data_fn02b2_a _audit_creation_date 2014-09-12 _audit_creation_method ; Olex2 1.2 (compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862) ; _shelxl_version_number 2014/6 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C28 H17 O5 P W' _chemical_formula_sum 'C28 H17 O5 P W' _chemical_formula_weight 648.23 _chemical_melting_point ? 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1311(4) _cell_length_b 19.9977(7) _cell_length_c 11.6468(4) _cell_angle_alpha 90 _cell_angle_beta 109.4260(11) _cell_angle_gamma 90 _cell_volume 2444.95(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9743 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.350 _cell_measurement_theta_min 2.813 _shelx_estimated_absorpt_T_max 0.910 _shelx_estimated_absorpt_T_min 0.512 _exptl_absorpt_coefficient_mu 4.827 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6427 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing, 1995' _exptl_absorpt_special_details ? _exptl_crystal_colour 'yellow' _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_unetI/netI 0.0234 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 34007 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 28.351 _diffrn_reflns_theta_min 2.191 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5320 _reflns_number_total 6093 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _refine_diff_density_max 1.798 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.097 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 316 _refine_ls_number_reflns 6093 _refine_ls_number_restraints 288 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0207 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0174P)^2^+2.3527P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0439 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.77043(2) 0.24188(2) 0.24700(2) 0.01590(3) Uani 1 1 d . . . . . P1 P 0.74349(6) 0.31585(3) 0.41034(5) 0.01558(12) Uani 1 1 d . . . . . O1 O 0.6806(2) 0.36553(12) 0.0659(2) 0.0481(6) Uani 1 1 d . . . . . O2 O 1.06603(19) 0.26624(10) 0.2958(2) 0.0369(5) Uani 1 1 d . . . . . O3 O 0.8696(2) 0.11586(10) 0.41738(18) 0.0366(5) Uani 1 1 d . . . . . O4 O 0.4817(2) 0.19477(13) 0.1812(2) 0.0495(6) Uani 1 1 d . . . . . O5 O 0.78345(19) 0.15025(10) 0.03173(17) 0.0327(5) Uani 1 1 d . . . . . C1 C 0.7810(2) 0.40010(12) 0.4352(2) 0.0169(5) Uani 1 1 d . . . . . C2 C 0.7386(2) 0.43829(12) 0.5138(2) 0.0175(5) Uani 1 1 d . . . . . H2 H 0.7617 0.4842 0.5217 0.021 Uiso 1 1 calc R . . . . C3 C 0.6648(2) 0.41518(11) 0.5826(2) 0.0164(5) Uani 1 1 d . . . . . C4 C 0.6254(2) 0.34886(12) 0.5751(2) 0.0169(5) Uani 1 1 d . . . . . H4 H 0.5756 0.3359 0.6236 0.020 Uiso 1 1 calc R . . . . C5 C 0.6525(2) 0.29974(12) 0.5024(2) 0.0165(5) Uani 1 1 d . . . . . C6 C 0.5946(2) 0.23220(12) 0.4994(2) 0.0177(5) Uani 1 1 d . . . . . C7 C 0.4632(2) 0.22539(13) 0.4491(2) 0.0244(5) Uani 1 1 d . . . . . H7 H 0.4120 0.2633 0.4159 0.029 Uiso 1 1 calc R . . . . C8 C 0.4063(3) 0.16311(14) 0.4472(3) 0.0297(6) Uani 1 1 d . . . . . H8 H 0.3165 0.1586 0.4121 0.036 Uiso 1 1 calc R . . . . C9 C 0.4805(3) 0.10792(14) 0.4964(2) 0.0309(6) Uani 1 1 d . . . . . H9 H 0.4417 0.0656 0.4957 0.037 Uiso 1 1 calc R . . . . C10 C 0.6109(3) 0.11453(13) 0.5464(3) 0.0289(6) Uani 1 1 d . . . . . H10 H 0.6618 0.0766 0.5801 0.035 Uiso 1 1 calc R . . . . C11 C 0.6684(3) 0.17615(12) 0.5480(2) 0.0234(5) Uani 1 1 d . . . . . H11 H 0.7583 0.1802 0.5823 0.028 Uiso 1 1 calc R . . . . C12 C 0.8608(2) 0.43269(12) 0.3711(2) 0.0178(5) Uani 1 1 d . . . . . C13 C 0.9805(2) 0.40721(12) 0.3823(2) 0.0185(5) Uani 1 1 d . . . . . H13 H 1.0114 0.3690 0.4317 0.022 Uiso 1 1 calc R . . . . C14 C 1.0553(2) 0.43707(12) 0.3223(2) 0.0219(5) Uani 1 1 d . . . . . H14 H 1.1360 0.4187 0.3289 0.026 Uiso 1 1 calc R . . . . C15 C 1.0118(3) 0.49383(13) 0.2527(2) 0.0250(6) Uani 1 1 d . . . . . H15 H 1.0632 0.5148 0.2124 0.030 Uiso 1 1 calc R . . . . C16 C 0.8938(3) 0.51998(13) 0.2418(3) 0.0275(6) Uani 1 1 d . . . . . H16 H 0.8645 0.5590 0.1942 0.033 Uiso 1 1 calc R . . . . C17 C 0.8174(3) 0.48945(12) 0.3002(3) 0.0246(6) Uani 1 1 d . . . . . H17 H 0.7358 0.5074 0.2917 0.030 Uiso 1 1 calc R . . . . C18 C 0.6271(2) 0.46308(12) 0.6626(2) 0.0171(5) Uani 1 1 d . . . . . C19 C 0.6082(2) 0.53075(12) 0.6314(2) 0.0194(5) Uani 1 1 d . . . . . H19 H 0.6216 0.5464 0.5595 0.023 Uiso 1 1 calc R . . . . C20 C 0.5703(2) 0.57550(12) 0.7041(2) 0.0213(5) Uani 1 1 d . . . . . H20 H 0.5573 0.6213 0.6814 0.026 Uiso 1 1 calc R . . . . C21 C 0.5514(2) 0.55338(13) 0.8099(2) 0.0236(5) Uani 1 1 d . . . . . H21 H 0.5250 0.5839 0.8594 0.028 Uiso 1 1 calc R . . . . C22 C 0.5712(2) 0.48678(13) 0.8430(2) 0.0239(5) Uani 1 1 d . . . . . H22 H 0.5595 0.4717 0.9158 0.029 Uiso 1 1 calc R . . . . C23 C 0.6082(2) 0.44200(12) 0.7700(2) 0.0203(5) Uani 1 1 d . . . . . H23 H 0.6209 0.3963 0.7932 0.024 Uiso 1 1 calc R . . . . C24 C 0.7142(3) 0.32170(14) 0.1313(2) 0.0292(6) Uani 1 1 d . . . . . C25 C 0.9596(3) 0.26135(13) 0.2793(2) 0.0235(5) Uani 1 1 d . . . . . C26 C 0.8312(2) 0.16196(13) 0.3593(2) 0.0221(5) Uani 1 1 d . . . . . C27 C 0.5845(3) 0.21281(15) 0.2073(2) 0.0291(6) Uani 1 1 d . . . . . C28 C 0.7780(2) 0.18411(13) 0.1095(2) 0.0231(5) 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 W1 0.01651(5) 0.01913(5) 0.01313(5) -0.00151(4) 0.00638(4) 0.00042(4) P1 0.0163(3) 0.0168(3) 0.0156(3) -0.0007(2) 0.0081(2) -0.0008(2) O1 0.0657(16) 0.0508(14) 0.0388(13) 0.0231(11) 0.0319(12) 0.0323(12) O2 0.0252(11) 0.0402(12) 0.0505(14) -0.0160(10) 0.0197(10) -0.0082(9) O3 0.0467(13) 0.0352(11) 0.0336(12) 0.0098(9) 0.0210(10) 0.0127(9) O4 0.0227(11) 0.0925(19) 0.0327(12) -0.0220(12) 0.0086(9) -0.0148(11) O5 0.0333(11) 0.0408(12) 0.0283(11) -0.0161(9) 0.0158(9) -0.0061(9) C1 0.0160(11) 0.0181(11) 0.0168(11) 0.0009(9) 0.0056(9) -0.0004(9) C2 0.0183(12) 0.0165(11) 0.0174(12) -0.0005(9) 0.0057(10) -0.0006(9) C3 0.0161(11) 0.0195(12) 0.0129(11) -0.0001(9) 0.0037(9) 0.0018(9) C4 0.0146(11) 0.0222(12) 0.0154(12) 0.0008(9) 0.0070(9) -0.0002(9) C5 0.0163(11) 0.0181(11) 0.0163(12) 0.0009(9) 0.0072(9) -0.0007(9) C6 0.0223(12) 0.0194(12) 0.0163(11) -0.0032(9) 0.0130(10) -0.0025(9) C7 0.0234(13) 0.0282(14) 0.0232(14) -0.0031(10) 0.0101(11) -0.0028(10) C8 0.0287(15) 0.0362(15) 0.0272(15) -0.0073(11) 0.0136(12) -0.0138(11) C9 0.0464(17) 0.0254(14) 0.0292(15) -0.0075(11) 0.0235(13) -0.0139(12) C10 0.0422(16) 0.0206(13) 0.0325(15) 0.0008(11) 0.0240(13) -0.0002(11) C11 0.0264(14) 0.0230(13) 0.0258(14) 0.0013(10) 0.0152(11) -0.0002(10) C12 0.0209(12) 0.0179(12) 0.0165(12) -0.0028(9) 0.0088(10) -0.0030(9) C13 0.0225(12) 0.0175(12) 0.0165(12) -0.0006(9) 0.0076(10) -0.0025(9) C14 0.0206(13) 0.0247(13) 0.0225(13) -0.0033(10) 0.0100(10) -0.0027(10) C15 0.0302(14) 0.0258(14) 0.0228(14) -0.0013(10) 0.0140(12) -0.0075(10) C16 0.0347(15) 0.0223(13) 0.0284(15) 0.0061(11) 0.0145(12) 0.0005(11) C17 0.0271(14) 0.0212(13) 0.0288(15) 0.0039(10) 0.0134(12) 0.0022(10) C18 0.0151(12) 0.0200(12) 0.0162(11) -0.0027(9) 0.0052(9) 0.0005(9) C19 0.0198(12) 0.0214(12) 0.0172(12) -0.0014(9) 0.0063(10) -0.0007(9) C20 0.0211(13) 0.0183(12) 0.0219(13) -0.0010(9) 0.0038(10) 0.0017(9) C21 0.0222(13) 0.0285(13) 0.0211(13) -0.0062(10) 0.0084(11) 0.0034(10) C22 0.0254(14) 0.0309(14) 0.0172(13) -0.0009(10) 0.0094(11) 0.0019(10) C23 0.0217(13) 0.0203(12) 0.0208(12) 0.0013(9) 0.0093(10) 0.0023(9) C24 0.0379(16) 0.0317(15) 0.0247(14) 0.0023(11) 0.0195(12) 0.0105(12) C25 0.0252(13) 0.0230(13) 0.0260(13) -0.0066(10) 0.0137(11) -0.0023(10) C26 0.0229(13) 0.0253(13) 0.0204(13) -0.0014(10) 0.0105(10) 0.0011(10) C27 0.0250(14) 0.0444(17) 0.0184(13) -0.0094(12) 0.0077(11) -0.0003(12) C28 0.0192(13) 0.0280(14) 0.0226(13) -0.0015(10) 0.0076(10) -0.0011(10) _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 W1 P1 2.5054(6) . ? W1 C24 2.048(3) . ? W1 C25 2.049(3) . ? W1 C26 2.033(3) . ? W1 C27 2.049(3) . ? W1 C28 1.999(3) . ? P1 C1 1.737(2) . ? P1 C5 1.732(2) . ? O1 C24 1.140(3) . ? O2 C25 1.140(3) . ? O3 C26 1.139(3) . ? O4 C27 1.140(3) . ? O5 C28 1.149(3) . ? C1 C2 1.390(3) . ? C1 C12 1.487(3) . ? C2 C3 1.403(3) . ? C3 C4 1.391(3) . ? C3 C18 1.490(3) . ? C4 C5 1.394(3) . ? C5 C6 1.492(3) . ? C6 C7 1.389(4) . ? C6 C11 1.393(3) . ? C7 C8 1.394(4) . ? C8 C9 1.383(4) . ? C9 C10 1.379(4) . ? C10 C11 1.386(4) . ? C12 C13 1.392(3) . ? C12 C17 1.392(3) . ? C13 C14 1.388(3) . ? C14 C15 1.385(4) . ? C15 C16 1.379(4) . ? C16 C17 1.394(4) . ? C18 C19 1.399(3) . ? C18 C23 1.400(3) . ? C19 C20 1.390(3) . ? C20 C21 1.390(4) . ? C21 C22 1.383(4) . ? C22 C23 1.388(3) . ? 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 C24 W1 P1 87.22(7) . . ? C24 W1 C25 92.49(11) . . ? C24 W1 C27 90.44(12) . . ? C25 W1 P1 97.11(7) . . ? C26 W1 P1 94.23(7) . . ? C26 W1 C24 178.00(10) . . ? C26 W1 C25 85.97(10) . . ? C26 W1 C27 90.98(11) . . ? C27 W1 P1 88.39(7) . . ? C27 W1 C25 173.89(10) . . ? C28 W1 P1 175.65(7) . . ? C28 W1 C24 90.50(11) . . ? C28 W1 C25 86.68(10) . . ? C28 W1 C26 88.14(10) . . ? C28 W1 C27 87.93(10) . . ? C1 P1 W1 128.06(8) . . ? C5 P1 W1 127.04(8) . . ? C5 P1 C1 103.59(11) . . ? C2 C1 P1 121.83(18) . . ? C2 C1 C12 118.7(2) . . ? C12 C1 P1 119.47(17) . . ? C1 C2 C3 125.9(2) . . ? C2 C3 C18 119.0(2) . . ? C4 C3 C2 120.7(2) . . ? C4 C3 C18 120.3(2) . . ? C3 C4 C5 125.7(2) . . ? C4 C5 P1 122.28(18) . . ? C4 C5 C6 118.2(2) . . ? C6 C5 P1 119.39(17) . . ? C7 C6 C5 119.0(2) . . ? C7 C6 C11 119.2(2) . . ? C11 C6 C5 121.8(2) . . ? C6 C7 C8 120.2(3) . . ? C9 C8 C7 120.0(3) . . ? C10 C9 C8 119.9(3) . . ? C9 C10 C11 120.5(3) . . ? C10 C11 C6 120.2(3) . . ? C13 C12 C1 120.4(2) . . ? C17 C12 C1 120.5(2) . . ? C17 C12 C13 119.1(2) . . ? C14 C13 C12 120.7(2) . . ? C15 C14 C13 119.7(2) . . ? C16 C15 C14 120.1(2) . . ? C15 C16 C17 120.4(2) . . ? C12 C17 C16 119.9(2) . . ? C19 C18 C3 120.6(2) . . ? C19 C18 C23 118.0(2) . . ? C23 C18 C3 121.5(2) . . ? C20 C19 C18 121.0(2) . . ? C19 C20 C21 120.1(2) . . ? C22 C21 C20 119.7(2) . . ? C21 C22 C23 120.2(2) . . ? C22 C23 C18 121.1(2) . . ? O1 C24 W1 178.6(3) . . ? O2 C25 W1 173.9(2) . . ? O3 C26 W1 175.5(2) . . ? O4 C27 W1 176.9(2) . . ? O5 C28 W1 179.0(2) . . ? 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 W1 P1 C1 C2 167.13(16) . . . . ? W1 P1 C1 C12 -12.9(2) . . . . ? W1 P1 C5 C4 -168.12(15) . . . . ? W1 P1 C5 C6 8.3(2) . . . . ? P1 C1 C2 C3 1.1(4) . . . . ? P1 C1 C12 C13 -56.1(3) . . . . ? P1 C1 C12 C17 124.6(2) . . . . ? P1 C5 C6 C7 -110.7(2) . . . . ? P1 C5 C6 C11 70.8(3) . . . . ? C1 P1 C5 C4 -0.4(2) . . . . ? C1 P1 C5 C6 176.02(19) . . . . ? C1 C2 C3 C4 -1.0(4) . . . . ? C1 C2 C3 C18 -179.8(2) . . . . ? C1 C12 C13 C14 179.6(2) . . . . ? C1 C12 C17 C16 179.2(2) . . . . ? C2 C1 C12 C13 123.8(3) . . . . ? C2 C1 C12 C17 -55.5(3) . . . . ? C2 C3 C4 C5 0.0(4) . . . . ? C2 C3 C18 C19 30.5(3) . . . . ? C2 C3 C18 C23 -150.1(2) . . . . ? C3 C4 C5 P1 0.7(4) . . . . ? C3 C4 C5 C6 -175.8(2) . . . . ? C3 C18 C19 C20 178.6(2) . . . . ? C3 C18 C23 C22 -179.1(2) . . . . ? C4 C3 C18 C19 -148.4(2) . . . . ? C4 C3 C18 C23 31.0(3) . . . . ? C4 C5 C6 C7 65.9(3) . . . . ? C4 C5 C6 C11 -112.6(3) . . . . ? C5 P1 C1 C2 -0.4(2) . . . . ? C5 P1 C1 C12 179.56(19) . . . . ? C5 C6 C7 C8 -178.7(2) . . . . ? C5 C6 C11 C10 178.3(2) . . . . ? C6 C7 C8 C9 0.5(4) . . . . ? C7 C6 C11 C10 -0.3(4) . . . . ? C7 C8 C9 C10 -0.5(4) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C9 C10 C11 C6 0.3(4) . . . . ? C11 C6 C7 C8 -0.2(4) . . . . ? C12 C1 C2 C3 -178.8(2) . . . . ? C12 C13 C14 C15 1.6(4) . . . . ? C13 C12 C17 C16 -0.1(4) . . . . ? C13 C14 C15 C16 -0.9(4) . . . . ? C14 C15 C16 C17 -0.2(4) . . . . ? C15 C16 C17 C12 0.7(4) . . . . ? C17 C12 C13 C14 -1.1(4) . . . . ? C18 C3 C4 C5 178.9(2) . . . . ? C18 C19 C20 C21 0.5(4) . . . . ? C19 C18 C23 C22 0.4(4) . . . . ? C19 C20 C21 C22 0.4(4) . . . . ? C20 C21 C22 C23 -0.8(4) . . . . ? C21 C22 C23 C18 0.5(4) . . . . ? C23 C18 C19 C20 -0.8(4) . . . . ? _shelx_res_file ; TITL FN02B2 in P2(1)/n CELL 0.71073 11.1311 19.9977 11.6468 90 109.426 90 ZERR 4 0.0004 0.0007 0.0004 0 0.0011 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O P W UNIT 112 68 20 4 4 RIGU L.S. 100 PLAN 20 SIZE 0.02 0.15 0.16 TEMP -173.15 REM Solution 1 R1 0.053 Rweak 0.003, Alpha = 0.0239 in P2(1)/n BOND LIST 6 MORE -1 CONF fmap 2 acta 52 REM C:/Users/Wiecko/Desktop/Strukturen/Massimo/FN02B2/FN02B2_a.hkl WGHT 0.017400 2.352700 FVAR 0.22201 W1 5 0.770432 0.241883 0.247003 11.00000 0.01651 0.01913 = 0.01313 -0.00151 0.00638 0.00042 P1 4 0.743488 0.315854 0.410345 11.00000 0.01634 0.01683 = 0.01565 -0.00067 0.00808 -0.00079 O1 3 0.680575 0.365532 0.065851 11.00000 0.06571 0.05079 = 0.03876 0.02312 0.03193 0.03231 O2 3 1.066031 0.266237 0.295787 11.00000 0.02524 0.04019 = 0.05053 -0.01604 0.01970 -0.00823 O3 3 0.869582 0.115859 0.417382 11.00000 0.04668 0.03523 = 0.03361 0.00976 0.02096 0.01265 O4 3 0.481663 0.194774 0.181216 11.00000 0.02271 0.09253 = 0.03271 -0.02205 0.00859 -0.01477 O5 3 0.783445 0.150253 0.031734 11.00000 0.03330 0.04081 = 0.02829 -0.01612 0.01579 -0.00610 C1 1 0.780995 0.400100 0.435210 11.00000 0.01600 0.01815 = 0.01677 0.00088 0.00555 -0.00035 C2 1 0.738590 0.438286 0.513815 11.00000 0.01829 0.01650 = 0.01741 -0.00049 0.00570 -0.00055 AFIX 43 H2 2 0.761659 0.484221 0.521655 11.00000 -1.20000 AFIX 0 C3 1 0.664825 0.415179 0.582638 11.00000 0.01614 0.01945 = 0.01286 -0.00007 0.00372 0.00180 C4 1 0.625376 0.348861 0.575072 11.00000 0.01456 0.02219 = 0.01543 0.00079 0.00695 -0.00024 AFIX 43 H4 2 0.575608 0.335911 0.623647 11.00000 -1.20000 AFIX 0 C5 1 0.652527 0.299735 0.502391 11.00000 0.01634 0.01813 = 0.01634 0.00087 0.00723 -0.00068 C6 1 0.594610 0.232205 0.499364 11.00000 0.02229 0.01938 = 0.01634 -0.00316 0.01299 -0.00254 C7 1 0.463233 0.225391 0.449067 11.00000 0.02341 0.02825 = 0.02322 -0.00312 0.01010 -0.00282 AFIX 43 H7 2 0.412027 0.263297 0.415852 11.00000 -1.20000 AFIX 0 C8 1 0.406275 0.163105 0.447168 11.00000 0.02875 0.03625 = 0.02722 -0.00728 0.01355 -0.01377 AFIX 43 H8 2 0.316486 0.158563 0.412061 11.00000 -1.20000 AFIX 0 C9 1 0.480501 0.107923 0.496400 11.00000 0.04638 0.02538 = 0.02919 -0.00751 0.02354 -0.01391 AFIX 43 H9 2 0.441689 0.065550 0.495740 11.00000 -1.20000 AFIX 0 C10 1 0.610944 0.114529 0.546443 11.00000 0.04218 0.02057 = 0.03251 0.00083 0.02396 -0.00018 AFIX 43 H10 2 0.661771 0.076566 0.580087 11.00000 -1.20000 AFIX 0 C11 1 0.668356 0.176151 0.547981 11.00000 0.02641 0.02302 = 0.02578 0.00129 0.01523 -0.00024 AFIX 43 H11 2 0.758301 0.180202 0.582296 11.00000 -1.20000 AFIX 0 C12 1 0.860761 0.432691 0.371107 11.00000 0.02090 0.01792 = 0.01650 -0.00284 0.00876 -0.00295 C13 1 0.980526 0.407214 0.382340 11.00000 0.02250 0.01748 = 0.01649 -0.00063 0.00764 -0.00246 AFIX 43 H13 2 1.011424 0.368952 0.431680 11.00000 -1.20000 AFIX 0 C14 1 1.055293 0.437074 0.322281 11.00000 0.02060 0.02472 = 0.02254 -0.00327 0.01005 -0.00268 AFIX 43 H14 2 1.135997 0.418668 0.328868 11.00000 -1.20000 AFIX 0 C15 1 1.011752 0.493835 0.252681 11.00000 0.03023 0.02577 = 0.02278 -0.00131 0.01401 -0.00752 AFIX 43 H15 2 1.063208 0.514781 0.212390 11.00000 -1.20000 AFIX 0 C16 1 0.893802 0.519983 0.241793 11.00000 0.03470 0.02229 = 0.02837 0.00609 0.01448 0.00046 AFIX 43 H16 2 0.864458 0.559013 0.194220 11.00000 -1.20000 AFIX 0 C17 1 0.817398 0.489451 0.300217 11.00000 0.02706 0.02115 = 0.02880 0.00391 0.01339 0.00219 AFIX 43 H17 2 0.735826 0.507365 0.291656 11.00000 -1.20000 AFIX 0 C18 1 0.627061 0.463078 0.662575 11.00000 0.01513 0.02000 = 0.01624 -0.00273 0.00524 0.00049 C19 1 0.608246 0.530753 0.631411 11.00000 0.01976 0.02144 = 0.01722 -0.00142 0.00629 -0.00068 AFIX 43 H19 2 0.621567 0.546362 0.559548 11.00000 -1.20000 AFIX 0 C20 1 0.570340 0.575502 0.704068 11.00000 0.02115 0.01833 = 0.02194 -0.00100 0.00381 0.00169 AFIX 43 H20 2 0.557345 0.621253 0.681359 11.00000 -1.20000 AFIX 0 C21 1 0.551423 0.553377 0.809936 11.00000 0.02220 0.02846 = 0.02113 -0.00617 0.00841 0.00342 AFIX 43 H21 2 0.525019 0.583870 0.859385 11.00000 -1.20000 AFIX 0 C22 1 0.571204 0.486782 0.842974 11.00000 0.02536 0.03088 = 0.01721 -0.00094 0.00939 0.00188 AFIX 43 H22 2 0.559451 0.471652 0.915829 11.00000 -1.20000 AFIX 0 C23 1 0.608181 0.441999 0.769970 11.00000 0.02165 0.02029 = 0.02076 0.00133 0.00931 0.00230 AFIX 43 H23 2 0.620882 0.396317 0.793239 11.00000 -1.20000 AFIX 0 C24 1 0.714159 0.321702 0.131347 11.00000 0.03788 0.03174 = 0.02468 0.00230 0.01949 0.01055 C25 1 0.959594 0.261346 0.279259 11.00000 0.02518 0.02304 = 0.02602 -0.00661 0.01369 -0.00228 C26 1 0.831188 0.161956 0.359320 11.00000 0.02295 0.02534 = 0.02036 -0.00138 0.01049 0.00109 C27 1 0.584468 0.212814 0.207295 11.00000 0.02498 0.04436 = 0.01843 -0.00936 0.00774 -0.00031 C28 1 0.777998 0.184115 0.109513 11.00000 0.01921 0.02805 = 0.02261 -0.00146 0.00765 -0.00113 HKLF 4 REM FN02B2 in P2(1)/n REM R1 = 0.0207 for 5320 Fo > 4sig(Fo) and 0.0286 for all 6093 data REM 316 parameters refined using 288 restraints END WGHT 0.0174 2.3526 REM Highest difference peak 1.798, deepest hole -0.853, 1-sigma level 0.097 Q1 1 0.7698 0.2829 0.2447 11.00000 0.05 1.80 Q2 1 0.7588 0.1948 0.2419 11.00000 0.05 0.94 Q3 1 0.7752 0.3576 0.4271 11.00000 0.05 0.53 Q4 1 0.6412 0.2408 0.2631 11.00000 0.05 0.45 Q5 1 1.0223 0.4600 0.2753 11.00000 0.05 0.43 Q6 1 0.5465 0.1175 0.4844 11.00000 0.05 0.41 Q7 1 0.4796 0.2303 0.1442 11.00000 0.05 0.41 Q8 1 0.7808 0.2205 0.1336 11.00000 0.05 0.38 Q9 1 0.5778 0.2561 0.1895 11.00000 0.05 0.38 Q10 1 0.6033 0.5548 0.6773 11.00000 0.05 0.38 Q11 1 0.7953 0.1155 0.0723 11.00000 0.05 0.38 Q12 1 0.4198 0.1998 0.4619 11.00000 0.05 0.36 Q13 1 0.8377 0.4589 0.3361 11.00000 0.05 0.36 Q14 1 0.7599 0.1619 0.3051 11.00000 0.05 0.36 Q15 1 0.9414 0.4971 0.2387 11.00000 0.05 0.36 Q16 1 0.7606 0.3305 0.2453 11.00000 0.05 0.35 Q17 1 1.0052 0.4176 0.3320 11.00000 0.05 0.35 Q18 1 0.5795 0.5231 0.8406 11.00000 0.05 0.35 Q19 1 0.7888 0.1543 0.2100 11.00000 0.05 0.35 Q20 1 0.6071 0.2794 0.1175 11.00000 0.05 0.35 ; _shelx_res_checksum 40819 _shelx_hkl_file ; 2 0 0 2864.21 62.59 2 0 0 3070.49 62.69 -2 0 0 2917.41 62.59 -2 0 0 3067.29 62.69 -3 0 0 -2.60 1.20 3 0 0 -3.00 1.30 3 0 0 -3.90 1.00 4 0 0 1962.20 42.50 -4 0 0 1972.30 42.80 -4 0 0 1996.00 43.00 4 0 0 1877.01 42.60 -4 0 0 1919.11 42.50 -5 0 0 0.70 1.90 5 0 0 -1.40 1.90 5 0 0 -0.30 1.70 -5 0 0 0.70 2.30 -5 0 0 0.90 2.10 -6 0 0 1807.02 41.10 -6 0 0 1826.72 41.60 6 0 0 1835.22 41.10 -6 0 0 1806.22 41.90 6 0 0 1797.42 41.50 7 0 0 5.80 3.00 7 0 0 1.20 2.60 -7 0 0 -2.60 2.70 -7 0 0 1.40 3.10 -7 0 0 4.00 3.50 -8 0 0 664.23 20.20 8 0 0 645.34 19.20 -8 0 0 666.73 18.90 8 0 0 649.43 18.60 -8 0 0 665.33 19.80 -9 0 0 -2.50 4.40 9 0 0 3.00 3.80 -9 0 0 -2.60 4.20 9 0 0 -3.60 3.70 -10 0 0 160.98 11.50 -10 0 0 155.38 12.10 10 0 0 164.78 11.20 -10 0 0 172.58 12.60 -11 0 0 18.30 7.40 11 0 0 0.50 5.10 -11 0 0 -5.80 5.70 -12 0 0 34.00 9.20 -12 0 0 8.60 7.30 12 0 0 2.20 6.00 -13 0 0 -5.90 8.50 13 0 0 16.70 7.70 -13 0 0 3.90 9.50 14 0 0 9.20 11.10 -14 0 0 16.10 11.50 1 1 0 -6.40 0.50 1 1 0 -6.60 0.30 2 -1 0 10.00 1.80 -2 -1 0 9.70 1.60 -2 -1 0 9.60 1.60 2 -1 0 8.70 1.70 -2 1 0 11.60 2.00 2 1 0 11.50 1.50 -2 1 0 7.30 1.40 -2 1 0 9.90 1.70 2 1 0 8.10 1.60 3 -1 0 483.35 12.40 -3 -1 0 477.65 12.00 -3 -1 0 508.05 12.20 3 -1 0 508.85 12.40 3 1 0 509.75 12.00 3 1 0 477.65 12.20 -3 1 0 512.55 12.80 -3 1 0 514.55 12.60 -3 1 0 496.35 12.30 4 -1 0 459.75 12.10 -4 -1 0 465.55 12.30 -4 -1 0 457.85 11.90 -4 -1 0 466.45 12.10 4 -1 0 444.56 12.20 4 1 0 446.96 12.00 -4 1 0 461.95 12.40 4 1 0 464.45 11.80 -4 1 0 458.55 12.10 -4 1 0 479.75 12.70 -5 -1 0 40.60 4.20 -5 -1 0 43.30 4.40 5 -1 0 36.80 4.40 5 -1 0 37.20 4.10 -5 1 0 41.10 4.50 -5 1 0 41.60 4.00 5 1 0 44.60 3.70 5 1 0 37.60 4.00 -5 1 0 38.30 4.60 -6 -1 0 1731.93 39.70 -6 -1 0 1732.43 40.10 6 -1 0 1705.33 39.80 -6 -1 0 1739.13 39.30 6 -1 0 1761.22 39.60 6 1 0 1679.23 39.60 -6 1 0 1709.63 40.40 -6 1 0 1761.52 39.60 6 1 0 1749.12 39.20 -6 1 0 1734.23 40.10 -7 -1 0 46.30 6.30 7 -1 0 44.50 5.30 7 -1 0 44.70 5.50 -7 -1 0 51.39 5.40 -7 -1 0 45.90 5.10 -7 1 0 49.30 5.70 -7 1 0 45.20 5.50 7 1 0 41.90 5.30 7 1 0 42.00 4.90 -7 1 0 49.80 6.50 -8 -1 0 767.02 20.40 8 -1 0 718.43 20.30 -8 -1 0 725.93 21.10 -8 -1 0 751.12 21.70 8 -1 0 730.63 20.80 8 1 0 728.53 20.80 -8 1 0 722.43 21.30 -8 1 0 722.63 20.50 -8 1 0 745.13 21.90 8 1 0 701.43 19.80 9 -1 0 1.60 3.90 -9 -1 0 -4.70 4.40 9 -1 0 9.50 4.50 -9 -1 0 6.90 4.80 -9 -1 0 2.70 4.30 -9 1 0 3.10 5.00 9 1 0 -1.40 3.80 9 1 0 3.30 3.90 -9 1 0 6.80 4.70 -9 1 0 -0.20 4.30 -10 -1 0 1142.89 31.30 -10 -1 0 1119.59 30.00 10 -1 0 1143.39 30.70 -10 -1 0 1123.39 31.70 10 1 0 1080.79 29.60 -10 1 0 1103.79 30.20 -10 1 0 1113.59 31.50 -10 1 0 1117.29 32.10 10 1 0 1100.49 31.20 -11 -1 0 26.00 14.00 11 -1 0 23.50 6.00 -11 1 0 16.70 6.60 -11 1 0 17.90 7.20 11 1 0 27.90 6.30 -12 -1 0 408.96 20.40 12 -1 0 399.06 17.80 -12 -1 0 388.06 19.60 -12 1 0 404.06 20.00 -12 1 0 416.66 20.90 12 1 0 459.65 18.70 -13 -1 0 17.80 9.70 13 -1 0 0.60 7.10 -13 -1 0 -3.10 8.20 13 1 0 -1.80 7.00 -13 1 0 -2.30 9.10 14 -1 0 293.47 29.70 14 1 0 292.97 21.10 1 -2 0 63.39 2.40 -1 -2 0 55.99 1.70 -1 -2 0 58.89 2.00 1 -2 0 62.69 2.40 1 -2 0 52.49 2.10 -1 2 0 63.69 2.50 1 2 0 56.19 1.70 1 2 0 56.69 2.10 -1 2 0 64.09 2.40 -2 -2 0 4228.28 89.69 2 -2 0 4234.18 89.29 -2 -2 0 4296.77 89.89 -2 2 0 4525.25 91.89 -2 2 0 4209.98 89.39 2 2 0 4285.27 89.99 2 2 0 4032.00 88.89 3 -2 0 57.39 3.50 -3 -2 0 52.49 2.90 3 -2 0 53.49 3.40 -3 -2 0 50.19 2.90 3 2 0 52.09 3.10 -3 2 0 53.49 3.30 -3 2 0 53.19 3.80 -3 2 0 52.69 3.70 3 2 0 57.29 2.80 -4 -2 0 3279.47 71.09 4 -2 0 3299.97 71.59 -4 -2 0 3361.16 71.09 4 -2 0 3392.16 72.19 4 2 0 3235.78 71.19 -4 2 0 3385.76 72.09 4 2 0 3309.27 70.79 -4 2 0 3399.16 71.59 -4 2 0 3408.16 71.89 -5 -2 0 2.10 2.30 -5 -2 0 1.10 2.10 5 -2 0 -1.30 1.80 -5 -2 0 2.20 1.90 5 -2 0 0.20 2.10 -5 2 0 0.60 2.20 -5 2 0 0.90 2.30 5 2 0 0.10 1.90 -6 -2 0 1286.47 30.10 -6 -2 0 1268.27 30.30 6 -2 0 1317.37 30.70 6 -2 0 1238.08 30.60 -6 -2 0 1299.07 30.80 6 2 0 1228.18 30.30 -6 2 0 1326.47 31.60 -6 2 0 1303.47 31.10 -6 2 0 1328.67 30.70 6 2 0 1252.97 29.70 7 -2 0 -1.80 2.60 7 -2 0 1.60 2.90 -7 -2 0 -3.60 2.50 -7 -2 0 3.90 3.40 -7 -2 0 -3.80 2.80 7 2 0 0.20 2.30 -7 2 0 0.70 2.80 -7 2 0 0.80 3.50 -7 2 0 1.70 3.20 7 2 0 -3.30 2.60 -8 -2 0 330.47 11.90 8 -2 0 306.87 12.30 -8 -2 0 317.27 13.00 -8 -2 0 340.37 12.80 8 -2 0 306.87 12.00 -8 2 0 341.97 13.70 8 2 0 308.57 11.30 8 2 0 322.27 12.30 -8 2 0 337.77 12.30 -8 2 0 334.77 13.30 -9 -2 0 57.99 6.10 9 -2 0 49.70 6.10 -9 -2 0 40.20 6.50 -9 -2 0 53.89 6.70 9 -2 0 44.80 5.90 -9 2 0 55.09 7.50 -9 2 0 40.20 6.70 9 2 0 60.19 7.40 9 2 0 43.40 5.30 -9 2 0 51.39 6.20 -10 -2 0 145.99 10.70 10 -2 0 142.59 10.40 -10 -2 0 165.48 12.10 -10 -2 0 143.99 11.60 10 2 0 142.29 10.20 -10 2 0 139.09 12.10 -10 2 0 150.18 11.90 10 2 0 136.09 11.50 -10 2 0 143.49 11.60 11 -2 0 1.80 5.30 -11 -2 0 0.00 6.80 -11 -2 0 -4.20 6.20 11 2 0 2.00 5.00 -11 2 0 2.00 6.20 -11 2 0 -0.20 6.40 -12 -2 0 26.40 8.80 -12 -2 0 15.80 7.70 12 -2 0 11.20 6.40 -12 2 0 21.10 8.40 12 2 0 17.30 6.80 -12 2 0 17.70 7.80 -13 -2 0 6.80 9.00 13 -2 0 3.80 7.30 -13 -2 0 8.10 9.80 13 2 0 21.80 7.80 -13 2 0 35.30 10.10 0 -3 0 -2.90 0.70 0 3 0 -2.50 0.70 0 3 0 -2.70 0.80 1 -3 0 80.89 3.00 1 -3 0 82.39 3.00 1 -3 0 72.69 2.70 -1 -3 0 73.79 2.10 -1 -3 0 74.39 2.60 -1 -3 0 75.89 2.20 -1 3 0 80.69 3.00 1 3 0 76.09 2.60 -1 3 0 80.89 3.10 1 3 0 76.99 2.10 -1 3 0 78.19 2.80 2 -3 0 54.09 3.60 2 -3 0 64.19 3.20 -2 -3 0 58.49 2.30 -2 -3 0 60.49 2.70 -2 3 0 57.29 3.40 -2 3 0 59.09 2.90 -2 3 0 62.29 3.30 2 3 0 56.29 2.70 2 3 0 55.39 2.20 3 -3 0 755.92 18.10 -3 -3 0 739.83 17.50 -3 -3 0 776.12 17.40 3 -3 0 810.62 18.40 -3 3 0 779.02 18.40 -3 3 0 753.32 18.10 -3 3 0 794.92 18.70 3 3 0 742.13 17.20 3 3 0 756.02 17.80 -4 -3 0 913.01 20.80 4 -3 0 949.60 21.90 4 -3 0 892.21 21.40 -4 -3 0 871.11 20.80 4 3 0 884.91 20.50 -4 3 0 902.61 21.80 4 3 0 863.11 21.00 -4 3 0 912.61 22.10 -4 3 0 911.61 21.50 5 -3 0 369.96 11.40 5 -3 0 388.26 11.50 -5 -3 0 380.76 10.90 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845.22 23.80 -10 3 0 866.11 26.70 -10 3 0 859.61 27.30 -11 -3 0 47.60 8.10 -11 -3 0 57.19 9.20 -11 -3 0 57.49 8.30 11 -3 0 55.79 7.80 -11 3 0 70.69 10.10 -11 3 0 54.79 9.00 11 3 0 68.29 8.10 -12 -3 0 367.26 19.10 12 -3 0 396.56 18.30 -12 -3 0 402.66 20.00 -12 3 0 419.66 21.30 -12 3 0 433.26 20.60 12 3 0 459.15 19.10 -13 -3 0 19.40 9.70 13 -3 0 26.60 8.20 -13 -3 0 32.40 10.90 -13 3 0 20.70 10.20 13 3 0 28.40 7.80 0 -4 0 3023.20 62.89 0 4 0 2984.50 63.29 0 4 0 3013.00 62.89 -1 -4 0 209.58 5.10 1 -4 0 228.98 6.20 1 -4 0 222.58 6.00 -1 -4 0 207.28 5.10 1 -4 0 208.08 5.80 -1 -4 0 211.18 5.60 -1 4 0 217.78 6.20 -1 4 0 214.58 5.90 1 4 0 219.18 5.20 -1 4 0 217.68 6.10 1 4 0 217.18 5.70 2 -4 0 936.01 20.40 -2 -4 0 895.21 19.10 -2 -4 0 887.01 19.60 2 -4 0 862.71 20.10 2 -4 0 919.61 20.50 2 4 0 844.12 19.70 2 4 0 859.51 19.00 -2 4 0 888.61 20.20 3 -4 0 295.27 8.60 3 -4 0 307.77 8.80 -3 -4 0 294.17 7.60 -3 -4 0 288.27 8.00 -3 4 0 308.37 9.00 -3 4 0 312.97 9.20 3 4 0 290.47 7.40 3 4 0 294.57 8.20 4 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0 512.25 12.60 2 -6 0 523.05 13.30 2 -6 0 546.05 13.50 -2 6 0 543.65 13.50 -2 6 0 542.55 13.90 -2 6 0 551.74 13.70 2 6 0 527.05 13.10 3 -6 0 31.00 3.30 -3 -6 0 29.90 2.70 -3 -6 0 28.00 2.10 -3 6 0 33.70 3.70 3 6 0 24.00 1.90 -3 6 0 28.10 3.20 3 6 0 28.40 3.10 -3 6 0 24.50 3.20 -4 -6 0 1156.48 25.70 4 -6 0 1181.08 27.60 4 -6 0 1123.89 27.20 -4 -6 0 1169.78 26.30 4 6 0 1144.29 25.50 -4 6 0 1167.48 27.80 -4 6 0 1183.48 28.10 -4 6 0 1152.58 27.30 4 6 0 1142.19 26.70 -5 -6 0 174.68 6.40 -5 -6 0 180.68 6.60 5 -6 0 163.88 7.40 5 -6 0 177.18 7.70 -5 6 0 177.48 8.40 5 6 0 179.78 5.90 -5 6 0 169.88 8.10 -5 6 0 168.28 7.30 5 6 0 164.98 7.00 -6 -6 0 806.02 20.20 6 -6 0 796.82 21.70 6 -6 0 820.92 21.60 6 6 0 858.71 20.80 -6 6 0 823.22 22.70 6 6 0 822.02 21.10 -6 6 0 817.42 21.60 -6 6 0 810.32 22.30 -7 -6 0 12.50 3.20 7 -6 0 7.40 3.60 7 -6 0 10.20 3.70 -7 -6 0 9.70 3.80 -7 -6 0 7.60 3.30 -7 6 0 6.30 3.50 7 6 0 11.50 2.80 -7 6 0 12.30 4.40 -7 6 0 11.20 4.30 7 6 0 7.50 3.40 -8 -6 0 137.59 8.00 8 -6 0 123.99 9.40 8 -6 0 131.59 9.00 -8 -6 0 126.09 8.60 -8 -6 0 151.48 8.70 8 6 0 138.09 7.10 8 6 0 121.69 8.30 -8 6 0 142.89 9.30 -8 6 0 116.99 9.60 -8 6 0 120.69 10.10 -9 -6 0 25.80 5.20 9 -6 0 24.10 5.20 -9 -6 0 28.80 5.20 -9 -6 0 30.00 5.80 9 6 0 33.10 4.60 -9 6 0 19.10 5.80 9 6 0 33.10 5.30 -9 6 0 32.60 6.60 -9 6 0 19.80 6.20 10 -6 0 82.19 10.00 -10 -6 0 78.59 10.60 -10 -6 0 87.69 10.40 -10 -6 0 85.89 9.80 10 6 0 82.39 9.50 10 6 0 88.59 9.00 -10 6 0 103.69 12.10 -10 6 0 111.89 11.80 11 -6 0 -5.40 5.50 -11 -6 0 5.90 6.30 -11 -6 0 -4.80 6.80 -11 -6 0 -1.10 6.30 11 6 0 -5.70 5.60 -11 6 0 -3.00 7.30 11 6 0 -2.10 5.40 -11 6 0 -13.60 5.80 -12 -6 0 12.50 8.80 -12 -6 0 30.40 9.60 12 -6 0 9.30 6.60 12 6 0 16.10 6.60 -12 6 0 -3.90 8.00 -13 -6 0 2.60 10.00 13 -6 0 -4.00 7.70 -13 6 0 11.80 10.00 13 6 0 13.40 8.00 0 -7 0 2.50 1.30 0 -7 0 3.70 1.40 0 7 0 0.30 1.40 0 7 0 1.60 1.70 0 7 0 2.90 1.30 1 -7 0 105.79 4.30 -1 -7 0 102.89 4.30 -1 -7 0 105.59 3.60 1 -7 0 102.79 4.30 1 -7 0 110.29 4.50 1 7 0 96.79 3.40 1 7 0 100.19 4.50 -1 7 0 107.69 4.50 -1 7 0 103.79 5.10 -2 -7 0 244.48 6.30 -2 -7 0 239.88 7.10 2 -7 0 242.68 7.60 2 -7 0 250.67 7.80 -2 -7 0 242.78 6.10 2 -7 0 255.17 8.10 -2 7 0 267.57 8.20 -2 7 0 255.37 8.30 2 7 0 254.37 7.60 -2 7 0 269.17 8.00 -3 -7 0 43.80 3.20 -3 -7 0 52.79 2.60 3 -7 0 46.00 4.30 -3 -7 0 49.20 2.50 3 -7 0 46.40 3.80 3 -7 0 54.89 4.20 -3 7 0 54.59 4.80 -3 7 0 58.49 4.10 3 7 0 50.49 2.40 3 7 0 50.69 3.80 -3 7 0 59.19 4.70 -4 -7 0 486.85 12.50 -4 -7 0 475.75 11.80 4 -7 0 496.45 13.90 4 -7 0 487.55 13.60 -4 7 0 496.65 14.60 -4 7 0 505.75 14.30 4 7 0 484.45 11.70 4 7 0 468.05 13.10 -4 7 0 494.85 13.70 5 -7 0 79.69 5.90 -5 -7 0 70.99 4.30 -5 -7 0 79.19 4.70 5 -7 0 79.39 5.50 -5 7 0 76.69 6.40 -5 7 0 75.69 5.30 5 7 0 74.59 3.80 5 7 0 82.89 5.30 -5 7 0 79.29 6.30 -6 -7 0 741.73 18.70 6 -7 0 744.23 20.70 6 -7 0 776.42 20.60 -6 7 0 738.53 21.50 6 7 0 750.02 18.30 -6 7 0 777.72 20.50 6 7 0 743.63 19.80 -6 7 0 744.33 21.10 -7 -7 0 64.39 6.40 7 -7 0 72.49 7.30 -7 -7 0 68.59 6.10 -7 -7 0 65.89 5.90 7 -7 0 66.09 6.80 -7 7 0 67.09 7.90 7 7 0 66.09 6.40 -7 7 0 66.69 7.60 7 7 0 64.89 4.90 -7 7 0 75.69 7.00 -8 -7 0 581.54 17.70 8 -7 0 594.24 18.70 -8 -7 0 589.64 17.30 8 -7 0 581.24 19.00 -8 -7 0 612.44 17.10 -8 7 0 592.64 20.20 8 7 0 603.54 16.30 8 7 0 612.54 18.30 -8 7 0 592.54 19.70 -8 7 0 584.94 18.90 -9 -7 0 118.19 9.60 -9 -7 0 118.89 9.20 -9 -7 0 103.19 8.50 9 -7 0 93.19 12.50 -9 7 0 106.89 11.20 9 7 0 106.79 7.60 9 7 0 104.49 8.70 -9 7 0 105.49 10.70 -10 -7 0 985.30 25.90 -10 -7 0 934.71 26.70 10 -7 0 969.00 27.80 -10 -7 0 933.21 27.20 10 7 0 939.71 27.20 -10 7 0 925.11 29.10 10 7 0 921.71 25.20 -10 7 0 959.60 30.00 -11 -7 0 19.40 6.80 11 -7 0 23.80 6.60 -11 -7 0 37.90 7.30 -11 -7 0 30.70 8.10 -11 7 0 35.60 8.70 11 7 0 37.70 6.70 11 7 0 26.40 6.70 -11 7 0 48.30 8.40 12 -7 0 533.65 20.90 -12 -7 0 451.55 33.70 -12 -7 0 488.95 25.20 -12 7 0 496.85 23.80 12 7 0 533.85 20.30 -13 -7 0 59.29 11.80 13 -7 0 53.09 9.70 13 7 0 49.99 9.70 -13 7 0 52.39 12.20 0 -8 0 1269.57 27.80 0 -8 0 1279.37 27.60 0 8 0 1251.57 28.80 0 8 0 1233.18 27.90 0 8 0 1250.47 28.30 -1 -8 0 360.46 9.10 1 -8 0 374.76 9.90 1 -8 0 377.96 10.20 -1 -8 0 372.26 10.00 1 -8 0 377.96 9.90 -1 8 0 360.96 10.30 -1 8 0 381.06 10.90 -1 8 0 376.16 10.50 1 8 0 354.26 10.20 1 8 0 357.26 9.10 -2 -8 0 784.12 17.50 2 -8 0 818.12 19.40 -2 -8 0 802.32 18.70 2 -8 0 831.72 19.80 2 -8 0 830.22 19.50 -2 -8 0 794.22 17.70 2 8 0 804.62 19.20 -2 8 0 768.22 20.70 -2 8 0 809.52 19.90 -3 -8 0 47.90 2.30 -3 -8 0 46.30 2.50 3 -8 0 47.30 4.00 -3 -8 0 50.29 3.50 -3 8 0 43.00 4.70 -3 8 0 47.80 4.80 3 8 0 50.19 4.00 -3 8 0 46.10 4.30 4 -8 0 775.02 19.80 4 -8 0 762.42 19.50 -4 -8 0 753.62 18.20 -4 -8 0 765.72 17.60 -4 -8 0 734.53 17.30 -4 8 0 801.02 19.80 4 8 0 761.12 17.30 -4 8 0 777.52 20.50 -4 8 0 771.12 20.20 4 8 0 732.63 18.90 -5 -8 0 152.28 6.20 5 -8 0 149.29 7.30 5 -8 0 148.09 7.70 -5 -8 0 151.88 5.80 -5 8 0 149.79 7.30 5 8 0 150.38 6.90 5 8 0 148.09 5.20 -5 8 0 157.38 8.20 -5 8 0 143.69 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1164.58 30.40 -10 1 4 1231.08 29.40 -10 1 4 1164.28 32.90 10 1 -4 1169.78 30.60 10 1 -4 1228.48 30.60 9 -1 -4 2.50 3.30 -9 -1 4 5.90 4.60 9 -1 -4 3.20 3.80 9 -1 -4 9.90 4.00 -9 -1 4 0.00 3.30 9 1 -4 8.70 3.80 9 1 -4 3.70 3.40 -9 1 4 4.00 3.00 -9 1 4 0.20 4.40 -9 1 4 3.00 3.70 9 1 -4 3.60 3.40 -8 -1 4 2012.20 45.00 -8 -1 4 2032.50 47.60 -8 -1 4 2039.90 44.60 8 -1 -4 2063.59 46.50 8 -1 -4 1994.60 47.00 8 -1 -4 2051.29 47.60 8 1 -4 2048.00 46.90 -8 1 4 1998.00 48.20 8 1 -4 2059.69 46.10 8 1 -4 2036.00 46.60 -8 1 4 1990.40 46.00 -8 1 4 2045.10 45.50 -7 -1 4 5.10 2.20 7 -1 -4 2.50 2.80 7 -1 -4 5.40 2.60 -7 -1 4 5.00 1.90 -7 -1 4 11.80 3.70 7 -1 -4 3.60 3.10 -7 1 4 6.20 2.80 -7 1 4 6.50 2.70 7 1 -4 0.00 2.70 -7 1 4 4.40 3.60 7 1 -4 0.30 2.20 7 1 -4 5.40 2.70 6 -1 -4 2317.17 51.19 6 -1 -4 2371.06 52.39 6 -1 -4 2373.96 52.79 -6 -1 4 2284.67 49.50 -6 -1 4 2318.07 52.09 -6 1 4 2299.17 50.59 -6 1 4 2286.67 52.69 6 1 -4 2329.47 50.69 -6 1 4 2328.97 50.39 6 1 -4 2393.36 51.99 6 1 -4 2315.47 52.39 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67.19 10.00 3 10 -14 50.39 8.70 2 -10 -14 277.87 20.60 2 10 -14 278.17 17.50 -2 10 14 294.17 18.30 6 -11 -14 219.38 19.60 -6 11 14 233.88 21.00 6 11 -14 235.88 14.60 5 -11 -14 19.40 9.50 -5 11 14 -3.10 10.30 -5 11 14 8.90 8.80 5 11 -14 -2.20 6.80 4 -11 -14 187.28 18.50 -4 11 14 147.29 15.90 4 11 -14 184.48 14.40 3 -11 -14 6.90 9.70 3 11 -14 14.30 7.40 -3 11 14 6.30 9.00 8 0 -15 1.00 7.30 7 0 -15 29.50 8.90 6 0 -15 -17.50 6.60 5 0 -15 27.80 8.10 4 0 -15 -6.00 7.30 3 0 -15 206.78 16.50 2 0 -15 10.00 8.20 8 -1 -15 3.40 7.70 8 1 -15 -0.90 7.60 7 -1 -15 422.16 21.10 7 1 -15 459.85 21.00 6 -1 -15 3.60 7.80 6 1 -15 -7.40 7.00 5 -1 -15 227.48 16.80 5 1 -15 206.88 15.80 4 -1 -15 23.90 8.50 4 1 -15 5.10 7.40 3 -1 -15 145.49 15.70 3 1 -15 162.38 15.70 2 -1 -15 12.60 8.20 2 1 -15 3.60 8.10 8 -2 -15 -2.90 8.10 8 2 -15 19.20 8.20 -8 2 15 14.80 9.80 7 -2 -15 9.00 7.80 7 2 -15 16.10 7.40 6 -2 -15 39.30 9.30 6 2 -15 32.50 8.10 5 -2 -15 87.59 11.00 5 2 -15 97.59 10.80 4 -2 -15 23.40 8.20 4 2 -15 20.30 8.10 3 -2 -15 314.67 19.30 3 2 -15 310.97 18.30 2 -2 -15 -9.00 8.20 2 2 -15 14.70 9.00 8 -3 -15 8.40 9.30 -8 3 15 15.70 10.10 8 3 -15 8.20 7.70 7 -3 -15 394.36 20.70 7 3 -15 375.76 19.00 6 -3 -15 5.90 8.10 6 3 -15 11.50 7.20 5 -3 -15 191.68 16.80 5 3 -15 193.58 15.60 4 -3 -15 6.10 8.00 4 3 -15 11.00 8.00 3 -3 -15 221.68 17.60 3 3 -15 254.37 16.80 2 -3 -15 14.00 8.80 2 3 -15 26.80 9.00 7 -4 -15 154.98 16.60 -7 4 15 149.79 18.00 7 4 -15 158.48 14.80 6 -4 -15 63.09 11.00 6 4 -15 47.20 9.00 5 -4 -15 169.48 16.90 5 4 -15 144.09 14.40 4 -4 -15 38.60 9.20 4 4 -15 37.60 8.60 3 -4 -15 272.17 19.10 3 4 -15 262.77 17.50 2 -4 -15 3.10 9.40 2 4 -15 13.30 8.50 7 -5 -15 281.07 19.60 -7 5 15 304.27 21.40 7 5 -15 267.37 16.70 6 -5 -15 81.89 11.20 6 5 -15 71.69 9.50 5 -5 -15 303.17 19.50 5 5 -15 284.77 17.30 4 -5 -15 24.00 8.80 4 5 -15 18.30 7.90 3 -5 -15 193.18 18.10 3 5 -15 202.38 16.20 6 -6 -15 -8.90 7.80 6 6 -15 15.20 7.40 5 -6 -15 152.48 17.50 5 6 -15 232.78 15.60 4 -6 -15 31.60 9.90 4 6 -15 33.50 8.80 3 -6 -15 361.06 21.70 3 6 -15 357.66 18.90 5 -7 -15 197.78 19.20 5 7 -15 244.28 16.10 ; _shelx_hkl_checksum 12696 _olex2_submission_special_instructions 'No special instructions were received' #============================================================================== _publ_requested_journal 'Chemistry - A European Journal' _publ_contact_author ; Prof. Dr.Christian M\"uller Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+49/(0)3083854004' _publ_contact_author_fax '+49/(0)3083852440' _publ_contact_author_email c.mueller@fu-berlin.de loop_ _publ_author_name _publ_author_address 'M\"uller, Christian' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Rigo, Massimo' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Wiecko, Jelena' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany 'Weber, Manuela' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_section_title ; ; _publ_section_abstract ; ... and following paragraphs: see the published paper. ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _publ_section_figure_captions ; ; #END==================================================== ;