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#$Date: 2016-03-23 16:21:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179373 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/70/4327073.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_4327073
loop_
_publ_author_name
'Cameron Jones'
'Simon J. Bonyhady'
'Nicole Holzmann'
'Gernot Frenking'
'Andreas Stasch'
_publ_section_title
;
 Preparation, Characterization, and Theoretical Analysis of Group 14
 Element(I) Dimers: A Case Study of Magnesium(I) Compounds as Reducing
 Agents in Inorganic Synthesis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12315
_journal_page_last               12325
_journal_paper_doi               10.1021/ic200682p
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C76 H108 Ge2 N4'
_chemical_formula_weight         1222.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.60(3)
_cell_angle_beta                 70.97(3)
_cell_angle_gamma                65.86(3)
_cell_formula_units_Z            1
_cell_length_a                   11.968(2)
_cell_length_b                   12.134(2)
_cell_length_c                   14.323(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1787.7(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13284
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.883
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            red-purple
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         7002
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.411
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0414
_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)+(0.0396P)²+0.7693P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                5543
_reflns_number_total             7002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200682p_si_001_07.cif
_cod_data_source_block           compound14
_cod_original_cell_volume        1787.9(6)
_cod_database_code               4327073
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.52355(3) 0.50805(3) 0.58165(3) 0.02809(13) Uani 1 1 d . . .
N1 N 0.4239(2) 0.4133(2) 0.65996(18) 0.0236(6) Uani 1 1 d . . .
C1 C 0.5298(3) 0.3090(3) 0.6430(2) 0.0234(7) Uani 1 1 d . . .
N2 N 0.6299(2) 0.3275(2) 0.57804(19) 0.0248(6) Uani 1 1 d . . .
C2 C 0.5394(3) 0.1933(3) 0.6866(2) 0.0260(7) Uani 1 1 d . . .
C3 C 0.4522(3) 0.1880(3) 0.7775(2) 0.0327(8) Uani 1 1 d . . .
H3 H 0.3813 0.2605 0.8116 0.039 Uiso 1 1 calc R . .
C4 C 0.4673(3) 0.0787(3) 0.8188(3) 0.0364(8) Uani 1 1 d . . .
H4 H 0.4068 0.0785 0.8812 0.044 Uiso 1 1 calc R . .
C5 C 0.5681(3) -0.0302(3) 0.7722(3) 0.0322(8) Uani 1 1 d . A .
C6 C 0.6524(3) -0.0247(3) 0.6799(3) 0.0360(8) Uani 1 1 d . . .
H6 H 0.7210 -0.0978 0.6445 0.043 Uiso 1 1 calc R . .
C7 C 0.6393(3) 0.0836(3) 0.6383(3) 0.0326(8) Uani 1 1 d . . .
H7 H 0.6994 0.0835 0.5756 0.039 Uiso 1 1 calc R . .
C8 C 0.5873(4) -0.1509(3) 0.8171(3) 0.0503(11) Uani 1 1 d D . .
C9 C 0.5585(13) -0.2276(8) 0.7450(6) 0.059(3) Uani 0.614(19) 1 d PD A 1
H9A H 0.4722 -0.1803 0.7400 0.088 Uiso 0.614(19) 1 calc PR A 1
H9B H 0.5620 -0.3043 0.7727 0.088 Uiso 0.614(19) 1 calc PR A 1
H9C H 0.6240 -0.2443 0.6789 0.088 Uiso 0.614(19) 1 calc PR A 1
C10 C 0.7249(9) -0.2242(11) 0.8100(12) 0.077(4) Uani 0.614(19) 1 d PDU A 1
H10A H 0.7792 -0.2452 0.7401 0.116 Uiso 0.614(19) 1 calc PR A 1
H10B H 0.7319 -0.2986 0.8432 0.116 Uiso 0.614(19) 1 calc PR A 1
H10C H 0.7541 -0.1771 0.8421 0.116 Uiso 0.614(19) 1 calc PR A 1
C11 C 0.4871(18) -0.1370(18) 0.9164(12) 0.084(7) Uani 0.614(19) 1 d PD A 1
H11A H 0.4994 -0.0924 0.9643 0.126 Uiso 0.614(19) 1 calc PR A 1
H11B H 0.4959 -0.2173 0.9384 0.126 Uiso 0.614(19) 1 calc PR A 1
H11C H 0.4004 -0.0922 0.9114 0.126 Uiso 0.614(19) 1 calc PR A 1
C12 C 0.2938(3) 0.4416(3) 0.7226(2) 0.0263(7) Uani 1 1 d . . .
C13 C 0.2526(3) 0.4942(3) 0.8195(2) 0.0307(7) Uani 1 1 d . . .
C14 C 0.1229(3) 0.5286(3) 0.8774(3) 0.0417(9) Uani 1 1 d . . .
H14 H 0.0933 0.5636 0.9432 0.050 Uiso 1 1 calc R . .
C15 C 0.0368(3) 0.5127(4) 0.8407(3) 0.0489(10) Uani 1 1 d . . .
H15 H -0.0514 0.5374 0.8809 0.059 Uiso 1 1 calc R . .
C16 C 0.0789(3) 0.4610(4) 0.7458(3) 0.0470(10) Uani 1 1 d . . .
H16 H 0.0191 0.4494 0.7215 0.056 Uiso 1 1 calc R . .
C17 C 0.2073(3) 0.4251(3) 0.6846(3) 0.0346(8) Uani 1 1 d . . .
C18 C 0.3449(3) 0.5119(3) 0.8632(3) 0.0390(9) Uani 1 1 d . . .
H18 H 0.4339 0.4742 0.8132 0.047 Uiso 1 1 calc R . .
C19 C 0.3145(5) 0.6436(4) 0.8823(4) 0.0702(14) Uani 1 1 d . . .
H19A H 0.2258 0.6847 0.9283 0.105 Uiso 1 1 calc R . .
H19B H 0.3224 0.6819 0.8197 0.105 Uiso 1 1 calc R . .
H19C H 0.3757 0.6499 0.9113 0.105 Uiso 1 1 calc R . .
C20 C 0.3497(6) 0.4481(4) 0.9573(4) 0.0737(15) Uani 1 1 d . . .
H20A H 0.2653 0.4862 1.0095 0.111 Uiso 1 1 calc R . .
H20B H 0.4168 0.4546 0.9787 0.111 Uiso 1 1 calc R . .
H20C H 0.3700 0.3624 0.9444 0.111 Uiso 1 1 calc R . .
C21 C 0.2516(4) 0.3663(4) 0.5804(3) 0.0445(10) Uani 1 1 d . . .
H21 H 0.3382 0.3668 0.5437 0.053 Uiso 1 1 calc R . .
C22 C 0.1601(5) 0.4369(5) 0.5235(3) 0.0707(14) Uani 1 1 d . . .
H22A H 0.0771 0.4301 0.5530 0.106 Uiso 1 1 calc R . .
H22B H 0.1990 0.4035 0.4541 0.106 Uiso 1 1 calc R . .
H22C H 0.1454 0.5224 0.5267 0.106 Uiso 1 1 calc R . .
C23 C 0.2700(5) 0.2341(4) 0.5835(4) 0.0656(13) Uani 1 1 d . . .
H23A H 0.3304 0.1909 0.6193 0.098 Uiso 1 1 calc R . .
H23B H 0.3052 0.1961 0.5157 0.098 Uiso 1 1 calc R . .
H23C H 0.1861 0.2306 0.6175 0.098 Uiso 1 1 calc R . .
C24 C 0.7650(3) 0.2595(3) 0.5638(2) 0.0263(7) Uani 1 1 d . . .
C25 C 0.8111(3) 0.2454(3) 0.6443(2) 0.0296(7) Uani 1 1 d . . .
C26 C 0.9444(3) 0.1815(3) 0.6256(3) 0.0374(8) Uani 1 1 d . . .
H26 H 0.9774 0.1699 0.6791 0.045 Uiso 1 1 calc R . .
C27 C 1.0284(3) 0.1352(3) 0.5319(3) 0.0402(9) Uani 1 1 d . . .
H27 H 1.1185 0.0911 0.5212 0.048 Uiso 1 1 calc R . .
C28 C 0.9825(3) 0.1524(3) 0.4528(3) 0.0363(8) Uani 1 1 d . . .
H28 H 1.0419 0.1212 0.3879 0.044 Uiso 1 1 calc R . .
C29 C 0.8505(3) 0.2147(3) 0.4668(2) 0.0294(7) Uani 1 1 d . . .
C30 C 0.7255(3) 0.3013(3) 0.7484(3) 0.0381(9) Uani 1 1 d . . .
H30 H 0.6336 0.3385 0.7491 0.046 Uiso 1 1 calc R . .
C31 C 0.7568(4) 0.4033(4) 0.7754(3) 0.0622(12) Uani 1 1 d . . .
H31A H 0.8435 0.3686 0.7816 0.093 Uiso 1 1 calc R . .
H31B H 0.6925 0.4469 0.8386 0.093 Uiso 1 1 calc R . .
H31C H 0.7543 0.4595 0.7234 0.093 Uiso 1 1 calc R . .
C32 C 0.7352(4) 0.2074(4) 0.8247(3) 0.0606(12) Uani 1 1 d . . .
H32A H 0.7136 0.1442 0.8059 0.091 Uiso 1 1 calc R . .
H32B H 0.6744 0.2470 0.8901 0.091 Uiso 1 1 calc R . .
H32C H 0.8238 0.1709 0.8271 0.091 Uiso 1 1 calc R . .
C33 C 0.8014(3) 0.2352(3) 0.3790(2) 0.0353(8) Uani 1 1 d . . .
H33 H 0.7359 0.3211 0.3880 0.042 Uiso 1 1 calc R . .
C34 C 0.9080(4) 0.2195(4) 0.2799(3) 0.0537(11) Uani 1 1 d . . .
H34A H 0.9534 0.2697 0.2835 0.081 Uiso 1 1 calc R . .
H34B H 0.8692 0.2447 0.2273 0.081 Uiso 1 1 calc R . .
H34C H 0.9697 0.1342 0.2654 0.081 Uiso 1 1 calc R . .
C35 C 0.7326(4) 0.1543(4) 0.3750(3) 0.0517(10) Uani 1 1 d . . .
H35A H 0.7937 0.0690 0.3673 0.078 Uiso 1 1 calc R . .
H35B H 0.7005 0.1722 0.3186 0.078 Uiso 1 1 calc R . .
H35C H 0.6595 0.1699 0.4366 0.078 Uiso 1 1 calc R . .
C36 C 0.0123(7) 0.0392(6) 0.9639(5) 0.101(2) Uani 1 1 d D . .
H36A H -0.0730 0.0963 0.9600 0.122 Uiso 1 1 calc R . .
H36B H 0.0601 -0.0108 0.8997 0.122 Uiso 1 1 calc R . .
C37 C 0.0817(6) 0.1122(6) 0.9685(6) 0.125(3) Uani 1 1 d D . .
H37A H 0.0341 0.1641 1.0318 0.150 Uiso 1 1 calc R . .
H37B H 0.1678 0.0563 0.9717 0.150 Uiso 1 1 calc R . .
C38 C 0.1024(7) 0.1897(7) 0.8900(6) 0.148(3) Uani 1 1 d D . .
H38A H 0.1514 0.1404 0.8264 0.222 Uiso 1 1 calc R . .
H38B H 0.1515 0.2315 0.9027 0.222 Uiso 1 1 calc R . .
H38C H 0.0185 0.2496 0.8877 0.222 Uiso 1 1 calc R . .
C10A C 0.7027(13) -0.1704(16) 0.8659(14) 0.061(5) Uani 0.386(19) 1 d PDU A 2
H10D H 0.7841 -0.1837 0.8125 0.092 Uiso 0.386(19) 1 calc PR A 2
H10E H 0.7153 -0.2410 0.9049 0.092 Uiso 0.386(19) 1 calc PR A 2
H10F H 0.6763 -0.0980 0.9088 0.092 Uiso 0.386(19) 1 calc PR A 2
C9A C 0.630(3) -0.2535(17) 0.7516(14) 0.098(7) Uani 0.386(19) 1 d PDU A 2
H9A1 H 0.5829 -0.2322 0.7043 0.148 Uiso 0.386(19) 1 calc PR A 2
H9A2 H 0.6148 -0.3188 0.7894 0.148 Uiso 0.386(19) 1 calc PR A 2
H9A3 H 0.7235 -0.2806 0.7156 0.148 Uiso 0.386(19) 1 calc PR A 2
C11A C 0.4832(16) -0.147(2) 0.9160(13) 0.037(5) Uani 0.386(19) 1 d PDU A 2
H11D H 0.4711 -0.0837 0.9627 0.055 Uiso 0.386(19) 1 calc PR A 2
H11E H 0.5111 -0.2255 0.9435 0.055 Uiso 0.386(19) 1 calc PR A 2
H11F H 0.4012 -0.1284 0.9047 0.055 Uiso 0.386(19) 1 calc PR A 2
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_1
_geom_angle_site_symmetry_3
N1 Ge1 N2 64.68(10) . .
N1 Ge1 Ge1 95.60(8) . 2_666
N2 Ge1 Ge1 94.57(8) . 2_666
C1 N1 C12 129.7(3) . .
C1 N1 Ge1 93.88(18) . .
C12 N1 Ge1 135.9(2) . .
N1 C1 N2 107.5(3) . .
N1 C1 C2 127.6(3) . .
N2 C1 C2 124.9(3) . .
C1 N2 C24 126.9(3) . .
C1 N2 Ge1 93.37(18) . .
C24 N2 Ge1 131.28(19) . .
C7 C2 C3 117.0(3) . .
C7 C2 C1 120.7(3) . .
C3 C2 C1 122.3(3) . .
C4 C3 C2 121.0(3) . .
C3 C4 C5 122.2(3) . .
C4 C5 C6 116.5(3) . .
C4 C5 C8 122.9(3) . .
C6 C5 C8 120.7(3) . .
C7 C6 C5 122.0(3) . .
C6 C7 C2 121.3(3) . .
C9A C8 C10 74.5(10) . .
C9A C8 C11 119.1(12) . .
C10 C8 C11 116.5(10) . .
C9A C8 C5 117.2(9) . .
C10 C8 C5 112.2(4) . .
C11 C8 C5 112.3(8) . .
C9A C8 C11A 113.9(13) . .
C10 C8 C11A 116.6(10) . .
C11 C8 C11A 5.2(18) . .
C5 C8 C11A 116.0(10) . .
C9A C8 C9 30.3(10) . .
C10 C8 C9 104.8(7) . .
C11 C8 C9 104.9(9) . .
C5 C8 C9 105.0(4) . .
C11A C8 C9 100.0(10) . .
C9A C8 C10A 108.4(10) . .
C10 C8 C10A 34.7(5) . .
C11 C8 C10A 93.1(10) . .
C5 C8 C10A 102.2(6) . .
C11A C8 C10A 95.8(10) . .
C9 C8 C10A 138.4(7) . .
C17 C12 C13 121.2(3) . .
C17 C12 N1 119.6(3) . .
C13 C12 N1 119.0(3) . .
C14 C13 C12 118.1(3) . .
C14 C13 C18 119.5(3) . .
C12 C13 C18 122.4(3) . .
C15 C14 C13 121.1(4) . .
C16 C15 C14 119.9(3) . .
C15 C16 C17 121.4(4) . .
C16 C17 C12 118.2(3) . .
C16 C17 C21 120.2(3) . .
C12 C17 C21 121.6(3) . .
C19 C18 C20 109.8(3) . .
C19 C18 C13 112.8(3) . .
C20 C18 C13 112.4(3) . .
C17 C21 C22 112.3(3) . .
C17 C21 C23 110.7(3) . .
C22 C21 C23 111.4(3) . .
C25 C24 C29 121.3(3) . .
C25 C24 N2 120.3(3) . .
C29 C24 N2 118.3(3) . .
C26 C25 C24 117.8(3) . .
C26 C25 C30 118.5(3) . .
C24 C25 C30 123.6(3) . .
C27 C26 C25 121.5(3) . .
C26 C27 C28 120.2(3) . .
C27 C28 C29 121.0(3) . .
C28 C29 C24 118.1(3) . .
C28 C29 C33 120.6(3) . .
C24 C29 C33 121.3(3) . .
C25 C30 C32 112.5(3) . .
C25 C30 C31 110.0(3) . .
C32 C30 C31 111.5(3) . .
C29 C33 C34 113.0(3) . .
C29 C33 C35 112.3(3) . .
C34 C33 C35 109.8(3) . .
C36 C36 C37 123.3(8) 2_557 .
C38 C37 C36 118.9(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 N1 2.025(2) .
Ge1 N2 2.028(3) .
Ge1 Ge1 2.6136(9) 2_666
N1 C1 1.338(4) .
N1 C12 1.427(4) .
C1 N2 1.350(4) .
C1 C2 1.478(4) .
N2 C24 1.432(4) .
C2 C7 1.395(4) .
C2 C3 1.396(4) .
C3 C4 1.386(5) .
C4 C5 1.387(5) .
C5 C6 1.395(5) .
C5 C8 1.524(5) .
C6 C7 1.381(5) .
C8 C9A 1.412(15) .
C8 C10 1.489(9) .
C8 C11 1.496(14) .
C8 C11A 1.538(16) .
C8 C9 1.631(9) .
C8 C10A 1.672(14) .
C12 C17 1.400(4) .
C12 C13 1.406(5) .
C13 C14 1.394(5) .
C13 C18 1.523(5) .
C14 C15 1.379(5) .
C15 C16 1.375(6) .
C16 C17 1.393(5) .
C17 C21 1.523(5) .
C18 C19 1.509(6) .
C18 C20 1.520(5) .
C21 C22 1.526(5) .
C21 C23 1.527(6) .
C24 C25 1.407(4) .
C24 C29 1.408(4) .
C25 C26 1.397(4) .
C25 C30 1.513(5) .
C26 C27 1.370(5) .
C27 C28 1.383(5) .
C28 C29 1.394(4) .
C29 C33 1.522(5) .
C30 C32 1.527(5) .
C30 C31 1.533(5) .
C33 C34 1.526(5) .
C33 C35 1.531(5) .
C36 C36 1.406(11) 2_557
C36 C37 1.456(8) .
C37 C38 1.447(8) .
