# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global #TrackingRef 'web_deposit_cif_file_0_Prof.Dr.ThomasStrassner_1366622569.bimetallic_dalton_strassner_revision.cif' #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'Sep 05 10:34:21 2012' _audit_creation_method 'PLATON option' _audit_update_record ; 05-Sept-12 Updated by the Author A.T Text writing by A.T. Checkcif ok 14-Nov-12 Updated by the Author A.T. 16-Nov-12 Updated by the Author A.T. 20-Mar-13 Updated by the Author A.T. 09-Apr-13 Updated by the Author A.T. ; #=============================================================================== data_compound_2b #TrackingRef 'web_deposit_cif_file_0_Prof.Dr.ThomasStrassner_1366622569.bimetallic_dalton_strassner_revision.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 N4, 2(Br)' _chemical_formula_sum 'C26 H24 Br2 N4' _chemical_formula_weight 552.31 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' Br Br -0.2901 2.4595 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 12.301(3) _cell_length_b 8.9810(18) _cell_length_c 11.865(2) _cell_angle_alpha 90 _cell_angle_beta 112.87(3) _cell_angle_gamma 90 _cell_volume 1207.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 198 _cell_measurement_reflns_used 328 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 25.51 _cell_special_details ; ; _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.750 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 556 _exptl_absorpt_coefficient_mu 3.377 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10.(Sheldrick,Bruker AXS Inc.,2002)' _exptl_absorpt_correction_T_min 0.173 _exptl_absorpt_correction_T_max 0.635 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Diffractometer operator A. Tronnier scanspeed 15 s per frame dx 30 mm ; _diffrn_ambient_temperature 198 _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method \f _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_wavelength_id x-ray # number of measured reflections (redundant set) _diffrn_reflns_number 19823 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 25.51 _diffrn_reflns_theta_full 25.51 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 2193 # number of observed reflections (> n sig(I)) _reflns_number_gt 1566 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius BV, 1999)' _computing_cell_refinement 'Dirax/lsq (Duisenberg, 1992)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)' _computing_molecular_graphics 'PLATON (Spek, 2011), ORTEP (Farrugia, L. J. 1997), MERCURY (van de Streek, J. 2006)' _computing_publication_material 'PLATON (Spek, 2011), enCIFer (Allen, 2004)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0256P)^2^+2.2519P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 2193 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.381 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.088 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N Uani 0.8732(2) 0.9884(3) 0.6529(2) 1.000 0.0212(8) d . . . N2 N Uani 0.7808(3) 0.8990(3) 0.7596(3) 1.000 0.0244(10) d . . . C1 C Uani 0.8350(3) 0.8633(4) 0.6868(3) 1.000 0.0244(11) d . . . C2 C Uani 0.7844(4) 1.0520(4) 0.7737(4) 1.000 0.0302(11) d . . . C3 C Uani 0.8419(3) 1.1080(4) 0.7077(3) 1.000 0.0277(11) d . . . C4 C Uani 0.9384(3) 0.9944(4) 0.5752(3) 1.000 0.0197(9) d . . . C5 C Uani 0.9805(3) 0.8639(4) 0.5441(3) 1.000 0.0242(11) d . . . C6 C Uani 1.0415(3) 0.8696(4) 0.4680(3) 1.000 0.0215(11) d . . . C7 C Uani 0.7208(3) 0.7935(4) 0.8114(3) 1.000 0.0284(12) d . . . C8 C Uani 0.5913(3) 0.8276(4) 0.7697(3) 1.000 0.0276(11) d . . . C9 C Uani 0.5165(5) 0.8142(6) 0.6492(4) 1.000 0.0625(19) d . . . C10 C Uani 0.3964(5) 0.8440(7) 0.6140(5) 1.000 0.076(2) d . . . C11 C Uani 0.3527(4) 0.8866(5) 0.6980(5) 1.000 0.0543(19) d . . . C12 C Uani 0.4254(4) 0.9002(6) 0.8157(5) 1.000 0.0577(19) d . . . C13 C Uani 0.5448(4) 0.8709(5) 0.8520(4) 1.000 0.0424(16) d . . . Br1 Br Uani 0.84507(3) 1.00815(4) 0.10861(3) 1.000 0.0281(1) d . . . H1 H Uiso 0.84520 0.76520 0.66250 1.000 0.0290 c R . . H2 H Uiso 0.75200 1.10740 0.82140 1.000 0.0360 c R . . H3 H Uiso 0.85810 1.21010 0.70000 1.000 0.0330 c R . . H5 H Uiso 0.96730 0.77100 0.57500 1.000 0.0290 c R . . H6 H Uiso 1.06960 0.78060 0.44550 1.000 0.0260 c R . . H7A H Uiso 0.75790 0.79820 0.90180 1.000 0.0340 c R . . H7B H Uiso 0.73090 0.69110 0.78620 1.000 0.0340 c R . . H9 H Uiso 0.54630 0.78470 0.58990 1.000 0.0750 c R . . H10 H Uiso 0.34470 0.83440 0.53050 1.000 0.0900 c R . . H11 H Uiso 0.27080 0.90660 0.67340 1.000 0.0660 c R . . H12 H Uiso 0.39500 0.93020 0.87450 1.000 0.0700 c R . . H13 H Uiso 0.59530 0.88120 0.93580 1.000 0.0510 c 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 N1 0.0225(14) 0.0194(15) 0.0230(14) -0.0007(13) 0.0104(12) 0.0021(13) N2 0.0283(18) 0.0207(16) 0.0288(17) 0.0010(13) 0.0162(15) -0.0002(13) C1 0.025(2) 0.0216(19) 0.030(2) -0.0043(16) 0.0145(18) 0.0011(15) C2 0.044(2) 0.0217(19) 0.034(2) -0.0006(16) 0.025(2) 0.0053(17) C3 0.039(2) 0.0183(18) 0.030(2) -0.0040(16) 0.018(2) 0.0021(16) C4 0.0176(15) 0.0233(18) 0.0182(16) -0.0007(17) 0.0070(13) 0.0001(16) C5 0.025(2) 0.0189(19) 0.028(2) 0.0015(16) 0.0095(18) 0.0003(15) C6 0.0238(19) 0.0167(18) 0.026(2) -0.0030(15) 0.0119(18) 0.0034(15) C7 0.033(2) 0.027(2) 0.030(2) 0.0045(17) 0.0174(18) 0.0006(17) C8 0.028(2) 0.0236(19) 0.033(2) 0.0015(17) 0.0139(18) -0.0026(16) C9 0.053(3) 0.094(4) 0.038(3) -0.014(3) 0.015(3) 0.004(3) C10 0.049(3) 0.100(5) 0.049(3) -0.005(3) -0.012(3) -0.002(3) C11 0.031(3) 0.038(3) 0.086(4) -0.001(3) 0.014(3) -0.006(2) C12 0.037(3) 0.070(3) 0.077(4) -0.010(3) 0.034(3) -0.001(3) C13 0.032(2) 0.059(3) 0.039(3) -0.005(2) 0.017(2) 0.001(2) Br1 0.0328(2) 0.0194(2) 0.0322(2) 0.0002(2) 0.0127(2) -0.0006(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.339(5) . . yes N1 C3 1.385(4) . . yes N1 C4 1.439(4) . . yes N2 C1 1.320(5) . . yes N2 C2 1.383(5) . . yes N2 C7 1.474(5) . . yes C2 C3 1.341(6) . . no C4 C5 1.388(5) . . no C4 C6 1.384(5) . 3_776 no C5 C6 1.381(5) . . no C7 C8 1.505(5) . . no C8 C9 1.372(6) . . no C8 C13 1.366(6) . . no C9 C10 1.396(9) . . no C10 C11 1.358(8) . . no C11 C12 1.340(8) . . no C12 C13 1.386(8) . . no C1 H1 0.9500 . . no C2 H2 0.9500 . . no C3 H3 0.9500 . . no C5 H5 0.9500 . . no C6 H6 0.9500 . . no C7 H7A 0.9900 . . no C7 H7B 0.9900 . . no C9 H9 0.9500 . . no C10 H10 0.9500 . . no C11 H11 0.9500 . . no C12 H12 0.9500 . . no C13 H13 0.9500 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C3 108.4(3) . . . yes C1 N1 C4 124.9(3) . . . yes C3 N1 C4 126.7(3) . . . yes C1 N2 C2 108.7(3) . . . yes C1 N2 C7 125.4(3) . . . yes C2 N2 C7 125.9(4) . . . yes N1 C1 N2 108.6(3) . . . yes N2 C2 C3 107.6(4) . . . yes N1 C3 C2 106.8(3) . . . yes N1 C4 C5 119.8(3) . . . yes N1 C4 C6 119.7(3) . . 3_776 yes C5 C4 C6 120.5(3) . . 3_776 no C4 C5 C6 119.8(3) . . . no C4 C6 C5 119.7(3) 3_776 . . no N2 C7 C8 111.7(3) . . . yes C7 C8 C9 121.4(4) . . . no C7 C8 C13 120.5(3) . . . no C9 C8 C13 118.2(4) . . . no C8 C9 C10 119.9(5) . . . no C9 C10 C11 120.6(5) . . . no C10 C11 C12 119.8(5) . . . no C11 C12 C13 120.3(5) . . . no C8 C13 C12 121.3(4) . . . no N1 C1 H1 126.00 . . . no N2 C1 H1 126.00 . . . no N2 C2 H2 126.00 . . . no C3 C2 H2 126.00 . . . no N1 C3 H3 127.00 . . . no C2 C3 H3 127.00 . . . no C4 C5 H5 120.00 . . . no C6 C5 H5 120.00 . . . no C5 C6 H6 120.00 . . . no C4 C6 H6 120.00 3_776 . . no N2 C7 H7A 109.00 . . . no N2 C7 H7B 109.00 . . . no C8 C7 H7A 109.00 . . . no C8 C7 H7B 109.00 . . . no H7A C7 H7B 108.00 . . . no C8 C9 H9 120.00 . . . no C10 C9 H9 120.00 . . . no C9 C10 H10 120.00 . . . no C11 C10 H10 120.00 . . . no C10 C11 H11 120.00 . . . no C12 C11 H11 120.00 . . . no C11 C12 H12 120.00 . . . no C13 C12 H12 120.00 . . . no C8 C13 H13 119.00 . . . no C12 C13 H13 119.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N1 C1 N2 0.3(4) . . . . no C4 N1 C1 N2 178.8(3) . . . . no C1 N1 C4 C5 -9.2(5) . . . . no C3 N1 C4 C5 169.0(3) . . . . no C1 N1 C4 C6 170.7(3) . . . 3_776 no C3 N1 C4 C6 -11.1(5) . . . 3_776 no C1 N1 C3 C2 -0.3(4) . . . . no C4 N1 C3 C2 -178.7(3) . . . . no C2 N2 C1 N1 -0.2(4) . . . . no C7 N2 C2 C3 -176.8(4) . . . . no C7 N2 C1 N1 176.6(3) . . . . no C1 N2 C2 C3 0.1(5) . . . . no C1 N2 C7 C8 -118.4(4) . . . . no C2 N2 C7 C8 58.0(5) . . . . no N2 C2 C3 N1 0.2(5) . . . . no C6 C4 C5 C6 -0.9(5) 3_776 . . . no N1 C4 C5 C6 179.0(3) . . . . no N1 C4 C6 C5 -179.0(3) . . 3_776 3_776 no C5 C4 C6 C5 0.9(5) . . 3_776 3_776 no C4 C5 C6 C4 0.9(5) . . . 3_776 no N2 C7 C8 C9 65.5(5) . . . . no N2 C7 C8 C13 -115.5(4) . . . . no C7 C8 C9 C10 178.8(5) . . . . no C13 C8 C9 C10 -0.3(7) . . . . no C7 C8 C13 C12 -178.8(4) . . . . no C9 C8 C13 C12 0.2(7) . . . . no C8 C9 C10 C11 0.2(8) . . . . no C9 C10 C11 C12 0.0(8) . . . . no C10 C11 C12 C13 -0.1(8) . . . . no C11 C12 C13 C8 -0.1(8) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C1 H1 Br1 0.9500 2.5400 3.478(4) 171.00 4_565 yes C3 H3 Br1 0.9500 2.7300 3.647(4) 162.00 4_575 yes C6 H6 Br1 0.9500 2.8300 3.781(4) 177.00 2_745 yes _iucr_refine_instructions_details ; TITL str-512x in P2(1)/c CELL 0.71073 12.3010 8.9810 11.8650 90.000 112.872 90.000 ZERR 2.00 0.0025 0.0018 0.0024 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N Br UNIT 52 48 8 4 L.S. 18 ACTA BOND $H FMAP 2 PLAN 0 LIST 4 CONF SIZE 0.148 0.752 0.800 SHEL 99 0.825 WGHT 0.025400 2.256100 FVAR 0.414440 TEMP -75 Br1 4 0.845070 0.008149 0.108613 11.000000 0.032810 0.019360 = 0.032250 0.000160 0.012720 -0.000630 C1 1 0.835023 0.863286 0.686771 11.000000 0.025470 0.021560 = 0.029590 0.004280 0.014480 -0.001120 AFIX 43 H1 2 0.845250 0.765224 0.662505 11.000000 -1.200000 AFIX 0 C2 1 0.784410 1.052002 0.773679 11.000000 0.044020 0.021720 = 0.034140 0.000570 0.024980 -0.005340 AFIX 43 H2 2 0.752022 1.107379 0.821428 11.000000 -1.200000 AFIX 0 C3 1 0.841926 1.108011 0.707704 11.000000 0.039290 0.018270 = 0.029560 0.003970 0.018450 -0.002140 AFIX 43 H3 2 0.858142 1.210079 0.700029 11.000000 -1.200000 AFIX 0 C4 1 0.938446 0.994396 0.575245 11.000000 0.017570 0.023260 = 0.018230 0.000670 0.006990 -0.000150 C5 1 0.980460 0.863854 0.544093 11.000000 0.024930 0.018890 = 0.027910 -0.001530 0.009540 -0.000270 AFIX 43 H5 2 0.967291 0.770957 0.574953 11.000000 -1.200000 AFIX 0 C6 1 1.041508 0.869623 0.468017 11.000000 0.023820 0.016670 = 0.025810 0.002960 0.011890 -0.003370 AFIX 43 H6 2 1.069616 0.780567 0.445493 11.000000 -1.200000 AFIX 0 C7 1 0.720825 0.793502 0.811435 11.000000 0.033180 0.026910 = 0.030220 -0.004480 0.017430 -0.000560 AFIX 23 H7A 2 0.757873 0.798195 0.901842 11.000000 -1.200000 H7B 2 0.730864 0.691053 0.786213 11.000000 -1.200000 AFIX 0 C8 1 0.591258 0.827602 0.769725 11.000000 0.028200 0.023640 = 0.033000 -0.001490 0.013910 0.002620 C9 1 0.516459 0.814182 0.649229 11.000000 0.053040 0.094010 = 0.038420 0.013860 0.015100 -0.003650 AFIX 43 H9 2 0.546348 0.784656 0.589886 11.000000 -1.200000 AFIX 0 C10 1 0.396363 0.843989 0.613982 11.000000 0.049230 0.099660 = 0.048640 0.004630 -0.011940 0.001510 AFIX 43 H10 2 0.344744 0.834401 0.530517 11.000000 -1.200000 AFIX 0 C11 1 0.352654 0.886591 0.698005 11.000000 0.031310 0.038410 = 0.086460 0.001440 0.014160 0.006010 AFIX 43 H11 2 0.270817 0.906621 0.673388 11.000000 -1.200000 AFIX 0 C12 1 0.425399 0.900236 0.815676 11.000000 0.037210 0.070480 = 0.077130 0.009570 0.033580 0.000550 AFIX 43 H12 2 0.394976 0.930165 0.874502 11.000000 -1.200000 AFIX 0 C13 1 0.544765 0.870935 0.852049 11.000000 0.031650 0.059000 = 0.038530 0.004840 0.016600 -0.000570 AFIX 43 H13 2 0.595265 0.881166 0.935832 11.000000 -1.200000 AFIX 0 N1 3 0.873174 0.988391 0.652857 11.000000 0.022520 0.019450 = 0.022950 0.000710 0.010430 -0.002140 N2 3 0.780771 0.899041 0.759635 11.000000 0.028340 0.020680 = 0.028810 -0.000990 0.016200 0.000250 HKLF 4 END ; _database_code_depnum_ccdc_archive 'CCDC 930701' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global #TrackingRef 'web_deposit_cif_file_0_Prof.Dr.ThomasStrassner_1366622569.bimetallic_dalton_strassner_revision.cif' #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'Sep 05 10:34:21 2012' _audit_creation_method 'PLATON
option' _audit_update_record ; 05-Sept-12 Updated by the Author A.T Text writing by A.T. Checkcif ok 14-Nov-12 Updated by the Author A.T. 16-Nov-12 Updated by the Author A.T. 20-Mar-13 Updated by the Author A.T. 09-Apr-13 Updated by the Author A.T. ; #===END #=============================================================================== data_compound_3b #TrackingRef 'web_deposit_cif_file_0_Prof.Dr.ThomasStrassner_1366622569.bimetallic_dalton_strassner_revision.cif' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H50 N4 O4 Pt2' _chemical_formula_sum 'C36 H50 N4 O4 Pt2' _chemical_formula_weight 992.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 11.198(3) _cell_length_b 12.003(2) _cell_length_c 13.678(2) _cell_angle_alpha 90 _cell_angle_beta 94.38(3) _cell_angle_gamma 90 _cell_volume 1833.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 198 _cell_measurement_reflns_used 847 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 26.38 _cell_special_details ; ; _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.440 _exptl_crystal_size_min 0.360 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 7.665 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10.(Sheldrick,Bruker AXS Inc.,2002)' _exptl_absorpt_correction_T_min 0.128 _exptl_absorpt_correction_T_max 0.169 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 198 _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method \f _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_wavelength_id x-ray # number of measured reflections (redundant set) _diffrn_reflns_number 37526 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_unetI/netI 0.0193 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 3721 # number of observed reflections (> n sig(I)) _reflns_number_gt 3193 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius BV, 1999)' _computing_cell_refinement 'Dirax/lsq (Duisenberg, 1992)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)' _computing_molecular_graphics 'PLATON (Spek, 2011), ORTEP (Farrugia, L. J. 1997), MERCURY (van de Streek, J. 2006)' _computing_publication_material 'PLATON (Spek, 2011), enCIFer (Allen, 2004)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0131P)^2^+2.3083P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 3721 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0178 _refine_ls_wR_factor_ref 0.0389 _refine_ls_wR_factor_gt 0.0368 _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.401 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.112 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt Uani 0.28043(1) -0.02126(1) 0.61496(1) 1.000 0.0192(1) d . . . O1 O Uani 0.45204(19) -0.04791(18) 0.68132(18) 1.000 0.0296(8) d . . . O2 O Uani 0.32165(19) 0.14321(18) 0.59477(16) 1.000 0.0244(7) d . . . N1 N Uani 0.1081(2) -0.1914(2) 0.57742(19) 1.000 0.0222(8) d . . . N2 N Uani 0.2520(2) -0.2710(2) 0.66393(19) 1.000 0.0242(8) d . . . C1 C Uani 0.2190(3) -0.1720(3) 0.6230(2) 1.000 0.0211(10) d . . . C2 C Uani 0.1642(3) -0.3503(3) 0.6432(3) 1.000 0.0310(11) d . . . C3 C Uani 0.0736(3) -0.3002(3) 0.5895(3) 1.000 0.0298(11) d . . . C4 C Uani 0.0475(3) -0.0961(3) 0.5350(2) 1.000 0.0204(9) d . . . C5 C Uani 0.1181(3) 0.0006(2) 0.5484(2) 1.000 0.0200(10) d . . . C6 C Uani -0.0666(3) -0.0989(3) 0.4893(2) 1.000 0.0224(10) d . . . C7 C Uani 0.3621(3) -0.2906(3) 0.7269(3) 1.000 0.0305(11) d . . . C8 C Uani 0.6893(3) -0.1230(3) 0.6716(3) 1.000 0.0444(14) d . . . C9 C Uani 0.6371(5) -0.0572(5) 0.8360(3) 1.000 0.0723(19) d . . . C10 C Uani 0.7588(4) 0.0634(4) 0.7308(5) 1.000 0.092(3) d . . . C11 C Uani 0.6562(3) -0.0215(3) 0.7312(3) 1.000 0.0379(11) d . . . C12 C Uani 0.5365(3) 0.0240(3) 0.6850(2) 1.000 0.0275(10) d . . . C13 C Uani 0.5265(3) 0.1336(3) 0.6528(3) 1.000 0.0303(11) d . . . C14 C Uani 0.4239(3) 0.1875(3) 0.6124(2) 1.000 0.0220(10) d . . . C15 C Uani 0.4320(3) 0.3108(3) 0.5844(2) 1.000 0.0269(11) d . . . C16 C Uani 0.3122(3) 0.3531(3) 0.5382(3) 1.000 0.0459(14) d . . . C17 C Uani 0.4680(4) 0.3814(3) 0.6753(3) 1.000 0.0393(12) d . . . C18 C Uani 0.5264(4) 0.3222(4) 0.5096(3) 1.000 0.0487(16) d . . . H2 H Uiso 0.16720 -0.42610 0.66310 1.000 0.0370 c R . . H3 H Uiso 0.00040 -0.33350 0.56490 1.000 0.0360 c R . . H6 H Uiso -0.10970 -0.16710 0.48360 1.000 0.0270 c R . . H7A H Uiso 0.34140 -0.30900 0.79340 1.000 0.0450 c R . . H7B H Uiso 0.41170 -0.22330 0.72890 1.000 0.0450 c R . . H7C H Uiso 0.40660 -0.35260 0.70050 1.000 0.0450 c R . . H8A H Uiso 0.69590 -0.10090 0.60320 1.000 0.0660 c R . . H8B H Uiso 0.62710 -0.18000 0.67450 1.000 0.0660 c R . . H8C H Uiso 0.76620 -0.15300 0.69880 1.000 0.0660 c R . . H9A H Uiso 0.70910 -0.09520 0.86440 1.000 0.1080 c R . . H9B H Uiso 0.56860 -0.10810 0.83540 1.000 0.1080 c R . . H9C H Uiso 0.62140 0.00860 0.87540 1.000 0.1080 c R . . H10A H Uiso 0.76340 0.09260 0.66430 1.000 0.1380 c R . . H10B H Uiso 0.83450 0.02700 0.75240 1.000 0.1380 c R . . H10C H Uiso 0.74380 0.12480 0.77550 1.000 0.1380 c R . . H13 H Uiso 0.59770 0.17680 0.65900 1.000 0.0360 c R . . H16A H Uiso 0.25140 0.34690 0.58570 1.000 0.0690 c R . . H16B H Uiso 0.28800 0.30840 0.48010 1.000 0.0690 c R . . H16C H Uiso 0.32030 0.43130 0.51900 1.000 0.0690 c R . . H17A H Uiso 0.54010 0.34990 0.70980 1.000 0.0590 c R . . H17B H Uiso 0.40260 0.38150 0.71900 1.000 0.0590 c R . . H17C H Uiso 0.48420 0.45790 0.65520 1.000 0.0590 c R . . H18A H Uiso 0.50640 0.27210 0.45410 1.000 0.0730 c R . . H18B H Uiso 0.60530 0.30240 0.54070 1.000 0.0730 c R . . H18C H Uiso 0.52800 0.39920 0.48600 1.000 0.0730 c 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 Pt1 0.0167(1) 0.0168(1) 0.0236(1) 0.0023(1) -0.0024(1) -0.0023(1) O1 0.0231(12) 0.0227(14) 0.0413(14) 0.0033(10) -0.0087(10) 0.0001(10) O2 0.0201(11) 0.0170(12) 0.0353(13) 0.0041(10) -0.0036(10) -0.0061(9) N1 0.0225(14) 0.0160(14) 0.0277(15) 0.0036(11) -0.0005(12) -0.0033(11) N2 0.0255(14) 0.0211(15) 0.0259(15) 0.0034(11) 0.0008(12) 0.0023(11) C1 0.0217(16) 0.0216(18) 0.0198(16) 0.0028(13) 0.0011(13) 0.0013(13) C2 0.0368(19) 0.0178(18) 0.038(2) 0.0065(15) 0.0013(16) -0.0042(15) C3 0.0312(19) 0.0203(19) 0.037(2) 0.0042(15) -0.0025(16) -0.0079(14) C4 0.0217(16) 0.0167(17) 0.0226(16) 0.0030(12) 0.0004(13) -0.0017(13) C5 0.0188(15) 0.020(2) 0.0210(16) 0.0001(12) -0.0005(12) -0.0024(12) C6 0.0225(16) 0.0173(17) 0.0271(18) -0.0002(13) -0.0007(14) -0.0064(13) C7 0.0280(18) 0.030(2) 0.033(2) 0.0082(15) -0.0015(15) 0.0054(15) C8 0.030(2) 0.042(2) 0.060(3) -0.009(2) -0.0039(19) 0.0092(17) C9 0.071(3) 0.095(4) 0.046(3) -0.012(3) -0.027(2) 0.044(3) C10 0.033(2) 0.037(3) 0.196(7) -0.003(4) -0.055(3) 0.002(2) C11 0.0284(18) 0.0260(19) 0.056(2) -0.0083(18) -0.0172(17) 0.0056(16) C12 0.0225(16) 0.0253(18) 0.0334(18) -0.0078(15) -0.0058(14) 0.0019(15) C13 0.0219(17) 0.025(2) 0.043(2) 0.0002(16) -0.0047(15) -0.0040(14) C14 0.0208(16) 0.0208(18) 0.0243(17) -0.0005(13) 0.0006(13) -0.0040(13) C15 0.0265(17) 0.0244(19) 0.0291(19) 0.0036(14) -0.0027(14) -0.0085(14) C16 0.042(2) 0.026(2) 0.066(3) 0.0159(19) -0.020(2) -0.0067(17) C17 0.052(2) 0.028(2) 0.037(2) -0.0009(16) -0.0022(18) -0.0024(18) C18 0.062(3) 0.043(3) 0.043(2) 0.0021(19) 0.017(2) -0.015(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O1 2.086(2) . . yes Pt1 O2 2.051(2) . . yes Pt1 C1 1.942(4) . . yes Pt1 C5 1.987(3) . . yes O1 C12 1.279(4) . . yes O2 C14 1.269(4) . . yes N1 C1 1.366(4) . . yes N1 C3 1.375(4) . . yes N1 C4 1.430(4) . . yes N2 C1 1.353(4) . . yes N2 C2 1.382(4) . . yes N2 C7 1.468(4) . . yes C2 C3 1.348(5) . . no C4 C5 1.408(4) . . no C4 C6 1.379(5) . . no C5 C6 1.395(4) . 3_556 no C8 C11 1.527(5) . . no C9 C11 1.527(6) . . no C10 C11 1.536(6) . . no C11 C12 1.538(5) . . no C12 C13 1.389(5) . . no C13 C14 1.395(5) . . no C14 C15 1.533(5) . . no C15 C16 1.526(5) . . no C15 C17 1.533(5) . . no C15 C18 1.532(5) . . no C2 H2 0.9500 . . no C3 H3 0.9500 . . no C6 H6 0.9500 . . no C7 H7A 0.9800 . . no C7 H7B 0.9800 . . no C7 H7C 0.9800 . . no C8 H8A 0.9800 . . no C8 H8B 0.9800 . . no C8 H8C 0.9800 . . no C9 H9A 0.9800 . . no C9 H9B 0.9800 . . no C9 H9C 0.9800 . . no C10 H10A 0.9800 . . no C10 H10B 0.9800 . . no C10 H10C 0.9800 . . no C13 H13 0.9500 . . no C16 H16A 0.9800 . . no C16 H16B 0.9800 . . no C16 H16C 0.9800 . . no C17 H17A 0.9800 . . no C17 H17B 0.9800 . . no C17 H17C 0.9800 . . no C18 H18A 0.9800 . . no C18 H18B 0.9800 . . no C18 H18C 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 O2 89.82(9) . . . yes O1 Pt1 C1 98.69(12) . . . yes O1 Pt1 C5 178.14(10) . . . yes O2 Pt1 C1 171.46(12) . . . yes O2 Pt1 C5 91.07(10) . . . yes C1 Pt1 C5 80.41(12) . . . yes Pt1 O1 C12 124.6(2) . . . yes Pt1 O2 C14 125.9(2) . . . yes C1 N1 C3 111.2(3) . . . yes C1 N1 C4 115.8(3) . . . yes C3 N1 C4 132.8(3) . . . yes C1 N2 C2 110.6(3) . . . yes C1 N2 C7 125.0(3) . . . yes C2 N2 C7 124.2(3) . . . yes Pt1 C1 N1 116.5(2) . . . yes Pt1 C1 N2 139.0(2) . . . yes N1 C1 N2 104.4(3) . . . yes N2 C2 C3 107.4(3) . . . yes N1 C3 C2 106.4(3) . . . yes N1 C4 C5 111.2(3) . . . yes N1 C4 C6 124.0(3) . . . yes C5 C4 C6 124.8(3) . . . no Pt1 C5 C4 115.8(2) . . . yes Pt1 C5 C6 128.2(2) . . 3_556 yes C4 C5 C6 115.9(3) . . 3_556 no C4 C6 C5 119.3(3) . . 3_556 no C8 C11 C9 109.5(3) . . . no C8 C11 C10 108.4(3) . . . no C8 C11 C12 107.7(3) . . . no C9 C11 C10 110.4(4) . . . no C9 C11 C12 107.8(3) . . . no C10 C11 C12 113.1(3) . . . no O1 C12 C11 113.3(3) . . . yes O1 C12 C13 125.8(3) . . . yes C11 C12 C13 120.9(3) . . . no C12 C13 C14 127.5(3) . . . no O2 C14 C13 125.8(3) . . . yes O2 C14 C15 115.3(3) . . . yes C13 C14 C15 118.9(3) . . . no C14 C15 C16 111.0(3) . . . no C14 C15 C17 110.4(3) . . . no C14 C15 C18 108.1(3) . . . no C16 C15 C17 108.7(3) . . . no C16 C15 C18 108.9(3) . . . no C17 C15 C18 109.9(3) . . . no N2 C2 H2 126.00 . . . no C3 C2 H2 126.00 . . . no N1 C3 H3 127.00 . . . no C2 C3 H3 127.00 . . . no C4 C6 H6 120.00 . . . no C5 C6 H6 120.00 3_556 . . no N2 C7 H7A 109.00 . . . no N2 C7 H7B 109.00 . . . no N2 C7 H7C 109.00 . . . no H7A C7 H7B 109.00 . . . no H7A C7 H7C 109.00 . . . no H7B C7 H7C 109.00 . . . no C11 C8 H8A 109.00 . . . no C11 C8 H8B 109.00 . . . no C11 C8 H8C 109.00 . . . no H8A C8 H8B 109.00 . . . no H8A C8 H8C 109.00 . . . no H8B C8 H8C 110.00 . . . no C11 C9 H9A 109.00 . . . no C11 C9 H9B 109.00 . . . no C11 C9 H9C 110.00 . . . no H9A C9 H9B 109.00 . . . no H9A C9 H9C 110.00 . . . no H9B C9 H9C 110.00 . . . no C11 C10 H10A 109.00 . . . no C11 C10 H10B 109.00 . . . no C11 C10 H10C 109.00 . . . no H10A C10 H10B 110.00 . . . no H10A C10 H10C 109.00 . . . no H10B C10 H10C 109.00 . . . no C12 C13 H13 116.00 . . . no C14 C13 H13 116.00 . . . no C15 C16 H16A 110.00 . . . no C15 C16 H16B 109.00 . . . no C15 C16 H16C 109.00 . . . no H16A C16 H16B 109.00 . . . no H16A C16 H16C 109.00 . . . no H16B C16 H16C 109.00 . . . no C15 C17 H17A 109.00 . . . no C15 C17 H17B 109.00 . . . no C15 C17 H17C 109.00 . . . no H17A C17 H17B 109.00 . . . no H17A C17 H17C 109.00 . . . no H17B C17 H17C 109.00 . . . no C15 C18 H18A 109.00 . . . no C15 C18 H18B 109.00 . . . no C15 C18 H18C 110.00 . . . no H18A C18 H18B 109.00 . . . no H18A C18 H18C 109.00 . . . no H18B C18 H18C 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Pt1 O1 C12 -7.5(2) . . . . no C1 Pt1 O1 C12 171.7(2) . . . . no O1 Pt1 O2 C14 6.5(2) . . . . no C5 Pt1 O2 C14 -171.9(2) . . . . no O1 Pt1 C1 N1 -174.1(2) . . . . no O1 Pt1 C1 N2 7.8(4) . . . . no C5 Pt1 C1 N1 4.3(2) . . . . no C5 Pt1 C1 N2 -173.9(4) . . . . no O2 Pt1 C5 C4 175.7(2) . . . . no O2 Pt1 C5 C6 -2.2(3) . . . 3_556 no C1 Pt1 C5 C4 -3.7(2) . . . . no C1 Pt1 C5 C6 178.4(3) . . . 3_556 no Pt1 O1 C12 C11 -175.4(2) . . . . no Pt1 O1 C12 C13 5.3(5) . . . . no Pt1 O2 C14 C13 -2.9(4) . . . . no Pt1 O2 C14 C15 176.17(18) . . . . no C3 N1 C1 Pt1 -179.0(2) . . . . no C3 N1 C1 N2 -0.3(3) . . . . no C4 N1 C1 Pt1 -4.1(3) . . . . no C4 N1 C1 N2 174.6(2) . . . . no C1 N1 C3 C2 -0.2(4) . . . . no C4 N1 C3 C2 -174.0(3) . . . . no C1 N1 C4 C5 0.9(4) . . . . no C1 N1 C4 C6 -177.5(3) . . . . no C3 N1 C4 C5 174.4(3) . . . . no C3 N1 C4 C6 -4.0(5) . . . . no C2 N2 C1 Pt1 179.0(3) . . . . no C2 N2 C1 N1 0.7(3) . . . . no C7 N2 C1 Pt1 2.5(5) . . . . no C7 N2 C1 N1 -175.7(3) . . . . no C1 N2 C2 C3 -0.9(4) . . . . no C7 N2 C2 C3 175.6(3) . . . . no N2 C2 C3 N1 0.6(4) . . . . no N1 C4 C5 Pt1 2.6(3) . . . . no N1 C4 C5 C6 -179.2(3) . . . 3_556 no C6 C4 C5 Pt1 -179.0(2) . . . . no C6 C4 C5 C6 -0.8(4) . . . 3_556 no N1 C4 C6 C5 179.1(3) . . . 3_556 no C5 C4 C6 C5 0.9(5) . . . 3_556 no Pt1 C5 C6 C4 178.7(2) . . 3_556 3_556 no C4 C5 C6 C4 0.8(4) . . 3_556 3_556 no C8 C11 C12 O1 57.5(4) . . . . no C8 C11 C12 C13 -123.2(3) . . . . no C9 C11 C12 O1 -60.6(4) . . . . no C9 C11 C12 C13 118.8(4) . . . . no C10 C11 C12 O1 177.2(4) . . . . no C10 C11 C12 C13 -3.5(5) . . . . no O1 C12 C13 C14 1.4(6) . . . . no C11 C12 C13 C14 -177.9(3) . . . . no C12 C13 C14 O2 -2.8(6) . . . . no C12 C13 C14 C15 178.2(3) . . . . no O2 C14 C15 C16 -1.3(4) . . . . no O2 C14 C15 C17 119.3(3) . . . . no O2 C14 C15 C18 -120.5(3) . . . . no C13 C14 C15 C16 177.9(3) . . . . no C13 C14 C15 C17 -61.6(4) . . . . no C13 C14 C15 C18 58.6(4) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C6 H6 O2 0.9500 2.5400 3.043(4) 113.00 3_556 yes C7 H7A O2 0.9800 2.5400 3.403(4) 147.00 2_546 yes C7 H7B O1 0.9800 2.2600 3.160(4) 152.00 . yes C9 H9B O1 0.9800 2.5000 2.848(5) 101.00 . yes _iucr_refine_instructions_details ; TITL str-446x in P2(1)/n CELL 0.71073 11.1980 12.0030 13.6780 90.000 94.375 90.000 ZERR 2 0.0027 0.0024 0.0022 0.000 0.030 0.0 LATT 1 SYMM 0.50000 - X , 0.50000 + Y , 0.50000 - Z SFAC C H N O Pt UNIT 72 100 8 8 4 L.S. 18 ACTA BOND $H FMAP 2 PLAN 10 CONF TEMP -75 SIZE 0.360 0.445 0.454 WGHT 0.013100 2.308300 FVAR 0.07378 PT1 5 0.280434 -0.021257 0.614961 11.00000 0.01665 0.01682 = 0.02359 0.00232 -0.00240 -0.00225 O1 4 0.452038 -0.047910 0.681320 11.00000 0.02312 0.02273 = 0.04128 0.00326 -0.00866 0.00009 O2 4 0.321649 0.143211 0.594768 11.00000 0.02007 0.01704 = 0.03529 0.00412 -0.00363 -0.00607 N1 3 0.108059 -0.191397 0.577421 11.00000 0.02249 0.01599 = 0.02772 0.00358 -0.00052 -0.00330 N2 3 0.252010 -0.271022 0.663927 11.00000 0.02552 0.02110 = 0.02589 0.00336 0.00083 0.00230 C1 1 0.218952 -0.172048 0.622997 11.00000 0.02171 0.02162 = 0.01980 0.00279 0.00108 0.00133 C2 1 0.164186 -0.350290 0.643169 11.00000 0.03679 0.01784 = 0.03751 0.00654 0.00132 -0.00417 AFIX 43 H2 2 0.167152 -0.426129 0.663075 11.00000 -1.20000 AFIX 0 C3 1 0.073598 -0.300218 0.589513 11.00000 0.03120 0.02032 = 0.03654 0.00424 -0.00250 -0.00787 AFIX 43 H3 2 0.000403 -0.333487 0.564900 11.00000 -1.20000 AFIX 0 C4 1 0.047535 -0.096109 0.534968 11.00000 0.02173 0.01668 = 0.02261 0.00302 0.00042 -0.00174 C5 1 0.118074 0.000610 0.548441 11.00000 0.01876 0.01959 = 0.02098 0.00010 -0.00047 -0.00240 C6 1 -0.066580 -0.098920 0.489299 11.00000 0.02255 0.01731 = 0.02713 -0.00023 -0.00071 -0.00638 AFIX 43 H6 2 -0.109656 -0.167089 0.483606 11.00000 -1.20000 AFIX 0 C7 1 0.362057 -0.290589 0.726909 11.00000 0.02801 0.02966 = 0.03258 0.00817 -0.00149 0.00537 AFIX 137 H7A 2 0.341392 -0.308994 0.793353 11.00000 -1.50000 H7B 2 0.411671 -0.223250 0.728922 11.00000 -1.50000 H7C 2 0.406591 -0.352590 0.700508 11.00000 -1.50000 AFIX 0 C8 1 0.689321 -0.122952 0.671576 11.00000 0.02963 0.04224 = 0.05985 -0.00940 -0.00386 0.00918 AFIX 137 H8A 2 0.695923 -0.100933 0.603206 11.00000 -1.50000 H8B 2 0.627109 -0.180019 0.674520 11.00000 -1.50000 H8C 2 0.766174 -0.153035 0.698753 11.00000 -1.50000 AFIX 0 C9 1 0.637142 -0.057246 0.835954 11.00000 0.07069 0.09544 = 0.04569 -0.01189 -0.02673 0.04373 AFIX 137 H9A 2 0.709126 -0.095185 0.864369 11.00000 -1.50000 H9B 2 0.568636 -0.108112 0.835384 11.00000 -1.50000 H9C 2 0.621421 0.008584 0.875365 11.00000 -1.50000 AFIX 0 C10 1 0.758760 0.063428 0.730794 11.00000 0.03286 0.03686 = 0.19608 -0.00305 -0.05548 0.00158 AFIX 137 H10A 2 0.763408 0.092643 0.664288 11.00000 -1.50000 H10B 2 0.834537 0.026979 0.752381 11.00000 -1.50000 H10C 2 0.743784 0.124837 0.775465 11.00000 -1.50000 AFIX 0 C11 1 0.656213 -0.021454 0.731182 11.00000 0.02837 0.02596 = 0.05556 -0.00828 -0.01716 0.00561 C12 1 0.536515 0.024041 0.684990 11.00000 0.02246 0.02534 = 0.03335 -0.00782 -0.00583 0.00187 C13 1 0.526521 0.133550 0.652826 11.00000 0.02188 0.02495 = 0.04266 0.00017 -0.00466 -0.00400 AFIX 43 H13 2 0.597746 0.176801 0.659028 11.00000 -1.20000 AFIX 0 C14 1 0.423856 0.187472 0.612407 11.00000 0.02082 0.02084 = 0.02430 -0.00052 0.00063 -0.00395 C15 1 0.432035 0.310805 0.584383 11.00000 0.02651 0.02442 = 0.02914 0.00360 -0.00268 -0.00851 C16 1 0.312184 0.353125 0.538155 11.00000 0.04238 0.02576 = 0.06553 0.01586 -0.01967 -0.00666 AFIX 137 H16A 2 0.251362 0.346922 0.585726 11.00000 -1.50000 H16B 2 0.287985 0.308354 0.480078 11.00000 -1.50000 H16C 2 0.320250 0.431272 0.518979 11.00000 -1.50000 AFIX 0 C17 1 0.467983 0.381387 0.675325 11.00000 0.05193 0.02787 = 0.03651 -0.00092 -0.00222 -0.00245 AFIX 137 H17A 2 0.540116 0.349865 0.709848 11.00000 -1.50000 H17B 2 0.402585 0.381479 0.719028 11.00000 -1.50000 H17C 2 0.484223 0.457932 0.655229 11.00000 -1.50000 AFIX 0 C18 1 0.526443 0.322173 0.509551 11.00000 0.06207 0.04320 = 0.04267 0.00212 0.01671 -0.01457 AFIX 137 H18A 2 0.506392 0.272138 0.454098 11.00000 -1.50000 H18B 2 0.605331 0.302400 0.540659 11.00000 -1.50000 H18C 2 0.527971 0.399250 0.486046 11.00000 -1.50000 HKLF 4 REM str-446x in P2(1)/n REM R1 = 0.0178 for 3193 Fo > 4sig(Fo) and 0.0275 for all 3721 data REM 215 parameters refined using 0 restraints END ; _database_code_depnum_ccdc_archive 'CCDC 930702' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_global #TrackingRef 'web_deposit_cif_file_0_Prof.Dr.ThomasStrassner_1366622569.bimetallic_dalton_strassner_revision.cif' #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'Sep 05 10:34:21 2012' _audit_creation_method 'PLATON
option' _audit_update_record ; 05-Sept-12 Updated by the Author A.T Text writing by A.T. Checkcif ok 14-Nov-12 Updated by the Author A.T. 16-Nov-12 Updated by the Author A.T. 20-Mar-13 Updated by the Author A.T. 09-Apr-13 Updated by the Author A.T. ; #===END #============================================================================== data_compound_3c #TrackingRef 'web_deposit_cif_file_0_Prof.Dr.ThomasStrassner_1366622569.bimetallic_dalton_strassner_revision.cif' #============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point 241 _chemical_formula_moiety 'C56 H58 N4 O4 Pt2' _chemical_formula_structural ? _chemical_formula_sum 'C56 H58 N4 O4 Pt2' _chemical_formula_weight 1241.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 11.342(2) _cell_length_b 19.880(3) _cell_length_c 12.6380(14) _cell_angle_alpha 90 _cell_angle_beta 101.411(9) _cell_angle_gamma 90 _cell_volume 2793.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 198 _cell_measurement_reflns_used 986 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 26.40 _cell_special_details ; ; _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.430 _exptl_crystal_size_min 0.290 _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 5.047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10.(Sheldrick,Bruker AXS Inc.,2002)' _exptl_absorpt_correction_T_min 0.208 _exptl_absorpt_correction_T_max 0.324 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 198 _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method \f _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_wavelength_id x-ray # number of measured reflections (redundant set) _diffrn_reflns_number 68874 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_unetI/netI 0.0324 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.40 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 5722 # number of observed reflections (> n sig(I)) _reflns_number_gt 4597 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius BV, 1999)' _computing_cell_refinement 'Dirax/lsq (Duisenberg, 1992)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)' _computing_molecular_graphics 'PLATON (Spek, 2011), ORTEP (Farrugia, L. J. 1997), MERCURY (van de Streek, J. 2006)' _computing_publication_material 'PLATON (Spek, 2011), enCIFer (Allen, 2004)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0368P)^2^+1.4333P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 5722 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.493 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.124 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt Uani 0.53033(1) 0.14311(1) 0.15055(1) 1.000 0.0230(1) d . . . O1 O Uani 0.5570(3) 0.23408(14) 0.2322(2) 1.000 0.0309(10) d . . . O2 O Uani 0.4538(3) 0.10416(14) 0.2708(2) 1.000 0.0279(10) d . . . N1 N Uani 0.6101(3) 0.11751(17) -0.0441(3) 1.000 0.0256(11) d . . . N2 N Uani 0.6541(3) 0.22146(18) -0.0086(3) 1.000 0.0314(12) d . . . C1 C Uani 0.6031(4) 0.1678(2) 0.0280(3) 1.000 0.0253(12) d . . . C2 C Uani 0.6944(4) 0.2043(2) -0.1025(4) 1.000 0.0377(17) d . . . C3 C Uani 0.6666(4) 0.1405(2) -0.1243(4) 1.000 0.0345(16) d . . . C4 C Uani 0.5549(4) 0.0552(2) -0.0255(3) 1.000 0.0239(12) d . . . C5 C Uani 0.5086(4) 0.0575(2) 0.0691(3) 1.000 0.0229(12) d . . . C6 C Uani 0.4508(4) -0.0006(2) 0.0943(3) 1.000 0.0232(12) d . . . C7 C Uani 0.6604(5) 0.2890(2) 0.0368(4) 1.000 0.0510(19) d . . . C8 C Uani 0.6281(5) 0.5270(2) 0.4312(5) 1.000 0.052(2) d . . . C9 C Uani 0.5986(4) 0.4540(2) 0.4068(4) 1.000 0.0368(17) d . . . C10 C Uani 0.6574(4) 0.4034(2) 0.4701(4) 1.000 0.0386(17) d . . . C11 C Uani 0.6325(4) 0.3354(2) 0.4482(4) 1.000 0.0329(17) d . . . C12 C Uani 0.7010(5) 0.2829(3) 0.5220(4) 1.000 0.0479(17) d . . . C13 C Uani 0.5462(4) 0.3191(2) 0.3558(3) 1.000 0.0263(12) d . . . C14 C Uani 0.4841(4) 0.3694(2) 0.2896(3) 1.000 0.0280(14) d . . . C15 C Uani 0.3908(4) 0.3536(2) 0.1900(4) 1.000 0.0389(17) d . . . C16 C Uani 0.5110(4) 0.4358(2) 0.3173(4) 1.000 0.0332(16) d . . . C17 C Uani 0.5237(4) 0.2475(2) 0.3209(3) 1.000 0.0275(12) d . . . C18 C Uani 0.4700(4) 0.2026(2) 0.3815(3) 1.000 0.0270(12) d . . . C19 C Uani 0.4386(4) 0.1364(2) 0.3554(3) 1.000 0.0253(14) d . . . C20 C Uani 0.3775(4) 0.0959(2) 0.4285(3) 1.000 0.0247(12) d . . . C21 C Uani 0.4398(4) 0.0774(2) 0.5325(3) 1.000 0.0312(16) d . . . C22 C Uani 0.5671(4) 0.0970(3) 0.5747(4) 1.000 0.0452(17) d . . . C23 C Uani 0.3791(5) 0.0388(3) 0.5963(4) 1.000 0.0440(19) d . . . C24 C Uani 0.2614(5) 0.0182(3) 0.5619(4) 1.000 0.0440(17) d . . . C25 C Uani 0.1993(6) -0.0250(4) 0.6328(5) 1.000 0.081(3) d . . . C26 C Uani 0.2025(4) 0.0379(2) 0.4595(4) 1.000 0.0370(17) d . . . C27 C Uani 0.2582(4) 0.0752(2) 0.3918(3) 1.000 0.0289(14) d . . . C28 C Uani 0.1889(4) 0.0952(3) 0.2810(4) 1.000 0.0418(17) d . . . H2 H Uiso 0.73470 0.23330 -0.14350 1.000 0.0450 c R . . H3 H Uiso 0.68240 0.11530 -0.18380 1.000 0.0410 c R . . H6 H Uiso 0.41630 -0.00260 0.15690 1.000 0.0280 c R . . H7A H Uiso 0.63330 0.28810 0.10580 1.000 0.0760 c R . . H7B H Uiso 0.60870 0.31920 -0.01330 1.000 0.0760 c R . . H7C H Uiso 0.74360 0.30520 0.04870 1.000 0.0760 c R . . H8A H Uiso 0.69150 0.54120 0.39350 1.000 0.0780 c R . . H8B H Uiso 0.65580 0.53280 0.50920 1.000 0.0780 c R . . H8C H Uiso 0.55600 0.55440 0.40680 1.000 0.0780 c R . . H10 H Uiso 0.71730 0.41510 0.53120 1.000 0.0460 c R . . H12A H Uiso 0.78030 0.30060 0.55530 1.000 0.0720 c R . . H12B H Uiso 0.71080 0.24240 0.48020 1.000 0.0720 c R . . H12C H Uiso 0.65640 0.27150 0.57850 1.000 0.0720 c R . . H15A H Uiso 0.34010 0.39320 0.16930 1.000 0.0580 c R . . H15B H Uiso 0.34080 0.31600 0.20520 1.000 0.0580 c R . . H15C H Uiso 0.43100 0.34130 0.13090 1.000 0.0580 c R . . H16 H Uiso 0.46830 0.47030 0.27380 1.000 0.0400 c R . . H18 H Uiso 0.45320 0.21900 0.44760 1.000 0.0320 c R . . H22A H Uiso 0.56920 0.13970 0.61360 1.000 0.0680 c R . . H22B H Uiso 0.60900 0.10210 0.51430 1.000 0.0680 c R . . H22C H Uiso 0.60690 0.06210 0.62380 1.000 0.0680 c R . . H23 H Uiso 0.42030 0.02610 0.66640 1.000 0.0530 c R . . H25A H Uiso 0.14380 0.00280 0.66440 1.000 0.1210 c R . . H25B H Uiso 0.25960 -0.04490 0.69060 1.000 0.1210 c R . . H25C H Uiso 0.15430 -0.06090 0.58930 1.000 0.1210 c R . . H26 H Uiso 0.12080 0.02520 0.43540 1.000 0.0450 c R . . H28A H Uiso 0.21090 0.06520 0.22640 1.000 0.0630 c R . . H28B H Uiso 0.20870 0.14170 0.26560 1.000 0.0630 c R . . H28C H Uiso 0.10240 0.09160 0.27940 1.000 0.0630 c 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 Pt1 0.0288(1) 0.0214(1) 0.0199(1) -0.0035(1) 0.0074(1) -0.0008(1) O1 0.0411(18) 0.0234(16) 0.0301(17) -0.0082(13) 0.0119(14) -0.0058(13) O2 0.0377(18) 0.0271(17) 0.0214(16) -0.0048(13) 0.0118(13) -0.0028(14) N1 0.034(2) 0.0231(18) 0.0216(18) -0.0010(15) 0.0103(16) -0.0008(16) N2 0.039(2) 0.029(2) 0.029(2) -0.0031(16) 0.0136(18) -0.0092(18) C1 0.027(2) 0.025(2) 0.023(2) -0.0018(18) 0.0026(19) -0.0020(19) C2 0.046(3) 0.037(3) 0.033(3) 0.003(2) 0.015(2) -0.011(2) C3 0.046(3) 0.036(3) 0.026(2) -0.001(2) 0.018(2) -0.005(2) C4 0.028(2) 0.022(2) 0.022(2) 0.0009(17) 0.0056(18) -0.0008(17) C5 0.027(2) 0.023(2) 0.019(2) -0.0011(17) 0.0054(18) 0.0026(18) C6 0.028(2) 0.026(2) 0.017(2) -0.0020(17) 0.0080(17) 0.0006(19) C7 0.076(4) 0.031(3) 0.052(3) -0.015(2) 0.027(3) -0.022(3) C8 0.056(4) 0.031(3) 0.072(4) -0.018(3) 0.017(3) -0.010(2) C9 0.037(3) 0.032(3) 0.045(3) -0.010(2) 0.017(2) -0.005(2) C10 0.038(3) 0.043(3) 0.033(3) -0.016(2) 0.003(2) -0.007(2) C11 0.036(3) 0.032(3) 0.030(3) -0.007(2) 0.005(2) -0.001(2) C12 0.047(3) 0.046(3) 0.042(3) -0.004(3) -0.012(2) -0.003(3) C13 0.028(2) 0.027(2) 0.025(2) -0.0065(19) 0.0078(19) -0.0019(19) C14 0.029(2) 0.029(3) 0.027(2) -0.0068(18) 0.0080(19) -0.0036(19) C15 0.035(3) 0.034(3) 0.044(3) -0.003(2) -0.001(2) 0.000(2) C16 0.034(3) 0.027(2) 0.039(3) 0.000(2) 0.008(2) 0.005(2) C17 0.027(2) 0.027(2) 0.027(2) -0.0077(19) 0.0016(19) 0.0006(19) C18 0.032(2) 0.029(2) 0.021(2) -0.0055(18) 0.008(2) 0.0020(19) C19 0.024(2) 0.033(3) 0.018(2) -0.0007(19) 0.0021(18) 0.0054(18) C20 0.032(2) 0.021(2) 0.021(2) -0.0036(17) 0.0052(19) 0.0056(18) C21 0.036(3) 0.032(3) 0.026(2) -0.005(2) 0.007(2) 0.011(2) C22 0.044(3) 0.050(3) 0.036(3) 0.000(2) -0.006(2) 0.008(2) C23 0.057(4) 0.053(3) 0.024(3) 0.009(2) 0.013(2) 0.012(3) C24 0.051(3) 0.047(3) 0.041(3) 0.008(2) 0.026(3) 0.006(3) C25 0.089(5) 0.097(6) 0.066(4) 0.030(4) 0.040(4) -0.002(4) C26 0.034(3) 0.034(3) 0.046(3) -0.002(2) 0.015(2) 0.000(2) C27 0.034(3) 0.025(2) 0.028(2) -0.0013(19) 0.007(2) 0.004(2) C28 0.036(3) 0.048(3) 0.038(3) 0.004(2) -0.001(2) -0.005(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O1 2.074(3) . . yes Pt1 O2 2.046(3) . . yes Pt1 C1 1.956(4) . . yes Pt1 C5 1.979(4) . . yes O1 C17 1.280(5) . . yes O2 C19 1.287(5) . . yes N1 C1 1.366(5) . . yes N1 C3 1.380(6) . . yes N1 C4 1.428(5) . . yes N2 C1 1.339(5) . . yes N2 C2 1.396(6) . . yes N2 C7 1.456(5) . . yes C2 C3 1.323(6) . . no C4 C5 1.398(6) . . no C4 C6 1.384(5) . 3_655 no C5 C6 1.396(6) . . no C8 C9 1.507(6) . . no C9 C10 1.373(6) . . no C9 C16 1.397(7) . . no C10 C11 1.398(6) . . no C11 C12 1.509(7) . . no C11 C13 1.405(6) . . no C13 C14 1.401(6) . . no C13 C17 1.497(6) . . no C14 C15 1.509(6) . . no C14 C16 1.384(6) . . no C17 C18 1.392(6) . . no C18 C19 1.386(6) . . no C19 C20 1.495(6) . . no C20 C21 1.412(5) . . no C20 C27 1.403(6) . . no C21 C22 1.489(7) . . no C21 C23 1.390(7) . . no C23 C24 1.382(8) . . no C24 C25 1.512(9) . . no C24 C26 1.390(7) . . no C26 C27 1.377(6) . . no C27 C28 1.517(6) . . no C2 H2 0.9500 . . no C3 H3 0.9500 . . no C6 H6 0.9500 . . no C7 H7A 0.9800 . . no C7 H7B 0.9800 . . no C7 H7C 0.9800 . . no C8 H8A 0.9800 . . no C8 H8B 0.9800 . . no C8 H8C 0.9800 . . no C10 H10 0.9500 . . no C12 H12A 0.9800 . . no C12 H12B 0.9800 . . no C12 H12C 0.9800 . . no C15 H15A 0.9800 . . no C15 H15B 0.9800 . . no C15 H15C 0.9800 . . no C16 H16 0.9500 . . no C18 H18 0.9500 . . no C22 H22A 0.9800 . . no C22 H22B 0.9800 . . no C22 H22C 0.9800 . . no C23 H23 0.9500 . . no C25 H25A 0.9800 . . no C25 H25B 0.9800 . . no C25 H25C 0.9800 . . no C26 H26 0.9500 . . no C28 H28A 0.9800 . . no C28 H28B 0.9800 . . no C28 H28C 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 O2 90.11(11) . . . yes O1 Pt1 C1 97.60(14) . . . yes O1 Pt1 C5 177.94(15) . . . yes O2 Pt1 C1 172.17(14) . . . yes O2 Pt1 C5 91.91(14) . . . yes C1 Pt1 C5 80.37(17) . . . yes Pt1 O1 C17 125.3(3) . . . yes Pt1 O2 C19 125.1(3) . . . yes C1 N1 C3 110.2(3) . . . yes C1 N1 C4 116.1(3) . . . yes C3 N1 C4 133.7(4) . . . yes C1 N2 C2 109.6(3) . . . yes C1 N2 C7 126.1(4) . . . yes C2 N2 C7 124.2(4) . . . yes Pt1 C1 N1 115.7(3) . . . yes Pt1 C1 N2 138.8(3) . . . yes N1 C1 N2 105.5(3) . . . yes N2 C2 C3 107.9(4) . . . yes N1 C3 C2 106.9(4) . . . yes N1 C4 C5 111.3(3) . . . yes N1 C4 C6 123.0(4) . . 3_655 yes C5 C4 C6 125.7(4) . . 3_655 no Pt1 C5 C4 116.3(3) . . . yes Pt1 C5 C6 127.5(3) . . . yes C4 C5 C6 116.2(4) . . . no C4 C6 C5 118.1(4) 3_655 . . no C8 C9 C10 121.6(4) . . . no C8 C9 C16 120.6(4) . . . no C10 C9 C16 117.9(4) . . . no C9 C10 C11 122.5(4) . . . no C10 C11 C12 119.2(4) . . . no C10 C11 C13 117.9(4) . . . no C12 C11 C13 122.9(4) . . . no C11 C13 C14 121.1(4) . . . no C11 C13 C17 121.0(4) . . . no C14 C13 C17 117.8(3) . . . no C13 C14 C15 122.4(4) . . . no C13 C14 C16 118.0(4) . . . no C15 C14 C16 119.5(4) . . . no C9 C16 C14 122.5(4) . . . no O1 C17 C13 113.2(3) . . . yes O1 C17 C18 125.8(4) . . . yes C13 C17 C18 121.0(4) . . . no C17 C18 C19 126.7(4) . . . no O2 C19 C18 126.9(4) . . . yes O2 C19 C20 113.6(3) . . . yes C18 C19 C20 119.5(3) . . . no C19 C20 C21 120.5(4) . . . no C19 C20 C27 119.2(3) . . . no C21 C20 C27 120.2(4) . . . no C20 C21 C22 122.4(4) . . . no C20 C21 C23 118.0(4) . . . no C22 C21 C23 119.6(4) . . . no C21 C23 C24 122.7(5) . . . no C23 C24 C25 121.1(5) . . . no C23 C24 C26 117.8(5) . . . no C25 C24 C26 121.2(5) . . . no C24 C26 C27 122.4(4) . . . no C20 C27 C26 118.9(4) . . . no C20 C27 C28 121.2(4) . . . no C26 C27 C28 119.8(4) . . . no N2 C2 H2 126.00 . . . no C3 C2 H2 126.00 . . . no N1 C3 H3 126.00 . . . no C2 C3 H3 127.00 . . . no C5 C6 H6 121.00 . . . no C4 C6 H6 121.00 3_655 . . no N2 C7 H7A 110.00 . . . no N2 C7 H7B 110.00 . . . no N2 C7 H7C 110.00 . . . no H7A C7 H7B 109.00 . . . no H7A C7 H7C 109.00 . . . no H7B C7 H7C 109.00 . . . no C9 C8 H8A 109.00 . . . no C9 C8 H8B 109.00 . . . no C9 C8 H8C 109.00 . . . no H8A C8 H8B 110.00 . . . no H8A C8 H8C 110.00 . . . no H8B C8 H8C 109.00 . . . no C9 C10 H10 119.00 . . . no C11 C10 H10 119.00 . . . no C11 C12 H12A 109.00 . . . no C11 C12 H12B 110.00 . . . no C11 C12 H12C 109.00 . . . no H12A C12 H12B 109.00 . . . no H12A C12 H12C 109.00 . . . no H12B C12 H12C 109.00 . . . no C14 C15 H15A 109.00 . . . no C14 C15 H15B 109.00 . . . no C14 C15 H15C 109.00 . . . no H15A C15 H15B 109.00 . . . no H15A C15 H15C 110.00 . . . no H15B C15 H15C 109.00 . . . no C9 C16 H16 119.00 . . . no C14 C16 H16 119.00 . . . no C17 C18 H18 117.00 . . . no C19 C18 H18 117.00 . . . no C21 C22 H22A 109.00 . . . no C21 C22 H22B 109.00 . . . no C21 C22 H22C 110.00 . . . no H22A C22 H22B 109.00 . . . no H22A C22 H22C 109.00 . . . no H22B C22 H22C 109.00 . . . no C21 C23 H23 119.00 . . . no C24 C23 H23 119.00 . . . no C24 C25 H25A 109.00 . . . no C24 C25 H25B 109.00 . . . no C24 C25 H25C 109.00 . . . no H25A C25 H25B 109.00 . . . no H25A C25 H25C 110.00 . . . no H25B C25 H25C 109.00 . . . no C24 C26 H26 119.00 . . . no C27 C26 H26 119.00 . . . no C27 C28 H28A 109.00 . . . no C27 C28 H28B 109.00 . . . no C27 C28 H28C 109.00 . . . no H28A C28 H28B 109.00 . . . no H28A C28 H28C 110.00 . . . no H28B C28 H28C 109.00 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Pt1 O1 C17 -2.6(3) . . . . no C1 Pt1 O1 C17 178.7(3) . . . . no O1 Pt1 O2 C19 0.7(3) . . . . no C5 Pt1 O2 C19 -179.7(4) . . . . no O1 Pt1 C1 N1 175.9(3) . . . . no O1 Pt1 C1 N2 -1.9(5) . . . . no C5 Pt1 C1 N1 -3.7(3) . . . . no C5 Pt1 C1 N2 178.5(5) . . . . no O2 Pt1 C5 C4 -176.7(3) . . . . no O2 Pt1 C5 C6 4.3(4) . . . . no C1 Pt1 C5 C4 2.0(3) . . . . no C1 Pt1 C5 C6 -177.0(4) . . . . no Pt1 O1 C17 C13 -175.2(3) . . . . no Pt1 O1 C17 C18 3.9(6) . . . . no Pt1 O2 C19 C18 0.2(6) . . . . no Pt1 O2 C19 C20 178.6(3) . . . . no C3 N1 C1 Pt1 -177.9(3) . . . . no C3 N1 C1 N2 0.6(5) . . . . no C4 N1 C1 Pt1 4.9(5) . . . . no C4 N1 C1 N2 -176.7(3) . . . . no C1 N1 C3 C2 0.0(5) . . . . no C4 N1 C3 C2 176.5(4) . . . . no C1 N1 C4 C5 -3.1(5) . . . . no C1 N1 C4 C6 176.7(4) . . . 3_655 no C3 N1 C4 C5 -179.5(4) . . . . no C3 N1 C4 C6 0.3(7) . . . 3_655 no C2 N2 C1 Pt1 177.1(4) . . . . no C2 N2 C1 N1 -0.9(5) . . . . no C7 N2 C1 Pt1 -6.8(8) . . . . no C7 N2 C1 N1 175.2(4) . . . . no C1 N2 C2 C3 0.9(5) . . . . no C7 N2 C2 C3 -175.3(4) . . . . no N2 C2 C3 N1 -0.5(5) . . . . no N1 C4 C5 Pt1 -0.1(5) . . . . no N1 C4 C5 C6 179.0(4) . . . . no C6 C4 C5 Pt1 -179.8(4) 3_655 . . . no C6 C4 C5 C6 -0.7(7) 3_655 . . . no N1 C4 C6 C5 -179.0(4) . . 3_655 3_655 no C5 C4 C6 C5 0.7(7) . . 3_655 3_655 no Pt1 C5 C6 C4 179.7(3) . . . 3_655 no C4 C5 C6 C4 0.7(6) . . . 3_655 no C8 C9 C10 C11 -179.2(5) . . . . no C16 C9 C10 C11 -0.1(7) . . . . no C8 C9 C16 C14 177.6(5) . . . . no C10 C9 C16 C14 -1.5(7) . . . . no C9 C10 C11 C12 -179.8(5) . . . . no C9 C10 C11 C13 1.9(7) . . . . no C10 C11 C13 C14 -2.1(7) . . . . no C10 C11 C13 C17 173.8(4) . . . . no C12 C11 C13 C14 179.7(4) . . . . no C12 C11 C13 C17 -4.5(7) . . . . no C11 C13 C14 C15 -179.9(4) . . . . no C11 C13 C14 C16 0.6(7) . . . . no C17 C13 C14 C15 4.2(6) . . . . no C17 C13 C14 C16 -175.4(4) . . . . no C11 C13 C17 O1 -112.0(5) . . . . no C11 C13 C17 C18 68.8(6) . . . . no C14 C13 C17 O1 63.9(5) . . . . no C14 C13 C17 C18 -115.2(5) . . . . no C13 C14 C16 C9 1.3(7) . . . . no C15 C14 C16 C9 -178.3(4) . . . . no O1 C17 C18 C19 -2.7(8) . . . . no C13 C17 C18 C19 176.4(4) . . . . no C17 C18 C19 O2 0.4(8) . . . . no C17 C18 C19 C20 -177.9(4) . . . . no O2 C19 C20 C21 113.6(4) . . . . no O2 C19 C20 C27 -65.1(5) . . . . no C18 C19 C20 C21 -67.9(6) . . . . no C18 C19 C20 C27 113.5(5) . . . . no C19 C20 C21 C22 0.3(6) . . . . no C19 C20 C21 C23 -179.0(4) . . . . no C27 C20 C21 C22 178.9(4) . . . . no C27 C20 C21 C23 -0.3(6) . . . . no C19 C20 C27 C26 180.0(4) . . . . no C19 C20 C27 C28 -2.2(6) . . . . no C21 C20 C27 C26 1.3(6) . . . . no C21 C20 C27 C28 179.2(4) . . . . no C20 C21 C23 C24 0.0(8) . . . . no C22 C21 C23 C24 -179.3(5) . . . . no C21 C23 C24 C25 178.7(5) . . . . no C21 C23 C24 C26 -0.6(8) . . . . no C23 C24 C26 C27 1.7(8) . . . . no C25 C24 C26 C27 -177.7(5) . . . . no C24 C26 C27 C20 -2.0(7) . . . . no C24 C26 C27 C28 -179.9(5) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C6 H6 O2 0.9500 2.5500 3.047(5) 113.00 . yes C7 H7A O1 0.9800 2.2400 3.132(6) 151.00 . yes loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.121 0.256 0.255 115 39 ' ' 2 0.120 0.744 0.745 115 39 ' ' 3 0.379 0.244 0.755 115 39 ' ' 4 0.620 0.756 0.245 115 39 ' ' _platon_squeeze_details ; The unit cell contains a dichloromethane molecule which haas been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _iucr_refine_instructions_details ; TITL AT176 CELL 0.71073 11.3420 19.8800 12.6380 90.0000 101.4110 90.0000 ZERR 2 0.0021 0.0033 0.0014 0.00 0.0088 0.0 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O Pt UNIT 112 116 8 8 4 L.S. 18 ACTA BOND $H FMAP -2 PLAN 10 LIST 4 SIZE 0.288 0.430 0.453 WGHT 0.036800 1.433400 FVAR 2.602880 TEMP -75 Pt1 5 0.530334 0.143113 0.150547 11.000000 0.028750 0.021390 = 0.019860 -0.003450 0.007440 -0.000800 O1 4 0.556964 0.234083 0.232231 11.000000 0.041070 0.023450 = 0.030070 -0.008190 0.011890 -0.005840 O2 4 0.453793 0.104159 0.270804 11.000000 0.037700 0.027110 = 0.021420 -0.004840 0.011780 -0.002820 N1 3 0.610139 0.117512 -0.044052 11.000000 0.034240 0.023080 = 0.021580 -0.001000 0.010340 -0.000780 C1 1 0.603081 0.167762 0.028037 11.000000 0.026880 0.024780 = 0.022850 -0.001830 0.002630 -0.001960 C19 1 0.438571 0.136436 0.355364 11.000000 0.024110 0.033240 = 0.017830 -0.000680 0.002120 0.005360 C8 1 0.628051 0.526976 0.431216 11.000000 0.055500 0.030640 = 0.071900 -0.017700 0.016930 -0.010430 AFIX 137 H8A 2 0.691507 0.541216 0.393543 11.000000 -1.500000 H8B 2 0.655838 0.532784 0.509171 11.000000 -1.500000 H8C 2 0.555987 0.554386 0.406800 11.000000 -1.500000 AFIX 0 C17 1 0.523672 0.247468 0.320929 11.000000 0.027440 0.026580 = 0.026660 -0.007710 0.001580 0.000620 C6 1 0.450753 -0.000618 0.094293 11.000000 0.028310 0.026440 = 0.017150 -0.002000 0.008010 0.000570 AFIX 43 H6 2 0.416268 -0.002639 0.156873 11.000000 -1.200000 AFIX 0 N2 3 0.654132 0.221457 -0.008591 11.000000 0.039290 0.029450 = 0.028910 -0.003070 0.013550 -0.009230 C15 1 0.390839 0.353572 0.190011 11.000000 0.035400 0.033920 = 0.043530 -0.002620 -0.001300 0.000040 AFIX 137 H15A 2 0.340112 0.393190 0.169266 11.000000 -1.500000 H15B 2 0.340817 0.315976 0.205196 11.000000 -1.500000 H15C 2 0.430986 0.341268 0.130874 11.000000 -1.500000 AFIX 0 C14 1 0.484114 0.369396 0.289591 11.000000 0.029070 0.028910 = 0.026830 -0.006810 0.007990 -0.003610 C21 1 0.439839 0.077360 0.532467 11.000000 0.036380 0.032070 = 0.026410 -0.005090 0.007500 0.010740 C11 1 0.632472 0.335395 0.448170 11.000000 0.036280 0.032230 = 0.029960 -0.007050 0.004910 -0.000870 C20 1 0.377513 0.095856 0.428506 11.000000 0.032250 0.021430 = 0.020740 -0.003640 0.005160 0.005600 C3 1 0.666597 0.140508 -0.124314 11.000000 0.046390 0.035760 = 0.025580 -0.000920 0.017560 -0.005340 AFIX 43 H3 2 0.682448 0.115328 -0.183848 11.000000 -1.200000 AFIX 0 C13 1 0.546211 0.319072 0.355840 11.000000 0.027730 0.026970 = 0.025330 -0.006470 0.007770 -0.001870 C10 1 0.657403 0.403421 0.470138 11.000000 0.038380 0.042760 = 0.033190 -0.016470 0.003400 -0.006600 AFIX 43 H10 2 0.717293 0.415083 0.531152 11.000000 -1.200000 AFIX 0 C9 1 0.598561 0.454010 0.406823 11.000000 0.036790 0.032220 = 0.045440 -0.009570 0.017270 -0.004750 C24 1 0.261441 0.018203 0.561921 11.000000 0.050700 0.046840 = 0.041000 0.007820 0.025850 0.005820 C27 1 0.258187 0.075223 0.391787 11.000000 0.033860 0.024530 = 0.028490 -0.001290 0.006570 0.004040 C5 1 0.508625 0.057479 0.069074 11.000000 0.027000 0.023050 = 0.018950 -0.001120 0.005410 0.002590 C2 1 0.694408 0.204281 -0.102511 11.000000 0.046050 0.037200 = 0.032520 0.002770 0.015010 -0.011060 AFIX 43 H2 2 0.734662 0.233272 -0.143498 11.000000 -1.200000 AFIX 0 C4 1 0.554904 0.055164 -0.025473 11.000000 0.027850 0.021540 = 0.022080 0.000930 0.005570 -0.000830 C16 1 0.510994 0.435757 0.317316 11.000000 0.034300 0.026920 = 0.038800 0.000230 0.008230 0.005090 AFIX 43 H16 2 0.468257 0.470268 0.273811 11.000000 -1.200000 AFIX 0 C22 1 0.567107 0.097006 0.574660 11.000000 0.043680 0.050430 = 0.035990 -0.000340 -0.005860 0.008110 AFIX 137 H22A 2 0.569245 0.139741 0.613647 11.000000 -1.500000 H22B 2 0.608969 0.102136 0.514330 11.000000 -1.500000 H22C 2 0.606893 0.062074 0.623780 11.000000 -1.500000 AFIX 0 C26 1 0.202455 0.037916 0.459527 11.000000 0.033770 0.034490 = 0.046200 -0.001870 0.015290 -0.000290 AFIX 43 H26 2 0.120812 0.025199 0.435439 11.000000 -1.200000 AFIX 0 C18 1 0.470012 0.202566 0.381521 11.000000 0.031660 0.029000 = 0.020690 -0.005540 0.008300 0.001960 AFIX 43 H18 2 0.453240 0.218968 0.447588 11.000000 -1.200000 AFIX 0 C28 1 0.188916 0.095192 0.281022 11.000000 0.035740 0.047780 = 0.038460 0.004500 -0.000610 -0.004950 AFIX 137 H28A 2 0.210854 0.065231 0.226442 11.000000 -1.500000 H28B 2 0.208710 0.141696 0.265601 11.000000 -1.500000 H28C 2 0.102415 0.091555 0.279437 11.000000 -1.500000 AFIX 0 C12 1 0.701002 0.282876 0.522019 11.000000 0.047420 0.046360 = 0.042090 -0.003810 -0.011670 -0.002540 AFIX 137 H12A 2 0.780335 0.300583 0.555250 11.000000 -1.500000 H12B 2 0.710782 0.242449 0.480223 11.000000 -1.500000 H12C 2 0.656384 0.271495 0.578533 11.000000 -1.500000 AFIX 0 C7 1 0.660437 0.289036 0.036845 11.000000 0.075560 0.031040 = 0.051860 -0.014560 0.027430 -0.022390 AFIX 137 H7A 2 0.633264 0.288106 0.105773 11.000000 -1.500000 H7B 2 0.608652 0.319236 -0.013349 11.000000 -1.500000 H7C 2 0.743634 0.305214 0.048668 11.000000 -1.500000 AFIX 0 C25 1 0.199304 -0.025014 0.632792 11.000000 0.088760 0.096910 = 0.066450 0.030350 0.040260 -0.002120 AFIX 137 H25A 2 0.143782 0.002770 0.664373 11.000000 -1.500000 H25B 2 0.259559 -0.044925 0.690633 11.000000 -1.500000 H25C 2 0.154305 -0.060894 0.589298 11.000000 -1.500000 AFIX 0 C23 1 0.379144 0.038802 0.596284 11.000000 0.057030 0.053160 = 0.024040 0.009210 0.013300 0.012450 AFIX 43 H23 2 0.420253 0.026095 0.666377 11.000000 -1.200000 AFIX 0 HKLF 4 END ; #===END _database_code_depnum_ccdc_archive 'CCDC 930703'