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_4334875
_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_moiety         'C21 H19 N Pt S, 0.5(C3 H6 O)'
_chemical_formula_sum            'C22.5 H22 N O0.5 Pt S'
_chemical_formula_weight         541.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 101.875(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.5046(14)
_cell_length_b                   9.9891(3)
_cell_length_c                   9.0748(3)
_cell_measurement_reflns_used    8592
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8477
_cell_measurement_theta_min      4.2038
_cell_volume                     3770.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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 0.995
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details
;
  1 omega   -6.00   25.00   1.0000   35.3400
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -99.0000  120.0000 31

  2 omega  -85.00   13.00   1.0000   35.3400
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -77.0000 -120.0000 98

  3 omega   20.00   52.00   1.0000   35.3400
omega____ theta____ kappa____ phi______ frames
    -       22.1490  -99.0000   30.0000 32

  4 omega  -42.00   45.00   1.0000   35.3400
omega____ theta____ kappa____ phi______ frames
    -       22.1490  -85.0000  109.0000 87

  5 omega  -38.00   90.00   1.0000   35.3400
omega____ theta____ kappa____ phi______ frames
    -       22.1490   19.0000   60.0000 128

  6 omega    0.00   44.00   1.0000   35.3400
omega____ theta____ kappa____ phi______ frames
    -       22.1490  -57.0000  120.0000 44

  7 omega  -25.00   25.00   1.0000   35.3400
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -99.0000   60.0000 50

  8 omega  -44.00   51.00   1.0000   35.3400
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   57.0000   30.0000 95

  9 omega  -44.00  -11.00   1.0000   35.3400
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   57.0000 -120.0000 33

 10 omega  -52.00   54.00   1.0000   35.3400
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   37.0000  -30.0000 106

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0017560000
_diffrn_orient_matrix_UB_12      -0.0514401000
_diffrn_orient_matrix_UB_13      -0.0515285000
_diffrn_orient_matrix_UB_21      0.0066847000
_diffrn_orient_matrix_UB_22      -0.0428957000
_diffrn_orient_matrix_UB_23      0.0608173000
_diffrn_orient_matrix_UB_31      -0.0155772000
_diffrn_orient_matrix_UB_32      -0.0240408000
_diffrn_orient_matrix_UB_33      0.0023383000
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23519
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         4.21
_exptl_absorpt_coefficient_mu    7.562
_exptl_absorpt_correction_T_max  0.2346
_exptl_absorpt_correction_T_min  0.1434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.790
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4560
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0182
_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/[\s^2^(Fo^2^)+(0.0200P)^2^+12.2019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0460
_reflns_number_gt                4463
_reflns_number_total             4560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400167w_si_002_1.cif
_cod_data_source_block           1
_cod_original_cell_volume        3770.6(2)
_cod_original_formula_sum        'C22.50 H22 N O0.50 Pt S'
_cod_database_code               4334875