#------------------------------------------------------------------------------ #$Date: 2012-02-28 14:14:52 +0200 (Tue, 28 Feb 2012) $ #$Revision: 35911 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/10/09/1100968.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_1100968 loop_ _publ_author_name 'Corrado Di Nicola' 'Agustin Galindo' 'John V. Hanna' 'Fabio Marchetti' 'Claudio Pettinari' 'Riccardo Pettinari' 'Eleonora Rivarola' 'Brian W. Skelton' 'Allan H. White' _publ_contact_author_address ; Department of Chemistry University of Western Australia 35 Stirling Highway Crawley Western Australia 6009 Australia ; _publ_contact_author_email bws@crystal.uwa.edu.au _publ_contact_author_fax (+61)_08_9380_1118 _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_phone (+61)_08-9380_3481 _publ_section_title ; Synthesis and Spectroscopic and X-ray Structural Characterization of R2SnIV-Oxydiacetate and -Iminodiacetate Complexes ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 3094 _journal_page_last 3102 _journal_volume 44 _journal_year 2005 _chemical_formula_moiety 'C12 H24 O12 Sn2' _chemical_formula_sum 'C12 H24 O12 Sn2' _chemical_formula_weight 597.73 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90.00000 _cell_angle_beta 125.015(2) _cell_angle_gamma 90.00000 _cell_formula_units_Z 4 _cell_length_a 22.608(2) _cell_length_b 6.6669(7) _cell_length_c 15.527(2) _cell_measurement_reflns_used 6427 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 35.5 _cell_measurement_theta_min 2.4 _cell_volume 1916.7(4) _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' _computing_structure_refinement 'xtal CRYLSQ' _computing_structure_solution xtal _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.0 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_radiation_detector 'CCD area detector' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .028 _diffrn_reflns_av_sigmaI/netI .014 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 19338 _diffrn_reflns_theta_full 37.49 _diffrn_reflns_theta_max 37.49 _diffrn_reflns_theta_min 2.2 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.663 _exptl_absorpt_correction_T_max .83 _exptl_absorpt_correction_T_min .64 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1168 _exptl_crystal_size_max .4 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .32 _refine_diff_density_max .766 _refine_diff_density_min -2.02 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.101 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 118 _refine_ls_number_reflns 4646 _refine_ls_number_restraints 0 _refine_ls_R_factor_all .027 _refine_ls_R_factor_gt .024 _refine_ls_shift/su_max .004 _refine_ls_shift/su_mean .001 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all .045 _refine_ls_wR_factor_ref .043 _reflns_d_resolution_high .584 _reflns_d_resolution_low 9.241 _reflns_Friedel_coverage 0 _reflns_limit_h_max 38 _reflns_limit_h_min 0 _reflns_limit_k_max 11 _reflns_limit_k_min 0 _reflns_limit_l_max 21 _reflns_limit_l_min -26 _reflns_number_gt 4646 _reflns_number_total 5001 _reflns_threshold_expression 'F > 4.00 sig(F )' _[local]_cod_data_source_file ic048240tsi20041215_025357_1.cif _[local]_cod_data_source_block cp2b _[local]_cod_cif_authors_sg_Hall -c_2yc _cod_database_code 1100968 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z loop_ _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_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Sn .358670(5) .311521(15) .568428(7) .01136(5) Uani ? ? 1.00000 ? ? O1 .37361(6) .1362(2) .45030(9) .0167(4) Uani ? ? 1.00000 ? ? C11 .31596(8) .0461(2) .35473(11) .0140(4) Uani ? ? 1.00000 ? ? C12 .24862(8) .0373(2) .35375(11) .0136(4) Uani ? ? 1.00000 ? ? O11 .24780(6) .1359(2) .42363(9) .0151(4) Uani ? ? 1.00000 ? ? O12 .19784(7) -.0643(2) .28205(11) .0220(5) Uani ? ? 1.00000 ? ? C21 .43210(9) .2052(2) .44676(13) .0154(5) Uani ? ? 1.00000 ? ? C22 .49053(9) .2871(2) .55435(13) .0141(5) Uani ? ? 1.00000 ? ? O21 .47060(7) .3334(2) .61534(10) .0166(4) Uani ? ? 1.00000 ? ? O22 .55192(7) .3067(2) .57805(12) .0201(5) Uani ? ? 1.00000 ? ? C01 .32200(9) .5642(3) .46952(13) .0183(5) Uani ? ? 1.00000 ? ? C02 .37926(10) .0502(3) .65756(14) .0196(5) Uani ? ? 1.00000 ? ? O03 .41201(6) .5082(2) .70906(9) .0160(4) Uani ? ? 1.00000 ? ? H11a .32955 -.08563 .34956 .01900 Uiso ? ? 1.00000 ? ? H12b .30660 .12413 .29689 .01900 Uiso ? ? 1.00000 ? ? H21a .41580 .30809 .39560 .02100 Uiso ? ? 1.00000 ? ? H21b .45088 .09702 .42936 .02100 Uiso ? ? 1.00000 ? ? H01a .36186 .64807 .48870 .02800 Uiso ? ? 1.00000 ? ? H01b .28880 .63763 .47634 .02800 Uiso ? ? 1.00000 ? ? H01c .29866 .52261 .39854 .02800 Uiso ? ? 1.00000 ? ? H02a .35315 -.05872 .61148 .03000 Uiso ? ? 1.00000 ? ? H02b .36376 .07051 .70246 .03000 Uiso ? ? 1.00000 ? ? H02c .42956 .02172 .69913 .03000 Uiso ? ? 1.00000 ? ? H03a .44899 .44762 .76462 .02400 Uiso ? ? 1.00000 ? ? H03b .38309 .53247 .72230 .02400 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sn .01047(6) .01353(6) .00862(6) -.00043(2) .00463(4) -.00014(2) O1 .0140(4) .0236(5) .0133(4) -.0049(4) .0084(4) -.0049(4) C11 .0142(5) .0163(6) .0108(5) -.0013(4) .0068(4) -.0022(4) C12 .0126(5) .0143(6) .0115(5) .0002(4) .0056(4) -.0020(4) O11 .0156(4) .0184(5) .0118(4) -.0024(4) .0082(4) -.0045(4) O12 .0144(5) .0287(6) .0200(5) -.0047(4) .0081(4) -.0133(5) C21 .0145(6) .0206(7) .0132(6) -.0010(5) .0091(5) -.0012(4) C22 .0127(5) .0156(6) .0138(6) .0007(4) .0075(5) .0005(4) O21 .0118(4) .0248(6) .0124(5) -.0019(4) .0065(4) -.0033(4) O22 .0124(5) .0270(7) .0221(6) -.0033(4) .0106(5) -.0030(4) C01 .0176(6) .0188(6) .0156(6) .0010(5) .0078(5) .0048(5) C02 .0199(6) .0192(7) .0172(6) .0012(5) .0091(5) .0041(5) O03 .0126(4) .0206(5) .0124(4) -.0002(4) .0058(4) -.0027(4) loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 48 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 96 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 48 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' Sn ? 0 8 -.873 1.424 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Sn O11 . . . 65.49(5) ? O1 Sn O21 . . . 68.86(5) ? O1 Sn C01 . . . 90.07(7) ? O1 Sn C02 . . . 91.43(7) ? O1 Sn O03 . . . 145.03(5) ? O1 Sn O11 . . '7 556' 132.74(4) ? O11 Sn O21 . . . 134.31(6) ? O11 Sn C01 . . . 86.94(5) ? O11 Sn C02 . . . 86.16(5) ? O11 Sn O03 . . . 149.43(6) ? O11 Sn O11 . . '7 556' 67.27(5) ? O21 Sn C01 . . . 94.89(7) ? O21 Sn C02 . . . 93.37(7) ? O21 Sn O03 . . . 76.26(6) ? O21 Sn O11 . . '7 556' 158.40(5) ? C01 Sn C02 . . . 171.59(7) ? C01 Sn O03 . . . 90.53(6) ? C01 Sn O11 . . '7 556' 86.37(7) ? C02 Sn O03 . . . 92.97(6) ? C02 Sn O11 . . '7 556' 86.54(7) ? O03 Sn O11 . . '7 556' 82.17(5) ? Sn O1 C11 . . . 124.33(13) ? Sn O1 C21 . . . 114.77(10) ? C11 O1 C21 . . . 114.06(16) ? O1 C11 C12 . . . 109.83(16) ? O1 C11 H11a . . . 109.28 ? O1 C11 H12b . . . 109.09 ? C12 C11 H11a . . . 109.60 ? C12 C11 H12b . . . 109.51 ? H11a C11 H12b . . . 109.5 ? C11 C12 O11 . . . 118.41(12) ? C11 C12 O12 . . . 115.84(18) ? O11 C12 O12 . . . 125.7(2) ? Sn O11 C12 . . . 120.62(12) ? Sn O11 Sn . . '7 556' 112.73(6) ? C12 O11 Sn . . '7 556' 126.61(10) ? O1 C21 C22 . . . 108.27(18) ? O1 C21 H21a . . . 109.93 ? O1 C21 H21b . . . 109.90 ? C22 C21 H21a . . . 109.62 ? C22 C21 H21b . . . 109.70 ? H21a C21 H21b . . . 109.4 ? C21 C22 O21 . . . 116.20(17) ? C21 C22 O22 . . . 119.4(2) ? O21 C22 O22 . . . 124.39(15) ? Sn O21 C22 . . . 123.88(9) ? Sn C01 H01a . . . 109.67 ? Sn C01 H01b . . . 109.66 ? Sn C01 H01c . . . 109.72 ? H01a C01 H01b . . . 109.17 ? H01a C01 H01c . . . 109.3 ? H01b C01 H01c . . . 109.30 ? Sn C02 H02a . . . 109.28 ? Sn C02 H02b . . . 109.18 ? Sn C02 H02c . . . 109.83 ? H02a C02 H02b . . . 109.2 ? H02a C02 H02c . . . 110.0 ? H02b C02 H02c . . . 109.30 ? Sn O03 H03a . . . 111.51 ? Sn O03 H03b . . . 107.88 ? H03a O03 H03b . . . 107.13 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn O1 . . 2.3570(17) ? Sn O11 . . 2.4982(11) ? Sn O21 . . 2.2000(16) ? Sn C01 . . 2.1029(18) ? Sn C02 . . 2.104(2) ? Sn O03 . . 2.2182(13) ? Sn O11 . '7 556' 2.5046(17) ? O1 C11 . . 1.4290(16) ? O1 C21 . . 1.430(3) ? C11 C12 . . 1.515(3) ? C11 H11a . . .9491 ? C11 H12b . . .9505 ? C12 O11 . . 1.278(2) ? C12 O12 . . 1.2449(17) ? C21 C22 . . 1.517(2) ? C21 H21a . . .9495 ? C21 H21b . . .951 ? C22 O21 . . 1.298(3) ? C22 O22 . . 1.222(3) ? C01 H01a . . .952 ? C01 H01b . . .952 ? C01 H01c . . .9499 ? C02 H02a . . .9505 ? C02 H02b . . .953 ? C02 H02c . . .9506 ? O03 H03a . . .8824 ? O03 H03b . . .8064 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ? 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 ? ? ? ? ? ? ? ? ? ?