F(110) F(111) F(112) AND 
CONT C(75) F(112) F(110) F(111) AND 
CONT C(75) F(111) F(112) F(110) AND 
CONT C(75) F(115) F(116) F(117) AND 
CONT C(75) F(117) F(115) F(116) AND 
CONT C(75) F(116) F(117) F(115) AND 
CONT C(47) F(120) F(121) F(122) AND 
CONT C(47) F(122) F(120) F(121) AND 
CONT C(47) F(121) F(122) F(120) AND 
CONT C(47) F(125) F(126) F(127) AND 
CONT C(47) F(127) F(125) F(126) AND 
CONT C(47) F(126) F(127) F(125) AND 
CONT C(61) F(130) F(131) F(132) AND 
CONT C(61) F(132) F(130) F(131) AND 
CONT C(61) F(131) F(132) F(130) AND 
CONT C(61) F(135) F(136) F(137) AND 
CONT C(61) F(137) F(135) F(136) AND 
CONT C(61) F(136) F(137) F(135) AND 
CONT C(65) F(140) F(141) F(142) AND 
CONT C(65) F(142) F(140) F(141) AND 
CONT C(65) F(141) F(142) F(140) AND 
CONT C(65) F(145) F(146) F(147) AND 
CONT C(65) F(147) F(145) F(146) AND 
CONT C(65) F(146) F(147) F(145) 
REM :TOL 
PLANAR C(100) C(101) C(102) C(103) C(104) C(105) C(106) 
PLANAR C(100) C(101) C(102) C(103) C(104) C(105) C(106) 
PLANAR C(120) C(121) C(122) C(123) C(124) C(125) C(126) 
PLANAR C(130) C(131) C(132) C(133) C(134) C(135) C(136) 
SAME C(106) C(104) C(105) C(100) C(101) C(102) C(103) AND 
CONT C(106) C(104) C(103) C(102) C(101) C(100) C(105) AND 
CONT C(116) C(114) C(115) C(110) C(111) C(112) C(113) AND 
CONT C(116) C(114) C(113) C(112) C(111) C(110) C(115) AND 
CONT C(126) C(120) C(125) C(124) C(123) C(122) C(121) AND 
CONT C(126) C(120) C(121) C(122) C(123) C(124) C(125) AND 
CONT C(136) C(130) C(135) C(134) C(133) C(132) C(131) AND 
CONT C(136) C(130) C(131) C(132) C(133) C(134) C(135) 
DELU 0.01 C(106) C(104) C(105) C(100) C(101) C(102) C(103) AND 
CONT C(106) C(104) C(103) C(102) C(101) C(100) C(105) AND 
CONT C(116) C(114) C(115) C(110) C(111) C(112) C(113) AND 
CONT C(116) C(114) C(113) C(112) C(111) C(110) C(115) AND 
CONT C(126) C(120) C(125) C(124) C(123) C(122) C(121) AND 
CONT C(126) C(120) C(121) C(122) C(123) C(124) C(125) AND 
CONT C(136) C(130) C(135) C(134) C(133) C(132) C(131) AND 
CONT C(136) C(130) C(131) C(132) C(133) C(134) C(135) 
SIMU 0.01 C(106) C(104) C(105) C(100) C(101) C(102) C(103) AND 
CONT C(106) C(104) C(103) C(102) C(101) C(100) C(105) AND 
CONT C(116) C(114) C(115) C(110) C(111) C(112) C(113) AND 
CONT C(116) C(114) C(113) C(112) C(111) C(110) C(115) AND 
CONT C(126) C(120) C(125) C(124) C(123) C(122) C(121) AND 
CONT C(126) C(120) C(121) C(122) C(123) C(124) C(125) AND 
CONT C(136) C(130) C(135) C(134) C(133) C(132) C(131) AND 
CONT C(136) C(130) C(131) C(132) C(133) C(134) C(135) 
DIST 1.54,0.01 = C(104) TO C(106) C(114) TO C(116) 
CONT C(120) TO C(126) C(130) TO C(136) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;