# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
2c.3THF  --  [Fe(k³-P,N,P-PNP-Et)(k²-P,N-PNP-Et)Cl].BPhMe₄.3THF
;
_chemical_name_common            
'[Fe(k3-P,N,P-PNP-Et)(k2-P,N-PNP-Et)Cl]BPhMe4.3THF'
_chemical_formula_moiety         
'C26 H50 Cl Fe N6 O0.16 P4, C28 H28 B, 3(C4 H8 O)'
_chemical_formula_sum            'C66 H102 B Cl Fe N6 O3.16 P4'
_chemical_formula_weight         1256.12

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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                   12.725(2)
_cell_length_b                   15.628(3)
_cell_length_c                   18.643(3)
_cell_angle_alpha                75.440(6)
_cell_angle_beta                 70.622(6)
_cell_angle_gamma                86.483(6)
_cell_volume                     3384.0(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9919
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      30.0

_exptl_crystal_description       rod
_exptl_crystal_colour            'clear green'
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1346.6
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_process_details   'program SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            155879
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         30.17
_reflns_number_total             19859
_reflns_number_gt                16152
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0507P)²+5.0136P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         19859
_refine_ls_number_parameters     772
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1236
_refine_ls_wR_factor_gt          0.1112
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_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 0.678905(19) 0.335817(15) 0.138402(13) 0.01074(6) Uani 1 1 d . . .
H1 H 0.408(2) 0.2000(17) 0.2258(15) 0.025(6) Uiso 1 1 d . . .
Cl1 Cl 0.67699(3) 0.47774(3) 0.05771(2) 0.01619(8) Uani 1 1 d . . .
P1 P 0.65496(4) 0.39431(3) 0.24067(2) 0.01285(8) Uani 1 1 d . . .
P2 P 0.75373(4) 0.28263(3) 0.03150(3) 0.01688(9) Uani 1 1 d . . .
N1 N 0.84347(12) 0.36581(10) 0.11731(8) 0.0147(3) Uani 1 1 d . . .
N2 N 0.78909(14) 0.41982(11) 0.22829(10) 0.0207(3) Uani 1 1 d . . .
N3 N 0.89169(14) 0.30914(13) 0.00851(10) 0.0254(4) Uani 1 1 d . . .
C1 C 0.87191(15) 0.41167(12) 0.16174(11) 0.0182(3) Uani 1 1 d . . .
C2 C 0.97979(16) 0.44524(13) 0.14284(13) 0.0259(4) Uani 1 1 d . . .
H2 H 0.9973 0.4761 0.1754 0.031 Uiso 1 1 calc R . .
C3 C 1.06012(16) 0.43238(14) 0.07562(13) 0.0288(5) Uani 1 1 d . . .
H3 H 1.1338 0.4549 0.0614 0.035 Uiso 1 1 calc R . .
C4 C 1.03390(16) 0.38707(14) 0.02924(12) 0.0273(4) Uani 1 1 d . . .
H4 H 1.0891 0.3777 -0.0168 0.033 Uiso 1 1 calc R . .
C5 C 0.92420(15) 0.35484(13) 0.05097(11) 0.0202(4) Uani 1 1 d . . .
H5 H 0.842(2) 0.2400(18) 0.1889(16) 0.027(6) Uiso 1 1 d . . .
C6 C 0.58178(16) 0.49823(11) 0.25137(11) 0.0184(3) Uani 1 1 d . . .
H6A H 0.5719 0.5281 0.2006 0.022 Uiso 1 1 calc R . .
H6B H 0.5065 0.4831 0.2903 0.022 Uiso 1 1 calc R . .
H6 H 0.808(2) 0.4467(18) 0.2576(16) 0.032(7) Uiso 1 1 d . . .
C7 C 0.63767(19) 0.56420(13) 0.27648(14) 0.0277(4) Uani 1 1 d . . .
H7A H 0.7121 0.5806 0.2383 0.042 Uiso 1 1 calc R . .
H7B H 0.6440 0.5371 0.3283 0.042 Uiso 1 1 calc R . .
H7C H 0.5926 0.6172 0.2790 0.042 Uiso 1 1 calc R . .
H7 H 0.942(3) 0.291(2) -0.0268(19) 0.045(8) Uiso 1 1 d . . .
C8 C 0.60722(16) 0.32079(12) 0.33881(10) 0.0188(3) Uani 1 1 d . . .
H8A H 0.5275 0.3058 0.3518 0.023 Uiso 1 1 calc R . .
H8B H 0.6487 0.2652 0.3377 0.023 Uiso 1 1 calc R . .
C9 C 0.61987(19) 0.35649(13) 0.40478(11) 0.0240(4) Uani 1 1 d . . .
H9A H 0.6975 0.3752 0.3915 0.036 Uiso 1 1 calc R . .
H9B H 0.5987 0.3100 0.4537 0.036 Uiso 1 1 calc R . .
H9C H 0.5714 0.4071 0.4115 0.036 Uiso 1 1 calc R . .
C10 C 0.72790(18) 0.32896(15) -0.06133(11) 0.0262(4) Uani 1 1 d . . .
H10A H 0.6524 0.3094 -0.0557 0.031 Uiso 1 1 calc R . .
H10B H 0.7278 0.3942 -0.0708 0.031 Uiso 1 1 calc R . .
C11 C 0.8101(2) 0.3048(2) -0.13299(13) 0.0458(7) Uani 1 1 d . . .
H11A H 0.7910 0.3350 -0.1797 0.069 Uiso 1 1 calc R . .
H11B H 0.8070 0.2407 -0.1265 0.069 Uiso 1 1 calc R . .
H11C H 0.8856 0.3230 -0.1391 0.069 Uiso 1 1 calc R . .
C12 C 0.7619(2) 0.16452(14) 0.03713(13) 0.0280(4) Uani 1 1 d . . .
H12A H 0.8246 0.1545 -0.0082 0.034 Uiso 1 1 calc R . .
H12B H 0.7786 0.1340 0.0854 0.034 Uiso 1 1 calc R . .
C13 C 0.6576(2) 0.12378(17) 0.03778(16) 0.0380(5) Uani 1 1 d . . .
H13A H 0.6418 0.1520 -0.0106 0.057 Uiso 1 1 calc R . .
H13B H 0.5952 0.1324 0.0830 0.057 Uiso 1 1 calc R . .
H13C H 0.6680 0.0604 0.0414 0.057 Uiso 1 1 calc R . .
P3 P 0.50198(3) 0.32472(3) 0.15359(2) 0.01173(8) Uani 1 1 d . . .
P4 P 0.94736(4) 0.13623(4) 0.23894(3) 0.02385(11) Uani 1 1 d . . .
N4 N 0.65428(12) 0.20518(9) 0.20976(8) 0.0121(2) Uani 1 1 d . . .
N5 N 0.46892(13) 0.22132(10) 0.21110(9) 0.0172(3) Uani 1 1 d . . .
N6 N 0.83600(13) 0.18714(10) 0.21379(10) 0.0200(3) Uani 1 1 d . . .
C14 C 0.54994(14) 0.16798(11) 0.23124(10) 0.0142(3) Uani 1 1 d . . .
C15 C 0.52223(16) 0.08004(12) 0.27159(11) 0.0196(3) Uani 1 1 d . . .
H15 H 0.4490 0.0573 0.2844 0.024 Uiso 1 1 calc R . .
C16 C 0.60271(16) 0.02670(12) 0.29252(11) 0.0215(4) Uani 1 1 d . . .
H16 H 0.5860 -0.0338 0.3191 0.026 Uiso 1 1 calc R . .
C17 C 0.70817(16) 0.06196(12) 0.27445(11) 0.0197(3) Uani 1 1 d . . .
H17 H 0.7640 0.0264 0.2898 0.024 Uiso 1 1 calc R . .
C18 C 0.73171(14) 0.15064(11) 0.23333(10) 0.0147(3) Uani 1 1 d . . .
C19 C 0.39440(14) 0.38968(11) 0.20850(10) 0.0159(3) Uani 1 1 d . . .
H19A H 0.3224 0.3566 0.2286 0.019 Uiso 1 1 calc R . .
H19B H 0.4136 0.3956 0.2544 0.019 Uiso 1 1 calc R . .
C20 C 0.37931(16) 0.48235(12) 0.16100(11) 0.0205(3) Uani 1 1 d . . .
H20A H 0.4504 0.5155 0.1399 0.031 Uiso 1 1 calc R . .
H20B H 0.3233 0.5134 0.1951 0.031 Uiso 1 1 calc R . .
H20C H 0.3546 0.4773 0.1177 0.031 Uiso 1 1 calc R . .
C21 C 0.45238(14) 0.32686(12) 0.07126(10) 0.0168(3) Uani 1 1 d . . .
H21A H 0.4693 0.3862 0.0348 0.020 Uiso 1 1 calc R . .
H21B H 0.4951 0.2837 0.0426 0.020 Uiso 1 1 calc R . .
C22 C 0.32754(16) 0.30600(14) 0.09336(12) 0.0223(4) Uani 1 1 d . . .
H22A H 0.3106 0.3036 0.0463 0.034 Uiso 1 1 calc R . .
H22B H 0.2839 0.3523 0.1161 0.034 Uiso 1 1 calc R . .
H22C H 0.3085 0.2488 0.1318 0.034 Uiso 1 1 calc R . .
C23 C 0.9896(2) 0.21969(16) 0.27819(17) 0.0367(5) Uani 1 1 d . . .
H23A H 1.0666 0.2084 0.2791 0.044 Uiso 1 1 calc R . .
H23B H 0.9894 0.2789 0.2432 0.044 Uiso 1 1 calc R . .
C24 C 0.9127(3) 0.2190(2) 0.3606(2) 0.0559(9) Uani 1 1 d . . .
H24A H 0.9424 0.2601 0.3815 0.084 Uiso 1 1 calc R . .
H24B H 0.9078 0.1592 0.3944 0.084 Uiso 1 1 calc R . .
H24C H 0.8383 0.2374 0.3589 0.084 Uiso 1 1 calc R . .
C25 C 1.05596(18) 0.15231(17) 0.14237(15) 0.0348(5) Uani 1 1 d . . .
H25A H 1.0530 0.2133 0.1112 0.042 Uiso 1 1 calc R . .
H25B H 1.1301 0.1448 0.1493 0.042 Uiso 1 1 calc R . .
C26 C 1.0412(2) 0.0866(2) 0.09785(17) 0.0481(7) Uani 1 1 d . . .
H26A H 0.9669 0.0926 0.0924 0.072 Uiso 1 1 calc R . .
H26B H 1.0492 0.0263 0.1269 0.072 Uiso 1 1 calc R . .
H26C H 1.0979 0.0989 0.0457 0.072 Uiso 1 1 calc R . .
C27 C 0.41206(14) 0.77520(11) 0.24421(10) 0.0143(3) Uani 1 1 d . . .
C28 C 0.45321(14) 0.72101(11) 0.19161(10) 0.0153(3) Uani 1 1 d . . .
H28 H 0.4371 0.6593 0.2102 0.018 Uiso 1 1 calc R . .
C29 C 0.51705(15) 0.75440(12) 0.11293(10) 0.0182(3) Uani 1 1 d . . .
H29 H 0.5442 0.7149 0.0800 0.022 Uiso 1 1 calc R . .
C30 C 0.54148(16) 0.84478(13) 0.08208(11) 0.0207(3) Uani 1 1 d . . .
C31 C 0.50105(17) 0.89977(13) 0.13325(12) 0.0244(4) Uani 1 1 d . . .
H31 H 0.5155 0.9617 0.1142 0.029 Uiso 1 1 calc R . .
C32 C 0.43995(16) 0.86550(12) 0.21160(11) 0.0209(4) Uani 1 1 d . . .
H32 H 0.4158 0.9051 0.2448 0.025 Uiso 1 1 calc R . .
C33 C 0.61059(19) 0.88232(15) -0.00270(12) 0.0291(4) Uani 1 1 d . . .
H33A H 0.5850 0.8560 -0.0366 0.044 Uiso 1 1 calc R . .
H33B H 0.6891 0.8687 -0.0100 0.044 Uiso 1 1 calc R . .
H33C H 0.6024 0.9466 -0.0164 0.044 Uiso 1 1 calc R . .
C34 C 0.39008(14) 0.78700(11) 0.38736(10) 0.0136(3) Uani 1 1 d . . .
C35 C 0.50415(14) 0.77510(11) 0.37828(10) 0.0155(3) Uani 1 1 d . . .
H35 H 0.5468 0.7433 0.3415 0.019 Uiso 1 1 calc R . .
C36 C 0.55707(14) 0.80767(11) 0.42062(11) 0.0170(3) Uani 1 1 d . . .
H36 H 0.6340 0.7972 0.4124 0.020 Uiso 1 1 calc R . .
C37 C 0.49880(15) 0.85568(11) 0.47515(11) 0.0175(3) Uani 1 1 d . . .
C38 C 0.38651(16) 0.87006(12) 0.48427(11) 0.0185(3) Uani 1 1 d . . .
H38 H 0.3447 0.9031 0.5202 0.022 Uiso 1 1 calc R . .
C39 C 0.33416(15) 0.83653(11) 0.44135(11) 0.0161(3) Uani 1 1 d . . .
H39 H 0.2575 0.8479 0.4492 0.019 Uiso 1 1 calc R . .
C40 C 0.55581(18) 0.88951(13) 0.52225(13) 0.0255(4) Uani 1 1 d . . .
H40A H 0.6170 0.9304 0.4866 0.038 Uiso 1 1 calc R . .
H40B H 0.5855 0.8396 0.5529 0.038 Uiso 1 1 calc R . .
H40C H 0.5020 0.9205 0.5577 0.038 Uiso 1 1 calc R . .
C41 C 0.20601(14) 0.77554(11) 0.34710(10) 0.0136(3) Uani 1 1 d . . .
C42 C 0.17047(15) 0.82842(12) 0.28690(10) 0.0174(3) Uani 1 1 d . . .
H42 H 0.2233 0.8463 0.2358 0.021 Uiso 1 1 calc R . .
C43 C 0.06060(16) 0.85580(13) 0.29912(12) 0.0210(4) Uani 1 1 d . . .
H43 H 0.0409 0.8916 0.2564 0.025 Uiso 1 1 calc R . .
C44 C -0.02028(15) 0.83162(12) 0.37260(12) 0.0200(3) Uani 1 1 d . . .
C45 C 0.01211(15) 0.77821(12) 0.43348(11) 0.0184(3) Uani 1 1 d . . .
H45 H -0.0412 0.7603 0.4844 0.022 Uiso 1 1 calc R . .
C46 C 0.12179(14) 0.75077(11) 0.42048(10) 0.0155(3) Uani 1 1 d . . .
H46 H 0.1405 0.7136 0.4631 0.019 Uiso 1 1 calc R . .
C47 C -0.13815(17) 0.86313(16) 0.38580(15) 0.0312(5) Uani 1 1 d . . .
H47A H -0.1670 0.8482 0.3477 0.047 Uiso 1 1 calc R . .
H47B H -0.1389 0.9274 0.3792 0.047 Uiso 1 1 calc R . .
H47C H -0.1851 0.8343 0.4391 0.047 Uiso 1 1 calc R . .
C48 C 0.32793(14) 0.63406(11) 0.36837(10) 0.0135(3) Uani 1 1 d . . .
C49 C 0.26810(15) 0.58279(11) 0.34192(10) 0.0166(3) Uani 1 1 d . . .
H49 H 0.2335 0.6122 0.3047 0.020 Uiso 1 1 calc R . .
C50 C 0.25727(15) 0.49084(12) 0.36779(11) 0.0179(3) Uani 1 1 d . . .
H50 H 0.2172 0.4595 0.3472 0.022 Uiso 1 1 calc R . .
C51 C 0.30436(15) 0.44452(11) 0.42325(11) 0.0186(3) Uani 1 1 d . . .
C52 C 0.36303(16) 0.49332(12) 0.45136(11) 0.0194(3) Uani 1 1 d . . .
H52 H 0.3956 0.4637 0.4897 0.023 Uiso 1 1 calc R . .
C53 C 0.37461(15) 0.58536(11) 0.42394(10) 0.0165(3) Uani 1 1 d . . .
H53 H 0.4161 0.6162 0.4439 0.020 Uiso 1 1 calc R . .
C54 C 0.29062(19) 0.34518(12) 0.45306(13) 0.0275(4) Uani 1 1 d . . .
H54A H 0.2831 0.3197 0.4120 0.041 Uiso 1 1 calc R . .
H54B H 0.2238 0.3304 0.4995 0.041 Uiso 1 1 calc R . .
H54C H 0.3561 0.3210 0.4670 0.041 Uiso 1 1 calc R . .
O1 O 0.24695(11) 0.13028(9) 0.29511(9) 0.0223(3) Uani 1 1 d . . .
C55 C 0.21633(18) 0.14852(13) 0.37159(12) 0.0246(4) Uani 1 1 d . . .
H55A H 0.1603 0.1954 0.3762 0.030 Uiso 1 1 calc R . .
H55B H 0.2825 0.1684 0.3803 0.030 Uiso 1 1 calc R . .
C56 C 0.1681(2) 0.06256(15) 0.43123(14) 0.0334(5) Uani 1 1 d . . .
H56A H 0.1079 0.0739 0.4773 0.040 Uiso 1 1 calc R . .
H56B H 0.2264 0.0278 0.4490 0.040 Uiso 1 1 calc R . .
C57 C 0.12275(17) 0.01527(13) 0.38485(12) 0.0243(4) Uani 1 1 d . . .
H57A H 0.1187 -0.0496 0.4064 0.029 Uiso 1 1 calc R . .
H57B H 0.0481 0.0364 0.3842 0.029 Uiso 1 1 calc R . .
C58 C 0.20914(17) 0.04132(13) 0.30393(13) 0.0248(4) Uani 1 1 d . . .
H58A H 0.2721 0.0002 0.2994 0.030 Uiso 1 1 calc R . .
H58B H 0.1759 0.0401 0.2631 0.030 Uiso 1 1 calc R . .
O2 O 0.92670(14) 0.77065(15) 0.09880(13) 0.0476(5) Uani 1 1 d . . .
C59 C 0.8118(2) 0.7498(2) 0.11846(17) 0.0446(6) Uani 1 1 d . . .
H59A H 0.7979 0.6851 0.1366 0.054 Uiso 1 1 calc R . .
H59B H 0.7861 0.7728 0.0727 0.054 Uiso 1 1 calc R . .
C60 C 0.7525(2) 0.7952(2) 0.18439(17) 0.0478(7) Uani 1 1 d . . .
H60A H 0.6735 0.8059 0.1886 0.057 Uiso 1 1 calc R . .
H60B H 0.7569 0.7603 0.2356 0.057 Uiso 1 1 calc R . .
C61 C 0.8184(3) 0.8789(2) 0.1569(2) 0.0624(9) Uani 1 1 d . . .
H61A H 0.8105 0.9067 0.2006 0.075 Uiso 1 1 calc R . .
H61B H 0.7965 0.9214 0.1153 0.075 Uiso 1 1 calc R . .
C62 C 0.9369(3) 0.8469(3) 0.1248(3) 0.0815(15) Uani 1 1 d . . .
H62A H 0.9831 0.8933 0.0807 0.098 Uiso 1 1 calc R . .
H62B H 0.9720 0.8318 0.1663 0.098 Uiso 1 1 calc R . .
O3 O 0.8794(2) 0.50071(16) 0.32138(15) 0.0683(7) Uani 1 1 d . . .
C63 C 0.9105(3) 0.4623(2) 0.3936(2) 0.0675(10) Uani 1 1 d . . .
H63A H 0.9704 0.4189 0.3840 0.081 Uiso 1 1 calc R . .
H63B H 0.8454 0.4335 0.4380 0.081 Uiso 1 1 calc R . .
C64 C 0.9508(2) 0.5435(3) 0.40859(18) 0.0637(11) Uani 1 1 d . . .
H64A H 0.8937 0.5624 0.4523 0.076 Uiso 1 1 calc R . .
H64B H 1.0206 0.5316 0.4214 0.076 Uiso 1 1 calc R . .
C65 C 0.9001(6) 0.5912(3) 0.3065(4) 0.127(3) Uani 1 1 d . . .
H65A H 0.9300 0.6161 0.2491 0.153 Uiso 1 1 calc R . .
H65B H 0.8290 0.6204 0.3268 0.153 Uiso 1 1 calc R . .
B1 B 0.33428(15) 0.74275(12) 0.33673(11) 0.0131(3) Uani 1 1 d . . .
C66 C 0.9688(7) 0.6081(4) 0.3378(3) 0.138(3) Uani 1 1 d . . .
H66A H 0.9563 0.6678 0.3478 0.165 Uiso 1 1 calc R . .
H66B H 1.0462 0.6060 0.3026 0.165 Uiso 1 1 calc R . .
O4 O 0.9373(9) 0.0577(7) 0.2781(6) 0.035(3) Uiso 0.162(7) 1 d P . .


_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 N1 2.0593(15) . ?
Fe1 N4 2.1148(14) . ?
Fe1 P3 2.1861(6) . ?
Fe1 P1 2.2405(6) . ?
Fe1 P2 2.2463(6) . ?
Fe1 Cl1 2.3500(6) . ?
P1 N2 1.7033(17) . ?
P1 C8 1.8243(18) . ?
P1 C6 1.8436(18) . ?
P2 N3 1.7140(19) . ?
P2 C12 1.821(2) . ?
P2 C10 1.8290(19) . ?
N1 C5 1.362(2) . ?
N1 C1 1.364(2) . ?
N2 C1 1.364(2) . ?
N2 H6 0.87(3) . ?
N3 C5 1.359(3) . ?
N3 H7 0.85(3) . ?
C1 C2 1.399(3) . ?
C2 C3 1.381(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.374(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.405(3) . ?
C4 H4 0.9500 . ?
C6 C7 1.530(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.529(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.517(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.502(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
P3 N5 1.6884(16) . ?
P3 C21 1.8356(18) . ?
P3 C19 1.8369(17) . ?
P4 O4 1.250(11) . ?
P4 N6 1.7251(16) . ?
P4 C23 1.831(2) . ?
P4 C25 1.838(2) . ?
N4 C14 1.373(2) . ?
N4 C18 1.373(2) . ?
N5 C14 1.376(2) . ?
N5 H1 0.80(3) . ?
N6 C18 1.374(2) . ?
N6 H5 0.83(3) . ?
C14 C15 1.394(2) . ?
C15 C16 1.376(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.384(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.401(2) . ?
C17 H17 0.9500 . ?
C19 C20 1.534(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.537(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.521(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.527(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C32 1.405(2) . ?
C27 C28 1.405(2) . ?
C27 B1 1.643(3) . ?
C28 C29 1.400(2) . ?
C28 H28 0.9500 . ?
C29 C30 1.396(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.395(3) . ?
C30 C33 1.513(3) . ?
C31 C32 1.389(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C39 1.403(2) . ?
C34 C35 1.411(2) . ?
C34 B1 1.645(2) . ?
C35 C36 1.390(2) . ?
C35 H35 0.9500 . ?
C36 C37 1.401(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.393(3) . ?
C37 C40 1.510(3) . ?
C38 C39 1.402(2) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.404(2) . ?
C41 C46 1.408(2) . ?
C41 B1 1.644(3) . ?
C42 C43 1.398(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.389(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.395(3) . ?
C44 C47 1.509(3) . ?
C45 C46 1.395(2) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C53 1.401(2) . ?
C48 C49 1.410(2) . ?
C48 B1 1.649(2) . ?
C49 C50 1.396(2) . ?
C49 H49 0.9500 . ?
C50 C51 1.391(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.394(3) . ?
C51 C54 1.511(3) . ?
C52 C53 1.399(2) . ?
C52 H52 0.9500 . ?
C53 H53 0.9500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
O1 C55 1.445(3) . ?
O1 C58 1.451(2) . ?
C55 C56 1.521(3) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.527(3) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.515(3) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
O2 C59 1.422(3) . ?
O2 C62 1.422(4) . ?
C59 C60 1.530(4) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 C61 1.480(5) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 C62 1.530(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
O3 C65 1.395(5) . ?
O3 C63 1.498(4) . ?
C63 C64 1.517(5) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 C66 1.404(6) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C66 1.272(6) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N4 104.41(6) . . ?
N1 Fe1 P3 171.56(4) . . ?
N4 Fe1 P3 83.86(4) . . ?
N1 Fe1 P1 81.92(4) . . ?
N4 Fe1 P1 92.66(4) . . ?
P3 Fe1 P1 96.173(19) . . ?
N1 Fe1 P2 81.96(5) . . ?
N4 Fe1 P2 89.80(4) . . ?
P3 Fe1 P2 100.01(2) . . ?
P1 Fe1 P2 163.81(2) . . ?
N1 Fe1 Cl1 84.95(4) . . ?
N4 Fe1 Cl1 170.50(4) . . ?
P3 Fe1 Cl1 86.838(18) . . ?
P1 Fe1 Cl1 90.24(2) . . ?
P2 Fe1 Cl1 89.93(2) . . ?
N2 P1 C8 103.39(9) . . ?
N2 P1 C6 103.46(9) . . ?
C8 P1 C6 104.57(9) . . ?
N2 P1 Fe1 101.09(6) . . ?
C8 P1 Fe1 117.88(6) . . ?
C6 P1 Fe1 123.52(6) . . ?
N3 P2 C12 100.46(10) . . ?
N3 P2 C10 102.62(10) . . ?
C12 P2 C10 103.19(10) . . ?
N3 P2 Fe1 100.50(6) . . ?
C12 P2 Fe1 122.18(7) . . ?
C10 P2 Fe1 123.41(7) . . ?
C5 N1 C1 117.53(16) . . ?
C5 N1 Fe1 120.94(13) . . ?
C1 N1 Fe1 120.51(12) . . ?
C1 N2 P1 119.56(13) . . ?
C1 N2 H6 115.6(18) . . ?
P1 N2 H6 124.0(18) . . ?
C5 N3 P2 120.39(13) . . ?
C5 N3 H7 118(2) . . ?
P2 N3 H7 121(2) . . ?
N1 C1 N2 115.58(15) . . ?
N1 C1 C2 122.80(18) . . ?
N2 C1 C2 121.57(18) . . ?
C3 C2 C1 118.3(2) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C4 C3 C2 120.27(18) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 118.99(19) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N3 C5 N1 115.33(17) . . ?
N3 C5 C4 122.62(18) . . ?
N1 C5 C4 122.04(19) . . ?
C7 C6 P1 116.59(14) . . ?
C7 C6 H6A 108.1 . . ?
P1 C6 H6A 108.1 . . ?
C7 C6 H6B 108.1 . . ?
P1 C6 H6B 108.1 . . ?
H6A C6 H6B 107.3 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 P1 116.18(13) . . ?
C9 C8 H8A 108.2 . . ?
P1 C8 H8A 108.2 . . ?
C9 C8 H8B 108.2 . . ?
P1 C8 H8B 108.2 . . ?
H8A C8 H8B 107.4 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 P2 115.96(15) . . ?
C11 C10 H10A 108.3 . . ?
P2 C10 H10A 108.3 . . ?
C11 C10 H10B 108.3 . . ?
P2 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 P2 114.09(16) . . ?
C13 C12 H12A 108.7 . . ?
P2 C12 H12A 108.7 . . ?
C13 C12 H12B 108.7 . . ?
P2 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N5 P3 C21 104.01(8) . . ?
N5 P3 C19 101.71(8) . . ?
C21 P3 C19 100.52(8) . . ?
N5 P3 Fe1 101.82(6) . . ?
C21 P3 Fe1 122.21(6) . . ?
C19 P3 Fe1 123.29(6) . . ?
O4 P4 N6 119.8(5) . . ?
O4 P4 C23 118.0(5) . . ?
N6 P4 C23 100.77(9) . . ?
O4 P4 C25 112.9(5) . . ?
N6 P4 C25 101.40(9) . . ?
C23 P4 C25 101.26(13) . . ?
C14 N4 C18 115.61(14) . . ?
C14 N4 Fe1 116.27(11) . . ?
C18 N4 Fe1 127.98(11) . . ?
C14 N5 P3 120.31(12) . . ?
C14 N5 H1 116.9(19) . . ?
P3 N5 H1 122.7(19) . . ?
C18 N6 P4 126.69(13) . . ?
C18 N6 H5 113.5(18) . . ?
P4 N6 H5 119.8(18) . . ?
N4 C14 N5 117.42(15) . . ?
N4 C14 C15 123.85(16) . . ?
N5 C14 C15 118.73(16) . . ?
C16 C15 C14 118.92(17) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C17 119.35(17) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C16 C17 C18 119.33(16) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
N4 C18 N6 116.50(15) . . ?
N4 C18 C17 122.87(16) . . ?
N6 C18 C17 120.62(16) . . ?
C20 C19 P3 114.69(12) . . ?
C20 C19 H19A 108.6 . . ?
P3 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
P3 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 P3 115.64(13) . . ?
C22 C21 H21A 108.4 . . ?
P3 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
P3 C21 H21B 108.4 . . ?
H21A C21 H21B 107.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 P4 112.0(2) . . ?
C24 C23 H23A 109.2 . . ?
P4 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
P4 C23 H23B 109.2 . . ?
H23A C23 H23B 107.9 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 P4 111.53(18) . . ?
C26 C25 H25A 109.3 . . ?
P4 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
P4 C25 H25B 109.3 . . ?
H25A C25 H25B 108.0 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C32 C27 C28 114.73(16) . . ?
C32 C27 B1 119.02(15) . . ?
C28 C27 B1 126.24(15) . . ?
C29 C28 C27 122.62(16) . . ?
C29 C28 H28 118.7 . . ?
C27 C28 H28 118.7 . . ?
C30 C29 C28 121.14(17) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C31 C30 C29 117.13(17) . . ?
C31 C30 C33 120.80(18) . . ?
C29 C30 C33 122.06(18) . . ?
C32 C31 C30 121.11(17) . . ?
C32 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
C31 C32 C27 123.24(17) . . ?
C31 C32 H32 118.4 . . ?
C27 C32 H32 118.4 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C39 C34 C35 114.66(15) . . ?
C39 C34 B1 126.01(15) . . ?
C35 C34 B1 119.32(15) . . ?
C36 C35 C34 123.09(16) . . ?
C36 C35 H35 118.5 . . ?
C34 C35 H35 118.5 . . ?
C35 C36 C37 121.07(16) . . ?
C35 C36 H36 119.5 . . ?
C37 C36 H36 119.5 . . ?
C38 C37 C36 117.17(16) . . ?
C38 C37 C40 121.79(17) . . ?
C36 C37 C40 121.04(17) . . ?
C37 C38 C39 121.11(16) . . ?
C37 C38 H38 119.4 . . ?
C39 C38 H38 119.4 . . ?
C38 C39 C34 122.88(16) . . ?
C38 C39 H39 118.6 . . ?
C34 C39 H39 118.6 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C46 114.73(15) . . ?
C42 C41 B1 124.94(15) . . ?
C46 C41 B1 120.32(15) . . ?
C43 C42 C41 122.71(17) . . ?
C43 C42 H42 118.6 . . ?
C41 C42 H42 118.6 . . ?
C44 C43 C42 121.23(17) . . ?
C44 C43 H43 119.4 . . ?
C42 C43 H43 119.4 . . ?
C43 C44 C45 117.45(17) . . ?
C43 C44 C47 120.96(18) . . ?
C45 C44 C47 121.59(18) . . ?
C46 C45 C44 120.82(17) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C45 C46 C41 123.04(16) . . ?
C45 C46 H46 118.5 . . ?
C41 C46 H46 118.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C53 C48 C49 114.53(15) . . ?
C53 C48 B1 125.18(15) . . ?
C49 C48 B1 120.23(15) . . ?
C50 C49 C48 123.08(16) . . ?
C50 C49 H49 118.5 . . ?
C48 C49 H49 118.5 . . ?
C51 C50 C49 120.91(17) . . ?
C51 C50 H50 119.5 . . ?
C49 C50 H50 119.5 . . ?
C50 C51 C52 117.50(16) . . ?
C50 C51 C54 121.25(18) . . ?
C52 C51 C54 121.24(18) . . ?
C51 C52 C53 120.90(17) . . ?
C51 C52 H52 119.5 . . ?
C53 C52 H52 119.5 . . ?
C52 C53 C48 123.06(17) . . ?
C52 C53 H53 118.5 . . ?
C48 C53 H53 118.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C55 O1 C58 109.07(15) . . ?
O1 C55 C56 106.57(16) . . ?
O1 C55 H55A 110.4 . . ?
C56 C55 H55A 110.4 . . ?
O1 C55 H55B 110.4 . . ?
C56 C55 H55B 110.4 . . ?
H55A C55 H55B 108.6 . . ?
C55 C56 C57 102.67(17) . . ?
C55 C56 H56A 111.2 . . ?
C57 C56 H56A 111.2 . . ?
C55 C56 H56B 111.2 . . ?
C57 C56 H56B 111.2 . . ?
H56A C56 H56B 109.1 . . ?
C58 C57 C56 101.73(17) . . ?
C58 C57 H57A 111.4 . . ?
C56 C57 H57A 111.4 . . ?
C58 C57 H57B 111.4 . . ?
C56 C57 H57B 111.4 . . ?
H57A C57 H57B 109.3 . . ?
O1 C58 C57 105.94(16) . . ?
O1 C58 H58A 110.5 . . ?
C57 C58 H58A 110.5 . . ?
O1 C58 H58B 110.5 . . ?
C57 C58 H58B 110.5 . . ?
H58A C58 H58B 108.7 . . ?
C59 O2 C62 109.0(2) . . ?
O2 C59 C60 104.7(2) . . ?
O2 C59 H59A 110.8 . . ?
C60 C59 H59A 110.8 . . ?
O2 C59 H59B 110.8 . . ?
C60 C59 H59B 110.8 . . ?
H59A C59 H59B 108.9 . . ?
C61 C60 C59 100.8(2) . . ?
C61 C60 H60A 111.6 . . ?
C59 C60 H60A 111.6 . . ?
C61 C60 H60B 111.6 . . ?
C59 C60 H60B 111.6 . . ?
H60A C60 H60B 109.4 . . ?
C60 C61 C62 101.6(3) . . ?
C60 C61 H61A 111.4 . . ?
C62 C61 H61A 111.4 . . ?
C60 C61 H61B 111.4 . . ?
C62 C61 H61B 111.4 . . ?
H61A C61 H61B 109.3 . . ?
O2 C62 C61 106.2(3) . . ?
O2 C62 H62A 110.5 . . ?
C61 C62 H62A 110.5 . . ?
O2 C62 H62B 110.5 . . ?
C61 C62 H62B 110.5 . . ?
H62A C62 H62B 108.7 . . ?
C65 O3 C63 103.6(3) . . ?
O3 C63 C64 102.3(3) . . ?
O3 C63 H63A 111.3 . . ?
C64 C63 H63A 111.3 . . ?
O3 C63 H63B 111.3 . . ?
C64 C63 H63B 111.3 . . ?
H63A C63 H63B 109.2 . . ?
C66 C64 C63 104.2(3) . . ?
C66 C64 H64A 110.9 . . ?
C63 C64 H64A 110.9 . . ?
C66 C64 H64B 110.9 . . ?
C63 C64 H64B 110.9 . . ?
H64A C64 H64B 108.9 . . ?
C66 C65 O3 112.5(4) . . ?
C66 C65 H65A 109.1 . . ?
O3 C65 H65A 109.1 . . ?
C66 C65 H65B 109.1 . . ?
O3 C65 H65B 109.1 . . ?
H65A C65 H65B 107.8 . . ?
C27 B1 C41 109.66(13) . . ?
C27 B1 C34 106.91(13) . . ?
C41 B1 C34 111.23(13) . . ?
C27 B1 C48 111.94(13) . . ?
C41 B1 C48 106.90(13) . . ?
C34 B1 C48 110.25(13) . . ?
C65 C66 C64 107.0(5) . . ?
C65 C66 H66A 110.3 . . ?
C64 C66 H66A 110.3 . . ?
C65 C66 H66B 110.3 . . ?
C64 C66 H66B 110.3 . . ?
H66A C66 H66B 108.6 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        30.17
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.561
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.077

# start Validation Reply Form
_vrf_PLAT360_2c                  
;
PROBLEM: Short  C(sp3)-C(sp3) Bond  C65    -   C66    ...       1.27 Ang.  
RESPONSE: C65 and C66 are part of a disordered THF molecule and feature
strongly enlarged APDs. Thus the C-C distance appears much smaller than
it is. Refinement of C65 and C66 as two positions did not lead to a
satisfactory model.
;
_database_code_depnum_ccdc_archive 'CCDC 1005380'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2d

# 5. CHEMICAL DATA

_chemical_name_systematic        
; 
2d.3THF  --  [Fe(k³-P,N,P-PNP-Et)(k²-P,N-PNP-Et)Br]BPhMe₄.3THF
;
_chemical_name_common            
'[Fe(k3-P,N,P-PNP-Et)(k2-P,N-PNP-Et)Br]BPhMe4.3THF'
_chemical_formula_moiety         'C26 H50 Br Fe N6 P4, C28 H28 B, 3(C4 H8 O) '
_chemical_formula_sum            'C66 H102 B1 Br1 Fe1 N6 O3 P4'
_chemical_formula_weight         1298

#==============================================================================0

# 6. CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   12.778(5)
_cell_length_b                   15.546(6)
_cell_length_c                   18.790(7)
_cell_angle_alpha                75.954(7)
_cell_angle_beta                 70.741(7)
_cell_angle_gamma                86.697(8)
_cell_volume                     3417(2)

_cell_formula_units_Z            2

_cell_measurement_reflns_used    9410
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      28.3
_cell_measurement_temperature    100
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.2611
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1380

_exptl_absorpt_coefficient_mu    0.947
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            green
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_T_max  0.95

#==============================================================================0

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      100
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'ω scans'

_diffrn_reflns_number            27496
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_max 0.97
_diffrn_measured_fraction_theta_full 0.98
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24

_diffrn_radiation_probe          X-ray

#==============================================================================0

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             16613
_reflns_number_gt                12623
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0436
_refine_ls_wR_factor_gt          0.1036
_refine_ls_R_factor_all          0.0599
_refine_ls_wR_factor_ref         0.1110
_refine_ls_goodness_of_fit_ref   1.42
_refine_ls_goodness_of_fit_gt    1.53
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         16613
_refine_ls_number_parameters     755
_refine_ls_number_restraints     0
_refine_ls_number_constraints    392
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0016I²)
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          0.0302
_refine_ls_shift/su_mean         0.0012
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     none

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
B 0.0013 0.0007 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Br -0.2901 2.4595 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
P 0.1023 0.0942 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'Jana2006 [Petricek et al., 2006]'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


#==============================================================================0

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.673650(19) 0.987428(14) 0.058625(12) Uani 0.02073(8) 2 1 d . . .
Fe1 Fe 0.67658(3) 0.836013(19) 0.140799(16) Uani 0.01377(10) 2 1 d . . .
P1 P 0.64994(5) 0.89282(4) 0.24421(3) Uani 0.01514(19) 2 1 d . . .
P2 P 0.75329(5) 0.78425(4) 0.03341(3) Uani 0.0184(2) 2 1 d . . .
N1 N 0.83991(15) 0.86730(12) 0.12158(10) Uani 0.0175(6) 2 1 d . . .
N2 N 0.78272(16) 0.91911(13) 0.23348(11) Uani 0.0207(7) 2 1 d . . .
N3 N 0.88930(18) 0.81330(14) 0.01111(12) Uani 0.0252(8) 2 1 d . . .
C1 C 0.86649(19) 0.91206(14) 0.16780(13) Uani 0.0196(8) 2 1 d . . .
C2 C 0.9726(2) 0.94626(16) 0.15047(14) Uani 0.0258(9) 2 1 d . . .
C3 C 1.0535(2) 0.93459(17) 0.08397(15) Uani 0.0289(9) 2 1 d . . .
C4 C 1.0293(2) 0.89015(16) 0.03536(14) Uani 0.0263(9) 2 1 d . . .
C5 C 0.9210(2) 0.85806(15) 0.05534(13) Uani 0.0217(8) 2 1 d . . .
C6 C 0.5743(2) 0.99529(14) 0.25772(13) Uani 0.0204(8) 2 1 d . . .
C7 C 0.6318(2) 1.06408(16) 0.27856(15) Uani 0.0273(9) 2 1 d . . .
C8 C 0.6034(2) 0.81858(15) 0.34058(12) Uani 0.0203(8) 2 1 d . . .
C9 C 0.6146(2) 0.85436(15) 0.40663(13) Uani 0.0237(9) 2 1 d . . .
C10 C 0.7264(2) 0.82815(16) -0.05878(13) Uani 0.0264(9) 2 1 d . . .
C11 C 0.8087(2) 0.8047(2) -0.13015(14) Uani 0.0387(11) 2 1 d . . .
C12 C 0.7645(2) 0.66542(15) 0.03852(13) Uani 0.0257(9) 2 1 d . . .
C13 C 0.6614(2) 0.62228(18) 0.03992(16) Uani 0.0359(11) 2 1 d . . .
P3 P 0.50044(5) 0.82424(4) 0.15517(3) Uani 0.01518(19) 2 1 d . . .
P4 P 0.94861(6) 0.63509(5) 0.23734(4) Uani 0.0299(3) 2 1 d . . .
N4 N 0.65391(16) 0.70459(12) 0.21015(10) Uani 0.0161(6) 2 1 d . . .
N5 N 0.46972(18) 0.72087(13) 0.21219(12) Uani 0.0209(7) 2 1 d . . .
N6 N 0.83705(17) 0.68628(14) 0.21215(12) Uani 0.0242(8) 2 1 d . . .
C14 C 0.55048(19) 0.66774(14) 0.23188(12) Uani 0.0171(7) 2 1 d . . .
C15 C 0.5236(2) 0.57986(15) 0.27234(13) Uani 0.0226(8) 2 1 d . . .
C16 C 0.6057(2) 0.52697(15) 0.29190(13) Uani 0.0253(9) 2 1 d . . .
C17 C 0.7094(2) 0.56201(15) 0.27331(13) Uani 0.0238(9) 2 1 d . . .
C18 C 0.73320(19) 0.65067(14) 0.23241(12) Uani 0.0173(8) 2 1 d . . .
C19 C 0.39117(19) 0.88788(14) 0.20991(13) Uani 0.0190(8) 2 1 d . . .
C20 C 0.3710(2) 0.97956(15) 0.16412(14) Uani 0.0241(9) 2 1 d . . .
C21 C 0.45130(19) 0.82397(15) 0.07351(13) Uani 0.0202(8) 2 1 d . . .
C22 C 0.3276(2) 0.80126(16) 0.09503(14) Uani 0.0253(9) 2 1 d . . .
C23 C 0.9906(3) 0.71874(19) 0.2770(2) Uani 0.0475(14) 2 1 d . . .
C24 C 0.9123(3) 0.7196(3) 0.3583(2) Uani 0.0683(19) 2 1 d . . .
C25 C 1.0564(2) 0.6517(2) 0.14186(17) Uani 0.0439(12) 2 1 d . . .
C26 C 1.0439(3) 0.5856(3) 0.09677(19) Uani 0.0580(15) 2 1 d . . .
C27 C 0.39005(18) 0.28753(13) 0.38739(12) Uani 0.0158(7) 2 1 d . . .
C28 C 0.50357(19) 0.27649(14) 0.37762(12) Uani 0.0178(8) 2 1 d . . .
C29 C 0.55669(19) 0.30918(14) 0.41970(13) Uani 0.0192(8) 2 1 d . . .
C30 C 0.4988(2) 0.35657(14) 0.47455(13) Uani 0.0196(8) 2 1 d . . .
C31 C 0.3872(2) 0.37033(14) 0.48428(13) Uani 0.0207(8) 2 1 d . . .
C32 C 0.33420(19) 0.33674(14) 0.44169(13) Uani 0.0188(8) 2 1 d . . .
C33 C 0.5570(2) 0.39075(16) 0.52148(15) Uani 0.0282(10) 2 1 d . . .
C34 C 0.32766(18) 0.13385(14) 0.36871(12) Uani 0.0164(7) 2 1 d . . .
C35 C 0.37309(19) 0.08612(14) 0.42485(12) Uani 0.0179(8) 2 1 d . . .
C36 C 0.3603(2) -0.00535(15) 0.45340(13) Uani 0.0221(8) 2 1 d . . .
C37 C 0.30265(19) -0.05516(14) 0.42557(13) Uani 0.0203(8) 2 1 d . . .
C38 C 0.25716(19) -0.01006(14) 0.36940(13) Uani 0.0204(8) 2 1 d . . .
C39 C 0.26888(19) 0.08165(14) 0.34201(13) Uani 0.0192(8) 2 1 d . . .
C40 C 0.2882(2) -0.15471(15) 0.45627(15) Uani 0.0307(10) 2 1 d . . .
C41 C 0.20567(19) 0.27582(13) 0.34679(12) Uani 0.0157(7) 2 1 d . . .
C42 C 0.12175(19) 0.25141(14) 0.41931(13) Uani 0.0179(8) 2 1 d . . .
C43 C 0.0126(2) 0.27899(15) 0.43183(14) Uani 0.0213(8) 2 1 d . . .
C44 C -0.0200(2) 0.33225(15) 0.37146(14) Uani 0.0222(8) 2 1 d . . .
C45 C 0.0608(2) 0.35543(15) 0.29883(14) Uani 0.0226(8) 2 1 d . . .
C46 C 0.1699(2) 0.32799(14) 0.28732(13) Uani 0.0196(8) 2 1 d . . .
C47 C -0.1375(2) 0.36405(19) 0.38402(16) Uani 0.0348(11) 2 1 d . . .
C48 C 0.41042(18) 0.27487(14) 0.24515(12) Uani 0.0166(7) 2 1 d . . .
C49 C 0.44997(18) 0.22120(14) 0.19189(12) Uani 0.0172(8) 2 1 d . . .
C50 C 0.51274(19) 0.25443(15) 0.11413(13) Uani 0.0204(8) 2 1 d . . .
C51 C 0.53719(19) 0.34477(15) 0.08459(13) Uani 0.0213(8) 2 1 d . . .
C52 C 0.4985(2) 0.39959(15) 0.13604(13) Uani 0.0240(8) 2 1 d . . .
C53 C 0.4390(2) 0.36525(15) 0.21353(13) Uani 0.0223(8) 2 1 d . . .
C54 C 0.6054(2) 0.38277(17) 0.00073(14) Uani 0.0300(9) 2 1 d . . .
B1 B 0.3338(2) 0.24266(16) 0.33680(14) Uani 0.0151(8) 2 1 d . . .
O1 O 0.24822(15) 0.63047(11) 0.29614(10) Uani 0.0286(7) 2 1 d . . .
C55 C 0.2100(2) 0.54185(16) 0.30400(16) Uani 0.0320(10) 2 1 d . . .
C56 C 0.1239(2) 0.51640(17) 0.38417(15) Uani 0.0299(10) 2 1 d . . .
C57 C 0.1686(3) 0.56351(18) 0.43031(17) Uani 0.0396(12) 2 1 d . . .
C58 C 0.2168(2) 0.64931(17) 0.37181(15) Uani 0.0313(10) 2 1 d . . .
O2 O 0.92754(16) 0.26531(15) 0.09678(13) Uani 0.0456(9) 2 1 d . . .
C59 C 0.8128(2) 0.2444(2) 0.11575(17) Uani 0.0413(12) 2 1 d . . .
C60 C 0.7522(3) 0.2902(2) 0.18099(18) Uani 0.0449(12) 2 1 d . . .
C61 C 0.8186(3) 0.3740(2) 0.1559(2) Uani 0.0584(16) 2 1 d . . .
C62 C 0.9360(3) 0.3410(3) 0.1255(2) Uani 0.073(2) 2 1 d . . .
O3 O 0.8654(2) 0.00209(14) 0.32874(12) Uani 0.0516(10) 2 1 d . . .
C63 C 0.8920(3) 0.0945(2) 0.3067(2) Uani 0.0613(17) 2 1 d . . .
C64 C 0.9854(4) 0.1039(3) 0.3312(2) Uani 0.069(2) 2 1 d . . .
C65 C 0.9572(2) 0.0404(2) 0.40773(17) Uani 0.0466(13) 2 1 d . . .
C66 C 0.9060(3) -0.0365(2) 0.39335(19) Uani 0.0508(14) 2 1 d . . .
H1n3 H 0.940(3) 0.798(2) -0.0234(18) Uiso 0.040(9) 2 1 d . . .
H1n5 H 0.415(2) 0.6975(16) 0.2252(14) Uiso 0.013(7) 2 1 d . . .
H1n6 H 0.841(3) 0.740(2) 0.1868(18) Uiso 0.045(9) 2 1 d . . .
H1n2 H 0.801(2) 0.9448(18) 0.2646(16) Uiso 0.031(7) 2 1 d . . .
H1c2 H 0.989042 0.977261 0.184051 Uiso 0.031 2 1 d . . .
H1c3 H 1.127304 0.957465 0.071166 Uiso 0.0347 2 1 d . . .
H1c4 H 1.085639 0.881649 -0.010852 Uiso 0.0316 2 1 d . . .
H1c6 H 0.554969 1.02223 0.212183 Uiso 0.0245 2 1 d . . .
H2c6 H 0.502357 0.980464 0.295933 Uiso 0.0245 2 1 d . . .
H1c7 H 0.587879 1.116212 0.280328 Uiso 0.0327 2 1 d . . .
H2c7 H 0.64042 1.040045 0.328387 Uiso 0.0327 2 1 d . . .
H3c7 H 0.703442 1.079317 0.240087 Uiso 0.0327 2 1 d . . .
H1c8 H 0.527802 0.800072 0.352754 Uiso 0.0244 2 1 d . . .
H2c8 H 0.641111 0.763468 0.339479 Uiso 0.0244 2 1 d . . .
H1c9 H 0.593708 0.808626 0.453774 Uiso 0.0284 2 1 d . . .
H2c9 H 0.690165 0.872979 0.394415 Uiso 0.0284 2 1 d . . .
H3c9 H 0.56713 0.903979 0.41323 Uiso 0.0284 2 1 d . . .
H1c10 H 0.652991 0.810392 -0.053511 Uiso 0.0316 2 1 d . . .
H2c10 H 0.720173 0.891419 -0.067647 Uiso 0.0316 2 1 d . . .
H1c11 H 0.789274 0.833885 -0.175165 Uiso 0.0464 2 1 d . . .
H2c11 H 0.881865 0.823805 -0.136132 Uiso 0.0464 2 1 d . . .
H3c11 H 0.806961 0.741707 -0.124332 Uiso 0.0464 2 1 d . . .
H1c12 H 0.825892 0.655339 -0.004449 Uiso 0.0308 2 1 d . . .
H2c12 H 0.7839 0.636177 0.083499 Uiso 0.0308 2 1 d . . .
H1c13 H 0.673372 0.560261 0.042335 Uiso 0.0431 2 1 d . . .
H2c13 H 0.600858 0.629365 0.08461 Uiso 0.0431 2 1 d . . .
H3c13 H 0.64393 0.649656 -0.006281 Uiso 0.0431 2 1 d . . .
H1c15 H 0.449789 0.556424 0.286398 Uiso 0.0271 2 1 d . . .
H1c16 H 0.589654 0.465748 0.31849 Uiso 0.0304 2 1 d . . .
H1c17 H 0.765896 0.526083 0.288186 Uiso 0.0286 2 1 d . . .
H1c19 H 0.323086 0.853567 0.232031 Uiso 0.0228 2 1 d . . .
H2c19 H 0.40714 0.893841 0.254981 Uiso 0.0228 2 1 d . . .
H1c20 H 0.315532 1.008841 0.198068 Uiso 0.0289 2 1 d . . .
H2c20 H 0.438739 1.014279 0.14284 Uiso 0.0289 2 1 d . . .
H3c20 H 0.346005 0.973014 0.122773 Uiso 0.0289 2 1 d . . .
H1c21 H 0.46883 0.880299 0.036724 Uiso 0.0242 2 1 d . . .
H2c21 H 0.494893 0.784252 0.044012 Uiso 0.0242 2 1 d . . .
H1c22 H 0.310619 0.801832 0.048817 Uiso 0.0304 2 1 d . . .
H2c22 H 0.310989 0.743409 0.129468 Uiso 0.0304 2 1 d . . .
H3c22 H 0.283913 0.844359 0.120248 Uiso 0.0304 2 1 d . . .
H1c23 H 1.06459 0.70756 0.278662 Uiso 0.057 2 1 d . . .
H2c23 H 0.992863 0.776252 0.24306 Uiso 0.057 2 1 d . . .
H1c24 H 0.940036 0.761256 0.378427 Uiso 0.082 2 1 d . . .
H2c24 H 0.839937 0.736559 0.355833 Uiso 0.082 2 1 d . . .
H3c24 H 0.907754 0.661438 0.39178 Uiso 0.082 2 1 d . . .
H1c25 H 1.053374 0.711015 0.112309 Uiso 0.0526 2 1 d . . .
H2c25 H 1.128169 0.646124 0.148324 Uiso 0.0526 2 1 d . . .
H1c26 H 1.096976 0.600165 0.045428 Uiso 0.0696 2 1 d . . .
H2c26 H 1.056629 0.526762 0.123011 Uiso 0.0696 2 1 d . . .
H3c26 H 0.97036 0.588137 0.093525 Uiso 0.0696 2 1 d . . .
H1c28 H 0.546435 0.244859 0.340095 Uiso 0.0213 2 1 d . . .
H1c29 H 0.634267 0.299057 0.410952 Uiso 0.023 2 1 d . . .
H1c31 H 0.345351 0.403478 0.520862 Uiso 0.0248 2 1 d . . .
H1c32 H 0.256895 0.347849 0.450013 Uiso 0.0225 2 1 d . . .
H1c33 H 0.585949 0.34171 0.550884 Uiso 0.0339 2 1 d . . .
H2c33 H 0.616638 0.430755 0.486957 Uiso 0.0339 2 1 d . . .
H3c33 H 0.504962 0.42134 0.556206 Uiso 0.0339 2 1 d . . .
H1c35 H 0.415001 0.118211 0.444454 Uiso 0.0215 2 1 d . . .
H1c36 H 0.391628 -0.034363 0.492718 Uiso 0.0265 2 1 d . . .
H1c38 H 0.216939 -0.042886 0.349192 Uiso 0.0245 2 1 d . . .
H1c39 H 0.235823 0.110394 0.303614 Uiso 0.023 2 1 d . . .
H1c40 H 0.277912 -0.180795 0.41759 Uiso 0.0368 2 1 d . . .
H2c40 H 0.352949 -0.178391 0.468401 Uiso 0.0368 2 1 d . . .
H3c40 H 0.224422 -0.168081 0.50227 Uiso 0.0368 2 1 d . . .
H1c42 H 0.140428 0.214144 0.462022 Uiso 0.0215 2 1 d . . .
H1c43 H -0.040989 0.261157 0.482709 Uiso 0.0256 2 1 d . . .
H1c45 H 0.041163 0.390944 0.255817 Uiso 0.0271 2 1 d . . .
H1c46 H 0.222994 0.34566 0.236221 Uiso 0.0236 2 1 d . . .
H1c47 H -0.18263 0.338628 0.436431 Uiso 0.0418 2 1 d . . .
H2c47 H -0.137508 0.427545 0.374843 Uiso 0.0418 2 1 d . . .
H3c47 H -0.166724 0.34614 0.348753 Uiso 0.0418 2 1 d . . .
H1c49 H 0.433029 0.158698 0.209798 Uiso 0.0206 2 1 d . . .
H1c50 H 0.539328 0.214424 0.080691 Uiso 0.0245 2 1 d . . .
H1c52 H 0.513417 0.462328 0.117492 Uiso 0.0288 2 1 d . . .
H1c53 H 0.416134 0.40527 0.247233 Uiso 0.0268 2 1 d . . .
H1c54 H 0.603586 0.446356 -0.010324 Uiso 0.036 2 1 d . . .
H2c54 H 0.680628 0.364227 -0.008024 Uiso 0.036 2 1 d . . .
H3c54 H 0.575133 0.361827 -0.03263 Uiso 0.036 2 1 d . . .
H1c55 H 0.270848 0.502097 0.30113 Uiso 0.0384 2 1 d . . .
H2c55 H 0.175786 0.542616 0.265431 Uiso 0.0384 2 1 d . . .
H1c56 H 0.124153 0.453452 0.404319 Uiso 0.0358 2 1 d . . .
H2c56 H 0.053834 0.540634 0.382134 Uiso 0.0358 2 1 d . . .
H1c57 H 0.227035 0.529674 0.444403 Uiso 0.0475 2 1 d . . .
H2c57 H 0.108382 0.576519 0.472604 Uiso 0.0475 2 1 d . . .
H1c58 H 0.16107 0.693702 0.375599 Uiso 0.0376 2 1 d . . .
H2c58 H 0.281332 0.667213 0.380464 Uiso 0.0376 2 1 d . . .
H1c59 H 0.800566 0.181435 0.134552 Uiso 0.0495 2 1 d . . .
H2c59 H 0.789506 0.268677 0.07145 Uiso 0.0495 2 1 d . . .
H1c60 H 0.678193 0.303394 0.180123 Uiso 0.0538 2 1 d . . .
H2c60 H 0.759277 0.256086 0.229051 Uiso 0.0538 2 1 d . . .
H1c61 H 0.811312 0.397053 0.200211 Uiso 0.0701 2 1 d . . .
H2c61 H 0.80016 0.41319 0.113869 Uiso 0.0701 2 1 d . . .
H1c62 H 0.980667 0.38647 0.083873 Uiso 0.0872 2 1 d . . .
H2c62 H 0.966082 0.323609 0.167299 Uiso 0.0872 2 1 d . . .
H1c63 H 0.83039 0.125718 0.333521 Uiso 0.0736 2 1 d . . .
H2c63 H 0.91295 0.114845 0.251302 Uiso 0.0736 2 1 d . . .
H1c64 H 0.98854 0.162971 0.337593 Uiso 0.0831 2 1 d . . .
H2c64 H 1.051222 0.085393 0.296169 Uiso 0.0831 2 1 d . . .
H1c65 H 0.902279 0.065269 0.445586 Uiso 0.0559 2 1 d . . .
H2c65 H 1.024011 0.02173 0.419206 Uiso 0.0559 2 1 d . . .
H1c66 H 0.962041 -0.0786 0.378454 Uiso 0.0609 2 1 d . . .
H2c66 H 0.844718 -0.061651 0.438506 Uiso 0.0609 2 1 d . . .



#==============================================================================0

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 Fe1 . . 2.4880(19) ?
Br1 N1 . . 3.087(2) ?
Fe1 P1 . . 2.2435(15) ?
Fe1 P2 . . 2.2523(16) ?
Fe1 N1 . . 2.063(3) ?
Fe1 P3 . . 2.1896(19) ?
P1 N2 . . 1.703(3) ?
P1 C6 . . 1.842(3) ?
P1 C8 . . 1.822(2) ?
P2 N3 . . 1.708(3) ?
P2 C10 . . 1.837(3) ?
P2 C12 . . 1.826(3) ?
N1 C1 . . 1.367(4) ?
N1 C5 . . 1.364(3) ?
N2 C1 . . 1.364(3) ?
N2 H1n2 . . 0.88(4) ?
N3 C5 . . 1.369(4) ?
N3 H1n3 . . 0.82(3) ?
C1 C2 . . 1.391(4) ?
C2 C3 . . 1.378(3) ?
C2 H1c2 . . 0.96 ?
C3 C4 . . 1.387(4) ?
C3 H1c3 . . 0.96 ?
C4 C5 . . 1.397(4) ?
C4 H1c4 . . 0.96 ?
C6 C7 . . 1.524(4) ?
C6 H1c6 . . 0.96 ?
C6 H2c6 . . 0.96 ?
C7 H1c7 . . 0.96 ?
C7 H2c7 . . 0.96 ?
C7 H3c7 . . 0.96 ?
C8 C9 . . 1.527(4) ?
C8 H1c8 . . 0.96 ?
C8 H2c8 . . 0.96 ?
C9 H1c9 . . 0.96 ?
C9 H2c9 . . 0.96 ?
C9 H3c9 . . 0.96 ?
C10 C11 . . 1.516(4) ?
C10 H1c10 . . 0.96 ?
C10 H2c10 . . 0.96 ?
C11 H1c11 . . 0.96 ?
C11 H2c11 . . 0.96 ?
C11 H3c11 . . 0.96 ?
C12 C13 . . 1.502(5) ?
C12 H1c12 . . 0.96 ?
C12 H2c12 . . 0.96 ?
C13 H1c13 . . 0.96 ?
C13 H2c13 . . 0.96 ?
C13 H3c13 . . 0.96 ?
P3 N5 . . 1.686(2) ?
P3 C19 . . 1.837(2) ?
P3 C21 . . 1.840(3) ?
P4 N6 . . 1.738(3) ?
P4 C23 . . 1.831(4) ?
P4 C25 . . 1.836(3) ?
N4 C14 . . 1.364(3) ?
N4 C18 . . 1.384(3) ?
N5 C14 . . 1.375(3) ?
N5 H1n5 . . 0.74(3) ?
N6 C18 . . 1.364(3) ?
N6 H1n6 . . 0.85(3) ?
C14 C15 . . 1.393(3) ?
C15 C16 . . 1.386(4) ?
C15 H1c15 . . 0.96 ?
C16 C17 . . 1.364(4) ?
C16 H1c16 . . 0.96 ?
C17 C18 . . 1.401(3) ?
C17 H1c17 . . 0.96 ?
C19 C20 . . 1.532(3) ?
C19 H1c19 . . 0.96 ?
C19 H2c19 . . 0.96 ?
C20 H1c20 . . 0.96 ?
C20 H2c20 . . 0.96 ?
C20 H3c20 . . 0.96 ?
C21 C22 . . 1.536(4) ?
C21 H1c21 . . 0.96 ?
C21 H2c21 . . 0.96 ?
C22 H1c22 . . 0.96 ?
C22 H2c22 . . 0.96 ?
C22 H3c22 . . 0.96 ?
C23 C24 . . 1.528(5) ?
C23 H1c23 . . 0.96 ?
C23 H2c23 . . 0.96 ?
C24 H1c24 . . 0.96 ?
C24 H2c24 . . 0.96 ?
C24 H3c24 . . 0.96 ?
C25 C26 . . 1.527(6) ?
C25 H1c25 . . 0.96 ?
C25 H2c25 . . 0.96 ?
C26 H1c26 . . 0.96 ?
C26 H2c26 . . 0.96 ?
C26 H3c26 . . 0.96 ?
C27 C28 . . 1.406(4) ?
C27 C32 . . 1.404(3) ?
C27 B1 . . 1.654(4) ?
C28 C29 . . 1.390(4) ?
C28 H1c28 . . 0.96 ?
C29 C30 . . 1.398(3) ?
C29 H1c29 . . 0.96 ?
C30 C31 . . 1.388(4) ?
C30 C33 . . 1.522(4) ?
C31 C32 . . 1.405(4) ?
C31 H1c31 . . 0.96 ?
C32 H1c32 . . 0.96 ?
C33 H1c33 . . 0.96 ?
C33 H2c33 . . 0.96 ?
C33 H3c33 . . 0.96 ?
C34 C35 . . 1.405(3) ?
C34 C39 . . 1.411(4) ?
C34 B1 . . 1.649(3) ?
C35 C36 . . 1.391(3) ?
C35 H1c35 . . 0.96 ?
C36 C37 . . 1.390(4) ?
C36 H1c36 . . 0.96 ?
C37 C38 . . 1.394(4) ?
C37 C40 . . 1.514(3) ?
C38 C39 . . 1.392(3) ?
C38 H1c38 . . 0.96 ?
C39 H1c39 . . 0.96 ?
C40 H1c40 . . 0.96 ?
C40 H2c40 . . 0.96 ?
C40 H3c40 . . 0.96 ?
C41 C42 . . 1.408(3) ?
C41 C46 . . 1.404(3) ?
C41 B1 . . 1.652(4) ?
C42 C43 . . 1.395(4) ?
C42 H1c42 . . 0.96 ?
C43 C44 . . 1.401(4) ?
C43 H1c43 . . 0.96 ?
C44 C45 . . 1.390(3) ?
C44 C47 . . 1.513(4) ?
C45 C46 . . 1.396(4) ?
C45 H1c45 . . 0.96 ?
C46 H1c46 . . 0.96 ?
C47 H1c47 . . 0.96 ?
C47 H2c47 . . 0.96 ?
C47 H3c47 . . 0.96 ?
C48 C49 . . 1.406(3) ?
C48 C53 . . 1.404(3) ?
C48 B1 . . 1.643(3) ?
C49 C50 . . 1.398(3) ?
C49 H1c49 . . 0.96 ?
C50 C51 . . 1.391(3) ?
C50 H1c50 . . 0.96 ?
C51 C52 . . 1.393(4) ?
C51 C54 . . 1.514(3) ?
C52 C53 . . 1.387(3) ?
C52 H1c52 . . 0.96 ?
C53 H1c53 . . 0.96 ?
C54 H1c54 . . 0.96 ?
C54 H2c54 . . 0.96 ?
C54 H3c54 . . 0.96 ?
O1 C55 . . 1.445(3) ?
O1 C58 . . 1.442(4) ?
C55 C56 . . 1.518(4) ?
C55 H1c55 . . 0.96 ?
C55 H2c55 . . 0.96 ?
C56 C57 . . 1.516(5) ?
C56 H1c56 . . 0.96 ?
C56 H2c56 . . 0.96 ?
C57 C58 . . 1.518(4) ?
C57 H1c57 . . 0.96 ?
C57 H2c57 . . 0.96 ?
C58 H1c58 . . 0.96 ?
C58 H2c58 . . 0.96 ?
O2 C59 . . 1.427(4) ?
O2 C62 . . 1.431(5) ?
C59 C60 . . 1.531(5) ?
C59 H1c59 . . 0.96 ?
C59 H2c59 . . 0.96 ?
C60 C61 . . 1.484(5) ?
C60 H1c60 . . 0.96 ?
C60 H2c60 . . 0.96 ?
C61 C62 . . 1.526(5) ?
C61 H1c61 . . 0.96 ?
C61 H2c61 . . 0.96 ?
C62 H1c62 . . 0.96 ?
C62 H2c62 . . 0.96 ?
O3 C63 . . 1.424(4) ?
O3 C66 . . 1.459(5) ?
C63 C64 . . 1.439(7) ?
C63 H1c63 . . 0.96 ?
C63 H2c63 . . 0.96 ?
C64 C65 . . 1.478(5) ?
C64 H1c64 . . 0.96 ?
C64 H2c64 . . 0.96 ?
C65 C66 . . 1.515(6) ?
C65 H1c65 . . 0.96 ?
C65 H2c65 . . 0.96 ?
C66 H1c66 . . 0.96 ?
C66 H2c66 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Br1 Fe1 P1 . . . 90.29(3) ?
Br1 Fe1 P2 . . . 90.06(3) ?
Br1 Fe1 N1 . . . 84.86(5) ?
Br1 Fe1 P3 . . . 86.87(2) ?
P1 Fe1 P2 . . . 163.98(3) ?
P1 Fe1 N1 . . . 82.00(6) ?
P1 Fe1 P3 . . . 95.64(3) ?
P2 Fe1 N1 . . . 82.08(6) ?
P2 Fe1 P3 . . . 100.37(3) ?
N1 Fe1 P3 . . . 171.39(5) ?
Fe1 P1 N2 . . . 101.01(8) ?
Fe1 P1 C6 . . . 123.91(9) ?
Fe1 P1 C8 . . . 118.55(9) ?
N2 P1 C6 . . . 103.91(11) ?
N2 P1 C8 . . . 102.74(11) ?
C6 P1 C8 . . . 103.65(10) ?
Fe1 P2 N3 . . . 100.47(9) ?
Fe1 P2 C10 . . . 124.37(9) ?
Fe1 P2 C12 . . . 121.42(8) ?
N3 P2 C10 . . . 103.04(11) ?
N3 P2 C12 . . . 100.60(12) ?
C10 P2 C12 . . . 102.64(13) ?
Br1 N1 Fe1 . . . 53.39(5) ?
Br1 N1 C1 . . . 104.34(13) ?
Br1 N1 C5 . . . 102.65(15) ?
Fe1 N1 C1 . . . 120.36(14) ?
Fe1 N1 C5 . . . 120.72(19) ?
C1 N1 C5 . . . 117.9(2) ?
P1 N2 C1 . . . 119.8(2) ?
P1 N2 H1n2 . . . 124.1(17) ?
C1 N2 H1n2 . . . 115.4(16) ?
P2 N3 C5 . . . 120.60(16) ?
P2 N3 H1n3 . . . 124(3) ?
C5 N3 H1n3 . . . 115(3) ?
N1 C1 N2 . . . 115.6(2) ?
N1 C1 C2 . . . 122.5(2) ?
N2 C1 C2 . . . 121.9(3) ?
C1 C2 C3 . . . 118.4(3) ?
C1 C2 H1c2 . . . 120.78 ?
C3 C2 H1c2 . . . 120.78 ?
C2 C3 C4 . . . 120.7(3) ?
C2 C3 H1c3 . . . 119.66 ?
C4 C3 H1c3 . . . 119.66 ?
C3 C4 C5 . . . 118.3(2) ?
C3 C4 H1c4 . . . 120.84 ?
C5 C4 H1c4 . . . 120.84 ?
N1 C5 N3 . . . 115.3(2) ?
N1 C5 C4 . . . 122.1(3) ?
N3 C5 C4 . . . 122.5(2) ?
P1 C6 C7 . . . 116.52(19) ?
P1 C6 H1c6 . . . 109.47 ?
P1 C6 H2c6 . . . 109.47 ?
C7 C6 H1c6 . . . 109.47 ?
C7 C6 H2c6 . . . 109.47 ?
H1c6 C6 H2c6 . . . 101.36 ?
C6 C7 H1c7 . . . 109.47 ?
C6 C7 H2c7 . . . 109.47 ?
C6 C7 H3c7 . . . 109.47 ?
H1c7 C7 H2c7 . . . 109.47 ?
H1c7 C7 H3c7 . . . 109.47 ?
H2c7 C7 H3c7 . . . 109.47 ?
P1 C8 C9 . . . 116.24(16) ?
P1 C8 H1c8 . . . 109.47 ?
P1 C8 H2c8 . . . 109.47 ?
C9 C8 H1c8 . . . 109.47 ?
C9 C8 H2c8 . . . 109.47 ?
H1c8 C8 H2c8 . . . 101.73 ?
C8 C9 H1c9 . . . 109.47 ?
C8 C9 H2c9 . . . 109.47 ?
C8 C9 H3c9 . . . 109.47 ?
H1c9 C9 H2c9 . . . 109.47 ?
H1c9 C9 H3c9 . . . 109.47 ?
H2c9 C9 H3c9 . . . 109.47 ?
P2 C10 C11 . . . 116.5(2) ?
P2 C10 H1c10 . . . 109.47 ?
P2 C10 H2c10 . . . 109.47 ?
C11 C10 H1c10 . . . 109.47 ?
C11 C10 H2c10 . . . 109.47 ?
H1c10 C10 H2c10 . . . 101.35 ?
C10 C11 H1c11 . . . 109.47 ?
C10 C11 H2c11 . . . 109.47 ?
C10 C11 H3c11 . . . 109.47 ?
H1c11 C11 H2c11 . . . 109.47 ?
H1c11 C11 H3c11 . . . 109.47 ?
H2c11 C11 H3c11 . . . 109.47 ?
P2 C12 C13 . . . 114.09(19) ?
P2 C12 H1c12 . . . 109.47 ?
P2 C12 H2c12 . . . 109.47 ?
C13 C12 H1c12 . . . 109.47 ?
C13 C12 H2c12 . . . 109.47 ?
H1c12 C12 H2c12 . . . 104.42 ?
C12 C13 H1c13 . . . 109.47 ?
C12 C13 H2c13 . . . 109.47 ?
C12 C13 H3c13 . . . 109.47 ?
H1c13 C13 H2c13 . . . 109.47 ?
H1c13 C13 H3c13 . . . 109.47 ?
H2c13 C13 H3c13 . . . 109.47 ?
Fe1 P3 N5 . . . 100.87(9) ?
Fe1 P3 C19 . . . 124.13(9) ?
Fe1 P3 C21 . . . 122.38(7) ?
N5 P3 C19 . . . 101.23(10) ?
N5 P3 C21 . . . 104.14(12) ?
C19 P3 C21 . . . 100.52(12) ?
N6 P4 C23 . . . 100.98(14) ?
N6 P4 C25 . . . 101.12(13) ?
C23 P4 C25 . . . 101.14(15) ?
C14 N4 C18 . . . 116.59(17) ?
P3 N5 C14 . . . 121.16(17) ?
P3 N5 H1n5 . . . 125.5(19) ?
C14 N5 H1n5 . . . 113.0(19) ?
P4 N6 C18 . . . 126.81(16) ?
P4 N6 H1n6 . . . 122(2) ?
C18 N6 H1n6 . . . 111(2) ?
N4 C14 N5 . . . 117.53(18) ?
N4 C14 C15 . . . 123.3(2) ?
N5 C14 C15 . . . 119.2(2) ?
C14 C15 C16 . . . 118.6(2) ?
C14 C15 H1c15 . . . 120.68 ?
C16 C15 H1c15 . . . 120.69 ?
C15 C16 C17 . . . 119.9(2) ?
C15 C16 H1c16 . . . 120.05 ?
C17 C16 H1c16 . . . 120.06 ?
C16 C17 C18 . . . 119.7(2) ?
C16 C17 H1c17 . . . 120.14 ?
C18 C17 H1c17 . . . 120.14 ?
N4 C18 N6 . . . 117.74(18) ?
N4 C18 C17 . . . 121.8(2) ?
N6 C18 C17 . . . 120.4(2) ?
P3 C19 C20 . . . 115.56(14) ?
P3 C19 H1c19 . . . 109.47 ?
P3 C19 H2c19 . . . 109.47 ?
C20 C19 H1c19 . . . 109.47 ?
C20 C19 H2c19 . . . 109.47 ?
H1c19 C19 H2c19 . . . 102.61 ?
C19 C20 H1c20 . . . 109.47 ?
C19 C20 H2c20 . . . 109.47 ?
C19 C20 H3c20 . . . 109.47 ?
H1c20 C20 H2c20 . . . 109.47 ?
H1c20 C20 H3c20 . . . 109.47 ?
H2c20 C20 H3c20 . . . 109.47 ?
P3 C21 C22 . . . 115.88(16) ?
P3 C21 H1c21 . . . 109.47 ?
P3 C21 H2c21 . . . 109.47 ?
C22 C21 H1c21 . . . 109.47 ?
C22 C21 H2c21 . . . 109.47 ?
H1c21 C21 H2c21 . . . 102.2 ?
C21 C22 H1c22 . . . 109.47 ?
C21 C22 H2c22 . . . 109.47 ?
C21 C22 H3c22 . . . 109.47 ?
H1c22 C22 H2c22 . . . 109.47 ?
H1c22 C22 H3c22 . . . 109.47 ?
H2c22 C22 H3c22 . . . 109.47 ?
P4 C23 C24 . . . 112.1(2) ?
P4 C23 H1c23 . . . 109.47 ?
P4 C23 H2c23 . . . 109.47 ?
C24 C23 H1c23 . . . 109.47 ?
C24 C23 H2c23 . . . 109.47 ?
H1c23 C23 H2c23 . . . 106.7 ?
C23 C24 H1c24 . . . 109.47 ?
C23 C24 H2c24 . . . 109.47 ?
C23 C24 H3c24 . . . 109.47 ?
H1c24 C24 H2c24 . . . 109.47 ?
H1c24 C24 H3c24 . . . 109.47 ?
H2c24 C24 H3c24 . . . 109.47 ?
P4 C25 C26 . . . 112.1(2) ?
P4 C25 H1c25 . . . 109.47 ?
P4 C25 H2c25 . . . 109.47 ?
C26 C25 H1c25 . . . 109.47 ?
C26 C25 H2c25 . . . 109.47 ?
H1c25 C25 H2c25 . . . 106.71 ?
C25 C26 H1c26 . . . 109.47 ?
C25 C26 H2c26 . . . 109.47 ?
C25 C26 H3c26 . . . 109.47 ?
H1c26 C26 H2c26 . . . 109.47 ?
H1c26 C26 H3c26 . . . 109.47 ?
H2c26 C26 H3c26 . . . 109.47 ?
C28 C27 C32 . . . 114.8(2) ?
C28 C27 B1 . . . 119.33(19) ?
C32 C27 B1 . . . 125.9(2) ?
C27 C28 C29 . . . 123.2(2) ?
C27 C28 H1c28 . . . 118.42 ?
C29 C28 H1c28 . . . 118.42 ?
C28 C29 C30 . . . 121.0(2) ?
C28 C29 H1c29 . . . 119.5 ?
C30 C29 H1c29 . . . 119.5 ?
C29 C30 C31 . . . 117.2(3) ?
C29 C30 C33 . . . 120.8(2) ?
C31 C30 C33 . . . 122.0(2) ?
C30 C31 C32 . . . 121.3(2) ?
C30 C31 H1c31 . . . 119.34 ?
C32 C31 H1c31 . . . 119.34 ?
C27 C32 C31 . . . 122.5(2) ?
C27 C32 H1c32 . . . 118.77 ?
C31 C32 H1c32 . . . 118.77 ?
C30 C33 H1c33 . . . 109.47 ?
C30 C33 H2c33 . . . 109.47 ?
C30 C33 H3c33 . . . 109.47 ?
H1c33 C33 H2c33 . . . 109.47 ?
H1c33 C33 H3c33 . . . 109.47 ?
H2c33 C33 H3c33 . . . 109.47 ?
C35 C34 C39 . . . 114.8(2) ?
C35 C34 B1 . . . 125.2(2) ?
C39 C34 B1 . . . 119.9(2) ?
C34 C35 C36 . . . 123.2(3) ?
C34 C35 H1c35 . . . 118.39 ?
C36 C35 H1c35 . . . 118.39 ?
C35 C36 C37 . . . 120.6(2) ?
C35 C36 H1c36 . . . 119.68 ?
C37 C36 H1c36 . . . 119.68 ?
C36 C37 C38 . . . 117.7(2) ?
C36 C37 C40 . . . 121.1(2) ?
C38 C37 C40 . . . 121.2(3) ?
C37 C38 C39 . . . 121.3(3) ?
C37 C38 H1c38 . . . 119.36 ?
C39 C38 H1c38 . . . 119.36 ?
C34 C39 C38 . . . 122.3(2) ?
C34 C39 H1c39 . . . 118.85 ?
C38 C39 H1c39 . . . 118.85 ?
C37 C40 H1c40 . . . 109.47 ?
C37 C40 H2c40 . . . 109.47 ?
C37 C40 H3c40 . . . 109.47 ?
H1c40 C40 H2c40 . . . 109.47 ?
H1c40 C40 H3c40 . . . 109.47 ?
H2c40 C40 H3c40 . . . 109.47 ?
C42 C41 C46 . . . 114.5(2) ?
C42 C41 B1 . . . 120.2(2) ?
C46 C41 B1 . . . 125.29(17) ?
C41 C42 C43 . . . 122.9(2) ?
C41 C42 H1c42 . . . 118.54 ?
C43 C42 H1c42 . . . 118.55 ?
C42 C43 C44 . . . 121.17(19) ?
C42 C43 H1c43 . . . 119.42 ?
C44 C43 H1c43 . . . 119.41 ?
C43 C44 C45 . . . 117.0(2) ?
C43 C44 C47 . . . 122.0(2) ?
C45 C44 C47 . . . 120.9(2) ?
C44 C45 C46 . . . 121.2(2) ?
C44 C45 H1c45 . . . 119.41 ?
C46 C45 H1c45 . . . 119.41 ?
C41 C46 C45 . . . 123.22(19) ?
C41 C46 H1c46 . . . 118.39 ?
C45 C46 H1c46 . . . 118.39 ?
C44 C47 H1c47 . . . 109.47 ?
C44 C47 H2c47 . . . 109.47 ?
C44 C47 H3c47 . . . 109.47 ?
H1c47 C47 H2c47 . . . 109.47 ?
H1c47 C47 H3c47 . . . 109.47 ?
H2c47 C47 H3c47 . . . 109.47 ?
C49 C48 C53 . . . 114.24(18) ?
C49 C48 B1 . . . 126.83(18) ?
C53 C48 B1 . . . 118.9(2) ?
C48 C49 C50 . . . 123.2(2) ?
C48 C49 H1c49 . . . 118.41 ?
C50 C49 H1c49 . . . 118.41 ?
C49 C50 C51 . . . 120.8(2) ?
C49 C50 H1c50 . . . 119.59 ?
C51 C50 H1c50 . . . 119.59 ?
C50 C51 C52 . . . 117.20(19) ?
C50 C51 C54 . . . 122.1(2) ?
C52 C51 C54 . . . 120.7(2) ?
C51 C52 C53 . . . 121.3(2) ?
C51 C52 H1c52 . . . 119.37 ?
C53 C52 H1c52 . . . 119.37 ?
C48 C53 C52 . . . 123.3(2) ?
C48 C53 H1c53 . . . 118.37 ?
C52 C53 H1c53 . . . 118.37 ?
C51 C54 H1c54 . . . 109.47 ?
C51 C54 H2c54 . . . 109.47 ?
C51 C54 H3c54 . . . 109.47 ?
H1c54 C54 H2c54 . . . 109.47 ?
H1c54 C54 H3c54 . . . 109.47 ?
H2c54 C54 H3c54 . . . 109.47 ?
C27 B1 C34 . . . 109.51(19) ?
C27 B1 C41 . . . 111.49(19) ?
C27 B1 C48 . . . 107.16(18) ?
C34 B1 C41 . . . 107.16(17) ?
C34 B1 C48 . . . 112.48(18) ?
C41 B1 C48 . . . 109.09(19) ?
C55 O1 C58 . . . 109.24(18) ?
O1 C55 C56 . . . 105.6(2) ?
O1 C55 H1c55 . . . 109.47 ?
O1 C55 H2c55 . . . 109.47 ?
C56 C55 H1c55 . . . 109.47 ?
C56 C55 H2c55 . . . 109.47 ?
H1c55 C55 H2c55 . . . 113.1 ?
C55 C56 C57 . . . 102.1(2) ?
C55 C56 H1c56 . . . 109.47 ?
C55 C56 H2c56 . . . 109.47 ?
C57 C56 H1c56 . . . 109.47 ?
C57 C56 H2c56 . . . 109.47 ?
H1c56 C56 H2c56 . . . 115.98 ?
C56 C57 C58 . . . 102.5(2) ?
C56 C57 H1c57 . . . 109.47 ?
C56 C57 H2c57 . . . 109.47 ?
C58 C57 H1c57 . . . 109.47 ?
C58 C57 H2c57 . . . 109.47 ?
H1c57 C57 H2c57 . . . 115.61 ?
O1 C58 C57 . . . 106.6(2) ?
O1 C58 H1c58 . . . 109.47 ?
O1 C58 H2c58 . . . 109.47 ?
C57 C58 H1c58 . . . 109.47 ?
C57 C58 H2c58 . . . 109.47 ?
H1c58 C58 H2c58 . . . 112.24 ?
C59 O2 C62 . . . 108.2(2) ?
O2 C59 C60 . . . 105.3(3) ?
O2 C59 H1c59 . . . 109.47 ?
O2 C59 H2c59 . . . 109.47 ?
C60 C59 H1c59 . . . 109.47 ?
C60 C59 H2c59 . . . 109.47 ?
H1c59 C59 H2c59 . . . 113.33 ?
C59 C60 C61 . . . 101.1(2) ?
C59 C60 H1c60 . . . 109.47 ?
C59 C60 H2c60 . . . 109.47 ?
C61 C60 H1c60 . . . 109.47 ?
C61 C60 H2c60 . . . 109.47 ?
H1c60 C60 H2c60 . . . 116.72 ?
C60 C61 C62 . . . 101.4(3) ?
C60 C61 H1c61 . . . 109.47 ?
C60 C61 H2c61 . . . 109.47 ?
C62 C61 H1c61 . . . 109.47 ?
C62 C61 H2c61 . . . 109.47 ?
H1c61 C61 H2c61 . . . 116.52 ?
O2 C62 C61 . . . 106.9(3) ?
O2 C62 H1c62 . . . 109.47 ?
O2 C62 H2c62 . . . 109.47 ?
C61 C62 H1c62 . . . 109.47 ?
C61 C62 H2c62 . . . 109.47 ?
H1c62 C62 H2c62 . . . 111.93 ?
C63 O3 C66 . . . 107.0(3) ?
O3 C63 C64 . . . 105.9(3) ?
O3 C63 H1c63 . . . 109.47 ?
O3 C63 H2c63 . . . 109.47 ?
C64 C63 H1c63 . . . 109.47 ?
C64 C63 H2c63 . . . 109.47 ?
H1c63 C63 H2c63 . . . 112.86 ?
C63 C64 C65 . . . 102.8(3) ?
C63 C64 H1c64 . . . 109.47 ?
C63 C64 H2c64 . . . 109.47 ?
C65 C64 H1c64 . . . 109.47 ?
C65 C64 H2c64 . . . 109.47 ?
H1c64 C64 H2c64 . . . 115.44 ?
C64 C65 C66 . . . 101.8(3) ?
C64 C65 H1c65 . . . 109.47 ?
C64 C65 H2c65 . . . 109.47 ?
C66 C65 H1c65 . . . 109.47 ?
C66 C65 H2c65 . . . 109.47 ?
H1c65 C65 H2c65 . . . 116.18 ?
O3 C66 C65 . . . 105.3(2) ?
O3 C66 H1c66 . . . 109.47 ?
O3 C66 H2c66 . . . 109.47 ?
C65 C66 H1c66 . . . 109.47 ?
C65 C66 H2c66 . . . 109.47 ?
H1c66 C66 H2c66 . . . 113.32 ?


loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N3 H1n3 O2 . . 2_765 0.82(3) 2.16(3) 2.971(3) 169(3) ?
N5 H1n5 O1 . . . 0.74(3) 2.26(2) 2.985(3) 165(3) ?
N6 H1n6 N1 . . . 0.85(3) 2.06(3) 2.909(3) 175(4) ?
N2 H1n2 O3 . . 1_565 0.88(4) 2.04(4) 2.917(4) 172(2) ?
_database_code_depnum_ccdc_archive 'CCDC 1005381'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

# 5. CHEMICAL DATA

_chemical_name_systematic        
; 
3  --  [Fe(k³-P,N,P-PNPMe-Ph)(k²-P,N-PNNHMe-Ph)Cl]BF₄
;
_chemical_name_common            
'3  [Fe(k3-P,N,P-PNPMe-Ph)(k2-P,N-PNNHMe-Ph)Cl]BF4'
_chemical_formula_moiety         'C50 H49 Cl Fe N6 P3, B F4 '
_chemical_formula_sum            'C50 H49 B1 Cl1 F4 Fe1 N6 P3'
_chemical_formula_weight         1005

#==============================================================================0

# 6. CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn '
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x+1/2,-y+1/2,z+1/2
_cell_length_a                   14.5198(17)
_cell_length_b                   21.308(3)
_cell_length_c                   15.1462(18)
_cell_angle_alpha                90
_cell_angle_beta                 99.710(4)
_cell_angle_gamma                90
_cell_volume                     4618.9(10)


_cell_formula_units_Z            4

_cell_measurement_reflns_used    9357
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      32.5
_cell_measurement_temperature    100
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.4448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2080

_exptl_absorpt_coefficient_mu    0.549
_exptl_crystal_description       'trapezoidal prism'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.19
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            'clear green'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  0.90

#==============================================================================0

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_reflns_number            275623
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         32.61
_diffrn_reflns_theta_full        32.61
_diffrn_measured_fraction_theta_max 1
_diffrn_measured_fraction_theta_full 1
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_reduction_process ?


_diffrn_radiation_probe          X-ray

#==============================================================================0

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             16814
_reflns_number_gt                13277
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_gt          0.0868
_refine_ls_R_factor_all          0.0487
_refine_ls_wR_factor_ref         0.0976
_refine_ls_goodness_of_fit_ref   1.63
_refine_ls_goodness_of_fit_gt    1.63
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         16814
_refine_ls_number_parameters     599
_refine_ls_number_restraints     0
_refine_ls_number_constraints    192
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0016I²)
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          0.0088
_refine_ls_shift/su_mean         0.0005
_refine_diff_density_max         0.42
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
B 0.0013 0.0007 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Cl 0.1484 0.1585 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
F 0.0171 0.0103 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
P 0.1023 0.0942 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'Jana2006 [Petricek et al., 2006]'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

#==============================================================================0

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_mutiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.190274(11) 0.811088(7) 0.203766(10) Uani 0.00781(4) 4 1 d . . .
Cl1 Cl 0.086429(19) 0.839850(12) 0.075440(18) Uani 0.01262(7) 4 1 d . . .
P1 P 0.07196(2) 0.790756(13) 0.276465(19) Uani 0.00983(7) 4 1 d . . .
P2 P 0.30741(2) 0.802411(13) 0.125269(19) Uani 0.00962(7) 4 1 d . . .
P3 P 0.20920(2) 0.909989(13) 0.240006(19) Uani 0.00955(7) 4 1 d . . .
F1 F 0.83968(6) 0.56577(4) 0.14519(6) Uani 0.0280(3) 4 1 d . . .
F2 F 0.91150(8) 0.48410(5) 0.22479(6) Uani 0.0389(3) 4 1 d . . .
F3 F 0.94793(6) 0.50812(4) 0.08852(6) Uani 0.0277(3) 4 1 d . . .
F4 F 0.80808(7) 0.46530(4) 0.09752(6) Uani 0.0331(3) 4 1 d . . .
N1 N 0.15965(7) 0.72293(4) 0.15348(6) Uani 0.0094(2) 4 1 d . . .
N2 N 0.03606(7) 0.71907(4) 0.23393(7) Uani 0.0120(2) 4 1 d . . .
N3 N 0.28259(7) 0.73181(5) 0.07355(7) Uani 0.0125(3) 4 1 d . . .
N4 N 0.28471(7) 0.79664(4) 0.32028(6) Uani 0.0099(2) 4 1 d . . .
N5 N 0.28616(7) 0.90719(4) 0.33716(6) Uani 0.0126(2) 4 1 d . . .
N6 N 0.28749(8) 0.68774(4) 0.30524(7) Uani 0.0143(3) 4 1 d . . .
C1 C 0.08396(8) 0.69107(5) 0.17288(7) Uani 0.0102(3) 4 1 d . . .
C2 C 0.05603(8) 0.63339(5) 0.13338(8) Uani 0.0128(3) 4 1 d . . .
C3 C 0.10312(8) 0.61044(5) 0.06794(8) Uani 0.0143(3) 4 1 d . . .
C4 C 0.17800(8) 0.64275(5) 0.04468(8) Uani 0.0136(3) 4 1 d . . .
C5 C 0.20561(8) 0.69847(5) 0.08970(7) Uani 0.0109(3) 4 1 d . . .
C6 C 0.10074(8) 0.77860(5) 0.39746(8) Uani 0.0129(3) 4 1 d . . .
C7 C 0.08978(9) 0.72116(6) 0.43861(8) Uani 0.0168(3) 4 1 d . . .
C8 C 0.11609(10) 0.71482(6) 0.53092(9) Uani 0.0214(4) 4 1 d . . .
C9 C 0.15556(10) 0.76460(7) 0.58273(9) Uani 0.0228(4) 4 1 d . . .
C10 C 0.16743(10) 0.82193(7) 0.54268(9) Uani 0.0229(4) 4 1 d . . .
C11 C 0.13937(9) 0.82885(6) 0.45108(8) Uani 0.0184(3) 4 1 d . . .
C12 C -0.03865(8) 0.83315(5) 0.26213(8) Uani 0.0142(3) 4 1 d . . .
C13 C -0.09663(9) 0.83115(6) 0.17849(9) Uani 0.0182(3) 4 1 d . . .
C14 C -0.18205(9) 0.86230(7) 0.16529(11) Uani 0.0250(4) 4 1 d . . .
C15 C -0.21032(10) 0.89581(7) 0.23434(12) Uani 0.0300(5) 4 1 d . . .
C16 C -0.15320(10) 0.89846(7) 0.31720(11) Uani 0.0272(4) 4 1 d . . .
C17 C -0.06772(9) 0.86713(6) 0.33167(9) Uani 0.0198(4) 4 1 d . . .
C18 C -0.05088(8) 0.68934(6) 0.25078(9) Uani 0.0165(3) 4 1 d . . .
C19 C 0.42363(8) 0.79055(5) 0.19112(8) Uani 0.0123(3) 4 1 d . . .
C20 C 0.45930(8) 0.73000(6) 0.20740(8) Uani 0.0155(3) 4 1 d . . .
C21 C 0.54246(9) 0.72031(6) 0.26641(9) Uani 0.0212(4) 4 1 d . . .
C22 C 0.59138(9) 0.77086(7) 0.30859(10) Uani 0.0234(4) 4 1 d . . .
C23 C 0.55701(9) 0.83126(6) 0.29297(9) Uani 0.0205(3) 4 1 d . . .
C24 C 0.47310(8) 0.84100(6) 0.23547(8) Uani 0.0154(3) 4 1 d . . .
C25 C 0.32500(8) 0.85018(5) 0.02916(8) Uani 0.0126(3) 4 1 d . . .
C26 C 0.25621(9) 0.84680(6) -0.04802(8) Uani 0.0163(3) 4 1 d . . .
C27 C 0.26585(10) 0.88114(6) -0.12400(8) Uani 0.0202(3) 4 1 d . . .
C28 C 0.34253(10) 0.92040(6) -0.12388(9) Uani 0.0207(4) 4 1 d . . .
C29 C 0.41015(9) 0.92403(6) -0.04758(9) Uani 0.0196(3) 4 1 d . . .
C30 C 0.40241(8) 0.88871(6) 0.02851(8) Uani 0.0159(3) 4 1 d . . .
C31 C 0.33859(9) 0.70664(6) 0.00938(8) Uani 0.0175(3) 4 1 d . . .
C32 C 0.31883(8) 0.84825(5) 0.36913(7) Uani 0.0119(3) 4 1 d . . .
C33 C 0.38420(9) 0.84454(6) 0.44769(8) Uani 0.0177(3) 4 1 d . . .
C34 C 0.41776(10) 0.78602(6) 0.47669(9) Uani 0.0211(3) 4 1 d . . .
C35 C 0.38580(9) 0.73313(6) 0.43013(8) Uani 0.0179(3) 4 1 d . . .
C36 C 0.31892(8) 0.73970(5) 0.35228(7) Uani 0.0116(3) 4 1 d . . .
C37 C 0.26093(8) 0.96358(5) 0.16656(8) Uani 0.0121(3) 4 1 d . . .
C38 C 0.34731(8) 0.99241(5) 0.19415(8) Uani 0.0152(3) 4 1 d . . .
C39 C 0.38249(9) 1.03474(6) 0.13798(9) Uani 0.0196(3) 4 1 d . . .
C40 C 0.33337(10) 1.04781(6) 0.05381(9) Uani 0.0207(4) 4 1 d . . .
C41 C 0.24851(9) 1.01771(6) 0.02404(8) Uani 0.0175(3) 4 1 d . . .
C42 C 0.21258(9) 0.97587(5) 0.07981(8) Uani 0.0143(3) 4 1 d . . .
C43 C 0.11187(8) 0.95942(5) 0.26404(8) Uani 0.0139(3) 4 1 d . . .
C44 C 0.10825(9) 0.98399(6) 0.34907(9) Uani 0.0186(3) 4 1 d . . .
C45 C 0.03487(11) 1.02294(7) 0.36329(10) Uani 0.0250(4) 4 1 d . . .
C46 C -0.03599(11) 1.03753(7) 0.29336(11) Uani 0.0275(4) 4 1 d . . .
C47 C -0.03448(10) 1.01263(6) 0.20897(10) Uani 0.0240(4) 4 1 d . . .
C48 C 0.03839(9) 0.97362(6) 0.19426(9) Uani 0.0174(3) 4 1 d . . .
C49 C 0.32323(9) 0.96245(5) 0.39009(8) Uani 0.0171(3) 4 1 d . . .
C50 C 0.32820(10) 0.62616(6) 0.32289(9) Uani 0.0198(3) 4 1 d . . .
B1 B 0.87637(11) 0.50578(6) 0.13924(10) Uani 0.0176(4) 4 1 d . . .
H21 H 0.005472 0.610232 0.151162 Uiso 0.0154 4 1 d . . .
H31 H 0.083518 0.571644 0.03839 Uiso 0.0172 4 1 d . . .
H41 H 0.210162 0.627236 -0.001272 Uiso 0.0163 4 1 d . . .
H71 H 0.064074 0.685956 0.403245 Uiso 0.0201 4 1 d . . .
H81 H 0.106749 0.675471 0.558979 Uiso 0.0256 4 1 d . . .
H91 H 0.174646 0.759463 0.646144 Uiso 0.0273 4 1 d . . .
H101 H 0.194908 0.8566 0.57818 Uiso 0.0274 4 1 d . . .
H111 H 0.146525 0.868833 0.423806 Uiso 0.0221 4 1 d . . .
H131 H -0.07745 0.808241 0.13011 Uiso 0.0218 4 1 d . . .
H141 H -0.221717 0.860557 0.107823 Uiso 0.03 4 1 d . . .
H151 H -0.269395 0.917149 0.224766 Uiso 0.036 4 1 d . . .
H161 H -0.172551 0.921986 0.364941 Uiso 0.0327 4 1 d . . .
H171 H -0.028663 0.868851 0.389462 Uiso 0.0238 4 1 d . . .
H181 H -0.076004 0.71302 0.295138 Uiso 0.0198 4 1 d . . .
H182 H -0.095446 0.688355 0.196228 Uiso 0.0198 4 1 d . . .
H183 H -0.037863 0.64728 0.271969 Uiso 0.0198 4 1 d . . .
H201 H 0.426228 0.694836 0.177679 Uiso 0.0186 4 1 d . . .
H211 H 0.56601 0.678483 0.277939 Uiso 0.0255 4 1 d . . .
H221 H 0.649154 0.764048 0.348681 Uiso 0.0281 4 1 d . . .
H231 H 0.59116 0.866304 0.321856 Uiso 0.0246 4 1 d . . .
H241 H 0.448735 0.882792 0.226029 Uiso 0.0185 4 1 d . . .
H261 H 0.202304 0.820669 -0.048285 Uiso 0.0195 4 1 d . . .
H271 H 0.219302 0.87776 -0.176921 Uiso 0.0243 4 1 d . . .
H281 H 0.348516 0.944667 -0.17601 Uiso 0.0248 4 1 d . . .
H291 H 0.463 0.951187 -0.047052 Uiso 0.0236 4 1 d . . .
H301 H 0.450455 0.890979 0.080394 Uiso 0.0191 4 1 d . . .
H311 H 0.393178 0.732185 0.010105 Uiso 0.021 4 1 d . . .
H312 H 0.357149 0.664408 0.025777 Uiso 0.021 4 1 d . . .
H313 H 0.302025 0.706895 -0.049671 Uiso 0.021 4 1 d . . .
H331 H 0.405423 0.881684 0.480855 Uiso 0.0213 4 1 d . . .
H341 H 0.463849 0.782487 0.52992 Uiso 0.0253 4 1 d . . .
H351 H 0.408655 0.692427 0.450317 Uiso 0.0214 4 1 d . . .
H381 H 0.382676 0.983058 0.252091 Uiso 0.0183 4 1 d . . .
H391 H 0.441391 1.054966 0.158029 Uiso 0.0235 4 1 d . . .
H401 H 0.357523 1.077515 0.015874 Uiso 0.0249 4 1 d . . .
H411 H 0.214916 1.025922 -0.035017 Uiso 0.021 4 1 d . . .
H421 H 0.15425 0.955161 0.058939 Uiso 0.0172 4 1 d . . .
H441 H 0.156865 0.973923 0.398243 Uiso 0.0223 4 1 d . . .
H451 H 0.033614 1.039672 0.421921 Uiso 0.03 4 1 d . . .
H461 H -0.086001 1.064754 0.303112 Uiso 0.033 4 1 d . . .
H471 H -0.083964 1.022358 0.160419 Uiso 0.0288 4 1 d . . .
H481 H 0.038323 0.956269 0.135755 Uiso 0.0209 4 1 d . . .
H491 H 0.300658 1.000001 0.358665 Uiso 0.0205 4 1 d . . .
H492 H 0.302908 0.961487 0.447191 Uiso 0.0205 4 1 d . . .
H493 H 0.390269 0.961846 0.398878 Uiso 0.0205 4 1 d . . .
H501 H 0.297835 0.597033 0.279059 Uiso 0.0238 4 1 d . . .
H502 H 0.393631 0.62789 0.31974 Uiso 0.0238 4 1 d . . .
H503 H 0.32016 0.61267 0.381582 Uiso 0.0238 4 1 d . . .
H1n H 0.2467(12) 0.6943(8) 0.2589(12) Uiso 0.018(4) 4 1 d . . .




#==============================================================================0

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 Cl1 . . 2.3320(5) ?
Fe1 P1 . . 2.2337(5) ?
Fe1 P2 . . 2.2411(5) ?
Fe1 P3 . . 2.1834(6) ?
Fe1 N1 . . 2.0476(10) ?
Fe1 N4 . . 2.0672(10) ?
Cl1 N1 . . 2.8829(11) ?
Cl1 N2 . . 3.6760(12) ?
Cl1 N3 . . 3.6662(12) ?
P1 N2 . . 1.7049(10) ?
P1 C6 . . 1.8281(12) ?
P1 C12 . . 1.8234(12) ?
P2 N3 . . 1.7064(11) ?
P2 C19 . . 1.8271(11) ?
P2 C25 . . 1.8290(12) ?
P3 N5 . . 1.6920(10) ?
P3 C37 . . 1.8405(12) ?
P3 C43 . . 1.8473(13) ?
F1 B1 . . 1.3936(17) ?
F2 B1 . . 1.3890(17) ?
F3 B1 . . 1.3933(19) ?
F4 B1 . . 1.3840(17) ?
N1 C1 . . 1.3651(15) ?
N1 C5 . . 1.3667(16) ?
N2 C1 . . 1.3827(16) ?
N2 C18 . . 1.4726(16) ?
N3 C5 . . 1.3806(16) ?
N3 C31 . . 1.4697(17) ?
N4 C32 . . 1.3706(14) ?
N4 C36 . . 1.3685(14) ?
N5 C32 . . 1.3996(15) ?
N5 C49 . . 1.4743(15) ?
N6 C36 . . 1.3535(15) ?
N6 C50 . . 1.4455(16) ?
N6 H1n . . 0.850(16) ?
C1 C2 . . 1.3969(15) ?
C2 C3 . . 1.3848(18) ?
C2 H21 . . 0.96 ?
C3 C4 . . 1.3818(18) ?
C3 H31 . . 0.96 ?
C4 C5 . . 1.3939(16) ?
C4 H41 . . 0.96 ?
C6 C7 . . 1.3946(17) ?
C6 C11 . . 1.4026(17) ?
C7 C8 . . 1.3924(18) ?
C7 H71 . . 0.96 ?
C8 C9 . . 1.3848(19) ?
C8 H81 . . 0.96 ?
C9 C10 . . 1.388(2) ?
C9 H91 . . 0.96 ?
C10 C11 . . 1.3863(18) ?
C10 H101 . . 0.96 ?
C11 H111 . . 0.96 ?
C12 C13 . . 1.3984(17) ?
C12 C17 . . 1.4007(19) ?
C13 C14 . . 1.3912(18) ?
C13 H131 . . 0.96 ?
C14 C15 . . 1.385(2) ?
C14 H141 . . 0.96 ?
C15 C16 . . 1.384(2) ?
C15 H151 . . 0.96 ?
C16 C17 . . 1.394(2) ?
C16 H161 . . 0.96 ?
C17 H171 . . 0.96 ?
C18 H181 . . 0.96 ?
C18 H182 . . 0.96 ?
C18 H183 . . 0.96 ?
C19 C20 . . 1.3969(17) ?
C19 C24 . . 1.4000(16) ?
C20 C21 . . 1.3911(17) ?
C20 H201 . . 0.96 ?
C21 C22 . . 1.3857(19) ?
C21 H211 . . 0.96 ?
C22 C23 . . 1.386(2) ?
C22 H221 . . 0.96 ?
C23 C24 . . 1.3885(17) ?
C23 H231 . . 0.96 ?
C24 H241 . . 0.96 ?
C25 C26 . . 1.4056(16) ?
C25 C30 . . 1.3933(17) ?
C26 C27 . . 1.3906(18) ?
C26 H261 . . 0.96 ?
C27 C28 . . 1.392(2) ?
C27 H271 . . 0.96 ?
C28 C29 . . 1.3866(18) ?
C28 H281 . . 0.96 ?
C29 C30 . . 1.3969(19) ?
C29 H291 . . 0.96 ?
C30 H301 . . 0.96 ?
C31 H311 . . 0.96 ?
C31 H312 . . 0.96 ?
C31 H313 . . 0.96 ?
C32 C33 . . 1.3935(16) ?
C33 C34 . . 1.3830(18) ?
C33 H331 . . 0.96 ?
C34 C35 . . 1.3684(18) ?
C34 H341 . . 0.96 ?
C35 C36 . . 1.4024(16) ?
C35 H351 . . 0.96 ?
C37 C38 . . 1.3958(16) ?
C37 C42 . . 1.4059(16) ?
C38 C39 . . 1.3947(19) ?
C38 H381 . . 0.96 ?
C39 C40 . . 1.3802(18) ?
C39 H391 . . 0.96 ?
C40 C41 . . 1.3947(19) ?
C40 H401 . . 0.96 ?
C41 C42 . . 1.3889(18) ?
C41 H411 . . 0.96 ?
C42 H421 . . 0.96 ?
C43 C44 . . 1.3994(18) ?
C43 C48 . . 1.4022(16) ?
C44 C45 . . 1.396(2) ?
C44 H441 . . 0.96 ?
C45 C46 . . 1.382(2) ?
C45 H451 . . 0.96 ?
C46 C47 . . 1.388(2) ?
C46 H461 . . 0.96 ?
C47 C48 . . 1.3928(19) ?
C47 H471 . . 0.96 ?
C48 H481 . . 0.96 ?
C49 H491 . . 0.96 ?
C49 H492 . . 0.96 ?
C49 H493 . . 0.96 ?
C50 H501 . . 0.96 ?
C50 H502 . . 0.96 ?
C50 H503 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Fe1 P1 . . . 91.084(15) ?
Cl1 Fe1 P2 . . . 91.225(15) ?
Cl1 Fe1 P3 . . . 89.550(12) ?
Cl1 Fe1 N1 . . . 82.06(3) ?
Cl1 Fe1 N4 . . . 173.33(3) ?
P1 Fe1 P2 . . . 163.965(13) ?
P1 Fe1 P3 . . . 97.929(13) ?
P1 Fe1 N1 . . . 82.45(3) ?
P1 Fe1 N4 . . . 90.28(3) ?
P2 Fe1 P3 . . . 97.955(13) ?
P2 Fe1 N1 . . . 82.16(3) ?
P2 Fe1 N4 . . . 89.26(3) ?
P3 Fe1 N1 . . . 171.60(3) ?
P3 Fe1 N4 . . . 83.79(3) ?
N1 Fe1 N4 . . . 104.60(4) ?
Fe1 P1 N2 . . . 101.48(4) ?
Fe1 P1 C6 . . . 117.19(4) ?
Fe1 P1 C12 . . . 125.48(4) ?
N2 P1 C6 . . . 104.80(5) ?
N2 P1 C12 . . . 101.07(5) ?
C6 P1 C12 . . . 103.73(6) ?
Fe1 P2 N3 . . . 101.30(4) ?
Fe1 P2 C19 . . . 115.82(4) ?
Fe1 P2 C25 . . . 126.63(4) ?
N3 P2 C19 . . . 103.46(5) ?
N3 P2 C25 . . . 99.92(5) ?
C19 P2 C25 . . . 105.74(5) ?
Fe1 P3 N5 . . . 102.78(3) ?
Fe1 P3 C37 . . . 119.59(4) ?
Fe1 P3 C43 . . . 122.13(4) ?
N5 P3 C37 . . . 105.70(5) ?
N5 P3 C43 . . . 105.29(5) ?
C37 P3 C43 . . . 99.74(5) ?
Fe1 N1 Cl1 . . . 53.24(2) ?
Fe1 N1 C1 . . . 120.55(8) ?
Fe1 N1 C5 . . . 120.76(7) ?
Cl1 N1 C1 . . . 105.27(6) ?
Cl1 N1 C5 . . . 103.29(6) ?
C1 N1 C5 . . . 117.99(9) ?
Cl1 N2 P1 . . . 62.46(3) ?
Cl1 N2 C1 . . . 71.79(6) ?
Cl1 N2 C18 . . . 133.24(7) ?
P1 N2 C1 . . . 118.89(8) ?
P1 N2 C18 . . . 122.43(8) ?
C1 N2 C18 . . . 118.23(9) ?
Cl1 N3 P2 . . . 63.06(3) ?
Cl1 N3 C5 . . . 70.64(6) ?
Cl1 N3 C31 . . . 138.72(7) ?
P2 N3 C5 . . . 119.14(8) ?
P2 N3 C31 . . . 121.85(8) ?
C5 N3 C31 . . . 118.96(9) ?
Fe1 N4 C32 . . . 117.95(7) ?
Fe1 N4 C36 . . . 125.68(7) ?
C32 N4 C36 . . . 116.34(9) ?
P3 N5 C32 . . . 117.91(7) ?
P3 N5 C49 . . . 124.87(8) ?
C32 N5 C49 . . . 117.20(9) ?
C36 N6 C50 . . . 123.65(10) ?
C36 N6 H1n . . . 115.2(11) ?
C50 N6 H1n . . . 120.5(11) ?
N1 C1 N2 . . . 116.32(9) ?
N1 C1 C2 . . . 122.11(11) ?
N2 C1 C2 . . . 121.58(11) ?
C1 C2 C3 . . . 118.33(11) ?
C1 C2 H21 . . . 120.84 ?
C3 C2 H21 . . . 120.84 ?
C2 C3 C4 . . . 120.74(10) ?
C2 C3 H31 . . . 119.63 ?
C4 C3 H31 . . . 119.63 ?
C3 C4 C5 . . . 118.27(11) ?
C3 C4 H41 . . . 120.87 ?
C5 C4 H41 . . . 120.87 ?
N1 C5 N3 . . . 115.82(9) ?
N1 C5 C4 . . . 122.42(11) ?
N3 C5 C4 . . . 121.75(11) ?
P1 C6 C7 . . . 123.25(9) ?
P1 C6 C11 . . . 118.28(9) ?
C7 C6 C11 . . . 118.42(11) ?
C6 C7 C8 . . . 120.08(11) ?
C6 C7 H71 . . . 119.96 ?
C8 C7 H71 . . . 119.96 ?
C7 C8 C9 . . . 120.79(12) ?
C7 C8 H81 . . . 119.6 ?
C9 C8 H81 . . . 119.6 ?
C8 C9 C10 . . . 119.78(12) ?
C8 C9 H91 . . . 120.11 ?
C10 C9 H91 . . . 120.11 ?
C9 C10 C11 . . . 119.60(12) ?
C9 C10 H101 . . . 120.2 ?
C11 C10 H101 . . . 120.2 ?
C6 C11 C10 . . . 121.31(12) ?
C6 C11 H111 . . . 119.35 ?
C10 C11 H111 . . . 119.35 ?
P1 C12 C13 . . . 118.44(10) ?
P1 C12 C17 . . . 122.52(9) ?
C13 C12 C17 . . . 119.03(11) ?
C12 C13 C14 . . . 120.10(13) ?
C12 C13 H131 . . . 119.95 ?
C14 C13 H131 . . . 119.95 ?
C13 C14 C15 . . . 120.54(13) ?
C13 C14 H141 . . . 119.73 ?
C15 C14 H141 . . . 119.73 ?
C14 C15 C16 . . . 119.83(13) ?
C14 C15 H151 . . . 120.08 ?
C16 C15 H151 . . . 120.08 ?
C15 C16 C17 . . . 120.31(15) ?
C15 C16 H161 . . . 119.84 ?
C17 C16 H161 . . . 119.84 ?
C12 C17 C16 . . . 120.17(12) ?
C12 C17 H171 . . . 119.91 ?
C16 C17 H171 . . . 119.91 ?
N2 C18 H181 . . . 109.47 ?
N2 C18 H182 . . . 109.47 ?
N2 C18 H183 . . . 109.47 ?
H181 C18 H182 . . . 109.47 ?
H181 C18 H183 . . . 109.47 ?
H182 C18 H183 . . . 109.47 ?
P2 C19 C20 . . . 120.33(8) ?
P2 C19 C24 . . . 120.51(9) ?
C20 C19 C24 . . . 118.66(10) ?
C19 C20 C21 . . . 120.42(11) ?
C19 C20 H201 . . . 119.79 ?
C21 C20 H201 . . . 119.79 ?
C20 C21 C22 . . . 120.19(12) ?
C20 C21 H211 . . . 119.91 ?
C22 C21 H211 . . . 119.91 ?
C21 C22 C23 . . . 120.08(12) ?
C21 C22 H221 . . . 119.96 ?
C23 C22 H221 . . . 119.96 ?
C22 C23 C24 . . . 119.89(12) ?
C22 C23 H231 . . . 120.06 ?
C24 C23 H231 . . . 120.05 ?
C19 C24 C23 . . . 120.74(11) ?
C19 C24 H241 . . . 119.63 ?
C23 C24 H241 . . . 119.63 ?
P2 C25 C26 . . . 117.29(9) ?
P2 C25 C30 . . . 123.68(8) ?
C26 C25 C30 . . . 119.03(11) ?
C25 C26 C27 . . . 120.32(12) ?
C25 C26 H261 . . . 119.84 ?
C27 C26 H261 . . . 119.84 ?
C26 C27 C28 . . . 120.47(11) ?
C26 C27 H271 . . . 119.77 ?
C28 C27 H271 . . . 119.77 ?
C27 C28 C29 . . . 119.23(12) ?
C27 C28 H281 . . . 120.38 ?
C29 C28 H281 . . . 120.38 ?
C28 C29 C30 . . . 120.88(12) ?
C28 C29 H291 . . . 119.56 ?
C30 C29 H291 . . . 119.56 ?
C25 C30 C29 . . . 120.04(11) ?
C25 C30 H301 . . . 119.98 ?
C29 C30 H301 . . . 119.98 ?
N3 C31 H311 . . . 109.47 ?
N3 C31 H312 . . . 109.47 ?
N3 C31 H313 . . . 109.47 ?
H311 C31 H312 . . . 109.47 ?
H311 C31 H313 . . . 109.47 ?
H312 C31 H313 . . . 109.47 ?
N4 C32 N5 . . . 117.55(9) ?
N4 C32 C33 . . . 123.19(10) ?
N5 C32 C33 . . . 119.25(10) ?
C32 C33 C34 . . . 118.37(11) ?
C32 C33 H331 . . . 120.82 ?
C34 C33 H331 . . . 120.82 ?
C33 C34 C35 . . . 120.54(11) ?
C33 C34 H341 . . . 119.73 ?
C35 C34 H341 . . . 119.73 ?
C34 C35 C36 . . . 118.53(11) ?
C34 C35 H351 . . . 120.73 ?
C36 C35 H351 . . . 120.73 ?
N4 C36 N6 . . . 117.95(9) ?
N4 C36 C35 . . . 123.01(10) ?
N6 C36 C35 . . . 119.03(10) ?
P3 C37 C38 . . . 121.99(9) ?
P3 C37 C42 . . . 119.35(9) ?
C38 C37 C42 . . . 118.66(11) ?
C37 C38 C39 . . . 120.34(11) ?
C37 C38 H381 . . . 119.83 ?
C39 C38 H381 . . . 119.83 ?
C38 C39 C40 . . . 120.57(12) ?
C38 C39 H391 . . . 119.72 ?
C40 C39 H391 . . . 119.72 ?
C39 C40 C41 . . . 119.77(13) ?
C39 C40 H401 . . . 120.11 ?
C41 C40 H401 . . . 120.12 ?
C40 C41 C42 . . . 120.04(11) ?
C40 C41 H411 . . . 119.98 ?
C42 C41 H411 . . . 119.98 ?
C37 C42 C41 . . . 120.55(11) ?
C37 C42 H421 . . . 119.73 ?
C41 C42 H421 . . . 119.73 ?
P3 C43 C44 . . . 122.91(9) ?
P3 C43 C48 . . . 118.99(9) ?
C44 C43 C48 . . . 118.10(11) ?
C43 C44 C45 . . . 120.84(12) ?
C43 C44 H441 . . . 119.58 ?
C45 C44 H441 . . . 119.58 ?
C44 C45 C46 . . . 120.31(14) ?
C44 C45 H451 . . . 119.85 ?
C46 C45 H451 . . . 119.84 ?
C45 C46 C47 . . . 119.64(14) ?
C45 C46 H461 . . . 120.18 ?
C47 C46 H461 . . . 120.18 ?
C46 C47 C48 . . . 120.40(13) ?
C46 C47 H471 . . . 119.8 ?
C48 C47 H471 . . . 119.8 ?
C43 C48 C47 . . . 120.68(12) ?
C43 C48 H481 . . . 119.66 ?
C47 C48 H481 . . . 119.66 ?
N5 C49 H491 . . . 109.47 ?
N5 C49 H492 . . . 109.47 ?
N5 C49 H493 . . . 109.47 ?
H491 C49 H492 . . . 109.47 ?
H491 C49 H493 . . . 109.47 ?
H492 C49 H493 . . . 109.47 ?
N6 C50 H501 . . . 109.47 ?
N6 C50 H502 . . . 109.47 ?
N6 C50 H503 . . . 109.47 ?
H501 C50 H502 . . . 109.47 ?
H501 C50 H503 . . . 109.47 ?
H502 C50 H503 . . . 109.47 ?
F1 B1 F2 . . . 109.20(11) ?
F1 B1 F3 . . . 109.36(11) ?
F1 B1 F4 . . . 110.42(11) ?
F2 B1 F3 . . . 109.61(12) ?
F2 B1 F4 . . . 109.93(11) ?
F3 B1 F4 . . . 108.30(11) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N6 H1n N1 . . . 0.850(16) 1.959(16) 2.8021(14) 171.1(16) ?
N6 H1n C1 . . . 0.850(16) 2.499(16) 3.2800(16) 153.1(16) ?
_database_code_depnum_ccdc_archive 'CCDC 1005382'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5b

# start Validation Reply Form
_vrf_PLAT602_5b                  
;
PROBLEM:     
PLAT602_ALERT_2_A VERY LARGE Solvent Accessible VOID(S) in Structure !
RESPONSE:
The title structure was obtained from methanol / diethyl ether. It is
a solvate with disordered solvent molecules. This solvent was SQUEEZED
with program PLATON. 
According to PLATON, the solvent accessible volume is 2562 A^3^ per unit
cell (36% of the unit cell volume) with an electron count of 305. It is 
estimated that there are at least 16 methanol molecules per unit cell
or 4 molecules per Fe complex, which may be O-H...Cl hydrogen bonded to the
the cloride anions. The solvent cavity forms a 3-dimensional infinte
structure between the Fe(PNP-Ph)2 complexes and the Cl anions. 
The solvent is not contained in chemical formula or quantities derived 
thereof.
;
# end Validation Reply Form



_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
5b.solv  --  [Fe(k³-P,N,P-PNP-Ph)₂](Cl)₂.solv
;
_chemical_name_common            
'5b.solv  [Fe(k3-P,N,P-PNP-Ph)2](Cl)2.solv   1610'
_chemical_formula_moiety         'C58 H50 Fe N6 P4, 2(Cl)'
_chemical_formula_sum            'C58 H50 Cl2 Fe N6 P4'
_chemical_formula_weight         1081.67

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I -4 2 d'
_symmetry_space_group_name_Hall  'I -4 2bw '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   15.1224(2)
_cell_length_b                   15.1224(2)
_cell_length_c                   30.8856(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7063.13(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9897
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      30.43

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2240
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_process_details   'program SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            31615
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         29.99
_reflns_number_total             5139
_reflns_number_gt                4943
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0450P)²+2.1416P] where P=(Fo²+2Fc²)/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, 2345 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.020(10)
_refine_ls_number_reflns         5139
_refine_ls_number_parameters     162
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0707
_refine_ls_wR_factor_gt          0.0692
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_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 0.5000 0.5000 0.5000 0.01227(7) Uani 1 4 d S . .
P1 P 0.406869(18) 0.615312(19) 0.507032(8) 0.01368(6) Uani 1 1 d . . .
N1 N 0.5000 0.5000 0.56334(4) 0.0129(2) Uani 1 2 d S . .
N2 N 0.40984(7) 0.62499(7) 0.56135(3) 0.01571(17) Uani 1 1 d . . .
H2N H 0.3828 0.6693 0.5742 0.019 Uiso 1 1 calc R . .
C1 C 0.45488(7) 0.56302(8) 0.58561(3) 0.0145(2) Uani 1 1 d . . .
C2 C 0.45337(8) 0.56457(8) 0.63084(4) 0.0178(2) Uani 1 1 d . . .
H2 H 0.4213 0.6087 0.6461 0.021 Uiso 1 1 calc R . .
C3 C 0.5000 0.5000 0.65274(5) 0.0201(3) Uani 1 2 d S . .
H3 H 0.5000 0.5000 0.6835 0.024 Uiso 1 2 calc SR . .
C4 C 0.28985(7) 0.62019(7) 0.49154(3) 0.0163(2) Uani 1 1 d . . .
C5 C 0.22420(9) 0.64699(9) 0.52049(4) 0.0206(2) Uani 1 1 d . . .
H5 H 0.2375 0.6536 0.5504 0.025 Uiso 1 1 calc R . .
C6 C 0.13894(9) 0.66401(9) 0.50533(5) 0.0259(3) Uani 1 1 d . . .
H6 H 0.0941 0.6818 0.5250 0.031 Uiso 1 1 calc R . .
C7 C 0.11930(9) 0.65506(10) 0.46161(5) 0.0285(3) Uani 1 1 d . . .
H7 H 0.0614 0.6677 0.4514 0.034 Uiso 1 1 calc R . .
C8 C 0.18419(9) 0.62772(9) 0.43282(4) 0.0252(3) Uani 1 1 d . . .
H8 H 0.1705 0.6210 0.4030 0.030 Uiso 1 1 calc R . .
C9 C 0.26916(9) 0.61017(8) 0.44761(4) 0.0203(2) Uani 1 1 d . . .
H9 H 0.3134 0.5913 0.4278 0.024 Uiso 1 1 calc R . .
C10 C 0.43016(8) 0.72429(8) 0.48418(4) 0.0175(2) Uani 1 1 d . . .
C11 C 0.41788(9) 0.80133(8) 0.50808(4) 0.0225(2) Uani 1 1 d . . .
H11 H 0.4058 0.7981 0.5382 0.027 Uiso 1 1 calc R . .
C12 C 0.42342(10) 0.88338(9) 0.48761(5) 0.0313(3) Uani 1 1 d . . .
H12 H 0.4159 0.9360 0.5040 0.038 Uiso 1 1 calc R . .
C13 C 0.43978(11) 0.88859(10) 0.44358(5) 0.0341(3) Uani 1 1 d . . .
H13 H 0.4423 0.9447 0.4298 0.041 Uiso 1 1 calc R . .
C14 C 0.45253(10) 0.81217(10) 0.41933(5) 0.0284(3) Uani 1 1 d . . .
H14 H 0.4648 0.8159 0.3892 0.034 Uiso 1 1 calc R . .
C15 C 0.44708(9) 0.73033(9) 0.43960(4) 0.0218(2) Uani 1 1 d . . .
H15 H 0.4549 0.6779 0.4231 0.026 Uiso 1 1 calc R . .
Cl1 Cl 0.30697(3) 0.7500 0.6250 0.02408(9) Uani 1 2 d S . .


_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 N1 1.9563(12) 3_566 ?
Fe1 N1 1.9563(12) . ?
Fe1 P1 2.2520(3) 4_656 ?
Fe1 P1 2.2520(3) 3_566 ?
Fe1 P1 2.2520(3) . ?
Fe1 P1 2.2520(3) 2_665 ?
P1 N2 1.6845(10) . ?
P1 C10 1.8271(12) . ?
P1 C4 1.8346(12) . ?
N1 C1 1.3591(13) . ?
N1 C1 1.3591(13) 2_665 ?
N2 C1 1.3797(15) . ?
N2 H2N 0.8800 . ?
C1 C2 1.3972(15) . ?
C2 C3 1.3814(14) . ?
C2 H2 0.9500 . ?
C3 C2 1.3814(14) 2_665 ?
C3 H3 0.9500 . ?
C4 C5 1.3960(17) . ?
C4 C9 1.4007(15) . ?
C5 C6 1.3956(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.389(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.387(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.3894(18) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.3917(17) . ?
C10 C15 1.4035(16) . ?
C11 C12 1.3951(19) . ?
C11 H11 0.9500 . ?
C12 C13 1.385(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.391(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.3894(18) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 180.0 3_566 . ?
N1 Fe1 P1 84.466(7) 3_566 4_656 ?
N1 Fe1 P1 95.534(7) . 4_656 ?
N1 Fe1 P1 84.466(7) 3_566 3_566 ?
N1 Fe1 P1 95.534(7) . 3_566 ?
P1 Fe1 P1 168.931(13) 4_656 3_566 ?
N1 Fe1 P1 95.534(7) 3_566 . ?
N1 Fe1 P1 84.466(7) . . ?
P1 Fe1 P1 90.533(1) 4_656 . ?
P1 Fe1 P1 90.533(1) 3_566 . ?
N1 Fe1 P1 95.535(7) 3_566 2_665 ?
N1 Fe1 P1 84.465(7) . 2_665 ?
P1 Fe1 P1 90.533(1) 4_656 2_665 ?
P1 Fe1 P1 90.533(1) 3_566 2_665 ?
P1 Fe1 P1 168.931(13) . 2_665 ?
N2 P1 C10 107.53(5) . . ?
N2 P1 C4 106.37(5) . . ?
C10 P1 C4 92.81(5) . . ?
N2 P1 Fe1 98.43(4) . . ?
C10 P1 Fe1 122.73(4) . . ?
C4 P1 Fe1 127.53(4) . . ?
C1 N1 C1 119.18(13) . 2_665 ?
C1 N1 Fe1 120.41(7) . . ?
C1 N1 Fe1 120.41(7) 2_665 . ?
C1 N2 P1 119.68(8) . . ?
C1 N2 H2N 120.2 . . ?
P1 N2 H2N 120.2 . . ?
N1 C1 N2 116.69(10) . . ?
N1 C1 C2 121.73(11) . . ?
N2 C1 C2 121.58(10) . . ?
C3 C2 C1 118.00(11) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C2 C3 C2 121.36(14) 2_665 . ?
C2 C3 H3 119.3 2_665 . ?
C2 C3 H3 119.3 . . ?
C5 C4 C9 119.53(11) . . ?
C5 C4 P1 122.05(9) . . ?
C9 C4 P1 117.62(9) . . ?
C6 C5 C4 119.72(11) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C7 C6 C5 120.37(13) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C8 C7 C6 120.05(12) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C9 120.03(12) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C8 C9 C4 120.29(12) . . ?
C8 C9 H9 119.9 . . ?
C4 C9 H9 119.9 . . ?
C11 C10 C15 119.36(11) . . ?
C11 C10 P1 121.63(9) . . ?
C15 C10 P1 118.22(9) . . ?
C10 C11 C12 119.75(12) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 120.43(14) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C12 C13 C14 120.44(13) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 119.29(13) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C10 120.72(13) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Fe1 P1 N2 -175.63(4) 3_566 . . . ?
N1 Fe1 P1 N2 4.37(4) . . . . ?
P1 Fe1 P1 N2 99.87(4) 4_656 . . . ?
P1 Fe1 P1 N2 -91.14(4) 3_566 . . . ?
P1 Fe1 P1 N2 4.37(4) 2_665 . . . ?
N1 Fe1 P1 C10 -58.42(4) 3_566 . . . ?
N1 Fe1 P1 C10 121.58(4) . . . . ?
P1 Fe1 P1 C10 -142.92(5) 4_656 . . . ?
P1 Fe1 P1 C10 26.07(4) 3_566 . . . ?
P1 Fe1 P1 C10 121.57(4) 2_665 . . . ?
N1 Fe1 P1 C4 66.12(5) 3_566 . . . ?
N1 Fe1 P1 C4 -113.88(5) . . . . ?
P1 Fe1 P1 C4 -18.37(4) 4_656 . . . ?
P1 Fe1 P1 C4 150.62(5) 3_566 . . . ?
P1 Fe1 P1 C4 -113.88(5) 2_665 . . . ?
P1 Fe1 N1 C1 -93.32(6) 4_656 . . . ?
P1 Fe1 N1 C1 86.68(6) 3_566 . . . ?
P1 Fe1 N1 C1 -3.32(6) . . . . ?
P1 Fe1 N1 C1 176.68(6) 2_665 . . . ?
P1 Fe1 N1 C1 86.68(6) 4_656 . . 2_665 ?
P1 Fe1 N1 C1 -93.32(6) 3_566 . . 2_665 ?
P1 Fe1 N1 C1 176.68(6) . . . 2_665 ?
P1 Fe1 N1 C1 -3.32(6) 2_665 . . 2_665 ?
C10 P1 N2 C1 -134.25(9) . . . . ?
C4 P1 N2 C1 127.33(9) . . . . ?
Fe1 P1 N2 C1 -5.94(10) . . . . ?
C1 N1 C1 N2 -179.61(12) 2_665 . . . ?
Fe1 N1 C1 N2 0.39(12) . . . . ?
C1 N1 C1 C2 -0.23(8) 2_665 . . . ?
Fe1 N1 C1 C2 179.77(8) . . . . ?
P1 N2 C1 N1 4.40(14) . . . . ?
P1 N2 C1 C2 -174.98(9) . . . . ?
N1 C1 C2 C3 0.46(16) . . . . ?
N2 C1 C2 C3 179.81(10) . . . . ?
C1 C2 C3 C2 -0.22(8) . . . 2_665 ?
N2 P1 C4 C5 12.64(11) . . . . ?
C10 P1 C4 C5 -96.55(11) . . . . ?
Fe1 P1 C4 C5 127.38(9) . . . . ?
N2 P1 C4 C9 -177.64(9) . . . . ?
C10 P1 C4 C9 73.16(10) . . . . ?
Fe1 P1 C4 C9 -62.91(10) . . . . ?
C9 C4 C5 C6 -0.38(19) . . . . ?
P1 C4 C5 C6 169.14(10) . . . . ?
C4 C5 C6 C7 -0.5(2) . . . . ?
C5 C6 C7 C8 1.0(2) . . . . ?
C6 C7 C8 C9 -0.7(2) . . . . ?
C7 C8 C9 C4 -0.2(2) . . . . ?
C5 C4 C9 C8 0.72(19) . . . . ?
P1 C4 C9 C8 -169.26(10) . . . . ?
N2 P1 C10 C11 -21.50(12) . . . . ?
C4 P1 C10 C11 86.65(11) . . . . ?
Fe1 P1 C10 C11 -134.19(9) . . . . ?
N2 P1 C10 C15 168.75(9) . . . . ?
C4 P1 C10 C15 -83.10(10) . . . . ?
Fe1 P1 C10 C15 56.06(11) . . . . ?
C15 C10 C11 C12 -0.66(19) . . . . ?
P1 C10 C11 C12 -170.29(10) . . . . ?
C10 C11 C12 C13 0.9(2) . . . . ?
C11 C12 C13 C14 -1.2(2) . . . . ?
C12 C13 C14 C15 1.2(2) . . . . ?
C13 C14 C15 C10 -0.9(2) . . . . ?
C11 C10 C15 C14 0.66(19) . . . . ?
P1 C10 C15 C14 170.64(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2N Cl1 0.88 2.29 3.1399(10) 161.0 .

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        29.99
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.056


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.033 -0.009 0.426 2562 305 ' '
_platon_squeeze_details          
;
The title structure was obtained from methanol / diethyl ether. It is
a solvate with disordered solvent molecules. This solvent was SQUEEZED
with program PLATON. 
According to PLATON, the solvent accessible volume is 2562 A³ per unit
cell (36% of the unit cell volume) with an electron count of 305. It is 
estimated that there are at least 16 methanol molecules per unit cell
or 4 molecules per Fe complex, which may be O-H...Cl hydrogen bonded to the
the cloride anions. The solvent cavity forms a 3-dimensional infinte
structure between the Fe(PNP-Ph)2 complexes and the Cl anions. 
The highest solvent denity peaks identified by procedure SQUEEZE were:
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.261 0.923 0.182 !       3.62 eA-3
C102 0.301 0.904 0.211 !       2.73 eA-3
C103 0.796 0.145 0.421 !       2.17 eA-3
C104 0.264 0.056 0.387 !       2.02 eA-3
C105 1.000 1.002 0.414 !       0.99 eA-3
C106 0.547 0.803 0.193 !       0.99 eA-3
C107 1.000 0.995 0.437 !       0.79 eA-3
;
_database_code_depnum_ccdc_archive 'CCDC 1005385'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5a


# start Validation Reply Form
_vrf_PLAT411_5a                  
;
PROBLEM: 
PLAT411_ALERT_2_A 
Short Inter H...H Contact  H68A .. H82B   ..   1.79 Ang.  
RESPONSE: 
Virtual H-H contact between two THF solvent molecules of
which one is disordered about an inversion (O21, C85, C86)
and appears therefore like a six-membered dioxane ring.
;
_vrf_DIFMX01_5a                  
;
PROBLEM: 
DIFMX01_ALERT_2_B  The maximum difference density is > 0.1*ZMAX*1.00
            _refine_diff_density_max given =      3.217
            Test value =      2.600
PLAT097_ALERT_2_B 
Large Reported Max.  (Positive) Residual Density       3.22 eA-3  
PLAT214_ALERT_2_B 
Atom C79     (Anion/Solvent) ADP max/min Ratio          5.1 prolat
PLAT341_ALERT_3_B 
Low Bond Precision on  C-C Bonds ...............     0.0157 Ang.  
PLAT360_ALERT_2_B S
hort  C(sp3)-C(sp3) Bond  C74    -   C75    ...       1.28 Ang.  

RESPONSE: 
The crystal structure is a solvent-rich solvate of a well ordered and
large Fe-complex and contains 6.5 THF 
molecules per asymmetric unit and Fe. Three of these THF molecules
(with O15, O16, O17) are well ordered. The rest of the THF molecules
is increasingly disordered and shows in part large anisotropic displacement
ellipsoids. In addition, one of the two CF3SO3 anions is orientation 
disordered and adopts two orientations in ca 65/35 proportion with F and O 
atoms for both approximately coinciding (therefore only S1 and C59
were split, but not O and F atoms). 
These features cause a number of checkCIF alerts like 
DIFMX01, PLAT097, PLAT214, PLAT341, PLAT360 and more.
;
_vrf_THETM01_5a                  
;
PROBLEM: 
THETM01_ALERT_3_B  The value of sine(theta_max)/wavelength is less than 0.575
            Calculated sin(theta_max)/wavelength =    0.5682
RESPONSE: 
As described above, the crystal structure is solvent-rich and scattered
weakly at higher Bragg angles in view of the comparatively thin plates 
that were available. Therefore a cutoff of theta 23.8 deg had to be used.
As far as the focus of this crystal structure determination, the Fe-complex
complex is concerned the crystal structure is very reasonable despite the
relatively large R-values.
;
# end Validation Reply Form


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
5a.6.5THF  --  [Fe(k³-PNP-bipol)₂](CF₃SO₃)₂.6.5THF
;
_chemical_name_common            
'5a*6.5THF  [Fe(k3-PNP-bipol)2](CF3SO3)2*6.5THF   1681'
_chemical_formula_moiety         
'C58 H42 Fe N6 O8 P4, 2(C F3 O3 S), 6.5(C4 H8 O)'
_chemical_formula_sum            'C86 H94 F6 Fe N6 O20.50 P4 S2'
_chemical_formula_weight         1897.52

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'
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'
S S 0.1246 0.1234 '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'

_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                   13.4039(8)
_cell_length_b                   16.9467(9)
_cell_length_c                   20.9385(13)
_cell_angle_alpha                78.058(4)
_cell_angle_beta                 80.833(4)
_cell_angle_gamma                68.818(3)
_cell_volume                     4320.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9989
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      23.71

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1976
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_process_details   'program SADABS'

_exptl_special_details           
; 
Plate crystals from THF / hexane. 
Crystals scattered weakly, therefore data collection 
limit below 50deg. 
The structure is highly solvated and contains 
seven independent THF molecules of which three well ordered ones 
are N-H...O hydrogen bonded to the Fe(PNP)2 complex. The remaing 
molecules display large displacement parameters as indication 
for disorder. The seventh THF molecule is arranged abot a centre 
of inversion and appears in molecular graphics as a six memebered 
ring. Moreover the OTF group 1 is orientation disordered adopting 
two orienations in ca 65/35 proportion with F and O atoms for 
both approximately coinciding. 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_reflns_number            41700
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         23.82
_reflns_number_total             12816
_reflns_number_gt                10115
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1205P)²+75.3870P] where P=(Fo²+2Fc²)/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         12816
_refine_ls_number_parameters     1141
_refine_ls_number_restraints     358
_refine_ls_R_factor_all          0.1353
_refine_ls_R_factor_gt           0.1130
_refine_ls_wR_factor_ref         0.3093
_refine_ls_wR_factor_gt          0.2895
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001

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 0.88909(9) 0.77772(7) 0.26085(5) 0.0100(3) Uani 1 1 d U . .
P1 P 0.90845(16) 0.79133(13) 0.15415(10) 0.0117(4) Uani 1 1 d U . .
P2 P 0.90799(16) 0.75281(12) 0.36552(10) 0.0106(4) Uani 1 1 d U . .
P3 P 0.87273(16) 0.91201(12) 0.25632(10) 0.0115(4) Uani 1 1 d U . .
P4 P 0.86713(16) 0.65464(13) 0.26862(10) 0.0117(4) Uani 1 1 d U . .
O1 O 0.8891(4) 0.8791(3) 0.1011(3) 0.0142(10) Uani 1 1 d U . .
O2 O 0.8484(4) 0.7462(3) 0.1214(3) 0.0139(10) Uani 1 1 d U . .
O3 O 0.8520(4) 0.8331(3) 0.4029(3) 0.0126(9) Uani 1 1 d U . .
O4 O 0.8816(4) 0.6799(3) 0.4216(3) 0.0136(10) Uani 1 1 d U . .
O5 O 0.9071(4) 0.9733(3) 0.1932(3) 0.0137(10) Uani 1 1 d U . .
O6 O 0.9213(5) 0.9365(3) 0.3111(3) 0.0154(10) Uani 1 1 d U . .
O7 O 0.9123(5) 0.6050(3) 0.2073(3) 0.0150(10) Uani 1 1 d U . .
O8 O 0.9023(4) 0.5746(3) 0.3273(3) 0.0136(10) Uani 1 1 d U . .
N1 N 1.0473(5) 0.7326(4) 0.2521(3) 0.0108(8) Uani 1 1 d U . .
N2 N 1.0408(5) 0.7489(4) 0.1404(3) 0.0131(11) Uani 1 1 d U . .
H2N H 1.0711 0.7435 0.1003 0.016 Uiso 1 1 calc R . .
N3 N 1.0402(5) 0.7190(4) 0.3656(3) 0.0124(11) Uani 1 1 d U . .
H3N H 1.0706 0.7076 0.4023 0.015 Uiso 1 1 calc R . .
N4 N 0.7310(5) 0.8219(4) 0.2708(3) 0.0125(9) Uani 1 1 d U . .
N5 N 0.7402(5) 0.9585(4) 0.2614(3) 0.0152(11) Uani 1 1 d U . .
H5N H 0.7107 1.0145 0.2586 0.018 Uiso 1 1 calc R . .
N6 N 0.7351(5) 0.6819(4) 0.2801(3) 0.0154(12) Uani 1 1 d U . .
H6N H 0.7041 0.6427 0.2868 0.019 Uiso 1 1 calc R . .
C1 C 1.1030(6) 0.7222(5) 0.1926(4) 0.0114(13) Uani 1 1 d U . .
C2 C 1.2138(7) 0.6920(6) 0.1853(4) 0.0212(17) Uani 1 1 d U . .
H2 H 1.2514 0.6878 0.1429 0.025 Uiso 1 1 calc R . .
C3 C 1.2688(7) 0.6680(6) 0.2399(4) 0.0218(17) Uani 1 1 d U . .
H3 H 1.3451 0.6459 0.2355 0.026 Uiso 1 1 calc R . .
C4 C 1.2137(7) 0.6757(5) 0.3020(4) 0.0185(16) Uani 1 1 d U . .
H4 H 1.2512 0.6588 0.3402 0.022 Uiso 1 1 calc R . .
C5 C 1.1015(6) 0.7092(5) 0.3060(4) 0.0122(13) Uani 1 1 d U . .
C6 C 0.7921(6) 0.9250(5) 0.0724(4) 0.0143(13) Uani 1 1 d U . .
C7 C 0.7367(7) 1.0062(5) 0.0889(4) 0.0183(15) Uani 1 1 d U . .
H7 H 0.7601 1.0258 0.1212 0.022 Uiso 1 1 calc R . .
C8 C 0.6472(7) 1.0574(5) 0.0571(4) 0.0205(16) Uani 1 1 d U . .
H8 H 0.6093 1.1137 0.0666 0.025 Uiso 1 1 calc R . .
C9 C 0.6120(7) 1.0273(6) 0.0112(4) 0.0231(17) Uani 1 1 d U . .
H9 H 0.5502 1.0628 -0.0106 0.028 Uiso 1 1 calc R . .
C10 C 0.6672(7) 0.9457(5) -0.0027(4) 0.0198(16) Uani 1 1 d U . .
H10 H 0.6419 0.9249 -0.0334 0.024 Uiso 1 1 calc R . .
C11 C 0.7600(7) 0.8929(5) 0.0279(4) 0.0163(14) Uani 1 1 d U . .
C12 C 0.8225(7) 0.8072(5) 0.0087(4) 0.0164(14) Uani 1 1 d U . .
C13 C 0.8357(7) 0.7935(6) -0.0557(4) 0.0209(16) Uani 1 1 d U . .
H13 H 0.8038 0.8399 -0.0886 0.025 Uiso 1 1 calc R . .
C14 C 0.8946(7) 0.7136(6) -0.0731(4) 0.0238(17) Uani 1 1 d U . .
H14 H 0.9027 0.7055 -0.1174 0.029 Uiso 1 1 calc R . .
C15 C 0.9412(8) 0.6459(6) -0.0252(5) 0.0268(19) Uani 1 1 d U . .
H15 H 0.9815 0.5911 -0.0368 0.032 Uiso 1 1 calc R . .
C16 C 0.9295(7) 0.6578(5) 0.0394(4) 0.0203(16) Uani 1 1 d U . .
H16 H 0.9623 0.6118 0.0723 0.024 Uiso 1 1 calc R . .
C17 C 0.8695(6) 0.7373(5) 0.0551(4) 0.0139(13) Uani 1 1 d U . .
C18 C 0.8689(7) 0.8301(5) 0.4684(4) 0.0150(13) Uani 1 1 d U . .
C19 C 0.9354(7) 0.8706(5) 0.4789(4) 0.0187(15) Uani 1 1 d U . .
H19 H 0.9741 0.8950 0.4432 0.022 Uiso 1 1 calc R . .
C20 C 0.9447(8) 0.8750(6) 0.5431(4) 0.0234(17) Uani 1 1 d U . .
H20 H 0.9912 0.9017 0.5519 0.028 Uiso 1 1 calc R . .
C21 C 0.8861(7) 0.8406(6) 0.5940(4) 0.0221(16) Uani 1 1 d U . .
H21 H 0.8912 0.8449 0.6378 0.026 Uiso 1 1 calc R . .
C22 C 0.8195(7) 0.7995(5) 0.5818(4) 0.0189(15) Uani 1 1 d U . .
H22 H 0.7791 0.7765 0.6173 0.023 Uiso 1 1 calc R . .
C23 C 0.8117(7) 0.7918(5) 0.5175(4) 0.0154(13) Uani 1 1 d U . .
C24 C 0.7453(7) 0.7456(5) 0.5036(4) 0.0164(13) Uani 1 1 d U . .
C25 C 0.6462(7) 0.7517(6) 0.5387(4) 0.0220(16) Uani 1 1 d U . .
H25 H 0.6207 0.7875 0.5714 0.026 Uiso 1 1 calc R . .
C26 C 0.5835(8) 0.7074(7) 0.5276(5) 0.0285(18) Uani 1 1 d U . .
H26 H 0.5157 0.7136 0.5518 0.034 Uiso 1 1 calc R . .
C27 C 0.6214(7) 0.6535(6) 0.4803(4) 0.0261(18) Uani 1 1 d U . .
H27 H 0.5800 0.6216 0.4729 0.031 Uiso 1 1 calc R . .
C28 C 0.7191(7) 0.6468(6) 0.4444(4) 0.0204(15) Uani 1 1 d U . .
H28 H 0.7448 0.6108 0.4117 0.024 Uiso 1 1 calc R . .
C29 C 0.7795(6) 0.6929(5) 0.4562(4) 0.0140(13) Uani 1 1 d U . .
C30 C 0.6767(6) 0.9073(5) 0.2703(4) 0.0162(15) Uani 1 1 d U . .
C31 C 0.5654(7) 0.9406(6) 0.2773(5) 0.0238(18) Uani 1 1 d U . .
H31 H 0.5287 1.0005 0.2756 0.029 Uiso 1 1 calc R . .
C32 C 0.5097(7) 0.8841(6) 0.2868(5) 0.028(2) Uani 1 1 d U . .
H32 H 0.4335 0.9052 0.2933 0.034 Uiso 1 1 calc R . .
C33 C 0.5631(7) 0.7972(6) 0.2872(5) 0.0235(18) Uani 1 1 d U . .
H33 H 0.5245 0.7586 0.2930 0.028 Uiso 1 1 calc R . .
C34 C 0.6738(6) 0.7682(5) 0.2790(4) 0.0151(14) Uani 1 1 d U . .
C35 C 1.0136(6) 0.9736(5) 0.1830(4) 0.0136(13) Uani 1 1 d U . .
C36 C 1.0794(7) 0.9363(5) 0.1309(4) 0.0189(15) Uani 1 1 d U . .
H36 H 1.0539 0.9096 0.1045 0.023 Uiso 1 1 calc R . .
C37 C 1.1832(8) 0.9390(6) 0.1184(4) 0.0249(18) Uani 1 1 d U . .
H37 H 1.2303 0.9121 0.0842 0.030 Uiso 1 1 calc R . .
C38 C 1.2181(7) 0.9806(6) 0.1556(5) 0.0248(17) Uani 1 1 d U . .
H38 H 1.2893 0.9821 0.1468 0.030 Uiso 1 1 calc R . .
C39 C 1.1513(7) 1.0201(6) 0.2053(4) 0.0205(16) Uani 1 1 d U . .
H39 H 1.1763 1.0490 0.2301 0.025 Uiso 1 1 calc R . .
C40 C 1.0463(7) 1.0181(5) 0.2195(4) 0.0168(14) Uani 1 1 d U . .
C41 C 0.9707(7) 1.0616(5) 0.2712(4) 0.0144(13) Uani 1 1 d U . .
C42 C 0.9597(7) 1.1450(5) 0.2781(4) 0.0164(15) Uani 1 1 d U . .
H42 H 1.0029 1.1740 0.2498 0.020 Uiso 1 1 calc R . .
C43 C 0.8878(7) 1.1848(6) 0.3250(4) 0.0209(16) Uani 1 1 d U . .
H43 H 0.8806 1.2416 0.3286 0.025 Uiso 1 1 calc R . .
C44 C 0.8244(7) 1.1437(5) 0.3679(4) 0.0200(16) Uani 1 1 d U . .
H44 H 0.7748 1.1722 0.4005 0.024 Uiso 1 1 calc R . .
C45 C 0.8342(7) 1.0602(5) 0.3627(4) 0.0171(15) Uani 1 1 d U . .
H45 H 0.7920 1.0309 0.3914 0.021 Uiso 1 1 calc R . .
C46 C 0.9073(6) 1.0221(5) 0.3144(4) 0.0141(13) Uani 1 1 d U . .
C47 C 0.8981(7) 0.5271(5) 0.2061(4) 0.0172(15) Uani 1 1 d U . .
C48 C 0.8251(7) 0.5270(5) 0.1672(4) 0.0195(16) Uani 1 1 d U . .
H48 H 0.7805 0.5797 0.1449 0.023 Uiso 1 1 calc R . .
C49 C 0.8159(8) 0.4503(6) 0.1600(4) 0.0225(17) Uani 1 1 d U . .
H49 H 0.7652 0.4493 0.1336 0.027 Uiso 1 1 calc R . .
C50 C 0.8841(8) 0.3749(6) 0.1933(4) 0.0222(17) Uani 1 1 d U . .
H50 H 0.8792 0.3216 0.1891 0.027 Uiso 1 1 calc R . .
C51 C 0.9579(7) 0.3748(5) 0.2318(4) 0.0189(15) Uani 1 1 d U . .
H51 H 1.0042 0.3220 0.2529 0.023 Uiso 1 1 calc R . .
C52 C 0.9650(7) 0.4521(5) 0.2402(4) 0.0160(14) Uani 1 1 d U . .
C53 C 1.0397(7) 0.4554(5) 0.2840(4) 0.0162(14) Uani 1 1 d U . .
C54 C 1.1441(7) 0.3946(5) 0.2869(4) 0.0185(15) Uani 1 1 d U . .
H54 H 1.1683 0.3521 0.2592 0.022 Uiso 1 1 calc R . .
C55 C 1.2121(7) 0.3964(6) 0.3299(4) 0.0220(16) Uani 1 1 d U . .
H55 H 1.2833 0.3566 0.3303 0.026 Uiso 1 1 calc R . .
C56 C 1.1764(7) 0.4557(5) 0.3718(4) 0.0207(16) Uani 1 1 d U . .
H56 H 1.2227 0.4557 0.4018 0.025 Uiso 1 1 calc R . .
C57 C 1.0739(7) 0.5152(5) 0.3705(4) 0.0164(14) Uani 1 1 d U . .
H57 H 1.0487 0.5554 0.4001 0.020 Uiso 1 1 calc R . .
C58 C 1.0080(7) 0.5153(5) 0.3254(4) 0.0151(13) Uani 1 1 d U . .
S1 S 0.6031(3) 0.5092(3) 0.3031(2) 0.0328(13) Uani 0.624(10) 1 d PDU A 1
O9T O 0.6587(7) 0.5496(5) 0.3326(4) 0.051(2) Uani 1 1 d DU A 1
O10T O 0.5479(8) 0.5561(9) 0.2464(5) 0.089(3) Uani 1 1 d DU A 1
O11T O 0.6398(10) 0.4200(6) 0.3008(6) 0.092(4) Uani 1 1 d DU A 1
C59T C 0.4968(14) 0.5088(11) 0.3682(9) 0.037(4) Uiso 0.624(10) 1 d PU A 1
F1 F 0.4233(7) 0.4834(7) 0.3473(6) 0.110(3) Uani 1 1 d U A 1
F2 F 0.5276(8) 0.4706(10) 0.4226(5) 0.132(4) Uani 1 1 d U A 1
F3 F 0.4448(7) 0.6006(8) 0.3733(7) 0.135(4) Uani 1 1 d U A 1
S1' S 0.5378(8) 0.5633(7) 0.3482(5) 0.056(4) Uiso 0.350(14) 1 d PU B 2
C59' C 0.531(4) 0.484(3) 0.305(2) 0.071(13) Uiso 0.350(14) 1 d PU B 2
S2 S 0.30172(17) 0.16597(13) 0.24239(11) 0.0210(5) Uani 1 1 d DU . .
O12T O 0.3317(6) 0.0790(4) 0.2759(4) 0.0463(19) Uani 1 1 d DU . .
O13T O 0.1960(5) 0.2002(4) 0.2209(3) 0.0276(13) Uani 1 1 d DU . .
O14T O 0.3310(5) 0.2222(5) 0.2728(4) 0.0373(16) Uani 1 1 d DU . .
C60T C 0.3922(8) 0.1578(8) 0.1678(5) 0.0366(14) Uani 1 1 d U . .
F4 F 0.3856(6) 0.0979(6) 0.1373(4) 0.067(2) Uani 1 1 d U . .
F5 F 0.4938(4) 0.1345(5) 0.1809(3) 0.0426(14) Uani 1 1 d U . .
F6 F 0.3699(7) 0.2307(6) 0.1267(3) 0.075(2) Uani 1 1 d U . .
O15 O 1.1411(5) 0.7989(4) 0.0182(3) 0.0275(13) Uani 1 1 d U . .
C61 C 1.0778(8) 0.8604(6) -0.0304(4) 0.0263(18) Uani 1 1 d U . .
H61A H 1.0933 0.9146 -0.0376 0.032 Uiso 1 1 calc R . .
H61B H 1.0004 0.8727 -0.0164 0.032 Uiso 1 1 calc R . .
C62 C 1.1083(8) 0.8209(6) -0.0936(5) 0.031(2) Uani 1 1 d U . .
H62A H 1.0442 0.8185 -0.1099 0.037 Uiso 1 1 calc R . .
H62B H 1.1434 0.8541 -0.1284 0.037 Uiso 1 1 calc R . .
C63 C 1.1865(8) 0.7307(6) -0.0722(5) 0.031(2) Uani 1 1 d U . .
H63A H 1.1486 0.6885 -0.0591 0.037 Uiso 1 1 calc R . .
H63B H 1.2438 0.7120 -0.1076 0.037 Uiso 1 1 calc R . .
C64 C 1.2310(8) 0.7420(6) -0.0149(5) 0.0290(18) Uani 1 1 d U . .
H64A H 1.2605 0.6865 0.0140 0.035 Uiso 1 1 calc R . .
H64B H 1.2884 0.7673 -0.0297 0.035 Uiso 1 1 calc R . .
O16 O 1.1486(5) 0.6173(4) 0.4722(3) 0.0212(12) Uani 1 1 d U . .
C65 C 1.0855(8) 0.5951(7) 0.5308(4) 0.0278(18) Uani 1 1 d U . .
H65A H 1.0986 0.5326 0.5395 0.033 Uiso 1 1 calc R . .
H65B H 1.0079 0.6259 0.5264 0.033 Uiso 1 1 calc R . .
C66 C 1.1214(8) 0.6221(6) 0.5864(5) 0.0303(19) Uani 1 1 d U . .
H66A H 1.0597 0.6630 0.6088 0.036 Uiso 1 1 calc R . .
H66B H 1.1549 0.5716 0.6191 0.036 Uiso 1 1 calc R . .
C67 C 1.2025(9) 0.6643(7) 0.5525(5) 0.033(2) Uani 1 1 d U . .
H67A H 1.1679 0.7272 0.5409 0.039 Uiso 1 1 calc R . .
H67B H 1.2613 0.6521 0.5802 0.039 Uiso 1 1 calc R . .
C68 C 1.2426(8) 0.6226(7) 0.4924(5) 0.0277(19) Uani 1 1 d U . .
H68A H 1.2752 0.6578 0.4578 0.033 Uiso 1 1 calc R . .
H68B H 1.2966 0.5648 0.5027 0.033 Uiso 1 1 calc R . .
O17 O 0.6429(5) 1.1303(4) 0.2702(3) 0.0274(14) Uani 1 1 d U . .
C69 C 0.5677(8) 1.1709(6) 0.3206(5) 0.0303(19) Uani 1 1 d U . .
H69A H 0.5965 1.1470 0.3638 0.036 Uiso 1 1 calc R . .
H69B H 0.4989 1.1609 0.3222 0.036 Uiso 1 1 calc R . .
C70 C 0.5504(9) 1.2642(7) 0.3046(6) 0.040(2) Uani 1 1 d U . .
H70A H 0.4753 1.2984 0.3175 0.048 Uiso 1 1 calc R . .
H70B H 0.5993 1.2791 0.3270 0.048 Uiso 1 1 calc R . .
C71 C 0.5751(11) 1.2792(7) 0.2323(6) 0.046(3) Uani 1 1 d U . .
H71A H 0.5996 1.3292 0.2179 0.056 Uiso 1 1 calc R . .
H71B H 0.5119 1.2883 0.2092 0.056 Uiso 1 1 calc R . .
C72 C 0.6657(9) 1.1953(6) 0.2207(5) 0.035(2) Uani 1 1 d U . .
H72A H 0.6662 1.1831 0.1764 0.042 Uiso 1 1 calc R . .
H72B H 0.7365 1.1987 0.2250 0.042 Uiso 1 1 calc R . .
O18 O 0.4684(10) 0.7679(12) 0.1367(7) 0.130(6) Uani 1 1 d U . .
C73 C 0.5803(11) 0.7546(11) 0.1154(8) 0.068(4) Uani 1 1 d U . .
H73A H 0.6265 0.7175 0.1501 0.081 Uiso 1 1 calc R . .
H73B H 0.5935 0.8099 0.1038 0.081 Uiso 1 1 calc R . .
C74 C 0.6017(13) 0.7113(17) 0.0559(10) 0.116(8) Uani 1 1 d U . .
H74A H 0.6249 0.7468 0.0168 0.139 Uiso 1 1 calc R . .
H74B H 0.6590 0.6546 0.0629 0.139 Uiso 1 1 calc R . .
C75 C 0.5137(16) 0.703(3) 0.0477(18) 0.25(2) Uani 1 1 d U . .
H75A H 0.5244 0.6406 0.0539 0.300 Uiso 1 1 calc R . .
H75B H 0.4965 0.7274 0.0020 0.300 Uiso 1 1 calc R . .
C76 C 0.4285(12) 0.7405(14) 0.0892(8) 0.090(6) Uani 1 1 d U . .
H76A H 0.3921 0.6992 0.1111 0.108 Uiso 1 1 calc R . .
H76B H 0.3759 0.7902 0.0645 0.108 Uiso 1 1 calc R . .
O19 O 0.3110(14) 0.4587(15) 0.1542(9) 0.169(8) Uani 1 1 d U . .
C77 C 0.380(2) 0.484(3) 0.099(2) 0.230(19) Uani 1 1 d U . .
H77A H 0.3990 0.5320 0.1079 0.276 Uiso 1 1 calc R . .
H77B H 0.4474 0.4355 0.0933 0.276 Uiso 1 1 calc R . .
C78 C 0.329(2) 0.511(2) 0.0406(16) 0.182(14) Uani 1 1 d U . .
H78A H 0.3412 0.5634 0.0158 0.218 Uiso 1 1 calc R . .
H78B H 0.3584 0.4652 0.0128 0.218 Uiso 1 1 calc R . .
C79 C 0.225(2) 0.525(3) 0.0579(16) 0.26(3) Uani 1 1 d U . .
H79A H 0.1967 0.5016 0.0284 0.310 Uiso 1 1 calc R . .
H79B H 0.1867 0.5879 0.0527 0.310 Uiso 1 1 calc R . .
C80 C 0.2061(19) 0.4881(19) 0.1232(11) 0.136(10) Uani 1 1 d U . .
H80A H 0.1825 0.4388 0.1245 0.164 Uiso 1 1 calc R . .
H80B H 0.1494 0.5306 0.1472 0.164 Uiso 1 1 calc R . .
O20 O 0.2032(11) 0.9367(7) 0.3813(5) 0.092(4) Uani 1 1 d U . .
C81 C 0.2235(13) 0.8568(9) 0.3515(9) 0.075(4) Uani 1 1 d U . .
H81A H 0.1590 0.8394 0.3597 0.090 Uiso 1 1 calc R . .
H81B H 0.2425 0.8674 0.3036 0.090 Uiso 1 1 calc R . .
C82 C 0.3032(12) 0.7979(9) 0.3804(7) 0.058(3) Uani 1 1 d U . .
H82A H 0.3658 0.7838 0.3473 0.069 Uiso 1 1 calc R . .
H82B H 0.2835 0.7456 0.3953 0.069 Uiso 1 1 calc R . .
C83 C 0.3351(11) 0.8159(8) 0.4325(6) 0.053(2) Uani 1 1 d U . .
H83A H 0.4046 0.8260 0.4209 0.064 Uiso 1 1 calc R . .
H83B H 0.3425 0.7686 0.4702 0.064 Uiso 1 1 calc R . .
C84 C 0.2297(10) 0.9111(10) 0.4509(7) 0.063(3) Uani 1 1 d U . .
H84A H 0.1707 0.8997 0.4819 0.076 Uiso 1 1 calc R . .
H84B H 0.2553 0.9517 0.4657 0.076 Uiso 1 1 calc R . .
O21 O 0.4020(18) 0.9764(15) 0.5246(8) 0.121(9) Uani 0.73(4) 1 d PU . .
C85 C 0.4636(14) 0.9857(12) 0.4562(11) 0.091(5) Uani 1 1 d U . .
C86 C 0.5781(16) 0.9804(13) 0.4422(18) 0.135(9) Uani 1 1 d U . .


_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 N4 1.967(7) . ?
Fe1 N1 1.969(6) . ?
Fe1 P4 2.180(2) . ?
Fe1 P1 2.181(2) . ?
Fe1 P2 2.182(2) . ?
Fe1 P3 2.189(2) . ?
P1 O2 1.595(6) . ?
P1 O1 1.626(6) . ?
P1 N2 1.657(7) . ?
P2 O3 1.595(5) . ?
P2 O4 1.617(5) . ?
P2 N3 1.655(7) . ?
P3 O6 1.594(6) . ?
P3 O5 1.618(5) . ?
P3 N5 1.659(7) . ?
P4 O7 1.598(6) . ?
P4 O8 1.614(6) . ?
P4 N6 1.650(7) . ?
O1 C6 1.408(10) . ?
O2 C17 1.400(10) . ?
O3 C18 1.413(10) . ?
O4 C29 1.406(10) . ?
O5 C35 1.411(10) . ?
O6 C46 1.409(9) . ?
O7 C47 1.407(10) . ?
O8 C58 1.410(10) . ?
N1 C5 1.351(10) . ?
N1 C1 1.356(10) . ?
N2 C1 1.381(10) . ?
N3 C5 1.386(10) . ?
N4 C34 1.358(10) . ?
N4 C30 1.363(10) . ?
N5 C30 1.388(11) . ?
N6 C34 1.392(10) . ?
C1 C2 1.379(12) . ?
C2 C3 1.370(13) . ?
C3 C4 1.395(12) . ?
C4 C5 1.398(11) . ?
C6 C11 1.362(12) . ?
C6 C7 1.393(12) . ?
C7 C8 1.379(12) . ?
C8 C9 1.389(13) . ?
C9 C10 1.379(13) . ?
C10 C11 1.404(12) . ?
C11 C12 1.493(12) . ?
C12 C13 1.386(12) . ?
C12 C17 1.387(12) . ?
C13 C14 1.389(13) . ?
C14 C15 1.384(13) . ?
C15 C16 1.385(13) . ?
C16 C17 1.374(12) . ?
C18 C19 1.370(12) . ?
C18 C23 1.378(12) . ?
C19 C20 1.390(12) . ?
C20 C21 1.378(13) . ?
C21 C22 1.394(13) . ?
C22 C23 1.403(12) . ?
C23 C24 1.474(12) . ?
C24 C29 1.385(12) . ?
C24 C25 1.391(12) . ?
C25 C26 1.383(13) . ?
C26 C27 1.396(14) . ?
C27 C28 1.382(13) . ?
C28 C29 1.389(12) . ?
C30 C31 1.385(12) . ?
C31 C32 1.380(13) . ?
C32 C33 1.385(13) . ?
C33 C34 1.378(12) . ?
C35 C40 1.388(12) . ?
C35 C36 1.395(12) . ?
C36 C37 1.390(13) . ?
C37 C38 1.381(13) . ?
C38 C39 1.374(13) . ?
C39 C40 1.403(12) . ?
C40 C41 1.478(12) . ?
C41 C46 1.381(12) . ?
C41 C42 1.403(11) . ?
C42 C43 1.360(12) . ?
C43 C44 1.392(13) . ?
C44 C45 1.398(12) . ?
C45 C46 1.376(12) . ?
C47 C48 1.369(12) . ?
C47 C52 1.391(12) . ?
C48 C49 1.389(12) . ?
C49 C50 1.394(13) . ?
C50 C51 1.372(13) . ?
C51 C52 1.395(12) . ?
C52 C53 1.484(12) . ?
C53 C58 1.377(12) . ?
C53 C54 1.408(12) . ?
C54 C55 1.391(13) . ?
C55 C56 1.375(13) . ?
C56 C57 1.380(12) . ?
C57 C58 1.391(12) . ?
S1 O11T 1.418(9) . ?
S1 O10T 1.433(9) . ?
S1 O9T 1.449(8) . ?
S1 C59T 1.809(18) . ?
C59T F2 1.24(2) . ?
C59T F1 1.37(2) . ?
C59T F3 1.48(2) . ?
S1' C59' 1.80(5) . ?
S2 O13T 1.431(6) . ?
S2 O12T 1.435(7) . ?
S2 O14T 1.438(7) . ?
S2 C60T 1.814(10) . ?
C60T F6 1.316(14) . ?
C60T F5 1.330(12) . ?
C60T F4 1.341(13) . ?
O15 C64 1.426(11) . ?
O15 C61 1.428(11) . ?
C61 C62 1.537(13) . ?
C62 C63 1.532(14) . ?
C63 C64 1.496(14) . ?
O16 C68 1.429(11) . ?
O16 C65 1.441(11) . ?
C65 C66 1.534(14) . ?
C66 C67 1.518(14) . ?
C67 C68 1.501(14) . ?
O17 C72 1.432(11) . ?
O17 C69 1.436(11) . ?
C69 C70 1.486(14) . ?
C70 C71 1.486(16) . ?
C71 C72 1.536(15) . ?
O18 C76 1.43(2) . ?
O18 C73 1.443(18) . ?
C73 C74 1.51(2) . ?
C74 C75 1.28(3) . ?
C75 C76 1.36(2) . ?
O19 C77 1.46(3) . ?
O19 C80 1.51(3) . ?
C77 C78 1.40(4) . ?
C78 C79 1.33(3) . ?
C79 C80 1.41(3) . ?
O20 C84 1.493(17) . ?
O20 C81 1.526(18) . ?
C81 C82 1.301(19) . ?
C82 C83 1.360(17) . ?
C83 C84 1.78(2) . ?
O21 C86 1.23(3) 2_676 ?
O21 C85 1.54(3) . ?
C85 C86 1.49(3) . ?
C86 O21 1.23(3) 2_676 ?

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
N4 Fe1 N1 179.2(3) . . ?
N4 Fe1 P4 83.5(2) . . ?
N1 Fe1 P4 96.14(19) . . ?
N4 Fe1 P1 97.0(2) . . ?
N1 Fe1 P1 83.73(19) . . ?
P4 Fe1 P1 90.70(8) . . ?
N4 Fe1 P2 95.5(2) . . ?
N1 Fe1 P2 83.73(19) . . ?
P4 Fe1 P2 90.48(8) . . ?
P1 Fe1 P2 167.47(9) . . ?
N4 Fe1 P3 83.9(2) . . ?
N1 Fe1 P3 96.39(19) . . ?
P4 Fe1 P3 167.45(9) . . ?
P1 Fe1 P3 91.29(8) . . ?
P2 Fe1 P3 90.27(8) . . ?
O2 P1 O1 98.7(3) . . ?
O2 P1 N2 111.6(3) . . ?
O1 P1 N2 98.8(3) . . ?
O2 P1 Fe1 117.2(2) . . ?
O1 P1 Fe1 128.0(2) . . ?
N2 P1 Fe1 101.1(2) . . ?
O3 P2 O4 98.7(3) . . ?
O3 P2 N3 111.2(3) . . ?
O4 P2 N3 99.5(3) . . ?
O3 P2 Fe1 115.7(2) . . ?
O4 P2 Fe1 128.7(2) . . ?
N3 P2 Fe1 101.7(2) . . ?
O6 P3 O5 98.7(3) . . ?
O6 P3 N5 110.0(3) . . ?
O5 P3 N5 100.5(3) . . ?
O6 P3 Fe1 118.7(2) . . ?
O5 P3 Fe1 126.0(2) . . ?
N5 P3 Fe1 101.2(2) . . ?
O7 P4 O8 99.4(3) . . ?
O7 P4 N6 110.2(3) . . ?
O8 P4 N6 100.7(3) . . ?
O7 P4 Fe1 117.3(2) . . ?
O8 P4 Fe1 125.8(2) . . ?
N6 P4 Fe1 101.8(3) . . ?
C6 O1 P1 124.0(5) . . ?
C17 O2 P1 122.3(5) . . ?
C18 O3 P2 122.3(5) . . ?
C29 O4 P2 122.3(5) . . ?
C35 O5 P3 119.3(5) . . ?
C46 O6 P3 122.2(5) . . ?
C47 O7 P4 121.9(5) . . ?
C58 O8 P4 120.3(5) . . ?
C5 N1 C1 119.3(7) . . ?
C5 N1 Fe1 120.0(5) . . ?
C1 N1 Fe1 120.7(5) . . ?
C1 N2 P1 119.2(5) . . ?
C5 N3 P2 117.7(5) . . ?
C34 N4 C30 118.6(7) . . ?
C34 N4 Fe1 120.9(5) . . ?
C30 N4 Fe1 120.5(5) . . ?
C30 N5 P3 118.8(5) . . ?
C34 N6 P4 118.5(6) . . ?
N1 C1 C2 121.7(7) . . ?
N1 C1 N2 115.1(7) . . ?
C2 C1 N2 123.1(7) . . ?
C3 C2 C1 119.0(8) . . ?
C2 C3 C4 120.6(8) . . ?
C3 C4 C5 117.7(8) . . ?
N1 C5 N3 116.7(7) . . ?
N1 C5 C4 121.7(7) . . ?
N3 C5 C4 121.6(7) . . ?
C11 C6 C7 123.1(8) . . ?
C11 C6 O1 120.8(7) . . ?
C7 C6 O1 115.9(7) . . ?
C8 C7 C6 118.3(8) . . ?
C7 C8 C9 120.4(8) . . ?
C10 C9 C8 119.7(8) . . ?
C9 C10 C11 121.1(8) . . ?
C6 C11 C10 117.3(8) . . ?
C6 C11 C12 122.6(8) . . ?
C10 C11 C12 120.0(8) . . ?
C13 C12 C17 117.1(8) . . ?
C13 C12 C11 122.0(8) . . ?
C17 C12 C11 120.9(7) . . ?
C12 C13 C14 121.5(8) . . ?
C15 C14 C13 119.4(8) . . ?
C14 C15 C16 120.3(8) . . ?
C17 C16 C15 118.8(8) . . ?
C16 C17 C12 122.9(8) . . ?
C16 C17 O2 118.2(7) . . ?
C12 C17 O2 118.7(7) . . ?
C19 C18 C23 124.4(8) . . ?
C19 C18 O3 117.9(7) . . ?
C23 C18 O3 117.6(7) . . ?
C18 C19 C20 118.3(8) . . ?
C21 C20 C19 119.7(8) . . ?
C20 C21 C22 120.7(8) . . ?
C21 C22 C23 120.5(8) . . ?
C18 C23 C22 116.3(8) . . ?
C18 C23 C24 122.1(7) . . ?
C22 C23 C24 121.5(8) . . ?
C29 C24 C25 117.1(8) . . ?
C29 C24 C23 121.7(7) . . ?
C25 C24 C23 121.2(8) . . ?
C26 C25 C24 122.3(8) . . ?
C25 C26 C27 119.1(9) . . ?
C28 C27 C26 119.8(8) . . ?
C27 C28 C29 119.6(8) . . ?
C24 C29 C28 122.0(8) . . ?
C24 C29 O4 120.0(7) . . ?
C28 C29 O4 117.8(7) . . ?
N4 C30 C31 122.1(8) . . ?
N4 C30 N5 115.5(7) . . ?
C31 C30 N5 122.4(7) . . ?
C32 C31 C30 117.9(8) . . ?
C31 C32 C33 121.1(8) . . ?
C34 C33 C32 118.2(8) . . ?
N4 C34 C33 122.1(8) . . ?
N4 C34 N6 115.2(7) . . ?
C33 C34 N6 122.7(7) . . ?
C40 C35 C36 121.9(8) . . ?
C40 C35 O5 120.1(7) . . ?
C36 C35 O5 117.6(7) . . ?
C37 C36 C35 118.5(8) . . ?
C38 C37 C36 120.2(8) . . ?
C39 C38 C37 120.8(8) . . ?
C38 C39 C40 120.5(8) . . ?
C35 C40 C39 118.0(8) . . ?
C35 C40 C41 119.8(7) . . ?
C39 C40 C41 122.3(7) . . ?
C46 C41 C42 117.1(8) . . ?
C46 C41 C40 121.3(7) . . ?
C42 C41 C40 121.5(7) . . ?
C43 C42 C41 120.7(8) . . ?
C42 C43 C44 121.1(8) . . ?
C43 C44 C45 119.7(8) . . ?
C46 C45 C44 117.7(8) . . ?
C45 C46 C41 123.7(8) . . ?
C45 C46 O6 117.9(7) . . ?
C41 C46 O6 118.3(7) . . ?
C48 C47 C52 122.5(8) . . ?
C48 C47 O7 118.8(7) . . ?
C52 C47 O7 118.5(7) . . ?
C47 C48 C49 120.4(8) . . ?
C48 C49 C50 117.3(8) . . ?
C51 C50 C49 122.4(8) . . ?
C50 C51 C52 120.1(8) . . ?
C47 C52 C51 117.2(8) . . ?
C47 C52 C53 120.7(7) . . ?
C51 C52 C53 122.1(7) . . ?
C58 C53 C54 117.6(8) . . ?
C58 C53 C52 121.4(7) . . ?
C54 C53 C52 120.9(7) . . ?
C55 C54 C53 120.4(8) . . ?
C56 C55 C54 120.2(8) . . ?
C55 C56 C57 120.4(8) . . ?
C56 C57 C58 119.0(8) . . ?
C53 C58 C57 122.2(8) . . ?
C53 C58 O8 120.0(7) . . ?
C57 C58 O8 117.5(7) . . ?
O11T S1 O10T 109.8(8) . . ?
O11T S1 O9T 123.7(7) . . ?
O10T S1 O9T 118.4(7) . . ?
O11T S1 C59T 96.4(8) . . ?
O10T S1 C59T 104.3(7) . . ?
O9T S1 C59T 98.0(7) . . ?
F2 C59T F1 114.8(15) . . ?
F2 C59T F3 107.3(15) . . ?
F1 C59T F3 107.2(13) . . ?
F2 C59T S1 115.0(13) . . ?
F1 C59T S1 108.8(12) . . ?
F3 C59T S1 102.8(11) . . ?
O13T S2 O12T 115.0(4) . . ?
O13T S2 O14T 115.3(4) . . ?
O12T S2 O14T 114.1(5) . . ?
O13T S2 C60T 105.2(4) . . ?
O12T S2 C60T 102.9(5) . . ?
O14T S2 C60T 102.2(5) . . ?
F6 C60T F5 107.9(9) . . ?
F6 C60T F4 108.1(9) . . ?
F5 C60T F4 107.2(9) . . ?
F6 C60T S2 112.2(8) . . ?
F5 C60T S2 111.2(7) . . ?
F4 C60T S2 110.1(7) . . ?
C64 O15 C61 107.7(7) . . ?
O15 C61 C62 106.7(7) . . ?
C63 C62 C61 103.3(8) . . ?
C64 C63 C62 102.5(8) . . ?
O15 C64 C63 104.2(8) . . ?
C68 O16 C65 106.9(7) . . ?
O16 C65 C66 106.0(7) . . ?
C67 C66 C65 104.4(7) . . ?
C68 C67 C66 101.9(8) . . ?
O16 C68 C67 104.2(8) . . ?
C72 O17 C69 108.7(7) . . ?
O17 C69 C70 107.6(8) . . ?
C71 C70 C69 103.8(9) . . ?
C70 C71 C72 102.0(9) . . ?
O17 C72 C71 105.3(8) . . ?
C76 O18 C73 106.2(12) . . ?
O18 C73 C74 104.3(12) . . ?
C75 C74 C73 107.2(16) . . ?
C74 C75 C76 114(2) . . ?
C75 C76 O18 107.7(15) . . ?
C77 O19 C80 100(2) . . ?
C78 C77 O19 111(3) . . ?
C79 C78 C77 107(3) . . ?
C78 C79 C80 112(3) . . ?
C79 C80 O19 107(2) . . ?
C84 O20 C81 109.7(12) . . ?
C82 C81 O20 105.3(14) . . ?
C81 C82 C83 117.5(15) . . ?
C82 C83 C84 103.6(12) . . ?
O20 C84 C83 91.5(10) . . ?
C86 O21 C85 108(3) 2_676 . ?
C86 C85 O21 126(2) . . ?
O21 C86 C85 110(3) 2_676 . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        23.82
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         3.217
_refine_diff_density_min         -1.375
_refine_diff_density_rms         0.167
_database_code_depnum_ccdc_archive 'CCDC 1005384'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
5d.2(Me2CO)  --  [Fe(k³-P,N,P-PNP-Me)₂](CF₃SO₃)₂.(Me₂CO)₂ 
;
_chemical_name_common            
'5d.2(Me2CO)   [Fe(k3-P,N,P-PNP-Me)2](CF3SO3)2.(Me2CO)2'
_chemical_formula_moiety         'C18 H34 Fe N6 P4, 2(C F3 O3 S), 2(C3 H6 O)'
_chemical_formula_sum            'C26 H46 F6 Fe N6 O8 P4 S2'
_chemical_formula_weight         928.54

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.6764(17)
_cell_length_b                   18.291(2)
_cell_length_c                   16.390(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.886(2)
_cell_angle_gamma                90.00
_cell_volume                     4051.0(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6729
_cell_measurement_theta_min      2.272
_cell_measurement_theta_max      31.986

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1920
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_process_details   'program SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'ω- and φ-scans'
_diffrn_reflns_number            33718
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         32.00
_reflns_number_total             6952
_reflns_number_gt                6060
_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 F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0695P)²+8.9523P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6952
_refine_ls_number_parameters     261
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1277
_refine_ls_wR_factor_gt          0.1237
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.006
_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 0.0000 0.139507(18) 0.2500 0.01447(8) Uani 1 2 d S . .
P1 P 0.11364(3) 0.04956(2) 0.24442(3) 0.01713(10) Uani 1 1 d . . .
P2 P -0.11368(3) 0.22956(3) 0.21545(3) 0.01771(10) Uani 1 1 d . . .
N1 N 0.00259(10) 0.14119(8) 0.12851(9) 0.0161(3) Uani 1 1 d . . .
N2 N 0.08391(11) 0.02983(9) 0.14185(9) 0.0194(3) Uani 1 1 d D . .
H2N H 0.1115(17) -0.0026(10) 0.1219(15) 0.023 Uiso 1 1 d D . .
N3 N -0.08317(11) 0.25066(9) 0.12189(9) 0.0199(3) Uani 1 1 d D . .
H3N H -0.1205(15) 0.2770(11) 0.0933(13) 0.024 Uiso 1 1 d D . .
C1 C 0.04528(12) 0.08621(9) 0.09061(10) 0.0172(3) Uani 1 1 d . . .
C2 C 0.04993(14) 0.08638(10) 0.00624(11) 0.0203(3) Uani 1 1 d . . .
H2 H 0.0805 0.0474 -0.0187 0.024 Uiso 1 1 calc R . .
C3 C 0.00853(14) 0.14517(10) -0.04028(11) 0.0222(3) Uani 1 1 d . . .
H3 H 0.0107 0.1467 -0.0979 0.027 Uiso 1 1 calc R . .
C4 C -0.03590(14) 0.20164(10) -0.00323(11) 0.0208(3) Uani 1 1 d . . .
H4 H -0.0640 0.2422 -0.0346 0.025 Uiso 1 1 calc R . .
C5 C -0.03831(12) 0.19728(9) 0.08129(10) 0.0175(3) Uani 1 1 d . . .
C6 C 0.11617(15) -0.03932(10) 0.29529(11) 0.0236(3) Uani 1 1 d . . .
H6A H 0.0490 -0.0527 0.3035 0.035 Uiso 1 1 calc R . .
H6B H 0.1590 -0.0367 0.3490 0.035 Uiso 1 1 calc R . .
H6C H 0.1418 -0.0762 0.2608 0.035 Uiso 1 1 calc R . .
C7 C 0.24747(14) 0.06025(12) 0.25214(13) 0.0266(4) Uani 1 1 d . . .
H7A H 0.2761 0.0153 0.2334 0.040 Uiso 1 1 calc R . .
H7B H 0.2761 0.0699 0.3097 0.040 Uiso 1 1 calc R . .
H7C H 0.2620 0.1013 0.2175 0.040 Uiso 1 1 calc R . .
C8 C -0.24803(14) 0.22174(12) 0.18831(13) 0.0259(4) Uani 1 1 d . . .
H8A H -0.2748 0.2671 0.1620 0.039 Uiso 1 1 calc R . .
H8B H -0.2772 0.2131 0.2384 0.039 Uiso 1 1 calc R . .
H8C H -0.2641 0.1808 0.1500 0.039 Uiso 1 1 calc R . .
C9 C -0.11479(16) 0.31642(11) 0.27029(12) 0.0259(4) Uani 1 1 d . . .
H9A H -0.0472 0.3291 0.2953 0.039 Uiso 1 1 calc R . .
H9B H -0.1564 0.3119 0.3136 0.039 Uiso 1 1 calc R . .
H9C H -0.1414 0.3548 0.2314 0.039 Uiso 1 1 calc R . .
S1 S 0.25862(3) 0.08849(2) 0.52478(3) 0.02073(10) Uani 1 1 d . . .
F1 F 0.3591(3) -0.03128(13) 0.5529(2) 0.1037(10) Uani 1 1 d . . .
F3 F 0.40751(17) 0.0368(2) 0.46307(14) 0.1022(11) Uani 1 1 d . . .
F2 F 0.44191(14) 0.06540(13) 0.59140(13) 0.0665(6) Uani 1 1 d . . .
O1 O 0.19446(12) 0.05486(9) 0.45743(10) 0.0326(3) Uani 1 1 d . . .
O2 O 0.28997(14) 0.16139(9) 0.50753(10) 0.0375(4) Uani 1 1 d . . .
O3 O 0.22953(12) 0.08090(9) 0.60545(10) 0.0322(3) Uani 1 1 d . . .
C10 C 0.3732(2) 0.03765(19) 0.5337(2) 0.0525(8) Uani 1 1 d . . .
O4 O 0.2332(4) 0.2114(3) 0.1039(3) 0.0554(11) Uani 0.50 1 d P . .
C11 C 0.2384(4) 0.2361(4) 0.0369(3) 0.0481(13) Uani 0.50 1 d P . .
C12 C 0.2794(5) 0.1884(4) -0.0239(3) 0.1048(19) Uani 1 1 d . . .
H12A H 0.2853 0.1395 -0.0024 0.157 Uiso 0.50 1 d PR . .
H12B H 0.2357 0.1887 -0.0757 0.157 Uiso 0.50 1 d PR . .
H12C H 0.3434 0.2059 -0.0319 0.157 Uiso 0.50 1 d PR . .
H12D H 0.3055 0.1685 -0.0702 0.157 Uiso 0.50 1 d PR . .
H12E H 0.2186 0.1642 -0.0183 0.157 Uiso 0.50 1 d PR . .
H12F H 0.3263 0.1813 0.0255 0.157 Uiso 0.50 1 d PR . .
O5 O 0.5000 0.2738(4) 0.2500 0.158(3) Uani 1 2 d S . .
C13 C 0.5000 0.2044(4) 0.2500 0.0765(17) Uani 1 2 d S . .
C14 C 0.4794(4) 0.1711(4) 0.1742(3) 0.0961(18) Uani 1 1 d . . .
H14A H 0.4176 0.1909 0.1440 0.144 Uiso 1 1 calc R . .
H14B H 0.4723 0.1183 0.1817 0.144 Uiso 1 1 calc R . .
H14C H 0.5335 0.1803 0.1427 0.144 Uiso 1 1 calc R . .


_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 N1 1.9973(14) 2 ?
Fe1 N1 1.9973(14) . ?
Fe1 P1 2.2748(5) . ?
Fe1 P1 2.2748(5) 2 ?
Fe1 P2 2.2758(5) . ?
Fe1 P2 2.2758(5) 2 ?
P1 N2 1.7062(16) . ?
P1 C6 1.8250(19) . ?
P1 C7 1.826(2) . ?
P2 N3 1.6947(16) . ?
P2 C9 1.827(2) . ?
P2 C8 1.8281(19) . ?
N1 C5 1.353(2) . ?
N1 C1 1.360(2) . ?
N2 C1 1.382(2) . ?
N2 H2N 0.80000(12) . ?
N3 C5 1.378(2) . ?
N3 H3N 0.80000(12) . ?
C1 C2 1.394(2) . ?
C2 C3 1.387(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(2) . ?
C4 H4 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
S1 O1 1.4380(15) . ?
S1 O2 1.4420(16) . ?
S1 O3 1.4451(16) . ?
S1 C10 1.808(3) . ?
F1 C10 1.321(5) . ?
F3 C10 1.315(4) . ?
F2 C10 1.327(4) . ?
O4 C11 1.199(7) . ?
C11 C11 1.393(11) 7 ?
C11 C12 1.412(9) 7 ?
C11 C12 1.496(9) . ?
C12 C11 1.412(9) 7 ?
C12 H12A 0.9600 . ?
C12 H12B 0.9601 . ?
C12 H12C 0.9600 . ?
C12 H12D 0.9601 . ?
C12 H12E 0.9600 . ?
C12 H12F 0.9600 . ?
O5 C13 1.269(9) . ?
C13 C14 1.374(6) . ?
C13 C14 1.374(6) 2_655 ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 178.23(9) 2 . ?
N1 Fe1 P1 99.71(4) 2 . ?
N1 Fe1 P1 81.58(4) . . ?
N1 Fe1 P1 81.58(4) 2 2 ?
N1 Fe1 P1 99.71(4) . 2 ?
P1 Fe1 P1 87.35(3) . 2 ?
N1 Fe1 P2 96.91(4) 2 . ?
N1 Fe1 P2 81.80(4) . . ?
P1 Fe1 P2 163.382(16) . . ?
P1 Fe1 P2 95.091(19) 2 . ?
N1 Fe1 P2 81.80(4) 2 2 ?
N1 Fe1 P2 96.91(4) . 2 ?
P1 Fe1 P2 95.092(19) . 2 ?
P1 Fe1 P2 163.383(16) 2 2 ?
P2 Fe1 P2 87.26(3) . 2 ?
N2 P1 C6 104.27(8) . . ?
N2 P1 C7 100.06(9) . . ?
C6 P1 C7 96.64(10) . . ?
N2 P1 Fe1 97.60(5) . . ?
C6 P1 Fe1 126.21(7) . . ?
C7 P1 Fe1 127.13(7) . . ?
N3 P2 C9 105.61(9) . . ?
N3 P2 C8 100.15(9) . . ?
C9 P2 C8 95.93(10) . . ?
N3 P2 Fe1 97.80(5) . . ?
C9 P2 Fe1 124.36(7) . . ?
C8 P2 Fe1 128.78(7) . . ?
C5 N1 C1 117.92(14) . . ?
C5 N1 Fe1 120.83(11) . . ?
C1 N1 Fe1 121.25(11) . . ?
C1 N2 P1 116.83(12) . . ?
C1 N2 H2N 117.8(19) . . ?
P1 N2 H2N 120.2(19) . . ?
C5 N3 P2 117.76(12) . . ?
C5 N3 H3N 115.8(19) . . ?
P2 N3 H3N 116.3(19) . . ?
N1 C1 N2 115.15(15) . . ?
N1 C1 C2 122.67(16) . . ?
N2 C1 C2 122.18(15) . . ?
C3 C2 C1 118.01(16) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C4 C3 C2 120.43(16) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 118.20(16) . . ?
C3 C4 H4 120.9 . . ?
C5 C4 H4 120.9 . . ?
N1 C5 N3 115.89(15) . . ?
N1 C5 C4 122.75(16) . . ?
N3 C5 C4 121.36(16) . . ?
P1 C6 H6A 109.5 . . ?
P1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
P1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P1 C7 H7A 109.5 . . ?
P1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
P1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
P2 C8 H8A 109.5 . . ?
P2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
P2 C9 H9A 109.5 . . ?
P2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 S1 O2 114.18(10) . . ?
O1 S1 O3 116.09(10) . . ?
O2 S1 O3 113.61(11) . . ?
O1 S1 C10 105.10(12) . . ?
O2 S1 C10 102.20(15) . . ?
O3 S1 C10 103.54(13) . . ?
F3 C10 F1 106.4(3) . . ?
F3 C10 F2 108.8(3) . . ?
F1 C10 F2 108.0(3) . . ?
F3 C10 S1 111.0(2) . . ?
F1 C10 S1 110.7(3) . . ?
F2 C10 S1 111.8(2) . . ?
O4 C11 C11 170.4(8) . 7 ?
O4 C11 C12 118.3(6) . 7 ?
C11 C11 C12 64.4(6) 7 7 ?
O4 C11 C12 118.1(7) . . ?
C11 C11 C12 58.4(5) 7 . ?
C12 C11 C12 122.8(5) 7 . ?
C11 C12 C11 57.2(5) 7 . ?
C11 C12 H12A 165.7 7 . ?
C11 C12 H12A 108.6 . . ?
C11 C12 H12B 78.0 7 . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 78.2 7 . ?
C11 C12 H12C 110.0 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C12 H12D 109.2 7 . ?
C11 C12 H12D 166.3 . . ?
H12A C12 H12D 85.1 . . ?
H12B C12 H12D 63.8 . . ?
H12C C12 H12D 63.8 . . ?
C11 C12 H12E 109.5 7 . ?
C11 C12 H12E 77.7 . . ?
H12A C12 H12E 63.8 . . ?
H12B C12 H12E 69.9 . . ?
H12C C12 H12E 171.6 . . ?
H12D C12 H12E 109.5 . . ?
C11 C12 H12F 109.7 7 . ?
C11 C12 H12F 77.8 . . ?
H12A C12 H12F 63.8 . . ?
H12B C12 H12F 171.6 . . ?
H12C C12 H12F 69.9 . . ?
H12D C12 H12F 109.5 . . ?
H12E C12 H12F 109.5 . . ?
O5 C13 C14 116.3(4) . . ?
O5 C13 C14 116.3(4) . 2_655 ?
C14 C13 C14 127.3(8) . 2_655 ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Fe1 P1 N2 161.25(7) 2 . . . ?
N1 Fe1 P1 N2 -19.97(7) . . . . ?
P1 Fe1 P1 N2 80.26(6) 2 . . . ?
P2 Fe1 P1 N2 -18.69(10) . . . . ?
P2 Fe1 P1 N2 -116.22(6) 2 . . . ?
N1 Fe1 P1 C6 47.29(9) 2 . . . ?
N1 Fe1 P1 C6 -133.93(9) . . . . ?
P1 Fe1 P1 C6 -33.70(8) 2 . . . ?
P2 Fe1 P1 C6 -132.65(10) . . . . ?
P2 Fe1 P1 C6 129.82(8) 2 . . . ?
N1 Fe1 P1 C7 -89.96(10) 2 . . . ?
N1 Fe1 P1 C7 88.82(10) . . . . ?
P1 Fe1 P1 C7 -170.95(9) 2 . . . ?
P2 Fe1 P1 C7 90.10(11) . . . . ?
P2 Fe1 P1 C7 -7.43(9) 2 . . . ?
N1 Fe1 P2 N3 160.48(7) 2 . . . ?
N1 Fe1 P2 N3 -18.30(7) . . . . ?
P1 Fe1 P2 N3 -19.58(10) . . . . ?
P1 Fe1 P2 N3 -117.41(6) 2 . . . ?
P2 Fe1 P2 N3 79.08(6) 2 . . . ?
N1 Fe1 P2 C9 45.48(10) 2 . . . ?
N1 Fe1 P2 C9 -133.30(10) . . . . ?
P1 Fe1 P2 C9 -134.58(10) . . . . ?
P1 Fe1 P2 C9 127.59(9) 2 . . . ?
P2 Fe1 P2 C9 -35.92(8) 2 . . . ?
N1 Fe1 P2 C8 -89.74(10) 2 . . . ?
N1 Fe1 P2 C8 91.48(10) . . . . ?
P1 Fe1 P2 C8 90.20(11) . . . . ?
P1 Fe1 P2 C8 -7.63(9) 2 . . . ?
P2 Fe1 P2 C8 -171.14(9) 2 . . . ?
P1 Fe1 N1 C5 -166.26(13) . . . . ?
P1 Fe1 N1 C5 107.91(13) 2 . . . ?
P2 Fe1 N1 C5 14.11(12) . . . . ?
P2 Fe1 N1 C5 -72.11(13) 2 . . . ?
P1 Fe1 N1 C1 13.79(12) . . . . ?
P1 Fe1 N1 C1 -72.04(13) 2 . . . ?
P2 Fe1 N1 C1 -165.84(13) . . . . ?
P2 Fe1 N1 C1 107.94(13) 2 . . . ?
C6 P1 N2 C1 159.38(14) . . . . ?
C7 P1 N2 C1 -101.05(14) . . . . ?
Fe1 P1 N2 C1 28.91(13) . . . . ?
C9 P2 N3 C5 154.12(14) . . . . ?
C8 P2 N3 C5 -106.73(15) . . . . ?
Fe1 P2 N3 C5 25.09(14) . . . . ?
C5 N1 C1 N2 -178.72(15) . . . . ?
Fe1 N1 C1 N2 1.2(2) . . . . ?
C5 N1 C1 C2 1.2(3) . . . . ?
Fe1 N1 C1 C2 -178.80(13) . . . . ?
P1 N2 C1 N1 -22.8(2) . . . . ?
P1 N2 C1 C2 157.19(14) . . . . ?
N1 C1 C2 C3 -0.4(3) . . . . ?
N2 C1 C2 C3 179.59(17) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
C1 N1 C5 N3 178.21(15) . . . . ?
Fe1 N1 C5 N3 -1.7(2) . . . . ?
C1 N1 C5 C4 -1.8(3) . . . . ?
Fe1 N1 C5 C4 178.27(14) . . . . ?
P2 N3 C5 N1 -18.3(2) . . . . ?
P2 N3 C5 C4 161.69(14) . . . . ?
C3 C4 C5 N1 1.4(3) . . . . ?
C3 C4 C5 N3 -178.58(17) . . . . ?
O1 S1 C10 F3 55.1(3) . . . . ?
O2 S1 C10 F3 -64.4(3) . . . . ?
O3 S1 C10 F3 177.3(3) . . . . ?
O1 S1 C10 F1 -62.9(3) . . . . ?
O2 S1 C10 F1 177.6(2) . . . . ?
O3 S1 C10 F1 59.4(3) . . . . ?
O1 S1 C10 F2 176.7(2) . . . . ?
O2 S1 C10 F2 57.2(3) . . . . ?
O3 S1 C10 F2 -61.1(3) . . . . ?
O4 C11 C12 C11 -169.7(9) . . . 7 ?
C12 C11 C12 C11 0.0 7 . . 7 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2N O3 0.80 2.205(10) 2.965(2) 159(3) 6
N3 H3N O2 0.80 2.052(4) 2.847(2) 173(3) 8_455

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        32.00
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.098

#===END
#==============================================================================0
#============================Finish=====================================




_database_code_depnum_ccdc_archive 'CCDC 1005387'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5c


# start Validation Reply Form
_vrf_PLAT041_5c                  
;
PROBLEM:     
PLAT041_ALERT_1_C Calc. and Reported SumFormula Strings Differ -- Please Check
RESPONSE:
In this CIF the chemical formula and Z=2 are given for the asymmetric unit.
The crystal structure contains a disordered diethyl ether solvent molecule
located across a centre of inversion (x,y,z = 1/2,1/2,1/2).
Therefore program PLATON doubles chemical formula and halves Z and 
generates the given alert.
;
# end Validation Reply Form



# 5. CHEMICAL DATA

_chemical_name_systematic        
; 
5c.0.5EtOEt  --  [Fe(k³-P,N,P-PNP-Et)₂](BPh₄)₂.0.5EtOEt  
;
_chemical_name_common            
'5c*0.5EtOEt   [Fe(k3-P,N,P-PNP-Et)2](BPh4)2*0.5EtOEt'
_chemical_formula_moiety         
'(C26 H50 Fe N6 P4), 2(C24 H20 B), 0.5(C4 H10 O)'
_chemical_formula_sum            'C76 H95 B2 Fe1 N6 O0.5 P4'
_chemical_formula_weight         1302

#==============================================================================0

# 6. CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   13.3977(13)
_cell_length_b                   14.1994(14)
_cell_length_c                   21.6176(19)
_cell_angle_alpha                93.677(3)
_cell_angle_beta                 105.861(3)
_cell_angle_gamma                117.314(3)
_cell_volume                     3427.3(6)

_cell_formula_units_Z            2

_cell_measurement_reflns_used    9847
_cell_measurement_theta_min      2.9
_cell_measurement_theta_max      27.5
_cell_measurement_temperature    293
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.2612
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1386

_exptl_absorpt_coefficient_mu    0.362
_exptl_crystal_description       block
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            'clear red'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_T_max  0.92

#==============================================================================0

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      293
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_reflns_number            134214
_diffrn_reflns_theta_min         1
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_max 1
_diffrn_measured_fraction_theta_full 1
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_reduction_process ?


_diffrn_radiation_probe          X-ray

#==============================================================================0

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             15798
_reflns_number_gt                12425
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_gt          0.0870
_refine_ls_R_factor_all          0.0489
_refine_ls_wR_factor_ref         0.0939
_refine_ls_goodness_of_fit_ref   1.53
_refine_ls_goodness_of_fit_gt    1.61
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         15798
_refine_ls_number_parameters     836
_refine_ls_number_restraints     0
_refine_ls_number_constraints    384
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0016I²)
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          0.0356
_refine_ls_shift/su_mean         0.0015
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
B 0.0013 0.0007 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
P 0.1023 0.0942 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'Jana2006 [Petricek et al., 2006]'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

#==============================================================================0

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_mutiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.904746(18) 0.666796(16) 0.241880(9) Uani 0.01036(9) 2 1 d . . .
N1 N 1.04959(11) 0.76912(10) 0.21988(6) Uani 0.0135(5) 2 1 d . . .
N2 N 1.16501(12) 0.79281(11) 0.32631(7) Uani 0.0169(6) 2 1 d . . .
N3 N 0.92299(11) 0.73635(10) 0.11477(6) Uani 0.0154(6) 2 1 d . . .
P1 P 1.03883(3) 0.76347(3) 0.344471(18) Uani 0.01339(16) 2 1 d . . .
P2 P 0.83220(3) 0.61484(3) 0.129278(17) Uani 0.01184(15) 2 1 d . . .
C1 C 1.16181(13) 0.81569(12) 0.26493(7) Uani 0.0158(6) 2 1 d . . .
C2 C 1.26338(14) 0.87978(13) 0.25038(8) Uani 0.0222(7) 2 1 d . . .
C3 C 1.24916(15) 0.89964(13) 0.18765(9) Uani 0.0263(7) 2 1 d . . .
C4 C 1.13652(15) 0.85757(13) 0.14144(8) Uani 0.0221(7) 2 1 d . . .
C5 C 1.03842(13) 0.79046(12) 0.15858(7) Uani 0.0159(6) 2 1 d . . .
C6 C 1.06150(14) 0.71110(12) 0.41899(7) Uani 0.0176(7) 2 1 d . . .
C7 C 0.96223(14) 0.68429(13) 0.44823(7) Uani 0.0202(7) 2 1 d . . .
C8 C 1.07123(14) 0.90133(12) 0.37722(7) Uani 0.0187(7) 2 1 d . . .
C9 C 1.19960(15) 0.97716(13) 0.42427(8) Uani 0.0255(7) 2 1 d . . .
C10 C 0.86088(13) 0.52386(12) 0.08145(7) Uani 0.0163(6) 2 1 d . . .
C11 C 0.99316(14) 0.56068(13) 0.09880(8) Uani 0.0193(7) 2 1 d . . .
C12 C 0.68529(13) 0.58137(12) 0.07357(7) Uani 0.0159(6) 2 1 d . . .
C13 C 0.59244(14) 0.46230(13) 0.06469(7) Uani 0.0194(7) 2 1 d . . .
P3 P 0.80396(3) 0.76180(3) 0.232275(18) Uani 0.01212(15) 2 1 d . . .
P4 P 0.94554(3) 0.52809(3) 0.262019(18) Uani 0.01204(15) 2 1 d . . .
N4 N 0.75820(10) 0.56353(9) 0.26105(6) Uani 0.0114(5) 2 1 d . . .
N5 N 0.66337(11) 0.65157(10) 0.20816(6) Uani 0.0141(5) 2 1 d . . .
N6 N 0.86468(11) 0.48446(10) 0.31369(6) Uani 0.0136(5) 2 1 d . . .
C14 C 0.65463(13) 0.56690(12) 0.23883(7) Uani 0.0128(6) 2 1 d . . .
C15 C 0.54995(13) 0.49238(12) 0.24723(7) Uani 0.0164(6) 2 1 d . . .
C16 C 0.55212(14) 0.41406(13) 0.28122(7) Uani 0.0176(7) 2 1 d . . .
C17 C 0.65701(13) 0.41096(12) 0.30639(7) Uani 0.0152(6) 2 1 d . . .
C18 C 0.75738(13) 0.48573(12) 0.29432(7) Uani 0.0126(6) 2 1 d . . .
C19 C 0.79584(14) 0.84363(12) 0.17155(7) Uani 0.0173(7) 2 1 d . . .
C20 C 0.91086(16) 0.95382(13) 0.19245(8) Uani 0.0255(8) 2 1 d . . .
C21 C 0.79749(13) 0.84158(13) 0.30012(7) Uani 0.0176(7) 2 1 d . . .
C22 C 0.76186(15) 0.78184(13) 0.35316(8) Uani 0.0222(7) 2 1 d . . .
C23 C 1.09209(13) 0.54384(12) 0.30690(7) Uani 0.0174(6) 2 1 d . . .
C24 C 1.09188(15) 0.46494(14) 0.35178(8) Uani 0.0263(8) 2 1 d . . .
C25 C 0.88321(13) 0.39911(11) 0.20317(7) Uani 0.0158(6) 2 1 d . . .
C26 C 0.74672(14) 0.33547(12) 0.17583(8) Uani 0.0203(7) 2 1 d . . .
B1 B 0.18559(15) 0.32042(14) 0.12656(8) Uani 0.0142(7) 2 1 d . . .
C27 C 0.04187(13) 0.27896(12) 0.10362(7) Uani 0.0152(6) 2 1 d . . .
C28 C -0.03482(14) 0.20941(12) 0.13342(8) Uani 0.0183(7) 2 1 d . . .
C29 C -0.15844(15) 0.16560(13) 0.10809(8) Uani 0.0228(7) 2 1 d . . .
C30 C -0.21020(15) 0.19081(13) 0.05174(8) Uani 0.0242(7) 2 1 d . . .
C31 C -0.13704(15) 0.26182(14) 0.02142(8) Uani 0.0234(7) 2 1 d . . .
C32 C -0.01374(14) 0.30469(13) 0.04745(7) Uani 0.0194(7) 2 1 d . . .
C33 C 0.20736(13) 0.24981(12) 0.07326(7) Uani 0.0148(6) 2 1 d . . .
C34 C 0.11408(14) 0.16276(12) 0.02206(7) Uani 0.0172(7) 2 1 d . . .
C35 C 0.13370(15) 0.09745(13) -0.01862(8) Uani 0.0207(7) 2 1 d . . .
C36 C 0.24808(15) 0.11813(13) -0.01049(8) Uani 0.0208(7) 2 1 d . . .
C37 C 0.34370(15) 0.20418(13) 0.03952(8) Uani 0.0196(7) 2 1 d . . .
C38 C 0.32211(14) 0.26661(12) 0.08077(7) Uani 0.0170(7) 2 1 d . . .
C39 C 0.25785(13) 0.45207(12) 0.12956(7) Uani 0.0139(6) 2 1 d . . .
C40 C 0.22980(14) 0.52173(13) 0.16079(7) Uani 0.0182(7) 2 1 d . . .
C41 C 0.28700(15) 0.63341(13) 0.16587(8) Uani 0.0228(7) 2 1 d . . .
C42 C 0.37466(14) 0.68167(13) 0.13772(8) Uani 0.0222(7) 2 1 d . . .
C43 C 0.40377(14) 0.61616(13) 0.10521(7) Uani 0.0191(7) 2 1 d . . .
C44 C 0.34685(13) 0.50429(12) 0.10191(7) Uani 0.0154(6) 2 1 d . . .
C45 C 0.22797(13) 0.29249(12) 0.19943(7) Uani 0.0162(6) 2 1 d . . .
C46 C 0.22548(14) 0.19315(13) 0.20402(8) Uani 0.0216(7) 2 1 d . . .
C47 C 0.25286(15) 0.16371(15) 0.26412(9) Uani 0.0264(8) 2 1 d . . .
C48 C 0.28350(15) 0.23312(15) 0.32244(8) Uani 0.0266(8) 2 1 d . . .
C49 C 0.28617(15) 0.33104(16) 0.31995(8) Uani 0.0252(8) 2 1 d . . .
C50 C 0.25931(14) 0.36007(14) 0.25962(8) Uani 0.0202(7) 2 1 d . . .
B2 B 0.65856(15) 0.07929(14) 0.33707(8) Uani 0.0148(7) 2 1 d . . .
C51 C 0.67730(14) 0.18735(12) 0.38336(7) Uani 0.0156(6) 2 1 d . . .
C52 C 0.78877(14) 0.28113(12) 0.41354(7) Uani 0.0177(7) 2 1 d . . .
C53 C 0.80522(16) 0.37169(13) 0.45368(8) Uani 0.0223(7) 2 1 d . . .
C54 C 0.70852(16) 0.37147(14) 0.46514(8) Uani 0.0248(8) 2 1 d . . .
C55 C 0.59648(16) 0.28139(14) 0.43571(8) Uani 0.0235(8) 2 1 d . . .
C56 C 0.58122(15) 0.19200(13) 0.39544(8) Uani 0.0199(7) 2 1 d . . .
C57 C 0.57486(13) -0.03266(12) 0.35840(7) Uani 0.0161(6) 2 1 d . . .
C58 C 0.55526(15) -0.03241(14) 0.41889(8) Uani 0.0223(7) 2 1 d . . .
C59 C 0.48754(16) -0.12704(14) 0.43764(9) Uani 0.0275(8) 2 1 d . . .
C60 C 0.43747(16) -0.22740(14) 0.39627(9) Uani 0.0275(8) 2 1 d . . .
C61 C 0.45610(15) -0.23179(14) 0.33639(8) Uani 0.0259(7) 2 1 d . . .
C62 C 0.52274(14) -0.13646(13) 0.31809(8) Uani 0.0207(7) 2 1 d . . .
C63 C 0.79202(13) 0.09297(12) 0.35119(7) Uani 0.0152(6) 2 1 d . . .
C64 C 0.86575(14) 0.14550(12) 0.31491(8) Uani 0.0189(7) 2 1 d . . .
C65 C 0.98413(14) 0.16867(13) 0.33211(8) Uani 0.0216(7) 2 1 d . . .
C66 C 1.03374(14) 0.13971(13) 0.38744(8) Uani 0.0226(7) 2 1 d . . .
C67 C 0.96372(14) 0.08654(13) 0.42439(8) Uani 0.0209(7) 2 1 d . . .
C68 C 0.84568(14) 0.06368(12) 0.40627(7) Uani 0.0175(7) 2 1 d . . .
C69 C 0.59587(13) 0.07236(12) 0.25830(7) Uani 0.0158(6) 2 1 d . . .
C70 C 0.53137(13) 0.12557(12) 0.23652(8) Uani 0.0173(6) 2 1 d . . .
C71 C 0.47856(14) 0.11923(13) 0.17001(8) Uani 0.0214(7) 2 1 d . . .
C72 C 0.48728(15) 0.05752(13) 0.12190(8) Uani 0.0242(7) 2 1 d . . .
C73 C 0.55006(15) 0.00292(13) 0.14106(8) Uani 0.0234(7) 2 1 d . . .
C74 C 0.60358(14) 0.01123(13) 0.20768(8) Uani 0.0206(7) 2 1 d . . .
O1 O 0.4531(4) 0.5192(3) 0.4763(2) Uani 0.077(3) 2 0.5 d . . .
C75 C 0.6509(4) 0.6336(4) 0.4768(2) Uani 0.148(4) 2 1 d . . .
C76 C 0.5437(6) 0.5646(5) 0.4435(3) Uani 0.079(4) 2 0.5 d . . .
C77 C 0.4468(7) 0.4389(5) 0.5056(3) Uani 0.070(4) 2 0.5 d . . .
H1c2 H 1.341494 0.909619 0.282895 Uiso 0.0266 2 1 d . . .
H1c3 H 1.318283 0.943089 0.176131 Uiso 0.0316 2 1 d . . .
H1c4 H 1.126121 0.874194 0.09857 Uiso 0.0266 2 1 d . . .
H1c6 H 1.067548 0.647332 0.409433 Uiso 0.0212 2 1 d . . .
H2c6 H 1.137072 0.763102 0.451437 Uiso 0.0212 2 1 d . . .
H1c7 H 0.978027 0.655891 0.486629 Uiso 0.0243 2 1 d . . .
H2c7 H 0.959468 0.749079 0.460311 Uiso 0.0243 2 1 d . . .
H3c7 H 0.886889 0.631072 0.416114 Uiso 0.0243 2 1 d . . .
H1c8 H 1.053685 0.93404 0.341266 Uiso 0.0224 2 1 d . . .
H2c8 H 1.016017 0.896612 0.398975 Uiso 0.0224 2 1 d . . .
H1c9 H 1.206349 1.043788 0.443157 Uiso 0.0306 2 1 d . . .
H2c9 H 1.218778 0.942597 0.45879 Uiso 0.0306 2 1 d . . .
H3c9 H 1.253969 0.992533 0.400304 Uiso 0.0306 2 1 d . . .
H1c10 H 0.819717 0.451629 0.08821 Uiso 0.0195 2 1 d . . .
H2c10 H 0.826712 0.518334 0.035218 Uiso 0.0195 2 1 d . . .
H1c11 H 1.002137 0.502985 0.08022 Uiso 0.0232 2 1 d . . .
H2c11 H 1.030328 0.62324 0.081239 Uiso 0.0232 2 1 d . . .
H3c11 H 1.03046 0.579058 0.145868 Uiso 0.0232 2 1 d . . .
H1c12 H 0.65982 0.627489 0.090485 Uiso 0.0191 2 1 d . . .
H2c12 H 0.690506 0.595803 0.031446 Uiso 0.0191 2 1 d . . .
H1c13 H 0.517953 0.446228 0.032592 Uiso 0.0233 2 1 d . . .
H2c13 H 0.619806 0.416255 0.049887 Uiso 0.0233 2 1 d . . .
H3c13 H 0.581286 0.44969 0.106022 Uiso 0.0233 2 1 d . . .
H1c15 H 0.477609 0.495257 0.229782 Uiso 0.0197 2 1 d . . .
H1c16 H 0.480561 0.361444 0.287454 Uiso 0.0212 2 1 d . . .
H1c17 H 0.660167 0.358449 0.331534 Uiso 0.0182 2 1 d . . .
H1c19 H 0.784226 0.805863 0.129506 Uiso 0.0207 2 1 d . . .
H2c19 H 0.728981 0.854703 0.167282 Uiso 0.0207 2 1 d . . .
H1c20 H 0.906527 0.994623 0.159062 Uiso 0.0306 2 1 d . . .
H2c20 H 0.920191 0.993255 0.233322 Uiso 0.0306 2 1 d . . .
H3c20 H 0.977989 0.942708 0.198081 Uiso 0.0306 2 1 d . . .
H1c21 H 0.873197 0.906946 0.320017 Uiso 0.0211 2 1 d . . .
H2c21 H 0.743953 0.868236 0.282441 Uiso 0.0211 2 1 d . . .
H1c22 H 0.769199 0.831497 0.38866 Uiso 0.0267 2 1 d . . .
H2c22 H 0.680564 0.723731 0.334731 Uiso 0.0267 2 1 d . . .
H3c22 H 0.813316 0.752585 0.369545 Uiso 0.0267 2 1 d . . .
H1c23 H 1.130331 0.539153 0.276128 Uiso 0.0209 2 1 d . . .
H2c23 H 1.144938 0.61718 0.332054 Uiso 0.0209 2 1 d . . .
H1c24 H 1.1699 0.472158 0.367424 Uiso 0.0315 2 1 d . . .
H2c24 H 1.071159 0.481246 0.388635 Uiso 0.0315 2 1 d . . .
H3c24 H 1.034438 0.39184 0.327477 Uiso 0.0315 2 1 d . . .
H1c25 H 0.913559 0.413121 0.167361 Uiso 0.019 2 1 d . . .
H2c25 H 0.912463 0.354558 0.223835 Uiso 0.019 2 1 d . . .
H1c26 H 0.720453 0.277181 0.139587 Uiso 0.0244 2 1 d . . .
H2c26 H 0.716794 0.306187 0.209841 Uiso 0.0244 2 1 d . . .
H3c26 H 0.717155 0.383061 0.160887 Uiso 0.0244 2 1 d . . .
H1c28 H -0.001054 0.191164 0.172797 Uiso 0.0219 2 1 d . . .
H1c29 H -0.207902 0.11767 0.129862 Uiso 0.0274 2 1 d . . .
H1c30 H -0.295391 0.159743 0.033825 Uiso 0.0291 2 1 d . . .
H1c31 H -0.171362 0.281185 -0.017253 Uiso 0.0281 2 1 d . . .
H1c32 H 0.035395 0.353969 0.026067 Uiso 0.0232 2 1 d . . .
H1c34 H 0.033623 0.147493 0.014695 Uiso 0.0207 2 1 d . . .
H1c35 H 0.067024 0.037685 -0.05251 Uiso 0.0249 2 1 d . . .
H1c36 H 0.26166 0.073871 -0.038891 Uiso 0.025 2 1 d . . .
H1c37 H 0.424068 0.220362 0.04552 Uiso 0.0235 2 1 d . . .
H1c38 H 0.388884 0.323833 0.116 Uiso 0.0204 2 1 d . . .
H1c40 H 0.167847 0.490585 0.17964 Uiso 0.0219 2 1 d . . .
H1c41 H 0.265747 0.677403 0.188971 Uiso 0.0274 2 1 d . . .
H1c42 H 0.414149 0.758714 0.140762 Uiso 0.0266 2 1 d . . .
H1c43 H 0.463332 0.647632 0.084798 Uiso 0.0229 2 1 d . . .
H1c44 H 0.369875 0.461075 0.079588 Uiso 0.0185 2 1 d . . .
H1c46 H 0.204073 0.143557 0.164185 Uiso 0.0259 2 1 d . . .
H1c47 H 0.250436 0.095198 0.265023 Uiso 0.0317 2 1 d . . .
H1c48 H 0.302605 0.213421 0.363957 Uiso 0.0319 2 1 d . . .
H1c49 H 0.306654 0.379624 0.360036 Uiso 0.0303 2 1 d . . .
H1c50 H 0.262445 0.428951 0.259378 Uiso 0.0242 2 1 d . . .
H1c52 H 0.857244 0.283231 0.406261 Uiso 0.0213 2 1 d . . .
H1c53 H 0.883581 0.434061 0.473307 Uiso 0.0268 2 1 d . . .
H1c54 H 0.719131 0.433028 0.493143 Uiso 0.0298 2 1 d . . .
H1c55 H 0.528588 0.280442 0.443102 Uiso 0.0282 2 1 d . . .
H1c56 H 0.50209 0.130985 0.375041 Uiso 0.0238 2 1 d . . .
H1c58 H 0.590122 0.036173 0.448815 Uiso 0.0268 2 1 d . . .
H1c59 H 0.475665 -0.122497 0.479317 Uiso 0.033 2 1 d . . .
H1c60 H 0.390622 -0.292898 0.408788 Uiso 0.033 2 1 d . . .
H1c61 H 0.422893 -0.300901 0.307401 Uiso 0.0311 2 1 d . . .
H1c62 H 0.533574 -0.141824 0.276162 Uiso 0.0249 2 1 d . . .
H1c64 H 0.833188 0.166439 0.276476 Uiso 0.0227 2 1 d . . .
H1c65 H 1.03113 0.20459 0.305703 Uiso 0.0259 2 1 d . . .
H1c66 H 1.115474 0.156211 0.400027 Uiso 0.0271 2 1 d . . .
H1c67 H 0.996859 0.065469 0.462588 Uiso 0.025 2 1 d . . .
H1c68 H 0.798882 0.026361 0.432446 Uiso 0.0211 2 1 d . . .
H1c70 H 0.523125 0.168414 0.268896 Uiso 0.0207 2 1 d . . .
H1c71 H 0.435986 0.157907 0.157629 Uiso 0.0257 2 1 d . . .
H1c72 H 0.450619 0.052445 0.076037 Uiso 0.0291 2 1 d . . .
H1c73 H 0.556575 -0.0407 0.10824 Uiso 0.0281 2 1 d . . .
H1c74 H 0.647604 -0.026302 0.219627 Uiso 0.0247 2 1 d . . .
H1n5 H 0.5994(18) 0.6603(15) 0.1993(9) Uiso 0.031(5) 2 1 d . . .
H1n6 H 0.8592(18) 0.4298(17) 0.3299(9) Uiso 0.034(6) 2 1 d . . .
H1n3 H 0.9170(18) 0.7473(16) 0.0772(10) Uiso 0.034(6) 2 1 d . . .
H1n2 H 1.228(2) 0.8205(17) 0.3541(10) Uiso 0.040(6) 2 1 d . . .
H1c76 H 0.541464 0.506169 0.417085 Uiso 0.0945 2 0.5 d . . .
H2c76 H 0.515127 0.591657 0.407178 Uiso 0.0945 2 0.5 d . . .
H1c77 H 0.519801 0.464033 0.541776 Uiso 0.0845 2 0.5 d . . .
H2c77 H 0.474607 0.398721 0.484786 Uiso 0.0845 2 0.5 d . . .
H1c75a H 0.684442 0.684039 0.450901 Uiso 0.1773 2 0.5 d . . .
H2c75a H 0.65365 0.672252 0.515921 Uiso 0.1773 2 0.5 d . . .
H3c75a H 0.696081 0.597182 0.488927 Uiso 0.1773 2 0.5 d . . .
H1c75b H 0.722245 0.634786 0.502862 Uiso 0.1773 2 0.5 d . . .
H2c75b H 0.635633 0.610044 0.430927 Uiso 0.1773 2 0.5 d . . .
H3c75b H 0.661052 0.705329 0.484718 Uiso 0.1773 2 0.5 d . . .




#==============================================================================0

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N1 . . 2.0269(14) ?
Fe1 P1 . . 2.2800(6) ?
Fe1 P2 . . 2.2875(6) ?
Fe1 P3 . . 2.2892(6) ?
Fe1 P4 . . 2.3099(6) ?
Fe1 N4 . . 2.0143(13) ?
N1 C1 . . 1.3604(18) ?
N1 C5 . . 1.362(2) ?
N2 P1 . . 1.7096(18) ?
N2 C1 . . 1.380(2) ?
N3 P2 . . 1.7049(14) ?
N3 C5 . . 1.3765(18) ?
N3 H1n3 . . 0.83(2) ?
P1 C6 . . 1.8258(17) ?
P1 C8 . . 1.8429(19) ?
P2 C10 . . 1.840(2) ?
P2 C12 . . 1.8229(16) ?
C1 C2 . . 1.383(2) ?
C2 C3 . . 1.383(3) ?
C2 H1c2 . . 0.96 ?
C3 C4 . . 1.380(2) ?
C3 H1c3 . . 0.96 ?
C4 C5 . . 1.391(2) ?
C4 H1c4 . . 0.96 ?
C6 C7 . . 1.530(3) ?
C6 H1c6 . . 0.96 ?
C6 H2c6 . . 0.96 ?
C7 H1c7 . . 0.96 ?
C7 H2c7 . . 0.96 ?
C7 H3c7 . . 0.96 ?
C8 C9 . . 1.5348(19) ?
C8 H1c8 . . 0.96 ?
C8 H2c8 . . 0.96 ?
C9 H1c9 . . 0.96 ?
C9 H2c9 . . 0.96 ?
C9 H3c9 . . 0.96 ?
C10 C11 . . 1.522(3) ?
C10 H1c10 . . 0.96 ?
C10 H2c10 . . 0.96 ?
C11 H1c11 . . 0.96 ?
C11 H2c11 . . 0.96 ?
C11 H3c11 . . 0.96 ?
C12 C13 . . 1.530(2) ?
C12 H1c12 . . 0.96 ?
C12 H2c12 . . 0.96 ?
C13 H1c13 . . 0.96 ?
C13 H2c13 . . 0.96 ?
C13 H3c13 . . 0.96 ?
P3 N5 . . 1.7095(12) ?
P3 C19 . . 1.8217(18) ?
P3 C21 . . 1.8408(19) ?
P4 N6 . . 1.7144(15) ?
P4 C23 . . 1.8368(18) ?
P4 C25 . . 1.8403(16) ?
N4 C14 . . 1.363(2) ?
N4 C18 . . 1.354(2) ?
N5 C14 . . 1.384(2) ?
N5 H1n5 . . 0.89(3) ?
N6 C18 . . 1.392(2) ?
N6 H1n6 . . 0.85(2) ?
C14 C15 . . 1.386(2) ?
C15 C16 . . 1.379(3) ?
C15 H1c15 . . 0.96 ?
C16 C17 . . 1.384(3) ?
C16 H1c16 . . 0.96 ?
C17 C18 . . 1.386(2) ?
C17 H1c17 . . 0.96 ?
C19 C20 . . 1.5307(19) ?
C19 H1c19 . . 0.96 ?
C19 H2c19 . . 0.96 ?
C20 H1c20 . . 0.96 ?
C20 H2c20 . . 0.96 ?
C20 H3c20 . . 0.96 ?
C21 C22 . . 1.521(2) ?
C21 H1c21 . . 0.96 ?
C21 H2c21 . . 0.96 ?
C22 H1c22 . . 0.96 ?
C22 H2c22 . . 0.96 ?
C22 H3c22 . . 0.96 ?
C23 C24 . . 1.528(3) ?
C23 H1c23 . . 0.96 ?
C23 H2c23 . . 0.96 ?
C24 H1c24 . . 0.96 ?
C24 H2c24 . . 0.96 ?
C24 H3c24 . . 0.96 ?
C25 C26 . . 1.528(2) ?
C25 H1c25 . . 0.96 ?
C25 H2c25 . . 0.96 ?
C26 H1c26 . . 0.96 ?
C26 H2c26 . . 0.96 ?
C26 H3c26 . . 0.96 ?
B1 C27 . . 1.643(3) ?
B1 C33 . . 1.650(3) ?
B1 C39 . . 1.651(2) ?
C27 C28 . . 1.399(2) ?
C27 C32 . . 1.405(2) ?
C28 C29 . . 1.395(2) ?
C28 H1c28 . . 0.96 ?
C29 C30 . . 1.384(3) ?
C29 H1c29 . . 0.96 ?
C30 C31 . . 1.391(3) ?
C30 H1c30 . . 0.96 ?
C31 C32 . . 1.393(2) ?
C31 H1c31 . . 0.96 ?
C32 H1c32 . . 0.96 ?
C33 C34 . . 1.4020(17) ?
C33 C38 . . 1.403(3) ?
C34 C35 . . 1.396(3) ?
C34 H1c34 . . 0.96 ?
C35 C36 . . 1.378(3) ?
C35 H1c35 . . 0.96 ?
C36 C37 . . 1.3928(18) ?
C36 H1c36 . . 0.96 ?
C37 C38 . . 1.393(3) ?
C37 H1c37 . . 0.96 ?
C38 H1c38 . . 0.96 ?
C39 C40 . . 1.403(3) ?
C39 C44 . . 1.401(2) ?
C40 C41 . . 1.389(2) ?
C40 H1c40 . . 0.96 ?
C41 C42 . . 1.387(3) ?
C41 H1c41 . . 0.96 ?
C42 C43 . . 1.382(3) ?
C42 H1c42 . . 0.96 ?
C43 C44 . . 1.398(2) ?
C43 H1c43 . . 0.96 ?
C44 H1c44 . . 0.96 ?
C45 C46 . . 1.406(3) ?
C45 C50 . . 1.400(2) ?
C46 C47 . . 1.395(3) ?
C46 H1c46 . . 0.96 ?
C47 C48 . . 1.384(3) ?
C47 H1c47 . . 0.96 ?
C48 C49 . . 1.379(3) ?
C48 H1c48 . . 0.96 ?
C49 C50 . . 1.396(3) ?
C49 H1c49 . . 0.96 ?
C50 H1c50 . . 0.96 ?
B2 C51 . . 1.653(3) ?
B2 C57 . . 1.655(2) ?
B2 C63 . . 1.644(3) ?
B2 C69 . . 1.654(2) ?
C51 C52 . . 1.4000(18) ?
C51 C56 . . 1.410(3) ?
C52 C53 . . 1.395(3) ?
C52 H1c52 . . 0.96 ?
C53 C54 . . 1.383(3) ?
C53 H1c53 . . 0.96 ?
C54 C55 . . 1.380(2) ?
C54 H1c54 . . 0.96 ?
C55 C56 . . 1.390(3) ?
C55 H1c55 . . 0.96 ?
C56 H1c56 . . 0.96 ?
C57 C58 . . 1.402(3) ?
C57 C62 . . 1.406(2) ?
C58 C59 . . 1.395(3) ?
C58 H1c58 . . 0.96 ?
C59 C60 . . 1.383(3) ?
C59 H1c59 . . 0.96 ?
C60 C61 . . 1.387(3) ?
C60 H1c60 . . 0.96 ?
C61 C62 . . 1.392(2) ?
C61 H1c61 . . 0.96 ?
C62 H1c62 . . 0.96 ?
C63 C64 . . 1.403(2) ?
C63 C68 . . 1.406(2) ?
C64 C65 . . 1.395(3) ?
C64 H1c64 . . 0.96 ?
C65 C66 . . 1.386(3) ?
C65 H1c65 . . 0.96 ?
C66 C67 . . 1.388(3) ?
C66 H1c66 . . 0.96 ?
C67 C68 . . 1.391(3) ?
C67 H1c67 . . 0.96 ?
C68 H1c68 . . 0.96 ?
C69 C70 . . 1.401(3) ?
C69 C74 . . 1.408(3) ?
C70 C71 . . 1.395(2) ?
C70 H1c70 . . 0.96 ?
C71 C72 . . 1.381(3) ?
C71 H1c71 . . 0.96 ?
C72 C73 . . 1.389(3) ?
C72 H1c72 . . 0.96 ?
C73 C74 . . 1.392(2) ?
C73 H1c73 . . 0.96 ?
C74 H1c74 . . 0.96 ?
O1 C76 . . 1.484(10) ?
O1 C77 . . 1.319(8) ?
O1 C77 . 2_666 1.121(9) ?
C75 C76 . . 1.262(6) ?
C75 C77 . 2_666 1.415(9) ?
C76 C77 . 2_666 1.079(9) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Fe1 P1 . . . 78.79(3) ?
N1 Fe1 P2 . . . 79.14(3) ?
N1 Fe1 P3 . . . 100.77(5) ?
N1 Fe1 P4 . . . 100.82(5) ?
N1 Fe1 N4 . . . 178.42(4) ?
P1 Fe1 P2 . . . 157.929(18) ?
P1 Fe1 P3 . . . 96.038(19) ?
P1 Fe1 P4 . . . 87.608(18) ?
P1 Fe1 N4 . . . 102.79(3) ?
P2 Fe1 P3 . . . 87.655(18) ?
P2 Fe1 P4 . . . 96.943(18) ?
P2 Fe1 N4 . . . 99.28(3) ?
P3 Fe1 P4 . . . 158.396(18) ?
P3 Fe1 N4 . . . 79.00(5) ?
P4 Fe1 N4 . . . 79.43(5) ?
Fe1 N1 C1 . . . 121.30(11) ?
Fe1 N1 C5 . . . 121.10(9) ?
C1 N1 C5 . . . 117.55(13) ?
P1 N2 C1 . . . 114.86(12) ?
P2 N3 C5 . . . 114.81(12) ?
P2 N3 H1n3 . . . 122.6(11) ?
C5 N3 H1n3 . . . 113.9(13) ?
Fe1 P1 N2 . . . 96.97(5) ?
Fe1 P1 C6 . . . 127.05(4) ?
Fe1 P1 C8 . . . 121.55(5) ?
N2 P1 C6 . . . 102.64(8) ?
N2 P1 C8 . . . 100.61(8) ?
C6 P1 C8 . . . 102.47(8) ?
Fe1 P2 N3 . . . 96.92(4) ?
Fe1 P2 C10 . . . 124.44(5) ?
Fe1 P2 C12 . . . 127.81(6) ?
N3 P2 C10 . . . 100.19(8) ?
N3 P2 C12 . . . 102.21(7) ?
C10 P2 C12 . . . 99.29(7) ?
N1 C1 N2 . . . 113.88(14) ?
N1 C1 C2 . . . 122.98(15) ?
N2 C1 C2 . . . 123.14(13) ?
C1 C2 C3 . . . 118.08(14) ?
C1 C2 H1c2 . . . 120.96 ?
C3 C2 H1c2 . . . 120.96 ?
C2 C3 C4 . . . 120.61(17) ?
C2 C3 H1c3 . . . 119.7 ?
C4 C3 H1c3 . . . 119.7 ?
C3 C4 C5 . . . 118.28(16) ?
C3 C4 H1c4 . . . 120.86 ?
C5 C4 H1c4 . . . 120.86 ?
N1 C5 N3 . . . 114.26(14) ?
N1 C5 C4 . . . 122.40(13) ?
N3 C5 C4 . . . 123.28(15) ?
P1 C6 C7 . . . 113.18(13) ?
P1 C6 H1c6 . . . 109.47 ?
P1 C6 H2c6 . . . 109.47 ?
C7 C6 H1c6 . . . 109.47 ?
C7 C6 H2c6 . . . 109.47 ?
H1c6 C6 H2c6 . . . 105.49 ?
C6 C7 H1c7 . . . 109.47 ?
C6 C7 H2c7 . . . 109.47 ?
C6 C7 H3c7 . . . 109.47 ?
H1c7 C7 H2c7 . . . 109.47 ?
H1c7 C7 H3c7 . . . 109.47 ?
H2c7 C7 H3c7 . . . 109.47 ?
P1 C8 C9 . . . 114.77(15) ?
P1 C8 H1c8 . . . 109.47 ?
P1 C8 H2c8 . . . 109.47 ?
C9 C8 H1c8 . . . 109.47 ?
C9 C8 H2c8 . . . 109.47 ?
H1c8 C8 H2c8 . . . 103.6 ?
C8 C9 H1c9 . . . 109.47 ?
C8 C9 H2c9 . . . 109.47 ?
C8 C9 H3c9 . . . 109.47 ?
H1c9 C9 H2c9 . . . 109.47 ?
H1c9 C9 H3c9 . . . 109.47 ?
H2c9 C9 H3c9 . . . 109.47 ?
P2 C10 C11 . . . 113.20(10) ?
P2 C10 H1c10 . . . 109.47 ?
P2 C10 H2c10 . . . 109.47 ?
C11 C10 H1c10 . . . 109.47 ?
C11 C10 H2c10 . . . 109.47 ?
H1c10 C10 H2c10 . . . 105.46 ?
C10 C11 H1c11 . . . 109.47 ?
C10 C11 H2c11 . . . 109.47 ?
C10 C11 H3c11 . . . 109.47 ?
H1c11 C11 H2c11 . . . 109.47 ?
H1c11 C11 H3c11 . . . 109.47 ?
H2c11 C11 H3c11 . . . 109.47 ?
P2 C12 C13 . . . 111.80(13) ?
P2 C12 H1c12 . . . 109.47 ?
P2 C12 H2c12 . . . 109.47 ?
C13 C12 H1c12 . . . 109.47 ?
C13 C12 H2c12 . . . 109.47 ?
H1c12 C12 H2c12 . . . 107.04 ?
C12 C13 H1c13 . . . 109.47 ?
C12 C13 H2c13 . . . 109.47 ?
C12 C13 H3c13 . . . 109.47 ?
H1c13 C13 H2c13 . . . 109.47 ?
H1c13 C13 H3c13 . . . 109.47 ?
H2c13 C13 H3c13 . . . 109.47 ?
Fe1 P3 N5 . . . 96.77(6) ?
Fe1 P3 C19 . . . 125.35(7) ?
Fe1 P3 C21 . . . 126.74(6) ?
N5 P3 C19 . . . 104.65(7) ?
N5 P3 C21 . . . 99.69(7) ?
C19 P3 C21 . . . 98.54(9) ?
Fe1 P4 N6 . . . 95.96(6) ?
Fe1 P4 C23 . . . 126.29(5) ?
Fe1 P4 C25 . . . 125.71(6) ?
N6 P4 C23 . . . 104.76(7) ?
N6 P4 C25 . . . 100.42(7) ?
C23 P4 C25 . . . 98.71(8) ?
Fe1 N4 C14 . . . 121.08(10) ?
Fe1 N4 C18 . . . 121.41(12) ?
C14 N4 C18 . . . 117.47(13) ?
P3 N5 C14 . . . 114.60(10) ?
P3 N5 H1n5 . . . 120.5(11) ?
C14 N5 H1n5 . . . 114.6(13) ?
P4 N6 C18 . . . 114.13(11) ?
P4 N6 H1n6 . . . 120.4(18) ?
C18 N6 H1n6 . . . 112.7(16) ?
N4 C14 N5 . . . 114.41(13) ?
N4 C14 C15 . . . 122.56(16) ?
N5 C14 C15 . . . 123.02(17) ?
C14 C15 C16 . . . 118.46(17) ?
C14 C15 H1c15 . . . 120.77 ?
C16 C15 H1c15 . . . 120.77 ?
C15 C16 C17 . . . 120.28(15) ?
C15 C16 H1c16 . . . 119.86 ?
C17 C16 H1c16 . . . 119.86 ?
C16 C17 C18 . . . 118.20(16) ?
C16 C17 H1c17 . . . 120.9 ?
C18 C17 H1c17 . . . 120.9 ?
N4 C18 N6 . . . 114.55(13) ?
N4 C18 C17 . . . 122.96(17) ?
N6 C18 C17 . . . 122.46(16) ?
P3 C19 C20 . . . 110.54(11) ?
P3 C19 H1c19 . . . 109.47 ?
P3 C19 H2c19 . . . 109.47 ?
C20 C19 H1c19 . . . 109.47 ?
C20 C19 H2c19 . . . 109.47 ?
H1c19 C19 H2c19 . . . 108.38 ?
C19 C20 H1c20 . . . 109.47 ?
C19 C20 H2c20 . . . 109.47 ?
C19 C20 H3c20 . . . 109.47 ?
H1c20 C20 H2c20 . . . 109.47 ?
H1c20 C20 H3c20 . . . 109.47 ?
H2c20 C20 H3c20 . . . 109.47 ?
P3 C21 C22 . . . 115.18(13) ?
P3 C21 H1c21 . . . 109.47 ?
P3 C21 H2c21 . . . 109.47 ?
C22 C21 H1c21 . . . 109.47 ?
C22 C21 H2c21 . . . 109.47 ?
H1c21 C21 H2c21 . . . 103.09 ?
C21 C22 H1c22 . . . 109.47 ?
C21 C22 H2c22 . . . 109.47 ?
C21 C22 H3c22 . . . 109.47 ?
H1c22 C22 H2c22 . . . 109.47 ?
H1c22 C22 H3c22 . . . 109.47 ?
H2c22 C22 H3c22 . . . 109.47 ?
P4 C23 C24 . . . 116.01(11) ?
P4 C23 H1c23 . . . 109.47 ?
P4 C23 H2c23 . . . 109.47 ?
C24 C23 H1c23 . . . 109.47 ?
C24 C23 H2c23 . . . 109.47 ?
H1c23 C23 H2c23 . . . 102.03 ?
C23 C24 H1c24 . . . 109.47 ?
C23 C24 H2c24 . . . 109.47 ?
C23 C24 H3c24 . . . 109.47 ?
H1c24 C24 H2c24 . . . 109.47 ?
H1c24 C24 H3c24 . . . 109.47 ?
H2c24 C24 H3c24 . . . 109.47 ?
P4 C25 C26 . . . 113.85(14) ?
P4 C25 H1c25 . . . 109.47 ?
P4 C25 H2c25 . . . 109.47 ?
C26 C25 H1c25 . . . 109.47 ?
C26 C25 H2c25 . . . 109.47 ?
H1c25 C25 H2c25 . . . 104.7 ?
C25 C26 H1c26 . . . 109.47 ?
C25 C26 H2c26 . . . 109.47 ?
C25 C26 H3c26 . . . 109.47 ?
H1c26 C26 H2c26 . . . 109.47 ?
H1c26 C26 H3c26 . . . 109.47 ?
H2c26 C26 H3c26 . . . 109.47 ?
C27 B1 C33 . . . 108.26(11) ?
C27 B1 C39 . . . 108.40(16) ?
C33 B1 C39 . . . 112.21(14) ?
B1 C27 C28 . . . 123.90(15) ?
B1 C27 C32 . . . 120.41(14) ?
C28 C27 C32 . . . 115.44(15) ?
C27 C28 C29 . . . 122.48(16) ?
C27 C28 H1c28 . . . 118.76 ?
C29 C28 H1c28 . . . 118.76 ?
C28 C29 C30 . . . 120.38(16) ?
C28 C29 H1c29 . . . 119.81 ?
C30 C29 H1c29 . . . 119.81 ?
C29 C30 C31 . . . 119.06(16) ?
C29 C30 H1c30 . . . 120.47 ?
C31 C30 H1c30 . . . 120.47 ?
C30 C31 C32 . . . 119.71(17) ?
C30 C31 H1c31 . . . 120.15 ?
C32 C31 H1c31 . . . 120.15 ?
C27 C32 C31 . . . 122.89(16) ?
C27 C32 H1c32 . . . 118.56 ?
C31 C32 H1c32 . . . 118.56 ?
B1 C33 C34 . . . 123.39(16) ?
B1 C33 C38 . . . 121.13(11) ?
C34 C33 C38 . . . 115.17(17) ?
C33 C34 C35 . . . 122.53(18) ?
C33 C34 H1c34 . . . 118.74 ?
C35 C34 H1c34 . . . 118.74 ?
C34 C35 C36 . . . 120.47(13) ?
C34 C35 H1c35 . . . 119.76 ?
C36 C35 H1c35 . . . 119.76 ?
C35 C36 C37 . . . 119.05(19) ?
C35 C36 H1c36 . . . 120.47 ?
C37 C36 H1c36 . . . 120.47 ?
C36 C37 C38 . . . 119.64(18) ?
C36 C37 H1c37 . . . 120.18 ?
C38 C37 H1c37 . . . 120.18 ?
C33 C38 C37 . . . 123.09(12) ?
C33 C38 H1c38 . . . 118.45 ?
C37 C38 H1c38 . . . 118.45 ?
B1 C39 C40 . . . 119.90(15) ?
B1 C39 C44 . . . 125.85(17) ?
C40 C39 C44 . . . 114.23(14) ?
C39 C40 C41 . . . 123.44(17) ?
C39 C40 H1c40 . . . 118.28 ?
C41 C40 H1c40 . . . 118.28 ?
C40 C41 C42 . . . 120.3(2) ?
C40 C41 H1c41 . . . 119.83 ?
C42 C41 H1c41 . . . 119.83 ?
C41 C42 C43 . . . 118.40(16) ?
C41 C42 H1c42 . . . 120.8 ?
C43 C42 H1c42 . . . 120.8 ?
C42 C43 C44 . . . 120.28(17) ?
C42 C43 H1c43 . . . 119.86 ?
C44 C43 H1c43 . . . 119.86 ?
C39 C44 C43 . . . 123.27(18) ?
C39 C44 H1c44 . . . 118.37 ?
C43 C44 H1c44 . . . 118.36 ?
C46 C45 C50 . . . 115.24(16) ?
C45 C46 C47 . . . 122.68(17) ?
C45 C46 H1c46 . . . 118.66 ?
C47 C46 H1c46 . . . 118.66 ?
C46 C47 C48 . . . 120.1(2) ?
C46 C47 H1c47 . . . 119.94 ?
C48 C47 H1c47 . . . 119.94 ?
C47 C48 C49 . . . 118.95(18) ?
C47 C48 H1c48 . . . 120.53 ?
C49 C48 H1c48 . . . 120.53 ?
C48 C49 C50 . . . 120.53(17) ?
C48 C49 H1c49 . . . 119.74 ?
C50 C49 H1c49 . . . 119.73 ?
C45 C50 C49 . . . 122.49(19) ?
C45 C50 H1c50 . . . 118.76 ?
C49 C50 H1c50 . . . 118.76 ?
C51 B2 C57 . . . 110.43(15) ?
C51 B2 C63 . . . 106.71(11) ?
C51 B2 C69 . . . 110.18(15) ?
C57 B2 C63 . . . 108.77(15) ?
C57 B2 C69 . . . 110.02(10) ?
C63 B2 C69 . . . 110.67(15) ?
B2 C51 C52 . . . 123.09(18) ?
B2 C51 C56 . . . 122.21(12) ?
C52 C51 C56 . . . 114.70(16) ?
C51 C52 C53 . . . 123.21(19) ?
C51 C52 H1c52 . . . 118.39 ?
C53 C52 H1c52 . . . 118.39 ?
C52 C53 C54 . . . 119.92(14) ?
C52 C53 H1c53 . . . 120.04 ?
C54 C53 H1c53 . . . 120.04 ?
C53 C54 C55 . . . 118.98(19) ?
C53 C54 H1c54 . . . 120.51 ?
C55 C54 H1c54 . . . 120.51 ?
C54 C55 C56 . . . 120.5(2) ?
C54 C55 H1c55 . . . 119.75 ?
C56 C55 H1c55 . . . 119.75 ?
C51 C56 C55 . . . 122.66(14) ?
C51 C56 H1c56 . . . 118.67 ?
C55 C56 H1c56 . . . 118.67 ?
B2 C57 C58 . . . 123.16(13) ?
B2 C57 C62 . . . 121.97(15) ?
C58 C57 C62 . . . 114.79(15) ?
C57 C58 C59 . . . 123.13(16) ?
C57 C58 H1c58 . . . 118.43 ?
C59 C58 H1c58 . . . 118.44 ?
C58 C59 C60 . . . 120.08(19) ?
C58 C59 H1c59 . . . 119.96 ?
C60 C59 H1c59 . . . 119.96 ?
C59 C60 C61 . . . 118.85(17) ?
C59 C60 H1c60 . . . 120.58 ?
C61 C60 H1c60 . . . 120.58 ?
C60 C61 C62 . . . 120.32(16) ?
C60 C61 H1c61 . . . 119.84 ?
C62 C61 H1c61 . . . 119.84 ?
C57 C62 C61 . . . 122.81(17) ?
C57 C62 H1c62 . . . 118.59 ?
C61 C62 H1c62 . . . 118.59 ?
B2 C63 C64 . . . 123.32(15) ?
B2 C63 C68 . . . 121.17(15) ?
C64 C63 C68 . . . 115.09(16) ?
C63 C64 C65 . . . 123.03(16) ?
C63 C64 H1c64 . . . 118.49 ?
C65 C64 H1c64 . . . 118.49 ?
C64 C65 C66 . . . 119.82(17) ?
C64 C65 H1c65 . . . 120.09 ?
C66 C65 H1c65 . . . 120.09 ?
C65 C66 C67 . . . 119.13(18) ?
C65 C66 H1c66 . . . 120.43 ?
C67 C66 H1c66 . . . 120.43 ?
C66 C67 C68 . . . 120.20(17) ?
C66 C67 H1c67 . . . 119.9 ?
C68 C67 H1c67 . . . 119.9 ?
C63 C68 C67 . . . 122.73(16) ?
C63 C68 H1c68 . . . 118.64 ?
C67 C68 H1c68 . . . 118.64 ?
B2 C69 C70 . . . 123.38(16) ?
B2 C69 C74 . . . 121.79(17) ?
C70 C69 C74 . . . 114.82(14) ?
C69 C70 C71 . . . 123.09(18) ?
C69 C70 H1c70 . . . 118.46 ?
C71 C70 H1c70 . . . 118.46 ?
C70 C71 C72 . . . 120.24(19) ?
C70 C71 H1c71 . . . 119.88 ?
C72 C71 H1c71 . . . 119.88 ?
C71 C72 C73 . . . 118.81(16) ?
C71 C72 H1c72 . . . 120.6 ?
C73 C72 H1c72 . . . 120.6 ?
C72 C73 C74 . . . 120.23(19) ?
C72 C73 H1c73 . . . 119.88 ?
C74 C73 H1c73 . . . 119.88 ?
C69 C74 C73 . . . 122.8(2) ?
C69 C74 H1c74 . . . 118.6 ?
C73 C74 H1c74 . . . 118.6 ?
C76 O1 C77 . . . 118.4(7) ?
C76 O1 C77 . . 2_666 46.4(4) ?
C77 O1 C77 . . 2_666 91.5(6) ?
C76 C75 C77 . . 2_666 47.1(4) ?
O1 C76 C75 . . . 120.4(6) ?
O1 C76 C77 . . 2_666 48.8(5) ?
C75 C76 C77 . . 2_666 73.9(5) ?
O1 C77 O1 . . 2_666 88.5(5) ?
O1 C77 C75 . . 2_666 126.4(8) ?
O1 C77 C76 . . 2_666 128.8(7) ?
O1 C77 C75 2_666 . 2_666 140.1(6) ?
O1 C77 C76 2_666 . 2_666 84.8(6) ?
C75 C77 C76 2_666 . 2_666 59.0(5) ?
O1 H1c77 C76 2_666 . 2_666 159.01 ?
O1 H1c77 C77 2_666 . . 89.15 ?
C76 H1c77 C77 2_666 . . 70.21 ?
_database_code_depnum_ccdc_archive 'CCDC 1005386'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Fe-bisPNPiPr
#=======================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C34 H66 Fe N6 P4, 2(B F4), 2(C3 H6 O)'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C40 H78 B2 F8 Fe1 N6 O2 P4'
_chemical_formula_weight         1028.5
_chemical_melting_point          ?
_chemical_compound_source        ?
_chemical_absolute_configuration .

#=======================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C c c e'
# this corresponds to   C c c b:1 
_symmetry_space_group_name_Hall  'C 2 2 -1bc '
# JANA _symmetry_space_group_name_Hall          '-C -2xac;-2yc;-2za'
_symmetry_Int_Tables_number      68

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,-y+1/2,z
3 -x,y,-z
4 x+1/2,-y+1/2,-z
5 -x,-y+1/2,-z+1/2
6 x+1/2,y,-z+1/2
7 x,-y+1/2,z+1/2
8 -x+1/2,y,z+1/2
9 x+1/2,y+1/2,z
10 -x,-y,z
11 -x+1/2,y+1/2,-z
12 x,-y,-z
13 -x+1/2,-y,-z+1/2
14 x,y+1/2,-z+1/2
15 x+1/2,-y,z+1/2
16 -x,y+1/2,z+1/2

_cell_length_a                   15.1780(6)
_cell_length_b                   21.4529(9)
_cell_length_c                   16.2363(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5286.7(4)


_cell_formula_units_Z            4

_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_cell_measurement_temperature    100
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.2921
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2176

_exptl_absorpt_coefficient_mu    0.473
_exptl_crystal_description       parallelepiped
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.10
_exptl_crystal_size_rad          ?
_exptl_crystal_colour            'translucent red'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_T_max  0.95

#=======================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           ?

_diffrn_ambient_temperature      100
_diffrn_source                   ?
_diffrn_source_power             ?
_diffrn_source_voltage           ?
_diffrn_source_current           ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD'
_diffrn_detector                 ?
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_method       ?
_diffrn_measurement_specimen_support ?

_diffrn_reflns_number            36808
_diffrn_reflns_theta_min         1.9
_diffrn_reflns_theta_max         34.93
_diffrn_reflns_theta_full        34.93
_diffrn_measured_fraction_theta_max 1
_diffrn_measured_fraction_theta_full 1
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_reduction_process ?


_diffrn_radiation_probe          X-ray

#=======================================================================

# 8. REFINEMENT DATA

_refine_special_details          
; ?
;

_reflns_number_total             5789
_reflns_number_gt                4405
_reflns_threshold_expression     I>3σ(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_gt          0.1036
_refine_ls_R_factor_all          0.0588
_refine_ls_wR_factor_ref         0.1117
_refine_ls_goodness_of_fit_ref   1.63
_refine_ls_goodness_of_fit_gt    1.74
_refine_ls_restrained_S_gt       ?
_refine_ls_restrained_S_all      ?
_refine_ls_number_reflns         5789
_refine_ls_number_parameters     150
_refine_ls_number_restraints     1
_refine_ls_number_constraints    74
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     w=1/(σ²(I)+0.0016I²)
_refine_ls_hydrogen_treatment    mixed
_refine_ls_shift/su_max          0.0185
_refine_ls_shift/su_mean         0.0018
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.29

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
B 0.0013 0.0007 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
F 0.0171 0.0103 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
Fe 0.3463 0.8444 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
P 0.1023 0.0942 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  ?
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_restr_distance_atom_site_label_1
_restr_distance_site_symmetry_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
N2 . H1n2 . 0.87 0.001

# no other restraints


#=======================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0 0.5 0.5 Uani 0.00846(7) 4 1 d . . .
P1 P -0.032526(19) 0.423493(13) 0.407950(17) Uani 0.01114(7) 16 1 d . . .
N1 N 0.13386(9) 0.5 0.5 Uani 0.0109(3) 8 1 d . . .
N2 N -0.12802(6) 0.39904(4) 0.45352(6) Uani 0.0129(2) 16 1 d . . .
C1 C 0.18038(7) 0.44825(5) 0.52188(7) Uani 0.0116(2) 16 1 d . . .
C2 C 0.27193(8) 0.44641(6) 0.52150(7) Uani 0.0151(3) 16 1 d . . .
C3 C 0.31753(11) 0.5 0.5 Uani 0.0163(4) 8 1 d . . .
C4 C 0.02457(8) 0.35027(6) 0.38712(8) Uani 0.0170(3) 16 1 d . . .
C5 C 0.10399(10) 0.35918(7) 0.33075(10) Uani 0.0274(4) 16 1 d . . .
C6 C 0.14944(12) 0.29783(8) 0.31108(12) Uani 0.0382(5) 16 1 d . . .
C7 C -0.07341(8) 0.44489(6) 0.30497(7) Uani 0.0184(3) 16 1 d . . .
C8 C -0.13294(11) 0.39768(8) 0.26234(9) Uani 0.0312(4) 16 1 d . . .
C9 C -0.16323(11) 0.42233(9) 0.17861(9) Uani 0.0354(5) 16 1 d . . .
F1 F -0.18757(8) 0.27919(5) 0.39497(7) Uani 0.0425(3) 16 1 d . . .
F2 F -0.28921(8) 0.29479(5) 0.49442(7) Uani 0.0448(4) 16 1 d . . .
B1 B -0.25 0.25 0.44500(17) Uani 0.0289(7) 8 1 d . . .
O1 O -0.5 0.41812(10) 0.5 Uani 0.0638(9) 8 1 d . . .
C10 C -0.5 0.36302(12) 0.5 Uani 0.0437(9) 8 1 d . . .
C11 C -0.49373(18) 0.32606(15) 0.4223(2) Uani 0.0820(12) 16 1 d . . .
H1c2 H 0.302865 0.408908 0.535786 Uiso 0.0181 16 1 d . . .
H1c4 H 0.043412 0.331978 0.438128 Uiso 0.0204 16 1 d . . .
H2c4 H -0.015681 0.321251 0.362412 Uiso 0.0204 16 1 d . . .
H1c5 H 0.085458 0.378765 0.280483 Uiso 0.0329 16 1 d . . .
H2c5 H 0.145255 0.387 0.356378 Uiso 0.0329 16 1 d . . .
H1c6 H 0.196444 0.305079 0.272696 Uiso 0.0459 16 1 d . . .
H2c6 H 0.172942 0.280191 0.360778 Uiso 0.0459 16 1 d . . .
H3c6 H 0.107629 0.269461 0.287336 Uiso 0.0459 16 1 d . . .
H1c7 H -0.102869 0.484437 0.307827 Uiso 0.0221 16 1 d . . .
H2c7 H -0.02446 0.454623 0.269805 Uiso 0.0221 16 1 d . . .
H1c8 H -0.183424 0.38954 0.2963 Uiso 0.0374 16 1 d . . .
H2c8 H -0.101475 0.359273 0.254831 Uiso 0.0374 16 1 d . . .
H1c9 H -0.200647 0.392045 0.152698 Uiso 0.0425 16 1 d . . .
H2c9 H -0.195285 0.46048 0.186182 Uiso 0.0425 16 1 d . . .
H3c9 H -0.112782 0.429939 0.144397 Uiso 0.0425 16 1 d . . .
H1c11 H -0.44657 0.296444 0.426904 Uiso 0.0983 16 1 d . . .
H2c11 H -0.548182 0.304387 0.413138 Uiso 0.0983 16 1 d . . .
H3c11 H -0.482389 0.353599 0.376919 Uiso 0.0983 16 1 d . . .
H1n2 H -0.1535(10) 0.3654(4) 0.4355(9) Uiso 0.022(4) 16 1 d . . .
H1c3 H 0.380781 0.5 0.5 Uiso 0.0195 8 1 d . . .



#=======================================================================

# 10. MOLECULAR GEOMETRY


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 P1 . . 2.2740(3) ?
Fe1 P1 . 10_565 2.2740(3) ?
Fe1 P1 . 3_556 2.2740(3) ?
Fe1 P1 . 12_566 2.2740(3) ?
Fe1 N1 . . 2.0317(13) ?
Fe1 N1 . 10_565 2.0317(13) ?
P1 N2 . . 1.7098(10) ?
P1 C4 . . 1.8256(12) ?
P1 C7 . . 1.8416(12) ?
N1 C1 . . 1.3628(13) ?
N1 C1 . 12_566 1.3628(13) ?
N2 C1 . 3_556 1.3805(15) ?
N2 F1 . . 2.8863(14) ?
N2 H1n2 . . 0.870(11) ?
C1 C2 . . 1.3901(16) ?
C2 C3 . . 1.3865(14) ?
C2 H1c2 . . 0.96 ?
C3 H1c3 . . 0.96 ?
C4 C5 . . 1.5257(19) ?
C4 H1c4 . . 0.96 ?
C4 H2c4 . . 0.96 ?
C5 C6 . . 1.520(2) ?
C5 H1c5 . . 0.96 ?
C5 H2c5 . . 0.96 ?
C6 H1c6 . . 0.96 ?
C6 H2c6 . . 0.96 ?
C6 H3c6 . . 0.96 ?
C7 C8 . . 1.524(2) ?
C7 H1c7 . . 0.96 ?
C7 H2c7 . . 0.96 ?
C8 C9 . . 1.530(2) ?
C8 H1c8 . . 0.96 ?
C8 H2c8 . . 0.96 ?
C9 H1c9 . . 0.96 ?
C9 H2c9 . . 0.96 ?
C9 H3c9 . . 0.96 ?
F1 B1 . . 1.396(2) ?
F2 B1 . . 1.3861(19) ?
O1 C10 . . 1.182(3) ?
C10 C11 . . 1.493(4) ?
C10 C11 . 3_456 1.493(4) ?
C11 H1c11 . . 0.96 ?
C11 H2c11 . . 0.96 ?
C11 H3c11 . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P1 Fe1 P1 . . 10_565 97.823(10) ?
P1 Fe1 P1 . . 3_556 87.601(10) ?
P1 Fe1 P1 . . 12_566 154.923(10) ?
P1 Fe1 N1 . . . 102.538(7) ?
P1 Fe1 N1 . . 10_565 77.462(7) ?
P1 Fe1 P1 10_565 . 3_556 154.923(10) ?
P1 Fe1 P1 10_565 . 12_566 87.601(10) ?
P1 Fe1 N1 10_565 . . 77.462(7) ?
P1 Fe1 N1 10_565 . 10_565 102.538(7) ?
P1 Fe1 P1 3_556 . 12_566 97.823(10) ?
P1 Fe1 N1 3_556 . . 77.462(7) ?
P1 Fe1 N1 3_556 . 10_565 102.538(7) ?
P1 Fe1 N1 12_566 . . 102.538(7) ?
P1 Fe1 N1 12_566 . 10_565 77.462(7) ?
N1 Fe1 N1 . . 10_565 180.0(5) ?
Fe1 P1 N2 . . . 96.95(3) ?
Fe1 P1 C4 . . . 129.77(4) ?
Fe1 P1 C7 . . . 119.33(4) ?
N2 P1 C4 . . . 102.62(5) ?
N2 P1 C7 . . . 100.59(5) ?
C4 P1 C7 . . . 101.91(6) ?
Fe1 N1 C1 . . . 121.21(7) ?
Fe1 N1 C1 . . 12_566 121.21(7) ?
C1 N1 C1 . . 12_566 117.59(11) ?
P1 N2 C1 . . 3_556 112.25(7) ?
P1 N2 F1 . . . 113.34(5) ?
P1 N2 H1n2 . . . 119.0(10) ?
C1 N2 F1 3_556 . . 126.60(7) ?
C1 N2 H1n2 3_556 . . 118.5(9) ?
N1 C1 N2 . . 3_556 113.59(10) ?
N1 C1 C2 . . . 122.68(11) ?
N2 C1 C2 3_556 . . 123.71(10) ?
C1 C2 C3 . . . 118.46(11) ?
C1 C2 H1c2 . . . 120.77 ?
C3 C2 H1c2 . . . 120.77 ?
C2 C3 C2 . . 12_566 120.11(14) ?
C2 C3 H1c3 . . . 119.95 ?
C2 C3 H1c3 12_566 . . 119.95 ?
P1 C4 C5 . . . 112.23(9) ?
P1 C4 H1c4 . . . 109.47 ?
P1 C4 H2c4 . . . 109.47 ?
C5 C4 H1c4 . . . 109.47 ?
C5 C4 H2c4 . . . 109.47 ?
H1c4 C4 H2c4 . . . 106.56 ?
C4 C5 C6 . . . 112.09(12) ?
C4 C5 H1c5 . . . 109.47 ?
C4 C5 H2c5 . . . 109.47 ?
C6 C5 H1c5 . . . 109.47 ?
C6 C5 H2c5 . . . 109.47 ?
H1c5 C5 H2c5 . . . 106.72 ?
C5 C6 H1c6 . . . 109.47 ?
C5 C6 H2c6 . . . 109.47 ?
C5 C6 H3c6 . . . 109.47 ?
H1c6 C6 H2c6 . . . 109.47 ?
H1c6 C6 H3c6 . . . 109.47 ?
H2c6 C6 H3c6 . . . 109.47 ?
P1 C7 C8 . . . 116.52(10) ?
P1 C7 H1c7 . . . 109.47 ?
P1 C7 H2c7 . . . 109.47 ?
C8 C7 H1c7 . . . 109.47 ?
C8 C7 H2c7 . . . 109.47 ?
H1c7 C7 H2c7 . . . 101.37 ?
C7 C8 C9 . . . 110.62(13) ?
C7 C8 H1c8 . . . 109.47 ?
C7 C8 H2c8 . . . 109.47 ?
C9 C8 H1c8 . . . 109.47 ?
C9 C8 H2c8 . . . 109.47 ?
H1c8 C8 H2c8 . . . 108.3 ?
C8 C9 H1c9 . . . 109.47 ?
C8 C9 H2c9 . . . 109.47 ?
C8 C9 H3c9 . . . 109.47 ?
H1c9 C9 H2c9 . . . 109.47 ?
H1c9 C9 H3c9 . . . 109.47 ?
H2c9 C9 H3c9 . . . 109.47 ?
N2 F1 B1 . . . 114.86(9) ?
F1 B1 F1 . . 2_455 108.9(2) ?
F1 B1 F2 . . . 108.49(6) ?
F1 B1 F2 . . 2_455 110.87(7) ?
F1 B1 F2 2_455 . . 110.87(7) ?
F1 B1 F2 2_455 . 2_455 108.49(6) ?
F2 B1 F2 . . 2_455 109.3(2) ?
O1 C10 C11 . . . 122.07(15) ?
O1 C10 C11 . . 3_456 122.07(15) ?
C11 C10 C11 . . 3_456 115.9(2) ?
C10 C11 H1c11 . . . 109.47 ?
C10 C11 H2c11 . . . 109.47 ?
C10 C11 H3c11 . . . 109.47 ?
H1c11 C11 H2c11 . . . 109.47 ?
H1c11 C11 H3c11 . . . 109.47 ?
H2c11 C11 H3c11 . . . 109.47 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
? ? ? ? ? ? ? ? ? ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N2 H1n2 F1 . . . 0.870(11) 2.030(10) 2.8863(14) 168.1(13) ?

# start Validation Reply Form
_vrf_PLAT021_Fe-bisPNPiPr        
;
PROBLEM: Ratio Unique / Expected Reflections too High ...      1.841       
RESPONSE: The online version of CheckCIF seems to misinterpret
reflection data for origin choice 1 of space group Ccce.
Moving the origin to -1 (origin choice 2) makes these warnings
disappear.
;
_vrf_PLAT911_Fe-bisPNPiPr        
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600       1075 Report
RESPONSE: The online version of CheckCIF seems to misinterpret
reflection data for origin choice 1 of space group Ccce.
Moving the origin to -1 (origin choice 2) makes these warnings
disappear.
;

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetone'
_database_code_depnum_ccdc_archive 'CCDC 1024076'
