Germanium(II) and Tin(II) Complexes of a Sterically Demanding Phosphanide Ligand
Keith Izod; John Stewart; Ewan R. Clark; William Clegg; Ross W. Harrington; Inorganic Chemistry 49 (2010) 4698–4707; doi:10.1021/ic1003534

data_4315529
_publ_section_title
;
 Germanium(II) and Tin(II) Complexes of a Sterically Demanding Phosphanide
 Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4698
_journal_page_last               4707
_journal_paper_doi               10.1021/ic1003534
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C16 H32 Li O4 +,C39 H72 P3 Si6 Sn -'
_chemical_formula_sum            'C55 H104 Li O4 P3 Si6 Sn'
_chemical_formula_weight         1216.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           219
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F -4a 2 3'
_symmetry_space_group_name_H-M   'F -4 3 c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   39.504(10)
_cell_length_b                   39.504(10)
_cell_length_c                   39.504(10)
_cell_measurement_reflns_used    293
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.50
_cell_volume                     61649(3)
_computing_cell_refinement       EvalCCD
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        EvalCCD
_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_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            36004
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         3.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  0.860
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             20736
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4471
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+722.9248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1456
_reflns_number_gt                2961
_reflns_number_total             4471
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic1003534_si_001_5.cif
_cod_data_source_block           ki312_compound_19a
_cod_original_cell_volume        61649(27)
_cod_database_code               4315529