# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Shuhei Furukawa' _publ_contact_author_email SHUHEI.FURUKAWA@KIP.JST.GO.JP _publ_section_title ; Control over the nucleation process determines the framework topology of porous coordination polymers ; loop_ _publ_author_name 'Shuhei Furukawa' 'Susumu Kitagawa' 'Mio Kondo' 'Joobeom Seo' 'Yohei Takashima' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-06-21 at 11:22:26 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : referee #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_referee _database_code_depnum_ccdc_archive 'CCDC 769113' #TrackingRef '2kgm_r.cif' _audit_creation_date 2010-06-21T11:22:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C26 H20 N2 O10 Zn2' _chemical_formula_weight 651.18 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 6/mmm' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' '-y, -x, -z' 'x-y, -y, -z' 'x, x-y, -z' 'y, x, -z' '-x+y, y, -z' '-x, -x+y, -z' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' 'y, x, z' '-x+y, y, z' '-x, -x+y, z' '-y, -x, z' 'x-y, -y, z' 'x, x-y, z' _cell_length_a 21.619(8) _cell_length_b 21.619(8) _cell_length_c 14.104(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 5709(4) _cell_formula_units_Z 3 _cell_measurement_temperature 223(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 0.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 990 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8477 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_unetI/netI 0.0198 _diffrn_reflns_number 45244 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 2544 _reflns_number_gt 2326 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. Diffuse electron densities resulting from residual solvent molecules were removed from the data set using the SQUEEZE routine of PLATON and refined further using the data generated. The contents of the solvent region calculated from the result of SQUEEZE routine are represented in the unit cell contents in crystal data. The carbon atoms C4 and C5 of the bpy molecule are disordered over two sites and were refined isotropically. Atoms N1,C4,C5,C6 were restrained to be planar by means of a FLAT command. ; _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^)+(0.1639P)^2^+1.6125P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2544 _refine_ls_number_parameters 51 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.2555 _refine_ls_wR_factor_gt 0.2446 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.988 _refine_diff_density_min -0.911 _refine_diff_density_rms 0.085 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.5 0.10489(4) 0.0458(3) Uani 1 4 d S . . O1 O 0.07652(13) 0.47395(16) 0.07921(18) 0.0734(7) Uani 1 1 d . . . N1 N 0 0.5 0.2488(4) 0.0558(14) Uani 1 4 d SD . . C1 C 0.1012(2) 0.4708(2) 0 0.0579(10) Uani 1 2 d S . . C2 C 0.1684(2) 0.4643(3) 0 0.0586(10) Uani 1 2 d S . . C3 C 0.1995(2) 0.4619(3) 0.0839(2) 0.0759(11) Uani 1 1 d . . . H3 H 0.1771 0.4603 0.1418 0.091 Uiso 1 1 calc R . . C4 C -0.0520(5) 0.4496(5) 0.2973(8) 0.099(3) Uiso 0.5 1 d PD . . H4 H -0.09 0.4127 0.2635 0.119 Uiso 0.5 1 calc PR . . C5 C -0.0553(7) 0.4466(7) 0.3996(7) 0.111(4) Uiso 0.5 1 d PD . . H5 H -0.0942 0.4092 0.4313 0.133 Uiso 0.5 1 calc PR . . C6 C 0 0.5 0.4486(5) 0.066(2) Uani 1 4 d SD . . 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 0.0338(4) 0.0670(5) 0.0255(4) 0 0 0.01688(19) O1 0.0523(12) 0.118(2) 0.0583(13) -0.0030(14) 0.0016(11) 0.0490(14) N1 0.042(2) 0.082(3) 0.030(2) 0 0 0.0210(11) C1 0.052(2) 0.073(3) 0.049(2) 0 0 0.031(2) C2 0.051(2) 0.076(3) 0.047(2) 0 0 0.030(2) C3 0.068(2) 0.132(3) 0.0436(14) 0.0018(18) 0.0011(14) 0.062(2) C6 0.052(3) 0.101(4) 0.027(3) 0 0 0.0259(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 2.029(2) 4_565 ? Zn1 O1 2.029(2) 24_565 ? Zn1 O1 2.029(2) 21 ? Zn1 O1 2.029(2) . ? Zn1 N1 2.030(6) . ? Zn1 Zn1 2.9588(15) 13_565 ? O1 C1 1.254(3) . ? N1 C4 1.301(10) 4_565 ? N1 C4 1.301(10) . ? N1 C4 1.301(10) 24_565 ? N1 C4 1.301(10) 21 ? C1 O1 1.254(3) 16 ? C1 C2 1.527(6) . ? C2 C3 1.375(4) . ? C2 C3 1.375(4) 16 ? C3 C3 1.361(7) 20 ? C3 H3 0.94 . ? C4 C5 1.444(13) . ? C4 C4 1.947(19) 21 ? C4 H4 0.94 . ? C5 C6 1.363(13) . ? C5 H5 0.94 . ? C6 C5 1.363(13) 4_565 ? C6 C5 1.363(13) 24_565 ? C6 C5 1.363(13) 21 ? C6 C6 1.451(13) 13_566 ? 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 O1 Zn1 O1 89.83(17) 4_565 24_565 ? O1 Zn1 O1 86.51(17) 4_565 21 ? O1 Zn1 O1 159.43(15) 24_565 21 ? O1 Zn1 O1 159.43(15) 4_565 . ? O1 Zn1 O1 86.51(17) 24_565 . ? O1 Zn1 O1 89.83(17) 21 . ? O1 Zn1 N1 100.28(7) 4_565 . ? O1 Zn1 N1 100.28(7) 24_565 . ? O1 Zn1 N1 100.28(7) 21 . ? O1 Zn1 N1 100.28(7) . . ? O1 Zn1 Zn1 79.72(7) 4_565 13_565 ? O1 Zn1 Zn1 79.72(7) 24_565 13_565 ? O1 Zn1 Zn1 79.72(7) 21 13_565 ? O1 Zn1 Zn1 79.72(7) . 13_565 ? N1 Zn1 Zn1 180.0000(10) . 13_565 ? C1 O1 Zn1 127.0(2) . . ? C4 N1 C4 116.6(11) 4_565 . ? C4 N1 C4 96.9(9) 4_565 24_565 ? C4 N1 C4 47.8(7) . 24_565 ? C4 N1 C4 47.8(7) 4_565 21 ? C4 N1 C4 96.9(9) . 21 ? C4 N1 C4 116.6(11) 24_565 21 ? C4 N1 Zn1 121.7(5) 4_565 . ? C4 N1 Zn1 121.7(5) . . ? C4 N1 Zn1 121.7(5) 24_565 . ? C4 N1 Zn1 121.7(5) 21 . ? O1 C1 O1 125.9(4) 16 . ? O1 C1 C2 117.0(2) 16 . ? O1 C1 C2 117.0(2) . . ? C3 C2 C3 118.8(4) . 16 ? C3 C2 C1 120.6(2) . . ? C3 C2 C1 120.6(2) 16 . ? C3 C3 C2 120.5(2) 20 . ? C3 C3 H3 119.7 20 . ? C2 C3 H3 119.7 . . ? N1 C4 C5 124.4(10) . . ? N1 C4 C4 41.6(4) . 21 ? C5 C4 C4 92.4(6) . 21 ? N1 C4 H4 117.8 . . ? C5 C4 H4 117.8 . . ? C4 C4 H4 139.1 21 . ? C6 C5 C4 117.8(10) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? C5 C6 C5 119.0(10) . 4_565 ? C5 C6 C5 48.2(8) . 24_565 ? C5 C6 C5 98.8(9) 4_565 24_565 ? C5 C6 C5 98.8(9) . 21 ? C5 C6 C5 48.2(8) 4_565 21 ? C5 C6 C5 119.0(10) 24_565 21 ? C5 C6 C6 120.5(5) . 13_566 ? C5 C6 C6 120.5(5) 4_565 13_566 ? C5 C6 C6 120.5(5) 24_565 13_566 ? C5 C6 C6 120.5(5) 21 13_566 ? 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 O1 Zn1 O1 C1 4.7(3) 4_565 . . . ? O1 Zn1 O1 C1 -75.5(4) 24_565 . . . ? O1 Zn1 O1 C1 84.2(4) 21 . . . ? N1 Zn1 O1 C1 -175.3(3) . . . . ? Zn1 Zn1 O1 C1 4.7(3) 13_565 . . . ? O1 Zn1 N1 C4 -107.4(4) 4_565 . . 4_565 ? O1 Zn1 N1 C4 -15.7(4) 24_565 . . 4_565 ? O1 Zn1 N1 C4 164.3(4) 21 . . 4_565 ? O1 Zn1 N1 C4 72.6(4) . . . 4_565 ? Zn1 Zn1 N1 C4 14E1(10) 13_565 . . 4_565 ? O1 Zn1 N1 C4 72.6(4) 4_565 . . . ? O1 Zn1 N1 C4 164.3(4) 24_565 . . . ? O1 Zn1 N1 C4 -15.7(4) 21 . . . ? O1 Zn1 N1 C4 -107.4(4) . . . . ? Zn1 Zn1 N1 C4 -4E1(10) 13_565 . . . ? O1 Zn1 N1 C4 15.7(4) 4_565 . . 24_565 ? O1 Zn1 N1 C4 107.4(4) 24_565 . . 24_565 ? O1 Zn1 N1 C4 -72.6(4) 21 . . 24_565 ? O1 Zn1 N1 C4 -164.3(4) . . . 24_565 ? Zn1 Zn1 N1 C4 -10E1(10) 13_565 . . 24_565 ? O1 Zn1 N1 C4 -164.3(4) 4_565 . . 21 ? O1 Zn1 N1 C4 -72.6(4) 24_565 . . 21 ? O1 Zn1 N1 C4 107.4(4) 21 . . 21 ? O1 Zn1 N1 C4 15.7(4) . . . 21 ? Zn1 Zn1 N1 C4 8E1(10) 13_565 . . 21 ? Zn1 O1 C1 O1 -10.1(7) . . . 16 ? Zn1 O1 C1 C2 168.3(3) . . . . ? O1 C1 C2 C3 178.8(4) 16 . . . ? O1 C1 C2 C3 0.2(7) . . . . ? O1 C1 C2 C3 -0.2(7) 16 . . 16 ? O1 C1 C2 C3 -178.8(4) . . . 16 ? C3 C2 C3 C3 4.3(7) 16 . . 20 ? C1 C2 C3 C3 -174.7(3) . . . 20 ? C4 N1 C4 C5 0.2(6) 4_565 . . . ? C4 N1 C4 C5 -73.9(8) 24_565 . . . ? C4 N1 C4 C5 46.1(10) 21 . . . ? Zn1 N1 C4 C5 -179.8(6) . . . . ? C4 N1 C4 C4 -45.9(6) 4_565 . . 21 ? C4 N1 C4 C4 -120.0(7) 24_565 . . 21 ? Zn1 N1 C4 C4 134.1(6) . . . 21 ? N1 C4 C5 C6 -0.4(11) . . . . ? C4 C4 C5 C6 28.2(7) 21 . . . ? C4 C5 C6 C5 0.2(5) . . . 4_565 ? C4 C5 C6 C5 74.9(8) . . . 24_565 ? C4 C5 C6 C5 -46.5(11) . . . 21 ? C4 C5 C6 C6 -179.8(5) . . . 13_566 ? # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.008 -0.006 -0.022 4160.6 234.4 _platon_squeeze_details ; ; # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _chemical_name_common Kagome_bpy