#------------------------------------------------------------------------------
#$Date: 2016-10-05 12:30:16 +0300 (Wed, 05 Oct 2016) $
#$Revision: 186949 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/67/4086740.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_4086740
loop_
_publ_author_name
'Komanduri, Sangeetha P.'
'Shumaker, F. Alexander'
'Roewe, Kimberly D.'
'Wolf, Melanie'
'Uhlig, Frank'
'Moore, Curtis E.'
'Rheingold, Arnold L.'
'Weinert, Charles S.'
_publ_section_title
;
 A Series of Isopropyl-Substituted Oligogermanes Pri3Ge(GePh2)nGePri3(n=
 0--3) Featuring a Luminescent and Dichroic Pentagermane
 Pri3Ge(GePh2)3GePri3
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3240
_journal_paper_doi               10.1021/acs.organomet.6b00596
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C42 H62 Ge4'
_chemical_formula_sum            'C42 H62 Ge4'
_chemical_formula_weight         857.27
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2013-06-24
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                106.109(5)
_cell_angle_beta                 99.150(5)
_cell_angle_gamma                108.601(6)
_cell_formula_units_Z            1
_cell_length_a                   9.4578(17)
_cell_length_b                   10.709(2)
_cell_length_c                   11.485(2)
_cell_measurement_reflns_used    2426
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.605
_cell_measurement_theta_min      2.321
_cell_volume                     1019.3(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'Bruker APEX2 v2013-2.0 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL-2012, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'Bruker APEX2 v2013-2.0 (Bruker, 2013)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0899
_diffrn_reflns_av_unetI/netI     0.1161
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15147
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.419
_diffrn_reflns_theta_min         1.918
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.947
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0871 before and 0.0579 after correction.
The Ratio of minimum to maximum transmission is 0.8547.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    Colorless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       Needle
_exptl_crystal_F_000             442
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0383P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2579
_reflns_number_total             4185
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00596_si_002.cif
_cod_data_source_block           Compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               4086740
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.792
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-3
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ge1 Ge 0.55543(6) 0.77516(5) 0.73361(4) 0.02169(17) Uani 1 1 d . .
Ge2 Ge 0.61243(6) 0.59646(5) 0.58222(4) 0.01993(16) Uani 1 1 d . .
C1 C 0.5171(6) 0.7188(5) 0.8799(4) 0.0294(13) Uani 1 1 d . .
H1 H 0.4811 0.7888 0.9306 0.035 Uiso 1 1 calc R U
C2 C 0.3656(6) 0.7963(5) 0.6528(4) 0.0263(12) Uani 1 1 d . .
H2 H 0.2938 0.7013 0.5917 0.032 Uiso 1 1 calc R U
C3 C 0.7316(6) 0.9611(5) 0.7930(4) 0.0273(13) Uani 1 1 d . .
H3 H 0.7219 1.0029 0.7258 0.033 Uiso 1 1 calc R U
C4 C 0.7198(5) 0.5182(5) 0.6853(4) 0.0213(12) Uani 1 1 d . .
C5 C 0.7650(5) 0.6842(5) 0.5006(4) 0.0195(11) Uani 1 1 d . .
C6 C 0.3844(6) 0.5766(6) 0.8400(5) 0.0367(15) Uani 1 1 d . .
H6A H 0.2937 0.5764 0.7850 0.055 Uiso 1 1 calc R U
H6B H 0.3582 0.5594 0.9148 0.055 Uiso 1 1 calc R U
H6C H 0.4158 0.5026 0.7945 0.055 Uiso 1 1 calc R U
C7 C 0.6582(6) 0.7240(6) 0.9700(4) 0.0384(15) Uani 1 1 d . .
H7A H 0.6971 0.6552 0.9258 0.058 Uiso 1 1 calc R U
H7B H 0.6284 0.7016 1.0419 0.058 Uiso 1 1 calc R U
H7C H 0.7395 0.8185 0.9999 0.058 Uiso 1 1 calc R U
C8 C 0.2781(6) 0.8459(6) 0.7448(5) 0.0395(15) Uani 1 1 d . .
H8A H 0.2559 0.7839 0.7940 0.059 Uiso 1 1 calc R U
H8B H 0.1805 0.8433 0.6978 0.059 Uiso 1 1 calc R U
H8C H 0.3417 0.9424 0.8018 0.059 Uiso 1 1 calc R U
C9 C 0.4029(6) 0.8947(5) 0.5772(5) 0.0313(13) Uani 1 1 d . .
H9A H 0.4705 0.9899 0.6347 0.047 Uiso 1 1 calc R U
H9B H 0.3064 0.8963 0.5328 0.047 Uiso 1 1 calc R U
H9C H 0.4555 0.8606 0.5160 0.047 Uiso 1 1 calc R U
C10 C 0.7183(7) 1.0605(5) 0.9117(5) 0.0415(16) Uani 1 1 d . .
H10A H 0.6172 1.0684 0.8946 0.062 Uiso 1 1 calc R U
H10B H 0.8009 1.1536 0.9364 0.062 Uiso 1 1 calc R U
H10C H 0.7281 1.0231 0.9801 0.062 Uiso 1 1 calc R U
C11 C 0.8923(6) 0.9539(5) 0.8158(4) 0.0331(14) Uani 1 1 d . .
H11A H 0.9036 0.9083 0.8779 0.050 Uiso 1 1 calc R U
H11B H 0.9720 1.0493 0.8474 0.050 Uiso 1 1 calc R U
H11C H 0.9040 0.8993 0.7365 0.050 Uiso 1 1 calc R U
C12 C 0.6425(6) 0.3956(5) 0.7042(4) 0.0287(13) Uani 1 1 d . .
H12 H 0.5358 0.3442 0.6609 0.034 Uiso 1 1 calc R U
C13 C 0.7147(7) 0.3444(6) 0.7845(5) 0.0375(15) Uani 1 1 d . .
H13 H 0.6577 0.2601 0.7961 0.045 Uiso 1 1 calc R U
C14 C 0.8702(7) 0.4174(6) 0.8471(4) 0.0352(15) Uani 1 1 d . .
H14 H 0.9216 0.3830 0.9011 0.042 Uiso 1 1 calc R U
C15 C 0.9494(6) 0.5402(6) 0.8303(4) 0.0305(13) Uani 1 1 d . .
H15 H 1.0557 0.5925 0.8746 0.037 Uiso 1 1 calc R U
C16 C 0.8754(6) 0.5881(5) 0.7494(4) 0.0245(12) Uani 1 1 d . .
H16 H 0.9331 0.6718 0.7373 0.029 Uiso 1 1 calc R U
C17 C 0.8757(5) 0.6296(5) 0.4731(4) 0.0228(12) Uani 1 1 d . .
H17 H 0.8799 0.5522 0.4967 0.027 Uiso 1 1 calc R U
C18 C 0.9800(6) 0.6866(6) 0.4118(4) 0.0279(13) Uani 1 1 d . .
H18 H 1.0578 0.6509 0.3967 0.033 Uiso 1 1 calc R U
C19 C 0.9712(6) 0.7942(6) 0.3729(5) 0.0331(14) Uani 1 1 d . .
H19 H 1.0408 0.8305 0.3282 0.040 Uiso 1 1 calc R U
C20 C 0.8622(6) 0.8504(6) 0.3980(5) 0.0322(13) Uani 1 1 d . .
H20 H 0.8565 0.9253 0.3711 0.039 Uiso 1 1 calc R U
C21 C 0.7606(6) 0.7959(5) 0.4634(4) 0.0247(12) Uani 1 1 d . .
H21 H 0.6871 0.8360 0.4828 0.030 Uiso 1 1 calc R U
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
C1 Ge1 Ge2 110.61(15) .
C1 Ge1 C2 107.6(2) .
C1 Ge1 C3 109.6(2) .
C2 Ge1 Ge2 110.49(13) .
C3 Ge1 Ge2 110.22(15) .
C3 Ge1 C2 108.2(2) .
Ge1 Ge2 Ge2 116.51(3) 2_666
C4 Ge2 Ge1 105.10(13) .
C4 Ge2 Ge2 109.50(14) 2_666
C4 Ge2 C5 104.9(2) .
C5 Ge2 Ge1 111.22(14) .
C5 Ge2 Ge2 108.89(12) 2_666
Ge1 C1 H1 105.8 .
C6 C1 Ge1 111.9(3) .
C6 C1 H1 105.8 .
C6 C1 C7 110.6(5) .
C7 C1 Ge1 116.1(4) .
C7 C1 H1 105.8 .
Ge1 C2 H2 107.2 .
C8 C2 Ge1 114.0(3) .
C8 C2 H2 107.2 .
C8 C2 C9 109.6(4) .
C9 C2 Ge1 111.4(3) .
C9 C2 H2 107.2 .
Ge1 C3 H3 107.2 .
C10 C3 Ge1 110.2(4) .
C10 C3 H3 107.2 .
C10 C3 C11 110.2(4) .
C11 C3 Ge1 114.5(4) .
C11 C3 H3 107.2 .
C12 C4 Ge2 121.9(4) .
C12 C4 C16 116.5(5) .
C16 C4 Ge2 121.5(4) .
C17 C5 Ge2 120.0(4) .
C21 C5 Ge2 121.7(4) .
C21 C5 C17 118.2(5) .
C1 C6 H6A 109.5 .
C1 C6 H6B 109.5 .
C1 C6 H6C 109.5 .
H6A C6 H6B 109.5 .
H6A C6 H6C 109.5 .
H6B C6 H6C 109.5 .
C1 C7 H7A 109.5 .
C1 C7 H7B 109.5 .
C1 C7 H7C 109.5 .
H7A C7 H7B 109.5 .
H7A C7 H7C 109.5 .
H7B C7 H7C 109.5 .
C2 C8 H8A 109.5 .
C2 C8 H8B 109.5 .
C2 C8 H8C 109.5 .
H8A C8 H8B 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
C2 C9 H9A 109.5 .
C2 C9 H9B 109.5 .
C2 C9 H9C 109.5 .
H9A C9 H9B 109.5 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
C3 C10 H10A 109.5 .
C3 C10 H10B 109.5 .
C3 C10 H10C 109.5 .
H10A C10 H10B 109.5 .
H10A C10 H10C 109.5 .
H10B C10 H10C 109.5 .
C3 C11 H11A 109.5 .
C3 C11 H11B 109.5 .
C3 C11 H11C 109.5 .
H11A C11 H11B 109.5 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
C4 C12 H12 118.8 .
C4 C12 C13 122.5(5) .
C13 C12 H12 118.8 .
C12 C13 H13 120.3 .
C14 C13 C12 119.3(5) .
C14 C13 H13 120.3 .
C13 C14 H14 120.4 .
C15 C14 C13 119.2(5) .
C15 C14 H14 120.4 .
C14 C15 H15 119.9 .
C14 C15 C16 120.3(5) .
C16 C15 H15 119.9 .
C4 C16 H16 118.9 .
C15 C16 C4 122.2(5) .
C15 C16 H16 118.9 .
C5 C17 H17 119.6 .
C18 C17 C5 120.7(5) .
C18 C17 H17 119.6 .
C17 C18 H18 119.9 .
C19 C18 C17 120.2(5) .
C19 C18 H18 119.9 .
C18 C19 H19 119.7 .
C18 C19 C20 120.5(5) .
C20 C19 H19 119.7 .
C19 C20 H20 120.4 .
C19 C20 C21 119.2(5) .
C21 C20 H20 120.4 .
C5 C21 C20 121.1(5) .
C5 C21 H21 119.5 .
C20 C21 H21 119.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 Ge2 2.4669(7) .
Ge1 C1 1.985(5) .
Ge1 C2 1.995(5) .
Ge1 C3 1.993(5) .
Ge2 Ge2 2.4723(10) 2_666
Ge2 C4 1.962(5) .
Ge2 C5 1.974(5) .
C1 H1 1.0000 .
C1 C6 1.521(7) .
C1 C7 1.528(7) .
C2 H2 1.0000 .
C2 C8 1.527(6) .
C2 C9 1.535(7) .
C3 H3 1.0000 .
C3 C10 1.530(7) .
C3 C11 1.531(7) .
C4 C12 1.379(7) .
C4 C16 1.383(7) .
C5 C17 1.391(6) .
C5 C21 1.388(7) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12 0.9500 .
C12 C13 1.391(7) .
C13 H13 0.9500 .
C13 C14 1.382(7) .
C14 H14 0.9500 .
C14 C15 1.374(7) .
C15 H15 0.9500 .
C15 C16 1.379(7) .
C16 H16 0.9500 .
C17 H17 0.9500 .
C17 C18 1.384(7) .
C18 H18 0.9500 .
C18 C19 1.367(7) .
C19 H19 0.9500 .
C19 C20 1.379(7) .
C20 H20 0.9500 .
C20 C21 1.394(7) .
C21 H21 0.9500 .
