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#$Date: 2022-09-15 01:26:15 +0300 (Thu, 15 Sep 2022) $
#$Revision: 277847 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/01/4060112.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_4060112
loop_
_publ_author_name
'Sasamori, Takahiro'
'Sasaki, Takayo'
'Takeda, Nobuhiro'
'Tokitoh, Norihiro'
_publ_section_title
;
 Reactions of a Germacyclopropabenzene with Elemental Chalcogens:
 Syntheses and Structures of a Series of Stable
 2H-Benzo[c][1,2]chalcogenagermetes
;
_journal_coden_ASTM              ORGND7
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              612
_journal_page_last               618
_journal_paper_doi               10.1021/om049216q
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C45 H80 Ge S Si6'
_chemical_formula_sum            'C45 H80 Ge S Si6'
_chemical_formula_weight         894.28
_chemical_name_common            benzothiagermete
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                76.768(11)
_cell_angle_beta                 83.650(12)
_cell_angle_gamma                72.101(9)
_cell_formula_units_Z            2
_cell_length_a                   10.125(3)
_cell_length_b                   11.941(3)
_cell_length_c                   22.971(7)
_cell_measurement_reflns_used    7207
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.2
_cell_volume                     2570.3(13)
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16974
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.9841
_exptl_absorpt_correction_T_min  0.7943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         8857
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0288P)²+3.5828P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                7760
_reflns_number_total             8857
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4060112
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.62297(15) 0.80539(14) 0.16362(8) 0.0138(2) Uani 0.867(3) 1 d PD A 1
S1 S 0.63308(9) 0.99638(8) 0.16617(4) 0.0198(3) Uani 0.867(3) 1 d PD A 1
C1 C 0.4295(4) 0.9011(3) 0.17667(14) 0.0172(8) Uani 0.867(3) 1 d PD A 1
C2 C 0.4530(4) 1.0081(3) 0.17944(14) 0.0211(8) Uani 0.867(3) 1 d PD A 1
C3 C 0.3466(4) 1.1080(4) 0.19072(16) 0.0269(9) Uani 0.867(3) 1 d P A 1
H1 H 0.3646 1.1806 0.1925 0.032 Uiso 0.867(3) 1 calc PR A 1
C4 C 0.2135(4) 1.0966(4) 0.19928(17) 0.0296(9) Uani 0.867(3) 1 d P A 1
H2 H 0.1385 1.1626 0.2076 0.036 Uiso 0.867(3) 1 calc PR A 1
C5 C 0.1875(4) 0.9917(4) 0.19598(16) 0.0288(9) Uani 0.867(3) 1 d P A 1
H3 H 0.0949 0.9868 0.2016 0.035 Uiso 0.867(3) 1 calc PR A 1
C6 C 0.2951(4) 0.8925(4) 0.18455(16) 0.0240(9) Uani 0.867(3) 1 d P A 1
H4 H 0.2766 0.8204 0.1822 0.029 Uiso 0.867(3) 1 calc PR A 1
C7 C 0.6989(3) 0.6641(3) 0.22938(12) 0.0171(6) Uani 1 1 d . . .
C8 C 0.7300(3) 0.6780(3) 0.28552(13) 0.0186(6) Uani 1 1 d . A .
C9 C 0.7870(3) 0.5745(3) 0.32892(13) 0.0210(7) Uani 1 1 d . . .
H5 H 0.8057 0.5843 0.3668 0.025 Uiso 1 1 calc R A .
C10 C 0.8172(3) 0.4588(3) 0.31895(13) 0.0201(7) Uani 1 1 d . A .
C11 C 0.7850(3) 0.4479(3) 0.26384(13) 0.0213(7) Uani 1 1 d . . .
H6 H 0.8068 0.3695 0.2557 0.026 Uiso 1 1 calc R A .
C12 C 0.7218(3) 0.5464(3) 0.21947(13) 0.0189(6) Uani 1 1 d . A .
C13 C 0.7036(3) 0.7978(3) 0.30320(13) 0.0208(7) Uani 1 1 d . . .
H7 H 0.6690 0.8586 0.2662 0.025 Uiso 1 1 calc R A .
C14 C 0.8741(3) 0.3461(3) 0.36579(13) 0.0224(7) Uani 1 1 d . . .
H8 H 0.8800 0.2800 0.3448 0.027 Uiso 1 1 calc R A .
C15 C 0.6736(3) 0.5141(3) 0.16673(13) 0.0200(7) Uani 1 1 d . . .
H9 H 0.6353 0.5921 0.1382 0.024 Uiso 1 1 calc R A .
Si1 Si 0.55492(9) 0.82925(9) 0.36094(4) 0.0266(2) Uani 1 1 d . A .
Si2 Si 0.86790(9) 0.83000(8) 0.31893(4) 0.0240(2) Uani 1 1 d . A .
Si3 Si 0.74661(10) 0.32236(8) 0.43106(4) 0.0275(2) Uani 1 1 d . A .
Si4 Si 1.06170(9) 0.32115(9) 0.38182(4) 0.0277(2) Uani 1 1 d . A .
Si5 Si 0.51903(9) 0.45264(9) 0.19450(4) 0.0284(2) Uani 1 1 d . A .
Si6 Si 0.81797(9) 0.41837(8) 0.12275(4) 0.02015(19) Uani 1 1 d . A .
C16 C 0.3959(4) 0.8086(4) 0.33719(16) 0.0438(10) Uani 1 1 d . . .
H10 H 0.4147 0.7254 0.3328 0.066 Uiso 1 1 calc R A .
H11 H 0.3685 0.8633 0.2988 0.066 Uiso 1 1 calc R . .
H12 H 0.3205 0.8264 0.3674 0.066 Uiso 1 1 calc R . .
C17 C 0.5160(4) 0.9889(3) 0.36857(19) 0.0478(11) Uani 1 1 d . . .
H13 H 0.4965 1.0424 0.3293 0.072 Uiso 1 1 calc R A .
H14 H 0.5963 0.9995 0.3845 0.072 Uiso 1 1 calc R . .
H15 H 0.4349 1.0085 0.3960 0.072 Uiso 1 1 calc R . .
C18 C 0.5905(4) 0.7304(4) 0.43685(14) 0.0376(9) Uani 1 1 d . . .
H16 H 0.6121 0.6461 0.4338 0.056 Uiso 1 1 calc R A .
H17 H 0.5084 0.7507 0.4637 0.056 Uiso 1 1 calc R . .
H18 H 0.6697 0.7426 0.4528 0.056 Uiso 1 1 calc R . .
C19 C 0.8495(4) 0.9938(3) 0.29125(17) 0.0373(9) Uani 1 1 d . . .
H19 H 0.7690 1.0411 0.3118 0.056 Uiso 1 1 calc R A .
H20 H 0.8362 1.0153 0.2481 0.056 Uiso 1 1 calc R . .
H21 H 0.9336 1.0108 0.2994 0.056 Uiso 1 1 calc R . .
C20 C 0.9078(4) 0.7965(4) 0.39990(15) 0.0370(9) Uani 1 1 d . . .
H22 H 0.8287 0.8417 0.4220 0.056 Uiso 1 1 calc R A .
H23 H 0.9905 0.8200 0.4038 0.056 Uiso 1 1 calc R . .
H24 H 0.9250 0.7101 0.4162 0.056 Uiso 1 1 calc R . .
C21 C 1.0208(3) 0.7421(3) 0.27907(16) 0.0352(9) Uani 1 1 d . . .
H25 H 1.0316 0.6560 0.2932 0.053 Uiso 1 1 calc R A .
H26 H 1.1046 0.7599 0.2870 0.053 Uiso 1 1 calc R . .
H27 H 1.0066 0.7643 0.2359 0.053 Uiso 1 1 calc R . .
C22 C 0.5654(4) 0.3969(4) 0.40589(16) 0.0411(10) Uani 1 1 d . . .
H28 H 0.5515 0.3659 0.3718 0.062 Uiso 1 1 calc R A .
H29 H 0.5503 0.4839 0.3939 0.062 Uiso 1 1 calc R . .
H30 H 0.4994 0.3799 0.4388 0.062 Uiso 1 1 calc R . .
C23 C 0.7695(4) 0.3835(4) 0.49571(15) 0.0408(10) Uani 1 1 d . . .
H31 H 0.7573 0.4700 0.4829 0.061 Uiso 1 1 calc R A .
H32 H 0.8630 0.3430 0.5106 0.061 Uiso 1 1 calc R . .
H33 H 0.7003 0.3695 0.5277 0.061 Uiso 1 1 calc R . .
C24 C 0.7718(4) 0.1576(4) 0.45596(19) 0.0508(11) Uani 1 1 d . . .
H34 H 0.7605 0.1247 0.4221 0.076 Uiso 1 1 calc R A .
H35 H 0.7028 0.1434 0.4880 0.076 Uiso 1 1 calc R . .
H36 H 0.8654 0.1182 0.4709 0.076 Uiso 1 1 calc R . .
C25 C 1.0888(4) 0.4356(4) 0.41891(18) 0.0443(10) Uani 1 1 d . . .
H37 H 1.0541 0.5159 0.3937 0.066 Uiso 1 1 calc R A .
H38 H 1.1881 0.4184 0.4245 0.066 Uiso 1 1 calc R . .
H39 H 1.0383 0.4327 0.4579 0.066 Uiso 1 1 calc R . .
C26 C 1.1302(4) 0.1695(3) 0.43120(18) 0.0457(10) Uani 1 1 d . . .
H40 H 1.1176 0.1077 0.4125 0.069 Uiso 1 1 calc R A .
H41 H 1.0795 0.1673 0.4701 0.069 Uiso 1 1 calc R . .
H42 H 1.2292 0.1540 0.4368 0.069 Uiso 1 1 calc R . .
C27 C 1.1630(4) 0.3257(4) 0.30876(17) 0.0475(11) Uani 1 1 d . . .
H43 H 1.1501 0.2657 0.2888 0.071 Uiso 1 1 calc R A .
H44 H 1.2618 0.3077 0.3158 0.071 Uiso 1 1 calc R . .
H45 H 1.1304 0.4059 0.2833 0.071 Uiso 1 1 calc R . .
C28 C 0.4283(4) 0.4440(4) 0.12998(19) 0.0568(13) Uani 1 1 d . . .
H46 H 0.4041 0.5225 0.1025 0.085 Uiso 1 1 calc R A .
H47 H 0.3435 0.4214 0.1447 0.085 Uiso 1 1 calc R . .
H48 H 0.4897 0.3834 0.1089 0.085 Uiso 1 1 calc R . .
C29 C 0.3953(4) 0.5581(4) 0.2381(2) 0.0607(14) Uani 1 1 d . . .
H49 H 0.4419 0.5628 0.2723 0.091 Uiso 1 1 calc R A .
H50 H 0.3148 0.5287 0.2526 0.091 Uiso 1 1 calc R . .
H51 H 0.3643 0.6381 0.2123 0.091 Uiso 1 1 calc R . .
C30 C 0.5620(4) 0.3011(3) 0.24514(17) 0.0385(9) Uani 1 1 d . . .
H52 H 0.6088 0.3030 0.2799 0.058 Uiso 1 1 calc R A .
H53 H 0.6235 0.2417 0.2235 0.058 Uiso 1 1 calc R . .
H54 H 0.4764 0.2792 0.2586 0.058 Uiso 1 1 calc R . .
C31 C 0.7787(4) 0.4612(3) 0.04208(15) 0.0366(9) Uani 1 1 d . . .
H55 H 0.6906 0.4471 0.0371 0.055 Uiso 1 1 calc R A .
H56 H 0.8534 0.4125 0.0195 0.055 Uiso 1 1 calc R . .
H57 H 0.7714 0.5465 0.0272 0.055 Uiso 1 1 calc R . .
C32 C 0.9853(4) 0.4469(4) 0.13007(18) 0.0387(9) Uani 1 1 d . . .
H58 H 1.0080 0.4253 0.1723 0.058 Uiso 1 1 calc R A .
H59 H 0.9768 0.5323 0.1146 0.058 Uiso 1 1 calc R . .
H60 H 1.0591 0.3982 0.1072 0.058 Uiso 1 1 calc R . .
C33 C 0.8414(4) 0.2532(3) 0.14572(16) 0.0312(8) Uani 1 1 d . . .
H61 H 0.8627 0.2260 0.1882 0.047 Uiso 1 1 calc R A .
H62 H 0.9182 0.2104 0.1216 0.047 Uiso 1 1 calc R . .
H63 H 0.7558 0.2364 0.1394 0.047 Uiso 1 1 calc R . .
C34 C 0.6953(3) 0.7889(3) 0.08205(12) 0.0166(6) Uani 1 1 d . . .
C35 C 0.8320(3) 0.7965(3) 0.06767(13) 0.0196(7) Uani 1 1 d . A .
C36 C 0.8859(3) 0.7945(3) 0.00934(14) 0.0241(7) Uani 1 1 d . . .
H64 H 0.9785 0.7976 -0.0004 0.029 Uiso 1 1 calc R A .
C37 C 0.8080(3) 0.7880(3) -0.03424(14) 0.0253(7) Uani 1 1 d . A .
H65 H 0.8465 0.7872 -0.0738 0.030 Uiso 1 1 calc R . .
C38 C 0.6732(3) 0.7827(3) -0.02059(14) 0.0233(7) Uani 1 1 d . . .
H66 H 0.6197 0.7788 -0.0511 0.028 Uiso 1 1 calc R A .
C39 C 0.6150(3) 0.7830(3) 0.03696(13) 0.0174(6) Uani 1 1 d . A .
C40 C 0.9223(3) 0.8178(3) 0.11074(15) 0.0278(8) Uani 1 1 d . . .
H67 H 0.8728 0.8141 0.1510 0.033 Uiso 1 1 calc R A .
C41 C 0.4628(3) 0.7856(3) 0.04809(14) 0.0234(7) Uani 1 1 d . . .
H68 H 0.4480 0.7508 0.0914 0.028 Uiso 1 1 calc R A .
C42 C 0.9401(4) 0.9446(3) 0.08920(17) 0.0386(9) Uani 1 1 d . A .
H69 H 0.9971 0.9587 0.1170 0.058 Uiso 1 1 calc R . .
H70 H 0.8487 1.0047 0.0877 0.058 Uiso 1 1 calc R . .
H71 H 0.9858 0.9511 0.0492 0.058 Uiso 1 1 calc R . .
C43 C 1.0664(4) 0.7255(3) 0.11784(18) 0.0387(9) Uani 1 1 d . A .
H72 H 1.1177 0.7442 0.1462 0.058 Uiso 1 1 calc R . .
H73 H 1.1173 0.7284 0.0789 0.058 Uiso 1 1 calc R . .
H74 H 1.0561 0.6447 0.1329 0.058 Uiso 1 1 calc R . .
C44 C 0.3690(3) 0.9153(3) 0.03463(14) 0.0278(8) Uani 1 1 d . A .
H75 H 0.3954 0.9625 0.0586 0.042 Uiso 1 1 calc R . .
H76 H 0.2720 0.9164 0.0446 0.042 Uiso 1 1 calc R . .
H77 H 0.3794 0.9502 -0.0080 0.042 Uiso 1 1 calc R . .
C45 C 0.4188(4) 0.7137(3) 0.01112(17) 0.0365(9) Uani 1 1 d . A .
H78 H 0.3207 0.7182 0.0205 0.055 Uiso 1 1 calc R . .
H79 H 0.4757 0.6295 0.0205 0.055 Uiso 1 1 calc R . .
H80 H 0.4317 0.7469 -0.0316 0.055 Uiso 1 1 calc R . .
Ge2 Ge 0.5960(10) 0.7836(9) 0.1673(6) 0.0162(16) Uani 0.133(3) 1 d PD A 2
S2 S 0.3611(7) 0.8081(7) 0.1799(3) 0.032(2) Uani 0.133(3) 1 d PD A 2
C46 C 0.5136(15) 0.9530(12) 0.1770(9) 0.028(7) Uiso 0.133(3) 1 d PGD A 2
C47 C 0.3756(17) 0.9528(13) 0.1819(9) 0.030(7) Uiso 0.133(3) 1 d PGD A 2
C48 C 0.2701(14) 1.0580(17) 0.1856(11) 0.040(8) Uiso 0.133(3) 1 d PG A 2
H81 H 0.1758 1.0579 0.1890 0.048 Uiso 0.133(3) 1 calc PR A 2
C49 C 0.3025(19) 1.1635(14) 0.1844(12) 0.074(15) Uiso 0.133(3) 1 d PG A 2
H82 H 0.2304 1.2354 0.1870 0.088 Uiso 0.133(3) 1 calc PR A 2
C50 C 0.441(2) 1.1637(12) 0.1795(11) 0.058(9) Uiso 0.133(3) 1 d PG A 2
H83 H 0.4627 1.2358 0.1787 0.070 Uiso 0.133(3) 1 calc PR A 2
C51 C 0.5461(16) 1.0585(15) 0.1758(9) 0.042(7) Uiso 0.133(3) 1 d PG A 2
H84 H 0.6404 1.0587 0.1725 0.050 Uiso 0.133(3) 1 calc PR A 2
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2021-10-23T20:00:00+03:00
'Updated bibliographic information.'
