# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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 1431706'
_audit_update_record             
;
2015-10-16 deposited with the CCDC.
2015-11-16 downloaded from the CCDC.
;
#_cambridge_data_id dw_b2_0027
#===============================================================================
# This structure contains pseudo-translations corresponding to [0.5,0.5,0].
# If these pseudo-translations are considered to be real, the structure can be
# described as essentially identical to the bromo derivative (3).
# However, reconstructed precession photographs show clearly that the
# additional diffraction peaks are present and that this cell is appropriate.
# For (2), there is no sign of any additional peaks to indicate a larger cell.
# Thus, we conclude that this "supercell" structure for the methyl derivative
# (2) is genuine (at least for the crystal that we looked at).
#
# The Flack parameter (Parsons quotients) is 0.034(7): just about statistically
# different from zero. However, refining as an inversion twin produces a scale
# factor of 0.04(2): not statistically different from zero. This CIF does
# **not** include any refinement of inversion twinning.
#==============================================================================
_audit_creation_method           SHELXL-2013

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H18 N3 P'
_chemical_formula_sum            'C18 H18 N3 P'
_chemical_formula_weight         307.32
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c :H'
_space_group_name_Hall           'R 3 -2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   30.7488(8)
_cell_length_b                   30.7488(8)
_cell_length_c                   11.8199(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9678.3(6)
_cell_formula_units_Z            24
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    35814
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      66.70

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_F_000             3888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.495
_shelx_estimated_absorpt_T_min   0.754
_shelx_estimated_absorpt_T_max   0.916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6333
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35814
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.874
_diffrn_reflns_theta_max         66.700
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3769
_reflns_number_gt                3534
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.972
_reflns_Friedel_fraction_max     0.980
_reflns_Friedel_fraction_full    0.956

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.

_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0428P)²+2.4332P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_Flack   0.034(7)
_refine_ls_abs_structure_details 
;
Flack x determined using 1656 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_number_reflns         3769
_refine_ls_number_parameters     275
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0742
_refine_ls_wR_factor_gt          0.0719
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.114
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.036

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.33298(2) 0.16169(2) 0.31579(6) 0.02578(16) Uani 1 1 d . . . . .
N1 N 0.43196(6) 0.19527(7) 0.32911(15) 0.0331(4) Uani 1 1 d . . . . .
N2 N 0.29456(7) 0.22264(7) 0.33767(17) 0.0359(4) Uani 1 1 d . . . . .
N3 N 0.26718(7) 0.06389(6) 0.34761(15) 0.0313(4) Uani 1 1 d . . . . .
C11 C 0.39511(8) 0.19834(7) 0.38370(19) 0.0289(5) Uani 1 1 d . . . . .
C12 C 0.40380(9) 0.22529(9) 0.4835(2) 0.0436(6) Uani 1 1 d . . . . .
H12 H 0.3773 0.2271 0.5204 0.052 Uiso 1 1 calc R U . . .
C13 C 0.45173(11) 0.24947(11) 0.5282(3) 0.0583(8) Uani 1 1 d . . . . .
H13 H 0.4585 0.2676 0.5971 0.070 Uiso 1 1 calc R U . . .
C14 C 0.48939(10) 0.24703(10) 0.4721(3) 0.0536(8) Uani 1 1 d . . . . .
H14 H 0.5227 0.2639 0.5010 0.064 Uiso 1 1 calc R U . . .
C15 C 0.47836(8) 0.21956(9) 0.3724(2) 0.0409(6) Uani 1 1 d . . . . .
C16 C 0.51887(10) 0.21576(12) 0.3083(3) 0.0628(8) Uani 1 1 d . . . . .
H16A H 0.5068 0.1806 0.2882 0.094 Uiso 1 1 calc R U . . .
H16B H 0.5489 0.2282 0.3559 0.094 Uiso 1 1 calc R U . . .
H16C H 0.5273 0.2360 0.2393 0.094 Uiso 1 1 calc R U . . .
C21 C 0.29783(7) 0.18642(8) 0.39393(18) 0.0287(5) Uani 1 1 d . . . . .
C22 C 0.27852(9) 0.17106(9) 0.5021(2) 0.0391(6) Uani 1 1 d . . . . .
H22 H 0.2809 0.1449 0.5390 0.047 Uiso 1 1 calc R U . . .
C23 C 0.25575(10) 0.19471(11) 0.5550(2) 0.0496(6) Uani 1 1 d . . . . .
H23 H 0.2430 0.1856 0.6296 0.059 Uiso 1 1 calc R U . . .
C24 C 0.25197(10) 0.23142(11) 0.4979(2) 0.0475(7) Uani 1 1 d . . . . .
H24 H 0.2361 0.2478 0.5323 0.057 Uiso 1 1 calc R U . . .
C25 C 0.27152(9) 0.24452(10) 0.3892(2) 0.0416(6) Uani 1 1 d . . . . .
C26 C 0.26722(12) 0.28394(13) 0.3233(3) 0.0677(9) Uani 1 1 d . . . . .
H26A H 0.3008 0.3126 0.3098 0.102 Uiso 1 1 calc R U . . .
H26B H 0.2473 0.2950 0.3665 0.102 Uiso 1 1 calc R U . . .
H26C H 0.2507 0.2699 0.2508 0.102 Uiso 1 1 calc R U . . .
C31 C 0.30998(8) 0.10145(8) 0.39167(18) 0.0291(5) Uani 1 1 d . . . . .
C32 C 0.33297(10) 0.09476(9) 0.4855(2) 0.0444(6) Uani 1 1 d . . . . .
H32 H 0.3631 0.1219 0.5149 0.053 Uiso 1 1 calc R U . . .
C33 C 0.31134(11) 0.04793(11) 0.5354(3) 0.0602(8) Uani 1 1 d . . . . .
H33 H 0.3263 0.0426 0.6003 0.072 Uiso 1 1 calc R U . . .
C34 C 0.26840(11) 0.00939(10) 0.4912(2) 0.0500(7) Uani 1 1 d . . . . .
H34 H 0.2533 -0.0231 0.5240 0.060 Uiso 1 1 calc R U . . .
C35 C 0.24695(9) 0.01866(8) 0.3965(2) 0.0379(6) Uani 1 1 d . . . . .
C36 C 0.19921(10) -0.02252(9) 0.3454(3) 0.0558(7) Uani 1 1 d . . . . .
H36A H 0.1703 -0.0243 0.3848 0.084 Uiso 1 1 calc R U . . .
H36B H 0.1984 -0.0546 0.3532 0.084 Uiso 1 1 calc R U . . .
H36C H 0.1978 -0.0154 0.2651 0.084 Uiso 1 1 calc R U . . .
P2 P 0.6667 0.3333 0.46991(7) 0.0249(3) Uani 1 3 d S T P . .
N4 N 0.60114(7) 0.36629(6) 0.49000(16) 0.0318(5) Uani 1 1 d . . . . .
C41 C 0.64075(8) 0.36842(7) 0.54351(19) 0.0280(5) Uani 1 1 d . . . . .
C42 C 0.65877(9) 0.39360(9) 0.6455(2) 0.0399(6) Uani 1 1 d . . . . .
H42 H 0.6869 0.3947 0.6814 0.046(7) Uiso 1 1 calc R . . . .
C43 C 0.63503(10) 0.41705(10) 0.6938(2) 0.0513(7) Uani 1 1 d . . . . .
H43 H 0.6462 0.4339 0.7643 0.069(9) Uiso 1 1 calc R . . . .
C44 C 0.59507(11) 0.41575(10) 0.6387(2) 0.0498(7) Uani 1 1 d . . . . .
H44 H 0.5788 0.4324 0.6696 0.067(9) Uiso 1 1 calc R . . . .
C45 C 0.57878(9) 0.38987(8) 0.5375(2) 0.0381(6) Uani 1 1 d . . . . .
C46 C 0.53448(11) 0.38660(13) 0.4746(3) 0.0584(8) Uani 1 1 d . . . . .
H46A H 0.5460 0.4053 0.4033 0.117(14) Uiso 1 1 calc R . . . .
H46B H 0.5185 0.4011 0.5211 0.098(11) Uiso 1 1 calc R . . . .
H46C H 0.5102 0.3513 0.4584 0.121(15) 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
P1 C11 1.847(2) . ?
P1 C21 1.849(2) . ?
P1 C31 1.851(2) . ?
N1 C15 1.338(3) . ?
N1 C11 1.348(3) . ?
N2 C25 1.342(3) . ?
N2 C21 1.344(3) . ?
N3 C35 1.338(3) . ?
N3 C31 1.348(3) . ?
C11 C12 1.389(3) . ?
C12 C13 1.381(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.369(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.512(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 C22 1.389(3) . ?
C22 C23 1.385(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.369(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.390(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.501(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C31 C32 1.384(3) . ?
C32 C33 1.381(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.362(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.399(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.504(3) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
P2 C41 1.848(2) 3_665 ?
P2 C41 1.848(2) 2_655 ?
P2 C41 1.848(2) . ?
N4 C41 1.345(3) . ?
N4 C45 1.346(3) . ?
C41 C42 1.390(3) . ?
C42 C43 1.380(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.374(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.384(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.511(4) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 P1 C21 99.84(9) . . ?
C11 P1 C31 99.27(10) . . ?
C21 P1 C31 99.21(9) . . ?
C15 N1 C11 118.5(2) . . ?
C25 N2 C21 117.9(2) . . ?
C35 N3 C31 118.1(2) . . ?
N1 C11 C12 122.1(2) . . ?
N1 C11 P1 113.49(16) . . ?
C12 C11 P1 124.40(17) . . ?
C13 C12 C11 118.8(2) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C14 C13 C12 119.3(3) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 119.2(2) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
N1 C15 C14 122.1(2) . . ?
N1 C15 C16 117.1(2) . . ?
C14 C15 C16 120.8(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C21 C22 122.7(2) . . ?
N2 C21 P1 113.27(16) . . ?
C22 C21 P1 123.94(18) . . ?
C23 C22 C21 118.6(2) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C24 C23 C22 119.0(2) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
C23 C24 C25 119.5(2) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
N2 C25 C24 122.3(2) . . ?
N2 C25 C26 116.8(2) . . ?
C24 C25 C26 120.9(2) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C31 C32 122.3(2) . . ?
N3 C31 P1 113.02(16) . . ?
C32 C31 P1 124.66(18) . . ?
C33 C32 C31 118.8(2) . . ?
C33 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
C34 C33 C32 119.7(3) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C33 C34 C35 118.7(2) . . ?
C33 C34 H34 120.7 . . ?
C35 C34 H34 120.7 . . ?
N3 C35 C34 122.4(2) . . ?
N3 C35 C36 116.9(2) . . ?
C34 C35 C36 120.7(2) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C41 P2 C41 99.65(9) 3_665 2_655 ?
C41 P2 C41 99.64(9) 3_665 . ?
C41 P2 C41 99.65(9) 2_655 . ?
C41 N4 C45 118.2(2) . . ?
N4 C41 C42 122.3(2) . . ?
N4 C41 P2 113.25(17) . . ?
C42 C41 P2 124.44(17) . . ?
C43 C42 C41 118.8(2) . . ?
C43 C42 H42 120.6 . . ?
C41 C42 H42 120.6 . . ?
C44 C43 C42 119.2(3) . . ?
C44 C43 H43 120.4 . . ?
C42 C43 H43 120.4 . . ?
C43 C44 C45 119.2(2) . . ?
C43 C44 H44 120.4 . . ?
C45 C44 H44 120.4 . . ?
N4 C45 C44 122.3(2) . . ?
N4 C45 C46 116.5(2) . . ?
C44 C45 C46 121.2(2) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 N1 C11 C12 -0.8(3) . . . . ?
C15 N1 C11 P1 -178.61(16) . . . . ?
C21 P1 C11 N1 -168.15(15) . . . . ?
C31 P1 C11 N1 90.74(17) . . . . ?
C21 P1 C11 C12 14.1(2) . . . . ?
C31 P1 C11 C12 -87.0(2) . . . . ?
N1 C11 C12 C13 -0.3(4) . . . . ?
P1 C11 C12 C13 177.3(2) . . . . ?
C11 C12 C13 C14 1.2(4) . . . . ?
C12 C13 C14 C15 -1.1(4) . . . . ?
C11 N1 C15 C14 0.9(3) . . . . ?
C11 N1 C15 C16 -179.3(2) . . . . ?
C13 C14 C15 N1 0.0(4) . . . . ?
C13 C14 C15 C16 -179.7(3) . . . . ?
C25 N2 C21 C22 -0.1(3) . . . . ?
C25 N2 C21 P1 -177.34(17) . . . . ?
C11 P1 C21 N2 97.96(17) . . . . ?
C31 P1 C21 N2 -160.88(16) . . . . ?
C11 P1 C21 C22 -79.3(2) . . . . ?
C31 P1 C21 C22 21.9(2) . . . . ?
N2 C21 C22 C23 -1.2(3) . . . . ?
P1 C21 C22 C23 175.76(18) . . . . ?
C21 C22 C23 C24 1.6(4) . . . . ?
C22 C23 C24 C25 -0.8(4) . . . . ?
C21 N2 C25 C24 1.0(3) . . . . ?
C21 N2 C25 C26 -178.5(2) . . . . ?
C23 C24 C25 N2 -0.6(4) . . . . ?
C23 C24 C25 C26 178.9(3) . . . . ?
C35 N3 C31 C32 -0.7(3) . . . . ?
C35 N3 C31 P1 -179.52(16) . . . . ?
C11 P1 C31 N3 -170.78(15) . . . . ?
C21 P1 C31 N3 87.57(17) . . . . ?
C11 P1 C31 C32 10.5(2) . . . . ?
C21 P1 C31 C32 -91.2(2) . . . . ?
N3 C31 C32 C33 0.2(4) . . . . ?
P1 C31 C32 C33 178.8(2) . . . . ?
C31 C32 C33 C34 0.6(4) . . . . ?
C32 C33 C34 C35 -0.8(5) . . . . ?
C31 N3 C35 C34 0.5(3) . . . . ?
C31 N3 C35 C36 -180.0(2) . . . . ?
C33 C34 C35 N3 0.3(4) . . . . ?
C33 C34 C35 C36 -179.2(3) . . . . ?
C45 N4 C41 C42 0.5(3) . . . . ?
C45 N4 C41 P2 178.85(15) . . . . ?
C41 P2 C41 N4 165.15(16) 3_665 . . . ?
C41 P2 C41 N4 -93.2(2) 2_655 . . . ?
C41 P2 C41 C42 -16.5(2) 3_665 . . . ?
C41 P2 C41 C42 85.07(15) 2_655 . . . ?
N4 C41 C42 C43 0.3(4) . . . . ?
P2 C41 C42 C43 -177.85(19) . . . . ?
C41 C42 C43 C44 -1.4(4) . . . . ?
C42 C43 C44 C45 1.7(4) . . . . ?
C41 N4 C45 C44 -0.2(3) . . . . ?
C41 N4 C45 C46 179.9(2) . . . . ?
C43 C44 C45 N4 -0.9(4) . . . . ?
C43 C44 C45 C46 179.0(3) . . . . ?

####################################################################### 
# 
# 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 1431707'
_audit_update_record             
;
2015-10-16 deposited with the CCDC.
2015-11-16 downloaded from the CCDC.
;
#_cambridge_data_id DW_B1_0021
#===============================================================================
_audit_creation_method           SHELXL-2013

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H9 Br3 N3 P'
_chemical_formula_sum            'C15 H9 Br3 N3 P'
_chemical_formula_weight         501.95
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c :H'
_space_group_name_Hall           'R 3 -2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'-y, -x, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-y+2/3, -x+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-y+1/3, -x+2/3, z+7/6'

_cell_length_a                   15.7876(6)
_cell_length_b                   15.7876(6)
_cell_length_c                   11.1637(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2409.7(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    4282
_cell_measurement_theta_min      5.60
_cell_measurement_theta_max      66.62

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_F_000             1440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    10.247
_shelx_estimated_absorpt_T_min   0.211
_shelx_estimated_absorpt_T_max   0.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4940
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7384
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         5.604
_diffrn_reflns_theta_max         66.738
_diffrn_reflns_theta_full        66.738
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             941
_reflns_number_gt                873
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_max     0.983
_reflns_Friedel_fraction_full    0.967

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.

_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0142P)²+16.7202P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_abs_structure_details 
;
Flack x determined using 393 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_number_reflns         941
_refine_ls_number_parameters     67
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0624
_refine_ls_wR_factor_gt          0.0609
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.089

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.10118(7) 0.38222(6) 0.62101(9) 0.0386(3) Uani 1 1 d . . . . .
P1 P 0.0000 0.0000 0.6076(3) 0.0208(7) Uani 1 3 d S T P . .
N1 N 0.0634(4) 0.1915(5) 0.6370(6) 0.0224(16) Uani 1 1 d . . . . .
C11 C 0.0722(5) 0.1180(5) 0.6870(6) 0.0206(17) Uani 1 1 d . . . . .
C12 C 0.1277(6) 0.1315(6) 0.7870(8) 0.0258(18) Uani 1 1 d . . . . .
H12 H 0.1313 0.0780 0.8205 0.031 Uiso 1 1 calc R U . . .
C13 C 0.1789(7) 0.2234(7) 0.8395(8) 0.033(2) Uani 1 1 d . . . . .
H13 H 0.2180 0.2338 0.9087 0.040 Uiso 1 1 calc R U . . .
C14 C 0.1718(6) 0.2987(6) 0.7895(8) 0.031(2) Uani 1 1 d . . . . .
H14 H 0.2060 0.3629 0.8220 0.037 Uiso 1 1 calc R U . . .
C15 C 0.1130(5) 0.2779(6) 0.6902(7) 0.0243(18) Uani 1 1 d . . . . .


_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
Br1 C15 1.912(8) . ?
P1 C11 1.852(8) . ?
P1 C11 1.852(8) 2 ?
P1 C11 1.852(8) 3 ?
N1 C15 1.326(10) . ?
N1 C11 1.356(9) . ?
C11 C12 1.369(11) . ?
C12 C13 1.390(12) . ?
C12 H12 0.9500 . ?
C13 C14 1.368(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.375(12) . ?
C14 H14 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 P1 C11 99.0(3) . 2 ?
C11 P1 C11 99.0(3) . 3 ?
C11 P1 C11 99.0(3) 2 3 ?
C15 N1 C11 115.8(7) . . ?
N1 C11 C12 122.3(7) . . ?
N1 C11 P1 112.9(5) . . ?
C12 C11 P1 124.8(6) . . ?
C11 C12 C13 120.0(8) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 118.6(8) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C13 C14 C15 117.4(8) . . ?
C13 C14 H14 121.3 . . ?
C15 C14 H14 121.3 . . ?
N1 C15 C14 126.1(8) . . ?
N1 C15 Br1 116.3(6) . . ?
C14 C15 Br1 117.6(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 N1 C11 C12 0.8(10) . . . . ?
C15 N1 C11 P1 179.7(5) . . . . ?
C11 P1 C11 N1 -87.3(7) 2 . . . ?
C11 P1 C11 N1 172.0(5) 3 . . . ?
C11 P1 C11 C12 91.5(5) 2 . . . ?
C11 P1 C11 C12 -9.2(7) 3 . . . ?
N1 C11 C12 C13 -1.2(12) . . . . ?
P1 C11 C12 C13 -179.9(6) . . . . ?
C11 C12 C13 C14 0.4(13) . . . . ?
C12 C13 C14 C15 0.6(13) . . . . ?
C11 N1 C15 C14 0.3(11) . . . . ?
C11 N1 C15 Br1 -179.9(5) . . . . ?
C13 C14 C15 N1 -1.0(13) . . . . ?
C13 C14 C15 Br1 179.2(7) . . . . ?

####################################################################### 
# 
# 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 1431708'
_audit_update_record             
;
2015-10-16 deposited with the CCDC.
2015-11-16 downloaded from the CCDC.
;
#_cambridge_data_id DW_B1_0024
#===============================================================================
_audit_creation_method           SHELXL-2013

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H24 Fe N6 P2 2+, 2(C F3 O3 S -)'
_chemical_formula_sum            'C32 H24 F6 Fe N6 O6 P2 S2'
_chemical_formula_weight         884.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   17.6327(9)
_cell_length_b                   20.0111(11)
_cell_length_c                   19.8093(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.836(2)
_cell_angle_gamma                90
_cell_volume                     6986.1(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9786
_cell_measurement_theta_min      3.97
_cell_measurement_theta_max      66.65

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_F_000             3584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    6.234
_shelx_estimated_absorpt_T_min   0.400
_shelx_estimated_absorpt_T_max   0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5267
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            103989
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.140
_diffrn_reflns_theta_max         66.729
_diffrn_reflns_theta_full        66.730
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12364
_reflns_number_gt                10244
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.

_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0478P)²+8.7109P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12364
_refine_ls_number_parameters     991
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1017
_refine_ls_wR_factor_gt          0.0939
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.167
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.073

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.01408(2) 0.68688(2) 0.74489(2) 0.01763(10) Uani 1 1 d . . . . .
Fe2 Fe 0.51070(2) 0.66848(2) 0.74133(2) 0.01758(10) Uani 1 1 d . . . . .
P1 P -0.07320(4) 0.70116(4) 0.89304(3) 0.02224(15) Uani 1 1 d . . . . .
P2 P 0.10268(4) 0.68262(4) 0.59699(3) 0.02456(16) Uani 1 1 d . . . . .
P3 P 0.32147(4) 0.66488(4) 0.73542(3) 0.02317(15) Uani 1 1 d . . . . .
P4 P 0.69982(4) 0.67242(4) 0.74741(4) 0.02507(16) Uani 1 1 d . . . . .
S1 S 0.62390(4) 0.37294(4) 0.96656(4) 0.03135(17) Uani 1 1 d . . . . .
N4 N 0.08787(12) 0.75533(11) 0.71536(10) 0.0213(5) Uani 1 1 d . . . . .
C41 C 0.12498(15) 0.75032(14) 0.65633(13) 0.0229(6) Uani 1 1 d . . . . .
C45 C 0.10569(16) 0.80767(14) 0.75558(14) 0.0256(6) Uani 1 1 d . . . . .
H45 H 0.0789 0.8130 0.7961 0.031 Uiso 1 1 calc R U . . .
C44 C 0.16081(16) 0.85398(15) 0.74096(15) 0.0309(6) Uani 1 1 d . . . . .
H44 H 0.1710 0.8903 0.7707 0.037 Uiso 1 1 calc R U . . .
C42 C 0.18172(16) 0.79472(15) 0.63965(14) 0.0290(6) Uani 1 1 d . . . . .
H42 H 0.2074 0.7893 0.5986 0.035 Uiso 1 1 calc R U . . .
C43 C 0.20093(17) 0.84687(15) 0.68266(16) 0.0336(7) Uani 1 1 d . . . . .
H43 H 0.2406 0.8770 0.6724 0.040 Uiso 1 1 calc R U . . .
C55 C 0.09424(16) 0.55837(14) 0.75624(14) 0.0267(6) Uani 1 1 d . . . . .
H55 H 0.0704 0.5569 0.7986 0.032 Uiso 1 1 calc R U . . .
C53 C 0.17600(16) 0.50707(15) 0.67844(15) 0.0318(7) Uani 1 1 d . . . . .
H53 H 0.2089 0.4719 0.6661 0.038 Uiso 1 1 calc R U . . .
C54 C 0.13983(16) 0.50540(15) 0.73905(15) 0.0310(6) Uani 1 1 d . . . . .
H54 H 0.1462 0.4683 0.7686 0.037 Uiso 1 1 calc R U . . .
C51 C 0.11609(14) 0.61232(14) 0.65577(13) 0.0223(5) Uani 1 1 d . . . . .
C52 C 0.16334(15) 0.56109(14) 0.63599(14) 0.0272(6) Uani 1 1 d . . . . .
H52 H 0.1869 0.5630 0.5936 0.033 Uiso 1 1 calc R U . . .
N1 N 0.06784(12) 0.68853(10) 0.83566(10) 0.0194(5) Uani 1 1 d . . . . .
N3 N -0.05954(12) 0.61975(11) 0.78006(10) 0.0211(5) Uani 1 1 d . . . . .
C35 C -0.07773(16) 0.56417(14) 0.74448(14) 0.0262(6) Uani 1 1 d . . . . .
H35 H -0.0568 0.5588 0.7012 0.031 Uiso 1 1 calc R U . . .
C15 C 0.14402(15) 0.68255(13) 0.84063(14) 0.0236(6) Uani 1 1 d . . . . .
H15 H 0.1710 0.6775 0.8002 0.028 Uiso 1 1 calc R U . . .
C14 C 0.18484(16) 0.68335(14) 0.90118(14) 0.0275(6) Uani 1 1 d . . . . .
H14 H 0.2384 0.6781 0.9021 0.033 Uiso 1 1 calc R U . . .
C32 C -0.13891(15) 0.57845(14) 0.86739(14) 0.0267(6) Uani 1 1 d . . . . .
H32 H -0.1592 0.5842 0.9108 0.032 Uiso 1 1 calc R U . . .
C31 C -0.09133(14) 0.62656(13) 0.84143(12) 0.0210(5) Uani 1 1 d . . . . .
C34 C -0.12500(17) 0.51479(15) 0.76740(15) 0.0325(7) Uani 1 1 d . . . . .
H34 H -0.1356 0.4763 0.7406 0.039 Uiso 1 1 calc R U . . .
C12 C 0.06866(16) 0.69854(14) 0.95650(13) 0.0261(6) Uani 1 1 d . . . . .
H12 H 0.0410 0.7046 0.9964 0.031 Uiso 1 1 calc R U . . .
C13 C 0.14673(17) 0.69189(15) 0.96056(14) 0.0302(6) Uani 1 1 d . . . . .
H13 H 0.1735 0.6931 1.0029 0.036 Uiso 1 1 calc R U . . .
C33 C -0.15664(17) 0.52215(15) 0.82986(16) 0.0342(7) Uani 1 1 d . . . . .
H33 H -0.1899 0.4892 0.8466 0.041 Uiso 1 1 calc R U . . .
C11 C 0.03059(15) 0.69640(13) 0.89407(13) 0.0206(5) Uani 1 1 d . . . . .
C75 C 0.48238(17) 0.54412(14) 0.81490(14) 0.0279(6) Uani 1 1 d . . . . .
H75 H 0.5361 0.5407 0.8144 0.033 Uiso 1 1 calc R U . . .
N7 N 0.44883(12) 0.59522(11) 0.78088(11) 0.0222(5) Uani 1 1 d . . . . .
C73 C 0.36520(18) 0.50145(15) 0.85204(14) 0.0331(7) Uani 1 1 d . . . . .
H73 H 0.3369 0.4708 0.8779 0.040 Uiso 1 1 calc R U . . .
C74 C 0.44323(18) 0.49676(15) 0.85024(14) 0.0322(7) Uani 1 1 d . . . . .
H74 H 0.4695 0.4615 0.8730 0.039 Uiso 1 1 calc R U . . .
C71 C 0.37191(15) 0.59745(14) 0.78026(13) 0.0225(6) Uani 1 1 d . . . . .
C72 C 0.32926(16) 0.55170(15) 0.81540(14) 0.0277(6) Uani 1 1 d . . . . .
H72 H 0.2755 0.5549 0.8143 0.033 Uiso 1 1 calc R U . . .
N8 N 0.44839(12) 0.66764(11) 0.65583(11) 0.0199(5) Uani 1 1 d . . . . .
C83 C 0.36294(17) 0.66467(16) 0.53472(14) 0.0322(7) Uani 1 1 d . . . . .
H83 H 0.3338 0.6637 0.4936 0.039 Uiso 1 1 calc R U . . .
C81 C 0.37151(14) 0.66613(13) 0.65576(13) 0.0213(5) Uani 1 1 d . . . . .
C85 C 0.48125(15) 0.66758(13) 0.59530(13) 0.0226(6) Uani 1 1 d . . . . .
H85 H 0.5351 0.6688 0.5945 0.027 Uiso 1 1 calc R U . . .
C82 C 0.32805(15) 0.66498(15) 0.59619(14) 0.0271(6) Uani 1 1 d . . . . .
H82 H 0.2743 0.6644 0.5976 0.032 Uiso 1 1 calc R U . . .
C84 C 0.44102(16) 0.66586(14) 0.53448(14) 0.0271(6) Uani 1 1 d . . . . .
H84 H 0.4667 0.6655 0.4931 0.033 Uiso 1 1 calc R U . . .
C102 C 0.69252(16) 0.78894(14) 0.67276(14) 0.0264(6) Uani 1 1 d . . . . .
H102 H 0.7463 0.7861 0.6743 0.032 Uiso 1 1 calc R U . . .
C105 C 0.53889(15) 0.79418(14) 0.67016(13) 0.0245(6) Uani 1 1 d . . . . .
H105 H 0.4850 0.7965 0.6689 0.029 Uiso 1 1 calc R U . . .
C104 C 0.57864(16) 0.84465(14) 0.63914(14) 0.0276(6) Uani 1 1 d . . . . .
H104 H 0.5525 0.8809 0.6180 0.033 Uiso 1 1 calc R U . . .
C103 C 0.65654(16) 0.84146(15) 0.63932(15) 0.0298(6) Uani 1 1 d . . . . .
H103 H 0.6851 0.8746 0.6170 0.036 Uiso 1 1 calc R U . . .
C101 C 0.64956(14) 0.74059(14) 0.70392(13) 0.0221(6) Uani 1 1 d . . . . .
N9 N 0.44524(12) 0.73879(11) 0.78094(10) 0.0203(5) Uani 1 1 d . . . . .
N10 N 0.57241(11) 0.74188(11) 0.70202(10) 0.0209(5) Uani 1 1 d . . . . .
C95 C 0.47681(15) 0.79147(14) 0.81362(13) 0.0236(6) Uani 1 1 d . . . . .
H95 H 0.5305 0.7958 0.8146 0.028 Uiso 1 1 calc R U . . .
C93 C 0.35697(16) 0.83340(14) 0.84580(14) 0.0286(6) Uani 1 1 d . . . . .
H93 H 0.3270 0.8649 0.8690 0.034 Uiso 1 1 calc R U . . .
C94 C 0.43467(16) 0.83956(14) 0.84579(14) 0.0277(6) Uani 1 1 d . . . . .
H94 H 0.4591 0.8764 0.8676 0.033 Uiso 1 1 calc R U . . .
C91 C 0.36835(14) 0.73460(14) 0.77917(13) 0.0212(5) Uani 1 1 d . . . . .
C92 C 0.32331(15) 0.78068(14) 0.81143(13) 0.0245(6) Uani 1 1 d . . . . .
H92 H 0.2697 0.7760 0.8099 0.029 Uiso 1 1 calc R U . . .
C125 C 0.54009(16) 0.66750(14) 0.88774(13) 0.0242(6) Uani 1 1 d . . . . .
H125 H 0.4863 0.6677 0.8886 0.029 Uiso 1 1 calc R U . . .
C121 C 0.65012(15) 0.67129(14) 0.82723(13) 0.0233(6) Uani 1 1 d . . . . .
C122 C 0.69326(16) 0.67097(15) 0.88656(15) 0.0312(7) Uani 1 1 d . . . . .
H122 H 0.7470 0.6733 0.8851 0.037 Uiso 1 1 calc R U . . .
C123 C 0.65883(18) 0.66725(17) 0.94817(15) 0.0360(7) Uani 1 1 d . . . . .
H123 H 0.6882 0.6660 0.9892 0.043 Uiso 1 1 calc R U . . .
C124 C 0.58053(17) 0.66547(15) 0.94847(14) 0.0305(6) Uani 1 1 d . . . . .
H124 H 0.5549 0.6629 0.9899 0.037 Uiso 1 1 calc R U . . .
N12 N 0.57304(12) 0.66922(11) 0.82692(11) 0.0216(5) Uani 1 1 d . . . . .
N6 N -0.03921(12) 0.68433(11) 0.65410(10) 0.0202(5) Uani 1 1 d . . . . .
C61 C -0.00135(15) 0.68511(13) 0.59564(13) 0.0233(6) Uani 1 1 d . . . . .
C65 C -0.11585(16) 0.68384(14) 0.64891(14) 0.0248(6) Uani 1 1 d . . . . .
H65 H -0.1434 0.6833 0.6894 0.030 Uiso 1 1 calc R U . . .
C64 C -0.15635(17) 0.68411(15) 0.58815(14) 0.0297(6) Uani 1 1 d . . . . .
H64 H -0.2102 0.6828 0.5871 0.036 Uiso 1 1 calc R U . . .
C63 C -0.11730(17) 0.68628(16) 0.52914(15) 0.0336(7) Uani 1 1 d . . . . .
H63 H -0.1438 0.6876 0.4866 0.040 Uiso 1 1 calc R U . . .
C62 C -0.03874(17) 0.68655(15) 0.53277(14) 0.0294(6) Uani 1 1 d . . . . .
H62 H -0.0106 0.6877 0.4927 0.035 Uiso 1 1 calc R U . . .
O1 O 0.62212(13) 0.36052(13) 1.03818(11) 0.0443(6) Uani 1 1 d . . . . .
O2 O 0.55272(12) 0.36478(12) 0.93001(11) 0.0404(5) Uani 1 1 d . . . . .
O3 O 0.68839(13) 0.34585(13) 0.93329(12) 0.0479(6) Uani 1 1 d . . . . .
C4 C 0.6399(2) 0.46280(18) 0.96084(16) 0.0418(8) Uani 1 1 d . . . . .
F13 F 0.70368(14) 0.48133(13) 0.99207(12) 0.0711(7) Uani 1 1 d . . . . .
F11 F 0.58427(14) 0.49792(11) 0.98721(11) 0.0626(6) Uani 1 1 d . . . . .
F12 F 0.64396(14) 0.48238(11) 0.89590(10) 0.0598(6) Uani 1 1 d . . . . .
S2 S 0.84837(4) 0.38738(4) 0.59224(4) 0.03534(18) Uani 1 1 d . . . . .
O4 O 0.90328(12) 0.33739(12) 0.57906(12) 0.0414(5) Uani 1 1 d . . . . .
O6 O 0.78151(13) 0.38599(13) 0.54918(16) 0.0630(8) Uani 1 1 d . . . . .
O5 O 0.83530(18) 0.39745(17) 0.66294(14) 0.0809(11) Uani 1 1 d . . . . .
C2 C 0.89473(18) 0.46472(17) 0.56823(17) 0.0406(8) Uani 1 1 d . . . . .
F4 F 0.95780(10) 0.47635(10) 0.60522(10) 0.0476(5) Uani 1 1 d . . . . .
F5 F 0.85013(14) 0.51699(12) 0.57757(18) 0.0897(9) Uani 1 1 d . . . . .
F6 F 0.91465(16) 0.46316(14) 0.50467(11) 0.0796(8) Uani 1 1 d . . . . .
S3 S 0.36673(4) 0.37759(4) 0.55827(4) 0.03525(18) Uani 1 1 d . . . . .
N5 N 0.08153(12) 0.61216(11) 0.71629(10) 0.0214(5) Uani 1 1 d . . . . .
C25 C -0.06936(16) 0.81051(14) 0.72284(14) 0.0251(6) Uani 1 1 d . . . . .
H25 H -0.0409 0.8118 0.6829 0.030 Uiso 1 1 calc R U . . .
C21 C -0.09205(15) 0.76313(13) 0.82665(13) 0.0217(5) Uani 1 1 d . . . . .
C24 C -0.12451(16) 0.85874(15) 0.73153(14) 0.0288(6) Uani 1 1 d . . . . .
H24 H -0.1332 0.8924 0.6983 0.035 Uiso 1 1 calc R U . . .
C22 C -0.14918(15) 0.80943(14) 0.83758(14) 0.0260(6) Uani 1 1 d . . . . .
H22 H -0.1762 0.8082 0.8783 0.031 Uiso 1 1 calc R U . . .
C23 C -0.16669(16) 0.85734(15) 0.78898(15) 0.0308(7) Uani 1 1 d . . . . .
H23 H -0.2067 0.8884 0.7951 0.037 Uiso 1 1 calc R U . . .
N2 N -0.05408(12) 0.76180(11) 0.76821(10) 0.0205(5) Uani 1 1 d . . . . .
S4 S 0.12542(5) 0.39955(5) 0.92941(4) 0.0445(2) Uani 1 1 d . . . . .
O10 O 0.19664(13) 0.38609(13) 0.96179(13) 0.0527(6) Uani 1 1 d . . . . .
O11 O 0.11893(15) 0.38840(14) 0.85816(12) 0.0541(7) Uani 1 1 d . . . . .
O12 O 0.06089(15) 0.37643(18) 0.96623(15) 0.0779(10) Uani 1 1 d . . . . .
C3 C 0.1151(2) 0.4893(2) 0.93730(19) 0.0574(10) Uani 1 1 d . . . . .
F7 F 0.11964(16) 0.51075(13) 1.00152(11) 0.0755(7) Uani 1 1 d . . . . .
F9 F 0.16962(15) 0.52040(13) 0.90399(12) 0.0709(7) Uani 1 1 d . . . . .
F8 F 0.04828(14) 0.51056(14) 0.91107(12) 0.0776(8) Uani 1 1 d . . . . .
O7 O 0.43822(13) 0.36430(13) 0.59339(12) 0.0477(6) Uani 1 1 d . . . . .
O8 O 0.36395(14) 0.36274(12) 0.48717(12) 0.0473(6) Uani 1 1 d . . . . .
O9 O 0.30135(14) 0.35831(14) 0.59498(13) 0.0564(7) Uani 1 1 d . . . . .
F3 F 0.42026(13) 0.49673(11) 0.53151(11) 0.0588(6) Uani 1 1 d . . . . .
F2 F 0.36270(13) 0.49070(11) 0.62531(10) 0.0582(6) Uani 1 1 d . . . . .
F1 F 0.29886(13) 0.49172(12) 0.53118(12) 0.0642(6) Uani 1 1 d . . . . .
C1 C 0.36191(19) 0.46832(17) 0.56100(17) 0.0411(8) Uani 1 1 d . . . . .
C111 C 0.65288(14) 0.60293(14) 0.70285(13) 0.0232(6) Uani 1 1 d . . . . .
C115 C 0.54492(16) 0.54589(14) 0.66770(13) 0.0257(6) Uani 1 1 d . . . . .
H115 H 0.4913 0.5411 0.6675 0.031 Uiso 1 1 calc R U . . .
C114 C 0.58640(17) 0.49917(15) 0.63365(15) 0.0320(7) Uani 1 1 d . . . . .
H114 H 0.5617 0.4631 0.6108 0.038 Uiso 1 1 calc R U . . .
C112 C 0.69764(16) 0.55733(15) 0.66901(14) 0.0290(6) Uani 1 1 d . . . . .
H112 H 0.7513 0.5620 0.6707 0.035 Uiso 1 1 calc R U . . .
C113 C 0.66440(17) 0.50548(15) 0.63311(15) 0.0327(7) Uani 1 1 d . . . . .
H113 H 0.6943 0.4749 0.6087 0.039 Uiso 1 1 calc R U . . .
N11 N 0.57649(12) 0.59840(11) 0.70144(11) 0.0224(5) Uani 1 1 d . . . . .


_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 N2 1.985(2) . ?
Fe1 N4 1.990(2) . ?
Fe1 N6 2.003(2) . ?
Fe1 N5 2.004(2) . ?
Fe1 N1 2.006(2) . ?
Fe1 N3 2.008(2) . ?
Fe2 N8 1.989(2) . ?
Fe2 N12 1.991(2) . ?
Fe2 N9 1.996(2) . ?
Fe2 N11 1.999(2) . ?
Fe2 N10 2.000(2) . ?
Fe2 N7 2.002(2) . ?
P1 C21 1.830(3) . ?
P1 C31 1.832(3) . ?
P1 C11 1.832(3) . ?
P2 C41 1.828(3) . ?
P2 C61 1.834(3) . ?
P2 C51 1.837(3) . ?
P3 C91 1.826(3) . ?
P3 C71 1.830(3) . ?
P3 C81 1.833(3) . ?
P4 C101 1.827(3) . ?
P4 C111 1.831(3) . ?
P4 C121 1.832(3) . ?
S1 O2 1.438(2) . ?
S1 O3 1.439(2) . ?
S1 O1 1.442(2) . ?
S1 C4 1.824(4) . ?
N4 C45 1.347(4) . ?
N4 C41 1.362(3) . ?
C41 C42 1.386(4) . ?
C45 C44 1.380(4) . ?
C45 H45 0.9500 . ?
C44 C43 1.381(4) . ?
C44 H44 0.9500 . ?
C42 C43 1.383(4) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C55 N5 1.350(4) . ?
C55 C54 1.380(4) . ?
C55 H55 0.9500 . ?
C53 C54 1.378(4) . ?
C53 C52 1.383(4) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C51 N5 1.362(3) . ?
C51 C52 1.386(4) . ?
C52 H52 0.9500 . ?
N1 C15 1.349(3) . ?
N1 C11 1.358(3) . ?
N3 C35 1.350(3) . ?
N3 C31 1.362(3) . ?
C35 C34 1.379(4) . ?
C35 H35 0.9500 . ?
C15 C14 1.379(4) . ?
C15 H15 0.9500 . ?
C14 C13 1.384(4) . ?
C14 H14 0.9500 . ?
C32 C33 1.380(4) . ?
C32 C31 1.387(4) . ?
C32 H32 0.9500 . ?
C34 C33 1.381(4) . ?
C34 H34 0.9500 . ?
C12 C13 1.383(4) . ?
C12 C11 1.389(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C33 H33 0.9500 . ?
C75 N7 1.351(4) . ?
C75 C74 1.377(4) . ?
C75 H75 0.9500 . ?
N7 C71 1.357(3) . ?
C73 C74 1.381(4) . ?
C73 C72 1.382(4) . ?
C73 H73 0.9500 . ?
C74 H74 0.9500 . ?
C71 C72 1.386(4) . ?
C72 H72 0.9500 . ?
N8 C85 1.348(3) . ?
N8 C81 1.356(3) . ?
C83 C84 1.377(4) . ?
C83 C82 1.382(4) . ?
C83 H83 0.9500 . ?
C81 C82 1.386(4) . ?
C85 C84 1.379(4) . ?
C85 H85 0.9500 . ?
C82 H82 0.9500 . ?
C84 H84 0.9500 . ?
C102 C103 1.385(4) . ?
C102 C101 1.386(4) . ?
C102 H102 0.9500 . ?
C105 N10 1.349(3) . ?
C105 C104 1.384(4) . ?
C105 H105 0.9500 . ?
C104 C103 1.375(4) . ?
C104 H104 0.9500 . ?
C103 H103 0.9500 . ?
C101 N10 1.360(3) . ?
N9 C95 1.348(3) . ?
N9 C91 1.358(3) . ?
C95 C94 1.384(4) . ?
C95 H95 0.9500 . ?
C93 C94 1.376(4) . ?
C93 C92 1.380(4) . ?
C93 H93 0.9500 . ?
C94 H94 0.9500 . ?
C91 C92 1.386(4) . ?
C92 H92 0.9500 . ?
C125 N12 1.355(3) . ?
C125 C124 1.379(4) . ?
C125 H125 0.9500 . ?
C121 N12 1.360(3) . ?
C121 C122 1.379(4) . ?
C122 C123 1.382(4) . ?
C122 H122 0.9500 . ?
C123 C124 1.381(4) . ?
C123 H123 0.9500 . ?
C124 H124 0.9500 . ?
N6 C65 1.352(4) . ?
N6 C61 1.355(3) . ?
C61 C62 1.391(4) . ?
C65 C64 1.380(4) . ?
C65 H65 0.9500 . ?
C64 C63 1.376(4) . ?
C64 H64 0.9500 . ?
C63 C62 1.385(4) . ?
C63 H63 0.9500 . ?
C62 H62 0.9500 . ?
C4 F13 1.319(4) . ?
C4 F11 1.327(4) . ?
C4 F12 1.349(4) . ?
S2 O4 1.422(2) . ?
S2 O6 1.433(2) . ?
S2 O5 1.441(3) . ?
S2 C2 1.821(4) . ?
C2 F6 1.318(4) . ?
C2 F5 1.325(4) . ?
C2 F4 1.333(4) . ?
S3 O9 1.436(2) . ?
S3 O8 1.439(2) . ?
S3 O7 1.445(2) . ?
S3 C1 1.819(4) . ?
C25 N2 1.347(3) . ?
C25 C24 1.385(4) . ?
C25 H25 0.9500 . ?
C21 N2 1.356(3) . ?
C21 C22 1.391(4) . ?
C24 C23 1.380(4) . ?
C24 H24 0.9500 . ?
C22 C23 1.386(4) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
S4 O10 1.418(2) . ?
S4 O11 1.430(3) . ?
S4 O12 1.447(3) . ?
S4 C3 1.813(5) . ?
C3 F9 1.337(5) . ?
C3 F8 1.342(4) . ?
C3 F7 1.342(4) . ?
F3 C1 1.327(4) . ?
F2 C1 1.350(4) . ?
F1 C1 1.328(4) . ?
C111 N11 1.349(3) . ?
C111 C112 1.392(4) . ?
C115 N11 1.355(4) . ?
C115 C114 1.377(4) . ?
C115 H115 0.9500 . ?
C114 C113 1.382(4) . ?
C114 H114 0.9500 . ?
C112 C113 1.378(4) . ?
C112 H112 0.9500 . ?
C113 H113 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N4 87.42(9) . . ?
N2 Fe1 N6 87.60(9) . . ?
N4 Fe1 N6 92.64(9) . . ?
N2 Fe1 N5 177.03(9) . . ?
N4 Fe1 N5 91.77(9) . . ?
N6 Fe1 N5 89.58(9) . . ?
N2 Fe1 N1 92.94(9) . . ?
N4 Fe1 N1 87.57(9) . . ?
N6 Fe1 N1 179.43(9) . . ?
N5 Fe1 N1 89.89(9) . . ?
N2 Fe1 N3 91.24(9) . . ?
N4 Fe1 N3 176.75(9) . . ?
N6 Fe1 N3 90.26(9) . . ?
N5 Fe1 N3 89.71(9) . . ?
N1 Fe1 N3 89.55(9) . . ?
N8 Fe2 N12 179.93(11) . . ?
N8 Fe2 N9 91.73(9) . . ?
N12 Fe2 N9 88.31(9) . . ?
N8 Fe2 N11 88.23(9) . . ?
N12 Fe2 N11 91.73(9) . . ?
N9 Fe2 N11 179.75(10) . . ?
N8 Fe2 N10 88.12(9) . . ?
N12 Fe2 N10 91.93(9) . . ?
N9 Fe2 N10 87.95(9) . . ?
N11 Fe2 N10 91.80(9) . . ?
N8 Fe2 N7 91.95(9) . . ?
N12 Fe2 N7 87.99(9) . . ?
N9 Fe2 N7 91.90(9) . . ?
N11 Fe2 N7 88.35(9) . . ?
N10 Fe2 N7 179.83(10) . . ?
C21 P1 C31 97.28(12) . . ?
C21 P1 C11 101.63(12) . . ?
C31 P1 C11 96.91(12) . . ?
C41 P2 C61 100.58(12) . . ?
C41 P2 C51 98.01(12) . . ?
C61 P2 C51 97.96(12) . . ?
C91 P3 C71 97.32(12) . . ?
C91 P3 C81 100.08(12) . . ?
C71 P3 C81 100.84(12) . . ?
C101 P4 C111 97.74(12) . . ?
C101 P4 C121 100.24(12) . . ?
C111 P4 C121 100.68(12) . . ?
O2 S1 O3 114.61(14) . . ?
O2 S1 O1 115.45(14) . . ?
O3 S1 O1 115.36(15) . . ?
O2 S1 C4 102.40(15) . . ?
O3 S1 C4 102.54(16) . . ?
O1 S1 C4 103.85(15) . . ?
C45 N4 C41 117.1(2) . . ?
C45 N4 Fe1 120.24(18) . . ?
C41 N4 Fe1 122.57(18) . . ?
N4 C41 C42 121.9(3) . . ?
N4 C41 P2 120.5(2) . . ?
C42 C41 P2 117.6(2) . . ?
N4 C45 C44 123.4(3) . . ?
N4 C45 H45 118.3 . . ?
C44 C45 H45 118.3 . . ?
C45 C44 C43 119.3(3) . . ?
C45 C44 H44 120.4 . . ?
C43 C44 H44 120.4 . . ?
C43 C42 C41 120.1(3) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C44 C43 C42 118.1(3) . . ?
C44 C43 H43 120.9 . . ?
C42 C43 H43 120.9 . . ?
N5 C55 C54 123.7(3) . . ?
N5 C55 H55 118.1 . . ?
C54 C55 H55 118.1 . . ?
C54 C53 C52 118.6(3) . . ?
C54 C53 H53 120.7 . . ?
C52 C53 H53 120.7 . . ?
C53 C54 C55 119.1(3) . . ?
C53 C54 H54 120.5 . . ?
C55 C54 H54 120.5 . . ?
N5 C51 C52 122.5(3) . . ?
N5 C51 P2 120.5(2) . . ?
C52 C51 P2 117.0(2) . . ?
C53 C52 C51 119.5(3) . . ?
C53 C52 H52 120.2 . . ?
C51 C52 H52 120.2 . . ?
C15 N1 C11 117.1(2) . . ?
C15 N1 Fe1 120.32(17) . . ?
C11 N1 Fe1 122.56(17) . . ?
C35 N3 C31 116.8(2) . . ?
C35 N3 Fe1 121.03(18) . . ?
C31 N3 Fe1 122.13(18) . . ?
N3 C35 C34 123.7(3) . . ?
N3 C35 H35 118.2 . . ?
C34 C35 H35 118.2 . . ?
N1 C15 C14 123.6(3) . . ?
N1 C15 H15 118.2 . . ?
C14 C15 H15 118.2 . . ?
C15 C14 C13 119.1(3) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C33 C32 C31 119.7(3) . . ?
C33 C32 H32 120.1 . . ?
C31 C32 H32 120.1 . . ?
N3 C31 C32 122.2(2) . . ?
N3 C31 P1 120.7(2) . . ?
C32 C31 P1 117.1(2) . . ?
C35 C34 C33 119.0(3) . . ?
C35 C34 H34 120.5 . . ?
C33 C34 H34 120.5 . . ?
C13 C12 C11 120.0(3) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 118.2(3) . . ?
C12 C13 H13 120.9 . . ?
C14 C13 H13 120.9 . . ?
C32 C33 C34 118.6(3) . . ?
C32 C33 H33 120.7 . . ?
C34 C33 H33 120.7 . . ?
N1 C11 C12 122.0(2) . . ?
N1 C11 P1 120.45(19) . . ?
C12 C11 P1 117.5(2) . . ?
N7 C75 C74 123.8(3) . . ?
N7 C75 H75 118.1 . . ?
C74 C75 H75 118.1 . . ?
C75 N7 C71 116.8(2) . . ?
C75 N7 Fe2 120.95(18) . . ?
C71 N7 Fe2 121.97(18) . . ?
C74 C73 C72 118.4(3) . . ?
C74 C73 H73 120.8 . . ?
C72 C73 H73 120.8 . . ?
C75 C74 C73 118.9(3) . . ?
C75 C74 H74 120.6 . . ?
C73 C74 H74 120.6 . . ?
N7 C71 C72 122.1(3) . . ?
N7 C71 P3 119.9(2) . . ?
C72 C71 P3 117.9(2) . . ?
C73 C72 C71 119.8(3) . . ?
C73 C72 H72 120.1 . . ?
C71 C72 H72 120.1 . . ?
C85 N8 C81 117.2(2) . . ?
C85 N8 Fe2 121.06(17) . . ?
C81 N8 Fe2 121.73(17) . . ?
C84 C83 C82 118.4(3) . . ?
C84 C83 H83 120.8 . . ?
C82 C83 H83 120.8 . . ?
N8 C81 C82 121.8(2) . . ?
N8 C81 P3 120.55(19) . . ?
C82 C81 P3 117.7(2) . . ?
N8 C85 C84 123.6(2) . . ?
N8 C85 H85 118.2 . . ?
C84 C85 H85 118.2 . . ?
C83 C82 C81 120.0(3) . . ?
C83 C82 H82 120.0 . . ?
C81 C82 H82 120.0 . . ?
C83 C84 C85 118.9(3) . . ?
C83 C84 H84 120.5 . . ?
C85 C84 H84 120.5 . . ?
C103 C102 C101 119.6(3) . . ?
C103 C102 H102 120.2 . . ?
C101 C102 H102 120.2 . . ?
N10 C105 C104 123.6(3) . . ?
N10 C105 H105 118.2 . . ?
C104 C105 H105 118.2 . . ?
C103 C104 C105 119.0(3) . . ?
C103 C104 H104 120.5 . . ?
C105 C104 H104 120.5 . . ?
C104 C103 C102 118.6(3) . . ?
C104 C103 H103 120.7 . . ?
C102 C103 H103 120.7 . . ?
N10 C101 C102 122.3(2) . . ?
N10 C101 P4 119.8(2) . . ?
C102 C101 P4 117.9(2) . . ?
C95 N9 C91 117.2(2) . . ?
C95 N9 Fe2 120.32(17) . . ?
C91 N9 Fe2 122.41(18) . . ?
C105 N10 C101 116.8(2) . . ?
C105 N10 Fe2 121.07(17) . . ?
C101 N10 Fe2 122.10(18) . . ?
N9 C95 C94 123.1(2) . . ?
N9 C95 H95 118.5 . . ?
C94 C95 H95 118.5 . . ?
C94 C93 C92 118.8(3) . . ?
C94 C93 H93 120.6 . . ?
C92 C93 H93 120.6 . . ?
C93 C94 C95 119.2(3) . . ?
C93 C94 H94 120.4 . . ?
C95 C94 H94 120.4 . . ?
N9 C91 C92 122.2(2) . . ?
N9 C91 P3 119.72(19) . . ?
C92 C91 P3 118.0(2) . . ?
C93 C92 C91 119.5(3) . . ?
C93 C92 H92 120.2 . . ?
C91 C92 H92 120.2 . . ?
N12 C125 C124 123.5(3) . . ?
N12 C125 H125 118.2 . . ?
C124 C125 H125 118.2 . . ?
N12 C121 C122 121.8(3) . . ?
N12 C121 P4 120.14(19) . . ?
C122 C121 P4 118.0(2) . . ?
C121 C122 C123 120.4(3) . . ?
C121 C122 H122 119.8 . . ?
C123 C122 H122 119.8 . . ?
C124 C123 C122 118.2(3) . . ?
C124 C123 H123 120.9 . . ?
C122 C123 H123 120.9 . . ?
C125 C124 C123 119.0(3) . . ?
C125 C124 H124 120.5 . . ?
C123 C124 H124 120.5 . . ?
C125 N12 C121 117.0(2) . . ?
C125 N12 Fe2 121.09(18) . . ?
C121 N12 Fe2 121.91(18) . . ?
C65 N6 C61 117.0(2) . . ?
C65 N6 Fe1 120.50(17) . . ?
C61 N6 Fe1 122.50(18) . . ?
N6 C61 C62 122.2(2) . . ?
N6 C61 P2 120.5(2) . . ?
C62 C61 P2 117.3(2) . . ?
N6 C65 C64 123.7(3) . . ?
N6 C65 H65 118.2 . . ?
C64 C65 H65 118.2 . . ?
C63 C64 C65 118.8(3) . . ?
C63 C64 H64 120.6 . . ?
C65 C64 H64 120.6 . . ?
C64 C63 C62 118.9(3) . . ?
C64 C63 H63 120.6 . . ?
C62 C63 H63 120.6 . . ?
C63 C62 C61 119.4(3) . . ?
C63 C62 H62 120.3 . . ?
C61 C62 H62 120.3 . . ?
F13 C4 F11 107.2(3) . . ?
F13 C4 F12 107.1(3) . . ?
F11 C4 F12 106.5(3) . . ?
F13 C4 S1 112.3(3) . . ?
F11 C4 S1 112.3(2) . . ?
F12 C4 S1 111.0(2) . . ?
O4 S2 O6 115.41(15) . . ?
O4 S2 O5 114.07(19) . . ?
O6 S2 O5 115.29(19) . . ?
O4 S2 C2 103.65(15) . . ?
O6 S2 C2 103.22(17) . . ?
O5 S2 C2 102.84(16) . . ?
F6 C2 F5 109.2(3) . . ?
F6 C2 F4 106.6(3) . . ?
F5 C2 F4 105.9(3) . . ?
F6 C2 S2 111.4(2) . . ?
F5 C2 S2 111.2(2) . . ?
F4 C2 S2 112.3(2) . . ?
O9 S3 O8 115.95(16) . . ?
O9 S3 O7 114.14(15) . . ?
O8 S3 O7 115.80(15) . . ?
O9 S3 C1 102.37(16) . . ?
O8 S3 C1 103.61(15) . . ?
O7 S3 C1 102.14(16) . . ?
C55 N5 C51 116.6(2) . . ?
C55 N5 Fe1 121.19(18) . . ?
C51 N5 Fe1 122.24(18) . . ?
N2 C25 C24 123.2(3) . . ?
N2 C25 H25 118.4 . . ?
C24 C25 H25 118.4 . . ?
N2 C21 C22 121.7(2) . . ?
N2 C21 P1 121.12(19) . . ?
C22 C21 P1 117.1(2) . . ?
C23 C24 C25 119.2(3) . . ?
C23 C24 H24 120.4 . . ?
C25 C24 H24 120.4 . . ?
C23 C22 C21 119.9(3) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C24 C23 C22 118.2(3) . . ?
C24 C23 H23 120.9 . . ?
C22 C23 H23 120.9 . . ?
C25 N2 C21 117.5(2) . . ?
C25 N2 Fe1 120.05(18) . . ?
C21 N2 Fe1 122.19(18) . . ?
O10 S4 O11 117.31(17) . . ?
O10 S4 O12 114.25(16) . . ?
O11 S4 O12 114.10(17) . . ?
O10 S4 C3 103.84(18) . . ?
O11 S4 C3 103.57(17) . . ?
O12 S4 C3 101.0(2) . . ?
F9 C3 F8 107.3(3) . . ?
F9 C3 F7 107.3(4) . . ?
F8 C3 F7 106.9(3) . . ?
F9 C3 S4 110.1(3) . . ?
F8 C3 S4 111.7(3) . . ?
F7 C3 S4 113.3(3) . . ?
F3 C1 F1 107.6(3) . . ?
F3 C1 F2 106.8(3) . . ?
F1 C1 F2 106.6(3) . . ?
F3 C1 S3 112.1(2) . . ?
F1 C1 S3 112.2(2) . . ?
F2 C1 S3 111.1(2) . . ?
N11 C111 C112 121.8(3) . . ?
N11 C111 P4 119.8(2) . . ?
C112 C111 P4 118.4(2) . . ?
N11 C115 C114 123.5(3) . . ?
N11 C115 H115 118.3 . . ?
C114 C115 H115 118.2 . . ?
C115 C114 C113 119.1(3) . . ?
C115 C114 H114 120.5 . . ?
C113 C114 H114 120.5 . . ?
C113 C112 C111 120.2(3) . . ?
C113 C112 H112 119.9 . . ?
C111 C112 H112 119.9 . . ?
C112 C113 C114 118.1(3) . . ?
C112 C113 H113 120.9 . . ?
C114 C113 H113 120.9 . . ?
C111 N11 C115 117.1(2) . . ?
C111 N11 Fe2 122.43(19) . . ?
C115 N11 Fe2 120.30(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C45 N4 C41 C42 3.5(4) . . . . ?
Fe1 N4 C41 C42 -173.4(2) . . . . ?
C45 N4 C41 P2 -178.02(19) . . . . ?
Fe1 N4 C41 P2 5.1(3) . . . . ?
C61 P2 C41 N4 45.8(2) . . . . ?
C51 P2 C41 N4 -53.9(2) . . . . ?
C61 P2 C41 C42 -135.7(2) . . . . ?
C51 P2 C41 C42 124.6(2) . . . . ?
C41 N4 C45 C44 -2.5(4) . . . . ?
Fe1 N4 C45 C44 174.5(2) . . . . ?
N4 C45 C44 C43 -0.6(4) . . . . ?
N4 C41 C42 C43 -1.5(4) . . . . ?
P2 C41 C42 C43 180.0(2) . . . . ?
C45 C44 C43 C42 2.7(4) . . . . ?
C41 C42 C43 C44 -1.7(4) . . . . ?
C52 C53 C54 C55 -2.0(4) . . . . ?
N5 C55 C54 C53 1.2(4) . . . . ?
C41 P2 C51 N5 50.6(2) . . . . ?
C61 P2 C51 N5 -51.4(2) . . . . ?
C41 P2 C51 C52 -128.4(2) . . . . ?
C61 P2 C51 C52 129.7(2) . . . . ?
C54 C53 C52 C51 1.1(4) . . . . ?
N5 C51 C52 C53 0.6(4) . . . . ?
P2 C51 C52 C53 179.5(2) . . . . ?
C31 N3 C35 C34 -1.0(4) . . . . ?
Fe1 N3 C35 C34 176.8(2) . . . . ?
C11 N1 C15 C14 0.7(4) . . . . ?
Fe1 N1 C15 C14 179.9(2) . . . . ?
N1 C15 C14 C13 -1.2(4) . . . . ?
C35 N3 C31 C32 1.3(4) . . . . ?
Fe1 N3 C31 C32 -176.38(19) . . . . ?
C35 N3 C31 P1 -178.05(19) . . . . ?
Fe1 N3 C31 P1 4.2(3) . . . . ?
C33 C32 C31 N3 -1.5(4) . . . . ?
C33 C32 C31 P1 177.9(2) . . . . ?
C21 P1 C31 N3 48.3(2) . . . . ?
C11 P1 C31 N3 -54.5(2) . . . . ?
C21 P1 C31 C32 -131.2(2) . . . . ?
C11 P1 C31 C32 126.1(2) . . . . ?
N3 C35 C34 C33 0.7(4) . . . . ?
C11 C12 C13 C14 0.2(4) . . . . ?
C15 C14 C13 C12 0.7(4) . . . . ?
C31 C32 C33 C34 1.2(4) . . . . ?
C35 C34 C33 C32 -0.8(4) . . . . ?
C15 N1 C11 C12 0.3(4) . . . . ?
Fe1 N1 C11 C12 -178.9(2) . . . . ?
C15 N1 C11 P1 -177.22(19) . . . . ?
Fe1 N1 C11 P1 3.6(3) . . . . ?
C13 C12 C11 N1 -0.7(4) . . . . ?
C13 C12 C11 P1 176.9(2) . . . . ?
C21 P1 C11 N1 -49.0(2) . . . . ?
C31 P1 C11 N1 50.0(2) . . . . ?
C21 P1 C11 C12 133.4(2) . . . . ?
C31 P1 C11 C12 -127.6(2) . . . . ?
C74 C75 N7 C71 -2.5(4) . . . . ?
C74 C75 N7 Fe2 171.8(2) . . . . ?
N7 C75 C74 C73 -0.7(4) . . . . ?
C72 C73 C74 C75 3.2(4) . . . . ?
C75 N7 C71 C72 3.1(4) . . . . ?
Fe2 N7 C71 C72 -171.1(2) . . . . ?
C75 N7 C71 P3 -179.99(19) . . . . ?
Fe2 N7 C71 P3 5.8(3) . . . . ?
C91 P3 C71 N7 -56.1(2) . . . . ?
C81 P3 C71 N7 45.7(2) . . . . ?
C91 P3 C71 C72 121.0(2) . . . . ?
C81 P3 C71 C72 -137.2(2) . . . . ?
C74 C73 C72 C71 -2.6(4) . . . . ?
N7 C71 C72 C73 -0.6(4) . . . . ?
P3 C71 C72 C73 -177.6(2) . . . . ?
C85 N8 C81 C82 -0.4(4) . . . . ?
Fe2 N8 C81 C82 -179.5(2) . . . . ?
C85 N8 C81 P3 179.13(19) . . . . ?
Fe2 N8 C81 P3 0.1(3) . . . . ?
C91 P3 C81 N8 50.1(2) . . . . ?
C71 P3 C81 N8 -49.4(2) . . . . ?
C91 P3 C81 C82 -130.4(2) . . . . ?
C71 P3 C81 C82 130.1(2) . . . . ?
C81 N8 C85 C84 -0.2(4) . . . . ?
Fe2 N8 C85 C84 178.9(2) . . . . ?
C84 C83 C82 C81 -0.3(4) . . . . ?
N8 C81 C82 C83 0.7(4) . . . . ?
P3 C81 C82 C83 -178.9(2) . . . . ?
C82 C83 C84 C85 -0.2(4) . . . . ?
N8 C85 C84 C83 0.5(4) . . . . ?
N10 C105 C104 C103 1.2(4) . . . . ?
C105 C104 C103 C102 -2.3(4) . . . . ?
C101 C102 C103 C104 1.2(4) . . . . ?
C103 C102 C101 N10 1.2(4) . . . . ?
C103 C102 C101 P4 -179.9(2) . . . . ?
C111 P4 C101 N10 54.3(2) . . . . ?
C121 P4 C101 N10 -48.1(2) . . . . ?
C111 P4 C101 C102 -124.6(2) . . . . ?
C121 P4 C101 C102 133.0(2) . . . . ?
C104 C105 N10 C101 1.1(4) . . . . ?
C104 C105 N10 Fe2 -176.7(2) . . . . ?
C102 C101 N10 C105 -2.3(4) . . . . ?
P4 C101 N10 C105 178.85(19) . . . . ?
C102 C101 N10 Fe2 175.48(19) . . . . ?
P4 C101 N10 Fe2 -3.3(3) . . . . ?
C91 N9 C95 C94 1.3(4) . . . . ?
Fe2 N9 C95 C94 -175.8(2) . . . . ?
C92 C93 C94 C95 -2.4(4) . . . . ?
N9 C95 C94 C93 1.1(4) . . . . ?
C95 N9 C91 C92 -2.4(4) . . . . ?
Fe2 N9 C91 C92 174.67(19) . . . . ?
C95 N9 C91 P3 179.67(19) . . . . ?
Fe2 N9 C91 P3 -3.3(3) . . . . ?
C71 P3 C91 N9 54.6(2) . . . . ?
C81 P3 C91 N9 -47.9(2) . . . . ?
C71 P3 C91 C92 -123.5(2) . . . . ?
C81 P3 C91 C92 134.0(2) . . . . ?
C94 C93 C92 C91 1.4(4) . . . . ?
N9 C91 C92 C93 1.0(4) . . . . ?
P3 C91 C92 C93 179.0(2) . . . . ?
C101 P4 C121 N12 50.8(2) . . . . ?
C111 P4 C121 N12 -49.2(2) . . . . ?
C101 P4 C121 C122 -130.8(2) . . . . ?
C111 P4 C121 C122 129.2(2) . . . . ?
N12 C121 C122 C123 1.2(5) . . . . ?
P4 C121 C122 C123 -177.2(2) . . . . ?
C121 C122 C123 C124 -1.5(5) . . . . ?
N12 C125 C124 C123 2.0(5) . . . . ?
C122 C123 C124 C125 0.0(5) . . . . ?
C124 C125 N12 C121 -2.3(4) . . . . ?
C124 C125 N12 Fe2 177.6(2) . . . . ?
C122 C121 N12 C125 0.7(4) . . . . ?
P4 C121 N12 C125 179.1(2) . . . . ?
C122 C121 N12 Fe2 -179.2(2) . . . . ?
P4 C121 N12 Fe2 -0.8(3) . . . . ?
C65 N6 C61 C62 1.1(4) . . . . ?
Fe1 N6 C61 C62 -176.9(2) . . . . ?
C65 N6 C61 P2 -177.67(19) . . . . ?
Fe1 N6 C61 P2 4.4(3) . . . . ?
C41 P2 C61 N6 -51.1(2) . . . . ?
C51 P2 C61 N6 48.7(2) . . . . ?
C41 P2 C61 C62 130.1(2) . . . . ?
C51 P2 C61 C62 -130.2(2) . . . . ?
C61 N6 C65 C64 0.0(4) . . . . ?
Fe1 N6 C65 C64 178.0(2) . . . . ?
N6 C65 C64 C63 -1.3(5) . . . . ?
C65 C64 C63 C62 1.5(5) . . . . ?
C64 C63 C62 C61 -0.5(5) . . . . ?
N6 C61 C62 C63 -0.9(4) . . . . ?
P2 C61 C62 C63 177.9(2) . . . . ?
O2 S1 C4 F13 179.8(2) . . . . ?
O3 S1 C4 F13 -61.1(3) . . . . ?
O1 S1 C4 F13 59.3(3) . . . . ?
O2 S1 C4 F11 58.9(3) . . . . ?
O3 S1 C4 F11 177.9(2) . . . . ?
O1 S1 C4 F11 -61.6(3) . . . . ?
O2 S1 C4 F12 -60.3(3) . . . . ?
O3 S1 C4 F12 58.8(3) . . . . ?
O1 S1 C4 F12 179.2(2) . . . . ?
O4 S2 C2 F6 57.8(3) . . . . ?
O6 S2 C2 F6 -62.9(3) . . . . ?
O5 S2 C2 F6 176.9(3) . . . . ?
O4 S2 C2 F5 179.9(3) . . . . ?
O6 S2 C2 F5 59.2(3) . . . . ?
O5 S2 C2 F5 -61.0(3) . . . . ?
O4 S2 C2 F4 -61.7(3) . . . . ?
O6 S2 C2 F4 177.6(2) . . . . ?
O5 S2 C2 F4 57.4(3) . . . . ?
C54 C55 N5 C51 0.5(4) . . . . ?
C54 C55 N5 Fe1 179.7(2) . . . . ?
C52 C51 N5 C55 -1.4(4) . . . . ?
P2 C51 N5 C55 179.72(19) . . . . ?
C52 C51 N5 Fe1 179.4(2) . . . . ?
P2 C51 N5 Fe1 0.5(3) . . . . ?
C31 P1 C21 N2 -55.9(2) . . . . ?
C11 P1 C21 N2 42.7(2) . . . . ?
C31 P1 C21 C22 121.2(2) . . . . ?
C11 P1 C21 C22 -140.1(2) . . . . ?
N2 C25 C24 C23 -0.4(4) . . . . ?
N2 C21 C22 C23 -2.3(4) . . . . ?
P1 C21 C22 C23 -179.4(2) . . . . ?
C25 C24 C23 C22 3.4(4) . . . . ?
C21 C22 C23 C24 -2.1(4) . . . . ?
C24 C25 N2 C21 -3.9(4) . . . . ?
C24 C25 N2 Fe1 170.3(2) . . . . ?
C22 C21 N2 C25 5.2(4) . . . . ?
P1 C21 N2 C25 -177.76(19) . . . . ?
C22 C21 N2 Fe1 -168.8(2) . . . . ?
P1 C21 N2 Fe1 8.2(3) . . . . ?
O10 S4 C3 F9 63.2(3) . . . . ?
O11 S4 C3 F9 -59.8(3) . . . . ?
O12 S4 C3 F9 -178.2(3) . . . . ?
O10 S4 C3 F8 -177.7(3) . . . . ?
O11 S4 C3 F8 59.3(3) . . . . ?
O12 S4 C3 F8 -59.1(3) . . . . ?
O10 S4 C3 F7 -56.8(3) . . . . ?
O11 S4 C3 F7 -179.9(3) . . . . ?
O12 S4 C3 F7 61.8(3) . . . . ?
O9 S3 C1 F3 177.5(2) . . . . ?
O8 S3 C1 F3 -61.6(3) . . . . ?
O7 S3 C1 F3 59.1(3) . . . . ?
O9 S3 C1 F1 -61.2(3) . . . . ?
O8 S3 C1 F1 59.7(3) . . . . ?
O7 S3 C1 F1 -179.6(2) . . . . ?
O9 S3 C1 F2 58.1(3) . . . . ?
O8 S3 C1 F2 179.0(2) . . . . ?
O7 S3 C1 F2 -60.3(3) . . . . ?
C101 P4 C111 N11 -54.9(2) . . . . ?
C121 P4 C111 N11 47.2(2) . . . . ?
C101 P4 C111 C112 122.8(2) . . . . ?
C121 P4 C111 C112 -135.2(2) . . . . ?
N11 C115 C114 C113 -0.3(4) . . . . ?
N11 C111 C112 C113 -0.4(4) . . . . ?
P4 C111 C112 C113 -178.0(2) . . . . ?
C111 C112 C113 C114 -2.0(4) . . . . ?
C115 C114 C113 C112 2.3(4) . . . . ?
C112 C111 N11 C115 2.4(4) . . . . ?
P4 C111 N11 C115 180.00(19) . . . . ?
C112 C111 N11 Fe2 -173.4(2) . . . . ?
P4 C111 N11 Fe2 4.2(3) . . . . ?
C114 C115 N11 C111 -2.1(4) . . . . ?
C114 C115 N11 Fe2 173.8(2) . . . . ?

####################################################################### 
# 
# 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_toluene
_database_code_depnum_ccdc_archive 'CCDC 1431709'
_audit_update_record             
;
2015-10-16 deposited with the CCDC.
2015-11-16 downloaded from the CCDC.
;
#_cambridge_data_id DW_B2_0023
#===============================================================================
_audit_creation_method           SHELXL-2013

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H18 Cl2 Fe N3 P, C7 H8'
_chemical_formula_sum            'C25 H26 Cl2 Fe N3 P'
_chemical_formula_weight         526.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0155(3)
_cell_length_b                   10.7101(4)
_cell_length_c                   15.0458(6)
_cell_angle_alpha                98.595(2)
_cell_angle_beta                 99.108(2)
_cell_angle_gamma                91.742(2)
_cell_volume                     1259.09(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    8640
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      66.78

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_F_000             544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    7.489
_shelx_estimated_absorpt_T_min   0.420
_shelx_estimated_absorpt_T_max   0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5452
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14375
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.011
_diffrn_reflns_theta_max         66.774
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             4367
_reflns_number_gt                3618
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.

_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0302P)²+1.5774P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4367
_refine_ls_number_parameters     304
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0921
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.066

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.10710(6) 0.90358(5) 0.24823(3) 0.02371(14) Uani 1 1 d . . . . .
Cl1 Cl -0.06199(11) 0.73232(8) 0.18591(6) 0.0412(2) Uani 1 1 d . . . . .
Cl2 Cl 0.04346(10) 1.07099(8) 0.34862(5) 0.0344(2) Uani 1 1 d . . . . .
P1 P 0.50105(10) 0.88898(8) 0.17253(6) 0.02534(19) Uani 1 1 d . . . . .
N1 N 0.3397(3) 0.8596(2) 0.32189(17) 0.0253(6) Uani 1 1 d . . . . .
N2 N 0.1841(3) 0.9989(2) 0.14739(16) 0.0204(5) Uani 1 1 d . . . . .
N3 N 0.3380(3) 0.7282(2) 0.02829(18) 0.0277(6) Uani 1 1 d . . . . .
C11 C 0.4882(4) 0.8823(3) 0.2927(2) 0.0252(7) Uani 1 1 d . . . . .
C12 C 0.6418(4) 0.8876(3) 0.3500(2) 0.0349(8) Uani 1 1 d . . . . .
H12 H 0.7438 0.9064 0.3288 0.042 Uiso 1 1 calc R U . . .
C13 C 0.6457(5) 0.8652(3) 0.4388(3) 0.0435(10) Uani 1 1 d . . . . .
H13 H 0.7501 0.8689 0.4794 0.052 Uiso 1 1 calc R U . . .
C14 C 0.4968(5) 0.8377(3) 0.4667(2) 0.0403(9) Uani 1 1 d . . . . .
H14 H 0.4976 0.8201 0.5268 0.048 Uiso 1 1 calc R U . . .
C15 C 0.3433(4) 0.8351(3) 0.4078(2) 0.0310(8) Uani 1 1 d . . . . .
C16 C 0.1794(5) 0.8030(4) 0.4366(3) 0.0456(10) Uani 1 1 d . . . . .
H16A H 0.1297 0.8809 0.4606 0.068 Uiso 1 1 calc R U . . .
H16B H 0.1995 0.7492 0.4841 0.068 Uiso 1 1 calc R U . . .
H16C H 0.1015 0.7577 0.3841 0.068 Uiso 1 1 calc R U . . .
C21 C 0.3476(4) 1.0022(3) 0.1337(2) 0.0209(6) Uani 1 1 d . . . . .
C22 C 0.4075(4) 1.0887(3) 0.0851(2) 0.0258(7) Uani 1 1 d . . . . .
H22 H 0.5234 1.0917 0.0784 0.031 Uiso 1 1 calc R U . . .
C23 C 0.2987(4) 1.1708(3) 0.0463(2) 0.0303(8) Uani 1 1 d . . . . .
H23 H 0.3385 1.2304 0.0126 0.036 Uiso 1 1 calc R U . . .
C24 C 0.1323(4) 1.1643(3) 0.0573(2) 0.0297(8) Uani 1 1 d . . . . .
H24 H 0.0547 1.2181 0.0299 0.036 Uiso 1 1 calc R U . . .
C25 C 0.0775(4) 1.0788(3) 0.1088(2) 0.0231(7) Uani 1 1 d . . . . .
C26 C -0.1031(4) 1.0720(3) 0.1234(2) 0.0308(8) Uani 1 1 d . . . . .
H26A H -0.1377 0.9844 0.1265 0.046 Uiso 1 1 calc R U . . .
H26B H -0.1756 1.1011 0.0726 0.046 Uiso 1 1 calc R U . . .
H26C H -0.1141 1.1260 0.1806 0.046 Uiso 1 1 calc R U . . .
C31 C 0.3921(4) 0.7359(3) 0.1184(2) 0.0246(7) Uani 1 1 d . . . . .
C32 C 0.3888(5) 0.6327(3) 0.1634(2) 0.0403(9) Uani 1 1 d . . . . .
H32 H 0.4322 0.6404 0.2266 0.048 Uiso 1 1 calc R U . . .
C33 C 0.3210(6) 0.5181(3) 0.1144(3) 0.0503(11) Uani 1 1 d . . . . .
H33 H 0.3152 0.4458 0.1438 0.060 Uiso 1 1 calc R U . . .
C34 C 0.2622(5) 0.5095(3) 0.0228(3) 0.0437(10) Uani 1 1 d . . . . .
H34 H 0.2135 0.4318 -0.0117 0.052 Uiso 1 1 calc R U . . .
C35 C 0.2749(5) 0.6159(3) -0.0187(2) 0.0324(8) Uani 1 1 d . . . . .
C36 C 0.2213(6) 0.6072(3) -0.1194(2) 0.0519(11) Uani 1 1 d . . . . .
H36A H 0.1040 0.6314 -0.1322 0.078 Uiso 1 1 calc R U . . .
H36B H 0.2297 0.5202 -0.1490 0.078 Uiso 1 1 calc R U . . .
H36C H 0.2950 0.6644 -0.1431 0.078 Uiso 1 1 calc R U . . .
C2T C 0.4010(7) 0.3983(5) 0.3439(3) 0.0638(13) Uani 1 1 d . . . . .
H2T H 0.2858 0.4170 0.3434 0.077 Uiso 0.258(10) 1 calc R U P A 2
C1T C 0.2263(10) 0.4289(8) 0.3422(6) 0.094(3) Uani 0.742(10) 1 d . . P A 1
H1T1 H 0.1977 0.4894 0.3001 0.141 Uiso 0.742(10) 1 calc R U P A 1
H1T2 H 0.2097 0.4663 0.4035 0.141 Uiso 0.742(10) 1 calc R U P A 1
H1T3 H 0.1530 0.3517 0.3219 0.141 Uiso 0.742(10) 1 calc R U P A 1
C3T C 0.5330(8) 0.4913(4) 0.3795(3) 0.0742(16) Uani 1 1 d . . . . .
H3T H 0.5080 0.5742 0.4042 0.089 Uiso 1 1 calc R U . . .
C4T C 0.6980(8) 0.4608(6) 0.3781(4) 0.0788(16) Uani 1 1 d . . . . .
H4T H 0.7866 0.5239 0.4008 0.095 Uiso 0.742(10) 1 calc R U P A 1
C1T' C 0.832(4) 0.548(3) 0.407(2) 0.142(13) Uani 0.258(10) 1 d . U P A 2
H1T4 H 0.8378 0.5806 0.4714 0.214 Uiso 0.258(10) 1 calc R U P A 2
H1T5 H 0.8172 0.6182 0.3714 0.214 Uiso 0.258(10) 1 calc R U P A 2
H1T6 H 0.9376 0.5079 0.3970 0.214 Uiso 0.258(10) 1 calc R U P A 2
C5T C 0.7363(8) 0.3433(6) 0.3452(3) 0.0725(15) Uani 1 1 d . . . . .
H5T H 0.8511 0.3232 0.3459 0.087 Uiso 1 1 calc R U . . .
C6T C 0.6106(7) 0.2544(5) 0.3113(3) 0.0616(13) Uani 1 1 d . . . . .
H6T H 0.6385 0.1718 0.2877 0.074 Uiso 1 1 calc R U . . .
C7T C 0.4455(7) 0.2794(4) 0.3101(3) 0.0545(12) Uani 1 1 d . . . . .
H7T H 0.3599 0.2146 0.2856 0.065 Uiso 1 1 calc R 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 N2 2.108(2) . ?
Fe1 N1 2.117(3) . ?
Fe1 Cl1 2.2390(9) . ?
Fe1 Cl2 2.2905(9) . ?
P1 C11 1.838(3) . ?
P1 C21 1.844(3) . ?
P1 C31 1.845(3) . ?
N1 C15 1.352(4) . ?
N1 C11 1.360(4) . ?
N2 C25 1.355(4) . ?
N2 C21 1.359(4) . ?
N3 C35 1.341(4) . ?
N3 C31 1.345(4) . ?
C11 C12 1.381(4) . ?
C12 C13 1.389(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.365(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.395(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.494(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 C22 1.382(4) . ?
C22 C23 1.383(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.371(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.387(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.500(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C31 C32 1.382(4) . ?
C32 C33 1.381(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.372(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.387(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.497(5) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C2T C7T 1.378(6) . ?
C2T C3T 1.413(7) . ?
C2T C1T 1.445(8) . ?
C2T H2T 0.9500 . ?
C1T H1T1 0.9800 . ?
C1T H1T2 0.9800 . ?
C1T H1T3 0.9800 . ?
C3T C4T 1.374(8) . ?
C3T H3T 0.9500 . ?
C4T C5T 1.344(7) . ?
C4T C1T' 1.37(3) . ?
C4T H4T 0.9500 . ?
C1T' H1T4 0.9800 . ?
C1T' H1T5 0.9800 . ?
C1T' H1T6 0.9800 . ?
C5T C6T 1.348(7) . ?
C5T H5T 0.9500 . ?
C6T C7T 1.356(6) . ?
C6T H6T 0.9500 . ?
C7T H7T 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N1 102.90(10) . . ?
N2 Fe1 Cl1 111.32(7) . . ?
N1 Fe1 Cl1 113.18(7) . . ?
N2 Fe1 Cl2 100.61(7) . . ?
N1 Fe1 Cl2 99.22(7) . . ?
Cl1 Fe1 Cl2 126.55(4) . . ?
C11 P1 C21 107.26(14) . . ?
C11 P1 C31 100.22(14) . . ?
C21 P1 C31 101.93(13) . . ?
C15 N1 C11 119.1(3) . . ?
C15 N1 Fe1 118.6(2) . . ?
C11 N1 Fe1 120.7(2) . . ?
C25 N2 C21 118.6(3) . . ?
C25 N2 Fe1 118.7(2) . . ?
C21 N2 Fe1 121.4(2) . . ?
C35 N3 C31 118.1(3) . . ?
N1 C11 C12 121.6(3) . . ?
N1 C11 P1 122.7(2) . . ?
C12 C11 P1 115.3(3) . . ?
C11 C12 C13 119.4(3) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C14 C13 C12 118.7(3) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 120.6(3) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
N1 C15 C14 120.5(3) . . ?
N1 C15 C16 118.2(3) . . ?
C14 C15 C16 121.3(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C21 C22 121.3(3) . . ?
N2 C21 P1 123.3(2) . . ?
C22 C21 P1 115.4(2) . . ?
C21 C22 C23 120.0(3) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 118.7(3) . . ?
C24 C23 H23 120.7 . . ?
C22 C23 H23 120.7 . . ?
C23 C24 C25 119.8(3) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
N2 C25 C24 121.6(3) . . ?
N2 C25 C26 117.7(3) . . ?
C24 C25 C26 120.7(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C31 C32 122.7(3) . . ?
N3 C31 P1 114.0(2) . . ?
C32 C31 P1 122.6(3) . . ?
C33 C32 C31 118.5(3) . . ?
C33 C32 H32 120.8 . . ?
C31 C32 H32 120.8 . . ?
C34 C33 C32 119.3(3) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C35 119.1(3) . . ?
C33 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
N3 C35 C34 122.1(3) . . ?
N3 C35 C36 117.7(3) . . ?
C34 C35 C36 120.2(3) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C7T C2T C3T 117.6(5) . . ?
C7T C2T C1T 121.9(6) . . ?
C3T C2T C1T 120.5(6) . . ?
C7T C2T H2T 121.2 . . ?
C3T C2T H2T 121.2 . . ?
C2T C1T H1T1 109.5 . . ?
C2T C1T H1T2 109.5 . . ?
H1T1 C1T H1T2 109.5 . . ?
C2T C1T H1T3 109.5 . . ?
H1T1 C1T H1T3 109.5 . . ?
H1T2 C1T H1T3 109.5 . . ?
C4T C3T C2T 119.4(5) . . ?
C4T C3T H3T 120.3 . . ?
C2T C3T H3T 120.3 . . ?
C5T C4T C3T 121.3(5) . . ?
C5T C4T C1T' 116.1(16) . . ?
C3T C4T C1T' 122.6(16) . . ?
C5T C4T H4T 119.4 . . ?
C3T C4T H4T 119.4 . . ?
C4T C1T' H1T4 109.5 . . ?
C4T C1T' H1T5 109.5 . . ?
H1T4 C1T' H1T5 109.5 . . ?
C4T C1T' H1T6 109.5 . . ?
H1T4 C1T' H1T6 109.5 . . ?
H1T5 C1T' H1T6 109.5 . . ?
C4T C5T C6T 119.4(6) . . ?
C4T C5T H5T 120.3 . . ?
C6T C5T H5T 120.3 . . ?
C5T C6T C7T 121.9(5) . . ?
C5T C6T H6T 119.1 . . ?
C7T C6T H6T 119.1 . . ?
C6T C7T C2T 120.4(5) . . ?
C6T C7T H7T 119.8 . . ?
C2T C7T H7T 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 N1 C11 C12 -3.5(4) . . . . ?
Fe1 N1 C11 C12 162.1(2) . . . . ?
C15 N1 C11 P1 169.0(2) . . . . ?
Fe1 N1 C11 P1 -25.4(3) . . . . ?
C21 P1 C11 N1 52.6(3) . . . . ?
C31 P1 C11 N1 -53.4(3) . . . . ?
C21 P1 C11 C12 -134.4(2) . . . . ?
C31 P1 C11 C12 119.6(3) . . . . ?
N1 C11 C12 C13 2.1(5) . . . . ?
P1 C11 C12 C13 -170.9(3) . . . . ?
C11 C12 C13 C14 0.4(5) . . . . ?
C12 C13 C14 C15 -1.5(5) . . . . ?
C11 N1 C15 C14 2.3(4) . . . . ?
Fe1 N1 C15 C14 -163.6(2) . . . . ?
C11 N1 C15 C16 -176.4(3) . . . . ?
Fe1 N1 C15 C16 17.7(4) . . . . ?
C13 C14 C15 N1 0.2(5) . . . . ?
C13 C14 C15 C16 178.9(3) . . . . ?
C25 N2 C21 C22 2.9(4) . . . . ?
Fe1 N2 C21 C22 -163.6(2) . . . . ?
C25 N2 C21 P1 -173.9(2) . . . . ?
Fe1 N2 C21 P1 19.6(3) . . . . ?
C11 P1 C21 N2 -49.2(3) . . . . ?
C31 P1 C21 N2 55.6(3) . . . . ?
C11 P1 C21 C22 133.8(2) . . . . ?
C31 P1 C21 C22 -121.4(2) . . . . ?
N2 C21 C22 C23 -2.5(4) . . . . ?
P1 C21 C22 C23 174.5(2) . . . . ?
C21 C22 C23 C24 0.1(5) . . . . ?
C22 C23 C24 C25 1.7(5) . . . . ?
C21 N2 C25 C24 -1.0(4) . . . . ?
Fe1 N2 C25 C24 165.9(2) . . . . ?
C21 N2 C25 C26 179.0(3) . . . . ?
Fe1 N2 C25 C26 -14.2(3) . . . . ?
C23 C24 C25 N2 -1.4(5) . . . . ?
C23 C24 C25 C26 178.7(3) . . . . ?
C35 N3 C31 C32 1.6(5) . . . . ?
C35 N3 C31 P1 172.5(2) . . . . ?
C11 P1 C31 N3 161.8(2) . . . . ?
C21 P1 C31 N3 51.5(3) . . . . ?
C11 P1 C31 C32 -27.3(3) . . . . ?
C21 P1 C31 C32 -137.6(3) . . . . ?
N3 C31 C32 C33 -2.6(6) . . . . ?
P1 C31 C32 C33 -172.7(3) . . . . ?
C31 C32 C33 C34 1.2(6) . . . . ?
C32 C33 C34 C35 1.1(6) . . . . ?
C31 N3 C35 C34 0.8(5) . . . . ?
C31 N3 C35 C36 -177.7(3) . . . . ?
C33 C34 C35 N3 -2.1(6) . . . . ?
C33 C34 C35 C36 176.3(4) . . . . ?
C7T C2T C3T C4T 0.7(7) . . . . ?
C1T C2T C3T C4T -178.2(6) . . . . ?
C2T C3T C4T C5T -1.4(8) . . . . ?
C2T C3T C4T C1T' 176.1(17) . . . . ?
C3T C4T C5T C6T 1.3(8) . . . . ?
C1T' C4T C5T C6T -176.3(15) . . . . ?
C4T C5T C6T C7T -0.6(7) . . . . ?
C5T C6T C7T C2T -0.1(7) . . . . ?
C3T C2T C7T C6T 0.0(7) . . . . ?
C1T C2T C7T C6T 178.9(5) . . . . ?

####################################################################### 
# 
# 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_THF
_database_code_depnum_ccdc_archive 'CCDC 1431710'
_audit_update_record             
;
2015-10-16 deposited with the CCDC.
2015-11-16 downloaded from the CCDC.
;
#_cambridge_data_id dw_b1_0065
#===============================================================================
_audit_creation_method           SHELXL-2013

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H18 Cl F3 Fe N3 O3 P S, C4 H8 O'
_chemical_formula_sum            'C23 H26 Cl F3 Fe N3 O4 P S'
_chemical_formula_weight         619.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.7879(4)
_cell_length_b                   8.6473(2)
_cell_length_c                   22.5638(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.0326(12)
_cell_angle_gamma                90
_cell_volume                     2679.87(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9884
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      66.67

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_F_000             1272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    7.225
_shelx_estimated_absorpt_T_min   0.341
_shelx_estimated_absorpt_T_max   0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5131
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32629
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.218
_diffrn_reflns_theta_max         66.664
_diffrn_reflns_theta_full        66.664
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4745
_reflns_number_gt                4204
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.

_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0452P)²+1.8986P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4745
_refine_ls_number_parameters     356
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0935
_refine_ls_wR_factor_gt          0.0889
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.063

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.75053(3) 0.23854(4) 0.37127(2) 0.03482(12) Uani 1 1 d . . . . .
Cl1 Cl 0.69871(7) 0.47016(9) 0.33885(3) 0.0754(3) Uani 1 1 d . . . . .
P1 P 0.85433(4) -0.10669(7) 0.37926(3) 0.03592(16) Uani 1 1 d . . . . .
N1 N 0.89801(13) 0.2050(2) 0.40327(8) 0.0293(4) Uani 1 1 d . . . . .
N2 N 0.76758(17) 0.0895(3) 0.29070(9) 0.0467(5) Uani 1 1 d . . . . .
N3 N 0.68133(13) 0.0441(2) 0.40224(9) 0.0361(4) Uani 1 1 d . . . . .
C11 C 0.92970(15) 0.0568(2) 0.40685(9) 0.0285(5) Uani 1 1 d . . . . .
C12 C 1.02440(16) 0.0193(3) 0.42738(10) 0.0353(5) Uani 1 1 d . . . . .
H12 H 1.0445 -0.0858 0.4300 0.042 Uiso 1 1 calc R U . . .
C13 C 1.08926(17) 0.1364(3) 0.44401(11) 0.0417(6) Uani 1 1 d . . . . .
H13 H 1.1549 0.1134 0.4575 0.050 Uiso 1 1 calc R U . . .
C14 C 1.05732(18) 0.2856(3) 0.44069(12) 0.0437(6) Uani 1 1 d . . . . .
H14 H 1.1010 0.3674 0.4521 0.052 Uiso 1 1 calc R U . . .
C15 C 0.96125(18) 0.3190(3) 0.42071(11) 0.0370(5) Uani 1 1 d . . . . .
C16 C 0.9261(2) 0.4825(3) 0.41702(16) 0.0563(8) Uani 1 1 d . . . . .
H16A H 0.9055 0.5082 0.3755 0.085 Uiso 1 1 calc R U . . .
H16B H 0.9789 0.5520 0.4319 0.085 Uiso 1 1 calc R U . . .
H16C H 0.8710 0.4946 0.4412 0.085 Uiso 1 1 calc R U . . .
C21 C 0.82127(19) -0.0405(3) 0.30265(11) 0.0440(6) Uani 1 1 d . . . . .
C22 C 0.8526(2) -0.1356(4) 0.25857(14) 0.0644(9) Uani 1 1 d . . . . .
H22 H 0.8922 -0.2235 0.2684 0.077 Uiso 1 1 calc R U . . .
C23 C 0.8241(3) -0.0981(5) 0.19912(16) 0.0837(12) Uani 1 1 d . . . . .
H23 H 0.8452 -0.1590 0.1676 0.100 Uiso 1 1 calc R U . . .
C24 C 0.7661(3) 0.0256(5) 0.18738(15) 0.0823(12) Uani 1 1 d . . . . .
H24 H 0.7440 0.0486 0.1473 0.099 Uiso 1 1 calc R U . . .
C25 C 0.7379(3) 0.1208(4) 0.23281(13) 0.0655(9) Uani 1 1 d . . . . .
C26 C 0.6725(4) 0.2557(5) 0.21918(16) 0.0896(14) Uani 1 1 d . . . . .
H26A H 0.6166 0.2493 0.2431 0.134 Uiso 1 1 calc R U . . .
H26B H 0.6495 0.2548 0.1768 0.134 Uiso 1 1 calc R U . . .
H26C H 0.7083 0.3516 0.2287 0.134 Uiso 1 1 calc R U . . .
C31 C 0.73561(17) -0.0860(3) 0.40967(11) 0.0351(5) Uani 1 1 d . . . . .
C32 C 0.7004(2) -0.2185(3) 0.43473(14) 0.0497(7) Uani 1 1 d . . . . .
H32 H 0.7407 -0.3071 0.4411 0.060 Uiso 1 1 calc R U . . .
C33 C 0.6061(2) -0.2198(4) 0.45029(17) 0.0641(9) Uani 1 1 d . . . . .
H33 H 0.5803 -0.3094 0.4676 0.077 Uiso 1 1 calc R U . . .
C34 C 0.5500(2) -0.0903(4) 0.44041(16) 0.0633(9) Uani 1 1 d . . . . .
H34 H 0.4840 -0.0914 0.4494 0.076 Uiso 1 1 calc R U . . .
C35 C 0.58868(18) 0.0426(3) 0.41735(13) 0.0481(7) Uani 1 1 d . . . . .
C36 C 0.5308(2) 0.1878(4) 0.40731(17) 0.0674(9) Uani 1 1 d . . . . .
H36A H 0.5579 0.2683 0.4345 0.101 Uiso 1 1 calc R U . . .
H36B H 0.4630 0.1681 0.4147 0.101 Uiso 1 1 calc R U . . .
H36C H 0.5337 0.2222 0.3661 0.101 Uiso 1 1 calc R U . . .
C1 C 0.6844(2) 0.4257(3) 0.57099(13) 0.0460(6) Uani 1 1 d . . . . .
F1 F 0.69235(18) 0.3993(3) 0.62930(8) 0.0872(7) Uani 1 1 d . . . . .
F2 F 0.71578(12) 0.56877(18) 0.56296(9) 0.0632(5) Uani 1 1 d . . . . .
F3 F 0.59094(11) 0.4242(2) 0.55186(10) 0.0765(6) Uani 1 1 d . . . . .
S1 S 0.75357(4) 0.28406(7) 0.53262(3) 0.03390(14) Uani 1 1 d . . . . .
O1 O 0.73409(13) 0.3309(2) 0.47122(8) 0.0451(4) Uani 1 1 d . . . . .
O2 O 0.85158(13) 0.3113(2) 0.55713(9) 0.0510(5) Uani 1 1 d . . . . .
O3 O 0.71193(15) 0.1389(2) 0.54722(9) 0.0527(5) Uani 1 1 d . . . . .
O1S O 1.0000 0.5715(4) 0.2500 0.0840(11) Uani 1 2 d DS T P . .
C2S C 0.9287(3) 0.4792(5) 0.2189(2) 0.0887(12) Uani 1 1 d D . . . .
H1S H 0.9297 0.4939 0.1755 0.106 Uiso 1 1 calc R U . . .
H2S H 0.8631 0.5062 0.2304 0.106 Uiso 1 1 calc R U . . .
C3S C 0.9533(4) 0.3191(5) 0.2356(3) 0.147(3) Uani 1 1 d D . . . .
H3S H 0.9062 0.2780 0.2623 0.176 Uiso 1 1 calc R U . . .
H4S H 0.9510 0.2531 0.1996 0.176 Uiso 1 1 calc R U . . .
O1A O 0.4544(10) 0.0677(12) 0.7586(8) 0.082(3) Uiso 0.25 1 d D . P A -1
C2A C 0.4185(9) 0.2141(15) 0.7335(8) 0.074(4) Uiso 0.25 1 d D . P A -1
H2AA H 0.3832 0.1973 0.6939 0.089 Uiso 0.25 1 calc R U P A -1
H2AB H 0.3735 0.2629 0.7598 0.089 Uiso 0.25 1 calc R U P A -1
C3A C 0.5030(12) 0.3120(15) 0.7284(11) 0.103(10) Uiso 0.25 1 d D . P A -1
H3AA H 0.4982 0.3657 0.6895 0.123 Uiso 0.25 1 calc R U P A -1
H3AB H 0.5085 0.3905 0.7604 0.123 Uiso 0.25 1 calc R U P A -1
C4A C 0.5860(9) 0.2090(17) 0.7337(8) 0.072(4) Uiso 0.25 1 d D . P A -1
H4AA H 0.6443 0.2627 0.7523 0.086 Uiso 0.25 1 calc R U P A -1
H4AB H 0.6004 0.1705 0.6941 0.086 Uiso 0.25 1 calc R U P A -1
C5A C 0.5579(13) 0.0820(19) 0.7711(11) 0.100(7) Uiso 0.25 1 d D . P A -1
H5AA H 0.5911 -0.0149 0.7611 0.120 Uiso 0.25 1 calc R U P A -1
H5AB H 0.5748 0.1057 0.8137 0.120 Uiso 0.25 1 calc R U P A -1
O1B O 0.4866(13) 0.0699(10) 0.7294(5) 0.076(3) Uiso 0.25 1 d D . P B -2
C2B C 0.4619(19) 0.1354(15) 0.7854(8) 0.121(8) Uiso 0.25 1 d D . P B -2
H2BA H 0.5078 0.0977 0.8184 0.145 Uiso 0.25 1 calc R U P B -2
H2BB H 0.3952 0.1040 0.7933 0.145 Uiso 0.25 1 calc R U P B -2
C3B C 0.4677(19) 0.3034(13) 0.7811(7) 0.078(6) Uiso 0.25 1 d D . P B -2
H3BA H 0.5013 0.3477 0.8179 0.093 Uiso 0.25 1 calc R U P B -2
H3BB H 0.4019 0.3494 0.7747 0.093 Uiso 0.25 1 calc R U P B -2
C4B C 0.5235(14) 0.3322(12) 0.7301(6) 0.050(4) Uiso 0.25 1 d D . P B -2
H4BA H 0.5023 0.4292 0.7096 0.060 Uiso 0.25 1 calc R U P B -2
H4BB H 0.5941 0.3386 0.7425 0.060 Uiso 0.25 1 calc R U P B -2
C5B C 0.5017(13) 0.1993(14) 0.6922(5) 0.085(5) Uiso 0.25 1 d D . P B -2
H5BA H 0.4425 0.2191 0.6652 0.103 Uiso 0.25 1 calc R U P B -2
H5BB H 0.5565 0.1785 0.6678 0.103 Uiso 0.25 1 calc R U P B -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N3 2.084(2) . ?
Fe1 N1 2.1172(18) . ?
Fe1 Cl1 2.2284(8) . ?
Fe1 N2 2.258(2) . ?
P1 C11 1.831(2) . ?
P1 C31 1.838(2) . ?
P1 C21 1.840(3) . ?
N1 C15 1.352(3) . ?
N1 C11 1.354(3) . ?
N2 C21 1.360(4) . ?
N2 C25 1.362(4) . ?
N3 C35 1.351(3) . ?
N3 C31 1.353(3) . ?
C11 C12 1.385(3) . ?
C12 C13 1.381(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.363(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.392(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.495(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C21 C22 1.388(4) . ?
C22 C23 1.402(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.347(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.397(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.490(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C31 C32 1.384(4) . ?
C32 C33 1.376(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.368(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.387(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.494(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C1 F3 1.322(3) . ?
C1 F2 1.328(3) . ?
C1 F1 1.330(3) . ?
C1 S1 1.818(3) . ?
S1 O3 1.4307(19) . ?
S1 O2 1.4339(18) . ?
S1 O1 1.4460(18) . ?
O1S C2S 1.405(4) 2_755 ?
O1S C2S 1.405(4) . ?
C2S C3S 1.467(5) . ?
C2S H1S 0.9900 . ?
C2S H2S 0.9900 . ?
C3S C3S 1.392(8) 2_755 ?
C3S H3S 0.9900 . ?
C3S H4S 0.9900 . ?
O1A C5A 1.435(10) . ?
O1A C2A 1.456(9) . ?
C2A C3A 1.453(10) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C3A C4A 1.447(10) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C4A C5A 1.459(10) . ?
C4A H4AA 0.9900 . ?
C4A H4AB 0.9900 . ?
C5A H5AA 0.9900 . ?
C5A H5AB 0.9900 . ?
O1B C5B 1.425(10) . ?
O1B C2B 1.451(10) . ?
C2B C3B 1.458(10) . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C3B C4B 1.461(10) . ?
C3B H3BA 0.9900 . ?
C3B H3BB 0.9900 . ?
C4B C5B 1.448(10) . ?
C4B H4BA 0.9900 . ?
C4B H4BB 0.9900 . ?
C5B H5BA 0.9900 . ?
C5B H5BB 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N1 103.27(7) . . ?
N3 Fe1 Cl1 133.81(6) . . ?
N1 Fe1 Cl1 120.38(6) . . ?
N3 Fe1 N2 83.82(8) . . ?
N1 Fe1 N2 91.81(8) . . ?
Cl1 Fe1 N2 107.57(6) . . ?
C11 P1 C31 107.18(10) . . ?
C11 P1 C21 99.54(11) . . ?
C31 P1 C21 99.51(12) . . ?
C15 N1 C11 118.45(19) . . ?
C15 N1 Fe1 125.10(16) . . ?
C11 N1 Fe1 116.44(14) . . ?
C21 N2 C25 117.9(2) . . ?
C21 N2 Fe1 113.94(16) . . ?
C25 N2 Fe1 128.0(2) . . ?
C35 N3 C31 119.1(2) . . ?
C35 N3 Fe1 124.30(18) . . ?
C31 N3 Fe1 116.59(15) . . ?
N1 C11 C12 122.1(2) . . ?
N1 C11 P1 122.67(16) . . ?
C12 C11 P1 115.04(17) . . ?
C13 C12 C11 119.2(2) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C14 C13 C12 118.7(2) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 120.5(2) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
N1 C15 C14 120.9(2) . . ?
N1 C15 C16 118.4(2) . . ?
C14 C15 C16 120.6(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N2 C21 C22 123.1(3) . . ?
N2 C21 P1 121.94(18) . . ?
C22 C21 P1 115.0(2) . . ?
C21 C22 C23 118.0(3) . . ?
C21 C22 H22 121.0 . . ?
C23 C22 H22 121.0 . . ?
C24 C23 C22 118.9(3) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 H23 120.5 . . ?
C23 C24 C25 121.5(3) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
N2 C25 C24 120.5(3) . . ?
N2 C25 C26 118.7(3) . . ?
C24 C25 C26 120.9(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C31 C32 121.9(2) . . ?
N3 C31 P1 122.38(18) . . ?
C32 C31 P1 115.32(19) . . ?
C33 C32 C31 119.0(3) . . ?
C33 C32 H32 120.5 . . ?
C31 C32 H32 120.5 . . ?
C34 C33 C32 119.0(3) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
C33 C34 C35 120.6(3) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
N3 C35 C34 120.4(3) . . ?
N3 C35 C36 117.2(3) . . ?
C34 C35 C36 122.4(3) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
F3 C1 F2 106.5(2) . . ?
F3 C1 F1 108.3(2) . . ?
F2 C1 F1 107.2(2) . . ?
F3 C1 S1 112.01(19) . . ?
F2 C1 S1 111.81(18) . . ?
F1 C1 S1 110.7(2) . . ?
O3 S1 O2 116.03(12) . . ?
O3 S1 O1 114.95(12) . . ?
O2 S1 O1 114.40(12) . . ?
O3 S1 C1 104.09(13) . . ?
O2 S1 C1 102.83(12) . . ?
O1 S1 C1 101.91(12) . . ?
C2S O1S C2S 110.8(4) 2_755 . ?
O1S C2S C3S 105.8(3) . . ?
O1S C2S H1S 110.6 . . ?
C3S C2S H1S 110.6 . . ?
O1S C2S H2S 110.6 . . ?
C3S C2S H2S 110.6 . . ?
H1S C2S H2S 108.7 . . ?
C3S C3S C2S 107.7(3) 2_755 . ?
C3S C3S H3S 110.2 2_755 . ?
C2S C3S H3S 110.2 . . ?
C3S C3S H4S 110.2 2_755 . ?
C2S C3S H4S 110.2 . . ?
H3S C3S H4S 108.5 . . ?
C5A O1A C2A 107.4(7) . . ?
C3A C2A O1A 106.9(7) . . ?
C3A C2A H2AA 110.3 . . ?
O1A C2A H2AA 110.3 . . ?
C3A C2A H2AB 110.3 . . ?
O1A C2A H2AB 110.3 . . ?
H2AA C2A H2AB 108.6 . . ?
C4A C3A C2A 105.6(6) . . ?
C4A C3A H3AA 110.6 . . ?
C2A C3A H3AA 110.6 . . ?
C4A C3A H3AB 110.6 . . ?
C2A C3A H3AB 110.6 . . ?
H3AA C3A H3AB 108.8 . . ?
C3A C4A C5A 105.2(8) . . ?
C3A C4A H4AA 110.7 . . ?
C5A C4A H4AA 110.7 . . ?
C3A C4A H4AB 110.7 . . ?
C5A C4A H4AB 110.7 . . ?
H4AA C4A H4AB 108.8 . . ?
O1A C5A C4A 105.2(7) . . ?
O1A C5A H5AA 110.7 . . ?
C4A C5A H5AA 110.7 . . ?
O1A C5A H5AB 110.7 . . ?
C4A C5A H5AB 110.7 . . ?
H5AA C5A H5AB 108.8 . . ?
C5B O1B C2B 105.3(6) . . ?
O1B C2B C3B 108.3(7) . . ?
O1B C2B H2BA 110.0 . . ?
C3B C2B H2BA 110.0 . . ?
O1B C2B H2BB 110.0 . . ?
C3B C2B H2BB 110.0 . . ?
H2BA C2B H2BB 108.4 . . ?
C2B C3B C4B 104.9(6) . . ?
C2B C3B H3BA 110.8 . . ?
C4B C3B H3BA 110.8 . . ?
C2B C3B H3BB 110.8 . . ?
C4B C3B H3BB 110.8 . . ?
H3BA C3B H3BB 108.8 . . ?
C5B C4B C3B 103.5(7) . . ?
C5B C4B H4BA 111.1 . . ?
C3B C4B H4BA 111.1 . . ?
C5B C4B H4BB 111.1 . . ?
C3B C4B H4BB 111.1 . . ?
H4BA C4B H4BB 109.0 . . ?
O1B C5B C4B 108.0(7) . . ?
O1B C5B H5BA 110.1 . . ?
C4B C5B H5BA 110.1 . . ?
O1B C5B H5BB 110.1 . . ?
C4B C5B H5BB 110.1 . . ?
H5BA C5B H5BB 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 N1 C11 C12 -0.4(3) . . . . ?
Fe1 N1 C11 C12 -179.62(16) . . . . ?
C15 N1 C11 P1 -175.09(17) . . . . ?
Fe1 N1 C11 P1 5.7(2) . . . . ?
C31 P1 C11 N1 -49.5(2) . . . . ?
C21 P1 C11 N1 53.7(2) . . . . ?
C31 P1 C11 C12 135.47(17) . . . . ?
C21 P1 C11 C12 -121.39(18) . . . . ?
N1 C11 C12 C13 -0.9(3) . . . . ?
P1 C11 C12 C13 174.16(18) . . . . ?
C11 C12 C13 C14 1.2(4) . . . . ?
C12 C13 C14 C15 -0.2(4) . . . . ?
C11 N1 C15 C14 1.4(3) . . . . ?
Fe1 N1 C15 C14 -179.45(18) . . . . ?
C11 N1 C15 C16 -179.7(2) . . . . ?
Fe1 N1 C15 C16 -0.6(3) . . . . ?
C13 C14 C15 N1 -1.1(4) . . . . ?
C13 C14 C15 C16 -180.0(3) . . . . ?
C25 N2 C21 C22 4.7(4) . . . . ?
Fe1 N2 C21 C22 -170.2(2) . . . . ?
C25 N2 C21 P1 -173.2(2) . . . . ?
Fe1 N2 C21 P1 11.9(3) . . . . ?
C11 P1 C21 N2 -63.3(2) . . . . ?
C31 P1 C21 N2 46.0(2) . . . . ?
C11 P1 C21 C22 118.6(2) . . . . ?
C31 P1 C21 C22 -132.0(2) . . . . ?
N2 C21 C22 C23 -2.5(5) . . . . ?
P1 C21 C22 C23 175.6(3) . . . . ?
C21 C22 C23 C24 -1.5(6) . . . . ?
C22 C23 C24 C25 3.0(6) . . . . ?
C21 N2 C25 C24 -3.1(5) . . . . ?
Fe1 N2 C25 C24 171.0(3) . . . . ?
C21 N2 C25 C26 175.2(3) . . . . ?
Fe1 N2 C25 C26 -10.7(5) . . . . ?
C23 C24 C25 N2 -0.8(6) . . . . ?
C23 C24 C25 C26 -179.0(4) . . . . ?
C35 N3 C31 C32 -2.9(4) . . . . ?
Fe1 N3 C31 C32 174.4(2) . . . . ?
C35 N3 C31 P1 169.52(19) . . . . ?
Fe1 N3 C31 P1 -13.2(2) . . . . ?
C11 P1 C31 N3 54.7(2) . . . . ?
C21 P1 C31 N3 -48.5(2) . . . . ?
C11 P1 C31 C32 -132.4(2) . . . . ?
C21 P1 C31 C32 124.4(2) . . . . ?
N3 C31 C32 C33 2.7(4) . . . . ?
P1 C31 C32 C33 -170.2(3) . . . . ?
C31 C32 C33 C34 0.1(5) . . . . ?
C32 C33 C34 C35 -2.6(5) . . . . ?
C31 N3 C35 C34 0.3(4) . . . . ?
Fe1 N3 C35 C34 -176.7(2) . . . . ?
C31 N3 C35 C36 -178.9(2) . . . . ?
Fe1 N3 C35 C36 4.1(3) . . . . ?
C33 C34 C35 N3 2.5(5) . . . . ?
C33 C34 C35 C36 -178.4(3) . . . . ?
F3 C1 S1 O3 -61.9(2) . . . . ?
F2 C1 S1 O3 178.63(19) . . . . ?
F1 C1 S1 O3 59.2(2) . . . . ?
F3 C1 S1 O2 176.7(2) . . . . ?
F2 C1 S1 O2 57.2(2) . . . . ?
F1 C1 S1 O2 -62.2(2) . . . . ?
F3 C1 S1 O1 58.0(2) . . . . ?
F2 C1 S1 O1 -61.5(2) . . . . ?
F1 C1 S1 O1 179.0(2) . . . . ?
C2S O1S C2S C3S 4.6(4) 2_755 . . . ?
O1S C2S C3S C3S -12.5(10) . . . 2_755 ?
C5A O1A C2A C3A 3(3) . . . . ?
O1A C2A C3A C4A 16(2) . . . . ?
C2A C3A C4A C5A -29(2) . . . . ?
C2A O1A C5A C4A -21(3) . . . . ?
C3A C4A C5A O1A 31(2) . . . . ?
C5B O1B C2B C3B -3(3) . . . . ?
O1B C2B C3B C4B -17(2) . . . . ?
C2B C3B C4B C5B 29.0(19) . . . . ?
C2B O1B C5B C4B 22(2) . . . . ?
C3B C4B C5B O1B -32.0(16) . . . . ?

####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1431711'
_audit_update_record             
;
2015-10-16 deposited with the CCDC.
2015-11-16 downloaded from the CCDC.
;
#_cambridge_data_id DW_B1_0061
#===============================================================================
_audit_creation_method           SHELXL-2013

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H30 Cu2 N7 P 2+, 2(F6 P -)'
_chemical_formula_sum            'C26 H30 Cu2 F12 N7 P3'
_chemical_formula_weight         888.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2686(5)
_cell_length_b                   14.9441(9)
_cell_length_c                   14.9496(8)
_cell_angle_alpha                78.976(2)
_cell_angle_beta                 80.942(2)
_cell_angle_gamma                84.159(2)
_cell_volume                     1785.67(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9814
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      66.70

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_F_000             892
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    3.598
_shelx_estimated_absorpt_T_min   0.548
_shelx_estimated_absorpt_T_max   0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5888
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            45856
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.021
_diffrn_reflns_theta_max         66.694
_diffrn_reflns_theta_full        66.694
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             6267
_reflns_number_gt                5586
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.

_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0630P)²+3.9764P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6267
_refine_ls_number_parameters     458
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1301
_refine_ls_wR_factor_gt          0.1255
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.081

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.51460(6) 0.25904(3) 0.38980(3) 0.02996(15) Uani 1 1 d . . . . .
P1 P 0.48951(9) 0.23482(5) 0.60708(5) 0.02472(18) Uani 1 1 d . . . . .
N1 N 0.6145(3) 0.14111(18) 0.46542(18) 0.0262(5) Uani 1 1 d . . . . .
C11 C 0.6048(4) 0.1400(2) 0.5569(2) 0.0257(6) Uani 1 1 d . . . . .
C12 C 0.6762(4) 0.0695(2) 0.6160(2) 0.0345(7) Uani 1 1 d . . . . .
H12A H 0.6673 0.0711 0.6798 0.041 Uiso 1 1 calc R U . . .
C13 C 0.7606(5) -0.0032(3) 0.5799(3) 0.0449(9) Uani 1 1 d . . . . .
H13A H 0.8126 -0.0521 0.6183 0.054 Uiso 1 1 calc R U . . .
C14 C 0.7682(5) -0.0036(3) 0.4876(3) 0.0421(9) Uani 1 1 d . . . . .
H14A H 0.8247 -0.0535 0.4621 0.051 Uiso 1 1 calc R U . . .
C15 C 0.6937(4) 0.0688(2) 0.4310(2) 0.0333(7) Uani 1 1 d . . . . .
C16 C 0.6987(5) 0.0694(3) 0.3307(3) 0.0476(9) Uani 1 1 d . . . . .
H16A H 0.5875 0.0830 0.3143 0.071 Uiso 1 1 calc R U . . .
H16B H 0.7421 0.0093 0.3167 0.071 Uiso 1 1 calc R U . . .
H16C H 0.7698 0.1162 0.2951 0.071 Uiso 1 1 calc R U . . .
N2 N 0.6109(3) 0.35271(18) 0.44956(18) 0.0279(6) Uani 1 1 d . . . . .
C21 C 0.5898(4) 0.3367(2) 0.5432(2) 0.0281(7) Uani 1 1 d . . . . .
C22 C 0.6424(4) 0.3932(2) 0.5939(3) 0.0376(8) Uani 1 1 d . . . . .
H22A H 0.6237 0.3805 0.6593 0.045 Uiso 1 1 calc R U . . .
C23 C 0.7233(5) 0.4691(3) 0.5474(3) 0.0505(10) Uani 1 1 d . . . . .
H23A H 0.7613 0.5093 0.5803 0.061 Uiso 1 1 calc R U . . .
C24 C 0.7476(5) 0.4852(3) 0.4526(3) 0.0476(10) Uani 1 1 d . . . . .
H24A H 0.8045 0.5363 0.4197 0.057 Uiso 1 1 calc R U . . .
C25 C 0.6888(4) 0.4269(2) 0.4049(3) 0.0368(8) Uani 1 1 d . . . . .
C26 C 0.7107(5) 0.4448(3) 0.3019(3) 0.0511(10) Uani 1 1 d . . . . .
H26A H 0.7720 0.3922 0.2790 0.077 Uiso 1 1 calc R U . . .
H26B H 0.7715 0.4994 0.2784 0.077 Uiso 1 1 calc R U . . .
H26C H 0.6028 0.4546 0.2808 0.077 Uiso 1 1 calc R U . . .
N3 N 0.2884(3) 0.25504(17) 0.47136(17) 0.0257(5) Uani 1 1 d . . . . .
C31 C 0.2925(4) 0.2437(2) 0.5625(2) 0.0264(6) Uani 1 1 d . . . . .
C32 C 0.1521(4) 0.2360(3) 0.6267(3) 0.0444(9) Uani 1 1 d . . . . .
H32A H 0.1583 0.2294 0.6906 0.053 Uiso 1 1 calc R U . . .
C33 C 0.0021(4) 0.2383(3) 0.5956(3) 0.0551(12) Uani 1 1 d . . . . .
H33A H -0.0963 0.2324 0.6379 0.066 Uiso 1 1 calc R U . . .
C34 C -0.0021(4) 0.2490(3) 0.5034(3) 0.0438(9) Uani 1 1 d . . . . .
H34A H -0.1041 0.2503 0.4813 0.053 Uiso 1 1 calc R U . . .
C35 C 0.1411(4) 0.2580(2) 0.4418(2) 0.0302(7) Uani 1 1 d . . . . .
C36 C 0.1376(5) 0.2707(3) 0.3405(3) 0.0447(9) Uani 1 1 d . . . . .
H36A H 0.2147 0.2249 0.3145 0.067 Uiso 1 1 calc R U . . .
H36B H 0.1693 0.3320 0.3113 0.067 Uiso 1 1 calc R U . . .
H36C H 0.0264 0.2634 0.3293 0.067 Uiso 1 1 calc R U . . .
Cu2 Cu 0.47026(6) 0.21273(3) 0.75819(3) 0.03263(15) Uani 1 1 d . . . . .
N4 N 0.5381(4) 0.2752(2) 0.2573(2) 0.0405(7) Uani 1 1 d . . . . .
N5 N 0.3790(4) 0.0921(2) 0.8237(2) 0.0397(7) Uani 1 1 d . . . . .
N6 N 0.6869(4) 0.1948(2) 0.8079(2) 0.0395(7) Uani 1 1 d . . . . .
N7 N 0.3381(4) 0.3009(2) 0.8304(2) 0.0387(7) Uani 1 1 d . . . . .
C41 C 0.5535(5) 0.2893(3) 0.1794(3) 0.0463(9) Uani 1 1 d . . . . .
C42 C 0.5761(8) 0.3083(4) 0.0792(3) 0.0769(17) Uani 1 1 d . . . . .
H42A H 0.5526 0.3738 0.0576 0.115 Uiso 1 1 calc R U . . .
H42B H 0.5012 0.2736 0.0569 0.115 Uiso 1 1 calc R U . . .
H42C H 0.6897 0.2902 0.0556 0.115 Uiso 1 1 calc R U . . .
C51 C 0.3620(5) 0.0242(3) 0.8705(3) 0.0397(8) Uani 1 1 d . . . . .
C52 C 0.3421(6) -0.0639(3) 0.9303(4) 0.0719(15) Uani 1 1 d . . . . .
H52A H 0.2618 -0.0962 0.9095 0.108 Uiso 1 1 calc R U . . .
H52B H 0.3033 -0.0547 0.9936 0.108 Uiso 1 1 calc R U . . .
H52C H 0.4478 -0.1002 0.9284 0.108 Uiso 1 1 calc R U . . .
C61 C 0.8037(5) 0.1885(3) 0.8396(2) 0.0392(8) Uani 1 1 d . . . . .
C62 C 0.9544(5) 0.1819(4) 0.8801(3) 0.0606(12) Uani 1 1 d . . . . .
H62A H 1.0239 0.1281 0.8653 0.091 Uiso 1 1 calc R U . . .
H62B H 0.9275 0.1762 0.9471 0.091 Uiso 1 1 calc R U . . .
H62C H 1.0132 0.2370 0.8552 0.091 Uiso 1 1 calc R U . . .
C71 C 0.2846(5) 0.3479(3) 0.8800(3) 0.0417(9) Uani 1 1 d . . . . .
C72 C 0.2200(7) 0.4081(4) 0.9444(4) 0.0758(17) Uani 1 1 d . . . . .
H72A H 0.1744 0.3719 1.0030 0.114 Uiso 1 1 calc R U . . .
H72B H 0.1334 0.4508 0.9194 0.114 Uiso 1 1 calc R U . . .
H72C H 0.3084 0.4425 0.9544 0.114 Uiso 1 1 calc R U . . .
P2 P 0.21991(13) 0.53690(7) 0.16874(7) 0.0446(2) Uani 1 1 d . . . . .
F1 F 0.1548(5) 0.6001(3) 0.0835(3) 0.1164(15) Uani 1 1 d . . . . .
F2 F 0.3560(5) 0.4924(3) 0.1004(3) 0.1183(15) Uani 1 1 d . . . . .
F3 F 0.0990(5) 0.4634(2) 0.1639(2) 0.0940(11) Uani 1 1 d . . . . .
F4 F 0.0864(5) 0.5833(3) 0.2342(3) 0.1241(15) Uani 1 1 d . . . . .
F5 F 0.2900(5) 0.4741(2) 0.2532(2) 0.0952(11) Uani 1 1 d . . . . .
F6 F 0.3425(5) 0.6092(2) 0.1713(3) 0.1081(13) Uani 1 1 d . . . . .
P3 P 0.14494(15) 0.10879(9) 0.13250(8) 0.0572(3) Uani 1 1 d . . . . .
F7 F 0.2819(5) 0.0291(4) 0.1331(5) 0.182(3) Uani 1 1 d . . . . .
F8 F -0.0010(7) 0.1798(4) 0.1288(6) 0.196(3) Uani 1 1 d . . . . .
F9 F 0.2219(7) 0.1458(5) 0.0351(3) 0.163(2) Uani 1 1 d . . . . .
F10 F 0.0745(6) 0.0763(8) 0.2310(3) 0.288(6) Uani 1 1 d . . . . .
F11 F 0.0322(7) 0.0511(4) 0.1002(6) 0.197(3) Uani 1 1 d . . . . .
F12 F 0.2637(7) 0.1631(7) 0.1632(5) 0.258(5) Uani 1 1 d . . . . .


_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
Cu1 N4 1.930(3) . ?
Cu1 N3 2.065(3) . ?
Cu1 N1 2.074(3) . ?
Cu1 N2 2.079(3) . ?
P1 C21 1.835(3) . ?
P1 C31 1.838(3) . ?
P1 C11 1.840(3) . ?
P1 Cu2 2.2021(9) . ?
N1 C15 1.350(4) . ?
N1 C11 1.354(4) . ?
C11 C12 1.386(5) . ?
C12 C13 1.382(5) . ?
C12 H12A 0.9500 . ?
C13 C14 1.373(6) . ?
C13 H13A 0.9500 . ?
C14 C15 1.395(5) . ?
C14 H14A 0.9500 . ?
C15 C16 1.492(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N2 C25 1.348(4) . ?
N2 C21 1.360(4) . ?
C21 C22 1.380(5) . ?
C22 C23 1.387(5) . ?
C22 H22A 0.9500 . ?
C23 C24 1.376(6) . ?
C23 H23A 0.9500 . ?
C24 C25 1.392(6) . ?
C24 H24A 0.9500 . ?
C25 C26 1.497(6) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
N3 C31 1.346(4) . ?
N3 C35 1.353(4) . ?
C31 C32 1.385(5) . ?
C32 C33 1.387(5) . ?
C32 H32A 0.9500 . ?
C33 C34 1.362(6) . ?
C33 H33A 0.9500 . ?
C34 C35 1.382(5) . ?
C34 H34A 0.9500 . ?
C35 C36 1.494(5) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
Cu2 N7 1.994(3) . ?
Cu2 N6 2.020(3) . ?
Cu2 N5 2.037(3) . ?
N4 C41 1.132(5) . ?
N5 C51 1.125(5) . ?
N6 C61 1.129(5) . ?
N7 C71 1.127(5) . ?
C41 C42 1.456(6) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C51 C52 1.452(6) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 C62 1.456(5) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C71 C72 1.448(6) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
P2 F4 1.556(3) . ?
P2 F6 1.564(3) . ?
P2 F1 1.568(3) . ?
P2 F5 1.574(3) . ?
P2 F3 1.577(3) . ?
P2 F2 1.581(4) . ?
P3 F10 1.503(4) . ?
P3 F12 1.510(4) . ?
P3 F9 1.517(4) . ?
P3 F11 1.520(4) . ?
P3 F8 1.524(5) . ?
P3 F7 1.557(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Cu1 N3 122.49(12) . . ?
N4 Cu1 N1 120.32(12) . . ?
N3 Cu1 N1 94.41(10) . . ?
N4 Cu1 N2 118.92(12) . . ?
N3 Cu1 N2 97.35(10) . . ?
N1 Cu1 N2 97.53(10) . . ?
C21 P1 C31 103.96(14) . . ?
C21 P1 C11 104.08(14) . . ?
C31 P1 C11 102.61(14) . . ?
C21 P1 Cu2 116.57(11) . . ?
C31 P1 Cu2 114.85(10) . . ?
C11 P1 Cu2 113.19(10) . . ?
C15 N1 C11 118.2(3) . . ?
C15 N1 Cu1 125.9(2) . . ?
C11 N1 Cu1 115.7(2) . . ?
N1 C11 C12 123.0(3) . . ?
N1 C11 P1 119.4(2) . . ?
C12 C11 P1 117.5(2) . . ?
C13 C12 C11 118.4(3) . . ?
C13 C12 H12A 120.8 . . ?
C11 C12 H12A 120.8 . . ?
C14 C13 C12 118.9(3) . . ?
C14 C13 H13A 120.5 . . ?
C12 C13 H13A 120.5 . . ?
C13 C14 C15 120.5(3) . . ?
C13 C14 H14A 119.8 . . ?
C15 C14 H14A 119.8 . . ?
N1 C15 C14 120.8(3) . . ?
N1 C15 C16 117.7(3) . . ?
C14 C15 C16 121.4(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C25 N2 C21 118.0(3) . . ?
C25 N2 Cu1 126.5(2) . . ?
C21 N2 Cu1 115.5(2) . . ?
N2 C21 C22 123.1(3) . . ?
N2 C21 P1 119.6(2) . . ?
C22 C21 P1 117.3(3) . . ?
C21 C22 C23 118.5(4) . . ?
C21 C22 H22A 120.8 . . ?
C23 C22 H22A 120.8 . . ?
C24 C23 C22 118.9(4) . . ?
C24 C23 H23A 120.5 . . ?
C22 C23 H23A 120.5 . . ?
C23 C24 C25 120.1(3) . . ?
C23 C24 H24A 119.9 . . ?
C25 C24 H24A 119.9 . . ?
N2 C25 C24 121.4(3) . . ?
N2 C25 C26 117.9(3) . . ?
C24 C25 C26 120.7(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C31 N3 C35 118.5(3) . . ?
C31 N3 Cu1 115.3(2) . . ?
C35 N3 Cu1 126.1(2) . . ?
N3 C31 C32 122.6(3) . . ?
N3 C31 P1 120.5(2) . . ?
C32 C31 P1 116.9(2) . . ?
C31 C32 C33 118.4(3) . . ?
C31 C32 H32A 120.8 . . ?
C33 C32 H32A 120.8 . . ?
C34 C33 C32 119.1(3) . . ?
C34 C33 H33A 120.4 . . ?
C32 C33 H33A 120.4 . . ?
C33 C34 C35 120.4(3) . . ?
C33 C34 H34A 119.8 . . ?
C35 C34 H34A 119.8 . . ?
N3 C35 C34 121.0(3) . . ?
N3 C35 C36 118.2(3) . . ?
C34 C35 C36 120.8(3) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N7 Cu2 N6 103.36(13) . . ?
N7 Cu2 N5 101.62(12) . . ?
N6 Cu2 N5 97.93(13) . . ?
N7 Cu2 P1 121.25(9) . . ?
N6 Cu2 P1 115.03(9) . . ?
N5 Cu2 P1 114.33(9) . . ?
C41 N4 Cu1 176.4(3) . . ?
C51 N5 Cu2 162.8(3) . . ?
C61 N6 Cu2 175.5(3) . . ?
C71 N7 Cu2 168.2(3) . . ?
N4 C41 C42 178.9(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N5 C51 C52 179.2(5) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N6 C61 C62 179.1(4) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
N7 C71 C72 178.5(4) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
F4 P2 F6 90.6(2) . . ?
F4 P2 F1 89.9(3) . . ?
F6 P2 F1 90.0(2) . . ?
F4 P2 F5 91.1(2) . . ?
F6 P2 F5 88.9(2) . . ?
F1 P2 F5 178.5(2) . . ?
F4 P2 F3 90.8(2) . . ?
F6 P2 F3 178.6(2) . . ?
F1 P2 F3 89.6(2) . . ?
F5 P2 F3 91.54(19) . . ?
F4 P2 F2 178.4(3) . . ?
F6 P2 F2 88.5(2) . . ?
F1 P2 F2 88.8(3) . . ?
F5 P2 F2 90.1(2) . . ?
F3 P2 F2 90.2(2) . . ?
F10 P3 F12 90.4(4) . . ?
F10 P3 F9 176.4(5) . . ?
F12 P3 F9 86.1(4) . . ?
F10 P3 F11 90.5(5) . . ?
F12 P3 F11 177.3(4) . . ?
F9 P3 F11 93.0(4) . . ?
F10 P3 F8 86.7(4) . . ?
F12 P3 F8 98.9(5) . . ?
F9 P3 F8 93.3(4) . . ?
F11 P3 F8 83.7(4) . . ?
F10 P3 F7 93.1(5) . . ?
F12 P3 F7 87.4(4) . . ?
F9 P3 F7 87.3(3) . . ?
F11 P3 F7 90.0(3) . . ?
F8 P3 F7 173.7(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 N1 C11 C12 1.9(4) . . . . ?
Cu1 N1 C11 C12 -175.0(2) . . . . ?
C15 N1 C11 P1 -177.1(2) . . . . ?
Cu1 N1 C11 P1 5.9(3) . . . . ?
C21 P1 C11 N1 -57.9(3) . . . . ?
C31 P1 C11 N1 50.2(3) . . . . ?
Cu2 P1 C11 N1 174.6(2) . . . . ?
C21 P1 C11 C12 123.0(3) . . . . ?
C31 P1 C11 C12 -128.8(3) . . . . ?
Cu2 P1 C11 C12 -4.5(3) . . . . ?
N1 C11 C12 C13 -0.3(5) . . . . ?
P1 C11 C12 C13 178.8(3) . . . . ?
C11 C12 C13 C14 -1.1(6) . . . . ?
C12 C13 C14 C15 0.8(6) . . . . ?
C11 N1 C15 C14 -2.1(5) . . . . ?
Cu1 N1 C15 C14 174.4(3) . . . . ?
C11 N1 C15 C16 178.0(3) . . . . ?
Cu1 N1 C15 C16 -5.4(4) . . . . ?
C13 C14 C15 N1 0.8(6) . . . . ?
C13 C14 C15 C16 -179.3(4) . . . . ?
C25 N2 C21 C22 0.9(5) . . . . ?
Cu1 N2 C21 C22 -178.4(3) . . . . ?
C25 N2 C21 P1 -178.3(2) . . . . ?
Cu1 N2 C21 P1 2.5(3) . . . . ?
C31 P1 C21 N2 -54.8(3) . . . . ?
C11 P1 C21 N2 52.3(3) . . . . ?
Cu2 P1 C21 N2 177.7(2) . . . . ?
C31 P1 C21 C22 126.0(3) . . . . ?
C11 P1 C21 C22 -126.9(3) . . . . ?
Cu2 P1 C21 C22 -1.5(3) . . . . ?
N2 C21 C22 C23 -1.2(5) . . . . ?
P1 C21 C22 C23 178.0(3) . . . . ?
C21 C22 C23 C24 0.2(6) . . . . ?
C22 C23 C24 C25 1.2(6) . . . . ?
C21 N2 C25 C24 0.5(5) . . . . ?
Cu1 N2 C25 C24 179.6(3) . . . . ?
C21 N2 C25 C26 -179.5(3) . . . . ?
Cu1 N2 C25 C26 -0.4(4) . . . . ?
C23 C24 C25 N2 -1.6(6) . . . . ?
C23 C24 C25 C26 178.5(4) . . . . ?
C35 N3 C31 C32 -0.8(5) . . . . ?
Cu1 N3 C31 C32 -177.4(3) . . . . ?
C35 N3 C31 P1 177.7(2) . . . . ?
Cu1 N3 C31 P1 1.0(3) . . . . ?
C21 P1 C31 N3 53.0(3) . . . . ?
C11 P1 C31 N3 -55.2(3) . . . . ?
Cu2 P1 C31 N3 -178.4(2) . . . . ?
C21 P1 C31 C32 -128.4(3) . . . . ?
C11 P1 C31 C32 123.4(3) . . . . ?
Cu2 P1 C31 C32 0.1(3) . . . . ?
N3 C31 C32 C33 1.4(6) . . . . ?
P1 C31 C32 C33 -177.1(3) . . . . ?
C31 C32 C33 C34 -0.8(7) . . . . ?
C32 C33 C34 C35 -0.3(7) . . . . ?
C31 N3 C35 C34 -0.4(5) . . . . ?
Cu1 N3 C35 C34 175.9(3) . . . . ?
C31 N3 C35 C36 180.0(3) . . . . ?
Cu1 N3 C35 C36 -3.7(4) . . . . ?
C33 C34 C35 N3 1.0(6) . . . . ?
C33 C34 C35 C36 -179.4(4) . . . . ?

