Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 # 1. SUBMISSION DETAILS _publ_contact_author ; YU, Jihong State Key Lab of Inorganic Synthesis and Preparative Chemistry College of Chemistry Jilin University Changchun 130023 P. R. China ; _publ_contact_author_phone '86 431 8499161' _publ_contact_author_fax '86 431 5671974' _publ_contact_author_email jihong@mail.jlu.edu.cn _publ_requested_coeditor_name ? #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and structure of a new layered zinc phosphite (C5H6N2)Zn(HPO3) containing helical chains ; loop_ _publ_author_name _publ_author_address 'Liang, Jing' ; State Key Lab of Inorganic Synthesis and Preparative Chemistry College of Chemistry Jilin University Changchun 130023 P. R. China ; 'Wang, Yu' ; State Key Lab of Inorganic Synthesis and Preparative Chemistry College of Chemistry Jilin University Changchun 130023 P. R. China ; 'Yu, Jihong' ; Stae Key Lab of Inorganic Synthesis and Preparative Chemistry College of Chemistry Jilin University Changchun 130023 P. R. China ; 'Li, Yi' ; State Key Lab of Inorganic Synthesis and Preparative Chemistry College of Chemistry Jilin University Changchun 130023 P. R. China ; 'Xu, Ruren' ; Stae Key Lab of Inorganic Synthesis and Preparative Chemistry College of Chemistry Jilin University Changchun 130023 P. R. China ; #complex A data_a _database_code_CSD 202906 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H7 N2 O3 P Zn' _chemical_formula_weight 239.47 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' N N 0.0061 0.0033 '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' Zn Zn 0.2839 1.4301 '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 11.3477(4) _cell_length_b 7.1079(3) _cell_length_c 10.4259(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.585(2) _cell_angle_gamma 90.00 _cell_volume 781.96(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.034 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 3.309 _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 ? _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 3557 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 23.24 _reflns_number_total 1113 _reflns_number_gt 966 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _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^)+(0.1000P)^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 1113 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 0.686 _refine_ls_restrained_S_all 0.686 _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 0.12752(4) -0.96276(6) 0.70892(4) 0.0204(2) Uani 1 1 d . . . P1 P -0.14636(8) -1.13080(14) 0.58749(10) 0.0193(3) Uani 1 1 d . . . H1 H -0.234(3) -1.010(5) 0.558(4) 0.015(9) Uiso 1 1 d . . . O1 O 0.1163(2) -0.8321(4) 0.5418(3) 0.0281(6) Uani 1 1 d . . . O2 O 0.2004(2) -0.8060(4) 0.8720(3) 0.0275(7) Uani 1 1 d . . . O3 O -0.0337(3) -1.0529(4) 0.7061(3) 0.0323(7) Uani 1 1 d . . . C1 C 0.2463(3) -1.3291(5) 0.6653(4) 0.0239(9) Uani 1 1 d . . . C2 C 0.3461(4) -1.4631(6) 0.7003(5) 0.0303(10) Uani 1 1 d . . . H2 H 0.339(4) -1.559(7) 0.645(5) 0.039(14) Uiso 1 1 d . . . C3 C 0.4521(4) -1.4380(6) 0.8147(4) 0.0317(10) Uani 1 1 d . . . H3 H 0.517(4) -1.518(6) 0.840(5) 0.036(13) Uiso 1 1 d . . . C4 C 0.4615(4) -1.2801(6) 0.8987(5) 0.0313(10) Uani 1 1 d . . . H4 H 0.534(4) -1.254(5) 0.983(4) 0.019(9) Uiso 1 1 d . . . C5 C 0.3640(4) -1.1574(6) 0.8610(4) 0.0291(10) Uani 1 1 d . . . H5 H 0.365(4) -1.057(6) 0.912(4) 0.024(11) Uiso 1 1 d . . . N1 N 0.2571(3) -1.1756(4) 0.7453(3) 0.0228(7) Uani 1 1 d . . . N2 N 0.1435(4) -1.3505(6) 0.5499(4) 0.0330(9) Uani 1 1 d . . . H6 H 0.137(4) -1.436(6) 0.507(5) 0.018(13) Uiso 1 1 d . . . H7 H 0.085(4) -1.288(6) 0.538(4) 0.018(12) Uiso 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 Zn1 0.0235(3) 0.0243(3) 0.0129(3) -0.00162(17) 0.0062(2) 0.00015(17) P1 0.0215(5) 0.0226(6) 0.0141(5) 0.0011(4) 0.0068(4) -0.0001(4) O1 0.0355(15) 0.0352(16) 0.0165(14) 0.0021(12) 0.0131(12) 0.0011(13) O2 0.0287(14) 0.0338(16) 0.0155(14) -0.0073(12) 0.0030(12) 0.0055(12) O3 0.0283(15) 0.0481(19) 0.0202(16) -0.0070(13) 0.0086(13) -0.0128(13) C1 0.030(2) 0.027(2) 0.018(2) 0.0003(17) 0.0119(18) -0.0004(17) C2 0.036(2) 0.028(3) 0.030(3) -0.002(2) 0.016(2) 0.0053(19) C3 0.030(2) 0.040(3) 0.027(3) 0.011(2) 0.013(2) 0.014(2) C4 0.027(2) 0.037(3) 0.027(2) 0.004(2) 0.006(2) -0.0004(19) C5 0.029(2) 0.029(2) 0.027(2) -0.006(2) 0.0069(19) -0.0044(19) N1 0.0286(17) 0.0221(18) 0.0179(17) 0.0009(14) 0.0086(14) 0.0025(13) N2 0.034(2) 0.032(2) 0.027(2) -0.0097(19) 0.0049(18) 0.0069(19) _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 O3 1.929(3) . ? Zn1 O1 1.936(3) . ? Zn1 O2 1.945(3) . ? Zn1 N1 2.045(3) . ? P1 O2 1.515(3) 2_546 ? P1 O3 1.519(3) . ? P1 O1 1.531(3) 3_536 ? P1 H1 1.26(3) . ? O1 P1 1.531(3) 3_536 ? O2 P1 1.515(3) 2_556 ? C1 N2 1.342(5) . ? C1 N1 1.351(5) . ? C1 C2 1.421(6) . ? C2 C3 1.359(6) . ? C2 H2 0.87(5) . ? C3 C4 1.403(6) . ? C3 H3 0.89(5) . ? C4 C5 1.349(6) . ? C4 H4 0.97(4) . ? C5 N1 1.366(5) . ? C5 H5 0.88(4) . ? N2 H6 0.74(4) . ? N2 H7 0.77(4) . ? 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 O3 Zn1 O1 113.43(11) . . ? O3 Zn1 O2 107.43(12) . . ? O1 Zn1 O2 112.20(13) . . ? O3 Zn1 N1 111.74(13) . . ? O1 Zn1 N1 109.06(12) . . ? O2 Zn1 N1 102.46(11) . . ? O2 P1 O3 112.23(15) 2_546 . ? O2 P1 O1 110.39(16) 2_546 3_536 ? O3 P1 O1 112.75(16) . 3_536 ? O2 P1 H1 105.2(16) 2_546 . ? O3 P1 H1 107.6(16) . . ? O1 P1 H1 108.3(17) 3_536 . ? P1 O1 Zn1 138.40(18) 3_536 . ? P1 O2 Zn1 128.96(15) 2_556 . ? P1 O3 Zn1 129.99(18) . . ? N2 C1 N1 119.8(4) . . ? N2 C1 C2 120.1(4) . . ? N1 C1 C2 120.0(3) . . ? C3 C2 C1 120.1(4) . . ? C3 C2 H2 121(3) . . ? C1 C2 H2 119(3) . . ? C2 C3 C4 119.5(4) . . ? C2 C3 H3 123(3) . . ? C4 C3 H3 117(3) . . ? C5 C4 C3 118.0(4) . . ? C5 C4 H4 118(2) . . ? C3 C4 H4 124(2) . . ? C4 C5 N1 124.3(4) . . ? C4 C5 H5 121(3) . . ? N1 C5 H5 115(3) . . ? C1 N1 C5 118.1(3) . . ? C1 N1 Zn1 125.9(2) . . ? C5 N1 Zn1 116.0(3) . . ? C1 N2 H6 119(3) . . ? C1 N2 H7 119(3) . . ? H6 N2 H7 119(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H6 O2 0.74(4) 2.57(5) 3.271(6) 158(4) 4_535 N2 H7 O1 0.77(4) 2.29(4) 3.036(5) 163(4) 3_536 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.390 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.117