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_4068949
_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         'C16 H31 Cl Ge N P Si2'
_chemical_formula_sum            'C16 H31 Cl Ge N P Si2'
_chemical_formula_weight         432.61
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.099(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1002(6)
_cell_length_b                   10.1387(3)
_cell_length_c                   11.5197(4)
_cell_measurement_reflns_used    7807
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      2.72
_cell_volume                     2143.32(13)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_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      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Oxford Diffraction Gemini A Ultra diffractometer'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'sealed tube with Enhance optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3740
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.72
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.738
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro and Scalepack'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.417
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0014(6)
_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   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+16.6315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1556
_reflns_number_gt                3270
_reflns_number_total             3740
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om8011757_si_002.cif
_cod_data_source_block           ki341_compound5
_cod_original_cell_volume        2143.32(12)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4068949