Donor-Stabilized Silyl Cations. 10. Pentacoordinate Siliconium-Ion Salts with a Triphenylphosphinimino-NLigand Group: Two-Bond P−N−Si Coupling as a Measure for Coordination Strength1
Sivaramakrishna, Akella; Kalikhman, Inna; Kertsnus, Evgenia; Korlyukov, Alexander A.; Kost, Daniel; Organometallics 25 (2006) 3665–; doi:10.1021/om0601347

data_4075220
_publ_section_title
;
 Donor-Stabilized Silyl Cations. 10. Pentacoordinate Siliconium-Ion Salts
 with a Triphenylphosphinimino-NLigand Group:&#x00A0; Two-Bond
 P&#x2212;N&#x2212;Si Coupling as a Measure for Coordination Strength1
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3665
_journal_paper_doi               10.1021/om0601347
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety
'C53 H47 N4 O2 P2 Si1, +1, Cl, -1, 3.5(CHCl3), 0.5((C2H5)2O)'
_chemical_formula_sum            'C58.5 H55.5 Cl11.5 N4 O2.5 P2 Si'
_chemical_formula_weight         1352.27
_chemical_melting_point          71.5(15)
_chemical_name_common            16
_chemical_name_systematic
;
 Bis[N-(triphenylphosphinimino)phenylacetimidato-N',O]methylsiliconium chloride
;
_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
_cell_angle_alpha                61.488(4)
_cell_angle_beta                 68.668(4)
_cell_angle_gamma                83.820(6)
_cell_formula_units_Z            2
_cell_length_a                   14.167(4)
_cell_length_b                   16.592(3)
_cell_length_c                   17.193(4)
_cell_measurement_reflns_used    868
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.04
_cell_measurement_theta_min      2.75
_cell_volume                     3297.1(14)
_computing_cell_refinement       'SAINTPlus (Bruker, 1998a)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Smart 1000  CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26714
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.8904
_exptl_absorpt_correction_T_min  0.8904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1998a)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         14364
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+2.945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1369
_reflns_number_gt                7030
_reflns_number_total             14364
_reflns_threshold_expression     I>2u(I)
_cod_data_source_file            om0601347si20060511_094428.cif
_cod_data_source_block           16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '70-73' was changed to '71.5(15)' -
the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Triclinic' changed to
'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3297.0(14)
_cod_original_formula_sum        'C58.50 H55.50 Cl11.50 N4 O2.50 P2 Si'
_cod_database_code               4075220