# Electronic Supplementary Material (ESI) for Chemical Communications # 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 _database_code_depnum_ccdc_archive 'CCDC 908735' #TrackingRef '2.cif' _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 12.30600(10) _cell_length_b 15.6594(2) _cell_length_c 13.3532(2) _cell_angle_alpha 90 _cell_angle_beta 92.9406(6) _cell_angle_gamma 90 _cell_volume 2569.83(5) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C28 B1 Cl1 Fe1 N1 O1 # Dc = 1.21 Fooo = 1048.00 Mu = 7.08 M = 468.42 # Found Formula = C25 H34 B1 Cl1 Fe1 N2 O2 # Dc = 1.28 FOOO = 1048.00 Mu = 7.14 M = 496.67 _chemical_formula_sum 'C25 H34 B1 Cl1 Fe1 N2 O2' _chemical_formula_moiety 'C25 H34 B1 Cl1 Fe1 N2 O2' _chemical_compound_source ? _chemical_formula_weight 496.67 _cell_measurement_reflns_used 6025 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_min 0.080 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.120 _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.714 # Sheldrick geometric approximatio 0.93 0.94 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.94 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 150 _diffrn_reflns_number 48165 _reflns_number_total 5857 _diffrn_reflns_av_R_equivalents 0.027 # Number of reflections without Friedels Law is 11314 # Number of reflections with Friedels Law is 5857 # Theoretical number of reflections is about 5909 _diffrn_reflns_theta_min 5.109 _diffrn_reflns_theta_max 27.510 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.959 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 2.29 _oxford_diffrn_Wilson_scale 12.04 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.48 _refine_diff_density_max 0.56 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 5857 _refine_ls_number_restraints 0 _refine_ls_number_parameters 289 _oxford_refine_ls_R_factor_ref 0.0577 _refine_ls_wR_factor_ref 0.1039 _refine_ls_goodness_of_fit_ref 0.9190 _refine_ls_shift/su_max 0.0008378 _refine_ls_shift/su_mean 0.0000396 # The values computed from all data _oxford_reflns_number_all 5857 _refine_ls_R_factor_all 0.0577 _refine_ls_wR_factor_all 0.1039 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4379 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_gt 0.0810 # 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 none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 13.8 20.2 9.89 2.56 ; # Insert your own references if required - in alphabetical order 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 0.69418(3) 0.84875(2) 0.66537(2) 0.0257 1.0000 Uani . . . . . . C2 C 0.75189(18) 0.93816(15) 0.77750(16) 0.0286 1.0000 Uani . . . . . . C3 C 0.83786(18) 0.88439(15) 0.74805(17) 0.0291 1.0000 Uani . . . . . . C4 C 0.85090(18) 0.89789(16) 0.64216(17) 0.0308 1.0000 Uani . . . . . . C5 C 0.77221(19) 0.95784(15) 0.60730(17) 0.0315 1.0000 Uani . . . . . . C6 C 0.70975(19) 0.98244(15) 0.69099(17) 0.0304 1.0000 Uani . . . . . . C7 C 0.6258(2) 1.05184(17) 0.6869(2) 0.0418 1.0000 Uani . . . . . . C8 C 0.7593(2) 0.99543(19) 0.50408(19) 0.0421 1.0000 Uani . . . . . . C9 C 0.9387(2) 0.85915(18) 0.5825(2) 0.0402 1.0000 Uani . . . . . . C10 C 0.9113(2) 0.83153(18) 0.81599(19) 0.0387 1.0000 Uani . . . . . . C11 C 0.7221(2) 0.95404(17) 0.88357(18) 0.0364 1.0000 Uani . . . . . . C12 C 0.5758(2) 0.85276(17) 0.58894(17) 0.0349 1.0000 Uani . . . . . . O13 O 0.49750(16) 0.85593(16) 0.53724(14) 0.0527 1.0000 Uani . . . . . . C14 C 0.7335(2) 0.74655(17) 0.63223(19) 0.0363 1.0000 Uani . . . . . . O15 O 0.76421(19) 0.68023(13) 0.61103(18) 0.0577 1.0000 Uani . . . . . . B16 B 0.5953(2) 0.78024(16) 0.76283(18) 0.0271 1.0000 Uani . . . . . . Cl17 Cl 0.66985(5) 0.73442(4) 0.87710(4) 0.0337 1.0000 Uani . . . . . . N18 N 0.48028(15) 0.81843(12) 0.79095(14) 0.0280 1.0000 Uani . . . . . . C19 C 0.4362(2) 0.90325(15) 0.81287(18) 0.0314 1.0000 Uani . . . . . . C20 C 0.3380(3) 0.92834(19) 0.7452(2) 0.0498 1.0000 Uani . . . . . . C21 C 0.4121(3) 0.9110(2) 0.9225(2) 0.0493 1.0000 Uani . . . . . . C22 C 0.43273(18) 0.75057(15) 0.74839(16) 0.0273 1.0000 Uani . . . . . . N23 N 0.51811(15) 0.70679(12) 0.71788(14) 0.0275 1.0000 Uani . . . . . . C24 C 0.5316(2) 0.61446(15) 0.70409(18) 0.0318 1.0000 Uani . . . . . . C25 C 0.4683(2) 0.56190(17) 0.7770(2) 0.0467 1.0000 Uani . . . . . . C26 C 0.5045(3) 0.5879(2) 0.5958(2) 0.0506 1.0000 Uani . . . . . . C27 C 0.31627(18) 0.72731(15) 0.73573(17) 0.0289 1.0000 Uani . . . . . . C28 C 0.2551(2) 0.71436(16) 0.81906(19) 0.0354 1.0000 Uani . . . . . . C29 C 0.1474(2) 0.68809(18) 0.8065(2) 0.0410 1.0000 Uani . . . . . . C30 C 0.1013(2) 0.67642(17) 0.7110(2) 0.0408 1.0000 Uani . . . . . . C31 C 0.1607(2) 0.69086(18) 0.6276(2) 0.0395 1.0000 Uani . . . . . . C32 C 0.26889(19) 0.71611(16) 0.64003(18) 0.0334 1.0000 Uani . . . . . . H71 H 0.5770 1.0436 0.6297 0.0625 1.0000 Uiso R . . . . . H72 H 0.6623 1.1032 0.6758 0.0623 1.0000 Uiso R . . . . . H73 H 0.5867 1.0543 0.7501 0.0637 1.0000 Uiso R . . . . . H81 H 0.6834 1.0026 0.4861 0.0632 1.0000 Uiso R . . . . . H82 H 0.7935 1.0506 0.4993 0.0636 1.0000 Uiso R . . . . . H83 H 0.7899 0.9577 0.4584 0.0638 1.0000 Uiso R . . . . . H91 H 0.9156 0.8572 0.5114 0.0565 1.0000 Uiso R . . . . . H92 H 1.0031 0.8944 0.5901 0.0588 1.0000 Uiso R . . . . . H93 H 0.9593 0.8028 0.6058 0.0574 1.0000 Uiso R . . . . . H103 H 0.9263 0.7788 0.7839 0.0573 1.0000 Uiso R . . . . . H102 H 0.9788 0.8623 0.8287 0.0582 1.0000 Uiso R . . . . . H101 H 0.8753 0.8214 0.8766 0.0575 1.0000 Uiso R . . . . . H111 H 0.6506 0.9789 0.8847 0.0554 1.0000 Uiso R . . . . . H112 H 0.7699 0.9964 0.9152 0.0548 1.0000 Uiso R . . . . . H113 H 0.7244 0.9033 0.9218 0.0555 1.0000 Uiso R . . . . . H191 H 0.4958 0.9430 0.7961 0.0352 1.0000 Uiso R . . . . . H201 H 0.3252 0.9883 0.7550 0.0728 1.0000 Uiso R . . . . . H202 H 0.3495 0.9174 0.6777 0.0734 1.0000 Uiso R . . . . . H203 H 0.2739 0.8955 0.7618 0.0734 1.0000 Uiso R . . . . . H211 H 0.3903 0.9695 0.9356 0.0753 1.0000 Uiso R . . . . . H212 H 0.4742 0.8958 0.9649 0.0745 1.0000 Uiso R . . . . . H213 H 0.3500 0.8740 0.9319 0.0754 1.0000 Uiso R . . . . . H241 H 0.6106 0.6036 0.7169 0.0385 1.0000 Uiso R . . . . . H251 H 0.4863 0.5039 0.7692 0.0670 1.0000 Uiso R . . . . . H252 H 0.4889 0.5784 0.8447 0.0679 1.0000 Uiso R . . . . . H253 H 0.3899 0.5675 0.7631 0.0674 1.0000 Uiso R . . . . . H263 H 0.5230 0.5274 0.5904 0.0757 1.0000 Uiso R . . . . . H262 H 0.5455 0.6238 0.5513 0.0773 1.0000 Uiso R . . . . . H261 H 0.4262 0.5957 0.5809 0.0762 1.0000 Uiso R . . . . . H281 H 0.2864 0.7223 0.8845 0.0433 1.0000 Uiso R . . . . . H291 H 0.1049 0.6785 0.8647 0.0496 1.0000 Uiso R . . . . . H301 H 0.0269 0.6587 0.7004 0.0486 1.0000 Uiso R . . . . . H311 H 0.1271 0.6812 0.5638 0.0476 1.0000 Uiso R . . . . . H321 H 0.3106 0.7255 0.5837 0.0415 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 0.02721(16) 0.02855(16) 0.02164(15) -0.00148(12) 0.00332(11) 0.00256(13) C2 0.0313(11) 0.0287(11) 0.0261(10) -0.0034(9) 0.0037(9) -0.0024(9) C3 0.0280(11) 0.0319(11) 0.0272(11) -0.0008(9) 0.0009(8) -0.0003(9) C4 0.0284(11) 0.0351(12) 0.0293(11) -0.0016(9) 0.0055(9) 0.0000(9) C5 0.0329(11) 0.0346(12) 0.0273(11) 0.0041(9) 0.0052(9) 0.0006(10) C6 0.0309(11) 0.0276(11) 0.0331(12) 0.0007(9) 0.0040(9) 0.0033(9) C7 0.0412(14) 0.0315(13) 0.0534(16) 0.0027(11) 0.0097(12) 0.0090(11) C8 0.0484(15) 0.0459(15) 0.0322(12) 0.0108(11) 0.0054(11) 0.0006(12) C9 0.0349(12) 0.0501(16) 0.0366(13) -0.0043(11) 0.0117(10) 0.0043(11) C10 0.0343(12) 0.0459(15) 0.0353(12) 0.0015(11) -0.0035(10) 0.0026(11) C11 0.0443(14) 0.0375(13) 0.0280(11) -0.0087(10) 0.0080(10) -0.0036(11) C12 0.0380(12) 0.0425(13) 0.0245(10) 0.0028(10) 0.0046(9) -0.0018(11) O13 0.0409(10) 0.0807(16) 0.0353(10) 0.0082(10) -0.0100(8) -0.0028(10) C14 0.0365(13) 0.0383(14) 0.0351(12) -0.0013(10) 0.0121(10) -0.0012(10) O15 0.0660(14) 0.0419(11) 0.0682(14) -0.0137(10) 0.0324(11) 0.0049(10) B16 0.0298(12) 0.0289(12) 0.0229(11) -0.0036(9) 0.0038(9) 0.0031(10) Cl17 0.0394(3) 0.0344(3) 0.0267(3) 0.0017(2) -0.0027(2) 0.0016(2) N18 0.0308(9) 0.0279(9) 0.0256(9) -0.0029(7) 0.0061(7) 0.0028(8) C19 0.0353(12) 0.0266(11) 0.0328(11) -0.0017(9) 0.0080(9) 0.0044(9) C20 0.0593(18) 0.0380(15) 0.0510(16) -0.0003(12) -0.0071(13) 0.0169(13) C21 0.0633(18) 0.0487(16) 0.0366(14) -0.0115(12) 0.0102(13) 0.0147(14) C22 0.0301(11) 0.0304(11) 0.0218(10) 0.0016(8) 0.0047(8) 0.0018(9) N23 0.0293(9) 0.0281(9) 0.0252(9) -0.0033(7) 0.0032(7) 0.0017(7) C24 0.0350(12) 0.0269(11) 0.0335(12) -0.0067(9) 0.0027(9) 0.0044(9) C25 0.0484(15) 0.0301(13) 0.0630(18) 0.0027(12) 0.0147(13) 0.0023(11) C26 0.0603(18) 0.0494(17) 0.0415(15) -0.0201(13) -0.0047(13) 0.0092(14) C27 0.0306(11) 0.0280(11) 0.0283(11) 0.0011(9) 0.0045(9) 0.0039(9) C28 0.0371(13) 0.0384(13) 0.0312(11) 0.0076(10) 0.0074(9) 0.0063(10) C29 0.0368(13) 0.0427(14) 0.0448(14) 0.0114(12) 0.0144(11) 0.0014(11) C30 0.0284(12) 0.0391(14) 0.0553(16) 0.0074(12) 0.0068(11) -0.0019(10) C31 0.0335(13) 0.0437(14) 0.0411(13) -0.0013(11) -0.0002(10) -0.0002(11) C32 0.0315(12) 0.0378(13) 0.0313(11) 0.0007(10) 0.0049(9) 0.0003(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2859(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 Fe1 . C2 . 2.144(2) yes Fe1 . C3 . 2.111(2) yes Fe1 . C4 . 2.114(2) yes Fe1 . C5 . 2.125(2) yes Fe1 . C6 . 2.128(2) yes Fe1 . C12 . 1.736(2) yes Fe1 . C14 . 1.736(3) yes Fe1 . B16 . 2.119(3) yes C2 . C3 . 1.423(3) yes C2 . C6 . 1.422(3) yes C2 . C11 . 1.502(3) yes C3 . C4 . 1.447(3) yes C3 . C10 . 1.497(3) yes C4 . C5 . 1.410(3) yes C4 . C9 . 1.502(3) yes C5 . C6 . 1.441(3) yes C5 . C8 . 1.500(3) yes C6 . C7 . 1.499(3) yes C7 . H71 . 0.956 no C7 . H72 . 0.936 no C7 . H73 . 0.993 no C8 . H81 . 0.959 no C8 . H82 . 0.964 no C8 . H83 . 0.941 no C9 . H91 . 0.978 no C9 . H92 . 0.967 no C9 . H93 . 0.964 no C10 . H103 . 0.953 no C10 . H102 . 0.968 no C10 . H101 . 0.956 no C11 . H111 . 0.963 no C11 . H112 . 0.968 no C11 . H113 . 0.944 no C12 . O13 . 1.157(3) yes C14 . O15 . 1.146(3) yes B16 . Cl17 . 1.882(3) yes B16 . N18 . 1.599(3) yes B16 . N23 . 1.589(3) yes N18 . C19 . 1.470(3) yes N18 . C22 . 1.327(3) yes C19 . C20 . 1.522(4) yes C19 . C21 . 1.513(3) yes C19 . H191 . 0.997 no C20 . H201 . 0.962 no C20 . H202 . 0.935 no C20 . H203 . 0.977 no C21 . H211 . 0.972 no C21 . H212 . 0.958 no C21 . H213 . 0.973 no C22 . N23 . 1.336(3) yes C22 . C27 . 1.480(3) yes N23 . C24 . 1.468(3) yes C24 . C25 . 1.520(4) yes C24 . C26 . 1.525(3) yes C24 . H241 . 0.993 no C25 . H251 . 0.941 no C25 . H252 . 0.963 no C25 . H253 . 0.977 no C26 . H263 . 0.979 no C26 . H262 . 0.977 no C26 . H261 . 0.981 no C27 . C28 . 1.390(3) yes C27 . C32 . 1.388(3) yes C28 . C29 . 1.389(4) yes C28 . H281 . 0.945 no C29 . C30 . 1.381(4) yes C29 . H291 . 0.970 no C30 . C31 . 1.381(4) yes C30 . H301 . 0.961 no C31 . C32 . 1.391(3) yes C31 . H311 . 0.940 no C32 . H321 . 0.944 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 C2 . Fe1 . C3 . 39.07(9) yes C2 . Fe1 . C4 . 65.96(9) yes C3 . Fe1 . C4 . 40.05(8) yes C2 . Fe1 . C5 . 65.81(9) yes C3 . Fe1 . C5 . 66.19(9) yes C4 . Fe1 . C5 . 38.86(9) yes C2 . Fe1 . C6 . 38.88(9) yes C3 . Fe1 . C6 . 65.78(9) yes C4 . Fe1 . C6 . 65.81(9) yes C5 . Fe1 . C6 . 39.60(9) yes C2 . Fe1 . C12 . 128.66(11) yes C3 . Fe1 . C12 . 162.32(11) yes C4 . Fe1 . C12 . 130.16(10) yes C5 . Fe1 . C12 . 97.91(11) yes C6 . Fe1 . C12 . 97.17(11) yes C2 . Fe1 . C14 . 133.89(11) yes C3 . Fe1 . C14 . 98.05(11) yes C4 . Fe1 . C14 . 91.71(10) yes C5 . Fe1 . C14 . 120.72(10) yes C6 . Fe1 . C14 . 157.50(10) yes C2 . Fe1 . B16 . 94.70(9) yes C3 . Fe1 . B16 . 107.74(9) yes C4 . Fe1 . B16 . 146.25(9) yes C5 . Fe1 . B16 . 156.29(9) yes C6 . Fe1 . B16 . 116.69(9) yes C12 . Fe1 . C14 . 96.89(12) yes C12 . Fe1 . B16 . 83.59(10) yes C14 . Fe1 . B16 . 82.31(10) yes Fe1 . C2 . C3 . 69.21(12) yes Fe1 . C2 . C6 . 69.95(13) yes C3 . C2 . C6 . 108.02(19) yes Fe1 . C2 . C11 . 132.72(17) yes C3 . C2 . C11 . 125.4(2) yes C6 . C2 . C11 . 126.1(2) yes Fe1 . C3 . C2 . 71.72(13) yes Fe1 . C3 . C4 . 70.09(13) yes C2 . C3 . C4 . 107.75(19) yes Fe1 . C3 . C10 . 129.36(18) yes C2 . C3 . C10 . 126.4(2) yes C4 . C3 . C10 . 125.4(2) yes Fe1 . C4 . C3 . 69.86(13) yes Fe1 . C4 . C5 . 71.01(13) yes C3 . C4 . C5 . 108.13(19) yes Fe1 . C4 . C9 . 128.09(18) yes C3 . C4 . C9 . 125.3(2) yes C5 . C4 . C9 . 126.4(2) yes Fe1 . C5 . C4 . 70.13(13) yes Fe1 . C5 . C6 . 70.30(13) yes C4 . C5 . C6 . 107.8(2) yes Fe1 . C5 . C8 . 128.48(18) yes C4 . C5 . C8 . 127.1(2) yes C6 . C5 . C8 . 124.9(2) yes Fe1 . C6 . C5 . 70.10(13) yes Fe1 . C6 . C2 . 71.16(13) yes C5 . C6 . C2 . 108.23(19) yes Fe1 . C6 . C7 . 130.64(18) yes C5 . C6 . C7 . 124.0(2) yes C2 . C6 . C7 . 127.2(2) yes C6 . C7 . H71 . 109.5 no C6 . C7 . H72 . 107.0 no H71 . C7 . H72 . 106.0 no C6 . C7 . H73 . 111.1 no H71 . C7 . H73 . 111.9 no H72 . C7 . H73 . 111.0 no C5 . C8 . H81 . 109.4 no C5 . C8 . H82 . 112.7 no H81 . C8 . H82 . 107.5 no C5 . C8 . H83 . 108.8 no H81 . C8 . H83 . 109.2 no H82 . C8 . H83 . 109.2 no C4 . C9 . H91 . 110.3 no C4 . C9 . H92 . 108.8 no H91 . C9 . H92 . 108.4 no C4 . C9 . H93 . 112.5 no H91 . C9 . H93 . 110.0 no H92 . C9 . H93 . 106.7 no C3 . C10 . H103 . 109.4 no C3 . C10 . H102 . 108.4 no H103 . C10 . H102 . 109.0 no C3 . C10 . H101 . 108.3 no H103 . C10 . H101 . 110.3 no H102 . C10 . H101 . 111.4 no C2 . C11 . H111 . 110.4 no C2 . C11 . H112 . 110.6 no H111 . C11 . H112 . 104.6 no C2 . C11 . H113 . 111.7 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.8 no Fe1 . C12 . O13 . 179.3(2) yes Fe1 . C14 . O15 . 176.9(2) yes Fe1 . B16 . Cl17 . 114.81(13) yes Fe1 . B16 . N18 . 119.88(15) yes Cl17 . B16 . N18 . 110.67(15) yes Fe1 . B16 . N23 . 119.04(15) yes Cl17 . B16 . N23 . 106.69(15) yes N18 . B16 . N23 . 80.82(15) yes B16 . N18 . C19 . 136.48(19) yes B16 . N18 . C22 . 88.63(17) yes C19 . N18 . C22 . 130.5(2) yes N18 . C19 . C20 . 113.9(2) yes N18 . C19 . C21 . 111.0(2) yes C20 . C19 . C21 . 111.4(2) yes N18 . C19 . H191 . 103.6 no C20 . C19 . H191 . 106.1 no C21 . C19 . H191 . 110.5 no C19 . C20 . H201 . 107.6 no C19 . C20 . H202 . 111.7 no H201 . C20 . H202 . 110.0 no C19 . C20 . H203 . 110.8 no H201 . C20 . H203 . 110.1 no H202 . C20 . H203 . 106.7 no C19 . C21 . H211 . 108.6 no C19 . C21 . H212 . 111.2 no H211 . C21 . H212 . 110.3 no C19 . C21 . H213 . 105.7 no H211 . C21 . H213 . 108.3 no H212 . C21 . H213 . 112.5 no N18 . C22 . N23 . 101.84(19) yes N18 . C22 . C27 . 130.5(2) yes N23 . C22 . C27 . 127.7(2) yes B16 . N23 . C22 . 88.71(17) yes B16 . N23 . C24 . 133.70(19) yes C22 . N23 . C24 . 129.8(2) yes N23 . C24 . C25 . 112.84(19) yes N23 . C24 . C26 . 111.5(2) yes C25 . C24 . C26 . 111.4(2) yes N23 . C24 . H241 . 105.2 no C25 . C24 . H241 . 109.1 no C26 . C24 . H241 . 106.3 no C24 . C25 . H251 . 108.7 no C24 . C25 . H252 . 109.7 no H251 . C25 . H252 . 108.1 no C24 . C25 . H253 . 111.3 no H251 . C25 . H253 . 107.5 no H252 . C25 . H253 . 111.4 no C24 . C26 . H263 . 107.1 no C24 . C26 . H262 . 109.0 no H263 . C26 . H262 . 112.5 no C24 . C26 . H261 . 108.8 no H263 . C26 . H261 . 109.6 no H262 . C26 . H261 . 109.7 no C22 . C27 . C28 . 120.4(2) yes C22 . C27 . C32 . 119.7(2) yes C28 . C27 . C32 . 119.9(2) yes C27 . C28 . C29 . 119.9(2) yes C27 . C28 . H281 . 120.5 no C29 . C28 . H281 . 119.5 no C28 . C29 . C30 . 119.7(2) yes C28 . C29 . H291 . 119.9 no C30 . C29 . H291 . 120.4 no C29 . C30 . C31 . 120.9(2) yes C29 . C30 . H301 . 121.2 no C31 . C30 . H301 . 117.9 no C30 . C31 . C32 . 119.6(2) yes C30 . C31 . H311 . 118.6 no C32 . C31 . H311 . 121.8 no C31 . C32 . C27 . 120.0(2) yes C31 . C32 . H321 . 120.4 no C27 . C32 . H321 . 119.6 no _iucr_refine_instruction_details_constraints ; # # Punched on 08/12/11 at 11:43:00 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S) H ( 73,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) H ( 93,X'S) RIDE C ( 10,X'S) H ( 103,X'S) H ( 102,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) H ( 203,X'S) RIDE C ( 21,X'S) H ( 211,X'S) H ( 212,X'S) H ( 213,X'S) RIDE C ( 24,X'S) H ( 241,X'S) RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S) H ( 253,X'S) RIDE C ( 26,X'S) H ( 263,X'S) H ( 262,X'S) H ( 261,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) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 08/12/11 at 11:43:00 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; data_3 _database_code_depnum_ccdc_archive 'CCDC 908736' #TrackingRef '3.cif' _audit_creation_date 12-06-21 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 062efnp12 _chemical_name_systematic . _chemical_melting_point . _cell_length_a 13.9947(2) _cell_length_b 16.4994(2) _cell_length_c 14.7643(2) _cell_angle_alpha 90 _cell_angle_beta 95.8847(6) _cell_angle_gamma 90 _cell_volume 3391.17(8) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' 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' 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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C35 H44 B1 Fe1 N2 O2 # Dc = 1.16 Fooo = 1328.00 Mu = 4.75 M = 591.40 # Found Formula = C35 H44 B1 Cl1 Fe1 N2 O2 # Dc = 1.23 FOOO = 1328.00 Mu = 5.55 M = 626.86 _chemical_formula_sum 'C35 H44 B Cl Fe N2 O2' _chemical_formula_moiety 'C35 H44 B Cl Fe N2 O2' _chemical_compound_source . _chemical_formula_weight 626.86 _cell_measurement_reflns_used 7928 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.200 _exptl_crystal_size_mid 0.380 _exptl_crystal_size_max 0.400 _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.555 # Sheldrick geometric approximatio 0.81 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.89 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _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 150 _diffrn_reflns_number 51634 _reflns_number_total 7705 _diffrn_reflns_av_R_equivalents 0.044 # Number of reflections without Friedels Law is 15117 # Number of reflections with Friedels Law is 7705 # Theoretical number of reflections is about 7779 _diffrn_reflns_theta_min 5.103 _diffrn_reflns_theta_max 27.486 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.936 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 2.52 _oxford_diffrn_Wilson_scale 21.13 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.66 _refine_diff_density_max 0.63 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 7704 _refine_ls_number_restraints 0 _refine_ls_number_parameters 379 _oxford_refine_ls_R_factor_ref 0.0859 _refine_ls_wR_factor_ref 0.1314 _refine_ls_goodness_of_fit_ref 0.9605 _refine_ls_shift/su_max 0.0005752 _refine_ls_shift/su_mean 0.0000171 # The values computed from all data _oxford_reflns_number_all 7705 _refine_ls_R_factor_all 0.0860 _refine_ls_wR_factor_all 0.1316 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5137 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_gt 0.0955 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 7.97 11.1 5.34 1.46 ; # Insert your own references if required - in alphabetical order 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 0.04318(3) 0.17908(3) 0.69041(3) 0.0293 1.0000 Uani . . . . . . C2 C -0.0460(2) 0.2493(2) 0.6560(2) 0.0361 1.0000 Uani . . . . . . O3 O -0.10580(17) 0.29559(15) 0.63332(18) 0.0499 1.0000 Uani . . . . . . C4 C 0.0422(2) 0.13287(19) 0.5837(2) 0.0332 1.0000 Uani . . . . . . O5 O 0.03653(17) 0.09825(16) 0.51545(16) 0.0460 1.0000 Uani . . . . . . C6 C 0.1146(2) 0.08169(19) 0.7619(2) 0.0348 1.0000 Uani . . . . . . C7 C 0.1349(2) 0.1546(2) 0.8118(2) 0.0358 1.0000 Uani . . . . . . C8 C 0.0453(2) 0.18708(19) 0.8339(2) 0.0349 1.0000 Uani . . . . . . C9 C -0.0299(2) 0.1328(2) 0.7985(2) 0.0347 1.0000 Uani . . . . . . C10 C 0.0121(2) 0.06834(19) 0.7542(2) 0.0355 1.0000 Uani . . . . . . C11 C -0.0389(3) -0.0039(2) 0.7098(3) 0.0514 1.0000 Uani . . . . . . C12 C -0.1346(3) 0.1424(3) 0.8097(3) 0.0547 1.0000 Uani . . . . . . C13 C 0.0328(3) 0.2579(2) 0.8951(2) 0.0521 1.0000 Uani . . . . . . C14 C 0.2332(2) 0.1861(3) 0.8435(2) 0.0494 1.0000 Uani . . . . . . C15 C 0.1874(3) 0.0232(2) 0.7326(3) 0.0503 1.0000 Uani . . . . . . B16 B 0.1295(2) 0.2694(2) 0.6550(2) 0.0314 1.0000 Uani . . . . . . Cl17 Cl 0.12885(6) 0.36342(5) 0.72293(6) 0.0414 1.0000 Uani . . . . . . N18 N 0.18557(18) 0.27941(14) 0.58060(17) 0.0307 1.0000 Uani . . . . . . C19 C 0.2160(2) 0.21322(17) 0.5266(2) 0.0302 1.0000 Uani . . . . . . C20 C 0.2673(2) 0.15264(18) 0.5680(2) 0.0326 1.0000 Uani . . . . . . C21 C 0.3034(2) 0.07871(18) 0.5262(2) 0.0320 1.0000 Uani . . . . . . N22 N 0.25883(19) 0.04822(15) 0.45415(17) 0.0343 1.0000 Uani . . . . . . C23 C 0.2932(2) -0.02429(18) 0.4165(2) 0.0331 1.0000 Uani . . . . . . C24 C 0.2662(2) -0.09967(19) 0.4501(2) 0.0350 1.0000 Uani . . . . . . C25 C 0.2049(3) -0.1041(2) 0.5284(2) 0.0445 1.0000 Uani . . . . . . C26 C 0.2967(2) -0.1703(2) 0.4105(2) 0.0379 1.0000 Uani . . . . . . C27 C 0.3526(2) -0.1683(2) 0.3385(2) 0.0374 1.0000 Uani . . . . . . C28 C 0.3844(3) -0.2468(2) 0.2987(3) 0.0526 1.0000 Uani . . . . . . C29 C 0.3760(2) -0.0933(2) 0.3043(2) 0.0389 1.0000 Uani . . . . . . C30 C 0.3466(2) -0.0205(2) 0.3414(2) 0.0382 1.0000 Uani . . . . . . C31 C 0.3724(3) 0.0601(2) 0.3025(3) 0.0574 1.0000 Uani . . . . . . C32 C 0.3940(2) 0.0443(2) 0.5758(2) 0.0463 1.0000 Uani . . . . . . C33 C 0.1886(2) 0.21905(19) 0.4259(2) 0.0380 1.0000 Uani . . . . . . C34 C 0.2184(2) 0.35785(18) 0.5509(2) 0.0334 1.0000 Uani . . . . . . C35 C 0.3144(2) 0.3802(2) 0.5737(2) 0.0378 1.0000 Uani . . . . . . C36 C 0.3811(2) 0.3282(2) 0.6349(3) 0.0485 1.0000 Uani . . . . . . C37 C 0.3464(3) 0.4532(2) 0.5399(2) 0.0430 1.0000 Uani . . . . . . C38 C 0.2866(3) 0.5039(2) 0.4850(2) 0.0459 1.0000 Uani . . . . . . C39 C 0.3250(3) 0.5798(2) 0.4441(3) 0.0604 1.0000 Uani . . . . . . C40 C 0.1909(3) 0.4817(2) 0.4665(2) 0.0437 1.0000 Uani . . . . . . C41 C 0.1553(2) 0.40928(19) 0.4989(2) 0.0381 1.0000 Uani . . . . . . C42 C 0.0501(3) 0.3894(2) 0.4778(3) 0.0496 1.0000 Uani . . . . . . H111 H -0.1022 0.0134 0.6845 0.0794 1.0000 Uiso R . . . . . H113 H -0.0429 -0.0464 0.7553 0.0790 1.0000 Uiso R . . . . . H112 H -0.0031 -0.0227 0.6609 0.0797 1.0000 Uiso R . . . . . H122 H -0.1732 0.1154 0.7597 0.0864 1.0000 Uiso R . . . . . H121 H -0.1469 0.1197 0.8669 0.0857 1.0000 Uiso R . . . . . H123 H -0.1494 0.1995 0.8098 0.0859 1.0000 Uiso R . . . . . H133 H -0.0293 0.2811 0.8764 0.0835 1.0000 Uiso R . . . . . H131 H 0.0357 0.2399 0.9581 0.0834 1.0000 Uiso R . . . . . H132 H 0.0827 0.2980 0.8873 0.0840 1.0000 Uiso R . . . . . H141 H 0.2303 0.2447 0.8507 0.0784 1.0000 Uiso R . . . . . H142 H 0.2545 0.1609 0.9023 0.0783 1.0000 Uiso R . . . . . H143 H 0.2786 0.1732 0.7997 0.0781 1.0000 Uiso R . . . . . H153 H 0.1708 0.0072 0.6703 0.0785 1.0000 Uiso R . . . . . H151 H 0.1922 -0.0243 0.7705 0.0785 1.0000 Uiso R . . . . . H152 H 0.2498 0.0496 0.7371 0.0791 1.0000 Uiso R . . . . . H201 H 0.2838 0.1577 0.6322 0.0418 1.0000 Uiso R . . . . . H251 H 0.1752 -0.1575 0.5301 0.0692 1.0000 Uiso R . . . . . H253 H 0.2472 -0.0953 0.5843 0.0691 1.0000 Uiso R . . . . . H252 H 0.1561 -0.0614 0.5208 0.0692 1.0000 Uiso R . . . . . H261 H 0.2794 -0.2225 0.4339 0.0476 1.0000 Uiso R . . . . . H281 H 0.4310 -0.2339 0.2557 0.0817 1.0000 Uiso R . . . . . H282 H 0.4142 -0.2814 0.3471 0.0823 1.0000 Uiso R . . . . . H283 H 0.3280 -0.2751 0.2677 0.0825 1.0000 Uiso R . . . . . H291 H 0.4124 -0.0900 0.2533 0.0486 1.0000 Uiso R . . . . . H312 H 0.4124 0.0523 0.2528 0.0895 1.0000 Uiso R . . . . . H313 H 0.4081 0.0913 0.3507 0.0896 1.0000 Uiso R . . . . . H311 H 0.3136 0.0893 0.2813 0.0892 1.0000 Uiso R . . . . . H321 H 0.4126 -0.0048 0.5460 0.0715 1.0000 Uiso R . . . . . H323 H 0.3826 0.0320 0.6377 0.0716 1.0000 Uiso R . . . . . H322 H 0.4447 0.0840 0.5766 0.0718 1.0000 Uiso R . . . . . H332 H 0.2280 0.1826 0.3939 0.0601 1.0000 Uiso R . . . . . H331 H 0.1965 0.2734 0.4050 0.0598 1.0000 Uiso R . . . . . H333 H 0.1211 0.2036 0.4120 0.0604 1.0000 Uiso R . . . . . H361 H 0.4389 0.3591 0.6559 0.0741 1.0000 Uiso R . . . . . H363 H 0.3489 0.3112 0.6873 0.0743 1.0000 Uiso R . . . . . H362 H 0.3982 0.2801 0.6027 0.0740 1.0000 Uiso R . . . . . H371 H 0.4118 0.4679 0.5559 0.0540 1.0000 Uiso R . . . . . H391 H 0.2735 0.6192 0.4311 0.0968 1.0000 Uiso R . . . . . H392 H 0.3745 0.6033 0.4862 0.0967 1.0000 Uiso R . . . . . H393 H 0.3524 0.5672 0.3891 0.0962 1.0000 Uiso R . . . . . H401 H 0.1495 0.5178 0.4306 0.0558 1.0000 Uiso R . . . . . H422 H 0.0211 0.4267 0.4319 0.0776 1.0000 Uiso R . . . . . H421 H 0.0194 0.3953 0.5337 0.0771 1.0000 Uiso R . . . . . H423 H 0.0428 0.3337 0.4567 0.0772 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 0.0311(2) 0.0295(2) 0.0274(2) -0.00020(18) 0.00313(15) 0.00132(18) C2 0.0349(16) 0.0393(17) 0.0343(16) -0.0006(13) 0.0043(13) -0.0013(14) O3 0.0406(13) 0.0410(13) 0.0668(17) 0.0067(12) -0.0006(12) 0.0083(11) C4 0.0349(16) 0.0305(15) 0.0346(16) 0.0019(13) 0.0047(12) -0.0028(12) O5 0.0501(14) 0.0516(15) 0.0370(12) -0.0120(11) 0.0076(10) -0.0119(11) C6 0.0383(17) 0.0364(16) 0.0302(15) 0.0049(13) 0.0057(12) 0.0070(13) C7 0.0348(16) 0.0417(17) 0.0300(15) 0.0038(13) -0.0002(12) 0.0035(13) C8 0.0399(16) 0.0376(17) 0.0268(14) 0.0005(13) 0.0011(12) 0.0094(14) C9 0.0331(16) 0.0446(18) 0.0267(14) 0.0077(13) 0.0040(12) 0.0037(13) C10 0.0422(17) 0.0360(16) 0.0281(15) 0.0044(12) 0.0026(12) -0.0009(13) C11 0.064(2) 0.0409(19) 0.048(2) 0.0063(16) 0.0006(17) -0.0125(18) C12 0.0397(19) 0.080(3) 0.047(2) 0.019(2) 0.0141(16) 0.0093(19) C13 0.073(3) 0.048(2) 0.0355(18) -0.0064(16) 0.0045(17) 0.0138(19) C14 0.0400(18) 0.060(2) 0.0453(19) 0.0062(18) -0.0081(15) -0.0029(17) C15 0.064(2) 0.045(2) 0.0450(19) 0.0087(16) 0.0184(17) 0.0213(18) B16 0.0334(17) 0.0298(16) 0.0304(17) -0.0028(13) 0.0006(13) 0.0022(14) Cl17 0.0477(5) 0.0342(4) 0.0438(4) -0.0104(3) 0.0124(3) -0.0048(3) N18 0.0351(13) 0.0240(12) 0.0335(13) -0.0020(10) 0.0052(10) 0.0007(10) C19 0.0330(15) 0.0252(14) 0.0330(15) -0.0025(12) 0.0068(12) -0.0026(12) C20 0.0348(15) 0.0300(15) 0.0332(15) -0.0036(12) 0.0043(12) -0.0008(12) C21 0.0308(15) 0.0292(15) 0.0363(16) -0.0030(12) 0.0039(12) -0.0008(12) N22 0.0378(14) 0.0283(13) 0.0359(14) -0.0045(11) 0.0002(11) 0.0005(11) C23 0.0342(16) 0.0300(15) 0.0336(15) -0.0056(12) -0.0046(12) 0.0044(12) C24 0.0364(16) 0.0324(16) 0.0350(16) -0.0012(13) -0.0024(12) 0.0011(13) C25 0.055(2) 0.0362(17) 0.0425(19) 0.0037(15) 0.0050(15) 0.0016(15) C26 0.0435(17) 0.0307(15) 0.0369(16) -0.0020(13) -0.0090(13) 0.0045(14) C27 0.0358(16) 0.0383(17) 0.0356(16) -0.0073(14) -0.0086(13) 0.0070(14) C28 0.062(2) 0.048(2) 0.045(2) -0.0106(17) -0.0070(17) 0.0174(18) C29 0.0346(16) 0.0489(19) 0.0332(16) -0.0082(14) 0.0029(13) -0.0001(14) C30 0.0352(16) 0.0376(17) 0.0413(17) -0.0058(14) 0.0016(13) -0.0026(13) C31 0.067(3) 0.045(2) 0.064(3) -0.0040(18) 0.023(2) -0.0101(19) C32 0.0371(17) 0.048(2) 0.052(2) -0.0136(16) -0.0038(15) 0.0104(15) C33 0.0496(19) 0.0299(16) 0.0349(16) 0.0020(13) 0.0067(14) 0.0009(14) C34 0.0395(16) 0.0264(14) 0.0354(16) -0.0012(12) 0.0097(13) -0.0013(13) C35 0.0414(17) 0.0348(16) 0.0386(17) -0.0088(13) 0.0110(14) -0.0041(14) C36 0.0375(17) 0.0423(19) 0.064(2) -0.0079(18) -0.0038(16) -0.0038(16) C37 0.0451(19) 0.0385(18) 0.0484(19) -0.0096(15) 0.0188(15) -0.0104(15) C38 0.064(2) 0.0303(16) 0.0472(19) -0.0058(15) 0.0251(17) -0.0070(16) C39 0.084(3) 0.0365(19) 0.067(3) 0.0001(18) 0.035(2) -0.0105(19) C40 0.057(2) 0.0300(16) 0.0461(19) 0.0013(14) 0.0163(16) 0.0053(15) C41 0.0440(18) 0.0303(16) 0.0410(17) -0.0009(13) 0.0100(14) 0.0033(14) C42 0.045(2) 0.045(2) 0.059(2) 0.0092(17) 0.0044(17) 0.0052(16) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.20348(12) 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 . C2 . 1.740(3) yes Fe1 . C4 . 1.750(3) yes Fe1 . C6 . 2.116(3) yes Fe1 . C7 . 2.133(3) yes Fe1 . C8 . 2.120(3) yes Fe1 . C9 . 2.124(3) yes Fe1 . C10 . 2.121(3) yes Fe1 . B16 . 2.021(4) yes C2 . O3 . 1.157(4) yes C4 . O5 . 1.154(4) yes C6 . C7 . 1.423(4) yes C6 . C10 . 1.444(4) yes C6 . C15 . 1.499(4) yes C7 . C8 . 1.433(4) yes C7 . C14 . 1.500(4) yes C8 . C9 . 1.439(4) yes C8 . C13 . 1.498(4) yes C9 . C10 . 1.408(4) yes C9 . C12 . 1.499(4) yes C10 . C11 . 1.504(5) yes C11 . H111 . 0.968 no C11 . H113 . 0.977 no C11 . H112 . 0.970 no C12 . H122 . 0.976 no C12 . H121 . 0.956 no C12 . H123 . 0.965 no C13 . H133 . 0.965 no C13 . H131 . 0.973 no C13 . H132 . 0.977 no C14 . H141 . 0.974 no C14 . H142 . 0.981 no C14 . H143 . 0.976 no C15 . H153 . 0.962 no C15 . H151 . 0.962 no C15 . H152 . 0.970 no B16 . Cl17 . 1.848(3) yes B16 . N18 . 1.423(4) yes N18 . C19 . 1.442(4) yes N18 . C34 . 1.456(4) yes C19 . C20 . 1.340(4) yes C19 . C33 . 1.500(4) yes C20 . C21 . 1.480(4) yes C20 . H201 . 0.957 no C21 . N22 . 1.280(4) yes C21 . C32 . 1.508(4) yes N22 . C23 . 1.423(4) yes C23 . C24 . 1.405(4) yes C23 . C30 . 1.401(5) yes C24 . C25 . 1.510(5) yes C24 . C26 . 1.390(4) yes C25 . H251 . 0.975 no C25 . H253 . 0.976 no C25 . H252 . 0.980 no C26 . C27 . 1.383(5) yes C26 . H261 . 0.969 no C27 . C28 . 1.509(5) yes C27 . C29 . 1.389(5) yes C28 . H281 . 0.979 no C28 . H282 . 0.974 no C28 . H283 . 0.989 no C29 . C30 . 1.399(4) yes C29 . H291 . 0.953 no C30 . C31 . 1.507(5) yes C31 . H312 . 0.976 no C31 . H313 . 0.974 no C31 . H311 . 0.977 no C32 . H321 . 0.971 no C32 . H323 . 0.965 no C32 . H322 . 0.965 no C33 . H332 . 0.972 no C33 . H331 . 0.959 no C33 . H333 . 0.978 no C34 . C35 . 1.401(4) yes C34 . C41 . 1.396(4) yes C35 . C36 . 1.500(5) yes C35 . C37 . 1.396(5) yes C36 . H361 . 0.979 no C36 . H363 . 0.975 no C36 . H362 . 0.969 no C37 . C38 . 1.384(5) yes C37 . H371 . 0.953 no C38 . C39 . 1.514(5) yes C38 . C40 . 1.388(5) yes C39 . H391 . 0.975 no C39 . H392 . 0.963 no C39 . H393 . 0.956 no C40 . C41 . 1.399(4) yes C40 . H401 . 0.953 no C41 . C42 . 1.510(5) yes C42 . H422 . 0.973 no C42 . H421 . 0.973 no C42 . H423 . 0.972 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 C2 . Fe1 . C4 . 95.07(15) yes C2 . Fe1 . C6 . 159.90(13) yes C4 . Fe1 . C6 . 94.46(13) yes C2 . Fe1 . C7 . 136.32(14) yes C4 . Fe1 . C7 . 128.49(13) yes C6 . Fe1 . C7 . 39.14(12) yes C2 . Fe1 . C8 . 100.73(13) yes C4 . Fe1 . C8 . 157.73(13) yes C6 . Fe1 . C8 . 65.89(12) yes C7 . Fe1 . C8 . 39.37(11) yes C2 . Fe1 . C9 . 94.16(13) yes C4 . Fe1 . C9 . 124.08(13) yes C6 . Fe1 . C9 . 65.89(12) yes C7 . Fe1 . C9 . 66.14(12) yes C8 . Fe1 . C9 . 39.63(12) yes C2 . Fe1 . C10 . 121.98(14) yes C4 . Fe1 . C10 . 92.39(13) yes C6 . Fe1 . C10 . 39.85(12) yes C7 . Fe1 . C10 . 66.22(12) yes C8 . Fe1 . C10 . 65.93(12) yes C2 . Fe1 . B16 . 82.14(14) yes C4 . Fe1 . B16 . 92.16(14) yes C6 . Fe1 . B16 . 115.13(13) yes C7 . Fe1 . B16 . 91.89(13) yes C8 . Fe1 . B16 . 105.40(13) yes C9 . Fe1 . C10 . 38.74(12) yes C9 . Fe1 . B16 . 143.76(13) yes C10 . Fe1 . B16 . 154.89(13) yes Fe1 . C2 . O3 . 179.5(3) yes Fe1 . C4 . O5 . 174.7(3) yes Fe1 . C6 . C7 . 71.08(17) yes Fe1 . C6 . C10 . 70.28(17) yes C7 . C6 . C10 . 108.3(3) yes Fe1 . C6 . C15 . 130.2(2) yes C7 . C6 . C15 . 125.9(3) yes C10 . C6 . C15 . 125.4(3) yes Fe1 . C7 . C6 . 69.78(17) yes Fe1 . C7 . C8 . 69.83(17) yes C6 . C7 . C8 . 107.5(3) yes Fe1 . C7 . C14 . 130.6(2) yes C6 . C7 . C14 . 125.7(3) yes C8 . C7 . C14 . 126.5(3) yes Fe1 . C8 . C7 . 70.81(17) yes Fe1 . C8 . C9 . 70.31(16) yes C7 . C8 . C9 . 108.0(3) yes Fe1 . C8 . C13 . 131.4(2) yes C7 . C8 . C13 . 126.0(3) yes C9 . C8 . C13 . 125.4(3) yes Fe1 . C9 . C8 . 70.05(17) yes Fe1 . C9 . C10 . 70.55(17) yes C8 . C9 . C10 . 108.3(3) yes Fe1 . C9 . C12 . 126.6(2) yes C8 . C9 . C12 . 125.5(3) yes C10 . C9 . C12 . 126.1(3) yes Fe1 . C10 . C6 . 69.87(17) yes Fe1 . C10 . C9 . 70.71(18) yes C6 . C10 . C9 . 107.9(3) yes Fe1 . C10 . C11 . 126.7(2) yes C6 . C10 . C11 . 125.3(3) yes C9 . C10 . C11 . 126.8(3) yes C10 . C11 . H111 . 108.0 no C10 . C11 . H113 . 109.1 no H111 . C11 . H113 . 111.2 no C10 . C11 . H112 . 108.7 no H111 . C11 . H112 . 109.2 no H113 . C11 . H112 . 110.6 no C9 . C12 . H122 . 109.9 no C9 . C12 . H121 . 108.9 no H122 . C12 . H121 . 110.7 no C9 . C12 . H123 . 108.4 no H122 . C12 . H123 . 110.1 no H121 . C12 . H123 . 108.8 no C8 . C13 . H133 . 107.1 no C8 . C13 . H131 . 110.1 no H133 . C13 . H131 . 110.0 no C8 . C13 . H132 . 109.2 no H133 . C13 . H132 . 109.3 no H131 . C13 . H132 . 111.1 no C7 . C14 . H141 . 109.4 no C7 . C14 . H142 . 108.4 no H141 . C14 . H142 . 109.6 no C7 . C14 . H143 . 110.8 no H141 . C14 . H143 . 109.0 no H142 . C14 . H143 . 109.6 no C6 . C15 . H153 . 110.3 no C6 . C15 . H151 . 111.4 no H153 . C15 . H151 . 109.2 no C6 . C15 . H152 . 109.0 no H153 . C15 . H152 . 108.4 no H151 . C15 . H152 . 108.4 no Fe1 . B16 . Cl17 . 116.22(18) yes Fe1 . B16 . N18 . 132.6(2) yes Cl17 . B16 . N18 . 110.8(2) yes B16 . N18 . C19 . 123.8(2) yes B16 . N18 . C34 . 123.5(2) yes C19 . N18 . C34 . 112.7(2) yes N18 . C19 . C20 . 119.2(3) yes N18 . C19 . C33 . 116.0(3) yes C20 . C19 . C33 . 124.8(3) yes C19 . C20 . C21 . 127.9(3) yes C19 . C20 . H201 . 116.8 no C21 . C20 . H201 . 115.3 no C20 . C21 . N22 . 120.8(3) yes C20 . C21 . C32 . 114.5(3) yes N22 . C21 . C32 . 124.7(3) yes C21 . N22 . C23 . 120.0(3) yes N22 . C23 . C24 . 119.5(3) yes N22 . C23 . C30 . 120.0(3) yes C24 . C23 . C30 . 120.2(3) yes C23 . C24 . C25 . 120.5(3) yes C23 . C24 . C26 . 119.2(3) yes C25 . C24 . C26 . 120.3(3) yes C24 . C25 . H251 . 109.9 no C24 . C25 . H253 . 107.2 no H251 . C25 . H253 . 109.7 no C24 . C25 . H252 . 108.7 no H251 . C25 . H252 . 111.1 no H253 . C25 . H252 . 110.2 no C24 . C26 . C27 . 121.7(3) yes C24 . C26 . H261 . 119.8 no C27 . C26 . H261 . 118.5 no C26 . C27 . C28 . 119.5(3) yes C26 . C27 . C29 . 118.3(3) yes C28 . C27 . C29 . 122.2(3) yes C27 . C28 . H281 . 108.1 no C27 . C28 . H282 . 109.8 no H281 . C28 . H282 . 109.8 no C27 . C28 . H283 . 109.4 no H281 . C28 . H283 . 110.8 no H282 . C28 . H283 . 108.9 no C27 . C29 . C30 . 122.2(3) yes C27 . C29 . H291 . 120.2 no C30 . C29 . H291 . 117.7 no C23 . C30 . C29 . 118.3(3) yes C23 . C30 . C31 . 120.6(3) yes C29 . C30 . C31 . 121.1(3) yes C30 . C31 . H312 . 110.5 no C30 . C31 . H313 . 108.2 no H312 . C31 . H313 . 109.1 no C30 . C31 . H311 . 109.3 no H312 . C31 . H311 . 110.7 no H313 . C31 . H311 . 109.0 no C21 . C32 . H321 . 110.2 no C21 . C32 . H323 . 109.1 no H321 . C32 . H323 . 109.4 no C21 . C32 . H322 . 109.3 no H321 . C32 . H322 . 109.8 no H323 . C32 . H322 . 108.9 no C19 . C33 . H332 . 110.0 no C19 . C33 . H331 . 110.6 no H332 . C33 . H331 . 109.4 no C19 . C33 . H333 . 109.6 no H332 . C33 . H333 . 108.7 no H331 . C33 . H333 . 108.5 no N18 . C34 . C35 . 119.1(3) yes N18 . C34 . C41 . 120.3(3) yes C35 . C34 . C41 . 120.6(3) yes C34 . C35 . C36 . 121.1(3) yes C34 . C35 . C37 . 118.5(3) yes C36 . C35 . C37 . 120.4(3) yes C35 . C36 . H361 . 109.7 no C35 . C36 . H363 . 109.4 no H361 . C36 . H363 . 109.4 no C35 . C36 . H362 . 110.1 no H361 . C36 . H362 . 110.1 no H363 . C36 . H362 . 108.1 no C35 . C37 . C38 . 122.2(3) yes C35 . C37 . H371 . 117.8 no C38 . C37 . H371 . 119.9 no C37 . C38 . C39 . 121.0(4) yes C37 . C38 . C40 . 118.0(3) yes C39 . C38 . C40 . 120.9(4) yes C38 . C39 . H391 . 110.2 no C38 . C39 . H392 . 109.7 no H391 . C39 . H392 . 109.1 no C38 . C39 . H393 . 110.4 no H391 . C39 . H393 . 109.3 no H392 . C39 . H393 . 108.1 no C38 . C40 . C41 . 121.8(3) yes C38 . C40 . H401 . 117.7 no C41 . C40 . H401 . 120.5 no C40 . C41 . C34 . 118.7(3) yes C40 . C41 . C42 . 119.3(3) yes C34 . C41 . C42 . 122.0(3) yes C41 . C42 . H422 . 109.5 no C41 . C42 . H421 . 107.9 no H422 . C42 . H421 . 109.7 no C41 . C42 . H423 . 109.9 no H422 . C42 . H423 . 110.7 no H421 . C42 . H423 . 109.0 no _iucr_refine_instruction_details_constraints ; # # Punched on 21/06/12 at 14:27:42 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 11,X'S) H ( 111,X'S) H ( 113,X'S) H ( 112,X'S) RIDE C ( 12,X'S) H ( 122,X'S) H ( 121,X'S) H ( 123,X'S) RIDE C ( 13,X'S) H ( 133,X'S) H ( 131,X'S) H ( 132,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 ( 153,X'S) H ( 151,X'S) H ( 152,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 25,X'S) H ( 251,X'S) H ( 253,X'S) H ( 252,X'S) RIDE C ( 26,X'S) H ( 261,X'S) RIDE C ( 28,X'S) H ( 281,X'S) H ( 282,X'S) H ( 283,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 31,X'S) H ( 312,X'S) H ( 313,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 323,X'S) H ( 322,X'S) RIDE C ( 33,X'S) H ( 332,X'S) H ( 331,X'S) H ( 333,X'S) RIDE C ( 36,X'S) H ( 361,X'S) H ( 363,X'S) H ( 362,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 39,X'S) H ( 391,X'S) H ( 392,X'S) H ( 393,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 42,X'S) H ( 422,X'S) H ( 421,X'S) H ( 423,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 21/06/12 at 14:27:42 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; data_4 _database_code_depnum_ccdc_archive 'CCDC 908737' #TrackingRef '4.cif' _audit_creation_date 12-07-13 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 063efnp12 _chemical_name_systematic . _chemical_melting_point . _cell_length_a 12.1918(3) _cell_length_b 16.3393(4) _cell_length_c 17.0192(5) _cell_angle_alpha 87.9149(9) _cell_angle_beta 87.6232(9) _cell_angle_gamma 78.9774(10) _cell_volume 3323.51(15) _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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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 2 # Given Formula = C67 H56 B2 F24 Fe1 N2 O2 # Dc = 1.45 Fooo = 1480.00 Mu = 3.40 M = 1454.61 # Found Formula = C67 H56 B2 F24 Fe1 N2 O2 # Dc = 1.45 FOOO = 1480.00 Mu = 3.40 M = 1454.61 _chemical_formula_sum 'C67 H56 B2 F24 Fe1 N2 O2' _chemical_formula_moiety 'C32 H12 B F24, C35 H44 B Fe N2 O2' _chemical_compound_source . _chemical_formula_weight 1454.61 _cell_measurement_reflns_used 13511 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.340 # Sheldrick geometric approximatio 0.93 0.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.93 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 50955 _reflns_number_total 14458 _diffrn_reflns_av_R_equivalents 0.036 # Number of reflections without Friedels Law is 25519 # Number of reflections with Friedels Law is 14458 # Theoretical number of reflections is about 14612 _diffrn_reflns_theta_min 5.121 _diffrn_reflns_theta_max 27.066 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.171 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -20 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 2.76 _oxford_diffrn_Wilson_scale 12.53 _atom_sites_solution_primary Direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.89 _refine_diff_density_max 1.02 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 14457 _refine_ls_number_restraints 648 _refine_ls_number_parameters 995 _oxford_refine_ls_R_factor_ref 0.1026 _refine_ls_wR_factor_ref 0.1827 _refine_ls_goodness_of_fit_ref 0.8912 _refine_ls_shift/su_max 0.0096230 _refine_ls_shift/su_mean 0.0001931 # The values computed from all data _oxford_reflns_number_all 14458 _refine_ls_R_factor_all 0.1026 _refine_ls_wR_factor_all 0.1827 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10180 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_gt 0.1546 # 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 noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 18.5 26.1 11.8 2.71 ; # Insert your own references if required - in alphabetical order 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 F600 F 0.4323(6) 0.0691(4) 0.1038(3) 0.0703 0.707(14) Uani D . P 4 1 . F601 F 0.4816(5) 0.0949(5) -0.0145(3) 0.0793 0.707(14) Uani D . P 4 1 . F602 F 0.3368(4) 0.1702(3) 0.0385(5) 0.0740 0.707(14) Uani D . P 4 1 . F603 F 0.4785(13) 0.0538(4) 0.0803(9) 0.0784 0.293(14) Uani D . P 4 2 . F604 F 0.4534(12) 0.1271(9) -0.0254(4) 0.0634 0.293(14) Uani D . P 4 2 . F605 F 0.3326(5) 0.1473(10) 0.0686(8) 0.0699 0.293(14) Uani D . P 4 2 . F500 F 0.6388(10) 0.5490(5) 0.0278(5) 0.0761 0.53(2) Uani D . P 3 1 . F501 F 0.6228(11) 0.6741(6) 0.0676(5) 0.0756 0.53(2) Uani D . P 3 1 . F502 F 0.4786(6) 0.6313(8) 0.0296(5) 0.0641 0.53(2) Uani D . P 3 1 . F503 F 0.6708(7) 0.5720(8) 0.0398(5) 0.0715 0.47(2) Uani D . P 3 2 . F504 F 0.5754(13) 0.6900(4) 0.0741(5) 0.0723 0.47(2) Uani D . P 3 2 . F505 F 0.4974(8) 0.6027(7) 0.0164(5) 0.0633 0.47(2) Uani D . P 3 2 . F400 F 0.4542(10) 0.1289(6) 0.5118(6) 0.0730 0.320(12) Uani D . P 2 1 . F401 F 0.6073(7) 0.0597(5) 0.4681(8) 0.0584 0.320(12) Uani D . P 2 1 . F402 F 0.4655(11) 0.0863(6) 0.3952(6) 0.0665 0.320(12) Uani D . P 2 1 . F403 F 0.5077(6) 0.1263(3) 0.5275(2) 0.0658 0.680(12) Uani D . P 2 2 . F404 F 0.5922(5) 0.0484(3) 0.4375(4) 0.0693 0.680(12) Uani D . P 2 2 . F405 F 0.4227(5) 0.1073(4) 0.4245(4) 0.0800 0.680(12) Uani D . P 2 2 . F300 F 0.4510(8) 0.7291(3) 0.3338(4) 0.0832 0.437(8) Uani D . P 1 1 . F301 F 0.5690(6) 0.6424(5) 0.3963(5) 0.0923 0.437(8) Uani D . P 1 1 . F302 F 0.3991(8) 0.6367(5) 0.4062(5) 0.0890 0.437(8) Uani D . P 1 1 . F303 F 0.5199(6) 0.7168(4) 0.3503(4) 0.0932 0.563(8) Uani D . P 1 2 . F304 F 0.5133(7) 0.6108(3) 0.4220(3) 0.0870 0.563(8) Uani D . P 1 2 . F305 F 0.3673(4) 0.6756(5) 0.3678(4) 0.0853 0.563(8) Uani D . P 1 2 . Fe1 Fe -0.12816(4) 0.89872(3) 0.24361(3) 0.0324 1.0000 Uani . . . . . . B2 B 0.0381(3) 0.8357(2) 0.2229(2) 0.0278 1.0000 Uani . . . . . . N3 N 0.0707(2) 0.74391(17) 0.20978(17) 0.0273 1.0000 Uani . . . . . . C4 C -0.0065(3) 0.6869(2) 0.2288(2) 0.0278 1.0000 Uani . . . . . . C5 C -0.0611(3) 0.6574(2) 0.1690(2) 0.0318 1.0000 Uani . . . . . . C6 C -0.0498(4) 0.6841(3) 0.0840(2) 0.0424 1.0000 Uani . . . . . . C7 C -0.1289(3) 0.5991(2) 0.1900(2) 0.0363 1.0000 Uani . . . . . . C8 C -0.1411(3) 0.5712(2) 0.2674(2) 0.0343 1.0000 Uani . . . . . . C9 C -0.0826(3) 0.6009(2) 0.3247(2) 0.0340 1.0000 Uani . . . . . . C10 C -0.0132(3) 0.6580(2) 0.3071(2) 0.0311 1.0000 Uani . . . . . . C11 C 0.0556(4) 0.6841(3) 0.3686(2) 0.0431 1.0000 Uani . . . . . . C12 C -0.2123(3) 0.5071(3) 0.2884(3) 0.0475 1.0000 Uani . . . . . . C13 C 0.1736(3) 0.7046(2) 0.1842(2) 0.0325 1.0000 Uani . . . . . . C14 C 0.2557(3) 0.7505(2) 0.1655(2) 0.0364 1.0000 Uani . . . . . . C15 C 0.2400(3) 0.8341(2) 0.1806(2) 0.0339 1.0000 Uani . . . . . . N16 N 0.1395(3) 0.87492(17) 0.20955(17) 0.0300 1.0000 Uani . . . . . . C17 C 0.1439(3) 0.9585(2) 0.2368(2) 0.0317 1.0000 Uani . . . . . . C18 C 0.1832(3) 0.9622(2) 0.3123(2) 0.0334 1.0000 Uani . . . . . . C19 C 0.2206(4) 0.8850(2) 0.3632(2) 0.0419 1.0000 Uani . . . . . . C20 C 0.1969(3) 1.0396(2) 0.3382(2) 0.0382 1.0000 Uani . . . . . . C21 C 0.1743(3) 1.1114(2) 0.2904(3) 0.0416 1.0000 Uani . . . . . . C22 C 0.1428(4) 1.1035(2) 0.2146(3) 0.0438 1.0000 Uani . . . . . . C23 C 0.1289(4) 1.0274(2) 0.1851(2) 0.0399 1.0000 Uani . . . . . . C24 C 0.1097(5) 1.0229(3) 0.0986(3) 0.0566 1.0000 Uani . . . . . . C25 C 0.1837(4) 1.1951(3) 0.3209(3) 0.0576 1.0000 Uani . . . . . . C26 C 0.3372(4) 0.8785(3) 0.1666(3) 0.0466 1.0000 Uani . . . . . . C27 C 0.2020(3) 0.6115(2) 0.1771(3) 0.0440 1.0000 Uani . . . . . . C28 C -0.2074(4) 0.8812(3) 0.3564(2) 0.0428 1.0000 Uani . . . . . . C29 C -0.1271(3) 0.9319(3) 0.3660(2) 0.0411 1.0000 Uani . . . . . . C30 C -0.1543(3) 1.0043(2) 0.3188(3) 0.0418 1.0000 Uani . . . . . . C31 C -0.2542(3) 1.0005(2) 0.2797(3) 0.0416 1.0000 Uani . . . . . . C32 C -0.2891(3) 0.9259(3) 0.3034(3) 0.0416 1.0000 Uani . . . . . . C33 C -0.3979(4) 0.9023(4) 0.2847(3) 0.0633 1.0000 Uani . . . . . . C34 C -0.3189(5) 1.0679(3) 0.2280(4) 0.0701 1.0000 Uani . . . . . . C35 C -0.1020(4) 1.0806(3) 0.3182(4) 0.0646 1.0000 Uani . . . . . . C36 C -0.0443(4) 0.9204(4) 0.4312(3) 0.0578 1.0000 Uani . . . . . . C37 C -0.2187(5) 0.8040(3) 0.4040(3) 0.0614 1.0000 Uani . . . . . . C38 C -0.1155(4) 0.9499(4) 0.1536(3) 0.0593 1.0000 Uani . . . . . . O39 O -0.1207(4) 0.9857(4) 0.0942(3) 0.1098 1.0000 Uani . . . . . . C40 C -0.1903(4) 0.8263(3) 0.1979(4) 0.0634 1.0000 Uani . . . . . . O41 O -0.2491(3) 0.7903(3) 0.1672(3) 0.1058 1.0000 Uani . . . . . . F42 F -0.0289(2) 0.4050(2) 0.15317(18) 0.0662 1.0000 Uani . . . . . . C43 C 0.0802(3) 0.3961(3) 0.1349(2) 0.0410 1.0000 Uani . . . . . . F44 F 0.0907(3) 0.4554(2) 0.08073(18) 0.0736 1.0000 Uani . . . . . . F45 F 0.1079(3) 0.32370(18) 0.09888(16) 0.0638 1.0000 Uani . . . . . . C46 C 0.1503(3) 0.3988(2) 0.2046(2) 0.0302 1.0000 Uani . . . . . . C47 C 0.2667(3) 0.3851(2) 0.1924(2) 0.0287 1.0000 Uani . . . . . . C48 C 0.3390(3) 0.37753(19) 0.25536(19) 0.0251 1.0000 Uani . . . . . . C49 C 0.2877(3) 0.3891(2) 0.33034(19) 0.0268 1.0000 Uani . . . . . . C50 C 0.1724(3) 0.4053(2) 0.3422(2) 0.0277 1.0000 Uani . . . . . . C51 C 0.1017(3) 0.4089(2) 0.2795(2) 0.0309 1.0000 Uani . . . . . . C52 C 0.1254(3) 0.4153(2) 0.4248(2) 0.0365 1.0000 Uani . . . . . . F53 F 0.0152(2) 0.4235(2) 0.43054(16) 0.0636 1.0000 Uani . . . . . . F54 F 0.1666(3) 0.3510(2) 0.47074(17) 0.0876 1.0000 Uani . . . . . . F55 F 0.1479(3) 0.4823(2) 0.45697(18) 0.0775 1.0000 Uani . . . . . . B56 B 0.4750(3) 0.3629(2) 0.2430(2) 0.0250 1.0000 Uani . . . . . . C57 C 0.5241(3) 0.3019(2) 0.1701(2) 0.0287 1.0000 Uani . . . . . . C58 C 0.4653(3) 0.2448(2) 0.1398(2) 0.0313 1.0000 Uani . . . . . . C59 C 0.5128(4) 0.1886(2) 0.0824(2) 0.0387 1.0000 Uani . . . . . . C60 C 0.6217(4) 0.1858(2) 0.0544(2) 0.0440 1.0000 Uani . . . . . . C61 C 0.6828(3) 0.2400(2) 0.0849(2) 0.0374 1.0000 Uani . . . . . . C62 C 0.6341(3) 0.2971(2) 0.1414(2) 0.0310 1.0000 Uani . . . . . . C63 C 0.8015(4) 0.2395(3) 0.0587(3) 0.0527 1.0000 Uani . . . . . . F64 F 0.8408(3) 0.1815(2) 0.00578(18) 0.0700 1.0000 Uani . . . . . . F65 F 0.8708(2) 0.2250(3) 0.11794(19) 0.0839 1.0000 Uani . . . . . . F66 F 0.8147(3) 0.3119(2) 0.0253(2) 0.0916 1.0000 Uani . . . . . . C67 C 0.4424(3) 0.13152(18) 0.05272(18) 0.0639 1.0000 Uani D . . . . . C71 C 0.5013(3) 0.4571(2) 0.2307(2) 0.0284 1.0000 Uani . . . . . . C72 C 0.5296(3) 0.4919(2) 0.1582(2) 0.0323 1.0000 Uani . . . . . . C73 C 0.5442(3) 0.5749(2) 0.1500(2) 0.0394 1.0000 Uani . . . . . . C74 C 0.5298(3) 0.6264(2) 0.2136(3) 0.0417 1.0000 Uani . . . . . . C75 C 0.4985(3) 0.5944(2) 0.2858(3) 0.0385 1.0000 Uani . . . . . . C76 C 0.4852(3) 0.5119(2) 0.2943(2) 0.0321 1.0000 Uani . . . . . . C77 C 0.4774(3) 0.6489(2) 0.35487(19) 0.0706 1.0000 Uani D . . . . . C81 C 0.5720(3) 0.60806(19) 0.07038(14) 0.0607 1.0000 Uani D . . . . . C85 C 0.5372(3) 0.3134(2) 0.31917(19) 0.0271 1.0000 Uani . . . . . . C86 C 0.5008(3) 0.2431(2) 0.3537(2) 0.0319 1.0000 Uani . . . . . . C87 C 0.5592(3) 0.1946(2) 0.4127(2) 0.0365 1.0000 Uani . . . . . . C88 C 0.6578(3) 0.2127(2) 0.4391(2) 0.0374 1.0000 Uani . . . . . . C89 C 0.6963(3) 0.2802(2) 0.4054(2) 0.0340 1.0000 Uani . . . . . . C90 C 0.6369(3) 0.3298(2) 0.3468(2) 0.0299 1.0000 Uani . . . . . . C91 C 0.8047(4) 0.3006(3) 0.4296(3) 0.0451 1.0000 Uani . . . . . . F92 F 0.7912(2) 0.37532(17) 0.46162(17) 0.0601 1.0000 Uani . . . . . . F93 F 0.8769(2) 0.30258(19) 0.36814(18) 0.0609 1.0000 Uani . . . . . . F94 F 0.8573(3) 0.24467(19) 0.4815(2) 0.0736 1.0000 Uani . . . . . . C95 C 0.5209(3) 0.11994(15) 0.44878(18) 0.0577 1.0000 Uani D . . . . . H61 H -0.1198 0.6856 0.0586 0.0660 1.0000 Uiso . . . . . . H63 H -0.0300 0.7387 0.0793 0.0664 1.0000 Uiso . . . . . . H62 H 0.0080 0.6450 0.0566 0.0667 1.0000 Uiso . . . . . . H71 H -0.1678 0.5780 0.1489 0.0450 1.0000 Uiso . . . . . . H91 H -0.0894 0.5810 0.3779 0.0415 1.0000 Uiso . . . . . . H111 H 0.0352 0.6633 0.4204 0.0678 1.0000 Uiso . . . . . . H112 H 0.0458 0.7446 0.3699 0.0679 1.0000 Uiso . . . . . . H113 H 0.1349 0.6613 0.3573 0.0677 1.0000 Uiso . . . . . . H122 H -0.2559 0.5218 0.3364 0.0767 1.0000 Uiso . . . . . . H121 H -0.2632 0.5042 0.2471 0.0765 1.0000 Uiso . . . . . . H123 H -0.1659 0.4524 0.2961 0.0769 1.0000 Uiso . . . . . . H141 H 0.3249 0.7235 0.1419 0.0457 1.0000 Uiso . . . . . . H191 H 0.2257 0.9002 0.4173 0.0664 1.0000 Uiso . . . . . . H192 H 0.2948 0.8564 0.3451 0.0664 1.0000 Uiso . . . . . . H193 H 0.1693 0.8457 0.3631 0.0658 1.0000 Uiso . . . . . . H201 H 0.2225 1.0426 0.3900 0.0478 1.0000 Uiso . . . . . . H221 H 0.1287 1.1532 0.1796 0.0534 1.0000 Uiso . . . . . . H241 H 0.0392 1.0590 0.0847 0.0882 1.0000 Uiso . . . . . . H243 H 0.1709 1.0404 0.0680 0.0881 1.0000 Uiso . . . . . . H242 H 0.1070 0.9657 0.0838 0.0878 1.0000 Uiso . . . . . . H251 H 0.2156 1.2266 0.2804 0.0893 1.0000 Uiso . . . . . . H252 H 0.2317 1.1872 0.3665 0.0895 1.0000 Uiso . . . . . . H253 H 0.1104 1.2257 0.3362 0.0891 1.0000 Uiso . . . . . . H261 H 0.3143 0.9267 0.1321 0.0732 1.0000 Uiso . . . . . . H262 H 0.3590 0.8975 0.2166 0.0729 1.0000 Uiso . . . . . . H263 H 0.4000 0.8419 0.1430 0.0731 1.0000 Uiso . . . . . . H271 H 0.2811 0.5938 0.1635 0.0683 1.0000 Uiso . . . . . . H272 H 0.1843 0.5845 0.2270 0.0683 1.0000 Uiso . . . . . . H273 H 0.1577 0.5944 0.1363 0.0684 1.0000 Uiso . . . . . . H332 H -0.4143 0.9192 0.2282 0.0991 1.0000 Uiso . . . . . . H331 H -0.4578 0.9309 0.3191 0.0993 1.0000 Uiso . . . . . . H333 H -0.3912 0.8412 0.2910 0.0993 1.0000 Uiso . . . . . . H342 H -0.3600 1.0430 0.1910 0.1076 1.0000 Uiso . . . . . . H341 H -0.3701 1.1064 0.2620 0.1074 1.0000 Uiso . . . . . . H343 H -0.2660 1.0982 0.2000 0.1073 1.0000 Uiso . . . . . . H351 H -0.0994 1.1034 0.2637 0.1027 1.0000 Uiso . . . . . . H353 H -0.1469 1.1222 0.3516 0.1023 1.0000 Uiso . . . . . . H352 H -0.0249 1.0656 0.3377 0.1023 1.0000 Uiso . . . . . . H361 H 0.0177 0.9510 0.4179 0.0893 1.0000 Uiso . . . . . . H363 H -0.0838 0.9404 0.4804 0.0893 1.0000 Uiso . . . . . . H362 H -0.0141 0.8597 0.4372 0.0893 1.0000 Uiso . . . . . . H371 H -0.2446 0.7654 0.3683 0.0976 1.0000 Uiso . . . . . . H372 H -0.2742 0.8185 0.4474 0.0973 1.0000 Uiso . . . . . . H373 H -0.1455 0.7786 0.4250 0.0973 1.0000 Uiso . . . . . . H471 H 0.2963 0.3802 0.1393 0.0364 1.0000 Uiso . . . . . . H491 H 0.3335 0.3857 0.3756 0.0333 1.0000 Uiso . . . . . . H511 H 0.0220 0.4183 0.2881 0.0388 1.0000 Uiso . . . . . . H581 H 0.3896 0.2433 0.1589 0.0395 1.0000 Uiso . . . . . . H601 H 0.6551 0.1469 0.0145 0.0546 1.0000 Uiso . . . . . . H621 H 0.6783 0.3339 0.1617 0.0392 1.0000 Uiso . . . . . . H721 H 0.5404 0.4578 0.1120 0.0410 1.0000 Uiso . . . . . . H741 H 0.5409 0.6821 0.2085 0.0514 1.0000 Uiso . . . . . . H761 H 0.4638 0.4915 0.3454 0.0406 1.0000 Uiso . . . . . . H861 H 0.4326 0.2282 0.3362 0.0396 1.0000 Uiso . . . . . . H881 H 0.6988 0.1792 0.4797 0.0461 1.0000 Uiso . . . . . . H901 H 0.6658 0.3771 0.3249 0.0376 1.0000 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 F600 0.091(3) 0.059(3) 0.071(3) -0.001(2) 0.012(3) -0.045(2) F601 0.108(4) 0.069(3) 0.072(3) -0.041(2) 0.029(3) -0.042(3) F602 0.080(3) 0.063(3) 0.088(4) -0.014(3) -0.014(2) -0.031(2) F603 0.110(6) 0.051(4) 0.081(5) -0.009(4) 0.000(5) -0.032(4) F604 0.085(5) 0.057(5) 0.057(4) -0.010(4) -0.009(4) -0.033(4) F605 0.083(4) 0.061(5) 0.075(5) -0.025(4) 0.027(4) -0.041(4) F500 0.090(4) 0.068(4) 0.070(4) 0.028(3) 0.029(3) -0.028(3) F501 0.093(4) 0.082(4) 0.068(4) 0.030(3) -0.013(3) -0.060(3) F502 0.081(3) 0.067(4) 0.044(3) 0.013(3) -0.018(3) -0.012(3) F503 0.075(4) 0.084(4) 0.062(4) 0.030(3) 0.010(3) -0.041(3) F504 0.102(5) 0.060(3) 0.064(4) 0.026(3) -0.007(4) -0.044(3) F505 0.094(4) 0.057(4) 0.046(3) 0.010(3) -0.021(3) -0.031(3) F400 0.066(5) 0.066(4) 0.089(5) 0.016(4) 0.024(4) -0.027(4) F401 0.064(4) 0.039(4) 0.075(5) 0.021(4) -0.021(4) -0.018(3) F402 0.066(5) 0.059(4) 0.084(5) 0.025(4) -0.001(4) -0.039(4) F403 0.069(3) 0.074(3) 0.059(2) 0.019(2) 0.014(2) -0.033(2) F404 0.087(3) 0.034(2) 0.084(4) 0.004(2) 0.023(3) -0.011(2) F405 0.066(3) 0.081(3) 0.104(4) 0.050(3) -0.023(3) -0.046(3) F300 0.107(5) 0.037(3) 0.102(4) -0.031(3) -0.014(4) 0.005(3) F301 0.106(5) 0.081(4) 0.089(5) -0.048(4) -0.016(4) -0.004(4) F302 0.119(5) 0.068(4) 0.090(5) -0.035(4) 0.042(4) -0.046(4) F303 0.128(5) 0.065(3) 0.104(4) -0.038(3) 0.030(4) -0.061(3) F304 0.131(5) 0.057(3) 0.070(3) -0.030(3) -0.017(3) -0.001(3) F305 0.084(3) 0.080(4) 0.083(4) -0.027(3) 0.017(3) 0.007(3) Fe1 0.0333(3) 0.0295(3) 0.0327(3) -0.0011(2) -0.0038(2) -0.0011(2) B2 0.0306(19) 0.0256(18) 0.0271(18) 0.0019(14) -0.0028(15) -0.0051(15) N3 0.0266(14) 0.0263(14) 0.0296(14) -0.0007(11) -0.0004(11) -0.0068(11) C4 0.0300(17) 0.0216(15) 0.0319(17) -0.0006(13) 0.0009(13) -0.0051(13) C5 0.0315(18) 0.0355(18) 0.0292(17) -0.0039(14) -0.0015(14) -0.0079(14) C6 0.049(2) 0.051(2) 0.0308(19) -0.0016(17) -0.0009(17) -0.0173(19) C7 0.0338(19) 0.0369(19) 0.041(2) -0.0022(16) -0.0023(16) -0.0128(15) C8 0.0281(17) 0.0253(16) 0.049(2) 0.0024(15) -0.0002(15) -0.0043(13) C9 0.0351(19) 0.0316(18) 0.0337(18) 0.0065(14) 0.0011(15) -0.0043(14) C10 0.0362(18) 0.0257(16) 0.0298(17) 0.0005(13) -0.0038(14) -0.0020(14) C11 0.056(3) 0.044(2) 0.0330(19) 0.0014(16) -0.0117(18) -0.0163(19) C12 0.031(2) 0.044(2) 0.070(3) 0.012(2) -0.0023(19) -0.0146(17) C13 0.0311(18) 0.0283(17) 0.0389(19) -0.0016(14) -0.0007(15) -0.0072(14) C14 0.0304(18) 0.0337(19) 0.045(2) -0.0040(16) 0.0040(15) -0.0060(15) C15 0.0360(19) 0.0340(18) 0.0331(18) -0.0003(14) 0.0025(15) -0.0115(15) N16 0.0355(16) 0.0246(14) 0.0305(15) 0.0006(11) -0.0009(12) -0.0080(12) C17 0.0346(18) 0.0250(16) 0.0372(19) 0.0014(14) -0.0013(15) -0.0104(14) C18 0.0362(19) 0.0268(17) 0.0382(19) 0.0007(14) -0.0034(15) -0.0085(14) C19 0.054(2) 0.0337(19) 0.039(2) 0.0049(16) -0.0119(18) -0.0092(17) C20 0.043(2) 0.0334(19) 0.040(2) -0.0038(16) 0.0000(16) -0.0125(16) C21 0.039(2) 0.0277(18) 0.061(3) -0.0023(17) 0.0012(18) -0.0131(16) C22 0.050(2) 0.0272(18) 0.056(3) 0.0063(17) -0.0011(19) -0.0136(17) C23 0.047(2) 0.0334(19) 0.041(2) 0.0054(16) -0.0052(17) -0.0107(16) C24 0.083(4) 0.050(3) 0.040(2) 0.013(2) -0.011(2) -0.021(2) C25 0.062(3) 0.032(2) 0.083(4) -0.010(2) 0.000(3) -0.020(2) C26 0.042(2) 0.045(2) 0.056(3) -0.0058(19) 0.0105(19) -0.0185(18) C27 0.035(2) 0.0285(19) 0.068(3) -0.0076(18) 0.0066(19) -0.0051(15) C28 0.049(2) 0.036(2) 0.041(2) 0.0032(17) 0.0065(18) -0.0059(17) C29 0.038(2) 0.047(2) 0.036(2) -0.0095(17) 0.0020(16) -0.0005(17) C30 0.039(2) 0.034(2) 0.052(2) -0.0110(17) 0.0108(18) -0.0051(16) C31 0.038(2) 0.0332(19) 0.048(2) 0.0019(17) 0.0095(17) 0.0046(16) C32 0.0329(19) 0.041(2) 0.050(2) -0.0014(18) 0.0031(17) -0.0061(16) C33 0.038(2) 0.077(4) 0.076(4) -0.007(3) 0.005(2) -0.015(2) C34 0.064(3) 0.054(3) 0.078(4) 0.022(3) 0.009(3) 0.016(2) C35 0.057(3) 0.041(2) 0.096(4) -0.022(3) 0.017(3) -0.012(2) C36 0.054(3) 0.081(3) 0.037(2) -0.014(2) -0.005(2) -0.006(2) C37 0.066(3) 0.052(3) 0.062(3) 0.019(2) 0.014(2) -0.008(2) C38 0.048(3) 0.080(3) 0.040(2) 0.013(2) -0.002(2) 0.009(2) O39 0.074(3) 0.184(5) 0.057(2) 0.058(3) -0.003(2) 0.000(3) C40 0.039(2) 0.057(3) 0.091(4) -0.032(3) -0.017(2) 0.008(2) O41 0.051(2) 0.090(3) 0.176(5) -0.077(3) -0.042(3) 0.009(2) F42 0.0372(14) 0.095(2) 0.0681(18) -0.0235(16) -0.0167(13) -0.0089(14) C43 0.040(2) 0.041(2) 0.042(2) -0.0035(17) -0.0139(17) -0.0032(17) F44 0.094(2) 0.075(2) 0.0597(17) 0.0280(15) -0.0457(17) -0.0327(17) F45 0.0714(19) 0.0620(17) 0.0554(16) -0.0279(13) -0.0274(14) 0.0041(14) C46 0.0305(17) 0.0237(16) 0.0363(18) -0.0024(13) -0.0086(14) -0.0032(13) C47 0.0326(17) 0.0269(16) 0.0269(16) -0.0016(13) -0.0019(13) -0.0061(13) C48 0.0268(16) 0.0209(14) 0.0275(16) -0.0008(12) -0.0006(12) -0.0044(12) C49 0.0287(16) 0.0247(15) 0.0275(16) -0.0010(12) 0.0002(13) -0.0061(13) C50 0.0309(17) 0.0203(15) 0.0323(17) -0.0036(13) 0.0025(14) -0.0059(13) C51 0.0292(17) 0.0264(16) 0.0372(19) -0.0021(14) 0.0015(14) -0.0054(13) C52 0.0310(18) 0.041(2) 0.038(2) -0.0046(16) 0.0064(15) -0.0075(15) F53 0.0382(14) 0.100(2) 0.0525(16) -0.0086(15) 0.0166(12) -0.0152(14) F54 0.108(3) 0.086(2) 0.0422(15) 0.0246(15) 0.0278(16) 0.038(2) F55 0.098(2) 0.086(2) 0.0614(18) -0.0451(17) 0.0341(17) -0.0505(19) B56 0.0259(17) 0.0254(17) 0.0237(17) -0.0001(14) -0.0012(14) -0.0047(14) C57 0.0329(18) 0.0242(16) 0.0278(16) 0.0041(13) -0.0005(13) -0.0029(13) C58 0.0379(19) 0.0241(16) 0.0313(17) -0.0010(13) 0.0035(14) -0.0053(14) C59 0.054(2) 0.0274(18) 0.0337(19) -0.0010(15) 0.0050(17) -0.0075(16) C60 0.060(3) 0.0328(19) 0.035(2) -0.0005(16) 0.0094(18) -0.0003(18) C61 0.038(2) 0.0368(19) 0.0329(19) 0.0039(15) 0.0076(15) 0.0016(16) C62 0.0321(18) 0.0312(17) 0.0281(17) 0.0017(14) 0.0022(14) -0.0033(14) C63 0.049(3) 0.053(3) 0.050(3) -0.002(2) 0.015(2) 0.002(2) F64 0.0595(18) 0.078(2) 0.0625(18) -0.0166(15) 0.0231(14) 0.0104(15) F65 0.0398(15) 0.147(3) 0.0604(19) -0.016(2) 0.0060(14) -0.0062(18) F66 0.071(2) 0.066(2) 0.130(3) 0.014(2) 0.059(2) -0.0082(16) C67 0.086(2) 0.050(2) 0.064(2) -0.0186(17) 0.011(2) -0.0312(19) C71 0.0241(16) 0.0273(16) 0.0335(18) 0.0019(13) -0.0033(13) -0.0043(13) C72 0.0316(18) 0.0314(18) 0.0345(18) 0.0082(14) -0.0073(14) -0.0076(14) C73 0.036(2) 0.0354(19) 0.048(2) 0.0171(17) -0.0105(17) -0.0109(16) C74 0.036(2) 0.0263(18) 0.065(3) 0.0070(17) -0.0122(18) -0.0100(15) C75 0.0342(19) 0.0263(17) 0.055(2) -0.0044(16) -0.0014(17) -0.0049(14) C76 0.0278(17) 0.0297(17) 0.0386(19) -0.0015(14) 0.0023(14) -0.0060(14) C77 0.092(3) 0.0451(19) 0.080(2) -0.0282(19) 0.009(2) -0.0222(19) C81 0.079(2) 0.059(2) 0.052(2) 0.0219(17) -0.0108(17) -0.0348(18) C85 0.0273(16) 0.0271(16) 0.0268(16) -0.0012(13) 0.0014(13) -0.0052(13) C86 0.0273(17) 0.0307(17) 0.0375(19) 0.0051(14) -0.0011(14) -0.0056(14) C87 0.040(2) 0.0309(18) 0.037(2) 0.0087(15) 0.0002(16) -0.0061(15) C88 0.040(2) 0.0365(19) 0.0343(19) 0.0069(15) -0.0077(16) -0.0038(16) C89 0.0367(19) 0.0356(19) 0.0308(18) 0.0018(14) -0.0097(15) -0.0081(15) C90 0.0309(17) 0.0286(16) 0.0307(17) 0.0015(13) -0.0022(14) -0.0071(13) C91 0.046(2) 0.043(2) 0.048(2) 0.0075(18) -0.0213(19) -0.0102(18) F92 0.0652(17) 0.0532(15) 0.0684(18) -0.0100(13) -0.0238(14) -0.0218(13) F93 0.0360(13) 0.0746(19) 0.0759(19) -0.0029(15) -0.0098(13) -0.0182(13) F94 0.076(2) 0.0617(18) 0.090(2) 0.0276(16) -0.0552(18) -0.0249(15) C95 0.060(2) 0.0474(18) 0.069(2) 0.0230(17) -0.0025(17) -0.0211(16) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3242(3) 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 F600 . C67 . 1.336(4) yes F601 . C67 . 1.338(4) yes F602 . C67 . 1.349(4) yes F603 . C67 . 1.337(6) yes F604 . C67 . 1.334(6) yes F605 . C67 . 1.332(6) yes F500 . C81 . 1.349(5) yes F501 . C81 . 1.342(5) yes F502 . C81 . 1.343(5) yes F503 . C81 . 1.329(5) yes F504 . C81 . 1.351(5) yes F505 . C81 . 1.337(5) yes F400 . C95 . 1.315(5) yes F401 . C95 . 1.340(5) yes F402 . C95 . 1.349(5) yes F403 . C95 . 1.348(4) yes F404 . C95 . 1.331(4) yes F405 . C95 . 1.337(4) yes F300 . C77 . 1.329(5) yes F301 . C77 . 1.331(5) yes F302 . C77 . 1.307(5) yes F303 . C77 . 1.310(5) yes F304 . C77 . 1.330(5) yes F305 . C77 . 1.342(5) yes Fe1 . B2 . 2.113(4) yes Fe1 . C28 . 2.147(4) yes Fe1 . C29 . 2.173(4) yes Fe1 . C30 . 2.152(4) yes Fe1 . C31 . 2.127(4) yes Fe1 . C32 . 2.148(4) yes Fe1 . C38 . 1.734(5) yes Fe1 . C40 . 1.742(5) yes B2 . N3 . 1.498(5) yes B2 . N16 . 1.503(5) yes N3 . C4 . 1.465(4) yes N3 . C13 . 1.358(4) yes C4 . C5 . 1.386(5) yes C4 . C10 . 1.401(5) yes C5 . C6 . 1.505(5) yes C5 . C7 . 1.404(5) yes C6 . H61 . 0.968 no C6 . H63 . 0.967 no C6 . H62 . 0.972 no C7 . C8 . 1.390(5) yes C7 . H71 . 0.971 no C8 . C9 . 1.386(5) yes C8 . C12 . 1.508(5) yes C9 . C10 . 1.391(5) yes C9 . H91 . 0.956 no C10 . C11 . 1.491(5) yes C11 . H111 . 0.973 no C11 . H112 . 0.974 no C11 . H113 . 0.981 no C12 . H122 . 0.967 no C12 . H121 . 0.965 no C12 . H123 . 0.969 no C13 . C14 . 1.382(5) yes C13 . C27 . 1.502(5) yes C14 . C15 . 1.375(5) yes C14 . H141 . 0.954 no C15 . N16 . 1.360(5) yes C15 . C26 . 1.509(5) yes N16 . C17 . 1.469(4) yes C17 . C18 . 1.397(5) yes C17 . C23 . 1.392(5) yes C18 . C19 . 1.510(5) yes C18 . C20 . 1.396(5) yes C19 . H191 . 0.970 no C19 . H192 . 0.979 no C19 . H193 . 0.978 no C20 . C21 . 1.393(6) yes C20 . H201 . 0.953 no C21 . C22 . 1.379(6) yes C21 . C25 . 1.507(5) yes C22 . C23 . 1.400(6) yes C22 . H221 . 0.981 no C23 . C24 . 1.507(6) yes C24 . H241 . 0.977 no C24 . H243 . 0.974 no C24 . H242 . 0.983 no C25 . H251 . 0.959 no C25 . H252 . 0.981 no C25 . H253 . 0.967 no C26 . H261 . 0.969 no C26 . H262 . 0.981 no C26 . H263 . 0.961 no C27 . H271 . 0.972 no C27 . H272 . 0.979 no C27 . H273 . 0.977 no C28 . C29 . 1.417(6) yes C28 . C32 . 1.445(6) yes C28 . C37 . 1.499(6) yes C29 . C30 . 1.399(6) yes C29 . C36 . 1.513(6) yes C30 . C31 . 1.425(6) yes C30 . C35 . 1.505(6) yes C31 . C32 . 1.405(6) yes C31 . C34 . 1.505(6) yes C32 . C33 . 1.501(6) yes C33 . H332 . 1.009 no C33 . H331 . 0.974 no C33 . H333 . 0.988 no C34 . H342 . 0.968 no C34 . H341 . 0.982 no C34 . H343 . 0.984 no C35 . H351 . 0.988 no C35 . H353 . 0.972 no C35 . H352 . 0.993 no C36 . H361 . 0.998 no C36 . H363 . 0.983 no C36 . H362 . 0.992 no C37 . H371 . 0.994 no C37 . H372 . 0.985 no C37 . H373 . 0.985 no C38 . O39 . 1.148(6) yes C40 . O41 . 1.163(6) yes F42 . C43 . 1.336(5) yes C43 . F44 . 1.333(5) yes C43 . F45 . 1.332(5) yes C43 . C46 . 1.497(5) yes C46 . C47 . 1.401(5) yes C46 . C51 . 1.385(5) yes C47 . C48 . 1.402(5) yes C47 . H471 . 0.960 no C48 . C49 . 1.400(5) yes C48 . B56 . 1.636(5) yes C49 . C50 . 1.387(5) yes C49 . H491 . 0.964 no C50 . C51 . 1.393(5) yes C50 . C52 . 1.498(5) yes C51 . H511 . 0.960 no C52 . F53 . 1.324(4) yes C52 . F54 . 1.319(5) yes C52 . F55 . 1.321(5) yes B56 . C57 . 1.641(5) yes B56 . C71 . 1.637(5) yes B56 . C85 . 1.637(5) yes C57 . C58 . 1.405(5) yes C57 . C62 . 1.398(5) yes C58 . C59 . 1.396(5) yes C58 . H581 . 0.970 no C59 . C60 . 1.384(6) yes C59 . C67 . 1.496(4) yes C60 . C61 . 1.388(6) yes C60 . H601 . 0.970 no C61 . C62 . 1.397(5) yes C61 . C63 . 1.495(6) yes C62 . H621 . 0.962 no C63 . F64 . 1.339(5) yes C63 . F65 . 1.328(6) yes C63 . F66 . 1.328(6) yes C71 . C72 . 1.398(5) yes C71 . C76 . 1.413(5) yes C72 . C73 . 1.402(5) yes C72 . H721 . 0.970 no C73 . C74 . 1.381(6) yes C73 . C81 . 1.490(4) yes C74 . C75 . 1.385(6) yes C74 . H741 . 0.946 no C75 . C76 . 1.389(5) yes C75 . C77 . 1.485(5) yes C76 . H761 . 0.963 no C85 . C86 . 1.409(5) yes C85 . C90 . 1.396(5) yes C86 . C87 . 1.389(5) yes C86 . H861 . 0.970 no C87 . C88 . 1.388(6) yes C87 . C95 . 1.491(4) yes C88 . C89 . 1.376(5) yes C88 . H881 . 0.961 no C89 . C90 . 1.398(5) yes C89 . C91 . 1.500(5) yes C90 . H901 . 0.966 no C91 . F92 . 1.334(5) yes C91 . F93 . 1.342(5) yes C91 . F94 . 1.339(5) 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 B2 . Fe1 . C28 . 118.36(15) yes B2 . Fe1 . C29 . 102.20(15) yes C28 . Fe1 . C29 . 38.29(16) yes B2 . Fe1 . C30 . 117.53(15) yes C28 . Fe1 . C30 . 64.39(16) yes C29 . Fe1 . C30 . 37.76(16) yes B2 . Fe1 . C31 . 154.88(16) yes C28 . Fe1 . C31 . 65.04(16) yes C29 . Fe1 . C31 . 64.20(16) yes C30 . Fe1 . C31 . 38.89(16) yes B2 . Fe1 . C32 . 156.58(15) yes C28 . Fe1 . C32 . 39.30(16) yes C29 . Fe1 . C32 . 64.40(16) yes C30 . Fe1 . C32 . 64.55(16) yes C31 . Fe1 . C32 . 38.38(15) yes B2 . Fe1 . C38 . 86.86(19) yes C28 . Fe1 . C38 . 153.9(2) yes C29 . Fe1 . C38 . 135.1(2) yes C30 . Fe1 . C38 . 99.2(2) yes C31 . Fe1 . C38 . 89.3(2) yes B2 . Fe1 . C40 . 95.62(18) yes C28 . Fe1 . C40 . 94.1(2) yes C29 . Fe1 . C40 . 131.8(2) yes C30 . Fe1 . C40 . 145.9(2) yes C31 . Fe1 . C40 . 109.19(19) yes C32 . Fe1 . C38 . 116.3(2) yes C32 . Fe1 . C40 . 82.0(2) yes C38 . Fe1 . C40 . 89.7(3) yes Fe1 . B2 . N3 . 124.0(3) yes Fe1 . B2 . N16 . 126.6(2) yes N3 . B2 . N16 . 109.0(3) yes B2 . N3 . C4 . 121.7(3) yes B2 . N3 . C13 . 124.8(3) yes C4 . N3 . C13 . 113.4(3) yes N3 . C4 . C5 . 119.8(3) yes N3 . C4 . C10 . 117.3(3) yes C5 . C4 . C10 . 122.6(3) yes C4 . C5 . C6 . 123.3(3) yes C4 . C5 . C7 . 117.4(3) yes C6 . C5 . C7 . 119.3(3) yes C5 . C6 . H61 . 109.6 no C5 . C6 . H63 . 110.8 no H61 . C6 . H63 . 109.3 no C5 . C6 . H62 . 110.6 no H61 . C6 . H62 . 108.3 no H63 . C6 . H62 . 108.1 no C5 . C7 . C8 . 121.9(3) yes C5 . C7 . H71 . 118.4 no C8 . C7 . H71 . 119.8 no C7 . C8 . C9 . 118.5(3) yes C7 . C8 . C12 . 121.0(4) yes C9 . C8 . C12 . 120.5(4) yes C8 . C9 . C10 . 122.1(3) yes C8 . C9 . H91 . 118.8 no C10 . C9 . H91 . 119.1 no C4 . C10 . C9 . 117.5(3) yes C4 . C10 . C11 . 121.4(3) yes C9 . C10 . C11 . 121.0(3) yes C10 . C11 . H111 . 110.8 no C10 . C11 . H112 . 111.3 no H111 . C11 . H112 . 108.4 no C10 . C11 . H113 . 109.5 no H111 . C11 . H113 . 108.3 no H112 . C11 . H113 . 108.5 no C8 . C12 . H122 . 110.2 no C8 . C12 . H121 . 110.5 no H122 . C12 . H121 . 108.3 no C8 . C12 . H123 . 110.5 no H122 . C12 . H123 . 108.7 no H121 . C12 . H123 . 108.6 no N3 . C13 . C14 . 119.7(3) yes N3 . C13 . C27 . 121.7(3) yes C14 . C13 . C27 . 118.6(3) yes C13 . C14 . C15 . 121.4(3) yes C13 . C14 . H141 . 119.2 no C15 . C14 . H141 . 119.4 no C14 . C15 . N16 . 120.2(3) yes C14 . C15 . C26 . 118.7(3) yes N16 . C15 . C26 . 121.2(3) yes C15 . N16 . B2 . 124.2(3) yes C15 . N16 . C17 . 112.7(3) yes B2 . N16 . C17 . 122.6(3) yes N16 . C17 . C18 . 116.3(3) yes N16 . C17 . C23 . 121.0(3) yes C18 . C17 . C23 . 121.8(3) yes C17 . C18 . C19 . 122.3(3) yes C17 . C18 . C20 . 118.1(3) yes C19 . C18 . C20 . 119.3(3) yes C18 . C19 . H191 . 110.1 no C18 . C19 . H192 . 109.8 no H191 . C19 . H192 . 107.8 no C18 . C19 . H193 . 112.9 no H191 . C19 . H193 . 107.4 no H192 . C19 . H193 . 108.6 no C18 . C20 . C21 . 121.7(4) yes C18 . C20 . H201 . 118.5 no C21 . C20 . H201 . 119.9 no C20 . C21 . C22 . 118.0(3) yes C20 . C21 . C25 . 120.8(4) yes C22 . C21 . C25 . 121.2(4) yes C21 . C22 . C23 . 122.8(4) yes C21 . C22 . H221 . 119.0 no C23 . C22 . H221 . 118.2 no C22 . C23 . C17 . 117.2(4) yes C22 . C23 . C24 . 118.6(4) yes C17 . C23 . C24 . 123.9(4) yes C23 . C24 . H241 . 110.5 no C23 . C24 . H243 . 109.7 no H241 . C24 . H243 . 109.3 no C23 . C24 . H242 . 111.5 no H241 . C24 . H242 . 108.3 no H243 . C24 . H242 . 107.4 no C21 . C25 . H251 . 109.5 no C21 . C25 . H252 . 109.6 no H251 . C25 . H252 . 109.5 no C21 . C25 . H253 . 110.0 no H251 . C25 . H253 . 108.8 no H252 . C25 . H253 . 109.5 no C15 . C26 . H261 . 108.9 no C15 . C26 . H262 . 109.9 no H261 . C26 . H262 . 108.7 no C15 . C26 . H263 . 110.5 no H261 . C26 . H263 . 109.8 no H262 . C26 . H263 . 109.1 no C13 . C27 . H271 . 110.4 no C13 . C27 . H272 . 109.7 no H271 . C27 . H272 . 109.3 no C13 . C27 . H273 . 109.6 no H271 . C27 . H273 . 109.3 no H272 . C27 . H273 . 108.4 no Fe1 . C28 . C29 . 71.8(2) yes Fe1 . C28 . C32 . 70.4(2) yes C29 . C28 . C32 . 107.1(3) yes Fe1 . C28 . C37 . 131.9(3) yes C29 . C28 . C37 . 126.2(4) yes C32 . C28 . C37 . 125.6(4) yes Fe1 . C29 . C28 . 69.9(2) yes Fe1 . C29 . C30 . 70.3(2) yes C28 . C29 . C30 . 108.8(4) yes Fe1 . C29 . C36 . 137.4(3) yes C28 . C29 . C36 . 124.8(4) yes C30 . C29 . C36 . 124.7(4) yes Fe1 . C30 . C29 . 71.9(2) yes Fe1 . C30 . C31 . 69.6(2) yes C29 . C30 . C31 . 108.0(4) yes Fe1 . C30 . C35 . 131.9(3) yes C29 . C30 . C35 . 127.4(4) yes C31 . C30 . C35 . 123.8(4) yes Fe1 . C31 . C30 . 71.5(2) yes Fe1 . C31 . C32 . 71.6(2) yes C30 . C31 . C32 . 108.5(4) yes Fe1 . C31 . C34 . 127.3(3) yes C30 . C31 . C34 . 126.4(4) yes C32 . C31 . C34 . 124.9(4) yes Fe1 . C32 . C28 . 70.3(2) yes Fe1 . C32 . C31 . 70.0(2) yes C28 . C32 . C31 . 107.5(4) yes Fe1 . C32 . C33 . 130.5(3) yes C28 . C32 . C33 . 126.2(4) yes C31 . C32 . C33 . 126.0(4) yes C32 . C33 . H332 . 108.3 no C32 . C33 . H331 . 110.0 no H332 . C33 . H331 . 109.7 no C32 . C33 . H333 . 109.4 no H332 . C33 . H333 . 108.8 no H331 . C33 . H333 . 110.6 no C31 . C34 . H342 . 109.4 no C31 . C34 . H341 . 108.0 no H342 . C34 . H341 . 110.9 no C31 . C34 . H343 . 108.6 no H342 . C34 . H343 . 110.4 no H341 . C34 . H343 . 109.4 no C30 . C35 . H351 . 108.8 no C30 . C35 . H353 . 109.4 no H351 . C35 . H353 . 109.5 no C30 . C35 . H352 . 109.8 no H351 . C35 . H352 . 109.5 no H353 . C35 . H352 . 109.7 no C29 . C36 . H361 . 110.8 no C29 . C36 . H363 . 108.9 no H361 . C36 . H363 . 110.6 no C29 . C36 . H362 . 107.3 no H361 . C36 . H362 . 110.0 no H363 . C36 . H362 . 109.1 no C28 . C37 . H371 . 107.2 no C28 . C37 . H372 . 109.6 no H371 . C37 . H372 . 109.8 no C28 . C37 . H373 . 109.2 no H371 . C37 . H373 . 110.8 no H372 . C37 . H373 . 110.1 no Fe1 . C38 . O39 . 171.9(5) yes Fe1 . C40 . O41 . 167.0(4) yes F42 . C43 . F44 . 106.3(3) yes F42 . C43 . F45 . 105.6(3) yes F44 . C43 . F45 . 106.4(4) yes F42 . C43 . C46 . 113.5(3) yes F44 . C43 . C46 . 112.7(3) yes F45 . C43 . C46 . 111.7(3) yes C43 . C46 . C47 . 118.0(3) yes C43 . C46 . C51 . 120.7(3) yes C47 . C46 . C51 . 121.2(3) yes C46 . C47 . C48 . 121.7(3) yes C46 . C47 . H471 . 118.0 no C48 . C47 . H471 . 120.3 no C47 . C48 . C49 . 116.0(3) yes C47 . C48 . B56 . 122.9(3) yes C49 . C48 . B56 . 121.0(3) yes C48 . C49 . C50 . 122.3(3) yes C48 . C49 . H491 . 119.4 no C50 . C49 . H491 . 118.3 no C49 . C50 . C51 . 121.1(3) yes C49 . C50 . C52 . 118.4(3) yes C51 . C50 . C52 . 120.5(3) yes C50 . C51 . C46 . 117.7(3) yes C50 . C51 . H511 . 120.8 no C46 . C51 . H511 . 121.5 no C50 . C52 . F53 . 113.8(3) yes C50 . C52 . F54 . 111.8(3) yes F53 . C52 . F54 . 106.5(3) yes C50 . C52 . F55 . 112.0(3) yes F53 . C52 . F55 . 105.4(3) yes F54 . C52 . F55 . 106.8(4) yes C48 . B56 . C57 . 113.6(3) yes C48 . B56 . C71 . 104.1(3) yes C57 . B56 . C71 . 113.1(3) yes C48 . B56 . C85 . 111.1(3) yes C57 . B56 . C85 . 103.0(3) yes C71 . B56 . C85 . 112.2(3) yes B56 . C57 . C58 . 123.0(3) yes B56 . C57 . C62 . 120.5(3) yes C58 . C57 . C62 . 116.0(3) yes C57 . C58 . C59 . 121.9(3) yes C57 . C58 . H581 . 120.1 no C59 . C58 . H581 . 118.0 no C58 . C59 . C60 . 120.8(4) yes C58 . C59 . C67 . 117.7(3) yes C60 . C59 . C67 . 121.4(3) yes C59 . C60 . C61 . 118.5(4) yes C59 . C60 . H601 . 121.2 no C61 . C60 . H601 . 120.3 no C60 . C61 . C62 . 120.3(4) yes C60 . C61 . C63 . 121.6(4) yes C62 . C61 . C63 . 118.1(4) yes C57 . C62 . C61 . 122.4(3) yes C57 . C62 . H621 . 118.8 no C61 . C62 . H621 . 118.8 no C61 . C63 . F64 . 113.3(4) yes C61 . C63 . F65 . 112.4(4) yes F64 . C63 . F65 . 106.1(4) yes C61 . C63 . F66 . 112.1(4) yes F64 . C63 . F66 . 106.0(4) yes F65 . C63 . F66 . 106.4(5) yes C59 . C67 . F602 . 113.2(3) yes C59 . C67 . F601 . 114.2(3) yes F602 . C67 . F601 . 105.34(6) yes C59 . C67 . F600 . 112.6(3) yes F602 . C67 . F600 . 105.33(6) yes F601 . C67 . F600 . 105.40(6) yes C59 . C67 . F603 . 109.9(5) yes C59 . C67 . F604 . 110.6(5) yes F603 . C67 . F604 . 105.37(6) yes C59 . C67 . F605 . 119.2(6) yes F603 . C67 . F605 . 105.35(6) yes F604 . C67 . F605 . 105.36(6) yes B56 . C71 . C72 . 124.2(3) yes B56 . C71 . C76 . 120.0(3) yes C72 . C71 . C76 . 115.5(3) yes C71 . C72 . C73 . 122.0(4) yes C71 . C72 . H721 . 119.5 no C73 . C72 . H721 . 118.5 no C72 . C73 . C74 . 121.1(4) yes C72 . C73 . C81 . 118.9(4) yes C74 . C73 . C81 . 120.0(3) yes C73 . C74 . C75 . 118.2(3) yes C73 . C74 . H741 . 121.3 no C75 . C74 . H741 . 120.5 no C74 . C75 . C76 . 120.8(4) yes C74 . C75 . C77 . 119.8(3) yes C76 . C75 . C77 . 119.3(4) yes C71 . C76 . C75 . 122.4(3) yes C71 . C76 . H761 . 118.9 no C75 . C76 . H761 . 118.7 no C75 . C77 . F301 . 111.0(4) yes C75 . C77 . F300 . 112.1(4) yes F301 . C77 . F300 . 104.89(6) yes C75 . C77 . F302 . 117.9(4) yes F301 . C77 . F302 . 104.95(6) yes F300 . C77 . F302 . 104.95(6) yes C75 . C77 . F305 . 110.6(4) yes C75 . C77 . F304 . 114.0(3) yes F305 . C77 . F304 . 104.86(6) yes C75 . C77 . F303 . 116.5(4) yes F305 . C77 . F303 . 104.91(6) yes F304 . C77 . F303 . 104.96(6) yes C73 . C81 . F500 . 111.4(4) yes C73 . C81 . F502 . 110.1(4) yes F500 . C81 . F502 . 105.90(6) yes C73 . C81 . F501 . 116.9(4) yes F500 . C81 . F501 . 105.89(6) yes F502 . C81 . F501 . 105.96(6) yes C73 . C81 . F504 . 109.7(4) yes C73 . C81 . F505 . 114.1(5) yes F504 . C81 . F505 . 105.92(6) yes C73 . C81 . F503 . 114.6(4) yes F504 . C81 . F503 . 105.97(6) yes F505 . C81 . F503 . 105.96(6) yes B56 . C85 . C86 . 120.7(3) yes B56 . C85 . C90 . 122.9(3) yes C86 . C85 . C90 . 115.8(3) yes C85 . C86 . C87 . 121.9(3) yes C85 . C86 . H861 . 119.3 no C87 . C86 . H861 . 118.8 no C86 . C87 . C88 . 121.0(3) yes C86 . C87 . C95 . 121.8(3) yes C88 . C87 . C95 . 117.2(3) yes C87 . C88 . C89 . 118.3(3) yes C87 . C88 . H881 . 121.3 no C89 . C88 . H881 . 120.5 no C88 . C89 . C90 . 120.9(3) yes C88 . C89 . C91 . 120.4(3) yes C90 . C89 . C91 . 118.7(3) yes C89 . C90 . C85 . 122.2(3) yes C89 . C90 . H901 . 118.7 no C85 . C90 . H901 . 119.2 no C89 . C91 . F92 . 112.4(4) yes C89 . C91 . F93 . 112.0(3) yes F92 . C91 . F93 . 105.9(4) yes C89 . C91 . F94 . 112.7(3) yes F92 . C91 . F94 . 107.3(3) yes F93 . C91 . F94 . 106.1(4) yes C87 . C95 . F402 . 109.1(5) yes C87 . C95 . F401 . 111.7(5) yes F402 . C95 . F401 . 105.31(6) yes C87 . C95 . F400 . 119.0(5) yes F402 . C95 . F400 . 105.37(6) yes F401 . C95 . F400 . 105.35(6) yes C87 . C95 . F403 . 110.7(3) yes C87 . C95 . F405 . 115.1(3) yes F403 . C95 . F405 . 105.29(6) yes C87 . C95 . F404 . 114.1(3) yes F403 . C95 . F404 . 105.33(6) yes F405 . C95 . F404 . 105.40(6) yes _iucr_refine_instruction_details_constraints ; # # Punched on 13/07/12 at 15:20:31 # #LIST 12 BLOCK SCALE X'S, U'S EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) EQUIV PART(2001,OCC) PART(2002,OCC) WEIGHT -1 PART(2002,OCC) EQUIV PART(3001,OCC) PART(3002,OCC) WEIGHT -1 PART(3002,OCC) EQUIV PART(4001,OCC) PART(4002,OCC) WEIGHT -1 PART(4002,OCC) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 13/07/12 at 15:20:31 # #LIST 16 SAME C(77) F(300) F(301) F(302) AND CONT C(77) F(301) F(302) F(300) AND CONT C(77) F(302) F(300) F(301) AND CONT C(77) F(303) F(304) F(305) AND CONT C(77) F(304) F(305) F(303) AND CONT C(77) F(305) F(303) F(304) SIMU 0.01 C(77) F(300) F(301) F(302) AND CONT C(77) F(301) F(302) F(300) AND CONT C(77) F(302) F(300) F(301) AND CONT C(77) F(303) F(304) F(305) AND CONT C(77) F(304) F(305) F(303) AND CONT C(77) F(305) F(303) F(304) DELU 0.01 C(77) F(300) F(301) F(302) AND CONT C(77) F(301) F(302) F(300) AND CONT C(77) F(302) F(300) F(301) AND CONT C(77) F(303) F(304) F(305) AND CONT C(77) F(304) F(305) F(303) AND CONT C(77) F(305) F(303) F(304) SAME C(95) F(400) F(401) F(402) AND CONT C(95) F(401) F(402) F(400) AND CONT C(95) F(402) F(400) F(401) AND CONT C(95) F(403) F(404) F(405) AND CONT C(95) F(404) F(405) F(403) AND CONT C(95) F(405) F(403) F(404) SIMU 0.01 C(95) F(400) F(401) F(402) AND CONT C(95) F(401) F(402) F(400) AND CONT C(95) F(402) F(400) F(401) AND CONT C(95) F(403) F(404) F(405) AND CONT C(95) F(404) F(405) F(403) AND CONT C(95) F(405) F(403) F(404) DELU 0.01 C(95) F(400) F(401) F(402) AND CONT C(95) F(401) F(402) F(400) AND CONT C(95) F(402) F(400) F(401) AND CONT C(95) F(403) F(404) F(405) AND CONT C(95) F(404) F(405) F(403) AND CONT C(95) F(405) F(403) F(404) SAME C(81) F(500) F(501) F(502) AND CONT C(81) F(501) F(502) F(500) AND CONT C(81) F(502) F(500) F(501) AND CONT C(81) F(503) F(504) F(505) AND CONT C(81) F(504) F(505) F(503) AND CONT C(81) F(505) F(503) F(504) SIMU 0.01 C(81) F(500) F(501) F(502) AND CONT C(81) F(501) F(502) F(500) AND CONT C(81) F(502) F(500) F(501) AND CONT C(81) F(503) F(504) F(505) AND CONT C(81) F(504) F(505) F(503) AND CONT C(81) F(505) F(503) F(504) DELU 0.01 C(81) F(500) F(501) F(502) AND CONT C(81) F(501) F(502) F(500) AND CONT C(81) F(502) F(500) F(501) AND CONT C(81) F(503) F(504) F(505) AND CONT C(81) F(504) F(505) F(503) AND CONT C(81) F(505) F(503) F(504) SAME C(67) F(600) F(601) F(602) AND CONT C(67) F(601) F(602) F(600) AND CONT C(67) F(602) F(600) F(601) AND CONT C(67) F(603) F(604) F(605) AND CONT C(67) F(604) F(605) F(603) AND CONT C(67) F(605) F(603) F(604) SIMU 0.01 C(67) F(600) F(601) F(602) AND CONT C(67) F(601) F(602) F(600) AND CONT C(67) F(602) F(600) F(601) AND CONT C(67) F(603) F(604) F(605) AND CONT C(67) F(604) F(605) F(603) AND CONT C(67) F(605) F(603) F(604) DELU 0.01 C(67) F(600) F(601) F(602) AND CONT C(67) F(601) F(602) F(600) AND CONT C(67) F(602) F(600) F(601) AND CONT C(67) F(603) F(604) F(605) AND CONT C(67) F(604) F(605) F(603) AND CONT C(67) F(605) F(603) F(604) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ;