# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1808 data_sbc1 _publ_contact_author_name 'Anthony K. Cheetham' _publ_contact_author_address ; Materials Research Laboratory University of California Santa Barbara CA 93106 U.S.A ; _publ_contact_author_phone '805-893 8767' _publ_contact_author_fax '805-893 8797' _publ_contact_author_email 'cheetham@mrl.ucsb.edu' _publ_requested_journal ; Journal of the Chemical Society, Chemical Communications ; _publ_requested_coeditor_name ? _publ_section_title ; The hybrid open-framework of tin(II)phosphonopropionate-oxalate, Sn4(O3PCH2CH2COO)2(C2O4) ; loop_ _publ_author_name _publ_author_address 'Stock, Norbert' ; Materials Research Laboratory University of California Santa Barbara CA 93106 U.S.A ; 'Stucky, Galen D.' ; Department of Chemistry University of California Santa Barbara CA 93106 U.S.A ; 'Cheetham, Anthony K.' ; Materials Research Laboratory University of California Santa Barbara CA 93106 U.S.A ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'tin phosphonopropionate-oxalate' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H8 O14 P2 Sn4' _chemical_formula_weight 864.84 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' 'P' 'P' 0.1023 0.0942 '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 P2(1)/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 4.7895(14) _cell_length_b 23.242(7) _cell_length_c 8.138(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.240(6) _cell_angle_gamma 90.00 _cell_volume 903.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(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 0.2 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 5.714 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _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 9081 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.30 _reflns_number_total 2105 _reflns_number_gt 1664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0267P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2105 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _refine_ls_shift/su_max 0.002 _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 -0.01347(5) 0.591106(10) 0.63990(3) 0.01804(8) Uani 1 1 d . . . Sn2 Sn -0.82486(5) 0.589573(11) 1.17284(3) 0.02053(9) Uani 1 1 d . . . P1 P -0.48653(19) 0.65471(4) 0.87333(11) 0.0150(2) Uani 1 1 d . . . O1 O -0.2616(5) 0.61031(11) 0.8404(3) 0.0218(6) Uani 1 1 d . . . O2 O -0.7303(5) 0.65326(11) 0.7410(3) 0.0205(6) Uani 1 1 d . . . O3 O -0.5815(6) 0.64625(11) 1.0480(3) 0.0240(6) Uani 1 1 d . . . O4 O -0.5437(6) 0.87719(11) 0.8974(3) 0.0251(6) Uani 1 1 d . . . O5 O -0.1865(5) 0.82964(11) 1.0206(3) 0.0238(6) Uani 1 1 d . . . O6 O -0.7892(5) 0.53741(11) 0.9158(3) 0.0228(6) Uani 1 1 d . . . O7 O -0.4823(6) 0.52546(11) 1.2027(3) 0.0253(6) Uani 1 1 d . . . C1 C -0.3353(8) 0.72499(16) 0.8736(4) 0.0199(8) Uani 1 1 d . . . H1A H -0.1953 0.7279 0.9656 0.024 Uiso 1 1 calc R . . H1B H -0.2408 0.7299 0.7731 0.024 Uiso 1 1 calc R . . C2 C -0.5473(8) 0.77372(16) 0.8861(5) 0.0214(8) Uani 1 1 d . . . H2A H -0.6536 0.7778 0.7806 0.026 Uiso 1 1 calc R . . H2B H -0.6775 0.7632 0.9668 0.026 Uiso 1 1 calc R . . C3 C -0.4184(8) 0.83106(16) 0.9339(4) 0.0183(8) Uani 1 1 d . . . C4 C -0.5888(7) 0.50342(15) 0.9169(4) 0.0164(7) 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 0.01918(15) 0.01680(14) 0.01779(14) -0.00199(10) -0.00097(10) 0.00105(11) Sn2 0.01863(15) 0.02355(15) 0.01990(15) -0.00010(10) 0.00477(10) 0.00004(11) P1 0.0152(5) 0.0150(5) 0.0149(5) -0.0004(4) 0.0016(3) -0.0007(4) O1 0.0208(14) 0.0184(13) 0.0267(15) 0.0020(11) 0.0061(11) 0.0050(11) O2 0.0170(13) 0.0233(14) 0.0202(14) 0.0011(10) -0.0045(10) -0.0040(11) O3 0.0332(16) 0.0226(14) 0.0165(13) -0.0006(11) 0.0043(11) -0.0023(12) O4 0.0378(16) 0.0175(14) 0.0191(14) 0.0004(11) -0.0036(11) 0.0023(13) O5 0.0234(15) 0.0213(14) 0.0255(15) -0.0038(11) -0.0059(11) -0.0022(12) O6 0.0236(14) 0.0227(14) 0.0213(14) 0.0006(11) -0.0026(11) 0.0053(12) O7 0.0314(15) 0.0238(14) 0.0199(14) -0.0044(11) -0.0033(11) 0.0050(12) C1 0.0205(19) 0.0195(19) 0.0198(19) -0.0011(15) 0.0027(15) -0.0031(16) C2 0.0205(19) 0.0202(19) 0.0229(19) 0.0015(16) -0.0028(14) -0.0037(16) C3 0.026(2) 0.0188(19) 0.0103(18) 0.0008(14) 0.0040(15) 0.0012(16) C4 0.0178(19) 0.0140(17) 0.0170(19) 0.0020(14) -0.0024(14) -0.0014(15) _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 O2 2.106(3) 1_655 ? Sn1 O1 2.136(3) . ? Sn1 O5 2.214(3) 4_575 ? Sn2 O3 2.074(3) . ? Sn2 O7 2.216(3) . ? Sn2 O4 2.320(3) 4_576 ? Sn2 O6 2.435(3) . ? P1 O2 1.529(3) . ? P1 O1 1.530(3) . ? P1 O3 1.537(3) . ? P1 C1 1.787(4) . ? O2 Sn1 2.106(2) 1_455 ? O4 C3 1.254(4) . ? O4 Sn2 2.320(3) 4_575 ? O5 C3 1.271(4) . ? O5 Sn1 2.214(3) 4_576 ? O6 C4 1.243(4) . ? O7 C4 1.250(4) 3_467 ? C1 C2 1.529(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.508(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 O7 1.250(4) 3_467 ? C4 C4 1.551(7) 3_467 ? 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 O2 Sn1 O1 86.37(10) 1_655 . ? O2 Sn1 O5 79.05(10) 1_655 4_575 ? O1 Sn1 O5 87.13(10) . 4_575 ? O3 Sn2 O7 92.43(11) . . ? O3 Sn2 O4 81.94(10) . 4_576 ? O7 Sn2 O4 75.86(10) . 4_576 ? O3 Sn2 O6 79.50(10) . . ? O7 Sn2 O6 70.18(9) . . ? O4 Sn2 O6 140.25(10) 4_576 . ? O2 P1 O1 111.89(15) . . ? O2 P1 O3 112.69(15) . . ? O1 P1 O3 109.63(15) . . ? O2 P1 C1 108.02(16) . . ? O1 P1 C1 109.05(16) . . ? O3 P1 C1 105.28(16) . . ? P1 O1 Sn1 135.53(16) . . ? P1 O2 Sn1 136.57(16) . 1_455 ? P1 O3 Sn2 138.58(16) . . ? C3 O4 Sn2 135.3(2) . 4_575 ? C3 O5 Sn1 120.3(2) . 4_576 ? C4 O6 Sn2 114.4(2) . . ? C4 O7 Sn2 121.2(2) 3_467 . ? C2 C1 P1 114.0(2) . . ? C2 C1 H1A 108.8 . . ? P1 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? P1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C3 C2 C1 114.2(3) . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2B 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? O4 C3 O5 122.5(4) . . ? O4 C3 C2 121.0(3) . . ? O5 C3 C2 116.4(3) . . ? O6 C4 O7 126.2(3) . 3_467 ? O6 C4 C4 116.4(4) . 3_467 ? O7 C4 C4 117.4(4) 3_467 3_467 ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.719 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.184