# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_date 2012-09-20 _audit_creation_method CRYSTALS_ver_14.43 _oxford_structure_analysis_title 'sk_674_0m in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.0198(3) _cell_length_b 11.1462(3) _cell_length_c 19.6789(5) _cell_angle_alpha 85.0180(10) _cell_angle_beta 79.607(2) _cell_angle_gamma 74.2580(10) _cell_volume 2078.99(10) _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' 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' V 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780 1.2199 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C45 H51 N3 P3 V1 # Dc = 1.24 Fooo = 820.00 Mu = 3.88 M = 777.78 # Found Formula = C45 H51 N3 P3 V1 # Dc = 1.24 FOOO = 820.00 Mu = 3.88 M = 777.78 _chemical_formula_sum 'C45 H51 N3 P3 V1' _chemical_formula_moiety 'C45 H51 N3 P3 V1' _chemical_compound_source ? _chemical_formula_weight 777.78 _cell_measurement_reflns_used 9871 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 135 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_min 0.140 _exptl_crystal_size_mid 0.330 _exptl_crystal_size_max 0.360 _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 0.388 # Sheldrick geometric approximatio 0.88 0.95 # No experimental values of Tmin/max available _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.95 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _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 135 _diffrn_reflns_number 53530 _reflns_number_total 12100 _diffrn_reflns_av_R_equivalents 0.039 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 12100 # Theoretical number of reflections is about 24259 _diffrn_reflns_theta_min 2.106 _diffrn_reflns_theta_max 30.001 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.001 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _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 Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.39 _refine_diff_density_max 0.69 # 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>-10.0\s(I) _refine_ls_number_reflns 12100 _refine_ls_number_restraints 0 _refine_ls_number_parameters 469 _oxford_refine_ls_R_factor_ref 0.0442 _refine_ls_wR_factor_ref 0.0834 _refine_ls_goodness_of_fit_ref 0.9947 _refine_ls_shift/su_max 0.0021021 _refine_ls_shift/su_mean 0.0000882 # The values computed with all filters except I/sigma _oxford_reflns_number_all 12100 _refine_ls_R_factor_all 0.0442 _refine_ls_wR_factor_all 0.0834 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9598 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_gt 0.0754 # 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 #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^) + ( 0.03P)^2^ + 1.03P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens V1 V 1.03883(2) 0.314715(18) 0.251323(10) 0.0145 1.0000 Uani . . . . . . P1 P 1.14856(4) 0.40942(3) 0.142803(17) 0.0191 1.0000 Uani . . . . . . P2 P 1.27921(3) 0.21278(3) 0.315176(17) 0.0174 1.0000 Uani . . . . . . P3 P 0.80756(3) 0.36804(3) 0.325183(17) 0.0168 1.0000 Uani . . . . . . N1 N 1.02025(12) 0.33864(10) 0.15489(5) 0.0185 1.0000 Uani . . . . . . N2 N 1.16582(11) 0.16069(9) 0.28030(6) 0.0175 1.0000 Uani . . . . . . N3 N 0.93190(11) 0.44170(10) 0.31544(5) 0.0171 1.0000 Uani . . . . . . C1 C 0.94580(15) 0.30775(12) 0.10333(7) 0.0216 1.0000 Uani . . . . . . C2 C 0.78836(16) 0.33888(14) 0.12976(8) 0.0273 1.0000 Uani . . . . . . C3 C 1.00150(18) 0.16949(14) 0.08851(8) 0.0298 1.0000 Uani . . . . . . C4 C 1.08376(15) 0.57117(12) 0.11337(7) 0.0211 1.0000 Uani . . . . . . C5 C 0.94258(16) 0.62125(13) 0.10904(8) 0.0263 1.0000 Uani . . . . . . C6 C 0.88965(18) 0.74819(14) 0.09571(8) 0.0319 1.0000 Uani . . . . . . C7 C 0.9775(2) 0.82670(14) 0.08777(8) 0.0344 1.0000 Uani . . . . . . C8 C 1.1175(2) 0.77856(15) 0.09160(9) 0.0357 1.0000 Uani . . . . . . C9 C 1.17151(17) 0.65167(14) 0.10411(8) 0.0297 1.0000 Uani . . . . . . C10 C 1.28427(14) 0.34138(13) 0.07136(7) 0.0227 1.0000 Uani . . . . . . C11 C 1.31004(16) 0.40083(16) 0.00709(8) 0.0310 1.0000 Uani . . . . . . C12 C 1.41442(19) 0.3401(2) -0.04431(9) 0.0440 1.0000 Uani . . . . . . C13 C 1.49288(19) 0.2209(2) -0.03273(10) 0.0457 1.0000 Uani . . . . . . C14 C 1.46930(19) 0.16120(18) 0.03146(10) 0.0440 1.0000 Uani . . . . . . C15 C 1.36625(17) 0.22079(15) 0.08310(9) 0.0339 1.0000 Uani . . . . . . C16 C 1.16818(14) 0.02740(12) 0.28206(7) 0.0220 1.0000 Uani . . . . . . C17 C 1.25460(16) -0.03218(13) 0.21570(8) 0.0284 1.0000 Uani . . . . . . C18 C 1.01974(16) 0.01136(14) 0.29170(9) 0.0313 1.0000 Uani . . . . . . C19 C 1.45389(13) 0.10499(12) 0.29053(7) 0.0186 1.0000 Uani . . . . . . C20 C 1.53915(15) 0.13723(13) 0.23160(7) 0.0248 1.0000 Uani . . . . . . C21 C 1.66697(16) 0.05546(15) 0.20625(8) 0.0312 1.0000 Uani . . . . . . C22 C 1.71262(15) -0.05833(14) 0.24019(8) 0.0294 1.0000 Uani . . . . . . C23 C 1.63023(15) -0.09089(13) 0.29945(7) 0.0256 1.0000 Uani . . . . . . C24 C 1.50189(14) -0.01019(13) 0.32463(7) 0.0223 1.0000 Uani . . . . . . C25 C 1.24616(14) 0.17532(12) 0.40833(7) 0.0193 1.0000 Uani . . . . . . C26 C 1.34401(15) 0.18039(14) 0.44968(7) 0.0263 1.0000 Uani . . . . . . C27 C 1.31488(16) 0.16423(16) 0.52104(8) 0.0304 1.0000 Uani . . . . . . C28 C 1.18658(16) 0.14414(14) 0.55234(7) 0.0284 1.0000 Uani . . . . . . C29 C 1.08786(15) 0.14104(14) 0.51220(8) 0.0272 1.0000 Uani . . . . . . C30 C 1.11752(14) 0.15714(13) 0.44065(7) 0.0230 1.0000 Uani . . . . . . C31 C 0.94024(14) 0.55312(12) 0.34803(7) 0.0203 1.0000 Uani . . . . . . C32 C 1.02347(18) 0.51450(14) 0.40739(8) 0.0307 1.0000 Uani . . . . . . C33 C 1.00753(15) 0.63525(13) 0.29461(7) 0.0248 1.0000 Uani . . . . . . C34 C 0.74301(14) 0.33186(13) 0.41555(7) 0.0212 1.0000 Uani . . . . . . C35 C 0.73535(15) 0.21131(13) 0.43657(8) 0.0263 1.0000 Uani . . . . . . C36 C 0.68971(17) 0.18169(15) 0.50559(8) 0.0345 1.0000 Uani . . . . . . C37 C 0.65199(17) 0.27251(17) 0.55372(8) 0.0363 1.0000 Uani . . . . . . C38 C 0.6575(2) 0.39308(18) 0.53349(9) 0.0413 1.0000 Uani . . . . . . C39 C 0.70175(18) 0.42322(15) 0.46466(8) 0.0343 1.0000 Uani . . . . . . C40 C 0.65025(13) 0.47038(11) 0.29752(6) 0.0176 1.0000 Uani . . . . . . C41 C 0.52910(14) 0.42842(12) 0.30376(7) 0.0222 1.0000 Uani . . . . . . C42 C 0.41287(15) 0.49932(13) 0.27673(8) 0.0278 1.0000 Uani . . . . . . C43 C 0.41436(15) 0.61455(13) 0.24458(8) 0.0272 1.0000 Uani . . . . . . C44 C 0.53346(15) 0.65786(13) 0.23821(8) 0.0258 1.0000 Uani . . . . . . C45 C 0.65169(14) 0.58531(12) 0.26372(7) 0.0222 1.0000 Uani . . . . . . H11 H 0.9641 0.3568 0.0596 0.0254 1.0000 Uiso R . . . . . H21 H 0.7499 0.4263 0.1386 0.0404 1.0000 Uiso R . . . . . H22 H 0.7409 0.3180 0.0962 0.0405 1.0000 Uiso R . . . . . H23 H 0.7686 0.2925 0.1729 0.0401 1.0000 Uiso R . . . . . H31 H 1.1008 0.1492 0.0692 0.0440 1.0000 Uiso R . . . . . H32 H 0.9501 0.1479 0.0563 0.0444 1.0000 Uiso R . . . . . H33 H 0.9894 0.1204 0.1319 0.0435 1.0000 Uiso R . . . . . H51 H 0.8815 0.5696 0.1154 0.0323 1.0000 Uiso R . . . . . H61 H 0.7935 0.7810 0.0920 0.0389 1.0000 Uiso R . . . . . H71 H 0.9401 0.9131 0.0797 0.0407 1.0000 Uiso R . . . . . H81 H 1.1777 0.8310 0.0856 0.0431 1.0000 Uiso R . . . . . H91 H 1.2665 0.6204 0.1064 0.0360 1.0000 Uiso R . . . . . H111 H 1.2550 0.4833 -0.0019 0.0370 1.0000 Uiso R . . . . . H121 H 1.4328 0.3806 -0.0872 0.0539 1.0000 Uiso R . . . . . H131 H 1.5629 0.1793 -0.0677 0.0549 1.0000 Uiso R . . . . . H141 H 1.5218 0.0818 0.0399 0.0538 1.0000 Uiso R . . . . . H151 H 1.3509 0.1808 0.1264 0.0420 1.0000 Uiso R . . . . . H161 H 1.2109 -0.0149 0.3221 0.0254 1.0000 Uiso R . . . . . H171 H 1.2545 -0.1187 0.2167 0.0433 1.0000 Uiso R . . . . . H172 H 1.2125 0.0096 0.1766 0.0423 1.0000 Uiso R . . . . . H173 H 1.3510 -0.0284 0.2096 0.0425 1.0000 Uiso R . . . . . H181 H 1.0217 -0.0750 0.2888 0.0470 1.0000 Uiso R . . . . . H182 H 0.9701 0.0592 0.2557 0.0463 1.0000 Uiso R . . . . . H183 H 0.9685 0.0386 0.3366 0.0461 1.0000 Uiso R . . . . . H201 H 1.5099 0.2136 0.2095 0.0305 1.0000 Uiso R . . . . . H211 H 1.7215 0.0791 0.1659 0.0383 1.0000 Uiso R . . . . . H221 H 1.8007 -0.1132 0.2224 0.0352 1.0000 Uiso R . . . . . H231 H 1.6612 -0.1685 0.3226 0.0316 1.0000 Uiso R . . . . . H241 H 1.4459 -0.0337 0.3660 0.0270 1.0000 Uiso R . . . . . H261 H 1.4324 0.1949 0.4284 0.0311 1.0000 Uiso R . . . . . H271 H 1.3831 0.1657 0.5485 0.0369 1.0000 Uiso R . . . . . H281 H 1.1675 0.1321 0.6013 0.0337 1.0000 Uiso R . . . . . H291 H 0.9997 0.1285 0.5327 0.0326 1.0000 Uiso R . . . . . H301 H 1.0500 0.1565 0.4139 0.0281 1.0000 Uiso R . . . . . H311 H 0.8435 0.6003 0.3655 0.0237 1.0000 Uiso R . . . . . H321 H 1.0247 0.5864 0.4304 0.0453 1.0000 Uiso R . . . . . H322 H 1.1200 0.4707 0.3899 0.0452 1.0000 Uiso R . . . . . H323 H 0.9809 0.4614 0.4407 0.0445 1.0000 Uiso R . . . . . H331 H 1.0212 0.7045 0.3164 0.0369 1.0000 Uiso R . . . . . H332 H 1.0986 0.5882 0.2726 0.0363 1.0000 Uiso R . . . . . H333 H 0.9509 0.6673 0.2581 0.0361 1.0000 Uiso R . . . . . H351 H 0.7607 0.1477 0.4034 0.0329 1.0000 Uiso R . . . . . H361 H 0.6841 0.0995 0.5190 0.0413 1.0000 Uiso R . . . . . H371 H 0.6221 0.2527 0.6000 0.0426 1.0000 Uiso R . . . . . H381 H 0.6329 0.4541 0.5660 0.0495 1.0000 Uiso R . . . . . H391 H 0.7035 0.5059 0.4514 0.0410 1.0000 Uiso R . . . . . H411 H 0.5259 0.3494 0.3265 0.0271 1.0000 Uiso R . . . . . H421 H 0.3331 0.4696 0.2803 0.0344 1.0000 Uiso R . . . . . H431 H 0.3342 0.6631 0.2264 0.0340 1.0000 Uiso R . . . . . H441 H 0.5337 0.7362 0.2167 0.0313 1.0000 Uiso R . . . . . H451 H 0.7330 0.6140 0.2578 0.0275 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 V1 0.01529(10) 0.01347(9) 0.01304(10) 0.00083(7) -0.00191(7) -0.00159(7) P1 0.02188(16) 0.02093(15) 0.01434(15) 0.00196(12) -0.00211(12) -0.00677(13) P2 0.01718(15) 0.01611(14) 0.01785(15) 0.00168(12) -0.00363(12) -0.00282(12) P3 0.01648(15) 0.01599(14) 0.01607(15) 0.00131(11) -0.00120(12) -0.00247(11) N1 0.0221(5) 0.0191(5) 0.0146(5) 0.0017(4) -0.0030(4) -0.0066(4) N2 0.0175(5) 0.0151(5) 0.0184(5) 0.0011(4) -0.0041(4) -0.0017(4) N3 0.0164(5) 0.0166(5) 0.0170(5) -0.0006(4) -0.0020(4) -0.0029(4) C1 0.0283(7) 0.0226(6) 0.0160(6) 0.0019(5) -0.0061(5) -0.0090(5) C2 0.0282(7) 0.0302(7) 0.0264(7) 0.0014(6) -0.0080(6) -0.0114(6) C3 0.0404(9) 0.0262(7) 0.0250(7) -0.0043(6) -0.0096(6) -0.0083(6) C4 0.0291(7) 0.0215(6) 0.0135(6) 0.0014(5) -0.0021(5) -0.0095(5) C5 0.0285(7) 0.0225(6) 0.0271(7) 0.0006(5) -0.0009(6) -0.0084(6) C6 0.0356(8) 0.0235(7) 0.0315(8) 0.0001(6) -0.0017(6) -0.0021(6) C7 0.0548(11) 0.0193(6) 0.0277(8) -0.0005(6) -0.0033(7) -0.0095(7) C8 0.0527(10) 0.0284(7) 0.0337(8) 0.0027(6) -0.0076(7) -0.0241(7) C9 0.0355(8) 0.0315(7) 0.0277(7) 0.0029(6) -0.0089(6) -0.0168(6) C10 0.0193(6) 0.0292(7) 0.0198(6) -0.0008(5) -0.0023(5) -0.0074(5) C11 0.0270(7) 0.0401(8) 0.0219(7) 0.0024(6) 0.0002(6) -0.0061(6) C12 0.0354(9) 0.0625(12) 0.0258(8) -0.0002(8) 0.0080(7) -0.0076(8) C13 0.0298(9) 0.0613(12) 0.0381(10) -0.0149(9) 0.0075(7) -0.0030(8) C14 0.0331(9) 0.0393(9) 0.0506(11) -0.0086(8) -0.0027(8) 0.0049(7) C15 0.0339(8) 0.0324(8) 0.0313(8) 0.0002(6) -0.0033(6) -0.0035(6) C16 0.0250(7) 0.0153(5) 0.0252(7) 0.0035(5) -0.0092(5) -0.0028(5) C17 0.0303(7) 0.0195(6) 0.0343(8) -0.0057(6) -0.0090(6) -0.0008(5) C18 0.0312(8) 0.0243(7) 0.0413(9) 0.0007(6) -0.0061(7) -0.0125(6) C19 0.0164(6) 0.0208(6) 0.0192(6) -0.0005(5) -0.0048(5) -0.0049(5) C20 0.0253(7) 0.0238(6) 0.0249(7) 0.0009(5) -0.0006(5) -0.0085(5) C21 0.0272(7) 0.0349(8) 0.0292(8) -0.0039(6) 0.0071(6) -0.0113(6) C22 0.0202(7) 0.0321(7) 0.0333(8) -0.0109(6) -0.0009(6) -0.0014(6) C23 0.0249(7) 0.0250(6) 0.0253(7) -0.0030(5) -0.0092(6) 0.0003(5) C24 0.0208(6) 0.0249(6) 0.0200(6) 0.0012(5) -0.0050(5) -0.0032(5) C25 0.0195(6) 0.0181(6) 0.0185(6) -0.0005(5) -0.0031(5) -0.0024(5) C26 0.0228(7) 0.0360(8) 0.0217(7) 0.0000(6) -0.0040(5) -0.0106(6) C27 0.0289(7) 0.0441(9) 0.0209(7) -0.0022(6) -0.0069(6) -0.0122(7) C28 0.0304(8) 0.0353(8) 0.0181(6) -0.0028(6) -0.0008(5) -0.0076(6) C29 0.0219(7) 0.0337(7) 0.0239(7) -0.0012(6) 0.0016(5) -0.0074(6) C30 0.0198(6) 0.0268(6) 0.0216(6) -0.0001(5) -0.0042(5) -0.0043(5) C31 0.0227(6) 0.0175(6) 0.0194(6) -0.0035(5) -0.0022(5) -0.0028(5) C32 0.0427(9) 0.0279(7) 0.0241(7) -0.0034(6) -0.0132(6) -0.0079(6) C33 0.0281(7) 0.0203(6) 0.0268(7) -0.0016(5) -0.0033(6) -0.0080(5) C34 0.0175(6) 0.0247(6) 0.0181(6) 0.0022(5) -0.0007(5) -0.0027(5) C35 0.0235(7) 0.0252(7) 0.0249(7) 0.0032(5) 0.0027(5) -0.0032(5) C36 0.0301(8) 0.0340(8) 0.0309(8) 0.0128(6) 0.0039(6) -0.0043(6) C37 0.0312(8) 0.0543(10) 0.0195(7) 0.0081(7) 0.0022(6) -0.0116(7) C38 0.0471(10) 0.0525(10) 0.0235(8) -0.0100(7) 0.0085(7) -0.0183(8) C39 0.0436(9) 0.0312(8) 0.0255(7) -0.0035(6) 0.0059(7) -0.0122(7) C40 0.0171(6) 0.0170(5) 0.0171(6) -0.0016(4) -0.0013(5) -0.0022(4) C41 0.0212(6) 0.0184(6) 0.0263(7) 0.0010(5) -0.0030(5) -0.0055(5) C42 0.0206(7) 0.0255(7) 0.0395(8) 0.0006(6) -0.0083(6) -0.0078(5) C43 0.0225(7) 0.0231(6) 0.0362(8) 0.0014(6) -0.0126(6) -0.0021(5) C44 0.0272(7) 0.0191(6) 0.0319(8) 0.0056(5) -0.0107(6) -0.0054(5) C45 0.0201(6) 0.0200(6) 0.0270(7) 0.0025(5) -0.0051(5) -0.0062(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.17090(4) 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 V1 . P1 . 2.5049(4) yes V1 . P2 . 2.8337(4) yes V1 . P3 . 2.4542(4) yes V1 . N1 . 1.9286(11) yes V1 . N2 . 1.9488(10) yes V1 . N3 . 1.9347(11) yes P1 . N1 . 1.6551(11) yes P1 . C4 . 1.8239(13) yes P1 . C10 . 1.8266(14) yes P2 . N2 . 1.6756(11) yes P2 . C19 . 1.8428(13) yes P2 . C25 . 1.8350(13) yes P3 . N3 . 1.6446(11) yes P3 . C34 . 1.8290(13) yes P3 . C40 . 1.8189(13) yes N1 . C1 . 1.4757(17) yes N2 . C16 . 1.4770(16) yes N3 . C31 . 1.4746(16) yes C1 . C2 . 1.522(2) yes C1 . C3 . 1.5244(19) yes C1 . H11 . 0.994 no C2 . H21 . 0.964 no C2 . H22 . 0.957 no C2 . H23 . 0.973 no C3 . H31 . 0.970 no C3 . H32 . 0.968 no C3 . H33 . 0.980 no C4 . C5 . 1.388(2) yes C4 . C9 . 1.3976(19) yes C5 . C6 . 1.389(2) yes C5 . H51 . 0.934 no C6 . C7 . 1.382(2) yes C6 . H61 . 0.947 no C7 . C8 . 1.373(3) yes C7 . H71 . 0.944 no C8 . C9 . 1.388(2) yes C8 . H81 . 0.933 no C9 . H91 . 0.929 no C10 . C11 . 1.391(2) yes C10 . C15 . 1.396(2) yes C11 . C12 . 1.389(2) yes C11 . H111 . 0.955 no C12 . C13 . 1.371(3) yes C12 . H121 . 0.934 no C13 . C14 . 1.388(3) yes C13 . H131 . 0.940 no C14 . C15 . 1.381(2) yes C14 . H141 . 0.917 no C15 . H151 . 0.934 no C16 . C17 . 1.525(2) yes C16 . C18 . 1.522(2) yes C16 . H161 . 0.987 no C17 . H171 . 0.963 no C17 . H172 . 0.967 no C17 . H173 . 0.964 no C18 . H181 . 0.964 no C18 . H182 . 0.975 no C18 . H183 . 0.967 no C19 . C20 . 1.3930(18) yes C19 . C24 . 1.4006(18) yes C20 . C21 . 1.391(2) yes C20 . H201 . 0.920 no C21 . C22 . 1.383(2) yes C21 . H211 . 0.941 no C22 . C23 . 1.384(2) yes C22 . H221 . 0.953 no C23 . C24 . 1.3886(19) yes C23 . H231 . 0.943 no C24 . H241 . 0.962 no C25 . C26 . 1.3973(19) yes C25 . C30 . 1.3895(18) yes C26 . C27 . 1.388(2) yes C26 . H261 . 0.958 no C27 . C28 . 1.389(2) yes C27 . H271 . 0.950 no C28 . C29 . 1.382(2) yes C28 . H281 . 0.954 no C29 . C30 . 1.392(2) yes C29 . H291 . 0.944 no C30 . H301 . 0.930 no C31 . C32 . 1.5214(19) yes C31 . C33 . 1.5198(19) yes C31 . H311 . 0.985 no C32 . H321 . 0.959 no C32 . H322 . 0.972 no C32 . H323 . 0.965 no C33 . H331 . 0.966 no C33 . H332 . 0.966 no C33 . H333 . 0.979 no C34 . C35 . 1.3894(19) yes C34 . C39 . 1.393(2) yes C35 . C36 . 1.394(2) yes C35 . H351 . 0.957 no C36 . C37 . 1.377(2) yes C36 . H361 . 0.944 no C37 . C38 . 1.381(3) yes C37 . H371 . 0.933 no C38 . C39 . 1.389(2) yes C38 . H381 . 0.928 no C39 . H391 . 0.940 no C40 . C41 . 1.3969(18) yes C40 . C45 . 1.3937(17) yes C41 . C42 . 1.3839(19) yes C41 . H411 . 0.959 no C42 . C43 . 1.384(2) yes C42 . H421 . 0.935 no C43 . C44 . 1.386(2) yes C43 . H431 . 0.949 no C44 . C45 . 1.3905(19) yes C44 . H441 . 0.938 no C45 . H451 . 0.939 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 P1 . V1 . P2 . 100.033(13) yes P1 . V1 . P3 . 134.470(14) yes P2 . V1 . P3 . 118.326(13) yes P1 . V1 . N1 . 41.33(3) yes P2 . V1 . N1 . 130.57(3) yes P3 . V1 . N1 . 110.86(4) yes P1 . V1 . N2 . 111.45(3) yes P2 . V1 . N2 . 35.24(3) yes P3 . V1 . N2 . 114.03(3) yes N1 . V1 . N2 . 117.87(5) yes P1 . V1 . N3 . 111.13(3) yes P2 . V1 . N3 . 100.65(3) yes P3 . V1 . N3 . 41.96(3) yes N1 . V1 . N3 . 119.65(5) yes N2 . V1 . N3 . 122.48(5) yes V1 . P1 . N1 . 50.32(4) yes V1 . P1 . C4 . 123.56(4) yes N1 . P1 . C4 . 109.99(6) yes V1 . P1 . C10 . 132.12(5) yes N1 . P1 . C10 . 110.24(6) yes C4 . P1 . C10 . 103.83(6) yes V1 . P2 . C19 . 135.89(4) yes N2 . P2 . C19 . 106.65(6) yes V1 . P2 . C25 . 116.31(4) yes N2 . P2 . C25 . 106.26(6) yes C19 . P2 . C25 . 100.62(6) yes V1 . P3 . N3 . 51.86(4) yes V1 . P3 . C34 . 134.05(4) yes N3 . P3 . C34 . 113.57(6) yes V1 . P3 . C40 . 124.03(4) yes N3 . P3 . C40 . 109.81(6) yes C34 . P3 . C40 . 101.85(6) yes P1 . N1 . V1 . 88.35(5) yes P1 . N1 . C1 . 128.93(9) yes V1 . N1 . C1 . 142.53(9) yes P2 . N2 . V1 . 102.60(5) yes P2 . N2 . C16 . 122.86(8) yes V1 . N2 . C16 . 134.25(9) yes V1 . N3 . P3 . 86.17(5) yes V1 . N3 . C31 . 142.34(9) yes P3 . N3 . C31 . 131.45(9) yes N1 . C1 . C2 . 110.30(11) yes N1 . C1 . C3 . 109.52(11) yes C2 . C1 . C3 . 110.11(12) yes N1 . C1 . H11 . 109.1 no C2 . C1 . H11 . 109.4 no C3 . C1 . H11 . 108.4 no C1 . C2 . H21 . 111.9 no C1 . C2 . H22 . 109.8 no H21 . C2 . H22 . 108.2 no C1 . C2 . H23 . 110.5 no H21 . C2 . H23 . 107.3 no H22 . C2 . H23 . 109.0 no C1 . C3 . H31 . 111.0 no C1 . C3 . H32 . 109.9 no H31 . C3 . H32 . 109.2 no C1 . C3 . H33 . 109.0 no H31 . C3 . H33 . 108.3 no H32 . C3 . H33 . 109.4 no P1 . C4 . C5 . 120.91(10) yes P1 . C4 . C9 . 120.15(11) yes C5 . C4 . C9 . 118.34(13) yes C4 . C5 . C6 . 120.92(14) yes C4 . C5 . H51 . 120.1 no C6 . C5 . H51 . 119.0 no C5 . C6 . C7 . 119.95(15) yes C5 . C6 . H61 . 120.1 no C7 . C6 . H61 . 119.9 no C6 . C7 . C8 . 119.85(14) yes C6 . C7 . H71 . 119.3 no C8 . C7 . H71 . 120.8 no C7 . C8 . C9 . 120.53(14) yes C7 . C8 . H81 . 120.2 no C9 . C8 . H81 . 119.2 no C4 . C9 . C8 . 120.40(15) yes C4 . C9 . H91 . 120.1 no C8 . C9 . H91 . 119.6 no P1 . C10 . C11 . 124.65(11) yes P1 . C10 . C15 . 116.64(11) yes C11 . C10 . C15 . 118.70(14) yes C10 . C11 . C12 . 120.19(15) yes C10 . C11 . H111 . 119.9 no C12 . C11 . H111 . 119.9 no C11 . C12 . C13 . 120.73(16) yes C11 . C12 . H121 . 120.1 no C13 . C12 . H121 . 119.1 no C12 . C13 . C14 . 119.59(16) yes C12 . C13 . H131 . 120.8 no C14 . C13 . H131 . 119.6 no C13 . C14 . C15 . 120.25(17) yes C13 . C14 . H141 . 120.3 no C15 . C14 . H141 . 119.4 no C10 . C15 . C14 . 120.52(16) yes C10 . C15 . H151 . 119.3 no C14 . C15 . H151 . 120.2 no N2 . C16 . C17 . 110.11(11) yes N2 . C16 . C18 . 110.90(11) yes C17 . C16 . C18 . 110.20(12) yes N2 . C16 . H161 . 108.6 no C17 . C16 . H161 . 109.5 no C18 . C16 . H161 . 107.5 no C16 . C17 . H171 . 109.9 no C16 . C17 . H172 . 109.3 no H171 . C17 . H172 . 108.1 no C16 . C17 . H173 . 112.2 no H171 . C17 . H173 . 107.8 no H172 . C17 . H173 . 109.5 no C16 . C18 . H181 . 110.8 no C16 . C18 . H182 . 110.2 no H181 . C18 . H182 . 108.0 no C16 . C18 . H183 . 110.5 no H181 . C18 . H183 . 107.7 no H182 . C18 . H183 . 109.5 no P2 . C19 . C20 . 117.44(10) yes P2 . C19 . C24 . 124.08(10) yes C20 . C19 . C24 . 118.35(12) yes C19 . C20 . C21 . 120.73(13) yes C19 . C20 . H201 . 119.1 no C21 . C20 . H201 . 120.2 no C20 . C21 . C22 . 120.28(14) yes C20 . C21 . H211 . 118.8 no C22 . C21 . H211 . 120.9 no C21 . C22 . C23 . 119.69(13) yes C21 . C22 . H221 . 119.4 no C23 . C22 . H221 . 120.9 no C22 . C23 . C24 . 120.30(13) yes C22 . C23 . H231 . 119.8 no C24 . C23 . H231 . 119.9 no C19 . C24 . C23 . 120.63(13) yes C19 . C24 . H241 . 119.9 no C23 . C24 . H241 . 119.5 no P2 . C25 . C26 . 120.01(10) yes P2 . C25 . C30 . 121.23(10) yes C26 . C25 . C30 . 118.26(12) yes C25 . C26 . C27 . 120.82(13) yes C25 . C26 . H261 . 119.5 no C27 . C26 . H261 . 119.7 no C26 . C27 . C28 . 120.08(14) yes C26 . C27 . H271 . 120.1 no C28 . C27 . H271 . 119.8 no C27 . C28 . C29 . 119.74(13) yes C27 . C28 . H281 . 119.7 no C29 . C28 . H281 . 120.5 no C28 . C29 . C30 . 120.02(13) yes C28 . C29 . H291 . 120.8 no C30 . C29 . H291 . 119.2 no C29 . C30 . C25 . 121.06(13) yes C29 . C30 . H301 . 119.7 no C25 . C30 . H301 . 119.3 no N3 . C31 . C32 . 110.12(11) yes N3 . C31 . C33 . 110.00(11) yes C32 . C31 . C33 . 110.65(12) yes N3 . C31 . H311 . 107.6 no C32 . C31 . H311 . 110.0 no C33 . C31 . H311 . 108.4 no C31 . C32 . H321 . 110.5 no C31 . C32 . H322 . 110.0 no H321 . C32 . H322 . 108.3 no C31 . C32 . H323 . 110.1 no H321 . C32 . H323 . 108.1 no H322 . C32 . H323 . 109.8 no C31 . C33 . H331 . 110.5 no C31 . C33 . H332 . 110.3 no H331 . C33 . H332 . 107.7 no C31 . C33 . H333 . 111.9 no H331 . C33 . H333 . 109.2 no H332 . C33 . H333 . 107.2 no P3 . C34 . C35 . 120.15(11) yes P3 . C34 . C39 . 121.21(11) yes C35 . C34 . C39 . 118.64(13) yes C34 . C35 . C36 . 120.77(14) yes C34 . C35 . H351 . 120.0 no C36 . C35 . H351 . 119.3 no C35 . C36 . C37 . 119.85(15) yes C35 . C36 . H361 . 119.8 no C37 . C36 . H361 . 120.3 no C36 . C37 . C38 . 120.06(14) yes C36 . C37 . H371 . 120.0 no C38 . C37 . H371 . 120.0 no C37 . C38 . C39 . 120.27(16) yes C37 . C38 . H381 . 120.0 no C39 . C38 . H381 . 119.7 no C34 . C39 . C38 . 120.39(15) yes C34 . C39 . H391 . 120.1 no C38 . C39 . H391 . 119.5 no P3 . C40 . C41 . 119.62(9) yes P3 . C40 . C45 . 121.34(10) yes C41 . C40 . C45 . 118.72(12) yes C40 . C41 . C42 . 120.70(12) yes C40 . C41 . H411 . 120.2 no C42 . C41 . H411 . 119.1 no C41 . C42 . C43 . 120.09(13) yes C41 . C42 . H421 . 120.0 no C43 . C42 . H421 . 119.9 no C42 . C43 . C44 . 119.95(13) yes C42 . C43 . H431 . 119.8 no C44 . C43 . H431 . 120.2 no C43 . C44 . C45 . 120.04(12) yes C43 . C44 . H441 . 119.6 no C45 . C44 . H441 . 120.3 no C40 . C45 . C44 . 120.46(12) yes C40 . C45 . H451 . 120.0 no C44 . C45 . H451 . 119.5 no _iucr_refine_instructions_details_constraints ; # # Punched on 20/09/12 at 10:22:58 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S) H ( 323,X'S) RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 20/09/12 at 10:22:58 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 938607' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_3 _audit_creation_date 2013-02-19 _audit_creation_method CRYSTALS_ver_14.52 _vrf_PLAT420_3 ; PROBLEM: D-H Without Acceptor *O1 - *H514 ... ? RESPONSE: The THF solvate molecule which contains atom O1 is disordered about a center of symmetry. Atoms H511 and H512, attached to C51, are associated with orientation 1 for O1, while H513 and H514 are associated with orientation 2 of O1. H514 is too near atom O1 in the asymmetric unit, and generates an H-bonding ALERT. However, H514 is assocaited only with the symmetry-related atom O1. There is no method to inform CheckCIF/PLATON of the details of the disorder, so it raises a false flag for this item. ; _oxford_structure_analysis_title 'sk_803_0m in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.7003(3) _cell_length_b 22.3479(5) _cell_length_c 22.5190(5) _cell_angle_alpha 62.0010(10) _cell_angle_beta 81.3130(10) _cell_angle_gamma 88.6370(10) _cell_volume 4693.3(2) _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' 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' V 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780 1.2199 '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' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 '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 4 # Given Formula = C48 H57 Fe1 I1 N3 O0.75 P3 V1 # Dc = 1.44 Fooo = 2076.00 Mu = 13.06 M = 2029.23 # Found Formula = C48 H57 Fe1 I1 N3 O0.75 P3 V1 # Dc = 1.44 FOOO = 2076.00 Mu = 13.06 M = 2029.23 _chemical_formula_sum 'C48 H57 Fe1 I1 N3 O0.75 P3 V1' _chemical_formula_moiety 'C48 H57 Fe1 I1 N3 O0.75 P3 V1' _chemical_compound_source ? _chemical_formula_weight 1014.61 _cell_measurement_reflns_used 9976 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_min 0.120 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_max 0.270 _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2076 _exptl_absorpt_coefficient_mu 1.306 # Sheldrick geometric approximatio 0.74 0.85 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.85 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _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 120 _diffrn_reflns_number 90229 _reflns_number_total 24941 _diffrn_reflns_av_R_equivalents 0.046 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 24941 # Theoretical number of reflections is about 50057 _diffrn_reflns_theta_min 2.455 _diffrn_reflns_theta_max 29.029 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.029 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -26 _reflns_limit_k_max 30 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.04 _refine_diff_density_max 1.49 # 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>-10.0\s(I) _refine_ls_number_reflns 24941 _refine_ls_number_restraints 0 _refine_ls_number_parameters 1039 _oxford_refine_ls_R_factor_ref 0.0550 _refine_ls_wR_factor_ref 0.0802 _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_shift/su_max 0.0025477 _refine_ls_shift/su_mean 0.0000502 # The values computed with all filters except I/sigma _oxford_reflns_number_all 24941 _refine_ls_R_factor_all 0.0550 _refine_ls_wR_factor_all 0.0802 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 19306 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_gt 0.0756 # 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 #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^) + ( 0.03P)^2^ + 4.98P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Fe1 Fe 0.61345(3) 0.714193(16) 0.018624(16) 0.0128 1.0000 Uani . . . . . . Fe101 Fe 0.93961(3) 0.762375(17) 0.450903(16) 0.0139 1.0000 Uani . . . . . . V1 V 0.78394(4) 0.766318(19) -0.037451(19) 0.0139 1.0000 Uani . . . . . . V101 V 1.09416(4) 0.80842(2) 0.460982(19) 0.0142 1.0000 Uani . . . . . . I1 I 0.395091(15) 0.648465(8) 0.093446(8) 0.0210 1.0000 Uani . . . . . . I101 I 0.744599(16) 0.704417(10) 0.435246(9) 0.0272 1.0000 Uani . . . . . . P1 P 0.63850(6) 0.70452(3) -0.07841(3) 0.0142 1.0000 Uani . . . . . . P2 P 0.76553(6) 0.65477(3) 0.08095(3) 0.0175 1.0000 Uani . . . . . . P3 P 0.59039(6) 0.82537(3) -0.00114(3) 0.0162 1.0000 Uani . . . . . . P101 P 0.95057(6) 0.87150(3) 0.36507(3) 0.0166 1.0000 Uani . . . . . . P102 P 1.10458(6) 0.69146(3) 0.45588(3) 0.0192 1.0000 Uani . . . . . . P103 P 0.88752(6) 0.76383(3) 0.55164(3) 0.0156 1.0000 Uani . . . . . . O1 O 0.4832(5) 0.5278(3) 0.4239(3) 0.0535(13) 0.5000 Uiso . . . . . . O2 O 0.57462(19) 0.34514(10) 0.35388(11) 0.0355 1.0000 Uani . . . . . . N1 N 0.76738(18) 0.75742(10) -0.11695(9) 0.0154 1.0000 Uani . . . . . . N2 N 0.88771(19) 0.70502(10) 0.02542(10) 0.0182 1.0000 Uani . . . . . . N3 N 0.74053(19) 0.85043(10) -0.03840(10) 0.0163 1.0000 Uani . . . . . . N101 N 1.07772(19) 0.89599(10) 0.38489(10) 0.0178 1.0000 Uani . . . . . . N102 N 1.21274(19) 0.74678(10) 0.45229(10) 0.0180 1.0000 Uani . . . . . . N103 N 1.02737(18) 0.79614(10) 0.55106(10) 0.0170 1.0000 Uani . . . . . . C1 C 0.8306(2) 0.77850(13) -0.18710(12) 0.0201 1.0000 Uani . . . . . . C2 C 0.9727(3) 0.78907(16) -0.19282(15) 0.0326 1.0000 Uani . . . . . . C3 C 0.7764(3) 0.84269(14) -0.23805(13) 0.0307 1.0000 Uani . . . . . . C4 C 0.6816(2) 0.62534(11) -0.07862(11) 0.0149 1.0000 Uani . . . . . . C5 C 0.8064(2) 0.60623(12) -0.07525(12) 0.0193 1.0000 Uani . . . . . . C6 C 0.8399(3) 0.54384(13) -0.07043(13) 0.0240 1.0000 Uani . . . . . . C7 C 0.7485(3) 0.50073(13) -0.06991(13) 0.0244 1.0000 Uani . . . . . . C8 C 0.6244(3) 0.51882(13) -0.07281(13) 0.0251 1.0000 Uani . . . . . . C9 C 0.5908(2) 0.58021(12) -0.07628(12) 0.0203 1.0000 Uani . . . . . . C10 C 0.5149(2) 0.73192(12) -0.13230(12) 0.0169 1.0000 Uani . . . . . . C11 C 0.5273(2) 0.72750(13) -0.19280(12) 0.0222 1.0000 Uani . . . . . . C12 C 0.4345(3) 0.75215(14) -0.23467(13) 0.0259 1.0000 Uani . . . . . . C13 C 0.3285(3) 0.77935(13) -0.21547(14) 0.0259 1.0000 Uani . . . . . . C14 C 0.3153(2) 0.78333(13) -0.15555(13) 0.0243 1.0000 Uani . . . . . . C15 C 0.4079(2) 0.75969(12) -0.11392(12) 0.0191 1.0000 Uani . . . . . . C16 C 1.0238(2) 0.69538(13) 0.03033(13) 0.0224 1.0000 Uani . . . . . . C17 C 1.0935(3) 0.76381(14) 0.00290(16) 0.0301 1.0000 Uani . . . . . . C18 C 1.0803(2) 0.65726(14) -0.00735(15) 0.0276 1.0000 Uani . . . . . . C19 C 0.7557(2) 0.66240(13) 0.15825(12) 0.0212 1.0000 Uani . . . . . . C20 C 0.8283(3) 0.71143(15) 0.16188(15) 0.0302 1.0000 Uani . . . . . . C21 C 0.8115(3) 0.71853(17) 0.22051(17) 0.0380 1.0000 Uani . . . . . . C22 C 0.7221(3) 0.67808(17) 0.27539(15) 0.0373 1.0000 Uani . . . . . . C23 C 0.6483(3) 0.63019(15) 0.27189(14) 0.0331 1.0000 Uani . . . . . . C24 C 0.6652(3) 0.62233(14) 0.21369(13) 0.0259 1.0000 Uani . . . . . . C25 C 0.7956(2) 0.56505(12) 0.11206(12) 0.0186 1.0000 Uani . . . . . . C26 C 0.8803(2) 0.53288(13) 0.15831(13) 0.0230 1.0000 Uani . . . . . . C27 C 0.9000(3) 0.46436(14) 0.18219(14) 0.0280 1.0000 Uani . . . . . . C28 C 0.8362(3) 0.42699(14) 0.16042(14) 0.0306 1.0000 Uani . . . . . . C29 C 0.7522(3) 0.45831(14) 0.11496(14) 0.0296 1.0000 Uani . . . . . . C30 C 0.7312(3) 0.52647(13) 0.09152(13) 0.0247 1.0000 Uani . . . . . . C31 C 0.8057(2) 0.91753(12) -0.06331(12) 0.0200 1.0000 Uani . . . . . . C32 C 0.9032(3) 0.93263(13) -0.12595(14) 0.0282 1.0000 Uani . . . . . . C33 C 0.8675(3) 0.91965(14) -0.00790(14) 0.0293 1.0000 Uani . . . . . . C34 C 0.4880(2) 0.88116(12) -0.06044(13) 0.0199 1.0000 Uani . . . . . . C35 C 0.5304(3) 0.91362(13) -0.13037(14) 0.0261 1.0000 Uani . . . . . . C36 C 0.4480(3) 0.95200(15) -0.17528(16) 0.0353 1.0000 Uani . . . . . . C37 C 0.3250(3) 0.95753(16) -0.15046(18) 0.0406 1.0000 Uani . . . . . . C38 C 0.2815(3) 0.92472(16) -0.08145(19) 0.0393 1.0000 Uani . . . . . . C39 C 0.3628(3) 0.88670(14) -0.03616(16) 0.0293 1.0000 Uani . . . . . . C40 C 0.5520(2) 0.84453(12) 0.06957(12) 0.0197 1.0000 Uani . . . . . . C41 C 0.5470(3) 0.91127(13) 0.05860(13) 0.0248 1.0000 Uani . . . . . . C42 C 0.5246(3) 0.92495(14) 0.11315(15) 0.0300 1.0000 Uani . . . . . . C43 C 0.5060(3) 0.87199(15) 0.17870(15) 0.0338 1.0000 Uani . . . . . . C44 C 0.5077(3) 0.80562(16) 0.19055(15) 0.0376 1.0000 Uani . . . . . . C45 C 0.5317(3) 0.79165(14) 0.13589(14) 0.0271 1.0000 Uani . . . . . . C46 C 0.5450(3) 0.37511(15) 0.28655(16) 0.0355 1.0000 Uani . . . . . . C47 C 0.5442(3) 0.45036(15) 0.26294(15) 0.0347 1.0000 Uani . . . . . . C48 C 0.5039(3) 0.45440(15) 0.32903(15) 0.0336 1.0000 Uani . . . . . . C49 C 0.5045(3) 0.38154(15) 0.38467(15) 0.0326 1.0000 Uani . . . . . . C51 C 0.5799(6) 0.5313(3) 0.4575(2) 0.0946 1.0000 Uani . . . . . . C101 C 1.1315(2) 0.96587(12) 0.35643(13) 0.0222 1.0000 Uani . . . . . . C102 C 1.2734(3) 0.96464(15) 0.35834(16) 0.0334 1.0000 Uani . . . . . . C103 C 1.0657(3) 1.00089(13) 0.39579(14) 0.0275 1.0000 Uani . . . . . . C104 C 0.9926(2) 0.88232(12) 0.27860(12) 0.0195 1.0000 Uani . . . . . . C105 C 1.1176(3) 0.88093(14) 0.25171(14) 0.0292 1.0000 Uani . . . . . . C106 C 1.1480(3) 0.88393(15) 0.18790(15) 0.0366 1.0000 Uani . . . . . . C107 C 1.0530(3) 0.88784(15) 0.15089(15) 0.0368 1.0000 Uani . . . . . . C108 C 0.9291(3) 0.88881(15) 0.17733(15) 0.0357 1.0000 Uani . . . . . . C109 C 0.8978(3) 0.88553(14) 0.24106(13) 0.0270 1.0000 Uani . . . . . . C110 C 0.8268(2) 0.93186(13) 0.35223(12) 0.0198 1.0000 Uani . . . . . . C111 C 0.8460(3) 0.99947(14) 0.30059(14) 0.0259 1.0000 Uani . . . . . . C112 C 0.7526(3) 1.04482(15) 0.29306(15) 0.0324 1.0000 Uani . . . . . . C113 C 0.6373(3) 1.02390(16) 0.33492(15) 0.0349 1.0000 Uani . . . . . . C114 C 0.6147(3) 0.95692(17) 0.38499(15) 0.0363 1.0000 Uani . . . . . . C115 C 0.7098(2) 0.91099(15) 0.39381(13) 0.0261 1.0000 Uani . . . . . . C116 C 1.3519(2) 0.74363(14) 0.44253(13) 0.0221 1.0000 Uani . . . . . . C117 C 1.4075(2) 0.77569(14) 0.47994(14) 0.0245 1.0000 Uani . . . . . . C118 C 1.4062(3) 0.78034(17) 0.36666(14) 0.0345 1.0000 Uani . . . . . . C119 C 1.1156(2) 0.61061(13) 0.53082(13) 0.0218 1.0000 Uani . . . . . . C120 C 1.1718(2) 0.60706(14) 0.58417(13) 0.0251 1.0000 Uani . . . . . . C121 C 1.1682(3) 0.54605(15) 0.64398(14) 0.0296 1.0000 Uani . . . . . . C122 C 1.1093(3) 0.48833(15) 0.65110(15) 0.0343 1.0000 Uani . . . . . . C123 C 1.0523(3) 0.49127(15) 0.59895(16) 0.0364 1.0000 Uani . . . . . . C124 C 1.0549(3) 0.55168(14) 0.53923(15) 0.0311 1.0000 Uani . . . . . . C125 C 1.1490(3) 0.67160(14) 0.38583(14) 0.0249 1.0000 Uani . . . . . . C126 C 1.2458(3) 0.62843(18) 0.38680(17) 0.0409 1.0000 Uani . . . . . . C127 C 1.2841(3) 0.61799(19) 0.33063(18) 0.0448 1.0000 Uani . . . . . . C128 C 1.2260(3) 0.64977(18) 0.27406(16) 0.0406 1.0000 Uani . . . . . . C129 C 1.1290(3) 0.69198(17) 0.27273(15) 0.0389 1.0000 Uani . . . . . . C130 C 1.0900(3) 0.70263(14) 0.32856(14) 0.0278 1.0000 Uani . . . . . . C131 C 1.0696(2) 0.80173(13) 0.60744(12) 0.0193 1.0000 Uani . . . . . . C132 C 1.1581(2) 0.86371(13) 0.58211(15) 0.0251 1.0000 Uani . . . . . . C133 C 1.1346(3) 0.73839(14) 0.65251(13) 0.0258 1.0000 Uani . . . . . . C134 C 0.7653(2) 0.81828(13) 0.56149(12) 0.0185 1.0000 Uani . . . . . . C135 C 0.7933(3) 0.88508(14) 0.54521(14) 0.0254 1.0000 Uani . . . . . . C136 C 0.6972(3) 0.92785(15) 0.54589(15) 0.0311 1.0000 Uani . . . . . . C137 C 0.5720(3) 0.90421(16) 0.56282(15) 0.0317 1.0000 Uani . . . . . . C138 C 0.5424(3) 0.83780(15) 0.57939(13) 0.0275 1.0000 Uani . . . . . . C139 C 0.6379(2) 0.79469(14) 0.57895(13) 0.0226 1.0000 Uani . . . . . . C140 C 0.8446(2) 0.68379(12) 0.62939(12) 0.0180 1.0000 Uani . . . . . . C141 C 0.8161(3) 0.68139(13) 0.69350(12) 0.0234 1.0000 Uani . . . . . . C142 C 0.7880(3) 0.61944(14) 0.75175(13) 0.0254 1.0000 Uani . . . . . . C143 C 0.7923(3) 0.55953(14) 0.74763(13) 0.0267 1.0000 Uani . . . . . . C144 C 0.8212(3) 0.56134(14) 0.68496(14) 0.0268 1.0000 Uani . . . . . . C145 C 0.8470(2) 0.62350(13) 0.62574(13) 0.0206 1.0000 Uani . . . . . . C500 C 0.3947(9) 0.4765(5) 0.4743(4) 0.061(2) 0.5000 Uiso . . . . . . C501 C 0.5313(11) 0.5210(5) 0.5213(5) 0.075(3) 0.5000 Uiso . . . . . . H11 H 0.8150 0.7415 -0.1969 0.0234 1.0000 Uiso R . . . . . H21 H 1.0082 0.7471 -0.1655 0.0484 1.0000 Uiso R . . . . . H22 H 0.9891 0.8218 -0.1775 0.0486 1.0000 Uiso R . . . . . H23 H 1.0122 0.8055 -0.2389 0.0487 1.0000 Uiso R . . . . . H31 H 0.6849 0.8379 -0.2333 0.0463 1.0000 Uiso R . . . . . H32 H 0.7971 0.8810 -0.2323 0.0454 1.0000 Uiso R . . . . . H33 H 0.8101 0.8531 -0.2839 0.0457 1.0000 Uiso R . . . . . H51 H 0.8669 0.6355 -0.0753 0.0223 1.0000 Uiso R . . . . . H61 H 0.9215 0.5311 -0.0674 0.0291 1.0000 Uiso R . . . . . H71 H 0.7718 0.4598 -0.0677 0.0287 1.0000 Uiso R . . . . . H81 H 0.5648 0.4899 -0.0730 0.0301 1.0000 Uiso R . . . . . H91 H 0.5088 0.5922 -0.0770 0.0254 1.0000 Uiso R . . . . . H111 H 0.5981 0.7086 -0.2052 0.0267 1.0000 Uiso R . . . . . H121 H 0.4424 0.7499 -0.2752 0.0318 1.0000 Uiso R . . . . . H131 H 0.2665 0.7952 -0.2430 0.0307 1.0000 Uiso R . . . . . H141 H 0.2453 0.8025 -0.1427 0.0280 1.0000 Uiso R . . . . . H151 H 0.3996 0.7616 -0.0730 0.0238 1.0000 Uiso R . . . . . H161 H 1.0305 0.6689 0.0782 0.0270 1.0000 Uiso R . . . . . H171 H 1.0606 0.7857 0.0286 0.0443 1.0000 Uiso R . . . . . H172 H 1.1804 0.7572 0.0053 0.0451 1.0000 Uiso R . . . . . H173 H 1.0836 0.7925 -0.0446 0.0447 1.0000 Uiso R . . . . . H181 H 1.0736 0.6839 -0.0552 0.0406 1.0000 Uiso R . . . . . H182 H 1.1675 0.6508 -0.0021 0.0409 1.0000 Uiso R . . . . . H183 H 1.0364 0.6140 0.0105 0.0404 1.0000 Uiso R . . . . . H201 H 0.8874 0.7405 0.1238 0.0359 1.0000 Uiso R . . . . . H211 H 0.8593 0.7506 0.2236 0.0452 1.0000 Uiso R . . . . . H221 H 0.7118 0.6837 0.3145 0.0434 1.0000 Uiso R . . . . . H231 H 0.5888 0.6023 0.3091 0.0399 1.0000 Uiso R . . . . . H241 H 0.6174 0.5894 0.2112 0.0307 1.0000 Uiso R . . . . . H261 H 0.9231 0.5577 0.1734 0.0277 1.0000 Uiso R . . . . . H271 H 0.9567 0.4426 0.2123 0.0340 1.0000 Uiso R . . . . . H281 H 0.8485 0.3815 0.1766 0.0371 1.0000 Uiso R . . . . . H291 H 0.7092 0.4338 0.1004 0.0351 1.0000 Uiso R . . . . . H301 H 0.6728 0.5468 0.0623 0.0296 1.0000 Uiso R . . . . . H311 H 0.7423 0.9515 -0.0755 0.0239 1.0000 Uiso R . . . . . H321 H 0.9652 0.8992 -0.1165 0.0415 1.0000 Uiso R . . . . . H322 H 0.9433 0.9765 -0.1439 0.0415 1.0000 Uiso R . . . . . H323 H 0.8603 0.9332 -0.1603 0.0418 1.0000 Uiso R . . . . . H331 H 0.8063 0.9091 0.0320 0.0437 1.0000 Uiso R . . . . . H332 H 0.9333 0.8880 0.0031 0.0437 1.0000 Uiso R . . . . . H333 H 0.9051 0.9643 -0.0250 0.0438 1.0000 Uiso R . . . . . H351 H 0.6140 0.9101 -0.1468 0.0308 1.0000 Uiso R . . . . . H361 H 0.4778 0.9746 -0.2226 0.0427 1.0000 Uiso R . . . . . H371 H 0.2697 0.9838 -0.1804 0.0492 1.0000 Uiso R . . . . . H381 H 0.2001 0.9286 -0.0649 0.0474 1.0000 Uiso R . . . . . H391 H 0.3353 0.8656 0.0104 0.0337 1.0000 Uiso R . . . . . H411 H 0.5595 0.9467 0.0145 0.0300 1.0000 Uiso R . . . . . H421 H 0.5243 0.9695 0.1052 0.0351 1.0000 Uiso R . . . . . H431 H 0.4908 0.8815 0.2149 0.0399 1.0000 Uiso R . . . . . H441 H 0.4953 0.7705 0.2344 0.0448 1.0000 Uiso R . . . . . H451 H 0.5344 0.7467 0.1437 0.0321 1.0000 Uiso R . . . . . H461 H 0.6118 0.3641 0.2579 0.0435 1.0000 Uiso R . . . . . H462 H 0.4608 0.3574 0.2867 0.0435 1.0000 Uiso R . . . . . H471 H 0.6287 0.4713 0.2426 0.0424 1.0000 Uiso R . . . . . H472 H 0.4857 0.4723 0.2300 0.0425 1.0000 Uiso R . . . . . H481 H 0.5631 0.4834 0.3337 0.0402 1.0000 Uiso R . . . . . H482 H 0.4192 0.4708 0.3305 0.0394 1.0000 Uiso R . . . . . H491 H 0.5469 0.3788 0.4221 0.0392 1.0000 Uiso R . . . . . H492 H 0.4183 0.3608 0.4029 0.0391 1.0000 Uiso R . . . . . H511 H 0.6228 0.5748 0.4326 0.1104 0.5000 Uiso R . . . . . H512 H 0.6376 0.4974 0.4602 0.1104 0.5000 Uiso R . . . . . H513 H 0.6506 0.5203 0.4341 0.1104 0.5000 Uiso R . . . . . H514 H 0.5577 0.5762 0.4294 0.1104 0.5000 Uiso R . . . . . H1011 H 1.1176 0.9905 0.3096 0.0269 1.0000 Uiso R . . . . . H1021 H 1.2884 0.9381 0.4056 0.0493 1.0000 Uiso R . . . . . H1022 H 1.3078 1.0103 0.3402 0.0491 1.0000 Uiso R . . . . . H1023 H 1.3125 0.9443 0.3316 0.0495 1.0000 Uiso R . . . . . H1031 H 1.0774 0.9753 0.4431 0.0405 1.0000 Uiso R . . . . . H1032 H 1.1041 1.0470 0.3763 0.0414 1.0000 Uiso R . . . . . H1033 H 0.9768 1.0031 0.3923 0.0407 1.0000 Uiso R . . . . . H1051 H 1.1826 0.8778 0.2770 0.0349 1.0000 Uiso R . . . . . H1061 H 1.2322 0.8828 0.1708 0.0445 1.0000 Uiso R . . . . . H1071 H 1.0732 0.8904 0.1083 0.0438 1.0000 Uiso R . . . . . H1081 H 0.8638 0.8919 0.1523 0.0426 1.0000 Uiso R . . . . . H1091 H 0.8118 0.8850 0.2590 0.0321 1.0000 Uiso R . . . . . H1111 H 0.9220 1.0130 0.2718 0.0309 1.0000 Uiso R . . . . . H1121 H 0.7653 1.0896 0.2589 0.0393 1.0000 Uiso R . . . . . H1131 H 0.5732 1.0548 0.3295 0.0422 1.0000 Uiso R . . . . . H1141 H 0.5369 0.9422 0.4123 0.0423 1.0000 Uiso R . . . . . H1151 H 0.6950 0.8657 0.4276 0.0304 1.0000 Uiso R . . . . . H1161 H 1.3734 0.6957 0.4622 0.0268 1.0000 Uiso R . . . . . H1171 H 1.3825 0.8226 0.4637 0.0368 1.0000 Uiso R . . . . . H1172 H 1.4992 0.7760 0.4721 0.0367 1.0000 Uiso R . . . . . H1173 H 1.3768 0.7500 0.5282 0.0367 1.0000 Uiso R . . . . . H1181 H 1.3914 0.8285 0.3486 0.0515 1.0000 Uiso R . . . . . H1182 H 1.4951 0.7752 0.3616 0.0518 1.0000 Uiso R . . . . . H1183 H 1.3651 0.7619 0.3430 0.0522 1.0000 Uiso R . . . . . H1201 H 1.2113 0.6469 0.5798 0.0292 1.0000 Uiso R . . . . . H1211 H 1.2059 0.5449 0.6798 0.0359 1.0000 Uiso R . . . . . H1221 H 1.1080 0.4473 0.6915 0.0408 1.0000 Uiso R . . . . . H1231 H 1.0106 0.4518 0.6040 0.0440 1.0000 Uiso R . . . . . H1241 H 1.0152 0.5540 0.5040 0.0374 1.0000 Uiso R . . . . . H1261 H 1.2852 0.6059 0.4258 0.0487 1.0000 Uiso R . . . . . H1271 H 1.3500 0.5891 0.3319 0.0543 1.0000 Uiso R . . . . . H1281 H 1.2522 0.6429 0.2361 0.0482 1.0000 Uiso R . . . . . H1291 H 1.0907 0.7143 0.2337 0.0467 1.0000 Uiso R . . . . . H1301 H 1.0240 0.7311 0.3269 0.0330 1.0000 Uiso R . . . . . H1311 H 0.9935 0.8063 0.6350 0.0226 1.0000 Uiso R . . . . . H1321 H 1.2282 0.8624 0.5532 0.0376 1.0000 Uiso R . . . . . H1322 H 1.1187 0.9020 0.5588 0.0379 1.0000 Uiso R . . . . . H1323 H 1.1842 0.8654 0.6167 0.0366 1.0000 Uiso R . . . . . H1331 H 1.0798 0.6979 0.6701 0.0385 1.0000 Uiso R . . . . . H1332 H 1.2108 0.7333 0.6273 0.0385 1.0000 Uiso R . . . . . H1333 H 1.1580 0.7411 0.6911 0.0388 1.0000 Uiso R . . . . . H1351 H 0.8778 0.9007 0.5338 0.0308 1.0000 Uiso R . . . . . H1361 H 0.7165 0.9731 0.5343 0.0376 1.0000 Uiso R . . . . . H1371 H 0.5077 0.9325 0.5630 0.0379 1.0000 Uiso R . . . . . H1381 H 0.4592 0.8218 0.5904 0.0328 1.0000 Uiso R . . . . . H1391 H 0.6174 0.7500 0.5905 0.0266 1.0000 Uiso R . . . . . H1411 H 0.8159 0.7198 0.6959 0.0285 1.0000 Uiso R . . . . . H1421 H 0.7653 0.6184 0.7940 0.0303 1.0000 Uiso R . . . . . H1431 H 0.7759 0.5181 0.7866 0.0322 1.0000 Uiso R . . . . . H1441 H 0.8254 0.5214 0.6811 0.0322 1.0000 Uiso R . . . . . H1451 H 0.8652 0.6236 0.5839 0.0249 1.0000 Uiso R . . . . . H5001 H 0.3111 0.4907 0.4681 0.0742 0.5000 Uiso R . . . . . H5002 H 0.4040 0.4349 0.4727 0.0742 0.5000 Uiso R . . . . . H5011 H 0.5176 0.5591 0.5290 0.0888 0.5000 Uiso R . . . . . H5012 H 0.6104 0.5032 0.5337 0.0888 0.5000 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 Fe1 0.01457(16) 0.01177(15) 0.01170(15) -0.00563(13) -0.00098(12) 0.00005(12) Fe101 0.01503(16) 0.01501(16) 0.01223(15) -0.00682(13) -0.00273(12) 0.00094(12) V1 0.01558(19) 0.01179(18) 0.01297(18) -0.00505(15) -0.00124(14) -0.00095(14) V101 0.01428(19) 0.01527(19) 0.01256(18) -0.00623(15) -0.00226(14) 0.00113(14) I1 0.01881(8) 0.02275(8) 0.02018(8) -0.01035(7) 0.00203(6) -0.00568(6) I101 0.02128(9) 0.03783(10) 0.03018(9) -0.02220(8) -0.00306(7) -0.00572(7) P1 0.0140(3) 0.0157(3) 0.0128(3) -0.0066(2) -0.0019(2) 0.0012(2) P2 0.0168(3) 0.0181(3) 0.0140(3) -0.0043(2) -0.0030(2) -0.0025(2) P3 0.0186(3) 0.0126(3) 0.0173(3) -0.0072(2) -0.0023(2) 0.0006(2) P101 0.0175(3) 0.0155(3) 0.0153(3) -0.0056(2) -0.0043(2) 0.0009(2) P102 0.0201(3) 0.0214(3) 0.0217(3) -0.0140(3) -0.0067(3) 0.0049(2) P103 0.0157(3) 0.0186(3) 0.0131(3) -0.0080(2) -0.0014(2) -0.0011(2) O2 0.0318(11) 0.0299(11) 0.0378(12) -0.0119(9) -0.0002(9) 0.0033(9) N1 0.0173(10) 0.0148(9) 0.0117(9) -0.0050(8) 0.0005(7) -0.0012(7) N2 0.0161(10) 0.0156(10) 0.0175(10) -0.0029(8) -0.0036(8) -0.0020(8) N3 0.0190(10) 0.0131(9) 0.0163(9) -0.0066(8) -0.0023(8) -0.0017(7) N101 0.0184(10) 0.0153(10) 0.0174(10) -0.0053(8) -0.0038(8) -0.0018(8) N102 0.0152(10) 0.0217(11) 0.0188(10) -0.0109(9) -0.0030(8) 0.0029(8) N103 0.0149(10) 0.0224(10) 0.0167(10) -0.0116(8) -0.0021(8) -0.0004(8) C1 0.0227(13) 0.0219(12) 0.0142(11) -0.0089(10) 0.0031(9) -0.0022(10) C2 0.0238(14) 0.0424(17) 0.0268(14) -0.0153(13) 0.0071(11) -0.0052(12) C3 0.0397(17) 0.0260(14) 0.0167(12) -0.0033(11) 0.0003(11) -0.0041(12) C4 0.0182(11) 0.0139(11) 0.0109(10) -0.0048(9) -0.0011(8) -0.0002(9) C5 0.0196(12) 0.0193(12) 0.0193(12) -0.0093(10) -0.0029(9) 0.0003(9) C6 0.0239(13) 0.0252(13) 0.0217(12) -0.0103(11) -0.0036(10) 0.0076(10) C7 0.0354(15) 0.0153(12) 0.0203(12) -0.0073(10) -0.0029(11) 0.0039(10) C8 0.0302(14) 0.0189(13) 0.0232(13) -0.0082(11) 0.0001(11) -0.0066(10) C9 0.0192(12) 0.0211(12) 0.0187(12) -0.0087(10) 0.0007(9) -0.0019(9) C10 0.0175(12) 0.0165(11) 0.0157(11) -0.0064(9) -0.0036(9) 0.0011(9) C11 0.0233(13) 0.0283(14) 0.0181(12) -0.0135(11) -0.0037(10) 0.0073(10) C12 0.0338(15) 0.0302(14) 0.0181(12) -0.0136(11) -0.0091(11) 0.0048(11) C13 0.0264(14) 0.0254(14) 0.0266(14) -0.0100(11) -0.0144(11) 0.0059(11) C14 0.0225(13) 0.0260(14) 0.0265(13) -0.0137(11) -0.0063(11) 0.0075(10) C15 0.0194(12) 0.0218(12) 0.0183(11) -0.0112(10) -0.0025(9) 0.0006(9) C16 0.0159(12) 0.0204(12) 0.0241(13) -0.0039(10) -0.0064(10) -0.0019(9) C17 0.0163(13) 0.0271(15) 0.0439(17) -0.0150(13) -0.0020(12) -0.0025(10) C18 0.0184(13) 0.0239(14) 0.0352(15) -0.0099(12) -0.0038(11) 0.0027(10) C19 0.0216(13) 0.0231(13) 0.0170(12) -0.0066(10) -0.0075(10) 0.0017(10) C20 0.0293(15) 0.0334(16) 0.0313(15) -0.0172(13) -0.0069(12) -0.0023(12) C21 0.0436(19) 0.0408(18) 0.0429(18) -0.0281(15) -0.0155(15) -0.0005(14) C22 0.051(2) 0.0444(19) 0.0268(15) -0.0230(14) -0.0162(14) 0.0111(15) C23 0.0445(18) 0.0304(16) 0.0199(13) -0.0086(12) -0.0037(12) 0.0014(13) C24 0.0323(15) 0.0226(13) 0.0211(13) -0.0089(11) -0.0042(11) -0.0017(11) C25 0.0201(12) 0.0180(12) 0.0130(11) -0.0042(9) 0.0006(9) -0.0033(9) C26 0.0203(13) 0.0230(13) 0.0218(12) -0.0069(11) -0.0048(10) -0.0017(10) C27 0.0217(13) 0.0291(15) 0.0249(13) -0.0065(12) -0.0020(11) 0.0048(11) C28 0.0352(16) 0.0195(13) 0.0295(15) -0.0072(12) 0.0015(12) 0.0020(11) C29 0.0383(16) 0.0229(14) 0.0260(14) -0.0110(12) -0.0011(12) -0.0074(12) C30 0.0267(14) 0.0248(14) 0.0168(12) -0.0050(10) -0.0026(10) -0.0041(11) C31 0.0249(13) 0.0142(11) 0.0203(12) -0.0080(10) -0.0010(10) -0.0039(9) C32 0.0331(15) 0.0194(13) 0.0270(14) -0.0094(11) 0.0068(11) -0.0108(11) C33 0.0317(15) 0.0283(15) 0.0314(15) -0.0163(12) -0.0062(12) -0.0059(11) C34 0.0236(13) 0.0144(11) 0.0273(13) -0.0124(10) -0.0104(10) 0.0022(9) C35 0.0366(16) 0.0218(13) 0.0269(14) -0.0154(11) -0.0120(12) 0.0069(11) C36 0.053(2) 0.0291(16) 0.0326(16) -0.0170(13) -0.0235(14) 0.0117(14) C37 0.047(2) 0.0295(16) 0.058(2) -0.0233(16) -0.0364(17) 0.0134(14) C38 0.0262(15) 0.0347(17) 0.064(2) -0.0260(17) -0.0196(15) 0.0088(12) C39 0.0262(14) 0.0214(14) 0.0389(16) -0.0123(12) -0.0075(12) -0.0004(11) C40 0.0206(12) 0.0178(12) 0.0202(12) -0.0092(10) -0.0007(10) 0.0017(9) C41 0.0354(15) 0.0179(12) 0.0207(12) -0.0098(10) -0.0008(11) 0.0028(11) C42 0.0388(16) 0.0228(14) 0.0340(15) -0.0192(12) -0.0020(13) 0.0031(12) C43 0.0466(18) 0.0345(16) 0.0280(15) -0.0220(13) -0.0038(13) 0.0077(13) C44 0.058(2) 0.0327(16) 0.0183(13) -0.0102(12) -0.0022(13) 0.0089(14) C45 0.0361(16) 0.0212(13) 0.0234(13) -0.0106(11) -0.0030(11) 0.0069(11) C46 0.0335(16) 0.0334(16) 0.0370(17) -0.0164(14) 0.0024(13) -0.0074(13) C47 0.0320(16) 0.0312(16) 0.0322(16) -0.0084(13) -0.0019(13) -0.0043(12) C48 0.0309(16) 0.0291(15) 0.0405(17) -0.0165(13) -0.0044(13) -0.0003(12) C49 0.0309(16) 0.0332(16) 0.0333(16) -0.0166(13) -0.0005(12) 0.0006(12) C51 0.129(5) 0.107(4) 0.033(2) -0.021(3) -0.005(3) -0.040(4) C101 0.0233(13) 0.0167(12) 0.0213(12) -0.0038(10) -0.0055(10) -0.0037(10) C102 0.0265(15) 0.0264(15) 0.0400(17) -0.0100(13) -0.0027(13) -0.0058(11) C103 0.0360(16) 0.0194(13) 0.0256(13) -0.0086(11) -0.0065(12) -0.0050(11) C104 0.0260(13) 0.0134(11) 0.0171(11) -0.0054(9) -0.0045(10) 0.0019(9) C105 0.0312(15) 0.0310(15) 0.0207(13) -0.0086(12) -0.0043(11) 0.0059(12) C106 0.0428(18) 0.0348(17) 0.0269(15) -0.0136(13) 0.0059(13) 0.0046(13) C107 0.062(2) 0.0289(16) 0.0197(14) -0.0128(12) -0.0005(14) 0.0000(14) C108 0.054(2) 0.0323(16) 0.0246(14) -0.0140(13) -0.0131(14) -0.0031(14) C109 0.0337(15) 0.0261(14) 0.0219(13) -0.0108(11) -0.0078(11) -0.0008(11) C110 0.0213(12) 0.0209(12) 0.0193(12) -0.0101(10) -0.0070(10) 0.0033(10) C111 0.0268(14) 0.0243(14) 0.0257(13) -0.0100(11) -0.0081(11) 0.0044(11) C112 0.0405(17) 0.0265(15) 0.0345(16) -0.0154(13) -0.0159(13) 0.0112(12) C113 0.0386(17) 0.0443(18) 0.0337(16) -0.0253(15) -0.0191(13) 0.0259(14) C114 0.0255(15) 0.056(2) 0.0295(15) -0.0214(15) -0.0073(12) 0.0137(14) C115 0.0224(13) 0.0313(15) 0.0205(13) -0.0085(11) -0.0055(10) 0.0030(11) C116 0.0182(12) 0.0301(14) 0.0208(12) -0.0142(11) -0.0040(10) 0.0068(10) C117 0.0169(12) 0.0308(14) 0.0260(13) -0.0136(12) -0.0033(10) 0.0011(10) C118 0.0217(14) 0.058(2) 0.0200(13) -0.0162(14) 0.0010(11) 0.0028(13) C119 0.0231(13) 0.0205(13) 0.0255(13) -0.0136(11) -0.0056(10) 0.0062(10) C120 0.0204(13) 0.0306(14) 0.0259(13) -0.0145(12) -0.0043(10) 0.0029(10) C121 0.0276(15) 0.0340(16) 0.0241(13) -0.0104(12) -0.0072(11) 0.0057(12) C122 0.0406(17) 0.0272(15) 0.0297(15) -0.0088(13) -0.0064(13) 0.0077(13) C123 0.054(2) 0.0211(14) 0.0362(16) -0.0148(13) -0.0077(14) -0.0012(13) C124 0.0435(17) 0.0262(15) 0.0297(15) -0.0164(12) -0.0118(13) 0.0028(12) C125 0.0271(14) 0.0272(14) 0.0265(13) -0.0177(12) -0.0044(11) 0.0047(11) C126 0.0423(19) 0.057(2) 0.0437(18) -0.0382(17) -0.0186(15) 0.0239(16) C127 0.0406(19) 0.064(2) 0.053(2) -0.046(2) -0.0110(16) 0.0213(16) C128 0.0448(19) 0.054(2) 0.0346(17) -0.0332(16) 0.0027(14) 0.0023(15) C129 0.052(2) 0.0454(19) 0.0248(15) -0.0210(14) -0.0068(14) 0.0090(15) C130 0.0332(15) 0.0280(14) 0.0250(13) -0.0149(12) -0.0049(11) 0.0065(11) C131 0.0192(12) 0.0259(13) 0.0169(11) -0.0131(10) -0.0041(9) 0.0024(10) C132 0.0204(13) 0.0243(13) 0.0372(15) -0.0194(12) -0.0054(11) -0.0031(10) C133 0.0275(14) 0.0297(14) 0.0226(13) -0.0122(11) -0.0121(11) 0.0055(11) C134 0.0182(12) 0.0241(13) 0.0151(11) -0.0110(10) -0.0023(9) 0.0023(9) C135 0.0252(14) 0.0257(14) 0.0296(14) -0.0156(12) -0.0077(11) 0.0006(11) C136 0.0343(16) 0.0301(15) 0.0411(17) -0.0248(14) -0.0141(13) 0.0091(12) C137 0.0324(16) 0.0408(17) 0.0310(15) -0.0233(14) -0.0105(12) 0.0174(13) C138 0.0179(13) 0.0390(16) 0.0228(13) -0.0130(12) -0.0009(10) 0.0023(11) C139 0.0212(13) 0.0257(13) 0.0190(12) -0.0094(10) -0.0021(10) -0.0013(10) C140 0.0167(12) 0.0211(12) 0.0150(11) -0.0078(10) -0.0018(9) 0.0004(9) C141 0.0377(15) 0.0192(12) 0.0137(11) -0.0093(10) 0.0000(10) 0.0029(11) C142 0.0265(14) 0.0320(15) 0.0151(12) -0.0097(11) -0.0011(10) 0.0024(11) C143 0.0270(14) 0.0242(14) 0.0177(12) -0.0010(10) -0.0016(10) 0.0002(11) C144 0.0270(14) 0.0217(13) 0.0304(14) -0.0115(12) -0.0031(11) 0.0018(11) C145 0.0197(12) 0.0237(13) 0.0189(12) -0.0108(10) -0.0013(10) 0.0012(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.082286(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 Fe1 . V1 . 2.0745(5) yes Fe1 . I1 . 2.6658(4) yes Fe1 . P1 . 2.2708(7) yes Fe1 . P2 . 2.2844(7) yes Fe1 . P3 . 2.3233(7) yes Fe101 . V101 . 2.0637(5) yes Fe101 . I101 . 2.6336(4) yes Fe101 . P101 . 2.2839(7) yes Fe101 . P102 . 2.3238(7) yes Fe101 . P103 . 2.2682(7) yes V1 . P1 . 2.6290(7) yes V1 . P2 . 2.6431(7) yes V1 . P3 . 2.6591(7) yes V1 . N1 . 1.9254(19) yes V1 . N2 . 1.922(2) yes V1 . N3 . 1.917(2) yes V101 . P101 . 2.6558(7) yes V101 . P102 . 2.6689(8) yes V101 . P103 . 2.6232(7) yes V101 . N101 . 1.929(2) yes V101 . N102 . 1.908(2) yes V101 . N103 . 1.936(2) yes P1 . N1 . 1.675(2) yes P1 . C4 . 1.820(2) yes P1 . C10 . 1.829(2) yes P2 . N2 . 1.671(2) yes P2 . C19 . 1.815(3) yes P2 . C25 . 1.826(3) yes P3 . N3 . 1.671(2) yes P3 . C34 . 1.831(3) yes P3 . C40 . 1.823(3) yes P101 . N101 . 1.673(2) yes P101 . C104 . 1.831(3) yes P101 . C110 . 1.822(3) yes P102 . N102 . 1.680(2) yes P102 . C119 . 1.820(3) yes P102 . C125 . 1.825(3) yes P103 . N103 . 1.673(2) yes P103 . C134 . 1.825(3) yes P103 . C140 . 1.825(2) yes O1 . H5012 2_666 1.233 no O1 . C501 2_666 1.192(11) yes O1 . C51 . 1.395(7) yes O1 . C500 . 1.416(10) yes O2 . C46 . 1.425(4) yes O2 . C49 . 1.431(3) yes N1 . C1 . 1.473(3) yes N2 . C16 . 1.480(3) yes N3 . C31 . 1.480(3) yes N101 . C101 . 1.474(3) yes N102 . C116 . 1.477(3) yes N103 . C131 . 1.469(3) yes C1 . C2 . 1.521(4) yes C1 . C3 . 1.525(4) yes C1 . H11 . 0.974 no C2 . H21 . 0.956 no C2 . H22 . 0.972 no C2 . H23 . 0.952 no C3 . H31 . 0.972 no C3 . H32 . 0.960 no C3 . H33 . 0.958 no C4 . C5 . 1.395(3) yes C4 . C9 . 1.395(3) yes C5 . C6 . 1.389(3) yes C5 . H51 . 0.931 no C6 . C7 . 1.384(4) yes C6 . H61 . 0.915 no C7 . C8 . 1.381(4) yes C7 . H71 . 0.923 no C8 . C9 . 1.379(4) yes C8 . H81 . 0.921 no C9 . H91 . 0.912 no C10 . C11 . 1.398(3) yes C10 . C15 . 1.390(3) yes C11 . C12 . 1.396(4) yes C11 . H111 . 0.929 no C12 . C13 . 1.381(4) yes C12 . H121 . 0.929 no C13 . C14 . 1.380(4) yes C13 . H131 . 0.926 no C14 . C15 . 1.389(3) yes C14 . H141 . 0.929 no C15 . H151 . 0.933 no C16 . C17 . 1.518(3) yes C16 . C18 . 1.520(4) yes C16 . H161 . 0.970 no C17 . H171 . 0.946 no C17 . H172 . 0.943 no C17 . H173 . 0.976 no C18 . H181 . 0.970 no C18 . H182 . 0.958 no C18 . H183 . 0.957 no C19 . C20 . 1.398(4) yes C19 . C24 . 1.387(4) yes C20 . C21 . 1.387(4) yes C20 . H201 . 0.943 no C21 . C22 . 1.376(5) yes C21 . H211 . 0.926 no C22 . C23 . 1.383(4) yes C22 . H221 . 0.936 no C23 . C24 . 1.387(4) yes C23 . H231 . 0.929 no C24 . H241 . 0.935 no C25 . C26 . 1.405(3) yes C25 . C30 . 1.390(4) yes C26 . C27 . 1.387(4) yes C26 . H261 . 0.932 no C27 . C28 . 1.384(4) yes C27 . H271 . 0.931 no C28 . C29 . 1.386(4) yes C28 . H281 . 0.920 no C29 . C30 . 1.383(4) yes C29 . H291 . 0.920 no C30 . H301 . 0.927 no C31 . C32 . 1.522(4) yes C31 . C33 . 1.518(4) yes C31 . H311 . 0.973 no C32 . H321 . 0.956 no C32 . H322 . 0.952 no C32 . H323 . 0.952 no C33 . H331 . 0.960 no C33 . H332 . 0.960 no C33 . H333 . 0.958 no C34 . C35 . 1.393(4) yes C34 . C39 . 1.393(4) yes C35 . C36 . 1.398(4) yes C35 . H351 . 0.931 no C36 . C37 . 1.377(5) yes C36 . H361 . 0.945 no C37 . C38 . 1.377(5) yes C37 . H371 . 0.939 no C38 . C39 . 1.393(4) yes C38 . H381 . 0.912 no C39 . H391 . 0.926 no C40 . C41 . 1.394(3) yes C40 . C45 . 1.390(3) yes C41 . C42 . 1.386(4) yes C41 . H411 . 0.927 no C42 . C43 . 1.379(4) yes C42 . H421 . 0.925 no C43 . C44 . 1.378(4) yes C43 . H431 . 0.925 no C44 . C45 . 1.393(4) yes C44 . H441 . 0.920 no C45 . H451 . 0.935 no C46 . C47 . 1.507(4) yes C46 . H461 . 0.994 no C46 . H462 . 0.992 no C47 . C48 . 1.529(4) yes C47 . H471 . 0.969 no C47 . H472 . 0.983 no C48 . C49 . 1.519(4) yes C48 . H481 . 0.967 no C48 . H482 . 0.971 no C49 . H491 . 0.993 no C49 . H492 . 0.980 no C51 . C501 2_666 1.542(11) yes C51 . C500 2_666 1.528(10) yes C51 . C501 . 1.362(11) yes C51 . H511 . 0.950 no C51 . H512 . 0.950 no C51 . H513 . 0.950 no C51 . H514 . 0.950 no C101 . C102 . 1.525(4) yes C101 . C103 . 1.527(4) yes C101 . H1011 . 0.967 no C102 . H1021 . 0.982 no C102 . H1022 . 0.962 no C102 . H1023 . 0.957 no C103 . H1031 . 0.970 no C103 . H1032 . 0.982 no C103 . H1033 . 0.966 no C104 . C105 . 1.388(4) yes C104 . C109 . 1.395(4) yes C105 . C106 . 1.394(4) yes C105 . H1051 . 0.946 no C106 . C107 . 1.385(5) yes C106 . H1061 . 0.930 no C107 . C108 . 1.373(5) yes C107 . H1071 . 0.925 no C108 . C109 . 1.391(4) yes C108 . H1081 . 0.943 no C109 . H1091 . 0.946 no C110 . C111 . 1.404(4) yes C110 . C115 . 1.388(4) yes C111 . C112 . 1.377(4) yes C111 . H1111 . 0.917 no C112 . C113 . 1.375(4) yes C112 . H1121 . 0.930 no C113 . C114 . 1.386(4) yes C113 . H1131 . 0.941 no C114 . C115 . 1.396(4) yes C114 . H1141 . 0.921 no C115 . H1151 . 0.937 no C116 . C117 . 1.522(4) yes C116 . C118 . 1.529(4) yes C116 . H1161 . 0.985 no C117 . H1171 . 0.980 no C117 . H1172 . 0.970 no C117 . H1173 . 0.967 no C118 . H1181 . 0.974 no C118 . H1182 . 0.951 no C118 . H1183 . 0.965 no C119 . C120 . 1.392(4) yes C119 . C124 . 1.401(4) yes C120 . C121 . 1.392(4) yes C120 . H1201 . 0.952 no C121 . C122 . 1.378(4) yes C121 . H1211 . 0.945 no C122 . C123 . 1.378(4) yes C122 . H1221 . 0.939 no C123 . C124 . 1.385(4) yes C123 . H1231 . 0.949 no C124 . H1241 . 0.935 no C125 . C126 . 1.394(4) yes C125 . C130 . 1.388(4) yes C126 . C127 . 1.392(4) yes C126 . H1261 . 0.943 no C127 . C128 . 1.372(5) yes C127 . H1271 . 0.939 no C128 . C129 . 1.380(5) yes C128 . H1281 . 0.939 no C129 . C130 . 1.389(4) yes C129 . H1291 . 0.936 no C130 . H1301 . 0.932 no C131 . C132 . 1.516(3) yes C131 . C133 . 1.528(3) yes C131 . H1311 . 0.982 no C132 . H1321 . 0.926 no C132 . H1322 . 0.901 no C132 . H1323 . 0.882 no C133 . H1331 . 0.969 no C133 . H1332 . 0.958 no C133 . H1333 . 0.969 no C134 . C135 . 1.388(4) yes C134 . C139 . 1.403(3) yes C135 . C136 . 1.390(4) yes C135 . H1351 . 0.931 no C136 . C137 . 1.382(4) yes C136 . H1361 . 0.938 no C137 . C138 . 1.381(4) yes C137 . H1371 . 0.924 no C138 . C139 . 1.390(4) yes C138 . H1381 . 0.920 no C139 . H1391 . 0.928 no C140 . C141 . 1.405(3) yes C140 . C145 . 1.387(3) yes C141 . C142 . 1.387(4) yes C141 . H1411 . 0.884 no C142 . C143 . 1.384(4) yes C142 . H1421 . 0.934 no C143 . C144 . 1.380(4) yes C143 . H1431 . 0.926 no C144 . C145 . 1.397(4) yes C144 . H1441 . 0.936 no C145 . H1451 . 0.931 no C500 . H5011 2_666 1.233 no C500 . C501 2_666 0.819(12) yes C500 . H5001 . 0.950 no C500 . H5002 . 0.950 no C501 . H5002 2_666 1.287 no C501 . C501 2_666 1.82(2) yes C501 . H5011 . 0.950 no C501 . H5012 . 0.950 no H511 . H514 . 0.709 no H512 . H513 . 0.569 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 V1 . Fe1 . I1 . 178.266(19) yes V1 . Fe1 . P1 . 74.31(2) yes I1 . Fe1 . P1 . 107.42(2) yes V1 . Fe1 . P2 . 74.48(2) yes I1 . Fe1 . P2 . 104.934(19) yes P1 . Fe1 . P2 . 108.21(3) yes V1 . Fe1 . P3 . 74.17(2) yes I1 . Fe1 . P3 . 104.83(2) yes P1 . Fe1 . P3 . 112.91(3) yes P2 . Fe1 . P3 . 117.72(3) yes V101 . Fe101 . I101 . 178.741(19) yes V101 . Fe101 . P101 . 75.11(2) yes I101 . Fe101 . P101 . 104.16(2) yes V101 . Fe101 . P102 . 74.67(2) yes I101 . Fe101 . P102 . 104.97(2) yes P101 . Fe101 . P102 . 120.87(3) yes V101 . Fe101 . P103 . 74.37(2) yes I101 . Fe101 . P103 . 106.87(2) yes P101 . Fe101 . P103 . 108.37(3) yes P102 . Fe101 . P103 . 110.55(3) yes Fe1 . V1 . P1 . 56.259(18) yes Fe1 . V1 . P2 . 56.384(19) yes P1 . V1 . P2 . 88.84(2) yes Fe1 . V1 . P3 . 57.196(18) yes P1 . V1 . P3 . 92.78(2) yes P2 . V1 . P3 . 96.11(2) yes Fe1 . V1 . N1 . 95.34(6) yes P1 . V1 . N1 . 39.49(6) yes P2 . V1 . N1 . 118.17(6) yes P3 . V1 . N1 . 113.02(6) yes Fe1 . V1 . N2 . 95.44(6) yes P1 . V1 . N2 . 112.57(6) yes P2 . V1 . N2 . 39.06(6) yes P3 . V1 . N2 . 123.24(7) yes N1 . V1 . N2 . 118.69(9) yes Fe1 . V1 . N3 . 95.70(6) yes P1 . V1 . N3 . 121.57(6) yes P2 . V1 . N3 . 118.81(6) yes P3 . V1 . N3 . 38.73(6) yes N1 . V1 . N3 . 117.62(8) yes N2 . V1 . N3 . 120.97(9) yes Fe101 . V101 . P101 . 56.212(18) yes Fe101 . V101 . P102 . 57.110(19) yes P101 . V101 . P102 . 97.65(2) yes Fe101 . V101 . P103 . 56.376(18) yes P101 . V101 . P103 . 88.73(2) yes P102 . V101 . P103 . 90.98(2) yes Fe101 . V101 . N101 . 95.09(6) yes P101 . V101 . N101 . 38.88(6) yes P102 . V101 . N101 . 124.95(6) yes P103 . V101 . N101 . 112.82(6) yes Fe101 . V101 . N102 . 95.34(6) yes P101 . V101 . N102 . 119.26(6) yes P102 . V101 . N102 . 38.75(6) yes P103 . V101 . N102 . 120.79(6) yes N101 . V101 . N102 . 121.32(9) yes Fe101 . V101 . N103 . 95.75(6) yes P101 . V101 . N103 . 116.58(6) yes P102 . V101 . N103 . 112.52(6) yes P103 . V101 . N103 . 39.55(6) yes N101 . V101 . N103 . 117.14(9) yes N102 . V101 . N103 . 118.93(9) yes V1 . P1 . Fe1 . 49.436(17) yes V1 . P1 . N1 . 46.97(7) yes Fe1 . P1 . N1 . 95.98(7) yes V1 . P1 . C4 . 121.31(8) yes Fe1 . P1 . C4 . 121.61(7) yes N1 . P1 . C4 . 105.98(10) yes V1 . P1 . C10 . 134.06(8) yes Fe1 . P1 . C10 . 119.71(8) yes N1 . P1 . C10 . 110.36(10) yes C4 . P1 . C10 . 102.18(11) yes V1 . P2 . Fe1 . 49.136(17) yes V1 . P2 . N2 . 46.48(7) yes Fe1 . P2 . N2 . 95.60(7) yes V1 . P2 . C19 . 118.99(8) yes Fe1 . P2 . C19 . 111.04(8) yes N2 . P2 . C19 . 108.05(11) yes V1 . P2 . C25 . 137.75(8) yes Fe1 . P2 . C25 . 127.94(8) yes N2 . P2 . C25 . 111.87(11) yes C19 . P2 . C25 . 101.47(11) yes V1 . P3 . Fe1 . 48.638(16) yes V1 . P3 . N3 . 45.85(7) yes Fe1 . P3 . N3 . 94.25(7) yes V1 . P3 . C34 . 123.13(9) yes Fe1 . P3 . C34 . 121.08(8) yes N3 . P3 . C34 . 107.81(11) yes V1 . P3 . C40 . 132.68(8) yes Fe1 . P3 . C40 . 120.77(8) yes N3 . P3 . C40 . 110.29(11) yes C34 . P3 . C40 . 101.81(11) yes V101 . P101 . Fe101 . 48.675(17) yes V101 . P101 . N101 . 46.39(7) yes Fe101 . P101 . N101 . 95.06(7) yes V101 . P101 . C104 . 122.79(8) yes Fe101 . P101 . C104 . 115.78(8) yes N101 . P101 . C104 . 107.68(11) yes V101 . P101 . C110 . 134.74(8) yes Fe101 . P101 . C110 . 126.01(8) yes N101 . P101 . C110 . 111.27(11) yes C104 . P101 . C110 . 100.29(11) yes V101 . P102 . Fe101 . 48.222(17) yes V101 . P102 . N102 . 45.33(7) yes Fe101 . P102 . N102 . 93.02(7) yes V101 . P102 . C119 . 122.11(8) yes Fe101 . P102 . C119 . 122.65(9) yes N102 . P102 . C119 . 107.86(11) yes V101 . P102 . C125 . 132.46(9) yes Fe101 . P102 . C125 . 119.16(9) yes N102 . P102 . C125 . 110.03(11) yes C119 . P102 . C125 . 102.98(12) yes V101 . P103 . Fe101 . 49.256(17) yes V101 . P103 . N103 . 47.49(7) yes Fe101 . P103 . N103 . 96.57(7) yes V101 . P103 . C134 . 124.11(8) yes Fe101 . P103 . C134 . 120.28(8) yes N103 . P103 . C134 . 107.94(11) yes V101 . P103 . C140 . 132.23(8) yes Fe101 . P103 . C140 . 119.04(8) yes N103 . P103 . C140 . 110.57(11) yes C134 . P103 . C140 . 101.99(11) yes H5012 2_666 O1 . C501 2_666 46.1 no H5012 2_666 O1 . C51 . 109.1 no C501 2_666 O1 . C51 . 72.7(6) yes C51 . O1 . C500 . 105.8(6) yes C46 . O2 . C49 . 104.5(2) yes P1 . N1 . V1 . 93.55(9) yes P1 . N1 . C1 . 124.85(16) yes V1 . N1 . C1 . 141.52(16) yes P2 . N2 . V1 . 94.46(10) yes P2 . N2 . C16 . 126.97(16) yes V1 . N2 . C16 . 138.51(16) yes P3 . N3 . V1 . 95.41(9) yes P3 . N3 . C31 . 128.34(16) yes V1 . N3 . C31 . 136.23(16) yes P101 . N101 . V101 . 94.73(9) yes P101 . N101 . C101 . 126.89(16) yes V101 . N101 . C101 . 137.47(16) yes P102 . N102 . V101 . 95.92(10) yes P102 . N102 . C116 . 127.62(17) yes V101 . N102 . C116 . 136.41(17) yes P103 . N103 . V101 . 92.96(9) yes P103 . N103 . C131 . 126.98(16) yes V101 . N103 . C131 . 139.74(16) yes N1 . C1 . C2 . 110.5(2) yes N1 . C1 . C3 . 111.3(2) yes C2 . C1 . C3 . 110.5(2) yes N1 . C1 . H11 . 106.7 no C2 . C1 . H11 . 108.6 no C3 . C1 . H11 . 109.1 no C1 . C2 . H21 . 110.3 no C1 . C2 . H22 . 109.5 no H21 . C2 . H22 . 109.4 no C1 . C2 . H23 . 110.0 no H21 . C2 . H23 . 108.2 no H22 . C2 . H23 . 109.5 no C1 . C3 . H31 . 111.7 no C1 . C3 . H32 . 111.0 no H31 . C3 . H32 . 108.4 no C1 . C3 . H33 . 111.1 no H31 . C3 . H33 . 107.1 no H32 . C3 . H33 . 107.4 no P1 . C4 . C5 . 119.57(18) yes P1 . C4 . C9 . 121.55(18) yes C5 . C4 . C9 . 118.7(2) yes C4 . C5 . C6 . 120.6(2) yes C4 . C5 . H51 . 119.0 no C6 . C5 . H51 . 120.3 no C5 . C6 . C7 . 119.5(2) yes C5 . C6 . H61 . 120.5 no C7 . C6 . H61 . 120.0 no C6 . C7 . C8 . 120.4(2) yes C6 . C7 . H71 . 119.0 no C8 . C7 . H71 . 120.5 no C7 . C8 . C9 . 120.0(2) yes C7 . C8 . H81 . 119.5 no C9 . C8 . H81 . 120.5 no C4 . C9 . C8 . 120.7(2) yes C4 . C9 . H91 . 118.4 no C8 . C9 . H91 . 120.9 no P1 . C10 . C11 . 121.50(18) yes P1 . C10 . C15 . 119.40(18) yes C11 . C10 . C15 . 119.1(2) yes C10 . C11 . C12 . 120.1(2) yes C10 . C11 . H111 . 119.6 no C12 . C11 . H111 . 120.3 no C11 . C12 . C13 . 120.0(2) yes C11 . C12 . H121 . 120.7 no C13 . C12 . H121 . 119.3 no C12 . C13 . C14 . 120.1(2) yes C12 . C13 . H131 . 119.9 no C14 . C13 . H131 . 120.0 no C13 . C14 . C15 . 120.3(2) yes C13 . C14 . H141 . 120.8 no C15 . C14 . H141 . 118.8 no C10 . C15 . C14 . 120.3(2) yes C10 . C15 . H151 . 118.5 no C14 . C15 . H151 . 121.2 no N2 . C16 . C17 . 109.7(2) yes N2 . C16 . C18 . 110.9(2) yes C17 . C16 . C18 . 111.2(2) yes N2 . C16 . H161 . 107.4 no C17 . C16 . H161 . 108.4 no C18 . C16 . H161 . 109.2 no C16 . C17 . H171 . 110.2 no C16 . C17 . H172 . 109.0 no H171 . C17 . H172 . 110.0 no C16 . C17 . H173 . 109.9 no H171 . C17 . H173 . 108.8 no H172 . C17 . H173 . 108.9 no C16 . C18 . H181 . 108.9 no C16 . C18 . H182 . 108.7 no H181 . C18 . H182 . 109.8 no C16 . C18 . H183 . 110.7 no H181 . C18 . H183 . 109.3 no H182 . C18 . H183 . 109.4 no P2 . C19 . C20 . 122.2(2) yes P2 . C19 . C24 . 118.8(2) yes C20 . C19 . C24 . 118.7(2) yes C19 . C20 . C21 . 120.3(3) yes C19 . C20 . H201 . 119.7 no C21 . C20 . H201 . 120.0 no C20 . C21 . C22 . 120.5(3) yes C20 . C21 . H211 . 121.1 no C22 . C21 . H211 . 118.4 no C21 . C22 . C23 . 119.7(3) yes C21 . C22 . H221 . 119.3 no C23 . C22 . H221 . 121.0 no C22 . C23 . C24 . 120.2(3) yes C22 . C23 . H231 . 120.0 no C24 . C23 . H231 . 119.8 no C23 . C24 . C19 . 120.6(3) yes C23 . C24 . H241 . 120.9 no C19 . C24 . H241 . 118.4 no P2 . C25 . C26 . 121.60(19) yes P2 . C25 . C30 . 119.91(19) yes C26 . C25 . C30 . 118.5(2) yes C25 . C26 . C27 . 120.6(2) yes C25 . C26 . H261 . 119.7 no C27 . C26 . H261 . 119.7 no C26 . C27 . C28 . 120.1(3) yes C26 . C27 . H271 . 121.4 no C28 . C27 . H271 . 118.5 no C27 . C28 . C29 . 119.7(3) yes C27 . C28 . H281 . 120.2 no C29 . C28 . H281 . 120.1 no C28 . C29 . C30 . 120.5(3) yes C28 . C29 . H291 . 120.2 no C30 . C29 . H291 . 119.3 no C25 . C30 . C29 . 120.7(3) yes C25 . C30 . H301 . 119.2 no C29 . C30 . H301 . 120.1 no N3 . C31 . C32 . 109.4(2) yes N3 . C31 . C33 . 110.8(2) yes C32 . C31 . C33 . 110.9(2) yes N3 . C31 . H311 . 107.9 no C32 . C31 . H311 . 109.5 no C33 . C31 . H311 . 108.2 no C31 . C32 . H321 . 112.1 no C31 . C32 . H322 . 110.5 no H321 . C32 . H322 . 110.1 no C31 . C32 . H323 . 108.4 no H321 . C32 . H323 . 108.7 no H322 . C32 . H323 . 106.9 no C31 . C33 . H331 . 110.9 no C31 . C33 . H332 . 109.3 no H331 . C33 . H332 . 110.2 no C31 . C33 . H333 . 108.5 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 108.4 no P3 . C34 . C35 . 120.5(2) yes P3 . C34 . C39 . 119.9(2) yes C35 . C34 . C39 . 119.3(2) yes C34 . C35 . C36 . 119.9(3) yes C34 . C35 . H351 . 119.7 no C36 . C35 . H351 . 120.5 no C35 . C36 . C37 . 120.1(3) yes C35 . C36 . H361 . 119.5 no C37 . C36 . H361 . 120.4 no C36 . C37 . C38 . 120.5(3) yes C36 . C37 . H371 . 120.3 no C38 . C37 . H371 . 119.2 no C37 . C38 . C39 . 120.0(3) yes C37 . C38 . H381 . 120.6 no C39 . C38 . H381 . 119.4 no C34 . C39 . C38 . 120.2(3) yes C34 . C39 . H391 . 119.1 no C38 . C39 . H391 . 120.7 no P3 . C40 . C41 . 121.31(19) yes P3 . C40 . C45 . 119.37(19) yes C41 . C40 . C45 . 119.3(2) yes C40 . C41 . C42 . 120.5(2) yes C40 . C41 . H411 . 119.7 no C42 . C41 . H411 . 119.8 no C41 . C42 . C43 . 119.6(3) yes C41 . C42 . H421 . 119.6 no C43 . C42 . H421 . 120.8 no C42 . C43 . C44 . 120.8(3) yes C42 . C43 . H431 . 119.1 no C44 . C43 . H431 . 120.1 no C43 . C44 . C45 . 119.8(3) yes C43 . C44 . H441 . 120.4 no C45 . C44 . H441 . 119.7 no C44 . C45 . C40 . 120.0(3) yes C44 . C45 . H451 . 120.1 no C40 . C45 . H451 . 119.9 no O2 . C46 . C47 . 105.8(2) yes O2 . C46 . H461 . 108.1 no C47 . C46 . H461 . 111.7 no O2 . C46 . H462 . 110.4 no C47 . C46 . H462 . 110.4 no H461 . C46 . H462 . 110.3 no C46 . C47 . C48 . 103.3(2) yes C46 . C47 . H471 . 110.3 no C48 . C47 . H471 . 109.4 no C46 . C47 . H472 . 111.5 no C48 . C47 . H472 . 112.7 no H471 . C47 . H472 . 109.5 no C47 . C48 . C49 . 104.1(2) yes C47 . C48 . H481 . 110.9 no C49 . C48 . H481 . 110.9 no C47 . C48 . H482 . 110.4 no C49 . C48 . H482 . 110.1 no H481 . C48 . H482 . 110.2 no C48 . C49 . O2 . 106.7(2) yes C48 . C49 . H491 . 111.3 no O2 . C49 . H491 . 108.8 no C48 . C49 . H492 . 111.2 no O2 . C49 . H492 . 108.8 no H491 . C49 . H492 . 110.0 no C501 2_666 C51 . C500 2_666 103.0(7) yes C501 2_666 C51 . O1 . 47.6(4) yes C500 2_666 C51 . O1 . 142.6(6) yes C501 2_666 C51 . C501 . 77.4(7) yes O1 . C51 . C501 . 110.4(7) yes C501 2_666 C51 . H511 . 155.2 no C500 2_666 C51 . H511 . 92.8 no O1 . C51 . H511 . 109.4 no C501 . C51 . H511 . 109.1 no C501 2_666 C51 . H512 . 89.5 no C500 2_666 C51 . H512 . 90.7 no O1 . C51 . H512 . 108.6 no C501 . C51 . H512 . 109.9 no H511 . C51 . H512 . 109.5 no C501 2_666 C51 . H513 . 109.8 no C500 2_666 C51 . H513 . 112.1 no O1 . C51 . H513 . 101.1 no C501 . C51 . H513 . 140.5 no H511 . C51 . H513 . 80.8 no C501 2_666 C51 . H514 . 111.8 no C500 2_666 C51 . H514 . 110.5 no O1 . C51 . H514 . 71.8 no C501 . C51 . H514 . 102.7 no H512 . C51 . H514 . 144.3 no H513 . C51 . H514 . 109.5 no N101 . C101 . C102 . 109.7(2) yes N101 . C101 . C103 . 110.6(2) yes C102 . C101 . C103 . 110.6(2) yes N101 . C101 . H1011 . 107.8 no C102 . C101 . H1011 . 109.2 no C103 . C101 . H1011 . 108.8 no C101 . C102 . H1021 . 109.6 no C101 . C102 . H1022 . 109.3 no H1021 . C102 . H1022 . 109.2 no C101 . C102 . H1023 . 108.7 no H1021 . C102 . H1023 . 109.7 no H1022 . C102 . H1023 . 110.2 no C101 . C103 . H1031 . 108.8 no C101 . C103 . H1032 . 109.0 no H1031 . C103 . H1032 . 109.5 no C101 . C103 . H1033 . 109.5 no H1031 . C103 . H1033 . 110.4 no H1032 . C103 . H1033 . 109.6 no P101 . C104 . C105 . 120.9(2) yes P101 . C104 . C109 . 120.1(2) yes C105 . C104 . C109 . 118.7(2) yes C104 . C105 . C106 . 120.7(3) yes C104 . C105 . H1051 . 119.6 no C106 . C105 . H1051 . 119.7 no C105 . C106 . C107 . 120.0(3) yes C105 . C106 . H1061 . 119.4 no C107 . C106 . H1061 . 120.6 no C106 . C107 . C108 . 119.7(3) yes C106 . C107 . H1071 . 120.0 no C108 . C107 . H1071 . 120.3 no C107 . C108 . C109 . 120.7(3) yes C107 . C108 . H1081 . 120.3 no C109 . C108 . H1081 . 119.0 no C104 . C109 . C108 . 120.3(3) yes C104 . C109 . H1091 . 120.2 no C108 . C109 . H1091 . 119.6 no P101 . C110 . C111 . 121.7(2) yes P101 . C110 . C115 . 119.79(19) yes C111 . C110 . C115 . 118.5(2) yes C110 . C111 . C112 . 120.8(3) yes C110 . C111 . H1111 . 118.8 no C112 . C111 . H1111 . 120.4 no C111 . C112 . C113 . 120.3(3) yes C111 . C112 . H1121 . 120.8 no C113 . C112 . H1121 . 118.9 no C112 . C113 . C114 . 120.0(3) yes C112 . C113 . H1131 . 120.3 no C114 . C113 . H1131 . 119.7 no C113 . C114 . C115 . 120.0(3) yes C113 . C114 . H1141 . 120.5 no C115 . C114 . H1141 . 119.4 no C114 . C115 . C110 . 120.3(3) yes C114 . C115 . H1151 . 120.4 no C110 . C115 . H1151 . 119.3 no N102 . C116 . C117 . 109.3(2) yes N102 . C116 . C118 . 110.2(2) yes C117 . C116 . C118 . 110.5(2) yes N102 . C116 . H1161 . 108.9 no C117 . C116 . H1161 . 108.5 no C118 . C116 . H1161 . 109.5 no C116 . C117 . H1171 . 110.4 no C116 . C117 . H1172 . 110.2 no H1171 . C117 . H1172 . 108.5 no C116 . C117 . H1173 . 109.5 no H1171 . C117 . H1173 . 108.9 no H1172 . C117 . H1173 . 109.4 no C116 . C118 . H1181 . 108.9 no C116 . C118 . H1182 . 108.6 no H1181 . C118 . H1182 . 108.5 no C116 . C118 . H1183 . 109.5 no H1181 . C118 . H1183 . 109.8 no H1182 . C118 . H1183 . 111.5 no P102 . C119 . C120 . 121.1(2) yes P102 . C119 . C124 . 120.1(2) yes C120 . C119 . C124 . 118.4(2) yes C119 . C120 . C121 . 120.4(3) yes C119 . C120 . H1201 . 119.5 no C121 . C120 . H1201 . 120.1 no C120 . C121 . C122 . 120.5(3) yes C120 . C121 . H1211 . 119.0 no C122 . C121 . H1211 . 120.5 no C121 . C122 . C123 . 119.7(3) yes C121 . C122 . H1221 . 119.9 no C123 . C122 . H1221 . 120.4 no C122 . C123 . C124 . 120.4(3) yes C122 . C123 . H1231 . 119.9 no C124 . C123 . H1231 . 119.8 no C119 . C124 . C123 . 120.6(3) yes C119 . C124 . H1241 . 118.8 no C123 . C124 . H1241 . 120.5 no P102 . C125 . C126 . 121.5(2) yes P102 . C125 . C130 . 119.7(2) yes C126 . C125 . C130 . 118.8(3) yes C125 . C126 . C127 . 120.4(3) yes C125 . C126 . H1261 . 119.9 no C127 . C126 . H1261 . 119.8 no C126 . C127 . C128 . 120.1(3) yes C126 . C127 . H1271 . 119.4 no C128 . C127 . H1271 . 120.5 no C127 . C128 . C129 . 120.1(3) yes C127 . C128 . H1281 . 120.2 no C129 . C128 . H1281 . 119.7 no C128 . C129 . C130 . 120.1(3) yes C128 . C129 . H1291 . 119.9 no C130 . C129 . H1291 . 120.0 no C129 . C130 . C125 . 120.5(3) yes C129 . C130 . H1301 . 119.0 no C125 . C130 . H1301 . 120.6 no N103 . C131 . C132 . 111.9(2) yes N103 . C131 . C133 . 111.7(2) yes C132 . C131 . C133 . 109.3(2) yes N103 . C131 . H1311 . 106.8 no C132 . C131 . H1311 . 108.5 no C133 . C131 . H1311 . 108.5 no C131 . C132 . H1321 . 110.5 no C131 . C132 . H1322 . 110.6 no H1321 . C132 . H1322 . 107.9 no C131 . C132 . H1323 . 110.3 no H1321 . C132 . H1323 . 108.6 no H1322 . C132 . H1323 . 108.9 no C131 . C133 . H1331 . 111.3 no C131 . C133 . H1332 . 110.5 no H1331 . C133 . H1332 . 108.6 no C131 . C133 . H1333 . 111.5 no H1331 . C133 . H1333 . 107.7 no H1332 . C133 . H1333 . 107.1 no P103 . C134 . C135 . 121.79(19) yes P103 . C134 . C139 . 119.28(19) yes C135 . C134 . C139 . 118.6(2) yes C134 . C135 . C136 . 120.8(3) yes C134 . C135 . H1351 . 118.6 no C136 . C135 . H1351 . 120.6 no C135 . C136 . C137 . 120.2(3) yes C135 . C136 . H1361 . 120.5 no C137 . C136 . H1361 . 119.4 no C136 . C137 . C138 . 119.9(3) yes C136 . C137 . H1371 . 120.6 no C138 . C137 . H1371 . 119.6 no C137 . C138 . C139 . 120.3(3) yes C137 . C138 . H1381 . 120.3 no C139 . C138 . H1381 . 119.4 no C134 . C139 . C138 . 120.3(2) yes C134 . C139 . H1391 . 119.8 no C138 . C139 . H1391 . 119.9 no P103 . C140 . C141 . 121.49(19) yes P103 . C140 . C145 . 119.38(18) yes C141 . C140 . C145 . 119.0(2) yes C140 . C141 . C142 . 119.9(2) yes C140 . C141 . H1411 . 119.1 no C142 . C141 . H1411 . 121.0 no C141 . C142 . C143 . 120.5(2) yes C141 . C142 . H1421 . 119.4 no C143 . C142 . H1421 . 120.0 no C142 . C143 . C144 . 119.9(2) yes C142 . C143 . H1431 . 120.6 no C144 . C143 . H1431 . 119.5 no C143 . C144 . C145 . 120.1(2) yes C143 . C144 . H1441 . 121.2 no C145 . C144 . H1441 . 118.6 no C144 . C145 . C140 . 120.4(2) yes C144 . C145 . H1451 . 118.7 no C140 . C145 . H1451 . 120.8 no C51 2_666 C500 . O1 . 105.8(7) yes C51 2_666 C500 . H5011 2_666 92.5 no O1 . C500 . H5011 2_666 80.7 no C51 2_666 C500 . C501 2_666 62.6(10) yes O1 . C500 . C501 2_666 57.3(10) yes H5011 2_666 C500 . C501 2_666 50.4 no C51 2_666 C500 . H5001 . 109.3 no O1 . C500 . H5001 . 109.7 no H5011 2_666 C500 . H5001 . 151.2 no C501 2_666 C500 . H5001 . 157.4 no C51 2_666 C500 . H5002 . 110.9 no O1 . C500 . H5002 . 111.6 no C501 2_666 C500 . H5002 . 93.0 no H5001 . C500 . H5002 . 109.5 no C51 2_666 C501 . C51 . 102.6(7) yes C51 2_666 C501 . H5002 2_666 154.2 no C51 . C501 . H5002 2_666 102.5 no C51 2_666 C501 . C501 2_666 46.9(5) yes C51 . C501 . C501 2_666 55.7(6) yes H5002 2_666 C501 . C501 2_666 157.6 no C51 2_666 C501 . O1 2_666 59.7(6) yes C51 . C501 . O1 2_666 133.5(10) yes H5002 2_666 C501 . O1 2_666 105.5 no C501 2_666 C501 . O1 2_666 95.1(9) yes C51 2_666 C501 . C500 2_666 141.3(14) yes C51 . C501 . C500 2_666 85.1(12) yes H5002 2_666 C501 . C500 2_666 47.5 no C501 2_666 C501 . C500 2_666 126.6(16) yes O1 2_666 C501 . C500 2_666 87.4(12) yes C51 2_666 C501 . H5011 . 118.7 no C51 . C501 . H5011 . 119.2 no C501 2_666 C501 . H5011 . 140.4 no O1 2_666 C501 . H5011 . 106.2 no C51 2_666 C501 . H5012 . 116.5 no C51 . C501 . H5012 . 86.3 no H5002 2_666 C501 . H5012 . 71.1 no C501 2_666 C501 . H5012 . 109.2 no O1 2_666 C501 . H5012 . 69.2 no C500 2_666 C501 . H5011 . 88.0 no H5011 . C501 . H5012 . 109.5 no C51 . H511 . H514 . 68.1 no C51 . H512 . H513 . 72.6 no H512 . H513 . C51 . 72.6 no H511 . H514 . C51 . 68.1 no C501 . H5012 . O1 2_666 64.7 no _iucr_refine_instructions_details_constraints ; # # Punched on 19/02/13 at 09:25:24 # #LIST 12 BLOCK CONT SCALE CONT FE ( 1 ,X'S,U'S) UNTIL P ( 103 ) CONT O ( 1 ,X'S,U[ISO]) CONT O ( 2 ,X'S,U'S) UNTIL C ( 145 ) CONT C ( 500 ,X'S,U[ISO]) UNTIL C ( 501 ) RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S) H ( 323,X'S) RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 46,X'S) H ( 461,X'S) H ( 462,X'S) RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S) RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S) RIDE C ( 51,X'S) H ( 511,X'S) H ( 512,X'S) H ( 513,X'S) H ( 514,X'S) RIDE C ( 101,X'S) H (1011,X'S) RIDE C ( 102,X'S) H (1021,X'S) H (1022,X'S) H (1023,X'S) RIDE C ( 103,X'S) H (1031,X'S) H (1032,X'S) H (1033,X'S) RIDE C ( 105,X'S) H (1051,X'S) RIDE C ( 106,X'S) H (1061,X'S) RIDE C ( 107,X'S) H (1071,X'S) RIDE C ( 108,X'S) H (1081,X'S) RIDE C ( 109,X'S) H (1091,X'S) RIDE C ( 111,X'S) H (1111,X'S) RIDE C ( 112,X'S) H (1121,X'S) RIDE C ( 113,X'S) H (1131,X'S) RIDE C ( 114,X'S) H (1141,X'S) RIDE C ( 115,X'S) H (1151,X'S) RIDE C ( 116,X'S) H (1161,X'S) RIDE C ( 117,X'S) H (1171,X'S) H (1172,X'S) H (1173,X'S) RIDE C ( 118,X'S) H (1181,X'S) H (1182,X'S) H (1183,X'S) RIDE C ( 120,X'S) H (1201,X'S) RIDE C ( 121,X'S) H (1211,X'S) RIDE C ( 122,X'S) H (1221,X'S) RIDE C ( 123,X'S) H (1231,X'S) RIDE C ( 124,X'S) H (1241,X'S) RIDE C ( 126,X'S) H (1261,X'S) RIDE C ( 127,X'S) H (1271,X'S) RIDE C ( 128,X'S) H (1281,X'S) RIDE C ( 129,X'S) H (1291,X'S) RIDE C ( 130,X'S) H (1301,X'S) RIDE C ( 131,X'S) H (1311,X'S) RIDE C ( 132,X'S) H (1321,X'S) H (1322,X'S) H (1323,X'S) RIDE C ( 133,X'S) H (1331,X'S) H (1332,X'S) H (1333,X'S) RIDE C ( 135,X'S) H (1351,X'S) RIDE C ( 136,X'S) H (1361,X'S) RIDE C ( 137,X'S) H (1371,X'S) RIDE C ( 138,X'S) H (1381,X'S) RIDE C ( 139,X'S) H (1391,X'S) RIDE C ( 141,X'S) H (1411,X'S) RIDE C ( 142,X'S) H (1421,X'S) RIDE C ( 143,X'S) H (1431,X'S) RIDE C ( 144,X'S) H (1441,X'S) RIDE C ( 145,X'S) H (1451,X'S) RIDE C ( 500,X'S) H (5001,X'S) H (5002,X'S) RIDE C ( 501,X'S) H (5011,X'S) H (5012,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 19/02/13 at 09:25:24 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 938608' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_4 _audit_creation_date 13-02-14 _audit_creation_method CRYSTALS_ver_14.41 _oxford_structure_analysis_title 'SK_747_0m in P-3c1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 16.3841(5) _cell_length_b 16.3841(5) _cell_length_c 22.8729(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 5317.4(3) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P -3 c 1' _symmetry_space_group_name_Hall '-P 3 2"c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -y,x-y,z y,-x+y,-z -x+y,-x,z x-y,x,-z -x+y,y,z+1/2 x-y,-y,-z+1/2 x,x-y,z+1/2 -x,-x+y,-z+1/2 -y,-x,z+1/2 y,x,-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' 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' V 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780 1.2199 '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' 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 4 # Given Formula = C48 H60 Fe1.00 N3 O1.00 P4.00 V1.00 # Dc = 1.16 Fooo = 1912.00 Mu = 6.03 M = 308.57 # Found Formula = C48 H60 Fe1 N3 P4 V1 # Dc = 1.14 FOOO = 1912.00 Mu = 6.00 M = 303.24 _chemical_formula_sum 'C48 H60 Fe1 N3 P4 V1' _chemical_formula_moiety 'C48 H60 Fe1 N3 P4 V1' _chemical_compound_source ? _chemical_formula_weight 909.71 _cell_measurement_reflns_used 9966 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_min 0.190 _exptl_crystal_size_mid 0.350 _exptl_crystal_size_max 0.490 _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.600 # Sheldrick geometric approximatio 0.81 0.89 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.89 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _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 120 _diffrn_reflns_number 5179 _reflns_number_total 5179 _diffrn_reflns_av_R_equivalents 0.061 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 5179 # Theoretical number of reflections is about 10346 _diffrn_reflns_theta_min 3.059 _diffrn_reflns_theta_max 30.006 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.006 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -19 _reflns_limit_h_max 0 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _oxford_diffrn_Wilson_B_factor 1.29 _oxford_diffrn_Wilson_scale 151.57 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.38 _refine_diff_density_max 0.50 # 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>-10.0\s(I) _refine_ls_number_reflns 5179 _refine_ls_number_restraints 0 _refine_ls_number_parameters 172 _oxford_refine_ls_R_factor_ref 0.0446 _refine_ls_wR_factor_ref 0.0993 _refine_ls_goodness_of_fit_ref 1.0130 _refine_ls_shift/su_max 0.0011931 _refine_ls_shift/su_mean 0.0000678 # The values computed with all filters except I/sigma _oxford_reflns_number_all 5179 _refine_ls_R_factor_all 0.0446 _refine_ls_wR_factor_all 0.0993 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4019 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_gt 0.0871 # 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 #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^) + ( 0.05P)^2^ + 3.29P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens C1 C 0.63585(13) 0.49392(12) 0.25906(7) 0.0258 1.0000 Uani . . . . . . C2 C 0.72920(16) 0.58509(13) 0.24990(9) 0.0378 1.0000 Uani . . . . . . C3 C 0.60332(16) 0.43607(15) 0.20286(7) 0.0349 1.0000 Uani . . . . . . C4 C 0.68418(11) 0.56243(11) 0.40094(6) 0.0200 1.0000 Uani . . . . . . C5 C 0.77447(12) 0.60252(12) 0.42497(7) 0.0242 1.0000 Uani . . . . . . C6 C 0.82288(13) 0.69693(13) 0.44079(9) 0.0347 1.0000 Uani . . . . . . C7 C 0.78154(15) 0.75228(13) 0.43360(10) 0.0411 1.0000 Uani . . . . . . C8 C 0.69226(16) 0.71343(13) 0.40993(10) 0.0393 1.0000 Uani . . . . . . C9 C 0.64408(13) 0.61958(12) 0.39383(8) 0.0305 1.0000 Uani . . . . . . C10 C 0.50136(11) 0.40878(11) 0.38264(7) 0.0201 1.0000 Uani . . . . . . C11 C 0.46576(12) 0.42098(12) 0.43544(7) 0.0253 1.0000 Uani . . . . . . C12 C 0.37084(13) 0.39164(14) 0.44180(9) 0.0322 1.0000 Uani . . . . . . C13 C 0.30982(13) 0.35045(15) 0.39526(9) 0.0362 1.0000 Uani . . . . . . C14 C 0.34371(13) 0.33738(15) 0.34286(8) 0.0342 1.0000 Uani . . . . . . C15 C 0.43852(12) 0.36576(12) 0.33661(7) 0.0258 1.0000 Uani . . . . . . C16 C 0.55509(14) 0.29411(16) 0.54162(8) 0.0371 1.0000 Uani . . . . . . Fe1 Fe 0.6667 0.3333 0.402167(14) 0.0122 1.0000 Uani S T . . . . V1 V 0.6667 0.3333 0.312565(17) 0.0137 1.0000 Uani S T . . . . P1 P 0.62482(3) 0.43812(3) 0.377379(16) 0.0159 1.0000 Uani . . . . . . N1 N 0.64366(9) 0.43639(9) 0.30530(5) 0.0188 1.0000 Uani . . . . . . P2 P 0.6667 0.3333 0.50363(3) 0.0172 1.0000 Uani S T . . . . H11 H 0.5885 0.5092 0.2700 0.0294 1.0000 Uiso R . . . . . H33 H 0.5982 0.4724 0.1725 0.0386 1.0000 Uiso R . . . . . H31 H 0.6497 0.4192 0.1917 0.0386 1.0000 Uiso R . . . . . H32 H 0.5452 0.3806 0.2089 0.0386 1.0000 Uiso R . . . . . H22 H 0.7223 0.6199 0.2196 0.0449 1.0000 Uiso R . . . . . H23 H 0.7476 0.6193 0.2848 0.0449 1.0000 Uiso R . . . . . H21 H 0.7757 0.5685 0.2387 0.0449 1.0000 Uiso R . . . . . H91 H 0.5816 0.5921 0.3773 0.0336 1.0000 Uiso R . . . . . H81 H 0.6626 0.7515 0.4055 0.0466 1.0000 Uiso R . . . . . H71 H 0.8172 0.8180 0.4431 0.0471 1.0000 Uiso R . . . . . H61 H 0.8836 0.7231 0.4581 0.0374 1.0000 Uiso R . . . . . H51 H 0.8031 0.5649 0.4297 0.0278 1.0000 Uiso R . . . . . H151 H 0.4599 0.3551 0.3007 0.0285 1.0000 Uiso R . . . . . H141 H 0.3025 0.3099 0.3103 0.0384 1.0000 Uiso R . . . . . H131 H 0.2443 0.3312 0.3994 0.0412 1.0000 Uiso R . . . . . H121 H 0.3486 0.4011 0.4780 0.0350 1.0000 Uiso R . . . . . H111 H 0.5070 0.4488 0.4679 0.0288 1.0000 Uiso R . . . . . H163 H 0.5083 0.2359 0.5274 0.0426 1.0000 Uiso R . . . . . H162 H 0.5635 0.2883 0.5831 0.0426 1.0000 Uiso R . . . . . H161 H 0.5353 0.3399 0.5377 0.0426 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 C1 0.0374(9) 0.0287(8) 0.0190(7) 0.0053(6) -0.0027(6) 0.0223(7) C2 0.0518(12) 0.0292(9) 0.0301(9) 0.0112(7) 0.0047(8) 0.0186(9) C3 0.0528(12) 0.0413(10) 0.0185(7) 0.0033(7) -0.0067(8) 0.0295(10) C4 0.0242(7) 0.0178(7) 0.0189(7) -0.0003(5) -0.0015(6) 0.0113(6) C5 0.0229(8) 0.0232(8) 0.0269(8) -0.0041(6) -0.0017(6) 0.0118(7) C6 0.0249(9) 0.0270(9) 0.0453(11) -0.0094(8) -0.0044(8) 0.0077(7) C7 0.0395(11) 0.0197(8) 0.0574(13) -0.0084(8) -0.0026(10) 0.0098(8) C8 0.0471(12) 0.0210(8) 0.0548(13) -0.0022(8) -0.0057(10) 0.0207(9) C9 0.0337(9) 0.0226(8) 0.0392(10) -0.0033(7) -0.0108(8) 0.0172(7) C10 0.0222(7) 0.0204(7) 0.0214(7) -0.0015(6) -0.0025(6) 0.0136(6) C11 0.0262(8) 0.0283(8) 0.0258(8) -0.0070(6) -0.0022(6) 0.0171(7) C12 0.0295(9) 0.0383(10) 0.0361(9) -0.0058(8) 0.0031(7) 0.0225(8) C13 0.0223(8) 0.0445(11) 0.0468(11) -0.0057(9) -0.0021(8) 0.0204(8) C14 0.0252(9) 0.0442(11) 0.0347(9) -0.0070(8) -0.0096(7) 0.0184(8) C15 0.0249(8) 0.0327(9) 0.0226(7) -0.0049(7) -0.0050(6) 0.0165(7) C16 0.0303(9) 0.0576(13) 0.0210(8) 0.0012(8) 0.0065(7) 0.0203(9) Fe1 0.01302(11) 0.01302(11) 0.01066(15) 0.0000 0.0000 0.00651(6) V1 0.01507(13) 0.01507(13) 0.01106(18) 0.0000 0.0000 0.00753(6) P1 0.01868(18) 0.01625(18) 0.01472(16) -0.00085(13) -0.00206(13) 0.01018(15) N1 0.0248(6) 0.0199(6) 0.0150(5) 0.0019(5) -0.0004(5) 0.0137(5) P2 0.01990(19) 0.01990(19) 0.0117(3) 0.0000 0.0000 0.00995(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.08230(2) 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 C1 . C2 . 1.526(3) yes C1 . C3 . 1.526(2) yes C1 . N1 . 1.4644(19) yes C1 . H11 . 0.959 no C2 . H22 . 0.939 no C2 . H23 . 0.935 no C2 . H21 . 0.963 no C3 . H33 . 0.946 no C3 . H31 . 0.964 no C3 . H32 . 0.941 no C4 . C5 . 1.396(2) yes C4 . C9 . 1.396(2) yes C4 . P1 . 1.8449(16) yes C5 . C6 . 1.388(2) yes C5 . H51 . 0.948 no C6 . C7 . 1.386(3) yes C6 . H61 . 0.951 no C7 . C8 . 1.381(3) yes C7 . H71 . 0.959 no C8 . C9 . 1.382(3) yes C8 . H81 . 0.968 no C9 . H91 . 0.965 no C10 . C11 . 1.398(2) yes C10 . C15 . 1.393(2) yes C10 . P1 . 1.8344(16) yes C11 . C12 . 1.387(2) yes C11 . H111 . 0.952 no C12 . C13 . 1.383(3) yes C12 . H121 . 0.947 no C13 . C14 . 1.382(3) yes C13 . H131 . 0.961 no C14 . C15 . 1.388(2) yes C14 . H141 . 0.953 no C15 . H151 . 0.943 no C16 . P2 . 1.8263(18) yes C16 . H163 . 0.933 no C16 . H162 . 0.971 no C16 . H161 . 0.960 no Fe1 . P1 3_655 2.2172(4) yes Fe1 . P1 5_665 2.2172(4) yes Fe1 . V1 . 2.0495(5) yes Fe1 . P1 . 2.2172(4) yes Fe1 . P2 . 2.3206(7) yes V1 . P1 5_665 2.6062(4) yes V1 . P1 3_655 2.6062(4) yes V1 . N1 3_655 1.9123(12) yes V1 . N1 5_665 1.9123(12) yes V1 . P1 . 2.6062(4) yes V1 . N1 . 1.9123(12) yes P1 . N1 . 1.6801(13) 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 C2 . C1 . C3 . 111.10(15) yes C2 . C1 . N1 . 111.21(14) yes C3 . C1 . N1 . 108.93(14) yes C2 . C1 . H11 . 109.0 no C3 . C1 . H11 . 107.8 no N1 . C1 . H11 . 108.7 no C1 . C2 . H22 . 109.2 no C1 . C2 . H23 . 109.5 no H22 . C2 . H23 . 111.5 no C1 . C2 . H21 . 107.9 no H22 . C2 . H21 . 109.1 no H23 . C2 . H21 . 109.4 no C1 . C3 . H33 . 110.0 no C1 . C3 . H31 . 108.7 no H33 . C3 . H31 . 108.5 no C1 . C3 . H32 . 110.3 no H33 . C3 . H32 . 110.4 no H31 . C3 . H32 . 108.9 no C5 . C4 . C9 . 118.25(15) yes C5 . C4 . P1 . 118.95(12) yes C9 . C4 . P1 . 122.76(12) yes C4 . C5 . C6 . 120.50(16) yes C4 . C5 . H51 . 119.4 no C6 . C5 . H51 . 120.1 no C5 . C6 . C7 . 120.29(17) yes C5 . C6 . H61 . 119.8 no C7 . C6 . H61 . 119.9 no C6 . C7 . C8 . 119.75(17) yes C6 . C7 . H71 . 119.1 no C8 . C7 . H71 . 121.1 no C7 . C8 . C9 . 120.10(18) yes C7 . C8 . H81 . 120.1 no C9 . C8 . H81 . 119.8 no C4 . C9 . C8 . 121.11(17) yes C4 . C9 . H91 . 118.5 no C8 . C9 . H91 . 120.4 no C11 . C10 . C15 . 118.01(15) yes C11 . C10 . P1 . 120.22(12) yes C15 . C10 . P1 . 121.48(12) yes C10 . C11 . C12 . 121.11(16) yes C10 . C11 . H111 . 119.7 no C12 . C11 . H111 . 119.2 no C11 . C12 . C13 . 120.00(17) yes C11 . C12 . H121 . 119.4 no C13 . C12 . H121 . 120.6 no C12 . C13 . C14 . 119.65(17) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 120.2 no C13 . C14 . C15 . 120.43(17) yes C13 . C14 . H141 . 120.4 no C15 . C14 . H141 . 119.2 no C10 . C15 . C14 . 120.78(16) yes C10 . C15 . H151 . 120.2 no C14 . C15 . H151 . 119.0 no P2 . C16 . H163 . 111.2 no P2 . C16 . H162 . 109.4 no H163 . C16 . H162 . 108.9 no P2 . C16 . H161 . 110.6 no H163 . C16 . H161 . 109.9 no H162 . C16 . H161 . 106.8 no P1 3_655 Fe1 . P1 5_665 113.698(10) yes P1 3_655 Fe1 . V1 . 75.184(12) yes P1 5_665 Fe1 . V1 . 75.184(12) yes P1 3_655 Fe1 . P1 . 113.698(10) yes P1 5_665 Fe1 . P1 . 113.698(10) yes V1 . Fe1 . P1 . 75.184(12) yes P1 3_655 Fe1 . P2 . 104.816(12) yes P1 5_665 Fe1 . P2 . 104.816(12) yes V1 . Fe1 . P2 . 179.995 yes P1 . Fe1 . P2 . 104.816(12) yes P1 5_665 V1 . P1 3_655 90.840(15) yes P1 5_665 V1 . N1 3_655 122.24(4) yes P1 3_655 V1 . N1 3_655 40.08(4) yes P1 5_665 V1 . N1 5_665 40.08(4) yes P1 3_655 V1 . N1 5_665 112.32(4) yes N1 3_655 V1 . N1 5_665 119.254(12) yes P1 5_665 V1 . Fe1 . 55.332(11) yes P1 3_655 V1 . Fe1 . 55.332(11) yes N1 3_655 V1 . Fe1 . 94.98(4) yes N1 5_665 V1 . Fe1 . 94.98(4) yes P1 5_665 V1 . P1 . 90.840(15) yes P1 3_655 V1 . P1 . 90.840(15) yes N1 3_655 V1 . P1 . 112.32(4) yes N1 5_665 V1 . P1 . 122.24(4) yes Fe1 . V1 . P1 . 55.332(11) yes P1 5_665 V1 . N1 . 112.32(4) yes P1 3_655 V1 . N1 . 122.24(4) yes N1 3_655 V1 . N1 . 119.254(12) yes N1 5_665 V1 . N1 . 119.254(11) yes Fe1 . V1 . N1 . 94.98(4) yes P1 . V1 . N1 . 40.08(4) yes V1 . P1 . C4 . 136.58(5) yes V1 . P1 . C10 . 118.92(5) yes C4 . P1 . C10 . 100.00(7) yes V1 . P1 . Fe1 . 49.485(13) yes C4 . P1 . Fe1 . 125.71(5) yes C10 . P1 . Fe1 . 120.51(5) yes V1 . P1 . N1 . 47.13(4) yes C4 . P1 . N1 . 107.78(7) yes C10 . P1 . N1 . 104.35(7) yes Fe1 . P1 . N1 . 96.16(5) yes C1 . N1 . P1 . 128.46(11) yes C1 . N1 . V1 . 138.62(11) yes P1 . N1 . V1 . 92.79(6) yes C16 3_655 P2 . C16 . 99.22(8) yes C16 3_655 P2 . C16 5_665 99.22(8) yes C16 . P2 . C16 5_665 99.22(8) yes C16 3_655 P2 . Fe1 . 118.42(6) yes C16 . P2 . Fe1 . 118.42(6) yes C16 5_665 P2 . Fe1 . 118.42(6) yes _iucr_refine_instructions_details_constraints ; # # Punched on 14/02/13 at 13:07:02 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 22,X'S) H ( 23,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 33,X'S) H ( 31,X'S) H ( 32,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 163,X'S) H ( 162,X'S) H ( 161,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 14/02/13 at 13:07:02 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.000 0.000 -0.001 948 70 ' ' _platon_squeeze_details ; During the structure solution, electron density difference maps revealed that there was a disordered solvent molecule which could not be successfully modeled. The solvate was highly disordered due to symmetry in a volume of 949 cubic angstroms per unit cell. It appeared that the cavity area contained ca. 2 ether molecules, located near (0, 0, 0). Modeling with or without restraints was unsuccessful, as was step by step acquisition of peaks using successive electron density difference maps. Thus, the structure factors were modified using the PLATON SQUEEZE technique, in order to produce a "solvate-free" structure factor set. PLATON reported a total electron density of 70 e- per unit cell, likely representing two ether molecules, consistent with our earlier observations. Use of the SQUEEZE technique resulted in a decrease of ca. 1.6 % in R. ; _database_code_depnum_ccdc_archive 'CCDC 938609' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_5 _audit_creation_date 2012-11-27 _audit_creation_method CRYSTALS_ver_14.52 _oxford_structure_analysis_title 'SK_715_0m in P2(1)/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.0944(3) _cell_length_b 14.5742(4) _cell_length_c 28.4690(8) _cell_angle_alpha 90 _cell_angle_beta 95.9356(14) _cell_angle_gamma 90 _cell_volume 5403.9(2) _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' 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' V 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780 1.2199 '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' _cell_formula_units_Z 4 # Given Formula = C60 H69 Fe1 N4 P4 V1 # Dc = 1.32 Fooo = 2264.00 Mu = 6.03 M = 1076.92 # Found Formula = C60 H69 Fe1 N4 P4 V1 # Dc = 1.32 FOOO = 2264.00 Mu = 6.03 M = 1076.92 _chemical_formula_sum 'C60 H69 Fe1 N4 P4 V1' _chemical_formula_moiety 'C60 H69 Fe1 N4 P4 V1' _chemical_compound_source ? _chemical_formula_weight 1076.92 _cell_measurement_reflns_used 7457 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _cell_measurement_temperature 135 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_min 0.150 _exptl_crystal_size_mid 0.218 _exptl_crystal_size_max 0.226 _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 0.603 # Sheldrick geometric approximatio 0.88 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.91 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _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 135 _diffrn_reflns_number 13563 _reflns_number_total 13563 _diffrn_reflns_av_R_equivalents 0.000 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 13563 # Theoretical number of reflections is about 27312 _diffrn_reflns_theta_min 1.438 _diffrn_reflns_theta_max 28.467 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.898 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 38 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 38 _oxford_diffrn_Wilson_B_factor 1.39 _oxford_diffrn_Wilson_scale 36.88 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.77 _refine_diff_density_max 0.72 # 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>-10.0\s(I) _refine_ls_number_reflns 13563 _refine_ls_number_restraints 0 _refine_ls_number_parameters 631 _oxford_refine_ls_R_factor_ref 0.0859 _refine_ls_wR_factor_ref 0.1004 _refine_ls_goodness_of_fit_ref 0.9637 _refine_ls_shift/su_max 0.0013062 _refine_ls_shift/su_mean 0.0000733 # The values computed with all filters except I/sigma _oxford_reflns_number_all 13563 _refine_ls_R_factor_all 0.0859 _refine_ls_wR_factor_all 0.1004 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9252 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_gt 0.0915 # 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 #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^ + 3.30P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Fe1 Fe 0.75307(2) 0.73790(2) 0.623595(10) 0.0148 1.0000 Uani . . . . . . V1 V 0.90527(3) 0.74245(3) 0.649931(12) 0.0163 1.0000 Uani . . . . . . P1 P 0.83486(5) 0.65819(4) 0.571841(19) 0.0176 1.0000 Uani . . . . . . P2 P 0.79203(5) 0.88644(4) 0.62755(2) 0.0189 1.0000 Uani . . . . . . P3 P 0.76248(5) 0.66089(4) 0.692421(19) 0.0179 1.0000 Uani . . . . . . P4 P 0.57980(4) 0.74952(4) 0.595911(19) 0.0174 1.0000 Uani . . . . . . N1 N 0.95202(14) 0.66247(14) 0.60292(6) 0.0198 1.0000 Uani . . . . . . N2 N 0.91763(14) 0.87280(13) 0.64538(6) 0.0196 1.0000 Uani . . . . . . N3 N 0.88576(15) 0.68908(13) 0.70944(6) 0.0197 1.0000 Uani . . . . . . N4 N 0.51691(16) 0.83082(14) 0.62433(7) 0.0259 1.0000 Uani . . . . . . C1 C 0.79903(18) 0.53777(16) 0.55900(7) 0.0199 1.0000 Uani . . . . . . C2 C 0.8606(2) 0.47439(17) 0.53854(8) 0.0265 1.0000 Uani . . . . . . C3 C 0.8307(2) 0.38314(17) 0.53304(9) 0.0302 1.0000 Uani . . . . . . C4 C 0.7361(2) 0.35531(18) 0.54622(9) 0.0300 1.0000 Uani . . . . . . C5 C 0.6736(2) 0.41797(17) 0.56570(8) 0.0272 1.0000 Uani . . . . . . C6 C 0.70533(19) 0.50792(17) 0.57226(8) 0.0230 1.0000 Uani . . . . . . C7 C 0.86212(18) 0.70093(16) 0.51332(8) 0.0199 1.0000 Uani . . . . . . C8 C 0.91672(19) 0.78231(17) 0.51222(8) 0.0257 1.0000 Uani . . . . . . C9 C 0.9366(2) 0.82253(19) 0.47006(9) 0.0306 1.0000 Uani . . . . . . C10 C 0.9023(2) 0.78089(19) 0.42778(9) 0.0346 1.0000 Uani . . . . . . C11 C 0.8484(2) 0.6999(2) 0.42788(9) 0.0368 1.0000 Uani . . . . . . C12 C 0.8280(2) 0.65962(18) 0.47041(8) 0.0269 1.0000 Uani . . . . . . C13 C 1.04931(18) 0.62849(18) 0.58777(9) 0.0253 1.0000 Uani . . . . . . C14 C 1.1334(2) 0.7002(2) 0.59751(11) 0.0439 1.0000 Uani . . . . . . C15 C 1.0820(2) 0.5386(2) 0.61178(10) 0.0374 1.0000 Uani . . . . . . C16 C 0.74206(19) 0.96044(17) 0.67266(8) 0.0255 1.0000 Uani . . . . . . C17 C 0.7774(2) 0.94620(19) 0.72007(9) 0.0308 1.0000 Uani . . . . . . C18 C 0.7365(2) 0.9972(2) 0.75518(10) 0.0399 1.0000 Uani . . . . . . C19 C 0.6618(3) 1.0616(2) 0.74337(12) 0.0504 1.0000 Uani . . . . . . C20 C 0.6259(3) 1.0756(2) 0.69727(12) 0.0521 1.0000 Uani . . . . . . C21 C 0.6649(2) 1.0250(2) 0.66184(10) 0.0382 1.0000 Uani . . . . . . C22 C 0.78203(18) 0.96518(17) 0.57677(9) 0.0249 1.0000 Uani . . . . . . C23 C 0.8123(2) 1.05725(19) 0.58082(10) 0.0348 1.0000 Uani . . . . . . C24 C 0.8124(2) 1.1115(2) 0.54073(13) 0.0482 1.0000 Uani . . . . . . C25 C 0.7816(2) 1.0757(2) 0.49665(12) 0.0488 1.0000 Uani . . . . . . C26 C 0.7508(2) 0.9861(2) 0.49219(10) 0.0416 1.0000 Uani . . . . . . C27 C 0.75137(19) 0.93094(19) 0.53228(8) 0.0284 1.0000 Uani . . . . . . C28 C 0.99628(19) 0.94343(17) 0.65720(8) 0.0247 1.0000 Uani . . . . . . C29 C 1.0714(2) 0.9102(2) 0.69804(9) 0.0334 1.0000 Uani . . . . . . C30 C 1.0535(2) 0.9657(2) 0.61456(10) 0.0348 1.0000 Uani . . . . . . C31 C 0.76342(18) 0.53427(16) 0.69397(8) 0.0211 1.0000 Uani . . . . . . C32 C 0.84440(19) 0.49067(17) 0.67449(8) 0.0244 1.0000 Uani . . . . . . C33 C 0.8484(2) 0.39658(18) 0.67026(9) 0.0299 1.0000 Uani . . . . . . C34 C 0.7721(2) 0.34281(19) 0.68557(9) 0.0350 1.0000 Uani . . . . . . C35 C 0.6913(2) 0.38365(19) 0.70519(9) 0.0357 1.0000 Uani . . . . . . C36 C 0.6868(2) 0.47909(18) 0.70948(9) 0.0300 1.0000 Uani . . . . . . C37 C 0.69034(18) 0.69004(17) 0.74274(8) 0.0206 1.0000 Uani . . . . . . C38 C 0.7008(2) 0.64447(18) 0.78629(8) 0.0277 1.0000 Uani . . . . . . C39 C 0.6544(2) 0.6789(2) 0.82428(9) 0.0343 1.0000 Uani . . . . . . C40 C 0.5965(2) 0.7575(2) 0.81963(9) 0.0333 1.0000 Uani . . . . . . C41 C 0.5837(2) 0.80266(19) 0.77660(9) 0.0314 1.0000 Uani . . . . . . C42 C 0.63095(19) 0.76880(18) 0.73871(8) 0.0273 1.0000 Uani . . . . . . C43 C 0.94660(19) 0.66218(18) 0.75344(8) 0.0264 1.0000 Uani . . . . . . C44 C 1.0559(2) 0.6415(2) 0.74421(10) 0.0388 1.0000 Uani . . . . . . C45 C 0.9438(2) 0.7366(2) 0.79090(9) 0.0378 1.0000 Uani . . . . . . C46 C 0.54887(18) 0.77991(16) 0.53325(7) 0.0200 1.0000 Uani . . . . . . C47 C 0.5846(2) 0.72380(18) 0.49889(8) 0.0276 1.0000 Uani . . . . . . C48 C 0.5651(2) 0.7452(2) 0.45143(9) 0.0355 1.0000 Uani . . . . . . C49 C 0.5096(2) 0.8233(2) 0.43730(9) 0.0336 1.0000 Uani . . . . . . C50 C 0.4742(2) 0.87982(19) 0.47087(8) 0.0295 1.0000 Uani . . . . . . C51 C 0.49455(19) 0.85845(17) 0.51859(8) 0.0251 1.0000 Uani . . . . . . C52 C 0.49456(17) 0.64898(16) 0.59854(8) 0.0194 1.0000 Uani . . . . . . C53 C 0.4275(2) 0.61832(19) 0.56101(9) 0.0327 1.0000 Uani . . . . . . C54 C 0.3692(2) 0.5395(2) 0.56493(10) 0.0397 1.0000 Uani . . . . . . C55 C 0.3765(2) 0.49054(18) 0.60631(9) 0.0306 1.0000 Uani . . . . . . C56 C 0.4425(2) 0.52077(19) 0.64401(9) 0.0325 1.0000 Uani . . . . . . C57 C 0.5007(2) 0.59857(18) 0.64005(8) 0.0287 1.0000 Uani . . . . . . C58 C 0.40610(19) 0.84488(19) 0.62622(9) 0.0290 1.0000 Uani . . . . . . C59 C 0.3668(2) 0.7968(2) 0.66834(10) 0.0413 1.0000 Uani . . . . . . C60 C 0.3840(2) 0.9473(2) 0.62843(11) 0.0416 1.0000 Uani . . . . . . H4 H 0.5560 0.8639 0.6431 0.0316 1.0000 Uiso R . . . . . H21 H 0.9227 0.4932 0.5281 0.0323 1.0000 Uiso R . . . . . H31 H 0.8736 0.3404 0.5208 0.0356 1.0000 Uiso R . . . . . H41 H 0.7140 0.2938 0.5414 0.0355 1.0000 Uiso R . . . . . H51 H 0.6103 0.3994 0.5746 0.0333 1.0000 Uiso R . . . . . H61 H 0.6622 0.5493 0.5857 0.0270 1.0000 Uiso R . . . . . H81 H 0.9396 0.8116 0.5410 0.0309 1.0000 Uiso R . . . . . H91 H 0.9720 0.8772 0.4705 0.0367 1.0000 Uiso R . . . . . H101 H 0.9168 0.8071 0.3992 0.0425 1.0000 Uiso R . . . . . H111 H 0.8253 0.6714 0.3999 0.0445 1.0000 Uiso R . . . . . H121 H 0.7913 0.6052 0.4707 0.0315 1.0000 Uiso R . . . . . H131 H 1.0383 0.6178 0.5535 0.0290 1.0000 Uiso R . . . . . H141 H 1.1962 0.6777 0.5878 0.0656 1.0000 Uiso R . . . . . H142 H 1.1429 0.7115 0.6310 0.0654 1.0000 Uiso R . . . . . H143 H 1.1137 0.7558 0.5813 0.0654 1.0000 Uiso R . . . . . H151 H 1.1423 0.5137 0.5996 0.0551 1.0000 Uiso R . . . . . H152 H 1.0964 0.5483 0.6453 0.0556 1.0000 Uiso R . . . . . H153 H 1.0265 0.4938 0.6060 0.0555 1.0000 Uiso R . . . . . H171 H 0.8272 0.9017 0.7281 0.0362 1.0000 Uiso R . . . . . H181 H 0.7605 0.9858 0.7871 0.0475 1.0000 Uiso R . . . . . H191 H 0.6347 1.0968 0.7662 0.0604 1.0000 Uiso R . . . . . H201 H 0.5750 1.1194 0.6895 0.0622 1.0000 Uiso R . . . . . H211 H 0.6381 1.0346 0.6303 0.0462 1.0000 Uiso R . . . . . H231 H 0.8330 1.0822 0.6102 0.0413 1.0000 Uiso R . . . . . H241 H 0.8335 1.1727 0.5443 0.0573 1.0000 Uiso R . . . . . H251 H 0.7814 1.1126 0.4694 0.0591 1.0000 Uiso R . . . . . H261 H 0.7286 0.9614 0.4626 0.0503 1.0000 Uiso R . . . . . H271 H 0.7301 0.8694 0.5293 0.0330 1.0000 Uiso R . . . . . H281 H 0.9618 0.9998 0.6671 0.0303 1.0000 Uiso R . . . . . H291 H 1.1038 0.8533 0.6897 0.0489 1.0000 Uiso R . . . . . H292 H 1.1244 0.9552 0.7052 0.0498 1.0000 Uiso R . . . . . H293 H 1.0374 0.9009 0.7254 0.0494 1.0000 Uiso R . . . . . H301 H 1.0918 0.9138 0.6056 0.0522 1.0000 Uiso R . . . . . H302 H 1.1023 1.0146 0.6219 0.0519 1.0000 Uiso R . . . . . H303 H 1.0076 0.9848 0.5878 0.0516 1.0000 Uiso R . . . . . H321 H 0.8960 0.5265 0.6646 0.0288 1.0000 Uiso R . . . . . H331 H 0.9046 0.3689 0.6566 0.0360 1.0000 Uiso R . . . . . H341 H 0.7744 0.2784 0.6831 0.0417 1.0000 Uiso R . . . . . H351 H 0.6392 0.3486 0.7163 0.0432 1.0000 Uiso R . . . . . H361 H 0.6328 0.5070 0.7235 0.0355 1.0000 Uiso R . . . . . H381 H 0.7402 0.5915 0.7898 0.0329 1.0000 Uiso R . . . . . H391 H 0.6645 0.6490 0.8525 0.0411 1.0000 Uiso R . . . . . H401 H 0.5645 0.7810 0.8452 0.0394 1.0000 Uiso R . . . . . H411 H 0.5442 0.8543 0.7731 0.0378 1.0000 Uiso R . . . . . H421 H 0.6215 0.7994 0.7095 0.0327 1.0000 Uiso R . . . . . H431 H 0.9175 0.6069 0.7648 0.0320 1.0000 Uiso R . . . . . H441 H 1.0584 0.5908 0.7226 0.0574 1.0000 Uiso R . . . . . H442 H 1.0885 0.6943 0.7309 0.0578 1.0000 Uiso R . . . . . H443 H 1.0961 0.6249 0.7733 0.0573 1.0000 Uiso R . . . . . H451 H 0.8739 0.7497 0.7965 0.0564 1.0000 Uiso R . . . . . H452 H 0.9741 0.7913 0.7797 0.0557 1.0000 Uiso R . . . . . H453 H 0.9834 0.7161 0.8199 0.0566 1.0000 Uiso R . . . . . H471 H 0.6214 0.6703 0.5082 0.0324 1.0000 Uiso R . . . . . H481 H 0.5888 0.7055 0.4299 0.0430 1.0000 Uiso R . . . . . H491 H 0.4960 0.8381 0.4053 0.0402 1.0000 Uiso R . . . . . H501 H 0.4351 0.9332 0.4616 0.0341 1.0000 Uiso R . . . . . H511 H 0.4718 0.8989 0.5410 0.0298 1.0000 Uiso R . . . . . H531 H 0.4211 0.6511 0.5320 0.0393 1.0000 Uiso R . . . . . H541 H 0.3249 0.5197 0.5397 0.0482 1.0000 Uiso R . . . . . H551 H 0.3367 0.4374 0.6095 0.0369 1.0000 Uiso R . . . . . H561 H 0.4481 0.4877 0.6726 0.0395 1.0000 Uiso R . . . . . H571 H 0.5460 0.6180 0.6656 0.0340 1.0000 Uiso R . . . . . H581 H 0.3685 0.8190 0.5963 0.0335 1.0000 Uiso R . . . . . H591 H 0.4027 0.8225 0.6975 0.0619 1.0000 Uiso R . . . . . H592 H 0.2928 0.8099 0.6683 0.0615 1.0000 Uiso R . . . . . H593 H 0.3782 0.7306 0.6670 0.0619 1.0000 Uiso R . . . . . H601 H 0.3085 0.9559 0.6284 0.0611 1.0000 Uiso R . . . . . H602 H 0.4191 0.9721 0.6581 0.0610 1.0000 Uiso R . . . . . H603 H 0.4070 0.9796 0.6005 0.0619 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 Fe1 0.01671(16) 0.01335(16) 0.01438(15) -0.00016(12) 0.00132(11) -0.00047(14) V1 0.0185(2) 0.0145(2) 0.01607(18) -0.00004(14) 0.00201(14) -0.00001(16) P1 0.0212(3) 0.0155(3) 0.0163(3) -0.0014(2) 0.0029(2) -0.0007(3) P2 0.0198(3) 0.0147(3) 0.0220(3) -0.0001(2) 0.0017(2) 0.0003(3) P3 0.0203(3) 0.0175(3) 0.0161(3) 0.0007(2) 0.0023(2) -0.0002(3) P4 0.0197(3) 0.0176(3) 0.0148(3) 0.0002(2) 0.0011(2) -0.0007(3) N1 0.0195(10) 0.0204(10) 0.0194(9) -0.0037(8) 0.0023(7) 0.0023(9) N2 0.0196(10) 0.0156(10) 0.0236(10) -0.0014(8) 0.0016(8) -0.0026(8) N3 0.0214(11) 0.0203(10) 0.0168(9) 0.0008(8) -0.0002(7) -0.0018(8) N4 0.0271(12) 0.0259(12) 0.0239(10) -0.0045(8) -0.0009(8) 0.0023(10) C1 0.0252(13) 0.0193(12) 0.0148(11) -0.0016(9) 0.0006(9) 0.0009(10) C2 0.0322(15) 0.0252(14) 0.0236(12) -0.0027(10) 0.0103(10) -0.0020(11) C3 0.0418(17) 0.0177(13) 0.0323(14) -0.0054(10) 0.0089(11) 0.0033(12) C4 0.0372(16) 0.0191(13) 0.0333(14) -0.0023(10) 0.0012(11) -0.0042(12) C5 0.0286(14) 0.0227(13) 0.0302(13) 0.0014(10) 0.0031(10) -0.0057(11) C6 0.0238(13) 0.0211(13) 0.0239(12) -0.0012(9) 0.0018(9) 0.0014(10) C7 0.0211(13) 0.0193(12) 0.0201(11) 0.0007(9) 0.0057(9) 0.0007(10) C8 0.0276(14) 0.0250(14) 0.0250(12) -0.0014(10) 0.0051(10) -0.0020(11) C9 0.0341(15) 0.0259(14) 0.0337(14) 0.0050(11) 0.0123(11) -0.0057(12) C10 0.0484(18) 0.0318(16) 0.0256(13) 0.0090(11) 0.0134(12) 0.0033(13) C11 0.0532(19) 0.0393(17) 0.0179(12) -0.0025(11) 0.0027(12) -0.0007(14) C12 0.0356(15) 0.0225(13) 0.0227(12) -0.0007(10) 0.0033(10) -0.0053(12) C13 0.0219(13) 0.0261(14) 0.0282(13) -0.0055(10) 0.0047(10) 0.0031(11) C14 0.0244(15) 0.0431(18) 0.066(2) -0.0207(15) 0.0106(14) -0.0014(14) C15 0.0326(16) 0.0391(17) 0.0412(16) 0.0019(13) 0.0068(12) 0.0185(14) C16 0.0256(14) 0.0203(13) 0.0312(13) -0.0070(10) 0.0056(10) -0.0058(11) C17 0.0277(15) 0.0317(15) 0.0331(14) -0.0049(11) 0.0041(11) -0.0045(12) C18 0.0425(18) 0.0445(18) 0.0343(15) -0.0159(13) 0.0122(13) -0.0138(15) C19 0.051(2) 0.0423(19) 0.062(2) -0.0239(16) 0.0262(16) -0.0012(16) C20 0.046(2) 0.043(2) 0.069(2) -0.0112(17) 0.0138(17) 0.0163(16) C21 0.0372(17) 0.0323(16) 0.0448(17) -0.0043(13) 0.0034(13) 0.0102(13) C22 0.0177(13) 0.0200(13) 0.0372(14) 0.0077(10) 0.0028(10) 0.0009(10) C23 0.0275(15) 0.0247(15) 0.0511(17) 0.0082(12) -0.0016(12) 0.0004(12) C24 0.0285(17) 0.0245(16) 0.093(3) 0.0292(16) 0.0112(16) 0.0038(13) C25 0.0339(17) 0.057(2) 0.058(2) 0.0393(17) 0.0156(15) 0.0123(16) C26 0.0338(16) 0.055(2) 0.0373(16) 0.0226(14) 0.0094(12) 0.0100(15) C27 0.0234(14) 0.0321(15) 0.0301(13) 0.0098(11) 0.0040(10) 0.0043(12) C28 0.0246(14) 0.0150(12) 0.0344(13) -0.0031(10) 0.0024(10) -0.0034(10) C29 0.0306(15) 0.0321(15) 0.0356(14) -0.0030(12) -0.0059(11) -0.0054(12) C30 0.0260(15) 0.0315(16) 0.0478(17) 0.0099(12) 0.0090(12) -0.0029(12) C31 0.0243(13) 0.0192(12) 0.0193(11) 0.0021(9) -0.0013(9) 0.0003(10) C32 0.0278(14) 0.0212(13) 0.0236(12) 0.0026(10) -0.0004(10) 0.0008(11) C33 0.0349(15) 0.0258(14) 0.0283(13) 0.0020(11) -0.0005(11) 0.0054(12) C34 0.0487(18) 0.0201(13) 0.0347(14) 0.0030(11) -0.0029(12) 0.0028(13) C35 0.0398(17) 0.0266(15) 0.0401(16) 0.0058(12) 0.0018(12) -0.0095(13) C36 0.0322(15) 0.0283(15) 0.0294(13) 0.0031(11) 0.0034(11) -0.0003(12) C37 0.0193(12) 0.0240(13) 0.0186(11) -0.0009(9) 0.0022(9) -0.0048(10) C38 0.0323(15) 0.0265(14) 0.0245(12) 0.0028(10) 0.0042(10) -0.0012(12) C39 0.0443(17) 0.0408(17) 0.0190(12) 0.0026(11) 0.0095(11) -0.0100(14) C40 0.0390(16) 0.0370(16) 0.0260(13) -0.0081(11) 0.0137(11) -0.0120(14) C41 0.0358(16) 0.0280(14) 0.0317(14) -0.0053(11) 0.0091(11) 0.0017(12) C42 0.0323(14) 0.0296(14) 0.0200(12) -0.0016(10) 0.0035(10) 0.0007(12) C43 0.0276(14) 0.0282(14) 0.0223(12) 0.0073(10) -0.0026(10) -0.0039(12) C44 0.0313(16) 0.0448(19) 0.0383(16) 0.0054(13) -0.0063(12) 0.0082(14) C45 0.0424(17) 0.0482(18) 0.0219(13) -0.0004(12) -0.0013(11) -0.0127(15) C46 0.0212(12) 0.0210(12) 0.0176(11) 0.0022(9) 0.0006(9) -0.0026(10) C47 0.0337(15) 0.0271(14) 0.0214(12) 0.0006(10) 0.0007(10) 0.0084(12) C48 0.0439(17) 0.0416(17) 0.0206(12) -0.0029(11) 0.0023(11) 0.0124(14) C49 0.0367(16) 0.0454(18) 0.0189(12) 0.0066(11) 0.0034(11) 0.0094(13) C50 0.0330(15) 0.0293(14) 0.0258(13) 0.0108(11) 0.0017(10) 0.0074(12) C51 0.0283(14) 0.0246(13) 0.0226(12) 0.0008(10) 0.0038(10) 0.0009(11) C52 0.0153(11) 0.0192(12) 0.0239(12) -0.0015(9) 0.0025(9) -0.0004(10) C53 0.0376(16) 0.0333(15) 0.0255(13) 0.0038(11) -0.0047(11) -0.0099(13) C54 0.0423(18) 0.0385(17) 0.0354(15) -0.0009(12) -0.0101(12) -0.0180(14) C55 0.0276(15) 0.0209(14) 0.0435(15) 0.0026(11) 0.0050(11) -0.0056(11) C56 0.0343(16) 0.0322(15) 0.0311(14) 0.0101(11) 0.0041(11) -0.0055(13) C57 0.0290(14) 0.0316(15) 0.0245(12) 0.0028(10) -0.0020(10) -0.0067(12) C58 0.0249(14) 0.0340(15) 0.0275(13) -0.0050(11) -0.0002(10) 0.0063(12) C59 0.0362(17) 0.050(2) 0.0395(16) 0.0020(14) 0.0118(13) 0.0016(14) C60 0.0388(18) 0.0388(18) 0.0473(17) -0.0043(14) 0.0046(13) 0.0102(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.16819(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 Fe1 . V1 . 2.0565(5) yes Fe1 . P1 . 2.2346(6) yes Fe1 . P2 . 2.2244(7) yes Fe1 . P3 . 2.2504(6) yes Fe1 . P4 . 2.3298(6) yes V1 . P1 . 2.6223(7) yes V1 . P2 . 2.6103(7) yes V1 . P3 . 2.6153(7) yes V1 . N1 . 1.9220(18) yes V1 . N2 . 1.9123(19) yes V1 . N3 . 1.9053(18) yes P1 . N1 . 1.6909(19) yes P1 . C1 . 1.843(2) yes P1 . C7 . 1.848(2) yes P2 . N2 . 1.682(2) yes P2 . C16 . 1.848(2) yes P2 . C22 . 1.840(2) yes P3 . N3 . 1.687(2) yes P3 . C31 . 1.846(2) yes P3 . C37 . 1.845(2) yes P4 . N4 . 1.695(2) yes P4 . C46 . 1.842(2) yes P4 . C52 . 1.848(2) yes N1 . C13 . 1.472(3) yes N2 . C28 . 1.470(3) yes N3 . C43 . 1.467(3) yes N4 . C58 . 1.472(3) yes N4 . H4 . 0.852 no C1 . C2 . 1.393(3) yes C1 . C6 . 1.390(3) yes C2 . C3 . 1.391(3) yes C2 . H21 . 0.936 no C3 . C4 . 1.392(4) yes C3 . H31 . 0.930 no C4 . C5 . 1.380(4) yes C4 . H41 . 0.947 no C5 . C6 . 1.382(3) yes C5 . H51 . 0.931 no C6 . H61 . 0.935 no C7 . C8 . 1.387(3) yes C7 . C12 . 1.393(3) yes C8 . C9 . 1.384(3) yes C8 . H81 . 0.945 no C9 . C10 . 1.381(4) yes C9 . H91 . 0.922 no C10 . C11 . 1.376(4) yes C10 . H101 . 0.935 no C11 . C12 . 1.396(3) yes C11 . H111 . 0.922 no C12 . H121 . 0.928 no C13 . C14 . 1.523(4) yes C13 . C15 . 1.519(4) yes C13 . H131 . 0.985 no C14 . H141 . 0.953 no C14 . H142 . 0.964 no C14 . H143 . 0.955 no C15 . H151 . 0.966 no C15 . H152 . 0.963 no C15 . H153 . 0.978 no C16 . C17 . 1.396(3) yes C16 . C21 . 1.392(4) yes C17 . C18 . 1.396(4) yes C17 . H171 . 0.932 no C18 . C19 . 1.373(4) yes C18 . H181 . 0.945 no C19 . C20 . 1.363(5) yes C19 . H191 . 0.927 no C20 . C21 . 1.388(4) yes C20 . H201 . 0.933 no C21 . H211 . 0.941 no C22 . C23 . 1.400(4) yes C22 . C27 . 1.382(4) yes C23 . C24 . 1.389(4) yes C23 . H231 . 0.926 no C24 . C25 . 1.380(5) yes C24 . H241 . 0.936 no C25 . C26 . 1.368(5) yes C25 . H251 . 0.944 no C26 . C27 . 1.396(3) yes C26 . H261 . 0.936 no C27 . H271 . 0.941 no C28 . C29 . 1.522(3) yes C28 . C30 . 1.526(3) yes C28 . H281 . 0.993 no C29 . H291 . 0.972 no C29 . H292 . 0.962 no C29 . H293 . 0.946 no C30 . H301 . 0.957 no C30 . H302 . 0.965 no C30 . H303 . 0.961 no C31 . C32 . 1.399(3) yes C31 . C36 . 1.393(3) yes C32 . C33 . 1.378(4) yes C32 . H321 . 0.921 no C33 . C34 . 1.376(4) yes C33 . H331 . 0.956 no C34 . C35 . 1.381(4) yes C34 . H341 . 0.942 no C35 . C36 . 1.398(4) yes C35 . H351 . 0.934 no C36 . H361 . 0.939 no C37 . C38 . 1.401(3) yes C37 . C42 . 1.385(3) yes C38 . C39 . 1.388(3) yes C38 . H381 . 0.928 no C39 . C40 . 1.373(4) yes C39 . H391 . 0.912 no C40 . C41 . 1.385(4) yes C40 . H401 . 0.941 no C41 . C42 . 1.389(3) yes C41 . H411 . 0.913 no C42 . H421 . 0.940 no C43 . C44 . 1.512(4) yes C43 . C45 . 1.524(4) yes C43 . H431 . 0.961 no C44 . H441 . 0.964 no C44 . H442 . 0.975 no C44 . H443 . 0.965 no C45 . H451 . 0.964 no C45 . H452 . 0.959 no C45 . H453 . 0.976 no C46 . C47 . 1.392(3) yes C46 . C51 . 1.389(3) yes C47 . C48 . 1.385(3) yes C47 . H471 . 0.941 no C48 . C49 . 1.387(4) yes C48 . H481 . 0.919 no C49 . C50 . 1.378(4) yes C49 . H491 . 0.935 no C50 . C51 . 1.393(3) yes C50 . H501 . 0.954 no C51 . H511 . 0.938 no C52 . C53 . 1.385(3) yes C52 . C57 . 1.387(3) yes C53 . C54 . 1.390(4) yes C53 . H531 . 0.951 no C54 . C55 . 1.372(4) yes C54 . H541 . 0.922 no C55 . C56 . 1.379(4) yes C55 . H551 . 0.943 no C56 . C57 . 1.378(4) yes C56 . H561 . 0.942 no C57 . H571 . 0.934 no C58 . C59 . 1.523(4) yes C58 . C60 . 1.523(4) yes C58 . H581 . 1.011 no C59 . H591 . 0.984 no C59 . H592 . 0.988 no C59 . H593 . 0.977 no C60 . H601 . 0.996 no C60 . H602 . 0.987 no C60 . H603 . 0.997 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 V1 . Fe1 . P1 . 75.21(2) yes V1 . Fe1 . P2 . 75.03(2) yes P1 . Fe1 . P2 . 114.60(3) yes V1 . Fe1 . P3 . 74.63(2) yes P1 . Fe1 . P3 . 109.15(3) yes P2 . Fe1 . P3 . 116.72(3) yes V1 . Fe1 . P4 . 173.78(2) yes P1 . Fe1 . P4 . 109.34(2) yes P2 . Fe1 . P4 . 99.01(2) yes P3 . Fe1 . P4 . 107.13(2) yes Fe1 . V1 . P1 . 55.480(18) yes Fe1 . V1 . P2 . 55.409(18) yes P1 . V1 . P2 . 91.63(2) yes Fe1 . V1 . P3 . 56.066(18) yes P1 . V1 . P3 . 88.50(2) yes P2 . V1 . P3 . 93.61(2) yes Fe1 . V1 . N1 . 95.33(6) yes P1 . V1 . N1 . 40.09(6) yes P2 . V1 . N1 . 122.10(6) yes P3 . V1 . N1 . 109.93(6) yes Fe1 . V1 . N2 . 95.33(6) yes P1 . V1 . N2 . 115.63(6) yes P2 . V1 . N2 . 40.06(6) yes P3 . V1 . N2 . 123.54(6) yes N1 . V1 . N2 . 121.33(8) yes Fe1 . V1 . N3 . 95.57(6) yes P1 . V1 . N3 . 119.67(6) yes P2 . V1 . N3 . 114.85(6) yes P3 . V1 . N3 . 40.11(6) yes N1 . V1 . N3 . 116.96(8) yes N2 . V1 . N3 . 119.07(8) yes V1 . P1 . Fe1 . 49.311(16) yes V1 . P1 . N1 . 47.06(6) yes Fe1 . P1 . N1 . 96.12(7) yes V1 . P1 . C1 . 132.37(7) yes Fe1 . P1 . C1 . 119.74(8) yes N1 . P1 . C1 . 109.72(10) yes V1 . P1 . C7 . 121.52(8) yes Fe1 . P1 . C7 . 124.73(8) yes N1 . P1 . C7 . 102.12(10) yes C1 . P1 . C7 . 102.19(10) yes V1 . P2 . Fe1 . 49.563(17) yes V1 . P2 . N2 . 47.03(7) yes Fe1 . P2 . N2 . 96.44(7) yes V1 . P2 . C16 . 122.19(9) yes Fe1 . P2 . C16 . 120.49(8) yes N2 . P2 . C16 . 105.35(10) yes V1 . P2 . C22 . 133.29(8) yes Fe1 . P2 . C22 . 124.75(9) yes N2 . P2 . C22 . 107.37(10) yes C16 . P2 . C22 . 100.40(12) yes V1 . P3 . Fe1 . 49.307(16) yes V1 . P3 . N3 . 46.67(6) yes Fe1 . P3 . N3 . 95.35(7) yes V1 . P3 . C31 . 117.52(8) yes Fe1 . P3 . C31 . 121.26(7) yes N3 . P3 . C31 . 103.46(10) yes V1 . P3 . C37 . 134.61(8) yes Fe1 . P3 . C37 . 125.09(8) yes N3 . P3 . C37 . 105.80(10) yes C31 . P3 . C37 . 102.38(11) yes Fe1 . P4 . N4 . 113.17(7) yes Fe1 . P4 . C46 . 117.00(8) yes N4 . P4 . C46 . 103.01(10) yes Fe1 . P4 . C52 . 119.98(8) yes N4 . P4 . C52 . 102.09(10) yes C46 . P4 . C52 . 99.01(10) yes P1 . N1 . V1 . 92.85(9) yes P1 . N1 . C13 . 126.87(15) yes V1 . N1 . C13 . 139.06(15) yes P2 . N2 . V1 . 92.92(9) yes P2 . N2 . C28 . 128.77(16) yes V1 . N2 . C28 . 137.92(16) yes P3 . N3 . V1 . 93.23(8) yes P3 . N3 . C43 . 126.81(16) yes V1 . N3 . C43 . 139.25(16) yes P4 . N4 . C58 . 130.10(17) yes P4 . N4 . H4 . 113.9 no C58 . N4 . H4 . 115.4 no P1 . C1 . C2 . 124.61(18) yes P1 . C1 . C6 . 117.24(18) yes C2 . C1 . C6 . 118.1(2) yes C1 . C2 . C3 . 120.9(2) yes C1 . C2 . H21 . 119.9 no C3 . C2 . H21 . 119.3 no C2 . C3 . C4 . 119.8(2) yes C2 . C3 . H31 . 120.6 no C4 . C3 . H31 . 119.7 no C3 . C4 . C5 . 119.8(2) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 120.0 no C4 . C5 . C6 . 120.0(2) yes C4 . C5 . H51 . 119.8 no C6 . C5 . H51 . 120.2 no C1 . C6 . C5 . 121.4(2) yes C1 . C6 . H61 . 119.8 no C5 . C6 . H61 . 118.7 no P1 . C7 . C8 . 117.19(17) yes P1 . C7 . C12 . 124.79(19) yes C8 . C7 . C12 . 118.0(2) yes C7 . C8 . C9 . 121.7(2) yes C7 . C8 . H81 . 119.0 no C9 . C8 . H81 . 119.3 no C8 . C9 . C10 . 119.8(2) yes C8 . C9 . H91 . 119.6 no C10 . C9 . H91 . 120.6 no C9 . C10 . C11 . 119.7(2) yes C9 . C10 . H101 . 120.1 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 120.4(2) yes C10 . C11 . H111 . 120.4 no C12 . C11 . H111 . 119.1 no C11 . C12 . C7 . 120.4(2) yes C11 . C12 . H121 . 120.8 no C7 . C12 . H121 . 118.8 no N1 . C13 . C14 . 110.3(2) yes N1 . C13 . C15 . 111.7(2) yes C14 . C13 . C15 . 110.2(2) yes N1 . C13 . H131 . 107.5 no C14 . C13 . H131 . 108.6 no C15 . C13 . H131 . 108.4 no C13 . C14 . H141 . 109.9 no C13 . C14 . H142 . 108.3 no H141 . C14 . H142 . 108.6 no C13 . C14 . H143 . 109.9 no H141 . C14 . H143 . 110.4 no H142 . C14 . H143 . 109.6 no C13 . C15 . H151 . 111.4 no C13 . C15 . H152 . 109.6 no H151 . C15 . H152 . 109.1 no C13 . C15 . H153 . 109.3 no H151 . C15 . H153 . 108.1 no H152 . C15 . H153 . 109.3 no P2 . C16 . C17 . 118.6(2) yes P2 . C16 . C21 . 122.8(2) yes C17 . C16 . C21 . 118.3(2) yes C16 . C17 . C18 . 120.0(3) yes C16 . C17 . H171 . 119.6 no C18 . C17 . H171 . 120.3 no C17 . C18 . C19 . 120.3(3) yes C17 . C18 . H181 . 118.8 no C19 . C18 . H181 . 120.9 no C18 . C19 . C20 . 120.3(3) yes C18 . C19 . H191 . 121.4 no C20 . C19 . H191 . 118.3 no C19 . C20 . C21 . 120.3(3) yes C19 . C20 . H201 . 119.8 no C21 . C20 . H201 . 119.9 no C16 . C21 . C20 . 120.7(3) yes C16 . C21 . H211 . 120.1 no C20 . C21 . H211 . 119.1 no P2 . C22 . C23 . 122.4(2) yes P2 . C22 . C27 . 119.04(19) yes C23 . C22 . C27 . 118.3(2) yes C22 . C23 . C24 . 120.2(3) yes C22 . C23 . H231 . 120.3 no C24 . C23 . H231 . 119.5 no C23 . C24 . C25 . 120.4(3) yes C23 . C24 . H241 . 118.6 no C25 . C24 . H241 . 120.9 no C24 . C25 . C26 . 120.1(3) yes C24 . C25 . H251 . 120.6 no C26 . C25 . H251 . 119.4 no C25 . C26 . C27 . 119.8(3) yes C25 . C26 . H261 . 120.9 no C27 . C26 . H261 . 119.3 no C26 . C27 . C22 . 121.2(3) yes C26 . C27 . H271 . 119.9 no C22 . C27 . H271 . 118.9 no N2 . C28 . C29 . 109.5(2) yes N2 . C28 . C30 . 110.9(2) yes C29 . C28 . C30 . 110.1(2) yes N2 . C28 . H281 . 108.5 no C29 . C28 . H281 . 108.9 no C30 . C28 . H281 . 109.0 no C28 . C29 . H291 . 110.4 no C28 . C29 . H292 . 109.9 no H291 . C29 . H292 . 108.1 no C28 . C29 . H293 . 110.6 no H291 . C29 . H293 . 109.5 no H292 . C29 . H293 . 108.3 no C28 . C30 . H301 . 111.0 no C28 . C30 . H302 . 110.7 no H301 . C30 . H302 . 106.7 no C28 . C30 . H303 . 111.9 no H301 . C30 . H303 . 108.6 no H302 . C30 . H303 . 107.6 no P3 . C31 . C32 . 116.62(18) yes P3 . C31 . C36 . 125.55(19) yes C32 . C31 . C36 . 117.6(2) yes C31 . C32 . C33 . 121.6(2) yes C31 . C32 . H321 . 118.3 no C33 . C32 . H321 . 120.1 no C32 . C33 . C34 . 120.2(3) yes C32 . C33 . H331 . 119.5 no C34 . C33 . H331 . 120.2 no C33 . C34 . C35 . 119.6(3) yes C33 . C34 . H341 . 121.0 no C35 . C34 . H341 . 119.3 no C34 . C35 . C36 . 120.4(3) yes C34 . C35 . H351 . 121.2 no C36 . C35 . H351 . 118.4 no C35 . C36 . C31 . 120.5(3) yes C35 . C36 . H361 . 120.6 no C31 . C36 . H361 . 118.9 no P3 . C37 . C38 . 124.54(19) yes P3 . C37 . C42 . 117.05(17) yes C38 . C37 . C42 . 118.0(2) yes C37 . C38 . C39 . 120.5(3) yes C37 . C38 . H381 . 119.5 no C39 . C38 . H381 . 119.9 no C38 . C39 . C40 . 120.5(2) yes C38 . C39 . H391 . 118.7 no C40 . C39 . H391 . 120.7 no C39 . C40 . C41 . 119.8(2) yes C39 . C40 . H401 . 120.9 no C41 . C40 . H401 . 119.2 no C40 . C41 . C42 . 119.7(3) yes C40 . C41 . H411 . 120.2 no C42 . C41 . H411 . 120.2 no C41 . C42 . C37 . 121.5(2) yes C41 . C42 . H421 . 119.3 no C37 . C42 . H421 . 119.2 no N3 . C43 . C44 . 110.20(19) yes N3 . C43 . C45 . 110.9(2) yes C44 . C43 . C45 . 110.8(2) yes N3 . C43 . H431 . 108.1 no C44 . C43 . H431 . 107.9 no C45 . C43 . H431 . 108.8 no C43 . C44 . H441 . 111.1 no C43 . C44 . H442 . 111.7 no H441 . C44 . H442 . 108.2 no C43 . C44 . H443 . 110.0 no H441 . C44 . H443 . 107.8 no H442 . C44 . H443 . 108.0 no C43 . C45 . H451 . 110.4 no C43 . C45 . H452 . 108.5 no H451 . C45 . H452 . 108.9 no C43 . C45 . H453 . 108.9 no H451 . C45 . H453 . 110.6 no H452 . C45 . H453 . 109.6 no P4 . C46 . C47 . 118.88(18) yes P4 . C46 . C51 . 122.94(18) yes C47 . C46 . C51 . 118.1(2) yes C46 . C47 . C48 . 120.8(2) yes C46 . C47 . H471 . 119.3 no C48 . C47 . H471 . 119.9 no C47 . C48 . C49 . 120.4(2) yes C47 . C48 . H481 . 117.8 no C49 . C48 . H481 . 121.8 no C48 . C49 . C50 . 119.6(2) yes C48 . C49 . H491 . 120.9 no C50 . C49 . H491 . 119.5 no C49 . C50 . C51 . 119.9(2) yes C49 . C50 . H501 . 120.3 no C51 . C50 . H501 . 119.8 no C50 . C51 . C46 . 121.2(2) yes C50 . C51 . H511 . 118.6 no C46 . C51 . H511 . 120.2 no P4 . C52 . C53 . 124.19(18) yes P4 . C52 . C57 . 118.18(17) yes C53 . C52 . C57 . 117.6(2) yes C52 . C53 . C54 . 120.9(2) yes C52 . C53 . H531 . 120.0 no C54 . C53 . H531 . 119.1 no C53 . C54 . C55 . 120.6(2) yes C53 . C54 . H541 . 120.1 no C55 . C54 . H541 . 119.3 no C54 . C55 . C56 . 119.0(2) yes C54 . C55 . H551 . 121.3 no C56 . C55 . H551 . 119.7 no C55 . C56 . C57 . 120.5(2) yes C55 . C56 . H561 . 119.7 no C57 . C56 . H561 . 119.9 no C52 . C57 . C56 . 121.4(2) yes C52 . C57 . H571 . 118.6 no C56 . C57 . H571 . 119.9 no N4 . C58 . C59 . 112.3(2) yes N4 . C58 . C60 . 109.3(2) yes C59 . C58 . C60 . 109.7(2) yes N4 . C58 . H581 . 108.3 no C59 . C58 . H581 . 108.4 no C60 . C58 . H581 . 108.8 no C58 . C59 . H591 . 108.5 no C58 . C59 . H592 . 108.8 no H591 . C59 . H592 . 108.1 no C58 . C59 . H593 . 110.9 no H591 . C59 . H593 . 110.3 no H592 . C59 . H593 . 110.1 no C58 . C60 . H601 . 108.4 no C58 . C60 . H602 . 108.7 no H601 . C60 . H602 . 109.2 no C58 . C60 . H603 . 110.8 no H601 . C60 . H603 . 108.9 no H602 . C60 . H603 . 110.9 no _iucr_refine_instructions_details_constraints ; # # Punched on 27/11/12 at 13:15:57 # #LIST 12 BLOCK SCALE X'S, U'S RIDE N ( 4,X'S) H ( 4,X'S) RIDE C ( 2,X'S) H ( 21,X'S) RIDE C ( 3,X'S) H ( 31,X'S) RIDE C ( 4,X'S) H ( 41,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 152,X'S) H ( 153,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) H ( 292,X'S) H ( 293,X'S) RIDE C ( 30,X'S) H ( 301,X'S) H ( 302,X'S) H ( 303,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 341,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) H ( 442,X'S) H ( 443,X'S) RIDE C ( 45,X'S) H ( 451,X'S) H ( 452,X'S) H ( 453,X'S) RIDE C ( 47,X'S) H ( 471,X'S) RIDE C ( 48,X'S) H ( 481,X'S) RIDE C ( 49,X'S) H ( 491,X'S) RIDE C ( 50,X'S) H ( 501,X'S) RIDE C ( 51,X'S) H ( 511,X'S) RIDE C ( 53,X'S) H ( 531,X'S) RIDE C ( 54,X'S) H ( 541,X'S) RIDE C ( 55,X'S) H ( 551,X'S) RIDE C ( 56,X'S) H ( 561,X'S) RIDE C ( 57,X'S) H ( 571,X'S) RIDE C ( 58,X'S) H ( 581,X'S) RIDE C ( 59,X'S) H ( 591,X'S) H ( 592,X'S) H ( 593,X'S) RIDE C ( 60,X'S) H ( 601,X'S) H ( 602,X'S) H ( 603,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 27/11/12 at 13:15:57 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; _database_code_depnum_ccdc_archive 'CCDC 938610' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_6 _audit_creation_date 2012-11-26 _audit_creation_method CRYSTALS_ver_14.43 _oxford_structure_analysis_title 'sk_739_0m in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.7611(3) _cell_length_b 22.0867(6) _cell_length_c 22.4678(7) _cell_angle_alpha 63.2680(10) _cell_angle_beta 80.585(2) _cell_angle_gamma 85.642(2) _cell_volume 4705.1(2) _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' 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' 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' V 0.3005 0.5294 10.2971 6.8657 7.3511 0.4385 2.0703 26.8938 2.0571 102.4780 1.2199 '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' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 '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 4 # Given Formula = C48 H57 F1 Fe1 I1 N3 O0.75 P3 V1 # Dc = 1.46 Fooo = 2112.00 Mu = 13.07 M = 2067.22 # Found Formula = C48 H57 F1 Fe1 I1 N3 O0.75 P3 V1 # Dc = 1.46 FOOO = 2112.00 Mu = 13.07 M = 2067.22 _chemical_formula_sum 'C48 H57 F1 Fe1 I1 N3 O0.75 P3 V1' _chemical_formula_moiety 'C48 H57 F1 Fe1 I1 N3 O0.75 P3 V1' _chemical_compound_source ? _chemical_formula_weight 1033.61 _cell_measurement_reflns_used 9566 _cell_measurement_theta_min 3 _cell_measurement_theta_max 29 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_min 0.140 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_max 0.220 _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.307 # Sheldrick geometric approximatio 0.80 0.83 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.83 _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Apex2 (Bruker AXS, 2006)' _computing_cell_refinement 'Apex2 (Bruker AXS, 2006)' _computing_data_reduction 'Apex2 (Bruker AXS, 2006)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _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 120 _diffrn_reflns_number 98637 _reflns_number_total 25039 _diffrn_reflns_av_R_equivalents 0.050 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 25039 # Theoretical number of reflections is about 50439 _diffrn_reflns_theta_min 2.486 _diffrn_reflns_theta_max 29.083 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.502 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -26 _reflns_limit_k_max 30 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -1.21 _refine_diff_density_max 1.50 # 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>-10.0\s(I) _refine_ls_number_reflns 25039 _refine_ls_number_restraints 0 _refine_ls_number_parameters 1057 _oxford_refine_ls_R_factor_ref 0.0538 _refine_ls_wR_factor_ref 0.0745 _refine_ls_goodness_of_fit_ref 1.0000 _refine_ls_shift/su_max 0.0088794 _refine_ls_shift/su_mean 0.0003557 # The values computed with all filters except I/sigma _oxford_reflns_number_all 25039 _refine_ls_R_factor_all 0.0538 _refine_ls_wR_factor_all 0.0745 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 19036 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_gt 0.0694 # 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 mixed #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^) + ( 0.02P)^2^ + 6.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached 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 _atom_site_attached_hydrogens Fe1 Fe 0.60729(3) 0.714255(15) 0.019686(16) 0.0130 1.0000 Uani . . . . . . Fe101 Fe 0.94047(3) 0.752835(15) 0.450424(16) 0.0130 1.0000 Uani . . . . . . V1 V 0.80714(4) 0.771411(18) -0.043563(19) 0.0140 1.0000 Uani . . . . . . V101 V 1.11846(4) 0.810282(18) 0.457251(19) 0.0135 1.0000 Uani . . . . . . I1 I 0.410029(16) 0.645971(8) 0.093577(8) 0.0214 1.0000 Uani . . . . . . I101 I 0.773110(16) 0.678374(9) 0.447417(9) 0.0258 1.0000 Uani . . . . . . P1 P 0.64632(6) 0.71083(3) -0.08304(3) 0.0146 1.0000 Uani . . . . . . P2 P 0.76951(6) 0.66422(3) 0.08153(3) 0.0159 1.0000 Uani . . . . . . P3 P 0.59945(6) 0.82799(3) -0.00353(3) 0.0146 1.0000 Uani . . . . . . P101 P 0.95827(6) 0.86125(3) 0.36115(3) 0.0155 1.0000 Uani . . . . . . P102 P 1.12274(6) 0.68993(3) 0.45248(3) 0.0168 1.0000 Uani . . . . . . P103 P 0.90504(6) 0.76631(3) 0.54818(3) 0.0146 1.0000 Uani . . . . . . F1 F 0.96288(13) 0.81071(7) -0.09126(7) 0.0227 1.0000 Uani . . . . . . F101 F 1.25373(14) 0.85772(7) 0.45949(7) 0.0240 1.0000 Uani . . . . . . O1 O 0.5016(4) 0.52188(19) 0.4194(2) 0.0322(9) 0.5000 Uiso . . . . . . O2 O 0.4835(3) 0.46560(16) 0.30490(16) 0.0775 1.0000 Uani . . . . . . N1 N 0.77849(19) 0.75420(9) -0.11758(10) 0.0164 1.0000 Uani . . . . . . N2 N 0.89206(19) 0.70845(9) 0.03038(10) 0.0178 1.0000 Uani . . . . . . N3 N 0.74234(19) 0.85476(9) -0.04330(10) 0.0156 1.0000 Uani . . . . . . N101 N 1.08224(19) 0.88877(9) 0.37589(10) 0.0172 1.0000 Uani . . . . . . N102 N 1.22989(19) 0.74002(10) 0.45154(10) 0.0176 1.0000 Uani . . . . . . N103 N 1.03729(19) 0.80184(10) 0.54438(10) 0.0170 1.0000 Uani . . . . . . C1 C 0.8428(2) 0.76890(12) -0.18618(12) 0.0216 1.0000 Uani . . . . . . C2 C 0.9836(3) 0.75504(16) -0.18937(15) 0.0356 1.0000 Uani . . . . . . C3 C 0.8159(3) 0.84134(13) -0.23551(14) 0.0371 1.0000 Uani . . . . . . C4 C 0.6780(2) 0.62792(11) -0.08147(11) 0.0159 1.0000 Uani . . . . . . C5 C 0.7984(2) 0.60106(12) -0.07564(12) 0.0209 1.0000 Uani . . . . . . C6 C 0.8244(3) 0.53690(12) -0.07187(12) 0.0236 1.0000 Uani . . . . . . C7 C 0.7292(3) 0.49959(12) -0.07376(13) 0.0264 1.0000 Uani . . . . . . C8 C 0.6086(3) 0.52525(12) -0.07864(13) 0.0274 1.0000 Uani . . . . . . C9 C 0.5823(3) 0.58918(12) -0.08248(13) 0.0221 1.0000 Uani . . . . . . C10 C 0.5206(2) 0.74317(11) -0.13563(12) 0.0176 1.0000 Uani . . . . . . C11 C 0.5350(3) 0.74721(14) -0.20028(13) 0.0272 1.0000 Uani . . . . . . C12 C 0.4378(3) 0.77017(15) -0.23819(14) 0.0311 1.0000 Uani . . . . . . C13 C 0.3236(3) 0.78805(13) -0.21194(13) 0.0261 1.0000 Uani . . . . . . C14 C 0.3075(2) 0.78392(12) -0.14798(13) 0.0231 1.0000 Uani . . . . . . C15 C 0.4052(2) 0.76144(11) -0.10967(12) 0.0189 1.0000 Uani . . . . . . C16 C 1.0258(2) 0.69319(12) 0.04069(13) 0.0239 1.0000 Uani . . . . . . C17 C 1.0963(3) 0.75544(13) 0.03010(15) 0.0297 1.0000 Uani . . . . . . C18 C 1.0895(3) 0.66248(13) -0.00511(15) 0.0301 1.0000 Uani . . . . . . C19 C 0.7498(2) 0.67145(11) 0.15982(12) 0.0188 1.0000 Uani . . . . . . C20 C 0.8117(3) 0.72091(14) 0.16602(14) 0.0283 1.0000 Uani . . . . . . C21 C 0.7898(3) 0.72668(16) 0.22598(16) 0.0365 1.0000 Uani . . . . . . C22 C 0.7054(3) 0.68421(16) 0.27897(15) 0.0349 1.0000 Uani . . . . . . C23 C 0.6418(3) 0.63564(14) 0.27284(13) 0.0302 1.0000 Uani . . . . . . C24 C 0.6642(2) 0.62893(12) 0.21389(12) 0.0227 1.0000 Uani . . . . . . C25 C 0.7954(2) 0.57274(11) 0.11137(12) 0.0182 1.0000 Uani . . . . . . C26 C 0.8719(2) 0.53675(12) 0.16129(13) 0.0246 1.0000 Uani . . . . . . C27 C 0.8910(3) 0.46748(14) 0.18310(15) 0.0330 1.0000 Uani . . . . . . C28 C 0.8349(3) 0.43381(13) 0.15521(15) 0.0335 1.0000 Uani . . . . . . C29 C 0.7592(3) 0.46906(13) 0.10608(14) 0.0309 1.0000 Uani . . . . . . C30 C 0.7387(3) 0.53802(12) 0.08497(12) 0.0229 1.0000 Uani . . . . . . C31 C 0.7948(2) 0.92348(11) -0.06691(12) 0.0192 1.0000 Uani . . . . . . C32 C 0.8631(3) 0.95143(12) -0.13895(13) 0.0287 1.0000 Uani . . . . . . C33 C 0.8798(3) 0.92173(13) -0.01870(14) 0.0288 1.0000 Uani . . . . . . C34 C 0.4867(2) 0.87874(11) -0.05929(12) 0.0174 1.0000 Uani . . . . . . C35 C 0.5216(3) 0.90705(11) -0.12882(12) 0.0207 1.0000 Uani . . . . . . C36 C 0.4345(3) 0.94192(12) -0.17152(14) 0.0263 1.0000 Uani . . . . . . C37 C 0.3116(3) 0.94816(13) -0.14567(15) 0.0326 1.0000 Uani . . . . . . C38 C 0.2748(3) 0.91967(14) -0.07683(16) 0.0338 1.0000 Uani . . . . . . C39 C 0.3620(3) 0.88515(13) -0.03352(14) 0.0264 1.0000 Uani . . . . . . C40 C 0.5561(2) 0.84652(11) 0.06846(12) 0.0182 1.0000 Uani . . . . . . C41 C 0.5569(3) 0.91262(13) 0.06136(14) 0.0282 1.0000 Uani . . . . . . C42 C 0.5255(3) 0.92542(14) 0.11694(16) 0.0345 1.0000 Uani . . . . . . C43 C 0.4901(3) 0.87270(15) 0.18007(15) 0.0346 1.0000 Uani . . . . . . C44 C 0.4857(3) 0.80735(14) 0.18742(14) 0.0335 1.0000 Uani . . . . . . C45 C 0.5187(3) 0.79439(13) 0.13185(12) 0.0249 1.0000 Uani . . . . . . C46 C 0.5181(4) 0.45794(18) 0.24276(17) 0.0597 1.0000 Uani . . . . . . C47 C 0.5270(5) 0.3835(2) 0.2634(3) 0.0972 1.0000 Uani . . . . . . C48 C 0.5647(3) 0.35667(19) 0.3325(2) 0.0543 1.0000 Uani . . . . . . C49 C 0.4931(5) 0.3987(2) 0.3592(2) 0.0737 1.0000 Uani . . . . . . C51 C 0.5772(4) 0.5367(2) 0.45928(18) 0.0587 1.0000 Uani . . . . . . C101 C 1.1339(2) 0.95843(12) 0.33920(13) 0.0228 1.0000 Uani . . . . . . C102 C 1.2734(3) 0.95912(14) 0.31272(15) 0.0342 1.0000 Uani . . . . . . C103 C 1.1066(3) 0.99387(13) 0.38462(15) 0.0347 1.0000 Uani . . . . . . C104 C 0.9884(2) 0.87176(11) 0.27440(12) 0.0188 1.0000 Uani . . . . . . C105 C 1.1081(3) 0.85845(12) 0.24851(13) 0.0251 1.0000 Uani . . . . . . C106 C 1.1319(3) 0.86275(13) 0.18409(14) 0.0302 1.0000 Uani . . . . . . C107 C 1.0361(3) 0.88030(13) 0.14495(14) 0.0329 1.0000 Uani . . . . . . C108 C 0.9176(3) 0.89371(14) 0.16988(14) 0.0335 1.0000 Uani . . . . . . C109 C 0.8928(3) 0.88898(13) 0.23444(13) 0.0260 1.0000 Uani . . . . . . C110 C 0.8182(2) 0.91385(12) 0.35969(12) 0.0185 1.0000 Uani . . . . . . C111 C 0.8193(3) 0.98443(13) 0.32395(15) 0.0319 1.0000 Uani . . . . . . C112 C 0.7095(3) 1.02168(14) 0.32348(16) 0.0365 1.0000 Uani . . . . . . C113 C 0.5970(3) 0.98942(14) 0.35702(14) 0.0298 1.0000 Uani . . . . . . C114 C 0.5931(3) 0.92002(14) 0.39176(14) 0.0288 1.0000 Uani . . . . . . C115 C 0.7032(3) 0.88236(13) 0.39347(13) 0.0233 1.0000 Uani . . . . . . C116 C 1.3681(2) 0.72926(13) 0.44313(12) 0.0214 1.0000 Uani . . . . . . C117 C 1.4304(2) 0.74163(15) 0.49258(13) 0.0271 1.0000 Uani . . . . . . C118 C 1.4251(3) 0.77353(15) 0.37060(14) 0.0319 1.0000 Uani . . . . . . C119 C 1.1278(2) 0.60883(12) 0.52711(12) 0.0204 1.0000 Uani . . . . . . C120 C 1.1853(2) 0.60372(13) 0.58020(13) 0.0249 1.0000 Uani . . . . . . C121 C 1.1829(3) 0.54289(14) 0.63823(14) 0.0324 1.0000 Uani . . . . . . C122 C 1.1219(3) 0.48697(14) 0.64463(14) 0.0339 1.0000 Uani . . . . . . C123 C 1.0617(3) 0.49163(14) 0.59291(15) 0.0357 1.0000 Uani . . . . . . C124 C 1.0656(3) 0.55196(13) 0.53431(14) 0.0310 1.0000 Uani . . . . . . C125 C 1.1607(2) 0.66603(13) 0.38370(13) 0.0223 1.0000 Uani . . . . . . C126 C 1.2580(3) 0.62034(17) 0.38371(17) 0.0378 1.0000 Uani . . . . . . C127 C 1.2879(3) 0.60404(19) 0.33048(18) 0.0455 1.0000 Uani . . . . . . C128 C 1.2211(3) 0.63288(16) 0.27667(16) 0.0378 1.0000 Uani . . . . . . C129 C 1.1222(3) 0.67623(14) 0.27671(14) 0.0353 1.0000 Uani . . . . . . C130 C 1.0920(3) 0.69272(12) 0.33038(12) 0.0250 1.0000 Uani . . . . . . C131 C 1.0756(2) 0.81118(13) 0.60025(13) 0.0228 1.0000 Uani . . . . . . C132 C 1.1320(3) 0.88086(15) 0.57664(16) 0.0340 1.0000 Uani . . . . . . C133 C 1.1662(3) 0.75511(14) 0.63614(14) 0.0288 1.0000 Uani . . . . . . C134 C 0.7732(2) 0.82092(12) 0.55460(12) 0.0185 1.0000 Uani . . . . . . C135 C 0.7905(3) 0.88892(12) 0.53633(14) 0.0249 1.0000 Uani . . . . . . C136 C 0.6878(3) 0.93090(14) 0.53714(15) 0.0323 1.0000 Uani . . . . . . C137 C 0.5674(3) 0.90538(14) 0.55553(14) 0.0292 1.0000 Uani . . . . . . C138 C 0.5485(3) 0.83774(14) 0.57279(13) 0.0255 1.0000 Uani . . . . . . C139 C 0.6507(2) 0.79564(12) 0.57291(12) 0.0211 1.0000 Uani . . . . . . C140 C 0.8692(2) 0.68878(11) 0.62642(11) 0.0172 1.0000 Uani . . . . . . C141 C 0.8397(3) 0.68964(13) 0.68883(13) 0.0263 1.0000 Uani . . . . . . C142 C 0.8154(3) 0.62989(14) 0.74728(14) 0.0352 1.0000 Uani . . . . . . C143 C 0.8188(3) 0.56859(13) 0.74454(13) 0.0272 1.0000 Uani . . . . . . C144 C 0.8450(2) 0.56700(12) 0.68330(13) 0.0236 1.0000 Uani . . . . . . C145 C 0.8706(2) 0.62678(12) 0.62461(12) 0.0215 1.0000 Uani . . . . . . C500 C 0.4290(8) 0.4660(4) 0.4686(4) 0.0528(19) 0.5000 Uiso . . . . . . C501 C 0.5131(7) 0.5225(3) 0.5206(4) 0.0437(16) 0.5000 Uiso . . . . . . H11 H 0.8080 0.7398 -0.2002 0.0245 1.0000 Uiso R . . . . . H21 H 1.0008 0.7102 -0.1571 0.0534 1.0000 Uiso R . . . . . H22 H 1.0246 0.7864 -0.1799 0.0520 1.0000 Uiso R . . . . . H23 H 1.0182 0.7612 -0.2333 0.0528 1.0000 Uiso R . . . . . H31 H 0.7263 0.8503 -0.2335 0.0561 1.0000 Uiso R . . . . . H32 H 0.8543 0.8725 -0.2251 0.0553 1.0000 Uiso R . . . . . H33 H 0.8508 0.8499 -0.2811 0.0560 1.0000 Uiso R . . . . . H51 H 0.8623 0.6264 -0.0739 0.0248 1.0000 Uiso R . . . . . H61 H 0.9055 0.5193 -0.0677 0.0275 1.0000 Uiso R . . . . . H71 H 0.7443 0.4567 -0.0710 0.0326 1.0000 Uiso R . . . . . H81 H 0.5460 0.4994 -0.0800 0.0330 1.0000 Uiso R . . . . . H91 H 0.5016 0.6064 -0.0856 0.0265 1.0000 Uiso R . . . . . H111 H 0.6099 0.7337 -0.2171 0.0328 1.0000 Uiso R . . . . . H121 H 0.4478 0.7735 -0.2811 0.0371 1.0000 Uiso R . . . . . H131 H 0.2575 0.8022 -0.2366 0.0302 1.0000 Uiso R . . . . . H141 H 0.2317 0.7963 -0.1295 0.0281 1.0000 Uiso R . . . . . H151 H 0.3933 0.7589 -0.0671 0.0233 1.0000 Uiso R . . . . . H161 H 1.0276 0.6594 0.0869 0.0285 1.0000 Uiso R . . . . . H171 H 1.0553 0.7738 0.0590 0.0442 1.0000 Uiso R . . . . . H172 H 1.1800 0.7427 0.0395 0.0444 1.0000 Uiso R . . . . . H173 H 1.0991 0.7890 -0.0167 0.0431 1.0000 Uiso R . . . . . H181 H 1.0866 0.6941 -0.0514 0.0445 1.0000 Uiso R . . . . . H182 H 1.1759 0.6526 0.0021 0.0449 1.0000 Uiso R . . . . . H183 H 1.0494 0.6212 0.0054 0.0446 1.0000 Uiso R . . . . . H201 H 0.8677 0.7503 0.1295 0.0336 1.0000 Uiso R . . . . . H211 H 0.8308 0.7597 0.2302 0.0445 1.0000 Uiso R . . . . . H221 H 0.6910 0.6880 0.3192 0.0425 1.0000 Uiso R . . . . . H231 H 0.5850 0.6074 0.3084 0.0354 1.0000 Uiso R . . . . . H241 H 0.6225 0.5957 0.2101 0.0268 1.0000 Uiso R . . . . . H261 H 0.9094 0.5590 0.1802 0.0306 1.0000 Uiso R . . . . . H271 H 0.9418 0.4439 0.2170 0.0405 1.0000 Uiso R . . . . . H281 H 0.8489 0.3873 0.1704 0.0394 1.0000 Uiso R . . . . . H291 H 0.7212 0.4470 0.0873 0.0378 1.0000 Uiso R . . . . . H301 H 0.6854 0.5611 0.0534 0.0258 1.0000 Uiso R . . . . . H311 H 0.7244 0.9539 -0.0667 0.0225 1.0000 Uiso R . . . . . H321 H 0.9334 0.9231 -0.1422 0.0426 1.0000 Uiso R . . . . . H322 H 0.8929 0.9962 -0.1535 0.0424 1.0000 Uiso R . . . . . H323 H 0.8087 0.9535 -0.1697 0.0428 1.0000 Uiso R . . . . . H331 H 0.8358 0.9050 0.0267 0.0423 1.0000 Uiso R . . . . . H332 H 0.9504 0.8918 -0.0187 0.0427 1.0000 Uiso R . . . . . H333 H 0.9119 0.9666 -0.0324 0.0426 1.0000 Uiso R . . . . . H351 H 0.6051 0.9021 -0.1461 0.0244 1.0000 Uiso R . . . . . H361 H 0.4596 0.9617 -0.2178 0.0319 1.0000 Uiso R . . . . . H371 H 0.2532 0.9710 -0.1745 0.0390 1.0000 Uiso R . . . . . H381 H 0.1924 0.9242 -0.0595 0.0408 1.0000 Uiso R . . . . . H391 H 0.3375 0.8660 0.0130 0.0318 1.0000 Uiso R . . . . . H411 H 0.5788 0.9488 0.0188 0.0341 1.0000 Uiso R . . . . . H421 H 0.5279 0.9691 0.1118 0.0412 1.0000 Uiso R . . . . . H431 H 0.4679 0.8817 0.2176 0.0419 1.0000 Uiso R . . . . . H441 H 0.4641 0.7718 0.2300 0.0393 1.0000 Uiso R . . . . . H451 H 0.5158 0.7502 0.1380 0.0298 1.0000 Uiso R . . . . . H461 H 0.5982 0.4799 0.2200 0.0715 1.0000 Uiso R . . . . . H462 H 0.4542 0.4782 0.2135 0.0725 1.0000 Uiso R . . . . . H471 H 0.5882 0.3722 0.2344 0.1175 1.0000 Uiso R . . . . . H472 H 0.4471 0.3656 0.2668 0.1162 1.0000 Uiso R . . . . . H481 H 0.6415 0.3713 0.3280 0.0653 1.0000 Uiso R . . . . . H482 H 0.5519 0.3141 0.3547 0.0658 1.0000 Uiso R . . . . . H491 H 0.5366 0.4010 0.3935 0.0900 1.0000 Uiso R . . . . . H492 H 0.4074 0.3790 0.3789 0.0899 1.0000 Uiso R . . . . . H511 H 0.5997 0.5832 0.4346 0.0705 0.5000 Uiso R . . . . . H512 H 0.6510 0.5094 0.4631 0.0705 0.5000 Uiso R . . . . . H1011 H 1.0892 0.9821 0.3009 0.0269 1.0000 Uiso R . . . . . H1021 H 1.3191 0.9356 0.3495 0.0501 1.0000 Uiso R . . . . . H1022 H 1.3033 1.0053 0.2876 0.0502 1.0000 Uiso R . . . . . H1023 H 1.2888 0.9369 0.2834 0.0510 1.0000 Uiso R . . . . . H1031 H 1.1479 0.9704 0.4233 0.0517 1.0000 Uiso R . . . . . H1032 H 1.1389 1.0392 0.3603 0.0509 1.0000 Uiso R . . . . . H1033 H 1.0163 0.9943 0.3987 0.0512 1.0000 Uiso R . . . . . H1051 H 1.1737 0.8460 0.2751 0.0291 1.0000 Uiso R . . . . . H1061 H 1.2134 0.8536 0.1677 0.0363 1.0000 Uiso R . . . . . H1071 H 1.0529 0.8828 0.1021 0.0391 1.0000 Uiso R . . . . . H1081 H 0.8525 0.9063 0.1438 0.0396 1.0000 Uiso R . . . . . H1091 H 0.8112 0.8972 0.2513 0.0316 1.0000 Uiso R . . . . . H1111 H 0.8931 1.0058 0.3001 0.0384 1.0000 Uiso R . . . . . H1121 H 0.7127 1.0687 0.2994 0.0439 1.0000 Uiso R . . . . . H1131 H 0.5231 1.0145 0.3564 0.0359 1.0000 Uiso R . . . . . H1141 H 0.5177 0.8986 0.4151 0.0352 1.0000 Uiso R . . . . . H1151 H 0.7012 0.8345 0.4177 0.0272 1.0000 Uiso R . . . . . H1161 H 1.3835 0.6811 0.4533 0.0257 1.0000 Uiso R . . . . . H1171 H 1.4213 0.7886 0.4839 0.0401 1.0000 Uiso R . . . . . H1172 H 1.5186 0.7314 0.4873 0.0402 1.0000 Uiso R . . . . . H1173 H 1.3916 0.7135 0.5386 0.0414 1.0000 Uiso R . . . . . H1181 H 1.4134 0.8210 0.3598 0.0473 1.0000 Uiso R . . . . . H1182 H 1.5138 0.7643 0.3637 0.0474 1.0000 Uiso R . . . . . H1183 H 1.3858 0.7643 0.3397 0.0474 1.0000 Uiso R . . . . . H1201 H 1.2233 0.6417 0.5771 0.0295 1.0000 Uiso R . . . . . H1211 H 1.2227 0.5404 0.6731 0.0389 1.0000 Uiso R . . . . . H1221 H 1.1223 0.4457 0.6846 0.0409 1.0000 Uiso R . . . . . H1231 H 1.0200 0.4533 0.5976 0.0432 1.0000 Uiso R . . . . . H1241 H 1.0250 0.5550 0.4992 0.0364 1.0000 Uiso R . . . . . H1261 H 1.3034 0.6009 0.4195 0.0456 1.0000 Uiso R . . . . . H1271 H 1.3557 0.5738 0.3308 0.0554 1.0000 Uiso R . . . . . H1281 H 1.2430 0.6222 0.2402 0.0452 1.0000 Uiso R . . . . . H1291 H 1.0751 0.6941 0.2420 0.0419 1.0000 Uiso R . . . . . H1301 H 1.0242 0.7221 0.3308 0.0300 1.0000 Uiso R . . . . . H1311 H 0.9996 0.8071 0.6318 0.0266 1.0000 Uiso R . . . . . H1321 H 1.2109 0.8871 0.5469 0.0503 1.0000 Uiso R . . . . . H1322 H 1.0747 0.9158 0.5527 0.0509 1.0000 Uiso R . . . . . H1323 H 1.1466 0.8860 0.6152 0.0502 1.0000 Uiso R . . . . . H1331 H 1.1288 0.7108 0.6536 0.0419 1.0000 Uiso R . . . . . H1332 H 1.2425 0.7576 0.6052 0.0421 1.0000 Uiso R . . . . . H1333 H 1.1889 0.7601 0.6735 0.0430 1.0000 Uiso R . . . . . H1351 H 0.8711 0.9069 0.5229 0.0292 1.0000 Uiso R . . . . . H1361 H 0.7012 0.9766 0.5248 0.0385 1.0000 Uiso R . . . . . H1371 H 0.4995 0.9335 0.5556 0.0345 1.0000 Uiso R . . . . . H1381 H 0.4666 0.8205 0.5852 0.0308 1.0000 Uiso R . . . . . H1391 H 0.6372 0.7505 0.5845 0.0253 1.0000 Uiso R . . . . . H1411 H 0.8341 0.7308 0.6911 0.0315 1.0000 Uiso R . . . . . H1421 H 0.7964 0.6316 0.7883 0.0425 1.0000 Uiso R . . . . . H1431 H 0.8039 0.5283 0.7841 0.0328 1.0000 Uiso R . . . . . H1441 H 0.8454 0.5265 0.6806 0.0278 1.0000 Uiso R . . . . . H1451 H 0.8881 0.6255 0.5834 0.0260 1.0000 Uiso R . . . . . H5001 H 0.4788 0.4279 0.4705 0.0728 0.5000 Uiso R . . . . . H5002 H 0.3490 0.4631 0.4573 0.0728 0.5000 Uiso R . . . . . H5011 H 0.5750 0.5082 0.5500 0.0728 0.5000 Uiso R . . . . . H5012 H 0.4718 0.5619 0.5209 0.0728 0.5000 Uiso R . . . . . H513 H 0.5478 0.5788 0.4271 0.0711 0.5000 Uiso . . . . . . H514 H 0.6604 0.5285 0.4413 0.0711 0.5000 Uiso . . . . . . 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 Fe1 0.01541(17) 0.01173(14) 0.01198(15) -0.00558(12) -0.00148(12) -0.00061(12) Fe101 0.01420(17) 0.01327(14) 0.01176(15) -0.00551(12) -0.00315(12) 0.00045(12) V1 0.0156(2) 0.01196(17) 0.01388(18) -0.00525(14) -0.00134(15) -0.00115(14) V101 0.0136(2) 0.01414(17) 0.01228(18) -0.00505(14) -0.00276(15) -0.00017(14) I1 0.01961(9) 0.02200(8) 0.02051(8) -0.00839(6) 0.00202(6) -0.00592(6) I101 0.02035(9) 0.02945(9) 0.03447(10) -0.01862(7) -0.00742(7) -0.00346(7) P1 0.0172(3) 0.0144(3) 0.0132(3) -0.0071(2) -0.0012(2) -0.0010(2) P2 0.0174(3) 0.0135(3) 0.0151(3) -0.0046(2) -0.0028(2) -0.0009(2) P3 0.0187(3) 0.0119(2) 0.0137(3) -0.0061(2) -0.0027(2) 0.0003(2) P101 0.0177(3) 0.0136(3) 0.0136(3) -0.0038(2) -0.0047(2) 0.0001(2) P102 0.0167(3) 0.0190(3) 0.0176(3) -0.0103(2) -0.0050(2) 0.0033(2) P103 0.0158(3) 0.0161(3) 0.0131(3) -0.0075(2) -0.0021(2) -0.0004(2) F1 0.0195(8) 0.0222(7) 0.0229(7) -0.0079(6) 0.0009(6) -0.0035(6) F101 0.0208(8) 0.0236(7) 0.0266(8) -0.0081(6) -0.0078(6) -0.0041(6) O2 0.083(2) 0.085(2) 0.069(2) -0.0422(18) 0.0060(17) -0.0158(18) N1 0.0189(11) 0.0155(9) 0.0145(9) -0.0073(8) 0.0015(8) -0.0024(8) N2 0.0150(10) 0.0167(9) 0.0177(10) -0.0037(8) -0.0039(8) 0.0000(8) N3 0.0181(10) 0.0126(8) 0.0168(10) -0.0072(7) -0.0023(8) -0.0004(7) N101 0.0173(10) 0.0158(9) 0.0157(10) -0.0033(8) -0.0044(8) -0.0024(8) N102 0.0140(10) 0.0213(10) 0.0193(10) -0.0105(8) -0.0038(8) 0.0020(8) N103 0.0172(10) 0.0214(10) 0.0166(10) -0.0120(8) -0.0019(8) -0.0023(8) C1 0.0287(14) 0.0204(11) 0.0163(12) -0.0105(10) 0.0048(10) -0.0057(10) C2 0.0289(16) 0.0519(18) 0.0293(15) -0.0243(14) 0.0099(12) -0.0077(14) C3 0.063(2) 0.0209(13) 0.0186(13) -0.0050(11) 0.0083(14) -0.0039(13) C4 0.0212(13) 0.0137(10) 0.0128(11) -0.0071(8) 0.0011(9) -0.0004(9) C5 0.0232(13) 0.0177(11) 0.0203(12) -0.0072(9) -0.0017(10) -0.0027(9) C6 0.0293(15) 0.0201(12) 0.0193(12) -0.0083(10) -0.0014(11) 0.0041(10) C7 0.0431(17) 0.0143(11) 0.0206(13) -0.0073(10) -0.0025(12) 0.0002(11) C8 0.0379(17) 0.0179(12) 0.0274(14) -0.0101(11) -0.0044(12) -0.0062(11) C9 0.0233(14) 0.0184(11) 0.0235(13) -0.0081(10) -0.0027(10) -0.0021(10) C10 0.0227(13) 0.0131(10) 0.0163(11) -0.0054(9) -0.0037(10) -0.0009(9) C11 0.0238(14) 0.0385(15) 0.0210(13) -0.0155(12) -0.0022(11) 0.0037(11) C12 0.0345(17) 0.0431(16) 0.0178(13) -0.0146(12) -0.0069(12) 0.0017(13) C13 0.0277(15) 0.0232(12) 0.0248(13) -0.0058(10) -0.0110(11) -0.0010(11) C14 0.0206(13) 0.0223(12) 0.0276(14) -0.0127(10) -0.0012(11) -0.0009(10) C15 0.0240(13) 0.0180(11) 0.0171(11) -0.0097(9) -0.0025(10) -0.0020(9) C16 0.0180(13) 0.0221(12) 0.0255(13) -0.0039(10) -0.0071(10) 0.0003(10) C17 0.0182(14) 0.0304(14) 0.0392(16) -0.0127(12) -0.0084(12) -0.0021(11) C18 0.0193(14) 0.0246(13) 0.0406(16) -0.0108(12) -0.0009(12) 0.0021(10) C19 0.0209(13) 0.0170(11) 0.0184(12) -0.0064(9) -0.0084(10) 0.0038(9) C20 0.0286(15) 0.0302(14) 0.0289(14) -0.0145(12) -0.0068(12) -0.0024(11) C21 0.0410(19) 0.0430(17) 0.0395(17) -0.0272(14) -0.0151(14) -0.0017(14) C22 0.0417(19) 0.0478(17) 0.0256(15) -0.0234(13) -0.0153(13) 0.0091(14) C23 0.0357(17) 0.0332(14) 0.0151(12) -0.0051(11) -0.0040(11) 0.0019(12) C24 0.0255(14) 0.0229(12) 0.0183(12) -0.0072(10) -0.0057(10) 0.0010(10) C25 0.0172(12) 0.0163(10) 0.0163(11) -0.0042(9) 0.0007(9) 0.0006(9) C26 0.0226(14) 0.0220(12) 0.0247(13) -0.0062(10) -0.0047(11) 0.0015(10) C27 0.0287(16) 0.0264(13) 0.0317(15) -0.0032(12) -0.0051(12) 0.0075(11) C28 0.0382(18) 0.0169(12) 0.0368(16) -0.0083(11) 0.0043(13) 0.0050(11) C29 0.0426(18) 0.0223(13) 0.0275(14) -0.0133(11) 0.0041(13) -0.0034(12) C30 0.0287(15) 0.0193(11) 0.0183(12) -0.0074(10) -0.0003(10) 0.0002(10) C31 0.0247(13) 0.0125(10) 0.0209(12) -0.0074(9) -0.0036(10) -0.0020(9) C32 0.0402(17) 0.0172(11) 0.0237(13) -0.0053(10) 0.0023(12) -0.0107(11) C33 0.0330(16) 0.0266(13) 0.0301(15) -0.0139(11) -0.0056(12) -0.0086(11) C34 0.0205(13) 0.0136(10) 0.0201(12) -0.0082(9) -0.0056(10) -0.0016(9) C35 0.0248(14) 0.0186(11) 0.0216(12) -0.0106(10) -0.0065(10) 0.0010(10) C36 0.0338(16) 0.0219(12) 0.0240(13) -0.0083(10) -0.0121(12) 0.0007(11) C37 0.0303(16) 0.0240(13) 0.0401(17) -0.0065(12) -0.0220(13) 0.0047(11) C38 0.0207(15) 0.0338(15) 0.0419(17) -0.0111(13) -0.0095(13) 0.0023(11) C39 0.0231(14) 0.0254(13) 0.0244(13) -0.0058(11) -0.0010(11) -0.0028(10) C40 0.0201(13) 0.0184(11) 0.0190(12) -0.0105(9) -0.0048(10) 0.0023(9) C41 0.0368(17) 0.0215(12) 0.0273(14) -0.0138(11) 0.0035(12) -0.0029(11) C42 0.0425(18) 0.0286(14) 0.0421(17) -0.0264(13) 0.0019(14) -0.0023(13) C43 0.0429(19) 0.0446(17) 0.0293(15) -0.0291(14) -0.0052(13) 0.0091(14) C44 0.049(2) 0.0318(14) 0.0182(13) -0.0117(11) -0.0051(13) 0.0112(13) C45 0.0362(16) 0.0212(12) 0.0186(12) -0.0113(10) -0.0030(11) 0.0056(11) C46 0.094(3) 0.052(2) 0.0316(18) -0.0169(16) 0.0067(19) -0.037(2) C47 0.124(4) 0.072(3) 0.107(4) -0.070(3) 0.075(3) -0.067(3) C48 0.035(2) 0.052(2) 0.070(3) -0.0223(19) -0.0124(19) 0.0163(16) C49 0.099(4) 0.073(3) 0.053(3) -0.029(2) -0.027(3) 0.014(3) C51 0.060(3) 0.066(2) 0.040(2) -0.0094(18) -0.0138(18) -0.025(2) C101 0.0260(14) 0.0153(11) 0.0212(12) -0.0009(9) -0.0068(10) -0.0064(10) C102 0.0231(15) 0.0290(14) 0.0339(16) 0.0012(12) -0.0030(12) -0.0080(11) C103 0.054(2) 0.0180(12) 0.0311(15) -0.0066(11) -0.0138(14) -0.0060(12) C104 0.0260(14) 0.0124(10) 0.0165(11) -0.0044(9) -0.0052(10) -0.0007(9) C105 0.0305(15) 0.0213(12) 0.0207(13) -0.0074(10) -0.0033(11) 0.0024(10) C106 0.0377(17) 0.0257(13) 0.0257(14) -0.0128(11) 0.0045(12) -0.0016(12) C107 0.056(2) 0.0243(13) 0.0196(13) -0.0113(11) -0.0011(13) -0.0062(13) C108 0.048(2) 0.0347(15) 0.0210(14) -0.0118(12) -0.0136(13) -0.0022(13) C109 0.0314(15) 0.0276(13) 0.0201(13) -0.0102(11) -0.0073(11) -0.0014(11) C110 0.0212(13) 0.0191(11) 0.0168(11) -0.0077(9) -0.0094(10) 0.0036(9) C111 0.0279(15) 0.0198(12) 0.0427(17) -0.0068(11) -0.0130(13) 0.0008(10) C112 0.0424(19) 0.0188(12) 0.0511(19) -0.0148(13) -0.0207(15) 0.0086(12) C113 0.0302(16) 0.0371(15) 0.0327(15) -0.0237(13) -0.0153(13) 0.0151(12) C114 0.0254(15) 0.0364(15) 0.0233(13) -0.0119(12) -0.0067(11) 0.0056(12) C115 0.0257(14) 0.0228(12) 0.0198(12) -0.0075(10) -0.0066(10) 0.0034(10) C116 0.0164(13) 0.0295(13) 0.0196(12) -0.0131(10) -0.0014(10) 0.0045(10) C117 0.0145(13) 0.0431(15) 0.0248(14) -0.0154(12) -0.0059(11) 0.0021(11) C118 0.0199(14) 0.0491(17) 0.0245(14) -0.0162(13) 0.0021(11) 0.0004(12) C119 0.0219(13) 0.0208(11) 0.0196(12) -0.0100(10) -0.0054(10) 0.0052(10) C120 0.0205(14) 0.0308(13) 0.0256(13) -0.0141(11) -0.0052(11) 0.0027(11) C121 0.0306(16) 0.0381(15) 0.0231(14) -0.0075(12) -0.0099(12) 0.0036(12) C122 0.0387(18) 0.0271(14) 0.0265(15) -0.0037(11) -0.0092(13) 0.0091(12) C123 0.052(2) 0.0207(13) 0.0330(16) -0.0090(12) -0.0116(14) 0.0017(13) C124 0.0445(18) 0.0214(12) 0.0287(15) -0.0096(11) -0.0155(13) 0.0027(12) C125 0.0213(13) 0.0265(12) 0.0245(13) -0.0166(11) -0.0028(10) 0.0017(10) C126 0.0271(16) 0.059(2) 0.0472(19) -0.0400(17) -0.0155(14) 0.0156(14) C127 0.0295(18) 0.071(2) 0.058(2) -0.050(2) -0.0072(16) 0.0149(16) C128 0.0416(19) 0.0486(18) 0.0331(16) -0.0306(15) 0.0092(14) -0.0060(14) C129 0.056(2) 0.0323(15) 0.0190(13) -0.0131(12) -0.0044(13) 0.0018(14) C130 0.0352(16) 0.0213(12) 0.0180(12) -0.0090(10) -0.0036(11) 0.0045(11) C131 0.0196(13) 0.0336(13) 0.0247(13) -0.0211(11) -0.0037(10) -0.0005(10) C132 0.0370(17) 0.0394(16) 0.0415(17) -0.0302(14) -0.0101(14) -0.0017(13) C133 0.0233(15) 0.0427(16) 0.0270(14) -0.0197(12) -0.0111(11) 0.0049(12) C134 0.0200(13) 0.0221(11) 0.0155(11) -0.0101(9) -0.0041(9) 0.0020(9) C135 0.0233(14) 0.0221(12) 0.0328(15) -0.0137(11) -0.0096(11) 0.0014(10) C136 0.0356(17) 0.0251(13) 0.0460(18) -0.0227(13) -0.0150(14) 0.0070(12) C137 0.0273(15) 0.0349(14) 0.0319(15) -0.0206(12) -0.0110(12) 0.0141(12) C138 0.0179(13) 0.0356(14) 0.0228(13) -0.0135(11) -0.0019(10) 0.0021(11) C139 0.0212(13) 0.0223(12) 0.0193(12) -0.0088(10) -0.0025(10) -0.0002(10) C140 0.0165(12) 0.0189(11) 0.0142(11) -0.0052(9) -0.0037(9) 0.0009(9) C141 0.0392(17) 0.0215(12) 0.0186(12) -0.0103(10) -0.0023(11) 0.0024(11) C142 0.058(2) 0.0299(14) 0.0146(13) -0.0089(11) -0.0015(13) 0.0037(13) C143 0.0312(16) 0.0242(12) 0.0179(12) -0.0023(10) -0.0038(11) 0.0015(11) C144 0.0242(14) 0.0192(11) 0.0252(13) -0.0088(10) -0.0005(11) -0.0012(10) C145 0.0240(14) 0.0238(12) 0.0168(12) -0.0102(10) 0.0007(10) -0.0016(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.080345(6) 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 Fe1 . V1 . 2.4571(5) yes Fe1 . I1 . 2.5725(4) yes Fe1 . P1 . 2.3118(7) yes Fe1 . P2 . 2.3061(7) yes Fe1 . P3 . 2.3222(6) yes Fe101 . V101 . 2.4377(5) yes Fe101 . I101 . 2.5579(4) yes Fe101 . P101 . 2.3274(6) yes Fe101 . P102 . 2.3103(7) yes Fe101 . P103 . 2.3141(7) yes V1 . P1 . 2.7375(7) yes V1 . P2 . 2.7304(7) yes V1 . P3 . 2.7009(7) yes V1 . F1 . 1.8727(14) yes V1 . N1 . 1.939(2) yes V1 . N2 . 1.937(2) yes V1 . N3 . 1.9205(19) yes V101 . P101 . 2.7636(7) yes V101 . P102 . 2.7048(7) yes V101 . P103 . 2.7222(7) yes V101 . F101 . 1.8768(14) yes V101 . N101 . 1.9438(19) yes V101 . N102 . 1.926(2) yes V101 . N103 . 1.941(2) yes P1 . N1 . 1.649(2) yes P1 . C4 . 1.823(2) yes P1 . C10 . 1.831(3) yes P2 . N2 . 1.644(2) yes P2 . C19 . 1.814(2) yes P2 . C25 . 1.835(2) yes P3 . N3 . 1.651(2) yes P3 . C34 . 1.823(2) yes P3 . C40 . 1.822(2) yes P101 . N101 . 1.646(2) yes P101 . C104 . 1.832(2) yes P101 . C110 . 1.827(3) yes P102 . N102 . 1.649(2) yes P102 . C119 . 1.826(2) yes P102 . C125 . 1.824(3) yes P103 . N103 . 1.649(2) yes P103 . C134 . 1.821(3) yes P103 . C140 . 1.828(2) yes O1 . H5011 2_666 1.040 no O1 . C501 2_666 1.252(8) yes O1 . C51 . 1.453(5) yes O1 . C500 . 1.411(8) yes O2 . C46 . 1.466(4) yes O2 . C49 . 1.441(5) yes N1 . C1 . 1.481(3) yes N2 . C16 . 1.485(3) yes N3 . C31 . 1.487(3) yes N101 . C101 . 1.481(3) yes N102 . C116 . 1.483(3) yes N103 . C131 . 1.485(3) yes C1 . C2 . 1.520(4) yes C1 . C3 . 1.520(3) yes C1 . H11 . 0.953 no C2 . H21 . 0.954 no C2 . H22 . 0.965 no C2 . H23 . 0.947 no C3 . H31 . 0.967 no C3 . H32 . 0.958 no C3 . H33 . 0.967 no C4 . C5 . 1.385(3) yes C4 . C9 . 1.397(3) yes C5 . C6 . 1.390(3) yes C5 . H51 . 0.935 no C6 . C7 . 1.380(4) yes C6 . H61 . 0.930 no C7 . C8 . 1.376(4) yes C7 . H71 . 0.925 no C8 . C9 . 1.385(3) yes C8 . H81 . 0.927 no C9 . H91 . 0.922 no C10 . C11 . 1.398(3) yes C10 . C15 . 1.394(3) yes C11 . C12 . 1.378(4) yes C11 . H111 . 0.921 no C12 . C13 . 1.383(4) yes C12 . H121 . 0.921 no C13 . C14 . 1.381(4) yes C13 . H131 . 0.922 no C14 . C15 . 1.388(4) yes C14 . H141 . 0.932 no C15 . H151 . 0.921 no C16 . C17 . 1.526(3) yes C16 . C18 . 1.521(4) yes C16 . H161 . 0.971 no C17 . H171 . 0.947 no C17 . H172 . 0.951 no C17 . H173 . 0.974 no C18 . H181 . 0.961 no C18 . H182 . 0.962 no C18 . H183 . 0.951 no C19 . C20 . 1.391(3) yes C19 . C24 . 1.395(3) yes C20 . C21 . 1.390(4) yes C20 . H201 . 0.936 no C21 . C22 . 1.376(4) yes C21 . H211 . 0.929 no C22 . C23 . 1.383(4) yes C22 . H221 . 0.932 no C23 . C24 . 1.379(4) yes C23 . H231 . 0.923 no C24 . H241 . 0.931 no C25 . C26 . 1.403(3) yes C25 . C30 . 1.382(3) yes C26 . C27 . 1.391(4) yes C26 . H261 . 0.927 no C27 . C28 . 1.387(4) yes C27 . H271 . 0.942 no C28 . C29 . 1.382(4) yes C28 . H281 . 0.934 no C29 . C30 . 1.388(3) yes C29 . H291 . 0.925 no C30 . H301 . 0.925 no C31 . C32 . 1.524(3) yes C31 . C33 . 1.514(4) yes C31 . H311 . 0.975 no C32 . H321 . 0.959 no C32 . H322 . 0.953 no C32 . H323 . 0.960 no C33 . H331 . 0.965 no C33 . H332 . 0.969 no C33 . H333 . 0.968 no C34 . C35 . 1.392(3) yes C34 . C39 . 1.396(4) yes C35 . C36 . 1.382(4) yes C35 . H351 . 0.938 no C36 . C37 . 1.378(4) yes C36 . H361 . 0.928 no C37 . C38 . 1.381(4) yes C37 . H371 . 0.927 no C38 . C39 . 1.390(4) yes C38 . H381 . 0.925 no C39 . H391 . 0.933 no C40 . C41 . 1.396(3) yes C40 . C45 . 1.387(3) yes C41 . C42 . 1.385(4) yes C41 . H411 . 0.936 no C42 . C43 . 1.385(4) yes C42 . H421 . 0.920 no C43 . C44 . 1.381(4) yes C43 . H431 . 0.942 no C44 . C45 . 1.389(4) yes C44 . H441 . 0.930 no C45 . H451 . 0.924 no C46 . C47 . 1.494(5) yes C46 . H461 . 0.967 no C46 . H462 . 0.970 no C47 . C48 . 1.506(7) yes C47 . H471 . 0.950 no C47 . H472 . 0.951 no C48 . C49 . 1.434(5) yes C48 . H481 . 0.885 no C48 . H482 . 0.852 no C49 . H491 . 0.986 no C49 . H492 . 0.995 no C51 . C501 2_666 1.541(8) yes C51 . C500 2_666 1.586(9) yes C51 . C501 . 1.344(8) yes C51 . H511 . 0.950 no C51 . H512 . 0.950 no C51 . H513 . 0.956 no C51 . H514 . 0.959 no C101 . C102 . 1.520(4) yes C101 . C103 . 1.525(4) yes C101 . H1011 . 0.969 no C102 . H1021 . 0.951 no C102 . H1022 . 0.967 no C102 . H1023 . 0.972 no C103 . H1031 . 0.954 no C103 . H1032 . 0.960 no C103 . H1033 . 0.972 no C104 . C105 . 1.390(4) yes C104 . C109 . 1.395(4) yes C105 . C106 . 1.389(4) yes C105 . H1051 . 0.945 no C106 . C107 . 1.385(4) yes C106 . H1061 . 0.938 no C107 . C108 . 1.373(4) yes C107 . H1071 . 0.928 no C108 . C109 . 1.388(4) yes C108 . H1081 . 0.933 no C109 . H1091 . 0.936 no C110 . C111 . 1.396(3) yes C110 . C115 . 1.393(4) yes C111 . C112 . 1.387(4) yes C111 . H1111 . 0.911 no C112 . C113 . 1.375(4) yes C112 . H1121 . 0.930 no C113 . C114 . 1.372(4) yes C113 . H1131 . 0.932 no C114 . C115 . 1.390(4) yes C114 . H1141 . 0.924 no C115 . H1151 . 0.946 no C116 . C117 . 1.518(4) yes C116 . C118 . 1.522(4) yes C116 . H1161 . 0.988 no C117 . H1171 . 0.966 no C117 . H1172 . 0.959 no C117 . H1173 . 0.974 no C118 . H1181 . 0.967 no C118 . H1182 . 0.963 no C118 . H1183 . 0.969 no C119 . C120 . 1.389(4) yes C119 . C124 . 1.400(4) yes C120 . C121 . 1.387(4) yes C120 . H1201 . 0.930 no C121 . C122 . 1.382(4) yes C121 . H1211 . 0.932 no C122 . C123 . 1.381(4) yes C122 . H1221 . 0.950 no C123 . C124 . 1.387(4) yes C123 . H1231 . 0.945 no C124 . H1241 . 0.938 no C125 . C126 . 1.398(4) yes C125 . C130 . 1.385(4) yes C126 . C127 . 1.381(4) yes C126 . H1261 . 0.926 no C127 . C128 . 1.381(5) yes C127 . H1271 . 0.950 no C128 . C129 . 1.376(4) yes C128 . H1281 . 0.940 no C129 . C130 . 1.393(4) yes C129 . H1291 . 0.918 no C130 . H1301 . 0.940 no C131 . C132 . 1.523(4) yes C131 . C133 . 1.520(4) yes C131 . H1311 . 0.972 no C132 . H1321 . 0.968 no C132 . H1322 . 0.963 no C132 . H1323 . 0.962 no C133 . H1331 . 0.967 no C133 . H1332 . 0.973 no C133 . H1333 . 0.966 no C134 . C135 . 1.386(3) yes C134 . C139 . 1.396(3) yes C135 . C136 . 1.391(4) yes C135 . H1351 . 0.927 no C136 . C137 . 1.376(4) yes C136 . H1361 . 0.934 no C137 . C138 . 1.387(4) yes C137 . H1371 . 0.923 no C138 . C139 . 1.384(4) yes C138 . H1381 . 0.935 no C139 . H1391 . 0.927 no C140 . C141 . 1.394(3) yes C140 . C145 . 1.387(3) yes C141 . C142 . 1.384(4) yes C141 . H1411 . 0.930 no C142 . C143 . 1.380(4) yes C142 . H1421 . 0.928 no C143 . C144 . 1.374(4) yes C143 . H1431 . 0.933 no C144 . C145 . 1.389(3) yes C144 . H1441 . 0.922 no C145 . H1451 . 0.926 no C500 . H5012 2_666 1.195 no C500 . C501 2_666 0.801(9) yes C500 . H5001 . 0.950 no C500 . H5002 . 0.950 no C501 . H5001 2_666 1.209 no C501 . C501 2_666 1.697(14) yes C501 . H5011 . 0.950 no C501 . H5012 . 0.950 no H511 . H513 . 0.636 no H512 . H514 . 0.482 no H5001 . H5012 2_666 0.678 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 V1 . Fe1 . I1 . 174.737(18) yes V1 . Fe1 . P1 . 69.99(2) yes I1 . Fe1 . P1 . 111.92(2) yes V1 . Fe1 . P2 . 69.87(2) yes I1 . Fe1 . P2 . 104.949(19) yes P1 . Fe1 . P2 . 110.87(3) yes V1 . Fe1 . P3 . 68.755(19) yes I1 . Fe1 . P3 . 114.56(2) yes P1 . Fe1 . P3 . 106.61(2) yes P2 . Fe1 . P3 . 107.91(2) yes V101 . Fe101 . I101 . 172.218(17) yes V101 . Fe101 . P101 . 70.85(2) yes I101 . Fe101 . P101 . 114.82(2) yes V101 . Fe101 . P102 . 69.40(2) yes I101 . Fe101 . P102 . 103.032(19) yes P101 . Fe101 . P102 . 112.37(3) yes V101 . Fe101 . P103 . 69.85(2) yes I101 . Fe101 . P103 . 112.04(2) yes P101 . Fe101 . P103 . 106.62(2) yes P102 . Fe101 . P103 . 107.87(3) yes Fe1 . V1 . P1 . 52.515(16) yes Fe1 . V1 . P2 . 52.466(17) yes P1 . V1 . P2 . 88.13(2) yes Fe1 . V1 . P3 . 53.260(16) yes P1 . V1 . P3 . 86.19(2) yes P2 . V1 . P3 . 87.10(2) yes Fe1 . V1 . F1 . 177.10(5) yes P1 . V1 . F1 . 126.32(5) yes P2 . V1 . F1 . 125.84(5) yes P3 . V1 . F1 . 129.63(5) yes Fe1 . V1 . N1 . 88.96(6) yes P1 . V1 . N1 . 36.50(6) yes P2 . V1 . N1 . 116.03(6) yes P3 . V1 . N1 . 109.78(6) yes F1 . V1 . N1 . 90.02(7) yes Fe1 . V1 . N2 . 88.96(6) yes P1 . V1 . N2 . 113.94(6) yes P2 . V1 . N2 . 36.50(6) yes P3 . V1 . N2 . 113.24(6) yes F1 . V1 . N2 . 89.35(7) yes Fe1 . V1 . N3 . 90.49(6) yes P1 . V1 . N3 . 113.20(6) yes P2 . V1 . N3 . 112.31(6) yes P3 . V1 . N3 . 37.26(6) yes F1 . V1 . N3 . 92.39(7) yes N1 . V1 . N2 . 123.73(8) yes N1 . V1 . N3 . 117.27(8) yes N2 . V1 . N3 . 118.98(9) yes Fe101 . V101 . P101 . 52.710(16) yes Fe101 . V101 . P102 . 53.082(17) yes P101 . V101 . P102 . 89.59(2) yes Fe101 . V101 . P103 . 52.943(17) yes P101 . V101 . P103 . 85.44(2) yes P102 . V101 . P103 . 87.07(2) yes Fe101 . V101 . F101 . 177.66(5) yes P101 . V101 . F101 . 124.96(5) yes P102 . V101 . F101 . 128.35(5) yes P103 . V101 . F101 . 127.92(5) yes Fe101 . V101 . N101 . 88.56(6) yes P101 . V101 . N101 . 35.85(6) yes P102 . V101 . N101 . 115.34(6) yes P103 . V101 . N101 . 110.45(6) yes F101 . V101 . N101 . 89.11(7) yes Fe101 . V101 . N102 . 90.09(6) yes P101 . V101 . N102 . 114.14(6) yes P102 . V101 . N102 . 37.13(6) yes P103 . V101 . N102 . 115.39(6) yes F101 . V101 . N102 . 91.26(8) yes Fe101 . V101 . N103 . 89.70(6) yes P101 . V101 . N103 . 112.50(6) yes P102 . V101 . N103 . 110.99(6) yes P103 . V101 . N103 . 36.82(6) yes F101 . V101 . N103 . 91.28(7) yes N101 . V101 . N102 . 120.39(9) yes N101 . V101 . N103 . 119.45(9) yes N102 . V101 . N103 . 120.14(8) yes V1 . P1 . Fe1 . 57.496(17) yes Fe1 . P1 . N1 . 101.80(7) yes V1 . P1 . C4 . 122.56(8) yes Fe1 . P1 . C4 . 117.01(8) yes N1 . P1 . C4 . 106.44(10) yes V1 . P1 . C10 . 133.24(7) yes Fe1 . P1 . C10 . 116.11(8) yes N1 . P1 . C10 . 113.54(10) yes C4 . P1 . C10 . 101.99(11) yes V1 . P2 . Fe1 . 57.664(18) yes Fe1 . P2 . N2 . 102.15(7) yes V1 . P2 . C19 . 124.42(8) yes Fe1 . P2 . C19 . 112.72(8) yes N2 . P2 . C19 . 110.32(11) yes V1 . P2 . C25 . 132.46(8) yes Fe1 . P2 . C25 . 118.48(8) yes N2 . P2 . C25 . 111.94(11) yes C19 . P2 . C25 . 101.44(11) yes V1 . P3 . Fe1 . 57.985(17) yes Fe1 . P3 . N3 . 102.72(7) yes V1 . P3 . C34 . 123.37(8) yes Fe1 . P3 . C34 . 114.79(7) yes N3 . P3 . C34 . 107.96(10) yes V1 . P3 . C40 . 132.24(8) yes Fe1 . P3 . C40 . 116.39(8) yes N3 . P3 . C40 . 112.52(11) yes C34 . P3 . C40 . 102.51(11) yes V101 . P101 . Fe101 . 56.437(17) yes Fe101 . P101 . N101 . 100.21(7) yes V101 . P101 . C104 . 128.20(9) yes Fe101 . P101 . C104 . 119.73(7) yes N101 . P101 . C104 . 108.15(11) yes V101 . P101 . C110 . 127.76(8) yes Fe101 . P101 . C110 . 113.73(8) yes N101 . P101 . C110 . 113.35(11) yes C104 . P101 . C110 . 102.02(11) yes V101 . P102 . Fe101 . 57.521(18) yes Fe101 . P102 . N102 . 102.19(7) yes V101 . P102 . C119 . 122.58(8) yes Fe101 . P102 . C119 . 116.06(8) yes N102 . P102 . C119 . 108.16(11) yes V101 . P102 . C125 . 132.88(8) yes Fe101 . P102 . C125 . 115.34(9) yes N102 . P102 . C125 . 112.46(11) yes C119 . P102 . C125 . 102.76(11) yes V101 . P103 . Fe101 . 57.210(17) yes Fe101 . P103 . N103 . 102.00(7) yes V101 . P103 . C134 . 124.27(8) yes Fe101 . P103 . C134 . 115.91(8) yes N103 . P103 . C134 . 109.06(11) yes V101 . P103 . C140 . 132.10(8) yes Fe101 . P103 . C140 . 115.70(8) yes N103 . P103 . C140 . 112.42(11) yes C134 . P103 . C140 . 101.97(11) yes H5011 2_666 O1 . C501 2_666 47.9 no H5011 2_666 O1 . C51 . 110.5 no C501 2_666 O1 . C51 . 69.0(4) yes C51 . O1 . C500 . 102.6(4) yes C46 . O2 . C49 . 105.7(3) yes V1 . N1 . P1 . 99.13(10) yes V1 . N1 . C1 . 137.25(16) yes P1 . N1 . C1 . 123.60(16) yes V1 . N2 . P2 . 99.00(10) yes V1 . N2 . C16 . 134.67(16) yes P2 . N2 . C16 . 125.90(16) yes P3 . N3 . V1 . 97.98(9) yes P3 . N3 . C31 . 126.92(16) yes V1 . N3 . C31 . 135.07(16) yes V101 . N101 . P101 . 100.37(9) yes V101 . N101 . C101 . 132.98(16) yes P101 . N101 . C101 . 126.20(16) yes P102 . N102 . V101 . 98.04(10) yes P102 . N102 . C116 . 125.72(16) yes V101 . N102 . C116 . 136.08(16) yes V101 . N103 . P103 . 98.32(10) yes V101 . N103 . C131 . 135.89(16) yes P103 . N103 . C131 . 125.17(16) yes N1 . C1 . C2 . 113.3(2) yes N1 . C1 . C3 . 110.3(2) yes C2 . C1 . C3 . 111.0(2) yes N1 . C1 . H11 . 107.9 no C2 . C1 . H11 . 107.0 no C3 . C1 . H11 . 107.0 no C1 . C2 . H21 . 111.1 no C1 . C2 . H22 . 110.2 no H21 . C2 . H22 . 108.0 no C1 . C2 . H23 . 109.6 no H21 . C2 . H23 . 110.0 no H22 . C2 . H23 . 107.8 no C1 . C3 . H31 . 111.1 no C1 . C3 . H32 . 110.0 no H31 . C3 . H32 . 108.6 no C1 . C3 . H33 . 110.7 no H31 . C3 . H33 . 108.8 no H32 . C3 . H33 . 107.5 no P1 . C4 . C5 . 119.28(18) yes P1 . C4 . C9 . 121.60(19) yes C5 . C4 . C9 . 119.0(2) yes C4 . C5 . C6 . 120.6(2) yes C4 . C5 . H51 . 119.3 no C6 . C5 . H51 . 120.1 no C5 . C6 . C7 . 119.7(3) yes C5 . C6 . H61 . 119.8 no C7 . C6 . H61 . 120.5 no C6 . C7 . C8 . 120.4(2) yes C6 . C7 . H71 . 121.1 no C8 . C7 . H71 . 118.5 no C7 . C8 . C9 . 120.1(2) yes C7 . C8 . H81 . 119.1 no C9 . C8 . H81 . 120.8 no C4 . C9 . C8 . 120.2(2) yes C4 . C9 . H91 . 119.6 no C8 . C9 . H91 . 120.3 no P1 . C10 . C11 . 121.8(2) yes P1 . C10 . C15 . 119.42(18) yes C11 . C10 . C15 . 118.8(2) yes C10 . C11 . C12 . 120.6(3) yes C10 . C11 . H111 . 119.2 no C12 . C11 . H111 . 120.2 no C11 . C12 . C13 . 120.2(3) yes C11 . C12 . H121 . 120.6 no C13 . C12 . H121 . 119.3 no C12 . C13 . C14 . 120.0(3) yes C12 . C13 . H131 . 120.5 no C14 . C13 . H131 . 119.5 no C13 . C14 . C15 . 120.2(2) yes C13 . C14 . H141 . 121.4 no C15 . C14 . H141 . 118.4 no C10 . C15 . C14 . 120.2(2) yes C10 . C15 . H151 . 120.4 no C14 . C15 . H151 . 119.4 no N2 . C16 . C17 . 112.2(2) yes N2 . C16 . C18 . 109.5(2) yes C17 . C16 . C18 . 111.6(2) yes N2 . C16 . H161 . 108.1 no C17 . C16 . H161 . 107.6 no C18 . C16 . H161 . 107.7 no C16 . C17 . H171 . 110.3 no C16 . C17 . H172 . 109.2 no H171 . C17 . H172 . 109.5 no C16 . C17 . H173 . 108.6 no H171 . C17 . H173 . 110.0 no H172 . C17 . H173 . 109.2 no C16 . C18 . H181 . 109.8 no C16 . C18 . H182 . 108.9 no H181 . C18 . H182 . 109.3 no C16 . C18 . H183 . 110.4 no H181 . C18 . H183 . 110.3 no H182 . C18 . H183 . 108.1 no P2 . C19 . C20 . 121.80(19) yes P2 . C19 . C24 . 118.92(18) yes C20 . C19 . C24 . 119.2(2) yes C19 . C20 . C21 . 120.0(3) yes C19 . C20 . H201 . 119.5 no C21 . C20 . H201 . 120.5 no C20 . C21 . C22 . 120.1(3) yes C20 . C21 . H211 . 120.2 no C22 . C21 . H211 . 119.6 no C21 . C22 . C23 . 120.2(3) yes C21 . C22 . H221 . 120.1 no C23 . C22 . H221 . 119.7 no C22 . C23 . C24 . 120.1(3) yes C22 . C23 . H231 . 119.9 no C24 . C23 . H231 . 120.0 no C19 . C24 . C23 . 120.4(2) yes C19 . C24 . H241 . 119.6 no C23 . C24 . H241 . 120.0 no P2 . C25 . C26 . 121.01(19) yes P2 . C25 . C30 . 120.15(19) yes C26 . C25 . C30 . 118.8(2) yes C25 . C26 . C27 . 120.3(3) yes C25 . C26 . H261 . 120.1 no C27 . C26 . H261 . 119.6 no C26 . C27 . C28 . 120.0(3) yes C26 . C27 . H271 . 119.3 no C28 . C27 . H271 . 120.7 no C27 . C28 . C29 . 119.9(2) yes C27 . C28 . H281 . 118.8 no C29 . C28 . H281 . 121.3 no C28 . C29 . C30 . 120.1(3) yes C28 . C29 . H291 . 120.6 no C30 . C29 . H291 . 119.3 no C29 . C30 . C25 . 120.8(3) yes C29 . C30 . H301 . 119.9 no C25 . C30 . H301 . 119.2 no N3 . C31 . C32 . 112.19(19) yes N3 . C31 . C33 . 109.62(19) yes C32 . C31 . C33 . 111.5(2) yes N3 . C31 . H311 . 107.7 no C32 . C31 . H311 . 107.0 no C33 . C31 . H311 . 108.6 no C31 . C32 . H321 . 110.6 no C31 . C32 . H322 . 110.6 no H321 . C32 . H322 . 108.7 no C31 . C32 . H323 . 111.6 no H321 . C32 . H323 . 107.5 no H322 . C32 . H323 . 107.7 no C31 . C33 . H331 . 111.4 no C31 . C33 . H332 . 109.2 no H331 . C33 . H332 . 108.1 no C31 . C33 . H333 . 110.5 no H331 . C33 . H333 . 108.8 no H332 . C33 . H333 . 108.6 no P3 . C34 . C35 . 120.04(19) yes P3 . C34 . C39 . 120.90(19) yes C35 . C34 . C39 . 118.8(2) yes C34 . C35 . C36 . 120.5(3) yes C34 . C35 . H351 . 118.8 no C36 . C35 . H351 . 120.7 no C35 . C36 . C37 . 120.3(3) yes C35 . C36 . H361 . 119.6 no C37 . C36 . H361 . 120.1 no C36 . C37 . C38 . 120.1(3) yes C36 . C37 . H371 . 120.1 no C38 . C37 . H371 . 119.9 no C37 . C38 . C39 . 120.0(3) yes C37 . C38 . H381 . 120.1 no C39 . C38 . H381 . 119.9 no C34 . C39 . C38 . 120.3(3) yes C34 . C39 . H391 . 119.5 no C38 . C39 . H391 . 120.2 no P3 . C40 . C41 . 121.55(19) yes P3 . C40 . C45 . 119.84(18) yes C41 . C40 . C45 . 118.6(2) yes C40 . C41 . C42 . 120.6(2) yes C40 . C41 . H411 . 120.0 no C42 . C41 . H411 . 119.4 no C41 . C42 . C43 . 120.1(2) yes C41 . C42 . H421 . 119.8 no C43 . C42 . H421 . 120.1 no C42 . C43 . C44 . 119.8(3) yes C42 . C43 . H431 . 119.8 no C44 . C43 . H431 . 120.4 no C43 . C44 . C45 . 120.1(3) yes C43 . C44 . H441 . 119.8 no C45 . C44 . H441 . 120.1 no C44 . C45 . C40 . 120.8(2) yes C44 . C45 . H451 . 118.6 no C40 . C45 . H451 . 120.6 no O2 . C46 . C47 . 106.5(3) yes O2 . C46 . H461 . 109.0 no C47 . C46 . H461 . 111.0 no O2 . C46 . H462 . 110.4 no C47 . C46 . H462 . 110.2 no H461 . C46 . H462 . 109.8 no C46 . C47 . C48 . 101.9(3) yes C46 . C47 . H471 . 113.1 no C48 . C47 . H471 . 111.0 no C46 . C47 . H472 . 110.8 no C48 . C47 . H472 . 109.5 no H471 . C47 . H472 . 110.3 no C47 . C48 . C49 . 102.4(3) yes C47 . C48 . H481 . 108.2 no C49 . C48 . H481 . 99.9 no C47 . C48 . H482 . 111.0 no C49 . C48 . H482 . 116.5 no H481 . C48 . H482 . 117.4 no O2 . C49 . C48 . 108.6(4) yes O2 . C49 . H491 . 109.9 no C48 . C49 . H491 . 109.1 no O2 . C49 . H492 . 109.5 no C48 . C49 . H492 . 108.5 no H491 . C49 . H492 . 111.2 no C501 2_666 C51 . C500 2_666 98.1(5) yes C501 2_666 C51 . O1 . 49.3(3) yes C500 2_666 C51 . O1 . 141.1(4) yes C501 2_666 C51 . C501 . 71.7(5) yes O1 . C51 . C501 . 110.8(5) yes C501 2_666 C51 . H511 . 151.6 no C500 2_666 C51 . H511 . 95.6 no O1 . C51 . H511 . 106.9 no C501 . C51 . H511 . 112.0 no C501 2_666 C51 . H512 . 94.3 no C500 2_666 C51 . H512 . 94.2 no O1 . C51 . H512 . 107.1 no C501 . C51 . H512 . 110.4 no H511 . C51 . H512 . 109.5 no C501 2_666 C51 . H513 . 112.6 no C500 2_666 C51 . H513 . 112.8 no O1 . C51 . H513 . 72.2 no C501 . C51 . H513 . 109.2 no C501 2_666 C51 . H514 . 112.4 no C500 2_666 C51 . H514 . 112.6 no O1 . C51 . H514 . 101.0 no C501 . C51 . H514 . 136.6 no H511 . C51 . H514 . 84.7 no H512 . C51 . H513 . 137.4 no H513 . C51 . H514 . 108.2 no N101 . C101 . C102 . 112.2(2) yes N101 . C101 . C103 . 109.3(2) yes C102 . C101 . C103 . 112.1(2) yes N101 . C101 . H1011 . 106.6 no C102 . C101 . H1011 . 107.9 no C103 . C101 . H1011 . 108.6 no C101 . C102 . H1021 . 109.4 no C101 . C102 . H1022 . 110.1 no H1021 . C102 . H1022 . 109.2 no C101 . C102 . H1023 . 110.9 no H1021 . C102 . H1023 . 108.4 no H1022 . C102 . H1023 . 108.8 no C101 . C103 . H1031 . 109.6 no C101 . C103 . H1032 . 108.9 no H1031 . C103 . H1032 . 108.5 no C101 . C103 . H1033 . 109.6 no H1031 . C103 . H1033 . 109.5 no H1032 . C103 . H1033 . 110.7 no P101 . C104 . C105 . 119.50(19) yes P101 . C104 . C109 . 121.9(2) yes C105 . C104 . C109 . 118.5(2) yes C104 . C105 . C106 . 120.7(3) yes C104 . C105 . H1051 . 119.7 no C106 . C105 . H1051 . 119.6 no C105 . C106 . C107 . 120.0(3) yes C105 . C106 . H1061 . 119.2 no C107 . C106 . H1061 . 120.8 no C106 . C107 . C108 . 119.8(3) yes C106 . C107 . H1071 . 119.4 no C108 . C107 . H1071 . 120.8 no C107 . C108 . C109 . 120.5(3) yes C107 . C108 . H1081 . 120.7 no C109 . C108 . H1081 . 118.8 no C104 . C109 . C108 . 120.4(3) yes C104 . C109 . H1091 . 119.9 no C108 . C109 . H1091 . 119.7 no P101 . C110 . C111 . 123.2(2) yes P101 . C110 . C115 . 118.89(18) yes C111 . C110 . C115 . 117.9(2) yes C110 . C111 . C112 . 120.7(3) yes C110 . C111 . H1111 . 119.1 no C112 . C111 . H1111 . 120.2 no C111 . C112 . C113 . 120.4(3) yes C111 . C112 . H1121 . 119.1 no C113 . C112 . H1121 . 120.6 no C112 . C113 . C114 . 120.0(3) yes C112 . C113 . H1131 . 120.2 no C114 . C113 . H1131 . 119.8 no C113 . C114 . C115 . 120.0(3) yes C113 . C114 . H1141 . 119.8 no C115 . C114 . H1141 . 120.2 no C110 . C115 . C114 . 121.1(2) yes C110 . C115 . H1151 . 118.6 no C114 . C115 . H1151 . 120.3 no N102 . C116 . C117 . 112.2(2) yes N102 . C116 . C118 . 109.7(2) yes C117 . C116 . C118 . 111.5(2) yes N102 . C116 . H1161 . 107.8 no C117 . C116 . H1161 . 106.5 no C118 . C116 . H1161 . 109.0 no C116 . C117 . H1171 . 110.3 no C116 . C117 . H1172 . 109.4 no H1171 . C117 . H1172 . 108.3 no C116 . C117 . H1173 . 110.3 no H1171 . C117 . H1173 . 108.5 no H1172 . C117 . H1173 . 110.0 no C116 . C118 . H1181 . 110.5 no C116 . C118 . H1182 . 110.4 no H1181 . C118 . H1182 . 109.0 no C116 . C118 . H1183 . 110.6 no H1181 . C118 . H1183 . 108.6 no H1182 . C118 . H1183 . 107.7 no P102 . C119 . C120 . 120.46(19) yes P102 . C119 . C124 . 120.83(19) yes C120 . C119 . C124 . 118.5(2) yes C119 . C120 . C121 . 120.1(3) yes C119 . C120 . H1201 . 119.5 no C121 . C120 . H1201 . 120.3 no C120 . C121 . C122 . 120.8(3) yes C120 . C121 . H1211 . 118.8 no C122 . C121 . H1211 . 120.4 no C121 . C122 . C123 . 119.8(3) yes C121 . C122 . H1221 . 119.3 no C123 . C122 . H1221 . 120.9 no C122 . C123 . C124 . 119.7(3) yes C122 . C123 . H1231 . 119.4 no C124 . C123 . H1231 . 120.9 no C119 . C124 . C123 . 121.0(3) yes C119 . C124 . H1241 . 119.4 no C123 . C124 . H1241 . 119.6 no P102 . C125 . C126 . 121.3(2) yes P102 . C125 . C130 . 120.11(19) yes C126 . C125 . C130 . 118.6(2) yes C125 . C126 . C127 . 120.7(3) yes C125 . C126 . H1261 . 120.0 no C127 . C126 . H1261 . 119.3 no C126 . C127 . C128 . 119.9(3) yes C126 . C127 . H1271 . 119.6 no C128 . C127 . H1271 . 120.5 no C127 . C128 . C129 . 120.3(3) yes C127 . C128 . H1281 . 119.4 no C129 . C128 . H1281 . 120.2 no C128 . C129 . C130 . 119.8(3) yes C128 . C129 . H1291 . 120.9 no C130 . C129 . H1291 . 119.3 no C129 . C130 . C125 . 120.6(3) yes C129 . C130 . H1301 . 120.2 no C125 . C130 . H1301 . 119.2 no N103 . C131 . C132 . 112.6(2) yes N103 . C131 . C133 . 109.8(2) yes C132 . C131 . C133 . 111.2(2) yes N103 . C131 . H1311 . 106.7 no C132 . C131 . H1311 . 107.9 no C133 . C131 . H1311 . 108.4 no C131 . C132 . H1321 . 112.0 no C131 . C132 . H1322 . 110.2 no H1321 . C132 . H1322 . 108.0 no C131 . C132 . H1323 . 109.1 no H1321 . C132 . H1323 . 108.7 no H1322 . C132 . H1323 . 108.8 no C131 . C133 . H1331 . 111.4 no C131 . C133 . H1332 . 109.9 no H1331 . C133 . H1332 . 108.9 no C131 . C133 . H1333 . 110.0 no H1331 . C133 . H1333 . 107.9 no H1332 . C133 . H1333 . 108.6 no P103 . C134 . C135 . 121.5(2) yes P103 . C134 . C139 . 119.61(18) yes C135 . C134 . C139 . 118.7(2) yes C134 . C135 . C136 . 120.6(3) yes C134 . C135 . H1351 . 119.9 no C136 . C135 . H1351 . 119.4 no C135 . C136 . C137 . 120.2(2) yes C135 . C136 . H1361 . 119.5 no C137 . C136 . H1361 . 120.3 no C136 . C137 . C138 . 119.8(3) yes C136 . C137 . H1371 . 119.9 no C138 . C137 . H1371 . 120.3 no C137 . C138 . C139 . 120.1(2) yes C137 . C138 . H1381 . 119.7 no C139 . C138 . H1381 . 120.2 no C134 . C139 . C138 . 120.6(2) yes C134 . C139 . H1391 . 119.9 no C138 . C139 . H1391 . 119.5 no P103 . C140 . C141 . 121.99(18) yes P103 . C140 . C145 . 119.82(18) yes C141 . C140 . C145 . 118.2(2) yes C140 . C141 . C142 . 120.6(2) yes C140 . C141 . H1411 . 119.7 no C142 . C141 . H1411 . 119.7 no C141 . C142 . C143 . 120.4(2) yes C141 . C142 . H1421 . 119.2 no C143 . C142 . H1421 . 120.4 no C142 . C143 . C144 . 119.7(2) yes C142 . C143 . H1431 . 120.3 no C144 . C143 . H1431 . 120.0 no C143 . C144 . C145 . 120.0(2) yes C143 . C144 . H1441 . 120.6 no C145 . C144 . H1441 . 119.3 no C144 . C145 . C140 . 121.1(2) yes C144 . C145 . H1451 . 119.8 no C140 . C145 . H1451 . 119.1 no C51 2_666 C500 . H5012 2_666 84.8 no C51 2_666 C500 . O1 . 110.2(6) yes H5012 2_666 C500 . O1 . 84.9 no C51 2_666 C500 . C501 2_666 57.8(8) yes H5012 2_666 C500 . C501 2_666 52.4 no O1 . C500 . C501 2_666 61.8(8) yes C51 2_666 C500 . H5001 . 104.8 no O1 . C500 . H5001 . 103.6 no C501 2_666 C500 . H5001 . 86.9 no C51 2_666 C500 . H5002 . 113.9 no H5012 2_666 C500 . H5002 . 143.9 no O1 . C500 . H5002 . 113.9 no C501 2_666 C500 . H5002 . 163.5 no H5001 . C500 . H5002 . 109.5 no C51 2_666 C501 . H5001 2_666 140.3 no C51 2_666 C501 . C501 2_666 48.8(4) yes H5001 2_666 C501 . C501 2_666 157.4 no C51 2_666 C501 . C51 . 108.3(5) yes H5001 2_666 C501 . C51 . 106.5 no C501 2_666 C501 . C51 . 59.5(4) yes C51 2_666 C501 . O1 2_666 61.7(4) yes H5001 2_666 C501 . O1 2_666 99.4 no C501 2_666 C501 . O1 2_666 101.6(6) yes C51 . C501 . O1 2_666 143.0(7) yes C51 2_666 C501 . C500 2_666 143.5(10) yes H5001 2_666 C501 . C500 2_666 51.7 no C501 2_666 C501 . C500 2_666 139.1(12) yes C51 . C501 . C500 2_666 91.8(9) yes O1 2_666 C501 . C500 2_666 83.8(9) yes C51 2_666 C501 . H5011 . 109.5 no H5001 2_666 C501 . H5011 . 78.7 no C501 2_666 C501 . H5011 . 120.8 no C51 . C501 . H5011 . 105.3 no O1 2_666 C501 . H5011 . 54.3 no C51 2_666 C501 . H5012 . 113.5 no C501 2_666 C501 . H5012 . 129.7 no C51 . C501 . H5012 . 110.5 no O1 2_666 C501 . H5012 . 105.8 no C500 2_666 C501 . H5012 . 85.6 no H5011 . C501 . H5012 . 109.5 no C51 . H511 . H513 . 71.0 no C51 . H512 . H514 . 76.4 no H5012 2_666 H5001 . C501 2_666 51.5 no H5012 2_666 H5001 . C500 . 93.0 no O1 2_666 H5011 . C501 . 77.8 no H5001 2_666 H5012 . C500 2_666 52.6 no H5001 2_666 H5012 . C501 . 94.5 no H511 . H513 . C51 . 70.0 no C51 . H514 . H512 . 74.3 no _iucr_refine_instructions_details_constraints ; # # Punched on 26/11/12 at 17:59:58 # #LIST 12 BLOCK CONT SCALE CONT FE ( 1 ,X'S,U'S) UNTIL F ( 101 ) CONT O ( 1 ,X'S,U[ISO]) CONT O ( 2 ,X'S,U'S) UNTIL C ( 145 ) CONT C ( 500 ,X'S,U[ISO]) UNTIL C ( 501 ) RIDE C ( 1,X'S) H ( 11,X'S) RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S) RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S) RIDE C ( 5,X'S) H ( 51,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,X'S) RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 322,X'S) H ( 323,X'S) RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C ( 36,X'S) H ( 361,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H ( 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 46,X'S) H ( 461,X'S) H ( 462,X'S) RIDE C ( 47,X'S) H ( 471,X'S) H ( 472,X'S) RIDE C ( 48,X'S) H ( 481,X'S) H ( 482,X'S) RIDE C ( 49,X'S) H ( 491,X'S) H ( 492,X'S) RIDE C ( 51,X'S) H ( 511,X'S) H ( 512,X'S) RIDE C ( 101,X'S) H (1011,X'S) RIDE C ( 102,X'S) H (1021,X'S) H (1022,X'S) H (1023,X'S) RIDE C ( 103,X'S) H (1031,X'S) H (1032,X'S) H (1033,X'S) RIDE C ( 105,X'S) H (1051,X'S) RIDE C ( 106,X'S) H (1061,X'S) RIDE C ( 107,X'S) H (1071,X'S) RIDE C ( 108,X'S) H (1081,X'S) RIDE C ( 109,X'S) H (1091,X'S) RIDE C ( 111,X'S) H (1111,X'S) RIDE C ( 112,X'S) H (1121,X'S) RIDE C ( 113,X'S) H (1131,X'S) RIDE C ( 114,X'S) H (1141,X'S) RIDE C ( 115,X'S) H (1151,X'S) RIDE C ( 116,X'S) H (1161,X'S) RIDE C ( 117,X'S) H (1171,X'S) H (1172,X'S) H (1173,X'S) RIDE C ( 118,X'S) H (1181,X'S) H (1182,X'S) H (1183,X'S) RIDE C ( 120,X'S) H (1201,X'S) RIDE C ( 121,X'S) H (1211,X'S) RIDE C ( 122,X'S) H (1221,X'S) RIDE C ( 123,X'S) H (1231,X'S) RIDE C ( 124,X'S) H (1241,X'S) RIDE C ( 126,X'S) H (1261,X'S) RIDE C ( 127,X'S) H (1271,X'S) RIDE C ( 128,X'S) H (1281,X'S) RIDE C ( 129,X'S) H (1291,X'S) RIDE C ( 130,X'S) H (1301,X'S) RIDE C ( 131,X'S) H (1311,X'S) RIDE C ( 132,X'S) H (1321,X'S) H (1322,X'S) H (1323,X'S) RIDE C ( 133,X'S) H (1331,X'S) H (1332,X'S) H (1333,X'S) RIDE C ( 135,X'S) H (1351,X'S) RIDE C ( 136,X'S) H (1361,X'S) RIDE C ( 137,X'S) H (1371,X'S) RIDE C ( 138,X'S) H (1381,X'S) RIDE C ( 139,X'S) H (1391,X'S) RIDE C ( 141,X'S) H (1411,X'S) RIDE C ( 142,X'S) H (1421,X'S) RIDE C ( 143,X'S) H (1431,X'S) RIDE C ( 144,X'S) H (1441,X'S) RIDE C ( 145,X'S) H (1451,X'S) REM TOO MANY H ATOMS ON C ( 500), - 4 RIDE C ( 500,X'S) H (5001,X'S) H (5002,X'S) REM TOO MANY H ATOMS ON C ( 501), - 4 RIDE C ( 501,X'S) H (5011,X'S) H (5012,X'S) END ; _iucr_refine_instructions_details_restraints ; # # Punched on 26/11/12 at 17:59:58 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END _database_code_depnum_ccdc_archive 'CCDC 938611'