Syntheses, Structures, and Electrochemistry of the Defective ccp [Pt33(CO)38](2-) and the bcc [Pt40(CO)40](6-) Molecular Nanoclusters.
Cattabriga, Enrico; Ciabatti, Iacopo; Femoni, Cristina; Funaioli, Tiziana; Iapalucci, Maria Carmela; Zacchini, Stefano; Inorganic chemistry 55 (2016) 6068–6079; doi:10.1021/acs.inorgchem.6b00607

data_4347789
_publ_section_title
;
 Syntheses, Structures, and Electrochemistry of the Defective ccp
 [Pt33(CO)38](2-) and the bcc [Pt40(CO)40](6-) Molecular Nanoclusters.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6068
_journal_page_last               6079
_journal_paper_doi               10.1021/acs.inorgchem.6b00607
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C104 H109 N9 O40 Pt40'
_chemical_formula_weight         9928.60
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                81.061(2)
_cell_angle_beta                 81.175(2)
_cell_angle_gamma                89.248(2)
_cell_formula_units_Z            2
_cell_length_a                   15.778(2)
_cell_length_b                   16.481(2)
_cell_length_c                   28.555(4)
_cell_measurement_reflns_used    9501
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.4135
_cell_measurement_theta_min      2.349
_cell_volume                     7247.9(16)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            80199
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.251
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    38.484
_exptl_absorpt_correction_T_max  0.1010
_exptl_absorpt_correction_T_min  0.0633
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1679 (selected reflections only, before parameter refinement)
 R(int) = 0.0676 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.549
_exptl_crystal_description       prism
_exptl_crystal_F_000             8472
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         4.408
_refine_diff_density_min         -2.797
_refine_diff_density_rms         0.531
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1740
_refine_ls_number_reflns         31343
_refine_ls_number_restraints     199
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0841P)^2^+67.0561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23029
_reflns_number_total             31343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00607_si_002.cif
_cod_data_source_block           p-1
_cod_original_cell_volume        7248.3(18)
_cod_database_code               4347789
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.063
_shelx_estimated_absorpt_t_max   0.101
_shelx_res_checksum              9571
_shelx_hkl_checksum              18468