# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_se20006
_database_code_depnum_ccdc_archive 'CCDC 2073339'
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2021-03-26 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_audit_creation_date             2020-07-10
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
g.s.nichol@ed.ac.uk
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H42 Fe N4 O2 P4'
_chemical_formula_sum            'C20 H42 Fe N4 O2 P4'
_chemical_formula_weight         550.30
_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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   10.4604(6)
_cell_length_b                   17.5579(11)
_cell_length_c                   14.6107(9)
_cell_angle_alpha                90
_cell_angle_beta                 91.861(2)
_cell_angle_gamma                90
_cell_volume                     2682.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9509
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      35.31
_cell_measurement_theta_min      2.70
_shelx_estimated_absorpt_T_max   0.833
_shelx_estimated_absorpt_T_min   0.684
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.6628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1129 before and 0.0479 after correction.
The Ratio of minimum to maximum transmission is 0.8873.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 1.00 0.1770
1.00 0.00 -1.00 0.1430
1.00 2.00 -2.00 0.1800
-1.00 -2.00 2.00 0.1600
0.00 2.00 -1.00 0.2120
0.00 -2.00 1.00 0.1620
-1.00 2.00 0.00 0.2150
1.00 -2.00 0.00 0.1700
-1.00 0.00 -1.00 0.1150
1.00 0.00 1.00 0.0530
1.00 -1.00 -2.00 0.1850
-1.00 1.00 2.00 0.2060
0.00 -2.00 -1.00 0.1900
0.00 2.00 1.00 0.2350
-1.00 -2.00 0.00 0.2040
1.00 2.00 -1.00 0.1910
0.00 1.00 0.00 0.2430
-1.00 1.00 -2.00 0.1340
0.00 -1.00 -1.00 0.1760
-2.00 -2.00 -1.00 0.1740

_exptl_crystal_recrystallization_method 
'The material was recrystallised from pentane by slow cooling'
_exptl_crystal_size_max          0.498
_exptl_crystal_size_mid          0.368
_exptl_crystal_size_min          0.23
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            241200
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.598
_diffrn_reflns_theta_min         2.267
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10664
_reflns_number_total             11736
_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 V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         11736
_refine_ls_number_restraints     262
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.193
_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)+(0.0155P)²+2.6678P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0932
_refine_special_details          
;
The dmpe ligands were modelled as disodered (approx 2:1 ratio) consistent with peaks in a difference map.  Displacement ellipsoid and geometric restraints were used.  Despite this , some of the minor component ellipsoids remain rather elongated.





#===============================================================================
#>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text

213_ALERT_2_B Atom C1A             has ADP max/min Ratio .....        4.2 prolat
220_ALERT_2_B NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        6.6 Ratio

See above for a comment on disorder and ellipsoids

#===============================================================================
213_ALERT_2_C Atom C3              has ADP max/min Ratio .....        3.1 prolat
213_ALERT_2_C Atom C2A             has ADP max/min Ratio .....        3.5 prolat
213_ALERT_2_C Atom C3A             has ADP max/min Ratio .....        3.8 prolat
213_ALERT_2_C Atom C4A             has ADP max/min Ratio .....        3.1 prolat
213_ALERT_2_C Atom C6A             has ADP max/min Ratio .....        3.2 prolat
222_ALERT_3_C NonSolvent Resd 1  H   Uiso(max)/Uiso(min) Range        6.7 Ratio
906_ALERT_3_C Large K Value in the Analysis of Variance ......      3.123 Check

See above for a comment on disorder and ellipsoids


918_ALERT_3_C Reflection(s) with I(obs) much Smaller I(calc) .          1 Check
977_ALERT_2_C Check Negative Difference Density on H19C             -0.31 eA-3
#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C3, C4A}
3. Restrained distances
 Fe1-P1A \\sim Fe1-P1
 with sigma of 0.02
 P2A-C6A \\sim P2-C6
 with sigma of 0.02
 P3-C9A \\sim P3-C9
 with sigma of 0.02
 Fe1-P2A \\sim Fe1-P2
 with sigma of 0.02
 P3-C7A \\sim P3-C7
 with sigma of 0.02
 P1A-C1A \\sim P1-C1
 with sigma of 0.02
 P4A-C11A \\sim P4-C11
 with sigma of 0.02
 C2A-C1A \\sim C2-C1
 with sigma of 0.02
 P2A-C2A \\sim P2-C2
 with sigma of 0.02
 P4A-C8A \\sim P4-C8
 with sigma of 0.02
 P1A-C3A \\sim P1-C3
 with sigma of 0.02
 P3-C10A \\sim P3-C10
 with sigma of 0.02
 P1A-C4A \\sim P1-C4
 with sigma of 0.02
 C8A-C7A \\sim C8-C7
 with sigma of 0.02
 P2A-C5A \\sim P2-C5
 with sigma of 0.02
 P4A-C12A \\sim P4-C12
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(C4A)
5. Rigid body (RIGU) restrains
 Fe1, P1A, P2A, P3, P4A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A,
 C11A, C12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Fe1, P1, P2, P3, P4, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(P1A)=Sof(P2A)=Sof(P4A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=
 Sof(H4AC)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=
 Sof(H6AC)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=
 Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=1-FVAR(1)
 Sof(P1)=Sof(P2)=Sof(P4)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=
 Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=
 Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=
 Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1A(H1AA,H1AB), C2(H2A,H2B), C2A(H2AA,H2AB), C7(H7A,H7B),
 C7A(H7AA,H7AB), C8(H8A,H8B), C8A(H8AA,H8AB)
7.b Me refined with riding coordinates:
 C4A(H4AA,H4AB,H4AC)
7.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C),
 C5A(H5AA,H5AB,H5AC), C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC), C9(H9A,H9B,H9C),
 C9A(H9AA,H9AB,H9AC), C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F), C11(H11A,H11B,
 H11C), C11A(H11D,H11E,H11F), C12(H12A,H12B,H12C), C12A(H12D,H12E,H12F),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.27964(2) 0.37055(2) 0.21096(2) 0.01631(4) Uani 1 1 d D . . . .
H H 0.325(2) 0.2945(14) 0.2340(16) 0.042(6) Uiso 1 1 d . . . . .
P1 P 0.4623(2) 0.41572(18) 0.2557(2) 0.0218(3) Uani 0.6360(16) 1 d D . P A 1
P1A P 0.4809(4) 0.4063(3) 0.2449(4) 0.0207(5) Uani 0.3640(16) 1 d D . P A 2
P2 P 0.36740(9) 0.33532(5) 0.08845(6) 0.02168(15) Uani 0.6360(16) 1 d D . P A 1
P2A P 0.25256(11) 0.49194(6) 0.17457(8) 0.0220(3) Uani 0.3640(16) 1 d D . P A 2
P3 P 0.09376(3) 0.31866(2) 0.18089(2) 0.02007(7) Uani 1 1 d D . . . .
P4 P 0.17987(6) 0.47702(3) 0.16522(4) 0.01732(13) Uani 0.6360(16) 1 d D . P A 1
P4A P 0.33134(15) 0.31974(9) 0.07467(10) 0.0209(3) Uani 0.3640(16) 1 d D . P A
2
O1 O 0.15990(12) 0.51156(7) 0.69005(8) 0.0301(2) Uani 1 1 d . . . . .
O2 O 0.25339(11) 0.26577(6) 0.61065(7) 0.0256(2) Uani 1 1 d . . . . .
N1 N 0.21245(11) 0.44882(6) 0.38255(8) 0.01903(19) Uani 1 1 d . . . . .
N2 N 0.17820(12) 0.48673(7) 0.53859(8) 0.0213(2) Uani 1 1 d . . . . .
N3 N 0.20327(11) 0.38909(7) 0.64764(8) 0.0213(2) Uani 1 1 d . . . . .
N4 N 0.25237(12) 0.32583(6) 0.40869(8) 0.0199(2) Uani 1 1 d . . . . .
C1 C 0.5841(3) 0.3975(2) 0.1664(3) 0.0323(7) Uani 0.6360(16) 1 d D . P A 1
H1A H 0.645128 0.440517 0.164705 0.039 Uiso 0.6360(16) 1 calc R U P A 1
H1B H 0.632848 0.350590 0.181842 0.039 Uiso 0.6360(16) 1 calc R U P A 1
C1A C 0.4934(10) 0.5129(5) 0.2535(13) 0.119(6) Uani 0.3640(16) 1 d D . P A 2
H1AA H 0.504125 0.527382 0.318817 0.143 Uiso 0.3640(16) 1 calc R U P A 2
H1AB H 0.570490 0.529956 0.221738 0.143 Uiso 0.3640(16) 1 calc R U P A 2
C2 C 0.5178(3) 0.38867(16) 0.0754(2) 0.0333(5) Uani 0.6360(16) 1 d D . P A 1
H2A H 0.573710 0.360996 0.033269 0.040 Uiso 0.6360(16) 1 calc R U P A 1
H2B H 0.498914 0.439464 0.048800 0.040 Uiso 0.6360(16) 1 calc R U P A 1
C2A C 0.3884(7) 0.5494(3) 0.2163(8) 0.082(3) Uani 0.3640(16) 1 d D . P A 2
H2AA H 0.417260 0.580684 0.164521 0.098 Uiso 0.3640(16) 1 calc R U P A 2
H2AB H 0.356783 0.584954 0.263014 0.098 Uiso 0.3640(16) 1 calc R U P A 2
C3 C 0.5433(2) 0.3776(2) 0.3571(2) 0.0748(10) Uani 0.6360(16) 1 d D . P A 1
H3A H 0.634536 0.390238 0.355961 0.112 Uiso 0.6360(16) 1 calc R U P A 1
H3B H 0.532972 0.322158 0.358315 0.112 Uiso 0.6360(16) 1 calc R U P A 1
H3C H 0.506378 0.399832 0.411756 0.112 Uiso 0.6360(16) 1 calc R U P A 1
C3A C 0.6173(8) 0.3907(9) 0.1820(10) 0.119(6) Uani 0.3640(16) 1 d D . P A 2
H3AA H 0.685039 0.425781 0.202907 0.179 Uiso 0.3640(16) 1 calc R U P A 2
H3AB H 0.597193 0.399482 0.116918 0.179 Uiso 0.3640(16) 1 calc R U P A 2
H3AC H 0.646366 0.338073 0.190953 0.179 Uiso 0.3640(16) 1 calc R U P A 2
C4 C 0.4801(4) 0.5151(3) 0.2783(2) 0.0307(7) Uani 0.6360(16) 1 d D . P A 1
H4A H 0.454264 0.544151 0.223546 0.046 Uiso 0.6360(16) 1 calc R U P A 1
H4B H 0.569753 0.526184 0.294800 0.046 Uiso 0.6360(16) 1 calc R U P A 1
H4C H 0.426113 0.529490 0.329103 0.046 Uiso 0.6360(16) 1 calc R U P A 1
C4A C 0.5433(2) 0.3776(2) 0.3571(2) 0.0748(10) Uani 0.3640(16) 1 d D . P A 2
H4AA H 0.476390 0.383108 0.401980 0.112 Uiso 0.3640(16) 1 calc R U P A 2
H4AB H 0.570969 0.324333 0.354902 0.112 Uiso 0.3640(16) 1 calc R U P A 2
H4AC H 0.616367 0.409949 0.374835 0.112 Uiso 0.3640(16) 1 calc R U P A 2
C5 C 0.4285(13) 0.2387(6) 0.0898(10) 0.0296(18) Uani 0.6360(16) 1 d D . P A 1
H5A H 0.488651 0.232273 0.142026 0.044 Uiso 0.6360(16) 1 calc R U P A 1
H5B H 0.472524 0.228731 0.032813 0.044 Uiso 0.6360(16) 1 calc R U P A 1
H5C H 0.357315 0.202858 0.095205 0.044 Uiso 0.6360(16) 1 calc R U P A 1
C5A C 0.1211(8) 0.5489(5) 0.2140(6) 0.0386(17) Uani 0.3640(16) 1 d D . P A 2
H5AA H 0.102617 0.534680 0.277038 0.058 Uiso 0.3640(16) 1 calc R U P A 2
H5AB H 0.045193 0.540004 0.174372 0.058 Uiso 0.3640(16) 1 calc R U P A 2
H5AC H 0.144368 0.602952 0.211876 0.058 Uiso 0.3640(16) 1 calc R U P A 2
C6 C 0.3012(3) 0.3365(2) -0.03015(18) 0.0405(7) Uani 0.6360(16) 1 d D . P A 1
H6A H 0.230491 0.300013 -0.035962 0.061 Uiso 0.6360(16) 1 calc R U P A 1
H6B H 0.368223 0.322338 -0.072309 0.061 Uiso 0.6360(16) 1 calc R U P A 1
H6C H 0.269789 0.387701 -0.045167 0.061 Uiso 0.6360(16) 1 calc R U P A 1
C6A C 0.2455(16) 0.5226(8) 0.0561(9) 0.065(4) Uani 0.3640(16) 1 d D . P A 2
H6AA H 0.228166 0.577455 0.053288 0.097 Uiso 0.3640(16) 1 calc R U P A 2
H6AB H 0.177014 0.495078 0.022812 0.097 Uiso 0.3640(16) 1 calc R U P A 2
H6AC H 0.327414 0.511968 0.028023 0.097 Uiso 0.3640(16) 1 calc R U P A 2
C7 C 0.0000(2) 0.37264(14) 0.09647(17) 0.0220(4) Uani 0.6360(16) 1 d D . P A 1
H7A H 0.033602 0.365291 0.034524 0.026 Uiso 0.6360(16) 1 calc R U P A 1
H7B H -0.090677 0.356421 0.095784 0.026 Uiso 0.6360(16) 1 calc R U P A 1
C7A C 0.0992(4) 0.2495(3) 0.0956(3) 0.0275(8) Uani 0.3640(16) 1 d D . P A 2
H7AA H 0.133614 0.201328 0.121598 0.033 Uiso 0.3640(16) 1 calc R U P A 2
H7AB H 0.011972 0.239631 0.070006 0.033 Uiso 0.3640(16) 1 calc R U P A 2
C8 C 0.0128(2) 0.45597(13) 0.12609(16) 0.0224(4) Uani 0.6360(16) 1 d D . P A 1
H8A H -0.045912 0.466308 0.176429 0.027 Uiso 0.6360(16) 1 calc R U P A 1
H8B H -0.011671 0.489592 0.074014 0.027 Uiso 0.6360(16) 1 calc R U P A 1
C8A C 0.1852(4) 0.2781(3) 0.0203(3) 0.0303(9) Uani 0.3640(16) 1 d D . P A 2
H8AA H 0.139520 0.317120 -0.017233 0.036 Uiso 0.3640(16) 1 calc R U P A 2
H8AB H 0.208211 0.235428 -0.020218 0.036 Uiso 0.3640(16) 1 calc R U P A 2
C9 C -0.0213(3) 0.30594(19) 0.2711(3) 0.0242(6) Uani 0.6360(16) 1 d D . P A 1
H9A H -0.098716 0.281498 0.245498 0.036 Uiso 0.6360(16) 1 calc R U P A 1
H9B H -0.043374 0.355704 0.296552 0.036 Uiso 0.6360(16) 1 calc R U P A 1
H9C H 0.016487 0.273794 0.319702 0.036 Uiso 0.6360(16) 1 calc R U P A 1
C9A C -0.0345(4) 0.3846(3) 0.1334(4) 0.0289(9) Uani 0.3640(16) 1 d D . P A 2
H9AA H 0.000580 0.415994 0.084749 0.043 Uiso 0.3640(16) 1 calc R U P A 2
H9AB H -0.064275 0.417621 0.182436 0.043 Uiso 0.3640(16) 1 calc R U P A 2
H9AC H -0.106336 0.354499 0.108399 0.043 Uiso 0.3640(16) 1 calc R U P A 2
C10 C 0.0824(3) 0.22012(16) 0.1298(2) 0.0293(5) Uani 0.6360(16) 1 d D . P A 1
H10A H -0.007798 0.206082 0.120511 0.044 Uiso 0.6360(16) 1 calc R U P A 1
H10B H 0.124607 0.183561 0.171425 0.044 Uiso 0.6360(16) 1 calc R U P A 1
H10C H 0.124394 0.219539 0.070783 0.044 Uiso 0.6360(16) 1 calc R U P A 1
C10A C 0.0072(7) 0.2803(5) 0.2743(5) 0.0406(17) Uani 0.3640(16) 1 d D . P A 2
H10D H -0.079096 0.265883 0.252626 0.061 Uiso 0.3640(16) 1 calc R U P A 2
H10E H 0.001353 0.318831 0.322575 0.061 Uiso 0.3640(16) 1 calc R U P A 2
H10F H 0.051915 0.235340 0.298818 0.061 Uiso 0.3640(16) 1 calc R U P A 2
C11 C 0.1473(4) 0.5618(2) 0.2352(3) 0.0234(6) Uani 0.6360(16) 1 d D . P A 1
H11A H 0.228271 0.583120 0.259075 0.035 Uiso 0.6360(16) 1 calc R U P A 1
H11B H 0.094079 0.547290 0.286333 0.035 Uiso 0.6360(16) 1 calc R U P A 1
H11C H 0.102284 0.599954 0.197319 0.035 Uiso 0.6360(16) 1 calc R U P A 1
C11A C 0.3997(6) 0.3642(3) -0.0266(4) 0.0422(12) Uani 0.3640(16) 1 d D . P A 2
H11D H 0.409362 0.325744 -0.074440 0.063 Uiso 0.3640(16) 1 calc R U P A 2
H11E H 0.483613 0.385885 -0.009856 0.063 Uiso 0.3640(16) 1 calc R U P A 2
H11F H 0.342667 0.404734 -0.049358 0.063 Uiso 0.3640(16) 1 calc R U P A 2
C12 C 0.2423(4) 0.5279(4) 0.0654(4) 0.0279(9) Uani 0.6360(16) 1 d D . P A 1
H12A H 0.184682 0.570047 0.048601 0.042 Uiso 0.6360(16) 1 calc R U P A 1
H12B H 0.247649 0.492667 0.013731 0.042 Uiso 0.6360(16) 1 calc R U P A 1
H12C H 0.327554 0.548107 0.081082 0.042 Uiso 0.6360(16) 1 calc R U P A 1
C12A C 0.4323(18) 0.2339(9) 0.0813(16) 0.022(2) Uani 0.3640(16) 1 d D . P A 2
H12D H 0.391218 0.195374 0.118905 0.033 Uiso 0.3640(16) 1 calc R U P A 2
H12E H 0.516056 0.247032 0.109013 0.033 Uiso 0.3640(16) 1 calc R U P A 2
H12F H 0.443530 0.213716 0.019572 0.033 Uiso 0.3640(16) 1 calc R U P A 2
C13 C 0.24273(13) 0.38115(7) 0.34098(9) 0.0182(2) Uani 1 1 d . . . . .
C14 C 0.20572(12) 0.43418(7) 0.47218(9) 0.0185(2) Uani 1 1 d . . . . .
C15 C 0.17927(13) 0.46544(8) 0.62901(10) 0.0217(2) Uani 1 1 d . . . . .
C16 C 0.23125(12) 0.33106(8) 0.58337(9) 0.0198(2) Uani 1 1 d . . . . .
C17 C 0.22982(13) 0.35926(7) 0.49298(9) 0.0188(2) Uani 1 1 d . . . . .
C18 C 0.14754(16) 0.56485(8) 0.51281(11) 0.0274(3) Uani 1 1 d . . . . .
H18A H 0.226463 0.592230 0.499576 0.041 Uiso 1 1 calc R U . . .
H18B H 0.104922 0.590102 0.563284 0.041 Uiso 1 1 calc R U . . .
H18C H 0.090584 0.564834 0.458213 0.041 Uiso 1 1 calc R U . . .
C19 C 0.20381(16) 0.36644(10) 0.74390(10) 0.0287(3) Uani 1 1 d . . . . .
H19A H 0.149847 0.321291 0.750698 0.043 Uiso 1 1 calc R U . . .
H19B H 0.170446 0.408213 0.780658 0.043 Uiso 1 1 calc R U . . .
H19C H 0.291503 0.354614 0.764907 0.043 Uiso 1 1 calc R U . . .
C20 C 0.2825(2) 0.24548(8) 0.40005(11) 0.0314(3) Uani 1 1 d . . . . .
H20A H 0.375263 0.238332 0.406312 0.047 Uiso 1 1 calc R U . . .
H20B H 0.252041 0.227078 0.339887 0.047 Uiso 1 1 calc R U . . .
H20C H 0.240443 0.216806 0.448134 0.047 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 H 1.45(2) . ?
Fe1 P1 2.151(3) . ?
Fe1 P1A 2.237(5) . ?
Fe1 P2 2.1298(9) . ?
Fe1 P2A 2.2127(10) . ?
Fe1 P3 2.1791(4) . ?
Fe1 P4 2.2329(6) . ?
Fe1 P4A 2.2636(15) . ?
Fe1 C13 1.9595(13) . ?
P1 C1 1.881(4) . ?
P1 C3 1.811(4) . ?
P1 C4 1.784(5) . ?
P1A C1A 1.880(10) . ?
P1A C3A 1.743(9) . ?
P1A C4A 1.815(6) . ?
P2 C2 1.846(3) . ?
P2 C5 1.813(10) . ?
P2 C6 1.845(3) . ?
P2A C2A 1.831(6) . ?
P2A C5A 1.810(8) . ?
P2A C6A 1.813(12) . ?
P3 C7 1.817(2) . ?
P3 C7A 1.742(4) . ?
P3 C9 1.827(4) . ?
P3 C9A 1.887(4) . ?
P3 C10 1.887(2) . ?
P3 C10A 1.794(7) . ?
P4 C8 1.858(2) . ?
P4 C11 1.843(4) . ?
P4 C12 1.847(5) . ?
P4A C8A 1.850(4) . ?
P4A C11A 1.838(5) . ?
P4A C12A 1.841(14) . ?
O1 C15 1.2264(17) . ?
O2 C16 1.2332(17) . ?
N1 C13 1.3761(17) . ?
N1 C14 1.3387(17) . ?
N2 C14 1.3761(17) . ?
N2 C15 1.3726(19) . ?
N2 C18 1.4556(19) . ?
N3 C15 1.3892(19) . ?
N3 C16 1.4224(18) . ?
N3 C19 1.4615(19) . ?
N4 C13 1.3877(17) . ?
N4 C17 1.3913(17) . ?
N4 C20 1.4518(18) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.488(5) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1A C2A 1.369(11) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5A H5AA 0.9800 . ?
C5A H5AB 0.9800 . ?
C5A H5AC 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6A H6AA 0.9800 . ?
C6A H6AB 0.9800 . ?
C6A H6AC 0.9800 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.530(3) . ?
C7A H7AA 0.9900 . ?
C7A H7AB 0.9900 . ?
C7A C8A 1.529(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8A H8AA 0.9900 . ?
C8A H8AB 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10A H10D 0.9800 . ?
C10A H10E 0.9800 . ?
C10A H10F 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C14 C17 1.3716(18) . ?
C16 C17 1.4101(18) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 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
P1 Fe1 H 89.3(10) . . ?
P1 Fe1 P3 173.48(9) . . ?
P1 Fe1 P4 100.61(9) . . ?
P1A Fe1 H 84.7(10) . . ?
P1A Fe1 P4A 93.18(11) . . ?
P2 Fe1 H 77.3(9) . . ?
P2 Fe1 P1 87.69(7) . . ?
P2 Fe1 P3 96.61(3) . . ?
P2 Fe1 P4 101.63(3) . . ?
P2A Fe1 H 168.2(10) . . ?
P2A Fe1 P1A 84.00(15) . . ?
P2A Fe1 P4A 101.57(5) . . ?
P3 Fe1 H 86.9(10) . . ?
P3 Fe1 P1A 171.55(14) . . ?
P3 Fe1 P2A 104.35(3) . . ?
P3 Fe1 P4 83.36(2) . . ?
P3 Fe1 P4A 83.97(4) . . ?
P4 Fe1 H 170.1(10) . . ?
P4A Fe1 H 75.9(9) . . ?
C13 Fe1 H 86.3(9) . . ?
C13 Fe1 P1 82.61(8) . . ?
C13 Fe1 P1A 88.40(13) . . ?
C13 Fe1 P2 161.12(5) . . ?
C13 Fe1 P2A 96.53(5) . . ?
C13 Fe1 P3 91.87(4) . . ?
C13 Fe1 P4 96.07(4) . . ?
C13 Fe1 P4A 161.90(5) . . ?
C1 P1 Fe1 109.98(18) . . ?
C3 P1 Fe1 120.01(19) . . ?
C3 P1 C1 101.2(2) . . ?
C4 P1 Fe1 120.22(19) . . ?
C4 P1 C1 103.1(2) . . ?
C4 P1 C3 99.6(2) . . ?
C1A P1A Fe1 110.9(4) . . ?
C3A P1A Fe1 128.3(4) . . ?
C3A P1A C1A 97.8(7) . . ?
C3A P1A C4A 99.0(6) . . ?
C4A P1A Fe1 115.5(3) . . ?
C4A P1A C1A 101.1(6) . . ?
C2 P2 Fe1 109.37(10) . . ?
C5 P2 Fe1 115.1(5) . . ?
C5 P2 C2 100.1(5) . . ?
C5 P2 C6 98.2(5) . . ?
C6 P2 Fe1 128.85(11) . . ?
C6 P2 C2 101.08(16) . . ?
C2A P2A Fe1 111.0(2) . . ?
C5A P2A Fe1 123.3(3) . . ?
C5A P2A C2A 100.3(4) . . ?
C5A P2A C6A 97.6(6) . . ?
C6A P2A Fe1 121.1(5) . . ?
C6A P2A C2A 99.3(6) . . ?
C7 P3 Fe1 112.16(8) . . ?
C7 P3 C9 101.52(14) . . ?
C7 P3 C10 100.59(12) . . ?
C7A P3 Fe1 112.72(15) . . ?
C7A P3 C9A 101.8(2) . . ?
C7A P3 C10A 108.2(3) . . ?
C9 P3 Fe1 120.66(13) . . ?
C9 P3 C10 97.99(15) . . ?
C9A P3 Fe1 115.88(14) . . ?
C10 P3 Fe1 120.51(8) . . ?
C10A P3 Fe1 118.2(2) . . ?
C10A P3 C9A 98.0(3) . . ?
C8 P4 Fe1 110.57(7) . . ?
C11 P4 Fe1 127.07(14) . . ?
C11 P4 C8 98.18(14) . . ?
C11 P4 C12 97.1(3) . . ?
C12 P4 Fe1 117.9(2) . . ?
C12 P4 C8 101.91(16) . . ?
C8A P4A Fe1 108.39(15) . . ?
C11A P4A Fe1 130.6(2) . . ?
C11A P4A C8A 99.2(3) . . ?
C11A P4A C12A 98.8(8) . . ?
C12A P4A Fe1 115.4(7) . . ?
C12A P4A C8A 99.5(6) . . ?
C14 N1 C13 106.63(11) . . ?
C14 N2 C18 119.91(12) . . ?
C15 N2 C14 120.05(12) . . ?
C15 N2 C18 120.04(12) . . ?
C15 N3 C16 126.99(12) . . ?
C15 N3 C19 116.50(12) . . ?
C16 N3 C19 116.48(12) . . ?
C13 N4 C17 108.98(11) . . ?
C13 N4 C20 128.98(12) . . ?
C17 N4 C20 122.03(11) . . ?
P1 C1 H1A 109.8 . . ?
P1 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
C2 C1 P1 109.3(2) . . ?
C2 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 . . ?
P1A C1A H1AA 109.0 . . ?
P1A C1A H1AB 109.0 . . ?
H1AA C1A H1AB 107.8 . . ?
C2A C1A P1A 112.7(7) . . ?
C2A C1A H1AA 109.0 . . ?
C2A C1A H1AB 109.0 . . ?
P2 C2 H2A 109.8 . . ?
P2 C2 H2B 109.8 . . ?
C1 C2 P2 109.5(2) . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
P2A C2A H2AA 107.7 . . ?
P2A C2A H2AB 107.7 . . ?
C1A C2A P2A 118.6(5) . . ?
C1A C2A H2AA 107.7 . . ?
C1A C2A H2AB 107.7 . . ?
H2AA C2A H2AB 107.1 . . ?
P1 C3 H3A 109.5 . . ?
P1 C3 H3B 109.5 . . ?
P1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
P1A C3A H3AA 109.5 . . ?
P1A C3A H3AB 109.5 . . ?
P1A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
P1 C4 H4A 109.5 . . ?
P1 C4 H4B 109.5 . . ?
P1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
P1A C4A H4AA 109.5 . . ?
P1A C4A H4AB 109.5 . . ?
P1A C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
P2 C5 H5A 109.5 . . ?
P2 C5 H5B 109.5 . . ?
P2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
P2A C5A H5AA 109.5 . . ?
P2A C5A H5AB 109.5 . . ?
P2A C5A H5AC 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
P2 C6 H6A 109.5 . . ?
P2 C6 H6B 109.5 . . ?
P2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P2A C6A H6AA 109.5 . . ?
P2A C6A H6AB 109.5 . . ?
P2A C6A H6AC 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
P3 C7 H7A 110.7 . . ?
P3 C7 H7B 110.7 . . ?
H7A C7 H7B 108.8 . . ?
C8 C7 P3 105.45(15) . . ?
C8 C7 H7A 110.7 . . ?
C8 C7 H7B 110.7 . . ?
P3 C7A H7AA 110.0 . . ?
P3 C7A H7AB 110.0 . . ?
H7AA C7A H7AB 108.3 . . ?
C8A C7A P3 108.6(3) . . ?
C8A C7A H7AA 110.0 . . ?
C8A C7A H7AB 110.0 . . ?
P4 C8 H8A 109.6 . . ?
P4 C8 H8B 109.6 . . ?
C7 C8 P4 110.47(15) . . ?
C7 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
P4A C8A H8AA 110.0 . . ?
P4A C8A H8AB 110.0 . . ?
C7A C8A P4A 108.5(3) . . ?
C7A C8A H8AA 110.0 . . ?
C7A C8A H8AB 110.0 . . ?
H8AA C8A H8AB 108.4 . . ?
P3 C9 H9A 109.5 . . ?
P3 C9 H9B 109.5 . . ?
P3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P3 C9A H9AA 109.5 . . ?
P3 C9A H9AB 109.5 . . ?
P3 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
P3 C10 H10A 109.5 . . ?
P3 C10 H10B 109.5 . . ?
P3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P3 C10A H10D 109.5 . . ?
P3 C10A H10E 109.5 . . ?
P3 C10A H10F 109.5 . . ?
H10D C10A H10E 109.5 . . ?
H10D C10A H10F 109.5 . . ?
H10E C10A H10F 109.5 . . ?
P4 C11 H11A 109.5 . . ?
P4 C11 H11B 109.5 . . ?
P4 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P4A C11A H11D 109.5 . . ?
P4A C11A H11E 109.5 . . ?
P4A C11A H11F 109.5 . . ?
H11D C11A H11E 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
P4 C12 H12A 109.5 . . ?
P4 C12 H12B 109.5 . . ?
P4 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
P4A C12A H12D 109.5 . . ?
P4A C12A H12E 109.5 . . ?
P4A C12A H12F 109.5 . . ?
H12D C12A H12E 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
N1 C13 Fe1 124.42(9) . . ?
N1 C13 N4 107.59(11) . . ?
N4 C13 Fe1 127.78(9) . . ?
N1 C14 N2 125.45(12) . . ?
N1 C14 C17 112.69(12) . . ?
C17 C14 N2 121.86(12) . . ?
O1 C15 N2 121.58(14) . . ?
O1 C15 N3 121.86(14) . . ?
N2 C15 N3 116.56(12) . . ?
O2 C16 N3 119.53(12) . . ?
O2 C16 C17 128.71(13) . . ?
C17 C16 N3 111.76(12) . . ?
N4 C17 C16 133.15(12) . . ?
C14 C17 N4 104.11(11) . . ?
C14 C17 C16 122.72(12) . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N4 C20 H20A 109.5 . . ?
N4 C20 H20B 109.5 . . ?
N4 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 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
Fe1 P1 C1 C2 24.5(3) . . . . ?
Fe1 P1A C1A C2A -15.1(15) . . . . ?
Fe1 P2 C2 C1 39.0(2) . . . . ?
Fe1 P2A C2A C1A 7.4(13) . . . . ?
Fe1 P3 C7 C8 -45.43(19) . . . . ?
Fe1 P3 C7A C8A -41.2(4) . . . . ?
Fe1 P4 C8 C7 -23.71(18) . . . . ?
Fe1 P4A C8A C7A -31.5(4) . . . . ?
P1 C1 C2 P2 -38.6(3) . . . . ?
P1A C1A C2A P2A 4.9(17) . . . . ?
P3 C7 C8 P4 41.2(2) . . . . ?
P3 C7A C8A P4A 44.8(4) . . . . ?
O2 C16 C17 N4 -0.6(3) . . . . ?
O2 C16 C17 C14 -178.80(14) . . . . ?
N1 C14 C17 N4 -0.31(15) . . . . ?
N1 C14 C17 C16 178.33(12) . . . . ?
N2 C14 C17 N4 179.80(12) . . . . ?
N2 C14 C17 C16 -1.6(2) . . . . ?
N3 C16 C17 N4 179.02(14) . . . . ?
N3 C16 C17 C14 0.83(18) . . . . ?
C3 P1 C1 C2 152.5(2) . . . . ?
C3A P1A C1A C2A 121.1(13) . . . . ?
C4 P1 C1 C2 -104.8(3) . . . . ?
C4A P1A C1A C2A -138.2(12) . . . . ?
C5 P2 C2 C1 -82.3(5) . . . . ?
C5A P2A C2A C1A 139.3(13) . . . . ?
C6 P2 C2 C1 177.3(2) . . . . ?
C6A P2A C2A C1A -121.2(13) . . . . ?
C9 P3 C7 C8 84.7(2) . . . . ?
C9A P3 C7A C8A 83.6(3) . . . . ?
C10 P3 C7 C8 -174.76(18) . . . . ?
C10A P3 C7A C8A -173.8(4) . . . . ?
C11 P4 C8 C7 -158.5(2) . . . . ?
C11A P4A C8A C7A -170.0(3) . . . . ?
C12 P4 C8 C7 102.4(3) . . . . ?
C12A P4A C8A C7A 89.4(8) . . . . ?
C13 N1 C14 N2 179.69(13) . . . . ?
C13 N1 C14 C17 -0.19(16) . . . . ?
C13 N4 C17 C14 0.69(15) . . . . ?
C13 N4 C17 C16 -177.74(14) . . . . ?
C14 N1 C13 Fe1 -174.41(9) . . . . ?
C14 N1 C13 N4 0.62(15) . . . . ?
C14 N2 C15 O1 177.21(13) . . . . ?
C14 N2 C15 N3 -2.84(19) . . . . ?
C15 N2 C14 N1 -177.28(13) . . . . ?
C15 N2 C14 C17 2.6(2) . . . . ?
C15 N3 C16 O2 178.36(13) . . . . ?
C15 N3 C16 C17 -1.31(19) . . . . ?
C16 N3 C15 O1 -177.69(13) . . . . ?
C16 N3 C15 N2 2.4(2) . . . . ?
C17 N4 C13 Fe1 173.98(10) . . . . ?
C17 N4 C13 N1 -0.83(15) . . . . ?
C18 N2 C14 N1 2.9(2) . . . . ?
C18 N2 C14 C17 -177.20(13) . . . . ?
C18 N2 C15 O1 -3.0(2) . . . . ?
C18 N2 C15 N3 176.95(12) . . . . ?
C19 N3 C15 O1 0.2(2) . . . . ?
C19 N3 C15 N2 -179.74(12) . . . . ?
C19 N3 C16 O2 0.45(19) . . . . ?
C19 N3 C16 C17 -179.22(12) . . . . ?
C20 N4 C13 Fe1 -5.1(2) . . . . ?
C20 N4 C13 N1 -179.90(15) . . . . ?
C20 N4 C17 C14 179.83(14) . . . . ?
C20 N4 C17 C16 1.4(2) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 800'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil.'
_olex2_submission_original_sample_id JD12.021
_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_se20003
_database_code_depnum_ccdc_archive 'CCDC 2073340'
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2021-03-26 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
_audit_creation_date             2020-07-06
_audit_creation_method           
;
Olex2 1.3-beta
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H38 Fe O P4'
_chemical_formula_sum            'C17 H38 Fe O P4'
_chemical_formula_weight         438.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C34 H76 Fe2 O2 P8 '
_chemical_oxdiff_usercomment     '@ 120 K JD12.020'
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'
Fe Fe 0.3463 0.8444 '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                   8.9533(2)
_cell_length_b                   10.1488(3)
_cell_length_c                   13.3681(4)
_cell_angle_alpha                90.181(2)
_cell_angle_beta                 106.444(3)
_cell_angle_gamma                106.680(2)
_cell_volume                     1111.27(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11006
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      32.5210
_cell_measurement_theta_min      3.9410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.546
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             468
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
10 -9 -11 0.0361
-10 9 11 0.0361
-8 -4 -7 0.3076
-3 -8 16 0.0752
7 2 11 0.2670
3 8 -16 0.0978
-2 4 -17 0.1878

_exptl_crystal_recrystallization_method 
'The material was recrystallised from pentane by slow cooling'
_exptl_crystal_size_max          0.617
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.072
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
9.8948 -9.3361 -11.2111 -0.8772 -0.4770 -0.0545
-9.8948 9.3361 11.2111 0.8772 0.4770 0.0545
-7.8991 -4.2646 -6.6293 -0.1350 0.1556 0.9785
-2.7420 -7.6892 15.6782 0.6359 -0.7440 0.2050
6.7291 1.7927 10.9762 0.3174 -0.3691 -0.8735
2.9163 7.7711 -15.5388 -0.6334 0.7401 -0.2259
-2.0586 4.0913 -16.7251 -0.6044 0.7075 0.3662

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28848
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.850
_diffrn_reflns_theta_min         3.329
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -52.00   8.00   1.00   15.00    --  -17.52  88.00  27.00   60
  2  ω    -30.00  17.00   1.00   15.00    --  -17.52 -88.00 -89.00   47
  3  ω    -30.00  54.00   1.00   15.00    --   18.93 -88.00 -89.00   84
  4  ω    -49.00  21.00   1.00   15.00    --  -17.52  77.00 -90.00   70
  5  ω    -49.00  21.00   1.00   15.00    --  -17.52  77.00 -30.00   70
  6  ω    -42.00  14.00   1.00   15.00    --  -17.52 -77.00 150.00   56
  7  ω     -4.00  92.00   1.00   15.00    --   18.93  38.00 150.00   96
  8  ω     -4.00  92.00   1.00   15.00    --   18.93  38.00  60.00   96
  9  ω     39.00 106.00   1.00   15.00    --   18.93 178.00-120.00   67
 10  ω    -54.00  37.00   1.00   15.00    --   18.93 -38.00 -30.00   91
 11  ω     -4.00  92.00   1.00   15.00    --   18.93  38.00 -60.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0266015000
_diffrn_orient_matrix_UB_12      0.0142523000
_diffrn_orient_matrix_UB_13      0.0428989000
_diffrn_orient_matrix_UB_21      -0.0269329000
_diffrn_orient_matrix_UB_22      0.0536134000
_diffrn_orient_matrix_UB_23      -0.0258720000
_diffrn_orient_matrix_UB_31      -0.0778821000
_diffrn_orient_matrix_UB_32      -0.0478637000
_diffrn_orient_matrix_UB_33      -0.0240186000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6581
_reflns_number_total             7639
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3-beta (Bourhis et al., 2015)'
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7639
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0390
_refine_ls_restrained_S_all      1.094
_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)+(0.0236P)²+0.4413P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0743
_refine_special_details          
;
H atoms were identified from a difference Fourier map and freely refined.


#===============================================================================
#>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text

222_ALERT_3_C NonSolvent Resd 1  H   Uiso(max)/Uiso(min) Range        4.3 Ratio
906_ALERT_3_C Large K Value in the Analysis of Variance ......      5.000 Check
910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min).          9 Note

Noted, but no action taken

#===============================================================================
;
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_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 0.29223(2) 0.19214(2) 0.72422(2) 0.00930(5) Uani 1 1 d . . . . .
H H 0.120(3) 0.116(2) 0.6630(17) 0.041(6) Uiso 1 1 d . . . . .
P1 P 0.20976(5) 0.14948(4) 0.86253(3) 0.01719(9) Uani 1 1 d . . . . .
P2 P 0.33108(4) -0.00948(4) 0.73343(3) 0.01224(8) Uani 1 1 d . . . . .
P3 P 0.21885(5) 0.37951(4) 0.70268(3) 0.01356(8) Uani 1 1 d . . . . .
P4 P 0.34332(4) 0.21991(4) 0.57456(3) 0.01209(8) Uani 1 1 d . . . . .
O1 O 0.59254(12) 0.42944(10) 0.77586(8) 0.0166(2) Uani 1 1 d . . . . .
C1 C 0.52248(17) 0.29532(14) 0.80440(12) 0.0142(3) Uani 1 1 d . . . . .
C2 C 0.6459(2) 0.27311(17) 0.88329(14) 0.0222(3) Uani 1 1 d . . . . .
H2 H 0.641(2) 0.194(2) 0.9189(16) 0.030(5) Uiso 1 1 d . . . . .
C3 C 0.7898(2) 0.39024(17) 0.90366(15) 0.0246(4) Uani 1 1 d . . . . .
H3 H 0.889(3) 0.402(2) 0.9516(17) 0.037(6) Uiso 1 1 d . . . . .
C4 C 0.75231(18) 0.48155(16) 0.83701(13) 0.0187(3) Uani 1 1 d . . . . .
C5 C 0.8459(2) 0.61842(19) 0.81333(16) 0.0273(4) Uani 1 1 d . . . . .
H5A H 0.949(3) 0.649(2) 0.8631(18) 0.043(6) Uiso 1 1 d . . . . .
H5B H 0.863(3) 0.617(2) 0.7447(19) 0.043(6) Uiso 1 1 d . . . . .
H5C H 0.794(3) 0.689(2) 0.8143(18) 0.044(7) Uiso 1 1 d . . . . .
C6 C 0.2019(2) -0.02950(17) 0.89543(15) 0.0239(4) Uani 1 1 d . . . . .
H6A H 0.206(2) -0.036(2) 0.9650(17) 0.032(6) Uiso 1 1 d . . . . .
H6B H 0.093(3) -0.086(2) 0.8558(16) 0.029(5) Uiso 1 1 d . . . . .
C7 C 0.3331(2) -0.07020(16) 0.86361(12) 0.0180(3) Uani 1 1 d . . . . .
H7A H 0.320(2) -0.168(2) 0.8607(15) 0.028(5) Uiso 1 1 d . . . . .
H7B H 0.445(2) -0.0251(19) 0.9118(15) 0.021(5) Uiso 1 1 d . . . . .
C8 C 0.3281(3) 0.2477(2) 0.99008(15) 0.0326(4) Uani 1 1 d . . . . .
H8A H 0.441(3) 0.247(3) 1.007(2) 0.065(8) Uiso 1 1 d . . . . .
H8B H 0.319(3) 0.336(2) 0.9871(18) 0.045(7) Uiso 1 1 d . . . . .
H8C H 0.282(3) 0.204(2) 1.0429(18) 0.040(6) Uiso 1 1 d . . . . .
C9 C 0.0041(3) 0.1463(3) 0.8609(2) 0.0401(6) Uani 1 1 d . . . . .
H9A H -0.007(3) 0.236(3) 0.8633(19) 0.049(7) Uiso 1 1 d . . . . .
H9B H -0.019(3) 0.107(3) 0.919(2) 0.058(8) Uiso 1 1 d . . . . .
H9C H -0.074(3) 0.093(3) 0.798(2) 0.055(8) Uiso 1 1 d . . . . .
C10 C 0.5122(2) -0.04490(19) 0.71674(16) 0.0243(4) Uani 1 1 d . . . . .
H10A H 0.505(3) -0.047(2) 0.6421(18) 0.036(6) Uiso 1 1 d . . . . .
H10B H 0.519(3) -0.135(2) 0.7389(17) 0.038(6) Uiso 1 1 d . . . . .
H10C H 0.605(3) 0.024(2) 0.7559(17) 0.034(6) Uiso 1 1 d . . . . .
C11 C 0.1703(2) -0.15567(16) 0.65017(15) 0.0232(4) Uani 1 1 d . . . . .
H11A H 0.147(2) -0.136(2) 0.5788(17) 0.030(5) Uiso 1 1 d . . . . .
H11B H 0.203(3) -0.237(2) 0.6581(18) 0.046(7) Uiso 1 1 d . . . . .
H11C H 0.073(3) -0.170(2) 0.6696(18) 0.044(7) Uiso 1 1 d . . . . .
C12 C 0.2970(2) 0.47375(15) 0.60079(13) 0.0181(3) Uani 1 1 d . . . . .
H12A H 0.237(2) 0.544(2) 0.5753(15) 0.026(5) Uiso 1 1 d . . . . .
H12B H 0.409(2) 0.5227(19) 0.6331(15) 0.022(5) Uiso 1 1 d . . . . .
C13 C 0.2787(2) 0.36676(16) 0.51429(13) 0.0180(3) Uani 1 1 d . . . . .
H13A H 0.341(2) 0.4038(19) 0.4670(15) 0.023(5) Uiso 1 1 d . . . . .
H13B H 0.165(2) 0.3282(17) 0.4721(14) 0.015(4) Uiso 1 1 d . . . . .
C14 C 0.2825(3) 0.51689(17) 0.80842(14) 0.0244(4) Uani 1 1 d . . . . .
H14A H 0.225(3) 0.490(2) 0.8568(17) 0.031(6) Uiso 1 1 d . . . . .
H14B H 0.394(3) 0.536(2) 0.8431(16) 0.032(6) Uiso 1 1 d . . . . .
H14C H 0.262(3) 0.599(2) 0.7819(18) 0.042(6) Uiso 1 1 d . . . . .
C15 C 0.0019(2) 0.3651(2) 0.65034(16) 0.0245(4) Uani 1 1 d . . . . .
H15A H -0.047(3) 0.306(2) 0.5884(18) 0.040(6) Uiso 1 1 d . . . . .
H15B H -0.010(3) 0.454(2) 0.6346(17) 0.035(6) Uiso 1 1 d . . . . .
H15C H -0.055(3) 0.328(2) 0.6967(18) 0.038(6) Uiso 1 1 d . . . . .
C16 C 0.55435(19) 0.26326(18) 0.56892(14) 0.0195(3) Uani 1 1 d . . . . .
H16A H 0.613(2) 0.346(2) 0.6060(15) 0.024(5) Uiso 1 1 d . . . . .
H16B H 0.604(3) 0.196(2) 0.5982(17) 0.036(6) Uiso 1 1 d . . . . .
H16C H 0.553(2) 0.268(2) 0.4970(17) 0.028(5) Uiso 1 1 d . . . . .
C17 C 0.2450(2) 0.08685(17) 0.46371(13) 0.0187(3) Uani 1 1 d . . . . .
H17A H 0.263(2) 0.127(2) 0.3991(16) 0.027(5) Uiso 1 1 d . . . . .
H17B H 0.294(2) 0.015(2) 0.4748(15) 0.024(5) Uiso 1 1 d . . . . .
H17C H 0.131(2) 0.0495(19) 0.4557(15) 0.022(5) Uiso 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 H 1.50(2) . ?
Fe1 P1 2.1785(4) . ?
Fe1 P2 2.1700(4) . ?
Fe1 P3 2.1781(4) . ?
Fe1 P4 2.1768(4) . ?
Fe1 C1 1.9995(14) . ?
P1 C6 1.8566(17) . ?
P1 C8 1.839(2) . ?
P1 C9 1.826(2) . ?
P2 C7 1.8450(16) . ?
P2 C10 1.8300(17) . ?
P2 C11 1.8353(16) . ?
P3 C12 1.8501(16) . ?
P3 C14 1.8283(17) . ?
P3 C15 1.8301(18) . ?
P4 C13 1.8558(16) . ?
P4 C16 1.8365(16) . ?
P4 C17 1.8333(16) . ?
O1 C1 1.4285(17) . ?
O1 C4 1.3766(17) . ?
C1 C2 1.367(2) . ?
C2 H2 0.93(2) . ?
C2 C3 1.438(2) . ?
C3 H3 0.91(2) . ?
C3 C4 1.334(2) . ?
C4 C5 1.489(2) . ?
C5 H5A 0.93(2) . ?
C5 H5B 0.97(2) . ?
C5 H5C 0.96(2) . ?
C6 H6A 0.92(2) . ?
C6 H6B 0.97(2) . ?
C6 C7 1.514(2) . ?
C7 H7A 0.96(2) . ?
C7 H7B 0.997(18) . ?
C8 H8A 0.97(3) . ?
C8 H8B 0.92(2) . ?
C8 H8C 0.96(2) . ?
C9 H9A 0.94(3) . ?
C9 H9B 0.92(3) . ?
C9 H9C 0.97(3) . ?
C10 H10A 0.98(2) . ?
C10 H10B 0.97(2) . ?
C10 H10C 0.93(2) . ?
C11 H11A 0.95(2) . ?
C11 H11B 0.94(2) . ?
C11 H11C 0.95(2) . ?
C12 H12A 1.01(2) . ?
C12 H12B 0.953(19) . ?
C12 C13 1.525(2) . ?
C13 H13A 0.968(19) . ?
C13 H13B 0.973(17) . ?
C14 H14A 0.93(2) . ?
C14 H14B 0.94(2) . ?
C14 H14C 0.95(2) . ?
C15 H15A 0.94(2) . ?
C15 H15B 0.96(2) . ?
C15 H15C 0.93(2) . ?
C16 H16A 0.91(2) . ?
C16 H16B 0.95(2) . ?
C16 H16C 0.96(2) . ?
C17 H17A 0.99(2) . ?
C17 H17B 0.94(2) . ?
C17 H17C 0.958(19) . ?

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
P1 Fe1 H 85.7(9) . . ?
P2 Fe1 H 85.8(8) . . ?
P2 Fe1 P1 86.092(16) . . ?
P2 Fe1 P3 172.135(17) . . ?
P2 Fe1 P4 93.099(16) . . ?
P3 Fe1 H 86.3(8) . . ?
P3 Fe1 P1 93.345(17) . . ?
P4 Fe1 H 87.0(9) . . ?
P4 Fe1 P1 172.738(18) . . ?
P4 Fe1 P3 86.467(16) . . ?
C1 Fe1 H 179.2(9) . . ?
C1 Fe1 P1 94.94(4) . . ?
C1 Fe1 P2 94.74(4) . . ?
C1 Fe1 P3 93.13(4) . . ?
C1 Fe1 P4 92.32(4) . . ?
C6 P1 Fe1 110.23(6) . . ?
C8 P1 Fe1 121.28(8) . . ?
C8 P1 C6 101.01(9) . . ?
C9 P1 Fe1 121.14(8) . . ?
C9 P1 C6 99.39(10) . . ?
C9 P1 C8 100.06(12) . . ?
C7 P2 Fe1 110.37(5) . . ?
C10 P2 Fe1 124.07(6) . . ?
C10 P2 C7 101.01(8) . . ?
C10 P2 C11 100.16(9) . . ?
C11 P2 Fe1 117.75(6) . . ?
C11 P2 C7 99.78(8) . . ?
C12 P3 Fe1 109.77(5) . . ?
C14 P3 Fe1 122.24(6) . . ?
C14 P3 C12 101.74(8) . . ?
C14 P3 C15 100.41(9) . . ?
C15 P3 Fe1 119.23(6) . . ?
C15 P3 C12 100.07(8) . . ?
C13 P4 Fe1 110.36(6) . . ?
C16 P4 Fe1 120.20(6) . . ?
C16 P4 C13 101.71(8) . . ?
C17 P4 Fe1 122.02(6) . . ?
C17 P4 C13 100.10(8) . . ?
C17 P4 C16 99.01(8) . . ?
C4 O1 C1 109.54(12) . . ?
O1 C1 Fe1 118.08(10) . . ?
C2 C1 Fe1 137.66(11) . . ?
C2 C1 O1 104.22(12) . . ?
C1 C2 H2 126.2(13) . . ?
C1 C2 C3 110.11(15) . . ?
C3 C2 H2 123.6(13) . . ?
C2 C3 H3 128.2(14) . . ?
C4 C3 C2 106.71(14) . . ?
C4 C3 H3 125.1(14) . . ?
O1 C4 C5 116.30(15) . . ?
C3 C4 O1 109.42(13) . . ?
C3 C4 C5 134.21(15) . . ?
C4 C5 H5A 109.6(14) . . ?
C4 C5 H5B 113.6(13) . . ?
C4 C5 H5C 113.5(14) . . ?
H5A C5 H5B 107.6(19) . . ?
H5A C5 H5C 107.1(19) . . ?
H5B C5 H5C 105.0(19) . . ?
P1 C6 H6A 109.0(13) . . ?
P1 C6 H6B 105.0(12) . . ?
H6A C6 H6B 105.7(17) . . ?
C7 C6 P1 109.26(11) . . ?
C7 C6 H6A 115.5(13) . . ?
C7 C6 H6B 111.9(12) . . ?
P2 C7 H7A 109.4(12) . . ?
P2 C7 H7B 106.9(11) . . ?
C6 C7 P2 107.27(11) . . ?
C6 C7 H7A 114.3(12) . . ?
C6 C7 H7B 112.8(11) . . ?
H7A C7 H7B 106.0(15) . . ?
P1 C8 H8A 109.9(16) . . ?
P1 C8 H8B 108.3(14) . . ?
P1 C8 H8C 108.7(13) . . ?
H8A C8 H8B 113(2) . . ?
H8A C8 H8C 108(2) . . ?
H8B C8 H8C 108.7(19) . . ?
P1 C9 H9A 112.0(15) . . ?
P1 C9 H9B 109.5(16) . . ?
P1 C9 H9C 109.5(15) . . ?
H9A C9 H9B 107(2) . . ?
H9A C9 H9C 109(2) . . ?
H9B C9 H9C 110(2) . . ?
P2 C10 H10A 108.8(13) . . ?
P2 C10 H10B 111.9(13) . . ?
P2 C10 H10C 108.7(13) . . ?
H10A C10 H10B 106.8(17) . . ?
H10A C10 H10C 111.1(18) . . ?
H10B C10 H10C 109.6(18) . . ?
P2 C11 H11A 110.1(12) . . ?
P2 C11 H11B 110.2(14) . . ?
P2 C11 H11C 109.6(14) . . ?
H11A C11 H11B 110.4(18) . . ?
H11A C11 H11C 107.6(18) . . ?
H11B C11 H11C 108.8(19) . . ?
P3 C12 H12A 110.1(11) . . ?
P3 C12 H12B 107.0(12) . . ?
H12A C12 H12B 108.0(15) . . ?
C13 C12 P3 107.53(10) . . ?
C13 C12 H12A 113.4(11) . . ?
C13 C12 H12B 110.7(12) . . ?
P4 C13 H13A 109.4(11) . . ?
P4 C13 H13B 106.2(10) . . ?
C12 C13 P4 109.10(11) . . ?
C12 C13 H13A 113.0(11) . . ?
C12 C13 H13B 111.7(11) . . ?
H13A C13 H13B 107.2(15) . . ?
P3 C14 H14A 110.1(13) . . ?
P3 C14 H14B 110.2(13) . . ?
P3 C14 H14C 110.9(14) . . ?
H14A C14 H14B 108.4(18) . . ?
H14A C14 H14C 108.4(18) . . ?
H14B C14 H14C 108.8(18) . . ?
P3 C15 H15A 111.5(14) . . ?
P3 C15 H15B 109.8(13) . . ?
P3 C15 H15C 111.6(14) . . ?
H15A C15 H15B 107.5(18) . . ?
H15A C15 H15C 106.0(19) . . ?
H15B C15 H15C 110.3(19) . . ?
P4 C16 H16A 109.4(12) . . ?
P4 C16 H16B 110.9(13) . . ?
P4 C16 H16C 108.5(12) . . ?
H16A C16 H16B 108.5(17) . . ?
H16A C16 H16C 110.0(16) . . ?
H16B C16 H16C 109.6(18) . . ?
P4 C17 H17A 109.6(11) . . ?
P4 C17 H17B 109.5(11) . . ?
P4 C17 H17C 110.8(11) . . ?
H17A C17 H17B 106.7(16) . . ?
H17A C17 H17C 110.7(15) . . ?
H17B C17 H17C 109.5(16) . . ?

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
Fe1 P1 C6 C7 31.36(14) . . . . ?
Fe1 P2 C7 C6 39.47(12) . . . . ?
Fe1 P3 C12 C13 39.49(12) . . . . ?
Fe1 P4 C13 C12 31.13(12) . . . . ?
Fe1 C1 C2 C3 177.55(14) . . . . ?
P1 C6 C7 P2 -42.96(14) . . . . ?
P3 C12 C13 P4 -43.03(13) . . . . ?
O1 C1 C2 C3 -0.06(19) . . . . ?
C1 O1 C4 C3 -0.38(18) . . . . ?
C1 O1 C4 C5 176.99(14) . . . . ?
C1 C2 C3 C4 -0.2(2) . . . . ?
C2 C3 C4 O1 0.3(2) . . . . ?
C2 C3 C4 C5 -176.38(19) . . . . ?
C4 O1 C1 Fe1 -177.91(10) . . . . ?
C4 O1 C1 C2 0.26(17) . . . . ?
C8 P1 C6 C7 -98.09(14) . . . . ?
C9 P1 C6 C7 159.64(14) . . . . ?
C10 P2 C7 C6 172.40(12) . . . . ?
C11 P2 C7 C6 -85.14(13) . . . . ?
C14 P3 C12 C13 170.31(12) . . . . ?
C15 P3 C12 C13 -86.72(12) . . . . ?
C16 P4 C13 C12 -97.54(12) . . . . ?
C17 P4 C13 C12 160.96(11) . . . . ?

_olex2_date_sample_data_collection 2020-07-01
_olex2_date_sample_submission    2020-07-01
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil.'
_olex2_submission_original_sample_id JD12.020
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.324
_oxdiff_exptl_absorpt_empirical_full_min 0.815
####################################################################### 
# 
# 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_se22002
_database_code_depnum_ccdc_archive 'CCDC 2159501'
loop_
_audit_author_name
_audit_author_address
'Gary Stephen Nichol'
;The University of Edinburgh
United Kingdom
;
_audit_update_record             
;
2022-03-16 deposited with the CCDC.	2022-08-09 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_se22002             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note
RESPONSE: Not significant.
;
# Added during the CSD deposition process: Wednesday 16 March 2022 06:54 PM
# end Validation Reply Form

_audit_creation_date             2022-01-20
_audit_creation_method           
;
Olex2 1.5-beta
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
g.s.nichol@ed.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H38 Fe O P4'
_chemical_formula_sum            'C16 H38 Fe O P4'
_chemical_formula_weight         426.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C14 H37 B1 Fe1 O2 P4'
_chemical_oxdiff_usercomment     '@ 120 K LAB302'
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'
Fe Fe 0.3463 0.8444 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   14.6983(3)
_cell_length_b                   17.3967(3)
_cell_length_c                   17.9529(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.957(2)
_cell_angle_gamma                90
_cell_volume                     4341.61(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    34876
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      31.1810
_cell_measurement_theta_min      3.6860
_shelx_estimated_absorpt_T_max   0.834
_shelx_estimated_absorpt_T_min   0.736
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'translucent dark yellow'
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-20 2 1 0.0653
14 18 -3 0.0982
17 -11 1 0.1086
2 -24 3 0.0954
-2 -24 -5 0.0954
0 23 8 0.0814
10 -9 -23 0.1099
-12 -13 19 0.1182
-11 8 23 0.0891
8 22 -7 0.1164
11 -6 15 0.1187
-8 -6 -18 0.1198

_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of pentane and THF  by slow cooling'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-19.7337 1.6482 0.7072 0.9611 0.1788 -0.2106
14.2209 17.6703 -3.2056 -0.4509 -0.0826 0.8888
17.3292 -10.9499 0.7374 -0.9658 -0.1803 -0.1864
2.2345 -24.0008 3.3244 -0.4141 -0.0786 -0.9068
-2.1068 -23.7753 -4.5225 -0.0424 -0.3326 -0.9421
0.1658 23.0975 7.9841 0.0602 0.4676 0.8819
10.2218 -9.2267 -22.8286 -0.1275 -0.9772 -0.1697
-12.4581 -13.3021 19.0014 0.0897 0.6805 -0.7273
-10.7621 7.6773 23.3032 0.1288 0.9865 0.1012
8.0648 22.1807 -7.4240 -0.0217 -0.1583 0.9872
11.0587 -5.7461 15.0585 -0.8985 0.4273 -0.1007
-7.8450 -5.8141 -18.2988 0.6929 -0.6572 -0.2966

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            114056
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.324
_diffrn_reflns_theta_min         3.156
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -62.00  46.00   1.00    7.50    --   14.65 -23.00 135.00  108
  2  ω    -17.00  92.00   1.00    7.50    --   14.65  23.00 -59.00  109
  3  ω    -44.00  21.00   1.00    7.50    --  -12.93  77.00  30.00   65
  4  ω    -42.00  18.00   1.00    7.50    --  -12.93 -77.00  90.00   60
  5  ω    -42.00  18.00   1.00    7.50    --  -12.93 -77.00 -30.00   60
  6  ω    -42.00  46.00   1.00    7.50    --   14.65 -77.00  90.00   88
  7  ω    -56.00  41.00   1.00    7.50    --   14.65 -57.00-150.00   97
  8  ω    -12.00  85.00   1.00    7.50    --   14.65  57.00-150.00   97
  9  ω    -15.00  55.00   1.00    7.50    --   14.65 -99.00 -60.00   70
 10  ω    -44.00  13.00   1.00    7.50    --  -12.93  77.00 -30.00   57
 11  ω    -42.00  18.00   1.00    7.50    --  -12.93 -77.00  30.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0485970000
_diffrn_orient_matrix_UB_12      0.0099319000
_diffrn_orient_matrix_UB_13      -0.0201886000
_diffrn_orient_matrix_UB_21      -0.0071084000
_diffrn_orient_matrix_UB_22      0.0076727000
_diffrn_orient_matrix_UB_23      0.0365225000
_diffrn_orient_matrix_UB_31      0.0138382000
_diffrn_orient_matrix_UB_32      0.0387885000
_diffrn_orient_matrix_UB_33      -0.0020470000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10498
_reflns_number_total             13141
_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       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         13141
_refine_ls_number_restraints     153
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0336
_refine_ls_restrained_S_all      1.037
_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)+(0.0289P)²+1.7633P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0754
_refine_special_details          
;
Atoms O51 to C54 were modelled as disordered, corresponding with a 180 degree rotation about the Fe51-C51 bond.  Displacement ellipsoid and geometric restraints were used on the disorder components (roughly 2:1 disorder ratio).  Disordered H atoms were placed using HADD in Olex2.  All other H atoms were identified from a difference map and freely refined.

#===============================================================================
#>>> The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text

910_ALERT_3_B Missing # of FCF Reflection(s) Below Theta(Min).         16 Note

Not significant

#===============================================================================
213_ALERT_2_C Atom C53A            has ADP max/min Ratio .....        3.2 prolat

Disordered, as discussed above.

906_ALERT_3_C Large K Value in the Analysis of Variance ......      2.590 Check
911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Fe51-C51 \\sim Fe51-C51A
 with sigma of 0.02
 O51-C51 \\sim O51A-C51A
 with sigma of 0.02
 O51-C54 \\sim O51A-C54A
 with sigma of 0.02
 C51-C52 \\sim C51A-C52A
 with sigma of 0.02
 C51-C54 \\sim C51A-C54A
 with sigma of 0.04
 C52-C53 \\sim C52A-C53A
 with sigma of 0.02
 C51-C53 \\sim C51A-C53A
 with sigma of 0.04
 C53-C54 \\sim C53A-C54A
 with sigma of 0.02
 C52-C54 \\sim C52A-C54A
 with sigma of 0.04
 Fe51-O51 \\sim Fe51-O51A
 with sigma of 0.04
 Fe51-C52 \\sim Fe51-C52A
 with sigma of 0.04
 O51-C52 \\sim O51A-C52A
 with sigma of 0.04
 O51-C53 \\sim O51A-C53A
 with sigma of 0.04
3. Rigid bond restraints
 O51, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O51A, C51A, C52A, C53A, C54A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O51A \\sim C51A \\sim C52A \\sim C53A \\sim C54A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
O51 \\sim C51 \\sim C52 \\sim C53 \\sim C54: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 O51A, C51A, C52A, C53A, C54A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O51, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O51A)=Sof(C51A)=Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(H53C)=Sof(H53D)=
 Sof(C54A)=Sof(H54C)=Sof(H54D)=1-FVAR(1)
 Sof(O51)=Sof(C51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C54)=
 Sof(H54A)=Sof(H54B)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C53A(H53C,H53D), C54(H54A,H54B), C54A(H54C,H54D)
7.b Aromatic/amide H refined with riding coordinates:
 C52(H52), C52A(H52A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.79050(2) 0.58968(2) 0.38271(2) 0.01450(5) Uani 1 1 d . . . . .
H H 0.8696(15) 0.5659(12) 0.4546(12) 0.044(6) Uiso 1 1 d . . . . .
P1 P 0.68983(3) 0.53778(2) 0.43422(2) 0.01894(8) Uani 1 1 d . . . . .
P2 P 0.80765(3) 0.47459(2) 0.34181(2) 0.02061(8) Uani 1 1 d . . . . .
P3 P 0.79740(3) 0.69825(2) 0.44442(3) 0.02289(9) Uani 1 1 d . . . . .
P4 P 0.89974(3) 0.63922(2) 0.33923(2) 0.02083(8) Uani 1 1 d . . . . .
O1 O 0.69809(9) 0.69521(6) 0.25265(8) 0.0348(3) Uani 1 1 d . . . . .
C1 C 0.68582(10) 0.62290(8) 0.28589(9) 0.0187(3) Uani 1 1 d . . . . .
C2 C 0.60270(12) 0.59323(10) 0.23954(11) 0.0317(4) Uani 1 1 d . . . . .
H2 H 0.5788(15) 0.5472(13) 0.2474(12) 0.044(6) Uiso 1 1 d . . . . .
C3 C 0.55167(13) 0.64242(11) 0.16993(12) 0.0345(4) Uani 1 1 d . . . . .
H3A H 0.5508(16) 0.6221(13) 0.1180(14) 0.049(6) Uiso 1 1 d . . . . .
H3B H 0.4878(19) 0.6543(14) 0.1679(14) 0.064(8) Uiso 1 1 d . . . . .
C4 C 0.61304(13) 0.71401(10) 0.18909(11) 0.0290(4) Uani 1 1 d . . . . .
H4A H 0.6319(14) 0.7341(11) 0.1469(11) 0.031(5) Uiso 1 1 d . . . . .
H4B H 0.5811(16) 0.7551(13) 0.2049(13) 0.049(6) Uiso 1 1 d . . . . .
C5 C 0.65428(12) 0.44124(9) 0.39150(10) 0.0263(3) Uani 1 1 d . . . . .
H5A H 0.6062(14) 0.4481(10) 0.3417(11) 0.028(5) Uiso 1 1 d . . . . .
H5B H 0.6254(15) 0.4133(11) 0.4238(12) 0.039(6) Uiso 1 1 d . . . . .
C6 C 0.74459(14) 0.40349(9) 0.38446(11) 0.0276(4) Uani 1 1 d . . . . .
H6A H 0.7894(13) 0.3885(10) 0.4390(11) 0.027(5) Uiso 1 1 d . . . . .
H6B H 0.7313(14) 0.3590(12) 0.3539(12) 0.038(5) Uiso 1 1 d . . . . .
C7 C 0.57358(13) 0.58062(12) 0.42757(12) 0.0324(4) Uani 1 1 d . . . . .
H7A H 0.5343(16) 0.5447(12) 0.4415(13) 0.045(6) Uiso 1 1 d . . . . .
H7B H 0.5437(15) 0.6004(11) 0.3756(13) 0.037(6) Uiso 1 1 d . . . . .
H7C H 0.5817(15) 0.6229(12) 0.4636(12) 0.040(6) Uiso 1 1 d . . . . .
C8 C 0.73158(15) 0.51172(12) 0.53884(10) 0.0312(4) Uani 1 1 d . . . . .
H8A H 0.6856(18) 0.4876(13) 0.5539(14) 0.052(7) Uiso 1 1 d . . . . .
H8B H 0.7877(17) 0.4800(13) 0.5487(13) 0.049(6) Uiso 1 1 d . . . . .
H8C H 0.7505(16) 0.5571(14) 0.5673(14) 0.050(6) Uiso 1 1 d . . . . .
C9 C 0.92731(14) 0.43033(10) 0.36924(14) 0.0337(4) Uani 1 1 d . . . . .
H9A H 0.9607(15) 0.4524(12) 0.3356(13) 0.042(6) Uiso 1 1 d . . . . .
H9B H 0.9180(16) 0.3783(14) 0.3595(13) 0.051(6) Uiso 1 1 d . . . . .
H9C H 0.9614(16) 0.4403(12) 0.4253(14) 0.044(6) Uiso 1 1 d . . . . .
C10 C 0.76185(19) 0.44656(12) 0.23780(11) 0.0385(5) Uani 1 1 d . . . . .
H10A H 0.6972(17) 0.4576(12) 0.2175(13) 0.041(6) Uiso 1 1 d . . . . .
H10B H 0.7890(16) 0.4771(13) 0.2062(13) 0.047(6) Uiso 1 1 d . . . . .
H10C H 0.7745(16) 0.3930(13) 0.2320(13) 0.047(6) Uiso 1 1 d . . . . .
C11 C 0.89372(14) 0.76045(10) 0.43202(13) 0.0355(4) Uani 1 1 d . . . . .
H11A H 0.8790(16) 0.8112(13) 0.4374(13) 0.048(6) Uiso 1 1 d . . . . .
H11B H 0.9501(15) 0.7472(11) 0.4731(12) 0.034(5) Uiso 1 1 d . . . . .
C12 C 0.90332(14) 0.74459(10) 0.35184(13) 0.0329(4) Uani 1 1 d . . . . .
H12A H 0.8518(15) 0.7638(12) 0.3123(12) 0.038(6) Uiso 1 1 d . . . . .
H12B H 0.9604(16) 0.7650(12) 0.3469(12) 0.042(6) Uiso 1 1 d . . . . .
C13 C 0.82919(16) 0.70130(13) 0.55181(12) 0.0376(4) Uani 1 1 d . . . . .
H13A H 0.8780(15) 0.6663(12) 0.5740(12) 0.037(6) Uiso 1 1 d . . . . .
H13B H 0.7770(17) 0.6862(12) 0.5680(13) 0.045(6) Uiso 1 1 d . . . . .
H13C H 0.8464(16) 0.7518(14) 0.5668(13) 0.051(6) Uiso 1 1 d . . . . .
C14 C 0.69515(15) 0.76467(11) 0.41609(15) 0.0376(5) Uani 1 1 d . . . . .
H14A H 0.7073(16) 0.8068(14) 0.4475(14) 0.052(7) Uiso 1 1 d . . . . .
H14B H 0.6818(17) 0.7769(13) 0.3637(15) 0.053(7) Uiso 1 1 d . . . . .
H14C H 0.6430(19) 0.7411(14) 0.4252(15) 0.065(8) Uiso 1 1 d . . . . .
C15 C 1.02676(12) 0.61740(12) 0.39017(13) 0.0344(4) Uani 1 1 d . . . . .
H15A H 1.0373(15) 0.5628(13) 0.3899(13) 0.046(6) Uiso 1 1 d . . . . .
H15B H 1.0425(15) 0.6338(11) 0.4426(13) 0.037(6) Uiso 1 1 d . . . . .
H15C H 1.0674(15) 0.6414(12) 0.3653(12) 0.040(6) Uiso 1 1 d . . . . .
C16 C 0.89447(15) 0.62904(13) 0.23652(12) 0.0353(4) Uani 1 1 d . . . . .
H16A H 0.9394(17) 0.6610(13) 0.2255(13) 0.049(6) Uiso 1 1 d . . . . .
H16B H 0.8345(17) 0.6443(12) 0.2057(13) 0.046(6) Uiso 1 1 d . . . . .
H16C H 0.9076(15) 0.5765(13) 0.2254(13) 0.046(6) Uiso 1 1 d . . . . .
Fe51 Fe 0.21391(2) 0.40984(2) 0.12128(2) 0.01373(5) Uani 1 1 d D . . . .
HA H 0.1448(15) 0.4447(12) 0.0515(12) 0.044(6) Uiso 1 1 d . . . . .
P51 P 0.17244(3) 0.30084(2) 0.06161(2) 0.02481(9) Uani 1 1 d . . . . .
P52 P 0.31573(3) 0.41915(2) 0.05683(2) 0.02273(9) Uani 1 1 d . . . . .
P53 P 0.09513(3) 0.40848(2) 0.16829(3) 0.02167(9) Uani 1 1 d . . . . .
P54 P 0.24449(3) 0.52403(2) 0.17245(2) 0.01977(8) Uani 1 1 d . . . . .
O51 O 0.2966(5) 0.3686(6) 0.2890(4) 0.0246(15) Uani 0.628(8) 1 d D U P A 1
O51A O 0.3885(9) 0.3306(6) 0.2151(6) 0.0201(17) Uani 0.372(8) 1 d D U P A 2
C51 C 0.3106(8) 0.3606(10) 0.2140(5) 0.0157(14) Uani 0.628(8) 1 d D U P A 1
C51A C 0.3003(14) 0.3618(15) 0.2194(9) 0.017(2) Uani 0.372(8) 1 d D U P A 2
C52 C 0.3883(8) 0.3146(5) 0.2258(5) 0.0249(14) Uani 0.628(8) 1 d D U P A 1
H52 H 0.412064 0.299854 0.184580 0.030 Uiso 0.628(8) 1 calc R U P A 1
C52A C 0.3025(12) 0.3570(15) 0.2957(10) 0.024(2) Uani 0.372(8) 1 d D U P A 2
H52A H 0.251628 0.373959 0.313444 0.029 Uiso 0.372(8) 1 calc R U P A 2
C53 C 0.4336(6) 0.2891(5) 0.3092(3) 0.0246(11) Uani 0.628(8) 1 d D U P A 1
H53A H 0.503770 0.298946 0.328427 0.029 Uiso 0.628(8) 1 calc R U P A 1
H53B H 0.421395 0.234033 0.316069 0.029 Uiso 0.628(8) 1 calc R U P A 1
C53A C 0.3933(10) 0.3223(8) 0.3482(8) 0.027(2) Uani 0.372(8) 1 d D U P A 2
H53C H 0.380496 0.280680 0.381043 0.033 Uiso 0.372(8) 1 calc R U P A 2
H53D H 0.435626 0.361362 0.382582 0.033 Uiso 0.372(8) 1 calc R U P A 2
C54 C 0.3807(6) 0.3405(5) 0.3492(5) 0.0273(12) Uani 0.628(8) 1 d D U P A 1
H54A H 0.361937 0.311177 0.389210 0.033 Uiso 0.628(8) 1 calc R U P A 1
H54B H 0.422170 0.383922 0.375682 0.033 Uiso 0.628(8) 1 calc R U P A 1
C54A C 0.4352(10) 0.2917(9) 0.2881(5) 0.0227(17) Uani 0.372(8) 1 d D U P A 2
H54C H 0.505397 0.301297 0.305246 0.027 Uiso 0.372(8) 1 calc R U P A 2
H54D H 0.424223 0.235578 0.281545 0.027 Uiso 0.372(8) 1 calc R U P A 2
C55 C 0.23039(18) 0.28754(13) -0.01444(13) 0.0436(5) Uani 1 1 d . . . . .
H55A H 0.1860(17) 0.3139(13) -0.0618(14) 0.050(7) Uiso 1 1 d . . . . .
H55B H 0.2327(18) 0.2346(15) -0.0287(14) 0.064(7) Uiso 1 1 d . . . . .
C56 C 0.32869(16) 0.32443(12) 0.01416(13) 0.0387(5) Uani 1 1 d . . . . .
H56A H 0.3742(16) 0.2926(12) 0.0577(13) 0.043(6) Uiso 1 1 d . . . . .
H56B H 0.3579(16) 0.3344(12) -0.0244(13) 0.045(6) Uiso 1 1 d . . . . .
C57 C 0.2041(2) 0.21041(11) 0.11715(15) 0.0439(5) Uani 1 1 d . . . . .
H57A H 0.1816(18) 0.1691(15) 0.0831(15) 0.062(7) Uiso 1 1 d . . . . .
H57B H 0.175(2) 0.2103(15) 0.1580(17) 0.072(9) Uiso 1 1 d . . . . .
H57C H 0.271(2) 0.2093(14) 0.1391(15) 0.064(8) Uiso 1 1 d . . . . .
C58 C 0.04751(17) 0.27828(15) 0.00420(15) 0.0481(6) Uani 1 1 d . . . . .
H58A H 0.0272(16) 0.3182(13) -0.0316(14) 0.046(6) Uiso 1 1 d . . . . .
H58B H 0.0470(17) 0.2315(14) -0.0262(14) 0.060(7) Uiso 1 1 d . . . . .
H58C H 0.006(2) 0.2720(15) 0.0385(16) 0.075(9) Uiso 1 1 d . . . . .
C59 C 0.28092(17) 0.47768(14) -0.03322(12) 0.0405(5) Uani 1 1 d . . . . .
H59A H 0.2851(17) 0.5301(14) -0.0152(14) 0.054(7) Uiso 1 1 d . . . . .
H59B H 0.3280(17) 0.4735(13) -0.0606(14) 0.053(7) Uiso 1 1 d . . . . .
H59C H 0.2180(18) 0.4585(13) -0.0702(14) 0.055(7) Uiso 1 1 d . . . . .
C60 C 0.44150(14) 0.44833(12) 0.10078(14) 0.0361(4) Uani 1 1 d . . . . .
H60A H 0.4759(16) 0.4369(12) 0.0663(13) 0.047(6) Uiso 1 1 d . . . . .
H60B H 0.4677(16) 0.4226(12) 0.1460(14) 0.043(6) Uiso 1 1 d . . . . .
H60C H 0.4420(14) 0.5040(12) 0.1124(12) 0.038(5) Uiso 1 1 d . . . . .
C61 C 0.11132(15) 0.48525(11) 0.24261(13) 0.0361(4) Uani 1 1 d . . . . .
H61A H 0.1573(18) 0.4640(14) 0.2908(15) 0.059(7) Uiso 1 1 d . . . . .
H61B H 0.0522(17) 0.4933(12) 0.2502(13) 0.048(6) Uiso 1 1 d . . . . .
C62 C 0.14934(14) 0.55551(10) 0.21222(13) 0.0350(4) Uani 1 1 d . . . . .
H62A H 0.1728(15) 0.5948(12) 0.2502(12) 0.039(6) Uiso 1 1 d . . . . .
H62B H 0.0962(17) 0.5778(13) 0.1672(14) 0.051(7) Uiso 1 1 d . . . . .
C63 C 0.06645(17) 0.32619(12) 0.22037(14) 0.0380(4) Uani 1 1 d . . . . .
H63A H 0.0389(16) 0.2853(13) 0.1831(13) 0.045(6) Uiso 1 1 d . . . . .
H63B H 0.0191(17) 0.3420(13) 0.2435(13) 0.051(6) Uiso 1 1 d . . . . .
H63C H 0.1244(18) 0.3071(13) 0.2591(14) 0.055(7) Uiso 1 1 d . . . . .
C64 C -0.02507(13) 0.43291(13) 0.10246(15) 0.0391(5) Uani 1 1 d . . . . .
H64A H -0.0413(15) 0.3964(12) 0.0633(13) 0.037(6) Uiso 1 1 d . . . . .
H64B H -0.0726(17) 0.4313(12) 0.1302(13) 0.048(6) Uiso 1 1 d . . . . .
H64C H -0.0237(15) 0.4810(13) 0.0806(12) 0.040(6) Uiso 1 1 d . . . . .
C65 C 0.35292(14) 0.53996(11) 0.25696(12) 0.0327(4) Uani 1 1 d . . . . .
H65A H 0.3481(16) 0.5088(13) 0.3004(14) 0.051(7) Uiso 1 1 d . . . . .
H65B H 0.3591(16) 0.5932(14) 0.2687(13) 0.052(7) Uiso 1 1 d . . . . .
H65C H 0.4073(18) 0.5269(13) 0.2434(14) 0.055(7) Uiso 1 1 d . . . . .
C66 C 0.24964(16) 0.60829(10) 0.11311(14) 0.0361(4) Uani 1 1 d . . . . .
H66A H 0.2516(15) 0.6530(13) 0.1425(12) 0.040(6) Uiso 1 1 d . . . . .
H66B H 0.3061(17) 0.6072(12) 0.0962(13) 0.044(6) Uiso 1 1 d . . . . .
H66C H 0.1942(17) 0.6093(12) 0.0658(14) 0.046(6) Uiso 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 H 1.49(2) . ?
Fe1 P1 2.1793(4) . ?
Fe1 P2 2.1753(4) . ?
Fe1 P3 2.1753(4) . ?
Fe1 P4 2.1781(4) . ?
Fe1 C1 1.9962(15) . ?
P1 C5 1.8497(17) . ?
P1 C7 1.8321(18) . ?
P1 C8 1.8333(18) . ?
P2 C6 1.8537(17) . ?
P2 C9 1.8348(19) . ?
P2 C10 1.8333(19) . ?
P3 C11 1.8520(19) . ?
P3 C13 1.831(2) . ?
P3 C14 1.8320(18) . ?
P4 C12 1.8457(18) . ?
P4 C15 1.8321(18) . ?
P4 C16 1.829(2) . ?
O1 C1 1.4286(18) . ?
O1 C4 1.430(2) . ?
C1 C2 1.338(2) . ?
C2 H2 0.90(2) . ?
C2 C3 1.499(2) . ?
C3 H3A 0.99(2) . ?
C3 H3B 0.95(3) . ?
C3 C4 1.510(3) . ?
C4 H4A 0.95(2) . ?
C4 H4B 0.95(2) . ?
C5 H5A 0.950(19) . ?
C5 H5B 0.96(2) . ?
C5 C6 1.523(3) . ?
C6 H6A 1.021(19) . ?
C6 H6B 0.93(2) . ?
C7 H7A 0.94(2) . ?
C7 H7B 0.96(2) . ?
C7 H7C 0.96(2) . ?
C8 H8A 0.91(2) . ?
C8 H8B 0.96(2) . ?
C8 H8C 0.93(2) . ?
C9 H9A 0.97(2) . ?
C9 H9B 0.92(2) . ?
C9 H9C 0.98(2) . ?
C10 H10A 0.92(2) . ?
C10 H10B 0.95(2) . ?
C10 H10C 0.96(2) . ?
C11 H11A 0.92(2) . ?
C11 H11B 0.94(2) . ?
C11 C12 1.517(3) . ?
C12 H12A 0.92(2) . ?
C12 H12B 0.94(2) . ?
C13 H13A 0.93(2) . ?
C13 H13B 0.94(2) . ?
C13 H13C 0.93(2) . ?
C14 H14A 0.91(2) . ?
C14 H14B 0.92(2) . ?
C14 H14C 0.93(3) . ?
C15 H15A 0.96(2) . ?
C15 H15B 0.94(2) . ?
C15 H15C 0.95(2) . ?
C16 H16A 0.93(2) . ?
C16 H16B 0.91(2) . ?
C16 H16C 0.97(2) . ?
Fe51 HA 1.46(2) . ?
Fe51 P51 2.1658(4) . ?
Fe51 P52 2.1749(5) . ?
Fe51 P53 2.1722(4) . ?
Fe51 P54 2.1734(4) . ?
Fe51 C51 1.997(6) . ?
Fe51 C51A 1.990(9) . ?
P51 C55 1.844(2) . ?
P51 C57 1.840(2) . ?
P51 C58 1.833(2) . ?
P52 C56 1.8529(19) . ?
P52 C59 1.8370(19) . ?
P52 C60 1.830(2) . ?
P53 C61 1.8477(19) . ?
P53 C63 1.8323(19) . ?
P53 C64 1.8282(19) . ?
P54 C62 1.8478(18) . ?
P54 C65 1.8298(18) . ?
P54 C66 1.8281(19) . ?
O51 C51 1.433(10) . ?
O51 C54 1.438(7) . ?
O51A C51A 1.431(17) . ?
O51A C54A 1.437(9) . ?
C51 C52 1.354(11) . ?
C51A C52A 1.362(18) . ?
C52 H52 0.9500 . ?
C52 C53 1.496(8) . ?
C52A H52A 0.9500 . ?
C52A C53A 1.489(14) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.511(6) . ?
C53A H53C 0.9900 . ?
C53A H53D 0.9900 . ?
C53A C54A 1.504(10) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C54A H54C 0.9900 . ?
C54A H54D 0.9900 . ?
C55 H55A 1.00(2) . ?
C55 H55B 0.96(3) . ?
C55 C56 1.510(3) . ?
C56 H56A 1.01(2) . ?
C56 H56B 0.94(2) . ?
C57 H57A 0.93(3) . ?
C57 H57B 0.96(3) . ?
C57 H57C 0.94(3) . ?
C58 H58A 0.93(2) . ?
C58 H58B 0.98(3) . ?
C58 H58C 1.00(3) . ?
C59 H59A 0.96(2) . ?
C59 H59B 0.97(2) . ?
C59 H59C 1.00(2) . ?
C60 H60A 0.94(2) . ?
C60 H60B 0.90(2) . ?
C60 H60C 0.99(2) . ?
C61 H61A 0.98(2) . ?
C61 H61B 0.93(2) . ?
C61 C62 1.517(3) . ?
C62 H62A 0.95(2) . ?
C62 H62B 1.00(2) . ?
C63 H63A 0.97(2) . ?
C63 H63B 0.96(2) . ?
C63 H63C 0.97(2) . ?
C64 H64A 0.92(2) . ?
C64 H64B 0.98(2) . ?
C64 H64C 0.93(2) . ?
C65 H65A 0.97(2) . ?
C65 H65B 0.95(2) . ?
C65 H65C 0.94(3) . ?
C66 H66A 0.94(2) . ?
C66 H66B 0.97(2) . ?
C66 H66C 0.97(2) . ?

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
P1 Fe1 H 87.9(8) . . ?
P2 Fe1 H 83.9(8) . . ?
P2 Fe1 P1 86.040(16) . . ?
P2 Fe1 P3 168.445(19) . . ?
P2 Fe1 P4 93.640(17) . . ?
P3 Fe1 H 84.6(8) . . ?
P3 Fe1 P1 93.975(17) . . ?
P3 Fe1 P4 85.481(17) . . ?
P4 Fe1 H 87.8(8) . . ?
P4 Fe1 P1 175.710(18) . . ?
C1 Fe1 H 179.0(8) . . ?
C1 Fe1 P1 92.98(4) . . ?
C1 Fe1 P2 96.53(4) . . ?
C1 Fe1 P3 95.01(4) . . ?
C1 Fe1 P4 91.31(4) . . ?
C5 P1 Fe1 109.85(6) . . ?
C7 P1 Fe1 123.45(7) . . ?
C7 P1 C5 102.15(9) . . ?
C7 P1 C8 99.33(9) . . ?
C8 P1 Fe1 119.33(7) . . ?
C8 P1 C5 98.96(9) . . ?
C6 P2 Fe1 110.27(6) . . ?
C9 P2 Fe1 120.12(7) . . ?
C9 P2 C6 99.99(9) . . ?
C10 P2 Fe1 122.97(7) . . ?
C10 P2 C6 100.12(9) . . ?
C10 P2 C9 99.47(11) . . ?
C11 P3 Fe1 110.92(6) . . ?
C13 P3 Fe1 121.01(7) . . ?
C13 P3 C11 99.56(10) . . ?
C13 P3 C14 100.36(11) . . ?
C14 P3 Fe1 120.53(7) . . ?
C14 P3 C11 100.85(10) . . ?
C12 P4 Fe1 110.12(6) . . ?
C15 P4 Fe1 119.31(7) . . ?
C15 P4 C12 99.25(9) . . ?
C16 P4 Fe1 121.89(7) . . ?
C16 P4 C12 102.12(10) . . ?
C16 P4 C15 100.70(10) . . ?
C1 O1 C4 109.78(12) . . ?
O1 C1 Fe1 116.90(10) . . ?
C2 C1 Fe1 136.01(12) . . ?
C2 C1 O1 107.07(13) . . ?
C1 C2 H2 124.6(14) . . ?
C1 C2 C3 113.99(15) . . ?
C3 C2 H2 121.4(14) . . ?
C2 C3 H3A 115.4(13) . . ?
C2 C3 H3B 112.1(15) . . ?
C2 C3 C4 100.41(14) . . ?
H3A C3 H3B 109.3(19) . . ?
C4 C3 H3A 109.4(13) . . ?
C4 C3 H3B 109.8(15) . . ?
O1 C4 C3 107.20(13) . . ?
O1 C4 H4A 108.2(12) . . ?
O1 C4 H4B 108.8(13) . . ?
C3 C4 H4A 115.3(11) . . ?
C3 C4 H4B 111.9(14) . . ?
H4A C4 H4B 105.2(17) . . ?
P1 C5 H5A 107.5(11) . . ?
P1 C5 H5B 109.4(12) . . ?
H5A C5 H5B 107.1(16) . . ?
C6 C5 P1 106.83(11) . . ?
C6 C5 H5A 112.2(11) . . ?
C6 C5 H5B 113.7(12) . . ?
P2 C6 H6A 108.3(10) . . ?
P2 C6 H6B 110.4(13) . . ?
C5 C6 P2 108.23(11) . . ?
C5 C6 H6A 109.8(11) . . ?
C5 C6 H6B 112.7(13) . . ?
H6A C6 H6B 107.4(16) . . ?
P1 C7 H7A 110.7(13) . . ?
P1 C7 H7B 109.5(12) . . ?
P1 C7 H7C 110.9(12) . . ?
H7A C7 H7B 111.9(18) . . ?
H7A C7 H7C 106.4(18) . . ?
H7B C7 H7C 107.4(17) . . ?
P1 C8 H8A 112.7(15) . . ?
P1 C8 H8B 108.2(14) . . ?
P1 C8 H8C 107.0(14) . . ?
H8A C8 H8B 111(2) . . ?
H8A C8 H8C 110(2) . . ?
H8B C8 H8C 107.5(19) . . ?
P2 C9 H9A 107.5(12) . . ?
P2 C9 H9B 106.9(14) . . ?
P2 C9 H9C 109.0(13) . . ?
H9A C9 H9B 110.0(18) . . ?
H9A C9 H9C 112.0(18) . . ?
H9B C9 H9C 111.2(18) . . ?
P2 C10 H10A 109.8(14) . . ?
P2 C10 H10B 111.8(13) . . ?
P2 C10 H10C 110.3(13) . . ?
H10A C10 H10B 103.0(18) . . ?
H10A C10 H10C 111.7(19) . . ?
H10B C10 H10C 110.0(19) . . ?
P3 C11 H11A 109.4(14) . . ?
P3 C11 H11B 106.0(12) . . ?
H11A C11 H11B 109.2(18) . . ?
C12 C11 P3 108.56(12) . . ?
C12 C11 H11A 111.8(14) . . ?
C12 C11 H11B 111.6(12) . . ?
P4 C12 H12A 106.5(13) . . ?
P4 C12 H12B 110.7(13) . . ?
C11 C12 P4 106.82(13) . . ?
C11 C12 H12A 111.1(13) . . ?
C11 C12 H12B 112.4(13) . . ?
H12A C12 H12B 109.1(18) . . ?
P3 C13 H13A 109.3(13) . . ?
P3 C13 H13B 111.3(14) . . ?
P3 C13 H13C 106.6(14) . . ?
H13A C13 H13B 106.2(18) . . ?
H13A C13 H13C 113.4(19) . . ?
H13B C13 H13C 110.2(19) . . ?
P3 C14 H14A 111.0(15) . . ?
P3 C14 H14B 108.2(15) . . ?
P3 C14 H14C 108.8(16) . . ?
H14A C14 H14B 112(2) . . ?
H14A C14 H14C 105(2) . . ?
H14B C14 H14C 112(2) . . ?
P4 C15 H15A 110.0(13) . . ?
P4 C15 H15B 108.5(13) . . ?
P4 C15 H15C 111.6(13) . . ?
H15A C15 H15B 108.5(18) . . ?
H15A C15 H15C 107.7(18) . . ?
H15B C15 H15C 110.5(17) . . ?
P4 C16 H16A 110.8(14) . . ?
P4 C16 H16B 107.3(14) . . ?
P4 C16 H16C 110.7(13) . . ?
H16A C16 H16B 108.0(19) . . ?
H16A C16 H16C 108.5(19) . . ?
H16B C16 H16C 111.5(18) . . ?
P51 Fe51 HA 86.2(8) . . ?
P51 Fe51 P52 86.206(18) . . ?
P51 Fe51 P53 92.872(18) . . ?
P51 Fe51 P54 174.642(18) . . ?
P52 Fe51 HA 85.4(8) . . ?
P53 Fe51 HA 85.1(8) . . ?
P53 Fe51 P52 170.539(18) . . ?
P53 Fe51 P54 85.850(16) . . ?
P54 Fe51 HA 88.5(8) . . ?
P54 Fe51 P52 94.199(17) . . ?
C51 Fe51 HA 178.0(9) . . ?
C51 Fe51 P51 92.7(5) . . ?
C51 Fe51 P52 92.8(3) . . ?
C51 Fe51 P53 96.6(3) . . ?
C51 Fe51 P54 92.7(5) . . ?
C51A Fe51 HA 175.9(10) . . ?
C51A Fe51 P51 93.8(8) . . ?
C51A Fe51 P52 98.7(6) . . ?
C51A Fe51 P53 90.8(6) . . ?
C51A Fe51 P54 91.4(8) . . ?
C55 P51 Fe51 110.65(7) . . ?
C57 P51 Fe51 119.98(8) . . ?
C57 P51 C55 101.42(11) . . ?
C58 P51 Fe51 122.36(8) . . ?
C58 P51 C55 100.15(12) . . ?
C58 P51 C57 98.76(12) . . ?
C56 P52 Fe51 109.55(7) . . ?
C59 P52 Fe51 117.80(8) . . ?
C59 P52 C56 99.54(10) . . ?
C60 P52 Fe51 124.37(7) . . ?
C60 P52 C56 101.53(10) . . ?
C60 P52 C59 100.33(11) . . ?
C61 P53 Fe51 109.97(6) . . ?
C63 P53 Fe51 123.64(7) . . ?
C63 P53 C61 101.14(10) . . ?
C64 P53 Fe51 118.44(8) . . ?
C64 P53 C61 99.76(10) . . ?
C64 P53 C63 100.21(11) . . ?
C62 P54 Fe51 110.83(6) . . ?
C65 P54 Fe51 119.59(6) . . ?
C65 P54 C62 101.50(10) . . ?
C66 P54 Fe51 121.91(7) . . ?
C66 P54 C62 99.64(10) . . ?
C66 P54 C65 99.90(10) . . ?
C51 O51 C54 108.9(6) . . ?
C51A O51A C54A 107.6(8) . . ?
O51 C51 Fe51 117.5(6) . . ?
C52 C51 Fe51 136.0(8) . . ?
C52 C51 O51 106.4(5) . . ?
O51A C51A Fe51 116.1(10) . . ?
C52A C51A Fe51 135.7(13) . . ?
C52A C51A O51A 107.8(9) . . ?
C51 C52 H52 122.9 . . ?
C51 C52 C53 114.2(7) . . ?
C53 C52 H52 122.9 . . ?
C51A C52A H52A 123.7 . . ?
C51A C52A C53A 112.7(12) . . ?
C53A C52A H52A 123.7 . . ?
C52 C53 H53A 111.8 . . ?
C52 C53 H53B 111.8 . . ?
C52 C53 C54 99.8(6) . . ?
H53A C53 H53B 109.5 . . ?
C54 C53 H53A 111.8 . . ?
C54 C53 H53B 111.8 . . ?
C52A C53A H53C 111.7 . . ?
C52A C53A H53D 111.7 . . ?
C52A C53A C54A 100.5(11) . . ?
H53C C53A H53D 109.5 . . ?
C54A C53A H53C 111.7 . . ?
C54A C53A H53D 111.7 . . ?
O51 C54 C53 107.0(6) . . ?
O51 C54 H54A 110.3 . . ?
O51 C54 H54B 110.3 . . ?
C53 C54 H54A 110.3 . . ?
C53 C54 H54B 110.3 . . ?
H54A C54 H54B 108.6 . . ?
O51A C54A C53A 107.6(10) . . ?
O51A C54A H54C 110.2 . . ?
O51A C54A H54D 110.2 . . ?
C53A C54A H54C 110.2 . . ?
C53A C54A H54D 110.2 . . ?
H54C C54A H54D 108.5 . . ?
P51 C55 H55A 104.0(13) . . ?
P51 C55 H55B 112.5(15) . . ?
H55A C55 H55B 106.5(19) . . ?
C56 C55 P51 108.43(13) . . ?
C56 C55 H55A 112.4(13) . . ?
C56 C55 H55B 112.7(15) . . ?
P52 C56 H56A 107.3(12) . . ?
P52 C56 H56B 105.8(13) . . ?
C55 C56 P52 107.64(14) . . ?
C55 C56 H56A 110.5(12) . . ?
C55 C56 H56B 116.3(13) . . ?
H56A C56 H56B 108.9(18) . . ?
P51 C57 H57A 109.3(15) . . ?
P51 C57 H57B 108.7(16) . . ?
P51 C57 H57C 106.9(16) . . ?
H57A C57 H57B 110(2) . . ?
H57A C57 H57C 111(2) . . ?
H57B C57 H57C 110(2) . . ?
P51 C58 H58A 105.5(14) . . ?
P51 C58 H58B 108.5(14) . . ?
P51 C58 H58C 111.8(16) . . ?
H58A C58 H58B 107.1(19) . . ?
H58A C58 H58C 113(2) . . ?
H58B C58 H58C 111(2) . . ?
P52 C59 H59A 105.0(14) . . ?
P52 C59 H59B 111.2(14) . . ?
P52 C59 H59C 109.4(13) . . ?
H59A C59 H59B 105.2(19) . . ?
H59A C59 H59C 118.7(19) . . ?
H59B C59 H59C 107.2(19) . . ?
P52 C60 H60A 109.9(14) . . ?
P52 C60 H60B 109.2(14) . . ?
P52 C60 H60C 107.4(12) . . ?
H60A C60 H60B 109.0(19) . . ?
H60A C60 H60C 112.1(18) . . ?
H60B C60 H60C 109.0(18) . . ?
P53 C61 H61A 104.8(14) . . ?
P53 C61 H61B 107.8(13) . . ?
H61A C61 H61B 109.6(19) . . ?
C62 C61 P53 107.38(13) . . ?
C62 C61 H61A 113.0(14) . . ?
C62 C61 H61B 113.7(13) . . ?
P54 C62 H62A 110.3(13) . . ?
P54 C62 H62B 106.9(13) . . ?
C61 C62 P54 108.28(12) . . ?
C61 C62 H62A 114.4(12) . . ?
C61 C62 H62B 108.7(13) . . ?
H62A C62 H62B 107.9(17) . . ?
P53 C63 H63A 109.5(13) . . ?
P53 C63 H63B 108.4(13) . . ?
P53 C63 H63C 110.0(14) . . ?
H63A C63 H63B 108.0(18) . . ?
H63A C63 H63C 108.5(19) . . ?
H63B C63 H63C 112.4(19) . . ?
P53 C64 H64A 106.8(13) . . ?
P53 C64 H64B 111.3(13) . . ?
P53 C64 H64C 109.5(13) . . ?
H64A C64 H64B 108.6(18) . . ?
H64A C64 H64C 109.6(18) . . ?
H64B C64 H64C 110.9(18) . . ?
P54 C65 H65A 108.1(13) . . ?
P54 C65 H65B 109.1(14) . . ?
P54 C65 H65C 109.5(15) . . ?
H65A C65 H65B 113.1(19) . . ?
H65A C65 H65C 111.4(19) . . ?
H65B C65 H65C 105.5(19) . . ?
P54 C66 H66A 109.7(13) . . ?
P54 C66 H66B 111.5(13) . . ?
P54 C66 H66C 110.1(13) . . ?
H66A C66 H66B 108.7(18) . . ?
H66A C66 H66C 110.0(18) . . ?
H66B C66 H66C 106.8(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
Fe1 P1 C5 C6 40.43(12) . . . . ?
Fe1 P2 C6 C5 34.63(13) . . . . ?
Fe1 P3 C11 C12 31.90(15) . . . . ?
Fe1 P4 C12 C11 41.39(14) . . . . ?
Fe1 C1 C2 C3 -177.45(14) . . . . ?
P1 C5 C6 P2 -45.52(14) . . . . ?
P3 C11 C12 P4 -44.24(16) . . . . ?
O1 C1 C2 C3 0.8(2) . . . . ?
C1 O1 C4 C3 -12.4(2) . . . . ?
C1 C2 C3 C4 -7.8(2) . . . . ?
C2 C3 C4 O1 11.7(2) . . . . ?
C4 O1 C1 Fe1 -174.01(11) . . . . ?
C4 O1 C1 C2 7.38(19) . . . . ?
C7 P1 C5 C6 173.05(12) . . . . ?
C8 P1 C5 C6 -85.31(13) . . . . ?
C9 P2 C6 C5 162.09(13) . . . . ?
C10 P2 C6 C5 -96.31(14) . . . . ?
C13 P3 C11 C12 160.49(14) . . . . ?
C14 P3 C11 C12 -96.92(15) . . . . ?
C15 P4 C12 C11 -84.61(14) . . . . ?
C16 P4 C12 C11 172.24(13) . . . . ?
Fe51 P51 C55 C56 33.99(17) . . . . ?
Fe51 P52 C56 C55 38.81(16) . . . . ?
Fe51 P53 C61 C62 40.02(16) . . . . ?
Fe51 P54 C62 C61 32.84(16) . . . . ?
Fe51 C51 C52 C53 -176.2(13) . . . . ?
Fe51 C51A C52A C53A -172(2) . . . . ?
P51 C55 C56 P52 -44.24(18) . . . . ?
P53 C61 C62 P54 -44.09(17) . . . . ?
O51 C51 C52 C53 -0.9(16) . . . . ?
O51A C51A C52A C53A 0(3) . . . . ?
C51 O51 C54 C53 -19.8(13) . . . . ?
C51 C52 C53 C54 -10.4(13) . . . . ?
C51A O51A C54A C53A -19.8(19) . . . . ?
C51A C52A C53A C54A -12(3) . . . . ?
C52 C53 C54 O51 17.6(10) . . . . ?
C52A C53A C54A O51A 18.7(18) . . . . ?
C54 O51 C51 Fe51 -170.8(9) . . . . ?
C54 O51 C51 C52 13.0(15) . . . . ?
C54A O51A C51A Fe51 -173.8(14) . . . . ?
C54A O51A C51A C52A 12(3) . . . . ?
C57 P51 C55 C56 -94.39(17) . . . . ?
C58 P51 C55 C56 164.43(16) . . . . ?
C59 P52 C56 C55 -85.35(16) . . . . ?
C60 P52 C56 C55 171.95(15) . . . . ?
C63 P53 C61 C62 172.26(15) . . . . ?
C64 P53 C61 C62 -85.19(16) . . . . ?
C65 P54 C62 C61 -95.23(16) . . . . ?
C66 P54 C62 C61 162.51(15) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id LAB302
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.429
_oxdiff_exptl_absorpt_empirical_full_min 0.812
