#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:07:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179232 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/52/4315261.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_4315261
loop_
_publ_author_name
'Elisabeth Oehlke'
'Roger Alberto'
'Ulrich Abram'
_publ_contact_author
;
      Ulrich Abram
      Free University of Berlin
      Institute of Chemistry
      Fabeckstrasse 34-36
      D-14195 Berlin 
      Germany
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
 Synthesis, Characterization, and Structures of R3EOTcO3 Complexes (E = C,
 Si, Ge, Sn, Pb) and Related Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3525
_journal_page_last               3530
_journal_paper_doi               10.1021/ic1001094
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C22 H23 O5 Sn Tc'
_chemical_formula_sum            'C22 H23 O5 Sn Tc'
_chemical_formula_weight         584.09
_chemical_name_common            '[O3TcOSnPh3(THF)]'
_chemical_name_systematic
;
 Triphenyltetrahydrofuranestannylpertechnetat
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.893(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.7204(8)
_cell_length_b                   14.4758(10)
_cell_length_c                   16.7801(8)
_cell_measurement_reflns_used    20977
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.23
_cell_volume                     4432.6(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-Red'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0872
_diffrn_reflns_av_sigmaI/netI    0.0881
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25944
_diffrn_reflns_theta_full        29.30
_diffrn_reflns_theta_max         29.30
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    1.779
_exptl_absorpt_correction_T_max  0.6873
_exptl_absorpt_correction_T_min  0.3914
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED 32'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyeder
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.310
_refine_diff_density_min         -1.938
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         11847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0470
_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)+(0.0834P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1332
_reflns_number_gt                8084
_reflns_number_total             11847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1001094_si_002_4.cif
_cod_data_source_block           eosn
_cod_database_code               4315261
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Sn1 Sn 0.146851(16) -0.48086(2) 0.697469(19) 0.02781(8) Uani 1 1 d . . .
Tc1 Tc 0.34699(2) -0.41197(4) 0.73460(3) 0.04533(13) Uani 1 1 d . . .
O11 O 0.2524(2) -0.4059(3) 0.7222(3) 0.0482(10) Uani 1 1 d . . .
O12 O 0.03912(19) -0.5669(2) 0.6722(2) 0.0351(8) Uani 1 1 d . . .
O13 O 0.3799(4) -0.4921(7) 0.8067(4) 0.130(4) Uani 1 1 d . . .
O14 O 0.3694(3) -0.4520(5) 0.6492(3) 0.0834(18) Uani 1 1 d . . .
O15 O 0.3836(4) -0.3139(6) 0.7602(10) 0.230(8) Uani 1 1 d . . .
C1 C 0.0890(3) -0.3618(3) 0.6426(3) 0.0303(9) Uani 1 1 d . . .
C2 C 0.1280(3) -0.2828(4) 0.6312(3) 0.0389(11) Uani 1 1 d . . .
H2 H 0.1789 -0.2849 0.6421 0.047 Uiso 1 1 calc R . .
C3 C 0.0919(4) -0.2005(4) 0.6037(3) 0.0517(15) Uani 1 1 d . . .
H3 H 0.1186 -0.1481 0.5969 0.062 Uiso 1 1 calc R . .
C4 C 0.0160(4) -0.1974(4) 0.5866(3) 0.0508(15) Uani 1 1 d . . .
H4 H -0.0083 -0.1429 0.5679 0.061 Uiso 1 1 calc R . .
C5 C -0.0229(4) -0.2740(5) 0.5971(4) 0.0499(14) Uani 1 1 d . . .
H5 H -0.0739 -0.2716 0.5850 0.060 Uiso 1 1 calc R . .
C6 C 0.0129(3) -0.3571(4) 0.6261(3) 0.0399(11) Uani 1 1 d . . .
H6 H -0.0142 -0.4086 0.6343 0.048 Uiso 1 1 calc R . .
C7 C 0.1507(2) -0.4942(3) 0.8241(3) 0.0308(9) Uani 1 1 d . . .
C8 C 0.0934(3) -0.4596(4) 0.8543(3) 0.0370(11) Uani 1 1 d . . .
H8 H 0.0545 -0.4304 0.8192 0.044 Uiso 1 1 calc R . .
C9 C 0.0934(4) -0.4681(5) 0.9366(4) 0.0502(14) Uani 1 1 d . . .
H9 H 0.0542 -0.4454 0.9565 0.060 Uiso 1 1 calc R . .
C10 C 0.1522(4) -0.5108(4) 0.9896(4) 0.0553(16) Uani 1 1 d . . .
H10 H 0.1521 -0.5173 1.0447 0.066 Uiso 1 1 calc R . .
C11 C 0.2099(4) -0.5429(5) 0.9600(4) 0.0552(16) Uani 1 1 d . . .
H11 H 0.2498 -0.5700 0.9954 0.066 Uiso 1 1 calc R . .
C12 C 0.2094(3) -0.5354(4) 0.8781(4) 0.0446(13) Uani 1 1 d . . .
H12 H 0.2487 -0.5581 0.8586 0.054 Uiso 1 1 calc R . .
C13 C 0.1903(3) -0.5809(3) 0.6291(3) 0.0306(9) Uani 1 1 d . . .
C14 C 0.1971(3) -0.5605(4) 0.5504(4) 0.0460(13) Uani 1 1 d . . .
H14 H 0.1830 -0.5029 0.5278 0.055 Uiso 1 1 calc R . .
C15 C 0.2252(4) -0.6264(5) 0.5054(4) 0.0563(16) Uani 1 1 d . . .
H15 H 0.2297 -0.6126 0.4526 0.068 Uiso 1 1 calc R . .
C16 C 0.2465(4) -0.7121(5) 0.5385(5) 0.0592(17) Uani 1 1 d . . .
H16 H 0.2654 -0.7558 0.5082 0.071 Uiso 1 1 calc R . .
C17 C 0.2397(4) -0.7321(4) 0.6157(5) 0.0586(17) Uani 1 1 d . . .
H17 H 0.2540 -0.7898 0.6381 0.070 Uiso 1 1 calc R . .
C18 C 0.2116(3) -0.6675(4) 0.6610(4) 0.0473(13) Uani 1 1 d . . .
H18 H 0.2069 -0.6822 0.7136 0.057 Uiso 1 1 calc R . .
C41 C 0.0053(4) -0.6007(5) 0.5909(3) 0.0522(15) Uani 1 1 d . . .
H41A H -0.0321 -0.5579 0.5634 0.063 Uiso 1 1 calc R . .
H41B H 0.0418 -0.6073 0.5583 0.063 Uiso 1 1 calc R . .
C42 C -0.0257(9) -0.6857(10) 0.6009(5) 0.163(8) Uani 1 1 d . . .
H42A H 0.0024 -0.7341 0.5823 0.196 Uiso 1 1 calc R . .
H42B H -0.0752 -0.6878 0.5676 0.196 Uiso 1 1 calc R . .
C43 C -0.0276(4) -0.7019(5) 0.6837(4) 0.0618(19) Uani 1 1 d . . .
H43A H -0.0096 -0.7634 0.7003 0.074 Uiso 1 1 calc R . .
H43B H -0.0773 -0.6963 0.6914 0.074 Uiso 1 1 calc R . .
C44 C 0.0205(3) -0.6306(4) 0.7321(3) 0.0369(11) Uani 1 1 d . . .
H44A H -0.0050 -0.5984 0.7682 0.044 Uiso 1 1 calc R . .
H44B H 0.0644 -0.6587 0.7648 0.044 Uiso 1 1 calc R . .
Sn2 Sn 0.344672(17) -0.49263(2) 0.286050(19) 0.02833(9) Uani 1 1 d . . .
Tc2 Tc 0.14815(2) -0.57552(3) 0.25077(3) 0.04033(12) Uani 1 1 d . . .
O21 O 0.23684(19) -0.5551(3) 0.2364(2) 0.0413(8) Uani 1 1 d . . .
O22 O 0.45636(19) -0.4168(2) 0.3319(2) 0.0361(8) Uani 1 1 d . . .
O23 O 0.1311(3) -0.5056(4) 0.3247(4) 0.0698(14) Uani 1 1 d . . .
O24 O 0.1438(3) -0.6848(3) 0.2842(4) 0.0688(14) Uani 1 1 d . . .
O25 O 0.0871(3) -0.5574(7) 0.1628(4) 0.117(3) Uani 1 1 d . . .
C21 C 0.2968(2) -0.3960(3) 0.3528(3) 0.0287(9) Uani 1 1 d . . .
C22 C 0.2592(3) -0.3194(4) 0.3155(4) 0.0446(13) Uani 1 1 d . . .
H22 H 0.2551 -0.3100 0.2598 0.054 Uiso 1 1 calc R . .
C23 C 0.2275(3) -0.2568(4) 0.3594(4) 0.0498(14) Uani 1 1 d . . .
H23 H 0.2033 -0.2052 0.3334 0.060 Uiso 1 1 calc R . .
C24 C 0.2316(3) -0.2703(4) 0.4402(4) 0.0486(14) Uani 1 1 d . . .
H24 H 0.2093 -0.2287 0.4692 0.058 Uiso 1 1 calc R . .
C25 C 0.2687(4) -0.3453(6) 0.4794(4) 0.0600(17) Uani 1 1 d . . .
H25 H 0.2722 -0.3537 0.5351 0.072 Uiso 1 1 calc R . .
C26 C 0.3011(3) -0.4090(4) 0.4357(3) 0.0461(13) Uani 1 1 d . . .
H26 H 0.3255 -0.4602 0.4622 0.055 Uiso 1 1 calc R . .
C27 C 0.3630(2) -0.4795(3) 0.1664(3) 0.0304(9) Uani 1 1 d . . .
C28 C 0.3433(3) -0.4044(4) 0.1141(3) 0.0423(12) Uani 1 1 d . . .
H28 H 0.3179 -0.3550 0.1301 0.051 Uiso 1 1 calc R . .
C29 C 0.3617(3) -0.4032(5) 0.0376(4) 0.0508(15) Uani 1 1 d . . .
H29 H 0.3476 -0.3532 0.0029 0.061 Uiso 1 1 calc R . .
C30 C 0.3994(3) -0.4734(5) 0.0133(3) 0.0531(15) Uani 1 1 d . . .
H30 H 0.4117 -0.4714 -0.0374 0.064 Uiso 1 1 calc R . .
C31 C 0.4196(4) -0.5485(5) 0.0650(4) 0.0603(17) Uani 1 1 d . . .
H31 H 0.4453 -0.5975 0.0489 0.072 Uiso 1 1 calc R . .
C33 C 0.3902(3) -0.6188(3) 0.3403(3) 0.0295(9) Uani 1 1 d . . .
C34 C 0.4662(3) -0.6301(4) 0.3620(3) 0.0350(10) Uani 1 1 d . . .
H34 H 0.4966 -0.5800 0.3588 0.042 Uiso 1 1 calc R . .
C35 C 0.4967(3) -0.7150(4) 0.3883(3) 0.0393(11) Uani 1 1 d . . .
H35 H 0.5474 -0.7216 0.4023 0.047 Uiso 1 1 calc R . .
C36 C 0.4529(3) -0.7895(4) 0.3939(3) 0.0414(12) Uani 1 1 d . . .
H36 H 0.4736 -0.8466 0.4108 0.050 Uiso 1 1 calc R . .
C37 C 0.3777(3) -0.7790(4) 0.3741(4) 0.0439(12) Uani 1 1 d . . .
H37 H 0.3477 -0.8288 0.3793 0.053 Uiso 1 1 calc R . .
C38 C 0.3465(3) -0.6942(4) 0.3463(3) 0.0383(11) Uani 1 1 d . . .
H38 H 0.2958 -0.6883 0.3317 0.046 Uiso 1 1 calc R . .
C45 C 0.4837(4) -0.3840(6) 0.4154(4) 0.0614(19) Uani 1 1 d . . .
H45A H 0.4526 -0.3351 0.4282 0.074 Uiso 1 1 calc R . .
H45B H 0.4848 -0.4340 0.4542 0.074 Uiso 1 1 calc R . .
C46 C 0.5568(5) -0.3499(9) 0.4186(5) 0.103(4) Uani 1 1 d . . .
H46A H 0.5926 -0.3985 0.4352 0.124 Uiso 1 1 calc R . .
H46B H 0.5683 -0.2991 0.4571 0.124 Uiso 1 1 calc R . .
C47 C 0.5569(4) -0.3182(6) 0.3348(4) 0.066(2) Uani 1 1 d . . .
H47A H 0.6042 -0.3297 0.3221 0.079 Uiso 1 1 calc R . .
H47B H 0.5466 -0.2526 0.3293 0.079 Uiso 1 1 calc R . .
C48 C 0.4983(3) -0.3723(4) 0.2789(3) 0.0411(12) Uani 1 1 d . . .
H48A H 0.4672 -0.3317 0.2400 0.049 Uiso 1 1 calc R . .
H48B H 0.5197 -0.4181 0.2490 0.049 Uiso 1 1 calc R . .
C32 C 0.4012(4) -0.5501(4) 0.1409(4) 0.0483(14) Uani 1 1 d . . .
H32 H 0.4152 -0.6005 0.1752 0.058 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'
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'
Tc Tc -1.4390 0.7593 '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
C13 Sn1 C7 123.30(18) . . ?
C13 Sn1 C1 122.53(18) . . ?
C7 Sn1 C1 114.06(18) . . ?
C13 Sn1 O11 90.13(17) . . ?
C7 Sn1 O11 91.58(17) . . ?
C1 Sn1 O11 91.74(17) . . ?
C13 Sn1 O12 87.55(16) . . ?
C7 Sn1 O12 88.17(15) . . ?
C1 Sn1 O12 91.04(16) . . ?
O11 Sn1 O12 177.05(14) . . ?
O15 Tc1 O14 111.3(6) . . ?
O15 Tc1 O13 110.6(7) . . ?
O14 Tc1 O13 104.6(4) . . ?
O15 Tc1 O11 110.6(3) . . ?
O14 Tc1 O11 110.8(2) . . ?
O13 Tc1 O11 108.7(3) . . ?
Tc1 O11 Sn1 147.3(2) . . ?
C41 O12 C44 108.2(4) . . ?
C41 O12 Sn1 121.9(3) . . ?
C44 O12 Sn1 122.8(3) . . ?
C6 C1 C2 118.5(5) . . ?
C6 C1 Sn1 121.6(4) . . ?
C2 C1 Sn1 119.5(4) . . ?
C1 C2 C3 121.1(5) . . ?
C1 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
C4 C3 C2 119.6(6) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C5 C4 C3 120.1(5) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.8(6) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 119.9(5) . . ?
C1 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C8 C7 C12 118.8(5) . . ?
C8 C7 Sn1 118.7(3) . . ?
C12 C7 Sn1 122.5(4) . . ?
C7 C8 C9 120.5(5) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C8 C9 C10 119.8(6) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 119.7(6) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 120.3(6) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C11 C12 C7 120.9(6) . . ?
C11 C12 H12 119.6 . . ?
C7 C12 H12 119.6 . . ?
C18 C13 C14 118.7(5) . . ?
C18 C13 Sn1 121.4(4) . . ?
C14 C13 Sn1 119.9(4) . . ?
C13 C14 C15 119.9(6) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 120.5(6) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C17 C16 C15 119.6(6) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 120.5(6) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C17 C18 C13 120.8(6) . . ?
C17 C18 H18 119.6 . . ?
C13 C18 H18 119.6 . . ?
C42 C41 O12 106.9(6) . . ?
C42 C41 H41A 110.3 . . ?
O12 C41 H41A 110.3 . . ?
C42 C41 H41B 110.3 . . ?
O12 C41 H41B 110.3 . . ?
H41A C41 H41B 108.6 . . ?
C41 C42 C43 111.7(6) . . ?
C41 C42 H42A 109.3 . . ?
C43 C42 H42A 109.3 . . ?
C41 C42 H42B 109.3 . . ?
C43 C42 H42B 109.3 . . ?
H42A C42 H42B 107.9 . . ?
C42 C43 C44 106.0(6) . . ?
C42 C43 H43A 110.5 . . ?
C44 C43 H43A 110.5 . . ?
C42 C43 H43B 110.5 . . ?
C44 C43 H43B 110.5 . . ?
H43A C43 H43B 108.7 . . ?
O12 C44 C43 105.7(4) . . ?
O12 C44 H44A 110.6 . . ?
C43 C44 H44A 110.6 . . ?
O12 C44 H44B 110.6 . . ?
C43 C44 H44B 110.6 . . ?
H44A C44 H44B 108.7 . . ?
C21 Sn2 C27 128.35(18) . . ?
C21 Sn2 C33 121.16(18) . . ?
C27 Sn2 C33 110.33(18) . . ?
C21 Sn2 O21 90.64(16) . . ?
C27 Sn2 O21 90.38(16) . . ?
C33 Sn2 O21 93.20(16) . . ?
C21 Sn2 O22 88.19(15) . . ?
C27 Sn2 O22 87.02(14) . . ?
C33 Sn2 O22 91.04(15) . . ?
O21 Sn2 O22 175.60(14) . . ?
O25 Tc2 O23 110.6(4) . . ?
O25 Tc2 O24 111.5(4) . . ?
O23 Tc2 O24 106.7(3) . . ?
O25 Tc2 O21 109.4(2) . . ?
O23 Tc2 O21 109.9(2) . . ?
O24 Tc2 O21 108.8(2) . . ?
Tc2 O21 Sn2 146.5(2) . . ?
C45 O22 C48 108.6(4) . . ?
C45 O22 Sn2 124.5(3) . . ?
C48 O22 Sn2 124.8(3) . . ?
C22 C21 C26 118.1(5) . . ?
C22 C21 Sn2 121.5(4) . . ?
C26 C21 Sn2 120.3(4) . . ?
C23 C22 C21 121.2(5) . . ?
C23 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
C24 C23 C22 120.2(5) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.2(6) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C26 120.1(6) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 120.1(5) . . ?
C21 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C32 C27 C28 117.9(5) . . ?
C32 C27 Sn2 115.9(4) . . ?
C28 C27 Sn2 126.1(4) . . ?
C27 C28 C29 120.1(5) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 121.3(6) . . ?
C30 C29 H29 119.3 . . ?
C28 C29 H29 119.3 . . ?
C29 C30 C31 119.1(6) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C30 C31 C32 119.7(6) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C38 C33 C34 118.3(4) . . ?
C38 C33 Sn2 121.4(3) . . ?
C34 C33 Sn2 119.9(3) . . ?
C35 C34 C33 120.7(5) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C36 C35 C34 120.6(5) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C35 C36 C37 119.4(5) . . ?
C35 C36 H36 120.3 . . ?
C37 C36 H36 120.3 . . ?
C36 C37 C38 120.4(5) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C33 C38 C37 120.6(5) . . ?
C33 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C46 C45 O22 105.9(6) . . ?
C46 C45 H45A 110.6 . . ?
O22 C45 H45A 110.6 . . ?
C46 C45 H45B 110.6 . . ?
O22 C45 H45B 110.6 . . ?
H45A C45 H45B 108.7 . . ?
C45 C46 C47 105.9(6) . . ?
C45 C46 H46A 110.6 . . ?
C47 C46 H46A 110.6 . . ?
C45 C46 H46B 110.6 . . ?
C47 C46 H46B 110.6 . . ?
H46A C46 H46B 108.7 . . ?
C46 C47 C48 106.1(6) . . ?
C46 C47 H47A 110.5 . . ?
C48 C47 H47A 110.5 . . ?
C46 C47 H47B 110.5 . . ?
C48 C47 H47B 110.5 . . ?
H47A C47 H47B 108.7 . . ?
O22 C48 C47 105.5(5) . . ?
O22 C48 H48A 110.6 . . ?
C47 C48 H48A 110.6 . . ?
O22 C48 H48B 110.6 . . ?
C47 C48 H48B 110.6 . . ?
H48A C48 H48B 108.8 . . ?
C27 C32 C31 121.8(6) . . ?
C27 C32 H32 119.1 . . ?
C31 C32 H32 119.1 . . ?
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
Sn1 C13 2.119(5) . ?
Sn1 C7 2.119(5) . ?
Sn1 C1 2.132(5) . ?
Sn1 O11 2.211(4) . ?
Sn1 O12 2.327(3) . ?
Tc1 O15 1.594(7) . ?
Tc1 O14 1.684(6) . ?
Tc1 O13 1.689(7) . ?
Tc1 O11 1.738(4) . ?
O12 C41 1.456(6) . ?
O12 C44 1.462(6) . ?
C1 C6 1.391(7) . ?
C1 C2 1.392(7) . ?
C2 C3 1.396(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.361(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.410(8) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.379(7) . ?
C7 C12 1.391(6) . ?
C8 C9 1.387(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.396(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.368(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.377(9) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C18 1.386(7) . ?
C13 C14 1.386(7) . ?
C14 C15 1.390(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.381(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.361(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.383(9) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C41 C42 1.386(11) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.418(11) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.486(7) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
Sn2 C21 2.112(5) . ?
Sn2 C27 2.119(5) . ?
Sn2 C33 2.133(4) . ?
Sn2 O21 2.199(3) . ?
Sn2 O22 2.334(3) . ?
Tc2 O25 1.674(5) . ?
Tc2 O23 1.686(5) . ?
Tc2 O24 1.686(5) . ?
Tc2 O21 1.755(4) . ?
O22 C45 1.459(6) . ?
O22 C48 1.462(6) . ?
C21 C22 1.386(7) . ?
C21 C26 1.388(7) . ?
C22 C23 1.384(8) . ?
C22 H22 0.9300 . ?
C23 C24 1.354(9) . ?
C23 H23 0.9300 . ?
C24 C25 1.375(9) . ?
C24 H24 0.9300 . ?
C25 C26 1.398(9) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C32 1.369(8) . ?
C27 C28 1.395(7) . ?
C28 C29 1.402(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.352(10) . ?
C29 H29 0.9300 . ?
C30 C31 1.390(10) . ?
C30 H30 0.9300 . ?
C31 C32 1.392(9) . ?
C31 H31 0.9300 . ?
C33 C38 1.381(7) . ?
C33 C34 1.396(7) . ?
C34 C35 1.386(7) . ?
C34 H34 0.9300 . ?
C35 C36 1.371(8) . ?
C35 H35 0.9300 . ?
C36 C37 1.380(8) . ?
C36 H36 0.9300 . ?
C37 C38 1.394(7) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C45 C46 1.445(10) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.479(12) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.495(8) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C32 H32 0.9300 . ?
