# 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_ok
_database_code_depnum_ccdc_archive 'CCDC 1495096'
_audit_update_record             
;
2016-07-21 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H36 Cl3 Fe2 N O4 P2 S2'
_chemical_formula_weight         890.77

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'
S S 0.1246 0.1234 '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           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   11.1740(5)
_cell_length_b                   11.2358(5)
_cell_length_c                   16.7264(8)
_cell_angle_alpha                71.493(2)
_cell_angle_beta                 72.711(2)
_cell_angle_gamma                84.664(2)
_cell_volume                     1901.40(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8862
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      27.88

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    1.208
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15320
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         27.89
_reflns_number_total             8882
_reflns_number_gt                7905
_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)+(0.1083P)²+5.6058P] 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         8882
_refine_ls_number_parameters     451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1806
_refine_ls_wR_factor_gt          0.1747
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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 0.99141(4) 0.35228(4) 0.26279(3) 0.01550(13) Uani 1 1 d . . .
Fe2 Fe 0.88283(5) 0.45608(5) 0.38170(3) 0.02043(14) Uani 1 1 d . . .
S2 S 0.81404(8) 0.28190(8) 0.36919(6) 0.02402(19) Uani 1 1 d . . .
S1 S 1.05606(8) 0.33434(8) 0.38167(5) 0.02223(19) Uani 1 1 d . . .
P2 P 1.15497(8) 0.46143(7) 0.16545(5) 0.01624(17) Uani 1 1 d . . .
P1 P 1.04601(8) 0.18515(8) 0.21901(5) 0.01637(18) Uani 1 1 d . . .
C7 C 1.1056(3) 0.2229(3) 0.0977(2) 0.0211(6) Uani 1 1 d . . .
H7A H 1.1230 0.1456 0.0822 0.025 Uiso 1 1 calc R . .
H7B H 1.0419 0.2683 0.0712 0.025 Uiso 1 1 calc R . .
C58 C 1.1675(3) 0.0750(3) 0.2523(2) 0.0200(6) Uani 1 1 d . . .
C57 C 1.1419(3) 0.6336(3) 0.1216(2) 0.0206(6) Uani 1 1 d . . .
O1 O 0.8475(3) 0.4554(3) 0.13721(19) 0.0337(6) Uani 1 1 d . . .
N1 N 1.2196(3) 0.2986(3) 0.06318(18) 0.0207(6) Uani 1 1 d . . .
O2 O 0.7487(3) 0.4167(4) 0.5686(2) 0.0477(8) Uani 1 1 d . . .
C19 C 1.3230(3) 0.5100(4) 0.2455(2) 0.0265(7) Uani 1 1 d . . .
H19A H 1.2565 0.5537 0.2720 0.032 Uiso 1 1 calc R . .
C18 C 0.9139(3) 0.0816(3) 0.2419(2) 0.0209(6) Uani 1 1 d . . .
C17 C 1.2467(3) 0.1067(3) 0.2929(2) 0.0245(7) Uani 1 1 d . . .
H17A H 1.2370 0.1833 0.3044 0.029 Uiso 1 1 calc R . .
C16 C 1.1854(3) -0.0397(3) 0.2343(3) 0.0267(7) Uani 1 1 d . . .
H16A H 1.1353 -0.0605 0.2051 0.032 Uiso 1 1 calc R . .
C15 C 1.0271(4) 0.6938(3) 0.1388(2) 0.0263(7) Uani 1 1 d . . .
H15A H 0.9560 0.6478 0.1762 0.032 Uiso 1 1 calc R . .
C1 C 0.9058(3) 0.4142(3) 0.1870(2) 0.0211(6) Uani 1 1 d . . .
C14 C 1.3067(3) 0.4486(3) 0.1884(2) 0.0195(6) Uani 1 1 d . . .
C4 C 0.9740(4) 0.5914(4) 0.3616(3) 0.0279(7) Uani 1 1 d . . .
C8 C 1.1932(3) 0.4301(3) 0.0580(2) 0.0209(6) Uani 1 1 d . . .
H8A H 1.1234 0.4573 0.0333 0.025 Uiso 1 1 calc R . .
H8B H 1.2656 0.4801 0.0182 0.025 Uiso 1 1 calc R . .
C9 C 1.2953(4) 0.2842(4) -0.0223(2) 0.0278(8) Uani 1 1 d . . .
H9A H 1.3513 0.3555 -0.0539 0.033 Uiso 1 1 calc R . .
H9B H 1.2401 0.2834 -0.0573 0.033 Uiso 1 1 calc R . .
C2 C 0.8024(4) 0.4330(4) 0.4968(3) 0.0294(8) Uani 1 1 d . . .
C61 C 1.2769(4) -0.1228(4) 0.2594(3) 0.0332(9) Uani 1 1 d . . .
H61A H 1.2864 -0.1997 0.2483 0.040 Uiso 1 1 calc R . .
C60 C 1.4384(4) 0.5061(4) 0.2630(3) 0.0350(9) Uani 1 1 d . . .
H60A H 1.4486 0.5481 0.3004 0.042 Uiso 1 1 calc R . .
O3 O 0.6987(3) 0.6070(3) 0.2982(2) 0.0419(7) Uani 1 1 d . . .
O4 O 1.0307(3) 0.6771(3) 0.3498(3) 0.0436(8) Uani 1 1 d . . .
C32 C 0.8247(4) 0.1197(4) 0.1950(3) 0.0305(8) Uani 1 1 d . . .
H32A H 0.8345 0.1963 0.1507 0.037 Uiso 1 1 calc R . .
C31 C 1.4070(3) 0.3808(4) 0.1508(3) 0.0276(7) Uani 1 1 d . . .
H31A H 1.3970 0.3380 0.1138 0.033 Uiso 1 1 calc R . .
C30 C 1.2484(4) 0.7050(3) 0.0658(3) 0.0287(8) Uani 1 1 d . . .
H30A H 1.3261 0.6662 0.0543 0.034 Uiso 1 1 calc R . .
C29 C 0.8948(3) -0.0331(4) 0.3087(3) 0.0277(7) Uani 1 1 d . . .
H29A H 0.9512 -0.0592 0.3421 0.033 Uiso 1 1 calc R . .
C3 C 0.7703(4) 0.5476(4) 0.3313(3) 0.0271(7) Uani 1 1 d . . .
C10 C 1.3722(4) 0.1635(4) -0.0107(3) 0.0370(9) Uani 1 1 d . . .
H10A H 1.4297 0.1656 0.0224 0.044 Uiso 1 1 calc R . .
H10B H 1.3165 0.0923 0.0227 0.044 Uiso 1 1 calc R . .
C27 C 1.3544(4) -0.0917(4) 0.3011(3) 0.0347(9) Uani 1 1 d . . .
H27A H 1.4152 -0.1478 0.3185 0.042 Uiso 1 1 calc R . .
C26 C 1.3403(4) 0.0242(4) 0.3166(3) 0.0335(9) Uani 1 1 d . . .
H26A H 1.3936 0.0467 0.3429 0.040 Uiso 1 1 calc R . .
C25 C 1.5219(4) 0.3772(4) 0.1687(3) 0.0346(9) Uani 1 1 d . . .
H25A H 1.5885 0.3327 0.1430 0.042 Uiso 1 1 calc R . .
C24 C 1.2382(4) 0.8334(4) 0.0276(3) 0.0349(9) Uani 1 1 d . . .
H24A H 1.3089 0.8803 -0.0093 0.042 Uiso 1 1 calc R . .
C5 C 0.9885(4) 0.1857(4) 0.4622(3) 0.0347(9) Uani 1 1 d . . .
H5A H 1.0455 0.1177 0.4527 0.042 Uiso 1 1 calc R . .
H5B H 0.9794 0.1890 0.5210 0.042 Uiso 1 1 calc R . .
C23 C 1.0179(4) 0.8240(4) 0.0999(3) 0.0328(8) Uani 1 1 d . . .
H23A H 0.9408 0.8639 0.1119 0.039 Uiso 1 1 calc R . .
C6 C 0.8617(4) 0.1587(4) 0.4557(3) 0.0345(9) Uani 1 1 d . . .
H6A H 0.7993 0.1512 0.5117 0.041 Uiso 1 1 calc R . .
H6B H 0.8653 0.0792 0.4438 0.041 Uiso 1 1 calc R . .
C22 C 0.7926(4) -0.1088(4) 0.3261(3) 0.0378(10) Uani 1 1 d . . .
H22A H 0.7822 -0.1858 0.3699 0.045 Uiso 1 1 calc R . .
C21 C 1.5372(4) 0.4400(5) 0.2247(3) 0.0370(9) Uani 1 1 d . . .
H21A H 1.6139 0.4373 0.2364 0.044 Uiso 1 1 calc R . .
C20 C 1.1222(5) 0.8919(4) 0.0446(3) 0.0342(9) Uani 1 1 d . . .
H20A H 1.1155 0.9776 0.0181 0.041 Uiso 1 1 calc R . .
C33 C 0.7220(4) 0.0446(5) 0.2137(3) 0.0419(10) Uani 1 1 d . . .
H33A H 0.6633 0.0716 0.1823 0.050 Uiso 1 1 calc R . .
C34 C 0.7065(4) -0.0697(4) 0.2784(4) 0.0425(11) Uani 1 1 d . . .
H34A H 0.6384 -0.1204 0.2898 0.051 Uiso 1 1 calc R . .
Cl2 Cl 0.51768(19) 0.6641(2) 0.48739(15) 0.0865(6) Uani 1 1 d . . .
Cl1 Cl 0.6684(4) 0.7572(4) 0.5554(2) 0.1492(13) Uani 1 1 d . . .
Cl3 Cl 0.5021(7) 0.9161(4) 0.5106(4) 0.217(3) Uani 1 1 d . . .
C11 C 1.4459(6) 0.1469(5) -0.0986(4) 0.0553(14) Uani 1 1 d . . .
H11A H 1.4931 0.0703 -0.0891 0.083 Uiso 1 1 calc R . .
H11B H 1.5022 0.2165 -0.1314 0.083 Uiso 1 1 calc R . .
H11C H 1.3891 0.1433 -0.1311 0.083 Uiso 1 1 calc R . .
C41 C 0.5276(8) 0.7624(9) 0.5471(8) 0.094(3) Uani 1 1 d . . .
H41A H 0.4707 0.7299 0.6065 0.113 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 C1 1.744(3) . ?
Fe1 P1 2.1976(9) . ?
Fe1 P2 2.2081(9) . ?
Fe1 S2 2.2410(9) . ?
Fe1 S1 2.2558(9) . ?
Fe1 Fe2 2.5618(7) . ?
Fe2 C3 1.785(4) . ?
Fe2 C4 1.794(4) . ?
Fe2 C2 1.811(4) . ?
Fe2 S2 2.2582(10) . ?
Fe2 S1 2.2639(10) . ?
S2 C6 1.829(4) . ?
S1 C5 1.838(4) . ?
P2 C14 1.830(3) . ?
P2 C57 1.847(3) . ?
P2 C8 1.858(3) . ?
P1 C18 1.839(3) . ?
P1 C58 1.839(3) . ?
P1 C7 1.855(3) . ?
C7 N1 1.460(4) . ?
C58 C17 1.394(5) . ?
C58 C16 1.398(5) . ?
C57 C15 1.389(5) . ?
C57 C30 1.405(5) . ?
O1 C1 1.164(4) . ?
N1 C8 1.460(4) . ?
N1 C9 1.480(4) . ?
O2 C2 1.135(5) . ?
C19 C60 1.398(5) . ?
C19 C14 1.402(5) . ?
C18 C29 1.396(5) . ?
C18 C32 1.402(5) . ?
C17 C26 1.394(5) . ?
C16 C61 1.387(5) . ?
C15 C23 1.408(5) . ?
C14 C31 1.400(5) . ?
C4 O4 1.135(5) . ?
C9 C10 1.527(6) . ?
C61 C27 1.389(6) . ?
C60 C21 1.382(6) . ?
O3 C3 1.151(5) . ?
C32 C33 1.388(5) . ?
C31 C25 1.396(5) . ?
C30 C24 1.389(5) . ?
C29 C22 1.393(5) . ?
C10 C11 1.517(6) . ?
C27 C26 1.394(6) . ?
C25 C21 1.395(6) . ?
C24 C20 1.390(7) . ?
C5 C6 1.518(7) . ?
C23 C20 1.369(7) . ?
C22 C34 1.382(7) . ?
C33 C34 1.377(7) . ?
Cl2 C41 1.738(10) . ?
Cl1 C41 1.614(9) . ?
Cl3 C41 1.667(10) . ?
Cl3 Cl3 1.803(9) 2_676 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 P1 92.74(12) . . ?
C1 Fe1 P2 88.52(11) . . ?
P1 Fe1 P2 92.98(3) . . ?
C1 Fe1 S2 90.24(11) . . ?
P1 Fe1 S2 99.93(4) . . ?
P2 Fe1 S2 167.07(4) . . ?
C1 Fe1 S1 156.34(12) . . ?
P1 Fe1 S1 110.17(4) . . ?
P2 Fe1 S1 95.85(4) . . ?
S2 Fe1 S1 80.34(4) . . ?
C1 Fe1 Fe2 101.22(11) . . ?
P1 Fe1 Fe2 151.35(3) . . ?
P2 Fe1 Fe2 112.08(3) . . ?
S2 Fe1 Fe2 55.61(3) . . ?
S1 Fe1 Fe2 55.62(3) . . ?
C3 Fe2 C4 92.85(17) . . ?
C3 Fe2 C2 100.89(18) . . ?
C4 Fe2 C2 98.52(18) . . ?
C3 Fe2 S2 89.85(12) . . ?
C4 Fe2 S2 162.23(13) . . ?
C2 Fe2 S2 98.20(13) . . ?
C3 Fe2 S1 153.40(13) . . ?
C4 Fe2 S1 90.16(12) . . ?
C2 Fe2 S1 104.79(13) . . ?
S2 Fe2 S1 79.80(4) . . ?
C3 Fe2 Fe1 98.74(12) . . ?
C4 Fe2 Fe1 107.26(13) . . ?
C2 Fe2 Fe1 146.57(13) . . ?
S2 Fe2 Fe1 54.98(3) . . ?
S1 Fe2 Fe1 55.32(2) . . ?
C6 S2 Fe1 105.81(15) . . ?
C6 S2 Fe2 101.59(14) . . ?
Fe1 S2 Fe2 69.41(3) . . ?
C5 S1 Fe1 105.02(14) . . ?
C5 S1 Fe2 101.21(15) . . ?
Fe1 S1 Fe2 69.06(3) . . ?
C14 P2 C57 100.51(15) . . ?
C14 P2 C8 103.51(16) . . ?
C57 P2 C8 96.36(15) . . ?
C14 P2 Fe1 120.94(11) . . ?
C57 P2 Fe1 119.35(12) . . ?
C8 P2 Fe1 112.40(11) . . ?
C18 P1 C58 103.23(15) . . ?
C18 P1 C7 100.42(15) . . ?
C58 P1 C7 100.27(16) . . ?
C18 P1 Fe1 113.76(11) . . ?
C58 P1 Fe1 122.95(11) . . ?
C7 P1 Fe1 113.13(12) . . ?
N1 C7 P1 111.1(2) . . ?
C17 C58 C16 118.7(3) . . ?
C17 C58 P1 120.5(3) . . ?
C16 C58 P1 120.8(3) . . ?
C15 C57 C30 118.9(3) . . ?
C15 C57 P2 121.2(3) . . ?
C30 C57 P2 119.8(3) . . ?
C8 N1 C7 112.2(3) . . ?
C8 N1 C9 112.0(3) . . ?
C7 N1 C9 110.9(3) . . ?
C60 C19 C14 120.7(4) . . ?
C29 C18 C32 117.9(3) . . ?
C29 C18 P1 121.9(3) . . ?
C32 C18 P1 120.1(3) . . ?
C58 C17 C26 120.5(4) . . ?
C61 C16 C58 120.8(4) . . ?
C57 C15 C23 120.3(4) . . ?
O1 C1 Fe1 179.2(3) . . ?
C31 C14 C19 118.9(3) . . ?
C31 C14 P2 122.6(3) . . ?
C19 C14 P2 118.5(3) . . ?
O4 C4 Fe2 179.1(4) . . ?
N1 C8 P2 114.1(2) . . ?
N1 C9 C10 111.8(3) . . ?
O2 C2 Fe2 177.7(4) . . ?
C16 C61 C27 120.2(4) . . ?
C21 C60 C19 119.9(4) . . ?
C33 C32 C18 120.8(4) . . ?
C14 C31 C25 120.1(4) . . ?
C24 C30 C57 120.3(4) . . ?
C22 C29 C18 120.9(4) . . ?
O3 C3 Fe2 179.4(4) . . ?
C11 C10 C9 111.5(4) . . ?
C61 C27 C26 119.5(4) . . ?
C27 C26 C17 120.2(4) . . ?
C21 C25 C31 120.3(4) . . ?
C30 C24 C20 120.1(4) . . ?
C6 C5 S1 112.3(3) . . ?
C20 C23 C15 120.0(4) . . ?
C5 C6 S2 112.0(3) . . ?
C34 C22 C29 120.2(4) . . ?
C60 C21 C25 120.1(4) . . ?
C23 C20 C24 120.3(4) . . ?
C34 C33 C32 120.5(4) . . ?
C33 C34 C22 119.7(4) . . ?
C41 Cl3 Cl3 165.3(7) . 2_676 ?
Cl1 C41 Cl3 102.6(6) . . ?
Cl1 C41 Cl2 108.9(5) . . ?
Cl3 C41 Cl2 120.8(7) . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        27.89
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         1.177
_refine_diff_density_min         -2.262
_refine_diff_density_rms         0.145
####################################################################### 
# 
# 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_ok
_database_code_depnum_ccdc_archive 'CCDC 1495097'
_audit_update_record             
;
2016-07-21 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H39 Cl2 Fe2 N O4 P2 S2'
_chemical_formula_weight         918.39

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

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

_cell_length_a                   17.3996(3)
_cell_length_b                   13.0180(2)
_cell_length_c                   20.6028(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.5930(10)
_cell_angle_gamma                90.00
_cell_volume                     4276.62(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9171
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      27.24

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29983
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         27.52
_reflns_number_total             9832
_reflns_number_gt                7575
_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)+(0.0664P)²+4.7940P] 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         9832
_refine_ls_number_parameters     487
_refine_ls_number_restraints     165
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1383
_refine_ls_wR_factor_gt          0.1261
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.011
_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 0.45805(2) 0.12289(3) 0.170535(19) 0.02936(11) Uani 1 1 d U . .
Fe2 Fe 0.43137(3) 0.31169(3) 0.18556(2) 0.04505(13) Uani 1 1 d U . .
P1 P 0.49734(4) -0.03227(6) 0.21400(4) 0.02954(15) Uani 1 1 d U . .
P2 P 0.36230(4) 0.06251(6) 0.07066(4) 0.03020(16) Uani 1 1 d U . .
S2 S 0.36471(5) 0.17997(6) 0.21392(4) 0.04369(19) Uani 1 1 d U . .
S1 S 0.54479(6) 0.22131(7) 0.26080(5) 0.0540(2) Uani 1 1 d U . .
N1 N 0.41967(15) -0.14192(19) 0.09120(13) 0.0384(6) Uani 1 1 d U . .
C66 C 0.25876(17) 0.0310(2) 0.06823(14) 0.0356(6) Uani 1 1 d U . .
C65 C 0.44007(18) -0.1096(2) 0.25419(15) 0.0357(6) Uani 1 1 d U . .
C7 C 0.50305(18) -0.1241(2) 0.14723(15) 0.0380(6) Uani 1 1 d U . .
H7A H 0.5401 -0.0970 0.1265 0.046 Uiso 1 1 calc R . .
H7B H 0.5262 -0.1888 0.1701 0.046 Uiso 1 1 calc R . .
C63 C 0.4722(2) -0.2030(3) 0.2858(2) 0.0517(8) Uani 1 1 d U . .
H63A H 0.5244 -0.2242 0.2884 0.062 Uiso 1 1 calc R . .
O1 O 0.58176(16) 0.1321(2) 0.10922(15) 0.0680(8) Uani 1 1 d U . .
C62 C 0.60513(17) -0.0383(2) 0.28173(15) 0.0369(6) Uani 1 1 d U . .
C61 C 0.33399(18) 0.1360(2) -0.01187(15) 0.0372(6) Uani 1 1 d U . .
C8 C 0.39450(19) -0.0578(2) 0.04005(15) 0.0389(6) Uani 1 1 d U . .
H8A H 0.3482 -0.0812 -0.0023 0.047 Uiso 1 1 calc R . .
H8B H 0.4409 -0.0422 0.0270 0.047 Uiso 1 1 calc R . .
C59 C 0.2411(2) -0.0662(3) 0.08536(19) 0.0501(8) Uani 1 1 d U . .
H59A H 0.2816 -0.1175 0.0965 0.060 Uiso 1 1 calc R . .
C58 C 0.3772(2) 0.2232(3) -0.01557(18) 0.0461(7) Uani 1 1 d U . .
H58A H 0.4227 0.2455 0.0243 0.055 Uiso 1 1 calc R . .
C1 C 0.53086(18) 0.1275(3) 0.13199(16) 0.0407(7) Uani 1 1 d U . .
C9 C 0.4165(2) -0.2404(3) 0.05443(19) 0.0573(9) Uani 1 1 d U . .
H9A H 0.4650 -0.2446 0.0425 0.069 Uiso 1 1 calc R . .
H9B H 0.3669 -0.2408 0.0104 0.069 Uiso 1 1 calc R . .
C55 C 0.1966(2) 0.1060(3) 0.05106(19) 0.0474(8) Uani 1 1 d U . .
H55A H 0.2073 0.1721 0.0396 0.057 Uiso 1 1 calc R . .
C54 C 0.67344(19) -0.0456(3) 0.26345(19) 0.0520(9) Uani 1 1 d U . .
H54A H 0.6649 -0.0482 0.2159 0.062 Uiso 1 1 calc R . .
C53 C 0.3623(2) -0.0794(3) 0.25153(18) 0.0478(8) Uani 1 1 d U . .
H53A H 0.3398 -0.0165 0.2316 0.057 Uiso 1 1 calc R . .
C3 C 0.3369(3) 0.3464(3) 0.1133(2) 0.0535(8) Uani 1 1 d U . .
C51 C 0.6199(2) -0.0320(3) 0.35303(17) 0.0508(8) Uani 1 1 d U . .
H51A H 0.5749 -0.0274 0.3664 0.061 Uiso 1 1 calc R . .
O3 O 0.2763(2) 0.3707(3) 0.06762(18) 0.0826(9) Uani 1 1 d U . .
C32 C 0.2670(2) 0.1035(3) -0.07319(16) 0.0493(8) Uani 1 1 d U . .
H32A H 0.2376 0.0444 -0.0720 0.059 Uiso 1 1 calc R . .
C31 C 0.1626(2) -0.0877(3) 0.0860(2) 0.0657(11) Uani 1 1 d U . .
H31A H 0.1514 -0.1531 0.0981 0.079 Uiso 1 1 calc R . .
C30 C 0.7017(3) -0.0327(3) 0.4048(2) 0.0668(11) Uani 1 1 d U . .
H30A H 0.7112 -0.0264 0.4524 0.080 Uiso 1 1 calc R . .
C29 C 0.1024(2) -0.0132(4) 0.0688(2) 0.0604(10) Uani 1 1 d U . .
H29A H 0.0503 -0.0280 0.0694 0.073 Uiso 1 1 calc R . .
C28 C 0.7547(2) -0.0491(4) 0.3155(2) 0.0681(11) Uani 1 1 d U . .
H28A H 0.8000 -0.0556 0.3027 0.082 Uiso 1 1 calc R . .
C6 C 0.4275(3) 0.1749(3) 0.30873(19) 0.0614(10) Uani 1 1 d U . .
C26 C 0.2444(3) 0.1584(3) -0.13537(19) 0.0623(10) Uani 1 1 d U . .
H26A H 0.2003 0.1354 -0.1760 0.075 Uiso 1 1 calc R . .
C5 C 0.5122(3) 0.1952(3) 0.32966(19) 0.0631(10) Uani 1 1 d U . .
C24 C 0.3529(3) 0.2781(3) -0.0788(2) 0.0618(10) Uani 1 1 d U . .
H24A H 0.3823 0.3368 -0.0809 0.074 Uiso 1 1 calc R . .
C23 C 0.1187(2) 0.0825(3) 0.0510(2) 0.0572(9) Uani 1 1 d U . .
H23A H 0.0772 0.1327 0.0386 0.069 Uiso 1 1 calc R . .
C22 C 0.2862(3) 0.2462(4) -0.1377(2) 0.0667(11) Uani 1 1 d U . .
H22A H 0.2692 0.2842 -0.1793 0.080 Uiso 1 1 calc R . .
C21 C 0.4287(3) -0.2653(3) 0.3135(2) 0.0678(11) Uani 1 1 d U . .
H21A H 0.4518 -0.3273 0.3350 0.081 Uiso 1 1 calc R . .
C2 C 0.4311(4) 0.4116(3) 0.2461(2) 0.0786(13) Uani 1 1 d U . .
C19 C 0.7679(2) -0.0429(4) 0.3851(2) 0.0692(11) Uani 1 1 d U . .
H19A H 0.8223 -0.0455 0.4197 0.083 Uiso 1 1 calc R . .
C68 C 0.3181(2) -0.1429(4) 0.2786(2) 0.0701(12) Uani 1 1 d U . .
H68A H 0.2656 -0.1226 0.2759 0.084 Uiso 1 1 calc R . .
C67 C 0.3510(3) -0.2351(4) 0.3093(3) 0.0759(13) Uani 1 1 d U . .
H67A H 0.3209 -0.2772 0.3272 0.091 Uiso 1 1 calc R . .
O4 O 0.5321(2) 0.4033(3) 0.1168(2) 0.0998(12) Uani 1 1 d U . .
C14 C 0.4527(5) 0.1464(4) 0.4315(3) 0.0907(17) Uani 1 1 d U . .
C4 C 0.4933(3) 0.3671(3) 0.1443(2) 0.0621(10) Uani 1 1 d U . .
O2 O 0.4326(4) 0.4743(3) 0.2844(2) 0.1394(19) Uani 1 1 d U . .
C12 C 0.5659(4) 0.1927(3) 0.4012(2) 0.0864(15) Uani 1 1 d U . .
H12A H 0.6225 0.2082 0.4155 0.104 Uiso 1 1 calc R . .
C13 C 0.5348(5) 0.1674(4) 0.4497(3) 0.1037(18) Uani 1 1 d U . .
H13A H 0.5712 0.1644 0.4972 0.124 Uiso 1 1 calc R . .
C10 C 0.4149(3) -0.3347(3) 0.0969(3) 0.0840(15) Uani 1 1 d U . .
H10A H 0.4178 -0.3953 0.0706 0.101 Uiso 1 1 calc R . .
H10B H 0.4646 -0.3342 0.1409 0.101 Uiso 1 1 calc R . .
C11 C 0.3388(4) -0.3429(4) 0.1140(3) 0.1047(19) Uani 1 1 d U . .
H11A H 0.3426 -0.4040 0.1411 0.157 Uiso 1 1 calc R . .
H11B H 0.2893 -0.3459 0.0708 0.157 Uiso 1 1 calc R . .
H11C H 0.3359 -0.2839 0.1409 0.157 Uiso 1 1 calc R . .
C15 C 0.3941(4) 0.1496(3) 0.3573(2) 0.0822(14) Uani 1 1 d U . .
H15A H 0.3373 0.1354 0.3435 0.099 Uiso 1 1 calc R . .
C16 C 0.4258(6) 0.1233(6) 0.4885(4) 0.159(4) Uani 1 1 d U . .
H16A H 0.4734 0.1254 0.5331 0.238 Uiso 1 1 calc R . .
H16B H 0.4011 0.0561 0.4814 0.238 Uiso 1 1 calc R . .
H16C H 0.3852 0.1733 0.4885 0.238 Uiso 1 1 calc R . .
C90 C 0.2007(3) -0.1771(6) -0.1573(4) 0.123(2) Uani 1 1 d U . .
H90A H 0.2006 -0.2486 -0.1706 0.148 Uiso 1 1 calc R . .
H90B H 0.2574 -0.1513 -0.1431 0.148 Uiso 1 1 calc R . .
Cl1 Cl 0.17295(11) -0.16980(14) -0.08678(8) 0.1168(6) Uani 1 1 d U . .
Cl2 Cl 0.13372(13) -0.10747(16) -0.23099(10) 0.1297(7) Uani 1 1 d U . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 1.745(3) . ?
Fe1 P1 2.2043(8) . ?
Fe1 P2 2.2098(8) . ?
Fe1 S1 2.2651(9) . ?
Fe1 S2 2.2695(8) . ?
Fe1 Fe2 2.5429(6) . ?
Fe2 C3 1.779(4) . ?
Fe2 C4 1.771(4) . ?
Fe2 C2 1.804(4) . ?
Fe2 S2 2.2737(10) . ?
Fe2 S1 2.2875(10) . ?
P1 C65 1.831(3) . ?
P1 C62 1.837(3) . ?
P1 C7 1.855(3) . ?
P2 C66 1.829(3) . ?
P2 C61 1.838(3) . ?
P2 C8 1.857(3) . ?
S2 C6 1.818(4) . ?
S1 C5 1.759(4) . ?
N1 C8 1.460(4) . ?
N1 C7 1.466(4) . ?
N1 C9 1.479(4) . ?
C66 C59 1.381(5) . ?
C66 C55 1.394(4) . ?
C65 C63 1.387(4) . ?
C65 C53 1.388(4) . ?
C63 C21 1.379(5) . ?
O1 C1 1.158(4) . ?
C62 C51 1.389(4) . ?
C62 C54 1.386(4) . ?
C61 C58 1.380(5) . ?
C61 C32 1.398(4) . ?
C59 C31 1.400(5) . ?
C58 C24 1.395(5) . ?
C9 C10 1.514(6) . ?
C55 C23 1.389(5) . ?
C54 C28 1.392(5) . ?
C53 C68 1.390(5) . ?
C3 O3 1.141(5) . ?
C51 C30 1.396(5) . ?
C32 C26 1.379(5) . ?
C31 C29 1.367(6) . ?
C30 C19 1.372(6) . ?
C29 C23 1.361(6) . ?
C28 C19 1.363(6) . ?
C6 C5 1.385(6) . ?
C6 C15 1.385(5) . ?
C26 C22 1.366(6) . ?
C5 C12 1.395(6) . ?
C24 C22 1.365(6) . ?
C21 C67 1.378(6) . ?
C2 O2 1.127(5) . ?
C68 C67 1.371(6) . ?
O4 C4 1.143(5) . ?
C14 C13 1.352(9) . ?
C14 C16 1.458(7) . ?
C14 C15 1.459(8) . ?
C12 C13 1.353(8) . ?
C10 C11 1.504(8) . ?
C90 Cl1 1.707(7) . ?
C90 Cl2 1.753(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
C1 Fe1 P1 93.02(11) . . ?
C1 Fe1 P2 90.15(10) . . ?
P1 Fe1 P2 92.75(3) . . ?
C1 Fe1 S1 89.29(11) . . ?
P1 Fe1 S1 100.86(3) . . ?
P2 Fe1 S1 166.39(4) . . ?
C1 Fe1 S2 158.81(11) . . ?
P1 Fe1 S2 107.12(3) . . ?
P2 Fe1 S2 95.25(3) . . ?
S1 Fe1 S2 80.69(4) . . ?
C1 Fe1 Fe2 102.91(11) . . ?
P1 Fe1 Fe2 151.42(3) . . ?
P2 Fe1 Fe2 110.54(3) . . ?
S1 Fe1 Fe2 56.46(3) . . ?
S2 Fe1 Fe2 56.04(3) . . ?
C3 Fe2 C4 91.75(18) . . ?
C3 Fe2 C2 98.0(2) . . ?
C4 Fe2 C2 102.1(2) . . ?
C3 Fe2 S2 90.63(12) . . ?
C4 Fe2 S2 154.33(14) . . ?
C2 Fe2 S2 102.91(16) . . ?
C3 Fe2 S1 162.82(12) . . ?
C4 Fe2 S1 90.54(14) . . ?
C2 Fe2 S1 98.17(17) . . ?
S2 Fe2 S1 80.12(4) . . ?
C3 Fe2 Fe1 107.22(12) . . ?
C4 Fe2 Fe1 99.17(14) . . ?
C2 Fe2 Fe1 146.33(15) . . ?
S2 Fe2 Fe1 55.89(2) . . ?
S1 Fe2 Fe1 55.63(2) . . ?
C65 P1 C62 102.00(13) . . ?
C65 P1 C7 100.45(14) . . ?
C62 P1 C7 101.19(13) . . ?
C65 P1 Fe1 123.44(10) . . ?
C62 P1 Fe1 113.83(10) . . ?
C7 P1 Fe1 112.91(10) . . ?
C66 P2 C61 101.25(13) . . ?
C66 P2 C8 103.26(14) . . ?
C61 P2 C8 97.50(13) . . ?
C66 P2 Fe1 118.21(9) . . ?
C61 P2 Fe1 119.94(10) . . ?
C8 P2 Fe1 113.50(10) . . ?
C6 S2 Fe1 101.18(14) . . ?
C6 S2 Fe2 98.87(15) . . ?
Fe1 S2 Fe2 68.07(3) . . ?
C5 S1 Fe1 103.24(15) . . ?
C5 S1 Fe2 100.17(15) . . ?
Fe1 S1 Fe2 67.91(3) . . ?
C8 N1 C7 111.5(2) . . ?
C8 N1 C9 110.0(2) . . ?
C7 N1 C9 111.2(2) . . ?
C59 C66 C55 118.5(3) . . ?
C59 C66 P2 121.1(2) . . ?
C55 C66 P2 120.4(2) . . ?
C63 C65 C53 118.0(3) . . ?
C63 C65 P1 120.3(2) . . ?
C53 C65 P1 121.6(2) . . ?
N1 C7 P1 110.83(19) . . ?
C21 C63 C65 121.7(3) . . ?
C51 C62 C54 118.4(3) . . ?
C51 C62 P1 120.1(2) . . ?
C54 C62 P1 121.5(2) . . ?
C58 C61 C32 118.3(3) . . ?
C58 C61 P2 121.9(2) . . ?
C32 C61 P2 119.7(2) . . ?
N1 C8 P2 115.6(2) . . ?
C66 C59 C31 120.2(3) . . ?
C61 C58 C24 120.3(3) . . ?
O1 C1 Fe1 177.0(3) . . ?
N1 C9 C10 114.4(3) . . ?
C66 C55 C23 120.3(3) . . ?
C62 C54 C28 120.7(3) . . ?
C65 C53 C68 120.2(3) . . ?
O3 C3 Fe2 178.5(4) . . ?
C62 C51 C30 120.5(3) . . ?
C26 C32 C61 120.5(4) . . ?
C29 C31 C59 120.4(4) . . ?
C19 C30 C51 119.7(4) . . ?
C23 C29 C31 119.9(3) . . ?
C19 C28 C54 120.0(4) . . ?
C5 C6 C15 121.5(4) . . ?
C5 C6 S2 115.8(3) . . ?
C15 C6 S2 122.7(4) . . ?
C22 C26 C32 120.5(4) . . ?
C6 C5 C12 120.2(4) . . ?
C6 C5 S1 115.6(3) . . ?
C12 C5 S1 124.2(4) . . ?
C22 C24 C58 120.4(4) . . ?
C29 C23 C55 120.7(3) . . ?
C26 C22 C24 119.9(3) . . ?
C63 C21 C67 119.5(4) . . ?
O2 C2 Fe2 178.7(6) . . ?
C28 C19 C30 120.6(3) . . ?
C67 C68 C53 120.6(4) . . ?
C68 C67 C21 119.9(4) . . ?
C13 C14 C16 117.5(6) . . ?
C13 C14 C15 120.2(5) . . ?
C16 C14 C15 122.2(7) . . ?
O4 C4 Fe2 178.9(4) . . ?
C13 C12 C5 119.3(6) . . ?
C12 C13 C14 122.3(5) . . ?
C11 C10 C9 114.5(4) . . ?
C6 C15 C14 116.3(5) . . ?
Cl1 C90 Cl2 113.1(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.119
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.071
####################################################################### 
# 
# 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_b
_database_code_depnum_ccdc_archive 'CCDC 1495098'
_audit_update_record             
;
2016-07-21 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H37 Fe N O P2 S2'
_chemical_formula_weight         693.59

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/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                   9.7553(17)
_cell_length_b                   16.584(3)
_cell_length_c                   21.460(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.659(4)
_cell_angle_gamma                90.00
_cell_volume                     3432.3(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    1580
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      20.32

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_absorpt_coefficient_mu    0.685
_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       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23573
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_av_sigmaI/netI    0.1099
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         27.50
_reflns_number_total             7851
_reflns_number_gt                3617
_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)+(0.0737P)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         7851
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_ref         0.1647
_refine_ls_wR_factor_gt          0.1274
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_restrained_S_all      0.904
_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 0.74668(5) 0.30796(3) 0.77333(3) 0.03980(18) Uani 1 1 d . . .
P1 P 0.59392(10) 0.30318(7) 0.68568(5) 0.0426(3) Uani 1 1 d . . .
S2 S 0.86311(11) 0.30045(7) 0.86915(5) 0.0488(3) Uani 1 1 d . . .
P2 P 0.64560(10) 0.42040(7) 0.79960(5) 0.0427(3) Uani 1 1 d . . .
S1 S 0.78340(11) 0.17937(7) 0.76086(5) 0.0507(3) Uani 1 1 d . . .
N1 N 0.5050(3) 0.4610(2) 0.68202(16) 0.0515(9) Uani 1 1 d . . .
C22 C 1.0268(4) 0.1802(3) 0.9293(2) 0.0586(12) Uani 1 1 d . . .
H22A H 1.0539 0.2172 0.9614 0.070 Uiso 1 1 calc R . .
C6 C 0.9339(4) 0.2044(3) 0.8760(2) 0.0464(11) Uani 1 1 d . . .
C21 C 0.4836(4) 0.4040(3) 0.8296(2) 0.0486(11) Uani 1 1 d . . .
O1 O 0.9473(3) 0.3914(2) 0.71316(16) 0.0704(10) Uani 1 1 d . . .
C20 C 0.5820(5) 0.1705(3) 0.6037(2) 0.0733(15) Uani 1 1 d . . .
H20A H 0.5115 0.1508 0.6242 0.088 Uiso 1 1 calc R . .
C1 C 0.8630(4) 0.3581(3) 0.7372(2) 0.0461(11) Uani 1 1 d . . .
C19 C 0.6018(4) 0.4930(2) 0.73500(19) 0.0506(11) Uani 1 1 d . . .
H19A H 0.5614 0.5406 0.7512 0.061 Uiso 1 1 calc R . .
H19B H 0.6864 0.5094 0.7199 0.061 Uiso 1 1 calc R . .
C18 C 0.6433(4) 0.2429(3) 0.62186(19) 0.0446(10) Uani 1 1 d . . .
C17 C 0.5663(4) 0.4012(3) 0.6455(2) 0.0526(12) Uani 1 1 d . . .
H17A H 0.6547 0.4212 0.6365 0.063 Uiso 1 1 calc R . .
H17B H 0.5064 0.3935 0.6056 0.063 Uiso 1 1 calc R . .
C16 C 0.4195(4) 0.2697(3) 0.6931(2) 0.0505(11) Uani 1 1 d . . .
C15 C 0.7454(4) 0.4847(2) 0.8584(2) 0.0448(10) Uani 1 1 d . . .
C14 C 0.9508(5) 0.0708(3) 0.8330(2) 0.0663(14) Uani 1 1 d . . .
H14A H 0.9274 0.0338 0.8007 0.080 Uiso 1 1 calc R . .
C5 C 0.8954(4) 0.1488(3) 0.8272(2) 0.0492(11) Uani 1 1 d . . .
C13 C 1.0396(6) 0.0485(3) 0.8862(2) 0.0755(15) Uani 1 1 d . . .
H13A H 1.0739 -0.0039 0.8894 0.091 Uiso 1 1 calc R . .
C12 C 0.4802(5) 0.3462(3) 0.8757(2) 0.0649(14) Uani 1 1 d . . .
H12A H 0.5604 0.3177 0.8907 0.078 Uiso 1 1 calc R . .
C11 C 0.6915(5) 0.5130(3) 0.9105(2) 0.0589(12) Uani 1 1 d . . .
H11A H 0.6011 0.5000 0.9155 0.071 Uiso 1 1 calc R . .
C1O C 0.7519(5) 0.2687(3) 0.5912(2) 0.0593(13) Uani 1 1 d . . .
H1OA H 0.7982 0.3164 0.6037 0.071 Uiso 1 1 calc R . .
C42 C 0.7915(5) 0.2241(3) 0.5424(2) 0.0661(14) Uani 1 1 d . . .
H42A H 0.8622 0.2428 0.5216 0.079 Uiso 1 1 calc R . .
C41 C 0.3932(5) 0.2293(3) 0.7452(3) 0.0612(13) Uani 1 1 d . . .
H41A H 0.4664 0.2172 0.7768 0.073 Uiso 1 1 calc R . .
C40 C 0.8785(5) 0.5068(3) 0.8524(3) 0.0724(15) Uani 1 1 d . . .
H40A H 0.9166 0.4900 0.8174 0.087 Uiso 1 1 calc R . .
C39 C 0.2604(5) 0.2056(3) 0.7523(3) 0.0780(16) Uani 1 1 d . . .
H39A H 0.2448 0.1780 0.7883 0.094 Uiso 1 1 calc R . .
C38 C 0.7282(5) 0.1534(3) 0.5248(2) 0.0661(14) Uani 1 1 d . . .
H38A H 0.7557 0.1236 0.4921 0.079 Uiso 1 1 calc R . .
C37 C 0.4237(5) 0.5227(3) 0.6426(2) 0.0717(15) Uani 1 1 d . . .
H37A H 0.3483 0.4957 0.6159 0.086 Uiso 1 1 calc R . .
H37B H 0.3825 0.5587 0.6702 0.086 Uiso 1 1 calc R . .
C36 C 0.7711(6) 0.5605(3) 0.9553(2) 0.0781(16) Uani 1 1 d . . .
H36A H 0.7329 0.5796 0.9896 0.094 Uiso 1 1 calc R . .
C35 C 0.9568(5) 0.5541(3) 0.8979(3) 0.0880(19) Uani 1 1 d . . .
H35A H 1.0467 0.5687 0.8931 0.106 Uiso 1 1 calc R . .
C34 C 0.9026(6) 0.5794(3) 0.9499(3) 0.0776(16) Uani 1 1 d . . .
H34A H 0.9564 0.6094 0.9811 0.093 Uiso 1 1 calc R . .
C33 C 1.0789(5) 0.1020(3) 0.9351(2) 0.0690(14) Uani 1 1 d . . .
C32 C 0.4998(6) 0.5720(3) 0.6020(3) 0.0900(18) Uani 1 1 d . . .
H32A H 0.5444 0.5370 0.5750 0.108 Uiso 1 1 calc R . .
H32B H 0.5715 0.6026 0.6281 0.108 Uiso 1 1 calc R . .
C31 C 0.1522(5) 0.2233(4) 0.7059(4) 0.089(2) Uani 1 1 d . . .
H31A H 0.0624 0.2085 0.7107 0.107 Uiso 1 1 calc R . .
C30 C 0.2405(5) 0.3714(4) 0.8768(3) 0.095(2) Uani 1 1 d . . .
H30A H 0.1583 0.3604 0.8921 0.114 Uiso 1 1 calc R . .
C29 C 0.3588(6) 0.3300(4) 0.9000(3) 0.0831(17) Uani 1 1 d . . .
H29A H 0.3578 0.2916 0.9315 0.100 Uiso 1 1 calc R . .
C28 C 0.3627(5) 0.4448(4) 0.8081(2) 0.0773(17) Uani 1 1 d . . .
H28A H 0.3624 0.4841 0.7772 0.093 Uiso 1 1 calc R . .
C27 C 0.2427(5) 0.4282(5) 0.8318(3) 0.100(2) Uani 1 1 d . . .
H27A H 0.1620 0.4563 0.8167 0.120 Uiso 1 1 calc R . .
C26 C 0.1757(6) 0.2620(5) 0.6536(4) 0.111(2) Uani 1 1 d . . .
H26A H 0.1020 0.2732 0.6220 0.133 Uiso 1 1 calc R . .
C25 C 0.3084(5) 0.2855(4) 0.6462(3) 0.0891(19) Uani 1 1 d . . .
H25A H 0.3232 0.3120 0.6096 0.107 Uiso 1 1 calc R . .
C24 C 0.6242(6) 0.1262(4) 0.5549(3) 0.0892(19) Uani 1 1 d . . .
H24A H 0.5808 0.0776 0.5428 0.107 Uiso 1 1 calc R . .
C23 C 1.1769(6) 0.0763(4) 0.9931(3) 0.108(2) Uani 1 1 d . . .
H23A H 1.2017 0.0207 0.9890 0.162 Uiso 1 1 calc R . .
H23B H 1.1322 0.0827 1.0297 0.162 Uiso 1 1 calc R . .
H23C H 1.2589 0.1090 0.9973 0.162 Uiso 1 1 calc R . .
C45 C 0.4020(7) 0.6303(3) 0.5612(3) 0.106(2) Uani 1 1 d . . .
H45A H 0.4542 0.6619 0.5355 0.159 Uiso 1 1 calc R . .
H45B H 0.3585 0.6654 0.5879 0.159 Uiso 1 1 calc R . .
H45C H 0.3323 0.6001 0.5346 0.159 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 C1 1.688(4) . ?
Fe1 S1 2.1855(13) . ?
Fe1 S2 2.1979(13) . ?
Fe1 P1 2.2184(12) . ?
Fe1 P2 2.2213(13) . ?
P1 C18 1.818(4) . ?
P1 C16 1.819(4) . ?
P1 C17 1.840(4) . ?
S2 C6 1.734(4) . ?
P2 C21 1.815(4) . ?
P2 C15 1.819(4) . ?
P2 C19 1.837(4) . ?
S1 C5 1.736(4) . ?
N1 C17 1.448(5) . ?
N1 C19 1.464(5) . ?
N1 C37 1.480(5) . ?
C22 C33 1.391(6) . ?
C22 C6 1.407(6) . ?
C6 C5 1.403(6) . ?
C21 C28 1.379(6) . ?
C21 C12 1.380(6) . ?
O1 C1 1.171(4) . ?
C20 C18 1.372(6) . ?
C20 C24 1.390(6) . ?
C18 C1O 1.396(6) . ?
C16 C41 1.361(6) . ?
C16 C25 1.389(6) . ?
C15 C40 1.374(6) . ?
C15 C11 1.387(6) . ?
C14 C13 1.376(6) . ?
C14 C5 1.400(6) . ?
C13 C33 1.383(7) . ?
C12 C29 1.390(6) . ?
C11 C36 1.386(6) . ?
C1O C42 1.383(6) . ?
C42 C38 1.351(6) . ?
C41 C39 1.384(6) . ?
C40 C35 1.389(6) . ?
C39 C31 1.369(8) . ?
C38 C24 1.360(7) . ?
C37 C32 1.474(7) . ?
C36 C34 1.342(7) . ?
C35 C34 1.369(7) . ?
C33 C23 1.512(6) . ?
C32 C45 1.537(7) . ?
C31 C26 1.343(8) . ?
C30 C27 1.351(8) . ?
C30 C29 1.370(8) . ?
C28 C27 1.371(7) . ?
C26 C25 1.384(7) . ?

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
C1 Fe1 S1 106.89(15) . . ?
C1 Fe1 S2 99.75(14) . . ?
S1 Fe1 S2 89.32(5) . . ?
C1 Fe1 P1 92.31(14) . . ?
S1 Fe1 P1 87.87(5) . . ?
S2 Fe1 P1 167.92(5) . . ?
C1 Fe1 P2 93.32(15) . . ?
S1 Fe1 P2 159.61(5) . . ?
S2 Fe1 P2 89.82(4) . . ?
P1 Fe1 P2 88.74(4) . . ?
C18 P1 C16 104.8(2) . . ?
C18 P1 C17 99.74(19) . . ?
C16 P1 C17 103.7(2) . . ?
C18 P1 Fe1 115.99(13) . . ?
C16 P1 Fe1 117.03(16) . . ?
C17 P1 Fe1 113.44(15) . . ?
C6 S2 Fe1 105.94(15) . . ?
C21 P2 C15 104.18(19) . . ?
C21 P2 C19 104.5(2) . . ?
C15 P2 C19 100.3(2) . . ?
C21 P2 Fe1 114.05(15) . . ?
C15 P2 Fe1 117.17(13) . . ?
C19 P2 Fe1 114.84(14) . . ?
C5 S1 Fe1 106.22(16) . . ?
C17 N1 C19 113.4(3) . . ?
C17 N1 C37 113.2(3) . . ?
C19 N1 C37 114.9(4) . . ?
C33 C22 C6 121.4(4) . . ?
C5 C6 C22 119.1(4) . . ?
C5 C6 S2 118.8(3) . . ?
C22 C6 S2 122.1(4) . . ?
C28 C21 C12 118.0(4) . . ?
C28 C21 P2 123.7(4) . . ?
C12 C21 P2 118.4(3) . . ?
C18 C20 C24 120.7(5) . . ?
O1 C1 Fe1 177.7(4) . . ?
N1 C19 P2 113.5(3) . . ?
C20 C18 C1O 117.6(4) . . ?
C20 C18 P1 122.8(4) . . ?
C1O C18 P1 119.5(3) . . ?
N1 C17 P1 113.3(3) . . ?
C41 C16 C25 117.7(4) . . ?
C41 C16 P1 121.1(3) . . ?
C25 C16 P1 121.1(4) . . ?
C40 C15 C11 117.6(4) . . ?
C40 C15 P2 120.4(3) . . ?
C11 C15 P2 122.0(3) . . ?
C13 C14 C5 120.6(5) . . ?
C14 C5 C6 119.0(4) . . ?
C14 C5 S1 122.0(4) . . ?
C6 C5 S1 119.0(3) . . ?
C14 C13 C33 121.6(5) . . ?
C21 C12 C29 121.1(5) . . ?
C36 C11 C15 120.7(4) . . ?
C42 C1O C18 120.7(5) . . ?
C38 C42 C1O 120.6(5) . . ?
C16 C41 C39 121.7(5) . . ?
C15 C40 C35 120.9(5) . . ?
C31 C39 C41 119.4(6) . . ?
C42 C38 C24 119.7(5) . . ?
C32 C37 N1 116.6(4) . . ?
C34 C36 C11 121.0(5) . . ?
C34 C35 C40 120.4(5) . . ?
C36 C34 C35 119.4(5) . . ?
C13 C33 C22 118.3(4) . . ?
C13 C33 C23 120.8(5) . . ?
C22 C33 C23 120.9(5) . . ?
C37 C32 C45 111.2(5) . . ?
C26 C31 C39 120.0(5) . . ?
C27 C30 C29 120.4(5) . . ?
C30 C29 C12 119.0(6) . . ?
C27 C28 C21 120.8(5) . . ?
C30 C27 C28 120.7(5) . . ?
C31 C26 C25 120.8(6) . . ?
C26 C25 C16 120.3(6) . . ?
C38 C24 C20 120.6(5) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.074
####################################################################### 
# 
# 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_ok
_database_code_depnum_ccdc_archive 'CCDC 1495099'
_audit_update_record             
;
2016-07-21 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H42 Fe2 N2 O4 P2 S2'
_chemical_formula_weight         876.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

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

_cell_length_a                   11.2393(3)
_cell_length_b                   11.3322(3)
_cell_length_c                   16.6630(4)
_cell_angle_alpha                81.605(2)
_cell_angle_beta                 78.208(2)
_cell_angle_gamma                87.034(2)
_cell_volume                     2054.72(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1804
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      23.45

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             908
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16974
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_sigmaI/netI    0.1263
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         27.49
_reflns_number_total             9240
_reflns_number_gt                4403
_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)+(0.1042P)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         9240
_refine_ls_number_parameters     487
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1943
_refine_ls_wR_factor_gt          0.1400
_refine_ls_goodness_of_fit_ref   0.847
_refine_ls_restrained_S_all      0.847
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.008

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 0.82892(7) 0.49391(6) 0.24475(4) 0.0378(2) Uani 1 1 d . . .
Fe2 Fe 0.84789(7) 0.31440(7) 0.35663(5) 0.0467(2) Uani 1 1 d . . .
P1 P 0.80099(13) 0.68681(12) 0.20730(8) 0.0408(3) Uani 1 1 d . . .
S1 S 0.68181(12) 0.43612(13) 0.35485(8) 0.0459(4) Uani 1 1 d . . .
S2 S 0.94719(12) 0.48846(12) 0.33972(8) 0.0429(3) Uani 1 1 d . . .
P2 P 0.73084(13) 0.44491(12) 0.15189(8) 0.0414(3) Uani 1 1 d . . .
C39 C 0.8814(6) 0.8525(5) 0.2968(4) 0.0524(15) Uani 1 1 d . . .
H39A H 0.8012 0.8576 0.3249 0.063 Uiso 1 1 calc R . .
O1 O 1.0547(4) 0.4819(4) 0.1255(3) 0.0697(13) Uani 1 1 d . . .
C38 C 0.6564(5) 0.7656(5) 0.2375(3) 0.0474(13) Uani 1 1 d . . .
N1 N 0.7378(4) 0.6720(4) 0.0589(3) 0.0508(12) Uani 1 1 d . . .
C37 C 0.9107(5) 0.7808(5) 0.2345(3) 0.0464(14) Uani 1 1 d . . .
C36 C 0.5089(6) 0.3374(5) 0.2221(3) 0.0562(16) Uani 1 1 d . . .
H36A H 0.5564 0.2760 0.2436 0.067 Uiso 1 1 calc R . .
C1 C 0.9645(5) 0.4861(5) 0.1718(3) 0.0494(14) Uani 1 1 d . . .
C34 C 0.5652(5) 0.4377(5) 0.1730(3) 0.0458(13) Uani 1 1 d . . .
N2 N 0.7735(4) 0.5191(4) 0.4783(3) 0.0507(12) Uani 1 1 d . . .
C6 C 0.8826(5) 0.5690(5) 0.4260(3) 0.0501(14) Uani 1 1 d . . .
H6A H 0.9432 0.5712 0.4597 0.060 Uiso 1 1 calc R . .
H6B H 0.8648 0.6506 0.4042 0.060 Uiso 1 1 calc R . .
C32 C 0.7744(6) 0.3048(5) 0.1079(3) 0.0498(14) Uani 1 1 d . . .
O4 O 0.7086(5) 0.1234(4) 0.3213(3) 0.0859(15) Uani 1 1 d . . .
C7 C 0.8261(6) 0.7264(5) 0.0933(3) 0.0506(15) Uani 1 1 d . . .
H7A H 0.8207 0.8124 0.0795 0.061 Uiso 1 1 calc R . .
H7B H 0.9072 0.7002 0.0688 0.061 Uiso 1 1 calc R . .
O3 O 1.0765(4) 0.2111(4) 0.2755(3) 0.0788(14) Uani 1 1 d . . .
C4 C 0.7642(6) 0.1985(6) 0.3356(4) 0.0574(16) Uani 1 1 d . . .
C29 C 0.7229(6) 0.7023(5) 0.5522(3) 0.0502(14) Uani 1 1 d . . .
C12 C 0.7441(6) 0.5687(5) 0.5582(3) 0.0598(17) Uani 1 1 d . . .
H12A H 0.8102 0.5473 0.5873 0.072 Uiso 1 1 calc R . .
H12B H 0.6718 0.5303 0.5916 0.072 Uiso 1 1 calc R . .
C27 C 0.5516(5) 0.7050(5) 0.2760(3) 0.0524(14) Uani 1 1 d . . .
H27A H 0.5553 0.6223 0.2877 0.063 Uiso 1 1 calc R . .
C5 C 0.6712(5) 0.5294(6) 0.4375(3) 0.0577(16) Uani 1 1 d . . .
H5A H 0.6619 0.6121 0.4141 0.069 Uiso 1 1 calc R . .
H5B H 0.5983 0.5087 0.4787 0.069 Uiso 1 1 calc R . .
C25 C 0.3663(7) 0.5194(7) 0.1634(5) 0.076(2) Uani 1 1 d . . .
H25A H 0.3174 0.5815 0.1443 0.091 Uiso 1 1 calc R . .
C24 C 0.8733(6) 0.2363(5) 0.1247(4) 0.0614(17) Uani 1 1 d . . .
H24A H 0.9177 0.2587 0.1612 0.074 Uiso 1 1 calc R . .
C23 C 0.3843(6) 0.3280(6) 0.2393(4) 0.0669(18) Uani 1 1 d . . .
H23A H 0.3482 0.2594 0.2702 0.080 Uiso 1 1 calc R . .
C3 C 0.9872(6) 0.2514(5) 0.3086(4) 0.0574(16) Uani 1 1 d . . .
C21 C 0.9683(7) 0.9161(5) 0.3177(4) 0.0649(17) Uani 1 1 d . . .
H21A H 0.9462 0.9634 0.3598 0.078 Uiso 1 1 calc R . .
C20 C 0.4915(6) 0.5291(6) 0.1434(4) 0.0644(17) Uani 1 1 d . . .
H20A H 0.5263 0.5967 0.1101 0.077 Uiso 1 1 calc R . .
C8 C 0.7663(6) 0.5456(5) 0.0531(3) 0.0530(15) Uani 1 1 d . . .
H8A H 0.8523 0.5370 0.0300 0.064 Uiso 1 1 calc R . .
H8B H 0.7218 0.5202 0.0148 0.064 Uiso 1 1 calc R . .
C2 C 0.8402(6) 0.2652(5) 0.4651(4) 0.0637(17) Uani 1 1 d . . .
C17 C 0.3139(6) 0.4206(7) 0.2104(4) 0.074(2) Uani 1 1 d . . .
H17A H 0.2297 0.4155 0.2232 0.089 Uiso 1 1 calc R . .
C16 C 0.7095(7) 0.2681(5) 0.0533(4) 0.0667(18) Uani 1 1 d . . .
H16A H 0.6414 0.3120 0.0418 0.080 Uiso 1 1 calc R . .
C15 C 0.7453(8) 0.1673(6) 0.0163(4) 0.075(2) Uani 1 1 d . . .
H15A H 0.7016 0.1444 -0.0204 0.090 Uiso 1 1 calc R . .
O2 O 0.8377(5) 0.2298(5) 0.5336(3) 0.0971(18) Uani 1 1 d . . .
C14 C 0.4416(7) 0.7640(7) 0.2976(5) 0.084(2) Uani 1 1 d . . .
H14A H 0.3723 0.7216 0.3234 0.100 Uiso 1 1 calc R . .
C9 C 0.7248(8) 0.7376(6) -0.0228(4) 0.084(2) Uani 1 1 d . . .
H9A H 0.6901 0.6853 -0.0528 0.100 Uiso 1 1 calc R . .
H9B H 0.8046 0.7599 -0.0547 0.100 Uiso 1 1 calc R . .
C72 C 1.1203(6) 0.8399(6) 0.2161(5) 0.075(2) Uani 1 1 d . . .
H72A H 1.2011 0.8355 0.1891 0.090 Uiso 1 1 calc R . .
C71 C 0.8175(7) 0.7780(7) 0.5463(4) 0.074(2) Uani 1 1 d . . .
H71A H 0.8956 0.7464 0.5460 0.089 Uiso 1 1 calc R . .
C70 C 1.0867(7) 0.9111(6) 0.2776(5) 0.0726(19) Uani 1 1 d . . .
H70A H 1.1446 0.9555 0.2919 0.087 Uiso 1 1 calc R . .
C69 C 0.6085(6) 0.7523(6) 0.5521(4) 0.0694(19) Uani 1 1 d . . .
H69A H 0.5428 0.7038 0.5559 0.083 Uiso 1 1 calc R . .
C68 C 0.6471(6) 0.8902(5) 0.2190(4) 0.0662(18) Uani 1 1 d . . .
H68A H 0.7153 0.9334 0.1919 0.079 Uiso 1 1 calc R . .
C67 C 0.5371(8) 0.9488(6) 0.2407(5) 0.087(3) Uani 1 1 d . . .
H67A H 0.5319 1.0314 0.2283 0.104 Uiso 1 1 calc R . .
C66 C 1.0334(6) 0.7748(5) 0.1943(4) 0.0631(17) Uani 1 1 d . . .
H66A H 1.0565 0.7267 0.1528 0.076 Uiso 1 1 calc R . .
C65 C 0.9083(7) 0.1333(6) 0.0875(5) 0.076(2) Uani 1 1 d . . .
H65A H 0.9747 0.0872 0.1000 0.091 Uiso 1 1 calc R . .
C64 C 0.8446(8) 0.1007(6) 0.0331(4) 0.080(2) Uani 1 1 d . . .
H64A H 0.8686 0.0334 0.0075 0.096 Uiso 1 1 calc R . .
C63 C 0.6868(9) 0.9471(7) 0.5396(5) 0.091(3) Uani 1 1 d . . .
H63A H 0.6742 1.0295 0.5339 0.110 Uiso 1 1 calc R . .
C62 C 0.4359(7) 0.8873(8) 0.2803(5) 0.091(3) Uani 1 1 d . . .
H62A H 0.3628 0.9282 0.2957 0.109 Uiso 1 1 calc R . .
C60 C 0.7981(8) 0.9005(7) 0.5410(5) 0.090(2) Uani 1 1 d . . .
H60A H 0.8625 0.9501 0.5384 0.108 Uiso 1 1 calc R . .
C50 C 0.5918(8) 0.8741(7) 0.5464(5) 0.093(3) Uani 1 1 d . . .
H50A H 0.5142 0.9072 0.5472 0.111 Uiso 1 1 calc R . .
C10 C 0.6468(11) 0.8460(7) -0.0150(6) 0.132(4) Uani 1 1 d . . .
H10A H 0.5680 0.8237 0.0185 0.158 Uiso 1 1 calc R . .
H10B H 0.6829 0.8991 0.0136 0.158 Uiso 1 1 calc R . .
C11 C 0.6294(12) 0.9113(9) -0.0962(7) 0.175(6) Uani 1 1 d . . .
H11A H 0.5778 0.9802 -0.0873 0.262 Uiso 1 1 calc R . .
H11B H 0.5925 0.8598 -0.1246 0.262 Uiso 1 1 calc R . .
H11C H 0.7069 0.9359 -0.1292 0.262 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 C1 1.751(6) . ?
Fe1 P1 2.2084(15) . ?
Fe1 P2 2.2201(16) . ?
Fe1 S1 2.2473(14) . ?
Fe1 S2 2.2578(16) . ?
Fe1 Fe2 2.5825(10) . ?
Fe2 C3 1.772(7) . ?
Fe2 C4 1.769(7) . ?
Fe2 C2 1.797(7) . ?
Fe2 S1 2.2654(16) . ?
Fe2 S2 2.2699(16) . ?
P1 C38 1.827(6) . ?
P1 C37 1.834(6) . ?
P1 C7 1.854(5) . ?
S1 C5 1.836(6) . ?
S2 C6 1.821(5) . ?
P2 C34 1.826(6) . ?
P2 C32 1.847(6) . ?
P2 C8 1.844(5) . ?
C39 C37 1.387(8) . ?
C39 C21 1.372(8) . ?
O1 C1 1.146(6) . ?
C38 C27 1.384(8) . ?
C38 C68 1.404(7) . ?
N1 C7 1.447(7) . ?
N1 C8 1.464(7) . ?
N1 C9 1.484(7) . ?
C37 C66 1.407(8) . ?
C36 C23 1.378(8) . ?
C36 C34 1.397(7) . ?
C34 C20 1.390(8) . ?
N2 C5 1.443(7) . ?
N2 C6 1.440(7) . ?
N2 C12 1.488(7) . ?
C32 C24 1.375(8) . ?
C32 C16 1.395(9) . ?
O4 C4 1.160(7) . ?
O3 C3 1.150(7) . ?
C29 C71 1.380(9) . ?
C29 C69 1.378(8) . ?
C29 C12 1.512(8) . ?
C27 C14 1.381(8) . ?
C25 C20 1.385(9) . ?
C25 C17 1.356(9) . ?
C24 C65 1.402(8) . ?
C23 C17 1.371(9) . ?
C21 C70 1.364(9) . ?
C2 O2 1.149(7) . ?
C16 C15 1.380(8) . ?
C15 C64 1.368(10) . ?
C14 C62 1.386(10) . ?
C9 C10 1.478(10) . ?
C72 C66 1.388(9) . ?
C72 C70 1.377(9) . ?
C71 C60 1.386(10) . ?
C69 C50 1.376(9) . ?
C68 C67 1.380(9) . ?
C67 C62 1.362(11) . ?
C65 C64 1.364(10) . ?
C63 C60 1.336(11) . ?
C63 C50 1.360(11) . ?
C10 C11 1.488(11) . ?

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
C1 Fe1 P1 93.52(18) . . ?
C1 Fe1 P2 88.21(19) . . ?
P1 Fe1 P2 92.59(6) . . ?
C1 Fe1 S1 158.44(18) . . ?
P1 Fe1 S1 107.53(6) . . ?
P2 Fe1 S1 95.28(6) . . ?
C1 Fe1 S2 86.37(19) . . ?
P1 Fe1 S2 103.32(6) . . ?
P2 Fe1 S2 163.47(6) . . ?
S1 Fe1 S2 84.32(5) . . ?
C1 Fe1 Fe2 103.51(17) . . ?
P1 Fe1 Fe2 150.96(5) . . ?
P2 Fe1 Fe2 111.05(5) . . ?
S1 Fe1 Fe2 55.42(4) . . ?
S2 Fe1 Fe2 55.44(4) . . ?
C3 Fe2 C4 91.7(3) . . ?
C3 Fe2 C2 103.7(3) . . ?
C4 Fe2 C2 98.1(3) . . ?
C3 Fe2 S1 152.6(2) . . ?
C4 Fe2 S1 88.7(2) . . ?
C2 Fe2 S1 103.3(2) . . ?
C3 Fe2 S2 87.01(19) . . ?
C4 Fe2 S2 160.5(2) . . ?
C2 Fe2 S2 101.1(2) . . ?
S1 Fe2 S2 83.63(6) . . ?
C3 Fe2 Fe1 99.12(18) . . ?
C4 Fe2 Fe1 106.2(2) . . ?
C2 Fe2 Fe1 145.9(2) . . ?
S1 Fe2 Fe1 54.76(4) . . ?
S2 Fe2 Fe1 55.00(4) . . ?
C38 P1 C37 102.8(3) . . ?
C38 P1 C7 100.1(3) . . ?
C37 P1 C7 102.0(3) . . ?
C38 P1 Fe1 123.10(18) . . ?
C37 P1 Fe1 113.90(17) . . ?
C7 P1 Fe1 112.11(19) . . ?
C5 S1 Fe1 112.6(2) . . ?
C5 S1 Fe2 107.89(19) . . ?
Fe1 S1 Fe2 69.82(5) . . ?
C6 S2 Fe1 114.01(19) . . ?
C6 S2 Fe2 108.47(19) . . ?
Fe1 S2 Fe2 69.55(5) . . ?
C34 P2 C32 101.1(3) . . ?
C34 P2 C8 103.6(3) . . ?
C32 P2 C8 96.4(2) . . ?
C34 P2 Fe1 121.37(18) . . ?
C32 P2 Fe1 118.9(2) . . ?
C8 P2 Fe1 111.8(2) . . ?
C37 C39 C21 121.3(6) . . ?
C27 C38 C68 117.7(5) . . ?
C27 C38 P1 121.6(4) . . ?
C68 C38 P1 120.6(5) . . ?
C7 N1 C8 112.0(5) . . ?
C7 N1 C9 111.5(4) . . ?
C8 N1 C9 110.8(5) . . ?
C39 C37 C66 117.4(6) . . ?
C39 C37 P1 123.6(4) . . ?
C66 C37 P1 118.9(5) . . ?
C23 C36 C34 121.2(6) . . ?
O1 C1 Fe1 178.3(6) . . ?
C36 C34 C20 118.0(6) . . ?
C36 C34 P2 119.2(4) . . ?
C20 C34 P2 122.8(4) . . ?
C5 N2 C6 113.1(4) . . ?
C5 N2 C12 111.7(5) . . ?
C6 N2 C12 111.6(5) . . ?
N2 C6 S2 114.8(4) . . ?
C24 C32 C16 118.0(6) . . ?
C24 C32 P2 121.9(5) . . ?
C16 C32 P2 120.1(5) . . ?
N1 C7 P1 111.6(4) . . ?
O4 C4 Fe2 179.4(6) . . ?
C71 C29 C69 117.9(6) . . ?
C71 C29 C12 121.1(6) . . ?
C69 C29 C12 121.0(6) . . ?
N2 C12 C29 116.2(4) . . ?
C38 C27 C14 121.8(6) . . ?
N2 C5 S1 115.2(4) . . ?
C20 C25 C17 121.0(6) . . ?
C32 C24 C65 120.9(7) . . ?
C36 C23 C17 119.5(6) . . ?
O3 C3 Fe2 178.2(6) . . ?
C70 C21 C39 120.9(6) . . ?
C25 C20 C34 119.9(6) . . ?
N1 C8 P2 115.1(4) . . ?
O2 C2 Fe2 177.4(6) . . ?
C25 C17 C23 120.5(6) . . ?
C15 C16 C32 120.8(7) . . ?
C64 C15 C16 120.5(7) . . ?
C27 C14 C62 119.1(7) . . ?
N1 C9 C10 112.3(7) . . ?
C66 C72 C70 120.0(7) . . ?
C29 C71 C60 121.1(7) . . ?
C21 C70 C72 119.8(7) . . ?
C29 C69 C50 119.8(7) . . ?
C67 C68 C38 120.3(7) . . ?
C62 C67 C68 120.9(7) . . ?
C72 C66 C37 120.6(6) . . ?
C64 C65 C24 119.9(7) . . ?
C15 C64 C65 119.9(7) . . ?
C60 C63 C50 119.9(8) . . ?
C67 C62 C14 120.2(7) . . ?
C63 C60 C71 120.0(8) . . ?
C63 C50 C69 121.2(8) . . ?
C11 C10 C9 113.2(9) . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.078
