# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010

data_1
_publ_requested_journal          Chem.Commun.
_publ_contact_author_name        'Prof. Hiroki Oshio'
_publ_contact_author_address     
;
 Graduate School of Pure and Applied Sciences
 University of Tsukuba
 Tennodai 1-1-1, Tsukuba 305-8571
;
_publ_contact_author_email       oshio@chem.tsukuba.ac.jp
_publ_contact_author_phone       +81-29-853-4238
_publ_contact_author_fax         +81-29-853-4238
loop_
_publ_author_name
_publ_author_address
'Hoshino, N.'
;
 Graduate School of Pure and Applied Sciences
 University of Tsukuba
 Tennodai 1-1-1, Tsukuba 305-8571
;
'Sekine, Y.'
;
 Graduate School of Pure and Applied Sciences
 University of Tsukuba
 Tennodai 1-1-1, Tsukuba 305-8571
;
'Nihei, M.'
;
 Graduate School of Pure and Applied Sciences
 University of Tsukuba
 Tennodai 1-1-1, Tsukuba 305-8571
;
'Oshio, H.'
;
 Graduate School of Pure and Applied Sciences
 University of Tsukuba
 Tennodai 1-1-1, Tsukuba 305-8571
;

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 [Fe(III)2Ni(II)2(CN)6(tp)2((R)-pabn))((S)-pabn)](PF6)2.H2O.4CH3CN
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety 
 '(C88 H72 B2 Fe2 N26 Ni2 2+), 2(F6 P -), 4(C2 H3 N), H2 O' 
_chemical_formula_sum 
 'C96 H86 B2 F12 Fe2 N30 Ni2 O P2' 
_chemical_formula_weight          2216.63 
 
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' 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'P'  'P'   0.1023   0.0942 
 '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' 
 'B'  'B'   0.0013   0.0007 
 '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' 
 
_symmetry_cell_setting            'Triclinic' 
_symmetry_space_group_name_H-M    'P -1' 
_symmetry_space_group_name_Hall   '-P 1' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    9.212(4) 
_cell_length_b                    13.535(6) 
_cell_length_c                    20.115(9) 
_cell_angle_alpha                 101.840(6) 
_cell_angle_beta                  92.846(6) 
_cell_angle_gamma                 100.063(6) 
_cell_volume                      2407.5(18) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     93(2) 
_cell_measurement_reflns_used     1743 
_cell_measurement_theta_min       2.254 
_cell_measurement_theta_max       19.007 
 
_exptl_crystal_description        'needle' 
_exptl_crystal_colour             'brown' 
_exptl_crystal_size_max           0.10 
_exptl_crystal_size_mid           0.05 
_exptl_crystal_size_min           0.01 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.529 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1136 
_exptl_absorpt_coefficient_mu     0.804 
_exptl_absorpt_correction_type    'empirical' 
_exptl_absorpt_correction_T_min   0.9239 
_exptl_absorpt_correction_T_max   0.9920 
_exptl_absorpt_process_details    'Bruker SADABS'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       93(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            'MoK\a'
_diffrn_radiation_source          'Bruker TXS fine-focus rotating anode' 
_diffrn_radiation_monochromator   'Bruker Helios multilayer confocal mirror' 
_diffrn_measurement_device_type   'Bruker APEXII CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  8.333 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             9735 
_diffrn_reflns_av_R_equivalents   0.0630 
_diffrn_reflns_av_sigmaI/netI     0.2225 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        5 
_diffrn_reflns_limit_l_min        -22 
_diffrn_reflns_limit_l_max        23 
_diffrn_reflns_theta_min          1.57 
_diffrn_reflns_theta_max          24.15 
_reflns_number_total              7406 
_reflns_number_gt                 3503 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection      'Bruker APEX2' 
_computing_cell_refinement      'Bruker SAINT' 
_computing_data_reduction       'Bruker SAINT' 
_computing_structure_solution   'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics   'Bruker SHELXTL' 
_computing_publication_material 'Bruker SHELXTL' 
 
_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. 

 The following restrains are used on bridging cyanide ions to improve
 unnatural ADPs : SIMU 0.01 C1 N1 C2 N2.
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.1262P)^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 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7406 
_refine_ls_number_parameters      671 
_refine_ls_number_restraints      18 
_refine_ls_R_factor_all           0.1917 
_refine_ls_R_factor_gt            0.0854 
_refine_ls_wR_factor_ref          0.2614 
_refine_ls_wR_factor_gt           0.2022 
_refine_ls_goodness_of_fit_ref    0.988 
_refine_ls_restrained_S_all       0.987 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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 
Ni1 Ni 0.06715(15) 0.37285(10) 0.31926(7) 0.0189(6) Uani 1 1 d . . . 
Fe1 Fe -0.03284(17) 0.28116(11) 0.54383(8) 0.0206(6) Uani 1 1 d . . . 
P1 P 0.4262(5) 0.7063(3) 0.1994(2) 0.0598(13) Uani 1 1 d . . . 
F1 F 0.2546(9) 0.6893(7) 0.1729(5) 0.076(3) Uani 1 1 d . . . 
F2 F 0.3874(7) 0.6588(6) 0.2625(3) 0.046(2) Uani 1 1 d . . . 
F3 F 0.4690(11) 0.7481(9) 0.1334(6) 0.115(4) Uani 1 1 d . . . 
F4 F 0.4330(12) 0.5908(7) 0.1607(5) 0.096(3) Uani 1 1 d . . . 
F5 F 0.4192(11) 0.8210(7) 0.2356(6) 0.108(4) Uani 1 1 d . . . 
F6 F 0.5979(10) 0.7242(8) 0.2274(6) 0.099(3) Uani 1 1 d . . . 
N1 N -0.0431(9) 0.3327(6) 0.4005(4) 0.0171(19) Uani 1 1 d U . . 
N2 N 0.1270(9) 0.5224(7) 0.3792(4) 0.021(2) Uani 1 1 d U . . 
N3 N -0.3575(11) 0.1625(7) 0.5168(5) 0.031(2) Uani 1 1 d . . . 
N4 N 0.1975(9) 0.4192(7) 0.2392(4) 0.022(2) Uani 1 1 d . . . 
H1 H 0.2085 0.4905 0.2483 0.026 Uiso 1 1 calc R . . 
N5 N -0.0194(9) 0.2189(6) 0.2586(4) 0.020(2) Uani 1 1 d . . . 
H2 H -0.0490 0.1792 0.2900 0.024 Uiso 1 1 calc R . . 
N6 N 0.2653(9) 0.3312(6) 0.3466(4) 0.019(2) Uani 1 1 d . . . 
N7 N -0.1178(9) 0.4018(6) 0.2671(4) 0.019(2) Uani 1 1 d . . . 
N8 N -0.0102(9) 0.2409(6) 0.6318(4) 0.021(2) Uani 1 1 d . . . 
N9 N 0.0473(9) 0.1608(7) 0.5012(4) 0.021(2) Uani 1 1 d . . . 
N10 N 0.1733(9) 0.3588(6) 0.5630(4) 0.022(2) Uani 1 1 d . . . 
N11 N 0.1146(10) 0.2047(7) 0.6494(4) 0.027(2) Uani 1 1 d . . . 
N12 N 0.1717(9) 0.1390(6) 0.5322(4) 0.022(2) Uani 1 1 d . . . 
N13 N 0.2830(10) 0.3149(7) 0.5903(4) 0.025(2) Uani 1 1 d . . . 
B1 B 0.2370(14) 0.2050(9) 0.6017(6) 0.022(3) Uani 1 1 d . . . 
H30 H 0.3231 0.1797 0.6199 0.026 Uiso 1 1 calc R . . 
C1 C -0.0466(11) 0.3162(8) 0.4551(6) 0.021(2) Uani 1 1 d U . . 
C2 C 0.1004(11) 0.5977(8) 0.4113(5) 0.019(2) Uani 1 1 d U . . 
C3 C -0.2338(13) 0.2089(8) 0.5258(6) 0.026(3) Uani 1 1 d . . . 
C4 C 0.0931(12) 0.2841(8) 0.1372(5) 0.023(3) Uani 1 1 d . . . 
C5 C 0.1236(12) 0.3850(8) 0.1705(5) 0.023(3) Uani 1 1 d . . . 
C6 C 0.0731(11) 0.4591(8) 0.1406(5) 0.022(3) Uani 1 1 d . . . 
H3 H 0.0969 0.5293 0.1635 0.026 Uiso 1 1 calc R . . 
C7 C -0.0090(12) 0.4326(9) 0.0796(6) 0.030(3) Uani 1 1 d . . . 
H4 H -0.0409 0.4847 0.0606 0.035 Uiso 1 1 calc R . . 
C8 C -0.0482(12) 0.3290(8) 0.0437(5) 0.026(3) Uani 1 1 d . . . 
C9 C 0.0035(11) 0.2516(8) 0.0723(5) 0.021(3) Uani 1 1 d . . . 
C10 C -0.0414(12) 0.1470(8) 0.0388(5) 0.025(3) Uani 1 1 d . . . 
H5 H -0.0057 0.0950 0.0564 0.030 Uiso 1 1 calc R . . 
C11 C -0.1367(13) 0.1213(9) -0.0192(6) 0.033(3) Uani 1 1 d . . . 
H6 H -0.1706 0.0507 -0.0398 0.040 Uiso 1 1 calc R . . 
C12 C -0.1848(13) 0.1948(9) -0.0487(6) 0.033(3) Uani 1 1 d . . . 
H7 H -0.2453 0.1741 -0.0906 0.040 Uiso 1 1 calc R . . 
C13 C -0.1460(12) 0.2983(9) -0.0178(6) 0.032(3) Uani 1 1 d . . . 
H8 H -0.1835 0.3482 -0.0370 0.038 Uiso 1 1 calc R . . 
C14 C 0.1514(11) 0.2036(8) 0.1679(5) 0.021(3) Uani 1 1 d . . . 
C15 C 0.0948(12) 0.1714(8) 0.2232(5) 0.022(3) Uani 1 1 d . . . 
C16 C 0.1497(13) 0.0946(8) 0.2501(6) 0.031(3) Uani 1 1 d . . . 
H9 H 0.1057 0.0726 0.2875 0.037 Uiso 1 1 calc R . . 
C17 C 0.2625(13) 0.0517(8) 0.2242(5) 0.027(3) Uani 1 1 d . . . 
H10 H 0.2975 0.0008 0.2434 0.033 Uiso 1 1 calc R . . 
C18 C 0.3282(12) 0.0840(8) 0.1675(5) 0.026(3) Uani 1 1 d . . . 
C19 C 0.2700(12) 0.1587(8) 0.1376(5) 0.025(3) Uani 1 1 d . . . 
C20 C 0.3378(12) 0.1866(8) 0.0799(5) 0.026(3) Uani 1 1 d . . . 
H11 H 0.3032 0.2367 0.0598 0.031 Uiso 1 1 calc R . . 
C21 C 0.4511(13) 0.1430(9) 0.0530(6) 0.033(3) Uani 1 1 d . . . 
H12 H 0.4910 0.1612 0.0136 0.039 Uiso 1 1 calc R . . 
C22 C 0.5088(13) 0.0720(9) 0.0830(6) 0.034(3) Uani 1 1 d . . . 
H13 H 0.5892 0.0439 0.0643 0.041 Uiso 1 1 calc R . . 
C23 C 0.4519(12) 0.0428(9) 0.1381(6) 0.033(3) Uani 1 1 d . . . 
H14 H 0.4932 -0.0051 0.1579 0.039 Uiso 1 1 calc R . . 
C24 C 0.3500(11) 0.4000(9) 0.2481(5) 0.025(3) Uani 1 1 d . . . 
H15 H 0.4200 0.4667 0.2586 0.030 Uiso 1 1 calc R . . 
H16 H 0.3740 0.3595 0.2046 0.030 Uiso 1 1 calc R . . 
C25 C 0.3729(11) 0.3429(8) 0.3044(5) 0.021(3) Uani 1 1 d . . . 
C26 C 0.5087(13) 0.3108(8) 0.3149(6) 0.031(3) Uani 1 1 d . . . 
H17 H 0.5827 0.3193 0.2843 0.037 Uiso 1 1 calc R . . 
C27 C 0.5339(12) 0.2672(9) 0.3695(5) 0.029(3) Uani 1 1 d . . . 
H18 H 0.6254 0.2464 0.3773 0.034 Uiso 1 1 calc R . . 
C28 C 0.4235(12) 0.2543(8) 0.4127(6) 0.027(3) Uani 1 1 d . . . 
H19 H 0.4372 0.2241 0.4507 0.032 Uiso 1 1 calc R . . 
C29 C 0.2899(12) 0.2869(8) 0.3992(6) 0.026(3) Uani 1 1 d . . . 
H20 H 0.2136 0.2772 0.4286 0.031 Uiso 1 1 calc R . . 
C30 C -0.1565(11) 0.2176(8) 0.2164(5) 0.022(3) Uani 1 1 d . . . 
H21 H -0.2414 0.1775 0.2334 0.027 Uiso 1 1 calc R . . 
H22 H -0.1482 0.1827 0.1688 0.027 Uiso 1 1 calc R . . 
C31 C -0.1860(11) 0.3240(8) 0.2171(5) 0.020(3) Uani 1 1 d . . . 
C32 C -0.2865(12) 0.3406(9) 0.1671(5) 0.028(3) Uani 1 1 d . . . 
H23 H -0.3303 0.2860 0.1301 0.034 Uiso 1 1 calc R . . 
C33 C -0.3203(12) 0.4379(9) 0.1725(6) 0.032(3) Uani 1 1 d . . . 
H24 H -0.3881 0.4502 0.1394 0.038 Uiso 1 1 calc R . . 
C34 C -0.2552(11) 0.5166(9) 0.2262(5) 0.023(3) Uani 1 1 d . . . 
H25 H -0.2803 0.5828 0.2317 0.028 Uiso 1 1 calc R . . 
C35 C -0.1520(12) 0.4970(8) 0.2722(5) 0.025(3) Uani 1 1 d . . . 
H26 H -0.1038 0.5516 0.3083 0.029 Uiso 1 1 calc R . . 
C36 C -0.1027(13) 0.2321(8) 0.6829(6) 0.032(3) Uani 1 1 d . . . 
H34 H -0.1965 0.2522 0.6848 0.038 Uiso 1 1 calc R . . 
C37 C -0.0369(14) 0.1889(8) 0.7319(6) 0.033(3) Uani 1 1 d . . . 
H35 H -0.0771 0.1728 0.7719 0.040 Uiso 1 1 calc R . . 
C38 C 0.0986(14) 0.1749(9) 0.7094(6) 0.036(3) Uani 1 1 d . . . 
H36 H 0.1702 0.1483 0.7325 0.043 Uiso 1 1 calc R . . 
C39 C 0.0128(12) 0.0920(8) 0.4400(5) 0.023(3) Uani 1 1 d . . . 
H37 H -0.0685 0.0886 0.4081 0.027 Uiso 1 1 calc R . . 
C40 C 0.1183(12) 0.0264(8) 0.4319(6) 0.028(3) Uani 1 1 d . . . 
H38 H 0.1233 -0.0278 0.3941 0.034 Uiso 1 1 calc R . . 
C41 C 0.2118(12) 0.0590(8) 0.4910(6) 0.026(3) Uani 1 1 d . . . 
H39 H 0.2936 0.0288 0.5011 0.031 Uiso 1 1 calc R . . 
C42 C 0.2451(12) 0.4493(8) 0.5516(5) 0.024(3) Uani 1 1 d . . . 
H40 H 0.1986 0.4966 0.5335 0.029 Uiso 1 1 calc R . . 
C43 C 0.3952(12) 0.4635(8) 0.5700(5) 0.025(3) Uani 1 1 d . . . 
H41 H 0.4693 0.5200 0.5665 0.030 Uiso 1 1 calc R . . 
C44 C 0.4149(13) 0.3786(9) 0.5945(5) 0.030(3) Uani 1 1 d . . . 
H42 H 0.5067 0.3667 0.6117 0.036 Uiso 1 1 calc R . . 
C1S C 0.4892(15) -0.0123(11) 0.3690(7) 0.053(4) Uani 1 1 d . . . 
H27 H 0.4143 0.0285 0.3614 0.080 Uiso 1 1 calc R . . 
H28 H 0.5106 -0.0059 0.4181 0.080 Uiso 1 1 calc R . . 
H29 H 0.4519 -0.0847 0.3472 0.080 Uiso 1 1 calc R . . 
C2S C 0.6279(16) 0.0261(10) 0.3389(6) 0.040(3) Uani 1 1 d . . . 
N1S N 0.7325(10) 0.0531(8) 0.3134(6) 0.039(3) Uani 1 1 d . . . 
C3S C 0.8042(19) 0.7659(14) 0.0987(8) 0.078(5) Uani 1 1 d . . . 
H31 H 0.8427 0.7371 0.1353 0.117 Uiso 1 1 calc R . . 
H32 H 0.8602 0.7512 0.0589 0.117 Uiso 1 1 calc R . . 
H33 H 0.6995 0.7349 0.0863 0.117 Uiso 1 1 calc R . . 
C4S C 0.819(2) 0.8771(17) 0.1222(9) 0.072(5) Uani 1 1 d . . . 
N2S N 0.8222(18) 0.9629(14) 0.1409(9) 0.094(5) Uani 1 1 d . . . 
O1S O 0.593(4) 0.524(2) 0.0000(12) 0.126(13) Uani 0.50 1 d PU . . 
 
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 
Ni1 0.0192(9) 0.0174(9) 0.0195(9) 0.0019(6) 0.0047(6) 0.0029(6) 
Fe1 0.0226(10) 0.0172(10) 0.0222(10) 0.0033(7) 0.0034(7) 0.0051(7) 
P1 0.049(3) 0.058(3) 0.072(3) 0.013(2) 0.004(2) 0.011(2) 
F1 0.040(5) 0.077(6) 0.108(7) 0.022(5) 0.000(5) 0.003(4) 
F2 0.038(4) 0.068(5) 0.041(4) 0.031(4) 0.004(3) 0.011(4) 
F3 0.079(7) 0.173(11) 0.139(10) 0.114(9) 0.046(7) 0.046(7) 
F4 0.112(8) 0.061(6) 0.111(8) -0.002(6) -0.004(7) 0.032(6) 
F5 0.095(8) 0.046(6) 0.160(10) -0.025(6) -0.035(7) 0.024(5) 
F6 0.056(6) 0.107(8) 0.135(9) 0.037(7) -0.014(6) 0.014(6) 
N1 0.015(4) 0.017(4) 0.019(5) 0.001(4) -0.003(4) 0.005(4) 
N2 0.024(5) 0.024(5) 0.019(5) 0.010(4) 0.005(4) 0.008(4) 
N3 0.029(6) 0.014(5) 0.051(7) 0.008(5) 0.005(5) 0.006(5) 
N4 0.019(5) 0.022(5) 0.025(5) 0.005(4) 0.002(4) 0.002(4) 
N5 0.019(5) 0.022(5) 0.015(5) -0.001(4) -0.003(4) 0.004(4) 
N6 0.025(5) 0.013(5) 0.018(5) -0.001(4) 0.008(4) 0.002(4) 
N7 0.019(5) 0.019(5) 0.018(5) -0.001(4) 0.010(4) 0.001(4) 
N8 0.022(5) 0.023(5) 0.018(5) 0.003(4) 0.002(4) 0.003(4) 
N9 0.011(5) 0.038(6) 0.016(5) 0.008(4) -0.005(4) 0.005(4) 
N10 0.021(5) 0.017(5) 0.024(5) -0.001(4) 0.005(4) 0.005(4) 
N11 0.036(6) 0.023(5) 0.023(5) 0.005(4) 0.004(5) 0.010(5) 
N12 0.023(5) 0.016(5) 0.031(6) 0.010(4) 0.006(4) 0.009(4) 
N13 0.028(6) 0.022(5) 0.026(5) 0.003(4) 0.004(4) 0.011(4) 
B1 0.030(8) 0.026(8) 0.014(7) 0.010(6) 0.006(6) 0.013(6) 
C1 0.010(5) 0.018(5) 0.031(6) -0.004(5) -0.004(5) 0.001(4) 
C2 0.011(5) 0.028(6) 0.016(5) 0.011(5) -0.005(4) -0.002(5) 
C3 0.030(7) 0.013(6) 0.035(7) 0.000(5) 0.014(6) 0.008(5) 
C4 0.023(6) 0.025(7) 0.022(6) 0.003(5) 0.009(5) 0.008(5) 
C5 0.025(7) 0.027(7) 0.016(6) 0.005(5) 0.012(5) 0.002(5) 
C6 0.021(6) 0.026(6) 0.024(7) 0.009(5) 0.014(5) 0.009(5) 
C7 0.030(7) 0.043(8) 0.024(7) 0.020(6) 0.009(6) 0.013(6) 
C8 0.028(7) 0.027(7) 0.017(6) -0.001(5) 0.008(5) 0.000(5) 
C9 0.014(6) 0.025(6) 0.022(6) 0.000(5) 0.009(5) 0.002(5) 
C10 0.027(7) 0.017(6) 0.028(7) 0.001(5) 0.002(5) 0.000(5) 
C11 0.034(7) 0.032(7) 0.028(7) -0.004(6) -0.008(6) 0.004(6) 
C12 0.038(8) 0.031(7) 0.023(7) -0.002(6) -0.002(6) -0.001(6) 
C13 0.030(7) 0.041(8) 0.026(7) 0.007(6) 0.006(6) 0.010(6) 
C14 0.014(6) 0.019(6) 0.026(7) 0.000(5) -0.003(5) -0.003(5) 
C15 0.023(7) 0.014(6) 0.023(6) -0.004(5) 0.007(5) -0.003(5) 
C16 0.037(8) 0.024(7) 0.029(7) 0.003(5) 0.000(6) 0.001(6) 
C17 0.042(7) 0.025(7) 0.022(6) 0.004(5) 0.000(6) 0.025(6) 
C18 0.032(7) 0.019(6) 0.024(7) -0.003(5) -0.005(5) 0.007(5) 
C19 0.025(7) 0.025(7) 0.017(6) -0.007(5) -0.004(5) -0.003(5) 
C20 0.028(7) 0.020(6) 0.026(7) -0.005(5) -0.001(5) 0.005(5) 
C21 0.031(7) 0.033(7) 0.026(7) -0.008(6) 0.004(6) -0.001(6) 
C22 0.021(7) 0.037(8) 0.036(8) -0.014(6) 0.005(6) 0.007(6) 
C23 0.030(7) 0.023(7) 0.040(8) -0.006(6) -0.002(6) 0.010(6) 
C24 0.012(6) 0.034(7) 0.025(6) 0.000(5) 0.007(5) -0.002(5) 
C25 0.020(6) 0.013(6) 0.025(6) -0.002(5) 0.005(5) -0.002(5) 
C26 0.025(7) 0.028(7) 0.038(8) 0.003(6) 0.010(6) 0.005(5) 
C27 0.016(6) 0.045(8) 0.024(7) 0.003(6) 0.003(5) 0.008(5) 
C28 0.028(7) 0.017(6) 0.032(7) 0.000(5) -0.005(6) 0.003(5) 
C29 0.021(6) 0.025(7) 0.028(7) -0.002(5) 0.015(5) 0.002(5) 
C30 0.014(6) 0.034(7) 0.018(6) -0.001(5) 0.005(5) 0.008(5) 
C31 0.014(6) 0.024(6) 0.020(6) 0.009(5) -0.001(5) -0.003(5) 
C32 0.026(7) 0.035(7) 0.020(6) 0.001(5) 0.004(5) 0.001(6) 
C33 0.019(7) 0.037(8) 0.043(8) 0.018(6) 0.005(6) 0.001(6) 
C34 0.017(6) 0.030(7) 0.024(6) 0.007(5) 0.010(5) 0.006(5) 
C35 0.025(7) 0.026(7) 0.020(6) 0.004(5) 0.006(5) -0.003(5) 
C36 0.031(7) 0.030(7) 0.037(8) 0.008(6) 0.016(6) 0.004(6) 
C37 0.058(9) 0.028(7) 0.021(7) 0.013(6) 0.010(6) 0.014(6) 
C38 0.042(8) 0.041(8) 0.035(8) 0.017(6) 0.009(6) 0.025(6) 
C39 0.024(6) 0.019(6) 0.025(7) 0.006(5) 0.008(5) -0.001(5) 
C40 0.033(7) 0.018(6) 0.030(7) -0.004(5) 0.013(6) 0.004(5) 
C41 0.025(7) 0.024(7) 0.033(7) 0.009(6) 0.011(6) 0.012(5) 
C42 0.032(7) 0.021(6) 0.021(6) 0.007(5) 0.000(5) 0.008(5) 
C43 0.020(6) 0.022(7) 0.027(7) -0.005(5) -0.004(5) -0.001(5) 
C44 0.026(7) 0.027(7) 0.028(7) -0.010(6) 0.006(5) -0.005(6) 
C1S 0.046(9) 0.064(10) 0.061(10) 0.025(8) 0.026(8) 0.021(8) 
C2S 0.051(9) 0.041(8) 0.027(7) -0.003(6) -0.008(7) 0.020(7) 
N1S 0.010(5) 0.044(7) 0.073(8) 0.038(6) 0.012(5) 0.005(5) 
C3S 0.074(12) 0.111(16) 0.053(11) 0.021(10) 0.019(9) 0.024(11) 
C4S 0.089(14) 0.091(15) 0.051(11) 0.031(11) 0.010(10) 0.039(13) 
N2S 0.092(13) 0.096(13) 0.102(13) 0.033(12) 0.013(10) 0.022(11) 
O1S 0.27(4) 0.09(2) 0.031(12) 0.007(13) 0.01(2) 0.08(3) 
 
_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. 
; 
 
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 
Ni1 N1 2.083(9) . ? 
Ni1 N6 2.083(9) . ? 
Ni1 N7 2.094(9) . ? 
Ni1 N2 2.097(9) . ? 
Ni1 N5 2.178(8) . ? 
Ni1 N4 2.185(8) . ? 
Fe1 C3 1.916(12) . ? 
Fe1 C2 1.922(12) 2_566 ? 
Fe1 C1 1.942(12) . ? 
Fe1 N9 1.960(9) . ? 
Fe1 N8 1.967(8) . ? 
Fe1 N10 1.980(9) . ? 
P1 F2 1.567(7) . ? 
P1 F3 1.586(10) . ? 
P1 F5 1.588(9) . ? 
P1 F1 1.605(9) . ? 
P1 F4 1.610(10) . ? 
P1 F6 1.613(10) . ? 
N1 C1 1.165(13) . ? 
N2 C2 1.161(13) . ? 
N3 C3 1.186(13) . ? 
N4 C5 1.456(13) . ? 
N4 C24 1.482(13) . ? 
N4 H1 0.9300 . ? 
N5 C15 1.467(13) . ? 
N5 C30 1.483(13) . ? 
N5 H2 0.9300 . ? 
N6 C25 1.345(12) . ? 
N6 C29 1.347(13) . ? 
N7 C31 1.336(12) . ? 
N7 C35 1.364(13) . ? 
N8 C36 1.379(13) . ? 
N8 N11 1.383(12) . ? 
N9 C39 1.368(13) . ? 
N9 N12 1.384(11) . ? 
N10 C42 1.355(12) . ? 
N10 N13 1.402(12) . ? 
N11 C38 1.356(13) . ? 
N11 B1 1.517(15) . ? 
N12 C41 1.341(13) . ? 
N12 B1 1.526(15) . ? 
N13 C44 1.349(13) . ? 
N13 B1 1.540(14) . ? 
B1 H30 1.0000 . ? 
C2 Fe1 1.923(12) 2_566 ? 
C4 C5 1.365(14) . ? 
C4 C9 1.453(15) . ? 
C4 C14 1.517(15) . ? 
C5 C6 1.402(15) . ? 
C6 C7 1.356(15) . ? 
C6 H3 0.9500 . ? 
C7 C8 1.414(15) . ? 
C7 H4 0.9500 . ? 
C8 C9 1.430(15) . ? 
C8 C13 1.436(15) . ? 
C9 C10 1.416(14) . ? 
C10 C11 1.370(15) . ? 
C10 H5 0.9500 . ? 
C11 C12 1.380(16) . ? 
C11 H6 0.9500 . ? 
C12 C13 1.387(15) . ? 
C12 H7 0.9500 . ? 
C13 H8 0.9500 . ? 
C14 C15 1.369(14) . ? 
C14 C19 1.443(15) . ? 
C15 C16 1.420(15) . ? 
C16 C17 1.352(15) . ? 
C16 H9 0.9500 . ? 
C17 C18 1.428(15) . ? 
C17 H10 0.9500 . ? 
C18 C19 1.440(15) . ? 
C18 C23 1.453(15) . ? 
C19 C20 1.432(15) . ? 
C20 C21 1.368(15) . ? 
C20 H11 0.9500 . ? 
C21 C22 1.397(17) . ? 
C21 H12 0.9500 . ? 
C22 C23 1.352(16) . ? 
C22 H13 0.9500 . ? 
C23 H14 0.9500 . ? 
C24 C25 1.521(15) . ? 
C24 H15 0.9900 . ? 
C24 H16 0.9900 . ? 
C25 C26 1.414(15) . ? 
C26 C27 1.376(15) . ? 
C26 H17 0.9500 . ? 
C27 C28 1.382(15) . ? 
C27 H18 0.9500 . ? 
C28 C29 1.411(15) . ? 
C28 H19 0.9500 . ? 
C29 H20 0.9500 . ? 
C30 C31 1.508(14) . ? 
C30 H21 0.9900 . ? 
C30 H22 0.9900 . ? 
C31 C32 1.413(15) . ? 
C32 C33 1.390(15) . ? 
C32 H23 0.9500 . ? 
C33 C34 1.379(15) . ? 
C33 H24 0.9500 . ? 
C34 C35 1.389(15) . ? 
C34 H25 0.9500 . ? 
C35 H26 0.9500 . ? 
C36 C37 1.408(16) . ? 
C36 H34 0.9500 . ? 
C37 C38 1.380(16) . ? 
C37 H35 0.9500 . ? 
C38 H36 0.9500 . ? 
C39 C40 1.420(15) . ? 
C39 H37 0.9500 . ? 
C40 C41 1.378(15) . ? 
C40 H38 0.9500 . ? 
C41 H39 0.9500 . ? 
C42 C43 1.383(14) . ? 
C42 H40 0.9500 . ? 
C43 C44 1.375(16) . ? 
C43 H41 0.9500 . ? 
C44 H42 0.9500 . ? 
C1S C2S 1.498(18) . ? 
C1S H27 0.9800 . ? 
C1S H28 0.9800 . ? 
C1S H29 0.9800 . ? 
C2S N1S 1.152(15) . ? 
C3S C4S 1.46(2) . ? 
C3S H31 0.9800 . ? 
C3S H32 0.9800 . ? 
C3S H33 0.9800 . ? 
C4S N2S 1.14(2) . ? 
 
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 Ni1 N6 95.9(3) . . ? 
N1 Ni1 N7 96.0(3) . . ? 
N6 Ni1 N7 165.6(3) . . ? 
N1 Ni1 N2 87.5(3) . . ? 
N6 Ni1 N2 93.7(3) . . ? 
N7 Ni1 N2 94.9(3) . . ? 
N1 Ni1 N5 89.1(3) . . ? 
N6 Ni1 N5 91.7(3) . . ? 
N7 Ni1 N5 80.4(3) . . ? 
N2 Ni1 N5 173.9(3) . . ? 
N1 Ni1 N4 175.8(3) . . ? 
N6 Ni1 N4 80.8(3) . . ? 
N7 Ni1 N4 87.7(3) . . ? 
N2 Ni1 N4 90.1(3) . . ? 
N5 Ni1 N4 93.6(3) . . ? 
C3 Fe1 C2 89.7(4) . 2_566 ? 
C3 Fe1 C1 89.0(4) . . ? 
C2 Fe1 C1 93.1(4) 2_566 . ? 
C3 Fe1 N9 93.4(4) . . ? 
C2 Fe1 N9 176.6(4) 2_566 . ? 
C1 Fe1 N9 88.3(4) . . ? 
C3 Fe1 N8 92.4(4) . . ? 
C2 Fe1 N8 89.9(4) 2_566 . ? 
C1 Fe1 N8 176.7(4) . . ? 
N9 Fe1 N8 88.6(4) . . ? 
C3 Fe1 N10 178.7(4) . . ? 
C2 Fe1 N10 89.1(4) 2_566 . ? 
C1 Fe1 N10 90.7(4) . . ? 
N9 Fe1 N10 87.9(3) . . ? 
N8 Fe1 N10 87.9(4) . . ? 
F2 P1 F3 176.5(6) . . ? 
F2 P1 F5 95.8(6) . . ? 
F3 P1 F5 87.6(7) . . ? 
F2 P1 F1 91.7(4) . . ? 
F3 P1 F1 89.3(5) . . ? 
F5 P1 F1 89.0(5) . . ? 
F2 P1 F4 85.7(5) . . ? 
F3 P1 F4 91.0(6) . . ? 
F5 P1 F4 178.4(7) . . ? 
F1 P1 F4 90.5(5) . . ? 
F2 P1 F6 87.5(5) . . ? 
F3 P1 F6 91.5(6) . . ? 
F5 P1 F6 90.3(6) . . ? 
F1 P1 F6 178.9(6) . . ? 
F4 P1 F6 90.2(6) . . ? 
C1 N1 Ni1 153.0(8) . . ? 
C2 N2 Ni1 153.1(8) . . ? 
C5 N4 C24 116.3(8) . . ? 
C5 N4 Ni1 114.9(6) . . ? 
C24 N4 Ni1 110.3(6) . . ? 
C5 N4 H1 104.6 . . ? 
C24 N4 H1 104.6 . . ? 
Ni1 N4 H1 104.6 . . ? 
C15 N5 C30 116.3(8) . . ? 
C15 N5 Ni1 112.7(6) . . ? 
C30 N5 Ni1 110.6(6) . . ? 
C15 N5 H2 105.4 . . ? 
C30 N5 H2 105.4 . . ? 
Ni1 N5 H2 105.4 . . ? 
C25 N6 C29 118.0(9) . . ? 
C25 N6 Ni1 116.2(7) . . ? 
C29 N6 Ni1 125.6(7) . . ? 
C31 N7 C35 119.7(9) . . ? 
C31 N7 Ni1 114.9(7) . . ? 
C35 N7 Ni1 124.1(7) . . ? 
C36 N8 N11 106.3(8) . . ? 
C36 N8 Fe1 133.1(8) . . ? 
N11 N8 Fe1 120.3(6) . . ? 
C39 N9 N12 107.3(9) . . ? 
C39 N9 Fe1 132.9(7) . . ? 
N12 N9 Fe1 119.6(6) . . ? 
C42 N10 N13 105.4(8) . . ? 
C42 N10 Fe1 134.7(8) . . ? 
N13 N10 Fe1 119.7(6) . . ? 
C38 N11 N8 109.0(9) . . ? 
C38 N11 B1 132.9(10) . . ? 
N8 N11 B1 118.1(8) . . ? 
C41 N12 N9 108.4(9) . . ? 
C41 N12 B1 132.7(10) . . ? 
N9 N12 B1 118.9(8) . . ? 
C44 N13 N10 108.9(9) . . ? 
C44 N13 B1 133.3(10) . . ? 
N10 N13 B1 117.4(8) . . ? 
N11 B1 N12 107.9(9) . . ? 
N11 B1 N13 108.4(9) . . ? 
N12 B1 N13 105.7(8) . . ? 
N11 B1 H30 111.6 . . ? 
N12 B1 H30 111.6 . . ? 
N13 B1 H30 111.6 . . ? 
N1 C1 Fe1 173.3(9) . . ? 
N2 C2 Fe1 172.3(9) . 2_566 ? 
N3 C3 Fe1 177.4(11) . . ? 
C5 C4 C9 120.8(10) . . ? 
C5 C4 C14 120.4(10) . . ? 
C9 C4 C14 118.8(9) . . ? 
C4 C5 C6 119.9(10) . . ? 
C4 C5 N4 122.6(10) . . ? 
C6 C5 N4 117.4(9) . . ? 
C7 C6 C5 121.4(11) . . ? 
C7 C6 H3 119.3 . . ? 
C5 C6 H3 119.3 . . ? 
C6 C7 C8 121.4(11) . . ? 
C6 C7 H4 119.3 . . ? 
C8 C7 H4 119.3 . . ? 
C7 C8 C9 118.7(10) . . ? 
C7 C8 C13 122.2(11) . . ? 
C9 C8 C13 119.0(10) . . ? 
C10 C9 C8 119.2(10) . . ? 
C10 C9 C4 122.8(10) . . ? 
C8 C9 C4 117.9(9) . . ? 
C11 C10 C9 119.6(11) . . ? 
C11 C10 H5 120.2 . . ? 
C9 C10 H5 120.2 . . ? 
C10 C11 C12 122.1(11) . . ? 
C10 C11 H6 119.0 . . ? 
C12 C11 H6 119.0 . . ? 
C11 C12 C13 120.8(11) . . ? 
C11 C12 H7 119.6 . . ? 
C13 C12 H7 119.6 . . ? 
C12 C13 C8 119.1(11) . . ? 
C12 C13 H8 120.5 . . ? 
C8 C13 H8 120.5 . . ? 
C15 C14 C19 118.5(10) . . ? 
C15 C14 C4 122.4(10) . . ? 
C19 C14 C4 119.0(9) . . ? 
C14 C15 C16 121.2(10) . . ? 
C14 C15 N5 120.9(10) . . ? 
C16 C15 N5 117.8(9) . . ? 
C17 C16 C15 122.3(11) . . ? 
C17 C16 H9 118.9 . . ? 
C15 C16 H9 118.9 . . ? 
C16 C17 C18 119.0(10) . . ? 
C16 C17 H10 120.5 . . ? 
C18 C17 H10 120.5 . . ? 
C17 C18 C19 119.5(10) . . ? 
C17 C18 C23 121.8(10) . . ? 
C19 C18 C23 118.6(10) . . ? 
C20 C19 C18 117.2(10) . . ? 
C20 C19 C14 123.4(11) . . ? 
C18 C19 C14 119.4(10) . . ? 
C21 C20 C19 121.8(11) . . ? 
C21 C20 H11 119.1 . . ? 
C19 C20 H11 119.1 . . ? 
C20 C21 C22 120.7(11) . . ? 
C20 C21 H12 119.7 . . ? 
C22 C21 H12 119.7 . . ? 
C23 C22 C21 121.0(11) . . ? 
C23 C22 H13 119.5 . . ? 
C21 C22 H13 119.5 . . ? 
C22 C23 C18 120.7(11) . . ? 
C22 C23 H14 119.7 . . ? 
C18 C23 H14 119.7 . . ? 
N4 C24 C25 113.8(8) . . ? 
N4 C24 H15 108.8 . . ? 
C25 C24 H15 108.8 . . ? 
N4 C24 H16 108.8 . . ? 
C25 C24 H16 108.8 . . ? 
H15 C24 H16 107.7 . . ? 
N6 C25 C26 121.4(10) . . ? 
N6 C25 C24 118.1(9) . . ? 
C26 C25 C24 120.3(9) . . ? 
C27 C26 C25 120.2(10) . . ? 
C27 C26 H17 119.9 . . ? 
C25 C26 H17 119.9 . . ? 
C26 C27 C28 118.7(11) . . ? 
C26 C27 H18 120.6 . . ? 
C28 C27 H18 120.6 . . ? 
C27 C28 C29 118.4(11) . . ? 
C27 C28 H19 120.8 . . ? 
C29 C28 H19 120.8 . . ? 
N6 C29 C28 123.2(10) . . ? 
N6 C29 H20 118.4 . . ? 
C28 C29 H20 118.4 . . ? 
N5 C30 C31 112.7(8) . . ? 
N5 C30 H21 109.0 . . ? 
C31 C30 H21 109.0 . . ? 
N5 C30 H22 109.0 . . ? 
C31 C30 H22 109.0 . . ? 
H21 C30 H22 107.8 . . ? 
N7 C31 C32 120.6(10) . . ? 
N7 C31 C30 118.7(9) . . ? 
C32 C31 C30 120.7(9) . . ? 
C33 C32 C31 119.1(10) . . ? 
C33 C32 H23 120.4 . . ? 
C31 C32 H23 120.4 . . ? 
C34 C33 C32 119.8(11) . . ? 
C34 C33 H24 120.1 . . ? 
C32 C33 H24 120.1 . . ? 
C33 C34 C35 118.6(11) . . ? 
C33 C34 H25 120.7 . . ? 
C35 C34 H25 120.7 . . ? 
N7 C35 C34 122.0(10) . . ? 
N7 C35 H26 119.0 . . ? 
C34 C35 H26 119.0 . . ? 
N8 C36 C37 109.6(11) . . ? 
N8 C36 H34 125.2 . . ? 
C37 C36 H34 125.2 . . ? 
C38 C37 C36 105.1(10) . . ? 
C38 C37 H35 127.5 . . ? 
C36 C37 H35 127.5 . . ? 
N11 C38 C37 110.0(11) . . ? 
N11 C38 H36 125.0 . . ? 
C37 C38 H36 125.0 . . ? 
N9 C39 C40 108.9(10) . . ? 
N9 C39 H37 125.5 . . ? 
C40 C39 H37 125.5 . . ? 
C41 C40 C39 104.5(10) . . ? 
C41 C40 H38 127.7 . . ? 
C39 C40 H38 127.7 . . ? 
N12 C41 C40 110.9(10) . . ? 
N12 C41 H39 124.6 . . ? 
C40 C41 H39 124.6 . . ? 
N10 C42 C43 110.8(10) . . ? 
N10 C42 H40 124.6 . . ? 
C43 C42 H40 124.6 . . ? 
C44 C43 C42 105.7(10) . . ? 
C44 C43 H41 127.2 . . ? 
C42 C43 H41 127.2 . . ? 
N13 C44 C43 109.2(11) . . ? 
N13 C44 H42 125.4 . . ? 
C43 C44 H42 125.4 . . ? 
C2S C1S H27 109.5 . . ? 
C2S C1S H28 109.5 . . ? 
H27 C1S H28 109.5 . . ? 
C2S C1S H29 109.5 . . ? 
H27 C1S H29 109.5 . . ? 
H28 C1S H29 109.5 . . ? 
N1S C2S C1S 177.4(14) . . ? 
C4S C3S H31 109.5 . . ? 
C4S C3S H32 109.5 . . ? 
H31 C3S H32 109.5 . . ? 
C4S C3S H33 109.5 . . ? 
H31 C3S H33 109.5 . . ? 
H32 C3S H33 109.5 . . ? 
N2S C4S C3S 176(2) . . ? 
 
_diffrn_measured_fraction_theta_max    0.962 
_diffrn_reflns_theta_full              24.15 
_diffrn_measured_fraction_theta_full   0.962 
_refine_diff_density_max    0.821 
_refine_diff_density_min   -0.859 
_refine_diff_density_rms    0.132 


data_2
_publ_requested_journal          Chem.Commun.
_publ_contact_author_name        'Prof. Hiroki Oshio'
_publ_contact_author_address     
;
 Graduate School of Pure and Applied Sciences
 University of Tsukuba
 Tennodai 1-1-1, Tsukuba 305-8571
;
_publ_contact_author_email       oshio@chem.tsukuba.ac.jp
_publ_contact_author_phone       +81-29-853-4238
_publ_contact_author_fax         +81-29-853-4238
loop_
_publ_author_name
_publ_author_address
'Hoshino, N.'
;
 Graduate School of Pure and Applied Sciences
 University of Tsukuba
 Tennodai 1-1-1, Tsukuba 305-8571
;
'Sekine, Y.'
;
 Graduate School of Pure and Applied Sciences
 University of Tsukuba
 Tennodai 1-1-1, Tsukuba 305-8571
;
'Nihei, M.'
;
 Graduate School of Pure and Applied Sciences
 University of Tsukuba
 Tennodai 1-1-1, Tsukuba 305-8571
;
'Oshio, H.'
;
 Graduate School of Pure and Applied Sciences
 University of Tsukuba
 Tennodai 1-1-1, Tsukuba 305-8571
;

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 catena-[Ni(II)((R)-pabn))][Fe(III)(tp)(CN)3]PF6.2MeOH
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety
 'C44 H36 B Fe N13 Ni, F6 P, 2(C H4 O)'
_chemical_formula_sum 
 'C46 H44 B F6 Fe N13 Ni O2 P' 
_chemical_formula_weight          1081.28 
_chemical_absolute_configuration  'ad' 
 
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' 
 'B'  'B'   0.0013   0.0007 
 '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' 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'P'  'P'   0.1023   0.0942 
 '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' 
 
_symmetry_cell_setting           'Orthorhombic'
_symmetry_space_group_name_H-M   'P2(1)2(1)2(1) '
_symmetry_space_group_name_Hall  'P 2ac 2ab'
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 
_cell_length_a                    10.6762(9) 
_cell_length_b                    17.5426(15) 
_cell_length_c                    25.176(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      4715.2(7) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     7730
_cell_measurement_theta_min       2.23
_cell_measurement_theta_max       22.31
 
_exptl_crystal_description        'tablet' 
_exptl_crystal_colour             'brown' 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.04 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.523 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2220 
_exptl_absorpt_coefficient_mu     0.820 
_exptl_absorpt_correction_type    'empirical'
_exptl_absorpt_correction_T_min   0.8532 
_exptl_absorpt_correction_T_max   0.9758 
_exptl_absorpt_process_details    'SADABS (Sheldrick, 1996)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Bruker TXS fine-focus rotating anode' 
_diffrn_radiation_monochromator   'Bruker Helios multilayer confocal mirror' 
_diffrn_measurement_device_type   'Bruker APEXII CCD area detector' 
_diffrn_measurement_method        'phi and omega scans' 
_diffrn_detector_area_resol_mean  8.333
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             53177 
_diffrn_reflns_av_R_equivalents   0.0731 
_diffrn_reflns_av_sigmaI/netI     0.0637 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        22 
_diffrn_reflns_limit_l_min        -31 
_diffrn_reflns_limit_l_max        32 
_diffrn_reflns_theta_min          1.41 
_diffrn_reflns_theta_max          27.00 
_reflns_number_total              10307 
_reflns_number_gt                 8348 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement        'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction         'SAINT (Bruker AXS, 2004)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'XSHEL (Bruker AXS,2002)'
_computing_publication_material   'XCIF (Bruker AXS, 2001)' 
 
_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. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+4.5324P] 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 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.012(14) 
_refine_ls_number_reflns          10307 
_refine_ls_number_parameters      642 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0687 
_refine_ls_R_factor_gt            0.0475 
_refine_ls_wR_factor_ref          0.1149 
_refine_ls_wR_factor_gt           0.1051 
_refine_ls_goodness_of_fit_ref    1.057 
_refine_ls_restrained_S_all       1.057 
_refine_ls_shift/su_max           0.000 
_refine_ls_shift/su_mean          0.000 
 
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 0.36446(5) 0.27903(3) 0.07906(2) 0.01322(12) Uani 1 1 d . . . 
Ni1 Ni 0.79244(4) 0.40297(3) 0.069921(19) 0.01359(11) Uani 1 1 d . . . 
N1 N 0.6141(3) 0.36074(19) 0.05762(13) 0.0165(7) Uani 1 1 d . . . 
N2 N 0.8633(3) 0.32327(19) 0.01904(13) 0.0169(7) Uani 1 1 d . . . 
N3 N 0.2107(4) 0.3910(2) 0.01165(14) 0.0249(8) Uani 1 1 d . . . 
N4 N 0.9806(3) 0.44110(18) 0.08781(13) 0.0142(7) Uani 1 1 d . . . 
H1 H 1.0290 0.4243 0.0594 0.017 Uiso 1 1 calc R . . 
N5 N 0.7042(3) 0.49190(19) 0.11674(13) 0.0187(7) Uani 1 1 d . . . 
H2 H 0.6244 0.4734 0.1239 0.022 Uiso 1 1 calc R . . 
N6 N 0.8244(3) 0.3397(2) 0.13767(13) 0.0173(8) Uani 1 1 d . . . 
N7 N 0.7750(3) 0.48753(19) 0.01207(13) 0.0159(7) Uani 1 1 d . . . 
N8 N 0.3545(3) 0.3434(2) 0.14337(14) 0.0203(8) Uani 1 1 d . . . 
N9 N 0.4563(3) 0.19949(18) 0.11981(14) 0.0171(7) Uani 1 1 d . . . 
N10 N 0.2095(3) 0.22954(19) 0.10137(12) 0.0162(7) Uani 1 1 d . . . 
N11 N 0.3314(3) 0.3105(2) 0.19165(14) 0.0229(8) Uani 1 1 d . . . 
N12 N 0.4179(3) 0.1827(2) 0.17014(14) 0.0204(8) Uani 1 1 d . . . 
N13 N 0.1957(3) 0.2095(2) 0.15382(13) 0.0197(8) Uani 1 1 d . . . 
B1 B 0.3045(5) 0.2251(3) 0.19325(19) 0.0250(11) Uani 1 1 d . . . 
H3 H 0.2840 0.2073 0.2300 0.030 Uiso 1 1 calc R . . 
C1 C 0.5197(4) 0.3300(2) 0.06147(15) 0.0149(8) Uani 1 1 d . . . 
C2 C 0.3700(4) 0.2180(2) 0.01644(15) 0.0152(8) Uani 1 1 d . . . 
C3 C 0.2707(4) 0.3505(2) 0.03703(16) 0.0168(8) Uani 1 1 d . . . 
C4 C 0.9453(4) 0.5671(2) 0.12871(16) 0.0138(8) Uani 1 1 d . . . 
C5 C 0.9957(4) 0.5222(2) 0.08830(15) 0.0143(8) Uani 1 1 d . . . 
C6 C 1.0567(4) 0.5560(2) 0.04420(16) 0.0173(9) Uani 1 1 d . . . 
H4 H 1.0927 0.5243 0.0177 0.021 Uiso 1 1 calc R . . 
C7 C 1.0645(4) 0.6330(2) 0.03920(17) 0.0221(10) Uani 1 1 d . . . 
H5 H 1.1055 0.6545 0.0093 0.027 Uiso 1 1 calc R . . 
C8 C 1.0116(4) 0.6816(2) 0.07860(18) 0.0226(9) Uani 1 1 d . . . 
C9 C 0.9541(4) 0.6487(2) 0.12342(16) 0.0178(9) Uani 1 1 d . . . 
C10 C 0.8978(4) 0.6981(2) 0.16210(17) 0.0211(9) Uani 1 1 d . . . 
H6 H 0.8581 0.6771 0.1925 0.025 Uiso 1 1 calc R . . 
C11 C 0.9012(4) 0.7748(3) 0.15538(17) 0.0250(10) Uani 1 1 d . . . 
H7 H 0.8636 0.8069 0.1812 0.030 Uiso 1 1 calc R . . 
C12 C 0.9590(5) 0.8071(3) 0.11119(19) 0.0304(11) Uani 1 1 d . . . 
H8 H 0.9606 0.8609 0.1071 0.037 Uiso 1 1 calc R . . 
C13 C 1.0135(4) 0.7616(2) 0.0738(2) 0.0306(11) Uani 1 1 d . . . 
H9 H 1.0534 0.7842 0.0440 0.037 Uiso 1 1 calc R . . 
C14 C 0.8782(4) 0.5330(2) 0.17438(15) 0.0136(8) Uani 1 1 d . . . 
C15 C 0.7613(4) 0.5013(2) 0.16867(16) 0.0153(8) Uani 1 1 d . . . 
C16 C 0.6970(4) 0.4700(2) 0.21296(16) 0.0212(9) Uani 1 1 d . . . 
H10 H 0.6147 0.4505 0.2083 0.025 Uiso 1 1 calc R . . 
C17 C 0.7498(4) 0.4673(2) 0.26107(17) 0.0224(10) Uani 1 1 d . . . 
H11 H 0.7043 0.4463 0.2900 0.027 Uiso 1 1 calc R . . 
C18 C 0.8742(4) 0.4956(2) 0.26947(16) 0.0187(9) Uani 1 1 d . . . 
C19 C 0.9380(4) 0.5302(2) 0.22575(16) 0.0163(8) Uani 1 1 d . . . 
C20 C 1.0606(4) 0.5562(2) 0.23362(17) 0.0179(9) Uani 1 1 d . . . 
H12 H 1.1036 0.5803 0.2052 0.021 Uiso 1 1 calc R . . 
C21 C 1.1196(4) 0.5475(2) 0.28133(17) 0.0232(10) Uani 1 1 d . . . 
H13 H 1.2028 0.5658 0.2857 0.028 Uiso 1 1 calc R . . 
C22 C 1.0581(5) 0.5117(2) 0.32442(18) 0.0270(10) Uani 1 1 d . . . 
H14 H 1.1003 0.5047 0.3573 0.032 Uiso 1 1 calc R . . 
C23 C 0.9369(5) 0.4872(2) 0.31813(17) 0.0257(10) Uani 1 1 d . . . 
H15 H 0.8947 0.4642 0.3472 0.031 Uiso 1 1 calc R . . 
C24 C 0.7394(4) 0.2936(2) 0.16158(17) 0.0222(10) Uani 1 1 d . . . 
H16 H 0.6645 0.2818 0.1430 0.027 Uiso 1 1 calc R . . 
C25 C 0.7562(4) 0.2631(3) 0.21131(17) 0.0263(10) Uani 1 1 d . . . 
H17 H 0.6947 0.2306 0.2264 0.032 Uiso 1 1 calc R . . 
C26 C 0.8652(5) 0.2809(3) 0.23919(17) 0.0278(10) Uani 1 1 d . . . 
H18 H 0.8788 0.2617 0.2740 0.033 Uiso 1 1 calc R . . 
C27 C 0.9531(4) 0.3271(2) 0.21500(18) 0.0226(9) Uani 1 1 d . . . 
H19 H 1.0280 0.3403 0.2332 0.027 Uiso 1 1 calc R . . 
C28 C 0.9313(4) 0.3541(2) 0.16406(16) 0.0160(8) Uani 1 1 d . . . 
C29 C 0.8180(4) 0.4820(3) -0.03780(16) 0.0240(10) Uani 1 1 d . . . 
H20 H 0.8439 0.4335 -0.0505 0.029 Uiso 1 1 calc R . . 
C30 C 0.8261(4) 0.5437(3) -0.07140(19) 0.0294(10) Uani 1 1 d . . . 
H21 H 0.8549 0.5373 -0.1068 0.035 Uiso 1 1 calc R . . 
C31 C 0.7920(5) 0.6153(3) -0.05314(18) 0.0332(11) Uani 1 1 d . . . 
H22 H 0.7998 0.6590 -0.0752 0.040 Uiso 1 1 calc R . . 
C32 C 0.7462(4) 0.6215(3) -0.00175(19) 0.0292(11) Uani 1 1 d . . . 
H23 H 0.7205 0.6696 0.0118 0.035 Uiso 1 1 calc R . . 
C33 C 0.7383(4) 0.5561(2) 0.02990(16) 0.0185(9) Uani 1 1 d . . . 
C34 C 1.0297(4) 0.3989(2) 0.13492(15) 0.0163(8) Uani 1 1 d . . . 
H24 H 1.0680 0.4359 0.1598 0.020 Uiso 1 1 calc R . . 
H25 H 1.0964 0.3636 0.1230 0.020 Uiso 1 1 calc R . . 
C35 C 0.6828(4) 0.5613(2) 0.08485(16) 0.0231(10) Uani 1 1 d . . . 
H26 H 0.7199 0.6056 0.1035 0.028 Uiso 1 1 calc R . . 
H27 H 0.5915 0.5703 0.0818 0.028 Uiso 1 1 calc R . . 
C36 C 0.3297(4) 0.3665(3) 0.22906(18) 0.0289(11) Uani 1 1 d . . . 
H28 H 0.3157 0.3590 0.2660 0.035 Uiso 1 1 calc R . . 
C37 C 0.3514(4) 0.4357(3) 0.20481(19) 0.0304(11) Uani 1 1 d . . . 
H29 H 0.3556 0.4845 0.2211 0.036 Uiso 1 1 calc R . . 
C38 C 0.3655(4) 0.4185(2) 0.15184(18) 0.0247(10) Uani 1 1 d . . . 
H30 H 0.3811 0.4551 0.1248 0.030 Uiso 1 1 calc R . . 
C39 C 0.4821(4) 0.1208(3) 0.1871(2) 0.0305(11) Uani 1 1 d . . . 
H31 H 0.4731 0.0975 0.2210 0.037 Uiso 1 1 calc R . . 
C40 C 0.5623(4) 0.0968(3) 0.14767(19) 0.0310(11) Uani 1 1 d . . . 
H32 H 0.6180 0.0546 0.1486 0.037 Uiso 1 1 calc R . . 
C41 C 0.5439(4) 0.1482(2) 0.10598(18) 0.0209(9) Uani 1 1 d . . . 
H33 H 0.5868 0.1470 0.0729 0.025 Uiso 1 1 calc R . . 
C42 C 0.0832(4) 0.1767(2) 0.16022(18) 0.0232(10) Uani 1 1 d . . . 
H34 H 0.0507 0.1576 0.1927 0.028 Uiso 1 1 calc R . . 
C43 C 0.0219(4) 0.1753(3) 0.11157(19) 0.0246(10) Uani 1 1 d . . . 
H35 H -0.0591 0.1556 0.1042 0.030 Uiso 1 1 calc R . . 
C44 C 0.1042(3) 0.2087(2) 0.07637(17) 0.0182(8) Uani 1 1 d . . . 
H36 H 0.0885 0.2159 0.0396 0.022 Uiso 1 1 calc R . . 
P1 P 0.40246(14) 0.66440(8) 0.15519(5) 0.0364(3) Uani 1 1 d . . . 
F1 F 0.2976(5) 0.7226(3) 0.14223(18) 0.1025(16) Uani 1 1 d . . . 
F2 F 0.4656(5) 0.7250(3) 0.19310(16) 0.0970(16) Uani 1 1 d . . . 
F3 F 0.5087(4) 0.6051(3) 0.17056(17) 0.111(2) Uani 1 1 d . . . 
F4 F 0.3474(7) 0.6015(3) 0.11910(16) 0.128(2) Uani 1 1 d . . . 
F5 F 0.4806(5) 0.6941(2) 0.10557(16) 0.0852(14) Uani 1 1 d . . . 
F6 F 0.3266(3) 0.63361(19) 0.20513(13) 0.0554(10) Uani 1 1 d . . . 
C1S C 0.6094(7) 0.8566(4) 0.1186(3) 0.073(2) Uani 1 1 d . . . 
H37 H 0.6257 0.8111 0.1401 0.109 Uiso 1 1 calc . . . 
H38 H 0.6274 0.8456 0.0813 0.109 Uiso 1 1 calc . . . 
H39 H 0.5213 0.8714 0.1224 0.109 Uiso 1 1 calc . . . 
O1S O 0.6859(5) 0.9163(3) 0.13599(18) 0.0642(13) Uani 1 1 d . . . 
H40 H 0.7244 0.9349 0.1099 0.080 Uiso 1 1 calc R . . 
C2S C 0.9063(9) 0.9665(5) 0.0123(3) 0.108(4) Uani 1 1 d . . . 
H41 H 0.9026 0.9120 0.0041 0.161 Uiso 1 1 calc . . . 
H42 H 0.9879 0.9787 0.0279 0.161 Uiso 1 1 calc . . . 
H43 H 0.8947 0.9961 -0.0203 0.161 Uiso 1 1 calc . . . 
O2S O 0.8107(4) 0.9850(2) 0.04874(14) 0.0467(10) Uani 1 1 d . . . 
H44 H 0.7778 1.0267 0.0400 0.080 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 0.0109(3) 0.0138(3) 0.0150(3) -0.0012(2) 0.0001(2) -0.0007(2) 
Ni1 0.0115(2) 0.0166(2) 0.0127(2) -0.0023(2) 0.0007(2) -0.0018(2) 
N1 0.0175(18) 0.0176(17) 0.0144(17) -0.0020(13) 0.0001(14) 0.0008(14) 
N2 0.0156(17) 0.0162(18) 0.0189(18) 0.0008(14) -0.0008(15) -0.0010(15) 
N3 0.0214(19) 0.024(2) 0.029(2) -0.0014(16) -0.0017(17) 0.0038(18) 
N4 0.0117(16) 0.0154(16) 0.0153(17) -0.0043(13) 0.0037(13) -0.0013(13) 
N5 0.0130(17) 0.0285(19) 0.0148(16) -0.0039(14) 0.0021(15) -0.0032(16) 
N6 0.0157(18) 0.0209(19) 0.0153(17) -0.0011(14) -0.0005(14) -0.0029(14) 
N7 0.0109(17) 0.0224(18) 0.0144(17) -0.0016(14) -0.0020(14) 0.0007(14) 
N8 0.0138(17) 0.026(2) 0.0207(18) -0.0034(15) 0.0004(15) 0.0003(16) 
N9 0.0122(17) 0.0185(18) 0.0205(18) 0.0038(14) -0.0032(14) -0.0036(14) 
N10 0.0145(16) 0.0176(17) 0.0167(16) -0.0002(13) -0.0017(14) -0.0018(15) 
N11 0.0166(18) 0.035(2) 0.0170(19) -0.0021(16) -0.0025(14) -0.0074(15) 
N12 0.0190(18) 0.0236(19) 0.0187(18) 0.0092(15) -0.0059(15) -0.0054(15) 
N13 0.0174(17) 0.0242(19) 0.0174(17) 0.0069(15) 0.0012(15) -0.0051(16) 
B1 0.022(2) 0.036(3) 0.017(2) 0.003(2) 0.000(2) 0.001(2) 
C1 0.019(2) 0.0138(19) 0.012(2) -0.0026(15) 0.0011(16) 0.0020(16) 
C2 0.0092(18) 0.0153(19) 0.021(2) 0.0042(18) 0.0010(16) -0.0025(17) 
C3 0.011(2) 0.019(2) 0.020(2) -0.0009(17) 0.0033(17) -0.0028(17) 
C4 0.0111(19) 0.0146(19) 0.016(2) -0.0029(15) -0.0011(16) 0.0019(15) 
C5 0.0106(18) 0.0155(19) 0.017(2) -0.0012(16) -0.0022(15) -0.0040(15) 
C6 0.014(2) 0.020(2) 0.018(2) -0.0013(17) 0.0033(17) -0.0001(17) 
C7 0.027(2) 0.021(2) 0.019(2) 0.0012(17) 0.0094(19) -0.0041(18) 
C8 0.023(2) 0.020(2) 0.026(2) -0.0014(19) 0.001(2) -0.0033(17) 
C9 0.015(2) 0.021(2) 0.017(2) -0.0034(17) -0.0044(17) 0.0033(17) 
C10 0.022(2) 0.023(2) 0.018(2) -0.0070(17) -0.0054(18) 0.0030(17) 
C11 0.028(2) 0.024(2) 0.024(2) -0.010(2) -0.0044(18) 0.006(2) 
C12 0.043(3) 0.017(2) 0.031(3) 0.002(2) -0.005(2) -0.001(2) 
C13 0.039(3) 0.025(2) 0.028(2) 0.003(2) 0.006(2) -0.0065(19) 
C14 0.017(2) 0.0090(18) 0.0152(19) -0.0028(15) 0.0053(16) 0.0015(16) 
C15 0.014(2) 0.0171(19) 0.015(2) -0.0045(16) 0.0004(16) 0.0026(16) 
C16 0.015(2) 0.027(2) 0.022(2) -0.0059(18) 0.0046(18) -0.0055(18) 
C17 0.024(2) 0.025(2) 0.018(2) -0.0045(18) 0.0089(18) -0.0060(18) 
C18 0.023(2) 0.016(2) 0.017(2) -0.0050(16) -0.0017(18) -0.0037(18) 
C19 0.019(2) 0.014(2) 0.016(2) -0.0022(16) 0.0001(17) -0.0008(17) 
C20 0.018(2) 0.015(2) 0.021(2) -0.0068(17) 0.0013(17) 0.0000(16) 
C21 0.022(2) 0.022(2) 0.025(2) -0.0062(18) -0.0067(19) 0.0012(19) 
C22 0.039(3) 0.023(2) 0.019(2) -0.0029(18) -0.012(2) 0.006(2) 
C23 0.039(3) 0.021(2) 0.017(2) 0.0027(18) 0.000(2) -0.001(2) 
C24 0.019(2) 0.023(2) 0.024(2) 0.0023(18) -0.0030(18) -0.0098(18) 
C25 0.029(2) 0.025(2) 0.025(2) 0.0030(19) 0.0004(19) -0.0082(19) 
C26 0.035(3) 0.024(2) 0.025(2) 0.0091(19) -0.002(2) -0.005(2) 
C27 0.018(2) 0.024(2) 0.025(2) -0.0013(19) -0.0008(18) 0.0018(18) 
C28 0.013(2) 0.017(2) 0.019(2) -0.0007(16) 0.0020(16) -0.0005(16) 
C29 0.021(2) 0.033(3) 0.018(2) -0.0040(19) 0.0032(17) 0.0028(19) 
C30 0.037(3) 0.034(3) 0.018(2) 0.002(2) 0.003(2) 0.004(2) 
C31 0.043(3) 0.028(3) 0.029(2) 0.0108(19) 0.000(2) 0.007(2) 
C32 0.026(2) 0.028(3) 0.034(3) 0.003(2) -0.001(2) 0.0118(19) 
C33 0.011(2) 0.026(2) 0.019(2) -0.0024(17) -0.0039(16) 0.0021(17) 
C34 0.0136(19) 0.017(2) 0.019(2) -0.0004(17) -0.0004(16) 0.0026(17) 
C35 0.019(2) 0.028(2) 0.022(2) -0.0029(19) -0.0045(18) 0.0046(17) 
C36 0.021(2) 0.048(3) 0.018(2) -0.014(2) 0.0053(18) -0.004(2) 
C37 0.018(2) 0.038(3) 0.035(3) -0.018(2) 0.006(2) -0.007(2) 
C38 0.014(2) 0.026(2) 0.035(2) -0.0127(19) 0.006(2) -0.0033(19) 
C39 0.027(3) 0.028(3) 0.036(3) 0.012(2) -0.013(2) -0.002(2) 
C40 0.029(2) 0.026(2) 0.039(3) 0.000(2) -0.017(2) 0.005(2) 
C41 0.020(2) 0.017(2) 0.026(2) -0.0015(18) -0.0067(18) 0.0005(18) 
C42 0.016(2) 0.026(2) 0.028(2) 0.0084(19) 0.0047(19) -0.0036(18) 
C43 0.013(2) 0.027(2) 0.033(3) 0.001(2) 0.0021(19) -0.0069(18) 
C44 0.0120(18) 0.021(2) 0.021(2) -0.0011(18) -0.0025(17) -0.0004(15) 
P1 0.0389(8) 0.0352(8) 0.0350(8) -0.0030(6) 0.0037(6) 0.0086(6) 
F1 0.089(3) 0.112(4) 0.107(3) 0.032(3) 0.010(3) 0.065(3) 
F2 0.118(4) 0.111(4) 0.062(3) 0.000(3) 0.004(3) -0.065(3) 
F3 0.095(3) 0.165(5) 0.071(3) 0.047(3) 0.040(3) 0.080(4) 
F4 0.258(7) 0.074(3) 0.052(2) -0.015(2) -0.005(3) -0.068(4) 
F5 0.132(4) 0.060(2) 0.063(3) 0.009(2) 0.048(3) 0.023(3) 
F6 0.060(2) 0.050(2) 0.057(2) -0.0084(17) 0.0152(17) -0.0115(17) 
C1S 0.063(5) 0.082(5) 0.074(5) 0.017(4) -0.031(4) -0.026(4) 
O1S 0.068(3) 0.059(3) 0.065(3) 0.002(2) 0.013(2) -0.005(2) 
C2S 0.125(8) 0.117(7) 0.081(5) 0.071(5) 0.067(5) 0.092(6) 
O2S 0.045(2) 0.061(3) 0.035(2) 0.0087(19) -0.0002(18) 0.012(2) 
 
_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. 
; 
 
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 C2 1.906(4) . ? 
Fe1 C3 1.922(4) . ? 
Fe1 C1 1.934(4) . ? 
Fe1 N10 1.951(3) . ? 
Fe1 N8 1.977(3) . ? 
Fe1 N9 1.990(3) . ? 
Ni1 N2 2.042(3) . ? 
Ni1 N6 2.064(3) . ? 
Ni1 N1 2.067(3) . ? 
Ni1 N7 2.087(3) . ? 
Ni1 N4 2.164(3) . ? 
Ni1 N5 2.170(3) . ? 
N1 C1 1.148(5) . ? 
N2 C2 1.152(5) 4 ? 
N3 C3 1.150(5) . ? 
N4 C5 1.433(5) . ? 
N4 C34 1.493(5) . ? 
N4 H1 0.9300 . ? 
N5 C15 1.452(5) . ? 
N5 C35 1.477(5) . ? 
N5 H2 0.9300 . ? 
N6 C28 1.345(5) . ? 
N6 C24 1.355(5) . ? 
N7 C29 1.340(5) . ? 
N7 C33 1.342(5) . ? 
N8 C38 1.340(6) . ? 
N8 N11 1.368(5) . ? 
N9 C41 1.344(5) . ? 
N9 N12 1.364(5) . ? 
N10 C44 1.339(5) . ? 
N10 N13 1.375(4) . ? 
N11 C36 1.360(6) . ? 
N11 B1 1.527(7) . ? 
N12 C39 1.353(6) . ? 
N12 B1 1.535(6) . ? 
N13 C42 1.341(5) . ? 
N13 B1 1.553(6) . ? 
B1 H3 1.0000 . ? 
C2 N2 1.152(5) 4_455 ? 
C4 C5 1.395(5) . ? 
C4 C9 1.440(6) . ? 
C4 C14 1.481(5) . ? 
C5 C6 1.417(5) . ? 
C6 C7 1.358(6) . ? 
C6 H4 0.9500 . ? 
C7 C8 1.426(6) . ? 
C7 H5 0.9500 . ? 
C8 C13 1.407(6) . ? 
C8 C9 1.408(6) . ? 
C9 C10 1.436(6) . ? 
C10 C11 1.355(6) . ? 
C10 H6 0.9500 . ? 
C11 C12 1.393(6) . ? 
C11 H7 0.9500 . ? 
C12 C13 1.364(7) . ? 
C12 H8 0.9500 . ? 
C13 H9 0.9500 . ? 
C14 C15 1.374(6) . ? 
C14 C19 1.443(6) . ? 
C15 C16 1.420(6) . ? 
C16 C17 1.337(6) . ? 
C16 H10 0.9500 . ? 
C17 C18 1.434(6) . ? 
C17 H11 0.9500 . ? 
C18 C23 1.404(6) . ? 
C18 C19 1.430(6) . ? 
C19 C20 1.401(6) . ? 
C20 C21 1.365(6) . ? 
C20 H12 0.9500 . ? 
C21 C22 1.415(7) . ? 
C21 H13 0.9500 . ? 
C22 C23 1.373(7) . ? 
C22 H14 0.9500 . ? 
C23 H15 0.9500 . ? 
C24 C25 1.373(6) . ? 
C24 H16 0.9500 . ? 
C25 C26 1.395(6) . ? 
C25 H17 0.9500 . ? 
C26 C27 1.381(6) . ? 
C26 H18 0.9500 . ? 
C27 C28 1.387(6) . ? 
C27 H19 0.9500 . ? 
C28 C34 1.503(5) . ? 
C29 C30 1.376(6) . ? 
C29 H20 0.9500 . ? 
C30 C31 1.387(6) . ? 
C30 H21 0.9500 . ? 
C31 C32 1.388(6) . ? 
C31 H22 0.9500 . ? 
C32 C33 1.400(6) . ? 
C32 H23 0.9500 . ? 
C33 C35 1.508(6) . ? 
C34 H24 0.9900 . ? 
C34 H25 0.9900 . ? 
C35 H26 0.9900 . ? 
C35 H27 0.9900 . ? 
C36 C37 1.379(7) . ? 
C36 H28 0.9500 . ? 
C37 C38 1.375(6) . ? 
C37 H29 0.9500 . ? 
C38 H30 0.9500 . ? 
C39 C40 1.377(7) . ? 
C39 H31 0.9500 . ? 
C40 C41 1.397(6) . ? 
C40 H32 0.9500 . ? 
C41 H33 0.9500 . ? 
C42 C43 1.389(6) . ? 
C42 H34 0.9500 . ? 
C43 C44 1.379(6) . ? 
C43 H35 0.9500 . ? 
C44 H36 0.9500 . ? 
P1 F4 1.546(4) . ? 
P1 F1 1.550(4) . ? 
P1 F2 1.579(4) . ? 
P1 F3 1.587(4) . ? 
P1 F5 1.590(4) . ? 
P1 F6 1.590(4) . ? 
C1S O1S 1.397(8) . ? 
C1S H37 0.9800 . ? 
C1S H38 0.9800 . ? 
C1S H39 0.9800 . ? 
O1S H40 0.8400 . ? 
C2S O2S 1.410(8) . ? 
C2S H41 0.9800 . ? 
C2S H42 0.9800 . ? 
C2S H43 0.9800 . ? 
O2S H44 0.8400 . ? 
 
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 
C2 Fe1 C3 85.83(17) . . ? 
C2 Fe1 C1 92.48(16) . . ? 
C3 Fe1 C1 91.06(16) . . ? 
C2 Fe1 N10 90.85(15) . . ? 
C3 Fe1 N10 90.42(15) . . ? 
C1 Fe1 N10 176.45(15) . . ? 
C2 Fe1 N8 178.51(16) . . ? 
C3 Fe1 N8 92.87(16) . . ? 
C1 Fe1 N8 88.27(15) . . ? 
N10 Fe1 N8 88.43(14) . . ? 
C2 Fe1 N9 91.00(15) . . ? 
C3 Fe1 N9 176.22(16) . . ? 
C1 Fe1 N9 91.14(15) . . ? 
N10 Fe1 N9 87.56(14) . . ? 
N8 Fe1 N9 90.27(15) . . ? 
N2 Ni1 N6 95.09(14) . . ? 
N2 Ni1 N1 90.11(13) . . ? 
N6 Ni1 N1 94.76(13) . . ? 
N2 Ni1 N7 94.70(13) . . ? 
N6 Ni1 N7 166.89(13) . . ? 
N1 Ni1 N7 93.90(13) . . ? 
N2 Ni1 N4 89.90(13) . . ? 
N6 Ni1 N4 80.86(13) . . ? 
N1 Ni1 N4 175.61(13) . . ? 
N7 Ni1 N4 90.47(13) . . ? 
N2 Ni1 N5 173.66(13) . . ? 
N6 Ni1 N5 90.55(13) . . ? 
N1 Ni1 N5 86.52(13) . . ? 
N7 Ni1 N5 80.18(13) . . ? 
N4 Ni1 N5 93.87(13) . . ? 
C1 N1 Ni1 164.9(3) . . ? 
C2 N2 Ni1 160.0(3) 4 . ? 
C5 N4 C34 116.5(3) . . ? 
C5 N4 Ni1 114.4(2) . . ? 
C34 N4 Ni1 109.8(2) . . ? 
C5 N4 H1 105.0 . . ? 
C34 N4 H1 105.0 . . ? 
Ni1 N4 H1 105.0 . . ? 
C15 N5 C35 117.5(3) . . ? 
C15 N5 Ni1 112.8(3) . . ? 
C35 N5 Ni1 111.4(2) . . ? 
C15 N5 H2 104.5 . . ? 
C35 N5 H2 104.5 . . ? 
Ni1 N5 H2 104.5 . . ? 
C28 N6 C24 117.4(4) . . ? 
C28 N6 Ni1 116.6(3) . . ? 
C24 N6 Ni1 125.3(3) . . ? 
C29 N7 C33 118.6(4) . . ? 
C29 N7 Ni1 124.9(3) . . ? 
C33 N7 Ni1 115.4(3) . . ? 
C38 N8 N11 106.8(3) . . ? 
C38 N8 Fe1 133.4(3) . . ? 
N11 N8 Fe1 119.8(3) . . ? 
C41 N9 N12 107.8(3) . . ? 
C41 N9 Fe1 132.8(3) . . ? 
N12 N9 Fe1 118.8(3) . . ? 
C44 N10 N13 106.9(3) . . ? 
C44 N10 Fe1 134.3(3) . . ? 
N13 N10 Fe1 118.8(2) . . ? 
C36 N11 N8 108.3(4) . . ? 
C36 N11 B1 133.4(4) . . ? 
N8 N11 B1 118.1(3) . . ? 
C39 N12 N9 108.3(4) . . ? 
C39 N12 B1 131.9(4) . . ? 
N9 N12 B1 119.0(3) . . ? 
C42 N13 N10 108.8(3) . . ? 
C42 N13 B1 132.0(4) . . ? 
N10 N13 B1 119.2(3) . . ? 
N11 B1 N12 108.5(4) . . ? 
N11 B1 N13 107.3(4) . . ? 
N12 B1 N13 105.2(3) . . ? 
N11 B1 H3 111.8 . . ? 
N12 B1 H3 111.8 . . ? 
N13 B1 H3 111.8 . . ? 
N1 C1 Fe1 171.6(4) . . ? 
N2 C2 Fe1 172.8(4) 4_455 . ? 
N3 C3 Fe1 177.1(4) . . ? 
C5 C4 C9 117.9(4) . . ? 
C5 C4 C14 121.7(3) . . ? 
C9 C4 C14 120.3(3) . . ? 
C4 C5 C6 120.8(4) . . ? 
C4 C5 N4 121.6(3) . . ? 
C6 C5 N4 117.4(3) . . ? 
C7 C6 C5 121.1(4) . . ? 
C7 C6 H4 119.4 . . ? 
C5 C6 H4 119.4 . . ? 
C6 C7 C8 120.4(4) . . ? 
C6 C7 H5 119.8 . . ? 
C8 C7 H5 119.8 . . ? 
C13 C8 C9 118.9(4) . . ? 
C13 C8 C7 122.1(4) . . ? 
C9 C8 C7 119.0(4) . . ? 
C8 C9 C10 118.5(4) . . ? 
C8 C9 C4 120.7(4) . . ? 
C10 C9 C4 120.7(4) . . ? 
C11 C10 C9 120.2(4) . . ? 
C11 C10 H6 119.9 . . ? 
C9 C10 H6 119.9 . . ? 
C10 C11 C12 121.0(4) . . ? 
C10 C11 H7 119.5 . . ? 
C12 C11 H7 119.5 . . ? 
C13 C12 C11 120.1(4) . . ? 
C13 C12 H8 120.0 . . ? 
C11 C12 H8 120.0 . . ? 
C12 C13 C8 121.2(4) . . ? 
C12 C13 H9 119.4 . . ? 
C8 C13 H9 119.4 . . ? 
C15 C14 C19 118.8(4) . . ? 
C15 C14 C4 121.4(4) . . ? 
C19 C14 C4 119.7(4) . . ? 
C14 C15 C16 120.9(4) . . ? 
C14 C15 N5 121.4(4) . . ? 
C16 C15 N5 117.4(4) . . ? 
C17 C16 C15 121.5(4) . . ? 
C17 C16 H10 119.3 . . ? 
C15 C16 H10 119.3 . . ? 
C16 C17 C18 120.8(4) . . ? 
C16 C17 H11 119.6 . . ? 
C18 C17 H11 119.6 . . ? 
C23 C18 C19 119.3(4) . . ? 
C23 C18 C17 122.3(4) . . ? 
C19 C18 C17 118.3(4) . . ? 
C20 C19 C18 118.3(4) . . ? 
C20 C19 C14 122.0(4) . . ? 
C18 C19 C14 119.6(4) . . ? 
C21 C20 C19 121.3(4) . . ? 
C21 C20 H12 119.3 . . ? 
C19 C20 H12 119.3 . . ? 
C20 C21 C22 120.7(4) . . ? 
C20 C21 H13 119.7 . . ? 
C22 C21 H13 119.7 . . ? 
C23 C22 C21 119.2(4) . . ? 
C23 C22 H14 120.4 . . ? 
C21 C22 H14 120.4 . . ? 
C22 C23 C18 121.2(4) . . ? 
C22 C23 H15 119.4 . . ? 
C18 C23 H15 119.4 . . ? 
N6 C24 C25 123.4(4) . . ? 
N6 C24 H16 118.3 . . ? 
C25 C24 H16 118.3 . . ? 
C24 C25 C26 118.7(4) . . ? 
C24 C25 H17 120.6 . . ? 
C26 C25 H17 120.6 . . ? 
C27 C26 C25 118.4(4) . . ? 
C27 C26 H18 120.8 . . ? 
C25 C26 H18 120.8 . . ? 
C26 C27 C28 119.6(4) . . ? 
C26 C27 H19 120.2 . . ? 
C28 C27 H19 120.2 . . ? 
N6 C28 C27 122.4(4) . . ? 
N6 C28 C34 116.8(3) . . ? 
C27 C28 C34 120.8(4) . . ? 
N7 C29 C30 122.7(4) . . ? 
N7 C29 H20 118.6 . . ? 
C30 C29 H20 118.6 . . ? 
C29 C30 C31 119.5(4) . . ? 
C29 C30 H21 120.2 . . ? 
C31 C30 H21 120.2 . . ? 
C30 C31 C32 118.2(4) . . ? 
C30 C31 H22 120.9 . . ? 
C32 C31 H22 120.9 . . ? 
C31 C32 C33 119.2(4) . . ? 
C31 C32 H23 120.4 . . ? 
C33 C32 H23 120.4 . . ? 
N7 C33 C32 121.8(4) . . ? 
N7 C33 C35 118.4(4) . . ? 
C32 C33 C35 119.7(4) . . ? 
N4 C34 C28 113.7(3) . . ? 
N4 C34 H24 108.8 . . ? 
C28 C34 H24 108.8 . . ? 
N4 C34 H25 108.8 . . ? 
C28 C34 H25 108.8 . . ? 
H24 C34 H25 107.7 . . ? 
N5 C35 C33 112.8(3) . . ? 
N5 C35 H26 109.0 . . ? 
C33 C35 H26 109.0 . . ? 
N5 C35 H27 109.0 . . ? 
C33 C35 H27 109.0 . . ? 
H26 C35 H27 107.8 . . ? 
N11 C36 C37 109.1(4) . . ? 
N11 C36 H28 125.5 . . ? 
C37 C36 H28 125.5 . . ? 
C38 C37 C36 104.8(4) . . ? 
C38 C37 H29 127.6 . . ? 
C36 C37 H29 127.6 . . ? 
N8 C38 C37 111.1(4) . . ? 
N8 C38 H30 124.5 . . ? 
C37 C38 H30 124.5 . . ? 
N12 C39 C40 109.4(4) . . ? 
N12 C39 H31 125.3 . . ? 
C40 C39 H31 125.3 . . ? 
C39 C40 C41 104.9(4) . . ? 
C39 C40 H32 127.5 . . ? 
C41 C40 H32 127.5 . . ? 
N9 C41 C40 109.6(4) . . ? 
N9 C41 H33 125.2 . . ? 
C40 C41 H33 125.2 . . ? 
N13 C42 C43 108.9(4) . . ? 
N13 C42 H34 125.6 . . ? 
C43 C42 H34 125.6 . . ? 
C44 C43 C42 105.0(4) . . ? 
C44 C43 H35 127.5 . . ? 
C42 C43 H35 127.5 . . ? 
N10 C44 C43 110.4(4) . . ? 
N10 C44 H36 124.8 . . ? 
C43 C44 H36 124.8 . . ? 
F4 P1 F1 94.1(3) . . ? 
F4 P1 F2 176.3(3) . . ? 
F1 P1 F2 89.6(3) . . ? 
F4 P1 F3 86.9(3) . . ? 
F1 P1 F3 178.0(2) . . ? 
F2 P1 F3 89.4(3) . . ? 
F4 P1 F5 88.4(3) . . ? 
F1 P1 F5 89.9(2) . . ? 
F2 P1 F5 91.7(2) . . ? 
F3 P1 F5 91.8(2) . . ? 
F4 P1 F6 91.6(2) . . ? 
F1 P1 F6 91.3(2) . . ? 
F2 P1 F6 88.2(2) . . ? 
F3 P1 F6 87.1(2) . . ? 
F5 P1 F6 178.9(2) . . ? 
O1S C1S H37 109.5 . . ? 
O1S C1S H38 109.5 . . ? 
H37 C1S H38 109.5 . . ? 
O1S C1S H39 109.5 . . ? 
H37 C1S H39 109.5 . . ? 
H38 C1S H39 109.5 . . ? 
C1S O1S H40 109.5 . . ? 
O2S C2S H41 109.5 . . ? 
O2S C2S H42 109.5 . . ? 
H41 C2S H42 109.5 . . ? 
O2S C2S H43 109.5 . . ? 
H41 C2S H43 109.5 . . ? 
H42 C2S H43 109.5 . . ? 
C2S O2S H44 109.5 . . ? 
 
_diffrn_measured_fraction_theta_max    1.000 
_diffrn_reflns_theta_full              27.00 
_diffrn_measured_fraction_theta_full   1.000 
_refine_diff_density_max    0.775 
_refine_diff_density_min   -0.514 
_refine_diff_density_rms    0.084