Metal Scrambling in the Trinuclear {Pt2Se2M} (M = Pt, Pd, Au) System Using an Electrospray Mass Spectrometry (ESMS) Directed Synthetic Methodology; Isolation and Crystallographic Characterization of {Pt2(μ3-Se)2(PPh3)4[Pt(cod)]}{PF6}2 and {Pt(μ3-Se)2(PPh3)2[Pt(cod)]2}{PF6}2 (cod = Cyclo-octa-1,5-diene)
Jeremy S. L. Yeo; Jagadese J. Vittal; William Henderson; T. S. Andy Hor; Inorganic Chemistry 41 (2002) 1194–1198; doi:10.1021/ic010905t

data_4317627
_publ_section_title
;
 Metal Scrambling in the Trinuclear {Pt2Se2M} (M = Pt, Pd, Au) System
 Using an Electrospray Mass Spectrometry (ESMS) Directed Synthetic
 Methodology; Isolation and Crystallographic Characterization of
 {Pt2(\m3-Se)2(PPh3)4[Pt(cod)]}{PF6}2 and
 {Pt(\m3-Se)2(PPh3)2[Pt(cod)]2}{PF6}2 (cod = Cyclo-octa-1,5-diene)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1194
_journal_page_last               1198
_journal_paper_doi               10.1021/ic010905t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C82.5 H84 Cl5 F12 O3.5 P6 Pt3 Se2'
_chemical_formula_weight         2465.76
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.272(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.693(3)
_cell_length_b                   23.952(4)
_cell_length_c                   21.129(4)
_cell_measurement_reflns_used    9046
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.25
_cell_volume                     8952(3)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_method       '\w 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  0.0655
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            51943
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    5.818
_exptl_absorpt_correction_T_max  0.6195
_exptl_absorpt_correction_T_min  0.3550
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle, cut'
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.961
_refine_diff_density_min         -1.103
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         15750
_refine_ls_number_restraints     372
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                10184
_reflns_number_total             15750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010905t_2.cif
_cod_data_source_block           1050
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C82.50 H84 Cl5 F12 O3.50 P6 Pt3 Se2'
_cod_database_code               4317627