#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/91/2019155.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2019155
loop_
_publ_author_name
'Dias, H. V. Rasika'
'Thankamani, Jose'
_publ_section_title
;
 Thallium(I) complexes of fluorinated bis- and tris(pyrazolyl)borate
 ligands: [H₂B{3,5-(CF₃)₂pz}₂]Tl and [HB{3,5-(CF₃)₂pz}₃]Tl
;
_journal_coeditor_code           YP3035
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              959
_journal_page_last               962
_journal_paper_doi               10.1107/S0108270113016612
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Tl (C15 H4 B F18 N6)]'
_chemical_formula_sum            'C15 H4 B F18 N6 Tl'
_chemical_formula_weight         825.42
_chemical_name_common            '[HB(3,5-(CF3)2Pz)3]Tl'
_chemical_name_systematic
{Tris[3,5-bis(trifluoromethyl)-1Hpyrazol-1-yl-κN²]borato}thallium(I)
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 100.0340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1068(4)
_cell_length_b                   15.1155(8)
_cell_length_c                   9.1676(5)
_cell_measurement_reflns_used    5385
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.55
_cell_volume                     1106.20(10)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8569
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    7.472
_exptl_absorpt_correction_T_max  0.8069
_exptl_absorpt_correction_T_min  0.2127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.859
_refine_diff_density_min         -0.733
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0263
_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/[σ²(Fo²)+(0.0408P)²+1.9558P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0684
_reflns_number_gt                2196
_reflns_number_total             2256
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            yp3035.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2019155
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Tl Tl1 1.00262(2) 0.2500 0.279599(19) 0.01610(10) Uani d S 1 2
N N1 0.8302(5) 0.2500 0.6258(5) 0.0123(8) Uani d S 1 2
N N2 0.7962(5) 0.2500 0.4760(5) 0.0133(9) Uani d S 1 2
N N3 1.1077(4) 0.33435(19) 0.6650(3) 0.0129(6) Uani d . 1 1
N N4 1.1234(4) 0.3510(2) 0.5229(4) 0.0143(6) Uani d . 1 1
B B1 1.0159(7) 0.2500 0.7066(6) 0.0112(11) Uani d S 1 2
H H 1.0177 0.2500 0.8160 0.013 Uiso calc SR 1 2
C C1 0.6290(7) 0.2500 0.4409(6) 0.0146(10) Uani d S 1 2
C C2 0.5513(7) 0.2500 0.5638(7) 0.0169(11) Uani d S 1 2
H H2 0.4348 0.2500 0.5671 0.020 Uiso calc SR 1 2
C C3 0.6845(7) 0.2500 0.6807(6) 0.0151(10) Uani d S 1 2
C C4 0.5491(7) 0.2500 0.2811(6) 0.0179(11) Uani d S 1 2
C C5 0.6710(7) 0.2500 0.8409(7) 0.0214(12) Uani d S 1 2
C C6 1.2027(5) 0.4285(2) 0.5245(4) 0.0164(7) Uani d . 1 1
C C7 1.2403(5) 0.4633(3) 0.6672(4) 0.0180(8) Uani d . 1 1
H H7 1.2963 0.5171 0.6979 0.022 Uiso calc R 1 1
C C8 1.1778(5) 0.4021(2) 0.7525(4) 0.0158(7) Uani d . 1 1
C C9 1.2442(5) 0.4668(3) 0.3867(5) 0.0187(8) Uani d . 1 1
C C10 1.1810(5) 0.4079(3) 0.9163(5) 0.0194(8) Uani d . 1 1
F F1 0.5950(3) 0.17874(16) 0.2085(3) 0.0249(5) Uani d . 1 1
F F2 0.3829(4) 0.2500 0.2660(4) 0.0205(7) Uani d S 1 2
F F3 0.5091(4) 0.2500 0.8543(4) 0.0317(9) Uani d S 1 2
F F4 0.7404(4) 0.3208(2) 0.9134(3) 0.0404(7) Uani d . 1 1
F F5 1.1390(4) 0.44023(17) 0.2660(3) 0.0305(6) Uani d . 1 1
F F6 1.3988(3) 0.44397(18) 0.3657(3) 0.0326(6) Uani d . 1 1
F F7 1.2403(4) 0.55464(16) 0.3885(3) 0.0318(6) Uani d . 1 1
F F8 1.0285(3) 0.40954(16) 0.9512(3) 0.0246(5) Uani d . 1 1
F F9 1.2637(3) 0.34124(17) 0.9912(3) 0.0288(6) Uani d . 1 1
F F10 1.2583(4) 0.48295(18) 0.9673(3) 0.0326(6) Uani d . 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Tl1 N4 . . 68.10(10) y
N2 Tl1 N4 . 4_565 68.10(10) y
N4 Tl1 N4 . 4_565 67.74(13) y
N2 N1 C3 . . 109.8(4) ?
N2 N1 B1 . . 119.5(4) ?
C3 N1 B1 . . 130.7(4) ?
C1 N2 N1 . . 105.3(4) ?
C1 N2 Tl1 . . 124.5(3) ?
N1 N2 Tl1 . . 130.2(3) ?
N4 N3 C8 . . 109.1(3) ?
N4 N3 B1 . . 121.1(3) ?
C8 N3 B1 . . 129.8(3) ?
C6 N4 N3 . . 106.1(3) ?
C6 N4 Tl1 . . 127.0(3) ?
N3 N4 Tl1 . . 126.8(2) ?
N3 B1 N3 4_565 . 110.0(4) y
N3 B1 N1 4_565 . 110.3(3) y
N3 B1 N1 . . 110.3(3) y
N3 B1 H 4_565 . 108.7 ?
N3 B1 H . . 108.7 ?
N1 B1 H . . 108.7 ?
N2 C1 C2 . . 113.0(5) ?
N2 C1 C4 . . 119.0(5) ?
C2 C1 C4 . . 128.1(5) ?
C3 C2 C1 . . 103.1(5) ?
C3 C2 H2 . . 128.5 ?
C1 C2 H2 . . 128.5 ?
N1 C3 C2 . . 108.9(5) ?
N1 C3 C5 . . 125.5(5) ?
C2 C3 C5 . . 125.6(5) ?
F2 C4 F1 . 4_565 108.0(3) ?
F2 C4 F1 . . 108.0(3) ?
F1 C4 F1 4_565 . 105.6(4) ?
F2 C4 C1 . . 111.1(5) ?
F1 C4 C1 4_565 . 111.9(3) ?
F1 C4 C1 . . 111.9(3) ?
F4 C5 F4 4_565 . 107.0(5) ?
F4 C5 F3 4_565 . 106.8(3) ?
F4 C5 F3 . . 106.8(3) ?
F4 C5 C3 4_565 . 113.2(3) ?
F4 C5 C3 . . 113.2(3) ?
F3 C5 C3 . . 109.3(5) ?
N4 C6 C7 . . 111.6(3) ?
N4 C6 C9 . . 120.9(4) ?
C7 C6 C9 . . 127.4(3) ?
C8 C7 C6 . . 103.9(3) ?
C8 C7 H7 . . 128.1 ?
C6 C7 H7 . . 128.1 ?
N3 C8 C7 . . 109.3(3) ?
N3 C8 C10 . . 124.5(3) ?
C7 C8 C10 . . 126.2(4) ?
F7 C9 F5 . . 107.3(3) ?
F7 C9 F6 . . 106.4(3) ?
F5 C9 F6 . . 106.3(3) ?
F7 C9 C6 . . 111.8(3) ?
F5 C9 C6 . . 112.4(3) ?
F6 C9 C6 . . 112.2(3) ?
F8 C10 F9 . . 107.2(3) ?
F8 C10 F10 . . 107.4(3) ?
F9 C10 F10 . . 107.3(3) ?
F8 C10 C8 . . 112.8(3) ?
F9 C10 C8 . . 113.0(3) ?
F10 C10 C8 . . 108.9(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Tl1 N2 . 2.663(4) y
Tl1 N4 . 2.739(3) y
Tl1 N4 4_565 2.739(3) y
N1 N2 . 1.352(6) y
N1 C3 . 1.363(7) ?
N1 B1 . 1.557(7) y
N2 C1 . 1.338(7) ?
N3 N4 . 1.355(4) y
N3 C8 . 1.363(5) ?
N3 B1 . 1.557(4) y
N4 C6 . 1.335(5) ?
B1 N3 4_565 1.557(4) y
B1 H . 1.0000 ?
C1 C2 . 1.384(8) ?
C1 C4 . 1.495(7) ?
C2 C3 . 1.383(8) ?
C2 H2 . 0.9500 ?
C3 C5 . 1.492(8) ?
C4 F2 . 1.330(6) ?
C4 F1 4_565 1.352(4) ?
C4 F1 . 1.352(4) ?
C5 F4 4_565 1.332(4) ?
C5 F4 . 1.332(4) ?
C5 F3 . 1.340(7) ?
C6 C7 . 1.393(6) ?
C6 C9 . 1.481(5) ?
C7 C8 . 1.364(5) ?
C7 H7 . 0.9500 ?
C8 C10 . 1.500(5) ?
C9 F7 . 1.328(5) ?
C9 F5 . 1.336(5) ?
C9 F6 . 1.345(5) ?
C10 F8 . 1.330(5) ?
C10 F9 . 1.333(5) ?
C10 F10 . 1.340(5) ?
