# 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 loop_ _publ_author_name 'Clearfield, A.' 'Mao, Jiang-Gao' 'Wang, Zhike' _publ_contact_author_name 'Prof A Clearfield' _publ_contact_author_address ; Department of Chemistry Texas A & M University College Station TEXAS TX 77843 U S A ; _publ_contact_author_email 'CLEARFIELD@MAIL.CHEM.TAMU.EDU' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Hydrothermal Synthesis, Characterization and Crystal Structures of two New Zinc(II) Phosphonates: Zn2{(O3PCH2 )2NHCH2CO2} and Zn2{ HO3PCH2NH(CH2PO3)2} ; data_maoc7 _database_code_CSD 187598 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H8 N O9 P3 Zn2' _chemical_formula_weight 425.75 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 Hexagonal _symmetry_space_group_name_H-M P6(1) _symmetry_Int_Tables_number 169 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' '-x, -y, z+1/2' 'y, -x+y, z+5/6' 'x-y, x, z+1/6' _cell_length_a 8.3553(8) _cell_length_b 8.3553(8) _cell_length_c 26.657(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1611.6(3) _cell_formula_units_Z 6 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 4.952 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.636 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker Smart CCD' _diffrn_measurement_method 'narrow frame method, hemisphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0% _diffrn_reflns_number 9968 _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_sigmaI/netI 0.0911 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 28.28 _reflns_number_total 2599 _reflns_number_gt 2051 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+19.9217P] 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 0.0019(2) _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 0.04(3) _refine_ls_number_reflns 2599 _refine_ls_number_parameters 161 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1269 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.001 _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 0.1909(2) 0.0042(2) 0.10793(6) 0.0215(4) Uani 0.896(5) 1 d P . . Zn1' Zn 0.028(2) -0.178(2) 0.0925(6) 0.038(5) Uani 0.104(5) 1 d P . . Zn2 Zn 0.30538(16) -0.52296(17) 0.01613(4) 0.0124(3) Uani 1 1 d . . . P1 P 0.3215(5) -0.1437(4) 0.00821(13) 0.0253(8) Uani 1 1 d D . . P2 P 0.7129(4) 0.5317(4) 0.02098(19) 0.0283(8) Uani 1 1 d D . . P3 P 0.9397(4) 0.1816(4) 0.08094(10) 0.0108(5) Uani 1 1 d D . . N1 N 0.6704(11) 0.1787(11) 0.0179(4) 0.024(2) Uani 1 1 d D . . H11A H 0.6211 0.1821 0.0480 0.029 Uiso 1 1 calc R . . C1 C 0.5138(15) 0.0657(15) -0.0172(5) 0.029(3) Uiso 1 1 d D . . H1A H 0.5626 0.0319 -0.0458 0.034 Uiso 1 1 calc R . . H1B H 0.4664 0.1431 -0.0296 0.034 Uiso 1 1 calc R . . C2 C 0.7857(15) 0.3744(14) -0.0004(4) 0.020(2) Uiso 1 1 d D . . H2A H 0.7846 0.3736 -0.0367 0.024 Uiso 1 1 calc R . . H2B H 0.9123 0.4207 0.0103 0.024 Uiso 1 1 calc R . . C3 C 0.7909(15) 0.0898(15) 0.0261(4) 0.019(3) Uani 1 1 d D . . H3A H 0.8670 0.1106 -0.0034 0.023 Uiso 1 1 calc R . . H3B H 0.7115 -0.0425 0.0301 0.023 Uiso 1 1 calc R . . O1 O 0.199(3) -0.124(3) 0.0553(8) 0.037(5) Uiso 0.50 1 d P . . O1' O 0.255(3) -0.050(3) 0.0402(8) 0.035(5) Uiso 0.50 1 d P . . O2 O 0.3957(11) -0.2603(10) 0.0296(3) 0.0180(17) Uani 1 1 d . . . O3 O 0.1952(12) -0.2350(12) -0.0362(4) 0.037(3) Uani 1 1 d . . . O4 O 0.5073(10) 0.4293(10) 0.0254(3) 0.0181(18) Uani 1 1 d . . . O5 O 0.818(2) 0.712(2) 0.0005(6) 0.020(3) Uiso 0.50 1 d P . . O5' O 0.766(2) 0.671(2) -0.0288(6) 0.022(4) Uiso 0.50 1 d P . . O6 O 0.775(2) 0.556(2) 0.0849(7) 0.024(4) Uiso 0.50 1 d P . . O6' O 0.814(2) 0.625(2) 0.0642(7) 0.024(4) Uiso 0.50 1 d P . . O7 O 0.8148(10) 0.2086(10) 0.1176(3) 0.0178(17) Uani 1 1 d . . . O8 O 1.1120(10) 0.3625(10) 0.0656(3) 0.0166(16) Uani 1 1 d . . . O9 O 0.9819(10) 0.0356(10) 0.0975(3) 0.0171(17) 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 Zn1 0.0105(7) 0.0115(7) 0.0413(10) 0.0034(7) -0.0065(7) 0.0045(6) Zn1' 0.035(9) 0.040(10) 0.037(10) -0.003(8) 0.003(8) 0.018(8) Zn2 0.0136(6) 0.0126(6) 0.0112(5) 0.0004(5) 0.0010(5) 0.0067(5) P1 0.0313(18) 0.0207(16) 0.033(2) -0.0154(15) -0.0189(15) 0.0197(15) P2 0.0146(15) 0.0086(14) 0.062(2) 0.0029(15) 0.0132(17) 0.0057(12) P3 0.0112(13) 0.0118(13) 0.0090(12) 0.0012(11) -0.0006(10) 0.0054(11) N1 0.015(5) 0.015(5) 0.040(6) 0.015(5) 0.006(5) 0.007(4) C3 0.025(6) 0.009(5) 0.020(6) 0.002(4) 0.003(5) 0.005(5) O2 0.020(4) 0.020(4) 0.016(4) 0.004(3) -0.007(3) 0.012(4) O3 0.029(5) 0.020(5) 0.061(7) -0.012(4) -0.028(5) 0.010(4) O4 0.013(4) 0.015(4) 0.022(4) 0.000(3) -0.001(3) 0.004(3) O7 0.010(4) 0.021(4) 0.020(4) 0.000(3) -0.001(3) 0.005(3) O8 0.018(4) 0.016(4) 0.012(4) 0.001(3) 0.003(3) 0.006(3) O9 0.024(4) 0.018(4) 0.015(4) 0.012(3) 0.003(3) 0.015(3) _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 Zn1' 1.503(17) . ? Zn1 O1 1.79(2) . ? Zn1 O5' 1.908(16) 6_545 ? Zn1 O9 1.912(7) 1_455 ? Zn1 O3 1.928(9) 6 ? Zn1 O1' 2.00(2) . ? Zn1 O5 2.077(16) 6_545 ? Zn1' O5' 1.50(2) 6_545 ? Zn1' O1 1.61(3) . ? Zn1' O6' 1.88(2) 1_445 ? Zn1' O9 2.010(19) 1_455 ? Zn1' O5 2.10(2) 6_545 ? Zn1' O1' 2.16(3) . ? Zn1' O6 2.18(2) 1_445 ? Zn2 O7 1.896(8) 5_554 ? Zn2 O8 1.928(7) 1_445 ? Zn2 O4 1.934(8) 1_545 ? Zn2 O2 1.964(8) . ? P1 O1' 1.44(2) . ? P1 O2 1.504(8) . ? P1 O3 1.514(9) . ? P1 O1 1.68(2) . ? P1 C1 1.814(11) . ? P2 O6' 1.411(17) . ? P2 O5 1.420(15) . ? P2 O4 1.492(8) . ? P2 O5' 1.674(17) . ? P2 O6 1.762(18) . ? P2 C2 1.794(10) . ? P3 O9 1.496(7) . ? P3 O7 1.526(8) . ? P3 O8 1.532(8) . ? P3 C3 1.821(10) . ? N1 C1 1.498(12) . ? N1 C2 1.505(11) . ? N1 C3 1.537(12) . ? O1 O1' 0.69(2) . ? O3 Zn1 1.928(9) 5_554 ? O4 Zn2 1.934(8) 1_565 ? O5 O5' 0.87(2) . ? O5 Zn1 2.077(16) 5_664 ? O5 Zn1' 2.10(2) 5_664 ? O5' Zn1' 1.50(2) 5_664 ? O5' Zn1 1.908(16) 5_664 ? O6 O6' 0.74(2) . ? O6 Zn1' 2.18(2) 1_665 ? O6' Zn1' 1.88(2) 1_665 ? O7 Zn2 1.896(8) 6 ? O8 Zn2 1.928(7) 1_665 ? O9 Zn1 1.912(7) 1_655 ? O9 Zn1' 2.010(19) 1_655 ? 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 Zn1' Zn1 O1 57.7(9) . . ? Zn1' Zn1 O5' 50.5(8) . 6_545 ? O1 Zn1 O5' 80.0(9) . 6_545 ? Zn1' Zn1 O9 71.0(7) . 1_455 ? O1 Zn1 O9 106.3(7) . 1_455 ? O5' Zn1 O9 105.5(5) 6_545 1_455 ? Zn1' Zn1 O3 164.0(7) . 6 ? O1 Zn1 O3 113.9(7) . 6 ? O5' Zn1 O3 117.0(6) 6_545 6 ? O9 Zn1 O3 124.9(4) 1_455 6 ? Zn1' Zn1 O1' 74.4(8) . . ? O1 Zn1 O1' 19.9(8) . . ? O5' Zn1 O1' 99.3(8) 6_545 . ? O9 Zn1 O1' 105.5(6) 1_455 . ? O3 Zn1 O1' 100.6(7) 6 . ? Zn1' Zn1 O5 69.8(8) . 6_545 ? O1 Zn1 O5 104.4(8) . 6_545 ? O5' Zn1 O5 24.9(6) 6_545 6_545 ? O9 Zn1 O5 102.7(5) 1_455 6_545 ? O3 Zn1 O5 102.0(6) 6 6_545 ? O1' Zn1 O5 123.1(7) . 6_545 ? O5' Zn1' Zn1 78.8(10) 6_545 . ? O5' Zn1' O1 99.7(14) 6_545 . ? Zn1 Zn1' O1 70.1(10) . . ? O5' Zn1' O6' 112.9(13) 6_545 1_445 ? Zn1 Zn1' O6' 168.0(13) . 1_445 ? O1 Zn1' O6' 108.8(12) . 1_445 ? O5' Zn1' O9 119.2(12) 6_545 1_455 ? Zn1 Zn1' O9 64.1(7) . 1_455 ? O1 Zn1' O9 109.5(12) . 1_455 ? O6' Zn1' O9 106.3(10) 1_445 1_455 ? O5' Zn1' O5 20.7(8) 6_545 6_545 ? Zn1 Zn1' O5 68.1(7) . 6_545 ? O1 Zn1' O5 110.5(13) . 6_545 ? O6' Zn1' O5 122.1(11) 1_445 6_545 ? O9 Zn1' O5 98.6(8) 1_455 6_545 ? O5' Zn1' O1' 107.8(12) 6_545 . ? Zn1 Zn1' O1' 63.4(8) . . ? O1 Zn1' O1' 12.8(9) . . ? O6' Zn1' O1' 113.0(11) 1_445 . ? O9 Zn1' O1' 96.8(9) 1_455 . ? O5 Zn1' O1' 114.8(10) 6_545 . ? O5' Zn1' O6 94.5(11) 6_545 1_445 ? Zn1 Zn1' O6 168.9(11) . 1_445 ? O1 Zn1' O6 120.1(13) . 1_445 ? O6' Zn1' O6 19.3(6) 1_445 1_445 ? O9 Zn1' O6 112.9(9) 1_455 1_445 ? O5 Zn1' O6 102.8(9) 6_545 1_445 ? O1' Zn1' O6 127.5(10) . 1_445 ? O7 Zn2 O8 110.3(3) 5_554 1_445 ? O7 Zn2 O4 107.3(3) 5_554 1_545 ? O8 Zn2 O4 114.3(3) 1_445 1_545 ? O7 Zn2 O2 115.7(3) 5_554 . ? O8 Zn2 O2 100.8(3) 1_445 . ? O4 Zn2 O2 108.6(3) 1_545 . ? O1' P1 O2 121.4(9) . . ? O1' P1 O3 112.1(9) . . ? O2 P1 O3 112.3(5) . . ? O1' P1 O1 24.0(9) . . ? O2 P1 O1 104.3(8) . . ? O3 P1 O1 109.2(9) . . ? O1' P1 C1 95.4(10) . . ? O2 P1 C1 108.3(6) . . ? O3 P1 C1 104.6(6) . . ? O1 P1 C1 118.3(8) . . ? O6' P2 O5 81.1(10) . . ? O6' P2 O4 116.8(8) . . ? O5 P2 O4 124.3(7) . . ? O6' P2 O5' 112.6(9) . . ? O5 P2 O5' 31.5(8) . . ? O4 P2 O5' 106.9(7) . . ? O6' P2 O6 24.0(8) . . ? O5 P2 O6 104.9(9) . . ? O4 P2 O6 100.2(7) . . ? O5' P2 O6 136.4(8) . . ? O6' P2 C2 109.7(8) . . ? O5 P2 C2 113.5(8) . . ? O4 P2 C2 108.6(5) . . ? O5' P2 C2 101.0(7) . . ? O6 P2 C2 101.8(7) . . ? O9 P3 O7 112.9(5) . . ? O9 P3 O8 113.3(4) . . ? O7 P3 O8 113.6(4) . . ? O9 P3 C3 106.4(5) . . ? O7 P3 C3 101.7(5) . . ? O8 P3 C3 107.9(5) . . ? C1 N1 C2 111.5(9) . . ? C1 N1 C3 111.2(9) . . ? C2 N1 C3 110.7(8) . . ? N1 C1 P1 116.6(8) . . ? N1 C2 P2 115.2(7) . . ? N1 C3 P3 112.7(7) . . ? O1' O1 Zn1' 136(3) . . ? O1' O1 P1 58(3) . . ? Zn1' O1 P1 159.1(16) . . ? O1' O1 Zn1 98(3) . . ? Zn1' O1 Zn1 52.2(9) . . ? P1 O1 Zn1 148.7(14) . . ? O1 O1' P1 98(3) . . ? O1 O1' Zn1 62(3) . . ? P1 O1' Zn1 151.3(14) . . ? O1 O1' Zn1' 31(2) . . ? P1 O1' Zn1' 126.6(14) . . ? Zn1 O1' Zn1' 42.2(6) . . ? P1 O2 Zn2 127.0(5) . . ? P1 O3 Zn1 125.5(6) . 5_554 ? P2 O4 Zn2 138.1(5) . 1_565 ? O5' O5 P2 90.5(17) . . ? O5' O5 Zn1 66.6(15) . 5_664 ? P2 O5 Zn1 131.6(10) . 5_664 ? O5' O5 Zn1' 37.3(14) . 5_664 ? P2 O5 Zn1' 127.6(11) . 5_664 ? Zn1 O5 Zn1' 42.2(6) 5_664 5_664 ? O5 O5' Zn1' 122(2) . 5_664 ? O5 O5' P2 58.0(14) . . ? Zn1' O5' P2 176.7(13) 5_664 . ? O5 O5' Zn1 88.5(16) . 5_664 ? Zn1' O5' Zn1 50.6(8) 5_664 5_664 ? P2 O5' Zn1 126.6(9) . 5_664 ? O6' O6 P2 50.5(18) . . ? O6' O6 Zn1' 56.9(19) . 1_665 ? P2 O6 Zn1' 106.7(9) . 1_665 ? O6 O6' P2 105(2) . . ? O6 O6' Zn1' 104(2) . 1_665 ? P2 O6' Zn1' 148.8(13) . 1_665 ? P3 O7 Zn2 138.6(5) . 6 ? P3 O8 Zn2 144.4(5) . 1_665 ? P3 O9 Zn1 139.4(5) . 1_655 ? P3 O9 Zn1' 158.8(7) . 1_655 ? Zn1 O9 Zn1' 45.0(5) 1_655 1_655 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.246 _refine_diff_density_min -1.231 _refine_diff_density_rms 0.259 data_maoc6 _database_code_CSD 187599 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H7 N O8 P2 Zn2' _chemical_formula_weight 389.79 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 Hexagonal _symmetry_space_group_name_H-M P6(1) _symmetry_Int_Tables_number 169 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' '-x, -y, z+1/2' 'y, -x+y, z+5/6' 'x-y, x, z+1/6' _cell_length_a 8.0677(12) _cell_length_b 8.0677(12) _cell_length_c 27.283(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1537.9(5) _cell_formula_units_Z 6 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 5.021 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 1.000 _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_% <1.0% _diffrn_reflns_number 3597 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0891 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1851 _reflns_number_gt 1380 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0435P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_number_reflns 1851 _refine_ls_number_parameters 154 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.954 _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 0.79044(15) 0.98467(15) 0.08961(3) 0.0216(3) Uani 1 1 d . . . Zn2 Zn 0.46793(15) 0.32374(14) 0.01164(3) 0.0209(3) Uani 1 1 d . . . P1 P -0.1485(3) 0.3218(3) 0.02380(8) 0.0211(5) Uani 1 1 d . . . P2 P 0.1742(3) 0.9495(3) -0.05545(8) 0.0205(5) Uani 1 1 d . . . O1 O -0.0669(10) 0.2381(10) -0.0110(3) 0.0324(16) Uani 1 1 d . . . O2 O -0.2726(9) 0.3879(9) -0.0014(2) 0.0244(14) Uani 1 1 d . . . O3 O -0.2500(8) 0.1895(8) 0.0671(2) 0.0234(14) Uani 1 1 d . . . O4 O 0.0070(9) 0.9697(8) -0.0747(3) 0.0259(15) Uani 1 1 d . . . O5 O 0.3443(9) 1.1383(8) -0.0403(2) 0.0248(14) Uani 1 1 d . . . O6 O 0.2252(10) 0.8346(9) -0.0892(2) 0.0313(16) Uani 1 1 d . . . O7 O 0.4047(9) 0.5304(9) 0.0025(2) 0.0240(14) Uani 1 1 d . . . O8 O 0.6398(9) 0.7537(9) 0.0480(2) 0.0281(14) Uani 1 1 d . . . N1 N 0.1722(10) 0.6775(10) 0.0094(3) 0.0183(16) Uani 1 1 d . . . H11A H 0.1696 0.6134 -0.0183 0.022 Uiso 1 1 calc R . . C1 C 0.0594(12) 0.5335(12) 0.0484(3) 0.021(2) Uani 1 1 d . . . H1A H 0.0173 0.5926 0.0726 0.026 Uiso 1 1 calc R . . H1B H 0.1416 0.4952 0.0648 0.026 Uiso 1 1 calc R . . C2 C 0.0823(13) 0.7992(12) -0.0019(3) 0.0190(18) Uani 1 1 d . . . H2A H 0.1003 0.8801 0.0262 0.023 Uiso 1 1 calc R . . H2B H -0.0543 0.7151 -0.0061 0.023 Uiso 1 1 calc R . . C3 C 0.3758(13) 0.8006(12) 0.0248(3) 0.025(2) Uani 1 1 d . . . H3A H 0.3798 0.8517 0.0572 0.030 Uiso 1 1 calc R . . H3B H 0.4392 0.9076 0.0023 0.030 Uiso 1 1 calc R . . C4 C 0.4849(12) 0.6871(13) 0.0255(3) 0.021(2) 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 Zn1 0.0242(6) 0.0240(6) 0.0164(5) -0.0002(4) -0.0006(4) 0.0120(5) Zn2 0.0231(6) 0.0240(6) 0.0156(5) -0.0004(4) -0.0004(4) 0.0118(5) P1 0.0222(12) 0.0229(13) 0.0169(11) 0.0007(10) 0.0011(10) 0.0104(11) P2 0.0255(12) 0.0243(12) 0.0119(9) -0.0013(9) -0.0015(9) 0.0126(11) O1 0.037(4) 0.032(4) 0.028(3) 0.001(3) 0.008(3) 0.018(3) O2 0.025(3) 0.032(4) 0.018(3) -0.002(3) -0.002(3) 0.016(3) O3 0.022(3) 0.020(3) 0.028(3) 0.001(3) -0.003(3) 0.010(3) O4 0.028(3) 0.024(3) 0.029(3) -0.005(3) -0.012(3) 0.015(3) O5 0.030(3) 0.024(3) 0.019(3) -0.004(3) -0.008(3) 0.012(3) O6 0.043(4) 0.029(4) 0.025(3) 0.001(3) 0.002(3) 0.019(3) O7 0.023(3) 0.027(3) 0.024(4) 0.008(3) -0.001(3) 0.014(3) O8 0.028(4) 0.033(4) 0.025(3) -0.005(3) -0.007(3) 0.016(3) N1 0.030(4) 0.019(4) 0.008(3) 0.002(3) -0.002(3) 0.014(4) C1 0.020(5) 0.023(5) 0.022(4) 0.011(4) 0.003(4) 0.013(4) C2 0.025(5) 0.018(4) 0.019(4) -0.001(3) 0.001(4) 0.015(4) C3 0.029(5) 0.020(5) 0.022(5) -0.004(4) -0.008(4) 0.010(4) C4 0.021(5) 0.021(5) 0.019(4) 0.001(4) -0.001(4) 0.008(4) _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 O4 1.909(6) 6_765 ? Zn1 O1 1.922(7) 6_665 ? Zn1 O3 1.937(6) 1_665 ? Zn1 O8 1.992(7) . ? Zn2 O2 1.922(6) 1_655 ? Zn2 O5 1.936(6) 1_545 ? Zn2 O6 1.937(6) 6_655 ? Zn2 O7 1.988(6) . ? P1 O1 1.495(7) . ? P1 O2 1.515(6) . ? P1 O3 1.528(7) . ? P1 C1 1.821(9) . ? P2 O6 1.503(7) . ? P2 O5 1.511(6) . ? P2 O4 1.530(7) . ? P2 C2 1.804(9) . ? O1 Zn1 1.922(7) 5_454 ? O2 Zn2 1.922(6) 1_455 ? O3 Zn1 1.937(6) 1_445 ? O4 Zn1 1.909(6) 5_464 ? O5 Zn2 1.936(6) 1_565 ? O6 Zn2 1.937(6) 5_564 ? O7 C4 1.263(10) . ? O8 C4 1.247(10) . ? N1 C3 1.493(11) . ? N1 C1 1.501(10) . ? N1 C2 1.516(10) . ? C3 C4 1.556(13) . ? 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 O4 Zn1 O1 106.0(3) 6_765 6_665 ? O4 Zn1 O3 122.9(3) 6_765 1_665 ? O1 Zn1 O3 105.2(3) 6_665 1_665 ? O4 Zn1 O8 103.1(3) 6_765 . ? O1 Zn1 O8 109.9(3) 6_665 . ? O3 Zn1 O8 109.5(3) 1_665 . ? O2 Zn2 O5 98.2(3) 1_655 1_545 ? O2 Zn2 O6 111.5(3) 1_655 6_655 ? O5 Zn2 O6 115.2(3) 1_545 6_655 ? O2 Zn2 O7 116.9(3) 1_655 . ? O5 Zn2 O7 107.9(3) 1_545 . ? O6 Zn2 O7 107.2(3) 6_655 . ? O1 P1 O2 112.9(4) . . ? O1 P1 O3 112.3(4) . . ? O2 P1 O3 112.3(3) . . ? O1 P1 C1 104.5(4) . . ? O2 P1 C1 107.4(4) . . ? O3 P1 C1 106.9(4) . . ? O6 P2 O5 113.5(4) . . ? O6 P2 O4 112.5(4) . . ? O5 P2 O4 113.0(4) . . ? O6 P2 C2 103.2(4) . . ? O5 P2 C2 108.5(4) . . ? O4 P2 C2 105.2(4) . . ? P1 O1 Zn1 149.7(5) . 5_454 ? P1 O2 Zn2 130.1(4) . 1_455 ? P1 O3 Zn1 125.5(4) . 1_445 ? P2 O4 Zn1 128.2(4) . 5_464 ? P2 O5 Zn2 146.7(4) . 1_565 ? P2 O6 Zn2 137.8(4) . 5_564 ? C4 O7 Zn2 124.0(6) . . ? C4 O8 Zn1 134.0(6) . . ? C3 N1 C1 110.8(7) . . ? C3 N1 C2 110.5(6) . . ? C1 N1 C2 110.2(6) . . ? N1 C1 P1 112.5(6) . . ? N1 C2 P2 115.6(6) . . ? N1 C3 C4 111.7(7) . . ? O8 C4 O7 125.3(9) . . ? O8 C4 C3 119.5(8) . . ? O7 C4 C3 115.1(8) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.303 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.172