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_7050797
_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 Cl4 Ge N2'
_chemical_formula_sum            'C6 H16 Cl4 Ge N2'
_chemical_formula_weight         330.60
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.633(2)
_cell_length_b                   7.328(3)
_cell_length_c                   11.7250(10)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      9
_cell_volume                     1257.3(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1672
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        no
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.248
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   COSABS99
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needles
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.646
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1603
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1642
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+4.2083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1418
_reflns_number_gt                718
_reflns_number_total             1603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b110770b.txt
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'orthorombic' was replaced with
'orthorhombic' 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^)+(0.0457P)^2^+4.2083P] 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^)+(0.0457P)^2^+4.2083P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               7050797