Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Long, Nicholas J.' 'Parker, D.' 'Speyer, Paul R.' 'White, Andrew J. P.' 'Williams, D.' _publ_contact_author_name 'Dr Nicholas J Long' _publ_contact_author_address ; Department of Chemistry Imperial College of Science, Technology and Medicine South Kensington London SW7 2AY UNITED KINGDOM ; _publ_contact_author_email 'N.LONG@IC.AC.UK' _publ_section_title ; Synthesis, Characterisation and Polymerisation of Vinylbenzene-Substituted Triazacyclododecanes and their Transition Metal Complexes ; data_NL9703 _database_code_CSD 170670 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H30 Cl N3 O' _chemical_formula_weight 351.91 _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' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 10.5465(4) _cell_length_b 12.7121(7) _cell_length_c 14.9812(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.868(4) _cell_angle_gamma 90.00 _cell_volume 1958.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 11.13 _cell_measurement_theta_max 27.96 _exptl_crystal_description 'Prismatic needles' _exptl_crystal_colour Clear _exptl_crystal_size_max 0.93 _exptl_crystal_size_mid 0.57 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method ? _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.796 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5038 _exptl_absorpt_correction_T_max 0.8425 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.37 _diffrn_reflns_number 3299 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.61 _diffrn_reflns_theta_max 62.98 _reflns_number_total 3116 _reflns_number_observed 2548 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 178 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^)+(0.0507P)^2^+0.5968P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0092(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2938 _refine_ls_number_parameters 234 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_obs 0.0457 _refine_ls_wR_factor_all 0.1203 _refine_ls_wR_factor_obs 0.1106 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.084 _refine_ls_restrained_S_all 1.061 _refine_ls_restrained_S_obs 1.086 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group N1 N 0.7263(2) 0.23647(12) 0.40697(11) 0.0462(4) Uani 1 d . . C2 C 0.7498(2) 0.3030(2) 0.4891(2) 0.0572(6) Uani 1 d . . H2A H 0.8312(2) 0.3403(2) 0.4938(2) 0.069 Uiso 1 calc R . H2B H 0.7586(2) 0.2584(2) 0.5427(2) 0.069 Uiso 1 calc R . C3 C 0.6415(2) 0.3829(2) 0.4889(2) 0.0666(7) Uani 1 d . . H3A H 0.5588(2) 0.3462(2) 0.4756(2) 0.080 Uiso 1 calc R . H3B H 0.6533(2) 0.4125(2) 0.5499(2) 0.080 Uiso 1 calc R . C4 C 0.6350(3) 0.4724(2) 0.4210(2) 0.0658(6) Uani 1 d . . H4A H 0.5666(3) 0.5206(2) 0.4280(2) 0.079 Uiso 1 calc R . H4B H 0.7166(3) 0.5106(2) 0.4350(2) 0.079 Uiso 1 calc R . N5 N 0.6099(2) 0.43662(13) 0.32545(13) 0.0515(4) Uani 1 d . . C6 C 0.4773(2) 0.4142(2) 0.2773(2) 0.0685(7) Uani 1 d . . H6A H 0.4224(2) 0.4745(2) 0.2810(2) 0.082 Uiso 1 calc R . H6B H 0.4441(2) 0.3547(2) 0.3056(2) 0.082 Uiso 1 calc R . C7 C 0.4743(3) 0.3896(2) 0.1783(2) 0.0768(8) Uani 1 d . . H7A H 0.3878(3) 0.3663(2) 0.1480(2) 0.092 Uiso 1 calc R . H7B H 0.4942(3) 0.4527(2) 0.1476(2) 0.092 Uiso 1 calc R . C8 C 0.5714(2) 0.3052(2) 0.1715(2) 0.0669(6) Uani 1 d . . H8A H 0.5456(2) 0.2395(2) 0.1952(2) 0.080 Uiso 1 calc R . H8B H 0.5747(2) 0.2946(2) 0.1080(2) 0.080 Uiso 1 calc R . N9 N 0.6995(2) 0.33691(13) 0.22446(13) 0.0543(5) Uani 1 d . . C10 C 0.8138(3) 0.2735(2) 0.2195(2) 0.0657(6) Uani 1 d . . H10A H 0.8913(3) 0.3164(2) 0.2379(2) 0.079 Uiso 1 calc R . H10B H 0.8076(3) 0.2519(2) 0.1566(2) 0.079 Uiso 1 calc R . C11 C 0.8274(2) 0.1757(2) 0.2804(2) 0.0609(6) Uani 1 d . . H11A H 0.7503(2) 0.1326(2) 0.2609(2) 0.073 Uiso 1 calc R . H11B H 0.9012(2) 0.1351(2) 0.2711(2) 0.073 Uiso 1 calc R . C12 C 0.8456(2) 0.1981(2) 0.3826(2) 0.0546(5) Uani 1 d . . H12A H 0.8737(2) 0.1342(2) 0.4167(2) 0.066 Uiso 1 calc R . H12B H 0.9136(2) 0.2503(2) 0.4006(2) 0.066 Uiso 1 calc R . C13 C 0.7080(2) 0.39504(15) 0.29779(15) 0.0495(5) Uani 1 d . . H13A H 0.7908(2) 0.40785(15) 0.33321(15) 0.059 Uiso 1 calc R . C14 C 0.6273(2) 0.1539(2) 0.40620(14) 0.0500(5) Uani 1 d . . H14A H 0.6109(2) 0.1190(2) 0.34714(14) 0.060 Uiso 1 calc R . H14B H 0.5469(2) 0.1877(2) 0.41174(14) 0.060 Uiso 1 calc R . C15 C 0.6609(2) 0.0708(2) 0.48006(14) 0.0487(5) Uani 1 d . . C16 C 0.7285(2) -0.0194(2) 0.4676(2) 0.0613(6) Uani 1 d . . H16A H 0.7541(2) -0.0293(2) 0.4126(2) 0.074 Uiso 1 calc R . C17 C 0.7587(3) -0.0951(2) 0.5354(2) 0.0730(7) Uani 1 d . . H17A H 0.8048(3) -0.1548(2) 0.5254(2) 0.088 Uiso 1 calc R . C18 C 0.7214(3) -0.0834(2) 0.6176(2) 0.0712(7) Uani 1 d D . C19 C 0.6516(2) 0.0055(2) 0.6298(2) 0.0673(7) Uani 1 d . . H19A H 0.6243(2) 0.0146(2) 0.6842(2) 0.081 Uiso 1 calc R . C20 C 0.6221(2) 0.0809(2) 0.56226(15) 0.0561(5) Uani 1 d . . H20A H 0.5750(2) 0.1400(2) 0.57201(15) 0.067 Uiso 1 calc R . C21 C 0.7418(4) -0.1529(4) 0.6982(3) 0.0652(11) Uani 0.62 d PD 1 H21A H 0.7073(4) -0.1331(4) 0.7477(3) 0.078 Uiso 0.62 calc PR 1 C22 C 0.8064(5) -0.2414(4) 0.7029(4) 0.094(2) Uani 0.62 d PD 1 H22A H 0.8416(5) -0.2624(4) 0.6540(4) 0.113 Uiso 0.62 calc PR 1 H22B H 0.8172(5) -0.2831(4) 0.7550(4) 0.113 Uiso 0.62 calc PR 1 C21' C 0.7778(9) -0.1862(7) 0.6713(6) 0.069(2) Uiso 0.38 d PD 2 H21B H 0.8200(9) -0.2388(7) 0.6460(6) 0.082 Uiso 0.38 calc PR 2 C22' C 0.7595(9) -0.1902(7) 0.7543(6) 0.086(2) Uiso 0.38 d PD 2 H22C H 0.7167(9) -0.1356(7) 0.7766(6) 0.104 Uiso 0.38 calc PR 2 H22D H 0.7893(9) -0.2478(7) 0.7914(6) 0.104 Uiso 0.38 calc PR 2 Cl Cl 0.01103(7) 0.51355(5) 0.33959(4) 0.0725(3) Uani 1 d . . O30 O 0.1080(2) 0.3636(2) 0.5103(2) 0.0838(6) Uani 1 d D . H30A H 0.0741(31) 0.3981(24) 0.5520(18) 0.112(13) Uiso 1 d D . H30B H 0.0892(42) 0.4049(27) 0.4603(17) 0.154(17) Uiso 1 d 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 N1 0.0410(9) 0.0445(9) 0.0513(9) -0.0035(7) 0.0062(7) -0.0040(7) C2 0.0569(13) 0.0556(12) 0.0551(13) -0.0062(10) 0.0038(10) -0.0048(10) C3 0.0663(15) 0.0706(15) 0.0640(14) -0.0194(12) 0.0170(12) -0.0027(12) C4 0.0626(14) 0.0512(13) 0.084(2) -0.0207(12) 0.0163(12) 0.0025(11) N5 0.0447(9) 0.0403(9) 0.0680(11) -0.0020(8) 0.0090(8) 0.0023(7) C6 0.0454(12) 0.0648(15) 0.090(2) -0.0034(13) 0.0050(12) 0.0076(11) C7 0.064(2) 0.069(2) 0.084(2) -0.0008(14) -0.0109(13) 0.0043(13) C8 0.074(2) 0.0597(14) 0.0626(14) -0.0027(11) 0.0048(12) -0.0043(12) N9 0.0572(10) 0.0492(10) 0.0578(11) 0.0039(8) 0.0155(8) 0.0010(8) C10 0.070(2) 0.0631(14) 0.072(2) 0.0041(12) 0.0327(12) 0.0083(12) C11 0.0600(13) 0.0495(12) 0.078(2) -0.0045(11) 0.0266(12) 0.0074(10) C12 0.0415(11) 0.0478(11) 0.0727(14) 0.0041(10) 0.0088(10) 0.0001(9) C13 0.0471(11) 0.0388(10) 0.0614(13) 0.0058(9) 0.0096(9) -0.0040(9) C14 0.0445(11) 0.0533(12) 0.0491(11) -0.0009(9) 0.0039(9) -0.0067(9) C15 0.0445(10) 0.0522(11) 0.0477(11) -0.0024(9) 0.0063(9) -0.0124(9) C16 0.0712(15) 0.0545(12) 0.0600(13) -0.0013(11) 0.0185(11) -0.0059(11) C17 0.073(2) 0.0526(13) 0.090(2) 0.0074(13) 0.0104(14) -0.0049(12) C18 0.0646(15) 0.075(2) 0.066(2) 0.0198(13) -0.0041(12) -0.0296(13) C19 0.0653(15) 0.085(2) 0.0507(13) 0.0015(12) 0.0100(11) -0.0307(14) C20 0.0486(12) 0.0661(14) 0.0540(12) -0.0055(11) 0.0125(10) -0.0155(10) C21 0.068(3) 0.070(3) 0.056(2) 0.016(2) 0.010(2) -0.011(2) C22 0.084(3) 0.088(3) 0.113(4) 0.048(3) 0.024(3) 0.018(3) Cl 0.0789(4) 0.0775(4) 0.0637(4) 0.0010(3) 0.0209(3) -0.0142(3) O30 0.0896(14) 0.0746(13) 0.0867(15) 0.0065(11) 0.0188(12) -0.0044(11) _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 N1 C2 1.467(3) . ? N1 C12 1.469(3) . ? N1 C14 1.479(2) . ? C2 C3 1.528(3) . ? C3 C4 1.517(4) . ? C4 N5 1.468(3) . ? N5 C13 1.309(3) . ? N5 C6 1.452(3) . ? C6 C7 1.509(4) . ? C7 C8 1.503(3) . ? C8 N9 1.463(3) . ? N9 C13 1.310(3) . ? N9 C10 1.466(3) . ? C10 C11 1.530(3) . ? C11 C12 1.527(3) . ? C14 C15 1.513(3) . ? C15 C16 1.385(3) . ? C15 C20 1.387(3) . ? C16 C17 1.384(3) . ? C17 C18 1.383(4) . ? C18 C19 1.383(4) . ? C18 C21 1.472(4) . ? C18 C21' 1.579(9) . ? C19 C20 1.378(3) . ? C21 C22 1.309(7) . ? C21' C22' 1.301(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C12 113.9(2) . . ? C2 N1 C14 113.7(2) . . ? C12 N1 C14 113.9(2) . . ? N1 C2 C3 113.3(2) . . ? C4 C3 C2 115.0(2) . . ? N5 C4 C3 113.2(2) . . ? C13 N5 C6 120.3(2) . . ? C13 N5 C4 116.8(2) . . ? C6 N5 C4 119.3(2) . . ? N5 C6 C7 109.7(2) . . ? C8 C7 C6 110.4(2) . . ? N9 C8 C7 109.1(2) . . ? C13 N9 C8 119.5(2) . . ? C13 N9 C10 116.7(2) . . ? C8 N9 C10 119.5(2) . . ? N9 C10 C11 112.7(2) . . ? C12 C11 C10 114.8(2) . . ? N1 C12 C11 112.8(2) . . ? N5 C13 N9 125.6(2) . . ? N1 C14 C15 116.1(2) . . ? C16 C15 C20 117.3(2) . . ? C16 C15 C14 121.5(2) . . ? C20 C15 C14 121.2(2) . . ? C17 C16 C15 121.2(2) . . ? C18 C17 C16 120.9(3) . . ? C17 C18 C19 118.1(2) . . ? C17 C18 C21 130.4(3) . . ? C19 C18 C21 111.5(3) . . ? C17 C18 C21' 102.4(4) . . ? C19 C18 C21' 139.5(4) . . ? C20 C19 C18 120.7(2) . . ? C19 C20 C15 121.7(2) . . ? C22 C21 C18 122.5(5) . . ? C22' C21' C18 113.6(9) . . ? _refine_diff_density_max 0.260 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.029 data_NL9801 _database_code_CSD 170671 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38.75 H61.50 Cl9.50 N6 Ni2 O' _chemical_formula_weight 1081.63 _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' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.8284(13) _cell_length_b 28.2797(14) _cell_length_c 38.356(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.750(6) _cell_angle_gamma 90.00 _cell_volume 20399.6(24) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 10.69 _cell_measurement_theta_max 22.51 _exptl_crystal_description prisms _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method ? _exptl_crystal_F_000 8984 _exptl_absorpt_coefficient_mu 5.778 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.0936 _exptl_absorpt_correction_T_max 0.2163 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15672 _diffrn_reflns_av_R_equivalents 0.0854 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 60.01 _reflns_number_total 15145 _reflns_number_observed 10581 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1353 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^)+(0.1413P)^2^+84.1615P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000015(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13792 _refine_ls_number_parameters 1102 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.1265 _refine_ls_R_factor_obs 0.0875 _refine_ls_wR_factor_all 0.2692 _refine_ls_wR_factor_obs 0.2239 _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.107 _refine_ls_restrained_S_all 1.108 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max -0.060 _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 Ni1 Ni 0.22115(6) 0.48359(4) 0.08801(3) 0.0369(3) Uani 1 d . . Ni2 Ni 0.22266(6) 0.48044(4) 0.17098(3) 0.0367(3) Uani 1 d . . O1 O 0.2301(3) 0.5348(2) 0.13047(14) 0.0411(11) Uani 1 d D . H1A H 0.1895(27) 0.5515(29) 0.1305(25) 0.055(26) Uiso 1 d D . H1B H 0.2687(50) 0.5524(48) 0.1363(44) 0.133(62) Uiso 1 d D . Cl1 Cl 0.12486(9) 0.46096(6) 0.12753(4) 0.0382(4) Uani 1 d . . Cl2 Cl 0.29520(9) 0.43875(7) 0.12990(5) 0.0439(4) Uani 1 d . . Cl3 Cl 0.37041(11) 0.58057(9) 0.13355(6) 0.0620(6) Uani 1 d . . Cl4 Cl 0.10973(11) 0.60050(8) 0.12961(6) 0.0551(5) Uani 1 d . . N1 N 0.2119(3) 0.4274(2) 0.0517(2) 0.0385(13) Uani 1 d . . C2 C 0.1796(4) 0.4449(3) 0.0179(2) 0.044(2) Uani 1 d . . H2A H 0.1799(4) 0.4186(3) 0.0009(2) 0.053 Uiso 1 calc R . H2B H 0.2109(4) 0.4700(3) 0.0092(2) 0.053 Uiso 1 calc R . C3 C 0.1039(4) 0.4647(3) 0.0178(2) 0.042(2) Uani 1 d . . H3A H 0.0942(4) 0.4811(3) -0.0048(2) 0.051 Uiso 1 calc R . H3B H 0.0707(4) 0.4376(3) 0.0184(2) 0.051 Uiso 1 calc R . C4 C 0.0859(4) 0.4984(3) 0.0466(2) 0.043(2) Uani 1 d . . H4A H 0.0488(4) 0.5205(3) 0.0375(2) 0.051 Uiso 1 calc R . H4B H 0.0655(4) 0.4800(3) 0.0657(2) 0.051 Uiso 1 calc R . N5 N 0.1463(3) 0.5260(2) 0.0612(2) 0.0429(14) Uani 1 d . . C6 C 0.1692(5) 0.5618(3) 0.0359(2) 0.054(2) Uani 1 d . . H6A H 0.1326(5) 0.5869(3) 0.0335(2) 0.064 Uiso 1 calc R . H6B H 0.1730(5) 0.5467(3) 0.0128(2) 0.064 Uiso 1 calc R . C7 C 0.2403(5) 0.5842(3) 0.0470(2) 0.055(2) Uani 1 d . . H7A H 0.2463(5) 0.6137(3) 0.0336(2) 0.066 Uiso 1 calc R . H7B H 0.2403(5) 0.5925(3) 0.0720(2) 0.066 Uiso 1 calc R . C8 C 0.3027(5) 0.5515(3) 0.0410(2) 0.054(2) Uani 1 d . . H8A H 0.2961(5) 0.5370(3) 0.0175(2) 0.065 Uiso 1 calc R . H8B H 0.3469(5) 0.5705(3) 0.0413(2) 0.065 Uiso 1 calc R . N9 N 0.3110(4) 0.5136(3) 0.0672(2) 0.049(2) Uani 1 d . . C10 C 0.3660(4) 0.4788(3) 0.0573(2) 0.051(2) Uani 1 d . . H10A H 0.3844(4) 0.4622(3) 0.0786(2) 0.061 Uiso 1 calc R . H10B H 0.4062(4) 0.4960(3) 0.0476(2) 0.061 Uiso 1 calc R . C11 C 0.3388(5) 0.4424(4) 0.0310(2) 0.056(2) Uani 1 d . . H11A H 0.3797(5) 0.4240(4) 0.0230(2) 0.068 Uiso 1 calc R . H11B H 0.3172(5) 0.4592(4) 0.0104(2) 0.068 Uiso 1 calc R . C12 C 0.2838(5) 0.4079(3) 0.0446(2) 0.049(2) Uani 1 d . . H12A H 0.2773(5) 0.3819(3) 0.0274(2) 0.059 Uiso 1 calc R . H12B H 0.3040(5) 0.3937(3) 0.0665(2) 0.059 Uiso 1 calc R . C13 C 0.1688(4) 0.3895(3) 0.0671(2) 0.045(2) Uani 1 d . . H13A H 0.1209(4) 0.4026(3) 0.0705(2) 0.053 Uiso 1 calc R . H13B H 0.1904(4) 0.3824(3) 0.0906(2) 0.053 Uiso 1 calc R . C14 C 0.1591(4) 0.3427(3) 0.0477(2) 0.044(2) Uani 1 d . . C15 C 0.2081(5) 0.3067(3) 0.0514(2) 0.053(2) Uani 1 d . . H15A H 0.2505(5) 0.3120(3) 0.0653(2) 0.064 Uiso 1 calc R . C16 C 0.1979(5) 0.2633(3) 0.0356(2) 0.054(2) Uani 1 d . . H16A H 0.2332(5) 0.2395(3) 0.0389(2) 0.065 Uiso 1 calc R . C17 C 0.1371(5) 0.2539(3) 0.0151(2) 0.053(2) Uani 1 d . . C18 C 0.0844(6) 0.2895(3) 0.0120(2) 0.060(2) Uani 1 d . . H18A H 0.0409(6) 0.2838(3) -0.0008(2) 0.071 Uiso 1 calc R . C19 C 0.0972(5) 0.3333(3) 0.0281(2) 0.051(2) Uani 1 d . . H19A H 0.0622(5) 0.3575(3) 0.0253(2) 0.061 Uiso 1 calc R . C20 C 0.1285(7) 0.2071(4) -0.0022(3) 0.070(3) Uani 1 d . . H20A H 0.1629(7) 0.1835(4) 0.0037(3) 0.084 Uiso 1 calc R . C21 C 0.0770(9) 0.1958(5) -0.0250(5) 0.113(5) Uani 1 d . . H21A H 0.0415(9) 0.2184(5) -0.0316(5) 0.135 Uiso 1 calc R . H21B H 0.0752(9) 0.1650(5) -0.0350(5) 0.135 Uiso 1 calc R . N22 N 0.2170(3) 0.4221(2) 0.2054(2) 0.0407(14) Uani 1 d . . C23 C 0.1869(4) 0.4379(3) 0.2390(2) 0.045(2) Uani 1 d . . H23A H 0.2176(4) 0.4634(3) 0.2490(2) 0.054 Uiso 1 calc R . H23B H 0.1899(4) 0.4110(3) 0.2556(2) 0.054 Uiso 1 calc R . C24 C 0.1101(4) 0.4559(3) 0.2371(2) 0.047(2) Uani 1 d . . H24A H 0.0783(4) 0.4281(3) 0.2344(2) 0.056 Uiso 1 calc R . H24B H 0.1007(4) 0.4707(3) 0.2598(2) 0.056 Uiso 1 calc R . C25 C 0.0887(4) 0.4911(3) 0.2085(2) 0.046(2) Uani 1 d . . H25A H 0.0676(4) 0.4734(3) 0.1883(2) 0.055 Uiso 1 calc R . H25B H 0.0514(4) 0.5121(3) 0.2172(2) 0.055 Uiso 1 calc R . N26 N 0.1474(3) 0.5207(2) 0.1964(2) 0.0416(14) Uani 1 d . . C27 C 0.1699(5) 0.5563(3) 0.2225(2) 0.051(2) Uani 1 d . . H27A H 0.1721(5) 0.5412(3) 0.2458(2) 0.061 Uiso 1 calc R . H27B H 0.1332(5) 0.5814(3) 0.2228(2) 0.061 Uiso 1 calc R . C28 C 0.2413(5) 0.5792(3) 0.2167(2) 0.057(2) Uani 1 d . . H28A H 0.2415(5) 0.5904(3) 0.1922(2) 0.068 Uiso 1 calc R . H28B H 0.2468(5) 0.6073(3) 0.2320(2) 0.068 Uiso 1 calc R . C29 C 0.3044(5) 0.5470(3) 0.2235(2) 0.055(2) Uani 1 d . . H29A H 0.3481(5) 0.5665(3) 0.2257(2) 0.067 Uiso 1 calc R . H29B H 0.2990(5) 0.5307(3) 0.2461(2) 0.067 Uiso 1 calc R . N30 N 0.3132(3) 0.5106(2) 0.1958(2) 0.0446(14) Uani 1 d . . C31 C 0.3689(4) 0.4761(4) 0.2061(2) 0.057(2) Uani 1 d . . H31A H 0.4095(4) 0.4931(4) 0.2177(2) 0.068 Uiso 1 calc R . H31B H 0.3861(4) 0.4609(4) 0.1849(2) 0.068 Uiso 1 calc R . C32 C 0.3438(5) 0.4381(3) 0.2306(2) 0.055(2) Uani 1 d . . H32A H 0.3226(5) 0.4536(3) 0.2508(2) 0.066 Uiso 1 calc R . H32B H 0.3856(5) 0.4198(3) 0.2395(2) 0.066 Uiso 1 calc R . C33 C 0.2891(5) 0.4038(3) 0.2138(2) 0.051(2) Uani 1 d . . H33A H 0.3084(5) 0.3917(3) 0.1919(2) 0.062 Uiso 1 calc R . H33B H 0.2848(5) 0.3765(3) 0.2297(2) 0.062 Uiso 1 calc R . C34 C 0.1739(4) 0.3833(3) 0.1885(2) 0.045(2) Uani 1 d . . H34A H 0.1922(4) 0.3776(3) 0.1651(2) 0.054 Uiso 1 calc R . H34B H 0.1244(4) 0.3947(3) 0.1850(2) 0.054 Uiso 1 calc R . C35 C 0.1723(4) 0.3369(3) 0.2072(2) 0.046(2) Uani 1 d . . C36 C 0.2221(5) 0.3016(3) 0.2004(2) 0.052(2) Uani 1 d . . H36A H 0.2568(5) 0.3073(3) 0.1838(2) 0.062 Uiso 1 calc R . C37 C 0.2217(5) 0.2586(3) 0.2175(2) 0.055(2) Uani 1 d . . H37A H 0.2576(5) 0.2360(3) 0.2132(2) 0.067 Uiso 1 calc R . C38 C 0.1696(5) 0.2477(3) 0.2408(2) 0.050(2) Uani 1 d . . C39 C 0.1182(5) 0.2814(3) 0.2467(2) 0.057(2) Uani 1 d . . H39A H 0.0816(5) 0.2743(3) 0.2620(2) 0.068 Uiso 1 calc R . C40 C 0.1189(5) 0.3263(3) 0.2303(2) 0.054(2) Uani 1 d . . H40A H 0.0835(5) 0.3491(3) 0.2349(2) 0.065 Uiso 1 calc R . C41 C 0.1713(5) 0.2015(3) 0.2584(3) 0.058(2) Uani 1 d . . H41A H 0.1951(5) 0.1766(3) 0.2471(3) 0.069 Uiso 1 calc R . C42 C 0.1438(7) 0.1909(4) 0.2879(4) 0.090(4) Uani 1 d . . H42A H 0.1195(7) 0.2144(4) 0.3004(4) 0.108 Uiso 1 calc R . H42B H 0.1481(7) 0.1597(4) 0.2970(4) 0.108 Uiso 1 calc R . Ni1' Ni 0.15408(6) 0.11148(4) 0.12830(3) 0.0375(3) Uani 1 d . . Ni2' Ni 0.32319(6) 0.11558(4) 0.13084(3) 0.0366(3) Uani 1 d . . O1' O 0.2418(3) 0.0595(2) 0.12545(13) 0.0380(11) Uani 1 d D . H1'A H 0.2538(44) 0.0382(22) 0.1093(16) 0.042(22) Uiso 1 d D . H1'B H 0.2495(67) 0.0369(32) 0.1417(24) 0.085(38) Uiso 1 d D . Cl1' Cl 0.23476(9) 0.15411(7) 0.09168(5) 0.0478(4) Uani 1 d . . Cl2' Cl 0.23978(9) 0.13657(7) 0.17570(5) 0.0444(4) Uani 1 d . . Cl3' Cl 0.24761(11) -0.00337(8) 0.18686(5) 0.0539(5) Uani 1 d . . Cl4' Cl 0.24077(11) 0.00741(8) 0.05760(5) 0.0532(5) Uani 1 d . . N1' N 0.0795(3) 0.1671(2) 0.1300(2) 0.0399(13) Uani 1 d . . C2' C 0.0585(4) 0.1830(3) 0.0939(2) 0.049(2) Uani 1 d . . H2'A H 0.1009(4) 0.1967(3) 0.0835(2) 0.059 Uiso 1 calc R . H2'B H 0.0232(4) 0.2088(3) 0.0956(2) 0.059 Uiso 1 calc R . C3' C 0.0269(5) 0.1454(3) 0.0686(2) 0.054(2) Uani 1 d . . H3'A H -0.0118(5) 0.1286(3) 0.0800(2) 0.065 Uiso 1 calc R . H3'B H 0.0056(5) 0.1615(3) 0.0477(2) 0.065 Uiso 1 calc R . C4' C 0.0806(5) 0.1092(3) 0.0569(2) 0.054(2) Uani 1 d . . H4'A H 0.0587(5) 0.0902(3) 0.0376(2) 0.064 Uiso 1 calc R . H4'B H 0.1221(5) 0.1259(3) 0.0479(2) 0.064 Uiso 1 calc R . N5' N 0.1056(3) 0.0768(3) 0.0856(2) 0.0470(15) Uani 1 d . . C6' C 0.0512(5) 0.0396(3) 0.0916(3) 0.054(2) Uani 1 d . . H6'A H 0.0463(5) 0.0192(3) 0.0706(3) 0.065 Uiso 1 calc R . H6'B H 0.0047(5) 0.0550(3) 0.0947(3) 0.065 Uiso 1 calc R . C7' C 0.0697(5) 0.0091(3) 0.1231(3) 0.057(2) Uani 1 d . . H7'A H 0.0419(5) -0.0206(3) 0.1213(3) 0.069 Uiso 1 calc R . H7'B H 0.1207(5) 0.0007(3) 0.1232(3) 0.069 Uiso 1 calc R . C8' C 0.0549(5) 0.0331(3) 0.1570(2) 0.053(2) Uani 1 d . . H8'A H 0.0068(5) 0.0473(3) 0.1550(2) 0.063 Uiso 1 calc R . H8'B H 0.0550(5) 0.0091(3) 0.1758(2) 0.063 Uiso 1 calc R . N9' N 0.1078(4) 0.0708(2) 0.1669(2) 0.0454(15) Uani 1 d . . C10' C 0.0829(4) 0.1006(3) 0.1953(2) 0.051(2) Uani 1 d . . H10C H 0.1232(4) 0.1198(3) 0.2048(2) 0.061 Uiso 1 calc R . H10D H 0.0675(4) 0.0798(3) 0.2143(2) 0.061 Uiso 1 calc R . C11' C 0.0212(4) 0.1338(3) 0.1844(2) 0.051(2) Uani 1 d . . H11C H -0.0236(4) 0.1181(3) 0.1904(2) 0.062 Uiso 1 calc R . H11D H 0.0260(4) 0.1627(3) 0.1988(2) 0.062 Uiso 1 calc R . C12' C 0.0135(4) 0.1489(3) 0.1465(2) 0.047(2) Uani 1 d . . H12C H -0.0047(4) 0.1216(3) 0.1327(2) 0.057 Uiso 1 calc R . H12D H -0.0232(4) 0.1740(3) 0.1446(2) 0.057 Uiso 1 calc R . C13' C 0.1107(4) 0.2081(3) 0.1497(2) 0.046(2) Uani 1 d . . H13C H 0.1577(4) 0.2151(3) 0.1405(2) 0.055 Uiso 1 calc R . H13D H 0.1189(4) 0.1985(3) 0.1744(2) 0.055 Uiso 1 calc R . C14' C 0.0668(4) 0.2543(3) 0.1489(2) 0.044(2) Uani 1 d . . C15' C 0.0122(5) 0.2617(3) 0.1714(3) 0.057(2) Uani 1 d . . H15B H 0.0001(5) 0.2374(3) 0.1872(3) 0.069 Uiso 1 calc R . C16' C -0.0248(5) 0.3039(4) 0.1711(3) 0.063(3) Uani 1 d . . H16B H -0.0642(5) 0.3073(4) 0.1854(3) 0.075 Uiso 1 calc R . C17' C -0.0058(5) 0.3407(3) 0.1505(2) 0.047(2) Uani 1 d . . C18' C 0.0491(5) 0.3331(3) 0.1276(3) 0.057(2) Uani 1 d . . H18B H 0.0618(5) 0.3577(3) 0.1122(3) 0.069 Uiso 1 calc R . C19' C 0.0842(5) 0.2915(3) 0.1271(2) 0.053(2) Uani 1 d . . H19B H 0.1215(5) 0.2874(3) 0.1115(2) 0.063 Uiso 1 calc R . C20' C -0.0397(5) 0.3871(3) 0.1516(3) 0.058(2) Uani 1 d . . H20B H -0.0233(5) 0.4103(3) 0.1359(3) 0.069 Uiso 1 calc R . C21' C -0.0915(6) 0.4002(3) 0.1723(3) 0.069(3) Uani 1 d . . H21C H -0.1098(6) 0.3784(3) 0.1883(3) 0.083 Uiso 1 calc R . H21D H -0.1100(6) 0.4315(3) 0.1709(3) 0.083 Uiso 1 calc R . N22' N 0.3921(3) 0.1747(2) 0.1374(2) 0.0453(15) Uani 1 d . . C23' C 0.4087(5) 0.1945(4) 0.1026(3) 0.064(2) Uani 1 d . . H23C H 0.4411(5) 0.2218(4) 0.1064(3) 0.077 Uiso 1 calc R . H23D H 0.3640(5) 0.2067(4) 0.0913(3) 0.077 Uiso 1 calc R . C24' C 0.4421(4) 0.1608(3) 0.0775(2) 0.053(2) Uani 1 d . . H24C H 0.4827(4) 0.1448(3) 0.0899(2) 0.063 Uiso 1 calc R . H24D H 0.4612(4) 0.1794(3) 0.0582(2) 0.063 Uiso 1 calc R . C25' C 0.3919(4) 0.1231(3) 0.0619(2) 0.049(2) Uani 1 d . . H25C H 0.3485(4) 0.1388(3) 0.0520(2) 0.058 Uiso 1 calc R . H25D H 0.4153(4) 0.1073(3) 0.0425(2) 0.058 Uiso 1 calc R . N26' N 0.3706(3) 0.0865(2) 0.0874(2) 0.0429(14) Uani 1 d . . C27' C 0.4289(4) 0.0505(3) 0.0930(2) 0.051(2) Uani 1 d . . H27C H 0.4319(4) 0.0311(3) 0.0716(2) 0.061 Uiso 1 calc R . H27D H 0.4748(4) 0.0671(3) 0.0969(2) 0.061 Uiso 1 calc R . C28' C 0.4173(4) 0.0187(3) 0.1231(2) 0.051(2) Uani 1 d . . H28C H 0.4477(4) -0.0096(3) 0.1210(2) 0.061 Uiso 1 calc R . H28D H 0.3672(4) 0.0080(3) 0.1218(2) 0.061 Uiso 1 calc R . C29' C 0.4330(5) 0.0407(3) 0.1586(2) 0.052(2) Uani 1 d . . H29C H 0.4368(5) 0.0153(3) 0.1763(2) 0.062 Uiso 1 calc R . H29D H 0.4796(5) 0.0570(3) 0.1585(2) 0.062 Uiso 1 calc R . N30' N 0.3785(3) 0.0748(2) 0.1686(2) 0.0450(14) Uani 1 d . . C31' C 0.4025(4) 0.1024(3) 0.1993(2) 0.051(2) Uani 1 d . . H31C H 0.4222(4) 0.0806(3) 0.2174(2) 0.061 Uiso 1 calc R . H31D H 0.3609(4) 0.1185(3) 0.2089(2) 0.061 Uiso 1 calc R . C32' C 0.4583(5) 0.1393(3) 0.1917(2) 0.054(2) Uani 1 d . . H32C H 0.5056(5) 0.1253(3) 0.1976(2) 0.065 Uiso 1 calc R . H32D H 0.4523(5) 0.1661(3) 0.2079(2) 0.065 Uiso 1 calc R . C33' C 0.4598(5) 0.1595(3) 0.1549(2) 0.055(2) Uani 1 d . . H33C H 0.4923(5) 0.1870(3) 0.1557(2) 0.066 Uiso 1 calc R . H33D H 0.4811(5) 0.1353(3) 0.1400(2) 0.066 Uiso 1 calc R . C34' C 0.3574(5) 0.2123(4) 0.1582(3) 0.062(2) Uani 1 d . . H34C H 0.3521(5) 0.1999(4) 0.1821(3) 0.075 Uiso 1 calc R . H34D H 0.3090(5) 0.2175(4) 0.1477(3) 0.075 Uiso 1 calc R . C35' C 0.3938(5) 0.2603(4) 0.1615(3) 0.067(3) Uani 1 d . . C36' C 0.4409(8) 0.2687(5) 0.1902(3) 0.087(4) Uani 1 d . . H36B H 0.4499(8) 0.2445(5) 0.2070(3) 0.104 Uiso 1 calc R . C37' C 0.4742(9) 0.3118(5) 0.1943(4) 0.095(4) Uani 1 d . . H37B H 0.5043(9) 0.3178(5) 0.2144(4) 0.114 Uiso 1 calc R . C38' C 0.4637(7) 0.3468(4) 0.1689(3) 0.072(3) Uani 1 d . . C39' C 0.4194(7) 0.3388(4) 0.1419(4) 0.076(3) Uani 1 d . . H39B H 0.4121(7) 0.3628(4) 0.1248(4) 0.091 Uiso 1 calc R . C40' C 0.3830(5) 0.2960(4) 0.1376(3) 0.070(3) Uani 1 d . . H40B H 0.3506(5) 0.2916(4) 0.1181(3) 0.084 Uiso 1 calc R . C41' C 0.5048(8) 0.3923(4) 0.1722(4) 0.089(4) Uani 1 d . . H41B H 0.4910(8) 0.4165(4) 0.1561(4) 0.107 Uiso 1 calc R . C42' C 0.5536(13) 0.4022(6) 0.1929(6) 0.164(11) Uani 1 d U . H42C H 0.5701(13) 0.3796(6) 0.2098(6) 0.197 Uiso 1 calc R . H42D H 0.5753(13) 0.4325(6) 0.1923(6) 0.197 Uiso 1 calc R . C50 C -0.1456(7) 0.4026(5) 0.0680(3) 0.087(4) Uani 1 d . . H50A H -0.1361(7) 0.3870(5) 0.0909(3) 0.105 Uiso 1 calc R . H50B H -0.1757(7) 0.4306(5) 0.0719(3) 0.105 Uiso 1 calc R . Cl51 Cl -0.0649(2) 0.42178(13) 0.05253(9) 0.0888(8) Uani 1 d . . Cl52 Cl -0.1924(4) 0.3642(2) 0.04121(13) 0.152(2) Uani 1 d . . C55 C -0.2893(12) 0.3676(9) 0.1630(6) 0.147(8) Uani 1 d . . C55A H -0.3420(12) 0.3671(9) 0.1615(6) 0.176 Uiso 1 calc R . H55B H -0.2737(12) 0.4006(9) 0.1675(6) 0.176 Uiso 1 calc R . Cl56 Cl -0.2580(3) 0.3313(2) 0.19743(14) 0.146(2) Uani 1 d . . Cl57 Cl -0.2575(5) 0.3483(4) 0.1244(2) 0.233(4) Uani 1 d U . C60 C -0.3410(11) 0.2032(8) 0.1819(6) 0.144(8) Uani 1 d . . H60A H -0.3464(11) 0.1721(8) 0.1702(6) 0.173 Uiso 1 calc R . H60B H -0.2895(11) 0.2105(8) 0.1840(6) 0.173 Uiso 1 calc R . Cl61 Cl -0.3720(3) 0.1986(2) 0.2230(2) 0.156(2) Uani 1 d . . Cl62 Cl -0.3858(4) 0.2489(3) 0.1534(3) 0.230(5) Uani 1 d . . C65 C 0.7697(43) 0.1969(26) 0.1031(20) 0.214(27) Uani 0.50 d PU . Cl66 Cl 0.8760(11) 0.2859(8) -0.0424(8) 0.238(11) Uani 0.50 d P . Cl67 Cl 0.9196(15) 0.2324(10) -0.0880(9) 0.311(14) Uani 0.50 d PU . C70 C 0.6040(14) 0.4127(11) 0.0497(9) 0.125(10) Uani 0.75 d P 1 Cl71 Cl 0.5469(3) 0.4388(3) 0.01961(14) 0.128(3) Uani 0.70 d P 1 Cl72 Cl 0.5569(5) 0.3853(3) 0.0842(2) 0.151(3) Uani 0.65 d P 1 Cl73 Cl 0.6684(26) 0.3659(17) 0.0383(12) 0.157(13) Uiso 0.15 d P 1 C75 C 0.8811(35) 0.1032(21) -0.0495(16) 0.068(14) Uiso 0.25 d P 2 H75A H 0.8772(35) 0.1195(21) -0.0723(16) 0.081 Uiso 0.25 calc PR 2 H75B H 0.8416(35) 0.0803(21) -0.0479(16) 0.081 Uiso 0.25 calc PR 2 Cl76 Cl 0.8826(16) 0.1415(11) -0.0167(8) 0.166(9) Uiso 0.25 d P 2 Cl77 Cl 0.9599(17) 0.0774(11) -0.0427(8) 0.162(9) Uiso 0.25 d P 2 C80 C 0.8388(16) 0.1989(12) 0.0468(11) 0.095(8) Uani 0.50 d PU . Cl81 Cl 0.8505(19) 0.2146(13) 0.0600(11) 0.332(13) Uani 0.50 d PU . Cl82 Cl 0.8392(16) 0.2386(12) 0.1167(8) 0.311(11) Uani 0.50 d PU . C85 C 0.8543(52) 0.1931(35) 0.0213(30) 0.136(27) Uiso 0.25 d P . Cl86 Cl 0.8652(32) 0.2088(21) -0.0061(17) 0.290(25) Uiso 0.25 d P . Cl87 Cl 0.8371(18) 0.1956(12) 0.0963(9) 0.173(10) Uiso 0.25 d P . C90 C 0.8368(62) 0.2330(42) -0.0489(31) 0.168(37) Uiso 0.25 d P . Cl91 Cl 0.8595(32) 0.2853(22) -0.0769(17) 0.275(24) Uiso 0.25 d P . Cl92 Cl 0.8881(14) 0.3059(9) -0.0291(7) 0.131(7) Uiso 0.25 d P . 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 0.0326(6) 0.0435(7) 0.0354(6) -0.0019(5) 0.0099(5) -0.0001(5) Ni2 0.0351(6) 0.0408(6) 0.0348(6) -0.0036(5) 0.0062(5) 0.0006(5) O1 0.036(3) 0.045(3) 0.043(3) -0.003(2) 0.007(2) 0.003(2) Cl1 0.0360(8) 0.0434(9) 0.0360(8) -0.0026(7) 0.0103(6) -0.0038(7) Cl2 0.0397(9) 0.0511(10) 0.0414(9) -0.0021(7) 0.0085(7) 0.0094(8) Cl3 0.0414(10) 0.0736(14) 0.0715(13) -0.0014(11) 0.0075(9) -0.0196(10) Cl4 0.0416(10) 0.0565(11) 0.0678(12) -0.0029(9) 0.0089(9) 0.0113(9) N1 0.039(3) 0.043(3) 0.034(3) -0.002(2) 0.013(2) 0.003(3) C2 0.051(4) 0.050(4) 0.033(4) 0.003(3) 0.014(3) -0.004(3) C3 0.039(4) 0.053(4) 0.035(4) 0.001(3) 0.006(3) -0.003(3) C4 0.035(4) 0.054(4) 0.039(4) 0.003(3) 0.002(3) -0.004(3) N5 0.042(3) 0.045(3) 0.043(3) 0.001(3) 0.009(3) -0.001(3) C6 0.052(5) 0.055(5) 0.053(5) 0.013(4) 0.004(4) -0.003(4) C7 0.056(5) 0.055(5) 0.055(5) 0.012(4) 0.009(4) -0.011(4) C8 0.053(5) 0.059(5) 0.052(5) 0.003(4) 0.015(4) -0.012(4) N9 0.041(3) 0.054(4) 0.053(4) -0.001(3) 0.018(3) -0.003(3) C10 0.039(4) 0.066(5) 0.049(4) -0.002(4) 0.016(3) -0.004(4) C11 0.042(4) 0.074(6) 0.056(5) -0.011(4) 0.029(4) -0.001(4) C12 0.050(4) 0.053(5) 0.045(4) -0.011(3) 0.016(3) 0.005(4) C13 0.046(4) 0.048(4) 0.040(4) -0.001(3) 0.017(3) 0.005(3) C14 0.053(4) 0.042(4) 0.039(4) -0.005(3) 0.015(3) 0.000(3) C15 0.055(5) 0.048(5) 0.058(5) 0.003(4) 0.017(4) 0.000(4) C16 0.058(5) 0.043(4) 0.062(5) 0.001(4) 0.026(4) 0.006(4) C17 0.070(6) 0.038(4) 0.052(5) 0.002(3) 0.029(4) -0.003(4) C18 0.075(6) 0.050(5) 0.054(5) 0.003(4) 0.009(4) -0.012(4) C19 0.056(5) 0.039(4) 0.058(5) 0.001(4) 0.008(4) 0.005(4) C20 0.085(7) 0.052(5) 0.077(7) -0.010(5) 0.032(6) -0.008(5) C21 0.119(12) 0.075(8) 0.144(14) -0.041(9) 0.007(10) -0.025(8) N22 0.046(3) 0.043(3) 0.034(3) -0.004(3) 0.008(3) 0.003(3) C23 0.048(4) 0.050(4) 0.038(4) -0.004(3) 0.011(3) 0.006(4) C24 0.051(5) 0.050(4) 0.041(4) 0.004(3) 0.013(3) 0.006(4) C25 0.044(4) 0.056(5) 0.038(4) 0.003(3) 0.011(3) 0.006(4) N26 0.044(3) 0.039(3) 0.042(3) -0.006(3) 0.011(3) 0.000(3) C27 0.057(5) 0.044(4) 0.053(5) -0.015(4) 0.013(4) -0.002(4) C28 0.070(6) 0.045(4) 0.055(5) -0.011(4) 0.002(4) -0.004(4) C29 0.057(5) 0.060(5) 0.049(5) -0.003(4) 0.000(4) -0.013(4) N30 0.042(3) 0.049(4) 0.042(3) -0.006(3) 0.001(3) -0.008(3) C31 0.034(4) 0.082(6) 0.053(5) 0.006(4) -0.002(3) -0.002(4) C32 0.045(4) 0.060(5) 0.058(5) 0.001(4) -0.006(4) 0.004(4) C33 0.052(5) 0.053(5) 0.050(4) 0.000(4) 0.005(4) 0.010(4) C34 0.048(4) 0.046(4) 0.041(4) -0.002(3) 0.008(3) 0.002(3) C35 0.050(4) 0.047(4) 0.040(4) -0.004(3) 0.008(3) 0.005(4) C36 0.064(5) 0.039(4) 0.054(5) -0.003(3) 0.020(4) 0.008(4) C37 0.060(5) 0.057(5) 0.050(5) -0.003(4) 0.013(4) 0.009(4) C38 0.049(4) 0.049(4) 0.053(5) 0.000(4) 0.010(4) 0.001(4) C39 0.059(5) 0.053(5) 0.060(5) 0.006(4) 0.023(4) 0.000(4) C40 0.056(5) 0.048(5) 0.061(5) 0.004(4) 0.018(4) 0.002(4) C41 0.056(5) 0.046(5) 0.072(6) 0.007(4) 0.016(4) 0.001(4) C42 0.084(8) 0.064(7) 0.127(11) 0.033(7) 0.048(8) 0.019(6) Ni1' 0.0319(6) 0.0370(6) 0.0441(7) 0.0013(5) 0.0072(5) -0.0007(5) Ni2' 0.0303(6) 0.0393(6) 0.0408(6) 0.0002(5) 0.0085(5) 0.0018(5) O1' 0.036(3) 0.039(3) 0.039(3) 0.002(2) 0.006(2) 0.004(2) Cl1' 0.0351(9) 0.0517(10) 0.0571(11) 0.0152(8) 0.0072(7) 0.0020(8) Cl2' 0.0344(8) 0.0503(10) 0.0491(10) -0.0057(8) 0.0103(7) 0.0029(7) Cl3' 0.0559(11) 0.0592(12) 0.0472(10) 0.0154(9) 0.0071(8) 0.0059(9) Cl4' 0.0546(11) 0.0626(12) 0.0433(10) -0.0058(8) 0.0124(8) -0.0025(9) N1' 0.028(3) 0.041(3) 0.052(4) -0.001(3) 0.009(2) -0.002(3) C2' 0.044(4) 0.052(5) 0.051(4) 0.012(4) 0.006(3) 0.007(4) C3' 0.046(4) 0.066(6) 0.050(4) 0.004(4) -0.001(3) 0.017(4) C4' 0.054(5) 0.063(5) 0.044(4) -0.002(4) 0.002(4) 0.010(4) N5' 0.037(3) 0.051(4) 0.053(4) 0.004(3) 0.002(3) 0.002(3) C6' 0.044(4) 0.046(4) 0.073(6) -0.006(4) 0.000(4) -0.006(4) C7' 0.051(5) 0.045(5) 0.077(6) -0.002(4) 0.008(4) -0.012(4) C8' 0.044(4) 0.048(5) 0.067(5) 0.010(4) 0.011(4) -0.004(4) N9' 0.043(3) 0.044(3) 0.050(4) 0.009(3) 0.009(3) 0.005(3) C10' 0.042(4) 0.061(5) 0.050(4) 0.009(4) 0.012(3) 0.002(4) C11' 0.040(4) 0.057(5) 0.059(5) -0.001(4) 0.020(4) 0.000(4) C12' 0.037(4) 0.045(4) 0.061(5) 0.005(4) 0.014(3) 0.004(3) C13' 0.035(4) 0.040(4) 0.063(5) 0.000(4) 0.007(3) -0.001(3) C14' 0.037(4) 0.040(4) 0.057(5) 0.002(3) 0.010(3) 0.004(3) C15' 0.061(5) 0.045(5) 0.068(6) 0.012(4) 0.025(4) 0.003(4) C16' 0.058(5) 0.059(5) 0.074(6) 0.013(5) 0.035(5) 0.013(4) C17' 0.049(4) 0.044(4) 0.049(4) 0.003(3) 0.010(3) 0.000(3) C18' 0.052(5) 0.046(5) 0.076(6) 0.008(4) 0.027(4) 0.004(4) C19' 0.047(4) 0.051(5) 0.062(5) 0.001(4) 0.026(4) -0.001(4) C20' 0.055(5) 0.055(5) 0.065(5) 0.008(4) 0.019(4) -0.004(4) C21' 0.083(7) 0.047(5) 0.080(7) -0.001(5) 0.035(6) 0.012(5) N22' 0.033(3) 0.048(4) 0.056(4) 0.000(3) 0.011(3) 0.002(3) C23' 0.052(5) 0.062(6) 0.080(6) 0.004(5) 0.018(5) -0.006(4) C24' 0.041(4) 0.068(5) 0.049(4) 0.007(4) 0.010(3) -0.006(4) C25' 0.048(4) 0.063(5) 0.036(4) 0.001(4) 0.014(3) 0.002(4) N26' 0.039(3) 0.050(4) 0.040(3) -0.005(3) 0.013(3) -0.001(3) C27' 0.041(4) 0.053(5) 0.060(5) -0.011(4) 0.013(4) 0.009(4) C28' 0.040(4) 0.041(4) 0.074(6) -0.007(4) 0.015(4) 0.008(3) C29' 0.047(4) 0.050(5) 0.057(5) 0.009(4) 0.007(4) 0.009(4) N30' 0.037(3) 0.052(4) 0.045(3) 0.002(3) 0.005(3) 0.000(3) C31' 0.041(4) 0.070(6) 0.042(4) 0.000(4) 0.004(3) -0.003(4) C32' 0.044(4) 0.063(5) 0.055(5) 0.000(4) 0.004(4) -0.007(4) C33' 0.047(4) 0.058(5) 0.060(5) -0.008(4) 0.009(4) -0.009(4) C34' 0.046(5) 0.063(6) 0.079(6) -0.007(5) 0.021(4) 0.000(4) C35' 0.052(5) 0.061(6) 0.090(7) -0.005(5) 0.025(5) -0.004(4) C36' 0.121(11) 0.070(7) 0.070(7) 0.002(5) 0.002(7) -0.018(7) C37' 0.134(12) 0.067(7) 0.083(8) -0.016(6) -0.007(8) -0.023(8) C38' 0.084(7) 0.044(5) 0.091(8) -0.007(5) 0.021(6) -0.001(5) C39' 0.079(7) 0.052(6) 0.096(8) 0.003(5) 0.006(6) 0.009(5) C40' 0.048(5) 0.065(6) 0.096(8) -0.001(5) -0.002(5) 0.007(4) C41' 0.105(10) 0.049(6) 0.114(10) 0.012(6) 0.003(8) -0.013(6) C42' 0.233(25) 0.074(9) 0.174(19) 0.025(11) -0.113(19) -0.056(13) C50 0.083(8) 0.100(9) 0.079(7) 0.011(7) -0.002(6) -0.022(7) Cl51 0.068(2) 0.105(2) 0.094(2) 0.000(2) 0.0124(14) 0.000(2) Cl52 0.194(5) 0.157(4) 0.102(3) 0.011(3) -0.010(3) -0.095(4) C55 0.139(17) 0.150(18) 0.153(19) -0.001(15) 0.020(14) -0.031(15) Cl56 0.170(5) 0.153(4) 0.112(3) 0.009(3) -0.027(3) -0.055(4) Cl57 0.221(7) 0.324(11) 0.156(6) -0.006(6) 0.037(5) -0.148(8) C60 0.107(13) 0.164(19) 0.158(19) -0.013(15) -0.022(12) 0.044(13) Cl61 0.090(3) 0.177(5) 0.203(6) -0.076(5) 0.018(3) -0.030(3) Cl62 0.139(5) 0.173(6) 0.377(14) 0.002(8) -0.005(7) -0.075(5) C65 0.218(32) 0.206(32) 0.219(32) -0.007(19) 0.025(19) -0.002(19) Cl66 0.192(17) 0.226(21) 0.296(29) -0.076(20) 0.010(17) -0.055(15) Cl67 0.266(24) 0.263(24) 0.404(37) -0.045(24) 0.019(24) -0.140(21) C70 0.083(16) 0.113(22) 0.179(28) -0.021(19) 0.021(15) 0.008(15) Cl71 0.064(2) 0.244(8) 0.078(3) -0.035(4) 0.015(2) -0.027(4) Cl72 0.178(8) 0.144(6) 0.135(6) -0.041(5) 0.046(6) -0.046(6) C80 0.070(12) 0.086(14) 0.127(18) -0.019(13) -0.013(12) -0.011(11) Cl81 0.311(17) 0.349(18) 0.333(18) -0.018(15) -0.014(15) 0.036(15) Cl82 0.298(16) 0.325(17) 0.303(17) -0.031(14) -0.055(14) 0.017(14) _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 N5 2.084(7) . ? Ni1 N9 2.085(6) . ? Ni1 N1 2.116(6) . ? Ni1 O1 2.179(5) . ? Ni1 Cl2 2.433(2) . ? Ni1 Cl1 2.502(2) . ? Ni2 N30 2.094(6) . ? Ni2 N26 2.095(6) . ? Ni2 N22 2.119(7) . ? Ni2 O1 2.194(6) . ? Ni2 Cl2 2.438(2) . ? Ni2 Cl1 2.485(2) . ? O1 Cl4 2.931(5) . ? O1 Cl3 2.939(6) . ? N1 C13 1.484(10) . ? N1 C2 1.489(10) . ? N1 C12 1.498(10) . ? C2 C3 1.532(11) . ? C3 C4 1.510(11) . ? C4 N5 1.468(10) . ? N5 C6 1.481(10) . ? C6 C7 1.522(13) . ? C7 C8 1.521(13) . ? C8 N9 1.474(12) . ? N9 C10 1.491(11) . ? C10 C11 1.514(13) . ? C11 C12 1.533(12) . ? C13 C14 1.525(11) . ? C14 C15 1.376(12) . ? C14 C19 1.383(13) . ? C15 C16 1.378(13) . ? C16 C17 1.383(14) . ? C17 C18 1.415(14) . ? C17 C20 1.486(13) . ? C18 C19 1.399(13) . ? C20 C21 1.31(2) . ? N22 C33 1.474(11) . ? N22 C34 1.495(10) . ? N22 C23 1.500(9) . ? C23 C24 1.531(11) . ? C24 C25 1.523(11) . ? C25 N26 1.480(10) . ? N26 C27 1.469(10) . ? C27 C28 1.519(13) . ? C28 C29 1.510(14) . ? C29 N30 1.496(11) . ? N30 C31 1.472(11) . ? C31 C32 1.517(13) . ? C32 C33 1.535(13) . ? C34 C35 1.496(12) . ? C35 C36 1.403(12) . ? C35 C40 1.404(12) . ? C36 C37 1.379(13) . ? C37 C38 1.395(12) . ? C38 C39 1.384(13) . ? C38 C41 1.472(13) . ? C39 C40 1.417(13) . ? C41 C42 1.30(2) . ? Ni1' N5' 2.082(7) . ? Ni1' N9' 2.098(6) . ? Ni1' N1' 2.111(6) . ? Ni1' O1' 2.218(5) . ? Ni1' Cl1' 2.437(2) . ? Ni1' Cl2' 2.476(2) . ? Ni2' N30' 2.089(7) . ? Ni2' N26' 2.097(6) . ? Ni2' N22' 2.125(7) . ? Ni2' O1' 2.209(5) . ? Ni2' Cl1' 2.444(2) . ? Ni2' Cl2' 2.457(2) . ? O1' Cl3' 2.949(5) . ? O1' Cl4' 2.990(5) . ? N1' C13' 1.490(10) . ? N1' C2' 1.493(10) . ? N1' C12' 1.512(9) . ? C2' C3' 1.541(13) . ? C3' C4' 1.521(12) . ? C4' N5' 1.490(11) . ? N5' C6' 1.492(11) . ? C6' C7' 1.514(14) . ? C7' C8' 1.503(13) . ? C8' N9' 1.498(11) . ? N9' C10' 1.471(11) . ? C10' C11' 1.537(12) . ? C11' C12' 1.514(12) . ? C13' C14' 1.546(11) . ? C14' C15' 1.389(12) . ? C14' C19' 1.393(12) . ? C15' C16' 1.382(13) . ? C16' C17' 1.363(13) . ? C17' C18' 1.407(12) . ? C17' C20' 1.460(13) . ? C18' C19' 1.351(13) . ? C20' C21' 1.341(13) . ? N22' C33' 1.476(12) . ? N22' C23' 1.496(12) . ? N22' C34' 1.498(11) . ? C23' C24' 1.511(13) . ? C24' C25' 1.527(13) . ? C25' N26' 1.491(10) . ? N26' C27' 1.504(11) . ? C27' C28' 1.491(13) . ? C28' C29' 1.512(13) . ? C29' N30' 1.474(11) . ? N30' C31' 1.467(11) . ? C31' C32' 1.520(12) . ? C32' C33' 1.523(13) . ? C34' C35' 1.521(14) . ? C35' C40' 1.37(2) . ? C35' C36' 1.40(2) . ? C36' C37' 1.38(2) . ? C37' C38' 1.39(2) . ? C38' C39' 1.32(2) . ? C38' C41' 1.50(2) . ? C39' C40' 1.40(2) . ? C41' C42' 1.22(2) . ? C50 Cl52 1.710(14) . ? C50 Cl51 1.744(13) . ? C55 Cl57 1.71(2) . ? C55 Cl56 1.75(2) . ? C60 Cl61 1.71(2) . ? C60 Cl62 1.87(2) . ? C65 Cl87 1.31(8) . ? C65 Cl82 1.82(8) . ? Cl66 Cl92 0.79(3) . ? Cl66 Cl91 1.34(6) . ? Cl66 C90 1.68(12) . ? Cl66 Cl67 2.48(4) . ? Cl67 Cl91 1.93(6) . ? Cl67 C90 2.22(12) . ? C70 Cl71 1.71(3) . ? C70 Cl72 1.80(3) . ? C70 Cl73 1.86(5) . ? C75 Cl76 1.66(7) . ? C75 Cl77 1.66(7) . ? Cl76 Cl86 1.98(6) . ? Cl76 C85 2.15(11) . ? C80 Cl81 0.70(5) . ? C80 C85 1.05(11) . ? C80 Cl87 1.90(6) . ? C80 Cl86 2.13(7) . ? Cl81 Cl87 1.53(4) . ? Cl81 C85 1.61(11) . ? Cl81 Cl82 2.30(5) . ? Cl82 Cl87 1.45(4) . ? C85 Cl86 1.17(10) . ? Cl86 C90 1.83(12) . ? C90 Cl91 1.89(12) . ? Cl91 Cl92 1.98(7) . ? 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 N5 Ni1 N9 96.9(3) . . ? N5 Ni1 N1 94.3(3) . . ? N9 Ni1 N1 95.5(3) . . ? N5 Ni1 O1 90.7(2) . . ? N9 Ni1 O1 88.9(2) . . ? N1 Ni1 O1 172.8(2) . . ? N5 Ni1 Cl2 168.0(2) . . ? N9 Ni1 Cl2 90.8(2) . . ? N1 Ni1 Cl2 94.0(2) . . ? O1 Ni1 Cl2 80.3(2) . . ? N5 Ni1 Cl1 87.3(2) . . ? N9 Ni1 Cl1 163.9(2) . . ? N1 Ni1 Cl1 99.7(2) . . ? O1 Ni1 Cl1 75.49(14) . . ? Cl2 Ni1 Cl1 82.84(7) . . ? N30 Ni2 N26 97.0(3) . . ? N30 Ni2 N22 95.7(3) . . ? N26 Ni2 N22 94.5(2) . . ? N30 Ni2 O1 87.6(2) . . ? N26 Ni2 O1 90.9(2) . . ? N22 Ni2 O1 173.3(2) . . ? N30 Ni2 Cl2 91.2(2) . . ? N26 Ni2 Cl2 167.4(2) . . ? N22 Ni2 Cl2 94.2(2) . . ? O1 Ni2 Cl2 79.87(14) . . ? N30 Ni2 Cl1 162.9(2) . . ? N26 Ni2 Cl1 86.4(2) . . ? N22 Ni2 Cl1 100.8(2) . . ? O1 Ni2 Cl1 75.58(15) . . ? Cl2 Ni2 Cl1 83.08(7) . . ? Ni1 O1 Ni2 93.4(2) . . ? Ni1 O1 Cl4 112.4(2) . . ? Ni2 O1 Cl4 112.1(2) . . ? Ni1 O1 Cl3 111.1(2) . . ? Ni2 O1 Cl3 111.6(2) . . ? Cl4 O1 Cl3 114.5(2) . . ? Ni2 Cl1 Ni1 79.31(6) . . ? Ni1 Cl2 Ni2 81.59(7) . . ? C13 N1 C2 112.3(6) . . ? C13 N1 C12 108.8(6) . . ? C2 N1 C12 107.5(6) . . ? C13 N1 Ni1 107.9(4) . . ? C2 N1 Ni1 109.8(5) . . ? C12 N1 Ni1 110.4(5) . . ? N1 C2 C3 117.8(6) . . ? C4 C3 C2 117.9(6) . . ? N5 C4 C3 114.8(6) . . ? C4 N5 C6 111.0(6) . . ? C4 N5 Ni1 112.0(5) . . ? C6 N5 Ni1 120.3(5) . . ? N5 C6 C7 112.5(7) . . ? C8 C7 C6 112.4(8) . . ? N9 C8 C7 113.3(7) . . ? C8 N9 C10 111.0(6) . . ? C8 N9 Ni1 119.7(5) . . ? C10 N9 Ni1 114.5(5) . . ? N9 C10 C11 113.7(7) . . ? C10 C11 C12 114.7(7) . . ? N1 C12 C11 117.2(7) . . ? N1 C13 C14 119.1(6) . . ? C15 C14 C19 117.2(8) . . ? C15 C14 C13 121.9(8) . . ? C19 C14 C13 120.7(7) . . ? C14 C15 C16 122.4(9) . . ? C15 C16 C17 121.0(9) . . ? C16 C17 C18 117.9(8) . . ? C16 C17 C20 119.7(9) . . ? C18 C17 C20 122.3(10) . . ? C19 C18 C17 119.3(9) . . ? C14 C19 C18 122.1(9) . . ? C21 C20 C17 125.1(12) . . ? C33 N22 C34 108.1(6) . . ? C33 N22 C23 107.4(6) . . ? C34 N22 C23 111.8(6) . . ? C33 N22 Ni2 109.7(5) . . ? C34 N22 Ni2 110.1(5) . . ? C23 N22 Ni2 109.7(5) . . ? N22 C23 C24 117.0(7) . . ? C25 C24 C23 117.9(6) . . ? N26 C25 C24 114.9(7) . . ? C27 N26 C25 111.6(6) . . ? C27 N26 Ni2 120.8(5) . . ? C25 N26 Ni2 111.7(5) . . ? N26 C27 C28 114.7(7) . . ? C29 C28 C27 114.3(8) . . ? N30 C29 C28 113.8(7) . . ? C31 N30 C29 111.4(7) . . ? C31 N30 Ni2 114.0(5) . . ? C29 N30 Ni2 119.2(5) . . ? N30 C31 C32 113.4(7) . . ? C31 C32 C33 114.3(8) . . ? N22 C33 C32 117.5(7) . . ? N22 C34 C35 117.3(7) . . ? C36 C35 C40 118.0(8) . . ? C36 C35 C34 120.5(7) . . ? C40 C35 C34 121.5(7) . . ? C37 C36 C35 121.4(8) . . ? C36 C37 C38 121.2(8) . . ? C39 C38 C37 118.1(8) . . ? C39 C38 C41 122.6(8) . . ? C37 C38 C41 119.4(8) . . ? C38 C39 C40 121.6(8) . . ? C35 C40 C39 119.6(8) . . ? C42 C41 C38 127.0(9) . . ? N5' Ni1' N9' 96.7(3) . . ? N5' Ni1' N1' 96.2(3) . . ? N9' Ni1' N1' 95.0(2) . . ? N5' Ni1' O1' 87.1(2) . . ? N9' Ni1' O1' 90.4(2) . . ? N1' Ni1' O1' 173.4(2) . . ? N5' Ni1' Cl1' 92.4(2) . . ? N9' Ni1' Cl1' 165.9(2) . . ? N1' Ni1' Cl1' 94.8(2) . . ? O1' Ni1' Cl1' 79.24(14) . . ? N5' Ni1' Cl2' 163.4(2) . . ? N9' Ni1' Cl2' 85.2(2) . . ? N1' Ni1' Cl2' 100.1(2) . . ? O1' Ni1' Cl2' 76.44(14) . . ? Cl1' Ni1' Cl2' 83.05(7) . . ? N30' Ni2' N26' 96.8(3) . . ? N30' Ni2' N22' 94.1(3) . . ? N26' Ni2' N22' 97.0(3) . . ? N30' Ni2' O1' 89.4(2) . . ? N26' Ni2' O1' 87.9(2) . . ? N22' Ni2' O1' 173.6(2) . . ? N30' Ni2' Cl1' 166.9(2) . . ? N26' Ni2' Cl1' 89.4(2) . . ? N22' Ni2' Cl1' 96.7(2) . . ? O1' Ni2' Cl1' 79.25(14) . . ? N30' Ni2' Cl2' 87.8(2) . . ? N26' Ni2' Cl2' 164.2(2) . . ? N22' Ni2' Cl2' 97.7(2) . . ? O1' Ni2' Cl2' 77.00(14) . . ? Cl1' Ni2' Cl2' 83.29(7) . . ? Ni2' O1' Ni1' 92.0(2) . . ? Ni2' O1' Cl3' 111.0(2) . . ? Ni1' O1' Cl3' 111.1(2) . . ? Ni2' O1' Cl4' 114.3(2) . . ? Ni1' O1' Cl4' 113.3(2) . . ? Cl3' O1' Cl4' 113.4(2) . . ? Ni1' Cl1' Ni2' 81.40(7) . . ? Ni2' Cl2' Ni1' 80.36(7) . . ? C13' N1' C2' 108.4(6) . . ? C13' N1' C12' 111.4(6) . . ? C2' N1' C12' 107.7(6) . . ? C13' N1' Ni1' 110.4(4) . . ? C2' N1' Ni1' 110.1(5) . . ? C12' N1' Ni1' 108.8(5) . . ? N1' C2' C3' 117.0(7) . . ? C4' C3' C2' 114.1(7) . . ? N5' C4' C3' 112.8(7) . . ? C4' N5' C6' 110.6(7) . . ? C4' N5' Ni1' 113.7(5) . . ? C6' N5' Ni1' 119.3(6) . . ? N5' C6' C7' 113.1(7) . . ? C8' C7' C6' 112.8(8) . . ? N9' C8' C7' 113.2(7) . . ? C10' N9' C8' 111.3(6) . . ? C10' N9' Ni1' 111.6(5) . . ? C8' N9' Ni1' 120.3(5) . . ? N9' C10' C11' 114.2(7) . . ? C12' C11' C10' 118.2(6) . . ? N1' C12' C11' 117.0(7) . . ? N1' C13' C14' 116.8(7) . . ? C15' C14' C19' 117.5(7) . . ? C15' C14' C13' 121.7(7) . . ? C19' C14' C13' 120.6(7) . . ? C16' C15' C14' 120.8(8) . . ? C17' C16' C15' 121.2(8) . . ? C16' C17' C18' 117.9(8) . . ? C16' C17' C20' 122.9(8) . . ? C18' C17' C20' 119.2(8) . . ? C19' C18' C17' 121.0(8) . . ? C18' C19' C14' 121.4(7) . . ? C21' C20' C17' 126.7(8) . . ? C33' N22' C23' 107.7(6) . . ? C33' N22' C34' 110.7(7) . . ? C23' N22' C34' 109.0(7) . . ? C33' N22' Ni2' 109.4(5) . . ? C23' N22' Ni2' 109.9(6) . . ? C34' N22' Ni2' 110.1(5) . . ? N22' C23' C24' 116.3(8) . . ? C23' C24' C25' 114.9(7) . . ? N26' C25' C24' 114.2(7) . . ? C25' N26' C27' 110.2(6) . . ? C25' N26' Ni2' 112.7(5) . . ? C27' N26' Ni2' 119.2(5) . . ? C28' C27' N26' 112.7(6) . . ? C27' C28' C29' 114.9(7) . . ? N30' C29' C28' 113.2(7) . . ? C31' N30' C29' 111.4(7) . . ? C31' N30' Ni2' 112.8(5) . . ? C29' N30' Ni2' 120.8(5) . . ? N30' C31' C32' 113.7(7) . . ? C31' C32' C33' 118.5(7) . . ? N22' C33' C32' 118.5(7) . . ? N22' C34' C35' 118.1(7) . . ? C40' C35' C36' 117.9(10) . . ? C40' C35' C34' 123.2(11) . . ? C36' C35' C34' 118.9(11) . . ? C37' C36' C35' 120.5(12) . . ? C36' C37' C38' 120.1(13) . . ? C39' C38' C37' 119.3(11) . . ? C39' C38' C41' 121.2(12) . . ? C37' C38' C41' 119.5(12) . . ? C38' C39' C40' 122.1(12) . . ? C35' C40' C39' 120.1(11) . . ? C42' C41' C38' 128.4(14) . . ? Cl52 C50 Cl51 115.2(8) . . ? Cl57 C55 Cl56 110.2(15) . . ? Cl61 C60 Cl62 115.2(12) . . ? Cl87 C65 Cl82 52.0(33) . . ? Cl92 Cl66 Cl91 134.0(53) . . ? Cl92 Cl66 C90 147.5(59) . . ? Cl91 Cl66 C90 76.4(46) . . ? Cl92 Cl66 Cl67 143.0(33) . . ? Cl91 Cl66 Cl67 50.8(29) . . ? C90 Cl66 Cl67 60.8(40) . . ? Cl91 Cl67 C90 53.7(34) . . ? Cl91 Cl67 Cl66 32.5(18) . . ? C90 Cl67 Cl66 41.5(31) . . ? Cl71 C70 Cl72 111.5(15) . . ? Cl71 C70 Cl73 123.0(24) . . ? Cl72 C70 Cl73 102.3(22) . . ? Cl76 C75 Cl77 100.6(38) . . ? C75 Cl76 Cl86 141.9(34) . . ? C75 Cl76 C85 164.2(39) . . ? Cl86 Cl76 C85 32.6(28) . . ? Cl81 C80 C85 132.9(85) . . ? Cl81 C80 Cl87 48.0(53) . . ? C85 C80 Cl87 160.6(64) . . ? Cl81 C80 Cl86 121.6(61) . . ? C85 C80 Cl86 16.8(62) . . ? Cl87 C80 Cl86 166.6(24) . . ? C80 Cl81 Cl87 112.0(66) . . ? C80 Cl81 C85 28.5(56) . . ? Cl87 Cl81 C85 136.5(49) . . ? C80 Cl81 Cl82 146.1(65) . . ? Cl87 Cl81 Cl82 38.1(17) . . ? C85 Cl81 Cl82 174.3(47) . . ? Cl87 Cl82 C65 45.5(26) . . ? Cl87 Cl82 Cl81 40.6(18) . . ? C65 Cl82 Cl81 68.6(27) . . ? C80 C85 Cl86 148.2(100) . . ? C80 C85 Cl81 18.6(35) . . ? Cl86 C85 Cl81 134.8(91) . . ? C80 C85 Cl76 146.1(84) . . ? Cl86 C85 Cl76 65.6(63) . . ? Cl81 C85 Cl76 155.0(65) . . ? C85 Cl86 C90 152.9(83) . . ? C85 Cl86 Cl76 81.8(67) . . ? C90 Cl86 Cl76 102.7(48) . . ? C85 Cl86 C80 15.0(56) . . ? C90 Cl86 C80 146.1(50) . . ? Cl76 Cl86 C80 96.8(30) . . ? C65 Cl87 Cl82 82.5(40) . . ? C65 Cl87 Cl81 112.1(45) . . ? Cl82 Cl87 Cl81 101.3(29) . . ? C65 Cl87 C80 105.1(42) . . ? Cl82 Cl87 C80 119.8(27) . . ? Cl81 Cl87 C80 19.9(18) . . ? Cl66 C90 Cl86 95.4(62) . . ? Cl66 C90 Cl91 43.7(35) . . ? Cl86 C90 Cl91 137.5(75) . . ? Cl66 C90 Cl67 77.7(47) . . ? Cl86 C90 Cl67 114.8(60) . . ? Cl91 C90 Cl67 55.5(37) . . ? Cl66 Cl91 C90 59.9(43) . . ? Cl66 Cl91 Cl67 96.7(38) . . ? C90 Cl91 Cl67 70.8(42) . . ? Cl66 Cl91 Cl92 16.7(19) . . ? C90 Cl91 Cl92 76.2(44) . . ? Cl67 Cl91 Cl92 107.2(32) . . ? Cl66 Cl92 Cl91 29.3(35) . . ? _refine_diff_density_max 0.799 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.116 data_NL9808 _database_code_CSD 170672 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H27 N3 O5 W' _chemical_formula_weight 609.33 _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' '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6898(10) _cell_length_b 10.8424(15) _cell_length_c 13.733(2) _cell_angle_alpha 90.257(10) _cell_angle_beta 97.580(9) _cell_angle_gamma 109.314(9) _cell_volume 1208.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.74 _cell_measurement_theta_max 12.43 _exptl_crystal_description 'platy blocks' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method ? _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 4.815 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.4154 _exptl_absorpt_correction_T_max 0.7772 _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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 13.77 _diffrn_reflns_number 5920 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5551 _reflns_number_observed 4706 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 215 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^)+(0.0377P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5336 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_obs 0.0411 _refine_ls_wR_factor_all 0.0982 _refine_ls_wR_factor_obs 0.0914 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.051 _refine_ls_restrained_S_all 1.038 _refine_ls_restrained_S_obs 1.051 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W W -0.00617(3) 0.03536(2) 0.20344(2) 0.04037(8) Uani 1 d . . N1 N -0.2995(7) 0.3975(5) 0.1627(5) 0.0490(12) Uani 1 d . . C2 C -0.2836(10) 0.2926(7) 0.1035(6) 0.057(2) Uani 1 d . . H2A H -0.1672(10) 0.3070(7) 0.1042(6) 0.068 Uiso 1 calc R . H2B H -0.3295(10) 0.2990(7) 0.0361(6) 0.068 Uiso 1 calc R . C3 C -0.3642(9) 0.1547(7) 0.1334(6) 0.058(2) Uani 1 d . . H3A H -0.4827(9) 0.1330(7) 0.1187(6) 0.069 Uiso 1 calc R . H3B H -0.3332(9) 0.0955(7) 0.0932(6) 0.069 Uiso 1 calc R . C4 C -0.3220(9) 0.1305(6) 0.2401(6) 0.0514(14) Uani 1 d . . H4A H -0.3598(9) 0.1854(6) 0.2803(6) 0.062 Uiso 1 calc R . H4B H -0.3819(9) 0.0401(6) 0.2514(6) 0.062 Uiso 1 calc R . N5 N -0.1422(7) 0.1566(5) 0.2737(4) 0.0414(10) Uani 1 d . . C6 C -0.1166(12) 0.1619(8) 0.3845(5) 0.058(2) Uani 1 d . . H6A H -0.0254(12) 0.1317(8) 0.4073(5) 0.070 Uiso 1 calc R . H6B H -0.2145(12) 0.1028(8) 0.4071(5) 0.070 Uiso 1 calc R . C7 C -0.0812(13) 0.2983(9) 0.4295(5) 0.066(2) Uani 1 d . . H7A H -0.1685(13) 0.3312(9) 0.4032(5) 0.079 Uiso 1 calc R . H7B H -0.0806(13) 0.2937(9) 0.5001(5) 0.079 Uiso 1 calc R . C8 C 0.0819(12) 0.3923(9) 0.4090(7) 0.071(2) Uani 1 d . . H8A H 0.1085(12) 0.4727(9) 0.4489(7) 0.085 Uiso 1 calc R . H8B H 0.1674(12) 0.3544(9) 0.4279(7) 0.085 Uiso 1 calc R . N9 N 0.0797(8) 0.4231(6) 0.3048(5) 0.0561(14) Uani 1 d . . C10 C 0.0229(10) 0.5357(7) 0.2825(8) 0.066(2) Uani 1 d . . H10A H 0.1054(10) 0.6150(7) 0.3133(8) 0.079 Uiso 1 calc R . H10B H -0.0779(10) 0.5234(7) 0.3103(8) 0.079 Uiso 1 calc R . C11 C -0.0082(11) 0.5515(8) 0.1733(8) 0.071(2) Uani 1 d . . H11A H 0.0312(11) 0.4922(8) 0.1389(8) 0.086 Uiso 1 calc R . H11B H 0.0542(11) 0.6401(8) 0.1589(8) 0.086 Uiso 1 calc R . C12 C -0.1901(10) 0.5243(8) 0.1351(8) 0.068(2) Uani 1 d . . H12A H -0.2238(10) 0.5936(8) 0.1604(8) 0.081 Uiso 1 calc R . H12B H -0.2034(10) 0.5265(8) 0.0639(8) 0.081 Uiso 1 calc R . C13 C -0.4699(9) 0.3955(7) 0.1512(6) 0.055(2) Uani 1 d . . H13A H -0.5410(9) 0.3093(7) 0.1650(6) 0.066 Uiso 1 calc R . H13B H -0.5030(9) 0.4119(7) 0.0836(6) 0.066 Uiso 1 calc R . C14 C -0.4921(8) 0.4972(7) 0.2193(5) 0.0488(14) Uani 1 d . . C15 C -0.4513(10) 0.4988(7) 0.3195(6) 0.057(2) Uani 1 d . . H15A H -0.4105(10) 0.4355(7) 0.3468(6) 0.069 Uiso 1 calc R . C16 C -0.4702(10) 0.5937(8) 0.3805(6) 0.059(2) Uani 1 d . . H16A H -0.4450(10) 0.5913(8) 0.4482(6) 0.070 Uiso 1 calc R . C17 C -0.5267(9) 0.6932(7) 0.3418(6) 0.057(2) Uani 1 d . . C18 C -0.5673(10) 0.6900(8) 0.2394(6) 0.058(2) Uani 1 d . . H18A H -0.6064(10) 0.7537(8) 0.2111(6) 0.069 Uiso 1 calc R . C19 C -0.5502(9) 0.5945(8) 0.1801(6) 0.054(2) Uani 1 d . . H19A H -0.5780(9) 0.5946(8) 0.1123(6) 0.065 Uiso 1 calc R . C20 C -0.5451(12) 0.7913(9) 0.4081(7) 0.067(2) Uani 1 d . . H20A H -0.4999(12) 0.7927(9) 0.4736(7) 0.081 Uiso 1 calc R . C21 C -0.6184(14) 0.8779(10) 0.3858(8) 0.078(2) Uani 1 d . . H21A H -0.6658(14) 0.8810(10) 0.3215(8) 0.093 Uiso 1 calc R . H21B H -0.6229(14) 0.9362(10) 0.4344(8) 0.093 Uiso 1 calc R . C22 C 0.1269(10) -0.0546(7) 0.1456(6) 0.056(2) Uani 1 d . . O22 O 0.2074(9) -0.1031(7) 0.1114(5) 0.075(2) Uani 1 d . . C23 C -0.0633(11) -0.1039(7) 0.3040(6) 0.059(2) Uani 1 d . . O23 O -0.0889(12) -0.1808(8) 0.3608(7) 0.099(3) Uani 1 d . . C24 C -0.2073(9) -0.0801(6) 0.1114(5) 0.0496(14) Uani 1 d . . O24 O -0.3121(9) -0.1499(6) 0.0594(5) 0.077(2) Uani 1 d . . C25 C 0.0592(9) 0.1779(7) 0.1053(5) 0.0507(14) Uani 1 d . . O25 O 0.1047(9) 0.2573(6) 0.0527(5) 0.072(2) Uani 1 d . . C26 C 0.2025(10) 0.1316(7) 0.2937(6) 0.055(2) Uani 1 d . . O26 O 0.3280(8) 0.1792(7) 0.3414(5) 0.078(2) Uani 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 W 0.04240(12) 0.03823(11) 0.04192(11) 0.00399(7) 0.00401(8) 0.01609(8) N1 0.043(3) 0.050(3) 0.061(3) 0.014(2) 0.012(2) 0.022(2) C2 0.060(4) 0.066(4) 0.055(4) 0.010(3) 0.013(3) 0.034(3) C3 0.051(4) 0.053(3) 0.071(4) 0.002(3) -0.006(3) 0.025(3) C4 0.048(3) 0.047(3) 0.063(4) 0.013(3) 0.014(3) 0.018(3) N5 0.046(3) 0.041(2) 0.040(2) 0.005(2) 0.007(2) 0.017(2) C6 0.082(5) 0.066(4) 0.037(3) 0.009(3) 0.015(3) 0.034(4) C7 0.089(6) 0.076(5) 0.043(3) -0.004(3) 0.010(3) 0.041(4) C8 0.067(5) 0.077(5) 0.068(5) -0.028(4) -0.022(4) 0.033(4) N9 0.050(3) 0.048(3) 0.073(4) -0.007(3) 0.012(3) 0.019(2) C10 0.045(4) 0.049(3) 0.101(6) -0.013(4) 0.009(4) 0.014(3) C11 0.052(4) 0.061(4) 0.103(7) 0.023(4) 0.030(5) 0.014(3) C12 0.051(4) 0.060(4) 0.098(6) 0.032(4) 0.021(4) 0.021(3) C13 0.046(3) 0.059(3) 0.065(4) 0.002(3) 0.000(3) 0.026(3) C14 0.038(3) 0.052(3) 0.058(4) 0.008(3) 0.001(3) 0.020(2) C15 0.053(4) 0.058(3) 0.063(4) 0.016(3) 0.003(3) 0.024(3) C16 0.055(4) 0.062(4) 0.057(4) 0.014(3) 0.001(3) 0.019(3) C17 0.041(3) 0.059(3) 0.064(4) 0.005(3) 0.001(3) 0.012(3) C18 0.056(4) 0.065(4) 0.060(4) 0.018(3) 0.009(3) 0.030(3) C19 0.048(3) 0.069(4) 0.056(4) 0.013(3) 0.008(3) 0.032(3) C20 0.062(5) 0.071(4) 0.062(4) 0.002(3) 0.003(4) 0.016(4) C21 0.082(6) 0.073(5) 0.082(6) -0.004(4) 0.015(5) 0.030(5) C22 0.058(4) 0.046(3) 0.063(4) 0.002(3) 0.004(3) 0.018(3) O22 0.078(4) 0.080(4) 0.086(4) -0.004(3) 0.020(3) 0.047(3) C23 0.060(4) 0.053(3) 0.064(4) 0.011(3) 0.001(3) 0.020(3) O23 0.102(6) 0.087(5) 0.111(6) 0.059(4) 0.022(5) 0.034(4) C24 0.054(4) 0.043(3) 0.054(3) -0.001(2) -0.002(3) 0.023(3) O24 0.069(4) 0.067(3) 0.083(4) -0.020(3) -0.008(3) 0.016(3) C25 0.052(4) 0.056(3) 0.051(3) 0.008(3) 0.014(3) 0.025(3) O25 0.082(4) 0.070(3) 0.071(4) 0.029(3) 0.031(3) 0.026(3) C26 0.053(4) 0.051(3) 0.058(4) -0.001(3) 0.007(3) 0.015(3) O26 0.052(3) 0.084(4) 0.086(4) -0.005(3) -0.016(3) 0.016(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 W C22 1.975(8) . ? W C26 2.014(7) . ? W C23 2.034(8) . ? W C25 2.042(7) . ? W C24 2.043(7) . ? W N5 2.318(5) . ? N1 C2 1.449(9) . ? N1 C13 1.461(9) . ? N1 C12 1.474(9) . ? C2 C3 1.511(10) . ? C3 C4 1.509(10) . ? C4 N5 1.500(9) . ? N5 C6 1.508(8) . ? C6 C7 1.518(10) . ? C7 C8 1.509(14) . ? C8 N9 1.470(12) . ? N9 C10 1.481(10) . ? C10 C11 1.509(15) . ? C11 C12 1.527(12) . ? C13 C14 1.519(10) . ? C14 C15 1.373(10) . ? C14 C19 1.394(10) . ? C15 C16 1.388(12) . ? C16 C17 1.405(11) . ? C17 C18 1.402(11) . ? C17 C20 1.459(12) . ? C18 C19 1.373(11) . ? C20 C21 1.315(14) . ? C22 O22 1.147(10) . ? C23 O23 1.133(10) . ? C24 O24 1.132(9) . ? C25 O25 1.129(9) . ? C26 O26 1.150(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 C22 W C26 85.8(3) . . ? C22 W C23 90.6(3) . . ? C26 W C23 89.1(3) . . ? C22 W C25 88.9(3) . . ? C26 W C25 88.9(3) . . ? C23 W C25 178.0(3) . . ? C22 W C24 88.3(3) . . ? C26 W C24 173.3(3) . . ? C23 W C24 87.7(3) . . ? C25 W C24 94.3(3) . . ? C22 W N5 175.1(3) . . ? C26 W N5 90.0(3) . . ? C23 W N5 92.0(3) . . ? C25 W N5 88.3(2) . . ? C24 W N5 95.9(2) . . ? C2 N1 C13 111.1(6) . . ? C2 N1 C12 109.6(7) . . ? C13 N1 C12 110.4(6) . . ? N1 C2 C3 116.8(7) . . ? C4 C3 C2 115.6(6) . . ? N5 C4 C3 114.8(6) . . ? C4 N5 C6 107.6(6) . . ? C4 N5 W 119.8(4) . . ? C6 N5 W 113.7(4) . . ? N5 C6 C7 112.8(6) . . ? C8 C7 C6 112.3(7) . . ? N9 C8 C7 112.2(6) . . ? C8 N9 C10 112.4(7) . . ? N9 C10 C11 112.0(7) . . ? C10 C11 C12 112.8(7) . . ? N1 C12 C11 113.8(6) . . ? N1 C13 C14 112.0(6) . . ? C15 C14 C19 118.5(7) . . ? C15 C14 C13 121.6(6) . . ? C19 C14 C13 119.8(6) . . ? C14 C15 C16 120.8(7) . . ? C15 C16 C17 121.3(7) . . ? C18 C17 C16 117.0(8) . . ? C18 C17 C20 123.2(7) . . ? C16 C17 C20 119.8(8) . . ? C19 C18 C17 121.0(7) . . ? C18 C19 C14 121.4(7) . . ? C21 C20 C17 127.3(9) . . ? O22 C22 W 177.9(7) . . ? O23 C23 W 177.3(9) . . ? O24 C24 W 174.9(7) . . ? O25 C25 W 176.0(7) . . ? O26 C26 W 173.7(7) . . ? _refine_diff_density_max 1.206 _refine_diff_density_min -1.017 _refine_diff_density_rms 0.135