From a Zwitterionic Phosphasilene to Base Stabilized Silyliumylidene-Phosphide and Bis(silylene) Complexes
Nora C. Breit; Tibor Szilvási; Tsuyoshi Suzuki; Daniel Gallego; Shigeyoshi Inoue; Journal of the American Chemical Society 135 (2013) 17958–17968; doi:10.1021/ja409720c

data_4121215
_publ_contact_author_address
;
Institut f\"ur Chemie, Technische Universit\"at Berlin, 
Stra\&se des 17. Juni 135, Sekr. C2, D-10623 Berlin
;
_publ_contact_author_email       shigeyoshi.inoue@tu-berlin.de
_publ_contact_author_fax         49-30-314-29732
_publ_contact_author_name        'Shigeyoshi Inoue'
_publ_contact_author_phone       49-30-314-29734
_publ_section_title
;
 From a Zwitterionic Phosphasilene to Base Stabilized
 Silyliumylidene-Phosphide and Bis(silylene) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17958
_journal_page_last               17968
_journal_paper_doi               10.1021/ja409720c
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C126 H154 N4 P6 Pt4 Si6'
_chemical_formula_weight         2859.25
_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_creation_method
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 99.656(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   10.068(5)
_cell_length_b                   24.162(5)
_cell_length_c                   26.174(5)
_cell_measurement_reflns_used    13906
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.4207
_cell_measurement_theta_min      3.2508
_cell_volume                     6277(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            47151
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    4.625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            darkred
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       rod
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.846
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.447
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     670
_refine_ls_number_reflns         11013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.447
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.168
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                9842
_reflns_number_total             11013
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409720c_si_001_1.cif
_cod_data_source_block           c:\compound3
_cod_database_code               4121215