# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Douglas Stephan' _publ_contact_author_email dstephan@chem.utoronto.ca loop_ _publ_author_name M.Sgro G.Stephan data_mjs035_compound3a _database_code_depnum_ccdc_archive 'CCDC 867384' #TrackingRef '- All Cif Files Compiled.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C16 H39 Cl2 N3 Ni P2' _chemical_formula_weight 465.05 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' Ni Ni 0.3393 1.1124 '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 15.6535(9) _cell_length_b 18.4051(10) _cell_length_c 27.970(2) _cell_angle_alpha 104.784(3) _cell_angle_beta 97.910(3) _cell_angle_gamma 109.773(2) _cell_volume 7106.6(8) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9686 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 27.35 _exptl_crystal_description BLOCK _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 1.184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6785 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 117303 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.78 _diffrn_reflns_theta_max 27.54 _reflns_number_total 32132 _reflns_number_gt 23501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0401P)^2^+5.1735P] 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 32132 _refine_ls_number_parameters 1297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Ni1 Ni 0.94067(2) 0.370067(18) 0.180743(12) 0.02211(7) Uani 1 1 d . . . Ni2 Ni 0.55526(2) 0.624584(19) 0.320947(13) 0.02442(8) Uani 1 1 d . . . Ni3 Ni 0.28353(2) 0.704417(18) 0.518239(12) 0.02295(7) Uani 1 1 d . . . Ni4 Ni 0.22673(2) 0.279846(18) 0.982618(12) 0.02378(7) Uani 1 1 d . . . Ni5 Ni 0.42051(2) 0.943895(18) 0.135756(12) 0.02306(7) Uani 1 1 d . . . Ni6 Ni 0.94546(2) 0.978550(19) 0.647177(12) 0.02305(7) Uani 1 1 d . . . Cl1 Cl 0.99168(5) 0.37839(4) 0.11335(3) 0.03655(16) Uani 1 1 d . . . Cl2 Cl 0.48859(6) 0.61244(5) 0.38272(3) 0.04397(19) Uani 1 1 d . . . Cl3 Cl 0.34788(5) 0.74632(4) 0.46141(3) 0.04359(19) Uani 1 1 d . . . Cl4 Cl 0.15322(6) 0.24645(4) 1.03840(3) 0.0452(2) Uani 1 1 d . . . Cl5 Cl 0.29920(5) 0.95396(4) 0.09412(3) 0.04378(19) Uani 1 1 d . . . Cl6 Cl 0.80908(5) 0.93721(4) 0.59545(3) 0.04267(18) Uani 1 1 d . . . Cl7 Cl 0.88275(5) 0.04299(4) 0.21016(3) 0.03527(16) Uani 1 1 d . . . Cl8 Cl 0.96152(5) 0.34506(4) 0.40112(3) 0.03521(16) Uani 1 1 d . . . Cl9 Cl 0.67748(5) 0.32187(4) 0.25197(3) 0.03153(14) Uani 1 1 d . . . Cl10 Cl 0.80959(5) 0.67302(4) 0.24531(3) 0.04039(17) Uani 1 1 d . . . Cl11 Cl 0.59720(6) 0.97257(4) 0.29769(3) 0.04303(19) Uani 1 1 d . . . Cl12 Cl 0.48785(5) 0.34729(4) 0.90986(3) 0.03575(16) Uani 1 1 d . . . P1 P 0.91041(5) 0.48138(4) 0.18085(3) 0.02441(14) Uani 1 1 d . . . P2 P 0.98306(5) 0.26448(4) 0.17308(2) 0.02277(14) Uani 1 1 d . . . P3 P 0.55183(5) 0.74957(4) 0.34291(3) 0.03001(16) Uani 1 1 d . . . P4 P 0.57517(5) 0.50988(4) 0.32152(3) 0.02907(15) Uani 1 1 d . . . P5 P 0.19784(5) 0.58950(4) 0.45326(3) 0.02810(15) Uani 1 1 d . . . P6 P 0.36996(5) 0.83256(4) 0.56922(3) 0.02625(15) Uani 1 1 d . . . P7 P 0.30054(5) 0.40287(4) 1.04209(3) 0.02908(15) Uani 1 1 d . . . P8 P 0.15785(5) 0.14542(4) 0.94006(3) 0.02505(14) Uani 1 1 d . . . P9 P 0.34137(5) 0.80855(4) 0.09998(3) 0.02320(14) Uani 1 1 d . . . P10 P 0.48329(5) 1.08160(4) 0.16063(3) 0.02614(15) Uani 1 1 d . . . P11 P 0.92937(5) 1.09715(4) 0.67781(3) 0.02665(15) Uani 1 1 d . . . P12 P 0.94131(5) 0.85343(4) 0.60919(3) 0.02932(16) Uani 1 1 d . . . N1 N 0.88481(17) 0.52250(14) 0.23424(9) 0.0360(6) Uani 1 1 d . . . H1A H 0.8611 0.5594 0.2337 0.043 Uiso 1 1 calc R . . N2 N 0.97917(16) 0.23139(13) 0.22286(8) 0.0291(5) Uani 1 1 d . . . H2A H 0.9859 0.1852 0.2209 0.035 Uiso 1 1 calc R . . N3 N 0.89089(15) 0.36540(12) 0.24055(8) 0.0251(5) Uani 1 1 d . . . H3B H 0.8309 0.3643 0.2315 0.030 Uiso 1 1 calc R . . N4 N 0.58282(17) 0.79669(14) 0.30126(10) 0.0385(6) Uani 1 1 d . . . H4A H 0.5667 0.8377 0.2999 0.046 Uiso 1 1 calc R . . N5 N 0.5975(2) 0.46215(15) 0.26946(10) 0.0473(7) Uani 1 1 d . . . H5A H 0.6067 0.4174 0.2691 0.057 Uiso 1 1 calc R . . N6 N 0.59795(15) 0.62422(12) 0.25851(8) 0.0253(5) Uani 1 1 d . . . H6C H 0.6618 0.6358 0.2671 0.030 Uiso 1 1 calc R . . N7 N 0.12942(18) 0.51497(14) 0.47015(9) 0.0441(7) Uani 1 1 d . . . H7A H 0.0901 0.4709 0.4454 0.053 Uiso 1 1 calc R . . N8 N 0.36121(17) 0.84865(13) 0.62901(9) 0.0367(6) Uani 1 1 d . . . H8A H 0.3991 0.8955 0.6520 0.044 Uiso 1 1 calc R . . N9 N 0.23331(14) 0.66220(12) 0.57036(7) 0.0229(4) Uani 1 1 d . . . H9D H 0.1754 0.6662 0.5690 0.028 Uiso 1 1 calc R . . N10 N 0.35788(18) 0.47624(14) 1.02068(10) 0.0429(6) Uani 1 1 d . . . H10A H 0.3909 0.5245 1.0436 0.051 Uiso 1 1 calc R . . N11 N 0.17703(15) 0.12292(13) 0.88252(8) 0.0314(5) Uani 1 1 d . . . H11A H 0.1406 0.0759 0.8592 0.038 Uiso 1 1 calc R . . N12 N 0.28244(14) 0.31682(12) 0.93034(8) 0.0243(4) Uani 1 1 d . . . H12D H 0.3455 0.3258 0.9394 0.029 Uiso 1 1 calc R . . N13 N 0.38155(15) 0.75326(12) 0.12911(8) 0.0274(5) Uani 1 1 d . . . H13A H 0.3618 0.7000 0.1156 0.033 Uiso 1 1 calc R . . N14 N 0.59740(16) 1.12408(13) 0.18803(9) 0.0359(6) Uani 1 1 d . . . H14A H 0.6267 1.1764 0.1928 0.043 Uiso 1 1 calc R . . N15 N 0.53048(14) 0.93955(12) 0.17605(8) 0.0242(4) Uani 1 1 d . . . H15D H 0.5298 0.9617 0.2098 0.029 Uiso 1 1 calc R . . N16 N 1.00363(15) 1.15774(12) 0.73363(8) 0.0281(5) Uani 1 1 d . . . H16A H 1.0094 1.2085 0.7468 0.034 Uiso 1 1 calc R . . N17 N 1.04040(17) 0.84222(14) 0.62655(10) 0.0432(6) Uani 1 1 d . . . H17A H 1.0379 0.7920 0.6169 0.052 Uiso 1 1 calc R . . N18 N 1.06895(14) 1.01038(12) 0.69141(8) 0.0253(5) Uani 1 1 d . . . H18B H 1.0591 0.9763 0.7113 0.030 Uiso 1 1 calc R . . C1 C 0.80647(19) 0.45993(16) 0.13107(11) 0.0318(6) Uani 1 1 d . . . H1B H 0.7878 0.5076 0.1402 0.038 Uiso 1 1 calc R . . C2 C 1.00545(19) 0.56415(15) 0.17117(11) 0.0334(6) Uani 1 1 d . . . H2B H 1.0163 0.5427 0.1369 0.040 Uiso 1 1 calc R . . C3 C 0.90951(18) 0.17117(15) 0.11947(10) 0.0283(6) Uani 1 1 d . . . H3A H 0.9209 0.1249 0.1277 0.034 Uiso 1 1 calc R . . C4 C 1.10506(17) 0.28976(15) 0.16767(10) 0.0284(6) Uani 1 1 d . . . H4B H 1.1095 0.3008 0.1347 0.034 Uiso 1 1 calc R . . C5 C 0.8970(2) 0.50468(16) 0.28154(10) 0.0320(6) Uani 1 1 d . . . H5B H 0.8347 0.4817 0.2885 0.038 Uiso 1 1 calc R . . H5C H 0.9345 0.5564 0.3096 0.038 Uiso 1 1 calc R . . C6 C 0.94476(19) 0.44529(16) 0.28185(10) 0.0312(6) Uani 1 1 d . . . H6A H 1.0086 0.4692 0.2771 0.037 Uiso 1 1 calc R . . H6B H 0.9505 0.4362 0.3153 0.037 Uiso 1 1 calc R . . C7 C 0.9649(2) 0.27702(17) 0.26992(10) 0.0327(6) Uani 1 1 d . . . H7B H 1.0202 0.3290 0.2862 0.039 Uiso 1 1 calc R . . H7C H 0.9596 0.2451 0.2938 0.039 Uiso 1 1 calc R . . C8 C 0.8787(2) 0.29533(16) 0.26096(10) 0.0311(6) Uani 1 1 d . . . H8B H 0.8600 0.3079 0.2935 0.037 Uiso 1 1 calc R . . H8C H 0.8271 0.2459 0.2365 0.037 Uiso 1 1 calc R . . C9 C 0.7263(2) 0.38557(18) 0.13269(12) 0.0409(7) Uani 1 1 d . . . H9A H 0.6703 0.3734 0.1065 0.061 Uiso 1 1 calc R . . H9B H 0.7129 0.3971 0.1664 0.061 Uiso 1 1 calc R . . H9C H 0.7443 0.3385 0.1262 0.061 Uiso 1 1 calc R . . C10 C 0.8228(2) 0.44852(19) 0.07756(11) 0.0419(7) Uani 1 1 d . . . H10B H 0.7647 0.4375 0.0534 0.063 Uiso 1 1 calc R . . H10C H 0.8420 0.4025 0.0676 0.063 Uiso 1 1 calc R . . H10D H 0.8721 0.4983 0.0773 0.063 Uiso 1 1 calc R . . C11 C 0.9802(2) 0.63785(17) 0.17193(13) 0.0450(8) Uani 1 1 d . . . H11B H 1.0324 0.6803 0.1666 0.068 Uiso 1 1 calc R . . H11C H 0.9681 0.6594 0.2050 0.068 Uiso 1 1 calc R . . H11D H 0.9240 0.6211 0.1447 0.068 Uiso 1 1 calc R . . C12 C 1.0950(2) 0.58808(19) 0.21135(13) 0.0489(8) Uani 1 1 d . . . H12A H 1.1458 0.6321 0.2063 0.073 Uiso 1 1 calc R . . H12B H 1.1119 0.5407 0.2082 0.073 Uiso 1 1 calc R . . H12C H 1.0851 0.6069 0.2454 0.073 Uiso 1 1 calc R . . C13 C 0.8064(2) 0.1549(2) 0.11680(12) 0.0440(8) Uani 1 1 d . . . H13B H 0.7673 0.1051 0.0884 0.066 Uiso 1 1 calc R . . H13C H 0.7934 0.2011 0.1115 0.066 Uiso 1 1 calc R . . H13D H 0.7923 0.1480 0.1488 0.066 Uiso 1 1 calc R . . C14 C 0.9305(2) 0.16956(17) 0.06776(10) 0.0400(7) Uani 1 1 d . . . H14B H 0.8882 0.1177 0.0420 0.060 Uiso 1 1 calc R . . H14C H 0.9955 0.1752 0.0695 0.060 Uiso 1 1 calc R . . H14D H 0.9213 0.2148 0.0585 0.060 Uiso 1 1 calc R . . C15 C 1.1669(2) 0.36745(18) 0.21128(12) 0.0432(7) Uani 1 1 d . . . H15A H 1.2323 0.3823 0.2092 0.065 Uiso 1 1 calc R . . H15B H 1.1612 0.3583 0.2439 0.065 Uiso 1 1 calc R . . H15C H 1.1471 0.4118 0.2088 0.065 Uiso 1 1 calc R . . C16 C 1.1368(2) 0.21983(18) 0.16815(13) 0.0426(7) Uani 1 1 d . . . H16B H 1.2017 0.2355 0.1650 0.064 Uiso 1 1 calc R . . H16C H 1.0962 0.1710 0.1395 0.064 Uiso 1 1 calc R . . H16D H 1.1329 0.2082 0.2003 0.064 Uiso 1 1 calc R . . C17 C 0.6317(2) 0.82300(19) 0.40515(12) 0.0440(8) Uani 1 1 d . . . H17B H 0.6311 0.8775 0.4060 0.053 Uiso 1 1 calc R . . C18 C 0.43587(19) 0.74972(18) 0.34604(12) 0.0370(7) Uani 1 1 d . . . H18A H 0.4170 0.7268 0.3735 0.044 Uiso 1 1 calc R . . C19 C 0.6790(2) 0.53416(18) 0.37231(11) 0.0384(7) Uani 1 1 d . . . H19A H 0.6924 0.4837 0.3671 0.046 Uiso 1 1 calc R . . C20 C 0.4785(2) 0.43048(17) 0.33275(12) 0.0381(7) Uani 1 1 d . . . H20A H 0.4663 0.4550 0.3661 0.046 Uiso 1 1 calc R . . C21 C 0.6364(2) 0.77116(17) 0.26689(12) 0.0381(7) Uani 1 1 d . . . H21A H 0.6975 0.7784 0.2872 0.046 Uiso 1 1 calc R . . H21B H 0.6489 0.8067 0.2452 0.046 Uiso 1 1 calc R . . C22 C 0.5870(2) 0.68374(18) 0.23316(11) 0.0370(7) Uani 1 1 d . . . H22A H 0.5195 0.6718 0.2220 0.044 Uiso 1 1 calc R . . H22B H 0.6117 0.6763 0.2023 0.044 Uiso 1 1 calc R . . C23 C 0.6036(2) 0.48608(17) 0.22461(11) 0.0372(7) Uani 1 1 d . . . H23A H 0.5768 0.4364 0.1942 0.045 Uiso 1 1 calc R . . H23B H 0.6704 0.5142 0.2257 0.045 Uiso 1 1 calc R . . C24 C 0.5535(2) 0.54144(17) 0.21884(11) 0.0394(7) Uani 1 1 d . . . H24A H 0.5519 0.5478 0.1847 0.047 Uiso 1 1 calc R . . H24B H 0.4879 0.5153 0.2207 0.047 Uiso 1 1 calc R . . C25 C 0.7321(2) 0.8306(2) 0.40571(16) 0.0664(11) Uani 1 1 d . . . H25A H 0.7740 0.8695 0.4383 0.100 Uiso 1 1 calc R . . H25B H 0.7512 0.8500 0.3778 0.100 Uiso 1 1 calc R . . H25C H 0.7355 0.7772 0.4013 0.100 Uiso 1 1 calc R . . C26 C 0.6065(3) 0.8098(3) 0.45316(14) 0.0670(11) Uani 1 1 d . . . H26A H 0.6536 0.8526 0.4829 0.101 Uiso 1 1 calc R . . H26B H 0.6045 0.7563 0.4539 0.101 Uiso 1 1 calc R . . H26C H 0.5449 0.8119 0.4539 0.101 Uiso 1 1 calc R . . C27 C 0.4341(2) 0.83553(19) 0.35963(14) 0.0518(9) Uani 1 1 d . . . H27A H 0.3705 0.8316 0.3609 0.078 Uiso 1 1 calc R . . H27B H 0.4536 0.8601 0.3337 0.078 Uiso 1 1 calc R . . H27C H 0.4772 0.8695 0.3930 0.078 Uiso 1 1 calc R . . C28 C 0.3660(2) 0.6931(2) 0.29628(13) 0.0518(9) Uani 1 1 d . . . H28A H 0.3037 0.6928 0.2979 0.078 Uiso 1 1 calc R . . H28B H 0.3641 0.6377 0.2906 0.078 Uiso 1 1 calc R . . H28C H 0.3848 0.7119 0.2682 0.078 Uiso 1 1 calc R . . C29 C 0.6662(2) 0.5588(2) 0.42655(12) 0.0501(8) Uani 1 1 d . . . H29A H 0.7242 0.5707 0.4511 0.075 Uiso 1 1 calc R . . H29B H 0.6149 0.5141 0.4305 0.075 Uiso 1 1 calc R . . H29C H 0.6514 0.6076 0.4328 0.075 Uiso 1 1 calc R . . C30 C 0.7635(2) 0.5996(2) 0.36541(14) 0.0513(9) Uani 1 1 d . . . H30A H 0.8189 0.6128 0.3923 0.077 Uiso 1 1 calc R . . H30B H 0.7508 0.6488 0.3676 0.077 Uiso 1 1 calc R . . H30C H 0.7748 0.5790 0.3320 0.077 Uiso 1 1 calc R . . C31 C 0.3906(2) 0.4045(2) 0.29071(15) 0.0550(9) Uani 1 1 d . . . H31A H 0.3386 0.3622 0.2963 0.083 Uiso 1 1 calc R . . H31B H 0.4021 0.3828 0.2575 0.083 Uiso 1 1 calc R . . H31C H 0.3746 0.4518 0.2914 0.083 Uiso 1 1 calc R . . C32 C 0.5015(2) 0.35644(19) 0.33564(15) 0.0555(9) Uani 1 1 d . . . H32A H 0.4480 0.3162 0.3417 0.083 Uiso 1 1 calc R . . H32B H 0.5567 0.3743 0.3637 0.083 Uiso 1 1 calc R . . H32C H 0.5142 0.3318 0.3034 0.083 Uiso 1 1 calc R . . C33 C 0.2661(2) 0.54443(17) 0.41599(11) 0.0378(7) Uani 1 1 d . . . H33A H 0.3032 0.5854 0.4014 0.045 Uiso 1 1 calc R . . C34 C 0.1121(2) 0.60270(18) 0.40709(11) 0.0393(7) Uani 1 1 d . . . H34A H 0.0655 0.5467 0.3864 0.047 Uiso 1 1 calc R . . C35 C 0.49540(18) 0.86171(16) 0.57228(12) 0.0361(7) Uani 1 1 d . . . H35A H 0.5051 0.8650 0.5382 0.043 Uiso 1 1 calc R . . C36 C 0.3399(2) 0.91333(18) 0.55284(12) 0.0394(7) Uani 1 1 d . . . H36A H 0.3632 0.9610 0.5849 0.047 Uiso 1 1 calc R . . C37 C 0.1282(2) 0.51547(16) 0.52128(11) 0.0335(6) Uani 1 1 d . . . H37A H 0.1166 0.4598 0.5226 0.040 Uiso 1 1 calc R . . H37B H 0.0750 0.5289 0.5301 0.040 Uiso 1 1 calc R . . C38 C 0.2159(2) 0.57412(15) 0.56092(11) 0.0339(6) Uani 1 1 d . . . H38A H 0.2127 0.5624 0.5934 0.041 Uiso 1 1 calc R . . H38B H 0.2699 0.5643 0.5503 0.041 Uiso 1 1 calc R . . C39 C 0.2948(2) 0.79007(17) 0.64561(11) 0.0397(7) Uani 1 1 d . . . H39A H 0.2321 0.7908 0.6354 0.048 Uiso 1 1 calc R . . H39B H 0.3127 0.8069 0.6833 0.048 Uiso 1 1 calc R . . C40 C 0.2891(2) 0.70523(16) 0.62433(10) 0.0357(7) Uani 1 1 d . . . H40A H 0.2609 0.6732 0.6458 0.043 Uiso 1 1 calc R . . H40B H 0.3534 0.7068 0.6264 0.043 Uiso 1 1 calc R . . C41 C 0.3345(2) 0.5280(2) 0.45161(13) 0.0517(9) Uani 1 1 d . . . H41A H 0.3714 0.5041 0.4321 0.078 Uiso 1 1 calc R . . H41B H 0.2997 0.4899 0.4677 0.078 Uiso 1 1 calc R . . H41C H 0.3766 0.5793 0.4780 0.078 Uiso 1 1 calc R . . C42 C 0.2041(3) 0.46679(19) 0.37168(13) 0.0582(10) Uani 1 1 d . . . H42A H 0.2436 0.4453 0.3530 0.087 Uiso 1 1 calc R . . H42B H 0.1625 0.4796 0.3486 0.087 Uiso 1 1 calc R . . H42C H 0.1664 0.4258 0.3851 0.087 Uiso 1 1 calc R . . C43 C 0.0583(2) 0.6462(2) 0.43628(13) 0.0483(8) Uani 1 1 d . . . H43A H 0.0127 0.6534 0.4121 0.072 Uiso 1 1 calc R . . H43B H 0.1022 0.6997 0.4597 0.072 Uiso 1 1 calc R . . H43C H 0.0254 0.6134 0.4558 0.072 Uiso 1 1 calc R . . C44 C 0.1506(2) 0.6436(2) 0.36902(13) 0.0546(9) Uani 1 1 d . . . H44A H 0.0995 0.6474 0.3466 0.082 Uiso 1 1 calc R . . H44B H 0.1790 0.6111 0.3485 0.082 Uiso 1 1 calc R . . H44C H 0.1981 0.6985 0.3876 0.082 Uiso 1 1 calc R . . C45 C 0.5266(2) 0.7965(2) 0.58282(15) 0.0590(10) Uani 1 1 d . . . H45A H 0.5936 0.8123 0.5842 0.089 Uiso 1 1 calc R . . H45B H 0.4909 0.7444 0.5555 0.089 Uiso 1 1 calc R . . H45C H 0.5156 0.7906 0.6155 0.089 Uiso 1 1 calc R . . C46 C 0.5549(2) 0.94508(19) 0.61210(14) 0.0558(9) Uani 1 1 d . . . H46A H 0.6211 0.9583 0.6123 0.084 Uiso 1 1 calc R . . H46B H 0.5459 0.9436 0.6459 0.084 Uiso 1 1 calc R . . H46C H 0.5358 0.9867 0.6037 0.084 Uiso 1 1 calc R . . C47 C 0.2334(2) 0.8854(2) 0.53815(14) 0.0578(10) Uani 1 1 d . . . H47A H 0.2172 0.9283 0.5296 0.087 Uiso 1 1 calc R . . H47B H 0.2080 0.8745 0.5669 0.087 Uiso 1 1 calc R . . H47C H 0.2068 0.8355 0.5085 0.087 Uiso 1 1 calc R . . C48 C 0.3820(3) 0.9450(2) 0.51266(15) 0.0618(10) Uani 1 1 d . . . H48A H 0.3613 0.9878 0.5078 0.093 Uiso 1 1 calc R . . H48B H 0.3613 0.9001 0.4804 0.093 Uiso 1 1 calc R . . H48C H 0.4505 0.9675 0.5240 0.093 Uiso 1 1 calc R . . C49 C 0.3935(2) 0.40050(17) 1.08918(11) 0.0392(7) Uani 1 1 d . . . H49A H 0.4347 0.4584 1.1095 0.047 Uiso 1 1 calc R . . C50 C 0.2276(2) 0.44350(16) 1.07831(12) 0.0395(7) Uani 1 1 d . . . H50A H 0.1950 0.4027 1.0943 0.047 Uiso 1 1 calc R . . C51 C 0.1960(2) 0.07762(16) 0.96875(11) 0.0362(7) Uani 1 1 d . . . H51A H 0.1691 0.0228 0.9419 0.043 Uiso 1 1 calc R . . C52 C 0.02957(18) 0.10426(16) 0.92897(11) 0.0342(6) Uani 1 1 d . . . H52A H 0.0143 0.1080 0.9628 0.041 Uiso 1 1 calc R . . C53 C 0.3593(2) 0.46937(15) 0.96849(11) 0.0334(6) Uani 1 1 d . . . H53A H 0.4188 0.4652 0.9628 0.040 Uiso 1 1 calc R . . H53B H 0.3583 0.5199 0.9625 0.040 Uiso 1 1 calc R . . C54 C 0.2792(2) 0.39756(16) 0.93023(11) 0.0358(7) Uani 1 1 d . . . H54A H 0.2799 0.4021 0.8958 0.043 Uiso 1 1 calc R . . H54B H 0.2197 0.3992 0.9376 0.043 Uiso 1 1 calc R . . C55 C 0.25336(18) 0.17991(16) 0.87003(10) 0.0317(6) Uani 1 1 d . . . H55A H 0.2541 0.1558 0.8342 0.038 Uiso 1 1 calc R . . H55B H 0.3134 0.1885 0.8921 0.038 Uiso 1 1 calc R . . C56 C 0.2458(2) 0.26097(16) 0.87661(10) 0.0332(6) Uani 1 1 d . . . H56A H 0.2809 0.2876 0.8548 0.040 Uiso 1 1 calc R . . H56B H 0.1792 0.2517 0.8649 0.040 Uiso 1 1 calc R . . C57 C 0.4537(2) 0.3636(2) 1.06069(13) 0.0494(8) Uani 1 1 d . . . H57A H 0.5035 0.3622 1.0854 0.074 Uiso 1 1 calc R . . H57B H 0.4816 0.3971 1.0403 0.074 Uiso 1 1 calc R . . H57C H 0.4145 0.3080 1.0382 0.074 Uiso 1 1 calc R . . C58 C 0.3598(3) 0.3574(2) 1.12701(13) 0.0566(9) Uani 1 1 d . . . H58A H 0.4138 0.3592 1.1504 0.085 Uiso 1 1 calc R . . H58B H 0.3181 0.3005 1.1084 0.085 Uiso 1 1 calc R . . H58C H 0.3257 0.3849 1.1466 0.085 Uiso 1 1 calc R . . C59 C 0.2857(3) 0.52409(18) 1.12111(14) 0.0607(11) Uani 1 1 d . . . H59A H 0.2441 0.5432 1.1393 0.091 Uiso 1 1 calc R . . H59B H 0.3195 0.5650 1.1065 0.091 Uiso 1 1 calc R . . H59C H 0.3307 0.5157 1.1449 0.091 Uiso 1 1 calc R . . C60 C 0.1532(2) 0.4512(2) 1.04115(14) 0.0548(9) Uani 1 1 d . . . H60A H 0.1137 0.4726 1.0599 0.082 Uiso 1 1 calc R . . H60B H 0.1144 0.3975 1.0161 0.082 Uiso 1 1 calc R . . H60C H 0.1835 0.4886 1.0235 0.082 Uiso 1 1 calc R . . C61 C 0.3020(2) 0.1049(2) 0.97846(15) 0.0599(10) Uani 1 1 d . . . H61A H 0.3217 0.0687 0.9934 0.090 Uiso 1 1 calc R . . H61B H 0.3322 0.1610 1.0020 0.090 Uiso 1 1 calc R . . H61C H 0.3203 0.1026 0.9461 0.090 Uiso 1 1 calc R . . C62 C 0.1629(3) 0.0640(2) 1.01587(13) 0.0589(10) Uani 1 1 d . . . H62A H 0.1873 0.0270 1.0270 0.088 Uiso 1 1 calc R . . H62B H 0.0943 0.0400 1.0074 0.088 Uiso 1 1 calc R . . H62C H 0.1858 0.1164 1.0433 0.088 Uiso 1 1 calc R . . C63 C -0.0089(2) 0.1574(2) 0.90622(15) 0.0544(9) Uani 1 1 d . . . H63A H -0.0773 0.1357 0.9004 0.082 Uiso 1 1 calc R . . H63B H 0.0080 0.1571 0.8737 0.082 Uiso 1 1 calc R . . H63C H 0.0178 0.2134 0.9299 0.082 Uiso 1 1 calc R . . C64 C -0.0168(2) 0.01466(17) 0.89541(12) 0.0452(8) Uani 1 1 d . . . H64A H -0.0848 -0.0043 0.8908 0.068 Uiso 1 1 calc R . . H64B H 0.0067 -0.0183 0.9118 0.068 Uiso 1 1 calc R . . H64C H -0.0019 0.0091 0.8621 0.068 Uiso 1 1 calc R . . C65 C 0.21633(18) 0.77223(16) 0.09947(12) 0.0360(7) Uani 1 1 d . . . H65A H 0.1859 0.7981 0.0790 0.043 Uiso 1 1 calc R . . C66 C 0.3480(2) 0.76854(17) 0.03391(10) 0.0334(6) Uani 1 1 d . . . H66A H 0.3225 0.7077 0.0242 0.040 Uiso 1 1 calc R . . C67 C 0.4335(2) 1.13477(17) 0.20695(11) 0.0371(7) Uani 1 1 d . . . H67A H 0.4769 1.1936 0.2197 0.044 Uiso 1 1 calc R . . C68 C 0.4731(2) 1.11847(16) 0.10565(11) 0.0364(7) Uani 1 1 d . . . H68A H 0.4051 1.1036 0.0910 0.044 Uiso 1 1 calc R . . C69 C 0.4506(2) 0.79725(15) 0.17776(10) 0.0332(6) Uani 1 1 d . . . H69A H 0.4674 0.7578 0.1912 0.040 Uiso 1 1 calc R . . H69B H 0.4226 0.8248 0.2024 0.040 Uiso 1 1 calc R . . C70 C 0.53852(19) 0.86021(15) 0.17340(10) 0.0304(6) Uani 1 1 d . . . H70A H 0.5916 0.8698 0.2013 0.036 Uiso 1 1 calc R . . H70B H 0.5527 0.8383 0.1406 0.036 Uiso 1 1 calc R . . C71 C 0.65248(19) 1.08157(16) 0.20471(11) 0.0331(6) Uani 1 1 d . . . H71A H 0.6481 1.0815 0.2397 0.040 Uiso 1 1 calc R . . H71B H 0.7190 1.1118 0.2061 0.040 Uiso 1 1 calc R . . C72 C 0.62202(18) 0.99499(16) 0.17072(11) 0.0320(6) Uani 1 1 d . . . H72A H 0.6710 0.9743 0.1792 0.038 Uiso 1 1 calc R . . H72B H 0.6157 0.9938 0.1348 0.038 Uiso 1 1 calc R . . C73 C 0.2092(2) 0.8016(2) 0.15426(13) 0.0513(9) Uani 1 1 d . . . H73A H 0.1432 0.7835 0.1552 0.077 Uiso 1 1 calc R . . H73B H 0.2385 0.8614 0.1675 0.077 Uiso 1 1 calc R . . H73C H 0.2414 0.7790 0.1753 0.077 Uiso 1 1 calc R . . C74 C 0.1662(2) 0.67947(18) 0.07574(15) 0.0556(9) Uani 1 1 d . . . H74A H 0.0999 0.6632 0.0761 0.083 Uiso 1 1 calc R . . H74B H 0.1949 0.6531 0.0955 0.083 Uiso 1 1 calc R . . H74C H 0.1716 0.6628 0.0405 0.083 Uiso 1 1 calc R . . C75 C 0.2898(2) 0.7903(2) -0.00430(11) 0.0516(9) Uani 1 1 d . . . H75A H 0.2958 0.7670 -0.0387 0.077 Uiso 1 1 calc R . . H75B H 0.3123 0.8498 0.0046 0.077 Uiso 1 1 calc R . . H75C H 0.2239 0.7682 -0.0033 0.077 Uiso 1 1 calc R . . C76 C 0.4507(2) 0.7970(2) 0.03085(12) 0.0450(8) Uani 1 1 d . . . H76A H 0.4537 0.7751 -0.0044 0.068 Uiso 1 1 calc R . . H76B H 0.4850 0.7773 0.0530 0.068 Uiso 1 1 calc R . . H76C H 0.4789 0.8567 0.0420 0.068 Uiso 1 1 calc R . . C77 C 0.4371(3) 1.1039(2) 0.25260(13) 0.0564(9) Uani 1 1 d . . . H77A H 0.4110 1.1316 0.2778 0.085 Uiso 1 1 calc R . . H77B H 0.5023 1.1152 0.2681 0.085 Uiso 1 1 calc R . . H77C H 0.4004 1.0449 0.2412 0.085 Uiso 1 1 calc R . . C78 C 0.3370(3) 1.1320(3) 0.18657(15) 0.0702(12) Uani 1 1 d . . . H78A H 0.3176 1.1622 0.2143 0.105 Uiso 1 1 calc R . . H78B H 0.2920 1.0752 0.1728 0.105 Uiso 1 1 calc R . . H78C H 0.3391 1.1570 0.1595 0.105 Uiso 1 1 calc R . . C79 C 0.5233(3) 1.21085(18) 0.12047(14) 0.0592(10) Uani 1 1 d . . . H79A H 0.5154 1.2276 0.0901 0.089 Uiso 1 1 calc R . . H79B H 0.5902 1.2267 0.1350 0.089 Uiso 1 1 calc R . . H79C H 0.4967 1.2376 0.1458 0.089 Uiso 1 1 calc R . . C80 C 0.5110(3) 1.0744(2) 0.06508(12) 0.0522(9) Uani 1 1 d . . . H80A H 0.5054 1.0931 0.0354 0.078 Uiso 1 1 calc R . . H80B H 0.4749 1.0154 0.0546 0.078 Uiso 1 1 calc R . . H80C H 0.5770 1.0864 0.0792 0.078 Uiso 1 1 calc R . . C81 C 0.8146(2) 1.0892(2) 0.68835(14) 0.0525(9) Uani 1 1 d . . . H81A H 0.7672 1.0591 0.6549 0.063 Uiso 1 1 calc R . . C82 C 0.9551(2) 1.16367(19) 0.63705(12) 0.0474(8) Uani 1 1 d . . . H82A H 0.9598 1.2187 0.6575 0.057 Uiso 1 1 calc R . . C83 C 0.8568(2) 0.77035(17) 0.62429(13) 0.0436(8) Uani 1 1 d . . . H83A H 0.8796 0.7250 0.6188 0.052 Uiso 1 1 calc R . . C84 C 0.9134(2) 0.82540(19) 0.53895(11) 0.0440(8) Uani 1 1 d . . . H84A H 0.8464 0.8166 0.5268 0.053 Uiso 1 1 calc R . . C85 C 1.0587(2) 1.12313(17) 0.75973(10) 0.0376(7) Uani 1 1 d . . . H85A H 1.0158 1.0766 0.7676 0.045 Uiso 1 1 calc R . . H85B H 1.0990 1.1648 0.7925 0.045 Uiso 1 1 calc R . . C86 C 1.11937(19) 1.09416(16) 0.72872(11) 0.0354(7) Uani 1 1 d . . . H86A H 1.1439 1.1326 0.7100 0.042 Uiso 1 1 calc R . . H86B H 1.1735 1.0951 0.7522 0.042 Uiso 1 1 calc R . . C87 C 1.1303(2) 0.90500(18) 0.65552(12) 0.0400(7) Uani 1 1 d . . . H87A H 1.1789 0.8966 0.6382 0.048 Uiso 1 1 calc R . . H87B H 1.1446 0.8993 0.6896 0.048 Uiso 1 1 calc R . . C88 C 1.13565(19) 0.98970(17) 0.66204(11) 0.0362(7) Uani 1 1 d . . . H88A H 1.1215 0.9957 0.6280 0.043 Uiso 1 1 calc R . . H88B H 1.2003 1.0289 0.6801 0.043 Uiso 1 1 calc R . . C89 C 0.7921(3) 1.0396(2) 0.72296(17) 0.0765(13) Uani 1 1 d . . . H89A H 0.7305 1.0343 0.7292 0.115 Uiso 1 1 calc R . . H89B H 0.8398 1.0665 0.7554 0.115 Uiso 1 1 calc R . . H89C H 0.7914 0.9853 0.7071 0.115 Uiso 1 1 calc R . . C90 C 0.8094(3) 1.1724(2) 0.70965(15) 0.0664(11) Uani 1 1 d . . . H90A H 0.7464 1.1647 0.7144 0.100 Uiso 1 1 calc R . . H90B H 0.8230 1.2029 0.6857 0.100 Uiso 1 1 calc R . . H90C H 0.8555 1.2030 0.7425 0.100 Uiso 1 1 calc R . . C91 C 0.8799(3) 1.1352(2) 0.58862(14) 0.0739(13) Uani 1 1 d . . . H91A H 0.8984 1.1729 0.5692 0.111 Uiso 1 1 calc R . . H91B H 0.8208 1.1336 0.5971 0.111 Uiso 1 1 calc R . . H91C H 0.8718 1.0804 0.5680 0.111 Uiso 1 1 calc R . . C92 C 1.0511(3) 1.1743(2) 0.62580(13) 0.0567(9) Uani 1 1 d . . . H92A H 1.0645 1.2095 0.6044 0.085 Uiso 1 1 calc R . . H92B H 1.0505 1.1209 0.6078 0.085 Uiso 1 1 calc R . . H92C H 1.0995 1.1993 0.6579 0.085 Uiso 1 1 calc R . . C93 C 0.7569(2) 0.7345(2) 0.59213(16) 0.0683(11) Uani 1 1 d . . . H93A H 0.7182 0.6908 0.6033 0.102 Uiso 1 1 calc R . . H93B H 0.7560 0.7122 0.5562 0.102 Uiso 1 1 calc R . . H93C H 0.7319 0.7772 0.5961 0.102 Uiso 1 1 calc R . . C94 C 0.8594(3) 0.7991(2) 0.68107(14) 0.0560(9) Uani 1 1 d . . . H94A H 0.8146 0.7551 0.6894 0.084 Uiso 1 1 calc R . . H94B H 0.8428 0.8469 0.6887 0.084 Uiso 1 1 calc R . . H94C H 0.9226 0.8137 0.7014 0.084 Uiso 1 1 calc R . . C95 C 0.9745(3) 0.8963(2) 0.52387(13) 0.0598(10) Uani 1 1 d . . . H95A H 0.9597 0.8818 0.4866 0.090 Uiso 1 1 calc R . . H95B H 1.0407 0.9075 0.5367 0.090 Uiso 1 1 calc R . . H95C H 0.9623 0.9451 0.5387 0.090 Uiso 1 1 calc R . . C96 C 0.9256(3) 0.7464(2) 0.51376(13) 0.0703(12) Uani 1 1 d . . . H96A H 0.9097 0.7333 0.4766 0.105 Uiso 1 1 calc R . . H96B H 0.8841 0.7017 0.5231 0.105 Uiso 1 1 calc R . . H96C H 0.9908 0.7536 0.5255 0.105 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02457(17) 0.02151(15) 0.02466(17) 0.00997(13) 0.01050(14) 0.01074(14) Ni2 0.02499(17) 0.02955(17) 0.03078(18) 0.01876(15) 0.01315(14) 0.01607(14) Ni3 0.02033(16) 0.02275(16) 0.02040(17) 0.00518(13) 0.00578(13) 0.00298(13) Ni4 0.02264(17) 0.01981(15) 0.02441(17) 0.00365(13) 0.00842(14) 0.00446(13) Ni5 0.02506(17) 0.01862(15) 0.02666(18) 0.00975(13) 0.00641(14) 0.00809(13) Ni6 0.02258(16) 0.02242(16) 0.02112(17) 0.00400(13) 0.00271(13) 0.00841(14) Cl1 0.0537(4) 0.0403(4) 0.0369(4) 0.0226(3) 0.0280(3) 0.0299(4) Cl2 0.0613(5) 0.0513(4) 0.0563(5) 0.0390(4) 0.0427(4) 0.0394(4) Cl3 0.0437(4) 0.0379(4) 0.0289(4) 0.0072(3) 0.0146(3) -0.0080(3) Cl4 0.0559(5) 0.0259(3) 0.0393(4) 0.0013(3) 0.0294(4) -0.0015(3) Cl5 0.0310(4) 0.0299(3) 0.0669(5) 0.0203(4) -0.0034(4) 0.0102(3) Cl6 0.0310(4) 0.0388(4) 0.0422(4) -0.0063(3) -0.0088(3) 0.0155(3) Cl7 0.0503(4) 0.0231(3) 0.0295(4) 0.0087(3) 0.0077(3) 0.0115(3) Cl8 0.0293(3) 0.0250(3) 0.0438(4) 0.0009(3) 0.0145(3) 0.0069(3) Cl9 0.0328(3) 0.0256(3) 0.0374(4) 0.0090(3) 0.0127(3) 0.0121(3) Cl10 0.0325(4) 0.0272(3) 0.0654(5) 0.0148(3) 0.0200(4) 0.0134(3) Cl11 0.0753(6) 0.0241(3) 0.0310(4) 0.0092(3) 0.0169(4) 0.0192(4) Cl12 0.0289(3) 0.0251(3) 0.0451(4) 0.0012(3) 0.0120(3) 0.0069(3) P1 0.0266(3) 0.0206(3) 0.0289(4) 0.0093(3) 0.0108(3) 0.0101(3) P2 0.0257(3) 0.0207(3) 0.0239(3) 0.0081(3) 0.0081(3) 0.0101(3) P3 0.0305(4) 0.0322(4) 0.0424(4) 0.0216(3) 0.0173(3) 0.0202(3) P4 0.0297(4) 0.0307(4) 0.0386(4) 0.0189(3) 0.0132(3) 0.0185(3) P5 0.0255(3) 0.0252(3) 0.0237(4) 0.0039(3) 0.0098(3) -0.0004(3) P6 0.0240(3) 0.0216(3) 0.0284(4) 0.0044(3) 0.0048(3) 0.0065(3) P7 0.0321(4) 0.0193(3) 0.0298(4) 0.0032(3) 0.0127(3) 0.0043(3) P8 0.0214(3) 0.0213(3) 0.0264(4) 0.0022(3) 0.0056(3) 0.0052(3) P9 0.0245(3) 0.0199(3) 0.0261(3) 0.0085(3) 0.0084(3) 0.0081(3) P10 0.0311(4) 0.0194(3) 0.0280(4) 0.0108(3) 0.0063(3) 0.0081(3) P11 0.0265(3) 0.0269(3) 0.0239(3) 0.0035(3) 0.0019(3) 0.0124(3) P12 0.0330(4) 0.0263(3) 0.0249(4) 0.0015(3) 0.0027(3) 0.0137(3) N1 0.0502(15) 0.0341(12) 0.0374(14) 0.0144(11) 0.0217(12) 0.0264(12) N2 0.0416(13) 0.0259(11) 0.0273(12) 0.0131(9) 0.0123(10) 0.0172(10) N3 0.0257(11) 0.0262(11) 0.0270(12) 0.0105(9) 0.0092(9) 0.0119(9) N4 0.0430(14) 0.0378(13) 0.0623(17) 0.0345(13) 0.0315(13) 0.0283(12) N5 0.0676(18) 0.0447(15) 0.0550(17) 0.0239(13) 0.0308(15) 0.0405(15) N6 0.0249(11) 0.0316(11) 0.0256(11) 0.0144(9) 0.0070(9) 0.0143(10) N7 0.0443(15) 0.0322(13) 0.0321(14) 0.0043(11) 0.0139(12) -0.0109(12) N8 0.0457(15) 0.0230(11) 0.0279(13) -0.0006(10) 0.0076(11) 0.0041(11) N9 0.0225(11) 0.0241(10) 0.0215(11) 0.0071(9) 0.0051(9) 0.0084(9) N10 0.0491(16) 0.0255(12) 0.0379(15) 0.0043(11) 0.0169(12) -0.0030(11) N11 0.0239(11) 0.0280(11) 0.0271(12) -0.0038(9) 0.0051(10) 0.0018(10) N12 0.0208(11) 0.0263(11) 0.0240(11) 0.0082(9) 0.0037(9) 0.0075(9) N13 0.0342(12) 0.0160(10) 0.0301(12) 0.0082(9) 0.0063(10) 0.0079(9) N14 0.0319(13) 0.0211(11) 0.0496(15) 0.0132(11) 0.0028(11) 0.0056(10) N15 0.0274(11) 0.0205(10) 0.0243(11) 0.0073(9) 0.0056(9) 0.0092(9) N16 0.0345(12) 0.0220(10) 0.0242(12) 0.0034(9) 0.0020(10) 0.0118(10) N17 0.0434(15) 0.0309(13) 0.0484(16) -0.0007(11) -0.0026(12) 0.0215(12) N18 0.0239(11) 0.0231(10) 0.0277(12) 0.0088(9) 0.0036(9) 0.0081(9) C1 0.0332(15) 0.0286(14) 0.0380(16) 0.0129(12) 0.0073(13) 0.0163(12) C2 0.0355(15) 0.0250(13) 0.0404(17) 0.0123(12) 0.0171(13) 0.0086(12) C3 0.0301(14) 0.0223(12) 0.0294(14) 0.0072(11) 0.0072(12) 0.0074(11) C4 0.0254(13) 0.0322(14) 0.0311(15) 0.0103(12) 0.0096(12) 0.0142(12) C5 0.0372(16) 0.0251(13) 0.0276(15) 0.0024(11) 0.0094(12) 0.0087(12) C6 0.0315(15) 0.0326(14) 0.0256(14) 0.0072(12) 0.0046(12) 0.0103(12) C7 0.0443(17) 0.0332(14) 0.0288(15) 0.0147(12) 0.0147(13) 0.0196(13) C8 0.0391(16) 0.0296(14) 0.0302(15) 0.0146(12) 0.0152(13) 0.0141(13) C9 0.0306(15) 0.0394(16) 0.0477(19) 0.0125(14) 0.0057(14) 0.0102(14) C10 0.0481(19) 0.0454(17) 0.0372(17) 0.0201(14) 0.0054(15) 0.0212(15) C11 0.0513(19) 0.0261(14) 0.066(2) 0.0222(15) 0.0283(17) 0.0149(14) C12 0.0361(17) 0.0411(17) 0.058(2) 0.0151(16) 0.0109(16) 0.0025(15) C13 0.0309(16) 0.0514(19) 0.0367(17) 0.0064(15) 0.0080(14) 0.0063(15) C14 0.0437(18) 0.0352(15) 0.0286(16) 0.0008(13) 0.0121(14) 0.0059(14) C15 0.0295(16) 0.0449(17) 0.0439(18) 0.0035(14) 0.0058(14) 0.0102(14) C16 0.0380(17) 0.0471(18) 0.055(2) 0.0212(16) 0.0164(15) 0.0262(15) C17 0.0387(17) 0.0398(17) 0.053(2) 0.0090(15) 0.0110(15) 0.0194(15) C18 0.0342(16) 0.0460(17) 0.0520(19) 0.0293(15) 0.0235(14) 0.0263(14) C19 0.0390(17) 0.0418(16) 0.0456(18) 0.0199(14) 0.0068(14) 0.0264(14) C20 0.0380(16) 0.0374(15) 0.0539(19) 0.0272(15) 0.0182(15) 0.0208(14) C21 0.0378(16) 0.0437(17) 0.057(2) 0.0370(15) 0.0256(15) 0.0242(14) C22 0.0466(18) 0.0534(18) 0.0347(16) 0.0311(14) 0.0197(14) 0.0320(16) C23 0.0389(17) 0.0321(15) 0.0332(16) 0.0025(12) 0.0097(13) 0.0106(13) C24 0.0434(18) 0.0404(16) 0.0274(15) 0.0075(13) -0.0001(13) 0.0137(14) C25 0.0363(19) 0.070(3) 0.075(3) 0.005(2) 0.0050(19) 0.0167(19) C26 0.055(2) 0.079(3) 0.052(2) 0.011(2) 0.0125(19) 0.016(2) C27 0.0481(19) 0.0500(19) 0.083(3) 0.0356(19) 0.0300(19) 0.0338(17) C28 0.0350(17) 0.067(2) 0.062(2) 0.0271(19) 0.0172(17) 0.0242(17) C29 0.056(2) 0.060(2) 0.045(2) 0.0229(17) 0.0072(16) 0.0330(18) C30 0.0298(16) 0.057(2) 0.069(2) 0.0194(18) 0.0076(16) 0.0215(16) C31 0.0376(18) 0.0467(19) 0.081(3) 0.0326(19) 0.0114(18) 0.0091(16) C32 0.057(2) 0.0413(18) 0.089(3) 0.0398(19) 0.030(2) 0.0270(17) C33 0.0414(17) 0.0306(14) 0.0371(17) 0.0068(13) 0.0232(14) 0.0068(13) C34 0.0331(16) 0.0386(16) 0.0293(16) 0.0088(13) -0.0001(13) -0.0015(13) C35 0.0229(14) 0.0313(14) 0.0414(17) 0.0016(13) 0.0045(13) 0.0043(12) C36 0.0438(18) 0.0350(15) 0.0460(18) 0.0173(14) 0.0121(15) 0.0196(14) C37 0.0369(16) 0.0253(13) 0.0386(16) 0.0120(12) 0.0170(13) 0.0083(12) C38 0.0431(17) 0.0278(14) 0.0356(16) 0.0150(12) 0.0075(13) 0.0168(13) C39 0.0482(18) 0.0335(15) 0.0308(16) 0.0030(13) 0.0151(14) 0.0116(14) C40 0.0453(17) 0.0351(15) 0.0222(14) 0.0089(12) 0.0045(13) 0.0120(14) C41 0.060(2) 0.0509(19) 0.063(2) 0.0261(17) 0.0398(19) 0.0290(18) C42 0.065(2) 0.0419(18) 0.049(2) -0.0053(16) 0.0297(19) 0.0073(17) C43 0.0322(17) 0.056(2) 0.053(2) 0.0207(17) 0.0070(15) 0.0123(16) C44 0.048(2) 0.067(2) 0.042(2) 0.0254(18) 0.0050(16) 0.0104(18) C45 0.0303(17) 0.056(2) 0.085(3) 0.0132(19) 0.0026(18) 0.0213(16) C46 0.0302(17) 0.0433(18) 0.063(2) -0.0026(17) -0.0043(16) -0.0020(15) C47 0.053(2) 0.083(3) 0.066(2) 0.041(2) 0.0225(19) 0.045(2) C48 0.069(2) 0.055(2) 0.085(3) 0.048(2) 0.033(2) 0.029(2) C49 0.0365(16) 0.0292(14) 0.0367(17) 0.0046(13) 0.0025(13) 0.0017(13) C50 0.0528(19) 0.0263(14) 0.0457(18) 0.0121(13) 0.0329(16) 0.0145(14) C51 0.0375(16) 0.0249(13) 0.0397(17) 0.0053(12) 0.0034(13) 0.0107(13) C52 0.0200(13) 0.0316(14) 0.0414(17) 0.0036(13) 0.0080(12) 0.0043(12) C53 0.0378(16) 0.0242(13) 0.0440(17) 0.0164(12) 0.0154(14) 0.0129(12) C54 0.0412(17) 0.0322(15) 0.0382(17) 0.0159(13) 0.0064(14) 0.0174(13) C55 0.0273(14) 0.0372(15) 0.0248(14) 0.0035(12) 0.0089(12) 0.0095(12) C56 0.0325(15) 0.0373(15) 0.0221(14) 0.0089(12) 0.0041(12) 0.0057(13) C57 0.0328(17) 0.0488(19) 0.058(2) 0.0155(17) 0.0025(16) 0.0105(15) C58 0.055(2) 0.060(2) 0.048(2) 0.0232(18) 0.0085(17) 0.0116(18) C59 0.084(3) 0.0284(16) 0.064(2) 0.0019(16) 0.045(2) 0.0150(18) C60 0.061(2) 0.057(2) 0.075(3) 0.0345(19) 0.043(2) 0.0370(19) C61 0.043(2) 0.055(2) 0.080(3) 0.024(2) -0.0033(19) 0.0225(18) C62 0.090(3) 0.048(2) 0.047(2) 0.0228(17) 0.017(2) 0.031(2) C63 0.0276(16) 0.053(2) 0.078(3) 0.0142(18) 0.0058(17) 0.0178(15) C64 0.0258(15) 0.0376(16) 0.051(2) -0.0020(14) 0.0072(14) -0.0002(13) C65 0.0236(14) 0.0288(14) 0.0553(19) 0.0149(13) 0.0130(13) 0.0077(12) C66 0.0422(17) 0.0303(14) 0.0254(14) 0.0063(12) 0.0081(13) 0.0134(13) C67 0.0406(17) 0.0320(15) 0.0391(17) 0.0080(13) 0.0119(14) 0.0167(13) C68 0.0479(18) 0.0281(14) 0.0347(16) 0.0177(12) 0.0071(14) 0.0125(13) C69 0.0470(17) 0.0257(13) 0.0301(15) 0.0129(12) 0.0060(13) 0.0165(13) C70 0.0333(15) 0.0257(13) 0.0317(15) 0.0083(11) -0.0006(12) 0.0150(12) C71 0.0305(15) 0.0288(14) 0.0342(16) 0.0123(12) 0.0036(12) 0.0046(12) C72 0.0252(14) 0.0314(14) 0.0398(16) 0.0117(12) 0.0095(12) 0.0108(12) C73 0.0457(19) 0.052(2) 0.070(2) 0.0277(18) 0.0389(18) 0.0209(16) C74 0.0318(17) 0.0337(17) 0.090(3) 0.0179(18) 0.0140(18) 0.0014(14) C75 0.063(2) 0.061(2) 0.0282(17) 0.0112(15) 0.0007(16) 0.0267(19) C76 0.058(2) 0.057(2) 0.0381(18) 0.0250(15) 0.0281(16) 0.0307(17) C77 0.066(2) 0.069(2) 0.045(2) 0.0224(18) 0.0284(18) 0.031(2) C78 0.063(2) 0.093(3) 0.066(3) 0.008(2) 0.014(2) 0.058(2) C79 0.081(3) 0.0344(17) 0.054(2) 0.0287(16) 0.004(2) 0.0068(18) C80 0.068(2) 0.058(2) 0.0387(19) 0.0278(16) 0.0224(17) 0.0215(19) C81 0.0282(16) 0.0507(19) 0.058(2) -0.0076(17) 0.0057(15) 0.0106(15) C82 0.071(2) 0.0374(16) 0.0372(18) 0.0147(14) -0.0011(16) 0.0282(17) C83 0.0415(18) 0.0292(15) 0.057(2) 0.0130(14) 0.0061(16) 0.0125(14) C84 0.0492(19) 0.0482(18) 0.0280(16) -0.0038(14) 0.0001(14) 0.0266(16) C85 0.0467(18) 0.0305(14) 0.0265(15) 0.0013(12) -0.0078(13) 0.0164(14) C86 0.0261(14) 0.0280(14) 0.0415(17) 0.0053(12) -0.0078(13) 0.0085(12) C87 0.0357(16) 0.0470(17) 0.0403(17) 0.0096(14) 0.0086(14) 0.0233(15) C88 0.0278(15) 0.0399(16) 0.0414(17) 0.0112(13) 0.0112(13) 0.0143(13) C89 0.063(3) 0.055(2) 0.100(3) 0.009(2) 0.053(3) 0.009(2) C90 0.050(2) 0.070(2) 0.069(3) -0.009(2) 0.0058(19) 0.038(2) C91 0.104(3) 0.068(3) 0.051(2) 0.024(2) -0.008(2) 0.040(2) C92 0.077(3) 0.053(2) 0.045(2) 0.0238(17) 0.0268(19) 0.020(2) C93 0.044(2) 0.047(2) 0.097(3) 0.026(2) 0.000(2) 0.0015(17) C94 0.060(2) 0.055(2) 0.063(2) 0.0348(19) 0.0244(19) 0.0198(18) C95 0.069(2) 0.084(3) 0.0336(19) 0.0203(18) 0.0195(18) 0.035(2) C96 0.091(3) 0.074(3) 0.0353(19) -0.0160(18) -0.0012(19) 0.051(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 1.949(2) . ? Ni1 Cl1 2.1664(7) . ? Ni1 P2 2.2275(7) . ? Ni1 P1 2.2529(7) . ? Ni2 N6 1.953(2) . ? Ni2 Cl2 2.1586(8) . ? Ni2 P4 2.2396(7) . ? Ni2 P3 2.2457(7) . ? Ni3 N9 1.956(2) . ? Ni3 Cl3 2.1626(8) . ? Ni3 P6 2.2405(7) . ? Ni3 P5 2.2413(7) . ? Ni4 N12 1.954(2) . ? Ni4 Cl4 2.1545(8) . ? Ni4 P7 2.2377(7) . ? Ni4 P8 2.2449(7) . ? Ni5 N15 1.961(2) . ? Ni5 Cl5 2.1761(8) . ? Ni5 P9 2.2450(7) . ? Ni5 P10 2.2584(7) . ? Ni6 N18 1.953(2) . ? Ni6 Cl6 2.1722(8) . ? Ni6 P11 2.2448(7) . ? Ni6 P12 2.2512(7) . ? P1 N1 1.660(2) . ? P1 C2 1.843(3) . ? P1 C1 1.845(3) . ? P2 N2 1.657(2) . ? P2 C3 1.843(3) . ? P2 C4 1.844(3) . ? P3 N4 1.653(2) . ? P3 C18 1.830(3) . ? P3 C17 1.865(3) . ? P4 N5 1.646(3) . ? P4 C20 1.842(3) . ? P4 C19 1.846(3) . ? P5 N7 1.652(2) . ? P5 C33 1.839(3) . ? P5 C34 1.853(3) . ? P6 N8 1.656(2) . ? P6 C35 1.835(3) . ? P6 C36 1.845(3) . ? P7 N10 1.652(2) . ? P7 C50 1.844(3) . ? P7 C49 1.844(3) . ? P8 N11 1.652(2) . ? P8 C52 1.839(3) . ? P8 C51 1.855(3) . ? P9 N13 1.676(2) . ? P9 C66 1.838(3) . ? P9 C65 1.839(3) . ? P10 N14 1.662(2) . ? P10 C68 1.841(3) . ? P10 C67 1.842(3) . ? P11 N16 1.663(2) . ? P11 C81 1.824(3) . ? P11 C82 1.861(3) . ? P12 N17 1.657(2) . ? P12 C83 1.839(3) . ? P12 C84 1.847(3) . ? N1 C5 1.445(3) . ? N1 H1A 0.8800 . ? N2 C7 1.460(3) . ? N2 H2A 0.8800 . ? N3 C6 1.495(3) . ? N3 C8 1.505(3) . ? N3 H3B 0.9300 . ? N4 C21 1.451(3) . ? N4 H4A 0.8800 . ? N5 C23 1.436(4) . ? N5 H5A 0.8800 . ? N6 C22 1.491(3) . ? N6 C24 1.498(3) . ? N6 H6C 0.9300 . ? N7 C37 1.431(4) . ? N7 H7A 0.8800 . ? N8 C39 1.445(4) . ? N8 H8A 0.8800 . ? N9 C40 1.492(3) . ? N9 C38 1.495(3) . ? N9 H9D 0.9300 . ? N10 C53 1.437(4) . ? N10 H10A 0.8800 . ? N11 C55 1.451(3) . ? N11 H11A 0.8800 . ? N12 C56 1.490(3) . ? N12 C54 1.504(3) . ? N12 H12D 0.9300 . ? N13 C69 1.455(3) . ? N13 H13A 0.8800 . ? N14 C71 1.451(3) . ? N14 H14A 0.8800 . ? N15 C70 1.492(3) . ? N15 C72 1.505(3) . ? N15 H15D 0.9300 . ? N16 C85 1.455(3) . ? N16 H16A 0.8800 . ? N17 C87 1.442(4) . ? N17 H17A 0.8800 . ? N18 C86 1.490(3) . ? N18 C88 1.502(3) . ? N18 H18B 0.9300 . ? C1 C10 1.527(4) . ? C1 C9 1.528(4) . ? C1 H1B 1.0000 . ? C2 C12 1.523(4) . ? C2 C11 1.532(4) . ? C2 H2B 1.0000 . ? C3 C14 1.522(4) . ? C3 C13 1.525(4) . ? C3 H3A 1.0000 . ? C4 C15 1.523(4) . ? C4 C16 1.531(4) . ? C4 H4B 1.0000 . ? C5 C6 1.520(4) . ? C5 H5B 0.9900 . ? C5 H5C 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.502(4) . ? C7 H7B 0.9900 . ? C7 H7C 0.9900 . ? C8 H8B 0.9900 . ? C8 H8C 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13 H13D 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16 H16D 0.9800 . ? C17 C26 1.505(5) . ? C17 C25 1.526(4) . ? C17 H17B 1.0000 . ? C18 C28 1.513(4) . ? C18 C27 1.538(4) . ? C18 H18A 1.0000 . ? C19 C29 1.530(4) . ? C19 C30 1.533(4) . ? C19 H19A 1.0000 . ? C20 C31 1.526(4) . ? C20 C32 1.540(4) . ? C20 H20A 1.0000 . ? C21 C22 1.503(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.506(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C41 1.521(5) . ? C33 C42 1.532(4) . ? C33 H33A 1.0000 . ? C34 C43 1.525(4) . ? C34 C44 1.531(4) . ? C34 H34A 1.0000 . ? C35 C45 1.519(4) . ? C35 C46 1.529(4) . ? C35 H35A 1.0000 . ? C36 C48 1.521(4) . ? C36 C47 1.528(4) . ? C36 H36A 1.0000 . ? C37 C38 1.499(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.489(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C58 1.525(4) . ? C49 C57 1.532(4) . ? C49 H49A 1.0000 . ? C50 C60 1.520(5) . ? C50 C59 1.530(4) . ? C50 H50A 1.0000 . ? C51 C61 1.524(4) . ? C51 C62 1.529(4) . ? C51 H51A 1.0000 . ? C52 C63 1.528(4) . ? C52 C64 1.530(4) . ? C52 H52A 1.0000 . ? C53 C54 1.501(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.503(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C73 1.522(4) . ? C65 C74 1.531(4) . ? C65 H65A 1.0000 . ? C66 C75 1.527(4) . ? C66 C76 1.534(4) . ? C66 H66A 1.0000 . ? C67 C78 1.519(4) . ? C67 C77 1.526(4) . ? C67 H67A 1.0000 . ? C68 C79 1.526(4) . ? C68 C80 1.530(4) . ? C68 H68A 1.0000 . ? C69 C70 1.514(4) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 C72 1.503(4) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C89 1.490(5) . ? C81 C90 1.530(5) . ? C81 H81A 1.0000 . ? C82 C91 1.508(4) . ? C82 C92 1.536(5) . ? C82 H82A 1.0000 . ? C83 C93 1.517(4) . ? C83 C94 1.530(5) . ? C83 H83A 1.0000 . ? C84 C95 1.531(5) . ? C84 C96 1.533(4) . ? C84 H84A 1.0000 . ? C85 C86 1.507(4) . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C87 C88 1.494(4) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? 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 N3 Ni1 Cl1 177.16(6) . . ? N3 Ni1 P2 97.31(6) . . ? Cl1 Ni1 P2 85.29(3) . . ? N3 Ni1 P1 90.53(6) . . ? Cl1 Ni1 P1 86.91(3) . . ? P2 Ni1 P1 171.90(3) . . ? N6 Ni2 Cl2 171.65(7) . . ? N6 Ni2 P4 92.56(6) . . ? Cl2 Ni2 P4 86.29(3) . . ? N6 Ni2 P3 99.02(6) . . ? Cl2 Ni2 P3 83.69(3) . . ? P4 Ni2 P3 164.60(3) . . ? N9 Ni3 Cl3 175.00(7) . . ? N9 Ni3 P6 97.16(6) . . ? Cl3 Ni3 P6 83.69(3) . . ? N9 Ni3 P5 94.81(6) . . ? Cl3 Ni3 P5 84.84(3) . . ? P6 Ni3 P5 166.92(3) . . ? N12 Ni4 Cl4 172.70(7) . . ? N12 Ni4 P7 93.00(6) . . ? Cl4 Ni4 P7 85.60(3) . . ? N12 Ni4 P8 99.13(6) . . ? Cl4 Ni4 P8 83.37(3) . . ? P7 Ni4 P8 165.38(3) . . ? N15 Ni5 Cl5 177.17(7) . . ? N15 Ni5 P9 96.77(6) . . ? Cl5 Ni5 P9 85.53(3) . . ? N15 Ni5 P10 92.70(6) . . ? Cl5 Ni5 P10 85.11(3) . . ? P9 Ni5 P10 170.03(3) . . ? N18 Ni6 Cl6 176.80(6) . . ? N18 Ni6 P11 96.91(6) . . ? Cl6 Ni6 P11 86.21(3) . . ? N18 Ni6 P12 91.18(6) . . ? Cl6 Ni6 P12 85.70(3) . . ? P11 Ni6 P12 171.91(3) . . ? N1 P1 C2 106.54(12) . . ? N1 P1 C1 102.94(13) . . ? C2 P1 C1 104.81(13) . . ? N1 P1 Ni1 112.98(9) . . ? C2 P1 Ni1 114.94(9) . . ? C1 P1 Ni1 113.54(9) . . ? N2 P2 C3 102.47(11) . . ? N2 P2 C4 104.47(12) . . ? C3 P2 C4 107.08(12) . . ? N2 P2 Ni1 113.46(8) . . ? C3 P2 Ni1 115.84(9) . . ? C4 P2 Ni1 112.42(8) . . ? N4 P3 C18 104.61(12) . . ? N4 P3 C17 103.83(14) . . ? C18 P3 C17 105.25(14) . . ? N4 P3 Ni2 111.99(9) . . ? C18 P3 Ni2 114.01(10) . . ? C17 P3 Ni2 116.00(10) . . ? N5 P4 C20 104.73(14) . . ? N5 P4 C19 103.72(14) . . ? C20 P4 C19 105.59(14) . . ? N5 P4 Ni2 115.10(9) . . ? C20 P4 Ni2 116.75(9) . . ? C19 P4 Ni2 109.77(10) . . ? N7 P5 C33 105.11(13) . . ? N7 P5 C34 101.78(14) . . ? C33 P5 C34 106.47(14) . . ? N7 P5 Ni3 114.39(9) . . ? C33 P5 Ni3 114.84(10) . . ? C34 P5 Ni3 113.05(10) . . ? N8 P6 C35 105.74(13) . . ? N8 P6 C36 102.20(13) . . ? C35 P6 C36 105.56(14) . . ? N8 P6 Ni3 113.39(9) . . ? C35 P6 Ni3 112.65(9) . . ? C36 P6 Ni3 116.18(10) . . ? N10 P7 C50 104.87(13) . . ? N10 P7 C49 103.22(14) . . ? C50 P7 C49 106.77(15) . . ? N10 P7 Ni4 114.72(9) . . ? C50 P7 Ni4 116.47(10) . . ? C49 P7 Ni4 109.70(10) . . ? N11 P8 C52 104.68(12) . . ? N11 P8 C51 103.47(13) . . ? C52 P8 C51 105.18(13) . . ? N11 P8 Ni4 111.94(8) . . ? C52 P8 Ni4 113.57(9) . . ? C51 P8 Ni4 116.80(9) . . ? N13 P9 C66 102.68(12) . . ? N13 P9 C65 103.85(12) . . ? C66 P9 C65 106.60(14) . . ? N13 P9 Ni5 113.95(8) . . ? C66 P9 Ni5 113.88(9) . . ? C65 P9 Ni5 114.67(9) . . ? N14 P10 C68 103.87(13) . . ? N14 P10 C67 103.33(13) . . ? C68 P10 C67 106.25(13) . . ? N14 P10 Ni5 114.72(8) . . ? C68 P10 Ni5 111.18(9) . . ? C67 P10 Ni5 116.35(10) . . ? N16 P11 C81 104.17(13) . . ? N16 P11 C82 102.07(13) . . ? C81 P11 C82 105.50(17) . . ? N16 P11 Ni6 114.01(8) . . ? C81 P11 Ni6 115.90(11) . . ? C82 P11 Ni6 113.74(11) . . ? N17 P12 C83 101.60(14) . . ? N17 P12 C84 106.64(14) . . ? C83 P12 C84 106.47(15) . . ? N17 P12 Ni6 114.10(9) . . ? C83 P12 Ni6 114.82(11) . . ? C84 P12 Ni6 112.27(10) . . ? C5 N1 P1 127.51(18) . . ? C5 N1 H1A 116.2 . . ? P1 N1 H1A 116.2 . . ? C7 N2 P2 121.57(17) . . ? C7 N2 H2A 119.2 . . ? P2 N2 H2A 119.2 . . ? C6 N3 C8 111.0(2) . . ? C6 N3 Ni1 107.76(16) . . ? C8 N3 Ni1 121.60(16) . . ? C6 N3 H3B 105.0 . . ? C8 N3 H3B 105.0 . . ? Ni1 N3 H3B 105.0 . . ? C21 N4 P3 120.63(18) . . ? C21 N4 H4A 119.7 . . ? P3 N4 H4A 119.7 . . ? C23 N5 P4 126.61(19) . . ? C23 N5 H5A 116.7 . . ? P4 N5 H5A 116.7 . . ? C22 N6 C24 107.0(2) . . ? C22 N6 Ni2 118.28(16) . . ? C24 N6 Ni2 111.64(17) . . ? C22 N6 H6C 106.4 . . ? C24 N6 H6C 106.4 . . ? Ni2 N6 H6C 106.4 . . ? C37 N7 P5 126.03(19) . . ? C37 N7 H7A 117.0 . . ? P5 N7 H7A 117.0 . . ? C39 N8 P6 123.68(18) . . ? C39 N8 H8A 118.2 . . ? P6 N8 H8A 118.2 . . ? C40 N9 C38 105.68(19) . . ? C40 N9 Ni3 117.14(16) . . ? C38 N9 Ni3 113.45(16) . . ? C40 N9 H9D 106.6 . . ? C38 N9 H9D 106.6 . . ? Ni3 N9 H9D 106.6 . . ? C53 N10 P7 126.68(19) . . ? C53 N10 H10A 116.7 . . ? P7 N10 H10A 116.7 . . ? C55 N11 P8 120.62(17) . . ? C55 N11 H11A 119.7 . . ? P8 N11 H11A 119.7 . . ? C56 N12 C54 107.3(2) . . ? C56 N12 Ni4 118.19(16) . . ? C54 N12 Ni4 111.77(16) . . ? C56 N12 H12D 106.3 . . ? C54 N12 H12D 106.3 . . ? Ni4 N12 H12D 106.3 . . ? C69 N13 P9 117.09(16) . . ? C69 N13 H13A 121.5 . . ? P9 N13 H13A 121.5 . . ? C71 N14 P10 125.05(18) . . ? C71 N14 H14A 117.5 . . ? P10 N14 H14A 117.5 . . ? C70 N15 C72 106.92(19) . . ? C70 N15 Ni5 121.31(16) . . ? C72 N15 Ni5 113.54(16) . . ? C70 N15 H15D 104.5 . . ? C72 N15 H15D 104.5 . . ? Ni5 N15 H15D 104.5 . . ? C85 N16 P11 117.05(17) . . ? C85 N16 H16A 121.5 . . ? P11 N16 H16A 121.5 . . ? C87 N17 P12 127.74(19) . . ? C87 N17 H17A 116.1 . . ? P12 N17 H17A 116.1 . . ? C86 N18 C88 108.2(2) . . ? C86 N18 Ni6 121.05(16) . . ? C88 N18 Ni6 112.13(16) . . ? C86 N18 H18B 104.6 . . ? C88 N18 H18B 104.6 . . ? Ni6 N18 H18B 104.6 . . ? C10 C1 C9 111.4(2) . . ? C10 C1 P1 114.3(2) . . ? C9 C1 P1 108.32(19) . . ? C10 C1 H1B 107.5 . . ? C9 C1 H1B 107.5 . . ? P1 C1 H1B 107.5 . . ? C12 C2 C11 111.4(2) . . ? C12 C2 P1 109.2(2) . . ? C11 C2 P1 112.1(2) . . ? C12 C2 H2B 108.0 . . ? C11 C2 H2B 108.0 . . ? P1 C2 H2B 108.0 . . ? C14 C3 C13 110.8(2) . . ? C14 C3 P2 115.65(18) . . ? C13 C3 P2 109.49(19) . . ? C14 C3 H3A 106.8 . . ? C13 C3 H3A 106.8 . . ? P2 C3 H3A 106.8 . . ? C15 C4 C16 111.4(2) . . ? C15 C4 P2 107.93(18) . . ? C16 C4 P2 111.99(19) . . ? C15 C4 H4B 108.5 . . ? C16 C4 H4B 108.5 . . ? P2 C4 H4B 108.5 . . ? N1 C5 C6 114.2(2) . . ? N1 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? N1 C5 H5C 108.7 . . ? C6 C5 H5C 108.7 . . ? H5B C5 H5C 107.6 . . ? N3 C6 C5 111.4(2) . . ? N3 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N3 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 112.5(2) . . ? N2 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? N2 C7 H7C 109.1 . . ? C8 C7 H7C 109.1 . . ? H7B C7 H7C 107.8 . . ? C7 C8 N3 114.0(2) . . ? C7 C8 H8B 108.8 . . ? N3 C8 H8B 108.8 . . ? C7 C8 H8C 108.8 . . ? N3 C8 H8C 108.8 . . ? H8B C8 H8C 107.6 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C1 C10 H10D 109.5 . . ? H10B C10 H10D 109.5 . . ? H10C C10 H10D 109.5 . . ? C2 C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C11 H11D 109.5 . . ? H11B C11 H11D 109.5 . . ? H11C C11 H11D 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C13 H13D 109.5 . . ? H13B C13 H13D 109.5 . . ? H13C C13 H13D 109.5 . . ? C3 C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C3 C14 H14D 109.5 . . ? H14B C14 H14D 109.5 . . ? H14C C14 H14D 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C4 C16 H16D 109.5 . . ? H16B C16 H16D 109.5 . . ? H16C C16 H16D 109.5 . . ? C26 C17 C25 111.0(3) . . ? C26 C17 P3 117.7(2) . . ? C25 C17 P3 109.6(2) . . ? C26 C17 H17B 105.9 . . ? C25 C17 H17B 105.9 . . ? P3 C17 H17B 105.9 . . ? C28 C18 C27 111.6(3) . . ? C28 C18 P3 109.2(2) . . ? C27 C18 P3 113.4(2) . . ? C28 C18 H18A 107.5 . . ? C27 C18 H18A 107.5 . . ? P3 C18 H18A 107.5 . . ? C29 C19 C30 111.4(3) . . ? C29 C19 P4 114.6(2) . . ? C30 C19 P4 109.0(2) . . ? C29 C19 H19A 107.1 . . ? C30 C19 H19A 107.1 . . ? P4 C19 H19A 107.1 . . ? C31 C20 C32 110.9(3) . . ? C31 C20 P4 108.7(2) . . ? C32 C20 P4 112.7(2) . . ? C31 C20 H20A 108.1 . . ? C32 C20 H20A 108.1 . . ? P4 C20 H20A 108.1 . . ? N4 C21 C22 112.8(2) . . ? N4 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? N4 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? N6 C22 C21 113.5(2) . . ? N6 C22 H22A 108.9 . . ? C21 C22 H22A 108.9 . . ? N6 C22 H22B 108.9 . . ? C21 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? N5 C23 C24 113.8(2) . . ? N5 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? N5 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N6 C24 C23 113.5(2) . . ? N6 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? N6 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C17 C25 H25A 109.5 . . ? C17 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C17 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C17 C26 H26A 109.5 . . ? C17 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C17 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C18 C27 H27A 109.5 . . ? C18 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C18 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C19 C29 H29A 109.5 . . ? C19 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C19 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C19 C30 H30A 109.5 . . ? C19 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C19 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C20 C31 H31A 109.5 . . ? C20 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C20 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C20 C32 H32A 109.5 . . ? C20 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C20 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C41 C33 C42 111.1(3) . . ? C41 C33 P5 108.9(2) . . ? C42 C33 P5 112.6(2) . . ? C41 C33 H33A 108.0 . . ? C42 C33 H33A 108.0 . . ? P5 C33 H33A 108.0 . . ? C43 C34 C44 111.5(3) . . ? C43 C34 P5 108.9(2) . . ? C44 C34 P5 116.5(2) . . ? C43 C34 H34A 106.5 . . ? C44 C34 H34A 106.5 . . ? P5 C34 H34A 106.5 . . ? C45 C35 C46 110.7(3) . . ? C45 C35 P6 109.9(2) . . ? C46 C35 P6 112.2(2) . . ? C45 C35 H35A 107.9 . . ? C46 C35 H35A 107.9 . . ? P6 C35 H35A 107.9 . . ? C48 C36 C47 110.1(3) . . ? C48 C36 P6 117.5(2) . . ? C47 C36 P6 109.2(2) . . ? C48 C36 H36A 106.5 . . ? C47 C36 H36A 106.5 . . ? P6 C36 H36A 106.5 . . ? N7 C37 C38 115.0(2) . . ? N7 C37 H37A 108.5 . . ? C38 C37 H37A 108.5 . . ? N7 C37 H37B 108.5 . . ? C38 C37 H37B 108.5 . . ? H37A C37 H37B 107.5 . . ? N9 C38 C37 114.9(2) . . ? N9 C38 H38A 108.6 . . ? C37 C38 H38A 108.6 . . ? N9 C38 H38B 108.6 . . ? C37 C38 H38B 108.6 . . ? H38A C38 H38B 107.5 . . ? N8 C39 C40 113.6(2) . . ? N8 C39 H39A 108.8 . . ? C40 C39 H39A 108.8 . . ? N8 C39 H39B 108.8 . . ? C40 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C39 C40 N9 114.4(2) . . ? C39 C40 H40A 108.7 . . ? N9 C40 H40A 108.7 . . ? C39 C40 H40B 108.7 . . ? N9 C40 H40B 108.7 . . ? H40A C40 H40B 107.6 . . ? C33 C41 H41A 109.5 . . ? C33 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C33 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C33 C42 H42A 109.5 . . ? C33 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C33 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C34 C43 H43A 109.5 . . ? C34 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C34 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C34 C44 H44A 109.5 . . ? C34 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C34 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C35 C45 H45A 109.5 . . ? C35 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C35 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C35 C46 H46A 109.5 . . ? C35 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C35 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C36 C47 H47A 109.5 . . ? C36 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C36 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C36 C48 H48A 109.5 . . ? C36 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C36 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C58 C49 C57 111.2(3) . . ? C58 C49 P7 115.4(2) . . ? C57 C49 P7 108.7(2) . . ? C58 C49 H49A 107.0 . . ? C57 C49 H49A 107.0 . . ? P7 C49 H49A 107.0 . . ? C60 C50 C59 112.2(3) . . ? C60 C50 P7 108.6(2) . . ? C59 C50 P7 112.4(2) . . ? C60 C50 H50A 107.8 . . ? C59 C50 H50A 107.8 . . ? P7 C50 H50A 107.8 . . ? C61 C51 C62 110.9(3) . . ? C61 C51 P8 109.8(2) . . ? C62 C51 P8 117.6(2) . . ? C61 C51 H51A 105.9 . . ? C62 C51 H51A 105.9 . . ? P8 C51 H51A 105.9 . . ? C63 C52 C64 111.3(3) . . ? C63 C52 P8 109.3(2) . . ? C64 C52 P8 112.76(19) . . ? C63 C52 H52A 107.8 . . ? C64 C52 H52A 107.8 . . ? P8 C52 H52A 107.8 . . ? N10 C53 C54 114.1(2) . . ? N10 C53 H53A 108.7 . . ? C54 C53 H53A 108.7 . . ? N10 C53 H53B 108.7 . . ? C54 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? C53 C54 N12 113.3(2) . . ? C53 C54 H54A 108.9 . . ? N12 C54 H54A 108.9 . . ? C53 C54 H54B 108.9 . . ? N12 C54 H54B 108.9 . . ? H54A C54 H54B 107.7 . . ? N11 C55 C56 112.8(2) . . ? N11 C55 H55A 109.0 . . ? C56 C55 H55A 109.0 . . ? N11 C55 H55B 109.0 . . ? C56 C55 H55B 109.0 . . ? H55A C55 H55B 107.8 . . ? N12 C56 C55 113.2(2) . . ? N12 C56 H56A 108.9 . . ? C55 C56 H56A 108.9 . . ? N12 C56 H56B 108.9 . . ? C55 C56 H56B 108.9 . . ? H56A C56 H56B 107.7 . . ? C49 C57 H57A 109.5 . . ? C49 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C49 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C49 C58 H58A 109.5 . . ? C49 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C49 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C50 C59 H59A 109.5 . . ? C50 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C50 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C50 C60 H60A 109.5 . . ? C50 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C50 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C51 C61 H61A 109.5 . . ? C51 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C51 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C51 C62 H62A 109.5 . . ? C51 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C51 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C52 C63 H63A 109.5 . . ? C52 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C52 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C52 C64 H64A 109.5 . . ? C52 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C52 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C73 C65 C74 111.7(3) . . ? C73 C65 P9 107.5(2) . . ? C74 C65 P9 112.5(2) . . ? C73 C65 H65A 108.3 . . ? C74 C65 H65A 108.3 . . ? P9 C65 H65A 108.3 . . ? C75 C66 C76 111.1(3) . . ? C75 C66 P9 113.4(2) . . ? C76 C66 P9 110.0(2) . . ? C75 C66 H66A 107.4 . . ? C76 C66 H66A 107.4 . . ? P9 C66 H66A 107.4 . . ? C78 C67 C77 112.1(3) . . ? C78 C67 P10 116.4(2) . . ? C77 C67 P10 108.3(2) . . ? C78 C67 H67A 106.5 . . ? C77 C67 H67A 106.5 . . ? P10 C67 H67A 106.5 . . ? C79 C68 C80 111.1(3) . . ? C79 C68 P10 112.5(2) . . ? C80 C68 P10 108.6(2) . . ? C79 C68 H68A 108.2 . . ? C80 C68 H68A 108.2 . . ? P10 C68 H68A 108.2 . . ? N13 C69 C70 112.5(2) . . ? N13 C69 H69A 109.1 . . ? C70 C69 H69A 109.1 . . ? N13 C69 H69B 109.1 . . ? C70 C69 H69B 109.1 . . ? H69A C69 H69B 107.8 . . ? N15 C70 C69 113.1(2) . . ? N15 C70 H70A 109.0 . . ? C69 C70 H70A 109.0 . . ? N15 C70 H70B 109.0 . . ? C69 C70 H70B 109.0 . . ? H70A C70 H70B 107.8 . . ? N14 C71 C72 113.6(2) . . ? N14 C71 H71A 108.8 . . ? C72 C71 H71A 108.8 . . ? N14 C71 H71B 108.8 . . ? C72 C71 H71B 108.8 . . ? H71A C71 H71B 107.7 . . ? C71 C72 N15 112.5(2) . . ? C71 C72 H72A 109.1 . . ? N15 C72 H72A 109.1 . . ? C71 C72 H72B 109.1 . . ? N15 C72 H72B 109.1 . . ? H72A C72 H72B 107.8 . . ? C65 C73 H73A 109.5 . . ? C65 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C65 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C65 C74 H74A 109.5 . . ? C65 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C65 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C66 C75 H75A 109.5 . . ? C66 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C66 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C66 C76 H76A 109.5 . . ? C66 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C66 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C67 C77 H77A 109.5 . . ? C67 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C67 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C67 C78 H78A 109.5 . . ? C67 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C67 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C68 C79 H79A 109.5 . . ? C68 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C68 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C68 C80 H80A 109.5 . . ? C68 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C68 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C89 C81 C90 111.5(3) . . ? C89 C81 P11 107.9(3) . . ? C90 C81 P11 112.8(2) . . ? C89 C81 H81A 108.2 . . ? C90 C81 H81A 108.2 . . ? P11 C81 H81A 108.2 . . ? C91 C82 C92 111.4(3) . . ? C91 C82 P11 114.1(3) . . ? C92 C82 P11 109.7(2) . . ? C91 C82 H82A 107.1 . . ? C92 C82 H82A 107.1 . . ? P11 C82 H82A 107.1 . . ? C93 C83 C94 110.6(3) . . ? C93 C83 P12 116.4(2) . . ? C94 C83 P12 109.0(2) . . ? C93 C83 H83A 106.8 . . ? C94 C83 H83A 106.8 . . ? P12 C83 H83A 106.8 . . ? C95 C84 C96 111.2(3) . . ? C95 C84 P12 109.2(2) . . ? C96 C84 P12 111.9(2) . . ? C95 C84 H84A 108.1 . . ? C96 C84 H84A 108.1 . . ? P12 C84 H84A 108.1 . . ? N16 C85 C86 112.8(2) . . ? N16 C85 H85A 109.0 . . ? C86 C85 H85A 109.0 . . ? N16 C85 H85B 109.0 . . ? C86 C85 H85B 109.0 . . ? H85A C85 H85B 107.8 . . ? N18 C86 C85 113.3(2) . . ? N18 C86 H86A 108.9 . . ? C85 C86 H86A 108.9 . . ? N18 C86 H86B 108.9 . . ? C85 C86 H86B 108.9 . . ? H86A C86 H86B 107.7 . . ? N17 C87 C88 113.8(2) . . ? N17 C87 H87A 108.8 . . ? C88 C87 H87A 108.8 . . ? N17 C87 H87B 108.8 . . ? C88 C87 H87B 108.8 . . ? H87A C87 H87B 107.7 . . ? C87 C88 N18 112.8(2) . . ? C87 C88 H88A 109.0 . . ? N18 C88 H88A 109.0 . . ? C87 C88 H88B 109.0 . . ? N18 C88 H88B 109.0 . . ? H88A C88 H88B 107.8 . . ? C81 C89 H89A 109.5 . . ? C81 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C81 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C81 C90 H90A 109.5 . . ? C81 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C81 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C82 C91 H91A 109.5 . . ? C82 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C82 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C82 C92 H92A 109.5 . . ? C82 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C82 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C83 C93 H93A 109.5 . . ? C83 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C83 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C83 C94 H94A 109.5 . . ? C83 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C83 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C84 C95 H95A 109.5 . . ? C84 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C84 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C84 C96 H96A 109.5 . . ? C84 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C84 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.725 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.072 #=== END data_mjs056_compound4a _database_code_depnum_ccdc_archive 'CCDC 867385' #TrackingRef '- All Cif Files Compiled.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C16 H39 Cl2 N3 P2 Pd' _chemical_formula_weight 512.74 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' 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 Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 23.205(6) _cell_length_b 10.981(2) _cell_length_c 8.9992(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2293.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3484 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 23.27 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6058 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 16227 _diffrn_reflns_av_R_equivalents 0.0686 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.67 _reflns_number_total 4271 _reflns_number_gt 3147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0434P)^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 0.14(5) _refine_ls_number_reflns 4271 _refine_ls_number_parameters 217 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.613835(18) 0.71565(4) 0.75353(7) 0.03160(14) Uani 1 1 d . . . Cl1 Cl 0.71239(7) 0.71831(17) 0.7381(4) 0.0589(6) Uani 1 1 d . . . Cl2 Cl 0.49188(8) 0.75395(15) 0.1182(2) 0.0436(5) Uani 1 1 d . . . P1 P 0.61762(8) 0.92075(17) 0.6842(2) 0.0340(4) Uani 1 1 d . . . P2 P 0.62645(7) 0.51256(17) 0.8154(2) 0.0314(4) Uani 1 1 d . . . N1 N 0.5532(2) 0.9793(5) 0.6585(6) 0.0365(15) Uani 1 1 d . . . H1A H 0.5491 1.0421 0.5986 0.044 Uiso 1 1 calc R . . N2 N 0.5655(2) 0.4365(5) 0.8405(6) 0.0370(14) Uani 1 1 d . . . H2A H 0.5653 0.3565 0.8338 0.044 Uiso 1 1 calc R . . N3 N 0.5241(2) 0.7118(5) 0.7792(7) 0.0342(16) Uani 1 1 d . . . H3B H 0.5181 0.7332 0.8780 0.041 Uiso 1 1 calc R . . C1 C 0.6519(3) 1.0315(7) 0.8166(9) 0.052(2) Uani 1 1 d . . . H1B H 0.6384 1.1151 0.7899 0.062 Uiso 1 1 calc R . . C2 C 0.6540(3) 0.9406(6) 0.5066(8) 0.0364(18) Uani 1 1 d . . . H2B H 0.6956 0.9199 0.5211 0.044 Uiso 1 1 calc R . . C3 C 0.6664(3) 0.4994(6) 0.9915(8) 0.0335(17) Uani 1 1 d . . . H3A H 0.7074 0.5219 0.9721 0.040 Uiso 1 1 calc R . . C4 C 0.6609(3) 0.4135(7) 0.6820(8) 0.0402(18) Uani 1 1 d . . . H4A H 0.6456 0.3299 0.7018 0.048 Uiso 1 1 calc R . . C5 C 0.5031(3) 0.9298(6) 0.7320(10) 0.044(2) Uani 1 1 d . . . H5A H 0.4695 0.9814 0.7075 0.053 Uiso 1 1 calc R . . H5B H 0.5092 0.9348 0.8407 0.053 Uiso 1 1 calc R . . C6 C 0.4893(3) 0.8017(6) 0.6928(8) 0.045(2) Uani 1 1 d . . . H6A H 0.4964 0.7893 0.5854 0.054 Uiso 1 1 calc R . . H6B H 0.4478 0.7868 0.7116 0.054 Uiso 1 1 calc R . . C7 C 0.5128(3) 0.5006(6) 0.8732(9) 0.0374(17) Uani 1 1 d . . . H7A H 0.5172 0.5411 0.9708 0.045 Uiso 1 1 calc R . . H7B H 0.4815 0.4399 0.8830 0.045 Uiso 1 1 calc R . . C8 C 0.4947(2) 0.5935(5) 0.7629(10) 0.0346(14) Uani 1 1 d . . . H8A H 0.5022 0.5617 0.6618 0.042 Uiso 1 1 calc R . . H8B H 0.4526 0.6065 0.7724 0.042 Uiso 1 1 calc R . . C9 C 0.7161(3) 1.0319(9) 0.8148(10) 0.078(3) Uani 1 1 d . . . H9A H 0.7304 1.0926 0.8855 0.117 Uiso 1 1 calc R . . H9B H 0.7297 1.0521 0.7147 0.117 Uiso 1 1 calc R . . H9C H 0.7304 0.9511 0.8428 0.117 Uiso 1 1 calc R . . C10 C 0.6300(4) 1.0024(8) 0.9719(9) 0.059(2) Uani 1 1 d . . . H10A H 0.6468 1.0596 1.0432 0.088 Uiso 1 1 calc R . . H10B H 0.6411 0.9191 0.9986 0.088 Uiso 1 1 calc R . . H10C H 0.5879 1.0096 0.9739 0.088 Uiso 1 1 calc R . . C11 C 0.6507(3) 1.0718(7) 0.4494(9) 0.049(2) Uani 1 1 d . . . H11A H 0.6710 1.0779 0.3542 0.073 Uiso 1 1 calc R . . H11B H 0.6687 1.1267 0.5217 0.073 Uiso 1 1 calc R . . H11C H 0.6102 1.0948 0.4356 0.073 Uiso 1 1 calc R . . C12 C 0.6294(3) 0.8523(8) 0.3961(9) 0.055(2) Uani 1 1 d . . . H12A H 0.6493 0.8616 0.3008 0.083 Uiso 1 1 calc R . . H12B H 0.5882 0.8688 0.3826 0.083 Uiso 1 1 calc R . . H12C H 0.6346 0.7690 0.4327 0.083 Uiso 1 1 calc R . . C13 C 0.6426(3) 0.5867(7) 1.1048(8) 0.0450(19) Uani 1 1 d . . . H13A H 0.6643 0.5788 1.1977 0.068 Uiso 1 1 calc R . . H13B H 0.6019 0.5680 1.1230 0.068 Uiso 1 1 calc R . . H13C H 0.6461 0.6702 1.0674 0.068 Uiso 1 1 calc R . . C14 C 0.6651(3) 0.3690(7) 1.0503(8) 0.051(2) Uani 1 1 d . . . H14A H 0.6870 0.3645 1.1432 0.076 Uiso 1 1 calc R . . H14B H 0.6823 0.3142 0.9767 0.076 Uiso 1 1 calc R . . H14C H 0.6251 0.3447 1.0689 0.076 Uiso 1 1 calc R . . C15 C 0.6416(3) 0.4461(7) 0.5263(8) 0.045(2) Uani 1 1 d . . . H15A H 0.6604 0.3917 0.4548 0.068 Uiso 1 1 calc R . . H15B H 0.6524 0.5306 0.5047 0.068 Uiso 1 1 calc R . . H15C H 0.5997 0.4372 0.5187 0.068 Uiso 1 1 calc R . . C16 C 0.7265(3) 0.4034(7) 0.6902(8) 0.053(2) Uani 1 1 d . . . H16A H 0.7401 0.3467 0.6137 0.079 Uiso 1 1 calc R . . H16B H 0.7378 0.3731 0.7885 0.079 Uiso 1 1 calc R . . H16C H 0.7437 0.4837 0.6737 0.079 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 0.0248(2) 0.0404(2) 0.0296(2) 0.0064(3) -0.0006(3) 0.0015(2) Cl1 0.0267(8) 0.0612(10) 0.0888(16) 0.0249(13) 0.0046(14) 0.0007(8) Cl2 0.0600(13) 0.0304(8) 0.0405(9) -0.0008(8) 0.0071(9) 0.0037(8) P1 0.0353(11) 0.0399(10) 0.0266(9) 0.0079(9) -0.0001(9) 0.0009(9) P2 0.0241(9) 0.0399(10) 0.0301(10) 0.0025(8) -0.0030(7) 0.0018(8) N1 0.034(3) 0.038(3) 0.038(4) 0.020(3) 0.014(3) 0.014(3) N2 0.030(3) 0.034(3) 0.047(4) 0.001(3) 0.003(3) 0.005(3) N3 0.038(3) 0.042(3) 0.023(4) 0.004(3) -0.007(3) 0.001(3) C1 0.056(5) 0.047(5) 0.053(5) -0.002(4) -0.002(5) 0.002(4) C2 0.035(4) 0.042(4) 0.033(4) 0.005(4) 0.002(3) 0.005(3) C3 0.017(4) 0.045(4) 0.038(4) 0.008(4) -0.001(3) 0.004(3) C4 0.037(4) 0.057(5) 0.027(4) 0.002(4) -0.001(4) 0.006(4) C5 0.032(4) 0.045(4) 0.055(6) 0.019(4) 0.002(4) 0.014(3) C6 0.038(4) 0.047(4) 0.051(5) 0.010(4) -0.006(3) 0.006(4) C7 0.031(4) 0.032(3) 0.049(5) -0.007(3) 0.003(3) 0.001(3) C8 0.022(3) 0.042(4) 0.040(4) -0.003(4) 0.003(4) -0.005(3) C9 0.060(6) 0.125(9) 0.048(6) -0.025(5) -0.003(5) 0.015(6) C10 0.068(6) 0.066(6) 0.042(5) -0.010(4) 0.020(4) -0.009(5) C11 0.038(5) 0.063(5) 0.045(5) 0.018(4) 0.009(4) 0.006(4) C12 0.049(5) 0.076(6) 0.041(5) -0.005(5) 0.005(4) -0.005(4) C13 0.047(5) 0.062(5) 0.026(4) 0.003(4) -0.002(4) -0.007(4) C14 0.043(5) 0.071(6) 0.039(5) 0.021(4) -0.011(4) 0.004(4) C15 0.037(5) 0.068(6) 0.030(4) 0.001(4) -0.001(4) 0.005(4) C16 0.027(4) 0.083(6) 0.049(5) 0.005(4) -0.002(3) 0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N3 2.097(5) . ? Pd1 Cl1 2.2913(17) . ? Pd1 P2 2.3172(19) . ? Pd1 P1 2.3387(19) . ? P1 N1 1.644(5) . ? P1 C2 1.821(7) . ? P1 C1 1.879(8) . ? P2 N2 1.658(5) . ? P2 C4 1.806(7) . ? P2 C3 1.841(7) . ? N1 C5 1.443(8) . ? N1 H1A 0.8800 . ? N2 C7 1.441(8) . ? N2 H2A 0.8800 . ? N3 C8 1.474(7) . ? N3 C6 1.494(8) . ? N3 H3B 0.9300 . ? C1 C9 1.489(10) . ? C1 C10 1.521(10) . ? C1 H1B 1.0000 . ? C2 C12 1.502(10) . ? C2 C11 1.532(9) . ? C2 H2B 1.0000 . ? C3 C13 1.505(10) . ? C3 C14 1.527(10) . ? C3 H3A 1.0000 . ? C4 C15 1.513(9) . ? C4 C16 1.530(9) . ? C4 H4A 1.0000 . ? C5 C6 1.486(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.485(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 N3 Pd1 Cl1 177.1(2) . . ? N3 Pd1 P2 94.56(15) . . ? Cl1 Pd1 P2 84.30(6) . . ? N3 Pd1 P1 94.95(15) . . ? Cl1 Pd1 P1 86.22(7) . . ? P2 Pd1 P1 170.48(6) . . ? N1 P1 C2 104.6(3) . . ? N1 P1 C1 102.8(3) . . ? C2 P1 C1 106.4(3) . . ? N1 P1 Pd1 112.3(2) . . ? C2 P1 Pd1 111.5(2) . . ? C1 P1 Pd1 118.0(3) . . ? N2 P2 C4 99.4(3) . . ? N2 P2 C3 105.8(3) . . ? C4 P2 C3 107.6(3) . . ? N2 P2 Pd1 114.2(2) . . ? C4 P2 Pd1 118.4(3) . . ? C3 P2 Pd1 110.2(2) . . ? C5 N1 P1 121.3(4) . . ? C5 N1 H1A 119.3 . . ? P1 N1 H1A 119.3 . . ? C7 N2 P2 120.3(5) . . ? C7 N2 H2A 119.8 . . ? P2 N2 H2A 119.8 . . ? C8 N3 C6 106.3(5) . . ? C8 N3 Pd1 117.8(4) . . ? C6 N3 Pd1 117.8(4) . . ? C8 N3 H3B 104.4 . . ? C6 N3 H3B 104.4 . . ? Pd1 N3 H3B 104.4 . . ? C9 C1 C10 110.2(7) . . ? C9 C1 P1 114.7(6) . . ? C10 C1 P1 107.7(5) . . ? C9 C1 H1B 108.0 . . ? C10 C1 H1B 108.0 . . ? P1 C1 H1B 108.0 . . ? C12 C2 C11 111.4(7) . . ? C12 C2 P1 109.1(5) . . ? C11 C2 P1 112.6(5) . . ? C12 C2 H2B 107.8 . . ? C11 C2 H2B 107.8 . . ? P1 C2 H2B 107.8 . . ? C13 C3 C14 110.8(6) . . ? C13 C3 P2 110.4(5) . . ? C14 C3 P2 111.3(5) . . ? C13 C3 H3A 108.1 . . ? C14 C3 H3A 108.1 . . ? P2 C3 H3A 108.1 . . ? C15 C4 C16 110.8(6) . . ? C15 C4 P2 110.0(5) . . ? C16 C4 P2 116.9(5) . . ? C15 C4 H4A 106.1 . . ? C16 C4 H4A 106.1 . . ? P2 C4 H4A 106.1 . . ? N1 C5 C6 115.0(6) . . ? N1 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? N1 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 N3 112.6(6) . . ? C5 C6 H6A 109.1 . . ? N3 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? N3 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? N2 C7 C8 116.1(6) . . ? N2 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? N2 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N3 C8 C7 114.1(6) . . ? N3 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? N3 C8 H8B 108.7 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.070 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.100 #=== END data_mjs029_0m_compound5a _database_code_depnum_ccdc_archive 'CCDC 867386' #TrackingRef '- All Cif Files Compiled.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C17 H40 Cl4 N2 Ni P2 S' _chemical_formula_weight 567.02 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' S S 0.1246 0.1234 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4687(10) _cell_length_b 11.3598(13) _cell_length_c 15.5241(18) _cell_angle_alpha 82.318(7) _cell_angle_beta 74.896(7) _cell_angle_gamma 68.538(6) _cell_volume 1340.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3551 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 24.04 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4885 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 15080 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4503 _reflns_number_gt 2723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0572P)^2^+2.1456P] 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 4503 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1121 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1568 _refine_ls_wR_factor_gt 0.1273 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.97858(9) 0.36336(6) 0.27594(5) 0.0344(2) Uani 1 1 d . . . Cl1 Cl 1.0395(3) 0.32302(14) 0.40597(12) 0.0625(5) Uani 1 1 d . . . Cl2 Cl 0.8792(2) 0.90592(15) 0.13746(12) 0.0562(5) Uani 1 1 d . . . Cl3 Cl 0.4752(3) 0.6925(2) 0.94334(16) 0.0874(7) Uani 1 1 d . . . Cl4 Cl 0.4575(3) 0.86905(18) 1.06471(14) 0.0796(7) Uani 1 1 d . . . S1 S 0.9651(2) 0.41289(14) 0.13744(11) 0.0422(4) Uani 1 1 d . . . P1 P 1.01061(19) 0.15932(14) 0.27365(11) 0.0360(4) Uani 1 1 d . . . P2 P 0.91889(18) 0.56989(13) 0.29571(11) 0.0342(4) Uani 1 1 d . . . N1 N 1.0329(7) 0.1084(4) 0.1748(3) 0.0467(14) Uani 1 1 d . . . H1A H 1.0019 0.0429 0.1733 0.056 Uiso 1 1 calc R . . N2 N 0.7978(6) 0.6589(4) 0.2268(4) 0.0443(13) Uani 1 1 d . . . H2A H 0.8074 0.7323 0.2051 0.053 Uiso 1 1 calc R . . C1 C 0.8093(8) 0.1328(6) 0.3369(4) 0.0470(17) Uani 1 1 d . . . H1B H 0.8133 0.0505 0.3185 0.056 Uiso 1 1 calc R . . C2 C 1.1918(8) 0.0472(5) 0.3204(4) 0.0428(16) Uani 1 1 d . . . H2B H 1.1724 0.0672 0.3840 0.051 Uiso 1 1 calc R . . C3 C 0.7999(7) 0.6256(5) 0.4087(4) 0.0390(15) Uani 1 1 d . . . H3A H 0.8780 0.5817 0.4503 0.047 Uiso 1 1 calc R . . C4 C 1.1086(7) 0.6194(5) 0.2701(4) 0.0399(15) Uani 1 1 d . . . H4A H 1.0641 0.7140 0.2674 0.048 Uiso 1 1 calc R . . C5 C 1.0999(8) 0.1645(6) 0.0908(5) 0.0517(18) Uani 1 1 d . . . H5A H 1.1257 0.1070 0.0424 0.062 Uiso 1 1 calc R . . H5B H 1.2104 0.1740 0.0929 0.062 Uiso 1 1 calc R . . C6 C 0.9743(9) 0.2915(6) 0.0696(4) 0.0537(18) Uani 1 1 d . . . H6A H 0.8566 0.2861 0.0801 0.064 Uiso 1 1 calc R . . H6B H 1.0103 0.3151 0.0057 0.064 Uiso 1 1 calc R . . C7 C 0.6764(8) 0.6145(6) 0.2029(5) 0.0514(18) Uani 1 1 d . . . H7A H 0.5789 0.6885 0.1883 0.062 Uiso 1 1 calc R . . H7B H 0.6276 0.5680 0.2552 0.062 Uiso 1 1 calc R . . C8 C 0.7558(8) 0.5294(6) 0.1250(5) 0.0532(18) Uani 1 1 d . . . H8A H 0.7726 0.5807 0.0688 0.064 Uiso 1 1 calc R . . H8B H 0.6761 0.4854 0.1215 0.064 Uiso 1 1 calc R . . C9 C 0.7879(9) 0.1228(7) 0.4390(5) 0.068(2) Uani 1 1 d . . . H9A H 0.6784 0.1086 0.4680 0.101 Uiso 1 1 calc R . . H9B H 0.7858 0.2015 0.4593 0.101 Uiso 1 1 calc R . . H9C H 0.8858 0.0518 0.4548 0.101 Uiso 1 1 calc R . . C10 C 0.6514(8) 0.2359(7) 0.3113(5) 0.065(2) Uani 1 1 d . . . H10A H 0.5448 0.2210 0.3452 0.098 Uiso 1 1 calc R . . H10B H 0.6603 0.2340 0.2472 0.098 Uiso 1 1 calc R . . H10C H 0.6477 0.3187 0.3249 0.098 Uiso 1 1 calc R . . C11 C 1.2007(10) -0.0907(5) 0.3176(5) 0.066(2) Uani 1 1 d . . . H11A H 1.2968 -0.1484 0.3434 0.098 Uiso 1 1 calc R . . H11B H 1.2203 -0.1115 0.2556 0.098 Uiso 1 1 calc R . . H11C H 1.0906 -0.0995 0.3522 0.098 Uiso 1 1 calc R . . C12 C 1.3613(8) 0.0647(6) 0.2673(5) 0.065(2) Uani 1 1 d . . . H12A H 1.4588 0.0061 0.2917 0.098 Uiso 1 1 calc R . . H12B H 1.3538 0.1520 0.2716 0.098 Uiso 1 1 calc R . . H12C H 1.3803 0.0473 0.2046 0.098 Uiso 1 1 calc R . . C13 C 0.6372(8) 0.5899(7) 0.4398(5) 0.061(2) Uani 1 1 d . . . H13A H 0.5771 0.6193 0.5002 0.092 Uiso 1 1 calc R . . H13B H 0.6701 0.4977 0.4402 0.092 Uiso 1 1 calc R . . H13C H 0.5595 0.6296 0.3990 0.092 Uiso 1 1 calc R . . C14 C 0.7559(8) 0.7687(5) 0.4132(5) 0.057(2) Uani 1 1 d . . . H14A H 0.6937 0.7950 0.4741 0.086 Uiso 1 1 calc R . . H14B H 0.6821 0.8142 0.3716 0.086 Uiso 1 1 calc R . . H14C H 0.8639 0.7880 0.3968 0.086 Uiso 1 1 calc R . . C15 C 1.2140(8) 0.5767(6) 0.3413(5) 0.0556(19) Uani 1 1 d . . . H15A H 1.3131 0.6068 0.3240 0.083 Uiso 1 1 calc R . . H15B H 1.2569 0.4841 0.3474 0.083 Uiso 1 1 calc R . . H15C H 1.1400 0.6119 0.3984 0.083 Uiso 1 1 calc R . . C16 C 1.2257(9) 0.5770(7) 0.1776(5) 0.067(2) Uani 1 1 d . . . H16A H 1.3255 0.6058 0.1656 0.100 Uiso 1 1 calc R . . H16B H 1.1586 0.6138 0.1318 0.100 Uiso 1 1 calc R . . H16C H 1.2675 0.4844 0.1766 0.100 Uiso 1 1 calc R . . C17 C 0.3473(9) 0.8350(6) 0.9950(5) 0.067(2) Uani 1 1 d . . . H17A H 0.2351 0.8287 1.0308 0.081 Uiso 1 1 calc R . . H17B H 0.3220 0.9043 0.9491 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0341(4) 0.0267(4) 0.0412(5) -0.0022(3) -0.0128(3) -0.0061(3) Cl1 0.0998(14) 0.0321(8) 0.0542(11) -0.0048(8) -0.0413(10) -0.0040(9) Cl2 0.0742(11) 0.0444(9) 0.0614(12) 0.0079(8) -0.0286(9) -0.0282(8) Cl3 0.0602(12) 0.0794(14) 0.1126(19) -0.0443(13) -0.0237(12) 0.0039(10) Cl4 0.0966(15) 0.0557(11) 0.0726(14) -0.0098(10) -0.0210(12) -0.0069(11) S1 0.0405(8) 0.0419(9) 0.0438(10) -0.0016(7) -0.0136(7) -0.0112(7) P1 0.0369(8) 0.0292(8) 0.0415(10) -0.0050(7) -0.0096(7) -0.0094(7) P2 0.0262(8) 0.0270(8) 0.0484(10) -0.0017(7) -0.0123(7) -0.0055(6) N1 0.068(4) 0.038(3) 0.039(3) -0.010(2) -0.008(3) -0.024(3) N2 0.037(3) 0.031(3) 0.068(4) 0.011(3) -0.027(3) -0.009(2) C1 0.048(4) 0.046(4) 0.052(4) -0.006(3) -0.007(3) -0.023(3) C2 0.046(4) 0.028(3) 0.053(4) 0.000(3) -0.022(3) -0.004(3) C3 0.030(3) 0.029(3) 0.055(4) -0.011(3) -0.010(3) -0.003(2) C4 0.031(3) 0.034(3) 0.053(4) -0.009(3) -0.010(3) -0.007(3) C5 0.051(4) 0.049(4) 0.053(5) -0.016(3) -0.015(3) -0.007(3) C6 0.071(5) 0.052(4) 0.041(4) -0.007(3) -0.024(4) -0.015(4) C7 0.033(3) 0.054(4) 0.064(5) 0.004(4) -0.021(3) -0.007(3) C8 0.046(4) 0.051(4) 0.061(5) 0.006(4) -0.027(3) -0.008(3) C9 0.053(4) 0.070(5) 0.068(6) -0.002(4) -0.002(4) -0.017(4) C10 0.037(4) 0.085(5) 0.075(5) -0.004(4) -0.013(4) -0.020(4) C11 0.076(5) 0.029(3) 0.080(6) -0.001(3) -0.015(4) -0.008(3) C12 0.049(4) 0.054(4) 0.098(6) -0.012(4) -0.034(4) -0.009(3) C13 0.046(4) 0.067(5) 0.063(5) -0.017(4) 0.006(4) -0.020(3) C14 0.048(4) 0.034(3) 0.078(5) -0.014(3) -0.007(4) -0.001(3) C15 0.031(3) 0.057(4) 0.081(5) -0.003(4) -0.019(3) -0.013(3) C16 0.049(4) 0.085(5) 0.067(5) -0.011(4) 0.002(4) -0.032(4) C17 0.056(4) 0.052(4) 0.071(5) -0.008(4) -0.016(4) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 Cl1 2.1617(19) . ? Ni1 S1 2.1702(18) . ? Ni1 P1 2.2371(16) . ? Ni1 P2 2.2578(16) . ? Cl3 C17 1.746(7) . ? Cl4 C17 1.759(8) . ? S1 C6 1.812(7) . ? S1 C8 1.823(6) . ? P1 N1 1.652(5) . ? P1 C1 1.840(6) . ? P1 C2 1.846(6) . ? P2 N2 1.656(5) . ? P2 C4 1.823(6) . ? P2 C3 1.844(6) . ? N1 C5 1.445(8) . ? N1 H1A 0.8800 . ? N2 C7 1.442(8) . ? N2 H2A 0.8800 . ? C1 C10 1.524(9) . ? C1 C9 1.542(10) . ? C1 H1B 1.0000 . ? C2 C12 1.526(9) . ? C2 C11 1.546(8) . ? C2 H2B 1.0000 . ? C3 C13 1.518(8) . ? C3 C14 1.535(8) . ? C3 H3A 1.0000 . ? C4 C15 1.519(9) . ? C4 C16 1.540(9) . ? C4 H4A 1.0000 . ? C5 C6 1.501(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.505(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9900 . ? C17 H17B 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 Cl1 Ni1 S1 168.48(8) . . ? Cl1 Ni1 P1 88.08(7) . . ? S1 Ni1 P1 97.02(7) . . ? Cl1 Ni1 P2 87.64(7) . . ? S1 Ni1 P2 88.37(6) . . ? P1 Ni1 P2 172.23(7) . . ? C6 S1 C8 98.6(3) . . ? C6 S1 Ni1 118.2(2) . . ? C8 S1 Ni1 113.0(2) . . ? N1 P1 C1 101.4(3) . . ? N1 P1 C2 106.6(3) . . ? C1 P1 C2 107.5(3) . . ? N1 P1 Ni1 115.60(19) . . ? C1 P1 Ni1 109.9(2) . . ? C2 P1 Ni1 114.8(2) . . ? N2 P2 C4 104.3(3) . . ? N2 P2 C3 106.2(3) . . ? C4 P2 C3 104.8(3) . . ? N2 P2 Ni1 109.7(2) . . ? C4 P2 Ni1 114.99(19) . . ? C3 P2 Ni1 115.85(19) . . ? C5 N1 P1 124.3(4) . . ? C5 N1 H1A 117.9 . . ? P1 N1 H1A 117.9 . . ? C7 N2 P2 119.0(4) . . ? C7 N2 H2A 120.5 . . ? P2 N2 H2A 120.5 . . ? C10 C1 C9 110.5(5) . . ? C10 C1 P1 110.0(4) . . ? C9 C1 P1 114.2(5) . . ? C10 C1 H1B 107.3 . . ? C9 C1 H1B 107.3 . . ? P1 C1 H1B 107.3 . . ? C12 C2 C11 111.0(5) . . ? C12 C2 P1 108.5(4) . . ? C11 C2 P1 110.9(5) . . ? C12 C2 H2B 108.8 . . ? C11 C2 H2B 108.8 . . ? P1 C2 H2B 108.8 . . ? C13 C3 C14 111.3(5) . . ? C13 C3 P2 110.9(5) . . ? C14 C3 P2 111.6(4) . . ? C13 C3 H3A 107.6 . . ? C14 C3 H3A 107.6 . . ? P2 C3 H3A 107.6 . . ? C15 C4 C16 110.8(5) . . ? C15 C4 P2 113.4(4) . . ? C16 C4 P2 111.5(5) . . ? C15 C4 H4A 106.9 . . ? C16 C4 H4A 106.9 . . ? P2 C4 H4A 106.9 . . ? N1 C5 C6 112.5(5) . . ? N1 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N1 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C5 C6 S1 111.7(5) . . ? C5 C6 H6A 109.3 . . ? S1 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? S1 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 113.8(5) . . ? N2 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? N2 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 S1 110.2(5) . . ? C7 C8 H8A 109.6 . . ? S1 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? S1 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl3 C17 Cl4 110.0(4) . . ? Cl3 C17 H17A 109.7 . . ? Cl4 C17 H17A 109.7 . . ? Cl3 C17 H17B 109.7 . . ? Cl4 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.622 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.097 #=== END data_mjs025_0m_compound6a _database_code_depnum_ccdc_archive 'CCDC 867387' #TrackingRef '- All Cif Files Compiled.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C17 H40 Cl4 N2 P2 Pd S' _chemical_formula_weight 614.71 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' S S 0.1246 0.1234 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4324(4) _cell_length_b 11.4053(6) _cell_length_c 15.4027(8) _cell_angle_alpha 81.069(2) _cell_angle_beta 74.771(2) _cell_angle_gamma 68.760(2) _cell_volume 1329.25(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9701 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.51 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7801 _exptl_absorpt_correction_T_max 0.8804 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22016 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.56 _reflns_number_total 6060 _reflns_number_gt 5230 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0243P)^2^+0.6440P] 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 6060 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0244 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.391791(18) 0.354834(13) 0.278163(9) 0.01857(5) Uani 1 1 d . . . Cl1 Cl 0.24969(8) 0.30659(5) 0.42163(4) 0.03659(14) Uani 1 1 d . . . Cl2 Cl 0.08080(7) 0.90308(5) 0.13737(4) 0.03184(12) Uani 1 1 d . . . Cl3 Cl 0.88415(9) 0.69795(7) 0.94075(5) 0.04979(17) Uani 1 1 d . . . Cl4 Cl 0.61060(10) 0.86715(6) 1.06544(4) 0.04888(17) Uani 1 1 d . . . S1 S 0.49197(6) 0.41224(5) 0.13002(3) 0.02287(11) Uani 1 1 d . . . P1 P 0.21910(6) 0.56760(5) 0.29475(3) 0.01818(10) Uani 1 1 d . . . P2 P 0.57477(7) 0.14490(5) 0.27424(3) 0.02113(11) Uani 1 1 d . . . N1 N 0.3249(2) 0.65314(17) 0.22331(13) 0.0260(4) Uani 1 1 d . . . N2 N 0.6929(2) 0.10278(17) 0.17319(11) 0.0286(4) Uani 1 1 d . . . H2A H 0.7918 0.0393 0.1699 0.034 Uiso 1 1 calc R . . C1 C 0.1706(3) 0.62344(19) 0.40784(13) 0.0229(4) Uani 1 1 d . . . H1 H 0.0946 0.5794 0.4502 0.027 Uiso 1 1 calc R . . C2 C 0.0062(2) 0.61509(19) 0.26582(13) 0.0228(4) Uani 1 1 d . . . H2 H -0.0438 0.7092 0.2642 0.027 Uiso 1 1 calc R . . C3 C 0.7443(3) 0.1144(2) 0.33779(14) 0.0292(5) Uani 1 1 d . . . H3 H 0.8389 0.0340 0.3180 0.035 Uiso 1 1 calc R . . C4 C 0.4577(3) 0.03303(19) 0.32001(14) 0.0277(5) Uani 1 1 d . . . H4 H 0.3968 0.0515 0.3840 0.033 Uiso 1 1 calc R . . C5 C 0.5144(3) 0.6087(2) 0.20378(15) 0.0273(5) Uani 1 1 d . . . H5A H 0.5542 0.5589 0.2574 0.033 Uiso 1 1 calc R . . H5B H 0.5547 0.6823 0.1920 0.033 Uiso 1 1 calc R . . C6 C 0.5975(3) 0.5280(2) 0.12343(15) 0.0304(5) Uani 1 1 d . . . H6B H 0.7232 0.4843 0.1219 0.037 Uiso 1 1 calc R . . H6A H 0.5872 0.5825 0.0671 0.037 Uiso 1 1 calc R . . C7 C 0.6449(3) 0.1633(2) 0.08914(14) 0.0297(5) Uani 1 1 d . . . H7A H 0.5208 0.1751 0.0937 0.036 Uiso 1 1 calc R . . H7B H 0.7163 0.1076 0.0396 0.036 Uiso 1 1 calc R . . C8 C 0.6713(3) 0.2901(2) 0.06654(14) 0.0308(5) Uani 1 1 d . . . H8A H 0.6800 0.3129 0.0012 0.037 Uiso 1 1 calc R . . H8B H 0.7821 0.2841 0.0805 0.037 Uiso 1 1 calc R . . C9 C 0.0711(3) 0.7659(2) 0.40895(16) 0.0314(5) Uani 1 1 d . . . H9A H 0.0538 0.7938 0.4689 0.047 Uiso 1 1 calc R . . H9B H -0.0426 0.7843 0.3948 0.047 Uiso 1 1 calc R . . H9C H 0.1387 0.8107 0.3638 0.047 Uiso 1 1 calc R . . C10 C 0.3385(3) 0.5902(2) 0.44109(16) 0.0350(5) Uani 1 1 d . . . H10A H 0.4118 0.6367 0.4027 0.053 Uiso 1 1 calc R . . H10B H 0.4019 0.4995 0.4384 0.053 Uiso 1 1 calc R . . H10C H 0.3091 0.6133 0.5035 0.053 Uiso 1 1 calc R . . C11 C -0.1196(3) 0.5637(2) 0.33743(15) 0.0328(5) Uani 1 1 d . . . H11A H -0.2318 0.5898 0.3201 0.049 Uiso 1 1 calc R . . H11B H -0.1369 0.5969 0.3955 0.049 Uiso 1 1 calc R . . H11C H -0.0709 0.4715 0.3428 0.049 Uiso 1 1 calc R . . C12 C 0.0250(3) 0.5756(2) 0.17237(15) 0.0353(5) Uani 1 1 d . . . H12A H 0.0669 0.4834 0.1730 0.053 Uiso 1 1 calc R . . H12B H 0.1087 0.6084 0.1282 0.053 Uiso 1 1 calc R . . H12C H -0.0886 0.6098 0.1559 0.053 Uiso 1 1 calc R . . C13 C 0.8240(3) 0.2196(2) 0.31224(17) 0.0396(6) Uani 1 1 d . . . H13A H 0.7348 0.2998 0.3317 0.059 Uiso 1 1 calc R . . H13B H 0.8672 0.2262 0.2467 0.059 Uiso 1 1 calc R . . H13C H 0.9210 0.2002 0.3419 0.059 Uiso 1 1 calc R . . C14 C 0.6810(3) 0.0988(3) 0.43933(15) 0.0404(6) Uani 1 1 d . . . H14A H 0.7783 0.0816 0.4684 0.061 Uiso 1 1 calc R . . H14B H 0.6361 0.0283 0.4543 0.061 Uiso 1 1 calc R . . H14C H 0.5878 0.1763 0.4609 0.061 Uiso 1 1 calc R . . C15 C 0.5805(3) -0.1040(2) 0.31889(17) 0.0364(5) Uani 1 1 d . . . H15A H 0.5116 -0.1605 0.3376 0.055 Uiso 1 1 calc R . . H15B H 0.6568 -0.1183 0.3605 0.055 Uiso 1 1 calc R . . H15C H 0.6518 -0.1211 0.2578 0.055 Uiso 1 1 calc R . . C16 C 0.3186(3) 0.0546(2) 0.26626(18) 0.0400(6) Uani 1 1 d . . . H16A H 0.3758 0.0357 0.2034 0.060 Uiso 1 1 calc R . . H16B H 0.2413 0.1428 0.2685 0.060 Uiso 1 1 calc R . . H16C H 0.2500 -0.0008 0.2926 0.060 Uiso 1 1 calc R . . C17 C 0.8204(4) 0.8385(2) 0.99568(17) 0.0426(6) Uani 1 1 d . . . H17A H 0.9046 0.8308 1.0323 0.051 Uiso 1 1 calc R . . H17B H 0.8206 0.9101 0.9502 0.051 Uiso 1 1 calc R . . H1A H 0.274(3) 0.717(2) 0.1994(16) 0.033(7) Uiso 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 Pd1 0.01749(8) 0.01733(8) 0.01733(8) -0.00110(5) -0.00123(6) -0.00361(6) Cl1 0.0441(3) 0.0242(3) 0.0250(3) -0.0009(2) 0.0105(2) -0.0054(2) Cl2 0.0281(3) 0.0270(3) 0.0297(3) 0.0044(2) -0.0042(2) -0.0009(2) Cl3 0.0467(4) 0.0518(4) 0.0566(4) -0.0237(3) -0.0021(3) -0.0217(3) Cl4 0.0661(4) 0.0372(3) 0.0391(3) -0.0073(3) -0.0053(3) -0.0151(3) S1 0.0216(2) 0.0261(3) 0.0195(2) 0.00033(19) -0.00311(19) -0.0082(2) P1 0.0157(2) 0.0175(2) 0.0212(2) -0.00101(19) -0.00580(19) -0.00444(19) P2 0.0209(3) 0.0187(3) 0.0192(2) -0.00192(19) -0.0028(2) -0.0023(2) N1 0.0198(9) 0.0200(9) 0.0350(10) 0.0065(8) -0.0083(8) -0.0049(7) N2 0.0251(9) 0.0281(10) 0.0221(9) -0.0047(7) -0.0016(7) 0.0020(8) C1 0.0223(10) 0.0237(10) 0.0242(10) -0.0040(8) -0.0069(8) -0.0074(8) C2 0.0178(10) 0.0237(10) 0.0273(10) -0.0027(8) -0.0081(8) -0.0051(8) C3 0.0244(11) 0.0302(12) 0.0280(11) -0.0021(9) -0.0081(9) -0.0019(9) C4 0.0300(11) 0.0216(11) 0.0266(11) -0.0025(8) -0.0010(9) -0.0062(9) C5 0.0214(10) 0.0296(11) 0.0339(12) 0.0008(9) -0.0059(9) -0.0133(9) C6 0.0260(11) 0.0331(12) 0.0319(12) 0.0017(9) 0.0000(9) -0.0157(10) C7 0.0324(12) 0.0331(12) 0.0208(10) -0.0072(9) -0.0013(9) -0.0089(10) C8 0.0283(11) 0.0350(12) 0.0223(10) -0.0061(9) 0.0035(9) -0.0075(10) C9 0.0329(12) 0.0249(11) 0.0359(12) -0.0086(9) -0.0075(10) -0.0068(10) C10 0.0298(12) 0.0424(14) 0.0348(12) -0.0111(10) -0.0158(10) -0.0051(10) C11 0.0229(11) 0.0439(14) 0.0355(12) -0.0023(10) -0.0066(9) -0.0162(10) C12 0.0278(12) 0.0519(15) 0.0294(12) -0.0074(11) -0.0106(10) -0.0123(11) C13 0.0294(12) 0.0541(16) 0.0402(14) -0.0014(12) -0.0112(11) -0.0181(12) C14 0.0466(15) 0.0516(16) 0.0280(12) -0.0001(11) -0.0140(11) -0.0194(13) C15 0.0421(14) 0.0218(11) 0.0404(13) -0.0016(10) -0.0079(11) -0.0061(10) C16 0.0317(13) 0.0352(13) 0.0559(16) -0.0011(12) -0.0114(12) -0.0143(11) C17 0.0619(17) 0.0386(14) 0.0380(14) -0.0027(11) -0.0130(12) -0.0280(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 S1 2.2963(5) . ? Pd1 Cl1 2.3089(5) . ? Pd1 P2 2.3316(5) . ? Pd1 P1 2.3476(5) . ? Cl3 C17 1.770(2) . ? Cl4 C17 1.756(3) . ? S1 C8 1.818(2) . ? S1 C6 1.819(2) . ? P1 N1 1.6553(19) . ? P1 C2 1.8318(19) . ? P1 C1 1.841(2) . ? P2 N2 1.6481(17) . ? P2 C4 1.835(2) . ? P2 C3 1.842(2) . ? N1 C5 1.453(3) . ? N1 H1A 0.79(2) . ? N2 C7 1.453(3) . ? N2 H2A 0.8800 . ? C1 C10 1.530(3) . ? C1 C9 1.536(3) . ? C1 H1 1.0000 . ? C2 C11 1.523(3) . ? C2 C12 1.526(3) . ? C2 H2 1.0000 . ? C3 C14 1.519(3) . ? C3 C13 1.531(3) . ? C3 H3 1.0000 . ? C4 C15 1.531(3) . ? C4 C16 1.536(3) . ? C4 H4 1.0000 . ? C5 C6 1.516(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6B 0.9900 . ? C6 H6A 0.9900 . ? C7 C8 1.515(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9900 . ? C17 H17B 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 S1 Pd1 Cl1 171.19(2) . . ? S1 Pd1 P2 96.319(19) . . ? Cl1 Pd1 P2 88.241(19) . . ? S1 Pd1 P1 87.141(18) . . ? Cl1 Pd1 P1 88.984(19) . . ? P2 Pd1 P1 174.036(18) . . ? C8 S1 C6 99.90(10) . . ? C8 S1 Pd1 115.54(8) . . ? C6 S1 Pd1 110.01(7) . . ? N1 P1 C2 105.05(9) . . ? N1 P1 C1 107.53(10) . . ? C2 P1 C1 104.83(9) . . ? N1 P1 Pd1 107.39(7) . . ? C2 P1 Pd1 115.54(7) . . ? C1 P1 Pd1 115.76(7) . . ? N2 P2 C4 107.56(10) . . ? N2 P2 C3 101.87(10) . . ? C4 P2 C3 107.85(10) . . ? N2 P2 Pd1 114.36(7) . . ? C4 P2 Pd1 113.17(7) . . ? C3 P2 Pd1 111.26(7) . . ? C5 N1 P1 119.15(15) . . ? C5 N1 H1A 119.8(18) . . ? P1 N1 H1A 121.0(18) . . ? C7 N2 P2 124.50(14) . . ? C7 N2 H2A 117.8 . . ? P2 N2 H2A 117.8 . . ? C10 C1 C9 110.52(17) . . ? C10 C1 P1 110.70(14) . . ? C9 C1 P1 111.34(14) . . ? C10 C1 H1 108.1 . . ? C9 C1 H1 108.1 . . ? P1 C1 H1 108.1 . . ? C11 C2 C12 111.50(18) . . ? C11 C2 P1 111.12(14) . . ? C12 C2 P1 111.13(14) . . ? C11 C2 H2 107.6 . . ? C12 C2 H2 107.6 . . ? P1 C2 H2 107.6 . . ? C14 C3 C13 110.9(2) . . ? C14 C3 P2 114.12(16) . . ? C13 C3 P2 109.13(15) . . ? C14 C3 H3 107.5 . . ? C13 C3 H3 107.5 . . ? P2 C3 H3 107.5 . . ? C15 C4 C16 111.17(19) . . ? C15 C4 P2 112.36(15) . . ? C16 C4 P2 108.67(15) . . ? C15 C4 H4 108.2 . . ? C16 C4 H4 108.2 . . ? P2 C4 H4 108.2 . . ? N1 C5 C6 113.07(18) . . ? N1 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? N1 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C5 C6 S1 110.66(15) . . ? C5 C6 H6B 109.5 . . ? S1 C6 H6B 109.5 . . ? C5 C6 H6A 109.5 . . ? S1 C6 H6A 109.5 . . ? H6B C6 H6A 108.1 . . ? N2 C7 C8 112.31(18) . . ? N2 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N2 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C7 C8 S1 111.24(15) . . ? C7 C8 H8A 109.4 . . ? S1 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? S1 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl4 C17 Cl3 109.90(13) . . ? Cl4 C17 H17A 109.7 . . ? Cl3 C17 H17A 109.7 . . ? Cl4 C17 H17B 109.7 . . ? Cl3 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.616 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.066 #=== END data_mjs058_0ma_compound8a _database_code_depnum_ccdc_archive 'CCDC 867388' #TrackingRef '- All Cif Files Compiled.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C17 H42 Cl N3 P2 Pd' _chemical_formula_weight 492.33 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.040(3) _cell_length_b 8.6683(9) _cell_length_c 27.228(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.473(9) _cell_angle_gamma 90.00 _cell_volume 4808.2(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3911 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 24.35 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8619 _exptl_absorpt_correction_T_max 0.9137 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21062 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5482 _reflns_number_gt 4002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0301P)^2^+5.2867P] 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 5482 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.122785(12) 0.73469(3) 0.122310(9) 0.02285(8) Uani 1 1 d . . . Cl1 Cl 0.86768(4) 0.63633(11) 0.19802(3) 0.0360(2) Uani 1 1 d . . . P1 P 0.22984(4) 0.80212(10) 0.12390(3) 0.0242(2) Uani 1 1 d . . . P2 P 0.01438(4) 0.66493(10) 0.11466(3) 0.0236(2) Uani 1 1 d . . . N1 N 0.27435(14) 0.8352(3) 0.18246(10) 0.0324(7) Uani 1 1 d . . . H1A H 0.3141 0.8741 0.1872 0.039 Uiso 1 1 calc R . . N2 N -0.01606(15) 0.7734(3) 0.15322(11) 0.0356(7) Uani 1 1 d . . . H2A H -0.0478 0.7383 0.1660 0.043 Uiso 1 1 calc R . . N3 N 0.12659(14) 0.8349(3) 0.19743(10) 0.0296(7) Uani 1 1 d . . . H3B H 0.1195 0.7491 0.2158 0.036 Uiso 1 1 calc R . . C1 C 0.23566(17) 0.9830(4) 0.09017(12) 0.0303(8) Uani 1 1 d . . . H1B H 0.2826 1.0164 0.0998 0.036 Uiso 1 1 calc R . . C2 C 0.27842(17) 0.6596(4) 0.09851(13) 0.0308(8) Uani 1 1 d . . . H2B H 0.2547 0.6365 0.0626 0.037 Uiso 1 1 calc R . . C3 C -0.04256(16) 0.6875(4) 0.05106(12) 0.0290(8) Uani 1 1 d . . . H3A H -0.0296 0.6104 0.0280 0.035 Uiso 1 1 calc R . . C4 C 0.00079(17) 0.4676(4) 0.13383(13) 0.0291(8) Uani 1 1 d . . . H4A H -0.0459 0.4604 0.1360 0.035 Uiso 1 1 calc R . . C5 C 0.24828(18) 0.8004(4) 0.22616(12) 0.0361(9) Uani 1 1 d . . . H5A H 0.2834 0.8174 0.2575 0.043 Uiso 1 1 calc R . . H5B H 0.2361 0.6899 0.2250 0.043 Uiso 1 1 calc R . . C6 C 0.18926(18) 0.8956(4) 0.22899(13) 0.0384(9) Uani 1 1 d . . . H6A H 0.1865 0.9001 0.2647 0.046 Uiso 1 1 calc R . . H6B H 0.1955 1.0022 0.2180 0.046 Uiso 1 1 calc R . . C7 C 0.0100(2) 0.9259(5) 0.16566(19) 0.0617(13) Uani 1 1 d . . . H7A H -0.0228 0.9859 0.1781 0.074 Uiso 1 1 calc R . . H7B H 0.0143 0.9755 0.1339 0.074 Uiso 1 1 calc R . . C8 C 0.0728(2) 0.9406(4) 0.20283(15) 0.0470(11) Uani 1 1 d . . . H8A H 0.0652 0.9244 0.2369 0.056 Uiso 1 1 calc R . . H8B H 0.0883 1.0480 0.2016 0.056 Uiso 1 1 calc R . . C9 C 0.19510(19) 1.1094(4) 0.10742(14) 0.0416(10) Uani 1 1 d . . . H9A H 0.1988 1.2054 0.0893 0.062 Uiso 1 1 calc R . . H9B H 0.2116 1.1260 0.1440 0.062 Uiso 1 1 calc R . . H9C H 0.1490 1.0775 0.1000 0.062 Uiso 1 1 calc R . . C10 C 0.2157(2) 0.9656(4) 0.03310(14) 0.0442(10) Uani 1 1 d . . . H10A H 0.2200 1.0653 0.0172 0.066 Uiso 1 1 calc R . . H10B H 0.1700 0.9309 0.0225 0.066 Uiso 1 1 calc R . . H10C H 0.2442 0.8896 0.0226 0.066 Uiso 1 1 calc R . . C11 C 0.34725(18) 0.7165(5) 0.09901(16) 0.0449(10) Uani 1 1 d . . . H11A H 0.3705 0.6366 0.0849 0.067 Uiso 1 1 calc R . . H11B H 0.3714 0.7389 0.1340 0.067 Uiso 1 1 calc R . . H11C H 0.3441 0.8104 0.0785 0.067 Uiso 1 1 calc R . . C12 C 0.2827(2) 0.5110(4) 0.12923(16) 0.0494(11) Uani 1 1 d . . . H12A H 0.3083 0.4342 0.1159 0.074 Uiso 1 1 calc R . . H12B H 0.2384 0.4711 0.1266 0.074 Uiso 1 1 calc R . . H12C H 0.3042 0.5322 0.1649 0.074 Uiso 1 1 calc R . . C13 C -0.03436(19) 0.8482(4) 0.03017(14) 0.0443(10) Uani 1 1 d . . . H13A H -0.0643 0.8596 -0.0035 0.066 Uiso 1 1 calc R . . H13B H 0.0110 0.8613 0.0277 0.066 Uiso 1 1 calc R . . H13C H -0.0445 0.9267 0.0530 0.066 Uiso 1 1 calc R . . C14 C -0.11386(17) 0.6561(5) 0.05099(14) 0.0404(9) Uani 1 1 d . . . H14A H -0.1417 0.6695 0.0166 0.061 Uiso 1 1 calc R . . H14B H -0.1276 0.7285 0.0740 0.061 Uiso 1 1 calc R . . H14C H -0.1181 0.5502 0.0624 0.061 Uiso 1 1 calc R . . C15 C 0.01057(19) 0.3474(4) 0.09506(14) 0.0406(9) Uani 1 1 d . . . H15A H 0.0026 0.2440 0.1068 0.061 Uiso 1 1 calc R . . H15B H 0.0556 0.3537 0.0913 0.061 Uiso 1 1 calc R . . H15C H -0.0203 0.3677 0.0623 0.061 Uiso 1 1 calc R . . C16 C 0.0444(2) 0.4339(5) 0.18668(14) 0.0531(12) Uani 1 1 d . . . H16A H 0.0365 0.3283 0.1966 0.080 Uiso 1 1 calc R . . H16B H 0.0340 0.5067 0.2111 0.080 Uiso 1 1 calc R . . H16C H 0.0906 0.4452 0.1863 0.080 Uiso 1 1 calc R . . C17 C 0.11805(18) 0.6267(5) 0.05391(13) 0.0396(10) Uani 1 1 d . . . H17A H 0.1605 0.6362 0.0454 0.059 Uiso 1 1 calc R . . H17B H 0.0838 0.6752 0.0273 0.059 Uiso 1 1 calc R . . H17C H 0.1076 0.5173 0.0566 0.059 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 0.02465(14) 0.02417(15) 0.02001(13) -0.00401(10) 0.00608(9) -0.00699(11) Cl1 0.0342(5) 0.0460(6) 0.0293(5) -0.0071(4) 0.0108(4) -0.0145(4) P1 0.0231(5) 0.0253(5) 0.0223(4) 0.0017(3) 0.0024(3) -0.0064(4) P2 0.0253(5) 0.0216(5) 0.0253(4) -0.0006(3) 0.0091(4) -0.0049(4) N1 0.0257(16) 0.0401(18) 0.0269(15) 0.0025(13) -0.0020(12) -0.0110(13) N2 0.0451(19) 0.0280(17) 0.0419(18) -0.0083(13) 0.0260(15) -0.0115(14) N3 0.0397(18) 0.0242(16) 0.0233(14) -0.0039(12) 0.0048(13) -0.0041(13) C1 0.029(2) 0.032(2) 0.0280(19) 0.0091(15) 0.0033(15) -0.0046(15) C2 0.029(2) 0.030(2) 0.0321(19) 0.0027(15) 0.0058(15) -0.0026(15) C3 0.0271(19) 0.030(2) 0.0296(18) 0.0039(14) 0.0058(15) 0.0029(15) C4 0.030(2) 0.0227(19) 0.035(2) 0.0025(14) 0.0087(16) -0.0037(14) C5 0.037(2) 0.043(2) 0.0219(17) 0.0018(15) -0.0049(15) -0.0083(17) C6 0.050(3) 0.040(2) 0.0230(18) -0.0101(16) 0.0041(17) -0.0104(18) C7 0.062(3) 0.042(3) 0.082(4) -0.021(2) 0.020(3) 0.002(2) C8 0.055(3) 0.030(2) 0.049(2) -0.0159(18) 0.001(2) 0.0092(19) C9 0.052(3) 0.027(2) 0.043(2) 0.0033(17) 0.008(2) -0.0029(18) C10 0.053(3) 0.041(2) 0.038(2) 0.0146(18) 0.009(2) 0.0049(19) C11 0.032(2) 0.048(3) 0.056(3) 0.0048(19) 0.0142(19) 0.0013(18) C12 0.061(3) 0.030(2) 0.061(3) 0.0096(19) 0.024(2) 0.002(2) C13 0.049(3) 0.042(2) 0.038(2) 0.0136(18) 0.0034(19) -0.0053(19) C14 0.027(2) 0.047(2) 0.045(2) 0.0056(18) 0.0046(17) 0.0005(17) C15 0.049(3) 0.025(2) 0.047(2) -0.0019(16) 0.0097(19) -0.0038(17) C16 0.072(3) 0.039(3) 0.037(2) 0.0108(18) -0.006(2) -0.011(2) C17 0.031(2) 0.058(3) 0.033(2) -0.0214(18) 0.0127(17) -0.0166(18) _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 C17 2.065(3) . ? Pd1 N3 2.205(3) . ? Pd1 P1 2.3168(9) . ? Pd1 P2 2.3181(9) . ? P1 N1 1.660(3) . ? P1 C1 1.836(3) . ? P1 C2 1.844(4) . ? P2 N2 1.653(3) . ? P2 C4 1.831(3) . ? P2 C3 1.853(3) . ? N1 C5 1.461(4) . ? N1 H1A 0.8800 . ? N2 C7 1.439(5) . ? N2 H2A 0.8800 . ? N3 C6 1.479(4) . ? N3 C8 1.491(5) . ? N3 H3B 0.9300 . ? C1 C10 1.513(5) . ? C1 C9 1.533(5) . ? C1 H1B 1.0000 . ? C2 C12 1.527(5) . ? C2 C11 1.527(5) . ? C2 H2B 1.0000 . ? C3 C14 1.524(5) . ? C3 C13 1.531(5) . ? C3 H3A 1.0000 . ? C4 C16 1.529(5) . ? C4 C15 1.533(5) . ? C4 H4A 1.0000 . ? C5 C6 1.509(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.455(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 C17 Pd1 N3 176.17(13) . . ? C17 Pd1 P1 87.64(10) . . ? N3 Pd1 P1 94.21(8) . . ? C17 Pd1 P2 88.63(10) . . ? N3 Pd1 P2 89.59(8) . . ? P1 Pd1 P2 176.01(3) . . ? N1 P1 C1 103.93(15) . . ? N1 P1 C2 104.09(15) . . ? C1 P1 C2 105.76(16) . . ? N1 P1 Pd1 111.97(11) . . ? C1 P1 Pd1 113.08(12) . . ? C2 P1 Pd1 116.83(11) . . ? N2 P2 C4 103.73(15) . . ? N2 P2 C3 105.71(16) . . ? C4 P2 C3 104.74(15) . . ? N2 P2 Pd1 108.87(11) . . ? C4 P2 Pd1 115.99(12) . . ? C3 P2 Pd1 116.62(11) . . ? C5 N1 P1 120.7(2) . . ? C5 N1 H1A 119.7 . . ? P1 N1 H1A 119.7 . . ? C7 N2 P2 119.1(3) . . ? C7 N2 H2A 120.4 . . ? P2 N2 H2A 120.4 . . ? C6 N3 C8 108.2(3) . . ? C6 N3 Pd1 120.0(2) . . ? C8 N3 Pd1 118.7(2) . . ? C6 N3 H3B 102.2 . . ? C8 N3 H3B 102.2 . . ? Pd1 N3 H3B 102.2 . . ? C10 C1 C9 110.7(3) . . ? C10 C1 P1 113.1(2) . . ? C9 C1 P1 110.2(2) . . ? C10 C1 H1B 107.5 . . ? C9 C1 H1B 107.5 . . ? P1 C1 H1B 107.5 . . ? C12 C2 C11 110.0(3) . . ? C12 C2 P1 108.8(3) . . ? C11 C2 P1 113.2(3) . . ? C12 C2 H2B 108.2 . . ? C11 C2 H2B 108.2 . . ? P1 C2 H2B 108.2 . . ? C14 C3 C13 111.4(3) . . ? C14 C3 P2 112.9(2) . . ? C13 C3 P2 109.7(2) . . ? C14 C3 H3A 107.6 . . ? C13 C3 H3A 107.6 . . ? P2 C3 H3A 107.6 . . ? C16 C4 C15 111.5(3) . . ? C16 C4 P2 110.3(2) . . ? C15 C4 P2 112.4(2) . . ? C16 C4 H4A 107.5 . . ? C15 C4 H4A 107.5 . . ? P2 C4 H4A 107.5 . . ? N1 C5 C6 114.2(3) . . ? N1 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? N1 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? N3 C6 C5 113.7(3) . . ? N3 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? N3 C6 H6B 108.8 . . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? N2 C7 C8 118.1(4) . . ? N2 C7 H7A 107.8 . . ? C8 C7 H7A 107.8 . . ? N2 C7 H7B 107.8 . . ? C8 C7 H7B 107.8 . . ? H7A C7 H7B 107.1 . . ? C7 C8 N3 117.2(3) . . ? C7 C8 H8A 108.0 . . ? N3 C8 H8A 108.0 . . ? C7 C8 H8B 108.0 . . ? N3 C8 H8B 108.0 . . ? H8A C8 H8B 107.2 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Pd1 C17 H17A 109.5 . . ? Pd1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Pd1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.283 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.098 #=== END data_mjs057_0m_compound9a _database_code_depnum_ccdc_archive 'CCDC 867389' #TrackingRef '- All Cif Files Compiled.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C18 H43 Cl3 N2 P2 Pd S' _chemical_formula_weight 594.29 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' S S 0.1246 0.1234 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4214(15) _cell_length_b 11.430(2) _cell_length_c 15.337(3) _cell_angle_alpha 81.066(8) _cell_angle_beta 74.944(8) _cell_angle_gamma 69.118(8) _cell_volume 1328.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8019 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.55 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6629 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 21331 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.80 _reflns_number_total 6094 _reflns_number_gt 5046 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0325P)^2^+0.6153P] 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 6094 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.61078(2) 0.644546(17) 0.721900(12) 0.01667(6) Uani 1 1 d . . . Cl1 Cl 0.92548(8) 0.09629(6) 0.85660(4) 0.02786(15) Uani 1 1 d . . . Cl2 Cl 0.88307(11) 0.70244(8) 0.93649(6) 0.0444(2) Uani 1 1 d . . . Cl3 Cl 0.61983(12) 0.86877(7) 1.06440(5) 0.0443(2) Uani 1 1 d . . . S1 S 0.50520(8) 0.58369(6) 0.87585(4) 0.02000(13) Uani 1 1 d . . . P1 P 0.42870(8) 0.85080(6) 0.72607(4) 0.01828(14) Uani 1 1 d . . . P2 P 0.77930(8) 0.43491(6) 0.70547(4) 0.01608(13) Uani 1 1 d . . . N1 N 0.3099(3) 0.8893(2) 0.82776(14) 0.0256(5) Uani 1 1 d . . . H1A H 0.2097 0.9507 0.8309 0.031 Uiso 1 1 calc R . . N2 N 0.6730(3) 0.3489(2) 0.77679(14) 0.0225(5) Uani 1 1 d . . . H2A H 0.7312 0.2770 0.8018 0.027 Uiso 1 1 calc R . . C1 C 0.2567(3) 0.8845(3) 0.66304(17) 0.0252(6) Uani 1 1 d . . . H1B H 0.1647 0.9651 0.6833 0.030 Uiso 1 1 calc R . . C2 C 0.5371(3) 0.9691(2) 0.68216(18) 0.0246(6) Uani 1 1 d . . . H2B H 0.5989 0.9535 0.6178 0.029 Uiso 1 1 calc R . . C3 C 0.8293(3) 0.3756(2) 0.59312(17) 0.0221(5) Uani 1 1 d . . . H3A H 0.9026 0.4209 0.5497 0.027 Uiso 1 1 calc R . . C4 C 0.9912(3) 0.3840(2) 0.73600(17) 0.0210(5) Uani 1 1 d . . . H4A H 1.0384 0.2903 0.7379 0.025 Uiso 1 1 calc R . . C5 C 0.3569(4) 0.8303(2) 0.91290(17) 0.0251(6) Uani 1 1 d . . . H5A H 0.2871 0.8872 0.9618 0.030 Uiso 1 1 calc R . . H5B H 0.4814 0.8176 0.9082 0.030 Uiso 1 1 calc R . . C6 C 0.3269(3) 0.7054(2) 0.93762(17) 0.0265(6) Uani 1 1 d . . . H6A H 0.2163 0.7111 0.9231 0.032 Uiso 1 1 calc R . . H6B H 0.3170 0.6842 1.0035 0.032 Uiso 1 1 calc R . . C7 C 0.4829(3) 0.3928(2) 0.79810(18) 0.0222(5) Uani 1 1 d . . . H7A H 0.4425 0.3194 0.8071 0.027 Uiso 1 1 calc R . . H7B H 0.4410 0.4465 0.7460 0.027 Uiso 1 1 calc R . . C8 C 0.4034(3) 0.4660(2) 0.88162(18) 0.0262(6) Uani 1 1 d . . . H8A H 0.4204 0.4083 0.9362 0.031 Uiso 1 1 calc R . . H8B H 0.2767 0.5074 0.8862 0.031 Uiso 1 1 calc R . . C9 C 0.1736(4) 0.7817(3) 0.6886(2) 0.0365(7) Uani 1 1 d . . . H9A H 0.0817 0.7993 0.6554 0.055 Uiso 1 1 calc R . . H9B H 0.1230 0.7793 0.7538 0.055 Uiso 1 1 calc R . . H9C H 0.2625 0.7004 0.6731 0.055 Uiso 1 1 calc R . . C10 C 0.3174(4) 0.9005(3) 0.56087(18) 0.0364(7) Uani 1 1 d . . . H10A H 0.2187 0.9184 0.5325 0.055 Uiso 1 1 calc R . . H10B H 0.4087 0.8232 0.5389 0.055 Uiso 1 1 calc R . . H10C H 0.3637 0.9704 0.5454 0.055 Uiso 1 1 calc R . . C11 C 0.4098(4) 1.1034(2) 0.6850(2) 0.0329(7) Uani 1 1 d . . . H11A H 0.4742 1.1621 0.6609 0.049 Uiso 1 1 calc R . . H11B H 0.3478 1.1205 0.7477 0.049 Uiso 1 1 calc R . . H11C H 0.3257 1.1137 0.6483 0.049 Uiso 1 1 calc R . . C12 C 0.6741(4) 0.9501(3) 0.7373(2) 0.0359(7) Uani 1 1 d . . . H12A H 0.7339 1.0120 0.7149 0.054 Uiso 1 1 calc R . . H12B H 0.7591 0.8653 0.7308 0.054 Uiso 1 1 calc R . . H12C H 0.6165 0.9610 0.8012 0.054 Uiso 1 1 calc R . . C13 C 0.6608(4) 0.4047(3) 0.5611(2) 0.0358(7) Uani 1 1 d . . . H13A H 0.6885 0.3732 0.5012 0.054 Uiso 1 1 calc R . . H13B H 0.6013 0.4957 0.5576 0.054 Uiso 1 1 calc R . . H13C H 0.5848 0.3639 0.6040 0.054 Uiso 1 1 calc R . . C14 C 0.9310(4) 0.2356(2) 0.59228(19) 0.0295(6) Uani 1 1 d . . . H14A H 0.9549 0.2083 0.5313 0.044 Uiso 1 1 calc R . . H14B H 0.8623 0.1892 0.6352 0.044 Uiso 1 1 calc R . . H14C H 1.0413 0.2190 0.6098 0.044 Uiso 1 1 calc R . . C15 C 0.9739(4) 0.4234(3) 0.82922(18) 0.0315(6) Uani 1 1 d . . . H15A H 1.0890 0.3947 0.8437 0.047 Uiso 1 1 calc R . . H15B H 0.8968 0.3857 0.8744 0.047 Uiso 1 1 calc R . . H15C H 0.9247 0.5150 0.8296 0.047 Uiso 1 1 calc R . . C16 C 1.1209(3) 0.4344(3) 0.66514(19) 0.0304(6) Uani 1 1 d . . . H16A H 1.2330 0.4056 0.6831 0.046 Uiso 1 1 calc R . . H16B H 1.0759 0.5263 0.6607 0.046 Uiso 1 1 calc R . . H16C H 1.1369 0.4035 0.6063 0.046 Uiso 1 1 calc R . . C17 C 0.7411(4) 0.6894(3) 0.59388(18) 0.0345(7) Uani 1 1 d . . . H17A H 0.6603 0.7185 0.5531 0.052 Uiso 1 1 calc R . . H17B H 0.8377 0.6149 0.5711 0.052 Uiso 1 1 calc R . . H17C H 0.7868 0.7561 0.5970 0.052 Uiso 1 1 calc R . . C18 C 0.8279(4) 0.8400(3) 0.9925(2) 0.0383(7) Uani 1 1 d . . . H18A H 0.9150 0.8297 1.0283 0.046 Uiso 1 1 calc R . . H18B H 0.8283 0.9121 0.9474 0.046 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 0.01601(10) 0.01642(10) 0.01573(10) -0.00144(7) -0.00214(7) -0.00400(7) Cl1 0.0248(3) 0.0227(3) 0.0287(3) 0.0024(3) -0.0048(3) -0.0016(3) Cl2 0.0402(4) 0.0484(5) 0.0509(5) -0.0222(4) -0.0035(4) -0.0193(4) Cl3 0.0595(5) 0.0342(4) 0.0376(4) -0.0084(3) -0.0066(4) -0.0140(4) S1 0.0187(3) 0.0228(3) 0.0183(3) -0.0012(2) -0.0033(2) -0.0074(3) P1 0.0181(3) 0.0170(3) 0.0178(3) -0.0018(2) -0.0037(2) -0.0035(3) P2 0.0140(3) 0.0165(3) 0.0184(3) -0.0021(2) -0.0053(2) -0.0042(2) N1 0.0232(11) 0.0236(12) 0.0210(11) -0.0046(9) -0.0039(9) 0.0034(9) N2 0.0164(10) 0.0209(11) 0.0284(12) 0.0033(9) -0.0057(9) -0.0053(9) C1 0.0219(13) 0.0287(14) 0.0237(13) -0.0029(11) -0.0078(11) -0.0045(11) C2 0.0272(14) 0.0186(13) 0.0260(13) -0.0009(10) -0.0042(11) -0.0067(11) C3 0.0209(13) 0.0240(13) 0.0224(13) -0.0050(10) -0.0055(10) -0.0066(11) C4 0.0172(12) 0.0219(13) 0.0255(13) -0.0035(10) -0.0084(10) -0.0050(10) C5 0.0270(14) 0.0284(14) 0.0183(12) -0.0067(11) -0.0035(10) -0.0064(12) C6 0.0247(13) 0.0292(15) 0.0202(13) -0.0050(11) 0.0015(10) -0.0056(12) C7 0.0172(12) 0.0221(13) 0.0301(14) 0.0001(11) -0.0060(10) -0.0102(10) C8 0.0243(14) 0.0283(15) 0.0278(14) 0.0011(11) -0.0029(11) -0.0144(12) C9 0.0287(15) 0.0506(19) 0.0367(17) -0.0015(14) -0.0112(13) -0.0189(14) C10 0.0437(18) 0.0493(19) 0.0222(14) 0.0022(13) -0.0142(13) -0.0199(15) C11 0.0380(16) 0.0208(14) 0.0399(17) -0.0008(12) -0.0111(13) -0.0085(13) C12 0.0258(15) 0.0335(16) 0.0520(19) -0.0035(14) -0.0104(14) -0.0125(13) C13 0.0308(15) 0.0463(18) 0.0330(16) -0.0147(14) -0.0180(13) -0.0036(14) C14 0.0329(15) 0.0246(14) 0.0318(15) -0.0108(12) -0.0083(12) -0.0058(12) C15 0.0265(14) 0.0445(18) 0.0284(15) -0.0086(13) -0.0116(12) -0.0112(13) C16 0.0223(14) 0.0436(17) 0.0308(15) -0.0024(13) -0.0079(11) -0.0161(13) C17 0.0402(17) 0.0250(15) 0.0244(14) 0.0000(11) 0.0078(12) -0.0053(13) C18 0.055(2) 0.0346(17) 0.0368(17) -0.0033(13) -0.0121(15) -0.0269(16) _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 C17 2.071(3) . ? Pd1 P1 2.3091(8) . ? Pd1 P2 2.3230(7) . ? Pd1 S1 2.3852(7) . ? Cl2 C18 1.766(3) . ? Cl3 C18 1.759(3) . ? S1 C6 1.808(3) . ? S1 C8 1.815(3) . ? P1 N1 1.648(2) . ? P1 C2 1.842(3) . ? P1 C1 1.842(3) . ? P2 N2 1.657(2) . ? P2 C4 1.831(2) . ? P2 C3 1.841(2) . ? N1 C5 1.457(3) . ? N1 H1A 0.8800 . ? N2 C7 1.459(3) . ? N2 H2A 0.8800 . ? C1 C10 1.520(4) . ? C1 C9 1.525(4) . ? C1 H1B 1.0000 . ? C2 C11 1.526(4) . ? C2 C12 1.537(4) . ? C2 H2B 1.0000 . ? C3 C14 1.523(4) . ? C3 C13 1.529(4) . ? C3 H3A 1.0000 . ? C4 C15 1.520(3) . ? C4 C16 1.531(4) . ? C4 H4A 1.0000 . ? C5 C6 1.511(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.509(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 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 C17 Pd1 P1 88.45(8) . . ? C17 Pd1 P2 89.29(8) . . ? P1 Pd1 P2 173.63(2) . . ? C17 Pd1 S1 170.71(9) . . ? P1 Pd1 S1 96.15(2) . . ? P2 Pd1 S1 86.95(2) . . ? C6 S1 C8 101.05(13) . . ? C6 S1 Pd1 114.73(9) . . ? C8 S1 Pd1 110.22(9) . . ? N1 P1 C2 106.86(12) . . ? N1 P1 C1 100.67(12) . . ? C2 P1 C1 106.11(13) . . ? N1 P1 Pd1 113.68(8) . . ? C2 P1 Pd1 115.38(9) . . ? C1 P1 Pd1 112.84(9) . . ? N2 P2 C4 103.82(11) . . ? N2 P2 C3 106.35(12) . . ? C4 P2 C3 104.11(11) . . ? N2 P2 Pd1 107.68(8) . . ? C4 P2 Pd1 116.44(9) . . ? C3 P2 Pd1 117.25(8) . . ? C5 N1 P1 125.48(17) . . ? C5 N1 H1A 117.3 . . ? P1 N1 H1A 117.3 . . ? C7 N2 P2 119.85(17) . . ? C7 N2 H2A 120.1 . . ? P2 N2 H2A 120.1 . . ? C10 C1 C9 110.5(2) . . ? C10 C1 P1 114.50(19) . . ? C9 C1 P1 109.13(19) . . ? C10 C1 H1B 107.5 . . ? C9 C1 H1B 107.5 . . ? P1 C1 H1B 107.5 . . ? C11 C2 C12 111.0(2) . . ? C11 C2 P1 112.96(19) . . ? C12 C2 P1 108.00(19) . . ? C11 C2 H2B 108.3 . . ? C12 C2 H2B 108.3 . . ? P1 C2 H2B 108.3 . . ? C14 C3 C13 110.5(2) . . ? C14 C3 P2 112.33(18) . . ? C13 C3 P2 109.93(18) . . ? C14 C3 H3A 108.0 . . ? C13 C3 H3A 108.0 . . ? P2 C3 H3A 108.0 . . ? C15 C4 C16 110.4(2) . . ? C15 C4 P2 111.34(17) . . ? C16 C4 P2 111.23(18) . . ? C15 C4 H4A 107.9 . . ? C16 C4 H4A 107.9 . . ? P2 C4 H4A 107.9 . . ? N1 C5 C6 112.5(2) . . ? N1 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N1 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C5 C6 S1 110.26(18) . . ? C5 C6 H6A 109.6 . . ? S1 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? S1 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N2 C7 C8 113.1(2) . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7 C8 S1 109.87(18) . . ? C7 C8 H8A 109.7 . . ? S1 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? S1 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Pd1 C17 H17A 109.5 . . ? Pd1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Pd1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Cl3 C18 Cl2 109.37(16) . . ? Cl3 C18 H18A 109.8 . . ? Cl2 C18 H18A 109.8 . . ? Cl3 C18 H18B 109.8 . . ? Cl2 C18 H18B 109.8 . . ? H18A C18 H18B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.638 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.086 #=== END data_mjs072_0m_compound14b _database_code_depnum_ccdc_archive 'CCDC 867390' #TrackingRef '- All Cif Files Compiled.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C16 H39 F6 N3 P3 Pd' _chemical_formula_weight 586.81 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' F F 0.0171 0.0103 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5371(4) _cell_length_b 8.8800(4) _cell_length_c 27.0360(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.029(2) _cell_angle_gamma 90.00 _cell_volume 2526.21(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8054 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.41 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 0.976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6649 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 17068 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4447 _reflns_number_gt 3948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0482P)^2^+7.0908P] 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 4447 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.66200(2) 0.20450(3) 0.891096(10) 0.02349(11) Uani 1 1 d . . . P1 P 0.53393(9) 0.14521(12) 0.82308(3) 0.0242(2) Uani 1 1 d . . . P2 P 0.74184(9) 0.28626(11) 0.96683(4) 0.0281(2) Uani 1 1 d . . . P3 P 0.02600(13) 0.77205(14) 0.85947(4) 0.0391(3) Uani 1 1 d . . . F1 F 0.0462(3) 0.6729(5) 0.90696(13) 0.0851(13) Uani 1 1 d . . . F2 F 0.1181(4) 0.8958(5) 0.87880(14) 0.1126(18) Uani 1 1 d . . . F3 F 0.1248(7) 0.6907(6) 0.8317(3) 0.182(4) Uani 1 1 d . . . F4 F -0.0032(5) 0.8755(5) 0.81277(13) 0.1068(16) Uani 1 1 d . . . F5 F -0.0737(5) 0.6503(5) 0.83936(13) 0.1206(19) Uani 1 1 d . . . F6 F -0.0868(5) 0.8512(5) 0.8846(2) 0.133(2) Uani 1 1 d . . . N1 N 0.6158(3) 0.1480(5) 0.77239(12) 0.0396(9) Uani 1 1 d . . . H1A H 0.5754 0.1721 0.7442 0.048 Uiso 1 1 calc R . . N2 N 0.9003(3) 0.2944(4) 0.97035(15) 0.0406(9) Uani 1 1 d . . . H2A H 0.9394 0.3498 0.9935 0.049 Uiso 1 1 calc R . . N3 N 0.8418(3) 0.1803(4) 0.85651(14) 0.0356(8) Uani 1 1 d . . . H3B H 0.8607 0.0781 0.8588 0.043 Uiso 1 1 calc R . . C1 C 0.4058(4) 0.2791(5) 0.80788(15) 0.0323(9) Uani 1 1 d . . . H1B H 0.3718 0.2570 0.7734 0.039 Uiso 1 1 calc R . . C2 C 0.4568(4) -0.0388(5) 0.82658(14) 0.0328(9) Uani 1 1 d . . . H2B H 0.3989 -0.0354 0.8547 0.039 Uiso 1 1 calc R . . C3 C 0.6896(4) 0.4791(5) 0.97908(16) 0.0336(9) Uani 1 1 d . . . H3A H 0.5946 0.4786 0.9781 0.040 Uiso 1 1 calc R . . C4 C 0.6987(4) 0.1745(5) 1.02073(16) 0.0370(10) Uani 1 1 d . . . H4A H 0.7465 0.2158 1.0507 0.044 Uiso 1 1 calc R . . C5 C 0.7510(4) 0.1130(6) 0.77177(16) 0.0456(12) Uani 1 1 d . . . H5A H 0.7764 0.1175 0.7371 0.055 Uiso 1 1 calc R . . H5B H 0.7639 0.0081 0.7834 0.055 Uiso 1 1 calc R . . C6 C 0.8377(4) 0.2141(6) 0.80266(18) 0.0455(12) Uani 1 1 d . . . H6A H 0.9248 0.2054 0.7909 0.055 Uiso 1 1 calc R . . H6B H 0.8097 0.3197 0.7976 0.055 Uiso 1 1 calc R . . C7 C 0.9745(4) 0.2114(6) 0.9357(2) 0.0503(13) Uani 1 1 d . . . H7A H 0.9547 0.1029 0.9387 0.060 Uiso 1 1 calc R . . H7B H 1.0658 0.2247 0.9453 0.060 Uiso 1 1 calc R . . C8 C 0.9521(4) 0.2574(6) 0.8828(2) 0.0508(13) Uani 1 1 d . . . H8A H 1.0297 0.2357 0.8649 0.061 Uiso 1 1 calc R . . H8B H 0.9377 0.3675 0.8815 0.061 Uiso 1 1 calc R . . C9 C 0.4587(5) 0.4392(5) 0.8086(2) 0.0480(12) Uani 1 1 d . . . H9A H 0.3898 0.5105 0.8003 0.072 Uiso 1 1 calc R . . H9B H 0.5238 0.4478 0.7842 0.072 Uiso 1 1 calc R . . H9C H 0.4964 0.4619 0.8416 0.072 Uiso 1 1 calc R . . C10 C 0.2964(4) 0.2637(6) 0.84225(18) 0.0446(12) Uani 1 1 d . . . H10A H 0.2299 0.3369 0.8327 0.067 Uiso 1 1 calc R . . H10B H 0.3276 0.2826 0.8765 0.067 Uiso 1 1 calc R . . H10C H 0.2613 0.1616 0.8396 0.067 Uiso 1 1 calc R . . C11 C 0.3760(5) -0.0796(6) 0.77953(17) 0.0504(13) Uani 1 1 d . . . H11A H 0.3366 -0.1785 0.7838 0.076 Uiso 1 1 calc R . . H11B H 0.4302 -0.0828 0.7512 0.076 Uiso 1 1 calc R . . H11C H 0.3095 -0.0036 0.7736 0.076 Uiso 1 1 calc R . . C12 C 0.5574(5) -0.1590(5) 0.83867(18) 0.0473(12) Uani 1 1 d . . . H12A H 0.5164 -0.2576 0.8408 0.071 Uiso 1 1 calc R . . H12B H 0.6022 -0.1353 0.8704 0.071 Uiso 1 1 calc R . . H12C H 0.6184 -0.1612 0.8125 0.071 Uiso 1 1 calc R . . C13 C 0.7362(6) 0.5380(6) 1.0296(2) 0.0564(14) Uani 1 1 d . . . H13A H 0.7048 0.6408 1.0340 0.085 Uiso 1 1 calc R . . H13B H 0.8293 0.5382 1.0320 0.085 Uiso 1 1 calc R . . H13C H 0.7045 0.4730 1.0555 0.085 Uiso 1 1 calc R . . C14 C 0.7296(5) 0.5815(5) 0.93770(19) 0.0466(12) Uani 1 1 d . . . H14A H 0.7016 0.6847 0.9440 0.070 Uiso 1 1 calc R . . H14B H 0.6908 0.5464 0.9060 0.070 Uiso 1 1 calc R . . H14C H 0.8224 0.5796 0.9364 0.070 Uiso 1 1 calc R . . C15 C 0.7417(5) 0.0133(5) 1.01344(19) 0.0481(12) Uani 1 1 d . . . H15A H 0.7196 -0.0476 1.0420 0.072 Uiso 1 1 calc R . . H15B H 0.8340 0.0111 1.0104 0.072 Uiso 1 1 calc R . . H15C H 0.6993 -0.0278 0.9833 0.072 Uiso 1 1 calc R . . C16 C 0.5576(4) 0.1847(5) 1.02922(16) 0.0419(11) Uani 1 1 d . . . H16A H 0.5384 0.1245 1.0583 0.063 Uiso 1 1 calc R . . H16B H 0.5088 0.1463 1.0000 0.063 Uiso 1 1 calc R . . H16C H 0.5345 0.2900 1.0349 0.063 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 0.01517(16) 0.02338(18) 0.03174(18) 0.00177(12) -0.00045(11) -0.00122(12) P1 0.0219(5) 0.0269(5) 0.0239(5) 0.0027(4) 0.0019(4) 0.0009(4) P2 0.0221(5) 0.0204(5) 0.0405(6) 0.0011(4) -0.0110(4) -0.0027(4) P3 0.0517(7) 0.0341(7) 0.0306(6) 0.0007(5) -0.0060(5) 0.0002(6) F1 0.072(2) 0.104(3) 0.075(2) 0.051(2) -0.0347(18) -0.036(2) F2 0.136(4) 0.114(4) 0.081(3) 0.039(2) -0.055(2) -0.084(3) F3 0.212(6) 0.096(4) 0.255(7) 0.063(4) 0.178(6) 0.074(4) F4 0.180(4) 0.076(3) 0.059(2) 0.023(2) -0.041(2) -0.026(3) F5 0.208(5) 0.094(3) 0.055(2) 0.005(2) -0.034(3) -0.082(3) F6 0.120(4) 0.060(3) 0.227(6) 0.027(3) 0.086(4) 0.022(3) N1 0.0332(19) 0.059(3) 0.0275(18) 0.0136(17) 0.0073(14) 0.0106(19) N2 0.0229(18) 0.032(2) 0.065(3) -0.0081(18) -0.0146(17) -0.0038(16) N3 0.0226(17) 0.029(2) 0.056(2) 0.0026(16) 0.0086(15) -0.0004(15) C1 0.028(2) 0.035(2) 0.033(2) 0.0010(18) -0.0036(17) 0.0031(18) C2 0.043(2) 0.027(2) 0.028(2) -0.0013(16) -0.0024(17) -0.0042(19) C3 0.032(2) 0.021(2) 0.047(2) 0.0006(18) -0.0048(18) -0.0017(18) C4 0.045(3) 0.025(2) 0.039(2) 0.0052(18) -0.0196(19) -0.004(2) C5 0.038(2) 0.062(3) 0.039(2) 0.008(2) 0.020(2) 0.010(2) C6 0.032(2) 0.046(3) 0.060(3) 0.013(2) 0.020(2) 0.002(2) C7 0.019(2) 0.043(3) 0.088(4) -0.012(3) -0.012(2) 0.003(2) C8 0.020(2) 0.043(3) 0.090(4) -0.012(3) 0.016(2) -0.005(2) C9 0.045(3) 0.031(3) 0.068(3) 0.005(2) -0.006(2) 0.008(2) C10 0.027(2) 0.059(3) 0.048(3) -0.004(2) 0.0035(19) 0.010(2) C11 0.060(3) 0.047(3) 0.043(3) -0.008(2) -0.014(2) -0.014(3) C12 0.065(3) 0.028(2) 0.048(3) 0.003(2) -0.002(2) 0.002(2) C13 0.074(4) 0.028(3) 0.064(3) -0.011(2) -0.019(3) -0.004(3) C14 0.045(3) 0.027(2) 0.068(3) 0.011(2) 0.006(2) 0.001(2) C15 0.049(3) 0.031(3) 0.062(3) 0.012(2) -0.016(2) -0.003(2) C16 0.051(3) 0.042(3) 0.033(2) 0.0075(19) 0.003(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N3 2.167(3) . ? Pd1 P1 2.2841(10) . ? Pd1 P2 2.2902(11) . ? P1 N1 1.658(3) . ? P1 C1 1.829(4) . ? P1 C2 1.830(4) . ? P2 N2 1.669(4) . ? P2 C3 1.835(4) . ? P2 C4 1.839(5) . ? P3 F3 1.500(4) . ? P3 F2 1.538(4) . ? P3 F1 1.562(3) . ? P3 F6 1.566(4) . ? P3 F4 1.578(4) . ? P3 F5 1.584(4) . ? N1 C5 1.459(5) . ? N1 H1A 0.8800 . ? N2 C7 1.452(6) . ? N2 H2A 0.8800 . ? N3 C6 1.485(6) . ? N3 C8 1.496(6) . ? N3 H3B 0.9300 . ? C1 C10 1.525(6) . ? C1 C9 1.527(6) . ? C1 H1B 1.0000 . ? C2 C12 1.528(6) . ? C2 C11 1.536(6) . ? C2 H2B 1.0000 . ? C3 C14 1.519(6) . ? C3 C13 1.521(6) . ? C3 H3A 1.0000 . ? C4 C15 1.518(6) . ? C4 C16 1.519(7) . ? C4 H4A 1.0000 . ? C5 C6 1.503(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.496(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 N3 Pd1 P1 97.04(10) . . ? N3 Pd1 P2 97.41(10) . . ? P1 Pd1 P2 165.08(4) . . ? N1 P1 C1 102.40(19) . . ? N1 P1 C2 108.0(2) . . ? C1 P1 C2 105.5(2) . . ? N1 P1 Pd1 110.54(14) . . ? C1 P1 Pd1 115.40(14) . . ? C2 P1 Pd1 114.17(13) . . ? N2 P2 C3 104.96(19) . . ? N2 P2 C4 105.4(2) . . ? C3 P2 C4 105.8(2) . . ? N2 P2 Pd1 112.58(15) . . ? C3 P2 Pd1 110.96(14) . . ? C4 P2 Pd1 116.29(14) . . ? F3 P3 F2 94.1(4) . . ? F3 P3 F1 94.1(3) . . ? F2 P3 F1 93.8(2) . . ? F3 P3 F6 174.5(4) . . ? F2 P3 F6 90.7(3) . . ? F1 P3 F6 88.3(3) . . ? F3 P3 F4 89.5(3) . . ? F2 P3 F4 87.1(2) . . ? F1 P3 F4 176.2(3) . . ? F6 P3 F4 88.0(3) . . ? F3 P3 F5 88.0(4) . . ? F2 P3 F5 177.4(3) . . ? F1 P3 F5 87.5(2) . . ? F6 P3 F5 87.2(3) . . ? F4 P3 F5 91.4(2) . . ? C5 N1 P1 123.9(3) . . ? C5 N1 H1A 118.1 . . ? P1 N1 H1A 118.1 . . ? C7 N2 P2 120.8(3) . . ? C7 N2 H2A 119.6 . . ? P2 N2 H2A 119.6 . . ? C6 N3 C8 110.8(4) . . ? C6 N3 Pd1 115.0(3) . . ? C8 N3 Pd1 115.1(3) . . ? C6 N3 H3B 104.9 . . ? C8 N3 H3B 104.9 . . ? Pd1 N3 H3B 104.9 . . ? C10 C1 C9 111.3(4) . . ? C10 C1 P1 112.2(3) . . ? C9 C1 P1 109.7(3) . . ? C10 C1 H1B 107.8 . . ? C9 C1 H1B 107.8 . . ? P1 C1 H1B 107.8 . . ? C12 C2 C11 111.1(4) . . ? C12 C2 P1 109.2(3) . . ? C11 C2 P1 113.4(3) . . ? C12 C2 H2B 107.6 . . ? C11 C2 H2B 107.6 . . ? P1 C2 H2B 107.6 . . ? C14 C3 C13 111.5(4) . . ? C14 C3 P2 109.2(3) . . ? C13 C3 P2 113.4(3) . . ? C14 C3 H3A 107.5 . . ? C13 C3 H3A 107.5 . . ? P2 C3 H3A 107.5 . . ? C15 C4 C16 112.1(4) . . ? C15 C4 P2 108.6(3) . . ? C16 C4 P2 111.9(3) . . ? C15 C4 H4A 108.0 . . ? C16 C4 H4A 108.0 . . ? P2 C4 H4A 108.0 . . ? N1 C5 C6 115.6(4) . . ? N1 C5 H5A 108.4 . . ? C6 C5 H5A 108.4 . . ? N1 C5 H5B 108.4 . . ? C6 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? N3 C6 C5 114.2(4) . . ? N3 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? N3 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? N2 C7 C8 114.5(4) . . ? N2 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N2 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C7 C8 N3 114.2(4) . . ? C7 C8 H8A 108.7 . . ? N3 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? N3 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.088 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.089 #=== END data_mjs069_0m_compound16b _database_code_depnum_ccdc_archive 'CCDC 867391' #TrackingRef '- All Cif Files Compiled.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C16 H40 F6 N3 P3 Pt' _chemical_formula_weight 676.51 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' F F 0.0171 0.0103 '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' Pt Pt -1.7033 8.3905 '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 10.4144(5) _cell_length_b 10.5406(6) _cell_length_c 12.3384(7) _cell_angle_alpha 84.575(2) _cell_angle_beta 67.522(2) _cell_angle_gamma 88.505(2) _cell_volume 1245.85(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9976 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 5.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6493 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 17256 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4376 _reflns_number_gt 4217 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0130P)^2^+1.3087P] 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 4376 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0167 _refine_ls_R_factor_gt 0.0155 _refine_ls_wR_factor_ref 0.0358 _refine_ls_wR_factor_gt 0.0354 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.909272(10) 0.725893(9) 0.723733(8) 0.01719(4) Uani 1 1 d . . . P1 P 1.10863(7) 0.80389(6) 0.72779(6) 0.01853(14) Uani 1 1 d . . . P2 P 0.74008(7) 0.61527(7) 0.69889(6) 0.02155(15) Uani 1 1 d . . . P3 P 0.62761(8) 0.80909(8) 0.17540(7) 0.02952(17) Uani 1 1 d . . . F1 F 0.5760(2) 0.6924(2) 0.2722(2) 0.0675(7) Uani 1 1 d . . . F2 F 0.6841(2) 0.7148(2) 0.07464(18) 0.0564(6) Uani 1 1 d . . . F3 F 0.6775(3) 0.9267(2) 0.07719(19) 0.0682(7) Uani 1 1 d . . . F4 F 0.5730(3) 0.9079(2) 0.27169(19) 0.0705(7) Uani 1 1 d . . . F5 F 0.7725(2) 0.8053(3) 0.1885(2) 0.0725(7) Uani 1 1 d . . . F6 F 0.4813(2) 0.8128(2) 0.1625(2) 0.0586(6) Uani 1 1 d . . . N1 N 1.0960(2) 0.9555(2) 0.7578(2) 0.0262(5) Uani 1 1 d . . . H1A H 1.1718 1.0032 0.7292 0.031 Uiso 1 1 calc R . . N2 N 0.5819(2) 0.6756(2) 0.7643(2) 0.0273(5) Uani 1 1 d . . . H2A H 0.5139 0.6522 0.7445 0.033 Uiso 1 1 calc R . . N3 N 0.7794(2) 0.8738(2) 0.8173(2) 0.0227(5) Uani 1 1 d . . . H3B H 0.7631 0.8516 0.8963 0.027 Uiso 1 1 calc R . . C1 C 1.2535(3) 0.8041(3) 0.5854(2) 0.0225(6) Uani 1 1 d . . . H1B H 1.2712 0.7133 0.5673 0.027 Uiso 1 1 calc R . . C2 C 1.1670(3) 0.7126(3) 0.8349(2) 0.0267(6) Uani 1 1 d . . . H2B H 1.2490 0.7582 0.8369 0.032 Uiso 1 1 calc R . . C3 C 0.7633(3) 0.6131(3) 0.5440(2) 0.0265(6) Uani 1 1 d . . . H3A H 0.8480 0.5619 0.5048 0.032 Uiso 1 1 calc R . . C4 C 0.7265(3) 0.4478(3) 0.7583(3) 0.0335(7) Uani 1 1 d . . . H4A H 0.6439 0.4090 0.7510 0.040 Uiso 1 1 calc R . . C5 C 0.9657(3) 1.0136(3) 0.8293(3) 0.0315(7) Uani 1 1 d . . . H5A H 0.9833 1.1053 0.8301 0.038 Uiso 1 1 calc R . . H5B H 0.9364 0.9743 0.9113 0.038 Uiso 1 1 calc R . . C6 C 0.8476(3) 1.0015(3) 0.7891(3) 0.0296(7) Uani 1 1 d . . . H6A H 0.7766 1.0654 0.8256 0.036 Uiso 1 1 calc R . . H6B H 0.8830 1.0225 0.7028 0.036 Uiso 1 1 calc R . . C7 C 0.5529(3) 0.7660(3) 0.8535(3) 0.0322(7) Uani 1 1 d . . . H7A H 0.5687 0.7233 0.9222 0.039 Uiso 1 1 calc R . . H7B H 0.4536 0.7893 0.8802 0.039 Uiso 1 1 calc R . . C8 C 0.6396(3) 0.8859(3) 0.8119(3) 0.0300(7) Uani 1 1 d . . . H8A H 0.6509 0.9120 0.7295 0.036 Uiso 1 1 calc R . . H8B H 0.5891 0.9544 0.8605 0.036 Uiso 1 1 calc R . . C9 C 1.2129(3) 0.8730(3) 0.4891(3) 0.0329(7) Uani 1 1 d . . . H9A H 1.2912 0.8723 0.4131 0.049 Uiso 1 1 calc R . . H9B H 1.1888 0.9613 0.5066 0.049 Uiso 1 1 calc R . . H9C H 1.1326 0.8297 0.4856 0.049 Uiso 1 1 calc R . . C10 C 1.3888(3) 0.8587(3) 0.5830(3) 0.0355(7) Uani 1 1 d . . . H10A H 1.4614 0.8550 0.5043 0.053 Uiso 1 1 calc R . . H10B H 1.4171 0.8087 0.6411 0.053 Uiso 1 1 calc R . . H10C H 1.3749 0.9475 0.6020 0.053 Uiso 1 1 calc R . . C11 C 1.0512(4) 0.7101(4) 0.9571(3) 0.0438(8) Uani 1 1 d . . . H11A H 1.0817 0.6618 1.0148 0.066 Uiso 1 1 calc R . . H11B H 0.9681 0.6693 0.9563 0.066 Uiso 1 1 calc R . . H11C H 1.0295 0.7975 0.9788 0.066 Uiso 1 1 calc R . . C12 C 1.2111(3) 0.5785(3) 0.8027(3) 0.0376(8) Uani 1 1 d . . . H12A H 1.2415 0.5343 0.8622 0.056 Uiso 1 1 calc R . . H12B H 1.2880 0.5824 0.7256 0.056 Uiso 1 1 calc R . . H12C H 1.1324 0.5321 0.7996 0.056 Uiso 1 1 calc R . . C13 C 0.7901(3) 0.7482(3) 0.4829(3) 0.0339(7) Uani 1 1 d . . . H13A H 0.8030 0.7462 0.4001 0.051 Uiso 1 1 calc R . . H13B H 0.8741 0.7832 0.4873 0.051 Uiso 1 1 calc R . . H13C H 0.7106 0.8019 0.5220 0.051 Uiso 1 1 calc R . . C14 C 0.6412(3) 0.5506(3) 0.5287(3) 0.0358(7) Uani 1 1 d . . . H14A H 0.6594 0.5514 0.4447 0.054 Uiso 1 1 calc R . . H14B H 0.5561 0.5979 0.5675 0.054 Uiso 1 1 calc R . . H14C H 0.6297 0.4623 0.5643 0.054 Uiso 1 1 calc R . . C15 C 0.8540(4) 0.3706(3) 0.6925(3) 0.0476(9) Uani 1 1 d . . . H15A H 0.8409 0.2821 0.7276 0.071 Uiso 1 1 calc R . . H15B H 0.9364 0.4072 0.6983 0.071 Uiso 1 1 calc R . . H15C H 0.8664 0.3729 0.6095 0.071 Uiso 1 1 calc R . . C16 C 0.7017(4) 0.4413(3) 0.8884(3) 0.0444(9) Uani 1 1 d . . . H16A H 0.6941 0.3519 0.9206 0.067 Uiso 1 1 calc R . . H16B H 0.6154 0.4854 0.9305 0.067 Uiso 1 1 calc R . . H16C H 0.7796 0.4823 0.8979 0.067 Uiso 1 1 calc R . . H40 H 1.012(3) 0.608(3) 0.653(2) 0.025(7) Uiso 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 Pt1 0.01528(6) 0.01723(6) 0.02111(6) -0.00110(4) -0.00926(4) -0.00144(4) P1 0.0168(3) 0.0187(4) 0.0222(4) -0.0021(3) -0.0096(3) -0.0020(3) P2 0.0186(3) 0.0238(4) 0.0250(4) 0.0004(3) -0.0116(3) -0.0047(3) P3 0.0299(4) 0.0339(4) 0.0251(4) -0.0065(3) -0.0096(3) -0.0051(3) F1 0.0655(15) 0.0685(16) 0.0626(15) 0.0264(12) -0.0244(12) -0.0129(12) F2 0.0714(14) 0.0594(14) 0.0549(13) -0.0301(11) -0.0385(12) 0.0243(11) F3 0.0807(17) 0.0532(14) 0.0499(13) 0.0084(11) -0.0039(12) -0.0154(12) F4 0.0858(17) 0.0788(17) 0.0471(13) -0.0346(12) -0.0192(13) 0.0075(14) F5 0.0396(12) 0.117(2) 0.0744(16) -0.0293(15) -0.0311(12) -0.0065(13) F6 0.0441(12) 0.0487(13) 0.0935(17) -0.0068(12) -0.0383(12) 0.0056(10) N1 0.0218(12) 0.0196(12) 0.0376(14) -0.0071(10) -0.0103(11) -0.0045(10) N2 0.0173(12) 0.0378(15) 0.0310(13) -0.0036(11) -0.0135(10) -0.0040(10) N3 0.0201(12) 0.0239(12) 0.0255(12) -0.0039(10) -0.0102(10) 0.0022(10) C1 0.0209(14) 0.0218(15) 0.0237(14) -0.0015(11) -0.0072(12) -0.0033(11) C2 0.0220(14) 0.0353(17) 0.0265(15) -0.0016(13) -0.0138(12) 0.0003(12) C3 0.0241(15) 0.0309(16) 0.0268(15) -0.0058(12) -0.0114(12) -0.0018(12) C4 0.0296(16) 0.0279(17) 0.0457(19) 0.0120(14) -0.0200(15) -0.0142(13) C5 0.0311(16) 0.0249(16) 0.0418(18) -0.0134(14) -0.0150(14) 0.0013(13) C6 0.0286(15) 0.0201(15) 0.0395(18) -0.0033(13) -0.0121(14) 0.0029(12) C7 0.0176(14) 0.049(2) 0.0310(17) -0.0086(14) -0.0091(13) 0.0001(13) C8 0.0214(14) 0.0331(17) 0.0375(17) -0.0080(14) -0.0130(13) 0.0077(12) C9 0.0331(17) 0.0390(18) 0.0240(16) 0.0024(13) -0.0089(13) -0.0042(14) C10 0.0215(15) 0.046(2) 0.0341(18) 0.0018(15) -0.0054(13) -0.0109(14) C11 0.047(2) 0.059(2) 0.0260(17) 0.0014(16) -0.0172(16) 0.0136(17) C12 0.0393(18) 0.0385(19) 0.0368(18) 0.0042(15) -0.0189(15) 0.0085(15) C13 0.0370(17) 0.0385(18) 0.0298(17) 0.0034(14) -0.0179(14) -0.0061(14) C14 0.0375(18) 0.0395(19) 0.0388(18) -0.0112(15) -0.0218(15) -0.0059(14) C15 0.061(2) 0.0182(17) 0.061(2) 0.0011(16) -0.021(2) -0.0006(16) C16 0.0401(19) 0.043(2) 0.044(2) 0.0174(16) -0.0141(16) -0.0012(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N3 2.152(2) . ? Pt1 P2 2.2685(7) . ? Pt1 P1 2.2728(6) . ? Pt1 H40 1.69(3) . ? P1 N1 1.665(2) . ? P1 C1 1.826(3) . ? P1 C2 1.840(3) . ? P2 N2 1.672(2) . ? P2 C4 1.834(3) . ? P2 C3 1.835(3) . ? P3 F5 1.577(2) . ? P3 F1 1.579(2) . ? P3 F4 1.583(2) . ? P3 F2 1.588(2) . ? P3 F6 1.591(2) . ? P3 F3 1.595(2) . ? N1 C5 1.462(4) . ? N1 H1A 0.8800 . ? N2 C7 1.462(4) . ? N2 H2A 0.8800 . ? N3 C8 1.484(3) . ? N3 C6 1.486(4) . ? N3 H3B 0.9300 . ? C1 C10 1.524(4) . ? C1 C9 1.525(4) . ? C1 H1B 1.0000 . ? C2 C12 1.516(4) . ? C2 C11 1.528(4) . ? C2 H2B 1.0000 . ? C3 C13 1.527(4) . ? C3 C14 1.529(4) . ? C3 H3A 1.0000 . ? C4 C16 1.520(5) . ? C4 C15 1.525(5) . ? C4 H4A 1.0000 . ? C5 C6 1.504(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.503(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 N3 Pt1 P2 97.19(6) . . ? N3 Pt1 P1 94.99(6) . . ? P2 Pt1 P1 167.82(3) . . ? N3 Pt1 H40 178.7(9) . . ? P2 Pt1 H40 83.2(9) . . ? P1 Pt1 H40 84.6(9) . . ? N1 P1 C1 104.21(12) . . ? N1 P1 C2 107.35(12) . . ? C1 P1 C2 106.06(12) . . ? N1 P1 Pt1 112.87(8) . . ? C1 P1 Pt1 112.33(9) . . ? C2 P1 Pt1 113.35(9) . . ? N2 P2 C4 105.52(13) . . ? N2 P2 C3 104.92(12) . . ? C4 P2 C3 105.81(14) . . ? N2 P2 Pt1 112.91(8) . . ? C4 P2 Pt1 113.54(9) . . ? C3 P2 Pt1 113.36(9) . . ? F5 P3 F1 89.68(14) . . ? F5 P3 F4 90.11(13) . . ? F1 P3 F4 91.78(14) . . ? F5 P3 F2 90.10(12) . . ? F1 P3 F2 90.61(13) . . ? F4 P3 F2 177.60(14) . . ? F5 P3 F6 179.89(17) . . ? F1 P3 F6 90.23(12) . . ? F4 P3 F6 89.84(13) . . ? F2 P3 F6 89.96(12) . . ? F5 P3 F3 91.27(14) . . ? F1 P3 F3 179.03(14) . . ? F4 P3 F3 88.39(13) . . ? F2 P3 F3 89.22(13) . . ? F6 P3 F3 88.82(13) . . ? C5 N1 P1 123.52(19) . . ? C5 N1 H1A 118.2 . . ? P1 N1 H1A 118.2 . . ? C7 N2 P2 122.06(18) . . ? C7 N2 H2A 119.0 . . ? P2 N2 H2A 119.0 . . ? C8 N3 C6 109.2(2) . . ? C8 N3 Pt1 116.43(17) . . ? C6 N3 Pt1 114.10(17) . . ? C8 N3 H3B 105.3 . . ? C6 N3 H3B 105.3 . . ? Pt1 N3 H3B 105.3 . . ? C10 C1 C9 110.8(2) . . ? C10 C1 P1 114.3(2) . . ? C9 C1 P1 110.12(19) . . ? C10 C1 H1B 107.1 . . ? C9 C1 H1B 107.1 . . ? P1 C1 H1B 107.1 . . ? C12 C2 C11 110.8(3) . . ? C12 C2 P1 112.77(19) . . ? C11 C2 P1 109.01(19) . . ? C12 C2 H2B 108.0 . . ? C11 C2 H2B 108.0 . . ? P1 C2 H2B 108.0 . . ? C13 C3 C14 111.0(2) . . ? C13 C3 P2 109.92(19) . . ? C14 C3 P2 113.0(2) . . ? C13 C3 H3A 107.6 . . ? C14 C3 H3A 107.6 . . ? P2 C3 H3A 107.6 . . ? C16 C4 C15 110.4(3) . . ? C16 C4 P2 109.1(2) . . ? C15 C4 P2 112.9(2) . . ? C16 C4 H4A 108.1 . . ? C15 C4 H4A 108.1 . . ? P2 C4 H4A 108.1 . . ? N1 C5 C6 115.3(2) . . ? N1 C5 H5A 108.4 . . ? C6 C5 H5A 108.4 . . ? N1 C5 H5B 108.4 . . ? C6 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? N3 C6 C5 115.1(2) . . ? N3 C6 H6A 108.5 . . ? C5 C6 H6A 108.5 . . ? N3 C6 H6B 108.5 . . ? C5 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? N2 C7 C8 114.3(2) . . ? N2 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? N2 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? N3 C8 C7 114.3(2) . . ? N3 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? N3 C8 H8B 108.7 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C1 C10 H10A 109.5 . . ? C1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C2 C12 H12A 109.5 . . ? C2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C3 C13 H13A 109.5 . . ? C3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 H14A 109.5 . . ? C3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C4 C16 H16A 109.5 . . ? C4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.695 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.071 #=== END data_mjs064a_0m_compound17b _database_code_depnum_ccdc_archive 'CCDC 867392' #TrackingRef '- All Cif Files Compiled.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C12.80 H30.40 F4.80 N1.60 P2.40 Pt0.80 S0.80' _chemical_formula_weight 554.04 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.1465(4) _cell_length_b 20.2920(9) _cell_length_c 15.7726(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.056(2) _cell_angle_gamma 90.00 _cell_volume 2606.9(2) _cell_formula_units_Z 5 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9926 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 23.51 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 5.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5778 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 37621 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8621 _reflns_number_gt 7506 _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^)+(0.0816P)^2^+54.4267P] 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 0.984(15) _refine_ls_number_reflns 8621 _refine_ls_number_parameters 523 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1662 _refine_ls_wR_factor_gt 0.1594 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Pt1 Pt 0.71775(8) 0.69902(3) 0.45491(4) 0.02889(18) Uani 1 1 d . . . Pt2 Pt 0.20017(8) 0.80094(3) 0.04175(4) 0.02866(18) Uani 1 1 d . . . P6 P 0.4074(7) 0.5709(3) 0.7330(4) 0.0449(13) Uani 1 1 d . . . P5 P 0.8751(7) 0.9404(3) 0.7756(3) 0.0423(13) Uani 1 1 d . . . P2 P 0.7029(8) 0.6140(3) 0.3612(3) 0.0428(13) Uani 1 1 d . . . P3 P 0.2344(7) 0.8842(3) 0.1385(3) 0.0371(12) Uani 1 1 d . . . S2 S 0.4198(6) 0.8373(3) -0.0414(3) 0.0439(12) Uani 1 1 d . . . P4 P 0.1429(6) 0.7118(2) -0.0411(3) 0.0327(11) Uani 1 1 d . . . S1 S 0.9485(7) 0.6643(3) 0.5318(4) 0.0474(13) Uani 1 1 d . . . C20 C 0.254(3) 0.6367(10) -0.0104(13) 0.042(5) Uani 1 1 d . . . H20A H 0.2337 0.6027 -0.0554 0.050 Uiso 1 1 calc R . . P1 P 0.6831(7) 0.7916(3) 0.5371(3) 0.0372(12) Uani 1 1 d . . . N4 N 0.196(2) 0.7246(8) -0.1402(10) 0.045(4) Uani 1 1 d . . . H4A H 0.2128 0.6902 -0.1727 0.054 Uiso 1 1 calc R . . F5 F 0.916(2) 1.0148(7) 0.7724(10) 0.072(4) Uani 1 1 d . . . N1 N 0.756(2) 0.7769(8) 0.6330(10) 0.046(5) Uani 1 1 d . . . H1A H 0.7897 0.8101 0.6648 0.056 Uiso 1 1 calc R . . C5 C 0.766(3) 0.7087(14) 0.6676(14) 0.055(6) Uani 1 1 d . . . H5A H 0.6711 0.6829 0.6462 0.066 Uiso 1 1 calc R . . H5B H 0.7606 0.7105 0.7302 0.066 Uiso 1 1 calc R . . F1 F 0.799(3) 0.9460(9) 0.6840(10) 0.100(6) Uani 1 1 d . . . F9 F 0.243(2) 0.5800(9) 0.7804(12) 0.103(7) Uani 1 1 d . . . F3 F 0.955(3) 0.9343(9) 0.8668(11) 0.111(7) Uani 1 1 d . . . F12 F 0.388(3) 0.4939(8) 0.7258(12) 0.105(6) Uani 1 1 d . . . C4 C 0.734(3) 0.6411(12) 0.2523(14) 0.052(6) Uani 1 1 d . . . H4B H 0.6479 0.6749 0.2391 0.063 Uiso 1 1 calc R . . N3 N 0.324(3) 0.9493(10) 0.0978(14) 0.062(6) Uani 1 1 d . . . H3A H 0.3706 0.9784 0.1320 0.075 Uiso 1 1 calc R . . C19 C -0.077(3) 0.6907(12) -0.0465(13) 0.048(5) Uani 1 1 d . . . H19A H -0.1105 0.6795 0.0123 0.058 Uiso 1 1 calc R . . C32 C 0.186(4) 0.6093(14) 0.0761(14) 0.076(9) Uani 1 1 d . . . H32A H 0.2458 0.5691 0.0918 0.113 Uiso 1 1 calc R . . H32B H 0.0689 0.5994 0.0694 0.113 Uiso 1 1 calc R . . H32C H 0.2020 0.6425 0.1206 0.113 Uiso 1 1 calc R . . C31 C 0.440(3) 0.6514(11) -0.0056(18) 0.056(6) Uani 1 1 d . . . H31A H 0.4995 0.6113 0.0105 0.084 Uiso 1 1 calc R . . H31B H 0.4613 0.6858 0.0369 0.084 Uiso 1 1 calc R . . H31C H 0.4768 0.6666 -0.0611 0.084 Uiso 1 1 calc R . . N2 N 0.819(3) 0.5489(9) 0.3854(14) 0.060(6) Uani 1 1 d . . . H2A H 0.7863 0.5098 0.3677 0.071 Uiso 1 1 calc R . . F11 F 0.431(3) 0.6468(7) 0.7441(15) 0.127(9) Uani 1 1 d . . . C1 C 0.469(3) 0.8138(11) 0.5448(13) 0.050(6) Uani 1 1 d . . . H1B H 0.4251 0.8253 0.4870 0.060 Uiso 1 1 calc R . . F6 F 0.831(3) 0.8648(8) 0.7779(10) 0.112(7) Uani 1 1 d . . . F2 F 1.046(2) 0.9281(9) 0.7366(16) 0.116(7) Uani 1 1 d . . . C23 C 0.215(3) 0.7897(13) -0.1765(12) 0.052(6) Uani 1 1 d . . . H23A H 0.1268 0.8187 -0.1561 0.062 Uiso 1 1 calc R . . H23B H 0.2041 0.7866 -0.2390 0.062 Uiso 1 1 calc R . . C11 C 0.716(5) 0.8869(16) 0.4123(17) 0.089(10) Uani 1 1 d . . . H11A H 0.7738 0.9266 0.3934 0.133 Uiso 1 1 calc R . . H11B H 0.5991 0.8965 0.4173 0.133 Uiso 1 1 calc R . . H11C H 0.7316 0.8515 0.3711 0.133 Uiso 1 1 calc R . . C10 C 0.441(3) 0.8739(12) 0.6067(17) 0.061(7) Uani 1 1 d . . . H10A H 0.3230 0.8841 0.6083 0.092 Uiso 1 1 calc R . . H10B H 0.5006 0.9124 0.5864 0.092 Uiso 1 1 calc R . . H10C H 0.4802 0.8623 0.6638 0.092 Uiso 1 1 calc R . . C30 C -0.113(3) 0.6310(13) -0.1016(17) 0.063(7) Uani 1 1 d . . . H30A H -0.2317 0.6221 -0.1018 0.095 Uiso 1 1 calc R . . H30B H -0.0541 0.5927 -0.0789 0.095 Uiso 1 1 calc R . . H30C H -0.0783 0.6397 -0.1596 0.095 Uiso 1 1 calc R . . C24 C 0.381(4) 0.8204(15) -0.1536(12) 0.078(10) Uani 1 1 d . . . H24A H 0.3912 0.8623 -0.1852 0.094 Uiso 1 1 calc R . . H24B H 0.4685 0.7906 -0.1736 0.094 Uiso 1 1 calc R . . F4 F 0.708(2) 0.9567(12) 0.8141(15) 0.130(9) Uani 1 1 d . . . C3 C 0.491(3) 0.5753(13) 0.3608(18) 0.070(8) Uani 1 1 d . . . H3B H 0.4979 0.5342 0.3260 0.084 Uiso 1 1 calc R . . C2 C 0.789(3) 0.8648(11) 0.5015(14) 0.048(6) Uani 1 1 d . . . H2B H 0.7670 0.9009 0.5430 0.057 Uiso 1 1 calc R . . C7 C 0.968(3) 0.5534(15) 0.4337(19) 0.076(9) Uani 1 1 d . . . H7A H 1.0411 0.5847 0.4044 0.091 Uiso 1 1 calc R . . H7B H 1.0223 0.5097 0.4321 0.091 Uiso 1 1 calc R . . C8 C 0.960(4) 0.5737(12) 0.5225(17) 0.070(8) Uani 1 1 d . . . H8A H 1.0590 0.5576 0.5537 0.084 Uiso 1 1 calc R . . H8B H 0.8627 0.5536 0.5486 0.084 Uiso 1 1 calc R . . C17 C 0.045(3) 0.9133(12) 0.1863(15) 0.052(6) Uani 1 1 d . . . H17A H -0.0065 0.8752 0.2160 0.063 Uiso 1 1 calc R . . C9 C 0.370(3) 0.7563(13) 0.5804(19) 0.070(7) Uani 1 1 d . . . H9A H 0.2542 0.7691 0.5840 0.105 Uiso 1 1 calc R . . H9B H 0.4123 0.7449 0.6371 0.105 Uiso 1 1 calc R . . H9C H 0.3795 0.7180 0.5429 0.105 Uiso 1 1 calc R . . F8 F 0.568(3) 0.5667(11) 0.683(3) 0.200(17) Uani 1 1 d . . . C12 C 0.966(3) 0.8537(12) 0.5003(18) 0.064(7) Uani 1 1 d . . . H12A H 1.0214 0.8939 0.4813 0.096 Uiso 1 1 calc R . . H12B H 0.9907 0.8176 0.4613 0.096 Uiso 1 1 calc R . . H12C H 1.0061 0.8423 0.5575 0.096 Uiso 1 1 calc R . . C6 C 0.923(3) 0.6742(12) 0.6431(15) 0.062(7) Uani 1 1 d . . . H6A H 0.9252 0.6301 0.6700 0.074 Uiso 1 1 calc R . . H6B H 1.0173 0.6995 0.6663 0.074 Uiso 1 1 calc R . . C14 C 0.444(3) 0.5551(13) 0.4465(15) 0.059(7) Uani 1 1 d . . . H14A H 0.3351 0.5348 0.4441 0.089 Uiso 1 1 calc R . . H14B H 0.4423 0.5938 0.4836 0.089 Uiso 1 1 calc R . . H14C H 0.5242 0.5231 0.4689 0.089 Uiso 1 1 calc R . . C13 C 0.364(3) 0.6201(14) 0.3169(19) 0.073(8) Uani 1 1 d . . . H13A H 0.2561 0.5989 0.3175 0.110 Uiso 1 1 calc R . . H13B H 0.3959 0.6279 0.2581 0.110 Uiso 1 1 calc R . . H13C H 0.3590 0.6623 0.3470 0.110 Uiso 1 1 calc R . . F10 F 0.489(4) 0.5627(12) 0.8202(16) 0.165(13) Uani 1 1 d . . . C26 C 0.074(4) 0.9681(14) 0.2515(19) 0.075(8) Uani 1 1 d . . . H26A H -0.0309 0.9815 0.2753 0.112 Uiso 1 1 calc R . . H26B H 0.1253 1.0059 0.2239 0.112 Uiso 1 1 calc R . . H26C H 0.1469 0.9518 0.2971 0.112 Uiso 1 1 calc R . . C18 C 0.366(4) 0.8574(16) 0.2277(16) 0.074(8) Uani 1 1 d . . . H18A H 0.3932 0.8972 0.2626 0.089 Uiso 1 1 calc R . . C28 C 0.286(5) 0.8097(18) 0.283(2) 0.113(13) Uani 1 1 d . . . H28A H 0.3619 0.7976 0.3295 0.170 Uiso 1 1 calc R . . H28B H 0.2565 0.7703 0.2504 0.170 Uiso 1 1 calc R . . H28C H 0.1870 0.8294 0.3065 0.170 Uiso 1 1 calc R . . C16 C 0.712(4) 0.5841(14) 0.1860(14) 0.076(8) Uani 1 1 d . . . H16A H 0.7308 0.6011 0.1290 0.114 Uiso 1 1 calc R . . H16B H 0.5996 0.5666 0.1888 0.114 Uiso 1 1 calc R . . H16C H 0.7904 0.5488 0.1989 0.114 Uiso 1 1 calc R . . C29 C -0.175(3) 0.7480(13) -0.074(2) 0.071(8) Uani 1 1 d . . . H29A H -0.2918 0.7358 -0.0761 0.106 Uiso 1 1 calc R . . H29B H -0.1411 0.7621 -0.1303 0.106 Uiso 1 1 calc R . . H29C H -0.1590 0.7842 -0.0335 0.106 Uiso 1 1 calc R . . F7 F 0.323(5) 0.5775(17) 0.6462(14) 0.219(19) Uani 1 1 d . . . C22 C 0.429(7) 0.9250(18) -0.038(3) 0.16(3) Uani 1 1 d . . . H22A H 0.5419 0.9371 -0.0206 0.191 Uiso 1 1 calc R . . H22B H 0.4134 0.9407 -0.0975 0.191 Uiso 1 1 calc R . . C15 C 0.900(4) 0.6754(17) 0.248(2) 0.103(12) Uani 1 1 d . . . H15A H 0.9186 0.6901 0.1901 0.155 Uiso 1 1 calc R . . H15B H 0.9865 0.6446 0.2659 0.155 Uiso 1 1 calc R . . H15C H 0.9006 0.7136 0.2863 0.155 Uiso 1 1 calc R . . C25 C -0.072(3) 0.9353(15) 0.116(2) 0.082(10) Uani 1 1 d . . . H25A H -0.1741 0.9510 0.1406 0.123 Uiso 1 1 calc R . . H25B H -0.0952 0.8981 0.0780 0.123 Uiso 1 1 calc R . . H25C H -0.0212 0.9710 0.0838 0.123 Uiso 1 1 calc R . . C27 C 0.527(4) 0.8282(19) 0.197(2) 0.112(13) Uani 1 1 d . . . H27A H 0.5952 0.8147 0.2457 0.168 Uiso 1 1 calc R . . H27B H 0.5860 0.8615 0.1640 0.168 Uiso 1 1 calc R . . H27C H 0.5040 0.7898 0.1609 0.168 Uiso 1 1 calc R . . C21 C 0.328(11) 0.9596(16) 0.009(3) 0.24(5) Uani 1 1 d . . . H21B H 0.2154 0.9522 -0.0138 0.290 Uiso 1 1 calc R . . H21A H 0.3535 1.0068 -0.0004 0.290 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0368(4) 0.0240(4) 0.0256(3) -0.0027(3) -0.0059(3) 0.0011(3) Pt2 0.0350(4) 0.0248(4) 0.0263(3) -0.0019(3) 0.0046(3) -0.0050(3) P6 0.049(3) 0.042(3) 0.044(3) 0.005(2) 0.003(2) 0.009(3) P5 0.052(3) 0.035(3) 0.039(3) 0.001(2) -0.004(2) -0.004(2) P2 0.063(4) 0.034(3) 0.031(3) -0.005(2) -0.001(2) 0.005(3) P3 0.048(3) 0.031(3) 0.033(3) -0.008(2) 0.001(2) -0.010(2) S2 0.042(3) 0.046(3) 0.044(3) -0.005(2) 0.012(2) -0.007(2) P4 0.045(3) 0.026(3) 0.027(2) -0.0016(19) 0.0060(19) 0.002(2) S1 0.041(3) 0.056(3) 0.046(3) -0.002(2) -0.005(2) 0.000(3) C20 0.062(14) 0.032(12) 0.033(11) 0.006(9) 0.016(10) 0.019(10) P1 0.055(3) 0.030(3) 0.027(2) 0.001(2) -0.007(2) 0.002(2) N4 0.068(12) 0.036(10) 0.031(9) -0.003(7) 0.014(8) 0.000(8) F5 0.097(11) 0.038(8) 0.081(10) -0.006(7) -0.002(8) -0.007(7) N1 0.085(14) 0.030(9) 0.024(8) -0.002(7) -0.008(8) -0.002(8) C5 0.058(14) 0.068(18) 0.039(11) 0.003(12) -0.008(10) 0.016(14) F1 0.159(18) 0.091(13) 0.049(9) -0.008(8) -0.030(10) 0.002(12) F9 0.095(12) 0.091(13) 0.124(15) -0.058(12) 0.056(11) -0.025(10) F3 0.18(2) 0.087(13) 0.063(11) 0.002(9) -0.044(12) 0.012(13) F12 0.150(17) 0.056(10) 0.112(14) -0.032(10) 0.049(13) -0.025(10) C4 0.066(15) 0.042(13) 0.048(13) -0.012(10) -0.003(11) 0.017(11) N3 0.081(15) 0.040(11) 0.066(14) -0.014(10) 0.012(11) -0.025(10) C19 0.065(14) 0.043(13) 0.036(10) -0.006(10) 0.013(9) -0.006(11) C32 0.14(3) 0.064(19) 0.028(12) 0.026(12) 0.009(14) -0.006(17) C31 0.052(14) 0.030(12) 0.085(18) 0.003(11) -0.009(13) 0.012(10) N2 0.078(14) 0.023(10) 0.077(14) -0.005(9) -0.001(11) 0.021(9) F11 0.140(16) 0.034(8) 0.21(2) 0.002(11) 0.117(17) 0.002(9) C1 0.066(14) 0.047(14) 0.036(11) -0.012(10) -0.008(10) -0.012(11) F6 0.21(2) 0.059(10) 0.062(10) 0.010(8) -0.018(12) -0.056(12) F2 0.084(12) 0.072(12) 0.19(2) 0.020(13) 0.023(13) 0.023(10) C23 0.070(15) 0.066(17) 0.020(9) 0.012(10) -0.003(9) -0.003(13) C11 0.16(3) 0.06(2) 0.049(17) 0.006(14) -0.002(18) 0.003(19) C10 0.057(14) 0.047(14) 0.080(17) -0.023(13) 0.009(13) 0.005(11) C30 0.044(13) 0.064(16) 0.081(18) -0.023(14) 0.000(12) -0.003(12) C24 0.11(2) 0.11(2) 0.013(9) 0.011(11) 0.033(12) -0.045(18) F4 0.086(13) 0.16(2) 0.15(2) -0.030(16) 0.059(14) -0.012(13) C3 0.081(19) 0.052(16) 0.076(18) -0.032(13) -0.019(15) -0.002(14) C2 0.071(16) 0.030(12) 0.042(12) -0.003(9) 0.000(11) -0.016(10) C7 0.064(17) 0.08(2) 0.09(2) -0.021(16) -0.002(15) 0.037(15) C8 0.10(2) 0.042(15) 0.070(18) 0.004(12) -0.028(15) 0.024(14) C17 0.040(12) 0.049(14) 0.067(15) 0.003(11) -0.005(11) -0.009(11) C9 0.054(15) 0.065(17) 0.09(2) -0.004(15) 0.018(14) -0.003(13) F8 0.125(18) 0.084(15) 0.40(5) -0.04(2) 0.16(3) 0.000(13) C12 0.081(19) 0.039(14) 0.073(17) 0.005(12) 0.020(14) -0.017(12) C6 0.063(15) 0.055(15) 0.065(15) -0.025(12) -0.035(13) 0.018(12) C14 0.057(15) 0.069(17) 0.053(14) 0.007(12) 0.006(11) -0.027(13) C13 0.059(16) 0.066(18) 0.09(2) -0.008(15) -0.017(15) -0.010(13) F10 0.23(3) 0.119(18) 0.14(2) -0.044(15) -0.11(2) 0.082(19) C26 0.074(19) 0.069(19) 0.08(2) -0.019(15) 0.001(15) -0.021(15) C18 0.10(2) 0.08(2) 0.041(14) -0.026(14) -0.013(14) -0.001(17) C28 0.19(4) 0.08(2) 0.07(2) 0.010(19) -0.03(2) 0.02(3) C16 0.10(2) 0.09(2) 0.034(13) -0.009(13) -0.010(13) 0.005(17) C29 0.044(14) 0.064(18) 0.10(2) -0.023(15) -0.018(14) 0.001(12) F7 0.32(4) 0.26(4) 0.074(14) -0.050(18) -0.09(2) 0.19(3) C22 0.27(6) 0.08(3) 0.13(3) -0.03(2) 0.15(4) -0.07(3) C15 0.07(2) 0.10(3) 0.14(3) 0.00(2) 0.03(2) -0.032(18) C25 0.054(16) 0.08(2) 0.11(3) -0.041(19) 0.010(16) 0.004(15) C27 0.08(2) 0.14(3) 0.11(3) -0.03(2) -0.05(2) 0.02(2) C21 0.61(14) 0.020(17) 0.10(3) 0.009(18) 0.10(6) -0.03(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.274(5) . ? Pt1 P1 2.302(5) . ? Pt1 S1 2.327(5) . ? Pt2 P4 2.274(5) . ? Pt2 P3 2.289(5) . ? Pt2 S2 2.356(5) . ? P6 F7 1.53(2) . ? P6 F10 1.53(2) . ? P6 F8 1.54(2) . ? P6 F9 1.557(16) . ? P6 F11 1.563(16) . ? P6 F12 1.573(17) . ? P5 F4 1.539(19) . ? P5 F5 1.547(15) . ? P5 F2 1.55(2) . ? P5 F1 1.566(16) . ? P5 F3 1.572(17) . ? P5 F6 1.576(16) . ? P2 N2 1.664(19) . ? P2 C4 1.82(2) . ? P2 C3 1.89(3) . ? P3 N3 1.65(2) . ? P3 C17 1.83(2) . ? P3 C18 1.84(3) . ? S2 C22 1.78(4) . ? S2 C24 1.82(2) . ? P4 N4 1.650(16) . ? P4 C20 1.83(2) . ? P4 C19 1.84(2) . ? S1 C6 1.78(2) . ? S1 C8 1.85(2) . ? C20 C31 1.55(3) . ? C20 C32 1.58(3) . ? P1 N1 1.643(16) . ? P1 C1 1.81(2) . ? P1 C2 1.81(2) . ? N4 C23 1.45(3) . ? N1 C5 1.49(3) . ? C5 C6 1.51(3) . ? C4 C15 1.52(4) . ? C4 C16 1.57(3) . ? N3 C21 1.42(5) . ? C19 C29 1.47(3) . ? C19 C30 1.52(3) . ? N2 C7 1.43(3) . ? C1 C9 1.53(3) . ? C1 C10 1.58(3) . ? C23 C24 1.53(4) . ? C11 C2 1.58(4) . ? C3 C14 1.47(4) . ? C3 C13 1.53(4) . ? C2 C12 1.47(3) . ? C7 C8 1.46(4) . ? C17 C25 1.51(4) . ? C17 C26 1.53(3) . ? C18 C28 1.46(4) . ? C18 C27 1.53(4) . ? C22 C21 1.32(6) . ? 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 P2 Pt1 P1 168.4(2) . . ? P2 Pt1 S1 98.1(2) . . ? P1 Pt1 S1 93.43(19) . . ? P4 Pt2 P3 172.09(18) . . ? P4 Pt2 S2 94.56(18) . . ? P3 Pt2 S2 93.18(19) . . ? F7 P6 F10 179(2) . . ? F7 P6 F8 85(2) . . ? F10 P6 F8 95(2) . . ? F7 P6 F9 92.5(16) . . ? F10 P6 F9 86.8(15) . . ? F8 P6 F9 175.8(15) . . ? F7 P6 F11 93.7(17) . . ? F10 P6 F11 87.5(14) . . ? F8 P6 F11 90.5(11) . . ? F9 P6 F11 86.1(9) . . ? F7 P6 F12 88.9(16) . . ? F10 P6 F12 89.9(13) . . ? F8 P6 F12 89.6(11) . . ? F9 P6 F12 93.9(10) . . ? F11 P6 F12 177.4(14) . . ? F4 P5 F5 89.7(11) . . ? F4 P5 F2 176.8(12) . . ? F5 P5 F2 87.2(9) . . ? F4 P5 F1 90.5(13) . . ? F5 P5 F1 88.8(9) . . ? F2 P5 F1 89.3(13) . . ? F4 P5 F3 90.6(14) . . ? F5 P5 F3 91.3(10) . . ? F2 P5 F3 89.6(13) . . ? F1 P5 F3 178.9(13) . . ? F4 P5 F6 89.9(13) . . ? F5 P5 F6 179.1(11) . . ? F2 P5 F6 93.2(12) . . ? F1 P5 F6 90.3(10) . . ? F3 P5 F6 89.6(10) . . ? N2 P2 C4 111.6(11) . . ? N2 P2 C3 100.6(12) . . ? C4 P2 C3 105.3(12) . . ? N2 P2 Pt1 115.5(8) . . ? C4 P2 Pt1 112.1(8) . . ? C3 P2 Pt1 110.8(8) . . ? N3 P3 C17 106.6(11) . . ? N3 P3 C18 106.2(13) . . ? C17 P3 C18 105.3(12) . . ? N3 P3 Pt2 112.5(7) . . ? C17 P3 Pt2 114.8(7) . . ? C18 P3 Pt2 110.8(9) . . ? C22 S2 C24 102.7(18) . . ? C22 S2 Pt2 109.2(12) . . ? C24 S2 Pt2 111.2(8) . . ? N4 P4 C20 104.2(9) . . ? N4 P4 C19 105.2(9) . . ? C20 P4 C19 107.0(11) . . ? N4 P4 Pt2 111.4(7) . . ? C20 P4 Pt2 114.5(8) . . ? C19 P4 Pt2 113.6(7) . . ? C6 S1 C8 101.4(12) . . ? C6 S1 Pt1 111.8(8) . . ? C8 S1 Pt1 107.6(9) . . ? C31 C20 C32 112(2) . . ? C31 C20 P4 109.3(15) . . ? C32 C20 P4 110.0(16) . . ? N1 P1 C1 108.5(10) . . ? N1 P1 C2 105.6(10) . . ? C1 P1 C2 106.2(11) . . ? N1 P1 Pt1 108.9(6) . . ? C1 P1 Pt1 111.7(7) . . ? C2 P1 Pt1 115.5(8) . . ? C23 N4 P4 123.4(14) . . ? C5 N1 P1 121.6(14) . . ? N1 C5 C6 112(2) . . ? C15 C4 C16 114(2) . . ? C15 C4 P2 108(2) . . ? C16 C4 P2 112.9(17) . . ? C21 N3 P3 121(2) . . ? C29 C19 C30 111(2) . . ? C29 C19 P4 110.8(17) . . ? C30 C19 P4 113.2(16) . . ? C7 N2 P2 123.1(18) . . ? C9 C1 C10 106.0(19) . . ? C9 C1 P1 110.5(17) . . ? C10 C1 P1 112.8(15) . . ? N4 C23 C24 113(2) . . ? C23 C24 S2 116.3(14) . . ? C14 C3 C13 113(2) . . ? C14 C3 P2 111.4(17) . . ? C13 C3 P2 111(2) . . ? C12 C2 C11 113(2) . . ? C12 C2 P1 110.6(17) . . ? C11 C2 P1 109.8(17) . . ? N2 C7 C8 118(2) . . ? C7 C8 S1 111(2) . . ? C25 C17 C26 111(2) . . ? C25 C17 P3 108.5(18) . . ? C26 C17 P3 113.0(17) . . ? C5 C6 S1 114.7(16) . . ? C28 C18 C27 109(3) . . ? C28 C18 P3 113(2) . . ? C27 C18 P3 111(2) . . ? C21 C22 S2 121(3) . . ? C22 C21 N3 120(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.793 _refine_diff_density_min -1.084 _refine_diff_density_rms 0.174