# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1831 data_jp01 _audit_creation_date 00-06-19 _audit_creation_method CRYSTALS_ver_07-07-97 # jp01 Jenny phosphite #**************************************************************************** #========================================================================== _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall #**************************************************************************** _cell_length_a 5.9335(3) _cell_angle_alpha 90. _cell_length_b 10.886(5) _cell_angle_beta 102.066(1) _cell_length_c 7.7611(4) _cell_angle_gamma 90. _cell_volume 490.2 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Zn ' 0.2220 1.4310 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International_Tables_Vol_IV_Table_2.2B' 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C1 H5 Zn1 P1 O3 N1 ' _chemical_formula_moiety ' C1 H5 Zn1 P1 O3 N1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 175.42 _cell_measurement_reflns_used 3479 _cell_measurement_theta_min 6.4 _cell_measurement_theta_max 65.0 _cell_measurement_temperature 298 _cell_formula_units_Z 4 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' colourless ' _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_max 0.31 _exptl_crystal_density_diffrn 2.38 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 348 _exptl_absorpt_coefficient_mu 5.22 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.543 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details SADABS _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 298 _diffrn_reflns_number 4999 _reflns_number_total 1752 _diffrn_reflns_av_R_equivalents 0.02 # Number of reflections with Friedels Law is 1752 # Number of reflections without Friedels Law is 0 _reflns_number_observed 1649 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 32.5 _reflns_limit_h_min -8 _reflns_limit_h_max 8 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 11 _reflns_observed_criterion >1.00\s(I) _refine_diff_density_min -0.40 _refine_diff_density_max 0.87 _refine_ls_number_reflns 1649 _refine_ls_number_parameters 85 _refine_ls_R_factor_obs 0.0217 _refine_ls_wR_factor_obs 0.0263 _refine_ls_goodness_of_fit_obs 1.0219 _refine_ls_shift/su_max 0.001618 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 0.552 0.439 0.353 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type Zn1 0.03319(2) 0.879144(12) 0.769487(17) 0.0164 1.0000 Uani P1 0.27766(5) 0.65160(3) 0.59762(4) 0.0159 1.0000 Uani O1 0.1754(2) 1.03914(9) 0.78564(16) 0.0323 1.0000 Uani O2 0.2524(2) 0.76399(9) 0.70734(14) 0.0267 1.0000 Uani O3 -0.0393(2) 0.8276(1) 0.99015(15) 0.0289 1.0000 Uani N1 -0.2478(2) 0.8908(1) 0.57248(16) 0.0215 1.0000 Uani C1 -0.3958(2) 0.99985(12) 0.57607(18) 0.0235 1.0000 Uani H1 0.076(4) 0.6309(18) 0.485(3) 0.023(5) 1.0000 Uiso H2 -0.196(5) 0.889(2) 0.478(4) 0.035(6) 1.0000 Uiso H3 -0.341(4) 0.825(2) 0.561(4) 0.035(6) 1.0000 Uiso H4 -0.434(5) 1.004(2) 0.689(4) 0.039(6) 1.0000 Uiso H5 -0.306(4) 1.071(3) 0.571(4) 0.039(6) 1.0000 Uiso 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 0.02082(9) 0.01316(8) 0.01675(9) 0.00063(4) 0.00732(5) 0.00145(4) P1 0.01927(13) 0.01374(13) 0.01574(12) -0.00040(9) 0.00589(9) 0.00095(9) O1 0.0507(6) 0.0183(4) 0.0343(5) -0.0085(4) 0.0234(5) -0.0110(4) O2 0.0342(5) 0.0183(4) 0.0310(5) -0.0044(3) 0.0149(4) 0.0072(3) O3 0.0403(6) 0.0265(5) 0.0262(5) 0.0063(4) 0.0214(4) 0.0083(4) N1 0.0223(5) 0.0206(4) 0.0213(5) 0.0000(3) 0.0038(4) 0.0013(3) C1 0.0231(5) 0.0233(5) 0.0227(5) -0.0011(4) 0.0016(4) 0.0045(4) _refine_ls_extinction_coef 9.4(20) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 . O1 . 1.928(1) yes Zn1 . O2 . 1.9386(9) yes Zn1 . O3 . 1.934(1) yes Zn1 . N1 . 2.0171(12) yes P1 . O1 3_546 1.514(1) yes P1 . O2 . 1.516(1) yes P1 . O3 4_564 1.518(1) yes P1 . H1 . 1.35(3) no N1 . C1 . 1.4804(17) yes N1 . H2 . 0.85(3) no N1 . H3 . 0.90(3) no C1 . C1 2_476 1.520(3) yes C1 . H4 . 0.95(3) no C1 . H5 . 0.94(3) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 . Zn1 . O2 . 107.04(5) yes O1 . Zn1 . O3 . 112.32(5) yes O2 . Zn1 . O3 . 108.53(4) yes O1 . Zn1 . N1 . 105.89(5) yes O2 . Zn1 . N1 . 110.08(5) yes O3 . Zn1 . N1 . 112.81(5) yes O1 3_546 P1 . O2 . 110.12(6) yes O1 3_546 P1 . O3 4_564 112.72(7) yes O2 . P1 . O3 4_564 110.76(6) yes O1 3_546 P1 . H1 . 106.3(9) no O2 . P1 . H1 . 108.7(9) no O3 4_564 P1 . H1 . 108.0(10) no Zn1 . O1 . P1 3_556 142.44(7) yes Zn1 . O2 . P1 . 144.29(8) yes Zn1 . O3 . P1 4_465 139.50(7) yes Zn1 . N1 . C1 . 115.84(8) yes Zn1 . N1 . H2 . 104.9(19) no C1 . N1 . H2 . 111.3(17) no Zn1 . N1 . H3 . 114.7(17) no C1 . N1 . H3 . 106.6(16) no H2 . N1 . H3 . 102.8(23) no N1 . C1 . C1 2_476 112.10(14) yes N1 . C1 . H4 . 108.5(16) no C1 2_476 C1 . H4 . 113.6(16) no N1 . C1 . H5 . 108.2(16) no C1 2_476 C1 . H5 . 109.8(17) no H4 . C1 . H5 . 104.2(24) no # end of file