#------------------------------------------------------------------------------
#$Date: 2024-07-05 20:01:01 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293152 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/58/7715898.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7715898
loop_
_publ_author_name
'Visinescu, Diana'
'Shylin, Sergii I.'
'Shova, Sergiu'
'Novitchi, Ghenadie'
'Popescu, Delia-Laura'
'Alexandru, Maria-Gabriela'
_publ_section_title
;
 New cyanido-bridged iron(II) spin crossover coordination polymers with an
 unusual ladder-like topology: an alternative to Hofmann clathrates.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9062
_journal_page_last               9071
_journal_paper_doi               10.1039/d4dt00870g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C22 H12 Fe N10 Pd, C2 H3 N, 2(H2 O)'
_chemical_formula_sum            'C24 H19 Fe N11 O2 Pd'
_chemical_formula_weight         655.75
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-21 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                94.756(5)
_cell_angle_beta                 94.062(5)
_cell_angle_gamma                115.990(6)
_cell_formula_units_Z            2
_cell_length_a                   9.1702(6)
_cell_length_b                   10.3930(6)
_cell_length_c                   15.0356(10)
_cell_measurement_reflns_used    5183
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      29.7870
_cell_measurement_theta_min      2.4690
_cell_volume                     1274.41(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  74.00   0.50   10.00    --   11.27  63.00 171.00  166
  2  ω    -63.00  34.00   0.50   10.00    --   11.27 -63.00  35.00  194
  3  ω     -3.00  28.00   0.50   10.00    --  -11.03 -99.00-120.00   62
  4  ω    -42.00  56.00   0.50   10.00    --  -11.03  77.00-150.00  196
  5  ω    -22.00  26.00   0.50   10.00    --  -11.03 -99.00  90.00   96
  6  ω    -64.00   4.00   0.50   10.00    --   11.27 -19.00  60.00  136
  7  ω    -17.00  35.50   0.50   10.00    --   11.27 -99.00 -30.00  105
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0670834000
_diffrn_orient_matrix_UB_12      0.0697972000
_diffrn_orient_matrix_UB_13      0.0081127000
_diffrn_orient_matrix_UB_21      -0.0371675000
_diffrn_orient_matrix_UB_22      0.0232501000
_diffrn_orient_matrix_UB_23      -0.0339498000
_diffrn_orient_matrix_UB_31      -0.0403818000
_diffrn_orient_matrix_UB_32      0.0211496000
_diffrn_orient_matrix_UB_33      0.0324805000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7027
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.437
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense brown'
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       plate
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.942
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         7027
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0419
_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)+(0.0679P)²+3.4670P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6419
_reflns_number_total             7027
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by -179.9623° 
around [-0.00 0.00 1.00] (reciprocal) or [0.21 0.20 0.96] (direct)
;
_cod_data_source_file            d4dt00870g2.cif
_cod_data_source_block           shs_78_gaal_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7715897--7715901.cif.'
_cod_original_cell_volume        1274.41(15)
_cod_database_code               7715898
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H30N12FePd1
_chemical_oxdiff_usercomment     M2Pd(compusil1)
_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.
;
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.734
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4881(12)
 0.5119(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C23-C23X
 0.56 with sigma of 0.001
 C23X-C24 = C24-C23
 1.5 with sigma of 0.01
 C23X-C24 \\sim C24-C23
 with sigma of 0.01
 N11-C23 \\sim N11X-C23X
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(N11) = Uanis(N11X)
Uanis(C23) = Uanis(C23X)
5. Others
 Sof(N11)=Sof(C23)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(N11X)=Sof(C23X)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
6.a Riding coordinates:
 C24(H24A,H24B,H24C,H24D,H24E,H24F), O2W(H2WA,H2WB), O1W(H1WA,H1WB)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18)
;
_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 1.551
_oxdiff_exptl_absorpt_empirical_full_min 0.684
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.60829(5) 0.30917(4) 0.66428(3) 0.01955(14) Uani 1 1 d . . . . .
Fe1 Fe 0.39703(9) 0.18946(8) 0.32395(4) 0.01540(18) Uani 1 1 d . . . . .
N1 N 0.6223(6) 0.2773(5) 0.2605(4) 0.0316(12) Uani 1 1 d . . . . .
N2 N 0.3256(5) 0.1856(5) 0.1916(3) 0.0209(10) Uani 1 1 d . . . . .
N3 N 0.1334(6) 0.0990(5) 0.3126(3) 0.0273(11) Uani 1 1 d . . . . .
N4 N 0.3996(5) 0.2809(5) 0.0554(3) 0.0232(10) Uani 1 1 d . . . . .
N5 N 0.1206(5) 0.1797(5) 0.0855(3) 0.0222(10) Uani 1 1 d . . . . .
N6 N 0.0278(5) 0.2131(5) -0.0813(3) 0.0255(10) Uani 1 1 d . . . . .
N7 N 0.4735(6) 0.2230(5) 0.4588(3) 0.0248(11) Uani 1 1 d . . . . .
N8 N 0.5982(5) 0.6061(5) 0.6622(3) 0.0216(10) Uani 1 1 d . . . . .
N9 N 0.6145(5) 0.0120(5) 0.6792(3) 0.0219(10) Uani 1 1 d . . . . .
N10 N 0.7127(6) 0.3997(6) 0.8713(3) 0.0294(11) Uani 1 1 d . . . . .
C1 C 0.7744(8) 0.3163(7) 0.3000(6) 0.0451(18) Uani 1 1 d . U . . .
H1 H 0.792813 0.309362 0.361987 0.054 Uiso 1 1 calc R U . . .
C2 C 0.9087(8) 0.3686(7) 0.2474(6) 0.0499(19) Uani 1 1 d . U . . .
H2 H 1.015589 0.396681 0.276218 0.060 Uiso 1 1 calc R U . . .
C3 C 0.8906(8) 0.3796(8) 0.1595(6) 0.0484(18) Uani 1 1 d . U . . .
H3 H 0.981356 0.413637 0.125994 0.058 Uiso 1 1 calc R U . . .
C4 C 0.7346(7) 0.3394(6) 0.1202(5) 0.0346(15) Uani 1 1 d . U . . .
H4 H 0.714919 0.344831 0.058076 0.042 Uiso 1 1 calc R U . . .
C5 C 0.6060(6) 0.2907(6) 0.1720(4) 0.0262(13) Uani 1 1 d . . . . .
C6 C 0.4361(6) 0.2509(5) 0.1347(4) 0.0212(12) Uani 1 1 d . . . . .
C7 C 0.2391(6) 0.2405(6) 0.0326(4) 0.0220(12) Uani 1 1 d . . . . .
C8 C 0.1717(6) 0.1562(6) 0.1638(4) 0.0217(11) Uani 1 1 d . . . . .
C9 C 0.0582(6) 0.0974(6) 0.2317(4) 0.0234(12) Uani 1 1 d . . . . .
C10 C -0.1090(7) 0.0464(6) 0.2121(5) 0.0318(14) Uani 1 1 d . . . . .
H10 H -0.156622 0.046660 0.153999 0.038 Uiso 1 1 calc R U . . .
C11 C -0.2039(8) -0.0049(7) 0.2806(6) 0.0432(19) Uani 1 1 d . . . . .
H11 H -0.319010 -0.039935 0.270038 0.052 Uiso 1 1 calc R U . . .
C12 C -0.1320(9) -0.0053(7) 0.3635(6) 0.050(2) Uani 1 1 d . . . . .
H12 H -0.196727 -0.040510 0.410687 0.061 Uiso 1 1 calc R U . . .
C13 C 0.0370(9) 0.0465(7) 0.3778(5) 0.0416(17) Uani 1 1 d . . . . .
H13 H 0.086112 0.044863 0.435218 0.050 Uiso 1 1 calc R U . . .
C14 C 0.1900(7) 0.2641(6) -0.0584(4) 0.0231(12) Uani 1 1 d . . . . .
C15 C 0.3052(7) 0.3312(6) -0.1159(4) 0.0255(12) Uani 1 1 d . . . . .
H15 H 0.418653 0.367316 -0.097014 0.031 Uiso 1 1 calc R U . . .
C16 C 0.2507(7) 0.3441(6) -0.2010(4) 0.0289(13) Uani 1 1 d . . . . .
H16 H 0.326399 0.388570 -0.242003 0.035 Uiso 1 1 calc R U . . .
C17 C 0.0844(7) 0.2914(6) -0.2260(4) 0.0287(13) Uani 1 1 d . . . . .
H17 H 0.043686 0.298578 -0.284265 0.034 Uiso 1 1 calc R U . . .
C18 C -0.0219(7) 0.2273(6) -0.1629(4) 0.0275(13) Uani 1 1 d . . . . .
H18 H -0.135893 0.192082 -0.179693 0.033 Uiso 1 1 calc R U . . .
C19 C 0.5246(7) 0.2524(6) 0.5336(4) 0.0214(11) Uani 1 1 d . . . . .
C20 C 0.6025(6) 0.4976(6) 0.6602(4) 0.0200(11) Uani 1 1 d . . . . .
C21 C 0.6142(6) 0.1215(6) 0.6726(3) 0.0194(11) Uani 1 1 d . . . . .
C22 C 0.6793(6) 0.3672(6) 0.7949(4) 0.0228(12) Uani 1 1 d . . . . .
N11 N 1.0965(15) 0.746(3) 0.4822(15) 0.093(6) Uani 0.518(18) 1 d D . P A 2
N11X N 1.074(2) 0.638(3) 0.4794(16) 0.093(6) Uani 0.482(18) 1 d D . P A 1
C23 C 0.9594(11) 0.681(3) 0.471(3) 0.045(6) Uani 0.518(18) 1 d D . P A 2
C23X C 0.9489(15) 0.631(3) 0.474(4) 0.045(6) Uani 0.482(18) 1 d D . P A 1
C24 C 0.7808(8) 0.6089(9) 0.4588(5) 0.0504(19) Uani 1 1 d D . . . .
H24A H 0.765506 0.671536 0.505818 0.076 Uiso 0.482(18) 1 d R U P A 1
H24B H 0.707086 0.507876 0.463328 0.076 Uiso 0.482(18) 1 d R U P A 1
H24C H 0.756506 0.632896 0.399678 0.076 Uiso 0.482(18) 1 d R U P A 1
H24D H 0.737816 0.606816 0.516818 0.076 Uiso 0.518(18) 1 d R U P A 2
H24E H 0.743406 0.509936 0.429888 0.076 Uiso 0.518(18) 1 d R U P A 2
H24F H 0.741576 0.661416 0.420168 0.076 Uiso 0.518(18) 1 d R U P A 2
O2W O 0.4989(5) -0.0764(5) 0.1078(3) 0.0438(12) Uani 1 1 d . . . . .
H2WA H 0.589148 -0.043248 0.083052 0.066 Uiso 1 1 d R U . . .
H2WB H 0.470798 -0.168018 0.107262 0.066 Uiso 1 1 d R U . . .
O1W O 0.2610(5) -0.0424(4) 0.0031(3) 0.0351(10) Uani 1 1 d . . . . .
H1WA H 0.157894 -0.095104 0.006993 0.053 Uiso 1 1 d R U . . .
H1WB H 0.319374 -0.070464 0.037193 0.053 Uiso 1 1 d R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C20 Pd1 C19 90.6(2) . . ?
C20 Pd1 C21 178.2(2) . . ?
C21 Pd1 C19 91.1(2) . . ?
C22 Pd1 C19 176.5(2) . . ?
C22 Pd1 C20 87.5(2) . . ?
C22 Pd1 C21 90.8(2) . . ?
N2 Fe1 N1 74.40(18) . . ?
N2 Fe1 N3 74.98(18) . . ?
N2 Fe1 N7 171.88(18) . . ?
N2 Fe1 N8 83.98(18) . 2_666 ?
N2 Fe1 N9 99.88(18) . 2_656 ?
N3 Fe1 N1 149.4(2) . . ?
N7 Fe1 N1 104.7(2) . . ?
N7 Fe1 N3 105.63(19) . . ?
N7 Fe1 N8 87.95(19) . 2_666 ?
N8 Fe1 N1 89.81(17) 2_666 . ?
N8 Fe1 N3 87.30(17) 2_666 . ?
N9 Fe1 N1 93.95(18) 2_656 . ?
N9 Fe1 N3 90.96(18) 2_656 . ?
N9 Fe1 N7 88.22(18) 2_656 . ?
N9 Fe1 N8 175.21(17) 2_656 2_666 ?
C1 N1 Fe1 126.7(5) . . ?
C1 N1 C5 116.9(6) . . ?
C5 N1 Fe1 116.4(4) . . ?
C6 N2 Fe1 121.3(4) . . ?
C8 N2 Fe1 120.6(4) . . ?
C8 N2 C6 115.5(5) . . ?
C9 N3 Fe1 116.0(3) . . ?
C9 N3 C13 116.9(5) . . ?
C13 N3 Fe1 127.1(5) . . ?
C6 N4 C7 114.8(5) . . ?
C8 N5 C7 114.5(5) . . ?
C18 N6 C14 117.5(5) . . ?
C19 N7 Fe1 174.8(5) . . ?
C20 N8 Fe1 175.3(5) . 2_666 ?
C21 N9 Fe1 173.4(4) . 2_656 ?
N1 C1 H1 120.4 . . ?
N1 C1 C2 119.3(7) . . ?
C2 C1 H1 120.4 . . ?
C1 C2 H2 118.4 . . ?
C3 C2 C1 123.2(7) . . ?
C3 C2 H2 118.4 . . ?
C2 C3 H3 121.6 . . ?
C2 C3 C4 116.8(7) . . ?
C4 C3 H3 121.6 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.5(7) . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 124.3(6) . . ?
N1 C5 C6 113.5(5) . . ?
C4 C5 C6 122.2(6) . . ?
N2 C6 C5 113.1(5) . . ?
N4 C6 N2 124.5(5) . . ?
N4 C6 C5 122.5(5) . . ?
N4 C7 C14 117.0(5) . . ?
N5 C7 N4 125.2(5) . . ?
N5 C7 C14 117.7(5) . . ?
N2 C8 C9 113.5(5) . . ?
N5 C8 N2 125.3(5) . . ?
N5 C8 C9 121.2(5) . . ?
N3 C9 C8 113.8(5) . . ?
N3 C9 C10 124.3(5) . . ?
C10 C9 C8 121.9(6) . . ?
C9 C10 H10 121.3 . . ?
C11 C10 C9 117.3(7) . . ?
C11 C10 H10 121.3 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.1(6) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 120.4 . . ?
C11 C12 C13 119.3(6) . . ?
C13 C12 H12 120.4 . . ?
N3 C13 C12 122.1(7) . . ?
N3 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
N6 C14 C7 115.4(5) . . ?
N6 C14 C15 123.2(6) . . ?
C15 C14 C7 121.4(5) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 C14 118.4(5) . . ?
C16 C15 H15 120.8 . . ?
C15 C16 H16 120.4 . . ?
C15 C16 C17 119.2(5) . . ?
C17 C16 H16 120.4 . . ?
C16 C17 H17 120.9 . . ?
C16 C17 C18 118.1(6) . . ?
C18 C17 H17 120.9 . . ?
N6 C18 C17 123.5(5) . . ?
N6 C18 H18 118.2 . . ?
C17 C18 H18 118.2 . . ?
N7 C19 Pd1 177.4(5) . . ?
N8 C20 Pd1 176.6(5) . . ?
N9 C21 Pd1 178.0(5) . . ?
N10 C22 Pd1 176.5(5) . . ?
N11 C23 C24 175(3) . . ?
N11X C23X C24 174(5) . . ?
C23 C24 H24D 110.9 . . ?
C23 C24 H24E 109.0 . . ?
C23 C24 H24F 108.5 . . ?
C23X C24 H24A 107.9 . . ?
C23X C24 H24B 109.1 . . ?
C23X C24 H24C 111.3 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
H24D C24 H24E 109.5 . . ?
H24D C24 H24F 109.5 . . ?
H24E C24 H24F 109.5 . . ?
H2WA O2W H2WB 104.5 . . ?
H1WA O1W H1WB 109.4 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C19 1.999(6) . ?
Pd1 C20 1.988(6) . ?
Pd1 C21 1.988(6) . ?
Pd1 C22 1.981(6) . ?
Fe1 N1 2.186(5) . ?
Fe1 N2 2.042(5) . ?
Fe1 N3 2.163(5) . ?
Fe1 N7 2.047(5) . ?
Fe1 N8 2.099(5) 2_666 ?
Fe1 N9 2.046(5) 2_656 ?
N1 C1 1.345(8) . ?
N1 C5 1.355(8) . ?
N2 C6 1.355(7) . ?
N2 C8 1.333(7) . ?
N3 C9 1.349(8) . ?
N3 C13 1.353(8) . ?
N4 C6 1.314(8) . ?
N4 C7 1.350(7) . ?
N5 C7 1.348(7) . ?
N5 C8 1.316(8) . ?
N6 C14 1.349(7) . ?
N6 C18 1.320(8) . ?
N7 C19 1.149(8) . ?
N8 C20 1.143(7) . ?
N9 C21 1.152(7) . ?
N10 C22 1.150(7) . ?
C1 H1 0.9500 . ?
C1 C2 1.435(11) . ?
C2 H2 0.9500 . ?
C2 C3 1.341(12) . ?
C3 H3 0.9500 . ?
C3 C4 1.373(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.388(8) . ?
C5 C6 1.479(7) . ?
C7 C14 1.483(8) . ?
C8 C9 1.483(7) . ?
C9 C10 1.384(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.382(9) . ?
C11 H11 0.9500 . ?
C11 C12 1.369(12) . ?
C12 H12 0.9500 . ?
C12 C13 1.393(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.390(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.378(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.386(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.400(8) . ?
C18 H18 0.9500 . ?
N11 C23 1.128(14) . ?
N11X C23X 1.112(14) . ?
C23 C24 1.462(9) . ?
C23X C24 1.454(9) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9799 . ?
C24 H24C 0.9801 . ?
C24 H24D 0.9800 . ?
C24 H24E 0.9800 . ?
C24 H24F 0.9801 . ?
O2W H2WA 0.8700 . ?
O2W H2WB 0.8699 . ?
O1W H1WA 0.8698 . ?
O1W H1WB 0.8702 . ?
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 N1 C1 C2 178.3(4) . . . . ?
Fe1 N1 C5 C4 -177.6(4) . . . . ?
Fe1 N1 C5 C6 3.6(6) . . . . ?
Fe1 N2 C6 N4 -164.2(4) . . . . ?
Fe1 N2 C6 C5 13.9(6) . . . . ?
Fe1 N2 C8 N5 165.1(4) . . . . ?
Fe1 N2 C8 C9 -12.7(6) . . . . ?
Fe1 N3 C9 C8 1.2(6) . . . . ?
Fe1 N3 C9 C10 -178.8(4) . . . . ?
Fe1 N3 C13 C12 178.0(5) . . . . ?
N1 C1 C2 C3 -0.7(10) . . . . ?
N1 C5 C6 N2 -10.7(7) . . . . ?
N1 C5 C6 N4 167.4(5) . . . . ?
N2 C8 C9 N3 6.9(7) . . . . ?
N2 C8 C9 C10 -173.2(5) . . . . ?
N3 C9 C10 C11 0.5(8) . . . . ?
N4 C7 C14 N6 175.4(5) . . . . ?
N4 C7 C14 C15 -3.0(8) . . . . ?
N5 C7 C14 N6 -4.1(7) . . . . ?
N5 C7 C14 C15 177.5(5) . . . . ?
N5 C8 C9 N3 -171.0(5) . . . . ?
N5 C8 C9 C10 9.0(8) . . . . ?
N6 C14 C15 C16 -1.1(8) . . . . ?
C1 N1 C5 C4 1.0(8) . . . . ?
C1 N1 C5 C6 -177.8(5) . . . . ?
C1 C2 C3 C4 0.6(10) . . . . ?
C2 C3 C4 C5 0.2(9) . . . . ?
C3 C4 C5 N1 -1.0(9) . . . . ?
C3 C4 C5 C6 177.7(5) . . . . ?
C4 C5 C6 N2 170.5(5) . . . . ?
C4 C5 C6 N4 -11.4(8) . . . . ?
C5 N1 C1 C2 -0.2(8) . . . . ?
C6 N2 C8 N5 3.1(8) . . . . ?
C6 N2 C8 C9 -174.6(4) . . . . ?
C6 N4 C7 N5 2.9(8) . . . . ?
C6 N4 C7 C14 -176.6(5) . . . . ?
C7 N4 C6 N2 -0.4(8) . . . . ?
C7 N4 C6 C5 -178.3(5) . . . . ?
C7 N5 C8 N2 -0.9(8) . . . . ?
C7 N5 C8 C9 176.6(5) . . . . ?
C7 C14 C15 C16 177.2(5) . . . . ?
C8 N2 C6 N4 -2.4(8) . . . . ?
C8 N2 C6 C5 175.7(4) . . . . ?
C8 N5 C7 N4 -2.3(8) . . . . ?
C8 N5 C7 C14 177.2(5) . . . . ?
C8 C9 C10 C11 -179.4(5) . . . . ?
C9 N3 C13 C12 -0.9(9) . . . . ?
C9 C10 C11 C12 -0.6(9) . . . . ?
C10 C11 C12 C13 0.0(10) . . . . ?
C11 C12 C13 N3 0.8(10) . . . . ?
C13 N3 C9 C8 -179.8(5) . . . . ?
C13 N3 C9 C10 0.3(8) . . . . ?
C14 N6 C18 C17 0.2(8) . . . . ?
C14 C15 C16 C17 0.6(8) . . . . ?
C15 C16 C17 C18 0.2(8) . . . . ?
C16 C17 C18 N6 -0.7(9) . . . . ?
C18 N6 C14 C7 -177.7(5) . . . . ?
C18 N6 C14 C15 0.7(8) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4881(12) 5333 10353 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.5119(12) 5290 10353 nmt -0.9996 -0.0011 0.0000 -0.0005 -0.9978 0.0000 0.4306
0.4086 0.9995
