data_MR336_a _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H19 F6 O P Si' _chemical_formula_weight 412.38 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9992(2) _cell_length_b 10.1647(3) _cell_length_c 11.3907(3) _cell_angle_alpha 99.1849(11) _cell_angle_beta 91.1844(10) _cell_angle_gamma 112.8005(9) _cell_volume 944.31(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7640 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 26.42 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_F_000 424 _exptl_transmission_factor_min 0.9285 _exptl_transmission_factor_max 0.9582 _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.090 _exptl_absorpt_coefficient_mu 0.269 _shelx_estimated_absorpt_T_min 0.929 _shelx_estimated_absorpt_T_max 0.976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'D8 Venture, Bruker Photon CMOS Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14905 _diffrn_reflns_av_unetI/netI 0.0413 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.465 _diffrn_reflns_theta_max 26.430 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 3879 _reflns_number_gt 3092 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'Microsoft Word' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.7203P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3879 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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_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 C1 C 0.6979(2) 0.3287(2) 0.67640(17) 0.0133(4) Uani 1 1 d . . . . . H1 H 0.707(2) 0.525(2) 0.5598(18) 0.016(5) Uiso 1 1 d . . . . . C2 C 0.7672(2) 0.2276(2) 0.67049(16) 0.0127(4) Uani 1 1 d . . . . . C3 C 0.8312(2) 0.1778(2) 0.56875(17) 0.0154(4) Uani 1 1 d . . . . . H3 H 0.8734 0.1065 0.5746 0.018 Uiso 1 1 calc R U . . . C4 C 0.8366(2) 0.2255(2) 0.46185(17) 0.0149(4) Uani 1 1 d . . . . . C5 C 0.7793(2) 0.3315(2) 0.44029(17) 0.0153(4) Uani 1 1 d . . . . . C6 C 0.7790(2) 0.1618(2) 0.77673(17) 0.0148(4) Uani 1 1 d . . . . . C7 C 0.9281(3) 0.2038(2) 0.84154(18) 0.0215(5) Uani 1 1 d . . . . . H7 H 1.0223 0.2743 0.8181 0.026 Uiso 1 1 calc R U . . . C8 C 0.9391(3) 0.1426(3) 0.9402(2) 0.0286(5) Uani 1 1 d . . . . . H8 H 1.0403 0.1736 0.9857 0.034 Uiso 1 1 calc R U . . . C9 C 0.8036(3) 0.0370(3) 0.97257(19) 0.0289(6) Uani 1 1 d . . . . . H9 H 0.8118 -0.0047 1.0401 0.035 Uiso 1 1 calc R U . . . C10 C 0.6558(3) -0.0082(2) 0.90693(19) 0.0245(5) Uani 1 1 d . . . . . H10 H 0.5631 -0.0824 0.9282 0.029 Uiso 1 1 calc R U . . . C11 C 0.6433(3) 0.0550(2) 0.80986(17) 0.0179(4) Uani 1 1 d . . . . . H11 H 0.5414 0.0252 0.7658 0.022 Uiso 1 1 calc R U . . . C12 C 0.9125(3) 0.1578(2) 0.36588(18) 0.0202(5) Uani 1 1 d . . . . . C13 C 0.7910(3) 0.3896(2) 0.32770(18) 0.0211(5) Uani 1 1 d . . . . . C14 C 0.7477(3) 0.4271(2) 0.95442(18) 0.0233(5) Uani 1 1 d . . . . . H14A H 0.7308 0.3319 0.9734 0.035 Uiso 1 1 calc R U . . . H14B H 0.7171 0.4835 1.0203 0.035 Uiso 1 1 calc R U . . . H14C H 0.8620 0.4788 0.9429 0.035 Uiso 1 1 calc R U . . . C15 C 0.4060(3) 0.2797(2) 0.8252(2) 0.0240(5) Uani 1 1 d . . . . . H15A H 0.3390 0.2752 0.7546 0.036 Uiso 1 1 calc R U . . . H15B H 0.3665 0.3171 0.8972 0.036 Uiso 1 1 calc R U . . . H15C H 0.4000 0.1822 0.8293 0.036 Uiso 1 1 calc R U . . . C16 C 0.6270(3) 0.5849(2) 0.79934(19) 0.0223(5) Uani 1 1 d . . . . . H16A H 0.7394 0.6516 0.7968 0.033 Uiso 1 1 calc R U . . . H16B H 0.5813 0.6224 0.8677 0.033 Uiso 1 1 calc R U . . . H16C H 0.5636 0.5762 0.7254 0.033 Uiso 1 1 calc R U . . . C17 C 0.3831(3) 0.1854(2) 0.4750(2) 0.0238(5) Uani 1 1 d . . . . . H17A H 0.2723 0.1692 0.4940 0.036 Uiso 1 1 calc R U . . . H17B H 0.4259 0.1330 0.5219 0.036 Uiso 1 1 calc R U . . . H17C H 0.3827 0.1500 0.3897 0.036 Uiso 1 1 calc R U . . . O1 O 0.48402(17) 0.33913(14) 0.50349(12) 0.0180(3) Uani 1 1 d . . . . . F1 F 0.91983(16) 0.03451(13) 0.38831(11) 0.0277(3) Uani 1 1 d . . . . . F2 F 1.06586(15) 0.24549(14) 0.35502(11) 0.0302(3) Uani 1 1 d . . . . . F3 F 0.83099(16) 0.12316(14) 0.25835(10) 0.0291(3) Uani 1 1 d . . . . . F4 F 0.93286(16) 0.41730(15) 0.28090(11) 0.0317(3) Uani 1 1 d . . . . . F5 F 0.67624(15) 0.30168(14) 0.23916(10) 0.0281(3) Uani 1 1 d . . . . . F6 F 0.77005(17) 0.51617(14) 0.34501(11) 0.0314(3) Uani 1 1 d . . . . . Si1 Si 0.62049(7) 0.40253(6) 0.81491(5) 0.01411(14) Uani 1 1 d . . . . . P1 P 0.67147(6) 0.38798(5) 0.54623(4) 0.01390(13) 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 C1 0.0120(10) 0.0118(9) 0.0132(9) 0.0018(7) 0.0010(8) 0.0019(8) C2 0.0086(10) 0.0127(9) 0.0123(9) 0.0007(7) -0.0011(7) 0.0001(8) C3 0.0145(10) 0.0147(10) 0.0159(10) 0.0007(8) -0.0005(8) 0.0054(8) C4 0.0104(10) 0.0154(10) 0.0144(10) 0.0006(8) 0.0006(8) 0.0013(8) C5 0.0136(10) 0.0159(10) 0.0115(9) 0.0023(8) -0.0001(8) 0.0005(8) C6 0.0205(11) 0.0152(10) 0.0123(9) 0.0007(8) 0.0029(8) 0.0114(9) C7 0.0202(12) 0.0254(12) 0.0213(11) 0.0027(9) 0.0008(9) 0.0123(9) C8 0.0353(14) 0.0368(14) 0.0217(12) 0.0018(10) -0.0053(10) 0.0246(12) C9 0.0540(17) 0.0315(13) 0.0145(11) 0.0068(9) 0.0052(10) 0.0301(12) C10 0.0383(14) 0.0204(11) 0.0200(11) 0.0069(9) 0.0129(10) 0.0154(10) C11 0.0230(12) 0.0169(10) 0.0161(10) 0.0019(8) 0.0052(8) 0.0105(9) C12 0.0158(11) 0.0252(11) 0.0167(10) 0.0029(9) 0.0031(8) 0.0052(9) C13 0.0205(12) 0.0221(11) 0.0184(11) 0.0060(9) 0.0029(9) 0.0051(9) C14 0.0303(13) 0.0269(12) 0.0157(10) -0.0022(9) -0.0007(9) 0.0168(10) C15 0.0215(12) 0.0227(11) 0.0284(12) 0.0042(9) 0.0091(9) 0.0094(9) C16 0.0277(13) 0.0191(11) 0.0217(11) 0.0010(9) 0.0044(9) 0.0122(10) C17 0.0170(11) 0.0200(11) 0.0292(12) 0.0000(9) -0.0040(9) 0.0036(9) O1 0.0186(8) 0.0162(7) 0.0199(7) 0.0021(6) -0.0020(6) 0.0083(6) F1 0.0372(8) 0.0276(7) 0.0242(7) 0.0032(5) 0.0120(6) 0.0191(6) F2 0.0163(7) 0.0375(8) 0.0310(7) 0.0040(6) 0.0105(5) 0.0048(6) F3 0.0301(8) 0.0401(8) 0.0137(6) -0.0053(5) -0.0005(5) 0.0145(6) F4 0.0234(7) 0.0424(8) 0.0271(7) 0.0185(6) 0.0111(6) 0.0054(6) F5 0.0277(7) 0.0382(8) 0.0151(6) 0.0037(5) -0.0036(5) 0.0101(6) F6 0.0453(9) 0.0265(7) 0.0263(7) 0.0149(6) 0.0056(6) 0.0143(6) Si1 0.0158(3) 0.0144(3) 0.0128(3) 0.0010(2) 0.0018(2) 0.0072(2) P1 0.0166(3) 0.0103(3) 0.0129(3) 0.00160(19) -0.0006(2) 0.0035(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 C1 C2 1.388(3) . ? C1 P1 1.7320(19) . ? C1 Si1 1.900(2) . ? C2 C3 1.413(3) . ? C2 C6 1.494(3) . ? C3 C4 1.376(3) . ? C3 H3 0.9500 . ? C4 C5 1.413(3) . ? C4 C12 1.513(3) . ? C5 C13 1.485(3) . ? C5 P1 1.728(2) . ? C6 C11 1.390(3) . ? C6 C7 1.394(3) . ? C7 C8 1.388(3) . ? C7 H7 0.9500 . ? C8 C9 1.380(4) . ? C8 H8 0.9500 . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.388(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 F3 1.337(2) . ? C12 F2 1.343(2) . ? C12 F1 1.343(2) . ? C13 F4 1.338(2) . ? C13 F6 1.356(2) . ? C13 F5 1.355(2) . ? C14 Si1 1.864(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 Si1 1.867(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 Si1 1.869(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O1 1.448(2) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O1 P1 1.6028(15) . ? P1 H1 1.28(2) . ? 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 C1 P1 117.94(15) . . ? C2 C1 Si1 125.33(14) . . ? P1 C1 Si1 116.67(11) . . ? C1 C2 C3 125.14(18) . . ? C1 C2 C6 120.49(17) . . ? C3 C2 C6 114.36(17) . . ? C4 C3 C2 124.55(18) . . ? C4 C3 H3 117.7 . . ? C2 C3 H3 117.7 . . ? C3 C4 C5 124.03(18) . . ? C3 C4 C12 115.15(18) . . ? C5 C4 C12 120.82(17) . . ? C4 C5 C13 124.94(18) . . ? C4 C5 P1 118.52(14) . . ? C13 C5 P1 116.29(15) . . ? C11 C6 C7 119.23(19) . . ? C11 C6 C2 120.71(18) . . ? C7 C6 C2 120.02(18) . . ? C8 C7 C6 120.0(2) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 120.3(2) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.2(2) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 119.8(2) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C6 C11 C10 120.5(2) . . ? C6 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? F3 C12 F2 107.25(16) . . ? F3 C12 F1 105.92(16) . . ? F2 C12 F1 105.38(17) . . ? F3 C12 C4 112.76(17) . . ? F2 C12 C4 112.28(17) . . ? F1 C12 C4 112.71(16) . . ? F4 C13 F6 106.22(17) . . ? F4 C13 F5 105.78(16) . . ? F6 C13 F5 104.77(17) . . ? F4 C13 C5 114.51(18) . . ? F6 C13 C5 110.88(17) . . ? F5 C13 C5 113.92(17) . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C17 O1 P1 118.35(12) . . ? C14 Si1 C15 110.54(11) . . ? C14 Si1 C16 107.39(10) . . ? C15 Si1 C16 108.56(10) . . ? C14 Si1 C1 112.65(9) . . ? C15 Si1 C1 109.47(9) . . ? C16 Si1 C1 108.11(9) . . ? O1 P1 C5 113.97(8) . . ? O1 P1 C1 112.18(9) . . ? C5 P1 C1 108.23(10) . . ? O1 P1 H1 95.9(9) . . ? C5 P1 H1 112.1(9) . . ? C1 P1 H1 114.2(9) . . ? 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 P1 C1 C2 C3 5.8(3) . . . . ? Si1 C1 C2 C3 -177.01(15) . . . . ? P1 C1 C2 C6 -174.20(14) . . . . ? Si1 C1 C2 C6 3.0(3) . . . . ? C1 C2 C3 C4 1.4(3) . . . . ? C6 C2 C3 C4 -178.53(18) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? C2 C3 C4 C12 179.35(18) . . . . ? C3 C4 C5 C13 176.91(19) . . . . ? C12 C4 C5 C13 -2.1(3) . . . . ? C3 C4 C5 P1 -9.0(3) . . . . ? C12 C4 C5 P1 172.01(14) . . . . ? C1 C2 C6 C11 75.8(2) . . . . ? C3 C2 C6 C11 -104.3(2) . . . . ? C1 C2 C6 C7 -106.4(2) . . . . ? C3 C2 C6 C7 73.6(2) . . . . ? C11 C6 C7 C8 -2.1(3) . . . . ? C2 C6 C7 C8 -179.98(18) . . . . ? C6 C7 C8 C9 1.9(3) . . . . ? C7 C8 C9 C10 -0.2(3) . . . . ? C8 C9 C10 C11 -1.4(3) . . . . ? C7 C6 C11 C10 0.5(3) . . . . ? C2 C6 C11 C10 178.41(18) . . . . ? C9 C10 C11 C6 1.2(3) . . . . ? C3 C4 C12 F3 137.75(18) . . . . ? C5 C4 C12 F3 -43.2(3) . . . . ? C3 C4 C12 F2 -101.0(2) . . . . ? C5 C4 C12 F2 78.1(2) . . . . ? C3 C4 C12 F1 17.9(2) . . . . ? C5 C4 C12 F1 -163.07(17) . . . . ? C4 C5 C13 F4 -42.1(3) . . . . ? P1 C5 C13 F4 143.76(15) . . . . ? C4 C5 C13 F6 -162.21(18) . . . . ? P1 C5 C13 F6 23.6(2) . . . . ? C4 C5 C13 F5 79.9(3) . . . . ? P1 C5 C13 F5 -94.29(19) . . . . ? C17 O1 P1 C5 62.49(17) . . . . ? C17 O1 P1 C1 -60.95(16) . . . . ? C4 C5 P1 O1 -111.68(15) . . . . ? C13 C5 P1 O1 62.91(17) . . . . ? C4 C5 P1 C1 13.87(18) . . . . ? C13 C5 P1 C1 -171.55(15) . . . . ? C2 C1 P1 O1 114.28(15) . . . . ? Si1 C1 P1 O1 -63.13(12) . . . . ? C2 C1 P1 C5 -12.32(18) . . . . ? Si1 C1 P1 C5 170.27(10) . . . . ? _refine_diff_density_max 0.360 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.057 _shelx_res_file ; MR336_a.res created by SHELXL-2014/7 TITL MR336_a.res in P-1 REM Old TITL MR336 in P-1 REM SHELXT solution in P-1 REM R1 0.107, Rweak 0.009, Alpha 0.044, Orientation as input REM Formula found by SHELXT: C17 O F6 Si P CELL 0.71073 8.9992 10.1647 11.3907 99.1849 91.1844 112.8005 ZERR 2.000 0.0002 0.0003 0.0003 0.0011 0.0010 0.0009 LATT 1 SFAC C H O F SI P UNIT 34 38 2 12 2 2 TEMP -173.120 SIZE 0.09 0.21 0.28 L.S. 30 BOND $H LIST 6 acta conf FMAP 2 PLAN 20 WGHT 0.034600 0.720300 FVAR 0.94017 C1 1 0.697942 0.328726 0.676401 11.00000 0.01199 0.01176 = 0.01320 0.00179 0.00099 0.00187 H1 2 0.707418 0.524710 0.559754 11.00000 0.01640 C2 1 0.767191 0.227582 0.670489 11.00000 0.00865 0.01266 = 0.01230 0.00073 -0.00113 0.00014 C3 1 0.831213 0.177816 0.568750 11.00000 0.01446 0.01474 = 0.01586 0.00075 -0.00048 0.00543 AFIX 43 H3 2 0.873432 0.106475 0.574585 11.00000 -1.20000 AFIX 0 C4 1 0.836647 0.225503 0.461847 11.00000 0.01038 0.01540 = 0.01443 0.00058 0.00064 0.00129 C5 1 0.779276 0.331451 0.440287 11.00000 0.01358 0.01589 = 0.01151 0.00231 -0.00007 0.00054 C6 1 0.778976 0.161787 0.776730 11.00000 0.02050 0.01515 = 0.01235 0.00073 0.00290 0.01138 C7 1 0.928147 0.203787 0.841542 11.00000 0.02021 0.02545 = 0.02134 0.00269 0.00084 0.01231 AFIX 43 H7 2 1.022323 0.274293 0.818142 11.00000 -1.20000 AFIX 0 C8 1 0.939103 0.142636 0.940223 11.00000 0.03531 0.03677 = 0.02174 0.00182 -0.00532 0.02459 AFIX 43 H8 2 1.040255 0.173587 0.985704 11.00000 -1.20000 AFIX 0 C9 1 0.803594 0.037002 0.972565 11.00000 0.05399 0.03153 = 0.01450 0.00683 0.00520 0.03008 AFIX 43 H9 2 0.811835 -0.004726 1.040055 11.00000 -1.20000 AFIX 0 C10 1 0.655806 -0.008246 0.906927 11.00000 0.03832 0.02038 = 0.02002 0.00693 0.01290 0.01537 AFIX 43 H10 2 0.563126 -0.082429 0.928236 11.00000 -1.20000 AFIX 0 C11 1 0.643312 0.055031 0.809862 11.00000 0.02299 0.01689 = 0.01614 0.00194 0.00522 0.01054 AFIX 43 H11 2 0.541375 0.025198 0.765765 11.00000 -1.20000 AFIX 0 C12 1 0.912494 0.157766 0.365882 11.00000 0.01581 0.02520 = 0.01668 0.00290 0.00307 0.00522 C13 1 0.791046 0.389620 0.327698 11.00000 0.02053 0.02208 = 0.01840 0.00595 0.00292 0.00513 C14 1 0.747656 0.427087 0.954417 11.00000 0.03028 0.02689 = 0.01568 -0.00224 -0.00067 0.01683 AFIX 137 H14A 2 0.730765 0.331892 0.973411 11.00000 -1.50000 H14B 2 0.717089 0.483467 1.020281 11.00000 -1.50000 H14C 2 0.861979 0.478811 0.942912 11.00000 -1.50000 AFIX 0 C15 1 0.405995 0.279668 0.825216 11.00000 0.02151 0.02267 = 0.02841 0.00419 0.00906 0.00938 AFIX 137 H15A 2 0.338989 0.275241 0.754578 11.00000 -1.50000 H15B 2 0.366453 0.317105 0.897157 11.00000 -1.50000 H15C 2 0.399978 0.182179 0.829320 11.00000 -1.50000 AFIX 0 C16 1 0.626955 0.584890 0.799341 11.00000 0.02773 0.01912 = 0.02171 0.00096 0.00445 0.01216 AFIX 137 H16A 2 0.739407 0.651617 0.796817 11.00000 -1.50000 H16B 2 0.581276 0.622450 0.867663 11.00000 -1.50000 H16C 2 0.563577 0.576231 0.725378 11.00000 -1.50000 AFIX 0 C17 1 0.383080 0.185408 0.474955 11.00000 0.01695 0.01995 = 0.02917 -0.00001 -0.00400 0.00356 AFIX 137 H17A 2 0.272340 0.169245 0.493962 11.00000 -1.50000 H17B 2 0.425891 0.132969 0.521919 11.00000 -1.50000 H17C 2 0.382716 0.150000 0.389680 11.00000 -1.50000 AFIX 0 O1 3 0.484016 0.339131 0.503486 11.00000 0.01863 0.01616 = 0.01989 0.00207 -0.00195 0.00835 F1 4 0.919830 0.034510 0.388313 11.00000 0.03716 0.02757 = 0.02424 0.00319 0.01203 0.01913 F2 4 1.065857 0.245493 0.355024 11.00000 0.01633 0.03747 = 0.03098 0.00404 0.01053 0.00482 F3 4 0.830991 0.123157 0.258349 11.00000 0.03010 0.04013 = 0.01371 -0.00535 -0.00047 0.01447 F4 4 0.932859 0.417297 0.280900 11.00000 0.02337 0.04239 = 0.02706 0.01852 0.01109 0.00543 F5 4 0.676244 0.301677 0.239158 11.00000 0.02766 0.03817 = 0.01513 0.00369 -0.00362 0.01009 F6 4 0.770055 0.516168 0.345008 11.00000 0.04526 0.02652 = 0.02634 0.01486 0.00560 0.01428 SI1 5 0.620486 0.402534 0.814914 11.00000 0.01579 0.01436 = 0.01282 0.00103 0.00176 0.00721 P1 6 0.671472 0.387975 0.546229 11.00000 0.01656 0.01032 = 0.01288 0.00160 -0.00064 0.00353 HKLF 4 REM MR336_a.res in P-1 REM R1 = 0.0391 for 3092 Fo > 4sig(Fo) and 0.0578 for all 3879 data REM 243 parameters refined using 0 restraints END WGHT 0.0319 0.7372 REM Highest difference peak 0.360, deepest hole -0.330, 1-sigma level 0.057 Q1 1 0.6150 0.5029 0.7964 11.00000 0.05 0.36 Q2 1 0.6642 0.3505 0.7344 11.00000 0.05 0.33 Q3 1 0.7673 0.3481 0.3841 11.00000 0.05 0.32 Q4 1 0.3011 0.1636 0.4169 11.00000 0.05 0.31 Q5 1 0.7106 0.3412 0.4732 11.00000 0.05 0.31 Q6 1 0.7096 0.3742 0.6197 11.00000 0.05 0.30 Q7 1 0.8753 0.2021 0.4167 11.00000 0.05 0.30 Q8 1 0.8399 0.2410 0.6193 11.00000 0.05 0.29 Q9 1 0.6812 0.4189 0.8964 11.00000 0.05 0.27 Q10 1 0.7541 0.1794 0.7187 11.00000 0.05 0.26 Q11 1 0.4996 0.3321 0.8053 11.00000 0.05 0.25 Q12 1 0.6633 0.0165 0.8456 11.00000 0.05 0.24 Q13 1 0.4769 0.1039 0.4270 11.00000 0.05 0.24 Q14 1 0.7057 0.2548 0.6637 11.00000 0.05 0.24 Q15 1 0.4311 0.1357 0.4530 11.00000 0.05 0.23 Q16 1 0.8068 0.1733 0.5056 11.00000 0.05 0.23 Q17 1 0.7673 0.1846 0.6192 11.00000 0.05 0.23 Q18 1 0.8489 0.3017 0.4455 11.00000 0.05 0.22 Q19 1 0.9131 0.1772 0.9003 11.00000 0.05 0.22 Q20 1 0.7223 0.0963 0.7745 11.00000 0.05 0.21 ; _shelx_res_checksum 41510 _shelx_hkl_file ; -1 0 0 18.60 2.70 1 0 0 14.70 2.30 -2 0 0 2777.32 46.90 2 0 0 2814.82 47.70 -3 0 0 735.03 21.80 3 0 0 750.02 23.00 -4 0 0 794.92 26.00 4 0 0 793.32 18.30 4 0 0 824.22 28.00 4 0 0 837.42 15.40 5 0 0 6.80 8.20 5 0 0 7.80 3.50 5 0 0 4.40 4.60 6 0 0 3.00 3.80 6 0 0 -1.20 10.10 6 0 0 9.00 5.40 6 0 0 -2.40 5.50 7 0 0 1928.61 37.50 7 0 0 1834.52 38.20 7 0 0 1800.62 58.69 7 0 0 1895.11 34.10 8 0 0 86.59 11.30 8 0 0 119.39 24.00 8 0 0 111.59 13.10 8 0 0 95.49 10.60 9 0 0 53.29 11.90 9 0 0 43.30 22.90 9 0 0 27.80 8.80 9 0 0 50.09 14.10 10 0 0 -15.50 30.90 10 0 0 24.40 17.20 10 0 0 -8.20 17.50 10 0 0 3.60 11.10 10 -1 0 62.19 29.50 10 -1 0 72.19 15.60 10 -1 0 50.39 17.90 9 -1 0 -23.30 25.10 9 -1 0 19.50 10.80 9 -1 0 0.30 10.50 8 -1 0 0.50 15.20 8 -1 0 -0.30 7.80 7 -1 0 43.50 7.80 6 -1 0 47.70 11.80 6 -1 0 49.30 7.20 5 -1 0 337.47 20.00 5 -1 0 352.76 12.90 4 -1 0 867.41 26.80 4 -1 0 895.71 19.30 3 -1 0 0.80 4.10 3 -1 0 3.30 2.30 2 -1 0 138.59 5.20 -2 1 0 135.49 5.20 1 -1 0 2106.69 32.50 1 -1 0 2379.16 32.00 1 -1 0 2421.56 33.70 -1 1 0 2310.27 31.70 -1 1 0 2355.36 31.60 -1 1 0 2476.85 33.80 -2 -1 0 2912.71 42.50 -2 -1 0 3030.20 53.29 2 1 0 2974.80 43.80 2 1 0 2931.61 44.80 2 1 0 3032.10 53.29 -3 -1 0 2972.50 57.39 3 1 0 2993.40 45.10 3 1 0 2936.71 58.09 3 1 0 2963.60 46.50 -4 -1 0 -4.60 6.60 4 1 0 0.50 3.20 4 1 0 -9.00 7.20 4 1 0 1.60 4.20 -5 -1 0 236.48 19.20 5 1 0 252.97 20.70 5 1 0 266.77 12.90 5 1 0 281.87 10.80 -6 -1 0 41.80 13.30 6 1 0 25.30 8.40 6 1 0 30.20 6.00 6 1 0 33.10 12.60 6 1 0 31.70 7.60 7 1 0 325.97 19.60 7 1 0 357.56 16.80 7 1 0 321.97 14.70 8 1 0 207.68 17.50 8 1 0 218.28 21.10 8 1 0 214.68 15.10 9 1 0 68.29 13.40 9 1 0 96.99 32.10 9 1 0 74.19 12.30 9 1 0 76.19 17.50 10 -2 0 -0.70 25.20 10 -2 0 68.99 15.20 9 -2 0 42.60 20.60 9 -2 0 14.70 10.70 8 -2 0 24.20 8.80 8 -2 0 24.50 16.60 7 -2 0 60.19 9.40 7 -2 0 67.39 16.00 6 -2 0 22.30 6.10 6 -2 0 6.90 9.60 5 -2 0 51.59 10.50 5 -2 0 28.40 5.50 4 -2 0 991.50 21.70 -4 2 0 1007.20 21.90 3 -2 0 94.19 5.80 -3 2 0 90.49 5.70 2 -2 0 7157.18 95.99 2 -2 0 7139.79 98.99 2 -2 0 7067.19 95.79 -2 2 0 7203.88 98.99 1 -2 0 136.49 5.20 1 -2 0 129.89 5.70 -1 2 0 130.59 5.40 -1 2 0 135.59 5.30 -1 2 0 133.09 5.00 0 -2 0 197.08 6.80 0 -2 0 193.88 7.60 0 2 0 203.28 6.90 0 2 0 195.38 7.70 -1 -2 0 660.03 15.90 -1 -2 0 669.53 14.70 -1 -2 0 662.33 19.40 1 2 0 679.33 14.90 1 2 0 668.63 16.40 -2 -2 0 2365.96 38.90 -2 -2 0 2303.47 37.40 -2 -2 0 2312.87 47.60 2 2 0 2310.67 47.70 2 2 0 2344.87 40.50 2 2 0 2361.36 38.50 -3 -2 0 233.18 8.80 -3 -2 0 261.07 16.50 3 2 0 223.98 11.90 3 2 0 234.08 9.80 3 2 0 259.17 17.00 -4 -2 0 1018.50 34.60 -4 -2 0 1058.79 19.60 4 2 0 1020.30 25.90 4 2 0 1040.40 23.30 4 2 0 1042.50 35.90 -5 -2 0 216.18 20.10 5 2 0 259.37 22.80 5 2 0 205.48 14.40 5 2 0 225.58 11.40 -6 -2 0 50.09 14.20 6 2 0 52.09 11.30 6 2 0 50.09 8.00 6 2 0 82.69 18.70 -7 -2 0 16.50 17.10 7 2 0 5.60 11.50 7 2 0 21.40 8.40 7 2 0 25.80 9.50 8 2 0 132.09 14.00 8 2 0 142.09 18.30 8 2 0 107.59 13.90 9 2 0 43.10 21.20 9 2 0 56.49 36.30 9 2 0 42.50 12.90 9 2 0 28.90 13.90 11 -3 0 34.20 18.00 11 -3 0 20.50 35.50 10 -3 0 200.98 22.40 10 -3 0 151.88 30.90 9 -3 0 226.88 19.00 9 -3 0 218.68 29.10 8 -3 0 12.70 8.10 8 -3 0 -7.70 13.90 7 -3 0 36.80 8.60 7 -3 0 34.40 13.30 6 -3 0 4.70 5.60 6 -3 0 22.40 8.70 -6 3 0 0.80 4.90 5 -3 0 479.35 15.90 -5 3 0 464.75 15.70 4 -3 0 999.60 17.10 4 -3 0 942.41 22.20 -4 3 0 958.80 22.30 3 -3 0 24.10 3.40 3 -3 0 29.60 4.70 3 -3 0 28.30 3.80 -3 3 0 32.50 4.80 2 -3 0 8.10 3.20 2 -3 0 10.50 2.70 -2 3 0 6.10 2.50 -2 3 0 7.40 2.20 -2 3 0 10.20 2.70 1 -3 0 9859.41 138.29 1 -3 0 9962.70 136.29 -1 3 0 9867.81 135.59 -1 3 0 9999.00 137.69 0 -3 0 242.88 9.30 0 -3 0 230.28 10.10 0 3 0 220.78 10.00 0 3 0 232.08 8.80 -1 -3 0 9.60 3.90 -1 -3 0 7.20 3.70 -1 -3 0 4.70 5.10 1 3 0 10.30 3.40 1 3 0 7.30 4.40 -2 -3 0 -3.10 6.10 -2 -3 0 4.50 3.60 -2 -3 0 4.90 4.30 2 3 0 -0.60 3.60 2 3 0 -2.00 4.90 -3 -3 0 3330.07 53.69 -3 -3 0 3324.77 69.49 -3 -3 0 3367.46 54.89 3 3 0 3285.77 69.89 3 3 0 3394.16 56.09 3 3 0 3328.27 59.59 -4 -3 0 336.57 12.40 -4 -3 0 370.96 24.00 4 3 0 360.16 18.10 4 3 0 334.97 14.20 4 3 0 351.46 23.80 -5 -3 0 322.77 25.60 5 3 0 328.57 15.40 5 3 0 332.17 19.50 5 3 0 256.37 31.00 -6 -3 0 943.31 42.60 6 3 0 901.51 26.60 6 3 0 914.41 31.60 -7 -3 0 13.10 19.20 7 3 0 4.80 10.20 7 3 0 21.80 15.70 8 3 0 19.30 12.90 8 3 0 54.39 18.90 8 3 0 24.50 29.70 8 3 0 42.20 13.40 11 -4 0 -29.40 36.50 11 -4 0 67.99 18.20 10 -4 0 144.69 17.90 10 -4 0 104.19 30.60 9 -4 0 13.30 11.10 9 -4 0 40.60 21.20 8 -4 0 -4.30 13.10 8 -4 0 -9.10 7.30 7 -4 0 4.80 10.50 7 -4 0 -1.80 6.10 -7 4 0 14.90 7.20 6 -4 0 207.38 13.00 6 -4 0 242.38 9.30 -6 4 0 233.68 13.10 5 -4 0 102.39 9.30 5 -4 0 113.79 7.00 5 -4 0 113.89 6.80 -5 4 0 102.89 9.20 4 -4 0 22.10 4.50 4 -4 0 28.80 4.40 4 -4 0 29.00 6.20 -4 4 0 24.50 5.40 3 -4 0 73.89 6.80 3 -4 0 68.59 6.40 -3 4 0 65.59 5.20 -3 4 0 50.49 6.20 -3 4 0 68.29 5.10 2 -4 0 666.33 16.90 2 -4 0 666.03 18.30 -2 4 0 664.33 15.80 -2 4 0 660.33 17.00 -2 4 0 645.74 17.10 1 -4 0 675.73 17.70 -1 4 0 663.53 18.90 -1 4 0 704.73 17.30 0 -4 0 615.14 17.50 0 -4 0 600.84 19.20 0 4 0 634.14 19.50 0 4 0 607.64 17.00 -1 -4 0 341.67 18.30 -1 -4 0 341.07 15.20 -1 -4 0 341.57 13.50 1 4 0 347.77 15.70 1 4 0 322.27 13.00 -2 -4 0 112.09 10.50 -2 -4 0 119.39 9.60 -2 -4 0 114.99 14.80 2 4 0 128.89 9.50 2 4 0 122.29 12.00 -3 -4 0 353.16 15.80 -3 -4 0 360.66 14.50 -3 -4 0 374.96 23.20 3 4 0 344.37 15.00 3 4 0 322.37 17.70 -4 -4 0 256.67 13.10 -4 -4 0 238.88 23.20 4 4 0 240.98 14.40 4 4 0 231.08 17.80 -5 -4 0 23.90 7.40 -5 -4 0 11.30 14.90 -5 -4 0 23.50 7.10 5 4 0 59.49 13.50 5 4 0 38.70 9.00 -6 -4 0 276.07 32.80 6 4 0 286.47 19.30 6 4 0 299.97 24.90 -7 -4 0 43.80 23.80 7 4 0 47.10 13.90 7 4 0 75.29 18.50 -8 -4 0 21.70 30.50 8 4 0 8.20 22.80 8 4 0 32.20 15.40 8 4 0 1.70 15.00 11 -5 0 24.60 17.90 11 -5 0 79.99 44.70 10 -5 0 39.50 26.40 10 -5 0 18.70 14.30 9 -5 0 227.38 19.50 9 -5 0 260.87 32.80 8 -5 0 17.40 6.60 8 -5 0 17.10 14.40 -8 5 0 13.70 9.50 7 -5 0 285.77 11.70 7 -5 0 296.97 16.80 7 -5 0 287.57 12.30 -7 5 0 294.97 17.00 6 -5 0 1.70 5.90 6 -5 0 -4.30 4.40 6 -5 0 2.90 4.80 -6 5 0 0.30 5.90 5 -5 0 55.69 7.40 5 -5 0 48.30 6.70 -5 5 0 47.40 7.60 4 -5 0 687.93 19.60 4 -5 0 675.73 18.30 -4 5 0 661.33 14.90 -4 5 0 662.93 14.60 -4 5 0 685.13 20.40 3 -5 0 283.07 13.20 3 -5 0 277.57 12.10 -3 5 0 298.77 12.90 -3 5 0 300.37 10.80 -3 5 0 297.07 11.80 2 -5 0 87.99 9.50 2 -5 0 89.99 8.60 -2 5 0 88.69 8.90 -2 5 0 88.59 7.30 -2 5 0 63.59 7.30 1 -5 0 293.77 13.10 1 -5 0 265.27 14.30 -1 5 0 297.37 12.30 -1 5 0 290.37 14.20 0 -5 0 1997.00 39.70 0 -5 0 1967.10 42.70 0 5 0 2003.20 42.70 0 5 0 2006.60 39.20 -1 -5 0 207.38 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_shelx_hkl_checksum 4690 #=================================================================== _publ_requested_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 ; 'Weber, Manuela' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_section_title ; ... see the published paper. ; _publ_section_abstract ; ... and following paragraphs: see the published paper. ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #END===============================================