# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm #TrackingRef '- ZBHAN11120613_r.cif' _journal_coden_cambridge 1350 #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; 'Han, Zheng-Bo' College of Chemistry liaoning University Shenyang, 110036 P. R. China ; _publ_contact_author_phone 86-24-62207849 _publ_contact_author_fax 86-24-62202380 _publ_contact_author_email ceshzb@lnu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to CrystEngComm. Sep.1, 2011 ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; loop_ _publ_author_name _publ_author_address 'Zheng-Bo Han' ; College of Chemistry Liaoning University Shenyang 110036 People's Republic of China ; 'Yan-Fang Liang' ; College of Chemistry Liaoning University Shenyang 110036 People's Republic of China ; 'Ming Zhou' ; College of Chemistry Liaoning University Shenyang 110036 People's Republic of China ; 'Ya-Ru Zhang' ; College of Chemistry Liaoning University Shenyang 110036 People's Republic of China ; 'Li, Li' ; College of Chemistry Liaoning University Shenyang 110036 People's Republic of China ; ; Jian Tong ; ; College of Chemistry Liaoning University Shenyang 110036 People's Republic of China ; _publ_contact_author_name 'Han, Zheng-Bo' #====================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 842641' #TrackingRef '- ZBHAN11120613_r.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H123 Zn N13 O20' _chemical_formula_weight 1688.33 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 hexagonal _symmetry_space_group_name_H-M P6522 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+5/6' '-y, x-y, z+2/3' '-x, -y, z+1/2' '-x+y, -x, z+1/3' 'y, -x+y, z+1/6' 'x-y, -y, -z' '-x, -x+y, -z+1/3' 'y, x, -z+2/3' '-y, -x, -z+1/6' '-x+y, y, -z+1/2' 'x, x-y, -z+5/6' _cell_length_a 23.9581(9) _cell_length_b 23.9581(9) _cell_length_c 29.2285(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14529.2(10) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5619 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 20.38 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.274 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9059 _exptl_absorpt_correction_T_max 0.9302 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX area-detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 57960 _diffrn_reflns_av_R_equivalents 0.0987 _diffrn_reflns_av_sigmaI/netI 0.2010 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 23.28 _reflns_number_total 6965 _reflns_number_gt 1797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00011(4) _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 0.24(3) _refine_ls_number_reflns 6965 _refine_ls_number_parameters 195 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1937 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1836 _refine_ls_wR_factor_gt 0.1767 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.027 _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 0.44131(8) 0.56441(8) 0.13889(3) 0.1089(6) Uani 0.50 1 d P . . O1 O 0.4782(2) 0.5138(2) 0.12407(16) 0.1822(19) Uani 1 1 d . . . O2 O 0.4694(2) -0.3568(3) 0.11533(19) 0.1923(19) Uiso 1 1 d . . . O3 O 0.4852(2) -0.3472(2) 0.03718(14) 0.1628(18) Uani 1 1 d . . . O1W O 0.4553(3) 0.5688(2) 0.20387(10) 0.210(2) Uani 1 1 d . . . C1 C 0.4983(4) 0.5017(4) 0.0833 0.169(4) Uiso 1 2 d S . . C2 C 0.5310(3) 0.4690(3) 0.0833 0.146(4) Uiso 1 2 d SD . . C3 C 0.5465(3) 0.4489(4) 0.1289(2) 0.164(3) Uani 1 1 d D . . C4 C 0.5804(3) 0.4145(3) 0.12905(19) 0.120(2) Uani 1 1 d D . . C5 C 0.5959(3) 0.4041(3) 0.0833 0.154(4) Uiso 1 2 d SD . . C6 C 0.6318(5) 0.3682(5) 0.0833 0.201(7) Uiso 1 2 d SD . . C7 C 0.6167(4) 0.3144(5) 0.1115(3) 0.154(3) Uani 1 1 d D . . C8 C 0.6543(4) 0.2820(4) 0.1134(2) 0.147(3) Uani 1 1 d D . . C9 C 0.7041(3) 0.2959(3) 0.0833 0.140(4) Uani 1 2 d SD . . C10 C 0.7433(5) 0.2567(5) 0.0833 0.278(8) Uiso 1 2 d S . . C11 C 0.7063(4) 0.1885(4) 0.0856(2) 0.178(3) Uiso 1 1 d . . . C12 C 0.7438(3) 0.1567(4) 0.08706(18) 0.120(2) Uiso 1 1 d . . . C13 C 0.8121(2) 0.1879(2) 0.0833 0.146(3) Uiso 1 2 d S . . C14 C 0.6959(5) 0.0867(3) 0.0891(3) 0.131(2) Uani 1 1 d D . . C15 C 0.6414(5) 0.0572(5) 0.1192(3) 0.197(5) Uani 1 1 d D . . C16 C 0.6148(5) -0.0072(7) 0.1163(3) 0.186(5) Uani 1 1 d D . . C17 C 0.6361(5) -0.0358(4) 0.0827(4) 0.189(4) Uani 1 1 d D . . C18 C 0.6939(4) -0.0121(5) 0.05865(19) 0.143(3) Uani 1 1 d D . . C19 C 0.7290(4) 0.0582(5) 0.0643(3) 0.167(4) Uiso 1 1 d D . . C20 C 0.6020(5) -0.1033(8) 0.0815(4) 0.229(5) Uiso 1 1 d D . . C21 C 0.5746(3) -0.1439(5) 0.1216(3) 0.194(3) Uani 1 1 d D . . C22 C 0.5400(3) -0.2115(5) 0.1241(2) 0.131(2) Uiso 1 1 d D . . C23 C 0.5330(3) -0.2405(4) 0.0799(5) 0.234(6) Uani 1 1 d D . . C24 C 0.5582(5) -0.2064(8) 0.0359(5) 0.351(10) Uiso 1 1 d D . . C25 C 0.5910(3) -0.1386(4) 0.0400(3) 0.177(3) Uani 1 1 d D . . C26 C 0.4945(5) -0.3103(6) 0.0752(4) 0.208(4) 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 0.1359(16) 0.1461(15) 0.0559(7) 0.0060(9) -0.0005(9) 0.0789(13) O1 0.206(5) 0.265(6) 0.128(4) 0.030(3) 0.048(3) 0.157(4) O3 0.199(5) 0.195(5) 0.109(4) -0.049(3) -0.030(3) 0.109(4) O1W 0.372(6) 0.335(6) 0.072(3) -0.019(3) 0.025(3) 0.289(6) C3 0.081(6) 0.194(9) 0.177(7) 0.098(6) 0.021(4) 0.040(5) C4 0.149(7) 0.133(6) 0.102(6) 0.007(4) 0.027(5) 0.088(5) C7 0.158(7) 0.192(9) 0.121(6) -0.031(7) 0.020(5) 0.095(7) C8 0.180(9) 0.164(7) 0.074(5) -0.017(5) 0.052(5) 0.068(6) C9 0.174(7) 0.174(7) 0.035(6) 0.006(6) 0.006(6) 0.058(9) C14 0.188(8) 0.107(7) 0.133(6) -0.031(5) -0.064(6) 0.101(7) C15 0.219(11) 0.153(9) 0.148(8) 0.003(7) 0.079(7) 0.040(9) C16 0.242(11) 0.343(16) 0.085(5) -0.056(9) -0.007(6) 0.231(13) C17 0.194(10) 0.035(5) 0.269(12) -0.005(6) 0.014(9) 0.005(6) C18 0.099(6) 0.199(11) 0.096(5) 0.063(5) 0.024(5) 0.049(7) C21 0.203(8) 0.109(7) 0.217(9) -0.083(6) -0.036(7) 0.037(6) C23 0.151(7) 0.067(7) 0.46(2) -0.117(9) -0.086(9) 0.034(6) C25 0.167(7) 0.124(7) 0.240(9) -0.005(6) -0.057(6) 0.073(6) _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 1.794(6) 1_565 ? Zn1 O1 1.873(4) . ? Zn1 O1W 1.922(3) . ? Zn1 O3 1.972(5) 10_565 ? O1 C1 1.369(7) . ? O2 C26 1.521(9) . ? O2 Zn1 1.794(6) 1_545 ? O3 C26 1.367(10) . ? O3 Zn1 1.972(5) 10_655 ? C1 C2 1.357(12) . ? C1 O1 1.369(7) 10_665 ? C2 C3 1.525(6) 10_665 ? C2 C3 1.525(6) . ? C3 C4 1.418(7) . ? C4 C5 1.441(6) . ? C5 C6 1.490(14) . ? C5 C4 1.441(6) 10_665 ? C6 C7 1.414(9) 10_665 ? C6 C7 1.414(9) . ? C7 C8 1.455(8) . ? C8 C9 1.384(7) . ? C9 C8 1.384(7) 10_665 ? C9 C10 1.623(16) . ? C10 C11 1.419(10) . ? C10 C11 1.419(10) 10_665 ? C11 C12 1.440(7) . ? C12 C13 1.424(6) . ? C12 C14 1.486(7) . ? C13 C12 1.424(6) 10_665 ? C14 C15 1.434(10) . ? C14 C19 1.471(8) . ? C15 C16 1.346(10) . ? C16 C17 1.430(9) . ? C17 C18 1.396(8) . ? C17 C20 1.402(13) . ? C18 C19 1.467(8) . ? C20 C25 1.426(10) . ? C20 C21 1.452(10) . ? C21 C22 1.403(7) . ? C22 C23 1.438(9) . ? C23 C26 1.456(10) . ? C23 C24 1.480(12) . ? C24 C25 1.412(12) . ? 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 O1 122.8(2) 1_565 . ? O2 Zn1 O1W 111.0(2) 1_565 . ? O1 Zn1 O1W 97.96(19) . . ? O2 Zn1 O3 107.2(2) 1_565 10_565 ? O1 Zn1 O3 110.13(19) . 10_565 ? O1W Zn1 O3 106.6(2) . 10_565 ? C1 O1 Zn1 131.9(8) . . ? C26 O2 Zn1 150.5(6) . 1_545 ? C26 O3 Zn1 131.6(6) . 10_655 ? C2 C1 O1 119.2(7) . 10_665 ? C2 C1 O1 119.2(7) . . ? O1 C1 O1 121.5(13) 10_665 . ? C1 C2 C3 119.0(5) . 10_665 ? C1 C2 C3 119.0(5) . . ? C3 C2 C3 122.1(11) 10_665 . ? C4 C3 C2 119.1(8) . . ? C3 C4 C5 111.7(8) . . ? C6 C5 C4 111.9(5) . 10_665 ? C6 C5 C4 111.9(5) . . ? C4 C5 C4 136.2(11) 10_665 . ? C5 C6 C7 124.5(7) . 10_665 ? C5 C6 C7 124.5(7) . . ? C7 C6 C7 111.0(14) 10_665 . ? C8 C7 C6 124.3(11) . . ? C9 C8 C7 122.6(9) . . ? C8 C9 C8 114.6(11) 10_665 . ? C8 C9 C10 122.7(6) 10_665 . ? C8 C9 C10 122.7(6) . . ? C11 C10 C11 125.6(18) . 10_665 ? C11 C10 C9 117.2(9) . . ? C11 C10 C9 117.2(9) 10_665 . ? C10 C11 C12 114.6(11) . . ? C13 C12 C11 125.4(8) . . ? C13 C12 C14 129.2(7) . . ? C11 C12 C14 105.3(7) . . ? C12 C13 C12 114.4(10) 10_665 . ? C15 C14 C19 130.0(8) . . ? C15 C14 C12 125.4(8) . . ? C19 C14 C12 102.3(9) . . ? C16 C15 C14 108.6(10) . . ? C15 C16 C17 120.9(11) . . ? C18 C17 C20 110.1(10) . . ? C18 C17 C16 132.1(8) . . ? C20 C17 C16 115.4(12) . . ? C17 C18 C19 107.0(7) . . ? C14 C19 C18 117.1(7) . . ? C17 C20 C25 122.2(13) . . ? C17 C20 C21 124.2(12) . . ? C25 C20 C21 113.6(13) . . ? C22 C21 C20 128.6(10) . . ? C21 C22 C23 111.7(7) . . ? C22 C23 C26 119.6(13) . . ? C22 C23 C24 126.6(10) . . ? C26 C23 C24 113.6(12) . . ? C25 C24 C23 113.6(11) . . ? C24 C25 C20 125.9(12) . . ? O3 C26 C23 128.7(10) . . ? O3 C26 O2 106.0(9) . . ? C23 C26 O2 124.0(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.166 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.035 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.000 0.000 -0.004 10178 3699 ' ' _platon_squeeze_details ; ; #====================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 842642' #TrackingRef '- ZBHAN11120613_r.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85 H110 Zn2 N12 O20' _chemical_formula_weight 1750.64 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 hexagonal _symmetry_space_group_name_H-M P6(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/6' '-y, x-y, z+1/3' '-x, -y, z+1/2' '-x+y, -x, z+2/3' 'y, -x+y, z+5/6' _cell_length_a 23.965(3) _cell_length_b 23.965(3) _cell_length_c 26.192(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13027(4) _cell_formula_units_Z 6 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3719 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 12.96 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2790 _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8139 _exptl_absorpt_correction_T_max 0.8853 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX area-detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18297 _diffrn_reflns_av_R_equivalents 0.0977 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 13.07 _reflns_number_total 2318 _reflns_number_gt 1902 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.1492P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _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 0.14(9) _refine_ls_number_reflns 2318 _refine_ls_number_parameters 131 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2012 _refine_ls_wR_factor_gt 0.1947 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.699 _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 0.4516(2) 0.5453(2) 0.43281(16) 0.079(3) Uani 1 1 d . . . Zn2 Zn 0.45462(19) 0.5487(2) 0.55699(16) 0.069(3) Uani 1 1 d . . . C1 C 0.7520(15) 0.2472(15) 0.4970(12) 0.106(14) Uiso 1 1 d G . . C2 C 0.8189(15) 0.2805(8) 0.5003(11) 0.071(13) Uiso 1 1 d G . . C3 C 0.8522(8) 0.2469(15) 0.4998(10) 0.087(14) Uiso 1 1 d G . . C4 C 0.8188(15) 0.1801(15) 0.4961(11) 0.052(10) Uiso 1 1 d G . . C5 C 0.7519(15) 0.1468(8) 0.4929(10) 0.044(11) Uiso 1 1 d G . . C6 C 0.7185(8) 0.1804(15) 0.4933(11) 0.075(13) Uiso 1 1 d G . . C7 C 0.7182(16) 0.2845(16) 0.4977(15) 0.092(13) Uiso 1 1 d G . . C8 C 0.6638(18) 0.2633(10) 0.4672(11) 0.132(18) Uiso 1 1 d G . . C9 C 0.6286(10) 0.2950(17) 0.4686(11) 0.108(16) Uiso 1 1 d G . . C10 C 0.6476(16) 0.3479(16) 0.5004(14) 0.081(13) Uiso 1 1 d G . . C11 C 0.7020(18) 0.3691(10) 0.5310(10) 0.107(16) Uiso 1 1 d G . . C12 C 0.7372(10) 0.3374(18) 0.5296(11) 0.103(15) Uiso 1 1 d G . . C13 C 0.6166(8) 0.3881(8) 0.4928(12) 0.043(10) Uiso 1 1 d G . . C14 C 0.5886(9) 0.3937(8) 0.4480(9) 0.065(13) Uiso 1 1 d G . . C15 C 0.5538(7) 0.4259(7) 0.4485(7) 0.088(14) Uiso 1 1 d GD . . C16 C 0.5470(6) 0.4524(5) 0.4936(9) 0.096(12) Uiso 1 1 d GD . . C17 C 0.5750(8) 0.4468(7) 0.5383(7) 0.16(2) Uiso 1 1 d GD . . C18 C 0.6098(8) 0.4146(9) 0.5379(9) 0.129(17) Uiso 1 1 d G . . C19 C 0.5181(7) 0.5070(6) 0.4905(15) 0.105(14) Uiso 1 1 d GD . . C20 C 0.9266(8) 0.2836(14) 0.5049(11) 0.056(12) Uiso 1 1 d G . . C21 C 0.9600(16) 0.2599(9) 0.4777(9) 0.095(15) Uiso 1 1 d G . . C22 C 1.0270(16) 0.2928(16) 0.4783(10) 0.074(13) Uiso 1 1 d G . . C23 C 1.0605(8) 0.3494(15) 0.5062(12) 0.095(14) Uiso 1 1 d G . . C24 C 1.0270(17) 0.3732(10) 0.5335(10) 0.102(16) Uiso 1 1 d G . . C25 C 0.9601(17) 0.3402(16) 0.5329(9) 0.087(14) Uiso 1 1 d G . . C26 C 1.1335(8) 0.3924(9) 0.5082(10) 0.067(13) Uiso 1 1 d G . . C27 C 1.1604(11) 0.3904(10) 0.4617(9) 0.077(14) Uiso 1 1 d G . . C28 C 1.2270(12) 0.4229(11) 0.4558(6) 0.092(15) Uiso 1 1 d G . . C29 C 1.2666(8) 0.4574(8) 0.4964(7) 0.070(13) Uiso 1 1 d G . . C30 C 1.2398(10) 0.4594(9) 0.5429(6) 0.055(12) Uiso 1 1 d G . . C31 C 1.1732(10) 0.4269(11) 0.5488(8) 0.080(14) Uiso 1 1 d G . . C32 C 1.3341(8) 0.4973(11) 0.5014(12) 0.069(12) Uiso 1 1 d G . . C33 C 0.7188(13) 0.0744(7) 0.4861(10) 0.050(11) Uiso 1 1 d G . . C34 C 0.6603(15) 0.0419(15) 0.4604(9) 0.067(13) Uiso 1 1 d G . . C35 C 0.6258(9) -0.0250(15) 0.4601(9) 0.071(13) Uiso 1 1 d G . . C36 C 0.6498(14) -0.0595(7) 0.4856(11) 0.084(14) Uiso 1 1 d G . . C37 C 0.7082(15) -0.0271(15) 0.5113(9) 0.086(14) Uiso 1 1 d G . . C38 C 0.7428(9) 0.0399(16) 0.5116(9) 0.078(14) Uiso 1 1 d G . . C39 C 0.6122(7) -0.1342(7) 0.4819(7) 0.054(12) Uiso 1 1 d G . . C40 C 0.5773(7) -0.1700(8) 0.4399(6) 0.049(12) Uiso 1 1 d G . . C41 C 0.5395(8) -0.2366(8) 0.4435(6) 0.066(13) Uiso 1 1 d G . . C42 C 0.5365(7) -0.2674(7) 0.4893(6) 0.049(12) Uiso 1 1 d G . . C43 C 0.5713(9) -0.2316(8) 0.5313(6) 0.123(17) Uiso 1 1 d G . . C44 C 0.6092(10) -0.1650(8) 0.5277(7) 0.109(16) Uiso 1 1 d G . . C45 C 0.5113(8) -0.3367(7) 0.4931(8) 0.049(11) Uiso 1 1 d G . . C46 C 0.563(3) 0.5053(19) 0.146(2) 0.22(3) Uiso 1 1 d G . . C47 C 0.5321(4) 0.4997(4) 0.1988(5) 0.142(18) Uiso 1 1 d G . . C48 C 0.4781(4) 0.4619(4) 0.2286(5) 0.18(2) Uiso 1 1 d G . . C49 C 0.4725(4) 0.4830(4) 0.2767(5) 0.21(2) Uiso 1 1 d G . . C50 C 0.5209(4) 0.5419(4) 0.2951(5) 0.137(18) Uiso 1 1 d G . . C51 C 0.5749(4) 0.5797(4) 0.2653(5) 0.25(3) Uiso 1 1 d G . . C52 C 0.5805(4) 0.5586(4) 0.2171(5) 0.19(2) Uiso 1 1 d G . . C53 C 0.5070(4) 0.5648(4) 0.3508(5) 0.19(2) Uiso 1 1 d G . . N1 N 0.6310(4) 0.6512(4) 0.2991(5) 0.27(2) Uiso 1 1 d G . . O1 O 0.4844(4) 0.4925(4) 0.4555(5) 0.121(11) Uiso 1 1 d GD . . O2 O 0.5062(4) 0.5083(4) 0.5335(5) 0.107(10) Uiso 1 1 d GD . . O3 O 1.3670(4) 0.5202(6) 0.5395(7) 0.097(9) Uiso 1 1 d G . . O4 O 1.3584(4) 0.4930(6) 0.4590(7) 0.079(9) Uiso 1 1 d G . . O5 O 0.5015(6) -0.3635(4) 0.5346(6) 0.058(7) Uiso 1 1 d G . . O6 O 0.4738(6) -0.3679(4) 0.4539(6) 0.132(11) Uiso 1 1 d G . . O7 O 0.5388(5) 0.4517(5) 0.1349(5) 0.069(10) Uiso 1 1 d G . . O8 O 0.6055(5) 0.5462(5) 0.1213(5) 0.194(15) Uiso 1 1 d G . . O9 O 0.5507(4) 0.6012(4) 0.3789(5) 0.185(14) Uiso 1 1 d G . . O10 O 0.4524(4) 0.5377(4) 0.3672(5) 0.116(12) Uiso 1 1 d G . . 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 0.075(5) 0.075(5) 0.091(6) -0.017(3) -0.011(3) 0.040(3) Zn2 0.051(4) 0.056(4) 0.096(6) 0.007(3) 0.001(3) 0.024(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 O10 1.730(15) . ? Zn1 O1 1.890(9) . ? Zn1 O6 1.950(10) 1_565 ? Zn1 O4 2.056(10) 1_455 ? Zn1 C53 2.445(13) . ? Zn2 O3 1.911(11) 1_455 ? Zn2 O5 1.915(11) 1_565 ? Zn2 O2 2.009(8) . ? Zn2 O7 2.048(15) 4_665 ? Zn2 C46 2.59(7) 4_665 ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 C7 1.48(2) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 C20 1.55(2) . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C5 C33 1.52(2) . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C10 C13 1.50(2) . ? C11 C12 1.3900 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C16 C19 1.7618 . ? C17 C18 1.3900 . ? C19 O1 1.16(4) . ? C19 O2 1.17(4) . ? C20 C21 1.3900 . ? C20 C25 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C23 C26 1.52(2) . ? C24 C25 1.3900 . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C29 C32 1.4147 . ? C30 C31 1.3900 . ? C32 O3 1.22(3) . ? C32 O4 1.28(3) . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C36 C39 1.55(2) . ? C37 C38 1.3900 . ? C39 C40 1.3900 . ? C39 C44 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C42 C45 1.4592 . ? C43 C44 1.3900 . ? C45 O5 1.22(2) . ? C45 O6 1.32(2) . ? C46 O7 1.15(5) . ? C46 O8 1.19(5) . ? C46 C47 1.54(6) . ? C46 Zn2 2.59(6) 4_664 ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C50 C53 1.6514 . ? C51 C52 1.3900 . ? C51 N1 1.7952 . ? C53 O10 1.2114 . ? C53 O9 1.2187 . ? O3 Zn2 1.911(8) 1_655 ? O4 Zn1 2.056(11) 1_655 ? O5 Zn2 1.915(9) 1_545 ? O6 Zn1 1.950(9) 1_545 ? O7 Zn2 2.048(13) 4_664 ? 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 O10 Zn1 O1 102.1(5) . . ? O10 Zn1 O6 112.6(6) . 1_565 ? O1 Zn1 O6 129.9(7) . 1_565 ? O10 Zn1 O4 109.5(6) . 1_455 ? O1 Zn1 O4 100.1(5) . 1_455 ? O6 Zn1 O4 101.0(4) 1_565 1_455 ? O10 Zn1 C53 27.50(19) . . ? O1 Zn1 C53 92.0(4) . . ? O6 Zn1 C53 102.3(5) 1_565 . ? O4 Zn1 C53 136.9(6) 1_455 . ? O3 Zn2 O5 104.8(5) 1_455 1_565 ? O3 Zn2 O2 125.8(6) 1_455 . ? O5 Zn2 O2 105.7(5) 1_565 . ? O3 Zn2 O7 108.1(6) 1_455 4_665 ? O5 Zn2 O7 107.8(5) 1_565 4_665 ? O2 Zn2 O7 103.6(4) . 4_665 ? O3 Zn2 C46 99(3) 1_455 4_665 ? O5 Zn2 C46 133(2) 1_565 4_665 ? O2 Zn2 C46 91.1(17) . 4_665 ? O7 Zn2 C46 25.4(17) 4_665 4_665 ? C2 C1 C6 120.0 . . ? C2 C1 C7 119(3) . . ? C6 C1 C7 121(3) . . ? C1 C2 C3 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 C20 120(3) . . ? C4 C3 C20 120(3) . . ? C5 C4 C3 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 C33 123(3) . . ? C4 C5 C33 117(3) . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 C1 118(4) . . ? C12 C7 C1 122(4) . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 C13 121(4) . . ? C9 C10 C13 118(4) . . ? C10 C11 C12 120.0 . . ? C11 C12 C7 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 C10 127(3) . . ? C18 C13 C10 113(3) . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 C19 118.7 . . ? C17 C16 C19 119.9 . . ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? O1 C19 O2 129.2(12) . . ? O1 C19 C16 106.8(14) . . ? O2 C19 C16 99.7(13) . . ? C21 C20 C25 120.0 . . ? C21 C20 C3 117(3) . . ? C25 C20 C3 123(3) . . ? C20 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C24 C23 C26 114(3) . . ? C22 C23 C26 126(3) . . ? C25 C24 C23 120.0 . . ? C24 C25 C20 120.0 . . ? C27 C26 C31 120.0 . . ? C27 C26 C23 110(2) . . ? C31 C26 C23 130(2) . . ? C28 C27 C26 120.0 . . ? C27 C28 C29 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 C32 106.8 . . ? C28 C29 C32 133.1 . . ? C31 C30 C29 120.0 . . ? C30 C31 C26 120.0 . . ? O3 C32 O4 122.0(15) . . ? O3 C32 C29 130.0(16) . . ? O4 C32 C29 106.1(15) . . ? C34 C33 C38 120.0 . . ? C34 C33 C5 120(3) . . ? C38 C33 C5 119(3) . . ? C33 C34 C35 120.0 . . ? C34 C35 C36 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 C39 121(3) . . ? C35 C36 C39 119(3) . . ? C36 C37 C38 120.0 . . ? C37 C38 C33 120.0 . . ? C40 C39 C44 120.0 . . ? C40 C39 C36 125.7(14) . . ? C44 C39 C36 113.9(14) . . ? C41 C40 C39 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 C45 123.1 . . ? C43 C42 C45 115.3 . . ? C44 C43 C42 120.0 . . ? C43 C44 C39 120.0 . . ? O5 C45 O6 119.6(15) . . ? O5 C45 C42 121.3(11) . . ? O6 C45 C42 111.6(8) . . ? O7 C46 O8 122(5) . . ? O7 C46 C47 100(3) . . ? O8 C46 C47 137(4) . . ? O7 C46 Zn2 50(2) . 4_664 ? O8 C46 Zn2 78(3) . 4_664 ? C47 C46 Zn2 144(3) . 4_664 ? C48 C47 C52 120.0 . . ? C48 C47 C46 144(2) . . ? C52 C47 C46 96(2) . . ? C49 C48 C47 120.0 . . ? C48 C49 C50 120.0 . . ? C51 C50 C49 120.0 . . ? C51 C50 C53 123.8 . . ? C49 C50 C53 116.0 . . ? C50 C51 C52 120.0 . . ? C50 C51 N1 110.7 . . ? C52 C51 N1 129.2 . . ? C51 C52 C47 120.0 . . ? O10 C53 O9 118.8 . . ? O10 C53 C50 118.5 . . ? O9 C53 C50 121.8 . . ? O10 C53 Zn1 41.2(3) . . ? O9 C53 Zn1 78.3(3) . . ? C50 C53 Zn1 153.4(2) . . ? C19 O1 Zn1 120.7(10) . . ? C19 O2 Zn2 121.8(11) . . ? C32 O3 Zn2 134.8(13) . 1_655 ? C32 O4 Zn1 129.6(11) . 1_655 ? C45 O5 Zn2 134.6(12) . 1_545 ? C45 O6 Zn1 124.7(9) . 1_545 ? C46 O7 Zn2 105(2) . 4_664 ? C53 O10 Zn1 111.3(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 13.07 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.433 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.055 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.000 0.000 -0.002 7841 1199 ' ' _platon_squeeze_details ; ; #End of Crystallographic Information File