Synthesis and structural characterisation of germanium(II) halide complexes with neutral N-donor ligands.
Cheng, Fei; Dyke, John M.; Ferrante, Francesco; Hector, Andrew L.; Levason, William; Reid, Gillian; Webster, Michael; Zhang, Wenjian; Dalton transactions (Cambridge, England : 2003) 39 (2010) 847–856; doi:10.1039/b911016j

data_7024099
_publ_section_title
;
 Synthesis and structural characterisation of germanium(II) halide
 complexes with neutral N-donor ligands.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              847
_journal_page_last               856
_journal_paper_doi               10.1039/b911016j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C9 H23 Cl Ge N3 1+, Cl3 Ge 1-'
_chemical_formula_sum            'C9 H23 Cl4 Ge2 N3'
_chemical_formula_weight         460.28
_chemical_name_common
;
chloro(N,N,N',N'',N''-pentamethyl-
diethylenetriamine)germanium(ii) trichlorogermanate(ii)
;
_chemical_name_systematic
;
chloro(N,N,N',N",N"-pentamethyl-diethylenetriamine)germanium(II)
trichlorogermanate(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             2007-11-20
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                112.008(10)
_cell_angle_beta                 98.953(10)
_cell_angle_gamma                93.393(15)
_cell_formula_units_Z            2
_cell_length_a                   6.3451(10)
_cell_length_b                   11.813(2)
_cell_length_c                   13.166(3)
_cell_measurement_reflns_used    16701
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     896.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0671
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13899
_diffrn_reflns_theta_full        27.74
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         3.40
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.938
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6744
_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    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0000P)^2^+7.6800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                3115
_reflns_number_total             4100
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b911016j.txt
_cod_data_source_block           07wz201
_cod_original_cell_volume        896.4(3)
_cod_database_code               7024099