#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:57:47 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180116 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/14/7101450.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_7101450
loop_
_publ_author_name
'Cameron Jones'
'Shaun P. Green'
'Peter Junk'
'Kai-Alexander Lippert'
'Andreas Stasch'
_publ_section_title
;
Synthetic, Structural and Theoretical Studies of
Amidinate and Guanidinate Stabilised Germanium(I) Dimers
;
_journal_issue                   38
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b610645e
_journal_year                    2006
_chemical_formula_sum            'C62 H96 Ge2 N6'
_chemical_formula_weight         1070.63
_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                 103.72(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.818(2)
_cell_length_b                   14.892(3)
_cell_length_c                   17.589(4)
_cell_measurement_temperature    150(2)
_cell_volume                     3007.3(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0960
_diffrn_reflns_av_sigmaI/netI    0.1409
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10393
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.041
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            lime-green
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.090
_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     328
_refine_ls_number_reflns         5573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_gt           0.0761
_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)+(0.0181P)²+6.4333P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                3594
_reflns_number_total             5573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b610645e.txt
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7101450
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
Ge1 Ge 0.55446(4) 0.98878(3) 0.07513(3) 0.02233(16) Uani 1 1 d .
N1 N 0.5911(3) 0.8548(2) 0.0658(2) 0.0193(9) Uani 1 1 d .
N2 N 0.4424(3) 0.9003(2) 0.1075(2) 0.0183(9) Uani 1 1 d .
N3 N 0.4804(3) 0.7393(2) 0.1119(2) 0.0209(9) Uani 1 1 d .
C1 C 0.5020(4) 0.8271(3) 0.0965(2) 0.0177(10) Uani 1 1 d .
C2 C 0.7010(4) 0.8103(3) 0.0754(3) 0.0200(11) Uani 1 1 d .
C3 C 0.7772(4) 0.7991(3) 0.1505(3) 0.0243(11) Uani 1 1 d .
C4 C 0.8865(4) 0.7615(3) 0.1556(3) 0.0332(13) Uani 1 1 d .
H4 H 0.9389 0.7553 0.2054 0.040 Uiso 1 1 calc R
C5 C 0.9200(4) 0.7331(3) 0.0895(3) 0.0319(13) Uani 1 1 d .
H5 H 0.9950 0.7075 0.0941 0.038 Uiso 1 1 calc R
C6 C 0.8452(4) 0.7418(3) 0.0172(3) 0.0261(12) Uani 1 1 d .
H6 H 0.8685 0.7207 -0.0277 0.031 Uiso 1 1 calc R
C7 C 0.7362(4) 0.7808(3) 0.0085(3) 0.0212(11) Uani 1 1 d .
C8 C 0.7461(4) 0.8287(3) 0.2255(3) 0.0297(12) Uani 1 1 d .
H8 H 0.6593 0.8329 0.2149 0.036 Uiso 1 1 calc R
C9 C 0.7869(5) 0.7606(4) 0.2928(3) 0.0460(15) Uani 1 1 d .
H9A H 0.7667 0.6996 0.2732 0.069 Uiso 1 1 calc R
H9B H 0.7485 0.7738 0.3351 0.069 Uiso 1 1 calc R
H9C H 0.8715 0.7652 0.3126 0.069 Uiso 1 1 calc R
C10 C 0.7962(5) 0.9216(4) 0.2529(3) 0.0443(15) Uani 1 1 d .
H10A H 0.8814 0.9195 0.2637 0.067 Uiso 1 1 calc R
H10B H 0.7724 0.9387 0.3006 0.067 Uiso 1 1 calc R
H10C H 0.7668 0.9660 0.2118 0.067 Uiso 1 1 calc R
C11 C 0.6616(5) 0.7904(3) -0.0743(3) 0.0361(14) Uani 1 1 d .
H11 H 0.5866 0.8197 -0.0716 0.043 Uiso 1 1 calc R
C12 C 0.7227(6) 0.8503(4) -0.1235(3) 0.0530(18) Uani 1 1 d .
H12A H 0.7409 0.9085 -0.0977 0.079 Uiso 1 1 calc R
H12B H 0.6712 0.8591 -0.1755 0.079 Uiso 1 1 calc R
H12C H 0.7949 0.8213 -0.1287 0.079 Uiso 1 1 calc R
C13 C 0.6340(4) 0.6994(4) -0.1147(3) 0.0461(16) Uani 1 1 d .
H13A H 0.7069 0.6687 -0.1161 0.069 Uiso 1 1 calc R
H13B H 0.5877 0.7085 -0.1683 0.069 Uiso 1 1 calc R
H13C H 0.5898 0.6627 -0.0856 0.069 Uiso 1 1 calc R
C14 C 0.3368(4) 0.9086(3) 0.1334(3) 0.0195(11) Uani 1 1 d .
C15 C 0.3458(4) 0.9314(3) 0.2127(3) 0.0239(11) Uani 1 1 d .
C16 C 0.2433(5) 0.9447(3) 0.2371(3) 0.0288(12) Uani 1 1 d .
H16 H 0.2476 0.9604 0.2900 0.035 Uiso 1 1 calc R
C17 C 0.1358(5) 0.9354(3) 0.1861(3) 0.0325(13) Uani 1 1 d .
H17 H 0.0669 0.9443 0.2041 0.039 Uiso 1 1 calc R
C18 C 0.1281(4) 0.9133(3) 0.1096(3) 0.0265(12) Uani 1 1 d .
H18 H 0.0534 0.9064 0.0752 0.032 Uiso 1 1 calc R
C19 C 0.2275(4) 0.9006(3) 0.0807(3) 0.0212(11) Uani 1 1 d .
C20 C 0.4627(4) 0.9406(3) 0.2705(3) 0.0291(12) Uani 1 1 d .
H20 H 0.5224 0.9124 0.2462 0.035 Uiso 1 1 calc R
C21 C 0.4975(5) 1.0389(3) 0.2873(3) 0.0426(15) Uani 1 1 d .
H21A H 0.5047 1.0682 0.2388 0.064 Uiso 1 1 calc R
H21B H 0.5723 1.0419 0.3259 0.064 Uiso 1 1 calc R
H21C H 0.4377 1.0696 0.3078 0.064 Uiso 1 1 calc R
C22 C 0.4675(5) 0.8916(4) 0.3480(3) 0.0478(16) Uani 1 1 d .
H22A H 0.4167 0.9223 0.3764 0.072 Uiso 1 1 calc R
H22B H 0.5477 0.8918 0.3798 0.072 Uiso 1 1 calc R
H22C H 0.4411 0.8296 0.3372 0.072 Uiso 1 1 calc R
C23 C 0.2138(4) 0.8823(3) -0.0059(3) 0.0257(12) Uani 1 1 d .
H23 H 0.2920 0.8666 -0.0147 0.031 Uiso 1 1 calc R
C24 C 0.1704(5) 0.9676(4) -0.0526(3) 0.0407(14) Uani 1 1 d .
H24A H 0.1687 0.9578 -0.1079 0.061 Uiso 1 1 calc R
H24B H 0.2229 1.0176 -0.0325 0.061 Uiso 1 1 calc R
H24C H 0.0917 0.9819 -0.0471 0.061 Uiso 1 1 calc R
C25 C 0.1301(5) 0.8055(4) -0.0367(3) 0.0396(14) Uani 1 1 d .
H25A H 0.1573 0.7507 -0.0072 0.059 Uiso 1 1 calc R
H25B H 0.1272 0.7956 -0.0922 0.059 Uiso 1 1 calc R
H25C H 0.0522 0.8208 -0.0305 0.059 Uiso 1 1 calc R
C26 C 0.5036(4) 0.6718(3) 0.0555(3) 0.0301(12) Uani 1 1 d .
H26 H 0.5328 0.7067 0.0155 0.036 Uiso 1 1 calc R
C27 C 0.6003(5) 0.6043(4) 0.0897(4) 0.0569(18) Uani 1 1 d .
H27A H 0.6639 0.6353 0.1262 0.085 Uiso 1 1 calc R
H27B H 0.6297 0.5776 0.0473 0.085 Uiso 1 1 calc R
H27C H 0.5690 0.5570 0.1176 0.085 Uiso 1 1 calc R
C28 C 0.3945(5) 0.6245(4) 0.0106(4) 0.0606(19) Uani 1 1 d .
H28A H 0.3682 0.5819 0.0453 0.091 Uiso 1 1 calc R
H28B H 0.4116 0.5921 -0.0339 0.091 Uiso 1 1 calc R
H28C H 0.3332 0.6689 -0.0085 0.091 Uiso 1 1 calc R
C29 C 0.4258(4) 0.7170(3) 0.1770(3) 0.0265(12) Uani 1 1 d .
H29 H 0.4299 0.7729 0.2090 0.032 Uiso 1 1 calc R
C30 C 0.4943(5) 0.6454(4) 0.2319(3) 0.0441(15) Uani 1 1 d .
H30A H 0.4814 0.5865 0.2065 0.066 Uiso 1 1 calc R
H30B H 0.4677 0.6441 0.2806 0.066 Uiso 1 1 calc R
H30C H 0.5776 0.6598 0.2437 0.066 Uiso 1 1 calc R
C31 C 0.2979(4) 0.6895(4) 0.1553(3) 0.0387(14) Uani 1 1 d .
H31A H 0.2545 0.7302 0.1150 0.058 Uiso 1 1 calc R
H31B H 0.2659 0.6928 0.2018 0.058 Uiso 1 1 calc R
H31C H 0.2911 0.6279 0.1352 0.058 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'
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_3
N2 Ge1 N1 63.84(14) .
N2 Ge1 Ge1 99.47(10) 3_675
N1 Ge1 Ge1 95.97(10) 3_675
C1 N1 C2 125.5(4) .
C1 N1 Ge1 93.8(2) .
C2 N1 Ge1 130.0(3) .
C1 N2 C14 130.2(4) .
C1 N2 Ge1 95.0(3) .
C14 N2 Ge1 134.8(3) .
C1 N3 C29 120.2(4) .
C1 N3 C26 116.2(4) .
C29 N3 C26 123.3(4) .
N2 C1 N1 107.1(4) .
N2 C1 N3 128.3(4) .
N1 C1 N3 124.5(4) .
C7 C2 C3 119.6(4) .
C7 C2 N1 119.0(4) .
C3 C2 N1 121.4(4) .
C4 C3 C2 118.8(4) .
C4 C3 C8 118.3(4) .
C2 C3 C8 123.0(4) .
C5 C4 C3 121.1(4) .
C6 C5 C4 120.1(4) .
C5 C6 C7 121.3(4) .
C6 C7 C2 119.2(4) .
C6 C7 C11 117.2(4) .
C2 C7 C11 123.6(4) .
C3 C8 C10 112.3(4) .
C3 C8 C9 112.3(4) .
C10 C8 C9 108.9(4) .
C7 C11 C13 111.9(4) .
C7 C11 C12 110.6(4) .
C13 C11 C12 109.2(4) .
C19 C14 C15 120.9(4) .
C19 C14 N2 121.2(4) .
C15 C14 N2 117.8(4) .
C16 C15 C14 118.1(4) .
C16 C15 C20 120.2(4) .
C14 C15 C20 121.8(4) .
C17 C16 C15 121.4(4) .
C18 C17 C16 120.1(5) .
C17 C18 C19 121.6(5) .
C18 C19 C14 118.0(4) .
C18 C19 C23 119.4(4) .
C14 C19 C23 122.6(4) .
C15 C20 C21 112.1(4) .
C15 C20 C22 112.9(4) .
C21 C20 C22 109.4(4) .
C19 C23 C25 113.4(4) .
C19 C23 C24 109.3(4) .
C25 C23 C24 108.9(4) .
N3 C26 C28 113.2(4) .
N3 C26 C27 114.9(4) .
C28 C26 C27 111.3(5) .
N3 C29 C31 117.0(4) .
N3 C29 C30 112.4(4) .
C31 C29 C30 108.3(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 N2 2.043(3) .
Ge1 N1 2.056(3) .
Ge1 Ge1 2.6721(13) 3_675
N1 C1 1.357(5) .
N1 C2 1.433(5) .
N2 C1 1.337(5) .
N2 C14 1.432(5) .
N3 C1 1.371(5) .
N3 C29 1.480(5) .
N3 C26 1.483(6) .
C2 C7 1.408(6) .
C2 C3 1.419(6) .
C3 C4 1.391(6) .
C3 C8 1.518(6) .
C4 C5 1.381(7) .
C5 C6 1.371(6) .
C6 C7 1.388(6) .
C7 C11 1.520(6) .
C8 C10 1.537(7) .
C8 C9 1.546(7) .
C11 C13 1.529(7) .
C11 C12 1.536(7) .
C14 C19 1.405(6) .
C14 C15 1.415(6) .
C15 C16 1.391(6) .
C15 C20 1.515(7) .
C16 C17 1.378(7) .
C17 C18 1.367(7) .
C18 C19 1.399(6) .
C19 C23 1.518(6) .
C20 C21 1.531(7) .
C20 C22 1.534(7) .
C23 C25 1.525(7) .
C23 C24 1.533(6) .
C26 C28 1.516(7) .
C26 C27 1.533(7) .
C29 C31 1.525(6) .
C29 C30 1.535(7) .
