# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New journal of Chemistry' loop_ _publ_author_name 'Shannon, Ian J.' 'Kariuki, Benson M.' 'Menaa, Bouzid' _publ_contact_author_name 'Dr Ian J Shannon' _publ_contact_author_address ; School of Chemical Sciences University of Birmingham Edgbaston Birmingham West Midlands B15 2TT UNITED KINGDOM ; _publ_contact_author_email 'i.shannon@bham.ac.uk' _publ_section_title ; Preparation of copper and zinc vinylphosphonate materials M(03PC2H3).H2O using metal oxide precursors and their crystal structure ; _publ_section_references ; PLATON- (a) Spek, A. L. (1990) Acta Cryst. A46, C34. (b) Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. SHELXTL, program suite for structure solution and refinement, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA SMART, program for instrument control and data aquisition, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA SAINTPLUS, program suite for data processing, Bruker AXS, Inc. 5465 East Cheryl Parkway, Nadison, Wisconsin 53711-5373, USA ; data_bm4 _database_code_CSD 182285 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H3 Cu O3 P, H2 O' _chemical_formula_sum 'C2 H5 Cu O4 P' _chemical_formula_weight 187.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 '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 9.86990(10) _cell_length_b 7.61920(10) _cell_length_c 7.31710(10) _cell_angle_alpha 90.0000(10) _cell_angle_beta 95.8030(10) _cell_angle_gamma 90.0000(10) _cell_volume 547.432(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 976 _cell_measurement_theta_min 7.36 _cell_measurement_theta_max 70.83 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 372 _exptl_absorpt_coefficient_mu 7.854 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1369 _exptl_absorpt_correction_T_max 0.5072 _exptl_absorpt_process_details 'DIFABS in SAINTPLUS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD ' _diffrn_measurement_method 'CCD slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2230 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 4.50 _diffrn_reflns_theta_max 70.83 _reflns_number_total 982 _reflns_number_gt 974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart software' _computing_cell_refinement 'SaintPlus' _computing_data_reduction 'SainPlus' _computing_structure_solution ' SHELX86' _computing_structure_refinement 'SHELXL-97' _computing_molecular_graphics 'Platon' _computing_publication_material 'Platon' _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^)+(0.0377P)^2^+0.4652P] 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 SHELXL _refine_ls_extinction_coef 0.0197(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 982 _refine_ls_number_parameters 85 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 Cu1 Cu 0.54400(3) -0.18908(4) 0.06303(4) 0.0142(2) Uani 1 1 d . . . P1 P 0.65814(5) -0.54981(7) 0.17799(7) 0.0106(2) Uani 1 1 d . . . O1 O 0.65094(17) -0.3984(2) 0.0405(2) 0.0164(4) Uani 1 1 d . . . O2 O 0.38106(18) -0.2754(2) -0.0862(2) 0.0189(4) Uani 1 1 d . . . O3 O 0.42908(17) -0.0085(2) 0.1660(2) 0.0155(4) Uani 1 1 d . . . O4 O 0.70541(19) -0.0654(2) 0.1927(2) 0.0200(4) Uani 1 1 d D . . C1 C 0.8311(3) -0.5726(4) 0.2718(4) 0.0253(6) Uani 1 1 d . . . H1 H 0.8525 -0.6634 0.3546 0.053(12) Uiso 1 1 calc R . . C2 C 0.9287(3) -0.4706(6) 0.2318(6) 0.0540(10) Uani 1 1 d . . . H2 H 0.9105 -0.3786 0.1494 0.056(12) Uiso 1 1 calc R . . H3 H 1.0170 -0.4893 0.2854 0.099(19) Uiso 1 1 calc R . . H5 H 0.675(6) 0.061(3) 0.180(7) 0.085(17) Uiso 1 1 d D . . H4 H 0.701(4) -0.069(6) 0.324(3) 0.051(11) Uiso 1 1 d 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 Cu1 0.0213(3) 0.0072(3) 0.0136(3) -0.00259(11) -0.00107(15) 0.00134(12) P1 0.0163(3) 0.0057(3) 0.0097(3) 0.00002(18) 0.0001(2) 0.0001(2) O1 0.0277(9) 0.0092(8) 0.0130(7) 0.0026(6) 0.0046(6) 0.0027(7) O2 0.0258(9) 0.0086(8) 0.0214(8) -0.0032(6) -0.0019(7) 0.0005(7) O3 0.0251(8) 0.0087(8) 0.0131(8) -0.0009(6) 0.0042(6) 0.0008(6) O4 0.0264(9) 0.0178(9) 0.0153(8) -0.0019(6) 0.0001(7) 0.0001(7) C1 0.0225(13) 0.0246(14) 0.0273(13) -0.0010(11) -0.0054(10) 0.0029(11) C2 0.0257(16) 0.063(3) 0.071(2) 0.011(2) -0.0071(15) -0.0110(16) _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 Cu1 O1 1.9288(16) . ? Cu1 O2 1.9636(17) . ? Cu1 O3 1.9801(16) . ? Cu1 O4 2.0052(18) . ? Cu1 O3 2.2881(16) 3_655 ? P1 O2 1.5240(17) 3_645 ? P1 O1 1.5272(16) . ? P1 O3 1.5302(16) 2_645 ? P1 C1 1.782(3) . ? O2 P1 1.5240(17) 3_645 ? O3 P1 1.5302(16) 2_655 ? O3 Cu1 2.2881(16) 3_655 ? C1 C2 1.294(5) . ? 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 O1 Cu1 O2 95.75(7) . . ? O1 Cu1 O3 161.19(7) . . ? O2 Cu1 O3 88.62(7) . . ? O1 Cu1 O4 90.78(7) . . ? O2 Cu1 O4 170.87(7) . . ? O3 Cu1 O4 87.22(7) . . ? O1 Cu1 O3 112.12(6) . 3_655 ? O2 Cu1 O3 87.84(6) . 3_655 ? O3 Cu1 O3 86.28(6) . 3_655 ? O4 Cu1 O3 83.78(6) . 3_655 ? O2 P1 O1 112.14(9) 3_645 . ? O2 P1 O3 111.82(10) 3_645 2_645 ? O1 P1 O3 110.09(9) . 2_645 ? O2 P1 C1 105.97(12) 3_645 . ? O1 P1 C1 107.82(12) . . ? O3 P1 C1 108.78(11) 2_645 . ? P1 O1 Cu1 123.91(10) . . ? P1 O2 Cu1 134.02(11) 3_645 . ? P1 O3 Cu1 121.87(10) 2_655 . ? P1 O3 Cu1 142.89(10) 2_655 3_655 ? Cu1 O3 Cu1 93.72(6) . 3_655 ? C2 C1 P1 124.1(3) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 70.83 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.582 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.122 ############################################################################ data_bm5 _database_code_CSD 182286 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H3 Zn O3 P, H2 O' _chemical_formula_sum 'C2 H5 O4 P Zn' _chemical_formula_weight 189.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pmn21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 5.68050(10) _cell_length_b 9.81010(10) _cell_length_c 4.79880(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 267.419(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 425 _cell_measurement_theta_min 9.02 _cell_measurement_theta_max 69.86 _exptl_crystal_description needle _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 188 _exptl_absorpt_coefficient_mu 8.652 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3783 _exptl_absorpt_correction_T_max 0.7235 _exptl_absorpt_process_details 'DIFABS in SAINTPLUS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 6000 CCD' _diffrn_measurement_method 'CCD slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 864 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 9.02 _diffrn_reflns_theta_max 69.86 _reflns_number_total 425 _reflns_number_gt 425 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINTPLUS _computing_data_reduction SAINTPLUS _computing_structure_solution SHELXTL _computing_structure_refinement SHELXL _computing_molecular_graphics PLATON _computing_publication_material PLATON _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^)+(0.0598P)^2^+0.2712P] 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 SHELXL _refine_ls_extinction_coef 0.075(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.27(10) _refine_ls_number_reflns 425 _refine_ls_number_parameters 47 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.075 _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 Zn1 Zn 0.0000 0.52546(8) 0.8308(3) 0.0225(5) Uani 1 2 d S . . P1 P 0.0000 0.33260(14) 1.2778(3) 0.0193(6) Uani 1 2 d S . . O1 O 0.0000 0.3515(5) 1.5931(14) 0.0258(12) Uani 1 2 d S . . O3 O 0.0000 0.6842(5) 1.1375(15) 0.0276(13) Uani 1 2 d S . . O2 O 0.2148(6) 0.3969(3) 1.1327(8) 0.0267(9) Uani 1 1 d . . . C1 C 0.0000 0.1564(7) 1.202(2) 0.041(2) Uani 1 2 d SD . . H1 H 0.0000 0.1333 1.0141 0.049 Uiso 1 2 calc SR . . C2 C 0.0000 0.0554(12) 1.376(4) 0.201(17) Uani 1 2 d SD . . H2A H 0.0000 0.0721 1.5669 0.242 Uiso 1 2 calc SR . . H2B H 0.0000 -0.0337 1.3103 0.242 Uiso 1 2 calc SR . . 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 Zn1 0.0177(5) 0.0289(6) 0.0210(6) 0.0021(5) 0.000 0.000 P1 0.0158(7) 0.0208(8) 0.0211(12) 0.0003(6) 0.000 0.000 O1 0.026(2) 0.027(2) 0.024(3) 0.000(2) 0.000 0.000 O3 0.022(2) 0.030(2) 0.031(3) -0.006(2) 0.000 0.000 O2 0.0200(17) 0.0372(16) 0.0229(18) -0.0004(13) 0.0008(16) -0.0051(12) C1 0.053(4) 0.025(4) 0.044(5) -0.003(4) 0.000 0.000 C2 0.29(4) 0.049(7) 0.27(5) -0.061(19) 0.000 0.000 _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 Zn1 O2 2.027(3) 4_464 ? Zn1 O2 2.027(4) 2_564 ? Zn1 O1 2.052(5) 1_554 ? Zn1 O3 2.143(6) . ? Zn1 O2 2.275(4) . ? Zn1 O2 2.275(4) 3 ? Zn1 P1 2.8601(19) . ? P1 O1 1.525(7) . ? P1 O2 1.540(4) . ? P1 O2 1.540(4) 3 ? P1 C1 1.766(7) . ? O1 Zn1 2.052(5) 1_556 ? O2 Zn1 2.027(3) 2_565 ? C1 C2 1.296(5) . ? 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 Zn1 O2 106.1(2) 4_464 2_564 ? O2 Zn1 O1 92.96(14) 4_464 1_554 ? O2 Zn1 O1 92.96(14) 2_564 1_554 ? O2 Zn1 O3 92.82(16) 4_464 . ? O2 Zn1 O3 92.82(16) 2_564 . ? O1 Zn1 O3 170.4(3) 1_554 . ? O2 Zn1 O2 159.30(17) 4_464 . ? O2 Zn1 O2 94.48(8) 2_564 . ? O1 Zn1 O2 83.87(17) 1_554 . ? O3 Zn1 O2 88.02(18) . . ? O2 Zn1 O2 94.48(8) 4_464 3 ? O2 Zn1 O2 159.30(17) 2_564 3 ? O1 Zn1 O2 83.87(17) 1_554 3 ? O3 Zn1 O2 88.02(18) . 3 ? O2 Zn1 O2 64.86(18) . 3 ? O2 Zn1 P1 126.89(10) 4_464 . ? O2 Zn1 P1 126.89(10) 2_564 . ? O1 Zn1 P1 82.35(17) 1_554 . ? O3 Zn1 P1 88.04(19) . . ? O2 Zn1 P1 32.43(9) . . ? O2 Zn1 P1 32.43(9) 3 . ? O1 P1 O2 113.50(18) . . ? O1 P1 O2 113.50(18) . 3 ? O2 P1 O2 104.8(3) . 3 ? O1 P1 C1 108.9(4) . . ? O2 P1 C1 107.9(2) . . ? O2 P1 C1 107.9(3) 3 . ? O1 P1 Zn1 131.6(2) . . ? O2 P1 Zn1 52.41(14) . . ? O2 P1 Zn1 52.41(14) 3 . ? C1 P1 Zn1 119.5(4) . . ? P1 O1 Zn1 130.8(3) . 1_556 ? P1 O2 Zn1 125.1(2) . 2_565 ? P1 O2 Zn1 95.16(17) . . ? Zn1 O2 Zn1 121.27(16) 2_565 . ? C2 C1 P1 128.0(10) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 69.86 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.654 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.148