#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:11:39 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179743 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/39/7003911.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_7003911
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            'C31 H48 Cl4 Ga Ge N3'
_chemical_formula_weight         746.83
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 110.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.025(3)
_cell_length_b                   12.550(3)
_cell_length_c                   19.558(4)
_cell_measurement_temperature    150(2)
_cell_volume                     3675.3(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15624
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    1.865
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         8003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0353
_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)+(0.0232P)²+2.4273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                6406
_reflns_number_total             8003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801168k.txt
_cod_data_source_block           compound8
_cod_original_cell_volume        3675.4(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7003911
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.175276(16) 0.409600(19) 0.141569(13) 0.02369(7) Uani 1 1 d . . .
Ga1 Ga 0.250911(18) 0.61046(2) 0.299049(14) 0.02943(8) Uani 1 1 d . . .
Cl1 Cl 0.30045(4) 0.53125(5) 0.21683(3) 0.03507(15) Uani 1 1 d . . .
N1 N 0.25144(12) 0.28580(14) 0.14941(10) 0.0221(4) Uani 1 1 d . . .
C1 C 0.25745(14) 0.30198(17) 0.08261(12) 0.0203(5) Uani 1 1 d . . .
Cl2 Cl 0.14096(5) 0.51466(6) 0.30329(4) 0.04699(18) Uani 1 1 d . . .
N2 N 0.22189(11) 0.40192(13) 0.06192(9) 0.0190(4) Uani 1 1 d . . .
C2 C 0.29165(16) 0.20758(17) 0.20472(12) 0.0269(5) Uani 1 1 d . . .
Cl3 Cl 0.36146(5) 0.61060(6) 0.40107(4) 0.04805(18) Uani 1 1 d . . .
N3 N 0.28992(13) 0.23609(14) 0.04397(10) 0.0247(4) Uani 1 1 d . . .
C3 C 0.23468(19) 0.13187(19) 0.21866(13) 0.0350(6) Uani 1 1 d . . .
Cl4 Cl 0.21050(6) 0.76669(6) 0.25608(4) 0.0595(2) Uani 1 1 d . . .
C4 C 0.2740(2) 0.0550(2) 0.27241(15) 0.0485(8) Uani 1 1 d . . .
H4 H 0.2374 0.0034 0.2835 0.058 Uiso 1 1 calc R . .
C5 C 0.3645(3) 0.0528(2) 0.30932(16) 0.0563(9) Uani 1 1 d . . .
H5 H 0.3901 -0.0021 0.3439 0.068 Uiso 1 1 calc R . .
C6 C 0.4187(2) 0.1295(2) 0.29667(15) 0.0478(8) Uani 1 1 d . . .
H6 H 0.4811 0.1276 0.3235 0.057 Uiso 1 1 calc R . .
C7 C 0.38381(17) 0.21032(19) 0.24506(13) 0.0329(6) Uani 1 1 d . . .
C8 C 0.13432(19) 0.1353(2) 0.17854(15) 0.0392(6) Uani 1 1 d . . .
H8 H 0.1229 0.1759 0.1321 0.047 Uiso 1 1 calc R . .
C9 C 0.0885(2) 0.1955(2) 0.22341(17) 0.0496(8) Uani 1 1 d . . .
H9A H 0.0985 0.1576 0.2695 0.074 Uiso 1 1 calc R . .
H9B H 0.0243 0.1999 0.1956 0.074 Uiso 1 1 calc R . .
H9C H 0.1135 0.2675 0.2340 0.074 Uiso 1 1 calc R . .
C10 C 0.0927(2) 0.0240(2) 0.15780(19) 0.0604(9) Uani 1 1 d . . .
H10A H 0.0993 -0.0162 0.2024 0.091 Uiso 1 1 calc R . .
H10B H 0.1232 -0.0139 0.1296 0.091 Uiso 1 1 calc R . .
H10C H 0.0292 0.0312 0.1282 0.091 Uiso 1 1 calc R . .
C11 C 0.44513(16) 0.2983(2) 0.23783(14) 0.0378(6) Uani 1 1 d . . .
H11 H 0.4099 0.3454 0.1963 0.045 Uiso 1 1 calc R . .
C12 C 0.4769(2) 0.3662(2) 0.30799(17) 0.0579(9) Uani 1 1 d . . .
H12A H 0.4249 0.3916 0.3186 0.087 Uiso 1 1 calc R . .
H12B H 0.5111 0.4273 0.3011 0.087 Uiso 1 1 calc R . .
H12C H 0.5148 0.3228 0.3489 0.087 Uiso 1 1 calc R . .
C13 C 0.5261(2) 0.2576(3) 0.22194(19) 0.0579(9) Uani 1 1 d . . .
H13A H 0.5621 0.2117 0.2622 0.087 Uiso 1 1 calc R . .
H13B H 0.5623 0.3182 0.2172 0.087 Uiso 1 1 calc R . .
H13C H 0.5060 0.2168 0.1762 0.087 Uiso 1 1 calc R . .
C14 C 0.17774(14) 0.44657(17) -0.00952(11) 0.0200(5) Uani 1 1 d . . .
C15 C 0.21215(15) 0.54191(18) -0.02588(13) 0.0257(5) Uani 1 1 d . . .
C16 C 0.16571(17) 0.5918(2) -0.09243(14) 0.0334(6) Uani 1 1 d . . .
H16 H 0.1884 0.6560 -0.1048 0.040 Uiso 1 1 calc R . .
C17 C 0.08781(18) 0.5496(2) -0.14030(13) 0.0357(6) Uani 1 1 d . . .
H17 H 0.0571 0.5847 -0.1853 0.043 Uiso 1 1 calc R . .
C18 C 0.05393(16) 0.4562(2) -0.12325(13) 0.0316(6) Uani 1 1 d . . .
H18 H -0.0001 0.4279 -0.1569 0.038 Uiso 1 1 calc R . .
C19 C 0.09721(14) 0.40290(17) -0.05787(12) 0.0246(5) Uani 1 1 d . . .
C20 C 0.29720(16) 0.59286(19) 0.02616(14) 0.0325(6) Uani 1 1 d . . .
H20 H 0.3212 0.5455 0.0699 0.039 Uiso 1 1 calc R . .
C21 C 0.27825(19) 0.7016(2) 0.05271(16) 0.0465(7) Uani 1 1 d . . .
H21A H 0.2540 0.7497 0.0108 0.070 Uiso 1 1 calc R . .
H21B H 0.3338 0.7314 0.0872 0.070 Uiso 1 1 calc R . .
H21C H 0.2348 0.6934 0.0771 0.070 Uiso 1 1 calc R . .
C22 C 0.36877(19) 0.6021(2) -0.00844(18) 0.0510(8) Uani 1 1 d . . .
H22A H 0.3473 0.6489 -0.0513 0.077 Uiso 1 1 calc R . .
H22B H 0.3814 0.5313 -0.0235 0.077 Uiso 1 1 calc R . .
H22C H 0.4234 0.6319 0.0273 0.077 Uiso 1 1 calc R . .
C23 C 0.05374(15) 0.30485(18) -0.03954(14) 0.0300(5) Uani 1 1 d . . .
H23 H 0.0990 0.2690 0.0034 0.036 Uiso 1 1 calc R . .
C24 C -0.02568(17) 0.3370(2) -0.01744(17) 0.0449(7) Uani 1 1 d . . .
H24A H -0.0056 0.3879 0.0232 0.067 Uiso 1 1 calc R . .
H24B H -0.0501 0.2736 -0.0022 0.067 Uiso 1 1 calc R . .
H24C H -0.0720 0.3702 -0.0593 0.067 Uiso 1 1 calc R . .
C25 C 0.02272(19) 0.2244(2) -0.10203(17) 0.0485(8) Uani 1 1 d . . .
H25A H -0.0251 0.2559 -0.1436 0.073 Uiso 1 1 calc R . .
H25B H 0.0003 0.1604 -0.0856 0.073 Uiso 1 1 calc R . .
H25C H 0.0730 0.2053 -0.1170 0.073 Uiso 1 1 calc R . .
C26 C 0.29459(18) 0.11870(18) 0.06020(14) 0.0338(6) Uani 1 1 d . . .
H26 H 0.2946 0.1121 0.1112 0.041 Uiso 1 1 calc R . .
C27 C 0.2117(2) 0.0604(2) 0.01163(16) 0.0457(7) Uani 1 1 d . . .
H27A H 0.1584 0.0974 0.0128 0.068 Uiso 1 1 calc R . .
H27B H 0.2123 -0.0127 0.0294 0.068 Uiso 1 1 calc R . .
H27C H 0.2109 0.0589 -0.0387 0.068 Uiso 1 1 calc R . .
C28 C 0.3795(2) 0.0645(2) 0.06077(18) 0.0547(8) Uani 1 1 d . . .
H28A H 0.3820 0.0664 0.0115 0.082 Uiso 1 1 calc R . .
H28B H 0.3798 -0.0098 0.0764 0.082 Uiso 1 1 calc R . .
H28C H 0.4314 0.1017 0.0948 0.082 Uiso 1 1 calc R . .
C29 C 0.31876(15) 0.28212(19) -0.01462(12) 0.0275(5) Uani 1 1 d . . .
H29 H 0.2923 0.3552 -0.0243 0.033 Uiso 1 1 calc R . .
C30 C 0.28260(19) 0.2234(2) -0.08729(14) 0.0429(7) Uani 1 1 d . . .
H30A H 0.3100 0.1526 -0.0820 0.064 Uiso 1 1 calc R . .
H30B H 0.2968 0.2638 -0.1246 0.064 Uiso 1 1 calc R . .
H30C H 0.2177 0.2160 -0.1021 0.064 Uiso 1 1 calc R . .
C31 C 0.41910(17) 0.2978(2) 0.01132(17) 0.0477(7) Uani 1 1 d . . .
H31A H 0.4486 0.2282 0.0169 0.072 Uiso 1 1 calc R . .
H31B H 0.4394 0.3348 0.0585 0.072 Uiso 1 1 calc R . .
H31C H 0.4342 0.3404 -0.0246 0.072 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'
Ga Ga 0.2307 1.6083 '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'
Cl Cl 0.1484 0.1585 '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
N1 Ge1 N2 67.47(7) . . ?
N1 Ge1 Cl1 95.20(6) . . ?
N2 Ge1 Cl1 92.55(5) . . ?
Cl4 Ga1 Cl3 113.49(3) . . ?
Cl4 Ga1 Cl2 112.85(4) . . ?
Cl3 Ga1 Cl2 112.31(3) . . ?
Cl4 Ga1 Cl1 104.91(3) . . ?
Cl3 Ga1 Cl1 106.20(3) . . ?
Cl2 Ga1 Cl1 106.29(3) . . ?
Ga1 Cl1 Ge1 105.80(3) . . ?
C1 N1 C2 131.41(19) . . ?
C1 N1 Ge1 93.56(13) . . ?
C2 N1 Ge1 134.97(15) . . ?
N3 C1 N1 128.52(19) . . ?
N3 C1 N2 126.7(2) . . ?
N1 C1 N2 104.76(18) . . ?
C1 N2 C14 130.53(18) . . ?
C1 N2 Ge1 92.66(13) . . ?
C14 N2 Ge1 124.08(13) . . ?
C7 C2 C3 122.1(2) . . ?
C7 C2 N1 120.5(2) . . ?
C3 C2 N1 117.4(2) . . ?
C1 N3 C29 118.70(18) . . ?
C1 N3 C26 118.98(19) . . ?
C29 N3 C26 122.31(18) . . ?
C4 C3 C2 117.4(3) . . ?
C4 C3 C8 121.2(2) . . ?
C2 C3 C8 121.4(2) . . ?
C5 C4 C3 121.2(3) . . ?
C4 C5 C6 120.6(3) . . ?
C5 C6 C7 121.4(3) . . ?
C6 C7 C2 117.2(3) . . ?
C6 C7 C11 119.3(2) . . ?
C2 C7 C11 123.5(2) . . ?
C3 C8 C9 110.7(2) . . ?
C3 C8 C10 113.0(2) . . ?
C9 C8 C10 110.4(2) . . ?
C7 C11 C13 113.6(2) . . ?
C7 C11 C12 109.8(2) . . ?
C13 C11 C12 109.4(2) . . ?
C15 C14 C19 121.3(2) . . ?
C15 C14 N2 117.24(19) . . ?
C19 C14 N2 121.10(19) . . ?
C16 C15 C14 118.2(2) . . ?
C16 C15 C20 119.2(2) . . ?
C14 C15 C20 122.5(2) . . ?
C17 C16 C15 121.1(2) . . ?
C16 C17 C18 120.2(2) . . ?
C17 C18 C19 121.3(2) . . ?
C18 C19 C14 117.9(2) . . ?
C18 C19 C23 119.1(2) . . ?
C14 C19 C23 122.9(2) . . ?
C15 C20 C21 111.3(2) . . ?
C15 C20 C22 111.7(2) . . ?
C21 C20 C22 110.7(2) . . ?
C19 C23 C25 113.2(2) . . ?
C19 C23 C24 110.4(2) . . ?
C25 C23 C24 109.5(2) . . ?
N3 C26 C28 114.7(2) . . ?
N3 C26 C27 111.9(2) . . ?
C28 C26 C27 111.8(2) . . ?
N3 C29 C31 111.9(2) . . ?
N3 C29 C30 114.2(2) . . ?
C31 C29 C30 112.4(2) . . ?
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 N1 1.9477(18) . ?
Ge1 N2 1.9552(18) . ?
Ge1 Cl1 2.5333(9) . ?
Ga1 Cl4 2.1406(8) . ?
Ga1 Cl3 2.1451(11) . ?
Ga1 Cl2 2.1590(8) . ?
Ga1 Cl1 2.2613(8) . ?
N1 C1 1.359(3) . ?
N1 C2 1.433(3) . ?
C1 N3 1.344(3) . ?
C1 N2 1.377(3) . ?
N2 C14 1.436(3) . ?
C2 C7 1.405(3) . ?
C2 C3 1.410(3) . ?
N3 C29 1.496(3) . ?
N3 C26 1.503(3) . ?
C3 C4 1.401(4) . ?
C3 C8 1.518(4) . ?
C4 C5 1.371(5) . ?
C5 C6 1.377(4) . ?
C6 C7 1.399(4) . ?
C7 C11 1.518(4) . ?
C8 C9 1.529(4) . ?
C8 C10 1.539(4) . ?
C11 C13 1.526(4) . ?
C11 C12 1.539(4) . ?
C14 C15 1.401(3) . ?
C14 C19 1.411(3) . ?
C15 C16 1.396(3) . ?
C15 C20 1.521(3) . ?
C16 C17 1.372(4) . ?
C17 C18 1.382(4) . ?
C18 C19 1.390(3) . ?
C19 C23 1.519(3) . ?
C20 C21 1.529(4) . ?
C20 C22 1.530(4) . ?
C23 C25 1.526(3) . ?
C23 C24 1.537(3) . ?
C26 C28 1.518(4) . ?
C26 C27 1.518(4) . ?
C29 C31 1.517(3) . ?
C29 C30 1.520(3) . ?
