# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_mh5clo4
_database_code_depnum_ccdc_archive 'CCDC 2332656'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_audit_creation_date             2023-08-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
;
Bis[2,6-di{pyrazol-1-yl}pyridine]nickel(II) diperchlorate
;
_chemical_formula_moiety         'C22 H18 N10 Ni, 2(Cl O4)'
_chemical_formula_sum            'C22 H18 Cl2 N10 Ni O8'
_chemical_formula_weight         680.07
_chemical_absolute_configuration ab
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C44  H36  Cl4  N20  Ni2  O16  '
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'
Cl Cl 0.1484 0.1585 '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'
Ni Ni 0.3393 1.1124 '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'

_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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.5069(3)
_cell_length_b                   8.5670(2)
_cell_length_c                   18.8513(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.645(3)
_cell_angle_gamma                90
_cell_volume                     1361.64(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9067
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.4450
_cell_measurement_theta_min      2.2260
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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            blue
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             692
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 0 20 0.0706
-7 0 -20 0.0706
1 -12 0 0.1353
-1 12 0 0.1353
10 1 -18 0.1136
-10 -1 18 0.1136
0 11 9 0.1199
0 -11 -9 0.1199
0 0 -26 0.0694
0 0 26 0.0694

_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.14
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
6.6696 0.4741 19.9019 0.8261 0.4332 -0.3604
-6.6696 -0.4741 -19.9019 -0.8261 -0.4332 0.3604
0.5128 -12.0654 -0.4107 0.3038 0.1487 0.9411
-0.5128 12.0654 0.4107 -0.3038 -0.1487 -0.9411
9.9690 0.6223 -17.5248 0.4615 -0.8869 -0.0198
-9.9690 -0.6223 17.5248 -0.4615 0.8869 0.0198
0.3468 11.2765 9.2903 -0.0746 0.1248 -0.9894
-0.3468 -11.2765 -9.2903 0.0746 -0.1248 0.9894
0.0223 -0.0050 -26.3434 -0.4302 -0.8564 0.2855
-0.0223 0.0050 26.3434 0.4302 0.8564 -0.2855

_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15835
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.749
_diffrn_reflns_theta_min         2.180
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -65.00   3.00   1.00    4.00    --    9.61 -25.00 131.00   68
  2  ω    -16.00  82.00   1.00    4.00    --    9.61  25.00 -64.00   98
  3  ω     -3.00  46.00   1.00    4.00    --    9.61 -99.00  90.00   49
  4  ω    -41.00  20.00   1.00    4.00    --   -9.92 -77.00  30.00   61
  5  ω    -35.00  19.00   1.00    4.00    --   -9.92 -77.00 120.00   54
  6  ω    -11.00  15.00   1.00    4.00    --   -9.92  77.00 -60.00   26
  7  ω    -30.00  -1.00   1.00    4.00    --   -9.92  77.00 -30.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0765238000
_diffrn_orient_matrix_UB_12      -0.0224817000
_diffrn_orient_matrix_UB_13      0.0163992000
_diffrn_orient_matrix_UB_21      -0.0309395000
_diffrn_orient_matrix_UB_22      -0.0147471000
_diffrn_orient_matrix_UB_23      0.0324864000
_diffrn_orient_matrix_UB_31      -0.0161423000
_diffrn_orient_matrix_UB_32      -0.0783148000
_diffrn_orient_matrix_UB_33      -0.0108346000
_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         0.827
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.831
_reflns_number_gt                6197
_reflns_number_total             6658
_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 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-TL (Sheldrick, 2015)'
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 
;
 Flack x determined using 2507 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         6658
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0351
_refine_ls_restrained_S_all      1.050
_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)+(0.0215P)²+0.4088P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0686
_refine_special_details          
;
 One ClO₄⁻ ion is disordered over two orientations, with a refined
 occupancy ratio of 0.71:0.29. This was treated using the refined 
 distance restraints listed below. All non-H atoms except the minor 
 anion disorder site were refined anisotropically, and H atoms were 
 placed in calculated positions and refined using a riding model.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Cl3A-O40A
 1.44286 with sigma of 0.02
 Cl3A-O41A
 1.44286 with sigma of 0.02
 Cl3A-O42A
 1.44286 with sigma of 0.02
 Cl3A-O43A
 1.44286 with sigma of 0.02
 O40A-O41A
 2.35619 with sigma of 0.02
 O40A-O42A
 2.35619 with sigma of 0.02
 O40A-O43A
 2.35619 with sigma of 0.02
 O41A-O42A
 2.35619 with sigma of 0.02
 O41A-O43A
 2.35619 with sigma of 0.02
 O42A-O43A
 2.35619 with sigma of 0.02
 Cl3B-O40B
 1.44286 with sigma of 0.02
 Cl3B-O41B
 1.44286 with sigma of 0.02
 Cl3B-O42B
 1.44286 with sigma of 0.02
 Cl3B-O43B
 1.44286 with sigma of 0.02
 O40B-O41B
 2.35619 with sigma of 0.02
 O40B-O42B
 2.35619 with sigma of 0.02
 O40B-O43B
 2.35619 with sigma of 0.02
 O41B-O42B
 2.35619 with sigma of 0.02
 O41B-O43B
 2.35619 with sigma of 0.02
 O42B-O43B
 2.35619 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=
 1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl3A(0.71) O40A(0.71) O41A(0.71) O42A(0.71) O43A(0.71) Cl3B(0.29)
 O40B(0.29) O41B(0.29) O42B(0.29) O43B(0.29)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.22055(5) 0.24520(4) 0.24674(2) 0.01264(10) Uani 1 1 d . . . . .
N2 N 0.2142(3) 0.2294(3) 0.14005(14) 0.0126(5) Uani 1 1 d . . . . .
C3 C 0.0878(4) 0.1714(4) 0.09974(19) 0.0144(7) Uani 1 1 d . . . . .
C4 C 0.0765(4) 0.1582(4) 0.02634(19) 0.0163(7) Uani 1 1 d . . . . .
H4 H -0.015311 0.116772 -0.001510 0.020 Uiso 1 1 calc R U . . .
C5 C 0.2080(4) 0.2094(4) -0.0049(2) 0.0194(8) Uani 1 1 d . . . . .
H5 H 0.206021 0.201831 -0.055332 0.023 Uiso 1 1 calc R U . . .
C6 C 0.3402(4) 0.2705(4) 0.03611(18) 0.0180(7) Uani 1 1 d . . . . .
H6 H 0.429647 0.304591 0.015076 0.022 Uiso 1 1 calc R U . . .
C7 C 0.3368(4) 0.2799(3) 0.10891(18) 0.0145(7) Uani 1 1 d . . . . .
N8 N -0.0327(3) 0.1278(3) 0.14066(16) 0.0138(6) Uani 1 1 d . . . . .
N9 N -0.0070(3) 0.1500(3) 0.21302(16) 0.0138(6) Uani 1 1 d . . . . .
C10 C -0.1390(4) 0.1032(4) 0.2365(2) 0.0168(7) Uani 1 1 d . . . . .
H10 H -0.156413 0.106362 0.285207 0.020 Uiso 1 1 calc R U . . .
C11 C -0.2495(4) 0.0484(4) 0.1805(2) 0.0192(8) Uani 1 1 d . . . . .
H11 H -0.352079 0.007602 0.183932 0.023 Uiso 1 1 calc R U . . .
C12 C -0.1792(4) 0.0656(4) 0.1199(2) 0.0175(7) Uani 1 1 d . . . . .
H12 H -0.223706 0.039449 0.072459 0.021 Uiso 1 1 calc R U . . .
N13 N 0.4586(3) 0.3429(3) 0.15831(15) 0.0142(6) Uani 1 1 d . . . . .
N14 N 0.4399(4) 0.3366(3) 0.22943(16) 0.0157(6) Uani 1 1 d . . . . .
C15 C 0.5643(4) 0.4112(4) 0.2630(2) 0.0204(8) Uani 1 1 d . . . . .
H15 H 0.584447 0.425332 0.313410 0.025 Uiso 1 1 calc R U . . .
C16 C 0.6624(5) 0.4667(4) 0.2143(2) 0.0235(8) Uani 1 1 d . . . . .
H16 H 0.758320 0.523879 0.225052 0.028 Uiso 1 1 calc R U . . .
C17 C 0.5923(4) 0.4220(4) 0.1487(2) 0.0193(8) Uani 1 1 d . . . . .
H17 H 0.629683 0.442200 0.104261 0.023 Uiso 1 1 calc R U . . .
N18 N 0.2254(3) 0.2727(3) 0.35257(15) 0.0132(6) Uani 1 1 d . . . . .
C19 C 0.2823(4) 0.1611(4) 0.39827(19) 0.0145(7) Uani 1 1 d . . . . .
C20 C 0.2883(4) 0.1753(4) 0.4711(2) 0.0177(7) Uani 1 1 d . . . . .
H20 H 0.328546 0.093748 0.502591 0.021 Uiso 1 1 calc R U . . .
C21 C 0.2331(4) 0.3140(4) 0.4968(2) 0.0194(8) Uani 1 1 d . . . . .
H21 H 0.234666 0.327750 0.546891 0.023 Uiso 1 1 calc R U . . .
C22 C 0.1757(4) 0.4330(4) 0.45045(19) 0.0168(7) Uani 1 1 d . . . . .
H22 H 0.138900 0.528684 0.467643 0.020 Uiso 1 1 calc R U . . .
C23 C 0.1745(4) 0.4059(4) 0.37891(19) 0.0143(7) Uani 1 1 d . . . . .
N24 N 0.3365(3) 0.0308(3) 0.36264(15) 0.0141(6) Uani 1 1 d . . . . .
N25 N 0.3225(3) 0.0334(3) 0.28945(16) 0.0151(6) Uani 1 1 d . . . . .
C26 C 0.3916(4) -0.0971(4) 0.2714(2) 0.0191(8) Uani 1 1 d . . . . .
H26 H 0.399951 -0.128055 0.223700 0.023 Uiso 1 1 calc R U . . .
C27 C 0.4508(5) -0.1833(4) 0.3328(2) 0.0226(8) Uani 1 1 d . . . . .
H27 H 0.505506 -0.280184 0.334324 0.027 Uiso 1 1 calc R U . . .
C28 C 0.4133(4) -0.0989(4) 0.3896(2) 0.0197(8) Uani 1 1 d . . . . .
H28 H 0.436648 -0.126073 0.438706 0.024 Uiso 1 1 calc R U . . .
N29 N 0.1197(3) 0.5126(3) 0.32388(16) 0.0150(6) Uani 1 1 d . . . . .
N30 N 0.1293(3) 0.4714(3) 0.25481(16) 0.0148(6) Uani 1 1 d . . . . .
C31 C 0.0804(4) 0.5950(4) 0.2163(2) 0.0180(7) Uani 1 1 d . . . . .
H31 H 0.075646 0.601003 0.165757 0.022 Uiso 1 1 calc R U . . .
C32 C 0.0362(4) 0.7161(4) 0.2595(2) 0.0205(8) Uani 1 1 d . . . . .
H32 H -0.003235 0.816069 0.244347 0.025 Uiso 1 1 calc R U . . .
C33 C 0.0618(4) 0.6603(4) 0.3279(2) 0.0197(8) Uani 1 1 d . . . . .
H33 H 0.042986 0.713943 0.370094 0.024 Uiso 1 1 calc R U . . .
Cl34 Cl 0.70158(10) 0.28137(9) -0.06886(5) 0.01779(18) Uani 1 1 d . . . . .
O35 O 0.5458(3) 0.3256(4) -0.10191(16) 0.0376(8) Uani 1 1 d . . . . .
O36 O 0.8184(3) 0.3437(3) -0.10940(14) 0.0240(6) Uani 1 1 d . . . . .
O37 O 0.7148(3) 0.1134(3) -0.06735(15) 0.0264(6) Uani 1 1 d . . . . .
O38 O 0.7286(3) 0.3392(3) 0.00382(14) 0.0256(6) Uani 1 1 d . . . . .
Cl3A Cl 0.2146(4) 0.8060(3) 0.56041(16) 0.0171(5) Uani 0.71 1 d D . P A 1
O40A O 0.1420(10) 0.8229(10) 0.4869(3) 0.0228(15) Uani 0.71 1 d D . P A 1
O41A O 0.1795(5) 0.9439(5) 0.5998(2) 0.0187(8) Uani 0.71 1 d D . P A 1
O42A O 0.3849(5) 0.7945(7) 0.5610(2) 0.0265(10) Uani 0.71 1 d D . P A 1
O43A O 0.1555(6) 0.6693(5) 0.5917(2) 0.0332(10) Uani 0.71 1 d D . P A 1
Cl3B Cl 0.2450(9) 0.7945(10) 0.5675(5) 0.026(2) Uiso 0.29 1 d D . P B 2
O40B O 0.156(3) 0.797(2) 0.4958(9) 0.020(5) Uiso 0.29 1 d D . P B 2
O41B O 0.1674(14) 0.8877(12) 0.6163(6) 0.028(3) Uiso 0.29 1 d D . P B 2
O42B O 0.4006(15) 0.8549(14) 0.5669(8) 0.032(4) Uiso 0.29 1 d D . P B 2
O43B O 0.2503(16) 0.6371(12) 0.5947(7) 0.045(3) Uiso 0.29 1 d D . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 2.009(3) . ?
Ni1 N9 2.119(3) . ?
Ni1 N14 2.089(3) . ?
Ni1 N18 2.004(3) . ?
Ni1 N25 2.123(3) . ?
Ni1 N30 2.101(3) . ?
N2 C3 1.328(4) . ?
N2 C7 1.336(4) . ?
C3 C4 1.379(5) . ?
C3 N8 1.413(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.402(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.381(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(5) . ?
C7 N13 1.405(4) . ?
N8 N9 1.366(4) . ?
N8 C12 1.364(4) . ?
N9 C10 1.323(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.398(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.367(5) . ?
C12 H12 0.9500 . ?
N13 N14 1.372(4) . ?
N13 C17 1.356(4) . ?
N14 C15 1.323(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.405(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.355(5) . ?
C17 H17 0.9500 . ?
N18 C19 1.334(4) . ?
N18 C23 1.340(4) . ?
C19 C20 1.373(5) . ?
C19 N24 1.411(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.389(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.388(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.367(5) . ?
C23 N29 1.414(4) . ?
N24 N25 1.369(4) . ?
N24 C28 1.353(4) . ?
N25 C26 1.328(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.407(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.364(5) . ?
C28 H28 0.9500 . ?
N29 N30 1.362(4) . ?
N29 C33 1.364(4) . ?
N30 C31 1.319(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.401(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.366(5) . ?
C33 H33 0.9500 . ?
Cl34 O35 1.438(3) . ?
Cl34 O36 1.435(3) . ?
Cl34 O37 1.444(3) . ?
Cl34 O38 1.446(3) . ?
Cl3A O40A 1.448(7) . ?
Cl3A O41A 1.448(4) . ?
Cl3A O42A 1.450(5) . ?
Cl3A O43A 1.432(5) . ?
Cl3B O40B 1.460(15) . ?
Cl3B O41B 1.442(13) . ?
Cl3B O42B 1.423(13) . ?
Cl3B O43B 1.441(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N9 76.81(11) . . ?
N2 Ni1 N14 76.97(11) . . ?
N2 Ni1 N25 106.09(11) . . ?
N2 Ni1 N30 100.00(11) . . ?
N9 Ni1 N25 95.49(11) . . ?
N14 Ni1 N9 153.75(11) . . ?
N14 Ni1 N25 92.94(11) . . ?
N14 Ni1 N30 90.68(11) . . ?
N18 Ni1 N2 177.10(12) . . ?
N18 Ni1 N9 103.95(11) . . ?
N18 Ni1 N14 102.18(11) . . ?
N18 Ni1 N25 76.68(11) . . ?
N18 Ni1 N30 77.20(11) . . ?
N30 Ni1 N9 92.59(11) . . ?
N30 Ni1 N25 153.81(11) . . ?
C3 N2 Ni1 120.7(2) . . ?
C3 N2 C7 119.4(3) . . ?
C7 N2 Ni1 120.0(2) . . ?
N2 C3 C4 123.2(3) . . ?
N2 C3 N8 112.2(3) . . ?
C4 C3 N8 124.6(3) . . ?
C3 C4 H4 121.8 . . ?
C3 C4 C5 116.3(3) . . ?
C5 C4 H4 121.8 . . ?
C4 C5 H5 119.4 . . ?
C6 C5 C4 121.2(3) . . ?
C6 C5 H5 119.4 . . ?
C5 C6 H6 121.4 . . ?
C7 C6 C5 117.2(3) . . ?
C7 C6 H6 121.4 . . ?
N2 C7 C6 122.6(3) . . ?
N2 C7 N13 112.5(3) . . ?
C6 C7 N13 124.8(3) . . ?
N9 N8 C3 118.5(3) . . ?
C12 N8 C3 130.4(3) . . ?
C12 N8 N9 111.1(3) . . ?
N8 N9 Ni1 111.8(2) . . ?
C10 N9 Ni1 143.0(3) . . ?
C10 N9 N8 105.2(3) . . ?
N9 C10 H10 124.3 . . ?
N9 C10 C11 111.4(3) . . ?
C11 C10 H10 124.3 . . ?
C10 C11 H11 127.2 . . ?
C12 C11 C10 105.6(3) . . ?
C12 C11 H11 127.2 . . ?
N8 C12 C11 106.7(3) . . ?
N8 C12 H12 126.7 . . ?
C11 C12 H12 126.7 . . ?
N14 N13 C7 117.5(3) . . ?
C17 N13 C7 131.3(3) . . ?
C17 N13 N14 111.1(3) . . ?
N13 N14 Ni1 112.9(2) . . ?
C15 N14 Ni1 141.3(3) . . ?
C15 N14 N13 105.0(3) . . ?
N14 C15 H15 124.5 . . ?
N14 C15 C16 110.9(3) . . ?
C16 C15 H15 124.5 . . ?
C15 C16 H16 127.1 . . ?
C17 C16 C15 105.9(3) . . ?
C17 C16 H16 127.1 . . ?
N13 C17 H17 126.4 . . ?
C16 C17 N13 107.1(3) . . ?
C16 C17 H17 126.4 . . ?
C19 N18 Ni1 121.1(2) . . ?
C19 N18 C23 118.6(3) . . ?
C23 N18 Ni1 120.3(2) . . ?
N18 C19 C20 123.0(3) . . ?
N18 C19 N24 111.9(3) . . ?
C20 C19 N24 125.1(3) . . ?
C19 C20 H20 121.5 . . ?
C19 C20 C21 117.1(3) . . ?
C21 C20 H20 121.5 . . ?
C20 C21 H21 119.5 . . ?
C22 C21 C20 121.1(3) . . ?
C22 C21 H21 119.5 . . ?
C21 C22 H22 121.6 . . ?
C23 C22 C21 116.9(3) . . ?
C23 C22 H22 121.6 . . ?
N18 C23 C22 123.3(3) . . ?
N18 C23 N29 111.7(3) . . ?
C22 C23 N29 124.9(3) . . ?
N25 N24 C19 118.4(3) . . ?
C28 N24 C19 130.0(3) . . ?
C28 N24 N25 111.4(3) . . ?
N24 N25 Ni1 111.9(2) . . ?
C26 N25 Ni1 142.7(3) . . ?
C26 N25 N24 105.1(3) . . ?
N25 C26 H26 124.6 . . ?
N25 C26 C27 110.7(3) . . ?
C27 C26 H26 124.6 . . ?
C26 C27 H27 127.1 . . ?
C28 C27 C26 105.7(3) . . ?
C28 C27 H27 127.1 . . ?
N24 C28 C27 107.0(3) . . ?
N24 C28 H28 126.5 . . ?
C27 C28 H28 126.5 . . ?
N30 N29 C23 118.6(3) . . ?
N30 N29 C33 111.2(3) . . ?
C33 N29 C23 130.1(3) . . ?
N29 N30 Ni1 112.2(2) . . ?
C31 N30 Ni1 142.5(3) . . ?
C31 N30 N29 105.3(3) . . ?
N30 C31 H31 124.3 . . ?
N30 C31 C32 111.4(3) . . ?
C32 C31 H31 124.3 . . ?
C31 C32 H32 127.2 . . ?
C33 C32 C31 105.6(3) . . ?
C33 C32 H32 127.2 . . ?
N29 C33 C32 106.6(3) . . ?
N29 C33 H33 126.7 . . ?
C32 C33 H33 126.7 . . ?
O35 Cl34 O37 109.62(18) . . ?
O35 Cl34 O38 109.98(17) . . ?
O36 Cl34 O35 109.58(17) . . ?
O36 Cl34 O37 108.88(16) . . ?
O36 Cl34 O38 110.05(16) . . ?
O37 Cl34 O38 108.70(16) . . ?
O40A Cl3A O42A 108.2(4) . . ?
O41A Cl3A O40A 108.6(4) . . ?
O41A Cl3A O42A 109.0(3) . . ?
O43A Cl3A O40A 110.3(4) . . ?
O43A Cl3A O41A 110.4(3) . . ?
O43A Cl3A O42A 110.3(4) . . ?
O41B Cl3B O40B 110.9(11) . . ?
O42B Cl3B O40B 110.9(12) . . ?
O42B Cl3B O41B 108.0(9) . . ?
O42B Cl3B O43B 111.0(9) . . ?
O43B Cl3B O40B 109.3(11) . . ?
O43B Cl3B O41B 106.7(9) . . ?

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 N2 C3 C4 179.8(2) . . . . ?
Ni1 N2 C3 N8 0.6(4) . . . . ?
Ni1 N2 C7 C6 179.2(2) . . . . ?
Ni1 N2 C7 N13 -1.0(3) . . . . ?
Ni1 N9 C10 C11 -179.7(3) . . . . ?
Ni1 N14 C15 C16 -168.1(3) . . . . ?
Ni1 N18 C19 C20 179.8(3) . . . . ?
Ni1 N18 C19 N24 0.7(4) . . . . ?
Ni1 N18 C23 C22 -179.5(3) . . . . ?
Ni1 N18 C23 N29 0.8(4) . . . . ?
Ni1 N25 C26 C27 172.2(3) . . . . ?
Ni1 N30 C31 C32 -178.1(3) . . . . ?
N2 C3 C4 C5 0.2(5) . . . . ?
N2 C3 N8 N9 0.4(4) . . . . ?
N2 C3 N8 C12 179.5(3) . . . . ?
N2 C7 N13 N14 3.3(4) . . . . ?
N2 C7 N13 C17 -171.2(3) . . . . ?
C3 N2 C7 C6 -1.9(5) . . . . ?
C3 N2 C7 N13 177.8(3) . . . . ?
C3 C4 C5 C6 -0.5(5) . . . . ?
C3 N8 N9 Ni1 -1.1(3) . . . . ?
C3 N8 N9 C10 178.5(3) . . . . ?
C3 N8 C12 C11 -178.8(3) . . . . ?
C4 C3 N8 N9 -178.7(3) . . . . ?
C4 C3 N8 C12 0.3(5) . . . . ?
C4 C5 C6 C7 -0.4(5) . . . . ?
C5 C6 C7 N2 1.6(5) . . . . ?
C5 C6 C7 N13 -178.1(3) . . . . ?
C6 C7 N13 N14 -176.9(3) . . . . ?
C6 C7 N13 C17 8.6(5) . . . . ?
C7 N2 C3 C4 0.9(5) . . . . ?
C7 N2 C3 N8 -178.2(3) . . . . ?
C7 N13 N14 Ni1 -4.0(3) . . . . ?
C7 N13 N14 C15 -176.2(3) . . . . ?
C7 N13 C17 C16 175.3(3) . . . . ?
N8 C3 C4 C5 179.3(3) . . . . ?
N8 N9 C10 C11 0.9(4) . . . . ?
N9 N8 C12 C11 0.3(4) . . . . ?
N9 C10 C11 C12 -0.8(4) . . . . ?
C10 C11 C12 N8 0.3(4) . . . . ?
C12 N8 N9 Ni1 179.6(2) . . . . ?
C12 N8 N9 C10 -0.8(3) . . . . ?
N13 N14 C15 C16 0.5(4) . . . . ?
N14 N13 C17 C16 0.5(4) . . . . ?
N14 C15 C16 C17 -0.2(4) . . . . ?
C15 C16 C17 N13 -0.2(4) . . . . ?
C17 N13 N14 Ni1 171.6(2) . . . . ?
C17 N13 N14 C15 -0.6(4) . . . . ?
N18 C19 C20 C21 -0.6(5) . . . . ?
N18 C19 N24 N25 -1.0(4) . . . . ?
N18 C19 N24 C28 173.9(3) . . . . ?
N18 C23 N29 N30 -1.9(4) . . . . ?
N18 C23 N29 C33 -178.6(3) . . . . ?
C19 N18 C23 C22 -1.0(5) . . . . ?
C19 N18 C23 N29 179.3(3) . . . . ?
C19 C20 C21 C22 -0.5(5) . . . . ?
C19 N24 N25 Ni1 0.9(3) . . . . ?
C19 N24 N25 C26 176.0(3) . . . . ?
C19 N24 C28 C27 -175.1(3) . . . . ?
C20 C19 N24 N25 179.9(3) . . . . ?
C20 C19 N24 C28 -5.1(6) . . . . ?
C20 C21 C22 C23 0.8(5) . . . . ?
C21 C22 C23 N18 0.0(5) . . . . ?
C21 C22 C23 N29 179.6(3) . . . . ?
C22 C23 N29 N30 178.4(3) . . . . ?
C22 C23 N29 C33 1.7(6) . . . . ?
C23 N18 C19 C20 1.3(5) . . . . ?
C23 N18 C19 N24 -177.8(3) . . . . ?
C23 N29 N30 Ni1 2.1(3) . . . . ?
C23 N29 N30 C31 -176.0(3) . . . . ?
C23 N29 C33 C32 175.8(3) . . . . ?
N24 C19 C20 C21 178.3(3) . . . . ?
N24 N25 C26 C27 -0.3(4) . . . . ?
N25 N24 C28 C27 0.1(4) . . . . ?
N25 C26 C27 C28 0.4(4) . . . . ?
C26 C27 C28 N24 -0.3(4) . . . . ?
C28 N24 N25 Ni1 -175.0(2) . . . . ?
C28 N24 N25 C26 0.1(4) . . . . ?
N29 N30 C31 C32 -1.0(4) . . . . ?
N30 N29 C33 C32 -1.0(4) . . . . ?
N30 C31 C32 C33 0.4(4) . . . . ?
C31 C32 C33 N29 0.4(4) . . . . ?
C33 N29 N30 Ni1 179.4(2) . . . . ?
C33 N29 N30 C31 1.2(4) . . . . ?

_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 1.316
_oxdiff_exptl_absorpt_empirical_full_min 0.796
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
####################################################################### 
# 
# 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_mh87rt
_database_code_depnum_ccdc_archive 'CCDC 2332657'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_audit_creation_date             2023-11-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
; 
Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) diperchlorate
;
_chemical_formula_moiety         'C22 H18 Fe N10, 2(Cl O4)'
_chemical_formula_sum            'C22 H18 Cl2 Fe N10 O8'
_chemical_formula_weight         677.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H18 Cl2 Fe1 N10 O8'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.5206(2)
_cell_length_b                   9.3323(1)
_cell_length_c                   20.1872(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.014(1)
_cell_angle_gamma                90
_cell_volume                     2701.80(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7619
_cell_measurement_temperature    300(1)
_cell_measurement_theta_max      72.73
_cell_measurement_theta_min      2.19
_exptl_absorpt_coefficient_mu    6.904
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.194
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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            yellow
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
5 5 3 0.0734
-5 -5 -3 0.0734
3 -5 4 0.0709
-3 5 -4 0.0709
-2 -6 0 0.0495
2 6 0 0.0495
6 3 6 0.0823
-6 -3 -6 0.0823
-8 0 8 0.1250
8 0 -8 0.1250

_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
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
5.2611 4.5896 3.2363 0.4200 0.0336 -0.9069
-5.2611 -4.5896 -3.2363 -0.4200 -0.0336 0.9069
2.7512 -5.3633 4.0862 -0.9974 -0.0604 -0.0385
-2.7512 5.3633 -4.0862 0.9974 0.0604 0.0385
-2.0460 -5.9087 0.0131 -0.8098 -0.0545 0.5842
2.0460 5.9087 -0.0131 0.8098 0.0545 -0.5842
6.3495 2.6223 6.3797 0.0138 -0.0849 -0.9963
-6.3495 -2.6223 -6.3797 -0.0138 0.0849 0.9963
-8.2601 -0.4852 7.9372 0.0516 -0.9064 0.4192
8.2601 0.4852 -7.9372 -0.0516 0.9064 -0.4192

_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12271
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.883
_diffrn_reflns_theta_min         4.435
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -72.00  31.00   1.00    1.50    --  -38.50  86.00  55.00  103
  2  ω    -10.00  76.00   1.00    1.50    --   42.71 -86.00 -62.00   86
  3  ω    101.00 178.00   1.00    6.00    --  103.10  86.00  55.00   77
  4  ω     28.00 137.00   1.00    6.00    --  103.10 -86.00 -62.00  109
  5  ω    -59.00  33.00   1.00    1.50    --  -38.50  37.00-180.00   92
  6  ω     22.00 114.00   1.00    1.50    --   42.71  37.00 -30.00   92
  7  ω    103.00 174.00   1.00    6.00    --  103.10  77.00  30.00   71
  8  ω    103.00 174.00   1.00    6.00    --  103.10  77.00 120.00   71
  9  ω     35.00 112.00   1.00    6.00    --  103.10-125.00 120.00   77
 10  ω     77.00 172.00   1.00    6.00    --  103.10  61.00   0.00   95
 11  ω     82.00 176.00   1.00    6.00    --  103.10  30.00-150.00   94
 12  ω     82.00 176.00   1.00    6.00    --  103.10  30.00   0.00   94
 13  ω    103.00 174.00   1.00    6.00    --  103.10  77.00-150.00   71
 14  ω     18.00 111.00   1.00    1.50    --   42.71  57.00-150.00   93
 15  ω     18.00 111.00   1.00    1.50    --   42.71  57.00  30.00   93
 16  ω     18.00 111.00   1.00    1.50    --   42.71  57.00 150.00   93
 17  ω      6.00  80.00   1.00    1.50    --   42.71 -99.00-180.00   74
 18  ω     18.00 111.00   1.00    1.50    --   42.71  57.00  90.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0368595000
_diffrn_orient_matrix_UB_12      0.1497652000
_diffrn_orient_matrix_UB_13      -0.0227067000
_diffrn_orient_matrix_UB_21      0.0515949000
_diffrn_orient_matrix_UB_22      -0.0087785000
_diffrn_orient_matrix_UB_23      -0.0610454000
_diffrn_orient_matrix_UB_31      -0.0866525000
_diffrn_orient_matrix_UB_32      -0.0689508000
_diffrn_orient_matrix_UB_33      -0.0415825000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2490
_reflns_number_total             2656
_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 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-TL (Sheldrick, 2015)'
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.00090(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2655
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0428
_refine_ls_restrained_S_all      1.123
_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)+(0.0826P)²+2.2754P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1266
_refine_special_details          
;
 The asymmetric unit contains half a formula unit, with Fe1 lying on the 
 crystallographic C2 axis -x, y, 0.5-z. The unique perchlorate ion is 
 disordered over two half-occupied orientations, which were modelled 
 using the refined distance restraints listed below. All non-H atoms 
 were refined anisotropically, with SHELXL ISOR constraints being applied
 to the partial O atoms. H atoms were placed in calculated positions and 
 refined using a riding model.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O19A-O20A
 2.31708 with sigma of 0.02
 O19A-O21A
 2.31708 with sigma of 0.02
 O19A-O22A
 2.31708 with sigma of 0.02
 O20A-O21A
 2.31708 with sigma of 0.02
 O20A-O22A
 2.31708 with sigma of 0.02
 O21A-O22A
 2.31708 with sigma of 0.02
 Cl1B-O19B
 1.41891 with sigma of 0.02
 Cl1B-O20B
 1.41891 with sigma of 0.02
 Cl1B-O21B
 1.41891 with sigma of 0.02
 Cl1B-O22B
 1.41891 with sigma of 0.02
 O19B-O20B
 2.31708 with sigma of 0.02
 O19B-O21B
 2.31708 with sigma of 0.02
 O19B-O22B
 2.31708 with sigma of 0.02
 O20B-O21B
 2.31708 with sigma of 0.02
 O20B-O22B
 2.31708 with sigma of 0.02
 O21B-O22B
 2.31708 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O19A) \\sim Ueq, Uanis(O20A) \\sim Ueq, Uanis(O21A) \\sim Ueq,
Uanis(O22A) \\sim Ueq, Uanis(O19B) \\sim Ueq, Uanis(O20B) \\sim Ueq,
Uanis(O21B) \\sim Ueq, Uanis(O22B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.004
4. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=
 1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 Fixed Sof: Cl1A(0.5) O19A(0.5) O20A(0.5) O21A(0.5) O22A(0.5) Cl1B(0.5)
 O19B(0.5) O20B(0.5) O21B(0.5) O22B(0.5)
 Fixed X: Fe1(0)
 Fixed Z: Fe1(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.000000 0.69541(5) 0.250000 0.0367(2) Uani 1 2 d S T P . .
N2 N 0.01402(14) 0.7449(2) 0.35594(9) 0.0377(4) Uani 1 1 d . . . . .
C3 C -0.03019(17) 0.6665(3) 0.39615(11) 0.0396(5) Uani 1 1 d . . . . .
C4 C -0.0289(2) 0.6970(3) 0.46310(13) 0.0501(7) Uani 1 1 d . . . . .
H4 H -0.063296 0.643804 0.489561 0.060 Uiso 1 1 calc R U . . .
C5 C 0.0260(2) 0.8105(3) 0.48871(13) 0.0569(8) Uani 1 1 d . . . . .
H5 H 0.029405 0.834001 0.533791 0.068 Uiso 1 1 calc R U . . .
C6 C 0.0761(2) 0.8900(3) 0.44922(14) 0.0535(7) Uani 1 1 d . . . . .
H6 H 0.114311 0.965306 0.466758 0.064 Uiso 1 1 calc R U . . .
C7 C 0.06682(18) 0.8527(3) 0.38255(12) 0.0423(5) Uani 1 1 d . . . . .
N8 N -0.07665(15) 0.5483(2) 0.36367(9) 0.0408(5) Uani 1 1 d . . . . .
N9 N -0.06814(15) 0.5246(2) 0.29812(10) 0.0427(5) Uani 1 1 d . . . . .
C10 C -0.1051(2) 0.3971(3) 0.28394(14) 0.0512(6) Uani 1 1 d . . . . .
H10 H -0.109558 0.353239 0.242201 0.061 Uiso 1 1 calc R U . . .
C11 C -0.1369(2) 0.3359(3) 0.33980(15) 0.0570(7) Uani 1 1 d . . . . .
H11 H -0.165007 0.246945 0.342342 0.068 Uiso 1 1 calc R U . . .
C12 C -0.1177(2) 0.4350(3) 0.38919(14) 0.0511(6) Uani 1 1 d . . . . .
H12 H -0.130411 0.426585 0.432761 0.061 Uiso 1 1 calc R U . . .
N13 N 0.11191(15) 0.9243(2) 0.33520(11) 0.0451(5) Uani 1 1 d . . . . .
N14 N 0.10598(15) 0.8666(2) 0.27246(10) 0.0446(5) Uani 1 1 d . . . . .
C15 C 0.1540(2) 0.9550(3) 0.23968(16) 0.0531(7) Uani 1 1 d . . . . .
H15 H 0.162407 0.942549 0.195314 0.064 Uiso 1 1 calc R U . . .
C16 C 0.1904(2) 1.0696(3) 0.28020(18) 0.0615(8) Uani 1 1 d . . . . .
H16 H 0.226127 1.145358 0.268341 0.074 Uiso 1 1 calc R U . . .
C17 C 0.1625(2) 1.0467(3) 0.34067(17) 0.0572(7) Uani 1 1 d . . . . .
H17 H 0.175795 1.104320 0.378561 0.069 Uiso 1 1 calc R U . . .
Cl1A Cl 0.2891(6) 0.9586(9) 0.0846(4) 0.075(2) Uani 0.5 1 d . . P A 1
O19A O 0.2313(4) 0.8436(7) 0.1009(3) 0.0821(16) Uani 0.5 1 d D U P A 1
O20A O 0.3863(4) 0.8993(9) 0.1046(4) 0.0766(18) Uani 0.5 1 d D U P A 1
O21A O 0.2765(7) 1.0784(10) 0.1193(5) 0.124(3) Uani 0.5 1 d D U P A 1
O22A O 0.2800(5) 0.9723(8) 0.0153(3) 0.096(2) Uani 0.5 1 d D U P A 1
Cl1B Cl 0.2952(5) 0.9642(7) 0.0890(3) 0.0486(12) Uani 0.5 1 d D . P B 2
O19B O 0.2018(5) 0.9191(9) 0.0822(4) 0.106(2) Uani 0.5 1 d D U P B 2
O20B O 0.3613(6) 0.8605(10) 0.1042(6) 0.110(3) Uani 0.5 1 d D U P B 2
O21B O 0.3058(4) 1.0695(6) 0.1444(3) 0.0654(13) Uani 0.5 1 d D U P B 2
O22B O 0.3060(5) 1.0461(7) 0.0300(3) 0.0835(17) Uani 0.5 1 d D U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.1662(19) . ?
Fe1 N9 2.183(2) . ?
Fe1 N14 2.215(2) . ?
N2 C3 1.330(3) . ?
N2 C7 1.327(3) . ?
C3 C4 1.378(3) . ?
C3 N8 1.401(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.377(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.377(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.376(4) . ?
C7 N13 1.409(3) . ?
N8 N9 1.366(3) . ?
N8 C12 1.355(3) . ?
N9 C10 1.317(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.405(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.356(4) . ?
C12 H12 0.9300 . ?
N13 N14 1.366(3) . ?
N13 C17 1.354(3) . ?
N14 C15 1.322(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.399(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.362(5) . ?
C17 H17 0.9300 . ?
Cl1A O19A 1.432(9) . ?
Cl1A O20A 1.512(11) . ?
Cl1A O21A 1.347(12) . ?
Cl1A O22A 1.390(10) . ?
Cl1B O19B 1.405(8) . ?
Cl1B O20B 1.363(11) . ?
Cl1B O21B 1.479(9) . ?
Cl1B O22B 1.444(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 155.38(11) . 2 ?
N2 Fe1 N9 128.03(8) 2 . ?
N2 Fe1 N9 72.27(8) . . ?
N2 Fe1 N14 90.18(8) . 2 ?
N2 Fe1 N14 71.90(8) . . ?
N9 Fe1 N9 86.17(11) 2 . ?
N9 Fe1 N14 141.66(8) . . ?
N9 Fe1 N14 105.61(8) . 2 ?
N14 Fe1 N14 87.70(12) . 2 ?
C3 N2 Fe1 120.36(17) . . ?
C7 N2 Fe1 121.36(16) . . ?
C7 N2 C3 118.3(2) . . ?
N2 C3 C4 123.4(3) . . ?
N2 C3 N8 113.0(2) . . ?
C4 C3 N8 123.6(2) . . ?
C3 C4 H4 121.8 . . ?
C5 C4 C3 116.4(3) . . ?
C5 C4 H4 121.8 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.6(2) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 H6 121.6 . . ?
C7 C6 C5 116.7(3) . . ?
C7 C6 H6 121.6 . . ?
N2 C7 C6 123.3(3) . . ?
N2 C7 N13 112.7(2) . . ?
C6 C7 N13 124.0(3) . . ?
N9 N8 C3 118.09(19) . . ?
C12 N8 C3 130.2(2) . . ?
C12 N8 N9 110.7(2) . . ?
N8 N9 Fe1 115.38(15) . . ?
C10 N9 Fe1 139.47(17) . . ?
C10 N9 N8 105.1(2) . . ?
N9 C10 H10 124.2 . . ?
N9 C10 C11 111.5(3) . . ?
C11 C10 H10 124.2 . . ?
C10 C11 H11 127.6 . . ?
C12 C11 C10 104.9(3) . . ?
C12 C11 H11 127.6 . . ?
N8 C12 C11 107.7(2) . . ?
N8 C12 H12 126.1 . . ?
C11 C12 H12 126.1 . . ?
N14 N13 C7 118.3(2) . . ?
C17 N13 C7 130.5(2) . . ?
C17 N13 N14 111.3(2) . . ?
N13 N14 Fe1 114.50(15) . . ?
C15 N14 Fe1 138.7(2) . . ?
C15 N14 N13 104.9(2) . . ?
N14 C15 H15 124.3 . . ?
N14 C15 C16 111.4(3) . . ?
C16 C15 H15 124.3 . . ?
C15 C16 H16 127.3 . . ?
C17 C16 C15 105.4(3) . . ?
C17 C16 H16 127.3 . . ?
N13 C17 C16 107.0(3) . . ?
N13 C17 H17 126.5 . . ?
C16 C17 H17 126.5 . . ?
O19A Cl1A O20A 102.7(7) . . ?
O21A Cl1A O19A 111.8(7) . . ?
O21A Cl1A O20A 111.2(8) . . ?
O21A Cl1A O22A 116.6(8) . . ?
O22A Cl1A O19A 109.5(7) . . ?
O22A Cl1A O20A 103.9(7) . . ?
O19B Cl1B O21B 104.9(6) . . ?
O19B Cl1B O22B 107.8(6) . . ?
O20B Cl1B O19B 116.4(6) . . ?
O20B Cl1B O21B 108.4(7) . . ?
O20B Cl1B O22B 113.5(7) . . ?
O22B Cl1B O21B 105.0(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 N2 C3 C4 -176.0(2) . . . . ?
Fe1 N2 C3 N8 5.1(3) . . . . ?
Fe1 N2 C7 C6 178.5(2) . . . . ?
Fe1 N2 C7 N13 -1.5(3) . . . . ?
Fe1 N9 C10 C11 178.2(2) . . . . ?
Fe1 N14 C15 C16 161.8(2) . . . . ?
N2 C3 C4 C5 -3.8(4) . . . . ?
N2 C3 N8 N9 2.8(3) . . . . ?
N2 C3 N8 C12 169.9(2) . . . . ?
N2 C7 N13 N14 -7.8(3) . . . . ?
N2 C7 N13 C17 171.9(3) . . . . ?
C3 N2 C7 C6 -1.9(4) . . . . ?
C3 N2 C7 N13 178.2(2) . . . . ?
C3 C4 C5 C6 0.7(4) . . . . ?
C3 N8 N9 Fe1 -9.0(3) . . . . ?
C3 N8 N9 C10 170.2(2) . . . . ?
C3 N8 C12 C11 -168.3(3) . . . . ?
C4 C3 N8 N9 -176.1(2) . . . . ?
C4 C3 N8 C12 -9.0(4) . . . . ?
C4 C5 C6 C7 1.5(4) . . . . ?
C5 C6 C7 N2 -1.0(4) . . . . ?
C5 C6 C7 N13 179.0(2) . . . . ?
C6 C7 N13 N14 172.3(2) . . . . ?
C6 C7 N13 C17 -8.0(4) . . . . ?
C7 N2 C3 C4 4.4(4) . . . . ?
C7 N2 C3 N8 -174.5(2) . . . . ?
C7 N13 N14 Fe1 12.9(3) . . . . ?
C7 N13 N14 C15 -180.0(2) . . . . ?
C7 N13 C17 C16 -179.8(3) . . . . ?
N8 C3 C4 C5 175.0(2) . . . . ?
N8 N9 C10 C11 -0.7(3) . . . . ?
N9 N8 C12 C11 -0.4(3) . . . . ?
N9 C10 C11 C12 0.5(4) . . . . ?
C10 C11 C12 N8 -0.1(3) . . . . ?
C12 N8 N9 Fe1 -178.57(17) . . . . ?
C12 N8 N9 C10 0.7(3) . . . . ?
N13 N14 C15 C16 -0.4(3) . . . . ?
N14 N13 C17 C16 0.0(3) . . . . ?
N14 C15 C16 C17 0.3(4) . . . . ?
C15 C16 C17 N13 -0.2(3) . . . . ?
C17 N13 N14 Fe1 -166.89(18) . . . . ?
C17 N13 N14 C15 0.2(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
####################################################################### 
# 
# 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_mah35
_database_code_depnum_ccdc_archive 'CCDC 2332658'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-02-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
;
Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) di(hexafluorophosphate)
;
_chemical_formula_moiety         'C22 H18 Fe N10, 2(F6 P)'
_chemical_formula_sum            'C22 H18 F12 Fe N10 P2'
_chemical_formula_weight         768.25
_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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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'

_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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.6500(5)
_cell_length_b                   9.4890(4)
_cell_length_c                   20.6037(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.792(2)
_cell_angle_gamma                90
_cell_volume                     2830.54(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10906
_cell_measurement_temperature    300(2)
_cell_measurement_theta_min      2.81
_cell_measurement_theta_max      27.49
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 Using multiple and symmetry-related data measurements via the program SORTAV
 See R.H. Blessing, Acta Cryst (1995), A51, 33-38 
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            10906
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         2.814
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'Area detector scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2670
_reflns_number_total             3234
_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_data_collection       'COLLECT (Nonius, 1999)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1996)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-TL (Sheldrick, 2015)'
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0052(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3234
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0359
_refine_ls_restrained_S_all      1.023
_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)+(0.0491P)²+1.7095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0998
_refine_special_details          
;
 The asymmetric unit contains half a formula unit, with Fe1 lying on the 
 crystallographic C2 axis -x, y, 0.5-z. The F atoms in the unique PF₆⁻ 
 ion are disordered over two half-occupied orientations, which were 
 modelled using the refined distance restraints listed below. All non-H 
 atoms were refined anisotropically, and H atoms were placed in calculated 
 positions and refined using a riding model.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P18-F19A
 1.58095 with sigma of 0.02
 P18-F20A
 1.58095 with sigma of 0.02
 P18-F21A
 1.58095 with sigma of 0.02
 P18-F22A
 1.58095 with sigma of 0.02
 P18-F23A
 1.58095 with sigma of 0.02
 P18-F24A
 1.58095 with sigma of 0.02
 P18-F19B
 1.58095 with sigma of 0.02
 P18-F20B
 1.58095 with sigma of 0.02
 P18-F21B
 1.58095 with sigma of 0.02
 P18-F22B
 1.58095 with sigma of 0.02
 P18-F23B
 1.58095 with sigma of 0.02
 P18-F24B
 1.58095 with sigma of 0.02
3. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=
 1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 Fixed Sof: F19A(0.5) F20A(0.5) F21A(0.5) F22A(0.5) F23A(0.5) F24A(0.5)
 F19B(0.5) F20B(0.5) F21B(0.5) F22B(0.5) F23B(0.5) F24B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.000000 0.81485(4) 0.250000 0.03816(15) Uani 1 2 d S T P . .
N2 N 0.00985(10) 0.76470(16) 0.35357(7) 0.0379(3) Uani 1 1 d . . . . .
C3 C -0.03550(13) 0.8404(2) 0.39252(9) 0.0411(4) Uani 1 1 d . . . . .
C4 C -0.03742(15) 0.8080(2) 0.45765(10) 0.0524(5) Uani 1 1 d . . . . .
H4 H -0.071992 0.860597 0.483240 0.063 Uiso 1 1 calc R U . . .
C5 C 0.01449(17) 0.6940(2) 0.48277(10) 0.0551(5) Uani 1 1 d . . . . .
H5 H 0.015484 0.669173 0.526543 0.066 Uiso 1 1 calc R U . . .
C6 C 0.06501(15) 0.6158(2) 0.44444(9) 0.0506(5) Uani 1 1 d . . . . .
H6 H 0.101119 0.539860 0.461438 0.061 Uiso 1 1 calc R U . . .
C7 C 0.05929(13) 0.6558(2) 0.37972(9) 0.0412(4) Uani 1 1 d . . . . .
N8 N -0.07897(11) 0.95959(17) 0.36118(7) 0.0441(4) Uani 1 1 d . . . . .
N9 N -0.06937(11) 0.98310(17) 0.29706(8) 0.0454(4) Uani 1 1 d . . . . .
C10 C -0.10421(16) 1.1109(2) 0.28405(11) 0.0556(5) Uani 1 1 d . . . . .
H10 H -0.107244 1.155763 0.243642 0.067 Uiso 1 1 calc R U . . .
C11 C -0.13573(17) 1.1694(2) 0.33870(12) 0.0617(6) Uani 1 1 d . . . . .
H11 H -0.163033 1.257305 0.341388 0.074 Uiso 1 1 calc R U . . .
C12 C -0.11837(15) 1.0721(2) 0.38691(11) 0.0562(5) Uani 1 1 d . . . . .
H12 H -0.131011 1.080446 0.429625 0.067 Uiso 1 1 calc R U . . .
N13 N 0.10646(11) 0.58653(16) 0.33424(8) 0.0437(4) Uani 1 1 d . . . . .
N14 N 0.10301(11) 0.64381(17) 0.27337(8) 0.0445(4) Uani 1 1 d . . . . .
C15 C 0.15144(14) 0.5553(2) 0.24191(11) 0.0524(5) Uani 1 1 d . . . . .
H15 H 0.161046 0.566875 0.198647 0.063 Uiso 1 1 calc R U . . .
C16 C 0.18588(15) 0.4434(2) 0.28185(12) 0.0587(6) Uani 1 1 d . . . . .
H16 H 0.221945 0.369099 0.270818 0.070 Uiso 1 1 calc R U . . .
C17 C 0.15615(15) 0.4649(2) 0.34007(12) 0.0542(5) Uani 1 1 d . . . . .
H17 H 0.167503 0.407495 0.377012 0.065 Uiso 1 1 calc R U . . .
P18 P 0.22136(4) 1.02536(6) 0.41704(3) 0.05205(19) Uani 1 1 d D . . . .
F19A F 0.1848(10) 0.9642(15) 0.3459(6) 0.094(4) Uani 0.5 1 d D . P A 1
F20A F 0.2503(6) 1.0812(17) 0.4905(6) 0.069(2) Uani 0.5 1 d D . P A 1
F21A F 0.3283(7) 0.9873(16) 0.4163(7) 0.067(2) Uani 0.5 1 d D . P A 1
F22A F 0.2144(13) 0.8737(14) 0.4499(9) 0.113(4) Uani 0.5 1 d D . P A 1
F23A F 0.1161(6) 1.0492(11) 0.4203(4) 0.102(3) Uani 0.5 1 d D . P A 1
F24A F 0.2351(11) 1.1685(14) 0.3837(7) 0.089(3) Uani 0.5 1 d D . P A 1
F19B F 0.2513(11) 1.1625(15) 0.3799(8) 0.085(3) Uani 0.5 1 d D . P A 2
F20B F 0.1974(8) 0.9457(12) 0.3484(5) 0.0613(17) Uani 0.5 1 d D . P A 2
F21B F 0.1850(13) 0.9006(14) 0.4525(8) 0.123(5) Uani 0.5 1 d D . P A 2
F22B F 0.1236(6) 1.1051(13) 0.4127(5) 0.128(4) Uani 0.5 1 d D . P A 2
F23B F 0.2533(9) 1.1076(19) 0.4830(6) 0.090(4) Uani 0.5 1 d D . P A 2
F24B F 0.3186(8) 0.9652(16) 0.4159(8) 0.082(3) Uani 0.5 1 d D . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.1695(14) . ?
Fe1 N9 2.1961(16) . ?
Fe1 N14 2.2184(16) . ?
N2 C3 1.328(2) . ?
N2 C7 1.328(2) . ?
C3 C4 1.381(3) . ?
C3 N8 1.406(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.378(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.379(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.376(3) . ?
C7 N13 1.409(2) . ?
N8 N9 1.368(2) . ?
N8 C12 1.359(3) . ?
N9 C10 1.327(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.396(3) . ?
C11 H11 0.9300 . ?
C11 C12 1.352(3) . ?
C12 H12 0.9300 . ?
N13 N14 1.361(2) . ?
N13 C17 1.360(3) . ?
N14 C15 1.330(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.390(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.353(3) . ?
C17 H17 0.9300 . ?
P18 F19A 1.591(10) . ?
P18 F20A 1.598(9) . ?
P18 F21A 1.610(10) . ?
P18 F22A 1.600(11) . ?
P18 F23A 1.570(8) . ?
P18 F24A 1.549(10) . ?
P18 F19B 1.604(10) . ?
P18 F20B 1.595(8) . ?
P18 F21B 1.530(12) . ?
P18 F22B 1.611(9) . ?
P18 F23B 1.575(11) . ?
P18 F24B 1.539(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 154.66(8) 2 . ?
N2 Fe1 N9 128.90(6) . 2 ?
N2 Fe1 N9 71.99(6) . . ?
N2 Fe1 N14 89.64(6) . 2 ?
N2 Fe1 N14 71.66(6) . . ?
N9 Fe1 N9 86.73(9) 2 . ?
N9 Fe1 N14 106.40(6) . 2 ?
N9 Fe1 N14 141.39(6) . . ?
N14 Fe1 N14 85.95(9) . 2 ?
C3 N2 Fe1 120.76(12) . . ?
C7 N2 Fe1 121.32(12) . . ?
C7 N2 C3 117.89(15) . . ?
N2 C3 C4 123.59(18) . . ?
N2 C3 N8 113.00(15) . . ?
C4 C3 N8 123.38(17) . . ?
C3 C4 H4 121.7 . . ?
C5 C4 C3 116.60(19) . . ?
C5 C4 H4 121.7 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.43(18) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 121.7 . . ?
C7 C6 C5 116.62(19) . . ?
C7 C6 H6 121.7 . . ?
N2 C7 C6 123.79(18) . . ?
N2 C7 N13 112.68(15) . . ?
C6 C7 N13 123.52(18) . . ?
N9 N8 C3 117.95(15) . . ?
C12 N8 C3 129.95(17) . . ?
C12 N8 N9 111.18(17) . . ?
N8 N9 Fe1 115.50(11) . . ?
C10 N9 Fe1 139.89(14) . . ?
C10 N9 N8 104.53(16) . . ?
N9 C10 H10 124.3 . . ?
N9 C10 C11 111.4(2) . . ?
C11 C10 H10 124.3 . . ?
C10 C11 H11 127.1 . . ?
C12 C11 C10 105.80(19) . . ?
C12 C11 H11 127.1 . . ?
N8 C12 H12 126.5 . . ?
C11 C12 N8 107.07(19) . . ?
C11 C12 H12 126.5 . . ?
N14 N13 C7 118.29(15) . . ?
C17 N13 C7 130.33(17) . . ?
C17 N13 N14 111.37(16) . . ?
N13 N14 Fe1 114.86(11) . . ?
C15 N14 Fe1 138.76(14) . . ?
C15 N14 N13 104.45(16) . . ?
N14 C15 H15 124.3 . . ?
N14 C15 C16 111.5(2) . . ?
C16 C15 H15 124.3 . . ?
C15 C16 H16 127.1 . . ?
C17 C16 C15 105.83(19) . . ?
C17 C16 H16 127.1 . . ?
N13 C17 H17 126.6 . . ?
C16 C17 N13 106.86(19) . . ?
C16 C17 H17 126.6 . . ?
F19A P18 F20A 175.0(8) . . ?
F19A P18 F21A 95.8(7) . . ?
F19A P18 F22A 91.6(9) . . ?
F20A P18 F21A 88.1(6) . . ?
F20A P18 F22A 85.5(10) . . ?
F22A P18 F21A 85.8(9) . . ?
F23A P18 F19A 84.1(6) . . ?
F23A P18 F20A 91.8(4) . . ?
F23A P18 F21A 175.0(7) . . ?
F23A P18 F22A 89.1(8) . . ?
F24A P18 F19A 87.7(9) . . ?
F24A P18 F20A 95.5(9) . . ?
F24A P18 F21A 89.9(8) . . ?
F24A P18 F22A 175.6(9) . . ?
F24A P18 F23A 95.1(7) . . ?
F19B P18 F22B 84.1(7) . . ?
F20B P18 F19B 90.1(8) . . ?
F20B P18 F22B 95.7(6) . . ?
F21B P18 F19B 175.2(9) . . ?
F21B P18 F20B 90.7(8) . . ?
F21B P18 F22B 91.1(8) . . ?
F21B P18 F23B 92.9(10) . . ?
F21B P18 F24B 96.4(9) . . ?
F23B P18 F19B 86.7(10) . . ?
F23B P18 F20B 175.0(7) . . ?
F23B P18 F22B 87.7(6) . . ?
F24B P18 F19B 88.4(8) . . ?
F24B P18 F20B 83.6(7) . . ?
F24B P18 F22B 172.5(7) . . ?
F24B P18 F23B 92.5(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 175.24(15) . . . . ?
Fe1 N2 C3 N8 -6.7(2) . . . . ?
Fe1 N2 C7 C6 -177.33(15) . . . . ?
Fe1 N2 C7 N13 3.5(2) . . . . ?
Fe1 N9 C10 C11 -176.38(17) . . . . ?
Fe1 N14 C15 C16 -162.60(16) . . . . ?
N2 C3 C4 C5 2.9(3) . . . . ?
N2 C3 N8 N9 -0.4(2) . . . . ?
N2 C3 N8 C12 -168.30(19) . . . . ?
N2 C7 N13 N14 5.6(2) . . . . ?
N2 C7 N13 C17 -172.97(19) . . . . ?
C3 N2 C7 C6 1.0(3) . . . . ?
C3 N2 C7 N13 -178.11(16) . . . . ?
C3 C4 C5 C6 -0.5(3) . . . . ?
C3 N8 N9 Fe1 6.9(2) . . . . ?
C3 N8 N9 C10 -170.61(17) . . . . ?
C3 N8 C12 C11 169.3(2) . . . . ?
C4 C3 N8 N9 177.68(18) . . . . ?
C4 C3 N8 C12 9.8(3) . . . . ?
C4 C5 C6 C7 -1.3(3) . . . . ?
C5 C6 C7 N2 1.1(3) . . . . ?
C5 C6 C7 N13 -179.83(18) . . . . ?
C6 C7 N13 N14 -173.52(18) . . . . ?
C6 C7 N13 C17 7.9(3) . . . . ?
C7 N2 C3 C4 -3.1(3) . . . . ?
C7 N2 C3 N8 174.94(16) . . . . ?
C7 N13 N14 Fe1 -11.6(2) . . . . ?
C7 N13 N14 C15 -178.87(17) . . . . ?
C7 N13 C17 C16 179.00(19) . . . . ?
N8 C3 C4 C5 -174.99(18) . . . . ?
N8 N9 C10 C11 0.1(2) . . . . ?
N9 N8 C12 C11 0.8(2) . . . . ?
N9 C10 C11 C12 0.4(3) . . . . ?
C10 C11 C12 N8 -0.7(3) . . . . ?
C12 N8 N9 Fe1 176.97(13) . . . . ?
C12 N8 N9 C10 -0.5(2) . . . . ?
N13 N14 C15 C16 -0.3(2) . . . . ?
N14 N13 C17 C16 0.3(2) . . . . ?
N14 C15 C16 C17 0.5(3) . . . . ?
C15 C16 C17 N13 -0.5(2) . . . . ?
C17 N13 N14 Fe1 167.22(13) . . . . ?
C17 N13 N14 C15 0.0(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: nitromethane/diethyl ether'
####################################################################### 
# 
# 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_mh722rt
_database_code_depnum_ccdc_archive 'CCDC 2332659'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-02-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-nickel(II) ditetrafluoroborate 0.50:0.50 solid solution'
_chemical_formula_moiety         'C22 H18 Fe0.5 N10 Ni0.5, 2(Cl O4)'
_chemical_formula_sum            'C22 H18 Cl2 Fe0.50 N10 Ni0.50 O8'
_chemical_formula_weight         678.64
_chemical_absolute_configuration ab
_chemical_melting_point          ?
_chemical_oxdiff_formula         C22H18Cl2Fe0.5N10Ni0.5O8
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.5567(7)
_cell_length_b                   8.6233(6)
_cell_length_c                   19.2053(15)
_cell_angle_alpha                90
_cell_angle_beta                 96.371(7)
_cell_angle_gamma                90
_cell_volume                     1408.35(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4032
_cell_measurement_temperature    300.00(10)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.12
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             690
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 -26 0.0206
1 -1 26 0.0206
4 12 2 0.0591
-4 -12 -2 0.0591
-11 4 6 0.0590
11 -4 -6 0.0590
5 -11 -6 0.0761
-12 -3 4 0.0661

_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.041
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
-1.3019 0.9470 -26.3480 0.9945 0.0598 0.0857
1.3019 -0.9470 26.3480 -0.9945 -0.0598 -0.0857
3.5014 11.5408 2.3828 0.0132 -0.0743 -0.9971
-3.5014 -11.5408 -2.3828 -0.0132 0.0743 0.9971
-11.3977 3.6924 6.1332 0.0603 -0.9971 0.0461
11.3977 -3.6924 -6.1332 -0.0603 0.9971 -0.0461
5.0506 -10.8465 -5.8183 -0.0498 0.7184 0.6938
-11.7708 -2.5994 4.1752 0.0462 -0.8372 0.5450

_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11743
_diffrn_reflns_point_group_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.780
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.766
_diffrn_reflns_theta_min         2.134
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -58.00  16.00   1.00   60.00    --    9.61 -30.00-142.00   74
  2  ω     -5.00  83.00   1.00   60.00    --    9.61  30.00  18.00   88
  3  ω     -9.00  46.00   1.00   60.00    --    9.61 -99.00-180.00   55
  4  ω    -37.00  18.00   1.00   60.00    --  -10.00  77.00-150.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0200198000
_diffrn_orient_matrix_UB_12      0.0146991000
_diffrn_orient_matrix_UB_13      -0.0362284000
_diffrn_orient_matrix_UB_21      0.0747707000
_diffrn_orient_matrix_UB_22      -0.0276861000
_diffrn_orient_matrix_UB_23      -0.0069574000
_diffrn_orient_matrix_UB_31      -0.0310797000
_diffrn_orient_matrix_UB_32      -0.0760539000
_diffrn_orient_matrix_UB_33      -0.0044490000
_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         0.725
_reflns_Friedel_fraction_full    0.878
_reflns_Friedel_fraction_max     0.698
_reflns_number_gt                4681
_reflns_number_total             6235
_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 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-TL (Sheldrick, 2015)'
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 
;
 Flack x determined using 1511 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6235
_refine_ls_number_restraints     62
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0532
_refine_ls_restrained_S_all      1.106
_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)+(0.0463P)²+0.1990P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1210
_refine_special_details          
;
 The dataset was treated as a single, averaged [FeₓNi₁₋ₓ(bpp)₂]2+ 
 cation site. The metal composition x = 0.50(2) was used for the refinement,
 which was derived from the 100 K structure from the same crystal.

 Both anions are disordered. One anion site was treated as one half-occupied 
 ClO₄⁻ plus two more sites with occupancies of 0.35 and 0.15 which 
 shared a second half-occupied Cl atom. The O atoms of the other anion were 
 refined over three orientations with occupacnies 0.45:0.40:0.15. These were 
 treated with the refined distance restraints listed below; an antibumping
 restraint between an N atom and a partial O atom was also applied to avoid
 an unrealistic intermolecualr contact. Lastly, an EADP thermal parameter 
 constraint between the two partial metal atoms was required to make the 
 refinement converge.

 All crystallographically ordered non-H atoms plus the partial metal sites 
 and Cl atoms were refined anisotropically, and H atoms were placed in 
 calculated positions and refined using a riding model.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Cl3A-O35A = Cl3A-O36A = Cl3A-O37A = Cl3A-O38A
 1.44284 with sigma of 0.02
 Cl3B-O35B = Cl3B-O36B = Cl3B-O37B = Cl3B-O38B
 1.44284 with sigma of 0.02
 Cl3B-O35C = Cl3B-O36C = Cl3B-O37C = Cl3B-O38C
 1.44284 with sigma of 0.02
 Cl39-O40A = Cl39-O41A = Cl39-O42A = Cl39-O43A
 1.44284 with sigma of 0.02
 Cl39-O40B = Cl39-O41B = Cl39-O42B = Cl39-O43B
 1.44284 with sigma of 0.02
 Cl39-O40C = Cl39-O41C = Cl39-O42C = Cl39-O43C
 1.44284 with sigma of 0.02
 O35A-O36A = O35A-O37A = O35A-O38A = O36A-O37A = O36A-O38A = O37A-O38A
 2.356158 with sigma of 0.02
 O35B-O36B = O35B-O37B = O35B-O38B = O36B-O37B = O36B-O38B = O37B-O38B
 2.356158 with sigma of 0.02
 O35C-O36C = O35C-O37C = O35C-O38C = O36C-O37C = O36C-O38C = O37C-O38C
 2.356158 with sigma of 0.02
 O40A-O41A = O40A-O42A = O40A-O43A = O41A-O42A = O41A-O43A = O42A-O43A
 2.356158 with sigma of 0.02
 O40B-O41B = O40B-O42B = O40B-O43B = O41B-O42B = O41B-O43B = O42B-O43B
 2.356158 with sigma of 0.02
 O40C-O41C = O40C-O42C = O40C-O43C = O41C-O42C = O41C-O43C = O42C-O43C
 2.356158 with sigma of 0.02
 N13-O38C
 -3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Ni1)
4. Others
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1)
 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2)
 X(Fe1)=X(Ni1)=FVAR(2)
 Y(Fe1)=Y(Ni1)=FVAR(3)
 Z(Fe1)=Z(Ni1)=FVAR(4)
 Fixed Sof: Fe1(0.5) Ni1(0.5) Cl3A(0.5) O35A(0.5) O36A(0.5) O37A(0.5)
 O38A(0.5) Cl3B(0.5) O35B(0.35) O36B(0.35) O37B(0.35) O38B(0.35) O35C(0.15)
 O36C(0.15) O37C(0.15) O38C(0.15) O40A(0.45) O41A(0.45) O42A(0.45) O43A(0.45)
 O40B(0.15) O41B(0.15) O42B(0.15) O43B(0.15) O40C(0.4) O41C(0.4) O42C(0.4)
 O43C(0.4)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.72921(8) 0.81376(9) 0.74755(4) 0.0467(2) Uani 0.5 1 d . . P A 1
Ni1 Ni 0.72921(8) 0.81376(9) 0.74755(4) 0.0467(2) Uani 0.5 1 d . . P A 2
N2 N 0.7186(5) 0.8217(6) 0.6400(2) 0.0445(10) Uani 1 1 d . . . . .
C3 C 0.5917(7) 0.8786(6) 0.6013(3) 0.0475(13) Uani 1 1 d . . . . .
C4 C 0.5789(8) 0.8869(7) 0.5301(3) 0.0616(17) Uani 1 1 d . . . . .
H4 H 0.488711 0.925514 0.504480 0.074 Uiso 1 1 calc R U . . .
C5 C 0.7063(9) 0.8353(9) 0.4971(4) 0.0717(19) Uani 1 1 d . . . . .
H5 H 0.702618 0.840790 0.448618 0.086 Uiso 1 1 calc R U . . .
C6 C 0.8370(8) 0.7767(7) 0.5359(3) 0.0613(17) Uani 1 1 d . . . . .
H6 H 0.922715 0.741817 0.514398 0.074 Uiso 1 1 calc R U . . .
C7 C 0.8377(7) 0.7709(6) 0.6071(3) 0.0488(14) Uani 1 1 d . . . . .
N8 N 0.4739(6) 0.9254(5) 0.6432(3) 0.0481(11) Uani 1 1 d . . . . .
N9 N 0.5005(6) 0.9074(5) 0.7136(3) 0.0501(12) Uani 1 1 d . . . . .
C10 C 0.3718(8) 0.9583(7) 0.7379(4) 0.0616(17) Uani 1 1 d . . . . .
H10 H 0.356132 0.959469 0.785045 0.074 Uiso 1 1 calc R U . . .
C11 C 0.2632(8) 1.0098(8) 0.6842(4) 0.070(2) Uani 1 1 d . . . . .
H11 H 0.164565 1.051776 0.688386 0.084 Uiso 1 1 calc R U . . .
C12 C 0.3301(8) 0.9865(7) 0.6240(4) 0.0670(19) Uani 1 1 d . . . . .
H12 H 0.285748 1.008290 0.578637 0.080 Uiso 1 1 calc R U . . .
N13 N 0.9604(6) 0.7135(5) 0.6543(3) 0.0542(13) Uani 1 1 d D . . . .
N14 N 0.9469(6) 0.7196(6) 0.7238(3) 0.0592(14) Uani 1 1 d . . . . .
C15 C 1.0738(9) 0.6494(8) 0.7553(5) 0.074(2) Uani 1 1 d . . . . .
H15 H 1.097247 0.637641 0.803510 0.089 Uiso 1 1 calc R U . . .
C16 C 1.1660(10) 0.5963(9) 0.7052(6) 0.087(3) Uani 1 1 d . . . . .
H16 H 1.260398 0.542504 0.713552 0.105 Uiso 1 1 calc R U . . .
C17 C 1.0929(9) 0.6372(8) 0.6420(5) 0.075(2) Uani 1 1 d . . . . .
H17 H 1.126782 0.617060 0.598590 0.090 Uiso 1 1 calc R U . . .
N18 N 0.7325(5) 0.7905(5) 0.8546(2) 0.0446(11) Uani 1 1 d . . . . .
C19 C 0.7863(6) 0.9045(6) 0.8979(3) 0.0452(13) Uani 1 1 d . . . . .
C20 C 0.7898(8) 0.8951(8) 0.9686(3) 0.0582(16) Uani 1 1 d . . . . .
H20 H 0.827841 0.976036 0.997692 0.070 Uiso 1 1 calc R U . . .
C21 C 0.7341(8) 0.7595(9) 0.9953(3) 0.0666(19) Uani 1 1 d . . . . .
H21 H 0.733649 0.749335 1.043444 0.080 Uiso 1 1 calc R U . . .
C22 C 0.6792(8) 0.6386(8) 0.9520(4) 0.0608(17) Uani 1 1 d . . . . .
H22 H 0.643352 0.546532 0.969881 0.073 Uiso 1 1 calc R U . . .
C23 C 0.6804(7) 0.6612(6) 0.8823(3) 0.0485(14) Uani 1 1 d . . . . .
N24 N 0.8407(6) 1.0322(5) 0.8614(2) 0.0504(12) Uani 1 1 d . . . . .
N25 N 0.8302(6) 1.0272(6) 0.7900(3) 0.0523(12) Uani 1 1 d . . . . .
C26 C 0.8980(8) 1.1559(8) 0.7721(4) 0.0643(19) Uani 1 1 d . . . . .
H26 H 0.908418 1.184085 0.726147 0.077 Uiso 1 1 calc R U . . .
C27 C 0.9523(9) 1.2449(9) 0.8303(4) 0.076(2) Uani 1 1 d . . . . .
H27 H 1.003531 1.340059 0.830849 0.092 Uiso 1 1 calc R U . . .
C28 C 0.9144(8) 1.1627(8) 0.8855(4) 0.0683(19) Uani 1 1 d . . . . .
H28 H 0.935381 1.191093 0.932357 0.082 Uiso 1 1 calc R U . . .
N29 N 0.6269(6) 0.5516(5) 0.8295(3) 0.0530(12) Uani 1 1 d . . . . .
N30 N 0.6389(6) 0.5869(6) 0.7617(3) 0.0547(12) Uani 1 1 d . . . . .
C31 C 0.5872(8) 0.4627(8) 0.7264(4) 0.069(2) Uani 1 1 d . . . . .
H31 H 0.582926 0.452461 0.677973 0.083 Uiso 1 1 calc R U . . .
C32 C 0.5402(8) 0.3500(8) 0.7705(5) 0.080(2) Uani 1 1 d . . . . .
H32 H 0.498348 0.253338 0.757604 0.096 Uiso 1 1 calc R U . . .
C33 C 0.5669(8) 0.4077(7) 0.8361(5) 0.074(2) Uani 1 1 d . . . . .
H33 H 0.547993 0.358511 0.877454 0.088 Uiso 1 1 calc R U . . .
Cl3A Cl 0.7962(10) 0.2669(10) 0.5698(5) 0.051(2) Uani 0.5 1 d D . P B 1
O35A O 0.6676(16) 0.2213(17) 0.6077(8) 0.061(4) Uiso 0.5 1 d D . P B 1
O36A O 0.7529(17) 0.2139(15) 0.4963(6) 0.075(5) Uiso 0.5 1 d D . P B 1
O37A O 0.8102(17) 0.4268(13) 0.5603(7) 0.092(5) Uiso 0.5 1 d D . P B 1
O38A O 0.9406(14) 0.1976(17) 0.5978(7) 0.086(4) Uiso 0.5 1 d D . P B 1
Cl3B Cl 0.8026(15) 0.2746(14) 0.5750(7) 0.084(4) Uani 0.5 1 d D . P . .
O35B O 0.7088(18) 0.1940(18) 0.6198(8) 0.063(5) Uiso 0.35 1 d D . P B 2
O36B O 0.9656(14) 0.2695(17) 0.6084(7) 0.069(4) Uiso 0.35 1 d D . P B 2
O37B O 0.796(2) 0.208(2) 0.5072(8) 0.077(7) Uiso 0.35 1 d D . P B 2
O38B O 0.7571(18) 0.4386(13) 0.5733(8) 0.057(4) Uiso 0.35 1 d D . P B 2
O35C O 0.642(3) 0.243(4) 0.5916(19) 0.067(15) Uiso 0.15 1 d D . P B 3
O36C O 0.896(3) 0.134(2) 0.5862(14) 0.052(7) Uiso 0.15 1 d D . P B 3
O37C O 0.797(4) 0.319(4) 0.5026(11) 0.093(10) Uiso 0.15 1 d D . P B 3
O38C O 0.870(4) 0.394(3) 0.6190(16) 0.096(11) Uiso 0.15 1 d D . P B 3
Cl39 Cl 0.7348(2) 0.2738(2) 1.06856(10) 0.0768(5) Uani 1 1 d D . . . .
O40A O 0.6523(19) 0.2438(18) 0.9933(6) 0.070(5) Uiso 0.45 1 d D . P C 1
O41A O 0.6803(16) 0.1397(13) 1.1051(7) 0.062(3) Uiso 0.45 1 d D . P C 1
O42A O 0.8861(12) 0.2765(16) 1.0611(6) 0.081(3) Uiso 0.45 1 d D . P C 1
O43A O 0.670(2) 0.4142(15) 1.0940(8) 0.106(5) Uiso 0.45 1 d D . P C 1
O40B O 0.876(3) 0.355(4) 1.0964(18) 0.107(13) Uiso 0.15 1 d D . P C 2
O41B O 0.727(4) 0.276(3) 0.9933(9) 0.063(9) Uiso 0.15 1 d D . P C 2
O42B O 0.720(4) 0.120(2) 1.0920(17) 0.075(14) Uiso 0.15 1 d D . P C 2
O43B O 0.605(3) 0.375(3) 1.0873(14) 0.055(8) Uiso 0.15 1 d D . P C 2
O40C O 0.6605(15) 0.2044(15) 1.1228(6) 0.070(4) Uiso 0.4 1 d D . P C 3
O41C O 0.783(2) 0.4285(13) 1.0966(8) 0.091(4) Uiso 0.4 1 d D . P C 3
O42C O 0.8985(13) 0.1928(14) 1.0724(6) 0.067(3) Uiso 0.4 1 d D . P C 3
O43C O 0.658(2) 0.278(2) 1.0024(7) 0.074(6) Uiso 0.4 1 d D . P C 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.058(4) . ?
Fe1 N9 2.150(5) . ?
Fe1 N14 2.127(5) . ?
Fe1 N18 2.063(4) . ?
Fe1 N25 2.155(5) . ?
Fe1 N30 2.132(5) . ?
Ni1 N2 2.058(4) . ?
Ni1 N9 2.150(5) . ?
Ni1 N14 2.127(5) . ?
Ni1 N18 2.063(4) . ?
Ni1 N25 2.155(5) . ?
Ni1 N30 2.132(5) . ?
N2 C3 1.339(7) . ?
N2 C7 1.332(7) . ?
C3 C4 1.361(8) . ?
C3 N8 1.417(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.393(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.369(10) . ?
C6 H6 0.9300 . ?
C6 C7 1.368(8) . ?
C7 N13 1.400(8) . ?
N8 N9 1.355(7) . ?
N8 C12 1.351(8) . ?
N9 C10 1.318(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.383(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.361(10) . ?
C12 H12 0.9300 . ?
N13 N14 1.354(7) . ?
N13 C17 1.353(8) . ?
N14 C15 1.329(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.389(12) . ?
C16 H16 0.9300 . ?
C16 C17 1.348(12) . ?
C17 H17 0.9300 . ?
N18 C19 1.336(7) . ?
N18 C23 1.333(7) . ?
C19 C20 1.357(8) . ?
C19 N24 1.411(7) . ?
C20 H20 0.9300 . ?
C20 C21 1.383(9) . ?
C21 H21 0.9300 . ?
C21 C22 1.382(10) . ?
C22 H22 0.9300 . ?
C22 C23 1.354(9) . ?
C23 N29 1.424(8) . ?
N24 N25 1.367(6) . ?
N24 C28 1.346(8) . ?
N25 C26 1.315(8) . ?
C26 H26 0.9300 . ?
C26 C27 1.392(10) . ?
C27 H27 0.9300 . ?
C27 C28 1.345(10) . ?
C28 H28 0.9300 . ?
N29 N30 1.353(7) . ?
N29 C33 1.354(8) . ?
N30 C31 1.318(8) . ?
C31 H31 0.9300 . ?
C31 C32 1.378(10) . ?
C32 H32 0.9300 . ?
C32 C33 1.351(10) . ?
C33 H33 0.9300 . ?
Cl3A O35A 1.440(11) . ?
Cl3A O36A 1.492(13) . ?
Cl3A O37A 1.398(13) . ?
Cl3A O38A 1.423(13) . ?
Cl3B O35B 1.422(14) . ?
Cl3B O36B 1.470(15) . ?
Cl3B O37B 1.419(16) . ?
Cl3B O38B 1.466(15) . ?
Cl3B O35C 1.471(19) . ?
Cl3B O36C 1.454(18) . ?
Cl3B O37C 1.437(19) . ?
Cl3B O38C 1.413(18) . ?
Cl39 O40A 1.558(12) . ?
Cl39 O41A 1.456(9) . ?
Cl39 O42A 1.318(10) . ?
Cl39 O43A 1.441(12) . ?
Cl39 O40B 1.443(19) . ?
Cl39 O41B 1.440(17) . ?
Cl39 O42B 1.413(18) . ?
Cl39 O43B 1.489(17) . ?
Cl39 O40C 1.413(11) . ?
Cl39 O41C 1.481(12) . ?
Cl39 O42C 1.559(11) . ?
Cl39 O43C 1.365(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 75.29(19) . . ?
N2 Fe1 N14 74.9(2) . . ?
N2 Fe1 N18 175.9(2) . . ?
N2 Fe1 N25 108.78(19) . . ?
N2 Fe1 N30 100.5(2) . . ?
N9 Fe1 N25 96.15(18) . . ?
N14 Fe1 N9 150.2(2) . . ?
N14 Fe1 N25 94.76(19) . . ?
N14 Fe1 N30 90.9(2) . . ?
N18 Fe1 N9 104.47(18) . . ?
N18 Fe1 N14 105.1(2) . . ?
N18 Fe1 N25 75.28(19) . . ?
N18 Fe1 N30 75.5(2) . . ?
N30 Fe1 N9 93.03(19) . . ?
N30 Fe1 N25 150.66(19) . . ?
N2 Ni1 N9 75.29(19) . . ?
N2 Ni1 N14 74.9(2) . . ?
N2 Ni1 N18 175.9(2) . . ?
N2 Ni1 N25 108.78(19) . . ?
N2 Ni1 N30 100.5(2) . . ?
N9 Ni1 N25 96.15(18) . . ?
N14 Ni1 N9 150.2(2) . . ?
N14 Ni1 N25 94.76(19) . . ?
N14 Ni1 N30 90.9(2) . . ?
N18 Ni1 N9 104.47(18) . . ?
N18 Ni1 N14 105.1(2) . . ?
N18 Ni1 N25 75.28(19) . . ?
N18 Ni1 N30 75.5(2) . . ?
N30 Ni1 N9 93.03(19) . . ?
N30 Ni1 N25 150.66(19) . . ?
C3 N2 Fe1 120.8(4) . . ?
C3 N2 Ni1 120.8(4) . . ?
C7 N2 Fe1 121.0(4) . . ?
C7 N2 Ni1 121.0(4) . . ?
C7 N2 C3 118.2(5) . . ?
N2 C3 C4 123.1(5) . . ?
N2 C3 N8 111.9(5) . . ?
C4 C3 N8 125.0(6) . . ?
C3 C4 H4 121.3 . . ?
C3 C4 C5 117.4(6) . . ?
C5 C4 H4 121.3 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.3(6) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 121.0 . . ?
C7 C6 C5 118.0(6) . . ?
C7 C6 H6 121.0 . . ?
N2 C7 C6 123.0(6) . . ?
N2 C7 N13 111.5(5) . . ?
C6 C7 N13 125.5(6) . . ?
N9 N8 C3 118.9(5) . . ?
C12 N8 C3 129.7(6) . . ?
C12 N8 N9 111.4(5) . . ?
N8 N9 Fe1 113.1(3) . . ?
N8 N9 Ni1 113.1(3) . . ?
C10 N9 Fe1 141.8(5) . . ?
C10 N9 Ni1 141.8(5) . . ?
C10 N9 N8 105.1(5) . . ?
N9 C10 H10 124.4 . . ?
N9 C10 C11 111.2(6) . . ?
C11 C10 H10 124.4 . . ?
C10 C11 H11 127.0 . . ?
C12 C11 C10 106.0(6) . . ?
C12 C11 H11 127.0 . . ?
N8 C12 C11 106.4(7) . . ?
N8 C12 H12 126.8 . . ?
C11 C12 H12 126.8 . . ?
N14 N13 C7 119.0(5) . . ?
C17 N13 C7 129.9(6) . . ?
C17 N13 N14 110.9(6) . . ?
N13 N14 Fe1 113.5(4) . . ?
N13 N14 Ni1 113.5(4) . . ?
C15 N14 Fe1 140.1(6) . . ?
C15 N14 Ni1 140.1(6) . . ?
C15 N14 N13 106.0(6) . . ?
N14 C15 H15 125.3 . . ?
N14 C15 C16 109.4(8) . . ?
C16 C15 H15 125.3 . . ?
C15 C16 H16 126.4 . . ?
C17 C16 C15 107.2(7) . . ?
C17 C16 H16 126.4 . . ?
N13 C17 H17 126.7 . . ?
C16 C17 N13 106.5(7) . . ?
C16 C17 H17 126.7 . . ?
C19 N18 Fe1 121.0(4) . . ?
C19 N18 Ni1 121.0(4) . . ?
C23 N18 Fe1 120.7(4) . . ?
C23 N18 Ni1 120.7(4) . . ?
C23 N18 C19 118.3(5) . . ?
N18 C19 C20 123.1(5) . . ?
N18 C19 N24 112.0(5) . . ?
C20 C19 N24 124.8(5) . . ?
C19 C20 H20 121.6 . . ?
C19 C20 C21 116.8(6) . . ?
C21 C20 H20 121.6 . . ?
C20 C21 H21 119.2 . . ?
C22 C21 C20 121.6(6) . . ?
C22 C21 H21 119.2 . . ?
C21 C22 H22 121.8 . . ?
C23 C22 C21 116.5(6) . . ?
C23 C22 H22 121.8 . . ?
N18 C23 C22 123.7(6) . . ?
N18 C23 N29 111.5(5) . . ?
C22 C23 N29 124.8(5) . . ?
N25 N24 C19 119.0(5) . . ?
C28 N24 C19 130.5(5) . . ?
C28 N24 N25 110.4(5) . . ?
N24 N25 Fe1 112.7(3) . . ?
N24 N25 Ni1 112.7(3) . . ?
C26 N25 Fe1 142.4(5) . . ?
C26 N25 Ni1 142.4(5) . . ?
C26 N25 N24 104.7(5) . . ?
N25 C26 H26 124.0 . . ?
N25 C26 C27 112.0(6) . . ?
C27 C26 H26 124.0 . . ?
C26 C27 H27 127.6 . . ?
C28 C27 C26 104.7(6) . . ?
C28 C27 H27 127.6 . . ?
N24 C28 H28 125.9 . . ?
C27 C28 N24 108.3(7) . . ?
C27 C28 H28 125.9 . . ?
N30 N29 C23 118.9(5) . . ?
N30 N29 C33 111.5(6) . . ?
C33 N29 C23 129.6(6) . . ?
N29 N30 Fe1 113.4(4) . . ?
N29 N30 Ni1 113.4(4) . . ?
C31 N30 Fe1 141.8(5) . . ?
C31 N30 Ni1 141.8(5) . . ?
C31 N30 N29 104.9(6) . . ?
N30 C31 H31 124.4 . . ?
N30 C31 C32 111.1(7) . . ?
C32 C31 H31 124.4 . . ?
C31 C32 H32 126.8 . . ?
C33 C32 C31 106.5(6) . . ?
C33 C32 H32 126.8 . . ?
N29 C33 H33 127.0 . . ?
C32 C33 N29 106.1(7) . . ?
C32 C33 H33 127.0 . . ?
O35A Cl3A O36A 105.7(10) . . ?
O37A Cl3A O35A 114.7(9) . . ?
O37A Cl3A O36A 101.2(9) . . ?
O37A Cl3A O38A 112.4(11) . . ?
O38A Cl3A O35A 112.0(10) . . ?
O38A Cl3A O36A 110.0(9) . . ?
O35B Cl3B O36B 107.1(11) . . ?
O35B Cl3B O38B 108.6(12) . . ?
O37B Cl3B O35B 113.0(13) . . ?
O37B Cl3B O36B 109.1(12) . . ?
O37B Cl3B O38B 112.8(12) . . ?
O38B Cl3B O36B 105.9(11) . . ?
O36C Cl3B O35C 109.0(16) . . ?
O37C Cl3B O35C 109.2(16) . . ?
O37C Cl3B O36C 108.9(15) . . ?
O38C Cl3B O35C 109.6(17) . . ?
O38C Cl3B O36C 109.7(16) . . ?
O38C Cl3B O37C 110.6(17) . . ?
O41A Cl39 O40A 100.3(8) . . ?
O42A Cl39 O40A 104.6(8) . . ?
O42A Cl39 O41A 115.9(8) . . ?
O42A Cl39 O43A 116.3(9) . . ?
O43A Cl39 O40A 107.5(9) . . ?
O43A Cl39 O41A 110.3(8) . . ?
O40B Cl39 O43B 104.1(15) . . ?
O41B Cl39 O40B 108.0(15) . . ?
O41B Cl39 O43B 106.3(14) . . ?
O42B Cl39 O40B 116.0(17) . . ?
O42B Cl39 O41B 109.7(16) . . ?
O42B Cl39 O43B 112.1(16) . . ?
O40C Cl39 O41C 104.1(8) . . ?
O40C Cl39 O42C 104.6(7) . . ?
O41C Cl39 O42C 99.9(8) . . ?
O43C Cl39 O40C 119.3(10) . . ?
O43C Cl39 O41C 113.5(10) . . ?
O43C Cl39 O42C 113.2(9) . . ?

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 N2 C3 C4 179.8(4) . . . . ?
Fe1 N2 C3 N8 -1.2(6) . . . . ?
Fe1 N2 C7 C6 -178.7(4) . . . . ?
Fe1 N2 C7 N13 0.9(6) . . . . ?
Fe1 N9 C10 C11 178.1(5) . . . . ?
Fe1 N14 C15 C16 171.0(5) . . . . ?
Fe1 N18 C19 C20 179.5(4) . . . . ?
Fe1 N18 C19 N24 -1.6(6) . . . . ?
Fe1 N18 C23 C22 -180.0(5) . . . . ?
Fe1 N18 C23 N29 0.0(6) . . . . ?
Fe1 N25 C26 C27 -173.7(5) . . . . ?
Fe1 N30 C31 C32 -178.5(5) . . . . ?
Ni1 N2 C3 C4 179.8(4) . . . . ?
Ni1 N2 C3 N8 -1.2(6) . . . . ?
Ni1 N2 C7 C6 -178.7(4) . . . . ?
Ni1 N2 C7 N13 0.9(6) . . . . ?
Ni1 N9 C10 C11 178.1(5) . . . . ?
Ni1 N14 C15 C16 171.0(5) . . . . ?
Ni1 N18 C19 C20 179.5(4) . . . . ?
Ni1 N18 C19 N24 -1.6(6) . . . . ?
Ni1 N18 C23 C22 -180.0(5) . . . . ?
Ni1 N18 C23 N29 0.0(6) . . . . ?
Ni1 N25 C26 C27 -173.7(5) . . . . ?
Ni1 N30 C31 C32 -178.5(5) . . . . ?
N2 C3 C4 C5 -1.0(9) . . . . ?
N2 C3 N8 N9 -0.5(7) . . . . ?
N2 C3 N8 C12 -179.4(6) . . . . ?
N2 C7 N13 N14 -1.7(7) . . . . ?
N2 C7 N13 C17 172.1(6) . . . . ?
C3 N2 C7 C6 1.2(8) . . . . ?
C3 N2 C7 N13 -179.3(5) . . . . ?
C3 C4 C5 C6 1.0(10) . . . . ?
C3 N8 N9 Fe1 1.8(6) . . . . ?
C3 N8 N9 Ni1 1.8(6) . . . . ?
C3 N8 N9 C10 -179.2(5) . . . . ?
C3 N8 C12 C11 179.6(6) . . . . ?
C4 C3 N8 N9 178.5(5) . . . . ?
C4 C3 N8 C12 -0.4(9) . . . . ?
C4 C5 C6 C7 -0.1(10) . . . . ?
C5 C6 C7 N2 -1.1(9) . . . . ?
C5 C6 C7 N13 179.4(6) . . . . ?
C6 C7 N13 N14 177.9(5) . . . . ?
C6 C7 N13 C17 -8.3(10) . . . . ?
C7 N2 C3 C4 -0.1(8) . . . . ?
C7 N2 C3 N8 178.9(5) . . . . ?
C7 N13 N14 Fe1 1.7(6) . . . . ?
C7 N13 N14 Ni1 1.7(6) . . . . ?
C7 N13 N14 C15 176.2(5) . . . . ?
C7 N13 C17 C16 -175.1(6) . . . . ?
N8 C3 C4 C5 -179.9(6) . . . . ?
N8 N9 C10 C11 -0.4(7) . . . . ?
N9 N8 C12 C11 0.6(7) . . . . ?
N9 C10 C11 C12 0.8(8) . . . . ?
C10 C11 C12 N8 -0.8(7) . . . . ?
C12 N8 N9 Fe1 -179.1(4) . . . . ?
C12 N8 N9 Ni1 -179.1(4) . . . . ?
C12 N8 N9 C10 -0.1(6) . . . . ?
N13 N14 C15 C16 -1.2(8) . . . . ?
N14 N13 C17 C16 -0.9(8) . . . . ?
N14 C15 C16 C17 0.6(9) . . . . ?
C15 C16 C17 N13 0.2(9) . . . . ?
C17 N13 N14 Fe1 -173.2(4) . . . . ?
C17 N13 N14 Ni1 -173.2(4) . . . . ?
C17 N13 N14 C15 1.3(7) . . . . ?
N18 C19 C20 C21 0.0(9) . . . . ?
N18 C19 N24 N25 1.3(7) . . . . ?
N18 C19 N24 C28 -174.0(6) . . . . ?
N18 C23 N29 N30 2.0(7) . . . . ?
N18 C23 N29 C33 179.5(6) . . . . ?
C19 N18 C23 C22 -0.2(8) . . . . ?
C19 N18 C23 N29 179.8(4) . . . . ?
C19 C20 C21 C22 0.7(10) . . . . ?
C19 N24 N25 Fe1 -0.4(6) . . . . ?
C19 N24 N25 Ni1 -0.4(6) . . . . ?
C19 N24 N25 C26 -176.2(5) . . . . ?
C19 N24 C28 C27 175.8(6) . . . . ?
C20 C19 N24 N25 -179.9(5) . . . . ?
C20 C19 N24 C28 4.9(10) . . . . ?
C20 C21 C22 C23 -1.1(10) . . . . ?
C21 C22 C23 N18 0.8(9) . . . . ?
C21 C22 C23 N29 -179.2(6) . . . . ?
C22 C23 N29 N30 -178.0(5) . . . . ?
C22 C23 N29 C33 -0.5(10) . . . . ?
C23 N18 C19 C20 -0.2(8) . . . . ?
C23 N18 C19 N24 178.6(4) . . . . ?
C23 N29 N30 Fe1 -3.0(6) . . . . ?
C23 N29 N30 Ni1 -3.0(6) . . . . ?
C23 N29 N30 C31 177.4(5) . . . . ?
C23 N29 C33 C32 -177.7(6) . . . . ?
N24 C19 C20 C21 -178.7(5) . . . . ?
N24 N25 C26 C27 -0.1(7) . . . . ?
N25 N24 C28 C27 0.2(8) . . . . ?
N25 C26 C27 C28 0.2(9) . . . . ?
C26 C27 C28 N24 -0.3(8) . . . . ?
C28 N24 N25 Fe1 175.7(4) . . . . ?
C28 N24 N25 Ni1 175.7(4) . . . . ?
C28 N24 N25 C26 -0.1(6) . . . . ?
N29 N30 C31 C32 0.9(7) . . . . ?
N30 N29 C33 C32 0.0(7) . . . . ?
N30 C31 C32 C33 -0.9(8) . . . . ?
C31 C32 C33 N29 0.5(8) . . . . ?
C33 N29 N30 Fe1 179.1(4) . . . . ?
C33 N29 N30 Ni1 179.1(4) . . . . ?
C33 N29 N30 C31 -0.6(7) . . . . ?

_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 1.725
_oxdiff_exptl_absorpt_empirical_full_min 0.692
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_mh722
_database_code_depnum_ccdc_archive 'CCDC 2332660'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-02-12
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-nickel(II) ditetrafluoroborate 0.50:0.50 solid solution'
_chemical_formula_moiety         'C22 H18 Fe0.5 N10 Ni0.5, 2(Cl O4)'
_chemical_formula_sum            'C22 H18 Cl2 Fe0.50 N10 Ni0.50 O8'
_chemical_formula_weight         678.64
_chemical_absolute_configuration ab
_chemical_melting_point          ?
_chemical_oxdiff_formula         C22H18Cl2Fe0.5N10Ni0.5O8
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'
Cl Cl 0.1484 0.1585 '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'
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'

_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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.4913(4)
_cell_length_b                   8.5507(4)
_cell_length_c                   18.7250(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.181(4)
_cell_angle_gamma                90
_cell_volume                     1345.72(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5859
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.1750
_cell_measurement_theta_min      2.1950
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             690
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 1 -25 0.0206
2 -1 25 0.0206
4 11 1 0.0591
-4 -11 -1 0.0591
-11 4 7 0.0590
11 -4 -7 0.0590
5 -11 -6 0.0761
-12 -2 6 0.0661

_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.041
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
-1.6411 0.7894 -25.3178 0.9945 0.0598 0.0857
1.6411 -0.7894 25.3178 -0.9945 -0.0598 -0.0857
3.6619 11.4178 1.4261 0.0132 -0.0743 -0.9971
-3.6619 -11.4178 -1.4261 -0.0132 0.0743 0.9971
-11.2150 3.8365 7.3748 0.0603 -0.9971 0.0461
11.2150 -3.8365 -7.3748 -0.0603 0.9971 -0.0461
4.8123 -10.8531 -5.9505 -0.0498 0.7184 0.6938
-11.6917 -2.4108 5.7485 0.0462 -0.8372 0.5450

_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11197
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.771
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.895
_diffrn_reflns_theta_min         2.198
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -58.00  16.00   1.00   30.00    --    9.61 -30.00-142.00   74
  2  ω     -5.00  83.00   1.00   30.00    --    9.61  30.00  18.00   88
  3  ω     -9.00  46.00   1.00   30.00    --    9.61 -99.00-180.00   55
  4  ω    -37.00  18.00   1.00   30.00    --  -10.00  77.00-150.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0251087000
_diffrn_orient_matrix_UB_12      0.0138596000
_diffrn_orient_matrix_UB_13      -0.0372222000
_diffrn_orient_matrix_UB_21      0.0736569000
_diffrn_orient_matrix_UB_22      -0.0291257000
_diffrn_orient_matrix_UB_23      -0.0080426000
_diffrn_orient_matrix_UB_31      -0.0326502000
_diffrn_orient_matrix_UB_32      -0.0764056000
_diffrn_orient_matrix_UB_33      -0.0036495000
_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         0.714
_reflns_Friedel_fraction_full    0.874
_reflns_Friedel_fraction_max     0.685
_reflns_number_gt                5496
_reflns_number_total             5975
_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 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-TL (Sheldrick, 2015)'
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 
;
 Flack x determined using 2061 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5975
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0377
_refine_ls_restrained_S_all      1.033
_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)+(0.0184P)²+0.9072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0739
_refine_special_details          
;
 The dataset was treated as a single, averaged [FeₓNi₁₋ₓ(bpp)₂]2+ 
 cation site. Partial Fe and Ni atoms were refined with the same cartesian 
 coordinates, whose Ueq value converged to 0.013. The metal composition 
 x refined to 0.50(2) when the partial metal sites were constrained to have 
 that Ueq value, so this occupancy was used in the final least squares 
 cycles. The bond lengths and angles about Fe1/Ni1 agree well with weighted
 average values calculated from the pure Fe and Ni complex.

 No anion disorder is included in the model. However, an EADP thermal
 parameter constraint between the two partial metal atoms was required
  to make the model converge. All non-H atoms were refined anisotropically, 
 and H atoms were placed in calculated positions and refined using a 
 riding model. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Ni1)
3. Others
 X(Fe1)=X(Ni1)=FVAR(1)
 Y(Fe1)=Y(Ni1)=FVAR(2)
 Z(Fe1)=Z(Ni1)=FVAR(3)
 Fixed Sof: Fe1(0.5) Ni1(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.78397(6) 0.75127(5) 0.75337(3) 0.01262(12) Uani 0.5 1 d . . P A 1
Ni1 Ni 0.78397(6) 0.75127(5) 0.75337(3) 0.01262(12) Uani 0.5 1 d . . P A 2
N2 N 0.7897(4) 0.7705(4) 0.85758(16) 0.0141(7) Uani 1 1 d . . . . .
C3 C 0.9167(5) 0.8302(4) 0.8983(2) 0.0158(8) Uani 1 1 d . . . . .
C4 C 0.9268(5) 0.8442(4) 0.9722(2) 0.0181(8) Uani 1 1 d . . . . .
H4 H 1.018317 0.886881 1.000614 0.022 Uiso 1 1 calc R U . . .
C5 C 0.7965(5) 0.7927(4) 1.0033(2) 0.0197(9) Uani 1 1 d . . . . .
H5 H 0.798898 0.801008 1.054017 0.024 Uiso 1 1 calc R U . . .
C6 C 0.6636(5) 0.7298(5) 0.9620(2) 0.0195(8) Uani 1 1 d . . . . .
H6 H 0.574346 0.695101 0.983040 0.023 Uiso 1 1 calc R U . . .
C7 C 0.6671(4) 0.7198(4) 0.8886(2) 0.0139(8) Uani 1 1 d . . . . .
N8 N 1.0342(4) 0.8731(4) 0.85680(18) 0.0156(7) Uani 1 1 d . . . . .
N9 N 1.0046(4) 0.8471(4) 0.78380(18) 0.0165(7) Uani 1 1 d . . . . .
C10 C 1.1347(5) 0.8943(5) 0.7584(2) 0.0214(9) Uani 1 1 d . . . . .
H10 H 1.149063 0.890517 0.709025 0.026 Uiso 1 1 calc R U . . .
C11 C 1.2478(5) 0.9506(5) 0.8141(2) 0.0227(10) Uani 1 1 d . . . . .
H11 H 1.350432 0.990598 0.809794 0.027 Uiso 1 1 calc R U . . .
C12 C 1.1809(5) 0.9363(5) 0.8759(2) 0.0210(9) Uani 1 1 d . . . . .
H12 H 1.227951 0.965126 0.923152 0.025 Uiso 1 1 calc R U . . .
N13 N 0.5463(4) 0.6555(4) 0.83784(18) 0.0173(7) Uani 1 1 d . . . . .
N14 N 0.5696(4) 0.6611(4) 0.76662(18) 0.0179(7) Uani 1 1 d . . . . .
C15 C 0.4457(5) 0.5886(5) 0.7308(3) 0.0237(10) Uani 1 1 d . . . . .
H15 H 0.428083 0.574526 0.679994 0.028 Uiso 1 1 calc R U . . .
C16 C 0.3429(5) 0.5348(5) 0.7785(3) 0.0280(11) Uani 1 1 d . . . . .
H16 H 0.246192 0.478857 0.766224 0.034 Uiso 1 1 calc R U . . .
C17 C 0.4105(5) 0.5791(5) 0.8454(3) 0.0243(10) Uani 1 1 d . . . . .
H17 H 0.369850 0.560063 0.889273 0.029 Uiso 1 1 calc R U . . .
N18 N 0.7787(4) 0.7221(4) 0.64965(16) 0.0146(7) Uani 1 1 d . . . . .
C19 C 0.7193(5) 0.8333(5) 0.6035(2) 0.0158(8) Uani 1 1 d . . . . .
C20 C 0.7110(5) 0.8160(5) 0.5296(2) 0.0178(8) Uani 1 1 d . . . . .
H20 H 0.669051 0.896184 0.497288 0.021 Uiso 1 1 calc R U . . .
C21 C 0.7665(5) 0.6765(5) 0.5049(2) 0.0200(9) Uani 1 1 d . . . . .
H21 H 0.764062 0.661582 0.454435 0.024 Uiso 1 1 calc R U . . .
C22 C 0.8256(5) 0.5584(5) 0.5519(2) 0.0186(9) Uani 1 1 d . . . . .
H22 H 0.861460 0.461926 0.534905 0.022 Uiso 1 1 calc R U . . .
C23 C 0.8297(5) 0.5877(4) 0.6242(2) 0.0158(8) Uani 1 1 d . . . . .
N24 N 0.6659(4) 0.9623(4) 0.63907(18) 0.0165(7) Uani 1 1 d . . . . .
N25 N 0.6835(4) 0.9569(4) 0.71324(18) 0.0173(7) Uani 1 1 d . . . . .
C26 C 0.6160(5) 1.0876(5) 0.7325(3) 0.0238(10) Uani 1 1 d . . . . .
H26 H 0.609828 1.117268 0.780897 0.029 Uiso 1 1 calc R U . . .
C27 C 0.5551(5) 1.1754(5) 0.6718(3) 0.0278(10) Uani 1 1 d . . . . .
H27 H 0.501053 1.272745 0.671306 0.033 Uiso 1 1 calc R U . . .
C28 C 0.5888(5) 1.0933(5) 0.6134(2) 0.0220(9) Uani 1 1 d . . . . .
H28 H 0.563065 1.122599 0.564205 0.026 Uiso 1 1 calc R U . . .
N29 N 0.8859(4) 0.4845(4) 0.68061(18) 0.0168(7) Uani 1 1 d . . . . .
N30 N 0.8752(4) 0.5320(4) 0.74963(18) 0.0169(7) Uani 1 1 d . . . . .
C31 C 0.9245(5) 0.4110(5) 0.7906(3) 0.0236(10) Uani 1 1 d . . . . .
H31 H 0.928982 0.408912 0.841591 0.028 Uiso 1 1 calc R U . . .
C32 C 0.9691(5) 0.2866(5) 0.7496(3) 0.0274(10) Uani 1 1 d . . . . .
H32 H 1.009298 0.187832 0.766795 0.033 Uiso 1 1 calc R U . . .
C33 C 0.9429(5) 0.3365(5) 0.6798(3) 0.0230(10) Uani 1 1 d . . . . .
H33 H 0.961117 0.278625 0.638496 0.028 Uiso 1 1 calc R U . . .
Cl34 Cl 0.30209(12) 0.71677(10) 1.06459(5) 0.0200(2) Uani 1 1 d . . . . .
O35 O 0.4571(4) 0.6663(4) 1.09858(18) 0.0416(10) Uani 1 1 d . . . . .
O36 O 0.1819(4) 0.6604(3) 1.10485(16) 0.0259(7) Uani 1 1 d . . . . .
O37 O 0.2963(4) 0.8852(3) 1.06334(18) 0.0302(8) Uani 1 1 d . . . . .
O38 O 0.2729(4) 0.6597(4) 0.99165(16) 0.0283(7) Uani 1 1 d . . . . .
Cl39 Cl 0.78396(13) 0.18695(12) 0.44247(5) 0.0238(2) Uani 1 1 d . . . . .
O40 O 0.8615(4) 0.1710(4) 0.51581(15) 0.0275(7) Uani 1 1 d . . . . .
O41 O 0.8186(4) 0.0536(4) 0.40117(18) 0.0357(8) Uani 1 1 d . . . . .
O42 O 0.6159(4) 0.1937(5) 0.44270(17) 0.0444(10) Uani 1 1 d . . . . .
O43 O 0.8420(6) 0.3241(4) 0.4116(2) 0.0529(12) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.952(3) . ?
Fe1 N9 2.050(4) . ?
Fe1 N14 2.024(4) . ?
Fe1 N18 1.952(3) . ?
Fe1 N25 2.050(4) . ?
Fe1 N30 2.034(3) . ?
Ni1 N2 1.952(3) . ?
Ni1 N9 2.050(4) . ?
Ni1 N14 2.024(4) . ?
Ni1 N18 1.952(3) . ?
Ni1 N25 2.050(4) . ?
Ni1 N30 2.034(3) . ?
N2 C3 1.331(5) . ?
N2 C7 1.334(5) . ?
C3 C4 1.379(5) . ?
C3 N8 1.398(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.393(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.383(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.382(5) . ?
C7 N13 1.407(5) . ?
N8 N9 1.372(5) . ?
N8 C12 1.359(5) . ?
N9 C10 1.326(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.399(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.365(6) . ?
C12 H12 0.9500 . ?
N13 N14 1.377(5) . ?
N13 C17 1.350(5) . ?
N14 C15 1.319(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.411(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.355(6) . ?
C17 H17 0.9500 . ?
N18 C19 1.335(5) . ?
N18 C23 1.339(5) . ?
C19 C20 1.383(5) . ?
C19 N24 1.397(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.386(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.386(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.372(5) . ?
C23 N29 1.407(5) . ?
N24 N25 1.376(4) . ?
N24 C28 1.351(5) . ?
N25 C26 1.329(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.399(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.363(6) . ?
C28 H28 0.9500 . ?
N29 N30 1.370(4) . ?
N29 C33 1.356(5) . ?
N30 C31 1.320(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.395(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.363(6) . ?
C33 H33 0.9500 . ?
Cl34 O35 1.444(3) . ?
Cl34 O36 1.436(3) . ?
Cl34 O37 1.441(3) . ?
Cl34 O38 1.438(3) . ?
Cl39 O40 1.442(3) . ?
Cl39 O41 1.432(3) . ?
Cl39 O42 1.429(3) . ?
Cl39 O43 1.426(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 78.28(13) . . ?
N2 Fe1 N14 78.72(13) . . ?
N2 Fe1 N18 177.49(15) . . ?
N2 Fe1 N25 104.13(13) . . ?
N2 Fe1 N30 99.01(13) . . ?
N9 Fe1 N25 94.32(13) . . ?
N14 Fe1 N9 156.98(13) . . ?
N14 Fe1 N25 92.13(13) . . ?
N14 Fe1 N30 90.38(13) . . ?
N18 Fe1 N9 102.59(13) . . ?
N18 Fe1 N14 100.35(13) . . ?
N18 Fe1 N25 78.20(13) . . ?
N18 Fe1 N30 78.63(14) . . ?
N30 Fe1 N9 92.32(13) . . ?
N30 Fe1 N25 156.77(13) . . ?
N2 Ni1 N9 78.28(13) . . ?
N2 Ni1 N14 78.72(13) . . ?
N2 Ni1 N18 177.49(15) . . ?
N2 Ni1 N25 104.13(13) . . ?
N2 Ni1 N30 99.01(13) . . ?
N9 Ni1 N25 94.32(13) . . ?
N14 Ni1 N9 156.98(13) . . ?
N14 Ni1 N25 92.13(13) . . ?
N14 Ni1 N30 90.38(13) . . ?
N18 Ni1 N9 102.59(13) . . ?
N18 Ni1 N14 100.35(13) . . ?
N18 Ni1 N25 78.20(13) . . ?
N18 Ni1 N30 78.63(14) . . ?
N30 Ni1 N9 92.32(13) . . ?
N30 Ni1 N25 156.77(13) . . ?
C3 N2 Fe1 120.5(3) . . ?
C3 N2 Ni1 120.5(3) . . ?
C3 N2 C7 119.6(3) . . ?
C7 N2 Fe1 119.8(3) . . ?
C7 N2 Ni1 119.8(3) . . ?
N2 C3 C4 122.5(4) . . ?
N2 C3 N8 111.5(3) . . ?
C4 C3 N8 126.0(4) . . ?
C3 C4 H4 121.6 . . ?
C3 C4 C5 116.9(4) . . ?
C5 C4 H4 121.6 . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.5(4) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 H6 121.7 . . ?
C7 C6 C5 116.7(4) . . ?
C7 C6 H6 121.7 . . ?
N2 C7 C6 122.8(3) . . ?
N2 C7 N13 111.9(3) . . ?
C6 C7 N13 125.3(4) . . ?
N9 N8 C3 117.9(3) . . ?
C12 N8 C3 131.2(4) . . ?
C12 N8 N9 110.9(3) . . ?
N8 N9 Fe1 111.8(2) . . ?
N8 N9 Ni1 111.8(2) . . ?
C10 N9 Fe1 142.8(3) . . ?
C10 N9 Ni1 142.8(3) . . ?
C10 N9 N8 105.3(3) . . ?
N9 C10 H10 124.6 . . ?
N9 C10 C11 110.8(4) . . ?
C11 C10 H10 124.6 . . ?
C10 C11 H11 127.0 . . ?
C12 C11 C10 106.1(4) . . ?
C12 C11 H11 127.0 . . ?
N8 C12 C11 106.8(4) . . ?
N8 C12 H12 126.6 . . ?
C11 C12 H12 126.6 . . ?
N14 N13 C7 116.7(3) . . ?
C17 N13 C7 132.1(4) . . ?
C17 N13 N14 111.1(3) . . ?
N13 N14 Fe1 112.8(2) . . ?
N13 N14 Ni1 112.8(2) . . ?
C15 N14 Fe1 141.5(3) . . ?
C15 N14 Ni1 141.5(3) . . ?
C15 N14 N13 105.2(4) . . ?
N14 C15 H15 124.7 . . ?
N14 C15 C16 110.6(4) . . ?
C16 C15 H15 124.7 . . ?
C15 C16 H16 127.0 . . ?
C17 C16 C15 105.9(4) . . ?
C17 C16 H16 127.0 . . ?
N13 C17 C16 107.1(4) . . ?
N13 C17 H17 126.4 . . ?
C16 C17 H17 126.4 . . ?
C19 N18 Fe1 120.4(3) . . ?
C19 N18 Ni1 120.4(3) . . ?
C19 N18 C23 119.5(3) . . ?
C23 N18 Fe1 120.1(3) . . ?
C23 N18 Ni1 120.1(3) . . ?
N18 C19 C20 122.2(4) . . ?
N18 C19 N24 111.8(3) . . ?
C20 C19 N24 126.0(4) . . ?
C19 C20 H20 121.4 . . ?
C19 C20 C21 117.1(4) . . ?
C21 C20 H20 121.4 . . ?
C20 C21 H21 119.2 . . ?
C22 C21 C20 121.6(4) . . ?
C22 C21 H21 119.2 . . ?
C21 C22 H22 121.6 . . ?
C23 C22 C21 116.7(4) . . ?
C23 C22 H22 121.6 . . ?
N18 C23 C22 122.9(4) . . ?
N18 C23 N29 111.3(3) . . ?
C22 C23 N29 125.8(4) . . ?
N25 N24 C19 117.3(3) . . ?
C28 N24 C19 131.2(4) . . ?
C28 N24 N25 111.3(3) . . ?
N24 N25 Fe1 112.2(2) . . ?
N24 N25 Ni1 112.2(2) . . ?
C26 N25 Fe1 142.6(3) . . ?
C26 N25 Ni1 142.6(3) . . ?
C26 N25 N24 104.9(3) . . ?
N25 C26 H26 124.6 . . ?
N25 C26 C27 110.8(4) . . ?
C27 C26 H26 124.6 . . ?
C26 C27 H27 126.9 . . ?
C28 C27 C26 106.2(4) . . ?
C28 C27 H27 126.9 . . ?
N24 C28 C27 106.8(4) . . ?
N24 C28 H28 126.6 . . ?
C27 C28 H28 126.6 . . ?
N30 N29 C23 117.5(3) . . ?
C33 N29 C23 131.4(4) . . ?
C33 N29 N30 111.0(3) . . ?
N29 N30 Fe1 112.5(2) . . ?
N29 N30 Ni1 112.5(2) . . ?
C31 N30 Fe1 142.5(3) . . ?
C31 N30 Ni1 142.5(3) . . ?
C31 N30 N29 105.0(3) . . ?
N30 C31 H31 124.3 . . ?
N30 C31 C32 111.5(4) . . ?
C32 C31 H31 124.3 . . ?
C31 C32 H32 127.2 . . ?
C33 C32 C31 105.6(4) . . ?
C33 C32 H32 127.2 . . ?
N29 C33 C32 107.0(4) . . ?
N29 C33 H33 126.5 . . ?
C32 C33 H33 126.5 . . ?
O36 Cl34 O35 109.84(19) . . ?
O36 Cl34 O37 108.6(2) . . ?
O36 Cl34 O38 110.20(19) . . ?
O37 Cl34 O35 109.4(2) . . ?
O38 Cl34 O35 109.9(2) . . ?
O38 Cl34 O37 108.83(19) . . ?
O41 Cl39 O40 109.7(2) . . ?
O42 Cl39 O40 108.77(19) . . ?
O42 Cl39 O41 108.4(2) . . ?
O43 Cl39 O40 109.0(2) . . ?
O43 Cl39 O41 109.1(2) . . ?
O43 Cl39 O42 111.8(3) . . ?

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 N2 C3 C4 -179.2(3) . . . . ?
Fe1 N2 C3 N8 0.2(4) . . . . ?
Fe1 N2 C7 C6 179.9(3) . . . . ?
Fe1 N2 C7 N13 0.4(4) . . . . ?
Fe1 N9 C10 C11 -179.5(3) . . . . ?
Fe1 N14 C15 C16 170.1(3) . . . . ?
Fe1 N18 C19 C20 -178.9(3) . . . . ?
Fe1 N18 C19 N24 -0.1(4) . . . . ?
Fe1 N18 C23 C22 178.4(3) . . . . ?
Fe1 N18 C23 N29 -1.6(4) . . . . ?
Fe1 N25 C26 C27 -172.9(4) . . . . ?
Fe1 N30 C31 C32 177.2(3) . . . . ?
Ni1 N2 C3 C4 -179.2(3) . . . . ?
Ni1 N2 C3 N8 0.2(4) . . . . ?
Ni1 N2 C7 C6 179.9(3) . . . . ?
Ni1 N2 C7 N13 0.4(4) . . . . ?
Ni1 N9 C10 C11 -179.5(3) . . . . ?
Ni1 N14 C15 C16 170.1(3) . . . . ?
Ni1 N18 C19 C20 -178.9(3) . . . . ?
Ni1 N18 C19 N24 -0.1(4) . . . . ?
Ni1 N18 C23 C22 178.4(3) . . . . ?
Ni1 N18 C23 N29 -1.6(4) . . . . ?
Ni1 N25 C26 C27 -172.9(4) . . . . ?
Ni1 N30 C31 C32 177.2(3) . . . . ?
N2 C3 C4 C5 -0.1(6) . . . . ?
N2 C3 N8 N9 -0.8(5) . . . . ?
N2 C3 N8 C12 -179.4(4) . . . . ?
N2 C7 N13 N14 -2.6(5) . . . . ?
N2 C7 N13 C17 173.2(4) . . . . ?
C3 N2 C7 C6 1.7(6) . . . . ?
C3 N2 C7 N13 -177.8(3) . . . . ?
C3 C4 C5 C6 0.3(6) . . . . ?
C3 N8 N9 Fe1 1.1(4) . . . . ?
C3 N8 N9 Ni1 1.1(4) . . . . ?
C3 N8 N9 C10 -178.6(3) . . . . ?
C3 N8 C12 C11 178.3(4) . . . . ?
C4 C3 N8 N9 178.5(3) . . . . ?
C4 C3 N8 C12 -0.1(7) . . . . ?
C4 C5 C6 C7 0.3(6) . . . . ?
C5 C6 C7 N2 -1.4(6) . . . . ?
C5 C6 C7 N13 178.1(4) . . . . ?
C6 C7 N13 N14 177.9(3) . . . . ?
C6 C7 N13 C17 -6.3(7) . . . . ?
C7 N2 C3 C4 -0.9(6) . . . . ?
C7 N2 C3 N8 178.4(3) . . . . ?
C7 N13 N14 Fe1 3.5(4) . . . . ?
C7 N13 N14 Ni1 3.5(4) . . . . ?
C7 N13 N14 C15 177.2(3) . . . . ?
C7 N13 C17 C16 -176.4(4) . . . . ?
N8 C3 C4 C5 -179.3(4) . . . . ?
N8 N9 C10 C11 0.0(4) . . . . ?
N9 N8 C12 C11 -0.4(4) . . . . ?
N9 C10 C11 C12 -0.2(5) . . . . ?
C10 C11 C12 N8 0.3(5) . . . . ?
C12 N8 N9 Fe1 179.9(3) . . . . ?
C12 N8 N9 Ni1 179.9(3) . . . . ?
C12 N8 N9 C10 0.2(4) . . . . ?
N13 N14 C15 C16 -0.5(5) . . . . ?
N14 N13 C17 C16 -0.4(5) . . . . ?
N14 C15 C16 C17 0.3(5) . . . . ?
C15 C16 C17 N13 0.1(5) . . . . ?
C17 N13 N14 Fe1 -173.1(3) . . . . ?
C17 N13 N14 Ni1 -173.1(3) . . . . ?
C17 N13 N14 C15 0.6(4) . . . . ?
N18 C19 C20 C21 0.4(6) . . . . ?
N18 C19 N24 N25 0.8(5) . . . . ?
N18 C19 N24 C28 -174.7(4) . . . . ?
N18 C23 N29 N30 2.3(5) . . . . ?
N18 C23 N29 C33 177.7(4) . . . . ?
C19 N18 C23 C22 0.8(6) . . . . ?
C19 N18 C23 N29 -179.2(3) . . . . ?
C19 C20 C21 C22 1.0(6) . . . . ?
C19 N24 N25 Fe1 -1.0(4) . . . . ?
C19 N24 N25 Ni1 -1.0(4) . . . . ?
C19 N24 N25 C26 -176.5(3) . . . . ?
C19 N24 C28 C27 175.7(4) . . . . ?
C20 C19 N24 N25 179.4(4) . . . . ?
C20 C19 N24 C28 3.9(7) . . . . ?
C20 C21 C22 C23 -1.4(6) . . . . ?
C21 C22 C23 N18 0.5(6) . . . . ?
C21 C22 C23 N29 -179.5(4) . . . . ?
C22 C23 N29 N30 -177.6(4) . . . . ?
C22 C23 N29 C33 -2.3(7) . . . . ?
C23 N18 C19 C20 -1.3(6) . . . . ?
C23 N18 C19 N24 177.5(3) . . . . ?
C23 N29 N30 Fe1 -2.0(4) . . . . ?
C23 N29 N30 Ni1 -2.0(4) . . . . ?
C23 N29 N30 C31 175.6(3) . . . . ?
C23 N29 C33 C32 -175.3(4) . . . . ?
N24 C19 C20 C21 -178.1(4) . . . . ?
N24 N25 C26 C27 0.3(5) . . . . ?
N25 N24 C28 C27 0.0(5) . . . . ?
N25 C26 C27 C28 -0.3(5) . . . . ?
C26 C27 C28 N24 0.2(5) . . . . ?
C28 N24 N25 Fe1 175.4(3) . . . . ?
C28 N24 N25 Ni1 175.4(3) . . . . ?
C28 N24 N25 C26 -0.2(4) . . . . ?
N29 N30 C31 C32 0.8(5) . . . . ?
N30 N29 C33 C32 0.3(4) . . . . ?
N30 C31 C32 C33 -0.7(5) . . . . ?
C31 C32 C33 N29 0.2(5) . . . . ?
C33 N29 N30 Fe1 -178.3(3) . . . . ?
C33 N29 N30 Ni1 -178.3(3) . . . . ?
C33 N29 N30 C31 -0.7(4) . . . . ?

_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 1.723
_oxdiff_exptl_absorpt_empirical_full_min 0.665
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_mh723
_database_code_depnum_ccdc_archive 'CCDC 2332661'
loop_
_audit_author_name
_audit_author_address
'Malcolm Halcrow'
;University of Leeds
United Kingdom
;
_audit_update_record             
;
2024-02-13 deposited with the CCDC.	2024-03-26 downloaded from the CCDC.
;
_audit_creation_date             2024-01-31
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_shelx_SHELXL_version_number     2018/3

_chemical_name_common            ?
_chemical_name_systematic        
'Bis[2,6-di(pyrazol-1-yl)pyridine]iron(II) bis[2,6-di(pyrazol-1-yl)pyridine]-nickel(II) ditetrafluoroborate 0.76:0.24 solid solution'
_chemical_formula_moiety         'C22 H18 Fe0.76 N10 Ni0.24, 2(Cl O4)'
_chemical_formula_sum            'C22 H18 Cl2 Fe0.76 N10 Ni0.24 O8'
_chemical_formula_weight         677.90
_chemical_absolute_configuration ab
_chemical_melting_point          ?
_chemical_oxdiff_formula         C22H18Cl2Fe0.73N10Ni0.27O8
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'
Cl Cl 0.1484 0.1585 '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'
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'

_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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.4873(5)
_cell_length_b                   8.5486(5)
_cell_length_c                   18.6946(10)
_cell_angle_alpha                90
_cell_angle_beta                 98.424(5)
_cell_angle_gamma                90
_cell_volume                     1341.74(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5286
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.2810
_cell_measurement_theta_min      2.1770
_exptl_absorpt_coefficient_mu    0.868
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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            brown
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       lath
_exptl_crystal_F_000             689
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -1 -26 0.0206
-2 1 26 0.0206
12 -2 -1 0.0586
-12 2 1 0.0586
0 -12 7 0.0197
0 12 -7 0.0197

_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.051
_exptl_crystal_size_min          0.039
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
1.5380 -0.6663 -26.3052 -0.7418 0.1052 -0.6623
-1.5380 0.6663 26.3052 0.7418 -0.1052 0.6623
11.6885 -2.4158 -1.4755 -0.6892 0.1096 0.7163
-11.6885 2.4158 1.4755 0.6892 -0.1096 -0.7163
0.0824 -11.6069 6.9266 0.1437 0.9412 0.3058
-0.0824 11.6069 -6.9266 -0.1437 -0.9412 -0.3058

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10773
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.758
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.736
_diffrn_reflns_theta_min         2.203
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -77.00   8.00   1.00   30.00    --   -9.84 -52.00 165.00   85
  2  ω    -31.00  28.00   1.00   30.00    --   -9.84  52.00 -49.00   59
  3  ω    -13.00  29.00   1.00   30.00    --    9.45 -99.00  60.00   42
  4  ω    -42.00 -16.00   1.00   30.00    --    9.45 -77.00   0.00   26
  5  ω    -36.00  20.00   1.00   30.00    --   -9.84  77.00   0.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0553844000
_diffrn_orient_matrix_UB_12      0.0020910000
_diffrn_orient_matrix_UB_13      0.0249103000
_diffrn_orient_matrix_UB_21      -0.0079886000
_diffrn_orient_matrix_UB_22      -0.0825646000
_diffrn_orient_matrix_UB_23      -0.0023760000
_diffrn_orient_matrix_UB_31      0.0631872000
_diffrn_orient_matrix_UB_32      -0.0085358000
_diffrn_orient_matrix_UB_33      0.0290868000
_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         0.655
_reflns_Friedel_fraction_full    0.839
_reflns_Friedel_fraction_max     0.640
_reflns_number_gt                5420
_reflns_number_total             5799
_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 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'XSEED (Barbour, 2020)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-TL (Sheldrick, 2015)'
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 
;
 Flack x determined using 1895 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0487
_refine_ls_restrained_S_all      1.111
_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)+(0.0145P)²+2.1932P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0931
_refine_special_details          
;
 The dataset was treated as a single, averaged [FeₓNi₁₋ₓ(bpp)₂]2+ 
 cation site. Partial Fe and Ni atoms were refined with the same cartesian 
 coordinates. The metal composition x refined to 0.76(3) when the partial
 metal sites were constrained to have the same isotropic thermal parameter,
 so this occupancy was used in the final least squares cycles. No anion 
 disorder is included in the model. However, an EADP thermal parameter 
 constraint between the two partial metal atoms was required to make the 
 model converge.

 All non-H atoms were refined anisotropically, and H atoms were placed in 
 calculated positions and refined using a riding model. 
;

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(Ni1)
3. Others
 X(Fe1)=X(Ni1)=FVAR(1)
 Y(Fe1)=Y(Ni1)=FVAR(2)
 Z(Fe1)=Z(Ni1)=FVAR(3)
 Fixed Sof: Fe1(0.76) Ni1(0.24)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C33(H33)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.78589(8) 0.75146(8) 0.75344(3) 0.01029(15) Uani 0.76 1 d . . P A 1
Ni1 Ni 0.78589(8) 0.75146(8) 0.75344(3) 0.01029(15) Uani 0.24 1 d . . P A 2
N2 N 0.7919(5) 0.7716(5) 0.8572(2) 0.0122(9) Uani 1 1 d . . . . .
C3 C 0.9185(6) 0.8321(6) 0.8979(3) 0.0134(11) Uani 1 1 d . . . . .
C4 C 0.9288(7) 0.8467(6) 0.9718(3) 0.0168(11) Uani 1 1 d . . . . .
H4 H 1.019976 0.890445 1.000280 0.020 Uiso 1 1 calc R U . . .
C5 C 0.7978(7) 0.7937(6) 1.0028(3) 0.0166(12) Uani 1 1 d . . . . .
H5 H 0.800503 0.800941 1.053671 0.020 Uiso 1 1 calc R U . . .
C6 C 0.6650(6) 0.7314(7) 0.9611(2) 0.0170(11) Uani 1 1 d . . . . .
H6 H 0.575333 0.697773 0.982060 0.020 Uiso 1 1 calc R U . . .
C7 C 0.6683(6) 0.7201(6) 0.8877(2) 0.0131(11) Uani 1 1 d . . . . .
N8 N 1.0351(5) 0.8751(5) 0.8557(2) 0.0152(9) Uani 1 1 d . . . . .
N9 N 1.0037(5) 0.8471(5) 0.7825(2) 0.0147(9) Uani 1 1 d . . . . .
C10 C 1.1327(7) 0.8938(7) 0.7567(3) 0.0179(12) Uani 1 1 d . . . . .
H10 H 1.145987 0.888914 0.707145 0.021 Uiso 1 1 calc R U . . .
C11 C 1.2475(7) 0.9515(7) 0.8121(3) 0.0207(12) Uani 1 1 d . . . . .
H11 H 1.349790 0.991655 0.807270 0.025 Uiso 1 1 calc R U . . .
C12 C 1.1824(7) 0.9383(7) 0.8743(3) 0.0188(12) Uani 1 1 d . . . . .
H12 H 1.230608 0.967518 0.921531 0.023 Uiso 1 1 calc R U . . .
N13 N 0.5492(5) 0.6557(5) 0.8364(2) 0.0142(9) Uani 1 1 d . . . . .
N14 N 0.5739(5) 0.6616(5) 0.7648(2) 0.0156(10) Uani 1 1 d . . . . .
C15 C 0.4491(7) 0.5896(7) 0.7280(3) 0.0215(13) Uani 1 1 d . . . . .
H15 H 0.432395 0.575412 0.677092 0.026 Uiso 1 1 calc R U . . .
C16 C 0.3447(7) 0.5368(7) 0.7750(3) 0.0250(14) Uani 1 1 d . . . . .
H16 H 0.247262 0.482048 0.762116 0.030 Uiso 1 1 calc R U . . .
C17 C 0.4122(7) 0.5806(7) 0.8426(3) 0.0216(13) Uani 1 1 d . . . . .
H17 H 0.370391 0.561740 0.886268 0.026 Uiso 1 1 calc R U . . .
N18 N 0.7802(5) 0.7219(5) 0.6504(2) 0.0131(9) Uani 1 1 d . . . . .
C19 C 0.7200(6) 0.8325(7) 0.6043(3) 0.0157(11) Uani 1 1 d . . . . .
C20 C 0.7103(6) 0.8151(7) 0.5294(3) 0.0162(11) Uani 1 1 d . . . . .
H20 H 0.667886 0.895008 0.496836 0.019 Uiso 1 1 calc R U . . .
C21 C 0.7658(6) 0.6755(7) 0.5052(3) 0.0191(12) Uani 1 1 d . . . . .
H21 H 0.762857 0.659941 0.454718 0.023 Uiso 1 1 calc R U . . .
C22 C 0.8259(6) 0.5566(7) 0.5529(3) 0.0170(12) Uani 1 1 d . . . . .
H22 H 0.861660 0.459945 0.536005 0.020 Uiso 1 1 calc R U . . .
C23 C 0.8307(6) 0.5866(6) 0.6252(3) 0.0149(11) Uani 1 1 d . . . . .
N24 N 0.6672(5) 0.9611(5) 0.6399(2) 0.0156(10) Uani 1 1 d . . . . .
N25 N 0.6859(5) 0.9544(6) 0.7144(2) 0.0151(9) Uani 1 1 d . . . . .
C26 C 0.6191(7) 1.0843(7) 0.7346(3) 0.0213(13) Uani 1 1 d . . . . .
H26 H 0.614049 1.112357 0.783414 0.026 Uiso 1 1 calc R U . . .
C27 C 0.5571(7) 1.1749(7) 0.6746(3) 0.0238(13) Uani 1 1 d . . . . .
H27 H 0.503170 1.272189 0.674821 0.029 Uiso 1 1 calc R U . . .
C28 C 0.5908(7) 1.0931(7) 0.6149(3) 0.0199(12) Uani 1 1 d . . . . .
H28 H 0.565109 1.123761 0.565722 0.024 Uiso 1 1 calc R U . . .
N29 N 0.8881(5) 0.4854(5) 0.6824(2) 0.0157(10) Uani 1 1 d . . . . .
N30 N 0.8765(5) 0.5350(5) 0.7515(2) 0.0149(10) Uani 1 1 d . . . . .
C31 C 0.9258(7) 0.4151(7) 0.7931(3) 0.0215(13) Uani 1 1 d . . . . .
H31 H 0.930152 0.414837 0.844206 0.026 Uiso 1 1 calc R U . . .
C32 C 0.9708(7) 0.2893(7) 0.7537(3) 0.0254(14) Uani 1 1 d . . . . .
H32 H 1.010723 0.191047 0.771937 0.030 Uiso 1 1 calc R U . . .
C33 C 0.9451(7) 0.3373(6) 0.6827(3) 0.0194(12) Uani 1 1 d . . . . .
H33 H 0.963808 0.277960 0.641798 0.023 Uiso 1 1 calc R U . . .
Cl34 Cl 0.30405(16) 0.71730(14) 1.06299(6) 0.0179(3) Uani 1 1 d . . . . .
O35 O 0.4589(5) 0.6642(6) 1.0969(2) 0.0378(13) Uani 1 1 d . . . . .
O36 O 0.1823(5) 0.6633(5) 1.10305(19) 0.0222(9) Uani 1 1 d . . . . .
O37 O 0.3002(6) 0.8867(5) 1.0615(2) 0.0286(10) Uani 1 1 d . . . . .
O38 O 0.2740(5) 0.6606(5) 0.98961(19) 0.0269(10) Uani 1 1 d . . . . .
Cl39 Cl 0.78581(17) 0.18443(17) 0.44414(7) 0.0209(3) Uani 1 1 d . . . . .
O40 O 0.8645(5) 0.1674(5) 0.51793(19) 0.0226(9) Uani 1 1 d . . . . .
O41 O 0.8180(5) 0.0507(5) 0.4023(2) 0.0291(10) Uani 1 1 d . . . . .
O42 O 0.6167(5) 0.1937(7) 0.4446(2) 0.0394(13) Uani 1 1 d . . . . .
O43 O 0.8457(7) 0.3219(6) 0.4132(2) 0.0461(14) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.940(4) . ?
Fe1 N9 2.022(5) . ?
Fe1 N14 1.996(5) . ?
Fe1 N18 1.936(4) . ?
Fe1 N25 2.019(5) . ?
Fe1 N30 2.007(5) . ?
Ni1 N2 1.940(4) . ?
Ni1 N9 2.022(5) . ?
Ni1 N14 1.996(5) . ?
Ni1 N18 1.936(4) . ?
Ni1 N25 2.019(5) . ?
Ni1 N30 2.007(5) . ?
N2 C3 1.327(7) . ?
N2 C7 1.340(6) . ?
C3 C4 1.376(7) . ?
C3 N8 1.403(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.402(8) . ?
C5 H5 0.9500 . ?
C5 C6 1.379(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.382(6) . ?
C7 N13 1.400(6) . ?
N8 N9 1.375(6) . ?
N8 C12 1.360(7) . ?
N9 C10 1.321(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.404(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.363(8) . ?
C12 H12 0.9500 . ?
N13 N14 1.385(6) . ?
N13 C17 1.348(7) . ?
N14 C15 1.327(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.410(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.362(8) . ?
C17 H17 0.9500 . ?
N18 C19 1.331(7) . ?
N18 C23 1.343(7) . ?
C19 C20 1.398(7) . ?
C19 N24 1.393(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.383(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.398(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.371(7) . ?
C23 N29 1.405(7) . ?
N24 N25 1.380(6) . ?
N24 C28 1.351(7) . ?
N25 C26 1.327(7) . ?
C26 H26 0.9500 . ?
C26 C27 1.401(8) . ?
C27 H27 0.9500 . ?
C27 C28 1.381(8) . ?
C28 H28 0.9500 . ?
N29 N30 1.377(6) . ?
N29 C33 1.355(7) . ?
N30 C31 1.318(7) . ?
C31 H31 0.9500 . ?
C31 C32 1.388(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.376(8) . ?
C33 H33 0.9500 . ?
Cl34 O35 1.446(4) . ?
Cl34 O36 1.438(4) . ?
Cl34 O37 1.449(4) . ?
Cl34 O38 1.442(4) . ?
Cl39 O40 1.449(4) . ?
Cl39 O41 1.434(4) . ?
Cl39 O42 1.439(4) . ?
Cl39 O43 1.436(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N9 78.82(17) . . ?
N2 Fe1 N14 79.64(17) . . ?
N2 Fe1 N25 103.46(18) . . ?
N2 Fe1 N30 98.39(18) . . ?
N14 Fe1 N9 158.45(16) . . ?
N14 Fe1 N25 91.79(19) . . ?
N14 Fe1 N30 90.05(19) . . ?
N18 Fe1 N2 177.6(2) . . ?
N18 Fe1 N9 102.07(18) . . ?
N18 Fe1 N14 99.43(17) . . ?
N18 Fe1 N25 78.76(18) . . ?
N18 Fe1 N30 79.36(18) . . ?
N25 Fe1 N9 93.95(19) . . ?
N30 Fe1 N9 92.30(19) . . ?
N30 Fe1 N25 158.04(17) . . ?
N2 Ni1 N9 78.82(17) . . ?
N2 Ni1 N14 79.64(17) . . ?
N2 Ni1 N25 103.46(18) . . ?
N2 Ni1 N30 98.39(18) . . ?
N14 Ni1 N9 158.45(16) . . ?
N14 Ni1 N25 91.79(19) . . ?
N14 Ni1 N30 90.05(19) . . ?
N18 Ni1 N2 177.6(2) . . ?
N18 Ni1 N9 102.07(18) . . ?
N18 Ni1 N14 99.43(17) . . ?
N18 Ni1 N25 78.76(18) . . ?
N18 Ni1 N30 79.36(18) . . ?
N25 Ni1 N9 93.95(19) . . ?
N30 Ni1 N9 92.30(19) . . ?
N30 Ni1 N25 158.04(17) . . ?
C3 N2 Fe1 120.6(3) . . ?
C3 N2 Ni1 120.6(3) . . ?
C3 N2 C7 120.2(4) . . ?
C7 N2 Fe1 119.2(3) . . ?
C7 N2 Ni1 119.2(3) . . ?
N2 C3 C4 122.5(5) . . ?
N2 C3 N8 110.9(4) . . ?
C4 C3 N8 126.5(5) . . ?
C3 C4 H4 121.7 . . ?
C3 C4 C5 116.6(5) . . ?
C5 C4 H4 121.7 . . ?
C4 C5 H5 119.2 . . ?
C6 C5 C4 121.5(5) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 H6 121.5 . . ?
C5 C6 C7 117.0(5) . . ?
C7 C6 H6 121.5 . . ?
N2 C7 C6 122.1(5) . . ?
N2 C7 N13 111.7(4) . . ?
C6 C7 N13 126.2(5) . . ?
N9 N8 C3 117.7(4) . . ?
C12 N8 C3 131.1(5) . . ?
C12 N8 N9 111.2(4) . . ?
N8 N9 Fe1 112.0(3) . . ?
N8 N9 Ni1 112.0(3) . . ?
C10 N9 Fe1 142.9(4) . . ?
C10 N9 Ni1 142.9(4) . . ?
C10 N9 N8 105.1(4) . . ?
N9 C10 H10 124.5 . . ?
N9 C10 C11 111.0(5) . . ?
C11 C10 H10 124.5 . . ?
C10 C11 H11 127.0 . . ?
C12 C11 C10 106.0(5) . . ?
C12 C11 H11 127.0 . . ?
N8 C12 C11 106.6(5) . . ?
N8 C12 H12 126.7 . . ?
C11 C12 H12 126.7 . . ?
N14 N13 C7 116.8(4) . . ?
C17 N13 C7 132.3(5) . . ?
C17 N13 N14 110.9(4) . . ?
N13 N14 Fe1 112.5(3) . . ?
N13 N14 Ni1 112.5(3) . . ?
C15 N14 Fe1 142.0(4) . . ?
C15 N14 Ni1 142.0(4) . . ?
C15 N14 N13 105.1(5) . . ?
N14 C15 H15 124.6 . . ?
N14 C15 C16 110.7(5) . . ?
C16 C15 H15 124.6 . . ?
C15 C16 H16 127.1 . . ?
C17 C16 C15 105.8(5) . . ?
C17 C16 H16 127.1 . . ?
N13 C17 C16 107.5(5) . . ?
N13 C17 H17 126.2 . . ?
C16 C17 H17 126.2 . . ?
C19 N18 Fe1 120.2(4) . . ?
C19 N18 Ni1 120.2(4) . . ?
C19 N18 C23 119.8(4) . . ?
C23 N18 Fe1 119.9(4) . . ?
C23 N18 Ni1 119.9(4) . . ?
N18 C19 C20 122.3(5) . . ?
N18 C19 N24 111.7(4) . . ?
N24 C19 C20 126.0(5) . . ?
C19 C20 H20 121.7 . . ?
C21 C20 C19 116.5(5) . . ?
C21 C20 H20 121.7 . . ?
C20 C21 H21 119.0 . . ?
C20 C21 C22 121.9(5) . . ?
C22 C21 H21 119.0 . . ?
C21 C22 H22 121.7 . . ?
C23 C22 C21 116.6(5) . . ?
C23 C22 H22 121.7 . . ?
N18 C23 C22 122.8(5) . . ?
N18 C23 N29 110.9(4) . . ?
C22 C23 N29 126.3(5) . . ?
N25 N24 C19 116.9(4) . . ?
C28 N24 C19 131.7(5) . . ?
C28 N24 N25 111.3(4) . . ?
N24 N25 Fe1 112.4(3) . . ?
N24 N25 Ni1 112.4(3) . . ?
C26 N25 Fe1 142.3(4) . . ?
C26 N25 Ni1 142.3(4) . . ?
C26 N25 N24 105.1(5) . . ?
N25 C26 H26 124.4 . . ?
N25 C26 C27 111.1(5) . . ?
C27 C26 H26 124.4 . . ?
C26 C27 H27 127.2 . . ?
C28 C27 C26 105.7(5) . . ?
C28 C27 H27 127.2 . . ?
N24 C28 C27 106.8(5) . . ?
N24 C28 H28 126.6 . . ?
C27 C28 H28 126.6 . . ?
N30 N29 C23 117.3(4) . . ?
C33 N29 C23 131.5(5) . . ?
C33 N29 N30 110.9(4) . . ?
N29 N30 Fe1 112.4(3) . . ?
N29 N30 Ni1 112.4(3) . . ?
C31 N30 Fe1 142.7(4) . . ?
C31 N30 Ni1 142.7(4) . . ?
C31 N30 N29 104.8(5) . . ?
N30 C31 H31 123.9 . . ?
N30 C31 C32 112.1(5) . . ?
C32 C31 H31 123.9 . . ?
C31 C32 H32 127.3 . . ?
C33 C32 C31 105.3(5) . . ?
C33 C32 H32 127.3 . . ?
N29 C33 C32 106.8(5) . . ?
N29 C33 H33 126.6 . . ?
C32 C33 H33 126.6 . . ?
O35 Cl34 O37 109.8(3) . . ?
O36 Cl34 O35 110.3(2) . . ?
O36 Cl34 O37 108.4(3) . . ?
O36 Cl34 O38 110.3(2) . . ?
O38 Cl34 O35 109.6(3) . . ?
O38 Cl34 O37 108.5(3) . . ?
O41 Cl39 O40 110.0(3) . . ?
O41 Cl39 O42 108.5(3) . . ?
O41 Cl39 O43 109.0(3) . . ?
O42 Cl39 O40 108.7(2) . . ?
O43 Cl39 O40 109.0(3) . . ?
O43 Cl39 O42 111.7(3) . . ?

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 N2 C3 C4 -179.1(4) . . . . ?
Fe1 N2 C3 N8 0.2(6) . . . . ?
Fe1 N2 C7 C6 -179.8(4) . . . . ?
Fe1 N2 C7 N13 0.5(6) . . . . ?
Fe1 N9 C10 C11 -179.3(5) . . . . ?
Fe1 N14 C15 C16 171.2(5) . . . . ?
Fe1 N18 C19 C20 -178.6(4) . . . . ?
Fe1 N18 C19 N24 0.0(6) . . . . ?
Fe1 N18 C23 C22 178.2(4) . . . . ?
Fe1 N18 C23 N29 -2.2(6) . . . . ?
Fe1 N25 C26 C27 -173.4(5) . . . . ?
Fe1 N30 C31 C32 177.1(5) . . . . ?
Ni1 N2 C3 C4 -179.1(4) . . . . ?
Ni1 N2 C3 N8 0.2(6) . . . . ?
Ni1 N2 C7 C6 -179.8(4) . . . . ?
Ni1 N2 C7 N13 0.5(6) . . . . ?
Ni1 N9 C10 C11 -179.3(5) . . . . ?
Ni1 N14 C15 C16 171.2(5) . . . . ?
Ni1 N18 C19 C20 -178.6(4) . . . . ?
Ni1 N18 C19 N24 0.0(6) . . . . ?
Ni1 N18 C23 C22 178.2(4) . . . . ?
Ni1 N18 C23 N29 -2.2(6) . . . . ?
Ni1 N25 C26 C27 -173.4(5) . . . . ?
Ni1 N30 C31 C32 177.1(5) . . . . ?
N2 C3 C4 C5 0.1(8) . . . . ?
N2 C3 N8 N9 -1.0(7) . . . . ?
N2 C3 N8 C12 -178.9(5) . . . . ?
N2 C7 N13 N14 -2.8(6) . . . . ?
N2 C7 N13 C17 174.3(6) . . . . ?
C3 N2 C7 C6 1.8(8) . . . . ?
C3 N2 C7 N13 -177.9(5) . . . . ?
C3 C4 C5 C6 -0.5(8) . . . . ?
C3 N8 N9 Fe1 1.3(6) . . . . ?
C3 N8 N9 Ni1 1.3(6) . . . . ?
C3 N8 N9 C10 -178.3(5) . . . . ?
C3 N8 C12 C11 178.0(5) . . . . ?
C4 C3 N8 N9 178.3(5) . . . . ?
C4 C3 N8 C12 0.5(9) . . . . ?
C4 C5 C6 C7 1.5(8) . . . . ?
C5 C6 C7 N2 -2.1(8) . . . . ?
C5 C6 C7 N13 177.6(5) . . . . ?
C6 C7 N13 N14 177.5(5) . . . . ?
C6 C7 N13 C17 -5.4(9) . . . . ?
C7 N2 C3 C4 -0.8(8) . . . . ?
C7 N2 C3 N8 178.6(5) . . . . ?
C7 N13 N14 Fe1 3.7(5) . . . . ?
C7 N13 N14 Ni1 3.7(5) . . . . ?
C7 N13 N14 C15 177.9(4) . . . . ?
C7 N13 C17 C16 -177.4(5) . . . . ?
N8 C3 C4 C5 -179.1(5) . . . . ?
N8 N9 C10 C11 0.1(6) . . . . ?
N9 N8 C12 C11 0.0(6) . . . . ?
N9 C10 C11 C12 -0.1(7) . . . . ?
C10 C11 C12 N8 0.0(6) . . . . ?
C12 N8 N9 Fe1 179.6(4) . . . . ?
C12 N8 N9 Ni1 179.6(4) . . . . ?
C12 N8 N9 C10 0.0(6) . . . . ?
N13 N14 C15 C16 -0.2(6) . . . . ?
N14 N13 C17 C16 -0.3(6) . . . . ?
N14 C15 C16 C17 0.0(7) . . . . ?
C15 C16 C17 N13 0.1(7) . . . . ?
C17 N13 N14 Fe1 -174.0(4) . . . . ?
C17 N13 N14 Ni1 -174.0(4) . . . . ?
C17 N13 N14 C15 0.3(6) . . . . ?
N18 C19 C20 C21 0.4(8) . . . . ?
N18 C19 N24 N25 0.5(7) . . . . ?
N18 C19 N24 C28 -175.4(5) . . . . ?
N18 C23 N29 N30 3.1(7) . . . . ?
N18 C23 N29 C33 177.6(5) . . . . ?
C19 N18 C23 C22 1.0(8) . . . . ?
C19 N18 C23 N29 -179.4(5) . . . . ?
C19 C20 C21 C22 1.1(8) . . . . ?
C19 N24 N25 Fe1 -0.8(6) . . . . ?
C19 N24 N25 Ni1 -0.8(6) . . . . ?
C19 N24 N25 C26 -176.6(5) . . . . ?
C19 N24 C28 C27 175.6(6) . . . . ?
C20 C19 N24 N25 179.1(5) . . . . ?
C20 C19 N24 C28 3.2(10) . . . . ?
C20 C21 C22 C23 -1.4(8) . . . . ?
C21 C22 C23 N18 0.4(8) . . . . ?
C21 C22 C23 N29 -179.1(5) . . . . ?
C22 C23 N29 N30 -177.3(5) . . . . ?
C22 C23 N29 C33 -2.9(9) . . . . ?
C23 N18 C19 C20 -1.5(8) . . . . ?
C23 N18 C19 N24 177.2(5) . . . . ?
C23 N29 N30 Fe1 -2.6(6) . . . . ?
C23 N29 N30 Ni1 -2.6(6) . . . . ?
C23 N29 N30 C31 175.1(5) . . . . ?
C23 N29 C33 C32 -174.6(5) . . . . ?
N24 C19 C20 C21 -178.0(5) . . . . ?
N24 N25 C26 C27 0.2(6) . . . . ?
N25 N24 C28 C27 -0.5(6) . . . . ?
N25 C26 C27 C28 -0.5(7) . . . . ?
C26 C27 C28 N24 0.6(6) . . . . ?
C28 N24 N25 Fe1 176.0(4) . . . . ?
C28 N24 N25 Ni1 176.0(4) . . . . ?
C28 N24 N25 C26 0.2(6) . . . . ?
N29 N30 C31 C32 0.6(6) . . . . ?
N30 N29 C33 C32 0.2(6) . . . . ?
N30 C31 C32 C33 -0.5(7) . . . . ?
C31 C32 C33 N29 0.2(6) . . . . ?
C33 N29 N30 Fe1 -178.2(4) . . . . ?
C33 N29 N30 Ni1 -178.2(4) . . . . ?
C33 N29 N30 C31 -0.4(6) . . . . ?

_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 1.280
_oxdiff_exptl_absorpt_empirical_full_min 0.820
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_preparation       'Magnetic properties'
