#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:29:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179113 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/75/4307512.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_4307512
loop_
_publ_author_name
'Martin Bröring'
'Serguei Prikhodovski'
'Carsten D. Brandt'
'Esther Cónsul Tejero'
'Silke Köhler'
'Clemens Pietzonka'
_publ_section_title
;
Cyanide-Promoted Demetalation of TrpyNiNCO: A Route to Sensitive
Metallotripyrrins of CoII, FeII, and MnII
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              917
_journal_page_last               925
_journal_paper_doi               10.1021/ic062009t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C54 H68 Fe2 N8 O3'
_chemical_formula_weight         988.86
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.337(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.9641(14)
_cell_length_b                   14.0552(16)
_cell_length_c                   19.4466(14)
_cell_measurement_reflns_used    7225
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      1.8
_cell_volume                     5160.9(8)
_computing_cell_refinement       'STOE Wincell (X-Area)'
_computing_data_collection       'STOE WinXpose (X-Area)'
_computing_data_reduction        'STOE WinIntegrate (X-Area)'
_computing_publication_material  'WinGx-Version 1.70.00'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'IPDS1 (Stoe)'
_diffrn_measurement_method       phi-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1634
_diffrn_reflns_av_sigmaI/netI    0.2412
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38292
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.85613
_exptl_absorpt_correction_T_min  0.78860
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Face-indexed absorption correction'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.583
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         9064
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.582
_refine_ls_R_factor_all          0.1495
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0655
_reflns_number_gt                3442
_reflns_number_total             9418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062009tsi20061019_115859_5.cif
_cod_data_source_block           sp30eca
_cod_database_code               4307512
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
C1 C 0.1733(2) 0.9204(3) 0.8488(2) 0.0437(13) Uani 1 1 d . . .
H1A H 0.1599 0.9402 0.8941 0.066 Uiso 1 1 calc R . .
H1B H 0.1831 0.8519 0.8493 0.066 Uiso 1 1 calc R . .
H1C H 0.1344 0.9343 0.8134 0.066 Uiso 1 1 calc R . .
C2 C 0.2373(2) 0.9727(3) 0.8329(2) 0.0298(10) Uani 1 1 d . . .
C3 C 0.2796(2) 0.9542(3) 0.7763(2) 0.0368(11) Uani 1 1 d . . .
C4 C 0.3321(2) 1.0205(3) 0.7798(2) 0.0365(11) Uani 1 1 d . . .
C5 C 0.3231(2) 1.0795(3) 0.8403(2) 0.0297(11) Uani 1 1 d . . .
C6 C 0.3648(2) 1.1513(3) 0.8666(2) 0.0359(11) Uani 1 1 d . . .
H6 H 0.4047 1.1650 0.8423 0.043 Uiso 1 1 calc R . .
C7 C 0.3574(2) 1.2087(3) 0.9248(2) 0.0319(11) Uani 1 1 d . A .
C8 C 0.4038(2) 1.2856(3) 0.9458(2) 0.0397(12) Uani 1 1 d . . .
C9 C 0.3761(2) 1.3285(3) 1.0013(2) 0.0344(11) Uani 1 1 d . A .
C10 C 0.3144(2) 1.2759(3) 1.0138(2) 0.0276(10) Uani 1 1 d . . .
C11 C 0.2707(2) 1.2949(3) 1.0671(2) 0.0306(11) Uani 1 1 d . A .
H11 H 0.2865 1.3451 1.0975 0.037 Uiso 1 1 calc R . .
C12 C 0.2096(2) 1.2523(3) 1.0815(2) 0.0265(10) Uani 1 1 d . . .
C13 C 0.1659(2) 1.2750(3) 1.1368(2) 0.0295(10) Uani 1 1 d . A .
C14 C 0.1095(2) 1.2151(3) 1.1292(2) 0.0299(10) Uani 1 1 d . . .
C15 C 0.1202(2) 1.1545(3) 1.0705(2) 0.0300(11) Uani 1 1 d . A .
C16 C 0.0717(2) 1.0760(3) 1.0446(2) 0.0373(12) Uani 1 1 d . . .
H16A H 0.0360 1.1010 1.0095 0.056 Uiso 1 1 calc R A .
H16B H 0.0481 1.0496 1.0831 0.056 Uiso 1 1 calc R . .
H16C H 0.0991 1.0260 1.0242 0.056 Uiso 1 1 calc R . .
C17 C 0.2691(2) 0.8730(3) 0.7244(2) 0.0525(14) Uani 1 1 d . . .
H17A H 0.3151 0.8411 0.7206 0.063 Uiso 1 1 calc R . .
H17B H 0.2362 0.8257 0.7416 0.063 Uiso 1 1 calc R . .
C18 C 0.2404(3) 0.9061(4) 0.6557(2) 0.0766(17) Uani 1 1 d . . .
H18A H 0.1951 0.9385 0.6593 0.115 Uiso 1 1 calc R . .
H18B H 0.2330 0.8515 0.6245 0.115 Uiso 1 1 calc R . .
H18C H 0.2739 0.9504 0.6374 0.115 Uiso 1 1 calc R . .
C19 C 0.3891(2) 1.0351(4) 0.7330(2) 0.0550(14) Uani 1 1 d . . .
H19A H 0.3929 0.9785 0.7041 0.083 Uiso 1 1 calc R . .
H19B H 0.4343 1.0460 0.7606 0.083 Uiso 1 1 calc R . .
H19C H 0.3775 1.0905 0.7034 0.083 Uiso 1 1 calc R . .
C20 C 0.4699(9) 1.3062(11) 0.9165(9) 0.068(2) Uani 0.681(7) 1 d PU A 1
H20A H 0.4932 1.2451 0.9071 0.081 Uiso 0.681(7) 1 calc PR A 1
H20B H 0.5014 1.3407 0.9515 0.081 Uiso 0.681(7) 1 calc PR A 1
C21 C 0.4635(4) 1.3631(6) 0.8520(4) 0.069(2) Uani 0.681(7) 1 d PU A 1
H21A H 0.4264 1.3359 0.8194 0.104 Uiso 0.681(7) 1 calc PR A 1
H21B H 0.5088 1.3622 0.8314 0.104 Uiso 0.681(7) 1 calc PR A 1
H21C H 0.4512 1.4289 0.8626 0.104 Uiso 0.681(7) 1 calc PR A 1
C20' C 0.4673(16) 1.327(2) 0.906(2) 0.068(2) Uani 0.319(7) 1 d PU A 2
H20C H 0.4572 1.3189 0.8557 0.082 Uiso 0.319(7) 1 calc PR A 2
H20D H 0.4746 1.3952 0.9166 0.082 Uiso 0.319(7) 1 calc PR A 2
C21' C 0.5252(9) 1.2758(12) 0.9297(9) 0.068(2) Uani 0.319(7) 1 d PU A 2
H21D H 0.5361 1.2874 0.9793 0.102 Uiso 0.319(7) 1 calc PR A 2
H21E H 0.5656 1.2951 0.9050 0.102 Uiso 0.319(7) 1 calc PR A 2
H21F H 0.5157 1.2079 0.9219 0.102 Uiso 0.319(7) 1 calc PR A 2
C22 C 0.4039(2) 1.4156(3) 1.0390(2) 0.0487(13) Uani 1 1 d . . .
H22A H 0.4563 1.4149 1.0419 0.058 Uiso 1 1 calc R A .
H22B H 0.3897 1.4140 1.0867 0.058 Uiso 1 1 calc R . .
C23 C 0.3772(3) 1.5072(3) 1.0044(3) 0.0627(16) Uani 1 1 d . A .
H23A H 0.3965 1.5134 0.9595 0.094 Uiso 1 1 calc R . .
H23B H 0.3925 1.5615 1.0337 0.094 Uiso 1 1 calc R . .
H23C H 0.3254 1.5059 0.9975 0.094 Uiso 1 1 calc R . .
C24 C 0.1813(2) 1.3507(3) 1.1905(2) 0.0455(13) Uani 1 1 d . . .
H24A H 0.1411 1.3565 1.2184 0.068 Uiso 1 1 calc R A .
H24B H 0.1890 1.4116 1.1678 0.068 Uiso 1 1 calc R . .
H24C H 0.2239 1.3335 1.2203 0.068 Uiso 1 1 calc R . .
C25 C 0.0464(2) 1.2106(3) 1.1697(2) 0.0380(12) Uani 1 1 d . A .
H25A H 0.0588 1.2396 1.2157 0.046 Uiso 1 1 calc R . .
H25B H 0.0342 1.1431 1.1769 0.046 Uiso 1 1 calc R . .
C26 C -0.0180(2) 1.2615(4) 1.1345(3) 0.0682(16) Uani 1 1 d . . .
H26A H -0.0070 1.3290 1.1292 0.102 Uiso 1 1 calc R A .
H26B H -0.0579 1.2549 1.1628 0.102 Uiso 1 1 calc R . .
H26C H -0.0305 1.2332 1.0890 0.102 Uiso 1 1 calc R . .
C27 C 0.1023(2) 1.1796(3) 0.8609(2) 0.0412(11) Uani 1 1 d . . .
C28 C 0.2872(2) 1.0710(3) 1.1788(2) 0.0382(12) Uani 1 1 d . . .
H28A H 0.3280 1.0420 1.2056 0.057 Uiso 1 1 calc R . .
H28B H 0.2788 1.1346 1.1971 0.057 Uiso 1 1 calc R . .
H28C H 0.2969 1.0762 1.1303 0.057 Uiso 1 1 calc R . .
C29 C 0.2235(2) 1.0109(3) 1.1840(2) 0.0287(10) Uani 1 1 d . . .
C30 C 0.1716(2) 1.0240(3) 1.2337(2) 0.0319(11) Uani 1 1 d . . .
C31 C 0.1226(2) 0.9548(3) 1.2210(2) 0.0313(10) Uani 1 1 d . . .
C32 C 0.1449(2) 0.8992(3) 1.1643(2) 0.0294(10) Uani 1 1 d . . .
C33 C 0.1120(2) 0.8206(3) 1.1343(2) 0.0313(10) Uani 1 1 d . . .
H33 H 0.0697 0.8015 1.1528 0.038 Uiso 1 1 calc R . .
C34 C 0.1328(2) 0.7645(3) 1.0796(2) 0.0267(10) Uani 1 1 d . . .
C35 C 0.0976(2) 0.6791(3) 1.0559(2) 0.0273(10) Uani 1 1 d . . .
C36 C 0.1339(2) 0.6434(3) 1.0034(2) 0.0307(10) Uani 1 1 d . . .
C37 C 0.1908(2) 0.7069(3) 0.9960(2) 0.0269(10) Uani 1 1 d . . .
C38 C 0.2414(2) 0.6965(3) 0.9470(2) 0.0315(11) Uani 1 1 d . . .
H38 H 0.2351 0.6421 0.9181 0.038 Uiso 1 1 calc R . .
C39 C 0.2967(2) 0.7521(3) 0.9353(2) 0.0308(11) Uani 1 1 d . . .
C40 C 0.3463(2) 0.7408(3) 0.8820(2) 0.0340(11) Uani 1 1 d . . .
C41 C 0.3921(2) 0.8155(3) 0.8904(2) 0.0344(11) Uani 1 1 d . . .
C42 C 0.3712(2) 0.8699(3) 0.9488(2) 0.0300(11) Uani 1 1 d . . .
C43 C 0.4097(2) 0.9551(3) 0.9782(2) 0.0432(13) Uani 1 1 d . . .
H43A H 0.3762 0.9978 0.9982 0.065 Uiso 1 1 calc R . .
H43B H 0.4318 0.9884 0.9416 0.065 Uiso 1 1 calc R . .
H43C H 0.4462 0.9351 1.0142 0.065 Uiso 1 1 calc R . .
C44 C 0.1738(2) 1.1024(3) 1.28669(19) 0.0370(10) Uani 1 1 d . . .
H44A H 0.1262 1.1084 1.3034 0.044 Uiso 1 1 calc R . .
H44B H 0.1843 1.1631 1.2639 0.044 Uiso 1 1 calc R . .
C45 C 0.2274(2) 1.0883(3) 1.3482(2) 0.0485(13) Uani 1 1 d . . .
H45A H 0.2181 1.0279 1.3708 0.073 Uiso 1 1 calc R . .
H45B H 0.2238 1.1408 1.3809 0.073 Uiso 1 1 calc R . .
H45C H 0.2751 1.0872 1.3327 0.073 Uiso 1 1 calc R . .
C46 C 0.0562(2) 0.9358(3) 1.2554(2) 0.0539(14) Uani 1 1 d . . .
H46A H 0.0528 0.9813 1.2932 0.081 Uiso 1 1 calc R . .
H46B H 0.0576 0.8709 1.2739 0.081 Uiso 1 1 calc R . .
H46C H 0.0149 0.9428 1.2216 0.081 Uiso 1 1 calc R . .
C47 C 0.0332(2) 0.6379(3) 1.0843(2) 0.0454(13) Uani 1 1 d . . .
H47A H 0.0096 0.5937 1.0497 0.054 Uiso 1 1 calc R . .
H47B H -0.0004 0.6900 1.0915 0.054 Uiso 1 1 calc R . .
C48 C 0.0501(3) 0.5843(4) 1.1526(3) 0.0782(19) Uani 1 1 d . . .
H48A H 0.0860 0.5356 1.1467 0.117 Uiso 1 1 calc R . .
H48B H 0.0069 0.5539 1.1660 0.117 Uiso 1 1 calc R . .
H48C H 0.0680 0.6292 1.1886 0.117 Uiso 1 1 calc R . .
C49 C 0.1175(2) 0.5539(3) 0.9633(2) 0.0357(11) Uani 1 1 d . . .
H49A H 0.1370 0.5593 0.9180 0.043 Uiso 1 1 calc R . .
H49B H 0.0654 0.5476 0.9544 0.043 Uiso 1 1 calc R . .
C50 C 0.1465(3) 0.4647(3) 0.9988(3) 0.0530(14) Uani 1 1 d . . .
H50A H 0.1983 0.4684 1.0053 0.079 Uiso 1 1 calc R . .
H50B H 0.1324 0.4092 0.9703 0.079 Uiso 1 1 calc R . .
H50C H 0.1277 0.4587 1.0438 0.079 Uiso 1 1 calc R . .
C51 C 0.3440(3) 0.6638(4) 0.8307(3) 0.0614(16) Uani 1 1 d . . .
H51A H 0.3795 0.6758 0.7981 0.092 Uiso 1 1 calc R . .
H51B H 0.2968 0.6613 0.8056 0.092 Uiso 1 1 calc R . .
H51C H 0.3543 0.6030 0.8542 0.092 Uiso 1 1 calc R . .
C52 C 0.4516(2) 0.8405(4) 0.8480(2) 0.0517(14) Uani 1 1 d . . .
H52A H 0.4525 0.9104 0.8418 0.062 Uiso 1 1 calc R . .
H52B H 0.4421 0.8115 0.8017 0.062 Uiso 1 1 calc R . .
C53 C 0.5232(2) 0.8085(4) 0.8789(3) 0.0836(19) Uani 1 1 d . . .
H53A H 0.5326 0.8355 0.9253 0.125 Uiso 1 1 calc R . .
H53B H 0.5595 0.8302 0.8498 0.125 Uiso 1 1 calc R . .
H53C H 0.5241 0.7389 0.8818 0.125 Uiso 1 1 calc R . .
C54 C 0.4013(2) 0.8824(4) 1.1496(2) 0.0584(14) Uani 1 1 d . . .
N1 N 0.26312(16) 1.0468(2) 0.87065(17) 0.0271(8) Uani 1 1 d . A .
N2 N 0.30316(16) 1.2025(2) 0.96643(17) 0.0269(8) Uani 1 1 d . A .
N3 N 0.17964(16) 1.1760(2) 1.04274(17) 0.0263(8) Uani 1 1 d . A .
N4 N 0.20747(17) 0.9365(2) 1.14310(18) 0.0269(9) Uani 1 1 d . A .
N5 N 0.19048(16) 0.7809(2) 1.04255(16) 0.0239(8) Uani 1 1 d . A .
N6 N 0.31556(16) 0.8334(2) 0.97474(17) 0.0273(8) Uani 1 1 d . A .
N7 N 0.13439(18) 1.1346(3) 0.90207(19) 0.0426(10) Uani 1 1 d . A .
N8 N 0.34699(18) 0.8766(3) 1.11810(18) 0.0453(10) Uani 1 1 d . A .
O1 O 0.06602(18) 1.2253(3) 0.81765(18) 0.0779(12) Uani 1 1 d . . .
O2 O 0.45771(16) 0.8853(4) 1.18359(19) 0.1151(16) Uani 1 1 d . . .
O3 O 0.23763(14) 0.9982(2) 1.00903(15) 0.0286(6) Uani 1 1 d . A .
Fe1 Fe 0.22302(3) 1.10536(5) 0.96033(3) 0.02515(15) Uani 1 1 d . . .
Fe2 Fe 0.25975(3) 0.89165(5) 1.05564(3) 0.02500(15) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
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 C2 C3 110.9(4) . . ?
N1 C2 C1 122.6(4) . . ?
C3 C2 C1 126.5(4) . . ?
C4 C3 C2 107.1(4) . . ?
C4 C3 C17 126.6(4) . . ?
C2 C3 C17 126.3(4) . . ?
C3 C4 C5 106.8(4) . . ?
C3 C4 C19 129.2(4) . . ?
C5 C4 C19 124.0(4) . . ?
C6 C5 N1 123.4(4) . . ?
C6 C5 C4 128.3(4) . . ?
N1 C5 C4 108.2(4) . . ?
C5 C6 C7 129.4(4) . . ?
N2 C7 C6 125.1(4) . . ?
N2 C7 C8 110.8(4) . . ?
C6 C7 C8 124.0(4) . . ?
C9 C8 C7 106.6(4) . . ?
C9 C8 C20 128.5(9) . . ?
C7 C8 C20 124.7(9) . . ?
C9 C8 C20' 125.2(16) . . ?
C7 C8 C20' 127.5(16) . . ?
C20 C8 C20' 12.1(13) . . ?
C8 C9 C10 106.5(4) . . ?
C8 C9 C22 126.7(4) . . ?
C10 C9 C22 126.7(4) . . ?
N2 C10 C11 124.4(4) . . ?
N2 C10 C9 110.5(4) . . ?
C11 C10 C9 125.1(4) . . ?
C12 C11 C10 129.7(4) . . ?
C11 C12 N3 122.6(4) . . ?
C11 C12 C13 127.8(4) . . ?
N3 C12 C13 109.6(3) . . ?
C14 C13 C12 106.3(4) . . ?
C14 C13 C24 128.0(4) . . ?
C12 C13 C24 125.6(4) . . ?
C13 C14 C15 106.4(4) . . ?
C13 C14 C25 129.0(4) . . ?
C15 C14 C25 124.5(4) . . ?
N3 C15 C14 111.8(4) . . ?
N3 C15 C16 123.4(4) . . ?
C14 C15 C16 124.8(4) . . ?
C18 C17 C3 112.3(4) . . ?
C8 C20 C21 115.7(10) . . ?
C21' C20' C8 105.6(19) . . ?
C9 C22 C23 112.9(4) . . ?
C14 C25 C26 113.0(4) . . ?
N7 C27 O1 177.6(5) . . ?
N4 C29 C30 111.4(4) . . ?
N4 C29 C28 123.3(4) . . ?
C30 C29 C28 125.3(4) . . ?
C31 C30 C29 106.5(4) . . ?
C31 C30 C44 128.8(4) . . ?
C29 C30 C44 124.7(4) . . ?
C30 C31 C32 106.5(4) . . ?
C30 C31 C46 129.5(4) . . ?
C32 C31 C46 124.0(4) . . ?
C33 C32 N4 122.9(4) . . ?
C33 C32 C31 127.3(4) . . ?
N4 C32 C31 109.8(4) . . ?
C32 C33 C34 128.7(4) . . ?
N5 C34 C33 126.1(4) . . ?
N5 C34 C35 109.9(3) . . ?
C33 C34 C35 124.0(4) . . ?
C36 C35 C34 107.1(3) . . ?
C36 C35 C47 127.7(4) . . ?
C34 C35 C47 125.2(4) . . ?
C35 C36 C37 106.5(4) . . ?
C35 C36 C49 126.7(4) . . ?
C37 C36 C49 126.9(4) . . ?
N5 C37 C36 111.0(4) . . ?
N5 C37 C38 124.3(4) . . ?
C36 C37 C38 124.7(4) . . ?
C39 C38 C37 129.7(4) . . ?
C38 C39 N6 122.9(4) . . ?
C38 C39 C40 128.1(4) . . ?
N6 C39 C40 109.0(4) . . ?
C41 C40 C51 128.9(4) . . ?
C41 C40 C39 105.9(4) . . ?
C51 C40 C39 125.2(4) . . ?
C40 C41 C42 106.4(4) . . ?
C40 C41 C52 128.2(4) . . ?
C42 C41 C52 125.4(4) . . ?
N6 C42 C41 112.4(4) . . ?
N6 C42 C43 123.3(4) . . ?
C41 C42 C43 124.3(4) . . ?
C30 C44 C45 114.8(4) . . ?
C35 C47 C48 113.3(4) . . ?
C36 C49 C50 114.2(3) . . ?
C41 C52 C53 114.1(4) . . ?
N8 C54 O2 177.6(7) . . ?
C2 N1 C5 107.0(3) . . ?
C2 N1 Fe1 127.5(3) . . ?
C5 N1 Fe1 125.6(3) . . ?
C7 N2 C10 105.6(3) . . ?
C7 N2 Fe1 127.2(3) . . ?
C10 N2 Fe1 127.2(3) . . ?
C15 N3 C12 105.8(3) . . ?
C15 N3 Fe1 127.2(3) . . ?
C12 N3 Fe1 126.9(3) . . ?
C29 N4 C32 105.8(4) . . ?
C29 N4 Fe2 127.5(3) . . ?
C32 N4 Fe2 126.4(3) . . ?
C37 N5 C34 105.6(3) . . ?
C37 N5 Fe2 128.0(3) . . ?
C34 N5 Fe2 126.5(3) . . ?
C42 N6 C39 106.3(3) . . ?
C42 N6 Fe2 127.0(3) . . ?
C39 N6 Fe2 126.6(3) . . ?
C27 N7 Fe1 151.5(4) . . ?
C54 N8 Fe2 168.1(4) . . ?
Fe2 O3 Fe1 175.12(17) . . ?
O3 Fe1 N7 124.01(15) . . ?
O3 Fe1 N2 117.13(14) . . ?
N7 Fe1 N2 118.85(15) . . ?
O3 Fe1 N3 92.65(13) . . ?
N7 Fe1 N3 88.10(14) . . ?
N2 Fe1 N3 88.95(13) . . ?
O3 Fe1 N1 93.35(13) . . ?
N7 Fe1 N1 87.73(14) . . ?
N2 Fe1 N1 89.18(12) . . ?
N3 Fe1 N1 173.92(13) . . ?
O3 Fe2 N8 123.29(16) . . ?
O3 Fe2 N5 117.41(13) . . ?
N8 Fe2 N5 119.30(15) . . ?
O3 Fe2 N6 93.24(13) . . ?
N8 Fe2 N6 88.15(13) . . ?
N5 Fe2 N6 88.46(13) . . ?
O3 Fe2 N4 92.99(13) . . ?
N8 Fe2 N4 88.07(13) . . ?
N5 Fe2 N4 89.05(13) . . ?
N6 Fe2 N4 173.75(13) . . ?
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
C1 C2 1.476(5) . ?
C2 N1 1.340(5) . ?
C2 C3 1.445(6) . ?
C3 C4 1.361(6) . ?
C3 C17 1.523(6) . ?
C4 C5 1.461(6) . ?
C4 C19 1.491(6) . ?
C5 C6 1.353(6) . ?
C5 N1 1.407(5) . ?
C6 C7 1.407(6) . ?
C7 N2 1.370(5) . ?
C7 C8 1.428(6) . ?
C8 C9 1.382(6) . ?
C8 C20 1.454(17) . ?
C8 C20' 1.60(4) . ?
C9 C10 1.425(5) . ?
C9 C22 1.497(6) . ?
C10 N2 1.386(5) . ?
C10 C11 1.411(6) . ?
C11 C12 1.356(5) . ?
C12 N3 1.400(5) . ?
C12 C13 1.454(6) . ?
C13 C14 1.359(5) . ?
C13 C24 1.500(6) . ?
C14 C15 1.454(6) . ?
C14 C25 1.492(5) . ?
C15 N3 1.329(5) . ?
C15 C16 1.493(5) . ?
C17 C18 1.471(6) . ?
C20 C21 1.482(15) . ?
C20' C21' 1.35(3) . ?
C22 C23 1.518(6) . ?
C25 C26 1.522(5) . ?
C27 N7 1.149(5) . ?
C27 O1 1.219(5) . ?
C28 C29 1.485(5) . ?
C29 N4 1.332(5) . ?
C29 C30 1.455(6) . ?
C30 C31 1.352(5) . ?
C30 C44 1.507(5) . ?
C31 C32 1.447(5) . ?
C31 C46 1.504(6) . ?
C32 C33 1.371(6) . ?
C32 N4 1.395(5) . ?
C33 C34 1.409(5) . ?
C34 N5 1.385(5) . ?
C34 C35 1.428(5) . ?
C35 C36 1.378(6) . ?
C35 C47 1.502(6) . ?
C36 C37 1.418(5) . ?
C36 C49 1.499(5) . ?
C37 N5 1.379(5) . ?
C37 C38 1.421(6) . ?
C38 C39 1.345(6) . ?
C39 N6 1.404(5) . ?
C39 C40 1.471(6) . ?
C40 C41 1.362(6) . ?
C40 C51 1.469(6) . ?
C41 C42 1.455(6) . ?
C41 C52 1.500(6) . ?
C42 N6 1.315(5) . ?
C42 C43 1.488(6) . ?
C44 C45 1.509(5) . ?
C47 C48 1.534(7) . ?
C49 C50 1.510(5) . ?
C52 C53 1.502(6) . ?
C54 N8 1.151(5) . ?
C54 O2 1.205(5) . ?
N1 Fe1 2.132(3) . ?
N2 Fe1 2.039(3) . ?
N3 Fe1 2.116(3) . ?
N4 Fe2 2.142(4) . ?
N5 Fe2 2.038(3) . ?
N6 Fe2 2.139(3) . ?
N7 Fe1 1.981(4) . ?
N8 Fe2 1.971(4) . ?
O3 Fe2 1.780(3) . ?
O3 Fe1 1.788(3) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 C4 -0.8(5) . . . . ?
C1 C2 C3 C4 178.3(4) . . . . ?
N1 C2 C3 C17 176.8(4) . . . . ?
C1 C2 C3 C17 -4.0(7) . . . . ?
C2 C3 C4 C5 1.2(5) . . . . ?
C17 C3 C4 C5 -176.4(4) . . . . ?
C2 C3 C4 C19 -178.2(4) . . . . ?
C17 C3 C4 C19 4.1(8) . . . . ?
C3 C4 C5 C6 176.3(4) . . . . ?
C19 C4 C5 C6 -4.2(7) . . . . ?
C3 C4 C5 N1 -1.3(5) . . . . ?
C19 C4 C5 N1 178.2(4) . . . . ?
N1 C5 C6 C7 -2.4(7) . . . . ?
C4 C5 C6 C7 -179.6(4) . . . . ?
C5 C6 C7 N2 -1.3(8) . . . . ?
C5 C6 C7 C8 -177.2(4) . . . . ?
N2 C7 C8 C9 -0.9(5) . . . . ?
C6 C7 C8 C9 175.5(4) . . . . ?
N2 C7 C8 C20 174.1(7) . . . . ?
C6 C7 C8 C20 -9.5(9) . . . . ?
N2 C7 C8 C20' -171.3(13) . . . . ?
C6 C7 C8 C20' 5.1(14) . . . . ?
C7 C8 C9 C10 1.0(5) . . . . ?
C20 C8 C9 C10 -173.8(7) . . . . ?
C20' C8 C9 C10 171.7(13) . . . . ?
C7 C8 C9 C22 -176.6(4) . . . . ?
C20 C8 C9 C22 8.6(10) . . . . ?
C20' C8 C9 C22 -6.0(14) . . . . ?
C8 C9 C10 N2 -0.8(5) . . . . ?
C22 C9 C10 N2 176.8(4) . . . . ?
C8 C9 C10 C11 178.8(4) . . . . ?
C22 C9 C10 C11 -3.6(7) . . . . ?
N2 C10 C11 C12 -3.7(7) . . . . ?
C9 C10 C11 C12 176.7(4) . . . . ?
C10 C11 C12 N3 1.3(7) . . . . ?
C10 C11 C12 C13 -179.4(4) . . . . ?
C11 C12 C13 C14 178.4(4) . . . . ?
N3 C12 C13 C14 -2.2(5) . . . . ?
C11 C12 C13 C24 -1.1(7) . . . . ?
N3 C12 C13 C24 178.3(4) . . . . ?
C12 C13 C14 C15 1.6(5) . . . . ?
C24 C13 C14 C15 -179.0(4) . . . . ?
C12 C13 C14 C25 -176.7(4) . . . . ?
C24 C13 C14 C25 2.8(7) . . . . ?
C13 C14 C15 N3 -0.5(5) . . . . ?
C25 C14 C15 N3 177.9(4) . . . . ?
C13 C14 C15 C16 178.3(4) . . . . ?
C25 C14 C15 C16 -3.4(7) . . . . ?
C4 C3 C17 C18 -75.1(6) . . . . ?
C2 C3 C17 C18 107.6(5) . . . . ?
C9 C8 C20 C21 -102.2(13) . . . . ?
C7 C8 C20 C21 83.9(13) . . . . ?
C20' C8 C20 C21 -24(10) . . . . ?
C9 C8 C20' C21' 102(2) . . . . ?
C7 C8 C20' C21' -89(3) . . . . ?
C20 C8 C20' C21' -8(9) . . . . ?
C8 C9 C22 C23 84.3(6) . . . . ?
C10 C9 C22 C23 -92.9(6) . . . . ?
C13 C14 C25 C26 98.2(5) . . . . ?
C15 C14 C25 C26 -79.7(5) . . . . ?
N4 C29 C30 C31 -0.7(5) . . . . ?
C28 C29 C30 C31 -180.0(4) . . . . ?
N4 C29 C30 C44 -179.1(4) . . . . ?
C28 C29 C30 C44 1.6(6) . . . . ?
C29 C30 C31 C32 0.7(4) . . . . ?
C44 C30 C31 C32 179.0(4) . . . . ?
C29 C30 C31 C46 -178.3(4) . . . . ?
C44 C30 C31 C46 0.0(7) . . . . ?
C30 C31 C32 C33 178.9(4) . . . . ?
C46 C31 C32 C33 -2.0(7) . . . . ?
C30 C31 C32 N4 -0.5(5) . . . . ?
C46 C31 C32 N4 178.6(4) . . . . ?
N4 C32 C33 C34 0.1(7) . . . . ?
C31 C32 C33 C34 -179.3(4) . . . . ?
C32 C33 C34 N5 -3.1(7) . . . . ?
C32 C33 C34 C35 174.6(4) . . . . ?
N5 C34 C35 C36 -0.5(4) . . . . ?
C33 C34 C35 C36 -178.6(4) . . . . ?
N5 C34 C35 C47 179.4(4) . . . . ?
C33 C34 C35 C47 1.4(6) . . . . ?
C34 C35 C36 C37 0.4(5) . . . . ?
C47 C35 C36 C37 -179.6(4) . . . . ?
C34 C35 C36 C49 179.0(4) . . . . ?
C47 C35 C36 C49 -1.0(7) . . . . ?
C35 C36 C37 N5 -0.1(5) . . . . ?
C49 C36 C37 N5 -178.7(4) . . . . ?
C35 C36 C37 C38 -179.7(4) . . . . ?
C49 C36 C37 C38 1.7(7) . . . . ?
N5 C37 C38 C39 0.1(7) . . . . ?
C36 C37 C38 C39 179.7(4) . . . . ?
C37 C38 C39 N6 2.5(7) . . . . ?
C37 C38 C39 C40 -177.3(4) . . . . ?
C38 C39 C40 C41 178.9(4) . . . . ?
N6 C39 C40 C41 -0.9(5) . . . . ?
C38 C39 C40 C51 -0.3(7) . . . . ?
N6 C39 C40 C51 179.8(4) . . . . ?
C51 C40 C41 C42 -179.6(5) . . . . ?
C39 C40 C41 C42 1.2(5) . . . . ?
C51 C40 C41 C52 1.7(8) . . . . ?
C39 C40 C41 C52 -177.5(4) . . . . ?
C40 C41 C42 N6 -1.1(5) . . . . ?
C52 C41 C42 N6 177.6(4) . . . . ?
C40 C41 C42 C43 176.6(4) . . . . ?
C52 C41 C42 C43 -4.7(7) . . . . ?
C31 C30 C44 C45 105.6(5) . . . . ?
C29 C30 C44 C45 -76.4(5) . . . . ?
C36 C35 C47 C48 101.4(5) . . . . ?
C34 C35 C47 C48 -78.6(5) . . . . ?
C35 C36 C49 C50 -82.5(6) . . . . ?
C37 C36 C49 C50 95.9(5) . . . . ?
C40 C41 C52 C53 -98.5(6) . . . . ?
C42 C41 C52 C53 83.0(6) . . . . ?
C3 C2 N1 C5 0.0(4) . . . . ?
C1 C2 N1 C5 -179.2(4) . . . . ?
C3 C2 N1 Fe1 -179.5(3) . . . . ?
C1 C2 N1 Fe1 1.3(6) . . . . ?
C6 C5 N1 C2 -176.9(4) . . . . ?
C4 C5 N1 C2 0.7(4) . . . . ?
C6 C5 N1 Fe1 2.6(6) . . . . ?
C4 C5 N1 Fe1 -179.7(3) . . . . ?
C6 C7 N2 C10 -175.9(4) . . . . ?
C8 C7 N2 C10 0.4(4) . . . . ?
C6 C7 N2 Fe1 4.4(6) . . . . ?
C8 C7 N2 Fe1 -179.3(3) . . . . ?
C11 C10 N2 C7 -179.3(4) . . . . ?
C9 C10 N2 C7 0.3(4) . . . . ?
C11 C10 N2 Fe1 0.3(6) . . . . ?
C9 C10 N2 Fe1 179.9(3) . . . . ?
C14 C15 N3 C12 -0.9(4) . . . . ?
C16 C15 N3 C12 -179.7(4) . . . . ?
C14 C15 N3 Fe1 176.3(3) . . . . ?
C16 C15 N3 Fe1 -2.4(6) . . . . ?
C11 C12 N3 C15 -178.7(4) . . . . ?
C13 C12 N3 C15 1.9(4) . . . . ?
C11 C12 N3 Fe1 4.1(6) . . . . ?
C13 C12 N3 Fe1 -175.3(3) . . . . ?
C30 C29 N4 C32 0.4(4) . . . . ?
C28 C29 N4 C32 179.7(4) . . . . ?
C30 C29 N4 Fe2 174.3(2) . . . . ?
C28 C29 N4 Fe2 -6.5(6) . . . . ?
C33 C32 N4 C29 -179.4(4) . . . . ?
C31 C32 N4 C29 0.0(4) . . . . ?
C33 C32 N4 Fe2 6.6(6) . . . . ?
C31 C32 N4 Fe2 -173.9(3) . . . . ?
C36 C37 N5 C34 -0.3(4) . . . . ?
C38 C37 N5 C34 179.4(4) . . . . ?
C36 C37 N5 Fe2 179.5(3) . . . . ?
C38 C37 N5 Fe2 -0.8(6) . . . . ?
C33 C34 N5 C37 178.5(4) . . . . ?
C35 C34 N5 C37 0.5(4) . . . . ?
C33 C34 N5 Fe2 -1.3(5) . . . . ?
C35 C34 N5 Fe2 -179.3(3) . . . . ?
C41 C42 N6 C39 0.5(5) . . . . ?
C43 C42 N6 C39 -177.2(4) . . . . ?
C41 C42 N6 Fe2 -175.2(3) . . . . ?
C43 C42 N6 Fe2 7.1(6) . . . . ?
C38 C39 N6 C42 -179.6(4) . . . . ?
C40 C39 N6 C42 0.2(4) . . . . ?
C38 C39 N6 Fe2 -3.9(6) . . . . ?
C40 C39 N6 Fe2 176.0(3) . . . . ?
O1 C27 N7 Fe1 -178(100) . . . . ?
O2 C54 N8 Fe2 -173(100) . . . . ?
Fe2 O3 Fe1 N7 142(2) . . . . ?
Fe2 O3 Fe1 N2 -38(2) . . . . ?
Fe2 O3 Fe1 N3 -128(2) . . . . ?
Fe2 O3 Fe1 N1 53(2) . . . . ?
C27 N7 Fe1 O3 -168.5(7) . . . . ?
C27 N7 Fe1 N2 11.9(8) . . . . ?
C27 N7 Fe1 N3 99.6(7) . . . . ?
C27 N7 Fe1 N1 -75.9(7) . . . . ?
C7 N2 Fe1 O3 90.2(3) . . . . ?
C10 N2 Fe1 O3 -89.4(3) . . . . ?
C7 N2 Fe1 N7 -90.1(3) . . . . ?
C10 N2 Fe1 N7 90.3(3) . . . . ?
C7 N2 Fe1 N3 -177.4(3) . . . . ?
C10 N2 Fe1 N3 3.0(3) . . . . ?
C7 N2 Fe1 N1 -3.1(3) . . . . ?
C10 N2 Fe1 N1 177.2(3) . . . . ?
C15 N3 Fe1 O3 -64.8(3) . . . . ?
C12 N3 Fe1 O3 111.9(3) . . . . ?
C15 N3 Fe1 N7 59.2(3) . . . . ?
C12 N3 Fe1 N7 -124.1(3) . . . . ?
C15 N3 Fe1 N2 178.1(3) . . . . ?
C12 N3 Fe1 N2 -5.2(3) . . . . ?
C15 N3 Fe1 N1 105.9(12) . . . . ?
C12 N3 Fe1 N1 -77.4(13) . . . . ?
C2 N1 Fe1 O3 62.2(3) . . . . ?
C5 N1 Fe1 O3 -117.3(3) . . . . ?
C2 N1 Fe1 N7 -61.8(3) . . . . ?
C5 N1 Fe1 N7 118.8(3) . . . . ?
C2 N1 Fe1 N2 179.3(3) . . . . ?
C5 N1 Fe1 N2 -0.1(3) . . . . ?
C2 N1 Fe1 N3 -108.5(12) . . . . ?
C5 N1 Fe1 N3 72.0(13) . . . . ?
Fe1 O3 Fe2 N8 45(2) . . . . ?
Fe1 O3 Fe2 N5 -134(2) . . . . ?
Fe1 O3 Fe2 N6 -44(2) . . . . ?
Fe1 O3 Fe2 N4 135(2) . . . . ?
C54 N8 Fe2 O3 -10.6(18) . . . . ?
C54 N8 Fe2 N5 169.3(18) . . . . ?
C54 N8 Fe2 N6 82.1(18) . . . . ?
C54 N8 Fe2 N4 -102.9(18) . . . . ?
C37 N5 Fe2 O3 92.6(3) . . . . ?
C34 N5 Fe2 O3 -87.7(3) . . . . ?
C37 N5 Fe2 N8 -87.3(4) . . . . ?
C34 N5 Fe2 N8 92.4(3) . . . . ?
C37 N5 Fe2 N6 -0.3(3) . . . . ?
C34 N5 Fe2 N6 179.4(3) . . . . ?
C37 N5 Fe2 N4 -174.6(3) . . . . ?
C34 N5 Fe2 N4 5.2(3) . . . . ?
C42 N6 Fe2 O3 60.0(3) . . . . ?
C39 N6 Fe2 O3 -114.8(3) . . . . ?
C42 N6 Fe2 N8 -63.2(3) . . . . ?
C39 N6 Fe2 N8 121.9(3) . . . . ?
C42 N6 Fe2 N5 177.4(3) . . . . ?
C39 N6 Fe2 N5 2.6(3) . . . . ?
C42 N6 Fe2 N4 -116.0(11) . . . . ?
C39 N6 Fe2 N4 69.1(12) . . . . ?
C29 N4 Fe2 O3 -63.1(3) . . . . ?
C32 N4 Fe2 O3 109.6(3) . . . . ?
C29 N4 Fe2 N8 60.1(3) . . . . ?
C32 N4 Fe2 N8 -127.2(3) . . . . ?
C29 N4 Fe2 N5 179.5(3) . . . . ?
C32 N4 Fe2 N5 -7.8(3) . . . . ?
C29 N4 Fe2 N6 113.0(11) . . . . ?
C32 N4 Fe2 N6 -74.4(12) . . . . ?
