#------------------------------------------------------------------------------
#$Date: 2017-01-07 17:18:33 +0200 (Sat, 07 Jan 2017) $
#$Revision: 190012 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/25/7012522.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_7012522
loop_
_publ_author_name
'Ding, Yuqiang'
'Ma, Qingjun'
'Roesky, Herbert W.'
'Usón, Isabel'
'Noltemeyer, Mathias'
'Schmidt, Hans-Georg'
_publ_section_title
;
 Syntheses, structures and properties of [{HC(CMeNAr)2}Ge(E)X] (Ar =
 2,6-iPr2C6H3; E = S, Se; X = F, Cl)
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1094
_journal_paper_doi               10.1039/b211617k
_journal_year                    2003
_chemical_formula_sum            'C36 H49 F Ge N2 S'
_chemical_formula_weight         633.42
_chemical_name_systematic        ?
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.783(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.467(2)
_cell_length_b                   16.804(3)
_cell_length_c                   15.668(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     3541.5(11)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE AED2'
_diffrn_measurement_method       'profile fit'
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9893
_diffrn_reflns_theta_full        25.13
_diffrn_reflns_theta_max         25.13
_diffrn_reflns_theta_min         3.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '90 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  0.7015
_exptl_absorpt_correction_T_min  0.4488
_exptl_absorpt_correction_type   'azimuthal scans'
_exptl_crystal_colour            none
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0469
_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)+(0.0800P)²+2.2444P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                5424
_reflns_number_total             6266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211617k.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C36 H49 F Ge N2 S incl. toluene'
_cod_database_code               7012522
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C36 H49 F Ge N2 S cl e en in lu to' to 'C36 H49 F Ge N2 S'.

 Antanas Vaitkus,
 2017-01-07
;
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 0.75960(2) 0.948809(16) 0.815971(18) 0.03453(12) Uani 1 1 d . . .
S1 S 0.70759(8) 1.06330(5) 0.82064(6) 0.0582(3) Uani 1 1 d . . .
F1 F 0.85510(15) 0.92010(13) 0.89896(14) 0.0654(6) Uani 1 1 d . . .
N1 N 0.67134(15) 0.86216(13) 0.82630(14) 0.0326(5) Uani 1 1 d . . .
C1 C 0.6915(2) 0.79086(16) 0.79317(18) 0.0377(6) Uani 1 1 d . . .
N2 N 0.82221(16) 0.91329(13) 0.71798(14) 0.0328(5) Uani 1 1 d . . .
C2 C 0.7690(2) 0.77810(17) 0.73849(19) 0.0423(7) Uani 1 1 d . . .
H2A H 0.7845 0.7242 0.7268 0.051 Uiso 1 1 calc R . .
C3 C 0.8257(2) 0.83490(17) 0.69951(18) 0.0387(6) Uani 1 1 d . . .
C4 C 0.6267(3) 0.72111(18) 0.8131(2) 0.0537(8) Uani 1 1 d . . .
H4A H 0.6310 0.7110 0.8748 0.081 Uiso 1 1 calc R . .
H4B H 0.6493 0.6739 0.7828 0.081 Uiso 1 1 calc R . .
H4C H 0.5577 0.7329 0.7948 0.081 Uiso 1 1 calc R . .
C5 C 0.8925(2) 0.80734(19) 0.6310(2) 0.0526(8) Uani 1 1 d . . .
H5A H 0.9617 0.8202 0.6479 0.079 Uiso 1 1 calc R . .
H5B H 0.8737 0.8343 0.5772 0.079 Uiso 1 1 calc R . .
H5C H 0.8856 0.7497 0.6235 0.079 Uiso 1 1 calc R . .
C11 C 0.58380(19) 0.87473(15) 0.87557(17) 0.0349(6) Uani 1 1 d . . .
C12 C 0.5913(2) 0.86511(17) 0.96450(18) 0.0388(6) Uani 1 1 d . . .
C13 C 0.5073(2) 0.8829(2) 1.0099(2) 0.0482(7) Uani 1 1 d . . .
H13A H 0.5105 0.8780 1.0704 0.058 Uiso 1 1 calc R . .
C14 C 0.4203(2) 0.9073(2) 0.9690(2) 0.0544(8) Uani 1 1 d . . .
H14A H 0.3643 0.9197 1.0011 0.065 Uiso 1 1 calc R . .
C15 C 0.4141(2) 0.9138(2) 0.8812(2) 0.0540(8) Uani 1 1 d . . .
H15A H 0.3528 0.9293 0.8534 0.065 Uiso 1 1 calc R . .
C16 C 0.4957(2) 0.89827(19) 0.83249(19) 0.0445(7) Uani 1 1 d . . .
C21 C 0.8719(2) 0.97056(16) 0.66539(17) 0.0359(6) Uani 1 1 d . . .
C22 C 0.8172(2) 1.00567(17) 0.59702(18) 0.0414(6) Uani 1 1 d . . .
C23 C 0.8680(3) 1.05697(18) 0.5446(2) 0.0505(8) Uani 1 1 d . . .
H23A H 0.8335 1.0801 0.4964 0.061 Uiso 1 1 calc R . .
C24 C 0.9659(3) 1.07496(19) 0.5607(2) 0.0544(9) Uani 1 1 d . . .
H24A H 0.9986 1.1100 0.5237 0.065 Uiso 1 1 calc R . .
C25 C 1.0176(3) 1.04245(19) 0.6303(2) 0.0532(8) Uani 1 1 d . . .
H25A H 1.0851 1.0569 0.6420 0.064 Uiso 1 1 calc R . .
C26 C 0.9720(2) 0.98843(18) 0.6838(2) 0.0432(7) Uani 1 1 d . . .
C31 C 0.0918(6) 0.7846(4) 0.9488(4) 0.118(2) Uani 1 1 d . . .
C32 C 0.0321(6) 0.7481(4) 0.8878(5) 0.130(3) Uani 1 1 d . . .
H32A H -0.0382 0.7503 0.8898 0.155 Uiso 1 1 calc R . .
C33 C 0.0759(10) 0.7085(5) 0.8242(6) 0.162(4) Uani 1 1 d . . .
H33A H 0.0346 0.6820 0.7823 0.194 Uiso 1 1 calc R . .
C34 C 0.1861(13) 0.7045(5) 0.8169(6) 0.186(6) Uani 1 1 d . . .
H34A H 0.2187 0.6775 0.7729 0.223 Uiso 1 1 calc R . .
C35 C 0.2304(8) 0.7432(5) 0.8792(6) 0.150(3) Uani 1 1 d . . .
H35A H 0.3009 0.7440 0.8782 0.180 Uiso 1 1 calc R . .
C36 C 0.1930(5) 0.7825(3) 0.9450(4) 0.0979(16) Uani 1 1 d . . .
H36A H 0.2351 0.8078 0.9872 0.117 Uiso 1 1 calc R . .
C37 C 0.0472(8) 0.8243(6) 1.0183(5) 0.188(4) Uani 1 1 d . . .
H37A H 0.0708 0.8794 1.0216 0.283 Uiso 1 1 calc R . .
H37B H 0.0656 0.7968 1.0719 0.283 Uiso 1 1 calc R . .
H37C H -0.0253 0.8239 1.0089 0.283 Uiso 1 1 calc R . .
C121 C 0.6846(2) 0.83579(19) 1.01223(19) 0.0461(7) Uani 1 1 d . . .
H12A H 0.7341 0.8219 0.9690 0.055 Uiso 1 1 calc R . .
C122 C 0.7311(3) 0.8997(2) 1.0712(3) 0.0683(10) Uani 1 1 d . . .
H12B H 0.7442 0.9476 1.0378 0.102 Uiso 1 1 calc R . .
H12C H 0.7936 0.8797 1.0976 0.102 Uiso 1 1 calc R . .
H12D H 0.6852 0.9127 1.1158 0.102 Uiso 1 1 calc R . .
C123 C 0.6638(3) 0.7602(2) 1.0637(2) 0.0622(9) Uani 1 1 d . . .
H12E H 0.6313 0.7205 1.0260 0.093 Uiso 1 1 calc R . .
H12F H 0.6202 0.7733 1.1100 0.093 Uiso 1 1 calc R . .
H12G H 0.7266 0.7386 1.0880 0.093 Uiso 1 1 calc R . .
C161 C 0.4853(2) 0.9071(3) 0.7361(2) 0.0617(10) Uani 1 1 d . . .
H16A H 0.5524 0.8987 0.7130 0.074 Uiso 1 1 calc R . .
C162 C 0.4150(4) 0.8444(3) 0.6958(3) 0.0854(13) Uani 1 1 d . . .
H16B H 0.4359 0.7913 0.7155 0.128 Uiso 1 1 calc R . .
H16C H 0.4170 0.8470 0.6335 0.128 Uiso 1 1 calc R . .
H16D H 0.3471 0.8546 0.7128 0.128 Uiso 1 1 calc R . .
C163 C 0.4501(4) 0.9903(3) 0.7100(3) 0.0890(15) Uani 1 1 d . . .
H16E H 0.4948 1.0300 0.7369 0.134 Uiso 1 1 calc R . .
H16F H 0.3825 0.9988 0.7287 0.134 Uiso 1 1 calc R . .
H16G H 0.4505 0.9956 0.6477 0.134 Uiso 1 1 calc R . .
C221 C 0.7081(3) 0.9904(2) 0.5793(2) 0.0562(8) Uani 1 1 d . . .
H22A H 0.6825 0.9645 0.6313 0.067 Uiso 1 1 calc R . .
C222 C 0.6487(3) 1.0663(3) 0.5639(3) 0.0762(12) Uani 1 1 d . . .
H22B H 0.6587 1.1017 0.6133 0.114 Uiso 1 1 calc R . .
H22C H 0.5780 1.0533 0.5558 0.114 Uiso 1 1 calc R . .
H22D H 0.6712 1.0930 0.5127 0.114 Uiso 1 1 calc R . .
C223 C 0.6900(5) 0.9329(3) 0.5054(4) 0.123(2) Uani 1 1 d . . .
H22E H 0.7207 0.8815 0.5199 0.184 Uiso 1 1 calc R . .
H22F H 0.7193 0.9544 0.4542 0.184 Uiso 1 1 calc R . .
H22G H 0.6183 0.9257 0.4943 0.184 Uiso 1 1 calc R . .
C261 C 1.0308(2) 0.9546(2) 0.7598(3) 0.0591(9) Uani 1 1 d . . .
H26A H 0.9915 0.9095 0.7825 0.071 Uiso 1 1 calc R . .
C262 C 1.1318(3) 0.9216(3) 0.7366(4) 0.0937(16) Uani 1 1 d . . .
H26B H 1.1227 0.8845 0.6886 0.141 Uiso 1 1 calc R . .
H26C H 1.1625 0.8935 0.7860 0.141 Uiso 1 1 calc R . .
H26D H 1.1749 0.9655 0.7204 0.141 Uiso 1 1 calc R . .
C263 C 1.0414(4) 1.0176(4) 0.8300(3) 0.0989(17) Uani 1 1 d . . .
H26E H 0.9754 1.0371 0.8436 0.148 Uiso 1 1 calc R . .
H26F H 1.0814 1.0620 0.8103 0.148 Uiso 1 1 calc R . .
H26G H 1.0741 0.9941 0.8813 0.148 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 Ge1 N2 99.61(9) . . ?
F1 Ge1 N1 99.07(9) . . ?
N2 Ge1 N1 97.69(10) . . ?
F1 Ge1 S1 116.57(8) . . ?
N2 Ge1 S1 119.58(7) . . ?
N1 Ge1 S1 120.14(7) . . ?
C1 N1 C11 121.3(2) . . ?
C1 N1 Ge1 121.04(18) . . ?
C11 N1 Ge1 117.53(17) . . ?
N1 C1 C2 123.1(2) . . ?
N1 C1 C4 119.1(2) . . ?
C2 C1 C4 117.8(3) . . ?
C3 N2 C21 120.2(2) . . ?
C3 N2 Ge1 120.36(18) . . ?
C21 N2 Ge1 119.31(17) . . ?
C3 C2 C1 127.5(3) . . ?
N2 C3 C2 123.6(3) . . ?
N2 C3 C5 118.7(3) . . ?
C2 C3 C5 117.6(3) . . ?
C16 C11 C12 122.2(3) . . ?
C16 C11 N1 118.5(2) . . ?
C12 C11 N1 119.3(2) . . ?
C13 C12 C11 117.4(3) . . ?
C13 C12 C121 119.4(3) . . ?
C11 C12 C121 123.2(3) . . ?
C14 C13 C12 121.4(3) . . ?
C13 C14 C15 120.0(3) . . ?
C14 C15 C16 121.4(3) . . ?
C15 C16 C11 117.6(3) . . ?
C15 C16 C161 119.3(3) . . ?
C11 C16 C161 123.0(3) . . ?
C26 C21 C22 122.3(3) . . ?
C26 C21 N2 119.5(3) . . ?
C22 C21 N2 118.3(2) . . ?
C23 C22 C21 117.2(3) . . ?
C23 C22 C221 120.0(3) . . ?
C21 C22 C221 122.8(3) . . ?
C24 C23 C22 121.8(3) . . ?
C23 C24 C25 120.3(3) . . ?
C24 C25 C26 120.8(3) . . ?
C21 C26 C25 117.6(3) . . ?
C21 C26 C261 123.1(3) . . ?
C25 C26 C261 119.3(3) . . ?
C32 C31 C36 120.8(8) . . ?
C32 C31 C37 119.2(9) . . ?
C36 C31 C37 120.0(7) . . ?
C33 C32 C31 118.2(9) . . ?
C32 C33 C34 123.2(9) . . ?
C35 C34 C33 110.0(10) . . ?
C34 C35 C36 130.5(12) . . ?
C35 C36 C31 117.2(7) . . ?
C12 C121 C122 112.0(3) . . ?
C12 C121 C123 111.1(3) . . ?
C122 C121 C123 110.0(3) . . ?
C16 C161 C163 111.6(4) . . ?
C16 C161 C162 111.6(3) . . ?
C163 C161 C162 110.0(3) . . ?
C22 C221 C222 112.8(3) . . ?
C22 C221 C223 111.6(4) . . ?
C222 C221 C223 110.5(4) . . ?
C26 C261 C262 112.9(3) . . ?
C26 C261 C263 109.5(4) . . ?
C262 C261 C263 111.7(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 F1 1.848(2) . ?
Ge1 N2 1.884(2) . ?
Ge1 N1 1.892(2) . ?
Ge1 S1 2.0499(9) . ?
N1 C1 1.339(4) . ?
N1 C11 1.456(3) . ?
C1 C2 1.399(4) . ?
C1 C4 1.503(4) . ?
N2 C3 1.350(4) . ?
N2 C21 1.452(3) . ?
C2 C3 1.383(4) . ?
C3 C5 1.506(4) . ?
C11 C16 1.394(4) . ?
C11 C12 1.401(4) . ?
C12 C13 1.398(4) . ?
C12 C121 1.513(4) . ?
C13 C14 1.371(5) . ?
C14 C15 1.378(5) . ?
C15 C16 1.394(4) . ?
C16 C161 1.517(4) . ?
C21 C26 1.397(4) . ?
C21 C22 1.401(4) . ?
C22 C23 1.392(4) . ?
C22 C221 1.505(5) . ?
C23 C24 1.365(5) . ?
C24 C25 1.378(5) . ?
C25 C26 1.398(4) . ?
C26 C261 1.508(5) . ?
C31 C32 1.364(8) . ?
C31 C36 1.368(9) . ?
C31 C37 1.433(10) . ?
C32 C33 1.356(13) . ?
C33 C34 1.495(14) . ?
C34 C35 1.296(13) . ?
C35 C36 1.342(10) . ?
C121 C122 1.530(5) . ?
C121 C123 1.538(5) . ?
C161 C163 1.526(6) . ?
C161 C162 1.532(6) . ?
C221 C222 1.518(5) . ?
C221 C223 1.519(6) . ?
C261 C262 1.529(6) . ?
C261 C263 1.529(6) . ?
