# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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 
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data_fenife_073122_0m_4
_database_code_depnum_ccdc_archive 'CCDC 2231567'
loop_
_audit_author_name
_audit_author_address
'Nattamai S. Bhuvanesh'
;Texas A and M University
United States of America
;
_audit_update_record             
;
2022-12-19 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_audit_creation_date             2022-11-11
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
marcetta@chem.tamu.edu
nbhuv@mail.chem.tamu.edu
_chemical_name_common            ?
_chemical_name_systematic        FeNiFe
_chemical_formula_moiety         
'2(C9 H18 Fe N3 Ni0.5 O S2), 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C22 H42 B2 F8 Fe2 N8 Ni O2 S4'
_chemical_formula_weight         922.90
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
S S 0.1246 0.1234 '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                   7.7964(6)
_cell_length_b                   11.2004(8)
_cell_length_c                   20.4101(14)
_cell_angle_alpha                85.406(2)
_cell_angle_beta                 89.714(2)
_cell_angle_gamma                82.273(2)
_cell_volume                     1760.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5275
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      24.883
_cell_measurement_theta_min      2.609
_shelx_estimated_absorpt_T_max   0.976
_shelx_estimated_absorpt_T_min   0.799
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0886 before and 0.0441 after correction.
 
For component 2:
 wR2(int) was 0.0950 before and 0.0491 after correction.
 The Ratio of minimum to maximum transmission is 0.79.

Final HKLF 4 output contains 42174 reflections, Rint = 0.0817
 (20391 with I > 3sig(I), Rint = 0.0642)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic greenish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             944
_exptl_crystal_preparation       'CH3CN and Et2O,Magnetic properties'
_exptl_crystal_recrystallization_method 'vapor diffusion'
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.015
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.875
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5987
_diffrn_reflns_point_group_measured_fraction_full 0.875
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.070
_diffrn_reflns_theta_max         25.070
_diffrn_reflns_theta_min         1.841
_diffrn_ambient_temperature      110.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.875
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'Bruker Quest (PHOTON III)'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_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                5045
_reflns_number_total             5987
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX 4 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         5987
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0675
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+28.4729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1709
_refine_special_details          
;1.	Several crystals were tried and found all of them
 multiply twinned/cracked. The best data was taken, containing
 only twin components, and was used for further analysis.
 Significant number of reflections (40293) were in both the
 domains. Both the first and the second domains had similar
 number of non-overlapping reflections (1492 and 1356
 respectively) with similar mean(I/sigma) (11.8 and 13.4
 respectively). 
2.	TWINABS as implemented in APEX4 was used for
 correcting absorption and systematic errors, and also
 to generate hklf4 (containing non-overlapping reflections)
 and hklf5 (containing reflections only from the major
 component). While the former was used for structure solution,
 the latter was used for the final least squares refinement.  
3.	A few reflections showed higher than 10 error/esd
 in the list of Bad Reflections after final least squares
 refinement. Our effort to omit them resulted in a few more
 reflections with the value greater than 10. Since this was
 continuing with an increase in wR2, only the first set of
 Bad Reflections were omitted. 
4.	It should be noted that the completeness was
 slightly lower (94.6 percent at 0.84 ang resolution), as
 the SAINT (as implemented in APEX4) rejected significant
 amount of reflections 23010 out of 103480 predicted
 reflections). Several trials were made to modify the
 data integration and absorption correction parameters.
 These efforts did not improve the completeness or final
 reliability factors. 
 Also, Our efforts to increase the crystal to detector
 distance to improve the data integration nor improve
 the final results. 
 We had very similar issues, twinning with high overlap,
 in this class of compounds that we have tried.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.54635
 0.45365
2. Restrained distances
 C13-C14 \\sim C13-C12
 with sigma of 0.02
 C4-C3 \\sim C4-C5
 with sigma of 0.02
 C7-C6 \\sim C16-C15
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C7)
Uanis(C8) = Uanis(C9)
Uanis(C6) = Uanis(C15)
Uanis(C6) = Uanis(C7) = Uanis(C15)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B)
4.b Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C6S(H6SA,H6SB,H6SC)
;
_atom_sites_solution_hydrogens   geom
_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
Ni1 Ni 1.000000 0.500000 0.000000 0.0147(5) Uani 1 2 d S . P . .
Fe1 Fe 0.7784(2) 0.58941(16) 0.10842(8) 0.0160(4) Uani 1 1 d . . . . .
S1 S 0.7217(4) 0.4985(3) 0.01899(15) 0.0174(7) Uani 1 1 d . . . . .
S2 S 0.9610(4) 0.6762(3) 0.04216(14) 0.0164(6) Uani 1 1 d . . . . .
O1 O 0.5118(13) 0.7850(9) 0.1011(6) 0.048(3) Uani 1 1 d . . . . .
N1 N 0.7342(13) 0.4402(10) 0.1631(5) 0.023(2) Uani 1 1 d . . . . .
N2 N 0.9448(13) 0.5927(9) 0.1830(5) 0.017(2) Uani 1 1 d . . . . .
N3 N 0.6119(13) 0.7006(9) 0.1153(5) 0.023(2) Uani 1 1 d . . . . .
C1 C 0.6851(16) 0.3500(12) 0.0577(6) 0.022(3) Uani 1 1 d . . . . .
H1A H 0.596256 0.317018 0.032675 0.027 Uiso 1 1 calc R U . . .
H1B H 0.793643 0.292892 0.057710 0.027 Uiso 1 1 calc R U . . .
C2 C 0.6259(18) 0.3646(12) 0.1265(6) 0.025(3) Uani 1 1 d . . . . .
H2A H 0.630671 0.283767 0.150430 0.030 Uiso 1 1 calc R U . . .
H2B H 0.503898 0.403115 0.125737 0.030 Uiso 1 1 calc R U . . .
C3 C 0.6425(17) 0.4694(12) 0.2257(6) 0.024(3) Uani 1 1 d D . . . .
H3A H 0.601151 0.395602 0.246374 0.029 Uiso 1 1 calc R U . . .
H3B H 0.540073 0.530399 0.215477 0.029 Uiso 1 1 calc R U . . .
C4 C 0.7575(17) 0.5176(12) 0.2740(6) 0.028(3) Uani 1 1 d D . . . .
H4A H 0.845080 0.450385 0.291417 0.033 Uiso 1 1 calc R U . . .
H4B H 0.685994 0.545633 0.311382 0.033 Uiso 1 1 calc R U . . .
C5 C 0.8506(19) 0.6205(12) 0.2457(6) 0.026(3) Uani 1 1 d D . . . .
H5A H 0.765206 0.693848 0.237025 0.031 Uiso 1 1 calc R U . . .
H5B H 0.934697 0.638136 0.278577 0.031 Uiso 1 1 calc R U . . .
C6 C 0.9125(16) 0.3756(11) 0.1777(7) 0.0219(16) Uani 1 1 d D . . . .
H6A H 0.952754 0.327519 0.140621 0.026 Uiso 1 1 calc R U . . .
H6B H 0.909587 0.319392 0.217564 0.026 Uiso 1 1 calc R U . . .
C7 C 1.0387(16) 0.4654(11) 0.1886(7) 0.0219(16) Uani 1 1 d D . . . .
H7A H 1.092494 0.446979 0.232703 0.026 Uiso 1 1 calc R U . . .
H7B H 1.131828 0.457853 0.155428 0.026 Uiso 1 1 calc R U . . .
C8 C 1.0660(16) 0.6845(12) 0.1693(6) 0.022(2) Uani 1 1 d . . . . .
H8A H 1.163525 0.667796 0.201074 0.026 Uiso 1 1 calc R U . . .
H8B H 1.004325 0.765857 0.175817 0.026 Uiso 1 1 calc R U . . .
C9 C 1.1365(16) 0.6838(12) 0.1004(6) 0.022(2) Uani 1 1 d . . . . .
H9A H 1.226637 0.613170 0.097400 0.026 Uiso 1 1 calc R U . . .
H9B H 1.190245 0.757990 0.089371 0.026 Uiso 1 1 calc R U . . .
Ni2 Ni 0.500000 0.000000 0.500000 0.0170(5) Uani 1 2 d S . P . .
Fe2 Fe 0.2701(2) 0.05847(17) 0.38435(8) 0.0175(4) Uani 1 1 d . . . . .
S3 S 0.2210(4) -0.0087(3) 0.48821(15) 0.0182(7) Uani 1 1 d . . . . .
S4 S 0.4459(4) 0.1653(3) 0.43339(15) 0.0197(7) Uani 1 1 d . . . . .
F1 F 0.7638(12) -0.0784(8) 0.1919(4) 0.046(2) Uani 1 1 d . . . . .
F2 F 0.6744(11) 0.0669(8) 0.1108(5) 0.045(2) Uani 1 1 d . . . . .
F3 F 0.8762(13) 0.0961(8) 0.1834(5) 0.053(3) Uani 1 1 d . . . . .
F4 F 0.9422(11) -0.0416(7) 0.1083(4) 0.040(2) Uani 1 1 d . . . . .
B1 B 0.815(2) 0.0130(15) 0.1474(8) 0.027(3) Uani 1 1 d . . . . .
F5 F 0.3252(14) 0.3928(7) 0.3196(5) 0.054(3) Uani 1 1 d . . . . .
F6 F 0.1346(10) 0.5130(8) 0.3750(4) 0.041(2) Uani 1 1 d . . . . .
F7 F 0.3045(11) 0.5932(7) 0.2973(4) 0.0332(19) Uani 1 1 d . . . . .
F8 F 0.4194(12) 0.5098(11) 0.3942(5) 0.069(3) Uani 1 1 d . . . . .
B2 B 0.298(2) 0.5005(16) 0.3473(7) 0.030(4) Uani 1 1 d . . . . .
O2 O -0.0019(13) 0.2449(10) 0.3500(6) 0.048(3) Uani 1 1 d . . . . .
N1S N 0.2698(15) 0.2553(11) 0.1059(6) 0.034(3) Uani 1 1 d . . . . .
C2S C 0.2765(16) 0.1690(12) 0.0785(6) 0.023(3) Uani 1 1 d . . . . .
C3S C 0.2859(19) 0.0602(12) 0.0446(7) 0.032(3) Uani 1 1 d . . . . .
H3SA H 0.380557 0.000940 0.063225 0.047 Uiso 1 1 calc R U . . .
H3SB H 0.307088 0.079083 -0.002165 0.047 Uiso 1 1 calc R U . . .
H3SC H 0.176329 0.026729 0.049865 0.047 Uiso 1 1 calc R U . . .
N4 N 0.2383(13) -0.1061(9) 0.3579(5) 0.019(2) Uani 1 1 d . . . . .
N4S N 0.7794(15) 0.7122(12) 0.4277(7) 0.042(3) Uani 1 1 d . . . . .
C5S C 0.7856(17) 0.6135(13) 0.4427(7) 0.028(3) Uani 1 1 d . . . . .
C6S C 0.7919(18) 0.4850(12) 0.4613(7) 0.030(3) Uani 1 1 d . . . . .
H6SA H 0.686105 0.457070 0.446127 0.045 Uiso 1 1 calc R U . . .
H6SB H 0.801027 0.470507 0.509193 0.045 Uiso 1 1 calc R U . . .
H6SC H 0.892706 0.440654 0.440985 0.045 Uiso 1 1 calc R U . . .
N5 N 0.4392(13) 0.0435(10) 0.3097(5) 0.021(2) Uani 1 1 d . . . . .
N6 N 0.1019(14) 0.1595(9) 0.3585(5) 0.021(2) Uani 1 1 d . . . . .
C10 C 0.1868(17) -0.1634(12) 0.4762(7) 0.025(3) Uani 1 1 d . . . . .
H10A H 0.295139 -0.218956 0.485951 0.030 Uiso 1 1 calc R U . . .
H10B H 0.096146 -0.188225 0.506498 0.030 Uiso 1 1 calc R U . . .
C11 C 0.1317(16) -0.1706(12) 0.4057(6) 0.022(3) Uani 1 1 d . . . . .
H11A H 0.141351 -0.256587 0.396191 0.026 Uiso 1 1 calc R U . . .
H11B H 0.008812 -0.135223 0.400172 0.026 Uiso 1 1 calc R U . . .
C12 C 0.1523(18) -0.1001(13) 0.2919(6) 0.027(3) Uani 1 1 d D . . . .
H12A H 0.046487 -0.040247 0.291159 0.033 Uiso 1 1 calc R U . . .
H12B H 0.116847 -0.179867 0.285244 0.033 Uiso 1 1 calc R U . . .
C13 C 0.2687(17) -0.0653(12) 0.2361(6) 0.028(3) Uani 1 1 d D . . . .
H13A H 0.360910 -0.133924 0.231174 0.034 Uiso 1 1 calc R U . . .
H13B H 0.199691 -0.052695 0.194920 0.034 Uiso 1 1 calc R U . . .
C14 C 0.3525(19) 0.0461(13) 0.2438(6) 0.031(3) Uani 1 1 d D . . . .
H14A H 0.263458 0.118024 0.238276 0.037 Uiso 1 1 calc R U . . .
H14B H 0.439542 0.053723 0.208807 0.037 Uiso 1 1 calc R U . . .
C15 C 0.4208(16) -0.1673(11) 0.3551(6) 0.0219(16) Uani 1 1 d D . . . .
H15A H 0.426105 -0.235159 0.326626 0.026 Uiso 1 1 calc R U . . .
H15B H 0.459741 -0.200714 0.399749 0.026 Uiso 1 1 calc R U . . .
C16 C 0.5418(16) -0.0777(11) 0.3279(6) 0.025(3) Uani 1 1 d D . . . .
H16A H 0.629843 -0.069835 0.361542 0.030 Uiso 1 1 calc R U . . .
H16B H 0.602610 -0.108451 0.288731 0.030 Uiso 1 1 calc R U . . .
C17 C 0.5493(16) 0.1434(11) 0.3057(6) 0.022(3) Uani 1 1 d . . . . .
H17A H 0.480439 0.218220 0.285965 0.026 Uiso 1 1 calc R U . . .
H17B H 0.648360 0.122341 0.276324 0.026 Uiso 1 1 calc R U . . .
C18 C 0.6167(16) 0.1670(12) 0.3713(6) 0.020(3) Uani 1 1 d . . . . .
H18A H 0.659288 0.246690 0.368098 0.024 Uiso 1 1 calc R U . . .
H18B H 0.715090 0.104470 0.384581 0.024 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
Ni1 Fe1 2.9558(17) 2_765 ?
Ni1 Fe1 2.9558(17) . ?
Ni1 S1 2.204(3) 2_765 ?
Ni1 S1 2.204(3) . ?
Ni1 S2 2.199(3) 2_765 ?
Ni1 S2 2.199(3) . ?
Fe1 S1 2.234(3) . ?
Fe1 S2 2.223(3) . ?
Fe1 N1 2.002(11) . ?
Fe1 N2 2.011(10) . ?
Fe1 N3 1.687(10) . ?
S1 C1 1.841(13) . ?
S2 C9 1.832(12) . ?
O1 N3 1.161(13) . ?
N1 C2 1.512(16) . ?
N1 C3 1.499(15) . ?
N1 C6 1.498(16) . ?
N2 C5 1.505(16) . ?
N2 C7 1.509(15) . ?
N2 C8 1.497(15) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.490(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.512(14) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.518(14) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.527(15) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.508(17) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
Ni2 Fe2 2.9480(18) 2_656 ?
Ni2 Fe2 2.9481(18) . ?
Ni2 S3 2.206(3) . ?
Ni2 S3 2.206(3) 2_656 ?
Ni2 S4 2.202(3) . ?
Ni2 S4 2.202(3) 2_656 ?
Fe2 S3 2.241(3) . ?
Fe2 S4 2.227(4) . ?
Fe2 N4 2.009(10) . ?
Fe2 N5 2.012(10) . ?
Fe2 N6 1.671(11) . ?
S3 C10 1.824(13) . ?
S4 C18 1.835(12) . ?
F1 B1 1.409(18) . ?
F2 B1 1.371(18) . ?
F3 B1 1.367(18) . ?
F4 B1 1.380(17) . ?
F5 B2 1.363(19) . ?
F6 B2 1.388(18) . ?
F7 B2 1.402(18) . ?
F8 B2 1.367(18) . ?
O2 N6 1.169(14) . ?
N1S C2S 1.150(16) . ?
C2S C3S 1.441(18) . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?
N4 C11 1.485(15) . ?
N4 C12 1.500(16) . ?
N4 C15 1.497(15) . ?
N4S C5S 1.118(18) . ?
C5S C6S 1.453(19) . ?
C6S H6SA 0.9800 . ?
C6S H6SB 0.9800 . ?
C6S H6SC 0.9800 . ?
N5 C14 1.505(15) . ?
N5 C16 1.501(16) . ?
N5 C17 1.496(15) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.515(18) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.512(14) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.504(15) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.537(15) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.496(17) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Fe1 Ni1 Fe1 180.0 . 2_765 ?
S1 Ni1 Fe1 48.67(8) 2_765 2_765 ?
S1 Ni1 Fe1 131.33(8) . 2_765 ?
S1 Ni1 Fe1 48.67(8) . . ?
S1 Ni1 Fe1 131.33(8) 2_765 . ?
S1 Ni1 S1 180.0 2_765 . ?
S2 Ni1 Fe1 48.41(8) 2_765 2_765 ?
S2 Ni1 Fe1 131.59(8) 2_765 . ?
S2 Ni1 Fe1 131.59(8) . 2_765 ?
S2 Ni1 Fe1 48.41(8) . . ?
S2 Ni1 S1 95.16(11) 2_765 . ?
S2 Ni1 S1 84.84(11) . . ?
S2 Ni1 S1 95.16(11) . 2_765 ?
S2 Ni1 S1 84.84(11) 2_765 2_765 ?
S2 Ni1 S2 180.0 . 2_765 ?
S1 Fe1 Ni1 47.80(8) . . ?
S2 Fe1 Ni1 47.71(9) . . ?
S2 Fe1 S1 83.57(12) . . ?
N1 Fe1 Ni1 104.8(3) . . ?
N1 Fe1 S1 88.5(3) . . ?
N1 Fe1 S2 146.5(3) . . ?
N1 Fe1 N2 80.0(4) . . ?
N2 Fe1 Ni1 104.2(3) . . ?
N2 Fe1 S1 145.8(3) . . ?
N2 Fe1 S2 88.5(3) . . ?
N3 Fe1 Ni1 135.4(4) . . ?
N3 Fe1 S1 105.8(4) . . ?
N3 Fe1 S2 103.4(4) . . ?
N3 Fe1 N1 110.1(5) . . ?
N3 Fe1 N2 108.4(5) . . ?
Ni1 S1 Fe1 83.53(11) . . ?
C1 S1 Ni1 109.8(4) . . ?
C1 S1 Fe1 99.7(4) . . ?
Ni1 S2 Fe1 83.88(11) . . ?
C9 S2 Ni1 109.3(4) . . ?
C9 S2 Fe1 99.9(4) . . ?
C2 N1 Fe1 111.8(8) . . ?
C3 N1 Fe1 112.0(8) . . ?
C3 N1 C2 107.8(10) . . ?
C6 N1 Fe1 103.2(7) . . ?
C6 N1 C2 111.9(10) . . ?
C6 N1 C3 110.2(10) . . ?
C5 N2 Fe1 111.3(8) . . ?
C5 N2 C7 110.7(9) . . ?
C7 N2 Fe1 102.5(7) . . ?
C8 N2 Fe1 112.5(7) . . ?
C8 N2 C5 107.8(9) . . ?
C8 N2 C7 112.0(9) . . ?
O1 N3 Fe1 159.8(11) . . ?
S1 C1 H1A 109.9 . . ?
S1 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
C2 C1 S1 108.8(9) . . ?
C2 C1 H1A 109.9 . . ?
C2 C1 H1B 109.9 . . ?
N1 C2 H2A 109.0 . . ?
N1 C2 H2B 109.0 . . ?
C1 C2 N1 112.8(10) . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N1 C3 H3A 109.1 . . ?
N1 C3 H3B 109.1 . . ?
N1 C3 C4 112.4(10) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C3 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
C3 C4 C5 114.8(10) . . ?
H4A C4 H4B 107.5 . . ?
C5 C4 H4A 108.6 . . ?
C5 C4 H4B 108.6 . . ?
N2 C5 C4 112.8(10) . . ?
N2 C5 H5A 109.0 . . ?
N2 C5 H5B 109.0 . . ?
C4 C5 H5A 109.0 . . ?
C4 C5 H5B 109.0 . . ?
H5A C5 H5B 107.8 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 C7 110.8(10) . . ?
H6A C6 H6B 108.1 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
N2 C7 C6 110.1(10) . . ?
N2 C7 H7A 109.6 . . ?
N2 C7 H7B 109.6 . . ?
C6 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.2 . . ?
N2 C8 H8A 109.1 . . ?
N2 C8 H8B 109.1 . . ?
N2 C8 C9 112.3(10) . . ?
H8A C8 H8B 107.9 . . ?
C9 C8 H8A 109.1 . . ?
C9 C8 H8B 109.1 . . ?
S2 C9 H9A 109.7 . . ?
S2 C9 H9B 109.7 . . ?
C8 C9 S2 109.7(8) . . ?
C8 C9 H9A 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
Fe2 Ni2 Fe2 180.0 2_656 . ?
S3 Ni2 Fe2 131.02(9) 2_656 . ?
S3 Ni2 Fe2 48.98(9) 2_656 2_656 ?
S3 Ni2 Fe2 48.98(9) . . ?
S3 Ni2 Fe2 131.02(9) . 2_656 ?
S3 Ni2 S3 180.0 2_656 . ?
S4 Ni2 Fe2 131.37(9) . 2_656 ?
S4 Ni2 Fe2 131.37(9) 2_656 . ?
S4 Ni2 Fe2 48.63(9) 2_656 2_656 ?
S4 Ni2 Fe2 48.63(9) . . ?
S4 Ni2 S3 83.89(11) . . ?
S4 Ni2 S3 96.11(11) . 2_656 ?
S4 Ni2 S3 96.11(11) 2_656 . ?
S4 Ni2 S3 83.89(11) 2_656 2_656 ?
S4 Ni2 S4 180.00(16) 2_656 . ?
S3 Fe2 Ni2 47.96(9) . . ?
S4 Fe2 Ni2 47.90(9) . . ?
S4 Fe2 S3 82.50(13) . . ?
N4 Fe2 Ni2 102.3(3) . . ?
N4 Fe2 S3 87.8(3) . . ?
N4 Fe2 S4 145.1(3) . . ?
N4 Fe2 N5 79.8(4) . . ?
N5 Fe2 Ni2 102.0(3) . . ?
N5 Fe2 S3 144.1(3) . . ?
N5 Fe2 S4 88.7(3) . . ?
N6 Fe2 Ni2 139.2(4) . . ?
N6 Fe2 S3 108.4(4) . . ?
N6 Fe2 S4 104.7(4) . . ?
N6 Fe2 N4 110.1(5) . . ?
N6 Fe2 N5 107.5(5) . . ?
Ni2 S3 Fe2 83.07(11) . . ?
C10 S3 Ni2 109.7(4) . . ?
C10 S3 Fe2 100.2(4) . . ?
Ni2 S4 Fe2 83.46(12) . . ?
C18 S4 Ni2 109.2(4) . . ?
C18 S4 Fe2 99.5(4) . . ?
F2 B1 F1 109.4(12) . . ?
F2 B1 F4 111.4(12) . . ?
F3 B1 F1 107.6(12) . . ?
F3 B1 F2 109.8(13) . . ?
F3 B1 F4 111.5(13) . . ?
F4 B1 F1 107.1(12) . . ?
F5 B2 F6 108.6(13) . . ?
F5 B2 F7 108.1(12) . . ?
F5 B2 F8 112.7(13) . . ?
F6 B2 F7 108.8(12) . . ?
F8 B2 F6 109.6(12) . . ?
F8 B2 F7 109.0(14) . . ?
N1S C2S C3S 179.5(16) . . ?
C2S C3S H3SA 109.5 . . ?
C2S C3S H3SB 109.5 . . ?
C2S C3S H3SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
C11 N4 Fe2 112.3(7) . . ?
C11 N4 C12 107.3(9) . . ?
C11 N4 C15 112.4(10) . . ?
C12 N4 Fe2 112.1(8) . . ?
C15 N4 Fe2 102.4(7) . . ?
C15 N4 C12 110.4(10) . . ?
N4S C5S C6S 179.0(17) . . ?
C5S C6S H6SA 109.5 . . ?
C5S C6S H6SB 109.5 . . ?
C5S C6S H6SC 109.5 . . ?
H6SA C6S H6SB 109.5 . . ?
H6SA C6S H6SC 109.5 . . ?
H6SB C6S H6SC 109.5 . . ?
C14 N5 Fe2 113.0(8) . . ?
C16 N5 Fe2 101.7(7) . . ?
C16 N5 C14 111.1(10) . . ?
C17 N5 Fe2 111.6(8) . . ?
C17 N5 C14 107.1(10) . . ?
C17 N5 C16 112.4(9) . . ?
O2 N6 Fe2 165.5(11) . . ?
S3 C10 H10A 109.8 . . ?
S3 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
C11 C10 S3 109.3(9) . . ?
C11 C10 H10A 109.8 . . ?
C11 C10 H10B 109.8 . . ?
N4 C11 C10 112.4(10) . . ?
N4 C11 H11A 109.1 . . ?
N4 C11 H11B 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
N4 C12 H12A 109.0 . . ?
N4 C12 H12B 109.0 . . ?
N4 C12 C13 112.7(10) . . ?
H12A C12 H12B 107.8 . . ?
C13 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C12 C13 H13A 108.4 . . ?
C12 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
C14 C13 C12 115.3(11) . . ?
C14 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
N5 C14 H14A 109.1 . . ?
N5 C14 H14B 109.1 . . ?
C13 C14 N5 112.6(11) . . ?
C13 C14 H14A 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
N4 C15 C16 110.7(10) . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
N5 C16 C15 110.0(10) . . ?
N5 C16 H16A 109.7 . . ?
N5 C16 H16B 109.7 . . ?
C15 C16 H16A 109.7 . . ?
C15 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
N5 C17 H17A 109.0 . . ?
N5 C17 H17B 109.0 . . ?
N5 C17 C18 112.9(10) . . ?
H17A C17 H17B 107.8 . . ?
C18 C17 H17A 109.0 . . ?
C18 C17 H17B 109.0 . . ?
S4 C18 H18A 109.5 . . ?
S4 C18 H18B 109.5 . . ?
C17 C18 S4 110.5(9) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?

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
Ni1 Fe1 N3 O1 -8(3) . . . . ?
Ni1 S1 C1 C2 112.6(8) . . . . ?
Ni1 S2 C9 C8 -111.8(8) . . . . ?
Fe1 S1 C1 C2 26.0(9) . . . . ?
Fe1 S2 C9 C8 -24.9(9) . . . . ?
Fe1 N1 C2 C1 45.3(13) . . . . ?
Fe1 N1 C3 C4 -70.9(12) . . . . ?
Fe1 N1 C6 C7 36.9(11) . . . . ?
Fe1 N2 C5 C4 70.4(12) . . . . ?
Fe1 N2 C7 C6 -38.8(11) . . . . ?
Fe1 N2 C8 C9 -43.6(12) . . . . ?
S1 Fe1 N3 O1 -53(3) . . . . ?
S1 C1 C2 N1 -46.5(13) . . . . ?
S2 Fe1 N3 O1 34(3) . . . . ?
N1 Fe1 N3 O1 -147(3) . . . . ?
N1 C3 C4 C5 50.6(16) . . . . ?
N1 C6 C7 N2 1.4(14) . . . . ?
N2 Fe1 N3 O1 127(3) . . . . ?
N2 C8 C9 S2 44.7(13) . . . . ?
C2 N1 C3 C4 165.8(11) . . . . ?
C2 N1 C6 C7 157.3(10) . . . . ?
C3 N1 C2 C1 168.7(11) . . . . ?
C3 N1 C6 C7 -82.8(13) . . . . ?
C3 C4 C5 N2 -50.8(16) . . . . ?
C5 N2 C7 C6 80.0(13) . . . . ?
C5 N2 C8 C9 -166.7(11) . . . . ?
C6 N1 C2 C1 -69.9(14) . . . . ?
C6 N1 C3 C4 43.4(14) . . . . ?
C7 N2 C5 C4 -43.0(14) . . . . ?
C7 N2 C8 C9 71.3(13) . . . . ?
C8 N2 C5 C4 -165.8(11) . . . . ?
C8 N2 C7 C6 -159.7(10) . . . . ?
Ni2 Fe2 N6 O2 24(4) . . . . ?
Ni2 S3 C10 C11 -109.1(8) . . . . ?
Ni2 S4 C18 C17 107.8(8) . . . . ?
Fe2 S3 C10 C11 -22.9(9) . . . . ?
Fe2 S4 C18 C17 21.5(9) . . . . ?
Fe2 N4 C11 C10 -46.3(12) . . . . ?
Fe2 N4 C12 C13 70.8(12) . . . . ?
Fe2 N4 C15 C16 -37.2(11) . . . . ?
Fe2 N5 C14 C13 -69.2(13) . . . . ?
Fe2 N5 C16 C15 40.4(11) . . . . ?
Fe2 N5 C17 C18 44.8(12) . . . . ?
S3 Fe2 N6 O2 70(4) . . . . ?
S3 C10 C11 N4 44.9(13) . . . . ?
S4 Fe2 N6 O2 -17(4) . . . . ?
N4 Fe2 N6 O2 164(4) . . . . ?
N4 C12 C13 C14 -51.0(16) . . . . ?
N4 C15 C16 N5 -2.3(14) . . . . ?
N5 Fe2 N6 O2 -111(4) . . . . ?
N5 C17 C18 S4 -43.2(13) . . . . ?
C11 N4 C12 C13 -165.5(11) . . . . ?
C11 N4 C15 C16 -157.9(10) . . . . ?
C12 N4 C11 C10 -169.9(11) . . . . ?
C12 N4 C15 C16 82.3(12) . . . . ?
C12 C13 C14 N5 49.8(17) . . . . ?
C14 N5 C16 C15 -80.1(12) . . . . ?
C14 N5 C17 C18 168.9(11) . . . . ?
C15 N4 C11 C10 68.5(13) . . . . ?
C15 N4 C12 C13 -42.7(14) . . . . ?
C16 N5 C14 C13 44.4(15) . . . . ?
C16 N5 C17 C18 -68.8(13) . . . . ?
C17 N5 C14 C13 167.5(11) . . . . ?
C17 N5 C16 C15 159.9(10) . . . . ?

_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id MDB_MQ_221109_dQ_FeNiFe_073122
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.54635
2 0.45365

_vrf_PLAT341_fenife_073122_0m_4  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01833 Ang.  
RESPONSE: Please refer to _refine_special_details  
;
_vrf_PLAT911_fenife_073122_0m_4  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.596        709 Report
RESPONSE: Please refer to _refine_special_details  
;
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_mq_q_feptfe_107b2_0m_4
_database_code_depnum_ccdc_archive 'CCDC 2231569'
loop_
_audit_author_name
_audit_author_address
'Nattamai S. Bhuvanesh'
;Texas A and M University
United States of America
;
_audit_update_record             
;
2022-12-19 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_audit_creation_date             2022-12-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
marcetta@chem.tamu.edu
nbhuv@mail.chem.tamu.edu
_chemical_name_common            ?
_chemical_name_systematic        FePtFe
_chemical_formula_moiety         
'2(C9 H18 Fe N3 O Pt0.5 S2), 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C22 H42 B2 F8 Fe2 N8 O2 Pt S4'
_chemical_formula_weight         1059.28
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   7.9001(10)
_cell_length_b                   11.1920(13)
_cell_length_c                   20.377(2)
_cell_angle_alpha                85.430(3)
_cell_angle_beta                 89.241(3)
_cell_angle_gamma                82.767(2)
_cell_volume                     1781.7(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3588
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      27.495
_cell_measurement_theta_min      2.613
_shelx_estimated_absorpt_T_max   0.314
_shelx_estimated_absorpt_T_min   0.314
_exptl_absorpt_coefficient_mu    5.033
_exptl_absorpt_correction_T_max  0.745830
_exptl_absorpt_correction_T_min  0.466403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0680 before and 0.0296 after correction.
 
For component 2:
 wR2(int) was 0.0707 before and 0.0318 after correction.
 The Ratio of minimum to maximum transmission is 0.63.

Final HKLF 4 output contains 35307 reflections, Rint = 0.0659
 (12785 with I > 3sig(I), Rint = 0.0499)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic brownish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_preparation       'CH3CN and Et2O,Magnetic properties'
_exptl_crystal_recrystallization_method 'vapor diffusion'
_exptl_crystal_size_max          0.117
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.013
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.916
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8623
_diffrn_reflns_point_group_measured_fraction_full 0.916
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.210
_diffrn_reflns_theta_min         1.840
_diffrn_ambient_temperature      120.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'Bruker Quest (PHOTON III)'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7595
_reflns_number_total             8623
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'APEX 3 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_refine_diff_density_max         1.643
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         8623
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0355
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0444P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0806
_refine_special_details          
;Several crystals were tried and found all of them multiply
twinned/cracked. The best data was taken, containing only
twin components, and was used for further analysis. Significant
number of reflections (32611) were in both the domains. Both
the first and the second domains had similar number of 
non-overlapping reflections (1473 and 1492) with similar 
mean(I/sigma) (14.5 and 14.2 respectively). TWINABS as implemented
in APEX4 was used for correcting absorption and systematic errors, 
and also to generate hklf4 (containing non-overlapping reflections)
and hklf5 (containing reflections only from the major component).
While the former was used for structure solution, the latter was 
used for the final least squares refinement. 

A few reflections showed higher than 10 error/esd in the list of 
Bad Reflections. Our effort to omit them resulted in a few more
reflections with the value greater than 10. Since this was continuing
with an increase in wR2, only the first set of Bad Reflections were
omitted.

It should be noted that the completeness was slightly lower (92 percent
at 0.73 ang resolution), as the
SAINT (as implemented in APEX4) rejected significant amount of 
reflections (17829 out of 59413 predicted reflections). 
Several trials were
made to modify the data integration and absorption correction
parameters. These efforts did not improve the completeness or 
final reliability factors.

Our efforts to increase the crystal to detector distance to improve
the data integration did not improve the final results. We have also
tried using Cu-radiation to resolve the overlapping peaks with no
success.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5157(7)
 0.4843(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B)
3.b Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C6S(H6SA,H6SB,H6SC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.500000 0.000000 0.000000 0.01366(8) Uani 1 2 d S . P . .
Fe1 Fe 0.27788(11) 0.09057(8) 0.10876(4) 0.01494(18) Uani 1 1 d . . . . .
S1 S 0.2101(2) 0.00072(14) 0.01865(8) 0.0160(3) Uani 1 1 d . . . . .
S2 S 0.45323(19) 0.18792(13) 0.04200(8) 0.0154(3) Uani 1 1 d . . . . .
O10 O 0.0082(7) 0.2795(5) 0.1057(4) 0.0487(17) Uani 1 1 d . . . . .
N1 N 0.2362(7) -0.0609(5) 0.1631(3) 0.0173(10) Uani 1 1 d . . . . .
N2 N 0.4440(7) 0.0934(5) 0.1822(3) 0.0187(12) Uani 1 1 d . . . . .
N3 N 0.1120(7) 0.1988(5) 0.1184(3) 0.0219(12) Uani 1 1 d . . . . .
C1 C 0.1807(8) -0.1478(6) 0.0583(3) 0.0191(13) Uani 1 1 d . . . . .
H1A H 0.092496 -0.182686 0.034574 0.023 Uiso 1 1 calc R U . . .
H1B H 0.288831 -0.202796 0.056603 0.023 Uiso 1 1 calc R U . . .
C2 C 0.1273(8) -0.1358(6) 0.1284(3) 0.0197(13) Uani 1 1 d . . . . .
H2A H 0.134107 -0.217196 0.151796 0.024 Uiso 1 1 calc R U . . .
H2B H 0.006997 -0.098332 0.129638 0.024 Uiso 1 1 calc R U . . .
C3 C 0.1504(9) -0.0345(6) 0.2269(3) 0.0256(15) Uani 1 1 d . . . . .
H3A H 0.111620 -0.109497 0.247452 0.031 Uiso 1 1 calc R U . . .
H3B H 0.048147 0.025256 0.218105 0.031 Uiso 1 1 calc R U . . .
C4 C 0.2645(10) 0.0143(7) 0.2749(4) 0.0297(16) Uani 1 1 d . . . . .
H4A H 0.351609 -0.052268 0.291581 0.036 Uiso 1 1 calc R U . . .
H4B H 0.194592 0.041119 0.312923 0.036 Uiso 1 1 calc R U . . .
C5 C 0.3551(9) 0.1190(6) 0.2462(3) 0.0245(15) Uani 1 1 d . . . . .
H5A H 0.270562 0.191932 0.238958 0.029 Uiso 1 1 calc R U . . .
H5B H 0.439899 0.136289 0.278326 0.029 Uiso 1 1 calc R U . . .
C6 C 0.4155(9) -0.1239(6) 0.1744(4) 0.0237(16) Uani 1 1 d . . . . .
H6A H 0.453983 -0.167622 0.135407 0.028 Uiso 1 1 calc R U . . .
H6B H 0.416510 -0.183700 0.212904 0.028 Uiso 1 1 calc R U . . .
C7 C 0.5377(9) -0.0319(6) 0.1864(4) 0.0187(15) Uani 1 1 d . . . . .
H7A H 0.590040 -0.051024 0.230421 0.022 Uiso 1 1 calc R U . . .
H7B H 0.630240 -0.036834 0.153078 0.022 Uiso 1 1 calc R U . . .
C8 C 0.5604(9) 0.1870(6) 0.1687(3) 0.0209(15) Uani 1 1 d . . . . .
H8A H 0.657206 0.170571 0.199866 0.025 Uiso 1 1 calc R U . . .
H8B H 0.498215 0.266993 0.176756 0.025 Uiso 1 1 calc R U . . .
C9 C 0.6295(8) 0.1918(6) 0.0994(3) 0.0189(13) Uani 1 1 d . . . . .
H9A H 0.717697 0.122009 0.094388 0.023 Uiso 1 1 calc R U . . .
H9B H 0.682543 0.266830 0.089739 0.023 Uiso 1 1 calc R U . . .
Pt2 Pt 0.000000 0.500000 0.500000 0.01503(9) Uani 1 2 d S . P . .
Fe2 Fe -0.23255(11) 0.55841(8) 0.38557(4) 0.01573(18) Uani 1 1 d . . . . .
S3 S -0.2897(2) 0.49183(14) 0.49061(9) 0.0169(3) Uani 1 1 d . . . . .
S4 S -0.06454(19) 0.67604(14) 0.43181(8) 0.0173(3) Uani 1 1 d . . . . .
O2 O -0.5056(7) 0.7393(5) 0.3507(4) 0.0528(19) Uani 1 1 d . . . . .
N4 N -0.2613(7) 0.3933(5) 0.3588(3) 0.0192(11) Uani 1 1 d . . . . .
N5 N -0.0656(7) 0.5444(5) 0.3102(3) 0.0208(13) Uani 1 1 d . . . . .
N6 N -0.4016(7) 0.6568(5) 0.3590(3) 0.0203(11) Uani 1 1 d . . . . .
C10 C -0.3167(8) 0.3351(6) 0.4773(3) 0.0214(14) Uani 1 1 d . . . . .
H10A H -0.208858 0.282022 0.487539 0.026 Uiso 1 1 calc R U . . .
H10B H -0.406581 0.307781 0.507166 0.026 Uiso 1 1 calc R U . . .
C11 C -0.3658(8) 0.3261(6) 0.4069(3) 0.0228(14) Uani 1 1 d . . . . .
H11A H -0.352454 0.239953 0.397623 0.027 Uiso 1 1 calc R U . . .
H11B H -0.487628 0.358419 0.400950 0.027 Uiso 1 1 calc R U . . .
C12 C -0.3463(9) 0.3985(7) 0.2931(3) 0.0279(16) Uani 1 1 d . . . . .
H12A H -0.450709 0.457594 0.292823 0.034 Uiso 1 1 calc R U . . .
H12B H -0.381365 0.318324 0.286749 0.034 Uiso 1 1 calc R U . . .
C13 C -0.2330(9) 0.4336(7) 0.2367(4) 0.0290(16) Uani 1 1 d . . . . .
H13A H -0.301447 0.445469 0.195844 0.035 Uiso 1 1 calc R U . . .
H13B H -0.141757 0.365829 0.231470 0.035 Uiso 1 1 calc R U . . .
C14 C -0.1514(10) 0.5462(7) 0.2443(3) 0.0296(17) Uani 1 1 d . . . . .
H14A H -0.239743 0.617348 0.239100 0.035 Uiso 1 1 calc R U . . .
H14B H -0.065771 0.554959 0.208860 0.035 Uiso 1 1 calc R U . . .
C15 C -0.0819(9) 0.3338(6) 0.3554(4) 0.0242(15) Uani 1 1 d . . . . .
H15A H -0.076463 0.264909 0.327503 0.029 Uiso 1 1 calc R U . . .
H15B H -0.042538 0.302123 0.400099 0.029 Uiso 1 1 calc R U . . .
C16 C 0.0369(9) 0.4260(7) 0.3261(4) 0.0211(15) Uani 1 1 d . . . . .
H16A H 0.126461 0.434335 0.358353 0.025 Uiso 1 1 calc R U . . .
H16B H 0.093378 0.396541 0.285747 0.025 Uiso 1 1 calc R U . . .
C17 C 0.0428(9) 0.6462(6) 0.3043(4) 0.0243(16) Uani 1 1 d . . . . .
H17A H -0.025002 0.719254 0.283159 0.029 Uiso 1 1 calc R U . . .
H17B H 0.141675 0.624176 0.275383 0.029 Uiso 1 1 calc R U . . .
C18 C 0.1068(8) 0.6751(6) 0.3700(3) 0.0238(15) Uani 1 1 d . . . . .
H18A H 0.148474 0.755153 0.365440 0.029 Uiso 1 1 calc R U . . .
H18B H 0.203357 0.614012 0.384597 0.029 Uiso 1 1 calc R U . . .
F1 F -0.1862(7) -0.1092(4) 0.3153(3) 0.0455(13) Uani 1 1 d . . . . .
F2 F -0.3603(6) 0.0140(5) 0.3764(2) 0.0448(12) Uani 1 1 d . . . . .
F3 F -0.0750(7) -0.0008(6) 0.3894(2) 0.0559(15) Uani 1 1 d . . . . .
F4 F -0.1957(6) 0.0924(4) 0.2959(2) 0.0334(10) Uani 1 1 d . . . . .
B1 B -0.2039(10) -0.0022(7) 0.3451(4) 0.0247(16) Uani 1 1 d . . . . .
F5 F 0.2594(7) 0.4194(4) 0.1908(3) 0.0513(14) Uani 1 1 d . . . . .
F6 F 0.3706(7) 0.5945(5) 0.1866(3) 0.0556(15) Uani 1 1 d . . . . .
F7 F 0.4419(6) 0.4624(4) 0.1090(2) 0.0406(12) Uani 1 1 d . . . . .
F8 F 0.1768(6) 0.5663(4) 0.1114(3) 0.0505(14) Uani 1 1 d . . . . .
B2 B 0.3130(10) 0.5112(7) 0.1493(4) 0.0261(17) Uani 1 1 d . . . . .
N1S N -0.2262(8) 0.7526(6) 0.1071(3) 0.0322(15) Uani 1 1 d . . . . .
C2S C -0.2183(9) 0.6679(7) 0.0803(4) 0.0255(15) Uani 1 1 d . . . . .
C3S C -0.2077(10) 0.5566(7) 0.0456(4) 0.0349(18) Uani 1 1 d . . . . .
H3SA H -0.176582 0.574296 -0.000539 0.052 Uiso 1 1 calc R U . . .
H3SB H -0.318588 0.525799 0.047767 0.052 Uiso 1 1 calc R U . . .
H3SC H -0.120903 0.495635 0.066492 0.052 Uiso 1 1 calc R U . . .
N4S N 0.2775(9) 0.2161(7) 0.4250(4) 0.049(2) Uani 1 1 d . . . . .
C5S C 0.2822(9) 0.1149(8) 0.4410(4) 0.0288(16) Uani 1 1 d . . . . .
C6S C 0.2891(9) -0.0116(7) 0.4610(4) 0.0295(16) Uani 1 1 d . . . . .
H6SA H 0.397672 -0.054211 0.446687 0.044 Uiso 1 1 calc R U . . .
H6SB H 0.194483 -0.044130 0.440822 0.044 Uiso 1 1 calc R U . . .
H6SC H 0.279829 -0.022802 0.509020 0.044 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
Pt1 Fe1 2.9707(9) . ?
Pt1 Fe1 2.9707(9) 2_655 ?
Pt1 S1 2.3156(16) . ?
Pt1 S1 2.3156(16) 2_655 ?
Pt1 S2 2.3185(15) 2_655 ?
Pt1 S2 2.3185(15) . ?
Fe1 S1 2.2638(19) . ?
Fe1 S2 2.2474(18) . ?
Fe1 N1 2.010(5) . ?
Fe1 N2 2.009(6) . ?
Fe1 N3 1.689(5) . ?
S1 C1 1.829(6) . ?
S2 C9 1.837(6) . ?
O10 N3 1.156(7) . ?
N1 C2 1.496(8) . ?
N1 C3 1.491(8) . ?
N1 C6 1.512(8) . ?
N2 C5 1.503(9) . ?
N2 C7 1.498(8) . ?
N2 C8 1.486(9) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.495(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.517(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.523(10) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.532(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.506(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
Pt2 Fe2 2.9678(9) . ?
Pt2 Fe2 2.9677(9) 2_566 ?
Pt2 S3 2.3127(16) 2_566 ?
Pt2 S3 2.3127(16) . ?
Pt2 S4 2.3242(16) 2_566 ?
Pt2 S4 2.3242(16) . ?
Fe2 S3 2.268(2) . ?
Fe2 S4 2.2480(18) . ?
Fe2 N4 2.009(6) . ?
Fe2 N5 2.013(6) . ?
Fe2 N6 1.686(5) . ?
S3 C10 1.835(7) . ?
S4 C18 1.836(7) . ?
O2 N6 1.159(7) . ?
N4 C11 1.493(9) . ?
N4 C12 1.498(8) . ?
N4 C15 1.491(8) . ?
N5 C14 1.511(9) . ?
N5 C16 1.478(9) . ?
N5 C17 1.505(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.505(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.505(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.506(11) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.560(10) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.511(10) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
F1 B1 1.377(9) . ?
F2 B1 1.381(9) . ?
F3 B1 1.372(9) . ?
F4 B1 1.407(9) . ?
F5 B2 1.383(10) . ?
F6 B2 1.372(9) . ?
F7 B2 1.385(9) . ?
F8 B2 1.384(9) . ?
N1S C2S 1.126(10) . ?
C2S C3S 1.474(11) . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?
N4S C5S 1.150(11) . ?
C5S C6S 1.436(11) . ?
C6S H6SA 0.9800 . ?
C6S H6SB 0.9800 . ?
C6S H6SC 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
Fe1 Pt1 Fe1 180.0 2_655 . ?
S1 Pt1 Fe1 48.80(4) 2_655 2_655 ?
S1 Pt1 Fe1 131.20(4) 2_655 . ?
S1 Pt1 Fe1 48.80(4) . . ?
S1 Pt1 Fe1 131.20(4) . 2_655 ?
S1 Pt1 S1 180.0 2_655 . ?
S1 Pt1 S2 83.39(5) . . ?
S1 Pt1 S2 96.61(5) 2_655 . ?
S1 Pt1 S2 83.39(5) 2_655 2_655 ?
S1 Pt1 S2 96.61(5) . 2_655 ?
S2 Pt1 Fe1 131.62(4) 2_655 . ?
S2 Pt1 Fe1 131.62(4) . 2_655 ?
S2 Pt1 Fe1 48.38(4) . . ?
S2 Pt1 Fe1 48.38(4) 2_655 2_655 ?
S2 Pt1 S2 180.00(7) 2_655 . ?
S1 Fe1 Pt1 50.32(4) . . ?
S2 Fe1 Pt1 50.46(4) . . ?
S2 Fe1 S1 86.20(7) . . ?
N1 Fe1 Pt1 103.58(15) . . ?
N1 Fe1 S1 87.97(16) . . ?
N1 Fe1 S2 148.33(16) . . ?
N2 Fe1 Pt1 102.95(18) . . ?
N2 Fe1 S1 147.12(17) . . ?
N2 Fe1 S2 88.31(18) . . ?
N2 Fe1 N1 80.0(2) . . ?
N3 Fe1 Pt1 137.7(2) . . ?
N3 Fe1 S1 104.4(2) . . ?
N3 Fe1 S2 102.4(2) . . ?
N3 Fe1 N1 109.2(3) . . ?
N3 Fe1 N2 108.4(3) . . ?
Fe1 S1 Pt1 80.88(6) . . ?
C1 S1 Pt1 106.9(2) . . ?
C1 S1 Fe1 98.8(2) . . ?
Fe1 S2 Pt1 81.16(5) . . ?
C9 S2 Pt1 105.7(2) . . ?
C9 S2 Fe1 99.4(2) . . ?
C2 N1 Fe1 112.5(4) . . ?
C2 N1 C6 112.2(5) . . ?
C3 N1 Fe1 112.1(4) . . ?
C3 N1 C2 107.1(5) . . ?
C3 N1 C6 110.9(5) . . ?
C6 N1 Fe1 102.1(4) . . ?
C5 N2 Fe1 112.0(4) . . ?
C7 N2 Fe1 102.9(4) . . ?
C7 N2 C5 110.6(5) . . ?
C8 N2 Fe1 112.5(4) . . ?
C8 N2 C5 106.7(5) . . ?
C8 N2 C7 112.2(5) . . ?
O10 N3 Fe1 160.1(6) . . ?
S1 C1 H1A 109.7 . . ?
S1 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C2 C1 S1 109.7(4) . . ?
C2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
N1 C2 H2A 109.2 . . ?
N1 C2 H2B 109.2 . . ?
C1 C2 N1 112.2(5) . . ?
C1 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N1 C3 H3A 108.9 . . ?
N1 C3 H3B 108.9 . . ?
N1 C3 C4 113.3(6) . . ?
H3A C3 H3B 107.7 . . ?
C4 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
C3 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
C3 C4 C5 114.6(6) . . ?
H4A C4 H4B 107.6 . . ?
C5 C4 H4A 108.6 . . ?
C5 C4 H4B 108.6 . . ?
N2 C5 C4 112.7(6) . . ?
N2 C5 H5A 109.1 . . ?
N2 C5 H5B 109.1 . . ?
C4 C5 H5A 109.1 . . ?
C4 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
N1 C6 H6A 109.6 . . ?
N1 C6 H6B 109.6 . . ?
N1 C6 C7 110.4(6) . . ?
H6A C6 H6B 108.1 . . ?
C7 C6 H6A 109.6 . . ?
C7 C6 H6B 109.6 . . ?
N2 C7 C6 110.4(5) . . ?
N2 C7 H7A 109.6 . . ?
N2 C7 H7B 109.6 . . ?
C6 C7 H7A 109.6 . . ?
C6 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
N2 C8 H8A 108.9 . . ?
N2 C8 H8B 108.9 . . ?
N2 C8 C9 113.3(5) . . ?
H8A C8 H8B 107.7 . . ?
C9 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
S2 C9 H9A 109.9 . . ?
S2 C9 H9B 109.9 . . ?
C8 C9 S2 108.9(4) . . ?
C8 C9 H9A 109.9 . . ?
C8 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
Fe2 Pt2 Fe2 180.0 2_566 . ?
S3 Pt2 Fe2 131.03(5) . 2_566 ?
S3 Pt2 Fe2 131.03(5) 2_566 . ?
S3 Pt2 Fe2 48.97(5) 2_566 2_566 ?
S3 Pt2 Fe2 48.97(5) . . ?
S3 Pt2 S3 180.0 2_566 . ?
S3 Pt2 S4 82.36(6) . . ?
S3 Pt2 S4 82.36(6) 2_566 2_566 ?
S3 Pt2 S4 97.64(6) 2_566 . ?
S3 Pt2 S4 97.64(6) . 2_566 ?
S4 Pt2 Fe2 131.58(4) 2_566 . ?
S4 Pt2 Fe2 48.42(4) . . ?
S4 Pt2 Fe2 131.58(4) . 2_566 ?
S4 Pt2 Fe2 48.42(4) 2_566 2_566 ?
S4 Pt2 S4 180.00(7) . 2_566 ?
S3 Fe2 Pt2 50.28(4) . . ?
S4 Fe2 Pt2 50.66(4) . . ?
S4 Fe2 S3 85.07(7) . . ?
N4 Fe2 Pt2 101.88(15) . . ?
N4 Fe2 S3 88.11(16) . . ?
N4 Fe2 S4 147.39(16) . . ?
N4 Fe2 N5 79.2(2) . . ?
N5 Fe2 Pt2 101.03(18) . . ?
N5 Fe2 S3 145.58(18) . . ?
N5 Fe2 S4 88.64(18) . . ?
N6 Fe2 Pt2 141.1(2) . . ?
N6 Fe2 S3 107.19(19) . . ?
N6 Fe2 S4 103.3(2) . . ?
N6 Fe2 N4 109.2(2) . . ?
N6 Fe2 N5 107.2(3) . . ?
Fe2 S3 Pt2 80.75(6) . . ?
C10 S3 Pt2 107.1(2) . . ?
C10 S3 Fe2 99.1(2) . . ?
Fe2 S4 Pt2 80.93(5) . . ?
C18 S4 Pt2 105.8(2) . . ?
C18 S4 Fe2 99.5(2) . . ?
C11 N4 Fe2 112.4(4) . . ?
C11 N4 C12 107.0(5) . . ?
C12 N4 Fe2 112.1(4) . . ?
C15 N4 Fe2 102.8(4) . . ?
C15 N4 C11 111.9(5) . . ?
C15 N4 C12 110.6(6) . . ?
C14 N5 Fe2 113.0(4) . . ?
C16 N5 Fe2 103.4(4) . . ?
C16 N5 C14 110.2(6) . . ?
C16 N5 C17 112.1(5) . . ?
C17 N5 Fe2 112.3(4) . . ?
C17 N5 C14 105.9(6) . . ?
O2 N6 Fe2 165.2(6) . . ?
S3 C10 H10A 109.7 . . ?
S3 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C11 C10 S3 110.0(5) . . ?
C11 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
N4 C11 C10 113.0(5) . . ?
N4 C11 H11A 109.0 . . ?
N4 C11 H11B 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N4 C12 H12A 109.0 . . ?
N4 C12 H12B 109.0 . . ?
N4 C12 C13 112.9(6) . . ?
H12A C12 H12B 107.8 . . ?
C13 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C12 C13 H13A 108.6 . . ?
C12 C13 H13B 108.6 . . ?
C12 C13 C14 114.8(6) . . ?
H13A C13 H13B 107.5 . . ?
C14 C13 H13A 108.6 . . ?
C14 C13 H13B 108.6 . . ?
N5 C14 H14A 109.1 . . ?
N5 C14 H14B 109.1 . . ?
C13 C14 N5 112.5(6) . . ?
C13 C14 H14A 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
N4 C15 H15A 109.6 . . ?
N4 C15 H15B 109.6 . . ?
N4 C15 C16 110.2(5) . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
N5 C16 C15 109.4(6) . . ?
N5 C16 H16A 109.8 . . ?
N5 C16 H16B 109.8 . . ?
C15 C16 H16A 109.8 . . ?
C15 C16 H16B 109.8 . . ?
H16A C16 H16B 108.2 . . ?
N5 C17 H17A 109.0 . . ?
N5 C17 H17B 109.0 . . ?
N5 C17 C18 112.7(6) . . ?
H17A C17 H17B 107.8 . . ?
C18 C17 H17A 109.0 . . ?
C18 C17 H17B 109.0 . . ?
S4 C18 H18A 109.6 . . ?
S4 C18 H18B 109.6 . . ?
C17 C18 S4 110.5(5) . . ?
C17 C18 H18A 109.6 . . ?
C17 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
F1 B1 F2 109.9(6) . . ?
F1 B1 F4 108.0(6) . . ?
F2 B1 F4 109.1(6) . . ?
F3 B1 F1 110.8(6) . . ?
F3 B1 F2 110.1(7) . . ?
F3 B1 F4 108.9(6) . . ?
F5 B2 F7 108.9(6) . . ?
F5 B2 F8 109.2(7) . . ?
F6 B2 F5 108.9(7) . . ?
F6 B2 F7 110.6(7) . . ?
F6 B2 F8 109.3(6) . . ?
F8 B2 F7 109.8(7) . . ?
N1S C2S C3S 179.7(9) . . ?
C2S C3S H3SA 109.5 . . ?
C2S C3S H3SB 109.5 . . ?
C2S C3S H3SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
N4S C5S C6S 179.7(9) . . ?
C5S C6S H6SA 109.5 . . ?
C5S C6S H6SB 109.5 . . ?
C5S C6S H6SC 109.5 . . ?
H6SA C6S H6SB 109.5 . . ?
H6SA C6S H6SC 109.5 . . ?
H6SB C6S H6SC 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
Pt1 Fe1 N3 O10 -2.9(17) . . . . ?
Pt1 S1 C1 C2 110.5(4) . . . . ?
Pt1 S2 C9 C8 -109.6(4) . . . . ?
Fe1 S1 C1 C2 27.4(4) . . . . ?
Fe1 S2 C9 C8 -26.3(4) . . . . ?
Fe1 N1 C2 C1 44.9(6) . . . . ?
Fe1 N1 C3 C4 -70.1(6) . . . . ?
Fe1 N1 C6 C7 39.0(6) . . . . ?
Fe1 N2 C5 C4 70.4(6) . . . . ?
Fe1 N2 C7 C6 -37.6(6) . . . . ?
Fe1 N2 C8 C9 -43.7(7) . . . . ?
S1 Fe1 N3 O10 -48.8(16) . . . . ?
S1 C1 C2 N1 -47.6(6) . . . . ?
S2 Fe1 N3 O10 40.5(16) . . . . ?
N1 Fe1 N3 O10 -141.7(15) . . . . ?
N1 C3 C4 C5 49.9(8) . . . . ?
N1 C6 C7 N2 -1.0(8) . . . . ?
N2 Fe1 N3 O10 132.9(15) . . . . ?
N2 C8 C9 S2 46.0(7) . . . . ?
C2 N1 C3 C4 166.0(6) . . . . ?
C2 N1 C6 C7 159.6(6) . . . . ?
C3 N1 C2 C1 168.6(5) . . . . ?
C3 N1 C6 C7 -80.6(7) . . . . ?
C3 C4 C5 N2 -49.8(9) . . . . ?
C5 N2 C7 C6 82.1(7) . . . . ?
C5 N2 C8 C9 -166.9(5) . . . . ?
C6 N1 C2 C1 -69.5(7) . . . . ?
C6 N1 C3 C4 43.3(8) . . . . ?
C7 N2 C5 C4 -43.8(8) . . . . ?
C7 N2 C8 C9 71.8(7) . . . . ?
C8 N2 C5 C4 -166.1(6) . . . . ?
C8 N2 C7 C6 -158.8(6) . . . . ?
Pt2 Fe2 N6 O2 21(2) . . . . ?
Pt2 S3 C10 C11 -106.9(4) . . . . ?
Pt2 S4 C18 C17 106.3(5) . . . . ?
Fe2 S3 C10 C11 -23.9(5) . . . . ?
Fe2 S4 C18 C17 23.1(5) . . . . ?
Fe2 N4 C11 C10 -44.9(6) . . . . ?
Fe2 N4 C12 C13 71.6(7) . . . . ?
Fe2 N4 C15 C16 -38.5(6) . . . . ?
Fe2 N5 C14 C13 -69.6(7) . . . . ?
Fe2 N5 C16 C15 39.0(6) . . . . ?
Fe2 N5 C17 C18 43.4(7) . . . . ?
S3 Fe2 N6 O2 68(2) . . . . ?
S3 C10 C11 N4 45.0(6) . . . . ?
S4 Fe2 N6 O2 -21(2) . . . . ?
N4 Fe2 N6 O2 162(2) . . . . ?
N4 C12 C13 C14 -51.1(9) . . . . ?
N4 C15 C16 N5 -0.3(8) . . . . ?
N5 Fe2 N6 O2 -114(2) . . . . ?
N5 C17 C18 S4 -43.4(7) . . . . ?
C11 N4 C12 C13 -164.7(6) . . . . ?
C11 N4 C15 C16 -159.4(6) . . . . ?
C12 N4 C11 C10 -168.4(6) . . . . ?
C12 N4 C15 C16 81.4(7) . . . . ?
C12 C13 C14 N5 49.8(9) . . . . ?
C14 N5 C16 C15 -82.0(7) . . . . ?
C14 N5 C17 C18 167.2(6) . . . . ?
C15 N4 C11 C10 70.3(7) . . . . ?
C15 N4 C12 C13 -42.6(8) . . . . ?
C16 N5 C14 C13 45.6(8) . . . . ?
C16 N5 C17 C18 -72.6(7) . . . . ?
C17 N5 C14 C13 167.0(6) . . . . ?
C17 N5 C16 C15 160.3(6) . . . . ?

_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder'
_olex2_submission_original_sample_id MDB_MQ_221206_dQ_FePtFe_107B2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.5157(7)
2 0.4843(7)

_vrf_PLAT029_mq_q_feptfe_107b2_0m_4 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.916 Why?  
RESPONSE: Please refer to _refine_special_details
;
_vrf_PLAT911_mq_q_feptfe_107b2_0m_4 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        543 Report
RESPONSE: Please refer to _refine_special_details
;
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_fepdfe_2_0m_4
_database_code_depnum_ccdc_archive 'CCDC 2231568'
loop_
_audit_author_name
_audit_author_address
'Nattamai S. Bhuvanesh'
;Texas A and M University
United States of America
;
_audit_update_record             
;
2022-12-19 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_audit_creation_date             2022-11-10
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
marcetta@chem.tamu.edu
nbhuv@mail.chem.tamu.edu
_chemical_name_common            ?
_chemical_name_systematic        FePdFe
_chemical_formula_moiety         
'2(C9 H18 Fe N3 O Pd0.5 S2), 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C22 H42 B2 F8 Fe2 N8 O2 Pd S4'
_chemical_formula_weight         970.59
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   7.8814(4)
_cell_length_b                   11.2000(5)
_cell_length_c                   20.5038(9)
_cell_angle_alpha                85.3290(10)
_cell_angle_beta                 89.1940(10)
_cell_angle_gamma                82.4020(10)
_cell_volume                     1788.05(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9564
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      30.029
_cell_measurement_theta_min      2.603
_shelx_estimated_absorpt_T_max   0.644
_shelx_estimated_absorpt_T_min   0.644
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0653 before and 0.0411 after correction.
 
For component 2:
 wR2(int) was 0.0598 before and 0.0399 after correction.
 The Ratio of minimum to maximum transmission is 0.88.

Final HKLF 4 output contains 59074 reflections, Rint = 0.0503
 (35158 with I > 3sig(I), Rint = 0.0424)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic greenish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.903
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9317
_diffrn_reflns_point_group_measured_fraction_full 0.903
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.062
_diffrn_reflns_theta_min         1.840
_diffrn_ambient_temperature      110.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type  'Bruker Quest (PHOTON III)'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8521
_reflns_number_total             9317
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'APEX 4 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         9317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0422
_refine_ls_restrained_S_all      1.172
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0414P)²+8.4548P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1219
_refine_special_details          
;Several crystals were tried and found all of them multiply
twinned/cracked. The best data was taken, containing only
twin components, and was used for further analysis. Significant
number of reflections (55611) were in both the domains. Both
the first and the second domains had similar number of 
non-overlapping reflections (2668 and 2554) with similar 
mean(I/sigma) (20.1 and 23.3 respectively). TWINABS as implemented
in APEX4 was used for correcting absorption and systematic errors, 
and also to generate hklf4 (containing non-overlapping reflections)
and hklf5 (containing reflections only from the major component).
While the former was used for structure solution, the latter was 
used for the final least squares refinement. 

A few reflections showed higher than 10 error/esd in the list of 
Bad Reflections. Our effort to omit them resulted in a few more
reflections with the value greater than 10. Since this was continuing
with an increase in wR2, only the first set of Bad Reflections were
omitted.

It should be noted that the completeness was slightly lower (93 percent
at 0.71 ang resolution), as the
SAINT (as implemented in APEX4) rejected significant amount of 
reflections (20853 out of 123597 predicted reflections). 
Several trials were
made to modify the data integration and absorption correction
parameters. These efforts did not improve the completeness or 
final reliability factors.

Our efforts to increase the crystal to detector distance to improve
the data integration nor improve the final results. 

The structure was solved and refined in P-1, with Z=2, and Z'= 2 x 0.5.
Absence of additional symmetry was confirmed by PLATON. Also, we could
not find any smaller unit cell options in CELL_NOW.,Twin
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.4936(10)
 0.5064(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B)
3.b Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C6S(H6SA,H6SB,H6SC)
;
_atom_sites_solution_hydrogens   geom
_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
Pd1 Pd 1.000000 0.500000 1.000000 0.01243(12) Uani 1 2 d S . P . .
Fe1 Fe 0.76551(11) 0.55941(8) 0.88439(4) 0.01334(16) Uani 1 1 d . . . . .
S1 S 0.70997(18) 0.49137(13) 0.98829(7) 0.0147(3) Uani 1 1 d . . . . .
S2 S 0.93516(19) 0.67437(13) 0.93043(7) 0.0157(3) Uani 1 1 d . . . . .
O1 O 0.4926(7) 0.7440(5) 0.8536(4) 0.0454(16) Uani 1 1 d . . . . .
N1 N 0.7348(7) 0.3942(5) 0.8577(3) 0.0177(10) Uani 1 1 d . . . . .
N2 N 0.9335(7) 0.5466(5) 0.8093(2) 0.0169(10) Uani 1 1 d . . . . .
N3 N 0.5948(7) 0.6592(5) 0.8590(3) 0.0205(11) Uani 1 1 d . . . . .
C1 C 0.6825(8) 0.3343(6) 0.9754(3) 0.0198(12) Uani 1 1 d . . . . .
H1A H 0.791377 0.280790 0.984391 0.024 Uiso 1 1 calc R U . . .
H1B H 0.594015 0.306720 1.005661 0.024 Uiso 1 1 calc R U . . .
C2 C 0.6294(8) 0.3285(6) 0.9059(3) 0.0206(12) Uani 1 1 d . . . . .
H2A H 0.639086 0.242731 0.896039 0.025 Uiso 1 1 calc R U . . .
H2B H 0.507798 0.363506 0.900856 0.025 Uiso 1 1 calc R U . . .
C3 C 0.6481(9) 0.4004(7) 0.7921(3) 0.0243(14) Uani 1 1 d . . . . .
H3A H 0.543843 0.460409 0.791649 0.029 Uiso 1 1 calc R U . . .
H3B H 0.612593 0.320719 0.785468 0.029 Uiso 1 1 calc R U . . .
C4 C 0.7656(10) 0.4355(7) 0.7362(3) 0.0288(15) Uani 1 1 d . . . . .
H4A H 0.858270 0.367774 0.731793 0.035 Uiso 1 1 calc R U . . .
H4B H 0.699200 0.446989 0.694985 0.035 Uiso 1 1 calc R U . . .
C5 C 0.8452(9) 0.5485(7) 0.7442(3) 0.0259(14) Uani 1 1 d . . . . .
H5A H 0.754890 0.619029 0.739823 0.031 Uiso 1 1 calc R U . . .
H5B H 0.929468 0.558749 0.708631 0.031 Uiso 1 1 calc R U . . .
C6 C 0.9178(8) 0.3339(6) 0.8549(4) 0.0223(13) Uani 1 1 d . . . . .
H6A H 0.924830 0.265060 0.827154 0.027 Uiso 1 1 calc R U . . .
H6B H 0.956817 0.302176 0.899444 0.027 Uiso 1 1 calc R U . . .
C7 C 1.0350(8) 0.4262(6) 0.8263(3) 0.0199(12) Uani 1 1 d . . . . .
H7A H 1.123774 0.434399 0.858727 0.024 Uiso 1 1 calc R U . . .
H7B H 1.093433 0.396296 0.786574 0.024 Uiso 1 1 calc R U . . .
C8 C 1.0414(9) 0.6464(6) 0.8032(3) 0.0217(13) Uani 1 1 d . . . . .
H8A H 0.973434 0.720029 0.782437 0.026 Uiso 1 1 calc R U . . .
H8B H 1.140095 0.623971 0.774229 0.026 Uiso 1 1 calc R U . . .
C9 C 1.1067(8) 0.6741(6) 0.8684(3) 0.0216(13) Uani 1 1 d . . . . .
H9A H 1.148080 0.754097 0.864065 0.026 Uiso 1 1 calc R U . . .
H9B H 1.204057 0.612642 0.882513 0.026 Uiso 1 1 calc R U . . .
Pd2 Pd 0.500000 0.000000 0.500000 0.01150(12) Uani 1 2 d S . P . .
Fe2 Fe 0.27702(11) 0.09165(7) 0.61035(4) 0.01307(16) Uani 1 1 d . . . . .
S3 S 0.45469(19) 0.18570(13) 0.54410(7) 0.0142(3) Uani 1 1 d . . . . .
S4 S 0.21015(18) 0.00121(13) 0.52170(7) 0.0144(3) Uani 1 1 d . . . . .
O2 O 0.0084(7) 0.2837(5) 0.6045(4) 0.0452(16) Uani 1 1 d . . . . .
N4 N 0.4434(7) 0.0948(4) 0.6839(2) 0.0171(10) Uani 1 1 d . . . . .
N5 N 0.2328(7) -0.0592(5) 0.6653(2) 0.0171(10) Uani 1 1 d . . . . .
N6 N 0.1100(7) 0.2016(4) 0.6189(3) 0.0196(11) Uani 1 1 d . . . . .
C10 C 0.6319(8) 0.1894(6) 0.6012(3) 0.0188(12) Uani 1 1 d . . . . .
H10A H 0.719426 0.118341 0.597085 0.023 Uiso 1 1 calc R U . . .
H10B H 0.686496 0.263332 0.590834 0.023 Uiso 1 1 calc R U . . .
C11 C 0.5611(8) 0.1879(5) 0.6706(3) 0.0178(12) Uani 1 1 d . . . . .
H11A H 0.657420 0.171448 0.701967 0.021 Uiso 1 1 calc R U . . .
H11B H 0.498744 0.268463 0.677724 0.021 Uiso 1 1 calc R U . . .
C12 C 0.3526(9) 0.1206(6) 0.7474(3) 0.0232(13) Uani 1 1 d . . . . .
H12A H 0.268440 0.194227 0.739912 0.028 Uiso 1 1 calc R U . . .
H12B H 0.437206 0.137298 0.779537 0.028 Uiso 1 1 calc R U . . .
C13 C 0.2607(11) 0.0179(7) 0.7759(3) 0.0305(16) Uani 1 1 d . . . . .
H13A H 0.190290 0.045864 0.813408 0.037 Uiso 1 1 calc R U . . .
H13B H 0.347265 -0.049167 0.792888 0.037 Uiso 1 1 calc R U . . .
C14 C 0.1456(9) -0.0308(6) 0.7282(3) 0.0243(14) Uani 1 1 d . . . . .
H14A H 0.105610 -0.104995 0.749018 0.029 Uiso 1 1 calc R U . . .
H14B H 0.043723 0.029712 0.718864 0.029 Uiso 1 1 calc R U . . .
C15 C 0.5365(8) -0.0310(6) 0.6873(3) 0.0209(13) Uani 1 1 d . . . . .
H15A H 0.592153 -0.050465 0.730516 0.025 Uiso 1 1 calc R U . . .
H15B H 0.626874 -0.036535 0.653247 0.025 Uiso 1 1 calc R U . . .
C16 C 0.4115(8) -0.1236(5) 0.6769(3) 0.0199(12) Uani 1 1 d . . . . .
H16A H 0.449345 -0.169410 0.638843 0.024 Uiso 1 1 calc R U . . .
H16B H 0.412155 -0.181642 0.716015 0.024 Uiso 1 1 calc R U . . .
C17 C 0.1237(8) -0.1345(5) 0.6307(3) 0.0178(12) Uani 1 1 d . . . . .
H17A H 0.003210 -0.095970 0.631185 0.021 Uiso 1 1 calc R U . . .
H17B H 0.129149 -0.215243 0.654718 0.021 Uiso 1 1 calc R U . . .
C18 C 0.1795(8) -0.1494(5) 0.5606(3) 0.0167(11) Uani 1 1 d . . . . .
H18A H 0.091248 -0.183691 0.536831 0.020 Uiso 1 1 calc R U . . .
H18B H 0.287921 -0.205121 0.559484 0.020 Uiso 1 1 calc R U . . .
F1 F 0.1747(6) 0.5686(4) 0.6118(3) 0.0456(12) Uani 1 1 d . . . . .
F2 F 0.4413(6) 0.4625(4) 0.6093(2) 0.0383(11) Uani 1 1 d . . . . .
F3 F 0.3702(7) 0.5973(5) 0.6861(3) 0.0499(14) Uani 1 1 d . . . . .
F4 F 0.2591(7) 0.4206(4) 0.6914(3) 0.0475(14) Uani 1 1 d . . . . .
B1 B 0.3129(10) 0.5123(7) 0.6494(4) 0.0250(15) Uani 1 1 d . . . . .
F5 F 0.8119(7) -0.1076(4) 0.8154(2) 0.0389(11) Uani 1 1 d . . . . .
F6 F 0.8020(6) 0.0945(4) 0.7971(2) 0.0294(9) Uani 1 1 d . . . . .
F7 F 0.9241(7) -0.0012(6) 0.8897(2) 0.0522(15) Uani 1 1 d . . . . .
F8 F 0.6361(6) 0.0150(5) 0.8767(2) 0.0386(11) Uani 1 1 d . . . . .
B2 B 0.7933(9) -0.0002(7) 0.8455(4) 0.0212(14) Uani 1 1 d . . . . .
N1S N 0.2731(8) 0.2174(7) 0.9249(4) 0.0406(17) Uani 1 1 d . . . . .
C2S C 0.2809(9) 0.1176(7) 0.9411(4) 0.0295(15) Uani 1 1 d . . . . .
C3S C 0.2890(9) -0.0108(7) 0.9614(4) 0.0286(15) Uani 1 1 d . . . . .
H3SA H 0.386203 -0.055637 0.939841 0.043 Uiso 1 1 calc R U . . .
H3SB H 0.182713 -0.039618 0.949073 0.043 Uiso 1 1 calc R U . . .
H3SC H 0.303378 -0.023371 1.008975 0.043 Uiso 1 1 calc R U . . .
N4S N 0.7688(8) 0.7559(6) 0.6058(3) 0.0319(14) Uani 1 1 d . . . . .
C5S C 0.7781(9) 0.6706(6) 0.5793(3) 0.0231(13) Uani 1 1 d . . . . .
C6S C 0.7898(10) 0.5595(7) 0.5456(4) 0.0311(16) Uani 1 1 d . . . . .
H6SA H 0.801178 0.578830 0.498434 0.047 Uiso 1 1 calc R U . . .
H6SB H 0.686060 0.521166 0.554378 0.047 Uiso 1 1 calc R U . . .
H6SC H 0.889944 0.503975 0.561557 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
Pd1 Fe1 3.0030(8) . ?
Pd1 Fe1 3.0030(8) 2_767 ?
Pd1 S1 2.3173(14) . ?
Pd1 S1 2.3173(14) 2_767 ?
Pd1 S2 2.3266(15) 2_767 ?
Pd1 S2 2.3265(15) . ?
Fe1 S1 2.2602(17) . ?
Fe1 S2 2.2416(17) . ?
Fe1 N1 2.017(5) . ?
Fe1 N2 2.018(5) . ?
Fe1 N3 1.691(5) . ?
S1 C1 1.841(6) . ?
S2 C9 1.843(7) . ?
O1 N3 1.160(7) . ?
N1 C2 1.492(8) . ?
N1 C3 1.511(8) . ?
N1 C6 1.513(8) . ?
N2 C5 1.512(8) . ?
N2 C7 1.492(8) . ?
N2 C8 1.488(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.500(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.523(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.506(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.551(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.510(9) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
Pd2 Fe2 3.0084(8) 2_656 ?
Pd2 Fe2 3.0084(8) . ?
Pd2 S3 2.3177(14) 2_656 ?
Pd2 S3 2.3177(14) . ?
Pd2 S4 2.3197(14) 2_656 ?
Pd2 S4 2.3197(14) . ?
Fe2 S3 2.2403(17) . ?
Fe2 S4 2.2528(17) . ?
Fe2 N4 2.017(5) . ?
Fe2 N5 2.020(5) . ?
Fe2 N6 1.697(5) . ?
S3 C10 1.842(6) . ?
S4 C18 1.851(6) . ?
O2 N6 1.159(7) . ?
N4 C11 1.491(8) . ?
N4 C12 1.508(8) . ?
N4 C15 1.497(8) . ?
N5 C14 1.490(8) . ?
N5 C16 1.508(8) . ?
N5 C17 1.503(8) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.520(9) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.513(10) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.523(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.549(9) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.513(9) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
F1 B1 1.393(9) . ?
F2 B1 1.382(9) . ?
F3 B1 1.384(9) . ?
F4 B1 1.392(9) . ?
F5 B2 1.386(9) . ?
F6 B2 1.400(8) . ?
F7 B2 1.380(8) . ?
F8 B2 1.383(9) . ?
N1S C2S 1.134(10) . ?
C2S C3S 1.458(11) . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?
N4S C5S 1.131(9) . ?
C5S C6S 1.463(10) . ?
C6S H6SA 0.9800 . ?
C6S H6SB 0.9800 . ?
C6S H6SC 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
Fe1 Pd1 Fe1 180.0 2_767 . ?
S1 Pd1 Fe1 131.82(4) . 2_767 ?
S1 Pd1 Fe1 48.18(4) . . ?
S1 Pd1 Fe1 131.82(4) 2_767 . ?
S1 Pd1 Fe1 48.18(4) 2_767 2_767 ?
S1 Pd1 S1 180.0 . 2_767 ?
S1 Pd1 S2 81.91(5) 2_767 2_767 ?
S1 Pd1 S2 81.91(5) . . ?
S1 Pd1 S2 98.09(5) . 2_767 ?
S1 Pd1 S2 98.09(5) 2_767 . ?
S2 Pd1 Fe1 47.69(4) 2_767 2_767 ?
S2 Pd1 Fe1 132.31(4) 2_767 . ?
S2 Pd1 Fe1 132.31(4) . 2_767 ?
S2 Pd1 Fe1 47.69(4) . . ?
S2 Pd1 S2 180.0 . 2_767 ?
S1 Fe1 Pd1 49.83(4) . . ?
S2 Fe1 Pd1 50.13(4) . . ?
S2 Fe1 S1 85.09(6) . . ?
N1 Fe1 Pd1 102.32(15) . . ?
N1 Fe1 S1 87.58(16) . . ?
N1 Fe1 S2 147.27(16) . . ?
N1 Fe1 N2 80.1(2) . . ?
N2 Fe1 Pd1 101.40(15) . . ?
N2 Fe1 S1 145.42(16) . . ?
N2 Fe1 S2 88.10(16) . . ?
N3 Fe1 Pd1 140.0(2) . . ?
N3 Fe1 S1 106.91(19) . . ?
N3 Fe1 S2 103.4(2) . . ?
N3 Fe1 N1 109.3(2) . . ?
N3 Fe1 N2 107.7(2) . . ?
Fe1 S1 Pd1 81.99(5) . . ?
C1 S1 Pd1 107.9(2) . . ?
C1 S1 Fe1 99.7(2) . . ?
Fe1 S2 Pd1 82.18(5) . . ?
C9 S2 Pd1 106.9(2) . . ?
C9 S2 Fe1 99.7(2) . . ?
C2 N1 Fe1 112.2(4) . . ?
C2 N1 C3 107.1(5) . . ?
C2 N1 C6 112.2(5) . . ?
C3 N1 Fe1 112.1(4) . . ?
C3 N1 C6 111.4(5) . . ?
C6 N1 Fe1 101.9(4) . . ?
C5 N2 Fe1 112.1(4) . . ?
C7 N2 Fe1 101.9(4) . . ?
C7 N2 C5 110.6(5) . . ?
C8 N2 Fe1 113.1(4) . . ?
C8 N2 C5 106.5(5) . . ?
C8 N2 C7 112.7(5) . . ?
O1 N3 Fe1 162.7(6) . . ?
S1 C1 H1A 109.9 . . ?
S1 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
C2 C1 S1 108.9(4) . . ?
C2 C1 H1A 109.9 . . ?
C2 C1 H1B 109.9 . . ?
N1 C2 C1 112.9(5) . . ?
N1 C2 H2A 109.0 . . ?
N1 C2 H2B 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N1 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
N1 C3 C4 111.8(6) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
C3 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
C5 C4 C3 114.6(6) . . ?
C5 C4 H4A 108.6 . . ?
C5 C4 H4B 108.6 . . ?
N2 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
C4 C5 N2 113.2(6) . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.8 . . ?
N1 C6 H6A 109.7 . . ?
N1 C6 H6B 109.7 . . ?
N1 C6 C7 109.9(5) . . ?
H6A C6 H6B 108.2 . . ?
C7 C6 H6A 109.7 . . ?
C7 C6 H6B 109.7 . . ?
N2 C7 C6 110.9(5) . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N2 C8 H8A 109.1 . . ?
N2 C8 H8B 109.1 . . ?
N2 C8 C9 112.5(5) . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 H8A 109.1 . . ?
C9 C8 H8B 109.1 . . ?
S2 C9 H9A 109.6 . . ?
S2 C9 H9B 109.6 . . ?
C8 C9 S2 110.3(4) . . ?
C8 C9 H9A 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
Fe2 Pd2 Fe2 180.0 . 2_656 ?
S3 Pd2 Fe2 47.60(4) 2_656 2_656 ?
S3 Pd2 Fe2 132.40(4) 2_656 . ?
S3 Pd2 Fe2 47.60(4) . . ?
S3 Pd2 Fe2 132.40(4) . 2_656 ?
S3 Pd2 S3 180.0 2_656 . ?
S3 Pd2 S4 97.08(5) . 2_656 ?
S3 Pd2 S4 82.92(5) 2_656 2_656 ?
S3 Pd2 S4 97.08(5) 2_656 . ?
S3 Pd2 S4 82.92(5) . . ?
S4 Pd2 Fe2 132.09(4) . 2_656 ?
S4 Pd2 Fe2 47.91(4) 2_656 2_656 ?
S4 Pd2 Fe2 132.09(4) 2_656 . ?
S4 Pd2 Fe2 47.91(4) . . ?
S4 Pd2 S4 180.0 2_656 . ?
S3 Fe2 Pd2 49.82(4) . . ?
S3 Fe2 S4 86.21(6) . . ?
S4 Fe2 Pd2 49.82(4) . . ?
N4 Fe2 Pd2 103.80(16) . . ?
N4 Fe2 S3 88.15(16) . . ?
N4 Fe2 S4 147.17(15) . . ?
N4 Fe2 N5 80.2(2) . . ?
N5 Fe2 Pd2 104.45(15) . . ?
N5 Fe2 S3 148.23(16) . . ?
N5 Fe2 S4 87.87(15) . . ?
N6 Fe2 Pd2 136.5(2) . . ?
N6 Fe2 S3 102.66(18) . . ?
N6 Fe2 S4 104.3(2) . . ?
N6 Fe2 N4 108.4(2) . . ?
N6 Fe2 N5 109.0(2) . . ?
Fe2 S3 Pd2 82.58(5) . . ?
C10 S3 Pd2 106.9(2) . . ?
C10 S3 Fe2 99.8(2) . . ?
Fe2 S4 Pd2 82.27(5) . . ?
C18 S4 Pd2 107.7(2) . . ?
C18 S4 Fe2 99.9(2) . . ?
C11 N4 Fe2 112.9(4) . . ?
C11 N4 C12 107.0(5) . . ?
C11 N4 C15 112.2(5) . . ?
C12 N4 Fe2 111.8(4) . . ?
C15 N4 Fe2 101.9(4) . . ?
C15 N4 C12 111.2(5) . . ?
C14 N5 Fe2 112.0(4) . . ?
C14 N5 C16 111.2(5) . . ?
C14 N5 C17 107.3(5) . . ?
C16 N5 Fe2 102.1(4) . . ?
C17 N5 Fe2 112.6(4) . . ?
C17 N5 C16 111.7(5) . . ?
O2 N6 Fe2 158.6(6) . . ?
S3 C10 H10A 109.9 . . ?
S3 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C11 C10 S3 108.8(4) . . ?
C11 C10 H10A 109.9 . . ?
C11 C10 H10B 109.9 . . ?
N4 C11 C10 112.2(5) . . ?
N4 C11 H11A 109.2 . . ?
N4 C11 H11B 109.2 . . ?
C10 C11 H11A 109.2 . . ?
C10 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
N4 C12 H12A 108.9 . . ?
N4 C12 H12B 108.9 . . ?
N4 C12 C13 113.2(5) . . ?
H12A C12 H12B 107.7 . . ?
C13 C12 H12A 108.9 . . ?
C13 C12 H12B 108.9 . . ?
C12 C13 H13A 108.5 . . ?
C12 C13 H13B 108.5 . . ?
C12 C13 C14 115.0(6) . . ?
H13A C13 H13B 107.5 . . ?
C14 C13 H13A 108.5 . . ?
C14 C13 H13B 108.5 . . ?
N5 C14 C13 113.1(6) . . ?
N5 C14 H14A 109.0 . . ?
N5 C14 H14B 109.0 . . ?
C13 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
N4 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
N4 C15 C16 110.8(5) . . ?
H15A C15 H15B 108.1 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
N5 C16 C15 110.2(5) . . ?
N5 C16 H16A 109.6 . . ?
N5 C16 H16B 109.6 . . ?
C15 C16 H16A 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
N5 C17 H17A 109.1 . . ?
N5 C17 H17B 109.1 . . ?
N5 C17 C18 112.6(5) . . ?
H17A C17 H17B 107.8 . . ?
C18 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
S4 C18 H18A 110.1 . . ?
S4 C18 H18B 110.1 . . ?
C17 C18 S4 108.0(4) . . ?
C17 C18 H18A 110.1 . . ?
C17 C18 H18B 110.1 . . ?
H18A C18 H18B 108.4 . . ?
F2 B1 F1 110.1(6) . . ?
F2 B1 F3 111.2(6) . . ?
F2 B1 F4 108.9(6) . . ?
F3 B1 F1 108.3(6) . . ?
F3 B1 F4 109.1(7) . . ?
F4 B1 F1 109.2(6) . . ?
F5 B2 F6 108.1(6) . . ?
F7 B2 F5 110.0(6) . . ?
F7 B2 F6 109.0(6) . . ?
F7 B2 F8 110.6(6) . . ?
F8 B2 F5 109.5(6) . . ?
F8 B2 F6 109.6(6) . . ?
N1S C2S C3S 179.2(9) . . ?
C2S C3S H3SA 109.5 . . ?
C2S C3S H3SB 109.5 . . ?
C2S C3S H3SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
N4S C5S C6S 179.4(8) . . ?
C5S C6S H6SA 109.5 . . ?
C5S C6S H6SB 109.5 . . ?
C5S C6S H6SC 109.5 . . ?
H6SA C6S H6SB 109.5 . . ?
H6SA C6S H6SC 109.5 . . ?
H6SB C6S H6SC 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
Pd1 Fe1 N3 O1 20(2) . . . . ?
Pd1 S1 C1 C2 -109.5(4) . . . . ?
Pd1 S2 C9 C8 107.4(4) . . . . ?
Fe1 S1 C1 C2 -24.9(4) . . . . ?
Fe1 S2 C9 C8 22.7(5) . . . . ?
Fe1 N1 C2 C1 -46.4(6) . . . . ?
Fe1 N1 C3 C4 71.4(6) . . . . ?
Fe1 N1 C6 C7 -38.4(6) . . . . ?
Fe1 N2 C5 C4 -70.0(6) . . . . ?
Fe1 N2 C7 C6 39.2(6) . . . . ?
Fe1 N2 C8 C9 43.5(6) . . . . ?
S1 Fe1 N3 O1 66.7(18) . . . . ?
S1 C1 C2 N1 46.4(6) . . . . ?
S2 Fe1 N3 O1 -22.2(19) . . . . ?
N1 Fe1 N3 O1 160.1(18) . . . . ?
N1 C3 C4 C5 -52.3(8) . . . . ?
N1 C6 C7 N2 -0.6(7) . . . . ?
N2 Fe1 N3 O1 -114.5(18) . . . . ?
N2 C8 C9 S2 -43.0(7) . . . . ?
C2 N1 C3 C4 -165.1(6) . . . . ?
C2 N1 C6 C7 -158.6(5) . . . . ?
C3 N1 C2 C1 -169.9(5) . . . . ?
C3 N1 C6 C7 81.4(6) . . . . ?
C3 C4 C5 N2 51.9(8) . . . . ?
C5 N2 C7 C6 -80.2(6) . . . . ?
C5 N2 C8 C9 167.1(5) . . . . ?
C6 N1 C2 C1 67.6(6) . . . . ?
C6 N1 C3 C4 -42.1(7) . . . . ?
C7 N2 C5 C4 43.0(7) . . . . ?
C7 N2 C8 C9 -71.4(7) . . . . ?
C8 N2 C5 C4 165.7(6) . . . . ?
C8 N2 C7 C6 160.8(5) . . . . ?
Pd2 Fe2 N6 O2 -4.9(15) . . . . ?
Pd2 S3 C10 C11 -112.0(4) . . . . ?
Pd2 S4 C18 C17 112.7(4) . . . . ?
Fe2 S3 C10 C11 -26.8(4) . . . . ?
Fe2 S4 C18 C17 27.7(4) . . . . ?
Fe2 N4 C11 C10 -44.2(6) . . . . ?
Fe2 N4 C12 C13 69.7(6) . . . . ?
Fe2 N4 C15 C16 -39.3(6) . . . . ?
Fe2 N5 C14 C13 -70.2(6) . . . . ?
Fe2 N5 C16 C15 37.9(6) . . . . ?
Fe2 N5 C17 C18 45.2(6) . . . . ?
S3 Fe2 N6 O2 38.7(14) . . . . ?
S3 C10 C11 N4 46.3(6) . . . . ?
S4 Fe2 N6 O2 -50.6(14) . . . . ?
N4 Fe2 N6 O2 130.9(14) . . . . ?
N4 C12 C13 C14 -49.8(9) . . . . ?
N4 C15 C16 N5 0.9(7) . . . . ?
N5 Fe2 N6 O2 -143.4(13) . . . . ?
N5 C17 C18 S4 -47.5(6) . . . . ?
C11 N4 C12 C13 -166.2(6) . . . . ?
C11 N4 C15 C16 -160.4(5) . . . . ?
C12 N4 C11 C10 -167.6(5) . . . . ?
C12 N4 C15 C16 79.9(7) . . . . ?
C12 C13 C14 N5 50.1(8) . . . . ?
C14 N5 C16 C15 -81.7(6) . . . . ?
C14 N5 C17 C18 168.9(5) . . . . ?
C15 N4 C11 C10 70.3(6) . . . . ?
C15 N4 C12 C13 -43.4(8) . . . . ?
C16 N5 C14 C13 43.3(7) . . . . ?
C16 N5 C17 C18 -68.9(6) . . . . ?
C17 N5 C14 C13 165.8(5) . . . . ?
C17 N5 C16 C15 158.4(5) . . . . ?

_olex2_submission_original_sample_id MDB_MQ_221109_dQ_NOFePdFeNO
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.4936(10)
2 0.5064(10)

_vrf_PLAT029_fepdfe_2_0m_4       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.903 Why?
RESPONSE: Several crystals were tried and found all of them multiply
twinned/cracked. The best data was taken, containing only
twin components, and was used for further analysis. Significant
number of reflections (55611) were in both the domains. Both
the first and the second domains had similar number of 
non-overlapping reflections (2668 and 2554) with similar 
mean(I/sigma) (20.1 and 23.3 respectively). TWINABS as implemented
in APEX4 was used for correcting absorption and systematic errors, 
and also to generate hklf4 (containing non-overlapping reflections)
and hklf5 (containing reflections only from the major component).
While the former was used for structure solution, the latter was 
used for the final least squares refinement. 

A few reflections showed higher than 10 error/esd in the list of 
Bad Reflections. Our effort to omit them resulted in a few more
reflections with the value greater than 10. Since this was continuing
with an increase in wR2, only the first set of Bad Reflections were
omitted.

It should be noted that the completeness was slightly lower (93 percent
at 0.71 ang resolution), as the
SAINT (as implemented in APEX4) rejected significant amount of 
reflections (20853 out of 123597 predicted reflections). 
Several trials were
made to modify the data integration and absorption correction
parameters. These efforts did not improve the completeness or 
final reliability factors.

Our efforts to increase the crystal to detector distance to improve
the data integration nor improve the final results. 
;
_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
