Syntheses of new hexacoordinate germanium(IV) complexes. Crystal structures and properties of [GeCl4(TMEDA)] and [GeCl2(N3)2(TMEDA)]
Ejfler, Jolanta; Szafert, Slawomir; Jiao, Haijun; Sobota, Piotr; New Journal of Chemistry 26 (2002) 803–; doi:10.1039/b110770b

data_7050798
_publ_section_title
;
 Syntheses of new hexacoordinate germanium(IV) complexes. Crystal
 structures and properties of [GeCl4(TMEDA)] and [GeCl2(N3)2(TMEDA)]
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              803
_journal_paper_doi               10.1039/b110770b
_journal_volume                  26
_journal_year                    2002
_chemical_formula_moiety         'C6 H16 Cl2 Ge N8'
_chemical_formula_sum            'C6 H16 Cl2 Ge N8'
_chemical_formula_weight         343.76
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 108.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.570(2)
_cell_length_b                   13.350(3)
_cell_length_c                   12.227(2)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     1325.6(5)
_computing_cell_refinement       'KUMA KM4 software'
_computing_data_collection       'KUMA KM4 software'
_computing_data_reduction        'KUMA KM4 software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.476
_diffrn_measured_fraction_theta_max 0.476
_diffrn_measurement_device_type  'KUMA KM4'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_sigmaI/netI    0.0927
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2511
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        no
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.707
_exptl_absorpt_correction_T_max  no
_exptl_absorpt_correction_T_min  no
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needles
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+3.5439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                1000
_reflns_number_total             1174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110770b.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'no' was replaced with
'none' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+3.5439P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+3.5439P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7050798