# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Susumu Kitagawa' 'Shuhei Furukawa' _publ_contact_author_name 'Susumu Kitagawa' _publ_contact_author_email KITAGAWA@SBCHEM.KYOTO-U.AC.JP _publ_section_title ; A block PCP crystal: anisotropic hybridization of porous coordination frameworks by face-selective epitaxial growth ; # Attachment 'framework2.cif' data___ZnJ_ndi2 _database_code_depnum_ccdc_archive 'CCDC 733385' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C48 H24 N4 O12 Zn2 ' _chemical_formula_moiety 'C48 H24 N4 O12 Zn2 ' _chemical_formula_weight 979.50 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/m m m' _symmetry_space_group_name_Hall '-P 4 2' _symmetry_Int_Tables_number 123 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X,+Z 3 -X,-Y,+Z 4 +Y,-X,+Z 5 -X,+Y,+Z 6 +Y,+X,+Z 7 +X,-Y,+Z 8 -Y,-X,+Z 9 -X,-Y,-Z 10 +Y,-X,-Z 11 +X,+Y,-Z 12 -Y,+X,-Z 13 +X,-Y,-Z 14 -Y,-X,-Z 15 -X,+Y,-Z 16 +Y,+X,-Z #------------------------------------------------------------------------------ _cell_length_a 10.906(2) _cell_length_b 10.906(2) _cell_length_c 22.456(4) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2670.8(9) _cell_formula_units_Z 1 _cell_measurement_reflns_used 7156 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 223.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 0.609 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496.00 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 0.909 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 21571 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_theta_max 27.53 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1839 _reflns_number_gt 1325 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_ref 0.0748 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1339 _refine_ls_number_parameters 99 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 96.2923 -31.5927 93.5597 ; _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.82 _refine_diff_density_min -0.98 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Zn Zn 0.284 1.430 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Zn(1) Zn 0.5000 0.5000 0.43384(2) 0.0417(2) Uani 1.00 8 d S . . O(1) O 0.5000 0.3167(2) 0.45060(16) 0.0901(9) Uani 1.00 2 d S . . O(2) O 0.303(2) 0.5000 0.1574(4) 0.399(13) Uani 0.50 2 d SP . . N(1) N 0.5000 0.5000 0.3440(2) 0.0482(8) Uani 1.00 8 d S . . N(2) N 0.5000 0.5000 0.1548(2) 0.094(2) Uani 1.00 8 d S . . C(1) C 0.5000 0.2664(4) 0.5000 0.0795(15) Uani 1.00 4 d S . . C(2) C 0.5000 0.1289(4) 0.5000 0.111(2) Uani 1.00 4 d S . . C(3) C 0.5833(13) 0.0652(5) 0.4636(3) 0.152(3) Uani 0.50 1 d P . . C(4) C 0.7041(13) 0.1339(10) 0.4311(5) 0.085(3) Uani 0.25 1 d P . . C(5) C 0.799(2) 0.063(2) 0.3994(9) 0.131(6) Uani 0.25 1 d P . . C(6) C 0.3986(7) 0.500000(10) 0.3122(3) 0.105(3) Uani 0.50 2 d SP . . C(7) C 0.3950(11) 0.500000(10) 0.2504(3) 0.111(4) Uani 0.50 2 d SP . . C(8) C 0.5000 0.5000 0.2207(3) 0.0766(14) Uani 1.00 8 d S . . C(9) C 0.3977(13) 0.5000 0.1294(3) 0.199(7) Uani 0.50 2 d SP . . C(10) C 0.397(2) 0.5000 0.0622(4) 0.180(10) Uani 0.50 2 d SP . . C(11) C 0.5000 0.5000 0.0319(3) 0.094(2) Uani 1.00 8 d S . . C(12) C 0.288(3) 0.500000(10) 0.0320(5) 0.58(3) Uani 0.50 2 d SP . . H(1) H 0.3231 0.5000 0.3333 0.127 Uiso 0.50 2 c R . . H(2) H 0.3184 0.5000 0.2303 0.133 Uiso 0.50 2 c R . . H(3) H 0.2121 0.5000 0.0530 0.702 Uiso 0.50 2 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn(1) 0.0489(3) 0.0489(3) 0.0274(4) 0.0000 0.0000 0.0000 O(1) 0.160(3) 0.0504(13) 0.0597(13) 0.0000 0.0000 0.0040(10) O(2) 0.202(16) 0.96(6) 0.033(3) 0.0000 0.026(6) 0.0000 N(1) 0.0620(14) 0.0620(14) 0.021(2) 0.0000 0.0000 0.0000 N(2) 0.134(4) 0.134(4) 0.015(3) 0.0000 0.0000 0.0000 C(1) 0.147(4) 0.045(2) 0.047(2) 0.0000 0.0000 0.0000 C(2) 0.249(9) 0.0418(19) 0.042(2) 0.0000 0.0000 0.0000 C(3) 0.334(15) 0.056(2) 0.067(4) -0.009(4) 0.025(5) 0.004(2) C(4) 0.097(7) 0.057(4) 0.102(9) 0.006(4) 0.026(5) 0.010(4) C(5) 0.116(12) 0.117(9) 0.161(18) 0.015(9) 0.050(12) -0.021(10) C(6) 0.065(4) 0.216(12) 0.036(2) 0.0000 0.020(3) 0.0000 C(7) 0.099(7) 0.194(12) 0.040(4) 0.0000 -0.023(4) 0.0000 C(8) 0.102(3) 0.102(3) 0.025(2) 0.0000 0.0000 0.0000 C(9) 0.112(9) 0.46(2) 0.028(3) 0.0000 0.008(4) 0.0000 C(10) 0.131(15) 0.37(4) 0.038(4) 0.0000 -0.006(5) 0.0000 C(11) 0.124(5) 0.124(5) 0.033(4) 0.0000 0.0000 0.0000 C(12) 0.151(16) 1.57(18) 0.032(5) 0.0000 0.009(6) 0.0000 #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2002 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Zn(1) Zn(1) 2.9713(6) yes . 9_666 Zn(1) O(1) 2.034(2) yes . . Zn(1) O(1) 2.0337(6) yes . 2_655 Zn(1) O(1) 2.034(2) yes . 3_665 Zn(1) O(1) 2.0337(6) yes . 4_565 Zn(1) N(1) 2.018(4) yes . . O(1) C(1) 1.238(3) yes . . O(2) C(9) 1.21(2) yes . . N(1) C(6) 1.316(8) yes . . N(1) C(6) 1.316(5) yes . 2_655 N(1) C(6) 1.316(8) yes . 3_665 N(1) C(6) 1.316(5) yes . 4_565 N(2) C(8) 1.478(10) yes . . N(2) C(9) 1.253(13) yes . . N(2) C(9) 1.253(4) yes . 2_655 N(2) C(9) 1.253(13) yes . 3_665 N(2) C(9) 1.253(4) yes . 4_565 C(1) C(2) 1.500(6) yes . . C(2) C(3) 1.406(11) yes . . C(2) C(3) 1.406(10) yes . 5_655 C(2) C(3) 1.406(11) yes . 11_556 C(2) C(3) 1.406(10) yes . 15_656 C(3) C(3) 1.82(2) yes . 5_655 C(3) C(3) 1.423(8) yes . 7_555 C(3) C(3) 1.636(9) yes . 11_556 C(3) C(4) 1.681(18) yes . . C(4) C(5) 1.48(2) yes . . C(5) C(5) 1.38(3) yes . 7_555 C(6) C(6) 1.564(8) yes . 2_655 C(6) C(6) 1.564(8) yes . 4_565 C(6) C(7) 1.389(12) yes . . C(7) C(7) 1.620(12) yes . 2_655 C(7) C(7) 1.620(12) yes . 4_565 C(7) C(8) 1.326(12) yes . . C(9) C(9) 1.577(14) yes . 2_655 C(9) C(9) 1.577(14) yes . 4_565 C(9) C(10) 1.509(12) yes . . C(10) C(10) 1.60(2) yes . 2_655 C(10) C(10) 1.60(2) yes . 4_565 C(10) C(11) 1.317(19) yes . . C(10) C(12) 1.37(3) yes . . C(11) C(11) 1.434(12) yes . 9_665 C(12) C(12) 1.436(16) yes . 11_555 C(6) H(1) 0.950(11) no . . C(7) H(2) 0.950 no . . C(12) H(3) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Zn(1) Zn(1) O(1) 79.34(10) yes 9_666 . . Zn(1) Zn(1) O(1) 79.34(10) yes 9_666 . 2_655 Zn(1) Zn(1) O(1) 79.34(10) yes 9_666 . 3_665 Zn(1) Zn(1) O(1) 79.34(10) yes 9_666 . 4_565 Zn(1) Zn(1) N(1) 180.0000 yes 9_666 . . O(1) Zn(1) O(1) 88.04(7) yes . . 2_655 O(1) Zn(1) O(1) 158.67(14) yes . . 3_665 O(1) Zn(1) O(1) 88.04(7) yes . . 4_565 O(1) Zn(1) N(1) 100.66(10) yes . . . O(1) Zn(1) O(1) 88.04(7) yes 2_655 . 3_665 O(1) Zn(1) O(1) 158.67(14) yes 2_655 . 4_565 O(1) Zn(1) N(1) 100.66(10) yes 2_655 . . O(1) Zn(1) O(1) 88.04(7) yes 3_665 . 4_565 O(1) Zn(1) N(1) 100.66(10) yes 3_665 . . O(1) Zn(1) N(1) 100.66(10) yes 4_565 . . Zn(1) O(1) C(1) 127.0(2) yes . . . Zn(1) N(1) C(6) 122.8(4) yes . . . Zn(1) N(1) C(6) 122.8(3) yes . . 2_655 Zn(1) N(1) C(6) 122.8(4) yes . . 3_665 Zn(1) N(1) C(6) 122.8(3) yes . . 4_565 C(6) N(1) C(6) 72.9(4) yes . . 2_655 C(6) N(1) C(6) 114.4(6) yes . . 3_665 C(6) N(1) C(6) 72.9(4) yes . . 4_565 C(6) N(1) C(6) 72.9(4) yes 2_655 . 3_665 C(6) N(1) C(6) 114.4(5) yes 2_655 . 4_565 C(6) N(1) C(6) 72.9(4) yes 3_665 . 4_565 C(8) N(2) C(9) 117.1(5) yes . . . C(8) N(2) C(9) 117.1(4) yes . . 2_655 C(8) N(2) C(9) 117.1(5) yes . . 3_665 C(8) N(2) C(9) 117.1(4) yes . . 4_565 C(9) N(2) C(9) 78.0(6) yes . . 2_655 C(9) N(2) C(9) 125.8(8) yes . . 3_665 C(9) N(2) C(9) 78.0(6) yes . . 4_565 C(9) N(2) C(9) 78.0(6) yes 2_655 . 3_665 C(9) N(2) C(9) 125.8(6) yes 2_655 . 4_565 C(9) N(2) C(9) 78.0(6) yes 3_665 . 4_565 O(1) C(1) O(1) 127.4(4) yes . . 11_556 O(1) C(1) C(2) 116.3(2) yes . . . O(1) C(1) C(2) 116.3(2) yes 11_556 . . C(1) C(2) C(3) 119.6(3) yes . . . C(1) C(2) C(3) 119.6(3) yes . . 5_655 C(1) C(2) C(3) 119.6(3) yes . . 11_556 C(1) C(2) C(3) 119.6(3) yes . . 15_656 C(3) C(2) C(3) 80.5(7) yes . . 5_655 C(3) C(2) C(3) 71.1(5) yes . . 11_556 C(3) C(2) C(3) 120.8(5) yes . . 15_656 C(3) C(2) C(3) 120.8(5) yes 5_655 . 11_556 C(3) C(2) C(3) 71.1(5) yes 5_655 . 15_656 C(3) C(2) C(3) 80.5(7) yes 11_556 . 15_656 C(2) C(3) C(3) 49.7(5) yes . . 5_655 C(2) C(3) C(3) 119.6(9) yes . . 7_555 C(2) C(3) C(3) 54.4(5) yes . . 11_556 C(2) C(3) C(4) 122.6(6) yes . . . C(3) C(3) C(3) 90.0(8) yes 5_655 . 7_555 C(3) C(3) C(3) 90.0(7) yes 5_655 . 11_556 C(3) C(3) C(4) 141.6(6) yes 5_655 . . C(3) C(3) C(3) 90.0(4) yes 7_555 . 11_556 C(3) C(3) C(4) 116.5(10) yes 7_555 . . C(3) C(3) C(4) 115.7(9) yes 11_556 . . C(3) C(4) C(5) 121.9(11) yes . . . C(4) C(5) C(5) 121.4(18) yes . . 7_555 N(1) C(6) C(6) 53.5(3) yes . . 2_655 N(1) C(6) C(6) 53.5(3) yes . . 4_565 N(1) C(6) C(7) 124.5(8) yes . . . C(6) C(6) C(6) 90.0(5) yes 2_655 . 4_565 C(6) C(6) C(7) 91.2(6) yes 2_655 . . C(6) C(6) C(7) 91.2(6) yes 4_565 . . C(6) C(7) C(7) 88.8(6) yes . . 2_655 C(6) C(7) C(7) 88.8(6) yes . . 4_565 C(6) C(7) C(8) 118.6(9) yes . . . C(7) C(7) C(7) 90.0(7) yes 2_655 . 4_565 C(7) C(7) C(8) 52.3(5) yes 2_655 . . C(7) C(7) C(8) 52.3(5) yes 4_565 . . N(2) C(8) C(7) 120.2(5) yes . . . N(2) C(8) C(7) 120.2(4) yes . . 2_655 N(2) C(8) C(7) 120.2(5) yes . . 3_665 N(2) C(8) C(7) 120.2(4) yes . . 4_565 C(7) C(8) C(7) 75.3(6) yes . . 2_655 C(7) C(8) C(7) 119.5(8) yes . . 3_665 C(7) C(8) C(7) 75.3(6) yes . . 4_565 C(7) C(8) C(7) 75.3(6) yes 2_655 . 3_665 C(7) C(8) C(7) 119.5(7) yes 2_655 . 4_565 C(7) C(8) C(7) 75.3(6) yes 3_665 . 4_565 O(2) C(9) N(2) 121.5(10) yes . . . O(2) C(9) C(9) 127.1(6) yes . . 2_655 O(2) C(9) C(9) 127.1(6) yes . . 4_565 O(2) C(9) C(10) 120.9(14) yes . . . N(2) C(9) C(9) 51.0(5) yes . . 2_655 N(2) C(9) C(9) 51.0(5) yes . . 4_565 N(2) C(9) C(10) 117.6(12) yes . . . C(9) C(9) C(9) 90.0(9) yes 2_655 . 4_565 C(9) C(9) C(10) 90.3(8) yes 2_655 . . C(9) C(9) C(10) 90.3(8) yes 4_565 . . C(9) C(10) C(10) 89.7(8) yes . . 2_655 C(9) C(10) C(10) 89.7(8) yes . . 4_565 C(9) C(10) C(11) 120.6(15) yes . . . C(9) C(10) C(12) 120.2(16) yes . . . C(10) C(10) C(10) 90.0(13) yes 2_655 . 4_565 C(10) C(10) C(11) 52.7(8) yes 2_655 . . C(10) C(10) C(12) 127.9(7) yes 2_655 . . C(10) C(10) C(11) 52.7(8) yes 4_565 . . C(10) C(10) C(12) 127.9(7) yes 4_565 . . C(11) C(10) C(12) 119.2(11) yes . . . C(10) C(11) C(10) 74.5(9) yes . . 2_655 C(10) C(11) C(10) 117.8(10) yes . . 3_665 C(10) C(11) C(10) 74.5(9) yes . . 4_565 C(10) C(11) C(11) 121.1(6) yes . . 9_665 C(10) C(11) C(10) 74.5(9) yes 2_655 . 3_665 C(10) C(11) C(10) 117.8(7) yes 2_655 . 4_565 C(10) C(11) C(11) 121.1(4) yes 2_655 . 9_665 C(10) C(11) C(10) 74.5(9) yes 3_665 . 4_565 C(10) C(11) C(11) 121.1(6) yes 3_665 . 9_665 C(10) C(11) C(11) 121.1(4) yes 4_565 . 9_665 C(10) C(12) C(12) 120(2) yes . . 11_555 N(1) C(6) H(1) 117.3(9) no . . . C(6) C(6) H(1) 127.8(5) no 2_655 . . C(6) C(6) H(1) 127.8(5) no 4_565 . . C(7) C(6) H(1) 118.3(10) no . . . C(6) C(7) H(2) 120.1 no . . . C(7) C(7) H(2) 128.4 no 2_655 . . C(7) C(7) H(2) 128.4 no 4_565 . . C(8) C(7) H(2) 121.3 no . . . C(10) C(12) H(3) 120.4 no . . . C(12) C(12) H(3) 119.8 no 11_555 . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Zn(1) O(1) 3.275(2) ? . 10_566 Zn(1) O(1) 3.275(2) ? . 12_656 O(1) O(1) 3.593(3) ? . 10_566 O(1) O(1) 3.593(3) ? . 12_656 C(1) O(1) 3.423(4) ? . 10_566 C(1) O(1) 3.423(4) ? . 12_656 C(2) C(2) 2.811(6) ? . 3_655 C(2) C(3) 2.445(9) ? . 3_655 C(2) C(3) 2.445(9) ? . 9_656 C(2) C(3) 2.445(9) ? . 13_556 C(3) C(2) 2.445(9) ? . 3_655 C(3) C(3) 2.308(17) ? . 3_655 C(3) C(3) 2.829(15) ? . 9_656 C(3) C(3) 2.168(9) ? . 13_556 C(3) C(4) 3.470(14) ? . 13_556 C(4) C(3) 3.470(14) ? . 13_556 C(4) C(4) 2.499(18) ? . 8_665 C(4) C(5) 2.73(2) ? . 8_665 C(5) C(4) 2.73(2) ? . 8_665 C(5) C(5) 3.25(3) ? . 2_645 C(5) C(5) 3.25(3) ? . 4_665 C(5) C(5) 2.12(3) ? . 8_665 C(10) C(10) 3.218(15) ? . 10_565 C(10) C(10) 3.218(15) ? . 12_655 C(10) C(12) 3.333(16) ? . 10_565 C(10) C(12) 3.333(16) ? . 12_655 C(11) C(10) 2.396(10) ? . 10_565 C(11) C(10) 2.396(10) ? . 12_655 C(11) C(12) 2.725(7) ? . 10_565 C(11) C(12) 2.725(7) ? . 12_655 C(12) C(10) 3.33(2) ? . 10_565 C(12) C(10) 3.33(2) ? . 12_655 C(12) C(12) 3.58(3) ? . 10_565 C(12) C(12) 3.58(3) ? . 12_655 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #==============================================================================