#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:53:03 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179819 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/15/7011556.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7011556
loop_
_publ_author_name
'Mitzel, Norbert W.'
'Vojinović, Krunoslav'
_publ_section_title
;
 (4+4)-Coordinate germanium atoms in tetrakis(dialkylaminoxy)germanes
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2341
_journal_paper_doi               10.1039/b201472f
_journal_year                    2002
_chemical_formula_sum            'C12 H28 Ge O4'
_chemical_formula_weight         308.93
_chemical_name_systematic
; 
Tetrakis(isopropoxy)germane
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   difmap
_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                   8.0693(6)
_cell_length_b                   8.0693(6)
_cell_length_c                   24.7868(13)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.3
_cell_measurement_theta_min      23.0
_cell_volume                     1613.96(19)
_computing_cell_refinement       'Nonius-CAD4 Software'
_computing_data_collection       'Nonius-CAD4 Software'
_computing_data_reduction        'XCAD4P, Harms, Marburg'
_computing_molecular_graphics    'SHELXTL 5.01'
_computing_publication_material  'SHELXTL 5.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NONIUS Turbo CAD4'
_diffrn_measurement_method       omega-2theta-scans
_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  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4677
_diffrn_reflns_theta_full        30.09
_diffrn_reflns_theta_max         30.09
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.900
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.127
_exptl_absorpt_correction_type   'DELABS from PLATON'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cylinder
_exptl_crystal_F_000             656
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.789
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0355
_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/[σ²(Fo²)+(0.0623P)²+0.4053P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                1101
_reflns_number_total             1185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b201472f.txt
_cod_data_source_block           kruno9
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      I41/a
_cod_database_code               7011556
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge Ge 0.5000 0.7500 0.1250 0.02018(13) Uani 1 4 d S . .
O O 0.31888(15) 0.77057(14) 0.08714(4) 0.0291(2) Uani 1 1 d . . .
C1 C 0.2787(2) 0.92894(18) 0.06301(6) 0.0259(3) Uani 1 1 d . . .
H1 H 0.363(3) 1.011(3) 0.0700(9) 0.029(5) Uiso 1 1 d . . .
C2 C 0.1212(3) 0.9908(3) 0.08895(9) 0.0412(4) Uani 1 1 d . . .
H2A H 0.026(5) 0.909(5) 0.0819(14) 0.074(10) Uiso 1 1 d . . .
H2B H 0.089(4) 1.101(4) 0.0754(11) 0.054(7) Uiso 1 1 d . . .
H2C H 0.138(5) 1.004(4) 0.1300(11) 0.048(8) Uiso 1 1 d . . .
C3 C 0.2633(3) 0.9033(2) 0.00283(7) 0.0432(5) Uani 1 1 d . . .
H3A H 0.233(4) 0.999(4) -0.0152(14) 0.051(7) Uiso 1 1 d . . .
H3B H 0.363(4) 0.858(4) -0.0109(12) 0.055(8) Uiso 1 1 d . . .
H3C H 0.168(4) 0.831(4) -0.0035(13) 0.059(8) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge 0.02025(15) 0.02025(15) 0.02004(17) 0.000 0.000 0.000
O 0.0334(6) 0.0208(5) 0.0331(5) 0.0048(4) -0.0130(4) -0.0042(4)
C1 0.0300(7) 0.0194(6) 0.0282(6) 0.0033(5) -0.0077(5) -0.0017(5)
C2 0.0428(10) 0.0302(9) 0.0506(10) 0.0016(7) 0.0057(8) 0.0056(8)
C3 0.0703(15) 0.0318(9) 0.0274(7) 0.0029(6) -0.0066(8) 0.0068(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O Ge O 106.82(4) . 12_766 ?
O Ge O 114.92(8) . 6_564 ?
O Ge O 106.82(4) 12_766 6_564 ?
O Ge O 106.82(4) . 15_565 ?
O Ge O 114.92(8) 12_766 15_565 ?
O Ge O 106.82(4) 6_564 15_565 ?
C1 O Ge 119.58(9) . . ?
O C1 C2 107.73(13) . . ?
O C1 C3 107.79(13) . . ?
C2 C1 C3 113.35(16) . . ?
O C1 H1 111.8(13) . . ?
C2 C1 H1 107.0(14) . . ?
C3 C1 H1 109.3(13) . . ?
C1 C2 H2A 110(2) . . ?
C1 C2 H2B 112.1(17) . . ?
H2A C2 H2B 109(3) . . ?
C1 C2 H2C 110(2) . . ?
H2A C2 H2C 109(3) . . ?
H2B C2 H2C 106(3) . . ?
C1 C3 H3A 113(2) . . ?
C1 C3 H3B 109.6(19) . . ?
H3A C3 H3B 112(3) . . ?
C1 C3 H3C 107.8(19) . . ?
H3A C3 H3C 102(3) . . ?
H3B C3 H3C 113(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge O 1.7449(11) . ?
Ge O 1.7448(11) 12_766 ?
Ge O 1.7448(11) 6_564 ?
Ge O 1.7449(11) 15_565 ?
O C1 1.4477(18) . ?
C1 C2 1.509(3) . ?
C1 C3 1.511(2) . ?
C1 H1 0.97(2) . ?
C2 H2A 1.03(4) . ?
C2 H2B 0.99(3) . ?
C2 H2C 1.03(3) . ?
C3 H3A 0.92(4) . ?
C3 H3B 0.95(3) . ?
C3 H3C 0.98(3) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O Ge O C1 163.34(13) 12_766 . . . ?
O Ge O C1 -78.39(11) 6_564 . . . ?
O Ge O C1 39.89(9) 15_565 . . . ?
Ge O C1 C2 -115.56(14) . . . . ?
Ge O C1 C3 121.79(14) . . . . ?
