Dynamic Behavior of Intramolecularly Base-Stabilized Phosphatetrylenes. Insights into the Inversion Processes of Trigonal Pyramidal Geramanium(II) and Tin(II) Centers
Izod, Keith; Stewart, John; Clark, Ewan R.; McFarlane, William; Allen, Ben; Clegg, William; Harrington, Ross W.; Organometallics 28 (2009) 3327–; doi:10.1021/om8011757

data_4068950
_publ_section_title
;
 Dynamic Behavior of Intramolecularly Base-Stabilized Phosphatetrylenes.
 Insights into the Inversion Processes of Trigonal Pyramidal
 Geramanium(II) and Tin(II) Centers
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3327
_journal_paper_doi               10.1021/om8011757
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C32 H62 N2 P2 Si4 Sn'
_chemical_formula_sum            'C32 H62 N2 P2 Si4 Sn'
_chemical_formula_weight         767.83
_chemical_name_systematic
;
 ?
;
_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                90.789(2)
_cell_angle_beta                 90.187(2)
_cell_angle_gamma                101.872(2)
_cell_formula_units_Z            4
_cell_length_a                   12.7543(6)
_cell_length_b                   12.8444(6)
_cell_length_c                   25.4612(12)
_cell_measurement_reflns_used    23295
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.20
_cell_volume                     4081.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34437
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.884
_refine_diff_density_min         -0.996
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00070(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         18159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.9422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                14131
_reflns_number_total             18159
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om8011757_si_002.cif
_cod_data_source_block           ki82_compound8
_cod_database_code               4068950