data_ejw5b # 1. SUBMISSION DETAILS _publ_contact_author ; Jeffrey R. Long Department of Chemistry University of California, Berkeley United States of America ; _publ_contact_author_phone '510 642-0860' _publ_contact_author_fax '510 643-3832' _publ_contact_author_email jlong@cchem.berkeley.edu _publ_requested_journal 'Journal of the American Chemical Society' _publ_requested_category 'FI' _publ_requested_coeditor_name ? _publ_contact_letter ; These structures are part of a paper being submitted to the Journal of the American Chemical Society. ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; New Routes to Transition Metal-Carbido Species: Synthesis and Characterization of the Carbon-Centered Trigonal Prismatic Clusters [W6CCl18]n- (n=1,2,3) ; loop_ _publ_author_name _publ_author_address 'Welch, Eric J.' ; Department of Chemistry University of California, Berkeley United States of America ; 'Crawford, Nathan R. M.' ; Department of Chemistry University of California, Berkeley United States of America ; 'Bergman, Robert G.' ; Department of Chemistry University of California, Berkeley United States of America ; 'Long, Jeffrey R.' ; Department of Chemistry University of California, Berkeley United States of America ; #============================================================================== # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; ? ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C33 H68 Cl18 N2 W6' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H68 Cl18 N2 W6' _chemical_formula_weight 2238.21 _chemical_melting_point ? _chemical_compound_source 'synthetic' 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Fd-3c _symmetry_Int_Tables_number 228 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+3/4, z+1/2' '-x+3/4, y+1/2, -z+1/4' 'x+1/2, -y+1/4, -z+3/4' 'z, x, y' 'z+1/2, -x+1/4, -y+3/4' '-z+1/4, -x+3/4, y+1/2' '-z+3/4, x+1/2, -y+1/4' 'y, z, x' '-y+3/4, z+1/2, -x+1/4' 'y+1/2, -z+1/4, -x+3/4' '-y+1/4, -z+3/4, x+1/2' 'y+3/4, x+1/4, -z' '-y+1/2, -x+1/2, -z+1/2' 'y+1/4, -x, z+3/4' '-y, x+3/4, z+1/4' 'x+3/4, z+1/4, -y' '-x, z+3/4, y+1/4' '-x+1/2, -z+1/2, -y+1/2' 'x+1/4, -z, y+3/4' 'z+3/4, y+1/4, -x' 'z+1/4, -y, x+3/4' '-z, y+3/4, x+1/4' '-z+1/2, -y+1/2, -x+1/2' 'x, y+1/2, z+1/2' '-x+1/4, -y+5/4, z+1' '-x+3/4, y+1, -z+3/4' 'x+1/2, -y+3/4, -z+5/4' 'z, x+1/2, y+1/2' 'z+1/2, -x+3/4, -y+5/4' '-z+1/4, -x+5/4, y+1' '-z+3/4, x+1, -y+3/4' 'y, z+1/2, x+1/2' '-y+3/4, z+1, -x+3/4' 'y+1/2, -z+3/4, -x+5/4' '-y+1/4, -z+5/4, x+1' 'y+3/4, x+3/4, -z+1/2' '-y+1/2, -x+1, -z+1' 'y+1/4, -x+1/2, z+5/4' '-y, x+5/4, z+3/4' 'x+3/4, z+3/4, -y+1/2' '-x, z+5/4, y+3/4' '-x+1/2, -z+1, -y+1' 'x+1/4, -z+1/2, y+5/4' 'z+3/4, y+3/4, -x+1/2' 'z+1/4, -y+1/2, x+5/4' '-z, y+5/4, x+3/4' '-z+1/2, -y+1, -x+1' 'x+1/2, y, z+1/2' '-x+3/4, -y+3/4, z+1' '-x+5/4, y+1/2, -z+3/4' 'x+1, -y+1/4, -z+5/4' 'z+1/2, x, y+1/2' 'z+1, -x+1/4, -y+5/4' '-z+3/4, -x+3/4, y+1' '-z+5/4, x+1/2, -y+3/4' 'y+1/2, z, x+1/2' '-y+5/4, z+1/2, -x+3/4' 'y+1, -z+1/4, -x+5/4' '-y+3/4, -z+3/4, x+1' 'y+5/4, x+1/4, -z+1/2' '-y+1, -x+1/2, -z+1' 'y+3/4, -x, z+5/4' '-y+1/2, x+3/4, z+3/4' 'x+5/4, z+1/4, -y+1/2' '-x+1/2, z+3/4, y+3/4' '-x+1, -z+1/2, -y+1' 'x+3/4, -z, y+5/4' 'z+5/4, y+1/4, -x+1/2' 'z+3/4, -y, x+5/4' '-z+1/2, y+3/4, x+3/4' '-z+1, -y+1/2, -x+1' 'x+1/2, y+1/2, z' '-x+3/4, -y+5/4, z+1/2' '-x+5/4, y+1, -z+1/4' 'x+1, -y+3/4, -z+3/4' 'z+1/2, x+1/2, y' 'z+1, -x+3/4, -y+3/4' '-z+3/4, -x+5/4, y+1/2' '-z+5/4, x+1, -y+1/4' 'y+1/2, z+1/2, x' '-y+5/4, z+1, -x+1/4' 'y+1, -z+3/4, -x+3/4' '-y+3/4, -z+5/4, x+1/2' 'y+5/4, x+3/4, -z' '-y+1, -x+1, -z+1/2' 'y+3/4, -x+1/2, z+3/4' '-y+1/2, x+5/4, z+1/4' 'x+5/4, z+3/4, -y' '-x+1/2, z+5/4, y+1/4' '-x+1, -z+1, -y+1/2' 'x+3/4, -z+1/2, y+3/4' 'z+5/4, y+3/4, -x' 'z+3/4, -y+1/2, x+3/4' '-z+1/2, y+5/4, x+1/4' '-z+1, -y+1, -x+1/2' '-x, -y, -z' 'x-1/4, y-3/4, -z-1/2' 'x-3/4, -y-1/2, z-1/4' '-x-1/2, y-1/4, z-3/4' '-z, -x, -y' '-z-1/2, x-1/4, y-3/4' 'z-1/4, x-3/4, -y-1/2' 'z-3/4, -x-1/2, y-1/4' '-y, -z, -x' 'y-3/4, -z-1/2, x-1/4' '-y-1/2, z-1/4, x-3/4' 'y-1/4, z-3/4, -x-1/2' '-y-3/4, -x-1/4, z' 'y-1/2, x-1/2, z-1/2' '-y-1/4, x, -z-3/4' 'y, -x-3/4, -z-1/4' '-x-3/4, -z-1/4, y' 'x, -z-3/4, -y-1/4' 'x-1/2, z-1/2, y-1/2' '-x-1/4, z, -y-3/4' '-z-3/4, -y-1/4, x' '-z-1/4, y, -x-3/4' 'z, -y-3/4, -x-1/4' 'z-1/2, y-1/2, x-1/2' '-x, -y+1/2, -z+1/2' 'x-1/4, y-1/4, -z' 'x-3/4, -y, z+1/4' '-x-1/2, y+1/4, z-1/4' '-z, -x+1/2, -y+1/2' '-z-1/2, x+1/4, y-1/4' 'z-1/4, x-1/4, -y' 'z-3/4, -x, y+1/4' '-y, -z+1/2, -x+1/2' 'y-3/4, -z, x+1/4' '-y-1/2, z+1/4, x-1/4' 'y-1/4, z-1/4, -x' '-y-3/4, -x+1/4, z+1/2' 'y-1/2, x, z' '-y-1/4, x+1/2, -z-1/4' 'y, -x-1/4, -z+1/4' '-x-3/4, -z+1/4, y+1/2' 'x, -z-1/4, -y+1/4' 'x-1/2, z, y' '-x-1/4, z+1/2, -y-1/4' '-z-3/4, -y+1/4, x+1/2' '-z-1/4, y+1/2, -x-1/4' 'z, -y-1/4, -x+1/4' 'z-1/2, y, x' '-x+1/2, -y, -z+1/2' 'x+1/4, y-3/4, -z' 'x-1/4, -y-1/2, z+1/4' '-x, y-1/4, z-1/4' '-z+1/2, -x, -y+1/2' '-z, x-1/4, y-1/4' 'z+1/4, x-3/4, -y' 'z-1/4, -x-1/2, y+1/4' '-y+1/2, -z, -x+1/2' 'y-1/4, -z-1/2, x+1/4' '-y, z-1/4, x-1/4' 'y+1/4, z-3/4, -x' '-y-1/4, -x-1/4, z+1/2' 'y, x-1/2, z' '-y+1/4, x, -z-1/4' 'y+1/2, -x-3/4, -z+1/4' '-x-1/4, -z-1/4, y+1/2' 'x+1/2, -z-3/4, -y+1/4' 'x, z-1/2, y' '-x+1/4, z, -y-1/4' '-z-1/4, -y-1/4, x+1/2' '-z+1/4, y, -x-1/4' 'z+1/2, -y-3/4, -x+1/4' 'z, y-1/2, x' '-x+1/2, -y+1/2, -z' 'x+1/4, y-1/4, -z-1/2' 'x-1/4, -y, z-1/4' '-x, y+1/4, z-3/4' '-z+1/2, -x+1/2, -y' '-z, x+1/4, y-3/4' 'z+1/4, x-1/4, -y-1/2' 'z-1/4, -x, y-1/4' '-y+1/2, -z+1/2, -x' 'y-1/4, -z, x-1/4' '-y, z+1/4, x-3/4' 'y+1/4, z-1/4, -x-1/2' '-y-1/4, -x+1/4, z' 'y, x, z-1/2' '-y+1/4, x+1/2, -z-3/4' 'y+1/2, -x-1/4, -z-1/4' '-x-1/4, -z+1/4, y' 'x+1/2, -z-1/4, -y-1/4' 'x, z, y-1/2' '-x+1/4, z+1/2, -y-3/4' '-z-1/4, -y+1/4, x' '-z+1/4, y+1/2, -x-3/4' 'z+1/2, -y-1/4, -x-1/4' 'z, y, x-1/2' _cell_length_a 36.0040(5) _cell_length_b 36.0040(5) _cell_length_c 36.0040(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 46671.6(11) _cell_formula_units_Z 32 _cell_measurement_temperature 129 _cell_measurement_reflns_used 24495 _cell_measurement_theta_min 4.51 _cell_measurement_theta_max 49.25 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.528 _exptl_crystal_density_method ? _exptl_crystal_F_000 32512 _exptl_absorpt_coefficient_mu 12.633 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3341 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'SMART' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24495 _diffrn_reflns_av_R_equivalents 0.1105 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 20.78 _reflns_number_total 1011 _reflns_number_observed 829 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement ; SMART (Siemens, 1995), SAINT (Siemens, 1995) ; _computing_data_reduction ; SAINT (Siemens, 1995), XPREP (Siemens, 1995) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or 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 w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+2945.4414P] 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 SHELXL _refine_ls_extinction_coef 0.000001(0) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1011 _refine_ls_number_parameters 67 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_obs 0.0428 _refine_ls_wR_factor_all 0.1142 _refine_ls_wR_factor_obs 0.1032 _refine_ls_goodness_of_fit_all 1.126 _refine_ls_goodness_of_fit_obs 1.131 _refine_ls_restrained_S_all 1.126 _refine_ls_restrained_S_obs 1.131 _refine_ls_shift/esd_max -0.156 _refine_ls_shift/esd_mean 0.019 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 W W 0.22567(2) 0.49401(2) 0.55449(2) 0.0516(4) Uani 1 d . . C1 C 0.2500 0.5000 0.5000 0.054(10) Uani 1 d S . Cl1 Cl 0.2067(2) 0.4699(2) 0.61500(12) 0.100(2) Uani 1 d . . Cl2 Cl 0.16250(13) 0.5126(2) 0.55025(14) 0.087(2) Uani 1 d . . Cl3 Cl 0.28571(13) 0.46559(11) 0.57029(11) 0.0639(12) Uani 1 d . . N1 N 0.3750 0.6250 0.6250 0.120(13) Uiso 1 d S . C2 C 0.3949(13) 0.6132(15) 0.5771(13) 0.238(23) Uiso 1 d . . H2A H 0.3770(13) 0.5953(15) 0.5678(13) 0.286 Uiso 1 calc R . H2B H 0.3900(13) 0.6358(15) 0.5632(13) 0.286 Uiso 1 calc R . C3 C 0.4219(20) 0.6031(22) 0.5642(22) 0.381(45) Uiso 1 d . . H3A H 0.4275(20) 0.5785(22) 0.5736(22) 0.457 Uiso 1 calc R . H3B H 0.4419(20) 0.6196(22) 0.5716(22) 0.457 Uiso 1 calc R . C4 C 0.4198(9) 0.6019(9) 0.5220(9) 0.150(11) Uiso 1 d . . H4A H 0.3960(9) 0.5932(9) 0.5127(9) 0.180 Uiso 1 calc R . H4B H 0.4267(9) 0.6251(9) 0.5102(9) 0.180 Uiso 1 calc R . C5 C 0.4465(12) 0.5760(13) 0.5206(14) 0.245(22) Uiso 1 d . . H5A H 0.4638(64) 0.5821(61) 0.5012(76) 0.367 Uiso 1 calc R . H5B H 0.4355(18) 0.5522(22) 0.5155(115) 0.367 Uiso 1 calc R . H5C H 0.4593(75) 0.5751(81) 0.5440(40) 0.367 Uiso 1 calc R . N2 N 0.1250 0.6250 0.6250 0.107(20) Uiso 1 d SD . C6 C 0.1490(5) 0.6490(5) 0.6010(5) 0.378(62) Uiso 1 d SD . C7 C 0.1930(21) 0.6930(21) 0.5570(21) 0.253(45) Uiso 1 d S . C8 C 0.1747(18) 0.6747(18) 0.5753(18) 0.280(49) Uiso 1 d S . C9 C 0.2092(17) 0.7092(17) 0.5408(17) 0.288(55) Uiso 1 d S . 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 W 0.0626(6) 0.0563(5) 0.0359(5) 0.0044(3) -0.0037(3) -0.0163(3) C1 0.054(10) 0.054(10) 0.054(10) 0.000(11) 0.000(11) 0.000(11) Cl1 0.140(5) 0.125(5) 0.035(3) 0.012(3) 0.005(3) -0.047(4) Cl2 0.058(3) 0.121(4) 0.082(3) 0.003(3) 0.013(3) -0.006(3) Cl3 0.087(3) 0.049(3) 0.055(2) 0.015(2) -0.036(2) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W C1 2.1595(6) . ? W Cl2 2.376(5) . ? W Cl2 2.386(5) 34_545 ? W Cl1 2.443(4) . ? W Cl3 2.458(4) . ? W Cl3 2.459(4) 43 ? W W 2.6673(11) 55_554 ? W W 2.6674(11) 34_545 ? W W 3.0278(14) 43 ? C1 W 2.1594(6) 43 ? C1 W 2.1594(6) 13_456 ? C1 W 2.1595(6) 70_464 ? C1 W 2.1595(6) 55_554 ? C1 W 2.1596(6) 34_545 ? Cl2 W 2.386(5) 55_554 ? Cl3 W 2.460(4) 43 ? N1 C2 1.91(5) 116_657 ? N1 C2 1.91(5) . ? N1 C2 1.91(5) 52_465 ? N1 C2 1.91(5) 185_665 ? C2 C3 1.14(8) . ? C3 C4 1.52(8) . ? C4 C5 1.34(5) . ? N2 C6 1.49(3) 26_554 ? N2 C6 1.49(3) 52_465 ? N2 C6 1.49(3) . ? N2 C6 1.49(3) 75_446 ? C6 C8 1.61(11) . ? C7 C9 1.01(14) . ? C7 C8 1.14(13) . ? 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 C1 W Cl2 107.56(12) . . ? C1 W Cl2 107.21(13) . 34_545 ? Cl2 W Cl2 87.9(3) . 34_545 ? C1 W Cl1 163.6(2) . . ? Cl2 W Cl1 83.6(2) . . ? Cl2 W Cl1 84.7(2) 34_545 . ? C1 W Cl3 83.97(10) . . ? Cl2 W Cl3 166.9(2) . . ? Cl2 W Cl3 94.7(2) 34_545 . ? Cl1 W Cl3 83.8(2) . . ? C1 W Cl3 83.95(9) . 43 ? Cl2 W Cl3 95.0(2) . 43 ? Cl2 W Cl3 167.1(2) 34_545 43 ? Cl1 W Cl3 83.2(2) . 43 ? Cl3 W Cl3 79.8(2) . 43 ? C1 W W 51.861(14) . 55_554 ? Cl2 W W 56.11(12) . 55_554 ? Cl2 W W 97.55(12) 34_545 55_554 ? Cl1 W W 139.4(2) . 55_554 ? Cl3 W W 135.83(10) . 55_554 ? Cl3 W W 94.44(10) 43 55_554 ? C1 W W 51.862(14) . 34_545 ? Cl2 W W 97.80(14) . 34_545 ? Cl2 W W 55.75(12) 34_545 34_545 ? Cl1 W W 140.15(13) . 34_545 ? Cl3 W W 94.24(10) . 34_545 ? Cl3 W W 135.80(9) 43 34_545 ? W W W 60.0 55_554 34_545 ? C1 W W 45.49(2) . 43 ? Cl2 W W 132.79(13) . 43 ? Cl2 W W 132.39(15) 34_545 43 ? Cl1 W W 118.1(2) . 43 ? Cl3 W W 52.02(10) . 43 ? Cl3 W W 51.98(10) 43 43 ? W W W 90.045(11) 55_554 43 ? W W W 89.953(12) 34_545 43 ? W C1 W 76.28(3) 43 13_456 ? W C1 W 76.28(3) 43 70_464 ? W C1 W 76.28(3) 13_456 70_464 ? W C1 W 89.02(4) 43 . ? W C1 W 138.11(3) 13_456 . ? W C1 W 138.34(3) 70_464 . ? W C1 W 138.35(3) 43 55_554 ? W C1 W 89.02(4) 13_456 55_554 ? W C1 W 138.10(3) 70_464 55_554 ? W C1 W 76.28(3) . 55_554 ? W C1 W 138.10(3) 43 34_545 ? W C1 W 138.34(3) 13_456 34_545 ? W C1 W 89.02(4) 70_464 34_545 ? W C1 W 76.28(3) . 34_545 ? W C1 W 76.27(3) 55_554 34_545 ? W Cl2 W 68.14(13) . 55_554 ? W Cl3 W 76.00(11) . 43 ? C2 N1 C2 98.0(10) 116_657 . ? C2 N1 C2 98.0(10) 116_657 52_465 ? C2 N1 C2 136.1(28) . 52_465 ? C2 N1 C2 136.1(28) 116_657 185_665 ? C2 N1 C2 98.0(10) . 185_665 ? C2 N1 C2 98.0(10) 52_465 185_665 ? C3 C2 N1 139.2(63) . . ? C2 C3 C4 111.9(69) . . ? C5 C4 C3 91.3(41) . . ? C6 N2 C6 109.462(1) 26_554 52_465 ? C6 N2 C6 109.452(2) 26_554 . ? C6 N2 C6 109.503(4) 52_465 . ? C6 N2 C6 109.505(4) 26_554 75_446 ? C6 N2 C6 109.454(5) 52_465 75_446 ? C6 N2 C6 109.451(2) . 75_446 ? N2 C6 C8 179.9(11) . . ? C9 C7 C8 179.8(65) . . ? C7 C8 C6 179.6(15) . . ? _refine_diff_density_max 1.628 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.181