#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:31:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179451 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/48/4334876.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_4334876
loop_
_publ_author_name
'Úrsula Belío'
'Sara Fuertes'
'Antonio Martín'
_publ_section_title
;
 Synthesis and Characterization of a "Pt3Tl" Cluster Containing an
 Unprecedented Trigonal Environment for Thallium(I)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5627
_journal_page_last               5629
_journal_paper_doi               10.1021/ic400167w
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C63 H57 F6 N3 P Pt3 S3 Tl'
_chemical_formula_weight         1886.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           190
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_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            2
_cell_length_a                   15.6681(8)
_cell_length_b                   15.6681(8)
_cell_length_c                   13.2867(8)
_cell_measurement_reflns_used    7424
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7336
_cell_measurement_theta_min      4.2587
_cell_volume                     2824.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -24.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928   19.0000 -150.0000 120

  2 omega    5.00   37.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928  -57.0000  -90.0000 32

  3 omega  -91.00  -22.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -57.0000    0.0000 69

  4 omega  -52.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   37.0000  150.0000 106

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0100490000
_diffrn_orient_matrix_UB_12      -0.0437666000
_diffrn_orient_matrix_UB_13      0.0258830000
_diffrn_orient_matrix_UB_21      0.0443965000
_diffrn_orient_matrix_UB_22      0.0040916000
_diffrn_orient_matrix_UB_23      -0.0189094000
_diffrn_orient_matrix_UB_31      0.0256915000
_diffrn_orient_matrix_UB_32      0.0282981000
_diffrn_orient_matrix_UB_33      0.0428364000
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14729
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         4.26
_exptl_absorpt_coefficient_mu    10.453
_exptl_absorpt_correction_T_max  0.1719
_exptl_absorpt_correction_T_min  0.0995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.830
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1939
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0500P)²+43.8638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                1904
_reflns_number_total             1939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400167w_si_002_2.cif
_cod_data_source_block           2
_cod_database_code               4334876
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'
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
Pt Pt 0.45186(4) 0.57123(4) 0.7500 0.01292(14) Uani 1 2 d S
Tl Tl 0.3333 0.6667 0.7500 0.0185(2) Uani 1 6 d S
S S 0.3140(3) 0.4211(3) 0.7500 0.0187(8) Uani 1 2 d S
N N 0.5869(9) 0.6893(9) 0.7500 0.022(3) Uani 1 2 d S
C1 C 0.4702(9) 0.5971(8) 0.5965(8) 0.028(2) Uani 1 1 d U
C2 C 0.4036(10) 0.5617(9) 0.5160(8) 0.034(3) Uani 1 1 d U
H2 H 0.3384 0.5098 0.5288 0.041 Uiso 1 1 calc R
C3 C 0.4276(13) 0.5983(12) 0.4189(10) 0.046(3) Uani 1 1 d U
H3 H 0.3798 0.5735 0.3667 0.056 Uiso 1 1 calc R
C4 C 0.5241(14) 0.6726(13) 0.4000(14) 0.061(4) Uani 1 1 d U
H4 H 0.5439 0.6942 0.3328 0.073 Uiso 1 1 calc R
C5 C 0.5931(13) 0.7163(13) 0.4794(13) 0.053(4) Uani 1 1 d U
H5 H 0.6571 0.7706 0.4668 0.063 Uiso 1 1 calc R
C6 C 0.5658(9) 0.6789(9) 0.5740(10) 0.031(3) Uani 1 1 d U
C7 C 0.6311(8) 0.7235(8) 0.6598(10) 0.028(3) Uani 1 1 d U
C8 C 0.7322(10) 0.7959(10) 0.6609(13) 0.042(3) Uani 1 1 d U
H8 H 0.7665 0.8175 0.5988 0.051 Uiso 1 1 calc R
C9 C 0.7830(16) 0.8365(17) 0.7500 0.050(5) Uani 1 2 d SU
H9 H 0.8492 0.8894 0.7500 0.060 Uiso 1 2 calc SR
C10 C 0.3225(11) 0.3459(10) 0.6482(10) 0.041(3) Uani 1 1 d U
H10A H 0.2690 0.3284 0.5987 0.050 Uiso 1 1 calc R
H10B H 0.3865 0.3833 0.6130 0.050 Uiso 1 1 calc R
C11 C 0.313(2) 0.255(2) 0.6936(4) 0.106(8) Uani 1 1 d DU
H11A H 0.3689 0.2472 0.6697 0.127 Uiso 1 1 calc R
H11B H 0.2516 0.1977 0.6697 0.127 Uiso 1 1 calc R
P P 0.0000 0.0000 0.5000 0.0311(14) Uani 1 6 d SD
F1 F 0.0000 0.0000 0.6176(10) 0.103(5) Uani 1 3 d SD
F2 F 0.062(4) -0.050(4) 0.466(2) 0.103(5) Uani 0.33 1 d PD
F3 F 0.1005(13) 0.1005(13) 0.5000 0.103(5) Uani 0.33 2 d SPD
F3' F -0.0998(13) -0.0998(13) 0.5000 0.103(5) Uani 0.33 2 d SPD
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'
F F 0.0171 0.0103 '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'
Pt Pt -1.7033 8.3905 '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
N Pt C1 80.8(3) . 4_556
N Pt C1 80.8(3) . .
C1 Pt C1 159.9(6) 4_556 .
N Pt S 169.1(3) . .
C1 Pt S 99.8(3) 4_556 .
C1 Pt S 99.8(3) . .
N Pt Tl 100.2(3) . .
C1 Pt Tl 87.8(3) 4_556 .
C1 Pt Tl 87.8(3) . .
S Pt Tl 90.68(10) . .
Pt Tl Pt 120.0 2_665 3_565
Pt Tl Pt 120.0 2_665 .
Pt Tl Pt 120.0 3_565 .
C10 S C10 94.5(9) . 4_556
C10 S Pt 109.2(5) . .
C10 S Pt 109.2(5) 4_556 .
C7 N C7 124.6(14) 4_556 .
C7 N Pt 117.6(7) 4_556 .
C7 N Pt 117.6(7) . .
C2 C1 C6 115.8(10) . .
C2 C1 Pt 132.1(9) . .
C6 C1 Pt 111.1(8) . .
C3 C2 C1 123.5(13) . .
C2 C3 C4 118.0(15) . .
C3 C4 C5 121.1(16) . .
C6 C5 C4 118.6(16) . .
C5 C6 C1 122.6(14) . .
C5 C6 C7 121.4(13) . .
C1 C6 C7 115.9(11) . .
N C7 C8 117.1(13) . .
N C7 C6 113.9(10) . .
C8 C7 C6 129.0(12) . .
C9 C8 C7 122.1(15) . .
C8 C9 C8 117(2) . 4_556
C11 C10 S 108.1(10) . .
C10 C11 C11 114.0(7) . 4_556
F1 P F1 180.000(2) 7_556 .
F1 P F3' 90.000(1) 7_556 3
F1 P F3' 90.000(2) . 3
F1 P F3' 90.000(5) 7_556 .
F1 P F3' 90.000(5) . .
F3' P F3' 120.0 3 .
F1 P F3' 90.000(1) 7_556 2
F1 P F3' 90.000(2) . 2
F3' P F3' 120.000(5) 3 2
F3' P F3' 120.000(2) . 2
F1 P F3 90.000(4) 7_556 .
F1 P F3 90.000(5) . .
F3' P F3 60.000(2) 3 .
F3' P F3 180(2) . .
F3' P F3 60.000(2) 2 .
F1 P F3 90.000(2) 7_556 2
F1 P F3 90.000(1) . 2
F3' P F3 60.000(2) 3 2
F3' P F3 60.000(2) . 2
F3' P F3 180.000(3) 2 2
F3 P F3 120.000(2) . 2
F1 P F3 90.000(2) 7_556 3
F1 P F3 90.000(1) . 3
F3' P F3 180.000(3) 3 3
F3' P F3 60.000(2) . 3
F3' P F3 60.000(2) 2 3
F3 P F3 120.000(2) . 3
F3 P F3 120.000(6) 2 3
F1 P F2 106.4(11) 7_556 8_556
F1 P F2 73.6(11) . 8_556
F3' P F2 93(2) 3 8_556
F3' P F2 143(2) . 8_556
F3' P F2 31(2) 2 8_556
F3 P F2 37(2) . 8_556
F3 P F2 149(2) 2 8_556
F3 P F2 87(2) 3 8_556
F1 P F2 73.6(11) 7_556 2
F1 P F2 106.4(11) . 2
F3' P F2 31(2) 3 2
F3' P F2 143(2) . 2
F3' P F2 93(2) 2 2
F3 P F2 37(2) . 2
F3 P F2 87(2) 2 2
F3 P F2 149(2) 3 2
F2 P F2 74(4) 8_556 2
F1 P F2 106.4(11) 7_556 7_556
F1 P F2 73.6(11) . 7_556
F3' P F2 31(2) 3 7_556
F3' P F2 93(2) . 7_556
F3' P F2 143(2) 2 7_556
F3 P F2 87(2) . 7_556
F3 P F2 37(2) 2 7_556
F3 P F2 149(2) 3 7_556
F2 P F2 112.4(10) 8_556 7_556
F2 P F2 62(4) 2 7_556
F1 P F2 73.6(11) 7_556 3
F1 P F2 106.4(11) . 3
F3' P F2 93(2) 3 3
F3' P F2 31(2) . 3
F3' P F2 143(2) 2 3
F3 P F2 149(2) . 3
F3 P F2 37(2) 2 3
F3 P F2 87(2) 3 3
F2 P F2 173(5) 8_556 3
F2 P F2 112.4(10) 2 3
F2 P F2 74(4) 7_556 3
F3' F2 F3 117(3) 2 3
F3' F2 P 73.4(17) 2 .
F3 F2 P 71.1(15) 3 .
F3' F2 F2 14.1(18) 2 8_556
F3 F2 F2 109(3) 3 8_556
P F2 F2 59(2) . 8_556
F2 F3 F2 144(3) 2 8_556
F2 F3 F3' 28(2) 2 3
F2 F3 F3' 124.6(17) 8_556 3
F2 F3 F3' 124.6(17) 2 2
F2 F3 F3' 28(2) 8_556 2
F3' F3 F3' 119.3(13) 3 2
F2 F3 P 72.0(16) 2 .
F2 F3 P 72.0(16) 8_556 .
F3' F3 P 59.7(7) 3 .
F3' F3 P 59.7(7) 2 .
F2 F3' F2 152(4) 9_556 3
F2 F3' P 75.9(18) 9_556 .
F2 F3' P 75.9(18) 3 .
F2 F3' F3 126(2) 9_556 2
F2 F3' F3 35(3) 3 2
P F3' F3 60.3(7) . 2
F2 F3' F3 35(3) 9_556 3
F2 F3' F3 126(2) 3 3
P F3' F3 60.3(7) . 3
F3 F3' F3 120.7(13) 2 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt N 1.996(13) .
Pt C1 2.072(10) 4_556
Pt C1 2.072(10) .
Pt S 2.262(4) .
Pt Tl 2.9088(5) .
Tl Pt 2.9088(5) 2_665
Tl Pt 2.9088(5) 3_565
S C10 1.842(13) .
S C10 1.842(13) 4_556
N C7 1.353(14) 4_556
N C7 1.353(14) .
C1 C2 1.400(16) .
C1 C6 1.433(16) .
C2 C3 1.386(18) .
C3 C4 1.39(2) .
C4 C5 1.42(3) .
C5 C6 1.36(2) .
C6 C7 1.456(19) .
C7 C8 1.414(17) .
C8 C9 1.39(2) .
C9 C8 1.39(2) 4_556
C10 C11 1.48(3) .
C11 C11 1.498(10) 4_556
P F1 1.562(14) 7_556
P F1 1.562(14) .
P F3' 1.56(2) 3
P F3' 1.56(2) .
P F3' 1.56(2) 2
P F3 1.57(2) .
P F3 1.57(2) 2
P F3 1.57(2) 3
P F2 1.582(19) 8_556
P F2 1.582(19) 2
P F2 1.582(19) 7_556
P F2 1.582(19) 3
F2 F3' 0.84(6) 2
F2 F3 1.00(6) 3
F2 F2 1.62(10) 8_556
F3 F2 1.00(6) 2
F3 F2 1.00(6) 8_556
F3 F3' 1.569(17) 3
F3 F3' 1.569(17) 2
F3' F2 0.84(6) 9_556
F3' F2 0.84(6) 3
F3' F3 1.569(17) 2
F3' F3 1.569(17) 3
