# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_xsc1102
_database_code_depnum_ccdc_archive 'CCDC 1820797'
_audit_update_record             
;
2018-02-15 deposited with the CCDC.
2018-04-05 downloaded from the CCDC.
;
_audit_creation_date             2018-02-06
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H30 Fe N12 O2, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C32 H33 F12 Fe N13 O2 P2'
_chemical_formula_weight         977.50
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4972(14)
_cell_length_b                   14.741(2)
_cell_length_c                   16.340(3)
_cell_angle_alpha                73.026(2)
_cell_angle_beta                 81.584(2)
_cell_angle_gamma                87.250(2)
_cell_volume                     1936.3(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4938
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.183
_cell_measurement_theta_min      2.217
_shelx_estimated_absorpt_T_max   0.944
_shelx_estimated_absorpt_T_min   0.918
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0470 before and 0.0392 after correction.
The Ratio of minimum to maximum transmission is 0.9088.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method 'Recystallized from acetonitrile/ether'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17668
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.217
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5378
_reflns_number_total             7042
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.161
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         7042
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0515
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0701P)²+2.3245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1412
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C13A(H13A)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C5A(H5A), C6A(H6A), C9(H9), C4(H4), C6(H6), C7(H7), C7A(H7A),
 C4A(H4A), C10(H10), C5(H5), C8(H8), C8A(H8A), C11A(H11A), C10A(H10A), C9A(H9A)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C15A(H15A,H15B,H15C), C14(H14A,H14B,H14C), C14A(H14D,
 H14E,H14F), C15(H15D,H15E,H15F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.01096(5) 0.72626(3) 0.74554(3) 0.02288(14) Uani 1 1 d . . . . .
P2 P 0.28710(13) 0.09986(7) 0.63769(7) 0.0378(3) Uani 1 1 d . . . . .
P1 P 0.44904(13) 0.55597(8) 0.23706(8) 0.0453(3) Uani 1 1 d . . . . .
O1 O 0.0882(3) 0.9726(2) 0.89938(19) 0.0481(7) Uani 1 1 d . . . . .
F8 F 0.3938(3) 0.04426(17) 0.57923(16) 0.0568(7) Uani 1 1 d . . . . .
N1 N -0.0471(3) 0.8310(2) 0.78321(17) 0.0260(6) Uani 1 1 d . . . . .
N1A N 0.0724(3) 0.62236(19) 0.70650(18) 0.0265(6) Uani 1 1 d . . . . .
F11 F 0.4225(3) 0.0844(2) 0.69968(17) 0.0666(8) Uani 1 1 d . . . . .
F12 F 0.1814(3) 0.1556(2) 0.69538(17) 0.0617(7) Uani 1 1 d . . . . .
N6A N -0.0749(3) 0.6211(2) 0.84630(18) 0.0309(7) Uani 1 1 d . . . . .
N3A N 0.1533(4) 0.4736(2) 0.6454(2) 0.0370(7) Uani 1 1 d . . . . .
N5A N 0.1111(3) 0.79145(18) 0.62496(17) 0.0228(6) Uani 1 1 d . . . . .
N5 N -0.1978(3) 0.75656(19) 0.70161(17) 0.0241(6) Uani 1 1 d . . . . .
N3 N -0.1243(4) 0.9923(2) 0.8253(2) 0.0383(8) Uani 1 1 d . . . . .
F5 F 0.5139(3) 0.46958(18) 0.30958(18) 0.0642(7) Uani 1 1 d . . . . .
F6 F 0.4846(4) 0.62698(19) 0.2879(2) 0.0756(9) Uani 1 1 d . . . . .
F57 F 0.3862(4) 0.64040(19) 0.1647(2) 0.0770(9) Uani 1 1 d . . . . .
O1A O 0.0491(4) 0.3719(2) 0.7762(2) 0.0581(8) Uani 1 1 d . . . . .
F10 F 0.2143(4) 0.0022(2) 0.69557(18) 0.0895(11) Uani 1 1 d . . . . .
N2 N 0.0481(3) 0.8633(2) 0.82969(18) 0.0283(6) Uani 1 1 d . . . . .
F3 F 0.4129(4) 0.4830(2) 0.1874(2) 0.0837(10) Uani 1 1 d . . . . .
F7 F 0.3719(4) 0.19484(19) 0.58198(19) 0.0759(9) Uani 1 1 d . . . . .
F4 F 0.2753(3) 0.5376(2) 0.2895(2) 0.0921(11) Uani 1 1 d . . . . .
F9 F 0.1593(3) 0.1150(2) 0.57468(19) 0.0767(9) Uani 1 1 d . . . . .
N2A N 0.0371(3) 0.5320(2) 0.7592(2) 0.0344(7) Uani 1 1 d . . . . .
N4 N -0.2217(4) 0.9611(2) 0.7791(2) 0.0358(7) Uani 1 1 d . . . . .
N6 N 0.1972(3) 0.73913(19) 0.80126(17) 0.0252(6) Uani 1 1 d . . . . .
N4A N 0.1856(4) 0.5625(2) 0.5919(2) 0.0374(7) Uani 1 1 d . . . . .
C12 C 0.1881(4) 0.8088(2) 0.8403(2) 0.0279(7) Uani 1 1 d . . . . .
C11 C 0.3053(4) 0.8244(3) 0.8850(2) 0.0342(8) Uani 1 1 d . . . . .
H11 H 0.2952 0.8744 0.9114 0.041 Uiso 1 1 calc R . . . .
C2A C 0.1454(4) 0.6323(2) 0.6256(2) 0.0270(7) Uani 1 1 d . . . . .
F1 F 0.6245(3) 0.5689(3) 0.1873(2) 0.0871(10) Uani 1 1 d . . . . .
C3 C -0.2641(4) 0.8394(2) 0.7109(2) 0.0263(7) Uani 1 1 d . . . . .
C5A C 0.2458(4) 0.8614(3) 0.4539(2) 0.0354(9) Uani 1 1 d . . . . .
H5A H 0.2933 0.8859 0.3956 0.042 Uiso 1 1 calc R . . . .
C1 C 0.0092(4) 0.9459(3) 0.8549(2) 0.0336(8) Uani 1 1 d . . . . .
C12A C -0.0484(4) 0.5328(3) 0.8383(2) 0.0342(8) Uani 1 1 d . . . . .
C6A C 0.1847(4) 0.9218(3) 0.5008(2) 0.0323(8) Uani 1 1 d . . . . .
H6A H 0.1878 0.9885 0.4749 0.039 Uiso 1 1 calc R . . . .
C9 C 0.4486(4) 0.6939(3) 0.8515(2) 0.0332(8) Uani 1 1 d . . . . .
H9 H 0.5385 0.6528 0.8551 0.040 Uiso 1 1 calc R . . . .
C4 C -0.3967(4) 0.8788(3) 0.6746(2) 0.0295(8) Uani 1 1 d . . . . .
H4 H -0.4407 0.9366 0.6826 0.035 Uiso 1 1 calc R . . . .
C2 C -0.1778(4) 0.8825(2) 0.7613(2) 0.0272(7) Uani 1 1 d . . . . .
C6 C -0.4018(4) 0.7467(3) 0.6195(2) 0.0315(8) Uani 1 1 d . . . . .
H6 H -0.4502 0.7126 0.5887 0.038 Uiso 1 1 calc R . . . .
C7 C -0.2692(4) 0.7104(2) 0.6571(2) 0.0272(7) Uani 1 1 d . . . . .
H7 H -0.2268 0.6513 0.6515 0.033 Uiso 1 1 calc R . . . .
C3A C 0.1673(4) 0.7319(2) 0.5781(2) 0.0256(7) Uani 1 1 d . . . . .
C7A C 0.1190(4) 0.8849(2) 0.5855(2) 0.0270(7) Uani 1 1 d . . . . .
H7A H 0.0775 0.9274 0.6174 0.032 Uiso 1 1 calc R . . . .
C4A C 0.2375(4) 0.7649(3) 0.4924(2) 0.0321(8) Uani 1 1 d . . . . .
H4A H 0.2788 0.7218 0.4611 0.039 Uiso 1 1 calc R . . . .
C10 C 0.4361(4) 0.7663(3) 0.8905(2) 0.0363(9) Uani 1 1 d . . . . .
H10 H 0.5183 0.7755 0.9209 0.044 Uiso 1 1 calc R . . . .
C13 C -0.1751(6) 1.0826(3) 0.8455(3) 0.0569(13) Uani 1 1 d . . . . .
H13 H -0.0844 1.1058 0.8665 0.068 Uiso 1 1 calc R . . . .
C1A C 0.0797(4) 0.4530(2) 0.7289(3) 0.0367(9) Uani 1 1 d . . . . .
C5 C -0.4648(4) 0.8325(3) 0.6263(2) 0.0321(8) Uani 1 1 d . . . . .
H5 H -0.5536 0.8593 0.5983 0.038 Uiso 1 1 calc R . . . .
N7 N 0.7568(5) 0.8167(3) -0.0132(3) 0.0717(13) Uani 1 1 d . . . . .
C17 C 0.7099(6) 0.8105(3) 0.1471(3) 0.0565(12) Uani 1 1 d . . . . .
H17A H 0.7165 0.8750 0.1517 0.085 Uiso 1 1 calc GR . . . .
H17B H 0.7902 0.7702 0.1779 0.085 Uiso 1 1 calc GR . . . .
H17C H 0.6038 0.7848 0.1725 0.085 Uiso 1 1 calc GR . . . .
C8 C 0.3281(4) 0.6827(2) 0.8074(2) 0.0281(7) Uani 1 1 d . . . . .
H8 H 0.3371 0.6334 0.7802 0.034 Uiso 1 1 calc R . . . .
C13A C 0.1944(5) 0.3928(3) 0.6083(3) 0.0479(11) Uani 1 1 d . . . . .
H13A H 0.2258 0.3373 0.6553 0.058 Uiso 1 1 calc R . . . .
C8A C -0.1595(4) 0.6309(3) 0.9202(2) 0.0405(10) Uani 1 1 d . . . . .
H8A H -0.1771 0.6925 0.9270 0.049 Uiso 1 1 calc R . . . .
C11A C -0.1061(5) 0.4524(3) 0.9032(3) 0.0484(11) Uani 1 1 d . . . . .
H11A H -0.0860 0.3908 0.8965 0.058 Uiso 1 1 calc R . . . .
C10A C -0.1913(6) 0.4642(4) 0.9760(3) 0.0582(13) Uani 1 1 d . . . . .
H10A H -0.2314 0.4101 1.0210 0.070 Uiso 1 1 calc R . . . .
C15A C 0.3337(8) 0.4185(4) 0.5382(4) 0.0773(17) Uani 1 1 d . . . . .
H15A H 0.2997 0.4643 0.4871 0.116 Uiso 1 1 calc GR . . . .
H15B H 0.3753 0.3613 0.5234 0.116 Uiso 1 1 calc GR . . . .
H15C H 0.4170 0.4467 0.5584 0.116 Uiso 1 1 calc GR . . . .
C14 C -0.3131(8) 1.0632(4) 0.9175(3) 0.087(2) Uani 1 1 d . . . . .
H14A H -0.4007 1.0356 0.9000 0.130 Uiso 1 1 calc GR . . . .
H14B H -0.3487 1.1227 0.9297 0.130 Uiso 1 1 calc GR . . . .
H14C H -0.2796 1.0187 0.9694 0.130 Uiso 1 1 calc GR . . . .
C14A C 0.0476(8) 0.3658(4) 0.5778(4) 0.086(2) Uani 1 1 d . . . . .
H14D H -0.0419 0.3559 0.6247 0.129 Uiso 1 1 calc GR . . . .
H14E H 0.0688 0.3072 0.5611 0.129 Uiso 1 1 calc GR . . . .
H14F H 0.0211 0.4169 0.5280 0.129 Uiso 1 1 calc GR . . . .
C16 C 0.7379(5) 0.8128(3) 0.0577(3) 0.0480(10) Uani 1 1 d . . . . .
C15 C -0.2129(6) 1.1576(3) 0.7657(3) 0.0617(13) Uani 1 1 d . . . . .
H15D H -0.1242 1.1626 0.7190 0.093 Uiso 1 1 calc GR . . . .
H15E H -0.2292 1.2187 0.7783 0.093 Uiso 1 1 calc GR . . . .
H15F H -0.3098 1.1402 0.7481 0.093 Uiso 1 1 calc GR . . . .
C9A C -0.2212(5) 0.5532(4) 0.9861(3) 0.0555(13) Uani 1 1 d . . . . .
H9A H -0.2826 0.5611 1.0371 0.067 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.843(3) . ?
Fe1 N1A 1.850(3) . ?
Fe1 N6A 1.978(3) . ?
Fe1 N5A 2.003(3) . ?
Fe1 N5 1.993(3) . ?
Fe1 N6 1.980(3) . ?
P2 F8 1.593(3) . ?
P2 F11 1.607(3) . ?
P2 F12 1.583(3) . ?
P2 F10 1.572(3) . ?
P2 F7 1.571(3) . ?
P2 F9 1.568(3) . ?
P1 F5 1.604(3) . ?
P1 F6 1.577(3) . ?
P1 F57 1.579(3) . ?
P1 F3 1.589(3) . ?
P1 F4 1.587(3) . ?
P1 F1 1.582(3) . ?
O1 C1 1.212(4) . ?
N1 N2 1.373(4) . ?
N1 C2 1.347(4) . ?
N1A N2A 1.378(4) . ?
N1A C2A 1.345(4) . ?
N6A C12A 1.351(5) . ?
N6A C8A 1.354(5) . ?
N3A N4A 1.361(4) . ?
N3A C1A 1.368(5) . ?
N3A C13A 1.492(5) . ?
N5A C3A 1.352(4) . ?
N5A C7A 1.340(4) . ?
N5 C3 1.360(4) . ?
N5 C7 1.349(4) . ?
N3 N4 1.374(4) . ?
N3 C1 1.372(5) . ?
N3 C13 1.492(5) . ?
O1A C1A 1.235(4) . ?
N2 C12 1.406(4) . ?
N2 C1 1.406(4) . ?
N2A C12A 1.390(5) . ?
N2A C1A 1.406(5) . ?
N4 C2 1.300(4) . ?
N6 C12 1.352(4) . ?
N6 C8 1.354(4) . ?
N4A C2A 1.312(4) . ?
C12 C11 1.383(5) . ?
C11 C10 1.368(5) . ?
C2A C3A 1.453(5) . ?
C3 C4 1.375(5) . ?
C3 C2 1.465(5) . ?
C5A C6A 1.374(5) . ?
C5A C4A 1.378(5) . ?
C12A C11A 1.393(5) . ?
C6A C7A 1.373(5) . ?
C9 C10 1.387(5) . ?
C9 C8 1.377(5) . ?
C4 C5 1.382(5) . ?
C6 C7 1.373(5) . ?
C6 C5 1.377(5) . ?
C3A C4A 1.393(5) . ?
C13 C14 1.507(7) . ?
C13 C15 1.507(7) . ?
N7 C16 1.132(5) . ?
C17 C16 1.435(6) . ?
C13A C15A 1.499(7) . ?
C13A C14A 1.520(6) . ?
C8A C9A 1.385(6) . ?
C11A C10A 1.351(7) . ?
C10A C9A 1.376(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1A 178.97(12) . . ?
N1 Fe1 N6A 101.99(13) . . ?
N1 Fe1 N5A 99.44(11) . . ?
N1 Fe1 N5 80.13(11) . . ?
N1 Fe1 N6 78.85(11) . . ?
N1A Fe1 N6A 78.91(12) . . ?
N1A Fe1 N5A 79.69(11) . . ?
N1A Fe1 N5 100.35(12) . . ?
N1A Fe1 N6 100.65(12) . . ?
N6A Fe1 N5A 158.35(12) . . ?
N6A Fe1 N5 94.01(11) . . ?
N6A Fe1 N6 91.61(11) . . ?
N5 Fe1 N5A 86.64(11) . . ?
N6 Fe1 N5A 95.50(11) . . ?
N6 Fe1 N5 158.94(12) . . ?
F8 P2 F11 89.96(14) . . ?
F12 P2 F8 179.68(17) . . ?
F12 P2 F11 90.11(14) . . ?
F10 P2 F8 88.52(16) . . ?
F10 P2 F11 88.20(18) . . ?
F10 P2 F12 91.79(17) . . ?
F7 P2 F8 89.68(15) . . ?
F7 P2 F11 88.05(17) . . ?
F7 P2 F12 90.01(16) . . ?
F7 P2 F10 175.8(2) . . ?
F9 P2 F8 88.45(14) . . ?
F9 P2 F11 178.14(16) . . ?
F9 P2 F12 91.48(15) . . ?
F9 P2 F10 92.7(2) . . ?
F9 P2 F7 90.98(19) . . ?
F6 P1 F5 90.00(15) . . ?
F6 P1 F57 90.62(16) . . ?
F6 P1 F3 178.98(19) . . ?
F6 P1 F4 90.94(19) . . ?
F6 P1 F1 90.13(18) . . ?
F57 P1 F5 179.23(18) . . ?
F57 P1 F3 90.29(16) . . ?
F57 P1 F4 91.10(19) . . ?
F57 P1 F1 91.56(19) . . ?
F3 P1 F5 89.10(16) . . ?
F4 P1 F5 89.35(18) . . ?
F4 P1 F3 88.6(2) . . ?
F1 P1 F5 87.97(18) . . ?
F1 P1 F3 90.31(19) . . ?
F1 P1 F4 177.1(2) . . ?
N2 N1 Fe1 120.8(2) . . ?
C2 N1 Fe1 121.6(2) . . ?
C2 N1 N2 117.4(3) . . ?
N2A N1A Fe1 120.1(2) . . ?
C2A N1A Fe1 121.6(2) . . ?
C2A N1A N2A 118.2(3) . . ?
C12A N6A Fe1 116.0(2) . . ?
C12A N6A C8A 118.4(3) . . ?
C8A N6A Fe1 125.6(3) . . ?
N4A N3A C1A 125.1(3) . . ?
N4A N3A C13A 117.1(3) . . ?
C1A N3A C13A 117.7(3) . . ?
C3A N5A Fe1 114.3(2) . . ?
C7A N5A Fe1 127.6(2) . . ?
C7A N5A C3A 118.0(3) . . ?
C3 N5 Fe1 114.0(2) . . ?
C7 N5 Fe1 127.6(2) . . ?
C7 N5 C3 118.0(3) . . ?
N4 N3 C13 115.3(3) . . ?
C1 N3 N4 125.1(3) . . ?
C1 N3 C13 119.5(3) . . ?
N1 N2 C12 111.5(3) . . ?
N1 N2 C1 121.4(3) . . ?
C1 N2 C12 127.0(3) . . ?
N1A N2A C12A 111.9(3) . . ?
N1A N2A C1A 120.3(3) . . ?
C12A N2A C1A 127.7(3) . . ?
C2 N4 N3 115.5(3) . . ?
C12 N6 Fe1 116.0(2) . . ?
C12 N6 C8 117.4(3) . . ?
C8 N6 Fe1 126.5(2) . . ?
C2A N4A N3A 115.9(3) . . ?
N6 C12 N2 112.7(3) . . ?
N6 C12 C11 123.1(3) . . ?
C11 C12 N2 124.2(3) . . ?
C10 C11 C12 118.4(3) . . ?
N1A C2A C3A 110.8(3) . . ?
N4A C2A N1A 125.2(3) . . ?
N4A C2A C3A 123.9(3) . . ?
N5 C3 C4 122.7(3) . . ?
N5 C3 C2 113.2(3) . . ?
C4 C3 C2 124.1(3) . . ?
C6A C5A C4A 119.3(3) . . ?
O1 C1 N3 123.7(3) . . ?
O1 C1 N2 122.0(3) . . ?
N3 C1 N2 114.4(3) . . ?
N6A C12A N2A 113.1(3) . . ?
N6A C12A C11A 122.1(4) . . ?
N2A C12A C11A 124.8(4) . . ?
C7A C6A C5A 119.4(3) . . ?
C8 C9 C10 118.7(3) . . ?
C3 C4 C5 118.6(3) . . ?
N1 C2 C3 110.4(3) . . ?
N4 C2 N1 126.1(3) . . ?
N4 C2 C3 123.5(3) . . ?
C7 C6 C5 120.2(3) . . ?
N5 C7 C6 121.6(3) . . ?
N5A C3A C2A 113.5(3) . . ?
N5A C3A C4A 122.2(3) . . ?
C4A C3A C2A 124.3(3) . . ?
N5A C7A C6A 122.6(3) . . ?
C5A C4A C3A 118.5(3) . . ?
C11 C10 C9 119.8(3) . . ?
N3 C13 C14 109.3(4) . . ?
N3 C13 C15 111.0(3) . . ?
C15 C13 C14 112.6(4) . . ?
N3A C1A N2A 115.3(3) . . ?
O1A C1A N3A 124.3(4) . . ?
O1A C1A N2A 120.4(4) . . ?
C6 C5 C4 118.9(3) . . ?
N6 C8 C9 122.5(3) . . ?
N3A C13A C15A 109.9(3) . . ?
N3A C13A C14A 108.9(4) . . ?
C15A C13A C14A 113.3(5) . . ?
N6A C8A C9A 121.7(4) . . ?
C10A C11A C12A 118.2(4) . . ?
C11A C10A C9A 121.2(4) . . ?
N7 C16 C17 178.0(6) . . ?
C10A C9A C8A 118.3(4) . . ?

_olex2_submission_special_instructions 'No special instructions were received'

####################################################################### 
# 
# 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_2H7A
_database_code_depnum_ccdc_archive 'CCDC 1820962'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-04-05 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            Fe(dipyvd)2PF6
_chemical_formula_moiety         'C30 H30 Fe N12 O2,F6 P, 2(C2 H3 N)'
_chemical_formula_sum            'C34 H36 F6 Fe N14 O2 P'
_chemical_formula_iupac          ?
_chemical_formula_weight         873.59
_chemical_absolute_configuration ad

_chemical_melting_point          ?

_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   16.3724(2)
_cell_length_b                   16.3724
_cell_length_c                   14.2233(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3812.63(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9895
_cell_measurement_theta_min      2.4880
_cell_measurement_theta_max      35.9844
_cell_measurement_temperature    105.(2)

_exptl_crystal_description       needle
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.054
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1796

_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L.; Herbst-Irmer, R.; Sheldrick, G. M.; Stalke, D. (2015). J. Appl.
Cryst. 48, 3-10.
;
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      105.(2)

_diffrn_source                   ' microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  'multilayer mirror'

_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'ω and φ scans'

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            28554
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         36.39
_diffrn_reflns_theta_full        36.39
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       21

_refine_special_details          
;                
Crystal found to be merohedral twin, twin law (0 1 0, 1 0 0, 0 0 -1).
The ratio between domains is 0.3309(14).
;

_reflns_number_total             9280
_reflns_number_gt                8756
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0982
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_number_reflns         9280
_refine_ls_number_parameters     269
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0471P)²+0.4136P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.301
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;

Flack x determined using 3767 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(9)

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       
'Bruker Instrument Service v6.2.6-RC1 (Bruker AXS Inc., 2017)'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2016)'
_computing_structure_solution    'XT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 758)'
_computing_publication_material  'APEX3 v2017.3-rc2 (Bruker AXS Inc., 2017)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe1 0.5 0.5 0.23721(3) 0.01539(7) Uani d T P S 1 . .
O O1 0.71007(12) 0.27248(12) 0.13811(13) 0.0237(4) Uani d . . . 1 . .
N N1 0.60625(12) 0.44161(12) 0.24107(15) 0.0174(3) Uani d . . . 1 . .
N N2 0.61942(12) 0.37056(12) 0.18859(13) 0.0165(3) Uani d . . . 1 . .
N N3 0.74835(12) 0.35760(12) 0.25655(17) 0.0198(3) Uani d . . . 1 . .
N N4 0.73574(12) 0.42449(13) 0.31522(15) 0.0188(3) Uani d . . . 1 . .
N N5 0.57245(13) 0.56691(13) 0.33926(12) 0.0180(3) Uani d . . . 1 . .
N N6 0.49023(12) 0.40197(12) 0.13894(13) 0.0173(3) Uani d . . . 1 . .
C C1 0.69456(13) 0.32927(13) 0.19129(16) 0.0174(4) Uani d . . . 1 . .
C C2 0.66623(13) 0.46159(14) 0.30253(15) 0.0160(3) Uani d . . . 1 . .
C C3 0.64733(15) 0.53562(14) 0.35710(16) 0.0164(3) Uani d . . . 1 . .
C C4 0.70122(17) 0.57152(16) 0.42015(18) 0.0217(4) Uani d . . . 1 . .
H H4 0.752896 0.547531 0.432782 0.026 Uiso calc U . R 1 . .
C C5 0.67759(19) 0.64348(17) 0.46431(18) 0.0247(5) Uani d . . . 1 . .
H H5 0.71327 0.669674 0.507503 0.03 Uiso calc U . R 1 . .
C C6 0.6014(2) 0.67682(18) 0.44483(19) 0.0253(5) Uani d . . . 1 . .
H H6 0.584601 0.726265 0.473957 0.03 Uiso calc U . R 1 . .
C C7 0.55027(18) 0.63680(16) 0.38220(19) 0.0232(5) Uani d . . . 1 . .
H H7 0.498015 0.659356 0.369203 0.028 Uiso calc U . R 1 . .
C C8 0.42111(16) 0.38576(17) 0.09022(18) 0.0222(4) Uani d . . . 1 . .
H H8 0.37767 0.42417 0.092596 0.027 Uiso calc U . R 1 . .
C C9 0.41096(18) 0.31584(18) 0.03721(19) 0.0239(5) Uani d . . . 1 . .
H H9 0.361778 0.30624 0.003542 0.029 Uiso calc U . R 1 . .
C C10 0.47526(18) 0.25950(16) 0.03450(18) 0.0232(4) Uani d . . . 1 . .
H H10 0.469731 0.210663 -0.001001 0.028 Uiso calc U . R 1 . .
C C11 0.54641(16) 0.27453(15) 0.08300(18) 0.0205(4) Uani d . . . 1 . .
H H11 0.590345 0.236646 0.081533 0.025 Uiso calc U . R 1 . .
C C12 0.55241(14) 0.34772(14) 0.13500(15) 0.0160(3) Uani d . . . 1 . .
C C13 0.83048(14) 0.32017(15) 0.2636(2) 0.0233(4) Uani d . . . 1 . .
H H13 0.82945 0.267378 0.228267 0.028 Uiso calc U . R 1 . .
C C14 0.8928(2) 0.3751(2) 0.2176(4) 0.0489(11) Uani d . . . 1 . .
H H14A 0.878198 0.383405 0.151507 0.073 Uiso calc U . R 1 . .
H H14B 0.946899 0.349544 0.221411 0.073 Uiso calc U . R 1 . .
H H14C 0.893947 0.427841 0.250069 0.073 Uiso calc U . R 1 . .
C C15 0.8493(3) 0.3013(3) 0.3657(3) 0.0566(13) Uani d . . . 1 . .
H H15A 0.856399 0.352415 0.400515 0.085 Uiso calc U . R 1 . .
H H15B 0.899629 0.269 0.36947 0.085 Uiso calc U . R 1 . .
H H15C 0.804068 0.27011 0.393092 0.085 Uiso calc U . R 1 . .
P P1 0.5 0 0.47769(7) 0.0410(3) Uani d T P S 1 . .
F F1 0.56099(19) 0.0768(3) 0.4769(2) 0.0658(9) Uani d . . . 1 . .
F F2 0.5763(2) -0.0605(3) 0.4743(3) 0.0751(11) Uani d . . . 1 . .
F F3 0.5 0 0.3646(2) 0.0793(15) Uani d T P S 1 . .
F F4 0.5 0 0.5879(2) 0.0791(16) Uani d T P S 1 . .
N N7 0.6005(2) 0.22706(19) 0.3331(2) 0.0371(6) Uani d . . . 1 . .
C C16 0.6229(2) 0.16856(18) 0.2985(2) 0.0280(5) Uani d . . . 1 . .
C C17 0.6514(2) 0.0943(2) 0.2532(3) 0.0380(7) Uani d . . . 1 . .
H H17A 0.635713 0.094995 0.186746 0.057 Uiso calc U . R 1 . .
H H17B 0.626697 0.0468 0.284082 0.057 Uiso calc U . R 1 . .
H H17C 0.71099 0.090957 0.258367 0.057 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N1 2_665 1.9857(18) ?
Fe1 N1 . 1.9857(18) ?
Fe1 N6 . 2.1343(19) ?
Fe1 N6 2_665 2.134(2) ?
Fe1 N5 . 2.1712(19) ?
Fe1 N5 2_665 2.1712(19) ?
O1 C1 . 1.225(3) ?
N1 C2 . 1.355(3) ?
N1 N2 . 1.399(3) ?
N2 C12 . 1.387(3) ?
N2 C1 . 1.404(3) ?
N3 C1 . 1.361(3) ?
N3 N4 . 1.392(3) ?
N3 C13 . 1.481(3) ?
N4 C2 . 1.303(3) ?
N5 C7 . 1.347(3) ?
N5 C3 . 1.353(3) ?
N6 C12 . 1.352(3) ?
N6 C8 . 1.353(3) ?
C2 C3 . 1.472(3) ?
C3 C4 . 1.389(3) ?
C4 C5 . 1.390(4) ?
C4 H4 . 0.95 ?
C5 C6 . 1.389(4) ?
C5 H5 . 0.95 ?
C6 C7 . 1.387(4) ?
C6 H6 . 0.95 ?
C7 H7 . 0.95 ?
C8 C9 . 1.381(4) ?
C8 H8 . 0.95 ?
C9 C10 . 1.400(4) ?
C9 H9 . 0.95 ?
C10 C11 . 1.376(4) ?
C10 H10 . 0.95 ?
C11 C12 . 1.411(3) ?
C11 H11 . 0.95 ?
C13 C14 . 1.509(5) ?
C13 C15 . 1.516(5) ?
C13 H13 . 1.0 ?
C14 H14A . 0.98 ?
C14 H14B . 0.98 ?
C14 H14C . 0.98 ?
C15 H15A . 0.98 ?
C15 H15B . 0.98 ?
C15 H15C . 0.98 ?
P1 F4 . 1.568(3) ?
P1 F2 2_655 1.594(3) ?
P1 F2 . 1.594(3) ?
P1 F1 2_655 1.605(4) ?
P1 F1 . 1.606(4) ?
P1 F3 . 1.609(4) ?
N7 C16 . 1.138(4) ?
C16 C17 . 1.453(4) ?
C17 H17A . 0.98 ?
C17 H17B . 0.98 ?
C17 H17C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Fe1 N1 2_665 . 176.83(13) ?
N1 Fe1 N6 2_665 . 108.33(8) ?
N1 Fe1 N6 . . 73.84(8) ?
N1 Fe1 N6 2_665 2_665 73.84(8) ?
N1 Fe1 N6 . 2_665 108.33(8) ?
N6 Fe1 N6 . 2_665 98.18(10) ?
N1 Fe1 N5 2_665 . 102.55(9) ?
N1 Fe1 N5 . . 75.27(8) ?
N6 Fe1 N5 . . 149.11(8) ?
N6 Fe1 N5 2_665 . 91.00(7) ?
N1 Fe1 N5 2_665 2_665 75.27(8) ?
N1 Fe1 N5 . 2_665 102.55(9) ?
N6 Fe1 N5 . 2_665 91.00(7) ?
N6 Fe1 N5 2_665 2_665 149.11(8) ?
N5 Fe1 N5 . 2_665 96.09(10) ?
C2 N1 N2 . . 115.68(18) ?
C2 N1 Fe1 . . 122.45(16) ?
N2 N1 Fe1 . . 121.38(14) ?
C12 N2 N1 . . 113.29(17) ?
C12 N2 C1 . . 125.32(19) ?
N1 N2 C1 . . 121.39(19) ?
C1 N3 N4 . . 125.51(18) ?
C1 N3 C13 . . 119.5(2) ?
N4 N3 C13 . . 114.8(2) ?
C2 N4 N3 . . 114.4(2) ?
C7 N5 C3 . . 118.8(2) ?
C7 N5 Fe1 . . 125.76(19) ?
C3 N5 Fe1 . . 115.44(16) ?
C12 N6 C8 . . 118.7(2) ?
C12 N6 Fe1 . . 117.68(15) ?
C8 N6 Fe1 . . 123.06(16) ?
O1 C1 N3 . . 123.1(2) ?
O1 C1 N2 . . 122.0(2) ?
N3 C1 N2 . . 114.93(19) ?
N4 C2 N1 . . 127.6(2) ?
N4 C2 C3 . . 119.6(2) ?
N1 C2 C3 . . 112.75(19) ?
N5 C3 C4 . . 122.5(2) ?
N5 C3 C2 . . 113.8(2) ?
C4 C3 C2 . . 123.8(2) ?
C3 C4 C5 . . 118.3(3) ?
C3 C4 H4 . . 120.9 ?
C5 C4 H4 . . 120.9 ?
C6 C5 C4 . . 119.5(2) ?
C6 C5 H5 . . 120.2 ?
C4 C5 H5 . . 120.2 ?
C7 C6 C5 . . 119.0(2) ?
C7 C6 H6 . . 120.5 ?
C5 C6 H6 . . 120.5 ?
N5 C7 C6 . . 122.0(3) ?
N5 C7 H7 . . 119.0 ?
C6 C7 H7 . . 119.0 ?
N6 C8 C9 . . 122.9(2) ?
N6 C8 H8 . . 118.6 ?
C9 C8 H8 . . 118.6 ?
C8 C9 C10 . . 118.1(2) ?
C8 C9 H9 . . 121.0 ?
C10 C9 H9 . . 121.0 ?
C11 C10 C9 . . 120.3(2) ?
C11 C10 H10 . . 119.8 ?
C9 C10 H10 . . 119.8 ?
C10 C11 C12 . . 118.3(2) ?
C10 C11 H11 . . 120.9 ?
C12 C11 H11 . . 120.9 ?
N6 C12 N2 . . 113.31(19) ?
N6 C12 C11 . . 121.8(2) ?
N2 C12 C11 . . 124.9(2) ?
N3 C13 C14 . . 109.8(2) ?
N3 C13 C15 . . 109.5(3) ?
C14 C13 C15 . . 113.5(4) ?
N3 C13 H13 . . 107.9 ?
C14 C13 H13 . . 108.0 ?
C15 C13 H13 . . 108.0 ?
C13 C14 H14A . . 109.5 ?
C13 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C13 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
C13 C15 H15A . . 109.5 ?
C13 C15 H15B . . 109.5 ?
H15A C15 H15B . . 109.5 ?
C13 C15 H15C . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
F4 P1 F2 . 2_655 91.74(15) ?
F4 P1 F2 . . 91.74(15) ?
F2 P1 F2 2_655 . 176.5(3) ?
F4 P1 F1 . 2_655 90.42(13) ?
F2 P1 F1 2_655 2_655 89.9(2) ?
F2 P1 F1 . 2_655 90.0(2) ?
F4 P1 F1 . . 90.42(13) ?
F2 P1 F1 2_655 . 90.0(2) ?
F2 P1 F1 . . 89.9(2) ?
F1 P1 F1 2_655 . 179.2(3) ?
F4 P1 F3 . . 180.0 ?
F2 P1 F3 2_655 . 88.26(15) ?
F2 P1 F3 . . 88.26(15) ?
F1 P1 F3 2_655 . 89.58(12) ?
F1 P1 F3 . . 89.58(12) ?
N7 C16 C17 . . 179.4(4) ?
C16 C17 H17A . . 109.5 ?
C16 C17 H17B . . 109.5 ?
H17A C17 H17B . . 109.5 ?
C16 C17 H17C . . 109.5 ?
H17A C17 H17C . . 109.5 ?
H17B C17 H17C . . 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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 N1 N2 C12 . . . . 172.93(19) ?
Fe1 N1 N2 C12 . . . . 0.8(3) ?
C2 N1 N2 C1 . . . . -7.9(3) ?
Fe1 N1 N2 C1 . . . . 179.98(16) ?
C1 N3 N4 C2 . . . . -1.2(3) ?
C13 N3 N4 C2 . . . . 174.1(2) ?
N4 N3 C1 O1 . . . . 176.4(2) ?
C13 N3 C1 O1 . . . . 1.3(4) ?
N4 N3 C1 N2 . . . . -3.1(3) ?
C13 N3 C1 N2 . . . . -178.2(2) ?
C12 N2 C1 O1 . . . . 7.3(4) ?
N1 N2 C1 O1 . . . . -171.7(2) ?
C12 N2 C1 N3 . . . . -173.2(2) ?
N1 N2 C1 N3 . . . . 7.8(3) ?
N3 N4 C2 N1 . . . . 1.1(3) ?
N3 N4 C2 C3 . . . . -177.1(2) ?
N2 N1 C2 N4 . . . . 3.3(3) ?
Fe1 N1 C2 N4 . . . . 175.32(19) ?
N2 N1 C2 C3 . . . . -178.43(19) ?
Fe1 N1 C2 C3 . . . . -6.4(3) ?
C7 N5 C3 C4 . . . . 2.0(3) ?
Fe1 N5 C3 C4 . . . . 179.61(19) ?
C7 N5 C3 C2 . . . . -177.0(2) ?
Fe1 N5 C3 C2 . . . . 0.6(2) ?
N4 C2 C3 N5 . . . . -178.3(2) ?
N1 C2 C3 N5 . . . . 3.3(3) ?
N4 C2 C3 C4 . . . . 2.8(4) ?
N1 C2 C3 C4 . . . . -175.7(2) ?
N5 C3 C4 C5 . . . . -1.8(4) ?
C2 C3 C4 C5 . . . . 177.1(2) ?
C3 C4 C5 C6 . . . . 0.4(4) ?
C4 C5 C6 C7 . . . . 0.6(4) ?
C3 N5 C7 C6 . . . . -0.8(4) ?
Fe1 N5 C7 C6 . . . . -178.2(2) ?
C5 C6 C7 N5 . . . . -0.4(4) ?
C12 N6 C8 C9 . . . . 0.6(4) ?
Fe1 N6 C8 C9 . . . . -170.4(2) ?
N6 C8 C9 C10 . . . . 0.2(4) ?
C8 C9 C10 C11 . . . . -0.5(4) ?
C9 C10 C11 C12 . . . . 0.0(4) ?
C8 N6 C12 N2 . . . . -179.3(2) ?
Fe1 N6 C12 N2 . . . . -7.9(3) ?
C8 N6 C12 C11 . . . . -1.1(3) ?
Fe1 N6 C12 C11 . . . . 170.32(18) ?
N1 N2 C12 N6 . . . . 4.6(3) ?
C1 N2 C12 N6 . . . . -174.5(2) ?
N1 N2 C12 C11 . . . . -173.5(2) ?
C1 N2 C12 C11 . . . . 7.4(4) ?
C10 C11 C12 N6 . . . . 0.8(4) ?
C10 C11 C12 N2 . . . . 178.8(2) ?
C1 N3 C13 C14 . . . . 102.6(3) ?
N4 N3 C13 C14 . . . . -73.0(3) ?
C1 N3 C13 C15 . . . . -132.2(3) ?
N4 N3 C13 C15 . . . . 52.3(4) ?


# start Validation Reply Form
_vrf_PLAT220_3_2H7A              
;
PROBLEM: Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 3.5 Ratio
RESPONSE: This difference is between the C of the aromatic ring system
and the terminal C of the isopropyl functional group.
;
_vrf_PLAT242_3_2H7A              
;
PROBLEM: Low \"i?1/2MainMol\"i?1/2 Ueq as Compared to Neighbors of C13 Check
RESPONSE: C13 is the "pivot atom" of the isopropyl group. The terminal
atoms show much more apparent motion than this atom.
;
# end Validation Reply Form


####################################################################### 
# 
# 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_sjsu001_0m_tet
_database_code_depnum_ccdc_archive 'CCDC 1824292'
_audit_update_record             
;
2018-02-15 deposited with the CCDC.
2018-04-05 downloaded from the CCDC.
;
_audit_creation_date             2018-02-06
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_chemical_formula_moiety         'C30 H30 Fe N12 O2, 2(F6 P)'
_chemical_formula_sum            'C30 H30 F12 Fe N12 O2 P2'
_chemical_formula_weight         936.45

_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'
_chemical_absolute_configuration unk
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 y,-x,-z
3 -y,x,-z
4 x+1/2,-y+1/2,-z+1/2
5 -x+1/2,y+1/2,-z+1/2
6 -x,-y,z
7 -y+1/2,-x+1/2,z+1/2
8 y+1/2,x+1/2,z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00400 0.00200 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom
F 0.02200 0.01300 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom
H -0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom
O 0.01400 0.00700 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom
N 0.00800 0.00400 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom
P 0.12000 0.11500 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom
Fe 0.36800 0.99500 11.76950 7.35730 3.52220 2.30450 4.76110 0.30720 15.35350
76.88050 1.03690004349
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' custom
_cell_length_a                   15.8913(15)
_cell_length_b                   15.8913(15)
_cell_length_c                   14.8198(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3742.5(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150
_cell_measurement_reflns_used    4496
_cell_measurement_theta_max      21.16
_cell_measurement_theta_min      2.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014.5 (Sheldrick)'
_exptl_absorpt_coefficient_mu    0.757
_exptl_crystal_recrystallization_method 'Recystallized from acetone/ether'
_exptl_crystal_description       needle
_exptl_crystal_colour            red
_diffrn_ambient_temperature      150
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.6618
_exptl_crystal_F_000             1900.0303
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.002
_diffrn_reflns_av_R_equivalents  0.1032
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27667
_diffrn_reflns_theta_full        22.9012
_diffrn_reflns_theta_max         22.90
_diffrn_reflns_theta_min         2.05
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.9960
_diffrn_measured_fraction_theta_max 0.9960
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'ALS beamline 11.3.1'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS'
_diffrn_measurement_method       'omega-phi scans'
_diffrn_source_target            Mo
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.993
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              14
_reflns_limit_l_min              -14
_reflns_number_gt                1530
_reflns_number_total             1985
_reflns_threshold_expression     I>=2u(I)
_computing_data_collection       'Bruker APEX2 v2014.11.0'
_computing_cell_refinement       'Bruker SAINT v8.34A'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.4147
_refine_diff_density_min         -0.3647
_refine_diff_density_rms         0.0831
_refine_ls_abs_structure_details 
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.06(6)
_refine_ls_d_res_high            0.9956
_refine_ls_d_res_low             10.8382
_refine_ls_goodness_of_fit_ref   1.1493
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    44
_refine_ls_number_parameters     277
_refine_ls_number_reflns         1985
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0539
_refine_ls_restrained_S_all      1.1473
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1589
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C1B, N4A}
{n4b, C1A}
{C2B, n2a}
{N2B, C2A}
3. Restrained distances
 C13A-C14A
 1.5 with sigma of 0.02
 C13A-C15A
 1.5 with sigma of 0.02
 C13B-C14B
 1.5 with sigma of 0.02
 C13B-C15B
 1.5 with sigma of 0.02
 C14B-C15B
 2.44 with sigma of 0.04
 C14A-C15A
 2.44 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C2A) = Uanis(N2B)
Uanis(C2B) = Uanis(n2a)
Uanis(C1B) = Uanis(N4A)
Uanis(C1A) = Uanis(n4b)
5. Others
 Fixed Sof: C2B(0.5) N2B(0.5) C1B(0.5) n4b(0.5) O1B(0.5) C13A(0.5) H13A(0.5)
 O1A(0.5) C15B(0.5) H15a(0.5) H15b(0.5) H15c(0.5) C14B(0.5) H14a(0.5) H14b(0.5)
 H14c(0.5) C15A(0.5) H15d(0.5) H15e(0.5) H15f(0.5) C14A(0.5) H14d(0.5)
 H14e(0.5) H14f(0.5) C13B(0.5) H13B(0.5) N4A(0.5) C1A(0.5) n2a(0.5) C2A(0.5)
6.a Ternary CH refined with riding coordinates:
 C13A(H13A), C13B(H13B)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C6(H6), C8(H8), C5(H5), C10(H10), C4(H4), C7(H7), C11(H11)
6.c Idealised Me refined as rotating group:
 C15B(H15a,H15b,H15c), C14B(H14a,H14b,H14c), C15A(H15d,H15e,H15f), C14A(H14d,
 H14e,H14f)
;
_atom_sites_solution_primary     direct
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_group
Fe1 Fe 0.0 0.0 0.251441(3) 0.0380(3) Uani 1.000000 2 S T P .
P1 P 0.188377(3) 0.316949(3) 0.342237(3) 0.0642(3) Uani 1.000000 1 . . . .
N1 N 0.114147(3) 0.028644(3) 0.250979(3) 0.0384(4) Uani 1.000000 1 . . . .
F6 F 0.171481(3) 0.219328(3) 0.336054(3) 0.0939(4) Uani 1.000000 1 . . . .
F1 F 0.264772(3) 0.304814(3) 0.277106(3) 0.1210(4) Uani 1.000000 1 . . . .
C9 C -0.056974(3) 0.191321(3) 0.056840(3) 0.0568(4) Uani 1.000000 1 . . . .
H9 H -0.105286(3) 0.211731(3) 0.026075(3) 0.0682(5) Uiso 1.000000 1 R . . .
N6 N -0.000592(3) 0.090781(3) 0.159709(3) 0.0413(4) Uani 1.000000 1 . . . .
C6 C 0.040476(3) -0.196754(3) 0.444237(3) 0.0507(4) Uani 1.000000 1 . . . .
H6 H 0.007398(3) -0.238028(3) 0.474110(3) 0.0609(5) Uiso 1.000000 1 R . . .
N3 N 0.276943(3) 0.069824(3) 0.248388(3) 0.0624(4) Uani 1.000000 1 . . . .
C12 C 0.075448(3) 0.127832(3) 0.144757(3) 0.0479(4) Uani 1.000000 1 . . . .
F4 F 0.114952(3) 0.325902(3) 0.412585(3) 0.1235(4) Uani 1.000000 1 . . . .
N5 N 0.045170(3) -0.079597(3) 0.343658(3) 0.0394(4) Uani 1.000000 1 . . . .
F2 F 0.247258(3) 0.296074(3) 0.424860(3) 0.0970(4) Uani 1.000000 1 . . . .
C8 C -0.064205(3) 0.123492(3) 0.113849(3) 0.0533(4) Uani 1.000000 1 . . . .
H8 H -0.118143(3) 0.098539(3) 0.120786(3) 0.0640(5) Uiso 1.000000 1 R . . .
C2B C 0.143057(3) 0.090449(3) 0.195613(3) 0.0468(4) Uani 0.500000 1 . . . 2
N2B N 0.170004(3) -0.009611(3) 0.306818(3) 0.0412(4) Uani 0.500000 1 . . . 2
F5 F 0.131550(3) 0.334877(3) 0.263772(3) 0.1870(4) Uani 1.000000 1 . . . .
C1B C 0.251180(3) 0.012411(3) 0.311359(3) 0.0587(4) Uani 0.500000 1 . . . 2
C5 C 0.125653(3) -0.192995(3) 0.457851(3) 0.0580(4) Uani 1.000000 1 . . . .
H5 H 0.152585(3) -0.232622(3) 0.496187(3) 0.0696(5) Uiso 1.000000 1 R . . .
n4b N 0.226994(3) 0.109010(3) 0.188506(3) 0.0509(4) Uani 0.500000 1 . . . 2
C10 C 0.018830(3) 0.229576(3) 0.044025(3) 0.0628(4) Uani 1.000000 1 . . . .
H10 H 0.023901(3) 0.276531(3) 0.004724(3) 0.0753(5) Uiso 1.000000 1 R . . .
C4 C 0.172425(3) -0.130579(3) 0.415008(3) 0.0556(4) Uani 1.000000 1 . . . .
H4 H 0.231466(3) -0.126560(3) 0.424091(3) 0.0668(5) Uiso 1.000000 1 R . . .
F3 F 0.216777(3) 0.413680(3) 0.354835(3) 0.1067(4) Uani 1.000000 1 . . . .
C7 C 0.003399(3) -0.139433(3) 0.386246(3) 0.0487(4) Uani 1.000000 1 . . . .
H7 H -0.055558(3) -0.143372(3) 0.376514(3) 0.0584(5) Uiso 1.000000 1 R . . .
O1B O 0.304201(3) -0.020764(3) 0.364559(3) 0.0727(4) Uani 0.500000 1 . . . 2
C13A C 0.366252(3) 0.099048(3) 0.256640(3) 0.078245(3) Uiso 0.500000 1 D . . 1
H13A H 0.369586(3) 0.160759(3) 0.243925(3) 0.093894(3) Uiso 0.500000 1 R . . 1
C11 C 0.086705(3) 0.199243(3) 0.088477(3) 0.0634(4) Uani 1.000000 1 . . . .
H11 H 0.140347(3) 0.224977(3) 0.082218(3) 0.0761(5) Uiso 1.000000 1 R . . .
C3 C 0.131075(3) -0.074488(3) 0.358884(3) 0.0457(4) Uani 1.000000 1 . . . .
O1A O 0.251988(3) 0.160235(3) 0.134611(3) 0.0662(4) Uani 0.500000 1 . . . 1
C15B C 0.397808(3) 0.089097(3) 0.135722(3) 0.058027(3) Uiso 0.500000 1 D . . 2
H15a H 0.396826(3) 0.033392(3) 0.107371(3) 0.087040(4) Uiso 0.500000 1 GR . . 2
H15b H 0.357817(3) 0.126206(3) 0.104890(3) 0.087040(4) Uiso 0.500000 1 GR . . 2
H15c H 0.454565(3) 0.112846(3) 0.131219(3) 0.087040(4) Uiso 0.500000 1 GR . . 2
C14B C 0.393243(3) 0.160655(3) 0.281883(3) 0.130283(3) Uiso 0.500000 1 D . . 2
H14a H 0.340655(3) 0.186318(3) 0.302756(3) 0.195425(4) Uiso 0.500000 1 GR . . 2
H14b H 0.429022(3) 0.147755(3) 0.333937(3) 0.195425(4) Uiso 0.500000 1 GR . . 2
H14c H 0.422669(3) 0.199903(3) 0.241808(3) 0.195425(4) Uiso 0.500000 1 GR . . 2
C15A C 0.398375(3) 0.081413(3) 0.349976(3) 0.120500(3) Uiso 0.500000 1 D . . 1
H15d H 0.403201(3) 0.134358(3) 0.383486(3) 0.180750(4) Uiso 0.500000 1 GR . . 1
H15e H 0.359138(3) 0.043829(3) 0.381255(3) 0.180750(4) Uiso 0.500000 1 GR . . 1
H15f H 0.453764(3) 0.054536(3) 0.346134(3) 0.180750(4) Uiso 0.500000 1 GR . . 1
C14A C 0.421088(3) 0.051615(3) 0.191184(3) 0.133360(3) Uiso 0.500000 1 D . . 1
H14d H 0.476942(3) 0.077679(3) 0.189044(3) 0.200039(4) Uiso 0.500000 1 GR . . 1
H14e H 0.426403(3) -0.007003(3) 0.210922(3) 0.200039(4) Uiso 0.500000 1 GR . .
1
H14f H 0.395597(3) 0.053305(3) 0.130997(3) 0.200039(4) Uiso 0.500000 1 GR . . 1
C13B C 0.374000(3) 0.081324(3) 0.231776(3) 0.085854(3) Uiso 0.500000 1 D . . 2
H13B H 0.405335(3) 0.033377(3) 0.259719(3) 0.103025(3) Uiso 0.500000 1 R . . 2
N4A N 0.251180(3) 0.012411(3) 0.311359(3) 0.0587(4) Uani 0.500000 1 . . . 1
C1A C 0.226994(3) 0.109010(3) 0.188506(3) 0.0509(4) Uani 0.500000 1 . . . 1
n2a N 0.143057(3) 0.090449(3) 0.195613(3) 0.0468(4) Uani 0.500000 1 . . . 1
C2A C 0.170004(3) -0.009611(3) 0.306818(3) 0.0412(4) Uani 0.500000 1 . . . 1


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.87020(18) . ?
Fe1 N1 1.87020(18) 6 ?
Fe1 N6 1.98226(15) 6 ?
Fe1 N6 1.98226(15) . ?
Fe1 N5 1.99573(15) . ?
Fe1 N5 1.99573(15) 6 ?
P1 F6 1.57706(16) . ?
P1 F1 1.56292(13) . ?
P1 F4 1.57118(13) . ?
P1 F2 1.57634(13) . ?
P1 F5 1.49963(13) . ?
P1 F3 1.61291(16) . ?
N1 C2B 1.35976(12) . ?
N1 N2B 1.35730(12) . ?
N1 n2a 1.35976(12) . ?
N1 C2A 1.35730(12) . ?
C9 C8 1.37435(12) . ?
C9 C10 1.36264(14) . ?
N6 C12 1.36233(14) . ?
N6 C8 1.32439(12) . ?
C6 C5 1.36983(14) . ?
C6 C7 1.38403(12) . ?
N3 C1B 1.36782(12) . ?
N3 n4b 1.34364(11) . ?
N3 C13A 1.49830(15) . ?
N3 C13B 1.57254(16) . ?
N3 N4A 1.36782(12) . ?
N3 C1A 1.34364(11) . ?
C12 C2B 1.44058(12) . ?
C12 C11 1.41966(12) . ?
C12 n2a 1.44058(12) . ?
N5 C7 1.32027(12) . ?
N5 C3 1.38606(14) . ?
C2B n4b 1.37014(14) . ?
N2B C1B 1.33831(14) . ?
N2B C3 1.42863(12) . ?
C1B O1B 1.26865(11) . ?
C5 C4 1.39262(13) . ?
C10 C11 1.35269(12) . ?
C4 C3 1.38495(12) . ?
C13A C15A 1.50081(15) . ?
C13A C14A 1.50617(12) . ?
C3 C2A 1.42863(12) . ?
O1A C1A 1.20763(11) . ?
C15B C13B 1.47810(16) . ?
C14B C13B 1.49473(13) . ?
N4A C2A 1.33831(14) . ?
C1A n2a 1.37014(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 179.581(4) 6 . ?
N6 Fe1 N1 99.789(2) 6 . ?
N6 Fe1 N1 79.919(2) . . ?
N6 Fe1 N1 99.789(2) . 6 ?
N6 Fe1 N1 79.919(2) 6 6 ?
N6 Fe1 N6 93.402(3) 6 . ?
N5 Fe1 N1 101.367(2) . 6 ?
N5 Fe1 N1 78.925(2) . . ?
N5 Fe1 N1 78.925(2) 6 6 ?
N5 Fe1 N1 101.367(2) 6 . ?
N5 Fe1 N6 158.8437(19) 6 6 ?
N5 Fe1 N6 90.3815(18) . 6 ?
N5 Fe1 N6 158.8437(19) . . ?
N5 Fe1 N6 90.3815(18) 6 . ?
N5 Fe1 N5 93.563(3) 6 . ?
F1 P1 F6 88.567(3) . . ?
F4 P1 F6 90.068(3) . . ?
F4 P1 F1 176.219(4) . . ?
F2 P1 F6 86.513(3) . . ?
F2 P1 F1 89.581(3) . . ?
F2 P1 F4 86.816(3) . . ?
F5 P1 F6 92.253(3) . . ?
F5 P1 F1 90.705(3) . . ?
F5 P1 F4 92.872(3) . . ?
F5 P1 F2 178.726(4) . . ?
F3 P1 F6 172.688(4) . . ?
F3 P1 F1 88.380(3) . . ?
F3 P1 F4 92.562(3) . . ?
F3 P1 F2 86.822(3) . . ?
F3 P1 F5 94.427(3) . . ?
N2B N1 C2B 118.065(4) . . ?
C2A N1 n2a 118.065(4) . . ?
C10 C9 C8 120.630(4) . . ?
C12 N6 Fe1 114.953(3) . . ?
C8 N6 Fe1 129.882(4) . . ?
C8 N6 C12 115.083(4) . . ?
C7 C6 C5 118.909(4) . . ?
n4b N3 C1B 125.657(4) . . ?
C13B N3 C1B 118.548(4) . . ?
C13B N3 n4b 114.971(4) . . ?
N4A N3 C13A 115.759(4) . . ?
C1A N3 C13A 118.024(4) . . ?
C1A N3 N4A 125.657(4) . . ?
C11 C12 N6 123.560(4) . . ?
C7 N5 Fe1 127.084(4) . 6 ?
C3 N5 Fe1 115.379(3) . 6 ?
C3 N5 C7 117.358(4) . . ?
N6 C8 C9 124.020(4) . . ?
C12 C2B N1 111.197(4) . . ?
C3 N2B N1 111.674(4) . . ?
O1B C1B N2B 124.247(4) . . ?
C4 C5 C6 119.426(4) . . ?
C11 C10 C9 118.559(4) . . ?
C3 C4 C5 118.619(4) . . ?
N5 C7 C6 123.836(4) . . ?
C14A C13A C15A 107.658(4) . . ?
C10 C11 C12 118.066(4) . . ?
C4 C3 N5 121.828(4) . . ?
C14B C13B C15B 110.830(4) . . ?
n2a C1A O1A 121.074(4) . . ?
C12 n2a N1 111.197(4) . . ?
C3 C2A N1 111.674(4) . . ?

_olex2_submission_original_sample_id sjsu001
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
C13A C15A 1 1.5000 0.0200 -0.0008
C13A C14A 1 1.5000 0.0200 -0.0062
C14B C15B 1 2.4400 0.0400 -0.0075
C14A C15A 1 2.4400 0.0400 0.0126
C13B C15B 1 1.5000 0.0200 0.0219
C13B C14B 1 1.5000 0.0200 0.0053



