#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:33:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179334 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/31/4323160.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_4323160
loop_
_publ_author_name
'Gleb A. Abakumov'
'Vladimir K. Cherkasov'
'Vladimir I. Nevodchikov'
'Vyacheslav A. Kuropatov'
'Bruce C. Noll'
'Cortlandt G. Pierpont'
_publ_section_title
;
 Synthesis and Structure of a Polymeric Complex of Tl(III) Containing
 Bis(semiquinone) Bridging Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6117
_journal_page_last               6119
_journal_paper_doi               10.1021/ic980364g
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C17 H27 O3 Tl'
_chemical_formula_weight         483.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.7022(2)
_cell_length_b                   12.61970(10)
_cell_length_c                   23.01100(10)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    166(2)
_cell_measurement_theta_max      62.48
_cell_measurement_theta_min      1.77
_cell_volume                     3688.62(7)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      166(2)
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            30737
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    8.764
_exptl_absorpt_correction_T_max  0.223
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, R. H Acta Cryst. 1995 A51, 33-38.'
_exptl_crystal_colour            'deep green'
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.097
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         5335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_obs          0.0279
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0307P)²+6.9764P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0736
_refine_ls_wR_factor_obs         0.0647
_reflns_number_observed          4177
_reflns_number_total             5367
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980364g.cif
_cod_data_source_block           cp2
_cod_database_code               4323160
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Tl Tl 0.359200(10) 0.435097(12) 0.515815(5) 0.02629(5) Uani 1 d . .
O1 O 0.4771(2) 0.4599(2) 0.43173(10) 0.0291(6) Uani 1 d . .
O2 O 0.2874(2) 0.3641(3) 0.42311(11) 0.0361(7) Uani 1 d . .
C1 C 0.4465(3) 0.4275(3) 0.38086(14) 0.0222(7) Uani 1 d . .
C2 C 0.3401(3) 0.3760(3) 0.37685(14) 0.0236(7) Uani 1 d . .
C3 C 0.3011(3) 0.3421(3) 0.32040(14) 0.0215(7) Uani 1 d . .
C4 C 0.3647(3) 0.3594(3) 0.27352(14) 0.0224(7) Uani 1 d . .
H4A H 0.3390(3) 0.3394(3) 0.23633(14) 0.027 Uiso 1 calc R .
C5 C 0.4686(3) 0.4061(3) 0.27672(13) 0.0207(7) Uani 1 d . .
C6 C 0.5081(3) 0.4401(3) 0.33052(13) 0.0209(6) Uani 1 d . .
C7 C 0.6107(3) 0.4990(3) 0.33636(15) 0.0285(8) Uani 1 d . .
H7A H 0.6236(3) 0.5152(3) 0.37740(15) 0.043 Uiso 1 calc R .
H7B H 0.6072(3) 0.5651(3) 0.31410(15) 0.043 Uiso 1 calc R .
H7C H 0.6682(3) 0.4549(3) 0.32138(15) 0.043 Uiso 1 calc R .
C8 C 0.1938(3) 0.2880(3) 0.3155(2) 0.0290(8) Uani 1 d . .
C9 C 0.1934(4) 0.1846(4) 0.3508(2) 0.0502(12) Uani 1 d . .
H9A H 0.2493(4) 0.1378(4) 0.3366(2) 0.075 Uiso 1 calc R .
H9B H 0.1251(4) 0.1494(4) 0.3464(2) 0.075 Uiso 1 calc R .
H9C H 0.2055(4) 0.2008(4) 0.3919(2) 0.075 Uiso 1 calc R .
C10 C 0.1675(3) 0.2589(5) 0.2518(2) 0.0478(13) Uani 1 d . .
H10A H 0.2222(3) 0.2120(5) 0.2364(2) 0.072 Uiso 1 calc R .
H10B H 0.1642(3) 0.3236(5) 0.2284(2) 0.072 Uiso 1 calc R .
H10C H 0.0993(3) 0.2227(5) 0.2504(2) 0.072 Uiso 1 calc R .
C11 C 0.1065(3) 0.3610(4) 0.3377(2) 0.0448(11) Uani 1 d . .
H11A H 0.0384(3) 0.3251(4) 0.3342(2) 0.067 Uiso 1 calc R .
H11B H 0.1056(3) 0.4262(4) 0.3145(2) 0.067 Uiso 1 calc R .
H11C H 0.1197(3) 0.3786(4) 0.3785(2) 0.067 Uiso 1 calc R .
C12 C 0.2817(4) 0.5837(4) 0.5070(2) 0.0453(11) Uani 1 d . .
H12A H 0.2900(4) 0.6096(4) 0.4671(2) 0.068 Uiso 1 calc R .
H12B H 0.3126(4) 0.6348(4) 0.5342(2) 0.068 Uiso 1 calc R .
H12C H 0.2066(4) 0.5751(4) 0.5157(2) 0.068 Uiso 1 calc R .
C13 C 0.4248(4) 0.2884(4) 0.5437(2) 0.0405(9) Uani 1 d . .
H13A H 0.4620(4) 0.2549(4) 0.5112(2) 0.061 Uiso 1 calc R .
H13B H 0.3683(4) 0.2415(4) 0.5571(2) 0.061 Uiso 1 calc R .
H13C H 0.4743(4) 0.3012(4) 0.5756(2) 0.061 Uiso 1 calc R .
O3 O 0.1659(3) 0.3723(4) 0.5697(2) 0.086(2) Uani 1 d . .
C14 C 0.1535(5) 0.3228(7) 0.6230(3) 0.081(2) Uani 1 d . .
H14A H 0.2122(5) 0.3417(7) 0.6493(3) 0.097 Uiso 1 calc R .
H14B H 0.1528(5) 0.2449(7) 0.6180(3) 0.097 Uiso 1 calc R .
C15 C 0.0477(5) 0.3608(5) 0.6488(3) 0.064(2) Uani 1 d . .
H15A H 0.0154(5) 0.3066(5) 0.6743(3) 0.077 Uiso 1 calc R .
H15B H 0.0555(5) 0.4281(5) 0.6705(3) 0.077 Uiso 1 calc R .
C16 C -0.0128(4) 0.3752(5) 0.5937(3) 0.0592(14) Uani 1 d . .
H16A H -0.0703(4) 0.4272(5) 0.5989(3) 0.071 Uiso 1 calc R .
H16B H -0.0430(4) 0.3072(5) 0.5803(3) 0.071 Uiso 1 calc R .
C17 C 0.0686(5) 0.4156(6) 0.5516(3) 0.079(2) Uani 1 d . .
H17A H 0.0517(5) 0.3925(6) 0.5116(3) 0.095 Uiso 1 calc R .
H17B H 0.0714(5) 0.4940(6) 0.5524(3) 0.095 Uiso 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'
O O 0.0106 0.0060 '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
C12 Tl C13 167.5(2) . . ?
C12 Tl O1 95.4(2) . . ?
C13 Tl O1 96.27(15) . . ?
C12 Tl O2 93.8(2) . . ?
C13 Tl O2 95.07(14) . . ?
O1 Tl O2 66.15(8) . . ?
C12 Tl O1 88.1(2) . 5_666 ?
C13 Tl O1 89.47(14) . 5_666 ?
O1 Tl O1 79.85(8) . 5_666 ?
O2 Tl O1 145.98(8) . 5_666 ?
C1 O1 Tl 119.0(2) . . ?
C1 O1 Tl 140.8(2) . 5_666 ?
Tl O1 Tl 100.15(8) . 5_666 ?
C2 O2 Tl 118.9(2) . . ?
O1 C1 C6 122.6(3) . . ?
O1 C1 C2 117.4(3) . . ?
C6 C1 C2 119.9(3) . . ?
O2 C2 C3 122.4(3) . . ?
O2 C2 C1 118.4(3) . . ?
C3 C2 C1 119.2(3) . . ?
C4 C3 C2 117.2(3) . . ?
C4 C3 C8 122.7(3) . . ?
C2 C3 C8 120.1(3) . . ?
C3 C4 C5 124.3(3) . . ?
C6 C5 C4 119.7(3) . . ?
C6 C5 C5 123.1(4) . 3_655 ?
C4 C5 C5 117.0(3) . 3_655 ?
C5 C6 C1 119.5(3) . . ?
C5 C6 C7 122.6(3) . . ?
C1 C6 C7 117.6(3) . . ?
C11 C8 C3 110.6(3) . . ?
C11 C8 C9 109.4(4) . . ?
C3 C8 C9 110.0(3) . . ?
C11 C8 C10 107.6(3) . . ?
C3 C8 C10 111.6(3) . . ?
C9 C8 C10 107.4(4) . . ?
C14 O3 C17 109.6(5) . . ?
O3 C14 C15 107.4(5) . . ?
C16 C15 C14 99.1(5) . . ?
C15 C16 C17 103.5(5) . . ?
O3 C17 C16 106.2(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
Tl C12 2.128(5) . ?
Tl C13 2.129(4) . ?
Tl O1 2.467(2) . ?
Tl O2 2.487(3) . ?
Tl O1 2.745(3) 5_666 ?
O1 C1 1.300(4) . ?
O1 Tl 2.745(3) 5_666 ?
O2 C2 1.267(4) . ?
C1 C6 1.407(4) . ?
C1 C2 1.502(5) . ?
C2 C3 1.455(4) . ?
C3 C4 1.364(5) . ?
C3 C8 1.530(5) . ?
C4 C5 1.448(5) . ?
C5 C6 1.403(4) . ?
C5 C5 1.465(6) 3_655 ?
C6 C7 1.506(5) . ?
C8 C11 1.529(6) . ?
C8 C9 1.537(6) . ?
C8 C10 1.546(5) . ?
O3 C14 1.385(7) . ?
O3 C17 1.414(8) . ?
C14 C15 1.545(9) . ?
C15 C16 1.493(8) . ?
C16 C17 1.506(8) . ?
