# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1485924'
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H52 Cl3 Fe N2 P '
_chemical_formula_sum            'C45 H52 Cl3 Fe N2 P '
_chemical_formula_weight         814.06

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'
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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pna21

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'

_cell_length_a                   17.2349(13)
_cell_length_b                   14.0856(9)
_cell_length_c                   17.5383(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4257.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9702
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      38.24

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2398
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(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  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29854
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         27.50
_reflns_number_total             9027
_reflns_number_gt                8855
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0885P)²+2.4344P] 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     SHELXL
_refine_ls_extinction_coef       0.090(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         9027
_refine_ls_number_parameters     478
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1528
_refine_ls_wR_factor_gt          0.1474
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_restrained_S_all      1.163
_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 0.28055(2) 0.55342(3) 0.11162(3) 0.02555(15) Uani 1 1 d . . .
P1 P 0.19398(4) 0.58943(5) 0.21935(4) 0.02056(18) Uani 1 1 d . . .
Cl1 Cl 0.39689(5) 0.52426(6) 0.17167(7) 0.0431(2) Uani 1 1 d . . .
Cl2 Cl 0.23426(7) 0.42005(7) 0.05507(6) 0.0505(3) Uani 1 1 d . . .
Cl3 Cl 0.26556(7) 0.68863(7) 0.04276(5) 0.0465(3) Uani 1 1 d . . .
C7 C 0.22933(16) 0.6874(2) 0.27722(19) 0.0252(6) Uani 1 1 d . . .
C1 C 0.17455(17) 0.4970(2) 0.28928(16) 0.0234(5) Uani 1 1 d . . .
C13 C 0.09855(17) 0.6259(2) 0.18664(18) 0.0272(6) Uani 1 1 d . . .
N2 N 0.04478(15) 0.20519(19) 0.23554(18) 0.0308(6) Uani 1 1 d . . .
N1 N 0.08602(17) 0.1797(2) 0.1227(2) 0.0397(7) Uani 1 1 d . . .
C6 C 0.23366(19) 0.4340(2) 0.3086(2) 0.0297(6) Uani 1 1 d . . .
H6 H 0.2809 0.4368 0.2832 0.036 Uiso 1 1 calc R . .
C34 C 0.00318(19) 0.2027(2) 0.3068(2) 0.0329(7) Uani 1 1 d . . .
C22 C 0.0943(2) 0.1434(3) 0.0457(3) 0.0434(9) Uani 1 1 d . . .
C12 C 0.2743(2) 0.7565(3) 0.2415(2) 0.0415(9) Uani 1 1 d . . .
H12 H 0.2853 0.7515 0.1898 0.050 Uiso 1 1 calc R . .
C11 C 0.3028(3) 0.8332(3) 0.2834(3) 0.0526(11) Uani 1 1 d . . .
H11 H 0.3329 0.8790 0.2593 0.063 Uiso 1 1 calc R . .
C2 C 0.10344(18) 0.4910(2) 0.32845(19) 0.0306(6) Uani 1 1 d . . .
H2 H 0.0635 0.5329 0.3167 0.037 Uiso 1 1 calc R . .
C4 C 0.1522(2) 0.3618(3) 0.4044(2) 0.0389(8) Uani 1 1 d . . .
H4 H 0.1452 0.3176 0.4432 0.047 Uiso 1 1 calc R . .
C8 C 0.2155(2) 0.6950(3) 0.3547(2) 0.0391(8) Uani 1 1 d . . .
H8 H 0.1873 0.6483 0.3799 0.047 Uiso 1 1 calc R . .
C19 C 0.03428(18) 0.1525(2) 0.1741(3) 0.0371(8) Uani 1 1 d . . .
H19 H -0.0027 0.1050 0.1680 0.045 Uiso 1 1 calc R . .
C18 C 0.0619(2) 0.5675(3) 0.1329(2) 0.0394(8) Uani 1 1 d . . .
H18 H 0.0864 0.5125 0.1160 0.047 Uiso 1 1 calc R . .
C14 C 0.0626(2) 0.7094(3) 0.2089(2) 0.0382(8) Uani 1 1 d . . .
H14 H 0.0867 0.7490 0.2442 0.046 Uiso 1 1 calc R . .
C21 C 0.1042(2) 0.2693(2) 0.2221(2) 0.0386(8) Uani 1 1 d . . .
H21 H 0.1224 0.3151 0.2558 0.046 Uiso 1 1 calc R . .
C3 C 0.0926(2) 0.4231(3) 0.3843(2) 0.0372(7) Uani 1 1 d . . .
H3 H 0.0448 0.4185 0.4087 0.045 Uiso 1 1 calc R . .
C20 C 0.1302(2) 0.2530(3) 0.1523(2) 0.0395(8) Uani 1 1 d . . .
H20 H 0.1704 0.2847 0.1279 0.047 Uiso 1 1 calc R . .
C17 C -0.0109(2) 0.5914(4) 0.1047(3) 0.0524(10) Uani 1 1 d . . .
H17 H -0.0366 0.5507 0.0715 0.063 Uiso 1 1 calc R . .
C10 C 0.2868(2) 0.8419(3) 0.3598(3) 0.0420(9) Uani 1 1 d . . .
H10 H 0.3047 0.8939 0.3873 0.050 Uiso 1 1 calc R . .
C27 C 0.1420(2) 0.0656(3) 0.0334(3) 0.0433(9) Uani 1 1 d . . .
C26 C 0.1499(3) 0.0353(3) -0.0422(3) 0.0525(11) Uani 1 1 d . . .
H26 H 0.1807 -0.0173 -0.0527 0.063 Uiso 1 1 calc R . .
C35 C -0.0570(2) 0.2667(3) 0.3169(3) 0.0425(9) Uani 1 1 d . . .
C23 C 0.0570(3) 0.1912(3) -0.0104(3) 0.0512(11) Uani 1 1 d . . .
C9 C 0.2440(3) 0.7729(3) 0.3949(2) 0.0459(9) Uani 1 1 d . . .
H9 H 0.2336 0.7780 0.4467 0.055 Uiso 1 1 calc R . .
C15 C -0.0091(2) 0.7343(3) 0.1789(3) 0.0489(10) Uani 1 1 d . . .
H15 H -0.0329 0.7904 0.1944 0.059 Uiso 1 1 calc R . .
C39 C 0.0301(3) 0.1437(3) 0.3654(3) 0.0611(14) Uani 1 1 d . . .
C31 C 0.1833(2) 0.0163(3) 0.0982(3) 0.0476(10) Uani 1 1 d . . .
H31 H 0.1847 0.0608 0.1412 0.057 Uiso 1 1 calc R . .
C25 C 0.1143(3) 0.0798(4) -0.0998(3) 0.0527(11) Uani 1 1 d . . .
H25 H 0.1211 0.0580 -0.1494 0.063 Uiso 1 1 calc R . .
C40 C 0.0919(4) 0.0705(4) 0.3527(6) 0.097(3) Uani 1 1 d . . .
H40 H 0.0787 0.0312 0.3085 0.116 Uiso 1 1 calc R . .
C28 C 0.0050(3) 0.2757(4) 0.0062(3) 0.0624(14) Uani 1 1 d . . .
H28 H 0.0172 0.2943 0.0587 0.075 Uiso 1 1 calc R . .
C41 C 0.1714(4) 0.0991(6) 0.3486(5) 0.0814(19) Uani 1 1 d . . .
H41A H 0.1812 0.1278 0.2998 0.122 Uiso 1 1 calc R . .
H41B H 0.2042 0.0446 0.3548 0.122 Uiso 1 1 calc R . .
H41C H 0.1821 0.1442 0.3883 0.122 Uiso 1 1 calc R . .
C43 C -0.0877(2) 0.3263(3) 0.2508(3) 0.0506(11) Uani 1 1 d . . .
H43 H -0.0462 0.3298 0.2127 0.061 Uiso 1 1 calc R . .
C5 C 0.2224(2) 0.3669(2) 0.3659(2) 0.0367(8) Uani 1 1 d . . .
H5 H 0.2623 0.3252 0.3784 0.044 Uiso 1 1 calc R . .
C16 C -0.0452(2) 0.6768(4) 0.1266(3) 0.0494(10) Uani 1 1 d . . .
H16 H -0.0926 0.6949 0.1058 0.059 Uiso 1 1 calc R . .
C38 C -0.0081(6) 0.1588(7) 0.4373(4) 0.100(3) Uani 1 1 d . . .
H38 H 0.0068 0.1224 0.4790 0.120 Uiso 1 1 calc R . .
C24 C 0.0674(3) 0.1580(4) -0.0863(3) 0.0591(12) Uani 1 1 d . . .
H24 H 0.0429 0.1886 -0.1267 0.071 Uiso 1 1 calc R . .
C44 C -0.1561(3) 0.2752(4) 0.2130(4) 0.0609(12) Uani 1 1 d . . .
H44A H -0.1970 0.2668 0.2496 0.091 Uiso 1 1 calc R . .
H44B H -0.1394 0.2143 0.1948 0.091 Uiso 1 1 calc R . .
H44C H -0.1748 0.3124 0.1710 0.091 Uiso 1 1 calc R . .
C36 C -0.0889(3) 0.2751(5) 0.3904(4) 0.0753(18) Uani 1 1 d . . .
H36 H -0.1284 0.3190 0.3983 0.090 Uiso 1 1 calc R . .
C32 C 0.1386(4) -0.0710(4) 0.1244(6) 0.087(2) Uani 1 1 d . . .
H32A H 0.0857 -0.0538 0.1346 0.130 Uiso 1 1 calc R . .
H32B H 0.1619 -0.0958 0.1699 0.130 Uiso 1 1 calc R . .
H32C H 0.1401 -0.1184 0.0851 0.130 Uiso 1 1 calc R . .
C33 C 0.2667(3) -0.0108(6) 0.0803(4) 0.0725(17) Uani 1 1 d . . .
H33A H 0.2675 -0.0697 0.0528 0.109 Uiso 1 1 calc R . .
H33B H 0.2953 -0.0177 0.1270 0.109 Uiso 1 1 calc R . .
H33C H 0.2901 0.0380 0.0497 0.109 Uiso 1 1 calc R . .
C45 C -0.1093(5) 0.4274(5) 0.2710(8) 0.105(3) Uani 1 1 d . . .
H45A H -0.1267 0.4599 0.2260 0.158 Uiso 1 1 calc R . .
H45B H -0.0648 0.4594 0.2916 0.158 Uiso 1 1 calc R . .
H45C H -0.1502 0.4269 0.3082 0.158 Uiso 1 1 calc R . .
C30 C -0.0781(4) 0.2427(7) 0.0082(6) 0.101(3) Uani 1 1 d . . .
H30A H -0.0990 0.2433 -0.0425 0.152 Uiso 1 1 calc R . .
H30B H -0.1079 0.2844 0.0401 0.152 Uiso 1 1 calc R . .
H30C H -0.0803 0.1794 0.0283 0.152 Uiso 1 1 calc R . .
C29 C 0.0229(5) 0.3647(5) -0.0431(5) 0.091(2) Uani 1 1 d . . .
H29A H 0.0764 0.3820 -0.0369 0.137 Uiso 1 1 calc R . .
H29B H -0.0096 0.4164 -0.0270 0.137 Uiso 1 1 calc R . .
H29C H 0.0128 0.3507 -0.0957 0.137 Uiso 1 1 calc R . .
C37 C -0.0657(6) 0.2248(10) 0.4467(4) 0.116(4) Uani 1 1 d . . .
H37 H -0.0881 0.2332 0.4945 0.139 Uiso 1 1 calc R . .
C42 C 0.0876(7) 0.0068(10) 0.4309(8) 0.129(4) Uani 1 1 d . . .
H42A H 0.0352 0.0055 0.4492 0.193 Uiso 1 1 calc R . .
H42B H 0.1207 0.0344 0.4690 0.193 Uiso 1 1 calc R . .
H42C H 0.1045 -0.0568 0.4202 0.193 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 Cl2 2.2692(9) . ?
Fe1 Cl3 2.2698(10) . ?
Fe1 Cl1 2.3020(10) . ?
Fe1 P1 2.4604(8) . ?
P1 C13 1.816(3) . ?
P1 C7 1.818(3) . ?
P1 C1 1.820(3) . ?
C7 C8 1.384(5) . ?
C7 C12 1.392(5) . ?
C1 C6 1.393(4) . ?
C1 C2 1.407(4) . ?
C13 C14 1.385(4) . ?
C13 C18 1.402(5) . ?
N2 C19 1.321(5) . ?
N2 C21 1.385(4) . ?
N2 C34 1.441(5) . ?
N1 C19 1.324(5) . ?
N1 C20 1.384(4) . ?
N1 C22 1.451(5) . ?
C6 C5 1.393(5) . ?
C34 C35 1.386(6) . ?
C34 C39 1.401(6) . ?
C22 C23 1.354(7) . ?
C22 C27 1.388(5) . ?
C12 C11 1.396(5) . ?
C11 C10 1.374(7) . ?
C2 C3 1.381(5) . ?
C4 C5 1.387(6) . ?
C4 C3 1.388(6) . ?
C8 C9 1.392(5) . ?
C18 C17 1.391(5) . ?
C14 C15 1.388(5) . ?
C21 C20 1.324(6) . ?
C17 C16 1.394(7) . ?
C10 C9 1.366(7) . ?
C27 C26 1.400(6) . ?
C27 C31 1.510(7) . ?
C26 C25 1.337(8) . ?
C35 C36 1.405(7) . ?
C35 C43 1.527(7) . ?
C23 C24 1.422(7) . ?
C23 C28 1.518(6) . ?
C15 C16 1.373(7) . ?
C39 C38 1.439(12) . ?
C39 C40 1.499(9) . ?
C31 C33 1.521(7) . ?
C31 C32 1.521(7) . ?
C25 C24 1.386(7) . ?
C40 C41 1.429(10) . ?
C40 C42 1.641(15) . ?
C28 C30 1.506(10) . ?
C28 C29 1.553(10) . ?
C43 C45 1.514(8) . ?
C43 C44 1.531(7) . ?
C38 C37 1.369(16) . ?
C36 C37 1.280(14) . ?

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
Cl2 Fe1 Cl3 114.97(5) . . ?
Cl2 Fe1 Cl1 111.01(5) . . ?
Cl3 Fe1 Cl1 119.50(4) . . ?
Cl2 Fe1 P1 107.04(3) . . ?
Cl3 Fe1 P1 99.59(4) . . ?
Cl1 Fe1 P1 102.33(4) . . ?
C13 P1 C7 105.36(14) . . ?
C13 P1 C1 104.40(14) . . ?
C7 P1 C1 103.21(14) . . ?
C13 P1 Fe1 111.40(11) . . ?
C7 P1 Fe1 112.45(10) . . ?
C1 P1 Fe1 118.80(9) . . ?
C8 C7 C12 118.9(3) . . ?
C8 C7 P1 123.3(3) . . ?
C12 C7 P1 117.8(3) . . ?
C6 C1 C2 118.6(3) . . ?
C6 C1 P1 119.0(2) . . ?
C2 C1 P1 122.2(2) . . ?
C14 C13 C18 119.2(3) . . ?
C14 C13 P1 123.8(3) . . ?
C18 C13 P1 117.0(2) . . ?
C19 N2 C21 109.2(3) . . ?
C19 N2 C34 128.7(3) . . ?
C21 N2 C34 122.1(3) . . ?
C19 N1 C20 109.3(3) . . ?
C19 N1 C22 126.7(3) . . ?
C20 N1 C22 123.9(3) . . ?
C5 C6 C1 120.4(3) . . ?
C35 C34 C39 122.7(4) . . ?
C35 C34 N2 117.9(3) . . ?
C39 C34 N2 119.1(4) . . ?
C23 C22 C27 124.1(4) . . ?
C23 C22 N1 117.1(3) . . ?
C27 C22 N1 118.7(4) . . ?
C7 C12 C11 120.0(4) . . ?
C10 C11 C12 120.7(4) . . ?
C3 C2 C1 120.4(3) . . ?
C5 C4 C3 119.3(3) . . ?
C7 C8 C9 119.8(4) . . ?
N2 C19 N1 107.5(3) . . ?
C17 C18 C13 120.2(4) . . ?
C13 C14 C15 120.4(4) . . ?
C20 C21 N2 107.1(3) . . ?
C2 C3 C4 120.7(3) . . ?
C21 C20 N1 106.9(3) . . ?
C18 C17 C16 119.6(4) . . ?
C9 C10 C11 118.9(4) . . ?
C22 C27 C26 116.4(5) . . ?
C22 C27 C31 121.7(4) . . ?
C26 C27 C31 121.9(4) . . ?
C25 C26 C27 121.9(4) . . ?
C34 C35 C36 117.7(5) . . ?
C34 C35 C43 121.3(4) . . ?
C36 C35 C43 120.9(5) . . ?
C22 C23 C24 117.2(4) . . ?
C22 C23 C28 122.0(4) . . ?
C24 C23 C28 120.8(5) . . ?
C10 C9 C8 121.6(4) . . ?
C16 C15 C14 120.5(4) . . ?
C34 C39 C38 113.8(6) . . ?
C34 C39 C40 122.3(6) . . ?
C38 C39 C40 123.9(6) . . ?
C27 C31 C33 113.9(4) . . ?
C27 C31 C32 111.1(4) . . ?
C33 C31 C32 109.8(5) . . ?
C26 C25 C24 120.8(5) . . ?
C41 C40 C39 119.7(5) . . ?
C41 C40 C42 103.9(7) . . ?
C39 C40 C42 102.7(8) . . ?
C30 C28 C23 108.9(6) . . ?
C30 C28 C29 116.8(6) . . ?
C23 C28 C29 114.2(5) . . ?
C45 C43 C35 115.1(6) . . ?
C45 C43 C44 110.8(4) . . ?
C35 C43 C44 109.7(4) . . ?
C4 C5 C6 120.5(3) . . ?
C15 C16 C17 120.1(3) . . ?
C37 C38 C39 122.6(5) . . ?
C25 C24 C23 119.6(5) . . ?
C37 C36 C35 122.6(8) . . ?
C36 C37 C38 120.6(7) . . ?

_diffrn_measured_fraction_theta_max 0.948
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.948
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.122
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1485926'
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H52 Br3 Fe N2 P'
_chemical_formula_sum            'C45 H52 Br3 Fe N2 P'
_chemical_formula_weight         947.44

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pna21

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

_cell_length_a                   17.4631(9)
_cell_length_b                   14.2501(5)
_cell_length_c                   17.9938(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4477.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4868
_cell_measurement_theta_min      0.45195
_cell_measurement_theta_max      1.00000

_exptl_crystal_description       block
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    3.081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.45195
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17111
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6816
_reflns_number_gt                4984
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0601P)²+4.4415P] 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'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_number_reflns         6816
_refine_ls_number_parameters     469
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0540
_refine_ls_wR_factor_ref         0.1347
_refine_ls_wR_factor_gt          0.1179
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.22182(6) 0.44278(7) 0.48835(7) 0.0417(3) Uani 1 1 d . . .
Br1 Br 0.09861(5) 0.47140(6) 0.54723(9) 0.0865(4) Uani 1 1 d . . .
Br2 Br 0.26695(8) 0.57889(7) 0.42580(7) 0.0991(5) Uani 1 1 d . . .
Br3 Br 0.24166(6) 0.30134(6) 0.41769(6) 0.0701(3) Uani 1 1 d . . .
P1 P 0.30490(9) 0.40909(12) 0.59574(11) 0.0298(4) Uani 1 1 d . . .
N1 N 0.4114(3) 0.8146(4) 0.5011(3) 0.0336(14) Uani 1 1 d . . .
N2 N 0.4513(3) 0.7916(4) 0.6131(4) 0.0337(14) Uani 1 1 d . . .
C1 C 0.2705(4) 0.3117(5) 0.6525(4) 0.0368(18) Uani 1 1 d . . .
C2 C 0.2237(5) 0.2465(6) 0.6184(5) 0.061(3) Uani 1 1 d . . .
H2A H 0.2109 0.2530 0.5674 0.073 Uiso 1 1 calc R . .
C3 C 0.1952(6) 0.1710(6) 0.6595(6) 0.073(3) Uani 1 1 d . . .
H3A H 0.1629 0.1260 0.6363 0.088 Uiso 1 1 calc R . .
C4 C 0.2133(5) 0.1618(6) 0.7321(6) 0.052(2) Uani 1 1 d . . .
H4A H 0.1951 0.1094 0.7596 0.063 Uiso 1 1 calc R . .
C5 C 0.2579(5) 0.2278(6) 0.7657(6) 0.066(3) Uani 1 1 d . . .
H5A H 0.2696 0.2221 0.8171 0.079 Uiso 1 1 calc R . .
C6 C 0.2861(5) 0.3025(6) 0.7260(5) 0.063(3) Uani 1 1 d . . .
H6A H 0.3168 0.3483 0.7502 0.075 Uiso 1 1 calc R . .
C7 C 0.3231(4) 0.5003(5) 0.6654(4) 0.0337(17) Uani 1 1 d . . .
C8 C 0.3919(4) 0.5076(5) 0.7036(4) 0.0395(18) Uani 1 1 d . . .
H8A H 0.4329 0.4666 0.6912 0.047 Uiso 1 1 calc R . .
C9 C 0.4021(5) 0.5729(6) 0.7588(5) 0.053(2) Uani 1 1 d . . .
H9A H 0.4499 0.5775 0.7836 0.063 Uiso 1 1 calc R . .
C10 C 0.3434(6) 0.6309(5) 0.7779(5) 0.054(2) Uani 1 1 d . . .
H10A H 0.3502 0.6753 0.8166 0.064 Uiso 1 1 calc R . .
C11 C 0.2739(5) 0.6258(5) 0.7414(5) 0.053(2) Uani 1 1 d . . .
H11A H 0.2331 0.6663 0.7552 0.064 Uiso 1 1 calc R . .
C12 C 0.2641(4) 0.5615(5) 0.6845(5) 0.042(2) Uani 1 1 d . . .
H12A H 0.2169 0.5591 0.6583 0.050 Uiso 1 1 calc R . .
C13 C 0.4004(4) 0.3763(5) 0.5649(4) 0.0355(17) Uani 1 1 d . . .
C14 C 0.4371(5) 0.4344(7) 0.5159(5) 0.069(3) Uani 1 1 d . . .
H14A H 0.4130 0.4912 0.5014 0.083 Uiso 1 1 calc R . .
C15 C 0.5083(6) 0.4128(10) 0.4871(7) 0.096(4) Uani 1 1 d . . .
H15A H 0.5340 0.4554 0.4550 0.115 Uiso 1 1 calc R . .
C16 C 0.5411(6) 0.3289(10) 0.5057(7) 0.089(4) Uani 1 1 d . . .
H16A H 0.5886 0.3110 0.4842 0.107 Uiso 1 1 calc R . .
C17 C 0.5063(6) 0.2718(7) 0.5543(9) 0.094(4) Uani 1 1 d . . .
H17A H 0.5306 0.2150 0.5686 0.112 Uiso 1 1 calc R . .
C18 C 0.4351(5) 0.2941(6) 0.5841(6) 0.069(3) Uani 1 1 d . . .
H18A H 0.4108 0.2523 0.6178 0.083 Uiso 1 1 calc R . .
C19 C 0.4617(4) 0.8408(4) 0.5509(5) 0.0368(17) Uani 1 1 d . . .
H19A H 0.4997 0.8877 0.5438 0.044 Uiso 1 1 calc R . .
C20 C 0.3663(4) 0.7454(5) 0.5317(5) 0.0392(18) Uani 1 1 d . . .
H20A H 0.3251 0.7136 0.5080 0.047 Uiso 1 1 calc R . .
C21 C 0.3913(4) 0.7313(5) 0.6008(5) 0.0396(19) Uani 1 1 d . . .
H21A H 0.3711 0.6874 0.6354 0.047 Uiso 1 1 calc R . .
C22 C 0.4030(4) 0.8498(5) 0.4253(5) 0.0382(18) Uani 1 1 d . . .
C23 C 0.4403(5) 0.8030(6) 0.3701(5) 0.047(2) Uani 1 1 d . . .
C24 C 0.4300(5) 0.8363(7) 0.2975(6) 0.065(3) Uani 1 1 d . . .
H24A H 0.4549 0.8059 0.2573 0.078 Uiso 1 1 calc R . .
C25 C 0.3841(6) 0.9126(7) 0.2843(6) 0.069(3) Uani 1 1 d . . .
H25A H 0.3779 0.9349 0.2350 0.082 Uiso 1 1 calc R . .
C26 C 0.3474(5) 0.9568(7) 0.3412(6) 0.063(3) Uani 1 1 d . . .
H26A H 0.3156 1.0091 0.3305 0.075 Uiso 1 1 calc R . .
C27 C 0.3551(4) 0.9273(5) 0.4148(5) 0.0438(19) Uani 1 1 d . . .
C28 C 0.3143(5) 0.9766(5) 0.4779(6) 0.054(2) Uani 1 1 d . . .
H28A H 0.3154 0.9340 0.5221 0.065 Uiso 1 1 calc R . .
C29 C 0.3561(6) 1.0666(7) 0.4988(8) 0.096(4) Uani 1 1 d . . .
H29A H 0.4095 1.0521 0.5109 0.144 Uiso 1 1 calc R . .
H29B H 0.3312 1.0952 0.5420 0.144 Uiso 1 1 calc R . .
H29C H 0.3544 1.1104 0.4568 0.144 Uiso 1 1 calc R . .
C30 C 0.2317(5) 0.9970(8) 0.4600(6) 0.080(3) Uani 1 1 d . . .
H30A H 0.2056 0.9385 0.4466 0.119 Uiso 1 1 calc R . .
H30B H 0.2290 1.0410 0.4183 0.119 Uiso 1 1 calc R . .
H30C H 0.2067 1.0248 0.5036 0.119 Uiso 1 1 calc R . .
C31 C 0.4941(5) 0.7204(7) 0.3849(6) 0.063(3) Uani 1 1 d . . .
H31A H 0.4823 0.6968 0.4360 0.076 Uiso 1 1 calc R . .
C32 C 0.5766(6) 0.7566(10) 0.3862(8) 0.114(5) Uani 1 1 d . . .
H32A H 0.6116 0.7043 0.3962 0.171 Uiso 1 1 calc R . .
H32B H 0.5819 0.8040 0.4254 0.171 Uiso 1 1 calc R . .
H32C H 0.5891 0.7847 0.3380 0.171 Uiso 1 1 calc R . .
C33 C 0.4824(7) 0.6395(9) 0.3323(7) 0.111(5) Uani 1 1 d . . .
H33A H 0.4292 0.6181 0.3351 0.167 Uiso 1 1 calc R . .
H33B H 0.5167 0.5879 0.3460 0.167 Uiso 1 1 calc R . .
H33C H 0.4939 0.6598 0.2814 0.167 Uiso 1 1 calc R . .
C34 C 0.4917(4) 0.7988(5) 0.6834(5) 0.0385(18) Uani 1 1 d . . .
C35 C 0.4634(5) 0.8619(6) 0.7345(6) 0.056(2) Uani 1 1 d . B .
C36 C 0.4960(7) 0.8588(9) 0.8044(7) 0.084(3) Uani 1 1 d . . .
H36A H 0.4784 0.8996 0.8426 0.101 Uiso 1 1 calc R . .
C37 C 0.5545(8) 0.7955(12) 0.8184(7) 0.103(5) Uani 1 1 d . . .
H37A H 0.5759 0.7932 0.8669 0.124 Uiso 1 1 calc R . .
C38 C 0.5826(6) 0.7367(8) 0.7658(7) 0.071(3) Uani 1 1 d . . .
H38A H 0.6240 0.6960 0.7772 0.085 Uiso 1 1 calc R . .
C39 C 0.5511(4) 0.7362(5) 0.6958(5) 0.048(2) Uani 1 1 d . . .
C40 C 0.3999(5) 0.9326(6) 0.7141(8) 0.082(4) Uani 1 1 d D . .
H40 H 0.4050 0.9325 0.6587 0.099 Uiso 1 1 calc R A 1
C41 C 0.4161(19) 1.0330(14) 0.730(2) 0.106(8) Uani 0.50 1 d PD B 1
H41A H 0.4708 1.0454 0.7224 0.159 Uiso 0.50 1 calc PR B 1
H41B H 0.4021 1.0473 0.7813 0.159 Uiso 0.50 1 calc PR B 1
H41C H 0.3861 1.0724 0.6960 0.159 Uiso 0.50 1 calc PR B 1
C42 C 0.3200(11) 0.8948(19) 0.722(2) 0.106(8) Uani 0.50 1 d PD B 1
H42A H 0.3202 0.8271 0.7122 0.159 Uiso 0.50 1 calc PR B 1
H42B H 0.2863 0.9261 0.6860 0.159 Uiso 0.50 1 calc PR B 1
H42C H 0.3014 0.9066 0.7724 0.159 Uiso 0.50 1 calc PR B 1
C41A C 0.4281(18) 1.0267(14) 0.690(2) 0.106(8) Uani 0.50 1 d PD B 2
H41D H 0.4751 1.0193 0.6611 0.159 Uiso 0.50 1 calc PR B 2
H41E H 0.4388 1.0651 0.7343 0.159 Uiso 0.50 1 calc PR B 2
H41F H 0.3889 1.0575 0.6599 0.159 Uiso 0.50 1 calc PR B 2
C42A C 0.3292(13) 0.9238(19) 0.7596(18) 0.106(8) Uani 0.50 1 d PD B 2
H42D H 0.3185 0.8573 0.7689 0.159 Uiso 0.50 1 calc PR B 2
H42E H 0.2861 0.9520 0.7328 0.159 Uiso 0.50 1 calc PR B 2
H42F H 0.3364 0.9564 0.8071 0.159 Uiso 0.50 1 calc PR B 2
C43 C 0.5822(5) 0.6737(6) 0.6374(6) 0.064(3) Uani 1 1 d . . .
H43A H 0.5404 0.6653 0.6001 0.077 Uiso 1 1 calc R . .
C44 C 0.6044(6) 0.5773(7) 0.6622(9) 0.118(5) Uani 1 1 d . . .
H44A H 0.5611 0.5480 0.6880 0.177 Uiso 1 1 calc R . .
H44B H 0.6482 0.5813 0.6960 0.177 Uiso 1 1 calc R . .
H44C H 0.6182 0.5394 0.6188 0.177 Uiso 1 1 calc R . .
C45 C 0.6485(6) 0.7206(8) 0.5961(7) 0.091(3) Uani 1 1 d . . .
H45A H 0.6683 0.6778 0.5581 0.136 Uiso 1 1 calc R . .
H45B H 0.6894 0.7358 0.6314 0.136 Uiso 1 1 calc R . .
H45C H 0.6303 0.7784 0.5724 0.136 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 Br2 2.3769(14) . ?
Fe1 Br3 2.4082(14) . ?
Fe1 Br1 2.4327(16) . ?
Fe1 P1 2.463(2) . ?
P1 C13 1.819(7) . ?
P1 C1 1.826(7) . ?
P1 C7 1.833(7) . ?
N1 C19 1.309(9) . ?
N1 C20 1.377(8) . ?
N1 C22 1.462(10) . ?
N2 C19 1.334(9) . ?
N2 C21 1.373(8) . ?
N2 C34 1.451(10) . ?
C1 C6 1.355(11) . ?
C1 C2 1.382(11) . ?
C2 C3 1.397(12) . ?
C3 C4 1.351(12) . ?
C4 C5 1.363(12) . ?
C5 C6 1.374(12) . ?
C7 C8 1.388(10) . ?
C7 C12 1.393(10) . ?
C8 C9 1.372(11) . ?
C9 C10 1.362(12) . ?
C10 C11 1.381(12) . ?
C11 C12 1.384(12) . ?
C13 C18 1.363(10) . ?
C13 C14 1.369(11) . ?
C14 C15 1.382(13) . ?
C15 C16 1.367(15) . ?
C16 C17 1.340(16) . ?
C17 C18 1.390(13) . ?
C20 C21 1.333(11) . ?
C22 C23 1.362(11) . ?
C22 C27 1.398(10) . ?
C23 C24 1.401(12) . ?
C23 C31 1.528(12) . ?
C24 C25 1.371(13) . ?
C25 C26 1.362(13) . ?
C26 C27 1.397(12) . ?
C27 C28 1.514(12) . ?
C28 C30 1.508(13) . ?
C28 C29 1.522(13) . ?
C31 C33 1.505(14) . ?
C31 C32 1.531(15) . ?
C34 C35 1.378(11) . ?
C34 C39 1.386(10) . ?
C35 C36 1.382(14) . ?
C35 C40 1.542(14) . ?
C36 C37 1.386(18) . ?
C37 C38 1.356(18) . ?
C38 C39 1.374(13) . ?
C39 C43 1.482(12) . ?
C40 C41 1.485(18) . ?
C40 C42A 1.487(17) . ?
C40 C41A 1.491(17) . ?
C40 C42 1.503(17) . ?
C43 C44 1.494(13) . ?
C43 C45 1.529(14) . ?

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
Br2 Fe1 Br3 112.66(7) . . ?
Br2 Fe1 Br1 111.27(6) . . ?
Br3 Fe1 Br1 119.83(5) . . ?
Br2 Fe1 P1 109.58(6) . . ?
Br3 Fe1 P1 99.57(6) . . ?
Br1 Fe1 P1 102.24(7) . . ?
C13 P1 C1 106.1(3) . . ?
C13 P1 C7 103.4(3) . . ?
C1 P1 C7 102.3(3) . . ?
C13 P1 Fe1 110.5(3) . . ?
C1 P1 Fe1 113.2(2) . . ?
C7 P1 Fe1 120.0(2) . . ?
C19 N1 C20 108.4(6) . . ?
C19 N1 C22 127.4(6) . . ?
C20 N1 C22 124.2(6) . . ?
C19 N2 C21 107.3(6) . . ?
C19 N2 C34 128.9(6) . . ?
C21 N2 C34 123.8(6) . . ?
C6 C1 C2 119.2(7) . . ?
C6 C1 P1 123.6(6) . . ?
C2 C1 P1 117.2(6) . . ?
C1 C2 C3 119.6(9) . . ?
C4 C3 C2 120.2(9) . . ?
C3 C4 C5 119.8(8) . . ?
C4 C5 C6 120.6(9) . . ?
C1 C6 C5 120.7(8) . . ?
C8 C7 C12 118.1(7) . . ?
C8 C7 P1 122.8(5) . . ?
C12 C7 P1 119.0(6) . . ?
C9 C8 C7 121.5(7) . . ?
C10 C9 C8 119.8(8) . . ?
C9 C10 C11 120.7(8) . . ?
C10 C11 C12 119.6(8) . . ?
C11 C12 C7 120.4(8) . . ?
C18 C13 C14 118.3(7) . . ?
C18 C13 P1 123.5(6) . . ?
C14 C13 P1 118.1(5) . . ?
C13 C14 C15 121.9(9) . . ?
C16 C15 C14 118.6(11) . . ?
C17 C16 C15 120.1(9) . . ?
C16 C17 C18 121.2(10) . . ?
C13 C18 C17 119.8(10) . . ?
N1 C19 N2 109.4(6) . . ?
C21 C20 N1 107.0(6) . . ?
C20 C21 N2 107.9(6) . . ?
C23 C22 C27 125.1(8) . . ?
C23 C22 N1 117.7(6) . . ?
C27 C22 N1 117.2(7) . . ?
C22 C23 C24 116.9(8) . . ?
C22 C23 C31 122.9(8) . . ?
C24 C23 C31 120.2(8) . . ?
C25 C24 C23 120.3(9) . . ?
C26 C25 C24 120.8(9) . . ?
C25 C26 C27 121.9(8) . . ?
C26 C27 C22 115.0(8) . . ?
C26 C27 C28 121.8(7) . . ?
C22 C27 C28 123.2(8) . . ?
C30 C28 C27 112.3(8) . . ?
C30 C28 C29 110.4(8) . . ?
C27 C28 C29 110.5(8) . . ?
C33 C31 C23 113.4(8) . . ?
C33 C31 C32 113.3(9) . . ?
C23 C31 C32 108.7(8) . . ?
C35 C34 C39 125.5(8) . . ?
C35 C34 N2 117.0(7) . . ?
C39 C34 N2 117.3(7) . . ?
C34 C35 C36 116.1(9) . . ?
C34 C35 C40 121.7(9) . . ?
C36 C35 C40 122.2(10) . . ?
C35 C36 C37 119.3(11) . . ?
C38 C37 C36 122.8(11) . . ?
C37 C38 C39 119.9(10) . . ?
C38 C39 C34 116.4(9) . . ?
C38 C39 C43 120.4(8) . . ?
C34 C39 C43 123.2(8) . . ?
C41 C40 C42A 97.7(17) . . ?
C41 C40 C41A 29(2) . . ?
C42A C40 C41A 120.5(16) . . ?
C41 C40 C42 120.3(16) . . ?
C42A C40 C42 31.5(16) . . ?
C41A C40 C42 131(2) . . ?
C41 C40 C35 116.6(17) . . ?
C42A C40 C35 114.3(15) . . ?
C41A C40 C35 114.7(15) . . ?
C42 C40 C35 114.3(14) . . ?
C39 C43 C44 115.9(10) . . ?
C39 C43 C45 111.1(7) . . ?
C44 C43 C45 110.6(8) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.073
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1485927'
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H70 Cl3 Fe N2 P, 3(C4H8O)'
_chemical_formula_sum            'C57 H94 Cl3 Fe N2 O3 P'
_chemical_formula_weight         1048.51

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'
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           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   17.6972(7)
_cell_length_b                   16.5426(7)
_cell_length_c                   22.9862(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6729.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9316
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      30.35

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2264
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9309
_exptl_absorpt_correction_T_max  0.9608
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32299
_diffrn_reflns_av_R_equivalents  0.0796
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6146
_reflns_number_gt                3984
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.2000P)²+0.0000P] 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         6146
_refine_ls_number_parameters     326
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.1008
_refine_ls_wR_factor_ref         0.3424
_refine_ls_wR_factor_gt          0.3036
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_restrained_S_all      1.209
_refine_ls_shift/su_max          0.018
_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 0.24087(5) 0.2500 0.48806(5) 0.0526(4) Uani 1 2 d S . .
P1 P 0.36546(10) 0.2500 0.53521(8) 0.0460(5) Uani 1 2 d S . .
Cl1 Cl 0.16307(10) 0.2500 0.56825(9) 0.0650(6) Uani 1 2 d S . .
Cl2 Cl 0.22576(9) 0.13606(10) 0.43367(7) 0.0785(6) Uani 1 1 d . . .
N1 N 0.9764(2) 0.1852(2) 0.41731(16) 0.0445(9) Uani 1 1 d . . .
C1 C 0.4445(5) 0.2500 0.4865(4) 0.096(4) Uani 1 2 d SDU . .
H1 H 0.4487 0.1910 0.4849 0.115 Uiso 0.50 1 calc PR A .
C2 C 0.4272(6) 0.260(2) 0.4234(4) 0.073(5) Uani 0.50 1 d PDU A -1
H2A H 0.4194 0.3166 0.4157 0.088 Uiso 0.50 1 calc PR A -1
H2B H 0.3798 0.2321 0.4155 0.088 Uiso 0.50 1 calc PR A -1
C3 C 0.4859(7) 0.2283(12) 0.3810(6) 0.105(7) Uani 0.50 1 d PDU A -1
H3A H 0.4733 0.2455 0.3419 0.126 Uiso 0.50 1 calc PR A -1
H3B H 0.4865 0.1697 0.3817 0.126 Uiso 0.50 1 calc PR A -1
C4 C 0.5641(7) 0.261(3) 0.3980(6) 0.110(7) Uani 0.50 1 d PDU A -1
H4A H 0.6020 0.2413 0.3711 0.132 Uiso 0.50 1 calc PR A -1
H4B H 0.5640 0.3197 0.3963 0.132 Uiso 0.50 1 calc PR A -1
C5 C 0.5825(6) 0.2332(17) 0.4592(6) 0.103(7) Uani 0.50 1 d PDU A -1
H5A H 0.5836 0.1746 0.4601 0.123 Uiso 0.50 1 calc PR A -1
H5B H 0.6322 0.2528 0.4700 0.123 Uiso 1 2 calc SR A -1
C6 C 0.5254(5) 0.263(2) 0.5025(5) 0.087(7) Uani 0.50 1 d PDU A -1
H6A H 0.5350 0.2369 0.5395 0.105 Uiso 0.50 1 calc PR A -1
H6B H 0.5334 0.3208 0.5081 0.105 Uiso 0.50 1 calc PR A -1
C7 C 0.3792(4) 0.1619(4) 0.5818(3) 0.086(2) Uani 1 1 d D . .
H7 H 0.4350(11) 0.159(5) 0.587(2) 0.104 Uiso 1 1 d D . .
C8 C 0.3470(10) 0.0869(8) 0.5603(7) 0.092(2) Uani 0.50 1 d PD A 1
H8A H 0.3794 0.0658 0.5298 0.111 Uiso 0.50 1 calc PR A 1
H8B H 0.2981 0.0983 0.5432 0.111 Uiso 0.50 1 calc PR A 1
C9 C 0.3373(8) 0.0217(9) 0.6071(7) 0.092(2) Uani 0.50 1 d PD A 1
H9A H 0.3243 -0.0296 0.5891 0.111 Uiso 0.50 1 calc PR A 1
H9B H 0.2970 0.0366 0.6336 0.111 Uiso 0.50 1 calc PR A 1
C10 C 0.4126(9) 0.0139(8) 0.6405(6) 0.092(2) Uani 0.50 1 d PD A 1
H10A H 0.4079 -0.0278 0.6700 0.111 Uiso 0.50 1 calc PR A 1
H10B H 0.4523 -0.0022 0.6138 0.111 Uiso 0.50 1 calc PR A 1
C11 C 0.4339(9) 0.0939(7) 0.6693(6) 0.092(2) Uani 0.50 1 d PD A 1
H11A H 0.3960 0.1079 0.6981 0.111 Uiso 0.50 1 calc PR A 1
H11B H 0.4819 0.0880 0.6891 0.111 Uiso 0.50 1 calc PR A 1
C12 C 0.4396(8) 0.1608(9) 0.6248(6) 0.092(2) Uani 0.50 1 d PD A 1
H12A H 0.4399 0.2122 0.6451 0.111 Uiso 0.50 1 calc PR A 1
H12B H 0.4875 0.1557 0.6047 0.111 Uiso 0.50 1 calc PR A 1
C8A C 0.3887(9) 0.0849(7) 0.5383(6) 0.0880(19) Uani 0.50 1 d PD A 2
H8A1 H 0.3425 0.0784 0.5160 0.106 Uiso 0.50 1 calc PR A 2
H8A2 H 0.4292 0.0961 0.5110 0.106 Uiso 0.50 1 calc PR A 2
C9A C 0.4061(8) 0.0044(8) 0.5702(6) 0.0880(19) Uani 0.50 1 d PD A 2
H9A1 H 0.3985 -0.0406 0.5437 0.106 Uiso 0.50 1 calc PR A 2
H9A2 H 0.4585 0.0040 0.5825 0.106 Uiso 0.50 1 calc PR A 2
C10A C 0.3554(9) -0.0058(8) 0.6226(6) 0.0880(19) Uani 0.50 1 d PD A 2
H10C H 0.3042 -0.0161 0.6095 0.106 Uiso 0.50 1 calc PR A 2
H10D H 0.3720 -0.0525 0.6447 0.106 Uiso 0.50 1 calc PR A 2
C11A C 0.3551(9) 0.0661(7) 0.6614(6) 0.0880(19) Uani 0.50 1 d PD A 2
H11C H 0.4051 0.0734 0.6779 0.106 Uiso 0.50 1 calc PR A 2
H11D H 0.3201 0.0570 0.6932 0.106 Uiso 0.50 1 calc PR A 2
C12A C 0.3320(8) 0.1437(8) 0.6284(6) 0.0880(19) Uani 0.50 1 d PD A 2
H12C H 0.2808 0.1374 0.6141 0.106 Uiso 0.50 1 calc PR A 2
H12D H 0.3323 0.1888 0.6553 0.106 Uiso 0.50 1 calc PR A 2
C19 C 0.9415(4) 0.2500 0.3964(3) 0.0469(16) Uani 1 2 d S . .
H19 H 0.9000 0.2500 0.3716 0.056 Uiso 1 2 calc SR . .
C20 C 1.0342(3) 0.2107(3) 0.4526(2) 0.0518(12) Uani 1 1 d . . .
H20 H 1.0675 0.1776 0.4729 0.062 Uiso 1 1 calc R . .
C21 C 0.9521(3) 0.1024(3) 0.4048(2) 0.0458(11) Uani 1 1 d . . .
C22 C 0.9006(3) 0.0674(3) 0.4435(2) 0.0519(13) Uani 1 1 d . . .
C23 C 0.8784(3) -0.0115(4) 0.4305(3) 0.0721(17) Uani 1 1 d . . .
H23 H 0.8464 -0.0388 0.4559 0.087 Uiso 1 1 calc R . .
C24 C 0.9030(4) -0.0494(3) 0.3810(3) 0.0779(18) Uani 1 1 d . . .
H24 H 0.8840 -0.1001 0.3713 0.093 Uiso 1 1 calc R . .
C25 C 0.9555(4) -0.0131(4) 0.3455(3) 0.0796(18) Uani 1 1 d . . .
H25 H 0.9740 -0.0413 0.3136 0.096 Uiso 1 1 calc R . .
C26 C 0.9817(3) 0.0646(3) 0.3562(2) 0.0629(15) Uani 1 1 d . . .
C27 C 0.8716(3) 0.1094(4) 0.4971(3) 0.0625(15) Uani 1 1 d . . .
H27 H 0.8981 0.1612 0.5001 0.075 Uiso 1 1 calc R . .
C28 C 0.8879(6) 0.0634(5) 0.5507(3) 0.112(3) Uani 1 1 d . . .
H28A H 0.8646 0.0897 0.5833 0.168 Uiso 1 1 calc R . .
H28B H 0.9416 0.0609 0.5567 0.168 Uiso 1 1 calc R . .
H28C H 0.8682 0.0095 0.5471 0.168 Uiso 1 1 calc R . .
C29 C 0.7888(5) 0.1277(7) 0.4893(4) 0.133(4) Uani 1 1 d . . .
H29A H 0.7610 0.0780 0.4863 0.200 Uiso 1 1 calc R . .
H29B H 0.7817 0.1589 0.4545 0.200 Uiso 1 1 calc R . .
H29C H 0.7708 0.1579 0.5222 0.200 Uiso 1 1 calc R . .
C30 C 1.0400(4) 0.1042(4) 0.3166(3) 0.081(2) Uani 1 1 d . . .
H30 H 1.0581 0.1533 0.3360 0.097 Uiso 1 1 calc R . .
C31 C 1.0028(6) 0.1294(7) 0.2599(4) 0.140(4) Uani 1 1 d . . .
H31A H 0.9863 0.0821 0.2392 0.210 Uiso 1 1 calc R . .
H31B H 1.0385 0.1585 0.2365 0.210 Uiso 1 1 calc R . .
H31C H 0.9602 0.1634 0.2680 0.210 Uiso 1 1 calc R . .
C32 C 1.1080(4) 0.0500(5) 0.3057(3) 0.089(2) Uani 1 1 d . . .
H32A H 1.1366 0.0447 0.3409 0.134 Uiso 1 1 calc R . .
H32B H 1.1392 0.0735 0.2760 0.134 Uiso 1 1 calc R . .
H32C H 1.0910 -0.0023 0.2933 0.134 Uiso 1 1 calc R . .
O1 O 0.7955(6) 0.2500 0.3222(5) 0.157(4) Uani 1 2 d S . .
C33 C 0.7748(6) 0.1805(8) 0.2909(5) 0.145(4) Uani 1 1 d . . .
H33A H 0.7251 0.1616 0.3024 0.174 Uiso 1 1 calc R . .
H33B H 0.8112 0.1374 0.2965 0.174 Uiso 1 1 calc R . .
C34 C 0.7748(12) 0.2086(9) 0.2317(8) 0.245(9) Uani 1 1 d . . .
H34A H 0.8193 0.1886 0.2116 0.294 Uiso 1 1 calc R . .
H34B H 0.7304 0.1886 0.2116 0.294 Uiso 1 1 calc R . .
O2 O -0.0033(7) 0.7683(15) 0.3123(7) 0.199(4) Uiso 0.50 1 d PD B -1
C37 C 0.0461(13) 0.8001(17) 0.2702(9) 0.199(4) Uiso 0.50 1 d PD B -1
H37A H 0.0362 0.8573 0.2646 0.239 Uiso 0.50 1 calc PR B -1
H37B H 0.0389 0.7727 0.2333 0.239 Uiso 0.50 1 calc PR B -1
C38 C 0.1266(10) 0.7877(17) 0.2916(10) 0.199(4) Uiso 0.50 1 d PD B -1
H38A H 0.1530 0.8390 0.2934 0.239 Uiso 0.50 1 calc PR B -1
H38B H 0.1539 0.7521 0.2654 0.239 Uiso 1 2 calc SR B -1
C39 C 0.1218(9) 0.750(4) 0.3528(10) 0.199(4) Uiso 1 2 d SD B -1
H39A H 0.1487 0.7819 0.3813 0.239 Uiso 0.50 1 calc PR B -1
H39B H 0.1418 0.6951 0.3530 0.239 Uiso 0.50 1 calc PR B -1
O3 O 0.6885(13) 0.0562(15) 0.7191(9) 0.222(6) Uiso 0.50 1 d PD C -1
C41 C 0.6813(19) 0.0115(14) 0.6683(13) 0.222(6) Uiso 0.50 1 d PD C -1
H41A H 0.6504 -0.0358 0.6759 0.266 Uiso 0.50 1 calc PR C -1
H41B H 0.7308 -0.0070 0.6560 0.266 Uiso 0.50 1 calc PR C -1
C42 C 0.6453(19) 0.0614(19) 0.6192(10) 0.222(6) Uiso 0.50 1 d PD C -1
H42A H 0.5939 0.0439 0.6114 0.266 Uiso 0.50 1 calc PR C -1
H42B H 0.6747 0.0581 0.5837 0.266 Uiso 0.50 1 calc PR C -1
C43 C 0.647(2) 0.1487(15) 0.6454(12) 0.222(6) Uiso 0.50 1 d PD C -1
H43A H 0.6856 0.1809 0.6264 0.266 Uiso 0.50 1 calc PR C -1
H43B H 0.5986 0.1750 0.6402 0.266 Uiso 0.50 1 calc PR C -1
C44 C 0.665(2) 0.1392(16) 0.7107(11) 0.222(6) Uiso 0.50 1 d PD C -1
H44A H 0.7051 0.1759 0.7221 0.266 Uiso 0.50 1 calc PR C -1
H44B H 0.6206 0.1508 0.7340 0.266 Uiso 0.50 1 calc PR C -1
C40 C 0.0336(10) 0.7500 0.3649(8) 0.199(4) Uiso 1 2 d SD . .
H40A H 0.0175 0.6975 0.3790 0.239 Uiso 0.50 1 calc PR B .
H40B H 0.0214 0.7902 0.3941 0.239 Uiso 0.50 1 calc PR . .


_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 Cl2 2.2777(16) . ?
Fe1 Cl2 2.2777(16) 7_565 ?
Fe1 Cl1 2.301(2) . ?
Fe1 P1 2.457(2) . ?
P1 C1 1.791(9) . ?
P1 C7 1.824(6) 7_565 ?
P1 C7 1.824(6) . ?
N1 C19 1.326(5) . ?
N1 C20 1.371(6) . ?
N1 C21 1.464(6) . ?
C1 C2 1.492(11) 7_565 ?
C1 C2 1.492(11) . ?
C1 C6 1.495(12) 7_565 ?
C1 C6 1.495(12) . ?
C2 C3 1.516(15) . ?
C3 C4 1.538(17) . ?
C4 C5 1.515(17) . ?
C5 C6 1.502(16) . ?
C7 C12A 1.390(13) . ?
C7 C8 1.451(13) . ?
C7 C12 1.458(12) . ?
C7 C8A 1.629(14) . ?
C8 C9 1.532(14) . ?
C9 C10 1.543(14) . ?
C10 C11 1.527(15) . ?
C11 C12 1.510(14) . ?
C8A C9A 1.551(14) . ?
C9A C10A 1.512(15) . ?
C10A C11A 1.486(15) . ?
C11A C12A 1.547(13) . ?
C19 N1 1.326(5) 7_565 ?
C20 C20 1.301(10) 7_565 ?
C21 C26 1.382(7) . ?
C21 C22 1.399(7) . ?
C22 C23 1.395(8) . ?
C22 C27 1.504(8) . ?
C23 C24 1.371(9) . ?
C24 C25 1.375(9) . ?
C25 C26 1.387(8) . ?
C26 C30 1.526(8) . ?
C27 C28 1.478(9) . ?
C27 C29 1.508(10) . ?
C30 C31 1.518(11) . ?
C30 C32 1.521(9) . ?
O1 C33 1.404(11) . ?
O1 C33 1.404(11) 7_565 ?
C33 C34 1.438(16) . ?
C34 C34 1.37(3) 7_565 ?
O2 C37 1.406(15) . ?
O2 C40 1.408(14) . ?
C37 C38 1.522(16) . ?
C38 C39 1.543(18) . ?
C39 C40 1.585(15) . ?
O3 C41 1.388(16) . ?
O3 C44 1.447(16) . ?
C41 C42 1.537(16) . ?
C42 C43 1.565(17) . ?
C43 C44 1.543(17) . ?
C40 O2 1.408(14) 7_575 ?

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
Cl2 Fe1 Cl2 111.70(10) . 7_565 ?
Cl2 Fe1 Cl1 111.69(6) . . ?
Cl2 Fe1 Cl1 111.69(6) 7_565 . ?
Cl2 Fe1 P1 110.33(5) . . ?
Cl2 Fe1 P1 110.33(5) 7_565 . ?
Cl1 Fe1 P1 100.58(8) . . ?
C1 P1 C7 105.2(3) . 7_565 ?
C1 P1 C7 105.2(3) . . ?
C7 P1 C7 106.1(4) 7_565 . ?
C1 P1 Fe1 115.2(3) . . ?
C7 P1 Fe1 112.2(2) 7_565 . ?
C7 P1 Fe1 112.2(2) . . ?
C19 N1 C20 108.3(4) . . ?
C19 N1 C21 123.2(4) . . ?
C20 N1 C21 128.5(4) . . ?
C2 C1 C2 12(3) 7_565 . ?
C2 C1 C6 114.8(9) 7_565 7_565 ?
C2 C1 C6 116.8(8) . 7_565 ?
C2 C1 C6 116.8(8) 7_565 . ?
C2 C1 C6 114.8(9) . . ?
C6 C1 C6 17(3) 7_565 . ?
C2 C1 P1 116.5(6) 7_565 . ?
C2 C1 P1 116.5(6) . . ?
C6 C1 P1 126.5(7) 7_565 . ?
C6 C1 P1 126.5(7) . . ?
C1 C2 C3 116.6(13) . . ?
C2 C3 C4 109.5(14) . . ?
C5 C4 C3 108.7(18) . . ?
C6 C5 C4 111.7(16) . . ?
C1 C6 C5 115.6(14) . . ?
C12A C7 C8 80.9(10) . . ?
C12A C7 C12 85.1(9) . . ?
C8 C7 C12 120.5(9) . . ?
C12A C7 C8A 111.5(9) . . ?
C8 C7 C8A 33.2(8) . . ?
C12 C7 C8A 109.3(10) . . ?
C12A C7 P1 123.0(7) . . ?
C8 C7 P1 115.6(6) . . ?
C12 C7 P1 120.4(6) . . ?
C8A C7 P1 106.2(6) . . ?
C7 C8 C9 114.1(11) . . ?
C8 C9 C10 108.1(11) . . ?
C11 C10 C9 110.9(12) . . ?
C12 C11 C10 111.0(11) . . ?
C7 C12 C11 114.8(10) . . ?
C9A C8A C7 113.7(11) . . ?
C10A C9A C8A 110.7(12) . . ?
C11A C10A C9A 113.1(12) . . ?
C10A C11A C12A 111.7(11) . . ?
C7 C12A C11A 113.5(11) . . ?
N1 C19 N1 107.8(6) 7_565 . ?
C20 C20 N1 107.9(3) 7_565 . ?
C26 C21 C22 124.9(4) . . ?
C26 C21 N1 118.2(4) . . ?
C22 C21 N1 116.9(4) . . ?
C23 C22 C21 115.8(5) . . ?
C23 C22 C27 120.7(5) . . ?
C21 C22 C27 123.5(4) . . ?
C24 C23 C22 121.1(6) . . ?
C23 C24 C25 120.4(5) . . ?
C24 C25 C26 121.7(6) . . ?
C21 C26 C25 115.9(5) . . ?
C21 C26 C30 122.9(5) . . ?
C25 C26 C30 121.2(6) . . ?
C28 C27 C22 112.3(6) . . ?
C28 C27 C29 113.1(7) . . ?
C22 C27 C29 109.1(5) . . ?
C31 C30 C32 111.3(6) . . ?
C31 C30 C26 109.8(7) . . ?
C32 C30 C26 112.3(5) . . ?
C33 O1 C33 109.9(12) . 7_565 ?
O1 C33 C34 102.7(12) . . ?
C34 C34 C33 108.8(8) 7_565 . ?
C37 O2 C40 112.5(10) . . ?
O2 C37 C38 108.0(10) . . ?
C37 C38 C39 107.3(10) . . ?
C38 C39 C40 102.4(10) . . ?
C41 O3 C44 111.6(11) . . ?
O3 C41 C42 111.7(11) . . ?
C41 C42 C43 101.8(10) . . ?
C44 C43 C42 106.5(10) . . ?
O3 C44 C43 106.6(10) . . ?
O2 C40 O2 25(2) 7_575 . ?
O2 C40 C39 107.7(16) 7_575 . ?
O2 C40 C39 107.8(9) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.098
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1485929'
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C49 H78 Br3 Fe N2 O P'
_chemical_formula_sum            'C49 H78 Br3 Fe N2 O P'
_chemical_formula_weight         1037.65

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   14.7396(4)
_cell_length_b                   15.5290(5)
_cell_length_c                   23.4470(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5366.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    31300
_cell_measurement_theta_min      2.90
_cell_measurement_theta_max      30.32

_exptl_crystal_description       Block
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2144
_exptl_absorpt_coefficient_mu    2.577
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24539
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9306
_reflns_number_gt                6780
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0424P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(8)
_refine_ls_number_reflns         9306
_refine_ls_number_parameters     522
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.0965
_refine_ls_wR_factor_gt          0.0844
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
O1 O 0.6351(3) 0.0161(4) 0.2591(2) 0.0915(16) Uani 1 1 d . . .
P1 P 0.32784(8) 0.98952(9) 0.06722(5) 0.0346(3) Uani 1 1 d . . .
Br1 Br 0.22476(4) 1.04498(4) 0.21921(2) 0.05460(18) Uani 1 1 d . . .
Br2 Br 0.09101(4) 0.87808(4) 0.12121(3) 0.06620(19) Uani 1 1 d . . .
Br3 Br 0.12284(4) 1.12567(4) 0.06890(2) 0.05112(16) Uani 1 1 d . . .
Fe1 Fe 0.18633(4) 1.00387(5) 0.12175(3) 0.03737(18) Uani 1 1 d . . .
N2 N 0.8928(2) 0.0131(2) 0.24674(13) 0.0277(9) Uani 1 1 d . . .
N1 N 0.8783(3) 0.0908(2) 0.17136(13) 0.0260(9) Uani 1 1 d . . .
C19 C 0.8340(3) 0.0463(3) 0.21087(16) 0.0282(11) Uani 1 1 d . . .
H19 H 0.7713 0.0396 0.2128 0.034 Uiso 1 1 calc R . .
C20 C 0.9686(4) 0.0861(3) 0.18323(18) 0.0341(12) Uani 1 1 d . . .
H20 H 1.0151 0.1115 0.1624 0.041 Uiso 1 1 calc R . .
C21 C 0.9783(3) 0.0388(3) 0.22975(17) 0.0305(11) Uani 1 1 d . . .
H21 H 1.0327 0.0253 0.2477 0.037 Uiso 1 1 calc R . .
C34 C 0.8726(3) -0.0433(3) 0.29501(16) 0.0293(11) Uani 1 1 d . . .
C35 C 0.8582(3) -0.1291(3) 0.28450(17) 0.0327(11) Uani 1 1 d . . .
C36 C 0.8401(4) -0.1816(4) 0.3312(2) 0.0444(14) Uani 1 1 d . . .
H36 H 0.8296 -0.2401 0.3259 0.053 Uiso 1 1 calc R . .
C37 C 0.8376(4) -0.1470(4) 0.38517(19) 0.0459(14) Uani 1 1 d . . .
H37 H 0.8263 -0.1827 0.4162 0.055 Uiso 1 1 calc R . .
C38 C 0.8514(4) -0.0611(4) 0.39374(19) 0.0474(15) Uani 1 1 d . . .
H38 H 0.8493 -0.0395 0.4307 0.057 Uiso 1 1 calc R . .
C39 C 0.8685(3) -0.0051(3) 0.34897(17) 0.0342(12) Uani 1 1 d . . .
C22 C 0.8349(3) 0.1386(3) 0.12545(17) 0.0306(11) Uani 1 1 d . . .
C23 C 0.8061(3) 0.2218(3) 0.13670(19) 0.0389(13) Uani 1 1 d . . .
C24 C 0.7613(4) 0.2640(4) 0.0936(2) 0.0530(16) Uani 1 1 d . . .
H24 H 0.7388 0.3191 0.0999 0.064 Uiso 1 1 calc R . .
C25 C 0.7493(4) 0.2255(5) 0.0410(3) 0.0597(18) Uani 1 1 d . . .
H25 H 0.7184 0.2549 0.0124 0.072 Uiso 1 1 calc R . .
C26 C 0.7819(4) 0.1458(4) 0.0306(2) 0.0560(17) Uani 1 1 d . . .
H26 H 0.7744 0.1220 -0.0056 0.067 Uiso 1 1 calc R . .
C27 C 0.8266(4) 0.0979(3) 0.07240(19) 0.0427(14) Uani 1 1 d . . .
C40 C 0.8803(4) 0.0915(3) 0.35869(19) 0.0416(13) Uani 1 1 d . . .
H40 H 0.9027 0.1158 0.3228 0.050 Uiso 1 1 calc R . .
C41 C 0.9499(6) 0.1122(5) 0.4035(3) 0.108(3) Uani 1 1 d . . .
H41A H 0.9305 0.0893 0.4396 0.162 Uiso 1 1 calc R . .
H41B H 0.9565 0.1736 0.4066 0.162 Uiso 1 1 calc R . .
H41C H 1.0070 0.0871 0.3931 0.162 Uiso 1 1 calc R . .
C42 C 0.7915(5) 0.1336(5) 0.3707(4) 0.122(3) Uani 1 1 d . . .
H42A H 0.7677 0.1123 0.4062 0.184 Uiso 1 1 calc R . .
H42B H 0.7497 0.1207 0.3405 0.184 Uiso 1 1 calc R . .
H42C H 0.7998 0.1948 0.3733 0.184 Uiso 1 1 calc R . .
C43 C 0.8577(4) -0.1671(3) 0.2246(2) 0.0430(14) Uani 1 1 d . . .
H43 H 0.8826 -0.1237 0.1985 0.052 Uiso 1 1 calc R . .
C44 C 0.7613(4) -0.1861(5) 0.2062(2) 0.0672(19) Uani 1 1 d . . .
H44A H 0.7614 -0.2074 0.1678 0.101 Uiso 1 1 calc R . .
H44B H 0.7259 -0.1343 0.2082 0.101 Uiso 1 1 calc R . .
H44C H 0.7356 -0.2287 0.2311 0.101 Uiso 1 1 calc R . .
C45 C 0.9168(4) -0.2487(4) 0.2198(2) 0.0562(16) Uani 1 1 d . . .
H45A H 0.9779 -0.2355 0.2309 0.084 Uiso 1 1 calc R . .
H45B H 0.9162 -0.2689 0.1811 0.084 Uiso 1 1 calc R . .
H45C H 0.8929 -0.2926 0.2444 0.084 Uiso 1 1 calc R . .
C28 C 0.8619(5) 0.0085(4) 0.0611(2) 0.0612(17) Uani 1 1 d . . .
H28 H 0.9060 -0.0056 0.0910 0.073 Uiso 1 1 calc R . .
C29 C 0.7855(7) -0.0559(5) 0.0647(3) 0.112(3) Uani 1 1 d . . .
H29A H 0.7521 -0.0470 0.0994 0.167 Uiso 1 1 calc R . .
H29B H 0.8099 -0.1132 0.0644 0.167 Uiso 1 1 calc R . .
H29C H 0.7457 -0.0486 0.0327 0.167 Uiso 1 1 calc R . .
C30 C 0.9095(5) 0.0004(5) 0.0036(2) 0.089(2) Uani 1 1 d . . .
H30A H 0.8672 0.0130 -0.0264 0.133 Uiso 1 1 calc R . .
H30B H 0.9320 -0.0572 -0.0009 0.133 Uiso 1 1 calc R . .
H30C H 0.9591 0.0403 0.0020 0.133 Uiso 1 1 calc R . .
C31 C 0.8238(4) 0.2656(4) 0.1939(2) 0.0542(16) Uani 1 1 d . . .
H31 H 0.8556 0.2245 0.2185 0.065 Uiso 1 1 calc R . .
C32 C 0.7368(6) 0.2912(6) 0.2233(3) 0.115(3) Uani 1 1 d . . .
H32A H 0.7032 0.3296 0.1992 0.173 Uiso 1 1 calc R . .
H32B H 0.7507 0.3195 0.2586 0.173 Uiso 1 1 calc R . .
H32C H 0.7012 0.2406 0.2308 0.173 Uiso 1 1 calc R . .
C33 C 0.8848(5) 0.3440(4) 0.1861(3) 0.0729(19) Uani 1 1 d . . .
H33A H 0.9436 0.3257 0.1733 0.109 Uiso 1 1 calc R . .
H33B H 0.8908 0.3738 0.2218 0.109 Uiso 1 1 calc R . .
H33C H 0.8586 0.3819 0.1583 0.109 Uiso 1 1 calc R . .
C1 C 0.3143(4) 0.9456(3) -0.00560(19) 0.0438(14) Uani 1 1 d . . .
H1 H 0.3750 0.9395 -0.0223 0.053 Uiso 1 1 calc R . .
C2 C 0.2701(5) 0.8563(4) -0.0048(2) 0.0632(17) Uani 1 1 d . . .
H2A H 0.3063 0.8175 0.0183 0.076 Uiso 1 1 calc R . .
H2B H 0.2102 0.8602 0.0121 0.076 Uiso 1 1 calc R . .
C3 C 0.2625(5) 0.8211(4) -0.0651(3) 0.078(2) Uani 1 1 d . . .
H3A H 0.2337 0.7649 -0.0641 0.094 Uiso 1 1 calc R . .
H3B H 0.3227 0.8141 -0.0811 0.094 Uiso 1 1 calc R . .
C4 C 0.2066(5) 0.8820(5) -0.1033(3) 0.076(2) Uani 1 1 d . . .
H4A H 0.2039 0.8591 -0.1417 0.091 Uiso 1 1 calc R . .
H4B H 0.1451 0.8861 -0.0888 0.091 Uiso 1 1 calc R . .
C5 C 0.2490(5) 0.9691(4) -0.1041(2) 0.075(2) Uani 1 1 d . . .
H5A H 0.2114 1.0078 -0.1264 0.090 Uiso 1 1 calc R . .
H5B H 0.3079 0.9656 -0.1224 0.090 Uiso 1 1 calc R . .
C6 C 0.2603(4) 1.0058(4) -0.0434(2) 0.0549(16) Uani 1 1 d . . .
H6A H 0.2910 1.0610 -0.0455 0.066 Uiso 1 1 calc R . .
H6B H 0.2009 1.0152 -0.0267 0.066 Uiso 1 1 calc R . .
C7 C 0.4163(4) 0.9234(4) 0.1025(2) 0.0553(16) Uani 1 1 d . . .
H7 H 0.4484 0.9628 0.1282 0.066 Uiso 1 1 calc R . .
C8 C 0.3756(5) 0.8554(5) 0.1404(3) 0.078(2) Uani 1 1 d . . .
H8A H 0.3414 0.8153 0.1171 0.094 Uiso 1 1 calc R . .
H8B H 0.3336 0.8825 0.1667 0.094 Uiso 1 1 calc R . .
C9 C 0.4469(5) 0.8053(5) 0.1746(3) 0.094(3) Uani 1 1 d . . .
H9A H 0.4746 0.8433 0.2024 0.113 Uiso 1 1 calc R . .
H9B H 0.4175 0.7587 0.1951 0.113 Uiso 1 1 calc R . .
C10 C 0.5177(5) 0.7695(5) 0.1372(3) 0.101(3) Uani 1 1 d . . .
H10A H 0.4912 0.7256 0.1130 0.121 Uiso 1 1 calc R . .
H10B H 0.5640 0.7424 0.1605 0.121 Uiso 1 1 calc R . .
C11 C 0.5616(5) 0.8384(6) 0.0999(3) 0.107(3) Uani 1 1 d . . .
H11A H 0.6056 0.8119 0.0746 0.128 Uiso 1 1 calc R . .
H11B H 0.5932 0.8798 0.1237 0.128 Uiso 1 1 calc R . .
C12 C 0.4889(4) 0.8843(5) 0.0648(3) 0.074(2) Uani 1 1 d . . .
H12A H 0.5170 0.9294 0.0423 0.088 Uiso 1 1 calc R . .
H12B H 0.4611 0.8436 0.0388 0.088 Uiso 1 1 calc R . .
C13 C 0.3787(3) 1.0968(3) 0.05687(19) 0.0405(13) Uani 1 1 d . . .
H13 H 0.3333 1.1298 0.0356 0.049 Uiso 1 1 calc R . .
C14 C 0.3904(4) 1.1452(3) 0.1135(2) 0.0498(15) Uani 1 1 d . . .
H14A H 0.3336 1.1446 0.1343 0.060 Uiso 1 1 calc R . .
H14B H 0.4358 1.1163 0.1366 0.060 Uiso 1 1 calc R . .
C15 C 0.4193(4) 1.2374(4) 0.1030(3) 0.0684(19) Uani 1 1 d . . .
H15A H 0.3705 1.2676 0.0837 0.082 Uiso 1 1 calc R . .
H15B H 0.4293 1.2655 0.1394 0.082 Uiso 1 1 calc R . .
C16 C 0.5027(5) 1.2447(4) 0.0682(3) 0.0743(19) Uani 1 1 d . . .
H16A H 0.5537 1.2218 0.0895 0.089 Uiso 1 1 calc R . .
H16B H 0.5148 1.3049 0.0604 0.089 Uiso 1 1 calc R . .
C17 C 0.4933(4) 1.1967(4) 0.0131(3) 0.0634(18) Uani 1 1 d . . .
H17A H 0.5507 1.1982 -0.0071 0.076 Uiso 1 1 calc R . .
H17B H 0.4483 1.2251 -0.0105 0.076 Uiso 1 1 calc R . .
C18 C 0.4656(4) 1.1043(4) 0.0221(2) 0.0566(17) Uani 1 1 d . . .
H18A H 0.5141 1.0741 0.0417 0.068 Uiso 1 1 calc R . .
H18B H 0.4568 1.0769 -0.0146 0.068 Uiso 1 1 calc R . .
C61 C 0.6140(5) -0.0330(7) 0.3068(4) 0.118(3) Uani 1 1 d . . .
H61A H 0.6540 -0.0176 0.3380 0.142 Uiso 1 1 calc R . .
H61B H 0.6228 -0.0936 0.2983 0.142 Uiso 1 1 calc R . .
C62 C 0.5237(7) -0.0187(9) 0.3229(4) 0.157(5) Uani 1 1 d . . .
H62A H 0.5209 0.0093 0.3598 0.189 Uiso 1 1 calc R . .
H62B H 0.4909 -0.0728 0.3251 0.189 Uiso 1 1 calc R . .
C63 C 0.4848(6) 0.0367(8) 0.2788(5) 0.136(4) Uani 1 1 d . . .
H63A H 0.4388 0.0060 0.2573 0.163 Uiso 1 1 calc R . .
H63B H 0.4574 0.0874 0.2957 0.163 Uiso 1 1 calc R . .
C64 C 0.5583(6) 0.0604(6) 0.2428(4) 0.103(3) Uani 1 1 d . . .
H64A H 0.5436 0.0469 0.2035 0.124 Uiso 1 1 calc R . .
H64B H 0.5690 0.1218 0.2456 0.124 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
O1 C64 1.378(8) . ?
O1 C61 1.390(8) . ?
P1 C13 1.843(5) . ?
P1 C1 1.849(5) . ?
P1 C7 1.855(6) . ?
P1 Fe1 2.4566(14) . ?
Br1 Fe1 2.4393(9) . ?
Br2 Fe1 2.4062(10) . ?
Br3 Fe1 2.4473(9) . ?
N2 C19 1.314(5) . ?
N2 C21 1.380(6) . ?
N2 C34 1.462(5) . ?
N1 C19 1.328(5) . ?
N1 C20 1.362(6) . ?
N1 C22 1.455(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.323(6) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C34 C35 1.372(7) . ?
C34 C39 1.399(6) . ?
C35 C36 1.390(6) . ?
C35 C43 1.523(7) . ?
C36 C37 1.376(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.365(7) . ?
C37 H37 0.9300 . ?
C38 C39 1.386(6) . ?
C38 H38 0.9300 . ?
C39 C40 1.527(7) . ?
C22 C23 1.385(7) . ?
C22 C27 1.401(7) . ?
C23 C24 1.374(7) . ?
C23 C31 1.527(7) . ?
C24 C25 1.381(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.351(8) . ?
C25 H25 0.9300 . ?
C26 C27 1.396(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.506(8) . ?
C40 C42 1.491(9) . ?
C40 C41 1.503(8) . ?
C40 H40 0.9800 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C44 1.514(8) . ?
C43 C45 1.542(7) . ?
C43 H43 0.9800 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C28 C29 1.509(10) . ?
C28 C30 1.524(8) . ?
C28 H28 0.9800 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.509(9) . ?
C31 C33 1.525(8) . ?
C31 H31 0.9800 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C1 C6 1.515(7) . ?
C1 C2 1.532(8) . ?
C1 H1 0.9800 . ?
C2 C3 1.521(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.541(9) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.491(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.543(7) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.505(8) . ?
C7 C12 1.515(8) . ?
C7 H7 0.9800 . ?
C8 C9 1.533(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.472(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.526(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.528(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C18 1.523(7) . ?
C13 C14 1.535(7) . ?
C13 H13 0.9800 . ?
C14 C15 1.515(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.478(8) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.500(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.506(8) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C61 C62 1.401(11) . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C62 C63 1.463(13) . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?
C63 C64 1.421(11) . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?

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
C64 O1 C61 108.2(6) . . ?
C13 P1 C1 104.8(2) . . ?
C13 P1 C7 105.9(3) . . ?
C1 P1 C7 106.5(3) . . ?
C13 P1 Fe1 109.40(16) . . ?
C1 P1 Fe1 114.99(19) . . ?
C7 P1 Fe1 114.49(17) . . ?
Br2 Fe1 Br1 110.67(3) . . ?
Br2 Fe1 Br3 113.67(4) . . ?
Br1 Fe1 Br3 111.15(4) . . ?
Br2 Fe1 P1 114.80(4) . . ?
Br1 Fe1 P1 108.31(4) . . ?
Br3 Fe1 P1 97.54(4) . . ?
C19 N2 C21 107.7(4) . . ?
C19 N2 C34 126.6(4) . . ?
C21 N2 C34 125.7(4) . . ?
C19 N1 C20 108.0(4) . . ?
C19 N1 C22 124.5(4) . . ?
C20 N1 C22 127.4(4) . . ?
N2 C19 N1 109.0(4) . . ?
N2 C19 H19 125.5 . . ?
N1 C19 H19 125.5 . . ?
C21 C20 N1 107.7(4) . . ?
C21 C20 H20 126.1 . . ?
N1 C20 H20 126.1 . . ?
C20 C21 N2 107.4(4) . . ?
C20 C21 H21 126.3 . . ?
N2 C21 H21 126.3 . . ?
C35 C34 C39 124.6(4) . . ?
C35 C34 N2 118.3(4) . . ?
C39 C34 N2 117.1(4) . . ?
C34 C35 C36 117.3(4) . . ?
C34 C35 C43 122.8(4) . . ?
C36 C35 C43 119.9(5) . . ?
C37 C36 C35 120.1(5) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C38 C37 C36 120.9(5) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C37 C38 C39 121.9(4) . . ?
C37 C38 H38 119.0 . . ?
C39 C38 H38 119.0 . . ?
C38 C39 C34 115.3(5) . . ?
C38 C39 C40 121.6(4) . . ?
C34 C39 C40 123.1(4) . . ?
C23 C22 C27 124.3(4) . . ?
C23 C22 N1 118.0(4) . . ?
C27 C22 N1 117.7(4) . . ?
C24 C23 C22 116.9(5) . . ?
C24 C23 C31 121.1(5) . . ?
C22 C23 C31 122.0(4) . . ?
C23 C24 C25 120.8(6) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C26 C25 C24 120.9(5) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 121.9(5) . . ?
C25 C26 H26 119.1 . . ?
C27 C26 H26 119.1 . . ?
C26 C27 C22 115.2(5) . . ?
C26 C27 C28 122.0(5) . . ?
C22 C27 C28 122.8(4) . . ?
C42 C40 C41 111.9(6) . . ?
C42 C40 C39 111.0(5) . . ?
C41 C40 C39 113.1(5) . . ?
C42 C40 H40 106.8 . . ?
C41 C40 H40 106.8 . . ?
C39 C40 H40 106.8 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C35 110.0(4) . . ?
C44 C43 C45 110.4(5) . . ?
C35 C43 C45 112.5(4) . . ?
C44 C43 H43 107.9 . . ?
C35 C43 H43 107.9 . . ?
C45 C43 H43 107.9 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C29 C28 C27 110.1(6) . . ?
C29 C28 C30 109.8(5) . . ?
C27 C28 C30 112.9(5) . . ?
C29 C28 H28 107.9 . . ?
C27 C28 H28 107.9 . . ?
C30 C28 H28 107.9 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C33 110.3(5) . . ?
C32 C31 C23 111.9(5) . . ?
C33 C31 C23 110.5(4) . . ?
C32 C31 H31 108.0 . . ?
C33 C31 H31 108.0 . . ?
C23 C31 H31 108.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C6 C1 C2 110.0(5) . . ?
C6 C1 P1 111.7(4) . . ?
C2 C1 P1 111.6(3) . . ?
C6 C1 H1 107.8 . . ?
C2 C1 H1 107.8 . . ?
P1 C1 H1 107.8 . . ?
C3 C2 C1 110.2(5) . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C2 C3 C4 111.0(5) . . ?
C2 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C5 C4 C3 109.9(6) . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C4 C5 C6 111.6(5) . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C1 C6 C5 111.7(5) . . ?
C1 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C1 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C8 C7 C12 110.2(5) . . ?
C8 C7 P1 111.8(4) . . ?
C12 C7 P1 117.2(4) . . ?
C8 C7 H7 105.5 . . ?
C12 C7 H7 105.5 . . ?
P1 C7 H7 105.5 . . ?
C7 C8 C9 113.1(6) . . ?
C7 C8 H8A 109.0 . . ?
C9 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C8 111.4(6) . . ?
C10 C9 H9A 109.3 . . ?
C8 C9 H9A 109.3 . . ?
C10 C9 H9B 109.3 . . ?
C8 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
C9 C10 C11 112.2(6) . . ?
C9 C10 H10A 109.2 . . ?
C11 C10 H10A 109.2 . . ?
C9 C10 H10B 109.2 . . ?
C11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
C10 C11 C12 109.8(6) . . ?
C10 C11 H11A 109.7 . . ?
C12 C11 H11A 109.7 . . ?
C10 C11 H11B 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
C7 C12 C11 111.6(5) . . ?
C7 C12 H12A 109.3 . . ?
C11 C12 H12A 109.3 . . ?
C7 C12 H12B 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
C18 C13 C14 109.3(4) . . ?
C18 C13 P1 118.8(4) . . ?
C14 C13 P1 112.0(3) . . ?
C18 C13 H13 105.2 . . ?
C14 C13 H13 105.2 . . ?
P1 C13 H13 105.2 . . ?
C15 C14 C13 110.7(4) . . ?
C15 C14 H14A 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C16 C15 C14 113.3(5) . . ?
C16 C15 H15A 108.9 . . ?
C14 C15 H15A 108.9 . . ?
C16 C15 H15B 108.9 . . ?
C14 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 C17 111.1(5) . . ?
C15 C16 H16A 109.4 . . ?
C17 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
C17 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
C16 C17 C18 112.1(5) . . ?
C16 C17 H17A 109.2 . . ?
C18 C17 H17A 109.2 . . ?
C16 C17 H17B 109.2 . . ?
C18 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C17 C18 C13 112.1(5) . . ?
C17 C18 H18A 109.2 . . ?
C13 C18 H18A 109.2 . . ?
C17 C18 H18B 109.2 . . ?
C13 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
O1 C61 C62 110.1(8) . . ?
O1 C61 H61A 109.6 . . ?
C62 C61 H61A 109.6 . . ?
O1 C61 H61B 109.6 . . ?
C62 C61 H61B 109.6 . . ?
H61A C61 H61B 108.2 . . ?
C61 C62 C63 105.9(8) . . ?
C61 C62 H62A 110.5 . . ?
C63 C62 H62A 110.5 . . ?
C61 C62 H62B 110.5 . . ?
C63 C62 H62B 110.5 . . ?
H62A C62 H62B 108.7 . . ?
C64 C63 C62 105.9(7) . . ?
C64 C63 H63A 110.6 . . ?
C62 C63 H63A 110.6 . . ?
C64 C63 H63B 110.6 . . ?
C62 C63 H63B 110.6 . . ?
H63A C63 H63B 108.7 . . ?
O1 C64 C63 109.4(7) . . ?
O1 C64 H64A 109.8 . . ?
C63 C64 H64A 109.8 . . ?
O1 C64 H64B 109.8 . . ?
C63 C64 H64B 109.8 . . ?
H64A C64 H64B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.067
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1485930'
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H53 Cl3 Fe N2 O2'
_chemical_formula_sum            'C35 H53 Cl3 Fe N2 O2'
_chemical_formula_weight         695.99

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'
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           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   12.168(2)
_cell_length_b                   32.246(6)
_cell_length_c                   9.841(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.59(3)
_cell_angle_gamma                90.00
_cell_volume                     3835.7(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7089
_cell_measurement_theta_min      3.5650
_cell_measurement_theta_max      27.3080

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8947
_exptl_absorpt_correction_T_max  0.9395
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22584
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.82
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6751
_reflns_number_gt                5351
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0465P)²+4.5317P] 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         6751
_refine_ls_number_parameters     396
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1288
_refine_ls_wR_factor_gt          0.1213
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_restrained_S_all      0.989
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.83581(4) 0.172345(14) 0.31140(5) 0.04979(15) Uani 1 1 d . . .
Cl2 Cl 0.68122(7) 0.17769(3) 0.15835(9) 0.0652(3) Uani 1 1 d . . .
Cl3 Cl 0.82453(8) 0.13739(3) 0.50936(9) 0.0622(2) Uani 1 1 d . . .
Cl1 Cl 0.99467(9) 0.15871(5) 0.21612(10) 0.0941(4) Uani 1 1 d . . .
N1 N 0.81599(18) -0.08234(6) 0.3686(2) 0.0347(5) Uani 1 1 d . . .
N2 N 0.73087(18) -0.13758(6) 0.4212(2) 0.0341(5) Uani 1 1 d . . .
C20 C 0.6410(2) -0.16697(8) 0.4286(3) 0.0368(6) Uani 1 1 d . . .
C5 C 0.7202(2) -0.10235(8) 0.3513(3) 0.0346(6) Uani 1 1 d . . .
H5 H 0.6549 -0.0930 0.2978 0.042 Uiso 1 1 calc R . .
C8 C 0.8339(2) -0.04136(8) 0.3127(3) 0.0369(6) Uani 1 1 d . . .
C21 C 0.5688(2) -0.15976(8) 0.5250(3) 0.0412(7) Uani 1 1 d . . .
C9 C 0.8203(2) -0.00738(8) 0.3966(3) 0.0396(6) Uani 1 1 d . . .
C25 C 0.6326(2) -0.20002(8) 0.3360(3) 0.0413(7) Uani 1 1 d . . .
C17 C 0.7834(3) -0.01148(9) 0.5379(3) 0.0467(7) Uani 1 1 d . . .
H17 H 0.7976 -0.0408 0.5685 0.056 Uiso 1 1 calc R . .
C22 C 0.4807(3) -0.18753(10) 0.5266(3) 0.0500(8) Uani 1 1 d . . .
H22 H 0.4285 -0.1837 0.5903 0.060 Uiso 1 1 calc R . .
C14 C 0.8797(3) -0.07669(10) 0.0932(3) 0.0532(8) Uani 1 1 d . . .
H14 H 0.8358 -0.1000 0.1266 0.064 Uiso 1 1 calc R . .
C12 C 0.8786(3) 0.00117(10) 0.1314(3) 0.0536(8) Uani 1 1 d . . .
H12 H 0.8980 0.0046 0.0413 0.064 Uiso 1 1 calc R . .
C13 C 0.8625(2) -0.03868(9) 0.1798(3) 0.0439(7) Uani 1 1 d . . .
C6 C 0.8902(2) -0.10553(9) 0.4528(3) 0.0433(7) Uani 1 1 d . . .
H6 H 0.9650 -0.0985 0.4822 0.052 Uiso 1 1 calc R . .
C24 C 0.5430(3) -0.22669(9) 0.3432(3) 0.0512(8) Uani 1 1 d . . .
H24 H 0.5331 -0.2496 0.2823 0.061 Uiso 1 1 calc R . .
C29 C 0.5822(3) -0.12405(9) 0.6269(3) 0.0511(8) Uani 1 1 d . . .
H29 H 0.6455 -0.1066 0.6041 0.061 Uiso 1 1 calc R . .
C7 C 0.8369(2) -0.13997(8) 0.4857(3) 0.0428(7) Uani 1 1 d . . .
H7 H 0.8670 -0.1619 0.5428 0.051 Uiso 1 1 calc R . .
C10 C 0.8378(3) 0.03163(9) 0.3409(3) 0.0499(8) Uani 1 1 d . . .
H10 H 0.8293 0.0558 0.3940 0.060 Uiso 1 1 calc R . .
C23 C 0.4689(3) -0.22039(10) 0.4367(3) 0.0531(8) Uani 1 1 d . . .
H23 H 0.4086 -0.2390 0.4393 0.064 Uiso 1 1 calc R . .
O1 O 0.8580(2) 0.23384(8) 0.3688(3) 0.0892(10) Uani 1 1 d . . .
C26 C 0.7126(3) -0.20546(10) 0.2307(3) 0.0538(8) Uani 1 1 d . . .
H26 H 0.7828 -0.1909 0.2655 0.065 Uiso 1 1 calc R . .
C11 C 0.8670(3) 0.03564(9) 0.2109(4) 0.0563(9) Uani 1 1 d . . .
H11 H 0.8793 0.0624 0.1755 0.068 Uiso 1 1 calc R . .
C30 C 0.4790(3) -0.09681(12) 0.6152(4) 0.0769(11) Uani 1 1 d . . .
H30A H 0.4626 -0.0870 0.5209 0.115 Uiso 1 1 calc R . .
H30B H 0.4918 -0.0730 0.6768 0.115 Uiso 1 1 calc R . .
H30C H 0.4163 -0.1130 0.6405 0.115 Uiso 1 1 calc R . .
C16 C 1.0013(3) -0.08939(11) 0.1104(4) 0.0643(10) Uani 1 1 d . . .
H16A H 1.0467 -0.0660 0.0868 0.096 Uiso 1 1 calc R . .
H16B H 1.0119 -0.1128 0.0498 0.096 Uiso 1 1 calc R . .
H16C H 1.0233 -0.0976 0.2055 0.096 Uiso 1 1 calc R . .
C18 C 0.8482(3) 0.01665(12) 0.6426(4) 0.0705(10) Uani 1 1 d . . .
H18A H 0.8310 0.0457 0.6197 0.106 Uiso 1 1 calc R . .
H18B H 0.9276 0.0118 0.6415 0.106 Uiso 1 1 calc R . .
H18C H 0.8276 0.0105 0.7339 0.106 Uiso 1 1 calc R . .
C15 C 0.8402(3) -0.06980(13) -0.0586(4) 0.0741(11) Uani 1 1 d . . .
H15A H 0.7641 -0.0593 -0.0684 0.111 Uiso 1 1 calc R . .
H15B H 0.8426 -0.0961 -0.1079 0.111 Uiso 1 1 calc R . .
H15C H 0.8885 -0.0496 -0.0966 0.111 Uiso 1 1 calc R . .
C28 C 0.7410(4) -0.25088(12) 0.2071(5) 0.0782(12) Uani 1 1 d . . .
H28A H 0.7703 -0.2636 0.2942 0.117 Uiso 1 1 calc R . .
H28B H 0.7967 -0.2525 0.1428 0.117 Uiso 1 1 calc R . .
H28C H 0.6741 -0.2657 0.1691 0.117 Uiso 1 1 calc R . .
C31 C 0.6100(3) -0.13992(12) 0.7719(4) 0.0695(10) Uani 1 1 d . . .
H31A H 0.5503 -0.1580 0.7956 0.104 Uiso 1 1 calc R . .
H31B H 0.6183 -0.1164 0.8353 0.104 Uiso 1 1 calc R . .
H31C H 0.6793 -0.1556 0.7784 0.104 Uiso 1 1 calc R . .
C19 C 0.6598(3) -0.00378(15) 0.5329(5) 0.0831(12) Uani 1 1 d . . .
H19A H 0.6434 0.0250 0.5057 0.125 Uiso 1 1 calc R . .
H19B H 0.6364 -0.0088 0.6236 0.125 Uiso 1 1 calc R . .
H19C H 0.6199 -0.0226 0.4663 0.125 Uiso 1 1 calc R . .
C27 C 0.6676(4) -0.18500(13) 0.0961(4) 0.0858(13) Uani 1 1 d . . .
H27A H 0.5981 -0.1984 0.0600 0.129 Uiso 1 1 calc R . .
H27B H 0.7216 -0.1879 0.0301 0.129 Uiso 1 1 calc R . .
H27C H 0.6542 -0.1555 0.1117 0.129 Uiso 1 1 calc R . .
C2 C 0.8488(4) 0.30552(12) 0.3527(5) 0.0839(13) Uani 1 1 d . . .
H2A H 0.8259 0.3231 0.2720 0.101 Uiso 1 1 calc R . .
H2B H 0.8375 0.3212 0.4366 0.101 Uiso 1 1 calc R . .
C1 C 0.7864(4) 0.26683(14) 0.3455(8) 0.132(3) Uani 1 1 d . . .
H1A H 0.7336 0.2670 0.4149 0.159 Uiso 1 1 calc R . .
H1B H 0.7437 0.2640 0.2541 0.159 Uiso 1 1 calc R . .
C3 C 0.9629(5) 0.29296(16) 0.3550(7) 0.124(2) Uani 1 1 d . . .
H3A H 1.0133 0.3121 0.4108 0.149 Uiso 1 1 calc R . .
H3B H 0.9852 0.2912 0.2615 0.149 Uiso 1 1 calc R . .
C4 C 0.9601(6) 0.25086(18) 0.4202(11) 0.211(5) Uani 1 1 d . . .
H4A H 1.0217 0.2334 0.3954 0.253 Uiso 1 1 calc R . .
H4B H 0.9661 0.2533 0.5211 0.253 Uiso 1 1 calc R . .
O2 O 0.5003(3) -0.08171(13) 0.1996(5) 0.1514(19) Uani 1 1 d . . .
C34 C 0.3237(4) -0.08723(19) 0.0957(6) 0.1095(18) Uani 1 1 d . . .
H34A H 0.2702 -0.0730 0.1483 0.131 Uiso 1 1 calc R . .
H34B H 0.2832 -0.1068 0.0307 0.131 Uiso 1 1 calc R . .
C35 C 0.4069(5) -0.1083(2) 0.1853(7) 0.134(2) Uani 1 1 d . . .
H35A H 0.3805 -0.1135 0.2753 0.161 Uiso 1 1 calc R . .
H35B H 0.4256 -0.1352 0.1454 0.161 Uiso 1 1 calc R . .
C32 C 0.4893(4) -0.0514(2) 0.1012(7) 0.133(2) Uani 1 1 d . . .
H32A H 0.5491 -0.0536 0.0413 0.160 Uiso 1 1 calc R . .
H32B H 0.4927 -0.0236 0.1438 0.160 Uiso 1 1 calc R . .
C33 C 0.3856(6) -0.0579(3) 0.0254(8) 0.181(4) Uani 1 1 d . . .
H33A H 0.3957 -0.0686 -0.0667 0.217 Uiso 1 1 calc R . .
H33B H 0.3448 -0.0313 0.0143 0.217 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 O1 2.071(3) . ?
Fe1 Cl3 2.2684(10) . ?
Fe1 Cl2 2.2774(12) . ?
Fe1 Cl1 2.2857(13) . ?
N1 C5 1.326(3) . ?
N1 C6 1.374(3) . ?
N1 C8 1.457(3) . ?
N2 C5 1.327(3) . ?
N2 C7 1.373(4) . ?
N2 C20 1.455(3) . ?
C20 C21 1.385(4) . ?
C20 C25 1.399(4) . ?
C8 C9 1.393(4) . ?
C8 C13 1.395(4) . ?
C21 C22 1.398(4) . ?
C21 C29 1.523(4) . ?
C9 C10 1.398(4) . ?
C9 C17 1.516(4) . ?
C25 C24 1.396(4) . ?
C25 C26 1.512(4) . ?
C17 C19 1.519(5) . ?
C17 C18 1.523(5) . ?
C22 C23 1.377(4) . ?
C14 C13 1.521(4) . ?
C14 C16 1.526(5) . ?
C14 C15 1.532(5) . ?
C12 C11 1.376(5) . ?
C12 C13 1.392(4) . ?
C6 C7 1.344(4) . ?
C24 C23 1.376(5) . ?
C29 C31 1.517(5) . ?
C29 C30 1.526(5) . ?
C10 C11 1.373(5) . ?
O1 C1 1.378(5) . ?
O1 C4 1.398(6) . ?
C26 C27 1.524(5) . ?
C26 C28 1.529(5) . ?
C2 C3 1.444(7) . ?
C2 C1 1.458(6) . ?
C3 C4 1.504(9) . ?
O2 C32 1.371(6) . ?
O2 C35 1.419(6) . ?
C34 C35 1.435(7) . ?
C34 C33 1.436(8) . ?
C32 C33 1.406(8) . ?

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
O1 Fe1 Cl3 105.08(10) . . ?
O1 Fe1 Cl2 100.38(8) . . ?
Cl3 Fe1 Cl2 118.61(4) . . ?
O1 Fe1 Cl1 101.89(10) . . ?
Cl3 Fe1 Cl1 113.21(5) . . ?
Cl2 Fe1 Cl1 114.61(4) . . ?
C5 N1 C6 108.6(2) . . ?
C5 N1 C8 124.1(2) . . ?
C6 N1 C8 127.2(2) . . ?
C5 N2 C7 108.6(2) . . ?
C5 N2 C20 123.7(2) . . ?
C7 N2 C20 127.7(2) . . ?
C21 C20 C25 124.7(3) . . ?
C21 C20 N2 117.7(2) . . ?
C25 C20 N2 117.6(3) . . ?
N1 C5 N2 108.5(2) . . ?
C9 C8 C13 124.5(2) . . ?
C9 C8 N1 117.2(2) . . ?
C13 C8 N1 118.3(2) . . ?
C20 C21 C22 116.6(3) . . ?
C20 C21 C29 123.3(3) . . ?
C22 C21 C29 120.1(3) . . ?
C8 C9 C10 116.2(3) . . ?
C8 C9 C17 122.9(2) . . ?
C10 C9 C17 120.8(3) . . ?
C24 C25 C20 115.8(3) . . ?
C24 C25 C26 122.1(3) . . ?
C20 C25 C26 122.0(3) . . ?
C9 C17 C19 110.7(3) . . ?
C9 C17 C18 112.6(3) . . ?
C19 C17 C18 111.0(3) . . ?
C23 C22 C21 120.6(3) . . ?
C13 C14 C16 110.4(3) . . ?
C13 C14 C15 112.4(3) . . ?
C16 C14 C15 109.8(3) . . ?
C11 C12 C13 121.6(3) . . ?
C12 C13 C8 116.0(3) . . ?
C12 C13 C14 121.2(3) . . ?
C8 C13 C14 122.7(3) . . ?
C7 C6 N1 107.0(2) . . ?
C23 C24 C25 121.2(3) . . ?
C31 C29 C21 111.1(3) . . ?
C31 C29 C30 110.9(3) . . ?
C21 C29 C30 111.1(3) . . ?
C6 C7 N2 107.2(2) . . ?
C11 C10 C9 121.2(3) . . ?
C24 C23 C22 121.0(3) . . ?
C1 O1 C4 106.0(4) . . ?
C1 O1 Fe1 129.3(3) . . ?
C4 O1 Fe1 123.9(3) . . ?
C25 C26 C27 110.5(3) . . ?
C25 C26 C28 112.9(3) . . ?
C27 C26 C28 110.4(3) . . ?
C10 C11 C12 120.5(3) . . ?
C3 C2 C1 104.8(4) . . ?
O1 C1 C2 109.7(4) . . ?
C2 C3 C4 101.0(5) . . ?
O1 C4 C3 105.2(5) . . ?
C32 O2 C35 110.4(4) . . ?
C35 C34 C33 103.7(5) . . ?
O2 C35 C34 106.0(5) . . ?
O2 C32 C33 106.2(5) . . ?
C32 C33 C34 109.3(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.049
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6
_database_code_depnum_ccdc_archive 'CCDC 1485931'
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2016-09-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H58 Br3 Fe N2 P, 2(C4H8O)'
_chemical_formula_sum            'C47 H74 Br3 Fe N2 O2 P'
_chemical_formula_weight         1025.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3255(4)
_cell_length_b                   13.2264(5)
_cell_length_c                   18.6540(9)
_cell_angle_alpha                99.408(4)
_cell_angle_beta                 102.800(4)
_cell_angle_gamma                105.251(3)
_cell_volume                     2554.82(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6448
_cell_measurement_theta_min      3.2120
_cell_measurement_theta_max      24.6740

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_size_max          0.7500
_exptl_crystal_size_mid          0.5500
_exptl_crystal_size_min          0.3500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    2.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.16758
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) 
(compiled Aug  2 2013,16:46:58) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4471
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23091
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9001
_reflns_number_gt                5344
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) 
(compiled Aug  2 2013,16:46:58) 
;
_computing_cell_refinement       
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) 
(compiled Aug  2 2013,16:46:58) 
;
_computing_data_reduction        
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) 
(compiled Aug  2 2013,16:46:58) 
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.1218P)²+0.0000P] 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         9001
_refine_ls_number_parameters     451
_refine_ls_number_restraints     136
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0782
_refine_ls_wR_factor_ref         0.2405
_refine_ls_wR_factor_gt          0.2108
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.011
_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 0.08788(9) 0.28526(8) 0.25167(6) 0.0530(3) Uani 1 1 d . . .
Br1 Br -0.03646(7) 0.11387(6) 0.16172(5) 0.0667(3) Uani 1 1 d . . .
Br2 Br -0.02906(8) 0.41491(6) 0.25371(5) 0.0740(3) Uani 1 1 d . . .
Br3 Br 0.29759(8) 0.35393(7) 0.23619(6) 0.0780(3) Uani 1 1 d . . .
N1 N 0.3306(5) 0.8279(4) 0.0415(3) 0.0501(14) Uani 1 1 d . . .
N3 N 0.2639(6) 0.6527(5) 0.0052(4) 0.0553(15) Uani 1 1 d . . .
O1 O 1.049(3) 0.745(3) 0.3351(13) 0.416(17) Uani 1 1 d DU . .
O2 O 0.4836(10) 0.7235(7) 0.2119(5) 0.143(3) Uani 1 1 d DU . .
P1 P 0.13247(17) 0.25374(14) 0.37885(11) 0.0479(5) Uani 1 1 d . . .
C1 C 0.1844(13) 0.3823(8) 0.4503(6) 0.1240(18) Uani 1 1 d D . .
H1 H 0.1127 0.4131 0.4378 0.149 Uiso 1 1 calc R . .
C2 C 0.2969(13) 0.4643(7) 0.4402(7) 0.1240(18) Uani 1 1 d D . .
H2A H 0.2844 0.4642 0.3860 0.149 Uiso 1 1 calc R . .
H2B H 0.3757 0.4456 0.4584 0.149 Uiso 1 1 calc R . .
C3 C 0.3096(14) 0.5789(8) 0.4866(6) 0.1240(18) Uani 1 1 d D . .
H3A H 0.3848 0.6326 0.4813 0.149 Uiso 1 1 calc R . .
H3B H 0.2332 0.5990 0.4655 0.149 Uiso 1 1 calc R . .
C4 C 0.3232(13) 0.5820(8) 0.5660(6) 0.1240(18) Uani 1 1 d D . .
H4A H 0.3256 0.6540 0.5925 0.149 Uiso 1 1 calc R . .
H4B H 0.4045 0.5699 0.5887 0.149 Uiso 1 1 calc R . .
C5 C 0.2183(13) 0.5002(7) 0.5756(7) 0.1240(18) Uani 1 1 d D . .
H5A H 0.1382 0.5167 0.5572 0.149 Uiso 1 1 calc R . .
H5B H 0.2315 0.5023 0.6302 0.149 Uiso 1 1 calc R . .
C6 C 0.2046(14) 0.3840(8) 0.5323(6) 0.1240(18) Uani 1 1 d D . .
H6A H 0.2826 0.3650 0.5518 0.149 Uiso 1 1 calc R . .
H6B H 0.1313 0.3308 0.5398 0.149 Uiso 1 1 calc R . .
C7 C -0.0017(10) 0.1686(9) 0.4045(9) 0.147(2) Uani 1 1 d D . .
H7 H 0.0243 0.1717 0.4598 0.176 Uiso 1 1 calc R . .
C8 C -0.1169(10) 0.2076(10) 0.3865(10) 0.147(2) Uani 1 1 d D . .
H8A H -0.1436 0.2041 0.3317 0.176 Uiso 1 1 calc R . .
H8B H -0.0944 0.2836 0.4142 0.176 Uiso 1 1 calc R . .
C9 C -0.2297(10) 0.1361(9) 0.4097(9) 0.147(2) Uani 1 1 d DU . .
H9A H -0.2040 0.1430 0.4650 0.176 Uiso 1 1 calc R . .
H9B H -0.3038 0.1630 0.3977 0.176 Uiso 1 1 calc R . .
C10 C -0.2663(10) 0.0261(9) 0.3722(9) 0.147(2) Uani 1 1 d DU . .
H10A H -0.3040 0.0184 0.3176 0.176 Uiso 1 1 calc R . .
H10B H -0.3331 -0.0155 0.3918 0.176 Uiso 1 1 calc R . .
C11 C -0.1604(10) -0.0207(10) 0.3812(10) 0.147(2) Uani 1 1 d D . .
H11A H -0.1891 -0.0936 0.3474 0.176 Uiso 1 1 calc R . .
H11B H -0.1331 -0.0272 0.4340 0.176 Uiso 1 1 calc R . .
C12 C -0.0466(10) 0.0537(9) 0.3612(9) 0.147(2) Uani 1 1 d D . .
H12A H 0.0257 0.0241 0.3705 0.176 Uiso 1 1 calc R . .
H12B H -0.0722 0.0515 0.3065 0.176 Uiso 1 1 calc R . .
C13 C 0.2642(7) 0.1938(6) 0.3946(4) 0.063(2) Uani 1 1 d D . .
H13 H 0.3420 0.2528 0.3968 0.076 Uiso 1 1 calc R . .
C14 C 0.2963(10) 0.1590(9) 0.4673(5) 0.104(4) Uani 1 1 d D . .
H14A H 0.2246 0.0978 0.4682 0.125 Uiso 1 1 calc R . .
H14B H 0.3104 0.2193 0.5107 0.125 Uiso 1 1 calc R . .
C15 C 0.4192(10) 0.1246(9) 0.4738(7) 0.126(4) Uani 1 1 d D . .
H15A H 0.4917 0.1865 0.4749 0.151 Uiso 1 1 calc R . .
H15B H 0.4404 0.1004 0.5212 0.151 Uiso 1 1 calc R . .
C16 C 0.3958(10) 0.0343(8) 0.4069(6) 0.099(3) Uani 1 1 d D . .
H16A H 0.4715 0.0091 0.4116 0.119 Uiso 1 1 calc R . .
H16B H 0.3222 -0.0269 0.4056 0.119 Uiso 1 1 calc R . .
C17 C 0.3701(11) 0.0709(9) 0.3370(6) 0.110(4) Uani 1 1 d D . .
H17A H 0.3593 0.0119 0.2935 0.132 Uiso 1 1 calc R . .
H17B H 0.4435 0.1325 0.3387 0.132 Uiso 1 1 calc R . .
C18 C 0.2477(9) 0.1058(7) 0.3259(5) 0.084(3) Uani 1 1 d D . .
H18A H 0.2336 0.1334 0.2795 0.101 Uiso 1 1 calc R . .
H18B H 0.1728 0.0432 0.3204 0.101 Uiso 1 1 calc R . .
C19 C 0.3379(7) 0.7357(6) 0.0613(4) 0.0531(18) Uani 1 1 d . . .
H19 H 0.3881 0.7310 0.1080 0.064 Uiso 1 1 calc R . .
C20 C 0.2514(7) 0.8003(6) -0.0310(5) 0.062(2) Uani 1 1 d . . .
H20 H 0.2306 0.8491 -0.0601 0.074 Uiso 1 1 calc R . .
C21 C 0.2081(7) 0.6906(7) -0.0537(5) 0.065(2) Uani 1 1 d . . .
H21 H 0.1507 0.6485 -0.1009 0.078 Uiso 1 1 calc R . .
C22 C 0.3982(6) 0.9341(5) 0.0875(4) 0.0517(17) Uani 1 1 d . . .
C23 C 0.5292(7) 0.9702(6) 0.1069(5) 0.0578(19) Uani 1 1 d . . .
C24 C 0.5899(7) 1.0725(6) 0.1493(5) 0.0609(19) Uani 1 1 d . . .
H24 H 0.6803 1.0989 0.1621 0.073 Uiso 1 1 calc R . .
C25 C 0.5231(8) 1.1409(6) 0.1748(4) 0.0609(19) Uani 1 1 d . . .
C26 C 0.3929(7) 1.1001(6) 0.1530(5) 0.062(2) Uani 1 1 d . . .
H26 H 0.3460 1.1455 0.1683 0.075 Uiso 1 1 calc R . .
C27 C 0.3257(7) 0.9968(6) 0.1100(5) 0.0565(19) Uani 1 1 d . . .
C28 C 0.6060(8) 0.9033(7) 0.0794(6) 0.088(3) Uani 1 1 d . . .
H28A H 0.6921 0.9500 0.0850 0.132 Uiso 1 1 calc R . .
H28B H 0.5650 0.8668 0.0260 0.132 Uiso 1 1 calc R . .
H28C H 0.6110 0.8494 0.1093 0.132 Uiso 1 1 calc R . .
C29 C 0.5951(9) 1.2546(6) 0.2217(5) 0.079(2) Uani 1 1 d . . .
H29A H 0.6257 1.3001 0.1889 0.119 Uiso 1 1 calc R . .
H29B H 0.6679 1.2533 0.2610 0.119 Uiso 1 1 calc R . .
H29C H 0.5383 1.2838 0.2454 0.119 Uiso 1 1 calc R . .
C30 C 0.1833(7) 0.9552(7) 0.0903(6) 0.082(3) Uani 1 1 d . . .
H30A H 0.1518 1.0081 0.1170 0.123 Uiso 1 1 calc R . .
H30B H 0.1573 0.8870 0.1054 0.123 Uiso 1 1 calc R . .
H30C H 0.1476 0.9434 0.0356 0.123 Uiso 1 1 calc R . .
C31 C 0.2422(7) 0.5405(5) 0.0077(5) 0.0576(19) Uani 1 1 d . . .
C32 C 0.1708(7) 0.4992(6) 0.0539(4) 0.0571(18) Uani 1 1 d . . .
C33 C 0.1501(8) 0.3899(6) 0.0521(5) 0.070(2) Uani 1 1 d . . .
H33 H 0.1023 0.3591 0.0835 0.084 Uiso 1 1 calc R . .
C34 C 0.1959(8) 0.3236(6) 0.0068(5) 0.067(2) Uani 1 1 d . . .
C35 C 0.2686(8) 0.3708(6) -0.0360(5) 0.076(2) Uani 1 1 d . . .
H35 H 0.3060 0.3284 -0.0644 0.091 Uiso 1 1 calc R . .
C36 C 0.2898(8) 0.4784(7) -0.0393(5) 0.072(2) Uani 1 1 d . . .
C37 C 0.1175(8) 0.5646(6) 0.1018(5) 0.074(2) Uani 1 1 d . . .
H37A H 0.1869 0.6245 0.1378 0.110 Uiso 1 1 calc R . .
H37B H 0.0707 0.5195 0.1295 0.110 Uiso 1 1 calc R . .
H37C H 0.0595 0.5932 0.0699 0.110 Uiso 1 1 calc R . .
C38 C 0.1730(9) 0.2082(6) 0.0108(6) 0.089(3) Uani 1 1 d . . .
H38A H 0.1381 0.1618 -0.0404 0.133 Uiso 1 1 calc R . .
H38B H 0.1122 0.1895 0.0403 0.133 Uiso 1 1 calc R . .
H38C H 0.2536 0.1979 0.0352 0.133 Uiso 1 1 calc R . .
C39 C 0.3685(10) 0.5259(7) -0.0884(6) 0.097(3) Uani 1 1 d . . .
H39A H 0.4101 0.4749 -0.1070 0.146 Uiso 1 1 calc R . .
H39B H 0.4334 0.5936 -0.0586 0.146 Uiso 1 1 calc R . .
H39C H 0.3131 0.5400 -0.1314 0.146 Uiso 1 1 calc R . .
C40 C 1.1096(19) 0.782(3) 0.2794(16) 0.325(15) Uani 1 1 d DU . .
H40A H 1.1516 0.7307 0.2605 0.390 Uiso 1 1 calc R . .
H40B H 1.1748 0.8535 0.3020 0.390 Uiso 1 1 calc R . .
C41 C 1.006(2) 0.7900(15) 0.2149(11) 0.236(10) Uani 1 1 d DU . .
H41A H 1.0189 0.8661 0.2124 0.283 Uiso 1 1 calc R . .
H41B H 1.0082 0.7488 0.1661 0.283 Uiso 1 1 calc R . .
C42 C 0.8811(18) 0.743(3) 0.2312(13) 0.327(14) Uani 1 1 d DU . .
H42A H 0.8279 0.6770 0.1920 0.392 Uiso 1 1 calc R . .
H42B H 0.8334 0.7958 0.2330 0.392 Uiso 1 1 calc R . .
C43 C 0.917(3) 0.717(3) 0.3077(17) 0.320(15) Uani 1 1 d DU . .
H43A H 0.8836 0.7568 0.3438 0.383 Uiso 1 1 calc R . .
H43B H 0.8790 0.6388 0.3029 0.383 Uiso 1 1 calc R . .
C44 C 0.470(3) 0.7937(15) 0.2705(12) 0.308(14) Uani 1 1 d DU . .
H44A H 0.4126 0.8349 0.2521 0.369 Uiso 1 1 calc R . .
H44B H 0.5526 0.8441 0.3029 0.369 Uiso 1 1 calc R . .
C45 C 0.409(3) 0.712(3) 0.3109(18) 0.324(16) Uani 1 1 d DU . .
H45A H 0.4060 0.7466 0.3613 0.389 Uiso 1 1 calc R . .
H45B H 0.3223 0.6660 0.2804 0.389 Uiso 1 1 calc R . .
C46 C 0.500(2) 0.6513(13) 0.3163(10) 0.217(10) Uani 1 1 d DU . .
H46A H 0.4679 0.5830 0.3313 0.261 Uiso 1 1 calc R . .
H46B H 0.5842 0.6944 0.3510 0.261 Uiso 1 1 calc R . .
C47 C 0.5008(17) 0.6330(12) 0.2360(9) 0.161(6) Uani 1 1 d DU . .
H47A H 0.5830 0.6242 0.2311 0.194 Uiso 1 1 calc R . .
H47B H 0.4312 0.5673 0.2053 0.194 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 Br3 2.4092(12) . ?
Fe1 Br2 2.4274(11) . ?
Fe1 P1 2.441(2) . ?
Fe1 Br1 2.4428(13) . ?
N1 C19 1.347(8) . ?
N1 C20 1.378(10) . ?
N1 C22 1.430(9) . ?
N3 C19 1.325(9) . ?
N3 C21 1.377(9) . ?
N3 C31 1.449(8) . ?
O1 C43 1.393(15) . ?
O1 C40 1.446(15) . ?
O2 C44 1.379(15) . ?
O2 C47 1.390(12) . ?
P1 C1 1.844(10) . ?
P1 C7 1.845(10) . ?
P1 C13 1.856(7) . ?
C1 C6 1.491(13) . ?
C1 C2 1.510(12) . ?
C2 C3 1.572(11) . ?
C3 C4 1.447(12) . ?
C4 C5 1.449(12) . ?
C5 C6 1.566(11) . ?
C7 C12 1.493(14) . ?
C7 C8 1.516(12) . ?
C8 C9 1.567(11) . ?
C9 C10 1.413(13) . ?
C10 C11 1.478(12) . ?
C11 C12 1.561(11) . ?
C13 C14 1.501(10) . ?
C13 C18 1.524(10) . ?
C14 C15 1.561(11) . ?
C15 C16 1.500(12) . ?
C16 C17 1.460(11) . ?
C17 C18 1.555(10) . ?
C20 C21 1.363(11) . ?
C22 C23 1.376(10) . ?
C22 C27 1.391(9) . ?
C23 C24 1.360(11) . ?
C23 C28 1.502(10) . ?
C24 C25 1.414(10) . ?
C25 C26 1.369(11) . ?
C25 C29 1.516(11) . ?
C26 C27 1.383(11) . ?
C27 C30 1.498(10) . ?
C31 C32 1.387(10) . ?
C31 C36 1.392(10) . ?
C32 C33 1.396(10) . ?
C32 C37 1.474(10) . ?
C33 C34 1.395(10) . ?
C34 C35 1.374(10) . ?
C34 C38 1.497(10) . ?
C35 C36 1.394(10) . ?
C36 C39 1.511(11) . ?
C40 C41 1.518(15) . ?
C41 C42 1.510(14) . ?
C42 C43 1.516(15) . ?
C44 C45 1.522(17) . ?
C45 C46 1.454(16) . ?
C46 C47 1.481(14) . ?

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
Br3 Fe1 Br2 114.05(5) . . ?
Br3 Fe1 P1 102.89(6) . . ?
Br2 Fe1 P1 106.04(5) . . ?
Br3 Fe1 Br1 112.28(5) . . ?
Br2 Fe1 Br1 112.16(5) . . ?
P1 Fe1 Br1 108.65(6) . . ?
C19 N1 C20 107.5(6) . . ?
C19 N1 C22 125.2(6) . . ?
C20 N1 C22 127.3(6) . . ?
C19 N3 C21 109.0(6) . . ?
C19 N3 C31 124.7(6) . . ?
C21 N3 C31 126.2(7) . . ?
C43 O1 C40 110.4(11) . . ?
C44 O2 C47 109.3(12) . . ?
C1 P1 C7 103.9(6) . . ?
C1 P1 C13 107.2(5) . . ?
C7 P1 C13 107.9(4) . . ?
C1 P1 Fe1 110.3(4) . . ?
C7 P1 Fe1 116.8(5) . . ?
C13 P1 Fe1 110.2(2) . . ?
C6 C1 C2 109.1(10) . . ?
C6 C1 P1 120.8(7) . . ?
C2 C1 P1 112.6(7) . . ?
C1 C2 C3 108.9(9) . . ?
C4 C3 C2 112.0(9) . . ?
C3 C4 C5 110.7(10) . . ?
C4 C5 C6 112.6(9) . . ?
C1 C6 C5 108.3(9) . . ?
C12 C7 C8 105.1(11) . . ?
C12 C7 P1 113.3(8) . . ?
C8 C7 P1 110.6(7) . . ?
C7 C8 C9 110.3(9) . . ?
C10 C9 C8 112.4(10) . . ?
C9 C10 C11 113.9(11) . . ?
C10 C11 C12 109.2(9) . . ?
C7 C12 C11 114.7(10) . . ?
C14 C13 C18 112.1(6) . . ?
C14 C13 P1 117.5(5) . . ?
C18 C13 P1 110.9(5) . . ?
C13 C14 C15 109.3(8) . . ?
C16 C15 C14 108.7(8) . . ?
C17 C16 C15 110.2(8) . . ?
C16 C17 C18 110.9(7) . . ?
C13 C18 C17 108.7(8) . . ?
N3 C19 N1 109.1(7) . . ?
C21 C20 N1 107.8(6) . . ?
C20 C21 N3 106.5(7) . . ?
C23 C22 C27 123.1(7) . . ?
C23 C22 N1 119.8(6) . . ?
C27 C22 N1 117.1(6) . . ?
C24 C23 C22 118.1(6) . . ?
C24 C23 C28 119.3(7) . . ?
C22 C23 C28 122.5(7) . . ?
C23 C24 C25 122.2(7) . . ?
C26 C25 C24 116.6(7) . . ?
C26 C25 C29 123.1(7) . . ?
C24 C25 C29 120.2(7) . . ?
C25 C26 C27 123.9(7) . . ?
C26 C27 C22 116.1(7) . . ?
C26 C27 C30 121.5(6) . . ?
C22 C27 C30 122.4(7) . . ?
C32 C31 C36 123.4(6) . . ?
C32 C31 N3 118.7(6) . . ?
C36 C31 N3 117.8(6) . . ?
C31 C32 C33 116.0(7) . . ?
C31 C32 C37 123.1(6) . . ?
C33 C32 C37 120.9(7) . . ?
C34 C33 C32 123.4(7) . . ?
C35 C34 C33 117.3(7) . . ?
C35 C34 C38 123.0(7) . . ?
C33 C34 C38 119.5(7) . . ?
C34 C35 C36 122.6(7) . . ?
C31 C36 C35 117.2(7) . . ?
C31 C36 C39 122.2(7) . . ?
C35 C36 C39 120.5(7) . . ?
O1 C40 C41 107.5(10) . . ?
C42 C41 C40 106.5(9) . . ?
C41 C42 C43 104.9(10) . . ?
O1 C43 C42 110.2(10) . . ?
O2 C44 C45 98.7(16) . . ?
C46 C45 C44 99.0(17) . . ?
C45 C46 C47 97.3(16) . . ?
O2 C47 C46 106.2(12) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.106
