#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:11:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179743 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/39/7003909.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_7003909
loop_
_publ_author_name
'Jones, Cameron'
'Rose, Richard P.'
'Stasch, Andreas'
_publ_section_title
;
 Synthesis, characterisation and reactivity of germanium(ii) amidinate
 and guanidinate complexes
;
_journal_issue                   21
_journal_name_full               'Dalton Transactions'
_journal_page_first              2871
_journal_page_last               2878
_journal_paper_doi               10.1039/b801168k
_journal_year                    2008
_chemical_formula_sum            'C29 H45 Cl3 Ge N2'
_chemical_formula_weight         600.61
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.93(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.665(2)
_cell_length_b                   18.049(4)
_cell_length_c                   17.156(3)
_cell_measurement_temperature    150(2)
_cell_volume                     3218.7(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0900
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18619
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.220
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0405P)²+3.5099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                4608
_reflns_number_total             6527
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801168k.txt
_cod_data_source_block           compound5
_cod_original_cell_volume        3218.7(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7003909
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Ge1 Ge 0.56226(4) 0.16313(2) 0.18917(2) 0.02866(13) Uani 1 1 d . . .
Cl1 Cl 0.50029(9) 0.10479(6) 0.06529(5) 0.0332(2) Uani 1 1 d . . .
Cl2 Cl 0.77859(9) 0.17048(6) 0.18897(6) 0.0401(3) Uani 1 1 d . . .
Cl3 Cl 0.57183(11) 0.05502(6) 0.25880(5) 0.0414(3) Uani 1 1 d . . .
N1 N 0.0205(3) 0.27276(15) 0.27976(16) 0.0191(6) Uani 1 1 d . . .
H1 H -0.0599 0.2578 0.2720 0.023 Uiso 1 1 calc R . .
N2 N -0.0121(2) 0.31018(15) 0.39947(16) 0.0190(6) Uani 1 1 d . . .
H2 H 0.0179 0.3336 0.4448 0.023 Uiso 1 1 calc R . .
C1 C 0.0634(3) 0.30815(18) 0.34818(19) 0.0170(7) Uani 1 1 d . . .
C2 C 0.1923(3) 0.34945(18) 0.3750(2) 0.0208(7) Uani 1 1 d . . .
C3 C 0.1595(3) 0.43181(19) 0.3847(2) 0.0274(8) Uani 1 1 d . . .
H3A H 0.2392 0.4602 0.4016 0.041 Uiso 1 1 calc R . .
H3B H 0.1080 0.4364 0.4252 0.041 Uiso 1 1 calc R . .
H3C H 0.1104 0.4511 0.3335 0.041 Uiso 1 1 calc R . .
C4 C 0.2829(3) 0.3452(2) 0.3172(2) 0.0309(9) Uani 1 1 d . . .
H4A H 0.3617 0.3730 0.3394 0.046 Uiso 1 1 calc R . .
H4B H 0.2403 0.3667 0.2656 0.046 Uiso 1 1 calc R . .
H4C H 0.3044 0.2933 0.3096 0.046 Uiso 1 1 calc R . .
C5 C 0.2621(3) 0.3185(2) 0.4566(2) 0.0328(9) Uani 1 1 d . . .
H5A H 0.2744 0.2650 0.4522 0.049 Uiso 1 1 calc R . .
H5B H 0.2105 0.3281 0.4961 0.049 Uiso 1 1 calc R . .
H5C H 0.3460 0.3428 0.4736 0.049 Uiso 1 1 calc R . .
C6 C 0.0835(3) 0.25420(19) 0.21493(19) 0.0211(8) Uani 1 1 d . . .
C7 C 0.0758(3) 0.3039(2) 0.1519(2) 0.0256(8) Uani 1 1 d . . .
C8 C 0.1357(4) 0.2831(2) 0.0906(2) 0.0350(9) Uani 1 1 d . . .
H8 H 0.1326 0.3159 0.0469 0.042 Uiso 1 1 calc R . .
C9 C 0.1992(4) 0.2163(2) 0.0919(2) 0.0396(10) Uani 1 1 d . . .
H9 H 0.2425 0.2044 0.0508 0.048 Uiso 1 1 calc R . .
C10 C 0.1995(4) 0.1671(2) 0.1532(2) 0.0338(9) Uani 1 1 d . . .
H10 H 0.2411 0.1205 0.1529 0.041 Uiso 1 1 calc R . .
C11 C 0.1398(3) 0.1840(2) 0.2157(2) 0.0248(8) Uani 1 1 d . . .
C12 C 0.0022(4) 0.37667(19) 0.1451(2) 0.0269(8) Uani 1 1 d . . .
H12 H -0.0081 0.3906 0.1997 0.032 Uiso 1 1 calc R . .
C13 C -0.1318(4) 0.3663(3) 0.0917(3) 0.0500(12) Uani 1 1 d . . .
H13A H -0.1244 0.3556 0.0369 0.075 Uiso 1 1 calc R . .
H13B H -0.1821 0.4117 0.0922 0.075 Uiso 1 1 calc R . .
H13C H -0.1750 0.3249 0.1118 0.075 Uiso 1 1 calc R . .
C14 C 0.0718(5) 0.4401(2) 0.1134(3) 0.0457(11) Uani 1 1 d . . .
H14A H 0.1597 0.4443 0.1459 0.069 Uiso 1 1 calc R . .
H14B H 0.0256 0.4866 0.1162 0.069 Uiso 1 1 calc R . .
H14C H 0.0749 0.4301 0.0577 0.069 Uiso 1 1 calc R . .
C15 C 0.1375(4) 0.1272(2) 0.2806(2) 0.0286(9) Uani 1 1 d . . .
H15 H 0.0697 0.1427 0.3092 0.034 Uiso 1 1 calc R . .
C16 C 0.2646(4) 0.1238(2) 0.3419(3) 0.0433(11) Uani 1 1 d . . .
H16A H 0.3332 0.1088 0.3156 0.065 Uiso 1 1 calc R . .
H16B H 0.2582 0.0877 0.3835 0.065 Uiso 1 1 calc R . .
H16C H 0.2845 0.1728 0.3663 0.065 Uiso 1 1 calc R . .
C17 C 0.1018(4) 0.0500(2) 0.2458(3) 0.0455(11) Uani 1 1 d . . .
H17A H 0.0215 0.0529 0.2048 0.068 Uiso 1 1 calc R . .
H17B H 0.0902 0.0164 0.2885 0.068 Uiso 1 1 calc R . .
H17C H 0.1707 0.0313 0.2217 0.068 Uiso 1 1 calc R . .
C18 C -0.1390(3) 0.27789(19) 0.38914(19) 0.0195(7) Uani 1 1 d . . .
C19 C -0.1494(3) 0.2041(2) 0.41481(19) 0.0223(8) Uani 1 1 d . . .
C20 C -0.2726(4) 0.1767(2) 0.4076(2) 0.0290(9) Uani 1 1 d . . .
H20 H -0.2834 0.1269 0.4228 0.035 Uiso 1 1 calc R . .
C21 C -0.3795(4) 0.2191(2) 0.3793(2) 0.0326(9) Uani 1 1 d . . .
H21 H -0.4626 0.1991 0.3768 0.039 Uiso 1 1 calc R . .
C22 C -0.3672(3) 0.2908(2) 0.3544(2) 0.0305(9) Uani 1 1 d . . .
H22 H -0.4421 0.3194 0.3341 0.037 Uiso 1 1 calc R . .
C23 C -0.2459(3) 0.3218(2) 0.3585(2) 0.0233(8) Uani 1 1 d . . .
C24 C -0.0329(4) 0.1576(2) 0.4511(2) 0.0295(9) Uani 1 1 d . . .
H24 H 0.0428 0.1784 0.4330 0.035 Uiso 1 1 calc R . .
C25 C -0.0052(5) 0.1626(3) 0.5421(3) 0.0555(13) Uani 1 1 d . . .
H25A H 0.0100 0.2144 0.5586 0.083 Uiso 1 1 calc R . .
H25B H 0.0713 0.1331 0.5651 0.083 Uiso 1 1 calc R . .
H25C H -0.0791 0.1435 0.5611 0.083 Uiso 1 1 calc R . .
C26 C -0.0499(4) 0.0769(2) 0.4234(3) 0.0438(11) Uani 1 1 d . . .
H26A H -0.1129 0.0526 0.4486 0.066 Uiso 1 1 calc R . .
H26B H 0.0328 0.0510 0.4386 0.066 Uiso 1 1 calc R . .
H26C H -0.0805 0.0753 0.3651 0.066 Uiso 1 1 calc R . .
C27 C -0.2369(4) 0.4015(2) 0.3317(2) 0.0342(9) Uani 1 1 d . . .
H27 H -0.1453 0.4114 0.3299 0.041 Uiso 1 1 calc R . .
C28 C -0.2741(4) 0.4557(2) 0.3911(3) 0.0490(12) Uani 1 1 d . . .
H28A H -0.3647 0.4484 0.3924 0.073 Uiso 1 1 calc R . .
H28B H -0.2615 0.5066 0.3744 0.073 Uiso 1 1 calc R . .
H28C H -0.2200 0.4470 0.4445 0.073 Uiso 1 1 calc R . .
C29 C -0.3194(5) 0.4139(3) 0.2480(3) 0.0540(13) Uani 1 1 d . . .
H29A H -0.2971 0.3772 0.2113 0.081 Uiso 1 1 calc R . .
H29B H -0.3038 0.4638 0.2297 0.081 Uiso 1 1 calc R . .
H29C H -0.4105 0.4088 0.2491 0.081 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
Cl3 Ge1 Cl2 97.02(5) . . ?
Cl3 Ge1 Cl1 93.52(4) . . ?
Cl2 Ge1 Cl1 95.97(5) . . ?
C1 N1 C6 131.2(3) . . ?
C1 N2 C18 126.9(3) . . ?
N2 C1 N1 117.6(3) . . ?
N2 C1 C2 115.1(3) . . ?
N1 C1 C2 127.3(3) . . ?
C4 C2 C5 108.9(3) . . ?
C4 C2 C1 115.6(3) . . ?
C5 C2 C1 108.4(3) . . ?
C4 C2 C3 107.9(3) . . ?
C5 C2 C3 109.1(3) . . ?
C1 C2 C3 106.8(3) . . ?
C7 C6 C11 122.7(3) . . ?
C7 C6 N1 119.1(3) . . ?
C11 C6 N1 117.9(3) . . ?
C6 C7 C8 117.0(3) . . ?
C6 C7 C12 123.7(3) . . ?
C8 C7 C12 119.3(3) . . ?
C9 C8 C7 121.8(4) . . ?
C10 C9 C8 119.6(3) . . ?
C9 C10 C11 121.4(4) . . ?
C10 C11 C6 117.2(3) . . ?
C10 C11 C15 120.0(3) . . ?
C6 C11 C15 122.8(3) . . ?
C7 C12 C13 109.8(3) . . ?
C7 C12 C14 112.9(3) . . ?
C13 C12 C14 110.0(3) . . ?
C11 C15 C16 112.1(3) . . ?
C11 C15 C17 111.8(3) . . ?
C16 C15 C17 109.9(3) . . ?
C23 C18 C19 122.6(3) . . ?
C23 C18 N2 118.8(3) . . ?
C19 C18 N2 118.5(3) . . ?
C20 C19 C18 116.6(3) . . ?
C20 C19 C24 120.9(3) . . ?
C18 C19 C24 122.5(3) . . ?
C21 C20 C19 122.1(4) . . ?
C20 C21 C22 120.4(3) . . ?
C21 C22 C23 120.8(3) . . ?
C18 C23 C22 117.5(3) . . ?
C18 C23 C27 123.4(3) . . ?
C22 C23 C27 119.0(3) . . ?
C19 C24 C25 109.9(3) . . ?
C19 C24 C26 111.8(3) . . ?
C25 C24 C26 110.9(4) . . ?
C23 C27 C29 111.3(3) . . ?
C23 C27 C28 111.1(3) . . ?
C29 C27 C28 110.6(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
Ge1 Cl3 2.2782(11) . ?
Ge1 Cl2 2.3118(11) . ?
Ge1 Cl1 2.3311(11) . ?
N1 C1 1.325(4) . ?
N1 C6 1.461(4) . ?
N2 C1 1.319(4) . ?
N2 C18 1.448(4) . ?
C1 C2 1.541(5) . ?
C2 C4 1.534(5) . ?
C2 C5 1.536(5) . ?
C2 C3 1.544(5) . ?
C6 C7 1.394(5) . ?
C6 C11 1.401(5) . ?
C7 C8 1.397(5) . ?
C7 C12 1.521(5) . ?
C8 C9 1.381(6) . ?
C9 C10 1.375(6) . ?
C10 C11 1.399(5) . ?
C11 C15 1.517(5) . ?
C12 C13 1.526(6) . ?
C12 C14 1.530(5) . ?
C15 C16 1.520(6) . ?
C15 C17 1.530(5) . ?
C18 C23 1.391(5) . ?
C18 C19 1.415(5) . ?
C19 C20 1.384(5) . ?
C19 C24 1.513(5) . ?
C20 C21 1.369(5) . ?
C21 C22 1.378(6) . ?
C22 C23 1.396(5) . ?
C23 C27 1.520(5) . ?
C24 C25 1.526(6) . ?
C24 C26 1.530(5) . ?
C27 C29 1.524(6) . ?
C27 C28 1.528(6) . ?
