#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:58:59 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179087 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/49/4304933.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_4304933
loop_
_publ_author_name
'Hyui Sul Lee'
'Sven-Oliver Hauber'
'Denis Vinduš'
'Mark Niemeyer'
_publ_contact_author_address
;
Institut für Anorganische und Analytische Chemie
Johannes Gutenberg-Universität Mainz
Duesbergweg 10-14
D-55099 Mainz
Germany
;
_publ_contact_author_email       niemeyer@uni-mainz.de
_publ_contact_author_name        'Mark Niemeyer'
_publ_section_title
;
Isostructural Potassium and Thallium Salts of Sterically Crowded Triazenes:
A Structural and Computational Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4401
_journal_page_last               4412
_journal_paper_doi               10.1021/ic800029z
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C42 H54 N3 Tl'
_chemical_formula_weight         805.25
_chemical_melting_point          '289-293 deg.C (dec.)'
_chemical_name_systematic
;
((1,3-bis-(2',4',6'-triisopropylbiphenyl-2))(triazenido-N,N'))thallium
;
_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                101.603(8)
_cell_angle_beta                 104.350(10)
_cell_angle_gamma                90.816(11)
_cell_formula_units_Z            2
_cell_length_a                   9.4318(14)
_cell_length_b                   14.4350(16)
_cell_length_c                   14.8042(15)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      6.0
_cell_volume                     1908.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P3'
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9757
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        1.5
_diffrn_standards_interval_count 298
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.263
_exptl_absorpt_correction_T_max  0.4827
_exptl_absorpt_correction_T_min  0.2244
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         9211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0355P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                8042
_reflns_number_total             9211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800029z-file003_6.cif
_cod_data_source_block           3a
_cod_database_code               4304933
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Tl Tl 0.574452(16) 0.746669(9) 0.750711(10) 0.03481(5) Uani 1 1 d . . .
N1 N 0.7361(3) 0.60658(19) 0.7232(2) 0.0281(6) Uani 1 1 d . . .
N2 N 0.8159(3) 0.63634(18) 0.67315(19) 0.0245(5) Uani 1 1 d . . .
N3 N 0.7813(3) 0.72086(18) 0.6614(2) 0.0268(6) Uani 1 1 d . . .
C11 C 0.7616(3) 0.5172(2) 0.7440(2) 0.0249(6) Uani 1 1 d . . .
C12 C 0.6713(3) 0.4857(2) 0.7963(2) 0.0241(6) Uani 1 1 d . . .
C13 C 0.6935(4) 0.3988(2) 0.8232(2) 0.0325(7) Uani 1 1 d . . .
H13A H 0.6332 0.3774 0.8587 0.042(4) Uiso 1 1 calc R . .
C14 C 0.8032(4) 0.3432(2) 0.7987(3) 0.0365(8) Uani 1 1 d . . .
H14A H 0.8189 0.2847 0.8186 0.042(4) Uiso 1 1 calc R . .
C15 C 0.8890(4) 0.3731(2) 0.7457(3) 0.0344(8) Uani 1 1 d . . .
H15A H 0.9623 0.3342 0.7280 0.042(4) Uiso 1 1 calc R . .
C16 C 0.8698(4) 0.4595(2) 0.7176(2) 0.0307(7) Uani 1 1 d . . .
H16A H 0.9293 0.4793 0.6809 0.042(4) Uiso 1 1 calc R . .
C21 C 0.5537(3) 0.5459(2) 0.8224(2) 0.0228(6) Uani 1 1 d . . .
C22 C 0.5812(4) 0.6102(2) 0.9114(2) 0.0251(6) Uani 1 1 d . . .
C23 C 0.4704(4) 0.6662(2) 0.9337(2) 0.0285(7) Uani 1 1 d . . .
H23A H 0.4899 0.7094 0.9937 0.036(3) Uiso 1 1 calc R . .
C24 C 0.3326(4) 0.6609(2) 0.8712(2) 0.0303(7) Uani 1 1 d . B .
C25 C 0.3080(4) 0.5977(2) 0.7844(2) 0.0316(7) Uani 1 1 d . . .
H25A H 0.2141 0.5931 0.7408 0.036(3) Uiso 1 1 calc R . .
C26 C 0.4146(4) 0.5404(2) 0.7580(2) 0.0262(6) Uani 1 1 d . . .
C31 C 0.8516(3) 0.7609(2) 0.6037(2) 0.0247(6) Uani 1 1 d . . .
C32 C 0.8035(3) 0.8484(2) 0.5850(2) 0.0243(6) Uani 1 1 d . . .
C33 C 0.8657(4) 0.8917(2) 0.5271(3) 0.0341(7) Uani 1 1 d . . .
H33A H 0.8339 0.9512 0.5150 0.042(4) Uiso 1 1 calc R . .
C34 C 0.9731(4) 0.8502(3) 0.4864(3) 0.0402(9) Uani 1 1 d . . .
H34A H 1.0131 0.8801 0.4457 0.042(4) Uiso 1 1 calc R . .
C35 C 1.0215(4) 0.7638(3) 0.5063(3) 0.0408(9) Uani 1 1 d . . .
H35A H 1.0958 0.7351 0.4794 0.042(4) Uiso 1 1 calc R . .
C36 C 0.9628(4) 0.7199(2) 0.5643(3) 0.0308(7) Uani 1 1 d . . .
H36A H 0.9976 0.6614 0.5778 0.042(4) Uiso 1 1 calc R . .
C41 C 0.6872(3) 0.8941(2) 0.6285(2) 0.0237(6) Uani 1 1 d . . .
C42 C 0.7272(4) 0.9534(2) 0.7202(2) 0.0278(7) Uani 1 1 d . . .
C43 C 0.6180(4) 0.9944(2) 0.7603(2) 0.0301(7) Uani 1 1 d . . .
H43A H 0.6451 1.0344 0.8221 0.036(3) Uiso 1 1 calc R . .
C44 C 0.4697(4) 0.9782(2) 0.7120(3) 0.0323(7) Uani 1 1 d . . .
C45 C 0.4331(4) 0.9199(2) 0.6225(2) 0.0289(7) Uani 1 1 d . . .
H45A H 0.3325 0.9082 0.5891 0.036(3) Uiso 1 1 calc R . .
C46 C 0.5389(3) 0.8772(2) 0.5790(2) 0.0248(6) Uani 1 1 d . . .
C221 C 0.7311(4) 0.6194(3) 0.9830(2) 0.0325(7) Uani 1 1 d . . .
H22A H 0.8013 0.5831 0.9513 0.036(3) Uiso 1 1 calc R . .
C222 C 0.7912(5) 0.7227(3) 1.0193(4) 0.0601(13) Uani 1 1 d . . .
H22B H 0.8866 0.7258 1.0654 0.090(3) Uiso 1 1 calc R . .
H22C H 0.7228 0.7590 1.0501 0.090(3) Uiso 1 1 calc R . .
H22D H 0.8028 0.7495 0.9655 0.090(3) Uiso 1 1 calc R . .
C223 C 0.7191(6) 0.5782(5) 1.0682(4) 0.0778(19) Uani 1 1 d . . .
H22E H 0.8166 0.5809 1.1121 0.090(3) Uiso 1 1 calc R . .
H22F H 0.6794 0.5122 1.0459 0.090(3) Uiso 1 1 calc R . .
H22G H 0.6537 0.6151 1.1014 0.090(3) Uiso 1 1 calc R . .
C241 C 0.2083(5) 0.7188(3) 0.8946(3) 0.0466(10) Uani 1 1 d . . .
H24A H 0.1648 0.7481 0.8391 0.036(3) Uiso 0.75 1 calc PR A 1
H24B H 0.1227 0.6780 0.8960 0.036(3) Uiso 0.25 1 calc PR A 2
C242 C 0.2553(7) 0.7989(4) 0.9838(4) 0.0805(18) Uani 1 1 d . B .
H24C H 0.3006 0.7721 1.0391 0.090(3) Uiso 1 1 calc R . .
H24D H 0.1692 0.8318 0.9950 0.090(3) Uiso 1 1 calc R . .
H24E H 0.3263 0.8438 0.9743 0.090(3) Uiso 1 1 calc R . .
C243 C 0.0896(6) 0.6588(5) 0.9097(5) 0.0652(19) Uani 0.75 1 d P B 1
H24F H 0.1306 0.6264 0.9616 0.090(3) Uiso 0.75 1 calc PR B 1
H24G H 0.0473 0.6116 0.8510 0.090(3) Uiso 0.75 1 calc PR B 1
H24H H 0.0130 0.6988 0.9263 0.090(3) Uiso 0.75 1 calc PR B 1
C244 C 0.167(3) 0.7797(16) 0.8195(15) 0.079(8) Uani 0.25 1 d P B 2
H24I H 0.0816 0.8146 0.8284 0.090(3) Uiso 0.25 1 calc PR B 2
H24J H 0.1439 0.7388 0.7556 0.090(3) Uiso 0.25 1 calc PR B 2
H24K H 0.2500 0.8247 0.8265 0.090(3) Uiso 0.25 1 calc PR B 2
C261 C 0.3797(4) 0.4707(2) 0.6621(2) 0.0322(7) Uani 1 1 d . . .
H26A H 0.4743 0.4573 0.6446 0.036(3) Uiso 1 1 calc R . .
C262 C 0.2789(6) 0.5085(3) 0.5813(3) 0.0535(11) Uani 1 1 d . . .
H26B H 0.3181 0.5713 0.5800 0.090(3) Uiso 1 1 calc R . .
H26C H 0.1805 0.5132 0.5918 0.090(3) Uiso 1 1 calc R . .
H26D H 0.2737 0.4651 0.5202 0.090(3) Uiso 1 1 calc R . .
C263 C 0.3111(5) 0.3775(3) 0.6706(3) 0.0477(10) Uani 1 1 d . . .
H26E H 0.3794 0.3507 0.7186 0.090(3) Uiso 1 1 calc R . .
H26F H 0.2904 0.3328 0.6088 0.090(3) Uiso 1 1 calc R . .
H26G H 0.2196 0.3891 0.6897 0.090(3) Uiso 1 1 calc R . .
C421 C 0.8866(4) 0.9737(3) 0.7764(3) 0.0368(8) Uani 1 1 d . . .
H42A H 0.9483 0.9369 0.7377 0.036(3) Uiso 1 1 calc R . .
C422 C 0.9134(6) 0.9415(5) 0.8702(4) 0.0802(18) Uani 1 1 d . . .
H42B H 1.0173 0.9541 0.9043 0.090(3) Uiso 1 1 calc R . .
H42C H 0.8869 0.8733 0.8578 0.090(3) Uiso 1 1 calc R . .
H42D H 0.8533 0.9761 0.9093 0.090(3) Uiso 1 1 calc R . .
C423 C 0.9332(5) 1.0779(3) 0.7930(5) 0.0692(16) Uani 1 1 d . . .
H42E H 0.9208 1.0964 0.7314 0.090(3) Uiso 1 1 calc R . .
H42F H 1.0365 1.0892 0.8287 0.090(3) Uiso 1 1 calc R . .
H42G H 0.8726 1.1157 0.8295 0.090(3) Uiso 1 1 calc R . .
C441 C 0.3528(5) 1.0261(3) 0.7564(3) 0.0430(9) Uani 1 1 d . . .
H44A H 0.2556 0.9961 0.7159 0.036(3) Uiso 1 1 calc R . .
C442 C 0.3651(8) 1.0108(6) 0.8555(5) 0.098(2) Uani 1 1 d . . .
H44B H 0.2858 1.0412 0.8799 0.090(3) Uiso 1 1 calc R . .
H44C H 0.4600 1.0386 0.8973 0.090(3) Uiso 1 1 calc R . .
H44D H 0.3573 0.9427 0.8539 0.090(3) Uiso 1 1 calc R . .
C443 C 0.3529(6) 1.1299(3) 0.7543(4) 0.0629(13) Uani 1 1 d . . .
H44E H 0.2741 1.1581 0.7807 0.090(3) Uiso 1 1 calc R . .
H44F H 0.3372 1.1374 0.6882 0.090(3) Uiso 1 1 calc R . .
H44G H 0.4475 1.1617 0.7924 0.090(3) Uiso 1 1 calc R . .
C461 C 0.4905(4) 0.8124(2) 0.4811(2) 0.0302(7) Uani 1 1 d . . .
H46A H 0.5778 0.8053 0.4539 0.036(3) Uiso 1 1 calc R . .
C462 C 0.4388(4) 0.7142(2) 0.4880(3) 0.0395(9) Uani 1 1 d . . .
H46B H 0.5213 0.6844 0.5230 0.090(3) Uiso 1 1 calc R . .
H46C H 0.4010 0.6753 0.4236 0.090(3) Uiso 1 1 calc R . .
H46D H 0.3610 0.7199 0.5216 0.090(3) Uiso 1 1 calc R . .
C463 C 0.3710(4) 0.8532(3) 0.4122(3) 0.0390(8) Uani 1 1 d . . .
H46E H 0.4007 0.9190 0.4139 0.090(3) Uiso 1 1 calc R . .
H46F H 0.2789 0.8512 0.4314 0.090(3) Uiso 1 1 calc R . .
H46G H 0.3570 0.8155 0.3474 0.090(3) 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'
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
N1 Tl N3 48.42(8) . . ?
N2 N1 C11 116.9(3) . . ?
N2 N1 Tl 101.74(18) . . ?
C11 N1 Tl 141.4(2) . . ?
N1 N2 N3 109.6(2) . . ?
N2 N3 C31 116.7(3) . . ?
N2 N3 Tl 100.28(18) . . ?
C31 N3 Tl 142.8(2) . . ?
N1 C11 C16 124.6(3) . . ?
N1 C11 C12 115.8(3) . . ?
C16 C11 C12 119.6(3) . . ?
C13 C12 C11 119.4(3) . . ?
C13 C12 C21 120.9(3) . . ?
C11 C12 C21 119.7(3) . . ?
C14 C13 C12 120.6(3) . . ?
C15 C14 C13 119.9(3) . . ?
C14 C15 C16 120.9(3) . . ?
C15 C16 C11 119.6(3) . . ?
C26 C21 C22 119.0(3) . . ?
C26 C21 C12 120.5(3) . . ?
C22 C21 C12 120.5(3) . . ?
C23 C22 C21 119.5(3) . . ?
C23 C22 C221 119.7(3) . . ?
C21 C22 C221 120.8(3) . . ?
C24 C23 C22 122.1(3) . . ?
C25 C24 C23 117.6(3) . . ?
C25 C24 C241 119.1(3) . . ?
C23 C24 C241 123.3(3) . . ?
C24 C25 C26 122.9(3) . . ?
C25 C26 C21 119.0(3) . . ?
C25 C26 C261 120.4(3) . . ?
C21 C26 C261 120.6(3) . . ?
C32 C31 N3 115.8(3) . . ?
C32 C31 C36 119.2(3) . . ?
N3 C31 C36 125.0(3) . . ?
C33 C32 C31 119.2(3) . . ?
C33 C32 C41 121.0(3) . . ?
C31 C32 C41 119.8(3) . . ?
C34 C33 C32 121.6(3) . . ?
C33 C34 C35 118.8(3) . . ?
C36 C35 C34 120.8(3) . . ?
C35 C36 C31 120.3(3) . . ?
C46 C41 C42 119.8(3) . . ?
C46 C41 C32 120.4(3) . . ?
C42 C41 C32 119.8(3) . . ?
C43 C42 C41 119.2(3) . . ?
C43 C42 C421 119.2(3) . . ?
C41 C42 C421 121.6(3) . . ?
C42 C43 C44 121.7(3) . . ?
C45 C44 C43 118.1(3) . . ?
C45 C44 C441 121.4(3) . . ?
C43 C44 C441 120.6(3) . . ?
C44 C45 C46 122.4(3) . . ?
C41 C46 C45 118.8(3) . . ?
C41 C46 C461 121.6(3) . . ?
C45 C46 C461 119.6(3) . . ?
C223 C221 C22 109.8(3) . . ?
C223 C221 C222 108.5(4) . . ?
C22 C221 C222 111.9(3) . . ?
C243 C241 C24 112.0(4) . . ?
C243 C241 C244 118.4(12) . . ?
C24 C241 C244 106.4(8) . . ?
C243 C241 C242 106.7(5) . . ?
C24 C241 C242 114.3(4) . . ?
C244 C241 C242 98.5(10) . . ?
C26 C261 C263 110.0(3) . . ?
C26 C261 C262 113.6(3) . . ?
C263 C261 C262 109.6(3) . . ?
C422 C421 C423 110.8(4) . . ?
C422 C421 C42 111.3(4) . . ?
C423 C421 C42 110.9(3) . . ?
C442 C441 C443 111.3(4) . . ?
C442 C441 C44 112.8(4) . . ?
C443 C441 C44 111.3(3) . . ?
C46 C461 C462 111.0(3) . . ?
C46 C461 C463 112.5(3) . . ?
C462 C461 C463 110.2(3) . . ?
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
Tl N1 2.578(3) . ?
Tl N3 2.607(3) . ?
N1 N2 1.301(4) . ?
N1 C11 1.396(4) . ?
N2 N3 1.301(4) . ?
N3 C31 1.403(4) . ?
C11 C16 1.407(4) . ?
C11 C12 1.410(4) . ?
C12 C13 1.394(4) . ?
C12 C21 1.497(4) . ?
C13 C14 1.393(5) . ?
C14 C15 1.379(5) . ?
C15 C16 1.393(5) . ?
C21 C26 1.408(4) . ?
C21 C22 1.412(4) . ?
C22 C23 1.394(5) . ?
C22 C221 1.527(5) . ?
C23 C24 1.388(5) . ?
C24 C25 1.383(5) . ?
C24 C241 1.519(5) . ?
C25 C26 1.391(5) . ?
C26 C261 1.524(4) . ?
C31 C32 1.403(4) . ?
C31 C36 1.405(4) . ?
C32 C33 1.388(5) . ?
C32 C41 1.501(4) . ?
C33 C34 1.386(5) . ?
C34 C35 1.395(6) . ?
C35 C36 1.375(5) . ?
C41 C46 1.401(5) . ?
C41 C42 1.410(4) . ?
C42 C43 1.394(5) . ?
C42 C421 1.519(5) . ?
C43 C44 1.397(5) . ?
C44 C45 1.378(5) . ?
C44 C441 1.524(5) . ?
C45 C46 1.402(5) . ?
C46 C461 1.516(4) . ?
C221 C223 1.526(6) . ?
C221 C222 1.528(5) . ?
C241 C243 1.493(8) . ?
C241 C244 1.53(2) . ?
C241 C242 1.536(7) . ?
C261 C263 1.526(5) . ?
C261 C262 1.531(6) . ?
C421 C422 1.516(6) . ?
C421 C423 1.516(6) . ?
C441 C442 1.504(7) . ?
C441 C443 1.504(6) . ?
C461 C462 1.523(5) . ?
C461 C463 1.533(5) . ?
