PPh3-Derivatives of [Pt3n(CO)6n]2- (n= 2-6) Chini's Clusters: Syntheses, Structures, and 31P NMR Studies
Iacopo Ciabatti; Cristina Femoni; Maria Carmela Iapalucci; Giuliano Longoni; Tatiana Lovato; Stefano Zacchini; Inorganic Chemistry 52 (2013) 4384–4395; doi:10.1021/ic3025414

data_4334459
_publ_section_title
;
 PPh3-Derivatives of [Pt3n(CO)6n]2- (n= 2-6) Chini's Clusters: Syntheses,
 Structures, and 31P NMR Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4384
_journal_page_last               4395
_journal_paper_doi               10.1021/ic3025414
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C86 H118 N2 O12 P2 Pt6'
_chemical_formula_weight         2604.30
_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                 108.1410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.3714(9)
_cell_length_b                   13.3264(7)
_cell_length_c                   19.5839(10)
_cell_measurement_reflns_used    3593
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.175
_cell_measurement_theta_min      2.4285
_cell_volume                     4308.3(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1182
_diffrn_reflns_av_sigmaI/netI    0.0954
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39055
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    9.800
_exptl_absorpt_correction_T_max  0.4407
_exptl_absorpt_correction_T_min  0.3031
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_description       plate
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.686
_refine_diff_density_min         -1.292
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8463
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                5663
_reflns_number_total             8463
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3025414_si_001_1.cif
_cod_data_source_block           p21n_[NBu4]2[Pt6(CO)11(PPh3)]thf
_cod_database_code               4334459