#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/06/7010684.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7010684
loop_
_publ_author_name
'Motson, Graham R.'
'Mamula, Olimpia'
'Jeffery, John C.'
'McCleverty, Jon A.'
'Ward, Michael D.'
'von Zelewsky, Alex'
_publ_section_title
;
 A C3-symmetric chiral hexadentate podand ligand based on a
 tris(pyrazolyl)borate core
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1389
_journal_paper_doi               10.1039/b102295b
_journal_year                    2001
_chemical_formula_sum            'C45 H49 B N9 Tl'
_chemical_formula_weight         931.11
_space_group_IT_number           146
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   20.3970(18)
_cell_length_b                   20.3970(18)
_cell_length_c                   17.347(3)
_cell_measurement_temperature    173(2)
_cell_volume                     6250.1(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART Area Detector'
_diffrn_measurement_method
'ω rotation with narrow frames (0.3 degrees)'
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21871
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    3.920
_exptl_absorpt_correction_T_max  0.6953
_exptl_absorpt_correction_T_min  0.5078
_exptl_absorpt_correction_type   'Empirical, pseudo-azimuthal scan (SADABS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6361
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          1.143
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0230P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0502
_reflns_number_gt                5565
_reflns_number_total             6361
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b102295b.txt
_cod_data_source_block           1
_cod_original_cell_volume        6250.1(12)
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7010684
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl1 Tl 0.6667 0.3333 0.424739(10) 0.04137(12) Uani 1 3 d S . .
B1 B 0.6667 0.3333 0.6452(4) 0.063(3) Uani 1 3 d S . .
H1 H 0.6667 0.3333 0.7029 0.076 Uiso 1 3 calc SR . .
N11 N 0.6070(2) 0.3525(2) 0.61787(18) 0.0628(10) Uani 1 1 d . . .
N12 N 0.6003(2) 0.3670(2) 0.54239(18) 0.0546(9) Uani 1 1 d . . .
C13 C 0.5445(2) 0.3823(2) 0.5390(2) 0.0554(10) Uani 1 1 d . . .
C14 C 0.5152(3) 0.3763(3) 0.6128(3) 0.0831(17) Uani 1 1 d . . .
H14 H 0.4742 0.3834 0.6268 0.100 Uiso 1 1 calc R . .
C15 C 0.5558(3) 0.3587(3) 0.6602(3) 0.0829(16) Uani 1 1 d . . .
H15 H 0.5493 0.3518 0.7144 0.099 Uiso 1 1 calc R . .
N21 N 0.54487(18) 0.38011(19) 0.4012(2) 0.0511(8) Uani 1 1 d . . .
C22 C 0.5227(2) 0.4003(2) 0.4651(2) 0.0516(10) Uani 1 1 d . . .
C23 C 0.4814(3) 0.4380(3) 0.4596(3) 0.0693(15) Uani 1 1 d . . .
H23 H 0.4666 0.4525 0.5055 0.083 Uiso 1 1 calc R . .
C24 C 0.4619(3) 0.4544(2) 0.3902(3) 0.0647(13) Uani 1 1 d . . .
C25 C 0.4848(2) 0.4325(2) 0.3240(3) 0.0606(12) Uani 1 1 d . . .
C26 C 0.5256(2) 0.3958(3) 0.3336(3) 0.0595(11) Uani 1 1 d . . .
H26 H 0.5410 0.3806 0.2886 0.071 Uiso 1 1 calc R . .
C31 C 0.4184(3) 0.4964(3) 0.3788(4) 0.0923(18) Uani 1 1 d . . .
H31A H 0.3668 0.4658 0.4004 0.111 Uiso 1 1 calc R . .
H31B H 0.4442 0.5450 0.4070 0.111 Uiso 1 1 calc R . .
C32 C 0.4130(3) 0.5114(3) 0.2946(4) 0.100(2) Uani 1 1 d . . .
H32 H 0.3888 0.5425 0.2832 0.120 Uiso 1 1 calc R . .
C33 C 0.4919(4) 0.5387(3) 0.2549(5) 0.125(3) Uani 1 1 d . . .
H33A H 0.4983 0.5648 0.2050 0.150 Uiso 1 1 calc R . .
H33B H 0.5359 0.5678 0.2892 0.150 Uiso 1 1 calc R . .
C34 C 0.4671(3) 0.4543(3) 0.2477(3) 0.0809(16) Uani 1 1 d . . .
H34 H 0.4848 0.4391 0.2009 0.097 Uiso 1 1 calc R . .
C35 C 0.3829(3) 0.4373(3) 0.2467(3) 0.0718(14) Uani 1 1 d . . .
C36 C 0.3230(3) 0.3637(3) 0.2814(3) 0.0670(15) Uani 1 1 d . . .
H36A H 0.2752 0.3641 0.2852 0.101 Uiso 1 1 calc R . .
H36B H 0.3390 0.3577 0.3329 0.101 Uiso 1 1 calc R . .
H36C H 0.3158 0.3215 0.2486 0.101 Uiso 1 1 calc R . .
C37 C 0.3588(3) 0.4454(4) 0.1644(3) 0.104(2) Uani 1 1 d . . .
H37A H 0.3499 0.4015 0.1334 0.155 Uiso 1 1 calc R . .
H37B H 0.3990 0.4917 0.1406 0.155 Uiso 1 1 calc R . .
H37C H 0.3121 0.4480 0.1669 0.155 Uiso 1 1 calc R . .
Tl2 Tl 0.0000 0.0000 0.575041(10) 0.04899(14) Uani 1 3 d S . .
B2 B 0.0000 0.0000 0.7985(7) 0.072(4) Uani 1 3 d S . .
H2 H 0.0000 0.0000 0.8562 0.000(17) Uiso 1 3 calc SR . .
N41 N 0.0800(2) 0.0215(2) 0.76872(18) 0.0657(10) Uani 1 1 d . . .
N42 N 0.0994(2) 0.0309(2) 0.69285(18) 0.0577(9) Uani 1 1 d . . .
C43 C 0.1720(3) 0.0491(2) 0.6903(2) 0.0576(11) Uani 1 1 d . . .
C44 C 0.1989(3) 0.0511(3) 0.7647(3) 0.0787(15) Uani 1 1 d . . .
H44 H 0.2485 0.0629 0.7793 0.080(15) Uiso 1 1 calc R . .
C45 C 0.1387(4) 0.0326(3) 0.8119(3) 0.0803(15) Uani 1 1 d . . .
H45 H 0.1386 0.0283 0.8664 0.12(2) Uiso 1 1 calc R . .
N51 N 0.1668(2) 0.03509(19) 0.55259(19) 0.0553(8) Uani 1 1 d . . .
C52 C 0.2101(3) 0.0595(2) 0.6164(2) 0.0532(10) Uani 1 1 d . . .
C53 C 0.2888(3) 0.0903(3) 0.6107(3) 0.0683(16) Uani 1 1 d . . .
H53 H 0.3188 0.1079 0.6561 0.078(15) Uiso 1 1 calc R . .
C54 C 0.3228(3) 0.0954(3) 0.5425(3) 0.0631(12) Uani 1 1 d . . .
C55A C 0.2778(3) 0.0666(2) 0.4775(3) 0.0603(11) Uani 1 1 d . . .
C56A C 0.2007(3) 0.0387(2) 0.4859(2) 0.0592(11) Uani 1 1 d . . .
H56 H 0.1701 0.0209 0.4410 0.032(9) Uiso 1 1 calc R . .
C61 C 0.4088(4) 0.1336(6) 0.5323(4) 0.111(3) Uani 1 1 d . . .
H61A H 0.4327 0.1880 0.5456 0.23(6) Uiso 1 1 calc R . .
H61B H 0.4295 0.1099 0.5672 0.15(3) Uiso 1 1 calc R . .
C62 C 0.4266(4) 0.1251(6) 0.4495(4) 0.123(3) Uani 1 1 d . . .
H62 H 0.4816 0.1457 0.4383 0.094(17) Uiso 1 1 calc R . .
C63 C 0.3749(6) 0.0434(6) 0.4237(5) 0.123(3) Uani 1 1 d . . .
H63A H 0.3593 0.0056 0.4657 0.12(2) Uiso 1 1 calc R . .
H63B H 0.3938 0.0281 0.3784 0.15(3) Uiso 1 1 calc R . .
C64 C 0.3159(3) 0.0680(3) 0.4040(3) 0.0796(15) Uani 1 1 d . . .
H64 H 0.2827 0.0435 0.3582 0.096(17) Uiso 1 1 calc R . .
C65 C 0.3853(3) 0.1497(4) 0.3922(3) 0.0821(16) Uani 1 1 d . . .
C66 C 0.4179(4) 0.1618(5) 0.3113(4) 0.121(3) Uani 1 1 d . . .
H66A H 0.3882 0.1746 0.2765 0.17(3) Uiso 1 1 calc R . .
H66B H 0.4161 0.1153 0.2935 0.078(18) Uiso 1 1 calc R . .
H66C H 0.4706 0.2032 0.3119 0.17(3) Uiso 1 1 calc R . .
C67 C 0.3752(3) 0.2154(3) 0.4106(4) 0.085(2) Uani 1 1 d . . .
H67A H 0.4247 0.2618 0.4116 0.071(16) Uiso 1 1 calc R . .
H67B H 0.3509 0.2077 0.4611 0.082(19) Uiso 1 1 calc R . .
H67C H 0.3433 0.2200 0.3712 0.070(15) Uiso 1 1 calc R . .
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N12 Tl1 N12 69.83(12) 3_665 2_655 ?
N12 Tl1 N12 69.83(12) 3_665 . ?
N12 Tl1 N12 69.83(12) 2_655 . ?
N11 B1 N11 110.8(3) 2_655 3_665 ?
N11 B1 N11 110.8(3) 2_655 . ?
N11 B1 N11 110.8(3) 3_665 . ?
C15 N11 N12 109.8(4) . . ?
C15 N11 B1 128.0(4) . . ?
N12 N11 B1 122.2(4) . . ?
C13 N12 N11 106.6(3) . . ?
C13 N12 Tl1 128.4(3) . . ?
N11 N12 Tl1 123.3(2) . . ?
N12 C13 C14 108.7(4) . . ?
N12 C13 C22 120.3(4) . . ?
C14 C13 C22 131.1(4) . . ?
C15 C14 C13 107.0(4) . . ?
N11 C15 C14 107.9(4) . . ?
C26 N21 C22 118.2(4) . . ?
N21 C22 C23 120.1(4) . . ?
N21 C22 C13 117.2(4) . . ?
C23 C22 C13 122.7(4) . . ?
C24 C23 C22 121.7(5) . . ?
C23 C24 C25 117.6(4) . . ?
C23 C24 C31 125.2(5) . . ?
C25 C24 C31 117.2(5) . . ?
C26 C25 C24 117.7(5) . . ?
C26 C25 C34 124.6(5) . . ?
C24 C25 C34 117.6(4) . . ?
N21 C26 C25 124.7(4) . . ?
C32 C31 C24 111.2(5) . . ?
C31 C32 C35 110.7(4) . . ?
C31 C32 C33 109.3(5) . . ?
C35 C32 C33 87.1(5) . . ?
C34 C33 C32 86.2(4) . . ?
C25 C34 C33 105.5(5) . . ?
C25 C34 C35 110.1(4) . . ?
C33 C34 C35 87.6(4) . . ?
C36 C35 C37 109.4(5) . . ?
C36 C35 C32 118.9(5) . . ?
C37 C35 C32 112.5(4) . . ?
C36 C35 C34 117.8(4) . . ?
C37 C35 C34 110.9(4) . . ?
C32 C35 C34 85.5(4) . . ?
N42 Tl2 N42 69.75(12) . 2 ?
N42 Tl2 N42 69.75(12) . 3 ?
N42 Tl2 N42 69.75(12) 2 3 ?
N41 B2 N41 109.5(5) 3 . ?
N41 B2 N41 109.5(5) 3 2 ?
N41 B2 N41 109.5(5) . 2 ?
C45 N41 N42 110.2(4) . . ?
C45 N41 B2 126.1(6) . . ?
N42 N41 B2 123.6(6) . . ?
C43 N42 N41 106.0(3) . . ?
C43 N42 Tl2 129.3(3) . . ?
N41 N42 Tl2 124.3(3) . . ?
N42 C43 C44 110.1(4) . . ?
N42 C43 C52 120.4(4) . . ?
C44 C43 C52 129.4(5) . . ?
C45 C44 C43 105.1(5) . . ?
N41 C45 C44 108.6(4) . . ?
C56A N51 C52 117.8(4) . . ?
N51 C52 C53 120.0(4) . . ?
N51 C52 C43 117.7(4) . . ?
C53 C52 C43 122.3(4) . . ?
C54 C53 C52 121.6(5) . . ?
C53 C54 C55A 118.3(5) . . ?
C53 C54 C61 123.6(5) . . ?
C55A C54 C61 118.0(5) . . ?
C54 C55A C56A 117.7(4) . . ?
C54 C55A C64 117.4(5) . . ?
C56A C55A C64 124.9(4) . . ?
N51 C56A C55A 124.4(4) . . ?
C62 C61 C54 109.2(6) . . ?
C61 C62 C63 109.3(7) . . ?
C61 C62 C65 111.9(5) . . ?
C63 C62 C65 88.6(6) . . ?
C62 C63 C64 86.3(5) . . ?
C55A C64 C63 106.7(5) . . ?
C55A C64 C65 108.5(4) . . ?
C63 C64 C65 86.5(5) . . ?
C67 C65 C66 107.4(6) . . ?
C67 C65 C62 120.0(6) . . ?
C66 C65 C62 112.5(5) . . ?
C67 C65 C64 118.1(4) . . ?
C66 C65 C64 112.4(6) . . ?
C62 C65 C64 85.4(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tl1 N12 2.719(3) 3_665 ?
Tl1 N12 2.719(3) 2_655 ?
Tl1 N12 2.719(3) . ?
B1 N11 1.527(4) 2_655 ?
B1 N11 1.527(4) 3_665 ?
B1 N11 1.527(4) . ?
N11 C15 1.334(6) . ?
N11 N12 1.364(4) . ?
N12 C13 1.324(5) . ?
C13 C14 1.392(6) . ?
C13 C22 1.462(6) . ?
C14 C15 1.337(8) . ?
N21 C26 1.325(5) . ?
N21 C22 1.338(5) . ?
C22 C23 1.400(6) . ?
C23 C24 1.362(7) . ?
C24 C25 1.394(7) . ?
C24 C31 1.522(6) . ?
C25 C26 1.381(6) . ?
C25 C34 1.497(7) . ?
C31 C32 1.508(8) . ?
C32 C35 1.556(8) . ?
C32 C33 1.572(10) . ?
C33 C34 1.538(8) . ?
C34 C35 1.573(6) . ?
C35 C36 1.509(7) . ?
C35 C37 1.546(7) . ?
Tl2 N42 2.721(3) . ?
Tl2 N42 2.721(3) 2 ?
Tl2 N42 2.721(3) 3 ?
B2 N41 1.550(6) 3 ?
B2 N41 1.550(6) . ?
B2 N41 1.550(6) 2 ?
N41 C45 1.333(6) . ?
N41 N42 1.360(4) . ?
N42 C43 1.335(5) . ?
C43 C44 1.395(6) . ?
C43 C52 1.458(6) . ?
C44 C45 1.363(7) . ?
N51 C56A 1.332(5) . ?
N51 C52 1.347(5) . ?
C52 C53 1.405(7) . ?
C53 C54 1.350(7) . ?
C54 C55A 1.385(6) . ?
C54 C61 1.533(7) . ?
C55A C56A 1.385(6) . ?
C55A C64 1.487(6) . ?
C61 C62 1.513(9) . ?
C62 C63 1.527(11) . ?
C62 C65 1.539(8) . ?
C63 C64 1.557(9) . ?
C64 C65 1.570(8) . ?
C65 C67 1.489(8) . ?
C65 C66 1.519(8) . ?
