Reactions of R2P‒P(SiMe3)Li with [(R′3P)2PtCl2]. A general and efficient entry to phosphanylphosphinidene complexes of platinum. Syntheses and structures of [(η2-PPiPr2)Pt(p-Tol3P)2], [(η2-PPtBu2)Pt(p-Tol3P)2], [{η2-PP(NiPr2)2}Pt(p-Tol3P)2] and [{(Et2PhP)2Pt}2P2]
Domańska-Babul, Wioleta; Chojnacki, Jaroslaw; Matern, Eberhard; Pikies, Jerzy; Dalton Transactions  (2009) 146–151; doi:10.1039/b807811d

data_7000238
_publ_section_title
;
 Reactions of R2P--P(SiMe3)Li with [(R&#x2032;3P)2PtCl2]. A general and
 efficient entry to phosphanylphosphinidene complexes of platinum.
 Syntheses and structures of [(\h2-P&#xE001;PiPr2)Pt(p-Tol3P)2],
 [(\h2-P&#xE001;PtBu2)Pt(p-Tol3P)2],
 [{\h2-P&#xE001;P(NiPr2)2}Pt(p-Tol3P)2] and [{(Et2PhP)2Pt}2P2]
;
_journal_issue                   1
_journal_name_full               'Dalton Transactions'
_journal_page_first              146
_journal_page_last               151
_journal_paper_doi               10.1039/b807811d
_journal_year                    2009
_chemical_formula_moiety         'C56 H60 P6 Pt2'
_chemical_formula_sum            'C56 H60 P6 Pt2'
_chemical_formula_weight         1309.04
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-11-30T12:59:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 107.751(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.5441(16)
_cell_length_b                   9.6862(10)
_cell_length_c                   29.7907(17)
_cell_measurement_reflns_used    17040
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.4158
_cell_measurement_theta_min      2.0949
_cell_volume                     5371.1(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.1883
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device       '\k geometry, 4 circle diffractometer'
_diffrn_measurement_device_type  'KM4 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0195339994
_diffrn_orient_matrix_UB_12      0.0493796644
_diffrn_orient_matrix_UB_13      -0.0087736697
_diffrn_orient_matrix_UB_21      0.0325642044
_diffrn_orient_matrix_UB_22      -0.0251419278
_diffrn_orient_matrix_UB_23      0.0157810488
_diffrn_orient_matrix_UB_31      0.003007081
_diffrn_orient_matrix_UB_32      -0.0479401519
_diffrn_orient_matrix_UB_33      -0.0172860068
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1484
_diffrn_reflns_av_unetI/netI     0.144
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            27697
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    5.417
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.427
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            pale-brown
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.0696
_exptl_crystal_size_min          0.0108
_platon_squeeze_details          ' Program fails before normal ending.'
_refine_diff_density_max         4.351
_refine_diff_density_min         -4.018
_refine_diff_density_rms         0.38
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.14
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         9542
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.1777
_refine_ls_R_factor_gt           0.1227
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+407.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2875
_refine_ls_wR_factor_ref         0.3115
_reflns_number_gt                6149
_reflns_number_total             9542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b807811d.txt
_cod_data_source_block           compound_14
_cod_database_code               7000238