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_7038145
_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
'2(C85 H62 Ag  Cl F10 O5 P6 Pt3), C H2 Cl2, 8(C6 H14)'
_chemical_formula_sum            'C109.5 H119 Ag Cl2 F10 O5 P6 Pt3'
_chemical_formula_weight         2654.91
_chemical_name_systematic
; 
 ? 
;
_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                81.8870(10)
_cell_angle_beta                 73.1160(10)
_cell_angle_gamma                82.8390(10)
_cell_formula_units_Z            2
_cell_length_a                   14.1168(7)
_cell_length_b                   19.3240(10)
_cell_length_c                   19.3754(10)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.29
_cell_volume                     4987.5(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      200(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37463
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.07
_exptl_absorpt_coefficient_mu    4.611
_exptl_absorpt_correction_T_max  0.8022
_exptl_absorpt_correction_T_min  0.6310
_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            yellow
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2622
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
 The unit cell contains 8 hexane molecules which have been treated as a 
 diffuse contribution to the overall scattering without specific atom positions
 by SQUEEZE/PLATON
;
_refine_diff_density_max         7.070
_refine_diff_density_min         -2.964
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1049
_refine_ls_number_reflns         17412
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+52.2858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1706
_reflns_number_gt                13536
_reflns_number_total             17412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt02593a1.cif
_cod_data_source_block           ial289sq
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C109.50 H119 Ag Cl2 F10 O5 P6 Pt3'
_cod_database_code               7038145
_platon_squeeze_void_probe_radius 1.20