# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1148 data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Hubert Wadepohl Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Bundesrepublik Deutschland ; _publ_contact_author_phone '049 6221 54-4827' _publ_contact_author_fax '049 6221 54-5609' _publ_contact_author_email bu9@ix.urz.uni-heidelberg.de _publ_requested_journal 'J.Chem.Soc., Chem. Commun.' _publ_requested_coeditor_name ? #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and X-ray structure of a cluster complex with facial coordination of C8H8 to a Co2Ni triange. ; loop_ _publ_author_name _publ_author_address 'Wadepohl. Hubert' ; Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; 'Gebert, Stefan' ; Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; 'Merkel, Ruediger' ; Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; 'Pritzkow, Hans' ; Anorganisch-Chemisches Institut Universitaet Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg ; #============================================================================== data_sg191a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H14 Co2 Ni O6' _chemical_formula_weight 526.91 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 10.203(5) _cell_length_b 16.674(8) _cell_length_c 11.902(6) _cell_angle_alpha 90.00(3) _cell_angle_beta 101.19(2) _cell_angle_gamma 90.00(3) _cell_volume 1986.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 14.4 _cell_measurement_theta_max 15.1 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method ? _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 2.62 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.579 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens-Stoe AED2' _diffrn_measurement_method omega-scan _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3454 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.99 _reflns_number_total 3454 _reflns_number_observed 2261 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'DIF4 (Stoe)' _computing_cell_refinement 'DIF4 (Stoe)' _computing_data_reduction 'REDU4 (Stoe)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (C.K.Johnson, 1965)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; The identity of the metal atoms could not be determined unambigously. All metal atoms were refined as cobalt atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3454 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_obs 0.0401 _refine_ls_wR_factor_all 0.0942 _refine_ls_wR_factor_obs 0.0790 _refine_ls_goodness_of_fit_all 1.035 _refine_ls_goodness_of_fit_obs 1.101 _refine_ls_restrained_S_all 1.035 _refine_ls_restrained_S_obs 1.101 _refine_ls_shift/esd_max 0.008 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.27003(6) 0.55654(3) 0.25200(5) 0.03224(15) Uani 1 d . . Co2 Co 0.22031(6) 0.43363(3) 0.12899(5) 0.03118(15) Uani 1 d . . Co3 Co 0.40046(6) 0.43073(3) 0.30753(6) 0.0327(2) Uani 1 d . . O1 O 0.1560(4) 0.6928(2) 0.3541(4) 0.0635(11) Uani 1 d . . O2 O 0.0032(4) 0.3495(2) -0.0195(3) 0.0472(9) Uani 1 d . . O3 O 0.5321(4) 0.3336(2) 0.5006(3) 0.0517(9) Uani 1 d . . O4 O -0.0082(4) 0.5051(2) 0.2063(3) 0.0488(9) Uani 1 d . . O5 O 0.1993(4) 0.3056(2) 0.2923(3) 0.0514(9) Uani 1 d . . O6 O 0.2621(4) 0.4952(2) 0.4806(3) 0.0553(10) Uani 1 d . . C1 C 0.4438(5) 0.6045(3) 0.2049(5) 0.0415(12) Uani 1 d . . C2 C 0.3431(6) 0.6011(3) 0.1071(5) 0.0444(12) Uani 1 d . . C3 C 0.2915(6) 0.5399(3) 0.0283(5) 0.0443(12) Uani 1 d . . C4 C 0.3298(5) 0.4612(3) 0.0030(4) 0.0417(12) Uani 1 d . . C5 C 0.4099(5) 0.4034(3) 0.0707(5) 0.0402(11) Uani 1 d . . C6 C 0.5122(5) 0.4058(3) 0.1718(5) 0.0413(12) Uani 1 d . . C7 C 0.5704(5) 0.4668(3) 0.2476(5) 0.0410(11) Uani 1 d . . C8 C 0.5306(5) 0.5453(3) 0.2673(5) 0.0417(11) Uani 1 d . . C9 C 0.2023(5) 0.6420(3) 0.3105(5) 0.0435(12) Uani 1 d . . C10 C 0.0916(5) 0.3807(2) 0.0369(4) 0.0327(10) Uani 1 d . . C11 C 0.4816(5) 0.3709(2) 0.4226(5) 0.0365(11) Uani 1 d . . C12 C 0.1036(6) 0.4984(2) 0.1971(4) 0.0362(11) Uani 1 d . . C13 C 0.2463(5) 0.3619(2) 0.2568(5) 0.0356(11) Uani 1 d . . C14 C 0.2980(5) 0.4929(2) 0.3930(5) 0.0380(12) Uani 1 d . . C15 C 0.1772(6) 0.3087(3) 0.7651(6) 0.060(2) Uani 1 d . . C16 C 0.2027(8) 0.3051(4) 0.6531(6) 0.069(2) Uani 1 d . . C17 C 0.2934(7) 0.2493(4) 0.6274(7) 0.066(2) Uani 1 d . . C18 C 0.3572(7) 0.1987(4) 0.7125(7) 0.068(2) Uani 1 d . . C19 C 0.3322(6) 0.2022(3) 0.8204(6) 0.063(2) Uani 1 d . . C20 C 0.2412(6) 0.2579(3) 0.8466(6) 0.056(2) Uani 1 d . . H1 H 0.4680(58) 0.6582(31) 0.2414(50) 0.069(18) Uiso 1 d . . H2 H 0.2981(51) 0.6528(26) 0.0861(46) 0.045(14) Uiso 1 d . . H3 H 0.2248(51) 0.5607(26) -0.0300(45) 0.045(14) Uiso 1 d . . H4 H 0.2906(52) 0.4410(27) -0.0716(46) 0.049(15) Uiso 1 d . . H5 H 0.4109(50) 0.3489(27) 0.0277(44) 0.048(14) Uiso 1 d . . H6 H 0.5646(44) 0.3583(24) 0.1858(39) 0.032(12) Uiso 1 d . . H7 H 0.6525(46) 0.4545(24) 0.3005(39) 0.033(12) Uiso 1 d . . H8 H 0.5802(42) 0.5668(22) 0.3303(38) 0.021(11) Uiso 1 d . . H15 H 0.1107(58) 0.3459(31) 0.7772(49) 0.066(17) Uiso 1 d . . H16 H 0.1594(59) 0.3371(31) 0.6002(51) 0.063(19) Uiso 1 d . . H17 H 0.3118(56) 0.2460(31) 0.5487(49) 0.070(18) Uiso 1 d . . H18 H 0.4185(68) 0.1597(36) 0.6917(57) 0.087(21) Uiso 1 d . . H19 H 0.4000(78) 0.1737(42) 0.8935(68) 0.129(30) Uiso 1 d . . H20 H 0.2161(65) 0.2567(36) 0.9235(57) 0.097(23) Uiso 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 Co1 0.0352(3) 0.0276(2) 0.0348(3) -0.0019(3) 0.0091(2) -0.0015(3) Co2 0.0319(3) 0.0322(3) 0.0303(3) -0.0012(3) 0.0082(2) -0.0026(3) Co3 0.0307(3) 0.0350(3) 0.0327(4) 0.0043(3) 0.0067(2) 0.0000(3) O1 0.072(3) 0.045(2) 0.077(3) -0.018(2) 0.023(2) 0.005(2) O2 0.046(2) 0.050(2) 0.047(2) -0.007(2) 0.010(2) -0.011(2) O3 0.060(3) 0.047(2) 0.046(2) 0.010(2) 0.004(2) 0.005(2) O4 0.039(2) 0.045(2) 0.064(3) -0.006(2) 0.013(2) 0.003(2) O5 0.056(2) 0.042(2) 0.057(2) 0.009(2) 0.011(2) -0.010(2) O6 0.059(3) 0.071(2) 0.039(2) 0.001(2) 0.017(2) 0.009(2) C1 0.042(3) 0.034(2) 0.051(3) -0.005(2) 0.017(2) -0.010(2) C2 0.060(4) 0.034(2) 0.041(3) 0.006(2) 0.015(3) 0.002(2) C3 0.042(3) 0.055(3) 0.036(3) 0.014(2) 0.009(2) 0.001(2) C4 0.041(3) 0.056(3) 0.031(3) -0.006(2) 0.015(2) -0.016(2) C5 0.042(3) 0.040(2) 0.044(3) -0.006(2) 0.019(2) -0.001(2) C6 0.039(3) 0.040(2) 0.049(3) 0.008(2) 0.020(2) 0.010(2) C7 0.027(3) 0.054(3) 0.041(3) 0.013(2) 0.006(2) 0.001(2) C8 0.036(3) 0.051(3) 0.038(3) -0.005(2) 0.006(2) -0.013(2) C9 0.047(3) 0.039(2) 0.045(3) 0.001(2) 0.010(2) -0.006(2) C10 0.032(3) 0.032(2) 0.035(3) 0.000(2) 0.010(2) 0.003(2) C11 0.039(3) 0.033(2) 0.037(3) 0.001(2) 0.006(2) 0.002(2) C12 0.044(3) 0.033(2) 0.032(3) 0.005(2) 0.006(2) -0.001(2) C13 0.031(3) 0.033(2) 0.044(3) 0.006(2) 0.011(2) 0.004(2) C14 0.043(3) 0.035(2) 0.035(3) -0.002(2) 0.006(2) -0.004(2) C15 0.048(4) 0.055(3) 0.077(5) -0.020(3) 0.015(3) 0.003(3) C16 0.083(5) 0.053(3) 0.068(5) 0.003(3) 0.005(4) -0.017(3) C17 0.069(5) 0.072(4) 0.066(5) -0.030(4) 0.036(4) -0.033(3) C18 0.045(4) 0.071(4) 0.092(6) -0.036(4) 0.024(3) -0.008(3) C19 0.056(4) 0.057(3) 0.075(5) -0.014(3) 0.010(3) 0.000(3) C20 0.048(4) 0.062(3) 0.064(4) -0.021(3) 0.022(3) -0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C9 1.783(5) . ? Co1 C12 1.954(5) . ? Co1 C14 1.959(5) . ? Co1 C1 2.118(5) . ? Co1 C2 2.140(5) . ? Co1 Co3 2.5033(14) . ? Co1 Co2 2.5125(14) . ? Co2 C10 1.774(5) . ? Co2 C12 1.902(5) . ? Co2 C13 1.913(5) . ? Co2 C4 2.087(5) . ? Co2 C5 2.236(5) . ? Co2 C3 2.333(5) . ? Co2 Co3 2.5260(13) . ? Co3 C11 1.765(5) . ? Co3 C14 1.902(5) . ? Co3 C13 1.947(5) . ? Co3 C7 2.088(5) . ? Co3 C6 2.190(5) . ? Co3 C8 2.427(5) . ? O1 C9 1.143(5) . ? O2 C10 1.140(6) . ? O3 C11 1.153(6) . ? O4 C12 1.172(6) . ? O5 C13 1.169(5) . ? O6 C14 1.172(6) . ? C1 C2 1.396(8) . ? C1 C8 1.434(8) . ? C1 H1 1.00(5) . ? C2 C3 1.417(8) . ? C2 H2 0.99(5) . ? C3 C4 1.418(7) . ? C3 H3 0.94(5) . ? C4 C5 1.411(7) . ? C4 H4 0.96(5) . ? C5 C6 1.432(8) . ? C5 H5 1.04(5) . ? C6 C7 1.412(7) . ? C6 H6 0.95(4) . ? C7 C8 1.404(7) . ? C7 H7 0.97(5) . ? C8 H8 0.89(4) . ? C15 C20 1.357(9) . ? C15 C16 1.408(9) . ? C15 H15 0.95(5) . ? C16 C17 1.388(9) . ? C16 H16 0.88(6) . ? C17 C18 1.381(10) . ? C17 H17 0.99(5) . ? C18 C19 1.358(9) . ? C18 H18 0.97(6) . ? C19 C20 1.390(8) . ? C19 H19 1.11(8) . ? C20 H20 1.00(6) . ? 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 C9 Co1 C12 98.6(2) . . ? C9 Co1 C14 95.8(2) . . ? C12 Co1 C14 89.5(2) . . ? C9 Co1 C1 102.1(2) . . ? C12 Co1 C1 144.7(2) . . ? C14 Co1 C1 116.2(2) . . ? C9 Co1 C2 105.0(2) . . ? C12 Co1 C2 108.6(2) . . ? C14 Co1 C2 149.6(2) . . ? C1 Co1 C2 38.3(2) . . ? C9 Co1 Co3 142.5(2) . . ? C12 Co1 Co3 93.19(14) . . ? C14 Co1 Co3 48.59(14) . . ? C1 Co1 Co3 87.54(14) . . ? C2 Co1 Co3 104.68(15) . . ? C9 Co1 Co2 146.1(2) . . ? C12 Co1 Co2 48.43(14) . . ? C14 Co1 Co2 92.12(14) . . ? C1 Co1 Co2 103.81(14) . . ? C2 Co1 Co2 82.89(14) . . ? Co3 Co1 Co2 60.48(4) . . ? C10 Co2 C12 95.5(2) . . ? C10 Co2 C13 98.7(2) . . ? C12 Co2 C13 91.0(2) . . ? C10 Co2 C4 95.8(2) . . ? C12 Co2 C4 130.4(2) . . ? C13 Co2 C4 134.3(2) . . ? C10 Co2 C5 106.1(2) . . ? C12 Co2 C5 155.7(2) . . ? C13 Co2 C5 96.4(2) . . ? C4 Co2 C5 37.9(2) . . ? C10 Co2 C3 109.1(2) . . ? C12 Co2 C3 94.1(2) . . ? C13 Co2 C3 151.0(2) . . ? C4 Co2 C3 36.9(2) . . ? C5 Co2 C3 68.7(2) . . ? C10 Co2 Co1 143.84(14) . . ? C12 Co2 Co1 50.3(2) . . ? C13 Co2 Co1 93.8(2) . . ? C4 Co2 Co1 99.42(14) . . ? C5 Co2 Co1 106.00(13) . . ? C3 Co2 Co1 68.41(14) . . ? C10 Co2 Co3 147.25(15) . . ? C12 Co2 Co3 93.8(2) . . ? C13 Co2 Co3 49.7(2) . . ? C4 Co2 Co3 101.8(2) . . ? C5 Co2 Co3 74.01(15) . . ? C3 Co2 Co3 101.4(2) . . ? Co1 Co2 Co3 59.58(4) . . ? C11 Co3 C14 96.7(2) . . ? C11 Co3 C13 97.8(2) . . ? C14 Co3 C13 89.6(2) . . ? C11 Co3 C7 97.6(2) . . ? C14 Co3 C7 127.2(2) . . ? C13 Co3 C7 137.6(2) . . ? C11 Co3 C6 103.4(2) . . ? C14 Co3 C6 156.5(2) . . ? C13 Co3 C6 99.5(2) . . ? C7 Co3 C6 38.4(2) . . ? C11 Co3 C8 113.9(2) . . ? C14 Co3 C8 93.1(2) . . ? C13 Co3 C8 147.5(2) . . ? C7 Co3 C8 35.2(2) . . ? C6 Co3 C8 67.7(2) . . ? C11 Co3 Co1 145.5(2) . . ? C14 Co3 Co1 50.6(2) . . ? C13 Co3 Co1 93.23(14) . . ? C7 Co3 Co1 95.89(14) . . ? C6 Co3 Co1 106.88(13) . . ? C8 Co3 Co1 64.62(14) . . ? C11 Co3 Co2 144.9(2) . . ? C14 Co3 Co2 93.1(2) . . ? C13 Co3 Co2 48.6(2) . . ? C7 Co3 Co2 102.9(2) . . ? C6 Co3 Co2 77.4(2) . . ? C8 Co3 Co2 98.95(14) . . ? Co1 Co3 Co2 59.94(4) . . ? C2 C1 C8 133.2(5) . . ? C2 C1 Co1 71.7(3) . . ? C8 C1 Co1 93.9(3) . . ? C2 C1 H1 118.5(35) . . ? C8 C1 H1 108.3(35) . . ? Co1 C1 H1 111.7(30) . . ? C1 C2 C3 134.4(5) . . ? C1 C2 Co1 70.0(3) . . ? C3 C2 Co1 98.1(3) . . ? C1 C2 H2 114.0(32) . . ? C3 C2 H2 111.5(33) . . ? Co1 C2 H2 106.9(28) . . ? C2 C3 C4 136.5(5) . . ? C2 C3 Co2 108.6(3) . . ? C4 C3 Co2 62.1(3) . . ? C2 C3 H3 110.3(29) . . ? C4 C3 H3 112.0(29) . . ? Co2 C3 H3 114.0(29) . . ? C5 C4 C3 131.6(5) . . ? C5 C4 Co2 76.8(3) . . ? C3 C4 Co2 81.0(3) . . ? C5 C4 H4 112.3(29) . . ? C3 C4 H4 116.0(29) . . ? Co2 C4 H4 113.7(29) . . ? C4 C5 C6 135.1(5) . . ? C4 C5 Co2 65.3(3) . . ? C6 C5 Co2 105.5(3) . . ? C4 C5 H5 112.0(29) . . ? C6 C5 H5 111.2(30) . . ? Co2 C5 H5 116.1(27) . . ? C7 C6 C5 134.8(5) . . ? C7 C6 Co3 66.8(3) . . ? C5 C6 Co3 103.1(3) . . ? C7 C6 H6 109.6(29) . . ? C5 C6 H6 114.6(29) . . ? Co3 C6 H6 112.5(26) . . ? C8 C7 C6 132.8(5) . . ? C8 C7 Co3 85.7(3) . . ? C6 C7 Co3 74.7(3) . . ? C8 C7 H7 109.3(26) . . ? C6 C7 H7 117.9(25) . . ? Co3 C7 H7 112.8(26) . . ? C7 C8 C1 136.5(5) . . ? C7 C8 Co3 59.1(3) . . ? C1 C8 Co3 109.7(3) . . ? C7 C8 H8 112.3(26) . . ? C1 C8 H8 110.5(26) . . ? Co3 C8 H8 113.1(26) . . ? O1 C9 Co1 174.6(4) . . ? O2 C10 Co2 175.7(4) . . ? O3 C11 Co3 177.2(4) . . ? O4 C12 Co2 142.7(4) . . ? O4 C12 Co1 136.0(4) . . ? Co2 C12 Co1 81.3(2) . . ? O5 C13 Co2 141.8(5) . . ? O5 C13 Co3 136.4(5) . . ? Co2 C13 Co3 81.7(2) . . ? O6 C14 Co3 142.5(4) . . ? O6 C14 Co1 136.6(4) . . ? Co3 C14 Co1 80.8(2) . . ? C20 C15 C16 119.9(6) . . ? C20 C15 H15 123.9(35) . . ? C16 C15 H15 116.1(36) . . ? C17 C16 C15 119.4(7) . . ? C17 C16 H16 121.0(40) . . ? C15 C16 H16 119.6(40) . . ? C18 C17 C16 119.2(6) . . ? C18 C17 H17 120.7(33) . . ? C16 C17 H17 120.1(34) . . ? C19 C18 C17 121.3(6) . . ? C19 C18 H18 121.4(41) . . ? C17 C18 H18 117.3(41) . . ? C18 C19 C20 119.8(7) . . ? C18 C19 H19 121.3(39) . . ? C20 C19 H19 116.9(39) . . ? C15 C20 C19 120.4(6) . . ? C15 C20 H20 119.7(38) . . ? C19 C20 H20 119.6(38) . . ? _refine_diff_density_max 0.278 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.071