# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Parisa Mehrkhodavandi' 'Ira L Kraft' "Brian O'Patrick" 'Christopher J Wallis' _publ_contact_author_name 'Parisa Mehrkhodavandi' _publ_contact_author_email MEHR@CHEM.UBC.CA _publ_section_title ; Electron Rich Bidentate Phosphinimine-Imine Ligands: Synthesis and Reactivity of Late Transition Metal Complexes ; # Attachment 'Mehr_B912783F.cif' data_pm027 _database_code_depnum_ccdc_archive 'CCDC 738462' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H39 Cl6 N2 O5 P W' _chemical_formula_weight 1127.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 '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' Cl Cl 0.1484 0.1585 '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 12.1621(6) _cell_length_b 13.8626(7) _cell_length_c 15.8963(13) _cell_angle_alpha 101.352(4) _cell_angle_beta 102.052(4) _cell_angle_gamma 112.080(3) _cell_volume 2314.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8312 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.55 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 2.924 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.483 _exptl_absorpt_correction_T_max 0.704 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39716 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10320 _reflns_number_gt 9007 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0553P)^2^+13.9829P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10320 _refine_ls_number_parameters 608 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1259 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.058 _refine_ls_shift/su_mean 0.021 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 C1 C -0.1649(5) 0.6028(5) 0.3898(4) 0.0257(11) Uani 1 1 d . A 1 C2 C -0.1993(6) 0.5263(5) 0.4358(4) 0.0370(14) Uani 1 1 d . A 1 H2 H -0.2161 0.4528 0.4081 0.044 Uiso 1 1 calc R A 1 C3 C -0.2098(7) 0.5556(6) 0.5223(5) 0.0408(15) Uani 1 1 d . A 1 H3 H -0.2306 0.5030 0.5537 0.049 Uiso 1 1 calc R A 1 C4 C -0.1900(7) 0.6604(6) 0.5614(4) 0.0412(15) Uani 1 1 d . A 1 H4 H -0.1966 0.6807 0.6202 0.049 Uiso 1 1 calc R A 1 C5 C -0.1606(6) 0.7363(5) 0.5155(4) 0.0328(13) Uani 1 1 d . A 1 H5 H -0.1495 0.8082 0.5422 0.039 Uiso 1 1 calc R A 1 C6 C -0.1467(5) 0.7090(4) 0.4302(4) 0.0243(10) Uani 1 1 d . A 1 C7 C -0.1143(5) 0.7954(4) 0.3850(4) 0.0236(10) Uani 1 1 d . A 1 C8 C -0.1789(5) 0.8679(5) 0.3940(4) 0.0283(11) Uani 1 1 d . A 1 C9 C -0.1172(6) 0.9811(5) 0.4124(4) 0.0339(13) Uani 1 1 d . A 1 H9 H -0.0310 1.0146 0.4179 0.041 Uiso 1 1 calc R A 1 C10 C -0.1811(8) 1.0451(7) 0.4227(5) 0.0489(18) Uani 1 1 d . A 1 H10 H -0.1385 1.1223 0.4369 0.059 Uiso 1 1 calc R A 1 C11 C -0.3072(9) 0.9954(8) 0.4120(6) 0.061(2) Uani 1 1 d . A 1 H11 H -0.3518 1.0386 0.4175 0.073 Uiso 1 1 calc R A 1 C12 C -0.3678(8) 0.8861(8) 0.3938(7) 0.064(2) Uani 1 1 d . A 1 H12 H -0.4547 0.8533 0.3864 0.077 Uiso 1 1 calc R A 1 C13 C -0.3050(6) 0.8209(6) 0.3858(5) 0.0441(16) Uani 1 1 d . A 1 H13 H -0.3484 0.7444 0.3747 0.053 Uiso 1 1 calc R A 1 C14 C -0.0022(5) 0.8860(4) 0.2975(4) 0.0239(10) Uani 1 1 d . A 1 C15 C 0.1129(5) 0.9759(5) 0.3319(4) 0.0288(12) Uani 1 1 d . A 1 H15 H 0.1735 0.9810 0.3833 0.035 Uiso 1 1 calc R A 1 C16 C 0.1402(5) 1.0583(5) 0.2919(4) 0.0308(12) Uani 1 1 d . A 1 H16 H 0.2183 1.1211 0.3172 0.037 Uiso 1 1 calc R A 1 C17 C 0.0538(6) 1.0499(5) 0.2147(4) 0.0318(12) Uani 1 1 d . A 1 C18 C -0.0586(6) 0.9566(5) 0.1765(4) 0.0349(13) Uani 1 1 d . A 1 H18 H -0.1163 0.9480 0.1219 0.042 Uiso 1 1 calc R A 1 C19 C -0.0859(5) 0.8755(5) 0.2190(4) 0.0306(12) Uani 1 1 d . A 1 H19 H -0.1634 0.8121 0.1936 0.037 Uiso 1 1 calc R A 1 C20 C 0.0049(8) 1.1307(6) 0.1015(5) 0.0483(17) Uani 1 1 d . A 1 H20A H -0.0770 1.1198 0.1097 0.058 Uiso 1 1 calc R A 1 H20B H -0.0081 1.0687 0.0511 0.058 Uiso 1 1 calc R A 1 C21 C 0.0638(11) 1.2367(8) 0.0817(7) 0.085(4) Uani 1 1 d . A 1 H21A H 0.0663 1.2962 0.1282 0.128 Uiso 1 1 calc R A 1 H21B H 0.0145 1.2321 0.0225 0.128 Uiso 1 1 calc R A 1 H21C H 0.1489 1.2510 0.0814 0.128 Uiso 1 1 calc R A 1 C22 C 0.0224(6) 0.6925(5) 0.1847(4) 0.0311(12) Uani 1 1 d . A 1 C23 C 0.2193(6) 0.7927(6) 0.3349(5) 0.0370(14) Uani 1 1 d . A 1 C24 C 0.1057(6) 0.5725(6) 0.2749(4) 0.0373(14) Uani 1 1 d . A 1 C25 C 0.1139(5) 0.6836(5) 0.4403(4) 0.0311(12) Uani 1 1 d . A 1 C26 C -0.2414(6) 0.4790(5) 0.1172(4) 0.0326(12) Uani 1 1 d . A 1 C27 C -0.3023(6) 0.5319(6) 0.0731(5) 0.0418(15) Uani 1 1 d . A 1 H27 H -0.3489 0.5620 0.1011 0.050 Uiso 1 1 calc R A 1 C28 C -0.2945(8) 0.5401(8) -0.0106(5) 0.061(2) Uani 1 1 d . A 1 H28 H -0.3362 0.5757 -0.0404 0.073 Uiso 1 1 calc R A 1 C29 C -0.2271(8) 0.4974(8) -0.0511(5) 0.062(2) Uani 1 1 d . A 1 H29 H -0.2219 0.5035 -0.1087 0.074 Uiso 1 1 calc R A 1 C30 C -0.1674(7) 0.4463(7) -0.0088(5) 0.056(2) Uani 1 1 d . A 1 H30 H -0.1206 0.4172 -0.0373 0.067 Uiso 1 1 calc R A 1 C31 C -0.1740(7) 0.4360(6) 0.0755(5) 0.0426(15) Uani 1 1 d . A 1 H31 H -0.1324 0.3997 0.1042 0.051 Uiso 1 1 calc R A 1 C32 C -0.4027(6) 0.4476(5) 0.2337(4) 0.0336(13) Uani 1 1 d . A 1 C33 C -0.4288(6) 0.5371(6) 0.2445(4) 0.0410(15) Uani 1 1 d . A 1 H33 H -0.3682 0.6051 0.2453 0.049 Uiso 1 1 calc R A 1 C34 C -0.5422(7) 0.5291(8) 0.2543(5) 0.054(2) Uani 1 1 d . A 1 H34 H -0.5593 0.5911 0.2607 0.065 Uiso 1 1 calc R A 1 C35 C -0.6291(7) 0.4325(9) 0.2547(6) 0.063(2) Uani 1 1 d . A 1 H35 H -0.7061 0.4276 0.2625 0.076 Uiso 1 1 calc R A 1 C36 C -0.6056(8) 0.3433(9) 0.2440(7) 0.075(3) Uani 1 1 d . A 1 H36 H -0.6678 0.2754 0.2420 0.091 Uiso 1 1 calc R A 1 C37 C -0.4912(7) 0.3506(7) 0.2358(6) 0.055(2) Uani 1 1 d . A 1 H37 H -0.4739 0.2887 0.2317 0.066 Uiso 1 1 calc R A 1 C38 C -0.2342(6) 0.3427(5) 0.2277(4) 0.0336(13) Uani 1 1 d . A 1 C39 C -0.3205(8) 0.2453(6) 0.1635(6) 0.056(2) Uani 1 1 d . A 1 H39 H -0.3867 0.2438 0.1185 0.067 Uiso 1 1 calc R A 1 C40 C -0.3092(10) 0.1483(7) 0.1656(7) 0.070(3) Uani 1 1 d . A 1 H40 H -0.3685 0.0805 0.1225 0.084 Uiso 1 1 calc R A 1 C41 C -0.2124(9) 0.1526(7) 0.2300(6) 0.060(2) Uani 1 1 d . A 1 H41 H -0.2055 0.0870 0.2319 0.072 Uiso 1 1 calc R A 1 C42 C -0.1246(8) 0.2500(7) 0.2923(5) 0.0482(18) Uani 1 1 d . A 1 H42 H -0.0562 0.2518 0.3356 0.058 Uiso 1 1 calc R A 1 C43 C -0.1364(6) 0.3449(6) 0.2916(5) 0.0380(14) Uani 1 1 d . A 1 H43 H -0.0769 0.4122 0.3353 0.046 Uiso 1 1 calc R A 1 N1 N -0.1475(4) 0.5768(4) 0.3041(3) 0.0252(9) Uani 1 1 d . A 1 N2 N -0.0328(4) 0.8034(4) 0.3422(3) 0.0215(9) Uani 1 1 d . A 1 O1 O 0.0884(4) 1.1371(4) 0.1823(3) 0.0442(11) Uani 1 1 d . A 1 O2 O 0.0237(5) 0.7022(4) 0.1149(3) 0.0457(12) Uani 1 1 d . A 1 O3 O 0.3223(5) 0.8572(5) 0.3503(5) 0.0666(17) Uani 1 1 d . A 1 O4 O 0.1393(6) 0.5065(5) 0.2524(4) 0.0603(15) Uani 1 1 d . A 1 O5 O 0.1628(5) 0.6846(5) 0.5109(3) 0.0526(13) Uani 1 1 d . A 1 P1 P -0.24949(14) 0.46689(12) 0.22654(10) 0.0256(3) Uani 1 1 d . A 1 W1 W 0.05020(2) 0.684342(19) 0.312703(15) 0.02502(8) Uani 1 1 d . A 1 C44 C 0.2711(17) -0.0601(8) 0.1439(11) 0.141(7) Uani 1 1 d D . . H44A H 0.3300 -0.0433 0.2040 0.169 Uiso 1 1 calc R . . H44B H 0.1851 -0.0908 0.1477 0.169 Uiso 1 1 calc R . . Cl1 Cl 0.3013(6) 0.0579(4) 0.1133(5) 0.182(2) Uani 1 1 d D . . Cl2 Cl 0.2871(5) -0.1514(4) 0.0669(5) 0.205(3) Uani 1 1 d D . . C45 C 0.509(5) 0.172(3) 0.4411(19) 0.13(2) Uani 0.450(10) 1 d PD B 1 H45A H 0.5850 0.1807 0.4858 0.153 Uiso 0.450(10) 1 calc PR B 1 H45B H 0.4372 0.1079 0.4429 0.153 Uiso 0.450(10) 1 calc PR B 1 Cl3 Cl 0.4853(11) 0.2860(8) 0.4692(10) 0.120(4) Uani 0.450(10) 1 d PD B 1 Cl4 Cl 0.5249(8) 0.1477(6) 0.3356(5) 0.097(3) Uani 0.450(10) 1 d PD B 1 C46 C -0.4923(17) 0.774(2) 0.0638(8) 0.107(9) Uani 0.556(7) 1 d PD C 1 H46A H -0.5115 0.8305 0.0428 0.129 Uiso 0.556(7) 1 calc PR C 1 H46B H -0.5711 0.7065 0.0442 0.129 Uiso 0.556(7) 1 calc PR C 1 Cl5 Cl -0.4349(6) 0.8179(6) 0.1789(4) 0.105(3) Uani 0.556(7) 1 d PD C 1 Cl6 Cl -0.3885(6) 0.7495(7) 0.0154(4) 0.119(3) Uani 0.556(7) 1 d PD C 1 C46B C -0.407(2) 0.8482(14) 0.1364(14) 0.094(11) Uani 0.444(7) 1 d PD C 2 H46C H -0.4566 0.8869 0.1534 0.113 Uiso 0.444(7) 1 calc PR C 2 H46D H -0.3266 0.8802 0.1855 0.113 Uiso 0.444(7) 1 calc PR C 2 Cl5B Cl -0.3788(6) 0.8673(7) 0.0388(6) 0.105(3) Uani 0.444(7) 1 d PD C 2 Cl6B Cl -0.4860(8) 0.7123(7) 0.1259(8) 0.135(4) Uani 0.444(7) 1 d PD C 2 C45B C 0.5640(15) 0.2691(13) 0.4636(16) 0.100(8) Uani 0.550(10) 1 d PD B 2 H45C H 0.6182 0.3056 0.4300 0.120 Uiso 0.550(10) 1 calc PR B 2 H45D H 0.6185 0.2731 0.5212 0.120 Uiso 0.550(10) 1 calc PR B 2 Cl3B Cl 0.4758(7) 0.3361(9) 0.4860(6) 0.109(3) Uani 0.550(10) 1 d PD B 2 Cl4B Cl 0.4730(9) 0.1354(9) 0.4018(10) 0.139(5) Uani 0.550(10) 1 d PD B 2 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 C1 0.027(3) 0.027(3) 0.026(3) 0.011(2) 0.011(2) 0.012(2) C2 0.055(4) 0.029(3) 0.036(3) 0.015(3) 0.025(3) 0.019(3) C3 0.062(4) 0.038(4) 0.037(3) 0.023(3) 0.027(3) 0.024(3) C4 0.059(4) 0.041(4) 0.033(3) 0.016(3) 0.027(3) 0.022(3) C5 0.042(3) 0.029(3) 0.036(3) 0.012(3) 0.023(3) 0.018(3) C6 0.023(2) 0.025(3) 0.029(3) 0.011(2) 0.010(2) 0.011(2) C7 0.022(2) 0.023(3) 0.027(3) 0.008(2) 0.008(2) 0.009(2) C8 0.029(3) 0.032(3) 0.031(3) 0.011(2) 0.012(2) 0.018(2) C9 0.044(3) 0.030(3) 0.039(3) 0.015(3) 0.020(3) 0.022(3) C10 0.074(5) 0.049(4) 0.048(4) 0.020(4) 0.027(4) 0.045(4) C11 0.076(6) 0.069(6) 0.071(6) 0.024(5) 0.031(5) 0.060(5) C12 0.043(4) 0.082(6) 0.081(6) 0.015(5) 0.022(4) 0.044(4) C13 0.033(3) 0.045(4) 0.060(4) 0.011(3) 0.018(3) 0.023(3) C14 0.026(3) 0.027(3) 0.028(3) 0.015(2) 0.015(2) 0.015(2) C15 0.026(3) 0.035(3) 0.031(3) 0.016(3) 0.012(2) 0.015(2) C16 0.021(3) 0.030(3) 0.041(3) 0.014(3) 0.013(2) 0.007(2) C17 0.035(3) 0.031(3) 0.038(3) 0.019(3) 0.016(3) 0.017(2) C18 0.035(3) 0.037(3) 0.034(3) 0.018(3) 0.006(3) 0.016(3) C19 0.025(3) 0.029(3) 0.037(3) 0.015(3) 0.008(2) 0.009(2) C20 0.062(5) 0.046(4) 0.041(4) 0.026(3) 0.011(3) 0.024(4) C21 0.100(8) 0.066(6) 0.075(6) 0.053(6) 0.004(6) 0.016(5) C22 0.032(3) 0.033(3) 0.035(3) 0.010(3) 0.014(2) 0.018(2) C23 0.032(3) 0.051(4) 0.045(4) 0.024(3) 0.017(3) 0.028(3) C24 0.048(4) 0.048(4) 0.034(3) 0.019(3) 0.019(3) 0.033(3) C25 0.031(3) 0.035(3) 0.033(3) 0.010(3) 0.010(2) 0.021(3) C26 0.032(3) 0.032(3) 0.028(3) 0.008(3) 0.011(2) 0.009(2) C27 0.041(4) 0.058(4) 0.036(3) 0.023(3) 0.018(3) 0.024(3) C28 0.065(5) 0.086(6) 0.036(4) 0.029(4) 0.016(4) 0.033(5) C29 0.057(5) 0.083(6) 0.031(4) 0.013(4) 0.021(3) 0.014(4) C30 0.049(4) 0.058(5) 0.046(4) -0.003(4) 0.026(4) 0.014(4) C31 0.049(4) 0.037(4) 0.042(4) 0.006(3) 0.022(3) 0.017(3) C32 0.030(3) 0.041(3) 0.032(3) 0.014(3) 0.011(2) 0.015(3) C33 0.035(3) 0.050(4) 0.033(3) 0.006(3) 0.006(3) 0.019(3) C34 0.050(4) 0.079(6) 0.042(4) 0.011(4) 0.011(3) 0.042(4) C35 0.033(4) 0.102(8) 0.061(5) 0.027(5) 0.023(4) 0.031(4) C36 0.043(5) 0.086(7) 0.094(7) 0.046(6) 0.035(5) 0.008(5) C37 0.040(4) 0.057(5) 0.076(6) 0.035(4) 0.024(4) 0.018(4) C38 0.040(3) 0.028(3) 0.037(3) 0.010(3) 0.011(3) 0.019(3) C39 0.064(5) 0.028(3) 0.060(5) 0.002(3) -0.007(4) 0.022(3) C40 0.098(7) 0.038(4) 0.066(6) 0.002(4) 0.007(5) 0.037(5) C41 0.098(7) 0.045(4) 0.062(5) 0.022(4) 0.030(5) 0.050(5) C42 0.066(5) 0.057(5) 0.048(4) 0.027(4) 0.025(4) 0.045(4) C43 0.046(4) 0.040(4) 0.038(3) 0.017(3) 0.017(3) 0.024(3) N1 0.029(2) 0.025(2) 0.024(2) 0.0108(19) 0.0113(18) 0.0100(19) N2 0.022(2) 0.022(2) 0.025(2) 0.0100(18) 0.0100(17) 0.0111(17) O1 0.044(3) 0.039(3) 0.051(3) 0.030(2) 0.013(2) 0.013(2) O2 0.061(3) 0.057(3) 0.038(3) 0.027(2) 0.029(2) 0.031(3) O3 0.029(3) 0.083(4) 0.096(5) 0.043(4) 0.025(3) 0.022(3) O4 0.087(4) 0.067(4) 0.068(4) 0.028(3) 0.045(3) 0.061(4) O5 0.072(4) 0.067(4) 0.035(3) 0.020(3) 0.010(2) 0.047(3) P1 0.0297(7) 0.0242(7) 0.0266(7) 0.0098(6) 0.0105(6) 0.0136(6) W1 0.02757(12) 0.03010(13) 0.02769(12) 0.01338(9) 0.01305(9) 0.01855(9) C44 0.160(15) 0.068(8) 0.162(15) -0.010(9) 0.091(12) 0.016(9) Cl1 0.170(5) 0.117(4) 0.255(7) 0.055(4) 0.100(5) 0.042(3) Cl2 0.145(4) 0.130(4) 0.293(8) -0.047(4) 0.115(5) 0.042(3) C45 0.16(4) 0.08(2) 0.23(6) 0.10(4) 0.13(4) 0.08(3) Cl3 0.118(7) 0.085(6) 0.213(11) 0.067(7) 0.095(7) 0.068(5) Cl4 0.134(7) 0.116(6) 0.091(5) 0.065(4) 0.046(4) 0.084(5) C46 0.102(17) 0.12(2) 0.057(12) 0.024(13) -0.003(11) 0.018(15) Cl5 0.087(4) 0.134(7) 0.059(3) 0.014(3) 0.008(3) 0.027(4) Cl6 0.078(4) 0.163(8) 0.089(4) 0.018(4) 0.021(3) 0.036(4) C46B 0.054(13) 0.074(16) 0.18(4) 0.07(2) 0.037(18) 0.035(12) Cl5B 0.069(4) 0.109(6) 0.125(6) 0.052(5) 0.011(4) 0.029(4) Cl6B 0.103(6) 0.078(5) 0.189(11) 0.043(6) 0.009(6) 0.021(4) C45B 0.053(11) 0.13(2) 0.13(2) 0.038(17) 0.048(12) 0.038(13) Cl3B 0.081(4) 0.147(8) 0.145(7) 0.086(6) 0.067(4) 0.060(5) Cl4B 0.074(4) 0.156(9) 0.176(10) 0.013(7) 0.014(5) 0.071(6) _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 C1 C2 1.391(8) . ? C1 C6 1.397(8) . ? C1 N1 1.419(7) . ? C2 C3 1.403(9) . ? C2 H2 0.9500 . ? C3 C4 1.368(10) . ? C3 H3 0.9500 . ? C4 C5 1.377(8) . ? C4 H4 0.9500 . ? C5 C6 1.397(8) . ? C5 H5 0.9500 . ? C6 C7 1.486(7) . ? C7 N2 1.298(7) . ? C7 C8 1.493(7) . ? C8 C9 1.398(8) . ? C8 C13 1.388(9) . ? C9 C10 1.391(9) . ? C9 H9 0.9500 . ? C10 C11 1.381(12) . ? C10 H10 0.9500 . ? C11 C12 1.349(13) . ? C11 H11 0.9500 . ? C12 C13 1.389(10) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.383(8) . ? C14 C19 1.378(8) . ? C14 N2 1.438(6) . ? C15 C16 1.383(8) . ? C15 H15 0.9500 . ? C16 C17 1.390(8) . ? C16 H16 0.9500 . ? C17 O1 1.363(7) . ? C17 C18 1.387(9) . ? C18 C19 1.395(8) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 O1 1.426(8) . ? C20 C21 1.503(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 O2 1.145(7) . ? C22 W1 2.025(6) . ? C23 O3 1.171(8) . ? C23 W1 1.944(7) . ? C24 O4 1.159(8) . ? C24 W1 1.952(6) . ? C25 O5 1.150(7) . ? C25 W1 2.018(6) . ? C26 C31 1.380(9) . ? C26 C27 1.404(9) . ? C26 P1 1.798(6) . ? C27 C28 1.378(9) . ? C27 H27 0.9500 . ? C28 C29 1.369(13) . ? C28 H28 0.9500 . ? C29 C30 1.359(13) . ? C29 H29 0.9500 . ? C30 C31 1.391(10) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.383(9) . ? C32 C33 1.379(9) . ? C32 P1 1.812(6) . ? C33 C34 1.385(10) . ? C33 H33 0.9500 . ? C34 C35 1.360(13) . ? C34 H34 0.9500 . ? C35 C36 1.357(14) . ? C35 H35 0.9500 . ? C36 C37 1.392(12) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C43 1.379(9) . ? C38 C39 1.382(10) . ? C38 P1 1.804(6) . ? C39 C40 1.408(10) . ? C39 H39 0.9500 . ? C40 C41 1.363(13) . ? C40 H40 0.9500 . ? C41 C42 1.376(12) . ? C41 H41 0.9500 . ? C42 C43 1.379(9) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? N1 P1 1.606(5) . ? N1 W1 2.260(4) . ? N2 W1 2.260(4) . ? C44 Cl2 1.678(11) . ? C44 Cl1 1.727(12) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 Cl4 1.710(15) . ? C45 Cl3 1.707(15) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 Cl5 1.707(12) . ? C46 Cl6 1.713(14) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C46B Cl5B 1.707(15) . ? C46B Cl6B 1.716(14) . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? C45B Cl4B 1.707(13) . ? C45B Cl3B 1.708(13) . ? C45B H45C 0.9900 . ? C45B H45D 0.9900 . ? 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 C1 C6 118.3(5) . . ? C2 C1 N1 122.4(5) . . ? C6 C1 N1 119.3(5) . . ? C1 C2 C3 121.2(6) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 119.7(6) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.9(6) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 121.0(6) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 119.8(5) . . ? C5 C6 C7 117.9(5) . . ? C1 C6 C7 122.3(5) . . ? N2 C7 C6 118.7(5) . . ? N2 C7 C8 125.2(5) . . ? C6 C7 C8 116.1(5) . . ? C9 C8 C13 118.6(6) . . ? C9 C8 C7 122.9(5) . . ? C13 C8 C7 118.5(5) . . ? C10 C9 C8 120.5(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.3(7) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C12 C11 C10 120.7(7) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 121.0(8) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C8 119.9(7) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? C15 C14 C19 119.3(5) . . ? C15 C14 N2 120.2(5) . . ? C19 C14 N2 120.5(5) . . ? C14 C15 C16 120.3(5) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 120.3(5) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? O1 C17 C16 115.6(5) . . ? O1 C17 C18 124.8(5) . . ? C16 C17 C18 119.6(5) . . ? C19 C18 C17 119.3(6) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C14 121.0(5) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? O1 C20 C21 106.9(7) . . ? O1 C20 H20A 110.3 . . ? C21 C20 H20A 110.3 . . ? O1 C20 H20B 110.4 . . ? C21 C20 H20B 110.4 . . ? H20A C20 H20B 108.6 . . ? O2 C22 W1 170.8(5) . . ? O3 C23 W1 178.2(6) . . ? O4 C24 W1 179.6(6) . . ? O5 C25 W1 172.1(5) . . ? C31 C26 C27 119.1(6) . . ? C31 C26 P1 119.8(5) . . ? C27 C26 P1 121.2(5) . . ? C28 C27 C26 120.0(7) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 120.3(8) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C30 C29 C28 120.1(7) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 121.1(7) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C26 C31 C30 119.5(7) . . ? C26 C31 H31 120.3 . . ? C30 C31 H31 120.3 . . ? C37 C32 C33 118.2(6) . . ? C37 C32 P1 123.7(6) . . ? C33 C32 P1 117.9(5) . . ? C34 C33 C32 120.9(7) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C35 C34 C33 120.2(8) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 120.0(7) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.5(8) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C32 C37 C36 120.1(8) . . ? C32 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C43 C38 C39 120.2(6) . . ? C43 C38 P1 120.3(5) . . ? C39 C38 P1 119.5(5) . . ? C38 C39 C40 119.3(7) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.3 . . ? C41 C40 C39 119.3(8) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 120.4 . . ? C40 C41 C42 121.4(7) . . ? C40 C41 H41 119.3 . . ? C42 C41 H41 119.3 . . ? C41 C42 C43 119.5(7) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C38 C43 C42 120.2(7) . . ? C38 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C1 N1 P1 119.6(4) . . ? C1 N1 W1 109.6(3) . . ? P1 N1 W1 129.2(3) . . ? C7 N2 C14 119.1(4) . . ? C7 N2 W1 126.4(4) . . ? C14 N2 W1 114.0(3) . . ? C17 O1 C20 117.6(5) . . ? N1 P1 C38 117.0(3) . . ? N1 P1 C26 110.1(3) . . ? C38 P1 C26 103.8(3) . . ? N1 P1 C32 108.1(3) . . ? C38 P1 C32 108.4(3) . . ? C26 P1 C32 109.2(3) . . ? C23 W1 C24 87.6(3) . . ? C23 W1 C25 85.1(3) . . ? C24 W1 C25 87.1(2) . . ? C23 W1 C22 84.9(3) . . ? C24 W1 C22 86.6(2) . . ? C25 W1 C22 168.3(2) . . ? C23 W1 N2 96.8(2) . . ? C24 W1 N2 173.5(2) . . ? C25 W1 N2 98.0(2) . . ? C22 W1 N2 89.00(19) . . ? C23 W1 N1 171.3(2) . . ? C24 W1 N1 99.8(2) . . ? C25 W1 N1 90.8(2) . . ? C22 W1 N1 99.9(2) . . ? N2 W1 N1 76.21(16) . . ? Cl2 C44 Cl1 109.4(8) . . ? Cl2 C44 H44A 109.8 . . ? Cl1 C44 H44A 109.8 . . ? Cl2 C44 H44B 109.8 . . ? Cl1 C44 H44B 109.8 . . ? H44A C44 H44B 108.3 . . ? Cl4 C45 Cl3 111.0(12) . . ? Cl4 C45 H45A 109.1 . . ? Cl3 C45 H45A 109.0 . . ? Cl4 C45 H45B 109.7 . . ? Cl3 C45 H45B 109.8 . . ? H45A C45 H45B 108.0 . . ? Cl5 C46 Cl6 111.8(10) . . ? Cl5 C46 H46A 109.2 . . ? Cl6 C46 H46A 109.3 . . ? Cl5 C46 H46B 109.3 . . ? Cl6 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? Cl5B C46B Cl6B 112.0(13) . . ? Cl5B C46B H46C 109.2 . . ? Cl6B C46B H46C 109.2 . . ? Cl5B C46B H46D 109.2 . . ? Cl6B C46B H46D 109.2 . . ? H46C C46B H46D 107.9 . . ? Cl4B C45B Cl3B 111.6(10) . . ? Cl4B C45B H45C 109.2 . . ? Cl3B C45B H45C 109.3 . . ? Cl4B C45B H45D 109.3 . . ? Cl3B C45B H45D 109.3 . . ? H45C C45B H45D 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -3.1(10) . . . . ? N1 C1 C2 C3 176.8(6) . . . . ? C1 C2 C3 C4 2.2(11) . . . . ? C2 C3 C4 C5 0.3(11) . . . . ? C3 C4 C5 C6 -2.0(11) . . . . ? C4 C5 C6 C1 1.1(9) . . . . ? C4 C5 C6 C7 -179.8(6) . . . . ? C2 C1 C6 C5 1.4(8) . . . . ? N1 C1 C6 C5 -178.4(5) . . . . ? C2 C1 C6 C7 -177.7(5) . . . . ? N1 C1 C6 C7 2.4(8) . . . . ? C5 C6 C7 N2 138.8(6) . . . . ? C1 C6 C7 N2 -42.1(8) . . . . ? C5 C6 C7 C8 -40.5(7) . . . . ? C1 C6 C7 C8 138.6(5) . . . . ? N2 C7 C8 C9 -42.5(9) . . . . ? C6 C7 C8 C9 136.7(6) . . . . ? N2 C7 C8 C13 139.0(6) . . . . ? C6 C7 C8 C13 -41.7(8) . . . . ? C13 C8 C9 C10 0.3(10) . . . . ? C7 C8 C9 C10 -178.2(6) . . . . ? C8 C9 C10 C11 -1.8(11) . . . . ? C9 C10 C11 C12 1.5(13) . . . . ? C10 C11 C12 C13 0.3(14) . . . . ? C11 C12 C13 C8 -1.8(13) . . . . ? C9 C8 C13 C12 1.5(11) . . . . ? C7 C8 C13 C12 -180.0(7) . . . . ? C19 C14 C15 C16 4.7(9) . . . . ? N2 C14 C15 C16 -176.5(5) . . . . ? C14 C15 C16 C17 -2.3(9) . . . . ? C15 C16 C17 O1 178.1(6) . . . . ? C15 C16 C17 C18 -2.0(9) . . . . ? O1 C17 C18 C19 -176.4(6) . . . . ? C16 C17 C18 C19 3.6(10) . . . . ? C17 C18 C19 C14 -1.1(10) . . . . ? C15 C14 C19 C18 -3.0(9) . . . . ? N2 C14 C19 C18 178.2(5) . . . . ? C31 C26 C27 C28 0.1(11) . . . . ? P1 C26 C27 C28 180.0(6) . . . . ? C26 C27 C28 C29 -0.3(13) . . . . ? C27 C28 C29 C30 0.1(14) . . . . ? C28 C29 C30 C31 0.3(13) . . . . ? C27 C26 C31 C30 0.3(10) . . . . ? P1 C26 C31 C30 -179.6(6) . . . . ? C29 C30 C31 C26 -0.5(12) . . . . ? C37 C32 C33 C34 -2.1(10) . . . . ? P1 C32 C33 C34 -177.2(5) . . . . ? C32 C33 C34 C35 1.0(11) . . . . ? C33 C34 C35 C36 -1.2(13) . . . . ? C34 C35 C36 C37 2.4(15) . . . . ? C33 C32 C37 C36 3.3(12) . . . . ? P1 C32 C37 C36 178.2(7) . . . . ? C35 C36 C37 C32 -3.5(15) . . . . ? C43 C38 C39 C40 1.6(13) . . . . ? P1 C38 C39 C40 -179.0(7) . . . . ? C38 C39 C40 C41 -0.9(15) . . . . ? C39 C40 C41 C42 -0.9(15) . . . . ? C40 C41 C42 C43 2.0(13) . . . . ? C39 C38 C43 C42 -0.5(11) . . . . ? P1 C38 C43 C42 -179.9(5) . . . . ? C41 C42 C43 C38 -1.3(11) . . . . ? C2 C1 N1 P1 46.3(7) . . . . ? C6 C1 N1 P1 -133.9(5) . . . . ? C2 C1 N1 W1 -120.5(5) . . . . ? C6 C1 N1 W1 59.3(6) . . . . ? C6 C7 N2 C14 179.3(5) . . . . ? C8 C7 N2 C14 -1.5(8) . . . . ? C6 C7 N2 W1 8.5(7) . . . . ? C8 C7 N2 W1 -172.3(4) . . . . ? C15 C14 N2 C7 108.6(6) . . . . ? C19 C14 N2 C7 -72.6(7) . . . . ? C15 C14 N2 W1 -79.5(6) . . . . ? C19 C14 N2 W1 99.2(5) . . . . ? C16 C17 O1 C20 177.8(6) . . . . ? C18 C17 O1 C20 -2.2(10) . . . . ? C21 C20 O1 C17 179.1(7) . . . . ? C1 N1 P1 C38 -84.7(5) . . . . ? W1 N1 P1 C38 79.2(4) . . . . ? C1 N1 P1 C26 157.2(4) . . . . ? W1 N1 P1 C26 -38.9(4) . . . . ? C1 N1 P1 C32 37.9(5) . . . . ? W1 N1 P1 C32 -158.2(3) . . . . ? C43 C38 P1 N1 -1.7(6) . . . . ? C39 C38 P1 N1 178.9(6) . . . . ? C43 C38 P1 C26 119.8(5) . . . . ? C39 C38 P1 C26 -59.6(7) . . . . ? C43 C38 P1 C32 -124.2(5) . . . . ? C39 C38 P1 C32 56.4(7) . . . . ? C31 C26 P1 N1 96.9(6) . . . . ? C27 C26 P1 N1 -83.0(6) . . . . ? C31 C26 P1 C38 -29.1(6) . . . . ? C27 C26 P1 C38 151.1(5) . . . . ? C31 C26 P1 C32 -144.5(5) . . . . ? C27 C26 P1 C32 35.7(6) . . . . ? C37 C32 P1 N1 -130.1(6) . . . . ? C33 C32 P1 N1 44.8(6) . . . . ? C37 C32 P1 C38 -2.4(7) . . . . ? C33 C32 P1 C38 172.5(5) . . . . ? C37 C32 P1 C26 110.1(6) . . . . ? C33 C32 P1 C26 -75.0(6) . . . . ? O3 C23 W1 C24 -71(22) . . . . ? O3 C23 W1 C25 17(22) . . . . ? O3 C23 W1 C22 -158(22) . . . . ? O3 C23 W1 N2 114(22) . . . . ? O3 C23 W1 N1 78(22) . . . . ? O4 C24 W1 C23 -12(93) . . . . ? O4 C24 W1 C25 -97(93) . . . . ? O4 C24 W1 C22 73(93) . . . . ? O4 C24 W1 N2 121(93) . . . . ? O4 C24 W1 N1 173(100) . . . . ? O5 C25 W1 C23 -37(4) . . . . ? O5 C25 W1 C24 51(4) . . . . ? O5 C25 W1 C22 -6(5) . . . . ? O5 C25 W1 N2 -133(4) . . . . ? O5 C25 W1 N1 151(4) . . . . ? O2 C22 W1 C23 23(3) . . . . ? O2 C22 W1 C24 -65(3) . . . . ? O2 C22 W1 C25 -8(4) . . . . ? O2 C22 W1 N2 120(3) . . . . ? O2 C22 W1 N1 -165(3) . . . . ? C7 N2 W1 C23 -140.4(5) . . . . ? C14 N2 W1 C23 48.4(4) . . . . ? C7 N2 W1 C24 87.1(19) . . . . ? C14 N2 W1 C24 -84.1(19) . . . . ? C7 N2 W1 C25 -54.5(5) . . . . ? C14 N2 W1 C25 134.3(4) . . . . ? C7 N2 W1 C22 134.9(5) . . . . ? C14 N2 W1 C22 -36.3(4) . . . . ? C7 N2 W1 N1 34.4(4) . . . . ? C14 N2 W1 N1 -136.8(4) . . . . ? C1 N1 W1 C23 -27.3(15) . . . . ? P1 N1 W1 C23 167.6(13) . . . . ? C1 N1 W1 C24 121.3(4) . . . . ? P1 N1 W1 C24 -43.8(4) . . . . ? C1 N1 W1 C25 34.2(4) . . . . ? P1 N1 W1 C25 -131.0(3) . . . . ? C1 N1 W1 C22 -150.4(4) . . . . ? P1 N1 W1 C22 44.5(4) . . . . ? C1 N1 W1 N2 -63.9(3) . . . . ? P1 N1 W1 N2 131.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 5.100 _refine_diff_density_min -1.421 _refine_diff_density_rms 0.147 #===END data_pm038 _database_code_depnum_ccdc_archive 'CCDC 738463' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H31 Cl2 Co N2 P' _chemical_formula_weight 676.45 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 10.935(4) _cell_length_b 13.014(3) _cell_length_c 13.330(4) _cell_angle_alpha 118.200(10) _cell_angle_beta 94.80(2) _cell_angle_gamma 95.250(10) _cell_volume 1647.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9970 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.74 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31548 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.84 _reflns_number_total 7627 _reflns_number_gt 6505 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0290P)^2^+0.7006P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7627 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.034 _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 C1 C 0.04272(13) -0.21035(12) 0.13502(12) 0.0203(3) Uani 1 1 d . . . C2 C -0.06615(15) -0.20431(14) 0.07665(14) 0.0268(3) Uani 1 1 d . . . H2 H -0.0667 -0.1450 0.0543 0.032 Uiso 1 1 calc R . . C3 C -0.17294(15) -0.28265(15) 0.05067(14) 0.0319(4) Uani 1 1 d . . . H3 H -0.2466 -0.2751 0.0131 0.038 Uiso 1 1 calc R . . C4 C -0.17324(15) -0.37224(15) 0.07908(15) 0.0328(4) Uani 1 1 d . . . H4 H -0.2468 -0.4262 0.0612 0.039 Uiso 1 1 calc R . . C5 C -0.06614(14) -0.38246(13) 0.13347(13) 0.0269(3) Uani 1 1 d . . . H5 H -0.0663 -0.4447 0.1517 0.032 Uiso 1 1 calc R . . C6 C 0.04338(13) -0.30310(12) 0.16260(12) 0.0209(3) Uani 1 1 d . . . C7 C 0.15290(14) -0.32673(12) 0.21606(12) 0.0210(3) Uani 1 1 d . . . C8 C 0.13177(14) -0.38433(13) 0.28833(13) 0.0228(3) Uani 1 1 d . . . C9 C 0.09290(15) -0.32034(14) 0.39379(14) 0.0283(3) Uani 1 1 d . . . H9 H 0.0693 -0.2451 0.4147 0.034 Uiso 1 1 calc R . . C10 C 0.08826(17) -0.36576(17) 0.46913(16) 0.0380(4) Uani 1 1 d . . . H10 H 0.0631 -0.3211 0.5422 0.046 Uiso 1 1 calc R . . C11 C 0.12026(17) -0.47591(18) 0.43768(19) 0.0434(5) Uani 1 1 d . . . H11 H 0.1189 -0.5063 0.4899 0.052 Uiso 1 1 calc R . . C12 C 0.15397(18) -0.54168(17) 0.33130(19) 0.0444(5) Uani 1 1 d . . . H12 H 0.1732 -0.6186 0.3091 0.053 Uiso 1 1 calc R . . C13 C 0.16018(17) -0.49659(14) 0.25584(16) 0.0341(4) Uani 1 1 d . . . H13 H 0.1838 -0.5424 0.1822 0.041 Uiso 1 1 calc R . . C14 C 0.36739(14) -0.33105(13) 0.24934(14) 0.0241(3) Uani 1 1 d . . . C15 C 0.39579(15) -0.28801(14) 0.36636(14) 0.0284(3) Uani 1 1 d . . . H15 H 0.3505 -0.2317 0.4178 0.034 Uiso 1 1 calc R . . C16 C 0.49036(16) -0.32706(15) 0.40857(16) 0.0341(4) Uani 1 1 d . . . H16 H 0.5087 -0.2977 0.4892 0.041 Uiso 1 1 calc R . . C17 C 0.55889(16) -0.40825(15) 0.33541(17) 0.0365(4) Uani 1 1 d . . . C18 C 0.53380(16) -0.44500(16) 0.21912(17) 0.0376(4) Uani 1 1 d . . . H18 H 0.5822 -0.4978 0.1679 0.045 Uiso 1 1 calc R . . C19 C 0.43958(15) -0.40639(15) 0.17580(15) 0.0317(4) Uani 1 1 d . . . H19 H 0.4246 -0.4316 0.0958 0.038 Uiso 1 1 calc R . . C20 C 0.66000(19) -0.45328(18) 0.3818(2) 0.0522(6) Uani 1 1 d . . . H20A H 0.6745 -0.5296 0.3207 0.078 Uiso 1 1 calc R . . H20B H 0.6343 -0.4627 0.4460 0.078 Uiso 1 1 calc R . . H20C H 0.7367 -0.3967 0.4086 0.078 Uiso 1 1 calc R . . C21 C 0.20407(13) 0.05606(13) 0.39452(12) 0.0211(3) Uani 1 1 d . . . C22 C 0.29528(15) 0.00363(14) 0.42444(14) 0.0271(3) Uani 1 1 d . . . H22 H 0.3293 -0.0580 0.3659 0.033 Uiso 1 1 calc R . . C23 C 0.33679(15) 0.04073(15) 0.53892(14) 0.0309(4) Uani 1 1 d . . . H23 H 0.3996 0.0050 0.5587 0.037 Uiso 1 1 calc R . . C24 C 0.28718(15) 0.12942(15) 0.62423(14) 0.0306(4) Uani 1 1 d . . . H24 H 0.3155 0.1544 0.7027 0.037 Uiso 1 1 calc R . . C25 C 0.19668(16) 0.18189(16) 0.59592(14) 0.0343(4) Uani 1 1 d . . . H25 H 0.1624 0.2429 0.6549 0.041 Uiso 1 1 calc R . . C26 C 0.15545(15) 0.14596(15) 0.48160(14) 0.0288(3) Uani 1 1 d . . . H26 H 0.0935 0.1830 0.4625 0.035 Uiso 1 1 calc R . . C27 C 0.01525(14) 0.06935(12) 0.24001(13) 0.0222(3) Uani 1 1 d . . . C28 C -0.08688(14) 0.03997(14) 0.28307(14) 0.0283(3) Uani 1 1 d . . . H28 H -0.0805 -0.0082 0.3185 0.034 Uiso 1 1 calc R . . C29 C -0.19681(16) 0.08106(16) 0.27392(16) 0.0368(4) Uani 1 1 d . . . H29 H -0.2668 0.0595 0.3013 0.044 Uiso 1 1 calc R . . C30 C -0.20537(17) 0.15374(17) 0.22484(17) 0.0418(4) Uani 1 1 d . . . H30 H -0.2812 0.1822 0.2192 0.050 Uiso 1 1 calc R . . C31 C -0.10501(18) 0.18483(16) 0.18441(16) 0.0393(4) Uani 1 1 d . . . H31 H -0.1111 0.2358 0.1522 0.047 Uiso 1 1 calc R . . C32 C 0.00474(16) 0.14210(14) 0.19055(14) 0.0291(3) Uani 1 1 d . . . H32 H 0.0735 0.1624 0.1609 0.035 Uiso 1 1 calc R . . C33 C 0.27035(13) 0.08611(13) 0.20216(13) 0.0222(3) Uani 1 1 d . . . C34 C 0.33543(16) 0.19507(15) 0.28172(16) 0.0343(4) Uani 1 1 d . . . H34 H 0.3243 0.2288 0.3604 0.041 Uiso 1 1 calc R . . C35 C 0.41728(19) 0.25495(18) 0.24589(19) 0.0496(5) Uani 1 1 d . . . H35 H 0.4615 0.3303 0.3002 0.060 Uiso 1 1 calc R . . C36 C 0.43467(18) 0.20601(19) 0.13270(19) 0.0457(5) Uani 1 1 d . . . H36 H 0.4918 0.2469 0.1091 0.055 Uiso 1 1 calc R . . C37 C 0.36963(18) 0.09818(18) 0.05349(17) 0.0416(4) Uani 1 1 d . . . H37 H 0.3813 0.0648 -0.0250 0.050 Uiso 1 1 calc R . . C38 C 0.28701(16) 0.03795(15) 0.08781(15) 0.0321(4) Uani 1 1 d . . . H38 H 0.2417 -0.0365 0.0327 0.039 Uiso 1 1 calc R . . N1 N 0.15073(11) -0.12785(10) 0.16085(11) 0.0207(2) Uani 1 1 d . . . N2 N 0.26391(11) -0.30132(11) 0.19943(11) 0.0220(3) Uani 1 1 d . . . P1 P 0.15757(3) 0.01146(3) 0.24488(3) 0.01833(8) Uani 1 1 d . . . Cl1 Cl 0.48646(4) -0.10431(4) 0.18529(4) 0.03492(10) Uani 1 1 d . . . Cl2 Cl 0.26852(4) -0.33881(3) -0.07535(3) 0.03010(9) Uani 1 1 d . . . Co1 Co 0.298625(18) -0.211395(17) 0.112242(17) 0.02150(6) Uani 1 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 C1 0.0211(7) 0.0197(7) 0.0168(7) 0.0062(6) 0.0032(6) 0.0024(5) C2 0.0286(8) 0.0241(7) 0.0242(8) 0.0095(7) -0.0012(6) 0.0045(6) C3 0.0241(8) 0.0346(9) 0.0292(9) 0.0111(7) -0.0065(7) 0.0020(7) C4 0.0241(8) 0.0329(9) 0.0325(9) 0.0117(8) -0.0029(7) -0.0072(7) C5 0.0274(8) 0.0247(8) 0.0258(8) 0.0108(7) 0.0027(6) -0.0013(6) C6 0.0222(7) 0.0207(7) 0.0169(7) 0.0067(6) 0.0043(6) 0.0031(6) C7 0.0254(7) 0.0182(7) 0.0172(7) 0.0066(6) 0.0044(6) 0.0032(6) C8 0.0218(7) 0.0230(7) 0.0264(8) 0.0143(6) 0.0038(6) 0.0024(6) C9 0.0300(8) 0.0300(8) 0.0305(9) 0.0177(7) 0.0094(7) 0.0083(7) C10 0.0389(10) 0.0505(11) 0.0352(10) 0.0278(9) 0.0134(8) 0.0085(8) C11 0.0385(10) 0.0583(12) 0.0601(13) 0.0489(11) 0.0122(9) 0.0092(9) C12 0.0460(11) 0.0338(9) 0.0698(14) 0.0365(10) 0.0142(10) 0.0108(8) C13 0.0410(10) 0.0228(8) 0.0391(10) 0.0140(7) 0.0126(8) 0.0070(7) C14 0.0227(7) 0.0245(7) 0.0293(8) 0.0164(7) 0.0028(6) 0.0038(6) C15 0.0290(8) 0.0271(8) 0.0290(9) 0.0132(7) 0.0033(7) 0.0062(6) C16 0.0337(9) 0.0328(9) 0.0332(9) 0.0166(8) -0.0066(7) 0.0004(7) C17 0.0313(9) 0.0277(8) 0.0494(11) 0.0201(8) -0.0065(8) 0.0032(7) C18 0.0307(9) 0.0335(9) 0.0443(11) 0.0141(8) 0.0051(8) 0.0132(7) C19 0.0296(9) 0.0358(9) 0.0299(9) 0.0150(8) 0.0057(7) 0.0095(7) C20 0.0445(12) 0.0388(10) 0.0688(15) 0.0256(11) -0.0159(10) 0.0097(9) C21 0.0226(7) 0.0234(7) 0.0187(7) 0.0115(6) 0.0036(6) 0.0016(6) C22 0.0293(8) 0.0285(8) 0.0236(8) 0.0118(7) 0.0045(6) 0.0084(6) C23 0.0303(9) 0.0381(9) 0.0273(9) 0.0184(8) 0.0001(7) 0.0078(7) C24 0.0314(9) 0.0399(9) 0.0194(8) 0.0144(7) 0.0011(7) 0.0018(7) C25 0.0365(9) 0.0398(9) 0.0209(8) 0.0086(7) 0.0072(7) 0.0110(8) C26 0.0287(8) 0.0338(8) 0.0237(8) 0.0127(7) 0.0040(7) 0.0107(7) C27 0.0225(7) 0.0196(7) 0.0212(8) 0.0078(6) -0.0006(6) 0.0032(6) C28 0.0252(8) 0.0269(8) 0.0322(9) 0.0139(7) 0.0033(7) 0.0035(6) C29 0.0231(8) 0.0380(10) 0.0412(11) 0.0127(8) 0.0038(7) 0.0058(7) C30 0.0317(9) 0.0421(10) 0.0435(11) 0.0139(9) -0.0048(8) 0.0164(8) C31 0.0429(10) 0.0380(10) 0.0404(11) 0.0221(9) -0.0042(8) 0.0134(8) C32 0.0323(9) 0.0283(8) 0.0276(9) 0.0149(7) -0.0009(7) 0.0050(7) C33 0.0209(7) 0.0247(7) 0.0249(8) 0.0151(6) 0.0034(6) 0.0031(6) C34 0.0351(9) 0.0327(9) 0.0314(9) 0.0149(8) 0.0019(7) -0.0060(7) C35 0.0439(11) 0.0448(11) 0.0557(13) 0.0262(10) -0.0006(10) -0.0184(9) C36 0.0340(10) 0.0583(12) 0.0624(14) 0.0441(11) 0.0116(9) -0.0011(9) C37 0.0453(11) 0.0538(12) 0.0420(11) 0.0335(10) 0.0195(9) 0.0111(9) C38 0.0378(9) 0.0331(9) 0.0272(9) 0.0164(7) 0.0068(7) 0.0020(7) N1 0.0196(6) 0.0204(6) 0.0215(6) 0.0096(5) 0.0035(5) 0.0025(5) N2 0.0217(6) 0.0236(6) 0.0223(7) 0.0121(5) 0.0041(5) 0.0053(5) P1 0.01891(18) 0.01924(17) 0.01827(19) 0.01025(15) 0.00252(14) 0.00274(14) Cl1 0.02213(19) 0.0509(3) 0.0375(2) 0.0280(2) 0.00029(16) -0.00236(17) Cl2 0.0386(2) 0.02866(19) 0.0240(2) 0.01181(16) 0.00699(16) 0.01267(16) Co1 0.01987(11) 0.02599(11) 0.02211(11) 0.01369(9) 0.00583(8) 0.00514(8) _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 C1 C2 1.396(2) . ? C1 C6 1.419(2) . ? C1 N1 1.4201(18) . ? C2 C3 1.380(2) . ? C2 H2 0.9500 . ? C3 C4 1.385(2) . ? C3 H3 0.9500 . ? C4 C5 1.376(2) . ? C4 H4 0.9500 . ? C5 C6 1.403(2) . ? C5 H5 0.9500 . ? C6 C7 1.473(2) . ? C7 N2 1.2935(19) . ? C7 C8 1.494(2) . ? C8 C9 1.382(2) . ? C8 C13 1.388(2) . ? C9 C10 1.387(2) . ? C9 H9 0.9500 . ? C10 C11 1.379(3) . ? C10 H10 0.9500 . ? C11 C12 1.370(3) . ? C11 H11 0.9500 . ? C12 C13 1.387(2) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.380(2) . ? C14 C19 1.381(2) . ? C14 N2 1.4388(19) . ? C15 C16 1.383(2) . ? C15 H15 0.9500 . ? C16 C17 1.387(3) . ? C16 H16 0.9500 . ? C17 C18 1.382(3) . ? C17 C20 1.515(2) . ? C18 C19 1.385(2) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.390(2) . ? C21 C22 1.391(2) . ? C21 P1 1.8045(16) . ? C22 C23 1.384(2) . ? C22 H22 0.9500 . ? C23 C24 1.377(2) . ? C23 H23 0.9500 . ? C24 C25 1.376(2) . ? C24 H24 0.9500 . ? C25 C26 1.385(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.393(2) . ? C27 C28 1.400(2) . ? C27 P1 1.7993(16) . ? C28 C29 1.379(2) . ? C28 H28 0.9500 . ? C29 C30 1.386(3) . ? C29 H29 0.9500 . ? C30 C31 1.372(3) . ? C30 H30 0.9500 . ? C31 C32 1.380(2) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.382(2) . ? C33 C38 1.384(2) . ? C33 P1 1.7917(15) . ? C34 C35 1.390(2) . ? C34 H34 0.9500 . ? C35 C36 1.371(3) . ? C35 H35 0.9500 . ? C36 C37 1.372(3) . ? C36 H36 0.9500 . ? C37 C38 1.385(2) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? N1 P1 1.6089(13) . ? N1 Co1 2.0122(13) . ? N2 Co1 2.0353(13) . ? Cl1 Co1 2.2289(8) . ? Cl2 Co1 2.2259(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 C2 C1 C6 118.38(13) . . ? C2 C1 N1 119.89(13) . . ? C6 C1 N1 121.67(13) . . ? C3 C2 C1 121.43(15) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C3 C4 120.32(15) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.45(15) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.58(15) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 118.79(14) . . ? C5 C6 C7 116.21(13) . . ? C1 C6 C7 124.95(13) . . ? N2 C7 C6 121.62(13) . . ? N2 C7 C8 120.57(13) . . ? C6 C7 C8 117.79(12) . . ? C9 C8 C13 119.66(14) . . ? C9 C8 C7 118.89(13) . . ? C13 C8 C7 121.23(14) . . ? C8 C9 C10 120.10(15) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.87(17) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C12 C11 C10 120.20(16) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.36(16) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 119.72(17) . . ? C12 C13 H13 120.1 . . ? C8 C13 H13 120.1 . . ? C15 C14 C19 119.58(15) . . ? C15 C14 N2 122.60(14) . . ? C19 C14 N2 117.82(14) . . ? C14 C15 C16 119.91(16) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 121.21(17) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C18 C17 C16 117.95(16) . . ? C18 C17 C20 121.02(18) . . ? C16 C17 C20 121.01(18) . . ? C17 C18 C19 121.34(16) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C14 C19 C18 119.77(16) . . ? C14 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 118.77(14) . . ? C26 C21 P1 121.65(12) . . ? C22 C21 P1 119.50(11) . . ? C23 C22 C21 120.42(15) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.13(15) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.09(15) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.12(16) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.46(15) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C32 C27 C28 119.19(14) . . ? C32 C27 P1 120.04(12) . . ? C28 C27 P1 120.76(12) . . ? C29 C28 C27 119.83(16) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 120.14(17) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C31 C30 C29 120.41(16) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.06(17) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C27 120.33(16) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C34 C33 C38 119.74(14) . . ? C34 C33 P1 120.25(12) . . ? C38 C33 P1 119.90(12) . . ? C33 C34 C35 119.54(17) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 120.44(18) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 120.10(16) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C38 120.08(18) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C33 C38 C37 120.09(17) . . ? C33 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C1 N1 P1 122.90(10) . . ? C1 N1 Co1 110.51(9) . . ? P1 N1 Co1 124.93(7) . . ? C7 N2 C14 119.48(12) . . ? C7 N2 Co1 121.95(10) . . ? C14 N2 Co1 118.47(9) . . ? N1 P1 C33 107.48(7) . . ? N1 P1 C27 115.20(7) . . ? C33 P1 C27 106.80(7) . . ? N1 P1 C21 113.55(7) . . ? C33 P1 C21 107.96(7) . . ? C27 P1 C21 105.46(7) . . ? N1 Co1 N2 91.42(5) . . ? N1 Co1 Cl2 111.36(4) . . ? N2 Co1 Cl2 108.71(4) . . ? N1 Co1 Cl1 117.64(4) . . ? N2 Co1 Cl1 108.06(4) . . ? Cl2 Co1 Cl1 116.35(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 3.0(2) . . . . ? N1 C1 C2 C3 -179.67(14) . . . . ? C1 C2 C3 C4 -2.1(3) . . . . ? C2 C3 C4 C5 0.0(3) . . . . ? C3 C4 C5 C6 1.0(3) . . . . ? C4 C5 C6 C1 0.0(2) . . . . ? C4 C5 C6 C7 -177.47(14) . . . . ? C2 C1 C6 C5 -2.0(2) . . . . ? N1 C1 C6 C5 -179.25(13) . . . . ? C2 C1 C6 C7 175.27(14) . . . . ? N1 C1 C6 C7 -2.0(2) . . . . ? C5 C6 C7 N2 147.43(14) . . . . ? C1 C6 C7 N2 -29.9(2) . . . . ? C5 C6 C7 C8 -31.00(19) . . . . ? C1 C6 C7 C8 151.66(14) . . . . ? N2 C7 C8 C9 110.69(17) . . . . ? C6 C7 C8 C9 -70.86(19) . . . . ? N2 C7 C8 C13 -63.9(2) . . . . ? C6 C7 C8 C13 114.52(17) . . . . ? C13 C8 C9 C10 3.2(2) . . . . ? C7 C8 C9 C10 -171.50(15) . . . . ? C8 C9 C10 C11 -1.2(3) . . . . ? C9 C10 C11 C12 -1.4(3) . . . . ? C10 C11 C12 C13 2.1(3) . . . . ? C11 C12 C13 C8 -0.2(3) . . . . ? C9 C8 C13 C12 -2.5(3) . . . . ? C7 C8 C13 C12 172.07(16) . . . . ? C19 C14 C15 C16 -4.7(2) . . . . ? N2 C14 C15 C16 174.87(14) . . . . ? C14 C15 C16 C17 0.7(2) . . . . ? C15 C16 C17 C18 3.0(3) . . . . ? C15 C16 C17 C20 -178.30(17) . . . . ? C16 C17 C18 C19 -2.8(3) . . . . ? C20 C17 C18 C19 178.45(17) . . . . ? C15 C14 C19 C18 4.8(2) . . . . ? N2 C14 C19 C18 -174.75(15) . . . . ? C17 C18 C19 C14 -1.0(3) . . . . ? C26 C21 C22 C23 -0.1(2) . . . . ? P1 C21 C22 C23 176.70(12) . . . . ? C21 C22 C23 C24 0.5(2) . . . . ? C22 C23 C24 C25 -0.4(3) . . . . ? C23 C24 C25 C26 -0.2(3) . . . . ? C24 C25 C26 C21 0.6(3) . . . . ? C22 C21 C26 C25 -0.4(2) . . . . ? P1 C21 C26 C25 -177.20(13) . . . . ? C32 C27 C28 C29 1.4(2) . . . . ? P1 C27 C28 C29 -177.14(13) . . . . ? C27 C28 C29 C30 -1.6(3) . . . . ? C28 C29 C30 C31 0.4(3) . . . . ? C29 C30 C31 C32 1.1(3) . . . . ? C30 C31 C32 C27 -1.4(3) . . . . ? C28 C27 C32 C31 0.2(2) . . . . ? P1 C27 C32 C31 178.66(13) . . . . ? C38 C33 C34 C35 -0.2(3) . . . . ? P1 C33 C34 C35 -176.24(15) . . . . ? C33 C34 C35 C36 -0.7(3) . . . . ? C34 C35 C36 C37 1.1(3) . . . . ? C35 C36 C37 C38 -0.6(3) . . . . ? C34 C33 C38 C37 0.7(3) . . . . ? P1 C33 C38 C37 176.78(14) . . . . ? C36 C37 C38 C33 -0.3(3) . . . . ? C2 C1 N1 P1 63.55(18) . . . . ? C6 C1 N1 P1 -119.24(14) . . . . ? C2 C1 N1 Co1 -130.49(12) . . . . ? C6 C1 N1 Co1 46.72(16) . . . . ? C6 C7 N2 C14 -177.19(13) . . . . ? C8 C7 N2 C14 1.2(2) . . . . ? C6 C7 N2 Co1 6.50(19) . . . . ? C8 C7 N2 Co1 -175.11(10) . . . . ? C15 C14 N2 C7 -59.4(2) . . . . ? C19 C14 N2 C7 120.14(16) . . . . ? C15 C14 N2 Co1 117.03(14) . . . . ? C19 C14 N2 Co1 -63.42(16) . . . . ? C1 N1 P1 C33 -152.89(11) . . . . ? Co1 N1 P1 C33 43.20(10) . . . . ? C1 N1 P1 C27 -33.99(14) . . . . ? Co1 N1 P1 C27 162.10(8) . . . . ? C1 N1 P1 C21 87.78(13) . . . . ? Co1 N1 P1 C21 -76.13(10) . . . . ? C34 C33 P1 N1 -151.83(13) . . . . ? C38 C33 P1 N1 32.10(15) . . . . ? C34 C33 P1 C27 84.01(15) . . . . ? C38 C33 P1 C27 -92.05(14) . . . . ? C34 C33 P1 C21 -28.98(15) . . . . ? C38 C33 P1 C21 154.95(13) . . . . ? C32 C27 P1 N1 -109.37(13) . . . . ? C28 C27 P1 N1 69.11(14) . . . . ? C32 C27 P1 C33 9.90(15) . . . . ? C28 C27 P1 C33 -171.62(12) . . . . ? C32 C27 P1 C21 124.58(13) . . . . ? C28 C27 P1 C21 -56.93(14) . . . . ? C26 C21 P1 N1 -144.53(12) . . . . ? C22 C21 P1 N1 38.72(14) . . . . ? C26 C21 P1 C33 96.42(14) . . . . ? C22 C21 P1 C33 -80.34(13) . . . . ? C26 C21 P1 C27 -17.47(14) . . . . ? C22 C21 P1 C27 165.77(12) . . . . ? C1 N1 Co1 N2 -51.92(10) . . . . ? P1 N1 Co1 N2 113.69(9) . . . . ? C1 N1 Co1 Cl2 58.83(10) . . . . ? P1 N1 Co1 Cl2 -135.56(7) . . . . ? C1 N1 Co1 Cl1 -163.20(8) . . . . ? P1 N1 Co1 Cl1 2.41(10) . . . . ? C7 N2 Co1 N1 28.69(12) . . . . ? C14 N2 Co1 N1 -147.66(11) . . . . ? C7 N2 Co1 Cl2 -84.46(12) . . . . ? C14 N2 Co1 Cl2 99.19(11) . . . . ? C7 N2 Co1 Cl1 148.43(11) . . . . ? C14 N2 Co1 Cl1 -27.91(11) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.358 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.047 #===END data_pm037 _database_code_depnum_ccdc_archive 'CCDC 738464' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H37 Br2 Cl2 N2 Ni P' _chemical_formula_weight 878.13 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' P P 0.1023 0.0942 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P na21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 21.2062(12) _cell_length_b 13.2498(7) _cell_length_c 13.7667(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3868.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9950 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.85 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 2.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.642 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40528 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.90 _reflns_number_total 9177 _reflns_number_gt 7601 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0149P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(4) _refine_ls_number_reflns 9177 _refine_ls_number_parameters 445 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0517 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_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_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 C1 C 0.22362(11) 1.02234(16) 0.14613(19) 0.0209(5) Uani 1 1 d . . . C2 C 0.25246(13) 1.09625(17) 0.20387(18) 0.0250(6) Uani 1 1 d . . . H2 H 0.2415 1.1007 0.2706 0.030 Uiso 1 1 calc R . . C3 C 0.29610(13) 1.16234(18) 0.16685(17) 0.0276(6) Uani 1 1 d . . . H3 H 0.3147 1.2117 0.2079 0.033 Uiso 1 1 calc R . . C4 C 0.31292(13) 1.15734(19) 0.07058(18) 0.0303(6) Uani 1 1 d . . . H4 H 0.3438 1.2020 0.0452 0.036 Uiso 1 1 calc R . . C5 C 0.28438(13) 1.08652(19) 0.01088(18) 0.0281(6) Uani 1 1 d . . . H5 H 0.2961 1.0832 -0.0556 0.034 Uiso 1 1 calc R . . C6 C 0.23875(12) 1.01996(17) 0.04634(17) 0.0204(5) Uani 1 1 d . . . C7 C 0.20980(12) 0.94848(17) -0.02395(16) 0.0200(5) Uani 1 1 d . . . C8 C 0.24990(13) 0.91463(18) -0.10752(18) 0.0267(6) Uani 1 1 d . . . C9 C 0.23165(14) 0.9262(2) -0.20336(19) 0.0340(6) Uani 1 1 d . . . H9 H 0.1928 0.9582 -0.2186 0.041 Uiso 1 1 calc R . . C10 C 0.27065(17) 0.8908(2) -0.2775(2) 0.0463(8) Uani 1 1 d . . . H10 H 0.2582 0.8994 -0.3432 0.056 Uiso 1 1 calc R . . C11 C 0.32650(16) 0.8439(2) -0.2570(2) 0.0472(9) Uani 1 1 d . . . H11 H 0.3524 0.8193 -0.3081 0.057 Uiso 1 1 calc R . . C12 C 0.34483(16) 0.8326(2) -0.1624(2) 0.0459(8) Uani 1 1 d . . . H12 H 0.3835 0.7999 -0.1478 0.055 Uiso 1 1 calc R . . C13 C 0.30712(14) 0.8689(2) -0.0875(2) 0.0350(7) Uani 1 1 d . . . H13 H 0.3207 0.8622 -0.0221 0.042 Uiso 1 1 calc R . . C14 C 0.12350(12) 0.84899(18) -0.07939(17) 0.0235(5) Uani 1 1 d . . . C15 C 0.13667(13) 0.74619(18) -0.07100(17) 0.0281(6) Uani 1 1 d . . . C16 C 0.18333(16) 0.7072(2) 0.0021(2) 0.0418(8) Uani 1 1 d . . . H16A H 0.1758 0.6351 0.0132 0.063 Uiso 1 1 calc R . . H16B H 0.1784 0.7441 0.0633 0.063 Uiso 1 1 calc R . . H16C H 0.2262 0.7169 -0.0227 0.063 Uiso 1 1 calc R . . C17 C 0.10508(14) 0.6796(2) -0.13231(19) 0.0354(7) Uani 1 1 d . . . H17 H 0.1141 0.6095 -0.1281 0.042 Uiso 1 1 calc R . . C18 C 0.06079(15) 0.7127(2) -0.1994(2) 0.0396(7) Uani 1 1 d . . . C19 C 0.02740(17) 0.6382(3) -0.2651(3) 0.0618(10) Uani 1 1 d . . . H19A H -0.0114 0.6688 -0.2900 0.093 Uiso 1 1 calc R . . H19B H 0.0170 0.5772 -0.2282 0.093 Uiso 1 1 calc R . . H19C H 0.0550 0.6205 -0.3195 0.093 Uiso 1 1 calc R . . C20 C 0.04858(14) 0.8147(2) -0.2046(2) 0.0386(7) Uani 1 1 d . . . H20 H 0.0186 0.8383 -0.2506 0.046 Uiso 1 1 calc R . . C21 C 0.07852(13) 0.8841(2) -0.14498(19) 0.0309(6) Uani 1 1 d . . . C22 C 0.06349(15) 0.9957(2) -0.1535(2) 0.0445(8) Uani 1 1 d . . . H22A H 0.0403 1.0177 -0.0957 0.067 Uiso 1 1 calc R . . H22B H 0.0377 1.0073 -0.2114 0.067 Uiso 1 1 calc R . . H22C H 0.1028 1.0341 -0.1588 0.067 Uiso 1 1 calc R . . C23 C 0.17267(13) 0.99428(19) 0.39037(17) 0.0263(6) Uani 1 1 d . . . C24 C 0.11771(15) 1.0501(2) 0.3787(2) 0.0393(7) Uani 1 1 d . . . H24 H 0.0956 1.0474 0.3187 0.047 Uiso 1 1 calc R . . C25 C 0.09493(16) 1.1093(2) 0.4532(2) 0.0463(8) Uani 1 1 d . . . H25 H 0.0567 1.1458 0.4454 0.056 Uiso 1 1 calc R . . C26 C 0.12800(16) 1.1152(2) 0.5390(2) 0.0470(8) Uani 1 1 d . . . H26 H 0.1123 1.1554 0.5908 0.056 Uiso 1 1 calc R . . C27 C 0.18285(16) 1.0640(2) 0.5502(2) 0.0474(8) Uani 1 1 d . . . H27 H 0.2058 1.0702 0.6092 0.057 Uiso 1 1 calc R . . C28 C 0.20603(14) 1.0023(2) 0.47635(19) 0.0352(7) Uani 1 1 d . . . H28 H 0.2443 0.9662 0.4850 0.042 Uiso 1 1 calc R . . C29 C 0.27212(12) 0.85987(17) 0.31191(18) 0.0247(6) Uani 1 1 d . . . C30 C 0.28417(14) 0.8010(2) 0.3942(2) 0.0370(7) Uani 1 1 d . . . H30 H 0.2522 0.7927 0.4419 0.044 Uiso 1 1 calc R . . C31 C 0.34168(16) 0.7552(2) 0.4069(3) 0.0488(9) Uani 1 1 d . . . H31 H 0.3493 0.7162 0.4636 0.059 Uiso 1 1 calc R . . C32 C 0.38817(15) 0.7653(2) 0.3383(3) 0.0483(9) Uani 1 1 d . . . H32 H 0.4278 0.7334 0.3474 0.058 Uiso 1 1 calc R . . C33 C 0.37710(15) 0.8218(2) 0.2565(2) 0.0443(8) Uani 1 1 d . . . H33 H 0.4091 0.8286 0.2087 0.053 Uiso 1 1 calc R . . C34 C 0.31963(13) 0.8690(2) 0.2434(2) 0.0346(7) Uani 1 1 d . . . H34 H 0.3126 0.9082 0.1866 0.042 Uiso 1 1 calc R . . C35 C 0.14399(13) 0.79836(19) 0.31375(17) 0.0264(6) Uani 1 1 d . . . C36 C 0.09289(14) 0.7992(2) 0.3779(2) 0.0370(7) Uani 1 1 d . . . H36 H 0.0819 0.8594 0.4114 0.044 Uiso 1 1 calc R . . C37 C 0.05855(17) 0.7119(3) 0.3922(2) 0.0548(10) Uani 1 1 d . . . H37 H 0.0242 0.7120 0.4366 0.066 Uiso 1 1 calc R . . C38 C 0.07325(18) 0.6255(3) 0.3436(3) 0.0585(11) Uani 1 1 d . . . H38 H 0.0484 0.5667 0.3528 0.070 Uiso 1 1 calc R . . C39 C 0.12400(18) 0.6228(2) 0.2809(3) 0.0523(10) Uani 1 1 d . . . H39 H 0.1344 0.5622 0.2477 0.063 Uiso 1 1 calc R . . C40 C 0.15997(15) 0.7099(2) 0.2667(2) 0.0364(7) Uani 1 1 d . . . H40 H 0.1955 0.7082 0.2247 0.044 Uiso 1 1 calc R . . C41 C 0.02856(16) 0.5642(2) 0.0686(2) 0.0494(8) Uani 1 1 d . . . H41A H 0.0274 0.5640 0.1405 0.059 Uiso 1 1 calc R . . H41B H 0.0502 0.6266 0.0475 0.059 Uiso 1 1 calc R . . N1 N 0.18166(10) 0.94936(14) 0.18534(14) 0.0213(4) Uani 1 1 d . . . N2 N 0.15246(10) 0.91925(14) -0.01232(14) 0.0222(5) Uani 1 1 d . . . P1 P 0.19316(3) 0.90706(5) 0.29423(5) 0.02142(14) Uani 1 1 d . . . Ni1 Ni 0.102212(14) 0.94611(2) 0.10756(2) 0.02383(7) Uani 1 1 d . . . Br1 Br 0.071912(14) 1.119363(19) 0.10117(2) 0.03801(7) Uani 1 1 d . . . Br2 Br 0.025484(13) 0.822733(19) 0.13748(2) 0.03417(7) Uani 1 1 d . . . Cl1 Cl 0.07198(5) 0.45869(6) 0.02814(7) 0.0584(2) Uani 1 1 d . . . Cl2 Cl -0.04742(5) 0.56495(8) 0.02494(8) 0.0782(3) Uani 1 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 C1 0.0152(12) 0.0232(11) 0.0244(12) 0.0043(10) -0.0012(11) 0.0013(9) C2 0.0295(16) 0.0281(13) 0.0173(12) 0.0005(10) -0.0009(11) -0.0001(11) C3 0.0302(16) 0.0256(13) 0.0271(15) 0.0009(10) -0.0041(11) -0.0037(11) C4 0.0285(17) 0.0313(13) 0.0310(15) 0.0081(11) 0.0008(12) -0.0116(12) C5 0.0283(16) 0.0354(14) 0.0207(13) 0.0061(11) 0.0023(12) -0.0009(12) C6 0.0214(14) 0.0231(12) 0.0167(12) 0.0026(10) -0.0029(10) 0.0014(10) C7 0.0230(15) 0.0215(12) 0.0154(12) 0.0058(9) -0.0019(10) 0.0014(10) C8 0.0278(16) 0.0282(13) 0.0242(14) -0.0009(11) 0.0041(11) -0.0026(12) C9 0.0362(17) 0.0427(15) 0.0230(14) -0.0022(12) 0.0016(13) -0.0056(12) C10 0.057(2) 0.058(2) 0.0235(16) -0.0081(14) 0.0076(15) -0.0092(17) C11 0.059(2) 0.0397(17) 0.0426(19) -0.0142(14) 0.0247(17) -0.0077(16) C12 0.042(2) 0.0379(16) 0.058(2) 0.0015(14) 0.0190(17) 0.0056(15) C13 0.0365(19) 0.0382(15) 0.0304(15) 0.0031(12) 0.0063(13) 0.0043(13) C14 0.0215(15) 0.0325(13) 0.0166(12) 0.0001(10) -0.0003(10) -0.0043(11) C15 0.0324(17) 0.0298(14) 0.0222(13) 0.0021(11) 0.0046(12) -0.0018(12) C16 0.056(2) 0.0319(15) 0.0377(17) -0.0003(13) -0.0066(15) 0.0075(15) C17 0.0425(19) 0.0325(15) 0.0311(15) -0.0074(12) 0.0091(14) -0.0072(13) C18 0.0327(19) 0.0563(19) 0.0297(16) -0.0149(15) 0.0005(14) -0.0123(14) C19 0.057(3) 0.071(2) 0.057(2) -0.0259(18) -0.0069(19) -0.026(2) C20 0.0270(17) 0.0584(19) 0.0304(15) -0.0042(14) -0.0078(13) -0.0035(14) C21 0.0268(16) 0.0406(15) 0.0254(14) 0.0013(12) -0.0030(12) 0.0019(12) C22 0.047(2) 0.0447(17) 0.0415(17) 0.0014(14) -0.0170(16) 0.0125(15) C23 0.0267(15) 0.0322(13) 0.0200(13) 0.0052(11) 0.0049(11) -0.0031(11) C24 0.043(2) 0.0481(17) 0.0265(15) -0.0009(13) 0.0030(13) 0.0088(15) C25 0.046(2) 0.0562(19) 0.0367(17) 0.0014(15) 0.0117(16) 0.0133(16) C26 0.045(2) 0.057(2) 0.0387(18) -0.0159(15) 0.0159(16) -0.0001(16) C27 0.043(2) 0.071(2) 0.0278(16) -0.0111(15) -0.0001(14) -0.0074(17) C28 0.0321(17) 0.0466(16) 0.0269(15) -0.0034(13) 0.0025(12) -0.0035(14) C29 0.0242(15) 0.0242(12) 0.0256(14) 0.0014(10) -0.0052(11) -0.0034(10) C30 0.0354(19) 0.0361(15) 0.0394(17) 0.0146(13) -0.0093(14) -0.0040(13) C31 0.045(2) 0.0389(17) 0.063(2) 0.0153(15) -0.0263(18) 0.0019(15) C32 0.0279(19) 0.0319(16) 0.085(3) 0.0048(16) -0.0177(18) 0.0026(13) C33 0.0291(18) 0.0405(17) 0.063(2) 0.0006(16) 0.0016(15) 0.0032(14) C34 0.0280(17) 0.0356(15) 0.0402(17) 0.0044(12) 0.0001(14) 0.0051(13) C35 0.0245(15) 0.0320(14) 0.0227(13) 0.0139(11) -0.0084(11) -0.0074(11) C36 0.0282(17) 0.0528(18) 0.0300(15) 0.0137(13) -0.0082(13) -0.0100(14) C37 0.036(2) 0.082(3) 0.046(2) 0.035(2) -0.0132(16) -0.0288(19) C38 0.058(3) 0.058(2) 0.060(2) 0.0367(19) -0.033(2) -0.037(2) C39 0.068(3) 0.0344(16) 0.054(2) 0.0183(15) -0.037(2) -0.0126(16) C40 0.0402(19) 0.0330(15) 0.0361(16) 0.0108(13) -0.0147(14) -0.0075(13) C41 0.052(2) 0.0520(18) 0.0438(18) -0.0062(15) 0.0044(16) -0.0087(16) N1 0.0232(13) 0.0241(10) 0.0165(10) 0.0029(8) 0.0012(9) -0.0045(9) N2 0.0218(13) 0.0258(11) 0.0189(10) 0.0037(8) -0.0026(9) 0.0025(9) P1 0.0206(4) 0.0249(3) 0.0187(3) 0.0046(3) -0.0008(3) -0.0026(3) Ni1 0.01953(17) 0.03139(16) 0.02058(14) 0.00238(14) 0.00045(14) -0.00186(12) Br1 0.03984(17) 0.03688(13) 0.03732(14) 0.00768(13) 0.01223(14) 0.00950(12) Br2 0.02754(15) 0.04023(14) 0.03475(13) 0.00885(12) -0.00527(12) -0.00976(12) Cl1 0.0603(6) 0.0461(5) 0.0689(6) 0.0065(4) 0.0065(5) 0.0006(4) Cl2 0.0598(7) 0.0949(7) 0.0799(7) -0.0390(6) -0.0271(6) 0.0122(5) _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 C1 C2 1.402(3) . ? C1 C6 1.411(3) . ? C1 N1 1.420(3) . ? C2 C3 1.372(4) . ? C2 H2 0.9500 . ? C3 C4 1.374(4) . ? C3 H3 0.9500 . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C5 C6 1.397(3) . ? C5 H5 0.9500 . ? C6 C7 1.487(3) . ? C7 N2 1.286(3) . ? C7 C8 1.499(3) . ? C8 C9 1.383(4) . ? C8 C13 1.384(4) . ? C9 C10 1.395(4) . ? C9 H9 0.9500 . ? C10 C11 1.367(5) . ? C10 H10 0.9500 . ? C11 C12 1.367(4) . ? C11 H11 0.9500 . ? C12 C13 1.390(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C21 1.393(4) . ? C14 C15 1.395(3) . ? C14 N2 1.448(3) . ? C15 C17 1.392(4) . ? C15 C16 1.502(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.388(4) . ? C17 H17 0.9500 . ? C18 C20 1.379(4) . ? C18 C19 1.514(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.386(4) . ? C20 H20 0.9500 . ? C21 C22 1.517(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C28 1.383(4) . ? C23 C24 1.390(4) . ? C23 P1 1.810(3) . ? C24 C25 1.380(4) . ? C24 H24 0.9500 . ? C25 C26 1.376(4) . ? C25 H25 0.9500 . ? C26 C27 1.356(4) . ? C26 H26 0.9500 . ? C27 C28 1.394(4) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.385(4) . ? C29 C30 1.399(3) . ? C29 P1 1.804(3) . ? C30 C31 1.374(4) . ? C30 H30 0.9500 . ? C31 C32 1.372(5) . ? C31 H31 0.9500 . ? C32 C33 1.372(4) . ? C32 H32 0.9500 . ? C33 C34 1.381(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.382(4) . ? C35 C36 1.398(4) . ? C35 P1 1.798(2) . ? C36 C37 1.382(4) . ? C36 H36 0.9500 . ? C37 C38 1.362(5) . ? C37 H37 0.9500 . ? C38 C39 1.379(5) . ? C38 H38 0.9500 . ? C39 C40 1.397(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 Cl2 1.720(3) . ? C41 Cl1 1.764(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? N1 P1 1.619(2) . ? N1 Ni1 1.997(2) . ? N2 Ni1 1.997(2) . ? Ni1 Br2 2.3429(4) . ? Ni1 Br1 2.3854(4) . ? 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 C1 C6 117.9(2) . . ? C2 C1 N1 122.2(2) . . ? C6 C1 N1 119.8(2) . . ? C3 C2 C1 122.0(2) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C2 C3 C4 120.2(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C3 C4 C5 119.4(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 121.5(2) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 118.9(2) . . ? C5 C6 C7 117.4(2) . . ? C1 C6 C7 123.6(2) . . ? N2 C7 C6 120.1(2) . . ? N2 C7 C8 122.8(2) . . ? C6 C7 C8 117.1(2) . . ? C9 C8 C13 118.9(3) . . ? C9 C8 C7 122.7(2) . . ? C13 C8 C7 118.4(2) . . ? C8 C9 C10 119.6(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 121.0(3) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 119.5(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C8 C13 C12 120.5(3) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C21 C14 C15 121.1(2) . . ? C21 C14 N2 119.3(2) . . ? C15 C14 N2 119.3(2) . . ? C17 C15 C14 118.2(2) . . ? C17 C15 C16 120.3(2) . . ? C14 C15 C16 121.5(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C15 122.0(3) . . ? C18 C17 H17 119.0 . . ? C15 C17 H17 119.0 . . ? C20 C18 C17 118.1(3) . . ? C20 C18 C19 121.3(3) . . ? C17 C18 C19 120.6(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 C21 122.2(3) . . ? C18 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C20 C21 C14 118.4(2) . . ? C20 C21 C22 120.3(2) . . ? C14 C21 C22 121.3(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 119.1(3) . . ? C28 C23 P1 123.5(2) . . ? C24 C23 P1 117.1(2) . . ? C25 C24 C23 120.7(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C26 C25 C24 119.5(3) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C27 C26 C25 120.5(3) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 120.8(3) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C23 C28 C27 119.3(3) . . ? C23 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C34 C29 C30 117.9(3) . . ? C34 C29 P1 123.6(2) . . ? C30 C29 P1 118.2(2) . . ? C31 C30 C29 120.8(3) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 120.5(3) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 119.7(3) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C34 120.3(3) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C29 120.9(3) . . ? C33 C34 H34 119.6 . . ? C29 C34 H34 119.6 . . ? C40 C35 C36 119.5(3) . . ? C40 C35 P1 117.9(2) . . ? C36 C35 P1 122.5(2) . . ? C37 C36 C35 119.5(3) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C38 C37 C36 120.8(3) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 120.6(3) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C40 119.4(3) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C35 C40 C39 120.1(3) . . ? C35 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? Cl2 C41 Cl1 112.52(17) . . ? Cl2 C41 H41A 109.1 . . ? Cl1 C41 H41A 109.1 . . ? Cl2 C41 H41B 109.1 . . ? Cl1 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C1 N1 P1 119.55(16) . . ? C1 N1 Ni1 109.84(14) . . ? P1 N1 Ni1 128.03(12) . . ? C7 N2 C14 121.0(2) . . ? C7 N2 Ni1 123.63(17) . . ? C14 N2 Ni1 114.54(16) . . ? N1 P1 C35 109.17(11) . . ? N1 P1 C29 112.62(11) . . ? C35 P1 C29 103.91(12) . . ? N1 P1 C23 114.83(11) . . ? C35 P1 C23 105.24(12) . . ? C29 P1 C23 110.21(12) . . ? N2 Ni1 N1 89.81(9) . . ? N2 Ni1 Br2 113.06(6) . . ? N1 Ni1 Br2 120.45(5) . . ? N2 Ni1 Br1 106.55(6) . . ? N1 Ni1 Br1 103.08(5) . . ? Br2 Ni1 Br1 119.396(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -2.6(4) . . . . ? N1 C1 C2 C3 175.6(2) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C2 C3 C4 C5 1.4(4) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C4 C5 C6 C1 -2.8(4) . . . . ? C4 C5 C6 C7 178.5(2) . . . . ? C2 C1 C6 C5 4.0(3) . . . . ? N1 C1 C6 C5 -174.3(2) . . . . ? C2 C1 C6 C7 -177.5(2) . . . . ? N1 C1 C6 C7 4.3(4) . . . . ? C5 C6 C7 N2 -148.9(2) . . . . ? C1 C6 C7 N2 32.6(3) . . . . ? C5 C6 C7 C8 30.3(3) . . . . ? C1 C6 C7 C8 -148.3(2) . . . . ? N2 C7 C8 C9 55.1(3) . . . . ? C6 C7 C8 C9 -124.0(3) . . . . ? N2 C7 C8 C13 -124.1(3) . . . . ? C6 C7 C8 C13 56.7(3) . . . . ? C13 C8 C9 C10 0.8(4) . . . . ? C7 C8 C9 C10 -178.5(3) . . . . ? C8 C9 C10 C11 0.5(4) . . . . ? C9 C10 C11 C12 -0.8(5) . . . . ? C10 C11 C12 C13 -0.2(5) . . . . ? C9 C8 C13 C12 -1.8(4) . . . . ? C7 C8 C13 C12 177.5(2) . . . . ? C11 C12 C13 C8 1.6(4) . . . . ? C21 C14 C15 C17 2.1(4) . . . . ? N2 C14 C15 C17 175.9(2) . . . . ? C21 C14 C15 C16 -177.7(3) . . . . ? N2 C14 C15 C16 -3.9(4) . . . . ? C14 C15 C17 C18 -1.0(4) . . . . ? C16 C15 C17 C18 178.7(3) . . . . ? C15 C17 C18 C20 0.3(4) . . . . ? C15 C17 C18 C19 179.9(3) . . . . ? C17 C18 C20 C21 -0.6(4) . . . . ? C19 C18 C20 C21 179.9(3) . . . . ? C18 C20 C21 C14 1.6(4) . . . . ? C18 C20 C21 C22 180.0(3) . . . . ? C15 C14 C21 C20 -2.3(4) . . . . ? N2 C14 C21 C20 -176.2(2) . . . . ? C15 C14 C21 C22 179.2(3) . . . . ? N2 C14 C21 C22 5.4(4) . . . . ? C28 C23 C24 C25 -2.9(4) . . . . ? P1 C23 C24 C25 172.4(2) . . . . ? C23 C24 C25 C26 1.8(5) . . . . ? C24 C25 C26 C27 0.6(5) . . . . ? C25 C26 C27 C28 -1.7(5) . . . . ? C24 C23 C28 C27 1.8(4) . . . . ? P1 C23 C28 C27 -173.3(2) . . . . ? C26 C27 C28 C23 0.5(4) . . . . ? C34 C29 C30 C31 0.9(4) . . . . ? P1 C29 C30 C31 173.8(2) . . . . ? C29 C30 C31 C32 -0.8(4) . . . . ? C30 C31 C32 C33 0.1(5) . . . . ? C31 C32 C33 C34 0.5(5) . . . . ? C32 C33 C34 C29 -0.3(4) . . . . ? C30 C29 C34 C33 -0.4(4) . . . . ? P1 C29 C34 C33 -172.9(2) . . . . ? C40 C35 C36 C37 -0.9(4) . . . . ? P1 C35 C36 C37 -177.5(2) . . . . ? C35 C36 C37 C38 -1.0(4) . . . . ? C36 C37 C38 C39 1.9(5) . . . . ? C37 C38 C39 C40 -0.8(5) . . . . ? C36 C35 C40 C39 2.1(4) . . . . ? P1 C35 C40 C39 178.8(2) . . . . ? C38 C39 C40 C35 -1.2(4) . . . . ? C2 C1 N1 P1 -33.7(3) . . . . ? C6 C1 N1 P1 144.48(19) . . . . ? C2 C1 N1 Ni1 129.5(2) . . . . ? C6 C1 N1 Ni1 -52.3(2) . . . . ? C6 C7 N2 C14 -179.4(2) . . . . ? C8 C7 N2 C14 1.4(3) . . . . ? C6 C7 N2 Ni1 -10.3(3) . . . . ? C8 C7 N2 Ni1 170.54(17) . . . . ? C21 C14 N2 C7 -106.6(3) . . . . ? C15 C14 N2 C7 79.4(3) . . . . ? C21 C14 N2 Ni1 83.3(2) . . . . ? C15 C14 N2 Ni1 -90.6(2) . . . . ? C1 N1 P1 C35 -167.82(18) . . . . ? Ni1 N1 P1 C35 32.32(18) . . . . ? C1 N1 P1 C29 -52.9(2) . . . . ? Ni1 N1 P1 C29 147.20(13) . . . . ? C1 N1 P1 C23 74.3(2) . . . . ? Ni1 N1 P1 C23 -85.56(16) . . . . ? C40 C35 P1 N1 72.1(2) . . . . ? C36 C35 P1 N1 -111.3(2) . . . . ? C40 C35 P1 C29 -48.3(2) . . . . ? C36 C35 P1 C29 128.4(2) . . . . ? C40 C35 P1 C23 -164.15(19) . . . . ? C36 C35 P1 C23 12.5(2) . . . . ? C34 C29 P1 N1 6.7(3) . . . . ? C30 C29 P1 N1 -165.79(19) . . . . ? C34 C29 P1 C35 124.7(2) . . . . ? C30 C29 P1 C35 -47.8(2) . . . . ? C34 C29 P1 C23 -123.0(2) . . . . ? C30 C29 P1 C23 64.5(2) . . . . ? C28 C23 P1 N1 -143.8(2) . . . . ? C24 C23 P1 N1 41.0(2) . . . . ? C28 C23 P1 C35 96.1(2) . . . . ? C24 C23 P1 C35 -79.1(2) . . . . ? C28 C23 P1 C29 -15.4(3) . . . . ? C24 C23 P1 C29 169.5(2) . . . . ? C7 N2 Ni1 N1 -27.92(19) . . . . ? C14 N2 Ni1 N1 141.83(16) . . . . ? C7 N2 Ni1 Br2 -151.25(17) . . . . ? C14 N2 Ni1 Br2 18.50(17) . . . . ? C7 N2 Ni1 Br1 75.67(19) . . . . ? C14 N2 Ni1 Br1 -114.58(15) . . . . ? C1 N1 Ni1 N2 56.01(15) . . . . ? P1 N1 Ni1 N2 -142.56(14) . . . . ? C1 N1 Ni1 Br2 172.90(12) . . . . ? P1 N1 Ni1 Br2 -25.67(16) . . . . ? C1 N1 Ni1 Br1 -50.95(15) . . . . ? P1 N1 Ni1 Br1 110.48(13) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.433 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.059 #===END data_pm050_0m _database_code_depnum_ccdc_archive 'CCDC 738465' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H33 Cl4 N2 P Zn' _chemical_formula_weight 767.81 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 12.3640(9) _cell_length_b 17.4916(14) _cell_length_c 16.9571(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.222(3) _cell_angle_gamma 90.00 _cell_volume 3619.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9954 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.82 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.762 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41267 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.01 _reflns_number_total 8741 _reflns_number_gt 7001 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0346P)^2^+1.8083P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8741 _refine_ls_number_parameters 438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_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_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 C1 C 0.18415(13) 0.11741(10) 0.53748(10) 0.0199(3) Uani 1 1 d . . . C2 C 0.16663(15) 0.04000(11) 0.55128(11) 0.0274(4) Uani 1 1 d . . . H2 H 0.1662 0.0232 0.6045 0.033 Uiso 1 1 calc R . . C3 C 0.14998(16) -0.01278(11) 0.49007(12) 0.0316(4) Uani 1 1 d . . . H3 H 0.1381 -0.0650 0.5013 0.038 Uiso 1 1 calc R . . C4 C 0.15072(16) 0.01079(11) 0.41220(12) 0.0314(4) Uani 1 1 d . . . H4 H 0.1397 -0.0251 0.3697 0.038 Uiso 1 1 calc R . . C5 C 0.16755(14) 0.08687(11) 0.39705(11) 0.0256(4) Uani 1 1 d . . . H5 H 0.1688 0.1025 0.3435 0.031 Uiso 1 1 calc R . . C6 C 0.18292(13) 0.14200(10) 0.45765(10) 0.0207(3) Uani 1 1 d . . . C7 C 0.19518(13) 0.22253(10) 0.43334(10) 0.0194(3) Uani 1 1 d . . . C8 C 0.23815(15) 0.23579(10) 0.35692(10) 0.0232(4) Uani 1 1 d . . . C9 C 0.34527(16) 0.21575(11) 0.35093(12) 0.0286(4) Uani 1 1 d . . . H9 H 0.3894 0.1902 0.3940 0.034 Uiso 1 1 calc R . . C10 C 0.38771(19) 0.23297(12) 0.28246(14) 0.0387(5) Uani 1 1 d . . . H10 H 0.4616 0.2205 0.2791 0.046 Uiso 1 1 calc R . . C11 C 0.3234(2) 0.26804(14) 0.21943(13) 0.0457(6) Uani 1 1 d . . . H11 H 0.3530 0.2798 0.1725 0.055 Uiso 1 1 calc R . . C12 C 0.2164(2) 0.28623(14) 0.22380(13) 0.0457(6) Uani 1 1 d . . . H12 H 0.1719 0.3094 0.1794 0.055 Uiso 1 1 calc R . . C13 C 0.17290(17) 0.27090(12) 0.29272(11) 0.0335(4) Uani 1 1 d . . . H13 H 0.0993 0.2843 0.2960 0.040 Uiso 1 1 calc R . . C14 C 0.17845(14) 0.35679(10) 0.44967(10) 0.0218(4) Uani 1 1 d . . . C15 C 0.27854(15) 0.38732(11) 0.43903(11) 0.0257(4) Uani 1 1 d . . . H15 H 0.3430 0.3569 0.4489 0.031 Uiso 1 1 calc R . . C16 C 0.28420(16) 0.46223(11) 0.41392(12) 0.0297(4) Uani 1 1 d . . . H16 H 0.3530 0.4827 0.4065 0.036 Uiso 1 1 calc R . . C17 C 0.19111(17) 0.50834(11) 0.39931(11) 0.0303(4) Uani 1 1 d . . . C18 C 0.1982(2) 0.58850(13) 0.36896(15) 0.0476(6) Uani 1 1 d . . . H18A H 0.1798 0.5887 0.3106 0.071 Uiso 1 1 calc R . . H18B H 0.2728 0.6079 0.3849 0.071 Uiso 1 1 calc R . . H18C H 0.1466 0.6212 0.3916 0.071 Uiso 1 1 calc R . . C19 C 0.09306(16) 0.47815(11) 0.41369(12) 0.0311(4) Uani 1 1 d . . . H19 H 0.0292 0.5092 0.4059 0.037 Uiso 1 1 calc R . . C20 C 0.08617(15) 0.40322(11) 0.43942(11) 0.0285(4) Uani 1 1 d . . . H20 H 0.0183 0.3837 0.4500 0.034 Uiso 1 1 calc R . . C21 C 0.39021(14) 0.08707(10) 0.66598(10) 0.0234(4) Uani 1 1 d . . . C22 C 0.45935(17) 0.11023(12) 0.61390(14) 0.0386(5) Uani 1 1 d . . . H22 H 0.4501 0.1592 0.5896 0.046 Uiso 1 1 calc R . . C23 C 0.54200(19) 0.06236(14) 0.59705(16) 0.0508(6) Uani 1 1 d . . . H23 H 0.5887 0.0783 0.5608 0.061 Uiso 1 1 calc R . . C24 C 0.55634(18) -0.00820(14) 0.63275(16) 0.0470(6) Uani 1 1 d . . . H24 H 0.6141 -0.0405 0.6221 0.056 Uiso 1 1 calc R . . C25 C 0.48785(19) -0.03213(13) 0.68357(14) 0.0443(6) Uani 1 1 d . . . H25 H 0.4980 -0.0811 0.7079 0.053 Uiso 1 1 calc R . . C26 C 0.40364(17) 0.01476(12) 0.69967(12) 0.0342(5) Uani 1 1 d . . . H26 H 0.3550 -0.0027 0.7339 0.041 Uiso 1 1 calc R . . C27 C 0.21451(14) 0.11340(10) 0.76010(10) 0.0231(4) Uani 1 1 d . . . C28 C 0.27226(17) 0.08320(12) 0.83087(11) 0.0309(4) Uani 1 1 d . . . H28 H 0.3501 0.0826 0.8393 0.037 Uiso 1 1 calc R . . C29 C 0.21609(19) 0.05420(13) 0.88864(12) 0.0383(5) Uani 1 1 d . . . H29 H 0.2553 0.0324 0.9361 0.046 Uiso 1 1 calc R . . C30 C 0.10291(19) 0.05706(12) 0.87728(12) 0.0375(5) Uani 1 1 d . . . H30 H 0.0646 0.0380 0.9174 0.045 Uiso 1 1 calc R . . C31 C 0.04526(17) 0.08740(12) 0.80813(13) 0.0363(5) Uani 1 1 d . . . H31 H -0.0325 0.0894 0.8009 0.044 Uiso 1 1 calc R . . C32 C 0.10034(15) 0.11502(11) 0.74901(12) 0.0287(4) Uani 1 1 d . . . H32 H 0.0603 0.1350 0.7009 0.034 Uiso 1 1 calc R . . C33 C 0.34318(14) 0.24197(10) 0.71765(10) 0.0218(3) Uani 1 1 d . . . C34 C 0.35967(16) 0.26350(12) 0.79753(11) 0.0294(4) Uani 1 1 d . . . H34 H 0.3408 0.2294 0.8368 0.035 Uiso 1 1 calc R . . C35 C 0.40356(18) 0.33455(13) 0.82001(12) 0.0381(5) Uani 1 1 d . . . H35 H 0.4146 0.3491 0.8747 0.046 Uiso 1 1 calc R . . C36 C 0.43117(17) 0.38415(12) 0.76354(13) 0.0374(5) Uani 1 1 d . . . H36 H 0.4597 0.4333 0.7791 0.045 Uiso 1 1 calc R . . C37 C 0.41748(17) 0.36251(12) 0.68402(13) 0.0349(5) Uani 1 1 d . . . H37 H 0.4386 0.3963 0.6453 0.042 Uiso 1 1 calc R . . C38 C 0.37324(15) 0.29214(11) 0.66086(11) 0.0278(4) Uani 1 1 d . . . H38 H 0.3632 0.2777 0.6062 0.033 Uiso 1 1 calc R . . C39 C 0.6593(3) 0.26130(19) 0.4582(3) 0.0609(11) Uani 0.866(7) 1 d P A 1 H39A H 0.6512 0.2941 0.4100 0.073 Uiso 0.866(7) 1 calc PR A 1 H39B H 0.7341 0.2691 0.4881 0.073 Uiso 0.866(7) 1 calc PR A 1 N1 N 0.20280(11) 0.17090(8) 0.60063(8) 0.0202(3) Uani 1 1 d . . . N2 N 0.16663(11) 0.27901(8) 0.47459(8) 0.0197(3) Uani 1 1 d . . . P1 P 0.28293(3) 0.15220(3) 0.68275(3) 0.01909(9) Uani 1 1 d . . . Cl1 Cl -0.06886(4) 0.21767(3) 0.53216(3) 0.03474(12) Uani 1 1 d . . . Cl2 Cl 0.10835(4) 0.35662(3) 0.66172(3) 0.03660(12) Uani 1 1 d . . . Cl3 Cl 0.56149(16) 0.28975(16) 0.51922(13) 0.0540(4) Uani 0.866(7) 1 d P A 1 Cl4 Cl 0.64414(7) 0.16707(13) 0.42929(8) 0.0629(4) Uani 0.866(7) 1 d P A 1 Zn1 Zn 0.100734(16) 0.261204(12) 0.577125(11) 0.02046(6) Uani 1 1 d . . . Cl4B Cl 0.6437(5) 0.2011(8) 0.4137(5) 0.055(2) Uiso 0.134(7) 1 d P A 2 C39B C 0.6732(12) 0.2594(9) 0.4996(9) 0.019(3) Uiso 0.134(7) 1 d P A 2 H39C H 0.7041 0.2269 0.5455 0.023 Uiso 0.134(7) 1 calc PR A 2 H39D H 0.7302 0.2969 0.4910 0.023 Uiso 0.134(7) 1 calc PR A 2 Cl3B Cl 0.5639(14) 0.3075(9) 0.5234(10) 0.058(4) Uiso 0.134(7) 1 d P A 2 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 C1 0.0178(8) 0.0192(9) 0.0224(8) -0.0001(7) 0.0019(6) 0.0028(6) C2 0.0313(9) 0.0219(10) 0.0281(10) 0.0037(7) 0.0022(8) 0.0002(7) C3 0.0336(10) 0.0190(10) 0.0407(11) 0.0000(8) 0.0012(8) -0.0022(8) C4 0.0346(10) 0.0241(10) 0.0341(11) -0.0093(8) 0.0017(8) -0.0011(8) C5 0.0263(9) 0.0276(10) 0.0225(9) -0.0037(7) 0.0031(7) 0.0023(7) C6 0.0176(8) 0.0209(9) 0.0232(9) 0.0000(7) 0.0022(6) 0.0033(6) C7 0.0171(7) 0.0228(9) 0.0178(8) 0.0012(6) 0.0009(6) 0.0025(6) C8 0.0287(9) 0.0219(9) 0.0197(8) -0.0030(7) 0.0064(7) -0.0019(7) C9 0.0318(10) 0.0247(10) 0.0317(10) -0.0034(8) 0.0123(8) 0.0010(8) C10 0.0460(12) 0.0309(11) 0.0456(13) -0.0112(10) 0.0269(10) -0.0063(9) C11 0.0707(17) 0.0415(13) 0.0313(11) -0.0061(10) 0.0273(11) -0.0140(12) C12 0.0670(16) 0.0483(14) 0.0212(10) 0.0050(9) 0.0050(10) -0.0051(12) C13 0.0376(11) 0.0388(12) 0.0236(9) 0.0022(8) 0.0032(8) 0.0012(9) C14 0.0276(9) 0.0207(9) 0.0175(8) 0.0019(7) 0.0044(7) 0.0040(7) C15 0.0263(9) 0.0245(10) 0.0266(9) 0.0004(7) 0.0052(7) 0.0045(7) C16 0.0309(10) 0.0266(10) 0.0324(10) -0.0015(8) 0.0070(8) -0.0032(8) C17 0.0395(11) 0.0212(10) 0.0287(10) 0.0007(8) 0.0004(8) -0.0003(8) C18 0.0528(14) 0.0267(12) 0.0598(15) 0.0120(10) -0.0015(12) -0.0036(10) C19 0.0305(10) 0.0233(10) 0.0370(11) 0.0033(8) -0.0019(8) 0.0077(8) C20 0.0254(9) 0.0271(10) 0.0333(10) 0.0033(8) 0.0055(8) 0.0042(7) C21 0.0226(8) 0.0231(9) 0.0239(9) 0.0001(7) 0.0019(7) 0.0033(7) C22 0.0417(12) 0.0247(11) 0.0555(14) 0.0054(9) 0.0266(10) 0.0029(9) C23 0.0451(13) 0.0388(14) 0.0777(18) -0.0013(12) 0.0380(13) 0.0017(10) C24 0.0372(12) 0.0368(13) 0.0701(17) -0.0067(12) 0.0177(11) 0.0127(10) C25 0.0493(13) 0.0346(13) 0.0497(14) 0.0078(10) 0.0103(11) 0.0185(10) C26 0.0391(11) 0.0304(11) 0.0347(11) 0.0089(9) 0.0109(9) 0.0096(9) C27 0.0272(9) 0.0222(9) 0.0214(9) 0.0015(7) 0.0079(7) 0.0001(7) C28 0.0349(10) 0.0343(11) 0.0235(9) 0.0047(8) 0.0049(8) 0.0023(8) C29 0.0558(14) 0.0370(12) 0.0231(10) 0.0072(8) 0.0093(9) 0.0012(10) C30 0.0541(13) 0.0306(11) 0.0330(11) 0.0012(9) 0.0229(10) -0.0080(10) C31 0.0342(10) 0.0325(11) 0.0462(12) -0.0017(9) 0.0186(9) -0.0048(9) C32 0.0283(9) 0.0270(10) 0.0316(10) 0.0033(8) 0.0074(8) -0.0001(8) C33 0.0204(8) 0.0211(9) 0.0233(9) -0.0003(7) 0.0017(7) 0.0025(7) C34 0.0335(10) 0.0320(11) 0.0227(9) 0.0008(8) 0.0046(8) -0.0010(8) C35 0.0448(12) 0.0387(12) 0.0290(11) -0.0094(9) 0.0002(9) -0.0036(10) C36 0.0391(11) 0.0256(11) 0.0448(12) -0.0067(9) -0.0010(9) -0.0056(9) C37 0.0391(11) 0.0260(11) 0.0398(12) 0.0043(9) 0.0067(9) -0.0041(8) C38 0.0333(10) 0.0256(10) 0.0249(9) 0.0008(7) 0.0061(8) -0.0003(8) C39 0.0387(16) 0.0467(19) 0.101(4) 0.020(2) 0.023(2) 0.0044(13) N1 0.0247(7) 0.0181(7) 0.0174(7) 0.0014(5) 0.0023(6) 0.0030(6) N2 0.0206(7) 0.0185(8) 0.0204(7) 0.0018(6) 0.0044(6) 0.0039(5) P1 0.0207(2) 0.0191(2) 0.0176(2) 0.00272(16) 0.00351(16) 0.00139(16) Cl1 0.0246(2) 0.0452(3) 0.0353(3) -0.0113(2) 0.00715(19) -0.0039(2) Cl2 0.0363(3) 0.0350(3) 0.0378(3) -0.0157(2) 0.0040(2) 0.0079(2) Cl3 0.0446(6) 0.0611(11) 0.0565(7) 0.0048(8) 0.0088(4) -0.0111(7) Cl4 0.0478(5) 0.0569(9) 0.0829(6) 0.0080(6) 0.0076(4) 0.0006(4) Zn1 0.02278(10) 0.02034(11) 0.01901(10) 0.00025(8) 0.00568(7) 0.00393(8) _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 C1 C2 1.397(3) . ? C1 N1 1.413(2) . ? C1 C6 1.418(2) . ? C2 C3 1.380(3) . ? C2 H2 0.9500 . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.377(3) . ? C4 H4 0.9500 . ? C5 C6 1.400(2) . ? C5 H5 0.9500 . ? C6 C7 1.482(2) . ? C7 N2 1.292(2) . ? C7 C8 1.495(2) . ? C8 C9 1.389(3) . ? C8 C13 1.390(3) . ? C9 C10 1.382(3) . ? C9 H9 0.9500 . ? C10 C11 1.370(3) . ? C10 H10 0.9500 . ? C11 C12 1.375(4) . ? C11 H11 0.9500 . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.386(2) . ? C14 C20 1.388(2) . ? C14 N2 1.439(2) . ? C15 C16 1.383(3) . ? C15 H15 0.9500 . ? C16 C17 1.395(3) . ? C16 H16 0.9500 . ? C17 C19 1.379(3) . ? C17 C18 1.501(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.388(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.384(3) . ? C21 C26 1.387(3) . ? C21 P1 1.8052(18) . ? C22 C23 1.386(3) . ? C22 H22 0.9500 . ? C23 C24 1.374(3) . ? C23 H23 0.9500 . ? C24 C25 1.367(3) . ? C24 H24 0.9500 . ? C25 C26 1.387(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.394(2) . ? C27 C28 1.398(3) . ? C27 P1 1.8035(18) . ? C28 C29 1.385(3) . ? C28 H28 0.9500 . ? C29 C30 1.383(3) . ? C29 H29 0.9500 . ? C30 C31 1.377(3) . ? C30 H30 0.9500 . ? C31 C32 1.386(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.389(3) . ? C33 C38 1.396(3) . ? C33 P1 1.7971(18) . ? C34 C35 1.385(3) . ? C34 H34 0.9500 . ? C35 C36 1.375(3) . ? C35 H35 0.9500 . ? C36 C37 1.385(3) . ? C36 H36 0.9500 . ? C37 C38 1.378(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 Cl4 1.721(4) . ? C39 Cl3 1.785(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? N1 P1 1.6079(14) . ? N1 Zn1 2.0212(14) . ? N2 Zn1 2.0587(14) . ? Cl1 Zn1 2.2462(5) . ? Cl2 Zn1 2.1929(5) . ? Cl4B C39B 1.768(15) . ? C39B Cl3B 1.69(2) . ? C39B H39C 0.9900 . ? C39B H39D 0.9900 . ? 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 C1 N1 121.72(16) . . ? C2 C1 C6 118.40(16) . . ? N1 C1 C6 119.87(15) . . ? C3 C2 C1 122.08(18) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C2 C3 C4 119.68(18) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 119.33(18) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 122.37(17) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 118.12(16) . . ? C5 C6 C7 117.28(16) . . ? C1 C6 C7 124.59(15) . . ? N2 C7 C6 121.82(15) . . ? N2 C7 C8 121.09(16) . . ? C6 C7 C8 117.05(15) . . ? C9 C8 C13 119.65(17) . . ? C9 C8 C7 119.96(16) . . ? C13 C8 C7 120.34(16) . . ? C10 C9 C8 120.08(19) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.1(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.3(2) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C13 120.4(2) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 119.4(2) . . ? C12 C13 H13 120.3 . . ? C8 C13 H13 120.3 . . ? C15 C14 C20 119.42(17) . . ? C15 C14 N2 122.51(15) . . ? C20 C14 N2 118.01(16) . . ? C16 C15 C14 119.70(17) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.44(18) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C19 C17 C16 118.08(18) . . ? C19 C17 C18 121.29(19) . . ? C16 C17 C18 120.63(19) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 C20 121.12(18) . . ? C17 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C14 C20 C19 120.07(18) . . ? C14 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C26 118.96(18) . . ? C22 C21 P1 117.40(14) . . ? C26 C21 P1 123.59(15) . . ? C21 C22 C23 120.4(2) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 120.0(2) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.2(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.2(2) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.2(2) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? C32 C27 C28 119.36(17) . . ? C32 C27 P1 118.49(14) . . ? C28 C27 P1 122.14(14) . . ? C29 C28 C27 120.04(19) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C30 C29 C28 119.96(19) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.45(19) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.2(2) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C27 119.97(18) . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? C34 C33 C38 119.24(17) . . ? C34 C33 P1 123.11(14) . . ? C38 C33 P1 117.65(14) . . ? C35 C34 C33 120.09(19) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 120.30(19) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 120.04(19) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.17(19) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C33 120.14(18) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? Cl4 C39 Cl3 112.3(2) . . ? Cl4 C39 H39A 109.2 . . ? Cl3 C39 H39A 109.2 . . ? Cl4 C39 H39B 109.2 . . ? Cl3 C39 H39B 109.2 . . ? H39A C39 H39B 107.9 . . ? C1 N1 P1 121.65(12) . . ? C1 N1 Zn1 110.32(10) . . ? P1 N1 Zn1 127.47(8) . . ? C7 N2 C14 120.97(15) . . ? C7 N2 Zn1 121.40(12) . . ? C14 N2 Zn1 117.62(11) . . ? N1 P1 C33 105.84(8) . . ? N1 P1 C27 114.25(8) . . ? C33 P1 C27 107.89(8) . . ? N1 P1 C21 110.99(8) . . ? C33 P1 C21 109.09(8) . . ? C27 P1 C21 108.61(8) . . ? N1 Zn1 N2 88.04(6) . . ? N1 Zn1 Cl2 120.38(4) . . ? N2 Zn1 Cl2 117.13(4) . . ? N1 Zn1 Cl1 108.75(4) . . ? N2 Zn1 Cl1 103.82(4) . . ? Cl2 Zn1 Cl1 114.83(2) . . ? Cl3B C39B Cl4B 114.6(10) . . ? Cl3B C39B H39C 108.6 . . ? Cl4B C39B H39C 108.6 . . ? Cl3B C39B H39D 108.6 . . ? Cl4B C39B H39D 108.6 . . ? H39C C39B H39D 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -179.02(17) . . . . ? C6 C1 C2 C3 1.0(3) . . . . ? C1 C2 C3 C4 0.2(3) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C3 C4 C5 C6 -0.7(3) . . . . ? C4 C5 C6 C1 1.9(3) . . . . ? C4 C5 C6 C7 -177.27(16) . . . . ? C2 C1 C6 C5 -1.9(2) . . . . ? N1 C1 C6 C5 178.06(15) . . . . ? C2 C1 C6 C7 177.10(16) . . . . ? N1 C1 C6 C7 -2.9(2) . . . . ? C5 C6 C7 N2 151.85(16) . . . . ? C1 C6 C7 N2 -27.2(2) . . . . ? C5 C6 C7 C8 -25.8(2) . . . . ? C1 C6 C7 C8 155.13(16) . . . . ? N2 C7 C8 C9 115.6(2) . . . . ? C6 C7 C8 C9 -66.7(2) . . . . ? N2 C7 C8 C13 -61.8(2) . . . . ? C6 C7 C8 C13 115.89(19) . . . . ? C13 C8 C9 C10 2.1(3) . . . . ? C7 C8 C9 C10 -175.31(17) . . . . ? C8 C9 C10 C11 -1.7(3) . . . . ? C9 C10 C11 C12 -0.1(3) . . . . ? C10 C11 C12 C13 1.5(4) . . . . ? C11 C12 C13 C8 -1.0(3) . . . . ? C9 C8 C13 C12 -0.8(3) . . . . ? C7 C8 C13 C12 176.68(19) . . . . ? C20 C14 C15 C16 -3.7(3) . . . . ? N2 C14 C15 C16 179.11(16) . . . . ? C14 C15 C16 C17 0.3(3) . . . . ? C15 C16 C17 C19 2.6(3) . . . . ? C15 C16 C17 C18 -177.6(2) . . . . ? C16 C17 C19 C20 -2.1(3) . . . . ? C18 C17 C19 C20 178.0(2) . . . . ? C15 C14 C20 C19 4.2(3) . . . . ? N2 C14 C20 C19 -178.54(17) . . . . ? C17 C19 C20 C14 -1.2(3) . . . . ? C26 C21 C22 C23 -1.3(3) . . . . ? P1 C21 C22 C23 -178.65(19) . . . . ? C21 C22 C23 C24 -0.7(4) . . . . ? C22 C23 C24 C25 1.4(4) . . . . ? C23 C24 C25 C26 -0.2(4) . . . . ? C24 C25 C26 C21 -1.7(4) . . . . ? C22 C21 C26 C25 2.5(3) . . . . ? P1 C21 C26 C25 179.67(17) . . . . ? C32 C27 C28 C29 1.0(3) . . . . ? P1 C27 C28 C29 179.84(16) . . . . ? C27 C28 C29 C30 -1.8(3) . . . . ? C28 C29 C30 C31 1.1(3) . . . . ? C29 C30 C31 C32 0.3(3) . . . . ? C30 C31 C32 C27 -1.2(3) . . . . ? C28 C27 C32 C31 0.5(3) . . . . ? P1 C27 C32 C31 -178.41(15) . . . . ? C38 C33 C34 C35 1.2(3) . . . . ? P1 C33 C34 C35 -178.06(16) . . . . ? C33 C34 C35 C36 -0.1(3) . . . . ? C34 C35 C36 C37 -1.5(3) . . . . ? C35 C36 C37 C38 1.9(3) . . . . ? C36 C37 C38 C33 -0.7(3) . . . . ? C34 C33 C38 C37 -0.8(3) . . . . ? P1 C33 C38 C37 178.51(15) . . . . ? C2 C1 N1 P1 43.2(2) . . . . ? C6 C1 N1 P1 -136.77(14) . . . . ? C2 C1 N1 Zn1 -128.75(15) . . . . ? C6 C1 N1 Zn1 51.24(17) . . . . ? C6 C7 N2 C14 -179.55(15) . . . . ? C8 C7 N2 C14 -2.0(2) . . . . ? C6 C7 N2 Zn1 -0.4(2) . . . . ? C8 C7 N2 Zn1 177.14(12) . . . . ? C15 C14 N2 C7 -58.3(2) . . . . ? C20 C14 N2 C7 124.44(18) . . . . ? C15 C14 N2 Zn1 122.51(15) . . . . ? C20 C14 N2 Zn1 -54.71(19) . . . . ? C1 N1 P1 C33 147.90(13) . . . . ? Zn1 N1 P1 C33 -41.58(12) . . . . ? C1 N1 P1 C27 -93.54(15) . . . . ? Zn1 N1 P1 C27 76.98(12) . . . . ? C1 N1 P1 C21 29.67(16) . . . . ? Zn1 N1 P1 C21 -159.81(10) . . . . ? C34 C33 P1 N1 139.64(15) . . . . ? C38 C33 P1 N1 -39.61(16) . . . . ? C34 C33 P1 C27 16.94(18) . . . . ? C38 C33 P1 C27 -162.31(14) . . . . ? C34 C33 P1 C21 -100.87(16) . . . . ? C38 C33 P1 C21 79.88(15) . . . . ? C32 C27 P1 N1 -10.90(18) . . . . ? C28 C27 P1 N1 170.23(15) . . . . ? C32 C27 P1 C33 106.49(16) . . . . ? C28 C27 P1 C33 -72.39(17) . . . . ? C32 C27 P1 C21 -135.39(15) . . . . ? C28 C27 P1 C21 45.73(18) . . . . ? C22 C21 P1 N1 59.64(18) . . . . ? C26 C21 P1 N1 -117.61(17) . . . . ? C22 C21 P1 C33 -56.60(18) . . . . ? C26 C21 P1 C33 126.15(17) . . . . ? C22 C21 P1 C27 -173.97(16) . . . . ? C26 C21 P1 C27 8.78(19) . . . . ? C1 N1 Zn1 N2 -58.52(11) . . . . ? P1 N1 Zn1 N2 130.08(11) . . . . ? C1 N1 Zn1 Cl2 -179.11(9) . . . . ? P1 N1 Zn1 Cl2 9.49(12) . . . . ? C1 N1 Zn1 Cl1 45.41(12) . . . . ? P1 N1 Zn1 Cl1 -125.99(9) . . . . ? C7 N2 Zn1 N1 36.11(13) . . . . ? C14 N2 Zn1 N1 -144.74(12) . . . . ? C7 N2 Zn1 Cl2 159.55(11) . . . . ? C14 N2 Zn1 Cl2 -21.30(13) . . . . ? C7 N2 Zn1 Cl1 -72.71(13) . . . . ? C14 N2 Zn1 Cl1 106.43(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.447 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.058 #===END