#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:01:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179947 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/42/7024277.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_7024277
loop_
_publ_author_name
'Jana, Anukul'
'Roesky, Herbert W.'
'Schulzke, Carola'
_publ_section_title
;
 Reactivity of germanium(II) hydride with nitrous oxide, trimethylsilyl
 azide, ketones, and alkynes and the reaction of a methyl analogue with
 trimethylsilyl diazomethane.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              132
_journal_page_last               138
_journal_paper_doi               10.1039/b914164b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C35 H60 Ge N4 Si2'
_chemical_formula_weight         665.64
_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                 112.28(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.389(2)
_cell_length_b                   32.555(7)
_cell_length_c                   12.216(2)
_cell_measurement_reflns_used    30632
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      51.7
_cell_measurement_theta_min      3.6
_cell_volume                     3823.2(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  IPDSII
_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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30291
_diffrn_reflns_theta_full        25.84
_diffrn_reflns_theta_max         25.84
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.6626
_exptl_absorpt_correction_T_min  0.6012
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         7365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0304
_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)+(0.0383P)²+1.0380P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                6441
_reflns_number_total             7365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b914164b.txt
_cod_data_source_block           ja32a
_cod_original_cell_volume        3823.0(13)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7024277
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 0.018857(16) 0.132416(5) 0.291636(14) 0.01981(6) Uani 1 1 d .
Si1 Si 0.22051(5) 0.214067(15) 0.33791(4) 0.02492(11) Uani 1 1 d .
Si2 Si -0.31838(5) 0.144952(18) 0.15117(4) 0.03161(13) Uani 1 1 d .
N1 N 0.02978(14) 0.11211(4) 0.43560(12) 0.0231(3) Uani 1 1 d .
N2 N 0.03003(14) 0.08501(4) 0.21351(12) 0.0244(3) Uani 1 1 d .
N3 N 0.16619(15) 0.16379(5) 0.30300(13) 0.0244(3) Uani 1 1 d .
N4 N -0.14419(15) 0.15948(5) 0.21478(13) 0.0268(3) Uani 1 1 d .
C1 C 0.08566(17) 0.13565(5) 0.54408(14) 0.0230(3) Uani 1 1 d .
C2 C 0.22428(18) 0.12861(6) 0.62231(15) 0.0263(4) Uani 1 1 d .
C3 C 0.27687(18) 0.15125(6) 0.72671(15) 0.0312(4) Uani 1 1 d .
H3 H 0.3696 0.1465 0.7803 0.038(2) Uiso 1 1 calc R
C4 C 0.19750(19) 0.18048(6) 0.75418(16) 0.0339(4) Uani 1 1 d .
H4 H 0.2357 0.1959 0.8253 0.038(2) Uiso 1 1 calc R
C5 C 0.06212(19) 0.18706(6) 0.67726(16) 0.0316(4) Uani 1 1 d .
H5 H 0.0079 0.2073 0.6960 0.038(2) Uiso 1 1 calc R
C6 C 0.00326(17) 0.16470(6) 0.57295(15) 0.0260(4) Uani 1 1 d .
C7 C 0.31803(18) 0.09714(6) 0.59830(16) 0.0304(4) Uani 1 1 d .
H7 H 0.2750 0.0893 0.5129 0.033(3) Uiso 1 1 calc R
C8 C 0.4622(2) 0.11410(8) 0.6218(2) 0.0492(6) Uani 1 1 d .
H8A H 0.4544 0.1387 0.5736 0.0679(12) Uiso 1 1 calc R
H8B H 0.5176 0.0933 0.6013 0.0679(12) Uiso 1 1 calc R
H8C H 0.5076 0.1212 0.7057 0.0679(12) Uiso 1 1 calc R
C9 C 0.3285(3) 0.05861(8) 0.6719(3) 0.0630(7) Uani 1 1 d .
H9A H 0.3721 0.0655 0.7561 0.0679(12) Uiso 1 1 calc R
H9B H 0.3851 0.0380 0.6522 0.0679(12) Uiso 1 1 calc R
H9C H 0.2352 0.0475 0.6548 0.0679(12) Uiso 1 1 calc R
C10 C -0.14828(17) 0.17248(6) 0.49562(16) 0.0295(4) Uani 1 1 d .
H10 H -0.1730 0.1543 0.4247 0.033(3) Uiso 1 1 calc R
C11 C -0.2435(2) 0.16126(8) 0.56093(18) 0.0437(5) Uani 1 1 d .
H11A H -0.2330 0.1320 0.5815 0.0679(12) Uiso 1 1 calc R
H11B H -0.3404 0.1669 0.5098 0.0679(12) Uiso 1 1 calc R
H11C H -0.2181 0.1777 0.6333 0.0679(12) Uiso 1 1 calc R
C12 C -0.1734(2) 0.21674(7) 0.45226(18) 0.0391(5) Uani 1 1 d .
H12A H -0.1541 0.2352 0.5200 0.0679(12) Uiso 1 1 calc R
H12B H -0.2705 0.2200 0.3980 0.0679(12) Uiso 1 1 calc R
H12C H -0.1118 0.2235 0.4108 0.0679(12) Uiso 1 1 calc R
C13 C -0.03505(17) 0.07407(6) 0.43704(16) 0.0279(4) Uani 1 1 d .
C14 C -0.0585(2) 0.06046(7) 0.53254(18) 0.0406(5) Uani 1 1 d .
H14A H -0.0311 0.0767 0.6023 0.049 Uiso 1 1 calc R
H14B H -0.1025 0.0347 0.5298 0.049 Uiso 1 1 calc R
C15 C -0.07586(18) 0.04862(6) 0.33130(16) 0.0302(4) Uani 1 1 d .
H15 H -0.1354 0.0263 0.3302 0.038(2) Uiso 1 1 calc R
C16 C -0.04294(18) 0.05142(6) 0.23377(16) 0.0286(4) Uani 1 1 d .
C17 C -0.0899(2) 0.01925(6) 0.13965(19) 0.0412(5) Uani 1 1 d .
H17A H -0.1388 -0.0026 0.1636 0.0679(12) Uiso 1 1 calc R
H17B H -0.0089 0.0076 0.1281 0.0679(12) Uiso 1 1 calc R
H17C H -0.1528 0.0316 0.0655 0.0679(12) Uiso 1 1 calc R
C18 C 0.11782(18) 0.07931(5) 0.14699(15) 0.0263(4) Uani 1 1 d .
C19 C 0.08719(19) 0.09941(6) 0.03815(15) 0.0310(4) Uani 1 1 d .
C20 C 0.1730(2) 0.09228(7) -0.02451(17) 0.0361(4) Uani 1 1 d .
H20 H 0.1551 0.1064 -0.0969 0.038(2) Uiso 1 1 calc R
C21 C 0.2826(2) 0.06531(7) 0.01630(17) 0.0377(5) Uani 1 1 d .
H21 H 0.3381 0.0603 -0.0288 0.038(2) Uiso 1 1 calc R
C22 C 0.3119(2) 0.04552(6) 0.12308(17) 0.0353(4) Uani 1 1 d .
H22 H 0.3871 0.0266 0.1503 0.038(2) Uiso 1 1 calc R
C23 C 0.23320(19) 0.05276(6) 0.19162(16) 0.0293(4) Uani 1 1 d .
C24 C -0.0365(2) 0.12780(7) -0.01620(17) 0.0409(5) Uani 1 1 d .
H24 H -0.0908 0.1275 0.0361 0.033(3) Uiso 1 1 calc R
C25 C 0.0093(3) 0.17202(8) -0.0228(2) 0.0596(7) Uani 1 1 d .
H25A H 0.0689 0.1814 0.0566 0.0679(12) Uiso 1 1 calc R
H25B H -0.0729 0.1898 -0.0541 0.0679(12) Uiso 1 1 calc R
H25C H 0.0612 0.1733 -0.0750 0.0679(12) Uiso 1 1 calc R
C26 C -0.1320(3) 0.11257(10) -0.13798(19) 0.0635(8) Uani 1 1 d .
H26A H -0.0816 0.1127 -0.1914 0.0679(12) Uiso 1 1 calc R
H26B H -0.2132 0.1307 -0.1696 0.0679(12) Uiso 1 1 calc R
H26C H -0.1628 0.0846 -0.1313 0.0679(12) Uiso 1 1 calc R
C27 C 0.2789(2) 0.03288(6) 0.31286(18) 0.0353(4) Uani 1 1 d .
H27 H 0.2164 0.0431 0.3523 0.033(3) Uiso 1 1 calc R
C28 C 0.4274(2) 0.04599(7) 0.38820(18) 0.0418(5) Uani 1 1 d .
H28A H 0.4915 0.0348 0.3541 0.0679(12) Uiso 1 1 calc R
H28B H 0.4527 0.0356 0.4690 0.0679(12) Uiso 1 1 calc R
H28C H 0.4335 0.0760 0.3899 0.0679(12) Uiso 1 1 calc R
C29 C 0.2687(2) -0.01398(7) 0.3067(2) 0.0495(6) Uani 1 1 d .
H29A H 0.1716 -0.0221 0.2637 0.0679(12) Uiso 1 1 calc R
H29B H 0.3016 -0.0253 0.3870 0.0679(12) Uiso 1 1 calc R
H29C H 0.3262 -0.0246 0.2654 0.0679(12) Uiso 1 1 calc R
C30 C 0.0829(2) 0.25108(6) 0.2531(2) 0.0459(5) Uani 1 1 d .
H30A H 0.0587 0.2468 0.1682 0.0679(12) Uiso 1 1 calc R
H30B H 0.1170 0.2792 0.2743 0.0679(12) Uiso 1 1 calc R
H30C H 0.0003 0.2468 0.2720 0.0679(12) Uiso 1 1 calc R
C31 C 0.3740(2) 0.22011(7) 0.2964(2) 0.0488(6) Uani 1 1 d .
H31A H 0.4436 0.1992 0.3369 0.0679(12) Uiso 1 1 calc R
H31B H 0.4143 0.2475 0.3197 0.0679(12) Uiso 1 1 calc R
H31C H 0.3451 0.2169 0.2106 0.0679(12) Uiso 1 1 calc R
C32 C 0.2713(2) 0.22523(7) 0.49732(18) 0.0426(5) Uani 1 1 d .
H32A H 0.1914 0.2207 0.5200 0.0679(12) Uiso 1 1 calc R
H32B H 0.3016 0.2539 0.5129 0.0679(12) Uiso 1 1 calc R
H32C H 0.3477 0.2070 0.5436 0.0679(12) Uiso 1 1 calc R
C33 C -0.3827(2) 0.11983(8) 0.25651(19) 0.0462(5) Uani 1 1 d .
H33A H -0.3191 0.0976 0.2978 0.0679(12) Uiso 1 1 calc R
H33B H -0.4756 0.1085 0.2133 0.0679(12) Uiso 1 1 calc R
H33C H -0.3875 0.1401 0.3142 0.0679(12) Uiso 1 1 calc R
C34 C -0.4205(2) 0.19267(8) 0.0935(2) 0.0583(7) Uani 1 1 d .
H34A H -0.3974 0.2131 0.1569 0.0679(12) Uiso 1 1 calc R
H34B H -0.5201 0.1864 0.0648 0.0679(12) Uiso 1 1 calc R
H34C H -0.3977 0.2036 0.0283 0.0679(12) Uiso 1 1 calc R
C35 C -0.3576(2) 0.10950(10) 0.0237(2) 0.0625(8) Uani 1 1 d .
H35A H -0.3300 0.1223 -0.0367 0.0679(12) Uiso 1 1 calc R
H35B H -0.4576 0.1036 -0.0100 0.0679(12) Uiso 1 1 calc R
H35C H -0.3059 0.0838 0.0503 0.0679(12) Uiso 1 1 calc R
H3N H 0.226(2) 0.1491(8) 0.296(2) 0.044(7) Uiso 1 1 d .
H4N H -0.129(2) 0.1805(8) 0.196(2) 0.041(7) Uiso 1 1 d .
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'
Si Si 0.0817 0.0704 '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
N3 Ge1 N4 111.24(8)
N3 Ge1 N2 107.25(7)
N4 Ge1 N2 111.54(7)
N3 Ge1 N1 112.77(7)
N4 Ge1 N1 111.98(7)
N2 Ge1 N1 101.59(6)
N3 Si1 C32 112.40(9)
N3 Si1 C30 111.48(9)
C32 Si1 C30 108.16(11)
N3 Si1 C31 105.44(9)
C32 Si1 C31 109.56(11)
C30 Si1 C31 109.76(12)
N4 Si2 C33 113.44(9)
N4 Si2 C35 113.79(9)
C33 Si2 C35 106.66(12)
N4 Si2 C34 106.77(10)
C33 Si2 C34 109.15(12)
C35 Si2 C34 106.78(13)
C13 N1 C1 118.69(14)
C13 N1 Ge1 118.00(11)
C1 N1 Ge1 122.82(11)
C16 N2 C18 119.80(15)
C16 N2 Ge1 114.63(12)
C18 N2 Ge1 125.19(11)
Si1 N3 Ge1 138.01(10)
Si2 N4 Ge1 134.74(11)
C6 C1 C2 120.02(16)
C6 C1 N1 120.94(14)
C2 C1 N1 119.03(16)
C3 C2 C1 118.61(17)
C3 C2 C7 118.48(16)
C1 C2 C7 122.91(16)
C4 C3 C2 121.60(16)
C5 C4 C3 119.32(17)
C4 C5 C6 121.52(18)
C5 C6 C1 118.89(16)
C5 C6 C10 118.31(17)
C1 C6 C10 122.79(16)
C2 C7 C8 112.18(17)
C2 C7 C9 110.47(17)
C8 C7 C9 110.07(18)
C6 C10 C12 111.98(15)
C6 C10 C11 110.99(15)
C12 C10 C11 110.32(17)
C14 C13 N1 122.70(17)
C14 C13 C15 119.41(17)
N1 C13 C15 117.88(16)
C16 C15 C13 130.76(17)
C15 C16 N2 122.53(16)
C15 C16 C17 120.63(17)
N2 C16 C17 116.78(16)
C19 C18 C23 120.39(17)
C19 C18 N2 120.48(16)
C23 C18 N2 119.12(16)
C20 C19 C18 118.57(18)
C20 C19 C24 118.18(17)
C18 C19 C24 123.24(17)
C21 C20 C19 121.40(19)
C20 C21 C22 119.76(18)
C21 C22 C23 121.24(19)
C22 C23 C18 118.54(17)
C22 C23 C27 118.44(17)
C18 C23 C27 122.98(17)
C19 C24 C26 111.05(19)
C19 C24 C25 111.62(19)
C26 C24 C25 110.8(2)
C23 C27 C28 109.83(17)
C23 C27 C29 112.76(17)
C28 C27 C29 110.11(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ge1 N3 1.8011(14)
Ge1 N4 1.8224(15)
Ge1 N2 1.8413(15)
Ge1 N1 1.8416(14)
Si1 N3 1.7312(16)
Si1 C32 1.850(2)
Si1 C30 1.857(2)
Si1 C31 1.858(2)
Si2 N4 1.7424(16)
Si2 C33 1.850(2)
Si2 C35 1.856(2)
Si2 C34 1.862(2)
N1 C13 1.413(2)
N1 C1 1.448(2)
N2 C16 1.405(2)
N2 C18 1.445(2)
C1 C6 1.407(2)
C1 C2 1.413(2)
C2 C3 1.393(3)
C2 C7 1.517(3)
C3 C4 1.381(3)
C4 C5 1.380(3)
C5 C6 1.392(3)
C6 C10 1.519(2)
C7 C8 1.518(3)
C7 C9 1.523(3)
C10 C12 1.523(3)
C10 C11 1.532(3)
C13 C14 1.354(3)
C13 C15 1.456(3)
C15 C16 1.361(3)
C16 C17 1.494(3)
C18 C19 1.406(3)
C18 C23 1.409(3)
C19 C20 1.397(3)
C19 C24 1.516(3)
C20 C21 1.374(3)
C21 C22 1.381(3)
C22 C23 1.395(3)
C23 C27 1.518(3)
C24 C26 1.525(3)
C24 C25 1.528(3)
C27 C28 1.528(3)
C27 C29 1.529(3)
