# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_rt340_ohpmdpt_120kdes_0ma
_database_code_depnum_ccdc_archive 'CCDC 2209612'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_mo_rt340_ohpmdpt_120kdes_0ma 
;
PROBLEM: Check Calcd Resid. Dens.  1.39Ang From C5              3.68 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_mo_rt340_ohpmdpt_120kdes_0ma 
;
PROBLEM: Check Calcd Resid. Dens.  1.49Ang From C6             -5.72 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_mo_rt340_ohpmdpt_120kdes_0ma_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.63Ang From Pt1            -5.08 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_mo_rt340_ohpmdpt_120kdes_0ma_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.35Ang From C6             -4.28 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_mo_rt340_ohpmdpt_120kdes_0ma_4 
;
PROBLEM: Check Calcd Resid. Dens.  0.76Ang From Pt1            -4.12 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT420_mo_rt340_ohpmdpt_120kdes_0ma 
;
PROBLEM: D-H Bond Without Acceptor  O2       --H2       .     Please Check
RESPONSE: The O2 is not involved in H-bonding interactions
;
_vrf_PLAT430_mo_rt340_ohpmdpt_120kdes_0ma 
;
PROBLEM: Short Inter D...A Contact  N4       ..N4       .       2.73 Ang.
RESPONSE: These N atoms are not involved in H-bonding
;
_vrf_PLAT971_mo_rt340_ohpmdpt_120kdes_0ma_2 
;
PROBLEM: Check Calcd Resid. Dens.  1.50Ang From C5              3.50 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_mo_rt340_ohpmdpt_120kdes_0ma_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.00Ang From Pt1             3.32 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_mo_rt340_ohpmdpt_120kdes_0ma_4 
;
PROBLEM: Check Calcd Resid. Dens.  1.00Ang From Pt1             2.88 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_mo_rt340_ohpmdpt_120kdes_0ma_5 
;
PROBLEM: Check Calcd Resid. Dens.  0.99Ang From C6              2.54 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_mo_rt340_ohpmdpt_120kdes_0ma_5 
;
PROBLEM: Check Calcd Resid. Dens.  0.67Ang From Pt1            -3.00 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_mo_rt340_ohpmdpt_120kdes_0ma_6 
;
PROBLEM: Check Calcd Resid. Dens.  0.67Ang From Pt1            -2.71 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_mo_rt340_ohpmdpt_120kdes_0ma_7 
;
PROBLEM: Check Calcd Resid. Dens.  1.45Ang From N3             -2.71 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Monday 26 September 2022 03:56 PM
# end Validation Reply Form

_audit_creation_date             2022-06-10
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H8 Fe N8 O2 Pt'
_chemical_formula_sum            'C12 H8 Fe N8 O2 Pt'
_chemical_formula_weight         547.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   14.2054(6)
_cell_length_b                   7.1095(3)
_cell_length_c                   15.3043(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1545.63(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    121.72
_cell_measurement_theta_max      37.88
_cell_measurement_theta_min      2.87
_shelx_estimated_absorpt_T_max   0.753
_shelx_estimated_absorpt_T_min   0.153
_exptl_absorpt_coefficient_mu    10.004
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_correction_T_min  0.4793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0917 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.6413.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.352
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29764
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.884
_diffrn_reflns_theta_min         1.956
_diffrn_ambient_temperature      121.72
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3757
_reflns_number_total             4426
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         4.045
_refine_diff_density_min         -5.909
_refine_diff_density_rms         0.319
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         4426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0349
_refine_ls_restrained_S_all      1.156
_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)+16.3886P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0739
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1(0.5) H2(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2A), C1(H1A), C7(H7), C9(H9), C10(H10)
3.b Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.47287(2) -0.250000 0.76841(2) 0.00761(4) Uani 1 2 d S T P . .
Fe1 Fe 0.22464(4) 0.250000 0.72062(4) 0.00736(10) Uani 1 2 d S T P . .
O1 O 0.4378(3) 0.250000 0.4333(3) 0.0276(11) Uani 1 2 d S T P . .
H1 H 0.477978 0.282908 0.470633 0.041 Uiso 0.5 1 calc R U P . .
O2 O 0.3443(4) 0.250000 1.0452(3) 0.0333(12) Uani 1 2 d S T P . .
H2 H 0.330678 0.214220 1.095955 0.050 Uiso 0.5 1 calc R U P . .
N1 N 0.2466(3) 0.250000 0.5917(3) 0.0103(6) Uani 1 2 d S T P . .
N5 N 0.2049(3) 0.250000 0.8502(3) 0.0116(7) Uani 1 2 d S T P . .
N3 N 0.31928(19) 0.0582(4) 0.73461(19) 0.0101(4) Uani 1 1 d . . . . .
N4 N 0.6291(2) -0.5580(4) 0.78944(19) 0.0103(4) Uani 1 1 d . . . . .
N2 N 0.1854(4) 0.250000 0.4468(3) 0.0208(10) Uani 1 2 d S T P . .
N6 N 0.1010(4) 0.250000 0.9713(3) 0.0175(8) Uani 1 2 d S T P . .
C4 C 0.3349(4) 0.250000 0.5591(3) 0.0130(8) Uani 1 2 d S T P . .
H4 H 0.386785 0.250000 0.598215 0.016 Uiso 1 2 calc R U P . .
C3 C 0.3515(4) 0.250000 0.4701(3) 0.0158(9) Uani 1 2 d S T P . .
C2 C 0.2730(4) 0.250000 0.4152(3) 0.0195(10) Uani 1 2 d S T P . .
H2A H 0.282247 0.250000 0.353672 0.023 Uiso 1 2 calc R U P . .
C1 C 0.1755(4) 0.250000 0.5337(4) 0.0169(9) Uani 1 2 d S T P . .
H1A H 0.113225 0.250000 0.556203 0.020 Uiso 1 2 calc R U P . .
C7 C 0.2786(4) 0.250000 0.9054(3) 0.0136(8) Uani 1 2 d S T P . .
H7 H 0.340593 0.250000 0.882147 0.016 Uiso 1 2 calc R U P . .
C8 C 0.2663(4) 0.250000 0.9956(4) 0.0194(10) Uani 1 2 d S T P . .
C9 C 0.1738(5) 0.250000 1.0266(3) 0.0199(10) Uani 1 2 d S T P . .
H9 H 0.162509 0.250000 1.087757 0.024 Uiso 1 2 calc R U P . .
C10 C 0.1185(4) 0.250000 0.8860(3) 0.0139(8) Uani 1 2 d S T P . .
H10 H 0.066094 0.250000 0.847447 0.017 Uiso 1 2 calc R U P . .
C5 C 0.3764(2) -0.0543(5) 0.7476(2) 0.0101(5) Uani 1 1 d . . . . .
C6 C 0.5703(2) -0.4464(5) 0.7845(2) 0.0109(5) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.00619(6) 0.00622(6) 0.01043(6) 0.000 -0.00046(6) 0.000
Fe1 0.0063(2) 0.0065(2) 0.0093(2) 0.000 -0.00024(19) 0.000
O1 0.0151(18) 0.058(4) 0.0095(16) 0.000 0.0032(14) 0.000
O2 0.030(3) 0.056(4) 0.0144(19) 0.000 -0.0103(18) 0.000
N1 0.0106(16) 0.0086(15) 0.0119(16) 0.000 -0.0022(13) 0.000
N5 0.0095(15) 0.0109(16) 0.0145(17) 0.000 -0.0025(13) 0.000
N3 0.0093(10) 0.0108(10) 0.0102(10) -0.0001(9) -0.0003(9) 0.0003(9)
N4 0.0097(10) 0.0083(11) 0.0127(11) -0.0006(8) 0.0004(9) -0.0003(9)
N2 0.017(2) 0.034(3) 0.0122(18) 0.000 -0.0017(16) 0.000
N6 0.020(2) 0.021(2) 0.0116(17) 0.000 0.0030(16) 0.000
C4 0.0123(18) 0.018(2) 0.0088(17) 0.000 -0.0002(14) 0.000
C3 0.013(2) 0.023(2) 0.0110(19) 0.000 -0.0003(16) 0.000
C2 0.018(2) 0.031(3) 0.0088(18) 0.000 -0.0011(17) 0.000
C1 0.013(2) 0.024(3) 0.014(2) 0.000 -0.0025(17) 0.000
C7 0.0129(19) 0.016(2) 0.0115(18) 0.000 -0.0018(16) 0.000
C8 0.021(2) 0.024(3) 0.013(2) 0.000 -0.0058(18) 0.000
C9 0.027(3) 0.024(3) 0.0091(19) 0.000 0.0007(19) 0.000
C10 0.015(2) 0.016(2) 0.0112(18) 0.000 0.0023(16) 0.000
C5 0.0102(11) 0.0082(11) 0.0120(12) 0.0002(9) 0.0002(9) -0.0001(10)
C6 0.0105(12) 0.0100(12) 0.0122(12) 0.0000(9) -0.0013(10) 0.0003(10)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C5 1.979(3) 7 ?
Pt1 C5 1.979(3) . ?
Pt1 C6 1.981(3) 7 ?
Pt1 C6 1.981(3) . ?
Fe1 N1 1.997(4) . ?
Fe1 N5 2.004(5) . ?
Fe1 N3 1.927(3) . ?
Fe1 N3 1.927(3) 7_565 ?
Fe1 N4 1.932(3) 6_567 ?
Fe1 N4 1.932(3) 4_446 ?
O1 H1 0.8400 . ?
O1 H1 0.84(8) 7_565 ?
O1 C3 1.350(7) . ?
O2 H2 0.84(9) 7_565 ?
O2 H2 0.8400 . ?
O2 C8 1.343(7) . ?
N1 C4 1.350(7) . ?
N1 C1 1.345(7) . ?
N5 C7 1.344(6) . ?
N5 C10 1.343(7) . ?
N3 C5 1.156(4) . ?
N4 C6 1.154(4) . ?
N2 C2 1.336(8) . ?
N2 C1 1.337(7) . ?
N6 C9 1.335(8) . ?
N6 C10 1.330(7) . ?
C4 H4 0.9500 . ?
C4 C3 1.382(7) . ?
C3 C2 1.396(8) . ?
C2 H2A 0.9500 . ?
C1 H1A 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.392(8) . ?
C8 C9 1.397(9) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?

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
C5 Pt1 C5 89.36(19) 7 . ?
C5 Pt1 C6 90.48(13) 7 . ?
C5 Pt1 C6 90.48(14) . 7 ?
C5 Pt1 C6 177.88(13) . . ?
C5 Pt1 C6 177.87(13) 7 7 ?
C6 Pt1 C6 89.61(19) 7 . ?
N1 Fe1 N5 179.07(17) . . ?
N3 Fe1 N1 90.05(12) 7_565 . ?
N3 Fe1 N1 90.05(12) . . ?
N3 Fe1 N5 89.30(12) 7_565 . ?
N3 Fe1 N5 89.30(12) . . ?
N3 Fe1 N3 90.09(17) . 7_565 ?
N3 Fe1 N4 89.96(12) 7_565 6_567 ?
N3 Fe1 N4 89.95(12) . 4_446 ?
N3 Fe1 N4 178.18(13) . 6_567 ?
N3 Fe1 N4 178.18(13) 7_565 4_446 ?
N4 Fe1 N1 91.77(12) 4_446 . ?
N4 Fe1 N1 91.77(12) 6_567 . ?
N4 Fe1 N5 88.88(12) 4_446 . ?
N4 Fe1 N5 88.88(12) 6_567 . ?
N4 Fe1 N4 89.95(17) 4_446 6_567 ?
H1 O1 H1 32.3 . 7_565 ?
C3 O1 H1 109(2) . 7_565 ?
C3 O1 H1 109.5 . . ?
H2 O2 H2 35.3 . 7_565 ?
C8 O2 H2 109.5 . . ?
C8 O2 H2 109(2) . 7_565 ?
C4 N1 Fe1 120.7(3) . . ?
C1 N1 Fe1 122.4(4) . . ?
C1 N1 C4 116.9(4) . . ?
C7 N5 Fe1 120.8(3) . . ?
C10 N5 Fe1 122.1(3) . . ?
C10 N5 C7 117.1(5) . . ?
C5 N3 Fe1 176.4(3) . . ?
C6 N4 Fe1 171.5(3) . 6_647 ?
C2 N2 C1 117.3(5) . . ?
C10 N6 C9 118.5(5) . . ?
N1 C4 H4 119.2 . . ?
N1 C4 C3 121.6(5) . . ?
C3 C4 H4 119.2 . . ?
O1 C3 C4 124.5(5) . . ?
O1 C3 C2 118.3(5) . . ?
C4 C3 C2 117.2(5) . . ?
N2 C2 C3 121.7(5) . . ?
N2 C2 H2A 119.1 . . ?
C3 C2 H2A 119.1 . . ?
N1 C1 H1A 117.3 . . ?
N2 C1 N1 125.4(5) . . ?
N2 C1 H1A 117.3 . . ?
N5 C7 H7 119.2 . . ?
N5 C7 C8 121.7(5) . . ?
C8 C7 H7 119.2 . . ?
O2 C8 C7 117.2(6) . . ?
O2 C8 C9 125.7(5) . . ?
C7 C8 C9 117.1(5) . . ?
N6 C9 C8 120.9(5) . . ?
N6 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
N5 C10 H10 117.6 . . ?
N6 C10 N5 124.8(5) . . ?
N6 C10 H10 117.6 . . ?
N3 C5 Pt1 178.9(3) . . ?
N4 C6 Pt1 176.2(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 N1 C4 C3 180.000(1) . . . . ?
Fe1 N1 C1 N2 180.000(1) . . . . ?
Fe1 N5 C7 C8 180.000(1) . . . . ?
Fe1 N5 C10 N6 180.000(1) . . . . ?
O1 C3 C2 N2 180.000(1) . . . . ?
O2 C8 C9 N6 180.000(2) . . . . ?
N1 C4 C3 O1 180.000(1) . . . . ?
N1 C4 C3 C2 0.000(1) . . . . ?
N5 C7 C8 O2 180.000(2) . . . . ?
N5 C7 C8 C9 0.000(2) . . . . ?
C4 N1 C1 N2 0.000(1) . . . . ?
C4 C3 C2 N2 0.000(1) . . . . ?
C2 N2 C1 N1 0.000(1) . . . . ?
C1 N1 C4 C3 0.000(1) . . . . ?
C1 N2 C2 C3 0.000(1) . . . . ?
C7 N5 C10 N6 0.000(2) . . . . ?
C7 C8 C9 N6 0.000(2) . . . . ?
C9 N6 C10 N5 0.000(2) . . . . ?
C10 N5 C7 C8 0.000(2) . . . . ?
C10 N6 C9 C8 0.000(2) . . . . ?

_shelx_res_file                  
;
TITL mo_rt340_ohpmdpt_260kdes_0ma_a.res in Pnma
    mo_rt340_ohpmdpt_120kdes_0ma.res
    created by SHELXL-2018/3 at 15:04:50 on 10-Jun-2022
REM Old TITL mo_RT340_OHPmdPt_260Kdes_0ma in Pnma
REM SHELXT solution in Pnma
REM R1 0.052, Rweak 0.003, Alpha 0.061, Orientation as input
REM Formula found by SHELXT: C20 N5 Fe Pt
CELL 0.71073 14.2054 7.1095 15.3043 90 90 90
ZERR 4 0.0006 0.0003 0.0007 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Fe N O Pt
UNIT 48 32 4 32 8 4

L.S. 15
PLAN  5 0 0
SIZE 0.3 0.3 0.03
TEMP -151.43
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
OMIT 0 0 2
REM <olex2.extras>
REM <HklSrc "%.\\mo_RT340_OHPmdPt_120Kdes_0ma.hkl">
REM </olex2.extras>

WGHT    0.000000   16.388599
FVAR       0.21403
PT1   6    0.472868   -0.250000    0.768411    10.50000    0.00619    0.00622 =
         0.01043    0.00000   -0.00046    0.00000
FE1   3    0.224641    0.250000    0.720620    10.50000    0.00627    0.00648 =
         0.00933    0.00000   -0.00024    0.00000
O1    5    0.437841    0.250000    0.433338    10.50000    0.01512    0.05814 =
         0.00946    0.00000    0.00319    0.00000
AFIX 147
H1    2    0.477978    0.282908    0.470633    10.50000   -1.50000
AFIX   0
O2    5    0.344268    0.250000    1.045189    10.50000    0.02993    0.05551 =
         0.01443    0.00000   -0.01029    0.00000
AFIX 147
H2    2    0.330678    0.214220    1.095955    10.50000   -1.50000
AFIX   0
N1    4    0.246581    0.250000    0.591742    10.50000    0.01057    0.00859 =
         0.01188    0.00000   -0.00216    0.00000
N5    4    0.204882    0.250000    0.850244    10.50000    0.00952    0.01087 =
         0.01453    0.00000   -0.00245    0.00000
N3    4    0.319276    0.058239    0.734607    11.00000    0.00931    0.01078 =
         0.01016   -0.00009   -0.00030    0.00029
N4    4    0.629056   -0.557964    0.789441    11.00000    0.00973    0.00830 =
         0.01273   -0.00057    0.00038   -0.00035
N2    4    0.185405    0.250000    0.446770    10.50000    0.01665    0.03358 =
         0.01218    0.00000   -0.00168    0.00000
N6    4    0.101004    0.250000    0.971340    10.50000    0.02013    0.02083 =
         0.01163    0.00000    0.00304    0.00000
C4    1    0.334857    0.250000    0.559100    10.50000    0.01229    0.01792 =
         0.00879    0.00000   -0.00023    0.00000
AFIX  43
H4    2    0.386785    0.250000    0.598215    10.50000   -1.20000
AFIX   0
C3    1    0.351482    0.250000    0.470141    10.50000    0.01316    0.02328 =
         0.01103    0.00000   -0.00027    0.00000
C2    1    0.273042    0.250000    0.415155    10.50000    0.01831    0.03135 =
         0.00876    0.00000   -0.00111    0.00000
AFIX  43
H2A   2    0.282247    0.250000    0.353672    10.50000   -1.20000
AFIX   0
C1    1    0.175532    0.250000    0.533653    10.50000    0.01291    0.02382 =
         0.01392    0.00000   -0.00254    0.00000
AFIX  43
H1A   2    0.113225    0.250000    0.556203    10.50000   -1.20000
AFIX   0
C7    1    0.278570    0.250000    0.905363    10.50000    0.01287    0.01627 =
         0.01153    0.00000   -0.00177    0.00000
AFIX  43
H7    2    0.340593    0.250000    0.882147    10.50000   -1.20000
AFIX   0
C8    1    0.266274    0.250000    0.995572    10.50000    0.02149    0.02375 =
         0.01283    0.00000   -0.00582    0.00000
C9    1    0.173785    0.250000    1.026571    10.50000    0.02666    0.02401 =
         0.00909    0.00000    0.00073    0.00000
AFIX  43
H9    2    0.162509    0.250000    1.087757    10.50000   -1.20000
AFIX   0
C10   1    0.118521    0.250000    0.885985    10.50000    0.01460    0.01583 =
         0.01119    0.00000    0.00230    0.00000
AFIX  43
H10   2    0.066094    0.250000    0.847447    10.50000   -1.20000
AFIX   0
C5    1    0.376373   -0.054271    0.747630    11.00000    0.01022    0.00818 =
         0.01203    0.00020    0.00021   -0.00014
C6    1    0.570300   -0.446376    0.784485    11.00000    0.01049    0.00997 =
         0.01218    0.00002   -0.00130    0.00030
HKLF 4




REM  mo_rt340_ohpmdpt_260kdes_0ma_a.res in Pnma
REM wR2 = 0.0739, GooF = S = 1.156, Restrained GooF = 1.156 for all data
REM R1 = 0.0349 for 3757 Fo > 4sig(Fo) and 0.0498 for all 4426 data
REM 135 parameters refined using 0 restraints

END

WGHT      0.0000     16.3876

REM Highest difference peak  4.045,  deepest hole -5.909,  1-sigma level  0.319
Q1    1   0.3619 -0.2500  0.7429  10.50000  0.05    4.05
Q2    1   0.4721 -0.2500  0.6964  10.50000  0.05    3.53
Q3    1   0.5411 -0.2500  0.7704  10.50000  0.05    3.45
Q4    1   0.3598 -0.2500  0.7908  10.50000  0.05    3.23
Q5    1   0.5807 -0.3168  0.7434  11.00000  0.05    2.56
;
_shelx_res_checksum              92315
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rt340_ohpmdpt_230k_0m
_database_code_depnum_ccdc_archive 'CCDC 2209615'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT975_rt340_ohpmdpt_230k_0m 
;
PROBLEM: Check Calcd Resid. Dens.  0.56Ang From O3      .       2.16 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Monday 26 September 2022 03:56 PM
# end Validation Reply Form

_audit_creation_date             2022-05-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H8 Fe N8 O2 Pt, O'
_chemical_formula_sum            'C12 H8 Fe N8 O3 Pt'
_chemical_formula_weight         563.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.212(3)
_cell_length_b                   7.2863(11)
_cell_length_c                   14.572(2)
_cell_angle_alpha                90
_cell_angle_beta                 132.099(7)
_cell_angle_gamma                90
_cell_volume                     1671.1(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    229.99
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.80
_shelx_estimated_absorpt_T_max   0.769
_shelx_estimated_absorpt_T_min   0.168
_exptl_absorpt_coefficient_mu    9.260
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0854 before and 0.0329 after correction.
The Ratio of minimum to maximum transmission is 0.7108.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.239
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13486
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.485
_diffrn_reflns_theta_min         2.796
_diffrn_ambient_temperature      229.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2639
_reflns_number_total             2687
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.256
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2687
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_gt           0.0175
_refine_ls_restrained_S_all      1.163
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0084P)²+10.1726P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0431
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1(0.5) H2(0.5) O3(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C4(H4), C7(H7), C9(H9), C10(H10)
3.b Tetrahedral OH refined with riding coordinates:
 O2(H2)
3.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.48301(2) 0.500000 0.74282(2) 0.01201(4) Uani 1 2 d S T P . .
Fe1 Fe 0.500000 0.000000 0.500000 0.01341(13) Uani 1 4 d S T P . .
Fe2 Fe 0.500000 1.000000 1.000000 0.01136(12) Uani 1 4 d S T P . .
O1 O 0.1895(2) 0.000000 0.0132(3) 0.0502(12) Uani 1 2 d S T P . .
H1 H 0.222175 0.030654 0.003161 0.075 Uiso 0.5 1 calc R U P . .
O2 O 0.1683(2) 1.000000 0.6022(3) 0.0519(12) Uani 1 2 d S T P . .
H2 H 0.189789 0.998030 0.571244 0.078 Uiso 1 2 calc R U P . .
N1 N 0.3595(2) 0.000000 0.3475(3) 0.0238(7) Uani 1 2 d S T P . .
N2 N 0.2242(3) 0.000000 0.2901(4) 0.0384(10) Uani 1 2 d S T P . .
N3 N 0.49366(16) 0.2027(3) 0.5989(2) 0.0237(5) Uani 1 1 d . . . . .
N4 N 0.48207(14) 0.8099(3) 0.89141(19) 0.0164(4) Uani 1 1 d . . . . .
N5 N 0.3756(2) 1.000000 0.9110(3) 0.0180(6) Uani 1 2 d S T P . .
N6 N 0.2688(2) 1.000000 0.9222(4) 0.0294(8) Uani 1 2 d S T P . .
C1 C 0.3092(3) 0.000000 0.3730(4) 0.0303(9) Uani 1 2 d S T P . .
H1A H 0.336324 0.000000 0.456924 0.036 Uiso 1 2 calc R U P . .
C2 C 0.1856(3) 0.000000 0.1710(5) 0.0353(10) Uani 1 2 d S T P . .
H2A H 0.125881 0.000000 0.110342 0.042 Uiso 1 2 calc R U P . .
C3 C 0.2316(3) 0.000000 0.1344(4) 0.0290(9) Uani 1 2 d S T P . .
C4 C 0.3201(3) 0.000000 0.2278(4) 0.0260(8) Uani 1 2 d S T P . .
H4 H 0.352904 0.000000 0.205855 0.031 Uiso 1 2 calc R U P . .
C5 C 0.48921(16) 0.3094(3) 0.6521(2) 0.0172(5) Uani 1 1 d . . . . .
C6 C 0.47959(16) 0.6946(3) 0.8350(2) 0.0158(4) Uani 1 1 d . . . . .
C7 C 0.3157(3) 1.000000 0.7869(4) 0.0241(8) Uani 1 2 d S T P . .
H7 H 0.331962 1.000000 0.740622 0.029 Uiso 1 2 calc R U P . .
C8 C 0.2302(3) 1.000000 0.7264(4) 0.0323(10) Uani 1 2 d S T P . .
C9 C 0.2090(3) 1.000000 0.7978(5) 0.0342(10) Uani 1 2 d S T P . .
H9 H 0.151360 1.000000 0.758493 0.041 Uiso 1 2 calc R U P . .
C10 C 0.3494(3) 1.000000 0.9733(4) 0.0234(8) Uani 1 2 d S T P . .
H10 H 0.391546 1.000000 1.060134 0.028 Uiso 1 2 calc R U P . .
O3 O 0.2313(5) 1.0824(10) 0.4926(7) 0.0682(19) Uiso 0.5 1 d . . P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.01840(7) 0.00868(6) 0.01258(6) 0.000 0.01188(5) 0.000
Fe1 0.0205(3) 0.0102(3) 0.0145(3) 0.000 0.0138(3) 0.000
Fe2 0.0170(3) 0.0085(3) 0.0125(3) 0.000 0.0115(3) 0.000
O1 0.0229(16) 0.104(4) 0.0217(16) 0.000 0.0140(14) 0.000
O2 0.0245(17) 0.096(4) 0.0217(16) 0.000 0.0098(14) 0.000
N1 0.0235(16) 0.0269(17) 0.0240(16) 0.000 0.0171(14) 0.000
N2 0.032(2) 0.058(3) 0.035(2) 0.000 0.0264(19) 0.000
N3 0.0335(12) 0.0188(11) 0.0262(11) -0.0019(9) 0.0231(11) 0.0011(9)
N4 0.0226(10) 0.0134(9) 0.0168(9) -0.0007(7) 0.0147(8) -0.0005(8)
N5 0.0197(14) 0.0171(14) 0.0167(14) 0.000 0.0121(12) 0.000
N6 0.0251(17) 0.039(2) 0.0290(18) 0.000 0.0201(16) 0.000
C1 0.028(2) 0.043(3) 0.027(2) 0.000 0.0216(18) 0.000
C2 0.024(2) 0.051(3) 0.031(2) 0.000 0.0186(19) 0.000
C3 0.0224(19) 0.041(3) 0.0225(19) 0.000 0.0147(17) 0.000
C4 0.0222(18) 0.034(2) 0.0249(19) 0.000 0.0172(17) 0.000
C5 0.0233(11) 0.0143(11) 0.0168(10) 0.0005(9) 0.0146(10) 0.0004(9)
C6 0.0227(11) 0.0128(10) 0.0175(10) 0.0004(8) 0.0157(10) -0.0006(9)
C7 0.0260(19) 0.0254(19) 0.0189(17) 0.000 0.0142(16) 0.000
C8 0.025(2) 0.038(2) 0.0221(19) 0.000 0.0107(17) 0.000
C9 0.0206(19) 0.046(3) 0.032(2) 0.000 0.0163(18) 0.000
C10 0.0239(18) 0.028(2) 0.0215(17) 0.000 0.0165(16) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C5 1.982(3) . ?
Pt1 C5 1.982(3) 6_565 ?
Pt1 C6 1.987(3) 6_565 ?
Pt1 C6 1.987(2) . ?
Fe1 N1 2.223(4) 5_656 ?
Fe1 N1 2.223(4) . ?
Fe1 N3 2.130(2) 2_656 ?
Fe1 N3 2.130(2) . ?
Fe1 N3 2.130(2) 6 ?
Fe1 N3 2.130(2) 5_656 ?
Fe2 N4 1.939(2) 6_575 ?
Fe2 N4 1.939(2) 2_657 ?
Fe2 N4 1.939(2) . ?
Fe2 N4 1.939(2) 5_677 ?
Fe2 N5 2.014(3) . ?
Fe2 N5 2.014(3) 5_677 ?
O1 H1 0.83(7) 6 ?
O1 H1 0.8300 . ?
O1 C3 1.342(5) . ?
O2 H2 0.8300 . ?
O2 C8 1.346(6) . ?
N1 C1 1.343(6) . ?
N1 C4 1.337(5) . ?
N2 C1 1.338(6) . ?
N2 C2 1.333(7) . ?
N3 C5 1.146(4) . ?
N4 C6 1.152(3) . ?
N5 C7 1.343(5) . ?
N5 C10 1.345(5) . ?
N6 C9 1.346(6) . ?
N6 C10 1.331(5) . ?
C1 H1A 0.9400 . ?
C2 H2A 0.9400 . ?
C2 C3 1.391(7) . ?
C3 C4 1.396(6) . ?
C4 H4 0.9400 . ?
C7 H7 0.9400 . ?
C7 C8 1.386(6) . ?
C8 C9 1.385(7) . ?
C9 H9 0.9400 . ?
C10 H10 0.9400 . ?

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
C5 Pt1 C5 88.98(15) . 6_565 ?
C5 Pt1 C6 89.98(10) . 6_565 ?
C5 Pt1 C6 178.40(10) 6_565 6_565 ?
C5 Pt1 C6 178.40(11) . . ?
C5 Pt1 C6 89.98(10) 6_565 . ?
C6 Pt1 C6 91.03(14) 6_565 . ?
N1 Fe1 N1 180.00(18) . 5_656 ?
N3 Fe1 N1 91.48(10) 6 . ?
N3 Fe1 N1 91.48(10) . . ?
N3 Fe1 N1 91.48(10) 2_656 5_656 ?
N3 Fe1 N1 88.52(10) 6 5_656 ?
N3 Fe1 N1 88.52(10) 5_656 . ?
N3 Fe1 N1 88.52(10) 2_656 . ?
N3 Fe1 N1 88.52(10) . 5_656 ?
N3 Fe1 N1 91.48(10) 5_656 5_656 ?
N3 Fe1 N3 180.00(16) 5_656 . ?
N3 Fe1 N3 87.83(13) 5_656 2_656 ?
N3 Fe1 N3 92.17(14) 2_656 . ?
N3 Fe1 N3 180.0 6 2_656 ?
N3 Fe1 N3 92.17(14) 5_656 6 ?
N3 Fe1 N3 87.83(14) 6 . ?
N4 Fe2 N4 91.18(13) 5_677 2_657 ?
N4 Fe2 N4 88.82(13) 5_677 6_575 ?
N4 Fe2 N4 180.0 6_575 2_657 ?
N4 Fe2 N4 180.0 5_677 . ?
N4 Fe2 N4 91.18(13) 6_575 . ?
N4 Fe2 N4 88.82(13) 2_657 . ?
N4 Fe2 N5 91.09(9) 6_575 . ?
N4 Fe2 N5 91.09(9) 2_657 5_677 ?
N4 Fe2 N5 88.91(9) 2_657 . ?
N4 Fe2 N5 88.91(9) 5_677 . ?
N4 Fe2 N5 88.91(9) . 5_677 ?
N4 Fe2 N5 88.91(9) 6_575 5_677 ?
N4 Fe2 N5 91.09(9) 5_677 5_677 ?
N4 Fe2 N5 91.09(9) . . ?
N5 Fe2 N5 180.0 5_677 . ?
H1 O1 H1 31.2 . 6 ?
C3 O1 H1 109.5(17) . 6 ?
C3 O1 H1 109.5 . . ?
C8 O2 H2 109.5 . . ?
C1 N1 Fe1 120.3(3) . . ?
C4 N1 Fe1 123.4(3) . . ?
C4 N1 C1 116.3(4) . . ?
C2 N2 C1 117.2(4) . . ?
C5 N3 Fe1 178.6(2) . . ?
C6 N4 Fe2 173.5(2) . . ?
C7 N5 Fe2 121.0(3) . . ?
C7 N5 C10 117.6(4) . . ?
C10 N5 Fe2 121.4(3) . . ?
C10 N6 C9 116.8(4) . . ?
N1 C1 H1A 117.0 . . ?
N2 C1 N1 126.1(4) . . ?
N2 C1 H1A 117.0 . . ?
N2 C2 H2A 119.3 . . ?
N2 C2 C3 121.4(4) . . ?
C3 C2 H2A 119.3 . . ?
O1 C3 C2 119.0(4) . . ?
O1 C3 C4 123.8(4) . . ?
C2 C3 C4 117.2(4) . . ?
N1 C4 C3 121.8(4) . . ?
N1 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
N3 C5 Pt1 178.1(2) . . ?
N4 C6 Pt1 176.3(2) . . ?
N5 C7 H7 119.7 . . ?
N5 C7 C8 120.6(4) . . ?
C8 C7 H7 119.7 . . ?
O2 C8 C7 122.5(5) . . ?
O2 C8 C9 119.6(4) . . ?
C9 C8 C7 117.9(4) . . ?
N6 C9 C8 121.7(4) . . ?
N6 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
N5 C10 H10 117.3 . . ?
N6 C10 N5 125.4(4) . . ?
N6 C10 H10 117.3 . . ?

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 N1 C1 N2 180.000(1) . . . . ?
Fe1 N1 C4 C3 180.000(1) . . . . ?
Fe2 N5 C7 C8 180.000(2) . . . . ?
Fe2 N5 C10 N6 180.000(3) . . . . ?
O1 C3 C4 N1 180.000(1) . . . . ?
O2 C8 C9 N6 180.000(3) . . . . ?
N2 C2 C3 O1 180.000(1) . . . . ?
N2 C2 C3 C4 0.000(1) . . . . ?
N5 C7 C8 O2 180.000(3) . . . . ?
N5 C7 C8 C9 0.000(3) . . . . ?
C1 N1 C4 C3 0.000(1) . . . . ?
C1 N2 C2 C3 0.000(1) . . . . ?
C2 N2 C1 N1 0.000(1) . . . . ?
C2 C3 C4 N1 0.000(1) . . . . ?
C4 N1 C1 N2 0.000(2) . . . . ?
C7 N5 C10 N6 0.000(4) . . . . ?
C7 C8 C9 N6 0.000(3) . . . . ?
C9 N6 C10 N5 0.000(4) . . . . ?
C10 N5 C7 C8 0.000(3) . . . . ?
C10 N6 C9 C8 0.000(4) . . . . ?

_shelx_res_file                  
;
TITL rt340_ohpmdpt_230k_0m_a.res in C2/m
    rt340_ohpmdpt_230k_0m.res
    created by SHELXL-2018/3 at 23:21:48 on 19-May-2022
REM Old TITL rt340_ohpmdpt_230k_0m_a.res in C2/m
REM SHELXT solution in C2/m
REM R1 0.179, Rweak 0.022, Alpha 0.027, Orientation as input
REM Formula found by SHELXT: C23 I
CELL 0.71073 21.2119 7.2863 14.5719 90 132.099 90
ZERR 4 0.0033 0.0011 0.0022 0 0.007 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pt
UNIT 48 32 4 32 12 4

L.S. 30
PLAN  2
SIZE 0.3 0.3 0.03
TEMP -43.16
CONF
LIST 6
MORE -1
BOND $H
fmap 2
acta
OMIT 2 0 0
REM <olex2.extras>
REM <HklSrc "%.\\RT340_OHpmdPt_230K_0m.hkl">
REM </olex2.extras>

WGHT    0.008400   10.172600
FVAR       0.29360
PT1   6    0.483008    0.500000    0.742824    10.50000    0.01840    0.00868 =
         0.01258    0.00000    0.01188    0.00000
FE1   3    0.500000    0.000000    0.500000    10.25000    0.02050    0.01024 =
         0.01454    0.00000    0.01382    0.00000
FE2   3    0.500000    1.000000    1.000000    10.25000    0.01701    0.00854 =
         0.01245    0.00000    0.01150    0.00000
O1    5    0.189451    0.000000    0.013179    10.50000    0.02285    0.10392 =
         0.02166    0.00000    0.01404    0.00000
AFIX 147
H1    2    0.222175    0.030654    0.003161    10.50000   -1.50000
AFIX   0
O2    5    0.168278    1.000000    0.602246    10.50000    0.02453    0.09572 =
         0.02167    0.00000    0.00981    0.00000
AFIX  83
H2    2    0.189789    0.998030    0.571244    10.50000   -1.50000
AFIX   0
N1    4    0.359485    0.000000    0.347518    10.50000    0.02345    0.02688 =
         0.02401    0.00000    0.01714    0.00000
N2    4    0.224246    0.000000    0.290062    10.50000    0.03178    0.05798 =
         0.03509    0.00000    0.02638    0.00000
N3    4    0.493664    0.202709    0.598878    11.00000    0.03349    0.01879 =
         0.02616   -0.00190    0.02307    0.00114
N4    4    0.482066    0.809881    0.891408    11.00000    0.02264    0.01337 =
         0.01677   -0.00072    0.01467   -0.00052
N5    4    0.375610    1.000000    0.911006    10.50000    0.01975    0.01713 =
         0.01672    0.00000    0.01209    0.00000
N6    4    0.268771    1.000000    0.922220    10.50000    0.02511    0.03915 =
         0.02896    0.00000    0.02012    0.00000
C1    1    0.309238    0.000000    0.372998    10.50000    0.02795    0.04343 =
         0.02712    0.00000    0.02158    0.00000
AFIX  43
H1A   2    0.336324    0.000000    0.456924    10.50000   -1.20000
AFIX   0
C2    1    0.185565    0.000000    0.170960    10.50000    0.02409    0.05082 =
         0.03113    0.00000    0.01855    0.00000
AFIX  43
H2A   2    0.125881    0.000000    0.110342    10.50000   -1.20000
AFIX   0
C3    1    0.231626    0.000000    0.134403    10.50000    0.02241    0.04133 =
         0.02247    0.00000    0.01472    0.00000
C4    1    0.320117    0.000000    0.227776    10.50000    0.02223    0.03427 =
         0.02492    0.00000    0.01723    0.00000
AFIX  43
H4    2    0.352904    0.000000    0.205855    10.50000   -1.20000
AFIX   0
C5    1    0.489209    0.309387    0.652091    11.00000    0.02335    0.01432 =
         0.01680    0.00053    0.01465    0.00041
C6    1    0.479586    0.694574    0.834982    11.00000    0.02270    0.01282 =
         0.01746    0.00035    0.01571   -0.00056
C7    1    0.315739    1.000000    0.786873    10.50000    0.02598    0.02538 =
         0.01889    0.00000    0.01424    0.00000
AFIX  43
H7    2    0.331962    1.000000    0.740622    10.50000   -1.20000
AFIX   0
C8    1    0.230247    1.000000    0.726352    10.50000    0.02474    0.03777 =
         0.02207    0.00000    0.01066    0.00000
C9    1    0.208998    1.000000    0.797843    10.50000    0.02062    0.04648 =
         0.03213    0.00000    0.01630    0.00000
AFIX  43
H9    2    0.151360    1.000000    0.758493    10.50000   -1.20000
AFIX   0
C10   1    0.349410    1.000000    0.973296    10.50000    0.02393    0.02780 =
         0.02154    0.00000    0.01647    0.00000
AFIX  43
H10   2    0.391546    1.000000    1.060134    10.50000   -1.20000
AFIX   0

PART -1
O3    5    0.231269    1.082407    0.492600    10.50000    0.06815
HKLF 4




REM  rt340_ohpmdpt_230k_0m_a.res in C2/m
REM wR2 = 0.0431, GooF = S = 1.163, Restrained GooF = 1.163 for all data
REM R1 = 0.0175 for 2639 Fo > 4sig(Fo) and 0.0179 for all 2687 data
REM 140 parameters refined using 0 restraints

END

WGHT      0.0084     10.1847

REM Highest difference peak  2.256,  deepest hole -1.219,  1-sigma level  0.123
Q1    1   0.2299  1.0000  0.4910  10.50000  0.05    2.26
Q2    1   0.4826  0.5000  0.6884  10.50000  0.05    2.25
;
_shelx_res_checksum              79403
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_rt340_ohpmdpt_260k_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2209614'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_mo_rt340_ohpmdpt_260k_0m_a 
;
PROBLEM: Check Calcd Resid. Dens.  0.65Ang From Pt1            -3.70 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT029_mo_rt340_ohpmdpt_260k_0m_a 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.955 Why?
RESPONSE: We ignore the reason of the presence of this alert. The measurement strategy was the same as that used for the same structure at the LS structures whose theta full value is 1.00. In any case, the structural data is good enough to extract the needed structural parameters to the discussion of the paper.
;
_vrf_PLAT972_mo_rt340_ohpmdpt_260k_0m_a_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.72Ang From Pt1            -3.39 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_mo_rt340_ohpmdpt_260k_0m_a_3 
;
PROBLEM: Check Calcd Resid. Dens.  0.62Ang From Pt1            -3.29 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_mo_rt340_ohpmdpt_260k_0m_a_4 
;
PROBLEM: Check Calcd Resid. Dens.  0.69Ang From Pt1            -2.71 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT975_mo_rt340_ohpmdpt_260k_0m_a 
;
PROBLEM: Check Calcd Resid. Dens.  0.55Ang From O3      .       1.67 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Monday 26 September 2022 03:56 PM
# end Validation Reply Form

_audit_creation_date             2022-05-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H8 Fe N8 O2 Pt, O'
_chemical_formula_sum            'C12 H8 Fe N8 O3 Pt'
_chemical_formula_weight         563.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.669(2)
_cell_length_b                   7.4503(7)
_cell_length_c                   14.6204(15)
_cell_angle_alpha                90
_cell_angle_beta                 132.408(2)
_cell_angle_gamma                90
_cell_volume                     1742.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    259.98
_cell_measurement_theta_max      35.66
_cell_measurement_theta_min      2.79
_shelx_estimated_absorpt_T_max   0.777
_shelx_estimated_absorpt_T_min   0.176
_exptl_absorpt_coefficient_mu    8.879
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.5369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0838 before and 0.0334 after correction.
The Ratio of minimum to maximum transmission is 0.7187.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.146
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0935
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16424
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.714
_diffrn_reflns_theta_min         2.786
_diffrn_ambient_temperature      259.98
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3462
_reflns_number_total             3655
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.163
_refine_diff_density_min         -3.725
_refine_diff_density_rms         0.242
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         3655
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0368
_refine_ls_restrained_S_all      1.099
_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)+(0.0363P)²+18.5187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0962
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1(0.5) H2(0.5) O3(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C4(H4), C7(H7), C9(H9), C10(H10)
3.b Tetrahedral OH refined with riding coordinates:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.51518(2) 0.500000 0.26708(2) 0.01593(7) Uani 1 2 d S T P . .
Fe1 Fe 0.500000 0.000000 0.000000 0.01775(19) Uani 1 4 d S T P . .
Fe2 Fe 0.500000 1.000000 0.500000 0.01653(19) Uani 1 4 d S T P . .
O1 O 0.8102(4) 0.000000 0.1400(7) 0.068(3) Uani 1 2 d S T P . .
H1 H 0.785723 -0.060610 0.077171 0.101 Uiso 0.5 1 calc R U P . .
O2 O 0.8374(5) 1.000000 0.7776(9) 0.087(3) Uani 1 2 d S T P . .
H2 H 0.817380 0.976292 0.707440 0.130 Uiso 0.5 1 calc R U P . .
N1 N 0.6401(4) 0.000000 0.1307(5) 0.0315(12) Uani 1 2 d S T P . .
N2 N 0.7689(5) 0.000000 0.3391(7) 0.054(2) Uani 1 2 d S T P . .
N3 N 0.5026(3) 0.2003(6) 0.1061(4) 0.0311(8) Uani 1 1 d . . . . .
N4 N 0.5236(3) 0.7994(6) 0.4250(4) 0.0308(8) Uani 1 1 d . . . . .
N5 N 0.6336(4) 1.000000 0.6753(5) 0.0289(11) Uani 1 2 d S T P . .
N6 N 0.7372(4) 1.000000 0.8941(6) 0.0443(17) Uani 1 2 d S T P . .
C1 C 0.6869(5) 0.000000 0.2542(7) 0.0415(18) Uani 1 2 d S T P . .
H1A H 0.658742 0.000000 0.281610 0.050 Uiso 1 2 calc R U P . .
C2 C 0.8082(6) 0.000000 0.2989(8) 0.049(2) Uani 1 2 d S T P . .
H2A H 0.866287 0.000000 0.357223 0.059 Uiso 1 2 calc R U P . .
C3 C 0.7673(5) 0.000000 0.1738(8) 0.0411(18) Uani 1 2 d S T P . .
C4 C 0.6804(5) 0.000000 0.0918(6) 0.0342(14) Uani 1 2 d S T P . .
H4 H 0.649755 0.000000 0.007071 0.041 Uiso 1 2 calc R U P . .
C5 C 0.5068(3) 0.3110(6) 0.1644(4) 0.0237(7) Uani 1 1 d . . . . .
C6 C 0.5219(3) 0.6889(6) 0.3687(4) 0.0245(8) Uani 1 1 d . . . . .
C7 C 0.6925(5) 1.000000 0.6709(8) 0.0404(17) Uani 1 2 d S T P . .
H7 H 0.677506 1.000000 0.594429 0.049 Uiso 1 2 calc R U P . .
C8 C 0.7776(6) 1.000000 0.7800(10) 0.050(2) Uani 1 2 d S T P . .
C9 C 0.7938(6) 1.000000 0.8894(10) 0.052(2) Uani 1 2 d S T P . .
H9 H 0.849328 1.000000 0.963795 0.063 Uiso 1 2 calc R U P . .
C10 C 0.6581(5) 1.000000 0.7873(7) 0.0376(16) Uani 1 2 d S T P . .
H10 H 0.616750 1.000000 0.790724 0.045 Uiso 1 2 calc R U P . .
O3 O 0.7720(9) 0.9151(19) 0.5362(13) 0.081(4) Uiso 0.5 1 d . . P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.02601(11) 0.01261(10) 0.01728(9) 0.000 0.01788(9) 0.000
Fe1 0.0294(5) 0.0137(4) 0.0183(4) 0.000 0.0194(4) 0.000
Fe2 0.0268(5) 0.0130(4) 0.0162(4) 0.000 0.0171(4) 0.000
O1 0.033(3) 0.134(8) 0.039(3) 0.000 0.025(3) 0.000
O2 0.040(4) 0.164(11) 0.066(5) 0.000 0.039(4) 0.000
N1 0.030(3) 0.039(3) 0.023(2) 0.000 0.016(2) 0.000
N2 0.041(4) 0.091(7) 0.028(3) 0.000 0.022(3) 0.000
N3 0.050(2) 0.0229(18) 0.0325(18) -0.0055(15) 0.0328(19) -0.0007(16)
N4 0.050(2) 0.0225(17) 0.0347(19) -0.0038(15) 0.0345(19) 0.0013(16)
N5 0.030(3) 0.033(3) 0.027(2) 0.000 0.021(2) 0.000
N6 0.033(3) 0.064(5) 0.025(3) 0.000 0.015(3) 0.000
C1 0.042(4) 0.062(5) 0.029(3) 0.000 0.028(3) 0.000
C2 0.034(4) 0.076(7) 0.028(3) 0.000 0.017(3) 0.000
C3 0.035(3) 0.059(5) 0.034(3) 0.000 0.025(3) 0.000
C4 0.032(3) 0.047(4) 0.024(3) 0.000 0.018(3) 0.000
C5 0.035(2) 0.0196(17) 0.0211(15) -0.0025(14) 0.0211(16) -0.0013(15)
C6 0.040(2) 0.0188(17) 0.0277(17) -0.0008(14) 0.0280(18) 0.0011(15)
C7 0.034(3) 0.053(5) 0.037(4) 0.000 0.025(3) 0.000
C8 0.033(4) 0.059(6) 0.059(6) 0.000 0.031(4) 0.000
C9 0.034(4) 0.057(6) 0.046(5) 0.000 0.020(4) 0.000
C10 0.036(3) 0.054(5) 0.024(3) 0.000 0.021(3) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C5 1.975(4) 6_565 ?
Pt1 C5 1.975(4) . ?
Pt1 C6 1.979(4) . ?
Pt1 C6 1.979(4) 6_565 ?
Fe1 N1 2.245(6) 5_655 ?
Fe1 N1 2.245(6) . ?
Fe1 N3 2.125(4) 6 ?
Fe1 N3 2.125(4) 2_655 ?
Fe1 N3 2.125(4) 5_655 ?
Fe1 N3 2.125(4) . ?
Fe2 N4 2.111(4) 5_676 ?
Fe2 N4 2.111(4) 6_575 ?
Fe2 N4 2.111(4) 2_656 ?
Fe2 N4 2.111(4) . ?
Fe2 N5 2.223(6) 5_676 ?
Fe2 N5 2.223(6) . ?
O1 H1 0.8200 . ?
O1 H1 0.8200 6 ?
O1 C3 1.316(10) . ?
O2 H2 0.8200 6_575 ?
O2 H2 0.8200 . ?
O2 C8 1.320(12) . ?
N1 C1 1.348(9) . ?
N1 C4 1.328(9) . ?
N2 C1 1.313(12) . ?
N2 C2 1.320(12) . ?
N3 C5 1.145(6) . ?
N4 C6 1.147(6) . ?
N5 C7 1.322(10) . ?
N5 C10 1.338(9) . ?
N6 C9 1.273(13) . ?
N6 C10 1.330(10) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C2 C3 1.394(12) . ?
C3 C4 1.391(11) . ?
C4 H4 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.406(13) . ?
C8 C9 1.387(16) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?

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
C5 Pt1 C5 90.9(2) 6_565 . ?
C5 Pt1 C6 89.2(2) 6_565 . ?
C5 Pt1 C6 179.23(18) . . ?
C5 Pt1 C6 179.23(18) 6_565 6_565 ?
C5 Pt1 C6 89.2(2) . 6_565 ?
C6 Pt1 C6 90.6(2) . 6_565 ?
N1 Fe1 N1 180.0(3) . 5_655 ?
N3 Fe1 N1 88.68(17) 5_655 . ?
N3 Fe1 N1 88.68(17) 2_655 . ?
N3 Fe1 N1 91.32(17) 5_655 5_655 ?
N3 Fe1 N1 88.68(17) 6 5_655 ?
N3 Fe1 N1 91.31(17) . . ?
N3 Fe1 N1 91.32(17) 6 . ?
N3 Fe1 N1 91.32(17) 2_655 5_655 ?
N3 Fe1 N1 88.68(17) . 5_655 ?
N3 Fe1 N3 90.8(2) . 2_655 ?
N3 Fe1 N3 89.2(2) . 6 ?
N3 Fe1 N3 180.0(2) 6 2_655 ?
N3 Fe1 N3 90.8(2) 5_655 6 ?
N3 Fe1 N3 180.0 . 5_655 ?
N3 Fe1 N3 89.2(2) 5_655 2_655 ?
N4 Fe2 N4 90.1(2) . 6_575 ?
N4 Fe2 N4 180.0(3) . 5_676 ?
N4 Fe2 N4 89.9(2) 5_676 6_575 ?
N4 Fe2 N4 89.9(2) . 2_656 ?
N4 Fe2 N4 180.00(17) 6_575 2_656 ?
N4 Fe2 N4 90.1(2) 5_676 2_656 ?
N4 Fe2 N5 89.11(17) . 5_676 ?
N4 Fe2 N5 90.89(17) 6_575 . ?
N4 Fe2 N5 89.11(17) 6_575 5_676 ?
N4 Fe2 N5 90.89(17) 5_676 5_676 ?
N4 Fe2 N5 89.11(17) 2_656 . ?
N4 Fe2 N5 89.11(17) 5_676 . ?
N4 Fe2 N5 90.89(17) . . ?
N4 Fe2 N5 90.89(17) 2_656 5_676 ?
N5 Fe2 N5 180.0 . 5_676 ?
H1 O1 H1 66.8 . 6 ?
C3 O1 H1 109.5(4) . 6 ?
C3 O1 H1 109.5 . . ?
H2 O2 H2 24.9 . 6_575 ?
C8 O2 H2 109.5 . . ?
C8 O2 H2 109.5(6) . 6_575 ?
C1 N1 Fe1 120.4(5) . . ?
C4 N1 Fe1 122.6(5) . . ?
C4 N1 C1 117.0(6) . . ?
C1 N2 C2 116.5(7) . . ?
C5 N3 Fe1 177.3(4) . . ?
C6 N4 Fe2 168.3(4) . . ?
C7 N5 Fe2 119.6(5) . . ?
C7 N5 C10 117.4(7) . . ?
C10 N5 Fe2 123.0(5) . . ?
C9 N6 C10 117.6(8) . . ?
N1 C1 H1A 117.1 . . ?
N2 C1 N1 125.7(7) . . ?
N2 C1 H1A 117.1 . . ?
N2 C2 H2A 118.2 . . ?
N2 C2 C3 123.6(8) . . ?
C3 C2 H2A 118.2 . . ?
O1 C3 C2 120.5(8) . . ?
O1 C3 C4 124.4(7) . . ?
C4 C3 C2 115.1(7) . . ?
N1 C4 C3 122.0(7) . . ?
N1 C4 H4 119.0 . . ?
C3 C4 H4 119.0 . . ?
N3 C5 Pt1 179.2(5) . . ?
N4 C6 Pt1 178.2(5) . . ?
N5 C7 H7 119.5 . . ?
N5 C7 C8 121.0(8) . . ?
C8 C7 H7 119.5 . . ?
O2 C8 C7 121.9(10) . . ?
O2 C8 C9 122.7(10) . . ?
C9 C8 C7 115.3(8) . . ?
N6 C9 C8 123.9(9) . . ?
N6 C9 H9 118.1 . . ?
C8 C9 H9 118.1 . . ?
N5 C10 H10 117.6 . . ?
N6 C10 N5 124.8(7) . . ?
N6 C10 H10 117.6 . . ?

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 N2 180.000(2) . . . . ?
Fe1 N1 C4 C3 180.000(1) . . . . ?
Fe2 N5 C7 C8 180.000(5) . . . . ?
Fe2 N5 C10 N6 180.000(4) . . . . ?
O1 C3 C4 N1 180.000(1) . . . . ?
O2 C8 C9 N6 180.000(6) . . . . ?
N2 C2 C3 O1 180.000(2) . . . . ?
N2 C2 C3 C4 0.000(2) . . . . ?
N5 C7 C8 O2 180.000(5) . . . . ?
N5 C7 C8 C9 0.000(6) . . . . ?
C1 N1 C4 C3 0.000(1) . . . . ?
C1 N2 C2 C3 0.000(3) . . . . ?
C2 N2 C1 N1 0.000(2) . . . . ?
C2 C3 C4 N1 0.000(2) . . . . ?
C4 N1 C1 N2 0.000(2) . . . . ?
C7 N5 C10 N6 0.000(5) . . . . ?
C7 C8 C9 N6 0.000(7) . . . . ?
C9 N6 C10 N5 0.000(6) . . . . ?
C10 N5 C7 C8 0.000(6) . . . . ?
C10 N6 C9 C8 0.000(7) . . . . ?

_shelx_res_file                  
;
TITL mo_rt340_ohpmdpt_260k_0m_a_a.res in C2/m
    mo_rt340_ohpmdpt_260k_0m_a.res
    created by SHELXL-2018/3 at 23:26:07 on 19-May-2022
REM Old TITL mo_RT340_OHpmdPt_260K_0m_a.res in C2/m
REM SHELXT solution in C2/m
REM R1 0.100, Rweak 0.014, Alpha 0.118, Orientation as input
REM Formula found by SHELXT: C9 Fe N13 Pt
CELL 0.71073 21.6692 7.4503 14.6204 90 132.408 90
ZERR 4 0.0021 0.0007 0.0015 0 0.002 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pt
UNIT 48 32 4 32 12 4

L.S. 20
PLAN  2 0 0
SIZE 0.3 0.3 0.03
TEMP -13.17
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
OMIT 6 0 13
REM <olex2.extras>
REM <HklSrc "%.\\mo_RT340_OHpmdPt_260K_0m_a.hkl">
REM </olex2.extras>

WGHT    0.036300   18.518700
FVAR       0.34897
PT1   6    0.515181    0.500000    0.267080    10.50000    0.02601    0.01261 =
         0.01728    0.00000    0.01788    0.00000
FE1   3    0.500000    0.000000    0.000000    10.25000    0.02936    0.01368 =
         0.01830    0.00000    0.01935    0.00000
FE2   3    0.500000    1.000000    0.500000    10.25000    0.02684    0.01299 =
         0.01623    0.00000    0.01713    0.00000
O1    5    0.810242    0.000000    0.140042    10.50000    0.03281    0.13397 =
         0.03864    0.00000    0.02519    0.00000
AFIX  83
H1    2    0.785723   -0.060610    0.077171    10.50000   -1.50000
AFIX   0
O2    5    0.837397    1.000000    0.777646    10.50000    0.03984    0.16383 =
         0.06572    0.00000    0.03901    0.00000
AFIX  83
H2    2    0.817380    0.976292    0.707440    10.50000   -1.50000
AFIX   0
N1    4    0.640054    0.000000    0.130748    10.50000    0.02975    0.03858 =
         0.02298    0.00000    0.01650    0.00000
N2    4    0.768938    0.000000    0.339108    10.50000    0.04070    0.09051 =
         0.02766    0.00000    0.02170    0.00000
N3    4    0.502649    0.200279    0.106133    11.00000    0.05015    0.02287 =
         0.03249   -0.00545    0.03278   -0.00073
N4    4    0.523647    0.799427    0.425012    11.00000    0.04995    0.02248 =
         0.03473   -0.00379    0.03446    0.00126
N5    4    0.633556    1.000000    0.675304    10.50000    0.03041    0.03306 =
         0.02724    0.00000    0.02106    0.00000
N6    4    0.737249    1.000000    0.894117    10.50000    0.03320    0.06440 =
         0.02456    0.00000    0.01519    0.00000
C1    1    0.686949    0.000000    0.254187    10.50000    0.04244    0.06170 =
         0.02930    0.00000    0.02782    0.00000
AFIX  43
H1A   2    0.658742    0.000000    0.281610    10.50000   -1.20000
AFIX   0
C2    1    0.808161    0.000000    0.298893    10.50000    0.03412    0.07569 =
         0.02793    0.00000    0.01673    0.00000
AFIX  43
H2A   2    0.866287    0.000000    0.357223    10.50000   -1.20000
AFIX   0
C3    1    0.767289    0.000000    0.173832    10.50000    0.03520    0.05920 =
         0.03368    0.00000    0.02517    0.00000
C4    1    0.680444    0.000000    0.091768    10.50000    0.03153    0.04661 =
         0.02352    0.00000    0.01814    0.00000
AFIX  43
H4    2    0.649755    0.000000    0.007071    10.50000   -1.20000
AFIX   0
C5    1    0.506844    0.311010    0.164443    11.00000    0.03542    0.01959 =
         0.02108   -0.00246    0.02107   -0.00129
C6    1    0.521929    0.688851    0.368701    11.00000    0.03994    0.01878 =
         0.02767   -0.00080    0.02795    0.00111
C7    1    0.692520    1.000000    0.670888    10.50000    0.03429    0.05294 =
         0.03708    0.00000    0.02529    0.00000
AFIX  43
H7    2    0.677506    1.000000    0.594429    10.50000   -1.20000
AFIX   0
C8    1    0.777583    1.000000    0.780047    10.50000    0.03327    0.05897 =
         0.05884    0.00000    0.03097    0.00000
C9    1    0.793819    1.000000    0.889438    10.50000    0.03434    0.05734 =
         0.04619    0.00000    0.01962    0.00000
AFIX  43
H9    2    0.849328    1.000000    0.963795    10.50000   -1.20000
AFIX   0
C10   1    0.658086    1.000000    0.787321    10.50000    0.03610    0.05442 =
         0.02387    0.00000    0.02084    0.00000
AFIX  43
H10   2    0.616750    1.000000    0.790724    10.50000   -1.20000
AFIX   0

PART -1
O3    5    0.771955    0.915135    0.536246    10.50000    0.08097
HKLF 4




REM  mo_rt340_ohpmdpt_260k_0m_a_a.res in C2/m
REM wR2 = 0.0962, GooF = S = 1.099, Restrained GooF = 1.099 for all data
REM R1 = 0.0368 for 3462 Fo > 4sig(Fo) and 0.0397 for all 3655 data
REM 139 parameters refined using 0 restraints

END

WGHT      0.0363     18.5209

REM Highest difference peak  2.163,  deepest hole -3.725,  1-sigma level  0.242
Q1    1   0.5696  0.5000  0.3386  10.50000  0.05    2.16
Q2    1   0.4597  0.5000  0.1825  10.50000  0.05    2.11
;
_shelx_res_checksum              73001
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rt366_feohpmdpd_200k_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2209619'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_rt366_feohpmdpd_200k_0m_a 
;
PROBLEM: Check Calcd Resid. Dens.  0.90Ang From Pd1             4.04 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt366_feohpmdpd_200k_0m_a_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.83Ang From Pd1             3.28 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt366_feohpmdpd_200k_0m_a_3 
;
PROBLEM: Check Calcd Resid. Dens.  0.99Ang From Fe1             3.05 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt366_feohpmdpd_200k_0m_a_4 
;
PROBLEM: Check Calcd Resid. Dens.  1.10Ang From Fe2             2.87 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT975_rt366_feohpmdpd_200k_0m_a 
;
PROBLEM: Check Calcd Resid. Dens.  0.57Ang From O3      .       1.54 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Monday 26 September 2022 03:56 PM
# end Validation Reply Form

_audit_creation_date             2022-05-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H9 Fe N8 O2 Pd, O'
_chemical_formula_sum            'C12 H9 Fe N8 O3 Pd'
_chemical_formula_weight         475.52
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.0937(16)
_cell_length_b                   7.1552(5)
_cell_length_c                   14.3204(11)
_cell_angle_alpha                90
_cell_angle_beta                 132.571(2)
_cell_angle_gamma                90
_cell_volume                     1591.7(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7126
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.84
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.073
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1297 before and 0.0720 after correction.
The Ratio of minimum to maximum transmission is 0.8698.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15232
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.400
_diffrn_reflns_theta_min         2.622
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1893
_reflns_number_total             2138
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         3.754
_refine_diff_density_min         -1.756
_refine_diff_density_rms         0.251
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2138
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0677
_refine_ls_restrained_S_all      1.178
_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)+(0.0477P)²+61.1770P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1789
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H2(0.5) H1(0.5) O3(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2A), N2(H2B), C1(H1A), C7(H7), C9(H9), C10(H10)
3.b Tetrahedral OH refined with riding coordinates:
 O1(H1)
3.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.48466(5) 0.500000 0.73322(7) 0.0159(2) Uani 1 2 d S T P . .
Fe1 Fe 0.500000 1.000000 1.000000 0.0169(4) Uani 1 4 d S T P . .
Fe2 Fe 0.500000 0.000000 0.500000 0.0168(4) Uani 1 4 d S T P . .
N3 N 0.4981(4) 0.8092(9) 0.9020(5) 0.0200(12) Uani 1 1 d . . . . .
N1 N 0.3703(6) 1.000000 0.8785(9) 0.0220(17) Uani 1 2 d S T P . .
O2 O 0.1939(6) 1.000000 0.8690(8) 0.041(2) Uani 1 2 d S T P . .
H2 H 0.224499 0.957201 0.942925 0.061 Uiso 0.5 1 calc R U P . .
C6 C 0.4777(4) 0.3046(10) 0.6282(6) 0.0184(13) Uani 1 1 d . . . . .
N4 N 0.4797(4) 0.1916(8) 0.5724(5) 0.0194(11) Uani 1 1 d . . . . .
N5 N 0.3759(6) 0.000000 0.3410(8) 0.0214(17) Uani 1 2 d S T P . .
O1 O 0.1662(6) 0.000000 0.2355(10) 0.051(3) Uani 1 2 d S T P . .
H1 H 0.187502 -0.022062 0.309463 0.076 Uiso 0.5 1 calc R U P . .
N6 N 0.2692(7) 0.000000 0.1161(10) 0.034(2) Uani 1 2 d S T P . .
C5 C 0.4938(5) 0.6970(10) 0.8402(7) 0.0209(14) Uani 1 1 d . . . . .
C4 C 0.3287(7) 1.000000 0.9187(11) 0.024(2) Uani 1 2 d S T P . .
H4 H 0.360969 1.000000 1.007232 0.029 Uiso 1 2 calc R U P . .
C3 C 0.2393(7) 1.000000 0.8341(11) 0.027(2) Uani 1 2 d S T P . .
C2 C 0.1944(8) 1.000000 0.7047(12) 0.035(3) Uani 1 2 d S T P . .
H2A H 0.133277 1.000000 0.644162 0.042 Uiso 1 2 calc R U P . .
N2 N 0.2359(7) 1.000000 0.6652(10) 0.033(2) Uani 1 2 d S T P . .
H2B H 0.208106 1.000000 0.583942 0.040 Uiso 1 2 calc R U P . .
C1 C 0.3238(8) 1.000000 0.7562(11) 0.032(3) Uani 1 2 d S T P . .
H1A H 0.353644 1.000000 0.727999 0.038 Uiso 1 2 calc R U P . .
C7 C 0.3160(8) 0.000000 0.3458(12) 0.027(2) Uani 1 2 d S T P . .
H7 H 0.332029 0.000000 0.425795 0.032 Uiso 1 2 calc R U P . .
C8 C 0.2280(8) 0.000000 0.2335(14) 0.034(3) Uani 1 2 d S T P . .
C9 C 0.2096(8) 0.000000 0.1207(11) 0.031(2) Uani 1 2 d S T P . .
H9 H 0.151022 0.000000 0.043231 0.037 Uiso 1 2 calc R U P . .
C10 C 0.3501(7) 0.000000 0.2250(10) 0.026(2) Uani 1 2 d S T P . .
H10 H 0.393600 0.000000 0.221771 0.031 Uiso 1 2 calc R U P . .
O3 O 0.2313(12) 0.082(3) 0.4715(17) 0.071(5) Uiso 0.5 1 d . . P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0207(4) 0.0105(3) 0.0190(4) 0.000 0.0144(3) 0.000
Fe1 0.0269(10) 0.0111(9) 0.0213(9) 0.000 0.0198(9) 0.000
Fe2 0.0260(10) 0.0120(9) 0.0187(9) 0.000 0.0176(9) 0.000
N3 0.024(3) 0.019(3) 0.021(3) 0.001(2) 0.017(2) 0.001(2)
N1 0.024(4) 0.014(4) 0.026(4) 0.000 0.017(4) 0.000
O2 0.027(4) 0.068(7) 0.029(4) 0.000 0.020(4) 0.000
C6 0.023(3) 0.015(3) 0.021(3) 0.001(3) 0.016(3) -0.002(3)
N4 0.026(3) 0.016(3) 0.021(3) -0.001(2) 0.018(2) -0.002(2)
N5 0.024(4) 0.016(4) 0.022(4) 0.000 0.015(4) 0.000
O1 0.035(5) 0.077(8) 0.044(6) 0.000 0.028(5) 0.000
N6 0.037(6) 0.038(6) 0.028(5) 0.000 0.022(5) 0.000
C5 0.032(4) 0.014(3) 0.027(3) 0.002(3) 0.024(3) 0.002(3)
C4 0.026(5) 0.023(5) 0.026(5) 0.000 0.019(5) 0.000
C3 0.021(5) 0.029(6) 0.031(5) 0.000 0.018(5) 0.000
C2 0.027(6) 0.046(8) 0.028(6) 0.000 0.017(5) 0.000
N2 0.040(6) 0.033(5) 0.027(5) 0.000 0.023(5) 0.000
C1 0.035(6) 0.029(6) 0.028(6) 0.000 0.020(5) 0.000
C7 0.036(6) 0.018(5) 0.035(6) 0.000 0.028(5) 0.000
C8 0.031(6) 0.024(6) 0.053(8) 0.000 0.030(6) 0.000
C9 0.023(5) 0.030(6) 0.026(5) 0.000 0.011(5) 0.000
C10 0.028(5) 0.027(5) 0.021(5) 0.000 0.016(4) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C6 1.985(7) 6_565 ?
Pd1 C6 1.985(7) . ?
Pd1 C5 1.993(7) 6_565 ?
Pd1 C5 1.993(7) . ?
Fe1 N3 1.939(6) 5_677 ?
Fe1 N3 1.939(6) . ?
Fe1 N3 1.939(6) 2_657 ?
Fe1 N3 1.939(6) 6_575 ?
Fe1 N1 2.017(9) . ?
Fe1 N1 2.017(9) 5_677 ?
Fe2 N4 1.933(6) 6 ?
Fe2 N4 1.933(6) 5_656 ?
Fe2 N4 1.933(6) 2_656 ?
Fe2 N4 1.933(6) . ?
Fe2 N5 1.993(9) 5_656 ?
Fe2 N5 1.993(9) . ?
N3 C5 1.152(9) . ?
N1 C4 1.337(14) . ?
N1 C1 1.306(15) . ?
O2 H2 0.84(17) 6_575 ?
O2 H2 0.8400 . ?
O2 C3 1.348(14) . ?
C6 N4 1.158(9) . ?
N5 C7 1.310(14) . ?
N5 C10 1.354(13) . ?
O1 H1 0.8400 6 ?
O1 H1 0.8400 . ?
O1 C8 1.321(15) . ?
N6 C9 1.302(16) . ?
N6 C10 1.321(15) . ?
C4 H4 0.9500 . ?
C4 C3 1.391(15) . ?
C3 C2 1.399(17) . ?
C2 H2A 0.9500 . ?
C2 N2 1.325(16) . ?
N2 H2B 0.8800 . ?
N2 C1 1.366(16) . ?
C1 H1A 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.412(17) . ?
C8 C9 1.384(19) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?

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
C6 Pd1 C6 89.6(4) 6_565 . ?
C6 Pd1 C5 90.2(3) . 6_565 ?
C6 Pd1 C5 179.0(3) 6_565 6_565 ?
C6 Pd1 C5 179.0(3) . . ?
C6 Pd1 C5 90.2(3) 6_565 . ?
C5 Pd1 C5 90.1(4) 6_565 . ?
N3 Fe1 N3 180.0(4) . 5_677 ?
N3 Fe1 N3 90.4(3) . 2_657 ?
N3 Fe1 N3 90.4(3) 5_677 6_575 ?
N3 Fe1 N3 180.0 6_575 2_657 ?
N3 Fe1 N3 89.6(3) 5_677 2_657 ?
N3 Fe1 N3 89.6(3) . 6_575 ?
N3 Fe1 N1 91.4(3) . . ?
N3 Fe1 N1 91.4(3) 5_677 5_677 ?
N3 Fe1 N1 88.6(3) 2_657 . ?
N3 Fe1 N1 88.6(3) . 5_677 ?
N3 Fe1 N1 91.4(3) 6_575 . ?
N3 Fe1 N1 91.4(3) 2_657 5_677 ?
N3 Fe1 N1 88.6(3) 5_677 . ?
N3 Fe1 N1 88.6(3) 6_575 5_677 ?
N1 Fe1 N1 180.0 . 5_677 ?
N4 Fe2 N4 90.3(3) 5_656 2_656 ?
N4 Fe2 N4 180.0 . 5_656 ?
N4 Fe2 N4 89.7(3) . 2_656 ?
N4 Fe2 N4 90.3(3) . 6 ?
N4 Fe2 N4 89.7(3) 5_656 6 ?
N4 Fe2 N4 180.0 6 2_656 ?
N4 Fe2 N5 90.9(3) . . ?
N4 Fe2 N5 89.1(3) 2_656 . ?
N4 Fe2 N5 89.1(3) 5_656 . ?
N4 Fe2 N5 90.9(3) 5_656 5_656 ?
N4 Fe2 N5 89.1(3) . 5_656 ?
N4 Fe2 N5 90.9(3) 6 . ?
N4 Fe2 N5 89.1(3) 6 5_656 ?
N4 Fe2 N5 90.9(3) 2_656 5_656 ?
N5 Fe2 N5 180.0 . 5_656 ?
C5 N3 Fe1 177.5(6) . . ?
C4 N1 Fe1 122.1(7) . . ?
C1 N1 Fe1 120.5(8) . . ?
C1 N1 C4 117.5(10) . . ?
H2 O2 H2 42.8 . 6_575 ?
C3 O2 H2 109(4) . 6_575 ?
C3 O2 H2 109.5 . . ?
N4 C6 Pd1 175.3(6) . . ?
C6 N4 Fe2 172.0(6) . . ?
C7 N5 Fe2 120.5(8) . . ?
C7 N5 C10 117.6(10) . . ?
C10 N5 Fe2 121.9(7) . . ?
H1 O1 H1 21.7 . 6 ?
C8 O1 H1 109.5 . . ?
C8 O1 H1 109.5(8) . 6 ?
C9 N6 C10 117.4(10) . . ?
N3 C5 Pd1 178.7(6) . . ?
N1 C4 H4 119.2 . . ?
N1 C4 C3 121.6(10) . . ?
C3 C4 H4 119.2 . . ?
O2 C3 C4 124.2(11) . . ?
O2 C3 C2 118.6(10) . . ?
C4 C3 C2 117.2(10) . . ?
C3 C2 H2A 119.5 . . ?
N2 C2 C3 121.0(11) . . ?
N2 C2 H2A 119.5 . . ?
C2 N2 H2B 121.5 . . ?
C2 N2 C1 117.1(11) . . ?
C1 N2 H2B 121.5 . . ?
N1 C1 N2 125.7(12) . . ?
N1 C1 H1A 117.2 . . ?
N2 C1 H1A 117.2 . . ?
N5 C7 H7 119.6 . . ?
N5 C7 C8 120.8(11) . . ?
C8 C7 H7 119.6 . . ?
O1 C8 C7 122.1(12) . . ?
O1 C8 C9 121.5(12) . . ?
C9 C8 C7 116.3(11) . . ?
N6 C9 C8 122.8(11) . . ?
N6 C9 H9 118.6 . . ?
C8 C9 H9 118.6 . . ?
N5 C10 H10 117.4 . . ?
N6 C10 N5 125.1(11) . . ?
N6 C10 H10 117.4 . . ?

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 C4 C3 180.000(7) . . . . ?
Fe1 N1 C1 N2 180.000(5) . . . . ?
Fe2 N5 C7 C8 180.000(3) . . . . ?
Fe2 N5 C10 N6 180.000(2) . . . . ?
N1 C4 C3 O2 180.000(8) . . . . ?
N1 C4 C3 C2 0.000(8) . . . . ?
O2 C3 C2 N2 180.000(7) . . . . ?
N5 C7 C8 O1 180.000(3) . . . . ?
N5 C7 C8 C9 0.000(4) . . . . ?
O1 C8 C9 N6 180.000(2) . . . . ?
C4 N1 C1 N2 0.000(8) . . . . ?
C4 C3 C2 N2 0.000(8) . . . . ?
C3 C2 N2 C1 0.000(8) . . . . ?
C2 N2 C1 N1 0.000(8) . . . . ?
C1 N1 C4 C3 0.000(9) . . . . ?
C7 N5 C10 N6 0.000(3) . . . . ?
C7 C8 C9 N6 0.000(3) . . . . ?
C9 N6 C10 N5 0.000(2) . . . . ?
C10 N5 C7 C8 0.000(4) . . . . ?
C10 N6 C9 C8 0.000(3) . . . . ?

_shelx_res_file                  
;
TITL RT366_FeOHPmdPd_200K_0m_a.res in C2/m
    rt366_feohpmdpd_200k_0m_a.res
    created by SHELXL-2018/3 at 23:16:14 on 19-May-2022
CELL 0.71073 21.0937 7.1552 14.3204 90 132.571 90
ZERR 4 0.0016 0.0005 0.0011 0 0.002 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pd
UNIT 48 36 4 32 12 4

L.S. 10
PLAN  2 0 0
TEMP -73.15
CONF
HTAB
BOND $H
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\RT366_FeOHPmdPd_200K_0m_a.hkl">
REM </olex2.extras>

WGHT    0.047700   61.176998
FVAR       0.21170
PD1   6    0.484661    0.500000    0.733223    10.50000    0.02068    0.01051 =
         0.01896    0.00000    0.01443    0.00000
FE1   3    0.500000    1.000000    1.000000    10.25000    0.02693    0.01110 =
         0.02128    0.00000    0.01981    0.00000
FE2   3    0.500000    0.000000    0.500000    10.25000    0.02603    0.01203 =
         0.01868    0.00000    0.01764    0.00000
N3    4    0.498099    0.809150    0.902033    11.00000    0.02426    0.01852 =
         0.02087    0.00130    0.01679    0.00052
N1    4    0.370339    1.000000    0.878492    10.50000    0.02439    0.01411 =
         0.02633    0.00000    0.01665    0.00000
O2    5    0.193859    1.000000    0.869049    10.50000    0.02721    0.06780 =
         0.02902    0.00000    0.01994    0.00000
AFIX 147
H2    2    0.224499    0.957201    0.942925    10.50000   -1.50000
AFIX   0
C6    1    0.477695    0.304627    0.628206    11.00000    0.02293    0.01530 =
         0.02102    0.00135    0.01647   -0.00168
N4    4    0.479747    0.191642    0.572429    11.00000    0.02618    0.01566 =
         0.02140   -0.00131    0.01807   -0.00197
N5    4    0.375882    0.000000    0.341047    10.50000    0.02364    0.01612 =
         0.02224    0.00000    0.01466    0.00000
O1    5    0.166228    0.000000    0.235475    10.50000    0.03484    0.07680 =
         0.04414    0.00000    0.02842    0.00000
AFIX  83
H1    2    0.187502   -0.022062    0.309463    10.50000   -1.50000
AFIX   0
N6    4    0.269201    0.000000    0.116087    10.50000    0.03681    0.03799 =
         0.02757    0.00000    0.02222    0.00000
C5    1    0.493834    0.697039    0.840191    11.00000    0.03225    0.01402 =
         0.02674    0.00239    0.02412    0.00202
C4    1    0.328701    1.000000    0.918725    10.50000    0.02562    0.02285 =
         0.02647    0.00000    0.01871    0.00000
AFIX  43
H4    2    0.360969    1.000000    1.007232    10.50000   -1.20000
AFIX   0
C3    1    0.239268    1.000000    0.834052    10.50000    0.02104    0.02944 =
         0.03079    0.00000    0.01802    0.00000
C2    1    0.194431    1.000000    0.704668    10.50000    0.02676    0.04599 =
         0.02828    0.00000    0.01664    0.00000
AFIX  43
H2A   2    0.133277    1.000000    0.644162    10.50000   -1.20000
AFIX   0
N2    4    0.235931    1.000000    0.665196    10.50000    0.04025    0.03290 =
         0.02713    0.00000    0.02295    0.00000
AFIX  43
H2B   2    0.208106    1.000000    0.583942    10.50000   -1.20000
AFIX   0
C1    1    0.323794    1.000000    0.756153    10.50000    0.03517    0.02873 =
         0.02788    0.00000    0.01954    0.00000
AFIX  43
H1A   2    0.353644    1.000000    0.727999    10.50000   -1.20000
AFIX   0
C7    1    0.316017    0.000000    0.345815    10.50000    0.03611    0.01849 =
         0.03523    0.00000    0.02764    0.00000
AFIX  43
H7    2    0.332029    0.000000    0.425795    10.50000   -1.20000
AFIX   0
C8    1    0.227984    0.000000    0.233546    10.50000    0.03098    0.02390 =
         0.05304    0.00000    0.03023    0.00000
C9    1    0.209598    0.000000    0.120662    10.50000    0.02262    0.02993 =
         0.02638    0.00000    0.01065    0.00000
AFIX  43
H9    2    0.151022    0.000000    0.043231    10.50000   -1.20000
AFIX   0
C10   1    0.350096    0.000000    0.225044    10.50000    0.02783    0.02704 =
         0.02137    0.00000    0.01630    0.00000
AFIX  43
H10   2    0.393600    0.000000    0.221771    10.50000   -1.20000
AFIX   0

PART -1
O3    5    0.231340    0.081661    0.471458    10.50000    0.07057
HKLF 4




REM  RT366_FeOHPmdPd_200K_0m_a.res in C2/m
REM wR2 = 0.1789, GooF = S = 1.178, Restrained GooF = 1.178 for all data
REM R1 = 0.0677 for 1893 Fo > 4sig(Fo) and 0.0780 for all 2138 data
REM 140 parameters refined using 0 restraints

END

WGHT      0.0477     61.2275

REM Instructions for potential hydrogen bonds
EQIV $8 x, y+1, z+1
HTAB O2 N6_$8
HTAB O1 O3
EQIV $7 x, -y, z
HTAB O1 O3_$7
EQIV $9 x, y+1, z
HTAB N2 O3_$9
EQIV $4 x, -y+1, z
HTAB N2 O3_$4

REM Highest difference peak  3.754,  deepest hole -1.756,  1-sigma level  0.251
Q1    1   0.4886  0.5000  0.7976  10.50000  0.05    3.75
Q2    1   0.4810  0.5000  0.6693  10.50000  0.05    3.30
;
_shelx_res_checksum              7465
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rt340_ohpmdpt_120k_0m
_database_code_depnum_ccdc_archive 'CCDC 2209616'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
_audit_creation_date             2022-05-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H9 Fe N8 O2 Pt, H2 O'
_chemical_formula_sum            'C12 H11 Fe N8 O3 Pt'
_chemical_formula_weight         566.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.078(4)
_cell_length_b                   7.1279(13)
_cell_length_c                   14.407(2)
_cell_angle_alpha                90
_cell_angle_beta                 132.274(8)
_cell_angle_gamma                90
_cell_volume                     1601.7(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    120.02
_cell_measurement_theta_max      30.61
_cell_measurement_theta_min      2.84
_shelx_estimated_absorpt_T_max   0.760
_shelx_estimated_absorpt_T_min   0.160
_exptl_absorpt_coefficient_mu    9.662
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0963 before and 0.0342 after correction.
The Ratio of minimum to maximum transmission is 0.6783.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.348
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12214
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.487
_diffrn_reflns_theta_min         2.828
_diffrn_ambient_temperature      120.02
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2505
_reflns_number_total             2588
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2588
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0135
_refine_ls_R_factor_gt           0.0127
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0072P)²+3.7622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0292
_refine_ls_wR_factor_ref         0.0295
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H2(0.5) O3(0.5) H3A(0.5) H3B(0.5)
3.a Free rotating group:
 O3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C4(H4), C7(H7), C9(H9), C10(H10)
3.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.48398(2) 0.500000 0.23541(2) 0.00749(3) Uani 1 2 d S T P . .
Fe1 Fe 0.500000 0.000000 0.000000 0.00765(8) Uani 1 4 d S T P . .
Fe2 Fe 0.500000 1.000000 0.500000 0.00881(9) Uani 1 4 d S T P . .
O1 O 0.80531(13) 0.000000 0.47580(19) 0.0273(5) Uani 1 2 d S T P . .
H1 H 0.775616 -0.047542 0.489151 0.041 Uiso 1 1 calc R U . . .
O2 O 0.83564(14) 1.000000 0.8995(2) 0.0318(5) Uani 1 2 d S T P . .
H2 H 0.817026 0.955947 0.931368 0.048 Uiso 0.5 1 calc R U P . .
N1 N 0.62890(14) 0.000000 0.1365(2) 0.0125(4) Uani 1 2 d S T P . .
N2 N 0.76329(15) 0.000000 0.1897(2) 0.0212(5) Uani 1 2 d S T P . .
N3 N 0.49521(9) 0.1912(2) 0.09084(13) 0.0113(3) Uani 1 1 d . . . . .
N4 N 0.48106(10) 0.8078(2) 0.38849(14) 0.0129(3) Uani 1 1 d . . . . .
N5 N 0.62451(14) 1.000000 0.5879(2) 0.0125(4) Uani 1 2 d S T P . .
N6 N 0.73005(15) 1.000000 0.5728(2) 0.0201(5) Uani 1 2 d S T P . .
C1 C 0.67746(17) 0.000000 0.1069(3) 0.0169(5) Uani 1 2 d S T P . .
H1A H 0.648467 0.000000 0.020377 0.020 Uiso 1 2 calc R U P . .
C2 C 0.80432(18) 0.000000 0.3114(3) 0.0211(6) Uani 1 2 d S T P . .
H2A H 0.865232 0.000000 0.371758 0.025 Uiso 1 2 calc R U P . .
C3 C 0.76039(18) 0.000000 0.3525(3) 0.0182(5) Uani 1 2 d S T P . .
C4 C 0.67051(17) 0.000000 0.2593(2) 0.0150(5) Uani 1 2 d S T P . .
H4 H 0.638248 0.000000 0.283504 0.018 Uiso 1 2 calc R U P . .
C5 C 0.49112(11) 0.3033(2) 0.14452(16) 0.0111(3) Uani 1 1 d . . . . .
C6 C 0.47938(11) 0.6956(2) 0.32915(16) 0.0119(3) Uani 1 1 d . . . . .
C7 C 0.68618(18) 1.000000 0.7141(3) 0.0179(5) Uani 1 2 d S T P . .
H7 H 0.670725 1.000000 0.762659 0.021 Uiso 1 2 calc R U P . .
C8 C 0.77261(19) 1.000000 0.7740(3) 0.0237(6) Uani 1 2 d S T P . .
C9 C 0.79163(19) 1.000000 0.6980(3) 0.0231(6) Uani 1 2 d S T P . .
H9 H 0.849932 1.000000 0.736310 0.028 Uiso 1 2 calc R U P . .
C10 C 0.64903(17) 1.000000 0.5226(3) 0.0160(5) Uani 1 2 d S T P . .
H10 H 0.605195 1.000000 0.433664 0.019 Uiso 1 2 calc R U P . .
O3 O 0.7669(2) 0.9215(8) 1.0010(3) 0.0588(19) Uani 0.5 1 d G . P A -1
H3A H 0.773279 0.820041 1.040176 0.088 Uiso 0.5 1 d G U P A -1
H3B H 0.782687 1.011822 1.053395 0.088 Uiso 0.5 1 d G U P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.01036(4) 0.00602(4) 0.00772(4) 0.000 0.00674(4) 0.000
Fe1 0.0101(2) 0.00651(19) 0.00793(19) 0.000 0.00671(18) 0.000
Fe2 0.0137(2) 0.0063(2) 0.0090(2) 0.000 0.00873(19) 0.000
O1 0.0156(9) 0.0483(15) 0.0143(9) 0.000 0.0086(8) 0.000
O2 0.0197(10) 0.0500(15) 0.0146(10) 0.000 0.0070(9) 0.000
N1 0.0126(9) 0.0110(9) 0.0131(9) 0.000 0.0084(8) 0.000
N2 0.0164(11) 0.0284(13) 0.0220(12) 0.000 0.0143(10) 0.000
N3 0.0142(6) 0.0098(6) 0.0114(6) 0.0001(5) 0.0092(6) -0.0002(5)
N4 0.0186(7) 0.0105(7) 0.0133(6) 0.0005(5) 0.0122(6) -0.0003(5)
N5 0.0151(9) 0.0092(9) 0.0131(9) 0.000 0.0094(9) 0.000
N6 0.0183(11) 0.0218(12) 0.0222(12) 0.000 0.0144(10) 0.000
C1 0.0155(11) 0.0205(12) 0.0178(12) 0.000 0.0124(11) 0.000
C2 0.0184(12) 0.0246(14) 0.0212(13) 0.000 0.0137(12) 0.000
C3 0.0194(12) 0.0177(12) 0.0150(12) 0.000 0.0106(11) 0.000
C4 0.0172(12) 0.0151(11) 0.0145(11) 0.000 0.0114(10) 0.000
C5 0.0128(7) 0.0104(7) 0.0107(7) 0.0012(6) 0.0082(6) 0.0001(6)
C6 0.0169(8) 0.0100(7) 0.0124(7) 0.0008(6) 0.0113(7) -0.0004(6)
C7 0.0216(13) 0.0153(12) 0.0143(12) 0.000 0.0110(11) 0.000
C8 0.0202(13) 0.0196(13) 0.0163(13) 0.000 0.0062(11) 0.000
C9 0.0198(13) 0.0202(13) 0.0237(14) 0.000 0.0123(12) 0.000
C10 0.0176(12) 0.0160(12) 0.0175(12) 0.000 0.0130(11) 0.000
O3 0.0202(15) 0.135(6) 0.0196(14) 0.018(2) 0.0127(14) 0.001(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
Pt1 C5 1.9921(17) 6_565 ?
Pt1 C5 1.9920(17) . ?
Pt1 C6 1.9886(17) . ?
Pt1 C6 1.9886(17) 6_565 ?
Fe1 N1 2.015(2) 5_655 ?
Fe1 N1 2.015(2) . ?
Fe1 N3 1.9386(15) 6 ?
Fe1 N3 1.9386(15) 5_655 ?
Fe1 N3 1.9386(15) 2_655 ?
Fe1 N3 1.9385(15) . ?
Fe2 N4 1.9377(15) 5_676 ?
Fe2 N4 1.9377(15) 2_656 ?
Fe2 N4 1.9377(15) . ?
Fe2 N4 1.9377(15) 6_575 ?
Fe2 N5 2.005(2) . ?
Fe2 N5 2.005(2) 5_676 ?
O1 H1 0.8400 . ?
O1 H1 0.84(2) 6 ?
O1 C3 1.338(3) . ?
O2 H2 0.8400 . ?
O2 H2 0.84(4) 6_575 ?
O2 C8 1.343(3) . ?
N1 C1 1.347(3) . ?
N1 C4 1.347(3) . ?
N2 C1 1.339(3) . ?
N2 C2 1.335(4) . ?
N3 C5 1.155(2) . ?
N4 C6 1.153(2) . ?
N5 C7 1.347(3) . ?
N5 C10 1.345(3) . ?
N6 C9 1.337(4) . ?
N6 C10 1.333(3) . ?
C1 H1A 0.9500 . ?
C2 H2A 0.9500 . ?
C2 C3 1.395(4) . ?
C3 C4 1.403(4) . ?
C4 H4 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.396(4) . ?
C8 C9 1.396(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
O3 H3A 0.8709 . ?
O3 H3B 0.8701 . ?

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
C5 Pt1 C5 89.47(10) . 6_565 ?
C6 Pt1 C5 90.73(7) . 6_565 ?
C6 Pt1 C5 90.72(7) 6_565 . ?
C6 Pt1 C5 178.84(7) 6_565 6_565 ?
C6 Pt1 C5 178.84(7) . . ?
C6 Pt1 C6 89.05(10) 6_565 . ?
N1 Fe1 N1 180.0 5_655 . ?
N3 Fe1 N1 90.59(6) . 5_655 ?
N3 Fe1 N1 90.58(6) 5_655 . ?
N3 Fe1 N1 90.58(6) 2_655 . ?
N3 Fe1 N1 89.41(6) 5_655 5_655 ?
N3 Fe1 N1 89.42(6) 6 . ?
N3 Fe1 N1 90.59(6) 6 5_655 ?
N3 Fe1 N1 89.41(6) 2_655 5_655 ?
N3 Fe1 N1 89.41(6) . . ?
N3 Fe1 N3 89.32(9) 5_655 2_655 ?
N3 Fe1 N3 180.0 . 5_655 ?
N3 Fe1 N3 90.68(9) . 2_655 ?
N3 Fe1 N3 180.00(10) 6 2_655 ?
N3 Fe1 N3 89.32(9) . 6 ?
N3 Fe1 N3 90.68(9) 5_655 6 ?
N4 Fe2 N4 89.99(9) . 6_575 ?
N4 Fe2 N4 90.01(9) . 2_656 ?
N4 Fe2 N4 180.0 6_575 2_656 ?
N4 Fe2 N4 89.99(9) 5_676 2_656 ?
N4 Fe2 N4 180.0 . 5_676 ?
N4 Fe2 N4 90.01(9) 5_676 6_575 ?
N4 Fe2 N5 88.62(6) . . ?
N4 Fe2 N5 91.38(6) . 5_676 ?
N4 Fe2 N5 88.62(6) 2_656 5_676 ?
N4 Fe2 N5 91.38(6) 5_676 . ?
N4 Fe2 N5 88.62(6) 5_676 5_676 ?
N4 Fe2 N5 88.62(6) 6_575 . ?
N4 Fe2 N5 91.38(6) 2_656 . ?
N4 Fe2 N5 91.38(6) 6_575 5_676 ?
N5 Fe2 N5 180.0 . 5_676 ?
H1 O1 H1 47.6 . 6 ?
C3 O1 H1 109.5 . . ?
C3 O1 H1 109.5(5) . 6 ?
H2 O2 H2 43.9 . 6_575 ?
C8 O2 H2 109.5(10) . 6_575 ?
C8 O2 H2 109.5 . . ?
C1 N1 Fe1 120.27(18) . . ?
C4 N1 Fe1 122.73(18) . . ?
C4 N1 C1 117.0(2) . . ?
C2 N2 C1 117.6(2) . . ?
C5 N3 Fe1 178.74(15) . . ?
C6 N4 Fe2 172.33(15) . . ?
C7 N5 Fe2 121.17(19) . . ?
C10 N5 Fe2 120.92(18) . . ?
C10 N5 C7 117.9(2) . . ?
C10 N6 C9 117.3(3) . . ?
N1 C1 H1A 117.4 . . ?
N2 C1 N1 125.3(3) . . ?
N2 C1 H1A 117.4 . . ?
N2 C2 H2A 119.0 . . ?
N2 C2 C3 121.9(3) . . ?
C3 C2 H2A 119.0 . . ?
O1 C3 C2 119.0(3) . . ?
O1 C3 C4 124.4(3) . . ?
C2 C3 C4 116.6(3) . . ?
N1 C4 C3 121.6(2) . . ?
N1 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
N3 C5 Pt1 179.05(16) . . ?
N4 C6 Pt1 176.56(16) . . ?
N5 C7 H7 119.7 . . ?
N5 C7 C8 120.5(3) . . ?
C8 C7 H7 119.7 . . ?
O2 C8 C7 122.0(3) . . ?
O2 C8 C9 120.7(3) . . ?
C7 C8 C9 117.3(3) . . ?
N6 C9 C8 121.8(3) . . ?
N6 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
N5 C10 H10 117.4 . . ?
N6 C10 N5 125.1(3) . . ?
N6 C10 H10 117.4 . . ?
H3A O3 H3B 104.4 . . ?

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 N2 180.000(0) . . . . ?
Fe1 N1 C4 C3 180.000(1) . . . . ?
Fe2 N5 C7 C8 180.000(1) . . . . ?
Fe2 N5 C10 N6 180.000(1) . . . . ?
O1 C3 C4 N1 180.000(1) . . . . ?
O2 C8 C9 N6 180.000(2) . . . . ?
N2 C2 C3 O1 180.000(1) . . . . ?
N2 C2 C3 C4 0.000(1) . . . . ?
N5 C7 C8 O2 180.000(1) . . . . ?
N5 C7 C8 C9 0.000(2) . . . . ?
C1 N1 C4 C3 0.000(1) . . . . ?
C1 N2 C2 C3 0.000(1) . . . . ?
C2 N2 C1 N1 0.000(0) . . . . ?
C2 C3 C4 N1 0.000(1) . . . . ?
C4 N1 C1 N2 0.000(0) . . . . ?
C7 N5 C10 N6 0.000(2) . . . . ?
C7 C8 C9 N6 0.000(2) . . . . ?
C9 N6 C10 N5 0.000(2) . . . . ?
C10 N5 C7 C8 0.000(2) . . . . ?
C10 N6 C9 C8 0.000(2) . . . . ?

_shelx_res_file                  
;
TITL rt340_ohpmdpt_120k_0m_a.res in C2/m
    rt340_ohpmdpt_120k_0m.res
    created by SHELXL-2018/3 at 23:19:41 on 19-May-2022
REM Old TITL Integration of RT340_OHPmdPt_120K
REM SHELXT solution in C2/m: R1 0.175, Rweak 0.017, Alpha 0.019
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C24 I
CELL 0.71073 21.0783 7.1279 14.4071 90 132.274 90
ZERR 4 0.0038 0.0013 0.0023 0 0.008 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pt
UNIT 48 44 4 32 12 4

L.S. 15
PLAN  5
SIZE 0.3 0.3 0.03
TEMP -153.13
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
OMIT 2 0 0
REM <olex2.extras>
REM <HklSrc "%.\\RT340_OHPmdPt_120K_0m.hkl">
REM </olex2.extras>

WGHT    0.007200    3.762200
FVAR       0.20471
PT1   6    0.483984    0.500000    0.235407    10.50000    0.01036    0.00602 =
         0.00772    0.00000    0.00674    0.00000
FE1   3    0.500000    0.000000    0.000000    10.25000    0.01010    0.00651 =
         0.00793    0.00000    0.00671    0.00000
FE2   3    0.500000    1.000000    0.500000    10.25000    0.01372    0.00632 =
         0.00904    0.00000    0.00873    0.00000
O1    5    0.805310    0.000000    0.475797    10.50000    0.01560    0.04829 =
         0.01432    0.00000    0.00855    0.00000
AFIX 147
H1    2    0.775616   -0.047542    0.489151    11.00000   -1.50000
AFIX   0
O2    5    0.835636    1.000000    0.899498    10.50000    0.01966    0.04999 =
         0.01460    0.00000    0.00701    0.00000
AFIX 147
H2    2    0.817026    0.955947    0.931368    10.50000   -1.50000
AFIX   0
N1    4    0.628903    0.000000    0.136451    10.50000    0.01265    0.01099 =
         0.01312    0.00000    0.00840    0.00000
N2    4    0.763294    0.000000    0.189670    10.50000    0.01644    0.02840 =
         0.02203    0.00000    0.01425    0.00000
N3    4    0.495207    0.191172    0.090843    11.00000    0.01420    0.00979 =
         0.01136    0.00013    0.00920   -0.00016
N4    4    0.481062    0.807790    0.388486    11.00000    0.01856    0.01051 =
         0.01325    0.00055    0.01217   -0.00026
N5    4    0.624510    1.000000    0.587942    10.50000    0.01506    0.00923 =
         0.01314    0.00000    0.00944    0.00000
N6    4    0.730053    1.000000    0.572846    10.50000    0.01827    0.02179 =
         0.02224    0.00000    0.01439    0.00000
C1    1    0.677460    0.000000    0.106901    10.50000    0.01552    0.02052 =
         0.01777    0.00000    0.01243    0.00000
AFIX  43
H1A   2    0.648467    0.000000    0.020377    10.50000   -1.20000
AFIX   0
C2    1    0.804322    0.000000    0.311371    10.50000    0.01839    0.02460 =
         0.02125    0.00000    0.01373    0.00000
AFIX  43
H2A   2    0.865232    0.000000    0.371758    10.50000   -1.20000
AFIX   0
C3    1    0.760392    0.000000    0.352497    10.50000    0.01943    0.01775 =
         0.01499    0.00000    0.01062    0.00000
C4    1    0.670512    0.000000    0.259329    10.50000    0.01719    0.01513 =
         0.01455    0.00000    0.01143    0.00000
AFIX  43
H4    2    0.638248    0.000000    0.283504    10.50000   -1.20000
AFIX   0
C5    1    0.491122    0.303294    0.144519    11.00000    0.01284    0.01039 =
         0.01075    0.00122    0.00820    0.00006
C6    1    0.479377    0.695639    0.329151    11.00000    0.01689    0.00995 =
         0.01238    0.00077    0.01133   -0.00040
C7    1    0.686176    1.000000    0.714082    10.50000    0.02158    0.01526 =
         0.01433    0.00000    0.01104    0.00000
AFIX  43
H7    2    0.670725    1.000000    0.762659    10.50000   -1.20000
AFIX   0
C8    1    0.772614    1.000000    0.773999    10.50000    0.02018    0.01957 =
         0.01632    0.00000    0.00616    0.00000
C9    1    0.791629    1.000000    0.698016    10.50000    0.01978    0.02017 =
         0.02374    0.00000    0.01230    0.00000
AFIX  43
H9    2    0.849932    1.000000    0.736310    10.50000   -1.20000
AFIX   0
C10   1    0.649031    1.000000    0.522589    10.50000    0.01757    0.01601 =
         0.01748    0.00000    0.01298    0.00000
AFIX  43
H10   2    0.605195    1.000000    0.433664    10.50000   -1.20000
AFIX   6

PART -1
O3    5    0.766920    0.921539    1.000983    10.50000    0.02019    0.13503 =
         0.01964    0.01801    0.01275    0.00078
H3A   2    0.773279    0.820041    1.040176    10.50000   -1.50000
H3B   2    0.782687    1.011822    1.053395    10.50000   -1.50000
AFIX   0
HKLF 4




REM  rt340_ohpmdpt_120k_0m_a.res in C2/m
REM wR2 = 0.0295, GooF = S = 1.094, Restrained GooF = 1.094 for all data
REM R1 = 0.0127 for 2505 Fo > 4sig(Fo) and 0.0135 for all 2588 data
REM 149 parameters refined using 0 restraints

END

WGHT      0.0073      3.7550

REM Highest difference peak  0.725,  deepest hole -0.890,  1-sigma level  0.100
Q1    1   0.7687  1.0000  0.8414  10.50000  0.05    0.73
Q2    1   0.5301  0.5000  0.3312  10.50000  0.05    0.61
Q3    1   0.7292  0.0000  0.3907  10.50000  0.05    0.60
Q4    1   0.5452  0.5000  0.2221  10.50000  0.05    0.56
Q5    1   0.6485  1.0000  0.6496  10.50000  0.05    0.51
;
_shelx_res_checksum              54565
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_rt340_ohpmdpt_260kdes_0ma
_database_code_depnum_ccdc_archive 'CCDC 2209613'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_mo_rt340_ohpmdpt_260kdes_0ma 
;
PROBLEM: Check Calcd Resid. Dens.  1.52Ang From C6             -3.61 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT420_mo_rt340_ohpmdpt_260kdes_0ma 
;
PROBLEM: D-H Bond Without Acceptor  O2       --H2       .     Please Check
RESPONSE: The O2 atom is not involved in H-bonding interactions
;
# Added during the CSD deposition process: Monday 26 September 2022 03:56 PM
# end Validation Reply Form

_audit_creation_date             2022-06-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H8 Fe N8 O2 Pt'
_chemical_formula_sum            'C12 H8 Fe N8 O2 Pt'
_chemical_formula_weight         547.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   14.6027(8)
_cell_length_b                   7.3612(5)
_cell_length_c                   15.6975(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1687.38(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    259.81
_cell_measurement_theta_max      36.17
_cell_measurement_theta_min      2.79
_shelx_estimated_absorpt_T_max   0.771
_shelx_estimated_absorpt_T_min   0.170
_exptl_absorpt_coefficient_mu    9.163
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5049
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0908 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.6758.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_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            30240
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.246
_diffrn_reflns_theta_min         2.790
_diffrn_ambient_temperature      259.81
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3715
_reflns_number_total             4316
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.158
_refine_diff_density_min         -3.493
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         4316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0287
_refine_ls_restrained_S_all      1.175
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+5.7295P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0541
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H2(0.5) H1(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C7(H7), C4(H4), C2(H2A), C1(H1A)
3.b Idealised tetrahedral OH refined as rotating group:
 O2(H2), O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.53135(2) 0.250000 0.23030(2) 0.01424(3) Uani 1 2 d S T P . .
Fe1 Fe 0.77968(3) 0.750000 0.29002(3) 0.01439(9) Uani 1 2 d S T P . .
O2 O 0.6661(4) 0.750000 -0.0410(3) 0.090(2) Uani 1 2 d S T P . .
H2 H 0.679924 0.724853 -0.090248 0.135 Uiso 0.5 1 calc R U P . .
O1 O 0.5559(3) 0.750000 0.5718(3) 0.0726(19) Uani 1 2 d S T P . .
H1 H 0.521119 0.795261 0.536706 0.109 Uiso 0.5 1 calc R U P . .
N5 N 0.8022(3) 0.750000 0.1476(2) 0.0269(7) Uani 1 2 d S T P . .
N6 N 0.9027(3) 0.750000 0.0295(3) 0.0439(12) Uani 1 2 d S T P . .
N3 N 0.67793(16) 0.5469(4) 0.27155(18) 0.0252(5) Uani 1 1 d . . . . .
N4 N 0.38174(17) -0.0463(4) 0.19857(18) 0.0253(5) Uani 1 1 d . . . . .
N1 N 0.7490(3) 0.750000 0.4278(2) 0.0252(7) Uani 1 2 d S T P . .
N2 N 0.8003(3) 0.750000 0.5705(3) 0.0548(16) Uani 1 2 d S T P . .
C10 C 0.8853(4) 0.750000 0.1121(3) 0.0345(11) Uani 1 2 d S T P . .
H10 H 0.935317 0.750000 0.148741 0.041 Uiso 1 2 calc R U P . .
C9 C 0.8301(5) 0.750000 -0.0234(3) 0.0475(15) Uani 1 2 d S T P . .
H9 H 0.839681 0.750000 -0.081945 0.057 Uiso 1 2 calc R U P . .
C8 C 0.7417(4) 0.750000 0.0076(4) 0.0474(15) Uani 1 2 d S T P . .
C7 C 0.7305(4) 0.750000 0.0949(3) 0.0347(11) Uani 1 2 d S T P . .
H7 H 0.671693 0.750000 0.117513 0.042 Uiso 1 2 calc R U P . .
C5 C 0.62359(18) 0.4391(4) 0.25583(18) 0.0184(5) Uani 1 1 d . . . . .
C6 C 0.43802(18) 0.0608(4) 0.20820(18) 0.0197(5) Uani 1 1 d . . . . .
C4 C 0.6628(3) 0.750000 0.4547(3) 0.0306(10) Uani 1 2 d S T P . .
H4 H 0.615543 0.750000 0.414966 0.037 Uiso 1 2 calc R U P . .
C3 C 0.6417(4) 0.750000 0.5406(3) 0.0395(13) Uani 1 2 d S T P . .
C2 C 0.7137(4) 0.750000 0.5968(4) 0.0517(17) Uani 1 2 d S T P . .
H2A H 0.701585 0.750000 0.654954 0.062 Uiso 1 2 calc R U P . .
C1 C 0.8138(4) 0.750000 0.4872(3) 0.0384(12) Uani 1 2 d S T P . .
H1A H 0.874244 0.750000 0.468474 0.046 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.01049(5) 0.01034(5) 0.02190(6) 0.000 -0.00125(5) 0.000
Fe1 0.01111(19) 0.0110(2) 0.0210(2) 0.000 -0.00012(17) 0.000
O2 0.066(3) 0.167(7) 0.036(3) 0.000 -0.031(3) 0.000
O1 0.031(2) 0.163(6) 0.0239(19) 0.000 0.0052(16) 0.000
N5 0.0278(18) 0.0308(19) 0.0220(16) 0.000 -0.0046(14) 0.000
N6 0.043(3) 0.063(3) 0.025(2) 0.000 0.0071(19) 0.000
N3 0.0207(10) 0.0229(11) 0.0319(13) -0.0016(10) -0.0009(10) -0.0066(9)
N4 0.0209(10) 0.0205(11) 0.0345(13) 0.0001(10) -0.0016(10) -0.0073(9)
N1 0.0237(16) 0.0296(19) 0.0222(16) 0.000 -0.0017(13) 0.000
N2 0.035(2) 0.103(5) 0.027(2) 0.000 -0.0076(19) 0.000
C10 0.034(2) 0.045(3) 0.025(2) 0.000 0.0011(18) 0.000
C9 0.059(4) 0.063(4) 0.021(2) 0.000 0.001(2) 0.000
C8 0.051(3) 0.065(4) 0.026(2) 0.000 -0.014(2) 0.000
C7 0.030(2) 0.045(3) 0.028(2) 0.000 -0.0058(19) 0.000
C5 0.0173(10) 0.0142(10) 0.0238(12) -0.0008(9) -0.0004(9) -0.0004(9)
C6 0.0162(10) 0.0173(11) 0.0258(12) 0.0011(9) -0.0014(9) -0.0007(9)
C4 0.026(2) 0.047(3) 0.0187(19) 0.000 0.0006(16) 0.000
C3 0.032(2) 0.065(4) 0.022(2) 0.000 0.0023(19) 0.000
C2 0.045(3) 0.087(5) 0.023(2) 0.000 -0.002(2) 0.000
C1 0.027(2) 0.060(4) 0.028(2) 0.000 -0.0032(19) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C5 1.978(3) 7_565 ?
Pt1 C5 1.978(3) . ?
Pt1 C6 1.979(3) 7_565 ?
Pt1 C6 1.979(3) . ?
Fe1 N5 2.260(4) . ?
Fe1 N3 2.128(2) . ?
Fe1 N3 2.128(2) 7_575 ?
Fe1 N4 2.122(2) 6_666 ?
Fe1 N4 2.122(2) 4 ?
Fe1 N1 2.209(4) . ?
O2 H2 0.8200 . ?
O2 H2 0.82(11) 7_575 ?
O2 C8 1.342(7) . ?
O1 H1 0.8200 . ?
O1 H1 0.82(10) 7_575 ?
O1 C3 1.345(6) . ?
N5 C10 1.335(6) . ?
N5 C7 1.334(6) . ?
N6 C10 1.321(6) . ?
N6 C9 1.347(8) . ?
N3 C5 1.149(3) . ?
N4 C6 1.149(3) . ?
N1 C4 1.329(6) . ?
N1 C1 1.328(6) . ?
N2 C2 1.330(8) . ?
N2 C1 1.322(7) . ?
C10 H10 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.379(9) . ?
C8 C7 1.380(8) . ?
C7 H7 0.9300 . ?
C4 H4 0.9300 . ?
C4 C3 1.383(7) . ?
C3 C2 1.371(8) . ?
C2 H2A 0.9300 . ?
C1 H1A 0.9300 . ?

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
C5 Pt1 C5 89.46(15) 7_565 . ?
C5 Pt1 C6 178.37(12) 7_565 7_565 ?
C5 Pt1 C6 90.53(11) . 7_565 ?
C5 Pt1 C6 178.37(12) . . ?
C5 Pt1 C6 90.53(11) 7_565 . ?
C6 Pt1 C6 89.43(16) . 7_565 ?
N3 Fe1 N5 88.10(10) . . ?
N3 Fe1 N5 88.10(10) 7_575 . ?
N3 Fe1 N3 89.30(14) 7_575 . ?
N3 Fe1 N1 89.54(10) . . ?
N3 Fe1 N1 89.54(10) 7_575 . ?
N4 Fe1 N5 88.92(11) 6_666 . ?
N4 Fe1 N5 88.92(11) 4 . ?
N4 Fe1 N3 90.30(10) 6_666 7_575 ?
N4 Fe1 N3 90.30(10) 4 . ?
N4 Fe1 N3 177.01(11) 4 7_575 ?
N4 Fe1 N3 177.01(11) 6_666 . ?
N4 Fe1 N4 89.95(15) 6_666 4 ?
N4 Fe1 N1 93.42(10) 6_666 . ?
N4 Fe1 N1 93.42(10) 4 . ?
N1 Fe1 N5 176.68(14) . . ?
H2 O2 H2 26.1 . 7_575 ?
C8 O2 H2 109(3) . 7_575 ?
C8 O2 H2 109.5 . . ?
H1 O1 H1 47.9 . 7_575 ?
C3 O1 H1 109(2) . 7_575 ?
C3 O1 H1 109.5 . . ?
C10 N5 Fe1 123.0(3) . . ?
C7 N5 Fe1 119.9(3) . . ?
C7 N5 C10 117.0(4) . . ?
C10 N6 C9 116.9(5) . . ?
C5 N3 Fe1 175.4(3) . . ?
C6 N4 Fe1 167.5(3) . 6_546 ?
C4 N1 Fe1 120.2(3) . . ?
C1 N1 Fe1 122.9(3) . . ?
C1 N1 C4 116.9(4) . . ?
C1 N2 C2 116.7(5) . . ?
N5 C10 H10 117.1 . . ?
N6 C10 N5 125.8(5) . . ?
N6 C10 H10 117.1 . . ?
N6 C9 H9 119.3 . . ?
N6 C9 C8 121.3(5) . . ?
C8 C9 H9 119.3 . . ?
O2 C8 C9 124.7(6) . . ?
O2 C8 C7 117.9(6) . . ?
C9 C8 C7 117.4(5) . . ?
N5 C7 C8 121.6(5) . . ?
N5 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
N3 C5 Pt1 178.8(3) . . ?
N4 C6 Pt1 176.9(3) . . ?
N1 C4 H4 119.3 . . ?
N1 C4 C3 121.4(5) . . ?
C3 C4 H4 119.3 . . ?
O1 C3 C4 124.1(5) . . ?
O1 C3 C2 118.7(5) . . ?
C2 C3 C4 117.2(5) . . ?
N2 C2 C3 121.9(5) . . ?
N2 C2 H2A 119.0 . . ?
C3 C2 H2A 119.0 . . ?
N1 C1 H1A 117.0 . . ?
N2 C1 N1 126.0(5) . . ?
N2 C1 H1A 117.0 . . ?

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 N5 C10 N6 180.000(0) . . . . ?
Fe1 N5 C7 C8 180.000(0) . . . . ?
Fe1 N1 C4 C3 180.000(1) . . . . ?
Fe1 N1 C1 N2 180.000(1) . . . . ?
O2 C8 C7 N5 180.000(0) . . . . ?
O1 C3 C2 N2 180.000(1) . . . . ?
N6 C9 C8 O2 180.0 . . . . ?
N6 C9 C8 C7 0.000(0) . . . . ?
N1 C4 C3 O1 180.000(1) . . . . ?
N1 C4 C3 C2 0.000(1) . . . . ?
C10 N5 C7 C8 0.000(0) . . . . ?
C10 N6 C9 C8 0.000(0) . . . . ?
C9 N6 C10 N5 0.000(0) . . . . ?
C9 C8 C7 N5 0.000(0) . . . . ?
C7 N5 C10 N6 0.000(0) . . . . ?
C4 N1 C1 N2 0.000(1) . . . . ?
C4 C3 C2 N2 0.000(1) . . . . ?
C2 N2 C1 N1 0.000(1) . . . . ?
C1 N1 C4 C3 0.000(1) . . . . ?
C1 N2 C2 C3 0.000(1) . . . . ?

_shelx_res_file                  
;
TITL mo_rt340_ohpmdpt_260kdes_0ma_a.res in Pnma
    mo_rt340_ohpmdpt_260kdes_0ma.res
    created by SHELXL-2018/3 at 11:36:36 on 14-Jun-2022
REM Old TITL mo_RT340_OHPmdPt_260Kdes_0ma in Pnma
REM SHELXT solution in Pnma
REM R1 0.079, Rweak 0.002, Alpha 0.085, Orientation as input
REM Formula found by SHELXT: C13 N11 Fe Pt
CELL 0.71073 14.6027 7.3612 15.6975 90 90 90
ZERR 4 0.0008 0.0005 0.0009 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Fe N O Pt
UNIT 48 32 4 32 8 4

L.S. 13
PLAN  5 0 0
SIZE 0.3 0.03 0.03
TEMP -13.34
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\mo_RT340_OHPmdPt_260Kdes_0ma.hkl">
REM </olex2.extras>

WGHT    0.000000    5.729500
FVAR       0.22910
PT1   6    0.531354    0.250000    0.230299    10.50000    0.01049    0.01034 =
         0.02190    0.00000   -0.00125    0.00000
FE1   3    0.779682    0.750000    0.290019    10.50000    0.01111    0.01102 =
         0.02104    0.00000   -0.00012    0.00000
O2    5    0.666091    0.750000   -0.041012    10.50000    0.06611    0.16680 =
         0.03626    0.00000   -0.03109    0.00000
AFIX 147
H2    2    0.679924    0.724853   -0.090248    10.50000   -1.50000
AFIX   0
O1    5    0.555918    0.750000    0.571782    10.50000    0.03086    0.16312 =
         0.02394    0.00000    0.00522    0.00000
AFIX 147
H1    2    0.521119    0.795261    0.536706    10.50000   -1.50000
AFIX   0
N5    4    0.802222    0.750000    0.147579    10.50000    0.02781    0.03076 =
         0.02203    0.00000   -0.00463    0.00000
N6    4    0.902702    0.750000    0.029492    10.50000    0.04304    0.06307 =
         0.02546    0.00000    0.00711    0.00000
N3    4    0.677934    0.546854    0.271551    11.00000    0.02072    0.02294 =
         0.03187   -0.00161   -0.00086   -0.00662
N4    4    0.381743   -0.046280    0.198572    11.00000    0.02092    0.02047 =
         0.03450    0.00014   -0.00164   -0.00733
N1    4    0.749024    0.750000    0.427831    10.50000    0.02373    0.02962 =
         0.02224    0.00000   -0.00173    0.00000
N2    4    0.800271    0.750000    0.570462    10.50000    0.03530    0.10266 =
         0.02656    0.00000   -0.00763    0.00000
C10   1    0.885279    0.750000    0.112090    10.50000    0.03361    0.04536 =
         0.02454    0.00000    0.00110    0.00000
AFIX  43
H10   2    0.935317    0.750000    0.148741    10.50000   -1.20000
AFIX   0
C9    1    0.830050    0.750000   -0.023381    10.50000    0.05867    0.06329 =
         0.02062    0.00000    0.00129    0.00000
AFIX  43
H9    2    0.839681    0.750000   -0.081945    10.50000   -1.20000
AFIX   0
C8    1    0.741666    0.750000    0.007590    10.50000    0.05053    0.06537 =
         0.02628    0.00000   -0.01370    0.00000
C7    1    0.730549    0.750000    0.094879    10.50000    0.03027    0.04546 =
         0.02834    0.00000   -0.00584    0.00000
AFIX  43
H7    2    0.671693    0.750000    0.117513    10.50000   -1.20000
AFIX   0
C5    1    0.623588    0.439099    0.255827    11.00000    0.01731    0.01425 =
         0.02378   -0.00083   -0.00043   -0.00037
C6    1    0.438015    0.060836    0.208201    11.00000    0.01624    0.01725 =
         0.02576    0.00107   -0.00144   -0.00069
C4    1    0.662761    0.750000    0.454723    10.50000    0.02572    0.04725 =
         0.01873    0.00000    0.00062    0.00000
AFIX  43
H4    2    0.615543    0.750000    0.414966    10.50000   -1.20000
AFIX   0
C3    1    0.641735    0.750000    0.540642    10.50000    0.03164    0.06459 =
         0.02233    0.00000    0.00226    0.00000
C2    1    0.713680    0.750000    0.596787    10.50000    0.04476    0.08745 =
         0.02294    0.00000   -0.00222    0.00000
AFIX  43
H2A   2    0.701585    0.750000    0.654954    10.50000   -1.20000
AFIX   0
C1    1    0.813819    0.750000    0.487190    10.50000    0.02720    0.06033 =
         0.02775    0.00000   -0.00321    0.00000
AFIX  43
H1A   2    0.874244    0.750000    0.468474    10.50000   -1.20000
AFIX   0
HKLF 4




REM  mo_rt340_ohpmdpt_260kdes_0ma_a.res in Pnma
REM wR2 = 0.0541, GooF = S = 1.175, Restrained GooF = 1.175 for all data
REM R1 = 0.0287 for 3715 Fo > 4sig(Fo) and 0.0383 for all 4316 data
REM 135 parameters refined using 0 restraints

END

WGHT      0.0000      5.7240

REM Highest difference peak  2.158,  deepest hole -3.493,  1-sigma level  0.184
Q1    1   0.5339  0.2500  0.3066  10.50000  0.05    2.16
Q2    1   0.6577  0.2500  0.2423  10.50000  0.05    1.59
Q3    1   0.6596  0.2500  0.3081  10.50000  0.05    1.58
Q4    1   0.4123  0.1914  0.2330  11.00000  0.05    1.36
Q5    1   0.5565  0.1812  0.2290  11.00000  0.05    1.32
;
_shelx_res_checksum              39450
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_rt366_feohpmdpd_260kd_0ma
_database_code_depnum_ccdc_archive 'CCDC 2209617'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_mo_rt366_feohpmdpd_260kd_0ma 
;
PROBLEM: D-H Bond Without Acceptor  O2       --H2       .     Please Check
RESPONSE: The O2 atom is not involved in a H-bond interaction in this structure
;
_vrf_PLAT430_mo_rt366_feohpmdpd_260kd_0ma 
;
PROBLEM: Short Inter D...A Contact  N4       ..N4       .       2.75 Ang.
RESPONSE: The N4 atom is not involved in a H-bond interaction in this structure
;
# Added during the CSD deposition process: Monday 26 September 2022 03:56 PM
# end Validation Reply Form

_audit_creation_date             2022-06-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H10 Fe N8 O2 Pd'
_chemical_formula_sum            'C12 H10 Fe N8 O2 Pd'
_chemical_formula_weight         460.53
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   13.9761(9)
_cell_length_b                   7.1852(5)
_cell_length_c                   15.2495(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1531.37(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    179.61
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.67
_shelx_estimated_absorpt_T_max   0.958
_shelx_estimated_absorpt_T_min   0.565
_exptl_absorpt_coefficient_mu    2.146
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1348 before and 0.0764 after correction.
The Ratio of minimum to maximum transmission is 0.7342.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.997
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37708
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.219
_diffrn_reflns_theta_min         1.977
_diffrn_ambient_temperature      179.61
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1648
_reflns_number_total             2044
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.696
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2044
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0335
_refine_ls_restrained_S_all      1.226
_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)+(0.0094P)²+8.5667P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0835
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1(0.5) H2(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N6(H6), N2(H2A), C10(H10), C4(H4), C7(H7), C1(H1A), C9(H9), C2(H2B)
3.b Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.52765(3) 0.250000 0.23213(3) 0.01423(11) Uani 1 2 d S T P . .
Fe1 Fe 0.77560(5) 0.750000 0.28703(5) 0.01296(17) Uani 1 2 d S T P . .
O1 O 0.5567(3) 0.750000 0.5721(3) 0.0391(13) Uani 1 2 d S T P . .
H1 H 0.518567 0.698835 0.537056 0.059 Uiso 0.5 1 calc R U P . .
N5 N 0.7916(3) 0.750000 0.1567(3) 0.0169(9) Uani 1 2 d S T P . .
N3 N 0.6793(2) 0.5581(4) 0.2729(2) 0.0153(6) Uani 1 1 d . . . . .
N1 N 0.7531(3) 0.750000 0.4163(3) 0.0180(10) Uani 1 2 d S T P . .
N6 N 0.8943(4) 0.750000 0.0322(3) 0.0286(12) Uani 1 2 d S T P . .
H6 H 0.952751 0.750000 0.010709 0.034 Uiso 1 2 calc R U P . .
O2 O 0.6448(4) 0.750000 -0.0350(3) 0.0475(15) Uani 1 2 d S T P . .
H2 H 0.655907 0.709756 -0.085697 0.071 Uiso 0.5 1 calc R U P . .
C6 C 0.4302(3) 0.0532(5) 0.2104(2) 0.0162(7) Uani 1 1 d . . . . .
C5 C 0.6237(3) 0.4462(5) 0.2591(2) 0.0155(7) Uani 1 1 d . . . . .
N2 N 0.8123(4) 0.750000 0.5609(3) 0.0313(13) Uani 1 2 d S T P . .
H2A H 0.861825 0.750000 0.596536 0.038 Uiso 1 2 calc R U P . .
C10 C 0.8797(4) 0.750000 0.1181(4) 0.0215(12) Uani 1 2 d S T P . .
H10 H 0.934278 0.750000 0.155262 0.026 Uiso 1 2 calc R U P . .
C4 C 0.6637(4) 0.750000 0.4485(4) 0.0207(12) Uani 1 2 d S T P . .
H4 H 0.611394 0.750000 0.408698 0.025 Uiso 1 2 calc R U P . .
C3 C 0.6451(4) 0.750000 0.5375(4) 0.0246(13) Uani 1 2 d S T P . .
C7 C 0.7165(4) 0.750000 0.1030(4) 0.0211(12) Uani 1 2 d S T P . .
H7 H 0.653927 0.750000 0.127230 0.025 Uiso 1 2 calc R U P . .
C1 C 0.8251(4) 0.750000 0.4753(4) 0.0224(12) Uani 1 2 d S T P . .
H1A H 0.888832 0.750000 0.453738 0.027 Uiso 1 2 calc R U P . .
C9 C 0.8178(5) 0.750000 -0.0212(4) 0.0284(14) Uani 1 2 d S T P . .
H9 H 0.826855 0.750000 -0.082950 0.034 Uiso 1 2 calc R U P . .
C2 C 0.7240(4) 0.750000 0.5928(4) 0.0284(14) Uani 1 2 d S T P . .
H2B H 0.714607 0.750000 0.654522 0.034 Uiso 1 2 calc R U P . .
C8 C 0.7272(5) 0.750000 0.0125(4) 0.0286(14) Uani 1 2 d S T P . .
N4 N 0.3728(2) -0.0587(4) 0.20428(19) 0.0152(6) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.01231(19) 0.01175(19) 0.0186(2) 0.000 -0.00143(16) 0.000
Fe1 0.0106(3) 0.0106(3) 0.0177(4) 0.000 0.0000(3) 0.000
O1 0.022(2) 0.075(4) 0.020(2) 0.000 0.0046(18) 0.000
N5 0.021(2) 0.007(2) 0.023(2) 0.000 -0.0081(19) 0.000
N3 0.0154(14) 0.0141(15) 0.0163(15) 0.0011(12) -0.0012(13) 0.0023(12)
N1 0.022(2) 0.015(2) 0.017(2) 0.000 -0.0012(19) 0.000
N6 0.026(3) 0.034(3) 0.026(3) 0.000 0.008(2) 0.000
O2 0.043(3) 0.075(4) 0.025(3) 0.000 -0.012(2) 0.000
C6 0.0134(16) 0.0147(18) 0.0205(19) 0.0024(14) -0.0020(14) 0.0023(15)
C5 0.0145(16) 0.0121(16) 0.0200(18) -0.0002(14) -0.0002(14) 0.0019(14)
N2 0.027(3) 0.045(3) 0.022(3) 0.000 -0.004(2) 0.000
C10 0.019(3) 0.026(3) 0.019(3) 0.000 0.006(2) 0.000
C4 0.017(3) 0.024(3) 0.021(3) 0.000 0.000(2) 0.000
C3 0.024(3) 0.032(3) 0.018(3) 0.000 0.001(2) 0.000
C7 0.026(3) 0.021(3) 0.016(3) 0.000 0.004(2) 0.000
C1 0.019(3) 0.029(3) 0.019(3) 0.000 -0.002(2) 0.000
C9 0.036(4) 0.033(4) 0.016(3) 0.000 0.004(3) 0.000
C2 0.023(3) 0.043(4) 0.019(3) 0.000 -0.001(2) 0.000
C8 0.036(4) 0.030(3) 0.019(3) 0.000 -0.009(3) 0.000
N4 0.0135(14) 0.0171(15) 0.0149(14) 0.0005(12) -0.0008(12) 0.0004(13)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C6 1.991(4) . ?
Pd1 C6 1.991(4) 7_565 ?
Pd1 C5 1.989(4) . ?
Pd1 C5 1.989(4) 7_565 ?
Fe1 N5 2.000(5) . ?
Fe1 N3 1.938(3) . ?
Fe1 N3 1.938(3) 7_575 ?
Fe1 N1 1.997(5) . ?
Fe1 N4 1.937(3) 6_666 ?
Fe1 N4 1.937(3) 4 ?
O1 H1 0.84(9) 7_575 ?
O1 H1 0.8400 . ?
O1 C3 1.344(7) . ?
N5 C10 1.366(7) . ?
N5 C7 1.331(7) . ?
N3 C5 1.139(5) . ?
N1 C4 1.342(7) . ?
N1 C1 1.349(7) . ?
N6 H6 0.8800 . ?
N6 C10 1.325(8) . ?
N6 C9 1.344(8) . ?
O2 H2 0.84(9) 7_575 ?
O2 H2 0.8400 . ?
O2 C8 1.360(8) . ?
C6 N4 1.139(5) . ?
N2 H2A 0.8800 . ?
N2 C1 1.318(8) . ?
N2 C2 1.326(8) . ?
C10 H10 0.9500 . ?
C4 H4 0.9500 . ?
C4 C3 1.382(8) . ?
C3 C2 1.389(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.388(8) . ?
C1 H1A 0.9500 . ?
C9 H9 0.9500 . ?
C9 C8 1.367(9) . ?
C2 H2B 0.9500 . ?

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
C6 Pd1 C6 90.5(2) . 7_565 ?
C5 Pd1 C6 177.63(15) . . ?
C5 Pd1 C6 89.60(14) . 7_565 ?
C5 Pd1 C6 177.63(15) 7_565 7_565 ?
C5 Pd1 C6 89.60(14) 7_565 . ?
C5 Pd1 C5 90.2(2) . 7_565 ?
N3 Fe1 N5 88.13(13) . . ?
N3 Fe1 N5 88.13(13) 7_575 . ?
N3 Fe1 N3 90.69(18) . 7_575 ?
N3 Fe1 N1 89.99(13) 7_575 . ?
N3 Fe1 N1 90.00(13) . . ?
N1 Fe1 N5 177.3(2) . . ?
N4 Fe1 N5 89.41(13) 6_666 . ?
N4 Fe1 N5 89.41(13) 4 . ?
N4 Fe1 N3 177.53(13) 6_666 . ?
N4 Fe1 N3 177.53(13) 4 7_575 ?
N4 Fe1 N3 89.40(13) 6_666 7_575 ?
N4 Fe1 N3 89.40(13) 4 . ?
N4 Fe1 N1 92.47(13) 4 . ?
N4 Fe1 N1 92.47(13) 6_666 . ?
N4 Fe1 N4 90.40(19) 6_666 4 ?
H1 O1 H1 51.9 . 7_575 ?
C3 O1 H1 109(2) . 7_575 ?
C3 O1 H1 109.5 . . ?
C10 N5 Fe1 122.0(4) . . ?
C7 N5 Fe1 121.6(4) . . ?
C7 N5 C10 116.4(5) . . ?
C5 N3 Fe1 175.7(3) . . ?
C4 N1 Fe1 120.5(4) . . ?
C4 N1 C1 116.8(5) . . ?
C1 N1 Fe1 122.7(4) . . ?
C10 N6 H6 120.8 . . ?
C10 N6 C9 118.5(5) . . ?
C9 N6 H6 120.8 . . ?
H2 O2 H2 40.3 . 7_575 ?
C8 O2 H2 109(2) . 7_575 ?
C8 O2 H2 109.5 . . ?
N4 C6 Pd1 175.0(3) . . ?
N3 C5 Pd1 178.6(3) . . ?
C1 N2 H2A 120.3 . . ?
C1 N2 C2 119.3(6) . . ?
C2 N2 H2A 120.3 . . ?
N5 C10 H10 117.8 . . ?
N6 C10 N5 124.4(6) . . ?
N6 C10 H10 117.8 . . ?
N1 C4 H4 118.9 . . ?
N1 C4 C3 122.3(5) . . ?
C3 C4 H4 118.9 . . ?
O1 C3 C4 124.0(6) . . ?
O1 C3 C2 119.4(5) . . ?
C4 C3 C2 116.6(6) . . ?
N5 C7 H7 119.1 . . ?
N5 C7 C8 121.8(6) . . ?
C8 C7 H7 119.1 . . ?
N1 C1 H1A 118.0 . . ?
N2 C1 N1 124.0(6) . . ?
N2 C1 H1A 118.0 . . ?
N6 C9 H9 119.7 . . ?
N6 C9 C8 120.6(6) . . ?
C8 C9 H9 119.7 . . ?
N2 C2 C3 121.0(6) . . ?
N2 C2 H2B 119.5 . . ?
C3 C2 H2B 119.5 . . ?
O2 C8 C7 116.0(6) . . ?
O2 C8 C9 125.8(6) . . ?
C9 C8 C7 118.2(6) . . ?
C6 N4 Fe1 171.4(3) . 6_546 ?

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 N5 C10 N6 180.000(0) . . . . ?
Fe1 N5 C7 C8 180.000(0) . . . . ?
Fe1 N1 C4 C3 180.000(1) . . . . ?
Fe1 N1 C1 N2 180.000(1) . . . . ?
O1 C3 C2 N2 180.000(1) . . . . ?
N5 C7 C8 O2 180.000(0) . . . . ?
N5 C7 C8 C9 0.000(0) . . . . ?
N1 C4 C3 O1 180.000(1) . . . . ?
N1 C4 C3 C2 0.000(1) . . . . ?
N6 C9 C8 O2 180.0 . . . . ?
N6 C9 C8 C7 0.000(0) . . . . ?
C10 N5 C7 C8 0.000(0) . . . . ?
C10 N6 C9 C8 0.000(0) . . . . ?
C4 N1 C1 N2 0.000(1) . . . . ?
C4 C3 C2 N2 0.000(1) . . . . ?
C7 N5 C10 N6 0.000(0) . . . . ?
C1 N1 C4 C3 0.000(1) . . . . ?
C1 N2 C2 C3 0.000(1) . . . . ?
C9 N6 C10 N5 0.000(0) . . . . ?
C2 N2 C1 N1 0.000(1) . . . . ?

_shelx_res_file                  
;
TITL mo_rt366_feohpmdpd_260kd_0ma_a.res in Pnma
    mo_rt366_feohpmdpd_260kd_0ma.res
    created by SHELXL-2018/3 at 11:42:43 on 14-Jun-2022
REM Old TITL mo_RT366_FeOHPmdPd_260Kd_0ma in Pnma
REM SHELXT solution in Pnma: R1 0.076, Rweak 0.001, Alpha 0.030
REM <I/s> 0.263 for 137 systematic absences, Orientation as input
REM Formula found by SHELXT: C15 N6 O Fe Pd
CELL 0.71073 13.9761 7.1852 15.2495 90 90 90
ZERR 4 0.0009 0.0005 0.001 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Fe N O Pd
UNIT 48 40 4 32 8 4

L.S. 20
PLAN  5
SIZE 0.3 0.2 0.02
TEMP -93.54
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\mo_RT366_FeOHPmdPd_260Kd_0ma.hkl">
REM </olex2.extras>

WGHT    0.009400    8.566700
FVAR       0.23343
PD1   6    0.527654    0.250000    0.232125    10.50000    0.01231    0.01175 =
         0.01862    0.00000   -0.00143    0.00000
FE1   3    0.775602    0.750000    0.287033    10.50000    0.01058    0.01062 =
         0.01768    0.00000    0.00004    0.00000
O1    5    0.556725    0.750000    0.572128    10.50000    0.02155    0.07546 =
         0.02030    0.00000    0.00456    0.00000
AFIX 147
H1    2    0.518567    0.698835    0.537056    10.50000   -1.50000
AFIX   0
N5    4    0.791579    0.750000    0.156713    10.50000    0.02126    0.00675 =
         0.02262    0.00000   -0.00809    0.00000
N3    4    0.679344    0.558096    0.272945    11.00000    0.01539    0.01407 =
         0.01632    0.00111   -0.00123    0.00231
N1    4    0.753055    0.750000    0.416343    10.50000    0.02188    0.01492 =
         0.01732    0.00000   -0.00125    0.00000
N6    4    0.894335    0.750000    0.032245    10.50000    0.02621    0.03383 =
         0.02562    0.00000    0.00792    0.00000
AFIX  43
H6    2    0.952751    0.750000    0.010709    10.50000   -1.20000
AFIX   0
O2    5    0.644794    0.750000   -0.034993    10.50000    0.04253    0.07479 =
         0.02506    0.00000   -0.01228    0.00000
AFIX 147
H2    2    0.655907    0.709756   -0.085697    10.50000   -1.50000
AFIX   0
C6    1    0.430166    0.053211    0.210357    11.00000    0.01341    0.01470 =
         0.02051    0.00241   -0.00195    0.00229
C5    1    0.623680    0.446178    0.259126    11.00000    0.01454    0.01212 =
         0.01997   -0.00018   -0.00024    0.00195
N2    4    0.812292    0.750000    0.560910    10.50000    0.02729    0.04482 =
         0.02165    0.00000   -0.00426    0.00000
AFIX  43
H2A   2    0.861825    0.750000    0.596536    10.50000   -1.20000
AFIX   0
C10   1    0.879744    0.750000    0.118076    10.50000    0.01949    0.02607 =
         0.01903    0.00000    0.00554    0.00000
AFIX  43
H10   2    0.934278    0.750000    0.155262    10.50000   -1.20000
AFIX   0
C4    1    0.663694    0.750000    0.448490    10.50000    0.01726    0.02371 =
         0.02119    0.00000    0.00047    0.00000
AFIX  43
H4    2    0.611394    0.750000    0.408698    10.50000   -1.20000
AFIX   0
C3    1    0.645127    0.750000    0.537475    10.50000    0.02442    0.03151 =
         0.01799    0.00000    0.00125    0.00000
C7    1    0.716535    0.750000    0.102970    10.50000    0.02617    0.02083 =
         0.01623    0.00000    0.00359    0.00000
AFIX  43
H7    2    0.653927    0.750000    0.127230    10.50000   -1.20000
AFIX   0
C1    1    0.825051    0.750000    0.475277    10.50000    0.01943    0.02877 =
         0.01905    0.00000   -0.00159    0.00000
AFIX  43
H1A   2    0.888832    0.750000    0.453738    10.50000   -1.20000
AFIX   0
C9    1    0.817834    0.750000   -0.021204    10.50000    0.03623    0.03333 =
         0.01554    0.00000    0.00377    0.00000
AFIX  43
H9    2    0.826855    0.750000   -0.082950    10.50000   -1.20000
AFIX   0
C2    1    0.724014    0.750000    0.592824    10.50000    0.02277    0.04301 =
         0.01939    0.00000   -0.00108    0.00000
AFIX  43
H2B   2    0.714607    0.750000    0.654522    10.50000   -1.20000
AFIX   0
C8    1    0.727187    0.750000    0.012474    10.50000    0.03648    0.03002 =
         0.01931    0.00000   -0.00945    0.00000
N4    4    0.372821   -0.058685    0.204283    11.00000    0.01347    0.01706 =
         0.01493    0.00049   -0.00080    0.00043
HKLF 4




REM  mo_rt366_feohpmdpd_260kd_0ma_a.res in Pnma
REM wR2 = 0.0835, GooF = S = 1.226, Restrained GooF = 1.226 for all data
REM R1 = 0.0335 for 1648 Fo > 4sig(Fo) and 0.0566 for all 2044 data
REM 135 parameters refined using 0 restraints

END

WGHT      0.0094      8.5666

REM Highest difference peak  1.696,  deepest hole -1.029,  1-sigma level  0.166
Q1    1   0.5264  0.2500  0.3062  10.50000  0.05    1.70
Q2    1   0.4179  0.2500  0.2385  10.50000  0.05    1.32
Q3    1   0.6673  0.7500  0.2119  10.50000  0.05    1.27
Q4    1   0.7782  0.7500  0.2039  10.50000  0.05    1.13
Q5    1   0.7134  0.7500  0.2774  10.50000  0.05    1.01
;
_shelx_res_checksum              7208
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rt366_feohpmdpd_260kdt_0ma_a
_database_code_depnum_ccdc_archive 'CCDC 2209618'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_rt366_feohpmdpd_260kdt_0ma_a 
;
PROBLEM: D-H Bond Without Acceptor  O2       --H2       .     Please Check
RESPONSE: The O2 atom is not involved in a H-bond interaction in this structure
;
# Added during the CSD deposition process: Monday 26 September 2022 03:56 PM
# end Validation Reply Form

_audit_creation_date             2022-06-14
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H8 Fe N8 O2 Pd'
_chemical_formula_sum            'C12 H8 Fe N8 O2 Pd'
_chemical_formula_weight         458.51
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
'x-1/2, y, -z-1/2'

_cell_length_a                   14.2973(5)
_cell_length_b                   7.4281(3)
_cell_length_c                   15.6554(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1662.63(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    260.0
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.60
_shelx_estimated_absorpt_T_max   0.962
_shelx_estimated_absorpt_T_min   0.589
_exptl_absorpt_coefficient_mu    1.976
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0968 before and 0.0686 after correction.
The Ratio of minimum to maximum transmission is 0.8677.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51405
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.233
_diffrn_reflns_theta_min         2.602
_diffrn_ambient_temperature      260.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1670
_reflns_number_total             2012
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2012
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0268
_refine_ls_restrained_S_all      1.235
_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)+5.5403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0651
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1(0.5) H2(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1A), C10(H10), C9(H9), C2(H2A), C7(H7)
3.b Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.03557(2) -0.250000 0.23125(2) 0.01902(10) Uani 1 2 d S T P . .
Fe1 Fe 0.28370(4) 0.250000 0.29966(4) 0.01783(14) Uani 1 2 d S T P . .
N4 N -0.11239(19) -0.5470(4) 0.19018(19) 0.0294(6) Uani 1 1 d . . . . .
N3 N 0.17983(19) 0.0473(4) 0.28199(18) 0.0283(6) Uani 1 1 d . . . . .
N5 N 0.3010(3) 0.250000 0.1562(3) 0.0263(9) Uani 1 2 d S T P . .
N1 N 0.2518(3) 0.250000 0.4373(3) 0.0281(9) Uani 1 2 d S T P . .
O1 O 0.0510(3) 0.250000 0.5775(3) 0.0713(17) Uani 1 2 d S T P . .
H1 H 0.015264 0.230701 0.537548 0.107 Uiso 0.5 1 calc R U P . .
C5 C 0.1268(2) -0.0608(4) 0.2645(2) 0.0213(6) Uani 1 1 d . . . . .
C6 C -0.0572(2) -0.4397(4) 0.2021(2) 0.0244(7) Uani 1 1 d . . . . .
C8 C 0.2344(5) 0.250000 0.0177(4) 0.0519(17) Uani 1 2 d S T P . .
N6 N 0.3992(4) 0.250000 0.0329(3) 0.0472(13) Uani 1 2 d S T P . .
O2 O 0.1541(4) 0.250000 -0.0275(3) 0.095(2) Uani 1 2 d S T P . .
H2 H 0.164436 0.214103 -0.076138 0.143 Uiso 0.5 1 calc R U P . .
C3 C 0.1403(4) 0.250000 0.5486(3) 0.0415(14) Uani 1 2 d S T P . .
C4 C 0.1634(3) 0.250000 0.4631(3) 0.0324(12) Uani 1 2 d S T P . .
H4 H 0.115926 0.250000 0.422536 0.039 Uiso 1 2 calc R U P . .
N2 N 0.3014(3) 0.250000 0.5812(3) 0.0537(15) Uani 1 2 d S T P . .
C1 C 0.3173(4) 0.250000 0.4975(3) 0.0383(13) Uani 1 2 d S T P . .
H1A H 0.379307 0.250000 0.479606 0.046 Uiso 1 2 calc R U P . .
C10 C 0.3850(4) 0.250000 0.1165(3) 0.0392(13) Uani 1 2 d S T P . .
H10 H 0.437779 0.250000 0.151208 0.047 Uiso 1 2 calc R U P . .
C9 C 0.3234(5) 0.250000 -0.0166(4) 0.0526(17) Uani 1 2 d S T P . .
H9 H 0.330552 0.250000 -0.075666 0.063 Uiso 1 2 calc R U P . .
C2 C 0.2131(4) 0.250000 0.6061(4) 0.0520(17) Uani 1 2 d S T P . .
H2A H 0.199818 0.250000 0.664259 0.062 Uiso 1 2 calc R U P . .
C7 C 0.2273(4) 0.250000 0.1054(3) 0.0370(13) Uani 1 2 d S T P . .
H7 H 0.168014 0.250000 0.129883 0.044 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.01569(16) 0.01396(16) 0.02741(18) 0.000 -0.00260(14) 0.000
Fe1 0.0160(3) 0.0140(3) 0.0235(3) 0.000 0.0003(2) 0.000
N4 0.0241(14) 0.0250(15) 0.0392(17) -0.0004(13) -0.0009(12) -0.0089(12)
N3 0.0256(13) 0.0232(14) 0.0361(16) -0.0046(12) -0.0032(12) -0.0045(12)
N5 0.032(2) 0.0211(19) 0.026(2) 0.000 -0.0083(17) 0.000
N1 0.027(2) 0.030(2) 0.027(2) 0.000 -0.0003(17) 0.000
O1 0.038(2) 0.149(6) 0.027(2) 0.000 0.0078(19) 0.000
C5 0.0205(14) 0.0182(14) 0.0253(15) 0.0000(12) -0.0010(12) 0.0013(12)
C6 0.0220(15) 0.0210(15) 0.0302(17) 0.0031(13) -0.0023(13) 0.0015(13)
C8 0.060(4) 0.064(4) 0.032(3) 0.000 -0.013(3) 0.000
N6 0.052(3) 0.063(3) 0.026(2) 0.000 0.007(2) 0.000
O2 0.067(4) 0.181(7) 0.039(3) 0.000 -0.028(3) 0.000
C3 0.032(3) 0.068(4) 0.024(3) 0.000 0.003(2) 0.000
C4 0.024(2) 0.048(3) 0.026(3) 0.000 0.001(2) 0.000
N2 0.035(3) 0.093(5) 0.033(3) 0.000 -0.006(2) 0.000
C1 0.027(3) 0.056(4) 0.032(3) 0.000 -0.001(2) 0.000
C10 0.038(3) 0.052(4) 0.027(3) 0.000 0.001(2) 0.000
C9 0.066(4) 0.068(5) 0.024(3) 0.000 0.007(3) 0.000
C2 0.047(4) 0.086(5) 0.023(3) 0.000 -0.002(3) 0.000
C7 0.037(3) 0.048(3) 0.026(3) 0.000 -0.004(2) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C5 1.987(3) . ?
Pd1 C5 1.987(3) 7 ?
Pd1 C6 1.988(3) . ?
Pd1 C6 1.988(3) 7 ?
Fe1 N4 2.123(3) 2_545 ?
Fe1 N4 2.123(3) 8_666 ?
Fe1 N3 2.133(3) 7_565 ?
Fe1 N3 2.133(3) . ?
Fe1 N5 2.259(4) . ?
Fe1 N1 2.202(4) . ?
N4 C6 1.137(4) . ?
N3 C5 1.138(4) . ?
N5 C10 1.352(7) . ?
N5 C7 1.320(6) . ?
N1 C4 1.326(6) . ?
N1 C1 1.329(6) . ?
O1 H1 0.82(8) 7_565 ?
O1 H1 0.8200 . ?
O1 C3 1.354(7) . ?
C8 O2 1.350(8) . ?
C8 C9 1.381(9) . ?
C8 C7 1.376(8) . ?
N6 C10 1.324(7) . ?
N6 C9 1.333(8) . ?
O2 H2 0.82(11) 7_565 ?
O2 H2 0.8200 . ?
C3 C4 1.378(7) . ?
C3 C2 1.377(8) . ?
C4 H4 0.9300 . ?
N2 C1 1.330(7) . ?
N2 C2 1.320(8) . ?
C1 H1A 0.9300 . ?
C10 H10 0.9300 . ?
C9 H9 0.9300 . ?
C2 H2A 0.9300 . ?
C7 H7 0.9300 . ?

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
C5 Pd1 C5 90.04(17) . 7 ?
C5 Pd1 C6 178.07(13) . . ?
C5 Pd1 C6 89.82(12) . 7 ?
C5 Pd1 C6 178.07(13) 7 7 ?
C5 Pd1 C6 89.82(12) 7 . ?
C6 Pd1 C6 90.26(18) 7 . ?
N4 Fe1 N4 90.54(16) 8_666 2_545 ?
N4 Fe1 N3 176.84(12) 8_666 . ?
N4 Fe1 N3 89.74(11) 8_666 7_565 ?
N4 Fe1 N3 176.84(12) 2_545 7_565 ?
N4 Fe1 N3 89.74(11) 2_545 . ?
N4 Fe1 N5 89.88(11) 2_545 . ?
N4 Fe1 N5 89.88(11) 8_666 . ?
N4 Fe1 N1 94.12(11) 2_545 . ?
N4 Fe1 N1 94.12(11) 8_666 . ?
N3 Fe1 N3 89.81(15) 7_565 . ?
N3 Fe1 N5 86.98(11) . . ?
N3 Fe1 N5 86.98(11) 7_565 . ?
N3 Fe1 N1 89.00(11) . . ?
N3 Fe1 N1 89.00(11) 7_565 . ?
N1 Fe1 N5 174.31(15) . . ?
C6 N4 Fe1 166.3(3) . 2_445 ?
C5 N3 Fe1 173.4(3) . . ?
C10 N5 Fe1 123.6(3) . . ?
C7 N5 Fe1 120.8(4) . . ?
C7 N5 C10 115.6(4) . . ?
C4 N1 Fe1 119.7(3) . . ?
C4 N1 C1 117.1(4) . . ?
C1 N1 Fe1 123.2(3) . . ?
H1 O1 H1 20.1 . 7_565 ?
C3 O1 H1 109(2) . 7_565 ?
C3 O1 H1 109.5 . . ?
N3 C5 Pd1 178.7(3) . . ?
N4 C6 Pd1 175.9(3) . . ?
O2 C8 C9 125.4(6) . . ?
O2 C8 C7 117.4(6) . . ?
C7 C8 C9 117.2(6) . . ?
C10 N6 C9 116.8(5) . . ?
C8 O2 H2 109(3) . 7_565 ?
C8 O2 H2 109.5 . . ?
H2 O2 H2 38.0 . 7_565 ?
O1 C3 C4 123.4(5) . . ?
O1 C3 C2 119.6(5) . . ?
C2 C3 C4 117.0(5) . . ?
N1 C4 C3 121.7(5) . . ?
N1 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C2 N2 C1 117.0(5) . . ?
N1 C1 N2 125.3(5) . . ?
N1 C1 H1A 117.3 . . ?
N2 C1 H1A 117.3 . . ?
N5 C10 H10 116.9 . . ?
N6 C10 N5 126.2(5) . . ?
N6 C10 H10 116.9 . . ?
C8 C9 H9 119.3 . . ?
N6 C9 C8 121.5(5) . . ?
N6 C9 H9 119.3 . . ?
C3 C2 H2A 119.0 . . ?
N2 C2 C3 121.9(5) . . ?
N2 C2 H2A 119.0 . . ?
N5 C7 C8 122.8(6) . . ?
N5 C7 H7 118.6 . . ?
C8 C7 H7 118.6 . . ?

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 N5 C10 N6 180.000(0) . . . . ?
Fe1 N5 C7 C8 180.000(0) . . . . ?
Fe1 N1 C4 C3 180.000(1) . . . . ?
Fe1 N1 C1 N2 180.000(1) . . . . ?
O1 C3 C4 N1 180.000(1) . . . . ?
O1 C3 C2 N2 180.000(1) . . . . ?
O2 C8 C9 N6 180.0 . . . . ?
O2 C8 C7 N5 180.000(0) . . . . ?
C4 N1 C1 N2 0.000(1) . . . . ?
C4 C3 C2 N2 0.000(1) . . . . ?
C1 N1 C4 C3 0.000(1) . . . . ?
C1 N2 C2 C3 0.000(1) . . . . ?
C10 N5 C7 C8 0.000(0) . . . . ?
C10 N6 C9 C8 0.000(0) . . . . ?
C9 C8 C7 N5 0.000(0) . . . . ?
C9 N6 C10 N5 0.000(0) . . . . ?
C2 C3 C4 N1 0.000(1) . . . . ?
C2 N2 C1 N1 0.000(1) . . . . ?
C7 N5 C10 N6 0.000(0) . . . . ?
C7 C8 C9 N6 0.000(0) . . . . ?

_shelx_res_file                  
;
TITL RT366_FeOHPmdPd_260Kdt_0ma_a.res in Pnma
    rt366_feohpmdpd_260kdt_0ma_a.res
    created by SHELXL-2018/3 at 11:39:58 on 14-Jun-2022
CELL 0.71073 14.2973 7.4281 15.6554 90 90 90
ZERR 4 0.0005 0.0003 0.0005 0 0 0
LATT 1
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM -X,0.5+Y,-Z
SYMM 0.5-X,-Y,0.5+Z
SFAC C H Fe N O Pd
UNIT 48 32 4 32 8 4

L.S. 15
PLAN  5 0 0
SIZE 0.3 0.2 0.02
TEMP -13.15
CONF
BOND $H
MORE -1
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\RT366_FeOHPmdPd_260Kdt_0ma_a.hkl">
REM </olex2.extras>

WGHT    0.000000    5.540300
FVAR       0.29199
PD1   6    0.035573   -0.250000    0.231245    10.50000    0.01569    0.01396 =
         0.02741    0.00000   -0.00260    0.00000
FE1   3    0.283701    0.250000    0.299660    10.50000    0.01600    0.01404 =
         0.02346    0.00000    0.00032    0.00000
N4    4   -0.112390   -0.546961    0.190184    11.00000    0.02410    0.02498 =
         0.03923   -0.00037   -0.00086   -0.00885
N3    4    0.179829    0.047298    0.281991    11.00000    0.02556    0.02317 =
         0.03605   -0.00464   -0.00324   -0.00450
N5    4    0.300997    0.250000    0.156200    10.50000    0.03181    0.02115 =
         0.02605    0.00000   -0.00833    0.00000
N1    4    0.251756    0.250000    0.437272    10.50000    0.02697    0.02994 =
         0.02743    0.00000   -0.00034    0.00000
O1    5    0.051031    0.250000    0.577457    10.50000    0.03760    0.14930 =
         0.02702    0.00000    0.00776    0.00000
AFIX 147
H1    2    0.015264    0.230701    0.537548    10.50000   -1.50000
AFIX   0
C5    1    0.126811   -0.060804    0.264471    11.00000    0.02054    0.01821 =
         0.02527    0.00001   -0.00105    0.00134
C6    1   -0.057168   -0.439670    0.202057    11.00000    0.02204    0.02096 =
         0.03022    0.00309   -0.00230    0.00152
C8    1    0.234438    0.250000    0.017723    10.50000    0.06025    0.06384 =
         0.03152    0.00000   -0.01325    0.00000
N6    4    0.399180    0.250000    0.032925    10.50000    0.05241    0.06325 =
         0.02581    0.00000    0.00737    0.00000
O2    5    0.154076    0.250000   -0.027518    10.50000    0.06671    0.18056 =
         0.03863    0.00000   -0.02768    0.00000
AFIX 147
H2    2    0.164436    0.214103   -0.076138    10.50000   -1.50000
AFIX   0
C3    1    0.140296    0.250000    0.548572    10.50000    0.03199    0.06831 =
         0.02428    0.00000    0.00302    0.00000
C4    1    0.163446    0.250000    0.463101    10.50000    0.02372    0.04784 =
         0.02554    0.00000    0.00113    0.00000
AFIX  43
H4    2    0.115926    0.250000    0.422536    10.50000   -1.20000
AFIX   0
N2    4    0.301361    0.250000    0.581174    10.50000    0.03465    0.09332 =
         0.03304    0.00000   -0.00631    0.00000
C1    1    0.317267    0.250000    0.497461    10.50000    0.02678    0.05643 =
         0.03162    0.00000   -0.00135    0.00000
AFIX  43
H1A   2    0.379307    0.250000    0.479606    10.50000   -1.20000
AFIX   0
C10   1    0.384976    0.250000    0.116517    10.50000    0.03832    0.05221 =
         0.02706    0.00000    0.00122    0.00000
AFIX  43
H10   2    0.437779    0.250000    0.151208    10.50000   -1.20000
AFIX   0
C9    1    0.323375    0.250000   -0.016624    10.50000    0.06600    0.06793 =
         0.02389    0.00000    0.00708    0.00000
AFIX  43
H9    2    0.330552    0.250000   -0.075666    10.50000   -1.20000
AFIX   0
C2    1    0.213149    0.250000    0.606115    10.50000    0.04685    0.08617 =
         0.02295    0.00000   -0.00165    0.00000
AFIX  43
H2A   2    0.199818    0.250000    0.664259    10.50000   -1.20000
AFIX   0
C7    1    0.227276    0.250000    0.105393    10.50000    0.03740    0.04812 =
         0.02557    0.00000   -0.00357    0.00000
AFIX  43
H7    2    0.168014    0.250000    0.129883    10.50000   -1.20000
AFIX   0
HKLF 4




REM  RT366_FeOHPmdPd_260Kdt_0ma_a.res in Pnma
REM wR2 = 0.0651, GooF = S = 1.235, Restrained GooF = 1.235 for all data
REM R1 = 0.0268 for 1670 Fo > 4sig(Fo) and 0.0435 for all 2012 data
REM 135 parameters refined using 0 restraints

END

WGHT      0.0000      5.5404

REM Highest difference peak  1.318,  deepest hole -0.937,  1-sigma level  0.120
Q1    1   0.0340 -0.2500  0.3122  10.50000  0.05    1.32
Q2    1   0.2855  0.2500  0.2486  10.50000  0.05    0.90
Q3    1   0.1532  0.2500  0.2001  10.50000  0.05    0.79
Q4    1  -0.0273  0.2500  0.6306  10.50000  0.05    0.59
Q5    1   0.3368  0.2500  0.3704  10.50000  0.05    0.55
;
_shelx_res_checksum              20814
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rt590_ohpymptetoh_120k
_database_code_depnum_ccdc_archive 'CCDC 2209622'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_rt590_ohpymptetoh_120k 
;
PROBLEM: Check Calcd Resid. Dens.  1.14Ang From N6              3.73 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT342_rt590_ohpymptetoh_120k 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0425 Ang.
RESPONSE: This alerts arises from the strong disorder of the guest in the structural pores and from a deterioration of the crystal during the desorption readsorption processes
;
_vrf_PLAT430_rt590_ohpymptetoh_120k 
;
PROBLEM: Short Inter D...A Contact  O3       ..N2       .       2.60 Ang.
RESPONSE: There is a certain number of H-bonds which are properly discussed in the paper. This alert arises from the absence of H atoms which are not present due to the strong agitation of the molecular moieties involved in the H-bond interactions
;
_vrf_PLAT971_rt590_ohpymptetoh_120k_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.95Ang From Pt1             3.19 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt590_ohpymptetoh_120k_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.10Ang From O1              3.07 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt590_ohpymptetoh_120k_4 
;
PROBLEM: Check Calcd Resid. Dens.  0.94Ang From Pt1             3.04 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt590_ohpymptetoh_120k_5 
;
PROBLEM: Check Calcd Resid. Dens.  0.04Ang From N5              2.99 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt590_ohpymptetoh_120k_6 
;
PROBLEM: Check Calcd Resid. Dens.  0.85Ang From Pt1             2.93 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt590_ohpymptetoh_120k_7 
;
PROBLEM: Check Calcd Resid. Dens.  1.09Ang From C2              2.61 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt590_ohpymptetoh_120k_8 
;
PROBLEM: Check Calcd Resid. Dens.  1.06Ang From C8              2.61 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt590_ohpymptetoh_120k 
;
PROBLEM: Check Calcd Resid. Dens.  0.18Ang From O2             -2.72 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt590_ohpymptetoh_120k_2 
;
PROBLEM: Check Calcd Resid. Dens.  1.00Ang From Pt1            -2.65 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Monday 26 September 2022 03:56 PM
# end Validation Reply Form

_audit_creation_date             2022-09-26
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 Fe N8 O2 Pt, C O0.5'
_chemical_formula_sum            'C13 H6 Fe N8 O2.50 Pt'
_chemical_formula_weight         565.20
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'colourlesstablet 0.32 0.12 0.06'
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'
Pt Pt -1.7033 8.3905 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.123(4)
_cell_length_b                   7.1448(3)
_cell_length_c                   14.419(3)
_cell_angle_alpha                90
_cell_angle_beta                 132.39(3)
_cell_angle_gamma                90
_cell_volume                     1607.2(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3270
_cell_measurement_temperature    120.05(10)
_cell_measurement_theta_max      25.5890
_cell_measurement_theta_min      3.1290
_shelx_estimated_absorpt_T_max   0.645
_shelx_estimated_absorpt_T_min   0.249
_exptl_absorpt_coefficient_mu    9.627
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.336
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10085
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.820
_diffrn_reflns_theta_min         3.136
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  42.00   1.00    5.00    --   17.31  77.00 -60.00   56
  2  ω     -4.00  86.00   1.00    5.00    --   17.31  57.00 120.00   90
  3  ω    -32.00  92.00   1.00    5.00    --   17.31  19.00  90.00  124
  4  ω    -95.00 -37.00   1.00    5.00    --  -16.37 178.00 120.00   58
  5  ω    -15.00  59.00   1.00    5.00    --   17.31 -99.00 -90.00   74
  6  ω    -14.00  42.00   1.00    5.00    --   17.31  77.00-120.00   56
  7  ω    -14.00  42.00   1.00    5.00    --   17.31  77.00   0.00   56
  8  ω    -42.00  49.00   1.00    5.00    --   17.31 -77.00  90.00   91
  9  ω    -52.00  39.00   1.00    5.00    --   17.31 -57.00 -30.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0126955000
_diffrn_orient_matrix_UB_12      -0.0285080000
_diffrn_orient_matrix_UB_13      0.0324488000
_diffrn_orient_matrix_UB_21      -0.0434045000
_diffrn_orient_matrix_UB_22      0.0191947000
_diffrn_orient_matrix_UB_23      -0.0542095000
_diffrn_orient_matrix_UB_31      -0.0050484000
_diffrn_orient_matrix_UB_32      -0.0932054000
_diffrn_orient_matrix_UB_33      -0.0211149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1708
_reflns_number_total             1890
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.209
_refine_diff_density_min         -2.972
_refine_diff_density_rms         0.335
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1890
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0614
_refine_ls_restrained_S_all      1.151
_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)+(0.0492P)²+114.2136P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1515
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C11-O3
 1.2 with sigma of 0.02
 C3-C4
 1.4 with sigma of 0.001
 C2-N2
 1.33 with sigma of 0.001
 C8-C7
 1.33 with sigma of 0.001
 C9-N6
 1.33 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(N2) = Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(N1) =
Uanis(O1)
Uanis(C7) = Uanis(N5) = Uanis(C10) = Uanis(N6) = Uanis(C9) = Uanis(C8) =
Uanis(O2)
4. Others
 Fixed Sof: O3(0.25) C11(0.5)
 Fixed X: N6(0.26387) N2(0.230949)
 Fixed Y: N6(1) N2(0)
 Fixed Z: N6(0.916589) N2(0.30171)
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C2(H2), C10(H10), C1(H1), C4(H4), C7(H7)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.48338(4) 0.500000 0.73464(6) 0.0200(2) Uani 1 2 d S T P . .
Fe1 Fe 0.500000 0.000000 0.500000 0.0183(7) Uani 1 4 d S T P . .
Fe2 Fe 0.500000 1.000000 1.000000 0.0175(7) Uani 1 4 d S T P . .
N4 N 0.4846(6) 0.8068(14) 0.8906(9) 0.023(2) Uani 1 1 d . . . . .
N3 N 0.4901(7) 0.1943(14) 0.5861(10) 0.025(2) Uani 1 1 d . . . . .
C6 C 0.4822(7) 0.6949(16) 0.8321(11) 0.021(2) Uani 1 1 d . . . . .
C5 C 0.4872(8) 0.3038(16) 0.6408(11) 0.022(2) Uani 1 1 d . . . . .
N1 N 0.3691(16) 0.000000 0.350(2) 0.061(2) Uani 1 2 d S T P . .
N5 N 0.3725(15) 1.000000 0.903(3) 0.065(3) Uani 1 2 d S T P . .
O2 O 0.1673(12) 1.000000 0.610(2) 0.065(3) Uani 1 2 d S T P . .
C3 C 0.2371(11) 0.000000 0.142(2) 0.061(2) Uani 1 2 d DS T P . .
C9 C 0.2059(14) 1.000000 0.79172(10) 0.065(3) Uani 1 2 d DS T P . .
H9 H 0.146610 1.000000 0.748045 0.078 Uiso 1 2 calc R U P . .
O1 O 0.1975(13) 0.000000 0.0256(18) 0.061(2) Uani 1 2 d S T P . .
C2 C 0.1929(16) 0.000000 0.1816(7) 0.061(2) Uani 1 2 d DS T P . .
H2 H 0.132014 0.000000 0.119523 0.073 Uiso 1 2 calc R U P . .
N6 N 0.263870 1.000000 0.916589 0.065(3) Uani 1 2 d DS T P . .
O3 O 0.231(3) 0.000000 0.482(4) 0.078(12) Uiso 0.5 2 d DS . P . .
N2 N 0.230949 0.000000 0.301710 0.061(2) Uani 1 2 d DS T P . .
C10 C 0.3462(18) 1.000000 0.967(3) 0.065(3) Uani 1 2 d S T P . .
H10 H 0.389958 1.000000 1.055637 0.078 Uiso 1 2 calc R U P . .
C1 C 0.3191(19) 0.000000 0.385(3) 0.061(2) Uani 1 2 d S T P . .
H1 H 0.349367 0.000000 0.472372 0.073 Uiso 1 2 calc R U P . .
C4 C 0.3268(11) 0.000000 0.230(2) 0.061(2) Uani 1 2 d DS T P . .
H4 H 0.356982 0.000000 0.203010 0.073 Uiso 1 2 calc R U P . .
C7 C 0.3132(10) 1.000000 0.777(3) 0.065(3) Uani 1 2 d DS T P . .
H7 H 0.328444 1.000000 0.728735 0.078 Uiso 1 2 calc R U P . .
C8 C 0.2317(11) 1.000000 0.724(3) 0.065(3) Uani 1 2 d DS T P . .
C11 C 0.247(5) -0.159(4) 0.510(7) 0.13(2) Uiso 0.5 1 d D . P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0228(4) 0.0109(3) 0.0263(4) 0.000 0.0166(3) 0.000
Fe1 0.0238(17) 0.0088(14) 0.0261(17) 0.000 0.0184(15) 0.000
Fe2 0.0246(17) 0.0076(13) 0.0244(17) 0.000 0.0182(15) 0.000
N4 0.029(5) 0.016(5) 0.024(5) -0.001(4) 0.018(5) -0.002(4)
N3 0.033(6) 0.015(5) 0.033(5) 0.002(4) 0.025(5) 0.000(4)
C6 0.024(6) 0.014(5) 0.023(6) -0.002(5) 0.015(5) -0.003(4)
C5 0.030(6) 0.012(5) 0.035(6) 0.001(5) 0.027(6) 0.001(4)
N1 0.075(6) 0.041(5) 0.070(6) 0.000 0.050(5) 0.000
N5 0.053(5) 0.036(4) 0.094(7) 0.000 0.044(5) 0.000
O2 0.053(5) 0.036(4) 0.094(7) 0.000 0.044(5) 0.000
C3 0.075(6) 0.041(5) 0.070(6) 0.000 0.050(5) 0.000
C9 0.053(5) 0.036(4) 0.094(7) 0.000 0.044(5) 0.000
O1 0.075(6) 0.041(5) 0.070(6) 0.000 0.050(5) 0.000
C2 0.075(6) 0.041(5) 0.070(6) 0.000 0.050(5) 0.000
N6 0.053(5) 0.036(4) 0.094(7) 0.000 0.044(5) 0.000
N2 0.075(6) 0.041(5) 0.070(6) 0.000 0.050(5) 0.000
C10 0.053(5) 0.036(4) 0.094(7) 0.000 0.044(5) 0.000
C1 0.075(6) 0.041(5) 0.070(6) 0.000 0.050(5) 0.000
C4 0.075(6) 0.041(5) 0.070(6) 0.000 0.050(5) 0.000
C7 0.053(5) 0.036(4) 0.094(7) 0.000 0.044(5) 0.000
C8 0.053(5) 0.036(4) 0.094(7) 0.000 0.044(5) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C6 1.990(12) . ?
Pt1 C6 1.990(12) 6_565 ?
Pt1 C5 1.987(11) 6_565 ?
Pt1 C5 1.987(11) . ?
Fe1 N3 1.965(10) . ?
Fe1 N3 1.965(10) 2_656 ?
Fe1 N3 1.965(10) 5_656 ?
Fe1 N3 1.965(10) 6 ?
Fe1 N1 2.06(2) 5_656 ?
Fe1 N1 2.06(2) . ?
Fe2 N4 1.951(10) . ?
Fe2 N4 1.951(10) 5_677 ?
Fe2 N4 1.951(10) 2_657 ?
Fe2 N4 1.951(10) 6_575 ?
Fe2 N5 2.03(2) . ?
Fe2 N5 2.03(2) 5_677 ?
N4 C6 1.138(15) . ?
N3 C5 1.142(15) . ?
N1 C1 1.45(4) . ?
N1 C4 1.30(3) . ?
N5 C10 1.36(4) . ?
N5 C7 1.33(4) . ?
O2 C8 1.24(3) . ?
C3 O1 1.28(3) . ?
C3 C2 1.38(3) . ?
C3 C4 1.4001(13) . ?
C9 H9 0.9500 . ?
C9 N6 1.3298(13) . ?
C9 C8 1.40(4) . ?
C2 H2 0.9500 . ?
C2 N2 1.3298(11) . ?
N6 C10 1.36(3) . ?
O3 C11 1.18(2) . ?
O3 C11 1.18(2) 6 ?
N2 C1 1.38(3) . ?
C10 H10 0.9500 . ?
C1 H1 0.9500 . ?
C4 H4 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.3301(11) . ?
C11 C11 1.36(8) 7_546 ?

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
C6 Pt1 C6 88.8(7) . 6_565 ?
C5 Pt1 C6 178.7(5) . . ?
C5 Pt1 C6 90.7(5) . 6_565 ?
C5 Pt1 C6 90.7(5) 6_565 . ?
C5 Pt1 C6 178.7(5) 6_565 6_565 ?
C5 Pt1 C5 89.7(6) 6_565 . ?
N3 Fe1 N3 90.1(6) 5_656 6 ?
N3 Fe1 N3 180.0 5_656 . ?
N3 Fe1 N3 90.1(6) 2_656 . ?
N3 Fe1 N3 180.0 6 2_656 ?
N3 Fe1 N3 89.9(6) 6 . ?
N3 Fe1 N3 89.9(6) 5_656 2_656 ?
N3 Fe1 N1 91.4(6) 5_656 5_656 ?
N3 Fe1 N1 88.6(6) 2_656 . ?
N3 Fe1 N1 91.4(6) 6 . ?
N3 Fe1 N1 88.6(6) 5_656 . ?
N3 Fe1 N1 88.6(6) . 5_656 ?
N3 Fe1 N1 91.4(6) . . ?
N3 Fe1 N1 88.6(6) 6 5_656 ?
N3 Fe1 N1 91.4(6) 2_656 5_656 ?
N1 Fe1 N1 180.0 5_656 . ?
N4 Fe2 N4 90.0(6) 6_575 . ?
N4 Fe2 N4 90.0(6) 5_677 6_575 ?
N4 Fe2 N4 180.0 5_677 . ?
N4 Fe2 N4 90.0(6) 5_677 2_657 ?
N4 Fe2 N4 180.0 6_575 2_657 ?
N4 Fe2 N4 90.0(6) 2_657 . ?
N4 Fe2 N5 91.1(6) 6_575 . ?
N4 Fe2 N5 88.9(6) . 5_677 ?
N4 Fe2 N5 91.1(6) 5_677 5_677 ?
N4 Fe2 N5 91.1(6) . . ?
N4 Fe2 N5 88.9(6) 5_677 . ?
N4 Fe2 N5 91.1(6) 2_657 5_677 ?
N4 Fe2 N5 88.9(6) 2_657 . ?
N4 Fe2 N5 88.9(6) 6_575 5_677 ?
N5 Fe2 N5 180.0 5_677 . ?
C6 N4 Fe2 174.7(10) . . ?
C5 N3 Fe1 177.1(11) . . ?
N4 C6 Pt1 177.6(11) . . ?
N3 C5 Pt1 178.3(10) . . ?
C1 N1 Fe1 114.2(19) . . ?
C4 N1 Fe1 128.8(18) . . ?
C4 N1 C1 117(2) . . ?
C10 N5 Fe2 119(2) . . ?
C7 N5 Fe2 122(2) . . ?
C7 N5 C10 119(2) . . ?
O1 C3 C2 121.2(17) . . ?
O1 C3 C4 119(3) . . ?
C2 C3 C4 120(2) . . ?
N6 C9 H9 119.7 . . ?
N6 C9 C8 121(2) . . ?
C8 C9 H9 119.7 . . ?
C3 C2 H2 118.2 . . ?
N2 C2 C3 124(2) . . ?
N2 C2 H2 118.2 . . ?
C9 N6 C10 113(2) . . ?
C11 O3 C11 150(9) 6 . ?
C2 N2 C1 114.4(18) . . ?
N5 C10 N6 127(3) . . ?
N5 C10 H10 116.6 . . ?
N6 C10 H10 116.6 . . ?
N1 C1 H1 117.7 . . ?
N2 C1 N1 125(2) . . ?
N2 C1 H1 117.7 . . ?
N1 C4 C3 120(3) . . ?
N1 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
N5 C7 H7 121.6 . . ?
C8 C7 N5 117(3) . . ?
C8 C7 H7 121.6 . . ?
O2 C8 C9 109.3(16) . . ?
O2 C8 C7 127(3) . . ?
C7 C8 C9 124(3) . . ?
O3 C11 C11 153(10) . 7_546 ?

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 N2 180.000(5) . . . . ?
Fe1 N1 C4 C3 180.000(5) . . . . ?
Fe2 N5 C10 N6 180.000(10) . . . . ?
Fe2 N5 C7 C8 180.000(12) . . . . ?
N5 C7 C8 O2 180.000(15) . . . . ?
N5 C7 C8 C9 0.000(17) . . . . ?
C3 C2 N2 C1 0.000(7) . . . . ?
C9 N6 C10 N5 0.000(17) . . . . ?
O1 C3 C2 N2 180.000(1) . . . . ?
O1 C3 C4 N1 180.000(6) . . . . ?
C2 C3 C4 N1 0.000(6) . . . . ?
C2 N2 C1 N1 0.000(9) . . . . ?
N6 C9 C8 O2 180.000(9) . . . . ?
N6 C9 C8 C7 0.000(16) . . . . ?
C10 N5 C7 C8 0.000(18) . . . . ?
C1 N1 C4 C3 0.000(6) . . . . ?
C4 N1 C1 N2 0.000(9) . . . . ?
C4 C3 C2 N2 0.000(3) . . . . ?
C7 N5 C10 N6 0.000(16) . . . . ?
C8 C9 N6 C10 0.000(18) . . . . ?
C11 O3 C11 C11 -143(15) 6 . . 7_546 ?

_shelx_res_file                  
;
TITL rt590_ohpymptetoh_120k_a.res in C2/m
    rt590_ohpymptetoh_120k.res
    created by SHELXL-2018/3 at 11:58:51 on 26-Sep-2022
REM Old TITL RT590_OHPymPtEtOH_120K in C2/m
REM SHELXT solution in C2/m: R1 0.094, Rweak 0.018, Alpha 0.021
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C10 N13 Fe Pt
CELL 0.71073 21.1233 7.1448 14.419 90 132.393 90
ZERR 4 0.0038 0.0003 0.0027 0 0.031 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pt
UNIT 52 24 4 32 10 4
DFIX 1.2 C11 O3
DFIX 1.4 0.001 C3 C4
DFIX 1.33 0.001 C2 N2
DFIX 1.33 0.001 C8 C7
DFIX 1.33 0.001 C9 N6
EADP N2 C1 C2 C3 C4 N1 O1
EADP C7 N5 C10 N6 C9 C8 O2

L.S. 10
PLAN  2
SIZE 0.2 0.2 0.05
TEMP -153.1(1)
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\RT590_OHPymPtEtOH_120K.hkl">
REM </olex2.extras>

WGHT    0.049200  114.213600
FVAR       0.18049
PT1   6    0.483375    0.500000    0.734644    10.50000    0.02281    0.01085 =
         0.02631    0.00000    0.01656    0.00000
FE1   3    0.500000    0.000000    0.500000    10.25000    0.02384    0.00878 =
         0.02606    0.00000    0.01841    0.00000
FE2   3    0.500000    1.000000    1.000000    10.25000    0.02459    0.00764 =
         0.02442    0.00000    0.01825    0.00000
N4    4    0.484562    0.806803    0.890564    11.00000    0.02864    0.01575 =
         0.02448   -0.00064    0.01806   -0.00192
N3    4    0.490060    0.194266    0.586062    11.00000    0.03315    0.01465 =
         0.03343    0.00186    0.02537   -0.00035
C6    1    0.482234    0.694902    0.832116    11.00000    0.02395    0.01440 =
         0.02266   -0.00157    0.01507   -0.00280
C5    1    0.487167    0.303816    0.640805    11.00000    0.03032    0.01194 =
         0.03478    0.00086    0.02672    0.00065
N1    4    0.369056    0.000000    0.349948    10.50000    0.07531    0.04115 =
         0.07012    0.00000    0.05028    0.00000
N5    4    0.372469    1.000000    0.902560    10.50000    0.05287    0.03608 =
         0.09357    0.00000    0.04396    0.00000
O2    5    0.167299    1.000000    0.609867    10.50000    0.05287    0.03608 =
         0.09357    0.00000    0.04396    0.00000
C3    1    0.237075    0.000000    0.142137    10.50000    0.07531    0.04115 =
         0.07012    0.00000    0.05028    0.00000
C9    1    0.205926    1.000000    0.791720    10.50000    0.05287    0.03608 =
         0.09357    0.00000    0.04396    0.00000
AFIX  43
H9    2    0.146610    1.000000    0.748045    10.50000   -1.20000
AFIX   0
O1    5    0.197493    0.000000    0.025582    10.50000    0.07531    0.04115 =
         0.07012    0.00000    0.05028    0.00000
C2    1    0.192883    0.000000    0.181592    10.50000    0.07531    0.04115 =
         0.07012    0.00000    0.05028    0.00000
AFIX  43
H2    2    0.132014    0.000000    0.119523    10.50000   -1.20000
AFIX   0
N6    4   10.263870   11.000000   10.916589    10.50000    0.05287    0.03608 =
         0.09357    0.00000    0.04396    0.00000

O3    5    0.231123    0.000000    0.481897    10.25000    0.07806
N2    4   10.230949   10.000000   10.301710    10.50000    0.07531    0.04115 =
         0.07012    0.00000    0.05028    0.00000
C10   1    0.346210    1.000000    0.966595    10.50000    0.05287    0.03608 =
         0.09357    0.00000    0.04396    0.00000
AFIX  43
H10   2    0.389958    1.000000    1.055637    10.50000   -1.20000
AFIX   0
C1    1    0.319123    0.000000    0.385315    10.50000    0.07531    0.04115 =
         0.07012    0.00000    0.05028    0.00000
AFIX  43
H1    2    0.349367    0.000000    0.472372    10.50000   -1.20000
AFIX   0
C4    1    0.326822    0.000000    0.230458    10.50000    0.07531    0.04115 =
         0.07012    0.00000    0.05028    0.00000
AFIX  43
H4    2    0.356982    0.000000    0.203010    10.50000   -1.20000
AFIX   0
C7    1    0.313199    1.000000    0.777465    10.50000    0.05287    0.03608 =
         0.09357    0.00000    0.04396    0.00000
AFIX  43
H7    2    0.328444    1.000000    0.728735    10.50000   -1.20000
AFIX   0
C8    1    0.231694    1.000000    0.724040    10.50000    0.05287    0.03608 =
         0.09357    0.00000    0.04396    0.00000

C11   1    0.246565   -0.159126    0.510353    10.50000    0.13399
HKLF 4




REM  rt590_ohpymptetoh_120k_a.res in C2/m
REM wR2 = 0.1515, GooF = S = 1.152, Restrained GooF = 1.151 for all data
REM R1 = 0.0614 for 1708 Fo > 4sig(Fo) and 0.0695 for all 1890 data
REM 90 parameters refined using 5 restraints

END

WGHT      0.0492    114.3524

REM Highest difference peak  3.209,  deepest hole -2.972,  1-sigma level  0.335
Q1    1   0.1984  1.0000  0.8711  10.50000  0.05    3.21
Q2    1   0.2770  0.0000  0.1179  10.50000  0.05    2.85
;
_shelx_res_checksum              62501
_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 1.366
_oxdiff_exptl_absorpt_empirical_full_min 0.827
####################################################################### 
# 
# 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_rt475_ohpympt_meoh_120k
_database_code_depnum_ccdc_archive 'CCDC 2209629'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-27 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_rt475_ohpympt_meoh_120k 
;
PROBLEM: Check Calcd Resid. Dens.  0.82Ang From C8              3.87 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_120k_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.91Ang From C3              3.83 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_120k_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.00Ang From N2              3.57 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT342_rt475_ohpympt_meoh_120k 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.
RESPONSE: This alerts arises from the strong disorder of the guest in the structural pores and from the deterioration of the crystal due to the desorption/readsorption processes
;
_vrf_PLAT971_rt475_ohpympt_meoh_120k_4 
;
PROBLEM: Check Calcd Resid. Dens.  1.20Ang From N6              3.39 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_120k_5 
;
PROBLEM: Check Calcd Resid. Dens.  0.03Ang From N5              3.26 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_120k_6 
;
PROBLEM: Check Calcd Resid. Dens.  0.05Ang From N1              3.14 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_120k_7 
;
PROBLEM: Check Calcd Resid. Dens.  0.65Ang From C8              2.80 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C8 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_120k 
;
PROBLEM: Check Calcd Resid. Dens.  0.09Ang From O2             -2.60 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Tuesday 27 September 2022 04:39 PM
# end Validation Reply Form

_audit_creation_date             2022-09-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 Fe N8 O2 Pt, 0.25(C2 H8 O2)'
_chemical_formula_sum            'C12.50 H8 Fe N8 O2.50 Pt'
_chemical_formula_weight         561.21
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.2206(10)
_cell_length_b                   7.11020(10)
_cell_length_c                   15.5704(7)
_cell_angle_alpha                90
_cell_angle_beta                 137.204(9)
_cell_angle_gamma                90
_cell_volume                     1596.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3817
_cell_measurement_temperature    120.05(10)
_cell_measurement_theta_max      29.5450
_cell_measurement_theta_min      3.8430
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.693
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.335
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6547
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.759
_diffrn_reflns_theta_min         2.826
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00  42.00   1.00    5.00    --   22.05  77.00 -30.00   52
  2  ω    -15.00  66.00   1.00    5.00    --   22.05 -99.00  30.00   81
  3  ω    -52.00  96.00   1.00    5.00    --   22.05   0.00  30.00  148
  4  ω    -49.00 -24.00   1.00    5.00    --  -21.11  38.00 -90.00   25
  5  ω      0.00  91.00   1.00    5.00    --   22.05  57.00 150.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0099350000
_diffrn_orient_matrix_UB_12      -0.0974242000
_diffrn_orient_matrix_UB_13      -0.0064732000
_diffrn_orient_matrix_UB_21      -0.0303293000
_diffrn_orient_matrix_UB_22      0.0186017000
_diffrn_orient_matrix_UB_23      0.0045146000
_diffrn_orient_matrix_UB_31      -0.0374454000
_diffrn_orient_matrix_UB_32      0.0107762000
_diffrn_orient_matrix_UB_33      -0.0665745000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2125
_reflns_number_total             2231
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.790
_refine_diff_density_min         -2.640
_refine_diff_density_rms         0.315
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         2231
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0431
_refine_ls_restrained_S_all      1.132
_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)+(0.0314P)²+79.7543P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1053
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(C9) = Uanis(N6) = Uanis(C10) = Uanis(N5) = Uanis(C7) =
Uanis(O2)
Uanis(N1) = Uanis(C4) = Uanis(C3) = Uanis(O1) = Uanis(C2) = Uanis(N2) =
Uanis(C1)
3. Others
 Fixed Sof: O3(0.25) H3(0.25) C11(0.25) H11a(0.25) H11b(0.25) H11c(0.25)
 Fixed X: O3(0.25353) C11(0.24901)
 Fixed Y: O3(0.5) C11(0.6913)
 Fixed Z: O3(0.0141) C11(0.00136)
4.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C1(H1), C2(H2), C4(H4), C9(H9)
4.b Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c)
4.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.24943(2) 0.500000 0.23299(3) 0.00693(12) Uani 1 2 d S T P . .
Fe1 Fe 0.500000 1.000000 0.500000 0.0073(4) Uani 1 4 d S T P . .
Fe2 Fe 0.000000 0.000000 0.000000 0.0070(4) Uani 1 4 d S T P . .
N4 N 0.0938(4) 0.1930(9) 0.0780(6) 0.0133(12) Uani 1 1 d . . . . .
N3 N 0.4045(4) 0.8081(9) 0.3951(6) 0.0142(12) Uani 1 1 d . . . . .
C5 C 0.3471(5) 0.6970(10) 0.3350(6) 0.0126(13) Uani 1 1 d . . . . .
C6 C 0.1511(5) 0.3034(10) 0.1330(7) 0.0138(14) Uani 1 1 d . . . . .
N5 N -0.0297(10) 0.000000 -0.1555(13) 0.0379(12) Uani 1 2 d S T P . .
N1 N 0.4814(9) 1.000000 0.6093(13) 0.0378(12) Uani 1 2 d S T P . .
O2 O 0.0703(8) 0.000000 -0.2626(11) 0.0379(12) Uani 1 2 d S T P . .
O1 O 0.3201(8) 1.000000 0.6233(10) 0.0378(12) Uani 1 2 d S T P . .
C7 C 0.0370(12) 0.000000 -0.1466(16) 0.0379(12) Uani 1 2 d S T P . .
H7 H 0.100724 0.000000 -0.067420 0.046 Uiso 1 2 calc R U P . .
C10 C -0.1208(12) 0.000000 -0.2719(15) 0.0379(12) Uani 1 2 d S T P . .
H10 H -0.166434 0.000000 -0.273532 0.046 Uiso 1 2 calc R U P . .
C1 C 0.5595(12) 1.000000 0.7384(15) 0.0378(12) Uani 1 2 d S T P . .
H1 H 0.617389 1.000000 0.767043 0.045 Uiso 1 2 calc R U P . .
C3 C 0.4008(12) 1.000000 0.6627(15) 0.0378(12) Uani 1 2 d S T P . .
C2 C 0.4866(11) 1.000000 0.7883(15) 0.0378(12) Uani 1 2 d S T P . .
H2 H 0.487068 1.000000 0.849741 0.045 Uiso 1 2 calc R U P . .
N2 N 0.5632(9) 1.000000 0.8281(13) 0.0378(12) Uani 1 2 d S T P . .
C4 C 0.4032(12) 1.000000 0.5715(16) 0.0378(12) Uani 1 2 d S T P . .
H4 H 0.346828 1.000000 0.483555 0.045 Uiso 1 2 calc R U P . .
C9 C -0.0912(12) 0.000000 -0.3775(16) 0.0379(12) Uani 1 2 d S T P . .
H9 H -0.112014 0.000000 -0.456198 0.046 Uiso 1 2 calc R U P . .
O3 O 0.253530 0.500000 0.014100 0.036(5) Uiso 0.25 1 d S . P A -1
H3 H 0.303692 0.470184 0.088093 0.055 Uiso 0.25 1 calc R U P A -1
N6 N -0.1513(10) 0.000000 -0.3841(13) 0.0379(12) Uani 1 2 d S T P . .
C8 C 0.0052(12) 0.000000 -0.2700(16) 0.0379(12) Uani 1 2 d S T P . .
C11 C 0.249009 0.691301 0.001361 0.017(6) Uiso 0.25 1 d . . P A -1
H11A H 0.204102 0.723898 -0.088392 0.025 Uiso 0.25 1 calc R U P A -1
H11B H 0.310251 0.740212 0.046887 0.025 Uiso 0.25 1 calc R U P A -1
H11C H 0.229435 0.746862 0.036460 0.025 Uiso 0.25 1 calc R U P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.00418(17) 0.00665(18) 0.00728(18) 0.000 0.00336(15) 0.000
Fe1 0.0044(8) 0.0056(8) 0.0073(8) 0.000 0.0029(7) 0.000
Fe2 0.0043(8) 0.0056(8) 0.0075(8) 0.000 0.0032(7) 0.000
N4 0.008(3) 0.011(3) 0.018(3) 0.001(2) 0.009(2) 0.002(2)
N3 0.011(3) 0.010(3) 0.011(3) -0.001(2) 0.005(2) 0.000(2)
C5 0.009(3) 0.012(3) 0.008(3) 0.001(3) 0.003(3) 0.002(3)
C6 0.012(3) 0.011(3) 0.018(3) 0.002(3) 0.011(3) 0.002(3)
N5 0.052(3) 0.029(3) 0.043(3) 0.000 0.038(3) 0.000
N1 0.041(3) 0.041(3) 0.038(3) 0.000 0.031(3) 0.000
O2 0.052(3) 0.029(3) 0.043(3) 0.000 0.038(3) 0.000
O1 0.041(3) 0.041(3) 0.038(3) 0.000 0.031(3) 0.000
C7 0.052(3) 0.029(3) 0.043(3) 0.000 0.038(3) 0.000
C10 0.052(3) 0.029(3) 0.043(3) 0.000 0.038(3) 0.000
C1 0.041(3) 0.041(3) 0.038(3) 0.000 0.031(3) 0.000
C3 0.041(3) 0.041(3) 0.038(3) 0.000 0.031(3) 0.000
C2 0.041(3) 0.041(3) 0.038(3) 0.000 0.031(3) 0.000
N2 0.041(3) 0.041(3) 0.038(3) 0.000 0.031(3) 0.000
C4 0.041(3) 0.041(3) 0.038(3) 0.000 0.031(3) 0.000
C9 0.052(3) 0.029(3) 0.043(3) 0.000 0.038(3) 0.000
N6 0.052(3) 0.029(3) 0.043(3) 0.000 0.038(3) 0.000
C8 0.052(3) 0.029(3) 0.043(3) 0.000 0.038(3) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C5 1.987(7) . ?
Pt1 C5 1.987(7) 6_565 ?
Pt1 C6 1.991(7) 6_565 ?
Pt1 C6 1.991(7) . ?
Fe1 N3 1.944(6) 6_575 ?
Fe1 N3 1.944(6) 5_676 ?
Fe1 N3 1.944(6) . ?
Fe1 N3 1.944(6) 2_656 ?
Fe1 N1 2.010(13) . ?
Fe1 N1 2.010(13) 5_676 ?
Fe2 N4 1.942(6) 6 ?
Fe2 N4 1.942(6) 5 ?
Fe2 N4 1.942(6) 2 ?
Fe2 N4 1.942(6) . ?
Fe2 N5 2.006(13) . ?
Fe2 N5 2.005(13) 5 ?
N4 C6 1.140(10) . ?
N3 C5 1.145(10) . ?
N5 C7 1.32(2) . ?
N5 C10 1.37(2) . ?
N1 C1 1.38(2) . ?
N1 C4 1.29(2) . ?
O2 C8 1.300(19) . ?
O1 C3 1.329(19) . ?
C7 H7 0.9500 . ?
C7 C8 1.50(2) . ?
C10 H10 0.9500 . ?
C10 N6 1.35(2) . ?
C1 H1 0.9500 . ?
C1 N2 1.341(19) . ?
C3 C2 1.38(2) . ?
C3 C4 1.46(2) . ?
C2 H2 0.9500 . ?
C2 N2 1.24(2) . ?
C4 H4 0.9500 . ?
C9 H9 0.9500 . ?
C9 N6 1.20(2) . ?
C9 C8 1.40(2) . ?
O3 H3 0.8400 . ?
O3 C11 1.367751(19) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 Pt1 C5 89.6(4) . 6_565 ?
C5 Pt1 C6 178.7(3) 6_565 6_565 ?
C5 Pt1 C6 90.6(3) . 6_565 ?
C5 Pt1 C6 90.6(3) 6_565 . ?
C5 Pt1 C6 178.8(3) . . ?
C6 Pt1 C6 89.2(4) 6_565 . ?
N3 Fe1 N3 90.8(4) 5_676 6_575 ?
N3 Fe1 N3 180.0 5_676 . ?
N3 Fe1 N3 180.0 6_575 2_656 ?
N3 Fe1 N3 90.8(4) 2_656 . ?
N3 Fe1 N3 89.2(4) 6_575 . ?
N3 Fe1 N3 89.2(4) 5_676 2_656 ?
N3 Fe1 N1 91.1(3) 5_676 . ?
N3 Fe1 N1 91.1(3) 6_575 5_676 ?
N3 Fe1 N1 88.9(3) . . ?
N3 Fe1 N1 88.9(3) 5_676 5_676 ?
N3 Fe1 N1 91.1(3) 2_656 . ?
N3 Fe1 N1 88.9(3) 2_656 5_676 ?
N3 Fe1 N1 88.9(3) 6_575 . ?
N3 Fe1 N1 91.1(3) . 5_676 ?
N1 Fe1 N1 180.0 . 5_676 ?
N4 Fe2 N4 89.9(4) 5 2 ?
N4 Fe2 N4 180.0 . 5 ?
N4 Fe2 N4 90.1(4) . 2 ?
N4 Fe2 N4 89.9(4) . 6 ?
N4 Fe2 N4 90.1(4) 5 6 ?
N4 Fe2 N4 180.0(4) 6 2 ?
N4 Fe2 N5 88.6(3) . 5 ?
N4 Fe2 N5 91.4(3) 2 5 ?
N4 Fe2 N5 88.6(3) 6 5 ?
N4 Fe2 N5 88.6(3) 5 . ?
N4 Fe2 N5 91.4(3) . . ?
N4 Fe2 N5 91.4(3) 5 5 ?
N4 Fe2 N5 91.4(3) 6 . ?
N4 Fe2 N5 88.6(3) 2 . ?
N5 Fe2 N5 180.0 5 . ?
C6 N4 Fe2 174.2(6) . . ?
C5 N3 Fe1 177.5(6) . . ?
N3 C5 Pt1 178.8(7) . . ?
N4 C6 Pt1 177.2(7) . . ?
C7 N5 Fe2 120.7(12) . . ?
C7 N5 C10 120.3(14) . . ?
C10 N5 Fe2 119.0(11) . . ?
C1 N1 Fe1 117.5(10) . . ?
C4 N1 Fe1 126.8(11) . . ?
C4 N1 C1 115.7(14) . . ?
N5 C7 H7 122.3 . . ?
N5 C7 C8 115.3(16) . . ?
C8 C7 H7 122.3 . . ?
N5 C10 H10 117.1 . . ?
N6 C10 N5 125.7(15) . . ?
N6 C10 H10 117.1 . . ?
N1 C1 H1 116.3 . . ?
N2 C1 N1 127.4(15) . . ?
N2 C1 H1 116.3 . . ?
O1 C3 C2 124.5(14) . . ?
O1 C3 C4 120.3(14) . . ?
C2 C3 C4 115.2(14) . . ?
C3 C2 H2 117.0 . . ?
N2 C2 C3 126.1(15) . . ?
N2 C2 H2 117.0 . . ?
C2 N2 C1 115.1(14) . . ?
N1 C4 C3 120.5(15) . . ?
N1 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
N6 C9 H9 115.4 . . ?
N6 C9 C8 129.1(16) . . ?
C8 C9 H9 115.4 . . ?
C11 O3 H3 109.5 . . ?
C9 N6 C10 114.8(16) . . ?
O2 C8 C7 116.0(15) . . ?
O2 C8 C9 129.2(15) . . ?
C9 C8 C7 114.8(15) . . ?
O3 C11 H11A 109.5 . . ?
O3 C11 H11B 109.5 . . ?
O3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N1 C1 N2 180.000(9) . . . . ?
Fe1 N1 C4 C3 180.000(8) . . . . ?
Fe2 N5 C7 C8 180.000(3) . . . . ?
Fe2 N5 C10 N6 180.000(2) . . . . ?
N5 C7 C8 O2 180.000(3) . . . . ?
N5 C7 C8 C9 0.000(5) . . . . ?
N5 C10 N6 C9 0.000(6) . . . . ?
N1 C1 N2 C2 0.000(15) . . . . ?
O1 C3 C2 N2 180.000(12) . . . . ?
O1 C3 C4 N1 180.000(9) . . . . ?
C7 N5 C10 N6 0.000(5) . . . . ?
C10 N5 C7 C8 0.000(4) . . . . ?
C1 N1 C4 C3 0.000(11) . . . . ?
C3 C2 N2 C1 0.000(15) . . . . ?
C2 C3 C4 N1 0.000(12) . . . . ?
C4 N1 C1 N2 0.000(13) . . . . ?
C4 C3 C2 N2 0.000(14) . . . . ?
N6 C9 C8 O2 180.000(4) . . . . ?
N6 C9 C8 C7 0.000(7) . . . . ?
C8 C9 N6 C10 0.000(8) . . . . ?

_shelx_res_file                  
;
TITL rt475_ohpympt_meoh_120k_a.res in C2/m
    rt475_ohpympt_meoh_120k.res
    created by SHELXL-2018/3 at 15:59:47 on 27-Sep-2022
REM Old TITL RT475_OHPymPt_MeOH_120K in C2/m
REM SHELXT solution in C2/m: R1 0.052, Rweak 0.015, Alpha 0.023
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C11 N12 Fe Pt
CELL 0.71073 21.2206 7.1102 15.5704 90 137.204 90
ZERR 4 0.001 0.0001 0.0007 0 0.009 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pt
UNIT 50 32 4 32 10 4
EADP C8 C9 N6 C10 N5 C7 O2
EADP N1 C4 C3 O1 C2 N2 C1

L.S. 15
PLAN  1
TEMP -153.13
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\RT475_OHPymPt_MeOH_120K.hkl">
REM </olex2.extras>

WGHT    0.031400   79.754295
FVAR       0.17658
PT1   6    0.249426    0.500000    0.232993    10.50000    0.00418    0.00665 =
         0.00728    0.00000    0.00336    0.00000
FE1   3    0.500000    1.000000    0.500000    10.25000    0.00436    0.00556 =
         0.00732    0.00000    0.00287    0.00000
FE2   3    0.000000    0.000000    0.000000    10.25000    0.00427    0.00564 =
         0.00754    0.00000    0.00324    0.00000
N4    4    0.093781    0.192999    0.078000    11.00000    0.00827    0.01062 =
         0.01788    0.00111    0.00864    0.00164
N3    4    0.404525    0.808101    0.395122    11.00000    0.01071    0.01021 =
         0.01104   -0.00059    0.00467    0.00037
C5    1    0.347073    0.696978    0.335019    11.00000    0.00898    0.01212 =
         0.00792    0.00062    0.00348    0.00172
C6    1    0.151069    0.303385    0.132970    11.00000    0.01183    0.01141 =
         0.01841    0.00226    0.01122    0.00236
N5    4   -0.029698    0.000000   -0.155532    10.50000    0.05166    0.02895 =
         0.04344    0.00000    0.03811    0.00000
N1    4    0.481413    1.000000    0.609333    10.50000    0.04052    0.04089 =
         0.03838    0.00000    0.03092    0.00000
O2    5    0.070347    0.000000   -0.262628    10.50000    0.05166    0.02895 =
         0.04344    0.00000    0.03811    0.00000
O1    5    0.320053    1.000000    0.623256    10.50000    0.04052    0.04089 =
         0.03838    0.00000    0.03092    0.00000
C7    1    0.036954    0.000000   -0.146562    10.50000    0.05166    0.02895 =
         0.04344    0.00000    0.03811    0.00000
AFIX  43
H7    2    0.100724    0.000000   -0.067420    10.50000   -1.20000
AFIX   0
C10   1   -0.120808    0.000000   -0.271925    10.50000    0.05166    0.02895 =
         0.04344    0.00000    0.03811    0.00000
AFIX  43
H10   2   -0.166434    0.000000   -0.273532    10.50000   -1.20000
AFIX   0
C1    1    0.559522    1.000000    0.738357    10.50000    0.04052    0.04089 =
         0.03838    0.00000    0.03092    0.00000
AFIX  43
H1    2    0.617389    1.000000    0.767043    10.50000   -1.20000
AFIX   0
C3    1    0.400785    1.000000    0.662732    10.50000    0.04052    0.04089 =
         0.03838    0.00000    0.03092    0.00000
C2    1    0.486590    1.000000    0.788251    10.50000    0.04052    0.04089 =
         0.03838    0.00000    0.03092    0.00000
AFIX  43
H2    2    0.487068    1.000000    0.849741    10.50000   -1.20000
AFIX   0
N2    4    0.563247    1.000000    0.828139    10.50000    0.04052    0.04089 =
         0.03838    0.00000    0.03092    0.00000
C4    1    0.403236    1.000000    0.571504    10.50000    0.04052    0.04089 =
         0.03838    0.00000    0.03092    0.00000
AFIX  43
H4    2    0.346828    1.000000    0.483555    10.50000   -1.20000
AFIX   0
C9    1   -0.091202    0.000000   -0.377495    10.50000    0.05166    0.02895 =
         0.04344    0.00000    0.03811    0.00000
AFIX  43
H9    2   -0.112014    0.000000   -0.456198    10.50000   -1.20000
AFIX   0

PART -1
O3    5   10.253530   10.500000   10.014100    10.25000    0.03637
AFIX 147
H3    2    0.303692    0.470184    0.088093    10.25000   -1.50000
AFIX   0

PART 0
N6    4   -0.151268    0.000000   -0.384125    10.50000    0.05166    0.02895 =
         0.04344    0.00000    0.03811    0.00000
C8    1    0.005224    0.000000   -0.270048    10.50000    0.05166    0.02895 =
         0.04344    0.00000    0.03811    0.00000

PART -1
C11   1   10.249009   10.691301   10.001361    10.25000    0.01676
AFIX 137
H11A  2    0.204102    0.723898   -0.088392    10.25000   -1.50000
H11B  2    0.310251    0.740212    0.046887    10.25000   -1.50000
H11C  2    0.229435    0.746862    0.036460    10.25000   -1.50000
AFIX   0
HKLF 4




REM  rt475_ohpympt_meoh_120k_a.res in C2/m
REM wR2 = 0.1053, GooF = S = 1.132, Restrained GooF = 1.132 for all data
REM R1 = 0.0431 for 2125 Fo > 4sig(Fo) and 0.0456 for all 2231 data
REM 91 parameters refined using 0 restraints

END

WGHT      0.0314     79.7646

REM Highest difference peak  3.790,  deepest hole -2.640,  1-sigma level  0.315
Q1    1   0.0617  0.0000 -0.2012  10.50000  0.05    3.79
;
_shelx_res_checksum              50321
_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 1.397
_oxdiff_exptl_absorpt_empirical_full_min 0.653
####################################################################### 
# 
# 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_rt366_feohpmdpd_270k_0m_a
_database_code_depnum_ccdc_archive 'CCDC 2209621'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_rt366_feohpmdpd_270k_0m_a 
;
PROBLEM: Check Calcd Resid. Dens.  0.95Ang From Pd1             2.98 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Monday 26 September 2022 03:56 PM
# end Validation Reply Form

_audit_creation_date             2022-05-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H8 Fe N8 O2 Pd, O'
_chemical_formula_sum            'C12 H9 Fe N8 O3 Pd'
_chemical_formula_weight         475.52
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.491(9)
_cell_length_b                   7.501(3)
_cell_length_c                   16.009(8)
_cell_angle_alpha                90
_cell_angle_beta                 136.955(14)
_cell_angle_gamma                90
_cell_volume                     1761.5(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7100
_cell_measurement_temperature    270.0
_cell_measurement_theta_max      30.39
_cell_measurement_theta_min      2.79
_shelx_estimated_absorpt_T_max   0.964
_shelx_estimated_absorpt_T_min   0.603
_exptl_absorpt_coefficient_mu    1.873
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1071 before and 0.0699 after correction.
The Ratio of minimum to maximum transmission is 0.8613.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19447
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.366
_diffrn_reflns_theta_min         2.545
_diffrn_ambient_temperature      270.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2284
_reflns_number_total             2795
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.836
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.0065(8)
_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   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2795
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0586
_refine_ls_restrained_S_all      1.104
_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)+(0.0643P)²+27.4453P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1735
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1(0.5) H2(0.5) O3(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C7(H7), C1(H1A), C9(H9), C2(H2A)
3.b Tetrahedral OH refined with riding coordinates:
 O2(H2)
3.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.74784(3) 0.500000 0.23366(5) 0.0246(2) Uani 1 2 d S T P . .
Fe1 Fe 1.000000 1.000000 0.500000 0.0269(3) Uani 1 4 d S T P . .
Fe2 Fe 0.500000 0.000000 0.000000 0.0250(3) Uani 1 4 d S T P . .
N3 N 0.8962(3) 0.7992(7) 0.3970(5) 0.0360(11) Uani 1 1 d . . . . .
N4 N 0.5989(3) 0.2018(7) 0.0733(5) 0.0369(11) Uani 1 1 d . . . . .
N5 N 0.5419(5) 0.000000 0.1753(7) 0.0369(15) Uani 1 2 d S T P . .
C5 C 0.8427(3) 0.6905(7) 0.3384(5) 0.0277(10) Uani 1 1 d . . . . .
C6 C 0.6530(3) 0.3105(7) 0.1296(5) 0.0283(10) Uani 1 1 d . . . . .
O1 O 0.8253(5) 1.000000 0.6378(7) 0.072(3) Uani 1 2 d S T P . .
H1 H 0.783149 0.973888 0.565141 0.108 Uiso 0.5 1 calc R U P . .
N1 N 0.9908(5) 1.000000 0.6315(7) 0.0396(16) Uani 1 2 d S T P . .
N6 N 0.6558(6) 0.000000 0.3921(8) 0.053(2) Uani 1 2 d S T P . .
C4 C 0.9110(6) 1.000000 0.5919(8) 0.0378(18) Uani 1 2 d S T P . .
H4 H 0.857874 1.000000 0.508107 0.045 Uiso 1 2 calc R U P . .
N2 N 1.0663(6) 1.000000 0.8371(8) 0.058(2) Uani 1 2 d S T P . .
C10 C 0.6286(6) 0.000000 0.2853(8) 0.045(2) Uani 1 2 d S T P . .
H10 H 0.673526 0.000000 0.288348 0.054 Uiso 1 2 calc R U P . .
O2 O 0.4338(7) 0.000000 0.2703(10) 0.092(4) Uani 1 2 d S T P . .
H2 H 0.391772 -0.064355 0.213942 0.139 Uiso 0.5 1 calc R U P . .
C7 C 0.4766(7) 0.000000 0.1679(10) 0.045(2) Uani 1 2 d S T P . .
H7 H 0.415904 0.000000 0.091613 0.054 Uiso 1 2 calc R U P . .
C3 C 0.9040(7) 1.000000 0.6718(10) 0.050(2) Uani 1 2 d S T P . .
C1 C 1.0636(7) 1.000000 0.7483(9) 0.054(3) Uani 1 2 d S T P . .
H1A H 1.119234 1.000000 0.774991 0.065 Uiso 1 2 calc R U P . .
C9 C 0.5903(9) 0.000000 0.3845(10) 0.055(3) Uani 1 2 d S T P . .
H9 H 0.607161 0.000000 0.457064 0.066 Uiso 1 2 calc R U P . .
C8 C 0.4987(8) 0.000000 0.2761(11) 0.053(3) Uani 1 2 d S T P . .
C2 C 0.9870(8) 1.000000 0.7967(9) 0.057(3) Uani 1 2 d S T P . .
H2A H 0.985609 1.000000 0.853450 0.068 Uiso 1 2 calc R U P . .
O3 O 0.2614(9) -0.089(4) 0.0363(12) 0.140(14) Uani 0.5 1 d . . P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0200(3) 0.0172(3) 0.0290(3) 0.000 0.0154(3) 0.000
Fe1 0.0171(6) 0.0174(6) 0.0301(7) 0.000 0.0121(6) 0.000
Fe2 0.0159(6) 0.0182(6) 0.0266(7) 0.000 0.0109(6) 0.000
N3 0.029(2) 0.030(2) 0.039(2) -0.005(2) 0.021(2) -0.0025(19)
N4 0.029(2) 0.028(2) 0.040(3) -0.003(2) 0.021(2) -0.0032(19)
N5 0.036(4) 0.039(4) 0.035(3) 0.000 0.026(3) 0.000
C5 0.022(2) 0.020(2) 0.029(2) 0.0003(19) 0.015(2) 0.0009(18)
C6 0.021(2) 0.020(2) 0.032(2) -0.0016(19) 0.016(2) -0.0028(18)
O1 0.043(4) 0.135(9) 0.046(4) 0.000 0.035(4) 0.000
N1 0.041(4) 0.037(4) 0.031(3) 0.000 0.024(3) 0.000
N6 0.049(5) 0.069(6) 0.037(4) 0.000 0.030(4) 0.000
C4 0.036(4) 0.042(5) 0.032(4) 0.000 0.024(4) 0.000
N2 0.047(5) 0.080(7) 0.040(4) 0.000 0.030(4) 0.000
C10 0.036(4) 0.063(6) 0.036(4) 0.000 0.026(4) 0.000
O2 0.071(6) 0.162(12) 0.081(6) 0.000 0.067(6) 0.000
C7 0.042(5) 0.047(5) 0.047(5) 0.000 0.033(4) 0.000
C3 0.044(5) 0.065(7) 0.046(5) 0.000 0.035(5) 0.000
C1 0.039(5) 0.069(7) 0.040(5) 0.000 0.025(4) 0.000
C9 0.070(7) 0.061(7) 0.048(6) 0.000 0.048(6) 0.000
C8 0.066(7) 0.055(6) 0.063(6) 0.000 0.055(6) 0.000
C2 0.050(6) 0.083(9) 0.036(5) 0.000 0.031(5) 0.000
O3 0.060(7) 0.29(4) 0.063(8) -0.021(12) 0.043(7) -0.010(12)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C5 2.004(5) . ?
Pd1 C5 2.004(5) 6_565 ?
Pd1 C6 1.997(5) . ?
Pd1 C6 1.997(5) 6_565 ?
Fe1 N3 2.142(5) 5_776 ?
Fe1 N3 2.142(5) 6_575 ?
Fe1 N3 2.142(5) 2_756 ?
Fe1 N3 2.142(5) . ?
Fe1 N1 2.253(8) 5_776 ?
Fe1 N1 2.253(8) . ?
Fe2 N4 2.131(5) 5_655 ?
Fe2 N4 2.131(5) 6 ?
Fe2 N4 2.131(5) 2_655 ?
Fe2 N4 2.131(5) . ?
Fe2 N5 2.234(7) . ?
Fe2 N5 2.234(7) 5_655 ?
N3 C5 1.136(7) . ?
N4 C6 1.138(7) . ?
N5 C10 1.333(11) . ?
N5 C7 1.319(12) . ?
O1 H1 0.8200 . ?
O1 H1 0.82(16) 6_575 ?
O1 C3 1.344(12) . ?
N1 C4 1.326(12) . ?
N1 C1 1.292(12) . ?
N6 C10 1.344(12) . ?
N6 C9 1.322(15) . ?
C4 H4 0.9300 . ?
C4 C3 1.392(13) . ?
N2 C1 1.380(15) . ?
N2 C2 1.309(14) . ?
C10 H10 0.9300 . ?
O2 H2 0.8200 . ?
O2 H2 0.8200 6 ?
O2 C8 1.327(13) . ?
C7 H7 0.9300 . ?
C7 C8 1.423(15) . ?
C3 C2 1.403(15) . ?
C1 H1A 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.376(17) . ?
C2 H2A 0.9300 . ?

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
C5 Pd1 C5 91.0(3) . 6_565 ?
C6 Pd1 C5 89.1(2) 6_565 . ?
C6 Pd1 C5 179.7(2) 6_565 6_565 ?
C6 Pd1 C5 179.7(2) . . ?
C6 Pd1 C5 89.1(2) . 6_565 ?
C6 Pd1 C6 90.8(3) . 6_565 ?
N3 Fe1 N3 180.0 . 5_776 ?
N3 Fe1 N3 90.6(3) . 2_756 ?
N3 Fe1 N3 180.0 6_575 2_756 ?
N3 Fe1 N3 90.6(3) 5_776 6_575 ?
N3 Fe1 N3 89.4(3) 5_776 2_756 ?
N3 Fe1 N3 89.4(3) . 6_575 ?
N3 Fe1 N1 91.9(2) . 5_776 ?
N3 Fe1 N1 91.9(2) 5_776 . ?
N3 Fe1 N1 91.9(2) 2_756 . ?
N3 Fe1 N1 88.1(2) . . ?
N3 Fe1 N1 91.9(2) 6_575 5_776 ?
N3 Fe1 N1 88.1(2) 6_575 . ?
N3 Fe1 N1 88.1(2) 5_776 5_776 ?
N3 Fe1 N1 88.1(2) 2_756 5_776 ?
N1 Fe1 N1 180.0(4) 5_776 . ?
N4 Fe2 N4 90.5(3) 6 . ?
N4 Fe2 N4 89.5(3) 5_655 6 ?
N4 Fe2 N4 180.0(4) 5_655 . ?
N4 Fe2 N4 90.5(3) 5_655 2_655 ?
N4 Fe2 N4 180.0(3) 6 2_655 ?
N4 Fe2 N4 89.5(3) 2_655 . ?
N4 Fe2 N5 90.9(2) 5_655 . ?
N4 Fe2 N5 89.1(2) . . ?
N4 Fe2 N5 90.9(2) 2_655 . ?
N4 Fe2 N5 90.9(2) . 5_655 ?
N4 Fe2 N5 89.1(2) 5_655 5_655 ?
N4 Fe2 N5 89.1(2) 6 . ?
N4 Fe2 N5 89.1(2) 2_655 5_655 ?
N4 Fe2 N5 90.9(2) 6 5_655 ?
N5 Fe2 N5 180.0 . 5_655 ?
C5 N3 Fe1 175.4(5) . . ?
C6 N4 Fe2 167.1(5) . . ?
C10 N5 Fe2 123.4(6) . . ?
C7 N5 Fe2 117.5(6) . . ?
C7 N5 C10 119.1(8) . . ?
N3 C5 Pd1 179.5(5) . . ?
N4 C6 Pd1 177.6(5) . . ?
H1 O1 H1 27.6 . 6_575 ?
C3 O1 H1 109(4) . 6_575 ?
C3 O1 H1 109.5 . . ?
C4 N1 Fe1 121.4(6) . . ?
C1 N1 Fe1 120.8(7) . . ?
C1 N1 C4 117.8(9) . . ?
C9 N6 C10 116.1(9) . . ?
N1 C4 H4 118.9 . . ?
N1 C4 C3 122.2(9) . . ?
C3 C4 H4 118.9 . . ?
C2 N2 C1 115.6(9) . . ?
N5 C10 N6 124.7(9) . . ?
N5 C10 H10 117.7 . . ?
N6 C10 H10 117.7 . . ?
H2 O2 H2 72.1 . 6 ?
C8 O2 H2 109.5 . . ?
C8 O2 H2 109.5(5) . 6 ?
N5 C7 H7 119.8 . . ?
N5 C7 C8 120.3(9) . . ?
C8 C7 H7 119.8 . . ?
O1 C3 C4 125.2(10) . . ?
O1 C3 C2 119.3(10) . . ?
C4 C3 C2 115.5(9) . . ?
N1 C1 N2 125.9(10) . . ?
N1 C1 H1A 117.0 . . ?
N2 C1 H1A 117.0 . . ?
N6 C9 H9 117.9 . . ?
N6 C9 C8 124.2(10) . . ?
C8 C9 H9 117.9 . . ?
O2 C8 C7 121.1(11) . . ?
O2 C8 C9 123.3(11) . . ?
C9 C8 C7 115.6(10) . . ?
N2 C2 C3 123.0(10) . . ?
N2 C2 H2A 118.5 . . ?
C3 C2 H2A 118.5 . . ?

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 N1 C4 C3 180.000(3) . . . . ?
Fe1 N1 C1 N2 180.000(6) . . . . ?
Fe2 N5 C10 N6 180.000(3) . . . . ?
Fe2 N5 C7 C8 180.000(2) . . . . ?
N5 C7 C8 O2 180.000(2) . . . . ?
N5 C7 C8 C9 0.000(3) . . . . ?
O1 C3 C2 N2 180.000(5) . . . . ?
N1 C4 C3 O1 180.000(6) . . . . ?
N1 C4 C3 C2 0.000(6) . . . . ?
N6 C9 C8 O2 180.000(4) . . . . ?
N6 C9 C8 C7 0.000(5) . . . . ?
C4 N1 C1 N2 0.000(8) . . . . ?
C4 C3 C2 N2 0.000(8) . . . . ?
C10 N5 C7 C8 0.000(3) . . . . ?
C10 N6 C9 C8 0.000(5) . . . . ?
C7 N5 C10 N6 0.000(3) . . . . ?
C1 N1 C4 C3 0.000(7) . . . . ?
C1 N2 C2 C3 0.000(9) . . . . ?
C9 N6 C10 N5 0.000(4) . . . . ?
C2 N2 C1 N1 0.000(9) . . . . ?

_shelx_res_file                  
;
TITL RT366_FeOHPmdPd_270K_0m_a.res in C2/m
    rt366_feohpmdpd_270k_0m_a.res
    created by SHELXL-2018/3 at 22:56:44 on 19-May-2022
REM Old TITL Integration of RT366_FeOHPmdPd_270K
REM SHELXT solution in C2/m
REM R1 0.201, Rweak 0.014, Alpha 0.042, Orientation as input
REM Formula found by SHELXT: C12 I
CELL 0.71073 21.491 7.5008 16.0091 90 136.955 90
ZERR 4 0.0087 0.003 0.0079 0 0.014 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pd
UNIT 48 36 4 32 12 4

L.S. 10
PLAN  2
SIZE 0.2 0.3 0.02
TEMP -3.15
CONF
LIST 6
MORE -1
BOND $H
fmap 2
acta
OMIT -7 3 7
OMIT -8 2 6
OMIT -11 3 7
OMIT 16 0 4
REM <olex2.extras>
REM <HklSrc "%.\\RT366_FeOHPmdPd_270K_0m_a.hkl">
REM </olex2.extras>

WGHT    0.064300   27.445299
EXTI    0.006484
FVAR       0.28012
PD1   6    0.747838    0.500000    0.233658    10.50000    0.01996    0.01717 =
         0.02903    0.00000    0.01542    0.00000
FE1   3    1.000000    1.000000    0.500000    10.25000    0.01715    0.01737 =
         0.03005    0.00000    0.01213    0.00000
FE2   3    0.500000    0.000000    0.000000    10.25000    0.01590    0.01816 =
         0.02663    0.00000    0.01094    0.00000
N3    4    0.896210    0.799198    0.396955    11.00000    0.02892    0.02977 =
         0.03878   -0.00456    0.02138   -0.00251
N4    4    0.598924    0.201817    0.073281    11.00000    0.02880    0.02755 =
         0.04040   -0.00299    0.02080   -0.00322
N5    4    0.541924    0.000000    0.175300    10.50000    0.03585    0.03926 =
         0.03541    0.00000    0.02600    0.00000
C5    1    0.842722    0.690541    0.338382    11.00000    0.02169    0.01973 =
         0.02904    0.00029    0.01451    0.00094
C6    1    0.652965    0.310471    0.129575    11.00000    0.02135    0.01991 =
         0.03211   -0.00159    0.01585   -0.00281
O1    5    0.825336    1.000000    0.637829    10.50000    0.04297    0.13479 =
         0.04553    0.00000    0.03482    0.00000
AFIX 147
H1    2    0.783149    0.973888    0.565141    10.50000   -1.50000
AFIX   0
N1    4    0.990825    1.000000    0.631459    10.50000    0.04138    0.03714 =
         0.03115    0.00000    0.02362    0.00000
N6    4    0.655779    0.000000    0.392104    10.50000    0.04861    0.06918 =
         0.03716    0.00000    0.02990    0.00000
C4    1    0.910961    1.000000    0.591946    10.50000    0.03571    0.04204 =
         0.03248    0.00000    0.02392    0.00000
AFIX  43
H4    2    0.857874    1.000000    0.508107    10.50000   -1.20000
AFIX   0
N2    4    1.066322    1.000000    0.837140    10.50000    0.04728    0.07977 =
         0.03995    0.00000    0.03010    0.00000
C10   1    0.628623    0.000000    0.285305    10.50000    0.03574    0.06333 =
         0.03578    0.00000    0.02577    0.00000
AFIX  43
H10   2    0.673526    0.000000    0.288348    10.50000   -1.20000
AFIX   0
O2    5    0.433840    0.000000    0.270331    10.50000    0.07098    0.16210 =
         0.08120    0.00000    0.06743    0.00000
AFIX  83
H2    2    0.391772   -0.064355    0.213942    10.50000   -1.50000
AFIX   0
C7    1    0.476622    0.000000    0.167894    10.50000    0.04190    0.04693 =
         0.04740    0.00000    0.03322    0.00000
AFIX  43
H7    2    0.415904    0.000000    0.091613    10.50000   -1.20000
AFIX   0
C3    1    0.903956    1.000000    0.671801    10.50000    0.04407    0.06504 =
         0.04632    0.00000    0.03484    0.00000
C1    1    1.063619    1.000000    0.748317    10.50000    0.03938    0.06908 =
         0.03985    0.00000    0.02476    0.00000
AFIX  43
H1A   2    1.119234    1.000000    0.774991    10.50000   -1.20000
AFIX   0
C9    1    0.590268    0.000000    0.384499    10.50000    0.06983    0.06144 =
         0.04820    0.00000    0.04780    0.00000
AFIX  43
H9    2    0.607161    0.000000    0.457064    10.50000   -1.20000
AFIX   0
C8    1    0.498653    0.000000    0.276097    10.50000    0.06578    0.05473 =
         0.06336    0.00000    0.05495    0.00000
C2    1    0.986992    1.000000    0.796729    10.50000    0.05045    0.08291 =
         0.03563    0.00000    0.03074    0.00000
AFIX  43
H2A   2    0.985609    1.000000    0.853450    10.50000   -1.20000
AFIX   0

PART -1
O3    5    0.261424   -0.088805    0.036299    10.50000    0.06001    0.28975 =
         0.06315   -0.02145    0.04320   -0.01005
HKLF 4




REM  RT366_FeOHPmdPd_270K_0m_a.res in C2/m
REM wR2 = 0.1735, GooF = S = 1.104, Restrained GooF = 1.104 for all data
REM R1 = 0.0586 for 2284 Fo > 4sig(Fo) and 0.0807 for all 2795 data
REM 146 parameters refined using 0 restraints

END

WGHT      0.0638     28.6862

REM Highest difference peak  2.836,  deepest hole -1.148,  1-sigma level  0.211
Q1    1   0.8164  0.5000  0.3110  10.50000  0.05    2.84
Q2    1   0.6768  0.5000  0.1607  10.50000  0.05    2.42
;
_shelx_res_checksum              75137
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rt569_ohpympdmeoh_195k
_database_code_depnum_ccdc_archive 'CCDC 2209627'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-27 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_rt569_ohpympdmeoh_195k 
;
PROBLEM: Check Calcd Resid. Dens.  0.76Ang From Pd1             7.05 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_2 
;
PROBLEM: Check Calcd Resid. Dens.  1.15Ang From Pd1             6.04 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_3 
;
PROBLEM: Check Calcd Resid. Dens.  0.68Ang From Pd1             5.84 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_4 
;
PROBLEM: Check Calcd Resid. Dens.  1.38Ang From Pd1             5.11 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_5 
;
PROBLEM: Check Calcd Resid. Dens.  0.73Ang From C1              4.58 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_6 
;
PROBLEM: Check Calcd Resid. Dens.  0.51Ang From Fe1             4.33 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_7 
;
PROBLEM: Check Calcd Resid. Dens.  0.95Ang From N2              3.90 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k 
;
PROBLEM: Check Calcd Resid. Dens.  1.09Ang From Pd1            -9.31 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.54Ang From Fe1            -5.64 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k_3 
;
PROBLEM: Check Calcd Resid. Dens.  0.71Ang From Pd1            -5.62 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k_4 
;
PROBLEM: Check Calcd Resid. Dens.  0.56Ang From Fe2            -4.53 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k_5 
;
PROBLEM: Check Calcd Resid. Dens.  0.60Ang From Pd1            -4.11 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT973_rt569_ohpympdmeoh_195k 
;
PROBLEM: Check Calcd Positive Resid. Density on       Fe2       5.02 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT975_rt569_ohpympdmeoh_195k 
;
PROBLEM: Check Calcd Resid. Dens.  0.55Ang From C11     .       2.25 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_DIFMN02_rt569_ohpympdmeoh_195k 
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00
RESPONSE: This alerts may arise from the strong disorder of the guest in the structural pores as well as from the deterioration of the crystal during the desorption/adsorption events
;
_vrf_PLAT082_rt569_ohpympdmeoh_195k 
;
PROBLEM: High R1 Value ..................................       0.16 Report
RESPONSE: This alerts may arise from the strong disorder of the guest in the structural pores as well as from the deterioration of the crystal during the desorption/adsorption events
;
_vrf_PLAT097_rt569_ohpympdmeoh_195k 
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       6.06 eA-3
RESPONSE: This alerts may arise from the strong disorder of the guest in the structural pores as well as from the deterioration of the crystal during the desorption/adsorption events
;
_vrf_PLAT098_rt569_ohpympdmeoh_195k 
;
PROBLEM: Large Reported Min.  (Negative) Residual Density      -7.73 eA-3
RESPONSE: This alerts may arise from the strong disorder of the guest in the structural pores as well as from the deterioration of the crystal during the desorption/adsorption events
;
_vrf_PLAT250_rt569_ohpympdmeoh_195k 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        6.1 Note
RESPONSE: This alerts may arise from the strong disorder of the guest in the structural pores as well as from the deterioration of the crystal during the desorption/adsorption events
;
_vrf_PLAT342_rt569_ohpympdmeoh_195k 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.07 Ang.
RESPONSE: This alerts may arise from the strong disorder of the guest in the structural pores as well as from the deterioration of the crystal during the desorption/adsorption events
;
_vrf_PLAT430_rt569_ohpympdmeoh_195k 
;
PROBLEM: Short Inter D...A Contact  O2       ..O3       .       2.75 Ang.
RESPONSE: There is a certain number of H-bonds which are properly discussed in the paper. This alert arises from the absence of H atoms which are not present due to the strong agitation of the molecular moieties involved in the H-bond interactions
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_8 
;
PROBLEM: Check Calcd Resid. Dens.  0.83Ang From C8              3.28 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_9 
;
PROBLEM: Check Calcd Resid. Dens.  1.11Ang From N6              3.27 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_10 
;
PROBLEM: Check Calcd Resid. Dens.  0.87Ang From N5              3.25 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_11 
;
PROBLEM: Check Calcd Resid. Dens.  0.07Ang From C7              3.22 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_12 
;
PROBLEM: Check Calcd Resid. Dens.  1.23Ang From C3              3.01 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_13 
;
PROBLEM: Check Calcd Resid. Dens.  0.86Ang From C3              2.99 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_14 
;
PROBLEM: Check Calcd Resid. Dens.  1.18Ang From N1              2.90 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_15 
;
PROBLEM: Check Calcd Resid. Dens.  1.79Ang From Pd1             2.86 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_16 
;
PROBLEM: Check Calcd Resid. Dens.  0.78Ang From O3              2.79 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_17 
;
PROBLEM: Check Calcd Resid. Dens.  0.78Ang From C10             2.74 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_18 
;
PROBLEM: Check Calcd Resid. Dens.  2.02Ang From C9              2.70 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_195k_19 
;
PROBLEM: Check Calcd Resid. Dens.  0.13Ang From N1              2.64 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N1 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k_6 
;
PROBLEM: Check Calcd Resid. Dens.  0.19Ang From O2             -3.40 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k_7 
;
PROBLEM: Check Calcd Resid. Dens.  1.34Ang From N2             -3.16 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k_8 
;
PROBLEM: Check Calcd Resid. Dens.  0.38Ang From O1             -3.14 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k_9 
;
PROBLEM: Check Calcd Resid. Dens.  0.16Ang From O1             -3.09 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k_10 
;
PROBLEM: Check Calcd Resid. Dens.  0.92Ang From C1             -2.72 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k_11 
;
PROBLEM: Check Calcd Resid. Dens.  0.53Ang From C1             -2.59 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_195k_12 
;
PROBLEM: Check Calcd Resid. Dens.  1.33Ang From O3             -2.53 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT975_rt569_ohpympdmeoh_195k_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.66Ang From O2      .       1.98 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT977_rt569_ohpympdmeoh_195k 
;
PROBLEM: Check Negative Difference Density on H1        .      -1.55 eA-3
RESPONSE: This alerts may arise from the strong disorder of the guest in the structural pores as well as from the deterioration of the crystal during the desorption/adsorption events
;
# Added during the CSD deposition process: Tuesday 27 September 2022 04:39 PM
# end Validation Reply Form

_audit_creation_date             2022-09-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 Fe N8 O2 Pd, 0.25(C2 O2)'
_chemical_formula_sum            'C12.50 H6 Fe N8 O2.50 Pd'
_chemical_formula_weight         470.50
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.3476(12)
_cell_length_b                   7.3127(2)
_cell_length_c                   15.6544(9)
_cell_angle_alpha                90
_cell_angle_beta                 137.120(11)
_cell_angle_gamma                90
_cell_volume                     1662.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5037
_cell_measurement_temperature    195.10(14)
_cell_measurement_theta_max      27.1500
_cell_measurement_theta_min      3.0630
_shelx_estimated_absorpt_T_max   0.943
_shelx_estimated_absorpt_T_min   0.637
_exptl_absorpt_coefficient_mu    1.981
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8642
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.832
_diffrn_reflns_theta_min         3.075
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      195.10(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  42.00   1.00    2.50    --   17.15  77.00  90.00   56
  2  ω    -14.00  42.00   1.00    2.50    --   17.15  77.00 150.00   56
  3  ω    -14.00  42.00   1.00    2.50    --   17.15  77.00  60.00   56
  4  ω    -19.00  30.00   1.00    2.50    --   17.15  87.00 -97.00   49
  5  ω    -42.00  49.00   1.00    2.50    --   17.15 -77.00 -60.00   91
  6  ω    -95.00 -37.00   1.00    2.50    --  -16.21 178.00   0.00   58
  7  ω    -94.00 -39.00   1.00    2.50    --  -16.21-178.00  90.00   55
  8  ω    -55.00   8.00   1.00    2.50    --   17.15 -38.00 -30.00   63
  9  ω     -4.00  86.00   1.00    2.50    --   17.15  57.00 -60.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0248423000
_diffrn_orient_matrix_UB_12      -0.0795350000
_diffrn_orient_matrix_UB_13      -0.0129427000
_diffrn_orient_matrix_UB_21      0.0057444000
_diffrn_orient_matrix_UB_22      -0.0357692000
_diffrn_orient_matrix_UB_23      -0.0360458000
_diffrn_orient_matrix_UB_31      0.0416359000
_diffrn_orient_matrix_UB_32      -0.0425020000
_diffrn_orient_matrix_UB_33      0.0544692000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1888
_reflns_number_total             1935
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         6.061
_refine_diff_density_min         -7.728
_refine_diff_density_rms         0.508
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.298
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         1935
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1594
_refine_ls_R_factor_gt           0.1574
_refine_ls_restrained_S_all      1.298
_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)+(0.0001P)²+408.6588P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3502
_refine_ls_wR_factor_ref         0.3511
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(N2) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(N1)
Uanis(Fe2) = Uanis(N4) = Uanis(C6) = Uanis(Pd1) = Uanis(C5) = Uanis(N3) =
Uanis(Fe1)
Uanis(N5) = Uanis(C7) = Uanis(C8) = Uanis(O2) = Uanis(C9) = Uanis(N6) =
Uanis(C10) = Uanis(C1) = Uanis(N1) = Uanis(C4) = Uanis(C3) = Uanis(O1) =
Uanis(C2) = Uanis(N2)
3. Others
 Fixed Sof: O3(0.25) C11(0.25)
 Fixed X: O3(0.751221) C11(0.75004)
 Fixed Y: O3(1) C11(0.811371)
 Fixed Z: O3(-0.017511) C11(-0.020741)
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C1(H1), C4(H4), C9(H9), C2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.75684(14) 0.500000 0.2400(2) 0.0135(5) Uani 1 2 d S T P . .
Fe2 Fe 1.000000 1.000000 0.500000 0.0135(5) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.000000 0.000000 0.0135(5) Uani 1 4 d S T P . .
N4 N 0.9061(10) 0.808(2) 0.3898(14) 0.0135(5) Uani 1 1 d . . . . .
N3 N 0.6025(10) 0.200(2) 0.0948(13) 0.0135(5) Uani 1 1 d . . . . .
N5 N 1.0306(17) 1.000000 0.402(2) 0.038(2) Uani 1 2 d S T P . .
C6 C 0.8524(12) 0.694(2) 0.3331(16) 0.0135(5) Uani 1 1 d . . . . .
C5 C 0.6592(12) 0.309(2) 0.1476(16) 0.0135(5) Uani 1 1 d . . . . .
O1 O 0.3177(14) 0.000000 -0.493(2) 0.038(2) Uani 1 2 d S T P . .
N1 N 0.4857(17) 0.000000 -0.152(2) 0.038(2) Uani 1 2 d S T P . .
O2 O 0.9281(14) 1.000000 0.097(2) 0.038(2) Uani 1 2 d S T P . .
C10 C 1.117(2) 1.000000 0.464(3) 0.038(2) Uani 1 2 d S T P . .
H10 H 1.162807 1.000000 0.552831 0.046 Uiso 1 2 calc R U P . .
C3 C 0.394(2) 0.000000 -0.376(3) 0.038(2) Uani 1 2 d S T P . .
N6 N 1.1460(17) 1.000000 0.410(2) 0.038(2) Uani 1 2 d S T P . .
C7 C 0.964(2) 1.000000 0.280(3) 0.038(2) Uani 1 2 d S T P . .
H7 H 0.901000 1.000000 0.232901 0.046 Uiso 1 2 calc R U P . .
N2 N 0.5528(17) 0.000000 -0.226(2) 0.038(2) Uani 1 2 d S T P . .
C1 C 0.563(2) 0.000000 -0.125(3) 0.038(2) Uani 1 2 d S T P . .
H1 H 0.623073 0.000000 -0.040749 0.046 Uiso 1 2 calc R U P . .
C4 C 0.402(2) 0.000000 -0.275(3) 0.038(2) Uani 1 2 d S T P . .
H4 H 0.347556 0.000000 -0.295564 0.046 Uiso 1 2 calc R U P . .
C8 C 0.993(2) 1.000000 0.222(3) 0.038(2) Uani 1 2 d S T P . .
C9 C 1.088(2) 1.000000 0.298(3) 0.038(2) Uani 1 2 d S T P . .
H9 H 1.107194 1.000000 0.259036 0.046 Uiso 1 2 calc R U P . .
C2 C 0.473(2) 0.000000 -0.345(3) 0.038(2) Uani 1 2 d S T P . .
H2 H 0.470536 0.000000 -0.408064 0.046 Uiso 1 2 calc R U P . .
O3 O 0.751221 1.000000 -0.017511 0.045(13) Uiso 0.25 1 d S . P A -1
C11 C 0.750040 0.811371 -0.020741 0.05(3) Uiso 0.25 1 d . . P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0130(8) 0.0070(8) 0.0174(8) 0.000 0.0102(7) 0.000
Fe2 0.0130(8) 0.0070(8) 0.0174(8) 0.000 0.0102(7) 0.000
Fe1 0.0130(8) 0.0070(8) 0.0174(8) 0.000 0.0102(7) 0.000
N4 0.0130(8) 0.0070(8) 0.0174(8) 0.000 0.0102(7) 0.000
N3 0.0130(8) 0.0070(8) 0.0174(8) 0.000 0.0102(7) 0.000
N5 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
C6 0.0130(8) 0.0070(8) 0.0174(8) 0.000 0.0102(7) 0.000
C5 0.0130(8) 0.0070(8) 0.0174(8) 0.000 0.0102(7) 0.000
O1 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
N1 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
O2 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
C10 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
C3 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
N6 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
C7 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
N2 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
C1 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
C4 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
C8 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
C9 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000
C2 0.011(3) 0.044(5) 0.016(4) 0.000 -0.004(3) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C6 1.987(17) 6_565 ?
Pd1 C6 1.987(17) . ?
Pd1 C5 1.994(17) . ?
Pd1 C5 1.994(17) 6_565 ?
Fe2 N4 1.973(15) . ?
Fe2 N4 1.973(15) 5_776 ?
Fe2 N4 1.973(14) 2_756 ?
Fe2 N4 1.973(14) 6_575 ?
Fe2 N5 2.05(3) 5_776 ?
Fe2 N5 2.05(3) . ?
Fe1 N3 2.091(14) 5_655 ?
Fe1 N3 2.091(14) . ?
Fe1 N3 2.091(14) 2_655 ?
Fe1 N3 2.091(14) 6 ?
Fe1 N1 2.17(3) . ?
Fe1 N1 2.17(3) 5_655 ?
N4 C6 1.14(2) . ?
N3 C5 1.14(2) . ?
N5 C10 1.31(4) . ?
N5 C7 1.31(4) . ?
O1 C3 1.28(4) . ?
N1 C1 1.38(4) . ?
N1 C4 1.36(4) . ?
O2 C8 1.33(4) . ?
C10 H10 0.9500 . ?
C10 N6 1.36(5) . ?
C3 C4 1.47(5) . ?
C3 C2 1.37(5) . ?
N6 C9 1.19(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.43(5) . ?
N2 C1 1.41(5) . ?
N2 C2 1.31(4) . ?
C1 H1 0.9500 . ?
C4 H4 0.9500 . ?
C8 C9 1.42(4) . ?
C9 H9 0.9500 . ?
C2 H2 0.9500 . ?
O3 C11 1.37987(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
C6 Pd1 C6 91.3(10) 6_565 . ?
C6 Pd1 C5 178.4(7) . . ?
C6 Pd1 C5 89.8(6) 6_565 . ?
C6 Pd1 C5 89.8(6) . 6_565 ?
C6 Pd1 C5 178.4(7) 6_565 6_565 ?
C5 Pd1 C5 89.1(10) . 6_565 ?
N4 Fe2 N4 89.4(8) 5_776 6_575 ?
N4 Fe2 N4 180.0 5_776 . ?
N4 Fe2 N4 180.0 6_575 2_756 ?
N4 Fe2 N4 89.4(8) 2_756 . ?
N4 Fe2 N4 90.6(8) 6_575 . ?
N4 Fe2 N4 90.6(8) 5_776 2_756 ?
N4 Fe2 N5 88.7(6) 5_776 . ?
N4 Fe2 N5 91.3(6) 2_756 5_776 ?
N4 Fe2 N5 88.7(6) 6_575 5_776 ?
N4 Fe2 N5 91.3(6) 5_776 5_776 ?
N4 Fe2 N5 91.3(6) . . ?
N4 Fe2 N5 88.7(6) . 5_776 ?
N4 Fe2 N5 91.3(6) 6_575 . ?
N4 Fe2 N5 88.7(6) 2_756 . ?
N5 Fe2 N5 180.0 . 5_776 ?
N3 Fe1 N3 88.9(8) 6 . ?
N3 Fe1 N3 91.1(8) 5_655 6 ?
N3 Fe1 N3 180.0 5_655 . ?
N3 Fe1 N3 88.9(8) 5_655 2_655 ?
N3 Fe1 N3 180.0(10) 6 2_655 ?
N3 Fe1 N3 91.1(8) 2_655 . ?
N3 Fe1 N1 90.7(6) 5_655 5_655 ?
N3 Fe1 N1 90.7(6) 6 . ?
N3 Fe1 N1 89.3(6) . 5_655 ?
N3 Fe1 N1 89.3(6) 5_655 . ?
N3 Fe1 N1 90.7(6) 2_655 5_655 ?
N3 Fe1 N1 89.3(6) 2_655 . ?
N3 Fe1 N1 89.3(6) 6 5_655 ?
N3 Fe1 N1 90.7(6) . . ?
N1 Fe1 N1 180.0 5_655 . ?
C6 N4 Fe2 174.8(14) . . ?
C5 N3 Fe1 179.3(18) . . ?
C10 N5 Fe2 120(2) . . ?
C7 N5 Fe2 120(2) . . ?
C7 N5 C10 120(3) . . ?
N4 C6 Pd1 176.3(15) . . ?
N3 C5 Pd1 179.0(15) . . ?
C1 N1 Fe1 120(2) . . ?
C4 N1 Fe1 122(3) . . ?
C4 N1 C1 118(3) . . ?
N5 C10 H10 117.3 . . ?
N5 C10 N6 125(3) . . ?
N6 C10 H10 117.3 . . ?
O1 C3 C4 124(3) . . ?
O1 C3 C2 117(3) . . ?
C2 C3 C4 118(3) . . ?
C9 N6 C10 117(3) . . ?
N5 C7 H7 122.4 . . ?
N5 C7 C8 115(3) . . ?
C8 C7 H7 122.4 . . ?
C2 N2 C1 125(3) . . ?
N1 C1 N2 119(3) . . ?
N1 C1 H1 120.6 . . ?
N2 C1 H1 120.6 . . ?
N1 C4 C3 121(3) . . ?
N1 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
O2 C8 C7 118(3) . . ?
O2 C8 C9 123(4) . . ?
C9 C8 C7 119(3) . . ?
N6 C9 C8 123(4) . . ?
N6 C9 H9 118.7 . . ?
C8 C9 H9 118.7 . . ?
C3 C2 H2 120.6 . . ?
N2 C2 C3 119(4) . . ?
N2 C2 H2 120.6 . . ?

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
Fe2 N5 C10 N6 180.000(9) . . . . ?
Fe2 N5 C7 C8 180.000(7) . . . . ?
Fe1 N1 C1 N2 180.000(4) . . . . ?
Fe1 N1 C4 C3 180.000(7) . . . . ?
N5 C10 N6 C9 0.000(10) . . . . ?
N5 C7 C8 O2 180.000(8) . . . . ?
N5 C7 C8 C9 0.000(10) . . . . ?
O1 C3 C4 N1 180.000(11) . . . . ?
O1 C3 C2 N2 180.000(11) . . . . ?
O2 C8 C9 N6 180.000(5) . . . . ?
C10 N5 C7 C8 0.000(10) . . . . ?
C10 N6 C9 C8 0.000(13) . . . . ?
C7 N5 C10 N6 0.000(15) . . . . ?
C7 C8 C9 N6 0.000(11) . . . . ?
C1 N1 C4 C3 0.000(7) . . . . ?
C1 N2 C2 C3 0.000(10) . . . . ?
C4 N1 C1 N2 0.000(6) . . . . ?
C4 C3 C2 N2 0.000(11) . . . . ?
C2 C3 C4 N1 0.000(10) . . . . ?
C2 N2 C1 N1 0.000(7) . . . . ?

_shelx_res_file                  
;
TITL rt569_ohpympdmeoh_195k_a.res in C2/m
    rt569_ohpympdmeoh_195k.res
    created by SHELXL-2018/3 at 16:05:19 on 27-Sep-2022
REM Old TITL rt569_ohpympdmeoh_195k_a.res in C2/m
REM SHELXT solution in C2/m
REM R1 0.231, Rweak 0.065, Alpha 0.127, Orientation as input
REM Formula found by SHELXT: C10 N16 Pd I
CELL 0.71073 21.3476 7.3127 15.6544 90 137.12 90
ZERR 4 0.0012 0.0002 0.0009 0 0.011 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pd
UNIT 50 24 4 32 10 4
EADP C1 N2 C2 C3 C4 N1
EADP Fe2 N4 C6 Pd1 C5 N3 Fe1
EADP N5 C7 C8 O2 C9 N6 C10 C1 N1 C4 C3 O1 C2 N2

L.S. 10
PLAN  15
SIZE 0.25 0.2 0.03
TEMP -78.13
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\RT569_OHPymPdMeOH_195K.hkl">
REM </olex2.extras>

WGHT    0.000100  408.658783
FVAR       0.23101
PD1   6    0.756835    0.500000    0.240002    10.50000    0.01301    0.00703 =
         0.01742    0.00000    0.01018    0.00000
FE2   3    1.000000    1.000000    0.500000    10.25000    0.01301    0.00703 =
         0.01742    0.00000    0.01018    0.00000
FE1   3    0.500000    0.000000    0.000000    10.25000    0.01301    0.00703 =
         0.01742    0.00000    0.01018    0.00000
N4    4    0.906111    0.808231    0.389768    11.00000    0.01301    0.00703 =
         0.01742    0.00000    0.01018    0.00000
N3    4    0.602452    0.200264    0.094782    11.00000    0.01301    0.00703 =
         0.01742    0.00000    0.01018    0.00000
N5    4    1.030554    1.000000    0.402423    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
C6    1    0.852385    0.694296    0.333059    11.00000    0.01301    0.00703 =
         0.01742    0.00000    0.01018    0.00000
C5    1    0.659169    0.308624    0.147550    11.00000    0.01301    0.00703 =
         0.01742    0.00000    0.01018    0.00000
O1    5    0.317711    0.000000   -0.493325    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
N1    4    0.485659    0.000000   -0.152194    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
O2    5    0.928120    1.000000    0.097262    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
C10   1    1.116895    1.000000    0.463735    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
AFIX  43
H10   2    1.162807    1.000000    0.552831    10.50000   -1.20000
AFIX   0
C3    1    0.393965    0.000000   -0.376391    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
N6    4    1.146047    1.000000    0.410233    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
C7    1    0.964077    1.000000    0.279904    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
AFIX  43
H7    2    0.901000    1.000000    0.232901    10.50000   -1.20000
AFIX   0
N2    4    0.552775    0.000000   -0.225615    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
C1    1    0.563456    0.000000   -0.125271    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
AFIX  43
H1    2    0.623073    0.000000   -0.040749    10.50000   -1.20000
AFIX   0
C4    1    0.401857    0.000000   -0.275123    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
AFIX  43
H4    2    0.347556    0.000000   -0.295564    10.50000   -1.20000
AFIX   0
C8    1    0.992925    1.000000    0.221673    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
C9    1    1.088367    1.000000    0.298339    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
AFIX  43
H9    2    1.107194    1.000000    0.259036    10.50000   -1.20000
AFIX   0
C2    1    0.473200    0.000000   -0.344767    10.50000    0.01054    0.04397 =
         0.01611    0.00000   -0.00410    0.00000
AFIX  43
H2    2    0.470536    0.000000   -0.408064    10.50000   -1.20000
AFIX   0

PART -1
O3    5   10.751221   11.000000    9.982489    10.25000    0.04466
C11   1   10.750040   10.811371    9.979259    10.25000    0.04919
HKLF 4




REM  rt569_ohpympdmeoh_195k_a.res in C2/m
REM wR2 = 0.3511, GooF = S = 1.298, Restrained GooF = 1.298 for all data
REM R1 = 0.1574 for 1888 Fo > 4sig(Fo) and 0.1594 for all 1935 data
REM 53 parameters refined using 0 restraints

END

WGHT      0.0001    408.7210

REM Highest difference peak  6.061,  deepest hole -7.728,  1-sigma level  0.508
Q1    1   0.7113  0.5000  0.2009  10.50000  0.05    6.06
Q2    1   0.7751  0.5000  0.3311  10.50000  0.05    5.93
Q3    1   0.7791  0.5000  0.2298  10.50000  0.05    4.61
Q4    1   0.5693  0.0000 -0.2688  10.50000  0.05    3.93
Q5    1   0.5152  0.0000 -0.1816  10.50000  0.05    3.70
Q6    1   0.6909  0.5000  0.2391  10.50000  0.05    3.60
Q7    1   0.3247  0.0000 -0.4028  10.50000  0.05    3.15
Q8    1   1.0130  1.0000  0.1891  10.50000  0.05    2.96
Q9    1   1.1646  1.0000  0.3619  10.50000  0.05    2.91
Q10   1   0.4436  0.0000 -0.3036  10.50000  0.05    2.61
Q11   1   0.9249  1.0000  0.1613  10.50000  0.05    2.50
Q12   1   1.0242  1.0000  0.4522  10.50000  0.05    2.44
Q13   1   0.7003  1.0000 -0.0794  10.50000  0.05    2.34
Q14   1   0.5274  0.0000 -0.0531  10.50000  0.05    2.29
Q15   1   0.7500  0.7500  0.0000  10.50000  0.05    2.08
;
_shelx_res_checksum              72082
_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 1.303
_oxdiff_exptl_absorpt_empirical_full_min 0.781
####################################################################### 
# 
# 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_rt569_ohpympdmeoh_225k
_database_code_depnum_ccdc_archive 'CCDC 2209626'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-27 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_rt569_ohpympdmeoh_225k 
;
PROBLEM: Check Calcd Resid. Dens.  1.04Ang From Pd1            -3.93 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_225k_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.73Ang From Pd1            -3.73 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT342_rt569_ohpympdmeoh_225k 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.055 Ang.
RESPONSE: This alerts arises from the strong disorder of the guest in the structural pores and from the deterioration of the crystal due to the desorption/readsorption processes
;
_vrf_PLAT420_rt569_ohpympdmeoh_225k 
;
PROBLEM: D-H Bond Without Acceptor  O2       --H2       .     Please Check
RESPONSE: There is a certain number of H-bonds which are properly discussed in the paper. This alert arises from the absence of H atoms which are not present due to the strong agitation of the molecular moieties involved in the H-bond interactions
;
_vrf_PLAT430_rt569_ohpympdmeoh_225k 
;
PROBLEM: Short Inter D...A Contact  N2       ..O3       .       2.86 Ang.
RESPONSE: There is a certain number of H-bonds which are properly discussed in the paper. This alert arises from the absence of H atoms which are not present due to the strong agitation of the molecular moieties involved in the H-bond interactions
;
_vrf_PLAT721_rt569_ohpympdmeoh_225k 
;
PROBLEM: Bond    Calc     0.83000, Rep      0.8(4) Dev...       0.03 Ang.
RESPONSE: This alert refers to the H linked to the O of the hydroxy group
;
_vrf_PLAT971_rt569_ohpympdmeoh_225k 
;
PROBLEM: Check Calcd Resid. Dens.  0.76Ang From Pd1             3.47 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_225k_2 
;
PROBLEM: Check Calcd Resid. Dens.  1.37Ang From Pd1             3.35 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_225k_3 
;
PROBLEM: Check Calcd Resid. Dens.  0.12Ang From N5              3.16 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_225k_4 
;
PROBLEM: Check Calcd Resid. Dens.  0.96Ang From N2              3.14 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_225k_5 
;
PROBLEM: Check Calcd Resid. Dens.  1.08Ang From C9              2.87 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_225k_6 
;
PROBLEM: Check Calcd Resid. Dens.  0.05Ang From N1              2.86 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_225k_7 
;
PROBLEM: Check Calcd Resid. Dens.  0.96Ang From N5              2.80 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_225k_8 
;
PROBLEM: Check Calcd Resid. Dens.  0.68Ang From C1              2.60 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_225k_9 
;
PROBLEM: Check Calcd Resid. Dens.  0.74Ang From Pd1             2.59 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_225k_3 
;
PROBLEM: Check Calcd Resid. Dens.  0.16Ang From O2             -3.36 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O2 atom resulting from the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Tuesday 27 September 2022 04:39 PM
# end Validation Reply Form

_audit_creation_date             2022-09-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H7 Fe N8 O2 Pd, 0.25(C2 O2)'
_chemical_formula_sum            'C12.50 H7 Fe N8 O2.50 Pd'
_chemical_formula_weight         471.51
_chemical_melting_point          ?
_chemical_oxdiff_formula         FePdCN
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'

_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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.386(4)
_cell_length_b                   7.3624(4)
_cell_length_c                   14.569(3)
_cell_angle_alpha                90
_cell_angle_beta                 132.54(3)
_cell_angle_gamma                90
_cell_volume                     1690.1(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3734
_cell_measurement_temperature    225.00(10)
_cell_measurement_theta_max      27.6070
_cell_measurement_theta_min      3.7730
_shelx_estimated_absorpt_T_max   0.944
_shelx_estimated_absorpt_T_min   0.641
_exptl_absorpt_coefficient_mu    1.949
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8707
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.866
_diffrn_reflns_theta_min         3.054
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      225.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  20.00   1.00    2.50    --  -16.21 -87.00-110.00   50
  2  ω    -56.00  91.00   1.00    2.50    --   17.15   0.00 -90.00  147
  3  ω    -14.00  42.00   1.00    2.50    --   17.15  77.00 150.00   56
  4  ω    -42.00  15.00   1.00    2.50    --  -16.21 -77.00   0.00   57
  5  ω    -53.00  31.00   1.00    2.50    --  -16.21  87.00 -97.00   84
  6  ω    -52.00  25.00   1.00    2.50    --   17.15 -57.00  60.00   77
  7  ω    -52.00  39.00   1.00    2.50    --   17.15 -57.00 150.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0115440000
_diffrn_orient_matrix_UB_12      -0.0793415000
_diffrn_orient_matrix_UB_13      0.0361021000
_diffrn_orient_matrix_UB_21      -0.0416518000
_diffrn_orient_matrix_UB_22      -0.0347561000
_diffrn_orient_matrix_UB_23      -0.0471395000
_diffrn_orient_matrix_UB_31      0.0125586000
_diffrn_orient_matrix_UB_32      -0.0422356000
_diffrn_orient_matrix_UB_33      -0.0291130000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1813
_reflns_number_total             1914
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         3.195
_refine_diff_density_min         -3.269
_refine_diff_density_rms         0.343
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.304
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1914
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.1132
_refine_ls_restrained_S_all      1.304
_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)+(0.0001P)²+192.1881P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2629
_refine_ls_wR_factor_ref         0.2652
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4) = Uanis(C3) = Uanis(O1) = Uanis(C2) = Uanis(N2) = Uanis(C1) =
Uanis(N1)
Uanis(C7) = Uanis(N5) = Uanis(C10) = Uanis(N6) = Uanis(C9) = Uanis(C8) =
Uanis(O2)
3. Others
 Fixed Sof: H2(0.5) O3(0.25) C11(0.25)
 Fixed X: O3(0.728201) C11(0.74235)
 Fixed Y: O3(0.5) C11(0.310281)
 Fixed Z: O3(0.479029) C11(0.497419)
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C7(H7), C4(H4), C1(H1), C2(H2A)
4.b Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.51637(10) 0.500000 0.27123(14) 0.0200(4) Uani 1 2 d S T P . .
Fe2 Fe 0.500000 1.000000 0.500000 0.0129(7) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.000000 0.000000 0.0183(8) Uani 1 4 d S T P . .
N5 N 0.6291(16) 1.000000 0.662(2) 0.048(2) Uani 1 2 d S T P . .
N4 N 0.5183(8) 0.8051(16) 0.4228(11) 0.024(2) Uani 1 1 d . . . . .
C6 C 0.5194(8) 0.6923(17) 0.3702(12) 0.019(3) Uani 1 1 d . . . . .
N3 N 0.5072(10) 0.1998(18) 0.1092(12) 0.041(4) Uani 1 1 d . . . . .
O1 O 0.8120(14) 0.000000 0.127(2) 0.056(3) Uani 1 2 d S T P . .
N1 N 0.6381(17) 0.000000 0.121(3) 0.056(3) Uani 1 2 d S T P . .
C5 C 0.5098(11) 0.309(2) 0.1676(14) 0.037(4) Uani 1 1 d . . . . .
C10 C 0.654(2) 1.000000 0.773(3) 0.048(2) Uani 1 2 d S T P . .
H10 H 0.612540 1.000000 0.777253 0.058 Uiso 1 2 calc R U P . .
N6 N 0.7380(16) 1.000000 0.883(2) 0.048(2) Uani 1 2 d S T P . .
O2 O 0.8318(13) 1.000000 0.7585(19) 0.048(2) Uani 1 2 d S T P . .
H2 H 0.873351 1.061434 0.815961 0.072 Uiso 0.5 1 calc R U P . .
C3 C 0.769(2) 0.000000 0.164(3) 0.056(3) Uani 1 2 d S T P . .
C9 C 0.790(2) 1.000000 0.880(3) 0.048(2) Uani 1 2 d S T P . .
H9 H 0.846676 1.000000 0.956872 0.058 Uiso 1 2 calc R U P . .
O3 O 0.728201 0.500000 0.479029 0.051(10) Uiso 0.25 1 d S . P A -1
N2 N 0.7772(17) 0.000000 0.330(3) 0.056(3) Uani 1 2 d S T P . .
C7 C 0.6863(19) 1.000000 0.650(3) 0.048(2) Uani 1 2 d S T P . .
H7 H 0.670371 1.000000 0.572084 0.058 Uiso 1 2 calc R U P . .
C4 C 0.677(2) 0.000000 0.076(3) 0.056(3) Uani 1 2 d S T P . .
H4 H 0.645228 0.000000 -0.010272 0.067 Uiso 1 2 calc R U P . .
C8 C 0.775(2) 1.000000 0.767(3) 0.048(2) Uani 1 2 d S T P . .
C1 C 0.691(2) 0.000000 0.245(3) 0.056(3) Uani 1 2 d S T P . .
H1 H 0.665422 0.000000 0.277477 0.067 Uiso 1 2 calc R U P . .
C2 C 0.814(2) 0.000000 0.286(3) 0.056(3) Uani 1 2 d S T P . .
H2A H 0.873295 0.000000 0.342023 0.067 Uiso 1 2 calc R U P . .
C11 C 0.742350 0.310281 0.497419 0.038(15) Uiso 0.25 1 d . . P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0264(8) 0.0098(7) 0.0271(8) 0.000 0.0193(7) 0.000
Fe2 0.0273(18) 0.0081(15) 0.0082(14) 0.000 0.0140(15) 0.000
Fe1 0.0254(19) 0.0097(16) 0.0108(16) 0.000 0.0086(15) 0.000
N5 0.070(6) 0.047(5) 0.064(6) 0.000 0.060(5) 0.000
N4 0.044(7) 0.020(6) 0.035(6) 0.002(5) 0.038(6) 0.001(5)
C6 0.033(7) 0.013(6) 0.031(7) 0.000(5) 0.030(6) 0.002(5)
N3 0.059(9) 0.016(6) 0.031(7) -0.004(6) 0.024(7) -0.004(6)
O1 0.070(6) 0.054(6) 0.073(7) 0.000 0.061(6) 0.000
N1 0.070(6) 0.054(6) 0.073(7) 0.000 0.061(6) 0.000
C5 0.045(9) 0.018(7) 0.030(8) 0.006(6) 0.019(7) -0.002(7)
C10 0.070(6) 0.047(5) 0.064(6) 0.000 0.060(5) 0.000
N6 0.070(6) 0.047(5) 0.064(6) 0.000 0.060(5) 0.000
O2 0.070(6) 0.047(5) 0.064(6) 0.000 0.060(5) 0.000
C3 0.070(6) 0.054(6) 0.073(7) 0.000 0.061(6) 0.000
C9 0.070(6) 0.047(5) 0.064(6) 0.000 0.060(5) 0.000
N2 0.070(6) 0.054(6) 0.073(7) 0.000 0.061(6) 0.000
C7 0.070(6) 0.047(5) 0.064(6) 0.000 0.060(5) 0.000
C4 0.070(6) 0.054(6) 0.073(7) 0.000 0.061(6) 0.000
C8 0.070(6) 0.047(5) 0.064(6) 0.000 0.060(5) 0.000
C1 0.070(6) 0.054(6) 0.073(7) 0.000 0.061(6) 0.000
C2 0.070(6) 0.054(6) 0.073(7) 0.000 0.061(6) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C6 1.991(12) 6_565 ?
Pd1 C6 1.991(12) . ?
Pd1 C5 1.996(18) . ?
Pd1 C5 1.996(18) 6_565 ?
Fe2 N5 2.09(3) . ?
Fe2 N5 2.09(3) 5_676 ?
Fe2 N4 2.018(11) 6_575 ?
Fe2 N4 2.018(11) 2_656 ?
Fe2 N4 2.018(11) 5_676 ?
Fe2 N4 2.018(11) . ?
Fe1 N3 2.095(14) 5_655 ?
Fe1 N3 2.095(14) 6 ?
Fe1 N3 2.095(14) 2_655 ?
Fe1 N3 2.095(14) . ?
Fe1 N1 2.19(3) . ?
Fe1 N1 2.19(3) 5_655 ?
N5 C10 1.31(3) . ?
N5 C7 1.35(3) . ?
N4 C6 1.141(17) . ?
N3 C5 1.15(2) . ?
O1 C3 1.34(3) . ?
N1 C4 1.37(3) . ?
N1 C1 1.33(4) . ?
C10 H10 0.9400 . ?
C10 N6 1.38(4) . ?
N6 C9 1.14(3) . ?
O2 H2 0.8(4) 6_575 ?
O2 H2 0.8300 . ?
O2 C8 1.31(3) . ?
C3 C4 1.44(4) . ?
C3 C2 1.33(4) . ?
C9 H9 0.9400 . ?
C9 C8 1.45(4) . ?
O3 C11 1.41588(8) . ?
N2 C1 1.36(4) . ?
N2 C2 1.30(3) . ?
C7 H7 0.9400 . ?
C7 C8 1.46(4) . ?
C4 H4 0.9400 . ?
C1 H1 0.9400 . ?
C2 H2A 0.9400 . ?

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
C6 Pd1 C6 90.7(7) 6_565 . ?
C6 Pd1 C5 89.9(6) 6_565 . ?
C6 Pd1 C5 178.3(6) . . ?
C6 Pd1 C5 178.3(6) 6_565 6_565 ?
C6 Pd1 C5 89.9(6) . 6_565 ?
C5 Pd1 C5 89.4(9) . 6_565 ?
N5 Fe2 N5 180.0 5_676 . ?
N4 Fe2 N5 91.4(5) 5_676 5_676 ?
N4 Fe2 N5 91.4(5) 2_656 5_676 ?
N4 Fe2 N5 88.6(5) 5_676 . ?
N4 Fe2 N5 91.4(5) 6_575 . ?
N4 Fe2 N5 88.6(5) . 5_676 ?
N4 Fe2 N5 88.6(5) 6_575 5_676 ?
N4 Fe2 N5 88.6(5) 2_656 . ?
N4 Fe2 N5 91.4(5) . . ?
N4 Fe2 N4 89.3(6) . 2_656 ?
N4 Fe2 N4 90.7(6) . 6_575 ?
N4 Fe2 N4 180.0 6_575 2_656 ?
N4 Fe2 N4 89.3(6) 5_676 6_575 ?
N4 Fe2 N4 180.0 . 5_676 ?
N4 Fe2 N4 90.7(6) 5_676 2_656 ?
N3 Fe1 N3 89.2(8) . 6 ?
N3 Fe1 N3 180.0 . 5_655 ?
N3 Fe1 N3 90.8(8) 5_655 6 ?
N3 Fe1 N3 90.8(8) . 2_655 ?
N3 Fe1 N3 180.0(10) 6 2_655 ?
N3 Fe1 N3 89.2(8) 5_655 2_655 ?
N3 Fe1 N1 91.4(6) . . ?
N3 Fe1 N1 88.6(6) 6 5_655 ?
N3 Fe1 N1 91.4(6) 6 . ?
N3 Fe1 N1 88.6(6) 2_655 . ?
N3 Fe1 N1 91.4(6) 2_655 5_655 ?
N3 Fe1 N1 91.4(6) 5_655 5_655 ?
N3 Fe1 N1 88.6(6) . 5_655 ?
N3 Fe1 N1 88.6(6) 5_655 . ?
N1 Fe1 N1 180.0 5_655 . ?
C10 N5 Fe2 121.6(19) . . ?
C10 N5 C7 120(3) . . ?
C7 N5 Fe2 118.1(19) . . ?
C6 N4 Fe2 172.6(12) . . ?
N4 C6 Pd1 177.4(13) . . ?
C5 N3 Fe1 179.0(16) . . ?
C4 N1 Fe1 123(2) . . ?
C1 N1 Fe1 123(2) . . ?
C1 N1 C4 114(3) . . ?
N3 C5 Pd1 179.2(16) . . ?
N5 C10 H10 117.7 . . ?
N5 C10 N6 125(2) . . ?
N6 C10 H10 117.7 . . ?
C9 N6 C10 119(3) . . ?
H2 O2 H2 66.0 . 6_575 ?
C8 O2 H2 109.5 . . ?
C8 O2 H2 109(9) . 6_575 ?
O1 C3 C4 122(3) . . ?
C2 C3 O1 118(3) . . ?
C2 C3 C4 120(3) . . ?
N6 C9 H9 117.8 . . ?
N6 C9 C8 124(3) . . ?
C8 C9 H9 117.8 . . ?
C2 N2 C1 116(3) . . ?
N5 C7 H7 122.6 . . ?
N5 C7 C8 115(2) . . ?
C8 C7 H7 122.6 . . ?
N1 C4 C3 118(3) . . ?
N1 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
O2 C8 C9 127(3) . . ?
O2 C8 C7 116(2) . . ?
C9 C8 C7 117(2) . . ?
N1 C1 N2 129(3) . . ?
N1 C1 H1 115.7 . . ?
N2 C1 H1 115.7 . . ?
C3 C2 H2A 119.2 . . ?
N2 C2 C3 122(3) . . ?
N2 C2 H2A 119.2 . . ?

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
Fe2 N5 C10 N6 180.000(14) . . . . ?
Fe2 N5 C7 C8 180.000(14) . . . . ?
Fe1 N1 C4 C3 180.000(4) . . . . ?
Fe1 N1 C1 N2 180.000(6) . . . . ?
N5 C10 N6 C9 0.00(2) . . . . ?
N5 C7 C8 O2 180.000(14) . . . . ?
N5 C7 C8 C9 0.00(2) . . . . ?
O1 C3 C4 N1 180.000(3) . . . . ?
O1 C3 C2 N2 180.000(6) . . . . ?
C10 N5 C7 C8 0.000(19) . . . . ?
C10 N6 C9 C8 0.000(19) . . . . ?
N6 C9 C8 O2 180.00(2) . . . . ?
N6 C9 C8 C7 0.00(3) . . . . ?
C7 N5 C10 N6 0.00(2) . . . . ?
C4 N1 C1 N2 0.000(7) . . . . ?
C4 C3 C2 N2 0.000(8) . . . . ?
C1 N1 C4 C3 0.000(5) . . . . ?
C1 N2 C2 C3 0.000(10) . . . . ?
C2 C3 C4 N1 0.000(6) . . . . ?
C2 N2 C1 N1 0.000(9) . . . . ?

_shelx_res_file                  
;
TITL rt569_ohpympdmeoh_225k_a.res in C2/m
    rt569_ohpympdmeoh_225k.res
    created by SHELXL-2018/3 at 16:03:46 on 27-Sep-2022
REM Old TITL RT569_OHPymPdMeOH_225K in C2/m
REM SHELXT solution in C2/m
REM R1 0.169, Rweak 0.044, Alpha 0.118, Orientation as input
REM Formula found by SHELXT: C9 N11 Fe Pd
CELL 0.71073 21.3861 7.3624 14.5691 90 132.545 90
ZERR 4 0.0039 0.0004 0.0027 0 0.032 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pd
UNIT 50 28 4 32 10 4
EADP C4 C3 O1 C2 N2 C1 N1
EADP C7 N5 C10 N6 C9 C8 O2

L.S. 10
PLAN  5
SIZE 0.25 0.2 0.03
TEMP -48.13
CONF
LIST 6
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\RT569_OHPymPdMeOH_225K.hkl">
REM </olex2.extras>

WGHT    0.000100  192.188110
FVAR       0.23547
PD1   6    0.516375    0.500000    0.271226    10.50000    0.02636    0.00977 =
         0.02708    0.00000    0.01932    0.00000
FE2   3    0.500000    1.000000    0.500000    10.25000    0.02726    0.00813 =
         0.00825    0.00000    0.01397    0.00000
FE1   3    0.500000    0.000000    0.000000    10.25000    0.02541    0.00965 =
         0.01081    0.00000    0.00860    0.00000
N5    4    0.629061    1.000000    0.662301    10.50000    0.07027    0.04678 =
         0.06371    0.00000    0.05971    0.00000
N4    4    0.518302    0.805056    0.422841    11.00000    0.04386    0.01992 =
         0.03511    0.00240    0.03790    0.00111
C6    1    0.519429    0.692343    0.370225    11.00000    0.03318    0.01334 =
         0.03146   -0.00009    0.03034    0.00217
N3    4    0.507157    0.199831    0.109172    11.00000    0.05904    0.01624 =
         0.03111   -0.00351    0.02410   -0.00393
O1    5    0.811968    0.000000    0.127249    10.50000    0.07023    0.05371 =
         0.07321    0.00000    0.06075    0.00000
N1    4    0.638057    0.000000    0.120712    10.50000    0.07023    0.05371 =
         0.07321    0.00000    0.06075    0.00000
C5    1    0.509844    0.309258    0.167622    11.00000    0.04478    0.01818 =
         0.03033    0.00621    0.01878   -0.00160
C10   1    0.654391    1.000000    0.772810    10.50000    0.07027    0.04678 =
         0.06371    0.00000    0.05971    0.00000
AFIX  43
H10   2    0.612540    1.000000    0.777253    10.50000   -1.20000
AFIX   0
N6    4    0.738015    1.000000    0.883262    10.50000    0.07027    0.04678 =
         0.06371    0.00000    0.05971    0.00000
O2    5    0.831825    1.000000    0.758469    10.50000    0.07027    0.04678 =
         0.06371    0.00000    0.05971    0.00000
AFIX 147
H2    2    0.873351    1.061434    0.815961    10.50000   -1.50000
AFIX   0
C3    1    0.768812    0.000000    0.164017    10.50000    0.07023    0.05371 =
         0.07321    0.00000    0.06075    0.00000
C9    1    0.789996    1.000000    0.880481    10.50000    0.07027    0.04678 =
         0.06371    0.00000    0.05971    0.00000
AFIX  43
H9    2    0.846676    1.000000    0.956872    10.50000   -1.20000
AFIX   0

PART -1
O3    5   10.728201   10.500000   10.479029    10.25000    0.05127

PART 0
N2    4    0.777169    0.000000    0.329920    10.50000    0.07023    0.05371 =
         0.07321    0.00000    0.06075    0.00000
C7    1    0.686311    1.000000    0.650080    10.50000    0.07027    0.04678 =
         0.06371    0.00000    0.05971    0.00000
AFIX  43
H7    2    0.670371    1.000000    0.572084    10.50000   -1.20000
AFIX   0
C4    1    0.677196    0.000000    0.075934    10.50000    0.07023    0.05371 =
         0.07321    0.00000    0.06075    0.00000
AFIX  43
H4    2    0.645228    0.000000   -0.010272    10.50000   -1.20000
AFIX   0
C8    1    0.774676    1.000000    0.767228    10.50000    0.07027    0.04678 =
         0.06371    0.00000    0.05971    0.00000
C1    1    0.691127    0.000000    0.244767    10.50000    0.07023    0.05371 =
         0.07321    0.00000    0.06075    0.00000
AFIX  43
H1    2    0.665422    0.000000    0.277477    10.50000   -1.20000
AFIX   0
C2    1    0.813711    0.000000    0.286135    10.50000    0.07023    0.05371 =
         0.07321    0.00000    0.06075    0.00000
AFIX  43
H2A   2    0.873295    0.000000    0.342023    10.50000   -1.20000
AFIX   0

PART -1
C11   1   10.742350   10.310281   10.497419    10.25000    0.03801
HKLF 4




REM  rt569_ohpympdmeoh_225k_a.res in C2/m
REM wR2 = 0.2652, GooF = S = 1.304, Restrained GooF = 1.304 for all data
REM R1 = 0.1132 for 1813 Fo > 4sig(Fo) and 0.1178 for all 1914 data
REM 90 parameters refined using 0 restraints

END

WGHT      0.0001    192.2039

REM Highest difference peak  3.195,  deepest hole -3.269,  1-sigma level  0.343
Q1    1   0.5155  0.5000  0.2249  10.50000  0.05    3.20
Q2    1   0.8053  1.0000  0.9612  10.50000  0.05    2.99
Q3    1   0.8375  0.0000  0.4069  10.50000  0.05    2.98
Q4    1   0.4267  0.5000  0.2007  10.50000  0.05    2.70
Q5    1   0.5627  0.5000  0.3288  10.50000  0.05    2.41
;
_shelx_res_checksum              52907
_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 1.197
_oxdiff_exptl_absorpt_empirical_full_min 0.802
####################################################################### 
# 
# 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_rt569_ohpympdmeoh_260k_2
_database_code_depnum_ccdc_archive 'CCDC 2209628'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-27 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT342_rt569_ohpympdmeoh_260k_2 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0375 Ang.
RESPONSE: This alerts arises from the strong disorder of the guest in the structural pores and from a deterioration of the crystal during the desorption readsorption processes
;
_vrf_PLAT420_rt569_ohpympdmeoh_260k_2 
;
PROBLEM: D-H Bond Without Acceptor  O1       --H1A      .     Please Check
RESPONSE: There is a certain number of H-bonds which are properly discussed in the paper. This alert arises from the absence of H atoms which are not present due to the strong agitation of the molecular moieties involved in the H-bond interactions
;
_vrf_PLAT420_rt569_ohpympdmeoh_260k_2_2 
;
PROBLEM: D-H Bond Without Acceptor  O2       --H2       .     Please Check
RESPONSE: There is a certain number of H-bonds which are properly discussed in the paper. This alert arises from the absence of H atoms which are not present due to the strong agitation of the molecular moieties involved in the H-bond interactions
;
_vrf_PLAT430_rt569_ohpympdmeoh_260k_2 
;
PROBLEM: Short Inter D...A Contact  N2       ..O3       .       2.86 Ang.
RESPONSE: There is a certain number of H-bonds which are properly discussed in the paper. This alert arises from the absence of H atoms which are not present due to the strong agitation of the molecular moieties involved in the H-bond interactions
;
_vrf_PLAT971_rt569_ohpympdmeoh_260k_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.97Ang From Pd1             3.24 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_260k_2_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.92Ang From Pd1             3.15 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_260k_2_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.02Ang From Pd1             3.11 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT973_rt569_ohpympdmeoh_260k_2 
;
PROBLEM: Check Calcd Positive Resid. Density on       Pd1       1.72 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Tuesday 27 September 2022 04:39 PM
# end Validation Reply Form

_audit_creation_date             2022-09-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H8 Fe N8 O2 Pd, 0.25(C2 O2)'
_chemical_formula_sum            'C12.50 H8 Fe N8 O2.50 Pd'
_chemical_formula_weight         472.52
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.377(5)
_cell_length_b                   7.4740(5)
_cell_length_c                   15.967(4)
_cell_angle_alpha                90
_cell_angle_beta                 136.88(5)
_cell_angle_gamma                90
_cell_volume                     1743.6(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2668
_cell_measurement_temperature    260.00(10)
_cell_measurement_theta_max      27.3560
_cell_measurement_theta_min      3.7130
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.649
_exptl_absorpt_coefficient_mu    1.890
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7936
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.892
_diffrn_reflns_theta_min         3.009
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      260.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -48.00  42.00   1.00    2.50    --  -16.13  77.00  60.00   90
  2  ω    -94.00 -39.00   1.00    2.50    --  -16.13-178.00 120.00   55
  3  ω    -14.00  42.00   1.00    2.50    --   17.15  77.00-180.00   56
  4  ω    -57.00  67.00   1.00    2.50    --   17.15 -19.00-150.00  124
  5  ω    -85.00   5.00   1.00    2.50    --  -16.13 -57.00 -60.00   90
  6  ω    -14.00  42.00   1.00    2.50    --   17.15  77.00  90.00   56
  7  ω     -4.00  86.00   1.00    2.50    --   17.15  57.00-120.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0241744000
_diffrn_orient_matrix_UB_12      0.0784883000
_diffrn_orient_matrix_UB_13      -0.0352957000
_diffrn_orient_matrix_UB_21      0.0047172000
_diffrn_orient_matrix_UB_22      0.0334308000
_diffrn_orient_matrix_UB_23      0.0459521000
_diffrn_orient_matrix_UB_31      0.0418341000
_diffrn_orient_matrix_UB_32      0.0416020000
_diffrn_orient_matrix_UB_33      0.0295878000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1660
_reflns_number_total             1985
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.411
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.358
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1985
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0708
_refine_ls_restrained_S_all      1.171
_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)+(0.1013P)²+31.7018P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2036
_refine_ls_wR_factor_ref         0.2139
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1a(0.5) H2(0.5) O3(0.25) C11(0.25)
 Fixed X: O3(0.74563) C11(0.75327)
 Fixed Y: O3(0) C11(0.17873)
 Fixed Z: O3(-0.02651) C11(-0.0045)
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C7(H7), C1(H1), C4(H4), C2(H2a)
3.b Idealised tetrahedral OH refined as rotating group:
 O1(H1a), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.74835(5) 0.500000 0.23392(8) 0.0242(3) Uani 1 2 d S T P . .
Fe2 Fe 0.500000 0.000000 0.000000 0.0230(5) Uani 1 4 d S T P . .
Fe1 Fe 1.000000 1.000000 0.500000 0.0243(5) Uani 1 4 d S T P . .
N5 N 0.4618(7) 0.000000 -0.1720(10) 0.037(2) Uani 1 2 d S T P . .
N3 N 0.8966(5) 0.7998(11) 0.3936(7) 0.0414(18) Uani 1 1 d . . . . .
C6 C 0.6539(5) 0.3117(11) 0.1329(7) 0.0306(17) Uani 1 1 d . . . . .
N1 N 1.0167(8) 1.000000 0.3773(11) 0.041(3) Uani 1 2 d S T P . .
C5 C 0.8427(5) 0.6883(11) 0.3358(8) 0.0314(17) Uani 1 1 d . . . . .
N4 N 0.5998(5) 0.2007(10) 0.0770(7) 0.0374(17) Uani 1 1 d . . . . .
C10 C 0.3777(10) 0.000000 -0.2832(12) 0.051(4) Uani 1 2 d S T P . .
H10 H 0.331216 0.000000 -0.288769 0.061 Uiso 1 2 calc R U P . .
N6 N 0.3510(11) 0.000000 -0.3896(14) 0.067(4) Uani 1 2 d S T P . .
C9 C 0.4121(14) 0.000000 -0.3811(15) 0.062(5) Uani 1 2 d S T P . .
H9 H 0.395327 0.000000 -0.453680 0.074 Uiso 1 2 calc R U P . .
N2 N 0.9411(11) 1.000000 0.1695(14) 0.076(5) Uani 1 2 d S T P . .
C7 C 0.5300(12) 0.000000 -0.1612(16) 0.053(4) Uani 1 2 d S T P . .
H7 H 0.590793 0.000000 -0.084565 0.064 Uiso 1 2 calc R U P . .
C1 C 0.9433(14) 1.000000 0.2557(14) 0.067(5) Uani 1 2 d S T P . .
H1 H 0.886835 1.000000 0.227276 0.080 Uiso 1 2 calc R U P . .
O1 O 1.1794(9) 1.000000 0.3675(12) 0.095(6) Uani 1 2 d S T P . .
H1A H 1.172799 1.048644 0.315366 0.143 Uiso 0.5 1 calc R U P . .
C3 C 1.0997(11) 1.000000 0.3306(17) 0.054(4) Uani 1 2 d S T P . .
O2 O 0.5705(11) 0.000000 -0.2648(15) 0.112(6) Uani 1 2 d S T P . .
H2 H 0.551471 -0.050526 -0.325486 0.168 Uiso 0.5 1 calc R U P . .
C4 C 1.0968(12) 1.000000 0.4170(17) 0.055(4) Uani 1 2 d S T P . .
H4 H 1.150800 1.000000 0.500649 0.066 Uiso 1 2 calc R U P . .
C8 C 0.5072(14) 0.000000 -0.270(2) 0.067(5) Uani 1 2 d S T P . .
C2 C 1.0189(13) 1.000000 0.2101(16) 0.070(5) Uani 1 2 d S T P . .
H2A H 1.020569 1.000000 0.153484 0.084 Uiso 1 2 calc R U P . .
O3 O 0.745629 0.000000 -0.026511 0.076(7) Uiso 0.25 1 d S . P A -1
C11 C 0.753270 0.178730 -0.004500 0.063(12) Uiso 0.25 1 d . . P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0221(5) 0.0106(4) 0.0305(5) 0.000 0.0161(4) 0.000
Fe2 0.0199(10) 0.0103(10) 0.0288(11) 0.000 0.0146(10) 0.000
Fe1 0.0215(11) 0.0103(10) 0.0295(11) 0.000 0.0149(10) 0.000
N5 0.040(6) 0.031(6) 0.045(6) 0.000 0.033(5) 0.000
N3 0.029(4) 0.023(4) 0.044(4) -0.005(3) 0.017(3) -0.004(3)
C6 0.027(4) 0.020(4) 0.034(4) 0.003(3) 0.019(4) 0.003(3)
N1 0.047(6) 0.036(6) 0.051(6) 0.000 0.040(6) 0.000
C5 0.024(4) 0.021(4) 0.033(4) 0.001(3) 0.015(3) 0.001(3)
N4 0.031(4) 0.022(4) 0.047(4) -0.005(3) 0.025(3) -0.007(3)
C10 0.049(8) 0.054(9) 0.030(7) 0.000 0.023(7) 0.000
N6 0.071(9) 0.066(10) 0.057(8) 0.000 0.044(8) 0.000
C9 0.086(13) 0.063(11) 0.041(8) 0.000 0.048(10) 0.000
N2 0.067(10) 0.107(14) 0.055(8) 0.000 0.045(8) 0.000
C7 0.078(11) 0.035(8) 0.063(9) 0.000 0.057(9) 0.000
C1 0.086(12) 0.076(12) 0.039(8) 0.000 0.046(9) 0.000
O1 0.061(8) 0.177(18) 0.056(7) 0.000 0.045(7) 0.000
C3 0.051(8) 0.047(9) 0.077(11) 0.000 0.051(9) 0.000
O2 0.115(12) 0.17(2) 0.093(11) 0.000 0.090(11) 0.000
C4 0.062(10) 0.046(9) 0.069(10) 0.000 0.052(9) 0.000
C8 0.101(14) 0.054(10) 0.106(14) 0.000 0.095(13) 0.000
C2 0.073(12) 0.087(14) 0.049(9) 0.000 0.044(10) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C6 1.976(8) 6_565 ?
Pd1 C6 1.976(8) . ?
Pd1 C5 1.976(9) . ?
Pd1 C5 1.976(8) 6_565 ?
Fe2 N5 2.221(11) . ?
Fe2 N5 2.221(11) 5_655 ?
Fe2 N4 2.117(7) 6 ?
Fe2 N4 2.117(7) 5_655 ?
Fe2 N4 2.117(7) . ?
Fe2 N4 2.117(7) 2_655 ?
Fe1 N3 2.128(8) . ?
Fe1 N3 2.128(8) 2_756 ?
Fe1 N3 2.128(8) 5_776 ?
Fe1 N3 2.128(8) 6_575 ?
Fe1 N1 2.234(11) 5_776 ?
Fe1 N1 2.234(11) . ?
N5 C10 1.314(17) . ?
N5 C7 1.338(19) . ?
N3 C5 1.150(12) . ?
C6 N4 1.147(11) . ?
N1 C1 1.336(19) . ?
N1 C4 1.321(19) . ?
C10 H10 0.9300 . ?
C10 N6 1.34(2) . ?
N6 C9 1.21(2) . ?
C9 H9 0.9300 . ?
C9 C8 1.42(3) . ?
N2 C1 1.34(2) . ?
N2 C2 1.27(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.41(2) . ?
C1 H1 0.9300 . ?
O1 H1A 0.8200 . ?
O1 H1A 0.8(3) 6_575 ?
O1 C3 1.337(18) . ?
C3 C4 1.42(2) . ?
C3 C2 1.35(2) . ?
O2 H2 0.8200 . ?
O2 H2 0.8(3) 6 ?
O2 C8 1.30(2) . ?
C4 H4 0.9300 . ?
C2 H2A 0.9300 . ?
O3 C11 1.36045(9) . ?

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
C6 Pd1 C6 90.8(5) 6_565 . ?
C6 Pd1 C5 89.2(4) 6_565 . ?
C6 Pd1 C5 179.5(4) . . ?
C6 Pd1 C5 179.5(4) 6_565 6_565 ?
C6 Pd1 C5 89.2(4) . 6_565 ?
C5 Pd1 C5 90.8(5) . 6_565 ?
N5 Fe2 N5 180.0 5_655 . ?
N4 Fe2 N5 88.7(3) 6 5_655 ?
N4 Fe2 N5 88.7(3) . 5_655 ?
N4 Fe2 N5 88.7(3) 2_655 . ?
N4 Fe2 N5 91.3(3) 6 . ?
N4 Fe2 N5 91.3(3) 5_655 5_655 ?
N4 Fe2 N5 91.3(3) 2_655 5_655 ?
N4 Fe2 N5 91.3(3) . . ?
N4 Fe2 N5 88.7(3) 5_655 . ?
N4 Fe2 N4 180.0 5_655 . ?
N4 Fe2 N4 90.2(4) 5_655 2_655 ?
N4 Fe2 N4 89.8(4) 2_655 . ?
N4 Fe2 N4 180.0(5) 6 2_655 ?
N4 Fe2 N4 89.8(4) 5_655 6 ?
N4 Fe2 N4 90.2(4) 6 . ?
N3 Fe1 N3 89.4(4) 5_776 2_756 ?
N3 Fe1 N3 90.6(4) 5_776 6_575 ?
N3 Fe1 N3 180.0 6_575 2_756 ?
N3 Fe1 N3 180.0 5_776 . ?
N3 Fe1 N3 89.4(4) 6_575 . ?
N3 Fe1 N3 90.6(4) 2_756 . ?
N3 Fe1 N1 92.1(3) 6_575 . ?
N3 Fe1 N1 92.1(3) 2_756 5_776 ?
N3 Fe1 N1 87.9(3) 2_756 . ?
N3 Fe1 N1 87.9(3) 5_776 . ?
N3 Fe1 N1 87.9(3) . 5_776 ?
N3 Fe1 N1 87.9(3) 6_575 5_776 ?
N3 Fe1 N1 92.1(3) 5_776 5_776 ?
N3 Fe1 N1 92.1(3) . . ?
N1 Fe1 N1 180.0 5_776 . ?
C10 N5 Fe2 125.2(10) . . ?
C10 N5 C7 117.5(13) . . ?
C7 N5 Fe2 117.3(10) . . ?
C5 N3 Fe1 177.5(8) . . ?
N4 C6 Pd1 178.2(8) . . ?
C1 N1 Fe1 120.3(11) . . ?
C4 N1 Fe1 124.0(11) . . ?
C4 N1 C1 115.7(14) . . ?
N3 C5 Pd1 178.9(10) . . ?
C6 N4 Fe2 168.6(7) . . ?
N5 C10 H10 116.2 . . ?
N5 C10 N6 127.5(16) . . ?
N6 C10 H10 116.2 . . ?
C9 N6 C10 115.6(16) . . ?
N6 C9 H9 117.2 . . ?
N6 C9 C8 125.5(15) . . ?
C8 C9 H9 117.2 . . ?
C2 N2 C1 115.1(16) . . ?
N5 C7 H7 120.9 . . ?
N5 C7 C8 118.2(16) . . ?
C8 C7 H7 120.9 . . ?
N1 C1 N2 128.0(18) . . ?
N1 C1 H1 116.0 . . ?
N2 C1 H1 116.0 . . ?
H1A O1 H1A 52.6 . 6_575 ?
C3 O1 H1A 109(7) . 6_575 ?
C3 O1 H1A 109.5 . . ?
O1 C3 C4 121.1(16) . . ?
O1 C3 C2 121.2(16) . . ?
C2 C3 C4 117.7(15) . . ?
H2 O2 H2 54.8 . 6 ?
C8 O2 H2 109(9) . 6 ?
C8 O2 H2 109.5 . . ?
N1 C4 C3 119.4(15) . . ?
N1 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C7 C8 C9 115.6(15) . . ?
O2 C8 C9 123.5(17) . . ?
O2 C8 C7 120.9(19) . . ?
N2 C2 C3 124.1(17) . . ?
N2 C2 H2A 117.9 . . ?
C3 C2 H2A 117.9 . . ?

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
Fe2 N5 C10 N6 180.000(5) . . . . ?
Fe2 N5 C7 C8 180.000(4) . . . . ?
Fe1 N1 C1 N2 180.000(4) . . . . ?
Fe1 N1 C4 C3 180.000(5) . . . . ?
N5 C10 N6 C9 0.000(8) . . . . ?
N5 C7 C8 C9 0.000(5) . . . . ?
N5 C7 C8 O2 180.000(4) . . . . ?
C10 N5 C7 C8 0.000(5) . . . . ?
C10 N6 C9 C8 0.000(8) . . . . ?
N6 C9 C8 C7 0.000(8) . . . . ?
N6 C9 C8 O2 180.000(6) . . . . ?
C7 N5 C10 N6 0.000(5) . . . . ?
C1 N1 C4 C3 0.000(7) . . . . ?
C1 N2 C2 C3 0.000(6) . . . . ?
O1 C3 C4 N1 180.000(6) . . . . ?
O1 C3 C2 N2 180.000(5) . . . . ?
C4 N1 C1 N2 0.000(6) . . . . ?
C4 C3 C2 N2 0.000(4) . . . . ?
C2 N2 C1 N1 0.000(4) . . . . ?
C2 C3 C4 N1 0.000(7) . . . . ?

_shelx_res_file                  
;
TITL rt569_ohpympdmeoh_260k_2_a.res in C2/m
    rt569_ohpympdmeoh_260k_2.res
    created by SHELXL-2018/3 at 16:02:31 on 27-Sep-2022
REM Old TITL RT569_OHPymPdMeOH_260K_2 in C2/m
REM SHELXT solution in C2/m: R1 0.156, Rweak 0.007, Alpha 0.040
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C12 N2 Fe Pd
CELL 0.71073 21.3769 7.474 15.9668 90 136.884 90
ZERR 4 0.0054 0.0005 0.0041 0 0.048 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pd
UNIT 50 32 4 32 10 4

L.S. 10
PLAN  4
SIZE 0.2 0.25 0.03
TEMP -13.13
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
OMIT -2 0 4
REM <olex2.extras>
REM <HklSrc "%.\\RT569_OHPymPdMeOH_260K_2.hkl">
REM </olex2.extras>

WGHT    0.101300   31.701799
FVAR       0.16532
PD1   6    0.748352    0.500000    0.233919    10.50000    0.02209    0.01063 =
         0.03048    0.00000    0.01615    0.00000
FE2   3    0.500000    0.000000    0.000000    10.25000    0.01993    0.01034 =
         0.02881    0.00000    0.01459    0.00000
FE1   3    1.000000    1.000000    0.500000    10.25000    0.02154    0.01029 =
         0.02946    0.00000    0.01490    0.00000
N5    4    0.461813    0.000000   -0.171952    10.50000    0.04020    0.03117 =
         0.04545    0.00000    0.03285    0.00000
N3    4    0.896622    0.799846    0.393569    11.00000    0.02870    0.02309 =
         0.04357   -0.00486    0.01720   -0.00384
C6    1    0.653865    0.311728    0.132948    11.00000    0.02730    0.02029 =
         0.03395    0.00344    0.01909    0.00273
N1    4    1.016747    1.000000    0.377264    10.50000    0.04730    0.03566 =
         0.05104    0.00000    0.03987    0.00000
C5    1    0.842713    0.688337    0.335820    11.00000    0.02400    0.02080 =
         0.03255    0.00064    0.01525    0.00061
N4    4    0.599782    0.200734    0.077009    11.00000    0.03140    0.02211 =
         0.04711   -0.00507    0.02495   -0.00705
C10   1    0.377671    0.000000   -0.283187    10.50000    0.04873    0.05435 =
         0.03024    0.00000    0.02289    0.00000
AFIX  43
H10   2    0.331216    0.000000   -0.288769    10.50000   -1.20000
AFIX   0
N6    4    0.350989    0.000000   -0.389639    10.50000    0.07068    0.06615 =
         0.05741    0.00000    0.04428    0.00000
C9    1    0.412057    0.000000   -0.381131    10.50000    0.08579    0.06308 =
         0.04142    0.00000    0.04792    0.00000
AFIX  43
H9    2    0.395327    0.000000   -0.453680    10.50000   -1.20000
AFIX   0
N2    4    0.941081    1.000000    0.169488    10.50000    0.06710    0.10704 =
         0.05467    0.00000    0.04471    0.00000
C7    1    0.530002    0.000000   -0.161242    10.50000    0.07798    0.03481 =
         0.06301    0.00000    0.05660    0.00000
AFIX  43
H7    2    0.590793    0.000000   -0.084565    10.50000   -1.20000
AFIX   0
C1    1    0.943338    1.000000    0.255677    10.50000    0.08647    0.07579 =
         0.03931    0.00000    0.04611    0.00000
AFIX  43
H1    2    0.886835    1.000000    0.227276    10.50000   -1.20000
AFIX   0
O1    5    1.179424    1.000000    0.367473    10.50000    0.06118    0.17731 =
         0.05555    0.00000    0.04525    0.00000
AFIX 147
H1A   2    1.172799    1.048644    0.315366    10.50000   -1.50000
AFIX   0
C3    1    1.099672    1.000000    0.330650    10.50000    0.05101    0.04743 =
         0.07695    0.00000    0.05057    0.00000
O2    5    0.570500    0.000000   -0.264759    10.50000    0.11466    0.17353 =
         0.09260    0.00000    0.09001    0.00000
AFIX 147
H2    2    0.551471   -0.050526   -0.325486    10.50000   -1.50000
AFIX   0
C4    1    1.096812    1.000000    0.417032    10.50000    0.06170    0.04631 =
         0.06881    0.00000    0.05153    0.00000
AFIX  43
H4    2    1.150800    1.000000    0.500649    10.50000   -1.20000
AFIX   0
C8    1    0.507162    0.000000   -0.269677    10.50000    0.10136    0.05367 =
         0.10561    0.00000    0.09495    0.00000
C2    1    1.018936    1.000000    0.210115    10.50000    0.07320    0.08662 =
         0.04920    0.00000    0.04432    0.00000
AFIX  43
H2A   2    1.020569    1.000000    0.153484    10.50000   -1.20000
AFIX   0

PART -1
O3    5   10.745629   10.000000    9.973489    10.25000    0.07558
C11   1   10.753270   10.178730    9.995500    10.25000    0.06332
HKLF 4




REM  rt569_ohpympdmeoh_260k_2_a.res in C2/m
REM wR2 = 0.2139, GooF = S = 1.171, Restrained GooF = 1.171 for all data
REM R1 = 0.0708 for 1660 Fo > 4sig(Fo) and 0.0838 for all 1985 data
REM 139 parameters refined using 0 restraints

END

WGHT      0.1014     31.9956

REM Highest difference peak  3.411,  deepest hole -1.125,  1-sigma level  0.358
Q1    1   0.7525  0.5000  0.2988  10.50000  0.05    3.41
Q2    1   0.8111  0.5000  0.2987  10.50000  0.05    3.24
Q3    1   0.7531  0.5000  0.1791  10.50000  0.05    3.02
Q4    1   0.3276  0.0000 -0.4825  10.50000  0.05    2.31
;
_shelx_res_checksum              69334
_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 6.544
_oxdiff_exptl_absorpt_empirical_full_min 0.696
####################################################################### 
# 
# 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_rt366_feohpmdpd_240k_0m
_database_code_depnum_ccdc_archive 'CCDC 2209620'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_rt366_feohpmdpd_240k_0m 
;
PROBLEM: Check Calcd Resid. Dens.  1.05Ang From Pd1             3.87 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pd metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt366_feohpmdpd_240k_0m_2 
;
PROBLEM: Check Calcd Resid. Dens.  1.10Ang From Pd1             3.71 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the Pd atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT342_rt366_feohpmdpd_240k_0m 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0375 Ang.
RESPONSE: This alerts arises from the strong disorder of the guest in the structural pores
;
_vrf_PLAT430_rt366_feohpmdpd_240k_0m 
;
PROBLEM: Short Inter D...A Contact  O3       ..N2       .       2.86 Ang.
RESPONSE: There is a certain number of H-bonds which are properly discussed in the paper. This alert arises from the absence of H atoms which are not present due to the strong agitation of the molecular moieties involved in the H-bond interactions
;
_vrf_PLAT971_rt366_feohpmdpd_240k_0m_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.35Ang From Fe2             3.01 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt366_feohpmdpd_240k_0m_4 
;
PROBLEM: Check Calcd Resid. Dens.  1.39Ang From Fe1             2.86 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Monday 26 September 2022 03:56 PM
# end Validation Reply Form

_audit_creation_date             2022-05-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H8 Fe N8 O2 Pd, O'
_chemical_formula_sum            'C12 H8 Fe N8 O3 Pd'
_chemical_formula_weight         474.51
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.3012(13)
_cell_length_b                   7.3122(5)
_cell_length_c                   14.4884(9)
_cell_angle_alpha                90
_cell_angle_beta                 132.618(2)
_cell_angle_gamma                90
_cell_volume                     1660.66(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7083
_cell_measurement_temperature    240.0
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.60
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.987
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1167 before and 0.0744 after correction.
The Ratio of minimum to maximum transmission is 0.8836.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16475
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.290
_diffrn_reflns_theta_min         2.599
_diffrn_ambient_temperature      240.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1984
_reflns_number_total             2209
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         4.067
_refine_diff_density_min         -2.134
_refine_diff_density_rms         0.294
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.252
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0873
_refine_ls_restrained_S_all      1.252
_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)+(0.0234P)²+124.0986P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2278
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1(0.5) H2A(0.5) O3(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C4(H4), C7(H7), C2(H2), C9(H9), C1(H1A)
3.b Tetrahedral OH refined with riding coordinates:
 O1(H1), O2(H2A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.51662(7) 0.500000 0.25725(10) 0.0172(3) Uani 1 2 d S T P . .
Fe2 Fe 0.500000 0.000000 0.000000 0.0173(6) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 1.000000 0.500000 0.0190(6) Uani 1 4 d S T P . .
N5 N 0.6232(9) 0.000000 0.0902(14) 0.028(3) Uani 1 2 d S T P . .
N4 N 0.5190(6) 0.1899(13) 0.1099(9) 0.0261(18) Uani 1 1 d . . . . .
N1 N 0.6428(9) 1.000000 0.6551(14) 0.031(3) Uani 1 2 d S T P . .
O1 O 0.8105(9) 1.000000 0.9902(12) 0.060(5) Uani 1 2 d S T P . .
H1 H 0.786936 0.928285 1.003042 0.090 Uiso 0.5 1 calc R U P . .
N2 N 0.7762(10) 1.000000 0.7135(16) 0.040(4) Uani 1 2 d S T P . .
N6 N 0.7320(11) 0.000000 0.0820(14) 0.038(4) Uani 1 2 d S T P . .
O2 O 0.8304(9) 0.000000 0.4004(13) 0.061(5) Uani 1 2 d S T P . .
H2A H 0.809229 0.028363 0.429859 0.091 Uiso 0.5 1 calc R U P . .
N3 N 0.5014(7) 0.7973(14) 0.3966(9) 0.032(2) Uani 1 1 d . . . . .
C6 C 0.5213(7) 0.3042(14) 0.1657(9) 0.0210(19) Uani 1 1 d . . . . .
C10 C 0.6508(10) 0.000000 0.0298(15) 0.029(3) Uani 1 2 d S T P . .
H10 H 0.608659 0.000000 -0.058288 0.035 Uiso 1 2 calc R U P . .
C5 C 0.5074(7) 0.6905(14) 0.3437(10) 0.025(2) Uani 1 1 d . . . . .
C8 C 0.7716(11) 0.000000 0.2793(15) 0.036(4) Uani 1 2 d S T P . .
C4 C 0.6812(11) 1.000000 0.7752(15) 0.030(3) Uani 1 2 d S T P . .
H4 H 0.647955 1.000000 0.796185 0.035 Uiso 1 2 calc R U P . .
C3 C 0.7692(12) 1.000000 0.8698(17) 0.036(4) Uani 1 2 d S T P . .
C7 C 0.6830(11) 0.000000 0.2138(15) 0.028(3) Uani 1 2 d S T P . .
H7 H 0.666734 0.000000 0.260056 0.033 Uiso 1 2 calc R U P . .
C2 C 0.8138(12) 1.000000 0.8323(18) 0.041(4) Uani 1 2 d S T P . .
H2 H 0.873697 1.000000 0.894268 0.050 Uiso 1 2 calc R U P . .
C9 C 0.7911(11) 0.000000 0.2051(17) 0.038(4) Uani 1 2 d S T P . .
H9 H 0.848720 0.000000 0.244588 0.045 Uiso 1 2 calc R U P . .
C1 C 0.6893(13) 1.000000 0.6288(18) 0.043(5) Uani 1 2 d S T P . .
H1A H 0.660971 1.000000 0.543397 0.051 Uiso 1 2 calc R U P . .
O3 O 0.7725(16) 0.073(4) 0.516(3) 0.078(8) Uiso 0.5 1 d . . P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0242(5) 0.0141(5) 0.0172(5) 0.000 0.0156(4) 0.000
Fe2 0.0270(14) 0.0138(12) 0.0199(13) 0.000 0.0193(12) 0.000
Fe1 0.0311(15) 0.0151(13) 0.0212(14) 0.000 0.0218(13) 0.000
N5 0.044(8) 0.011(5) 0.045(8) 0.000 0.036(7) 0.000
N4 0.038(5) 0.022(4) 0.029(4) -0.001(4) 0.027(4) -0.001(4)
N1 0.039(8) 0.023(7) 0.038(8) 0.000 0.029(7) 0.000
O1 0.036(7) 0.115(15) 0.025(7) 0.000 0.018(6) 0.000
N2 0.035(8) 0.053(10) 0.042(9) 0.000 0.029(7) 0.000
N6 0.049(9) 0.045(9) 0.032(8) 0.000 0.032(7) 0.000
O2 0.039(8) 0.096(14) 0.031(7) 0.000 0.017(6) 0.000
N3 0.049(6) 0.024(5) 0.032(5) 0.004(4) 0.032(5) 0.007(4)
C6 0.031(5) 0.017(5) 0.023(5) -0.001(4) 0.022(4) -0.003(4)
C10 0.029(8) 0.037(9) 0.020(7) 0.000 0.016(6) 0.000
C5 0.045(6) 0.016(5) 0.023(5) -0.002(4) 0.027(5) -0.002(4)
C8 0.033(8) 0.036(9) 0.016(7) 0.000 0.009(7) 0.000
C4 0.032(8) 0.032(9) 0.027(8) 0.000 0.022(7) 0.000
C3 0.038(9) 0.039(10) 0.030(9) 0.000 0.022(8) 0.000
C7 0.036(8) 0.021(7) 0.026(7) 0.000 0.021(7) 0.000
C2 0.032(9) 0.057(12) 0.035(9) 0.000 0.023(8) 0.000
C9 0.019(7) 0.039(10) 0.037(9) 0.000 0.012(7) 0.000
C1 0.052(11) 0.053(12) 0.031(9) 0.000 0.031(9) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C6 2.000(10) . ?
Pd1 C6 2.000(10) 6_565 ?
Pd1 C5 1.970(10) . ?
Pd1 C5 1.970(10) 6_565 ?
Fe2 N5 1.988(14) 5_655 ?
Fe2 N5 1.988(14) . ?
Fe2 N4 1.938(9) 2_655 ?
Fe2 N4 1.938(9) . ?
Fe2 N4 1.938(9) 6 ?
Fe2 N4 1.938(9) 5_655 ?
Fe1 N1 2.246(15) 5_676 ?
Fe1 N1 2.246(15) . ?
Fe1 N3 2.123(9) 6_575 ?
Fe1 N3 2.123(9) . ?
Fe1 N3 2.123(9) 2_656 ?
Fe1 N3 2.123(9) 5_676 ?
N5 C10 1.34(2) . ?
N5 C7 1.32(2) . ?
N4 C6 1.140(13) . ?
N1 C4 1.33(2) . ?
N1 C1 1.28(2) . ?
O1 H1 0.8300 . ?
O1 H1 0.8299 6_575 ?
O1 C3 1.32(2) . ?
N2 C2 1.32(2) . ?
N2 C1 1.36(3) . ?
N6 C10 1.34(2) . ?
N6 C9 1.31(2) . ?
O2 H2A 0.8301 6 ?
O2 H2A 0.8300 . ?
O2 C8 1.29(2) . ?
N3 C5 1.160(14) . ?
C10 H10 0.9400 . ?
C8 C7 1.43(2) . ?
C8 C9 1.39(3) . ?
C4 H4 0.9400 . ?
C4 C3 1.38(2) . ?
C3 C2 1.38(3) . ?
C7 H7 0.9400 . ?
C2 H2 0.9400 . ?
C9 H9 0.9400 . ?
C1 H1A 0.9400 . ?

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
C6 Pd1 C6 91.4(5) 6_565 . ?
C5 Pd1 C6 177.8(4) . . ?
C5 Pd1 C6 177.8(4) 6_565 6_565 ?
C5 Pd1 C6 89.3(4) 6_565 . ?
C5 Pd1 C6 89.3(4) . 6_565 ?
C5 Pd1 C5 90.0(6) . 6_565 ?
N5 Fe2 N5 180.0 . 5_655 ?
N4 Fe2 N5 90.7(4) 6 . ?
N4 Fe2 N5 90.7(4) . . ?
N4 Fe2 N5 89.3(4) 6 5_655 ?
N4 Fe2 N5 90.7(4) 2_655 5_655 ?
N4 Fe2 N5 89.3(4) 5_655 . ?
N4 Fe2 N5 89.3(4) 2_655 . ?
N4 Fe2 N5 89.3(4) . 5_655 ?
N4 Fe2 N5 90.7(4) 5_655 5_655 ?
N4 Fe2 N4 180.0 5_655 . ?
N4 Fe2 N4 91.6(5) 5_655 2_655 ?
N4 Fe2 N4 88.4(5) 2_655 . ?
N4 Fe2 N4 180.0(6) 6 2_655 ?
N4 Fe2 N4 88.4(5) 5_655 6 ?
N4 Fe2 N4 91.6(5) 6 . ?
N1 Fe1 N1 180.0 . 5_676 ?
N3 Fe1 N1 87.2(4) . 5_676 ?
N3 Fe1 N1 87.2(4) 6_575 5_676 ?
N3 Fe1 N1 87.2(4) 2_656 . ?
N3 Fe1 N1 87.2(4) 5_676 . ?
N3 Fe1 N1 92.8(4) 5_676 5_676 ?
N3 Fe1 N1 92.8(4) 6_575 . ?
N3 Fe1 N1 92.8(4) 2_656 5_676 ?
N3 Fe1 N1 92.8(4) . . ?
N3 Fe1 N3 180.0(5) . 5_676 ?
N3 Fe1 N3 88.6(5) 5_676 2_656 ?
N3 Fe1 N3 88.6(5) . 6_575 ?
N3 Fe1 N3 91.4(5) . 2_656 ?
N3 Fe1 N3 91.4(5) 5_676 6_575 ?
N3 Fe1 N3 180.0 6_575 2_656 ?
C10 N5 Fe2 122.5(12) . . ?
C7 N5 Fe2 121.5(11) . . ?
C7 N5 C10 116.0(15) . . ?
C6 N4 Fe2 173.0(10) . . ?
C4 N1 Fe1 121.7(11) . . ?
C1 N1 Fe1 119.9(13) . . ?
C1 N1 C4 118.4(16) . . ?
H1 O1 H1 78.4 . 6_575 ?
C3 O1 H1 109.5 . . ?
C3 O1 H1 109.5(8) . 6_575 ?
C2 N2 C1 115.4(16) . . ?
C9 N6 C10 116.7(15) . . ?
H2A O2 H2A 28.9 . 6 ?
C8 O2 H2A 109.5(11) . 6 ?
C8 O2 H2A 109.5 . . ?
C5 N3 Fe1 175.6(10) . . ?
N4 C6 Pd1 175.8(9) . . ?
N5 C10 H10 116.6 . . ?
N6 C10 N5 126.8(15) . . ?
N6 C10 H10 116.6 . . ?
N3 C5 Pd1 177.3(9) . . ?
O2 C8 C7 122.2(18) . . ?
O2 C8 C9 121.8(18) . . ?
C9 C8 C7 116.0(15) . . ?
N1 C4 H4 119.5 . . ?
N1 C4 C3 121.1(16) . . ?
C3 C4 H4 119.5 . . ?
O1 C3 C4 123.6(17) . . ?
O1 C3 C2 120.0(17) . . ?
C2 C3 C4 116.4(16) . . ?
N5 C7 C8 122.0(15) . . ?
N5 C7 H7 119.0 . . ?
C8 C7 H7 119.0 . . ?
N2 C2 C3 122.9(18) . . ?
N2 C2 H2 118.5 . . ?
C3 C2 H2 118.5 . . ?
N6 C9 C8 122.5(16) . . ?
N6 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
N1 C1 N2 125.8(18) . . ?
N1 C1 H1A 117.1 . . ?
N2 C1 H1A 117.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe2 N5 C10 N6 180.000(1) . . . . ?
Fe2 N5 C7 C8 180.000(2) . . . . ?
Fe1 N1 C4 C3 180.000(10) . . . . ?
Fe1 N1 C1 N2 180.000(8) . . . . ?
N1 C4 C3 O1 180.000(10) . . . . ?
N1 C4 C3 C2 0.000(14) . . . . ?
O1 C3 C2 N2 180.000(13) . . . . ?
O2 C8 C7 N5 180.000(4) . . . . ?
O2 C8 C9 N6 180.000(4) . . . . ?
C10 N5 C7 C8 0.000(3) . . . . ?
C10 N6 C9 C8 0.000(3) . . . . ?
C4 N1 C1 N2 0.000(12) . . . . ?
C4 C3 C2 N2 0.000(15) . . . . ?
C7 N5 C10 N6 0.000(2) . . . . ?
C7 C8 C9 N6 0.000(4) . . . . ?
C2 N2 C1 N1 0.000(13) . . . . ?
C9 N6 C10 N5 0.000(2) . . . . ?
C9 C8 C7 N5 0.000(4) . . . . ?
C1 N1 C4 C3 0.000(13) . . . . ?
C1 N2 C2 C3 0.000(12) . . . . ?

_shelx_res_file                  
;
TITL rt366_feohpmdpd_240k_0m_a.res in C2/m
    rt366_feohpmdpd_240k_0m.res
    created by SHELXL-2018/3 at 23:13:24 on 19-May-2022
REM Old TITL RT366_FeOHPmdPd_240K_0m in C2/m
REM SHELXT solution in C2/m
REM R1 0.146, Rweak 0.020, Alpha 0.073, Orientation as input
REM Formula found by SHELXT: C9 N15 Fe Pd
CELL 0.71073 21.3012 7.3122 14.4884 90 132.618 90
ZERR 4 0.0013 0.0005 0.0009 0 0.002 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pd
UNIT 48 32 4 32 12 4

L.S. 15
PLAN  2
TEMP -33.15
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\RT366_FeOHPmdPd_240K_0m.hkl">
REM </olex2.extras>

WGHT    0.023400  124.098602
FVAR       0.24813
PD1   6    0.516621    0.500000    0.257250    10.50000    0.02424    0.01415 =
         0.01722    0.00000    0.01560    0.00000
FE2   3    0.500000    0.000000    0.000000    10.25000    0.02699    0.01379 =
         0.01985    0.00000    0.01931    0.00000
FE1   3    0.500000    1.000000    0.500000    10.25000    0.03106    0.01515 =
         0.02116    0.00000    0.02180    0.00000
N5    4    0.623223    0.000000    0.090151    10.50000    0.04430    0.01065 =
         0.04453    0.00000    0.03581    0.00000
N4    4    0.518995    0.189936    0.109908    11.00000    0.03847    0.02244 =
         0.02886   -0.00099    0.02742   -0.00088
N1    4    0.642757    1.000000    0.655102    10.50000    0.03903    0.02281 =
         0.03811    0.00000    0.02925    0.00000
O1    5    0.810535    1.000000    0.990203    10.50000    0.03579    0.11496 =
         0.02484    0.00000    0.01839    0.00000
AFIX  83
H1    2    0.786936    0.928285    1.003042    10.50000   -1.50000
AFIX   0
N2    4    0.776184    1.000000    0.713493    10.50000    0.03458    0.05251 =
         0.04243    0.00000    0.02944    0.00000
N6    4    0.732046    0.000000    0.082028    10.50000    0.04853    0.04498 =
         0.03224    0.00000    0.03217    0.00000
O2    5    0.830363    0.000000    0.400359    10.50000    0.03872    0.09640 =
         0.03124    0.00000    0.01733    0.00000
AFIX  83
H2A   2    0.809229    0.028363    0.429859    10.50000   -1.50000
AFIX   0
N3    4    0.501442    0.797293    0.396575    11.00000    0.04927    0.02370 =
         0.03232    0.00369    0.03153    0.00677
C6    1    0.521345    0.304250    0.165713    11.00000    0.03138    0.01684 =
         0.02349   -0.00093    0.02200   -0.00272
C10   1    0.650801    0.000000    0.029822    10.50000    0.02903    0.03684 =
         0.01958    0.00000    0.01573    0.00000
AFIX  43
H10   2    0.608659    0.000000   -0.058288    10.50000   -1.20000
AFIX   0
C5    1    0.507434    0.690459    0.343713    11.00000    0.04459    0.01592 =
         0.02313   -0.00199    0.02669   -0.00216
C8    1    0.771554    0.000000    0.279334    10.50000    0.03311    0.03633 =
         0.01649    0.00000    0.00853    0.00000
C4    1    0.681161    1.000000    0.775218    10.50000    0.03226    0.03245 =
         0.02750    0.00000    0.02171    0.00000
AFIX  43
H4    2    0.647955    1.000000    0.796185    10.50000   -1.20000
AFIX   0
C3    1    0.769190    1.000000    0.869766    10.50000    0.03751    0.03937 =
         0.03004    0.00000    0.02190    0.00000
C7    1    0.683000    0.000000    0.213802    10.50000    0.03637    0.02053 =
         0.02571    0.00000    0.02070    0.00000
AFIX  43
H7    2    0.666734    0.000000    0.260056    10.50000   -1.20000
AFIX   0
C2    1    0.813766    1.000000    0.832347    10.50000    0.03236    0.05724 =
         0.03485    0.00000    0.02288    0.00000
AFIX  43
H2    2    0.873697    1.000000    0.894268    10.50000   -1.20000
AFIX   0
C9    1    0.791087    0.000000    0.205139    10.50000    0.01922    0.03865 =
         0.03734    0.00000    0.01190    0.00000
AFIX  43
H9    2    0.848720    0.000000    0.244588    10.50000   -1.20000
AFIX   0
C1    1    0.689292    1.000000    0.628779    10.50000    0.05160    0.05338 =
         0.03059    0.00000    0.03087    0.00000
AFIX  43
H1A   2    0.660971    1.000000    0.543397    10.50000   -1.20000
AFIX   0

PART -1
O3    5    0.772545    0.073126    0.515688    10.50000    0.07832
HKLF 4




REM  rt366_feohpmdpd_240k_0m_a.res in C2/m
REM wR2 = 0.2278, GooF = S = 1.252, Restrained GooF = 1.252 for all data
REM R1 = 0.0873 for 1984 Fo > 4sig(Fo) and 0.0979 for all 2209 data
REM 139 parameters refined using 0 restraints

END

WGHT      0.0236    124.1154

REM Highest difference peak  4.067,  deepest hole -2.134,  1-sigma level  0.294
Q1    1   0.5202  0.5000  0.3367  10.50000  0.05    4.07
Q2    1   0.5240  0.5000  0.1912  10.50000  0.05    3.50
;
_shelx_res_checksum              16130
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_rt569_ohpympdmeoh_120k
_database_code_depnum_ccdc_archive 'CCDC 2209630'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-27 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_rt569_ohpympdmeoh_120k 
;
PROBLEM: Check Calcd Resid. Dens.  1.08Ang From C3              3.57 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C3 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT342_rt569_ohpympdmeoh_120k 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0325 Ang.
RESPONSE: This alerts arises from the strong disorder of the guest in the structural pores and from a deterioration of the crystal during the desorption readsorption processes
;
_vrf_PLAT971_rt569_ohpympdmeoh_120k_2 
;
PROBLEM: Check Calcd Resid. Dens.  1.07Ang From N2              3.37 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_120k_3 
;
PROBLEM: Check Calcd Resid. Dens.  0.73Ang From C8              3.36 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C8 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_120k_4 
;
PROBLEM: Check Calcd Resid. Dens.  1.35Ang From N6              3.32 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N6 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_120k_5 
;
PROBLEM: Check Calcd Resid. Dens.  0.03Ang From N5              2.89 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N5 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_120k_6 
;
PROBLEM: Check Calcd Resid. Dens.  0.69Ang From C8              2.71 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C8 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt569_ohpympdmeoh_120k_7 
;
PROBLEM: Check Calcd Resid. Dens.  0.47Ang From C11             2.51 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C11 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt569_ohpympdmeoh_120k 
;
PROBLEM: Check Calcd Resid. Dens.  0.07Ang From O2             -2.84 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O2 atom resulting from the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Tuesday 27 September 2022 04:39 PM
# end Validation Reply Form

_audit_creation_date             2022-09-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 Fe N8 O2 Pd, 0.25(C2 H8 O2)'
_chemical_formula_sum            'C12.50 H8 Fe N8 O2.50 Pd'
_chemical_formula_weight         472.52
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.068(3)
_cell_length_b                   7.1391(2)
_cell_length_c                   14.3733(17)
_cell_angle_alpha                90
_cell_angle_beta                 132.50(2)
_cell_angle_gamma                90
_cell_volume                     1593.9(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4372
_cell_measurement_temperature    119.8(2)
_cell_measurement_theta_max      27.6990
_cell_measurement_theta_min      3.1300
_shelx_estimated_absorpt_T_max   0.941
_shelx_estimated_absorpt_T_min   0.626
_exptl_absorpt_coefficient_mu    2.067
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8274
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.898
_diffrn_reflns_theta_min         3.140
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.8(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -91.00  33.00   1.00    5.00    --  -16.37 -19.00 -90.00  124
  2  ω    -94.00 -39.00   1.00    5.00    --  -16.37-178.00  30.00   55
  3  ω     39.00  95.00   1.00    5.00    --   17.31 178.00   0.00   56
  4  ω     39.00  95.00   1.00    5.00    --   17.31 178.00 -60.00   56
  5  ω    -85.00   5.00   1.00    5.00    --  -16.37 -57.00  60.00   90
  6  ω    -15.00  53.00   1.00    5.00    --   17.31 -99.00  60.00   68
  7  ω    -32.00  92.00   1.00    5.00    --   17.31  19.00 -90.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0139611000
_diffrn_orient_matrix_UB_12      -0.0790611000
_diffrn_orient_matrix_UB_13      0.0396154000
_diffrn_orient_matrix_UB_21      -0.0411779000
_diffrn_orient_matrix_UB_22      -0.0415134000
_diffrn_orient_matrix_UB_23      -0.0461473000
_diffrn_orient_matrix_UB_31      0.0138523000
_diffrn_orient_matrix_UB_32      -0.0435761000
_diffrn_orient_matrix_UB_33      -0.0280452000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1762
_reflns_number_total             1848
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         3.654
_refine_diff_density_min         -2.637
_refine_diff_density_rms         0.309
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1848
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0796
_refine_ls_restrained_S_all      1.156
_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)+(0.0340P)²+137.0227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1917
_refine_ls_wR_factor_ref         0.1936
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C11-O3
 1.43 with sigma of 0.02
 O3-C11
 1.43 with sigma of 0.02
 C2-N2
 1.33 with sigma of 0.001
 N6-C9
 1.33 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(N6) = Uanis(C10) = Uanis(N5) = Uanis(C7) = Uanis(C8) = Uanis(O2) =
Uanis(C9)
Uanis(N1) = Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(N2) = Uanis(C1) =
Uanis(O1)
4. Others
 Fixed Sof: O3(0.25) H3(0.25) C11(0.25) H11A(0.25) H11B(0.25) H11C(0.25)
 Fixed X: O3(0.23312) C11(0.255529)
 Fixed Y: O3(1) C11(1.1861)
 Fixed Z: O3(0.98103) C11(1.00783)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C1(H1), C9(H9), C7(H7), C2(H2)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
5.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd01 Pd 0.51531(6) 0.500000 0.76592(8) 0.0087(3) Uani 1 2 d S T P . .
Fe1 Fe 0.500000 0.000000 0.500000 0.0087(5) Uani 1 4 d S T P . .
Fe2 Fe 0.500000 1.000000 1.000000 0.0087(5) Uani 1 4 d S T P . .
N4 N 0.5166(5) 0.8080(11) 0.9232(7) 0.0134(15) Uani 1 1 d . . . . .
N3 N 0.5077(5) 0.1915(11) 0.6029(7) 0.0178(16) Uani 1 1 d . . . . .
N1 N 0.6283(10) 0.000000 0.6104(15) 0.0376(14) Uani 1 2 d S T P . .
N5 N 0.3740(10) 1.000000 0.8457(15) 0.0382(14) Uani 1 2 d S T P . .
C6 C 0.5181(6) 0.6958(13) 0.8670(8) 0.0137(17) Uani 1 1 d . . . . .
C5 C 0.5095(6) 0.3039(13) 0.6620(8) 0.0167(18) Uani 1 1 d . . . . .
O1 O 0.8059(8) 0.000000 0.6237(12) 0.0376(14) Uani 1 2 d S T P . .
O2 O 0.1649(8) 1.000000 0.7390(12) 0.0382(14) Uani 1 2 d S T P . .
C4 C 0.6679(12) 0.000000 0.5680(18) 0.0376(14) Uani 1 2 d S T P . .
H4 H 0.636606 0.000000 0.480206 0.045 Uiso 1 2 calc R U P . .
C10 C 0.3482(12) 1.000000 0.7293(18) 0.0382(14) Uani 1 2 d S T P . .
H10 H 0.392643 1.000000 0.728004 0.046 Uiso 1 2 calc R U P . .
C1 C 0.6812(12) 0.000000 0.7391(18) 0.0376(14) Uani 1 2 d S T P . .
H1 H 0.651804 0.000000 0.767967 0.045 Uiso 1 2 calc R U P . .
C3 C 0.7626(12) 0.000000 0.6629(18) 0.0376(14) Uani 1 2 d S T P . .
C9 C 0.2082(9) 1.000000 0.6247(15) 0.0382(14) Uani 1 2 d DS T P . .
H9 H 0.149376 1.000000 0.548253 0.046 Uiso 1 2 calc R U P . .
N6 N 0.2679(8) 1.000000 0.6176(13) 0.0382(14) Uani 1 2 d DS T P . .
N2 N 0.7652(8) 0.000000 0.8289(12) 0.0376(14) Uani 1 2 d DS T P . .
O3 O 0.233120 1.000000 0.981030 0.037(6) Uiso 0.25 1 d DS . P A -1
H3 H 0.216624 0.963529 1.017320 0.056 Uiso 0.25 1 calc R U P A -1
C7 C 0.3167(12) 1.000000 0.8555(18) 0.0382(14) Uani 1 2 d S T P . .
H7 H 0.332362 1.000000 0.934838 0.046 Uiso 1 2 calc R U P . .
C2 C 0.8057(9) 0.000000 0.7875(14) 0.0376(14) Uani 1 2 d DS T P . .
H2 H 0.866890 0.000000 0.847297 0.045 Uiso 1 2 calc R U P . .
C8 C 0.2268(12) 1.000000 0.7359(18) 0.0382(14) Uani 1 2 d S T P . .
C11 C 0.255529 1.186100 1.007830 0.036(10) Uiso 0.25 1 d D . P A -1
H11A H 0.274663 1.228716 0.965351 0.053 Uiso 0.25 1 calc R U P A -1
H11B H 0.302327 1.202260 1.099189 0.053 Uiso 0.25 1 calc R U P A -1
H11C H 0.205569 1.259960 0.978050 0.053 Uiso 0.25 1 calc R U P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd01 0.0143(5) 0.0042(4) 0.0110(4) 0.000 0.0100(4) 0.000
Fe1 0.0145(12) 0.0034(10) 0.0105(11) 0.000 0.0094(10) 0.000
Fe2 0.0142(12) 0.0039(11) 0.0105(11) 0.000 0.0093(10) 0.000
N4 0.022(4) 0.009(3) 0.020(4) 0.000(3) 0.019(3) -0.001(3)
N3 0.033(4) 0.008(3) 0.020(4) 0.001(3) 0.021(4) 0.001(3)
N1 0.038(3) 0.035(3) 0.041(3) 0.000 0.027(3) 0.000
N5 0.037(3) 0.027(3) 0.039(3) 0.000 0.021(3) 0.000
C6 0.020(4) 0.009(4) 0.017(4) 0.003(3) 0.014(4) 0.000(3)
C5 0.029(5) 0.008(4) 0.015(4) 0.002(3) 0.016(4) -0.001(4)
O1 0.038(3) 0.035(3) 0.041(3) 0.000 0.027(3) 0.000
O2 0.037(3) 0.027(3) 0.039(3) 0.000 0.021(3) 0.000
C4 0.038(3) 0.035(3) 0.041(3) 0.000 0.027(3) 0.000
C10 0.037(3) 0.027(3) 0.039(3) 0.000 0.021(3) 0.000
C1 0.038(3) 0.035(3) 0.041(3) 0.000 0.027(3) 0.000
C3 0.038(3) 0.035(3) 0.041(3) 0.000 0.027(3) 0.000
C9 0.037(3) 0.027(3) 0.039(3) 0.000 0.021(3) 0.000
N6 0.037(3) 0.027(3) 0.039(3) 0.000 0.021(3) 0.000
N2 0.038(3) 0.035(3) 0.041(3) 0.000 0.027(3) 0.000
C7 0.037(3) 0.027(3) 0.039(3) 0.000 0.021(3) 0.000
C2 0.038(3) 0.035(3) 0.041(3) 0.000 0.027(3) 0.000
C8 0.037(3) 0.027(3) 0.039(3) 0.000 0.021(3) 0.000

_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
Pd01 C6 1.988(9) 6_565 ?
Pd01 C6 1.988(9) . ?
Pd01 C5 1.990(9) 6_565 ?
Pd01 C5 1.990(9) . ?
Fe1 N3 1.938(8) 5_656 ?
Fe1 N3 1.938(8) . ?
Fe1 N3 1.938(8) 2_656 ?
Fe1 N3 1.938(8) 6 ?
Fe1 N1 2.007(16) 5_656 ?
Fe1 N1 2.007(16) . ?
Fe2 N4 1.935(7) 2_657 ?
Fe2 N4 1.935(8) 6_575 ?
Fe2 N4 1.935(7) . ?
Fe2 N4 1.935(7) 5_677 ?
Fe2 N5 2.003(16) 5_677 ?
Fe2 N5 2.003(15) . ?
N4 C6 1.152(12) . ?
N3 C5 1.151(12) . ?
N1 C4 1.32(2) . ?
N1 C1 1.37(2) . ?
N5 C10 1.37(2) . ?
N5 C7 1.30(3) . ?
O1 C3 1.36(2) . ?
O2 C8 1.33(2) . ?
C4 H4 0.9500 . ?
C4 C3 1.47(3) . ?
C10 H10 0.9500 . ?
C10 N6 1.33(2) . ?
C1 H1 0.9500 . ?
C1 N2 1.31(2) . ?
C3 C2 1.35(2) . ?
C9 H9 0.9500 . ?
C9 N6 1.3298(10) . ?
C9 C8 1.36(2) . ?
N2 C2 1.3298(10) . ?
O3 H3 0.8400 . ?
O3 C11 1.37503(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.46(3) . ?
C2 H2 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 Pd01 C6 89.3(5) 6_565 . ?
C6 Pd01 C5 90.6(4) . 6_565 ?
C6 Pd01 C5 178.7(4) 6_565 6_565 ?
C6 Pd01 C5 178.7(4) . . ?
C6 Pd01 C5 90.6(4) 6_565 . ?
C5 Pd01 C5 89.4(5) 6_565 . ?
N3 Fe1 N3 180.0 . 5_656 ?
N3 Fe1 N3 90.3(5) . 2_656 ?
N3 Fe1 N3 90.3(5) 5_656 6 ?
N3 Fe1 N3 180.0 6 2_656 ?
N3 Fe1 N3 89.7(5) 5_656 2_656 ?
N3 Fe1 N3 89.7(5) . 6 ?
N3 Fe1 N1 88.7(4) . 5_656 ?
N3 Fe1 N1 88.7(4) 5_656 . ?
N3 Fe1 N1 91.3(4) 2_656 5_656 ?
N3 Fe1 N1 91.3(4) . . ?
N3 Fe1 N1 88.7(4) 6 5_656 ?
N3 Fe1 N1 88.7(4) 2_656 . ?
N3 Fe1 N1 91.3(4) 5_656 5_656 ?
N3 Fe1 N1 91.3(4) 6 . ?
N1 Fe1 N1 180.0 5_656 . ?
N4 Fe2 N4 90.2(4) 6_575 . ?
N4 Fe2 N4 89.8(4) 5_677 6_575 ?
N4 Fe2 N4 180.0 5_677 . ?
N4 Fe2 N4 90.2(4) 5_677 2_657 ?
N4 Fe2 N4 180.0 6_575 2_657 ?
N4 Fe2 N4 89.8(4) 2_657 . ?
N4 Fe2 N5 90.9(4) 5_677 . ?
N4 Fe2 N5 89.1(4) . . ?
N4 Fe2 N5 89.1(4) 6_575 . ?
N4 Fe2 N5 90.9(4) 6_575 5_677 ?
N4 Fe2 N5 89.1(4) 5_677 5_677 ?
N4 Fe2 N5 90.9(4) 2_657 . ?
N4 Fe2 N5 89.1(4) 2_657 5_677 ?
N4 Fe2 N5 90.9(4) . 5_677 ?
N5 Fe2 N5 180.0 . 5_677 ?
C6 N4 Fe2 173.3(8) . . ?
C5 N3 Fe1 177.7(8) . . ?
C4 N1 Fe1 124.6(13) . . ?
C4 N1 C1 115.5(16) . . ?
C1 N1 Fe1 119.9(13) . . ?
C10 N5 Fe2 119.3(13) . . ?
C7 N5 Fe2 120.7(14) . . ?
C7 N5 C10 120.0(17) . . ?
N4 C6 Pd01 177.5(8) . . ?
N3 C5 Pd01 178.7(9) . . ?
N1 C4 H4 121.5 . . ?
N1 C4 C3 117.0(17) . . ?
C3 C4 H4 121.5 . . ?
N5 C10 H10 116.3 . . ?
N6 C10 N5 127.5(18) . . ?
N6 C10 H10 116.3 . . ?
N1 C1 H1 114.5 . . ?
N2 C1 N1 131.0(17) . . ?
N2 C1 H1 114.5 . . ?
O1 C3 C4 119.0(16) . . ?
C2 C3 O1 120.6(16) . . ?
C2 C3 C4 120.3(16) . . ?
N6 C9 H9 118.3 . . ?
N6 C9 C8 123.5(15) . . ?
C8 C9 H9 118.3 . . ?
C9 N6 C10 113.9(15) . . ?
C1 N2 C2 114.1(14) . . ?
C11 O3 H3 109.5 . . ?
N5 C7 H7 122.2 . . ?
N5 C7 C8 115.5(18) . . ?
C8 C7 H7 122.2 . . ?
C3 C2 H2 119.0 . . ?
N2 C2 C3 122.1(15) . . ?
N2 C2 H2 119.0 . . ?
O2 C8 C9 121.6(16) . . ?
O2 C8 C7 118.7(17) . . ?
C9 C8 C7 119.7(17) . . ?
O3 C11 H11A 109.5 . . ?
O3 C11 H11B 109.5 . . ?
O3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N1 C4 C3 180.000(8) . . . . ?
Fe1 N1 C1 N2 180.000(8) . . . . ?
Fe2 N5 C10 N6 180.000(8) . . . . ?
Fe2 N5 C7 C8 180.000(9) . . . . ?
N1 C4 C3 O1 180.000(8) . . . . ?
N1 C4 C3 C2 0.000(11) . . . . ?
N1 C1 N2 C2 0.000(12) . . . . ?
N5 C10 N6 C9 0.000(9) . . . . ?
N5 C7 C8 O2 180.000(10) . . . . ?
N5 C7 C8 C9 0.000(13) . . . . ?
O1 C3 C2 N2 180.000(10) . . . . ?
C4 N1 C1 N2 0.000(12) . . . . ?
C4 C3 C2 N2 0.000(10) . . . . ?
C10 N5 C7 C8 0.000(14) . . . . ?
C1 N1 C4 C3 0.000(10) . . . . ?
C1 N2 C2 C3 0.000(12) . . . . ?
N6 C9 C8 O2 180.000(8) . . . . ?
N6 C9 C8 C7 0.000(12) . . . . ?
C7 N5 C10 N6 0.000(14) . . . . ?
C8 C9 N6 C10 0.000(9) . . . . ?

_shelx_res_file                  
;
TITL rt569_ohpympdmeoh_120k_a.res in C2/m
    rt569_ohpympdmeoh_120k.res
    created by SHELXL-2018/3 at 16:07:11 on 27-Sep-2022
REM Old TITL RT569_OHPymPdMeOH_120K in C2/m
REM SHELXT solution in C2/m
REM R1 0.147, Rweak 0.017, Alpha 0.078, Orientation as input
REM Formula found by SHELXT: C5 N7 Pd
CELL 0.71073 21.068 7.1391 14.3733 90 132.499 90
ZERR 4 0.0026 0.0002 0.0017 0 0.021 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pd
UNIT 50 32 4 32 10 4
DFIX 1.43 C11 O3
DFIX 1.43 O3 C11
DFIX 1.33 0.001 C2 N2
DFIX 1.33 0.001 N6 C9
EADP N6 C10 N5 C7 C8 O2 C9
EADP N1 C4 C3 C2 N2 C1 O1

L.S. 10
PLAN  2
SIZE 0.25 0.2 0.03
TEMP -153.13
CONF
list 4
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\RT569_OHPymPdMeOH_120K.hkl">
REM </olex2.extras>

WGHT    0.034000  137.022705
FVAR       0.23019
PD01  6    0.515307    0.500000    0.765921    10.50000    0.01427    0.00425 =
         0.01103    0.00000    0.00995    0.00000
FE1   3    0.500000    0.000000    0.500000    10.25000    0.01451    0.00337 =
         0.01048    0.00000    0.00941    0.00000
FE2   3    0.500000    1.000000    1.000000    10.25000    0.01422    0.00389 =
         0.01049    0.00000    0.00934    0.00000
N4    4    0.516650    0.807959    0.923189    11.00000    0.02248    0.00914 =
         0.01992   -0.00011    0.01883   -0.00096
N3    4    0.507719    0.191518    0.602863    11.00000    0.03270    0.00768 =
         0.02025    0.00089    0.02082    0.00086
N1    4    0.628311    0.000000    0.610350    10.50000    0.03788    0.03485 =
         0.04063    0.00000    0.02673    0.00000
N5    4    0.373955    1.000000    0.845677    10.50000    0.03709    0.02708 =
         0.03942    0.00000    0.02144    0.00000
C6    1    0.518134    0.695777    0.867050    11.00000    0.02046    0.00891 =
         0.01655    0.00291    0.01444    0.00020
C5    1    0.509502    0.303880    0.662011    11.00000    0.02890    0.00789 =
         0.01496    0.00206    0.01553   -0.00105
O1    5    0.805875    0.000000    0.623736    10.50000    0.03788    0.03485 =
         0.04063    0.00000    0.02673    0.00000
O2    5    0.164906    1.000000    0.739004    10.50000    0.03709    0.02708 =
         0.03942    0.00000    0.02144    0.00000
C4    1    0.667939    0.000000    0.567995    10.50000    0.03788    0.03485 =
         0.04063    0.00000    0.02673    0.00000
AFIX  43
H4    2    0.636606    0.000000    0.480206    10.50000   -1.20000
AFIX   0
C10   1    0.348155    1.000000    0.729305    10.50000    0.03709    0.02708 =
         0.03942    0.00000    0.02144    0.00000
AFIX  43
H10   2    0.392643    1.000000    0.728004    10.50000   -1.20000
AFIX   0
C1    1    0.681164    0.000000    0.739060    10.50000    0.03788    0.03485 =
         0.04063    0.00000    0.02673    0.00000
AFIX  43
H1    2    0.651804    0.000000    0.767967    10.50000   -1.20000
AFIX   0
C3    1    0.762553    0.000000    0.662883    10.50000    0.03788    0.03485 =
         0.04063    0.00000    0.02673    0.00000
C9    1    0.208167    1.000000    0.624687    10.50000    0.03709    0.02708 =
         0.03942    0.00000    0.02144    0.00000
AFIX  43
H9    2    0.149376    1.000000    0.548253    10.50000   -1.20000
AFIX   0
N6    4    0.267914    1.000000    0.617590    10.50000    0.03709    0.02708 =
         0.03942    0.00000    0.02144    0.00000
N2    4    0.765190    0.000000    0.828888    10.50000    0.03788    0.03485 =
         0.04063    0.00000    0.02673    0.00000

PART -1
O3    5   10.233120   11.000000   10.981030    10.25000    0.03716
AFIX 147
H3    2    0.216624    0.963529    1.017320    10.25000   -1.50000
AFIX   0

PART 0
C7    1    0.316727    1.000000    0.855458    10.50000    0.03709    0.02708 =
         0.03942    0.00000    0.02144    0.00000
AFIX  43
H7    2    0.332362    1.000000    0.934838    10.50000   -1.20000
AFIX   0
C2    1    0.805735    0.000000    0.787550    10.50000    0.03788    0.03485 =
         0.04063    0.00000    0.02673    0.00000
AFIX  43
H2    2    0.866890    0.000000    0.847297    10.50000   -1.20000
AFIX   0
C8    1    0.226819    1.000000    0.735916    10.50000    0.03709    0.02708 =
         0.03942    0.00000    0.02144    0.00000

PART -1
C11   1   10.255529   11.186100   11.007830    10.25000    0.03555
AFIX 137
H11A  2    0.274663    1.228716    0.965351    10.25000   -1.50000
H11B  2    0.302327    1.202260    1.099189    10.25000   -1.50000
H11C  2    0.205569    1.259960    0.978050    10.25000   -1.50000
AFIX   0
HKLF 4




REM  rt569_ohpympdmeoh_120k_a.res in C2/m
REM wR2 = 0.1936, GooF = S = 1.153, Restrained GooF = 1.156 for all data
REM R1 = 0.0796 for 1762 Fo > 4sig(Fo) and 0.0827 for all 1848 data
REM 91 parameters refined using 4 restraints

END

WGHT      0.0337    137.3491

REM Highest difference peak  3.654,  deepest hole -2.637,  1-sigma level  0.309
Q1    1   0.7255  0.0000  0.5714  10.50000  0.05    3.65
Q2    1   0.1926  1.0000  0.5116  10.50000  0.05    3.54
;
_shelx_res_checksum              25657
_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 1.292
_oxdiff_exptl_absorpt_empirical_full_min 0.797
####################################################################### 
# 
# 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_rt475_ohpympt_meoh_160k
_database_code_depnum_ccdc_archive 'CCDC 2209624'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-10-19 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_rt475_ohpympt_meoh_160k 
;
PROBLEM: Check Calcd Resid. Dens.  0.76Ang From Pt1            13.85 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.96Ang From Pt1            12.83 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.19Ang From Pt1             6.82 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_4 
;
PROBLEM: Check Calcd Resid. Dens.  1.11Ang From N1              5.45 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N1 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_5 
;
PROBLEM: Check Calcd Resid. Dens.  0.52Ang From Fe1             5.43 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_6 
;
PROBLEM: Check Calcd Resid. Dens.  0.52Ang From Fe2             4.80 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_7 
;
PROBLEM: Check Calcd Resid. Dens.  0.70Ang From N5              4.28 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k 
;
PROBLEM: Check Calcd Resid. Dens.  1.21Ang From Pt1           -13.04 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.64Ang From Pt1            -7.64 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.41Ang From Pt1            -6.22 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k_4 
;
PROBLEM: Check Calcd Resid. Dens.  0.58Ang From Fe2            -5.56 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k_5 
;
PROBLEM: Check Calcd Resid. Dens.  0.59Ang From Fe1            -5.39 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k_6 
;
PROBLEM: Check Calcd Resid. Dens.  0.93Ang From N5             -3.85 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k_7 
;
PROBLEM: Check Calcd Resid. Dens.  0.16Ang From O2             -3.55 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT973_rt475_ohpympt_meoh_160k 
;
PROBLEM: Check Calcd Positive Resid. Density on       Fe2       3.79 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT973_rt475_ohpympt_meoh_160k_2 
;
PROBLEM: Check Calcd Positive Resid. Density on       Fe1       3.11 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT975_rt475_ohpympt_meoh_160k 
;
PROBLEM: Check Calcd Resid. Dens.  0.89Ang From N2      .       2.80 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT976_rt475_ohpympt_meoh_160k 
;
PROBLEM: Check Calcd Resid. Dens.  0.52Ang From O1      .      -2.28 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_DIFMN02_rt475_ohpympt_meoh_160k 
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00
RESPONSE: This alerts may arise from the strong disorder of the guest in the structural pores as well as from the deterioration of the crystal during the desorption/adsorption events
;
_vrf_PLAT097_rt475_ohpympt_meoh_160k 
;
PROBLEM: Large Reported Max.  (Positive) Residual Density      13.93 eA-3
RESPONSE: This alerts may arise from the strong disorder of the guest in the structural pores as well as from the deterioration of the crystal during the desorption/adsorption events
;
_vrf_PLAT098_rt475_ohpympt_meoh_160k 
;
PROBLEM: Large Reported Min.  (Negative) Residual Density     -12.73 eA-3
RESPONSE: This alerts arises from the strong disorder of the guest in the structural pores
;
_vrf_PLAT342_rt475_ohpympt_meoh_160k 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.095 Ang.
RESPONSE: This alerts arises from the strong disorder of the guest in the structural pores and from a deterioration of the crystal during the desorption readsorption processes
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_8 
;
PROBLEM: Check Calcd Resid. Dens.  1.45Ang From O1              3.45 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O1 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_9 
;
PROBLEM: Check Calcd Resid. Dens.  1.99Ang From O3              3.06 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O3 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_10 
;
PROBLEM: Check Calcd Resid. Dens.  0.78Ang From C3              2.95 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C3 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_11 
;
PROBLEM: Check Calcd Resid. Dens.  0.89Ang From N2              2.80 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_12 
;
PROBLEM: Check Calcd Resid. Dens.  0.94Ang From N2              2.77 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_13 
;
PROBLEM: Check Calcd Resid. Dens.  0.43Ang From C11             2.62 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_14 
;
PROBLEM: Check Calcd Resid. Dens.  1.53Ang From Pt1             2.58 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_160k_15 
;
PROBLEM: Check Calcd Resid. Dens.  1.38Ang From O1              2.52 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k_8 
;
PROBLEM: Check Calcd Resid. Dens.  0.90Ang From N1             -3.12 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k_9 
;
PROBLEM: Check Calcd Resid. Dens.  1.19Ang From N1             -3.09 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k_10 
;
PROBLEM: Check Calcd Resid. Dens.  1.14Ang From C1             -2.72 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C1 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k_11 
;
PROBLEM: Check Calcd Resid. Dens.  0.80Ang From C9             -2.68 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C9 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_160k_12 
;
PROBLEM: Check Calcd Resid. Dens.  1.09Ang From C9             -2.54 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C9 atom resulting from the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Wednesday 19 October 2022 02:14 PM
# end Validation Reply Form

_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 Fe N8 O2 Pt, 0.25(C2 H8 O2)'
_chemical_formula_sum            'C12.50 H8 Fe N8 O2.50 Pt'
_chemical_formula_weight         561.21
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.265(4)
_cell_length_b                   7.2848(3)
_cell_length_c                   15.680(3)
_cell_angle_alpha                90
_cell_angle_beta                 136.70(3)
_cell_angle_gamma                90
_cell_volume                     1665.8(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2108
_cell_measurement_temperature    160.05(10)
_cell_measurement_theta_max      29.3350
_cell_measurement_theta_min      3.7890
_shelx_estimated_absorpt_T_max   0.654
_shelx_estimated_absorpt_T_min   0.336
_exptl_absorpt_coefficient_mu    9.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4093
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.616
_diffrn_reflns_theta_min         3.083
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_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     -2.00  42.00   1.00    5.00    --   22.05  77.00  60.00   44
  2  ω    -23.00  95.00   1.00    5.00    --   22.05  19.00-180.00  118
  3  ω    -22.00  54.00   1.00    5.00    --   22.05 -77.00 -60.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0101439000
_diffrn_orient_matrix_UB_12      0.0948347000
_diffrn_orient_matrix_UB_13      0.0139434000
_diffrn_orient_matrix_UB_21      0.0296319000
_diffrn_orient_matrix_UB_22      -0.0193018000
_diffrn_orient_matrix_UB_23      0.0640340000
_diffrn_orient_matrix_UB_31      0.0372452000
_diffrn_orient_matrix_UB_32      -0.0104915000
_diffrn_orient_matrix_UB_33      0.0081381000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2181
_reflns_number_total             2234
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         13.934
_refine_diff_density_min         -12.731
_refine_diff_density_rms         0.594
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.382
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         2234
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.1139
_refine_ls_restrained_S_all      1.382
_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)+(0.0001P)²+499.0036P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2630
_refine_ls_wR_factor_ref         0.2636
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Fe1) = Uanis(N3) = Uanis(C5) = Uanis(Pt1) = Uanis(C6) = Uanis(N4) =
Uanis(Fe2)
Uanis(N1) = Uanis(C1) = Uanis(N2) = Uanis(C2) = Uanis(C3) = Uanis(C4) =
Uanis(O1)
Uanis(N5) = Uanis(C7) = Uanis(C8) = Uanis(O2) = Uanis(N6) = Uanis(C9) =
Uanis(C10)
3. Others
 Fixed Sof: O3(0.25) H3(0.25) C11(0.25) H11A(0.25) H11B(0.25) H11C(0.25)
 Fixed X: Fe2(1) N4(0.908) O3(0.74218) C11(0.74873)
 Fixed Y: Fe2(2) N4(1.80918) O3(1.5) C11(1.690881)
 Fixed Z: Fe2(1) N4(0.88998) O3(0.50595) C11(0.5004)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C2(H2), C7(H7), C10(H10), C9(H9)
4.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
4.c Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 1.000000 0.500000 0.0110(3) Uani 1 4 d S T P . .
Fe2 Fe 1.000000 2.000000 1.000000 0.0110(3) Uani 1 4 d S T P . .
Pt1 Pt 0.75881(8) 1.500000 0.74048(11) 0.0110(3) Uani 1 2 d S T P . .
N3 N 0.6037(11) 1.201(2) 0.5945(15) 0.0110(3) Uani 1 1 d . . . . .
C5 C 0.6625(13) 1.309(3) 0.6497(17) 0.0110(3) Uani 1 1 d . . . . .
N4 N 0.908000 1.809181 0.889980 0.0110(3) Uani 1 1 d . . . . .
C6 C 0.8549(13) 1.693(3) 0.8351(17) 0.0110(3) Uani 1 1 d . . . . .
N1 N 0.486(2) 1.000000 0.351(3) 0.038(3) Uani 1 2 d S T P . .
C1 C 0.555(3) 1.000000 0.364(4) 0.038(3) Uani 1 2 d S T P . .
H1 H 0.613153 1.000000 0.448396 0.046 Uiso 1 2 calc R U P . .
C4 C 0.403(3) 1.000000 0.226(4) 0.038(3) Uani 1 2 d S T P . .
H4 H 0.347390 1.000000 0.202128 0.046 Uiso 1 2 calc R U P . .
C3 C 0.401(3) 1.000000 0.131(4) 0.038(3) Uani 1 2 d S T P . .
C2 C 0.479(3) 1.000000 0.162(4) 0.038(3) Uani 1 2 d S T P . .
H2 H 0.476180 1.000000 0.098735 0.046 Uiso 1 2 calc R U P . .
N5 N 1.030(2) 2.000000 0.905(3) 0.032(3) Uani 1 2 d S T P . .
C7 C 0.968(3) 2.000000 0.785(3) 0.032(3) Uani 1 2 d S T P . .
H7 H 0.905136 2.000000 0.736252 0.038 Uiso 1 2 calc R U P . .
C10 C 1.120(3) 2.000000 0.967(3) 0.032(3) Uani 1 2 d S T P . .
H10 H 1.165842 2.000000 1.055140 0.038 Uiso 1 2 calc R U P . .
C9 C 1.089(3) 2.000000 0.800(3) 0.032(3) Uani 1 2 d S T P . .
H9 H 1.108001 2.000000 0.759872 0.038 Uiso 1 2 calc R U P . .
N6 N 1.151(2) 2.000000 0.916(3) 0.032(3) Uani 1 2 d S T P . .
O2 O 0.9296(18) 2.000000 0.597(2) 0.032(3) Uani 1 2 d S T P . .
O1 O 0.322(2) 1.000000 0.011(3) 0.038(3) Uani 1 2 d S T P . .
N2 N 0.558(2) 1.000000 0.279(3) 0.038(3) Uani 1 2 d S T P . .
C8 C 0.996(3) 2.000000 0.725(3) 0.032(3) Uani 1 2 d S T P . .
O3 O 0.742180 1.500000 0.505950 0.029(11) Uiso 0.25 1 d S . P A -1
H3 H 0.794424 1.452547 0.552742 0.043 Uiso 0.25 1 calc R U P A -1
C11 C 0.748730 1.690880 0.500400 0.021(16) Uiso 0.25 1 d . . P A -1
H11A H 0.687634 1.745995 0.444749 0.032 Uiso 0.25 1 calc R U P A -1
H11B H 0.774084 1.716223 0.468754 0.032 Uiso 0.25 1 calc R U P A -1
H11C H 0.789035 1.743423 0.583828 0.032 Uiso 0.25 1 calc R U P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0115(5) 0.0068(5) 0.0121(5) 0.000 0.0078(4) 0.000
Fe2 0.0115(5) 0.0068(5) 0.0121(5) 0.000 0.0078(4) 0.000
Pt1 0.0115(5) 0.0068(5) 0.0121(5) 0.000 0.0078(4) 0.000
N3 0.0115(5) 0.0068(5) 0.0121(5) 0.000 0.0078(4) 0.000
C5 0.0115(5) 0.0068(5) 0.0121(5) 0.000 0.0078(4) 0.000
N4 0.0115(5) 0.0068(5) 0.0121(5) 0.000 0.0078(4) 0.000
C6 0.0115(5) 0.0068(5) 0.0121(5) 0.000 0.0078(4) 0.000
N1 0.033(7) 0.045(8) 0.034(7) 0.000 0.024(6) 0.000
C1 0.033(7) 0.045(8) 0.034(7) 0.000 0.024(6) 0.000
C4 0.033(7) 0.045(8) 0.034(7) 0.000 0.024(6) 0.000
C3 0.033(7) 0.045(8) 0.034(7) 0.000 0.024(6) 0.000
C2 0.033(7) 0.045(8) 0.034(7) 0.000 0.024(6) 0.000
N5 0.024(6) 0.033(7) 0.019(6) 0.000 0.009(5) 0.000
C7 0.024(6) 0.033(7) 0.019(6) 0.000 0.009(5) 0.000
C10 0.024(6) 0.033(7) 0.019(6) 0.000 0.009(5) 0.000
C9 0.024(6) 0.033(7) 0.019(6) 0.000 0.009(5) 0.000
N6 0.024(6) 0.033(7) 0.019(6) 0.000 0.009(5) 0.000
O2 0.024(6) 0.033(7) 0.019(6) 0.000 0.009(5) 0.000
O1 0.033(7) 0.045(8) 0.034(7) 0.000 0.024(6) 0.000
N2 0.033(7) 0.045(8) 0.034(7) 0.000 0.024(6) 0.000
C8 0.024(6) 0.033(7) 0.019(6) 0.000 0.009(5) 0.000

_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 N3 2.107(16) 5_676 ?
Fe1 N3 2.107(16) 2_656 ?
Fe1 N3 2.107(16) . ?
Fe1 N3 2.107(16) 6_575 ?
Fe1 N1 2.13(4) 5_676 ?
Fe1 N1 2.13(4) . ?
Fe2 N4 1.9553(7) . ?
Fe2 N4 1.9553(7) 2_757 ?
Fe2 N4 1.9553(7) 6_595 ?
Fe2 N4 1.9553(7) 5_797 ?
Fe2 N5 1.99(3) . ?
Fe2 N5 1.99(3) 5_797 ?
Pt1 C5 1.977(19) 6_585 ?
Pt1 C5 1.977(19) . ?
Pt1 C6 1.987(19) 6_585 ?
Pt1 C6 1.986(19) . ?
N3 C5 1.17(2) . ?
N4 C6 1.146(19) . ?
N1 C1 1.32(5) . ?
N1 C4 1.38(5) . ?
C1 H1 0.9500 . ?
C1 N2 1.39(5) . ?
C4 H4 0.9500 . ?
C4 C3 1.45(6) . ?
C3 C2 1.35(6) . ?
C3 O1 1.33(5) . ?
C2 H2 0.9500 . ?
C2 N2 1.31(5) . ?
N5 C7 1.30(5) . ?
N5 C10 1.39(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.42(6) . ?
C10 H10 0.9500 . ?
C10 N6 1.34(5) . ?
C9 H9 0.9500 . ?
C9 N6 1.26(5) . ?
C9 C8 1.39(5) . ?
O2 C8 1.37(4) . ?
O3 H3 0.8400 . ?
O3 C11 1.40647(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe1 N3 92.1(9) 5_676 6_575 ?
N3 Fe1 N3 180.0 6_575 2_656 ?
N3 Fe1 N3 87.9(9) 5_676 2_656 ?
N3 Fe1 N3 87.8(9) 6_575 . ?
N3 Fe1 N3 180.0 5_676 . ?
N3 Fe1 N3 92.2(9) 2_656 . ?
N3 Fe1 N1 90.7(8) . . ?
N3 Fe1 N1 89.3(8) 2_656 . ?
N3 Fe1 N1 90.7(8) 2_656 5_676 ?
N3 Fe1 N1 89.3(8) 6_575 5_676 ?
N3 Fe1 N1 89.3(8) 5_676 . ?
N3 Fe1 N1 90.7(8) 5_676 5_676 ?
N3 Fe1 N1 89.3(8) . 5_676 ?
N3 Fe1 N1 90.7(8) 6_575 . ?
N1 Fe1 N1 180.0 . 5_676 ?
N4 Fe2 N4 180.0 6_595 2_757 ?
N4 Fe2 N4 180.0 . 5_797 ?
N4 Fe2 N4 89.38(4) . 2_757 ?
N4 Fe2 N4 90.62(4) 5_797 2_757 ?
N4 Fe2 N4 89.38(4) 5_797 6_595 ?
N4 Fe2 N4 90.62(4) . 6_595 ?
N4 Fe2 N5 90.1(6) . 5_797 ?
N4 Fe2 N5 90.0(6) 5_797 . ?
N4 Fe2 N5 90.0(6) 2_757 . ?
N4 Fe2 N5 89.9(6) . . ?
N4 Fe2 N5 90.0(6) 6_595 5_797 ?
N4 Fe2 N5 90.0(6) 6_595 . ?
N4 Fe2 N5 90.0(6) 2_757 5_797 ?
N4 Fe2 N5 90.0(6) 5_797 5_797 ?
N5 Fe2 N5 180.000(10) 5_797 . ?
C5 Pt1 C5 89.3(11) . 6_585 ?
C5 Pt1 C6 90.2(7) . 6_585 ?
C5 Pt1 C6 178.1(8) . . ?
C5 Pt1 C6 90.2(7) 6_585 . ?
C5 Pt1 C6 178.1(8) 6_585 6_585 ?
C6 Pt1 C6 90.3(11) . 6_585 ?
C5 N3 Fe1 178.2(15) . . ?
N3 C5 Pt1 178.0(17) . . ?
C6 N4 Fe2 172.9(9) . . ?
N4 C6 Pt1 177.0(15) . . ?
C1 N1 Fe1 125(3) . . ?
C1 N1 C4 110(4) . . ?
C4 N1 Fe1 125(3) . . ?
N1 C1 H1 113.7 . . ?
N1 C1 N2 133(4) . . ?
N2 C1 H1 113.7 . . ?
N1 C4 H4 119.6 . . ?
N1 C4 C3 121(4) . . ?
C3 C4 H4 119.6 . . ?
C2 C3 C4 121(4) . . ?
O1 C3 C4 121(4) . . ?
O1 C3 C2 118(4) . . ?
C3 C2 H2 120.3 . . ?
N2 C2 C3 119(4) . . ?
N2 C2 H2 120.3 . . ?
C7 N5 Fe2 124(3) . . ?
C7 N5 C10 115(4) . . ?
C10 N5 Fe2 121(2) . . ?
N5 C7 H7 119.8 . . ?
N5 C7 C8 120(4) . . ?
C8 C7 H7 119.8 . . ?
N5 C10 H10 116.1 . . ?
N6 C10 N5 128(3) . . ?
N6 C10 H10 116.1 . . ?
N6 C9 H9 118.1 . . ?
N6 C9 C8 124(4) . . ?
C8 C9 H9 118.1 . . ?
C9 N6 C10 115(3) . . ?
C2 N2 C1 116(4) . . ?
C9 C8 C7 118(3) . . ?
O2 C8 C7 119(3) . . ?
O2 C8 C9 123(4) . . ?
C11 O3 H3 109.5 . . ?
O3 C11 H11A 109.5 . . ?
O3 C11 H11B 109.5 . . ?
O3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N1 C1 N2 180.000(12) . . . . ?
Fe1 N1 C4 C3 180.000(9) . . . . ?
Fe2 N5 C7 C8 180.000(18) . . . . ?
Fe2 N5 C10 N6 180.000(17) . . . . ?
N1 C1 N2 C2 0.000(18) . . . . ?
N1 C4 C3 C2 0.000(11) . . . . ?
N1 C4 C3 O1 180.000(10) . . . . ?
C1 N1 C4 C3 0.000(12) . . . . ?
C4 N1 C1 N2 0.000(19) . . . . ?
C4 C3 C2 N2 0.000(10) . . . . ?
C3 C2 N2 C1 0.000(12) . . . . ?
N5 C7 C8 C9 0.00(3) . . . . ?
N5 C7 C8 O2 180.00(3) . . . . ?
N5 C10 N6 C9 0.00(3) . . . . ?
C7 N5 C10 N6 0.00(3) . . . . ?
C10 N5 C7 C8 0.00(3) . . . . ?
N6 C9 C8 C7 0.00(3) . . . . ?
N6 C9 C8 O2 180.00(3) . . . . ?
O1 C3 C2 N2 180.000(9) . . . . ?
C8 C9 N6 C10 0.00(3) . . . . ?

_shelx_res_file                  
;
TITL rt475_ohpympt_meoh_160k_c.res in C2/m
    rt475_ohpympt_meoh_160k.res
    created by SHELXL-2018/3 at 12:30:35 on 13-Oct-2022
REM Old TITL RT475_OHPymPt_MeOH_160K in C2/m
REM SHELXT solution in C2/m: R1 0.474, Rweak 0.471, Alpha 0.061
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C35 N14 Fe2 Pt
CELL 0.71073 21.2649 7.2848 15.6802 90 136.701 90
ZERR 4 0.0036 0.0003 0.0028 0 0.033 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pt
UNIT 50 32 4 32 10 4
EADP Fe1 N3 C5 Pt1 C6 N4 Fe2
EADP N1 C1 N2 C2 C3 C4 O1
EADP N5 C7 C8 O2 N6 C9 C10

L.S. 10
PLAN  18
SIZE 0.15 0.15 0.05
TEMP -113.13
CONF
LIST 6
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\RT475_OHPymPt_MeOH_160K.hkl">
REM </olex2.extras>

WGHT    0.000100  499.003601
FVAR       0.17853
FE1   3    0.500000    1.000000    0.500000    10.25000    0.01146    0.00682 =
         0.01212    0.00000    0.00776    0.00000
FE2   3   11.000000   12.000000   11.000000    10.25000    0.01146    0.00682 =
         0.01212    0.00000    0.00776    0.00000
PT1   6    0.758807    1.500000    0.740483    10.50000    0.01146    0.00682 =
         0.01212    0.00000    0.00776    0.00000
N3    4    0.603737    1.200689    0.594477    11.00000    0.01146    0.00682 =
         0.01212    0.00000    0.00776    0.00000
C5    1    0.662498    1.309288    0.649669    11.00000    0.01146    0.00682 =
         0.01212    0.00000    0.00776    0.00000
N4    4   10.908000   11.809180   10.889980    11.00000    0.01146    0.00682 =
         0.01212    0.00000    0.00776    0.00000
C6    1    0.854866    1.693338    0.835095    11.00000    0.01146    0.00682 =
         0.01212    0.00000    0.00776    0.00000
N1    4    0.485728    1.000000    0.350682    10.50000    0.03277    0.04538 =
         0.03403    0.00000    0.02375    0.00000
C1    1    0.554554    1.000000    0.364096    10.50000    0.03277    0.04538 =
         0.03403    0.00000    0.02375    0.00000
AFIX  43
H1    2    0.613153    1.000000    0.448396    10.50000   -1.20000
AFIX   0
C4    1    0.403223    1.000000    0.226025    10.50000    0.03277    0.04538 =
         0.03403    0.00000    0.02375    0.00000
AFIX  43
H4    2    0.347390    1.000000    0.202128    10.50000   -1.20000
AFIX   0
C3    1    0.400791    1.000000    0.131491    10.50000    0.03277    0.04538 =
         0.03403    0.00000    0.02375    0.00000
C2    1    0.478919    1.000000    0.161970    10.50000    0.03277    0.04538 =
         0.03403    0.00000    0.02375    0.00000
AFIX  43
H2    2    0.476180    1.000000    0.098735    10.50000   -1.20000
AFIX   0
N5    4    1.029741    2.000000    0.905437    10.50000    0.02352    0.03259 =
         0.01882    0.00000    0.00887    0.00000
C7    1    0.968475    2.000000    0.784614    10.50000    0.02352    0.03259 =
         0.01882    0.00000    0.00887    0.00000
AFIX  43
H7    2    0.905136    2.000000    0.736252    10.50000   -1.20000
AFIX   0
C10   1    1.120217    2.000000    0.966865    10.50000    0.02352    0.03259 =
         0.01882    0.00000    0.00887    0.00000
AFIX  43
H10   2    1.165842    2.000000    1.055140    10.50000   -1.20000
AFIX   0
C9    1    1.089404    2.000000    0.799581    10.50000    0.02352    0.03259 =
         0.01882    0.00000    0.00887    0.00000
AFIX  43
H9    2    1.108001    2.000000    0.759872    10.50000   -1.20000
AFIX   0
N6    4    1.150711    2.000000    0.916469    10.50000    0.02352    0.03259 =
         0.01882    0.00000    0.00887    0.00000
O2    5    0.929597    2.000000    0.597200    10.50000    0.02352    0.03259 =
         0.01882    0.00000    0.00887    0.00000
O1    5    0.321703    1.000000    0.011334    10.50000    0.03277    0.04538 =
         0.03403    0.00000    0.02375    0.00000
N2    4    0.558239    1.000000    0.279272    10.50000    0.03277    0.04538 =
         0.03403    0.00000    0.02375    0.00000
C8    1    0.995788    2.000000    0.724897    10.50000    0.02352    0.03259 =
         0.01882    0.00000    0.00887    0.00000

PART -1
O3    5   10.742180   11.500000   10.505950    10.25000    0.02873
AFIX 147
H3    2    0.794424    1.452547    0.552742    10.25000   -1.50000
AFIX   0
C11   1   10.748730   11.690881   10.500400    10.25000    0.02122
AFIX 137
H11A  2    0.687634    1.745995    0.444749    10.25000   -1.50000
H11B  2    0.774084    1.716223    0.468754    10.25000   -1.50000
H11C  2    0.789035    1.743423    0.583828    10.25000   -1.50000
AFIX   0
HKLF 4




REM  rt475_ohpympt_meoh_160k_c.res in C2/m
REM wR2 = 0.2636, GooF = S = 1.382, Restrained GooF = 1.382 for all data
REM R1 = 0.1139 for 2181 Fo > 4sig(Fo) and 0.1152 for all 2234 data
REM 56 parameters refined using 0 restraints

END

WGHT      0.0001    498.8681

REM Highest difference peak 13.934,  deepest hole-12.731,  1-sigma level  0.594
Q1    1   0.7078  1.5000  0.6897  10.50000  0.05   13.93
Q2    1   0.7711  1.5000  0.8207  10.50000  0.05   13.14
Q3    1   0.7920  1.5000  0.6985  10.50000  0.05    5.55
Q4    1   0.4807  1.0000  0.4473  10.50000  0.05    4.81
Q5    1   1.0219  2.0000  1.0559  10.50000  0.05    4.33
Q6    1   1.0432  2.0000  0.9717  10.50000  0.05    4.03
Q7    1   0.5311  1.0000  0.4494  10.50000  0.05    3.87
Q8    1   0.4415  1.0000  0.1992  10.50000  0.05    2.60
Q9    1   0.5810  1.0000  0.2501  10.50000  0.05    2.40
Q10   1   0.7327  1.5835  0.5008  11.00000  0.05    2.28
Q11   1   1.0601  2.0000  0.8708  10.50000  0.05    2.13
Q12   1   0.5058  1.0000  0.3226  10.50000  0.05    2.10
Q13   1   0.2335  1.0000 -0.1040  10.50000  0.05    2.06
Q14   1   0.2889  1.0000  0.0608  10.50000  0.05    1.93
Q15   1   0.3427  1.0000  0.1218  10.50000  0.05    1.92
Q16   1   0.8267  1.5000  0.6830  10.50000  0.05    1.86
Q17   1   0.6806  1.5000  0.7291  10.50000  0.05    1.85
Q18   1   1.1714  2.0000  0.8616  10.50000  0.05    1.80
;
_shelx_res_checksum              92385
_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 1.348
_oxdiff_exptl_absorpt_empirical_full_min 0.704
####################################################################### 
# 
# 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_rt475_ohpympt_meoh_215k
_database_code_depnum_ccdc_archive 'CCDC 2209625'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-29 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_rt475_ohpympt_meoh_215k 
;
PROBLEM: Check Calcd Resid. Dens.  1.34Ang From Pt1             6.64 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_215k_2 
;
PROBLEM: Check Calcd Resid. Dens.  1.23Ang From Pt1             6.55 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_215k_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.28Ang From Pt1             6.27 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_215k_4 
;
PROBLEM: Check Calcd Resid. Dens.  0.08Ang From N5              4.28 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N5 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_215k_5 
;
PROBLEM: Check Calcd Resid. Dens.  1.18Ang From C9              4.23 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C9 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_215k_6 
;
PROBLEM: Check Calcd Resid. Dens.  1.83Ang From Pt1             3.51 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_215k 
;
PROBLEM: Check Calcd Resid. Dens.  1.17Ang From Pt1           -10.35 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_215k_2 
;
PROBLEM: Check Calcd Resid. Dens.  1.38Ang From Pt1            -3.83 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_215k_3 
;
PROBLEM: Check Calcd Resid. Dens.  0.76Ang From Pt1            -3.73 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_DIFMN02_rt475_ohpympt_meoh_215k 
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00
RESPONSE: This alerts arises from the strong disorder of the guest in the structural pores and from the deterioration of the crystal due to the desorption/readsorption processes
;
_vrf_PLAT098_rt475_ohpympt_meoh_215k 
;
PROBLEM: Large Reported Min.  (Negative) Residual Density      -8.51 eA-3
RESPONSE: This alerts arises from the strong disorder of the guest in the structural pores and from the deterioration of the crystal due to the desorption/readsorption processes
;
_vrf_PLAT342_rt475_ohpympt_meoh_215k 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0675 Ang.
RESPONSE: This alerts arises from the strong disorder of the guest in the structural pores and from the deterioration of the crystal due to the desorption/readsorption processes
;
_vrf_PLAT430_rt475_ohpympt_meoh_215k 
;
PROBLEM: Short Inter D...A Contact  O2       ..O3       .       2.82 Ang.
RESPONSE: There is a certain number of H-bonds which are properly discussed in the paper. This alert arises from the absence of H atoms which are not present due to the strong agitation of the molecular moieties involved in the H-bond interactions
;
_vrf_PLAT971_rt475_ohpympt_meoh_215k_7 
;
PROBLEM: Check Calcd Resid. Dens.  1.04Ang From N5              3.29 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N5 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_215k_8 
;
PROBLEM: Check Calcd Resid. Dens.  1.15Ang From Fe1             3.01 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Fe metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_215k_9 
;
PROBLEM: Check Calcd Resid. Dens.  0.74Ang From Pt1             2.97 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_215k_10 
;
PROBLEM: Check Calcd Resid. Dens.  0.79Ang From O3              2.89 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O3 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_215k_11 
;
PROBLEM: Check Calcd Resid. Dens.  0.08Ang From N1              2.56 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N1 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_215k_4 
;
PROBLEM: Check Calcd Resid. Dens.  1.50Ang From Pt1            -3.47 eA-3
RESPONSE: The residual electronic density may be due to the strong absorption of the Pt metal and the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_215k_5 
;
PROBLEM: Check Calcd Resid. Dens.  1.65Ang From O1             -3.46 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_215k_6 
;
PROBLEM: Check Calcd Resid. Dens.  0.17Ang From O1             -3.03 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_215k_7 
;
PROBLEM: Check Calcd Resid. Dens.  1.41Ang From N2             -2.96 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_215k_8 
;
PROBLEM: Check Calcd Resid. Dens.  0.22Ang From C2             -2.71 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT975_rt475_ohpympt_meoh_215k 
;
PROBLEM: Check Calcd Resid. Dens.  0.48Ang From C11     .       1.88 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C11 atom resulting from the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Thursday 29 September 2022 02:44 PM
# end Validation Reply Form

_audit_creation_date             2022-09-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 Fe N8 O2 Pt, 0.25(C2 O2)'
_chemical_formula_sum            'C12.50 H6 Fe N8 O2.50 Pt'
_chemical_formula_weight         559.19
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.567(2)
_cell_length_b                   7.3471(2)
_cell_length_c                   14.6537(14)
_cell_angle_alpha                90
_cell_angle_beta                 132.689(16)
_cell_angle_gamma                90
_cell_volume                     1706.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3696
_cell_measurement_temperature    215.00(10)
_cell_measurement_theta_max      29.5650
_cell_measurement_theta_min      3.7730
_shelx_estimated_absorpt_T_max   0.660
_shelx_estimated_absorpt_T_min   0.343
_exptl_absorpt_coefficient_mu    9.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6019
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.682
_diffrn_reflns_theta_min         3.056
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      215.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -94.00   6.00   1.00    5.00    --  -20.96 -38.00 120.00  100
  2  ω    -10.00  42.00   1.00    5.00    --   21.90  77.00  90.00   52
  3  ω    -28.00  96.00   1.00    5.00    --   21.90  19.00 -30.00  124
  4  ω    -15.00  44.00   1.00    5.00    --   21.90 -99.00-120.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0041739000
_diffrn_orient_matrix_UB_12      -0.0937861000
_diffrn_orient_matrix_UB_13      0.0146027000
_diffrn_orient_matrix_UB_21      0.0339206000
_diffrn_orient_matrix_UB_22      0.0202551000
_diffrn_orient_matrix_UB_23      0.0637770000
_diffrn_orient_matrix_UB_31      -0.0289131000
_diffrn_orient_matrix_UB_32      0.0102237000
_diffrn_orient_matrix_UB_33      0.0077317000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2225
_reflns_number_total             2257
_reflns_odcompleteness_completeness 96.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         6.217
_refine_diff_density_min         -8.508
_refine_diff_density_rms         0.396
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.460
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         2257
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0802
_refine_ls_restrained_S_all      1.460
_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)+225.2493P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2021
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N6-C9
 1.4 with sigma of 0.02
 C3-O1
 1.1 with sigma of 0.002
 N2-C2
 1.33 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C1) = Uanis(N2) = Uanis(C2) = Uanis(C3) = Uanis(C4) =
Uanis(O1) = Uanis(O2) = Uanis(C8) = Uanis(C9) = Uanis(N6) = Uanis(C10) =
Uanis(N5) = Uanis(C7)
4. Others
 Fixed Sof: O3(0.25) C11(0.25)
 Fixed X: N2(0.77596) O3(0.73382) C11(0.745749)
 Fixed Y: N2(1) O3(0.5) C11(0.31439)
 Fixed Z: N2(0.722509) O3(0.48813) C11(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C1(H1), C10(H10), C7(H7), C9(H9), C2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.51776(5) 0.500000 0.26443(8) 0.0160(2) Uani 1 2 d S T P . .
Fe2 Fe 0.500000 0.000000 0.000000 0.0110(7) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 1.000000 0.500000 0.0151(8) Uani 1 4 d S T P . .
N5 N 0.6334(19) 0.000000 0.100(3) 0.060(2) Uani 1 2 d S T P . .
N3 N 0.5097(11) 0.799(2) 0.4077(16) 0.034(4) Uani 1 1 d . . . . .
C6 C 0.5187(10) 0.309(2) 0.1693(14) 0.022(3) Uani 1 1 d . . . . .
N4 N 0.5184(10) 0.1966(19) 0.1150(12) 0.027(3) Uani 1 1 d . . . . .
C5 C 0.5124(11) 0.689(2) 0.3543(16) 0.023(3) Uani 1 1 d . . . . .
N1 N 0.6364(19) 1.000000 0.658(3) 0.060(2) Uani 1 2 d S T P . .
C3 C 0.771(2) 1.000000 0.882(2) 0.060(2) Uani 1 2 d DS T P . .
O1 O 0.8077(15) 1.000000 0.983(2) 0.060(2) Uani 1 2 d DS T P . .
C4 C 0.676(2) 1.000000 0.778(4) 0.060(2) Uani 1 2 d S T P . .
H4 H 0.643408 1.000000 0.798546 0.072 Uiso 1 2 calc R U P . .
C1 C 0.688(2) 1.000000 0.633(4) 0.060(2) Uani 1 2 d S T P . .
H1 H 0.661758 1.000000 0.549228 0.072 Uiso 1 2 calc R U P . .
N6 N 0.7334(18) 0.000000 0.083(2) 0.060(2) Uani 1 2 d DS T P . .
C10 C 0.654(2) 0.000000 0.030(4) 0.060(2) Uani 1 2 d S T P . .
H10 H 0.610514 0.000000 -0.057360 0.072 Uiso 1 2 calc R U P . .
C8 C 0.774(2) 0.000000 0.282(4) 0.060(2) Uani 1 2 d S T P . .
C7 C 0.687(2) 0.000000 0.218(4) 0.060(2) Uani 1 2 d S T P . .
H7 H 0.669833 0.000000 0.261663 0.072 Uiso 1 2 calc R U P . .
N2 N 0.775960 1.000000 0.722509 0.060(2) Uani 1 2 d DS T P . .
C9 C 0.796(2) 0.000000 0.210(3) 0.060(2) Uani 1 2 d DS T P . .
H9 H 0.852631 0.000000 0.248586 0.072 Uiso 1 2 calc R U P . .
O2 O 0.8312(16) 0.000000 0.398(2) 0.060(2) Uani 1 2 d S T P . .
O3 O 0.733820 0.500000 0.488130 0.057(13) Uiso 0.25 1 d S . P A -1
C11 C 0.745749 0.314390 0.500000 0.032(15) Uiso 0.25 1 d . . P A -1
C2 C 0.814(2) 1.000000 0.8412(9) 0.060(2) Uani 1 2 d DS T P . .
H2 H 0.872954 1.000000 0.901574 0.072 Uiso 1 2 calc R U P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0182(4) 0.0085(3) 0.0198(4) 0.000 0.0123(3) 0.000
Fe2 0.0157(18) 0.0102(17) 0.0159(18) 0.000 0.0143(16) 0.000
Fe1 0.0147(19) 0.0104(18) 0.024(2) 0.000 0.0145(17) 0.000
N5 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
N3 0.051(10) 0.017(7) 0.054(10) 0.000(7) 0.044(9) 0.004(6)
C6 0.029(8) 0.015(7) 0.016(7) 0.005(6) 0.012(6) 0.002(6)
N4 0.043(8) 0.019(7) 0.018(6) -0.001(5) 0.020(6) -0.002(6)
C5 0.031(8) 0.017(7) 0.035(9) 0.002(6) 0.028(8) -0.001(6)
N1 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
C3 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
O1 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
C4 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
C1 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
N6 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
C10 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
C8 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
C7 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
N2 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
C9 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
O2 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000
C2 0.051(5) 0.055(5) 0.052(5) 0.000 0.027(4) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C6 1.990(16) . ?
Pt1 C6 1.990(16) 6_565 ?
Pt1 C5 1.972(16) 6_565 ?
Pt1 C5 1.972(16) . ?
Fe2 N5 2.17(3) . ?
Fe2 N5 2.17(3) 5_655 ?
Fe2 N4 2.043(14) 2_655 ?
Fe2 N4 2.043(14) . ?
Fe2 N4 2.043(14) 6 ?
Fe2 N4 2.043(14) 5_655 ?
Fe1 N3 2.104(15) 6_575 ?
Fe1 N3 2.104(15) 2_656 ?
Fe1 N3 2.104(15) . ?
Fe1 N3 2.104(15) 5_676 ?
Fe1 N1 2.18(3) 5_676 ?
Fe1 N1 2.18(3) . ?
N5 C10 1.36(5) . ?
N5 C7 1.27(5) . ?
N3 C5 1.15(2) . ?
C6 N4 1.14(2) . ?
N1 C4 1.34(5) . ?
N1 C1 1.39(5) . ?
C3 O1 1.100(2) . ?
C3 C4 1.51(5) . ?
C3 C2 1.40(5) . ?
C4 H4 0.9400 . ?
C1 H1 0.9400 . ?
C1 N2 1.39(4) . ?
N6 C10 1.32(5) . ?
N6 C9 1.369(19) . ?
C10 H10 0.9400 . ?
C8 C7 1.41(5) . ?
C8 C9 1.42(6) . ?
C8 O2 1.25(4) . ?
C7 H7 0.9400 . ?
N2 C2 1.3300(11) . ?
C9 H9 0.9400 . ?
O3 C11 1.37674(4) . ?
O3 C11 2.33579(6) 4_656 ?
C2 H2 0.9400 . ?

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
C6 Pt1 C6 89.9(9) 6_565 . ?
C5 Pt1 C6 90.2(6) 6_565 . ?
C5 Pt1 C6 90.2(6) . 6_565 ?
C5 Pt1 C6 178.0(7) . . ?
C5 Pt1 C6 178.0(7) 6_565 6_565 ?
C5 Pt1 C5 89.8(9) 6_565 . ?
N5 Fe2 N5 180.0 5_655 . ?
N4 Fe2 N5 89.0(8) 6 5_655 ?
N4 Fe2 N5 89.0(8) . 5_655 ?
N4 Fe2 N5 89.0(8) 2_655 . ?
N4 Fe2 N5 91.0(8) 6 . ?
N4 Fe2 N5 91.0(8) 5_655 5_655 ?
N4 Fe2 N5 91.0(8) 2_655 5_655 ?
N4 Fe2 N5 91.0(8) . . ?
N4 Fe2 N5 89.0(8) 5_655 . ?
N4 Fe2 N4 180.0 5_655 . ?
N4 Fe2 N4 90.0(8) 5_655 2_655 ?
N4 Fe2 N4 90.0(8) 2_655 . ?
N4 Fe2 N4 180.0(8) 6 2_655 ?
N4 Fe2 N4 90.0(8) 6 . ?
N4 Fe2 N4 90.0(8) 5_655 6 ?
N3 Fe1 N3 88.9(9) 5_676 2_656 ?
N3 Fe1 N3 91.1(9) 5_676 6_575 ?
N3 Fe1 N3 180.0 6_575 2_656 ?
N3 Fe1 N3 180.0 5_676 . ?
N3 Fe1 N3 88.9(9) 6_575 . ?
N3 Fe1 N3 91.1(9) 2_656 . ?
N3 Fe1 N1 88.2(8) 6_575 5_676 ?
N3 Fe1 N1 88.3(8) 2_656 . ?
N3 Fe1 N1 91.8(8) 2_656 5_676 ?
N3 Fe1 N1 88.2(8) . 5_676 ?
N3 Fe1 N1 91.7(8) . . ?
N3 Fe1 N1 91.7(8) 6_575 . ?
N3 Fe1 N1 88.3(8) 5_676 . ?
N3 Fe1 N1 91.8(8) 5_676 5_676 ?
N1 Fe1 N1 180.0 . 5_676 ?
C10 N5 Fe2 117(2) . . ?
C7 N5 Fe2 119(3) . . ?
C7 N5 C10 124(4) . . ?
C5 N3 Fe1 178.0(17) . . ?
N4 C6 Pt1 178.6(16) . . ?
C6 N4 Fe2 172.1(15) . . ?
N3 C5 Pt1 179.5(14) . . ?
C4 N1 Fe1 127(3) . . ?
C4 N1 C1 116(3) . . ?
C1 N1 Fe1 118(3) . . ?
O1 C3 C4 127(4) . . ?
O1 C3 C2 119(3) . . ?
C2 C3 C4 113(2) . . ?
N1 C4 C3 124(4) . . ?
N1 C4 H4 118.2 . . ?
C3 C4 H4 118.2 . . ?
N1 C1 H1 117.4 . . ?
N1 C1 N2 125(3) . . ?
N2 C1 H1 117.4 . . ?
C10 N6 C9 119(4) . . ?
N5 C10 H10 119.6 . . ?
N6 C10 N5 121(3) . . ?
N6 C10 H10 119.6 . . ?
C7 C8 C9 117(3) . . ?
O2 C8 C7 123(4) . . ?
O2 C8 C9 120(4) . . ?
N5 C7 C8 119(4) . . ?
N5 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
C2 N2 C1 118(2) . . ?
N6 C9 C8 120(4) . . ?
N6 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C11 O3 C11 163.833(4) . 4_656 ?
C3 C2 H2 117.8 . . ?
N2 C2 C3 124(3) . . ?
N2 C2 H2 117.8 . . ?

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
Fe2 N5 C10 N6 180.000(2) . . . . ?
Fe2 N5 C7 C8 180.000(6) . . . . ?
Fe1 N1 C4 C3 180.000(15) . . . . ?
Fe1 N1 C1 N2 180.000(5) . . . . ?
N1 C1 N2 C2 0.000(18) . . . . ?
O1 C3 C4 N1 180.00(2) . . . . ?
O1 C3 C2 N2 180.000(19) . . . . ?
C4 N1 C1 N2 0.000(19) . . . . ?
C4 C3 C2 N2 0.000(15) . . . . ?
C1 N1 C4 C3 0.00(2) . . . . ?
C1 N2 C2 C3 0.000(17) . . . . ?
C10 N5 C7 C8 0.000(6) . . . . ?
C10 N6 C9 C8 0.000(6) . . . . ?
C7 N5 C10 N6 0.000(4) . . . . ?
C7 C8 C9 N6 0.000(6) . . . . ?
C9 N6 C10 N5 0.000(4) . . . . ?
C9 C8 C7 N5 0.000(7) . . . . ?
O2 C8 C7 N5 180.000(10) . . . . ?
O2 C8 C9 N6 180.000(9) . . . . ?
C2 C3 C4 N1 0.00(2) . . . . ?

_shelx_res_file                  
;
TITL rt475_ohpympt_meoh_215k_a.res in C2/m
    rt475_ohpympt_meoh_215k.res
    created by SHELXL-2018/3 at 15:37:39 on 29-Sep-2022
REM Old TITL RT475_OHPymPt_MeOH_215K in C2/m
REM SHELXT solution in C2/m: R1 0.109, Rweak 0.052, Alpha 0.028
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C9 N2 Fe Pt
CELL 0.71073 21.5671 7.3471 14.6537 90 132.689 90
ZERR 4 0.0021 0.0002 0.0014 0 0.016 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pt
UNIT 50 24 4 32 10 4
EQIV $1 1.5-X,0.5+Y,1-Z
DFIX 1.4 N6 C9
DFIX 1.1 0.002 C3 O1
DFIX 1.33 0.001 N2 C2
EADP N1 C1 N2 C2 C3 C4 O1 O2 C8 C9 N6 C10 N5 C7

L.S. 10
PLAN  15
SIZE 0.15 0.15 0.05
TEMP -58.1
CONF
BIND O3 C11_$1
list 4
MORE -1
BOND $H
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\RT475_OHPymPt_MeOH_215K.hkl">
REM </olex2.extras>

WGHT    0.000000  225.249298
FVAR       0.17986
PT1   6    0.517763    0.500000    0.264434    10.50000    0.01821    0.00853 =
         0.01980    0.00000    0.01229    0.00000
FE2   3    0.500000    0.000000    0.000000    10.25000    0.01572    0.01021 =
         0.01592    0.00000    0.01425    0.00000
FE1   3    0.500000    1.000000    0.500000    10.25000    0.01470    0.01043 =
         0.02383    0.00000    0.01450    0.00000
N5    4    0.633381    0.000000    0.099659    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
N3    4    0.509686    0.799340    0.407718    11.00000    0.05080    0.01728 =
         0.05442   -0.00046    0.04434    0.00395
C6    1    0.518738    0.308725    0.169286    11.00000    0.02860    0.01471 =
         0.01578    0.00488    0.01211    0.00163
N4    4    0.518379    0.196586    0.114962    11.00000    0.04314    0.01873 =
         0.01774   -0.00112    0.02040   -0.00216
C5    1    0.512445    0.689382    0.354306    11.00000    0.03084    0.01699 =
         0.03476    0.00166    0.02757   -0.00076
N1    4    0.636364    1.000000    0.657653    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
C3    1    0.771103    1.000000    0.882310    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
O1    5    0.807685    1.000000    0.982642    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
C4    1    0.676236    1.000000    0.777884    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
AFIX  43
H4    2    0.643408    1.000000    0.798546    10.50000   -1.20000
AFIX   0
C1    1    0.688055    1.000000    0.632963    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
AFIX  43
H1    2    0.661758    1.000000    0.549228    10.50000   -1.20000
AFIX   0
N6    4    0.733388    0.000000    0.082643    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
C10   1    0.653686    0.000000    0.029694    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
AFIX  43
H10   2    0.610514    0.000000   -0.057360    10.50000   -1.20000
AFIX   0
C8    1    0.774052    0.000000    0.282319    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
C7    1    0.687416    0.000000    0.217946    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
AFIX  43
H7    2    0.669833    0.000000    0.261663    10.50000   -1.20000
AFIX   0
N2    4   10.775960   11.000000   10.722509    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
C9    1    0.795664    0.000000    0.209537    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
AFIX  43
H9    2    0.852631    0.000000    0.248586    10.50000   -1.20000
AFIX   0
O2    5    0.831151    0.000000    0.398403    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000

PART -1
O3    5   10.733820   10.500000   10.488130    10.25000    0.05693
C11   1   10.745749   10.314390   10.500000    10.25000    0.03211

PART 0
C2    1    0.813668    1.000000    0.841213    10.50000    0.05138    0.05469 =
         0.05183    0.00000    0.02664    0.00000
AFIX  43
H2    2    0.872954    1.000000    0.901574    10.50000   -1.20000
AFIX   0
HKLF 4




REM  rt475_ohpympt_meoh_215k_a.res in C2/m
REM wR2 = 0.2021, GooF = S = 1.460, Restrained GooF = 1.460 for all data
REM R1 = 0.0802 for 2225 Fo > 4sig(Fo) and 0.0806 for all 2257 data
REM 83 parameters refined using 3 restraints

END

WGHT      0.0000    225.0887

REM Highest difference peak  6.217,  deepest hole -8.508,  1-sigma level  0.396
Q1    1   0.4402  0.5000  0.1579  10.50000  0.05    6.22
Q2    1   0.5845  0.5000  0.3214  10.50000  0.05    4.77
Q3    1   0.4503  0.5000  0.2497  10.50000  0.05    4.70
Q4    1   0.8121  0.0000  0.1497  10.50000  0.05    3.20
Q5    1   0.5718  0.0000  0.0634  10.50000  0.05    2.85
Q6    1   0.5089  0.5000  0.3042  10.50000  0.05    2.64
Q7    1   0.5721  1.0000  0.5549  10.50000  0.05    2.62
Q8    1   0.8353  1.0000  0.7711  10.50000  0.05    2.42
Q9    1   0.7275  1.0000  0.8872  10.50000  0.05    2.26
Q10   1   0.5324  1.0000  0.4926  10.50000  0.05    2.08
Q11   1   0.7596  0.0000  0.3342  10.50000  0.05    1.96
Q12   1   0.6830  0.0000  0.0908  10.50000  0.05    1.92
Q13   1   0.7324  0.4025  0.4880  11.00000  0.05    1.92
Q14   1   0.7209  0.5000  0.4220  10.50000  0.05    1.77
Q15   1   0.8189  0.0000  0.3101  10.50000  0.05    1.65
;
_shelx_res_checksum              61268
_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 1.519
_oxdiff_exptl_absorpt_empirical_full_min 0.787
####################################################################### 
# 
# 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_rt590_ohpymptetoh_260k
_database_code_depnum_ccdc_archive 'CCDC 2209623'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-26 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT342_rt590_ohpymptetoh_260k 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0475 Ang.
RESPONSE: This alert is related to the inherent loss of diffraction quality at elevate temperatures and HS states and to the deterioration of the crystal as a result of the desolvation-resolvation processes 
;
_vrf_PLAT430_rt590_ohpymptetoh_260k 
;
PROBLEM: Short Inter D...A Contact  O3       ..N2       .       2.59 Ang.
RESPONSE: There is a certain number of H-bonds which are properly discussed in the paper. This alert arises from the absence of H atoms which are not present due to the strong agitation of the molecular moieties involved in the H-bond interactions
;
_vrf_PLAT971_rt590_ohpymptetoh_260k 
;
PROBLEM: Check Calcd Resid. Dens.  0.08Ang From N5              2.85 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt590_ohpymptetoh_260k_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.06Ang From N1              2.77 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N1 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt590_ohpymptetoh_260k_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.12Ang From C3              2.62 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C3 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt590_ohpymptetoh_260k 
;
PROBLEM: Check Calcd Resid. Dens.  0.29Ang From O2             -2.95 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Monday 26 September 2022 03:56 PM
# end Validation Reply Form

_audit_creation_date             2022-09-26
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H6 Fe N8 O2 Pt, C O0.5'
_chemical_formula_sum            'C13 H6 Fe N8 O2.50 Pt'
_chemical_formula_weight         565.20
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'colourlesstablet 0.32 0.12 0.06'
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'
Pt Pt -1.7033 8.3905 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.724(2)
_cell_length_b                   7.4168(2)
_cell_length_c                   14.7576(16)
_cell_angle_alpha                90
_cell_angle_beta                 132.570(18)
_cell_angle_gamma                90
_cell_volume                     1751.1(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3412
_cell_measurement_temperature    259.95(10)
_cell_measurement_theta_max      26.9880
_cell_measurement_theta_min      3.7410
_shelx_estimated_absorpt_T_max   0.666
_shelx_estimated_absorpt_T_min   0.271
_exptl_absorpt_coefficient_mu    8.836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10883
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.843
_diffrn_reflns_theta_min         3.027
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      259.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00   5.00   1.00    4.00    --  -16.21 -57.00 -60.00   90
  2  ω    -57.00  67.00   1.00    4.00    --   17.15 -19.00-120.00  124
  3  ω    -52.00  39.00   1.00    4.00    --   17.15 -57.00-150.00   91
  4  ω    -42.00  15.00   1.00    4.00    --  -16.21 -77.00-180.00   57
  5  ω    -42.00  15.00   1.00    4.00    --  -16.21 -77.00 120.00   57
  6  ω    -44.00  56.00   1.00    4.00    --  -16.21  38.00  90.00  100
  7  ω    -14.00  42.00   1.00    4.00    --   17.15  77.00  90.00   56
  8  ω     37.00  75.00   1.00    4.00    --   17.15-178.00-120.00   38
  9  ω     39.00  95.00   1.00    4.00    --   17.15 178.00-180.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0195042000
_diffrn_orient_matrix_UB_12      -0.0245635000
_diffrn_orient_matrix_UB_13      -0.0219259000
_diffrn_orient_matrix_UB_21      0.0394207000
_diffrn_orient_matrix_UB_22      0.0248795000
_diffrn_orient_matrix_UB_23      0.0573771000
_diffrn_orient_matrix_UB_31      0.0056379000
_diffrn_orient_matrix_UB_32      -0.0890126000
_diffrn_orient_matrix_UB_33      0.0220853000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1825
_reflns_number_total             2051
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.858
_refine_diff_density_min         -2.875
_refine_diff_density_rms         0.281
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         2051
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0521
_refine_ls_restrained_S_all      1.150
_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)+(0.0562P)²+54.6021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1349
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O3-C11
 1.35 with sigma of 0.02
 C3-C4
 1.4 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(N6) = Uanis(C10) = Uanis(N5) = Uanis(C7) = Uanis(C8) =
Uanis(O2)
Uanis(C2) = Uanis(C3) = Uanis(O1) = Uanis(C4) = Uanis(N1) = Uanis(C1) =
Uanis(N2)
4. Others
 Fixed Sof: O3(0.25) C11(0.5)
 Fixed X: N1(0.3599) C10(0.34012) C9(0.21146) C1(0.316) C2(0.193501)
 N2(0.239599)
 Fixed Y: N1(0) C10(1) C9(1) C1(0) C2(0) N2(0)
 Fixed Z: N1(0.34206) C10(0.96515) C9(0.81286) C1(0.3827) C2(0.186399)
 N2(0.318301)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10), C9(H9), C7(H7), C1(H1), C2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.48382(3) 0.500000 0.73451(5) 0.0222(2) Uani 1 2 d S T P . .
Fe2 Fe 0.500000 1.000000 1.000000 0.0224(6) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.000000 0.500000 0.0232(6) Uani 1 4 d S T P . .
C6 C 0.4825(7) 0.6888(13) 0.8278(9) 0.029(2) Uani 1 1 d . . . . .
N3 N 0.4895(7) 0.2023(13) 0.5913(9) 0.043(2) Uani 1 1 d . . . . .
N4 N 0.4822(7) 0.7968(13) 0.8823(8) 0.041(2) Uani 1 1 d . . . . .
C5 C 0.4872(7) 0.3096(13) 0.6437(10) 0.031(2) Uani 1 1 d . . . . .
N5 N 0.3646(13) 1.000000 0.899(2) 0.096(3) Uani 1 2 d S T P . .
N1 N 0.359900 0.000000 0.342060 0.103(4) Uani 1 2 d S T P . .
C3 C 0.2338(11) 0.000000 0.141(3) 0.103(4) Uani 1 2 d DS T P . .
C4 C 0.3212(11) 0.000000 0.224(3) 0.103(4) Uani 1 2 d DS T P . .
H4 H 0.350171 0.000000 0.198475 0.124 Uiso 1 2 calc R U P . .
N6 N 0.2607(13) 1.000000 0.913(2) 0.096(3) Uani 1 2 d S T P . .
O2 O 0.1652(11) 1.000000 0.6143(18) 0.096(3) Uani 1 2 d S T P . .
O1 O 0.1938(12) 0.000000 0.028(2) 0.103(4) Uani 1 2 d S T P . .
C8 C 0.2209(17) 1.000000 0.721(3) 0.096(3) Uani 1 2 d S T P . .
C10 C 0.340120 1.000000 0.965150 0.096(3) Uani 1 2 d S T P . .
H10 H 0.381474 1.000000 1.050620 0.116 Uiso 1 2 calc R U P . .
C9 C 0.211460 1.000000 0.812860 0.096(3) Uani 1 2 d S T P . .
H9 H 0.156965 1.000000 0.780524 0.116 Uiso 1 2 calc R U P . .
C7 C 0.3078(16) 1.000000 0.777(3) 0.096(3) Uani 1 2 d S T P . .
H7 H 0.322278 1.000000 0.730308 0.116 Uiso 1 2 calc R U P . .
O3 O 0.234(3) 0.000000 0.488(4) 0.108(13) Uiso 0.5 2 d DS . P . .
C11 C 0.229(4) -0.178(3) 0.485(7) 0.16(2) Uiso 0.5 1 d D . P . .
C1 C 0.316000 0.000000 0.382700 0.103(4) Uani 1 2 d S T P . .
H1 H 0.348757 0.000000 0.467380 0.124 Uiso 1 2 calc R U P . .
C2 C 0.193501 0.000000 0.186399 0.103(4) Uani 1 2 d S T P . .
H2 H 0.135392 0.000000 0.130240 0.124 Uiso 1 2 calc R U P . .
N2 N 0.239599 0.000000 0.318301 0.103(4) Uani 1 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0340(3) 0.0141(3) 0.0257(3) 0.000 0.0231(3) 0.000
Fe2 0.0381(16) 0.0117(12) 0.0260(13) 0.000 0.0251(13) 0.000
Fe1 0.0397(16) 0.0125(12) 0.0281(14) 0.000 0.0272(13) 0.000
C6 0.048(6) 0.018(5) 0.027(5) 0.002(4) 0.028(5) 0.000(4)
N3 0.073(7) 0.026(5) 0.060(6) -0.005(5) 0.057(6) 0.001(5)
N4 0.073(7) 0.025(5) 0.036(5) -0.003(4) 0.042(5) 0.000(4)
C5 0.052(6) 0.017(5) 0.045(6) 0.002(4) 0.042(6) 0.002(4)
N5 0.064(6) 0.072(6) 0.104(8) 0.000 0.037(5) 0.000
N1 0.071(6) 0.082(6) 0.122(8) 0.000 0.051(6) 0.000
C3 0.071(6) 0.082(6) 0.122(8) 0.000 0.051(6) 0.000
C4 0.071(6) 0.082(6) 0.122(8) 0.000 0.051(6) 0.000
N6 0.064(6) 0.072(6) 0.104(8) 0.000 0.037(5) 0.000
O2 0.064(6) 0.072(6) 0.104(8) 0.000 0.037(5) 0.000
O1 0.071(6) 0.082(6) 0.122(8) 0.000 0.051(6) 0.000
C8 0.064(6) 0.072(6) 0.104(8) 0.000 0.037(5) 0.000
C10 0.064(6) 0.072(6) 0.104(8) 0.000 0.037(5) 0.000
C9 0.064(6) 0.072(6) 0.104(8) 0.000 0.037(5) 0.000
C7 0.064(6) 0.072(6) 0.104(8) 0.000 0.037(5) 0.000
C1 0.071(6) 0.082(6) 0.122(8) 0.000 0.051(6) 0.000
C2 0.071(6) 0.082(6) 0.122(8) 0.000 0.051(6) 0.000
N2 0.071(6) 0.082(6) 0.122(8) 0.000 0.051(6) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C6 1.977(10) . ?
Pt1 C6 1.977(10) 6_565 ?
Pt1 C5 1.982(10) . ?
Pt1 C5 1.982(10) 6_565 ?
Fe2 N4 2.128(9) . ?
Fe2 N4 2.128(9) 5_677 ?
Fe2 N4 2.128(9) 2_657 ?
Fe2 N4 2.128(9) 6_575 ?
Fe2 N5 2.23(2) 5_677 ?
Fe2 N5 2.23(2) . ?
Fe1 N3 2.130(9) . ?
Fe1 N3 2.130(9) 6 ?
Fe1 N3 2.130(9) 2_656 ?
Fe1 N3 2.130(9) 5_656 ?
Fe1 N1 2.2578(8) 5_656 ?
Fe1 N1 2.2579(8) . ?
C6 N4 1.138(13) . ?
N3 C5 1.134(14) . ?
N5 C10 1.39(3) . ?
N5 C7 1.33(3) . ?
N1 C4 1.32(3) . ?
N1 C1 1.42938(15) . ?
C3 C4 1.4001(11) . ?
C3 O1 1.26(4) . ?
C3 C2 1.42(4) . ?
C4 H4 0.9300 . ?
N6 C10 1.33(2) . ?
N6 C9 1.09(2) . ?
O2 C8 1.17(3) . ?
C8 C9 1.50(4) . ?
C8 C7 1.46(4) . ?
C10 H10 0.9300 . ?
C9 H9 0.9300 . ?
C7 H7 0.9300 . ?
O3 C11 1.32(2) . ?
O3 C11 1.32(2) 6 ?
C11 C11 1.28(8) 7_546 ?
C1 H1 0.9300 . ?
C1 N2 1.2344(3) . ?
C2 H2 0.9300 . ?
C2 N2 1.4678(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
C6 Pt1 C6 90.2(5) . 6_565 ?
C6 Pt1 C5 89.5(4) 6_565 . ?
C6 Pt1 C5 179.0(5) . . ?
C6 Pt1 C5 179.0(5) 6_565 6_565 ?
C6 Pt1 C5 89.5(4) . 6_565 ?
C5 Pt1 C5 90.9(6) . 6_565 ?
N4 Fe2 N4 89.9(5) 5_677 6_575 ?
N4 Fe2 N4 180.0 5_677 . ?
N4 Fe2 N4 180.0 6_575 2_657 ?
N4 Fe2 N4 89.9(5) 2_657 . ?
N4 Fe2 N4 90.1(5) 6_575 . ?
N4 Fe2 N4 90.1(5) 5_677 2_657 ?
N4 Fe2 N5 91.6(6) 5_677 5_677 ?
N4 Fe2 N5 88.4(6) 2_657 . ?
N4 Fe2 N5 91.6(6) 6_575 . ?
N4 Fe2 N5 88.4(6) 5_677 . ?
N4 Fe2 N5 88.4(6) . 5_677 ?
N4 Fe2 N5 91.6(6) . . ?
N4 Fe2 N5 88.4(6) 6_575 5_677 ?
N4 Fe2 N5 91.6(6) 2_657 5_677 ?
N5 Fe2 N5 180.0 5_677 . ?
N3 Fe1 N3 89.5(5) 5_656 2_656 ?
N3 Fe1 N3 180.0 . 5_656 ?
N3 Fe1 N3 90.5(5) . 2_656 ?
N3 Fe1 N3 89.5(5) . 6 ?
N3 Fe1 N3 90.5(5) 5_656 6 ?
N3 Fe1 N3 180.0(7) 6 2_656 ?
N3 Fe1 N1 89.6(3) 5_656 . ?
N3 Fe1 N1 90.4(3) 2_656 5_656 ?
N3 Fe1 N1 89.6(3) . 5_656 ?
N3 Fe1 N1 89.6(3) 2_656 . ?
N3 Fe1 N1 90.4(3) . . ?
N3 Fe1 N1 89.6(3) 6 5_656 ?
N3 Fe1 N1 90.4(3) 6 . ?
N3 Fe1 N1 90.4(3) 5_656 5_656 ?
N1 Fe1 N1 180.0 5_656 . ?
N4 C6 Pt1 179.5(12) . . ?
C5 N3 Fe1 177.3(11) . . ?
C6 N4 Fe2 172.0(10) . . ?
N3 C5 Pt1 179.1(10) . . ?
C10 N5 Fe2 119.5(14) . . ?
C7 N5 Fe2 120(2) . . ?
C7 N5 C10 121(2) . . ?
C4 N1 Fe1 124.8(10) . . ?
C4 N1 C1 122.7(10) . . ?
C1 N1 Fe1 112.515(12) . . ?
C4 C3 C2 119(3) . . ?
O1 C3 C4 118(3) . . ?
O1 C3 C2 122.5(16) . . ?
N1 C4 C3 116(3) . . ?
N1 C4 H4 122.2 . . ?
C3 C4 H4 122.2 . . ?
C9 N6 C10 119(2) . . ?
O2 C8 C9 125(3) . . ?
O2 C8 C7 122(3) . . ?
C7 C8 C9 114(2) . . ?
N5 C10 H10 118.3 . . ?
N6 C10 N5 123.5(15) . . ?
N6 C10 H10 118.3 . . ?
N6 C9 C8 127.7(17) . . ?
N6 C9 H9 116.1 . . ?
C8 C9 H9 116.1 . . ?
N5 C7 C8 115(3) . . ?
N5 C7 H7 122.5 . . ?
C8 C7 H7 122.5 . . ?
C11 O3 C11 173(8) . 6 ?
C11 C11 O3 143(8) 7_546 . ?
N1 C1 H1 116.3 . . ?
N2 C1 N1 127.460(12) . . ?
N2 C1 H1 116.3 . . ?
C3 C2 H2 118.6 . . ?
C3 C2 N2 122.8(10) . . ?
N2 C2 H2 118.6 . . ?
C1 N2 C2 112.13(2) . . ?

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
Fe2 N5 C10 N6 180.000(15) . . . . ?
Fe2 N5 C7 C8 180.000(14) . . . . ?
Fe1 N1 C4 C3 180.000(2) . . . . ?
Fe1 N1 C1 N2 180.0 . . . . ?
N1 C1 N2 C2 0.0 . . . . ?
C3 C2 N2 C1 0.0 . . . . ?
C4 N1 C1 N2 0.0 . . . . ?
C4 C3 C2 N2 0.000(4) . . . . ?
O2 C8 C9 N6 180.000(15) . . . . ?
O2 C8 C7 N5 180.000(15) . . . . ?
O1 C3 C4 N1 180.000(2) . . . . ?
O1 C3 C2 N2 180.0 . . . . ?
C10 N5 C7 C8 0.000(17) . . . . ?
C10 N6 C9 C8 0.000(18) . . . . ?
C9 N6 C10 N5 0.000(17) . . . . ?
C9 C8 C7 N5 0.000(15) . . . . ?
C7 N5 C10 N6 0.000(16) . . . . ?
C7 C8 C9 N6 0.000(16) . . . . ?
C1 N1 C4 C3 0.000(4) . . . . ?
C2 C3 C4 N1 0.000(3) . . . . ?

_shelx_res_file                  
;
TITL rt590_ohpymptetoh_260k_a.res in C2/m
    rt590_ohpymptetoh_260k.res
    created by SHELXL-2018/3 at 12:08:46 on 26-Sep-2022
REM Old TITL RT590_OHPymPtEtOH_260K in C2/m
REM SHELXT solution in C2/m: R1 0.114, Rweak 0.012, Alpha 0.010
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C1 N6 Fe Pt
CELL 0.71073 21.7242 7.4168 14.7576 90 132.57 90
ZERR 4 0.0022 0.0002 0.0016 0 0.018 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pt
UNIT 52 24 4 32 10 4
DFIX 1.35 O3 C11
DFIX 1.4 0.001 C3 C4
EADP C9 N6 C10 N5 C7 C8 O2
EADP C2 C3 O1 C4 N1 C1 N2

L.S. 10 0 0
PLAN  5
SIZE 0.2 0.2 0.05
TEMP -13.13
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\RT590_OHPymPtEtOH_260K.hkl">
REM </olex2.extras>

WGHT    0.056200   54.602097
FVAR       0.18601
PT1   6    0.483824    0.500000    0.734509    10.50000    0.03402    0.01415 =
         0.02572    0.00000    0.02309    0.00000
FE2   3    0.500000    1.000000    1.000000    10.25000    0.03808    0.01175 =
         0.02604    0.00000    0.02513    0.00000
FE1   3    0.500000    0.000000    0.500000    10.25000    0.03967    0.01250 =
         0.02812    0.00000    0.02719    0.00000
C6    1    0.482533    0.688843    0.827800    11.00000    0.04775    0.01827 =
         0.02692    0.00151    0.02767   -0.00036
N3    4    0.489451    0.202294    0.591326    11.00000    0.07328    0.02565 =
         0.06005   -0.00487    0.05726    0.00089
N4    4    0.482225    0.796839    0.882289    11.00000    0.07314    0.02466 =
         0.03616   -0.00313    0.04183    0.00020
C5    1    0.487156    0.309645    0.643683    11.00000    0.05223    0.01725 =
         0.04515    0.00179    0.04172    0.00207
N5    4    0.364564    1.000000    0.899427    10.50000    0.06362    0.07192 =
         0.10353    0.00000    0.03655    0.00000
N1    4   10.359900   10.000000   10.342060    10.50000    0.07051    0.08222 =
         0.12166    0.00000    0.05066    0.00000
C3    1    0.233764    0.000000    0.141048    10.50000    0.07051    0.08222 =
         0.12166    0.00000    0.05066    0.00000
C4    1    0.321204    0.000000    0.224266    10.50000    0.07051    0.08222 =
         0.12166    0.00000    0.05066    0.00000
AFIX  43
H4    2    0.350171    0.000000    0.198475    10.50000   -1.20000
AFIX   0
N6    4    0.260690    1.000000    0.912532    10.50000    0.06362    0.07192 =
         0.10353    0.00000    0.03655    0.00000
O2    5    0.165156    1.000000    0.614294    10.50000    0.06362    0.07192 =
         0.10353    0.00000    0.03655    0.00000
O1    5    0.193781    0.000000    0.027618    10.50000    0.07051    0.08222 =
         0.12166    0.00000    0.05066    0.00000
C8    1    0.220883    1.000000    0.721098    10.50000    0.06362    0.07192 =
         0.10353    0.00000    0.03655    0.00000
C10   1   10.340120   11.000000   10.965150    10.50000    0.06362    0.07192 =
         0.10353    0.00000    0.03655    0.00000
AFIX  43
H10   2    0.381474    1.000000    1.050620    10.50000   -1.20000
AFIX   0
C9    1   10.211460   11.000000   10.812860    10.50000    0.06362    0.07192 =
         0.10353    0.00000    0.03655    0.00000
AFIX  43
H9    2    0.156965    1.000000    0.780524    10.50000   -1.20000
AFIX   0
C7    1    0.307769    1.000000    0.776883    10.50000    0.06362    0.07192 =
         0.10353    0.00000    0.03655    0.00000
AFIX  43
H7    2    0.322278    1.000000    0.730308    10.50000   -1.20000
AFIX   0

O3    5    0.233519    0.000000    0.487661    10.25000    0.10837
C11   1    0.228849   -0.178259    0.485325    10.50000    0.16246
C1    1   10.316000   10.000000   10.382700    10.50000    0.07051    0.08222 =
         0.12166    0.00000    0.05066    0.00000
AFIX  43
H1    2    0.348757    0.000000    0.467380    10.50000   -1.20000
AFIX   0
C2    1   10.193501   10.000000   10.186399    10.50000    0.07051    0.08222 =
         0.12166    0.00000    0.05066    0.00000
AFIX  43
H2    2    0.135392    0.000000    0.130240    10.50000   -1.20000
AFIX   0
N2    4   10.239599   10.000000   10.318301    10.50000    0.07051    0.08222 =
         0.12166    0.00000    0.05066    0.00000
HKLF 4




REM  rt590_ohpymptetoh_260k_a.res in C2/m
REM wR2 = 0.1349, GooF = S = 1.150, Restrained GooF = 1.150 for all data
REM R1 = 0.0521 for 1825 Fo > 4sig(Fo) and 0.0616 for all 2051 data
REM 82 parameters refined using 2 restraints

END

WGHT      0.0562     54.5848

REM Highest difference peak  2.858,  deepest hole -2.875,  1-sigma level  0.281
Q1    1   0.2666  0.0000  0.0974  10.50000  0.05    2.43
Q2    1   0.1958  1.0000  0.8783  10.50000  0.05    2.24
Q3    1   0.1595  0.0000  0.2119  10.50000  0.05    2.11
Q4    1   0.2357  1.0000  0.6638  10.50000  0.05    2.00
Q5    1   0.5435  0.5000  0.7731  10.50000  0.05    1.65
;
_shelx_res_checksum              32921
_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 1.333
_oxdiff_exptl_absorpt_empirical_full_min 0.783
####################################################################### 
# 
# 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_rt475_ohpympt_meoh_260k
_database_code_depnum_ccdc_archive 'CCDC 2209631'
loop_
_audit_author_name
_audit_author_address
'CARLOS BARTUAL MURGUI'
;University of Valencia
Spain
;
_audit_update_record             
;
2022-09-27 deposited with the CCDC.	2022-11-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_rt475_ohpympt_meoh_260k 
;
PROBLEM: Check Calcd Resid. Dens.  0.08Ang From N5              4.19 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT342_rt475_ohpympt_meoh_260k 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.04 Ang.
RESPONSE: This alert arises from the strong disorder of the guest in the structural pores and from a deterioration of the crystal during the desorption readsorption processes
;
_vrf_PLAT420_rt475_ohpympt_meoh_260k 
;
PROBLEM: D-H Bond Without Acceptor  O1       --H1       .     Please Check
RESPONSE: There is a certain number of H-bonds which are properly discussed in the paper. This alert arises from the absence of H atoms which are not present due to the strong agitation of the molecular moieties involved in the H-bond interactions
;
_vrf_PLAT971_rt475_ohpympt_meoh_260k_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.11Ang From N1              2.94 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the N1 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT971_rt475_ohpympt_meoh_260k_3 
;
PROBLEM: Check Calcd Resid. Dens.  1.02Ang From C3              2.82 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C3 atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_260k 
;
PROBLEM: Check Calcd Resid. Dens.  0.13Ang From O2             -3.01 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT972_rt475_ohpympt_meoh_260k_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.30Ang From O1             -2.54 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the O atom resulting from the deterioration of the crystal during the SCO process.
;
_vrf_PLAT975_rt475_ohpympt_meoh_260k 
;
PROBLEM: Check Calcd Resid. Dens.  0.51Ang From C11     .       1.91 eA-3
RESPONSE: The residual electronic density may be due to a ellipsoid elongation of the C11 atom resulting from the deterioration of the crystal during the SCO process.
;
# Added during the CSD deposition process: Tuesday 27 September 2022 09:42 PM
# end Validation Reply Form

_audit_creation_date             2022-09-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H8 Fe N8 O2 Pt, 0.25(C2 O2)'
_chemical_formula_sum            'C12.50 H8 Fe N8 O2.50 Pt'
_chemical_formula_weight         561.21
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.655(3)
_cell_length_b                   7.4564(3)
_cell_length_c                   15.983(2)
_cell_angle_alpha                90
_cell_angle_beta                 137.26(3)
_cell_angle_gamma                90
_cell_volume                     1751.4(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3651
_cell_measurement_temperature    260.00(10)
_cell_measurement_theta_max      29.5370
_cell_measurement_theta_min      3.7400
_shelx_estimated_absorpt_T_max   0.666
_shelx_estimated_absorpt_T_min   0.351
_exptl_absorpt_coefficient_mu    8.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7744
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.735
_diffrn_reflns_theta_min         3.015
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      260.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00  11.00   1.00    5.00    --  -20.96 -77.00 120.00   49
  2  ω    -81.00 -39.00   1.00    5.00    --  -20.96 -38.00-120.00   42
  3  ω    -10.00  40.00   1.00    5.00    --   22.05  77.00 -30.00   50
  4  ω      2.00  37.00   1.00    5.00    --   22.05  77.00  60.00   35
  5  ω    -43.00  39.00   1.00    5.00    --   22.05 -57.00-150.00   82
  6  ω    -51.00  45.00   1.00    5.00    --   22.05 -38.00 -30.00   96
  7  ω     -5.00  90.00   1.00    5.00    --   22.05  38.00 150.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0107435000
_diffrn_orient_matrix_UB_12      -0.0922253000
_diffrn_orient_matrix_UB_13      0.0055726000
_diffrn_orient_matrix_UB_21      0.0308766000
_diffrn_orient_matrix_UB_22      0.0223093000
_diffrn_orient_matrix_UB_23      -0.0016992000
_diffrn_orient_matrix_UB_31      0.0354933000
_diffrn_orient_matrix_UB_32      0.0084900000
_diffrn_orient_matrix_UB_33      0.0651027000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2252
_reflns_number_total             2450
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         4.051
_refine_diff_density_min         -3.184
_refine_diff_density_rms         0.316
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         2450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0480
_refine_ls_restrained_S_all      1.124
_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)+(0.0447P)²+51.3695P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1239
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N5) = Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(N6) = Uanis(C10) =
Uanis(N1) = Uanis(C1) = Uanis(N2) = Uanis(C2) = Uanis(C3) = Uanis(C4) =
Uanis(O1) = Uanis(O2)
3. Others
 Fixed Sof: H1(0.5) H2(0.5) O3(0.25) C11(0.25)
 Fixed X: O3(0.256599) C11(0.24866)
 Fixed Y: O3(-0.5) C11(-0.68398)
 Fixed Z: O3(0.025201) C11(0.006499)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2A), C4(H4), C7(H7), C9(H9), C10(H10)
4.b Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.24901(3) -0.500000 0.23271(4) 0.01597(14) Uani 1 2 d S T P . .
Fe2 Fe 0.000000 -1.000000 0.000000 0.0169(4) Uani 1 4 d S T P . .
Fe1 Fe 0.500000 0.000000 0.500000 0.0181(4) Uani 1 4 d S T P . .
O1 O 0.6782(10) 0.000000 0.3699(13) 0.0686(13) Uani 1 2 d S T P . .
H1 H 0.676201 -0.066053 0.326935 0.103 Uiso 0.5 1 calc R U P . .
O2 O 0.0627(10) -1.000000 -0.2723(13) 0.0686(13) Uani 1 2 d S T P . .
H2 H 0.109309 -1.045892 -0.207592 0.103 Uiso 0.5 1 calc R U P . .
N1 N 0.5219(13) 0.000000 0.3827(17) 0.0686(13) Uani 1 2 d S T P . .
N2 N 0.4410(13) 0.000000 0.1688(16) 0.0686(13) Uani 1 2 d S T P . .
N3 N 0.3970(5) -0.2021(10) 0.3878(7) 0.0343(18) Uani 1 1 d . . . . .
N4 N 0.0997(5) -0.7983(11) 0.0805(8) 0.0357(19) Uani 1 1 d . . . . .
N5 N -0.0363(13) -1.000000 -0.1718(17) 0.0686(13) Uani 1 2 d S T P . .
N6 N -0.1516(13) -1.000000 -0.3915(17) 0.0686(13) Uani 1 2 d S T P . .
C1 C 0.4430(16) 0.000000 0.254(2) 0.0686(13) Uani 1 2 d S T P . .
H1A H 0.387215 0.000000 0.225980 0.082 Uiso 1 2 calc R U P . .
C2 C 0.5171(15) 0.000000 0.211(2) 0.0686(13) Uani 1 2 d S T P . .
H2A H 0.516750 0.000000 0.152482 0.082 Uiso 1 2 calc R U P . .
C3 C 0.6002(16) 0.000000 0.329(2) 0.0686(13) Uani 1 2 d S T P . .
C4 C 0.5986(16) 0.000000 0.421(2) 0.0686(13) Uani 1 2 d S T P . .
H4 H 0.652655 0.000000 0.504970 0.082 Uiso 1 2 calc R U P . .
C5 C 0.3434(5) -0.3100(11) 0.3324(7) 0.0249(17) Uani 1 1 d . . . . .
C6 C 0.1538(5) -0.6904(11) 0.1345(8) 0.0250(17) Uani 1 1 d . . . . .
C7 C 0.0265(16) -1.000000 -0.166(2) 0.0686(13) Uani 1 2 d S T P . .
H7 H 0.087427 -1.000000 -0.089071 0.082 Uiso 1 2 calc R U P . .
C8 C 0.0027(16) -1.000000 -0.276(2) 0.0686(13) Uani 1 2 d S T P . .
C9 C -0.0943(15) -1.000000 -0.385(2) 0.0686(13) Uani 1 2 d S T P . .
H9 H -0.113808 -1.000000 -0.459627 0.082 Uiso 1 2 calc R U P . .
C10 C -0.1235(15) -1.000000 -0.284(2) 0.0686(13) Uani 1 2 d S T P . .
H10 H -0.168014 -1.000000 -0.286694 0.082 Uiso 1 2 calc R U P . .
O3 O 0.256599 -0.500000 0.025201 0.070(8) Uiso 0.25 1 d S . P A -1
C11 C 0.248660 -0.683980 0.006499 0.044(10) Uiso 0.25 1 d . . P A -1

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0112(2) 0.0118(2) 0.0180(2) 0.000 0.00858(18) 0.000
Fe2 0.0111(9) 0.0108(9) 0.0184(10) 0.000 0.0075(8) 0.000
Fe1 0.0131(10) 0.0118(9) 0.0201(10) 0.000 0.0093(9) 0.000
O1 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
O2 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
N1 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
N2 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
N3 0.023(4) 0.019(4) 0.032(4) -0.004(3) 0.011(3) -0.005(3)
N4 0.017(3) 0.025(4) 0.048(5) -0.004(4) 0.019(3) -0.005(3)
N5 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
N6 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
C1 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
C2 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
C3 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
C4 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
C5 0.019(4) 0.019(4) 0.023(4) -0.004(3) 0.011(3) -0.001(3)
C6 0.020(4) 0.016(4) 0.038(5) 0.007(3) 0.021(4) 0.005(3)
C7 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
C8 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
C9 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000
C10 0.079(3) 0.075(3) 0.071(3) 0.000 0.060(3) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C5 1.985(8) . ?
Pt1 C5 1.985(8) 6_545 ?
Pt1 C6 1.994(8) . ?
Pt1 C6 1.994(8) 6_545 ?
Fe2 N4 2.121(7) 6_535 ?
Fe2 N4 2.121(7) 5_535 ?
Fe2 N4 2.121(7) 2 ?
Fe2 N4 2.121(7) . ?
Fe2 N5 2.233(17) . ?
Fe2 N5 2.233(17) 5_535 ?
Fe1 N1 2.245(16) 5_656 ?
Fe1 N1 2.245(16) . ?
Fe1 N3 2.142(7) 6 ?
Fe1 N3 2.142(7) . ?
Fe1 N3 2.142(7) 5_656 ?
Fe1 N3 2.142(7) 2_656 ?
O1 H1 0.8200 . ?
O1 H1 0.8(3) 6 ?
O1 C3 1.29(2) . ?
O2 H2 0.8(3) 6_535 ?
O2 H2 0.8200 . ?
O2 C8 1.26(2) . ?
N1 C1 1.41(3) . ?
N1 C4 1.28(3) . ?
N2 C1 1.33(2) . ?
N2 C2 1.24(3) . ?
N3 C5 1.126(11) . ?
N4 C6 1.131(11) . ?
N5 C7 1.29(2) . ?
N5 C10 1.34(3) . ?
N6 C9 1.16(2) . ?
N6 C10 1.34(2) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C2 C3 1.35(3) . ?
C3 C4 1.49(3) . ?
C4 H4 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.43(3) . ?
C8 C9 1.44(3) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
O3 C11 2.39529(9) 7_535 ?
O3 C11 1.38756(6) . ?

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
C5 Pt1 C5 91.1(5) . 6_545 ?
C5 Pt1 C6 89.0(3) 6_545 . ?
C5 Pt1 C6 178.9(3) . . ?
C5 Pt1 C6 178.9(3) 6_545 6_545 ?
C5 Pt1 C6 89.0(3) . 6_545 ?
C6 Pt1 C6 90.8(5) . 6_545 ?
N4 Fe2 N4 89.7(4) 5_535 6_535 ?
N4 Fe2 N4 180.0 5_535 . ?
N4 Fe2 N4 180.0 6_535 2 ?
N4 Fe2 N4 89.7(4) 2 . ?
N4 Fe2 N4 90.3(4) 6_535 . ?
N4 Fe2 N4 90.3(4) 5_535 2 ?
N4 Fe2 N5 88.4(4) 5_535 . ?
N4 Fe2 N5 88.4(4) 6_535 5_535 ?
N4 Fe2 N5 88.4(4) . 5_535 ?
N4 Fe2 N5 91.6(4) 5_535 5_535 ?
N4 Fe2 N5 88.4(4) 2 . ?
N4 Fe2 N5 91.6(4) 2 5_535 ?
N4 Fe2 N5 91.6(4) 6_535 . ?
N4 Fe2 N5 91.6(4) . . ?
N5 Fe2 N5 180.0 . 5_535 ?
N1 Fe1 N1 180.00(19) 5_656 . ?
N3 Fe1 N1 91.7(4) . . ?
N3 Fe1 N1 88.3(4) 2_656 . ?
N3 Fe1 N1 91.7(4) 6 . ?
N3 Fe1 N1 88.3(4) 5_656 . ?
N3 Fe1 N1 88.3(4) 6 5_656 ?
N3 Fe1 N1 88.3(4) . 5_656 ?
N3 Fe1 N1 91.7(4) 5_656 5_656 ?
N3 Fe1 N1 91.7(4) 2_656 5_656 ?
N3 Fe1 N3 90.6(4) . 2_656 ?
N3 Fe1 N3 89.4(4) . 6 ?
N3 Fe1 N3 89.4(4) 5_656 2_656 ?
N3 Fe1 N3 90.6(4) 5_656 6 ?
N3 Fe1 N3 180.0 . 5_656 ?
N3 Fe1 N3 180.0 6 2_656 ?
H1 O1 H1 73.8 . 6 ?
C3 O1 H1 109.5 . . ?
C3 O1 H1 109(7) . 6 ?
H2 O2 H2 49.3 . 6_535 ?
C8 O2 H2 109(6) . 6_535 ?
C8 O2 H2 109.5 . . ?
C1 N1 Fe1 116.5(13) . . ?
C4 N1 Fe1 126.6(15) . . ?
C4 N1 C1 116.9(18) . . ?
C2 N2 C1 114(2) . . ?
C5 N3 Fe1 177.5(8) . . ?
C6 N4 Fe2 171.7(9) . . ?
C7 N5 Fe2 120.4(16) . . ?
C7 N5 C10 118.4(19) . . ?
C10 N5 Fe2 121.2(14) . . ?
C9 N6 C10 116(2) . . ?
N1 C1 H1A 117.0 . . ?
N2 C1 N1 126(2) . . ?
N2 C1 H1A 117.0 . . ?
N2 C2 H2A 115.3 . . ?
N2 C2 C3 129(2) . . ?
C3 C2 H2A 115.3 . . ?
O1 C3 C2 128(2) . . ?
O1 C3 C4 118(2) . . ?
C2 C3 C4 114(2) . . ?
N1 C4 C3 119(2) . . ?
N1 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N3 C5 Pt1 179.1(9) . . ?
N4 C6 Pt1 178.6(8) . . ?
N5 C7 H7 120.0 . . ?
N5 C7 C8 120(2) . . ?
C8 C7 H7 120.0 . . ?
O2 C8 C7 121(2) . . ?
O2 C8 C9 127(2) . . ?
C7 C8 C9 112.1(19) . . ?
N6 C9 C8 128(2) . . ?
N6 C9 H9 115.8 . . ?
C8 C9 H9 115.8 . . ?
N5 C10 H10 117.3 . . ?
N6 C10 N5 125(2) . . ?
N6 C10 H10 117.3 . . ?
C11 O3 C11 4.224(1) . 7_535 ?

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
Fe2 N5 C7 C8 180.000(4) . . . . ?
Fe2 N5 C10 N6 180.000(6) . . . . ?
Fe1 N1 C1 N2 180.000(4) . . . . ?
Fe1 N1 C4 C3 180.000(6) . . . . ?
O1 C3 C4 N1 180.000(8) . . . . ?
O2 C8 C9 N6 180.000(8) . . . . ?
N2 C2 C3 O1 180.000(6) . . . . ?
N2 C2 C3 C4 0.000(8) . . . . ?
N5 C7 C8 O2 180.000(4) . . . . ?
N5 C7 C8 C9 0.000(6) . . . . ?
C1 N1 C4 C3 0.000(8) . . . . ?
C1 N2 C2 C3 0.000(7) . . . . ?
C2 N2 C1 N1 0.000(6) . . . . ?
C2 C3 C4 N1 0.000(8) . . . . ?
C4 N1 C1 N2 0.000(8) . . . . ?
C7 N5 C10 N6 0.000(6) . . . . ?
C7 C8 C9 N6 0.000(9) . . . . ?
C9 N6 C10 N5 0.000(9) . . . . ?
C10 N5 C7 C8 0.000(6) . . . . ?
C10 N6 C9 C8 0.000(11) . . . . ?

_shelx_res_file                  
;
TITL rt475_ohpympt_meoh_260k_a.res in C2/m
    rt475_ohpympt_meoh_260k.res
    created by SHELXL-2018/3 at 22:21:57 on 27-Sep-2022
REM Old TITL RT475_OHPymPt_MeOH_260K in C2/m
REM SHELXT solution in C2/m: R1 0.095, Rweak 0.016, Alpha 0.069
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 N13 Fe Pt
CELL 0.71073 21.6553 7.4564 15.9834 90 137.263 90
ZERR 4 0.0032 0.0003 0.0023 0 0.028 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H Fe N O Pt
UNIT 50 32 4 32 10 4
EQIV $1 0.5-X,-1.5-Y,-Z
EADP N5 C7 C8 C9 N6 C10 N1 C1 N2 C2 C3 C4 O1 O2

L.S. 15
PLAN  15
SIZE 0.15 0.15 0.05
TEMP -13.13
CONF
BIND O3 C11_$1
list 4
MORE -1
BOND $H
fmap 2
acta
OMIT 1 9 5
OMIT -1 9 7
REM <olex2.extras>
REM <HklSrc "%.\\RT475_OHPymPt_MeOH_260K.hkl">
REM </olex2.extras>

WGHT    0.044700   51.369499
FVAR       0.16061
PT1   6    0.249014   -0.500000    0.232707    10.50000    0.01122    0.01184 =
         0.01800    0.00000    0.00858    0.00000
FE2   3    0.000000   -1.000000    0.000000    10.25000    0.01108    0.01077 =
         0.01839    0.00000    0.00754    0.00000
FE1   3    0.500000    0.000000    0.500000    10.25000    0.01312    0.01179 =
         0.02009    0.00000    0.00927    0.00000
O1    5    0.678247    0.000000    0.369946    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
AFIX 147
H1    2    0.676201   -0.066053    0.326935    10.50000   -1.50000
AFIX   0
O2    5    0.062655   -1.000000   -0.272282    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
AFIX 147
H2    2    0.109309   -1.045892   -0.207592    10.50000   -1.50000
AFIX   0
N1    4    0.521853    0.000000    0.382711    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
N2    4    0.441043    0.000000    0.168837    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
N3    4    0.396975   -0.202130    0.387845    11.00000    0.02253    0.01914 =
         0.03204   -0.00431    0.01092   -0.00535
N4    4    0.099705   -0.798298    0.080475    11.00000    0.01727    0.02524 =
         0.04823   -0.00393    0.01897   -0.00536
N5    4   -0.036311   -1.000000   -0.171822    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
N6    4   -0.151583   -1.000000   -0.391496    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
C1    1    0.442964    0.000000    0.253923    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
AFIX  43
H1A   2    0.387215    0.000000    0.225980    10.50000   -1.20000
AFIX   0
C2    1    0.517112    0.000000    0.211027    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
AFIX  43
H2A   2    0.516750    0.000000    0.152482    10.50000   -1.20000
AFIX   0
C3    1    0.600234    0.000000    0.329287    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
C4    1    0.598570    0.000000    0.420940    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
AFIX  43
H4    2    0.652655    0.000000    0.504970    10.50000   -1.20000
AFIX   0
C5    1    0.343362   -0.309973    0.332365    11.00000    0.01929    0.01881 =
         0.02265   -0.00380    0.01098   -0.00078
C6    1    0.153814   -0.690428    0.134548    11.00000    0.01992    0.01610 =
         0.03849    0.00698    0.02131    0.00467
C7    1    0.026536   -1.000000   -0.165509    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
AFIX  43
H7    2    0.087427   -1.000000   -0.089071    10.50000   -1.20000
AFIX   0
C8    1    0.002690   -1.000000   -0.276007    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
C9    1   -0.094326   -1.000000   -0.384881    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
AFIX  43
H9    2   -0.113808   -1.000000   -0.459627    10.50000   -1.20000
AFIX   0
C10   1   -0.123472   -1.000000   -0.283700    10.50000    0.07850    0.07470 =
         0.07073    0.00000    0.06050    0.00000
AFIX  43
H10   2   -0.168014   -1.000000   -0.286694    10.50000   -1.20000
AFIX   0

PART -1
O3    5   10.256599    9.500000   10.025201    10.25000    0.07045
C11   1   10.248660    9.316020   10.006499    10.25000    0.04434
HKLF 4




REM  rt475_ohpympt_meoh_260k_a.res in C2/m
REM wR2 = 0.1239, GooF = S = 1.124, Restrained GooF = 1.124 for all data
REM R1 = 0.0480 for 2252 Fo > 4sig(Fo) and 0.0542 for all 2450 data
REM 87 parameters refined using 0 restraints

END

WGHT      0.0447     51.4593

REM Highest difference peak  4.051,  deepest hole -3.184,  1-sigma level  0.316
Q1    1   0.6608  0.0000  0.4270  10.50000  0.05    2.67
Q2    1  -0.1785 -1.0000 -0.4878  10.50000  0.05    2.36
Q3    1   0.4406  0.0000  0.1021  10.50000  0.05    2.35
Q4    1   0.0583 -1.0000 -0.2120  10.50000  0.05    2.26
Q5    1   0.2436 -0.5000  0.1725  10.50000  0.05    1.78
Q6    1  -0.0903 -1.0000 -0.2814  10.50000  0.05    1.53
Q7    1   0.5058  0.0000  0.2395  10.50000  0.05    1.49
Q8    1   0.2804 -0.3695  0.2999  11.00000  0.05    1.38
Q9    1   0.2576 -0.5951  0.0315  11.00000  0.05    1.35
Q10   1   0.1774 -0.5000  0.2191  10.50000  0.05    1.35
Q11   1   0.7188  0.0000  0.2913  10.50000  0.05    1.32
Q12   1   0.0054 -1.0000 -0.0923  10.50000  0.05    1.25
Q13   1   0.2756 -0.5663  0.2178  11.00000  0.05    1.24
Q14   1   0.2494 -0.6784  0.2298  11.00000  0.05    1.15
Q15   1  -0.2093 -1.0000 -0.5583  10.50000  0.05    1.13
;
_shelx_res_checksum              86236
_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 1.842
_oxdiff_exptl_absorpt_empirical_full_min 0.697
