#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:56:29 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180203 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/97/7109741.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_7109741
loop_
_publ_author_name
'Kimberly D. Roewe'
'Arnold L. Rheingold'
'Charles S. Weinert'
_publ_section_title
;
 A luminescent and dichroic hexagermane
;
_journal_name_full               Chem.Commun.
_journal_page_first              8380
_journal_paper_doi               10.1039/c3cc45450a
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C66 H82 Ge6'
_chemical_formula_weight         1310.86
_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                97.447(2)
_cell_angle_beta                 91.495(2)
_cell_angle_gamma                108.292(2)
_cell_formula_units_Z            1
_cell_length_a                   11.0685(7)
_cell_length_b                   11.3771(6)
_cell_length_c                   12.7949(8)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.44
_cell_volume                     1513.09(16)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16375
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    2.980
_exptl_absorpt_correction_T_max  0.5871
_exptl_absorpt_correction_T_min  0.4684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0197
_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)+(0.0170P)²+0.7400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0487
_reflns_number_gt                6397
_reflns_number_total             7179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc45450a.txt
_cod_data_source_block           wein145
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7109741
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 0.704915(15) 0.852975(14) 0.817662(13) 0.01208(4) Uani 1 1 d .
Ge2 Ge 0.571423(14) 0.641957(13) 0.735726(12) 0.00947(4) Uani 1 1 d .
Ge3 Ge 0.519833(14) 0.608901(13) 0.542856(12) 0.00915(4) Uani 1 1 d .
C1 C 0.88373(14) 0.85972(14) 0.85343(13) 0.0162(3) Uani 1 1 d .
H1A H 0.9329 0.9497 0.8780 0.019 Uiso 1 1 calc R
C2 C 0.89895(16) 0.78783(17) 0.94374(14) 0.0237(4) Uani 1 1 d .
H2A H 0.9891 0.7959 0.9562 0.036 Uiso 1 1 calc R
H2B H 0.8489 0.6993 0.9246 0.036 Uiso 1 1 calc R
H2C H 0.8685 0.8224 1.0081 0.036 Uiso 1 1 calc R
C3 C 0.94776(15) 0.81886(15) 0.75687(14) 0.0186(3) Uani 1 1 d .
H3A H 1.0351 0.8237 0.7783 0.028 Uiso 1 1 calc R
H3B H 0.9499 0.8741 0.7038 0.028 Uiso 1 1 calc R
H3C H 0.8993 0.7326 0.7268 0.028 Uiso 1 1 calc R
C4 C 0.63034(16) 0.90227(15) 0.94944(13) 0.0203(3) Uani 1 1 d .
H4A H 0.5509 0.9195 0.9275 0.024 Uiso 1 1 calc R
C5 C 0.71990(18) 1.02425(17) 1.01217(15) 0.0298(4) Uani 1 1 d .
H5A H 0.6808 1.0461 1.0765 0.045 Uiso 1 1 calc R
H5B H 0.7348 1.0916 0.9687 0.045 Uiso 1 1 calc R
H5C H 0.8014 1.0128 1.0313 0.045 Uiso 1 1 calc R
C6 C 0.59121(17) 0.79950(17) 1.01960(14) 0.0255(4) Uani 1 1 d .
H6A H 0.5554 0.8297 1.0829 0.038 Uiso 1 1 calc R
H6B H 0.6662 0.7773 1.0405 0.038 Uiso 1 1 calc R
H6C H 0.5270 0.7256 0.9804 0.038 Uiso 1 1 calc R
C7 C 0.70870(16) 0.97508(14) 0.71811(14) 0.0196(3) Uani 1 1 d .
H7A H 0.6981 0.9284 0.6449 0.024 Uiso 1 1 calc R
C8 C 0.59706(17) 1.02737(16) 0.73070(15) 0.0241(4) Uani 1 1 d .
H8A H 0.6018 1.0868 0.6808 0.036 Uiso 1 1 calc R
H8B H 0.6017 1.0701 0.8030 0.036 Uiso 1 1 calc R
H8C H 0.5163 0.9586 0.7164 0.036 Uiso 1 1 calc R
C9 C 0.83588(17) 1.08132(16) 0.72750(18) 0.0297(4) Uani 1 1 d .
H9A H 0.8328 1.1385 0.6771 0.045 Uiso 1 1 calc R
H9B H 0.9050 1.0464 0.7119 0.045 Uiso 1 1 calc R
H9C H 0.8514 1.1271 0.7995 0.045 Uiso 1 1 calc R
C10 C 0.39932(14) 0.59978(14) 0.78787(12) 0.0125(3) Uani 1 1 d .
C11 C 0.32981(15) 0.47569(14) 0.79717(13) 0.0175(3) Uani 1 1 d .
H11A H 0.3693 0.4126 0.7854 0.021 Uiso 1 1 calc R
C12 C 0.20329(16) 0.44395(16) 0.82348(14) 0.0239(4) Uani 1 1 d .
H12A H 0.1572 0.3594 0.8292 0.029 Uiso 1 1 calc R
C13 C 0.14452(16) 0.53477(17) 0.84135(14) 0.0236(4) Uani 1 1 d .
H13A H 0.0582 0.5128 0.8591 0.028 Uiso 1 1 calc R
C14 C 0.21210(15) 0.65817(16) 0.83328(13) 0.0188(3) Uani 1 1 d .
H14A H 0.1723 0.7210 0.8460 0.023 Uiso 1 1 calc R
C15 C 0.33818(15) 0.68999(14) 0.80662(12) 0.0143(3) Uani 1 1 d .
H15A H 0.3836 0.7747 0.8011 0.017 Uiso 1 1 calc R
C16 C 0.65089(14) 0.52234(13) 0.77728(12) 0.0118(3) Uani 1 1 d .
C17 C 0.73758(14) 0.48582(14) 0.71399(12) 0.0143(3) Uani 1 1 d .
H17A H 0.7517 0.5134 0.6470 0.017 Uiso 1 1 calc R
C18 C 0.80365(16) 0.40974(15) 0.74719(14) 0.0203(3) Uani 1 1 d .
H18A H 0.8616 0.3850 0.7029 0.024 Uiso 1 1 calc R
C19 C 0.78418(16) 0.37039(15) 0.84554(14) 0.0219(4) Uani 1 1 d .
H19A H 0.8303 0.3201 0.8694 0.026 Uiso 1 1 calc R
C20 C 0.69754(16) 0.40440(15) 0.90887(14) 0.0208(3) Uani 1 1 d .
H20A H 0.6835 0.3766 0.9757 0.025 Uiso 1 1 calc R
C21 C 0.63115(15) 0.47912(14) 0.87473(13) 0.0165(3) Uani 1 1 d .
H21A H 0.5713 0.5013 0.9184 0.020 Uiso 1 1 calc R
C22 C 0.64212(14) 0.72189(13) 0.46241(12) 0.0118(3) Uani 1 1 d .
C23 C 0.77344(15) 0.75999(14) 0.48849(13) 0.0172(3) Uani 1 1 d .
H23A H 0.8049 0.7312 0.5466 0.021 Uiso 1 1 calc R
C24 C 0.85874(16) 0.83969(16) 0.43031(15) 0.0235(4) Uani 1 1 d .
H24A H 0.9478 0.8644 0.4485 0.028 Uiso 1 1 calc R
C25 C 0.81396(17) 0.88285(15) 0.34615(15) 0.0234(4) Uani 1 1 d .
H25A H 0.8721 0.9379 0.3070 0.028 Uiso 1 1 calc R
C26 C 0.68413(17) 0.84581(14) 0.31879(13) 0.0188(3) Uani 1 1 d .
H26A H 0.6533 0.8758 0.2612 0.023 Uiso 1 1 calc R
C27 C 0.59883(15) 0.76456(14) 0.37579(12) 0.0145(3) Uani 1 1 d .
H27A H 0.5101 0.7378 0.3555 0.017 Uiso 1 1 calc R
C28 C 0.36518(14) 0.65912(14) 0.54014(12) 0.0132(3) Uani 1 1 d .
C29 C 0.24624(15) 0.57750(16) 0.55909(12) 0.0181(3) Uani 1 1 d .
H29A H 0.2377 0.4933 0.5664 0.022 Uiso 1 1 calc R
C30 C 0.14023(16) 0.61856(19) 0.56727(14) 0.0262(4) Uani 1 1 d .
H30A H 0.0600 0.5623 0.5801 0.031 Uiso 1 1 calc R
C31 C 0.15153(18) 0.7411(2) 0.55677(15) 0.0317(5) Uani 1 1 d .
H31A H 0.0788 0.7684 0.5615 0.038 Uiso 1 1 calc R
C32 C 0.26767(19) 0.82330(18) 0.53953(15) 0.0284(4) Uani 1 1 d .
H32A H 0.2753 0.9075 0.5328 0.034 Uiso 1 1 calc R
C33 C 0.37454(16) 0.78316(15) 0.53185(13) 0.0190(3) Uani 1 1 d .
H33A H 0.4547 0.8408 0.5208 0.023 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'
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_3
C4 Ge1 C7 108.99(7) .
C4 Ge1 C1 108.74(7) .
C7 Ge1 C1 108.48(7) .
C4 Ge1 Ge2 109.19(5) .
C7 Ge1 Ge2 109.49(5) .
C1 Ge1 Ge2 111.91(4) .
C16 Ge2 C10 107.95(6) .
C16 Ge2 Ge1 107.71(4) .
C10 Ge2 Ge1 110.80(4) .
C16 Ge2 Ge3 111.71(4) .
C10 Ge2 Ge3 100.93(4) .
Ge1 Ge2 Ge3 117.330(8) .
C22 Ge3 C28 105.92(6) .
C22 Ge3 Ge2 115.68(4) .
C28 Ge3 Ge2 99.69(4) .
C22 Ge3 Ge3 108.47(4) 2_666
C28 Ge3 Ge3 112.43(4) 2_666
Ge2 Ge3 Ge3 114.153(10) 2_666
C3 C1 C2 109.86(14) .
C3 C1 Ge1 112.47(11) .
C2 C1 Ge1 114.69(11) .
C6 C4 C5 110.79(15) .
C6 C4 Ge1 113.61(12) .
C5 C4 Ge1 111.31(11) .
C9 C7 C8 110.75(13) .
C9 C7 Ge1 112.73(12) .
C8 C7 Ge1 111.64(11) .
C15 C10 C11 117.93(14) .
C15 C10 Ge2 121.04(11) .
C11 C10 Ge2 120.73(12) .
C12 C11 C10 120.70(16) .
C13 C12 C11 120.38(16) .
C12 C13 C14 119.71(15) .
C13 C14 C15 120.01(16) .
C14 C15 C10 121.26(15) .
C21 C16 C17 117.99(14) .
C21 C16 Ge2 121.11(12) .
C17 C16 Ge2 120.69(11) .
C18 C17 C16 121.26(15) .
C19 C18 C17 119.49(16) .
C20 C19 C18 120.08(15) .
C19 C20 C21 120.04(16) .
C20 C21 C16 121.12(15) .
C27 C22 C23 118.27(14) .
C27 C22 Ge3 120.13(11) .
C23 C22 Ge3 121.60(12) .
C24 C23 C22 120.80(15) .
C25 C24 C23 120.09(16) .
C24 C25 C26 119.99(15) .
C25 C26 C27 120.02(15) .
C26 C27 C22 120.80(15) .
C33 C28 C29 117.99(14) .
C33 C28 Ge3 120.09(12) .
C29 C28 Ge3 121.47(11) .
C30 C29 C28 120.68(16) .
C31 C30 C29 120.17(17) .
C32 C31 C30 120.16(16) .
C31 C32 C33 120.05(17) .
C32 C33 C28 120.93(17) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 C4 1.9892(16) .
Ge1 C7 1.9948(16) .
Ge1 C1 1.9952(16) .
Ge1 Ge2 2.4670(2) .
Ge2 C16 1.9552(15) .
Ge2 C10 1.9697(15) .
Ge2 Ge3 2.4715(3) .
Ge3 C22 1.9666(15) .
Ge3 C28 1.9682(15) .
Ge3 Ge3 2.4745(3) 2_666
C1 C3 1.532(2) .
C1 C2 1.534(2) .
C4 C6 1.528(3) .
C4 C5 1.536(2) .
C7 C9 1.531(2) .
C7 C8 1.534(2) .
C10 C15 1.396(2) .
C10 C11 1.402(2) .
C11 C12 1.394(2) .
C12 C13 1.383(3) .
C13 C14 1.387(2) .
C14 C15 1.391(2) .
C16 C21 1.396(2) .
C16 C17 1.397(2) .
C17 C18 1.393(2) .
C18 C19 1.389(2) .
C19 C20 1.385(3) .
C20 C21 1.387(2) .
C22 C27 1.397(2) .
C22 C23 1.398(2) .
C23 C24 1.394(2) .
C24 C25 1.381(3) .
C25 C26 1.386(2) .
C26 C27 1.393(2) .
C28 C33 1.400(2) .
C28 C29 1.401(2) .
C29 C30 1.394(2) .
C30 C31 1.385(3) .
C31 C32 1.375(3) .
C32 C33 1.397(2) .
