#------------------------------------------------------------------------------
#$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/54/2005495.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_2005495
loop_
_publ_author_name
'Flomer, W. A.'
'Kolis, J. W.'
'Pennington, W. T.'
_publ_contact_author
;
      William T. Pennington
      Department of Chemistry
      Clemson University
      Clemson, SC 29634-1905
      U.S.A.
;
_publ_section_title
;
 Tris(tetraphenylphosphonium) Decatelluriumtantalide Dimethylformamide
 (1/1), a Tetraphenylphosphonium Salt of TaTe~10~^3{-^}
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2445
_journal_page_last               2448
_journal_paper_doi               10.1107/S0108270196005847
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         '(C24 H20 P)3 [Ta Te10], C3 H7 N O'
_chemical_formula_sum            'C75 H67 N O P3 Ta Te10'
_chemical_formula_weight         2548.16
_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_type_scat_source           'SHELXTL-Plus (Sheldrick, 1990)'
_audit_creation_method           'manual editing of form.cif'
_cell_angle_alpha                82.26(4)
_cell_angle_beta                 102.89(3)
_cell_angle_gamma                109.25(3)
_cell_formula_units_Z            2
_cell_length_a                   13.193(6)
_cell_length_b                   14.523(7)
_cell_length_c                   23.784(9)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    295
_cell_measurement_theta_max      14
_cell_measurement_theta_min      13
_cell_volume                     4185(3)
_computing_cell_refinement       'P3 Software'
_computing_data_collection       'P3 Software (Siemens, 1976)'
_computing_data_reduction        'SHELXTL-Plus (Sheldrick, 1990)'
_computing_molecular_graphics    SHELXTL-Plus
_computing_structure_refinement  SHELXTL-Plus
_computing_structure_solution    SHELXTL-Plus
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Siemens R3m/V diffractometer'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  .0449
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11475
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.83
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type
'empirical via \y scans (SHELXLTL-Plus; Sheldrick, 1990)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.02
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2340
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.744
_refine_diff_density_min         -1.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.502
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4544
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          .0598
_refine_ls_shift/esd_max         .193
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(F)+0.0005F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         .0709
_reflns_number_observed          4544
_reflns_number_total             10909
_reflns_observed_criterion       F>6\s(F)
_cod_data_source_file            fg1123.cif
_cod_data_source_block           CS0022
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/[\s^2^(F)+0.0005F^2^]' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(F)+0.0005F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C75 H67 N O P3 Te10 Ta'
_cod_database_code               2005495
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
Ta(1) 0.0370(10) 0.0370(10) 0.0310(10) 0.0120(10) 0.0050(10) 0.0010(10) Ta
Te(1) 0.054(2) 0.068(2) 0.036(2) 0.0130(10) -0.0020(10) 0.0030(10) Te
Te(2) 0.067(2) 0.050(2) 0.047(2) 0.0130(10) 0.0230(10) -0.0040(10) Te
Te(3) 0.0410(10) 0.053(2) 0.059(2) 0.0060(10) 0.0080(10) -0.0080(10) Te
Te(4) 0.050(2) 0.048(2) 0.069(2) 0.0170(10) 0.0110(10) 0.0130(10) Te
Te(5) 0.059(2) 0.064(2) 0.101(3) 0.029(2) 0.026(2) -0.001(2) Te
Te(6) 0.085(2) 0.071(2) 0.062(2) 0.022(2) 0.045(2) 0.007(2) Te
Te(7) 0.051(2) 0.049(2) 0.116(3) 0.0110(10) 0.000(2) -0.028(2) Te
Te(8) 0.0430(10) 0.065(2) 0.060(2) 0.0190(10) -0.0010(10) -0.0050(10) Te
Te(9) 0.074(2) 0.056(2) 0.040(2) 0.0290(10) 0.0070(10) 0.0060(10) Te
Te(10) 0.061(2) 0.070(2) 0.056(2) 0.0270(10) -0.0060(10) -0.025(2) Te
P(1) 0.039(5) 0.051(6) 0.049(7) 0.007(5) 0.013(5) -0.010(5) P
P(2) 0.033(5) 0.035(5) 0.036(6) 0.011(4) 0.006(4) 0.001(4) P
P(3) 0.035(5) 0.047(6) 0.036(6) 0.005(4) 0.014(5) 0.002(5) P
loop_
_atom_site_label
_atom_site_occupancy
_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_calc_flag
_atom_site_refinement_flags
Ta(1) 1 0.4114(1) 0.1880(1) 0.2567(1) 0.035(1) Uani d .
Te(1) 1 0.5420(2) 0.1880(2) 0.3708(1) 0.057(1) Uani d .
Te(2) 1 0.3348(2) 0.2618(2) 0.3343(1) 0.054(1) Uani d .
Te(3) 1 0.6260(2) 0.3053(2) 0.2598(1) 0.053(1) Uani d .
Te(4) 1 0.4164(2) 0.0052(2) 0.3035(1) 0.057(1) Uani d .
Te(5) 1 0.1295(2) 0.2782(2) 0.2657(1) 0.071(1) Uani d .
Te(6) 1 0.6167(2) 0.4062(2) 0.1472(1) 0.069(1) Uani d .
Te(7) 1 0.3028(2) -0.1139(2) 0.2060(2) 0.074(1) Uani d .
Te(8) 1 0.1896(2) 0.1631(2) 0.2000(1) 0.057(1) Uani d .
Te(9) 1 0.3938(2) 0.3091(2) 0.1537(1) 0.056(1) Uani d .
Te(10) 1 0.3513(2) 0.0807(2) 0.1565(1) 0.062(1) Uani d .
P(1) 1 0.1155(7) 0.2196(7) 0.5468(4) 0.046(4) Uani d .
P(2) 1 0.0269(7) 0.3111(6) -0.0185(4) 0.035(4) Uani d .
P(3) 1 0.6542(7) 0.7625(7) 0.2020(4) 0.041(4) Uani d .
C(111) 1 0.0377(18) 0.2356(18) 0.4772(9) 0.052(10) Uiso d G
C(112) 1 -0.0679 0.1738 0.4588 0.047(10) Uiso d G
C(113) 1 -0.1291 0.1943 0.4056 0.085(14) Uiso d G
C(114) 1 -0.0849 0.2766 0.3708 0.093(15) Uiso d G
C(115) 1 0.0207 0.3384 0.3891 0.080(13) Uiso d G
C(116) 1 0.0820 0.3179 0.4424 0.067(12) Uiso d G
C(121) 1 0.2152(16) 0.1606(15) 0.5451(11) 0.035(8) Uiso d G
C(122) 1 0.2460 0.1611 0.4926 0.065(12) Uiso d G
C(123) 1 0.3212 0.1140 0.4897 0.072(12) Uiso d G
C(124) 1 0.3656 0.0666 0.5392 0.068(12) Uiso d G
C(125) 1 0.3347 0.0661 0.5917 0.087(14) Uiso d G
C(126) 1 0.2595 0.1132 0.5946 0.062(11) Uiso d G
C(131) 1 0.0258(17) 0.1401(16) 0.5943(9) 0.050(10) Uiso d G
C(132) 1 -0.0095 0.0393 0.5895 0.065(12) Uiso d G
C(133) 1 -0.0793 -0.0222 0.6247 0.077(13) Uiso d G
C(134) 1 -0.1138 0.0170 0.6646 0.061(11) Uiso d G
C(135) 1 -0.0785 0.1179 0.6694 0.074(13) Uiso d G
C(136) 1 -0.0087 0.1794 0.6342 0.057(11) Uiso d G
C(141) 1 0.181(2) 0.3372(15) 0.5763(11) 0.056(10) Uiso d G
C(142) 1 0.2917 0.3642 0.6017 0.059(11) Uiso d G
C(143) 1 0.3445 0.4580 0.6208 0.090(15) Uiso d G
C(144) 1 0.2865 0.5248 0.6144 0.094(15) Uiso d G
C(145) 1 0.1758 0.4978 0.5890 0.13(2) Uiso d G
C(146) 1 0.1230 0.4040 0.5699 0.073(13) Uiso d G
C(211) 1 -0.0320(16) 0.3686(14) -0.0855(8) 0.033(8) Uiso d G
C(212) 1 -0.1400 0.3239 -0.1119 0.043(9) Uiso d G
C(213) 1 -0.1869 0.3672 -0.1624 0.046(9) Uiso d G
C(214) 1 -0.1258 0.4553 -0.1866 0.064(11) Uiso d G
C(215) 1 -0.0178 0.5000 -0.1603 0.051(10) Uiso d G
C(216) 1 0.0291 0.4567 -0.1097 0.050(10) Uiso d G
C(221) 1 0.0524(16) 0.2001(12) -0.0312(9) 0.033(8) Uiso d G
C(222) 1 0.1368 0.1710 0.0051 0.038(9) Uiso d G
C(223) 1 0.1563 0.0862 -0.0046 0.037(8) Uiso d G
C(224) 1 0.0914 0.0307 -0.0506 0.056(10) Uiso d G
C(225) 1 0.0071 0.0598 -0.0869 0.046(9) Uiso d G
C(226) 1 -0.0124 0.1446 -0.0772 0.054(10) Uiso d G
C(231) 1 -0.0631(14) 0.2852(15) 0.0312(8) 0.026(7) Uiso d G
C(232) 1 -0.1440 0.3301 0.0247 0.038(9) Uiso d G
C(233) 1 -0.2085 0.3120 0.0667 0.043(9) Uiso d G
C(234) 1 -0.1920 0.2489 0.1150 0.048(10) Uiso d G
C(235) 1 -0.1111 0.2040 0.1215 0.069(12) Uiso d G
C(236) 1 -0.0467 0.2222 0.0796 0.048(10) Uiso d G
C(241) 1 0.1574(12) 0.3946(15) 0.0109(9) 0.041(9) Uiso d G
C(242) 1 0.2430 0.4179 -0.0192 0.055(10) Uiso d G
C(243) 1 0.3460 0.4792 0.0041 0.034(8) Uiso d G
C(244) 1 0.3633 0.5172 0.0576 0.048(10) Uiso d G
C(245) 1 0.2777 0.4938 0.0876 0.054(10) Uiso d G
C(246) 1 0.1747 0.4325 0.0643 0.036(8) Uiso d G
C(311) 1 0.6979(16) 0.8881(11) 0.2222(9) 0.034(8) Uiso d G
C(312) 1 0.8037 0.9305 0.2524 0.045(9) Uiso d G
C(313) 1 0.8372 1.0278 0.2662 0.073(12) Uiso d G
C(314) 1 0.7649 1.0826 0.2498 0.055(10) Uiso d G
C(315) 1 0.6592 1.0402 0.2196 0.048(10) Uiso d G
C(316) 1 0.6257 0.9430 0.2058 0.049(10) Uiso d G
C(321) 1 0.7700(15) 0.7170(15) 0.2150(10) 0.038(9) Uiso d G
C(322) 1 0.8672 0.7715 0.1968 0.055(10) Uiso d G
C(323) 1 0.9578 0.7376 0.2112 0.081(14) Uiso d G
C(324) 1 0.9511 0.6492 0.2439 0.066(12) Uiso d G
C(325) 1 0.8539 0.5947 0.2621 0.055(10) Uiso d G
C(326) 1 0.7634 0.6286 0.2477 0.055(10) Uiso d G
C(331) 1 0.5904(16) 0.7529(16) 0.1247(7) 0.044(9) Uiso d G
C(332) 1 0.6466 0.7457 0.0831 0.042(9) Uiso d G
C(333) 1 0.5980 0.7474 0.0247 0.074(13) Uiso d G
C(334) 1 0.4931 0.7562 0.0079 0.079(13) Uiso d G
C(335) 1 0.4369 0.7634 0.0494 0.040(9) Uiso d G
C(336) 1 0.4855 0.7617 0.1079 0.048(10) Uiso d G
C(341) 1 0.5485(15) 0.6887(14) 0.2393(9) 0.042(9) Uiso d G
C(342) 1 0.5166 0.7267 0.2809 0.048(10) Uiso d G
C(343) 1 0.4326 0.6679 0.3087 0.085(14) Uiso d G
C(344) 1 0.3805 0.5710 0.2949 0.058(11) Uiso d G
C(345) 1 0.4124 0.5329 0.2534 0.068(12) Uiso d G
C(346) 1 0.4963 0.5918 0.2256 0.043(9) Uiso d G
O(1) 1 0.159(5) -0.374(5) 0.380(3) 0.27(2) Uovl d .
N(1) 1 0.246(7) -0.294(7) 0.443(4) 0.27(2) Uovl d .
C(1) 1 0.241(9) -0.290(8) 0.384(5) 0.27(2) Uovl d .
C(2) 1 0.191(8) -0.363(8) 0.479(4) 0.27(2) Uovl d .
C(3) 1 0.317(8) -0.193(8) 0.445(4) 0.27(2) Uovl d .
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
2 -1 -3
2 5 5
3 2 4
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Te(1) Ta(1) Te(2) 68.20(10) yes
Te(1) Ta(1) Te(3) 67.90(10) yes
Te(2) Ta(1) Te(3) 105.50(10) yes
Te(1) Ta(1) Te(4) 66.10(10) yes
Te(2) Ta(1) Te(4) 105.50(10) yes
Te(3) Ta(1) Te(4) 107.40(10) yes
Te(1) Ta(1) Te(8) 140.50(10) yes
Te(2) Ta(1) Te(8) 78.30(10) yes
Te(3) Ta(1) Te(8) 144.20(10) yes
Te(4) Ta(1) Te(8) 105.60(10) yes
Te(1) Ta(1) Te(9) 141.10(10) yes
Te(2) Ta(1) Te(9) 105.60(10) yes
Te(3) Ta(1) Te(9) 77.80(10) yes
Te(4) Ta(1) Te(9) 145.50(10) yes
Te(8) Ta(1) Te(9) 67.10(10) yes
Te(1) Ta(1) Te(10) 138.60(10) yes
Te(2) Ta(1) Te(10) 145.10(10) yes
Te(3) Ta(1) Te(10) 106.40(10) yes
Te(4) Ta(1) Te(10) 78.00(10) yes
Te(8) Ta(1) Te(10) 67.60(10) yes
Te(9) Ta(1) Te(10) 68.00(10) yes
Ta(1) Te(1) Te(2) 54.30(10) ?
Ta(1) Te(1) Te(3) 54.60(10) ?
Te(2) Te(1) Te(3) 88.60(10) yes
Ta(1) Te(1) Te(4) 55.10(10) ?
Te(2) Te(1) Te(4) 89.70(10) yes
Te(3) Te(1) Te(4) 91.40(10) yes
Ta(1) Te(2) Te(1) 57.50(10) ?
Ta(1) Te(2) Te(5) 101.40(10) ?
Te(1) Te(2) Te(5) 157.40(10) yes
Ta(1) Te(3) Te(1) 57.50(10) ?
Ta(1) Te(3) Te(6) 102.70(10) ?
Te(1) Te(3) Te(6) 158.30(10) yes
Ta(1) Te(4) Te(1) 58.80(10) ?
Ta(1) Te(4) Te(7) 101.70(10) ?
Te(1) Te(4) Te(7) 159.30(10) yes
Te(2) Te(5) Te(8) 76.70(10) yes
Te(3) Te(6) Te(9) 76.00(10) yes
Te(4) Te(7) Te(10) 75.70(10) yes
Ta(1) Te(8) Te(5) 100.90(10) ?
Ta(1) Te(8) Te(9) 56.00(10) ?
Te(5) Te(8) Te(9) 104.20(10) yes
Ta(1) Te(8) Te(10) 56.00(10) ?
Te(5) Te(8) Te(10) 156.30(10) yes
Te(9) Te(8) Te(10) 60.30(10) yes
Ta(1) Te(9) Te(6) 102.10(10) ?
Ta(1) Te(9) Te(8) 56.90(10) ?
Te(6) Te(9) Te(8) 158.90(10) yes
Ta(1) Te(9) Te(10) 56.20(10) ?
Te(6) Te(9) Te(10) 108.40(10) yes
Te(8) Te(9) Te(10) 60.30(10) yes
Ta(1) Te(10) Te(7) 101.20(10) ?
Ta(1) Te(10) Te(8) 56.50(10) ?
Te(7) Te(10) Te(8) 103.10(10) yes
Ta(1) Te(10) Te(9) 55.80(10) ?
Te(7) Te(10) Te(9) 155.8(2) yes
Te(8) Te(10) Te(9) 59.50(10) yes
C(111) P(1) C(121) 112.2(14) ?
C(111) P(1) C(131) 110.0(10) ?
C(121) P(1) C(131) 106.1(12) ?
C(111) P(1) C(141) 108.6(12) ?
C(121) P(1) C(141) 110.6(11) ?
C(131) P(1) C(141) 109.3(13) ?
C(211) P(2) C(221) 111.9(11) ?
C(211) P(2) C(231) 108.7(10) ?
C(221) P(2) C(231) 110.8(10) ?
C(211) P(2) C(241) 108.6(9) ?
C(221) P(2) C(241) 106.7(10) ?
C(231) P(2) C(241) 110.1(10) ?
C(311) P(3) C(321) 110.2(10) ?
C(311) P(3) C(331) 111.5(11) ?
C(321) P(3) C(331) 108.1(12) ?
C(311) P(3) C(341) 109.9(12) ?
C(321) P(3) C(341) 112.5(11) ?
C(331) P(3) C(341) 104.5(9) ?
P(1) C(111) C(112) 122.2(7) ?
P(1) C(111) C(116) 117.5(7) ?
P(1) C(121) C(122) 118.7(8) ?
P(1) C(121) C(126) 121.2(8) ?
P(1) C(131) C(132) 119.2(9) ?
P(1) C(131) C(136) 120.8(9) ?
P(1) C(141) C(142) 120.0(9) ?
P(1) C(141) C(146) 119.9(9) ?
P(2) C(211) C(212) 119.1(6) ?
P(2) C(211) C(216) 120.9(6) ?
P(2) C(221) C(222) 120.0(6) ?
P(2) C(221) C(226) 120.0(6) ?
P(2) C(231) C(232) 122.1(7) ?
P(2) C(231) C(236) 117.8(7) ?
P(2) C(241) C(242) 119.2(8) ?
P(2) C(241) C(246) 120.7(8) ?
P(3) C(311) C(312) 120.6(7) ?
P(3) C(311) C(316) 119.4(7) ?
P(3) C(321) C(322) 121.4(7) ?
P(3) C(321) C(326) 118.5(7) ?
P(3) C(331) C(332) 122.3(8) ?
P(3) C(331) C(336) 117.4(8) ?
P(3) C(341) C(342) 121.2(8) ?
P(3) C(341) C(346) 118.8(8) ?
C(1) N(1) C(2) 132(9) ?
C(1) N(1) C(3) 90(8) ?
C(2) N(1) C(3) 138(10) ?
O(1) C(1) N(1) 91(8) ?
O(1) C(1) C(3) 136(9) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ta(1) Te(1) 2.870(3) yes
Ta(1) Te(2) 2.766(4) yes
Ta(1) Te(3) 2.772(3) yes
Ta(1) Te(4) 2.753(3) yes
Ta(1) Te(8) 2.860(3) yes
Ta(1) Te(9) 2.829(3) yes
Ta(1) Te(10) 2.843(4) yes
Te(1) Te(2) 3.161(4) yes
Te(1) Te(3) 3.153(4) yes
Te(1) Te(4) 3.068(4) yes
Te(2) Te(5) 2.899(4) yes
Te(3) Te(6) 2.873(4) yes
Te(4) Te(7) 2.905(4) yes
Te(5) Te(8) 2.827(5) yes
Te(6) Te(9) 2.841(4) yes
Te(7) Te(10) 2.834(4) yes
Te(8) Te(9) 3.146(4) yes
Te(8) Te(10) 3.171(5) yes
Te(9) Te(10) 3.170(4) yes
P(1) C(111) 1.77(2) ?
P(1) C(121) 1.80(3) ?
P(1) C(131) 1.83(2) ?
P(1) C(141) 1.80(2) ?
P(2) C(211) 1.83(2) ?
P(2) C(221) 1.83(2) ?
P(2) C(231) 1.78(2) ?
P(2) C(241) 1.798(16) ?
P(3) C(311) 1.819(19) ?
P(3) C(321) 1.81(3) ?
P(3) C(331) 1.846(19) ?
P(3) C(341) 1.79(2) ?
O(1) C(1) 1.34(11) ?
N(1) C(1) 1.37(16) ?
N(1) C(2) 1.35(14) ?
N(1) C(3) 1.46(13) ?