Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2006
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_cambridge 0222
_journal_year ?
_journal_volume ?
_journal_page_first ?
loop_
_publ_author_name
_publ_author_address
A.Deak
; Institute of Structural Chemistry,
Chemical Research Center,
Hungarian Academy of Sciences,
P.O. Box 17,
H-1525 Budapest,
Hungary
;
P.Kiraly
; Institute of Structural Chemistry,
Chemical Research Center,
Hungarian Academy of Sciences,
P.O. Box 17,
H-1525 Budapest,
Hungary
;
G.Tarkanyi
; Institute of Structural Chemistry,
Chemical Research Center,
Hungarian Academy of Sciences,
P.O. Box 17,
H-1525 Budapest,
Hungary
;
_publ_contact_author_address
; Institute of Structural Chemistry
Chemical Research Center,Hungarian Academy of Sciences,
H-1525-Budapest,
P.O.Box 17,
Hungary
;
_publ_contact_author_email deak@chemres.hu
_publ_contact_author_fax 00-36-1-438-4141/201
_publ_contact_author_phone 00-36-1-325-7547
_publ_contact_author_name 'Dr. Andrea Deak'
_publ_section_title
;
Preparation and Structural Characterization of Trimethyltin(IV)-Tropolonate.
Investigation of a Rare Methyl-Migrational Dismutation in the Liquid-,
Solid- and Molten-State.
;
data_complex1
_database_code_depnum_ccdc_archive 'CCDC 621188'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
trimethyltin(IV)-tropolonate
;
_chemical_name_common trimethyltin(IV)-tropolonate
_chemical_melting_point ?
_chemical_formula_moiety 'C10 H14 O2 Sn'
_chemical_formula_sum 'C10 H14 O2 Sn'
_chemical_formula_weight 284.90
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'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
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'
_cell_length_a 10.572(6)
_cell_length_b 8.576(4)
_cell_length_c 12.235(7)
_cell_angle_alpha 90.00
_cell_angle_beta 99.83(2)
_cell_angle_gamma 90.00
_cell_volume 1093.0(10)
_cell_formula_units_Z 4
_cell_measurement_temperature 93(2)
_cell_measurement_reflns_used 8053
_cell_measurement_theta_min 3.08
_cell_measurement_theta_max 27.45
_exptl_crystal_description block
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.17
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.731
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 560
_exptl_absorpt_coefficient_mu 2.305
_exptl_absorpt_correction_type empirical
_exptl_absorpt_correction_T_min 0.5283
_exptl_absorpt_correction_T_max 0.6744
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 93(2)
_diffrn_radiation_wavelength 0.71070
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'R Axis Rapid'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 9308
_diffrn_reflns_av_R_equivalents 0.0365
_diffrn_reflns_av_sigmaI/netI 0.0267
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 3.08
_diffrn_reflns_theta_max 27.46
_reflns_number_total 2493
_reflns_number_gt 2195
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 2003)'
_computing_publication_material 'WinGX (Farrugia, 1999), PLATON (Spek, 2003)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+0.0718P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2493
_refine_ls_number_parameters 121
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0290
_refine_ls_R_factor_gt 0.0238
_refine_ls_wR_factor_ref 0.0712
_refine_ls_wR_factor_gt 0.0691
_refine_ls_goodness_of_fit_ref 1.258
_refine_ls_restrained_S_all 1.258
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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 0.335278(18) 0.21004(2) 0.017742(16) 0.01502(9) Uani 1 1 d . . .
O1A O 0.3514(2) 0.0727(2) -0.12458(17) 0.0193(4) Uani 1 1 d . . .
O2A O 0.16971(19) 0.0288(3) -0.01463(16) 0.0190(5) Uani 1 1 d . . .
C1 C 0.5247(3) 0.2914(4) 0.0020(3) 0.0215(7) Uani 1 1 d . . .
H1A H 0.5789 0.2021 -0.0091 0.032 Uiso 1 1 calc R . .
H1B H 0.5625 0.3470 0.0697 0.032 Uiso 1 1 calc R . .
H1C H 0.5185 0.3620 -0.0617 0.032 Uiso 1 1 calc R . .
C2 C 0.1973(3) 0.3889(4) -0.0334(3) 0.0232(7) Uani 1 1 d . . .
H2A H 0.1591 0.3731 -0.1114 0.035 Uiso 1 1 calc R . .
H2B H 0.2396 0.4909 -0.0247 0.035 Uiso 1 1 calc R . .
H2C H 0.1299 0.3848 0.0125 0.035 Uiso 1 1 calc R . .
C3 C 0.3533(3) 0.1217(4) 0.1833(3) 0.0247(7) Uani 1 1 d . . .
H3A H 0.2679 0.0996 0.2003 0.037 Uiso 1 1 calc R . .
H3B H 0.3962 0.1995 0.2356 0.037 Uiso 1 1 calc R . .
H3C H 0.4043 0.0257 0.1898 0.037 Uiso 1 1 calc R . .
C1A C 0.2674(3) -0.0316(3) -0.1641(2) 0.0144(6) Uani 1 1 d . . .
C2A C 0.1643(3) -0.0578(3) -0.0996(2) 0.0150(6) Uani 1 1 d . . .
C3A C 0.0658(3) -0.1688(4) -0.1236(3) 0.0189(6) Uani 1 1 d . . .
H3A1 H 0.0078 -0.1711 -0.0723 0.023 Uiso 1 1 calc R . .
C4A C 0.0388(3) -0.2756(4) -0.2096(3) 0.0211(6) Uani 1 1 d . . .
H4A H -0.0338 -0.3400 -0.2074 0.025 Uiso 1 1 calc R . .
C5A C 0.1026(3) -0.3025(4) -0.2989(3) 0.0224(7) Uani 1 1 d . . .
H5A H 0.0694 -0.3833 -0.3488 0.027 Uiso 1 1 calc R . .
C6A C 0.2079(3) -0.2242(4) -0.3219(3) 0.0215(7) Uani 1 1 d . . .
H6A H 0.2355 -0.2548 -0.3886 0.026 Uiso 1 1 calc R . .
C7A C 0.2813(3) -0.1064(4) -0.2625(2) 0.0197(6) Uani 1 1 d . . .
H7A H 0.3522 -0.0717 -0.2944 0.024 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sn1 0.01627(12) 0.01512(12) 0.01436(12) -0.00152(8) 0.00461(8) -0.00167(7)
O1A 0.0205(11) 0.0187(10) 0.0211(11) -0.0041(9) 0.0099(9) -0.0041(8)
O2A 0.0229(11) 0.0201(11) 0.0156(10) -0.0044(9) 0.0081(9) -0.0024(8)
C1 0.0206(16) 0.0220(16) 0.0223(16) 0.0001(13) 0.0048(13) -0.0055(12)
C2 0.0246(16) 0.0174(15) 0.0279(17) 0.0005(14) 0.0049(13) 0.0020(12)
C3 0.0283(17) 0.0291(17) 0.0164(14) -0.0005(14) 0.0026(12) -0.0054(14)
C1A 0.0143(13) 0.0134(13) 0.0155(13) 0.0031(12) 0.0025(11) 0.0027(11)
C2A 0.0165(13) 0.0149(13) 0.0141(13) 0.0030(12) 0.0043(11) 0.0046(11)
C3A 0.0211(15) 0.0197(14) 0.0176(14) 0.0000(12) 0.0083(12) -0.0017(12)
C4A 0.0183(15) 0.0217(16) 0.0236(16) -0.0027(13) 0.0043(12) -0.0043(12)
C5A 0.0245(17) 0.0211(15) 0.0215(16) -0.0058(13) 0.0034(13) -0.0014(12)
C6A 0.0235(16) 0.0251(16) 0.0165(15) -0.0047(13) 0.0051(12) 0.0043(13)
C7A 0.0200(15) 0.0225(15) 0.0184(14) -0.0029(13) 0.0088(12) -0.0015(12)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O1A 2.133(2) . ?
Sn1 C2 2.136(3) . ?
Sn1 C3 2.140(3) . ?
Sn1 C1 2.160(3) . ?
Sn1 O2A 2.324(2) . ?
O1A C1A 1.295(3) . ?
O2A C2A 1.271(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C1A C7A 1.394(4) . ?
C1A C2A 1.467(4) . ?
C2A C3A 1.405(4) . ?
C3A C4A 1.386(4) . ?
C3A H3A1 0.9500 . ?
C4A C5A 1.398(5) . ?
C4A H4A 0.9500 . ?
C5A C6A 1.370(5) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.400(4) . ?
C6A H6A 0.9500 . ?
C7A H7A 0.9500 . ?
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
O1A Sn1 C2 107.66(11) . . ?
O1A Sn1 C3 124.78(12) . . ?
C2 Sn1 C3 118.52(13) . . ?
O1A Sn1 C1 84.33(11) . . ?
C2 Sn1 C1 109.81(13) . . ?
C3 Sn1 C1 105.33(13) . . ?
O1A Sn1 O2A 69.77(8) . . ?
C2 Sn1 O2A 88.49(12) . . ?
C3 Sn1 O2A 82.39(10) . . ?
C1 Sn1 O2A 152.09(10) . . ?
C1A O1A Sn1 122.73(18) . . ?
C2A O2A Sn1 117.22(18) . . ?
Sn1 C1 H1A 109.5 . . ?
Sn1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Sn1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Sn1 C2 H2A 109.5 . . ?
Sn1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Sn1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Sn1 C3 H3A 109.5 . . ?
Sn1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Sn1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O1A C1A C7A 118.2(3) . . ?
O1A C1A C2A 115.5(2) . . ?
C7A C1A C2A 126.3(3) . . ?
O2A C2A C3A 119.7(3) . . ?
O2A C2A C1A 114.6(3) . . ?
C3A C2A C1A 125.7(3) . . ?
C4A C3A C2A 131.0(3) . . ?
C4A C3A H3A1 114.5 . . ?
C2A C3A H3A1 114.5 . . ?
C3A C4A C5A 129.6(3) . . ?
C3A C4A H4A 115.2 . . ?
C5A C4A H4A 115.2 . . ?
C6A C5A C4A 126.7(3) . . ?
C6A C5A H5A 116.7 . . ?
C4A C5A H5A 116.7 . . ?
C5A C6A C7A 130.2(3) . . ?
C5A C6A H6A 114.9 . . ?
C7A C6A H6A 114.9 . . ?
C1A C7A C6A 130.5(3) . . ?
C1A C7A H7A 114.8 . . ?
C6A C7A H7A 114.8 . . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 Sn1 O1A C1A -77.9(2) . . . . ?
C3 Sn1 O1A C1A 68.3(2) . . . . ?
C1 Sn1 O1A C1A 173.1(2) . . . . ?
O2A Sn1 O1A C1A 3.7(2) . . . . ?
O1A Sn1 O2A C2A -2.50(19) . . . . ?
C2 Sn1 O2A C2A 107.0(2) . . . . ?
C3 Sn1 O2A C2A -134.0(2) . . . . ?
C1 Sn1 O2A C2A -25.5(3) . . . . ?
Sn1 O1A C1A C7A 175.0(2) . . . . ?
Sn1 O1A C1A C2A -4.3(3) . . . . ?
Sn1 O2A C2A C3A -179.6(2) . . . . ?
Sn1 O2A C2A C1A 1.3(3) . . . . ?
O1A C1A C2A O2A 1.7(4) . . . . ?
C7A C1A C2A O2A -177.5(3) . . . . ?
O1A C1A C2A C3A -177.3(3) . . . . ?
C7A C1A C2A C3A 3.4(5) . . . . ?
O2A C2A C3A C4A 180.0(3) . . . . ?
C1A C2A C3A C4A -1.0(5) . . . . ?
C2A C3A C4A C5A -0.7(6) . . . . ?
C3A C4A C5A C6A -1.1(6) . . . . ?
C4A C5A C6A C7A 3.3(6) . . . . ?
O1A C1A C7A C6A 178.4(3) . . . . ?
C2A C1A C7A C6A -2.4(5) . . . . ?
C5A C6A C7A C1A -1.6(6) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C3 H3B O1A 0.98 2.69 3.523(4) 142.9 4_566
C1 H1A C1A 0.98 2.85 3.499(4) 124.8 3_655
C3A H3A1 O2A 0.95 2.61 3.456(4) 148.1 3
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 27.46
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.570
_refine_diff_density_min -0.725
_refine_diff_density_rms 0.155
# Attachment 'complex2.cif'
data_complex2
_database_code_depnum_ccdc_archive 'CCDC 621189'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
dimethyltin(IV)-bis(tropolonate)
;
_chemical_name_common dimethyltin(IV)-bis(tropolonate)
_chemical_melting_point ?
_chemical_formula_moiety 'C16 H16 O4 Sn'
_chemical_formula_sum 'C16 H16 O4 Sn'
_chemical_formula_weight 390.98
_chemical_compound_source
'obtained from the melt, from Me3Sn(trop) dismutation'
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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
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'
_cell_length_a 10.732(4)
_cell_length_b 14.192(6)
_cell_length_c 10.561(4)
_cell_angle_alpha 90.00
_cell_angle_beta 98.24(4)
_cell_angle_gamma 90.00
_cell_volume 1591.9(11)
_cell_formula_units_Z 4
_cell_measurement_temperature 295(2)
_cell_measurement_reflns_used 11252
_cell_measurement_theta_min 3.14
_cell_measurement_theta_max 27.67
_exptl_crystal_description yellowish
_exptl_crystal_colour chunk
_exptl_crystal_size_max 0.41
_exptl_crystal_size_mid 0.41
_exptl_crystal_size_min 0.23
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.631
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 776
_exptl_absorpt_coefficient_mu 1.617
_exptl_absorpt_correction_type empirical
_exptl_absorpt_correction_T_min 0.5459
_exptl_absorpt_correction_T_max 0.6933
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 295(2)
_diffrn_radiation_wavelength 0.71070
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'R Axis Rapid'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 10055
_diffrn_reflns_av_R_equivalents 0.0310
_diffrn_reflns_av_sigmaI/netI 0.0260
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_theta_min 3.26
_diffrn_reflns_theta_max 25.01
_reflns_number_total 2750
_reflns_number_gt 2242
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 2003)'
_computing_publication_material 'WinGX (Farrugia, 1999), PLATON (Spek, 2003)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+1.0454P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2750
_refine_ls_number_parameters 192
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0457
_refine_ls_R_factor_gt 0.0329
_refine_ls_wR_factor_ref 0.1223
_refine_ls_wR_factor_gt 0.0943
_refine_ls_goodness_of_fit_ref 1.245
_refine_ls_restrained_S_all 1.245
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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 0.27408(4) -0.09256(3) 0.27115(4) 0.05143(18) Uani 1 1 d . . .
O1B O 0.3304(4) 0.0558(3) 0.2532(5) 0.0659(11) Uani 1 1 d . . .
O2A O 0.1547(4) -0.0483(4) 0.0959(4) 0.0703(12) Uani 1 1 d . . .
O2B O 0.1584(3) -0.0079(2) 0.3795(4) 0.0517(9) Uani 1 1 d . . .
O1A O 0.3784(4) -0.1182(3) 0.1174(4) 0.0658(11) Uani 1 1 d . . .
C1 C 0.4370(7) -0.1170(5) 0.4068(7) 0.0743(19) Uani 1 1 d . . .
H1A H 0.5065 -0.1329 0.3629 0.104 Uiso 1 1 calc R . .
H1B H 0.4213 -0.1680 0.4621 0.104 Uiso 1 1 calc R . .
H1C H 0.4570 -0.0611 0.4568 0.104 Uiso 1 1 calc R . .
C2B C 0.1843(5) 0.0820(3) 0.3911(5) 0.0453(12) Uani 1 1 d . . .
C2A C 0.2036(5) -0.0565(4) -0.0095(5) 0.0496(13) Uani 1 1 d . . .
C2 C 0.1451(7) -0.2075(5) 0.2765(9) 0.089(2) Uani 1 1 d . . .
H2A H 0.1543 -0.2509 0.2087 0.124 Uiso 1 1 calc R . .
H2B H 0.0605 -0.1838 0.2657 0.124 Uiso 1 1 calc R . .
H2C H 0.1629 -0.2393 0.3573 0.124 Uiso 1 1 calc R . .
C3B C 0.1182(6) 0.1352(4) 0.4685(6) 0.0619(15) Uani 1 1 d . . .
H3B H 0.0566 0.1017 0.5029 0.080 Uiso 1 1 calc R . .
C4B C 0.1263(8) 0.2281(5) 0.5040(7) 0.083(2) Uani 1 1 d . . .
H4B H 0.0720 0.2467 0.5604 0.107 Uiso 1 1 calc R . .
C7A C 0.4037(6) -0.0963(5) -0.0950(7) 0.0652(17) Uani 1 1 d . . .
H7A H 0.4859 -0.1167 -0.0701 0.085 Uiso 1 1 calc R . .
C5B C 0.2018(10) 0.2962(5) 0.4688(8) 0.096(3) Uani 1 1 d . . .
H5B H 0.1944 0.3551 0.5057 0.125 Uiso 1 1 calc R . .
C6A C 0.3747(6) -0.0753(5) -0.2218(7) 0.0724(19) Uani 1 1 d . . .
H6A H 0.4410 -0.0812 -0.2690 0.094 Uiso 1 1 calc R . .
C6B C 0.2893(8) 0.2893(5) 0.3840(9) 0.085(2) Uani 1 1 d . . .
H6B H 0.3317 0.3447 0.3702 0.110 Uiso 1 1 calc R . .
C5A C 0.2618(6) -0.0467(6) -0.2911(7) 0.0720(18) Uani 1 1 d . . .
H5A H 0.2605 -0.0394 -0.3788 0.094 Uiso 1 1 calc R . .
C7B C 0.3215(6) 0.2121(5) 0.3182(7) 0.0699(17) Uani 1 1 d . . .
H7B H 0.3804 0.2234 0.2634 0.091 Uiso 1 1 calc R . .
C4A C 0.1548(6) -0.0284(4) -0.2453(6) 0.0623(15) Uani 1 1 d . . .
H4A H 0.0881 -0.0107 -0.3069 0.081 Uiso 1 1 calc R . .
C1B C 0.2791(5) 0.1175(4) 0.3208(6) 0.0510(13) Uani 1 1 d . . .
C3A C 0.1265(5) -0.0312(4) -0.1231(6) 0.0551(14) Uani 1 1 d . . .
H3A H 0.0446 -0.0139 -0.1141 0.072 Uiso 1 1 calc R . .
C1A C 0.3290(5) -0.0920(4) 0.0046(6) 0.0516(13) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sn1 0.0529(3) 0.0521(3) 0.0483(3) -0.00091(16) 0.00374(17) 0.01051(16)
O1B 0.062(2) 0.057(2) 0.084(3) 0.011(2) 0.029(2) 0.005(2)
O2A 0.055(2) 0.102(3) 0.053(3) 0.001(2) 0.005(2) 0.030(2)
O2B 0.055(2) 0.046(2) 0.056(2) -0.0017(17) 0.0143(18) 0.0031(17)
O1A 0.053(2) 0.090(3) 0.052(3) -0.001(2) -0.0007(19) 0.028(2)
C1 0.070(4) 0.089(5) 0.059(4) -0.004(3) -0.005(3) 0.014(4)
C2B 0.042(3) 0.046(3) 0.046(3) 0.000(2) 0.001(2) 0.002(2)
C2A 0.041(3) 0.056(3) 0.051(3) -0.005(3) 0.005(2) 0.009(2)
C2 0.076(5) 0.064(4) 0.125(7) -0.002(4) 0.013(5) -0.014(4)
C3B 0.080(4) 0.054(3) 0.054(4) 0.001(3) 0.015(3) 0.005(3)
C4B 0.115(6) 0.067(4) 0.070(5) -0.010(4) 0.028(4) 0.010(4)
C7A 0.043(3) 0.088(5) 0.063(4) 0.001(3) 0.003(3) 0.010(3)
C5B 0.163(9) 0.049(4) 0.074(5) -0.007(3) 0.008(6) -0.016(5)
C6A 0.051(3) 0.105(5) 0.063(4) 0.006(4) 0.016(3) 0.004(3)
C6B 0.101(6) 0.051(4) 0.094(6) 0.011(4) -0.013(5) -0.008(4)
C5A 0.059(4) 0.104(5) 0.053(4) 0.014(4) 0.009(3) 0.004(4)
C7B 0.067(4) 0.060(4) 0.080(5) 0.016(4) 0.003(3) -0.003(3)
C4A 0.057(3) 0.073(4) 0.055(4) 0.009(3) -0.001(3) 0.006(3)
C1B 0.037(3) 0.056(3) 0.058(3) 0.005(3) 0.001(2) 0.004(2)
C3A 0.042(3) 0.070(4) 0.053(4) 0.002(3) 0.005(2) 0.011(3)
C1A 0.044(3) 0.063(3) 0.047(3) -0.005(3) 0.005(2) 0.014(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 C1 2.125(7) . ?
Sn1 O1A 2.132(4) . ?
Sn1 C2 2.145(7) . ?
Sn1 O2B 2.168(4) . ?
Sn1 O2A 2.187(4) . ?
Sn1 O1B 2.206(4) . ?
O1B C1B 1.302(8) . ?
O2A C2A 1.302(7) . ?
O2B C2B 1.308(6) . ?
O1A C1A 1.287(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2B C3B 1.380(8) . ?
C2B C1B 1.434(8) . ?
C2A C3A 1.404(8) . ?
C2A C1A 1.424(7) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3B C4B 1.369(9) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.348(11) . ?
C4B H4B 0.9300 . ?
C7A C6A 1.364(10) . ?
C7A C1A 1.412(9) . ?
C7A H7A 0.9300 . ?
C5B C6B 1.391(12) . ?
C5B H5B 0.9300 . ?
C6A C5A 1.383(9) . ?
C6A H6A 0.9300 . ?
C6B C7B 1.368(11) . ?
C6B H6B 0.9300 . ?
C5A C4A 1.335(9) . ?
C5A H5A 0.9300 . ?
C7B C1B 1.419(8) . ?
C7B H7B 0.9300 . ?
C4A C3A 1.368(9) . ?
C4A H4A 0.9300 . ?
C3A H3A 0.9300 . ?
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
C1 Sn1 O1A 90.8(2) . . ?
C1 Sn1 C2 109.3(3) . . ?
O1A Sn1 C2 107.5(3) . . ?
C1 Sn1 O2B 102.3(2) . . ?
O1A Sn1 O2B 154.10(16) . . ?
C2 Sn1 O2B 89.3(3) . . ?
C1 Sn1 O2A 160.7(2) . . ?
O1A Sn1 O2A 73.30(15) . . ?
C2 Sn1 O2A 86.5(3) . . ?
O2B Sn1 O2A 88.68(15) . . ?
C1 Sn1 O1B 90.2(2) . . ?
O1A Sn1 O1B 85.25(18) . . ?
C2 Sn1 O1B 156.0(2) . . ?
O2B Sn1 O1B 72.61(15) . . ?
O2A Sn1 O1B 77.74(19) . . ?
C1B O1B Sn1 116.9(4) . . ?
C2A O2A Sn1 116.0(3) . . ?
C2B O2B Sn1 117.4(3) . . ?
C1A O1A Sn1 117.6(3) . . ?
Sn1 C1 H1A 109.5 . . ?
Sn1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Sn1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2B C2B C3B 118.0(5) . . ?
O2B C2B C1B 116.8(5) . . ?
C3B C2B C1B 125.2(5) . . ?
O2A C2A C3A 116.5(5) . . ?
O2A C2A C1A 115.7(5) . . ?
C3A C2A C1A 127.8(5) . . ?
Sn1 C2 H2A 109.5 . . ?
Sn1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Sn1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4B C3B C2B 132.1(7) . . ?
C4B C3B H3B 113.9 . . ?
C2B C3B H3B 113.9 . . ?
C5B C4B C3B 129.2(7) . . ?
C5B C4B H4B 115.4 . . ?
C3B C4B H4B 115.4 . . ?
C6A C7A C1A 130.4(6) . . ?
C6A C7A H7A 114.8 . . ?
C1A C7A H7A 114.8 . . ?
C4B C5B C6B 128.0(7) . . ?
C4B C5B H5B 116.0 . . ?
C6B C5B H5B 116.0 . . ?
C7A C6A C5A 130.0(6) . . ?
C7A C6A H6A 115.0 . . ?
C5A C6A H6A 115.0 . . ?
C7B C6B C5B 128.8(7) . . ?
C7B C6B H6B 115.6 . . ?
C5B C6B H6B 115.6 . . ?
C4A C5A C6A 126.8(7) . . ?
C4A C5A H5A 116.6 . . ?
C6A C5A H5A 116.6 . . ?
C6B C7B C1B 130.0(7) . . ?
C6B C7B H7B 115.0 . . ?
C1B C7B H7B 115.0 . . ?
C5A C4A C3A 130.9(6) . . ?
C5A C4A H4A 114.5 . . ?
C3A C4A H4A 114.5 . . ?
O1B C1B C7B 117.7(6) . . ?
O1B C1B C2B 115.8(5) . . ?
C7B C1B C2B 126.5(6) . . ?
C4A C3A C2A 129.1(5) . . ?
C4A C3A H3A 115.5 . . ?
C2A C3A H3A 115.5 . . ?
O1A C1A C7A 118.3(5) . . ?
O1A C1A C2A 117.2(5) . . ?
C7A C1A C2A 124.5(5) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C3A H3A O2A 0.93 2.35 3.272(7) 173.1 3
C4A H4A O2B 0.93 2.66 3.494(7) 149.6 3
C6A H6A O1B 0.93 2.46 3.241(8) 141.5 3_655
_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full 25.01
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max 0.606
_refine_diff_density_min -0.596
_refine_diff_density_rms 0.183