# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_po001 #?# MeasurementCode _audit_update_record 24-Oct-2013 _chemical_name_common Fe12a(bipy) _chemical_compound_source ; Crystals obtained by slow diffusion setup. ; _exptl_crystal_description rod #?# e.g.: needle, platelet; prismatic _exptl_crystal_colour black #white, black, blue, violet, red, pink, yellow, gold, silver #bronze, grey, orange, green, colourless, brown, purple _exptl_crystal_size_max 0.23 #?# in millimeters _exptl_crystal_size_mid 0.07 #?# in millimeters _exptl_crystal_size_min 0.03 #?# in millimeters _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ; ? ; _audit_creation_date 2013-10-24 #?# style: 18-Aug-1998 _diffrn_ambient_temperature 173(2) #?# in K _diffrn_source_type 'Spellman generator' _diffrn_source_power 2.00 #?# in kW _diffrn_source_voltage 50 #?# in kV _diffrn_source_current 40 #?# in mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device 'CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Oxford XCalibur' _diffrn_measurement_method '\w scans' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -31.00 17.00 1.0000 150.0000 omega____ theta____ kappa____ phi______ frames - -13.9983 -38.0000 -30.0000 48 #__ type_ start__ end____ width___ exp.time_ 2 omega -53.00 90.00 1.0000 150.0000 omega____ theta____ kappa____ phi______ frames - 15.0139 0.0000 -120.0000 143 #__ type_ start__ end____ width___ exp.time_ 3 omega 60.00 95.00 1.0000 150.0000 omega____ theta____ kappa____ phi______ frames - 15.0139 179.0000 -120.0000 35 ; _diffrn_detector_area_resol_mean 15.9809 _diffrn_special_details ; crystal decays due to loss of included solvent molecules leading to a low data completeness ; _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 0.0544166739 _diffrn_orient_matrix_UB_12 0.0228866088 _diffrn_orient_matrix_UB_13 0.0025111906 _diffrn_orient_matrix_UB_21 0.0266613759 _diffrn_orient_matrix_UB_22 -0.0298992381 _diffrn_orient_matrix_UB_23 -0.0199355246 _diffrn_orient_matrix_UB_31 -0.0209048988 _diffrn_orient_matrix_UB_32 0.0212362265 _diffrn_orient_matrix_UB_33 -0.0308004670 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? ? _cell_length_a 11.1275(18) _cell_length_b 16.408(2) _cell_length_c 21.317(3) _cell_angle_alpha 90 _cell_angle_beta 115.206(11) _cell_angle_gamma 90 _cell_volume 3521.5(9) _cell_measurement_temperature 173(2) #?# in K _cell_measurement_reflns_used 2812 _cell_measurement_theta_min 4.2179 _cell_measurement_theta_max 26.0711 _cell_special_details ? #?# supposed (pseudo-)symmetries,subcells,deviation from standard setting loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #?# same style as for the absorption correction routine, e.g.: #?# -1 0 -1 .0424 #:---------------------------------------------------------------------------- #:---------------------------ABSORPTION CORRECTION---------------------------- #:---------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 0.492 _exptl_absorpt_correction_type multi-scan #numerical (using crystal faces), refdelf (using DIFABS) _exptl_absorpt_correction_T_min 0.96455 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #?# 'XRed, rev. 1.09, Stoe (Darmstadt, Germany)' #:---------------------------------------------------------------------------- #:------------------------REFLECTION DATA ANALYSIS---------------------------- #:---------------------------------------------------------------------------- _diffrn_reflns_number 12551 #xl _diffrn_reflns_av_R_equivalents 0.0487 #xl _diffrn_reflns_av_sigmaI/netI 0.1784 #xl _diffrn_reflns_limit_h_min -13 #xl _diffrn_reflns_limit_h_max 13 #xl _diffrn_reflns_limit_k_min -20 #xl _diffrn_reflns_limit_k_max 12 #xl _diffrn_reflns_limit_l_min -23 #xl _diffrn_reflns_limit_l_max 26 #xl _diffrn_reflns_theta_min 4.22 #xl _diffrn_reflns_theta_max 26.14 #xl _diffrn_measured_fraction_theta_max 0.82 #xl _diffrn_reflns_theta_full 26.14 #xl _diffrn_measured_fraction_theta_full 0.82 #xl #:---------------------------------------------------------------------------- #:---------------------STRUCTURE SOLUTION AND REFINEMENT---------------------- #:---------------------------------------------------------------------------- _symmetry_cell_setting monoclinic #triclinic, monoclinic, orthorhombic, tetragonal #rhombohedral, trigonal, hexagonal, cubic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 5806 #xl _reflns_number_gt 2722 #xl _reflns_threshold_expression >2sigma(I) #xl _reflns_special_details ? #?# "A description of reflection data not covered by the other data #?# names. It should include details of the Friedel pairs." _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0084P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr #?# mixed --> _refine_special_det #none, undef, noref, refall, refxyz, refU, constr, mixed _refine_ls_extinction_method none #xl _refine_ls_extinction_coef ? #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 5806 #xl _refine_ls_number_parameters 454 #xl _refine_ls_number_restraints 0 #xl _refine_ls_R_factor_all 0.1101 #xl _refine_ls_R_factor_gt 0.0410 #xl _refine_ls_wR_factor_ref 0.0519 #xl _refine_ls_wR_factor_gt 0.0463 #xl _refine_ls_goodness_of_fit_ref 0.69 #xl _refine_ls_restrained_S_all 0.69 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0 #xl _refine_diff_density_max 0.423 #xl _refine_diff_density_min -0.378 #xl _refine_diff_density_rms 0.053 #xl _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; #?# describe twinnung here, e.g.: twin axis: [100], #?# volume fraction of the twin component from refinement: 0.4767 #?# # details of H atom refinement: # 1 common U for all H atoms # riding with U(H)=1.2*U(C) for CH2 and CH, 1.5*U(C) for CH3 # C-bonded H: constr # N-bonded H: constr # O-bonded H: not considered # O-bonded H: O-H fixed to 0.83 \%A, H...H fixed to 1.31 \%A # O-bonded H: 1 common O-H, which refined to ? \%A, # H...H fixed to the 1.57fold of O-H (forcing H-O-H to 105\%) #?# exhaustive(!) comments on disorder here #:---------------------------------------------------------------------------- #:-----------------------------REFERENCES------------------------------------- #:---------------------------------------------------------------------------- _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ; ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ; PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; #:---------------------------------------------------------------------------- #:---------------------TABLES AND GEOMETRICAL DATA---------------------------- #:---------------------------------------------------------------------------- loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.67416(4) 0.26297(3) 0.07485(2) 0.01742(13) Uani 1 1 d . . . O1 O 0.70104(18) 0.37055(12) 0.11655(9) 0.0176(5) Uani 1 1 d . . . O2 O 0.59649(18) 0.31463(12) -0.01535(9) 0.0200(6) Uani 1 1 d . . . O3 O 0.8591(2) 0.43180(14) 0.32349(9) 0.0343(7) Uani 1 1 d . . . O4 O 0.8895(2) 0.30098(13) 0.35527(10) 0.0476(8) Uani 1 1 d . . . O5 O 0.5262(2) 0.08440(14) -0.15653(9) 0.0322(7) Uani 1 1 d . . . O6 O 0.4052(2) 0.19439(14) -0.20696(10) 0.0397(7) Uani 1 1 d . . . O7 O 0.8954(2) -0.06632(12) 0.25072(9) 0.0317(6) Uani 1 1 d . . . H7 H 0.9264 -0.0430 0.2895 0.048 Uiso 1 1 calc R . . O8 O 0.7853(2) -0.11991(13) 0.11703(9) 0.0379(7) Uani 1 1 d . . . H8 H 0.8195 -0.1465 0.1542 0.057 Uiso 1 1 calc R . . N1 N 0.7530(2) 0.21126(16) 0.16246(11) 0.0162(7) Uani 1 1 d . . . N2 N 0.6517(2) 0.15693(14) 0.03680(11) 0.0145(7) Uani 1 1 d . . . N3 N 0.8526(2) 0.26968(15) 0.07314(11) 0.0168(6) Uani 1 1 d . . . N4 N 0.4952(2) 0.25835(16) 0.07511(11) 0.0188(7) Uani 1 1 d . . . C1 C 0.7511(3) 0.39042(19) 0.18040(15) 0.0147(8) Uani 1 1 d . . . C2 C 0.7970(3) 0.3321(2) 0.23534(14) 0.0157(8) Uani 1 1 d . . . C3 C 0.7948(3) 0.2473(2) 0.22253(14) 0.0192(8) Uani 1 1 d . . . H3 H 0.8276 0.2129 0.2621 0.023 Uiso 1 1 calc R . . C4 C 0.7650(3) 0.1255(2) 0.15655(14) 0.0155(8) Uani 1 1 d . . . C5 C 0.8286(3) 0.0715(2) 0.21174(14) 0.0194(8) Uani 1 1 d . . . H5 H 0.8678 0.0915 0.2579 0.023 Uiso 1 1 calc R . . C6 C 0.8347(3) -0.0100(2) 0.19954(15) 0.0222(9) Uani 1 1 d . . . C7 C 0.7783(3) -0.0398(2) 0.13158(15) 0.0258(9) Uani 1 1 d . . . C8 C 0.7147(3) 0.0135(2) 0.07701(14) 0.0215(9) Uani 1 1 d . . . H8A H 0.6747 -0.0067 0.0309 0.026 Uiso 1 1 calc R . . C9 C 0.7089(3) 0.0956(2) 0.08889(14) 0.0162(8) Uani 1 1 d . . . C10 C 0.5978(3) 0.1382(2) -0.02849(14) 0.0185(8) Uani 1 1 d . . . H10 H 0.5933 0.0821 -0.0402 0.022 Uiso 1 1 calc R . . C11 C 0.5442(3) 0.1955(2) -0.08461(14) 0.0177(8) Uani 1 1 d . . . C12 C 0.5527(3) 0.2806(2) -0.07480(15) 0.0195(8) Uani 1 1 d . . . C13 C 0.5161(3) 0.34027(19) -0.13474(14) 0.0368(10) Uani 1 1 d . . . H13A H 0.4208 0.3521 -0.1539 0.055 Uiso 1 1 calc R . . H13B H 0.5374 0.3163 -0.1709 0.055 Uiso 1 1 calc R . . H13C H 0.5664 0.3909 -0.1180 0.055 Uiso 1 1 calc R . . C14 C 0.7549(3) 0.48135(18) 0.19141(13) 0.0301(9) Uani 1 1 d . . . H14A H 0.7241 0.5091 0.1465 0.045 Uiso 1 1 calc R . . H14B H 0.8461 0.4983 0.2211 0.045 Uiso 1 1 calc R . . H14C H 0.6969 0.4957 0.2138 0.045 Uiso 1 1 calc R . . C15 C 0.4846(3) 0.1613(2) -0.15471(16) 0.0261(9) Uani 1 1 d . . . C16 C 0.4658(3) 0.0414(2) -0.22136(14) 0.0388(10) Uani 1 1 d . . . H16A H 0.4985 0.0631 -0.2546 0.047 Uiso 1 1 calc R . . H16B H 0.3680 0.0478 -0.2418 0.047 Uiso 1 1 calc R . . C17 C 0.5031(4) -0.0466(2) -0.20612(16) 0.0543(12) Uani 1 1 d . . . H17A H 0.5998 -0.0522 -0.1875 0.081 Uiso 1 1 calc R . . H17B H 0.4610 -0.0784 -0.2489 0.081 Uiso 1 1 calc R . . H17C H 0.4729 -0.0667 -0.1720 0.081 Uiso 1 1 calc R . . C18 C 0.8532(3) 0.3517(2) 0.30984(15) 0.0258(9) Uani 1 1 d . . . C19 C 0.9156(4) 0.4538(2) 0.39610(14) 0.0430(11) Uani 1 1 d . . . H19A H 1.0034 0.4276 0.4211 0.052 Uiso 1 1 calc R . . H19B H 0.8566 0.4359 0.4175 0.052 Uiso 1 1 calc R . . C20 C 0.9299(3) 0.5453(2) 0.39970(15) 0.0502(11) Uani 1 1 d . . . H20A H 0.9869 0.5622 0.3775 0.075 Uiso 1 1 calc R . . H20B H 0.9698 0.5626 0.4483 0.075 Uiso 1 1 calc R . . H20C H 0.8421 0.5705 0.3757 0.075 Uiso 1 1 calc R . . C21 C 0.9926(3) 0.24779(19) 0.01503(12) 0.0196(8) Uani 1 1 d . . . H21 H 0.9989 0.2337 -0.0267 0.023 Uiso 1 1 calc R . . C22 C 0.8703(3) 0.24951(19) 0.01642(12) 0.0184(8) Uani 1 1 d . . . H22 H 0.7944 0.2358 -0.0247 0.022 Uiso 1 1 calc R . . C23 C 0.9630(3) 0.29038(18) 0.12922(14) 0.0210(9) Uani 1 1 d . . . H23 H 0.9537 0.3069 0.1696 0.025 Uiso 1 1 calc R . . C24 C 1.0885(3) 0.28924(18) 0.13198(13) 0.0206(9) Uani 1 1 d . . . H24 H 1.1628 0.3040 0.1735 0.025 Uiso 1 1 calc R . . C25 C 1.1062(3) 0.26622(19) 0.07336(13) 0.0160(8) Uani 1 1 d . . . C26 C 1.2400(3) 0.26216(19) 0.07434(13) 0.0170(8) Uani 1 1 d . . . C27 C 1.2605(3) 0.23265(19) 0.01864(13) 0.0215(8) Uani 1 1 d . . . H27 H 1.1873 0.2131 -0.0214 0.026 Uiso 1 1 calc R . . C28 C 0.3864(3) 0.23152(19) 0.02095(13) 0.0217(8) Uani 1 1 d . . . H28 H 0.3966 0.2105 -0.0180 0.026 Uiso 1 1 calc R . . C29 C 0.4759(3) 0.28364(18) 0.13015(13) 0.0199(9) Uani 1 1 d . . . H29 H 0.5513 0.3000 0.1705 0.024 Uiso 1 1 calc R . . C30 C 1.3535(3) 0.28731(19) 0.13149(14) 0.0228(9) Uani 1 1 d . . . H30 H 1.3464 0.3071 0.1716 0.027 Uiso 1 1 calc R . . O31 O 0.2371(2) 0.52706(16) -0.02068(13) 0.0549(8) Uani 1 1 d . . . H31 H 0.2732 0.5684 -0.0284 0.082 Uiso 1 1 calc R . . C31 C 0.3336(4) 0.4652(2) 0.00941(17) 0.0655(13) Uani 1 1 d . . . H31A H 0.3683 0.4482 -0.0238 0.098 Uiso 1 1 calc R . . H31B H 0.2928 0.4184 0.0214 0.098 Uiso 1 1 calc R . . H31C H 0.4065 0.4863 0.0514 0.098 Uiso 1 1 calc R . . O32 O 0.1589(2) 0.25509(16) 0.29597(12) 0.0568(8) Uani 1 1 d . . . H32 H 0.2367 0.2596 0.2995 0.085 Uiso 1 1 calc R . . C32 C 0.1501(4) 0.1862(2) 0.33186(19) 0.0736(14) Uani 1 1 d . . . H32A H 0.0797 0.1940 0.3474 0.110 Uiso 1 1 calc R . . H32B H 0.2350 0.1775 0.3722 0.110 Uiso 1 1 calc R . . H32C H 0.1294 0.1386 0.3013 0.110 Uiso 1 1 calc R . . O33 O 0.0025(2) 0.51045(17) 0.12622(10) 0.0510(8) Uani 1 1 d . . . H33 H -0.0694 0.4934 0.0952 0.077 Uiso 1 1 calc R . . C33 C 0.0907(4) 0.5302(3) 0.09649(18) 0.1024(19) Uani 1 1 d . . . H33A H 0.1120 0.4809 0.0774 0.154 Uiso 1 1 calc R . . H33B H 0.1724 0.5534 0.1322 0.154 Uiso 1 1 calc R . . H33C H 0.0487 0.5702 0.0593 0.154 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0142(3) 0.0219(3) 0.0163(2) 0.0003(2) 0.00669(19) -0.0003(3) O1 0.0182(14) 0.0200(14) 0.0148(11) 0.0004(10) 0.0072(10) 0.0007(11) O2 0.0159(14) 0.0258(15) 0.0188(12) -0.0020(11) 0.0077(11) -0.0004(11) O3 0.0534(18) 0.0232(16) 0.0158(12) -0.0079(11) 0.0047(12) 0.0007(14) O4 0.090(2) 0.0247(17) 0.0154(12) 0.0060(11) 0.0100(13) 0.0073(15) O5 0.0363(17) 0.0392(18) 0.0180(12) -0.0094(12) 0.0084(11) 0.0029(14) O6 0.0439(17) 0.0498(19) 0.0135(11) 0.0034(12) 0.0007(12) 0.0041(14) O7 0.0412(17) 0.0234(15) 0.0215(12) 0.0031(11) 0.0045(12) 0.0049(13) O8 0.0585(19) 0.0210(16) 0.0263(12) -0.0024(11) 0.0104(14) 0.0056(15) N1 0.0127(15) 0.0216(19) 0.0161(14) -0.0027(13) 0.0079(12) -0.0018(14) N2 0.0123(16) 0.0196(18) 0.0114(14) 0.0010(12) 0.0049(12) 0.0025(13) N3 0.0183(16) 0.0177(17) 0.0169(13) -0.0017(13) 0.0099(12) -0.0018(14) N4 0.0157(16) 0.0266(19) 0.0179(13) 0.0013(14) 0.0108(12) 0.0011(15) C1 0.015(2) 0.013(2) 0.0206(18) -0.0061(17) 0.0120(16) 0.0010(16) C2 0.012(2) 0.018(2) 0.0163(17) -0.0002(17) 0.0060(15) -0.0007(17) C3 0.0203(19) 0.020(2) 0.0172(17) 0.0041(17) 0.0078(14) 0.0002(18) C4 0.011(2) 0.017(2) 0.0178(18) -0.0058(17) 0.0059(15) -0.0024(17) C5 0.025(2) 0.020(2) 0.0148(17) -0.0008(16) 0.0094(16) -0.0006(18) C6 0.029(2) 0.021(2) 0.0161(18) 0.0044(18) 0.0085(17) 0.0003(19) C7 0.034(2) 0.014(2) 0.029(2) -0.0033(19) 0.0142(18) -0.001(2) C8 0.025(2) 0.025(2) 0.0105(16) -0.0018(17) 0.0027(16) -0.0014(18) C9 0.016(2) 0.018(2) 0.0146(18) 0.0002(16) 0.0063(15) -0.0001(17) C10 0.016(2) 0.023(2) 0.0207(18) -0.0059(17) 0.0119(16) -0.0014(18) C11 0.017(2) 0.028(2) 0.0087(17) 0.0036(17) 0.0056(15) -0.0003(18) C12 0.013(2) 0.029(3) 0.0171(18) 0.0016(18) 0.0069(15) 0.0013(18) C13 0.050(3) 0.030(3) 0.0269(19) 0.0052(18) 0.0129(19) 0.001(2) C14 0.043(3) 0.023(2) 0.0243(18) 0.0031(16) 0.0148(17) 0.003(2) C15 0.022(2) 0.033(3) 0.028(2) 0.000(2) 0.0151(19) -0.003(2) C16 0.041(3) 0.053(3) 0.022(2) -0.015(2) 0.0130(18) -0.002(2) C17 0.054(3) 0.051(3) 0.054(2) -0.028(2) 0.020(2) 0.004(3) C18 0.026(2) 0.028(3) 0.024(2) -0.0128(19) 0.0113(18) -0.006(2) C19 0.064(3) 0.035(3) 0.0200(19) -0.0136(18) 0.0086(19) -0.005(2) C20 0.058(3) 0.037(3) 0.041(2) -0.013(2) 0.007(2) 0.002(2) C21 0.0179(19) 0.031(2) 0.0147(15) -0.0019(16) 0.0118(14) 0.0001(19) C22 0.0104(18) 0.034(2) 0.0103(15) -0.0028(16) 0.0035(13) -0.0005(18) C23 0.020(2) 0.031(2) 0.0161(17) -0.0056(15) 0.0114(16) -0.0019(18) C24 0.014(2) 0.032(2) 0.0168(17) -0.0050(15) 0.0076(15) -0.0062(18) C25 0.0095(18) 0.020(2) 0.0197(17) 0.0009(16) 0.0072(14) -0.0022(17) C26 0.0140(19) 0.022(2) 0.0192(17) -0.0045(16) 0.0107(15) -0.0033(18) C27 0.0116(18) 0.030(2) 0.0198(16) -0.0059(17) 0.0035(14) -0.0050(19) C28 0.0173(19) 0.028(2) 0.0201(17) -0.0117(17) 0.0084(15) -0.0041(19) C29 0.0113(19) 0.033(2) 0.0123(16) -0.0064(15) 0.0021(15) -0.0022(17) C30 0.019(2) 0.035(3) 0.0191(17) -0.0037(15) 0.0128(16) 0.0020(18) O31 0.0512(19) 0.046(2) 0.0639(17) 0.0199(16) 0.0215(15) -0.0140(17) C31 0.078(4) 0.050(3) 0.053(3) 0.012(2) 0.013(2) -0.006(3) O32 0.065(2) 0.0422(19) 0.0518(14) 0.0085(14) 0.0142(16) -0.0007(18) C32 0.062(3) 0.044(3) 0.102(3) 0.022(3) 0.022(3) -0.007(3) O33 0.059(2) 0.057(2) 0.0303(14) 0.0027(14) 0.0130(14) -0.0073(17) C33 0.092(4) 0.164(5) 0.053(3) -0.004(3) 0.033(3) -0.037(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.891(2) . ? Fe1 N1 1.893(2) . ? Fe1 O2 1.9358(18) . ? Fe1 O1 1.941(2) . ? Fe1 N4 1.995(2) . ? Fe1 N3 2.004(2) . ? O1 C1 1.274(3) . ? O2 C12 1.277(3) . ? O3 C18 1.342(3) . ? O3 C19 1.447(3) . ? O4 C18 1.209(3) . ? O5 C15 1.351(3) . ? O5 C16 1.438(3) . ? O6 C15 1.215(3) . ? O7 C6 1.368(3) . ? O7 H7 0.8400 . ? O8 C7 1.360(3) . ? O8 H8 0.8400 . ? N1 C3 1.303(3) . ? N1 C4 1.424(3) . ? N2 C10 1.296(3) . ? N2 C9 1.431(3) . ? N3 C23 1.343(3) . ? N3 C22 1.347(3) . ? N4 C28 1.342(3) . ? N4 C29 1.345(3) . ? C1 C2 1.428(4) . ? C1 C14 1.508(4) . ? C2 C3 1.416(4) . ? C2 C18 1.473(4) . ? C3 H3 0.9500 . ? C4 C9 1.394(3) . ? C4 C5 1.401(4) . ? C5 C6 1.370(4) . ? C5 H5 0.9500 . ? C6 C7 1.399(4) . ? C7 C8 1.385(4) . ? C8 C9 1.377(4) . ? C8 H8A 0.9500 . ? C10 C11 1.436(4) . ? C10 H10 0.9500 . ? C11 C12 1.408(4) . ? C11 C15 1.464(4) . ? C12 C13 1.522(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 C17 1.500(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19 C20 1.508(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.374(3) . ? C21 C25 1.377(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.372(3) . ? C23 H23 0.9500 . ? C24 C25 1.398(3) . ? C24 H24 0.9500 . ? C25 C26 1.481(3) . ? C26 C27 1.388(3) . ? C26 C30 1.393(3) . ? C27 C28 1.381(3) 1_655 ? C27 H27 0.9500 . ? C28 C27 1.381(3) 1_455 ? C28 H28 0.9500 . ? C29 C30 1.375(3) 1_455 ? C29 H29 0.9500 . ? C30 C29 1.375(3) 1_655 ? C30 H30 0.9500 . ? O31 C31 1.417(4) . ? O31 H31 0.8400 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? O32 C32 1.391(3) . ? O32 H32 0.8400 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O33 C33 1.414(4) . ? O33 H33 0.8400 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N1 86.10(11) . . ? N2 Fe1 O2 93.17(9) . . ? N1 Fe1 O2 178.68(10) . . ? N2 Fe1 O1 178.28(10) . . ? N1 Fe1 O1 92.26(10) . . ? O2 Fe1 O1 88.46(8) . . ? N2 Fe1 N4 90.96(10) . . ? N1 Fe1 N4 91.37(9) . . ? O2 Fe1 N4 89.74(8) . . ? O1 Fe1 N4 89.58(10) . . ? N2 Fe1 N3 89.62(10) . . ? N1 Fe1 N3 89.79(9) . . ? O2 Fe1 N3 89.12(9) . . ? O1 Fe1 N3 89.87(9) . . ? N4 Fe1 N3 178.74(10) . . ? C1 O1 Fe1 129.33(19) . . ? C12 O2 Fe1 127.9(2) . . ? C18 O3 C19 115.8(2) . . ? C15 O5 C16 117.4(3) . . ? C6 O7 H7 109.5 . . ? C7 O8 H8 109.5 . . ? C3 N1 C4 121.8(2) . . ? C3 N1 Fe1 126.0(2) . . ? C4 N1 Fe1 112.15(17) . . ? C10 N2 C9 121.1(3) . . ? C10 N2 Fe1 126.5(2) . . ? C9 N2 Fe1 112.35(18) . . ? C23 N3 C22 115.6(2) . . ? C23 N3 Fe1 122.41(18) . . ? C22 N3 Fe1 121.87(18) . . ? C28 N4 C29 115.5(2) . . ? C28 N4 Fe1 123.06(18) . . ? C29 N4 Fe1 121.40(18) . . ? O1 C1 C2 123.1(3) . . ? O1 C1 C14 112.9(3) . . ? C2 C1 C14 124.0(3) . . ? C3 C2 C1 122.0(3) . . ? C3 C2 C18 112.8(3) . . ? C1 C2 C18 125.2(3) . . ? N1 C3 C2 127.2(3) . . ? N1 C3 H3 116.4 . . ? C2 C3 H3 116.4 . . ? C9 C4 C5 119.3(3) . . ? C9 C4 N1 115.0(3) . . ? C5 C4 N1 125.7(3) . . ? C6 C5 C4 120.4(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? O7 C6 C5 123.7(3) . . ? O7 C6 C7 116.2(3) . . ? C5 C6 C7 120.1(3) . . ? O8 C7 C8 118.5(3) . . ? O8 C7 C6 122.0(3) . . ? C8 C7 C6 119.5(3) . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C4 120.0(3) . . ? C8 C9 N2 125.8(3) . . ? C4 C9 N2 114.2(3) . . ? N2 C10 C11 125.3(3) . . ? N2 C10 H10 117.4 . . ? C11 C10 H10 117.4 . . ? C12 C11 C10 123.2(3) . . ? C12 C11 C15 120.3(3) . . ? C10 C11 C15 116.5(3) . . ? O2 C12 C11 123.7(3) . . ? O2 C12 C13 113.8(3) . . ? C11 C12 C13 122.4(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C1 C14 H14A 109.5 . . ? C1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O6 C15 O5 121.0(3) . . ? O6 C15 C11 126.9(3) . . ? O5 C15 C11 112.1(3) . . ? O5 C16 C17 106.9(3) . . ? O5 C16 H16A 110.3 . . ? C17 C16 H16A 110.3 . . ? O5 C16 H16B 110.3 . . ? C17 C16 H16B 110.3 . . ? H16A C16 H16B 108.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 O3 122.1(3) . . ? O4 C18 C2 123.8(3) . . ? O3 C18 C2 114.0(3) . . ? O3 C19 C20 106.9(3) . . ? O3 C19 H19A 110.3 . . ? C20 C19 H19A 110.3 . . ? O3 C19 H19B 110.3 . . ? C20 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C25 120.8(2) . . ? C22 C21 H21 119.6 . . ? C25 C21 H21 119.6 . . ? N3 C22 C21 123.3(2) . . ? N3 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? N3 C23 C24 124.3(3) . . ? N3 C23 H23 117.8 . . ? C24 C23 H23 117.8 . . ? C23 C24 C25 119.6(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C21 C25 C24 116.2(3) . . ? C21 C25 C26 122.2(2) . . ? C24 C25 C26 121.6(2) . . ? C27 C26 C30 115.7(3) . . ? C27 C26 C25 122.3(2) . . ? C30 C26 C25 122.1(2) . . ? C28 C27 C26 120.5(3) 1_655 . ? C28 C27 H27 119.7 1_655 . ? C26 C27 H27 119.7 . . ? N4 C28 C27 123.8(3) . 1_455 ? N4 C28 H28 118.1 . . ? C27 C28 H28 118.1 1_455 . ? N4 C29 C30 124.0(3) . 1_455 ? N4 C29 H29 118.0 . . ? C30 C29 H29 118.0 1_455 . ? C29 C30 C26 120.4(3) 1_655 . ? C29 C30 H30 119.8 1_655 . ? C26 C30 H30 119.8 . . ? C31 O31 H31 109.5 . . ? O31 C31 H31A 109.5 . . ? O31 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O31 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C32 O32 H32 109.5 . . ? O32 C32 H32A 109.5 . . ? O32 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O32 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 O33 H33 109.5 . . ? O33 C33 H33A 109.5 . . ? O33 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O33 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 O1 C1 -1.8(2) . . . . ? O2 Fe1 O1 C1 179.3(2) . . . . ? N4 Fe1 O1 C1 89.6(2) . . . . ? N3 Fe1 O1 C1 -91.6(2) . . . . ? N2 Fe1 O2 C12 -1.2(2) . . . . ? O1 Fe1 O2 C12 178.3(2) . . . . ? N4 Fe1 O2 C12 -92.1(2) . . . . ? N3 Fe1 O2 C12 88.4(2) . . . . ? N2 Fe1 N1 C3 -176.6(2) . . . . ? O1 Fe1 N1 C3 3.9(2) . . . . ? N4 Fe1 N1 C3 -85.8(2) . . . . ? N3 Fe1 N1 C3 93.7(2) . . . . ? N2 Fe1 N1 C4 4.4(2) . . . . ? N4 Fe1 N1 C4 95.3(2) . . . . ? N3 Fe1 N1 C4 -85.2(2) . . . . ? N1 Fe1 N2 C10 179.7(2) . . . . ? O2 Fe1 N2 C10 -1.4(2) . . . . ? N4 Fe1 N2 C10 88.4(2) . . . . ? N3 Fe1 N2 C10 -90.5(2) . . . . ? N1 Fe1 N2 C9 -3.60(19) . . . . ? O2 Fe1 N2 C9 175.31(19) . . . . ? N4 Fe1 N2 C9 -94.90(19) . . . . ? N3 Fe1 N2 C9 86.22(19) . . . . ? N2 Fe1 N3 C23 -128.2(2) . . . . ? N1 Fe1 N3 C23 -42.1(2) . . . . ? O2 Fe1 N3 C23 138.7(2) . . . . ? O1 Fe1 N3 C23 50.2(2) . . . . ? N2 Fe1 N3 C22 48.3(2) . . . . ? N1 Fe1 N3 C22 134.4(2) . . . . ? O2 Fe1 N3 C22 -44.9(2) . . . . ? O1 Fe1 N3 C22 -133.3(2) . . . . ? N2 Fe1 N4 C28 -45.6(3) . . . . ? N1 Fe1 N4 C28 -131.8(2) . . . . ? O2 Fe1 N4 C28 47.5(2) . . . . ? O1 Fe1 N4 C28 136.0(2) . . . . ? N2 Fe1 N4 C29 135.5(2) . . . . ? N1 Fe1 N4 C29 49.4(2) . . . . ? O2 Fe1 N4 C29 -131.4(2) . . . . ? O1 Fe1 N4 C29 -42.9(2) . . . . ? Fe1 O1 C1 C2 -1.0(4) . . . . ? Fe1 O1 C1 C14 179.77(19) . . . . ? O1 C1 C2 C3 2.6(5) . . . . ? C14 C1 C2 C3 -178.2(3) . . . . ? O1 C1 C2 C18 -178.8(3) . . . . ? C14 C1 C2 C18 0.4(5) . . . . ? C4 N1 C3 C2 175.3(3) . . . . ? Fe1 N1 C3 C2 -3.6(4) . . . . ? C1 C2 C3 N1 -0.2(5) . . . . ? C18 C2 C3 N1 -179.0(3) . . . . ? C3 N1 C4 C9 176.6(2) . . . . ? Fe1 N1 C4 C9 -4.4(3) . . . . ? C3 N1 C4 C5 -4.4(5) . . . . ? Fe1 N1 C4 C5 174.6(2) . . . . ? C9 C4 C5 C6 -0.6(5) . . . . ? N1 C4 C5 C6 -179.5(3) . . . . ? C4 C5 C6 O7 179.8(3) . . . . ? C4 C5 C6 C7 0.6(5) . . . . ? O7 C6 C7 O8 -1.1(5) . . . . ? C5 C6 C7 O8 178.1(3) . . . . ? O7 C6 C7 C8 179.8(3) . . . . ? C5 C6 C7 C8 -1.0(5) . . . . ? O8 C7 C8 C9 -177.8(3) . . . . ? C6 C7 C8 C9 1.3(5) . . . . ? C7 C8 C9 C4 -1.3(5) . . . . ? C7 C8 C9 N2 176.9(3) . . . . ? C5 C4 C9 C8 0.9(4) . . . . ? N1 C4 C9 C8 180.0(3) . . . . ? C5 C4 C9 N2 -177.5(3) . . . . ? N1 C4 C9 N2 1.6(4) . . . . ? C10 N2 C9 C8 0.6(5) . . . . ? Fe1 N2 C9 C8 -176.3(3) . . . . ? C10 N2 C9 C4 178.9(3) . . . . ? Fe1 N2 C9 C4 2.0(3) . . . . ? C9 N2 C10 C11 -176.6(3) . . . . ? Fe1 N2 C10 C11 -0.1(4) . . . . ? N2 C10 C11 C12 4.6(5) . . . . ? N2 C10 C11 C15 -178.6(3) . . . . ? Fe1 O2 C12 C11 5.4(5) . . . . ? Fe1 O2 C12 C13 -171.86(19) . . . . ? C10 C11 C12 O2 -7.3(5) . . . . ? C15 C11 C12 O2 176.0(3) . . . . ? C10 C11 C12 C13 169.7(3) . . . . ? C15 C11 C12 C13 -7.0(5) . . . . ? C16 O5 C15 O6 -4.4(5) . . . . ? C16 O5 C15 C11 174.6(3) . . . . ? C12 C11 C15 O6 -23.7(5) . . . . ? C10 C11 C15 O6 159.3(3) . . . . ? C12 C11 C15 O5 157.4(3) . . . . ? C10 C11 C15 O5 -19.6(4) . . . . ? C15 O5 C16 C17 -166.7(3) . . . . ? C19 O3 C18 O4 1.9(5) . . . . ? C19 O3 C18 C2 -179.1(3) . . . . ? C3 C2 C18 O4 -2.4(5) . . . . ? C1 C2 C18 O4 178.9(3) . . . . ? C3 C2 C18 O3 178.6(3) . . . . ? C1 C2 C18 O3 -0.1(4) . . . . ? C18 O3 C19 C20 172.4(3) . . . . ? C23 N3 C22 C21 1.5(4) . . . . ? Fe1 N3 C22 C21 -175.2(3) . . . . ? C25 C21 C22 N3 0.7(5) . . . . ? C22 N3 C23 C24 -2.3(4) . . . . ? Fe1 N3 C23 C24 174.4(2) . . . . ? N3 C23 C24 C25 0.7(5) . . . . ? C22 C21 C25 C24 -2.3(5) . . . . ? C22 C21 C25 C26 177.8(3) . . . . ? C23 C24 C25 C21 1.6(4) . . . . ? C23 C24 C25 C26 -178.5(3) . . . . ? C21 C25 C26 C27 -5.9(5) . . . . ? C24 C25 C26 C27 174.2(3) . . . . ? C21 C25 C26 C30 174.5(3) . . . . ? C24 C25 C26 C30 -5.4(5) . . . . ? C30 C26 C27 C28 -1.8(5) . . . 1_655 ? C25 C26 C27 C28 178.6(3) . . . 1_655 ? C29 N4 C28 C27 3.1(5) . . . 1_455 ? Fe1 N4 C28 C27 -175.8(2) . . . 1_455 ? C28 N4 C29 C30 -3.8(4) . . . 1_455 ? Fe1 N4 C29 C30 175.2(2) . . . 1_455 ? C27 C26 C30 C29 1.2(5) . . . 1_655 ? C25 C26 C30 C29 -179.1(3) . . . 1_655 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #?# use this item for nonbonding or very weakly bonding contacts, e.g.: #?# Sb1 N13 3.906(13) . . ? #?# Mn Mn 3.253(2) . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? #?# Do not(!) delete the #s to obtain a table header: # #D H A D - H H...A D...A D - H...A symm(A) publ_flag # #?# style: #?# N2 H721 O93 .72(4) 2.28(4) 2.868(4) 139(4) . ? #?# N2 H722 O1 .92(3) 2.44(3) 3.343(4) 171(3) 2_657 ? #?# #?# (1) This table may be copied from SHELXL97 (command HTAB D A_$n) #?# and rearranged (_geom_hbond_publ_flag missing); or #?# #?# (2) it may be copied from PLATON and rearranged; CAUTION! Check #?# symmetry operation numbers! They must(!) be identical from PLATON #?# and ACTA! "calc intra nomove" must(!) be used in PLATON runs! #?# Even then discrepancies may(!) occur! _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; #;Puckering parameters (\%A, \%) according to # D. Cremer, J. A. Pople, J. Am. Chem. Soc. 1975, 97, 1354--1358 #?# #?# style: #?# #?# Sb1 O2 C2 C3 O3 Q2 = 0.217(15) \f2 = 134(4) #?# O52 C12 C22 C32 C42 C52 Q = 0.577(5) \q = 3.2(6) \f = 271(9) #?# #?# or as a table: #?# #?# O5n - C1n - C2n - C3n - C4n - C5n #?# ------------------------------ #?# n Q theta phi #?# ------------------------------ #?# 11 .574(11) 6.3(11) 112(10) #?# 21 .557(10) 2.1(11) 86(22) #?# 31 .540(10) 6.2(11) 92(10) #?# 41 .571(10) 2.2(10) 221(34) #?# 51 .555(10) 10.6(10) 35(6) #?# 61 .571(10) 5.1(10) 13(13) #?# ------------------------------ #?# #?# least-squares planes be entered here, too #:---------------------------------------------------------------------------- #:--------------------------ARCHIVING AND CHECKING---------------------------- #:---------------------------------------------------------------------------- _audit_block_code Fe_L12a_Bipy_po001_Bauer #?# style: 'Element1_El2_Ligand1_Lig2_Anion_MeasurementCode_CrystalOwner' _audit_creation_method 'form98_oxf/compatible with shelxl97-2' _chemical_name_systematic ; ? ; #?# style: 'lithium meso-oxolanediolate monohydrate' _chemical_formula_moiety 'C30 H30 Fe N4 O8, 3(C H4 O)' #?# style: 'C36 H60 O30, 0.8(C5 H12), 4.25(H2 O)' _chemical_formula_sum 'C33 H42 Fe N4 O11' _chemical_formula_weight 726.552 #?# use the correct formula; take care of Hs not included in the atom list! _chemical_melting_point ? #?# in K! _cell_formula_units_Z 4 #?# adjust to _chemical_formula_[] _exptl_crystal_density_diffrn 1.3704 #?# include sigma (s) from: s(rho)=s(V)/V*rho _exptl_crystal_F_000 1528 _iucr_refine_instructions_details ; TITL po0019 P 21/n New: P21/c CELL 0.70930 11.1275 16.4080 21.3170 90.000 115.206 90.000 ZERR 1.00 0.0018 0.0020 0.0030 0.000 0.011 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H FE N O UNIT 132 168 4 16 44 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 10 TEMP -100.00 WGHT 0.008400 FVAR 0.65431 FE1 3 0.674161 0.262966 0.074853 11.00000 0.01422 0.02191 = 0.01632 0.00031 0.00669 -0.00034 O1 5 0.701038 0.370546 0.116546 11.00000 0.01818 0.01999 = 0.01481 0.00044 0.00721 0.00066 O2 5 0.596491 0.314633 -0.015346 11.00000 0.01587 0.02577 = 0.01882 -0.00196 0.00771 -0.00040 O3 5 0.859078 0.431804 0.323493 11.00000 0.05342 0.02320 = 0.01578 -0.00791 0.00475 0.00072 O4 5 0.889488 0.300979 0.355272 11.00000 0.08971 0.02471 = 0.01537 0.00597 0.01001 0.00732 O5 5 0.526204 0.084403 -0.156528 11.00000 0.03626 0.03918 = 0.01800 -0.00937 0.00839 0.00292 O6 5 0.405209 0.194389 -0.206956 11.00000 0.04386 0.04985 = 0.01352 0.00341 0.00072 0.00406 O7 5 0.895355 -0.066316 0.250722 11.00000 0.04122 0.02335 = 0.02151 0.00314 0.00455 0.00494 AFIX 147 H7 2 0.926445 -0.042977 0.289484 11.00000 -1.50000 AFIX 0 O8 5 0.785273 -0.119910 0.117032 11.00000 0.05854 0.02100 = 0.02629 -0.00243 0.01040 0.00561 AFIX 147 H8 2 0.819492 -0.146476 0.154194 11.00000 -1.50000 AFIX 0 N1 4 0.752971 0.211263 0.162465 11.00000 0.01268 0.02165 = 0.01608 -0.00273 0.00787 -0.00175 N2 4 0.651749 0.156933 0.036802 11.00000 0.01230 0.01959 = 0.01138 0.00102 0.00489 0.00252 N3 4 0.852556 0.269675 0.073142 11.00000 0.01833 0.01769 = 0.01686 -0.00172 0.00985 -0.00180 N4 4 0.495171 0.258345 0.075109 11.00000 0.01572 0.02660 = 0.01794 0.00126 0.01081 0.00108 C1 1 0.751101 0.390418 0.180402 11.00000 0.01480 0.01335 = 0.02057 -0.00611 0.01198 0.00099 C2 1 0.796993 0.332081 0.235345 11.00000 0.01249 0.01828 = 0.01627 -0.00024 0.00599 -0.00069 C3 1 0.794840 0.247293 0.222531 11.00000 0.02035 0.01997 = 0.01722 0.00408 0.00782 0.00018 AFIX 43 H3 2 0.827553 0.212851 0.262123 11.00000 -1.20000 AFIX 0 C4 1 0.765000 0.125536 0.156546 11.00000 0.01142 0.01690 = 0.01783 -0.00576 0.00593 -0.00238 C5 1 0.828580 0.071510 0.211737 11.00000 0.02451 0.01982 = 0.01484 -0.00082 0.00940 -0.00056 AFIX 43 H5 2 0.867757 0.091537 0.257944 11.00000 -1.20000 AFIX 0 C6 1 0.834657 -0.010026 0.199538 11.00000 0.02890 0.02058 = 0.01611 0.00444 0.00851 0.00029 C7 1 0.778280 -0.039797 0.131585 11.00000 0.03443 0.01432 = 0.02927 -0.00326 0.01425 -0.00079 C8 1 0.714718 0.013542 0.077012 11.00000 0.02465 0.02451 = 0.01051 -0.00182 0.00271 -0.00137 AFIX 43 H8A 2 0.674714 -0.006721 0.030892 11.00000 -1.20000 AFIX 0 C9 1 0.708895 0.095612 0.088895 11.00000 0.01607 0.01766 = 0.01457 0.00023 0.00632 -0.00011 C10 1 0.597764 0.138225 -0.028488 11.00000 0.01641 0.02252 = 0.02074 -0.00593 0.01188 -0.00140 AFIX 43 H10 2 0.593291 0.082082 -0.040167 11.00000 -1.20000 AFIX 0 C11 1 0.544160 0.195521 -0.084606 11.00000 0.01687 0.02770 = 0.00873 0.00364 0.00564 -0.00028 C12 1 0.552671 0.280550 -0.074799 11.00000 0.01285 0.02898 = 0.01706 0.00160 0.00688 0.00131 C13 1 0.516068 0.340272 -0.134735 11.00000 0.04964 0.03034 = 0.02694 0.00517 0.01286 0.00121 AFIX 137 H13A 2 0.420758 0.352120 -0.153924 11.00000 -1.50000 H13B 2 0.537441 0.316283 -0.170857 11.00000 -1.50000 H13C 2 0.566431 0.390879 -0.118026 11.00000 -1.50000 AFIX 0 C14 1 0.754859 0.481353 0.191406 11.00000 0.04343 0.02287 = 0.02429 0.00314 0.01479 0.00295 AFIX 137 H14A 2 0.724069 0.509131 0.146549 11.00000 -1.50000 H14B 2 0.846063 0.498287 0.221067 11.00000 -1.50000 H14C 2 0.696885 0.495729 0.213751 11.00000 -1.50000 AFIX 0 C15 1 0.484598 0.161335 -0.154713 11.00000 0.02244 0.03280 = 0.02775 0.00002 0.01507 -0.00334 C16 1 0.465753 0.041432 -0.221357 11.00000 0.04101 0.05270 = 0.02232 -0.01526 0.01301 -0.00165 AFIX 23 H16A 2 0.498529 0.063057 -0.254569 11.00000 -1.20000 H16B 2 0.368006 0.047769 -0.241765 11.00000 -1.20000 AFIX 0 C17 1 0.503098 -0.046602 -0.206122 11.00000 0.05428 0.05113 = 0.05450 -0.02796 0.02030 0.00400 AFIX 137 H17A 2 0.599808 -0.052217 -0.187546 11.00000 -1.50000 H17B 2 0.461001 -0.078442 -0.248911 11.00000 -1.50000 H17C 2 0.472886 -0.066666 -0.171956 11.00000 -1.50000 AFIX 0 C18 1 0.853183 0.351701 0.309837 11.00000 0.02644 0.02804 = 0.02356 -0.01282 0.01129 -0.00565 C19 1 0.915620 0.453818 0.396100 11.00000 0.06397 0.03543 = 0.01999 -0.01356 0.00859 -0.00505 AFIX 23 H19A 2 1.003391 0.427571 0.421114 11.00000 -1.20000 H19B 2 0.856633 0.435936 0.417502 11.00000 -1.20000 AFIX 0 C20 1 0.929852 0.545280 0.399699 11.00000 0.05812 0.03666 = 0.04077 -0.01308 0.00670 0.00218 AFIX 137 H20A 2 0.986850 0.562221 0.377459 11.00000 -1.50000 H20B 2 0.969849 0.562618 0.448322 11.00000 -1.50000 H20C 2 0.842109 0.570457 0.375656 11.00000 -1.50000 AFIX 0 C21 1 0.992617 0.247789 0.015025 11.00000 0.01785 0.03112 = 0.01473 -0.00189 0.01179 0.00008 AFIX 43 H21 2 0.998886 0.233705 -0.026706 11.00000 -1.20000 AFIX 0 C22 1 0.870312 0.249515 0.016416 11.00000 0.01042 0.03355 = 0.01030 -0.00282 0.00349 -0.00053 AFIX 43 H22 2 0.794406 0.235788 -0.024733 11.00000 -1.20000 AFIX 0 C23 1 0.963032 0.290377 0.129217 11.00000 0.02010 0.03060 = 0.01614 -0.00562 0.01141 -0.00194 AFIX 43 H23 2 0.953697 0.306895 0.169627 11.00000 -1.20000 AFIX 0 C24 1 1.088498 0.289242 0.131983 11.00000 0.01436 0.03165 = 0.01678 -0.00502 0.00765 -0.00623 AFIX 43 H24 2 1.162843 0.304014 0.173488 11.00000 -1.20000 AFIX 0 C25 1 1.106244 0.266218 0.073363 11.00000 0.00950 0.01993 = 0.01968 0.00087 0.00720 -0.00215 C26 1 1.240008 0.262160 0.074344 11.00000 0.01399 0.02159 = 0.01923 -0.00452 0.01068 -0.00326 C27 1 1.260504 0.232646 0.018644 11.00000 0.01157 0.02990 = 0.01977 -0.00589 0.00345 -0.00503 AFIX 43 H27 2 1.187327 0.213068 -0.021383 11.00000 -1.20000 AFIX 0 C28 1 0.386418 0.231517 0.020953 11.00000 0.01726 0.02817 = 0.02010 -0.01166 0.00843 -0.00409 AFIX 43 H28 2 0.396640 0.210546 -0.018033 11.00000 -1.20000 AFIX 0 C29 1 0.475869 0.283642 0.130153 11.00000 0.01133 0.03315 = 0.01227 -0.00637 0.00205 -0.00222 AFIX 43 H29 2 0.551342 0.299956 0.170548 11.00000 -1.20000 AFIX 0 C30 1 1.353540 0.287314 0.131494 11.00000 0.01876 0.03536 = 0.01909 -0.00369 0.01281 0.00197 AFIX 43 H30 2 1.346420 0.307132 0.171649 11.00000 -1.20000 AFIX 0 O31 5 0.237084 0.527061 -0.020681 11.00000 0.05117 0.04644 = 0.06388 0.01993 0.02153 -0.01397 AFIX 147 H31 2 0.273232 0.568439 -0.028357 11.00000 -1.50000 AFIX 0 C31 1 0.333612 0.465235 0.009415 11.00000 0.07819 0.04965 = 0.05285 0.01205 0.01257 -0.00639 AFIX 137 H31A 2 0.368315 0.448185 -0.023768 11.00000 -1.50000 H31B 2 0.292824 0.418419 0.021415 11.00000 -1.50000 H31C 2 0.406464 0.486336 0.051413 11.00000 -1.50000 AFIX 0 O32 5 0.158855 0.255087 0.295970 11.00000 0.06522 0.04224 = 0.05178 0.00854 0.01418 -0.00070 AFIX 147 H32 2 0.236684 0.259599 0.299506 11.00000 -1.50000 AFIX 0 C32 1 0.150084 0.186198 0.331863 11.00000 0.06192 0.04408 = 0.10182 0.02210 0.02240 -0.00689 AFIX 137 H32A 2 0.079675 0.193970 0.347385 11.00000 -1.50000 H32B 2 0.234995 0.177519 0.372201 11.00000 -1.50000 H32C 2 0.129406 0.138588 0.301282 11.00000 -1.50000 AFIX 0 O33 5 0.002476 0.510445 0.126217 11.00000 0.05933 0.05709 = 0.03034 0.00267 0.01304 -0.00733 AFIX 147 H33 2 -0.069445 0.493412 0.095161 11.00000 -1.50000 AFIX 0 C33 1 0.090664 0.530236 0.096495 11.00000 0.09205 0.16385 = 0.05330 -0.00388 0.03298 -0.03744 AFIX 137 H33A 2 0.111992 0.480870 0.077400 11.00000 -1.50000 H33B 2 0.172410 0.553366 0.132159 11.00000 -1.50000 H33C 2 0.048710 0.570189 0.059327 11.00000 -1.50000 HKLF 4 1.0 1.00 0.00 0.00 0.00 -1.00 0.00 -1.00 0.00 -1.00 REM po0019 P 21/n New: P21/c REM R1 = 0.0410 for 2722 Fo > 4sig(Fo) and 0.1101 for all 5806 data REM 454 parameters refined using 0 restraints END WGHT 0.0082 0.0000 REM Highest difference peak 0.423, deepest hole -0.378, 1-sigma level 0.053 Q1 1 0.7108 0.2461 0.0289 11.00000 0.05 0.29 Q2 1 0.5854 0.2629 0.0183 11.00000 0.05 0.28 Q3 1 0.6387 0.2537 0.1209 11.00000 0.05 0.26 Q4 1 0.9721 0.2384 0.2715 11.00000 0.05 0.25 Q5 1 0.0644 0.2360 0.3268 11.00000 0.05 0.24 Q6 1 0.7656 0.2149 0.0874 11.00000 0.05 0.24 Q7 1 0.6717 0.1999 0.0746 11.00000 0.05 0.23 Q8 1 0.9672 0.2414 0.2205 11.00000 0.05 0.22 Q9 1 0.8594 0.0646 0.1807 11.00000 0.05 0.21 Q10 1 0.8063 0.5147 0.2391 11.00000 0.05 0.20 Q11 1 0.7357 0.0977 0.1328 11.00000 0.05 0.20 Q12 1 0.1966 0.5154 0.1443 11.00000 0.05 0.19 Q13 1 0.3802 0.4522 0.0669 11.00000 0.05 0.19 Q14 1 1.0967 0.3045 0.1009 11.00000 0.05 0.19 Q15 1 0.7646 0.2985 0.1184 11.00000 0.05 0.19 Q16 1 0.7477 0.2478 0.1393 11.00000 0.05 0.19 Q17 1 0.0781 0.5393 0.0432 11.00000 0.05 0.19 Q18 1 0.1272 0.1775 0.2595 11.00000 0.05 0.19 Q19 1 0.7870 0.2586 0.0808 11.00000 0.05 0.19 Q20 1 0.7212 0.3451 0.0795 11.00000 0.05 0.19 ; _database_code_depnum_ccdc_archive 'CCDC 961712' ####################################################################### # # 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_pn011 _audit_update_record 17-Sep-13 _chemical_name_common Fe12b(bipy) _chemical_compound_source ? _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ? _audit_creation_date 17-Jan-11 _diffrn_ambient_temperature 173 _diffrn_source_type 'FR 591 generator' _diffrn_source_power 3.025 _diffrn_source_voltage 55.00 _diffrn_source_current 55.00 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'MONTEL, graded multilayered X-ray optics' _diffrn_radiation_collimation 0.20 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD; rotation images; thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_special_details ? _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.0855312 _diffrn_orient_matrix_UB_12 0.0072015 _diffrn_orient_matrix_UB_13 -0.0122332 _diffrn_orient_matrix_UB_21 -0.0321289 _diffrn_orient_matrix_UB_22 0.0305239 _diffrn_orient_matrix_UB_23 -0.0640069 _diffrn_orient_matrix_UB_31 0.0205914 _diffrn_orient_matrix_UB_32 0.0819826 _diffrn_orient_matrix_UB_33 0.0457542 loop_ _reflns_scale_group_code _reflns_scale_meas_F 1 1.0 _cell_length_a 11.12280(90) _cell_length_b 11.81290(90) _cell_length_c 13.31700(90) _cell_angle_alpha 102.2687(50) _cell_angle_beta 103.4396(41) _cell_angle_gamma 95.9468(39) _cell_volume 1641.283(220) _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5288 _cell_measurement_theta_min 3.134 _cell_measurement_theta_max 25.350 _cell_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.012000 0 1 0 0.024000 0 1 -5 0.040000 1 -4 19 0.032000 -8 0 7 0.106000 15 1 -16 0.082000 #:---------------------------------------------------------------------------- #:---------------------------ABSORPTION CORRECTION---------------------------- #:---------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type none # numerical (using crystal faces), refdelf (using DIFABS) # multi-scan (sadabs, scalepack) _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? #:---------------------------------------------------------------------------- #:------------------------REFLECTION DATA ANALYSIS---------------------------- #:---------------------------------------------------------------------------- _diffrn_reflns_number 10103 #xl _diffrn_reflns_av_R_equivalents 0.0718 #xl _diffrn_reflns_av_sigmaI/netI 0.0993 #xl _diffrn_reflns_limit_h_min -12 #xl _diffrn_reflns_limit_h_max 13 #xl _diffrn_reflns_limit_k_min -13 #xl _diffrn_reflns_limit_k_max 14 #xl _diffrn_reflns_limit_l_min -15 #xl _diffrn_reflns_limit_l_max 15 #xl _diffrn_reflns_theta_min 3.24 #xl _diffrn_reflns_theta_max 25.19 #xl _diffrn_measured_fraction_theta_max 0.984 #xl _diffrn_reflns_theta_full 25.19 #xl _diffrn_measured_fraction_theta_full 0.984 #xl #:---------------------------------------------------------------------------- #:---------------------STRUCTURE SOLUTION AND REFINEMENT---------------------- #:---------------------------------------------------------------------------- _symmetry_cell_setting triclinic #triclinic, monoclinic, orthorhombic, tetragonal #rhombohedral, trigonal, hexagonal, cubic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 5799 #xl _reflns_number_gt 3892 #xl _reflns_threshold_expression >2sigma(I) #xl _reflns_special_details ? #?# "A description of reflection data not covered by the other data #?# names. It should include details of the Friedel pairs." _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+4.6270P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none #xl _refine_ls_extinction_coef ? #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 5799 #xl _refine_ls_number_parameters 474 #xl _refine_ls_number_restraints 31 #xl _refine_ls_R_factor_all 0.1140 #xl _refine_ls_R_factor_gt 0.0699 #xl _refine_ls_wR_factor_ref 0.1853 #xl _refine_ls_wR_factor_gt 0.1644 #xl _refine_ls_goodness_of_fit_ref 1.056 #xl _refine_ls_restrained_S_all 1.064 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 0.604 #xl _refine_diff_density_min -0.734 #xl _refine_diff_density_rms 0.084 #xl _refine_special_details ? #:---------------------------------------------------------------------------- #:-----------------------------REFERENCES------------------------------------- #:---------------------------------------------------------------------------- _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution ; A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A. Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for crystal structure determination and refinement; J. Appl. Crystallogr. 1999, 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics ; ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid Plot Program for Crystal Structure Illustrations, Oak Ridge National Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ. Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau), Germany, 1995). ; _computing_publication_material ; PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version). --- T.B.Cohen, Pure Appl. Chem. 1996,68,2339-2359 (atomic masses). ; #:---------------------------------------------------------------------------- #:---------------------TABLES AND GEOMETRICAL DATA---------------------------- #:---------------------------------------------------------------------------- loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.26589(6) 0.39659(6) 0.68708(6) 0.0249(2) Uani 1 1 d . . . O1 O 0.2704(3) 0.5538(3) 0.6639(3) 0.0285(8) Uani 1 1 d . . . O2 O 0.2176(3) 0.3392(3) 0.5332(3) 0.0279(8) Uani 1 1 d . . . O3 O 0.2910(5) 0.8634(4) 0.8872(3) 0.0644(14) Uani 1 1 d . . . O4 O 0.0726(5) -0.0051(4) 0.3623(3) 0.0615(13) Uani 1 1 d . . . O5 O 0.3867(4) 0.2938(3) 1.1526(3) 0.0484(11) Uani 1 1 d . . . H5 H 0.3814 0.2288 1.1689 0.073 Uiso 1 1 calc R . . O6 O 0.3342(5) 0.0707(3) 1.0242(3) 0.0526(12) Uani 1 1 d . . . H6 H 0.3143 0.0071 0.9773 0.079 Uiso 1 1 calc R . . N1 N 0.3092(4) 0.4515(3) 0.8379(3) 0.0252(9) Uani 1 1 d . . . N2 N 0.2570(4) 0.2431(3) 0.7116(3) 0.0245(9) Uani 1 1 d . . . N3 N 0.0859(4) 0.3950(3) 0.6833(3) 0.0251(9) Uani 1 1 d . . . N4 N -0.5538(4) 0.4037(4) 0.6862(3) 0.0281(10) Uani 1 1 d . . . C1 C 0.2790(5) 0.6490(4) 0.7317(4) 0.0305(12) Uani 1 1 d . . . C2 C 0.2999(5) 0.6594(4) 0.8434(4) 0.0324(12) Uani 1 1 d . . . C3 C 0.3174(5) 0.5601(5) 0.8894(4) 0.0302(12) Uani 1 1 d . . . H3 H 0.3368 0.5755 0.9649 0.036 Uiso 1 1 calc R . . C4 C 0.3201(4) 0.3581(4) 0.8911(4) 0.0265(11) Uani 1 1 d . . . C5 C 0.3535(5) 0.3724(5) 1.0020(4) 0.0322(12) Uani 1 1 d . . . H5A H 0.3744 0.4490 1.0480 0.039 Uiso 1 1 calc R . . C6 C 0.3561(5) 0.2755(5) 1.0443(4) 0.0351(13) Uani 1 1 d . . . C7 C 0.3274(5) 0.1619(5) 0.9766(4) 0.0357(13) Uani 1 1 d . . . C8 C 0.2957(5) 0.1473(5) 0.8671(4) 0.0330(12) Uani 1 1 d . . . H8 H 0.2775 0.0705 0.8215 0.040 Uiso 1 1 calc R . . C9 C 0.2906(4) 0.2455(4) 0.8231(4) 0.0253(11) Uani 1 1 d . . . C10 C 0.2163(5) 0.1456(4) 0.6377(4) 0.0282(11) Uani 1 1 d . . . H10 H 0.2134 0.0749 0.6609 0.034 Uiso 1 1 calc R . . C11 C 0.1757(5) 0.1344(4) 0.5251(4) 0.0300(12) Uani 1 1 d . . . C12 C 0.1769(5) 0.2340(5) 0.4791(4) 0.0288(11) Uani 1 1 d . . . C13 C 0.1322(6) 0.2224(5) 0.3607(4) 0.0403(14) Uani 1 1 d . . . H13A H 0.1532 0.2984 0.3452 0.060 Uiso 1 1 calc R . . H13B H 0.0412 0.1975 0.3371 0.060 Uiso 1 1 calc R . . H13C H 0.1731 0.1640 0.3229 0.060 Uiso 1 1 calc R . . C14 C 0.2595(6) 0.7520(5) 0.6834(4) 0.0461(15) Uani 1 1 d . . . H14A H 0.2453 0.7264 0.6061 0.069 Uiso 1 1 calc R . . H14B H 0.3340 0.8126 0.7130 0.069 Uiso 1 1 calc R . . H14C H 0.1866 0.7840 0.6999 0.069 Uiso 1 1 calc R . . C15 C 0.1326(5) 0.0153(5) 0.4577(4) 0.0387(13) Uani 1 1 d . . . C16 C 0.1582(6) -0.0898(5) 0.5014(5) 0.0457(15) Uani 1 1 d . . . H16A H 0.1367 -0.1606 0.4428 0.069 Uiso 1 1 calc R . . H16B H 0.1074 -0.0977 0.5513 0.069 Uiso 1 1 calc R . . H16C H 0.2471 -0.0796 0.5385 0.069 Uiso 1 1 calc R . . C17 C 0.3092(6) 0.7725(5) 0.9160(5) 0.0426(14) Uani 1 1 d . . . C18 C 0.3402(8) 0.7819(5) 1.0346(5) 0.064(2) Uani 1 1 d . . . H18A H 0.3498 0.8642 1.0729 0.096 Uiso 1 1 calc R . . H18B H 0.4186 0.7518 1.0565 0.096 Uiso 1 1 calc R . . H18C H 0.2724 0.7356 1.0512 0.096 Uiso 1 1 calc R . . C19 C -0.1148(4) 0.4428(4) 0.6057(4) 0.0300(12) Uani 1 1 d . . . H19 H -0.1637 0.4732 0.5522 0.036 Uiso 1 1 calc R . . C20 C 0.0091(5) 0.4367(5) 0.6107(4) 0.0311(12) Uani 1 1 d . . . H20 H 0.0429 0.4639 0.5593 0.037 Uiso 1 1 calc R . . C21 C 0.0324(5) 0.3553(5) 0.7525(4) 0.0366(13) Uani 1 1 d . . . H21 H 0.0822 0.3221 0.8033 0.044 Uiso 1 1 calc R . . C22 C -0.0891(5) 0.3599(5) 0.7541(4) 0.0408(14) Uani 1 1 d . . . H22 H -0.1203 0.3325 0.8067 0.049 Uiso 1 1 calc R . . C23 C -0.1681(4) 0.4040(4) 0.6797(4) 0.0274(11) Uani 1 1 d . . . C24 C -0.3005(4) 0.4076(4) 0.6816(4) 0.0274(11) Uani 1 1 d . . . C25 C -0.3766(5) 0.4720(5) 0.6287(5) 0.0473(16) Uani 1 1 d . . . H25 H -0.3444 0.5201 0.5891 0.057 Uiso 1 1 calc R . . C26 C -0.4998(5) 0.4674(5) 0.6326(5) 0.0447(15) Uani 1 1 d . . . H26 H -0.5497 0.5128 0.5943 0.054 Uiso 1 1 calc R . . C27 C -0.4757(5) 0.3494(6) 0.7455(5) 0.0492(16) Uani 1 1 d . . . H27 H -0.5073 0.3086 0.7905 0.059 Uiso 1 1 calc R . . C28 C -0.3526(5) 0.3498(6) 0.7445(5) 0.0528(17) Uani 1 1 d . . . H28 H -0.3023 0.3092 0.7881 0.063 Uiso 1 1 calc R . . N30 N 0.4222(6) 0.1401(5) 0.2864(5) 0.0672(17) Uani 1 1 d . . . C30 C 0.4841(8) 0.0298(6) 0.4554(6) 0.070(2) Uani 1 1 d U . . C31 C 0.4486(7) 0.1974(6) 0.3881(6) 0.0633(19) Uani 1 1 d U . . H31 H 0.4462 0.2793 0.4038 0.076 Uiso 1 1 calc R . . C32 C 0.4792(7) 0.1459(6) 0.4727(6) 0.0625(18) Uani 1 1 d U . . H32 H 0.4970 0.1925 0.5436 0.075 Uiso 1 1 calc R . . C33 C 0.4667(14) -0.0259(8) 0.3513(7) 0.153(4) Uani 1 1 d U . . H33 H 0.4773 -0.1058 0.3326 0.184 Uiso 1 1 calc R . . C34 C 0.4336(16) 0.0336(9) 0.2730(8) 0.173(6) Uani 1 1 d U . . H34 H 0.4179 -0.0105 0.2014 0.208 Uiso 1 1 calc R . . O40 O 0.0845(9) -0.1264(6) 0.1672(5) 0.144(3) Uani 1 1 d . . . H40 H 0.0843 -0.0968 0.2303 0.216 Uiso 1 1 calc R . . C40 C 0.0577(11) -0.0477(5) 0.1076(4) 0.134(5) Uani 1 1 d . . . H40A H -0.0288 -0.0343 0.1025 0.201 Uiso 1 1 calc R . . H40B H 0.0674 -0.0786 0.0361 0.201 Uiso 1 1 calc R . . H40C H 0.1150 0.0265 0.1412 0.201 Uiso 1 1 calc R . . O50A O 0.0012(6) -0.3417(5) -0.0069(4) 0.099(7) Uani 0.501(14) 1 d PR A 1 H50A H 0.0319 -0.2839 0.0453 0.149 Uiso 0.501(14) 1 calc PR A 1 C50A C 0.0922(7) -0.4394(6) -0.0044(4) 0.057(5) Uani 0.501(14) 1 d PR A 1 H50B H 0.1734 -0.4048 0.0463 0.085 Uiso 0.501(14) 1 calc PR A 1 H50C H 0.1044 -0.4671 -0.0756 0.085 Uiso 0.501(14) 1 calc PR A 1 H50D H 0.0543 -0.5055 0.0175 0.085 Uiso 0.501(14) 1 calc PR A 1 O50B O 0.0012(6) -0.3417(5) -0.0069(4) 0.33(3) Uani 0.499(14) 1 d PR A 2 H50E H 0.0236 -0.2782 0.0401 0.500 Uiso 0.499(14) 1 calc PR A 2 C50B C -0.0410(6) -0.3187(5) -0.1052(4) 0.082(6) Uani 0.499(14) 1 d PR A 2 H50F H -0.1205 -0.2888 -0.1092 0.123 Uiso 0.499(14) 1 calc PR A 2 H50G H -0.0536 -0.3911 -0.1610 0.123 Uiso 0.499(14) 1 calc PR A 2 H50H H 0.0210 -0.2599 -0.1152 0.123 Uiso 0.499(14) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0206(4) 0.0279(4) 0.0298(4) 0.0102(3) 0.0086(3) 0.0085(3) O1 0.0232(18) 0.031(2) 0.036(2) 0.0144(17) 0.0105(15) 0.0070(15) O2 0.0266(18) 0.031(2) 0.0311(19) 0.0127(16) 0.0112(15) 0.0095(16) O3 0.113(4) 0.033(2) 0.049(3) 0.011(2) 0.017(3) 0.026(3) O4 0.094(4) 0.045(3) 0.034(2) 0.008(2) -0.001(2) 0.002(2) O5 0.073(3) 0.039(2) 0.034(2) 0.0138(18) 0.011(2) 0.013(2) O6 0.095(4) 0.033(2) 0.032(2) 0.0137(18) 0.013(2) 0.014(2) N1 0.020(2) 0.025(2) 0.034(2) 0.0090(19) 0.0096(18) 0.0082(18) N2 0.022(2) 0.027(2) 0.027(2) 0.0069(19) 0.0086(17) 0.0067(18) N3 0.023(2) 0.027(2) 0.027(2) 0.0080(18) 0.0058(18) 0.0071(18) N4 0.026(2) 0.032(2) 0.032(2) 0.0116(19) 0.0123(19) 0.0121(19) C1 0.024(3) 0.026(3) 0.044(3) 0.015(3) 0.007(2) 0.007(2) C2 0.035(3) 0.027(3) 0.037(3) 0.011(2) 0.008(2) 0.007(2) C3 0.027(3) 0.037(3) 0.028(3) 0.008(2) 0.009(2) 0.010(2) C4 0.021(2) 0.032(3) 0.030(3) 0.012(2) 0.008(2) 0.010(2) C5 0.038(3) 0.028(3) 0.028(3) 0.004(2) 0.007(2) 0.009(2) C6 0.043(3) 0.036(3) 0.031(3) 0.013(2) 0.010(2) 0.013(3) C7 0.046(3) 0.033(3) 0.035(3) 0.016(3) 0.012(3) 0.014(3) C8 0.044(3) 0.026(3) 0.030(3) 0.008(2) 0.009(2) 0.010(2) C9 0.017(2) 0.029(3) 0.032(3) 0.010(2) 0.010(2) 0.006(2) C10 0.027(3) 0.027(3) 0.036(3) 0.014(2) 0.012(2) 0.009(2) C11 0.032(3) 0.030(3) 0.030(3) 0.010(2) 0.009(2) 0.009(2) C12 0.025(3) 0.035(3) 0.027(3) 0.006(2) 0.007(2) 0.010(2) C13 0.052(4) 0.037(3) 0.035(3) 0.013(3) 0.012(3) 0.014(3) C14 0.070(4) 0.035(3) 0.039(3) 0.015(3) 0.015(3) 0.015(3) C15 0.045(3) 0.034(3) 0.039(3) 0.009(3) 0.012(3) 0.008(3) C16 0.056(4) 0.031(3) 0.044(3) 0.005(3) 0.005(3) 0.007(3) C17 0.056(4) 0.031(3) 0.043(3) 0.011(3) 0.014(3) 0.012(3) C18 0.116(6) 0.036(4) 0.044(4) 0.007(3) 0.021(4) 0.030(4) C19 0.021(3) 0.037(3) 0.036(3) 0.017(2) 0.007(2) 0.010(2) C20 0.025(3) 0.042(3) 0.034(3) 0.018(2) 0.011(2) 0.010(2) C21 0.027(3) 0.054(4) 0.038(3) 0.026(3) 0.009(2) 0.013(3) C22 0.034(3) 0.060(4) 0.041(3) 0.030(3) 0.017(3) 0.014(3) C23 0.021(3) 0.029(3) 0.032(3) 0.005(2) 0.008(2) 0.006(2) C24 0.023(3) 0.032(3) 0.029(3) 0.009(2) 0.008(2) 0.005(2) C25 0.033(3) 0.048(4) 0.080(5) 0.038(3) 0.027(3) 0.019(3) C26 0.029(3) 0.048(4) 0.075(4) 0.037(3) 0.022(3) 0.019(3) C27 0.037(3) 0.068(4) 0.058(4) 0.036(3) 0.019(3) 0.016(3) C28 0.032(3) 0.079(5) 0.065(4) 0.043(4) 0.018(3) 0.025(3) N30 0.098(5) 0.060(4) 0.052(4) 0.027(3) 0.019(3) 0.025(4) C30 0.109(6) 0.047(3) 0.057(3) 0.016(3) 0.021(4) 0.017(4) C31 0.083(5) 0.058(4) 0.057(4) 0.020(3) 0.021(4) 0.029(4) C32 0.082(5) 0.053(3) 0.060(4) 0.018(3) 0.024(4) 0.025(4) C33 0.324(13) 0.058(5) 0.053(4) 0.008(3) 0.008(7) 0.033(7) C34 0.368(16) 0.062(6) 0.055(5) 0.012(4) -0.006(8) 0.022(9) O40 0.297(11) 0.076(4) 0.084(5) 0.024(4) 0.090(6) 0.044(6) C40 0.253(15) 0.092(7) 0.049(5) 0.013(5) 0.038(7) -0.001(8) O50A 0.085(11) 0.131(16) 0.102(14) 0.093(13) 0.006(9) 0.020(10) C50A 0.063(9) 0.062(9) 0.038(7) -0.011(6) 0.033(6) -0.021(7) O50B 0.35(6) 0.39(7) 0.27(6) 0.07(5) 0.10(4) 0.08(5) C50B 0.093(13) 0.115(15) 0.021(7) 0.004(8) 0.004(7) -0.006(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.902(4) . ? Fe1 N2 1.905(4) . ? Fe1 O2 1.941(3) . ? Fe1 O1 1.944(3) . ? Fe1 N3 1.989(4) . ? Fe1 N4 2.001(4) 1_655 ? O1 C1 1.263(6) . ? O2 C12 1.273(6) . ? O3 C17 1.235(6) . ? O4 C15 1.249(6) . ? O5 C6 1.367(6) . ? O5 H5 0.8400 . ? O6 C7 1.360(6) . ? O6 H6 0.8400 . ? N1 C3 1.302(6) . ? N1 C4 1.433(6) . ? N2 C10 1.305(6) . ? N2 C9 1.438(6) . ? N3 C21 1.343(6) . ? N3 C20 1.346(6) . ? N4 C26 1.331(7) . ? N4 C27 1.342(7) . ? N4 Fe1 2.001(4) 1_455 ? C1 C2 1.427(7) . ? C1 C14 1.504(7) . ? C2 C3 1.445(7) . ? C2 C17 1.452(8) . ? C3 H3 0.9500 . ? C4 C9 1.398(7) . ? C4 C5 1.405(7) . ? C5 C6 1.379(7) . ? C5 H5A 0.9500 . ? C6 C7 1.407(8) . ? C7 C8 1.387(7) . ? C8 C9 1.408(7) . ? C8 H8 0.9500 . ? C10 C11 1.435(7) . ? C10 H10 0.9500 . ? C11 C12 1.437(7) . ? C11 C15 1.462(7) . ? C12 C13 1.512(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.505(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.513(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.374(7) . ? C19 C23 1.391(7) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.363(7) . ? C21 H21 0.9500 . ? C22 C23 1.392(7) . ? C22 H22 0.9500 . ? C23 C24 1.484(6) . ? C24 C25 1.369(7) . ? C24 C28 1.375(8) . ? C25 C26 1.380(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.372(8) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? N30 C34 1.256(11) . ? N30 C31 1.328(9) . ? C30 C32 1.351(9) . ? C30 C33 1.361(11) . ? C30 C30 1.498(13) 2_656 ? C31 C32 1.383(9) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.381(12) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? O40 C40 1.358(8) . ? O40 H40 0.8400 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? O50A C50A 1.6126(17) . ? O50A H50A 0.8400 . ? C50A H50B 0.9800 . ? C50A H50C 0.9800 . ? C50A H50D 0.9800 . ? O50B C50B 1.3783 . ? O50B H50E 0.8400 . ? C50B H50F 0.9800 . ? C50B H50G 0.9800 . ? C50B H50H 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 85.78(17) . . ? N1 Fe1 O2 178.62(16) . . ? N2 Fe1 O2 93.76(15) . . ? N1 Fe1 O1 93.50(16) . . ? N2 Fe1 O1 178.16(16) . . ? O2 Fe1 O1 86.93(14) . . ? N1 Fe1 N3 89.81(16) . . ? N2 Fe1 N3 90.42(16) . . ? O2 Fe1 N3 88.89(15) . . ? O1 Fe1 N3 87.88(15) . . ? N1 Fe1 N4 91.67(16) . 1_655 ? N2 Fe1 N4 92.10(16) . 1_655 ? O2 Fe1 N4 89.65(15) . 1_655 ? O1 Fe1 N4 89.61(15) . 1_655 ? N3 Fe1 N4 177.16(17) . 1_655 ? C1 O1 Fe1 127.8(3) . . ? C12 O2 Fe1 127.7(3) . . ? C6 O5 H5 109.5 . . ? C7 O6 H6 109.5 . . ? C3 N1 C4 122.0(4) . . ? C3 N1 Fe1 125.0(3) . . ? C4 N1 Fe1 112.7(3) . . ? C10 N2 C9 122.4(4) . . ? C10 N2 Fe1 125.0(3) . . ? C9 N2 Fe1 112.4(3) . . ? C21 N3 C20 115.1(4) . . ? C21 N3 Fe1 123.5(3) . . ? C20 N3 Fe1 121.4(3) . . ? C26 N4 C27 114.5(5) . . ? C26 N4 Fe1 123.3(3) . 1_455 ? C27 N4 Fe1 122.0(4) . 1_455 ? O1 C1 C2 124.3(4) . . ? O1 C1 C14 113.6(5) . . ? C2 C1 C14 122.1(5) . . ? C1 C2 C3 122.0(5) . . ? C1 C2 C17 120.7(5) . . ? C3 C2 C17 117.2(5) . . ? N1 C3 C2 126.5(5) . . ? N1 C3 H3 116.7 . . ? C2 C3 H3 116.7 . . ? C9 C4 C5 120.1(4) . . ? C9 C4 N1 114.5(4) . . ? C5 C4 N1 125.3(5) . . ? C6 C5 C4 120.2(5) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? O5 C6 C5 118.0(5) . . ? O5 C6 C7 121.8(5) . . ? C5 C6 C7 120.2(5) . . ? O6 C7 C8 123.3(5) . . ? O6 C7 C6 116.8(5) . . ? C8 C7 C6 119.9(5) . . ? C7 C8 C9 120.4(5) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C4 C9 C8 119.2(4) . . ? C4 C9 N2 114.6(4) . . ? C8 C9 N2 126.2(4) . . ? N2 C10 C11 126.6(5) . . ? N2 C10 H10 116.7 . . ? C11 C10 H10 116.7 . . ? C10 C11 C12 122.5(5) . . ? C10 C11 C15 116.7(4) . . ? C12 C11 C15 120.8(5) . . ? O2 C12 C11 123.7(5) . . ? O2 C12 C13 113.7(4) . . ? C11 C12 C13 122.6(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C1 C14 H14A 109.5 . . ? C1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O4 C15 C11 122.6(5) . . ? O4 C15 C16 116.5(5) . . ? C11 C15 C16 120.9(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 C2 124.0(5) . . ? O3 C17 C18 116.7(5) . . ? C2 C17 C18 119.3(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C23 119.5(4) . . ? C20 C19 H19 120.2 . . ? C23 C19 H19 120.2 . . ? N3 C20 C19 124.7(5) . . ? N3 C20 H20 117.7 . . ? C19 C20 H20 117.7 . . ? N3 C21 C22 123.8(5) . . ? N3 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? C21 C22 C23 120.9(5) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C19 C23 C22 115.9(5) . . ? C19 C23 C24 123.7(4) . . ? C22 C23 C24 120.5(4) . . ? C25 C24 C28 115.2(5) . . ? C25 C24 C23 124.4(5) . . ? C28 C24 C23 120.3(5) . . ? C24 C25 C26 120.4(5) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? N4 C26 C25 124.6(5) . . ? N4 C26 H26 117.7 . . ? C25 C26 H26 117.7 . . ? N4 C27 C28 123.5(5) . . ? N4 C27 H27 118.2 . . ? C28 C27 H27 118.2 . . ? C27 C28 C24 121.3(5) . . ? C27 C28 H28 119.3 . . ? C24 C28 H28 119.3 . . ? C34 N30 C31 113.6(7) . . ? C32 C30 C33 114.4(7) . . ? C32 C30 C30 122.2(8) . 2_656 ? C33 C30 C30 123.2(8) . 2_656 ? N30 C31 C32 124.4(7) . . ? N30 C31 H31 117.8 . . ? C32 C31 H31 117.8 . . ? C30 C32 C31 120.5(7) . . ? C30 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C30 C33 C34 120.0(9) . . ? C30 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? N30 C34 C33 126.8(9) . . ? N30 C34 H34 116.6 . . ? C33 C34 H34 116.6 . . ? C40 O40 H40 109.5 . . ? O40 C40 H40A 109.5 . . ? O40 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O40 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C50A O50A H50A 109.5 . . ? C50B O50B H50E 109.5 . . ? O50B C50B H50F 109.5 . . ? O50B C50B H50G 109.5 . . ? H50F C50B H50G 109.5 . . ? O50B C50B H50H 109.5 . . ? H50F C50B H50H 109.5 . . ? H50G C50B H50H 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Fe1 O1 C1 -10.0(4) . . . . ? O2 Fe1 O1 C1 168.7(4) . . . . ? N3 Fe1 O1 C1 79.7(4) . . . . ? N4 Fe1 O1 C1 -101.7(4) 1_655 . . . ? N2 Fe1 O2 C12 9.6(4) . . . . ? O1 Fe1 O2 C12 -168.7(4) . . . . ? N3 Fe1 O2 C12 -80.8(4) . . . . ? N4 Fe1 O2 C12 101.7(4) 1_655 . . . ? N2 Fe1 N1 C3 -170.8(4) . . . . ? O1 Fe1 N1 C3 7.6(4) . . . . ? N3 Fe1 N1 C3 -80.3(4) . . . . ? N4 Fe1 N1 C3 97.3(4) 1_655 . . . ? N2 Fe1 N1 C4 3.2(3) . . . . ? O1 Fe1 N1 C4 -178.5(3) . . . . ? N3 Fe1 N1 C4 93.7(3) . . . . ? N4 Fe1 N1 C4 -88.8(3) 1_655 . . . ? N1 Fe1 N2 C10 172.5(4) . . . . ? O2 Fe1 N2 C10 -6.2(4) . . . . ? N3 Fe1 N2 C10 82.8(4) . . . . ? N4 Fe1 N2 C10 -95.9(4) 1_655 . . . ? N1 Fe1 N2 C9 -2.5(3) . . . . ? O2 Fe1 N2 C9 178.8(3) . . . . ? N3 Fe1 N2 C9 -92.3(3) . . . . ? N4 Fe1 N2 C9 89.0(3) 1_655 . . . ? N1 Fe1 N3 C21 -42.7(4) . . . . ? N2 Fe1 N3 C21 43.1(4) . . . . ? O2 Fe1 N3 C21 136.9(4) . . . . ? O1 Fe1 N3 C21 -136.2(4) . . . . ? N1 Fe1 N3 C20 136.0(4) . . . . ? N2 Fe1 N3 C20 -138.2(4) . . . . ? O2 Fe1 N3 C20 -44.4(4) . . . . ? O1 Fe1 N3 C20 42.5(4) . . . . ? Fe1 O1 C1 C2 6.6(7) . . . . ? Fe1 O1 C1 C14 -170.9(3) . . . . ? O1 C1 C2 C3 2.1(8) . . . . ? C14 C1 C2 C3 179.4(5) . . . . ? O1 C1 C2 C17 179.7(5) . . . . ? C14 C1 C2 C17 -2.9(8) . . . . ? C4 N1 C3 C2 -175.7(5) . . . . ? Fe1 N1 C3 C2 -2.3(7) . . . . ? C1 C2 C3 N1 -4.4(8) . . . . ? C17 C2 C3 N1 177.9(5) . . . . ? C3 N1 C4 C9 170.9(4) . . . . ? Fe1 N1 C4 C9 -3.3(5) . . . . ? C3 N1 C4 C5 -7.3(7) . . . . ? Fe1 N1 C4 C5 178.6(4) . . . . ? C9 C4 C5 C6 -0.7(7) . . . . ? N1 C4 C5 C6 177.4(5) . . . . ? C4 C5 C6 O5 -178.7(5) . . . . ? C4 C5 C6 C7 1.1(8) . . . . ? O5 C6 C7 O6 -1.4(8) . . . . ? C5 C6 C7 O6 178.8(5) . . . . ? O5 C6 C7 C8 179.4(5) . . . . ? C5 C6 C7 C8 -0.4(8) . . . . ? O6 C7 C8 C9 -179.9(5) . . . . ? C6 C7 C8 C9 -0.8(8) . . . . ? C5 C4 C9 C8 -0.5(7) . . . . ? N1 C4 C9 C8 -178.8(4) . . . . ? C5 C4 C9 N2 179.5(4) . . . . ? N1 C4 C9 N2 1.3(6) . . . . ? C7 C8 C9 C4 1.3(7) . . . . ? C7 C8 C9 N2 -178.8(5) . . . . ? C10 N2 C9 C4 -173.9(4) . . . . ? Fe1 N2 C9 C4 1.4(5) . . . . ? C10 N2 C9 C8 6.1(7) . . . . ? Fe1 N2 C9 C8 -178.6(4) . . . . ? C9 N2 C10 C11 177.2(4) . . . . ? Fe1 N2 C10 C11 2.6(7) . . . . ? N2 C10 C11 C12 0.9(8) . . . . ? N2 C10 C11 C15 -179.4(5) . . . . ? Fe1 O2 C12 C11 -8.9(7) . . . . ? Fe1 O2 C12 C13 172.4(3) . . . . ? C10 C11 C12 O2 2.4(8) . . . . ? C15 C11 C12 O2 -177.3(5) . . . . ? C10 C11 C12 C13 -179.0(5) . . . . ? C15 C11 C12 C13 1.3(8) . . . . ? C10 C11 C15 O4 165.5(5) . . . . ? C12 C11 C15 O4 -14.7(8) . . . . ? C10 C11 C15 C16 -13.9(8) . . . . ? C12 C11 C15 C16 165.8(5) . . . . ? C1 C2 C17 O3 5.5(9) . . . . ? C3 C2 C17 O3 -176.7(6) . . . . ? C1 C2 C17 C18 -175.9(6) . . . . ? C3 C2 C17 C18 1.9(8) . . . . ? C21 N3 C20 C19 1.5(8) . . . . ? Fe1 N3 C20 C19 -177.3(4) . . . . ? C23 C19 C20 N3 0.1(8) . . . . ? C20 N3 C21 C22 -2.5(8) . . . . ? Fe1 N3 C21 C22 176.3(4) . . . . ? N3 C21 C22 C23 2.0(9) . . . . ? C20 C19 C23 C22 -0.7(8) . . . . ? C20 C19 C23 C24 179.5(5) . . . . ? C21 C22 C23 C19 -0.3(8) . . . . ? C21 C22 C23 C24 179.5(5) . . . . ? C19 C23 C24 C25 -15.5(8) . . . . ? C22 C23 C24 C25 164.7(6) . . . . ? C19 C23 C24 C28 168.7(6) . . . . ? C22 C23 C24 C28 -11.1(8) . . . . ? C28 C24 C25 C26 -5.9(9) . . . . ? C23 C24 C25 C26 178.1(5) . . . . ? C27 N4 C26 C25 5.3(9) . . . . ? Fe1 N4 C26 C25 -178.6(5) 1_455 . . . ? C24 C25 C26 N4 0.5(10) . . . . ? C26 N4 C27 C28 -5.7(9) . . . . ? Fe1 N4 C27 C28 178.1(5) 1_455 . . . ? N4 C27 C28 C24 0.3(11) . . . . ? C25 C24 C28 C27 5.5(9) . . . . ? C23 C24 C28 C27 -178.3(6) . . . . ? C34 N30 C31 C32 -3.3(14) . . . . ? C33 C30 C32 C31 5.0(13) . . . . ? C30 C30 C32 C31 -179.5(9) 2_656 . . . ? N30 C31 C32 C30 0.0(13) . . . . ? C32 C30 C33 C34 -6.6(19) . . . . ? C30 C30 C33 C34 178.0(13) 2_656 . . . ? C31 N30 C34 C33 2(2) . . . . ? C30 C33 C34 N30 4(3) . . . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #?# use this item for nonbonding or very weakly bonding contacts, e.g.: #?# Sb1 N13 3.906(13) . . ? #?# Mn Mn 3.253(2) . 2 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? #?# Do not(!) delete the #s to obtain a table header: # #D H A D - H H...A D...A D - H...A symm(A) publ_flag # #?# style: #?# N2 H721 O93 .72(4) 2.28(4) 2.868(4) 139(4) . ? #?# N2 H722 O1 .92(3) 2.44(3) 3.343(4) 171(3) 2_657 ? #?# #?# (1) This table may be copied from SHELXL97 (command HTAB D A_$n) #?# and rearranged (_geom_hbond_publ_flag missing); or #?# #?# (2) it may be copied from PLATON and rearranged; CAUTION! Check #?# symmetry operation numbers! They must(!) be identical from PLATON #?# and ACTA! "calc intra nomove" must(!) be used in PLATON runs! #?# Even then discrepancies may(!) occur! _geom_special_details ? #;Puckering parameters (\%A, \%) according to # D. Cremer, J. A. Pople, J. Am. Chem. Soc. 1975, 97, 1354--1358 #?# #?# style: #?# #?# Sb1 O2 C2 C3 O3 Q2 = 0.217(15) \f2 = 134(4) #?# O52 C12 C22 C32 C42 C52 Q = 0.577(5) \q = 3.2(6) \f = 271(9) #?# #?# or as a table: #?# #?# O5n - C1n - C2n - C3n - C4n - C5n #?# ------------------------------ #?# n Q theta phi #?# ------------------------------ #?# 11 .574(11) 6.3(11) 112(10) #?# 21 .557(10) 2.1(11) 86(22) #?# 31 .540(10) 6.2(11) 92(10) #?# 41 .571(10) 2.2(10) 221(34) #?# 51 .555(10) 10.6(10) 35(6) #?# 61 .571(10) 5.1(10) 13(13) #?# ------------------------------ #?# #?# least-squares planes be entered here, too #:---------------------------------------------------------------------------- #:--------------------------ARCHIVING AND CHECKING---------------------------- #:---------------------------------------------------------------------------- _audit_block_code Fe_L12b_Bipy_pn011_BauerW #?# style: 'Element1_El2_Ligand1_Lig2_Anion_MeasurementCode_CrystalOwner' _audit_creation_method 'form98_non/compatible with shelxl97-2' _chemical_name_systematic ? #?# style: 'lithium meso-oxolanediolate monohydrate' _chemical_formula_moiety 'C28 H26 Fe N4 O6, 0.5(C10 H8 N2), 2(C H4 O) ' #?# style: 'C36 H60 O30, 0.8(C5 H12), 4.25(H2 O)' _chemical_formula_sum 'C35 H38 Fe N5 O8' _chemical_formula_weight 712.550 #?# use the correct formula; take care of Hs not included in the atom list! _chemical_melting_point ? #?# in K! _cell_formula_units_Z 2 #?# adjust to _chemical_formula_[] _exptl_crystal_density_diffrn 1.44184 #?# include sigma (s) from: s(rho)=s(V)/V*rho _exptl_crystal_F_000 746 _iucr_refine_instructions_details ; TITL pn011 P -1 New: P-1 CELL 0.71073 11.1228 11.8129 13.3170 102.269 103.440 95.947 ZERR 2 0.0009 0.0009 0.0009 0.005 0.004 0.004 LATT 1 SFAC C H Fe N O UNIT 70 76 2 10 16 L.S. 15 FMAP 2 PLAN -20 ACTA BOND $H CONF HTAB TEMP -100 WGHT 0.055800 4.627000 FVAR 0.24994 0.50105 FE1 3 0.265894 0.396589 0.687077 11.00000 0.02061 0.02794 = 0.02978 0.01023 0.00858 0.00847 O1 5 0.270372 0.553811 0.663921 11.00000 0.02321 0.03089 = 0.03620 0.01439 0.01051 0.00702 O2 5 0.217618 0.339207 0.533245 11.00000 0.02656 0.03140 = 0.03109 0.01272 0.01120 0.00954 O3 5 0.290955 0.863375 0.887185 11.00000 0.11276 0.03299 = 0.04876 0.01078 0.01682 0.02592 O4 5 0.072631 -0.005087 0.362302 11.00000 0.09417 0.04455 = 0.03396 0.00761 -0.00068 0.00218 O5 5 0.386665 0.293769 1.152647 11.00000 0.07343 0.03912 = 0.03402 0.01379 0.01076 0.01265 AFIX 147 H5 2 0.381449 0.228834 1.168882 11.00000 -1.50000 AFIX 0 O6 5 0.334215 0.070724 1.024152 11.00000 0.09466 0.03298 = 0.03201 0.01374 0.01308 0.01425 AFIX 147 H6 2 0.314322 0.007082 0.977286 11.00000 -1.50000 AFIX 0 N1 4 0.309199 0.451507 0.837908 11.00000 0.01970 0.02480 = 0.03434 0.00904 0.00956 0.00823 N2 4 0.256966 0.243146 0.711567 11.00000 0.02188 0.02669 = 0.02692 0.00693 0.00856 0.00671 N3 4 0.085867 0.395020 0.683274 11.00000 0.02279 0.02654 = 0.02694 0.00804 0.00585 0.00712 N4 4 -0.553836 0.403685 0.686213 11.00000 0.02647 0.03173 = 0.03185 0.01156 0.01227 0.01211 C1 1 0.278952 0.648980 0.731713 11.00000 0.02428 0.02579 = 0.04444 0.01529 0.00744 0.00678 C2 1 0.299906 0.659408 0.843363 11.00000 0.03450 0.02652 = 0.03736 0.01100 0.00785 0.00707 C3 1 0.317408 0.560066 0.889442 11.00000 0.02718 0.03717 = 0.02810 0.00824 0.00883 0.00991 AFIX 47 H3 2 0.336850 0.575509 0.964891 11.00000 -1.20000 AFIX 0 C4 1 0.320095 0.358110 0.891108 11.00000 0.02136 0.03188 = 0.03015 0.01198 0.00810 0.00985 C5 1 0.353526 0.372416 1.002014 11.00000 0.03850 0.02805 = 0.02837 0.00434 0.00663 0.00874 AFIX 47 H5A 2 0.374401 0.449024 1.047978 11.00000 -1.20000 AFIX 0 C6 1 0.356109 0.275512 1.044315 11.00000 0.04287 0.03580 = 0.03086 0.01322 0.01043 0.01322 C7 1 0.327400 0.161856 0.976641 11.00000 0.04576 0.03309 = 0.03466 0.01632 0.01190 0.01446 C8 1 0.295742 0.147258 0.867114 11.00000 0.04421 0.02559 = 0.02993 0.00757 0.00896 0.00953 AFIX 47 H8 2 0.277453 0.070506 0.821518 11.00000 -1.20000 AFIX 0 C9 1 0.290553 0.245549 0.823106 11.00000 0.01740 0.02943 = 0.03223 0.00968 0.00988 0.00602 C10 1 0.216348 0.145644 0.637713 11.00000 0.02709 0.02682 = 0.03647 0.01387 0.01221 0.00853 AFIX 47 H10 2 0.213422 0.074917 0.660852 11.00000 -1.20000 AFIX 0 C11 1 0.175657 0.134372 0.525122 11.00000 0.03174 0.03026 = 0.03043 0.00964 0.00877 0.00926 C12 1 0.176887 0.233953 0.479139 11.00000 0.02524 0.03458 = 0.02698 0.00592 0.00666 0.00977 C13 1 0.132172 0.222446 0.360670 11.00000 0.05226 0.03708 = 0.03546 0.01318 0.01196 0.01411 AFIX 137 H13A 2 0.153233 0.298406 0.345161 11.00000 -1.50000 H13B 2 0.041207 0.197485 0.337103 11.00000 -1.50000 H13C 2 0.173088 0.163986 0.322941 11.00000 -1.50000 AFIX 0 C14 1 0.259513 0.751987 0.683437 11.00000 0.06950 0.03503 = 0.03852 0.01455 0.01517 0.01541 AFIX 137 H14A 2 0.245292 0.726371 0.606050 11.00000 -1.50000 H14B 2 0.334011 0.812644 0.712954 11.00000 -1.50000 H14C 2 0.186574 0.784049 0.699857 11.00000 -1.50000 AFIX 0 C15 1 0.132627 0.015311 0.457678 11.00000 0.04473 0.03356 = 0.03904 0.00944 0.01205 0.00781 C16 1 0.158197 -0.089805 0.501377 11.00000 0.05593 0.03073 = 0.04421 0.00481 0.00484 0.00703 AFIX 137 H16A 2 0.136694 -0.160610 0.442760 11.00000 -1.50000 H16B 2 0.107398 -0.097695 0.551319 11.00000 -1.50000 H16C 2 0.247150 -0.079561 0.538507 11.00000 -1.50000 AFIX 0 C17 1 0.309197 0.772532 0.916025 11.00000 0.05619 0.03059 = 0.04321 0.01073 0.01366 0.01172 C18 1 0.340224 0.781853 1.034626 11.00000 0.11613 0.03573 = 0.04370 0.00711 0.02136 0.02978 AFIX 137 H18A 2 0.349791 0.864222 1.072899 11.00000 -1.50000 H18B 2 0.418569 0.751809 1.056545 11.00000 -1.50000 H18C 2 0.272403 0.735566 1.051232 11.00000 -1.50000 AFIX 0 C19 1 -0.114792 0.442755 0.605749 11.00000 0.02146 0.03714 = 0.03589 0.01731 0.00652 0.01007 AFIX 47 H19 2 -0.163713 0.473170 0.552213 11.00000 -1.20000 AFIX 0 C20 1 0.009061 0.436695 0.610734 11.00000 0.02466 0.04215 = 0.03358 0.01833 0.01135 0.01004 AFIX 47 H20 2 0.042913 0.463870 0.559290 11.00000 -1.20000 AFIX 0 C21 1 0.032414 0.355309 0.752494 11.00000 0.02711 0.05352 = 0.03780 0.02551 0.00945 0.01279 AFIX 47 H21 2 0.082218 0.322102 0.803324 11.00000 -1.20000 AFIX 0 C22 1 -0.089083 0.359856 0.754090 11.00000 0.03392 0.06002 = 0.04145 0.02959 0.01654 0.01413 AFIX 47 H22 2 -0.120276 0.332492 0.806735 11.00000 -1.20000 AFIX 0 C23 1 -0.168072 0.404027 0.679673 11.00000 0.02091 0.02908 = 0.03200 0.00482 0.00797 0.00634 C24 1 -0.300540 0.407619 0.681579 11.00000 0.02283 0.03191 = 0.02898 0.00901 0.00780 0.00519 C25 1 -0.376614 0.471976 0.628697 11.00000 0.03274 0.04810 = 0.08043 0.03773 0.02714 0.01863 AFIX 47 H25 2 -0.344376 0.520079 0.589103 11.00000 -1.20000 AFIX 0 C26 1 -0.499845 0.467357 0.632588 11.00000 0.02862 0.04833 = 0.07453 0.03739 0.02161 0.01894 AFIX 47 H26 2 -0.549659 0.512835 0.594289 11.00000 -1.20000 AFIX 0 C27 1 -0.475683 0.349420 0.745481 11.00000 0.03702 0.06785 = 0.05767 0.03611 0.01925 0.01620 AFIX 47 H27 2 -0.507298 0.308571 0.790537 11.00000 -1.20000 AFIX 0 C28 1 -0.352575 0.349772 0.744494 11.00000 0.03167 0.07950 = 0.06549 0.04299 0.01806 0.02534 AFIX 47 H28 2 -0.302289 0.309246 0.788142 11.00000 -1.20000 AFIX 0 REM --bipy--- simu 0.02 C30 > C34 delu 0.005 C30 > C34 N30 4 0.422250 0.140073 0.286365 11.00000 0.09756 0.06002 = 0.05241 0.02679 0.01865 0.02532 C30 1 0.484068 0.029755 0.455369 11.00000 0.10909 0.04706 = 0.05669 0.01569 0.02063 0.01672 C31 1 0.448570 0.197397 0.388112 11.00000 0.08340 0.05756 = 0.05674 0.02006 0.02054 0.02916 AFIX 47 H31 2 0.446174 0.279302 0.403798 11.00000 -1.20000 AFIX 0 C32 1 0.479218 0.145886 0.472725 11.00000 0.08247 0.05325 = 0.05953 0.01791 0.02352 0.02512 AFIX 47 H32 2 0.496992 0.192507 0.543576 11.00000 -1.20000 AFIX 0 C33 1 0.466690 -0.025927 0.351338 11.00000 0.32430 0.05753 = 0.05337 0.00780 0.00790 0.03272 AFIX 47 H33 2 0.477291 -0.105774 0.332620 11.00000 -1.20000 AFIX 0 C34 1 0.433643 0.033632 0.272968 11.00000 0.36775 0.06151 = 0.05545 0.01175 -0.00628 0.02195 AFIX 47 H34 2 0.417877 -0.010530 0.201437 11.00000 -1.20000 AFIX 0 REM --MeOH 1-- O40 5 0.084543 -0.126392 0.167161 11.00000 0.29733 0.07586 = 0.08424 0.02429 0.09003 0.04354 AFIX 83 H40 2 0.084322 -0.096827 0.230314 11.00000 -1.50000 AFIX 0 C40 1 0.057686 -0.047710 0.107583 11.00000 0.25303 0.09185 = 0.04894 0.01323 0.03833 -0.00051 AFIX 137 H40A 2 -0.028764 -0.034283 0.102537 11.00000 -1.50000 H40B 2 0.067404 -0.078564 0.036052 11.00000 -1.50000 H40C 2 0.115034 0.026510 0.141156 11.00000 -1.50000 REM --MeOH 2-- free O50A O50B simu 0.02 O50A O40 simu 0.02 O50B O40 simu 0.02 C50A C40 simu 0.02 C50B C40 PART 1 O50A 5 0.001168 -0.341713 -0.006894 21.00000 0.08542 0.13092 = 0.10202 0.09272 0.00564 0.01974 AFIX 83 H50A 2 0.031855 -0.283856 0.045251 21.00000 -1.50000 AFIX 7 C50A 1 0.092234 -0.439365 -0.004442 21.00000 0.06311 0.06189 = 0.03771 -0.01113 0.03327 -0.02078 AFIX 137 H50B 2 0.173362 -0.404790 0.046282 21.00000 -1.50000 H50C 2 0.104399 -0.467108 -0.075597 21.00000 -1.50000 H50D 2 0.054283 -0.505541 0.017478 21.00000 -1.50000 AFIX 7 PART 2 O50B 5 0.001168 -0.341713 -0.006894 -21.00000 0.35007 0.38962 = 0.26962 0.06860 0.10217 0.08023 AFIX 83 H50E 2 0.023584 -0.278203 0.040079 -21.00000 -1.50000 AFIX 7 C50B 1 -0.041034 -0.318715 -0.105193 -21.00000 0.09300 0.11495 = 0.02141 0.00421 0.00426 -0.00562 AFIX 137 H50F 2 -0.120544 -0.288818 -0.109249 -21.00000 -1.50000 H50G 2 -0.053599 -0.391112 -0.161023 -21.00000 -1.50000 H50H 2 0.021035 -0.259863 -0.115201 -21.00000 -1.50000 PART 0 HKLF 4 REM pn011 P -1 New: P-1 REM R1 = 0.0699 for 3892 Fo > 4sig(Fo) and 0.1140 for all 5799 data REM 474 parameters refined using 31 restraints END WGHT 0.0558 4.6271 REM Highest difference peak 0.604, deepest hole -0.734, 1-sigma level 0.084 Q1 1 0.1915 -0.0705 0.2166 11.00000 0.05 0.60 Q2 1 0.3818 -0.0438 0.3643 11.00000 0.05 0.56 Q3 1 0.4799 0.0332 0.2722 11.00000 0.05 0.53 Q4 1 -0.0661 -0.4118 -0.0559 11.00000 0.05 0.48 Q5 1 0.0187 -0.3776 -0.0664 11.00000 0.05 0.47 Q6 1 0.5032 -0.0347 0.3424 11.00000 0.05 0.47 Q7 1 -0.5204 0.2883 0.6414 11.00000 0.05 0.44 Q8 1 -0.3879 0.2831 0.6344 11.00000 0.05 0.44 Q9 1 0.1298 -0.5028 0.0399 11.00000 0.05 0.44 Q10 1 0.1037 -0.0353 0.1418 11.00000 0.05 0.41 Q11 1 0.3426 0.0207 0.2618 11.00000 0.05 0.39 Q12 1 0.2633 0.3251 0.6331 11.00000 0.05 0.35 Q13 1 0.1582 -0.0002 0.3423 11.00000 0.05 0.35 Q14 1 -0.3350 0.4791 0.7174 11.00000 0.05 0.33 Q15 1 -0.4799 0.5064 0.7194 11.00000 0.05 0.32 Q16 1 0.0578 -0.1412 0.1642 11.00000 0.05 0.31 Q17 1 0.2091 0.4020 0.5949 11.00000 0.05 0.30 Q18 1 0.3407 -0.1393 0.3076 11.00000 0.05 0.30 Q19 1 0.0046 -0.2001 -0.1015 11.00000 0.05 0.29 Q20 1 0.2664 0.1514 0.5528 11.00000 0.05 0.29 ; _database_code_depnum_ccdc_archive 'CCDC 961713'