Tetrahedral [HnPt4(CO)4(P∧P)2]n+(n= 1, 2; P∧P = CH2═C(PPh2)2) Cationic Mono- and Dihydrido Carbonyl Clusters Obtained by Protonation of the Neutral Pt4(CO)4(P∧P)2
Ciabatti, Iacopo; Femoni, Cristina; Iapalucci, Maria Carmela; Longoni, Giuliano; Zacchini, Stefano; Organometallics 32 (2013) 5180–; doi:10.1021/om400723w

data_4081452
_publ_section_title
;
 Tetrahedral [HnPt4(CO)4(P&#x2227;P)2]n+(n= 1, 2; P&#x2227;P =
 CH2&#x2550;C(PPh2)2) Cationic Mono- and Dihydrido Carbonyl Clusters
 Obtained by Protonation of the Neutral Pt4(CO)4(P&#x2227;P)2
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5180
_journal_paper_doi               10.1021/om400723w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C81 H66 O6 P6 Pt6'
_chemical_formula_weight         2491.70
_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                 91.3390(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   52.082(3)
_cell_length_b                   12.8563(8)
_cell_length_c                   21.3839(14)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.0975
_cell_measurement_theta_min      2.1775
_cell_volume                     14314.4(15)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'SCHAKAL99 (Keller, 1999)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0714
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -66
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            75942
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    11.872
_exptl_absorpt_correction_T_max  0.3551
_exptl_absorpt_correction_T_min  0.2524
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1396 (selected reflections only, before parameter refinement)
 R(int) = 0.0607 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             9264
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.594
_refine_diff_density_min         -1.427
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         15599
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0593P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1123
_reflns_number_gt                11657
_reflns_number_total             15599
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400723w_si_001.cif
_cod_data_source_block           c2c_cif5
_cod_original_cell_volume        14314.2(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4081452