Heteroleptic Chini-Type Platinum Clusters: Synthesis and Characterization of Bis-Phospine Derivatives of [Pt3n(CO)6n](2-) (n = 2-4).
Cesari, Cristiana; Ciabatti, Iacopo; Femoni, Cristina; Iapalucci, Maria Carmela; Mancini, Federica; Zacchini, Stefano; Inorganic chemistry 56 (2017) 1655–1668; doi:10.1021/acs.inorgchem.6b02750

data_4345489
_publ_section_title
;
 Heteroleptic Chini-Type Platinum Clusters: Synthesis and Characterization
 of Bis-Phospine Derivatives of [Pt3n(CO)6n](2-) (n = 2-4).
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1655
_journal_page_last               1668
_journal_paper_doi               10.1021/acs.inorgchem.6b02750
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C64 H76 N2 O18 P2 Pt9'
_chemical_formula_weight         2979.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.341(6)
_cell_length_b                   14.916(3)
_cell_length_c                   17.883(4)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      22.1285
_cell_measurement_theta_min      2.256
_cell_volume                     7827(3)
_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      291(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0703
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            72956
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    16.121
_exptl_absorpt_correction_T_max  0.2284
_exptl_absorpt_correction_T_min  0.1328
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1473 (selected reflections only, before parameter refinement)
 R(int) = 0.0775 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5400
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.024(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         13712
_refine_ls_number_restraints     450
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0326P)^2^+1.9352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                10561
_reflns_number_total             13712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02750_si_002.cif
_cod_data_source_block           '[NEt4]2[Pt9(CO)16(dppe)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        7826(3)
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4345489