# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Han Vinh Huynh' _publ_contact_author_email chmhhv@nus.edu.sg _publ_section_title ; [2]Rotaxanes with Palladium(II)-NHC stoppers ; loop_ _publ_author_name 'Han Vinh Huynh' 'Weiheng Sim' 'Chee Fei Chin' # Attachment '- Complex2.cif' data_9153a _database_code_depnum_ccdc_archive 'CCDC 837382' #TrackingRef '- Complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H104 B2 Br4 F8 N8 O8 Pd2' _chemical_formula_weight 1987.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.4824(10) _cell_length_b 11.9020(7) _cell_length_c 45.221(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8871.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8622 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 24.12 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4024 _exptl_absorpt_coefficient_mu 2.278 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4943 _exptl_absorpt_correction_T_max 0.8042 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59467 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10199 _reflns_number_gt 6537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0763P)^2^+9.1562P] 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 10199 _refine_ls_number_parameters 469 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.53571(2) 0.54993(3) 0.164002(7) 0.04404(12) Uani 1 1 d . . . Br1 Br 0.61919(4) 0.39787(5) 0.144930(11) 0.06758(19) Uani 1 1 d . . . Br2 Br 0.45930(4) 0.70284(5) 0.185715(12) 0.0711(2) Uani 1 1 d . . . O1 O 0.6435(2) 0.5994(3) 0.05496(7) 0.0469(7) Uani 1 1 d . . . O2 O 0.6370(2) 0.3650(3) 0.03999(7) 0.0504(8) Uani 1 1 d . . . O3 O 0.4939(3) 0.2545(4) 0.03387(9) 0.0931(16) Uani 1 1 d DU . . O4 O 0.4368(2) 0.2443(3) -0.02633(7) 0.0496(8) Uani 1 1 d DU . . N1 N 0.5726(2) 0.4764(3) 0.22478(8) 0.0499(10) Uani 1 1 d . . . N2 N 0.6630(2) 0.5954(4) 0.20863(9) 0.0523(10) Uani 1 1 d . . . N3 N 0.4708(2) 0.5618(3) 0.12409(8) 0.0447(9) Uani 1 1 d . . . N4 N 0.4235(2) 0.6016(3) 0.01619(8) 0.0462(9) Uani 1 1 d . . . H4A H 0.4009 0.6241 -0.0012 0.055 Uiso 1 1 calc R . . H4B H 0.4594 0.6553 0.0220 0.055 Uiso 1 1 calc R . . C1 C 0.5950(3) 0.5396(4) 0.20129(10) 0.0462(11) Uani 1 1 d . . . C2 C 0.6281(3) 0.4936(5) 0.24790(11) 0.0594(13) Uani 1 1 d . . . C3 C 0.6319(4) 0.4491(6) 0.27656(12) 0.0792(19) Uani 1 1 d . . . H3 H 0.5945 0.3954 0.2834 0.095 Uiso 1 1 calc R . . C4 C 0.6938(5) 0.4889(8) 0.29416(13) 0.103(3) Uani 1 1 d . . . H4 H 0.6971 0.4638 0.3138 0.123 Uiso 1 1 calc R . . C5 C 0.7509(5) 0.5637(7) 0.28414(15) 0.099(2) Uani 1 1 d . . . H5 H 0.7928 0.5866 0.2969 0.119 Uiso 1 1 calc R . . C6 C 0.7481(4) 0.6062(6) 0.25558(13) 0.0784(18) Uani 1 1 d . . . H6 H 0.7871 0.6573 0.2486 0.094 Uiso 1 1 calc R . . C7 C 0.6847(3) 0.5696(5) 0.23775(11) 0.0583(13) Uani 1 1 d . . . C8 C 0.5001(3) 0.4050(5) 0.22503(11) 0.0604(14) Uani 1 1 d . . . H8 H 0.4729 0.4154 0.2057 0.073 Uiso 1 1 calc R . . C9 C 0.4406(4) 0.4441(7) 0.24873(15) 0.089(2) Uani 1 1 d . . . H9A H 0.4619 0.4257 0.2681 0.134 Uiso 1 1 calc R . . H9B H 0.3888 0.4068 0.2459 0.134 Uiso 1 1 calc R . . H9C H 0.4332 0.5248 0.2472 0.134 Uiso 1 1 calc R . . C10 C 0.5227(4) 0.2812(6) 0.22723(14) 0.084(2) Uani 1 1 d . . . H10A H 0.5597 0.2620 0.2114 0.126 Uiso 1 1 calc R . . H10B H 0.4740 0.2357 0.2256 0.126 Uiso 1 1 calc R . . H10C H 0.5486 0.2670 0.2461 0.126 Uiso 1 1 calc R . . C11 C 0.7072(3) 0.6689(4) 0.18794(11) 0.0561(13) Uani 1 1 d . . . H11 H 0.6754 0.6709 0.1694 0.067 Uiso 1 1 calc R . . C12 C 0.7887(4) 0.6205(5) 0.18042(13) 0.0719(17) Uani 1 1 d . . . H12A H 0.8218 0.6170 0.1981 0.108 Uiso 1 1 calc R . . H12B H 0.8151 0.6677 0.1658 0.108 Uiso 1 1 calc R . . H12C H 0.7818 0.5454 0.1725 0.108 Uiso 1 1 calc R . . C13 C 0.7102(4) 0.7888(5) 0.19966(14) 0.0767(17) Uani 1 1 d . . . H13A H 0.6555 0.8154 0.2032 0.115 Uiso 1 1 calc R . . H13B H 0.7364 0.8369 0.1852 0.115 Uiso 1 1 calc R . . H13C H 0.7408 0.7904 0.2180 0.115 Uiso 1 1 calc R . . C14 C 0.4417(3) 0.4724(4) 0.11036(10) 0.0524(12) Uani 1 1 d . . . H14 H 0.4480 0.4020 0.1195 0.063 Uiso 1 1 calc R . . C15 C 0.4025(3) 0.4766(4) 0.08337(11) 0.0535(12) Uani 1 1 d . . . H15 H 0.3818 0.4109 0.0746 0.064 Uiso 1 1 calc R . . C16 C 0.3944(3) 0.5795(4) 0.06954(10) 0.0411(10) Uani 1 1 d . . . C17 C 0.4224(3) 0.6732(4) 0.08393(10) 0.0450(11) Uani 1 1 d . . . H17 H 0.4164 0.7446 0.0753 0.054 Uiso 1 1 calc R . . C18 C 0.4596(3) 0.6624(4) 0.11122(10) 0.0463(11) Uani 1 1 d . . . H18 H 0.4776 0.7274 0.1211 0.056 Uiso 1 1 calc R . . C19 C 0.3581(3) 0.5897(4) 0.03922(11) 0.0526(12) Uani 1 1 d . . . H19A H 0.3223 0.6554 0.0385 0.063 Uiso 1 1 calc R . . H19B H 0.3254 0.5229 0.0349 0.063 Uiso 1 1 calc R . . C20 C 0.4674(3) 0.4935(4) 0.01154(10) 0.0524(12) Uani 1 1 d . . . H20A H 0.4288 0.4356 0.0052 0.063 Uiso 1 1 calc R . . H20B H 0.4918 0.4692 0.0302 0.063 Uiso 1 1 calc R . . C21 C 0.6334(3) 0.6968(4) 0.06950(10) 0.0438(10) Uani 1 1 d . . . C22 C 0.5905(3) 0.7813(4) 0.05438(11) 0.0468(11) Uani 1 1 d . . . C23 C 0.5761(3) 0.8844(4) 0.06767(13) 0.0582(13) Uani 1 1 d . . . H23 H 0.5463 0.9399 0.0576 0.070 Uiso 1 1 calc R . . C24 C 0.6058(4) 0.9055(5) 0.09587(13) 0.0673(15) Uani 1 1 d . . . H24 H 0.5963 0.9755 0.1048 0.081 Uiso 1 1 calc R . . C25 C 0.6487(4) 0.8252(5) 0.11056(13) 0.0705(16) Uani 1 1 d . . . H25 H 0.6694 0.8406 0.1295 0.085 Uiso 1 1 calc R . . C26 C 0.6622(3) 0.7209(5) 0.09782(11) 0.0559(13) Uani 1 1 d . . . H26 H 0.6910 0.6657 0.1084 0.067 Uiso 1 1 calc R . . C27 C 0.6980(3) 0.5182(4) 0.06796(10) 0.0493(11) Uani 1 1 d . . . H27A H 0.6752 0.4892 0.0865 0.059 Uiso 1 1 calc R . . H27B H 0.7504 0.5535 0.0723 0.059 Uiso 1 1 calc R . . C28 C 0.7091(3) 0.4249(4) 0.04638(11) 0.0527(12) Uani 1 1 d . . . H28A H 0.7308 0.4559 0.0279 0.063 Uiso 1 1 calc R . . H28B H 0.7494 0.3723 0.0543 0.063 Uiso 1 1 calc R . . C29 C 0.6103(4) 0.2927(5) 0.06238(11) 0.0629(14) Uani 1 1 d . . . H29A H 0.5848 0.3373 0.0781 0.076 Uiso 1 1 calc R . . H29B H 0.6572 0.2542 0.0710 0.076 Uiso 1 1 calc R . . C30 C 0.5536(4) 0.2108(5) 0.05208(14) 0.0783(19) Uani 1 1 d D . . H30A H 0.5832 0.1524 0.0412 0.094 Uiso 1 1 calc R . . H30B H 0.5277 0.1752 0.0692 0.094 Uiso 1 1 calc R . . C31 C 0.4294(5) 0.1850(6) 0.02488(12) 0.108(3) Uani 1 1 d DU . . H31A H 0.3783 0.2238 0.0291 0.129 Uiso 1 1 calc R . . H31B H 0.4305 0.1164 0.0368 0.129 Uiso 1 1 calc R . . C32 C 0.4302(5) 0.1536(5) -0.00600(12) 0.113(3) Uani 1 1 d DU . . H32A H 0.4758 0.1022 -0.0093 0.136 Uiso 1 1 calc R . . H32B H 0.3802 0.1122 -0.0103 0.136 Uiso 1 1 calc R . . B1 B 0.3099(4) 0.8796(5) 0.02477(16) 0.055(2) Uani 0.735(7) 1 d PDU A 1 F1 F 0.3869(3) 0.8504(5) 0.03121(15) 0.105(3) Uani 0.735(7) 1 d PDU A 1 F2 F 0.2589(3) 0.8490(4) 0.04698(11) 0.0814(17) Uani 0.735(7) 1 d PDU A 1 F3 F 0.3026(3) 0.9881(4) 0.01769(14) 0.088(2) Uani 0.735(7) 1 d PDU A 1 F4 F 0.2864(5) 0.8149(6) 0.00053(14) 0.176(4) Uani 0.735(7) 1 d PDU A 1 B1A B 0.3140(11) 0.8910(13) 0.0277(4) 0.100 Uiso 0.265(7) 1 d PD A 2 F1A F 0.3794(13) 0.8250(18) 0.0230(6) 0.120 Uiso 0.265(7) 1 d PD A 2 F2A F 0.2496(13) 0.8237(18) 0.0331(5) 0.120 Uiso 0.265(7) 1 d PD A 2 F3A F 0.2990(13) 0.9474(16) 0.0023(4) 0.120 Uiso 0.265(7) 1 d PD A 2 F4A F 0.3308(11) 0.9651(14) 0.0492(3) 0.120 Uiso 0.265(7) 1 d PD A 2 C1S C 0.3329(7) 0.2281(8) 0.1398(2) 0.223(7) Uiso 1 1 d G . . C2S C 0.3998(7) 0.1767(10) 0.15279(19) 0.212(6) Uiso 1 1 d GD . . H2S H 0.4233 0.2077 0.1699 0.255 Uiso 1 1 calc R . . C3S C 0.4319(6) 0.0793(10) 0.1405(3) 0.240(8) Uiso 1 1 d G . . H3S H 0.4771 0.0446 0.1492 0.289 Uiso 1 1 calc R . . C4S C 0.3971(8) 0.0334(8) 0.1152(3) 0.221(7) Uiso 1 1 d G . . H4S H 0.4188 -0.0324 0.1069 0.266 Uiso 1 1 calc R . . C5S C 0.3303(8) 0.0849(10) 0.1023(2) 0.266(9) Uiso 1 1 d G . . H5S H 0.3068 0.0538 0.0852 0.319 Uiso 1 1 calc R . . C6S C 0.2982(6) 0.1822(10) 0.1146(3) 0.230(7) Uiso 1 1 d GD . . H6S H 0.2530 0.2170 0.1058 0.276 Uiso 1 1 calc R . . C7S C 0.2949(17) 0.310(3) 0.1539(6) 0.457(19) Uiso 1 1 d D . . H7S1 H 0.2499 0.3365 0.1420 0.686 Uiso 1 1 calc R . . H7S2 H 0.3324 0.3716 0.1574 0.686 Uiso 1 1 calc R . . H7S3 H 0.2747 0.2825 0.1727 0.686 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0519(2) 0.0476(2) 0.03262(17) 0.00748(14) 0.00714(15) 0.00596(16) Br1 0.0871(4) 0.0697(4) 0.0459(3) 0.0036(2) 0.0002(3) 0.0348(3) Br2 0.0842(4) 0.0776(4) 0.0515(3) -0.0112(3) 0.0054(3) 0.0277(3) O1 0.0551(19) 0.0438(18) 0.0419(16) 0.0032(14) -0.0059(15) 0.0050(15) O2 0.061(2) 0.0452(19) 0.0453(17) 0.0088(14) -0.0125(16) 0.0002(16) O3 0.110(3) 0.083(3) 0.086(3) 0.046(2) -0.048(3) -0.054(3) O4 0.0503(18) 0.0412(17) 0.0575(19) 0.0109(15) -0.0100(16) 0.0009(15) N1 0.052(2) 0.061(3) 0.0368(19) 0.0120(18) 0.0057(18) -0.006(2) N2 0.050(2) 0.058(2) 0.049(2) 0.0111(19) 0.0090(19) -0.004(2) N3 0.052(2) 0.044(2) 0.0380(19) 0.0070(16) 0.0031(17) 0.0084(18) N4 0.057(2) 0.042(2) 0.0391(19) 0.0046(16) -0.0123(18) -0.0077(19) C1 0.049(3) 0.050(3) 0.039(2) 0.007(2) 0.006(2) 0.002(2) C2 0.055(3) 0.081(4) 0.042(3) 0.012(3) 0.001(2) -0.004(3) C3 0.076(4) 0.112(5) 0.050(3) 0.024(3) -0.003(3) -0.014(4) C4 0.096(5) 0.165(8) 0.046(3) 0.035(4) -0.020(3) -0.027(5) C5 0.077(4) 0.151(7) 0.070(4) 0.006(4) -0.024(4) -0.024(5) C6 0.064(4) 0.109(5) 0.062(3) 0.006(3) -0.009(3) -0.018(4) C7 0.054(3) 0.075(4) 0.046(3) 0.011(2) 0.004(2) -0.004(3) C8 0.059(3) 0.077(4) 0.045(3) 0.017(3) 0.003(2) -0.016(3) C9 0.067(4) 0.121(6) 0.080(4) 0.014(4) 0.026(3) -0.022(4) C10 0.106(5) 0.082(5) 0.065(4) 0.017(3) -0.001(4) -0.020(4) C11 0.064(3) 0.051(3) 0.053(3) 0.007(2) 0.014(3) -0.004(3) C12 0.071(4) 0.063(4) 0.082(4) 0.000(3) 0.034(3) -0.008(3) C13 0.081(4) 0.063(4) 0.086(4) -0.003(3) 0.028(4) -0.004(3) C14 0.074(3) 0.042(3) 0.041(2) 0.012(2) 0.002(2) 0.006(2) C15 0.070(3) 0.040(3) 0.051(3) 0.008(2) 0.001(3) -0.002(2) C16 0.036(2) 0.044(3) 0.043(2) 0.0063(19) 0.0017(19) -0.0016(19) C17 0.045(3) 0.040(2) 0.050(3) 0.013(2) -0.001(2) 0.003(2) C18 0.051(3) 0.041(3) 0.046(2) 0.004(2) 0.003(2) 0.000(2) C19 0.045(3) 0.053(3) 0.060(3) 0.012(2) -0.005(2) -0.004(2) C20 0.072(3) 0.043(3) 0.042(2) 0.004(2) 0.002(2) 0.002(2) C21 0.038(2) 0.045(3) 0.049(3) 0.004(2) 0.002(2) -0.006(2) C22 0.038(2) 0.051(3) 0.052(3) 0.004(2) 0.006(2) -0.007(2) C23 0.055(3) 0.044(3) 0.076(4) -0.001(3) 0.006(3) -0.002(2) C24 0.080(4) 0.052(3) 0.070(4) -0.012(3) 0.014(3) -0.008(3) C25 0.088(4) 0.070(4) 0.053(3) -0.005(3) 0.003(3) -0.017(3) C26 0.061(3) 0.063(3) 0.044(3) 0.008(2) -0.002(2) -0.011(3) C27 0.049(3) 0.052(3) 0.048(3) 0.011(2) -0.010(2) 0.002(2) C28 0.054(3) 0.051(3) 0.052(3) 0.008(2) 0.002(2) 0.011(2) C29 0.072(4) 0.065(3) 0.052(3) 0.019(3) -0.014(3) -0.007(3) C30 0.109(5) 0.052(3) 0.075(4) 0.025(3) -0.024(4) -0.010(3) C31 0.147(7) 0.094(5) 0.083(4) 0.048(4) -0.047(5) -0.073(5) C32 0.138(6) 0.121(6) 0.081(5) 0.043(4) -0.025(5) -0.085(5) B1 0.045(4) 0.043(4) 0.077(5) 0.017(4) 0.011(4) 0.011(3) F1 0.043(3) 0.122(5) 0.150(6) 0.082(5) 0.004(3) 0.021(3) F2 0.072(3) 0.082(3) 0.090(4) 0.018(3) 0.035(3) 0.000(3) F3 0.068(3) 0.061(3) 0.134(5) 0.041(3) 0.019(3) 0.012(2) F4 0.192(8) 0.210(8) 0.127(6) -0.050(5) -0.008(6) -0.013(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 Pd1 C1 1.953(5) . ? Pd1 N3 2.103(4) . ? Pd1 Br2 2.4212(7) . ? Pd1 Br1 2.4315(6) . ? O1 C21 1.343(5) . ? O1 C27 1.445(5) . ? O2 C29 1.400(6) . ? O2 C28 1.417(6) . ? O3 C30 1.385(4) . ? O3 C31 1.406(4) . ? O4 C22 1.380(6) 5_665 ? O4 C32 1.423(4) . ? N1 C1 1.353(5) . ? N1 C2 1.405(6) . ? N1 C8 1.466(7) . ? N2 C1 1.345(6) . ? N2 C7 1.399(6) . ? N2 C11 1.473(6) . ? N3 C14 1.322(6) . ? N3 C18 1.344(6) . ? N4 C20 1.490(6) . ? N4 C19 1.506(6) . ? C2 C7 1.378(7) . ? C2 C3 1.401(7) . ? C3 C4 1.379(9) . ? C4 C5 1.371(10) . ? C5 C6 1.388(9) . ? C6 C7 1.389(8) . ? C8 C10 1.523(9) . ? C8 C9 1.526(8) . ? C11 C12 1.501(7) . ? C11 C13 1.523(8) . ? C14 C15 1.382(7) . ? C15 C16 1.382(6) . ? C16 C17 1.371(6) . ? C16 C19 1.501(6) . ? C17 C18 1.384(6) . ? C20 C20 1.507(9) 5_665 ? C21 C26 1.395(6) . ? C21 C22 1.407(7) . ? C22 O4 1.380(6) 5_665 ? C22 C23 1.387(7) . ? C23 C24 1.389(8) . ? C24 C25 1.363(9) . ? C25 C26 1.387(8) . ? C27 C28 1.490(7) . ? C29 C30 1.428(8) . ? C31 C32 1.446(5) . ? B1 F3 1.335(7) . ? B1 F1 1.347(7) . ? B1 F2 1.360(7) . ? B1 F4 1.395(7) . ? B1A F4A 1.340(10) . ? B1A F1A 1.351(10) . ? B1A F3A 1.352(10) . ? B1A F2A 1.353(10) . ? C1S C7S 1.32(3) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N3 179.38(17) . . ? C1 Pd1 Br2 87.56(14) . . ? N3 Pd1 Br2 91.89(10) . . ? C1 Pd1 Br1 88.64(14) . . ? N3 Pd1 Br1 91.92(10) . . ? Br2 Pd1 Br1 176.06(3) . . ? C21 O1 C27 117.1(3) . . ? C29 O2 C28 115.2(4) . . ? C30 O3 C31 119.2(5) . . ? C22 O4 C32 113.7(4) 5_665 . ? C1 N1 C2 109.0(4) . . ? C1 N1 C8 123.4(4) . . ? C2 N1 C8 127.6(4) . . ? C1 N2 C7 109.7(4) . . ? C1 N2 C11 123.2(4) . . ? C7 N2 C11 127.0(4) . . ? C14 N3 C18 117.6(4) . . ? C14 N3 Pd1 122.3(3) . . ? C18 N3 Pd1 120.1(3) . . ? C20 N4 C19 111.3(3) . . ? N2 C1 N1 108.0(4) . . ? N2 C1 Pd1 126.8(3) . . ? N1 C1 Pd1 125.2(4) . . ? C7 C2 C3 121.7(5) . . ? C7 C2 N1 106.8(4) . . ? C3 C2 N1 131.5(5) . . ? C4 C3 C2 115.9(6) . . ? C5 C4 C3 122.7(6) . . ? C4 C5 C6 121.4(6) . . ? C5 C6 C7 116.8(6) . . ? C2 C7 C6 121.4(5) . . ? C2 C7 N2 106.5(5) . . ? C6 C7 N2 132.1(5) . . ? N1 C8 C10 111.3(5) . . ? N1 C8 C9 110.6(5) . . ? C10 C8 C9 114.0(5) . . ? N2 C11 C12 110.9(4) . . ? N2 C11 C13 110.6(4) . . ? C12 C11 C13 114.1(5) . . ? N3 C14 C15 123.7(4) . . ? C14 C15 C16 118.5(5) . . ? C17 C16 C15 118.3(4) . . ? C17 C16 C19 120.1(4) . . ? C15 C16 C19 121.6(4) . . ? C16 C17 C18 119.8(4) . . ? N3 C18 C17 122.0(4) . . ? C16 C19 N4 110.7(4) . . ? N4 C20 C20 110.9(5) . 5_665 ? O1 C21 C26 125.8(4) . . ? O1 C21 C22 116.2(4) . . ? C26 C21 C22 118.1(5) . . ? O4 C22 C23 122.6(5) 5_665 . ? O4 C22 C21 116.9(4) 5_665 . ? C23 C22 C21 120.5(5) . . ? C22 C23 C24 119.8(5) . . ? C25 C24 C23 120.2(5) . . ? C24 C25 C26 120.6(5) . . ? C25 C26 C21 120.7(5) . . ? O1 C27 C28 108.0(4) . . ? O2 C28 C27 113.9(4) . . ? O2 C29 C30 112.9(4) . . ? O3 C30 C29 113.7(4) . . ? O3 C31 C32 115.1(6) . . ? O4 C32 C31 115.4(5) . . ? F3 B1 F1 112.7(5) . . ? F3 B1 F2 112.4(5) . . ? F1 B1 F2 110.7(5) . . ? F3 B1 F4 108.7(6) . . ? F1 B1 F4 106.8(6) . . ? F2 B1 F4 105.1(5) . . ? F4A B1A F1A 109.4(9) . . ? F4A B1A F3A 109.0(9) . . ? F1A B1A F3A 107.5(9) . . ? F4A B1A F2A 115(2) . . ? F1A B1A F2A 108.1(9) . . ? F3A B1A F2A 107.7(9) . . ? C7S C1S C2S 119.8(8) . . ? C7S C1S C6S 119.4(8) . . ? C2S C1S C6S 120.0 . . ? C3S C2S C1S 120.0 . . ? C2S C3S C4S 120.0 . . ? C3S C4S C5S 120.0 . . ? C4S C5S C6S 120.0 . . ? C5S C6S C1S 120.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A O2 0.91 1.87 2.758(5) 165.6 5_665 N4 H4A O2 0.91 1.87 2.758(5) 165.6 5_665 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.847 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.091 # Attachment '- Complex3.cif' data_9126 _database_code_depnum_ccdc_archive 'CCDC 837383' #TrackingRef '- Complex3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H102 Br8 N16 Pd4' _chemical_formula_weight 2280.60 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.3588(6) _cell_length_b 17.5310(5) _cell_length_c 26.8606(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.9010(10) _cell_angle_gamma 90.00 _cell_volume 9122.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9587 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.68 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4488 _exptl_absorpt_coefficient_mu 4.326 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1811 _exptl_absorpt_correction_T_max 0.5444 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64361 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 20954 _reflns_number_gt 13533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0670P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20954 _refine_ls_number_parameters 940 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1354 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.60390(2) 0.52204(2) 0.816959(16) 0.04406(11) Uani 1 1 d . . . Pd2 Pd 0.46868(2) -0.17149(2) 0.563849(18) 0.04783(12) Uani 1 1 d . . . Pd3 Pd 0.513714(19) 0.16334(2) 0.867504(15) 0.03754(10) Uani 1 1 d . . . Pd4 Pd 0.29176(2) 0.03960(2) 0.714314(15) 0.03994(11) Uani 1 1 d . . . Br1 Br 0.57396(4) 0.51680(4) 0.72240(3) 0.0796(2) Uani 1 1 d . . . Br2 Br 0.64129(4) 0.54271(4) 0.91082(2) 0.06734(19) Uani 1 1 d . . . Br3 Br 0.35496(3) -0.13302(4) 0.50835(3) 0.06592(18) Uani 1 1 d . . . Br4 Br 0.58451(3) -0.21499(4) 0.61253(3) 0.06648(18) Uani 1 1 d . . . Br5 Br 0.48706(3) 0.20078(4) 0.94615(2) 0.05513(16) Uani 1 1 d . . . Br6 Br 0.54666(3) 0.12171(4) 0.79165(2) 0.05611(16) Uani 1 1 d . . . Br7 Br 0.33698(3) 0.15416(4) 0.68452(2) 0.05833(17) Uani 1 1 d . . . Br8 Br 0.23830(3) -0.07076(4) 0.74071(2) 0.05635(16) Uani 1 1 d . . . N1 N 0.6679(2) 0.6721(3) 0.8107(2) 0.0542(12) Uani 1 1 d . . . N2 N 0.7391(2) 0.5775(3) 0.81423(18) 0.0485(11) Uani 1 1 d . . . N3 N 0.4616(2) -0.2849(3) 0.4804(2) 0.0601(14) Uani 1 1 d . . . N4 N 0.5163(2) -0.1827(3) 0.47095(18) 0.0484(11) Uani 1 1 d . . . N5 N 0.6612(2) 0.1956(2) 0.91668(17) 0.0442(10) Uani 1 1 d . . . N6 N 0.6347(2) 0.0823(2) 0.93706(17) 0.0435(10) Uani 1 1 d . . . N7 N 0.1520(2) 0.1036(2) 0.66803(16) 0.0443(10) Uani 1 1 d . . . N8 N 0.1841(2) 0.0369(2) 0.61177(16) 0.0410(10) Uani 1 1 d . . . N9 N 0.5300(2) 0.4378(2) 0.81881(17) 0.0447(10) Uani 1 1 d . . . N10 N 0.4522(2) -0.1265(2) 0.63158(18) 0.0469(11) Uani 1 1 d . . . N11 N 0.4103(2) 0.1837(2) 0.81977(18) 0.0395(10) Uani 1 1 d . . . H11N H 0.412(2) 0.180(3) 0.7900(18) 0.029(14) Uiso 1 1 d . . . N12 N 0.3889(2) 0.0223(3) 0.77301(17) 0.0415(10) Uani 1 1 d . . . H12N H 0.415(3) 0.052(3) 0.762(2) 0.049(17) Uiso 1 1 d . . . C1 C 0.6741(3) 0.5957(3) 0.8143(2) 0.0450(13) Uani 1 1 d . . . C2 C 0.7307(3) 0.7039(3) 0.8087(2) 0.0572(15) Uani 1 1 d . . . C3 C 0.7507(4) 0.7790(4) 0.8052(3) 0.077(2) Uani 1 1 d . . . H3 H 0.7206 0.8200 0.8041 0.092 Uiso 1 1 calc R . . C4 C 0.8175(4) 0.7905(4) 0.8034(3) 0.086(2) Uani 1 1 d . . . H4 H 0.8329 0.8406 0.8014 0.103 Uiso 1 1 calc R . . C5 C 0.8608(4) 0.7316(5) 0.8046(3) 0.081(2) Uani 1 1 d . . . H5 H 0.9054 0.7418 0.8030 0.097 Uiso 1 1 calc R . . C6 C 0.8413(4) 0.6567(4) 0.8082(3) 0.0725(19) Uani 1 1 d . . . H6 H 0.8717 0.6159 0.8091 0.087 Uiso 1 1 calc R . . C7 C 0.7745(3) 0.6443(3) 0.8105(2) 0.0510(14) Uani 1 1 d . . . C8 C 0.6044(4) 0.7127(4) 0.8100(4) 0.085(3) Uani 1 1 d . . . H8 H 0.5705 0.6730 0.8117 0.102 Uiso 1 1 calc R . . C9 C 0.5739(5) 0.7543(6) 0.7589(5) 0.145(5) Uani 1 1 d . . . H9A H 0.6023 0.7982 0.7576 0.217 Uiso 1 1 calc R . . H9B H 0.5275 0.7711 0.7561 0.217 Uiso 1 1 calc R . . H9C H 0.5723 0.7203 0.7300 0.217 Uiso 1 1 calc R . . C10 C 0.6185(6) 0.7595(5) 0.8600(5) 0.154(5) Uani 1 1 d . . . H10A H 0.6477 0.7305 0.8892 0.230 Uiso 1 1 calc R . . H10B H 0.5752 0.7712 0.8664 0.230 Uiso 1 1 calc R . . H10C H 0.6416 0.8066 0.8563 0.230 Uiso 1 1 calc R . . C11 C 0.7663(3) 0.4979(3) 0.8235(3) 0.0604(16) Uani 1 1 d . . . H11 H 0.7279 0.4649 0.8260 0.073 Uiso 1 1 calc R . . C12 C 0.8221(4) 0.4938(5) 0.8752(3) 0.094(3) Uani 1 1 d . . . H12A H 0.8614 0.5240 0.8736 0.141 Uiso 1 1 calc R . . H12B H 0.8363 0.4412 0.8829 0.141 Uiso 1 1 calc R . . H12C H 0.8048 0.5137 0.9025 0.141 Uiso 1 1 calc R . . C13 C 0.7882(4) 0.4695(4) 0.7782(3) 0.086(2) Uani 1 1 d . . . H13A H 0.7488 0.4694 0.7468 0.129 Uiso 1 1 calc R . . H13B H 0.8062 0.4180 0.7855 0.129 Uiso 1 1 calc R . . H13C H 0.8238 0.5026 0.7733 0.129 Uiso 1 1 calc R . . C14 C 0.4828(3) -0.2151(3) 0.5012(2) 0.0481(13) Uani 1 1 d . . . C15 C 0.4839(3) -0.2982(3) 0.4372(3) 0.0579(16) Uani 1 1 d . . . C16 C 0.4779(3) -0.3602(4) 0.4037(3) 0.078(2) Uani 1 1 d . . . H16 H 0.4534 -0.4042 0.4073 0.094 Uiso 1 1 calc R . . C17 C 0.5086(4) -0.3548(5) 0.3661(3) 0.083(2) Uani 1 1 d . . . H17 H 0.5055 -0.3959 0.3429 0.100 Uiso 1 1 calc R . . C18 C 0.5444(4) -0.2903(5) 0.3608(3) 0.082(2) Uani 1 1 d . . . H18 H 0.5659 -0.2893 0.3344 0.098 Uiso 1 1 calc R . . C19 C 0.5504(4) -0.2276(4) 0.3921(2) 0.0649(18) Uani 1 1 d . . . H19 H 0.5744 -0.1835 0.3878 0.078 Uiso 1 1 calc R . . C20 C 0.5178(3) -0.2341(4) 0.4313(2) 0.0561(16) Uani 1 1 d . . . C21 C 0.4245(4) -0.3384(4) 0.5062(4) 0.095(3) Uani 1 1 d . . . H21 H 0.4174 -0.3115 0.5365 0.114 Uiso 1 1 calc R . . C22 C 0.4701(5) -0.4073(5) 0.5270(5) 0.135(4) Uani 1 1 d . . . H22A H 0.4879 -0.4269 0.4999 0.203 Uiso 1 1 calc R . . H22B H 0.4432 -0.4465 0.5372 0.203 Uiso 1 1 calc R . . H22C H 0.5083 -0.3923 0.5571 0.203 Uiso 1 1 calc R . . C23 C 0.3525(5) -0.3546(6) 0.4666(5) 0.158(5) Uani 1 1 d . . . H23A H 0.3289 -0.3067 0.4548 0.236 Uiso 1 1 calc R . . H23B H 0.3255 -0.3851 0.4833 0.236 Uiso 1 1 calc R . . H23C H 0.3579 -0.3821 0.4368 0.236 Uiso 1 1 calc R . . C24 C 0.5460(3) -0.1057(3) 0.4811(2) 0.0561(15) Uani 1 1 d . . . H24 H 0.5329 -0.0844 0.5109 0.067 Uiso 1 1 calc R . . C25 C 0.5162(5) -0.0536(4) 0.4346(3) 0.097(3) Uani 1 1 d . . . H25A H 0.5332 -0.0690 0.4061 0.146 Uiso 1 1 calc R . . H25B H 0.5302 -0.0014 0.4445 0.146 Uiso 1 1 calc R . . H25C H 0.4663 -0.0569 0.4235 0.146 Uiso 1 1 calc R . . C26 C 0.6255(4) -0.1106(4) 0.4983(3) 0.074(2) Uani 1 1 d . . . H26A H 0.6413 -0.1448 0.5280 0.111 Uiso 1 1 calc R . . H26B H 0.6449 -0.0603 0.5081 0.111 Uiso 1 1 calc R . . H26C H 0.6401 -0.1299 0.4695 0.111 Uiso 1 1 calc R . . C27 C 0.6090(3) 0.1450(3) 0.9103(2) 0.0402(12) Uani 1 1 d . . . C28 C 0.7225(3) 0.1622(3) 0.9487(2) 0.0464(13) Uani 1 1 d . . . C29 C 0.7892(3) 0.1900(4) 0.9663(2) 0.0595(16) Uani 1 1 d . . . H29 H 0.8006 0.2389 0.9572 0.071 Uiso 1 1 calc R . . C30 C 0.8382(3) 0.1418(5) 0.9983(3) 0.077(2) Uani 1 1 d . . . H30 H 0.8841 0.1588 1.0115 0.093 Uiso 1 1 calc R . . C31 C 0.8221(3) 0.0701(4) 1.0112(3) 0.0705(19) Uani 1 1 d . . . H31 H 0.8573 0.0389 1.0323 0.085 Uiso 1 1 calc R . . C32 C 0.7556(3) 0.0429(4) 0.9940(2) 0.0587(16) Uani 1 1 d . . . H32 H 0.7442 -0.0057 1.0035 0.070 Uiso 1 1 calc R . . C33 C 0.7056(3) 0.0912(3) 0.9615(2) 0.0449(13) Uani 1 1 d . . . C34 C 0.6513(3) 0.2740(3) 0.8961(2) 0.0557(15) Uani 1 1 d . . . H34 H 0.6017 0.2792 0.8765 0.067 Uiso 1 1 calc R . . C35 C 0.6663(4) 0.3311(4) 0.9401(3) 0.078(2) Uani 1 1 d . . . H35A H 0.6368 0.3210 0.9617 0.117 Uiso 1 1 calc R . . H35B H 0.6574 0.3822 0.9257 0.117 Uiso 1 1 calc R . . H35C H 0.7142 0.3270 0.9613 0.117 Uiso 1 1 calc R . . C36 C 0.6903(4) 0.2893(4) 0.8579(3) 0.077(2) Uani 1 1 d . . . H36A H 0.7395 0.2886 0.8761 0.115 Uiso 1 1 calc R . . H36B H 0.6773 0.3388 0.8418 0.115 Uiso 1 1 calc R . . H36C H 0.6793 0.2502 0.8310 0.115 Uiso 1 1 calc R . . C37 C 0.5917(3) 0.0142(3) 0.9383(3) 0.0641(18) Uani 1 1 d . . . H37 H 0.5436 0.0263 0.9175 0.077 Uiso 1 1 calc R . . C38 C 0.5918(4) -0.0035(4) 0.9936(3) 0.0723(19) Uani 1 1 d . . . H38A H 0.6385 -0.0155 1.0150 0.109 Uiso 1 1 calc R . . H38B H 0.5619 -0.0467 0.9931 0.109 Uiso 1 1 calc R . . H38C H 0.5753 0.0405 1.0080 0.109 Uiso 1 1 calc R . . C39 C 0.6153(4) -0.0526(4) 0.9120(3) 0.089(2) Uani 1 1 d . . . H39A H 0.6170 -0.0371 0.8778 0.134 Uiso 1 1 calc R . . H39B H 0.5832 -0.0946 0.9083 0.134 Uiso 1 1 calc R . . H39C H 0.6609 -0.0687 0.9333 0.134 Uiso 1 1 calc R . . C40 C 0.2036(3) 0.0605(3) 0.6611(2) 0.0406(12) Uani 1 1 d . . . C41 C 0.0995(3) 0.1112(3) 0.6207(2) 0.0417(12) Uani 1 1 d . . . C42 C 0.0379(3) 0.1516(3) 0.6060(2) 0.0531(14) Uani 1 1 d . . . H42 H 0.0236 0.1799 0.6306 0.064 Uiso 1 1 calc R . . C43 C -0.0015(3) 0.1487(4) 0.5541(3) 0.0637(17) Uani 1 1 d . . . H43 H -0.0432 0.1761 0.5428 0.076 Uiso 1 1 calc R . . C44 C 0.0195(3) 0.1059(4) 0.5185(2) 0.0591(16) Uani 1 1 d . . . H44 H -0.0087 0.1048 0.4835 0.071 Uiso 1 1 calc R . . C45 C 0.0794(3) 0.0654(3) 0.5321(2) 0.0505(14) Uani 1 1 d . . . H45 H 0.0928 0.0367 0.5073 0.061 Uiso 1 1 calc R . . C46 C 0.1202(3) 0.0685(3) 0.5844(2) 0.0446(13) Uani 1 1 d . . . C47 C 0.1540(3) 0.1373(4) 0.7188(2) 0.0561(15) Uani 1 1 d . . . H47 H 0.1972 0.1193 0.7446 0.067 Uiso 1 1 calc R . . C48 C 0.1590(5) 0.2245(4) 0.7172(3) 0.090(3) Uani 1 1 d . . . H48A H 0.1967 0.2387 0.7041 0.134 Uiso 1 1 calc R . . H48B H 0.1673 0.2449 0.7522 0.134 Uiso 1 1 calc R . . H48C H 0.1161 0.2450 0.6943 0.134 Uiso 1 1 calc R . . C49 C 0.0952(4) 0.1070(5) 0.7368(3) 0.088(2) Uani 1 1 d . . . H49A H 0.0515 0.1228 0.7123 0.132 Uiso 1 1 calc R . . H49B H 0.0992 0.1271 0.7713 0.132 Uiso 1 1 calc R . . H49C H 0.0973 0.0517 0.7383 0.132 Uiso 1 1 calc R . . C50 C 0.2286(3) -0.0105(3) 0.5898(2) 0.0499(14) Uani 1 1 d . . . H50 H 0.2705 -0.0229 0.6191 0.060 Uiso 1 1 calc R . . C51 C 0.1946(3) -0.0856(3) 0.5688(3) 0.0607(16) Uani 1 1 d . . . H51A H 0.1833 -0.1129 0.5965 0.091 Uiso 1 1 calc R . . H51B H 0.2260 -0.1161 0.5562 0.091 Uiso 1 1 calc R . . H51C H 0.1527 -0.0760 0.5403 0.091 Uiso 1 1 calc R . . C52 C 0.2526(4) 0.0338(4) 0.5499(3) 0.0718(19) Uani 1 1 d . . . H52A H 0.2131 0.0458 0.5199 0.108 Uiso 1 1 calc R . . H52B H 0.2852 0.0032 0.5388 0.108 Uiso 1 1 calc R . . H52C H 0.2748 0.0807 0.5657 0.108 Uiso 1 1 calc R . . C53 C 0.4927(3) 0.4411(3) 0.8515(2) 0.0527(14) Uani 1 1 d . . . H53 H 0.4989 0.4832 0.8742 0.063 Uiso 1 1 calc R . . C54 C 0.4448(3) 0.3853(3) 0.8538(2) 0.0503(14) Uani 1 1 d . . . H54 H 0.4194 0.3906 0.8775 0.060 Uiso 1 1 calc R . . C55 C 0.4347(3) 0.3226(3) 0.8215(2) 0.0429(12) Uani 1 1 d . . . C56 C 0.4748(3) 0.3193(3) 0.7877(2) 0.0492(14) Uani 1 1 d . . . H56 H 0.4708 0.2774 0.7651 0.059 Uiso 1 1 calc R . . C57 C 0.5197(3) 0.3769(3) 0.7871(2) 0.0457(13) Uani 1 1 d . . . H57 H 0.5448 0.3737 0.7631 0.055 Uiso 1 1 calc R . . C58 C 0.3842(3) 0.2613(3) 0.8240(2) 0.0448(13) Uani 1 1 d . . . H58A H 0.3738 0.2657 0.8572 0.054 Uiso 1 1 calc R . . H58B H 0.3412 0.2691 0.7955 0.054 Uiso 1 1 calc R . . C59 C 0.3617(3) 0.1249(3) 0.8283(2) 0.0444(13) Uani 1 1 d . . . H59A H 0.3166 0.1318 0.8019 0.053 Uiso 1 1 calc R . . H59B H 0.3558 0.1330 0.8627 0.053 Uiso 1 1 calc R . . C60 C 0.3855(3) 0.0446(3) 0.8252(2) 0.0442(13) Uani 1 1 d . . . H60A H 0.4314 0.0384 0.8507 0.053 Uiso 1 1 calc R . . H60B H 0.3540 0.0098 0.8352 0.053 Uiso 1 1 calc R . . C61 C 0.4198(3) -0.0551(3) 0.7754(2) 0.0471(13) Uani 1 1 d . . . H61A H 0.3894 -0.0924 0.7844 0.057 Uiso 1 1 calc R . . H61B H 0.4643 -0.0561 0.8032 0.057 Uiso 1 1 calc R . . C62 C 0.4989(3) -0.0843(3) 0.6669(2) 0.0545(15) Uani 1 1 d . . . H62 H 0.5403 -0.0720 0.6602 0.065 Uiso 1 1 calc R . . C63 C 0.4895(3) -0.0581(3) 0.7124(2) 0.0518(14) Uani 1 1 d . . . H63 H 0.5229 -0.0266 0.7350 0.062 Uiso 1 1 calc R . . C64 C 0.4308(3) -0.0779(3) 0.7249(2) 0.0448(13) Uani 1 1 d . . . C65 C 0.3824(3) -0.1219(3) 0.6885(2) 0.0510(14) Uani 1 1 d . . . H65 H 0.3413 -0.1363 0.6949 0.061 Uiso 1 1 calc R . . C66 C 0.3946(3) -0.1447(3) 0.6424(2) 0.0534(15) Uani 1 1 d . . . H66 H 0.3609 -0.1739 0.6181 0.064 Uiso 1 1 calc R . . N2S N 0.2677(5) 0.7314(5) 0.6360(4) 0.118(3) Uani 1 1 d . . . C3S C 0.2423(5) 0.7168(5) 0.5917(5) 0.097(3) Uani 1 1 d . . . C4S C 0.2069(6) 0.7037(6) 0.5387(4) 0.129(4) Uani 1 1 d . . . H4S1 H 0.1584 0.6952 0.5343 0.194 Uiso 1 1 calc R . . H4S2 H 0.2261 0.6592 0.5268 0.194 Uiso 1 1 calc R . . H4S3 H 0.2119 0.7478 0.5183 0.194 Uiso 1 1 calc R . . N3S N 0.0585(6) 0.3612(5) 0.6061(3) 0.129(3) Uani 1 1 d . . . C5S C 0.0968(6) 0.3362(5) 0.5901(4) 0.097(3) Uani 1 1 d . . . C6S C 0.1484(6) 0.3006(6) 0.5698(4) 0.122(3) Uani 1 1 d . . . H6S1 H 0.1798 0.3392 0.5647 0.183 Uiso 1 1 calc R . . H6S2 H 0.1254 0.2759 0.5367 0.183 Uiso 1 1 calc R . . H6S3 H 0.1741 0.2629 0.5947 0.183 Uiso 1 1 calc R . . N4S N 0.7628(6) -0.0217(6) 0.8641(4) 0.180(3) Uiso 1 1 d D . . C7S C 0.7868(8) 0.0368(7) 0.8572(6) 0.180(3) Uiso 1 1 d D . . C8S C 0.7960(7) 0.1172(7) 0.8379(5) 0.180(3) Uiso 1 1 d D . . H8S1 H 0.7520 0.1435 0.8279 0.270 Uiso 1 1 calc R . . H8S2 H 0.8129 0.1136 0.8079 0.270 Uiso 1 1 calc R . . H8S3 H 0.8290 0.1452 0.8656 0.270 Uiso 1 1 calc R . . N5S N 0.3623(16) 0.5850(19) 0.5944(12) 0.245(9) Uiso 0.50 1 d PD . . C9S C 0.4085(18) 0.617(2) 0.6208(15) 0.245(9) Uiso 0.50 1 d PD . . C10S C 0.4683(17) 0.664(2) 0.6584(13) 0.245(9) Uiso 0.50 1 d PD . . H7S H 0.4787 0.6436 0.6936 0.368 Uiso 0.50 1 calc PR . . H9S H 0.4546 0.7168 0.6581 0.368 Uiso 0.50 1 calc PR . . H8S H 0.5090 0.6600 0.6469 0.368 Uiso 0.50 1 calc PR . . N1SA N 0.7400(7) -0.0236(7) 1.1126(4) 0.073(3) Uani 0.50 1 d P . . C1SA C 0.7821(8) 0.0116(9) 1.1300(4) 0.068(4) Uani 0.50 1 d P . . C2SA C 0.8409(8) 0.0580(10) 1.1545(5) 0.101(7) Uani 0.50 1 d P . . H2SA H 0.8752 0.0516 1.1365 0.151 Uiso 0.50 1 calc PR . . H2SB H 0.8605 0.0429 1.1908 0.151 Uiso 0.50 1 calc PR . . H2SC H 0.8270 0.1111 1.1528 0.151 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0481(3) 0.0330(2) 0.0518(3) 0.00083(18) 0.01637(19) -0.00411(18) Pd2 0.0397(2) 0.0353(2) 0.0733(3) -0.0034(2) 0.0245(2) -0.00190(18) Pd3 0.02686(19) 0.0342(2) 0.0477(2) -0.00229(17) 0.00573(16) -0.00374(16) Pd4 0.0307(2) 0.0392(2) 0.0453(2) 0.00089(17) 0.00474(16) -0.00270(17) Br1 0.1020(6) 0.0815(5) 0.0532(4) -0.0021(3) 0.0208(4) -0.0442(4) Br2 0.0926(5) 0.0548(4) 0.0554(4) -0.0060(3) 0.0238(3) -0.0185(4) Br3 0.0490(4) 0.0646(4) 0.0834(5) -0.0036(3) 0.0193(3) 0.0131(3) Br4 0.0495(4) 0.0704(4) 0.0811(5) 0.0043(3) 0.0224(3) 0.0121(3) Br5 0.0488(3) 0.0621(4) 0.0514(3) -0.0064(3) 0.0109(3) 0.0030(3) Br6 0.0413(3) 0.0675(4) 0.0615(4) -0.0141(3) 0.0188(3) -0.0102(3) Br7 0.0554(4) 0.0549(4) 0.0565(4) 0.0114(3) 0.0051(3) -0.0131(3) Br8 0.0437(3) 0.0507(3) 0.0711(4) 0.0030(3) 0.0123(3) -0.0134(3) N1 0.050(3) 0.033(3) 0.083(3) 0.006(2) 0.024(3) -0.003(2) N2 0.044(3) 0.036(3) 0.063(3) 0.001(2) 0.013(2) -0.001(2) N3 0.041(3) 0.037(3) 0.104(4) -0.016(3) 0.025(3) -0.010(2) N4 0.045(3) 0.041(3) 0.062(3) -0.009(2) 0.021(2) 0.003(2) N5 0.031(2) 0.038(2) 0.058(3) -0.003(2) 0.0041(19) -0.0062(19) N6 0.028(2) 0.038(2) 0.060(3) -0.003(2) 0.0078(19) -0.0027(19) N7 0.036(2) 0.042(3) 0.049(3) -0.006(2) 0.0043(19) 0.002(2) N8 0.035(2) 0.045(3) 0.040(2) -0.0023(19) 0.0072(18) 0.0014(19) N9 0.048(3) 0.033(2) 0.055(3) 0.003(2) 0.018(2) -0.001(2) N10 0.043(3) 0.038(2) 0.065(3) -0.001(2) 0.024(2) 0.000(2) N11 0.031(2) 0.045(3) 0.041(3) 0.000(2) 0.0085(19) -0.0051(19) N12 0.036(2) 0.040(3) 0.046(3) 0.006(2) 0.0092(19) -0.007(2) C1 0.047(3) 0.032(3) 0.054(3) 0.000(2) 0.011(3) -0.004(2) C2 0.063(4) 0.040(3) 0.071(4) -0.002(3) 0.024(3) -0.009(3) C3 0.074(5) 0.048(4) 0.116(6) 0.004(4) 0.041(4) -0.008(4) C4 0.081(6) 0.050(4) 0.132(7) 0.004(4) 0.040(5) -0.026(4) C5 0.051(4) 0.084(6) 0.109(6) 0.004(4) 0.026(4) -0.022(4) C6 0.052(4) 0.060(4) 0.106(6) 0.003(4) 0.025(4) -0.009(3) C7 0.050(3) 0.042(3) 0.058(4) -0.008(3) 0.012(3) -0.007(3) C8 0.063(5) 0.042(4) 0.169(8) 0.007(4) 0.063(5) 0.004(3) C9 0.076(6) 0.116(8) 0.245(13) 0.104(9) 0.052(7) 0.041(6) C10 0.159(11) 0.074(6) 0.289(15) -0.084(8) 0.161(11) -0.043(6) C11 0.051(4) 0.040(3) 0.086(5) 0.001(3) 0.016(3) 0.008(3) C12 0.086(6) 0.084(6) 0.092(6) 0.013(4) -0.001(4) 0.028(5) C13 0.099(6) 0.057(5) 0.113(6) -0.013(4) 0.047(5) 0.012(4) C14 0.042(3) 0.035(3) 0.071(4) -0.008(3) 0.023(3) -0.002(2) C15 0.038(3) 0.048(4) 0.080(4) -0.019(3) 0.006(3) 0.003(3) C16 0.047(4) 0.060(4) 0.109(6) -0.039(4) -0.001(4) 0.001(3) C17 0.066(5) 0.081(6) 0.090(6) -0.046(4) 0.005(4) 0.012(4) C18 0.084(6) 0.096(6) 0.057(4) -0.022(4) 0.009(4) 0.023(5) C19 0.069(4) 0.062(4) 0.056(4) -0.012(3) 0.009(3) 0.013(3) C20 0.047(4) 0.052(4) 0.061(4) -0.015(3) 0.005(3) 0.010(3) C21 0.077(5) 0.056(5) 0.169(8) -0.023(5) 0.062(6) -0.031(4) C22 0.128(9) 0.061(6) 0.235(13) 0.040(7) 0.084(9) -0.004(6) C23 0.059(6) 0.098(8) 0.315(17) -0.026(9) 0.056(8) -0.038(5) C24 0.061(4) 0.031(3) 0.080(4) -0.005(3) 0.028(3) -0.001(3) C25 0.128(8) 0.045(4) 0.114(7) 0.004(4) 0.029(5) 0.014(4) C26 0.072(5) 0.059(4) 0.104(6) -0.015(4) 0.046(4) -0.015(4) C27 0.032(3) 0.035(3) 0.050(3) -0.002(2) 0.007(2) -0.001(2) C28 0.028(3) 0.049(3) 0.059(3) -0.008(3) 0.009(2) 0.002(2) C29 0.034(3) 0.052(4) 0.088(5) -0.009(3) 0.011(3) -0.006(3) C30 0.029(3) 0.085(6) 0.103(6) -0.022(4) -0.002(3) 0.006(3) C31 0.040(4) 0.075(5) 0.083(5) 0.000(4) -0.001(3) 0.016(3) C32 0.045(3) 0.057(4) 0.069(4) 0.005(3) 0.010(3) 0.015(3) C33 0.035(3) 0.039(3) 0.058(3) -0.008(2) 0.011(2) 0.005(2) C34 0.035(3) 0.039(3) 0.083(4) 0.003(3) 0.003(3) -0.002(2) C35 0.069(5) 0.041(4) 0.114(6) -0.019(4) 0.015(4) -0.003(3) C36 0.061(4) 0.067(5) 0.105(6) 0.021(4) 0.030(4) -0.004(4) C37 0.048(4) 0.036(3) 0.100(5) -0.003(3) 0.010(3) 0.000(3) C38 0.061(4) 0.065(4) 0.090(5) 0.015(4) 0.023(4) -0.005(3) C39 0.092(6) 0.042(4) 0.125(7) -0.021(4) 0.018(5) -0.013(4) C40 0.031(3) 0.042(3) 0.046(3) 0.004(2) 0.008(2) -0.003(2) C41 0.033(3) 0.046(3) 0.044(3) 0.005(2) 0.009(2) -0.004(2) C42 0.048(3) 0.051(4) 0.057(4) 0.001(3) 0.011(3) 0.008(3) C43 0.046(4) 0.065(4) 0.067(4) 0.008(3) -0.002(3) 0.010(3) C44 0.049(4) 0.063(4) 0.053(4) 0.007(3) -0.001(3) 0.000(3) C45 0.044(3) 0.046(3) 0.055(3) -0.001(3) 0.006(3) -0.007(3) C46 0.041(3) 0.041(3) 0.048(3) 0.003(2) 0.008(2) -0.001(2) C47 0.052(4) 0.061(4) 0.051(3) -0.007(3) 0.009(3) 0.009(3) C48 0.123(7) 0.061(5) 0.073(5) -0.018(4) 0.013(5) 0.014(5) C49 0.073(5) 0.137(8) 0.059(4) -0.003(4) 0.029(4) 0.005(5) C50 0.039(3) 0.059(4) 0.053(3) -0.002(3) 0.015(3) -0.001(3) C51 0.060(4) 0.049(4) 0.084(4) -0.008(3) 0.039(3) 0.003(3) C52 0.074(5) 0.065(4) 0.092(5) -0.006(4) 0.049(4) -0.011(4) C53 0.058(4) 0.033(3) 0.070(4) -0.005(3) 0.025(3) 0.000(3) C54 0.044(3) 0.041(3) 0.070(4) -0.002(3) 0.025(3) 0.002(3) C55 0.035(3) 0.041(3) 0.046(3) 0.008(2) 0.003(2) 0.003(2) C56 0.054(4) 0.043(3) 0.046(3) -0.002(2) 0.010(3) -0.008(3) C57 0.046(3) 0.047(3) 0.046(3) -0.001(2) 0.016(2) -0.007(3) C58 0.037(3) 0.041(3) 0.053(3) 0.003(2) 0.009(2) 0.001(2) C59 0.029(3) 0.054(3) 0.048(3) 0.001(2) 0.008(2) -0.013(2) C60 0.038(3) 0.046(3) 0.044(3) 0.005(2) 0.007(2) -0.012(2) C61 0.043(3) 0.040(3) 0.051(3) 0.009(2) 0.002(2) 0.001(2) C62 0.039(3) 0.051(4) 0.078(4) 0.002(3) 0.025(3) -0.004(3) C63 0.041(3) 0.045(3) 0.067(4) -0.004(3) 0.014(3) -0.003(3) C64 0.041(3) 0.029(3) 0.063(4) 0.008(2) 0.013(3) 0.008(2) C65 0.041(3) 0.047(3) 0.069(4) 0.002(3) 0.022(3) -0.004(3) C66 0.041(3) 0.047(3) 0.074(4) -0.008(3) 0.021(3) -0.005(3) N2S 0.116(7) 0.083(6) 0.163(8) -0.015(5) 0.053(6) -0.043(5) C3S 0.080(6) 0.071(6) 0.153(9) -0.034(6) 0.053(6) -0.032(5) C4S 0.137(9) 0.129(9) 0.128(9) -0.056(7) 0.050(7) -0.014(7) N3S 0.174(10) 0.124(7) 0.081(6) -0.027(5) 0.026(6) 0.032(7) C5S 0.138(10) 0.073(6) 0.080(6) -0.003(5) 0.033(6) -0.010(6) C6S 0.122(9) 0.131(9) 0.106(7) 0.022(6) 0.025(6) -0.023(7) N1SA 0.083(9) 0.088(9) 0.050(6) 0.009(6) 0.023(6) -0.042(7) C1SA 0.087(10) 0.093(10) 0.029(6) 0.007(6) 0.025(6) -0.045(9) C2SA 0.119(13) 0.160(16) 0.048(8) -0.027(9) 0.060(9) -0.092(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.944(5) . ? Pd1 N9 2.120(4) . ? Pd1 Br1 2.4248(8) . ? Pd1 Br2 2.4263(8) . ? Pd2 C14 1.949(6) . ? Pd2 N10 2.102(4) . ? Pd2 Br3 2.4323(8) . ? Pd2 Br4 2.4407(8) . ? Pd3 C27 1.955(5) . ? Pd3 N11 2.132(4) . ? Pd3 Br5 2.4274(7) . ? Pd3 Br6 2.4441(7) . ? Pd4 C40 1.954(5) . ? Pd4 N12 2.138(4) . ? Pd4 Br8 2.4300(7) . ? Pd4 Br7 2.4444(7) . ? N1 C1 1.346(7) . ? N1 C2 1.410(7) . ? N1 C8 1.472(8) . ? N2 C1 1.362(7) . ? N2 C7 1.394(7) . ? N2 C11 1.494(7) . ? N3 C14 1.358(7) . ? N3 C15 1.390(8) . ? N3 C21 1.500(9) . ? N4 C14 1.338(7) . ? N4 C20 1.401(7) . ? N4 C24 1.470(7) . ? N5 C27 1.354(6) . ? N5 C28 1.406(7) . ? N5 C34 1.472(7) . ? N6 C27 1.328(6) . ? N6 C33 1.399(6) . ? N6 C37 1.488(7) . ? N7 C40 1.352(6) . ? N7 C41 1.393(6) . ? N7 C47 1.476(7) . ? N8 C40 1.328(6) . ? N8 C46 1.397(6) . ? N8 C50 1.479(7) . ? N9 C53 1.326(7) . ? N9 C57 1.340(7) . ? N10 C66 1.332(7) . ? N10 C62 1.340(7) . ? N11 C58 1.477(7) . ? N11 C59 1.493(6) . ? N12 C60 1.478(7) . ? N12 C61 1.490(7) . ? C2 C7 1.365(8) . ? C2 C3 1.389(8) . ? C3 C4 1.388(10) . ? C4 C5 1.352(10) . ? C5 C6 1.383(10) . ? C6 C7 1.397(8) . ? C8 C9 1.510(12) . ? C8 C10 1.524(12) . ? C11 C12 1.502(9) . ? C11 C13 1.503(9) . ? C15 C20 1.353(9) . ? C15 C16 1.392(8) . ? C16 C17 1.345(11) . ? C17 C18 1.377(11) . ? C18 C19 1.365(9) . ? C19 C20 1.414(9) . ? C21 C22 1.521(12) . ? C21 C23 1.552(13) . ? C24 C25 1.517(9) . ? C24 C26 1.542(9) . ? C28 C33 1.364(8) . ? C28 C29 1.382(7) . ? C29 C30 1.386(9) . ? C30 C31 1.370(10) . ? C31 C32 1.375(9) . ? C32 C33 1.403(7) . ? C34 C36 1.504(9) . ? C34 C35 1.506(8) . ? C37 C38 1.516(9) . ? C37 C39 1.519(9) . ? C41 C42 1.388(7) . ? C41 C46 1.393(7) . ? C42 C43 1.381(8) . ? C43 C44 1.383(9) . ? C44 C45 1.361(8) . ? C45 C46 1.397(7) . ? C47 C49 1.517(9) . ? C47 C48 1.535(9) . ? C50 C51 1.514(8) . ? C50 C52 1.519(8) . ? C53 C54 1.396(8) . ? C54 C55 1.376(8) . ? C55 C56 1.397(8) . ? C55 C58 1.502(7) . ? C56 C57 1.365(7) . ? C59 C60 1.498(8) . ? C61 C64 1.494(8) . ? C62 C63 1.373(8) . ? C63 C64 1.382(7) . ? C64 C65 1.390(8) . ? C65 C66 1.392(8) . ? N2S C3S 1.170(11) . ? C3S C4S 1.403(13) . ? N3S C5S 1.092(12) . ? C5S C6S 1.463(14) . ? N4S C7S 1.175(7) . ? C7S C8S 1.533(7) . ? N5S C9S 1.137(8) . ? C9S C10S 1.556(8) . ? N1SA C1SA 1.043(15) . ? C1SA C2SA 1.430(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N9 177.4(2) . . ? C1 Pd1 Br1 86.39(16) . . ? N9 Pd1 Br1 92.66(12) . . ? C1 Pd1 Br2 86.57(16) . . ? N9 Pd1 Br2 94.46(12) . . ? Br1 Pd1 Br2 172.60(3) . . ? C14 Pd2 N10 178.8(2) . . ? C14 Pd2 Br3 86.85(17) . . ? N10 Pd2 Br3 92.96(13) . . ? C14 Pd2 Br4 87.99(17) . . ? N10 Pd2 Br4 92.19(13) . . ? Br3 Pd2 Br4 174.85(3) . . ? C27 Pd3 N11 179.1(2) . . ? C27 Pd3 Br5 88.83(15) . . ? N11 Pd3 Br5 91.98(13) . . ? C27 Pd3 Br6 87.94(15) . . ? N11 Pd3 Br6 91.26(13) . . ? Br5 Pd3 Br6 176.57(3) . . ? C40 Pd4 N12 177.3(2) . . ? C40 Pd4 Br8 88.27(15) . . ? N12 Pd4 Br8 93.88(12) . . ? C40 Pd4 Br7 87.71(15) . . ? N12 Pd4 Br7 90.11(12) . . ? Br8 Pd4 Br7 175.77(3) . . ? C1 N1 C2 109.3(5) . . ? C1 N1 C8 122.9(5) . . ? C2 N1 C8 127.8(5) . . ? C1 N2 C7 109.1(5) . . ? C1 N2 C11 121.9(5) . . ? C7 N2 C11 128.6(5) . . ? C14 N3 C15 110.4(5) . . ? C14 N3 C21 121.0(6) . . ? C15 N3 C21 128.4(5) . . ? C14 N4 C20 108.8(5) . . ? C14 N4 C24 122.3(5) . . ? C20 N4 C24 128.9(5) . . ? C27 N5 C28 108.6(4) . . ? C27 N5 C34 123.6(4) . . ? C28 N5 C34 127.7(4) . . ? C27 N6 C33 109.8(4) . . ? C27 N6 C37 122.7(4) . . ? C33 N6 C37 127.5(5) . . ? C40 N7 C41 109.8(4) . . ? C40 N7 C47 123.3(4) . . ? C41 N7 C47 126.8(5) . . ? C40 N8 C46 110.2(4) . . ? C40 N8 C50 122.8(4) . . ? C46 N8 C50 126.8(4) . . ? C53 N9 C57 116.5(5) . . ? C53 N9 Pd1 122.6(4) . . ? C57 N9 Pd1 120.9(4) . . ? C66 N10 C62 117.2(5) . . ? C66 N10 Pd2 119.0(4) . . ? C62 N10 Pd2 123.6(4) . . ? C58 N11 C59 110.7(4) . . ? C58 N11 Pd3 114.8(3) . . ? C59 N11 Pd3 111.8(3) . . ? C60 N12 C61 110.1(4) . . ? C60 N12 Pd4 111.1(3) . . ? C61 N12 Pd4 116.4(3) . . ? N1 C1 N2 107.6(5) . . ? N1 C1 Pd1 127.6(4) . . ? N2 C1 Pd1 124.8(4) . . ? C7 C2 C3 121.7(6) . . ? C7 C2 N1 106.6(5) . . ? C3 C2 N1 131.7(6) . . ? C4 C3 C2 116.8(7) . . ? C5 C4 C3 121.7(7) . . ? C4 C5 C6 121.9(7) . . ? C5 C6 C7 117.0(7) . . ? C2 C7 N2 107.4(5) . . ? C2 C7 C6 120.9(6) . . ? N2 C7 C6 131.7(6) . . ? N1 C8 C9 111.0(7) . . ? N1 C8 C10 108.8(7) . . ? C9 C8 C10 117.1(8) . . ? N2 C11 C12 109.6(5) . . ? N2 C11 C13 111.2(5) . . ? C12 C11 C13 113.7(6) . . ? N4 C14 N3 106.9(5) . . ? N4 C14 Pd2 126.6(4) . . ? N3 C14 Pd2 126.5(4) . . ? C20 C15 N3 105.5(5) . . ? C20 C15 C16 121.3(7) . . ? N3 C15 C16 133.2(7) . . ? C17 C16 C15 117.6(7) . . ? C16 C17 C18 121.2(7) . . ? C19 C18 C17 123.3(8) . . ? C18 C19 C20 114.9(7) . . ? C15 C20 N4 108.3(6) . . ? C15 C20 C19 121.8(6) . . ? N4 C20 C19 129.8(6) . . ? N3 C21 C22 109.3(6) . . ? N3 C21 C23 107.5(8) . . ? C22 C21 C23 116.6(7) . . ? N4 C24 C25 111.3(5) . . ? N4 C24 C26 109.8(5) . . ? C25 C24 C26 113.4(6) . . ? N6 C27 N5 108.2(4) . . ? N6 C27 Pd3 127.4(4) . . ? N5 C27 Pd3 124.4(4) . . ? C33 C28 C29 122.2(5) . . ? C33 C28 N5 106.8(4) . . ? C29 C28 N5 131.0(5) . . ? C28 C29 C30 116.2(6) . . ? C31 C30 C29 122.2(6) . . ? C30 C31 C32 121.3(6) . . ? C31 C32 C33 116.8(6) . . ? C28 C33 N6 106.7(4) . . ? C28 C33 C32 121.1(5) . . ? N6 C33 C32 132.2(5) . . ? N5 C34 C36 112.4(5) . . ? N5 C34 C35 110.8(5) . . ? C36 C34 C35 113.3(6) . . ? N6 C37 C38 111.2(5) . . ? N6 C37 C39 109.6(5) . . ? C38 C37 C39 113.1(6) . . ? N8 C40 N7 107.7(4) . . ? N8 C40 Pd4 126.7(4) . . ? N7 C40 Pd4 125.6(4) . . ? C42 C41 C46 121.1(5) . . ? C42 C41 N7 132.9(5) . . ? C46 C41 N7 105.9(5) . . ? C43 C42 C41 117.5(6) . . ? C42 C43 C44 120.8(6) . . ? C45 C44 C43 122.7(6) . . ? C44 C45 C46 117.1(6) . . ? C41 C46 C45 120.7(5) . . ? C41 C46 N8 106.2(4) . . ? C45 C46 N8 133.1(5) . . ? N7 C47 C49 110.8(5) . . ? N7 C47 C48 110.8(5) . . ? C49 C47 C48 115.1(6) . . ? N8 C50 C51 111.7(4) . . ? N8 C50 C52 111.3(5) . . ? C51 C50 C52 113.1(5) . . ? N9 C53 C54 123.2(5) . . ? C55 C54 C53 120.2(5) . . ? C54 C55 C56 116.0(5) . . ? C54 C55 C58 121.0(5) . . ? C56 C55 C58 122.9(5) . . ? C57 C56 C55 120.2(5) . . ? N9 C57 C56 123.8(5) . . ? N11 C58 C55 112.9(4) . . ? N11 C59 C60 113.6(4) . . ? N12 C60 C59 114.2(4) . . ? N12 C61 C64 112.6(4) . . ? N10 C62 C63 123.6(5) . . ? C62 C63 C64 120.0(5) . . ? C63 C64 C65 116.5(5) . . ? C63 C64 C61 122.4(5) . . ? C65 C64 C61 121.1(5) . . ? C64 C65 C66 120.3(5) . . ? N10 C66 C65 122.4(5) . . ? N2S C3S C4S 174.8(11) . . ? N3S C5S C6S 178.0(12) . . ? N4S C7S C8S 162.8(17) . . ? N5S C9S C10S 176(5) . . ? N1SA C1SA C2SA 178(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.187 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.117 # Attachment '- Complex4.cif' data_9441a _database_code_depnum_ccdc_archive 'CCDC 837384' #TrackingRef '- Complex4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H103 B2 Br4 F8 N13 O8 Pd2' _chemical_formula_weight 2104.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.8574(15) _cell_length_b 12.0368(9) _cell_length_c 17.6400(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.218(2) _cell_angle_gamma 90.00 _cell_volume 4628.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7176 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.28 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 2.189 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6445 _exptl_absorpt_correction_T_max 0.8443 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32347 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10636 _reflns_number_gt 7959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0619P)^2^+0.3252P] 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 10636 _refine_ls_number_parameters 595 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.152082(10) 0.498421(18) 0.189652(13) 0.02146(7) Uani 1 1 d . . . Br1 Br 0.101427(15) 0.33294(3) 0.137087(19) 0.03132(9) Uani 1 1 d . . . Br2 Br 0.202797(16) 0.67579(3) 0.22042(2) 0.03688(10) Uani 1 1 d . . . N1 N 0.07358(11) 0.6347(2) 0.07956(14) 0.0242(5) Uani 1 1 d . . . N2 N 0.03643(11) 0.6157(2) 0.19040(14) 0.0270(6) Uani 1 1 d . . . N3 N 0.22216(11) 0.4076(2) 0.24961(14) 0.0227(5) Uani 1 1 d . . . N4 N 0.46059(10) 0.1219(2) 0.45390(13) 0.0204(5) Uani 1 1 d . . . O1 O 0.34231(10) -0.00857(17) 0.54240(13) 0.0286(5) Uani 1 1 d . . . O2 O 0.43623(11) 0.0282(2) 0.67215(14) 0.0430(6) Uani 1 1 d . B . O4 O 0.64524(11) 0.1064(2) 0.58795(14) 0.0419(6) Uani 1 1 d D . . C1 C 0.08209(13) 0.5856(3) 0.14780(17) 0.0253(7) Uani 1 1 d . . . C2 C 0.02158(14) 0.7031(3) 0.07882(18) 0.0254(7) Uani 1 1 d . . . C3 C -0.00574(15) 0.7741(3) 0.02412(19) 0.0317(7) Uani 1 1 d . . . H3 H 0.0099 0.7819 -0.0244 0.038 Uiso 1 1 calc R . . C4 C -0.05673(16) 0.8330(3) 0.0436(2) 0.0375(8) Uani 1 1 d . . . H4 H -0.0764 0.8823 0.0075 0.045 Uiso 1 1 calc R . . C5 C -0.08003(16) 0.8220(3) 0.1144(2) 0.0386(9) Uani 1 1 d . . . H5 H -0.1150 0.8641 0.1255 0.046 Uiso 1 1 calc R . . C6 C -0.05342(15) 0.7513(3) 0.16897(19) 0.0345(8) Uani 1 1 d . . . H6 H -0.0695 0.7436 0.2173 0.041 Uiso 1 1 calc R . . C7 C -0.00216(14) 0.6917(3) 0.15017(18) 0.0277(7) Uani 1 1 d . . . C8 C 0.11212(14) 0.6116(3) 0.01595(18) 0.0304(7) Uani 1 1 d . . . H8 H 0.1431 0.5546 0.0343 0.037 Uiso 1 1 calc R . . C9 C 0.14728(16) 0.7147(3) -0.0042(2) 0.0445(9) Uani 1 1 d . . . H9A H 0.1184 0.7723 -0.0230 0.067 Uiso 1 1 calc R . . H9B H 0.1749 0.6964 -0.0437 0.067 Uiso 1 1 calc R . . H9C H 0.1713 0.7419 0.0411 0.067 Uiso 1 1 calc R . . C10 C 0.07385(15) 0.5605(3) -0.05040(19) 0.0350(8) Uani 1 1 d . . . H10A H 0.0558 0.4907 -0.0342 0.052 Uiso 1 1 calc R . . H10B H 0.1000 0.5458 -0.0921 0.052 Uiso 1 1 calc R . . H10C H 0.0411 0.6122 -0.0678 0.052 Uiso 1 1 calc R . . C11 C 0.03003(16) 0.5720(3) 0.26782(19) 0.0400(9) Uani 1 1 d . . . H11 H 0.0614 0.5118 0.2758 0.048 Uiso 1 1 calc R . . C12 C -0.03100(19) 0.5175(4) 0.2743(2) 0.0564(12) Uani 1 1 d . . . H12A H -0.0633 0.5741 0.2709 0.085 Uiso 1 1 calc R . . H12B H -0.0311 0.4791 0.3233 0.085 Uiso 1 1 calc R . . H12C H -0.0385 0.4637 0.2330 0.085 Uiso 1 1 calc R . . C13 C 0.0467(2) 0.6589(4) 0.3269(2) 0.0585(13) Uani 1 1 d . . . H13A H 0.0859 0.6932 0.3164 0.088 Uiso 1 1 calc R . . H13B H 0.0505 0.6243 0.3773 0.088 Uiso 1 1 calc R . . H13C H 0.0147 0.7159 0.3255 0.088 Uiso 1 1 calc R . . C15 C 0.24466(14) 0.4445(3) 0.31867(17) 0.0249(6) Uani 1 1 d . . . H15 H 0.2286 0.5112 0.3380 0.030 Uiso 1 1 calc R . . C16 C 0.29004(13) 0.3890(3) 0.36212(17) 0.0243(6) Uani 1 1 d . . . H16 H 0.3047 0.4172 0.4104 0.029 Uiso 1 1 calc R . . C17 C 0.31412(13) 0.2914(2) 0.33446(16) 0.0206(6) Uani 1 1 d . . . C18 C 0.28933(13) 0.2519(2) 0.26425(17) 0.0222(6) Uani 1 1 d . . . H18 H 0.3035 0.1840 0.2443 0.027 Uiso 1 1 calc R . . C19 C 0.24425(13) 0.3122(2) 0.22445(17) 0.0237(6) Uani 1 1 d . . . H19 H 0.2280 0.2847 0.1767 0.028 Uiso 1 1 calc R . . C20 C 0.42491(14) 0.1898(2) 0.49229(17) 0.0226(6) Uani 1 1 d . . . H20 H 0.4328 0.1991 0.5456 0.027 Uiso 1 1 calc R . . C21 C 0.37721(13) 0.2453(2) 0.45457(17) 0.0224(6) Uani 1 1 d . . . H21 H 0.3522 0.2933 0.4818 0.027 Uiso 1 1 calc R . . C22 C 0.36521(13) 0.2321(2) 0.37673(16) 0.0193(6) Uani 1 1 d . . . C23 C 0.40320(13) 0.1610(2) 0.33904(17) 0.0225(6) Uani 1 1 d . . . H23 H 0.3962 0.1495 0.2858 0.027 Uiso 1 1 calc R . . C24 C 0.45042(14) 0.1079(2) 0.37875(17) 0.0241(6) Uani 1 1 d . . . H24 H 0.4765 0.0604 0.3527 0.029 Uiso 1 1 calc R . . C25 C 0.51076(13) 0.0591(3) 0.49508(18) 0.0248(7) Uani 1 1 d . . . H25A H 0.5213 0.0934 0.5454 0.030 Uiso 1 1 calc R . . H25B H 0.5477 0.0600 0.4659 0.030 Uiso 1 1 calc R . . C26 C 0.21391(18) 0.0534(4) 0.3625(2) 0.0525(11) Uani 1 1 d . . . H26 H 0.1848 0.0660 0.3207 0.063 Uiso 1 1 calc R . . C27 C 0.20716(16) 0.1068(3) 0.4303(3) 0.0471(10) Uani 1 1 d . . . H27 H 0.1739 0.1566 0.4351 0.057 Uiso 1 1 calc R . . C28 C 0.24953(15) 0.0871(3) 0.4920(2) 0.0362(8) Uani 1 1 d . . . H28 H 0.2450 0.1235 0.5391 0.043 Uiso 1 1 calc R . . C29 C 0.29841(14) 0.0147(3) 0.4850(2) 0.0290(7) Uani 1 1 d . . . C30 C 0.32988(15) 0.0290(3) 0.61720(19) 0.0293(7) Uani 1 1 d . . . H30A H 0.2883 0.0050 0.6291 0.035 Uiso 1 1 calc R . . H30B H 0.3315 0.1112 0.6194 0.035 Uiso 1 1 calc R . . C31 C 0.37696(17) -0.0193(3) 0.6740(2) 0.0378(8) Uani 1 1 d . . . H31A H 0.3628 -0.0092 0.7256 0.045 Uiso 1 1 calc R . . H31B H 0.3800 -0.1001 0.6646 0.045 Uiso 1 1 calc R . . C32 C 0.44562(16) 0.1238(3) 0.7190(2) 0.0415(9) Uani 1 1 d D . . H32A H 0.4332 0.1071 0.7706 0.050 Uiso 1 1 calc R A 1 H32B H 0.4196 0.1854 0.6979 0.050 Uiso 1 1 calc R A 1 C33 C 0.5114(2) 0.1593(9) 0.7239(4) 0.048(2) Uani 0.710(8) 1 d PD B 1 H33A H 0.5165 0.2262 0.7564 0.058 Uiso 0.710(8) 1 calc PR B 1 H33B H 0.5373 0.0994 0.7476 0.058 Uiso 0.710(8) 1 calc PR B 1 O3 O 0.53044(18) 0.1830(4) 0.6519(3) 0.0446(11) Uani 0.710(8) 1 d PD B 1 C34 C 0.5880(2) 0.2382(5) 0.6520(3) 0.0497(18) Uani 0.710(8) 1 d PD B 1 H34A H 0.5907 0.2935 0.6937 0.060 Uiso 0.710(8) 1 calc PR B 1 H34B H 0.5895 0.2793 0.6036 0.060 Uiso 0.710(8) 1 calc PR B 1 C35 C 0.6432(2) 0.1637(5) 0.6614(3) 0.0419(15) Uani 0.710(8) 1 d PD B 1 H35A H 0.6810 0.2078 0.6729 0.050 Uiso 0.710(8) 1 calc PR B 1 H35B H 0.6389 0.1096 0.7029 0.050 Uiso 0.710(8) 1 calc PR B 1 C33A C 0.5121(4) 0.135(2) 0.7411(8) 0.038(5) Uiso 0.290(8) 1 d PD B 2 H33C H 0.5184 0.1984 0.7765 0.045 Uiso 0.290(8) 1 calc PR B 2 H33D H 0.5264 0.0669 0.7686 0.045 Uiso 0.290(8) 1 calc PR B 2 O3A O 0.5478(4) 0.1512(8) 0.6792(6) 0.029(2) Uiso 0.290(8) 1 d PD B 2 C34A C 0.6087(5) 0.1814(10) 0.6998(7) 0.036(3) Uiso 0.290(8) 1 d PD B 2 H34C H 0.6296 0.1199 0.7285 0.044 Uiso 0.290(8) 1 calc PR B 2 H34D H 0.6092 0.2474 0.7333 0.044 Uiso 0.290(8) 1 calc PR B 2 C35A C 0.6426(6) 0.2071(8) 0.6317(7) 0.034(3) Uiso 0.290(8) 1 d PD B 2 H35C H 0.6210 0.2660 0.6009 0.041 Uiso 0.290(8) 1 calc PR B 2 H35D H 0.6845 0.2333 0.6474 0.041 Uiso 0.290(8) 1 calc PR B 2 C36 C 0.69491(16) 0.0385(3) 0.5851(2) 0.0377(8) Uani 1 1 d . . . C37 C 0.73791(18) 0.0177(4) 0.6455(2) 0.0502(11) Uani 1 1 d . . . H37 H 0.7339 0.0533 0.6929 0.060 Uiso 1 1 calc R B . B1 B 0.3503(4) 0.0861(6) 0.1160(4) 0.0384(18) Uani 0.710(8) 1 d PD B 1 F1 F 0.4033(3) 0.1353(5) 0.1355(3) 0.0782(19) Uani 0.710(8) 1 d PD B 1 F3 F 0.3036(3) 0.1660(4) 0.0994(3) 0.0608(15) Uani 0.710(8) 1 d PD B 1 F2 F 0.35763(11) 0.02777(16) 0.04891(12) 0.0466(6) Uani 1 1 d D . . F4 F 0.33251(11) 0.01497(17) 0.17160(13) 0.0494(6) Uani 1 1 d D . . B1A B 0.3672(8) 0.0791(14) 0.1224(9) 0.0384(18) Uani 0.290(8) 1 d PD B 2 F1A F 0.4266(6) 0.0926(12) 0.1579(7) 0.058(3) Uani 0.290(8) 1 d PD B 2 F3A F 0.3402(6) 0.1864(7) 0.1179(5) 0.040(3) Uani 0.290(8) 1 d PD B 2 N1S N 0.5720(4) 1.0133(7) 0.1200(5) 0.070(2) Uani 0.50 1 d P C -1 C1S C 0.5396(4) 1.0076(7) 0.0664(6) 0.050(2) Uani 0.50 1 d PD C -1 C2S C 0.4959(16) 0.993(4) 0.0031(19) 0.044(5) Uani 0.50 1 d PD C -1 H2S1 H 0.5055 1.0437 -0.0379 0.066 Uiso 0.50 1 calc PR C -1 H2S2 H 0.4547 1.0092 0.0186 0.066 Uiso 0.50 1 calc PR C -1 H2S3 H 0.4975 0.9162 -0.0150 0.066 Uiso 0.50 1 calc PR C -1 N2S N 0.19005(19) -0.0093(3) -0.0180(2) 0.0664(11) Uani 1 1 d . . . C3S C 0.18718(19) -0.0017(3) 0.0454(3) 0.0532(11) Uani 1 1 d . . . C4S C 0.1830(2) 0.0064(4) 0.1277(3) 0.0734(15) Uani 1 1 d . . . H4S1 H 0.1637 -0.0609 0.1461 0.110 Uiso 1 1 calc R . . H4S2 H 0.1583 0.0713 0.1392 0.110 Uiso 1 1 calc R . . H4S3 H 0.2243 0.0141 0.1529 0.110 Uiso 1 1 calc R . . N3S N 0.43204(14) 0.7753(2) 0.0814(2) 0.0445(8) Uani 1 1 d . . . C5S C 0.38035(17) 0.7813(3) 0.0689(2) 0.0380(8) Uani 1 1 d . . . C6S C 0.31413(17) 0.7855(3) 0.0554(3) 0.0519(11) Uani 1 1 d . . . H6S1 H 0.2989 0.7131 0.0370 0.078 Uiso 1 1 calc R . . H6S2 H 0.3029 0.8425 0.0171 0.078 Uiso 1 1 calc R . . H6S3 H 0.2958 0.8039 0.1028 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01723(12) 0.02794(13) 0.01863(12) 0.00218(9) -0.00258(8) 0.00406(9) Br1 0.02607(17) 0.03611(19) 0.03076(18) 0.00218(13) -0.00478(14) -0.00290(13) Br2 0.0371(2) 0.03085(18) 0.0404(2) 0.00242(14) -0.01274(16) -0.00019(14) N1 0.0199(12) 0.0311(14) 0.0209(13) 0.0042(10) -0.0035(10) 0.0035(11) N2 0.0234(13) 0.0376(15) 0.0190(13) 0.0002(11) -0.0043(11) 0.0104(11) N3 0.0187(12) 0.0307(14) 0.0181(12) 0.0016(10) -0.0024(10) 0.0033(10) N4 0.0169(12) 0.0242(13) 0.0196(12) 0.0062(10) -0.0019(10) 0.0033(10) O1 0.0263(11) 0.0318(12) 0.0278(12) -0.0028(9) 0.0023(10) 0.0043(9) O2 0.0341(14) 0.0616(17) 0.0329(14) -0.0207(12) -0.0010(11) 0.0121(12) O4 0.0336(13) 0.0528(16) 0.0398(15) -0.0213(12) 0.0063(11) -0.0068(12) C1 0.0214(15) 0.0311(17) 0.0228(16) -0.0025(12) -0.0037(13) 0.0044(13) C2 0.0237(15) 0.0269(16) 0.0247(16) -0.0009(12) -0.0037(13) 0.0030(12) C3 0.0325(18) 0.0365(18) 0.0246(16) 0.0024(14) -0.0083(14) 0.0044(14) C4 0.0352(19) 0.0344(19) 0.040(2) -0.0018(15) -0.0159(16) 0.0110(15) C5 0.0305(18) 0.042(2) 0.042(2) -0.0157(16) -0.0108(16) 0.0157(15) C6 0.0286(17) 0.049(2) 0.0247(17) -0.0116(15) -0.0056(14) 0.0109(15) C7 0.0232(16) 0.0340(17) 0.0239(16) -0.0075(13) -0.0108(13) 0.0065(13) C8 0.0208(15) 0.0439(19) 0.0267(17) 0.0069(14) 0.0023(13) 0.0065(14) C9 0.0308(19) 0.063(3) 0.039(2) 0.0148(19) 0.0003(17) -0.0057(18) C10 0.0307(18) 0.051(2) 0.0236(17) -0.0033(15) 0.0016(14) 0.0066(16) C11 0.0347(19) 0.066(3) 0.0193(17) 0.0044(16) -0.0002(15) 0.0167(18) C12 0.043(2) 0.091(3) 0.036(2) 0.022(2) 0.0103(19) 0.010(2) C13 0.060(3) 0.089(3) 0.026(2) -0.013(2) -0.0068(19) 0.029(2) C15 0.0244(15) 0.0279(16) 0.0218(15) -0.0005(12) -0.0021(13) 0.0067(13) C16 0.0226(15) 0.0312(16) 0.0185(15) -0.0008(12) -0.0030(12) 0.0044(13) C17 0.0192(14) 0.0240(15) 0.0187(14) 0.0029(11) 0.0016(12) 0.0005(11) C18 0.0212(14) 0.0247(15) 0.0206(15) 0.0004(11) 0.0017(12) 0.0036(12) C19 0.0242(15) 0.0272(16) 0.0195(15) -0.0002(12) -0.0007(12) -0.0016(12) C20 0.0260(15) 0.0243(15) 0.0171(14) -0.0007(11) -0.0013(12) 0.0016(12) C21 0.0222(15) 0.0216(15) 0.0235(15) -0.0011(12) 0.0017(13) 0.0066(12) C22 0.0198(14) 0.0180(14) 0.0203(14) 0.0025(11) 0.0020(12) -0.0003(11) C23 0.0251(15) 0.0261(15) 0.0163(13) 0.0001(12) 0.0015(12) 0.0037(12) C24 0.0251(15) 0.0255(15) 0.0223(15) 0.0033(12) 0.0066(13) 0.0080(12) C25 0.0183(15) 0.0284(16) 0.0268(16) 0.0048(12) -0.0039(13) 0.0060(12) C26 0.033(2) 0.079(3) 0.044(2) 0.024(2) -0.0092(18) -0.014(2) C27 0.0252(18) 0.049(2) 0.066(3) 0.023(2) -0.0026(19) -0.0011(16) C28 0.0277(17) 0.039(2) 0.042(2) 0.0053(16) 0.0044(16) -0.0017(15) C29 0.0219(15) 0.0310(17) 0.0341(18) 0.0048(13) 0.0011(14) -0.0061(13) C30 0.0271(17) 0.0306(17) 0.0311(17) -0.0047(13) 0.0071(14) 0.0012(13) C31 0.044(2) 0.041(2) 0.0292(18) -0.0022(15) 0.0046(16) 0.0079(16) C32 0.042(2) 0.054(2) 0.0287(19) -0.0153(16) 0.0047(16) 0.0107(18) C33 0.042(4) 0.069(7) 0.032(4) -0.019(4) -0.006(3) 0.010(3) O3 0.038(2) 0.060(3) 0.036(2) -0.019(2) 0.0035(19) 0.011(2) C34 0.058(4) 0.050(4) 0.042(3) -0.021(3) 0.011(3) -0.004(3) C35 0.051(3) 0.055(4) 0.021(3) -0.012(3) 0.007(2) -0.017(3) C36 0.0301(18) 0.050(2) 0.0333(19) -0.0006(16) 0.0028(15) -0.0132(16) C37 0.038(2) 0.081(3) 0.032(2) 0.0058(19) 0.0002(17) -0.023(2) B1 0.059(5) 0.024(2) 0.037(3) 0.0005(19) 0.028(3) 0.005(3) F1 0.103(5) 0.084(4) 0.048(3) -0.012(3) 0.006(3) -0.044(4) F3 0.107(4) 0.042(2) 0.037(2) 0.0055(17) 0.027(3) 0.026(3) F2 0.0773(16) 0.0299(11) 0.0352(12) -0.0004(9) 0.0212(11) 0.0076(10) F4 0.0712(16) 0.0399(12) 0.0395(12) 0.0093(9) 0.0205(12) 0.0030(10) B1A 0.059(5) 0.024(2) 0.037(3) 0.0005(19) 0.028(3) 0.005(3) F1A 0.063(7) 0.076(9) 0.035(6) 0.001(5) -0.001(5) -0.021(6) F3A 0.070(7) 0.028(4) 0.024(4) -0.002(3) 0.018(5) 0.005(5) N1S 0.068(6) 0.082(6) 0.060(5) 0.018(4) 0.003(5) 0.013(5) C1S 0.044(5) 0.050(5) 0.058(5) 0.013(4) 0.014(4) 0.007(4) C2S 0.033(8) 0.040(9) 0.062(6) 0.020(7) 0.016(6) -0.009(7) N2S 0.074(3) 0.071(3) 0.056(3) 0.021(2) 0.016(2) 0.015(2) C3S 0.043(2) 0.055(3) 0.063(3) 0.017(2) 0.012(2) 0.0152(19) C4S 0.064(3) 0.100(4) 0.059(3) -0.001(3) 0.022(3) 0.015(3) N3S 0.0364(18) 0.0328(17) 0.064(2) -0.0009(15) 0.0038(16) 0.0030(14) C5S 0.041(2) 0.0238(17) 0.049(2) 0.0002(15) 0.0054(18) 0.0037(15) C6S 0.037(2) 0.039(2) 0.079(3) -0.010(2) -0.001(2) 0.0026(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.955(3) . ? Pd1 N3 2.103(2) . ? Pd1 Br1 2.4295(4) . ? Pd1 Br2 2.4481(4) . ? N1 C1 1.341(4) . ? N1 C2 1.403(4) . ? N1 C8 1.478(4) . ? N2 C1 1.342(4) . ? N2 C7 1.401(4) . ? N2 C11 1.480(4) . ? N3 C19 1.334(4) . ? N3 C15 1.355(4) . ? N4 C24 1.339(4) . ? N4 C20 1.346(4) . ? N4 C25 1.478(3) . ? O1 C29 1.371(4) . ? O1 C30 1.440(4) . ? O2 C31 1.419(4) . ? O2 C32 1.423(4) . ? O4 C36 1.363(4) . ? O4 C35A 1.439(8) . ? O4 C35 1.471(5) . ? C2 C3 1.391(4) . ? C2 C7 1.403(5) . ? C3 C4 1.385(5) . ? C4 C5 1.389(5) . ? C5 C6 1.382(5) . ? C6 C7 1.390(4) . ? C8 C9 1.516(5) . ? C8 C10 1.517(5) . ? C11 C12 1.498(5) . ? C11 C13 1.503(5) . ? C15 C16 1.380(4) . ? C16 C17 1.391(4) . ? C17 C18 1.398(4) . ? C17 C22 1.480(4) . ? C18 C19 1.375(4) . ? C20 C21 1.369(4) . ? C21 C22 1.388(4) . ? C22 C23 1.395(4) . ? C23 C24 1.363(4) . ? C25 C25 1.512(6) 3_656 ? C26 C37 1.373(6) 3_656 ? C26 C27 1.375(6) . ? C27 C28 1.396(5) . ? C28 C29 1.392(5) . ? C29 C36 1.410(5) 3_656 ? C30 C31 1.500(5) . ? C32 C33A 1.482(9) . ? C32 C33 1.496(6) . ? C33 O3 1.394(7) . ? O3 C34 1.424(6) . ? C34 C35 1.502(7) . ? C33A O3A 1.401(9) . ? O3A C34A 1.402(9) . ? C34A C35A 1.489(9) . ? C36 C37 1.390(5) . ? C36 C29 1.410(5) 3_656 ? C37 C26 1.373(6) 3_656 ? B1 F1 1.323(8) . ? B1 F4 1.380(8) . ? B1 F2 1.395(8) . ? B1 F3 1.418(8) . ? F2 B1A 1.438(16) . ? F4 B1A 1.420(17) . ? B1A F1A 1.409(17) . ? B1A F3A 1.419(17) . ? N1S C1S 1.141(11) . ? C1S C2S 1.426(19) . ? N2S C3S 1.128(6) . ? C3S C4S 1.464(7) . ? N3S C5S 1.137(4) . ? C5S C6S 1.451(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N3 171.91(11) . . ? C1 Pd1 Br1 88.52(9) . . ? N3 Pd1 Br1 93.46(7) . . ? C1 Pd1 Br2 86.81(9) . . ? N3 Pd1 Br2 92.33(7) . . ? Br1 Pd1 Br2 170.358(15) . . ? C1 N1 C2 109.0(3) . . ? C1 N1 C8 123.3(3) . . ? C2 N1 C8 127.6(2) . . ? C1 N2 C7 109.7(3) . . ? C1 N2 C11 123.0(3) . . ? C7 N2 C11 127.3(3) . . ? C19 N3 C15 117.7(2) . . ? C19 N3 Pd1 123.2(2) . . ? C15 N3 Pd1 119.0(2) . . ? C24 N4 C20 120.9(2) . . ? C24 N4 C25 119.1(2) . . ? C20 N4 C25 120.0(2) . . ? C29 O1 C30 116.3(2) . . ? C31 O2 C32 113.9(3) . . ? C36 O4 C35A 126.0(6) . . ? C36 O4 C35 112.9(3) . . ? C35A O4 C35 29.4(5) . . ? N1 C1 N2 108.9(3) . . ? N1 C1 Pd1 128.9(2) . . ? N2 C1 Pd1 121.8(2) . . ? C3 C2 N1 132.4(3) . . ? C3 C2 C7 120.9(3) . . ? N1 C2 C7 106.7(3) . . ? C4 C3 C2 117.0(3) . . ? C3 C4 C5 122.0(3) . . ? C6 C5 C4 121.4(3) . . ? C5 C6 C7 117.2(3) . . ? C6 C7 N2 132.9(3) . . ? C6 C7 C2 121.4(3) . . ? N2 C7 C2 105.6(3) . . ? N1 C8 C9 110.5(3) . . ? N1 C8 C10 110.4(3) . . ? C9 C8 C10 114.3(3) . . ? N2 C11 C12 111.8(3) . . ? N2 C11 C13 111.0(3) . . ? C12 C11 C13 115.1(3) . . ? N3 C15 C16 122.6(3) . . ? C15 C16 C17 119.3(3) . . ? C16 C17 C18 117.8(3) . . ? C16 C17 C22 121.5(3) . . ? C18 C17 C22 120.7(3) . . ? C19 C18 C17 119.3(3) . . ? N3 C19 C18 123.3(3) . . ? N4 C20 C21 120.0(3) . . ? C20 C21 C22 120.4(3) . . ? C21 C22 C23 117.8(3) . . ? C21 C22 C17 121.6(3) . . ? C23 C22 C17 120.6(3) . . ? C24 C23 C22 119.8(3) . . ? N4 C24 C23 121.0(3) . . ? N4 C25 C25 108.2(3) . 3_656 ? C37 C26 C27 120.9(4) 3_656 . ? C26 C27 C28 119.4(4) . . ? C29 C28 C27 120.5(4) . . ? O1 C29 C28 124.2(3) . . ? O1 C29 C36 116.3(3) . 3_656 ? C28 C29 C36 119.5(3) . 3_656 ? O1 C30 C31 108.9(3) . . ? O2 C31 C30 114.3(3) . . ? O2 C32 C33A 108.8(10) . . ? O2 C32 C33 111.2(4) . . ? C33A C32 C33 16.3(9) . . ? O3 C33 C32 110.8(5) . . ? C33 O3 C34 114.7(5) . . ? O3 C34 C35 115.1(5) . . ? O4 C35 C34 105.0(4) . . ? O3A C33A C32 113.5(9) . . ? C33A O3A C34A 114.1(9) . . ? O3A C34A C35A 111.4(10) . . ? O4 C35A C34A 107.4(9) . . ? O4 C36 C37 125.1(4) . . ? O4 C36 C29 116.0(3) . 3_656 ? C37 C36 C29 118.9(4) . 3_656 ? C26 C37 C36 120.9(4) 3_656 . ? F1 B1 F4 112.4(6) . . ? F1 B1 F2 107.1(6) . . ? F4 B1 F2 110.3(5) . . ? F1 B1 F3 110.7(6) . . ? F4 B1 F3 109.3(5) . . ? F2 B1 F3 107.0(6) . . ? B1 F2 B1A 15.6(9) . . ? B1 F4 B1A 15.8(9) . . ? F1A B1A F3A 106.6(13) . . ? F1A B1A F4 107.9(12) . . ? F3A B1A F4 106.9(12) . . ? F1A B1A F2 121.2(14) . . ? F3A B1A F2 107.9(12) . . ? F4 B1A F2 105.6(11) . . ? N1S C1S C2S 175(2) . . ? N2S C3S C4S 179.1(6) . . ? N3S C5S C6S 177.6(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.594 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.111 # Attachment '- Complex5.cif' data_a135a _database_code_depnum_ccdc_archive 'CCDC 837385' #TrackingRef '- Complex5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H80 B2 Br4 F8 N16 Pd2' _chemical_formula_weight 1779.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.8931(16) _cell_length_b 12.5992(10) _cell_length_c 14.5756(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.640(2) _cell_angle_gamma 90.00 _cell_volume 3871.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6464 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 26.95 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 2.596 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4233 _exptl_absorpt_correction_T_max 0.9033 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26567 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8890 _reflns_number_gt 6763 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0521P)^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_number_reflns 8890 _refine_ls_number_parameters 478 _refine_ls_number_restraints 82 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.169086(9) 0.450993(16) 0.292985(16) 0.02884(7) Uani 1 1 d . . . Br1 Br 0.177415(17) 0.31832(3) 0.41630(3) 0.05081(11) Uani 1 1 d . . . Br2 Br 0.157782(18) 0.59619(3) 0.18030(3) 0.05586(12) Uani 1 1 d . . . N1 N 0.04163(11) 0.50571(19) 0.30864(17) 0.0325(5) Uani 1 1 d . . . N2 N 0.11513(11) 0.59019(18) 0.41415(17) 0.0303(5) Uani 1 1 d . . . N3 N 0.23584(10) 0.36964(18) 0.23847(17) 0.0316(5) Uani 1 1 d . . . N4 N 0.45074(11) 0.05965(19) 0.07533(19) 0.0370(6) Uani 1 1 d . . . C1 C 0.10445(12) 0.5209(2) 0.3418(2) 0.0281(6) Uani 1 1 d . . . C2 C 0.01043(14) 0.5677(2) 0.3619(2) 0.0346(7) Uani 1 1 d . . . C3 C -0.05368(15) 0.5817(3) 0.3558(3) 0.0475(8) Uani 1 1 d . . . H3 H -0.0855 0.5456 0.3103 0.057 Uiso 1 1 calc R . . C4 C -0.06791(16) 0.6512(3) 0.4201(3) 0.0562(10) Uani 1 1 d . . . H4 H -0.1106 0.6615 0.4192 0.067 Uiso 1 1 calc R . . C5 C -0.02170(17) 0.7060(3) 0.4854(3) 0.0523(9) Uani 1 1 d . . . H5 H -0.0339 0.7539 0.5267 0.063 Uiso 1 1 calc R . . C6 C 0.04185(15) 0.6930(2) 0.4925(2) 0.0419(7) Uani 1 1 d . . . H6 H 0.0733 0.7299 0.5379 0.050 Uiso 1 1 calc R . . C7 C 0.05705(13) 0.6220(2) 0.4285(2) 0.0319(6) Uani 1 1 d . . . C8 C 0.01248(15) 0.4385(3) 0.2259(2) 0.0434(8) Uani 1 1 d . . . H8 H 0.0478 0.4046 0.2062 0.052 Uiso 1 1 calc R . . C9 C -0.0262(2) 0.3495(3) 0.2515(3) 0.0719(12) Uani 1 1 d . . . H9A H 0.0002 0.3081 0.3031 0.108 Uiso 1 1 calc R . . H9B H -0.0423 0.3043 0.1964 0.108 Uiso 1 1 calc R . . H9C H -0.0616 0.3791 0.2713 0.108 Uiso 1 1 calc R . . C10 C -0.02304(18) 0.5065(4) 0.1429(3) 0.0661(11) Uani 1 1 d . . . H10A H -0.0568 0.5445 0.1604 0.099 Uiso 1 1 calc R . . H10B H -0.0411 0.4617 0.0883 0.099 Uiso 1 1 calc R . . H10C H 0.0060 0.5570 0.1271 0.099 Uiso 1 1 calc R . . C11 C 0.17918(14) 0.6255(2) 0.4670(2) 0.0402(7) Uani 1 1 d . . . H11 H 0.2097 0.5883 0.4390 0.048 Uiso 1 1 calc R . . C12 C 0.18652(18) 0.7444(3) 0.4516(3) 0.0627(11) Uani 1 1 d . . . H12A H 0.1776 0.7589 0.3839 0.094 Uiso 1 1 calc R . . H12B H 0.2296 0.7660 0.4832 0.094 Uiso 1 1 calc R . . H12C H 0.1571 0.7835 0.4780 0.094 Uiso 1 1 calc R . . C13 C 0.19363(18) 0.5925(3) 0.5699(3) 0.0615(10) Uani 1 1 d . . . H13A H 0.1677 0.6334 0.6014 0.092 Uiso 1 1 calc R . . H13B H 0.2381 0.6053 0.6009 0.092 Uiso 1 1 calc R . . H13C H 0.1844 0.5176 0.5736 0.092 Uiso 1 1 calc R . . C14 C 0.22739(14) 0.2653(2) 0.2209(2) 0.0393(7) Uani 1 1 d . . . H14 H 0.1924 0.2317 0.2343 0.047 Uiso 1 1 calc R . . C15 C 0.26762(14) 0.2057(2) 0.1842(2) 0.0386(7) Uani 1 1 d . . . H15 H 0.2591 0.1334 0.1705 0.046 Uiso 1 1 calc R . . C16 C 0.32085(12) 0.2525(2) 0.1673(2) 0.0300(6) Uani 1 1 d . . . C17 C 0.33024(13) 0.3598(2) 0.1873(2) 0.0338(7) Uani 1 1 d . . . H17 H 0.3661 0.3945 0.1780 0.041 Uiso 1 1 calc R . . C18 C 0.28606(13) 0.4155(2) 0.2213(2) 0.0342(7) Uani 1 1 d . . . H18 H 0.2921 0.4887 0.2326 0.041 Uiso 1 1 calc R . . C19 C 0.47235(14) 0.1424(2) 0.1321(2) 0.0362(7) Uani 1 1 d . . . H19 H 0.5162 0.1561 0.1520 0.043 Uiso 1 1 calc R . . C20 C 0.43109(13) 0.2074(2) 0.1613(2) 0.0346(7) Uani 1 1 d . . . H20 H 0.4466 0.2654 0.2015 0.041 Uiso 1 1 calc R . . C21 C 0.36661(13) 0.1876(2) 0.1317(2) 0.0310(6) Uani 1 1 d . . . C22 C 0.34524(14) 0.1037(2) 0.0697(2) 0.0413(8) Uani 1 1 d . . . H22 H 0.3015 0.0905 0.0461 0.050 Uiso 1 1 calc R . . C23 C 0.38839(15) 0.0403(3) 0.0431(3) 0.0449(8) Uani 1 1 d . . . H23 H 0.3741 -0.0173 0.0020 0.054 Uiso 1 1 calc R . . C24 C 0.49616(15) -0.0147(3) 0.0486(2) 0.0426(8) Uani 1 1 d . . . H24A H 0.4803 -0.0876 0.0472 0.051 Uiso 1 1 calc R . . H24B H 0.5374 -0.0110 0.0962 0.051 Uiso 1 1 calc R . . N1S N 0.41449(16) 0.2214(3) 0.8986(3) 0.0699(10) Uani 1 1 d . . . C1S C 0.39403(18) 0.2960(3) 0.9172(3) 0.0591(10) Uani 1 1 d . . . C2S C 0.3689(3) 0.3951(4) 0.9420(5) 0.127(3) Uani 1 1 d . . . H2S1 H 0.3244 0.3862 0.9390 0.191 Uiso 1 1 calc R . . H2S2 H 0.3734 0.4499 0.8975 0.191 Uiso 1 1 calc R . . H2S3 H 0.3922 0.4155 1.0061 0.191 Uiso 1 1 calc R . . N2S N 0.3328(2) 0.6129(4) 0.0841(5) 0.120(2) Uani 1 1 d . . . C3S C 0.3814(2) 0.6368(3) 0.0831(4) 0.0698(12) Uani 1 1 d . . . C4S C 0.4450(2) 0.6658(4) 0.0806(4) 0.0808(14) Uani 1 1 d . . . H4S1 H 0.4750 0.6144 0.1167 0.121 Uiso 1 1 calc R . . H4S2 H 0.4552 0.7357 0.1084 0.121 Uiso 1 1 calc R . . H4S3 H 0.4473 0.6666 0.0151 0.121 Uiso 1 1 calc R . . N3S N 0.36669(19) 0.8547(3) 0.8837(3) 0.0908(13) Uani 1 1 d . . . C5S C 0.33748(19) 0.7914(3) 0.8380(3) 0.0610(10) Uani 1 1 d . . . C6S C 0.3006(2) 0.7118(4) 0.7778(4) 0.0916(17) Uani 1 1 d . . . H6S1 H 0.2607 0.7424 0.7414 0.137 Uiso 1 1 calc R . . H6S2 H 0.2922 0.6539 0.8165 0.137 Uiso 1 1 calc R . . H6S3 H 0.3238 0.6852 0.7345 0.137 Uiso 1 1 calc R . . N4S N 0.20054(18) 0.0081(3) 0.3041(3) 0.0746(10) Uani 1 1 d . . . C7S C 0.20052(17) 0.0212(3) 0.3807(3) 0.0543(9) Uani 1 1 d . . . C8S C 0.2008(2) 0.0365(3) 0.4788(3) 0.0651(11) Uani 1 1 d . . . H8S1 H 0.1619 0.0083 0.4890 0.098 Uiso 1 1 calc R . . H8S2 H 0.2037 0.1118 0.4935 0.098 Uiso 1 1 calc R . . H8S3 H 0.2369 0.0000 0.5199 0.098 Uiso 1 1 calc R . . B1 B 0.45818(19) 0.9203(3) 0.2881(3) 0.0469(10) Uani 1 1 d D . . F1 F 0.4205(7) 1.0066(10) 0.2886(13) 0.087(4) Uani 0.49(2) 1 d PD A 1 F2 F 0.5163(5) 0.9532(11) 0.2854(11) 0.083(4) Uani 0.49(2) 1 d PD A 1 F3 F 0.4581(6) 0.8562(10) 0.3595(11) 0.109(5) Uani 0.49(2) 1 d PDU A 1 F4 F 0.4304(7) 0.8683(13) 0.2032(8) 0.135(5) Uani 0.49(2) 1 d PDU A 1 F1A F 0.4111(7) 0.9915(9) 0.2677(11) 0.092(4) Uani 0.51(2) 1 d PDU A 2 F2A F 0.5103(6) 0.9539(11) 0.2623(12) 0.091(4) Uani 0.51(2) 1 d PD A 2 F4A F 0.4390(3) 0.8271(8) 0.2441(13) 0.115(5) Uani 0.51(2) 1 d PD A 2 F3A F 0.4773(7) 0.9014(15) 0.3853(6) 0.125(4) Uani 0.51(2) 1 d PDU 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 Pd1 0.02787(12) 0.03236(12) 0.02996(13) -0.00323(9) 0.01412(9) 0.00580(8) Br1 0.0644(2) 0.0474(2) 0.0496(2) 0.00970(16) 0.03087(19) 0.01686(16) Br2 0.0678(2) 0.0544(2) 0.0572(2) 0.01806(18) 0.0371(2) 0.02022(17) N1 0.0297(12) 0.0402(13) 0.0286(13) -0.0079(11) 0.0097(11) 0.0037(10) N2 0.0309(12) 0.0336(12) 0.0293(13) -0.0036(10) 0.0134(11) 0.0034(10) N3 0.0281(12) 0.0375(13) 0.0334(13) -0.0066(11) 0.0151(11) 0.0049(10) N4 0.0368(13) 0.0382(14) 0.0418(15) -0.0044(12) 0.0206(12) 0.0086(11) C1 0.0298(14) 0.0308(13) 0.0252(14) -0.0017(11) 0.0101(12) 0.0045(11) C2 0.0343(15) 0.0398(16) 0.0329(16) -0.0010(13) 0.0148(13) 0.0077(12) C3 0.0295(16) 0.071(2) 0.044(2) -0.0021(18) 0.0128(15) 0.0091(15) C4 0.0382(18) 0.086(3) 0.050(2) 0.002(2) 0.0205(18) 0.0215(18) C5 0.055(2) 0.062(2) 0.047(2) -0.0035(18) 0.0268(19) 0.0231(18) C6 0.0491(19) 0.0413(17) 0.0379(18) -0.0076(14) 0.0164(16) 0.0099(14) C7 0.0327(15) 0.0384(15) 0.0274(15) -0.0006(12) 0.0126(13) 0.0079(12) C8 0.0393(17) 0.056(2) 0.0346(17) -0.0179(16) 0.0097(14) -0.0010(15) C9 0.072(3) 0.072(3) 0.072(3) -0.028(2) 0.020(2) -0.024(2) C10 0.054(2) 0.104(3) 0.035(2) -0.010(2) 0.0023(18) 0.009(2) C11 0.0335(16) 0.0436(17) 0.0433(19) -0.0114(15) 0.0103(14) -0.0031(13) C12 0.062(2) 0.049(2) 0.084(3) -0.017(2) 0.032(2) -0.0226(17) C13 0.050(2) 0.077(3) 0.048(2) -0.011(2) -0.0026(18) 0.0025(19) C14 0.0349(16) 0.0409(17) 0.049(2) -0.0119(15) 0.0228(15) -0.0036(13) C15 0.0368(16) 0.0353(16) 0.049(2) -0.0117(14) 0.0206(15) -0.0047(12) C16 0.0276(14) 0.0366(15) 0.0280(15) -0.0036(12) 0.0111(12) 0.0066(11) C17 0.0279(14) 0.0372(15) 0.0407(18) -0.0001(13) 0.0169(14) 0.0036(12) C18 0.0363(15) 0.0290(14) 0.0418(18) -0.0036(13) 0.0180(14) 0.0051(12) C19 0.0311(15) 0.0391(16) 0.0401(18) -0.0053(14) 0.0124(14) 0.0024(12) C20 0.0328(15) 0.0361(15) 0.0367(17) -0.0069(13) 0.0127(14) 0.0025(12) C21 0.0308(14) 0.0346(15) 0.0305(15) -0.0030(12) 0.0131(13) 0.0029(11) C22 0.0292(15) 0.0477(18) 0.049(2) -0.0158(15) 0.0141(15) -0.0021(13) C23 0.0404(17) 0.0453(18) 0.052(2) -0.0223(16) 0.0178(16) -0.0020(14) C24 0.0442(17) 0.0390(16) 0.051(2) -0.0068(15) 0.0248(16) 0.0136(14) N1S 0.067(2) 0.079(2) 0.062(2) 0.004(2) 0.0159(19) 0.0168(19) C1S 0.058(2) 0.075(3) 0.048(2) 0.012(2) 0.021(2) 0.018(2) C2S 0.196(7) 0.102(4) 0.123(5) 0.037(4) 0.111(5) 0.077(4) N2S 0.070(3) 0.095(4) 0.199(6) 0.014(3) 0.043(4) -0.007(2) C3S 0.066(3) 0.058(2) 0.085(3) 0.000(2) 0.021(3) 0.001(2) C4S 0.076(3) 0.090(3) 0.079(3) 0.007(3) 0.026(3) -0.012(3) N3S 0.086(3) 0.075(3) 0.101(3) -0.041(2) 0.007(3) -0.004(2) C5S 0.062(2) 0.057(2) 0.062(3) -0.015(2) 0.013(2) 0.0000(19) C6S 0.061(3) 0.081(3) 0.129(5) -0.055(3) 0.017(3) -0.015(2) N4S 0.080(3) 0.082(3) 0.060(2) -0.001(2) 0.014(2) 0.000(2) C7S 0.045(2) 0.052(2) 0.062(3) 0.007(2) 0.008(2) -0.0025(16) C8S 0.076(3) 0.062(2) 0.054(2) 0.012(2) 0.012(2) -0.004(2) B1 0.063(3) 0.036(2) 0.049(3) 0.0073(18) 0.028(2) 0.0088(18) F1 0.085(6) 0.065(5) 0.122(9) -0.009(5) 0.050(6) 0.029(4) F2 0.062(5) 0.073(6) 0.121(9) 0.006(6) 0.033(5) -0.014(5) F3 0.121(7) 0.085(6) 0.151(10) 0.067(6) 0.091(7) 0.042(5) F4 0.215(11) 0.111(8) 0.108(7) -0.041(6) 0.091(7) -0.055(7) F1A 0.112(8) 0.088(7) 0.092(6) 0.039(6) 0.053(5) 0.033(5) F2A 0.105(8) 0.101(7) 0.088(6) 0.057(5) 0.063(5) 0.045(5) F4A 0.066(4) 0.076(5) 0.189(13) -0.039(6) 0.011(5) 0.003(3) F3A 0.162(9) 0.159(10) 0.064(5) 0.031(6) 0.045(5) 0.029(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.956(3) . ? Pd1 N3 2.108(2) . ? Pd1 Br1 2.4252(4) . ? Pd1 Br2 2.4262(4) . ? N1 C1 1.343(3) . ? N1 C2 1.402(3) . ? N1 C8 1.471(4) . ? N2 C1 1.340(4) . ? N2 C7 1.402(3) . ? N2 C11 1.475(4) . ? N3 C18 1.324(4) . ? N3 C14 1.343(4) . ? N4 C19 1.335(4) . ? N4 C23 1.341(4) . ? N4 C24 1.492(3) . ? C2 C7 1.385(4) . ? C2 C3 1.393(4) . ? C3 C4 1.379(5) . ? C4 C5 1.373(5) . ? C5 C6 1.377(4) . ? C6 C7 1.395(4) . ? C8 C9 1.511(5) . ? C8 C10 1.515(5) . ? C11 C13 1.506(5) . ? C11 C12 1.529(5) . ? C14 C15 1.371(4) . ? C15 C16 1.386(4) . ? C16 C17 1.386(4) . ? C16 C21 1.490(4) . ? C17 C18 1.390(4) . ? C19 C20 1.370(4) . ? C20 C21 1.383(4) . ? C21 C22 1.388(4) . ? C22 C23 1.370(4) . ? C24 C24 1.516(6) 3_655 ? N1S C1S 1.106(5) . ? C1S C2S 1.449(6) . ? N2S C3S 1.111(5) . ? C3S C4S 1.448(6) . ? N3S C5S 1.122(5) . ? C5S C6S 1.430(6) . ? N4S C7S 1.129(5) . ? C7S C8S 1.441(6) . ? B1 F3 1.318(8) . ? B1 F1A 1.338(9) . ? B1 F2 1.349(9) . ? B1 F4A 1.351(8) . ? B1 F2A 1.360(9) . ? B1 F1 1.365(9) . ? B1 F3A 1.386(9) . ? B1 F4 1.387(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N3 177.34(10) . . ? C1 Pd1 Br1 87.59(8) . . ? N3 Pd1 Br1 91.32(7) . . ? C1 Pd1 Br2 87.42(8) . . ? N3 Pd1 Br2 93.78(7) . . ? Br1 Pd1 Br2 174.280(14) . . ? C1 N1 C2 109.0(2) . . ? C1 N1 C8 123.6(2) . . ? C2 N1 C8 127.3(2) . . ? C1 N2 C7 109.3(2) . . ? C1 N2 C11 123.2(2) . . ? C7 N2 C11 127.5(2) . . ? C18 N3 C14 118.0(2) . . ? C18 N3 Pd1 123.67(19) . . ? C14 N3 Pd1 118.31(18) . . ? C19 N4 C23 121.1(2) . . ? C19 N4 C24 120.1(3) . . ? C23 N4 C24 118.8(3) . . ? N2 C1 N1 108.7(2) . . ? N2 C1 Pd1 126.1(2) . . ? N1 C1 Pd1 125.16(19) . . ? C7 C2 C3 121.5(3) . . ? C7 C2 N1 106.6(2) . . ? C3 C2 N1 131.9(3) . . ? C4 C3 C2 116.4(3) . . ? C5 C4 C3 122.1(3) . . ? C4 C5 C6 122.2(3) . . ? C5 C6 C7 116.4(3) . . ? C2 C7 C6 121.4(3) . . ? C2 C7 N2 106.3(2) . . ? C6 C7 N2 132.2(3) . . ? N1 C8 C9 111.9(3) . . ? N1 C8 C10 110.1(3) . . ? C9 C8 C10 114.5(3) . . ? N2 C11 C13 110.6(3) . . ? N2 C11 C12 110.0(3) . . ? C13 C11 C12 114.5(3) . . ? N3 C14 C15 122.7(3) . . ? C14 C15 C16 119.7(3) . . ? C15 C16 C17 117.5(2) . . ? C15 C16 C21 120.3(3) . . ? C17 C16 C21 122.2(2) . . ? C16 C17 C18 119.3(3) . . ? N3 C18 C17 122.7(3) . . ? N4 C19 C20 120.4(3) . . ? C19 C20 C21 119.9(3) . . ? C20 C21 C22 118.5(3) . . ? C20 C21 C16 121.2(2) . . ? C22 C21 C16 120.3(2) . . ? C23 C22 C21 119.4(3) . . ? N4 C23 C22 120.6(3) . . ? N4 C24 C24 109.9(3) . 3_655 ? N1S C1S C2S 178.4(5) . . ? N2S C3S C4S 178.7(6) . . ? N3S C5S C6S 178.6(6) . . ? N4S C7S C8S 179.3(5) . . ? F3 B1 F1A 114.9(8) . . ? F3 B1 F2 114.4(8) . . ? F1A B1 F2 117.7(11) . . ? F3 B1 F4A 77.0(7) . . ? F1A B1 F4A 110.8(8) . . ? F2 B1 F4A 115.4(9) . . ? F3 B1 F2A 126.0(8) . . ? F1A B1 F2A 112.6(7) . . ? F2 B1 F2A 13.8(11) . . ? F4A B1 F2A 108.4(7) . . ? F3 B1 F1 110.8(7) . . ? F1A B1 F1 15.7(13) . . ? F2 B1 F1 109.4(7) . . ? F4A B1 F1 125.7(9) . . ? F2A B1 F1 107.9(11) . . ? F3 B1 F3A 31.9(6) . . ? F1A B1 F3A 110.2(7) . . ? F2 B1 F3A 93.2(9) . . ? F4A B1 F3A 107.8(6) . . ? F2A B1 F3A 106.9(7) . . ? F1 B1 F3A 98.5(9) . . ? F3 B1 F4 108.7(6) . . ? F1A B1 F4 89.5(10) . . ? F2 B1 F4 108.1(7) . . ? F4A B1 F4 32.8(5) . . ? F2A B1 F4 95.7(9) . . ? F1 B1 F4 105.1(8) . . ? F3A B1 F4 140.3(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.935 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.087