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_4121216
_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            'C55 H83 N4 Ni P Si3'
_chemical_formula_weight         974.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
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                89.804(7)
_cell_angle_beta                 80.657(7)
_cell_angle_gamma                69.810(8)
_cell_formula_units_Z            2
_cell_length_a                   12.2099(11)
_cell_length_b                   13.6641(11)
_cell_length_c                   18.0233(17)
_cell_measurement_reflns_used    1793
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.3734
_cell_measurement_theta_min      3.3077
_cell_volume                     2780.3(5)
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_sigmaI/netI    0.1602
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22278
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       rod
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.535
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         9773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1562
_reflns_number_gt                6179
_reflns_number_total             9773
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409720c_si_001_2.cif
_cod_data_source_block           c:\compound5
_cod_original_cell_volume        2780.3(4)
_cod_original_formula_sum        'C27.50 H41.50 N2 Ni0.50 P0.50 Si1.50'
_cod_database_code               4121216