#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/61/2226153.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2226153
loop_
_publ_author_name
'Berends, Thorsten'
'Iovkova, Ljuba'
'Tiekink, Edward R. T.'
'Jurkschat, Klaus'
_publ_section_title
;
 Bis{decacarbonylbis[μ-2,2'-(phenylimino)diethanolato]ditin(II)ditungsten(0)(2
 Sn{---W})} hexacarbonyltungsten(0)
;
_journal_coeditor_code           HB5458
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m715
_journal_page_last               m716
_journal_paper_doi               10.1107/S1600536810019343
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Sn2 W2 (C10 H13 N O2)2 (C O)10]2 [W (C O)6]'
_chemical_formula_moiety         '2(C30 H26 N2 O14 Sn2 W2), C6 O6 W'
_chemical_formula_sum            'C66 H52 N4 O34 Sn4 W5'
_chemical_formula_weight         2839.15
_chemical_melting_point          460
_chemical_name_common
;
Bis{decacarbonylbis[μ-2,2'-(phenylimino)diethanolato]ditin(II)ditungsten(0)(2
Sn---W)} hexacarbonyltungsten(0)
;
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                108.715(4)
_cell_angle_beta                 92.758(4)
_cell_angle_gamma                115.350(4)
_cell_formula_units_Z            1
_cell_length_a                   11.3547(5)
_cell_length_b                   12.5454(5)
_cell_length_c                   16.8187(7)
_cell_measurement_reflns_used    35730
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.0
_cell_volume                     2001.90(18)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0560
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur2 CCD'
_diffrn_measurement_method
;
973 frames via ω-rotation (Δω = 1°) and two times 30 s
per frame (16 sets at different κ-angles)
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_sigmaI/netI    0.039
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39646
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.463
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1318
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.87
_refine_diff_density_min         -1.74
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.95
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9035
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.95
_refine_ls_R_factor_all          0.031
_refine_ls_R_factor_gt           0.020
_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)+(0.018P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.038
_refine_ls_wR_factor_ref         0.039
_reflns_number_gt                7218
_reflns_number_total             9035
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb5458.cif
_cod_data_source_block           I
_cod_original_cell_volume        2001.90(19)
_cod_database_code               2226153
_cod_database_fobs_code          2226153
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W W1 -0.282538(14) 0.425012(14) 0.091913(8) 0.01414(4) Uani d . 1 . .
W W2 0.204122(15) 0.964916(14) 0.386429(9) 0.02111(4) Uani d . 1 . .
W W3 0.0000 0.0000 0.0000 0.02888(6) Uani d S 1 . .
Sn Sn1 -0.12400(2) 0.43967(2) 0.226266(13) 0.01384(5) Uani d . 1 A .
Sn Sn2 0.17113(2) 0.72211(2) 0.335720(13) 0.01364(5) Uani d . 1 A .
O O11 -0.0388(2) 0.6118(2) 0.33287(13) 0.0172(5) Uani d . 1 . .
O O17 -0.0577(3) 0.3220(2) 0.24211(15) 0.0270(6) Uani d . 1 . .
O O21 0.0794(2) 0.5636(2) 0.21882(13) 0.0159(5) Uani d . 1 . .
O O27 0.2066(2) 0.6510(2) 0.42020(14) 0.0225(6) Uani d . 1 . .
O O31 0.1889(3) 0.9430(3) 0.19202(17) 0.0344(7) Uani d . 1 . .
O O32 0.5203(3) 1.0749(3) 0.4149(2) 0.0577(10) Uani d . 1 . .
O O33 -0.1126(3) 0.8466(3) 0.3463(2) 0.0481(8) Uani d . 1 . .
O O34 0.1939(3) 0.9427(3) 0.56971(17) 0.0458(9) Uani d . 1 . .
O O41 -0.4503(3) 0.4212(3) -0.06435(16) 0.0363(7) Uani d . 1 . .
O O42 -0.4920(3) 0.1343(3) 0.04587(17) 0.0441(8) Uani d . 1 . .
O O43 -0.0948(3) 0.3502(3) -0.02380(16) 0.0328(7) Uani d . 1 . .
O O44 -0.4392(3) 0.5231(3) 0.22452(17) 0.0350(7) Uani d . 1 . .
O O45 -0.0934(3) 0.7209(3) 0.13766(19) 0.0456(8) Uani d . 1 . .
O O1W -0.2172(3) 0.0976(3) 0.0011(2) 0.0499(8) Uani d . 1 . .
O O2W 0.2380(4) 0.2807(3) 0.0516(2) 0.0713(12) Uani d . 1 . .
O O3W -0.0041(3) 0.0494(4) 0.1977(2) 0.0575(10) Uani d . 1 . .
N N14 -0.2180(3) 0.3899(3) 0.34934(17) 0.0173(6) Uani d . 1 . .
N N24 0.3492(3) 0.6808(3) 0.29092(16) 0.0150(6) Uani d . 1 . .
C C12 -0.0998(4) 0.6237(3) 0.4054(2) 0.0210(8) Uani d . 1 A .
H H12A -0.1826 0.6285 0.3915 0.025 Uiso calc R 1 . .
H H12B -0.0382 0.7023 0.4549 0.025 Uiso calc R 1 . .
C C13 -0.1313(3) 0.5090(4) 0.4276(2) 0.0208(8) Uani d . 1 A .
H H13A -0.1787 0.5120 0.4755 0.025 Uiso calc R 1 . .
H H13B -0.0476 0.5084 0.4462 0.025 Uiso calc R 1 . .
C C15 -0.1904(4) 0.2831(4) 0.3487(2) 0.0275(9) Uani d . 1 A .
H H15A -0.2646 0.2009 0.3089 0.033 Uiso calc R 1 . .
H H15B -0.1842 0.2809 0.4070 0.033 Uiso calc R 1 . .
C C16 -0.0601(4) 0.3013(4) 0.3201(2) 0.0304(9) Uani d . 1 A .
H H16A 0.0156 0.3752 0.3655 0.037 Uiso calc R 1 . .
H H16B -0.0490 0.2248 0.3124 0.037 Uiso calc R 1 . .
C C22 0.1591(3) 0.5150(3) 0.1702(2) 0.0187(8) Uani d . 1 A .
H H22A 0.1856 0.5545 0.1273 0.022 Uiso calc R 1 . .
H H22B 0.1058 0.4217 0.1391 0.022 Uiso calc R 1 . .
C C23 0.2809(3) 0.5439(3) 0.2290(2) 0.0195(8) Uani d . 1 A .
H H23A 0.3436 0.5269 0.1945 0.023 Uiso calc R 1 . .
H H23B 0.2555 0.4873 0.2617 0.023 Uiso calc R 1 . .
C C25 0.4201(4) 0.6963(4) 0.3742(2) 0.0229(8) Uani d . 1 A .
H H25A 0.4738 0.7881 0.4102 0.027 Uiso calc R 1 . .
H H25B 0.4814 0.6587 0.3632 0.027 Uiso calc R 1 . .
C C26 0.3187(4) 0.6303(4) 0.4220(2) 0.0242(9) Uani d . 1 A .
H H26A 0.2883 0.5375 0.3961 0.029 Uiso calc R 1 . .
H H26B 0.3639 0.6612 0.4827 0.029 Uiso calc R 1 . .
C C31 0.1962(4) 0.9539(4) 0.2626(2) 0.0242(8) Uani d . 1 A .
C C32 0.4076(4) 1.0356(4) 0.4052(2) 0.0343(10) Uani d . 1 A .
C C33 0.0011(4) 0.8895(4) 0.3611(2) 0.0291(9) Uani d . 1 A .
C C34 0.2003(4) 0.9537(4) 0.5052(2) 0.0305(10) Uani d . 1 A .
C C35 0.2013(8) 1.1351(9) 0.4227(5) 0.0224(13) Uani d PU 0.50 A 1
O O35 0.2001(6) 1.2300(6) 0.4454(4) 0.0326(11) Uani d PU 0.50 A 1
C C35' 0.2389(9) 1.1409(9) 0.4413(5) 0.0224(13) Uani d P 0.50 A 2
O O35' 0.2527(6) 1.2454(6) 0.4726(4) 0.0326(11) Uani d P 0.50 A 2
C C41 -0.3904(4) 0.4216(3) -0.0074(2) 0.0206(8) Uani d . 1 . .
C C42 -0.4151(4) 0.2378(4) 0.0629(2) 0.0246(9) Uani d . 1 . .
C C43 -0.1640(4) 0.3754(3) 0.0168(2) 0.0197(8) Uani d . 1 . .
C C44 -0.3857(4) 0.4845(4) 0.1755(2) 0.0212(8) Uani d . 1 . .
C C45 -0.1578(4) 0.6146(4) 0.1211(2) 0.0249(9) Uani d . 1 . .
C C50 0.4344(3) 0.7664(3) 0.25168(19) 0.0164(7) Uani d . 1 A .
C C51 0.5718(3) 0.8100(4) 0.2657(2) 0.0225(8) Uani d . 1 . .
H H51A 0.6129 0.7849 0.3016 0.027 Uiso calc R 1 A .
C C52 0.6483(4) 0.8903(4) 0.2268(2) 0.0304(10) Uani d . 1 A .
H H52A 0.7422 0.9209 0.2370 0.037 Uiso calc R 1 . .
C C53 0.5899(4) 0.9265(4) 0.1735(2) 0.0305(10) Uani d . 1 . .
H H53A 0.6432 0.9809 0.1467 0.037 Uiso calc R 1 A .
C C54 0.4533(4) 0.8831(4) 0.1593(2) 0.0255(9) Uani d . 1 A .
H H54A 0.4124 0.9080 0.1231 0.031 Uiso calc R 1 . .
C C55 0.3757(4) 0.8024(3) 0.1985(2) 0.0186(8) Uani d . 1 . .
H H55A 0.2819 0.7720 0.1884 0.022 Uiso calc R 1 A .
C C60 -0.3583(4) 0.3562(3) 0.3345(2) 0.0204(8) Uani d . 1 A .
C C61 -0.4104(4) 0.4260(4) 0.3887(2) 0.0210(8) Uani d . 1 . .
H H61A -0.3540 0.4971 0.4394 0.025 Uiso calc R 1 A .
C C62 -0.5461(4) 0.3915(4) 0.3686(3) 0.0318(10) Uani d . 1 A .
H H62A -0.5816 0.4382 0.4067 0.038 Uiso calc R 1 . .
C C63 -0.6283(4) 0.2915(4) 0.2949(3) 0.0378(11) Uani d . 1 . .
H H63A -0.7201 0.2693 0.2814 0.045 Uiso calc R 1 A .
C C64 -0.5764(4) 0.2235(4) 0.2402(3) 0.0361(11) Uani d . 1 A .
H H64A -0.6326 0.1548 0.1885 0.043 Uiso calc R 1 . .
C C65 -0.4425(4) 0.2545(4) 0.2601(2) 0.0253(9) Uani d . 1 . .
H H65A -0.4085 0.2056 0.2225 0.030 Uiso calc R 1 A .
C C1W -0.1393(4) 0.0640(4) -0.0008(3) 0.0347(10) Uani d . 1 . .
C C3W -0.0019(4) 0.0314(5) 0.1270(3) 0.0398(11) Uani d . 1 . .
C C2W 0.1544(5) 0.1819(5) 0.0329(3) 0.0454(12) Uani d . 1 . .
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'
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'
W W -0.8490 6.8722 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C41 W1 C44 . . 92.39(14) ?
C41 W1 C43 . . 91.82(14) ?
C44 W1 C43 . . 174.81(14) ?
C41 W1 C42 . . 88.78(15) ?
C44 W1 C42 . . 91.70(14) ?
C43 W1 C42 . . 91.42(14) ?
C41 W1 C45 . . 89.43(15) ?
C44 W1 C45 . . 86.05(14) ?
C43 W1 C45 . . 90.96(14) ?
C42 W1 C45 . . 177.07(16) ?
C41 W1 Sn1 . . 176.98(10) ?
C44 W1 Sn1 . . 88.91(10) ?
C43 W1 Sn1 . . 86.74(10) ?
C42 W1 Sn1 . . 93.90(11) ?
C45 W1 Sn1 . . 87.94(11) ?
C35' W2 C31 . . 98.6(3) ?
C35' W2 C35 . . 13.6(3) ?
C31 W2 C35 . . 90.4(3) ?
C35' W2 C33 . . 95.2(3) ?
C31 W2 C33 . . 87.69(15) ?
C35 W2 C33 . . 84.0(3) ?
C35' W2 C34 . . 87.6(3) ?
C31 W2 C34 . . 173.43(15) ?
C35 W2 C34 . . 95.2(3) ?
C33 W2 C34 . . 89.53(15) ?
C35' W2 C32 . . 86.6(3) ?
C31 W2 C32 . . 89.70(15) ?
C35 W2 C32 . . 97.5(3) ?
C33 W2 C32 . . 177.00(15) ?
C34 W2 C32 . . 92.91(16) ?
C35' W2 Sn2 . . 170.6(2) ?
C31 W2 Sn2 . . 90.23(11) ?
C35 W2 Sn2 . . 172.2(2) ?
C33 W2 Sn2 . . 88.23(11) ?
C34 W2 Sn2 . . 83.74(11) ?
C32 W2 Sn2 . . 90.29(12) ?
C3W W3 C3W 2 . 180.0(3) ?
C3W W3 C1W 2 2 87.14(16) ?
C3W W3 C1W . 2 92.86(16) ?
C3W W3 C1W 2 . 92.86(16) ?
C3W W3 C1W . . 87.14(16) ?
C1W W3 C1W 2 . 180.0(3) ?
C3W W3 C2W 2 . 89.36(18) ?
C3W W3 C2W . . 90.64(18) ?
C1W W3 C2W 2 . 88.71(19) ?
C1W W3 C2W . . 91.29(19) ?
C3W W3 C2W 2 2 90.64(18) ?
C3W W3 C2W . 2 89.36(18) ?
C1W W3 C2W 2 2 91.29(19) ?
C1W W3 C2W . 2 88.71(19) ?
C2W W3 C2W . 2 180.0(3) ?
O17 Sn1 O11 . . 110.71(10) ?
O17 Sn1 O21 . . 88.04(10) ?
O11 Sn1 O21 . . 69.82(8) ?
O17 Sn1 N14 . . 76.52(9) ?
O11 Sn1 N14 . . 73.42(9) ?
O21 Sn1 N14 . . 131.57(8) ?
O17 Sn1 W1 . . 132.90(7) ?
O11 Sn1 W1 . . 116.19(7) ?
O21 Sn1 W1 . . 103.68(6) ?
N14 Sn1 W1 . . 120.53(7) ?
O27 Sn2 O21 . . 104.24(10) ?
O27 Sn2 O11 . . 85.86(9) ?
O21 Sn2 O11 . . 70.16(8) ?
O27 Sn2 N24 . . 78.41(9) ?
O21 Sn2 N24 . . 75.71(9) ?
O11 Sn2 N24 . . 137.35(9) ?
O27 Sn2 W2 . . 122.15(7) ?
O21 Sn2 W2 . . 132.75(7) ?
O11 Sn2 W2 . . 102.58(6) ?
N24 Sn2 W2 . . 119.42(7) ?
C12 O11 Sn1 . . 119.87(19) ?
C12 O11 Sn2 . . 125.65(19) ?
Sn1 O11 Sn2 . . 110.16(9) ?
C16 O17 Sn1 . . 119.0(2) ?
C22 O21 Sn2 . . 119.90(18) ?
C22 O21 Sn1 . . 122.88(19) ?
Sn2 O21 Sn1 . . 108.63(9) ?
C26 O27 Sn2 . . 118.74(19) ?
C60 N14 C15 . . 114.3(3) ?
C60 N14 C13 . . 114.8(3) ?
C15 N14 C13 . . 110.5(3) ?
C60 N14 Sn1 . . 109.40(19) ?
C15 N14 Sn1 . . 102.40(19) ?
C13 N14 Sn1 . . 104.16(18) ?
C50 N24 C25 . . 113.4(3) ?
C50 N24 C23 . . 111.8(2) ?
C25 N24 C23 . . 111.7(3) ?
C50 N24 Sn2 . . 114.0(2) ?
C25 N24 Sn2 . . 100.56(19) ?
C23 N24 Sn2 . . 104.57(19) ?
O11 C12 C13 . . 108.0(3) ?
O11 C12 H12A . . 110.1 ?
C13 C12 H12A . . 110.1 ?
O11 C12 H12B . . 110.1 ?
C13 C12 H12B . . 110.1 ?
H12A C12 H12B . . 108.4 ?
C12 C13 N14 . . 109.1(3) ?
C12 C13 H13A . . 109.9 ?
N14 C13 H13A . . 109.9 ?
C12 C13 H13B . . 109.9 ?
N14 C13 H13B . . 109.9 ?
H13A C13 H13B . . 108.3 ?
N14 C15 C16 . . 110.1(3) ?
N14 C15 H15A . . 109.6 ?
C16 C15 H15A . . 109.6 ?
N14 C15 H15B . . 109.6 ?
C16 C15 H15B . . 109.6 ?
H15A C15 H15B . . 108.2 ?
O17 C16 C15 . . 111.6(3) ?
O17 C16 H16A . . 109.3 ?
C15 C16 H16A . . 109.3 ?
O17 C16 H16B . . 109.3 ?
C15 C16 H16B . . 109.3 ?
H16A C16 H16B . . 108.0 ?
O21 C22 C23 . . 110.2(3) ?
O21 C22 H22A . . 109.6 ?
C23 C22 H22A . . 109.6 ?
O21 C22 H22B . . 109.6 ?
C23 C22 H22B . . 109.6 ?
H22A C22 H22B . . 108.1 ?
C22 C23 N24 . . 111.3(3) ?
C22 C23 H23A . . 109.4 ?
N24 C23 H23A . . 109.4 ?
C22 C23 H23B . . 109.4 ?
N24 C23 H23B . . 109.4 ?
H23A C23 H23B . . 108.0 ?
N24 C25 C26 . . 110.1(3) ?
N24 C25 H25A . . 109.6 ?
C26 C25 H25A . . 109.6 ?
N24 C25 H25B . . 109.6 ?
C26 C25 H25B . . 109.6 ?
H25A C25 H25B . . 108.2 ?
O27 C26 C25 . . 113.9(3) ?
O27 C26 H26A . . 108.8 ?
C25 C26 H26A . . 108.8 ?
O27 C26 H26B . . 108.8 ?
C25 C26 H26B . . 108.8 ?
H26A C26 H26B . . 107.7 ?
O31 C31 W2 . . 177.5(3) ?
O32 C32 W2 . . 179.3(4) ?
O33 C33 W2 . . 179.4(4) ?
O34 C34 W2 . . 177.3(3) ?
O35 C35 W2 . . 177.9(8) ?
O35' C35' W2 . . 176.3(8) ?
O41 C41 W1 . . 178.9(3) ?
O42 C42 W1 . . 177.8(4) ?
O43 C43 W1 . . 178.3(3) ?
O44 C44 W1 . . 177.1(3) ?
O45 C45 W1 . . 176.8(4) ?
C55 C50 C51 . . 119.6(3) ?
C55 C50 N24 . . 118.8(3) ?
C51 C50 N24 . . 121.6(3) ?
C52 C51 C50 . . 119.6(4) ?
C52 C51 H51A . . 120.2 ?
C50 C51 H51A . . 120.2 ?
C53 C52 C51 . . 120.9(4) ?
C53 C52 H52A . . 119.5 ?
C51 C52 H52A . . 119.5 ?
C52 C53 C54 . . 119.6(4) ?
C52 C53 H53A . . 120.2 ?
C54 C53 H53A . . 120.2 ?
C53 C54 C55 . . 119.7(4) ?
C53 C54 H54A . . 120.2 ?
C55 C54 H54A . . 120.2 ?
C50 C55 C54 . . 120.6(3) ?
C50 C55 H55A . . 119.7 ?
C54 C55 H55A . . 119.7 ?
C65 C60 C61 . . 118.7(3) ?
C65 C60 N14 . . 118.3(3) ?
C61 C60 N14 . . 122.8(3) ?
C60 C61 C62 . . 119.9(4) ?
C60 C61 H61A . . 120.0 ?
C62 C61 H61A . . 120.0 ?
C63 C62 C61 . . 121.0(4) ?
C63 C62 H62A . . 119.5 ?
C61 C62 H62A . . 119.5 ?
C62 C63 C64 . . 119.2(4) ?
C62 C63 H63A . . 120.4 ?
C64 C63 H63A . . 120.4 ?
C63 C64 C65 . . 120.7(4) ?
C63 C64 H64A . . 119.7 ?
C65 C64 H64A . . 119.7 ?
C60 C65 C64 . . 120.4(4) ?
C60 C65 H65A . . 119.8 ?
C64 C65 H65A . . 119.8 ?
O1W C1W W3 . . 177.5(4) ?
O3W C3W W3 . . 179.1(4) ?
O2W C2W W3 . . 179.2(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 C41 . 2.000(4) ?
W1 C44 . 2.035(4) ?
W1 C43 . 2.042(4) ?
W1 C42 . 2.046(4) ?
W1 C45 . 2.050(4) ?
W2 C35' . 1.947(10) ?
W2 C31 . 2.037(4) ?
W2 C35 . 2.038(10) ?
W2 C33 . 2.042(4) ?
W2 C34 . 2.049(4) ?
W2 C32 . 2.054(5) ?
W3 C3W 2 2.047(4) ?
W3 C3W . 2.047(4) ?
W3 C1W 2 2.059(5) ?
W3 C1W . 2.059(5) ?
W3 C2W . 2.064(5) ?
W3 C2W 2 2.064(5) ?
Sn1 W1 . 2.7274(3) y
Sn1 O11 . 2.091(2) y
Sn1 O17 . 2.001(3) y
Sn1 O21 . 2.201(2) y
Sn1 N14 . 2.507(3) y
Sn2 W2 . 2.7334(3) y
Sn2 O11 . 2.173(2) y
Sn2 O21 . 2.104(2) y
Sn2 O27 . 2.011(2) y
Sn2 N24 . 2.391(3) y
O11 C12 . 1.430(3) ?
O17 C16 . 1.416(4) ?
O21 C22 . 1.443(4) ?
O27 C26 . 1.405(4) ?
O31 C31 . 1.146(4) ?
O32 C32 . 1.138(5) ?
O33 C33 . 1.142(5) ?
O34 C34 . 1.138(4) ?
O41 C41 . 1.146(4) ?
O42 C42 . 1.139(4) ?
O43 C43 . 1.145(4) ?
O44 C44 . 1.152(4) ?
O45 C45 . 1.139(4) ?
O1W C1W . 1.129(5) ?
O2W C2W . 1.117(5) ?
O3W C3W . 1.140(5) ?
N14 C60 . 1.448(4) ?
N14 C15 . 1.498(5) ?
N14 C13 . 1.513(4) ?
N24 C50 . 1.467(4) ?
N24 C25 . 1.493(4) ?
N24 C23 . 1.506(4) ?
C12 C13 . 1.500(5) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C15 C16 . 1.524(5) ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C22 C23 . 1.494(5) ?
C22 H22A . 0.9900 ?
C22 H22B . 0.9900 ?
C23 H23A . 0.9900 ?
C23 H23B . 0.9900 ?
C25 C26 . 1.535(5) ?
C25 H25A . 0.9900 ?
C25 H25B . 0.9900 ?
C26 H26A . 0.9900 ?
C26 H26B . 0.9900 ?
C35 O35 . 1.134(11) ?
C35' O35' . 1.181(11) ?
C50 C55 . 1.381(5) ?
C50 C51 . 1.393(5) ?
C51 C52 . 1.387(5) ?
C51 H51A . 0.9500 ?
C52 C53 . 1.383(6) ?
C52 H52A . 0.9500 ?
C53 C54 . 1.384(5) ?
C53 H53A . 0.9500 ?
C54 C55 . 1.399(5) ?
C54 H54A . 0.9500 ?
C55 H55A . 0.9500 ?
C60 C65 . 1.387(5) ?
C60 C61 . 1.389(5) ?
C61 C62 . 1.401(5) ?
C61 H61A . 0.9500 ?
C62 C63 . 1.367(6) ?
C62 H62A . 0.9500 ?
C63 C64 . 1.378(6) ?
C63 H63A . 0.9500 ?
C64 C65 . 1.391(6) ?
C64 H64A . 0.9500 ?
C65 H65A . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C23 H23a O44 1_655 0.99 2.52 3.301(5) 136
C64 H64a O31 1_445 0.95 2.58 3.174(6) 121
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C41 W1 Sn1 O17 . . . . -110.4(19) ?
C44 W1 Sn1 O17 . . . . 134.13(14) ?
C43 W1 Sn1 O17 . . . . -48.71(14) ?
C42 W1 Sn1 O17 . . . . 42.50(14) ?
C45 W1 Sn1 O17 . . . . -139.78(14) ?
C41 W1 Sn1 O11 . . . . 63.9(19) ?
C44 W1 Sn1 O11 . . . . -51.63(12) ?
C43 W1 Sn1 O11 . . . . 125.54(12) ?
C42 W1 Sn1 O11 . . . . -143.25(12) ?
C45 W1 Sn1 O11 . . . . 34.46(12) ?
C41 W1 Sn1 O21 . . . . -10.1(19) ?
C44 W1 Sn1 O21 . . . . -125.61(12) ?
C43 W1 Sn1 O21 . . . . 51.55(11) ?
C42 W1 Sn1 O21 . . . . 142.76(12) ?
C45 W1 Sn1 O21 . . . . -39.52(12) ?
C41 W1 Sn1 N14 . . . . 149.3(19) ?
C44 W1 Sn1 N14 . . . . 33.84(13) ?
C43 W1 Sn1 N14 . . . . -149.00(13) ?
C42 W1 Sn1 N14 . . . . -57.79(13) ?
C45 W1 Sn1 N14 . . . . 119.93(12) ?
C35' W2 Sn2 O27 . . . . 5.0(16) ?
C31 W2 Sn2 O27 . . . . 165.61(13) ?
C35 W2 Sn2 O27 . . . . -99.6(18) ?
C33 W2 Sn2 O27 . . . . -106.71(13) ?
C34 W2 Sn2 O27 . . . . -16.99(14) ?
C32 W2 Sn2 O27 . . . . 75.91(13) ?
C35' W2 Sn2 O21 . . . . 172.6(16) ?
C31 W2 Sn2 O21 . . . . -26.87(13) ?
C35 W2 Sn2 O21 . . . . 67.9(18) ?
C33 W2 Sn2 O21 . . . . 60.82(13) ?
C34 W2 Sn2 O21 . . . . 150.54(14) ?
C32 W2 Sn2 O21 . . . . -116.57(13) ?
C35' W2 Sn2 O11 . . . . 98.1(16) ?
C31 W2 Sn2 O11 . . . . -101.36(12) ?
C35 W2 Sn2 O11 . . . . -6.6(18) ?
C33 W2 Sn2 O11 . . . . -13.68(12) ?
C34 W2 Sn2 O11 . . . . 76.04(13) ?
C32 W2 Sn2 O11 . . . . 168.94(12) ?
C35' W2 Sn2 N24 . . . . -89.7(16) ?
C31 W2 Sn2 N24 . . . . 70.91(13) ?
C35 W2 Sn2 N24 . . . . 165.7(18) ?
C33 W2 Sn2 N24 . . . . 158.59(13) ?
C34 W2 Sn2 N24 . . . . -111.69(13) ?
C32 W2 Sn2 N24 . . . . -18.79(13) ?
O17 Sn1 O11 C12 . . . . -86.7(2) ?
O21 Sn1 O11 C12 . . . . -166.5(3) ?
N14 Sn1 O11 C12 . . . . -18.6(2) ?
W1 Sn1 O11 C12 . . . . 97.8(2) ?
O17 Sn1 O11 Sn2 . . . . 71.24(12) ?
O21 Sn1 O11 Sn2 . . . . -8.51(10) ?
N14 Sn1 O11 Sn2 . . . . 139.37(13) ?
W1 Sn1 O11 Sn2 . . . . -104.25(9) ?
O27 Sn2 O11 C12 . . . . 58.5(3) ?
O21 Sn2 O11 C12 . . . . 165.3(3) ?
N24 Sn2 O11 C12 . . . . 126.4(2) ?
W2 Sn2 O11 C12 . . . . -63.5(3) ?
O27 Sn2 O11 Sn1 . . . . -97.87(12) ?
O21 Sn2 O11 Sn1 . . . . 8.89(10) ?
N24 Sn2 O11 Sn1 . . . . -29.95(18) ?
W2 Sn2 O11 Sn1 . . . . 140.09(9) ?
O11 Sn1 O17 C16 . . . . 49.0(3) ?
O21 Sn1 O17 C16 . . . . 116.6(3) ?
N14 Sn1 O17 C16 . . . . -17.1(3) ?
W1 Sn1 O17 C16 . . . . -136.5(2) ?
O27 Sn2 O21 C22 . . . . -76.9(2) ?
O11 Sn2 O21 C22 . . . . -157.1(3) ?
N24 Sn2 O21 C22 . . . . -3.1(2) ?
W2 Sn2 O21 C22 . . . . 114.0(2) ?
O27 Sn2 O21 Sn1 . . . . 71.81(12) ?
O11 Sn2 O21 Sn1 . . . . -8.36(10) ?
N24 Sn2 O21 Sn1 . . . . 145.64(12) ?
W2 Sn2 O21 Sn1 . . . . -97.32(10) ?
O17 Sn1 O21 C22 . . . . 43.4(2) ?
O11 Sn1 O21 C22 . . . . 156.3(3) ?
N14 Sn1 O21 C22 . . . . 113.4(2) ?
W1 Sn1 O21 C22 . . . . -90.5(2) ?
O17 Sn1 O21 Sn2 . . . . -104.22(11) ?
O11 Sn1 O21 Sn2 . . . . 8.71(10) ?
N14 Sn1 O21 Sn2 . . . . -34.23(17) ?
W1 Sn1 O21 Sn2 . . . . 121.94(8) ?
O21 Sn2 O27 C26 . . . . 80.3(3) ?
O11 Sn2 O27 C26 . . . . 148.6(3) ?
N24 Sn2 O27 C26 . . . . 8.4(2) ?
W2 Sn2 O27 C26 . . . . -109.2(2) ?
O17 Sn1 N14 C60 . . . . -132.3(2) ?
O11 Sn1 N14 C60 . . . . 110.9(2) ?
O21 Sn1 N14 C60 . . . . 152.7(2) ?
W1 Sn1 N14 C60 . . . . -0.2(2) ?
O17 Sn1 N14 C15 . . . . -10.7(2) ?
O11 Sn1 N14 C15 . . . . -127.5(2) ?
O21 Sn1 N14 C15 . . . . -85.7(2) ?
W1 Sn1 N14 C15 . . . . 121.5(2) ?
O17 Sn1 N14 C13 . . . . 104.4(2) ?
O11 Sn1 N14 C13 . . . . -12.4(2) ?
O21 Sn1 N14 C13 . . . . 29.5(3) ?
W1 Sn1 N14 C13 . . . . -123.40(19) ?
O27 Sn2 N24 C50 . . . . -150.5(2) ?
O21 Sn2 N24 C50 . . . . 101.4(2) ?
O11 Sn2 N24 C50 . . . . 138.88(19) ?
W2 Sn2 N24 C50 . . . . -29.9(2) ?
O27 Sn2 N24 C25 . . . . -28.8(2) ?
O21 Sn2 N24 C25 . . . . -137.0(2) ?
O11 Sn2 N24 C25 . . . . -99.5(2) ?
W2 Sn2 N24 C25 . . . . 91.7(2) ?
O27 Sn2 N24 C23 . . . . 87.1(2) ?
O21 Sn2 N24 C23 . . . . -21.01(19) ?
O11 Sn2 N24 C23 . . . . 16.5(2) ?
W2 Sn2 N24 C23 . . . . -152.35(17) ?
Sn1 O11 C12 C13 . . . . 47.2(3) ?
Sn2 O11 C12 C13 . . . . -107.1(3) ?
O11 C12 C13 N14 . . . . -56.1(3) ?
C60 N14 C13 C12 . . . . -80.8(3) ?
C15 N14 C13 C12 . . . . 148.2(3) ?
Sn1 N14 C13 C12 . . . . 38.9(3) ?
C60 N14 C15 C16 . . . . 151.8(3) ?
C13 N14 C15 C16 . . . . -76.8(3) ?
Sn1 N14 C15 C16 . . . . 33.6(3) ?
Sn1 O17 C16 C15 . . . . 43.3(4) ?
N14 C15 C16 O17 . . . . -51.5(4) ?
Sn2 O21 C22 C23 . . . . 27.6(4) ?
Sn1 O21 C22 C23 . . . . -116.6(3) ?
O21 C22 C23 N24 . . . . -47.2(4) ?
C50 N24 C23 C22 . . . . -81.7(3) ?
C25 N24 C23 C22 . . . . 150.0(3) ?
Sn2 N24 C23 C22 . . . . 42.1(3) ?
C50 N24 C25 C26 . . . . 165.6(3) ?
C23 N24 C25 C26 . . . . -67.0(4) ?
Sn2 N24 C25 C26 . . . . 43.5(3) ?
Sn2 O27 C26 C25 . . . . 14.6(4) ?
N24 C25 C26 O27 . . . . -42.8(4) ?
C25 N24 C50 C55 . . . . -152.8(3) ?
C23 N24 C50 C55 . . . . 79.9(4) ?
Sn2 N24 C50 C55 . . . . -38.5(3) ?
C25 N24 C50 C51 . . . . 28.4(4) ?
C23 N24 C50 C51 . . . . -99.0(4) ?
Sn2 N24 C50 C51 . . . . 142.7(3) ?
C55 C50 C51 C52 . . . . 0.8(5) ?
N24 C50 C51 C52 . . . . 179.6(3) ?
C50 C51 C52 C53 . . . . -0.8(6) ?
C51 C52 C53 C54 . . . . 0.6(6) ?
C52 C53 C54 C55 . . . . -0.5(6) ?
C51 C50 C55 C54 . . . . -0.7(5) ?
N24 C50 C55 C54 . . . . -179.5(3) ?
C53 C54 C55 C50 . . . . 0.5(5) ?
C15 N14 C60 C65 . . . . -56.2(4) ?
C13 N14 C60 C65 . . . . 174.6(3) ?
Sn1 N14 C60 C65 . . . . 58.0(3) ?
C15 N14 C60 C61 . . . . 127.9(3) ?
C13 N14 C60 C61 . . . . -1.3(5) ?
Sn1 N14 C60 C61 . . . . -117.9(3) ?
C65 C60 C61 C62 . . . . 1.3(5) ?
N14 C60 C61 C62 . . . . 177.2(3) ?
C60 C61 C62 C63 . . . . -1.7(6) ?
C61 C62 C63 C64 . . . . 0.6(6) ?
C62 C63 C64 C65 . . . . 0.9(6) ?
C61 C60 C65 C64 . . . . 0.2(5) ?
N14 C60 C65 C64 . . . . -175.9(3) ?
C63 C64 C65 C60 . . . . -1.3(6) ?
