data_Z:\structs\JWS\Me3snoh\TMT-P21C.CIF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Me3snoh' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H10 O Sn' _chemical_formula_weight 180.80 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 P21/c 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 10.793(2) _cell_length_b 6.6883(13) _cell_length_c 8.3828(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.130(3) _cell_angle_gamma 90.00 _cell_volume 605.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.985 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 4.087 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1798 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0896 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 24.92 _reflns_number_total 757 _reflns_number_gt 495 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect' _computing_cell_refinement 'DENZO-SMN' _computing_data_reduction 'DENZO-SMN' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed' _computing_publication_material ? _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^)+(0.0000P)^2^+0.8216P] 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 SHELXL _refine_ls_extinction_coef 0.0118(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 757 _refine_ls_number_parameters 80 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.003 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 0.75002(7) 0.25652(8) 0.16259(7) 0.0236(5) Uani 1 1 d . . . O1 O 0.7204(14) 0.351(3) 0.413(2) 0.022(5) Uani 0.50 1 d PU . 1 H1 H 0.6830 0.4799 0.4145 0.026 Uiso 0.50 1 calc PR . 1 C1 C 0.7495(8) 0.5621(13) 0.0880(10) 0.027(3) Uani 1 1 d . . . H1A H 0.8331 0.6007 0.0547 0.040 Uiso 1 1 calc R . . H1B H 0.7231 0.6471 0.1769 0.040 Uiso 1 1 calc R . . H1C H 0.6920 0.5786 -0.0016 0.040 Uiso 1 1 calc R . . C2 C 0.568(3) 0.102(5) 0.152(3) 0.048(10) Uani 0.50 1 d PU . 2 H2A H 0.5706 -0.0021 0.0697 0.072 Uiso 0.50 1 calc PR . 2 H2B H 0.5031 0.1985 0.1269 0.072 Uiso 0.50 1 calc PR . 2 H2C H 0.5509 0.0397 0.2559 0.072 Uiso 0.50 1 calc PR . 2 C3 C 0.909(3) 0.103(6) 0.225(4) 0.038(10) Uani 0.50 1 d PU . 1 H3A H 0.9766 0.1423 0.1534 0.058 Uiso 0.50 1 calc PR . 1 H3B H 0.8943 -0.0409 0.2152 0.058 Uiso 0.50 1 calc PR . 1 H3C H 0.9316 0.1355 0.3351 0.058 Uiso 0.50 1 calc PR . 1 O1A O 0.7849(15) 0.349(3) 0.419(2) 0.032(5) Uani 0.50 1 d PU . 2 H1A1 H 0.8284 0.4727 0.4219 0.038 Uiso 0.50 1 calc PR . 2 C2A C 0.585(2) 0.108(3) 0.226(3) 0.014(6) Uani 0.50 1 d PU . 1 H2A1 H 0.5856 -0.0267 0.1800 0.020 Uiso 0.50 1 calc PR . 1 H2A2 H 0.5141 0.1828 0.1840 0.020 Uiso 0.50 1 calc PR . 1 H2A3 H 0.5796 0.0995 0.3420 0.020 Uiso 0.50 1 calc PR . 1 C3A C 0.930(3) 0.110(6) 0.168(4) 0.050(11) Uani 0.50 1 d PU . 2 H3A1 H 0.9615 0.1085 0.2777 0.075 Uiso 0.50 1 calc PR . 2 H3A2 H 0.9877 0.1829 0.0995 0.075 Uiso 0.50 1 calc PR . 2 H3A3 H 0.9213 -0.0277 0.1294 0.075 Uiso 0.50 1 calc PR . 2 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 0.0255(6) 0.0277(7) 0.0174(6) 0.0011(4) -0.0010(3) -0.0004(5) O1 0.025(9) 0.023(8) 0.019(8) -0.015(6) 0.002(7) 0.001(7) C1 0.014(7) 0.039(7) 0.026(7) 0.000(5) -0.002(5) -0.008(5) C2 0.041(13) 0.056(12) 0.048(13) 0.001(9) 0.001(9) 0.004(9) C3 0.029(12) 0.048(12) 0.038(13) 0.000(9) -0.003(9) -0.002(9) O1A 0.025(9) 0.035(8) 0.035(8) -0.001(6) -0.005(8) -0.001(8) C2A 0.014(10) 0.014(9) 0.013(10) -0.002(8) 0.002(8) -0.001(7) C3A 0.047(14) 0.054(13) 0.050(14) -0.002(9) -0.005(9) -0.001(9) _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 C3 2.06(3) . ? Sn1 C2A 2.10(2) . ? Sn1 C1 2.137(8) . ? Sn1 C3A 2.17(4) . ? Sn1 O1A 2.194(19) 4_565 ? Sn1 C2 2.22(3) . ? Sn1 O1 2.214(17) . ? Sn1 O1 2.238(18) 4_565 ? Sn1 O1A 2.268(19) . ? O1 Sn1 2.238(18) 4_566 ? O1A Sn1 2.194(19) 4_566 ? 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 C3 Sn1 C2A 113.9(11) . . ? C3 Sn1 C1 123.4(10) . . ? C2A Sn1 C1 121.5(7) . . ? C3 Sn1 C3A 14.0(14) . . ? C2A Sn1 C3A 122.4(12) . . ? C1 Sn1 C3A 116.1(10) . . ? C3 Sn1 O1A 86.0(10) . 4_565 ? C2A Sn1 O1A 103.2(8) . 4_565 ? C1 Sn1 O1A 92.1(6) . 4_565 ? C3A Sn1 O1A 73.7(10) . 4_565 ? C3 Sn1 C2 120.8(13) . . ? C2A Sn1 C2 16.8(9) . . ? C1 Sn1 C2 115.7(8) . . ? C3A Sn1 C2 125.4(14) . . ? O1A Sn1 C2 88.1(8) 4_565 . ? C3 Sn1 O1 91.4(10) . . ? C2A Sn1 O1 76.9(7) . . ? C1 Sn1 O1 90.1(5) . . ? C3A Sn1 O1 103.9(10) . . ? O1A Sn1 O1 177.2(8) 4_565 . ? C2 Sn1 O1 92.4(8) . . ? C3 Sn1 O1 101.1(10) . 4_565 ? C2A Sn1 O1 87.9(7) . 4_565 ? C1 Sn1 O1 92.0(5) . 4_565 ? C3A Sn1 O1 90.0(10) . 4_565 ? O1A Sn1 O1 18.1(5) 4_565 4_565 ? C2 Sn1 O1 71.9(8) . 4_565 ? O1 Sn1 O1 163.4(8) . 4_565 ? C3 Sn1 O1A 76.1(10) . . ? C2A Sn1 O1A 91.7(7) . . ? C1 Sn1 O1A 90.9(6) . . ? C3A Sn1 O1A 87.5(10) . . ? O1A Sn1 O1A 160.3(8) 4_565 . ? C2 Sn1 O1A 108.0(8) . . ? O1 Sn1 O1A 17.9(5) . . ? O1 Sn1 O1A 176.8(8) 4_565 . ? Sn1 O1 Sn1 140.7(9) . 4_566 ? Sn1 O1A Sn1 139.9(10) 4_566 . ? _diffrn_measured_fraction_theta_max 0.724 _diffrn_reflns_theta_full 24.92 _diffrn_measured_fraction_theta_full 0.724 _refine_diff_density_max 0.823 _refine_diff_density_min -0.996 _refine_diff_density_rms 0.263