# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'James Wilton-Ely' _publ_contact_author_email JAMES.WILTON-ELY@CHEM.OX.AC.UK loop_ _publ_author_name J.Wilton-Ely A.R.Cowley G.Hogarth E.R.Knight N.H.Leung ; Y.H.Lin ; A.L.Thompson D.Watkin data_1 _database_code_depnum_ccdc_archive 'CCDC 703787' #============================================================================== _audit_creation_date 08-09-22 _audit_creation_method CRYSTALS_ver_12.86 _publ_section_exptl_refinement ; The difference map indicated the presence of diffuse electron density believed to be disordered solvent. SQUEEZE was used leaving a void of 213 \%A from which 23 e^-^ were removed. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.003 0.500 1.000 213 23 ' ' _platon_squeeze_details ; The discrete Fourier transform of the void region was treated as contributions to the A and B parts of the calculated structure factors. ; _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 9.27400(10) _cell_length_b 10.6853(2) _cell_length_c 21.3292(4) _cell_angle_alpha 86.3726(6) _cell_angle_beta 79.0768(7) _cell_angle_gamma 88.2028(7) _cell_volume 2070.77(6) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C78 H68 F12 N2 O2 P6 Pt2 S4 # Dc = 1.60 Fooo = 968.00 Mu = 36.63 M = 998.84 # Found Formula = C78 H68 F12 N2 P6 Pt2 S4 # Dc = 1.58 FOOO = 968.00 Mu = 36.60 M = 982.84 _chemical_formula_sum 'C78 H68 F12 N2 P6 Pt2 S4' _chemical_formula_moiety 'C78 H68 N2 P4 Pt2 S4, 2(F6 P)' _chemical_compound_source . _chemical_formula_weight 1965.67 _cell_measurement_reflns_used 8158 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour clear_pale_yellow _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 3.660 # Sheldrick geometric approximatio 0.48 0.48 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.48 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 28885 _reflns_number_total 9333 _diffrn_reflns_av_R_equivalents 0.046 # Number of reflections with Friedels Law is 9333 # Number of reflections without Friedels Law is 9333 # Theoretical number of reflections is about 9508 _diffrn_reflns_theta_min 5.117 _diffrn_reflns_theta_max 27.494 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.569 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -11 _reflns_limit_h_max 12 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 1.86 _oxford_diffrn_Wilson_scale 49.39 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.62 _refine_diff_density_max 1.91 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 9333 _refine_ls_number_restraints 18 _refine_ls_number_parameters 462 _oxford_refine_ls_R_factor_ref 0.0535 _refine_ls_wR_factor_ref 0.0967 _refine_ls_goodness_of_fit_ref 0.9992 _refine_ls_shift/su_max 0.000577 # The values computed from all data _oxford_reflns_number_all 9333 _refine_ls_R_factor_all 0.0535 _refine_ls_wR_factor_all 0.0967 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7901 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_gt 0.0911 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 7.22P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pt1 Pt 0.16422(2) 0.094171(17) 0.220447(9) 0.0214 1.0000 Uani . . . . . . . S2 S 0.10321(14) 0.19811(11) 0.12809(6) 0.0289 1.0000 Uani . . . . . . . C3 C 0.0344(5) 0.0575(5) 0.1130(2) 0.0268 1.0000 Uani . . . . . . . S4 S 0.04585(15) -0.05619(11) 0.17307(6) 0.0295 1.0000 Uani . . . . . . . N5 N -0.0227(5) 0.0382(4) 0.0625(2) 0.0333 1.0000 Uani . . . . . . . C6 C -0.0222(7) 0.1333(5) 0.0099(2) 0.0353 1.0000 Uani . . . . . . . C7 C 0.0749(7) 0.0856(5) -0.0503(3) 0.0370 1.0000 Uani . . . . . . . P8 P 0.24721(14) 0.26660(11) 0.25809(6) 0.0247 1.0000 Uani . . . . . . . C9 C 0.1485(5) 0.2903(4) 0.3389(2) 0.0267 1.0000 Uani . . . . . . . C10 C 0.0002(6) 0.2633(5) 0.3503(3) 0.0345 1.0000 Uani . . . . . . . C11 C -0.0884(6) 0.2820(5) 0.4094(3) 0.0397 1.0000 Uani . . . . . . . C12 C -0.0275(7) 0.3267(6) 0.4577(3) 0.0421 1.0000 Uani . . . . . . . C13 C 0.1213(6) 0.3525(6) 0.4473(3) 0.0402 1.0000 Uani . . . . . . . C14 C 0.2086(6) 0.3342(5) 0.3883(3) 0.0352 1.0000 Uani . . . . . . . C15 C 0.4450(6) 0.2684(5) 0.2508(2) 0.0289 1.0000 Uani . . . . . . . C16 C 0.5305(6) 0.1801(5) 0.2139(3) 0.0355 1.0000 Uani . . . . . . . C17 C 0.6813(6) 0.1807(6) 0.2045(3) 0.0452 1.0000 Uani . . . . . . . C18 C 0.7488(7) 0.2695(7) 0.2320(3) 0.0513 1.0000 Uani . . . . . . . C19 C 0.6683(6) 0.3586(7) 0.2681(3) 0.0496 1.0000 Uani . . . . . . . C20 C 0.5163(6) 0.3596(5) 0.2765(3) 0.0378 1.0000 Uani . . . . . . . C21 C 0.2130(6) 0.4102(5) 0.2115(3) 0.0313 1.0000 Uani . . . . . . . C22 C 0.0976(7) 0.4926(5) 0.2324(3) 0.0429 1.0000 Uani . . . . . . . C23 C 0.0764(8) 0.6001(6) 0.1946(4) 0.0567 1.0000 Uani . . . . . . . C24 C 0.1714(9) 0.6264(6) 0.1369(3) 0.0556 1.0000 Uani . . . . . . . C25 C 0.2833(9) 0.5449(6) 0.1164(3) 0.0542 1.0000 Uani . . . . . . . C26 C 0.3043(7) 0.4360(6) 0.1529(3) 0.0455 1.0000 Uani . . . . . . . P27 P 0.22286(14) -0.04914(12) 0.29641(6) 0.0251 1.0000 Uani . . . . . . . C28 C 0.2807(6) 0.0020(4) 0.3673(2) 0.0273 1.0000 Uani . . . . . . . C29 C 0.4234(6) 0.0435(5) 0.3633(2) 0.0303 1.0000 Uani . . . . . . . C30 C 0.4657(6) 0.0898(5) 0.4162(3) 0.0342 1.0000 Uani . . . . . . . C31 C 0.3669(6) 0.0941(5) 0.4735(3) 0.0371 1.0000 Uani . . . . . . . C32 C 0.2284(7) 0.0505(6) 0.4784(3) 0.0464 1.0000 Uani . . . . . . . C33 C 0.1837(6) 0.0052(5) 0.4255(3) 0.0373 1.0000 Uani . . . . . . . C34 C 0.0648(6) -0.1467(5) 0.3273(2) 0.0296 1.0000 Uani . . . . . . . C35 C -0.0743(6) -0.0927(5) 0.3319(3) 0.0355 1.0000 Uani . . . . . . . C36 C -0.1975(7) -0.1622(7) 0.3584(3) 0.0476 1.0000 Uani . . . . . . . C37 C -0.1836(8) -0.2842(7) 0.3801(3) 0.0508 1.0000 Uani . . . . . . . C38 C -0.0460(8) -0.3395(6) 0.3756(3) 0.0511 1.0000 Uani . . . . . . . C39 C 0.0789(7) -0.2704(5) 0.3494(3) 0.0400 1.0000 Uani . . . . . . . C40 C 0.3718(6) -0.1522(5) 0.2619(3) 0.0318 1.0000 Uani . . . . . . . C41 C 0.4174(6) -0.1533(5) 0.1966(3) 0.0349 1.0000 Uani . . . . . . . C42 C 0.5336(7) -0.2312(6) 0.1702(3) 0.0504 1.0000 Uani . . . . . . . C43 C 0.6041(7) -0.3087(6) 0.2096(4) 0.0562 1.0000 Uani . . . . . . . C44 C 0.5585(7) -0.3077(6) 0.2751(3) 0.0509 1.0000 Uani . . . . . . . C45 C 0.4469(6) -0.2303(5) 0.3016(3) 0.0378 1.0000 Uani . . . . . . . P46 P 0.5000 0.5000 0.5000 0.0446 1.0000 Uani S . . . . . . F47 F 0.6679(5) 0.4819(5) 0.4768(3) 0.1111 1.0000 Uani . . . . . . . F48 F 0.4682(6) 0.3604(4) 0.4949(4) 0.1301 1.0000 Uani . . . . . . . F49 F 0.4836(11) 0.5258(10) 0.4299(4) 0.1842 1.0000 Uani . . . . . . . P50 P 0.5037(4) 0.0292(3) 0.00068(19) 0.0500(9) 0.5000 Uiso D . . . . . . F51 F 0.4181(8) 0.1591(6) -0.0060(4) 0.0809(12) 0.5000 Uiso D . . . . . . F52 F 0.5896(8) -0.1009(6) 0.0073(4) 0.0809(12) 0.5000 Uiso D . . . . . . F53 F 0.5522(9) 0.0720(7) 0.0630(3) 0.0809(12) 0.5000 Uiso D . . . . . . F54 F 0.4540(9) -0.0118(7) -0.0622(3) 0.0809(12) 0.5000 Uiso D . . . . . . F55 F 0.6468(7) 0.0885(7) -0.0417(4) 0.0809(12) 0.5000 Uiso D . . . . . . F56 F 0.3584(7) -0.0282(7) 0.0434(4) 0.0809(12) 0.5000 Uiso D . . . . . . H61 H 0.0143 0.2115 0.0216 0.0438 1.0000 Uiso R . . . . . . H62 H -0.1221 0.1475 0.0028 0.0440 1.0000 Uiso R . . . . . . H71 H 0.0692 0.1442 -0.0869 0.0441 1.0000 Uiso R . . . . . . H72 H 0.1769 0.0772 -0.0442 0.0440 1.0000 Uiso R . . . . . . H101 H -0.0397 0.2317 0.3176 0.0418 1.0000 Uiso R . . . . . . H111 H -0.1882 0.2643 0.4165 0.0471 1.0000 Uiso R . . . . . . H121 H -0.0857 0.3397 0.4976 0.0490 1.0000 Uiso R . . . . . . H131 H 0.1631 0.3805 0.4802 0.0480 1.0000 Uiso R . . . . . . H141 H 0.3085 0.3518 0.3816 0.0412 1.0000 Uiso R . . . . . . H161 H 0.4847 0.1203 0.1950 0.0418 1.0000 Uiso R . . . . . . H171 H 0.7362 0.1210 0.1799 0.0530 1.0000 Uiso R . . . . . . H181 H 0.8513 0.2698 0.2254 0.0600 1.0000 Uiso R . . . . . . H191 H 0.7151 0.4185 0.2867 0.0612 1.0000 Uiso R . . . . . . H201 H 0.4613 0.4219 0.2994 0.0440 1.0000 Uiso R . . . . . . H221 H 0.0347 0.4761 0.2717 0.0510 1.0000 Uiso R . . . . . . H231 H -0.0022 0.6550 0.2084 0.0691 1.0000 Uiso R . . . . . . H241 H 0.1579 0.6995 0.1121 0.0690 1.0000 Uiso R . . . . . . H251 H 0.3463 0.5624 0.0776 0.0620 1.0000 Uiso R . . . . . . H261 H 0.3799 0.3801 0.1387 0.0559 1.0000 Uiso R . . . . . . H291 H 0.4906 0.0405 0.3252 0.0378 1.0000 Uiso R . . . . . . H301 H 0.5614 0.1182 0.4129 0.0431 1.0000 Uiso R . . . . . . H311 H 0.3952 0.1265 0.5089 0.0462 1.0000 Uiso R . . . . . . H321 H 0.1632 0.0506 0.5172 0.0540 1.0000 Uiso R . . . . . . H331 H 0.0880 -0.0232 0.4295 0.0461 1.0000 Uiso R . . . . . . H351 H -0.0848 -0.0093 0.3171 0.0439 1.0000 Uiso R . . . . . . H361 H -0.2910 -0.1253 0.3619 0.0571 1.0000 Uiso R . . . . . . H371 H -0.2665 -0.3303 0.3982 0.0640 1.0000 Uiso R . . . . . . H381 H -0.0353 -0.4231 0.3899 0.0622 1.0000 Uiso R . . . . . . H391 H 0.1722 -0.3080 0.3464 0.0481 1.0000 Uiso R . . . . . . H411 H 0.3710 -0.1005 0.1693 0.0441 1.0000 Uiso R . . . . . . H421 H 0.5625 -0.2310 0.1263 0.0630 1.0000 Uiso R . . . . . . H431 H 0.6816 -0.3607 0.1929 0.0709 1.0000 Uiso R . . . . . . H441 H 0.6036 -0.3616 0.3018 0.0630 1.0000 Uiso R . . . . . . H451 H 0.4206 -0.2289 0.3458 0.0489 1.0000 Uiso 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 0.02505(11) 0.02284(10) 0.01790(10) -0.00306(6) -0.00731(7) 0.00080(7) S2 0.0384(7) 0.0268(6) 0.0237(6) -0.0020(5) -0.0116(5) 0.0024(5) C3 0.027(2) 0.031(3) 0.023(2) -0.0056(19) -0.007(2) 0.0057(19) S4 0.0404(7) 0.0274(6) 0.0238(6) -0.0024(5) -0.0135(5) -0.0031(5) N5 0.046(3) 0.030(2) 0.028(2) -0.0038(18) -0.015(2) 0.0020(19) C6 0.053(3) 0.029(3) 0.029(3) -0.004(2) -0.020(3) 0.004(2) C7 0.050(3) 0.038(3) 0.027(3) -0.002(2) -0.016(2) -0.008(2) P8 0.0269(6) 0.0250(6) 0.0238(6) -0.0051(5) -0.0075(5) 0.0006(5) C9 0.028(3) 0.027(2) 0.025(2) -0.0004(19) -0.005(2) 0.0043(19) C10 0.031(3) 0.040(3) 0.034(3) -0.013(2) -0.006(2) 0.002(2) C11 0.037(3) 0.043(3) 0.038(3) -0.011(2) -0.004(3) -0.002(2) C12 0.052(4) 0.050(3) 0.023(3) -0.010(2) -0.002(3) 0.006(3) C13 0.044(3) 0.048(3) 0.032(3) -0.012(2) -0.013(3) 0.004(3) C14 0.036(3) 0.035(3) 0.037(3) -0.008(2) -0.012(2) 0.004(2) C15 0.031(3) 0.029(3) 0.027(3) 0.002(2) -0.006(2) 0.001(2) C16 0.037(3) 0.037(3) 0.031(3) -0.005(2) -0.004(2) 0.000(2) C17 0.037(3) 0.059(4) 0.037(3) -0.006(3) 0.000(3) 0.010(3) C18 0.029(3) 0.081(5) 0.046(4) -0.011(3) -0.011(3) 0.002(3) C19 0.032(3) 0.066(4) 0.055(4) -0.016(3) -0.013(3) -0.005(3) C20 0.035(3) 0.041(3) 0.038(3) -0.007(2) -0.007(2) -0.002(2) C21 0.035(3) 0.026(3) 0.036(3) -0.006(2) -0.013(2) 0.003(2) C22 0.050(4) 0.034(3) 0.047(4) -0.002(3) -0.017(3) 0.007(3) C23 0.072(5) 0.035(3) 0.067(5) -0.004(3) -0.025(4) 0.016(3) C24 0.089(5) 0.031(3) 0.053(4) 0.003(3) -0.031(4) 0.003(3) C25 0.081(5) 0.042(4) 0.039(4) 0.009(3) -0.013(3) 0.000(3) C26 0.058(4) 0.041(3) 0.034(3) 0.004(2) -0.001(3) 0.006(3) P27 0.0288(6) 0.0263(6) 0.0216(6) -0.0013(5) -0.0088(5) -0.0004(5) C28 0.034(3) 0.027(2) 0.025(3) -0.0027(19) -0.014(2) 0.002(2) C29 0.035(3) 0.030(3) 0.027(3) -0.001(2) -0.010(2) 0.001(2) C30 0.036(3) 0.033(3) 0.039(3) -0.002(2) -0.021(2) -0.003(2) C31 0.050(3) 0.038(3) 0.029(3) -0.005(2) -0.019(3) -0.002(2) C32 0.057(4) 0.060(4) 0.025(3) -0.010(3) -0.012(3) -0.001(3) C33 0.038(3) 0.047(3) 0.029(3) -0.004(2) -0.010(2) -0.006(2) C34 0.038(3) 0.033(3) 0.020(2) -0.003(2) -0.009(2) -0.010(2) C35 0.037(3) 0.041(3) 0.030(3) -0.006(2) -0.008(2) -0.009(2) C36 0.038(3) 0.074(5) 0.031(3) -0.001(3) -0.005(3) -0.021(3) C37 0.052(4) 0.071(4) 0.031(3) 0.003(3) -0.010(3) -0.032(3) C38 0.080(5) 0.044(3) 0.030(3) 0.010(3) -0.012(3) -0.027(3) C39 0.053(4) 0.037(3) 0.032(3) 0.004(2) -0.013(3) -0.005(3) C40 0.037(3) 0.030(3) 0.032(3) -0.006(2) -0.012(2) -0.002(2) C41 0.040(3) 0.036(3) 0.033(3) -0.008(2) -0.013(2) 0.004(2) C42 0.048(4) 0.060(4) 0.045(4) -0.023(3) -0.009(3) 0.017(3) C43 0.049(4) 0.057(4) 0.067(5) -0.028(3) -0.019(3) 0.022(3) C44 0.060(4) 0.040(3) 0.063(4) -0.018(3) -0.035(4) 0.020(3) C45 0.048(3) 0.031(3) 0.041(3) -0.003(2) -0.023(3) 0.005(2) P46 0.0342(11) 0.0378(11) 0.0584(15) -0.0092(10) 0.0040(10) -0.0100(9) F47 0.048(3) 0.082(3) 0.193(7) -0.010(4) 0.007(3) -0.004(2) F48 0.089(4) 0.044(3) 0.238(8) -0.035(4) 0.029(4) -0.018(3) F49 0.225(9) 0.255(10) 0.088(5) 0.040(6) -0.066(5) -0.122(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.14637(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . S2 . 2.3537(12) yes Pt1 . S4 . 2.3546(12) yes Pt1 . P8 . 2.2676(12) yes Pt1 . P27 . 2.2877(12) yes S2 . C3 . 1.723(5) yes C3 . S4 . 1.725(5) yes C3 . N5 . 1.318(6) yes N5 . C7 2_555 1.477(7) yes N5 . C6 . 1.465(7) yes C6 . C7 . 1.528(8) yes C6 . H61 . 0.976 no C6 . H62 . 0.972 no C7 . H71 . 0.978 no C7 . H72 . 0.980 no P8 . C9 . 1.820(5) yes P8 . C15 . 1.812(5) yes P8 . C21 . 1.827(5) yes C9 . C10 . 1.387(7) yes C9 . C14 . 1.395(7) yes C10 . C11 . 1.390(8) yes C10 . H101 . 0.934 no C11 . C12 . 1.382(8) yes C11 . H111 . 0.933 no C12 . C13 . 1.389(8) yes C12 . H121 . 0.932 no C13 . C14 . 1.382(8) yes C13 . H131 . 0.932 no C14 . H141 . 0.933 no C15 . C16 . 1.397(7) yes C15 . C20 . 1.390(7) yes C16 . C17 . 1.375(8) yes C16 . H161 . 0.930 no C17 . C18 . 1.373(9) yes C17 . H171 . 0.929 no C18 . C19 . 1.373(9) yes C18 . H181 . 0.934 no C19 . C20 . 1.387(8) yes C19 . H191 . 0.934 no C20 . H201 . 0.931 no C21 . C22 . 1.389(8) yes C21 . C26 . 1.387(8) yes C22 . C23 . 1.391(8) yes C22 . H221 . 0.936 no C23 . C24 . 1.389(10) yes C23 . H231 . 0.936 no C24 . C25 . 1.358(10) yes C24 . H241 . 0.934 no C25 . C26 . 1.389(8) yes C25 . H251 . 0.930 no C26 . H261 . 0.926 no P27 . C28 . 1.818(5) yes P27 . C34 . 1.820(5) yes P27 . C40 . 1.812(5) yes C28 . C29 . 1.394(7) yes C28 . C33 . 1.389(7) yes C29 . C30 . 1.386(7) yes C29 . H291 . 0.928 no C30 . C31 . 1.384(8) yes C30 . H301 . 0.936 no C31 . C32 . 1.364(8) yes C31 . H311 . 0.935 no C32 . C33 . 1.391(7) yes C32 . H321 . 0.928 no C33 . H331 . 0.934 no C34 . C35 . 1.384(8) yes C34 . C39 . 1.386(7) yes C35 . C36 . 1.390(8) yes C35 . H351 . 0.935 no C36 . C37 . 1.367(9) yes C36 . H361 . 0.933 no C37 . C38 . 1.378(10) yes C37 . H371 . 0.932 no C38 . C39 . 1.399(8) yes C38 . H381 . 0.933 no C39 . H391 . 0.935 no C40 . C41 . 1.377(7) yes C40 . C45 . 1.413(7) yes C41 . C42 . 1.394(8) yes C41 . H411 . 0.938 no C42 . C43 . 1.380(9) yes C42 . H421 . 0.925 no C43 . C44 . 1.382(10) yes C43 . H431 . 0.924 no C44 . C45 . 1.363(8) yes C44 . H441 . 0.931 no C45 . H451 . 0.930 no P46 . F47 2_666 1.552(5) yes P46 . F48 2_666 1.544(4) yes P46 . F49 2_666 1.539(7) yes P46 . F47 . 1.552(5) yes P46 . F48 . 1.544(4) yes P46 . F49 . 1.539(7) yes P50 . F51 . 1.589(6) yes P50 . F52 . 1.592(6) yes P50 . F53 . 1.579(6) yes P50 . F54 . 1.588(6) yes P50 . F55 . 1.583(6) yes P50 . F56 . 1.593(6) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S2 . Pt1 . S4 . 74.67(4) yes S2 . Pt1 . P8 . 95.63(4) yes S4 . Pt1 . P8 . 168.52(4) yes S2 . Pt1 . P27 . 166.05(4) yes S4 . Pt1 . P27 . 92.73(4) yes P8 . Pt1 . P27 . 97.50(4) yes Pt1 . S2 . C3 . 86.72(17) yes S2 . C3 . S4 . 111.8(3) yes S2 . C3 . N5 . 124.7(4) yes S4 . C3 . N5 . 123.4(4) yes C3 . S4 . Pt1 . 86.65(16) yes C7 2_555 N5 . C3 . 122.7(4) yes C7 2_555 N5 . C6 . 114.3(4) yes C3 . N5 . C6 . 122.5(4) yes N5 . C6 . C7 . 108.6(4) yes N5 . C6 . H61 . 109.0 no C7 . C6 . H61 . 111.2 no N5 . C6 . H62 . 109.2 no C7 . C6 . H62 . 109.9 no H61 . C6 . H62 . 108.9 no C6 . C7 . N5 2_555 108.9(4) yes C6 . C7 . H71 . 109.9 no N5 2_555 C7 . H71 . 109.3 no C6 . C7 . H72 . 109.9 no N5 2_555 C7 . H72 . 109.3 no H71 . C7 . H72 . 109.5 no Pt1 . P8 . C9 . 110.20(16) yes Pt1 . P8 . C15 . 113.96(17) yes C9 . P8 . C15 . 113.3(2) yes Pt1 . P8 . C21 . 112.31(16) yes C9 . P8 . C21 . 105.0(2) yes C15 . P8 . C21 . 101.5(2) yes P8 . C9 . C10 . 115.4(4) yes P8 . C9 . C14 . 125.8(4) yes C10 . C9 . C14 . 118.7(5) yes C9 . C10 . C11 . 121.0(5) yes C9 . C10 . H101 . 118.9 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 119.5(5) yes C10 . C11 . H111 . 120.3 no C12 . C11 . H111 . 120.1 no C11 . C12 . C13 . 120.1(5) yes C11 . C12 . H121 . 120.4 no C13 . C12 . H121 . 119.4 no C12 . C13 . C14 . 120.0(5) yes C12 . C13 . H131 . 120.2 no C14 . C13 . H131 . 119.7 no C9 . C14 . C13 . 120.6(5) yes C9 . C14 . H141 . 119.8 no C13 . C14 . H141 . 119.6 no P8 . C15 . C16 . 118.7(4) yes P8 . C15 . C20 . 122.8(4) yes C16 . C15 . C20 . 118.3(5) yes C15 . C16 . C17 . 121.1(5) yes C15 . C16 . H161 . 119.5 no C17 . C16 . H161 . 119.4 no C16 . C17 . C18 . 119.4(6) yes C16 . C17 . H171 . 119.8 no C18 . C17 . H171 . 120.7 no C17 . C18 . C19 . 121.1(6) yes C17 . C18 . H181 . 119.1 no C19 . C18 . H181 . 119.8 no C18 . C19 . C20 . 119.6(6) yes C18 . C19 . H191 . 120.5 no C20 . C19 . H191 . 119.9 no C15 . C20 . C19 . 120.5(5) yes C15 . C20 . H201 . 119.6 no C19 . C20 . H201 . 119.9 no P8 . C21 . C22 . 122.1(4) yes P8 . C21 . C26 . 118.5(4) yes C22 . C21 . C26 . 119.3(5) yes C21 . C22 . C23 . 119.5(6) yes C21 . C22 . H221 . 120.2 no C23 . C22 . H221 . 120.3 no C22 . C23 . C24 . 120.4(6) yes C22 . C23 . H231 . 119.5 no C24 . C23 . H231 . 120.1 no C23 . C24 . C25 . 119.8(6) yes C23 . C24 . H241 . 120.1 no C25 . C24 . H241 . 120.0 no C24 . C25 . C26 . 120.5(7) yes C24 . C25 . H251 . 119.7 no C26 . C25 . H251 . 119.9 no C25 . C26 . C21 . 120.4(6) yes C25 . C26 . H261 . 120.4 no C21 . C26 . H261 . 119.2 no Pt1 . P27 . C28 . 120.63(16) yes Pt1 . P27 . C34 . 109.17(17) yes C28 . P27 . C34 . 104.5(2) yes Pt1 . P27 . C40 . 110.70(18) yes C28 . P27 . C40 . 103.7(2) yes C34 . P27 . C40 . 107.2(2) yes P27 . C28 . C29 . 119.9(4) yes P27 . C28 . C33 . 121.3(4) yes C29 . C28 . C33 . 118.8(4) yes C28 . C29 . C30 . 120.2(5) yes C28 . C29 . H291 . 120.2 no C30 . C29 . H291 . 119.6 no C29 . C30 . C31 . 120.2(5) yes C29 . C30 . H301 . 119.6 no C31 . C30 . H301 . 120.2 no C30 . C31 . C32 . 120.0(5) yes C30 . C31 . H311 . 120.1 no C32 . C31 . H311 . 119.9 no C31 . C32 . C33 . 120.5(6) yes C31 . C32 . H321 . 120.0 no C33 . C32 . H321 . 119.5 no C32 . C33 . C28 . 120.3(5) yes C32 . C33 . H331 . 119.4 no C28 . C33 . H331 . 120.3 no P27 . C34 . C35 . 118.4(4) yes P27 . C34 . C39 . 122.4(4) yes C35 . C34 . C39 . 119.1(5) yes C34 . C35 . C36 . 120.2(6) yes C34 . C35 . H351 . 119.7 no C36 . C35 . H351 . 120.2 no C35 . C36 . C37 . 120.7(6) yes C35 . C36 . H361 . 120.0 no C37 . C36 . H361 . 119.3 no C36 . C37 . C38 . 119.8(6) yes C36 . C37 . H371 . 120.5 no C38 . C37 . H371 . 119.7 no C37 . C38 . C39 . 120.0(6) yes C37 . C38 . H381 . 120.5 no C39 . C38 . H381 . 119.4 no C38 . C39 . C34 . 120.1(6) yes C38 . C39 . H391 . 120.0 no C34 . C39 . H391 . 119.9 no P27 . C40 . C41 . 120.9(4) yes P27 . C40 . C45 . 120.6(4) yes C41 . C40 . C45 . 118.5(5) yes C40 . C41 . C42 . 120.8(5) yes C40 . C41 . H411 . 120.0 no C42 . C41 . H411 . 119.2 no C41 . C42 . C43 . 120.1(6) yes C41 . C42 . H421 . 119.6 no C43 . C42 . H421 . 120.3 no C42 . C43 . C44 . 119.2(6) yes C42 . C43 . H431 . 121.2 no C44 . C43 . H431 . 119.6 no C43 . C44 . C45 . 121.4(6) yes C43 . C44 . H441 . 119.6 no C45 . C44 . H441 . 119.0 no C40 . C45 . C44 . 120.0(6) yes C40 . C45 . H451 . 120.1 no C44 . C45 . H451 . 119.8 no F47 2_666 P46 . F48 2_666 93.5(3) yes F47 2_666 P46 . F49 2_666 88.9(5) yes F48 2_666 P46 . F49 2_666 89.4(5) yes F47 2_666 P46 . F47 . 179.993 yes F48 2_666 P46 . F47 . 86.5(3) yes F49 2_666 P46 . F47 . 91.1(5) yes F47 2_666 P46 . F48 . 86.5(3) yes F48 2_666 P46 . F48 . 179.993 yes F49 2_666 P46 . F48 . 90.6(5) yes F47 . P46 . F48 . 93.5(3) yes F47 2_666 P46 . F49 . 91.1(5) yes F48 2_666 P46 . F49 . 90.6(5) yes F49 2_666 P46 . F49 . 179.993 yes F47 . P46 . F49 . 88.9(5) yes F48 . P46 . F49 . 89.4(5) yes F51 . P50 . F52 . 179.9(5) yes F51 . P50 . F53 . 90.1(4) yes F52 . P50 . F53 . 89.9(4) yes F51 . P50 . F54 . 89.1(4) yes F52 . P50 . F54 . 90.9(4) yes F53 . P50 . F54 . 179.1(4) yes F51 . P50 . F55 . 89.7(4) yes F52 . P50 . F55 . 90.2(4) yes F53 . P50 . F55 . 90.0(4) yes F54 . P50 . F55 . 89.9(4) yes F51 . P50 . F56 . 89.3(4) yes F52 . P50 . F56 . 90.8(4) yes F53 . P50 . F56 . 89.8(4) yes F54 . P50 . F56 . 90.3(4) yes F55 . P50 . F56 . 179.0(4) yes _chemical_name_common . #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 703788' #============================================================================== _audit_creation_date 07-03-02 _audit_creation_method CRYSTALS_ver_12.84 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 10.9130(2) _cell_length_b 10.7573(2) _cell_length_c 21.0009(5) _cell_angle_alpha 90 _cell_angle_beta 91.3055(7) _cell_angle_gamma 90 _cell_volume 2464.75(9) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C28 H68 F12 N2 P4 Pt2 S4 # Dc = 1.76 Fooo = 1360.00 Mu = 60.36 M = 651.59 # Found Formula = C30 H68 F12 N2 P6 Pt2 S4 # Dc = 1.87 FOOO = 1360.00 Mu = 61.05 M = 694.57 _chemical_formula_sum 'C30 H68 F12 N2 P6 Pt2 S4' _chemical_formula_moiety 'C30 H68 F12 N2 P6 Pt2 S4' _chemical_compound_source . _chemical_formula_weight 1389.15 _cell_measurement_reflns_used 5026 _cell_measurement_theta_min 5 _cell_measurement_theta_max 29 _cell_measurement_temperature 150 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_min 0.13 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.872 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 6.105 # Sheldrick geometric approximatio 0.19 0.45 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_T_max 0.45 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 17146 _reflns_number_total 6229 _diffrn_reflns_av_R_equivalents 0.061 # Number of reflections with Friedels Law is 6229 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6621 _diffrn_reflns_theta_min 5.109 _diffrn_reflns_theta_max 29.109 _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.033 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _oxford_diffrn_Wilson_B_factor 1.48 _oxford_diffrn_Wilson_scale 45.33 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -2.00 _refine_diff_density_max 2.10 _refine_ls_number_reflns 6226 _refine_ls_number_restraints 18 _refine_ls_number_parameters 256 #_refine_ls_R_factor_ref 0.0478 _refine_ls_wR_factor_ref 0.1080 _refine_ls_goodness_of_fit_ref 0.9493 #_reflns_number_all 6226 _refine_ls_R_factor_all 0.0478 _refine_ls_wR_factor_all 0.1080 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5243 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_gt 0.1027 _refine_ls_shift/su_max 0.003418 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 0.56P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pt1 Pt 0.472345(14) 0.536070(14) 0.737081(8) 0.0183 1.0000 Uani . . . . . . . P2 P 1.0000 0.5000 0.5000 0.0276 1.0000 Uani DS U . . . . . F3 F 0.9718(4) 0.6177(3) 0.54413(18) 0.0493 1.0000 Uani D U . . . . . F4 F 0.9436(5) 0.4105(3) 0.5508(2) 0.0845 1.0000 Uani D U . . . . . F5 F 1.1300(4) 0.4835(5) 0.5325(3) 0.0915 1.0000 Uani D U . . . . . P6 P 0.5000 1.0000 0.5000 0.0311 1.0000 Uani DS U . . . . . F7 F 0.5096(4) 0.8549(3) 0.5162(2) 0.0537 1.0000 Uani D U . . . . . F8 F 0.4229(5) 1.0190(3) 0.5621(2) 0.0725 1.0000 Uani D U . . . . . F9 F 0.6225(5) 1.0242(5) 0.5386(3) 0.0838 1.0000 Uani D U . . . . . P10 P 0.56974(11) 0.43723(12) 0.65668(6) 0.0221 1.0000 Uani . . . . . . . C11 C 0.6508(5) 0.2998(5) 0.6872(3) 0.0322 1.0000 Uani . . . . . . . C12 C 0.7348(6) 0.2333(5) 0.6405(3) 0.0467 1.0000 Uani . . . . . . . C13 C 0.4790(5) 0.3794(5) 0.5890(3) 0.0301 1.0000 Uani . . . . . . . C14 C 0.3640(5) 0.3090(6) 0.6074(3) 0.0399 1.0000 Uani . . . . . . . C15 C 0.6872(5) 0.5329(4) 0.6199(3) 0.0324 1.0000 Uani . . . . . . . C16 C 0.7897(5) 0.5688(6) 0.6680(4) 0.0472 1.0000 Uani . . . . . . . P17 P 0.37124(11) 0.68596(11) 0.68044(6) 0.0236 1.0000 Uani . . . . . . . C18 C 0.2209(5) 0.7125(6) 0.7127(3) 0.0442 1.0000 Uani . . . . . . . C19 C 0.1363(6) 0.6022(7) 0.7070(4) 0.0576 1.0000 Uani . . . . . . . C20 C 0.3421(5) 0.6698(5) 0.5952(2) 0.0303 1.0000 Uani . . . . . . . C21 C 0.2500(5) 0.7643(5) 0.5667(3) 0.0347 1.0000 Uani . . . . . . . C22 C 0.4464(6) 0.8358(5) 0.6927(3) 0.0451 1.0000 Uani . . . . . . . S23 S 0.56206(10) 0.41591(10) 0.82078(5) 0.0222 1.0000 Uani . . . . . . . C24 C 0.4947(4) 0.5195(4) 0.8724(2) 0.0199 1.0000 Uani . . . . . . . S25 S 0.39981(12) 0.62213(12) 0.83213(6) 0.0307 1.0000 Uani . . . . . . . N26 N 0.5142(4) 0.5214(4) 0.9342(2) 0.0253 1.0000 Uani . . . . . . . C27 C 0.4649(5) 0.6200(5) 0.9753(2) 0.0306 1.0000 Uani . . . . . . . C28 C 0.4032(5) 0.5664(5) 1.0317(3) 0.0300 1.0000 Uani . . . . . . . C29 C 0.5779(6) 0.8438(6) 0.6775(4) 0.0585 1.0000 Uani . . . . . . . H111 H 0.6980 0.3253 0.7249 0.0373 1.0000 Uiso R . . . . . . H112 H 0.5888 0.2416 0.7000 0.0370 1.0000 Uiso R . . . . . . H121 H 0.7821 0.1709 0.6616 0.0679 1.0000 Uiso R . . . . . . H122 H 0.7887 0.2907 0.6200 0.0680 1.0000 Uiso R . . . . . . H123 H 0.6853 0.1936 0.6082 0.0677 1.0000 Uiso R . . . . . . H131 H 0.4532 0.4504 0.5640 0.0361 1.0000 Uiso R . . . . . . H132 H 0.5278 0.3248 0.5632 0.0361 1.0000 Uiso R . . . . . . H141 H 0.3144 0.2919 0.5706 0.0591 1.0000 Uiso R . . . . . . H142 H 0.3184 0.3575 0.6375 0.0591 1.0000 Uiso R . . . . . . H143 H 0.3869 0.2315 0.6275 0.0591 1.0000 Uiso R . . . . . . H151 H 0.6505 0.6070 0.6026 0.0366 1.0000 Uiso R . . . . . . H152 H 0.7233 0.4852 0.5864 0.0365 1.0000 Uiso R . . . . . . H161 H 0.8357 0.6376 0.6522 0.0692 1.0000 Uiso R . . . . . . H162 H 0.7526 0.5926 0.7070 0.0692 1.0000 Uiso R . . . . . . H163 H 0.8438 0.4997 0.6759 0.0692 1.0000 Uiso R . . . . . . H181 H 0.2310 0.7325 0.7577 0.0510 1.0000 Uiso R . . . . . . H182 H 0.1851 0.7823 0.6898 0.0509 1.0000 Uiso R . . . . . . H191 H 0.0515 0.6284 0.7081 0.0862 1.0000 Uiso R . . . . . . H192 H 0.1531 0.5464 0.7421 0.0863 1.0000 Uiso R . . . . . . H193 H 0.1495 0.5599 0.6681 0.0859 1.0000 Uiso R . . . . . . H201 H 0.4188 0.6803 0.5739 0.0350 1.0000 Uiso R . . . . . . H202 H 0.3124 0.5865 0.5876 0.0349 1.0000 Uiso R . . . . . . H211 H 0.2457 0.7577 0.5208 0.0488 1.0000 Uiso R . . . . . . H212 H 0.2727 0.8472 0.5779 0.0491 1.0000 Uiso R . . . . . . H213 H 0.1687 0.7468 0.5821 0.0492 1.0000 Uiso R . . . . . . H221 H 0.4359 0.8624 0.7362 0.0564 1.0000 Uiso R . . . . . . H222 H 0.4027 0.8932 0.6631 0.0560 1.0000 Uiso R . . . . . . H271 H 0.5321 0.6732 0.9891 0.0383 1.0000 Uiso R . . . . . . H272 H 0.4044 0.6687 0.9514 0.0379 1.0000 Uiso R . . . . . . H281 H 0.3839 0.6344 1.0602 0.0340 1.0000 Uiso R . . . . . . H282 H 0.3268 0.5239 1.0191 0.0341 1.0000 Uiso R . . . . . . H291 H 0.6176 0.9080 0.7024 0.0912 1.0000 Uiso R . . . . . . H292 H 0.6170 0.7650 0.6869 0.0909 1.0000 Uiso R . . . . . . H293 H 0.5859 0.8619 0.6331 0.0910 1.0000 Uiso 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 0.01903(11) 0.02210(12) 0.01372(11) -0.00034(6) -0.00041(7) 0.00181(5) P2 0.0278(9) 0.0259(8) 0.0294(10) -0.0015(7) 0.0069(8) -0.0030(8) F3 0.066(2) 0.0316(13) 0.051(2) -0.0128(13) 0.0193(18) -0.0057(14) F4 0.140(4) 0.0321(14) 0.084(3) 0.0114(18) 0.078(3) 0.005(2) F5 0.057(2) 0.096(3) 0.119(5) -0.036(3) -0.042(2) 0.0243(18) P6 0.0326(10) 0.0267(7) 0.0344(11) -0.0037(8) 0.0070(8) -0.0067(8) F7 0.078(3) 0.0287(10) 0.055(2) 0.0006(13) 0.0214(19) 0.0020(14) F8 0.112(3) 0.0391(18) 0.069(3) -0.0063(19) 0.057(3) -0.001(2) F9 0.065(2) 0.087(3) 0.097(4) 0.005(3) -0.035(2) -0.027(2) P10 0.0231(6) 0.0255(5) 0.0178(6) -0.0024(5) 0.0011(5) 0.0001(4) C11 0.037(3) 0.029(2) 0.031(3) -0.002(2) 0.001(2) 0.010(2) C12 0.055(4) 0.040(3) 0.045(4) -0.008(3) 0.006(3) 0.023(3) C13 0.033(3) 0.033(3) 0.024(3) -0.009(2) 0.003(2) -0.003(2) C14 0.031(3) 0.048(3) 0.041(3) -0.012(3) 0.003(2) -0.009(2) C15 0.033(3) 0.034(3) 0.031(3) -0.006(2) 0.010(2) -0.0026(19) C16 0.030(3) 0.055(3) 0.057(4) -0.009(3) 0.007(3) -0.015(3) P17 0.0247(6) 0.0270(6) 0.0190(6) 0.0025(5) -0.0036(5) 0.0025(4) C18 0.035(3) 0.064(4) 0.035(3) 0.018(3) 0.011(2) 0.025(3) C19 0.030(3) 0.088(5) 0.055(4) 0.031(4) 0.005(3) -0.004(3) C20 0.031(3) 0.038(3) 0.022(3) 0.011(2) -0.005(2) -0.003(2) C21 0.030(3) 0.046(3) 0.027(3) 0.010(2) -0.010(2) -0.002(2) C22 0.062(4) 0.026(3) 0.047(4) -0.001(2) -0.022(3) 0.004(2) S23 0.0246(5) 0.0266(6) 0.0155(5) -0.0021(4) -0.0003(4) 0.0055(4) C24 0.024(2) 0.024(2) 0.011(2) -0.0015(16) 0.0003(17) -0.0012(16) S25 0.0385(7) 0.0374(7) 0.0162(6) 0.0007(5) -0.0001(5) 0.0185(5) N26 0.033(2) 0.028(2) 0.015(2) 0.0004(15) -0.0014(17) 0.0069(16) C27 0.046(3) 0.026(2) 0.020(2) -0.0056(19) -0.004(2) 0.007(2) C28 0.029(3) 0.034(2) 0.026(3) -0.006(2) -0.008(2) 0.013(2) C29 0.060(4) 0.037(3) 0.077(6) 0.007(3) -0.031(4) -0.012(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.15043(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 . P10 . 2.2788(12) yes Pt1 . P17 . 2.2743(12) yes Pt1 . S23 . 2.3750(11) yes Pt1 . C24 . 2.853(5) yes Pt1 . S25 . 2.3538(12) yes P2 . F3 2_766 1.603(3) yes P2 . F4 2_766 1.573(3) yes P2 . F5 2_766 1.571(4) yes P2 . F3 . 1.603(3) yes P2 . F4 . 1.573(3) yes P2 . F5 . 1.571(4) yes P6 . F7 2_676 1.600(3) yes P6 . F8 2_676 1.581(4) yes P6 . F9 2_676 1.569(4) yes P6 . F7 . 1.600(3) yes P6 . F8 . 1.581(4) yes P6 . F9 . 1.569(4) yes P10 . C11 . 1.832(5) yes P10 . C13 . 1.824(5) yes P10 . C15 . 1.829(5) yes C11 . C12 . 1.534(7) yes C11 . H111 . 0.973 no C11 . H112 . 0.964 no C12 . H121 . 0.951 no C12 . H122 . 0.961 no C12 . H123 . 0.959 no C13 . C14 . 1.523(7) yes C13 . H131 . 0.965 no C13 . H132 . 0.967 no C14 . H141 . 0.952 no C14 . H142 . 0.966 no C14 . H143 . 0.966 no C15 . C16 . 1.538(9) yes C15 . H151 . 0.960 no C15 . H152 . 0.962 no C16 . H161 . 0.958 no C16 . H162 . 0.957 no C16 . H163 . 0.962 no P17 . C18 . 1.812(5) yes P17 . C20 . 1.820(5) yes P17 . C22 . 1.825(6) yes C18 . C19 . 1.506(9) yes C18 . H181 . 0.973 no C18 . H182 . 0.968 no C19 . H191 . 0.968 no C19 . H192 . 0.965 no C19 . H193 . 0.949 no C20 . C21 . 1.541(7) yes C20 . H201 . 0.964 no C20 . H202 . 0.964 no C21 . H211 . 0.967 no C21 . H212 . 0.954 no C21 . H213 . 0.969 no C22 . C29 . 1.479(10) yes C22 . H221 . 0.968 no C22 . H222 . 0.990 no S23 . C24 . 1.731(5) yes C24 . S25 . 1.723(5) yes C24 . N26 . 1.309(6) yes N26 . C28 2_667 1.479(6) yes N26 . C27 . 1.478(6) yes C27 . C28 . 1.491(8) yes C27 . H271 . 0.969 no C27 . H272 . 0.974 no C28 . H281 . 0.972 no C28 . H282 . 0.983 no C29 . H291 . 0.964 no C29 . H292 . 0.967 no C29 . H293 . 0.960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P10 . Pt1 . P17 . 99.91(5) yes P10 . Pt1 . S23 . 95.92(4) yes P17 . Pt1 . S23 . 163.71(4) yes P10 . Pt1 . C24 . 132.71(9) yes P17 . Pt1 . C24 . 126.51(10) yes S23 . Pt1 . C24 . 37.26(9) yes P10 . Pt1 . S25 . 169.56(4) yes P17 . Pt1 . S25 . 89.78(4) yes S23 . Pt1 . S25 . 74.18(4) yes C24 . Pt1 . S25 . 37.10(10) yes F3 2_766 P2 . F4 2_766 90.4(2) yes F3 2_766 P2 . F5 2_766 91.2(2) yes F4 2_766 P2 . F5 2_766 90.0(4) yes F3 2_766 P2 . F3 . 179.993 yes F4 2_766 P2 . F3 . 89.6(2) yes F5 2_766 P2 . F3 . 88.8(2) yes F3 2_766 P2 . F4 . 89.6(2) yes F4 2_766 P2 . F4 . 179.993 yes F5 2_766 P2 . F4 . 90.0(4) yes F3 . P2 . F4 . 90.4(2) yes F3 2_766 P2 . F5 . 88.8(2) yes F4 2_766 P2 . F5 . 90.0(4) yes F5 2_766 P2 . F5 . 179.993 yes F3 . P2 . F5 . 91.2(2) yes F4 . P2 . F5 . 90.0(4) yes F7 2_676 P6 . F8 2_676 89.13(19) yes F7 2_676 P6 . F9 2_676 90.1(2) yes F8 2_676 P6 . F9 2_676 90.9(3) yes F7 2_676 P6 . F7 . 179.993 yes F8 2_676 P6 . F7 . 90.87(19) yes F9 2_676 P6 . F7 . 89.9(2) yes F7 2_676 P6 . F8 . 90.87(19) yes F8 2_676 P6 . F8 . 179.993 yes F9 2_676 P6 . F8 . 89.1(3) yes F7 . P6 . F8 . 89.13(19) yes F7 2_676 P6 . F9 . 89.9(2) yes F8 2_676 P6 . F9 . 89.1(3) yes F9 2_676 P6 . F9 . 179.993 yes F7 . P6 . F9 . 90.1(2) yes F8 . P6 . F9 . 90.9(3) yes Pt1 . P10 . C11 . 110.29(18) yes Pt1 . P10 . C13 . 118.86(17) yes C11 . P10 . C13 . 104.3(2) yes Pt1 . P10 . C15 . 113.18(17) yes C11 . P10 . C15 . 105.3(3) yes C13 . P10 . C15 . 103.7(3) yes P10 . C11 . C12 . 116.3(4) yes P10 . C11 . H111 . 107.4 no C12 . C11 . H111 . 109.8 no P10 . C11 . H112 . 106.5 no C12 . C11 . H112 . 108.0 no H111 . C11 . H112 . 108.6 no C11 . C12 . H121 . 110.9 no C11 . C12 . H122 . 111.6 no H121 . C12 . H122 . 109.4 no C11 . C12 . H123 . 109.0 no H121 . C12 . H123 . 107.8 no H122 . C12 . H123 . 108.0 no P10 . C13 . C14 . 114.0(4) yes P10 . C13 . H131 . 107.5 no C14 . C13 . H131 . 107.5 no P10 . C13 . H132 . 110.3 no C14 . C13 . H132 . 108.0 no H131 . C13 . H132 . 109.4 no C13 . C14 . H141 . 110.2 no C13 . C14 . H142 . 109.8 no H141 . C14 . H142 . 110.2 no C13 . C14 . H143 . 109.5 no H141 . C14 . H143 . 109.0 no H142 . C14 . H143 . 108.2 no P10 . C15 . C16 . 111.7(4) yes P10 . C15 . H151 . 109.6 no C16 . C15 . H151 . 109.4 no P10 . C15 . H152 . 108.1 no C16 . C15 . H152 . 108.1 no H151 . C15 . H152 . 109.9 no C15 . C16 . H161 . 110.2 no C15 . C16 . H162 . 108.3 no H161 . C16 . H162 . 109.0 no C15 . C16 . H163 . 110.7 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.2 no Pt1 . P17 . C18 . 110.43(19) yes Pt1 . P17 . C20 . 121.24(17) yes C18 . P17 . C20 . 104.1(3) yes Pt1 . P17 . C22 . 109.97(18) yes C18 . P17 . C22 . 102.5(3) yes C20 . P17 . C22 . 106.9(3) yes P17 . C18 . C19 . 113.9(5) yes P17 . C18 . H181 . 108.3 no C19 . C18 . H181 . 107.9 no P17 . C18 . H182 . 107.1 no C19 . C18 . H182 . 109.4 no H181 . C18 . H182 . 110.2 no C18 . C19 . H191 . 110.7 no C18 . C19 . H192 . 108.9 no H191 . C19 . H192 . 109.2 no C18 . C19 . H193 . 109.9 no H191 . C19 . H193 . 108.8 no H192 . C19 . H193 . 109.2 no P17 . C20 . C21 . 114.6(4) yes P17 . C20 . H201 . 108.1 no C21 . C20 . H201 . 108.0 no P17 . C20 . H202 . 107.6 no C21 . C20 . H202 . 109.6 no H201 . C20 . H202 . 109.0 no C20 . C21 . H211 . 110.8 no C20 . C21 . H212 . 111.0 no H211 . C21 . H212 . 108.7 no C20 . C21 . H213 . 109.7 no H211 . C21 . H213 . 107.1 no H212 . C21 . H213 . 109.5 no P17 . C22 . C29 . 117.1(4) yes P17 . C22 . H221 . 109.3 no C29 . C22 . H221 . 108.9 no P17 . C22 . H222 . 104.7 no C29 . C22 . H222 . 106.6 no H221 . C22 . H222 . 110.0 no Pt1 . S23 . C24 . 86.55(16) yes S23 . C24 . Pt1 . 56.19(13) yes S23 . C24 . S25 . 111.3(3) yes Pt1 . C24 . S25 . 55.50(13) yes S23 . C24 . N26 . 124.7(4) yes Pt1 . C24 . N26 . 173.7(3) yes S25 . C24 . N26 . 124.0(3) yes C24 . S25 . Pt1 . 87.40(16) yes C28 2_667 N26 . C24 . 123.6(4) yes C28 2_667 N26 . C27 . 113.6(4) yes C24 . N26 . C27 . 122.5(4) yes N26 . C27 . C28 . 111.4(4) yes N26 . C27 . H271 . 108.3 no C28 . C27 . H271 . 110.1 no N26 . C27 . H272 . 109.6 no C28 . C27 . H272 . 107.8 no H271 . C27 . H272 . 109.6 no C27 . C28 . N26 2_667 110.5(4) yes C27 . C28 . H281 . 107.8 no N26 2_667 C28 . H281 . 108.7 no C27 . C28 . H282 . 111.1 no N26 2_667 C28 . H282 . 109.8 no H281 . C28 . H282 . 108.8 no C22 . C29 . H291 . 110.6 no C22 . C29 . H292 . 109.4 no H291 . C29 . H292 . 109.1 no C22 . C29 . H293 . 109.4 no H291 . C29 . H293 . 109.4 no H292 . C29 . H293 . 109.0 no _chemical_name_common . #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 703789' #============================================================================== _audit_creation_date 08-02-26 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title arc1609 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 10.5409(2) _cell_length_b 18.8334(3) _cell_length_c 21.2790(4) _cell_angle_alpha 90 _cell_angle_beta 97.2552(8) _cell_angle_gamma 90 _cell_volume 4190.51(13) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986 5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C78 H72 B2 Cl8 F8 Fe2 N2 P4 Pd2 S4 # Dc = 1.64 Fooo = 1962.40 Mu = 12.55 M = 1035.66 # Found Formula = C76.60 H69.20 B2 Cl5.20 F8 Fe2 N2 P4 Pd2 S4 # Dc = 1.55 FOOO = 1962.40 Mu = 11.64 M = 976.21 _chemical_formula_sum 'C76.60 H69.20 B2 Cl5.20 F8 Fe2 N2 P4 Pd2 S4' _chemical_formula_moiety 'C76.60 H69.20 B2 Cl5.20 F8 Fe2 N2 P4 Pd2 S4' _chemical_compound_source . _chemical_formula_weight 1952.42 _cell_measurement_reflns_used 45252 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.14 _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1962.400 _exptl_absorpt_coefficient_mu 1.164 # Sheldrick geometric approximatio 0.85 0.91 # No experimental values of Tmin/max available _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.91 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 45252 _reflns_number_total 9827 _diffrn_reflns_av_R_equivalents 0.081 # Number of reflections with Friedels Law is 9827 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9604 _diffrn_reflns_theta_min 5.131 _diffrn_reflns_theta_max 27.486 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.486 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 24 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.55 _refine_diff_density_max 2.09 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 5172 _refine_ls_number_restraints 51 _refine_ls_number_parameters 523 _oxford_refine_ls_R_factor_ref 0.0483 _refine_ls_wR_factor_ref 0.0558 _refine_ls_goodness_of_fit_ref 1.0797 _refine_ls_shift/su_max 0.000885 # The values computed from all data _oxford_reflns_number_all 9537 _refine_ls_R_factor_all 0.0948 _refine_ls_wR_factor_all 0.0959 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5911 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_gt 0.0598 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.445 0.263 0.218 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Pd1 Pd 0.07779(4) 0.58411(2) 0.264701(18) 0.0224 1.0000 Uani . . . . . . . Fe1 Fe 0.14388(8) 0.60826(5) 0.07576(4) 0.0346 1.0000 Uani . . . . . . . S1 S -0.06224(12) 0.51413(8) 0.31680(6) 0.0260 1.0000 Uani . . . . . . . S2 S 0.18952(13) 0.56169(8) 0.36473(6) 0.0281 1.0000 Uani . . . . . . . C1 C 0.0523(5) 0.5198(3) 0.3821(2) 0.0231 1.0000 Uani . . . . . . . N1 N 0.0365(4) 0.4949(2) 0.43865(19) 0.0253 1.0000 Uani . . . . . . . C2 C 0.1353(5) 0.5022(3) 0.4939(2) 0.0278 1.0000 Uani . . . . . . . C3 C 0.0799(5) 0.5410(3) 0.5469(2) 0.0292 1.0000 Uani . . . . . . . P1 P -0.07389(13) 0.60556(8) 0.17869(6) 0.0239 1.0000 Uani . . . . . . . C4 C -0.0324(5) 0.6271(3) 0.1014(2) 0.0287 1.0000 Uani . . . . . . . C5 C 0.0273(6) 0.6923(3) 0.0833(3) 0.0339 1.0000 Uani . . . . . . . C6 C 0.0502(6) 0.6855(4) 0.0190(3) 0.0436 1.0000 Uani . . . . . . . C7 C 0.0075(6) 0.6175(4) -0.0025(2) 0.0404 1.0000 Uani . . . . . . . C8 C -0.0430(5) 0.5810(4) 0.0475(2) 0.0303 1.0000 Uani . . . . . . . C9 C -0.1749(5) 0.6787(3) 0.1967(2) 0.0262 1.0000 Uani . . . . . . . C10 C -0.2434(6) 0.7194(4) 0.1496(3) 0.0364 1.0000 Uani . . . . . . . C11 C -0.3175(7) 0.7762(4) 0.1651(3) 0.0471 1.0000 Uani . . . . . . . C12 C -0.3213(7) 0.7932(4) 0.2275(3) 0.0448 1.0000 Uani . . . . . . . C13 C -0.2567(6) 0.7520(4) 0.2754(3) 0.0411 1.0000 Uani . . . . . . . C14 C -0.1849(6) 0.6954(3) 0.2605(3) 0.0311 1.0000 Uani . . . . . . . C15 C -0.1780(5) 0.5293(3) 0.1607(2) 0.0257 1.0000 Uani . . . . . . . C16 C -0.3091(6) 0.5364(3) 0.1466(3) 0.0344 1.0000 Uani . . . . . . . C17 C -0.3839(6) 0.4756(4) 0.1285(3) 0.0428 1.0000 Uani . . . . . . . C18 C -0.3260(7) 0.4111(4) 0.1239(3) 0.0403 1.0000 Uani . . . . . . . C19 C -0.1961(6) 0.4044(3) 0.1371(3) 0.0338 1.0000 Uani . . . . . . . C20 C -0.1217(6) 0.4626(3) 0.1570(3) 0.0307 1.0000 Uani . . . . . . . P2 P 0.24638(13) 0.64162(8) 0.22837(6) 0.0273 1.0000 Uani . . . . . . . C21 C 0.2753(5) 0.6062(4) 0.1529(3) 0.0344 1.0000 Uani . . . . . . . C22 C 0.2401(6) 0.5351(4) 0.1329(3) 0.0400 1.0000 Uani . . . . . . . C23 C 0.2719(7) 0.5256(5) 0.0708(3) 0.0547 1.0000 Uani . . . . . . . C24 C 0.3248(6) 0.5886(6) 0.0516(3) 0.0598 1.0000 Uani . . . . . . . C25 C 0.3291(6) 0.6394(5) 0.1014(3) 0.0504 1.0000 Uani . . . . . . . C26 C 0.3968(5) 0.6269(4) 0.2787(3) 0.0325 1.0000 Uani . . . . . . . C27 C 0.4787(6) 0.5739(4) 0.2647(3) 0.0409 1.0000 Uani . . . . . . . C28 C 0.5933(6) 0.5630(5) 0.3039(3) 0.0521 1.0000 Uani . . . . . . . C29 C 0.6221(7) 0.6034(5) 0.3569(3) 0.0601 1.0000 Uani . . . . . . . C30 C 0.5409(7) 0.6566(5) 0.3724(3) 0.0501 1.0000 Uani . . . . . . . C31 C 0.4275(6) 0.6679(4) 0.3333(3) 0.0423 1.0000 Uani . . . . . . . C32 C 0.2339(6) 0.7371(3) 0.2220(3) 0.0355 1.0000 Uani . . . . . . . C33 C 0.1228(6) 0.7713(4) 0.2376(3) 0.0442 1.0000 Uani . . . . . . . C34 C 0.1114(9) 0.8454(4) 0.2326(5) 0.0649 1.0000 Uani . . . . . . . C35 C 0.2102(10) 0.8847(5) 0.2127(6) 0.0811 1.0000 Uani . . . . . . . C36 C 0.3202(9) 0.8505(5) 0.1983(6) 0.0756 1.0000 Uani . . . . . . . C37 C 0.3313(7) 0.7781(4) 0.2035(4) 0.0532 1.0000 Uani . . . . . . . B1 B 0.1423(9) 0.2980(5) 0.5160(4) 0.0537 1.0000 Uani . . . . . . . F1 F 0.2483(5) 0.3298(3) 0.4954(3) 0.0733 1.0000 Uani . . . . . . . F2 F 0.0529(5) 0.2829(3) 0.4654(3) 0.0889 1.0000 Uani . . . . . . . F3 F 0.1833(6) 0.2371(3) 0.5477(3) 0.0836 1.0000 Uani . . . . . . . F4 F 0.0903(5) 0.3441(3) 0.5571(2) 0.0643 1.0000 Uani . . . . . . . C38 C 0.171(2) 0.8014(9) 0.4622(8) 0.0907 0.5000 Uani D U . 1 1 . . Cl1 Cl 0.2023(7) 0.8290(3) 0.3892(2) 0.0970 0.5000 Uani D U . 1 1 . . Cl2 Cl 0.1193(4) 0.8729(2) 0.50309(19) 0.0586 0.5000 Uani D U . 1 1 . . C39 C 0.4927(15) 0.6099(10) 0.5323(11) 0.0912 0.5000 Uani D U . 1 2 . . Cl3 Cl 0.3509(7) 0.6595(3) 0.5163(3) 0.0766 0.5000 Uani D U . 1 2 . . Cl4 Cl 0.4745(7) 0.5373(3) 0.5815(3) 0.1095 0.5000 Uani D U . 1 2 . . C40 C 0.632(4) 0.362(2) 0.4760(11) 0.0978 0.3000 Uani D U . 1 3 . . Cl5 Cl 0.7387(8) 0.2912(4) 0.5145(3) 0.0701 0.3000 Uani D U . 1 3 . . Cl6 Cl 0.6016(7) 0.3867(5) 0.3906(6) 0.0940 0.3000 Uani D U . 1 3 . . H21 H 0.2057 0.5301 0.4812 0.0321 1.0000 Uiso . . . . . . . H22 H 0.1669 0.4558 0.5078 0.0321 1.0000 Uiso . . . . . . . H31 H 0.1421 0.5421 0.5844 0.0352 1.0000 Uiso . . . . . . . H32 H 0.0582 0.5896 0.5334 0.0351 1.0000 Uiso . . . . . . . H51 H 0.0447 0.7342 0.1102 0.0398 1.0000 Uiso . . . . . . . H61 H 0.0865 0.7222 -0.0058 0.0518 1.0000 Uiso . . . . . . . H71 H 0.0124 0.5988 -0.0448 0.0469 1.0000 Uiso . . . . . . . H81 H -0.0782 0.5331 0.0454 0.0360 1.0000 Uiso . . . . . . . H101 H -0.2399 0.7086 0.1070 0.0428 1.0000 Uiso . . . . . . . H111 H -0.3644 0.8029 0.1333 0.0549 1.0000 Uiso . . . . . . . H121 H -0.3680 0.8326 0.2382 0.0540 1.0000 Uiso . . . . . . . H131 H -0.2621 0.7631 0.3175 0.0492 1.0000 Uiso . . . . . . . H141 H -0.1422 0.6677 0.2929 0.0371 1.0000 Uiso . . . . . . . H161 H -0.3493 0.5808 0.1488 0.0413 1.0000 Uiso . . . . . . . H171 H -0.4727 0.4795 0.1195 0.0502 1.0000 Uiso . . . . . . . H181 H -0.3758 0.3711 0.1117 0.0478 1.0000 Uiso . . . . . . . H191 H -0.1573 0.3605 0.1332 0.0423 1.0000 Uiso . . . . . . . H201 H -0.0327 0.4576 0.1681 0.0370 1.0000 Uiso . . . . . . . H221 H 0.2016 0.4988 0.1581 0.0468 1.0000 Uiso . . . . . . . H231 H 0.2581 0.4823 0.0452 0.0641 1.0000 Uiso . . . . . . . H241 H 0.3507 0.5977 0.0098 0.0719 1.0000 Uiso . . . . . . . H251 H 0.3605 0.6885 0.1007 0.0599 1.0000 Uiso . . . . . . . H271 H 0.4576 0.5455 0.2290 0.0481 1.0000 Uiso . . . . . . . H281 H 0.6504 0.5275 0.2938 0.0619 1.0000 Uiso . . . . . . . H291 H 0.6981 0.5958 0.3845 0.0698 1.0000 Uiso . . . . . . . H301 H 0.5612 0.6842 0.4086 0.0589 1.0000 Uiso . . . . . . . H311 H 0.3715 0.7036 0.3434 0.0502 1.0000 Uiso . . . . . . . H331 H 0.0577 0.7443 0.2512 0.0530 1.0000 Uiso . . . . . . . H341 H 0.0379 0.8681 0.2429 0.0790 1.0000 Uiso . . . . . . . H351 H 0.2036 0.9342 0.2092 0.0969 1.0000 Uiso . . . . . . . H361 H 0.3865 0.8772 0.1852 0.0919 1.0000 Uiso . . . . . . . H371 H 0.4056 0.7560 0.1940 0.0641 1.0000 Uiso . . . . . . . H381 H 0.2467 0.7808 0.4850 0.1080 0.5000 Uiso . . . 1 1 . . H382 H 0.1036 0.7647 0.4555 0.1080 0.5000 Uiso . . . 1 1 . . H391 H 0.5625 0.6399 0.5533 0.1082 0.5000 Uiso . . . 1 2 . . H392 H 0.5157 0.5920 0.4936 0.1080 0.5000 Uiso . . . 1 2 . . H401 H 0.6502 0.4030 0.4988 0.1341 0.3000 Uiso . . . 1 3 . . H402 H 0.5429 0.3438 0.4847 0.1340 0.3000 Uiso . . . 1 3 . . 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 0.02105(18) 0.0292(2) 0.01688(18) 0.00212(17) 0.00159(13) -0.00033(18) Fe1 0.0244(4) 0.0611(6) 0.0181(4) 0.0037(4) 0.0023(3) 0.0032(4) S1 0.0241(6) 0.0345(8) 0.0186(6) 0.0035(5) -0.0001(5) -0.0028(5) S2 0.0232(6) 0.0404(8) 0.0201(6) 0.0048(5) 0.0005(5) -0.0035(6) C1 0.024(2) 0.026(3) 0.020(2) 0.002(2) 0.0013(19) -0.001(2) N1 0.025(2) 0.033(3) 0.016(2) 0.0066(17) -0.0014(17) -0.0049(19) C2 0.025(3) 0.036(3) 0.020(2) 0.008(2) -0.006(2) -0.005(2) C3 0.032(3) 0.037(3) 0.020(2) 0.009(2) 0.004(2) -0.009(2) P1 0.0244(6) 0.0298(8) 0.0172(6) 0.0023(5) 0.0011(5) 0.0016(5) C4 0.022(3) 0.043(4) 0.020(2) 0.007(2) -0.001(2) 0.006(2) C5 0.029(3) 0.044(4) 0.029(3) 0.008(3) 0.004(2) -0.004(3) C6 0.039(3) 0.068(5) 0.024(3) 0.014(3) 0.002(2) -0.005(3) C7 0.032(3) 0.078(5) 0.011(2) 0.001(3) 0.001(2) 0.008(3) C8 0.022(2) 0.048(3) 0.021(2) 0.000(2) 0.0017(19) 0.002(3) C9 0.022(2) 0.031(3) 0.026(3) 0.002(2) 0.002(2) -0.003(2) C10 0.036(3) 0.044(4) 0.028(3) 0.002(3) -0.001(2) 0.012(3) C11 0.050(4) 0.049(4) 0.040(4) 0.006(3) -0.004(3) 0.014(3) C12 0.045(4) 0.034(4) 0.056(4) -0.001(3) 0.011(3) 0.015(3) C13 0.042(3) 0.041(4) 0.040(3) -0.008(3) 0.006(3) 0.002(3) C14 0.031(3) 0.036(3) 0.026(3) -0.001(2) 0.003(2) -0.001(2) C15 0.032(3) 0.029(3) 0.015(2) 0.004(2) 0.001(2) 0.001(2) C16 0.029(3) 0.039(4) 0.035(3) -0.002(2) 0.001(2) 0.001(3) C17 0.034(3) 0.045(4) 0.047(4) -0.008(3) -0.005(3) -0.007(3) C18 0.051(4) 0.039(4) 0.031(3) -0.005(3) 0.005(3) -0.014(3) C19 0.050(4) 0.028(3) 0.025(3) 0.000(2) 0.014(2) 0.002(3) C20 0.035(3) 0.031(3) 0.027(3) 0.005(2) 0.007(2) -0.005(2) P2 0.0230(7) 0.0379(8) 0.0209(6) 0.0033(6) 0.0021(5) -0.0030(6) C21 0.021(3) 0.060(4) 0.022(3) 0.004(2) 0.002(2) 0.000(3) C22 0.033(3) 0.055(4) 0.031(3) -0.003(3) 0.000(2) 0.009(3) C23 0.039(4) 0.092(6) 0.032(3) -0.013(4) 0.000(3) 0.022(4) C24 0.028(3) 0.129(8) 0.024(3) -0.002(4) 0.004(2) 0.015(4) C25 0.024(3) 0.097(6) 0.029(3) 0.004(3) -0.001(2) -0.006(3) C26 0.019(2) 0.055(4) 0.023(3) 0.006(3) 0.004(2) -0.008(3) C27 0.033(3) 0.060(5) 0.028(3) 0.001(3) 0.000(2) 0.004(3) C28 0.025(3) 0.086(6) 0.043(4) 0.002(4) -0.004(3) 0.004(3) C29 0.031(3) 0.114(7) 0.033(3) 0.008(4) -0.008(3) -0.002(4) C30 0.036(4) 0.079(5) 0.033(3) -0.002(3) -0.004(3) -0.003(4) C31 0.031(3) 0.068(5) 0.026(3) -0.005(3) -0.001(2) -0.008(3) C32 0.032(3) 0.040(4) 0.034(3) 0.005(3) 0.001(2) -0.006(3) C33 0.039(3) 0.041(4) 0.053(4) 0.000(3) 0.007(3) -0.003(3) C34 0.062(5) 0.043(4) 0.091(6) -0.002(4) 0.018(5) 0.006(4) C35 0.083(7) 0.038(5) 0.124(9) 0.020(5) 0.021(6) 0.002(5) C36 0.058(5) 0.050(5) 0.122(8) 0.026(5) 0.024(5) -0.009(4) C37 0.040(4) 0.052(5) 0.069(5) 0.018(4) 0.013(3) -0.004(3) B1 0.064(5) 0.037(5) 0.057(5) -0.004(4) -0.003(4) -0.006(4) F1 0.066(3) 0.074(3) 0.079(3) 0.002(3) 0.009(3) -0.009(3) F2 0.075(3) 0.091(4) 0.091(4) -0.024(3) -0.030(3) 0.002(3) F3 0.102(4) 0.056(3) 0.095(4) 0.021(3) 0.020(3) 0.028(3) F4 0.063(3) 0.066(3) 0.063(3) 0.003(2) 0.006(2) 0.014(2) C38 0.088(10) 0.106(10) 0.078(7) -0.010(6) 0.010(8) 0.021(9) Cl1 0.130(5) 0.099(4) 0.059(3) -0.016(3) 0.000(3) 0.040(4) Cl2 0.047(2) 0.073(3) 0.055(2) 0.0101(19) 0.0019(16) 0.0004(18) C39 0.070(8) 0.073(9) 0.125(11) 0.036(7) -0.010(9) -0.007(6) Cl3 0.074(3) 0.046(3) 0.107(4) -0.003(2) -0.001(3) -0.007(2) Cl4 0.118(5) 0.080(4) 0.113(4) 0.042(3) -0.051(4) -0.022(3) C40 0.057(12) 0.090(13) 0.141(9) -0.005(12) -0.012(12) -0.020(10) Cl5 0.073(4) 0.078(5) 0.058(4) -0.024(3) 0.004(3) -0.014(4) Cl6 0.046(4) 0.079(5) 0.151(8) 0.012(5) -0.012(4) 0.001(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.08517(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 . S1 . 2.3575(13) yes Pd1 . S2 . 2.3372(13) yes Pd1 . C1 . 2.819(5) yes Pd1 . P1 . 2.3088(14) yes Pd1 . P2 . 2.2969(14) yes Fe1 . C4 . 2.033(5) yes Fe1 . C5 . 2.022(6) yes Fe1 . C6 . 2.061(7) yes Fe1 . C7 . 2.066(6) yes Fe1 . C8 . 2.051(5) yes Fe1 . C21 . 2.010(6) yes Fe1 . C22 . 2.024(7) yes Fe1 . C23 . 2.072(8) yes Fe1 . C24 . 2.070(6) yes Fe1 . C25 . 2.046(6) yes S1 . C1 . 1.725(5) yes S2 . C1 . 1.728(5) yes C1 . N1 . 1.322(6) yes N1 . C3 2_566 1.466(7) yes N1 . C2 . 1.476(6) yes C2 . C3 . 1.521(8) yes C2 . H21 . 0.975 no C2 . H22 . 0.967 no C3 . H31 . 0.966 no C3 . H32 . 0.979 no P1 . C4 . 1.800(5) yes P1 . C9 . 1.812(6) yes P1 . C15 . 1.819(6) yes C4 . C5 . 1.453(8) yes C4 . C8 . 1.433(8) yes C5 . C6 . 1.424(8) yes C5 . H51 . 0.978 no C6 . C7 . 1.414(11) yes C6 . H61 . 0.978 no C7 . C8 . 1.425(8) yes C7 . H71 . 0.973 no C8 . H81 . 0.975 no C9 . C10 . 1.389(8) yes C9 . C14 . 1.409(8) yes C10 . C11 . 1.389(9) yes C10 . H101 . 0.936 no C11 . C12 . 1.371(10) yes C11 . H111 . 0.933 no C12 . C13 . 1.387(10) yes C12 . H121 . 0.935 no C13 . C14 . 1.367(9) yes C13 . H131 . 0.928 no C14 . H141 . 0.934 no C15 . C16 . 1.383(8) yes C15 . C20 . 1.395(8) yes C16 . C17 . 1.415(9) yes C16 . H161 . 0.941 no C17 . C18 . 1.369(10) yes C17 . H171 . 0.935 no C18 . C19 . 1.369(9) yes C18 . H181 . 0.936 no C19 . C20 . 1.382(8) yes C19 . H191 . 0.930 no C20 . H201 . 0.943 no P2 . C21 . 1.801(6) yes P2 . C26 . 1.819(6) yes P2 . C32 . 1.806(7) yes C21 . C22 . 1.440(10) yes C21 . C25 . 1.440(9) yes C22 . C23 . 1.414(9) yes C22 . H221 . 0.987 no C23 . C24 . 1.393(13) yes C23 . H231 . 0.982 no C24 . C25 . 1.425(12) yes C24 . H241 . 0.979 no C25 . H251 . 0.982 no C26 . C27 . 1.377(9) yes C26 . C31 . 1.398(9) yes C27 . C28 . 1.393(9) yes C27 . H271 . 0.932 no C28 . C29 . 1.362(11) yes C28 . H281 . 0.942 no C29 . C30 . 1.384(12) yes C29 . H291 . 0.943 no C30 . C31 . 1.383(9) yes C30 . H301 . 0.931 no C31 . H311 . 0.938 no C32 . C33 . 1.413(9) yes C32 . C37 . 1.380(9) yes C33 . C34 . 1.403(11) yes C33 . H331 . 0.929 no C34 . C35 . 1.387(13) yes C34 . H341 . 0.935 no C35 . C36 . 1.394(14) yes C35 . H351 . 0.937 no C36 . C37 . 1.372(12) yes C36 . H361 . 0.932 no C37 . H371 . 0.931 no B1 . F1 . 1.387(11) yes B1 . F2 . 1.367(10) yes B1 . F3 . 1.372(10) yes B1 . F4 . 1.395(10) yes C38 . Cl1 . 1.710(15) yes C38 . Cl2 . 1.726(14) yes C38 . H381 . 0.966 no C38 . H382 . 0.984 no C39 . Cl3 . 1.760(15) yes C39 . Cl4 . 1.747(14) yes C39 . H391 . 0.989 no C39 . H392 . 0.949 no C40 . Cl5 . 1.870(17) yes C40 . Cl6 . 1.862(18) yes C40 . H401 . 0.914 no C40 . H402 . 1.039 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 . Pd1 . S2 . 75.18(5) yes S1 . Pd1 . C1 . 37.60(11) yes S2 . Pd1 . C1 . 37.73(11) yes S1 . Pd1 . P1 . 93.36(5) yes S2 . Pd1 . P1 . 166.52(5) yes C1 . Pd1 . P1 . 130.05(11) yes S1 . Pd1 . P2 . 168.20(5) yes S2 . Pd1 . P2 . 93.98(5) yes C1 . Pd1 . P2 . 131.70(11) yes P1 . Pd1 . P2 . 97.96(5) yes C4 . Fe1 . C5 . 42.0(2) yes C4 . Fe1 . C6 . 69.4(2) yes C5 . Fe1 . C6 . 40.8(2) yes C4 . Fe1 . C7 . 68.6(2) yes C5 . Fe1 . C7 . 68.3(3) yes C6 . Fe1 . C7 . 40.1(3) yes C4 . Fe1 . C8 . 41.1(2) yes C5 . Fe1 . C8 . 69.4(2) yes C6 . Fe1 . C8 . 68.5(3) yes C7 . Fe1 . C8 . 40.5(2) yes C4 . Fe1 . C21 . 110.1(2) yes C5 . Fe1 . C21 . 108.3(3) yes C6 . Fe1 . C21 . 136.2(3) yes C7 . Fe1 . C21 . 176.2(3) yes C8 . Fe1 . C21 . 140.6(2) yes C4 . Fe1 . C22 . 111.3(2) yes C5 . Fe1 . C22 . 138.5(2) yes C6 . Fe1 . C22 . 178.0(3) yes C7 . Fe1 . C22 . 141.9(3) yes C8 . Fe1 . C22 . 113.3(3) yes C4 . Fe1 . C23 . 140.2(3) yes C5 . Fe1 . C23 . 176.7(3) yes C6 . Fe1 . C23 . 140.2(3) yes C7 . Fe1 . C23 . 114.5(3) yes C8 . Fe1 . C23 . 113.9(3) yes C4 . Fe1 . C24 . 178.8(2) yes C5 . Fe1 . C24 . 138.4(3) yes C6 . Fe1 . C24 . 111.7(3) yes C7 . Fe1 . C24 . 112.6(2) yes C8 . Fe1 . C24 . 139.7(3) yes C4 . Fe1 . C25 . 138.8(3) yes C5 . Fe1 . C25 . 108.9(3) yes C6 . Fe1 . C25 . 108.9(3) yes C7 . Fe1 . C25 . 137.3(3) yes C8 . Fe1 . C25 . 177.4(3) yes C21 . Fe1 . C22 . 41.8(3) yes C21 . Fe1 . C23 . 68.9(3) yes C22 . Fe1 . C23 . 40.4(3) yes C21 . Fe1 . C24 . 68.8(2) yes C22 . Fe1 . C24 . 67.6(3) yes C23 . Fe1 . C24 . 39.3(4) yes C21 . Fe1 . C25 . 41.6(2) yes C22 . Fe1 . C25 . 69.3(3) yes C23 . Fe1 . C25 . 67.9(4) yes C24 . Fe1 . C25 . 40.5(3) yes Pd1 . S1 . C1 . 85.88(17) yes Pd1 . S2 . C1 . 86.44(17) yes S2 . C1 . S1 . 112.1(3) yes S2 . C1 . Pd1 . 55.83(14) yes S1 . C1 . Pd1 . 56.52(14) yes S2 . C1 . N1 . 124.1(4) yes S1 . C1 . N1 . 123.8(4) yes Pd1 . C1 . N1 . 175.1(4) yes C3 2_566 N1 . C1 . 123.9(4) yes C3 2_566 N1 . C2 . 113.6(4) yes C1 . N1 . C2 . 122.4(4) yes N1 . C2 . C3 . 109.7(4) yes N1 . C2 . H21 . 108.3 no C3 . C2 . H21 . 108.9 no N1 . C2 . H22 . 109.9 no C3 . C2 . H22 . 110.9 no H21 . C2 . H22 . 109.0 no C2 . C3 . N1 2_566 110.1(5) yes C2 . C3 . H31 . 109.8 no N1 2_566 C3 . H31 . 109.7 no C2 . C3 . H32 . 109.2 no N1 2_566 C3 . H32 . 108.8 no H31 . C3 . H32 . 109.3 no Pd1 . P1 . C4 . 122.65(18) yes Pd1 . P1 . C9 . 109.38(17) yes C4 . P1 . C9 . 103.8(3) yes Pd1 . P1 . C15 . 111.56(17) yes C4 . P1 . C15 . 101.3(3) yes C9 . P1 . C15 . 106.9(2) yes P1 . C4 . Fe1 . 122.8(3) yes P1 . C4 . C5 . 126.6(4) yes Fe1 . C4 . C5 . 68.6(3) yes P1 . C4 . C8 . 126.3(5) yes Fe1 . C4 . C8 . 70.1(3) yes C5 . C4 . C8 . 106.9(5) yes C4 . C5 . Fe1 . 69.4(3) yes C4 . C5 . C6 . 108.1(6) yes Fe1 . C5 . C6 . 71.0(4) yes C4 . C5 . H51 . 125.5 no Fe1 . C5 . H51 . 127.3 no C6 . C5 . H51 . 126.3 no C5 . C6 . Fe1 . 68.2(4) yes C5 . C6 . C7 . 107.9(5) yes Fe1 . C6 . C7 . 70.2(4) yes C5 . C6 . H61 . 125.5 no Fe1 . C6 . H61 . 128.7 no C7 . C6 . H61 . 126.6 no C6 . C7 . Fe1 . 69.8(4) yes C6 . C7 . C8 . 109.1(5) yes Fe1 . C7 . C8 . 69.2(3) yes C6 . C7 . H71 . 125.1 no Fe1 . C7 . H71 . 127.0 no C8 . C7 . H71 . 125.7 no C4 . C8 . C7 . 107.9(6) yes C4 . C8 . Fe1 . 68.8(3) yes C7 . C8 . Fe1 . 70.3(3) yes C4 . C8 . H81 . 126.0 no C7 . C8 . H81 . 126.1 no Fe1 . C8 . H81 . 126.1 no P1 . C9 . C10 . 122.2(4) yes P1 . C9 . C14 . 119.4(4) yes C10 . C9 . C14 . 118.4(5) yes C9 . C10 . C11 . 120.7(6) yes C9 . C10 . H101 . 119.9 no C11 . C10 . H101 . 119.4 no C10 . C11 . C12 . 119.7(6) yes C10 . C11 . H111 . 120.3 no C12 . C11 . H111 . 120.0 no C11 . C12 . C13 . 120.6(6) yes C11 . C12 . H121 . 120.0 no C13 . C12 . H121 . 119.4 no C12 . C13 . C14 . 120.0(6) yes C12 . C13 . H131 . 119.8 no C14 . C13 . H131 . 120.2 no C9 . C14 . C13 . 120.6(5) yes C9 . C14 . H141 . 119.9 no C13 . C14 . H141 . 119.6 no P1 . C15 . C16 . 121.9(4) yes P1 . C15 . C20 . 118.3(4) yes C16 . C15 . C20 . 119.6(5) yes C15 . C16 . C17 . 119.2(6) yes C15 . C16 . H161 . 121.2 no C17 . C16 . H161 . 119.6 no C16 . C17 . C18 . 119.9(6) yes C16 . C17 . H171 . 120.1 no C18 . C17 . H171 . 119.9 no C17 . C18 . C19 . 120.7(6) yes C17 . C18 . H181 . 119.6 no C19 . C18 . H181 . 119.6 no C18 . C19 . C20 . 120.2(6) yes C18 . C19 . H191 . 120.2 no C20 . C19 . H191 . 119.6 no C15 . C20 . C19 . 120.2(5) yes C15 . C20 . H201 . 119.5 no C19 . C20 . H201 . 120.3 no Pd1 . P2 . C21 . 110.5(2) yes Pd1 . P2 . C26 . 112.60(18) yes C21 . P2 . C26 . 103.6(3) yes Pd1 . P2 . C32 . 116.3(2) yes C21 . P2 . C32 . 108.7(3) yes C26 . P2 . C32 . 104.2(3) yes P2 . C21 . Fe1 . 123.0(3) yes P2 . C21 . C22 . 122.8(4) yes Fe1 . C21 . C22 . 69.6(3) yes P2 . C21 . C25 . 130.2(6) yes Fe1 . C21 . C25 . 70.6(3) yes C22 . C21 . C25 . 106.9(6) yes C21 . C22 . Fe1 . 68.6(3) yes C21 . C22 . C23 . 108.1(6) yes Fe1 . C22 . C23 . 71.6(4) yes C21 . C22 . H221 . 126.2 no Fe1 . C22 . H221 . 126.1 no C23 . C22 . H221 . 125.7 no C22 . C23 . Fe1 . 68.0(4) yes C22 . C23 . C24 . 108.6(7) yes Fe1 . C23 . C24 . 70.3(5) yes C22 . C23 . H231 . 125.9 no Fe1 . C23 . H231 . 126.9 no C24 . C23 . H231 . 125.5 no Fe1 . C24 . C23 . 70.4(4) yes Fe1 . C24 . C25 . 68.8(4) yes C23 . C24 . C25 . 109.3(6) yes Fe1 . C24 . H241 . 124.5 no C23 . C24 . H241 . 125.8 no C25 . C24 . H241 . 124.8 no C21 . C25 . C24 . 107.1(7) yes C21 . C25 . Fe1 . 67.9(3) yes C24 . C25 . Fe1 . 70.7(4) yes C21 . C25 . H251 . 125.9 no C24 . C25 . H251 . 126.9 no Fe1 . C25 . H251 . 125.3 no P2 . C26 . C27 . 120.5(4) yes P2 . C26 . C31 . 119.9(5) yes C27 . C26 . C31 . 119.6(5) yes C26 . C27 . C28 . 119.8(6) yes C26 . C27 . H271 . 119.9 no C28 . C27 . H271 . 120.3 no C27 . C28 . C29 . 119.9(7) yes C27 . C28 . H281 . 119.8 no C29 . C28 . H281 . 120.3 no C28 . C29 . C30 . 121.4(6) yes C28 . C29 . H291 . 120.9 no C30 . C29 . H291 . 117.7 no C29 . C30 . C31 . 118.8(7) yes C29 . C30 . H301 . 121.1 no C31 . C30 . H301 . 120.1 no C26 . C31 . C30 . 120.4(7) yes C26 . C31 . H311 . 120.0 no C30 . C31 . H311 . 119.6 no P2 . C32 . C33 . 119.4(5) yes P2 . C32 . C37 . 121.9(5) yes C33 . C32 . C37 . 118.7(6) yes C32 . C33 . C34 . 120.1(7) yes C32 . C33 . H331 . 119.3 no C34 . C33 . H331 . 120.6 no C33 . C34 . C35 . 119.6(8) yes C33 . C34 . H341 . 120.1 no C35 . C34 . H341 . 120.3 no C34 . C35 . C36 . 119.8(8) yes C34 . C35 . H351 . 120.3 no C36 . C35 . H351 . 119.9 no C35 . C36 . C37 . 120.4(8) yes C35 . C36 . H361 . 119.5 no C37 . C36 . H361 . 120.1 no C32 . C37 . C36 . 121.4(7) yes C32 . C37 . H371 . 119.2 no C36 . C37 . H371 . 119.5 no F1 . B1 . F2 . 110.1(8) yes F1 . B1 . F3 . 107.4(7) yes F2 . B1 . F3 . 110.9(7) yes F1 . B1 . F4 . 109.0(7) yes F2 . B1 . F4 . 109.7(7) yes F3 . B1 . F4 . 109.6(7) yes Cl1 . C38 . Cl2 . 109.3(9) yes Cl1 . C38 . H381 . 109.5 no Cl2 . C38 . H381 . 110.6 no Cl1 . C38 . H382 . 107.5 no Cl2 . C38 . H382 . 110.8 no H381 . C38 . H382 . 109.0 no Cl3 . C39 . Cl4 . 112.1(9) yes Cl3 . C39 . H391 . 110.4 no Cl4 . C39 . H391 . 107.9 no Cl3 . C39 . H392 . 108.9 no Cl4 . C39 . H392 . 107.6 no H391 . C39 . H392 . 109.8 no Cl5 . C40 . Cl6 . 128.5(14) yes Cl5 . C40 . H401 . 107.0 no Cl6 . C40 . H401 . 108.0 no Cl5 . C40 . H402 . 100.9 no Cl6 . C40 . H402 . 102.1 no H401 . C40 . H402 . 108.8 no _chemical_name_common . #============================================================================== data_7 _database_code_depnum_ccdc_archive 'CCDC 703790' #============================================================================== _audit_creation_date 07-12-03 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 5643 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 10.5842(2) _cell_length_b 15.6670(2) _cell_length_c 18.2992(3) _cell_angle_alpha 90 _cell_angle_beta 95.6540(7) _cell_angle_gamma 90 _cell_volume 3019.66(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C58 H56 F12 N2 Ni2 P6 S4 # Dc = 1.58 Fooo = 1472.00 Mu = 9.99 M = 720.30 # Found Formula = C58 H56 F12 N2 Ni2 P6 S4 # Dc = 1.58 FOOO = 1472.00 Mu = 9.99 M = 720.30 _chemical_formula_sum 'C58 H56 F12 N2 Ni2 P6 S4' _chemical_formula_moiety 'C58 H56 N2 Ni2 P4 S4, 2(F6 P)' _chemical_compound_source . _chemical_formula_weight 1440.60 _cell_measurement_reflns_used 7096 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour clear_intense_orange _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_max 0.21 _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.999 # Sheldrick geometric approximatio 0.88 0.92 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.92 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 51733 _reflns_number_total 6845 _diffrn_reflns_av_R_equivalents 0.079 # Number of reflections with Friedels Law is 6845 # Number of reflections without Friedels Law is 13663 # Theoretical number of reflections is about 6911 _diffrn_reflns_theta_min 5.150 _diffrn_reflns_theta_max 27.463 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.913 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -13 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 1.98 _oxford_diffrn_Wilson_scale 52.19 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.78 _refine_diff_density_max 0.85 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 6845 _refine_ls_number_restraints 0 _refine_ls_number_parameters 379 _oxford_refine_ls_R_factor_ref 0.0677 _refine_ls_wR_factor_ref 0.1417 _refine_ls_goodness_of_fit_ref 0.9333 _refine_ls_shift/su_max 0.000756 # The values computed from all data _oxford_reflns_number_all 6845 _refine_ls_R_factor_all 0.0677 _refine_ls_wR_factor_all 0.1417 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4471 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_gt 0.0985 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 12.4 18.9 9.55 2.59 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ni1 Ni 0.81930(4) 0.75138(3) 0.56315(2) 0.0227 1.0000 Uani . . . . . . . S2 S 0.81136(8) 0.62828(5) 0.50315(5) 0.0289 1.0000 Uani . . . . . . . C3 C 0.6512(3) 0.6334(2) 0.51259(18) 0.0255 1.0000 Uani . . . . . . . S4 S 0.61344(8) 0.72584(5) 0.55604(5) 0.0287 1.0000 Uani . . . . . . . N5 N 0.5677(3) 0.57479(18) 0.48902(16) 0.0269 1.0000 Uani . . . . . . . C6 C 0.4328(3) 0.5803(2) 0.5013(2) 0.0289 1.0000 Uani . . . . . . . C7 C 0.3976(3) 0.5045(2) 0.5469(2) 0.0308 1.0000 Uani . . . . . . . P8 P 0.80759(8) 0.86798(5) 0.62432(5) 0.0243 1.0000 Uani . . . . . . . C9 C 0.7311(3) 0.9547(2) 0.57068(19) 0.0264 1.0000 Uani . . . . . . . C10 C 0.7011(3) 0.9442(2) 0.4952(2) 0.0315 1.0000 Uani . . . . . . . C11 C 0.6462(3) 1.0117(3) 0.4542(2) 0.0373 1.0000 Uani . . . . . . . C12 C 0.6204(3) 1.0871(3) 0.4870(2) 0.0386 1.0000 Uani . . . . . . . C13 C 0.6506(4) 1.0984(3) 0.5616(2) 0.0397 1.0000 Uani . . . . . . . C14 C 0.7075(4) 1.0326(2) 0.6037(2) 0.0356 1.0000 Uani . . . . . . . C15 C 0.7265(3) 0.8540(2) 0.70600(18) 0.0265 1.0000 Uani . . . . . . . C16 C 0.6012(4) 0.8790(3) 0.7101(2) 0.0375 1.0000 Uani . . . . . . . C17 C 0.5393(4) 0.8555(3) 0.7708(2) 0.0418 1.0000 Uani . . . . . . . C18 C 0.6002(4) 0.8075(3) 0.8264(2) 0.0418 1.0000 Uani . . . . . . . C19 C 0.7242(4) 0.7831(3) 0.8228(2) 0.0471 1.0000 Uani . . . . . . . C20 C 0.7876(4) 0.8067(3) 0.7637(2) 0.0407 1.0000 Uani . . . . . . . C21 C 0.9690(3) 0.9060(2) 0.6526(2) 0.0310 1.0000 Uani . . . . . . . C22 C 1.0481(3) 0.8883(2) 0.5892(2) 0.0308 1.0000 Uani . . . . . . . P23 P 1.01853(8) 0.77727(5) 0.55945(5) 0.0233 1.0000 Uani . . . . . . . C24 C 1.1280(3) 0.7102(2) 0.61696(17) 0.0267 1.0000 Uani . . . . . . . C25 C 1.2555(3) 0.7348(3) 0.63432(19) 0.0316 1.0000 Uani . . . . . . . C26 C 1.3386(3) 0.6805(3) 0.6744(2) 0.0361 1.0000 Uani . . . . . . . C27 C 1.2975(4) 0.6013(3) 0.69743(18) 0.0354 1.0000 Uani . . . . . . . C28 C 1.1722(4) 0.5772(3) 0.6811(2) 0.0362 1.0000 Uani . . . . . . . C29 C 1.0869(3) 0.6313(2) 0.64140(19) 0.0307 1.0000 Uani . . . . . . . C30 C 1.0673(3) 0.7682(2) 0.46746(18) 0.0261 1.0000 Uani . . . . . . . C31 C 1.0228(3) 0.8266(2) 0.41377(19) 0.0309 1.0000 Uani . . . . . . . C32 C 1.0549(3) 0.8182(3) 0.34243(19) 0.0339 1.0000 Uani . . . . . . . C33 C 1.1295(4) 0.7508(3) 0.3241(2) 0.0367 1.0000 Uani . . . . . . . C34 C 1.1707(4) 0.6911(3) 0.3756(2) 0.0411 1.0000 Uani . . . . . . . C35 C 1.1393(4) 0.6991(3) 0.4477(2) 0.0353 1.0000 Uani . . . . . . . P36 P 0.25445(10) 0.46857(7) 0.26030(6) 0.0360 1.0000 Uani . . . . . . . F37 F 0.2601(2) 0.56366(15) 0.22806(14) 0.0463 1.0000 Uani . . . . . . . F38 F 0.1892(3) 0.43747(18) 0.18202(13) 0.0519 1.0000 Uani . . . . . . . F39 F 0.3209(3) 0.50203(18) 0.33751(14) 0.0515 1.0000 Uani . . . . . . . F40 F 0.3913(3) 0.4491(2) 0.23441(16) 0.0621 1.0000 Uani . . . . . . . F41 F 0.1182(2) 0.4902(2) 0.28563(15) 0.0553 1.0000 Uani . . . . . . . F42 F 0.2447(4) 0.37550(18) 0.29250(17) 0.0685 1.0000 Uani . . . . . . . H61 H 0.4181 0.6332 0.5272 0.0339 1.0000 Uiso R . . . . . . H62 H 0.3828 0.5792 0.4536 0.0337 1.0000 Uiso R . . . . . . H71 H 0.4444 0.5069 0.5951 0.0367 1.0000 Uiso R . . . . . . H72 H 0.3066 0.5053 0.5509 0.0368 1.0000 Uiso R . . . . . . H101 H 0.7157 0.8917 0.4721 0.0382 1.0000 Uiso R . . . . . . H111 H 0.6261 1.0046 0.4040 0.0450 1.0000 Uiso R . . . . . . H121 H 0.5826 1.1318 0.4595 0.0461 1.0000 Uiso R . . . . . . H131 H 0.6327 1.1501 0.5838 0.0479 1.0000 Uiso R . . . . . . H141 H 0.7292 1.0391 0.6537 0.0421 1.0000 Uiso R . . . . . . H161 H 0.5598 0.9112 0.6723 0.0446 1.0000 Uiso R . . . . . . H171 H 0.4555 0.8720 0.7735 0.0512 1.0000 Uiso R . . . . . . H181 H 0.5561 0.7904 0.8656 0.0511 1.0000 Uiso R . . . . . . H191 H 0.7659 0.7507 0.8603 0.0566 1.0000 Uiso R . . . . . . H201 H 0.8726 0.7903 0.7615 0.0480 1.0000 Uiso R . . . . . . H211 H 0.9678 0.9663 0.6654 0.0379 1.0000 Uiso R . . . . . . H212 H 1.0025 0.8727 0.6943 0.0371 1.0000 Uiso R . . . . . . H221 H 1.1370 0.8987 0.6040 0.0373 1.0000 Uiso R . . . . . . H222 H 1.0203 0.9246 0.5483 0.0360 1.0000 Uiso R . . . . . . H251 H 1.2834 0.7874 0.6194 0.0385 1.0000 Uiso R . . . . . . H261 H 1.4224 0.6963 0.6863 0.0430 1.0000 Uiso R . . . . . . H271 H 1.3541 0.5654 0.7235 0.0420 1.0000 Uiso R . . . . . . H281 H 1.1449 0.5242 0.6959 0.0443 1.0000 Uiso R . . . . . . H291 H 1.0021 0.6157 0.6311 0.0362 1.0000 Uiso R . . . . . . H311 H 0.9697 0.8719 0.4261 0.0370 1.0000 Uiso R . . . . . . H321 H 1.0256 0.8576 0.3072 0.0402 1.0000 Uiso R . . . . . . H331 H 1.1519 0.7455 0.2764 0.0445 1.0000 Uiso R . . . . . . H341 H 1.2189 0.6450 0.3626 0.0492 1.0000 Uiso R . . . . . . H351 H 1.1661 0.6582 0.4822 0.0424 1.0000 Uiso 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 0.0198(2) 0.0228(2) 0.0256(2) -0.00337(15) 0.00267(14) -0.00160(15) S2 0.0220(4) 0.0276(4) 0.0377(5) -0.0091(3) 0.0061(3) -0.0024(3) C3 0.0239(15) 0.0251(16) 0.0277(16) -0.0017(12) 0.0037(12) -0.0006(12) S4 0.0211(4) 0.0242(4) 0.0411(5) -0.0086(3) 0.0046(3) -0.0013(3) N5 0.0225(13) 0.0250(13) 0.0333(14) -0.0079(11) 0.0031(11) 0.0019(11) C6 0.0216(15) 0.0270(16) 0.0377(18) -0.0101(14) 0.0007(13) 0.0016(12) C7 0.0258(16) 0.0260(16) 0.0411(19) -0.0140(15) 0.0061(14) -0.0037(13) P8 0.0218(4) 0.0253(4) 0.0255(4) -0.0048(3) 0.0008(3) 0.0000(3) C9 0.0205(14) 0.0271(16) 0.0312(16) 0.0000(13) 0.0009(12) -0.0009(12) C10 0.0254(16) 0.0352(19) 0.0343(18) -0.0006(15) 0.0053(13) -0.0013(14) C11 0.0265(17) 0.050(2) 0.0353(19) 0.0124(17) 0.0029(14) 0.0003(16) C12 0.0286(17) 0.037(2) 0.051(2) 0.0216(18) 0.0055(16) 0.0005(15) C13 0.0338(19) 0.0278(18) 0.058(3) -0.0019(17) 0.0074(17) -0.0021(15) C14 0.0356(19) 0.0308(18) 0.039(2) -0.0057(15) -0.0008(15) -0.0002(15) C15 0.0273(15) 0.0267(16) 0.0251(15) -0.0078(13) 0.0008(12) 0.0000(13) C16 0.0328(18) 0.042(2) 0.0372(19) 0.0022(16) 0.0035(15) 0.0029(16) C17 0.0338(19) 0.046(2) 0.047(2) -0.0017(18) 0.0139(16) 0.0077(17) C18 0.049(2) 0.046(2) 0.0316(18) -0.0032(17) 0.0096(16) -0.0013(18) C19 0.055(3) 0.054(3) 0.032(2) 0.0118(18) 0.0042(18) 0.010(2) C20 0.037(2) 0.049(2) 0.0356(19) 0.0005(17) 0.0027(16) 0.0102(17) C21 0.0275(16) 0.0308(18) 0.0338(18) -0.0054(14) -0.0020(13) -0.0030(14) C22 0.0270(16) 0.0276(17) 0.0374(18) -0.0035(14) 0.0009(14) -0.0037(13) P23 0.0200(4) 0.0252(4) 0.0249(4) -0.0008(3) 0.0032(3) -0.0016(3) C24 0.0279(16) 0.0321(17) 0.0204(14) 0.0005(13) 0.0045(12) -0.0021(13) C25 0.0269(16) 0.041(2) 0.0270(16) 0.0027(14) 0.0036(13) -0.0018(14) C26 0.0255(17) 0.053(2) 0.0304(17) -0.0003(16) 0.0034(13) 0.0001(16) C27 0.0357(19) 0.049(2) 0.0217(16) 0.0046(15) 0.0048(13) 0.0144(17) C28 0.044(2) 0.0366(19) 0.0284(17) 0.0032(15) 0.0073(15) 0.0032(16) C29 0.0269(16) 0.0366(19) 0.0287(16) 0.0004(14) 0.0028(13) -0.0028(14) C30 0.0207(14) 0.0324(17) 0.0255(15) 0.0004(13) 0.0040(12) -0.0043(12) C31 0.0286(17) 0.0324(18) 0.0320(17) 0.0037(14) 0.0046(13) -0.0014(14) C32 0.0335(18) 0.040(2) 0.0277(17) 0.0028(15) -0.0004(14) -0.0049(15) C33 0.0326(18) 0.054(2) 0.0235(15) -0.0022(16) 0.0017(13) -0.0084(17) C34 0.042(2) 0.049(2) 0.0328(19) -0.0081(17) 0.0059(16) 0.0122(18) C35 0.0374(19) 0.041(2) 0.0278(17) -0.0017(15) 0.0037(14) 0.0100(16) P36 0.0384(5) 0.0347(5) 0.0329(5) 0.0017(4) -0.0067(4) -0.0015(4) F37 0.0456(13) 0.0399(13) 0.0506(14) 0.0093(11) -0.0096(11) -0.0072(10) F38 0.0605(16) 0.0531(15) 0.0387(13) -0.0034(11) -0.0127(11) -0.0119(12) F39 0.0563(15) 0.0583(16) 0.0363(12) -0.0039(11) -0.0133(11) 0.0031(12) F40 0.0455(15) 0.081(2) 0.0588(17) -0.0108(15) -0.0012(12) 0.0183(14) F41 0.0407(14) 0.0731(19) 0.0525(15) 0.0104(14) 0.0075(11) -0.0019(13) F42 0.104(3) 0.0393(14) 0.0578(17) 0.0109(13) -0.0166(17) -0.0057(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.14209(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . S2 . 2.2167(9) yes Ni1 . S4 . 2.2065(9) yes Ni1 . P8 . 2.1524(9) yes Ni1 . P23 . 2.1549(9) yes S2 . C3 . 1.723(3) yes C3 . S4 . 1.719(3) yes C3 . N5 . 1.317(4) yes N5 . C7 2_666 1.469(4) yes N5 . C6 . 1.470(4) yes C6 . C7 . 1.519(5) yes C6 . H61 . 0.975 no C6 . H62 . 0.975 no C7 . H71 . 0.968 no C7 . H72 . 0.973 no P8 . C9 . 1.819(3) yes P8 . C15 . 1.809(3) yes P8 . C21 . 1.835(3) yes C9 . C10 . 1.397(5) yes C9 . C14 . 1.395(5) yes C10 . C11 . 1.391(5) yes C10 . H101 . 0.944 no C11 . C12 . 1.365(6) yes C11 . H111 . 0.929 no C12 . C13 . 1.383(6) yes C12 . H121 . 0.930 no C13 . C14 . 1.389(6) yes C13 . H131 . 0.933 no C14 . H141 . 0.927 no C15 . C16 . 1.391(5) yes C15 . C20 . 1.396(5) yes C16 . C17 . 1.393(6) yes C16 . H161 . 0.930 no C17 . C18 . 1.374(6) yes C17 . H171 . 0.931 no C18 . C19 . 1.375(6) yes C18 . H181 . 0.932 no C19 . C20 . 1.379(6) yes C19 . H191 . 0.929 no C20 . H201 . 0.940 no C21 . C22 . 1.521(5) yes C21 . H211 . 0.975 no C21 . H212 . 0.962 no C22 . P23 . 1.841(4) yes C22 . H221 . 0.966 no C22 . H222 . 0.963 no P23 . C24 . 1.820(3) yes P23 . C30 . 1.814(3) yes C24 . C25 . 1.410(5) yes C24 . C29 . 1.398(5) yes C25 . C26 . 1.382(5) yes C25 . H251 . 0.925 no C26 . C27 . 1.394(6) yes C26 . H261 . 0.926 no C27 . C28 . 1.383(5) yes C27 . H271 . 0.920 no C28 . C29 . 1.389(5) yes C28 . H281 . 0.928 no C29 . H291 . 0.931 no C30 . C31 . 1.390(5) yes C30 . C35 . 1.392(5) yes C31 . C32 . 1.387(5) yes C31 . H311 . 0.947 no C32 . C33 . 1.379(6) yes C32 . H321 . 0.923 no C33 . C34 . 1.368(6) yes C33 . H331 . 0.930 no C34 . C35 . 1.398(5) yes C34 . H341 . 0.928 no C35 . H351 . 0.924 no P36 . F37 . 1.606(3) yes P36 . F38 . 1.603(2) yes P36 . F39 . 1.603(3) yes P36 . F40 . 1.597(3) yes P36 . F41 . 1.594(3) yes P36 . F42 . 1.580(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S2 . Ni1 . S4 . 79.86(3) yes S2 . Ni1 . P8 . 174.08(4) yes S4 . Ni1 . P8 . 94.44(3) yes S2 . Ni1 . P23 . 97.91(3) yes S4 . Ni1 . P23 . 174.83(4) yes P8 . Ni1 . P23 . 87.89(3) yes Ni1 . S2 . C3 . 84.25(11) yes S2 . C3 . S4 . 111.18(18) yes S2 . C3 . N5 . 124.8(3) yes S4 . C3 . N5 . 124.0(2) yes C3 . S4 . Ni1 . 84.66(11) yes C7 2_666 N5 . C3 . 123.1(3) yes C7 2_666 N5 . C6 . 114.1(3) yes C3 . N5 . C6 . 122.7(3) yes N5 . C6 . C7 . 109.4(3) yes N5 . C6 . H61 . 109.1 no C7 . C6 . H61 . 109.8 no N5 . C6 . H62 . 108.1 no C7 . C6 . H62 . 109.7 no H61 . C6 . H62 . 110.7 no C6 . C7 . N5 2_666 109.3(3) yes C6 . C7 . H71 . 109.8 no N5 2_666 C7 . H71 . 108.2 no C6 . C7 . H72 . 109.2 no N5 2_666 C7 . H72 . 109.7 no H71 . C7 . H72 . 110.6 no Ni1 . P8 . C9 . 113.50(11) yes Ni1 . P8 . C15 . 112.55(11) yes C9 . P8 . C15 . 108.30(16) yes Ni1 . P8 . C21 . 108.81(12) yes C9 . P8 . C21 . 105.19(16) yes C15 . P8 . C21 . 108.11(16) yes P8 . C9 . C10 . 119.4(3) yes P8 . C9 . C14 . 120.6(3) yes C10 . C9 . C14 . 120.0(3) yes C9 . C10 . C11 . 119.1(4) yes C9 . C10 . H101 . 120.9 no C11 . C10 . H101 . 120.0 no C10 . C11 . C12 . 120.8(4) yes C10 . C11 . H111 . 119.0 no C12 . C11 . H111 . 120.2 no C11 . C12 . C13 . 120.6(4) yes C11 . C12 . H121 . 120.5 no C13 . C12 . H121 . 118.9 no C12 . C13 . C14 . 119.9(4) yes C12 . C13 . H131 . 120.2 no C14 . C13 . H131 . 119.9 no C9 . C14 . C13 . 119.7(4) yes C9 . C14 . H141 . 119.2 no C13 . C14 . H141 . 121.1 no P8 . C15 . C16 . 122.9(3) yes P8 . C15 . C20 . 117.8(3) yes C16 . C15 . C20 . 118.8(3) yes C15 . C16 . C17 . 119.6(4) yes C15 . C16 . H161 . 119.6 no C17 . C16 . H161 . 120.9 no C16 . C17 . C18 . 120.8(4) yes C16 . C17 . H171 . 119.6 no C18 . C17 . H171 . 119.5 no C17 . C18 . C19 . 119.8(4) yes C17 . C18 . H181 . 119.5 no C19 . C18 . H181 . 120.6 no C18 . C19 . C20 . 120.3(4) yes C18 . C19 . H191 . 120.2 no C20 . C19 . H191 . 119.5 no C15 . C20 . C19 . 120.7(4) yes C15 . C20 . H201 . 119.1 no C19 . C20 . H201 . 120.2 no P8 . C21 . C22 . 107.1(2) yes P8 . C21 . H211 . 110.4 no C22 . C21 . H211 . 112.5 no P8 . C21 . H212 . 107.9 no C22 . C21 . H212 . 108.5 no H211 . C21 . H212 . 110.3 no C21 . C22 . P23 . 107.9(2) yes C21 . C22 . H221 . 110.5 no P23 . C22 . H221 . 112.0 no C21 . C22 . H222 . 109.6 no P23 . C22 . H222 . 107.3 no H221 . C22 . H222 . 109.4 no C22 . P23 . Ni1 . 107.88(12) yes C22 . P23 . C24 . 107.13(16) yes Ni1 . P23 . C24 . 116.23(11) yes C22 . P23 . C30 . 107.05(16) yes Ni1 . P23 . C30 . 112.54(11) yes C24 . P23 . C30 . 105.54(15) yes P23 . C24 . C25 . 120.8(3) yes P23 . C24 . C29 . 119.7(3) yes C25 . C24 . C29 . 119.4(3) yes C24 . C25 . C26 . 119.7(3) yes C24 . C25 . H251 . 120.3 no C26 . C25 . H251 . 120.0 no C25 . C26 . C27 . 120.5(3) yes C25 . C26 . H261 . 120.3 no C27 . C26 . H261 . 119.2 no C26 . C27 . C28 . 119.9(3) yes C26 . C27 . H271 . 119.6 no C28 . C27 . H271 . 120.4 no C27 . C28 . C29 . 120.4(4) yes C27 . C28 . H281 . 120.0 no C29 . C28 . H281 . 119.6 no C24 . C29 . C28 . 120.0(3) yes C24 . C29 . H291 . 119.4 no C28 . C29 . H291 . 120.6 no P23 . C30 . C31 . 119.8(3) yes P23 . C30 . C35 . 121.0(3) yes C31 . C30 . C35 . 119.0(3) yes C30 . C31 . C32 . 120.3(3) yes C30 . C31 . H311 . 119.5 no C32 . C31 . H311 . 120.1 no C31 . C32 . C33 . 120.0(3) yes C31 . C32 . H321 . 119.8 no C33 . C32 . H321 . 120.2 no C32 . C33 . C34 . 120.5(4) yes C32 . C33 . H331 . 120.1 no C34 . C33 . H331 . 119.4 no C33 . C34 . C35 . 119.9(4) yes C33 . C34 . H341 . 120.2 no C35 . C34 . H341 . 119.9 no C34 . C35 . C30 . 120.1(4) yes C34 . C35 . H351 . 119.9 no C30 . C35 . H351 . 120.0 no F37 . P36 . F38 . 88.97(14) yes F37 . P36 . F39 . 89.50(14) yes F38 . P36 . F39 . 178.40(16) yes F37 . P36 . F40 . 90.02(16) yes F38 . P36 . F40 . 90.01(16) yes F39 . P36 . F40 . 89.52(15) yes F37 . P36 . F41 . 88.68(15) yes F38 . P36 . F41 . 90.14(15) yes F39 . P36 . F41 . 90.30(15) yes F40 . P36 . F41 . 178.69(17) yes F37 . P36 . F42 . 178.29(18) yes F38 . P36 . F42 . 90.83(16) yes F39 . P36 . F42 . 90.71(16) yes F40 . P36 . F42 . 91.7(2) yes F41 . P36 . F42 . 89.63(18) yes _chemical_name_common . #============================================================================== data_8 _database_code_depnum_ccdc_archive 'CCDC 703791' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; . ; _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C74 H64 Fe2 N2 Ni2 P4 S4, 2(F6 P), 4(C H2 Cl2)' _chemical_formula_sum 'C78 H72 Cl8 F12 Fe2 N2 Ni2 P6 S4' _chemical_formula_weight 2092.16 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 10.735(2) _cell_length_b 19.056(4) _cell_length_c 21.662(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.46(3) _cell_angle_gamma 90.00 _cell_volume 4430.0(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16773 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.75 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.252 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.422 _exptl_absorpt_correction_T_max 0.533 _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_special_details ; The data collection nominally covered a hemisphere of reciprocal Space, by a combination of \w and \f scans. ; _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 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 8 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 33360 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 5.03 _diffrn_reflns_theta_max 27.81 _reflns_number_total 9699 _reflns_number_gt 8732 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.1022P)^2^+13.4759P] 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 9699 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1774 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _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 0.13401(4) 0.43247(2) 0.228308(19) 0.01690(13) Uani 1 1 d . . . Fe1 Fe 0.25336(5) 0.41885(3) 0.41067(2) 0.02213(15) Uani 1 1 d . . . S1 S -0.01878(8) 0.49113(5) 0.18122(4) 0.01934(19) Uani 1 1 d . . . S2 S 0.22069(8) 0.45174(5) 0.13524(4) 0.0227(2) Uani 1 1 d . . . P1 P 0.30698(8) 0.38124(5) 0.26060(4) 0.0214(2) Uani 1 1 d . . . P2 P 0.01026(8) 0.41308(5) 0.31147(4) 0.01767(19) Uani 1 1 d . . . N1 N 0.0476(3) 0.50985(17) 0.06008(14) 0.0228(6) Uani 1 1 d . . . C1 C 0.3604(3) 0.4172(2) 0.33268(17) 0.0238(7) Uani 1 1 d . . . C2 C 0.4282(4) 0.3851(2) 0.38317(18) 0.0294(8) Uani 1 1 d . . . H2A H 0.4598 0.3369 0.3847 0.035 Uiso 1 1 calc R . . C3 C 0.4394(4) 0.4364(3) 0.4312(2) 0.0346(9) Uani 1 1 d . . . H3A H 0.4801 0.4286 0.4717 0.042 Uiso 1 1 calc R . . C4 C 0.3825(4) 0.5008(2) 0.4113(2) 0.0348(9) Uani 1 1 d . . . H4A H 0.3778 0.5443 0.4353 0.042 Uiso 1 1 calc R . . C5 C 0.3339(4) 0.4899(2) 0.35083(18) 0.0272(8) Uani 1 1 d . . . H5A H 0.2890 0.5247 0.3255 0.033 Uiso 1 1 calc R . . C6 C 0.0729(3) 0.3986(2) 0.38853(16) 0.0212(7) Uani 1 1 d . . . C7 C 0.1330(3) 0.3349(2) 0.41006(17) 0.0254(7) Uani 1 1 d . . . H7A H 0.1417 0.2911 0.3869 0.030 Uiso 1 1 calc R . . C8 C 0.1727(4) 0.3476(2) 0.47243(18) 0.0311(9) Uani 1 1 d . . . H8A H 0.2186 0.3144 0.4991 0.037 Uiso 1 1 calc R . . C9 C 0.1379(4) 0.4183(3) 0.48928(18) 0.0323(9) Uani 1 1 d . . . H9A H 0.1568 0.4412 0.5289 0.039 Uiso 1 1 calc R . . C10 C 0.0761(3) 0.4497(2) 0.43760(16) 0.0256(8) Uani 1 1 d . . . H10A H 0.0419 0.4973 0.4356 0.031 Uiso 1 1 calc R . . C11 C 0.0785(3) 0.48795(19) 0.11578(16) 0.0204(7) Uani 1 1 d . . . C12 C 0.1346(3) 0.5057(2) 0.00590(16) 0.0258(8) Uani 1 1 d . . . H12A H 0.1508 0.5525 -0.0094 0.031 Uiso 1 1 calc R . . H12B H 0.2133 0.4852 0.0194 0.031 Uiso 1 1 calc R . . C13 C 0.0765(3) 0.4614(2) -0.04538(16) 0.0242(7) Uani 1 1 d . . . H13A H 0.1278 0.4629 -0.0816 0.029 Uiso 1 1 calc R . . H13B H 0.0697 0.4130 -0.0321 0.029 Uiso 1 1 calc R . . C14 C 0.4450(4) 0.3918(2) 0.20909(18) 0.0312(9) Uani 1 1 d . . . C15 C 0.4620(5) 0.3462(3) 0.1582(2) 0.0456(12) Uani 1 1 d . . . H15A H 0.4046 0.3107 0.1498 0.055 Uiso 1 1 calc R . . C16 C 0.5680(6) 0.3549(4) 0.1198(3) 0.0630(18) Uani 1 1 d . . . H16A H 0.5792 0.3238 0.0873 0.076 Uiso 1 1 calc R . . C17 C 0.6524(5) 0.4072(4) 0.1293(3) 0.068(2) Uani 1 1 d . . . H17A H 0.7204 0.4121 0.1040 0.082 Uiso 1 1 calc R . . C18 C 0.6339(5) 0.4538(4) 0.1788(3) 0.0623(18) Uani 1 1 d . . . H18A H 0.6904 0.4901 0.1862 0.075 Uiso 1 1 calc R . . C19 C 0.5289(4) 0.4461(3) 0.2182(2) 0.0448(12) Uani 1 1 d . . . H19A H 0.5174 0.4779 0.2501 0.054 Uiso 1 1 calc R . . C20 C 0.2907(4) 0.2857(2) 0.26754(17) 0.0267(8) Uani 1 1 d . . . C21 C 0.1808(4) 0.2538(2) 0.2472(2) 0.0333(9) Uani 1 1 d . . . H21A H 0.1167 0.2810 0.2302 0.040 Uiso 1 1 calc R . . C22 C 0.1654(5) 0.1805(3) 0.2522(3) 0.0459(11) Uani 1 1 d . . . H22A H 0.0913 0.1599 0.2385 0.055 Uiso 1 1 calc R . . C23 C 0.2588(6) 0.1394(3) 0.2772(2) 0.0500(13) Uani 1 1 d . . . H23A H 0.2473 0.0913 0.2817 0.060 Uiso 1 1 calc R . . C24 C 0.3703(6) 0.1704(3) 0.2955(3) 0.0534(14) Uani 1 1 d . . . H24A H 0.4347 0.1426 0.3114 0.064 Uiso 1 1 calc R . . C25 C 0.3878(5) 0.2438(3) 0.2905(2) 0.0420(11) Uani 1 1 d . . . H25A H 0.4636 0.2639 0.3024 0.050 Uiso 1 1 calc R . . C26 C -0.0956(3) 0.4880(2) 0.32560(16) 0.0212(7) Uani 1 1 d . . . C27 C -0.0458(4) 0.5566(2) 0.32634(17) 0.0257(7) Uani 1 1 d . . . H27A H 0.0374 0.5638 0.3172 0.031 Uiso 1 1 calc R . . C28 C -0.1222(4) 0.6143(2) 0.3410(2) 0.0322(9) Uani 1 1 d . . . H28A H -0.0888 0.6593 0.3420 0.039 Uiso 1 1 calc R . . C29 C -0.2500(4) 0.6038(3) 0.3540(2) 0.0367(10) Uani 1 1 d . . . H29A H -0.3003 0.6418 0.3635 0.044 Uiso 1 1 calc R . . C30 C -0.2991(4) 0.5366(3) 0.3526(2) 0.0379(10) Uani 1 1 d . . . H30A H -0.3828 0.5298 0.3609 0.045 Uiso 1 1 calc R . . C31 C -0.2237(4) 0.4784(2) 0.3387(2) 0.0309(8) Uani 1 1 d . . . H31A H -0.2579 0.4335 0.3381 0.037 Uiso 1 1 calc R . . C32 C -0.0947(3) 0.3375(2) 0.30047(17) 0.0240(7) Uani 1 1 d . . . C33 C -0.1367(4) 0.3214(2) 0.24124(18) 0.0273(8) Uani 1 1 d . . . H33A H -0.1097 0.3471 0.2077 0.033 Uiso 1 1 calc R . . C34 C -0.2203(4) 0.2658(2) 0.2326(2) 0.0374(10) Uani 1 1 d . . . H34A H -0.2484 0.2546 0.1928 0.045 Uiso 1 1 calc R . . C35 C -0.2626(5) 0.2262(3) 0.2828(3) 0.0443(11) Uani 1 1 d . . . H35A H -0.3189 0.1898 0.2759 0.053 Uiso 1 1 calc R . . C36 C -0.2219(6) 0.2409(3) 0.3414(3) 0.0550(15) Uani 1 1 d . . . H36A H -0.2490 0.2146 0.3746 0.066 Uiso 1 1 calc R . . C37 C -0.1380(5) 0.2967(3) 0.3505(2) 0.0452(12) Uani 1 1 d . . . H37A H -0.1101 0.3073 0.3904 0.054 Uiso 1 1 calc R . . P3 P 0.96903(11) 0.27501(6) 0.04831(5) 0.0338(3) Uani 1 1 d . . . F1 F 0.9487(3) 0.35427(16) 0.07292(18) 0.0591(9) Uani 1 1 d . . . F2 F 0.9881(4) 0.19642(19) 0.0232(2) 0.0768(12) Uani 1 1 d . . . F3 F 1.1072(3) 0.2964(2) 0.0241(2) 0.0673(10) Uani 1 1 d . . . F4 F 0.8294(3) 0.25561(18) 0.07195(16) 0.0558(8) Uani 1 1 d . . . F5 F 0.9151(4) 0.2983(2) -0.01715(15) 0.0701(11) Uani 1 1 d . . . F6 F 1.0211(4) 0.2527(2) 0.11361(17) 0.0736(11) Uani 1 1 d . . . C38 C 0.4764(9) 0.5970(7) 0.0847(6) 0.120(4) Uani 1 1 d . . . H38A H 0.4575 0.5473 0.0877 0.145 Uiso 1 1 calc R . . H38B H 0.4982 0.6135 0.1259 0.145 Uiso 1 1 calc R . . C39 C 0.3300(8) 0.1771(5) 0.0311(4) 0.090(3) Uani 1 1 d . . . H39A H 0.4189 0.1809 0.0251 0.107 Uiso 1 1 calc R . . H39B H 0.2928 0.2217 0.0194 0.107 Uiso 1 1 calc R . . Cl1 Cl 0.34283(15) 0.64059(9) 0.05896(8) 0.0616(4) Uani 1 1 d . . . Cl2 Cl 0.6068(2) 0.60695(19) 0.03813(14) 0.1153(9) Uani 1 1 d . . . Cl3 Cl 0.3070(3) 0.16442(15) 0.10571(14) 0.1143(9) Uani 1 1 d . . . Cl4 Cl 0.2705(3) 0.11225(18) -0.01960(14) 0.1202(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0163(2) 0.0213(2) 0.0131(2) 0.00253(15) -0.00051(16) 0.00140(16) Fe1 0.0184(3) 0.0309(3) 0.0170(3) 0.00260(19) -0.00315(19) 0.0020(2) S1 0.0187(4) 0.0246(4) 0.0147(4) 0.0028(3) -0.0007(3) 0.0016(3) S2 0.0184(4) 0.0347(5) 0.0151(4) 0.0048(3) 0.0005(3) 0.0025(3) P1 0.0173(4) 0.0290(5) 0.0180(4) 0.0049(3) 0.0018(3) 0.0052(3) P2 0.0164(4) 0.0224(4) 0.0142(4) 0.0019(3) -0.0008(3) -0.0003(3) N1 0.0214(15) 0.0318(16) 0.0151(13) 0.0039(12) -0.0018(11) -0.0014(12) C1 0.0157(16) 0.034(2) 0.0214(17) 0.0054(14) 0.0007(13) 0.0010(14) C2 0.0185(17) 0.043(2) 0.0261(18) 0.0059(16) -0.0046(14) 0.0059(16) C3 0.0187(18) 0.054(3) 0.031(2) 0.0019(18) -0.0092(15) -0.0021(17) C4 0.030(2) 0.041(2) 0.033(2) -0.0021(18) -0.0076(17) -0.0066(18) C5 0.0201(17) 0.0317(19) 0.0296(19) 0.0057(15) -0.0009(14) -0.0022(15) C6 0.0180(16) 0.0274(17) 0.0183(16) 0.0038(13) 0.0001(12) -0.0022(14) C7 0.0242(17) 0.0295(19) 0.0223(17) 0.0078(14) -0.0016(14) -0.0012(15) C8 0.0266(19) 0.046(2) 0.0208(17) 0.0134(16) -0.0011(14) 0.0040(17) C9 0.0266(19) 0.055(3) 0.0153(17) 0.0020(16) -0.0013(14) 0.0054(18) C10 0.0211(17) 0.039(2) 0.0169(16) -0.0010(15) 0.0010(13) 0.0045(15) C11 0.0205(16) 0.0228(16) 0.0177(16) 0.0014(13) -0.0009(12) -0.0022(13) C12 0.0209(17) 0.041(2) 0.0154(16) 0.0063(14) -0.0007(13) -0.0009(15) C13 0.0225(17) 0.035(2) 0.0153(15) 0.0040(14) 0.0003(13) 0.0040(15) C14 0.0205(18) 0.050(2) 0.0234(18) 0.0144(17) 0.0040(14) 0.0111(17) C15 0.044(3) 0.061(3) 0.032(2) 0.006(2) 0.013(2) 0.016(2) C16 0.058(4) 0.096(5) 0.036(3) 0.016(3) 0.025(3) 0.032(4) C17 0.033(3) 0.122(6) 0.051(3) 0.041(4) 0.022(2) 0.024(3) C18 0.028(2) 0.108(5) 0.052(3) 0.030(3) 0.006(2) -0.009(3) C19 0.024(2) 0.074(4) 0.036(2) 0.012(2) 0.0027(18) -0.002(2) C20 0.031(2) 0.0282(19) 0.0208(17) 0.0010(14) 0.0043(14) 0.0092(15) C21 0.036(2) 0.029(2) 0.035(2) -0.0056(16) 0.0022(17) 0.0064(17) C22 0.054(3) 0.034(2) 0.050(3) -0.008(2) 0.007(2) -0.002(2) C23 0.082(4) 0.027(2) 0.041(3) -0.0020(19) 0.004(3) 0.009(2) C24 0.080(4) 0.037(3) 0.042(3) 0.002(2) -0.007(3) 0.026(3) C25 0.046(3) 0.036(2) 0.044(3) 0.0005(19) -0.006(2) 0.017(2) C26 0.0201(16) 0.0274(18) 0.0160(15) 0.0017(13) 0.0002(12) 0.0015(14) C27 0.0249(18) 0.0283(18) 0.0238(18) 0.0035(14) -0.0006(14) 0.0020(15) C28 0.037(2) 0.028(2) 0.032(2) 0.0028(16) 0.0003(17) 0.0057(17) C29 0.040(2) 0.040(2) 0.030(2) 0.0005(17) 0.0008(17) 0.021(2) C30 0.0195(18) 0.052(3) 0.042(2) 0.000(2) 0.0040(17) 0.0093(18) C31 0.0204(18) 0.039(2) 0.033(2) 0.0001(17) 0.0029(15) 0.0007(16) C32 0.0234(17) 0.0242(17) 0.0244(17) 0.0023(14) -0.0001(14) -0.0037(14) C33 0.0304(19) 0.0253(18) 0.0260(18) -0.0018(14) -0.0015(15) -0.0035(15) C34 0.040(2) 0.033(2) 0.039(2) -0.0064(18) -0.0068(18) -0.0101(19) C35 0.039(3) 0.034(2) 0.059(3) 0.002(2) -0.008(2) -0.015(2) C36 0.060(3) 0.060(3) 0.045(3) 0.020(2) -0.009(2) -0.033(3) C37 0.047(3) 0.058(3) 0.029(2) 0.014(2) -0.0071(19) -0.027(2) P3 0.0384(6) 0.0297(5) 0.0329(5) -0.0005(4) -0.0062(4) -0.0038(4) F1 0.0563(19) 0.0331(15) 0.087(3) -0.0091(15) -0.0064(17) -0.0066(14) F2 0.096(3) 0.0446(19) 0.090(3) -0.0269(19) 0.005(2) 0.0005(19) F3 0.0403(18) 0.070(2) 0.092(3) 0.012(2) 0.0065(17) 0.0001(16) F4 0.0531(18) 0.0569(19) 0.0576(19) -0.0047(15) 0.0083(15) -0.0207(15) F5 0.067(2) 0.106(3) 0.0362(16) 0.0093(18) -0.0139(15) 0.003(2) F6 0.091(3) 0.077(3) 0.051(2) 0.0114(18) -0.0307(19) 0.010(2) C38 0.071(6) 0.145(10) 0.144(10) 0.075(8) -0.014(6) 0.006(6) C39 0.062(4) 0.112(7) 0.095(6) -0.031(5) 0.009(4) 0.020(4) Cl1 0.0572(8) 0.0621(9) 0.0654(9) -0.0052(7) -0.0021(7) 0.0004(7) Cl2 0.0690(13) 0.160(3) 0.117(2) -0.0229(18) 0.0047(12) 0.0328(15) Cl3 0.134(2) 0.1024(18) 0.1048(18) 0.0043(14) -0.0282(16) 0.0048(16) Cl4 0.127(2) 0.133(2) 0.1008(19) 0.0049(17) 0.0219(16) -0.0158(19) _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 P1 2.1964(11) . ? Ni1 S1 2.2124(10) . ? Ni1 S2 2.2719(11) . ? Ni1 P2 2.2953(11) . ? Fe1 C6 2.021(4) . ? Fe1 C7 2.056(4) . ? Fe1 C3 2.063(4) . ? Fe1 C1 2.068(4) . ? Fe1 C5 2.078(4) . ? Fe1 C2 2.085(4) . ? Fe1 C10 2.088(4) . ? Fe1 C4 2.088(4) . ? Fe1 C8 2.108(4) . ? Fe1 C9 2.132(4) . ? S1 C11 1.783(4) . ? S2 C11 1.718(4) . ? P1 C1 1.786(4) . ? P1 C20 1.836(4) . ? P1 C14 1.888(4) . ? P2 C6 1.805(4) . ? P2 C32 1.840(4) . ? P2 C26 1.855(4) . ? N1 C11 1.311(5) . ? N1 C13 1.469(5) 3_565 ? N1 C12 1.520(5) . ? C1 C2 1.435(5) . ? C1 C5 1.470(6) . ? C2 C3 1.431(6) . ? C2 H2A 0.9800 . ? C3 C4 1.433(7) . ? C3 H3A 0.9800 . ? C4 C5 1.414(6) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C10 1.440(5) . ? C6 C7 1.447(5) . ? C7 C8 1.427(5) . ? C7 H7A 0.9800 . ? C8 C9 1.448(7) . ? C8 H8A 0.9800 . ? C9 C10 1.419(5) . ? C9 H9A 0.9800 . ? C10 H10A 0.9800 . ? C12 C13 1.516(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N1 1.469(5) 3_565 ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.382(7) . ? C14 C15 1.419(7) . ? C15 C16 1.436(7) . ? C15 H15A 0.9300 . ? C16 C17 1.359(11) . ? C16 H16A 0.9300 . ? C17 C18 1.410(11) . ? C17 H17A 0.9300 . ? C18 C19 1.438(7) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.389(6) . ? C20 C25 1.395(6) . ? C21 C22 1.411(7) . ? C21 H21A 0.9300 . ? C22 C23 1.372(8) . ? C22 H22A 0.9300 . ? C23 C24 1.385(9) . ? C23 H23A 0.9300 . ? C24 C25 1.415(7) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.413(5) . ? C26 C31 1.423(5) . ? C27 C28 1.413(6) . ? C27 H27A 0.9300 . ? C28 C29 1.422(7) . ? C28 H28A 0.9300 . ? C29 C30 1.385(7) . ? C29 H29A 0.9300 . ? C30 C31 1.410(6) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 C33 1.384(5) . ? C32 C37 1.421(6) . ? C33 C34 1.398(6) . ? C33 H33A 0.9300 . ? C34 C35 1.409(7) . ? C34 H34A 0.9300 . ? C35 C36 1.360(8) . ? C35 H35A 0.9300 . ? C36 C37 1.404(7) . ? C36 H36A 0.9300 . ? C37 H37A 0.9300 . ? P3 F6 1.566(3) . ? P3 F5 1.582(3) . ? P3 F2 1.609(4) . ? P3 F1 1.618(3) . ? P3 F3 1.638(4) . ? P3 F4 1.638(3) . ? C38 Cl1 1.737(9) . ? C38 Cl2 1.756(11) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 Cl3 1.660(10) . ? C39 Cl4 1.762(9) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? 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 P1 Ni1 S1 169.17(4) . . ? P1 Ni1 S2 89.56(4) . . ? S1 Ni1 S2 79.91(4) . . ? P1 Ni1 P2 100.37(4) . . ? S1 Ni1 P2 90.35(4) . . ? S2 Ni1 P2 168.78(4) . . ? C6 Fe1 C7 41.57(15) . . ? C6 Fe1 C3 177.87(18) . . ? C7 Fe1 C3 137.07(17) . . ? C6 Fe1 C1 110.65(14) . . ? C7 Fe1 C1 110.19(16) . . ? C3 Fe1 C1 67.89(16) . . ? C6 Fe1 C5 112.80(15) . . ? C7 Fe1 C5 140.73(15) . . ? C3 Fe1 C5 67.25(17) . . ? C1 Fe1 C5 41.53(16) . . ? C6 Fe1 C2 137.55(16) . . ? C7 Fe1 C2 109.16(17) . . ? C3 Fe1 C2 40.35(18) . . ? C1 Fe1 C2 40.43(14) . . ? C5 Fe1 C2 68.34(16) . . ? C6 Fe1 C10 40.99(15) . . ? C7 Fe1 C10 69.14(16) . . ? C3 Fe1 C10 141.10(17) . . ? C1 Fe1 C10 139.63(14) . . ? C5 Fe1 C10 112.80(16) . . ? C2 Fe1 C10 178.28(17) . . ? C6 Fe1 C4 140.93(17) . . ? C7 Fe1 C4 177.33(17) . . ? C3 Fe1 C4 40.40(18) . . ? C1 Fe1 C4 68.55(17) . . ? C5 Fe1 C4 39.68(16) . . ? C2 Fe1 C4 68.31(18) . . ? C10 Fe1 C4 113.40(18) . . ? C6 Fe1 C8 67.74(15) . . ? C7 Fe1 C8 40.06(15) . . ? C3 Fe1 C8 112.23(17) . . ? C1 Fe1 C8 139.00(17) . . ? C5 Fe1 C8 179.20(17) . . ? C2 Fe1 C8 111.71(17) . . ? C10 Fe1 C8 67.17(16) . . ? C4 Fe1 C8 139.54(17) . . ? C6 Fe1 C9 67.38(15) . . ? C7 Fe1 C9 67.87(17) . . ? C3 Fe1 C9 114.07(17) . . ? C1 Fe1 C9 177.88(16) . . ? C5 Fe1 C9 139.57(18) . . ? C2 Fe1 C9 140.59(15) . . ? C10 Fe1 C9 39.27(14) . . ? C4 Fe1 C9 113.42(18) . . ? C8 Fe1 C9 39.93(18) . . ? C11 S1 Ni1 84.67(12) . . ? C11 S2 Ni1 84.32(12) . . ? C1 P1 C20 109.76(18) . . ? C1 P1 C14 103.67(19) . . ? C20 P1 C14 103.43(19) . . ? C1 P1 Ni1 110.96(13) . . ? C20 P1 Ni1 112.67(14) . . ? C14 P1 Ni1 115.72(12) . . ? C6 P2 C32 102.29(17) . . ? C6 P2 C26 100.37(16) . . ? C32 P2 C26 104.33(17) . . ? C6 P2 Ni1 122.75(12) . . ? C32 P2 Ni1 112.90(13) . . ? C26 P2 Ni1 112.04(12) . . ? C11 N1 C13 121.7(3) . 3_565 ? C11 N1 C12 123.2(3) . . ? C13 N1 C12 115.1(3) 3_565 . ? C2 C1 C5 107.2(3) . . ? C2 C1 P1 130.4(3) . . ? C5 C1 P1 122.4(3) . . ? C2 C1 Fe1 70.4(2) . . ? C5 C1 Fe1 69.6(2) . . ? P1 C1 Fe1 123.2(2) . . ? C3 C2 C1 107.2(4) . . ? C3 C2 Fe1 69.0(2) . . ? C1 C2 Fe1 69.1(2) . . ? C3 C2 H2A 126.4 . . ? C1 C2 H2A 126.4 . . ? Fe1 C2 H2A 126.4 . . ? C2 C3 C4 109.8(4) . . ? C2 C3 Fe1 70.7(2) . . ? C4 C3 Fe1 70.8(2) . . ? C2 C3 H3A 125.1 . . ? C4 C3 H3A 125.1 . . ? Fe1 C3 H3A 125.1 . . ? C5 C4 C3 107.3(4) . . ? C5 C4 Fe1 69.8(2) . . ? C3 C4 Fe1 68.8(2) . . ? C5 C4 H4A 126.4 . . ? C3 C4 H4A 126.4 . . ? Fe1 C4 H4A 126.4 . . ? C4 C5 C1 108.5(4) . . ? C4 C5 Fe1 70.6(2) . . ? C1 C5 Fe1 68.9(2) . . ? C4 C5 H5A 125.7 . . ? C1 C5 H5A 125.7 . . ? Fe1 C5 H5A 125.7 . . ? C10 C6 C7 109.1(3) . . ? C10 C6 P2 125.5(3) . . ? C7 C6 P2 125.4(3) . . ? C10 C6 Fe1 72.0(2) . . ? C7 C6 Fe1 70.5(2) . . ? P2 C6 Fe1 121.52(18) . . ? C8 C7 C6 106.4(3) . . ? C8 C7 Fe1 71.9(2) . . ? C6 C7 Fe1 67.9(2) . . ? C8 C7 H7A 126.8 . . ? C6 C7 H7A 126.8 . . ? Fe1 C7 H7A 126.8 . . ? C7 C8 C9 108.9(3) . . ? C7 C8 Fe1 68.0(2) . . ? C9 C8 Fe1 70.9(2) . . ? C7 C8 H8A 125.5 . . ? C9 C8 H8A 125.5 . . ? Fe1 C8 H8A 125.5 . . ? C10 C9 C8 108.2(4) . . ? C10 C9 Fe1 68.7(2) . . ? C8 C9 Fe1 69.1(2) . . ? C10 C9 H9A 125.9 . . ? C8 C9 H9A 125.9 . . ? Fe1 C9 H9A 125.9 . . ? C9 C10 C6 107.5(4) . . ? C9 C10 Fe1 72.0(2) . . ? C6 C10 Fe1 67.0(2) . . ? C9 C10 H10A 126.3 . . ? C6 C10 H10A 126.3 . . ? Fe1 C10 H10A 126.3 . . ? N1 C11 S2 123.8(3) . . ? N1 C11 S1 125.5(3) . . ? S2 C11 S1 110.70(19) . . ? C13 C12 N1 110.2(3) . . ? C13 C12 H12A 109.6 . . ? N1 C12 H12A 109.6 . . ? C13 C12 H12B 109.6 . . ? N1 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N1 C13 C12 107.7(3) 3_565 . ? N1 C13 H13A 110.2 3_565 . ? C12 C13 H13A 110.2 . . ? N1 C13 H13B 110.2 3_565 . ? C12 C13 H13B 110.2 . . ? H13A C13 H13B 108.5 . . ? C19 C14 C15 118.2(4) . . ? C19 C14 P1 121.0(4) . . ? C15 C14 P1 120.8(4) . . ? C14 C15 C16 119.9(6) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C17 C16 C15 122.1(6) . . ? C17 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? C16 C17 C18 118.1(5) . . ? C16 C17 H17A 120.9 . . ? C18 C17 H17A 120.9 . . ? C17 C18 C19 120.9(6) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C14 C19 C18 120.7(6) . . ? C14 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? C21 C20 C25 118.9(4) . . ? C21 C20 P1 119.3(3) . . ? C25 C20 P1 121.7(4) . . ? C20 C21 C22 120.6(4) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C23 C22 C21 120.7(5) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 119.1(5) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? C23 C24 C25 121.0(5) . . ? C23 C24 H24A 119.5 . . ? C25 C24 H24A 119.5 . . ? C20 C25 C24 119.6(5) . . ? C20 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C27 C26 C31 118.9(4) . . ? C27 C26 P2 118.7(3) . . ? C31 C26 P2 122.3(3) . . ? C28 C27 C26 120.1(4) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C29 120.2(4) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C30 C29 C28 119.7(4) . . ? C30 C29 H29A 120.2 . . ? C28 C29 H29A 120.2 . . ? C29 C30 C31 120.8(4) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C30 C31 C26 120.3(4) . . ? C30 C31 H31A 119.8 . . ? C26 C31 H31A 119.8 . . ? C33 C32 C37 118.7(4) . . ? C33 C32 P2 118.6(3) . . ? C37 C32 P2 122.7(3) . . ? C32 C33 C34 119.1(4) . . ? C32 C33 H33A 120.5 . . ? C34 C33 H33A 120.5 . . ? C33 C34 C35 121.4(4) . . ? C33 C34 H34A 119.3 . . ? C35 C34 H34A 119.3 . . ? C36 C35 C34 120.5(4) . . ? C36 C35 H35A 119.7 . . ? C34 C35 H35A 119.7 . . ? C35 C36 C37 118.5(5) . . ? C35 C36 H36A 120.8 . . ? C37 C36 H36A 120.8 . . ? C36 C37 C32 121.9(4) . . ? C36 C37 H37A 119.1 . . ? C32 C37 H37A 119.1 . . ? F6 P3 F5 179.1(3) . . ? F6 P3 F2 90.4(2) . . ? F5 P3 F2 90.3(2) . . ? F6 P3 F1 90.2(2) . . ? F5 P3 F1 89.1(2) . . ? F2 P3 F1 179.3(2) . . ? F6 P3 F3 92.9(2) . . ? F5 P3 F3 87.6(2) . . ? F2 P3 F3 90.0(2) . . ? F1 P3 F3 90.2(2) . . ? F6 P3 F4 88.0(2) . . ? F5 P3 F4 91.5(2) . . ? F2 P3 F4 91.2(2) . . ? F1 P3 F4 88.60(19) . . ? F3 P3 F4 178.5(2) . . ? Cl1 C38 Cl2 115.3(6) . . ? Cl1 C38 H38A 108.4 . . ? Cl2 C38 H38A 108.4 . . ? Cl1 C38 H38B 108.4 . . ? Cl2 C38 H38B 108.4 . . ? H38A C38 H38B 107.5 . . ? Cl3 C39 Cl4 116.4(6) . . ? Cl3 C39 H39A 108.2 . . ? Cl4 C39 H39A 108.2 . . ? Cl3 C39 H39B 108.2 . . ? Cl4 C39 H39B 108.2 . . ? H39A C39 H39B 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Ni1 S1 C11 17.7(3) . . . . ? S2 Ni1 S1 C11 4.06(12) . . . . ? P2 Ni1 S1 C11 -170.33(12) . . . . ? P1 Ni1 S2 C11 178.32(12) . . . . ? S1 Ni1 S2 C11 -4.22(12) . . . . ? P2 Ni1 S2 C11 25.9(3) . . . . ? S1 Ni1 P1 C1 115.5(2) . . . . ? S2 Ni1 P1 C1 128.93(14) . . . . ? P2 Ni1 P1 C1 -56.32(14) . . . . ? S1 Ni1 P1 C20 -121.0(2) . . . . ? S2 Ni1 P1 C20 -107.53(14) . . . . ? P2 Ni1 P1 C20 67.21(14) . . . . ? S1 Ni1 P1 C14 -2.2(3) . . . . ? S2 Ni1 P1 C14 11.20(18) . . . . ? P2 Ni1 P1 C14 -174.06(17) . . . . ? P1 Ni1 P2 C6 24.68(16) . . . . ? S1 Ni1 P2 C6 -153.79(15) . . . . ? S2 Ni1 P2 C6 176.6(2) . . . . ? P1 Ni1 P2 C32 -98.45(14) . . . . ? S1 Ni1 P2 C32 83.08(14) . . . . ? S2 Ni1 P2 C32 53.5(3) . . . . ? P1 Ni1 P2 C26 144.11(13) . . . . ? S1 Ni1 P2 C26 -34.36(13) . . . . ? S2 Ni1 P2 C26 -64.0(2) . . . . ? C20 P1 C1 C2 23.6(4) . . . . ? C14 P1 C1 C2 -86.3(4) . . . . ? Ni1 P1 C1 C2 148.8(3) . . . . ? C20 P1 C1 C5 -153.7(3) . . . . ? C14 P1 C1 C5 96.4(3) . . . . ? Ni1 P1 C1 C5 -28.5(3) . . . . ? C20 P1 C1 Fe1 -68.2(3) . . . . ? C14 P1 C1 Fe1 -178.1(2) . . . . ? Ni1 P1 C1 Fe1 57.0(2) . . . . ? C6 Fe1 C1 C2 -140.7(2) . . . . ? C7 Fe1 C1 C2 -96.2(3) . . . . ? C3 Fe1 C1 C2 37.7(3) . . . . ? C5 Fe1 C1 C2 117.8(3) . . . . ? C10 Fe1 C1 C2 -177.4(3) . . . . ? C4 Fe1 C1 C2 81.3(3) . . . . ? C8 Fe1 C1 C2 -61.3(3) . . . . ? C6 Fe1 C1 C5 101.5(2) . . . . ? C7 Fe1 C1 C5 146.0(2) . . . . ? C3 Fe1 C1 C5 -80.2(2) . . . . ? C2 Fe1 C1 C5 -117.8(3) . . . . ? C10 Fe1 C1 C5 64.8(3) . . . . ? C4 Fe1 C1 C5 -36.5(2) . . . . ? C8 Fe1 C1 C5 -179.1(2) . . . . ? C6 Fe1 C1 P1 -14.6(3) . . . . ? C7 Fe1 C1 P1 29.9(3) . . . . ? C3 Fe1 C1 P1 163.8(3) . . . . ? C5 Fe1 C1 P1 -116.1(3) . . . . ? C2 Fe1 C1 P1 126.1(4) . . . . ? C10 Fe1 C1 P1 -51.2(4) . . . . ? C4 Fe1 C1 P1 -152.6(3) . . . . ? C8 Fe1 C1 P1 64.9(3) . . . . ? C5 C1 C2 C3 1.5(4) . . . . ? P1 C1 C2 C3 -176.1(3) . . . . ? Fe1 C1 C2 C3 -58.7(3) . . . . ? C5 C1 C2 Fe1 60.2(3) . . . . ? P1 C1 C2 Fe1 -117.4(3) . . . . ? C6 Fe1 C2 C3 -179.5(3) . . . . ? C7 Fe1 C2 C3 -142.0(3) . . . . ? C1 Fe1 C2 C3 119.0(4) . . . . ? C5 Fe1 C2 C3 79.9(3) . . . . ? C4 Fe1 C2 C3 37.1(3) . . . . ? C8 Fe1 C2 C3 -99.2(3) . . . . ? C9 Fe1 C2 C3 -63.9(4) . . . . ? C6 Fe1 C2 C1 61.5(3) . . . . ? C7 Fe1 C2 C1 99.0(2) . . . . ? C3 Fe1 C2 C1 -119.0(4) . . . . ? C5 Fe1 C2 C1 -39.1(2) . . . . ? C4 Fe1 C2 C1 -82.0(3) . . . . ? C8 Fe1 C2 C1 141.7(2) . . . . ? C9 Fe1 C2 C1 177.1(3) . . . . ? C1 C2 C3 C4 -1.4(5) . . . . ? Fe1 C2 C3 C4 -60.2(3) . . . . ? C1 C2 C3 Fe1 58.8(3) . . . . ? C7 Fe1 C3 C2 58.6(3) . . . . ? C1 Fe1 C3 C2 -37.7(2) . . . . ? C5 Fe1 C3 C2 -82.8(3) . . . . ? C10 Fe1 C3 C2 178.6(3) . . . . ? C4 Fe1 C3 C2 -120.2(4) . . . . ? C8 Fe1 C3 C2 97.8(3) . . . . ? C9 Fe1 C3 C2 141.4(3) . . . . ? C7 Fe1 C3 C4 178.8(3) . . . . ? C1 Fe1 C3 C4 82.4(3) . . . . ? C5 Fe1 C3 C4 37.3(3) . . . . ? C2 Fe1 C3 C4 120.2(4) . . . . ? C10 Fe1 C3 C4 -61.3(4) . . . . ? C8 Fe1 C3 C4 -142.0(3) . . . . ? C9 Fe1 C3 C4 -98.4(3) . . . . ? C2 C3 C4 C5 0.7(5) . . . . ? Fe1 C3 C4 C5 -59.4(3) . . . . ? C2 C3 C4 Fe1 60.1(3) . . . . ? C6 Fe1 C4 C5 -58.6(4) . . . . ? C3 Fe1 C4 C5 118.8(4) . . . . ? C1 Fe1 C4 C5 38.2(2) . . . . ? C2 Fe1 C4 C5 81.8(3) . . . . ? C10 Fe1 C4 C5 -98.0(3) . . . . ? C8 Fe1 C4 C5 -179.7(3) . . . . ? C9 Fe1 C4 C5 -141.0(2) . . . . ? C6 Fe1 C4 C3 -177.4(3) . . . . ? C1 Fe1 C4 C3 -80.7(3) . . . . ? C5 Fe1 C4 C3 -118.8(4) . . . . ? C2 Fe1 C4 C3 -37.0(3) . . . . ? C10 Fe1 C4 C3 143.1(3) . . . . ? C8 Fe1 C4 C3 61.4(4) . . . . ? C9 Fe1 C4 C3 100.2(3) . . . . ? C3 C4 C5 C1 0.2(5) . . . . ? Fe1 C4 C5 C1 -58.6(3) . . . . ? C3 C4 C5 Fe1 58.8(3) . . . . ? C2 C1 C5 C4 -1.1(4) . . . . ? P1 C1 C5 C4 176.7(3) . . . . ? Fe1 C1 C5 C4 59.6(3) . . . . ? C2 C1 C5 Fe1 -60.7(3) . . . . ? P1 C1 C5 Fe1 117.1(3) . . . . ? C6 Fe1 C5 C4 144.3(3) . . . . ? C7 Fe1 C5 C4 -175.9(3) . . . . ? C3 Fe1 C5 C4 -38.0(3) . . . . ? C1 Fe1 C5 C4 -119.8(3) . . . . ? C2 Fe1 C5 C4 -81.7(3) . . . . ? C10 Fe1 C5 C4 99.7(3) . . . . ? C9 Fe1 C5 C4 62.9(3) . . . . ? C6 Fe1 C5 C1 -95.9(2) . . . . ? C7 Fe1 C5 C1 -56.0(3) . . . . ? C3 Fe1 C5 C1 81.8(2) . . . . ? C2 Fe1 C5 C1 38.1(2) . . . . ? C10 Fe1 C5 C1 -140.5(2) . . . . ? C4 Fe1 C5 C1 119.8(3) . . . . ? C9 Fe1 C5 C1 -177.2(2) . . . . ? C32 P2 C6 C10 -129.3(3) . . . . ? C26 P2 C6 C10 -22.0(3) . . . . ? Ni1 P2 C6 C10 102.9(3) . . . . ? C32 P2 C6 C7 53.7(3) . . . . ? C26 P2 C6 C7 161.0(3) . . . . ? Ni1 P2 C6 C7 -74.2(3) . . . . ? C32 P2 C6 Fe1 141.1(2) . . . . ? C26 P2 C6 Fe1 -111.6(2) . . . . ? Ni1 P2 C6 Fe1 13.3(3) . . . . ? C7 Fe1 C6 C10 118.6(3) . . . . ? C1 Fe1 C6 C10 -143.9(2) . . . . ? C5 Fe1 C6 C10 -99.0(2) . . . . ? C2 Fe1 C6 C10 178.6(2) . . . . ? C4 Fe1 C6 C10 -62.8(3) . . . . ? C8 Fe1 C6 C10 80.3(2) . . . . ? C9 Fe1 C6 C10 37.0(2) . . . . ? C1 Fe1 C6 C7 97.5(2) . . . . ? C5 Fe1 C6 C7 142.3(2) . . . . ? C2 Fe1 C6 C7 60.0(3) . . . . ? C10 Fe1 C6 C7 -118.6(3) . . . . ? C4 Fe1 C6 C7 178.6(3) . . . . ? C8 Fe1 C6 C7 -38.3(2) . . . . ? C9 Fe1 C6 C7 -81.7(2) . . . . ? C7 Fe1 C6 P2 -120.2(3) . . . . ? C1 Fe1 C6 P2 -22.7(3) . . . . ? C5 Fe1 C6 P2 22.1(3) . . . . ? C2 Fe1 C6 P2 -60.2(3) . . . . ? C10 Fe1 C6 P2 121.2(3) . . . . ? C4 Fe1 C6 P2 58.4(4) . . . . ? C8 Fe1 C6 P2 -158.5(3) . . . . ? C9 Fe1 C6 P2 158.1(3) . . . . ? C10 C6 C7 C8 0.0(4) . . . . ? P2 C6 C7 C8 177.4(3) . . . . ? Fe1 C6 C7 C8 62.0(3) . . . . ? C10 C6 C7 Fe1 -62.1(3) . . . . ? P2 C6 C7 Fe1 115.4(3) . . . . ? C6 Fe1 C7 C8 -117.0(3) . . . . ? C3 Fe1 C7 C8 65.5(3) . . . . ? C1 Fe1 C7 C8 144.3(2) . . . . ? C5 Fe1 C7 C8 -179.8(3) . . . . ? C2 Fe1 C7 C8 101.3(3) . . . . ? C10 Fe1 C7 C8 -78.9(2) . . . . ? C9 Fe1 C7 C8 -36.6(2) . . . . ? C3 Fe1 C7 C6 -177.6(2) . . . . ? C1 Fe1 C7 C6 -98.7(2) . . . . ? C5 Fe1 C7 C6 -62.9(3) . . . . ? C2 Fe1 C7 C6 -141.8(2) . . . . ? C10 Fe1 C7 C6 38.0(2) . . . . ? C8 Fe1 C7 C6 117.0(3) . . . . ? C9 Fe1 C7 C6 80.4(2) . . . . ? C6 C7 C8 C9 -0.1(4) . . . . ? Fe1 C7 C8 C9 59.3(3) . . . . ? C6 C7 C8 Fe1 -59.4(2) . . . . ? C6 Fe1 C8 C7 39.7(2) . . . . ? C3 Fe1 C8 C7 -138.0(3) . . . . ? C1 Fe1 C8 C7 -56.6(3) . . . . ? C2 Fe1 C8 C7 -94.3(3) . . . . ? C10 Fe1 C8 C7 84.3(2) . . . . ? C4 Fe1 C8 C7 -175.9(3) . . . . ? C9 Fe1 C8 C7 120.6(3) . . . . ? C6 Fe1 C8 C9 -80.9(2) . . . . ? C7 Fe1 C8 C9 -120.6(3) . . . . ? C3 Fe1 C8 C9 101.4(3) . . . . ? C1 Fe1 C8 C9 -177.2(2) . . . . ? C2 Fe1 C8 C9 145.1(2) . . . . ? C10 Fe1 C8 C9 -36.3(2) . . . . ? C4 Fe1 C8 C9 63.5(3) . . . . ? C7 C8 C9 C10 0.2(5) . . . . ? Fe1 C8 C9 C10 57.8(3) . . . . ? C7 C8 C9 Fe1 -57.5(3) . . . . ? C6 Fe1 C9 C10 -38.5(2) . . . . ? C7 Fe1 C9 C10 -83.7(3) . . . . ? C3 Fe1 C9 C10 143.2(3) . . . . ? C5 Fe1 C9 C10 60.6(4) . . . . ? C2 Fe1 C9 C10 -177.3(3) . . . . ? C4 Fe1 C9 C10 98.8(3) . . . . ? C8 Fe1 C9 C10 -120.4(4) . . . . ? C6 Fe1 C9 C8 81.9(2) . . . . ? C7 Fe1 C9 C8 36.7(2) . . . . ? C3 Fe1 C9 C8 -96.4(3) . . . . ? C5 Fe1 C9 C8 -179.0(2) . . . . ? C2 Fe1 C9 C8 -56.9(4) . . . . ? C10 Fe1 C9 C8 120.4(4) . . . . ? C4 Fe1 C9 C8 -140.7(2) . . . . ? C8 C9 C10 C6 -0.2(5) . . . . ? Fe1 C9 C10 C6 57.8(3) . . . . ? C8 C9 C10 Fe1 -58.0(3) . . . . ? C7 C6 C10 C9 0.2(4) . . . . ? P2 C6 C10 C9 -177.3(3) . . . . ? Fe1 C6 C10 C9 -61.0(3) . . . . ? C7 C6 C10 Fe1 61.1(3) . . . . ? P2 C6 C10 Fe1 -116.3(3) . . . . ? C6 Fe1 C10 C9 118.7(4) . . . . ? C7 Fe1 C10 C9 80.2(3) . . . . ? C3 Fe1 C10 C9 -60.7(4) . . . . ? C1 Fe1 C10 C9 177.2(3) . . . . ? C5 Fe1 C10 C9 -142.2(3) . . . . ? C4 Fe1 C10 C9 -98.9(3) . . . . ? C8 Fe1 C10 C9 36.9(3) . . . . ? C7 Fe1 C10 C6 -38.6(2) . . . . ? C3 Fe1 C10 C6 -179.4(3) . . . . ? C1 Fe1 C10 C6 58.4(3) . . . . ? C5 Fe1 C10 C6 99.0(2) . . . . ? C4 Fe1 C10 C6 142.3(2) . . . . ? C8 Fe1 C10 C6 -81.8(2) . . . . ? C9 Fe1 C10 C6 -118.7(4) . . . . ? C13 N1 C11 S2 178.2(3) 3_565 . . . ? C12 N1 C11 S2 0.0(5) . . . . ? C13 N1 C11 S1 -1.7(5) 3_565 . . . ? C12 N1 C11 S1 -179.9(3) . . . . ? Ni1 S2 C11 N1 -174.4(3) . . . . ? Ni1 S2 C11 S1 5.52(16) . . . . ? Ni1 S1 C11 N1 174.3(3) . . . . ? Ni1 S1 C11 S2 -5.66(16) . . . . ? C11 N1 C12 C13 120.4(4) . . . . ? C13 N1 C12 C13 -57.9(5) 3_565 . . . ? N1 C12 C13 N1 53.7(4) . . . 3_565 ? C1 P1 C14 C19 -29.3(4) . . . . ? C20 P1 C14 C19 -143.9(4) . . . . ? Ni1 P1 C14 C19 92.4(4) . . . . ? C1 P1 C14 C15 153.7(3) . . . . ? C20 P1 C14 C15 39.1(4) . . . . ? Ni1 P1 C14 C15 -84.6(4) . . . . ? C19 C14 C15 C16 3.2(7) . . . . ? P1 C14 C15 C16 -179.6(4) . . . . ? C14 C15 C16 C17 -1.9(8) . . . . ? C15 C16 C17 C18 0.1(9) . . . . ? C16 C17 C18 C19 0.2(9) . . . . ? C15 C14 C19 C18 -3.0(7) . . . . ? P1 C14 C19 C18 179.9(4) . . . . ? C17 C18 C19 C14 1.3(8) . . . . ? C1 P1 C20 C21 130.3(3) . . . . ? C14 P1 C20 C21 -119.6(3) . . . . ? Ni1 P1 C20 C21 6.1(4) . . . . ? C1 P1 C20 C25 -52.3(4) . . . . ? C14 P1 C20 C25 57.8(4) . . . . ? Ni1 P1 C20 C25 -176.5(3) . . . . ? C25 C20 C21 C22 2.8(6) . . . . ? P1 C20 C21 C22 -179.7(4) . . . . ? C20 C21 C22 C23 -0.1(7) . . . . ? C21 C22 C23 C24 -2.2(8) . . . . ? C22 C23 C24 C25 1.8(8) . . . . ? C21 C20 C25 C24 -3.2(7) . . . . ? P1 C20 C25 C24 179.4(4) . . . . ? C23 C24 C25 C20 0.9(8) . . . . ? C6 P2 C26 C27 84.2(3) . . . . ? C32 P2 C26 C27 -170.2(3) . . . . ? Ni1 P2 C26 C27 -47.7(3) . . . . ? C6 P2 C26 C31 -92.7(3) . . . . ? C32 P2 C26 C31 13.0(3) . . . . ? Ni1 P2 C26 C31 135.5(3) . . . . ? C31 C26 C27 C28 1.1(5) . . . . ? P2 C26 C27 C28 -175.9(3) . . . . ? C26 C27 C28 C29 -1.0(6) . . . . ? C27 C28 C29 C30 0.3(6) . . . . ? C28 C29 C30 C31 0.4(7) . . . . ? C29 C30 C31 C26 -0.3(7) . . . . ? C27 C26 C31 C30 -0.4(6) . . . . ? P2 C26 C31 C30 176.4(3) . . . . ? C6 P2 C32 C33 -164.5(3) . . . . ? C26 P2 C32 C33 91.3(3) . . . . ? Ni1 P2 C32 C33 -30.6(4) . . . . ? C6 P2 C32 C37 18.0(4) . . . . ? C26 P2 C32 C37 -86.3(4) . . . . ? Ni1 P2 C32 C37 151.8(4) . . . . ? C37 C32 C33 C34 0.1(6) . . . . ? P2 C32 C33 C34 -177.6(3) . . . . ? C32 C33 C34 C35 0.2(7) . . . . ? C33 C34 C35 C36 -0.7(8) . . . . ? C34 C35 C36 C37 0.7(9) . . . . ? C35 C36 C37 C32 -0.3(10) . . . . ? C33 C32 C37 C36 -0.1(8) . . . . ? P2 C32 C37 C36 177.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.512 _refine_diff_density_min -1.934 _refine_diff_density_rms 0.129 #============================================================================== # start Validation Reply Form _vrf_PLAT601_1 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 214.00 A**3 RESPONSE: The difference map indicated the presence of diffuse electron density believed to be disordered solvent (thought to be ethanol methanol or a mixture). SQUEEZE was used leaving a void of 213 \%A from which 23 e^-^ were removed. ; _vrf_PLAT305_4 ; PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??) RESPONSE: This is thought to be a bug in checkCIF, because the parts are correct and if the occupancy of all atoms in the third part are altered to 0.5, the alert disappears. Chester has been notified. ; # end Validation Reply Form #==============================================================================