#------------------------------------------------------------------------------
#$Date: 2025-08-20 14:05:43 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301829 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/40/4064029.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_4064029
loop_
_publ_author_name
'Samanamu, Christian R.'
'Amadoruge, Monika L.'
'Yoder, Claude H.'
'Golen, James A.'
'Moore, Curtis E.'
'Rheingold, Arnold L.'
'Materer, Nicholas F.'
'Weinert, Charles S.'
_publ_section_title
;
 Syntheses, Structures, and Electronic Properties of the Branched
 Oligogermanes (Ph3Ge)3GeH and (Ph3Ge)3GeX (X = Cl, Br, I)†
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1046
_journal_paper_doi               10.1021/om101091c
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C78 H75 Cl Ge4'
_chemical_formula_weight         1338.19
_chemical_name_common            'COMPOUND 3b'
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   18.6792(14)
_cell_length_b                   18.6792(14)
_cell_length_c                   9.8740(7)
_cell_measurement_reflns_used    3092
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.18
_cell_volume                     2983.6(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12563
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    2.088
_exptl_absorpt_correction_T_max  0.8029
_exptl_absorpt_correction_T_min  0.6129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.032(17)
_refine_ls_extinction_coef       0.0002(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4404
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0487
_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)+(0.0560P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1173
_reflns_number_gt                3608
_reflns_number_total             4404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101091c_si_002.cif
_cod_data_source_block           wein72
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P6(3)
_cod_database_code               4064029
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, 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 0.3333 0.6667 0.57815(8) 0.0197(2) Uani 1 3 d S
Ge2 Ge 0.23741(3) 0.51942(3) 0.52720(6) 0.01936(14) Uani 1 1 d .
Cl1 Cl 0.3333 0.6667 0.8025(2) 0.0299(6) Uani 1 3 d S
C1 C 0.1265(3) 0.4863(3) 0.5975(5) 0.0229(10) Uani 1 1 d .
C2 C 0.1156(3) 0.5042(3) 0.7293(5) 0.0274(12) Uani 1 1 d .
H2 H 0.1622 0.5366 0.7852 0.033 Uiso 1 1 calc R
C3 C 0.0363(4) 0.4747(4) 0.7796(6) 0.0389(15) Uani 1 1 d .
H3 H 0.0285 0.4880 0.8693 0.047 Uiso 1 1 calc R
C4 C -0.0311(4) 0.4262(4) 0.6989(7) 0.0388(14) Uani 1 1 d .
H4 H -0.0854 0.4052 0.7335 0.047 Uiso 1 1 calc R
C5 C -0.0198(3) 0.4081(4) 0.5680(6) 0.0389(14) Uani 1 1 d .
H5 H -0.0664 0.3746 0.5126 0.047 Uiso 1 1 calc R
C6 C 0.0585(3) 0.4382(3) 0.5175(7) 0.0284(11) Uani 1 1 d .
H6 H 0.0659 0.4258 0.4270 0.034 Uiso 1 1 calc R
C7 C 0.2695(3) 0.4436(3) 0.6071(5) 0.0259(12) Uani 1 1 d .
C8 C 0.2166(4) 0.3847(3) 0.7033(6) 0.0342(13) Uani 1 1 d .
H8 H 0.1686 0.3855 0.7335 0.041 Uiso 1 1 calc R
C9 C 0.2340(5) 0.3263(4) 0.7537(6) 0.0460(17) Uani 1 1 d .
H9 H 0.1977 0.2863 0.8169 0.055 Uiso 1 1 calc R
C10 C 0.3055(4) 0.3260(4) 0.7113(7) 0.0467(17) Uani 1 1 d .
H10 H 0.3180 0.2862 0.7466 0.056 Uiso 1 1 calc R
C11 C 0.3565(4) 0.3824(4) 0.6200(7) 0.0451(17) Uani 1 1 d .
H11 H 0.4048 0.3818 0.5919 0.054 Uiso 1 1 calc R
C12 C 0.3399(3) 0.4416(3) 0.5662(6) 0.0330(13) Uani 1 1 d .
H12 H 0.3765 0.4805 0.5017 0.040 Uiso 1 1 calc R
C13 C 0.2269(3) 0.5014(3) 0.3322(5) 0.0211(11) Uani 1 1 d .
C14 C 0.2219(3) 0.4305(4) 0.2737(5) 0.0288(12) Uani 1 1 d .
H14 H 0.2248 0.3905 0.3294 0.035 Uiso 1 1 calc R
C15 C 0.2128(4) 0.4187(4) 0.1351(6) 0.0375(15) Uani 1 1 d .
H15 H 0.2085 0.3700 0.0970 0.045 Uiso 1 1 calc R
C16 C 0.2098(3) 0.4754(4) 0.0520(5) 0.0385(15) Uani 1 1 d .
H16 H 0.2046 0.4665 -0.0431 0.046 Uiso 1 1 calc R
C17 C 0.2145(3) 0.5468(4) 0.1071(6) 0.0353(14) Uani 1 1 d .
H17 H 0.2120 0.5863 0.0499 0.042 Uiso 1 1 calc R
C18 C 0.2227(3) 0.5588(3) 0.2455(5) 0.0283(12) Uani 1 1 d .
H18 H 0.2256 0.6070 0.2829 0.034 Uiso 1 1 calc R
C1S C 0.1583(8) 0.0532(7) 0.8998(10) 0.192(9) Uani 1 1 d G
H1S H 0.1385 0.0678 0.9776 0.230 Uiso 1 1 calc R
C2S C 0.1359(5) 0.0652(6) 0.7712(14) 0.129(6) Uani 1 1 d G
H2S H 0.1008 0.0881 0.7611 0.155 Uiso 1 1 calc R
C3S C 0.1648(8) 0.0437(6) 0.6574(9) 0.160(7) Uani 1 1 d G
H3S H 0.1495 0.0520 0.5695 0.192 Uiso 1 1 calc R
C4S C 0.2161(7) 0.0102(6) 0.6721(13) 0.207(11) Uani 1 1 d G
H4S H 0.2359 -0.0044 0.5943 0.248 Uiso 1 1 calc R
C5S C 0.2385(4) -0.0018(4) 0.8007(18) 0.113(5) Uani 1 1 d G
H5S H 0.2736 -0.0247 0.8108 0.136 Uiso 1 1 calc R
C6S C 0.2096(8) 0.0196(6) 0.9145(11) 0.235(12) Uani 1 1 d G
H6S H 0.2249 0.0114 1.0024 0.282 Uiso 1 1 calc R
C7S C 0.0661(3) 0.0094(3) 0.4985(6) 0.0329(14) Uani 1 1 d .
H7S1 H 0.0499 0.0063 0.4023 0.039 Uiso 1 1 calc R
H7S2 H 0.1228 0.0182 0.5057 0.039 Uiso 1 1 calc R
C8S C 0.0108(3) -0.0552(3) 0.5719(6) 0.0307(12) Uani 1 1 d .
H8S1 H 0.0088 -0.0406 0.6677 0.037 Uiso 1 1 calc R
H8S2 H 0.0192 -0.1034 0.5666 0.037 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'
Cl Cl 0.1484 0.1585 '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
Cl1 Ge1 Ge2 101.75(2) . 5_565
Cl1 Ge1 Ge2 101.75(2) . .
Ge2 Ge1 Ge2 115.962(16) 5_565 .
Cl1 Ge1 Ge2 101.75(2) . 4_665
Ge2 Ge1 Ge2 115.962(16) 5_565 4_665
Ge2 Ge1 Ge2 115.962(16) . 4_665
C13 Ge2 C7 108.3(2) . .
C13 Ge2 C1 107.1(2) . .
C7 Ge2 C1 106.5(2) . .
C13 Ge2 Ge1 110.36(15) . .
C7 Ge2 Ge1 114.17(16) . .
C1 Ge2 Ge1 110.01(15) . .
C6 C1 C2 119.7(5) . .
C6 C1 Ge2 119.0(4) . .
C2 C1 Ge2 121.0(4) . .
C1 C2 C3 119.9(5) . .
C1 C2 H2 120.1 . .
C3 C2 H2 120.1 . .
C4 C3 C2 119.7(6) . .
C4 C3 H3 120.1 . .
C2 C3 H3 120.1 . .
C3 C4 C5 120.2(5) . .
C3 C4 H4 119.9 . .
C5 C4 H4 119.9 . .
C6 C5 C4 120.1(6) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C5 C6 C1 120.4(6) . .
C5 C6 H6 119.8 . .
C1 C6 H6 119.8 . .
C12 C7 C8 118.4(5) . .
C12 C7 Ge2 122.4(4) . .
C8 C7 Ge2 119.0(4) . .
C9 C8 C7 120.5(6) . .
C9 C8 H8 119.8 . .
C7 C8 H8 119.8 . .
C8 C9 C10 119.9(6) . .
C8 C9 H9 120.0 . .
C10 C9 H9 120.0 . .
C11 C10 C9 119.8(6) . .
C11 C10 H10 120.1 . .
C9 C10 H10 120.1 . .
C10 C11 C12 121.6(6) . .
C10 C11 H11 119.2 . .
C12 C11 H11 119.2 . .
C11 C12 C7 119.8(6) . .
C11 C12 H12 120.1 . .
C7 C12 H12 120.1 . .
C18 C13 C14 117.8(5) . .
C18 C13 Ge2 120.7(4) . .
C14 C13 Ge2 121.5(4) . .
C15 C14 C13 120.1(6) . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C16 C15 C14 121.5(6) . .
C16 C15 H15 119.3 . .
C14 C15 H15 119.3 . .
C15 C16 C17 119.9(5) . .
C15 C16 H16 120.0 . .
C17 C16 H16 120.0 . .
C18 C17 C16 119.2(6) . .
C18 C17 H17 120.4 . .
C16 C17 H17 120.4 . .
C17 C18 C13 121.6(6) . .
C17 C18 H18 119.2 . .
C13 C18 H18 119.2 . .
C2S C1S C6S 120.0 . .
C2S C1S H1S 120.0 . .
C6S C1S H1S 120.0 . .
C3S C2S C1S 120.0 . .
C3S C2S H2S 120.0 . .
C1S C2S H2S 120.0 . .
C4S C3S C2S 120.0 . .
C4S C3S H3S 120.0 . .
C2S C3S H3S 120.0 . .
C3S C4S C5S 120.0 . .
C3S C4S H4S 120.0 . .
C5S C4S H4S 120.0 . .
C6S C5S C4S 120.0 . .
C6S C5S H5S 120.0 . .
C4S C5S H5S 120.0 . .
C5S C6S C1S 120.0 . .
C5S C6S H6S 120.0 . .
C1S C6S H6S 120.0 . .
C8S C7S C8S 93.5(6) . 4
C8S C7S C7S 43.2(4) . 5
C8S C7S C7S 89.0(3) 4 5
C8S C7S C7S 90.0(3) . 4
C8S C7S C7S 41.9(3) 4 4
C7S C7S C7S 60.000(1) 5 4
C8S C7S H7S1 113.0 . .
C8S C7S H7S1 113.0 4 .
C7S C7S H7S1 75.5 5 .
C7S C7S H7S1 76.3 4 .
C8S C7S H7S2 113.0 . .
C8S C7S H7S2 113.0 4 .
C7S C7S H7S2 150.5 5 .
C7S C7S H7S2 149.0 4 .
H7S1 C7S H7S2 110.4 . .
C7S C8S C7S 94.9(6) . 5
C7S C8S C8S 43.9(4) . 4
C7S C8S C8S 90.0(3) 5 4
C7S C8S C8S 91.0(3) . 5
C7S C8S C8S 42.5(3) 5 5
C8S C8S C8S 60.000(1) 4 5
C7S C8S H8S1 112.8 . .
C7S C8S H8S1 112.8 5 .
C8S C8S H8S1 74.8 4 .
C8S C8S H8S1 75.6 5 .
C7S C8S H8S2 112.8 . .
C7S C8S H8S2 112.8 5 .
C8S C8S H8S2 150.7 4 .
C8S C8S H8S2 149.1 5 .
H8S1 C8S H8S2 110.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 Cl1 2.215(2) .
Ge1 Ge2 2.4699(5) 5_565
Ge1 Ge2 2.4699(5) .
Ge1 Ge2 2.4699(5) 4_665
Ge2 C13 1.947(5) .
Ge2 C7 1.959(5) .
Ge2 C1 1.968(5) .
C1 C6 1.380(7) .
C1 C2 1.385(7) .
C2 C3 1.389(8) .
C2 H2 0.9500 .
C3 C4 1.378(9) .
C3 H3 0.9500 .
C4 C5 1.379(9) .
C4 H4 0.9500 .
C5 C6 1.371(7) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C12 1.394(7) .
C7 C8 1.415(8) .
C8 C9 1.380(8) .
C8 H8 0.9500 .
C9 C10 1.401(9) .
C9 H9 0.9500 .
C10 C11 1.352(9) .
C10 H10 0.9500 .
C11 C12 1.394(8) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C18 1.404(7) .
C13 C14 1.407(7) .
C14 C15 1.383(7) .
C14 H14 0.9500 .
C15 C16 1.362(8) .
C15 H15 0.9500 .
C16 C17 1.402(9) .
C16 H16 0.9500 .
C17 C18 1.382(7) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C1S C2S 1.3900 .
C1S C6S 1.3900 .
C1S H1S 0.9500 .
C2S C3S 1.3900 .
C2S H2S 0.9500 .
C3S C4S 1.3900 .
C3S H3S 0.9500 .
C4S C5S 1.3900 .
C4S H4S 0.9500 .
C5S C6S 1.3900 .
C5S H5S 0.9500 .
C6S H6S 0.9500 .
C7S C8S 1.342(7) .
C7S C8S 1.378(7) 4
C7S C7S 2.004(10) 5
C7S C7S 2.004(10) 4
C7S H7S1 0.9900 .
C7S H7S2 0.9900 .
C8S C7S 1.378(7) 5
C8S C8S 1.981(9) 4
C8S C8S 1.981(9) 5
C8S H8S1 0.9900 .
C8S H8S2 0.9900 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139097539
