#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:25:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179919 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/14/7021421.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_7021421
loop_
_publ_author_name
'Padělková, Zdeňka'
'Svec, Petr'
'Pejchal, Vladimír'
'R°užička, Aleš'
_publ_section_title
;
 Activation of E-Cl bonds (E = C, Si, Ge and Sn) by a C,N-chelated
 stannylene.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7660
_journal_page_last               7671
_journal_paper_doi               10.1039/c3dt50278c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C72 H60 Ge4 O8 Sn6'
_chemical_formula_sum            'C72 H60 Ge4 O8 Sn6'
_chemical_formula_weight         2055.70
_chemical_name_systematic
;
?
;
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.0010(7)
_cell_length_b                   16.0010(7)
_cell_length_c                   17.4671(15)
_cell_measurement_reflns_used    24025
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     3873.0(4)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23910
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.80
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.476
_exptl_absorpt_correction_T_max  0.675
_exptl_absorpt_correction_T_min  0.460
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5862
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0342
_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)+(0.0252P)²+5.5113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                5053
_reflns_number_total             5862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50278c.txt
_cod_data_source_block           shelxl5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               7021421
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, 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
Sn1 Sn 0.64583(2) 0.19694(2) 0.25851(2) 0.02401(8) Uani 1 1 d .
Sn2 Sn 0.52938(2) 0.22053(2) 0.094145(19) 0.02536(9) Uani 1 1 d .
Ge2 Ge 0.6667 0.3333 -0.08387(6) 0.02239(19) Uani 1 3 d S
Ge1 Ge 0.37721(3) 0.09361(3) 0.25482(3) 0.02308(11) Uani 1 1 d .
O3 O 0.6667 0.3333 0.2842(3) 0.0212(13) Uani 1 3 d S
O2 O 0.6447(2) 0.2139(2) 0.1399(2) 0.0222(7) Uani 1 1 d .
O4 O 0.6667 0.3333 0.0187(3) 0.0268(14) Uani 1 3 d S
O1 O 0.4927(2) 0.1926(2) 0.2294(2) 0.0258(8) Uani 1 1 d .
C1 C 0.3543(4) -0.0140(4) 0.1889(3) 0.0278(11) Uani 1 1 d .
C14 C 0.2075(4) 0.1080(4) 0.2921(4) 0.0368(13) Uani 1 1 d .
H14 H 0.2080 0.0780 0.3375 0.044 Uiso 1 1 d R
C8 C 0.3063(5) -0.0320(4) 0.3854(4) 0.0382(14) Uani 1 1 d .
H8 H 0.2602 -0.0750 0.3513 0.046 Uiso 1 1 d R
C7 C 0.3772(4) 0.0585(4) 0.3612(3) 0.0299(12) Uani 1 1 d .
C13 C 0.2800(3) 0.1306(4) 0.2380(3) 0.0265(11) Uani 1 1 d .
C20 C 0.8726(4) 0.3913(4) -0.0928(3) 0.0320(12) Uani 1 1 d .
H20 H 0.8817 0.4341 -0.0533 0.038 Uiso 1 1 d R
C6 C 0.4034(5) -0.0641(4) 0.2012(3) 0.0399(14) Uani 1 1 d .
H6 H 0.4447 -0.0483 0.2429 0.048 Uiso 1 1 d R
C15 C 0.1344(4) 0.1283(4) 0.2808(4) 0.0415(16) Uani 1 1 d .
H15 H 0.0854 0.1104 0.3168 0.050 Uiso 1 1 d R
C21 C 0.9505(4) 0.3882(4) -0.1220(4) 0.0387(14) Uani 1 1 d .
H21 H 1.0117 0.4289 -0.1023 0.046 Uiso 1 1 d R
C2 C 0.2897(4) -0.0426(5) 0.1272(4) 0.0400(15) Uani 1 1 d .
H2 H 0.2560 -0.0104 0.1172 0.048 Uiso 1 1 d R
C19 C 0.7800(4) 0.3316(4) -0.1212(3) 0.0248(11) Uani 1 1 d .
C23 C 0.8491(4) 0.2688(4) -0.2129(4) 0.0455(16) Uani 1 1 d .
H23 H 0.8416 0.2284 -0.2538 0.055 Uiso 1 1 d R
C12 C 0.4464(4) 0.1191(5) 0.4130(4) 0.0420(14) Uani 1 1 d .
H12 H 0.4965 0.1792 0.3980 0.050 Uiso 1 1 d R
C16 C 0.1341(5) 0.1740(5) 0.2127(4) 0.0457(16) Uani 1 1 d .
H16 H 0.0849 0.1878 0.2039 0.055 Uiso 1 1 d R
C17 C 0.2052(5) 0.2002(5) 0.1612(4) 0.0448(15) Uani 1 1 d .
H17 H 0.2053 0.2340 0.1178 0.054 Uiso 1 1 d R
C22 C 0.9386(5) 0.3262(5) -0.1810(4) 0.0460(17) Uani 1 1 d .
H22 H 0.9913 0.3230 -0.1997 0.055 Uiso 1 1 d R
C18 C 0.2776(4) 0.1785(4) 0.1717(3) 0.0389(14) Uani 1 1 d .
H18 H 0.3248 0.1959 0.1343 0.047 Uiso 1 1 d R
C5 C 0.3901(5) -0.1389(5) 0.1547(4) 0.0489(17) Uani 1 1 d .
H5 H 0.4254 -0.1702 0.1613 0.059 Uiso 1 1 d R
C4 C 0.3255(5) -0.1663(4) 0.0936(5) 0.0544(17) Uani 1 1 d .
H4 H 0.3136 -0.2192 0.0636 0.065 Uiso 1 1 d R
C24 C 0.7701(4) 0.2703(4) -0.1816(4) 0.0376(14) Uani 1 1 d .
H24 H 0.7092 0.2302 -0.2022 0.045 Uiso 1 1 d R
C9 C 0.3037(6) -0.0597(6) 0.4629(4) 0.0525(18) Uani 1 1 d .
H9 H 0.2552 -0.1197 0.4796 0.063 Uiso 1 1 d R
C11 C 0.4425(6) 0.0899(6) 0.4885(4) 0.058(2) Uani 1 1 d .
H11 H 0.4869 0.1320 0.5240 0.069 Uiso 1 1 d R
C3 C 0.2768(5) -0.1178(5) 0.0810(4) 0.0545(19) Uani 1 1 d .
H3 H 0.2348 -0.1356 0.0396 0.065 Uiso 1 1 d R
C10 C 0.3713(6) -0.0005(6) 0.5120(4) 0.059(2) Uani 1 1 d .
H10 H 0.3705 -0.0199 0.5623 0.071 Uiso 1 1 d 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 0 0.062
1 -1 0 0.108
0 1 0 0.097
0 -1 0 0.115
0 0 1 0.060
0 0 -1 0.060
-1 0 0 0.130
1 0 0 0.153
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
O3 Sn1 O2 94.86(19) . .
O3 Sn1 O1 76.36(10) . 3_655
O2 Sn1 O1 76.69(12) . 3_655
O3 Sn1 O1 73.20(9) . .
O2 Sn1 O1 74.18(12) . .
O1 Sn1 O1 135.31(14) 3_655 .
O2 Sn2 O2 94.97(18) . 4_665
O2 Sn2 O4 75.37(12) . .
O2 Sn2 O4 75.13(12) 4_665 .
O2 Sn2 O1 75.67(13) . .
O2 Sn2 O1 74.70(13) 4_665 .
O4 Sn2 O1 135.62(15) . .
O4 Ge2 C19 109.64(16) . .
O4 Ge2 C19 109.63(16) . 4_665
C19 Ge2 C19 109.34(16) . 4_665
O4 Ge2 C19 109.62(16) . 3_655
C19 Ge2 C19 109.31(16) . 3_655
C19 Ge2 C19 109.28(16) 4_665 3_655
O1 Ge1 C7 110.1(2) . .
O1 Ge1 C13 108.85(19) . .
C7 Ge1 C13 110.4(2) . .
O1 Ge1 C1 106.91(19) . .
C7 Ge1 C1 109.7(2) . .
C13 Ge1 C1 110.8(2) . .
Sn1 O3 Sn1 115.54(12) . 3_655
Sn1 O3 Sn1 115.50(11) . 4_665
Sn1 O3 Sn1 115.48(11) 3_655 4_665
Sn2 O2 Sn2 116.15(16) . 3_655
Sn2 O2 Sn1 117.17(16) . .
Sn2 O2 Sn1 113.79(15) 3_655 .
Ge2 O4 Sn2 123.01(12) . 3_655
Ge2 O4 Sn2 123.00(12) . .
Sn2 O4 Sn2 93.17(16) 3_655 .
Ge2 O4 Sn2 122.99(12) . 4_665
Sn2 O4 Sn2 93.16(16) 3_655 4_665
Sn2 O4 Sn2 93.14(16) . 4_665
Ge1 O1 Sn1 126.46(17) . 4_665
Ge1 O1 Sn2 116.95(17) . .
Sn1 O1 Sn2 94.73(12) 4_665 .
Ge1 O1 Sn1 123.08(16) . .
Sn1 O1 Sn1 94.73(12) 4_665 .
Sn2 O1 Sn1 92.87(11) . .
C6 C1 C2 117.8(5) . .
C6 C1 Ge1 120.5(4) . .
C2 C1 Ge1 121.7(4) . .
C15 C14 C13 122.5(6) . .
C15 C14 H14 118.1 . .
C13 C14 H14 119.4 . .
C7 C8 C9 119.9(7) . .
C7 C8 H8 120.7 . .
C9 C8 H8 119.5 . .
C8 C7 C12 118.9(6) . .
C8 C7 Ge1 118.4(5) . .
C12 C7 Ge1 122.6(4) . .
C14 C13 C18 117.0(5) . .
C14 C13 Ge1 120.5(4) . .
C18 C13 Ge1 122.5(4) . .
C21 C20 C19 121.1(5) . .
C21 C20 H20 119.5 . .
C19 C20 H20 119.4 . .
C5 C6 C1 121.8(6) . .
C5 C6 H6 118.6 . .
C1 C6 H6 119.6 . .
C14 C15 C16 118.0(6) . .
C14 C15 H15 121.0 . .
C16 C15 H15 121.0 . .
C20 C21 C22 120.3(6) . .
C20 C21 H21 119.7 . .
C22 C21 H21 120.0 . .
C3 C2 C1 120.0(6) . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
C20 C19 C24 117.4(5) . .
C20 C19 Ge2 123.5(4) . .
C24 C19 Ge2 119.1(4) . .
C22 C23 C24 118.7(6) . .
C22 C23 H23 120.4 . .
C24 C23 H23 120.8 . .
C7 C12 C11 119.9(6) . .
C7 C12 H12 120.9 . .
C11 C12 H12 119.1 . .
C17 C16 C15 120.7(6) . .
C17 C16 H16 120.0 . .
C15 C16 H16 119.3 . .
C16 C17 C18 121.3(6) . .
C16 C17 H17 118.9 . .
C18 C17 H17 119.8 . .
C23 C22 C21 120.6(6) . .
C23 C22 H22 119.4 . .
C21 C22 H22 120.0 . .
C17 C18 C13 120.4(6) . .
C17 C18 H18 119.3 . .
C13 C18 H18 120.3 . .
C6 C5 C4 119.6(6) . .
C6 C5 H5 121.7 . .
C4 C5 H5 118.6 . .
C3 C4 C5 119.2(6) . .
C3 C4 H4 120.6 . .
C5 C4 H4 120.0 . .
C23 C24 C19 121.7(6) . .
C23 C24 H24 118.9 . .
C19 C24 H24 119.3 . .
C10 C9 C8 120.4(7) . .
C10 C9 H9 119.6 . .
C8 C9 H9 120.1 . .
C10 C11 C12 120.6(7) . .
C10 C11 H11 119.3 . .
C12 C11 H11 120.0 . .
C4 C3 C2 121.6(7) . .
C4 C3 H3 118.8 . .
C2 C3 H3 119.6 . .
C9 C10 C11 120.2(7) . .
C9 C10 H10 120.0 . .
C11 C10 H10 119.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 O3 2.0844(14) .
Sn1 O2 2.090(4) .
Sn1 O1 2.323(3) 3_655
Sn1 O1 2.469(3) .
Sn2 O2 2.063(3) .
Sn2 O2 2.079(3) 4_665
Sn2 O4 2.420(3) .
Sn2 O1 2.422(3) .
Ge2 O4 1.791(6) .
Ge2 C19 1.940(5) .
Ge2 C19 1.941(5) 4_665
Ge2 C19 1.941(5) 3_655
Ge1 O1 1.787(3) .
Ge1 C7 1.941(6) .
Ge1 C13 1.943(5) .
Ge1 C1 1.947(5) .
O3 Sn1 2.0849(14) 3_655
O3 Sn1 2.0859(14) 4_665
O2 Sn2 2.079(3) 3_655
O4 Sn2 2.419(3) 3_655
O4 Sn2 2.420(3) 4_665
O1 Sn1 2.323(3) 4_665
C1 C6 1.390(8) .
C1 C2 1.403(8) .
C14 C15 1.377(8) .
C14 C13 1.396(8) .
C14 H14 0.9301 .
C8 C7 1.385(8) .
C8 C9 1.419(9) .
C8 H8 0.9301 .
C7 C12 1.383(8) .
C13 C18 1.400(8) .
C20 C21 1.371(8) .
C20 C19 1.393(7) .
C20 H20 0.9301 .
C6 C5 1.373(8) .
C6 H6 0.9300 .
C15 C16 1.398(9) .
C15 H15 0.9301 .
C21 C22 1.375(9) .
C21 H21 0.9300 .
C2 C3 1.375(9) .
C2 H2 0.9300 .
C19 C24 1.394(8) .
C23 C22 1.374(9) .
C23 C24 1.390(8) .
C23 H23 0.9300 .
C12 C11 1.389(9) .
C12 H12 0.9301 .
C16 C17 1.342(9) .
C16 H16 0.9300 .
C17 C18 1.379(8) .
C17 H17 0.9301 .
C22 H22 0.9299 .
C18 H18 0.9299 .
C5 C4 1.394(10) .
C5 H5 0.9300 .
C4 C3 1.366(10) .
C4 H4 0.9301 .
C24 H24 0.9300 .
C9 C10 1.334(11) .
C9 H9 0.9299 .
C11 C10 1.383(11) .
C11 H11 0.9300 .
C3 H3 0.9299 .
C10 H10 0.9300 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 -0.012 236.6 99.5
2 0.000 0.000 0.488 236.7 97.9
3 0.333 0.667 0.956 19.5 -0.2
4 0.333 0.667 0.214 7.3 -0.1
5 0.667 0.333 0.456 19.5 0.6
6 0.667 0.333 0.714 7.3 0.2
