#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:06:50 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179952 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/47/7024709.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_7024709
loop_
_publ_author_name
'Ritch, Jamie S.'
'Chivers, Tristram'
_publ_section_title
;
 Thallium(I) complexes of dichalcogenido imidodiphosphinates
 {Tl[(EP(i)Pr(2))(2)N]}(n) (E = Te, Se, S): Synthesis, NMR spectra and a
 structural comparison.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1745
_journal_page_last               1750
_journal_paper_doi               10.1039/b920388e
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C12 H28 N P2 S2 Tl'
_chemical_formula_sum            'C12 H28 N P2 S2 Tl'
_chemical_formula_weight         516.78
_chemical_name_systematic
;
?
;
_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                108.92(3)
_cell_angle_beta                 98.79(3)
_cell_angle_gamma                104.88(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3507(17)
_cell_length_b                   9.2269(18)
_cell_length_c                   13.319(3)
_cell_measurement_reflns_used    12739
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.61
_cell_volume                     906.4(5)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phiω 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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12739
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    9.303
_exptl_absorpt_correction_T_max  0.7073
_exptl_absorpt_correction_T_min  0.1548
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'HKL SCALEPACK (Otwinowski and Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.894
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.579
_refine_diff_density_min         -1.671
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         4105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0299
_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)+(0.0385P)²+3.7017P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                3971
_reflns_number_total             4105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b920388e.txt
_cod_data_source_block           compound3c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024709
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
Tl1 Tl 0.28084(2) 0.54484(2) 0.546051(14) 0.02839(7) Uani 1 1 d .
S1 S -0.02184(15) 0.25366(13) 0.44859(9) 0.0236(2) Uani 1 1 d .
P1 P 0.01055(14) 0.09587(12) 0.31320(8) 0.0169(2) Uani 1 1 d .
C1 C -0.3325(6) -0.0113(6) 0.2014(4) 0.0310(10) Uani 1 1 d .
H1A H -0.4392 -0.1026 0.1634 0.046 Uiso 1 1 calc R
H1B H -0.2954 0.0375 0.1500 0.046 Uiso 1 1 calc R
H1C H -0.3518 0.0701 0.2627 0.046 Uiso 1 1 calc R
C2 C -0.1934(6) -0.0718(5) 0.2455(3) 0.0210(8) Uani 1 1 d .
H2A H -0.1753 -0.1530 0.1812 0.025 Uiso 1 1 calc R
C3 C -0.2528(6) -0.1580(6) 0.3199(4) 0.0290(10) Uani 1 1 d .
H3A H -0.3569 -0.2510 0.2782 0.044 Uiso 1 1 calc R
H3B H -0.2773 -0.0827 0.3819 0.044 Uiso 1 1 calc R
H3C H -0.1624 -0.1959 0.3475 0.044 Uiso 1 1 calc R
C4 C 0.1733(7) -0.1396(6) 0.2679(4) 0.0302(10) Uani 1 1 d .
H4A H 0.2539 -0.1857 0.2973 0.045 Uiso 1 1 calc R
H4B H 0.2133 -0.1032 0.2120 0.045 Uiso 1 1 calc R
H4C H 0.0596 -0.2224 0.2349 0.045 Uiso 1 1 calc R
C5 C 0.1627(5) 0.0052(5) 0.3614(4) 0.0201(8) Uani 1 1 d .
H5A H 0.1216 -0.0350 0.4172 0.024 Uiso 1 1 calc R
C6 C 0.3416(6) 0.1310(6) 0.4168(4) 0.0270(9) Uani 1 1 d .
H6A H 0.4212 0.0788 0.4392 0.040 Uiso 1 1 calc R
H6B H 0.3368 0.2171 0.4817 0.040 Uiso 1 1 calc R
H6C H 0.3813 0.1779 0.3651 0.040 Uiso 1 1 calc R
N1 N 0.0641(5) 0.1550(4) 0.2196(3) 0.0201(7) Uani 1 1 d .
P2 P 0.16088(14) 0.31554(13) 0.20303(8) 0.0185(2) Uani 1 1 d .
C7 C -0.0982(7) 0.4492(6) 0.2321(4) 0.0300(10) Uani 1 1 d .
H7A H -0.1805 0.4936 0.2027 0.045 Uiso 1 1 calc R
H7B H -0.0187 0.5324 0.3005 0.045 Uiso 1 1 calc R
H7C H -0.1599 0.3556 0.2468 0.045 Uiso 1 1 calc R
C8 C 0.0026(6) 0.3956(5) 0.1480(4) 0.0254(9) Uani 1 1 d .
H8A H 0.0667 0.4936 0.1361 0.031 Uiso 1 1 calc R
C9 C -0.1174(7) 0.2734(7) 0.0378(4) 0.0332(11) Uani 1 1 d .
H9A H -0.2020 0.3190 0.0125 0.050 Uiso 1 1 calc R
H9B H -0.1767 0.1734 0.0463 0.050 Uiso 1 1 calc R
H9C H -0.0507 0.2494 -0.0162 0.050 Uiso 1 1 calc R
C10 C 0.4013(6) 0.1822(7) 0.1265(4) 0.0312(10) Uani 1 1 d .
H10A H 0.4510 0.1434 0.0651 0.047 Uiso 1 1 calc R
H10B H 0.3495 0.0920 0.1474 0.047 Uiso 1 1 calc R
H10C H 0.4915 0.2672 0.1893 0.047 Uiso 1 1 calc R
C11 C 0.2641(6) 0.2508(5) 0.0919(4) 0.0222(8) Uani 1 1 d .
H11A H 0.1740 0.1610 0.0284 0.027 Uiso 1 1 calc R
C12 C 0.3375(8) 0.3862(7) 0.0522(5) 0.0364(12) Uani 1 1 d .
H12A H 0.3961 0.3473 -0.0042 0.055 Uiso 1 1 calc R
H12B H 0.4193 0.4802 0.1143 0.055 Uiso 1 1 calc R
H12C H 0.2440 0.4177 0.0211 0.055 Uiso 1 1 calc R
S2 S 0.33886(16) 0.50301(14) 0.32923(9) 0.0278(2) Uani 1 1 d .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
S2 Tl1 S1 90.36(5) . .
S2 Tl1 S1 100.07(4) . 2_566
S1 Tl1 S1 86.70(4) . 2_566
S2 Tl1 S2 99.13(4) . 2_666
S1 Tl1 S2 116.05(4) . 2_666
S1 Tl1 S2 149.99(3) 2_566 2_666
P1 S1 Tl1 109.60(6) . .
N1 P1 C5 110.5(2) . .
N1 P1 C2 105.73(19) . .
C5 P1 C2 105.3(2) . .
N1 P1 S1 119.94(14) . .
C5 P1 S1 106.82(15) . .
C2 P1 S1 107.63(15) . .
C3 C2 C1 110.5(4) . .
C3 C2 P1 112.9(3) . .
C1 C2 P1 110.4(3) . .
C6 C5 C4 109.6(4) . .
C6 C5 P1 111.1(3) . .
C4 C5 P1 112.1(3) . .
P1 N1 P2 140.7(2) . .
N1 P2 C11 106.1(2) . .
N1 P2 C8 109.6(2) . .
C11 P2 C8 104.6(2) . .
N1 P2 S2 120.40(15) . .
C11 P2 S2 107.69(16) . .
C8 P2 S2 107.24(16) . .
C9 C8 C7 111.2(4) . .
C9 C8 P2 111.9(3) . .
C7 C8 P2 110.0(3) . .
C10 C11 C12 111.2(4) . .
C10 C11 P2 110.6(3) . .
C12 C11 P2 112.7(3) . .
P2 S2 Tl1 115.24(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tl1 S2 2.9196(13) .
Tl1 S1 2.9223(19) .
Tl1 S1 3.1885(14) 2_566
Tl1 S2 3.5528(16) 2_666
S1 P1 2.0232(16) .
P1 N1 1.593(4) .
P1 C5 1.836(4) .
P1 C2 1.839(4) .
C1 C2 1.530(6) .
C2 C3 1.523(6) .
C4 C5 1.536(6) .
C5 C6 1.530(6) .
N1 P2 1.596(4) .
P2 C11 1.836(4) .
P2 C8 1.840(5) .
P2 S2 2.0141(19) .
C7 C8 1.532(6) .
C8 C9 1.525(7) .
C10 C11 1.525(7) .
C11 C12 1.533(6) .
