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_7003521
_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 H17 O2 P2 1+, Cl3 Ge 1-'
_chemical_formula_sum            'C6 H17 Cl3 Ge O2 P2'
_chemical_formula_weight         362.08
_chemical_name_common
;
(2-(dimethylphosphinoyl)ethyl)-hydroxy-dimethylphosphonium
trichloridogermanate(ii)
;
_chemical_name_systematic
;
(2-(dimethylphosphinoyl)ethyl)-hydroxy-dimethylphosphonium
trichloridogermanate(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2007-10-05
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                66.397(10)
_cell_angle_beta                 89.283(10)
_cell_angle_gamma                60.695(10)
_cell_formula_units_Z            2
_cell_length_a                   9.0978(15)
_cell_length_b                   9.2599(15)
_cell_length_c                   11.1713(15)
_cell_measurement_reflns_used    23743
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     731.9(2)
_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
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11628
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.836
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         3353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0088P)^2^+0.8933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0590
_reflns_number_gt                2956
_reflns_number_total             3353
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b716765b.txt
_cod_data_source_block           07mfd020_[C6H17Cl3GeO2P2]
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003521