Germanium/Phosphorus Cage Compounds with Germanium in Three Different Oxidation States
Stefan Almstatter; Balazs Gabor; Michael Bodensteiner; Manfred Scheer; Chem.Commun. 47 (2011) 9998–; doi:10.1039/c1cc13937a

data_7106827
_publ_section_title
;
 Germanium/Phosphorus Cage Compounds with Germanium in Three Different
 Oxidation States
;
_journal_name_full               Chem.Commun.
_journal_page_first              9998
_journal_paper_doi               10.1039/c1cc13937a
_journal_volume                  47
_journal_year                    2011
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C16 H36 Cl6 Ge7 P4, C6 H14'
_chemical_formula_sum            'C22 H50 Cl6 Ge7 P4'
_chemical_formula_weight         1159.33
_chemical_name_systematic        ?
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      147
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.2614(4)
_cell_length_b                   14.2614(4)
_cell_length_c                   11.0241(2)
_cell_measurement_reflns_used    1543
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      62.8672
_cell_measurement_theta_min      3.5678
_cell_volume                     1941.77(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
;
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1993)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.826
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3245
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        63.07
_diffrn_reflns_theta_max         63.07
_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    11.567
_exptl_absorpt_correction_T_max  0.630
_exptl_absorpt_correction_T_min  0.209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.30.3 (release 12-05-2006 CrysAlis171 .NET)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_platon_squeeze_details
;
The struture contains severly disordered hexane molecules.
;
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0493P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                1154
_reflns_number_total             1745
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            c1cc13937a.txt
_cod_data_source_block           al91
_cod_database_code               7106827