#------------------------------------------------------------------------------
#$Date: 2025-08-20 14:05:43 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301829 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/40/4064030.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_4064030
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            'C72 H63 Br Ge4'
_chemical_formula_weight         1298.49
_chemical_name_common            'COMPUND 4'
_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                   18.6599(16)
_cell_length_b                   18.6599(16)
_cell_length_c                   10.0541(17)
_cell_measurement_reflns_used    6001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.18
_cell_volume                     3031.7(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29951
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    2.664
_exptl_absorpt_correction_T_max  0.7404
_exptl_absorpt_correction_T_min  0.5020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.127(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         4797
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0330P)²+2.5351P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                4090
_reflns_number_total             4797
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101091c_si_002.cif
_cod_data_source_block           wein95
_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               4064030
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.6667 0.3333 0.51116(6) 0.02977(18) Uani 1 3 d S . .
Ge1 Ge 0.6667 0.3333 0.74785(6) 0.01843(15) Uani 1 3 d S . .
Ge2 Ge 0.76314(2) 0.28229(2) 0.79633(5) 0.01849(9) Uani 1 1 d . . .
C1 C 0.7736(2) 0.2747(2) 0.9895(4) 0.0220(8) Uani 1 1 d . . .
C2 C 0.7787(2) 0.3365(3) 1.0739(4) 0.0256(8) Uani 1 1 d . . .
H2A H 0.7770 0.3825 1.0370 0.031 Uiso 1 1 calc R . .
C3 C 0.7862(3) 0.3320(3) 1.2099(4) 0.0323(10) Uani 1 1 d . . .
H3A H 0.7881 0.3740 1.2658 0.039 Uiso 1 1 calc R . .
C4 C 0.7910(3) 0.2666(3) 1.2650(4) 0.0346(11) Uani 1 1 d . . .
H4A H 0.7963 0.2635 1.3585 0.041 Uiso 1 1 calc R . .
C5 C 0.7881(3) 0.2060(3) 1.1830(4) 0.0380(12) Uani 1 1 d . . .
H5A H 0.7923 0.1615 1.2206 0.046 Uiso 1 1 calc R . .
C6 C 0.7792(2) 0.2089(3) 1.0462(4) 0.0278(9) Uani 1 1 d . . .
H6A H 0.7768 0.1664 0.9911 0.033 Uiso 1 1 calc R . .
C7 C 0.8736(2) 0.3594(2) 0.7277(4) 0.0246(8) Uani 1 1 d . . .
C8 C 0.9428(2) 0.3815(2) 0.8075(5) 0.0299(9) Uani 1 1 d . . .
H8A H 0.9354 0.3629 0.8971 0.036 Uiso 1 1 calc R . .
C9 C 1.0220(3) 0.4300(3) 0.7579(5) 0.0393(11) Uani 1 1 d . . .
H9A H 1.0685 0.4440 0.8133 0.047 Uiso 1 1 calc R . .
C10 C 1.0340(3) 0.4583(3) 0.6285(6) 0.0401(11) Uani 1 1 d . . .
H10A H 1.0885 0.4913 0.5948 0.048 Uiso 1 1 calc R . .
C11 C 0.9662(3) 0.4383(3) 0.5474(5) 0.0415(11) Uani 1 1 d . . .
H11A H 0.9744 0.4584 0.4587 0.050 Uiso 1 1 calc R . .
C12 C 0.8866(3) 0.3891(3) 0.5960(4) 0.0300(9) Uani 1 1 d . . .
H12A H 0.8405 0.3752 0.5400 0.036 Uiso 1 1 calc R . .
C13 C 0.7301(3) 0.1742(2) 0.7158(4) 0.0254(9) Uani 1 1 d . . .
C14 C 0.7808(3) 0.1687(3) 0.6196(5) 0.0378(10) Uani 1 1 d . . .
H14A H 0.8281 0.2177 0.5891 0.045 Uiso 1 1 calc R . .
C15 C 0.7631(4) 0.0920(3) 0.5672(5) 0.0508(13) Uani 1 1 d . . .
H15A H 0.7986 0.0890 0.5025 0.061 Uiso 1 1 calc R . .
C16 C 0.6940(3) 0.0212(3) 0.6098(6) 0.0502(14) Uani 1 1 d . . .
H16A H 0.6814 -0.0310 0.5742 0.060 Uiso 1 1 calc R . .
C17 C 0.6428(3) 0.0260(3) 0.7047(6) 0.0534(16) Uani 1 1 d . . .
H17A H 0.5949 -0.0230 0.7334 0.064 Uiso 1 1 calc R . .
C18 C 0.6608(2) 0.1018(2) 0.7584(5) 0.0377(11) Uani 1 1 d . . .
H18A H 0.6256 0.1042 0.8245 0.045 Uiso 1 1 calc R . .
C19 C 0.8661(7) 0.0478(6) 0.1841(6) 0.0733(13) Uani 0.558(9) 1 d PG A 1
H19A H 0.8804 0.0531 0.2757 0.088 Uiso 0.558(9) 1 calc PR A 1
C20 C 0.9280(4) 0.0783(5) 0.0880(12) 0.0733(13) Uani 0.558(9) 1 d PG A 1
H20A H 0.9844 0.1044 0.1139 0.088 Uiso 0.558(9) 1 calc PR A 1
C21 C 0.9071(6) 0.0706(6) -0.0461(10) 0.0733(13) Uani 0.558(9) 1 d PG A 1
H21A H 0.9494 0.0914 -0.1118 0.088 Uiso 0.558(9) 1 calc PR A 1
C22 C 0.8245(8) 0.0323(7) -0.0840(6) 0.0733(13) Uani 0.558(9) 1 d PG A 1
H22A H 0.8102 0.0270 -0.1756 0.088 Uiso 0.558(9) 1 calc PR A 1
C23 C 0.7627(4) 0.0018(6) 0.0122(12) 0.0733(13) Uani 0.558(9) 1 d PG A 1
H23A H 0.7062 -0.0244 -0.0138 0.088 Uiso 0.558(9) 1 calc PR A 1
C24 C 0.7835(6) 0.0095(6) 0.1462(10) 0.0733(13) Uani 0.558(9) 1 d PG A 1
H24A H 0.7413 -0.0113 0.2119 0.088 Uiso 0.558(9) 1 calc PR A 1
C19A C 0.8960(8) 0.0440(8) 0.1484(13) 0.0733(13) Uani 0.442(9) 1 d PG A 2
H19B H 0.9331 0.0539 0.2199 0.088 Uiso 0.442(9) 1 calc PR A 2
C20A C 0.9253(5) 0.0602(7) 0.0184(17) 0.0733(13) Uani 0.442(9) 1 d PG A 2
H20B H 0.9824 0.0812 0.0012 0.088 Uiso 0.442(9) 1 calc PR A 2
C21A C 0.8710(10) 0.0457(9) -0.0862(9) 0.0733(13) Uani 0.442(9) 1 d PG A 2
H21B H 0.8911 0.0568 -0.1750 0.088 Uiso 0.442(9) 1 calc PR A 2
C22A C 0.7875(9) 0.0150(9) -0.0610(12) 0.0733(13) Uani 0.442(9) 1 d PG A 2
H22B H 0.7504 0.0051 -0.1325 0.088 Uiso 0.442(9) 1 calc PR A 2
C23A C 0.7581(5) -0.0012(9) 0.0690(16) 0.0733(13) Uani 0.442(9) 1 d PG A 2
H23B H 0.7010 -0.0222 0.0863 0.088 Uiso 0.442(9) 1 calc PR A 2
C24A C 0.8124(9) 0.0133(9) 0.1737(9) 0.0733(13) Uani 0.442(9) 1 d PG A 2
H24B H 0.7924 0.0022 0.2625 0.088 Uiso 0.442(9) 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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
Br1 Ge1 Ge2 101.382(18) . .
Br1 Ge1 Ge2 101.382(18) . 3_665
Ge2 Ge1 Ge2 116.205(12) . 3_665
Br1 Ge1 Ge2 101.382(18) . 2_655
Ge2 Ge1 Ge2 116.205(12) . 2_655
Ge2 Ge1 Ge2 116.205(12) 3_665 2_655
C7 Ge2 C13 106.54(17) . .
C7 Ge2 C1 107.20(17) . .
C13 Ge2 C1 108.98(16) . .
C7 Ge2 Ge1 110.45(12) . .
C13 Ge2 Ge1 113.52(12) . .
C1 Ge2 Ge1 109.91(11) . .
C2 C1 C6 118.1(4) . .
C2 C1 Ge2 120.7(3) . .
C6 C1 Ge2 121.2(3) . .
C3 C2 C1 121.3(4) . .
C3 C2 H2A 119.4 . .
C1 C2 H2A 119.4 . .
C2 C3 C4 120.1(4) . .
C2 C3 H3A 119.9 . .
C4 C3 H3A 119.9 . .
C5 C4 C3 119.4(4) . .
C5 C4 H4A 120.3 . .
C3 C4 H4A 120.3 . .
C4 C5 C6 121.0(5) . .
C4 C5 H5A 119.5 . .
C6 C5 H5A 119.5 . .
C5 C6 C1 120.0(4) . .
C5 C6 H6A 120.0 . .
C1 C6 H6A 120.0 . .
C8 C7 C12 118.2(4) . .
C8 C7 Ge2 119.5(3) . .
C12 C7 Ge2 122.1(3) . .
C9 C8 C7 120.9(5) . .
C9 C8 H8A 119.6 . .
C7 C8 H8A 119.6 . .
C10 C9 C8 120.4(4) . .
C10 C9 H9A 119.8 . .
C8 C9 H9A 119.8 . .
C9 C10 C11 120.0(4) . .
C9 C10 H10A 120.0 . .
C11 C10 H10A 120.0 . .
C12 C11 C10 120.1(4) . .
C12 C11 H11A 120.0 . .
C10 C11 H11A 120.0 . .
C11 C12 C7 120.5(4) . .
C11 C12 H12A 119.7 . .
C7 C12 H12A 119.7 . .
C14 C13 C18 118.6(4) . .
C14 C13 Ge2 119.1(3) . .
C18 C13 Ge2 122.2(3) . .
C13 C14 C15 121.0(5) . .
C13 C14 H14A 119.5 . .
C15 C14 H14A 119.5 . .
C16 C15 C14 119.6(5) . .
C16 C15 H15A 120.2 . .
C14 C15 H15A 120.2 . .
C15 C16 C17 119.9(4) . .
C15 C16 H16A 120.1 . .
C17 C16 H16A 120.1 . .
C16 C17 C18 120.7(5) . .
C16 C17 H17A 119.6 . .
C18 C17 H17A 119.6 . .
C13 C18 C17 120.2(5) . .
C13 C18 H18A 119.9 . .
C17 C18 H18A 119.9 . .
C20 C19 C24 120.0 . .
C20 C19 H19A 120.0 . .
C24 C19 H19A 120.0 . .
C19 C20 C21 120.0 . .
C19 C20 H20A 120.0 . .
C21 C20 H20A 120.0 . .
C22 C21 C20 120.0 . .
C22 C21 H21A 120.0 . .
C20 C21 H21A 120.0 . .
C21 C22 C23 120.0 . .
C21 C22 H22A 120.0 . .
C23 C22 H22A 120.0 . .
C24 C23 C22 120.0 . .
C24 C23 H23A 120.0 . .
C22 C23 H23A 120.0 . .
C23 C24 C19 120.0 . .
C23 C24 H24A 120.0 . .
C19 C24 H24A 120.0 . .
C20A C19A C24A 120.0 . .
C20A C19A H19B 120.0 . .
C24A C19A H19B 120.0 . .
C21A C20A C19A 120.0 . .
C21A C20A H20B 120.0 . .
C19A C20A H20B 120.0 . .
C22A C21A C20A 120.0 . .
C22A C21A H21B 120.0 . .
C20A C21A H21B 120.0 . .
C21A C22A C23A 120.0 . .
C21A C22A H22B 120.0 . .
C23A C22A H22B 120.0 . .
C24A C23A C22A 120.0 . .
C24A C23A H23B 120.0 . .
C22A C23A H23B 120.0 . .
C23A C24A C19A 120.0 . .
C23A C24A H24B 120.0 . .
C19A C24A H24B 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Ge1 2.3796(9) .
Ge1 Ge2 2.4698(4) .
Ge1 Ge2 2.4698(4) 3_665
Ge1 Ge2 2.4698(4) 2_655
Ge2 C7 1.957(4) .
Ge2 C13 1.965(4) .
Ge2 C1 1.964(4) .
C1 C2 1.395(6) .
C1 C6 1.404(5) .
C2 C3 1.382(5) .
C2 H2A 0.9500 .
C3 C4 1.384(7) .
C3 H3A 0.9500 .
C4 C5 1.379(6) .
C4 H4A 0.9500 .
C5 C6 1.390(6) .
C5 H5A 0.9500 .
C6 H6A 0.9500 .
C7 C8 1.396(6) .
C7 C12 1.409(6) .
C8 C9 1.385(6) .
C8 H8A 0.9500 .
C9 C10 1.379(8) .
C9 H9A 0.9500 .
C10 C11 1.389(7) .
C10 H10A 0.9500 .
C11 C12 1.388(6) .
C11 H11A 0.9500 .
C12 H12A 0.9500 .
C13 C14 1.393(6) .
C13 C18 1.390(6) .
C14 C15 1.400(6) .
C14 H14A 0.9500 .
C15 C16 1.374(7) .
C15 H15A 0.9500 .
C16 C17 1.385(8) .
C16 H16A 0.9500 .
C17 C18 1.389(6) .
C17 H17A 0.9500 .
C18 H18A 0.9500 .
C19 C20 1.3900 .
C19 C24 1.3900 .
C19 H19A 0.9500 .
C20 C21 1.3900 .
C20 H20A 0.9500 .
C21 C22 1.3900 .
C21 H21A 0.9500 .
C22 C23 1.3900 .
C22 H22A 0.9500 .
C23 C24 1.3900 .
C23 H23A 0.9500 .
C24 H24A 0.9500 .
C19A C20A 1.3900 .
C19A C24A 1.3900 .
C19A H19B 0.9500 .
C20A C21A 1.3900 .
C20A H20B 0.9500 .
C21A C22A 1.3900 .
C21A H21B 0.9500 .
C22A C23A 1.3900 .
C22A H22B 0.9500 .
C23A C24A 1.3900 .
C23A H23B 0.9500 .
C24A H24B 0.9500 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139097540
