Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Abrahams, Brendan F.' 'Chen, Zhen-Feng' 'Fun, Hoong-Kun' 'You, Xiao-Zeng' 'Zhang, Jing' _publ_contact_author_name 'Prof Xiao-Zeng You' _publ_contact_author_address ; Prof Xiao-Zeng You Coordination Chemistry Inst, State Key Laboratory of Coordination Chemistry Nanjing University Nanjing 210093 CHINA ; _publ_contact_author_email 'xyz@netra.nju.edu.cn' _publ_contact_author_fax '86-25-3317761' _publ_contact_author_phone '86-25-3594724' _publ_section_title ; The First Four-fold Interpenetrating Diamondoid Framework That Traps Gaseous trans-2-Butene Molecules:{Zn(4-pyac)~2~dotB}~n~(4-pyac=4-pyridylacrilate, and B=trans-2-Butene ; _publ_section_references ; Allen, F.H., Kennard, O., Watson, D.G., Brammer, L., Orpen, A.G. & Taylor, R. (1987). Chem. Soc. Perkin Trans. II, S1-S19. Nardelli, M. (1995). J. Appl. Cryst. 28, 659. Orpen, A.G., Brammer, L., Allen, F.H., Kennard, O., Watson, D.G. & Taylor, R. (1989). J. Chem. Soc. Dalton Trans., S1-S83. Siemens (1996). SMART and SAINT. Area Detector Control and Integration Software. Siemens Analytical X-Ray Systems, Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data, University of G\"ottingen, Germany. Sheldrick, G.M. (1997). SHELXTL V5.1 Software Reference Manual, Bruker AXS, Inc., Madison, Wisconsin, USA. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_exptl_refinement ; The data collection covered over a hemisphere of reciprocal space by a combination of three sets of exposures; each set had a different \f angle (0, 88 and 180\%) for the crystal and each exposure of 10s covered 0.3\% in \w. The crystal-to-detector distance was 4 cm and the detector swing angle was -35\%. Coverage of the unique set is over 99% complete. Crystal decay was monitored by repeating fifty initial frames at the end of data collection and analysing the duplicate reflections, and was found to be negligible. ; #============================================================================ data_1 _database_code_CSD 156501 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H20 N2 O4 Zn' _chemical_formula_weight 417.75 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 12.471(1) _cell_length_b 13.804(1) _cell_length_c 12.005(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2066.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 4.94 _cell_measurement_theta_max 9.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 1.214 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6830 _exptl_absorpt_correction_T_max 0.7933 _exptl_absorpt_process_details '\y scans using XSCANS (Siemens, 1994)' _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 'Siemens P4 diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 3' _diffrn_reflns_number 3063 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2378 _reflns_number_gt 1279 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'XSCANS (Siemens, 1994)' _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _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^)+(0.0701P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2378 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1353 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 0.871 _refine_ls_restrained_S_all 0.871 _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 0.7500 0.0000 0.19654(5) 0.02927(19) Uani 1 2 d S . . O1 O 0.6015(4) 0.0305(3) 0.3492(4) 0.1044(19) Uani 1 1 d . . . O2 O 0.6557(2) -0.0987(2) 0.2628(3) 0.0434(7) Uani 1 1 d . . . N1 N 0.3251(3) -0.4068(2) 0.5868(3) 0.0351(8) Uani 1 1 d . . . C1 C 0.3871(4) -0.2466(3) 0.5511(4) 0.0604(15) Uani 1 1 d . . . H1B H 0.3862 -0.1815 0.5710 0.072 Uiso 1 1 calc R . . C2 C 0.3264(4) -0.3119(3) 0.6095(4) 0.0576(14) Uani 1 1 d . . . H2A H 0.2841 -0.2892 0.6677 0.069 Uiso 1 1 calc R . . C3 C 0.3803(4) -0.4358(3) 0.4988(4) 0.0450(11) Uani 1 1 d . . . H3A H 0.3770 -0.5007 0.4784 0.054 Uiso 1 1 calc R . . C4 C 0.4426(4) -0.3738(3) 0.4357(4) 0.0490(12) Uani 1 1 d . . . H4A H 0.4801 -0.3976 0.3746 0.059 Uiso 1 1 calc R . . C5 C 0.4494(4) -0.2770(3) 0.4629(4) 0.0396(10) Uani 1 1 d . . . C6 C 0.5206(4) -0.2127(3) 0.3979(3) 0.0434(11) Uani 1 1 d . . . H6A H 0.5663 -0.2422 0.3470 0.052 Uiso 1 1 calc R . . C7 C 0.5255(4) -0.1175(3) 0.4054(4) 0.0531(13) Uani 1 1 d . . . H7A H 0.4806 -0.0863 0.4559 0.064 Uiso 1 1 calc R . . C8 C 0.5998(4) -0.0574(3) 0.3366(4) 0.0471(13) Uani 1 1 d . . . C9 C 0.336(2) 0.2091(19) 0.258(7) 0.36(2) Uani 1 1 d . . . H9A H 0.2617 0.2046 0.2633 0.431 Uiso 1 1 d R . . C10 C 0.3473(18) 0.1097(12) 0.263(2) 0.296(12) Uani 1 1 d . . . H10A H 0.3331 0.0887 0.3382 0.445 Uiso 1 1 d R . . H10B H 0.4202 0.0947 0.2443 0.445 Uiso 1 1 d R . . H10C H 0.2997 0.0770 0.2131 0.445 Uiso 1 1 d R . . 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 0.0306(3) 0.0253(3) 0.0319(3) 0.000 0.000 -0.0014(4) O1 0.144(4) 0.0405(18) 0.129(4) -0.024(2) 0.094(4) -0.032(2) O2 0.0471(17) 0.0394(15) 0.0438(16) -0.0015(14) 0.0169(16) -0.0111(15) N1 0.0371(19) 0.0303(15) 0.0380(18) 0.0004(15) 0.0079(17) -0.0029(16) C1 0.092(4) 0.030(2) 0.059(3) -0.014(2) 0.033(3) -0.017(3) C2 0.086(4) 0.039(2) 0.048(3) -0.014(2) 0.034(3) -0.019(3) C3 0.053(3) 0.032(2) 0.051(3) -0.003(2) 0.017(2) 0.000(2) C4 0.063(3) 0.040(2) 0.044(3) -0.006(2) 0.020(2) -0.001(2) C5 0.045(2) 0.036(2) 0.038(2) -0.0002(19) 0.008(2) -0.003(2) C6 0.048(3) 0.045(2) 0.038(3) -0.003(2) 0.015(2) -0.005(2) C7 0.065(3) 0.041(2) 0.053(3) -0.008(2) 0.028(3) -0.010(2) C8 0.058(3) 0.038(2) 0.045(3) 0.000(2) 0.014(3) -0.012(2) C9 0.239(18) 0.32(6) 0.52(4) -0.06(9) -0.04(4) 0.04(3) C10 0.28(2) 0.25(2) 0.36(2) 0.02(2) -0.17(2) -0.04(2) _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 1.968(3) 2_655 ? Zn1 O2 1.968(3) . ? Zn1 N1 2.066(3) 7_655 ? Zn1 N1 2.066(3) 8_665 ? O1 C8 1.223(6) . ? O2 C8 1.263(5) . ? N1 C3 1.323(5) . ? N1 C2 1.339(5) . ? N1 Zn1 2.066(3) 7_556 ? C1 C2 1.369(6) . ? C1 C5 1.379(6) . ? C3 C4 1.382(6) . ? C4 C5 1.379(5) . ? C5 C6 1.478(5) . ? C6 C7 1.319(5) . ? C7 C8 1.493(6) . ? C9 C9 1.14(6) 4 ? C9 C10 1.38(2) . ? 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 132.28(18) 2_655 . ? O2 Zn1 N1 114.70(13) 2_655 7_655 ? O2 Zn1 N1 95.62(12) . 7_655 ? O2 Zn1 N1 95.62(12) 2_655 8_665 ? O2 Zn1 N1 114.70(13) . 8_665 ? N1 Zn1 N1 100.77(18) 7_655 8_665 ? C8 O2 Zn1 107.6(3) . . ? C3 N1 C2 116.9(4) . . ? C3 N1 Zn1 123.9(3) . 7_556 ? C2 N1 Zn1 119.1(3) . 7_556 ? C2 C1 C5 120.3(4) . . ? N1 C2 C1 123.2(4) . . ? N1 C3 C4 122.9(4) . . ? C5 C4 C3 120.4(4) . . ? C1 C5 C4 116.2(4) . . ? C1 C5 C6 124.2(4) . . ? C4 C5 C6 119.6(4) . . ? C7 C6 C5 126.2(4) . . ? C6 C7 C8 123.0(4) . . ? O1 C8 O2 121.6(5) . . ? O1 C8 C7 119.5(5) . . ? O2 C8 C7 118.7(4) . . ? C9 C9 C10 171(8) 4 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Zn1 O2 C8 48.4(3) 2_655 . . . ? N1 Zn1 O2 C8 179.4(3) 7_655 . . . ? N1 Zn1 O2 C8 -76.0(3) 8_665 . . . ? C3 N1 C2 C1 -4.6(8) . . . . ? Zn1 N1 C2 C1 170.1(4) 7_556 . . . ? C5 C1 C2 N1 1.2(9) . . . . ? C2 N1 C3 C4 4.0(7) . . . . ? Zn1 N1 C3 C4 -170.4(3) 7_556 . . . ? N1 C3 C4 C5 -0.2(8) . . . . ? C2 C1 C5 C4 2.7(8) . . . . ? C2 C1 C5 C6 -177.4(5) . . . . ? C3 C4 C5 C1 -3.2(8) . . . . ? C3 C4 C5 C6 176.9(4) . . . . ? C1 C5 C6 C7 -8.6(9) . . . . ? C4 C5 C6 C7 171.3(5) . . . . ? C5 C6 C7 C8 -179.9(4) . . . . ? Zn1 O2 C8 O1 7.2(7) . . . . ? Zn1 O2 C8 C7 -176.2(4) . . . . ? C6 C7 C8 O1 -178.7(6) . . . . ? C6 C7 C8 O2 4.6(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.516 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.084 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag # D H A symm D-H H...A D...A D-H...A flag example O7 H7 N10 . . 1_555 0.94(4) 1.74(3) 2.617(3) 154(3) yes #============================================================================ # END OF CIF