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_7000235
_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         'C54 H70 N2 P4 Pt, C7 H8'
_chemical_formula_sum            'C61 H78 N2 P4 Pt'
_chemical_formula_weight         1158.22
_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             2007-11-30T11:57:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 125.737(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.336(3)
_cell_length_b                   24.002(5)
_cell_length_c                   18.974(7)
_cell_measurement_reflns_used    14431
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     5669(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k geometry, 4 circle diffractometer'
_diffrn_measurement_device_type  'KM4 CCD'
_diffrn_measurement_method       '\w--scans 0.75\%, 612 frames'
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41630
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    2.627
_exptl_absorpt_correction_T_max  0.614
_exptl_absorpt_correction_T_min  0.53879
_exptl_absorpt_correction_type   numerical
_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            orange
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.245
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         13012
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+19.0456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0752
_reflns_number_gt                12026
_reflns_number_total             13012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b807811d.txt
_cod_data_source_block           compound_13
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7000235