# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Ken-ichi Sakai' _publ_contact_author_email K-SAKAI@PHOTON.CHITOSE.AC.JP _publ_section_title ; Excited state intramolecular proton transfer in six-coordinated zinc(II)-quinoxaline complexes with ligand hydrogen bonds: their fluorescent properties sensitive to axial positions ; loop_ _publ_author_name 'Ken-ichi Sakai' 'Tomoyuki Akutagawa' 'Masaaki Dosen' 'Masako Kato' 'Ataru Kobayashi' 'Umpei Nagashima' ; T.Nakamura ; 'Sami Takahashi' #============================================================================== # 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 #============================================================================== # Attachment 'Zn-hqxc-py.cif' #============================================================================== data__sakaia _database_code_depnum_ccdc_archive 'CCDC 681305' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C28 H20 N6 O6 Zn ' _chemical_formula_moiety 'C28 H20 N6 O6 Zn ' _chemical_formula_weight 601.88 _chemical_melting_point ? _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/4-X,1/4+Y,1/4+Z 3 1/4+X,1/4-Y,1/4+Z 4 1/2-X,-Y,1/2+Z 5 +X,1/2+Y,1/2+Z 6 1/4-X,3/4+Y,3/4+Z 7 1/4+X,3/4-Y,3/4+Z 8 1/2-X,1/2-Y,+Z 9 1/2+X,+Y,1/2+Z 10 3/4-X,1/4+Y,3/4+Z 11 3/4+X,1/4-Y,3/4+Z 12 -X,-Y,+Z 13 1/2+X,1/2+Y,+Z 14 3/4-X,3/4+Y,1/4+Z 15 3/4+X,3/4-Y,1/4+Z 16 -X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 35.8455(18) _cell_length_b 10.1477(5) _cell_length_c 14.0206(8) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 5100.0(5) _cell_formula_units_Z 8 _cell_measurement_reflns_used 11690 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.4 _cell_measurement_temperature 89.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464.00 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.903 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_ambient_temperature 89.1 _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 12022 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_theta_max 27.44 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2898 _reflns_number_gt 2823 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0192 _refine_ls_wR_factor_ref 0.0256 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2825 _refine_ls_number_parameters 207 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 2136.5900 2939.4200 844.0310 ; _refine_ls_shift/su_max 0.0083 _refine_diff_density_max 0.59 _refine_diff_density_min -0.41 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 1386 Friedel Pairs' _refine_ls_abs_structure_Flack 0.566(14) 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) ; 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) ; N N 0.006 0.003 ; 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 0.0000 0.5000 0.13746(5) 0.01024(2) Uani 1.00 2 d S . . O(1) O 0.01635(2) 0.69556(6) 0.13720(7) 0.01375(15) Uani 1.00 1 d . . . O(2) O 0.06536(2) 0.83190(7) 0.13600(8) 0.01981(18) Uani 1.00 1 d . . . O(3) O 0.13137(2) 0.74304(8) 0.15139(8) 0.0296(2) Uani 1.00 1 d . . . N(1) N 0.06257(2) 0.48333(9) 0.14297(12) 0.01266(19) Uani 1.00 1 d . . . N(2) N 0.14061(2) 0.52259(9) 0.15098(10) 0.0234(2) Uani 1.00 1 d . . . N(3) N 0.0000 0.5000 0.29217(12) 0.0148(5) Uani 1.00 2 d S . . N(4) N 0.0000 0.5000 -0.01603(12) 0.0140(5) Uani 1.00 2 d S . . C(1) C 0.07725(3) 0.60238(11) 0.14441(11) 0.0145(2) Uani 1.00 1 d . . . C(2) C 0.11711(3) 0.62118(11) 0.14907(11) 0.0189(2) Uani 1.00 1 d . . . C(4) C 0.12572(3) 0.39890(11) 0.14981(11) 0.0196(2) Uani 1.00 1 d . . . C(5) C 0.08637(3) 0.37750(11) 0.14633(11) 0.0156(2) Uani 1.00 1 d . . . C(6) C 0.14977(3) 0.28744(12) 0.15152(11) 0.0270(3) Uani 1.00 1 d . . . C(7) C 0.13498(3) 0.16260(12) 0.15117(12) 0.0293(3) Uani 1.00 1 d . . . C(8) C 0.09594(3) 0.14177(12) 0.14788(13) 0.0257(3) Uani 1.00 1 d . . . C(9) C 0.07181(3) 0.24735(11) 0.14537(10) 0.0207(2) Uani 1.00 1 d . . . C(10) C 0.05078(3) 0.71942(9) 0.13921(10) 0.0134(2) Uani 1.00 1 d . . . C(11) C -0.00665(4) 0.61119(13) 0.34150(9) 0.0203(3) Uani 1.00 1 d . . . C(12) C -0.00690(4) 0.61426(16) 0.44047(10) 0.0308(4) Uani 1.00 1 d . . . C(13) C 0.000000(10) 0.500000(10) 0.48989(17) 0.0340(9) Uani 1.00 2 d S . . C(14) C 0.02887(4) 0.45051(13) -0.06615(9) 0.0207(3) Uani 1.00 1 d . . . C(15) C 0.03001(4) 0.44957(14) -0.16465(10) 0.0259(3) Uani 1.00 1 d . . . C(16) C 0.000000(10) 0.500000(10) -0.21429(17) 0.0291(8) Uani 1.00 2 d S . . H(1) H 0.1760 0.2999 0.1534 0.032 Uiso 1.00 1 c R . . H(2) H 0.1513 0.0889 0.1528 0.034 Uiso 1.00 1 c R . . H(3) H 0.0863 0.0546 0.1476 0.031 Uiso 1.00 1 c R . . H(4) H 0.0456 0.2332 0.1433 0.025 Uiso 1.00 1 c R . . H(5) H -0.0114 0.6900 0.3070 0.024 Uiso 1.00 1 c R . . H(6) H -0.0118 0.6943 0.4733 0.037 Uiso 1.00 1 c R . . H(7) H 0.0000 0.5000 0.5576 0.041 Uiso 1.00 2 c R . . H(8) H 0.0495 0.4146 -0.0323 0.025 Uiso 1.00 1 c R . . H(9) H 0.0511 0.4150 -0.1973 0.032 Uiso 1.00 1 c R . . H(10) H 0.0000 0.5000 -0.2821 0.036 Uiso 1.00 2 c R . . H(12) H 0.1119(5) 0.8080(19) 0.1457(18) 0.067(5) Uiso 1.00 1 c . . . 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) 0.00989(6) 0.01011(6) 0.01072(6) -0.00049(8) 0.0000 0.0000 O(1) 0.0139(2) 0.0109(3) 0.0164(3) 0.0000(2) 0.0009(3) 0.0018(3) O(2) 0.0216(3) 0.0111(3) 0.0267(4) -0.0029(2) 0.0018(4) 0.0004(4) O(3) 0.0180(4) 0.0157(3) 0.0549(6) -0.0035(3) -0.0023(4) -0.0002(5) N(1) 0.0129(3) 0.0119(4) 0.0132(4) -0.0008(3) -0.0011(5) -0.0002(5) N(2) 0.0137(3) 0.0196(5) 0.0369(8) -0.0026(3) -0.0022(4) 0.0015(5) N(3) 0.0088(12) 0.0210(12) 0.0145(9) -0.0024(7) 0.0000 0.0000 N(4) 0.0197(13) 0.0117(11) 0.0106(8) -0.0027(7) 0.0000 0.0000 C(1) 0.0138(4) 0.0158(4) 0.0139(5) 0.0010(3) -0.0006(5) 0.0014(5) C(2) 0.0136(5) 0.0172(5) 0.0259(6) -0.0025(3) -0.0006(5) 0.0009(5) C(4) 0.0150(5) 0.0166(5) 0.0270(7) 0.0001(4) -0.0032(5) 0.0022(5) C(5) 0.0150(4) 0.0147(5) 0.0171(6) 0.0019(3) -0.0012(5) 0.0000(5) C(6) 0.0134(5) 0.0241(5) 0.0435(9) 0.0034(4) -0.0032(5) 0.0021(6) C(7) 0.0200(5) 0.0223(6) 0.0457(9) 0.0084(4) -0.0020(6) 0.0036(6) C(8) 0.0212(5) 0.0144(4) 0.0415(8) 0.0016(4) -0.0001(6) 0.0018(6) C(9) 0.0174(5) 0.0177(5) 0.0270(5) 0.0004(3) 0.0004(4) 0.0010(8) C(10) 0.0156(4) 0.0133(4) 0.0113(4) -0.0001(3) 0.0004(5) -0.0004(4) C(11) 0.0176(7) 0.0241(6) 0.0193(5) -0.0056(5) 0.0030(4) -0.0040(4) C(12) 0.0287(9) 0.0418(8) 0.0218(6) -0.0137(6) 0.0071(5) -0.0153(5) C(13) 0.041(2) 0.051(2) 0.0093(10) -0.0258(14) 0.0000 0.0000 C(14) 0.0172(6) 0.0267(6) 0.0184(5) 0.0039(5) -0.0003(4) -0.0022(4) C(15) 0.0246(7) 0.0350(7) 0.0179(6) 0.0018(6) 0.0044(5) -0.0056(5) C(16) 0.0263(18) 0.049(2) 0.0117(10) -0.0024(12) 0.0000 0.0000 #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _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) O(1) 2.0692(6) yes . . Zn(1) O(1) 2.0692(6) yes . 12_565 Zn(1) N(1) 2.2505(7) yes . . Zn(1) N(1) 2.2505(7) yes . 12_565 Zn(1) N(3) 2.1691(18) yes . . Zn(1) N(4) 2.1520(18) yes . . O(1) C(10) 1.2580(12) yes . . O(2) C(10) 1.2562(11) yes . . O(3) C(2) 1.3385(13) yes . . N(1) C(1) 1.3179(14) yes . . N(1) C(5) 1.3724(13) yes . . N(2) C(2) 1.3081(13) yes . . N(2) C(4) 1.3640(14) yes . . N(3) C(11) 1.3447(15) yes . . N(3) C(11) 1.3447(15) yes . 12_565 N(4) C(14) 1.3479(16) yes . . N(4) C(14) 1.3479(16) yes . 12_565 C(1) C(2) 1.4430(15) yes . . C(1) C(10) 1.5219(14) yes . . C(4) C(5) 1.4280(15) yes . . C(4) C(6) 1.4223(16) yes . . C(5) C(9) 1.4202(15) yes . . C(6) C(7) 1.3733(16) yes . . C(7) C(8) 1.4160(15) yes . . C(8) C(9) 1.3774(16) yes . . C(11) C(12) 1.3880(18) yes . . C(12) C(13) 1.3732(19) yes . . C(14) C(15) 1.3817(18) yes . . C(15) C(16) 1.3797(18) yes . . O(3) H(12) 0.96(2) no . . C(6) H(1) 0.950 no . . C(7) H(2) 0.950 no . . C(8) H(3) 0.950 no . . C(9) H(4) 0.950 no . . C(11) H(5) 0.950 no . . C(12) H(6) 0.950 no . . C(13) H(7) 0.950 no . . C(14) H(8) 0.950 no . . C(15) H(9) 0.950 no . . C(16) H(10) 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 O(1) Zn(1) O(1) 179.80(5) yes . . 12_565 O(1) Zn(1) N(1) 77.87(3) yes . . . O(1) Zn(1) N(1) 102.14(3) yes . . 12_565 O(1) Zn(1) N(3) 90.10(3) yes . . . O(1) Zn(1) N(4) 89.90(3) yes . . . O(1) Zn(1) N(1) 102.14(3) yes 12_565 . . O(1) Zn(1) N(1) 77.87(3) yes 12_565 . 12_565 O(1) Zn(1) N(3) 90.10(3) yes 12_565 . . O(1) Zn(1) N(4) 89.90(3) yes 12_565 . . N(1) Zn(1) N(1) 176.07(7) yes . . 12_565 N(1) Zn(1) N(3) 88.03(4) yes . . . N(1) Zn(1) N(4) 91.97(4) yes . . . N(1) Zn(1) N(3) 88.03(4) yes 12_565 . . N(1) Zn(1) N(4) 91.97(4) yes 12_565 . . N(3) Zn(1) N(4) 180.0000 yes . . . Zn(1) O(1) C(10) 117.54(5) yes . . . Zn(1) N(1) C(1) 109.24(6) yes . . . Zn(1) N(1) C(5) 132.81(6) yes . . . C(1) N(1) C(5) 117.94(8) yes . . . C(2) N(2) C(4) 116.84(8) yes . . . Zn(1) N(3) C(11) 120.95(8) yes . . . Zn(1) N(3) C(11) 120.95(8) yes . . 12_565 C(11) N(3) C(11) 118.09(14) yes . . 12_565 Zn(1) N(4) C(14) 121.42(8) yes . . . Zn(1) N(4) C(14) 121.42(8) yes . . 12_565 C(14) N(4) C(14) 117.16(14) yes . . 12_565 N(1) C(1) C(2) 121.15(9) yes . . . N(1) C(1) C(10) 117.76(9) yes . . . C(2) C(1) C(10) 121.09(9) yes . . . O(3) C(2) N(2) 117.40(9) yes . . . O(3) C(2) C(1) 120.09(9) yes . . . N(2) C(2) C(1) 122.51(9) yes . . . N(2) C(4) C(5) 121.79(9) yes . . . N(2) C(4) C(6) 119.63(9) yes . . . C(5) C(4) C(6) 118.58(9) yes . . . N(1) C(5) C(4) 119.75(9) yes . . . N(1) C(5) C(9) 119.93(9) yes . . . C(4) C(5) C(9) 120.32(9) yes . . . C(4) C(6) C(7) 119.97(9) yes . . . C(6) C(7) C(8) 121.29(10) yes . . . C(7) C(8) C(9) 120.35(10) yes . . . C(5) C(9) C(8) 119.50(9) yes . . . O(1) C(10) O(2) 125.61(9) yes . . . O(1) C(10) C(1) 117.55(8) yes . . . O(2) C(10) C(1) 116.84(9) yes . . . N(3) C(11) C(12) 122.29(13) yes . . . C(11) C(12) C(13) 118.97(15) yes . . . C(12) C(13) C(12) 119.39(19) yes . . 12_565 N(4) C(14) C(15) 123.12(13) yes . . . C(14) C(15) C(16) 118.59(14) yes . . . C(15) C(16) C(15) 119.41(19) yes . . 12_565 C(2) O(3) H(12) 110.7(11) no . . . C(4) C(6) H(1) 119.7 no . . . C(7) C(6) H(1) 120.3 no . . . C(6) C(7) H(2) 119.3 no . . . C(8) C(7) H(2) 119.5 no . . . C(7) C(8) H(3) 120.0 no . . . C(9) C(8) H(3) 119.6 no . . . C(5) C(9) H(4) 120.3 no . . . C(8) C(9) H(4) 120.2 no . . . N(3) C(11) H(5) 118.4 no . . . C(12) C(11) H(5) 119.3 no . . . C(11) C(12) H(6) 120.3 no . . . C(13) C(12) H(6) 120.7 no . . . C(12) C(13) H(7) 120.3 no . . . C(12) C(13) H(7) 120.3 no 12_565 . . N(4) C(14) H(8) 118.6 no . . . C(15) C(14) H(8) 118.3 no . . . C(14) C(15) H(9) 120.5 no . . . C(16) C(15) H(9) 120.9 no . . . C(15) C(16) H(10) 120.3 no . . . C(15) C(16) H(10) 120.3 no 12_565 . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Zn(1) O(1) C(10) -92(7) ? . . 12_565 12_565 O(1) Zn(1) O(1) C(10) -92(7) ? 12_565 . . . O(1) Zn(1) N(1) C(1) 0.77(11) ? . . . . O(1) Zn(1) N(1) C(5) 179.67(17) ? . . . . N(1) Zn(1) O(1) C(10) 0.53(10) ? . . . . O(1) Zn(1) N(1) C(1) -179.44(11) ? . . 12_565 12_565 O(1) Zn(1) N(1) C(5) -0.54(17) ? . . 12_565 12_565 N(1) Zn(1) O(1) C(10) 176.51(10) ? 12_565 . . . O(1) Zn(1) N(3) C(11) 28.38(7) ? . . . . O(1) Zn(1) N(3) C(11) -151.62(7) ? . . . 12_565 N(3) Zn(1) O(1) C(10) 88.50(9) ? . . . . O(1) Zn(1) N(4) C(14) 99.43(6) ? . . . . O(1) Zn(1) N(4) C(14) -80.57(6) ? . . . 12_565 N(4) Zn(1) O(1) C(10) -91.50(9) ? . . . . O(1) Zn(1) N(1) C(1) -179.44(11) ? 12_565 . . . O(1) Zn(1) N(1) C(5) -0.54(17) ? 12_565 . . . N(1) Zn(1) O(1) C(10) 176.51(10) ? . . 12_565 12_565 O(1) Zn(1) N(1) C(1) 0.77(11) ? 12_565 . 12_565 12_565 O(1) Zn(1) N(1) C(5) 179.67(17) ? 12_565 . 12_565 12_565 N(1) Zn(1) O(1) C(10) 0.53(10) ? 12_565 . 12_565 12_565 O(1) Zn(1) N(3) C(11) -151.62(7) ? 12_565 . . . O(1) Zn(1) N(3) C(11) 28.38(7) ? 12_565 . . 12_565 N(3) Zn(1) O(1) C(10) 88.50(9) ? . . 12_565 12_565 O(1) Zn(1) N(4) C(14) -80.57(6) ? 12_565 . . . O(1) Zn(1) N(4) C(14) 99.43(6) ? 12_565 . . 12_565 N(4) Zn(1) O(1) C(10) -91.50(9) ? . . 12_565 12_565 N(1) Zn(1) N(1) C(1) -89.8(4) ? . . 12_565 12_565 N(1) Zn(1) N(1) C(5) 89.1(5) ? . . 12_565 12_565 N(1) Zn(1) N(1) C(1) -89.8(4) ? 12_565 . . . N(1) Zn(1) N(1) C(5) 89.1(5) ? 12_565 . . . N(1) Zn(1) N(3) C(11) 106.24(7) ? . . . . N(1) Zn(1) N(3) C(11) -73.76(7) ? . . . 12_565 N(3) Zn(1) N(1) C(1) -89.76(11) ? . . . . N(3) Zn(1) N(1) C(5) 89.14(16) ? . . . . N(1) Zn(1) N(4) C(14) 21.57(7) ? . . . . N(1) Zn(1) N(4) C(14) -158.43(7) ? . . . 12_565 N(4) Zn(1) N(1) C(1) 90.24(11) ? . . . . N(4) Zn(1) N(1) C(5) -90.86(16) ? . . . . N(1) Zn(1) N(3) C(11) -73.76(7) ? 12_565 . . . N(1) Zn(1) N(3) C(11) 106.24(7) ? 12_565 . . 12_565 N(3) Zn(1) N(1) C(1) -89.76(11) ? . . 12_565 12_565 N(3) Zn(1) N(1) C(5) 89.14(16) ? . . 12_565 12_565 N(1) Zn(1) N(4) C(14) -158.43(7) ? 12_565 . . . N(1) Zn(1) N(4) C(14) 21.57(7) ? 12_565 . . 12_565 N(4) Zn(1) N(1) C(1) 90.24(11) ? . . 12_565 12_565 N(4) Zn(1) N(1) C(5) -90.86(16) ? . . 12_565 12_565 Zn(1) O(1) C(10) O(2) 177.34(11) ? . . . . Zn(1) O(1) C(10) C(1) -1.64(16) ? . . . . Zn(1) N(1) C(1) C(2) 179.28(11) ? . . . . Zn(1) N(1) C(1) C(10) -1.79(17) ? . . . . Zn(1) N(1) C(5) C(4) -179.73(12) ? . . . . Zn(1) N(1) C(5) C(9) 0.9(2) ? . . . . C(1) N(1) C(5) C(4) -0.9(2) ? . . . . C(1) N(1) C(5) C(9) 179.72(14) ? . . . . C(5) N(1) C(1) C(2) 0.2(2) ? . . . . C(5) N(1) C(1) C(10) 179.13(13) ? . . . . C(2) N(2) C(4) C(5) 0.2(2) ? . . . . C(2) N(2) C(4) C(6) 179.84(14) ? . . . . C(4) N(2) C(2) O(3) 179.19(13) ? . . . . C(4) N(2) C(2) C(1) -1.0(2) ? . . . . Zn(1) N(3) C(11) C(12) 179.89(10) ? . . . . Zn(1) N(3) C(11) C(12) 179.89(10) ? . . 12_565 12_565 C(11) N(3) C(11) C(12) -0.11(13) ? . . 12_565 12_565 C(11) N(3) C(11) C(12) -0.11(17) ? 12_565 . . . Zn(1) N(4) C(14) C(15) -179.54(9) ? . . . . Zn(1) N(4) C(14) C(15) -179.54(9) ? . . 12_565 12_565 C(14) N(4) C(14) C(15) 0.46(16) ? . . 12_565 12_565 C(14) N(4) C(14) C(15) 0.46(16) ? 12_565 . . . N(1) C(1) C(2) O(3) -179.35(14) ? . . . . N(1) C(1) C(2) N(2) 0.8(2) ? . . . . N(1) C(1) C(10) O(1) 2.4(2) ? . . . . N(1) C(1) C(10) O(2) -176.65(14) ? . . . . C(2) C(1) C(10) O(1) -178.64(13) ? . . . . C(2) C(1) C(10) O(2) 2.3(2) ? . . . . C(10) C(1) C(2) O(3) 1.7(2) ? . . . . C(10) C(1) C(2) N(2) -178.09(14) ? . . . . N(2) C(4) C(5) N(1) 0.7(2) ? . . . . N(2) C(4) C(5) C(9) -179.89(14) ? . . . . N(2) C(4) C(6) C(7) 179.45(14) ? . . . . C(5) C(4) C(6) C(7) -0.9(2) ? . . . . C(6) C(4) C(5) N(1) -178.89(14) ? . . . . C(6) C(4) C(5) C(9) 0.5(2) ? . . . . N(1) C(5) C(9) C(8) 179.41(15) ? . . . . C(4) C(5) C(9) C(8) 0.04(17) ? . . . . C(4) C(6) C(7) C(8) 0.8(2) ? . . . . C(6) C(7) C(8) C(9) -0.3(2) ? . . . . C(7) C(8) C(9) C(5) -0.1(2) ? . . . . N(3) C(11) C(12) C(13) 0.22(19) ? . . . . C(11) C(12) C(13) C(12) -0.11(13) ? . . . 12_565 N(4) C(14) C(15) C(16) -0.90(19) ? . . . . C(14) C(15) C(16) C(15) 0.42(16) ? . . . 12_565 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 O(1) C(12) 3.3834(17) ? . 16_564 O(2) C(8) 3.3342(14) ? . 1_565 O(2) C(12) 3.4936(17) ? . 16_564 O(2) C(13) 3.5490(16) ? . 5_554 O(2) C(15) 3.2930(17) ? . 5_555 O(2) C(16) 3.5784(16) ? . 5_555 O(3) N(2) 3.5995(17) ? . 2_555 O(3) C(14) 3.2781(16) ? . 2_555 O(3) C(15) 3.3381(16) ? . 2_555 N(2) O(3) 3.5995(17) ? . 6_544 N(2) C(14) 3.4355(16) ? . 2_555 N(2) C(15) 3.4883(16) ? . 2_555 C(2) C(4) 3.536(2) ? . 2_555 C(4) C(2) 3.536(2) ? . 6_544 C(4) C(7) 3.548(2) ? . 2_555 C(7) C(4) 3.548(2) ? . 6_544 C(8) O(2) 3.3342(14) ? . 1_545 C(12) O(1) 3.3834(17) ? . 16_565 C(12) O(2) 3.4936(17) ? . 16_565 C(13) O(2) 3.5490(16) ? . 5_545 C(13) O(2) 3.5490(16) ? . 16_565 C(14) O(3) 3.2781(16) ? . 6_544 C(14) N(2) 3.4355(16) ? . 6_544 C(15) O(2) 3.2930(17) ? . 5_544 C(15) O(3) 3.3381(16) ? . 6_544 C(15) N(2) 3.4883(16) ? . 6_544 C(16) O(2) 3.5784(16) ? . 5_544 C(16) O(2) 3.5784(16) ? . 16_564 O(1) H(6) 2.561 ? . 16_564 O(1) H(7) 3.336 ? . 5_554 O(1) H(9) 3.449 ? . 5_555 O(1) H(10) 3.342 ? . 5_555 O(2) H(2) 3.482 ? . 6_554 O(2) H(3) 2.386 ? . 1_565 O(2) H(6) 2.993 ? . 16_564 O(2) H(7) 3.099 ? . 5_554 O(2) H(9) 2.537 ? . 5_555 O(2) H(10) 3.118 ? . 5_555 O(3) H(2) 3.582 ? . 1_565 O(3) H(3) 3.552 ? . 1_565 O(3) H(8) 2.765 ? . 2_555 O(3) H(9) 2.899 ? . 2_555 N(2) H(8) 2.751 ? . 2_555 N(2) H(9) 2.891 ? . 2_555 N(2) H(12) 3.60(2) ? . 6_544 N(3) H(1) 3.118 ? . 2_555 N(3) H(1) 3.118 ? . 15_455 N(4) H(6) 3.134 ? . 5_544 N(4) H(6) 3.134 ? . 16_564 C(2) H(8) 3.173 ? . 2_555 C(2) H(9) 3.260 ? . 2_555 C(6) H(3) 3.491 ? . 2_555 C(7) H(12) 3.59(2) ? . 2_545 C(8) H(9) 3.549 ? . 5_545 C(8) H(12) 3.434(19) ? . 1_545 C(10) H(6) 2.851 ? . 16_564 C(10) H(7) 3.568 ? . 5_554 C(10) H(9) 3.032 ? . 5_555 C(10) H(10) 3.555 ? . 5_555 C(11) H(1) 3.081 ? . 2_555 C(11) H(1) 3.041 ? . 15_455 C(11) H(2) 3.447 ? . 15_455 C(12) H(1) 3.017 ? . 2_555 C(12) H(1) 2.971 ? . 15_455 C(12) H(2) 3.367 ? . 15_455 C(13) H(1) 2.959 ? . 2_555 C(13) H(1) 2.959 ? . 15_455 C(13) H(4) 3.592 ? . 5_555 C(13) H(4) 3.592 ? . 16_555 C(13) H(10) 3.198 ? . 1_556 C(14) H(5) 3.497 ? . 5_544 C(14) H(6) 3.032 ? . 5_544 C(15) H(3) 3.483 ? . 5_554 C(15) H(5) 3.048 ? . 5_544 C(15) H(6) 3.563 ? . 5_544 C(16) H(4) 3.502 ? . 5_554 C(16) H(4) 3.502 ? . 16_554 C(16) H(5) 3.186 ? . 5_544 C(16) H(5) 3.186 ? . 16_564 C(16) H(7) 3.198 ? . 1_554 H(1) N(3) 3.118 ? . 6_544 H(1) C(11) 3.081 ? . 6_544 H(1) C(11) 3.041 ? . 7_554 H(1) C(12) 3.017 ? . 6_544 H(1) C(12) 2.971 ? . 7_554 H(1) C(13) 2.959 ? . 6_544 H(1) H(3) 3.452 ? . 2_555 H(1) H(5) 3.577 ? . 7_554 H(1) H(6) 3.545 ? . 6_544 H(1) H(6) 3.473 ? . 7_554 H(1) H(7) 3.459 ? . 6_544 H(2) O(2) 3.482 ? . 2_545 H(2) O(3) 3.582 ? . 1_545 H(2) C(11) 3.447 ? . 7_554 H(2) C(12) 3.367 ? . 7_554 H(2) H(5) 3.420 ? . 7_554 H(2) H(6) 3.285 ? . 7_554 H(2) H(12) 3.183 ? . 1_545 H(2) H(12) 3.453 ? . 2_545 H(3) O(2) 2.386 ? . 1_545 H(3) O(3) 3.552 ? . 1_545 H(3) C(6) 3.491 ? . 6_544 H(3) C(15) 3.483 ? . 5_545 H(3) H(1) 3.452 ? . 6_544 H(3) H(7) 3.385 ? . 5_544 H(3) H(9) 2.885 ? . 5_545 H(3) H(10) 3.292 ? . 5_545 H(3) H(12) 2.665 ? . 1_545 H(4) C(13) 3.592 ? . 5_544 H(4) C(16) 3.502 ? . 5_545 H(4) H(6) 3.175 ? . 5_544 H(4) H(7) 3.117 ? . 5_544 H(4) H(10) 3.061 ? . 5_545 H(5) C(14) 3.497 ? . 5_555 H(5) C(15) 3.048 ? . 5_555 H(5) C(16) 3.186 ? . 5_555 H(5) H(1) 3.577 ? . 15_455 H(5) H(2) 3.420 ? . 15_455 H(5) H(9) 3.197 ? . 5_555 H(5) H(10) 3.409 ? . 5_555 H(6) O(1) 2.561 ? . 16_565 H(6) O(2) 2.993 ? . 16_565 H(6) N(4) 3.134 ? . 5_555 H(6) C(10) 2.851 ? . 16_565 H(6) C(14) 3.032 ? . 5_555 H(6) C(15) 3.563 ? . 5_555 H(6) H(1) 3.545 ? . 2_555 H(6) H(1) 3.473 ? . 15_455 H(6) H(2) 3.285 ? . 15_455 H(6) H(4) 3.175 ? . 5_555 H(6) H(8) 3.135 ? . 5_555 H(7) O(1) 3.336 ? . 5_545 H(7) O(1) 3.336 ? . 16_565 H(7) O(2) 3.099 ? . 5_545 H(7) O(2) 3.099 ? . 16_565 H(7) C(10) 3.568 ? . 5_545 H(7) C(10) 3.568 ? . 16_565 H(7) C(16) 3.198 ? . 1_556 H(7) H(1) 3.459 ? . 2_555 H(7) H(1) 3.459 ? . 15_455 H(7) H(3) 3.385 ? . 5_555 H(7) H(3) 3.385 ? . 16_555 H(7) H(4) 3.117 ? . 5_555 H(7) H(4) 3.117 ? . 16_555 H(7) H(10) 2.248 ? . 1_556 H(8) O(3) 2.765 ? . 6_544 H(8) N(2) 2.751 ? . 6_544 H(8) C(2) 3.173 ? . 6_544 H(8) H(6) 3.135 ? . 5_544 H(9) O(1) 3.449 ? . 5_544 H(9) O(2) 2.537 ? . 5_544 H(9) O(3) 2.899 ? . 6_544 H(9) N(2) 2.891 ? . 6_544 H(9) C(2) 3.260 ? . 6_544 H(9) C(8) 3.549 ? . 5_554 H(9) C(10) 3.032 ? . 5_544 H(9) H(3) 2.885 ? . 5_554 H(9) H(5) 3.197 ? . 5_544 H(9) H(12) 3.282 ? . 5_544 H(10) O(1) 3.342 ? . 5_544 H(10) O(1) 3.342 ? . 16_564 H(10) O(2) 3.118 ? . 5_544 H(10) O(2) 3.118 ? . 16_564 H(10) C(10) 3.555 ? . 5_544 H(10) C(10) 3.555 ? . 16_564 H(10) C(13) 3.198 ? . 1_554 H(10) H(3) 3.292 ? . 5_554 H(10) H(3) 3.292 ? . 16_554 H(10) H(4) 3.061 ? . 5_554 H(10) H(4) 3.061 ? . 16_554 H(10) H(5) 3.409 ? . 5_544 H(10) H(5) 3.409 ? . 16_564 H(10) H(7) 2.248 ? . 1_554 H(12) N(2) 3.60(2) ? . 2_555 H(12) C(7) 3.59(2) ? . 6_554 H(12) C(8) 3.434(19) ? . 1_565 H(12) H(2) 3.183 ? . 1_565 H(12) H(2) 3.453 ? . 6_554 H(12) H(3) 2.665 ? . 1_565 H(12) H(9) 3.282 ? . 5_555 _chemical_name_common zn-hqxc-dmso # Attachment 'Zn-hqxc-dmso.cif' ##============================================================================== data__zn-hqxc-dmso _database_code_depnum_ccdc_archive 'CCDC 746608' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C22 H22 N4 O8 S2 Zn ' _chemical_formula_moiety 'C22 H22 N4 O8 S2 Zn ' _chemical_formula_weight 599.94 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.7056(4) _cell_length_b 10.0802(6) _cell_length_c 12.8400(5) _cell_angle_alpha 90.0000 _cell_angle_beta 109.6550(12) _cell_angle_gamma 90.0000 _cell_volume 1183.00(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10503 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 90 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616.00 _exptl_absorpt_coefficient_mu 1.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.880 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_ambient_temperature 90 _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 11227 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_theta_max 27.46 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2675 _reflns_number_gt 2403 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0425 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2411 _refine_ls_number_parameters 183 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979) 2524.1800 3463.3300 986.0310 ; _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.85 _refine_diff_density_min -0.53 _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) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; Zn Zn 0.284 1.430 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; 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 0.0000 0.0000 0.01046(5) Uani 1.00 2 d S . . S(1) S 0.74929(4) -0.07737(4) 0.22485(3) 0.01359(8) Uani 1.00 1 d . . . O(1) O 0.56461(12) -0.19224(11) -0.00177(9) 0.0143(2) Uani 1.00 1 d . . . O(2) O 0.72362(13) -0.32583(12) -0.04117(10) 0.0191(3) Uani 1.00 1 d . . . O(3) O 0.91418(14) -0.23186(12) -0.11761(10) 0.0181(3) Uani 1.00 1 d . . . O(4) O 0.64198(12) 0.03184(11) 0.16614(9) 0.0156(2) Uani 1.00 1 d . . . N(1) N 0.68817(14) 0.02243(13) -0.06149(10) 0.0114(3) Uani 1.00 1 d . . . N(2) N 0.92513(13) -0.01028(15) -0.14039(10) 0.0133(3) Uani 1.00 1 d . . . C(1) C 0.75192(17) 0.13066(16) -0.09110(13) 0.0119(3) Uani 1.00 1 d . . . C(2) C 0.70057(18) 0.26014(16) -0.08121(13) 0.0134(3) Uani 1.00 1 d . . . C(3) C 0.76701(18) 0.36801(16) -0.10923(14) 0.0157(3) Uani 1.00 1 d . . . C(4) C 0.88467(18) 0.35054(17) -0.14945(14) 0.0171(3) Uani 1.00 1 d . . . C(5) C 0.93475(18) 0.22619(17) -0.16111(14) 0.0163(3) Uani 1.00 1 d . . . C(6) C 0.87042(18) 0.11307(16) -0.13149(13) 0.0131(3) Uani 1.00 1 d . . . C(8) C 0.86250(18) -0.11104(16) -0.10982(13) 0.0139(3) Uani 1.00 1 d . . . C(9) C 0.74143(17) -0.09523(16) -0.06951(13) 0.0122(3) Uani 1.00 1 d . . . C(10) C 0.67113(17) -0.21394(16) -0.03488(13) 0.0133(3) Uani 1.00 1 d . . . C(11) C 0.88636(18) 0.0033(2) 0.33583(14) 0.0222(3) Uani 1.00 1 d . . . C(12) C 0.6600(2) -0.16761(19) 0.30307(15) 0.0236(4) Uani 1.00 1 d . . . H(1) H 0.6209 0.2723 -0.0549 0.016 Uiso 1.00 1 c R . . H(2) H 0.7333 0.4548 -0.1018 0.019 Uiso 1.00 1 c R . . H(3) H 0.9299 0.4260 -0.1684 0.020 Uiso 1.00 1 c R . . H(4) H 1.0128 0.2159 -0.1895 0.020 Uiso 1.00 1 c R . . H(5) H 0.9630 0.0331 0.3112 0.026 Uiso 1.00 1 c R . . H(6) H 0.8441 0.0770 0.3600 0.025 Uiso 1.00 1 c R . . H(7) H 0.9247 -0.0571 0.3954 0.026 Uiso 1.00 1 c R . . H(8) H 0.5572 -0.1639 0.2666 0.029 Uiso 1.00 1 c R . . H(9) H 0.6837 -0.1295 0.3746 0.029 Uiso 1.00 1 c R . . H(10) H 0.6914 -0.2574 0.3097 0.029 Uiso 1.00 1 c R . . H(12) H 0.862(2) -0.280(2) -0.0932(18) 0.032(6) Uiso 1.00 1 c . . . 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) 0.01016(12) 0.00958(12) 0.01257(12) 0.00099(10) 0.00506(9) 0.00020(10) S(1) 0.01220(17) 0.01548(18) 0.01304(18) 0.00158(15) 0.00416(15) -0.00075(14) O(1) 0.0143(5) 0.0117(5) 0.0184(5) 0.0005(4) 0.0075(4) 0.0006(4) O(2) 0.0215(6) 0.0110(5) 0.0281(6) 0.0022(4) 0.0125(5) -0.0012(4) O(3) 0.0182(6) 0.0157(5) 0.0240(6) 0.0040(4) 0.0119(5) -0.0008(5) O(4) 0.0155(5) 0.0164(5) 0.0144(5) 0.0016(4) 0.0043(4) 0.0002(4) N(1) 0.0103(5) 0.0129(6) 0.0104(5) 0.0004(4) 0.0028(4) -0.0004(4) N(2) 0.0115(5) 0.0165(6) 0.0135(6) 0.0024(5) 0.0063(5) -0.0006(5) C(1) 0.0100(6) 0.0150(7) 0.0099(7) -0.0007(5) 0.0023(5) -0.0001(5) C(2) 0.0126(7) 0.0146(7) 0.0131(7) 0.0010(5) 0.0043(5) -0.0006(5) C(3) 0.0150(7) 0.0137(7) 0.0176(7) 0.0005(6) 0.0045(6) -0.0007(6) C(4) 0.0158(7) 0.0169(8) 0.0184(8) -0.0036(6) 0.0054(6) 0.0026(6) C(5) 0.0126(7) 0.0213(8) 0.0170(7) -0.0003(6) 0.0076(6) 0.0005(6) C(6) 0.0113(7) 0.0153(7) 0.0121(7) 0.0010(5) 0.0030(6) -0.0006(5) C(8) 0.0126(7) 0.0161(7) 0.0130(7) 0.0027(5) 0.0043(6) -0.0025(5) C(9) 0.0112(6) 0.0131(7) 0.0118(7) 0.0006(5) 0.0034(5) -0.0011(5) C(10) 0.0132(7) 0.0131(7) 0.0122(7) 0.0005(5) 0.0025(5) -0.0010(5) C(11) 0.0147(7) 0.0232(8) 0.0245(8) -0.0012(7) 0.0011(6) -0.0032(7) C(12) 0.0223(8) 0.0240(9) 0.0244(9) -0.0014(7) 0.0075(7) 0.0077(7) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _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) O(1) 2.0392(11) yes . . Zn(1) O(1) 2.0392(11) yes . 3_655 Zn(1) O(4) 2.1389(9) yes . . Zn(1) O(4) 2.1389(9) yes . 3_655 Zn(1) N(1) 2.2316(15) yes . . Zn(1) N(1) 2.2316(15) yes . 3_655 S(1) O(4) 1.5286(11) yes . . S(1) C(11) 1.7849(16) yes . . S(1) C(12) 1.781(2) yes . . O(1) C(10) 1.262(2) yes . . O(2) C(10) 1.251(2) yes . . O(3) C(8) 1.334(2) yes . . N(1) C(1) 1.370(2) yes . . N(1) C(9) 1.312(2) yes . . N(2) C(6) 1.372(2) yes . . N(2) C(8) 1.310(2) yes . . C(1) C(2) 1.418(2) yes . . C(1) C(6) 1.423(2) yes . . C(2) C(3) 1.372(2) yes . . C(3) C(4) 1.414(2) yes . . C(4) C(5) 1.371(2) yes . . C(5) C(6) 1.412(2) yes . . C(8) C(9) 1.443(2) yes . . C(9) C(10) 1.516(2) yes . . O(3) H(12) 0.83(2) no . . C(2) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(4) H(3) 0.950 no . . C(5) H(4) 0.950 no . . C(11) H(5) 0.950 no . . C(11) H(6) 0.950 no . . C(11) H(7) 0.950 no . . C(12) H(8) 0.950 no . . C(12) H(9) 0.950 no . . C(12) H(10) 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 O(1) Zn(1) O(1) 180.00(6) yes . . 3_655 O(1) Zn(1) O(4) 93.23(4) yes . . . O(1) Zn(1) O(4) 86.77(4) yes . . 3_655 O(1) Zn(1) N(1) 78.52(4) yes . . . O(1) Zn(1) N(1) 101.48(4) yes . . 3_655 O(1) Zn(1) O(4) 86.77(4) yes 3_655 . . O(1) Zn(1) O(4) 93.23(4) yes 3_655 . 3_655 O(1) Zn(1) N(1) 101.48(4) yes 3_655 . . O(1) Zn(1) N(1) 78.52(4) yes 3_655 . 3_655 O(4) Zn(1) O(4) 180.00(6) yes . . 3_655 O(4) Zn(1) N(1) 90.47(4) yes . . . O(4) Zn(1) N(1) 89.53(4) yes . . 3_655 O(4) Zn(1) N(1) 89.53(4) yes 3_655 . . O(4) Zn(1) N(1) 90.47(4) yes 3_655 . 3_655 N(1) Zn(1) N(1) 180.00(440) yes . . 3_655 O(4) S(1) C(11) 105.49(7) yes . . . O(4) S(1) C(12) 105.42(8) yes . . . C(11) S(1) C(12) 98.96(8) yes . . . Zn(1) O(1) C(10) 117.27(10) yes . . . Zn(1) O(4) S(1) 119.16(6) yes . . . Zn(1) N(1) C(1) 132.75(11) yes . . . Zn(1) N(1) C(9) 109.10(11) yes . . . C(1) N(1) C(9) 118.15(15) yes . . . C(6) N(2) C(8) 116.50(15) yes . . . N(1) C(1) C(2) 120.21(16) yes . . . N(1) C(1) C(6) 119.86(14) yes . . . C(2) C(1) C(6) 119.93(15) yes . . . C(1) C(2) C(3) 119.70(17) yes . . . C(2) C(3) C(4) 120.37(15) yes . . . C(3) C(4) C(5) 120.90(16) yes . . . C(4) C(5) C(6) 120.25(18) yes . . . N(2) C(6) C(1) 121.76(15) yes . . . N(2) C(6) C(5) 119.40(16) yes . . . C(1) C(6) C(5) 118.84(15) yes . . . O(3) C(8) N(2) 117.48(17) yes . . . O(3) C(8) C(9) 119.99(15) yes . . . N(2) C(8) C(9) 122.53(15) yes . . . N(1) C(9) C(8) 121.19(15) yes . . . N(1) C(9) C(10) 117.55(16) yes . . . C(8) C(9) C(10) 121.26(14) yes . . . O(1) C(10) O(2) 125.12(16) yes . . . O(1) C(10) C(9) 117.54(14) yes . . . O(2) C(10) C(9) 117.34(16) yes . . . C(8) O(3) H(12) 102.1(18) no . . . C(1) C(2) H(1) 120.2 no . . . C(3) C(2) H(1) 120.1 no . . . C(2) C(3) H(2) 119.7 no . . . C(4) C(3) H(2) 119.9 no . . . C(3) C(4) H(3) 119.6 no . . . C(5) C(4) H(3) 119.5 no . . . C(4) C(5) H(4) 119.9 no . . . C(6) C(5) H(4) 119.8 no . . . S(1) C(11) H(5) 109.6 no . . . S(1) C(11) H(6) 109.2 no . . . S(1) C(11) H(7) 109.6 no . . . H(5) C(11) H(6) 109.5 no . . . H(5) C(11) H(7) 109.5 no . . . H(6) C(11) H(7) 109.5 no . . . S(1) C(12) H(8) 109.4 no . . . S(1) C(12) H(9) 109.5 no . . . S(1) C(12) H(10) 109.6 no . . . H(8) C(12) H(9) 109.5 no . . . H(8) C(12) H(10) 109.5 no . . . H(9) C(12) H(10) 109.5 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Zn(1) O(4) S(1) 5.82(8) ? . . . . O(4) Zn(1) O(1) C(10) -90.66(10) ? . . . . O(1) Zn(1) O(4) S(1) 174.18(8) ? . . 3_655 3_655 O(4) Zn(1) O(1) C(10) 89.34(10) ? 3_655 . . . O(1) Zn(1) N(1) C(1) -179.46(12) ? . . . . O(1) Zn(1) N(1) C(9) 1.21(8) ? . . . . N(1) Zn(1) O(1) C(10) -0.83(9) ? . . . . O(1) Zn(1) N(1) C(1) -0.54(12) ? . . 3_655 3_655 O(1) Zn(1) N(1) C(9) 178.79(8) ? . . 3_655 3_655 N(1) Zn(1) O(1) C(10) 179.17(9) ? 3_655 . . . O(1) Zn(1) O(4) S(1) -174.18(8) ? 3_655 . . . O(4) Zn(1) O(1) C(10) -89.34(10) ? . . 3_655 3_655 O(1) Zn(1) O(4) S(1) -5.82(8) ? 3_655 . 3_655 3_655 O(4) Zn(1) O(1) C(10) 90.66(10) ? 3_655 . 3_655 3_655 O(1) Zn(1) N(1) C(1) 0.54(12) ? 3_655 . . . O(1) Zn(1) N(1) C(9) -178.79(8) ? 3_655 . . . N(1) Zn(1) O(1) C(10) -179.17(9) ? . . 3_655 3_655 O(1) Zn(1) N(1) C(1) 179.46(12) ? 3_655 . 3_655 3_655 O(1) Zn(1) N(1) C(9) -1.21(8) ? 3_655 . 3_655 3_655 N(1) Zn(1) O(1) C(10) 0.83(9) ? 3_655 . 3_655 3_655 O(4) Zn(1) N(1) C(1) -86.26(12) ? . . . . O(4) Zn(1) N(1) C(9) 94.40(9) ? . . . . N(1) Zn(1) O(4) S(1) -72.71(8) ? . . . . O(4) Zn(1) N(1) C(1) -93.74(12) ? . . 3_655 3_655 O(4) Zn(1) N(1) C(9) 85.60(9) ? . . 3_655 3_655 N(1) Zn(1) O(4) S(1) 107.29(8) ? 3_655 . . . O(4) Zn(1) N(1) C(1) 93.74(12) ? 3_655 . . . O(4) Zn(1) N(1) C(9) -85.60(9) ? 3_655 . . . N(1) Zn(1) O(4) S(1) -107.29(8) ? . . 3_655 3_655 O(4) Zn(1) N(1) C(1) 86.26(12) ? 3_655 . 3_655 3_655 O(4) Zn(1) N(1) C(9) -94.40(9) ? 3_655 . 3_655 3_655 N(1) Zn(1) O(4) S(1) 72.71(8) ? 3_655 . 3_655 3_655 C(11) S(1) O(4) Zn(1) 160.16(8) ? . . . . C(12) S(1) O(4) Zn(1) -95.71(9) ? . . . . Zn(1) O(1) C(10) O(2) -179.82(11) ? . . . . Zn(1) O(1) C(10) C(9) 0.35(15) ? . . . . Zn(1) N(1) C(1) C(2) 2.31(19) ? . . . . Zn(1) N(1) C(1) C(6) -177.94(9) ? . . . . Zn(1) N(1) C(9) C(8) 178.59(10) ? . . . . Zn(1) N(1) C(9) C(10) -1.41(14) ? . . . . C(1) N(1) C(9) C(8) -0.86(19) ? . . . . C(1) N(1) C(9) C(10) 179.14(11) ? . . . . C(9) N(1) C(1) C(2) -178.40(12) ? . . . . C(9) N(1) C(1) C(6) 1.35(19) ? . . . . C(6) N(2) C(8) O(3) -179.88(12) ? . . . . C(6) N(2) C(8) C(9) 0.48(19) ? . . . . C(8) N(2) C(6) C(1) 0.04(13) ? . . . . C(8) N(2) C(6) C(5) 178.83(13) ? . . . . N(1) C(1) C(2) C(3) 178.82(13) ? . . . . N(1) C(1) C(6) N(2) -1.0(2) ? . . . . N(1) C(1) C(6) C(5) -179.76(12) ? . . . . C(2) C(1) C(6) N(2) 178.78(12) ? . . . . C(2) C(1) C(6) C(5) -0.01(17) ? . . . . C(6) C(1) C(2) C(3) -0.9(2) ? . . . . C(1) C(2) C(3) C(4) 1.0(2) ? . . . . C(2) C(3) C(4) C(5) -0.09(19) ? . . . . C(3) C(4) C(5) C(6) -0.9(2) ? . . . . C(4) C(5) C(6) N(2) -177.91(13) ? . . . . C(4) C(5) C(6) C(1) 0.9(2) ? . . . . O(3) C(8) C(9) N(1) -179.71(12) ? . . . . O(3) C(8) C(9) C(10) 0.3(2) ? . . . . N(2) C(8) C(9) N(1) -0.08(17) ? . . . . N(2) C(8) C(9) C(10) 179.92(12) ? . . . . N(1) C(9) C(10) O(1) 0.84(19) ? . . . . N(1) C(9) C(10) O(2) -179.01(12) ? . . . . C(8) C(9) C(10) O(1) -179.16(12) ? . . . . C(8) C(9) C(10) O(2) 1.0(2) ? . . . . 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 O(2) C(3) 3.273(2) ? . 1_545 O(2) C(5) 3.5994(18) ? . 3_755 O(2) C(11) 3.599(2) ? . 2_645 O(2) C(11) 3.596(2) ? . 4_444 O(3) C(1) 3.5892(17) ? . 3_755 O(3) C(3) 3.5012(19) ? . 2_644 O(3) C(4) 3.4947(18) ? . 2_644 O(3) C(4) 3.5352(19) ? . 3_755 O(3) C(5) 3.381(2) ? . 3_755 O(3) C(6) 3.3965(18) ? . 3_755 O(3) C(12) 3.065(2) ? . 4_544 O(4) C(12) 3.538(2) ? . 2_655 N(2) N(2) 3.4100(16) ? . 3_755 N(2) C(3) 3.3593(19) ? . 2_644 N(2) C(4) 3.5823(18) ? . 2_644 N(2) C(6) 3.5409(18) ? . 3_755 N(2) C(8) 3.4075(18) ? . 3_755 N(2) C(11) 3.569(2) ? . 3_755 C(1) O(3) 3.5892(17) ? . 3_755 C(2) C(12) 3.445(2) ? . 2_655 C(3) O(2) 3.273(2) ? . 1_565 C(3) O(3) 3.5012(19) ? . 2_654 C(3) N(2) 3.3593(19) ? . 2_654 C(3) C(8) 3.404(2) ? . 2_654 C(4) O(3) 3.4947(18) ? . 2_654 C(4) O(3) 3.5352(19) ? . 3_755 C(4) N(2) 3.5823(18) ? . 2_654 C(4) C(8) 3.236(2) ? . 2_654 C(4) C(9) 3.442(2) ? . 2_654 C(5) O(2) 3.5994(18) ? . 3_755 C(5) O(3) 3.381(2) ? . 3_755 C(5) C(8) 3.566(2) ? . 3_755 C(6) O(3) 3.3965(18) ? . 3_755 C(6) N(2) 3.5409(18) ? . 3_755 C(6) C(8) 3.3041(19) ? . 3_755 C(8) N(2) 3.4075(18) ? . 3_755 C(8) C(3) 3.404(2) ? . 2_644 C(8) C(4) 3.236(2) ? . 2_644 C(8) C(5) 3.566(2) ? . 3_755 C(8) C(6) 3.3041(19) ? . 3_755 C(9) C(4) 3.442(2) ? . 2_644 C(11) O(2) 3.599(2) ? . 2_655 C(11) O(2) 3.596(2) ? . 4_545 C(11) N(2) 3.569(2) ? . 3_755 C(12) O(3) 3.065(2) ? . 4_445 C(12) O(4) 3.538(2) ? . 2_645 C(12) C(2) 3.445(2) ? . 2_645 S(1) H(4) 2.863 ? . 3_755 S(1) H(10) 3.332 ? . 2_655 O(1) H(6) 2.903 ? . 2_645 O(1) H(7) 2.961 ? . 4_444 O(2) H(2) 2.357 ? . 1_545 O(2) H(4) 3.474 ? . 2_644 O(2) H(4) 3.383 ? . 3_755 O(2) H(5) 3.337 ? . 4_444 O(2) H(6) 2.799 ? . 2_645 O(2) H(7) 3.581 ? . 2_645 O(2) H(7) 2.981 ? . 4_444 O(3) H(3) 3.523 ? . 1_545 O(3) H(8) 2.575 ? . 4_544 O(3) H(9) 2.997 ? . 4_544 O(3) H(10) 3.133 ? . 4_544 O(4) H(3) 3.445 ? . 4_455 O(4) H(10) 2.624 ? . 2_655 N(1) H(3) 3.408 ? . 2_644 N(2) H(2) 3.165 ? . 2_644 N(2) H(3) 3.553 ? . 2_644 N(2) H(5) 2.765 ? . 3_755 C(1) H(9) 3.577 ? . 2_655 C(2) H(5) 3.070 ? . 4_454 C(2) H(7) 3.537 ? . 2_655 C(2) H(9) 2.744 ? . 2_655 C(2) H(10) 3.291 ? . 2_655 C(3) H(5) 2.952 ? . 4_454 C(3) H(9) 2.887 ? . 2_655 C(4) H(12) 3.33(2) ? . 3_755 C(5) H(5) 3.580 ? . 3_755 C(5) H(12) 3.48(2) ? . 2_654 C(5) H(12) 3.24(2) ? . 3_755 C(6) H(5) 3.552 ? . 3_755 C(6) H(12) 3.59(2) ? . 3_755 C(8) H(2) 3.563 ? . 2_644 C(8) H(3) 3.296 ? . 2_644 C(9) H(3) 3.220 ? . 2_644 C(9) H(4) 3.591 ? . 3_755 C(10) H(2) 3.550 ? . 1_545 C(10) H(4) 3.459 ? . 2_644 C(10) H(4) 3.430 ? . 3_755 C(10) H(6) 3.119 ? . 2_645 C(10) H(7) 3.226 ? . 4_444 C(11) H(1) 3.181 ? . 4_555 C(11) H(2) 3.217 ? . 4_555 C(11) H(4) 3.257 ? . 3_755 C(11) H(7) 3.363 ? . 3_756 C(11) H(10) 2.988 ? . 2_655 C(12) H(1) 3.274 ? . 2_645 C(12) H(3) 3.406 ? . 4_455 C(12) H(5) 3.391 ? . 2_645 C(12) H(6) 3.310 ? . 2_645 H(1) C(11) 3.181 ? . 4_454 H(1) C(12) 3.274 ? . 2_655 H(1) H(5) 2.716 ? . 4_454 H(1) H(6) 2.957 ? . 4_454 H(1) H(7) 2.821 ? . 2_655 H(1) H(7) 3.385 ? . 4_454 H(1) H(9) 2.643 ? . 2_655 H(1) H(10) 3.077 ? . 2_655 H(2) O(2) 2.357 ? . 1_565 H(2) N(2) 3.165 ? . 2_654 H(2) C(8) 3.563 ? . 2_654 H(2) C(10) 3.550 ? . 1_565 H(2) C(11) 3.217 ? . 4_454 H(2) H(5) 2.485 ? . 4_454 H(2) H(7) 3.482 ? . 2_655 H(2) H(7) 3.157 ? . 4_454 H(2) H(9) 2.881 ? . 2_655 H(2) H(12) 2.937 ? . 1_565 H(3) O(3) 3.523 ? . 1_565 H(3) O(4) 3.445 ? . 4_554 H(3) N(1) 3.408 ? . 2_654 H(3) N(2) 3.553 ? . 2_654 H(3) C(8) 3.296 ? . 2_654 H(3) C(9) 3.220 ? . 2_654 H(3) C(12) 3.406 ? . 4_554 H(3) H(8) 2.944 ? . 4_554 H(3) H(9) 3.109 ? . 4_554 H(3) H(12) 3.254 ? . 1_565 H(4) S(1) 2.863 ? . 3_755 H(4) O(2) 3.474 ? . 2_654 H(4) O(2) 3.383 ? . 3_755 H(4) C(9) 3.591 ? . 3_755 H(4) C(10) 3.459 ? . 2_654 H(4) C(10) 3.430 ? . 3_755 H(4) C(11) 3.257 ? . 3_755 H(4) H(5) 3.008 ? . 3_755 H(4) H(7) 3.317 ? . 3_755 H(4) H(12) 3.478 ? . 3_755 H(5) O(2) 3.337 ? . 4_545 H(5) N(2) 2.765 ? . 3_755 H(5) C(2) 3.070 ? . 4_555 H(5) C(3) 2.952 ? . 4_555 H(5) C(5) 3.580 ? . 3_755 H(5) C(6) 3.552 ? . 3_755 H(5) C(12) 3.391 ? . 2_655 H(5) H(1) 2.716 ? . 4_555 H(5) H(2) 2.485 ? . 4_555 H(5) H(4) 3.008 ? . 3_755 H(5) H(7) 3.561 ? . 3_756 H(5) H(8) 3.199 ? . 2_655 H(5) H(10) 2.747 ? . 2_655 H(6) O(1) 2.903 ? . 2_655 H(6) O(2) 2.799 ? . 2_655 H(6) C(10) 3.119 ? . 2_655 H(6) C(12) 3.310 ? . 2_655 H(6) H(1) 2.957 ? . 4_555 H(6) H(7) 3.194 ? . 3_756 H(6) H(8) 3.381 ? . 2_655 H(6) H(10) 2.673 ? . 2_655 H(7) O(1) 2.961 ? . 4_545 H(7) O(2) 3.581 ? . 2_655 H(7) O(2) 2.981 ? . 4_545 H(7) C(2) 3.537 ? . 2_645 H(7) C(10) 3.226 ? . 4_545 H(7) C(11) 3.363 ? . 3_756 H(7) H(1) 2.821 ? . 2_645 H(7) H(1) 3.385 ? . 4_555 H(7) H(2) 3.482 ? . 2_645 H(7) H(2) 3.157 ? . 4_555 H(7) H(4) 3.317 ? . 3_755 H(7) H(5) 3.561 ? . 3_756 H(7) H(6) 3.194 ? . 3_756 H(7) H(7) 2.835 ? . 3_756 H(8) O(3) 2.575 ? . 4_445 H(8) H(3) 2.944 ? . 4_455 H(8) H(5) 3.199 ? . 2_645 H(8) H(6) 3.381 ? . 2_645 H(8) H(12) 3.074 ? . 4_445 H(9) O(3) 2.997 ? . 4_445 H(9) C(1) 3.577 ? . 2_645 H(9) C(2) 2.744 ? . 2_645 H(9) C(3) 2.887 ? . 2_645 H(9) H(1) 2.643 ? . 2_645 H(9) H(2) 2.881 ? . 2_645 H(9) H(3) 3.109 ? . 4_455 H(9) H(12) 3.410 ? . 4_445 H(10) S(1) 3.332 ? . 2_645 H(10) O(3) 3.133 ? . 4_445 H(10) O(4) 2.624 ? . 2_645 H(10) C(2) 3.291 ? . 2_645 H(10) C(11) 2.988 ? . 2_645 H(10) H(1) 3.077 ? . 2_645 H(10) H(5) 2.747 ? . 2_645 H(10) H(6) 2.673 ? . 2_645 H(12) C(4) 3.33(2) ? . 3_755 H(12) C(5) 3.48(2) ? . 2_644 H(12) C(5) 3.24(2) ? . 3_755 H(12) C(6) 3.59(2) ? . 3_755 H(12) H(2) 2.937 ? . 1_545 H(12) H(3) 3.254 ? . 1_545 H(12) H(4) 3.478 ? . 3_755 H(12) H(8) 3.074 ? . 4_544 H(12) H(9) 3.410 ? . 4_544 _chemical_name_common zn-hqxc-dmso #============================================================================== # 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 #============================================================================== # Attachment 'hqxcH.cif' #============================================================================== data__hqxcH _database_code_depnum_ccdc_archive 'CCDC 746609' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C9 H6 N2 O3 ' _chemical_formula_moiety 'C9 H6 N2 O3 ' _chemical_formula_weight 190.16 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.4307(7) _cell_length_b 7.8217(7) _cell_length_c 15.6209(13) _cell_angle_alpha 93.707(3) _cell_angle_beta 102.937(3) _cell_angle_gamma 111.884(4) _cell_volume 810.00(12) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5104 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 293 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392.00 _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.988 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_ambient_temperature 293 _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 7870 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_theta_max 27.46 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3661 _reflns_number_gt 2126 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1616 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3661 _refine_ls_number_parameters 270 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0706P)^2^+0.1653P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.27 _refine_diff_density_min -0.27 _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) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 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) ; #============================================================================== # 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 O(1) O -0.0689(2) -0.0202(2) 0.09994(11) 0.0615(5) Uani 1.00 1 d . . . O(2) O -0.1316(3) -0.0027(2) 0.25439(12) 0.0675(5) Uani 1.00 1 d . . . O(3) O -0.0258(2) 0.2712(2) 0.33824(10) 0.0557(4) Uani 1.00 1 d . . . O(4) O 0.9189(2) 0.6529(2) 0.39297(11) 0.0552(4) Uani 1.00 1 d . . . O(5) O 0.7533(3) 0.5622(2) 0.22624(13) 0.0724(5) Uani 1.00 1 d . . . O(6) O 0.4961(3) 0.2913(2) 0.17496(12) 0.0733(5) Uani 1.00 1 d . . . N(1) N 0.0976(2) 0.2482(2) 0.05301(12) 0.0449(4) Uani 1.00 1 d . . . N(2) N 0.1162(2) 0.4515(2) 0.20751(11) 0.0454(4) Uani 1.00 1 d . . . N(3) N 0.7601(2) 0.4862(2) 0.48739(12) 0.0416(4) Uani 1.00 1 d . . . N(4) N 0.4578(2) 0.2480(2) 0.34396(12) 0.0442(4) Uani 1.00 1 d . . . C(1) C -0.0430(3) 0.1817(3) 0.26871(14) 0.0468(5) Uani 1.00 1 d . . . C(2) C 0.0348(3) 0.2705(2) 0.19506(13) 0.0416(4) Uani 1.00 1 d . . . C(3) C 0.0174(3) 0.1547(3) 0.11345(14) 0.0460(5) Uani 1.00 1 d . . . C(4) C 0.1898(3) 0.4400(2) 0.06441(14) 0.0432(4) Uani 1.00 1 d . . . C(5) C 0.2748(3) 0.5316(3) 0.00116(15) 0.0528(5) Uani 1.00 1 d . . . C(6) C 0.3632(4) 0.7225(3) 0.01686(19) 0.0664(7) Uani 1.00 1 d . . . C(7) C 0.3639(4) 0.8263(3) 0.09357(18) 0.0664(7) Uani 1.00 1 d . . . C(8) C 0.2795(3) 0.7365(3) 0.15562(16) 0.0568(6) Uani 1.00 1 d . . . C(9) C 0.1935(3) 0.5411(2) 0.14319(14) 0.0444(5) Uani 1.00 1 d . . . C(10) C 0.6144(3) 0.4070(3) 0.23730(16) 0.0521(5) Uani 1.00 1 d . . . C(11) C 0.6097(3) 0.3856(2) 0.33186(14) 0.0420(4) Uani 1.00 1 d . . . C(12) C 0.7753(3) 0.5188(2) 0.40526(14) 0.0420(4) Uani 1.00 1 d . . . C(13) C 0.6017(2) 0.3427(2) 0.50328(14) 0.0378(4) Uani 1.00 1 d . . . C(14) C 0.5915(3) 0.3151(3) 0.58955(15) 0.0457(5) Uani 1.00 1 d . . . C(15) C 0.4291(3) 0.1712(3) 0.60126(16) 0.0521(5) Uani 1.00 1 d . . . C(16) C 0.2754(3) 0.0510(3) 0.52868(18) 0.0542(5) Uani 1.00 1 d . . . C(17) C 0.2849(3) 0.0766(2) 0.44418(16) 0.0495(5) Uani 1.00 1 d . . . C(18) C 0.4482(3) 0.2235(2) 0.42967(14) 0.0408(4) Uani 1.00 1 d . . . H(1) H 0.2718 0.4646 -0.0509 0.063 Uiso 1.00 1 c R . . H(2) H 0.4244 0.7849 -0.0243 0.080 Uiso 1.00 1 c R . . H(3) H 0.4218 0.9561 0.1021 0.080 Uiso 1.00 1 c R . . H(4) H 0.2789 0.8052 0.2064 0.068 Uiso 1.00 1 c R . . H(5) H 0.6934 0.3933 0.6384 0.055 Uiso 1.00 1 c R . . H(6) H 0.4207 0.1529 0.6587 0.062 Uiso 1.00 1 c R . . H(7) H 0.1666 -0.0465 0.5382 0.065 Uiso 1.00 1 c R . . H(8) H 0.1827 -0.0037 0.3960 0.059 Uiso 1.00 1 c R . . H(9) H 0.088(3) 0.177(3) 0.0020(18) 0.066(7) Uiso 1.00 1 c . . . H(10) H 0.859(4) 0.565(4) 0.536(2) 0.078(8) Uiso 1.00 1 c . . . H(11) H -0.144(6) -0.053(5) 0.186(3) 0.148(15) Uiso 1.00 1 c . . . H(12) H 0.836(5) 0.628(4) 0.291(2) 0.113(12) Uiso 1.00 1 c . . . 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 O(1) 0.0858(12) 0.0390(8) 0.0482(9) 0.0096(8) 0.0266(8) -0.0063(7) O(2) 0.0935(13) 0.0454(9) 0.0499(10) 0.0086(8) 0.0279(9) 0.0016(7) O(3) 0.0705(10) 0.0557(9) 0.0394(8) 0.0230(8) 0.0179(7) -0.0002(7) O(4) 0.0464(8) 0.0500(9) 0.0576(9) 0.0063(7) 0.0160(7) 0.0017(7) O(5) 0.0749(12) 0.0780(12) 0.0540(11) 0.0154(10) 0.0233(9) 0.0113(9) O(6) 0.0841(12) 0.0779(12) 0.0430(9) 0.0245(10) 0.0063(9) -0.0049(9) N(1) 0.0545(10) 0.0414(9) 0.0334(8) 0.0141(8) 0.0127(8) -0.0022(7) N(2) 0.0546(10) 0.0412(9) 0.0363(9) 0.0171(8) 0.0095(7) 0.0008(7) N(3) 0.0376(8) 0.0390(8) 0.0412(9) 0.0116(7) 0.0057(7) -0.0022(7) N(4) 0.0444(9) 0.0389(9) 0.0433(9) 0.0157(7) 0.0044(7) -0.0023(7) C(1) 0.0541(12) 0.0444(11) 0.0376(11) 0.0161(9) 0.0116(9) 0.0007(9) C(2) 0.0493(11) 0.0385(10) 0.0322(9) 0.0136(9) 0.0105(8) -0.0001(8) C(3) 0.0542(12) 0.0421(11) 0.0369(10) 0.0150(9) 0.0125(9) -0.0019(9) C(4) 0.0465(11) 0.0424(10) 0.0371(10) 0.0162(9) 0.0074(8) 0.0054(8) C(5) 0.0591(13) 0.0563(13) 0.0421(12) 0.0202(11) 0.0162(10) 0.0090(10) C(6) 0.0711(16) 0.0611(15) 0.0611(15) 0.0170(13) 0.0200(13) 0.0203(12) C(7) 0.0777(17) 0.0460(12) 0.0624(16) 0.0134(12) 0.0128(13) 0.0112(12) C(8) 0.0730(15) 0.0427(11) 0.0476(13) 0.0188(11) 0.0109(11) 0.0033(10) C(9) 0.0508(11) 0.0403(10) 0.0371(10) 0.0155(9) 0.0076(9) 0.0029(8) C(10) 0.0545(13) 0.0570(13) 0.0456(12) 0.0252(11) 0.0115(10) 0.0020(11) C(11) 0.0417(10) 0.0404(10) 0.0414(11) 0.0172(9) 0.0073(8) -0.0014(8) C(12) 0.0373(10) 0.0388(10) 0.0471(11) 0.0142(9) 0.0100(9) -0.0016(8) C(13) 0.0365(9) 0.0321(9) 0.0450(11) 0.0146(7) 0.0107(8) 0.0023(8) C(14) 0.0461(11) 0.0448(11) 0.0454(11) 0.0196(9) 0.0096(9) 0.0023(9) C(15) 0.0583(13) 0.0528(12) 0.0525(13) 0.0262(11) 0.0208(11) 0.0127(10) C(16) 0.0470(12) 0.0460(12) 0.0688(16) 0.0166(10) 0.0169(11) 0.0105(11) C(17) 0.0426(11) 0.0367(10) 0.0592(14) 0.0110(9) 0.0050(10) 0.0000(9) C(18) 0.0407(10) 0.0342(9) 0.0438(11) 0.0149(8) 0.0058(8) -0.0006(8) #============================================================================== _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution SHELXS97 _computing_structure_refinement SHELXL _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 O(1) C(3) 1.255(2) yes . . O(2) C(1) 1.322(2) yes . . O(3) C(1) 1.208(2) yes . . O(4) C(12) 1.249(2) yes . . O(5) C(10) 1.320(3) yes . . O(6) C(10) 1.204(2) yes . . N(1) C(3) 1.341(3) yes . . N(1) C(4) 1.377(2) yes . . N(2) C(2) 1.297(2) yes . . N(2) C(9) 1.372(2) yes . . N(3) C(12) 1.345(2) yes . . N(3) C(13) 1.374(2) yes . . N(4) C(11) 1.298(2) yes . . N(4) C(18) 1.378(2) yes . . C(1) C(2) 1.497(3) yes . . C(2) C(3) 1.467(3) yes . . C(4) C(5) 1.387(3) yes . . C(4) C(9) 1.408(3) yes . . C(5) C(6) 1.368(3) yes . . C(6) C(7) 1.401(4) yes . . C(7) C(8) 1.363(3) yes . . C(8) C(9) 1.400(3) yes . . C(10) C(11) 1.504(3) yes . . C(11) C(12) 1.474(2) yes . . C(13) C(14) 1.393(3) yes . . C(13) C(18) 1.405(2) yes . . C(14) C(15) 1.368(3) yes . . C(15) C(16) 1.398(2) yes . . C(16) C(17) 1.361(3) yes . . C(17) C(18) 1.401(2) yes . . O(2) H(11) 1.08(4) no . . O(5) H(12) 1.04(3) no . . N(1) H(9) 0.91(2) no . . N(3) H(10) 0.93(2) no . . C(5) H(1) 0.930 no . . C(6) H(2) 0.930 no . . C(7) H(3) 0.930 no . . C(8) H(4) 0.930 no . . C(14) H(5) 0.930 no . . C(15) H(6) 0.930 no . . C(16) H(7) 0.930 no . . C(17) H(8) 0.930 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 C(3) N(1) C(4) 123.58(19) yes . . . C(2) N(2) C(9) 119.58(19) yes . . . C(12) N(3) C(13) 123.49(15) yes . . . C(11) N(4) C(18) 119.00(15) yes . . . O(2) C(1) O(3) 120.8(2) yes . . . O(2) C(1) C(2) 116.46(19) yes . . . O(3) C(1) C(2) 122.71(19) yes . . . N(2) C(2) C(1) 116.79(19) yes . . . N(2) C(2) C(3) 122.75(19) yes . . . C(1) C(2) C(3) 120.46(17) yes . . . O(1) C(3) N(1) 121.8(2) yes . . . O(1) C(3) C(2) 122.7(2) yes . . . N(1) C(3) C(2) 115.58(18) yes . . . N(1) C(4) C(5) 121.9(2) yes . . . N(1) C(4) C(9) 117.3(2) yes . . . C(5) C(4) C(9) 120.78(19) yes . . . C(4) C(5) C(6) 118.7(2) yes . . . C(5) C(6) C(7) 121.5(2) yes . . . C(6) C(7) C(8) 119.8(2) yes . . . C(7) C(8) C(9) 120.2(2) yes . . . N(2) C(9) C(4) 121.14(18) yes . . . N(2) C(9) C(8) 119.9(2) yes . . . C(4) C(9) C(8) 118.9(2) yes . . . O(5) C(10) O(6) 121.7(2) yes . . . O(5) C(10) C(11) 116.15(17) yes . . . O(6) C(10) C(11) 122.2(2) yes . . . N(4) C(11) C(10) 117.26(16) yes . . . N(4) C(11) C(12) 123.5(2) yes . . . C(10) C(11) C(12) 119.19(17) yes . . . O(4) C(12) N(3) 122.01(16) yes . . . O(4) C(12) C(11) 123.1(2) yes . . . N(3) C(12) C(11) 114.90(17) yes . . . N(3) C(13) C(14) 121.50(15) yes . . . N(3) C(13) C(18) 118.09(19) yes . . . C(14) C(13) C(18) 120.41(17) yes . . . C(13) C(14) C(15) 118.88(17) yes . . . C(14) C(15) C(16) 121.4(2) yes . . . C(15) C(16) C(17) 120.0(2) yes . . . C(16) C(17) C(18) 120.14(17) yes . . . N(4) C(18) C(13) 120.95(17) yes . . . N(4) C(18) C(17) 119.90(16) yes . . . C(13) C(18) C(17) 119.1(2) yes . . . C(1) O(2) H(11) 109(2) no . . . C(10) O(5) H(12) 104(2) no . . . C(3) N(1) H(9) 116.3(17) no . . . C(4) N(1) H(9) 120.1(17) no . . . C(12) N(3) H(10) 119.0(19) no . . . C(13) N(3) H(10) 117.5(19) no . . . C(4) C(5) H(1) 120.7 no . . . C(6) C(5) H(1) 120.7 no . . . C(5) C(6) H(2) 119.2 no . . . C(7) C(6) H(2) 119.2 no . . . C(6) C(7) H(3) 120.1 no . . . C(8) C(7) H(3) 120.1 no . . . C(7) C(8) H(4) 119.9 no . . . C(9) C(8) H(4) 119.9 no . . . C(13) C(14) H(5) 120.6 no . . . C(15) C(14) H(5) 120.6 no . . . C(14) C(15) H(6) 119.3 no . . . C(16) C(15) H(6) 119.3 no . . . C(15) C(16) H(7) 120.0 no . . . C(17) C(16) H(7) 120.0 no . . . C(16) C(17) H(8) 119.9 no . . . C(18) C(17) H(8) 119.9 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(3) N(1) C(4) C(5) 178.6(2) ? . . . . C(3) N(1) C(4) C(9) -1.8(3) ? . . . . C(4) N(1) C(3) O(1) 178.6(2) ? . . . . C(4) N(1) C(3) C(2) -0.5(3) ? . . . . C(2) N(2) C(9) C(4) -1.3(3) ? . . . . C(2) N(2) C(9) C(8) 179.2(2) ? . . . . C(9) N(2) C(2) C(1) 178.8(2) ? . . . . C(9) N(2) C(2) C(3) -1.2(3) ? . . . . C(12) N(3) C(13) C(14) -179.5(2) ? . . . . C(12) N(3) C(13) C(18) 0.3(3) ? . . . . C(13) N(3) C(12) O(4) 178.3(2) ? . . . . C(13) N(3) C(12) C(11) -1.2(3) ? . . . . C(11) N(4) C(18) C(13) -1.2(3) ? . . . . C(11) N(4) C(18) C(17) 179.6(2) ? . . . . C(18) N(4) C(11) C(10) 179.8(2) ? . . . . C(18) N(4) C(11) C(12) 0.2(3) ? . . . . O(2) C(1) C(2) N(2) 177.9(2) ? . . . . O(2) C(1) C(2) C(3) -2.1(3) ? . . . . O(3) C(1) C(2) N(2) -2.6(3) ? . . . . O(3) C(1) C(2) C(3) 177.4(2) ? . . . . N(2) C(2) C(3) O(1) -176.9(2) ? . . . . N(2) C(2) C(3) N(1) 2.1(3) ? . . . . C(1) C(2) C(3) O(1) 3.0(3) ? . . . . C(1) C(2) C(3) N(1) -177.9(2) ? . . . . N(1) C(4) C(5) C(6) 179.8(2) ? . . . . N(1) C(4) C(9) N(2) 2.8(3) ? . . . . N(1) C(4) C(9) C(8) -177.7(2) ? . . . . C(5) C(4) C(9) N(2) -177.6(2) ? . . . . C(5) C(4) C(9) C(8) 1.9(3) ? . . . . C(9) C(4) C(5) C(6) 0.2(3) ? . . . . C(4) C(5) C(6) C(7) -2.0(4) ? . . . . C(5) C(6) C(7) C(8) 1.7(4) ? . . . . C(6) C(7) C(8) C(9) 0.5(4) ? . . . . C(7) C(8) C(9) N(2) 177.3(2) ? . . . . C(7) C(8) C(9) C(4) -2.2(3) ? . . . . O(5) C(10) C(11) N(4) 170.4(2) ? . . . . O(5) C(10) C(11) C(12) -9.9(3) ? . . . . O(6) C(10) C(11) N(4) -8.2(4) ? . . . . O(6) C(10) C(11) C(12) 171.5(2) ? . . . . N(4) C(11) C(12) O(4) -178.6(2) ? . . . . N(4) C(11) C(12) N(3) 1.0(3) ? . . . . C(10) C(11) C(12) O(4) 1.8(3) ? . . . . C(10) C(11) C(12) N(3) -178.7(2) ? . . . . N(3) C(13) C(14) C(15) 179.3(2) ? . . . . N(3) C(13) C(18) N(4) 0.9(3) ? . . . . N(3) C(13) C(18) C(17) -179.8(2) ? . . . . C(14) C(13) C(18) N(4) -179.3(2) ? . . . . C(14) C(13) C(18) C(17) 0.0(3) ? . . . . C(18) C(13) C(14) C(15) -0.5(4) ? . . . . C(13) C(14) C(15) C(16) 0.7(4) ? . . . . C(14) C(15) C(16) C(17) -0.4(4) ? . . . . C(15) C(16) C(17) C(18) -0.1(3) ? . . . . C(16) C(17) C(18) N(4) 179.6(2) ? . . . . C(16) C(17) C(18) C(13) 0.3(4) ? . . . . 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 O(1) O(1) 3.495(2) ? . 2_555 O(1) N(1) 2.806(2) ? . 2_555 O(1) C(3) 3.575(3) ? . 2_555 O(2) O(5) 3.158(2) ? . 1_445 O(2) C(15) 3.486(3) ? . 2_556 O(3) O(4) 3.249(2) ? . 1_455 O(3) O(5) 3.599(3) ? . 1_455 O(3) N(3) 3.008(2) ? . 2_666 O(3) C(10) 3.348(3) ? . 1_455 O(3) C(11) 3.138(3) ? . 1_455 O(3) C(12) 3.097(3) ? . 1_455 O(3) C(14) 3.503(2) ? . 2_666 O(3) C(17) 3.409(3) ? . . O(4) O(3) 3.249(2) ? . 1_655 O(4) N(3) 3.250(2) ? . 2_766 O(4) C(13) 3.554(2) ? . 2_766 O(4) C(14) 3.499(3) ? . 2_766 O(4) C(15) 3.366(3) ? . 2_666 O(4) C(16) 3.419(2) ? . 1_665 O(4) C(16) 3.444(3) ? . 2_666 O(4) C(17) 3.314(2) ? . 1_665 O(5) O(2) 3.158(2) ? . 1_665 O(5) O(3) 3.599(3) ? . 1_655 O(5) N(2) 3.189(3) ? . 1_655 O(5) C(5) 3.524(3) ? . 2_665 O(6) N(1) 3.026(2) ? . . O(6) C(2) 3.457(3) ? . . O(6) C(3) 3.197(3) ? . . O(6) C(4) 3.161(3) ? . . O(6) C(6) 3.395(3) ? . 2_665 O(6) C(7) 3.462(3) ? . 1_545 O(6) C(9) 3.468(3) ? . . N(1) O(1) 2.806(2) ? . 2_555 N(1) O(6) 3.026(2) ? . . N(1) C(6) 3.452(3) ? . 2_565 N(1) C(7) 3.488(3) ? . 2_565 N(2) O(5) 3.189(3) ? . 1_455 N(2) C(14) 3.363(2) ? . 2_666 N(3) O(3) 3.008(2) ? . 2_666 N(3) O(4) 3.250(2) ? . 2_766 N(3) N(3) 3.420(2) ? . 2_766 N(3) C(12) 3.499(2) ? . 2_766 N(3) C(13) 3.446(3) ? . 2_666 N(3) C(14) 3.542(3) ? . 2_666 N(3) C(18) 3.518(3) ? . 2_666 N(4) C(1) 3.467(3) ? . . N(4) C(2) 3.537(2) ? . . C(1) N(4) 3.467(3) ? . . C(1) C(10) 3.567(4) ? . 1_455 C(1) C(17) 3.594(3) ? . . C(2) O(6) 3.457(3) ? . . C(2) N(4) 3.537(2) ? . . C(3) O(1) 3.575(3) ? . 2_555 C(3) O(6) 3.197(3) ? . . C(3) C(6) 3.573(4) ? . 2_565 C(4) O(6) 3.161(3) ? . . C(4) C(4) 3.544(3) ? . 2_565 C(4) C(5) 3.469(3) ? . 2_565 C(5) O(5) 3.524(3) ? . 2_665 C(5) C(4) 3.469(3) ? . 2_565 C(5) C(5) 3.568(4) ? . 2_665 C(5) C(9) 3.516(3) ? . 2_565 C(6) O(6) 3.395(3) ? . 2_665 C(6) N(1) 3.452(3) ? . 2_565 C(6) C(3) 3.573(4) ? . 2_565 C(7) O(6) 3.462(3) ? . 1_565 C(7) N(1) 3.488(3) ? . 2_565 C(9) O(6) 3.468(3) ? . . C(9) C(5) 3.516(3) ? . 2_565 C(10) O(3) 3.348(3) ? . 1_655 C(10) C(1) 3.567(4) ? . 1_655 C(11) O(3) 3.138(3) ? . 1_655 C(11) C(14) 3.504(3) ? . 2_666 C(12) O(3) 3.097(3) ? . 1_655 C(12) N(3) 3.499(2) ? . 2_766 C(12) C(14) 3.442(3) ? . 2_666 C(12) C(15) 3.303(3) ? . 2_666 C(13) O(4) 3.554(2) ? . 2_766 C(13) N(3) 3.446(3) ? . 2_666 C(13) C(13) 3.329(3) ? . 2_666 C(13) C(16) 3.559(3) ? . 2_656 C(14) O(3) 3.503(2) ? . 2_666 C(14) O(4) 3.499(3) ? . 2_766 C(14) N(2) 3.363(2) ? . 2_666 C(14) N(3) 3.542(3) ? . 2_666 C(14) C(11) 3.504(3) ? . 2_666 C(14) C(12) 3.442(3) ? . 2_666 C(14) C(17) 3.552(3) ? . 2_656 C(15) O(2) 3.486(3) ? . 2_556 C(15) O(4) 3.366(3) ? . 2_666 C(15) C(12) 3.303(3) ? . 2_666 C(15) C(17) 3.513(4) ? . 2_656 C(15) C(18) 3.563(3) ? . 2_656 C(16) O(4) 3.419(2) ? . 1_445 C(16) O(4) 3.444(3) ? . 2_666 C(16) C(13) 3.559(3) ? . 2_656 C(16) C(18) 3.481(3) ? . 2_656 C(17) O(3) 3.409(3) ? . . C(17) O(4) 3.314(2) ? . 1_445 C(17) C(1) 3.594(3) ? . . C(17) C(14) 3.552(3) ? . 2_656 C(17) C(15) 3.513(4) ? . 2_656 C(18) N(3) 3.518(3) ? . 2_666 C(18) C(15) 3.563(3) ? . 2_656 C(18) C(16) 3.481(3) ? . 2_656 O(1) H(1) 3.190 ? . 2_555 O(1) H(2) 3.512 ? . 1_445 O(1) H(4) 3.509 ? . 1_545 O(1) H(9) 1.89(2) ? . 2_555 O(2) H(3) 3.513 ? . 1_445 O(2) H(6) 2.732 ? . 2_556 O(2) H(7) 3.318 ? . 2_556 O(2) H(8) 2.837 ? . . O(2) H(12) 2.91(4) ? . 1_445 O(3) H(5) 2.786 ? . 2_666 O(3) H(6) 3.527 ? . 2_556 O(3) H(7) 2.808 ? . 2_556 O(3) H(8) 3.154 ? . . O(3) H(10) 2.10(2) ? . 2_666 O(3) H(12) 3.38(4) ? . 1_455 O(4) H(5) 3.171 ? . 2_766 O(4) H(6) 3.381 ? . 2_666 O(4) H(7) 2.877 ? . 1_665 O(4) H(7) 3.518 ? . 2_666 O(4) H(8) 2.660 ? . 1_665 O(4) H(10) 2.89(3) ? . 2_766 O(5) H(1) 2.692 ? . 2_665 O(5) H(6) 3.541 ? . 2_666 O(5) H(11) 2.96(4) ? . 1_665 O(6) H(1) 3.146 ? . 2_665 O(6) H(2) 2.635 ? . 2_665 O(6) H(3) 2.593 ? . 1_545 O(6) H(9) 3.36(2) ? . . N(1) H(9) 3.07(2) ? . 2_555 N(2) H(5) 2.467 ? . 2_666 N(2) H(12) 3.32(4) ? . 1_455 N(3) H(10) 3.10(3) ? . 2_766 N(4) H(4) 3.565 ? . 1_545 N(4) H(5) 3.405 ? . 2_666 N(4) H(6) 3.572 ? . 2_656 C(1) H(5) 3.340 ? . 2_666 C(1) H(6) 3.513 ? . 2_556 C(1) H(7) 3.463 ? . 2_556 C(1) H(8) 3.092 ? . . C(1) H(10) 3.23(2) ? . 2_666 C(2) H(5) 3.251 ? . 2_666 C(3) H(2) 3.483 ? . 2_565 C(3) H(9) 2.80(2) ? . 2_555 C(5) H(1) 3.272 ? . 2_665 C(6) H(1) 3.492 ? . 2_665 C(6) H(2) 3.560 ? . 2_675 C(6) H(3) 3.357 ? . 2_675 C(7) H(2) 3.243 ? . 2_675 C(7) H(9) 3.35(2) ? . 2_565 C(7) H(11) 3.36(4) ? . 1_665 C(8) H(5) 3.422 ? . 2_666 C(8) H(6) 3.077 ? . 2_666 C(8) H(9) 3.54(2) ? . 2_565 C(9) H(1) 3.418 ? . 2_565 C(9) H(5) 3.283 ? . 2_666 C(10) H(1) 3.324 ? . 2_665 C(10) H(2) 3.465 ? . 2_665 C(10) H(3) 3.587 ? . 1_545 C(11) H(5) 3.398 ? . 2_666 C(12) H(6) 3.491 ? . 2_666 C(12) H(10) 2.99(3) ? . 2_766 C(13) H(7) 3.468 ? . 2_656 C(14) H(4) 3.416 ? . 2_666 C(14) H(8) 3.428 ? . 2_656 C(15) H(4) 3.238 ? . 2_666 C(15) H(8) 3.579 ? . 2_656 C(15) H(12) 3.56(4) ? . 2_666 C(16) H(7) 3.202 ? . 2_556 C(17) H(7) 3.350 ? . 2_556 C(17) H(10) 3.37(3) ? . 2_666 C(18) H(7) 3.572 ? . 2_656 C(18) H(10) 3.39(3) ? . 2_666 H(1) O(1) 3.190 ? . 2_555 H(1) O(5) 2.692 ? . 2_665 H(1) O(6) 3.146 ? . 2_665 H(1) C(5) 3.272 ? . 2_665 H(1) C(6) 3.492 ? . 2_665 H(1) C(9) 3.418 ? . 2_565 H(1) C(10) 3.324 ? . 2_665 H(1) H(1) 3.227 ? . 2_665 H(1) H(2) 3.561 ? . 2_665 H(1) H(11) 3.417 ? . 2_555 H(2) O(1) 3.512 ? . 1_665 H(2) O(6) 2.635 ? . 2_665 H(2) C(3) 3.483 ? . 2_565 H(2) C(6) 3.560 ? . 2_675 H(2) C(7) 3.243 ? . 2_675 H(2) C(10) 3.465 ? . 2_665 H(2) H(1) 3.561 ? . 2_665 H(2) H(2) 3.104 ? . 2_675 H(2) H(3) 2.470 ? . 2_675 H(2) H(9) 3.456 ? . 2_665 H(3) O(2) 3.513 ? . 1_665 H(3) O(6) 2.593 ? . 1_565 H(3) C(6) 3.357 ? . 2_675 H(3) C(10) 3.587 ? . 1_565 H(3) H(2) 2.470 ? . 2_675 H(3) H(9) 3.490 ? . 2_565 H(3) H(11) 3.233 ? . 1_665 H(4) O(1) 3.509 ? . 1_565 H(4) N(4) 3.565 ? . 1_565 H(4) C(14) 3.416 ? . 2_666 H(4) C(15) 3.238 ? . 2_666 H(4) H(5) 2.973 ? . 2_666 H(4) H(6) 2.606 ? . 2_666 H(4) H(8) 3.563 ? . 1_565 H(5) O(3) 2.786 ? . 2_666 H(5) O(4) 3.171 ? . 2_766 H(5) N(2) 2.467 ? . 2_666 H(5) N(4) 3.405 ? . 2_666 H(5) C(1) 3.340 ? . 2_666 H(5) C(2) 3.251 ? . 2_666 H(5) C(8) 3.422 ? . 2_666 H(5) C(9) 3.283 ? . 2_666 H(5) C(11) 3.398 ? . 2_666 H(5) H(4) 2.973 ? . 2_666 H(5) H(8) 3.539 ? . 2_656 H(5) H(12) 3.491 ? . 2_766 H(6) O(2) 2.732 ? . 2_556 H(6) O(3) 3.527 ? . 2_556 H(6) O(4) 3.381 ? . 2_666 H(6) O(5) 3.541 ? . 2_666 H(6) N(4) 3.572 ? . 2_656 H(6) C(1) 3.513 ? . 2_556 H(6) C(8) 3.077 ? . 2_666 H(6) C(12) 3.491 ? . 2_666 H(6) H(4) 2.606 ? . 2_666 H(6) H(11) 3.460 ? . 2_556 H(6) H(12) 3.188 ? . 2_666 H(7) O(2) 3.318 ? . 2_556 H(7) O(3) 2.808 ? . 2_556 H(7) O(4) 2.877 ? . 1_445 H(7) O(4) 3.518 ? . 2_666 H(7) C(1) 3.463 ? . 2_556 H(7) C(13) 3.468 ? . 2_656 H(7) C(16) 3.202 ? . 2_556 H(7) C(17) 3.350 ? . 2_556 H(7) C(18) 3.572 ? . 2_656 H(7) H(7) 2.866 ? . 2_556 H(7) H(8) 3.139 ? . 2_556 H(7) H(10) 3.037 ? . 1_445 H(8) O(2) 2.837 ? . . H(8) O(3) 3.154 ? . . H(8) O(4) 2.660 ? . 1_445 H(8) C(1) 3.092 ? . . H(8) C(14) 3.428 ? . 2_656 H(8) C(15) 3.579 ? . 2_656 H(8) H(4) 3.563 ? . 1_545 H(8) H(5) 3.539 ? . 2_656 H(8) H(7) 3.139 ? . 2_556 H(8) H(11) 3.510 ? . . H(8) H(12) 3.099 ? . 1_445 H(9) O(1) 1.89(3) ? . 2_555 H(9) O(6) 3.36(2) ? . . H(9) N(1) 3.07(2) ? . 2_555 H(9) C(3) 2.80(2) ? . 2_555 H(9) C(7) 3.35(2) ? . 2_565 H(9) C(8) 3.54(2) ? . 2_565 H(9) H(2) 3.456 ? . 2_665 H(9) H(3) 3.490 ? . 2_565 H(9) H(9) 2.58(3) ? . 2_555 H(9) H(11) 3.20(5) ? . 2_555 H(10) O(3) 2.10(2) ? . 2_666 H(10) O(4) 2.89(3) ? . 2_766 H(10) N(3) 3.10(3) ? . 2_766 H(10) C(1) 3.23(2) ? . 2_666 H(10) C(12) 2.99(3) ? . 2_766 H(10) C(17) 3.37(3) ? . 2_666 H(10) C(18) 3.39(3) ? . 2_666 H(10) H(7) 3.037 ? . 1_665 H(10) H(10) 3.03(5) ? . 2_766 H(11) O(5) 2.96(4) ? . 1_445 H(11) C(7) 3.36(4) ? . 1_445 H(11) H(1) 3.417 ? . 2_555 H(11) H(3) 3.233 ? . 1_445 H(11) H(6) 3.460 ? . 2_556 H(11) H(8) 3.510 ? . . H(11) H(9) 3.20(5) ? . 2_555 H(11) H(12) 3.04(6) ? . 1_445 H(12) O(2) 2.91(4) ? . 1_665 H(12) O(3) 3.38(4) ? . 1_655 H(12) N(2) 3.32(4) ? . 1_655 H(12) C(15) 3.56(4) ? . 2_666 H(12) H(5) 3.491 ? . 2_766 H(12) H(6) 3.188 ? . 2_666 H(12) H(8) 3.099 ? . 1_665 H(12) H(11) 3.04(6) ? . 1_665 #============================================================================== # 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 #============================================================================== _chemical_name_common zn-hqxc-dmso