Polynuclear platinum phosphanido/phosphinito complexes: formation of P-O and P-O-P bonds through reductive coupling processes.
Ara, Irene; Forniés, Juan; Ibáñez, Susana; Mastrorilli, Piero; Todisco, Stefano; Gallo, Vito; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2156–2171; doi:10.1039/c5dt02593a

data_7038146
_publ_section_title
;
 Polynuclear platinum phosphanido/phosphinito complexes: formation of P-O
 and P-O-P bonds through reductive coupling processes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2156
_journal_page_last               2171
_journal_paper_doi               10.1039/c5dt02593a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C120 H80 Cl2 F20 O2 P8 Pt6 2(C16 H36 N) 2(C3 H6 O) 1.5(C6 H14)'
_chemical_formula_sum            'C83.5 H92.5 Cl F10 N O2 P4 Pt3'
_chemical_formula_weight         2076.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-09 deposited with the CCDC.
2015-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                97.7560(10)
_cell_angle_beta                 95.6760(10)
_cell_angle_gamma                97.0240(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7673(6)
_cell_length_b                   14.5107(7)
_cell_length_c                   26.1772(13)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.35
_cell_measurement_theta_min      4.44
_cell_volume                     4365.3(4)
_computing_cell_refinement       'SAINT+ 6.02 (Bruker AXS, 1999)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ 6.02 (Bruker AXS, 1999)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.10 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.10 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            32602
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    4.963
_exptl_absorpt_correction_T_max  0.8654
_exptl_absorpt_correction_T_min  0.3821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Area-Detector Absorption Correction. Bruker-AXS
within SAINT+ package, v. 6.02 (1999).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2035
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.785
_refine_diff_density_min         -1.916
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         15258
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0502P)^2^+21.2791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                12176
_reflns_number_total             15258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02593a1.cif
_cod_data_source_block           ial291a
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C83.50 H92.50 Cl F10 N O2 P4 Pt3'
_cod_database_code               7038146