Synthesis and Characterization of a "Pt3Tl" Cluster Containing an Unprecedented Trigonal Environment for Thallium(I)
Úrsula Belío; Sara Fuertes; Antonio Martín; Inorganic Chemistry 52 (2013) 5627–5629; doi:10.1021/ic400167w

data_4334876
_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       '\w 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/[\s^2^(Fo^2^)+(0.0500P)^2^+43.8638P] where P=(Fo^2^+2Fc^2^)/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