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#$Date: 2021-10-23 20:05:01 +0300 (Sat, 23 Oct 2021) $
#$Revision: 270067 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/01/4060114.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_4060114
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 Si6 Te'
_chemical_formula_sum            'C45 H80 Ge Si6 Te'
_chemical_formula_weight         989.82
_chemical_name_common            compound5
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.7513(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8849(14)
_cell_length_b                   18.3366(13)
_cell_length_c                   20.7964(15)
_cell_measurement_reflns_used    14544
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.26
_cell_volume                     5283.5(8)
_diffrn_ambient_temperature      103(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  0.0935
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49865
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.9386
_exptl_absorpt_correction_T_min  0.7395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         9304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0596P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                6392
_reflns_number_total             9304
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4060114
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
Ge1 Ge -0.98969(3) -0.86768(3) -0.66527(2) 0.02049(12) Uani 1 1 d . . .
Te1 Te -0.96588(2) -0.972216(18) -0.579151(15) 0.02898(10) Uani 1 1 d . . .
C1 C -0.9389(3) -0.8154(3) -0.5858(2) 0.0250(11) Uani 1 1 d . . .
C2 C -0.9294(3) -0.8689(3) -0.5375(2) 0.0292(11) Uani 1 1 d . . .
C3 C -0.9019(3) -0.8521(3) -0.4749(2) 0.0350(12) Uani 1 1 d . . .
H1 H -0.8950 -0.8891 -0.4430 0.042 Uiso 1 1 calc R . .
C4 C -0.8843(3) -0.7789(3) -0.4591(2) 0.0374(13) Uani 1 1 d . . .
H2 H -0.8657 -0.7662 -0.4157 0.045 Uiso 1 1 calc R . .
C5 C -0.8934(3) -0.7248(3) -0.5051(2) 0.0331(12) Uani 1 1 d . . .
H3 H -0.8810 -0.6753 -0.4939 0.040 Uiso 1 1 calc R . .
C6 C -0.9213(3) -0.7442(3) -0.5690(2) 0.0298(11) Uani 1 1 d . . .
H4 H -0.9280 -0.7073 -0.6010 0.036 Uiso 1 1 calc R . .
C7 C -0.9136(3) -0.8809(2) -0.7412(2) 0.0214(10) Uani 1 1 d . . .
C8 C -0.9589(3) -0.8983(2) -0.8024(2) 0.0192(9) Uani 1 1 d . . .
C9 C -0.9060(3) -0.8915(2) -0.8575(2) 0.0199(10) Uani 1 1 d . . .
H5 H -0.9380 -0.9004 -0.8985 0.024 Uiso 1 1 calc R . .
C10 C -0.8085(3) -0.8722(2) -0.8547(2) 0.0199(10) Uani 1 1 d . . .
C11 C -0.7631(3) -0.8635(2) -0.7937(2) 0.0211(10) Uani 1 1 d . . .
H6 H -0.6957 -0.8539 -0.7902 0.025 Uiso 1 1 calc R . .
C12 C -0.8117(3) -0.8683(2) -0.7372(2) 0.0186(9) Uani 1 1 d . . .
C13 C -1.0595(3) -0.9324(2) -0.8133(2) 0.0198(10) Uani 1 1 d . . .
H7 H -1.0947 -0.9203 -0.7743 0.024 Uiso 1 1 calc R . .
C14 C -0.7559(3) -0.8651(2) -0.9167(2) 0.0225(10) Uani 1 1 d . . .
H8 H -0.8035 -0.8845 -0.9506 0.027 Uiso 1 1 calc R . .
C15 C -0.7508(3) -0.8636(2) -0.6739(2) 0.0212(10) Uani 1 1 d . . .
H9 H -0.7991 -0.8622 -0.6403 0.025 Uiso 1 1 calc R . .
Si1 Si -1.13895(8) -0.89825(7) -0.88559(6) 0.0233(3) Uani 1 1 d . . .
Si2 Si -1.04551(8) -1.03623(7) -0.81379(6) 0.0216(3) Uani 1 1 d . . .
Si3 Si -0.73935(10) -0.76621(8) -0.94120(7) 0.0322(3) Uani 1 1 d . . .
Si4 Si -0.64857(8) -0.92785(7) -0.92121(6) 0.0235(3) Uani 1 1 d . . .
Si5 Si -0.68176(8) -0.77499(7) -0.66214(6) 0.0225(3) Uani 1 1 d . . .
Si6 Si -0.68045(9) -0.95163(7) -0.65638(6) 0.0253(3) Uani 1 1 d . . .
C16 C -1.1301(3) -0.7987(3) -0.8996(2) 0.0309(11) Uani 1 1 d . . .
H10 H -1.1737 -0.7849 -0.9365 0.046 Uiso 1 1 calc R . .
H11 H -1.0636 -0.7862 -0.9085 0.046 Uiso 1 1 calc R . .
H12 H -1.1482 -0.7724 -0.8611 0.046 Uiso 1 1 calc R . .
C17 C -1.2680(3) -0.9163(3) -0.8698(2) 0.0304(11) Uani 1 1 d . . .
H13 H -1.2849 -0.8888 -0.8317 0.046 Uiso 1 1 calc R . .
H14 H -1.2769 -0.9685 -0.8622 0.046 Uiso 1 1 calc R . .
H15 H -1.3098 -0.9009 -0.9071 0.046 Uiso 1 1 calc R . .
C18 C -1.1126(3) -0.9412(3) -0.9644(2) 0.0293(11) Uani 1 1 d . . .
H16 H -1.1622 -0.9266 -0.9976 0.044 Uiso 1 1 calc R . .
H17 H -1.1128 -0.9944 -0.9599 0.044 Uiso 1 1 calc R . .
H18 H -1.0492 -0.9250 -0.9768 0.044 Uiso 1 1 calc R . .
C19 C -1.0218(3) -1.0707(3) -0.7302(2) 0.0295(11) Uani 1 1 d . . .
H19 H -1.0106 -1.1234 -0.7312 0.044 Uiso 1 1 calc R . .
H20 H -1.0777 -1.0604 -0.7052 0.044 Uiso 1 1 calc R . .
H21 H -0.9647 -1.0463 -0.7101 0.044 Uiso 1 1 calc R . .
C20 C -1.1544(3) -1.0870(3) -0.8482(2) 0.0308(11) Uani 1 1 d . . .
H22 H -1.1406 -1.1394 -0.8481 0.046 Uiso 1 1 calc R . .
H23 H -1.1703 -1.0706 -0.8924 0.046 Uiso 1 1 calc R . .
H24 H -1.2091 -1.0774 -0.8219 0.046 Uiso 1 1 calc R . .
C21 C -0.9420(3) -1.0633(3) -0.8620(2) 0.0306(11) Uani 1 1 d . . .
H25 H -0.8811 -1.0522 -0.8375 0.046 Uiso 1 1 calc R . .
H26 H -0.9453 -1.0361 -0.9027 0.046 Uiso 1 1 calc R . .
H27 H -0.9455 -1.1157 -0.8711 0.046 Uiso 1 1 calc R . .
C22 C -0.8601(4) -0.7212(3) -0.9470(3) 0.0551(17) Uani 1 1 d . . .
H28 H -0.8533 -0.6709 -0.9621 0.083 Uiso 1 1 calc R . .
H29 H -0.8866 -0.7209 -0.9045 0.083 Uiso 1 1 calc R . .
H30 H -0.9036 -0.7480 -0.9775 0.083 Uiso 1 1 calc R . .
C23 C -0.6880(4) -0.7617(3) -1.0217(3) 0.0443(14) Uani 1 1 d . . .
H31 H -0.7263 -0.7925 -1.0522 0.066 Uiso 1 1 calc R . .
H32 H -0.6212 -0.7790 -1.0181 0.066 Uiso 1 1 calc R . .
H33 H -0.6897 -0.7111 -1.0370 0.066 Uiso 1 1 calc R . .
C24 C -0.6582(4) -0.7148(3) -0.8827(3) 0.0468(15) Uani 1 1 d . . .
H34 H -0.5922 -0.7334 -0.8840 0.070 Uiso 1 1 calc R . .
H35 H -0.6802 -0.7210 -0.8392 0.070 Uiso 1 1 calc R . .
H36 H -0.6595 -0.6629 -0.8940 0.070 Uiso 1 1 calc R . .
C25 C -0.6258(4) -0.9446(3) -1.0076(2) 0.0380(13) Uani 1 1 d . . .
H37 H -0.5886 -0.9039 -1.0238 0.057 Uiso 1 1 calc R . .
H38 H -0.6876 -0.9486 -1.0329 0.057 Uiso 1 1 calc R . .
H39 H -0.5894 -0.9900 -1.0111 0.057 Uiso 1 1 calc R . .
C26 C -0.5342(3) -0.8922(3) -0.8797(2) 0.0335(12) Uani 1 1 d . . .
H40 H -0.5449 -0.8818 -0.8345 0.050 Uiso 1 1 calc R . .
H41 H -0.5149 -0.8473 -0.9010 0.050 Uiso 1 1 calc R . .
H42 H -0.4831 -0.9288 -0.8819 0.050 Uiso 1 1 calc R . .
C27 C -0.6771(3) -1.0181(3) -0.8860(2) 0.0344(12) Uani 1 1 d . . .
H43 H -0.6264 -1.0531 -0.8949 0.052 Uiso 1 1 calc R . .
H44 H -0.7392 -1.0356 -0.9053 0.052 Uiso 1 1 calc R . .
H45 H -0.6809 -1.0132 -0.8393 0.052 Uiso 1 1 calc R . .
C28 C -0.7581(3) -0.6987(2) -0.6969(2) 0.0286(11) Uani 1 1 d . . .
H46 H -0.7206 -0.6534 -0.6952 0.043 Uiso 1 1 calc R . .
H47 H -0.8150 -0.6929 -0.6718 0.043 Uiso 1 1 calc R . .
H48 H -0.7787 -0.7100 -0.7417 0.043 Uiso 1 1 calc R . .
C29 C -0.5639(3) -0.7712(3) -0.7010(2) 0.0330(12) Uani 1 1 d . . .
H49 H -0.5743 -0.7835 -0.7468 0.049 Uiso 1 1 calc R . .
H50 H -0.5188 -0.8062 -0.6799 0.049 Uiso 1 1 calc R . .
H51 H -0.5370 -0.7219 -0.6966 0.049 Uiso 1 1 calc R . .
C30 C -0.6535(3) -0.7614(3) -0.5738(2) 0.0345(12) Uani 1 1 d . . .
H52 H -0.6331 -0.7108 -0.5657 0.052 Uiso 1 1 calc R . .
H53 H -0.6015 -0.7945 -0.5587 0.052 Uiso 1 1 calc R . .
H54 H -0.7112 -0.7716 -0.5505 0.052 Uiso 1 1 calc R . .
C31 C -0.7491(3) -1.0316(3) -0.6894(2) 0.0317(11) Uani 1 1 d . . .
H55 H -0.7680 -1.0233 -0.7350 0.048 Uiso 1 1 calc R . .
H56 H -0.8069 -1.0385 -0.6655 0.048 Uiso 1 1 calc R . .
H57 H -0.7084 -1.0753 -0.6850 0.048 Uiso 1 1 calc R . .
C32 C -0.5602(3) -0.9560(3) -0.6917(3) 0.0429(14) Uani 1 1 d . . .
H58 H -0.5347 -1.0057 -0.6877 0.064 Uiso 1 1 calc R . .
H59 H -0.5155 -0.9222 -0.6686 0.064 Uiso 1 1 calc R . .
H60 H -0.5673 -0.9423 -0.7373 0.064 Uiso 1 1 calc R . .
C33 C -0.6603(4) -0.9619(3) -0.5674(3) 0.0476(15) Uani 1 1 d . . .
H61 H -0.7219 -0.9566 -0.5474 0.071 Uiso 1 1 calc R . .
H62 H -0.6153 -0.9243 -0.5506 0.071 Uiso 1 1 calc R . .
H63 H -0.6332 -1.0103 -0.5574 0.071 Uiso 1 1 calc R . .
C34 C -1.1209(3) -0.8288(2) -0.6908(2) 0.0228(10) Uani 1 1 d . . .
C35 C -1.2085(3) -0.8676(3) -0.6862(2) 0.0266(11) Uani 1 1 d . . .
C36 C -1.2950(3) -0.8341(3) -0.7066(2) 0.0327(12) Uani 1 1 d . . .
H64 H -1.3540 -0.8591 -0.7016 0.039 Uiso 1 1 calc R . .
C37 C -1.2974(3) -0.7659(3) -0.7339(2) 0.0337(12) Uani 1 1 d . . .
H65 H -1.3572 -0.7449 -0.7491 0.040 Uiso 1 1 calc R . .
C38 C -1.2122(3) -0.7278(3) -0.7391(2) 0.0301(11) Uani 1 1 d . . .
H66 H -1.2139 -0.6808 -0.7585 0.036 Uiso 1 1 calc R . .
C39 C -1.1242(3) -0.7572(2) -0.7165(2) 0.0235(10) Uani 1 1 d . . .
C40 C -1.2127(3) -0.9437(3) -0.6569(2) 0.0292(11) Uani 1 1 d . . .
H67 H -1.1458 -0.9642 -0.6555 0.035 Uiso 1 1 calc R . .
C41 C -1.0358(3) -0.7085(3) -0.7188(2) 0.0258(11) Uani 1 1 d . . .
H68 H -0.9809 -0.7340 -0.6947 0.031 Uiso 1 1 calc R . .
C42 C -1.2428(4) -0.9414(3) -0.5878(3) 0.0425(14) Uani 1 1 d . . .
H69 H -1.1975 -0.9109 -0.5616 0.064 Uiso 1 1 calc R . .
H70 H -1.2425 -0.9909 -0.5701 0.064 Uiso 1 1 calc R . .
H71 H -1.3079 -0.9208 -0.5872 0.064 Uiso 1 1 calc R . .
C43 C -1.2784(3) -0.9960(3) -0.6975(3) 0.0367(13) Uani 1 1 d . . .
H72 H -1.3459 -0.9812 -0.6951 0.055 Uiso 1 1 calc R . .
H73 H -1.2700 -1.0458 -0.6809 0.055 Uiso 1 1 calc R . .
H74 H -1.2613 -0.9945 -0.7425 0.055 Uiso 1 1 calc R . .
C44 C -1.0518(3) -0.6351(3) -0.6841(3) 0.0347(12) Uani 1 1 d . . .
H75 H -1.0987 -0.6056 -0.7099 0.052 Uiso 1 1 calc R . .
H76 H -0.9904 -0.6087 -0.6785 0.052 Uiso 1 1 calc R . .
H77 H -1.0763 -0.6446 -0.6417 0.052 Uiso 1 1 calc R . .
C45 C -1.0049(3) -0.6928(3) -0.7864(2) 0.0341(12) Uani 1 1 d . . .
H78 H -0.9890 -0.7388 -0.8074 0.051 Uiso 1 1 calc R . .
H79 H -0.9481 -0.6610 -0.7837 0.051 Uiso 1 1 calc R . .
H80 H -1.0578 -0.6687 -0.8117 0.051 Uiso 1 1 calc R . .
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.'
