# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 #TrackingRef '- naproxen_ni_cu_zn_cd_cd_r3.cif' #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Wang, Yong-Tao Department of Chemical Engineering Shandong Provincial Key Laboratory of Chemical Fines Shandong Polytechnic University Jinan, 250353 P. R. China ; _publ_contact_author_phone 86-531-89000551 _publ_contact_author_fax '86 531 89000551' _publ_contact_author_email ceswyt@yahoo.com.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 Crystal Growth & Design. Yong-Tao Wang March 1, 2012 ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; New homochiral ferroelectric supramolecular networks of complexes constructed by chiral S-Naproxen ligand ; loop_ _publ_author_name _publ_author_address 'Yong-Tao Wang' ; Department of Chemical Engineering Shandong Provincial Key Laboratory of Chemical Fines Shandong Polytechnic University Jinan, 250353 P. R. China ; 'Gui-Mei Tang' ; Department of Chemical Engineering Shandong Provincial Key Laboratory of Chemical Fines Shandong Polytechnic University Jinan, 250353 P. R. China ; 'Wen-Zhu Wan' ; Department of Chemical Engineering Shandong Provincial Key Laboratory of Chemical Fines Shandong Polytechnic University Jinan, 250353 P. R. China ; 'Yue Wu' ; Department of Chemical Engineering Shandong Provincial Key Laboratory of Chemical Fines Shandong Polytechnic University Jinan, 250353 P. R. China ; 'Ting-Cui Tian' ; Department of Chemical Engineering Shandong Provincial Key Laboratory of Chemical Fines Shandong Polytechnic University Jinan, 250353 P. R. China ; ; Jin-Hua Wang ; ; Department of Chemical Engineering Shandong Provincial Key Laboratory of Chemical Fines Shandong Polytechnic University Jinan, 250353 P. R. China ; 'Chao He' ; Fujian Institute of Research on the Structure of Matter Chinese Academy of Science Fuzhou, 350002 P. R. China ; 'Xi-Fa Long' ; Fujian Institute of Research on the Structure of Matter Chinese Academy of Science Fuzhou, 350002 P. R. China ; 'Jun-Jie Wang' ; Department of Chemistry & Chemical Engineering Anyang Normal University Anyang, 455002 P. R. China ; 'Seik Weng Ng' ; Department of Chemistry Univeristy of Malaya Kuala Lumpur, 50603 Malaysia ; _publ_contact_author_name 'Wang, Yong-Tao' #=======================================END data_compound_2 #TrackingRef '- naproxen_ni_cu_zn_cd_cd_r3.cif' _database_code_depnum_ccdc_archive 'CCDC 669852' _audit_creation_method SHELXL-97 _chemical_absolute_configuration rm _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H32 Cu O9, H2 O' _chemical_formula_sum 'C28 H34 Cu O10' _chemical_formula_weight 594.10 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 38.6025(14) _cell_length_b 5.7352(2) _cell_length_c 6.3225(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.318(2) _cell_angle_gamma 90.00 _cell_volume 1395.79(10) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5819 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 27.83 _exptl_crystal_description platelet _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 622 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details SADABS(Sheldrick,1996) _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12279 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 28.22 _reflns_number_total 3441 _reflns_number_gt 3143 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0798P)^2^+1.0592P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.058(18) _refine_ls_number_reflns 3441 _refine_ls_number_parameters 162 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _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 Cu1 Cu 0.5000 0.49729(6) 0.5000 0.04354(17) Uani 1 2 d S . . O1 O 0.53984(5) 0.4945(7) 0.3251(4) 0.0510(5) Uani 1 1 d . A . O2 O 0.55456(8) 0.8660(5) 0.3975(6) 0.0659(8) Uani 1 1 d . A . O3 O 0.72338(7) 0.4668(5) 1.2776(4) 0.0503(6) Uani 1 1 d . . . O1W O 0.49338(13) 0.0986(9) 0.4036(8) 0.0467(10) Uani 0.50 1 d PU A -1 H1WA H 0.5037 -0.0062 0.4797 0.056 Uiso 0.50 1 d PR A -1 H1WB H 0.4807 0.0607 0.2932 0.056 Uiso 0.50 1 d PR A -1 O2W O 0.53065(10) 0.5427(16) 0.7626(6) 0.125(2) Uani 1 1 d U A . H2WA H 0.5398 0.4259 0.8282 0.150 Uiso 1 1 d R . . H2WB H 0.5346 0.6797 0.8098 0.150 Uiso 1 1 d R . . O3W O 0.5044(4) 1.0437(18) 0.0451(13) 0.106(3) Uani 0.50 1 d PU B -1 H3WA H 0.5181 1.0113 -0.0500 0.127 Uiso 0.50 1 d PR B -1 H3WB H 0.5125 1.0767 0.1703 0.127 Uiso 0.50 1 d PR B -1 C1 C 0.56038(8) 0.6693(6) 0.3270(5) 0.0391(6) Uani 1 1 d . . . C2 C 0.59612(8) 0.6176(6) 0.2446(5) 0.0357(6) Uani 1 1 d . A . H2 H 0.5936 0.4823 0.1501 0.043 Uiso 1 1 calc R . . C3 C 0.60890(9) 0.8208(7) 0.1175(6) 0.0462(7) Uani 1 1 d . . . H3A H 0.5925 0.8518 -0.0008 0.069 Uiso 1 1 calc R A . H3B H 0.6310 0.7824 0.0668 0.069 Uiso 1 1 calc R . . H3C H 0.6113 0.9565 0.2063 0.069 Uiso 1 1 calc R . . C4 C 0.64728(4) 0.6884(2) 0.5249(2) 0.0354(6) Uani 1 1 d G A . H4 H 0.6526 0.8252 0.4553 0.042 Uiso 1 1 calc R . . C5 C 0.62045(4) 0.5464(3) 0.4416(2) 0.0345(6) Uani 1 1 d G . . C6 C 0.61248(4) 0.3419(3) 0.5456(3) 0.0393(7) Uani 1 1 d G A . H6 H 0.5945 0.2469 0.4898 0.047 Uiso 1 1 calc R . . C7 C 0.63135(4) 0.2796(2) 0.7330(3) 0.0406(7) Uani 1 1 d G . . H7 H 0.6260 0.1428 0.8026 0.049 Uiso 1 1 calc R A . C8 C 0.65817(3) 0.4216(2) 0.81636(19) 0.0347(6) Uani 1 1 d G A . C9 C 0.66614(3) 0.62606(19) 0.71235(19) 0.0351(6) Uani 1 1 d G . . C10 C 0.69297(4) 0.7681(3) 0.7957(3) 0.0438(7) Uani 1 1 d G A . H10 H 0.6983 0.9049 0.7261 0.053 Uiso 1 1 calc R . . C11 C 0.71183(4) 0.7058(3) 0.9831(3) 0.0456(7) Uani 1 1 d G . . H11 H 0.7298 0.8008 1.0389 0.055 Uiso 1 1 calc R A . C12 C 0.70387(4) 0.5013(3) 1.0871(2) 0.0411(6) Uani 1 1 d G A . C13 C 0.67704(4) 0.3593(3) 1.0038(2) 0.0411(7) Uani 1 1 d G . . H13 H 0.6717 0.2225 1.0734 0.049 Uiso 1 1 calc R A . C14 C 0.71645(12) 0.2647(8) 1.3964(6) 0.0563(9) Uani 1 1 d . . . H14A H 0.7316 0.2613 1.5237 0.084 Uiso 1 1 calc R . . H14B H 0.7203 0.1283 1.3133 0.084 Uiso 1 1 calc R . . H14C H 0.6927 0.2677 1.4326 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0295(2) 0.0401(3) 0.0612(3) 0.000 0.00476(19) 0.000 O1 0.0364(10) 0.0517(12) 0.0658(13) 0.0007(17) 0.0104(9) -0.0113(16) O2 0.0457(15) 0.0475(15) 0.108(2) -0.0030(15) 0.0274(15) 0.0031(12) O3 0.0494(12) 0.0542(17) 0.0456(11) 0.0034(12) -0.0063(9) 0.0013(13) O1W 0.046(2) 0.038(2) 0.057(2) 0.010(2) 0.010(2) 0.0013(19) O2W 0.061(2) 0.222(7) 0.092(2) 0.026(4) 0.0003(17) -0.022(4) O3W 0.133(7) 0.115(7) 0.069(6) 0.002(4) -0.003(6) 0.005(6) C1 0.0319(14) 0.0402(15) 0.0452(16) 0.0055(12) 0.0034(12) 0.0017(12) C2 0.0335(14) 0.0380(15) 0.0361(14) 0.0021(12) 0.0061(11) -0.0025(12) C3 0.0426(17) 0.0496(18) 0.0473(17) 0.0102(14) 0.0096(14) -0.0029(15) C4 0.0368(15) 0.0291(13) 0.0416(14) 0.0023(11) 0.0113(12) -0.0038(11) C5 0.0333(13) 0.0314(16) 0.0397(13) -0.0016(10) 0.0086(10) 0.0036(10) C6 0.0372(15) 0.0303(13) 0.0507(17) -0.0045(13) 0.0049(13) -0.0055(11) C7 0.0436(17) 0.0294(13) 0.0489(17) 0.0074(12) 0.0049(13) -0.0057(12) C8 0.0385(15) 0.0272(11) 0.0396(14) -0.0024(10) 0.0109(12) -0.0001(10) C9 0.0360(14) 0.0306(13) 0.0398(14) 0.0004(11) 0.0092(11) -0.0026(11) C10 0.0448(17) 0.0370(15) 0.0502(17) 0.0036(13) 0.0083(14) -0.0090(13) C11 0.0387(16) 0.0456(17) 0.0522(18) -0.0021(14) 0.0020(14) -0.0071(14) C12 0.0363(12) 0.0431(13) 0.0445(13) -0.0066(18) 0.0054(10) 0.003(2) C13 0.0428(16) 0.0345(15) 0.0467(16) 0.0038(12) 0.0071(13) 0.0008(12) C14 0.062(2) 0.062(2) 0.0446(18) 0.0053(16) -0.0015(17) 0.0111(19) _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 Cu1 O1 1.961(2) . ? Cu1 O1 1.961(2) 2_656 ? Cu1 O2W 1.982(4) . ? Cu1 O2W 1.982(4) 2_656 ? Cu1 O1W 2.375(5) . ? Cu1 O1W 2.375(5) 2_656 ? O1 C1 1.278(5) . ? O2 C1 1.240(5) . ? O3 C12 1.386(2) . ? O3 C14 1.417(5) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8501 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8499 . ? C1 C2 1.540(4) . ? C2 C3 1.518(4) . ? C2 C5 1.557(3) . ? C2 H2 0.9800 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.3900 . ? C4 C9 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C10 H10 0.9300 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O1 179.1(2) . 2_656 ? O1 Cu1 O2W 91.69(14) . . ? O1 Cu1 O2W 88.43(14) 2_656 . ? O1 Cu1 O2W 88.43(14) . 2_656 ? O1 Cu1 O2W 91.69(14) 2_656 2_656 ? O2W Cu1 O2W 164.9(5) . 2_656 ? O1 Cu1 O1W 85.48(16) . . ? O1 Cu1 O1W 93.62(16) 2_656 . ? O2W Cu1 O1W 112.8(3) . . ? O2W Cu1 O1W 82.3(3) 2_656 . ? O1 Cu1 O1W 93.62(16) . 2_656 ? O1 Cu1 O1W 85.48(16) 2_656 2_656 ? O2W Cu1 O1W 82.3(3) . 2_656 ? O2W Cu1 O1W 112.8(3) 2_656 2_656 ? O1W Cu1 O1W 31.4(2) . 2_656 ? C1 O1 Cu1 120.1(3) . . ? C12 O3 C14 117.8(3) . . ? Cu1 O1W H1WA 119.9 . . ? Cu1 O1W H1WB 120.1 . . ? H1WA O1W H1WB 120.0 . . ? Cu1 O2W H2WA 120.3 . . ? Cu1 O2W H2WB 119.7 . . ? H2WA O2W H2WB 120.0 . . ? H3WA O3W H3WB 120.3 . . ? O2 C1 O1 126.0(3) . . ? O2 C1 C2 119.2(3) . . ? O1 C1 C2 114.7(3) . . ? C3 C2 C1 111.5(3) . . ? C3 C2 C5 115.1(2) . . ? C1 C2 C5 106.4(2) . . ? C3 C2 H2 107.9 . . ? C1 C2 H2 107.9 . . ? C5 C2 H2 107.9 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 120.0 . . ? C5 C4 H4 120.0 . . ? C9 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 C2 117.28(14) . . ? C4 C5 C2 122.47(14) . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 C13 120.0 . . ? C9 C8 C13 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 C4 120.0 . . ? C8 C9 C4 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? O3 C12 C11 114.00(16) . . ? O3 C12 C13 125.91(16) . . ? C11 C12 C13 120.0 . . ? C12 C13 C8 120.0 . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.22 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.632 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.075 #=======================================END data_compound_3 #TrackingRef '- naproxen_ni_cu_zn_cd_cd_r3.cif' _database_code_depnum_ccdc_archive 'CCDC 669853' _audit_creation_method SHELXL-97 _chemical_absolute_configuration rm _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H30 O8 Zn, H2 O' _chemical_formula_sum 'C28 H32 O9 Zn' _chemical_formula_weight 577.93 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' 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 Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 29.5909(5) _cell_length_b 7.4519(2) _cell_length_c 6.2317(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.979(2) _cell_angle_gamma 90.00 _cell_volume 1373.94(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1640 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 24.75 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.719 _exptl_absorpt_correction_T_max 0.954 _exptl_absorpt_process_details SADABS(Sheldrick,1996) _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3592 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 27.57 _reflns_number_total 2407 _reflns_number_gt 2137 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(16) _refine_ls_number_reflns 2407 _refine_ls_number_parameters 173 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.5000 -0.31423(5) 1.0000 0.04226(19) Uani 1 2 d S . . C1 C 0.76317(11) -0.0385(5) 0.9305(5) 0.0400(8) Uani 1 1 d . . . H1A H 0.7667 0.0115 1.0665 0.048 Uiso 1 1 calc R . . C2 C 0.80020(12) -0.0924(5) 0.8184(6) 0.0409(8) Uani 1 1 d . . . C3 C 0.79458(13) -0.1710(6) 0.6128(6) 0.0464(9) Uani 1 1 d . . . H3A H 0.8198 -0.2096 0.5388 0.056 Uiso 1 1 calc R . . C4 C 0.75297(13) -0.1906(6) 0.5227(6) 0.0448(9) Uani 1 1 d . . . H4A H 0.7500 -0.2419 0.3871 0.054 Uiso 1 1 calc R . . C5 C 0.71397(12) -0.1348(5) 0.6307(5) 0.0382(8) Uani 1 1 d . . . C6 C 0.66967(12) -0.1484(5) 0.5389(6) 0.0409(8) Uani 1 1 d . . . H6A H 0.6660 -0.1996 0.4036 0.049 Uiso 1 1 calc R . . C7 C 0.63249(12) -0.0885(6) 0.6438(6) 0.0422(8) Uani 1 1 d . . . C8 C 0.63817(13) -0.0182(6) 0.8509(6) 0.0463(10) Uani 1 1 d . . . H8A H 0.6129 0.0193 0.9255 0.056 Uiso 1 1 calc R . . C9 C 0.68006(12) -0.0034(6) 0.9463(6) 0.0424(9) Uani 1 1 d . . . H9A H 0.6827 0.0440 1.0839 0.051 Uiso 1 1 calc R . . C10 C 0.71944(11) -0.0593(5) 0.8380(5) 0.0359(7) Uani 1 1 d . . . C11 C 0.85077(14) -0.0216(9) 1.1042(7) 0.0666(15) Uani 1 1 d . . . H11A H 0.8826 -0.0172 1.1370 0.100 Uiso 1 1 calc R . . H11B H 0.8364 -0.1043 1.1995 0.100 Uiso 1 1 calc R . . H11C H 0.8379 0.0956 1.1215 0.100 Uiso 1 1 calc R . . C12 C 0.58576(13) -0.0953(7) 0.5385(6) 0.0505(10) Uani 1 1 d . . . H12A H 0.5889 -0.1543 0.3989 0.061 Uiso 1 1 calc R . . C13 C 0.56768(15) 0.0953(8) 0.4961(9) 0.0771(17) Uani 1 1 d . . . H13A H 0.5888 0.1602 0.4103 0.116 Uiso 1 1 calc R . . H13B H 0.5639 0.1563 0.6303 0.116 Uiso 1 1 calc R . . H13C H 0.5391 0.0882 0.4214 0.116 Uiso 1 1 calc R . . C14 C 0.55500(14) -0.2121(7) 0.6731(7) 0.0408(11) Uani 1 1 d . . . O1 O 0.53388(9) -0.1373(4) 0.8249(4) 0.0536(7) Uani 1 1 d . . . O1W O 0.45854(10) -0.4760(5) 0.8251(5) 0.0673(9) Uani 1 1 d . . . H1WA H 0.4452 -0.5480 0.9088 0.101 Uiso 1 1 d R . . H1WB H 0.4390 -0.4120 0.7591 0.101 Uiso 1 1 d R . . O2 O 0.55239(11) -0.3729(5) 0.6368(5) 0.0514(9) Uani 1 1 d . . . O2W O 0.5000 0.1832(10) 1.0000 0.0718(11) Uani 1 2 d S . . H2WA H 0.4822 0.2450 0.9213 0.108 Uiso 0.50 1 d PR . . H2WB H 0.4868 0.0865 1.0354 0.108 Uiso 0.50 1 d PR . . O3 O 0.84407(8) -0.0792(5) 0.8898(4) 0.0534(7) Uani 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 0.0473(3) 0.0326(3) 0.0469(3) 0.000 0.0039(2) 0.000 C1 0.048(2) 0.038(2) 0.0349(17) -0.0009(15) 0.0041(14) -0.0029(16) C2 0.0411(18) 0.037(2) 0.0451(19) 0.0030(16) 0.0041(14) 0.0003(16) C3 0.048(2) 0.049(3) 0.042(2) 0.0036(18) 0.0106(16) 0.0089(18) C4 0.055(2) 0.046(2) 0.0337(18) -0.0029(17) 0.0080(16) 0.0046(18) C5 0.0469(19) 0.0315(19) 0.0364(17) 0.0042(15) 0.0027(14) -0.0037(16) C6 0.052(2) 0.040(2) 0.0306(16) -0.0005(16) 0.0030(14) -0.0039(17) C7 0.0463(19) 0.040(2) 0.0406(18) 0.0038(17) 0.0015(15) -0.0066(17) C8 0.043(2) 0.053(3) 0.043(2) -0.0059(19) 0.0084(15) -0.0029(19) C9 0.050(2) 0.044(2) 0.0342(18) -0.0074(16) 0.0060(15) -0.0030(17) C10 0.0428(18) 0.0305(19) 0.0345(17) 0.0008(14) 0.0052(13) -0.0035(15) C11 0.044(2) 0.092(5) 0.063(3) -0.005(3) -0.006(2) -0.012(3) C12 0.047(2) 0.063(3) 0.042(2) 0.0075(19) -0.0025(16) -0.009(2) C13 0.055(3) 0.086(4) 0.090(4) 0.050(3) -0.010(2) -0.005(2) C14 0.0345(19) 0.046(3) 0.042(2) 0.0049(19) -0.0060(16) -0.0073(18) O1 0.0634(17) 0.0392(16) 0.0586(17) -0.0021(14) 0.0164(14) -0.0064(14) O1W 0.072(2) 0.059(2) 0.070(2) 0.0056(17) -0.0009(16) -0.0124(17) O2 0.0543(17) 0.048(2) 0.0522(17) -0.0042(14) 0.0058(13) -0.0084(14) O2W 0.112(3) 0.034(2) 0.069(2) 0.000 -0.007(2) 0.000 O3 0.0400(13) 0.067(2) 0.0528(15) 0.0017(15) 0.0035(11) -0.0002(14) _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 O1 1.993(3) 2_657 ? Zn1 O1 1.993(3) . ? Zn1 O1W 2.025(3) . ? Zn1 O1W 2.025(3) 2_657 ? C1 C2 1.370(5) . ? C1 C10 1.416(5) . ? C1 H1A 0.9300 . ? C2 O3 1.368(4) . ? C2 C3 1.416(5) . ? C3 C4 1.352(5) . ? C3 H3A 0.9300 . ? C4 C5 1.408(5) . ? C4 H4A 0.9300 . ? C5 C10 1.416(5) . ? C5 C6 1.425(5) . ? C6 C7 1.364(5) . ? C6 H6A 0.9300 . ? C7 C8 1.400(5) . ? C7 C12 1.521(5) . ? C8 C9 1.370(5) . ? C8 H8A 0.9300 . ? C9 C10 1.419(5) . ? C9 H9A 0.9300 . ? C11 O3 1.414(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.522(6) . ? C12 C13 1.539(7) . ? C12 H12A 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 O2 1.221(5) . ? C14 O1 1.271(5) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8502 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 97.14(17) 2_657 . ? O1 Zn1 O1W 112.50(13) 2_657 . ? O1 Zn1 O1W 113.90(13) . . ? O1 Zn1 O1W 113.90(13) 2_657 2_657 ? O1 Zn1 O1W 112.50(13) . 2_657 ? O1W Zn1 O1W 106.9(2) . 2_657 ? C2 C1 C10 119.6(3) . . ? C2 C1 H1A 120.2 . . ? C10 C1 H1A 120.2 . . ? O3 C2 C1 125.2(3) . . ? O3 C2 C3 114.8(3) . . ? C1 C2 C3 120.0(3) . . ? C4 C3 C2 120.8(4) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 121.2(4) . . ? C3 C4 H4A 119.4 . . ? C5 C4 H4A 119.4 . . ? C4 C5 C10 118.1(3) . . ? C4 C5 C6 122.9(3) . . ? C10 C5 C6 119.0(3) . . ? C7 C6 C5 121.9(3) . . ? C7 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? C6 C7 C8 118.6(3) . . ? C6 C7 C12 121.1(3) . . ? C8 C7 C12 120.3(4) . . ? C9 C8 C7 121.5(4) . . ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C8 C9 C10 121.0(3) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C5 C10 C1 120.3(3) . . ? C5 C10 C9 117.9(3) . . ? C1 C10 C9 121.8(3) . . ? O3 C11 H11A 109.5 . . ? O3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 C14 109.2(3) . . ? C7 C12 C13 110.7(4) . . ? C14 C12 C13 114.4(4) . . ? C7 C12 H12A 107.4 . . ? C14 C12 H12A 107.4 . . ? C13 C12 H12A 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 C14 O1 122.5(5) . . ? O2 C14 C12 119.7(5) . . ? O1 C14 C12 117.7(4) . . ? C14 O1 Zn1 112.0(3) . . ? Zn1 O1W H1WA 109.2 . . ? Zn1 O1W H1WB 109.1 . . ? H1WA O1W H1WB 109.5 . . ? H2WA O2W H2WB 109.1 . . ? C2 O3 C11 116.5(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.495 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.166 #======================================= data_compound_5 #TrackingRef '- naproxen_ni_cu_zn_cd_cd_r3.cif' _database_code_depnum_ccdc_archive 'CCDC 669854' _audit_creation_method SHELXL-97 _chemical_absolute_configuration ad _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H28 Cd O7' _chemical_formula_sum 'C28 H28 Cd O7' _chemical_formula_weight 588.91 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 47.055(4) _cell_length_b 6.1619(5) _cell_length_c 8.4473(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.263(3) _cell_angle_gamma 90.00 _cell_volume 2410.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3203 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 26.5 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.954 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.769 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details SADABS(Sheldrick,1996) _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4581 _diffrn_reflns_av_R_equivalents 0.0125 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -60 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3323 _reflns_number_gt 3220 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0345P)^2^+1.2205P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(9) _refine_ls_number_reflns 3323 _refine_ls_number_parameters 330 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Cd1 Cd -0.272231(13) -0.51725(3) -0.04447(4) 0.02597(7) Uani 1 1 d . . . O1 O -0.25831(6) -0.3733(4) 0.2265(3) 0.0328(5) Uani 1 1 d . . . O1W O -0.27628(7) -0.8570(4) 0.0368(4) 0.0388(6) Uani 1 1 d . . . H1WA H -0.2858 -0.9310 -0.0396 0.058 Uiso 1 1 d R . . H1WB H -0.2850 -0.8582 0.1167 0.058 Uiso 1 1 d R . . O2 O -0.22723(7) -0.3963(6) 0.0644(4) 0.0383(7) Uani 1 1 d . . . O3 O -0.05398(8) -0.3017(5) 0.1001(5) 0.0561(9) Uani 1 1 d . . . O4 O -0.32172(8) -0.4564(5) -0.1156(5) 0.0450(9) Uani 1 1 d . . . O5 O -0.29279(6) -0.2014(4) -0.1697(3) 0.0346(6) Uani 1 1 d . . . O6 O -0.49843(7) -0.3235(6) -0.0697(5) 0.0592(9) Uani 1 1 d . . . C1 C -0.23298(8) -0.3398(5) 0.1959(4) 0.0273(7) Uani 1 1 d . . . C2 C -0.21062(8) -0.2193(6) 0.3183(5) 0.0318(8) Uani 1 1 d . . . H2 H -0.2120 -0.2758 0.4250 0.038 Uiso 1 1 calc R . . C3 C -0.21904(11) 0.0194(6) 0.3152(7) 0.0421(10) Uani 1 1 d . . . H3A H -0.2039 0.1011 0.3803 0.063 Uiso 1 1 calc R . . H3B H -0.2366 0.0357 0.3569 0.063 Uiso 1 1 calc R . . H3C H -0.2219 0.0719 0.2065 0.063 Uiso 1 1 calc R . . C4 C -0.18013(8) -0.2601(5) 0.2915(4) 0.0281(7) Uani 1 1 d . . . C5 C -0.16665(9) -0.4579(5) 0.3478(5) 0.0338(8) Uani 1 1 d . . . H5 H -0.1766 -0.5566 0.4007 0.041 Uiso 1 1 calc R . . C6 C -0.13942(10) -0.5065(5) 0.3263(6) 0.0350(9) Uani 1 1 d . . . H6 H -0.1311 -0.6375 0.3649 0.042 Uiso 1 1 calc R . . C7 C -0.12336(8) -0.3607(6) 0.2459(5) 0.0312(8) Uani 1 1 d . . . C8 C -0.09513(9) -0.4104(6) 0.2195(5) 0.0376(8) Uani 1 1 d . . . H8 H -0.0864 -0.5401 0.2577 0.045 Uiso 1 1 calc R . . C9 C -0.08090(9) -0.2684(7) 0.1383(5) 0.0379(9) Uani 1 1 d . . . C10 C -0.09373(10) -0.0683(7) 0.0819(6) 0.0414(9) Uani 1 1 d . . . H10 H -0.0837 0.0275 0.0267 0.050 Uiso 1 1 calc R . . C11 C -0.12049(10) -0.0159(6) 0.1080(6) 0.0353(9) Uani 1 1 d . . . H11 H -0.1285 0.1172 0.0723 0.042 Uiso 1 1 calc R . . C12 C -0.13657(8) -0.1618(5) 0.1896(4) 0.0281(7) Uani 1 1 d . . . C13 C -0.16492(8) -0.1162(6) 0.2149(5) 0.0321(8) Uani 1 1 d . . . H13 H -0.1735 0.0150 0.1786 0.039 Uiso 1 1 calc R . . C14 C -0.03998(14) -0.5020(8) 0.1517(11) 0.0673(18) Uani 1 1 d . . . H14A H -0.0210 -0.5030 0.1254 0.101 Uiso 1 1 calc R . . H14B H -0.0510 -0.6206 0.0983 0.101 Uiso 1 1 calc R . . H14C H -0.0386 -0.5169 0.2659 0.101 Uiso 1 1 calc R . . C15 C -0.31822(9) -0.2812(6) -0.1810(5) 0.0317(8) Uani 1 1 d . . . C16 C -0.34297(9) -0.1660(6) -0.2931(6) 0.0424(10) Uani 1 1 d . . . H16 H -0.3424 -0.2220 -0.4011 0.051 Uiso 1 1 calc R . . C17 C -0.33750(11) 0.0744(7) -0.3018(7) 0.0522(12) Uani 1 1 d . . . H17A H -0.3192 0.0982 -0.3337 0.078 Uiso 1 1 calc R . . H17B H -0.3374 0.1385 -0.1981 0.078 Uiso 1 1 calc R . . H17C H -0.3525 0.1396 -0.3792 0.078 Uiso 1 1 calc R . . C18 C -0.37277(9) -0.2270(7) -0.2588(6) 0.0404(10) Uani 1 1 d . . . C19 C -0.38501(10) -0.4266(6) -0.3179(6) 0.0418(9) Uani 1 1 d . . . H19 H -0.3746 -0.5181 -0.3739 0.050 Uiso 1 1 calc R . . C20 C -0.41149(10) -0.4877(6) -0.2951(6) 0.0396(10) Uani 1 1 d . . . H20 H -0.4188 -0.6211 -0.3344 0.048 Uiso 1 1 calc R . . C21 C -0.42841(8) -0.3524(6) -0.2121(5) 0.0324(8) Uani 1 1 d . . . C22 C -0.45639(9) -0.4133(6) -0.1875(5) 0.0384(9) Uani 1 1 d . . . H22 H -0.4643 -0.5447 -0.2277 0.046 Uiso 1 1 calc R . . C23 C -0.47178(10) -0.2793(6) -0.1048(6) 0.0410(9) Uani 1 1 d . . . C24 C -0.45995(10) -0.0769(7) -0.0457(6) 0.0460(10) Uani 1 1 d . . . H24 H -0.4705 0.0139 0.0102 0.055 Uiso 1 1 calc R . . C25 C -0.43334(11) -0.0149(6) -0.0701(6) 0.0413(10) Uani 1 1 d . . . H25 H -0.4259 0.1186 -0.0312 0.050 Uiso 1 1 calc R . . C26 C -0.41678(9) -0.1500(6) -0.1534(5) 0.0342(8) Uani 1 1 d . . . C27 C -0.38893(9) -0.0919(6) -0.1793(5) 0.0402(9) Uani 1 1 d . . . H27 H -0.3813 0.0414 -0.1416 0.048 Uiso 1 1 calc R . . C28 C -0.51149(15) -0.5227(8) -0.1259(11) 0.0691(18) Uani 1 1 d . . . H28A H -0.5306 -0.5300 -0.1008 0.104 Uiso 1 1 calc R . . H28B H -0.5001 -0.6410 -0.0747 0.104 Uiso 1 1 calc R . . H28C H -0.5126 -0.5322 -0.2403 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02379(11) 0.02801(10) 0.02648(11) -0.00015(18) 0.00550(7) 0.00031(18) O1 0.0242(13) 0.0456(13) 0.0300(14) 0.0006(11) 0.0083(10) -0.0070(11) O1W 0.0525(17) 0.0313(12) 0.0346(15) -0.0022(11) 0.0127(13) -0.0077(11) O2 0.0338(17) 0.046(2) 0.0375(17) -0.0106(16) 0.0121(13) -0.0085(16) O3 0.0360(18) 0.0569(17) 0.082(3) 0.0034(18) 0.0274(18) 0.0017(14) O4 0.0319(18) 0.0350(15) 0.066(3) 0.0144(15) 0.0024(17) 0.0000(12) O5 0.0257(13) 0.0343(12) 0.0441(16) 0.0043(11) 0.0070(12) 0.0005(10) O6 0.0424(19) 0.0614(18) 0.080(3) 0.0016(18) 0.0275(19) -0.0004(15) C1 0.0272(18) 0.0242(14) 0.0306(19) 0.0010(13) 0.0059(15) -0.0016(12) C2 0.030(2) 0.0349(16) 0.0302(19) -0.0037(14) 0.0055(15) -0.0063(14) C3 0.035(2) 0.0383(19) 0.054(3) -0.0107(17) 0.011(2) -0.0016(15) C4 0.0253(18) 0.0298(15) 0.0304(19) -0.0045(13) 0.0078(15) -0.0027(13) C5 0.033(2) 0.0292(15) 0.041(2) 0.0029(15) 0.0092(17) -0.0055(14) C6 0.031(2) 0.0306(17) 0.044(2) 0.0051(14) 0.0066(18) 0.0021(13) C7 0.0279(19) 0.0308(17) 0.035(2) -0.0002(14) 0.0059(15) -0.0009(14) C8 0.030(2) 0.0348(17) 0.047(2) -0.0007(17) 0.0043(17) 0.0022(15) C9 0.025(2) 0.043(2) 0.047(2) -0.0029(17) 0.0107(17) -0.0021(15) C10 0.038(2) 0.0401(18) 0.050(3) 0.0008(19) 0.018(2) -0.0086(17) C11 0.034(2) 0.0305(18) 0.042(2) 0.0048(15) 0.0095(18) -0.0044(14) C12 0.0242(17) 0.0281(14) 0.0318(19) -0.0005(13) 0.0044(14) -0.0022(13) C13 0.0296(19) 0.0288(17) 0.037(2) -0.0008(15) 0.0025(16) -0.0003(14) C14 0.041(3) 0.067(3) 0.099(6) -0.004(3) 0.025(3) 0.013(2) C15 0.031(2) 0.0293(17) 0.036(2) -0.0008(16) 0.0079(16) 0.0047(15) C16 0.034(2) 0.0408(19) 0.051(3) 0.0053(18) 0.0028(19) 0.0042(16) C17 0.046(3) 0.042(2) 0.067(3) 0.012(2) 0.006(2) 0.003(2) C18 0.029(2) 0.0357(19) 0.055(3) 0.0097(18) 0.0015(19) 0.0055(16) C19 0.040(2) 0.0357(18) 0.052(3) 0.0020(18) 0.013(2) 0.0099(17) C20 0.037(2) 0.0332(19) 0.047(3) -0.0044(16) 0.003(2) 0.0031(15) C21 0.0296(19) 0.0318(16) 0.034(2) 0.0022(14) 0.0017(16) 0.0017(14) C22 0.036(2) 0.0341(18) 0.044(2) -0.0005(17) 0.0044(18) -0.0023(16) C23 0.033(2) 0.045(2) 0.047(2) 0.0059(18) 0.0127(19) 0.0041(17) C24 0.047(3) 0.045(2) 0.048(3) -0.005(2) 0.014(2) 0.0113(19) C25 0.043(3) 0.0347(18) 0.045(3) -0.0050(16) 0.004(2) 0.0012(16) C26 0.034(2) 0.0310(17) 0.036(2) 0.0020(15) 0.0001(16) 0.0038(15) C27 0.035(2) 0.0291(16) 0.053(3) 0.0035(17) -0.0029(19) -0.0025(15) C28 0.049(3) 0.066(3) 0.097(6) 0.009(3) 0.026(4) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1W 2.222(2) . ? Cd1 O1 2.254(3) 2_544 ? Cd1 O2 2.278(3) . ? Cd1 O4 2.329(4) . ? Cd1 O5 2.341(2) . ? Cd1 O1 2.433(3) . ? Cd1 C15 2.691(4) . ? Cd1 C1 2.719(4) . ? O1 C1 1.281(4) . ? O1 Cd1 2.254(3) 2_545 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8499 . ? O2 C1 1.239(5) . ? O3 C9 1.377(5) . ? O3 C14 1.430(6) . ? O4 C15 1.237(4) . ? O5 C15 1.282(5) . ? O6 C23 1.367(5) . ? O6 C28 1.416(7) . ? C1 C2 1.529(5) . ? C2 C4 1.513(5) . ? C2 C3 1.522(5) . ? C2 H2 0.9800 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C13 1.372(5) . ? C4 C5 1.417(5) . ? C5 C6 1.359(6) . ? C5 H5 0.9300 . ? C6 C7 1.422(6) . ? C6 H6 0.9300 . ? C7 C12 1.418(5) . ? C7 C8 1.419(5) . ? C8 C9 1.360(6) . ? C8 H8 0.9300 . ? C9 C10 1.417(6) . ? C10 C11 1.356(6) . ? C10 H10 0.9300 . ? C11 C12 1.429(5) . ? C11 H11 0.9300 . ? C12 C13 1.416(5) . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.538(6) . ? C16 C17 1.507(6) . ? C16 C18 1.529(6) . ? C16 H16 0.9800 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C27 1.380(6) . ? C18 C19 1.411(6) . ? C19 C20 1.348(7) . ? C19 H19 0.9300 . ? C20 C21 1.421(6) . ? C20 H20 0.9300 . ? C21 C26 1.416(5) . ? C21 C22 1.419(6) . ? C22 C23 1.369(6) . ? C22 H22 0.9300 . ? C23 C24 1.420(6) . ? C24 C25 1.359(7) . ? C24 H24 0.9300 . ? C25 C26 1.412(6) . ? C25 H25 0.9300 . ? C26 C27 1.413(6) . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? 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 O1W Cd1 O1 92.12(10) . 2_544 ? O1W Cd1 O2 107.94(13) . . ? O1 Cd1 O2 93.05(11) 2_544 . ? O1W Cd1 O4 95.42(11) . . ? O1 Cd1 O4 104.88(14) 2_544 . ? O2 Cd1 O4 150.01(12) . . ? O1W Cd1 O5 150.68(11) . . ? O1 Cd1 O5 91.18(10) 2_544 . ? O2 Cd1 O5 100.96(11) . . ? O4 Cd1 O5 55.67(10) . . ? O1W Cd1 O1 94.39(10) . . ? O1 Cd1 O1 147.78(13) 2_544 . ? O2 Cd1 O1 54.96(10) . . ? O4 Cd1 O1 105.85(13) . . ? O5 Cd1 O1 98.18(9) . . ? O1W Cd1 C15 122.35(12) . . ? O1 Cd1 C15 97.38(11) 2_544 . ? O2 Cd1 C15 127.95(14) . . ? O4 Cd1 C15 27.34(10) . . ? O5 Cd1 C15 28.44(10) . . ? O1 Cd1 C15 105.50(10) . . ? O1W Cd1 C1 103.45(11) . . ? O1 Cd1 C1 119.92(11) 2_544 . ? O2 Cd1 C1 26.90(11) . . ? O4 Cd1 C1 130.00(13) . . ? O5 Cd1 C1 100.03(9) . . ? O1 Cd1 C1 28.09(9) . . ? C15 Cd1 C1 119.34(10) . . ? C1 O1 Cd1 130.2(2) . 2_545 ? C1 O1 Cd1 88.5(2) . . ? Cd1 O1 Cd1 128.88(11) 2_545 . ? Cd1 O1W H1WA 109.5 . . ? Cd1 O1W H1WB 109.5 . . ? H1WA O1W H1WB 109.5 . . ? C1 O2 Cd1 96.8(2) . . ? C9 O3 C14 116.8(4) . . ? C15 O4 Cd1 92.8(3) . . ? C15 O5 Cd1 91.1(2) . . ? C23 O6 C28 117.4(4) . . ? O2 C1 O1 119.7(3) . . ? O2 C1 C2 120.6(3) . . ? O1 C1 C2 119.6(3) . . ? O2 C1 Cd1 56.3(2) . . ? O1 C1 Cd1 63.46(18) . . ? C2 C1 Cd1 173.7(2) . . ? C4 C2 C3 114.1(3) . . ? C4 C2 C1 112.0(3) . . ? C3 C2 C1 108.2(3) . . ? C4 C2 H2 107.4 . . ? C3 C2 H2 107.4 . . ? C1 C2 H2 107.4 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C13 C4 C5 118.3(3) . . ? C13 C4 C2 123.5(3) . . ? C5 C4 C2 118.2(3) . . ? C6 C5 C4 121.4(3) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 121.2(3) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C12 C7 C8 120.1(3) . . ? C12 C7 C6 117.9(3) . . ? C8 C7 C6 122.0(3) . . ? C9 C8 C7 120.0(4) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 O3 125.4(4) . . ? C8 C9 C10 120.7(4) . . ? O3 C9 C10 113.9(4) . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 121.0(4) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C7 119.3(3) . . ? C13 C12 C11 122.8(3) . . ? C7 C12 C11 117.9(3) . . ? C4 C13 C12 121.8(3) . . ? C4 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O4 C15 O5 119.9(4) . . ? O4 C15 C16 122.1(4) . . ? O5 C15 C16 117.6(3) . . ? O4 C15 Cd1 59.8(2) . . ? O5 C15 Cd1 60.43(18) . . ? C16 C15 Cd1 167.6(3) . . ? C17 C16 C18 114.9(4) . . ? C17 C16 C15 111.5(4) . . ? C18 C16 C15 112.9(4) . . ? C17 C16 H16 105.5 . . ? C18 C16 H16 105.5 . . ? C15 C16 H16 105.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C27 C18 C19 118.2(4) . . ? C27 C18 C16 123.2(4) . . ? C19 C18 C16 118.5(4) . . ? C20 C19 C18 121.5(4) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 121.4(4) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C26 C21 C22 119.5(3) . . ? C26 C21 C20 118.3(4) . . ? C22 C21 C20 122.2(4) . . ? C23 C22 C21 120.3(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? O6 C23 C22 125.4(4) . . ? O6 C23 C24 114.6(4) . . ? C22 C23 C24 120.0(4) . . ? C25 C24 C23 120.5(4) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 121.0(4) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C25 C26 C27 122.5(4) . . ? C25 C26 C21 118.7(4) . . ? C27 C26 C21 118.7(4) . . ? C18 C27 C26 121.9(4) . . ? C18 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? O6 C28 H28A 109.5 . . ? O6 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O6 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Cd1 O1 C1 110.58(19) . . . . ? O1 Cd1 O1 C1 9.5(2) 2_544 . . . ? O2 Cd1 O1 C1 1.7(2) . . . . ? O4 Cd1 O1 C1 -152.51(19) . . . . ? O5 Cd1 O1 C1 -95.98(19) . . . . ? C15 Cd1 O1 C1 -124.09(19) . . . . ? O1W Cd1 O1 Cd1 -33.22(17) . . . 2_545 ? O1 Cd1 O1 Cd1 -134.27(16) 2_544 . . 2_545 ? O2 Cd1 O1 Cd1 -142.1(2) . . . 2_545 ? O4 Cd1 O1 Cd1 63.69(17) . . . 2_545 ? O5 Cd1 O1 Cd1 120.22(14) . . . 2_545 ? C15 Cd1 O1 Cd1 92.11(17) . . . 2_545 ? C1 Cd1 O1 Cd1 -143.8(3) . . . 2_545 ? O1W Cd1 O2 C1 -84.4(3) . . . . ? O1 Cd1 O2 C1 -177.6(2) 2_544 . . . ? O4 Cd1 O2 C1 55.0(4) . . . . ? O5 Cd1 O2 C1 90.6(3) . . . . ? O1 Cd1 O2 C1 -1.8(2) . . . . ? C15 Cd1 O2 C1 80.6(3) . . . . ? O1W Cd1 O4 C15 -170.7(3) . . . . ? O1 Cd1 O4 C15 -77.0(3) 2_544 . . . ? O2 Cd1 O4 C15 47.8(5) . . . . ? O5 Cd1 O4 C15 4.0(2) . . . . ? O1 Cd1 O4 C15 93.2(3) . . . . ? C1 Cd1 O4 C15 76.7(3) . . . . ? O1W Cd1 O5 C15 6.9(3) . . . . ? O1 Cd1 O5 C15 103.4(2) 2_544 . . . ? O2 Cd1 O5 C15 -163.3(2) . . . . ? O4 Cd1 O5 C15 -3.9(2) . . . . ? O1 Cd1 O5 C15 -107.5(2) . . . . ? C1 Cd1 O5 C15 -135.9(2) . . . . ? Cd1 O2 C1 O1 3.2(4) . . . . ? Cd1 O2 C1 C2 -173.5(3) . . . . ? Cd1 O1 C1 O2 140.1(3) 2_545 . . . ? Cd1 O1 C1 O2 -3.0(3) . . . . ? Cd1 O1 C1 C2 -43.2(4) 2_545 . . . ? Cd1 O1 C1 C2 173.8(3) . . . . ? Cd1 O1 C1 Cd1 143.0(3) 2_545 . . . ? O1W Cd1 C1 O2 103.2(3) . . . . ? O1 Cd1 C1 O2 2.7(3) 2_544 . . . ? O4 Cd1 C1 O2 -147.7(3) . . . . ? O5 Cd1 C1 O2 -94.5(3) . . . . ? O1 Cd1 C1 O2 176.9(4) . . . . ? C15 Cd1 C1 O2 -116.8(3) . . . . ? O1W Cd1 C1 O1 -73.7(2) . . . . ? O1 Cd1 C1 O1 -174.15(13) 2_544 . . . ? O2 Cd1 C1 O1 -176.9(4) . . . . ? O4 Cd1 C1 O1 35.4(2) . . . . ? O5 Cd1 C1 O1 88.61(19) . . . . ? C15 Cd1 C1 O1 66.3(2) . . . . ? O1W Cd1 C1 C2 166(2) . . . . ? O1 Cd1 C1 C2 65(2) 2_544 . . . ? O2 Cd1 C1 C2 62(2) . . . . ? O4 Cd1 C1 C2 -85(2) . . . . ? O5 Cd1 C1 C2 -32(2) . . . . ? O1 Cd1 C1 C2 -121(2) . . . . ? C15 Cd1 C1 C2 -54(2) . . . . ? O2 C1 C2 C4 -22.8(5) . . . . ? O1 C1 C2 C4 160.5(3) . . . . ? Cd1 C1 C2 C4 -82(2) . . . . ? O2 C1 C2 C3 103.9(4) . . . . ? O1 C1 C2 C3 -72.8(4) . . . . ? Cd1 C1 C2 C3 45(2) . . . . ? C3 C2 C4 C13 -22.8(6) . . . . ? C1 C2 C4 C13 100.6(4) . . . . ? C3 C2 C4 C5 157.6(4) . . . . ? C1 C2 C4 C5 -79.1(4) . . . . ? C13 C4 C5 C6 -0.4(6) . . . . ? C2 C4 C5 C6 179.2(4) . . . . ? C4 C5 C6 C7 -0.2(7) . . . . ? C5 C6 C7 C12 0.4(6) . . . . ? C5 C6 C7 C8 -178.7(4) . . . . ? C12 C7 C8 C9 -0.8(6) . . . . ? C6 C7 C8 C9 178.3(4) . . . . ? C7 C8 C9 O3 -177.5(4) . . . . ? C7 C8 C9 C10 1.2(7) . . . . ? C14 O3 C9 C8 -0.4(7) . . . . ? C14 O3 C9 C10 -179.2(5) . . . . ? C8 C9 C10 C11 -0.1(7) . . . . ? O3 C9 C10 C11 178.7(4) . . . . ? C9 C10 C11 C12 -1.3(7) . . . . ? C8 C7 C12 C13 179.1(4) . . . . ? C6 C7 C12 C13 -0.1(5) . . . . ? C8 C7 C12 C11 -0.5(6) . . . . ? C6 C7 C12 C11 -179.7(4) . . . . ? C10 C11 C12 C13 -178.0(4) . . . . ? C10 C11 C12 C7 1.6(6) . . . . ? C5 C4 C13 C12 0.8(6) . . . . ? C2 C4 C13 C12 -178.9(3) . . . . ? C7 C12 C13 C4 -0.5(6) . . . . ? C11 C12 C13 C4 179.0(4) . . . . ? Cd1 O4 C15 O5 -7.0(4) . . . . ? Cd1 O4 C15 C16 165.7(3) . . . . ? Cd1 O5 C15 O4 7.0(4) . . . . ? Cd1 O5 C15 C16 -166.1(3) . . . . ? O1W Cd1 C15 O4 11.0(3) . . . . ? O1 Cd1 C15 O4 108.3(3) 2_544 . . . ? O2 Cd1 C15 O4 -152.0(3) . . . . ? O5 Cd1 C15 O4 -173.0(4) . . . . ? O1 Cd1 C15 O4 -94.6(3) . . . . ? C1 Cd1 C15 O4 -121.2(3) . . . . ? O1W Cd1 C15 O5 -176.0(2) . . . . ? O1 Cd1 C15 O5 -78.7(2) 2_544 . . . ? O2 Cd1 C15 O5 21.0(3) . . . . ? O4 Cd1 C15 O5 173.0(4) . . . . ? O1 Cd1 C15 O5 78.4(2) . . . . ? C1 Cd1 C15 O5 51.8(3) . . . . ? O1W Cd1 C15 C16 -91.8(13) . . . . ? O1 Cd1 C15 C16 5.5(13) 2_544 . . . ? O2 Cd1 C15 C16 105.2(13) . . . . ? O4 Cd1 C15 C16 -102.8(14) . . . . ? O5 Cd1 C15 C16 84.2(13) . . . . ? O1 Cd1 C15 C16 162.6(13) . . . . ? C1 Cd1 C15 C16 136.0(13) . . . . ? O4 C15 C16 C17 156.4(4) . . . . ? O5 C15 C16 C17 -30.8(5) . . . . ? Cd1 C15 C16 C17 -108.3(13) . . . . ? O4 C15 C16 C18 25.2(6) . . . . ? O5 C15 C16 C18 -161.9(4) . . . . ? Cd1 C15 C16 C18 120.5(13) . . . . ? C17 C16 C18 C27 -25.3(7) . . . . ? C15 C16 C18 C27 104.1(5) . . . . ? C17 C16 C18 C19 151.5(4) . . . . ? C15 C16 C18 C19 -79.0(5) . . . . ? C27 C18 C19 C20 -1.4(7) . . . . ? C16 C18 C19 C20 -178.4(4) . . . . ? C18 C19 C20 C21 0.8(7) . . . . ? C19 C20 C21 C26 0.1(7) . . . . ? C19 C20 C21 C22 179.7(4) . . . . ? C26 C21 C22 C23 -1.3(6) . . . . ? C20 C21 C22 C23 179.1(4) . . . . ? C28 O6 C23 C22 -1.3(8) . . . . ? C28 O6 C23 C24 179.8(5) . . . . ? C21 C22 C23 O6 -177.9(4) . . . . ? C21 C22 C23 C24 1.0(7) . . . . ? O6 C23 C24 C25 178.9(4) . . . . ? C22 C23 C24 C25 -0.2(7) . . . . ? C23 C24 C25 C26 -0.4(7) . . . . ? C24 C25 C26 C27 -179.2(4) . . . . ? C24 C25 C26 C21 0.2(7) . . . . ? C22 C21 C26 C25 0.7(6) . . . . ? C20 C21 C26 C25 -179.7(4) . . . . ? C22 C21 C26 C27 -179.9(4) . . . . ? C20 C21 C26 C27 -0.2(6) . . . . ? C19 C18 C27 C26 1.3(7) . . . . ? C16 C18 C27 C26 178.1(4) . . . . ? C25 C26 C27 C18 179.0(4) . . . . ? C21 C26 C27 C18 -0.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.042 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.061 #==END of File #====================================== data_compound_1 #TrackingRef '- naproxen_ni_cu_zn_cd_cd_r3.cif' _database_code_depnum_ccdc_archive 'CCDC 717532' _audit_creation_method SHELXL-97 _chemical_absolute_configuration rm _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C14 H13 O3), H12 Ni O6, 2(H2 O)' _chemical_formula_sum 'C28 H42 Ni O14' _chemical_formula_weight 661.31 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.909(5) _cell_length_b 8.910(5) _cell_length_c 20.680(5) _cell_angle_alpha 90.753(5) _cell_angle_beta 99.662(5) _cell_angle_gamma 99.077(5) _cell_volume 1596.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4947 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 24.74 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.851 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details SADABS(Sheldrick,1996) _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29272 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.55 _reflns_number_total 13167 _reflns_number_gt 8334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 13167 _refine_ls_number_parameters 783 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2288 _refine_ls_wR_factor_gt 0.2019 _refine_ls_goodness_of_fit_ref 1.256 _refine_ls_restrained_S_all 1.256 _refine_ls_shift/su_max 0.010 _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 O1 O 0.3546(8) 0.6071(7) 0.7331(3) 0.0579(17) Uani 1 1 d . . . O2 O 0.2771(8) 0.3771(7) 0.6910(3) 0.0572(17) Uani 1 1 d . . . O3 O -0.1317(7) 0.8013(7) 1.0283(3) 0.0511(15) Uani 1 1 d . . . C1 C -0.0874(9) 0.6268(8) 0.9450(4) 0.0396(18) Uani 1 1 d . . . H1A H -0.1922 0.5905 0.9322 0.048 Uiso 1 1 calc R . . C2 C -0.0399(10) 0.7361(9) 0.9951(4) 0.0403(18) Uani 1 1 d . . . C3 C 0.1224(11) 0.7883(11) 1.0149(5) 0.046(2) Uani 1 1 d . . . H3A H 0.1559 0.8598 1.0495 0.056 Uiso 1 1 calc R . . C4 C 0.2276(11) 0.7361(11) 0.9843(4) 0.045(2) Uani 1 1 d . . . H4A H 0.3319 0.7730 0.9980 0.054 Uiso 1 1 calc R . . C5 C 0.1813(9) 0.6257(9) 0.9317(4) 0.0388(17) Uani 1 1 d . . . C6 C 0.2867(10) 0.5715(10) 0.8979(5) 0.038(2) Uani 1 1 d . . . H6A H 0.3913 0.6090 0.9102 0.045 Uiso 1 1 calc R . . C7 C 0.2411(8) 0.4660(8) 0.8475(4) 0.0331(15) Uani 1 1 d . . . C8 C 0.0811(9) 0.4072(9) 0.8294(4) 0.0403(18) Uani 1 1 d . . . H8A H 0.0488 0.3314 0.7964 0.048 Uiso 1 1 calc R . . C9 C -0.0248(9) 0.4605(10) 0.8596(4) 0.044(2) Uani 1 1 d . . . H9A H -0.1290 0.4247 0.8450 0.053 Uiso 1 1 calc R . . C10 C 0.0192(8) 0.5696(8) 0.9130(4) 0.0350(16) Uani 1 1 d . . . C11 C -0.2908(12) 0.7565(14) 1.0111(6) 0.060(3) Uani 1 1 d . . . H11A H -0.3420 0.8051 1.0408 0.091 Uiso 1 1 calc R . . H11B H -0.3156 0.6481 1.0135 0.091 Uiso 1 1 calc R . . H11C H -0.3244 0.7854 0.9671 0.091 Uiso 1 1 calc R . . C12 C 0.3510(8) 0.4070(9) 0.8072(4) 0.0360(16) Uani 1 1 d . . . H12A H 0.3262 0.2957 0.8032 0.043 Uiso 1 1 calc R . . C13 C 0.5230(9) 0.4519(10) 0.8369(4) 0.046(2) Uani 1 1 d . . . H13A H 0.5409 0.4181 0.8810 0.070 Uiso 1 1 calc R . . H13B H 0.5513 0.5605 0.8372 0.070 Uiso 1 1 calc R . . H13C H 0.5841 0.4052 0.8109 0.070 Uiso 1 1 calc R . . C14 C 0.3232(9) 0.4704(10) 0.7385(4) 0.035(2) Uani 1 1 d . . . O4 O 0.1748(8) 0.3522(8) 0.4655(3) 0.066(2) Uani 1 1 d . . . O5 O 0.3996(7) 0.4003(7) 0.4320(3) 0.0546(16) Uani 1 1 d . . . O6 O 0.4682(7) -0.2387(7) 0.1271(3) 0.0517(15) Uani 1 1 d . . . C15 C 0.3442(9) -0.1546(8) 0.2148(4) 0.0376(17) Uani 1 1 d . . . H15A H 0.3182 -0.2531 0.2282 0.045 Uiso 1 1 calc R . . C16 C 0.4214(9) -0.1292(9) 0.1627(4) 0.0408(18) Uani 1 1 d . . . C17 C 0.4594(12) 0.0214(11) 0.1417(5) 0.049(2) Uani 1 1 d . . . H17A H 0.5103 0.0382 0.1061 0.058 Uiso 1 1 calc R . . C18 C 0.4218(11) 0.1402(11) 0.1735(5) 0.047(2) Uani 1 1 d . . . H18A H 0.4478 0.2378 0.1591 0.057 Uiso 1 1 calc R . . C19 C 0.3447(8) 0.1211(8) 0.2279(4) 0.0340(16) Uani 1 1 d . . . C20 C 0.3023(10) 0.2431(10) 0.2612(4) 0.0357(19) Uani 1 1 d . . . H20A H 0.3270 0.3415 0.2474 0.043 Uiso 1 1 calc R . . C21 C 0.2251(8) 0.2197(8) 0.3138(4) 0.0344(16) Uani 1 1 d . . . C22 C 0.1879(9) 0.0706(8) 0.3333(4) 0.0412(19) Uani 1 1 d . . . H22A H 0.1350 0.0530 0.3683 0.049 Uiso 1 1 calc R . . C23 C 0.2281(10) -0.0516(9) 0.3018(4) 0.048(2) Uani 1 1 d . . . H23A H 0.2039 -0.1491 0.3166 0.057 Uiso 1 1 calc R . . C24 C 0.3046(8) -0.0306(8) 0.2479(4) 0.0345(16) Uani 1 1 d . . . C25 C 0.4356(13) -0.3904(12) 0.1447(6) 0.057(3) Uani 1 1 d . . . H25A H 0.4617 -0.4560 0.1125 0.086 Uiso 1 1 calc R . . H25B H 0.3277 -0.4160 0.1466 0.086 Uiso 1 1 calc R . . H25C H 0.4951 -0.4031 0.1869 0.086 Uiso 1 1 calc R . . C26 C 0.1752(8) 0.3475(8) 0.3489(4) 0.0351(16) Uani 1 1 d . . . H26A H 0.0639 0.3204 0.3481 0.042 Uiso 1 1 calc R . . C27 C 0.2020(10) 0.5007(8) 0.3186(4) 0.047(2) Uani 1 1 d . . . H27A H 0.1502 0.4929 0.2738 0.071 Uiso 1 1 calc R . . H27B H 0.3107 0.5326 0.3201 0.071 Uiso 1 1 calc R . . H27C H 0.1622 0.5738 0.3426 0.071 Uiso 1 1 calc R . . C28 C 0.2529(10) 0.3659(10) 0.4208(5) 0.038(2) Uani 1 1 d . . . O7 O 0.7161(7) 0.8235(8) 0.4628(3) 0.0564(16) Uani 1 1 d . . . O8 O 0.9249(6) 0.8795(7) 0.4204(3) 0.0550(16) Uani 1 1 d . . . O9 O 0.9745(7) 0.2464(7) 0.1254(3) 0.0535(15) Uani 1 1 d . . . C29 C 0.8399(8) 0.3316(9) 0.2079(4) 0.0395(18) Uani 1 1 d . . . H29A H 0.8099 0.2329 0.2203 0.047 Uiso 1 1 calc R . . C30 C 0.9239(9) 0.3572(9) 0.1588(4) 0.0409(18) Uani 1 1 d . . . C31 C 0.9652(11) 0.5045(12) 0.1389(5) 0.047(2) Uani 1 1 d . . . H31A H 1.0179 0.5192 0.1037 0.056 Uiso 1 1 calc R . . C32 C 0.9306(11) 0.6271(11) 0.1694(5) 0.046(2) Uani 1 1 d . . . H32A H 0.9623 0.7244 0.1559 0.055 Uiso 1 1 calc R . . C33 C 0.8463(8) 0.6069(9) 0.2219(4) 0.0380(17) Uani 1 1 d . . . C34 C 0.8078(10) 0.7304(10) 0.2555(5) 0.038(2) Uani 1 1 d . . . H34A H 0.8378 0.8288 0.2428 0.046 Uiso 1 1 calc R . . C35 C 0.7277(8) 0.7089(8) 0.3062(4) 0.0352(16) Uani 1 1 d . . . C36 C 0.6781(9) 0.5603(9) 0.3245(4) 0.0389(17) Uani 1 1 d . . . H36A H 0.6189 0.5447 0.3575 0.047 Uiso 1 1 calc R . . C37 C 0.7168(10) 0.4385(9) 0.2937(4) 0.0435(19) Uani 1 1 d . . . H37A H 0.6891 0.3413 0.3081 0.052 Uiso 1 1 calc R . . C38 C 0.7982(8) 0.4573(8) 0.2402(4) 0.0353(16) Uani 1 1 d . . . C39 C 0.9380(14) 0.0944(12) 0.1441(6) 0.064(3) Uani 1 1 d . . . H39A H 0.9591 0.0263 0.1116 0.095 Uiso 1 1 calc R . . H39B H 0.8307 0.0728 0.1475 0.095 Uiso 1 1 calc R . . H39C H 0.9996 0.0812 0.1858 0.095 Uiso 1 1 calc R . . C40 C 0.6894(8) 0.8403(8) 0.3464(3) 0.0336(16) Uani 1 1 d . . . H40A H 0.5802 0.8175 0.3506 0.040 Uiso 1 1 calc R . . C41 C 0.7185(10) 0.9967(9) 0.3165(4) 0.048(2) Uani 1 1 d . . . H41A H 0.6845 1.0708 0.3423 0.072 Uiso 1 1 calc R . . H41B H 0.6624 0.9919 0.2724 0.072 Uiso 1 1 calc R . . H41C H 0.8268 1.0252 0.3159 0.072 Uiso 1 1 calc R . . C42 C 0.7843(10) 0.8456(10) 0.4133(4) 0.034(2) Uani 1 1 d . . . O10 O 0.8029(9) -0.1657(8) 0.6880(3) 0.069(2) Uani 1 1 d . . . O11 O 0.8684(7) 0.0747(7) 0.7220(3) 0.0513(15) Uani 1 1 d . . . O12 O 0.3822(7) 0.2978(7) 1.0261(3) 0.0510(15) Uani 1 1 d . . . C43 C 0.4223(9) 0.1282(9) 0.9386(4) 0.0396(18) Uani 1 1 d . . . H43A H 0.3171 0.0952 0.9253 0.048 Uiso 1 1 calc R . . C44 C 0.4753(9) 0.2317(9) 0.9904(4) 0.0390(18) Uani 1 1 d . . . C45 C 0.6342(11) 0.2811(11) 1.0111(5) 0.046(2) Uani 1 1 d . . . H45A H 0.6678 0.3513 1.0463 0.055 Uiso 1 1 calc R . . C46 C 0.7399(11) 0.2265(11) 0.9799(4) 0.046(2) Uani 1 1 d . . . H46A H 0.8448 0.2591 0.9944 0.055 Uiso 1 1 calc R . . C47 C 0.6916(8) 0.1218(8) 0.9261(3) 0.0336(16) Uani 1 1 d . . . C48 C 0.7974(10) 0.0634(10) 0.8925(4) 0.037(2) Uani 1 1 d . . . H48A H 0.9026 0.0955 0.9062 0.044 Uiso 1 1 calc R . . C49 C 0.7485(8) -0.0391(8) 0.8406(4) 0.0335(16) Uani 1 1 d . . . C50 C 0.5897(8) -0.0875(9) 0.8207(4) 0.043(2) Uani 1 1 d . . . H50A H 0.5552 -0.1583 0.7858 0.052 Uiso 1 1 calc R . . C51 C 0.4845(9) -0.0320(10) 0.8518(4) 0.046(2) Uani 1 1 d . . . H51A H 0.3798 -0.0639 0.8368 0.055 Uiso 1 1 calc R . . C52 C 0.5313(8) 0.0729(8) 0.9062(4) 0.0362(17) Uani 1 1 d . . . C53 C 0.2251(12) 0.2552(12) 1.0107(6) 0.055(3) Uani 1 1 d . . . H53A H 0.1780 0.2854 1.0462 0.083 Uiso 1 1 calc R . . H53B H 0.2009 0.1467 1.0035 0.083 Uiso 1 1 calc R . . H53C H 0.1866 0.3036 0.9715 0.083 Uiso 1 1 calc R . . C54 C 0.8581(8) -0.1088(8) 0.8047(3) 0.0319(15) Uani 1 1 d . . . H54A H 0.8305 -0.2198 0.8047 0.038 Uiso 1 1 calc R . . C55 C 1.0260(9) -0.0666(10) 0.8350(4) 0.047(2) Uani 1 1 d . . . H55A H 1.0400 -0.0938 0.8802 0.070 Uiso 1 1 calc R . . H55B H 1.0576 0.0409 0.8326 0.070 Uiso 1 1 calc R . . H55C H 1.0871 -0.1202 0.8117 0.070 Uiso 1 1 calc R . . C56 C 0.8389(10) -0.0612(11) 0.7324(4) 0.040(2) Uani 1 1 d . . . Ni1 Ni 0.06513(9) 0.66871(9) 0.57678(5) 0.0262(2) Uani 1 1 d . . . O1W O -0.0739(8) 0.8330(7) 0.5764(3) 0.0569(17) Uani 1 1 d . . . H1 H -0.1481 0.8323 0.5445 0.085 Uiso 1 1 d R . . H2 H -0.0802 0.9017 0.6042 0.085 Uiso 1 1 d R . . O2W O -0.0918(10) 0.5340(9) 0.5027(4) 0.091(3) Uani 1 1 d . . . H3 H -0.1379 0.5406 0.4636 0.136 Uiso 1 1 d R . . H4 H -0.1209 0.4450 0.5149 0.136 Uiso 1 1 d R . . O3W O -0.0328(9) 0.5461(9) 0.6496(4) 0.083(2) Uani 1 1 d . . . H5 H -0.0234 0.4741 0.6758 0.124 Uiso 1 1 d R . . H6 H -0.0696 0.6137 0.6685 0.124 Uiso 1 1 d R . . O4W O 0.1643(7) 0.7974(8) 0.5045(3) 0.0539(16) Uani 1 1 d . . . H7 H 0.0920 0.7922 0.4716 0.081 Uiso 1 1 d R . . H8 H 0.2445 0.8491 0.4938 0.081 Uiso 1 1 d R . . O5W O 0.2308(7) 0.8042(7) 0.6487(3) 0.0469(14) Uani 1 1 d . . . H9 H 0.2438 0.7491 0.6818 0.070 Uiso 1 1 d R . . H10 H 0.2840 0.8916 0.6593 0.070 Uiso 1 1 d R . . O6W O 0.2291(8) 0.5298(8) 0.5777(3) 0.0600(18) Uani 1 1 d . . . H11 H 0.2576 0.4728 0.6085 0.090 Uiso 1 1 d R . . H12 H 0.2757 0.5141 0.5462 0.090 Uiso 1 1 d R . . Ni2 Ni 0.55506(10) 0.15817(10) 0.57682(6) 0.0285(3) Uani 1 1 d . . . O7W O 0.3123(8) 0.1319(8) 0.5593(4) 0.071(2) Uani 1 1 d . . . H13 H 0.2584 0.1119 0.5893 0.107 Uiso 1 1 d R . . H14 H 0.2573 0.1695 0.5280 0.107 Uiso 1 1 d R . . O8W O 0.5359(8) -0.0761(9) 0.5941(4) 0.074(2) Uani 1 1 d . . . H15 H 0.4751 -0.1574 0.5798 0.111 Uiso 1 1 d R . . H16 H 0.6056 -0.0999 0.6237 0.111 Uiso 1 1 d R . . O9W O 0.5692(9) 0.2098(9) 0.6774(4) 0.078(2) Uani 1 1 d . . . H17 H 0.6488 0.2380 0.7064 0.117 Uiso 1 1 d R . . H18 H 0.4935 0.1836 0.6972 0.117 Uiso 1 1 d R . . O10W O 0.5582(10) 0.1234(9) 0.4768(4) 0.085(2) Uani 1 1 d . . . H19 H 0.5857 0.1782 0.4461 0.128 Uiso 1 1 d R . . H20 H 0.4909 0.0494 0.4591 0.128 Uiso 1 1 d R . . O11W O 0.5736(7) 0.3897(6) 0.5550(3) 0.0507(15) Uani 1 1 d . . . H21 H 0.5556 0.4487 0.5237 0.076 Uiso 1 1 d R . . H22 H 0.6432 0.4387 0.5843 0.076 Uiso 1 1 d R . . O12W O 0.7966(7) 0.1889(7) 0.5986(3) 0.0516(16) Uani 1 1 d . . . H23 H 0.8541 0.1831 0.6354 0.077 Uiso 1 1 d R . . H24 H 0.8549 0.2103 0.5703 0.077 Uiso 1 1 d R . . O13W O 0.1697(9) 0.0781(7) 0.6924(4) 0.077(2) Uani 1 1 d . . . H25 H 0.2269 0.1438 0.7198 0.116 Uiso 1 1 d R . . H26 H 0.0947 0.0379 0.7103 0.116 Uiso 1 1 d R . . O14W O 0.4176(7) 0.7162(8) 0.4610(4) 0.076(2) Uani 1 1 d . . . H27 H 0.3863 0.6627 0.4256 0.114 Uiso 1 1 d R . . H28 H 0.5099 0.7583 0.4605 0.114 Uiso 1 1 d R . . O15W O 0.6112(8) 0.5671(6) 0.6693(4) 0.0650(19) Uani 1 1 d . . . H29 H 0.6577 0.5209 0.7003 0.097 Uiso 1 1 d R . . H30 H 0.5620 0.6269 0.6865 0.097 Uiso 1 1 d R . . O16W O 0.9177(7) 0.1680(7) 0.4845(4) 0.0645(19) Uani 1 1 d . . . H31 H 0.9620 0.2302 0.4601 0.097 Uiso 1 1 d R . . H32 H 0.8805 0.0869 0.4614 0.097 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.072(4) 0.048(4) 0.044(4) 0.023(3) -0.007(3) -0.003(3) O2 0.074(4) 0.051(4) 0.040(4) 0.002(3) 0.006(3) -0.007(3) O3 0.058(4) 0.063(4) 0.037(3) -0.006(3) 0.011(3) 0.022(3) C1 0.037(4) 0.036(4) 0.045(5) 0.000(3) 0.008(3) 0.002(3) C2 0.055(5) 0.043(4) 0.024(4) 0.003(3) 0.007(3) 0.011(4) C3 0.055(5) 0.057(5) 0.028(5) 0.000(4) 0.002(4) 0.017(4) C4 0.041(5) 0.052(5) 0.036(5) -0.003(4) -0.009(4) 0.009(4) C5 0.041(4) 0.039(4) 0.033(4) 0.002(3) 0.001(3) 0.002(3) C6 0.029(4) 0.040(4) 0.041(5) 0.003(4) -0.004(3) 0.003(3) C7 0.029(4) 0.034(4) 0.034(4) 0.007(3) -0.001(3) 0.003(3) C8 0.038(4) 0.043(4) 0.035(4) -0.001(3) 0.004(3) -0.003(3) C9 0.031(4) 0.050(5) 0.050(5) -0.012(4) 0.005(4) 0.004(4) C10 0.035(4) 0.034(4) 0.035(4) 0.004(3) 0.006(3) 0.004(3) C11 0.049(6) 0.073(7) 0.060(7) 0.000(5) 0.012(5) 0.009(5) C12 0.038(4) 0.036(4) 0.032(4) 0.004(3) 0.003(3) 0.004(3) C13 0.037(4) 0.064(5) 0.037(5) 0.009(4) 0.001(4) 0.009(4) C14 0.029(4) 0.039(5) 0.032(5) 0.010(4) -0.001(3) -0.004(4) O4 0.069(4) 0.088(5) 0.034(3) -0.005(3) 0.021(3) -0.019(4) O5 0.048(4) 0.064(4) 0.043(4) 0.013(3) -0.013(3) 0.003(3) O6 0.064(4) 0.054(4) 0.041(3) -0.005(3) 0.013(3) 0.016(3) C15 0.042(4) 0.033(4) 0.035(4) 0.001(3) 0.002(3) 0.005(3) C16 0.037(4) 0.047(4) 0.035(4) -0.002(4) -0.002(3) 0.005(4) C17 0.063(6) 0.053(5) 0.032(5) 0.008(4) 0.017(4) 0.005(5) C18 0.058(6) 0.045(5) 0.039(5) 0.015(4) 0.017(4) -0.001(4) C19 0.034(4) 0.037(4) 0.029(4) 0.008(3) 0.002(3) 0.001(3) C20 0.041(4) 0.033(4) 0.032(4) 0.007(3) 0.006(3) 0.000(3) C21 0.032(4) 0.033(4) 0.036(4) 0.002(3) 0.004(3) 0.000(3) C22 0.057(5) 0.029(4) 0.043(5) 0.004(3) 0.032(4) 0.001(3) C23 0.060(6) 0.033(4) 0.056(6) 0.022(4) 0.027(4) 0.005(4) C24 0.034(4) 0.037(4) 0.032(4) 0.003(3) 0.006(3) 0.005(3) C25 0.066(7) 0.051(6) 0.057(6) -0.018(5) 0.019(5) 0.009(5) C26 0.032(4) 0.039(4) 0.033(4) 0.004(3) -0.001(3) 0.008(3) C27 0.059(5) 0.035(4) 0.047(5) 0.001(4) -0.002(4) 0.016(4) C28 0.034(4) 0.033(4) 0.045(5) 0.001(4) 0.001(4) 0.001(4) O7 0.051(4) 0.071(4) 0.041(4) 0.008(3) 0.004(3) -0.006(3) O8 0.037(3) 0.077(4) 0.043(4) 0.018(3) -0.008(3) -0.001(3) O9 0.067(4) 0.058(4) 0.039(3) -0.005(3) 0.010(3) 0.020(3) C29 0.036(4) 0.037(4) 0.045(5) 0.001(3) 0.012(3) -0.002(3) C30 0.047(4) 0.044(5) 0.032(4) 0.002(3) 0.003(3) 0.012(4) C31 0.052(5) 0.064(6) 0.025(4) 0.001(4) 0.006(4) 0.011(5) C32 0.047(5) 0.051(5) 0.039(5) 0.013(4) 0.009(4) 0.005(4) C33 0.034(4) 0.041(4) 0.035(4) 0.004(3) 0.002(3) -0.001(3) C34 0.042(5) 0.033(4) 0.041(5) 0.011(3) 0.012(4) 0.005(4) C35 0.030(4) 0.036(4) 0.036(4) 0.004(3) -0.004(3) 0.003(3) C36 0.040(4) 0.043(4) 0.033(4) 0.002(3) 0.009(3) -0.001(3) C37 0.049(5) 0.031(4) 0.055(5) 0.005(4) 0.022(4) 0.006(4) C38 0.032(4) 0.036(4) 0.036(4) 0.006(3) 0.003(3) 0.002(3) C39 0.077(8) 0.052(6) 0.061(7) -0.020(5) 0.015(6) 0.007(5) C40 0.030(4) 0.037(4) 0.030(4) 0.005(3) -0.005(3) 0.002(3) C41 0.059(5) 0.040(4) 0.041(5) 0.009(4) -0.004(4) 0.011(4) C42 0.037(5) 0.035(5) 0.028(5) 0.007(3) 0.000(4) 0.002(4) O10 0.100(6) 0.065(4) 0.030(3) -0.006(3) 0.016(3) -0.029(4) O11 0.055(4) 0.055(4) 0.042(3) 0.024(3) 0.002(3) 0.008(3) O12 0.058(4) 0.060(4) 0.037(3) 0.001(3) 0.011(3) 0.013(3) C43 0.038(4) 0.043(4) 0.036(4) 0.003(3) 0.008(3) 0.000(3) C44 0.042(4) 0.045(4) 0.033(4) 0.011(3) 0.008(3) 0.015(4) C45 0.041(5) 0.058(5) 0.031(5) -0.001(4) -0.005(4) -0.002(4) C46 0.039(5) 0.060(6) 0.031(5) -0.006(4) -0.003(4) -0.003(4) C47 0.036(4) 0.038(4) 0.025(4) 0.003(3) -0.001(3) 0.004(3) C48 0.028(4) 0.044(5) 0.030(4) 0.004(3) -0.005(3) -0.008(3) C49 0.033(4) 0.033(4) 0.033(4) 0.009(3) 0.005(3) 0.000(3) C50 0.029(4) 0.049(5) 0.049(5) -0.016(4) 0.011(3) -0.003(3) C51 0.026(4) 0.054(5) 0.047(5) -0.015(4) -0.005(3) -0.014(4) C52 0.031(4) 0.038(4) 0.036(4) 0.000(3) 0.002(3) 0.000(3) C53 0.049(6) 0.056(6) 0.068(7) 0.004(5) 0.027(5) 0.015(5) C54 0.034(4) 0.036(4) 0.028(4) 0.008(3) 0.007(3) 0.011(3) C55 0.033(4) 0.066(5) 0.044(5) 0.013(4) 0.006(4) 0.015(4) C56 0.029(4) 0.052(5) 0.033(5) 0.005(4) -0.001(3) -0.011(4) Ni1 0.0253(5) 0.0268(5) 0.0269(4) 0.0017(4) 0.0032(4) 0.0068(4) O1W 0.072(4) 0.065(4) 0.042(4) -0.004(3) 0.004(3) 0.044(3) O2W 0.095(6) 0.076(5) 0.086(6) -0.013(5) -0.013(5) 0.002(5) O3W 0.101(6) 0.085(5) 0.079(6) 0.035(5) 0.043(5) 0.032(5) O4W 0.045(3) 0.077(4) 0.039(4) 0.019(3) 0.005(3) 0.007(3) O5W 0.052(3) 0.050(3) 0.036(3) 0.000(3) -0.006(3) 0.011(3) O6W 0.078(4) 0.073(4) 0.039(4) 0.003(3) 0.008(3) 0.046(4) Ni2 0.0293(5) 0.0290(5) 0.0282(4) 0.0025(4) 0.0040(4) 0.0091(4) O7W 0.057(4) 0.074(5) 0.079(5) 0.015(4) 0.004(4) 0.007(4) O8W 0.059(4) 0.070(5) 0.084(6) 0.014(4) 0.000(4) -0.003(4) O9W 0.087(5) 0.108(6) 0.047(5) 0.001(4) 0.009(4) 0.044(5) O10W 0.103(6) 0.088(6) 0.066(6) 0.007(4) 0.007(5) 0.028(5) O11W 0.063(4) 0.037(3) 0.047(4) 0.007(3) -0.009(3) 0.011(3) O12W 0.046(3) 0.065(4) 0.044(4) 0.014(3) 0.003(3) 0.013(3) O13W 0.090(6) 0.033(3) 0.116(7) -0.008(4) 0.054(5) -0.006(3) O14W 0.040(3) 0.073(5) 0.114(6) -0.041(4) 0.032(4) -0.006(3) O15W 0.073(4) 0.034(3) 0.096(5) -0.005(3) 0.041(4) 0.005(3) O16W 0.048(4) 0.049(3) 0.097(5) -0.015(4) 0.028(3) -0.007(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 O1 C14 1.217(10) . ? O2 C14 1.248(10) . ? O3 C2 1.344(9) . ? O3 C11 1.394(12) . ? C1 C2 1.378(10) . ? C1 C10 1.398(10) . ? C1 H1A 0.9300 . ? C2 C3 1.435(13) . ? C3 C4 1.350(14) . ? C3 H3A 0.9300 . ? C4 C5 1.420(11) . ? C4 H4A 0.9300 . ? C5 C6 1.400(12) . ? C5 C10 1.437(10) . ? C6 C7 1.358(11) . ? C6 H6A 0.9300 . ? C7 C8 1.424(10) . ? C7 C12 1.535(10) . ? C8 C9 1.355(11) . ? C8 H8A 0.9300 . ? C9 C10 1.424(11) . ? C9 H9A 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.533(11) . ? C12 C13 1.539(10) . ? C12 H12A 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? O4 C28 1.243(11) . ? O5 C28 1.275(10) . ? O6 C16 1.370(10) . ? O6 C25 1.403(13) . ? C15 C16 1.375(11) . ? C15 C24 1.413(10) . ? C15 H15A 0.9300 . ? C16 C17 1.423(13) . ? C17 C18 1.354(14) . ? C17 H17A 0.9300 . ? C18 C19 1.412(11) . ? C18 H18A 0.9300 . ? C19 C20 1.412(11) . ? C19 C24 1.428(10) . ? C20 C21 1.383(11) . ? C20 H20A 0.9300 . ? C21 C22 1.399(10) . ? C21 C26 1.506(10) . ? C22 C23 1.387(11) . ? C22 H22A 0.9300 . ? C23 C24 1.400(11) . ? C23 H23A 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.511(11) . ? C26 C28 1.526(12) . ? C26 H26A 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? O7 C42 1.278(10) . ? O8 C42 1.224(10) . ? O9 C30 1.372(9) . ? O9 C39 1.416(13) . ? C29 C30 1.360(11) . ? C29 C38 1.427(10) . ? C29 H29A 0.9300 . ? C30 C31 1.393(13) . ? C31 C32 1.355(14) . ? C31 H31A 0.9300 . ? C32 C33 1.418(12) . ? C32 H32A 0.9300 . ? C33 C34 1.411(12) . ? C33 C38 1.412(10) . ? C34 C35 1.363(11) . ? C34 H34A 0.9300 . ? C35 C36 1.406(10) . ? C35 C40 1.541(10) . ? C36 C37 1.370(11) . ? C36 H36A 0.9300 . ? C37 C38 1.418(11) . ? C37 H37A 0.9300 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C42 1.491(11) . ? C40 C41 1.535(10) . ? C40 H40A 0.9800 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? O10 C56 1.264(11) . ? O11 C56 1.228(11) . ? O12 C53 1.373(12) . ? O12 C44 1.388(9) . ? C43 C44 1.374(11) . ? C43 C52 1.413(11) . ? C43 H43A 0.9300 . ? C44 C45 1.405(12) . ? C45 C46 1.372(14) . ? C45 H45A 0.9300 . ? C46 C47 1.407(11) . ? C46 H46A 0.9300 . ? C47 C52 1.414(10) . ? C47 C48 1.416(12) . ? C48 C49 1.366(11) . ? C48 H48A 0.9300 . ? C49 C50 1.402(10) . ? C49 C54 1.522(10) . ? C50 C51 1.370(11) . ? C50 H50A 0.9300 . ? C51 C52 1.416(10) . ? C51 H51A 0.9300 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C55 1.508(10) . ? C54 C56 1.547(11) . ? C54 H54A 0.9800 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? Ni1 O6W 2.056(7) . ? Ni1 O1W 2.061(6) . ? Ni1 O3W 2.099(8) . ? Ni1 O2W 2.108(8) . ? Ni1 O4W 2.122(6) . ? Ni1 O5W 2.122(6) . ? O1W H1 0.8500 . ? O1W H2 0.8501 . ? O2W H3 0.8501 . ? O2W H4 0.8500 . ? O3W H5 0.8500 . ? O3W H6 0.8499 . ? O4W H7 0.8500 . ? O4W H8 0.8500 . ? O5W H9 0.8501 . ? O5W H10 0.8501 . ? O6W H11 0.8500 . ? O6W H12 0.8500 . ? Ni2 O10W 2.094(8) . ? Ni2 O12W 2.097(6) . ? Ni2 O9W 2.104(7) . ? Ni2 O11W 2.104(6) . ? Ni2 O7W 2.107(8) . ? Ni2 O8W 2.108(8) . ? O7W H13 0.8501 . ? O7W H14 0.8500 . ? O8W H15 0.8499 . ? O8W H16 0.8501 . ? O9W H17 0.8501 . ? O9W H18 0.8499 . ? O10W H19 0.8500 . ? O10W H20 0.8500 . ? O11W H21 0.8500 . ? O11W H22 0.8500 . ? O12W H23 0.8500 . ? O12W H24 0.8501 . ? O13W H25 0.8500 . ? O13W H26 0.8501 . ? O14W H27 0.8500 . ? O14W H28 0.8500 . ? O15W H29 0.8500 . ? O15W H30 0.8500 . ? O16W H31 0.8500 . ? O16W H32 0.8501 . ? 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 C2 O3 C11 118.1(7) . . ? C2 C1 C10 121.1(7) . . ? C2 C1 H1A 119.5 . . ? C10 C1 H1A 119.5 . . ? O3 C2 C1 126.2(8) . . ? O3 C2 C3 115.2(7) . . ? C1 C2 C3 118.5(8) . . ? C4 C3 C2 121.5(8) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 121.0(9) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C6 C5 C4 122.6(8) . . ? C6 C5 C10 119.7(7) . . ? C4 C5 C10 117.7(7) . . ? C7 C6 C5 122.1(7) . . ? C7 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? C6 C7 C8 118.8(7) . . ? C6 C7 C12 124.2(7) . . ? C8 C7 C12 117.0(6) . . ? C9 C8 C7 120.8(7) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 121.8(7) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C1 C10 C9 123.0(7) . . ? C1 C10 C5 120.2(7) . . ? C9 C10 C5 116.7(7) . . ? O3 C11 H11A 109.5 . . ? O3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C7 108.2(6) . . ? C14 C12 C13 108.6(6) . . ? C7 C12 C13 114.1(6) . . ? C14 C12 H12A 108.6 . . ? C7 C12 H12A 108.6 . . ? C13 C12 H12A 108.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O1 C14 O2 124.0(8) . . ? O1 C14 C12 118.3(8) . . ? O2 C14 C12 117.6(7) . . ? C16 O6 C25 118.1(7) . . ? C16 C15 C24 119.9(7) . . ? C16 C15 H15A 120.1 . . ? C24 C15 H15A 120.1 . . ? O6 C16 C15 125.6(8) . . ? O6 C16 C17 114.4(8) . . ? C15 C16 C17 120.0(8) . . ? C18 C17 C16 120.2(8) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 122.3(8) . . ? C17 C18 H18A 118.9 . . ? C19 C18 H18A 118.9 . . ? C18 C19 C20 123.2(7) . . ? C18 C19 C24 117.1(7) . . ? C20 C19 C24 119.6(7) . . ? C21 C20 C19 121.6(7) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C20 C21 C22 118.3(7) . . ? C20 C21 C26 122.5(7) . . ? C22 C21 C26 119.2(6) . . ? C23 C22 C21 121.6(7) . . ? C23 C22 H22A 119.2 . . ? C21 C22 H22A 119.2 . . ? C22 C23 C24 121.1(7) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? C23 C24 C15 121.6(7) . . ? C23 C24 C19 117.9(7) . . ? C15 C24 C19 120.5(7) . . ? O6 C25 H25A 109.5 . . ? O6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 C27 115.1(6) . . ? C21 C26 C28 111.6(6) . . ? C27 C26 C28 107.9(6) . . ? C21 C26 H26A 107.3 . . ? C27 C26 H26A 107.3 . . ? C28 C26 H26A 107.3 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O4 C28 O5 122.5(9) . . ? O4 C28 C26 120.8(8) . . ? O5 C28 C26 116.7(8) . . ? C30 O9 C39 117.4(7) . . ? C30 C29 C38 119.5(7) . . ? C30 C29 H29A 120.3 . . ? C38 C29 H29A 120.3 . . ? C29 C30 O9 124.9(7) . . ? C29 C30 C31 120.3(8) . . ? O9 C30 C31 114.8(7) . . ? C32 C31 C30 121.9(9) . . ? C32 C31 H31A 119.1 . . ? C30 C31 H31A 119.1 . . ? C31 C32 C33 120.0(9) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C38 119.3(7) . . ? C34 C33 C32 122.4(8) . . ? C38 C33 C32 118.3(8) . . ? C35 C34 C33 121.6(8) . . ? C35 C34 H34A 119.2 . . ? C33 C34 H34A 119.2 . . ? C34 C35 C36 119.6(7) . . ? C34 C35 C40 123.5(7) . . ? C36 C35 C40 116.9(7) . . ? C37 C36 C35 120.0(7) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 121.5(7) . . ? C36 C37 H37A 119.2 . . ? C38 C37 H37A 119.2 . . ? C33 C38 C37 117.9(7) . . ? C33 C38 C29 119.9(7) . . ? C37 C38 C29 122.1(7) . . ? O9 C39 H39A 109.5 . . ? O9 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O9 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C40 C41 109.3(6) . . ? C42 C40 C35 107.8(6) . . ? C41 C40 C35 114.4(6) . . ? C42 C40 H40A 108.4 . . ? C41 C40 H40A 108.4 . . ? C35 C40 H40A 108.4 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O8 C42 O7 121.0(8) . . ? O8 C42 C40 119.9(8) . . ? O7 C42 C40 119.0(8) . . ? C53 O12 C44 118.7(7) . . ? C44 C43 C52 118.5(7) . . ? C44 C43 H43A 120.8 . . ? C52 C43 H43A 120.8 . . ? C43 C44 O12 124.9(7) . . ? C43 C44 C45 121.0(8) . . ? O12 C44 C45 114.1(7) . . ? C46 C45 C44 120.5(8) . . ? C46 C45 H45A 119.8 . . ? C44 C45 H45A 119.8 . . ? C45 C46 C47 120.7(8) . . ? C45 C46 H46A 119.6 . . ? C47 C46 H46A 119.6 . . ? C46 C47 C52 117.9(7) . . ? C46 C47 C48 122.3(7) . . ? C52 C47 C48 119.8(7) . . ? C49 C48 C47 121.6(7) . . ? C49 C48 H48A 119.2 . . ? C47 C48 H48A 119.2 . . ? C48 C49 C50 118.8(7) . . ? C48 C49 C54 123.3(7) . . ? C50 C49 C54 117.8(6) . . ? C51 C50 C49 121.0(7) . . ? C51 C50 H50A 119.5 . . ? C49 C50 H50A 119.5 . . ? C50 C51 C52 121.7(7) . . ? C50 C51 H51A 119.2 . . ? C52 C51 H51A 119.2 . . ? C43 C52 C47 121.4(7) . . ? C43 C52 C51 121.4(7) . . ? C47 C52 C51 117.2(7) . . ? O12 C53 H53A 109.5 . . ? O12 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O12 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C49 114.2(6) . . ? C55 C54 C56 108.2(6) . . ? C49 C54 C56 110.2(6) . . ? C55 C54 H54A 108.0 . . ? C49 C54 H54A 108.0 . . ? C56 C54 H54A 108.0 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O11 C56 O10 124.2(9) . . ? O11 C56 C54 118.0(8) . . ? O10 C56 C54 117.7(8) . . ? O6W Ni1 O1W 171.9(3) . . ? O6W Ni1 O3W 92.0(3) . . ? O1W Ni1 O3W 93.5(3) . . ? O6W Ni1 O2W 93.0(3) . . ? O1W Ni1 O2W 92.8(3) . . ? O3W Ni1 O2W 90.7(4) . . ? O6W Ni1 O4W 88.8(3) . . ? O1W Ni1 O4W 85.6(3) . . ? O3W Ni1 O4W 178.7(4) . . ? O2W Ni1 O4W 90.3(3) . . ? O6W Ni1 O5W 85.3(3) . . ? O1W Ni1 O5W 88.6(3) . . ? O3W Ni1 O5W 91.3(3) . . ? O2W Ni1 O5W 177.5(4) . . ? O4W Ni1 O5W 87.7(2) . . ? Ni1 O1W H1 118.7 . . ? Ni1 O1W H2 133.3 . . ? H1 O1W H2 107.7 . . ? Ni1 O2W H3 139.8 . . ? Ni1 O2W H4 112.5 . . ? H3 O2W H4 107.7 . . ? Ni1 O3W H5 144.3 . . ? Ni1 O3W H6 102.2 . . ? H5 O3W H6 107.7 . . ? Ni1 O4W H7 104.9 . . ? Ni1 O4W H8 147.5 . . ? H7 O4W H8 107.6 . . ? Ni1 O5W H9 105.7 . . ? Ni1 O5W H10 146.4 . . ? H9 O5W H10 107.6 . . ? Ni1 O6W H11 126.2 . . ? Ni1 O6W H12 126.0 . . ? H11 O6W H12 107.6 . . ? O10W Ni2 O12W 91.3(3) . . ? O10W Ni2 O9W 174.7(4) . . ? O12W Ni2 O9W 84.8(3) . . ? O10W Ni2 O11W 84.6(3) . . ? O12W Ni2 O11W 88.0(2) . . ? O9W Ni2 O11W 91.6(3) . . ? O10W Ni2 O7W 91.3(3) . . ? O12W Ni2 O7W 177.3(4) . . ? O9W Ni2 O7W 92.6(3) . . ? O11W Ni2 O7W 91.5(3) . . ? O10W Ni2 O8W 92.8(3) . . ? O12W Ni2 O8W 92.2(3) . . ? O9W Ni2 O8W 91.0(3) . . ? O11W Ni2 O8W 177.4(4) . . ? O7W Ni2 O8W 88.4(3) . . ? Ni2 O7W H13 122.9 . . ? Ni2 O7W H14 125.8 . . ? H13 O7W H14 107.7 . . ? Ni2 O8W H15 137.5 . . ? Ni2 O8W H16 114.8 . . ? H15 O8W H16 107.7 . . ? Ni2 O9W H17 129.0 . . ? Ni2 O9W H18 121.9 . . ? H17 O9W H18 107.6 . . ? Ni2 O10W H19 135.8 . . ? Ni2 O10W H20 112.8 . . ? H19 O10W H20 107.6 . . ? Ni2 O11W H21 142.3 . . ? Ni2 O11W H22 107.3 . . ? H21 O11W H22 107.7 . . ? Ni2 O12W H23 128.5 . . ? Ni2 O12W H24 123.8 . . ? H23 O12W H24 107.7 . . ? H25 O13W H26 107.7 . . ? H27 O14W H28 107.6 . . ? H29 O15W H30 107.5 . . ? H31 O16W H32 107.2 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.419 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.167 #======================================= data_compound_4 #TrackingRef '- naproxen_ni_cu_zn_cd_cd_r3.cif' _database_code_depnum_ccdc_archive 'CCDC 728948' _audit_creation_method SHELXL-97 _chemical_absolute_configuration rm _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H30 Cd O8, H2 O' _chemical_formula_sum 'C28 H32 Cd O9' _chemical_formula_weight 624.95 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 28.998(12) _cell_length_b 5.760(2) _cell_length_c 8.162(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.364(5) _cell_angle_gamma 90.00 _cell_volume 1362.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1978 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 22.31 _exptl_crystal_description bar _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_process_details SADABS(Sheldrick,1996) _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5939 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 27.73 _reflns_number_total 3076 _reflns_number_gt 2761 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(4) _refine_ls_number_reflns 3076 _refine_ls_number_parameters 173 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0984 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Cd1 Cd 0.5000 -0.44841(2) 0.0000 0.03755(15) Uani 1 2 d S . . O1 O 0.54624(14) -0.1271(7) 0.0902(5) 0.0558(10) Uani 1 1 d . . . O1W O 0.45114(17) -0.6938(10) 0.1256(6) 0.0766(14) Uani 1 1 d . . . H1WA H 0.4601 -0.7397 0.2206 0.092 Uiso 1 1 d R . . H1WB H 0.4461 -0.8030 0.0570 0.092 Uiso 1 1 d R . . O2W O 0.5000 -0.6736(12) 0.5000 0.0734(19) Uani 1 2 d S . . H2WA H 0.4794 -0.5969 0.5477 0.088 Uiso 1 1 d R . . O2 O 0.54119(14) -0.4149(12) 0.2625(5) 0.0620(15) Uani 1 1 d . . . O3 O 0.84559(9) 0.0467(17) 0.1910(4) 0.0491(8) Uani 1 1 d . . . C1 C 0.76433(18) 0.1497(9) 0.1753(6) 0.0405(11) Uani 1 1 d . . . H1A H 0.7698 0.2816 0.1134 0.049 Uiso 1 1 calc R . . C2 C 0.79992(16) 0.0064(10) 0.2245(6) 0.0381(16) Uani 1 1 d . . . C3 C 0.79151(17) -0.1978(9) 0.3142(6) 0.0406(11) Uani 1 1 d . . . H3A H 0.8161 -0.2934 0.3467 0.049 Uiso 1 1 calc R . . C4 C 0.74780(17) -0.2565(8) 0.3536(6) 0.0379(11) Uani 1 1 d . . . H4A H 0.7427 -0.3933 0.4106 0.045 Uiso 1 1 calc R . . C5 C 0.71012(16) -0.1109(8) 0.3086(6) 0.0345(10) Uani 1 1 d . . . C6 C 0.66385(16) -0.1605(9) 0.3532(6) 0.0370(11) Uani 1 1 d . . . H6A H 0.6581 -0.2961 0.4107 0.044 Uiso 1 1 calc R . . C7 C 0.62829(16) -0.0156(8) 0.3140(6) 0.0341(11) Uani 1 1 d . . . C8 C 0.63732(18) 0.1901(9) 0.2258(8) 0.0443(13) Uani 1 1 d . . . H8A H 0.6132 0.2916 0.1990 0.053 Uiso 1 1 calc R . . C9 C 0.68134(18) 0.2421(9) 0.1789(7) 0.0466(13) Uani 1 1 d . . . H9A H 0.6865 0.3764 0.1193 0.056 Uiso 1 1 calc R . . C10 C 0.71827(16) 0.0932(10) 0.2208(6) 0.0375(15) Uani 1 1 d . . . C11 C 0.57847(18) -0.0629(10) 0.3606(6) 0.0428(12) Uani 1 1 d . . . H11A H 0.5627 0.0877 0.3584 0.051 Uiso 1 1 calc R . . C12 C 0.5752(2) -0.1556(15) 0.5334(7) 0.0633(18) Uani 1 1 d . . . H12A H 0.5433 -0.1801 0.5565 0.095 Uiso 1 1 calc R . . H12B H 0.5885 -0.0453 0.6099 0.095 Uiso 1 1 calc R . . H12C H 0.5916 -0.2999 0.5433 0.095 Uiso 1 1 calc R . . C13 C 0.55415(15) -0.2107(9) 0.2301(6) 0.0364(10) Uani 1 1 d . . . C14 C 0.8550(2) 0.2521(12) 0.1028(8) 0.0562(15) Uani 1 1 d . . . H14A H 0.8875 0.2615 0.0853 0.084 Uiso 1 1 calc R . . H14B H 0.8456 0.3847 0.1644 0.084 Uiso 1 1 calc R . . H14C H 0.8383 0.2491 -0.0012 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0408(3) 0.0371(2) 0.0343(2) 0.000 -0.00343(16) 0.000 O1 0.064(3) 0.056(2) 0.046(2) 0.0058(19) -0.0185(19) -0.009(2) O1W 0.093(3) 0.072(3) 0.064(3) 0.005(3) 0.000(3) -0.013(3) O2W 0.091(5) 0.052(4) 0.080(5) 0.000 0.039(4) 0.000 O2 0.083(3) 0.057(4) 0.0464(19) 0.001(2) -0.0019(17) -0.032(3) O3 0.0329(15) 0.0604(19) 0.0542(19) 0.016(4) 0.0042(13) -0.001(4) C1 0.047(3) 0.035(2) 0.039(3) 0.004(2) -0.004(2) -0.002(2) C2 0.039(2) 0.043(5) 0.033(2) -0.005(2) -0.0013(17) 0.002(2) C3 0.034(3) 0.040(3) 0.048(3) -0.001(2) -0.004(2) 0.008(2) C4 0.041(3) 0.030(2) 0.042(3) 0.002(2) -0.004(2) 0.006(2) C5 0.038(3) 0.031(2) 0.034(3) 0.002(2) -0.004(2) -0.0016(19) C6 0.033(3) 0.033(2) 0.044(3) -0.003(2) -0.003(2) -0.0021(19) C7 0.031(2) 0.035(3) 0.036(3) -0.0122(18) -0.0040(19) 0.0015(16) C8 0.035(3) 0.036(3) 0.061(4) 0.000(3) -0.010(3) 0.005(2) C9 0.050(3) 0.035(3) 0.054(3) 0.009(2) -0.010(3) 0.001(2) C10 0.036(2) 0.040(5) 0.036(2) -0.002(2) -0.0051(18) -0.004(2) C11 0.042(3) 0.047(3) 0.040(3) -0.008(2) 0.000(2) -0.002(2) C12 0.040(3) 0.106(6) 0.044(3) -0.012(3) 0.003(3) -0.013(3) C13 0.019(2) 0.047(3) 0.044(3) -0.001(2) 0.0000(19) 0.0059(19) C14 0.048(3) 0.065(4) 0.056(4) -0.004(3) 0.007(3) -0.013(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 Cd1 O1W 2.275(5) 2_655 ? Cd1 O1W 2.275(5) . ? Cd1 O1 2.384(4) . ? Cd1 O1 2.384(4) 2_655 ? Cd1 O2 2.417(4) . ? Cd1 O2 2.417(4) 2_655 ? O1 C13 1.252(6) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8499 . ? O2 C13 1.266(8) . ? O3 C2 1.382(6) . ? O3 C14 1.418(11) . ? C1 C2 1.368(7) . ? C1 C10 1.438(7) . ? C1 H1A 0.9300 . ? C2 C3 1.413(8) . ? C3 C4 1.363(7) . ? C3 H3A 0.9300 . ? C4 C5 1.414(6) . ? C4 H4A 0.9300 . ? C5 C10 1.402(7) . ? C5 C6 1.434(7) . ? C6 C7 1.355(7) . ? C6 H6A 0.9300 . ? C7 C8 1.417(7) . ? C7 C11 1.533(7) . ? C8 C9 1.380(8) . ? C8 H8A 0.9300 . ? C9 C10 1.403(7) . ? C9 H9A 0.9300 . ? C11 C13 1.515(7) . ? C11 C12 1.515(8) . ? C11 H11A 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 O1W Cd1 O1W 103.2(3) 2_655 . ? O1W Cd1 O1 105.59(18) 2_655 . ? O1W Cd1 O1 134.11(17) . . ? O1W Cd1 O1 134.11(17) 2_655 2_655 ? O1W Cd1 O1 105.59(18) . 2_655 ? O1 Cd1 O1 78.1(2) . 2_655 ? O1W Cd1 O2 98.90(19) 2_655 . ? O1W Cd1 O2 86.82(18) . . ? O1 Cd1 O2 54.08(17) . . ? O1 Cd1 O2 117.57(18) 2_655 . ? O1W Cd1 O2 86.82(18) 2_655 2_655 ? O1W Cd1 O2 98.90(19) . 2_655 ? O1 Cd1 O2 117.57(18) . 2_655 ? O1 Cd1 O2 54.08(17) 2_655 2_655 ? O2 Cd1 O2 170.8(3) . 2_655 ? C13 O1 Cd1 93.6(3) . . ? Cd1 O1W H1WA 115.5 . . ? Cd1 O1W H1WB 104.9 . . ? H1WA O1W H1WB 114.1 . . ? C13 O2 Cd1 91.7(3) . . ? C2 O3 C14 116.5(6) . . ? C2 C1 C10 119.0(5) . . ? C2 C1 H1A 120.5 . . ? C10 C1 H1A 120.5 . . ? C1 C2 O3 123.9(6) . . ? C1 C2 C3 120.7(5) . . ? O3 C2 C3 115.4(5) . . ? C4 C3 C2 120.7(5) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 120.5(5) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C10 C5 C4 119.0(4) . . ? C10 C5 C6 118.5(5) . . ? C4 C5 C6 122.5(5) . . ? C7 C6 C5 121.9(5) . . ? C7 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C6 C7 C8 118.7(5) . . ? C6 C7 C11 123.2(5) . . ? C8 C7 C11 118.1(4) . . ? C9 C8 C7 121.0(5) . . ? C9 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C8 C9 C10 120.4(5) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C5 C10 C9 119.6(5) . . ? C5 C10 C1 120.0(5) . . ? C9 C10 C1 120.4(5) . . ? C13 C11 C12 114.3(5) . . ? C13 C11 C7 110.0(4) . . ? C12 C11 C7 112.9(4) . . ? C13 C11 H11A 106.3 . . ? C12 C11 H11A 106.3 . . ? C7 C11 H11A 106.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C13 O2 120.2(5) . . ? O1 C13 C11 119.2(5) . . ? O2 C13 C11 120.6(5) . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.73 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.959 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.089