# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Wolfram Willy Seidel' _publ_contact_author_address ; Institut fuer Anorganische und Analytische Chemie Westfaelische Wilhelms-Universitaet Muenster Corrensstrasse 30/36 Muenster 48149 GERMANY ; _publ_contact_author_email SEIDELWW@UNI-MUENSTER.DE _publ_section_title ; Acetylenedithiolate alkyne complex formation renders it a dithiolate chelate ligand ; loop_ _publ_author_name 'Wolfram Willy Seidel' 'Tania Pape' 'Markus Schaffrath' data_Ni_complex_2 _database_code_depnum_ccdc_archive 'CCDC 610641' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H60 B2 N12 Ni O4 S4 W2' _chemical_formula_weight 1493.39 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(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 10.1411(17) _cell_length_b 18.928(3) _cell_length_c 15.605(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.751(3) _cell_angle_gamma 90.00 _cell_volume 2932.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description prism _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 4.427 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5564 _exptl_absorpt_correction_T_max 0.7771 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33188 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 30.06 _reflns_number_total 8547 _reflns_number_gt 7142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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^)+(0.0391P)^2^+7.1498P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8547 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 0.5000 0.5000 0.01912(17) Uani 1 2 d S . . S1 S 0.65364(12) 0.54833(6) 0.60451(8) 0.0242(2) Uani 1 1 d . . . S2 S 0.54598(13) 0.39185(6) 0.55164(8) 0.0254(3) Uani 1 1 d . . . C1 C 0.7175(4) 0.4768(2) 0.6624(3) 0.0202(9) Uani 1 1 d . . . C2 C 0.6726(5) 0.4103(2) 0.6363(3) 0.0213(9) Uani 1 1 d . . . W1 W 0.827945(18) 0.404932(9) 0.742379(11) 0.01825(6) Uani 1 1 d . . . C3 C 0.7919(5) 0.3089(3) 0.6883(3) 0.0271(10) Uani 1 1 d . . . C4 C 0.6825(5) 0.3862(3) 0.8104(3) 0.0256(10) Uani 1 1 d . . . O3 O 0.7674(4) 0.2549(2) 0.6553(3) 0.0415(10) Uani 1 1 d . . . O4 O 0.5981(4) 0.3744(2) 0.8467(3) 0.0404(10) Uani 1 1 d . . . B1 B 1.1420(5) 0.4461(3) 0.8309(4) 0.0242(11) Uani 1 1 d . . . H1 H 1.2373 0.4585 0.8579 0.029 Uiso 1 1 calc R . . N1 N 1.0020(4) 0.4227(2) 0.6816(3) 0.0232(8) Uani 1 1 d . . . N2 N 1.1227(4) 0.4447(2) 0.7307(3) 0.0245(8) Uani 1 1 d . . . C5 C 0.9080(6) 0.3958(3) 0.5250(3) 0.0372(13) Uani 1 1 d . . . H5A H 0.8838 0.3469 0.5355 0.056 Uiso 1 1 calc R . . H5B H 0.9391 0.3986 0.4696 0.056 Uiso 1 1 calc R . . H5C H 0.8290 0.4263 0.5220 0.056 Uiso 1 1 calc R . . C6 C 1.0178(5) 0.4198(3) 0.5979(3) 0.0271(10) Uani 1 1 d . . . C7 C 1.1465(6) 0.4408(3) 0.5937(4) 0.0340(12) Uani 1 1 d . . . H7 H 1.1833 0.4443 0.5426 0.041 Uiso 1 1 calc R . . C8 C 1.2112(5) 0.4557(3) 0.6783(3) 0.0280(11) Uani 1 1 d . . . C9 C 1.3536(5) 0.4782(3) 0.7126(4) 0.0405(14) Uani 1 1 d . . . H9A H 1.3553 0.5158 0.7560 0.061 Uiso 1 1 calc R . . H9B H 1.3928 0.4957 0.6642 0.061 Uiso 1 1 calc R . . H9C H 1.4061 0.4378 0.7401 0.061 Uiso 1 1 calc R . . N3 N 0.9759(4) 0.3487(2) 0.8434(3) 0.0237(8) Uani 1 1 d . . . N4 N 1.1072(4) 0.3722(2) 0.8618(3) 0.0239(8) Uani 1 1 d . . . C10 C 0.8510(5) 0.2436(3) 0.8843(4) 0.0348(12) Uani 1 1 d . . . H10A H 0.7751 0.2754 0.8856 0.052 Uiso 1 1 calc R . . H10B H 0.8658 0.2130 0.9360 0.052 Uiso 1 1 calc R . . H10C H 0.8309 0.2146 0.8312 0.052 Uiso 1 1 calc R . . C11 C 0.9741(5) 0.2860(3) 0.8842(3) 0.0253(10) Uani 1 1 d . . . C12 C 1.1040(5) 0.2700(3) 0.9284(3) 0.0275(10) Uani 1 1 d . . . H12 H 1.1314 0.2293 0.9631 0.033 Uiso 1 1 calc R . . C13 C 1.1848(5) 0.3243(3) 0.9122(3) 0.0246(10) Uani 1 1 d . . . C14 C 1.3345(5) 0.3318(3) 0.9402(4) 0.0363(13) Uani 1 1 d . . . H14A H 1.3761 0.3271 0.8891 0.054 Uiso 1 1 calc R . . H14B H 1.3692 0.2948 0.9828 0.054 Uiso 1 1 calc R . . H14C H 1.3560 0.3783 0.9670 0.054 Uiso 1 1 calc R . . N5 N 0.9094(4) 0.4937(2) 0.8286(2) 0.0215(8) Uani 1 1 d . . . N6 N 1.0462(4) 0.5001(2) 0.8576(2) 0.0233(8) Uani 1 1 d . . . C15 C 0.7031(5) 0.5592(3) 0.8478(4) 0.0329(12) Uani 1 1 d . . . H15A H 0.6689 0.5649 0.7848 0.049 Uiso 1 1 calc R . . H15B H 0.6847 0.6022 0.8784 0.049 Uiso 1 1 calc R . . H15C H 0.6583 0.5189 0.8692 0.049 Uiso 1 1 calc R . . C16 C 0.8513(5) 0.5464(3) 0.8647(3) 0.0256(10) Uani 1 1 d . . . C17 C 0.9509(6) 0.5870(3) 0.9165(3) 0.0319(12) Uani 1 1 d . . . H17 H 0.9376 0.6276 0.9494 0.038 Uiso 1 1 calc R . . C18 C 1.0720(6) 0.5571(3) 0.9109(3) 0.0285(11) Uani 1 1 d . . . C19 C 1.2114(6) 0.5805(3) 0.9516(4) 0.0399(14) Uani 1 1 d . . . H19A H 1.2588 0.5420 0.9871 0.060 Uiso 1 1 calc R . . H19B H 1.2069 0.6217 0.9889 0.060 Uiso 1 1 calc R . . H19C H 1.2600 0.5930 0.9055 0.060 Uiso 1 1 calc R . . C21 C -0.0258(7) 0.6447(4) 0.6964(4) 0.0567(19) Uani 1 1 d . . . H21A H -0.0576 0.6658 0.6385 0.085 Uiso 1 1 calc R . . H21B H -0.0950 0.6502 0.7315 0.085 Uiso 1 1 calc R . . H21C H -0.0077 0.5943 0.6898 0.085 Uiso 1 1 calc R . . C22 C 0.1011(7) 0.6809(4) 0.7413(4) 0.0447(15) Uani 1 1 d . . . C23 C 0.2236(7) 0.6620(4) 0.7243(4) 0.0460(15) Uani 1 1 d . . . H23 H 0.2286 0.6254 0.6834 0.055 Uiso 1 1 calc R . . C24 C 0.3418(8) 0.6962(5) 0.7664(5) 0.063(2) Uani 1 1 d . . . H24 H 0.4264 0.6831 0.7540 0.075 Uiso 1 1 calc R . . C25 C 0.3342(10) 0.7483(5) 0.8253(6) 0.078(3) Uani 1 1 d . . . H25 H 0.4135 0.7719 0.8541 0.094 Uiso 1 1 calc R . . C26 C 0.2111(11) 0.7667(4) 0.8432(6) 0.078(3) Uani 1 1 d . . . H26 H 0.2060 0.8026 0.8848 0.094 Uiso 1 1 calc R . . C27 C 0.0971(8) 0.7336(4) 0.8014(5) 0.0586(19) Uani 1 1 d . . . H27 H 0.0129 0.7472 0.8140 0.070 Uiso 1 1 calc 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 Ni1 0.0222(4) 0.0161(4) 0.0169(4) 0.0000(3) -0.0008(3) 0.0021(3) S1 0.0299(6) 0.0163(5) 0.0227(5) 0.0017(4) -0.0036(4) -0.0002(4) S2 0.0314(6) 0.0179(6) 0.0221(5) -0.0015(4) -0.0060(5) 0.0014(4) C1 0.023(2) 0.021(2) 0.018(2) -0.0021(17) 0.0047(16) 0.0011(17) C2 0.026(2) 0.018(2) 0.018(2) 0.0022(17) 0.0006(17) 0.0020(18) W1 0.02183(9) 0.01591(9) 0.01562(9) 0.00122(7) 0.00054(6) 0.00114(7) C3 0.029(2) 0.024(2) 0.025(2) 0.005(2) -0.0024(19) 0.004(2) C4 0.027(2) 0.025(2) 0.022(2) -0.0009(19) -0.0009(19) 0.0011(19) O3 0.055(3) 0.022(2) 0.041(2) -0.0070(17) -0.0039(19) 0.0023(18) O4 0.030(2) 0.055(3) 0.037(2) 0.012(2) 0.0111(17) -0.0037(19) B1 0.021(2) 0.029(3) 0.021(2) 0.004(2) 0.0013(19) 0.001(2) N1 0.028(2) 0.023(2) 0.0191(18) 0.0031(15) 0.0059(15) 0.0014(16) N2 0.025(2) 0.026(2) 0.0233(19) 0.0050(16) 0.0052(16) -0.0006(16) C5 0.050(3) 0.043(3) 0.020(2) -0.003(2) 0.009(2) 0.004(3) C6 0.034(3) 0.025(3) 0.023(2) 0.0037(19) 0.0072(19) 0.008(2) C7 0.041(3) 0.034(3) 0.033(3) 0.008(2) 0.020(2) 0.008(2) C8 0.033(3) 0.021(2) 0.033(3) 0.008(2) 0.013(2) 0.006(2) C9 0.030(3) 0.049(4) 0.046(3) 0.008(3) 0.015(3) 0.000(3) N3 0.026(2) 0.022(2) 0.0201(19) 0.0028(15) -0.0002(15) -0.0012(16) N4 0.024(2) 0.026(2) 0.0210(19) 0.0056(16) 0.0038(15) 0.0019(16) C10 0.037(3) 0.024(3) 0.041(3) 0.012(2) 0.001(2) -0.006(2) C11 0.032(3) 0.021(2) 0.022(2) 0.0069(18) 0.0031(19) 0.0033(19) C12 0.034(3) 0.025(3) 0.021(2) 0.0087(19) 0.0012(19) 0.004(2) C13 0.027(2) 0.028(3) 0.018(2) 0.0064(18) 0.0036(18) 0.0047(19) C14 0.028(3) 0.044(3) 0.035(3) 0.013(2) 0.001(2) 0.006(2) N5 0.0215(19) 0.024(2) 0.0179(18) 0.0003(15) 0.0025(14) -0.0005(15) N6 0.029(2) 0.021(2) 0.0179(18) -0.0007(15) -0.0005(15) -0.0071(16) C15 0.041(3) 0.029(3) 0.030(3) -0.006(2) 0.011(2) 0.009(2) C16 0.036(3) 0.022(2) 0.020(2) 0.0002(18) 0.0068(19) 0.002(2) C17 0.050(3) 0.023(3) 0.021(2) -0.0046(19) 0.005(2) -0.002(2) C18 0.043(3) 0.024(3) 0.017(2) -0.0007(18) 0.002(2) -0.008(2) C19 0.047(3) 0.037(3) 0.031(3) -0.002(2) -0.004(2) -0.014(3) C21 0.045(4) 0.081(6) 0.042(4) 0.015(4) 0.004(3) -0.002(4) C22 0.049(4) 0.045(4) 0.041(3) 0.019(3) 0.010(3) 0.007(3) C23 0.049(4) 0.047(4) 0.043(3) 0.013(3) 0.012(3) 0.007(3) C24 0.054(4) 0.072(6) 0.065(5) 0.023(4) 0.018(4) -0.013(4) C25 0.083(6) 0.066(6) 0.082(6) 0.000(5) 0.008(5) -0.037(5) C26 0.104(7) 0.045(5) 0.094(7) -0.006(4) 0.039(6) -0.010(5) C27 0.068(5) 0.040(4) 0.073(5) 0.011(4) 0.026(4) 0.006(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 Ni1 S1 2.2112(12) 3_666 ? Ni1 S1 2.2112(12) . ? Ni1 S2 2.2145(12) . ? Ni1 S2 2.2145(12) 3_666 ? S1 C1 1.682(5) . ? S2 C2 1.680(5) . ? C1 C2 1.373(6) . ? C1 W1 2.024(5) . ? C2 W1 2.043(4) . ? W1 C3 2.006(5) . ? W1 C4 2.016(5) . ? W1 N1 2.193(4) . ? W1 N5 2.205(4) . ? W1 N3 2.216(4) . ? C3 O3 1.148(6) . ? C4 O4 1.140(6) . ? B1 N6 1.525(7) . ? B1 N2 1.536(7) . ? B1 N4 1.545(7) . ? N1 C6 1.350(6) . ? N1 N2 1.370(6) . ? N2 C8 1.348(6) . ? C5 C6 1.491(8) . ? C6 C7 1.378(7) . ? C7 C8 1.379(8) . ? C8 C9 1.497(8) . ? N3 C11 1.348(6) . ? N3 N4 1.377(5) . ? N4 C13 1.344(6) . ? C10 C11 1.484(7) . ? C11 C12 1.390(7) . ? C12 C13 1.370(7) . ? C13 C14 1.498(7) . ? N5 C16 1.340(6) . ? N5 N6 1.374(5) . ? N6 C18 1.355(6) . ? C15 C16 1.492(7) . ? C16 C17 1.388(7) . ? C17 C18 1.371(8) . ? C18 C19 1.494(8) . ? C21 C22 1.501(10) . ? C22 C23 1.371(9) . ? C22 C27 1.375(10) . ? C23 C24 1.402(10) . ? C24 C25 1.361(12) . ? C25 C26 1.377(13) . ? C26 C27 1.358(12) . ? 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 S1 Ni1 S1 180.0 3_666 . ? S1 Ni1 S2 87.16(4) 3_666 . ? S1 Ni1 S2 92.84(4) . . ? S1 Ni1 S2 92.84(4) 3_666 3_666 ? S1 Ni1 S2 87.16(4) . 3_666 ? S2 Ni1 S2 180.00(6) . 3_666 ? C1 S1 Ni1 101.51(16) . . ? C2 S2 Ni1 99.49(16) . . ? C2 C1 S1 120.7(3) . . ? C2 C1 W1 71.0(3) . . ? S1 C1 W1 167.6(3) . . ? C1 C2 S2 125.3(4) . . ? C1 C2 W1 69.5(3) . . ? S2 C2 W1 165.2(3) . . ? C3 W1 C4 88.4(2) . . ? C3 W1 C1 108.62(18) . . ? C4 W1 C1 94.07(19) . . ? C3 W1 C2 70.08(18) . . ? C4 W1 C2 84.81(19) . . ? C1 W1 C2 39.47(18) . . ? C3 W1 N1 92.92(18) . . ? C4 W1 N1 173.73(17) . . ? C1 W1 N1 91.32(16) . . ? C2 W1 N1 101.42(17) . . ? C3 W1 N5 163.85(17) . . ? C4 W1 N5 92.05(17) . . ? C1 W1 N5 87.46(17) . . ? C2 W1 N5 126.04(16) . . ? N1 W1 N5 84.96(15) . . ? C3 W1 N3 84.42(17) . . ? C4 W1 N3 90.17(17) . . ? C1 W1 N3 166.37(17) . . ? C2 W1 N3 154.10(16) . . ? N1 W1 N3 83.86(15) . . ? N5 W1 N3 79.44(14) . . ? O3 C3 W1 177.5(4) . . ? O4 C4 W1 177.8(5) . . ? N6 B1 N2 109.5(4) . . ? N6 B1 N4 108.9(4) . . ? N2 B1 N4 108.1(4) . . ? C6 N1 N2 106.6(4) . . ? C6 N1 W1 132.6(3) . . ? N2 N1 W1 120.7(3) . . ? C8 N2 N1 109.7(4) . . ? C8 N2 B1 130.7(4) . . ? N1 N2 B1 119.3(4) . . ? N1 C6 C7 109.5(5) . . ? N1 C6 C5 122.3(5) . . ? C7 C6 C5 128.2(5) . . ? C6 C7 C8 106.5(5) . . ? N2 C8 C7 107.7(5) . . ? N2 C8 C9 122.7(5) . . ? C7 C8 C9 129.6(5) . . ? C11 N3 N4 106.9(4) . . ? C11 N3 W1 133.4(3) . . ? N4 N3 W1 118.6(3) . . ? C13 N4 N3 109.3(4) . . ? C13 N4 B1 130.5(4) . . ? N3 N4 B1 120.0(4) . . ? N3 C11 C12 108.9(4) . . ? N3 C11 C10 124.6(4) . . ? C12 C11 C10 126.4(4) . . ? C13 C12 C11 106.6(4) . . ? N4 C13 C12 108.2(4) . . ? N4 C13 C14 123.0(4) . . ? C12 C13 C14 128.7(4) . . ? C16 N5 N6 107.2(4) . . ? C16 N5 W1 133.0(3) . . ? N6 N5 W1 119.7(3) . . ? C18 N6 N5 109.2(4) . . ? C18 N6 B1 130.3(4) . . ? N5 N6 B1 120.5(4) . . ? N5 C16 C17 109.0(5) . . ? N5 C16 C15 124.0(4) . . ? C17 C16 C15 126.9(5) . . ? C18 C17 C16 106.9(5) . . ? N6 C18 C17 107.7(4) . . ? N6 C18 C19 123.0(5) . . ? C17 C18 C19 129.3(5) . . ? C23 C22 C27 118.4(7) . . ? C23 C22 C21 121.0(7) . . ? C27 C22 C21 120.6(7) . . ? C22 C23 C24 120.7(7) . . ? C25 C24 C23 119.4(8) . . ? C24 C25 C26 119.9(8) . . ? C27 C26 C25 120.3(9) . . ? C26 C27 C22 121.4(8) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.644 _refine_diff_density_min -1.295 _refine_diff_density_rms 0.165 #===END data_Pd_complex_3 _database_code_depnum_ccdc_archive 'CCDC 610642' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H60 B2 N12 O4 Pd S4 W2' _chemical_formula_weight 1541.08 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(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 10.1900(17) _cell_length_b 18.993(3) _cell_length_c 15.757(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.582(3) _cell_angle_gamma 90.00 _cell_volume 2987.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 4.332 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7232 _exptl_absorpt_correction_T_max 0.8125 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.815452 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28696 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6859 _reflns_number_gt 5325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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^)+(0.0310P)^2^+0.0000P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6859 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0669 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.5000 0.5000 0.02163(11) Uani 1 2 d S . . S1 S 0.66414(12) 0.54915(6) 0.60906(7) 0.0268(3) Uani 1 1 d . . . S2 S 0.55023(13) 0.38717(6) 0.55729(8) 0.0285(3) Uani 1 1 d . . . C1 C 0.7227(5) 0.4752(2) 0.6645(3) 0.0233(10) Uani 1 1 d . . . C2 C 0.6774(4) 0.4093(2) 0.6405(3) 0.0227(9) Uani 1 1 d . . . W1 W 0.832968(18) 0.404191(9) 0.744681(11) 0.02096(6) Uani 1 1 d . . . C3 C 0.7972(5) 0.3075(3) 0.6912(3) 0.0286(11) Uani 1 1 d . . . C4 C 0.6874(5) 0.3847(3) 0.8122(3) 0.0282(11) Uani 1 1 d . . . O3 O 0.7729(4) 0.25377(18) 0.6588(2) 0.0434(10) Uani 1 1 d . . . O4 O 0.6015(4) 0.3726(2) 0.8476(2) 0.0440(10) Uani 1 1 d . . . B1 B 1.1470(5) 0.4465(3) 0.8322(3) 0.0269(12) Uani 1 1 d . . . H1 H 1.2417 0.4591 0.8586 0.032 Uiso 1 1 calc R . . N1 N 1.0072(4) 0.4226(2) 0.6842(2) 0.0256(9) Uani 1 1 d . . . N2 N 1.1273(4) 0.4448(2) 0.7325(2) 0.0267(9) Uani 1 1 d . . . C5 C 0.9134(6) 0.3964(3) 0.5279(3) 0.0421(14) Uani 1 1 d . . . H5A H 0.8870 0.3483 0.5394 0.063 Uiso 1 1 calc R . . H5B H 0.9461 0.3974 0.4735 0.063 Uiso 1 1 calc R . . H5C H 0.8359 0.4278 0.5233 0.063 Uiso 1 1 calc R . . C6 C 1.0222(5) 0.4205(3) 0.6005(3) 0.0302(11) Uani 1 1 d . . . C7 C 1.1515(5) 0.4418(3) 0.5964(3) 0.0348(12) Uani 1 1 d . . . H7 H 1.1885 0.4456 0.5458 0.042 Uiso 1 1 calc R . . C8 C 1.2156(5) 0.4563(2) 0.6808(3) 0.0296(11) Uani 1 1 d . . . C9 C 1.3574(5) 0.4796(3) 0.7146(4) 0.0432(14) Uani 1 1 d . . . H9A H 1.3580 0.5180 0.7562 0.065 Uiso 1 1 calc R . . H9B H 1.3969 0.4960 0.6664 0.065 Uiso 1 1 calc R . . H9C H 1.4097 0.4399 0.7434 0.065 Uiso 1 1 calc R . . N3 N 0.9811(4) 0.34856(19) 0.8451(2) 0.0244(8) Uani 1 1 d . . . N4 N 1.1124(4) 0.3728(2) 0.8636(2) 0.0256(8) Uani 1 1 d . . . C10 C 0.8590(5) 0.2424(3) 0.8855(4) 0.0388(13) Uani 1 1 d . . . H10A H 0.7813 0.2734 0.8829 0.058 Uiso 1 1 calc R . . H10B H 0.8711 0.2136 0.9381 0.058 Uiso 1 1 calc R . . H10C H 0.8442 0.2116 0.8346 0.058 Uiso 1 1 calc R . . C11 C 0.9815(5) 0.2860(2) 0.8869(3) 0.0277(10) Uani 1 1 d . . . C12 C 1.1104(5) 0.2704(3) 0.9300(3) 0.0297(11) Uani 1 1 d . . . H12 H 1.1385 0.2297 0.9640 0.036 Uiso 1 1 calc R . . C13 C 1.1899(5) 0.3254(3) 0.9140(3) 0.0268(10) Uani 1 1 d . . . C14 C 1.3395(5) 0.3333(3) 0.9417(3) 0.0416(13) Uani 1 1 d . . . H14A H 1.3825 0.3192 0.8940 0.062 Uiso 1 1 calc R . . H14B H 1.3719 0.3032 0.9921 0.062 Uiso 1 1 calc R . . H14C H 1.3615 0.3825 0.9570 0.062 Uiso 1 1 calc R . . N5 N 0.9131(4) 0.4933(2) 0.8299(2) 0.0263(9) Uani 1 1 d . . . N6 N 1.0496(4) 0.5010(2) 0.8586(2) 0.0261(9) Uani 1 1 d . . . C15 C 0.7061(5) 0.5580(3) 0.8493(3) 0.0360(12) Uani 1 1 d . . . H15A H 0.6687 0.5522 0.7873 0.054 Uiso 1 1 calc R . . H15B H 0.6871 0.6056 0.8674 0.054 Uiso 1 1 calc R . . H15C H 0.6653 0.5234 0.8823 0.054 Uiso 1 1 calc R . . C16 C 0.8531(5) 0.5468(2) 0.8656(3) 0.0281(11) Uani 1 1 d . . . C17 C 0.9531(5) 0.5869(3) 0.9168(3) 0.0345(12) Uani 1 1 d . . . H17 H 0.9399 0.6270 0.9500 0.041 Uiso 1 1 calc R . . C18 C 1.0743(5) 0.5580(3) 0.9106(3) 0.0316(11) Uani 1 1 d . . . C19 C 1.2134(6) 0.5818(3) 0.9508(4) 0.0451(15) Uani 1 1 d . . . H19A H 1.2638 0.5422 0.9812 0.068 Uiso 1 1 calc R . . H19B H 1.2087 0.6199 0.9919 0.068 Uiso 1 1 calc R . . H19C H 1.2586 0.5987 0.9053 0.068 Uiso 1 1 calc R . . C21 C -0.0247(6) 0.6460(4) 0.6968(4) 0.0602(18) Uani 1 1 d . . . H21A H -0.0541 0.6657 0.6386 0.090 Uiso 1 1 calc R . . H21B H -0.0940 0.6540 0.7307 0.090 Uiso 1 1 calc R . . H21C H -0.0093 0.5953 0.6924 0.090 Uiso 1 1 calc R . . C22 C 0.1034(6) 0.6812(3) 0.7407(4) 0.0464(14) Uani 1 1 d . . . C23 C 0.2244(6) 0.6617(3) 0.7232(4) 0.0516(16) Uani 1 1 d . . . H23 H 0.2287 0.6256 0.6821 0.062 Uiso 1 1 calc R . . C24 C 0.3437(7) 0.6953(4) 0.7663(5) 0.0642(19) Uani 1 1 d . . . H24 H 0.4278 0.6812 0.7547 0.077 Uiso 1 1 calc R . . C25 C 0.3377(9) 0.7478(4) 0.8243(6) 0.081(3) Uani 1 1 d . . . H25 H 0.4173 0.7710 0.8521 0.097 Uiso 1 1 calc R . . C26 C 0.2156(10) 0.7672(4) 0.8429(5) 0.080(2) Uani 1 1 d . . . H26 H 0.2119 0.8034 0.8840 0.096 Uiso 1 1 calc R . . C27 C 0.1007(8) 0.7347(3) 0.8026(5) 0.0632(19) Uani 1 1 d . . . H27 H 0.0177 0.7482 0.8163 0.076 Uiso 1 1 calc 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 Pd1 0.0256(3) 0.0191(2) 0.0187(2) 0.00043(19) 0.00093(19) 0.0024(2) S1 0.0338(7) 0.0177(6) 0.0254(6) 0.0028(5) -0.0022(5) 0.0005(5) S2 0.0342(7) 0.0210(6) 0.0256(6) -0.0014(5) -0.0049(5) 0.0006(5) C1 0.028(2) 0.022(2) 0.020(2) 0.0030(18) 0.0047(19) 0.0022(19) C2 0.027(2) 0.023(2) 0.016(2) 0.0019(18) 0.0007(17) 0.003(2) W1 0.02486(10) 0.01852(9) 0.01846(9) 0.00117(8) 0.00185(6) 0.00115(8) C3 0.032(3) 0.025(3) 0.026(2) 0.005(2) -0.002(2) 0.004(2) C4 0.030(3) 0.027(3) 0.024(2) 0.0017(19) -0.003(2) 0.000(2) O3 0.058(3) 0.024(2) 0.042(2) -0.0047(17) -0.0034(19) 0.0011(18) O4 0.032(2) 0.065(3) 0.036(2) 0.0107(19) 0.0110(17) -0.0016(19) B1 0.020(3) 0.034(3) 0.025(3) 0.002(2) 0.000(2) -0.007(2) N1 0.027(2) 0.027(2) 0.0226(19) 0.0054(16) 0.0046(16) 0.0050(16) N2 0.028(2) 0.026(2) 0.027(2) 0.0043(17) 0.0078(16) 0.0002(17) C5 0.054(3) 0.051(4) 0.024(3) -0.005(2) 0.016(2) 0.005(3) C6 0.038(3) 0.028(3) 0.026(2) 0.0031(19) 0.010(2) 0.008(2) C7 0.043(3) 0.036(3) 0.030(3) 0.006(2) 0.019(2) 0.009(2) C8 0.034(3) 0.022(2) 0.036(3) 0.007(2) 0.015(2) 0.004(2) C9 0.033(3) 0.052(4) 0.049(3) 0.015(3) 0.018(3) 0.007(3) N3 0.029(2) 0.021(2) 0.0212(19) 0.0020(16) 0.0014(16) -0.0029(17) N4 0.028(2) 0.026(2) 0.023(2) 0.0031(16) 0.0042(16) -0.0036(17) C10 0.037(3) 0.031(3) 0.044(3) 0.010(2) 0.000(2) -0.006(2) C11 0.040(3) 0.024(2) 0.019(2) 0.0018(19) 0.008(2) -0.001(2) C12 0.037(3) 0.029(3) 0.024(2) 0.009(2) 0.007(2) 0.005(2) C13 0.026(2) 0.031(3) 0.023(2) 0.0021(19) 0.0035(19) 0.005(2) C14 0.035(3) 0.046(3) 0.042(3) 0.013(3) 0.004(2) 0.002(3) N5 0.029(2) 0.024(2) 0.027(2) 0.0012(17) 0.0071(17) 0.0003(17) N6 0.030(2) 0.026(2) 0.0209(19) 0.0019(16) 0.0009(16) -0.0043(17) C15 0.043(3) 0.032(3) 0.033(3) -0.002(2) 0.008(2) 0.009(2) C16 0.042(3) 0.024(2) 0.019(2) -0.0008(19) 0.008(2) -0.002(2) C17 0.050(3) 0.024(3) 0.030(3) -0.001(2) 0.009(2) -0.002(2) C18 0.046(3) 0.025(3) 0.024(2) -0.001(2) 0.007(2) -0.011(2) C19 0.054(4) 0.039(3) 0.036(3) -0.002(2) -0.005(3) -0.019(3) C21 0.051(4) 0.077(5) 0.050(4) 0.016(3) 0.003(3) 0.000(4) C22 0.051(4) 0.047(4) 0.043(3) 0.018(3) 0.013(3) 0.004(3) C23 0.057(4) 0.055(4) 0.045(3) 0.015(3) 0.015(3) 0.010(3) C24 0.051(4) 0.072(5) 0.071(5) 0.024(4) 0.014(3) -0.005(4) C25 0.088(6) 0.060(5) 0.096(6) -0.001(4) 0.018(5) -0.043(5) C26 0.114(7) 0.046(4) 0.087(6) -0.005(4) 0.036(5) -0.018(5) C27 0.076(5) 0.041(4) 0.079(5) 0.005(4) 0.033(4) 0.007(4) _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 Pd1 S1 2.3384(12) . ? Pd1 S1 2.3384(12) 3_666 ? Pd1 S2 2.3416(12) 3_666 ? Pd1 S2 2.3416(12) . ? S1 C1 1.698(4) . ? S2 C2 1.701(4) . ? C1 C2 1.360(6) . ? C1 W1 2.026(4) . ? C2 W1 2.042(4) . ? W1 C3 2.022(5) . ? W1 C4 2.025(5) . ? W1 N1 2.205(4) . ? W1 N5 2.212(4) . ? W1 N3 2.222(4) . ? C3 O3 1.147(6) . ? C4 O4 1.152(6) . ? B1 N2 1.543(6) . ? B1 N6 1.548(7) . ? B1 N4 1.549(7) . ? N1 C6 1.360(6) . ? N1 N2 1.371(5) . ? N2 C8 1.348(6) . ? C5 C6 1.496(7) . ? C6 C7 1.392(7) . ? C7 C8 1.387(7) . ? C8 C9 1.502(7) . ? N3 C11 1.359(6) . ? N3 N4 1.389(5) . ? N4 C13 1.346(6) . ? C10 C11 1.494(7) . ? C11 C12 1.385(7) . ? C12 C13 1.376(6) . ? C13 C14 1.507(7) . ? N5 C16 1.364(6) . ? N5 N6 1.381(5) . ? N6 C18 1.350(6) . ? C15 C16 1.483(7) . ? C16 C17 1.393(7) . ? C17 C18 1.373(7) . ? C18 C19 1.502(7) . ? C21 C22 1.506(8) . ? C22 C23 1.368(8) . ? C22 C27 1.412(9) . ? C23 C24 1.419(9) . ? C24 C25 1.361(10) . ? C25 C26 1.384(11) . ? C26 C27 1.362(10) . ? 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 S1 Pd1 S1 180.0 . 3_666 ? S1 Pd1 S2 89.24(4) . 3_666 ? S1 Pd1 S2 90.76(4) 3_666 3_666 ? S1 Pd1 S2 90.76(4) . . ? S1 Pd1 S2 89.24(4) 3_666 . ? S2 Pd1 S2 180.00(5) 3_666 . ? C1 S1 Pd1 99.98(16) . . ? C2 S2 Pd1 98.31(16) . . ? C2 C1 S1 123.6(3) . . ? C2 C1 W1 71.1(3) . . ? S1 C1 W1 164.7(3) . . ? C1 C2 S2 127.2(3) . . ? C1 C2 W1 69.8(3) . . ? S2 C2 W1 162.9(3) . . ? C3 W1 C4 87.9(2) . . ? C3 W1 C1 108.24(18) . . ? C4 W1 C1 94.35(18) . . ? C3 W1 C2 70.28(18) . . ? C4 W1 C2 84.19(18) . . ? C1 W1 C2 39.05(17) . . ? C3 W1 N1 93.29(17) . . ? C4 W1 N1 173.77(16) . . ? C1 W1 N1 91.08(16) . . ? C2 W1 N1 101.97(16) . . ? C3 W1 N5 163.97(16) . . ? C4 W1 N5 92.38(17) . . ? C1 W1 N5 87.72(17) . . ? C2 W1 N5 125.70(16) . . ? N1 W1 N5 84.79(14) . . ? C3 W1 N3 84.55(15) . . ? C4 W1 N3 90.22(16) . . ? C1 W1 N3 166.54(16) . . ? C2 W1 N3 154.35(16) . . ? N1 W1 N3 83.81(14) . . ? N5 W1 N3 79.43(14) . . ? O3 C3 W1 177.5(4) . . ? O4 C4 W1 177.3(4) . . ? N2 B1 N6 109.2(4) . . ? N2 B1 N4 108.3(4) . . ? N6 B1 N4 108.6(4) . . ? C6 N1 N2 106.6(4) . . ? C6 N1 W1 132.2(3) . . ? N2 N1 W1 121.0(3) . . ? C8 N2 N1 110.1(4) . . ? C8 N2 B1 130.2(4) . . ? N1 N2 B1 119.4(4) . . ? N1 C6 C7 109.2(4) . . ? N1 C6 C5 122.7(5) . . ? C7 C6 C5 128.1(5) . . ? C8 C7 C6 106.3(4) . . ? N2 C8 C7 107.7(4) . . ? N2 C8 C9 123.0(5) . . ? C7 C8 C9 129.3(5) . . ? C11 N3 N4 106.2(4) . . ? C11 N3 W1 134.2(3) . . ? N4 N3 W1 118.7(3) . . ? C13 N4 N3 109.2(4) . . ? C13 N4 B1 130.4(4) . . ? N3 N4 B1 120.3(4) . . ? N3 C11 C12 109.6(4) . . ? N3 C11 C10 123.8(4) . . ? C12 C11 C10 126.6(4) . . ? C13 C12 C11 106.4(4) . . ? N4 C13 C12 108.6(4) . . ? N4 C13 C14 122.9(4) . . ? C12 C13 C14 128.4(4) . . ? C16 N5 N6 107.0(4) . . ? C16 N5 W1 132.7(3) . . ? N6 N5 W1 120.3(3) . . ? C18 N6 N5 109.6(4) . . ? C18 N6 B1 130.4(4) . . ? N5 N6 B1 120.0(4) . . ? N5 C16 C17 108.0(4) . . ? N5 C16 C15 123.8(4) . . ? C17 C16 C15 128.2(5) . . ? C18 C17 C16 107.7(4) . . ? N6 C18 C17 107.6(4) . . ? N6 C18 C19 122.8(5) . . ? C17 C18 C19 129.5(5) . . ? C23 C22 C27 118.5(6) . . ? C23 C22 C21 121.4(6) . . ? C27 C22 C21 120.2(6) . . ? C22 C23 C24 120.1(7) . . ? C25 C24 C23 120.0(7) . . ? C24 C25 C26 120.0(7) . . ? C27 C26 C25 120.4(8) . . ? C26 C27 C22 120.9(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.923 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.140 #===END data_Pt_complex_4 _database_code_depnum_ccdc_archive 'CCDC 610643' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H60 B2 N12 O4 Pt S4 W2' _chemical_formula_weight 1629.77 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(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 10.1525(13) _cell_length_b 18.891(3) _cell_length_c 15.748(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.498(3) _cell_angle_gamma 90.00 _cell_volume 2959.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description plates _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 6.429 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5953 _exptl_absorpt_correction_T_max 0.8305 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.744265 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28647 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6793 _reflns_number_gt 5686 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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^)+(0.0378P)^2^+9.6984P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6793 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.5000 0.5000 0.5000 0.02496(8) Uani 1 2 d S . . S1 S 0.66359(15) 0.54825(7) 0.60841(9) 0.0298(3) Uani 1 1 d . . . S2 S 0.55240(16) 0.38822(8) 0.55756(10) 0.0310(3) Uani 1 1 d . . . C1 C 0.7251(6) 0.4752(3) 0.6654(4) 0.0254(11) Uani 1 1 d . . . C2 C 0.6802(6) 0.4092(3) 0.6410(4) 0.0289(12) Uani 1 1 d . . . W1 W 0.83436(2) 0.403968(11) 0.745264(14) 0.02503(7) Uani 1 1 d . . . C3 C 0.8014(6) 0.3073(3) 0.6923(4) 0.0330(13) Uani 1 1 d . . . C4 C 0.6880(6) 0.3848(3) 0.8126(4) 0.0329(13) Uani 1 1 d . . . O3 O 0.7763(5) 0.2533(2) 0.6598(3) 0.0483(12) Uani 1 1 d . . . O4 O 0.6032(5) 0.3721(3) 0.8477(3) 0.0473(12) Uani 1 1 d . . . B1 B 1.1486(7) 0.4467(4) 0.8327(5) 0.0339(15) Uani 1 1 d . . . H1 H 1.2435 0.4594 0.8592 0.041 Uiso 1 1 calc R . . N1 N 1.0093(5) 0.4224(3) 0.6854(3) 0.0309(11) Uani 1 1 d . . . N2 N 1.1290(5) 0.4449(3) 0.7340(3) 0.0296(10) Uani 1 1 d . . . C5 C 0.9159(7) 0.3972(4) 0.5293(4) 0.0430(16) Uani 1 1 d . . . H5A H 0.8843 0.3502 0.5426 0.064 Uiso 1 1 calc R . . H5B H 0.9509 0.3949 0.4757 0.064 Uiso 1 1 calc R . . H5C H 0.8411 0.4308 0.5220 0.064 Uiso 1 1 calc R . . C6 C 1.0258(7) 0.4212(3) 0.6027(4) 0.0335(13) Uani 1 1 d . . . C7 C 1.1536(7) 0.4421(3) 0.5985(4) 0.0389(15) Uani 1 1 d . . . H7 H 1.1907 0.4457 0.5478 0.047 Uiso 1 1 calc R . . C8 C 1.2179(6) 0.4570(3) 0.6822(4) 0.0358(14) Uani 1 1 d . . . C9 C 1.3595(7) 0.4795(4) 0.7165(5) 0.0471(17) Uani 1 1 d . . . H9A H 1.3602 0.5196 0.7559 0.071 Uiso 1 1 calc R . . H9B H 1.4016 0.4935 0.6682 0.071 Uiso 1 1 calc R . . H9C H 1.4098 0.4400 0.7478 0.071 Uiso 1 1 calc R . . N3 N 0.9826(5) 0.3482(3) 0.8453(3) 0.0298(11) Uani 1 1 d . . . N4 N 1.1130(5) 0.3721(3) 0.8641(3) 0.0294(11) Uani 1 1 d . . . C10 C 0.8597(7) 0.2419(3) 0.8849(5) 0.0442(17) Uani 1 1 d . . . H10A H 0.7824 0.2728 0.8857 0.066 Uiso 1 1 calc R . . H10B H 0.8736 0.2107 0.9356 0.066 Uiso 1 1 calc R . . H10C H 0.8425 0.2132 0.8319 0.066 Uiso 1 1 calc R . . C11 C 0.9820(6) 0.2859(3) 0.8870(4) 0.0319(13) Uani 1 1 d . . . C12 C 1.1110(6) 0.2703(3) 0.9302(4) 0.0339(14) Uani 1 1 d . . . H12 H 1.1385 0.2294 0.9643 0.041 Uiso 1 1 calc R . . C13 C 1.1916(6) 0.3249(3) 0.9145(4) 0.0326(13) Uani 1 1 d . . . C14 C 1.3405(7) 0.3331(4) 0.9427(5) 0.0458(17) Uani 1 1 d . . . H14A H 1.3831 0.3284 0.8923 0.069 Uiso 1 1 calc R . . H14B H 1.3752 0.2965 0.9853 0.069 Uiso 1 1 calc R . . H14C H 1.3607 0.3800 0.9688 0.069 Uiso 1 1 calc R . . N5 N 0.9135(5) 0.4929(2) 0.8304(3) 0.0284(10) Uani 1 1 d . . . N6 N 1.0503(5) 0.5006(2) 0.8594(3) 0.0294(11) Uani 1 1 d . . . C15 C 0.7071(7) 0.5578(3) 0.8499(4) 0.0388(15) Uani 1 1 d . . . H15A H 0.6695 0.5525 0.7879 0.058 Uiso 1 1 calc R . . H15B H 0.6883 0.6055 0.8687 0.058 Uiso 1 1 calc R . . H15C H 0.6659 0.5228 0.8826 0.058 Uiso 1 1 calc R . . C16 C 0.8536(6) 0.5463(3) 0.8658(4) 0.0317(13) Uani 1 1 d . . . C17 C 0.9538(7) 0.5876(3) 0.9166(4) 0.0387(15) Uani 1 1 d . . . H17 H 0.9402 0.6285 0.9489 0.046 Uiso 1 1 calc R . . C18 C 1.0743(7) 0.5582(3) 0.9111(4) 0.0379(15) Uani 1 1 d . . . C19 C 1.2129(8) 0.5825(4) 0.9504(5) 0.0482(18) Uani 1 1 d . . . H19A H 1.2618 0.5440 0.9847 0.072 Uiso 1 1 calc R . . H19B H 1.2078 0.6233 0.9880 0.072 Uiso 1 1 calc R . . H19C H 1.2601 0.5961 0.9043 0.072 Uiso 1 1 calc R . . C21 C -0.0251(9) 0.6448(5) 0.6960(5) 0.063(2) Uani 1 1 d . . . H21A H -0.0561 0.6656 0.6384 0.094 Uiso 1 1 calc R . . H21B H -0.0943 0.6512 0.7307 0.094 Uiso 1 1 calc R . . H21C H -0.0078 0.5942 0.6901 0.094 Uiso 1 1 calc R . . C22 C 0.1008(8) 0.6805(4) 0.7395(5) 0.0514(19) Uani 1 1 d . . . C23 C 0.2230(8) 0.6615(4) 0.7228(5) 0.0505(18) Uani 1 1 d . . . H23 H 0.2284 0.6247 0.6825 0.061 Uiso 1 1 calc R . . C24 C 0.3416(9) 0.6962(5) 0.7651(6) 0.068(2) Uani 1 1 d . . . H24 H 0.4261 0.6831 0.7525 0.082 Uiso 1 1 calc R . . C25 C 0.3346(11) 0.7482(5) 0.8239(7) 0.082(3) Uani 1 1 d . . . H25 H 0.4140 0.7710 0.8535 0.098 Uiso 1 1 calc R . . C26 C 0.2114(11) 0.7674(5) 0.8398(7) 0.080(3) Uani 1 1 d . . . H26 H 0.2061 0.8045 0.8797 0.096 Uiso 1 1 calc R . . C27 C 0.0952(10) 0.7339(4) 0.7991(6) 0.063(2) Uani 1 1 d . . . H27 H 0.0112 0.7475 0.8119 0.076 Uiso 1 1 calc 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 0.02938(16) 0.02159(15) 0.02339(15) -0.00103(11) 0.00406(12) 0.00119(12) S1 0.0378(8) 0.0197(6) 0.0298(7) 0.0022(6) 0.0014(6) 0.0003(6) S2 0.0378(8) 0.0238(7) 0.0277(7) -0.0019(6) -0.0025(6) 0.0006(6) C1 0.028(3) 0.024(3) 0.024(3) 0.003(2) 0.007(2) 0.006(2) C2 0.035(3) 0.027(3) 0.022(3) -0.003(2) 0.000(2) 0.001(2) W1 0.03059(13) 0.02131(12) 0.02278(12) 0.00017(8) 0.00433(9) 0.00007(9) C3 0.038(3) 0.027(3) 0.031(3) -0.003(3) 0.002(3) 0.004(3) C4 0.033(3) 0.033(3) 0.030(3) 0.001(3) 0.002(3) 0.000(3) O3 0.063(3) 0.030(3) 0.046(3) -0.005(2) -0.004(2) 0.003(2) O4 0.036(3) 0.063(3) 0.044(3) 0.009(2) 0.012(2) -0.005(2) B1 0.033(4) 0.033(4) 0.035(4) 0.002(3) 0.004(3) -0.010(3) N1 0.036(3) 0.030(3) 0.027(3) 0.004(2) 0.007(2) 0.005(2) N2 0.033(3) 0.029(3) 0.028(2) 0.006(2) 0.009(2) 0.001(2) C5 0.055(4) 0.049(4) 0.026(3) 0.000(3) 0.011(3) 0.003(3) C6 0.045(4) 0.030(3) 0.028(3) 0.005(2) 0.014(3) 0.009(3) C7 0.048(4) 0.041(4) 0.033(3) 0.009(3) 0.021(3) 0.013(3) C8 0.040(3) 0.031(3) 0.039(3) 0.008(3) 0.015(3) 0.007(3) C9 0.034(4) 0.056(4) 0.055(4) 0.013(4) 0.017(3) -0.002(3) N3 0.036(3) 0.025(2) 0.029(3) 0.000(2) 0.006(2) -0.004(2) N4 0.035(3) 0.029(3) 0.024(2) 0.005(2) 0.007(2) -0.003(2) C10 0.052(4) 0.033(3) 0.045(4) 0.015(3) 0.004(3) -0.005(3) C11 0.040(3) 0.026(3) 0.029(3) 0.005(2) 0.005(3) 0.001(2) C12 0.047(4) 0.026(3) 0.029(3) 0.007(2) 0.011(3) 0.005(3) C13 0.040(3) 0.033(3) 0.026(3) 0.003(2) 0.009(3) 0.003(3) C14 0.041(4) 0.048(4) 0.046(4) 0.017(3) 0.004(3) 0.004(3) N5 0.033(3) 0.025(2) 0.026(2) 0.0005(19) 0.005(2) -0.004(2) N6 0.035(3) 0.026(2) 0.026(2) -0.001(2) 0.005(2) -0.005(2) C15 0.048(4) 0.034(3) 0.039(4) -0.006(3) 0.019(3) 0.002(3) C16 0.047(4) 0.029(3) 0.021(3) -0.001(2) 0.010(3) -0.001(3) C17 0.058(4) 0.031(3) 0.029(3) -0.005(3) 0.012(3) -0.007(3) C18 0.055(4) 0.034(3) 0.024(3) 0.002(3) 0.005(3) -0.012(3) C19 0.060(5) 0.040(4) 0.039(4) -0.006(3) -0.004(3) -0.014(3) C21 0.067(5) 0.073(6) 0.048(5) 0.014(4) 0.010(4) -0.006(5) C22 0.058(5) 0.047(4) 0.049(4) 0.019(4) 0.009(4) -0.003(4) C23 0.057(5) 0.054(5) 0.042(4) 0.011(3) 0.014(3) 0.007(4) C24 0.059(5) 0.069(6) 0.081(6) 0.022(5) 0.024(5) -0.005(5) C25 0.087(7) 0.064(6) 0.093(8) 0.003(6) 0.016(6) -0.039(6) C26 0.092(8) 0.048(5) 0.107(8) 0.000(5) 0.036(7) -0.016(5) C27 0.075(6) 0.047(5) 0.073(6) 0.011(4) 0.024(5) 0.005(4) _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 Pt1 S2 2.3176(15) . ? Pt1 S2 2.3176(15) 3_666 ? Pt1 S1 2.3180(15) 3_666 ? Pt1 S1 2.3180(15) . ? S1 C1 1.695(6) . ? S2 C2 1.700(6) . ? C1 C2 1.358(8) . ? C1 W1 2.017(5) . ? C2 W1 2.032(6) . ? W1 C3 2.009(6) . ? W1 C4 2.022(6) . ? W1 N1 2.198(5) . ? W1 N5 2.198(5) . ? W1 N3 2.216(5) . ? C3 O3 1.146(7) . ? C4 O4 1.139(7) . ? B1 N2 1.527(8) . ? B1 N6 1.542(9) . ? B1 N4 1.559(8) . ? N1 C6 1.347(7) . ? N1 N2 1.368(7) . ? N2 C8 1.351(8) . ? C5 C6 1.507(9) . ? C6 C7 1.371(9) . ? C7 C8 1.378(9) . ? C8 C9 1.493(9) . ? N3 C11 1.348(7) . ? N3 N4 1.374(7) . ? N4 C13 1.345(7) . ? C10 C11 1.489(9) . ? C11 C12 1.382(9) . ? C12 C13 1.370(8) . ? C13 C14 1.496(9) . ? N5 C16 1.356(7) . ? N5 N6 1.380(7) . ? N6 C18 1.352(8) . ? C15 C16 1.475(9) . ? C16 C17 1.398(9) . ? C17 C18 1.362(10) . ? C18 C19 1.492(9) . ? C21 C22 1.486(11) . ? C22 C23 1.367(11) . ? C22 C27 1.387(12) . ? C23 C24 1.415(12) . ? C24 C25 1.362(14) . ? C25 C26 1.373(15) . ? C26 C27 1.379(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 S2 Pt1 S2 180.00(7) . 3_666 ? S2 Pt1 S1 90.27(5) . 3_666 ? S2 Pt1 S1 89.73(5) 3_666 3_666 ? S2 Pt1 S1 89.73(5) . . ? S2 Pt1 S1 90.27(5) 3_666 . ? S1 Pt1 S1 180.0 3_666 . ? C1 S1 Pt1 101.8(2) . . ? C2 S2 Pt1 99.8(2) . . ? C2 C1 S1 122.1(4) . . ? C2 C1 W1 71.0(3) . . ? S1 C1 W1 166.4(4) . . ? C1 C2 S2 126.4(5) . . ? C1 C2 W1 69.8(3) . . ? S2 C2 W1 163.7(3) . . ? C3 W1 C1 108.8(2) . . ? C3 W1 C4 88.6(3) . . ? C1 W1 C4 94.3(2) . . ? C3 W1 C2 70.8(2) . . ? C1 W1 C2 39.2(2) . . ? C4 W1 C2 84.5(2) . . ? C3 W1 N1 92.8(2) . . ? C1 W1 N1 91.0(2) . . ? C4 W1 N1 173.7(2) . . ? C2 W1 N1 101.8(2) . . ? C3 W1 N5 163.4(2) . . ? C1 W1 N5 87.6(2) . . ? C4 W1 N5 92.0(2) . . ? C2 W1 N5 125.8(2) . . ? N1 W1 N5 84.92(18) . . ? C3 W1 N3 84.0(2) . . ? C1 W1 N3 166.3(2) . . ? C4 W1 N3 90.5(2) . . ? C2 W1 N3 154.4(2) . . ? N1 W1 N3 83.56(18) . . ? N5 W1 N3 79.40(17) . . ? O3 C3 W1 176.5(5) . . ? O4 C4 W1 177.1(6) . . ? N2 B1 N6 109.4(5) . . ? N2 B1 N4 108.1(5) . . ? N6 B1 N4 107.9(5) . . ? C6 N1 N2 106.2(5) . . ? C6 N1 W1 132.8(4) . . ? N2 N1 W1 120.9(3) . . ? C8 N2 N1 109.9(5) . . ? C8 N2 B1 130.1(5) . . ? N1 N2 B1 119.8(5) . . ? N1 C6 C7 110.1(6) . . ? N1 C6 C5 122.1(6) . . ? C7 C6 C5 127.8(6) . . ? C6 C7 C8 106.6(6) . . ? N2 C8 C7 107.3(6) . . ? N2 C8 C9 122.8(6) . . ? C7 C8 C9 129.9(6) . . ? C11 N3 N4 106.3(5) . . ? C11 N3 W1 133.8(4) . . ? N4 N3 W1 119.0(3) . . ? C13 N4 N3 110.0(5) . . ? C13 N4 B1 129.6(5) . . ? N3 N4 B1 120.2(5) . . ? N3 C11 C12 109.3(5) . . ? N3 C11 C10 124.1(6) . . ? C12 C11 C10 126.6(5) . . ? C13 C12 C11 107.0(5) . . ? N4 C13 C12 107.5(5) . . ? N4 C13 C14 123.5(5) . . ? C12 C13 C14 129.0(6) . . ? C16 N5 N6 106.8(5) . . ? C16 N5 W1 132.9(4) . . ? N6 N5 W1 120.3(4) . . ? C18 N6 N5 109.5(5) . . ? C18 N6 B1 130.4(5) . . ? N5 N6 B1 120.2(5) . . ? N5 C16 C17 108.4(6) . . ? N5 C16 C15 124.0(5) . . ? C17 C16 C15 127.6(6) . . ? C18 C17 C16 107.3(6) . . ? N6 C18 C17 108.1(6) . . ? N6 C18 C19 122.6(6) . . ? C17 C18 C19 129.3(6) . . ? C23 C22 C27 118.9(8) . . ? C23 C22 C21 121.4(8) . . ? C27 C22 C21 119.6(8) . . ? C22 C23 C24 120.5(8) . . ? C25 C24 C23 119.9(9) . . ? C24 C25 C26 119.3(10) . . ? C25 C26 C27 121.3(10) . . ? C26 C27 C22 120.1(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 5.259 _refine_diff_density_min -1.346 _refine_diff_density_rms 0.166