Complexes of germanium(iv) fluoride with phosphane ligands: structural and spectroscopic authentication of germanium(iv) phosphane complexes
Davis, Martin F.; Levason, William; Reid, Gillian; Webster, Michael; Dalton Transactions  (2008) 2261–2269; doi:10.1039/b716765b

data_7003520
_publ_section_title
;
 Complexes of germanium(iv) fluoride with phosphane ligands: structural
 and spectroscopic authentication of germanium(iv) phosphane complexes
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              2261
_journal_page_last               2269
_journal_paper_doi               10.1039/b716765b
_journal_year                    2008
_chemical_formula_moiety         'C6 H18 P2 2+, 2(Cl3 Ge 1-)'
_chemical_formula_sum            'C6 H18 Cl6 Ge2 P2'
_chemical_formula_weight         510.02
_chemical_name_common
'1,2-bis(dimethylphosphonium)ethane bis(trichlorogermanate(ii))'
_chemical_name_systematic
;
1,2-bis(dimethylphosphonium)ethane bis(trichlorogermanate(II))
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2006-11-15
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.0377(13)
_cell_length_b                   12.5498(9)
_cell_length_c                   16.6597(7)
_cell_measurement_reflns_used    4763
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     3771.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'area detector, Nonius Kappa ccd'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2016
_diffrn_reflns_av_sigmaI/netI    0.2750
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29683
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.185
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.031(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         8233
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.2079
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1453
_reflns_number_gt                3819
_reflns_number_total             8233
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b716765b.txt
_cod_data_source_block           06mfd020_[C6H18Cl6Ge2P2]
_cod_database_code               7003520