#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:34:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179413 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/10/4331068.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_4331068
loop_
_publ_author_name
'Anangamohan Panja'
'Philippe Guionneau'
'Ie-Rang Jeon'
'Stephen M. Holmes'
'Rodolphe Clérac'
'Corine Mathonière'
_publ_section_title
;
 Syntheses, Structures, and Magnetic Properties of a Novel
 mer-[(bbp)FeIII(CN)3]2- Building Block (bbp:
 bis(2-benzimidazolyl)pyridine dianion) and Its Related Heterobimetallic
 Fe(III)-Ni(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12350
_journal_page_last               12359
_journal_paper_doi               10.1021/ic301661x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C147 H236 Fe4 N48 Ni4 O22'
_chemical_formula_weight         3486.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.8930(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.1754(3)
_cell_length_b                   19.2606(4)
_cell_length_c                   26.2796(5)
_cell_measurement_reflns_used    138492
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.0
_cell_volume                     9700.5(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997) and Mercury (CCDC)'
_computing_publication_material  'shelxl-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Shelxs-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_sigmaI/netI    0.1044
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            42504
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.9571
_exptl_absorpt_correction_T_min  0.7568
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   scalepack
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             3692
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.729
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1050
_refine_ls_number_reflns         22114
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1465
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [0.00000+1.00000exp(0.17(sinθ/λ)²)]/
   [σ²(Fo²)+0.1164+21.3761*P+(0.1033P)²+0.0895sinθ/λ]
 where P = -0.02561Fo² + 1.02561Fc²
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1997
_refine_ls_wR_factor_ref         0.2361
_reflns_number_gt                12229
_reflns_number_total             22114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301661x_si_002_4.cif
_cod_data_source_block           compound4_FeNi_chain
_cod_database_code               4331068
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_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
C1 C 0.9943(2) 0.7664(3) 0.6311(2) 0.0290(12) Uani 1 1 d .
C2 C 0.9859(3) 0.6952(3) 0.6435(2) 0.0385(14) Uani 1 1 d .
H2 H 0.9923 0.6786 0.6774 0.046 Uiso 1 1 calc R
C3 C 0.9679(4) 0.6512(3) 0.6034(3) 0.0530(18) Uani 1 1 d .
H3 H 0.9612 0.6033 0.6102 0.064 Uiso 1 1 calc R
C4 C 0.9592(4) 0.6750(4) 0.5535(3) 0.067(2) Uani 1 1 d .
H4 H 0.9483 0.6428 0.5271 0.081 Uiso 1 1 calc R
C5 C 0.9663(4) 0.7455(4) 0.5416(3) 0.0589(19) Uani 1 1 d .
H5 H 0.9587 0.7620 0.5078 0.071 Uiso 1 1 calc R
C6 C 0.9848(3) 0.7902(3) 0.5812(2) 0.0383(14) Uani 1 1 d .
C7 C 1.0129(2) 0.8769(3) 0.6279(2) 0.0279(12) Uani 1 1 d .
C8 C 1.0318(2) 0.9438(2) 0.6507(2) 0.0250(11) Uani 1 1 d .
C9 C 1.0359(3) 1.0086(3) 0.6275(2) 0.0329(12) Uani 1 1 d .
H9 H 1.0271 1.0140 0.5919 0.040 Uiso 1 1 calc R
C10 C 1.0535(3) 1.0649(3) 0.6580(2) 0.0339(13) Uani 1 1 d .
H10 H 1.0555 1.1099 0.6433 0.041 Uiso 1 1 calc R
C11 C 1.0680(3) 1.0571(3) 0.7094(2) 0.0300(12) Uani 1 1 d .
H11 H 1.0807 1.0960 0.7300 0.036 Uiso 1 1 calc R
C12 C 1.0637(2) 0.9908(3) 0.7306(2) 0.0246(11) Uani 1 1 d .
C13 C 1.0729(2) 0.9687(2) 0.7834(2) 0.0239(11) Uani 1 1 d .
C14 C 1.0907(3) 0.9587(3) 0.8632(2) 0.0320(12) Uani 1 1 d .
C15 C 1.1056(3) 0.9678(3) 0.9152(2) 0.0417(14) Uani 1 1 d .
H15 H 1.1216 1.0111 0.9283 0.050 Uiso 1 1 calc R
C16 C 1.0961(3) 0.9111(3) 0.9472(3) 0.0483(16) Uani 1 1 d .
H16 H 1.1063 0.9158 0.9827 0.058 Uiso 1 1 calc R
C17 C 1.0718(3) 0.8475(3) 0.9282(2) 0.0438(15) Uani 1 1 d .
H17 H 1.0651 0.8103 0.9512 0.053 Uiso 1 1 calc R
C18 C 1.0573(3) 0.8373(3) 0.8771(2) 0.0341(13) Uani 1 1 d .
H18 H 1.0408 0.7939 0.8645 0.041 Uiso 1 1 calc R
C19 C 1.0678(2) 0.8936(3) 0.8446(2) 0.0272(11) Uani 1 1 d .
C20 C 0.9333(2) 0.8631(2) 0.7405(2) 0.0242(11) Uani 1 1 d .
C21 C 1.1290(2) 0.8202(2) 0.72538(19) 0.0234(11) Uani 1 1 d .
C22 C 1.0176(2) 0.7595(3) 0.7639(2) 0.0289(12) Uani 1 1 d .
C23 C 0.6989(3) 0.8886(3) 0.6508(2) 0.0430(15) Uani 1 1 d .
H23C H 0.6822 0.9345 0.6387 0.052 Uiso 1 1 calc R
H23D H 0.6577 0.8579 0.6531 0.052 Uiso 1 1 calc R
C24 C 0.7478(3) 0.8583(3) 0.6116(2) 0.0414(14) Uani 1 1 d .
C25 C 0.7652(3) 0.7826(3) 0.6232(2) 0.0437(15) Uani 1 1 d .
H25A H 0.7210 0.7571 0.6275 0.052 Uiso 1 1 calc R
H25B H 0.7880 0.7625 0.5933 0.052 Uiso 1 1 calc R
C26 C 0.7072(4) 0.8597(4) 0.5605(3) 0.070(2) Uani 1 1 d .
H26A H 0.7361 0.8400 0.5340 0.105 Uiso 1 1 calc R
H26B H 0.6951 0.9077 0.5517 0.105 Uiso 1 1 calc R
H26C H 0.6644 0.8322 0.5630 0.105 Uiso 1 1 calc R
C27 C 0.8139(3) 0.9012(3) 0.6089(3) 0.0492(16) Uani 1 1 d .
H27A H 0.8384 0.9011 0.6422 0.074 Uiso 1 1 calc R
H27B H 0.8018 0.9490 0.5992 0.074 Uiso 1 1 calc R
H27C H 0.8442 0.8812 0.5834 0.074 Uiso 1 1 calc R
C28 C 0.7366(3) 0.8064(3) 0.8539(2) 0.0422(15) Uani 1 1 d .
H28A H 0.6916 0.7826 0.8466 0.051 Uiso 1 1 calc R
H28B H 0.7310 0.8355 0.8845 0.051 Uiso 1 1 calc R
C29 C 0.7923(3) 0.7515(3) 0.8659(2) 0.0422(15) Uani 1 1 d .
C30 C 0.7961(3) 0.6983(3) 0.8233(2) 0.0367(14) Uani 1 1 d .
H30A H 0.8241 0.6583 0.8359 0.044 Uiso 1 1 calc R
H30B H 0.7484 0.6811 0.8151 0.044 Uiso 1 1 calc R
C31 C 0.7692(4) 0.7133(4) 0.9131(3) 0.063(2) Uani 1 1 d .
H31A H 0.7260 0.6877 0.9050 0.094 Uiso 1 1 calc R
H31B H 0.7609 0.7469 0.9402 0.094 Uiso 1 1 calc R
H31C H 0.8057 0.6806 0.9244 0.094 Uiso 1 1 calc R
C32 C 0.8637(3) 0.7856(4) 0.8769(3) 0.0507(17) Uani 1 1 d .
H32A H 0.8988 0.7495 0.8838 0.076 Uiso 1 1 calc R
H32B H 0.8608 0.8160 0.9067 0.076 Uiso 1 1 calc R
H32C H 0.8770 0.8130 0.8474 0.076 Uiso 1 1 calc R
C33 C 0.6299(2) 0.7397(2) 0.73149(19) 0.0223(10) Uani 1 1 d .
C34 C 0.4993(2) 0.7970(3) 0.6338(2) 0.0264(11) Uani 1 1 d .
C35 C 0.4889(3) 0.8656(3) 0.6467(2) 0.0321(12) Uani 1 1 d .
H35 H 0.4937 0.8813 0.6808 0.039 Uiso 1 1 calc R
C36 C 0.4711(3) 0.9100(3) 0.6071(2) 0.0396(14) Uani 1 1 d .
H36 H 0.4640 0.9577 0.6145 0.047 Uiso 1 1 calc R
C37 C 0.4631(3) 0.8875(3) 0.5565(2) 0.0477(16) Uani 1 1 d .
H37 H 0.4512 0.9202 0.5306 0.057 Uiso 1 1 calc R
C38 C 0.4720(3) 0.8197(3) 0.5439(2) 0.0422(15) Uani 1 1 d .
H38 H 0.4653 0.8043 0.5098 0.051 Uiso 1 1 calc R
C39 C 0.4912(3) 0.7735(3) 0.5827(2) 0.0321(12) Uani 1 1 d .
C40 C 0.5208(2) 0.6859(3) 0.62831(19) 0.0238(11) Uani 1 1 d .
C41 C 0.5400(2) 0.6189(3) 0.6499(2) 0.0255(11) Uani 1 1 d .
C42 C 0.5485(3) 0.5551(3) 0.6259(2) 0.0333(13) Uani 1 1 d .
H42 H 0.5431 0.5510 0.5900 0.040 Uiso 1 1 calc R
C43 C 0.5652(3) 0.4975(3) 0.6560(2) 0.0346(13) Uani 1 1 d .
H43 H 0.5697 0.4533 0.6404 0.041 Uiso 1 1 calc R
C44 C 0.5752(3) 0.5037(3) 0.7081(2) 0.0318(12) Uani 1 1 d .
H44 H 0.5871 0.4645 0.7284 0.038 Uiso 1 1 calc R
C45 C 0.5675(2) 0.5693(2) 0.73003(19) 0.0221(10) Uani 1 1 d .
C46 C 0.5731(2) 0.5894(2) 0.7830(2) 0.0224(11) Uani 1 1 d .
C47 C 0.5894(3) 0.5982(3) 0.8641(2) 0.0293(12) Uani 1 1 d .
C48 C 0.6030(3) 0.5887(3) 0.9161(2) 0.0356(13) Uani 1 1 d .
H48 H 0.6195 0.5455 0.9292 0.043 Uiso 1 1 calc R
C49 C 0.5919(3) 0.6438(3) 0.9476(2) 0.0405(14) Uani 1 1 d .
H49 H 0.5998 0.6380 0.9832 0.049 Uiso 1 1 calc R
C50 C 0.5690(3) 0.7089(3) 0.9292(2) 0.0373(13) Uani 1 1 d .
H50 H 0.5630 0.7459 0.9525 0.045 Uiso 1 1 calc R
C51 C 0.5552(3) 0.7200(3) 0.8780(2) 0.0297(12) Uani 1 1 d .
H51 H 0.5397 0.7639 0.8657 0.036 Uiso 1 1 calc R
C52 C 0.5651(2) 0.6641(3) 0.84513(19) 0.0240(11) Uani 1 1 d .
C53 C 0.5148(2) 0.7995(3) 0.76583(19) 0.0235(11) Uani 1 1 d .
C54 C 1.4322(2) 0.6935(2) 0.73524(19) 0.0238(11) Uani 1 1 d .
C55 C 1.1934(3) 0.6739(3) 0.6394(2) 0.0439(15) Uani 1 1 d .
H55A H 1.1535 0.7057 0.6436 0.053 Uiso 1 1 calc R
H55B H 1.1746 0.6291 0.6266 0.053 Uiso 1 1 calc R
C56 C 1.2401(3) 0.7038(4) 0.5999(3) 0.0510(17) Uani 1 1 d .
C57 C 1.2613(3) 0.7789(3) 0.6121(2) 0.0450(15) Uani 1 1 d .
H57A H 1.2840 0.7989 0.5821 0.054 Uiso 1 1 calc R
H57B H 1.2186 0.8063 0.6179 0.054 Uiso 1 1 calc R
C58 C 1.1952(5) 0.7059(5) 0.5500(3) 0.082(3) Uani 1 1 d .
H58A H 1.1826 0.6585 0.5397 0.122 Uiso 1 1 calc R
H58B H 1.2218 0.7279 0.5231 0.122 Uiso 1 1 calc R
H58C H 1.1526 0.7327 0.5554 0.122 Uiso 1 1 calc R
C59 C 1.3041(4) 0.6590(4) 0.5928(3) 0.075(3) Uani 1 1 d .
H59A H 1.3302 0.6548 0.6254 0.113 Uiso 1 1 calc R
H59B H 1.3338 0.6805 0.5676 0.113 Uiso 1 1 calc R
H59C H 1.2896 0.6128 0.5810 0.113 Uiso 1 1 calc R
C60 C 1.2936(3) 0.8588(3) 0.8120(2) 0.0326(13) Uani 1 1 d .
H60A H 1.2456 0.8748 0.8033 0.039 Uiso 1 1 calc R
H60B H 1.3206 0.8995 0.8245 0.039 Uiso 1 1 calc R
C61 C 1.2903(3) 0.8057(3) 0.8551(2) 0.0378(14) Uani 1 1 d .
C62 C 1.2352(3) 0.7500(3) 0.8431(2) 0.0367(13) Uani 1 1 d .
H62A H 1.2302 0.7206 0.8736 0.044 Uiso 1 1 calc R
H62B H 1.1899 0.7731 0.8359 0.044 Uiso 1 1 calc R
C63 C 1.2676(3) 0.8440(4) 0.9028(3) 0.0536(18) Uani 1 1 d .
H63A H 1.2990 0.8834 0.9096 0.080 Uiso 1 1 calc R
H63B H 1.2697 0.8122 0.9319 0.080 Uiso 1 1 calc R
H63C H 1.2198 0.8610 0.8974 0.080 Uiso 1 1 calc R
C64 C 1.3623(3) 0.7732(4) 0.8661(3) 0.0479(16) Uani 1 1 d .
H64A H 1.3760 0.7460 0.8365 0.072 Uiso 1 1 calc R
H64B H 1.3601 0.7428 0.8959 0.072 Uiso 1 1 calc R
H64C H 1.3966 0.8100 0.8728 0.072 Uiso 1 1 calc R
C65 C 0.7520(4) 0.4748(4) 0.8251(4) 0.091(3) Uani 1 1 d .
H65A H 0.7551 0.5137 0.8012 0.137 Uiso 1 1 calc R
H65B H 0.7893 0.4415 0.8189 0.137 Uiso 1 1 calc R
H65C H 0.7569 0.4923 0.8601 0.137 Uiso 1 1 calc R
C66 C 0.7482(3) 0.5819(4) 0.6864(4) 0.079(3) Uani 1 1 d .
H66A H 0.7462 0.5475 0.7137 0.118 Uiso 1 1 calc R
H66B H 0.7419 0.5587 0.6533 0.118 Uiso 1 1 calc R
H66C H 0.7111 0.6163 0.6903 0.118 Uiso 1 1 calc R
C67 C 0.8675(4) 0.0613(4) 0.6866(3) 0.087(3) Uani 1 1 d D
H67A H 0.8879 0.0756 0.6546 0.130 Uiso 1 1 calc R
H67B H 0.8180 0.0506 0.6806 0.130 Uiso 1 1 calc R
H67C H 0.8919 0.0200 0.6998 0.130 Uiso 1 1 calc R
C68 C 0.6146(4) 0.0141(4) 0.7767(4) 0.087(3) Uani 1 1 d .
H68A H 0.5943 0.0291 0.8086 0.131 Uiso 1 1 calc R
H68B H 0.5833 0.0272 0.7480 0.131 Uiso 1 1 calc R
H68C H 0.6600 0.0365 0.7730 0.131 Uiso 1 1 calc R
C69 C 0.4500(5) 0.6012(6) 0.4802(4) 0.122(5) Uani 1 1 d .
H69A H 0.4462 0.5516 0.4722 0.183 Uiso 1 1 calc R
H69B H 0.4421 0.6284 0.4490 0.183 Uiso 1 1 calc R
H69C H 0.4151 0.6137 0.5050 0.183 Uiso 1 1 calc R
C70 C 0.4023(4) 0.5742(5) 0.8626(5) 0.113(4) Uani 1 1 d .
H70A H 0.4288 0.5980 0.8365 0.169 Uiso 1 1 calc R
H70B H 0.4148 0.5248 0.8632 0.169 Uiso 1 1 calc RD
H70C H 0.4135 0.5948 0.8960 0.169 Uiso 1 1 calc R
C71 C 0.8969(5) 0.0044(5) 0.8261(4) 0.090(3) Uani 1 1 d .
H71A H 0.9107 0.0505 0.8386 0.134 Uiso 1 1 calc R
H71B H 0.8987 0.0035 0.7889 0.134 Uiso 1 1 calc R
H71C H 0.9290 -0.0305 0.8406 0.134 Uiso 1 1 calc R
C72 C 0.9208(5) -0.0318(5) 0.9486(4) 0.095(3) Uani 1 1 d .
H72A H 0.9495 -0.0081 0.9238 0.142 Uiso 1 1 calc R
H72B H 0.9219 -0.0820 0.9425 0.142 Uiso 1 1 calc R
H72C H 0.9392 -0.0220 0.9831 0.142 Uiso 1 1 calc R
C74 C 0.6181(6) 0.9475(8) 0.9079(5) 0.054(4) Uani 0.50 1 d P
H74A H 0.5850 0.9859 0.9107 0.081 Uiso 0.50 1 calc PR
H74B H 0.5976 0.9113 0.8859 0.081 Uiso 0.50 1 calc PR
H74C H 0.6612 0.9645 0.8933 0.081 Uiso 0.50 1 calc PR
N1 N 1.01244(19) 0.8220(2) 0.66174(17) 0.0254(9) Uani 1 1 d .
N2 N 0.9970(2) 0.8621(2) 0.57980(18) 0.0386(12) Uani 1 1 d .
N3 N 1.04517(19) 0.9372(2) 0.70070(17) 0.0230(9) Uani 1 1 d .
N4 N 1.0938(2) 1.0059(2) 0.82373(17) 0.0292(10) Uani 1 1 d .
N5 N 1.05688(19) 0.9005(2) 0.79276(17) 0.0246(9) Uani 1 1 d .
N6 N 0.8737(2) 0.8640(2) 0.74345(17) 0.0296(10) Uani 1 1 d .
N7 N 1.0078(2) 0.7066(2) 0.7838(2) 0.0383(12) Uani 1 1 d .
N8 N 0.7318(2) 0.8966(2) 0.70201(18) 0.0349(11) Uani 1 1 d .
H8A H 0.6983 0.9135 0.7230 0.042 Uiso 1 1 calc R
H8B H 0.7654 0.9304 0.6998 0.042 Uiso 1 1 calc R
N9 N 0.8103(2) 0.7706(2) 0.66808(17) 0.0324(10) Uani 1 1 d .
H9A H 0.8534 0.7890 0.6617 0.039 Uiso 1 1 calc R
H9B H 0.8160 0.7234 0.6717 0.039 Uiso 1 1 calc R
N10 N 0.7515(2) 0.8522(2) 0.81042(17) 0.0315(10) Uani 1 1 d .
H10A H 0.7872 0.8813 0.8209 0.038 Uiso 1 1 calc R
H10B H 0.7127 0.8796 0.8047 0.038 Uiso 1 1 calc R
N11 N 0.8268(2) 0.7241(2) 0.77578(17) 0.0291(10) Uani 1 1 d .
H11A H 0.8268 0.6880 0.7529 0.035 Uiso 1 1 calc R
H11B H 0.8726 0.7354 0.7831 0.035 Uiso 1 1 calc R
N12 N 0.6867(2) 0.7578(2) 0.73272(17) 0.0288(10) Uani 1 1 d .
N13 N 0.51815(19) 0.7399(2) 0.66277(16) 0.0227(9) Uani 1 1 d .
N14 N 0.5058(2) 0.7023(2) 0.58040(17) 0.0311(10) Uani 1 1 d .
N15 N 0.54986(18) 0.62392(19) 0.70106(15) 0.0203(9) Uani 1 1 d .
N16 N 0.5943(2) 0.5522(2) 0.82336(17) 0.0280(10) Uani 1 1 d .
N17 N 0.55478(19) 0.6571(2) 0.79317(16) 0.0218(9) Uani 1 1 d .
N18 N 0.5036(2) 0.8516(2) 0.78495(18) 0.0326(10) Uani 1 1 d .
N19 N 1.3726(2) 0.6921(2) 0.73352(18) 0.0308(10) Uani 1 1 d .
N20 N 1.3091(2) 0.7865(2) 0.65700(17) 0.0327(11) Uani 1 1 d .
H20A H 1.3183 0.8331 0.6612 0.039 Uiso 1 1 calc R
H20B H 1.3506 0.7654 0.6495 0.039 Uiso 1 1 calc R
N21 N 1.2280(2) 0.6622(2) 0.69009(19) 0.0364(11) Uani 1 1 d .
H21A H 1.2610 0.6281 0.6863 0.044 Uiso 1 1 calc R
H21B H 1.1950 0.6446 0.7112 0.044 Uiso 1 1 calc R
N22 N 1.3251(2) 0.8327(2) 0.76550(17) 0.0287(10) Uani 1 1 d .
H22A H 1.3707 0.8209 0.7736 0.034 Uiso 1 1 calc R
H22B H 1.3262 0.8687 0.7425 0.034 Uiso 1 1 calc R
N23 N 1.2512(2) 0.7049(2) 0.79932(18) 0.0342(11) Uani 1 1 d .
H23A H 1.2131 0.6766 0.7936 0.041 Uiso 1 1 calc R
H23B H 1.2876 0.6765 0.8098 0.041 Uiso 1 1 calc R
N24 N 1.1854(2) 0.8010(2) 0.72285(17) 0.0295(10) Uani 1 1 d .
O1 O 0.68828(19) 0.44267(19) 0.81840(17) 0.0424(10) Uani 1 1 d D
O2 O 0.81406(19) 0.61570(19) 0.68880(17) 0.0421(10) Uani 1 1 d .
O3 O 0.8746(2) 0.1170(2) 0.72327(19) 0.0546(13) Uani 1 1 d D
O4 O 0.6233(2) -0.0594(2) 0.7773(2) 0.0586(13) Uani 1 1 d D
O5 O 0.5159(3) 0.6151(3) 0.50040(19) 0.0764(16) Uani 1 1 d D
O6 O 0.3285(2) 0.5813(3) 0.8510(2) 0.0829(18) Uani 1 1 d D
O7 O 0.8264(3) -0.0108(3) 0.8412(2) 0.0813(17) Uani 1 1 d D
O8 O 0.8496(3) -0.0071(4) 0.9434(3) 0.102(2) Uani 1 1 d D
O10 O 0.6322(5) 0.9213(7) 0.9537(3) 0.095(5) Uani 0.50 1 d PD
O12 O 0.2646(4) 0.5753(4) 0.9447(3) 0.140(3) Uani 1 1 d D
O13 O 0.7591(6) 0.9091(9) 1.0051(6) 0.1942(2) Uani 0.50 1 d PD
Fe1 Fe 1.03228(3) 0.84735(3) 0.73229(3) 0.02195(17) Uani 1 1 d .
Fe2 Fe 0.53272(3) 0.71171(3) 0.73327(3) 0.01900(17) Uani 1 1 d .
Ni1 Ni 0.77865(3) 0.81065(3) 0.73923(3) 0.02410(17) Uani 1 1 d .
Ni2 Ni 1.27729(3) 0.74664(3) 0.72833(3) 0.02557(17) Uani 1 1 d .
O9 O 0.1201(6) 0.5738(7) 0.9473(4) 0.085(4) Uani 0.50 1 d PD
C73 C 0.0814(7) 0.6389(6) 0.9536(6) 0.074(5) Uani 0.50 1 d PD
H73A H 0.0313 0.6291 0.9534 0.111 Uiso 0.50 1 calc PR
H73B H 0.0915 0.6705 0.9255 0.111 Uiso 0.50 1 calc PR
H73C H 0.0958 0.6606 0.9860 0.111 Uiso 0.50 1 calc PR
O11A O -0.0618(4) 0.5478(4) 1.0045(3) 0.0357(18) Uiso 0.50 1 d P
C11A C -0.1220(9) 0.5814(9) 0.9783(7) 0.079(5) Uiso 0.50 1 d P
H13A H 0.7466 0.8780 1.0332 0.118 Uiso 0.50 1 d PD
H4A H 0.6161 -0.0625 0.8142 0.118 Uiso 1 1 d D
H1A H 0.6478 0.4678 0.8254 0.118 Uiso 1 1 d D
H7 H 0.8254 -0.0310 0.8745 0.118 Uiso 1 1 d D
H6 H 0.3353 0.5580 0.8188 0.118 Uiso 1 1 d D
H8 H 0.8039 -0.0136 0.9599 0.118 Uiso 1 1 d D
H3A H 0.8732 0.0919 0.7549 0.118 Uiso 1 1 d D
H12B H 0.2166 0.5880 0.9428 0.118 Uiso 1 1 d D
H5A H 0.5059 0.6502 0.5259 0.118 Uiso 1 1 d D
H12A H 0.2868 0.5791 0.9135 0.118 Uiso 1 1 d D
H2A H 0.8522 0.5795 0.6856 0.118 Uiso 1 1 d .
H9C H 0.1341 0.5727 0.9825 0.118 Uiso 1 1 d D
H13B H 0.7212 0.9236 0.9830 0.118 Uiso 0.50 1 d PD
H10C H 0.6260 0.9464 0.9791 0.118 Uiso 1 1 d 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'
Ni Ni 0.3393 1.1124 '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_3
N1 C1 C6 108.4(5) .
N1 C1 C2 130.1(5) .
C6 C1 C2 121.5(5) .
C3 C2 C1 116.2(6) .
C2 C3 C4 122.2(6) .
C3 C4 C5 121.3(6) .
C6 C5 C4 117.2(7) .
C5 C6 C1 121.5(6) .
C5 C6 N2 129.1(6) .
C1 C6 N2 109.5(5) .
N2 C7 N1 116.4(5) .
N2 C7 C8 128.9(5) .
N1 C7 C8 114.7(5) .
N3 C8 C9 120.2(5) .
N3 C8 C7 110.9(4) .
C9 C8 C7 128.9(5) .
C10 C9 C8 117.7(5) .
C11 C10 C9 121.4(5) .
C10 C11 C12 118.5(5) .
N3 C12 C11 119.3(5) .
N3 C12 C13 110.8(4) .
C11 C12 C13 129.9(5) .
N4 C13 N5 115.8(5) .
N4 C13 C12 128.7(4) .
N5 C13 C12 115.5(4) .
N4 C14 C15 129.8(5) .
N4 C14 C19 110.2(5) .
C15 C14 C19 120.0(5) .
C16 C15 C14 117.8(5) .
C15 C16 C17 121.3(6) .
C18 C17 C16 121.9(6) .
C17 C18 C19 117.1(5) .
N5 C19 C18 131.1(5) .
N5 C19 C14 107.0(4) .
C18 C19 C14 121.8(5) .
N6 C20 Fe1 171.6(4) .
N24 C21 Fe1 176.3(5) .
N7 C22 Fe1 178.7(5) .
N8 C23 C24 113.6(4) .
C27 C24 C25 110.6(5) .
C27 C24 C26 110.5(6) .
C25 C24 C26 107.1(6) .
C27 C24 C23 110.8(5) .
C25 C24 C23 111.4(5) .
C26 C24 C23 106.2(5) .
N9 C25 C24 115.7(5) .
N10 C28 C29 114.9(4) .
C30 C29 C31 107.2(5) .
C30 C29 C28 111.4(5) .
C31 C29 C28 106.4(5) .
C30 C29 C32 111.3(5) .
C31 C29 C32 109.5(5) .
C28 C29 C32 110.8(5) .
N11 C30 C29 115.0(5) .
N12 C33 Fe2 176.6(5) .
C35 C34 N13 131.7(5) .
C35 C34 C39 121.6(5) .
N13 C34 C39 106.6(4) .
C34 C35 C36 116.3(5) .
C35 C36 C37 122.6(5) .
C38 C37 C36 121.2(6) .
C37 C38 C39 117.9(6) .
C38 C39 N14 129.9(5) .
C38 C39 C34 120.4(5) .
N14 C39 C34 109.7(5) .
N14 C40 N13 115.7(4) .
N14 C40 C41 129.0(5) .
N13 C40 C41 115.3(4) .
N15 C41 C42 119.9(5) .
N15 C41 C40 110.4(4) .
C42 C41 C40 129.7(5) .
C43 C42 C41 118.3(5) .
C44 C43 C42 121.0(5) .
C43 C44 C45 118.3(5) .
N15 C45 C44 120.3(5) .
N15 C45 C46 110.3(4) .
C44 C45 C46 129.4(5) .
N16 C46 N17 115.3(4) .
N16 C46 C45 129.3(4) .
N17 C46 C45 115.3(4) .
C48 C47 N16 130.8(5) .
C48 C47 C52 120.3(5) .
N16 C47 C52 108.9(5) .
C49 C48 C47 117.6(5) .
C48 C49 C50 122.4(6) .
C51 C50 C49 121.4(5) .
C50 C51 C52 117.3(5) .
N17 C52 C51 132.0(5) .
N17 C52 C47 107.0(4) .
C51 C52 C47 121.0(5) .
N18 C53 Fe2 179.4(5) .
N19 C54 Fe2 170.3(4) 1_655
N21 C55 C56 114.7(5) .
C55 C56 C59 111.6(6) .
C55 C56 C57 112.1(5) .
C59 C56 C57 110.6(5) .
C55 C56 C58 105.5(5) .
C59 C56 C58 109.9(6) .
C57 C56 C58 106.8(6) .
N20 C57 C56 114.4(5) .
N22 C60 C61 114.6(4) .
C60 C61 C62 111.1(5) .
C60 C61 C63 107.7(5) .
C62 C61 C63 107.1(5) .
C60 C61 C64 110.8(5) .
C62 C61 C64 111.2(5) .
C63 C61 C64 108.7(5) .
N23 C62 C61 114.4(4) .
C1 N1 C7 103.0(4) .
C1 N1 Fe1 142.3(4) .
C7 N1 Fe1 114.6(3) .
C7 N2 C6 102.7(5) .
C8 N3 C12 122.9(4) .
C8 N3 Fe1 118.8(3) .
C12 N3 Fe1 118.2(3) .
C13 N4 C14 103.0(4) .
C13 N5 C19 104.0(4) .
C13 N5 Fe1 114.1(4) .
C19 N5 Fe1 141.8(3) .
C20 N6 Ni1 148.8(4) .
C23 N8 Ni1 120.3(4) .
C25 N9 Ni1 118.4(4) .
C28 N10 Ni1 121.1(4) .
C30 N11 Ni1 117.8(3) .
C33 N12 Ni1 167.3(4) .
C34 N13 C40 104.7(4) .
C34 N13 Fe2 141.0(3) .
C40 N13 Fe2 114.1(3) .
C40 N14 C39 103.3(4) .
C45 N15 C41 122.2(4) .
C45 N15 Fe2 119.1(3) .
C41 N15 Fe2 118.6(3) .
C46 N16 C47 104.1(4) .
C52 N17 C46 104.7(4) .
C52 N17 Fe2 140.8(3) .
C46 N17 Fe2 114.1(3) .
C54 N19 Ni2 148.6(4) .
C57 N20 Ni2 118.6(3) .
C55 N21 Ni2 119.2(4) .
C60 N22 Ni2 117.8(3) .
C62 N23 Ni2 121.6(3) .
C21 N24 Ni2 166.0(4) .
C22 Fe1 N5 98.4(2) .
C22 Fe1 N3 178.74(19) .
N5 Fe1 N3 81.28(18) .
C22 Fe1 C20 86.1(2) .
N5 Fe1 C20 92.24(19) .
N3 Fe1 C20 92.70(18) .
C22 Fe1 C21 87.5(2) .
N5 Fe1 C21 90.68(18) .
N3 Fe1 C21 93.73(18) .
C20 Fe1 C21 173.3(2) .
C22 Fe1 N1 99.5(2) .
N5 Fe1 N1 162.05(18) .
N3 Fe1 N1 80.78(18) .
C20 Fe1 N1 89.06(19) .
C21 Fe1 N1 90.02(19) .
N15 Fe2 N17 81.02(17) .
N15 Fe2 C53 179.50(19) .
N17 Fe2 C53 98.81(19) .
N15 Fe2 C33 93.16(18) .
N17 Fe2 C33 89.20(18) .
C53 Fe2 C33 87.31(19) .
N15 Fe2 N13 81.22(17) .
N17 Fe2 N13 162.19(17) .
C53 Fe2 N13 98.96(19) .
C33 Fe2 N13 90.42(18) .
N15 Fe2 C54 92.11(18) 1_455
N17 Fe2 C54 94.03(18) 1_455
C53 Fe2 C54 87.43(19) 1_455
C33 Fe2 C54 174.20(19) 1_455
N13 Fe2 C54 87.97(19) 1_455
N12 Ni1 N6 178.13(18) .
N12 Ni1 N8 89.92(17) .
N6 Ni1 N8 89.77(17) .
N12 Ni1 N10 91.48(17) .
N6 Ni1 N10 90.37(17) .
N8 Ni1 N10 89.97(18) .
N12 Ni1 N11 90.45(16) .
N6 Ni1 N11 89.83(16) .
N8 Ni1 N11 179.17(18) .
N10 Ni1 N11 90.76(17) .
N12 Ni1 N9 90.94(17) .
N6 Ni1 N9 87.21(17) .
N8 Ni1 N9 90.36(18) .
N10 Ni1 N9 177.56(17) .
N11 Ni1 N9 88.89(17) .
N24 Ni2 N23 91.65(17) .
N24 Ni2 N19 179.14(18) .
N23 Ni2 N19 89.01(17) .
N24 Ni2 N22 89.49(16) .
N23 Ni2 N22 90.14(18) .
N19 Ni2 N22 89.95(16) .
N24 Ni2 N21 89.40(17) .
N23 Ni2 N21 90.66(19) .
N19 Ni2 N21 91.15(16) .
N22 Ni2 N21 178.65(18) .
N24 Ni2 N20 91.42(17) .
N23 Ni2 N20 176.91(17) .
N19 Ni2 N20 87.92(17) .
N22 Ni2 N20 89.51(17) .
N21 Ni2 N20 89.75(18) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.378(6) .
C1 C6 1.395(8) .
C1 C2 1.420(8) .
C2 C3 1.386(9) .
C3 C4 1.394(10) .
C4 C5 1.401(10) .
C5 C6 1.388(8) .
C6 N2 1.404(7) .
C7 N2 1.322(7) .
C7 N1 1.382(7) .
C7 C8 1.461(7) .
C8 N3 1.337(6) .
C8 C9 1.394(7) .
C9 C10 1.384(8) .
C10 C11 1.378(8) .
C11 C12 1.397(7) .
C12 N3 1.339(6) .
C12 C13 1.455(7) .
C13 N4 1.331(6) .
C13 N5 1.373(6) .
C14 N4 1.380(7) .
C14 C15 1.398(8) .
C14 C19 1.410(7) .
C15 C16 1.395(8) .
C16 C17 1.396(9) .
C17 C18 1.376(8) .
C18 C19 1.400(7) .
C19 N5 1.378(7) .
C20 N6 1.149(6) .
C20 Fe1 1.940(5) .
C21 N24 1.148(6) .
C21 Fe1 1.941(5) .
C22 N7 1.164(6) .
C22 Fe1 1.910(5) .
C23 N8 1.476(7) .
C23 C24 1.531(9) .
C24 C27 1.517(8) .
C24 C25 1.524(9) .
C24 C26 1.531(9) .
C25 N9 1.458(7) .
C28 N10 1.478(7) .
C28 C29 1.528(8) .
C29 C30 1.520(8) .
C29 C31 1.521(8) .
C29 C32 1.538(8) .
C30 N11 1.484(7) .
C33 N12 1.143(6) .
C33 Fe2 1.941(5) .
C34 C35 1.379(7) .
C34 N13 1.379(6) .
C34 C39 1.419(7) .
C35 C36 1.380(8) .
C36 C37 1.402(8) .
C37 C38 1.359(9) .
C38 C39 1.394(8) .
C39 N14 1.402(7) .
C40 N14 1.321(6) .
C40 N13 1.382(6) .
C40 C41 1.452(7) .
C41 N15 1.356(6) .
C41 C42 1.393(7) .
C42 C43 1.393(8) .
C43 C44 1.381(8) .
C44 C45 1.398(7) .
C45 N15 1.336(6) .
C45 C46 1.446(7) .
C46 N16 1.331(6) .
C46 N17 1.380(6) .
C47 C48 1.395(7) .
C47 N16 1.396(7) .
C47 C52 1.436(7) .
C48 C49 1.367(8) .
C49 C50 1.409(8) .
C50 C51 1.378(8) .
C51 C52 1.398(7) .
C52 N17 1.380(6) .
C53 N18 1.145(6) .
C53 Fe2 1.931(5) .
C54 N19 1.142(6) .
C54 Fe2 1.962(5) 1_655
C55 N21 1.485(8) .
C55 C56 1.506(9) .
C56 C59 1.517(10) .
C56 C57 1.534(9) .
C56 C58 1.546(10) .
C57 N20 1.477(7) .
C60 N22 1.471(7) .
C60 C61 1.527(8) .
C61 C62 1.531(8) .
C61 C63 1.529(8) .
C61 C64 1.534(8) .
C62 N23 1.482(7) .
C65 O1 1.376(8) .
C66 O2 1.419(7) .
C67 O3 1.444(8) .
C68 O4 1.427(8) .
C69 O5 1.379(10) .
C70 O6 1.444(9) .
C71 O7 1.451(10) .
C72 O8 1.448(10) .
C74 O10 1.323(15) .
N1 Fe1 1.943(4) .
N3 Fe1 1.939(4) .
N5 Fe1 1.936(4) .
N6 Ni1 2.093(4) .
N8 Ni1 2.108(4) .
N9 Ni1 2.129(4) .
N10 Ni1 2.116(4) .
N11 Ni1 2.120(4) .
N12 Ni1 2.039(4) .
N13 Fe2 1.942(4) .
N15 Fe2 1.924(4) .
N17 Fe2 1.928(4) .
N19 Ni2 2.108(4) .
N20 Ni2 2.133(5) .
N21 Ni2 2.118(4) .
N22 Ni2 2.117(4) .
N23 Ni2 2.107(5) .
N24 Ni2 2.050(4) .
Fe2 C54 1.962(5) 1_455
O9 C73 1.468(16) .
O11A C11A 1.472(18) .
