#------------------------------------------------------------------------------ #$Date: 2016-01-06 06:25:44 +0200 (Wed, 06 Jan 2016) $ #$Revision: 173540 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/19/1541900.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1541900 loop_ _publ_author_name 'Aromi, Guillem' 'Beavers, Christine' 'Costa, Jos\'e S\'anchez' 'Craig, Gavin A.' 'Minguez Espallargas, Guillermo' 'Orera, Alodia' 'Roubeau, Olivier' _publ_section_title ; Snapshots of a Solid-State Transformation: Coexistence of Three Phases Trapped in One Crystal. ; _journal_name_full 'Chem. Sci.' _journal_paper_doi 10.1039/C5SC04287A _journal_year 2016 _chemical_formula_moiety ; C36 H30 Fe N10 O2, C3 H6 O, 2(Cl O4) ; _chemical_formula_sum 'C39 H36 Cl2 Fe N10 O11' _chemical_formula_weight 947.53 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2015-12-22 deposited with the CCDC. 2016-01-05 downloaded from the CCDC. ; _cell_angle_alpha 71.88(3) _cell_angle_beta 69.89(3) _cell_angle_gamma 70.65(3) _cell_formula_units_Z 2 _cell_length_a 13.073(3) _cell_length_b 13.356(3) _cell_length_c 14.075(3) _cell_measurement_reflns_used 1378 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 22.7 _cell_measurement_theta_min 3.27 _cell_volume 2122.8(10) _computing_cell_refinement 'SAINT V8.27B(Bruker, 2012)' _computing_data_collection 'Apex2 v2012.10-0 (Bruker, 2012)' _computing_data_reduction SAINT _computing_molecular_graphics ; SHELXTL 5.1, XP (Sheldrick, 1994) ShelXle Rev 699 (Hubschle, 2011) ; _computing_publication_material SHELXL-2014/7 _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT (Sheldrick, 2012)' _diffrn_ambient_temperature 250(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.346 _diffrn_measured_fraction_theta_max 0.346 _diffrn_measurement_device_type 'Bruker Apex2' _diffrn_measurement_method \w _diffrn_radiation_monochromator silicon(111) _diffrn_radiation_source 'Advanced Light Source Beamline 11.3.1' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7749 _diffrn_reflns_av_unetI/netI 0.0595 _diffrn_reflns_laue_measured_fraction_full 0.346 _diffrn_reflns_laue_measured_fraction_max 0.346 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2413 _diffrn_reflns_point_group_measured_fraction_full 0.346 _diffrn_reflns_point_group_measured_fraction_max 0.346 _diffrn_reflns_theta_full 27.706 _diffrn_reflns_theta_max 27.719 _diffrn_reflns_theta_min 3.273 _exptl_absorpt_coefficient_mu 0.694 _exptl_absorpt_correction_T_max 0.745584 _exptl_absorpt_correction_T_min 0.524839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'TWINABS 2012/1 (Sheldrick, 2012)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.482 _exptl_crystal_description block _exptl_crystal_F_000 976 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.070 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.301 _refine_diff_density_min -0.308 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 561 _refine_ls_number_reflns 2413 _refine_ls_number_restraints 897 _refine_ls_restrained_S_all 0.923 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0685 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1561P)^2^+0.0246P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1821 _refine_ls_wR_factor_ref 0.2212 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1516 _reflns_number_total 2413 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5sc04287a2.cif _cod_data_source_block Stage2_Final _cod_original_cell_volume 2123.0(10) _cod_database_code 1541900 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.934 _shelx_estimated_absorpt_t_max 0.966 _shelx_res_file ; Final.res created by SHELXL-2014/7 REM Solution 1 R1 0.256 Rweak 0.023, Alpha = 0.1567 in P-1 REM Formula: C45 N7 O6 Cl Fe TITL samp3 in P-1 Sample folder: srj128c5 CELL 0.77490 13.0732 13.3559 14.0755 71.884 69.895 70.651 ZERR 2.00 0.00261 0.00267 0.00282 0.0300 0.0300 0.0300 LATT 1 SFAC C H N O CL FE DISP C -0.00202 0.00197 13.60 DISP H 0.00000 0.00000 0.67 DISP N -0.00306 0.00403 23.92 DISP O -0.00415 0.00737 40.17 DISP Cl 0.14076 0.18956 859.19 DISP Fe 0.20639 0.99298 4412.23 UNIT 78 72 20 22 4 2 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -23.000 SIZE 0.1 0.07 0.05 !dark red block L.S. 10 BOND $H ACTA RIGU FMAP 2 PLAN 20 HTAB HTAB N1 O1_2a HTAB N1 O1_4b HTAB N5 O2 HTAB N6 Cl1_1a HTAB N6 O2_1a HTAB N6 O4_1a HTAB N6 Cl1_3b HTAB N6 O1_3b HTAB N6 O2_3b HTAB N10 O3 EQIV $1 -x+1, -y+2, -z HTAB_1a C25_0 O2_$1 HTAB_3b C25_0 O2_$1 HTAB_3b C25_0 O4_$1 HTAB C26 N4_$1 HTAB C26 N5_$1 SADI_ClO4 0.01 Cl1 O1 Cl1 O2 Cl1 O3 Cl1 O4 SADI_ClO4 0.02 O1 O2 O1 O3 O1 O4 O2 O3 O2 O4 O3 O4 EADP O3_4 O3_2 EADP Cl1_1 Cl1_3 WGHT 0.156100 0.024600 BASF 0.51860 FVAR 0.51480 0.49837 0.45189 FE1 6 0.498095 0.752445 0.249529 11.00000 0.04220 0.04029 = 0.04665 -0.01190 -0.01466 -0.00912 O1 4 0.132720 0.915643 0.702111 11.00000 0.07997 0.13311 = 0.09392 -0.06406 0.00062 -0.01438 O2 4 0.835918 0.640007 -0.102210 11.00000 0.06477 0.10953 = 0.05672 -0.02570 -0.01766 -0.03181 N1 3 0.250618 0.808170 0.425580 11.00000 0.04595 0.04976 = 0.06106 -0.00766 -0.01434 -0.00999 AFIX 43 H1D 2 0.209410 0.787888 0.401554 11.00000 -1.20000 AFIX 0 N2 3 0.362327 0.803998 0.380548 11.00000 0.04778 0.04043 = 0.05019 -0.00773 -0.01263 -0.01151 N3 3 0.571424 0.807881 0.328684 11.00000 0.04957 0.03205 = 0.04585 -0.00899 -0.01351 -0.01044 N4 3 0.676167 0.737787 0.159771 11.00000 0.04676 0.05103 = 0.04928 -0.01604 -0.01361 -0.00970 N5 3 0.749917 0.697938 0.074293 11.00000 0.05034 0.04817 = 0.03718 -0.00913 -0.01243 -0.00880 AFIX 43 H5B 2 0.731950 0.675352 0.031926 11.00000 -1.20000 AFIX 0 N6 3 0.398056 0.987796 0.112952 11.00000 0.07096 0.04864 = 0.05805 -0.00261 -0.01414 -0.01160 AFIX 43 H6B 2 0.421186 1.027220 0.136228 11.00000 -1.20000 AFIX 0 N7 3 0.422282 0.879694 0.139268 11.00000 0.05721 0.04722 = 0.05228 -0.00614 -0.01709 -0.00904 N8 3 0.441520 0.675465 0.172291 11.00000 0.04105 0.05190 = 0.05277 -0.01762 -0.01374 -0.00920 N9 3 0.540985 0.579493 0.318160 11.00000 0.04437 0.03803 = 0.06286 -0.00919 -0.01960 -0.00544 N10 3 0.597093 0.513733 0.386461 11.00000 0.05909 0.04705 = 0.06209 -0.00263 -0.02487 -0.00233 AFIX 43 H10A 2 0.623978 0.535780 0.422761 11.00000 -1.20000 AFIX 0 C1 1 0.103507 0.933140 0.804227 11.00000 0.13378 0.09587 = 0.08279 -0.05159 0.00292 -0.02165 AFIX 137 H1A 2 0.155012 0.879252 0.841988 11.00000 -1.50000 H1B 2 0.027250 0.926640 0.840236 11.00000 -1.50000 H1C 2 0.108414 1.005416 0.799829 11.00000 -1.50000 AFIX 0 C2 1 -0.060488 0.914884 0.721228 11.00000 0.07099 0.10257 = 0.10288 -0.04412 0.00672 -0.01128 AFIX 43 H2A 2 -0.085649 0.936976 0.784398 11.00000 -1.20000 AFIX 0 C3 1 0.053286 0.897939 0.667423 11.00000 0.07200 0.06867 = 0.07713 -0.02671 -0.00229 -0.00611 C4 1 -0.135229 0.899663 0.682927 11.00000 0.07164 0.10301 = 0.11555 -0.03904 -0.00686 -0.00659 AFIX 43 H4A 2 -0.211603 0.911548 0.720139 11.00000 -1.20000 AFIX 0 C5 1 -0.100549 0.866479 0.588705 11.00000 0.05709 0.08192 = 0.11275 -0.02520 -0.01082 -0.00856 AFIX 43 H5A 2 -0.151513 0.855409 0.561753 11.00000 -1.20000 AFIX 0 C6 1 0.014705 0.850860 0.537271 11.00000 0.05818 0.09301 = 0.09741 -0.03813 -0.01280 -0.00480 AFIX 43 H6A 2 0.040599 0.829654 0.473606 11.00000 -1.20000 AFIX 0 C7 1 0.091219 0.864947 0.575139 11.00000 0.05449 0.06193 = 0.07871 -0.02040 -0.00857 -0.00357 C8 1 0.211419 0.848974 0.514648 11.00000 0.05148 0.04506 = 0.06612 -0.01305 -0.01690 -0.00052 C9 1 0.299749 0.867941 0.528184 11.00000 0.05598 0.05002 = 0.05756 -0.01271 -0.01081 -0.00975 AFIX 43 H9A 2 0.299783 0.894252 0.582833 11.00000 -1.20000 AFIX 0 C10 1 0.394131 0.839998 0.442494 11.00000 0.05386 0.03164 = 0.04759 -0.00421 -0.01419 -0.01014 C11 1 0.510313 0.841114 0.416748 11.00000 0.05051 0.03381 = 0.04096 -0.01223 -0.01156 -0.00774 C12 1 0.557477 0.872878 0.470018 11.00000 0.06239 0.05318 = 0.06262 -0.02861 -0.01604 -0.01150 AFIX 43 H12A 2 0.511961 0.896151 0.531185 11.00000 -1.20000 AFIX 0 C13 1 0.670803 0.872737 0.438398 11.00000 0.06367 0.06330 = 0.06621 -0.02295 -0.02316 -0.01397 AFIX 43 H13A 2 0.703288 0.892641 0.477645 11.00000 -1.20000 AFIX 0 C14 1 0.732968 0.841539 0.345666 11.00000 0.05642 0.05885 = 0.06783 -0.02190 -0.02175 -0.01328 AFIX 43 H14A 2 0.808761 0.843917 0.317029 11.00000 -1.20000 AFIX 0 C15 1 0.679747 0.806664 0.296412 11.00000 0.04928 0.03980 = 0.04215 -0.00288 -0.01361 -0.01525 C16 1 0.738517 0.763548 0.199326 11.00000 0.04603 0.04368 = 0.04281 -0.00611 -0.01697 -0.01041 C17 1 0.852481 0.744322 0.140799 11.00000 0.05036 0.06513 = 0.04584 -0.01410 -0.01228 -0.01465 AFIX 43 H17A 2 0.912473 0.759537 0.151400 11.00000 -1.20000 AFIX 0 C18 1 0.855250 0.700278 0.068155 11.00000 0.04694 0.06061 = 0.04370 -0.01343 -0.01137 -0.01123 C19 1 0.952939 0.663838 -0.021004 11.00000 0.05224 0.07439 = 0.04886 -0.01814 -0.00974 -0.01634 C20 1 1.058700 0.655177 -0.014844 11.00000 0.05389 0.09487 = 0.04896 -0.01633 -0.00896 -0.02316 AFIX 43 H20A 2 1.066365 0.673471 0.041245 11.00000 -1.20000 AFIX 0 C21 1 1.155081 0.619218 -0.091765 11.00000 0.06115 0.14211 = 0.06340 -0.03606 -0.00456 -0.01959 AFIX 43 H21A 2 1.227084 0.616009 -0.089332 11.00000 -1.20000 AFIX 0 C22 1 1.141637 0.588846 -0.170648 11.00000 0.07008 0.13097 = 0.05720 -0.03118 -0.00761 -0.01585 AFIX 43 H22A 2 1.205620 0.564466 -0.222345 11.00000 -1.20000 AFIX 0 C23 1 1.035261 0.593231 -0.176090 11.00000 0.07323 0.11700 = 0.06682 -0.03558 -0.00989 -0.01661 AFIX 43 H23A 2 1.026781 0.570992 -0.229498 11.00000 -1.20000 AFIX 0 C24 1 0.943200 0.631596 -0.099731 11.00000 0.06357 0.08203 = 0.05150 -0.02339 -0.01119 -0.02399 C25 1 0.821515 0.616437 -0.185911 11.00000 0.09160 0.12423 = 0.07160 -0.03554 -0.02592 -0.03941 AFIX 137 H25A 2 0.742085 0.637789 -0.182657 11.00000 -1.50000 H25B 2 0.850415 0.538938 -0.182991 11.00000 -1.50000 H25C 2 0.862025 0.656192 -0.250301 11.00000 -1.50000 AFIX 0 C26 1 0.335115 1.028287 0.047695 11.00000 0.08724 0.05823 = 0.07476 0.00157 -0.03483 -0.00196 AFIX 43 H26A 2 0.307063 1.102446 0.020230 11.00000 -1.20000 AFIX 0 C27 1 0.318466 0.943999 0.027696 11.00000 0.09551 0.07293 = 0.07805 -0.00309 -0.04157 -0.00870 AFIX 43 H27A 2 0.277643 0.946670 -0.016887 11.00000 -1.20000 AFIX 0 C28 1 0.374289 0.852042 0.086778 11.00000 0.05659 0.06163 = 0.04358 -0.00701 -0.01362 -0.01108 C29 1 0.386245 0.736645 0.100420 11.00000 0.05981 0.06392 = 0.05746 -0.01643 -0.02029 -0.00990 C30 1 0.347722 0.685769 0.053870 11.00000 0.05892 0.08828 = 0.07082 -0.02509 -0.02997 -0.01270 AFIX 43 H30A 2 0.306826 0.727676 0.005193 11.00000 -1.20000 AFIX 0 C31 1 0.367311 0.578159 0.076508 11.00000 0.07686 0.08665 = 0.08983 -0.03497 -0.03331 -0.01839 AFIX 43 H31A 2 0.341827 0.544972 0.042134 11.00000 -1.20000 AFIX 0 C32 1 0.423389 0.515160 0.148281 11.00000 0.07883 0.06715 = 0.08769 -0.03112 -0.03271 -0.02135 AFIX 43 H32A 2 0.436922 0.438944 0.164399 11.00000 -1.20000 AFIX 0 C33 1 0.459288 0.565709 0.196021 11.00000 0.04862 0.04750 = 0.06598 -0.02190 -0.01714 -0.00895 C34 1 0.517912 0.515098 0.275661 11.00000 0.04112 0.04419 = 0.06132 -0.01578 -0.01051 -0.00850 C35 1 0.558550 0.404117 0.325442 11.00000 0.07235 0.04318 = 0.07750 -0.01156 -0.02326 -0.00829 AFIX 43 H35A 2 0.552662 0.340866 0.313852 11.00000 -1.20000 AFIX 0 C36 1 0.606675 0.411274 0.392040 11.00000 0.07267 0.04816 = 0.07462 -0.00677 -0.02654 -0.00344 AFIX 43 H36A 2 0.642170 0.351676 0.436364 11.00000 -1.20000 AFIX 0 PART 1 RESI 1 CLO4 CL1 5 0.482702 1.156909 0.230640 21.00000 0.06957 O1 4 0.571696 1.189503 0.233708 21.00000 0.20264 O2 4 0.444583 1.221004 0.144687 21.00000 0.10653 O3 4 0.394100 1.167215 0.319061 21.00000 0.21881 O4 4 0.521307 1.049839 0.221291 21.00000 0.08207 RESI 2 CLO4 CL1 5 0.091342 0.739511 0.264038 31.00000 0.06629 O1 4 0.182996 0.740277 0.291868 31.00000 0.09807 O2 4 0.095948 0.795951 0.162787 31.00000 0.11305 O3 4 0.091611 0.632711 0.272494 31.00000 0.14420 O4 4 -0.006997 0.784923 0.331195 31.00000 0.09490 PART 2 RESI 4 CLO4 CL1 5 0.086557 0.714588 0.289344 -31.00000 0.06645 O1 4 0.181273 0.687773 0.325107 -31.00000 0.09085 O2 4 0.080520 0.813802 0.218606 -31.00000 0.16879 O3 4 0.095202 0.635893 0.239724 -31.00000 0.14420 O4 4 -0.008250 0.720567 0.372438 -31.00000 0.10540 RESI 3 CLO4 CL1 5 0.463803 1.169467 0.214498 -21.00000 0.06957 O1 4 0.450933 1.064821 0.264692 -21.00000 0.12920 O2 4 0.429131 1.201343 0.124782 -21.00000 0.13815 O3 4 0.577832 1.164952 0.188932 -21.00000 0.23842 O4 4 0.402319 1.238736 0.280586 -21.00000 0.09369 PART 0 RESI 0 C39 1 0.808269 0.607077 0.567979 11.00000 0.10345 0.09620 = 0.10278 -0.04313 -0.06037 -0.00317 AFIX 33 H39A 2 0.887830 0.575053 0.562404 11.00000 -1.50000 H39B 2 0.794917 0.685515 0.544199 11.00000 -1.50000 H39C 2 0.765524 0.589172 0.639783 11.00000 -1.50000 AFIX 0 C37 1 0.868256 0.497282 0.434368 11.00000 0.07222 0.17586 = 0.13907 -0.10054 -0.02512 -0.02413 AFIX 33 H37A 2 0.938166 0.484156 0.451335 11.00000 -1.50000 H37B 2 0.852242 0.428294 0.444149 11.00000 -1.50000 H37C 2 0.875143 0.536341 0.362629 11.00000 -1.50000 AFIX 0 C38 1 0.773278 0.564562 0.504672 11.00000 0.06924 0.07793 = 0.05250 -0.00923 -0.02374 -0.02547 O3 4 0.680300 0.590120 0.497399 11.00000 0.07233 0.10961 = 0.08720 -0.03870 -0.03603 -0.01251 HKLF 5 REM samp3 in P-1 Sample folder: srj128c5 REM R1 = 0.0685 for 1516 Fo > 4sig(Fo) and 0.1147 for all 2413 data REM 561 parameters refined using 897 restraints END WGHT 0.1561 0.0246 REM Instructions for potential hydrogen bonds HTAB N1 O1_2 HTAB N1 O1_4 HTAB N5 O2 HTAB N6 Cl1_1 HTAB N6 O4_1 HTAB N6 Cl1_3 HTAB N6 O1_3 HTAB N6 O2_3 HTAB N10 O3 HTAB C9 O1 EQIV $2 -x+1, -y+2, -z+1 HTAB_1 C12_0 O3_$2 EQIV $3 x+1, y, z HTAB_2 C14_0 O4_$3 HTAB_4 C14_0 O4_$3 HTAB_1 C25_0 O2_$1 HTAB_3 C25_0 O2_$1 HTAB_3 C25_0 O4_$1 EQIV $4 -x+1, -y+1, -z HTAB_4 C25_0 O3_$4 HTAB C26 N5_$1 EQIV $5 x, y-1, z HTAB_1 C35_0 O1_$5 REM Highest difference peak 0.301, deepest hole -0.308, 1-sigma level 0.057 Q1 1 0.5986 1.0785 0.1942 11.00000 0.05 0.30 Q2 1 0.3935 1.0772 0.3210 11.00000 0.05 0.27 Q3 1 0.1843 0.6285 0.2745 11.00000 0.05 0.27 Q4 1 0.4465 1.2207 0.3061 11.00000 0.05 0.25 Q5 1 0.1726 0.7534 0.1094 11.00000 0.05 0.25 Q6 1 0.4581 1.2427 0.2811 11.00000 0.05 0.24 Q7 1 -0.0046 0.5996 0.4285 11.00000 0.05 0.23 Q8 1 0.3722 1.1973 0.3153 11.00000 0.05 0.22 Q9 1 -0.0036 0.6483 0.3704 11.00000 0.05 0.22 Q10 1 0.7445 0.5174 0.6313 11.00000 0.05 0.20 Q11 1 0.6071 1.0882 0.2681 11.00000 0.05 0.20 Q12 1 0.1412 0.8229 0.2945 11.00000 0.05 0.20 Q13 1 0.1754 0.6387 0.1437 11.00000 0.05 0.20 Q14 1 1.2551 0.6839 -0.1568 11.00000 0.05 0.20 Q15 1 0.6781 0.6777 0.2356 11.00000 0.05 0.19 Q16 1 1.2423 0.6191 -0.1949 11.00000 0.05 0.19 Q17 1 0.3574 0.6239 0.3900 11.00000 0.05 0.19 Q18 1 0.2885 0.5988 0.3410 11.00000 0.05 0.19 Q19 1 0.1639 0.5662 0.3312 11.00000 0.05 0.19 Q20 1 1.3185 0.6573 -0.1201 11.00000 0.05 0.18 ; _shelx_res_checksum 98957 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.49810(13) 0.75244(11) 0.24953(15) 0.0421(6) Uani 1 1 d . U . . . O1 O 0.1327(10) 0.9156(11) 0.7021(11) 0.103(4) Uani 1 1 d . U . . . O2 O 0.8359(7) 0.6400(8) -0.1022(8) 0.072(3) Uani 1 1 d . U . . . N1 N 0.2506(8) 0.8082(7) 0.4256(9) 0.054(3) Uani 1 1 d . U . . . H1D H 0.2094 0.7879 0.4016 0.065 Uiso 1 1 calc R U . . . N2 N 0.3623(8) 0.8040(7) 0.3805(9) 0.047(2) Uani 1 1 d . U . . . N3 N 0.5714(7) 0.8079(6) 0.3287(8) 0.042(2) Uani 1 1 d . U . . . N4 N 0.6762(7) 0.7378(7) 0.1598(9) 0.048(2) Uani 1 1 d . U . . . N5 N 0.7499(8) 0.6979(7) 0.0743(9) 0.046(2) Uani 1 1 d . U . . . H5B H 0.7320 0.6754 0.0319 0.055 Uiso 1 1 calc R U . . . N6 N 0.3981(9) 0.9878(8) 0.1130(10) 0.063(3) Uani 1 1 d . U . . . H6B H 0.4212 1.0272 0.1362 0.076 Uiso 1 1 calc R U . . . N7 N 0.4223(9) 0.8797(7) 0.1393(10) 0.054(3) Uani 1 1 d . U . . . N8 N 0.4415(7) 0.6755(7) 0.1723(9) 0.047(2) Uani 1 1 d . U . . . N9 N 0.5410(8) 0.5795(7) 0.3182(10) 0.049(2) Uani 1 1 d . U . . . N10 N 0.5971(8) 0.5137(7) 0.3865(9) 0.059(3) Uani 1 1 d . U . . . H10A H 0.6240 0.5358 0.4228 0.071 Uiso 1 1 calc R U . . . C1 C 0.1035(18) 0.9331(14) 0.8042(16) 0.107(6) Uani 1 1 d . U . . . H1A H 0.1550 0.8793 0.8420 0.161 Uiso 1 1 calc R U . . . H1B H 0.0273 0.9266 0.8402 0.161 Uiso 1 1 calc R U . . . H1C H 0.1084 1.0054 0.7998 0.161 Uiso 1 1 calc R U . . . C2 C -0.0605(14) 0.9149(14) 0.7212(16) 0.098(5) Uani 1 1 d . U . . . H2A H -0.0856 0.9370 0.7844 0.118 Uiso 1 1 calc R U . . . C3 C 0.0533(13) 0.8979(11) 0.6674(14) 0.078(4) Uani 1 1 d . U . . . C4 C -0.1352(15) 0.8997(14) 0.6829(17) 0.102(5) Uani 1 1 d . U . . . H4A H -0.2116 0.9115 0.7201 0.123 Uiso 1 1 calc R U . . . C5 C -0.1005(12) 0.8665(12) 0.5887(15) 0.089(4) Uani 1 1 d . U . . . H5A H -0.1515 0.8554 0.5618 0.106 Uiso 1 1 calc R U . . . C6 C 0.0147(12) 0.8509(13) 0.5373(15) 0.085(4) Uani 1 1 d . U . . . H6A H 0.0406 0.8297 0.4736 0.102 Uiso 1 1 calc R U . . . C7 C 0.0912(11) 0.8649(10) 0.5751(13) 0.069(3) Uani 1 1 d . U . . . C8 C 0.2114(10) 0.8490(9) 0.5146(12) 0.057(3) Uani 1 1 d . U . . . C9 C 0.2997(10) 0.8679(9) 0.5282(12) 0.057(3) Uani 1 1 d . U . . . H9A H 0.2998 0.8943 0.5828 0.068 Uiso 1 1 calc R U . . . C10 C 0.3941(10) 0.8400(8) 0.4425(11) 0.046(2) Uani 1 1 d . U . . . C11 C 0.5103(9) 0.8411(7) 0.4167(10) 0.042(2) Uani 1 1 d . U . . . C12 C 0.5575(10) 0.8729(9) 0.4700(11) 0.057(3) Uani 1 1 d . U . . . H12A H 0.5120 0.8962 0.5312 0.068 Uiso 1 1 calc R U . . . C13 C 0.6708(10) 0.8727(10) 0.4384(12) 0.061(3) Uani 1 1 d . U . . . H13A H 0.7033 0.8926 0.4776 0.073 Uiso 1 1 calc R U . . . C14 C 0.7330(10) 0.8415(9) 0.3457(11) 0.058(3) Uani 1 1 d . U . . . H14A H 0.8088 0.8439 0.3170 0.070 Uiso 1 1 calc R U . . . C15 C 0.6797(9) 0.8067(8) 0.2964(10) 0.044(2) Uani 1 1 d . U . . . C16 C 0.7385(10) 0.7635(8) 0.1993(11) 0.044(2) Uani 1 1 d . U . . . C17 C 0.8525(10) 0.7443(9) 0.1408(11) 0.053(3) Uani 1 1 d . U . . . H17A H 0.9125 0.7595 0.1514 0.064 Uiso 1 1 calc R U . . . C18 C 0.8552(9) 0.7003(10) 0.0682(11) 0.051(3) Uani 1 1 d . U . . . C19 C 0.9529(10) 0.6638(10) -0.0210(12) 0.058(3) Uani 1 1 d . U . . . C20 C 1.0587(10) 0.6552(11) -0.0148(12) 0.066(4) Uani 1 1 d . U . . . H20A H 1.0664 0.6735 0.0412 0.079 Uiso 1 1 calc R U . . . C21 C 1.1551(13) 0.6192(15) -0.0918(15) 0.091(5) Uani 1 1 d . U . . . H21A H 1.2271 0.6160 -0.0893 0.109 Uiso 1 1 calc R U . . . C22 C 1.1416(13) 0.5888(14) -0.1706(15) 0.089(5) Uani 1 1 d . U . . . H22A H 1.2056 0.5645 -0.2223 0.106 Uiso 1 1 calc R U . . . C23 C 1.0353(13) 0.5932(14) -0.1761(15) 0.086(4) Uani 1 1 d . U . . . H23A H 1.0268 0.5710 -0.2295 0.104 Uiso 1 1 calc R U . . . C24 C 0.9432(11) 0.6316(11) -0.0997(13) 0.063(3) Uani 1 1 d . U . . . C25 C 0.8215(14) 0.6164(14) -0.1859(15) 0.088(5) Uani 1 1 d . U . . . H25A H 0.7421 0.6378 -0.1827 0.132 Uiso 1 1 calc R U . . . H25B H 0.8504 0.5389 -0.1830 0.132 Uiso 1 1 calc R U . . . H25C H 0.8620 0.6562 -0.2503 0.132 Uiso 1 1 calc R U . . . C26 C 0.3351(13) 1.0283(11) 0.0477(14) 0.078(4) Uani 1 1 d . U . . . H26A H 0.3071 1.1024 0.0202 0.094 Uiso 1 1 calc R U . . . C27 C 0.3185(14) 0.9440(11) 0.0277(14) 0.084(5) Uani 1 1 d . U . . . H27A H 0.2776 0.9467 -0.0169 0.101 Uiso 1 1 calc R U . . . C28 C 0.3743(11) 0.8520(10) 0.0868(12) 0.056(3) Uani 1 1 d . U . . . C29 C 0.3862(11) 0.7366(10) 0.1004(13) 0.060(3) Uani 1 1 d . U . . . C30 C 0.3477(11) 0.6858(12) 0.0539(13) 0.069(4) Uani 1 1 d . U . . . H30A H 0.3068 0.7277 0.0052 0.083 Uiso 1 1 calc R U . . . C31 C 0.3673(13) 0.5782(12) 0.0765(15) 0.078(4) Uani 1 1 d . U . . . H31A H 0.3418 0.5450 0.0421 0.094 Uiso 1 1 calc R U . . . C32 C 0.4234(11) 0.5152(10) 0.1483(14) 0.071(4) Uani 1 1 d . U . . . H32A H 0.4369 0.4389 0.1644 0.085 Uiso 1 1 calc R U . . . C33 C 0.4593(10) 0.5657(9) 0.1960(12) 0.052(3) Uani 1 1 d . U . . . C34 C 0.5179(10) 0.5151(9) 0.2757(12) 0.049(3) Uani 1 1 d . U . . . C35 C 0.5586(11) 0.4041(9) 0.3254(12) 0.066(4) Uani 1 1 d . U . . . H35A H 0.5527 0.3409 0.3139 0.079 Uiso 1 1 calc R U . . . C36 C 0.6067(12) 0.4113(10) 0.3920(13) 0.068(4) Uani 1 1 d . U . . . H36A H 0.6422 0.3517 0.4364 0.082 Uiso 1 1 calc R U . . . Cl1_1 Cl 0.4827(10) 1.1569(8) 0.2306(10) 0.0696(14) Uiso 0.50(3) 1 d D . P A 1 O1_1 O 0.5717(19) 1.190(2) 0.234(3) 0.20(2) Uiso 0.50(3) 1 d D . P A 1 O2_1 O 0.445(2) 1.2210(18) 0.1447(18) 0.107(10) Uiso 0.50(3) 1 d D . P A 1 O3_1 O 0.394(2) 1.167(3) 0.3191(18) 0.22(2) Uiso 0.50(3) 1 d D . P A 1 O4_1 O 0.521(2) 1.0498(10) 0.2213(19) 0.082(8) Uiso 0.50(3) 1 d D . P A 1 Cl1_2 Cl 0.0913(9) 0.7395(11) 0.2640(11) 0.066(3) Uiso 0.45(3) 1 d D . P B 1 O1_2 O 0.1830(14) 0.740(2) 0.292(2) 0.098(9) Uiso 0.45(3) 1 d D . P B 1 O2_2 O 0.096(2) 0.7960(19) 0.1628(16) 0.113(11) Uiso 0.45(3) 1 d D . P B 1 O3_2 O 0.092(2) 0.6327(13) 0.272(3) 0.144(5) Uiso 0.45(3) 1 d D . P B 1 O4_2 O -0.0070(14) 0.785(2) 0.3312(19) 0.095(10) Uiso 0.45(3) 1 d D . P B 1 Cl1_4 Cl 0.0866(8) 0.7146(10) 0.2893(11) 0.066(3) Uiso 0.55(3) 1 d D . P B 2 O1_4 O 0.1813(12) 0.6878(19) 0.3251(18) 0.091(7) Uiso 0.55(3) 1 d D . P B 2 O2_4 O 0.081(2) 0.8138(13) 0.219(2) 0.169(14) Uiso 0.55(3) 1 d D . P B 2 O3_4 O 0.095(2) 0.6359(15) 0.2397(19) 0.144(5) Uiso 0.55(3) 1 d D . P B 2 O4_4 O -0.0083(12) 0.721(2) 0.3724(15) 0.105(9) Uiso 0.55(3) 1 d D . P B 2 Cl1_3 Cl 0.4638(10) 1.1695(8) 0.2145(9) 0.0696(14) Uiso 0.50(3) 1 d D . P A 2 O1_3 O 0.451(3) 1.0648(13) 0.265(2) 0.129(12) Uiso 0.50(3) 1 d D . P A 2 O2_3 O 0.429(3) 1.201(2) 0.1248(16) 0.138(14) Uiso 0.50(3) 1 d D . P A 2 O3_3 O 0.5778(12) 1.165(2) 0.189(3) 0.24(3) Uiso 0.50(3) 1 d D . P A 2 O4_3 O 0.4023(17) 1.2387(17) 0.2806(17) 0.094(9) Uiso 0.50(3) 1 d D . P A 2 C39 C 0.8083(13) 0.6071(13) 0.5680(16) 0.092(6) Uani 1 1 d . U . . . H39A H 0.8878 0.5751 0.5624 0.139 Uiso 1 1 calc R U . . . H39B H 0.7949 0.6855 0.5442 0.139 Uiso 1 1 calc R U . . . H39C H 0.7655 0.5892 0.6398 0.139 Uiso 1 1 calc R U . . . C37 C 0.8683(12) 0.4973(17) 0.4344(18) 0.116(8) Uani 1 1 d . U . . . H37A H 0.9382 0.4842 0.4513 0.174 Uiso 1 1 calc R U . . . H37B H 0.8522 0.4283 0.4441 0.174 Uiso 1 1 calc R U . . . H37C H 0.8751 0.5363 0.3626 0.174 Uiso 1 1 calc R U . . . C38 C 0.7733(12) 0.5646(12) 0.5047(13) 0.064(4) Uani 1 1 d . U . . . O3 O 0.6803(8) 0.5901(9) 0.4974(9) 0.084(4) Uani 1 1 d . U . . . 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 0.0422(8) 0.0403(8) 0.0467(13) -0.0119(7) -0.0147(8) -0.0091(7) O1 0.080(6) 0.133(8) 0.094(10) -0.064(7) 0.001(6) -0.014(6) O2 0.065(4) 0.110(7) 0.057(8) -0.026(6) -0.018(5) -0.032(5) N1 0.046(4) 0.050(5) 0.061(7) -0.008(4) -0.014(4) -0.010(4) N2 0.048(4) 0.040(4) 0.050(5) -0.008(4) -0.013(3) -0.012(4) N3 0.050(3) 0.032(4) 0.046(5) -0.009(3) -0.014(3) -0.010(3) N4 0.047(4) 0.051(4) 0.049(6) -0.016(4) -0.014(3) -0.010(4) N5 0.050(4) 0.048(5) 0.037(6) -0.009(4) -0.012(4) -0.009(4) N6 0.071(7) 0.049(4) 0.058(8) -0.003(4) -0.014(6) -0.012(4) N7 0.057(5) 0.047(4) 0.052(6) -0.006(3) -0.017(5) -0.009(4) N8 0.041(5) 0.052(3) 0.053(6) -0.018(3) -0.014(4) -0.009(4) N9 0.044(5) 0.038(3) 0.063(6) -0.009(3) -0.020(5) -0.005(3) N10 0.059(6) 0.047(4) 0.062(7) -0.003(4) -0.025(5) -0.002(4) C1 0.134(13) 0.096(10) 0.083(11) -0.052(9) 0.003(9) -0.022(11) C2 0.071(6) 0.103(10) 0.103(11) -0.044(9) 0.007(6) -0.011(7) C3 0.072(6) 0.069(7) 0.077(8) -0.027(6) -0.002(5) -0.006(6) C4 0.072(7) 0.103(11) 0.116(13) -0.039(9) -0.007(7) -0.007(7) C5 0.057(6) 0.082(9) 0.113(12) -0.025(8) -0.011(6) -0.009(6) C6 0.058(5) 0.093(9) 0.097(10) -0.038(8) -0.013(6) -0.005(6) C7 0.054(5) 0.062(7) 0.079(8) -0.020(6) -0.009(4) -0.004(5) C8 0.051(4) 0.045(6) 0.066(7) -0.013(5) -0.017(4) -0.001(4) C9 0.056(5) 0.050(6) 0.058(7) -0.013(5) -0.011(4) -0.010(5) C10 0.054(4) 0.032(5) 0.048(7) -0.004(4) -0.014(4) -0.010(4) C11 0.051(4) 0.034(4) 0.041(6) -0.012(4) -0.012(4) -0.008(4) C12 0.062(5) 0.053(6) 0.063(8) -0.029(5) -0.016(5) -0.011(5) C13 0.064(5) 0.063(6) 0.066(8) -0.023(6) -0.023(5) -0.014(6) C14 0.056(5) 0.059(6) 0.068(8) -0.022(5) -0.022(5) -0.013(5) C15 0.049(4) 0.040(5) 0.042(6) -0.003(4) -0.014(4) -0.015(4) C16 0.046(4) 0.044(5) 0.043(6) -0.006(4) -0.017(4) -0.010(4) C17 0.050(5) 0.065(6) 0.046(7) -0.014(5) -0.012(4) -0.015(5) C18 0.047(4) 0.061(6) 0.044(7) -0.013(5) -0.011(4) -0.011(4) C19 0.052(4) 0.074(7) 0.049(7) -0.018(5) -0.010(4) -0.016(5) C20 0.054(5) 0.095(9) 0.049(9) -0.016(7) -0.009(5) -0.023(6) C21 0.061(6) 0.142(13) 0.063(10) -0.036(9) -0.005(6) -0.020(7) C22 0.070(6) 0.131(11) 0.057(11) -0.031(9) -0.008(6) -0.016(7) C23 0.073(5) 0.117(11) 0.067(9) -0.036(8) -0.010(5) -0.017(7) C24 0.064(5) 0.082(8) 0.051(8) -0.023(6) -0.011(4) -0.024(5) C25 0.092(9) 0.124(11) 0.072(12) -0.036(10) -0.026(9) -0.039(11) C26 0.087(9) 0.058(5) 0.075(10) 0.002(5) -0.035(8) -0.002(6) C27 0.096(9) 0.073(5) 0.078(11) -0.003(5) -0.042(9) -0.009(6) C28 0.057(7) 0.062(4) 0.044(8) -0.007(4) -0.014(6) -0.011(4) C29 0.060(6) 0.064(4) 0.057(8) -0.016(4) -0.020(6) -0.010(5) C30 0.059(7) 0.088(6) 0.071(10) -0.025(6) -0.030(7) -0.013(6) C31 0.077(9) 0.087(6) 0.090(10) -0.035(6) -0.033(8) -0.018(6) C32 0.079(8) 0.067(6) 0.088(10) -0.031(6) -0.033(7) -0.021(6) C33 0.049(6) 0.048(4) 0.066(7) -0.022(4) -0.017(5) -0.009(4) C34 0.041(6) 0.044(4) 0.061(7) -0.016(4) -0.011(5) -0.009(4) C35 0.072(8) 0.043(4) 0.077(9) -0.012(4) -0.023(7) -0.008(5) C36 0.073(8) 0.048(5) 0.075(10) -0.007(5) -0.027(7) -0.003(5) C39 0.103(10) 0.096(9) 0.103(14) -0.043(9) -0.060(10) -0.003(9) C37 0.072(8) 0.176(17) 0.139(16) -0.101(15) -0.025(8) -0.024(10) C38 0.069(6) 0.078(7) 0.053(10) -0.009(6) -0.024(6) -0.025(6) O3 0.072(5) 0.110(7) 0.087(10) -0.039(6) -0.036(6) -0.013(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' N N -0.0031 0.0040 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0074 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Cl Cl 0.1408 0.1896 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Fe Fe 0.2064 0.9930 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N3 Fe1 N8 172.0(3) N3 Fe1 N7 113.3(4) N8 Fe1 N7 73.7(4) N3 Fe1 N9 99.3(4) N8 Fe1 N9 73.6(4) N7 Fe1 N9 147.3(4) N3 Fe1 N2 74.4(4) N8 Fe1 N2 110.0(4) N7 Fe1 N2 92.4(4) N9 Fe1 N2 98.1(4) N3 Fe1 N4 73.7(4) N8 Fe1 N4 101.9(4) N7 Fe1 N4 98.4(4) N9 Fe1 N4 88.8(4) N2 Fe1 N4 148.0(4) C3 O1 C1 120.1(16) C24 O2 C25 119.3(12) N2 N1 C8 111.3(12) N2 N1 H1D 124.4 C8 N1 H1D 124.4 C10 N2 N1 105.5(11) C10 N2 Fe1 114.3(8) N1 N2 Fe1 140.1(9) C15 N3 C11 117.8(11) C15 N3 Fe1 121.6(8) C11 N3 Fe1 120.5(8) C16 N4 N5 105.2(10) C16 N4 Fe1 115.9(9) N5 N4 Fe1 138.6(8) C18 N5 N4 108.1(11) C18 N5 H5B 125.9 N4 N5 H5B 125.9 C26 N6 N7 112.2(14) C26 N6 H6B 123.9 N7 N6 H6B 123.9 C28 N7 N6 105.0(10) C28 N7 Fe1 117.2(8) N6 N7 Fe1 137.4(10) C29 N8 C33 119.8(12) C29 N8 Fe1 119.6(8) C33 N8 Fe1 120.6(8) N10 N9 C34 106.5(9) N10 N9 Fe1 137.3(9) C34 N9 Fe1 115.8(8) C36 N10 N9 111.2(13) C36 N10 H10A 124.4 N9 N10 H10A 124.4 O1 C1 H1A 109.5 O1 C1 H1B 109.5 H1A C1 H1B 109.5 O1 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 C4 C2 C3 120.5(19) C4 C2 H2A 119.8 C3 C2 H2A 119.8 C7 C3 C2 120.3(18) C7 C3 O1 117.2(15) C2 C3 O1 122.5(16) C2 C4 C5 121.3(17) C2 C4 H4A 119.3 C5 C4 H4A 119.3 C6 C5 C4 116.1(18) C6 C5 H5A 122.0 C4 C5 H5A 122.0 C7 C6 C5 123.3(17) C7 C6 H6A 118.3 C5 C6 H6A 118.3 C6 C7 C3 118.5(15) C6 C7 C8 119.9(15) C3 C7 C8 121.5(16) C9 C8 N1 107.0(12) C9 C8 C7 131.8(15) N1 C8 C7 121.2(13) C8 C9 C10 106.4(14) C8 C9 H9A 126.8 C10 C9 H9A 126.8 N2 C10 C9 109.9(12) N2 C10 C11 118.4(11) C9 C10 C11 131.7(13) N3 C11 C12 120.9(12) N3 C11 C10 112.4(11) C12 C11 C10 126.7(12) C11 C12 C13 122.8(13) C11 C12 H12A 118.6 C13 C12 H12A 118.6 C14 C13 C12 116.1(14) C14 C13 H13A 121.9 C12 C13 H13A 121.9 C13 C14 C15 117.9(14) C13 C14 H14A 121.0 C15 C14 H14A 121.0 N3 C15 C14 124.3(12) N3 C15 C16 112.0(11) C14 C15 C16 123.8(12) N4 C16 C17 111.9(12) N4 C16 C15 116.6(12) C17 C16 C15 131.4(12) C18 C17 C16 104.1(12) C18 C17 H17A 128.0 C16 C17 H17A 128.0 C17 C18 N5 110.5(11) C17 C18 C19 129.9(13) N5 C18 C19 119.3(12) C24 C19 C20 119.2(12) C24 C19 C18 124.7(12) C20 C19 C18 115.9(14) C19 C20 C21 120.5(16) C19 C20 H20A 119.7 C21 C20 H20A 119.7 C22 C21 C20 118.5(16) C22 C21 H21A 120.8 C20 C21 H21A 120.8 C21 C22 C23 121.8(15) C21 C22 H22A 119.1 C23 C22 H22A 119.1 C24 C23 C22 117.3(18) C24 C23 H23A 121.4 C22 C23 H23A 121.4 C19 C24 O2 117.4(12) C19 C24 C23 122.7(15) O2 C24 C23 120.0(16) O2 C25 H25A 109.5 O2 C25 H25B 109.5 H25A C25 H25B 109.5 O2 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 N6 C26 C27 107.1(12) N6 C26 H26A 126.4 C27 C26 H26A 126.4 C26 C27 C28 105.3(16) C26 C27 H27A 127.4 C28 C27 H27A 127.4 N7 C28 C27 110.3(13) N7 C28 C29 117.6(11) C27 C28 C29 132.1(16) N8 C29 C30 118.6(12) N8 C29 C28 111.7(14) C30 C29 C28 129.6(13) C31 C30 C29 120.9(13) C31 C30 H30A 119.5 C29 C30 H30A 119.5 C30 C31 C32 121.2(18) C30 C31 H31A 119.4 C32 C31 H31A 119.4 C33 C32 C31 117.8(13) C33 C32 H32A 121.1 C31 C32 H32A 121.1 C32 C33 N8 121.5(12) C32 C33 C34 127.0(11) N8 C33 C34 111.5(12) N9 C34 C35 108.1(12) N9 C34 C33 118.3(10) C35 C34 C33 133.5(13) C36 C35 C34 104.2(12) C36 C35 H35A 127.9 C34 C35 H35A 127.9 N10 C36 C35 110.0(12) N10 C36 H36A 125.0 C35 C36 H36A 125.0 O4_1 Cl1_1 O3_1 110.3(10) O4_1 Cl1_1 O1_1 108.3(10) O3_1 Cl1_1 O1_1 111.3(10) O4_1 Cl1_1 O2_1 108.9(9) O3_1 Cl1_1 O2_1 108.6(10) O1_1 Cl1_1 O2_1 109.5(10) O2_2 Cl1_2 O4_2 110.6(9) O2_2 Cl1_2 O1_2 110.5(10) O4_2 Cl1_2 O1_2 109.3(9) O2_2 Cl1_2 O3_2 108.5(10) O4_2 Cl1_2 O3_2 108.0(10) O1_2 Cl1_2 O3_2 109.8(10) O4_4 Cl1_4 O2_4 110.1(9) O4_4 Cl1_4 O3_4 110.2(10) O2_4 Cl1_4 O3_4 108.5(10) O4_4 Cl1_4 O1_4 109.1(9) O2_4 Cl1_4 O1_4 109.4(10) O3_4 Cl1_4 O1_4 109.5(9) O4_3 Cl1_3 O2_3 111.7(10) O4_3 Cl1_3 O3_3 110.1(10) O2_3 Cl1_3 O3_3 109.5(10) O4_3 Cl1_3 O1_3 109.2(9) O2_3 Cl1_3 O1_3 108.8(10) O3_3 Cl1_3 O1_3 107.4(10) C38 C39 H39A 109.5 C38 C39 H39B 109.5 H39A C39 H39B 109.5 C38 C39 H39C 109.5 H39A C39 H39C 109.5 H39B C39 H39C 109.5 C38 C37 H37A 109.5 C38 C37 H37B 109.5 H37A C37 H37B 109.5 C38 C37 H37C 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 O3 C38 C39 123.5(14) O3 C38 C37 120.9(16) C39 C38 C37 115.0(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 N3 2.104(10) Fe1 N8 2.130(11) Fe1 N7 2.140(10) Fe1 N9 2.170(9) Fe1 N2 2.181(10) Fe1 N4 2.210(10) O1 C3 1.40(2) O1 C1 1.43(2) O2 C24 1.381(18) O2 C25 1.39(2) N1 N2 1.367(15) N1 C8 1.389(18) N1 H1D 0.8700 N2 C10 1.344(16) N3 C15 1.326(15) N3 C11 1.341(15) N4 C16 1.308(17) N4 N5 1.386(14) N5 C18 1.360(17) N5 H5B 0.8700 N6 C26 1.31(2) N6 N7 1.329(14) N6 H6B 0.8700 N7 C28 1.311(19) N8 C29 1.346(17) N8 C33 1.356(15) N9 N10 1.329(15) N9 C34 1.343(18) N10 C36 1.312(18) N10 H10A 0.8700 C1 H1A 0.9700 C1 H1B 0.9700 C1 H1C 0.9700 C2 C4 1.36(3) C2 C3 1.40(2) C2 H2A 0.9400 C3 C7 1.38(2) C4 C5 1.41(3) C4 H4A 0.9400 C5 C6 1.40(2) C5 H5A 0.9400 C6 C7 1.37(2) C6 H6A 0.9400 C7 C8 1.487(19) C8 C9 1.35(2) C9 C10 1.438(19) C9 H9A 0.9400 C10 C11 1.439(17) C11 C12 1.346(17) C12 C13 1.392(19) C12 H12A 0.9400 C13 C14 1.386(19) C13 H13A 0.9400 C14 C15 1.389(18) C14 H14A 0.9400 C15 C16 1.505(18) C16 C17 1.414(18) C17 C18 1.314(19) C17 H17A 0.9400 C18 C19 1.520(19) C19 C24 1.36(2) C19 C20 1.38(2) C20 C21 1.41(2) C20 H20A 0.9400 C21 C22 1.37(3) C21 H21A 0.9400 C22 C23 1.40(3) C22 H22A 0.9400 C23 C24 1.38(2) C23 H23A 0.9400 C25 H25A 0.9700 C25 H25B 0.9700 C25 H25C 0.9700 C26 C27 1.34(3) C26 H26A 0.9400 C27 C28 1.386(19) C27 H27A 0.9400 C28 C29 1.45(2) C29 C30 1.37(2) C30 C31 1.33(2) C30 H30A 0.9400 C31 C32 1.36(2) C31 H31A 0.9400 C32 C33 1.36(2) C32 H32A 0.9400 C33 C34 1.441(19) C34 C35 1.435(17) C35 C36 1.34(2) C35 H35A 0.9400 C36 H36A 0.9400 Cl1_1 O4_1 1.382(8) Cl1_1 O3_1 1.385(9) Cl1_1 O1_1 1.388(9) Cl1_1 O2_1 1.390(9) Cl1_2 O2_2 1.381(9) Cl1_2 O4_2 1.385(9) Cl1_2 O1_2 1.387(9) Cl1_2 O3_2 1.393(9) Cl1_4 O4_4 1.381(9) Cl1_4 O2_4 1.385(9) Cl1_4 O3_4 1.389(9) Cl1_4 O1_4 1.392(8) Cl1_3 O4_3 1.377(9) Cl1_3 O2_3 1.383(9) Cl1_3 O3_3 1.393(9) Cl1_3 O1_3 1.393(9) C39 C38 1.45(2) C39 H39A 0.9700 C39 H39B 0.9700 C39 H39C 0.9700 C37 C38 1.52(2) C37 H37A 0.9700 C37 H37B 0.9700 C37 H37C 0.9700 C38 O3 1.180(16) 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 N1 H1D O1_2 0.87 2.01 2.81(2) 152.4 . N1 H1D O1_4 0.87 2.14 2.94(2) 153.8 . N5 H5B O2 0.87 2.00 2.595(15) 124.6 . N6 H6B Cl1_1 0.87 2.92 3.783(19) 175.0 . N6 H6B O2_1 0.87 2.75 3.55(3) 153.4 . N6 H6B O4_1 0.87 2.19 2.99(2) 153.4 . N6 H6B Cl1_3 0.87 2.75 3.613(19) 172.0 . N6 H6B O1_3 0.87 2.20 2.99(3) 150.7 . N6 H6B O2_3 0.87 2.32 3.07(3) 145.5 . N10 H10A O3 0.87 1.88 2.749(18) 177.3 . C25 H25A O2_1 0.97 2.55 3.40(3) 146.6 2_675 C25 H25A O2_3 0.97 2.63 3.39(3) 134.8 2_675 C25 H25A O4_3 0.97 2.55 3.38(2) 143.4 2_675 C26 H26A N4 0.94 2.75 3.554(17) 143.4 2_675 C26 H26A N5 0.94 2.57 3.503(15) 173.1 2_675