#------------------------------------------------------------------------------
#$Date: 2016-02-18 10:31:59 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176720 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/42/7224296.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_7224296
loop_
_publ_author_name
'Böserle, Jiří'
'Alonso, Mercedes'
'Jambor, Roman'
'R°užička, Aleš'
'Dostál, Libor'
_publ_section_title
;
 Synthesis and reactivity of a germylene stabilized by a boraguanidinate
 ligand
;
_journal_issue                   23
_journal_name_full               'RSC Adv.'
_journal_page_first              19377
_journal_paper_doi               10.1039/C6RA01187J
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C44 H64 B2 Ge2 N6'
_chemical_formula_sum            'C44 H64 B2 Ge2 N6'
_chemical_formula_weight         843.81
_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
_audit_update_record
;
2015-07-20 deposited with the CCDC.
2016-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                112.083(3)
_cell_angle_beta                 94.293(4)
_cell_angle_gamma                107.174(4)
_cell_formula_units_Z            1
_cell_length_a                   8.9930(5)
_cell_length_b                   11.4140(6)
_cell_length_c                   11.9331(6)
_cell_measurement_reflns_used    18055
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1060.25(11)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17968
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.122
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4807
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0271P)²+1.2349P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                4318
_reflns_number_total             4807
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra01187j2.cif
_cod_data_source_block           shelxl
_cod_database_code               7224296
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
Ge1 Ge 1.07823(2) 0.40911(2) 0.424326(19) 0.01619(7) Uani 1 1 d .
N3 N 0.85891(19) 0.29067(17) 0.34924(15) 0.0174(3) Uani 1 1 d .
N2 N 0.94572(19) 0.51896(16) 0.38976(15) 0.0161(3) Uani 1 1 d .
N1 N 0.6743(2) 0.36524(17) 0.23562(16) 0.0195(4) Uani 1 1 d .
C8 C 1.0034(2) 0.7406(2) 0.37512(19) 0.0216(4) Uani 1 1 d .
C7 C 1.0098(2) 0.6093(2) 0.33170(18) 0.0180(4) Uani 1 1 d .
C12 C 1.0775(2) 0.5647(2) 0.22752(19) 0.0215(4) Uani 1 1 d .
C15 C 0.7777(2) 0.1535(2) 0.32430(18) 0.0187(4) Uani 1 1 d .
C13 C 0.9105(3) 0.7937(2) 0.4698(2) 0.0249(5) Uani 1 1 d .
H13A H 0.8260 0.7197 0.4708 0.030 Uiso 1 1 d R
H13B H 0.8664 0.8517 0.4489 0.030 Uiso 1 1 d R
H13C H 0.9800 0.8439 0.5500 0.030 Uiso 1 1 d R
C16 C 0.8256(3) 0.0510(2) 0.24478(19) 0.0223(4) Uani 1 1 d .
C22 C 0.5937(3) 0.2263(2) 0.4647(2) 0.0254(5) Uani 1 1 d .
H22A H 0.4951 0.1840 0.4830 0.031 Uiso 1 1 d R
H22B H 0.5784 0.2829 0.4258 0.031 Uiso 1 1 d R
H22C H 0.6727 0.2800 0.5401 0.031 Uiso 1 1 d R
C17 C 0.7457(3) -0.0825(2) 0.2241(2) 0.0298(5) Uani 1 1 d .
H17 H 0.7788 -0.1504 0.1735 0.036 Uiso 1 1 d R
C14 C 1.0708(3) 0.4211(2) 0.1611(2) 0.0264(5) Uani 1 1 d .
H14A H 1.0897 0.4055 0.0794 0.032 Uiso 1 1 d R
H14B H 0.9679 0.3601 0.1554 0.032 Uiso 1 1 d R
H14C H 1.1511 0.4066 0.2064 0.032 Uiso 1 1 d R
B1 B 0.8107(3) 0.3841(2) 0.3174(2) 0.0170(4) Uani 1 1 d .
C1 C 0.6344(3) 0.4839(2) 0.2436(2) 0.0254(5) Uani 1 1 d .
H1 H 0.7320 0.5619 0.2889 0.030 Uiso 1 1 d R
C20 C 0.6483(2) 0.1200(2) 0.37921(19) 0.0212(4) Uani 1 1 d .
C21 C 0.9601(3) 0.0819(2) 0.1810(2) 0.0317(5) Uani 1 1 d .
H21A H 0.9771 -0.0002 0.1333 0.038 Uiso 1 1 d R
H21B H 1.0552 0.1442 0.2416 0.038 Uiso 1 1 d R
H21C H 0.9339 0.1210 0.1272 0.038 Uiso 1 1 d R
C10 C 1.1547(3) 0.7867(3) 0.2276(2) 0.0352(6) Uani 1 1 d .
H10 H 1.2084 0.8470 0.1966 0.042 Uiso 1 1 d R
C18 C 0.6180(3) -0.1157(2) 0.2780(2) 0.0335(5) Uani 1 1 d .
H18 H 0.5652 -0.2052 0.2631 0.040 Uiso 1 1 d R
C9 C 1.0789(3) 0.8270(2) 0.3232(2) 0.0298(5) Uani 1 1 d .
H9 H 1.0778 0.9146 0.3543 0.036 Uiso 1 1 d R
C4 C 0.5717(3) 0.2270(2) 0.1464(2) 0.0300(5) Uani 1 1 d .
H4 H 0.6067 0.1684 0.1763 0.036 Uiso 1 1 d R
C19 C 0.5689(3) -0.0155(2) 0.3535(2) 0.0284(5) Uani 1 1 d .
H19 H 0.4816 -0.0381 0.3883 0.034 Uiso 1 1 d R
C11 C 1.1500(3) 0.6550(3) 0.1785(2) 0.0305(5) Uani 1 1 d .
H11 H 1.1963 0.6255 0.1111 0.037 Uiso 1 1 d R
C2 C 0.5098(3) 0.5055(3) 0.3232(3) 0.0529(8) Uani 1 1 d .
H2A H 0.4119 0.4301 0.2849 0.063 Uiso 1 1 d R
H2B H 0.4920 0.5867 0.3307 0.063 Uiso 1 1 d R
H2C H 0.5480 0.5132 0.4039 0.063 Uiso 1 1 d R
C3 C 0.5933(6) 0.4895(3) 0.1222(3) 0.0683(12) Uani 1 1 d .
H3A H 0.6857 0.5013 0.0864 0.082 Uiso 1 1 d R
H3B H 0.5570 0.5637 0.1349 0.082 Uiso 1 1 d R
H3C H 0.5106 0.4066 0.0675 0.082 Uiso 1 1 d R
C5 C 0.3974(3) 0.1881(3) 0.1478(3) 0.0462(7) Uani 1 1 d .
H5A H 0.3508 0.2364 0.1139 0.055 Uiso 1 1 d R
H5B H 0.3840 0.2099 0.2315 0.055 Uiso 1 1 d R
H5C H 0.3460 0.0928 0.0992 0.055 Uiso 1 1 d R
C6 C 0.6068(4) 0.1891(3) 0.0194(2) 0.0434(7) Uani 1 1 d .
H6A H 0.5759 0.2422 -0.0177 0.052 Uiso 1 1 d R
H6B H 0.5480 0.0951 -0.0303 0.052 Uiso 1 1 d R
H6C H 0.7187 0.2054 0.0245 0.052 Uiso 1 1 d 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'
B B 0.0013 0.0007 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 0 0.081
-1 1 0 0.053
0 -1 0 0.160
1 1 0 0.134
0 0 -1 0.079
0 0 1 0.054
0 1 -1 0.151
0 -1 1 0.117
-1 0 0 0.144
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
N3 Ge1 N2 70.53(7) . .
N3 Ge1 N2 97.91(7) . 2_766
N2 Ge1 N2 89.84(6) . 2_766
N3 Ge1 B1 34.14(7) . .
N2 Ge1 B1 37.18(7) . .
N2 Ge1 B1 100.52(7) 2_766 .
C15 N3 B1 131.77(17) . .
C15 N3 Ge1 132.13(13) . .
B1 N3 Ge1 95.88(13) . .
C7 N2 B1 121.10(16) . .
C7 N2 Ge1 119.20(12) . .
B1 N2 Ge1 87.06(11) . .
C7 N2 Ge1 122.31(12) . 2_766
B1 N2 Ge1 107.80(12) . 2_766
Ge1 N2 Ge1 90.16(6) . 2_766
B1 N1 C1 118.93(17) . .
B1 N1 C4 119.93(18) . .
C1 N1 C4 121.12(17) . .
C9 C8 C7 119.3(2) . .
C9 C8 C13 116.0(2) . .
C7 C8 C13 124.57(19) . .
C8 C7 C12 118.43(18) . .
C8 C7 N2 121.71(18) . .
C12 C7 N2 119.85(18) . .
C11 C12 C7 119.5(2) . .
C11 C12 C14 116.8(2) . .
C7 C12 C14 123.65(19) . .
C20 C15 C16 119.85(19) . .
C20 C15 N3 119.66(18) . .
C16 C15 N3 120.49(19) . .
C8 C13 H13A 109.6 . .
C8 C13 H13B 109.4 . .
H13A C13 H13B 109.5 . .
C8 C13 H13C 109.4 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C17 C16 C15 119.2(2) . .
C17 C16 C21 119.2(2) . .
C15 C16 C21 121.6(2) . .
C20 C22 H22A 109.5 . .
C20 C22 H22B 109.4 . .
H22A C22 H22B 109.5 . .
C20 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C18 C17 C16 121.0(2) . .
C18 C17 H17 119.4 . .
C16 C17 H17 119.6 . .
C12 C14 H14A 109.6 . .
C12 C14 H14B 109.6 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.2 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
N1 B1 N3 131.09(19) . .
N1 B1 N2 124.57(18) . .
N3 B1 N2 104.31(17) . .
N1 B1 Ge1 168.28(15) . .
N3 B1 Ge1 49.98(10) . .
N2 B1 Ge1 55.77(9) . .
N1 C1 C3 115.0(2) . .
N1 C1 C2 111.8(2) . .
C3 C1 C2 112.6(3) . .
N1 C1 H1 105.5 . .
C3 C1 H1 105.3 . .
C2 C1 H1 105.6 . .
C19 C20 C15 119.1(2) . .
C19 C20 C22 119.4(2) . .
C15 C20 C22 121.48(18) . .
C16 C21 H21A 109.2 . .
C16 C21 H21B 109.6 . .
H21A C21 H21B 109.5 . .
C16 C21 H21C 109.6 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C9 C10 C11 118.7(2) . .
C9 C10 H10 120.7 . .
C11 C10 H10 120.6 . .
C19 C18 C17 119.7(2) . .
C19 C18 H18 120.1 . .
C17 C18 H18 120.2 . .
C10 C9 C8 122.0(2) . .
C10 C9 H9 119.0 . .
C8 C9 H9 119.0 . .
N1 C4 C6 113.4(2) . .
N1 C4 C5 116.3(2) . .
C6 C4 C5 114.0(2) . .
N1 C4 H4 103.7 . .
C6 C4 H4 103.6 . .
C5 C4 H4 103.9 . .
C18 C19 C20 121.2(2) . .
C18 C19 H19 119.6 . .
C20 C19 H19 119.2 . .
C10 C11 C12 121.7(2) . .
C10 C11 H11 119.2 . .
C12 C11 H11 119.1 . .
C1 C2 H2A 109.6 . .
C1 C2 H2B 109.4 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C1 C3 H3A 109.6 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.3 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C4 C5 H5A 109.8 . .
C4 C5 H5B 109.3 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.3 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C4 C6 H6A 109.5 . .
C4 C6 H6B 109.3 . .
H6A C6 H6B 109.5 . .
C4 C6 H6C 109.6 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 N3 1.9418(16) .
Ge1 N2 2.0881(16) .
Ge1 N2 2.1092(16) 2_766
Ge1 B1 2.522(2) .
N3 C15 1.420(3) .
N3 B1 1.423(3) .
N2 C7 1.456(2) .
N2 B1 1.526(3) .
N2 Ge1 2.1092(16) 2_766
N1 B1 1.417(3) .
N1 C1 1.473(3) .
N1 C4 1.484(3) .
C8 C9 1.394(3) .
C8 C7 1.411(3) .
C8 C13 1.506(3) .
C7 C12 1.413(3) .
C12 C11 1.393(3) .
C12 C14 1.509(3) .
C15 C20 1.403(3) .
C15 C16 1.407(3) .
C13 H13A 0.9601 .
C13 H13B 0.9601 .
C13 H13C 0.9600 .
C16 C17 1.395(3) .
C16 C21 1.501(3) .
C22 C20 1.500(3) .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9601 .
C17 C18 1.383(4) .
C17 H17 0.9300 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C1 C3 1.497(4) .
C1 C2 1.537(4) .
C1 H1 0.9800 .
C20 C19 1.399(3) .
C21 H21A 0.9601 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
C10 C9 1.373(4) .
C10 C11 1.379(4) .
C10 H10 0.9300 .
C18 C19 1.377(4) .
C18 H18 0.9300 .
C9 H9 0.9300 .
C4 C6 1.498(4) .
C4 C5 1.501(3) .
C4 H4 0.9800 .
C19 H19 0.9300 .
C11 H11 0.9300 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9599 .
C3 H3C 0.9600 .
C5 H5A 0.9600 .
C5 H5B 0.9599 .
C5 H5C 0.9600 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
