# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_1_293K
_database_code_depnum_ccdc_archive 'CCDC 2023229'
loop_
_audit_author_name
_audit_author_address
'Yue Li' 'Xiamen University'
_audit_update_record             
;
2020-08-13 deposited with the CCDC.	2020-12-22 downloaded from the CCDC.
;
_audit_creation_date             2020-07-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H10 Br2 Fe N6 Pt, 2(H4 O2)'
_chemical_formula_sum            'C16 H18 Br2 Fe N6 O4 Pt'
_chemical_formula_weight         769.12
_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'
Br Br -0.2901 2.4595 '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      tetragonal
_space_group_IT_number           83
_space_group_name_H-M_alt        'P 4/m'
_space_group_name_Hall           '-P 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'

_cell_length_a                   7.4386(2)
_cell_length_b                   7.4386(2)
_cell_length_c                   13.733(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     759.88(13)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1657
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6890
_cell_measurement_theta_min      4.1260
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0749
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4726
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.818
_diffrn_reflns_theta_min         3.874
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -15.00  10.00   0.50   30.00    --    0.10  47.00 137.00   50
  2  ω    -60.00  28.00   0.50   30.00    --    0.10 -82.00  60.00  176
  3  ω     35.00  60.00   0.50   30.00    --    0.10  38.00  30.00   50
  4  ω     11.00  36.00   0.50   30.00    --    0.10  47.00 137.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0279586000
_diffrn_orient_matrix_UB_12      0.0254012000
_diffrn_orient_matrix_UB_13      0.0474331000
_diffrn_orient_matrix_UB_21      -0.0807963000
_diffrn_orient_matrix_UB_22      0.0492827000
_diffrn_orient_matrix_UB_23      0.0061914000
_diffrn_orient_matrix_UB_31      -0.0421856000
_diffrn_orient_matrix_UB_32      -0.0776083000
_diffrn_orient_matrix_UB_33      0.0194678000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                910
_reflns_number_total             1043
_reflns_odcompleteness_completeness 99.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         6.245
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.286
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1043
_refine_ls_number_restraints     109
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0757
_refine_ls_restrained_S_all      1.244
_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)+(0.1258P)²+0.3917P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_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 O(H,H) groups
2. Restrained distances
 C6-C3
 1.5 with sigma of 0.02
 Br1-C6
 1.8 with sigma of 0.02
 C4-C6
 2.6 with sigma of 0.02
3. Restrained planarity
 Br1, C6, C3, C2, C4, C5, N1, C1
 with sigma of 0.1
4. Rigid bond restraints
 N1, C5, C4, C3, C2, C1, C6, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(Br1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Pt1) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(Fe1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O2) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
6. Others
 Fixed Sof: N1(0.25) C5(0.25) H5(0.25) C4(0.25) H4(0.25) C3(0.25) C2(0.25)
 H2(0.25) C1(0.25) H1(0.25) C6(0.25) H6(0.25) Br1(0.25) O1(0.25) H1A(0.25)
 H1B(0.25) O2(0.25) H2A(0.25) H2B(0.25)
7.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B)
7.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C2(H2), C1(H1), C6(H6)
7.c Fitted hexagon refined as free rotating group:
 N1(C5,C4,C3,C2,C1)
;
_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 1.000000 0.000000 0.500000 0.0366(4) Uani 1 8 d S TU P A .
Fe1 Fe 0.500000 0.500000 0.500000 0.0297(7) Uani 1 8 d S TU P . .
N2 N 0.7023(17) 0.2969(17) 0.500000 0.045(3) Uani 1 2 d S TU P A .
N1 N 0.491(14) 0.503(12) 0.6600(17) 0.087(8) Uani 0.25 1 d . U . A -1
C5 C 0.503(13) 0.329(11) 0.696(3) 0.108(10) Uani 0.25 1 d G U . A -1
H5 H 0.511891 0.232604 0.653295 0.130 Uiso 0.25 1 calc R . . A -1
C4 C 0.501(9) 0.299(7) 0.796(3) 0.113(10) Uani 0.25 1 d DG U . A -1
H4 H 0.508386 0.182660 0.820041 0.136 Uiso 0.25 1 calc R . . A -1
C3 C 0.487(8) 0.444(6) 0.8598(18) 0.126(10) Uani 0.25 1 d DG U . A -1
C2 C 0.475(12) 0.618(7) 0.824(3) 0.118(10) Uani 0.25 1 d G U . A -1
H2 H 0.465896 0.714314 0.866502 0.142 Uiso 0.25 1 calc R . . A -1
C1 C 0.477(14) 0.648(9) 0.724(3) 0.112(10) Uani 0.25 1 d G U . A -1
H1 H 0.469401 0.764261 0.699756 0.135 Uiso 0.25 1 calc R . . A -1
C7 C 0.8109(18) 0.1883(18) 0.500000 0.037(3) Uani 1 2 d S TU P . .
C6 C 0.483(8) 0.435(4) 0.969(2) 0.154(11) Uani 0.25 1 d D U . A -1
H6 H 0.472937 0.532866 1.011062 0.185 Uiso 0.25 1 calc R . . A -1
Br1 Br 0.500(4) 0.203(4) 1.005(4) 0.294(10) Uani 0.25 1 d D U . A -1
O1 O 0.500000 0.000000 0.719(10) 0.29(7) Uani 0.5 2 d S TU P . .
H1A H 0.465900 0.071170 0.763466 0.440 Uiso 0.25 1 d R . . . .
H1B H 0.583710 0.056400 0.689676 0.440 Uiso 0.25 1 d R . . . .
O2 O 0.871(15) -0.009(11) 0.794(9) 0.25(5) Uani 0.25 1 d . U . B -1
H2A H 0.779451 -0.049883 0.765040 0.370 Uiso 0.25 1 d R . . B -1
H2B H 0.828161 0.056497 0.839640 0.370 Uiso 0.25 1 d R . . B -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 0.0144(4) 0.0144(4) 0.0810(9) 0.000 0.000 0.000
Fe1 0.0144(9) 0.0144(9) 0.060(2) 0.000 0.000 0.000
N2 0.031(5) 0.030(5) 0.075(7) 0.000 0.000 0.008(4)
N1 0.080(12) 0.095(11) 0.085(9) 0.003(7) -0.001(10) -0.002(10)
C5 0.109(15) 0.103(11) 0.112(11) 0.010(9) -0.002(10) 0.000(10)
C4 0.116(15) 0.109(11) 0.114(11) 0.016(7) -0.002(10) -0.001(10)
C3 0.127(16) 0.128(12) 0.125(10) 0.000(6) 0.001(10) 0.001(10)
C2 0.121(15) 0.119(11) 0.114(10) -0.019(8) 0.001(10) 0.001(10)
C1 0.114(15) 0.109(11) 0.114(11) -0.011(8) 0.000(10) 0.001(10)
C7 0.029(5) 0.024(5) 0.057(7) 0.000 0.000 -0.009(4)
C6 0.157(16) 0.173(13) 0.132(11) -0.006(8) 0.001(10) -0.003(10)
Br1 0.42(2) 0.261(14) 0.199(12) 0.103(14) -0.005(18) 0.006(14)
O1 0.45(17) 0.16(7) 0.27(11) 0.000 0.000 0.01(8)
O2 0.38(11) 0.04(3) 0.33(9) -0.01(5) -0.01(7) 0.00(6)

_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 C7 1.985(14) . ?
Pt1 C7 1.985(15) 7_666 ?
Pt1 C7 1.985(15) 3_645 ?
Pt1 C7 1.985(14) 5_756 ?
Fe1 N2 2.132(12) 7_566 ?
Fe1 N2 2.132(12) 5_666 ?
Fe1 N2 2.132(12) 3_655 ?
Fe1 N2 2.132(12) . ?
Fe1 N1 2.20(2) . ?
N2 C7 1.14(2) . ?
N1 C5 1.3900 . ?
N1 C1 1.3900 . ?
C5 C4 1.3900 . ?
C4 C3 1.3900 . ?
C3 C2 1.3900 . ?
C3 C6 1.503(18) . ?
C2 C1 1.3900 . ?
C6 Br1 1.80(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Pt1 C7 90.0 . 7_666 ?
C7 Pt1 C7 180.0(5) 7_666 3_645 ?
C7 Pt1 C7 90.0 . 3_645 ?
C7 Pt1 C7 90.000(2) 7_666 5_756 ?
C7 Pt1 C7 180.0 . 5_756 ?
C7 Pt1 C7 90.000(2) 3_645 5_756 ?
N2 Fe1 N2 180.0(5) 7_566 3_655 ?
N2 Fe1 N2 90.000(1) 7_566 . ?
N2 Fe1 N2 90.000(3) 7_566 5_666 ?
N2 Fe1 N2 90.000(2) 3_655 5_666 ?
N2 Fe1 N2 90.000(3) 3_655 . ?
N2 Fe1 N2 180.0 . 5_666 ?
N2 Fe1 N1 89(3) 7_566 . ?
N2 Fe1 N1 92(2) . . ?
N2 Fe1 N1 88(2) 5_666 . ?
N2 Fe1 N1 91(3) 3_655 . ?
C7 N2 Fe1 179.9(13) . . ?
C5 N1 Fe1 110(4) . . ?
C5 N1 C1 120.0 . . ?
C1 N1 Fe1 130(4) . . ?
N1 C5 C4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C4 C3 C6 127(2) . . ?
C2 C3 C4 120.0 . . ?
C2 C3 C6 113(2) . . ?
C1 C2 C3 120.0 . . ?
C2 C1 N1 120.0 . . ?
N2 C7 Pt1 179.9(13) . . ?
C3 C6 Br1 108(3) . . ?

_iucr_refine_instructions_details 
;
TITL 1015007-4pt_a.res in P4/m
    1015007-4pt.res
    created by SHELXL-2018/3 at 09:42:05 on 14-Jul-2020
REM Old TITL 1015007-4pt_a.res in P4/m
REM SHELXT solution in P4/m
REM R1 0.256, Rweak 0.136, Alpha 0.071, Orientation as input
REM Formula found by SHELXT: C4 Br N4 O1 Pt
CELL 0.71073 7.4386 7.4386 13.7329 90 90 90
ZERR 1 0.0002 0.0002 0.0023 0 0 0
LATT 1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SFAC C H Br Fe N O Pt
UNIT 16 18 2 1 6 4 1
DFIX 1.5 C6 C3
DFIX 1.8 Br1 C6
DFIX 2.6 C4 C6
FLAT Br1 C6 C3 C2 C4 C5 N1 C1
DELU N1 C5 C4 C3 C2 C1 C6 Br1
ISOR 0.01 0.02 N1 C5 C4 C3 C2 C1 C6 Br1
ISOR 0.01 0.02 Pt1 C7 N2 Fe1
ISOR O1
ISOR 0.05 0.1 O2

L.S. 15 0 0
PLAN  20
list 4
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\1015007-4Pt.hkl">
REM </olex2.extras>

WGHT    0.125800    0.391700
FVAR       0.61564
PT1   7    1.000000    0.000000    0.500000    10.12500    0.01445    0.01445 =
         0.08104    0.00000    0.00000    0.00000
FE1   4    0.500000    0.500000    0.500000    10.12500    0.01444    0.01444 =
         0.06026    0.00000    0.00000    0.00000
N2    5    0.702310    0.296932    0.500000    10.50000    0.03060    0.03008 =
         0.07480    0.00000    0.00000    0.00758
PART -1
AFIX  66
N1    5    0.490993    0.503382    0.659994    10.25000    0.08002    0.09463 =
         0.08527    0.00274   -0.00056   -0.00220
C5    1    0.502672    0.329154    0.696028    10.25000    0.10888    0.10294 =
         0.11211    0.00964   -0.00169    0.00033
AFIX  43
H5    2    0.511891    0.232604    0.653295    10.25000   -1.20000
AFIX  65
C4    1    0.500573    0.299231    0.795932    10.25000    0.11595    0.10895 =
         0.11393    0.01624   -0.00236   -0.00074
AFIX  43
H4    2    0.508386    0.182660    0.820041    10.25000   -1.20000
AFIX  65
C3    1    0.486794    0.443536    0.859802    10.25000    0.12655    0.12762 =
         0.12530    0.00003    0.00105    0.00126
C2    1    0.475115    0.617765    0.823768    10.25000    0.12122    0.11891 =
         0.11442   -0.01929    0.00149    0.00081
AFIX  43
H2    2    0.465896    0.714314    0.866502    10.25000   -1.20000
AFIX  65
C1    1    0.477215    0.647690    0.723865    10.25000    0.11405    0.10950 =
         0.11362   -0.01090   -0.00037    0.00078
AFIX  43
H1    2    0.469401    0.764261    0.699756    10.25000   -1.20000
AFIX   0
PART 0
C7    1    0.810909    0.188316    0.500000    10.50000    0.02885    0.02365 =
         0.05730    0.00000    0.00000   -0.00864
PART -1
C6    1    0.482717    0.435141    0.969157    10.25000    0.15730    0.17296 =
         0.13228   -0.00599    0.00055   -0.00293
AFIX  43
H6    2    0.472937    0.532866    1.011062    10.25000   -1.20000
AFIX   0
BR1   3    0.500066    0.202970    1.004828    10.25000    0.42150    0.26079 =
         0.19877    0.10344   -0.00511    0.00607

PART 0
O1    6    0.500000    0.000000    0.718686    10.25000    0.45146    0.15790 =
         0.27110    0.00000    0.00000    0.00881
AFIX   3
H1A   2    0.465900    0.071170    0.763466    10.25000   -1.50000
H1B   2    0.583710    0.056400    0.689676    10.25000   -1.50000
AFIX   0

PART -1
O2    6    0.871171   -0.008583    0.794410    10.25000    0.37586    0.03665 =
         0.32660   -0.01437   -0.01252   -0.00458
AFIX   3
H2A   2    0.779451   -0.049883    0.765040    10.25000   -1.50000
H2B   2    0.828161    0.056497    0.839640    10.25000   -1.50000
AFIX   0
HKLF 4




REM  1015007-4pt_a.res in P4/m
REM wR2 = 0.193569, GooF = S = 1.20129, Restrained GooF = 1.24372 for all data
REM R1 = 0.075682 for 910 Fo > 4sig(Fo) and 0.088252 for all 1043 data
REM 91 parameters refined using 109 restraints

END  
     
WGHT      0.1258      0.3915 

REM Highest difference peak  6.245,  deepest hole -1.630,  1-sigma level  0.286
Q1    1   1.0000  0.0000  0.5782  10.25000  0.05    6.25
Q2    1   0.5000  0.5000  0.5723  10.25000  0.05    2.74
Q3    1   0.7251  0.2628  1.0000  10.50000  0.05    1.28
Q4    1   1.0548 -0.0049  0.5000  10.50000  0.05    1.01
Q5    1   1.0000  0.0000  0.6712  10.25000  0.05    0.95
Q6    1   0.7165  0.2946  0.5597  11.00000  0.05    0.91
Q7    1   0.5000  0.5000  0.8794  10.25000  0.05    0.80
Q8    1   0.6925  0.0096  1.0000  10.50000  0.05    0.78
Q9    1   0.8154  0.1995  0.5539  11.00000  0.05    0.76
Q10   1   0.5000  0.5000  0.7371  10.25000  0.05    0.75
Q11   1   1.0103  0.1596  0.4361  11.00000  0.05    0.72
Q12   1   0.2874  0.0017  1.0000  10.50000  0.05    0.65
Q13   1   1.0269  0.1179  0.4679  11.00000  0.05    0.64
Q14   1   1.0119  0.1053  0.5000  10.50000  0.05    0.63
Q15   1   0.5167  0.3935  0.9190  11.00000  0.05    0.54
Q16   1   0.8050  0.0844  0.5978  11.00000  0.05    0.49
Q17   1   0.5000  0.0000  0.5821  10.50000  0.05    0.48
Q18   1   0.5000  0.2830  0.5000  10.50000  0.05    0.47
Q19   1   0.4060  0.6012  1.0000  10.50000  0.05    0.47
Q20   1   0.4094  0.3456  0.8032  11.00000  0.05    0.46

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.075682 for 910 Fo > 4sig(Fo) and 0.088252 for all 4726 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 6.25, deepest hole -1.63
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.088252
  REM R1_gt = 0.075682
  REM wR_ref = 0.193569
  REM GOOF = 1.20129
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 4726
  REM Reflections_gt = 910
  REM Parameters = n/a
  REM Hole = -1.63
  REM Peak = 6.25
  REM Flack = n/a

  
;
_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 2.113
_oxdiff_exptl_absorpt_empirical_full_min 0.568
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2023232
_database_code_depnum_ccdc_archive 'CCDC 2023232'
_audit_update_record             
;
2020-11-29 deposited with the CCDC.	2020-12-22 downloaded from the CCDC.
;
_audit_creation_date             2020-11-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H10 Br2 Fe N6 Pd, 4(H2 O)'
_chemical_formula_sum            'C16 H18 Br2 Fe N6 O4 Pd'
_chemical_formula_weight         680.43
_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'
Br Br -0.2901 2.4595 '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      tetragonal
_space_group_IT_number           83
_space_group_name_H-M_alt        'P 4/m'
_space_group_name_Hall           '-P 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'

_cell_length_a                   7.2533(5)
_cell_length_b                   7.2533(5)
_cell_length_c                   13.346(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     702.16(14)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    514
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      26.4170
_cell_measurement_theta_min      4.2600
_shelx_estimated_absorpt_T_max   0.824
_shelx_estimated_absorpt_T_min   0.689
_exptl_absorpt_coefficient_mu    4.029
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             330
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_unetI/netI     0.0780
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3021
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.526
_diffrn_reflns_theta_min         4.150
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -60.00 -35.00   0.50   70.00    --    0.10 -40.00  -2.00   50
  2  ω    -40.00 -13.00   0.50   70.00    --    0.10 -77.00 -90.00   54
  3  ω    -62.00  -5.00   0.50   70.00    --    0.10 -82.00-150.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0615230000
_diffrn_orient_matrix_UB_12      0.0427340000
_diffrn_orient_matrix_UB_13      -0.0342045000
_diffrn_orient_matrix_UB_21      -0.0690348000
_diffrn_orient_matrix_UB_22      0.0025472000
_diffrn_orient_matrix_UB_23      0.0376131000
_diffrn_orient_matrix_UB_31      0.0315242000
_diffrn_orient_matrix_UB_32      0.0879757000
_diffrn_orient_matrix_UB_33      0.0155677000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                690
_reflns_number_total             924
_reflns_odcompleteness_completeness 98.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.823
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.222
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         924
_refine_ls_number_restraints     79
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0815
_refine_ls_restrained_S_all      1.175
_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)+(0.1556P)²+0.9865P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2282
_refine_ls_wR_factor_ref         0.2448
_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,H) groups
2. Restrained distances
 C3-C6
 1.45 with sigma of 0.02
 Br1-C6
 1.89 with sigma of 0.02
 C6-C2
 2.7 with sigma of 0.02
3. Restrained planarity
 Fe1, C1, C5, C2, C4, C3, C6, Br1
 with sigma of 0.1
4. Rigid bond restraints
 N1, C1, C2, C3, C4, C5, C6, Br1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(Br1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
6. Others
 Fixed Sof: Br1(0.25) C6(0.25) H6(0.25) N1(0.25) C1(0.25) H1(0.25) C2(0.25)
 H2(0.25) C3(0.25) C4(0.25) H4(0.25) C5(0.25) H5(0.25) O2(0.25) H2a(0.25)
 H2b(0.25) O1(0.25) H1a(0.25) H1b(0.25)
7.a Riding coordinates:
 O2(H2a,H2b), O1(H1a,H1b)
7.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C1(H1), C2(H2), C4(H4), C5(H5)
7.c Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.0000 -1.0000 1.0000 0.0186(5) Uani 1 8 d S T P . .
Fe1 Fe 0.5000 -1.5000 1.0000 0.0193(6) Uani 1 8 d S T P . .
N2 N 0.6947(12) -1.3044(12) 1.0000 0.0283(19) Uani 1 2 d S T P . .
C7 C 0.8038(13) -1.1959(13) 1.0000 0.0221(19) Uani 1 2 d S T P . .
Br1 Br 0.5075(19) -1.8159(14) 0.4992(15) 0.204(5) Uani 0.25 1 d D U . A -1
C6 C 0.512(5) -1.560(3) 0.5314(16) 0.105(10) Uani 0.25 1 d D U . A -1
H6 H 0.5153 -1.4594 0.4884 0.126 Uiso 0.25 1 calc R . . A -1
N1 N 0.5040(19) -1.496(6) 0.8485(10) 0.039(3) Uani 0.25 1 d . U . A -1
C1 C 0.5020(15) -1.676(5) 0.8128(16) 0.059(9) Uani 0.25 1 d G U . A -1
H1 H 0.4992 -1.7740 0.8575 0.070 Uiso 0.25 1 calc R . . A -1
C2 C 0.504(2) -1.709(4) 0.7102(18) 0.073(10) Uani 0.25 1 d DG U . A -1
H2 H 0.5028 -1.8295 0.6863 0.087 Uiso 0.25 1 calc R . . A -1
C3 C 0.508(4) -1.562(4) 0.6433(10) 0.087(10) Uani 0.25 1 d DG U . A -1
C4 C 0.510(5) -1.382(4) 0.6790(15) 0.083(10) Uani 0.25 1 d G U . A -1
H4 H 0.5131 -1.2839 0.6342 0.099 Uiso 0.25 1 calc R . . A -1
C5 C 0.508(5) -1.349(5) 0.7816(18) 0.059(8) Uani 0.25 1 d G U . A -1
H5 H 0.5095 -1.2285 0.8054 0.071 Uiso 0.25 1 calc R . . A -1
O2 O 0.999(19) -1.091(8) 0.708(4) 0.18(4) Uani 0.25 1 d . U . B -1
H2A H 0.9374 -0.9985 0.6882 0.276 Uiso 0.25 1 d R . . B -1
H2B H 1.0653 -1.1208 0.6582 0.276 Uiso 0.25 1 d R . . B -1
O1 O 0.983(12) -1.479(17) 0.783(6) 0.18(4) Uani 0.25 1 d . . . C -1
H1A H 0.9075 -1.4110 0.8149 0.277 Uiso 0.25 1 d R . . C -1
H1B H 1.0129 -1.4271 0.7285 0.277 Uiso 0.25 1 d R . . C -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 0.0139(6) 0.0139(6) 0.0280(9) 0.000 0.000 0.000
Fe1 0.0123(8) 0.0123(8) 0.0333(15) 0.000 0.000 0.000
N2 0.019(4) 0.022(4) 0.044(5) 0.000 0.000 0.003(3)
C7 0.016(4) 0.013(4) 0.037(5) 0.000 0.000 0.003(3)
Br1 0.395(15) 0.141(7) 0.077(4) -0.059(7) 0.007(14) -0.006(7)
C6 0.110(15) 0.106(10) 0.098(12) 0.008(9) -0.001(10) -0.001(10)
N1 0.031(8) 0.044(8) 0.041(6) -0.001(9) 0.001(10) 0.001(10)
C1 0.062(13) 0.057(11) 0.056(10) -0.007(9) -0.006(10) 0.000(9)
C2 0.080(14) 0.076(13) 0.062(11) -0.007(9) 0.005(10) 0.002(10)
C3 0.088(15) 0.083(12) 0.090(11) 0.004(8) 0.001(10) -0.004(10)
C4 0.089(15) 0.085(13) 0.074(11) 0.003(10) 0.001(10) 0.001(10)
C5 0.062(13) 0.054(12) 0.062(10) 0.005(8) 0.001(9) -0.003(9)
O2 0.06(3) 0.26(10) 0.23(6) 0.03(5) -0.02(6) 0.00(9)
O1 0.11(4) 0.28(9) 0.17(5) 0.13(6) 0.10(4) 0.07(4)

_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 C7 2.011(10) 5_737 ?
Pd1 C7 2.011(10) 7_757 ?
Pd1 C7 2.011(10) 3_535 ?
Pd1 C7 2.011(10) . ?
Fe1 N2 2.002(9) 5_627 ?
Fe1 N2 2.002(9) 3_435 ?
Fe1 N2 2.002(9) . ?
Fe1 N2 2.002(9) 7_747 ?
Fe1 N1 2.023(14) . ?
N2 C7 1.116(15) . ?
Br1 C6 1.904(19) . ?
C6 C3 1.494(16) . ?
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
C1 C2 1.3900 . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?

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
C7 Pd1 C7 90.000(3) 5_737 7_757 ?
C7 Pd1 C7 90.000(1) 5_737 3_535 ?
C7 Pd1 C7 180.0 7_757 3_535 ?
C7 Pd1 C7 180.0 5_737 . ?
C7 Pd1 C7 90.000(1) 7_757 . ?
C7 Pd1 C7 90.000(2) 3_535 . ?
N2 Fe1 N2 90.000(1) 5_627 7_747 ?
N2 Fe1 N2 90.000(1) 5_627 3_435 ?
N2 Fe1 N2 89.999(1) 7_747 . ?
N2 Fe1 N2 180.0 7_747 3_435 ?
N2 Fe1 N2 180.0 5_627 . ?
N2 Fe1 N2 90.001(1) 3_435 . ?
N2 Fe1 N1 91.2(9) 5_627 . ?
N2 Fe1 N1 88.8(9) . . ?
N2 Fe1 N1 90.0(9) 7_747 . ?
N2 Fe1 N1 90.0(9) 3_435 . ?
C7 N2 Fe1 179.7(9) . . ?
N2 C7 Pd1 179.9(9) . . ?
C3 C6 Br1 102.5(14) . . ?
C1 N1 Fe1 109(2) . . ?
C1 N1 C5 120.0 . . ?
C5 N1 Fe1 131(2) . . ?
N1 C1 C2 120.0 . . ?
C3 C2 C1 120.0 . . ?
C2 C3 C6 130.5(16) . . ?
C2 C3 C4 120.0 . . ?
C4 C3 C6 109.5(16) . . ?
C5 C4 C3 120.0 . . ?
C4 C5 N1 120.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1B O2 0.85 2.45 2.99(12) 121.6 .

_iucr_refine_instructions_details 
;

    cbrpd100k1@.res created by SHELXL-2014/7

TITL cbrpd100k1@_a.res in P4/m
REM Old TITL cbrpd100k1@_a.res in P4/m
REM SHELXT solution in P4/m
REM R1 0.162, Rweak 0.017, Alpha 0.049, Orientation as input
REM Formula found by SHELXT: C2 Fe N12 Pd
CELL 0.71073 7.2533 7.2533 13.3464 90 90 90
ZERR 1 0.0005 0.0005 0.002 0 0 0
LATT 1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SFAC C H Br Fe N O Pd
UNIT 16 18 2 1 6 4 1
EQIV $1 -1-Y,-2+X,+Z
DFIX 1.45 C3 C6
DFIX 1.89 Br1 C6
DFIX 2.7 C6 C2
FLAT Fe1 C1 C5 C2 C4 C3 C6 Br1
DELU 0.01 0.1 N1 C1 C2 C3 C4 C5 C6 Br1
ISOR 0.01 0.02 N1 C1 C2 C3 C4 C5 C6 Br1
ISOR O2
 
L.S. 54 0 0
PLAN  20
SIZE 0.1 0.1 0.05
HTAB C5 O1_$1
HTAB O1 O2
list 4
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\cbRpd100k1@.hkl">
REM </olex2.extras>
 
WGHT    0.155600    0.986500
FVAR       0.75848
PD1   7    1.000000   -1.000000    1.000000    10.12500    0.01390    0.01390 =
         0.02800    0.00000    0.00000    0.00000
FE1   4    0.500000   -1.500000    1.000000    10.12500    0.01231    0.01231 =
         0.03330    0.00000    0.00000    0.00000
N2    5    0.694662   -1.304367    1.000000    10.50000    0.01917    0.02168 =
         0.04418    0.00000    0.00000    0.00277
C7    1    0.803816   -1.195884    1.000000    10.50000    0.01564    0.01326 =
         0.03726    0.00000    0.00000    0.00346
PART -1
BR1   3    0.507527   -1.815857    0.499178    10.25000    0.39513    0.14072 =
         0.07705   -0.05923    0.00732   -0.00579
C6    1    0.511859   -1.560136    0.531431    10.25000    0.11044    0.10591 =
         0.09803    0.00829   -0.00130   -0.00051
AFIX  43
H6    2    0.515312   -1.459389    0.488372    10.25000   -1.20000
AFIX  66
N1    5    0.504011   -1.495767    0.848454    10.25000    0.03083    0.04375 =
         0.04136   -0.00097    0.00063    0.00076
C1    1    0.501995   -1.675798    0.812778    10.25000    0.06247    0.05732 =
         0.05614   -0.00668   -0.00579    0.00042
AFIX  43
H1    2    0.499208   -1.774035    0.857532    10.25000   -1.20000
AFIX  65
C2    1    0.504146   -1.709002    0.710212    10.25000    0.07970    0.07573 =
         0.06228   -0.00731    0.00483    0.00165
AFIX  43
H2    2    0.502798   -1.829455    0.686343    10.25000   -1.20000
AFIX  65
C3    1    0.508312   -1.562175    0.643322    10.25000    0.08791    0.08296 =
         0.08951    0.00355    0.00097   -0.00375
C4    1    0.510327   -1.382144    0.678997    10.25000    0.08922    0.08469 =
         0.07365    0.00272    0.00074    0.00051
AFIX  43
H4    2    0.513115   -1.283907    0.634243    10.25000   -1.20000
AFIX  65
C5    1    0.508177   -1.348937    0.781562    10.25000    0.06187    0.05430 =
         0.06213    0.00545    0.00076   -0.00334
AFIX  43
H5    2    0.509525   -1.228484    0.805431    10.25000   -1.20000
AFIX   0
 
O2    6    0.999140   -1.091084    0.708252    10.25000    0.06261    0.26050 =
         0.22896    0.02770   -0.02342    0.00153
AFIX   3
H2A   2    0.937450   -0.998544    0.688202    10.25000   -1.50000
H2B   2    1.065269   -1.120844    0.658222    10.25000   -1.50000
AFIX   0
 
O1    6    0.983305   -1.478912    0.783300    10.25000    0.11311    0.27572 =
         0.16603    0.13306    0.10024    0.07411
AFIX   3
H1A   2    0.907525   -1.410962    0.814870    10.25000   -1.50000
H1B   2    1.012935   -1.427052    0.728490    10.25000   -1.50000
AFIX   0
HKLF 4
 
REM  cbrpd100k1@_a.res in P4/m
REM R1 =  0.0815 for     690 Fo > 4sig(Fo)  and  0.1061 for all     924 data
REM     95 parameters refined using     79 restraints
 
END  
     
WGHT      0.1555      0.9860 

REM Highest difference peak  2.823,  deepest hole -1.374,  1-sigma level  0.222
Q1    1   0.6771 -1.9926  0.5000  10.50000  0.05    1.88
Q2    1   0.3117 -1.7749  0.5000  10.50000  0.05    1.60
Q3    1   0.7023 -1.7710  0.5000  10.50000  0.05    1.58
Q4    1   0.5000 -2.0000  0.5000  10.25000  0.05    1.12
Q5    1   0.8204 -1.1464  1.0000  10.50000  0.05    1.02
Q6    1   1.0000 -1.0000  0.9479  10.25000  0.05    0.77
Q7    1   0.5000 -1.5000  0.8210  10.25000  0.05    0.74
Q8    1   1.0000 -1.0000  1.1401  10.25000  0.05    0.63
Q9    1   1.0000 -1.5000  0.8042  10.50000  0.05    0.63
Q10   1   0.9941 -0.8372  0.9627  11.00000  0.05    0.60
Q11   1   0.6707 -1.1736  1.0000  10.50000  0.05    0.60
Q12   1   1.2241 -1.2402  0.6045  11.00000  0.05    0.59
Q13   1   0.4357 -1.6790  0.6965  11.00000  0.05    0.53
Q14   1   0.5248 -1.2107  1.0000  10.50000  0.05    0.50
Q15   1   0.5000 -1.5000  0.6364  10.25000  0.05    0.48
Q16   1   0.4645 -1.8399  0.7355  11.00000  0.05    0.47
Q17   1   0.5108 -1.8414  0.7330  11.00000  0.05    0.45
Q18   1   0.4973 -1.3745  0.7992  11.00000  0.05    0.42
Q19   1   0.6503 -1.3408  1.0000  10.50000  0.05    0.42
Q20   1   0.5732 -1.6168  0.5294  11.00000  0.05    0.41

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0815 for 690 Fo > 4sig(Fo) and 0.1061 for all 3021 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 2.82, deepest hole -1.37
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.1061
  REM R1_gt = 0.0815
  REM wR_ref = 0.2448
  REM GOOF = 1.121
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3021
  REM Reflections_gt = 690
  REM Parameters = n/a
  REM Hole = -1.37
  REM Peak = 2.82
  REM Flack = n/a

  
;
_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 1.902
_oxdiff_exptl_absorpt_empirical_full_min 0.612
####################################################################### 
# 
# 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_2023231
_database_code_depnum_ccdc_archive 'CCDC 2023231'
_audit_update_record             
;
2020-11-29 deposited with the CCDC.	2020-12-22 downloaded from the CCDC.
;
_audit_creation_date             2020-11-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H10 Br2 Fe N6 Pd, 4(H2 O)'
_chemical_formula_sum            'C16 H18 Br2 Fe N6 O4 Pd'
_chemical_formula_weight         680.43
_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'
Br Br -0.2901 2.4595 '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      tetragonal
_space_group_IT_number           83
_space_group_name_H-M_alt        'P 4/m'
_space_group_name_Hall           '-P 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'

_cell_length_a                   7.4285(7)
_cell_length_b                   7.4285(7)
_cell_length_c                   13.648(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     753.1(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    979
_cell_measurement_temperature    249.99(11)
_cell_measurement_theta_max      29.3040
_cell_measurement_theta_min      4.0240
_shelx_estimated_absorpt_T_max   0.834
_shelx_estimated_absorpt_T_min   0.705
_exptl_absorpt_coefficient_mu    3.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4906
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.505
_diffrn_reflns_theta_min         3.879
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      249.99(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -33.00  13.00   0.50   70.00    --    0.10 -63.00  -1.00   92
  2  ω    -52.00 -27.00   0.50   70.00    --    0.10 -82.00   0.00   50
  3  ω    -63.00  26.00   0.50   70.00    --    0.10 -82.00 -30.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0393812000
_diffrn_orient_matrix_UB_12      -0.0019004000
_diffrn_orient_matrix_UB_13      0.0473185000
_diffrn_orient_matrix_UB_21      0.0868777000
_diffrn_orient_matrix_UB_22      -0.0043980000
_diffrn_orient_matrix_UB_23      -0.0214393000
_diffrn_orient_matrix_UB_31      0.0046268000
_diffrn_orient_matrix_UB_32      0.0953910000
_diffrn_orient_matrix_UB_33      -0.0001184000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                839
_reflns_number_total             1009
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.853
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.201
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1009
_refine_ls_number_restraints     232
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0680
_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)+(0.1613P)²+0.0142P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2145
_refine_ls_wR_factor_ref         0.2230
_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,H) groups
2. Restrained distances
 C6-Br1
 1.9 with sigma of 0.02
 C5-C4
 1.38 with sigma of 0.02
 C5-C3
 2.38 with sigma of 0.02
 C4-C3
 1.38 with sigma of 0.02
 C3-Br1
 2.8 with sigma of 0.02
 N1-C5
 1.38 with sigma of 0.02
 C4-N1
 2.38 with sigma of 0.02
 C6-C3
 1.5 with sigma of 0.02
 C5-Fe1 \\sim Fe1-C1
 with sigma of 0.01
3. Restrained planarity
 N1, C5, C4, C3, C6, Br1
 with sigma of 0.01
4. Rigid bond restraints
 C3, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
Br1 \\sim N1 \\sim C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1 \\sim C6: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C5 \\sim C4 \\sim C3 \\sim C2 \\sim C1 \\sim C6 \\sim C7: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C6)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 Br1, N1, C5, C4, C3, C2, C1, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
7. Others
 Fixed Sof: Br1(0.25) N1(0.25) C5(0.25) H5(0.25) C4(0.25) H4(0.25) C3(0.25)
 C2(0.25) H2(0.25) C1(0.25) H1(0.25) C6(0.25) H6(0.25) O1(0.25) H1A(0.25)
 H1B(0.25) O2(0.25) H2A(0.25) H2B(0.25)
8.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B)
8.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C2(H2), C1(H1), C6(H6)
8.c Fitted hexagon refined as free rotating group:
 N1(C5,C4,C3,C2,C1)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.0000 1.0000 0.5000 0.0250(5) Uani 1 8 d S T P . .
Br1 Br 0.4989(14) 0.1915(10) -0.0015(16) 0.211(4) Uani 0.25 1 d D U . A -1
Fe1 Fe 0.5000 0.5000 0.5000 0.0267(5) Uani 1 8 d DS T P . .
N1 N 0.502(6) 0.4828(17) 0.3443(8) 0.063(3) Uani 0.25 1 d D U . A -1
C5 C 0.483(6) 0.6372(19) 0.2876(9) 0.090(4) Uani 0.25 1 d DG U . A -1
H5 H 0.4759 0.7493 0.3176 0.108 Uiso 0.25 1 calc R . . A -1
C4 C 0.476(5) 0.624(3) 0.1861(8) 0.095(4) Uani 0.25 1 d DG U . A -1
H4 H 0.4639 0.7272 0.1482 0.114 Uiso 0.25 1 calc R . . A -1
C3 C 0.487(3) 0.456(3) 0.1413(8) 0.096(4) Uani 0.25 1 d DG U . A -1
C2 C 0.505(4) 0.302(3) 0.1979(10) 0.095(4) Uani 0.25 1 d G U . A -1
H2 H 0.5128 0.1897 0.1679 0.114 Uiso 0.25 1 calc R . . A -1
C1 C 0.513(6) 0.3151(19) 0.2994(10) 0.090(4) Uani 0.25 1 d DG U . A -1
H1 H 0.5248 0.2118 0.3374 0.108 Uiso 0.25 1 calc R . . A -1
N2 N 0.7018(10) 0.7041(10) 0.5000 0.0413(17) Uani 1 2 d S T P A .
C6 C 0.480(3) 0.434(3) 0.0339(14) 0.099(4) Uani 0.25 1 d D U . A -1
H6 H 0.4677 0.5286 -0.0103 0.119 Uiso 0.25 1 calc R . . A -1
C7 C 0.8087(11) 0.8102(12) 0.5000 0.0363(17) Uani 1 2 d S TU P . .
O1 O 0.538(7) -0.020(8) 0.278(4) 0.134(17) Uani 0.25 1 d . U . B -1
H1A H 0.4823 -0.0145 0.2234 0.200 Uiso 0.25 1 d R . . B -1
H1B H 0.4810 -0.0996 0.3103 0.200 Uiso 0.25 1 d R . . B -1
O2 O 0.930(12) -0.029(7) 0.193(3) 0.21(4) Uani 0.25 1 d . U . C -1
H2A H 0.8351 -0.0225 0.2281 0.315 Uiso 0.25 1 d R . . C -1
H2B H 0.9491 0.0727 0.1664 0.315 Uiso 0.25 1 d R . . C -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 0.0138(5) 0.0138(5) 0.0472(7) 0.000 0.000 0.000
Br1 0.364(10) 0.130(4) 0.140(5) -0.049(8) 0.010(12) -0.026(5)
Fe1 0.0139(6) 0.0139(6) 0.0522(12) 0.000 0.000 0.000
N1 0.062(6) 0.061(6) 0.066(5) -0.006(6) 0.002(7) -0.004(6)
C5 0.095(6) 0.086(6) 0.088(5) -0.004(5) 0.003(5) -0.003(5)
C4 0.101(6) 0.091(6) 0.092(6) -0.004(5) 0.001(5) -0.003(5)
C3 0.102(6) 0.092(6) 0.094(5) -0.003(5) 0.002(5) -0.003(5)
C2 0.101(6) 0.091(6) 0.091(6) -0.004(5) 0.003(5) -0.004(5)
C1 0.096(6) 0.087(6) 0.089(5) -0.004(5) 0.001(5) -0.005(5)
N2 0.022(3) 0.020(3) 0.082(5) 0.000 0.000 -0.008(3)
C6 0.109(6) 0.093(6) 0.095(5) -0.005(5) 0.002(5) -0.004(5)
C7 0.021(3) 0.024(3) 0.064(5) 0.000 0.000 0.003(3)
O1 0.13(3) 0.13(2) 0.14(2) 0.026(17) 0.022(17) -0.007(19)
O2 0.25(12) 0.05(2) 0.33(5) 0.00(4) -0.05(6) -0.04(4)

_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 C7 2.002(9) 5_776 ?
Pd1 C7 2.002(9) 7_576 ?
Pd1 C7 2.002(9) 3_755 ?
Pd1 C7 2.002(9) . ?
Br1 C6 1.873(18) . ?
Fe1 N1 2.129(11) . ?
Fe1 N2 2.132(7) 7_566 ?
Fe1 N2 2.132(7) . ?
Fe1 N2 2.132(7) 3_655 ?
Fe1 N2 2.132(7) 5_666 ?
N1 C5 1.3900 . ?
N1 C1 1.3900 . ?
C5 C4 1.3900 . ?
C4 C3 1.3900 . ?
C3 C2 1.3900 . ?
C3 C6 1.475(18) . ?
C2 C1 1.3900 . ?
N2 C7 1.118(14) . ?

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
C7 Pd1 C7 90.0 5_776 7_576 ?
C7 Pd1 C7 180.0 7_576 3_755 ?
C7 Pd1 C7 90.000(1) 3_755 . ?
C7 Pd1 C7 90.000(1) 7_576 . ?
C7 Pd1 C7 90.000(2) 5_776 3_755 ?
C7 Pd1 C7 180.0 5_776 . ?
N1 Fe1 N2 92.2(10) . . ?
N1 Fe1 N2 92.6(9) . 3_655 ?
N1 Fe1 N2 87.4(9) . 7_566 ?
N1 Fe1 N2 87.8(10) . 5_666 ?
N2 Fe1 N2 90.001(2) . 7_566 ?
N2 Fe1 N2 180.0 . 5_666 ?
N2 Fe1 N2 180.0 7_566 3_655 ?
N2 Fe1 N2 90.000(2) 5_666 3_655 ?
N2 Fe1 N2 90.000(1) 5_666 7_566 ?
N2 Fe1 N2 89.999(1) . 3_655 ?
C5 N1 Fe1 120.4(4) . . ?
C5 N1 C1 120.0 . . ?
C1 N1 Fe1 119.6(4) . . ?
C4 C5 N1 120.0 . . ?
C5 C4 C3 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 C6 122.3(14) . . ?
C2 C3 C6 117.7(14) . . ?
C3 C2 C1 120.0 . . ?
C2 C1 N1 120.0 . . ?
C7 N2 Fe1 179.5(9) . . ?
C3 C6 Br1 111.2(15) . . ?
N2 C7 Pd1 180.0(9) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2 Br1 0.93 2.31 2.84(2) 115.6 .
C2 H2 O1 0.93 2.17 2.64(6) 110.2 .
C1 H1 O1 0.93 1.91 2.52(6) 120.9 .

_iucr_refine_instructions_details 
;

    exp_1252@.res created by SHELXL-2014/7

TITL exp_1252@_a.res in P4/m
REM Old TITL exp_1252@ in P4/m #83
REM SHELXT solution in P4/m
REM R1 0.180, Rweak 0.027, Alpha 0.093, Orientation as input
REM Formula found by SHELXT: O2 N4 O1 Fe Pd
CELL 0.71073 7.4285 7.4285 13.6479 90 90 90
ZERR 1 0.0007 0.0007 0.0031 0 0 0
LATT 1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SFAC C H Br Fe N O Pd
UNIT 16 18 2 1 6 4 1
EQIV $1 1-X,1-Y,+Z
DFIX 1.9 C6 Br1
DFIX 1.38 C5 C4
DFIX 2.38 C5 C3
DFIX 1.38 C4 C3
DFIX 2.8 C3 Br1
DFIX 1.38 N1 C5
DFIX 2.38 C4 N1
DFIX 1.5 C6 C3
SADI 0.01 C5 Fe1 Fe1 C1
FLAT 0.01 N1 C5 C4 C3 C6 Br1
DELU 0.001 0.001 C3 C6
SIMU 0.01 0.02 2 Br1 N1 C5 C4 C3 C2 C1 C6
SIMU 0.01 0.02 3.8 $C
RIGU 0.01 0.01 Br1 N1 C5 C4 C3 C2 C1 C6
ISOR 0.01 0.02 Br1 N1 C5 C4 C3 C2 C1 C6
ISOR O2
ISOR 0.01 0.02 O1
 
L.S. 54 0 0
PLAN  20
SIZE 0.1 0.1 0.05
HTAB C5 O1_$1
HTAB C2 Br1
HTAB C1 O1
HTAB C2 O1
list 4
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\exp_1252@.hkl">
REM </olex2.extras>
 
WGHT    0.161300    0.014200
FVAR       0.67538
PD1   7    1.000000    1.000000    0.500000    10.12500    0.01381    0.01381 =
         0.04724    0.00000    0.00000    0.00000
PART -1
BR1   3    0.498904    0.191462   -0.001521    10.25000    0.36386    0.12981 =
         0.14022   -0.04938    0.01021   -0.02578
PART 0
FE1   4    0.500000    0.500000    0.500000    10.12500    0.01390    0.01390 =
         0.05223    0.00000    0.00000    0.00000
PART -1
AFIX  66
N1    5    0.501556    0.482765    0.344288    10.25000    0.06236    0.06121 =
         0.06623   -0.00625    0.00190   -0.00437
C5    1    0.483299    0.637157    0.287613    10.25000    0.09512    0.08581 =
         0.08794   -0.00413    0.00258   -0.00331
AFIX  43
H5    2    0.475912    0.749321    0.317614    10.25000   -1.20000
AFIX  65
C4    1    0.476081    0.623909    0.186097    10.25000    0.10136    0.09132 =
         0.09163   -0.00355    0.00128   -0.00347
AFIX  43
H4    2    0.463865    0.727208    0.148178    10.25000   -1.20000
AFIX  65
C3    1    0.487121    0.456267    0.141257    10.25000    0.10178    0.09179 =
         0.09416   -0.00253    0.00180   -0.00330
C2    1    0.505379    0.301873    0.197930    10.25000    0.10137    0.09139 =
         0.09136   -0.00393    0.00305   -0.00380
AFIX  43
H2    2    0.512765    0.189710    0.167928    10.25000   -1.20000
AFIX  65
C1    1    0.512597    0.315119    0.299446    10.25000    0.09578    0.08682 =
         0.08859   -0.00410    0.00115   -0.00454
AFIX  43
H1    2    0.524813    0.211819    0.337364    10.25000   -1.20000
AFIX   0
PART 0
N2    5    0.701838    0.704109    0.500000    10.50000    0.02201    0.01969 =
         0.08222    0.00000    0.00000   -0.00789
PART -1
C6    1    0.479971    0.434232    0.033939    10.25000    0.10915    0.09321 =
         0.09483   -0.00550    0.00172   -0.00424
AFIX  43
H6    2    0.467666    0.528588   -0.010343    10.25000   -1.20000
AFIX   0
PART 0
C7    1    0.808659    0.810150    0.500000    10.50000    0.02097    0.02351 =
         0.06442    0.00000    0.00000    0.00303
PART -1
O1    6    0.537737   -0.020241    0.277772    10.25000    0.12957    0.13246 =
         0.13892    0.02647    0.02159   -0.00739
AFIX   3
H1A   2    0.482267   -0.014451    0.223392    10.25000   -1.50000
H1B   2    0.480967   -0.099631    0.310282    10.25000   -1.50000
AFIX   0
 
O2    6    0.929563   -0.028780    0.193092    10.25000    0.24586    0.05498 =
         0.32969   -0.00456   -0.04883   -0.04181
AFIX   3
H2A   2    0.835123   -0.022480    0.228092    10.25000   -1.50000
H2B   2    0.949103    0.072741    0.166382    10.25000   -1.50000
AFIX   0
HKLF 4
 
REM  exp_1252@_a.res in P4/m
REM R1 =  0.0680 for     839 Fo > 4sig(Fo)  and  0.0825 for all    1009 data
REM     95 parameters refined using    232 restraints
 
END  
     
WGHT      0.1612      0.0142 

REM Highest difference peak  1.853,  deepest hole -1.286,  1-sigma level  0.201
Q1    1   0.7011  0.2401  0.0000  10.50000  0.05    1.29
Q2    1   0.2916  0.2356  0.0000  10.50000  0.05    1.08
Q3    1   0.5384  0.0036  0.0000  10.50000  0.05    0.68
Q4    1   0.6817  0.0099  0.0000  10.50000  0.05    0.65
Q5    1   0.5036  0.1612  0.2255  11.00000  0.05    0.64
Q6    1   1.0000  1.0000  0.4268  10.25000  0.05    0.64
Q7    1   0.4932  0.0393  0.0000  10.50000  0.05    0.57
Q8    1   0.8149  0.9444  0.5000  10.50000  0.05    0.55
Q9    1   0.2393  0.7584  0.1037  11.00000  0.05    0.55
Q10   1   0.9329  0.8149  0.5000  10.50000  0.05    0.45
Q11   1   0.9937  1.1272  0.4397  11.00000  0.05    0.42
Q12   1   0.5000  0.5000  0.4259  10.25000  0.05    0.40
Q13   1   0.3788  0.5876  0.1812  11.00000  0.05    0.39
Q14   1   0.5465  0.6353  0.2888  11.00000  0.05    0.35
Q15   1   0.3126  0.6814  0.1026  11.00000  0.05    0.35
Q16   1   0.6696  0.6345  0.5000  10.50000  0.05    0.34
Q17   1   0.8947  0.0864  0.1595  11.00000  0.05    0.33
Q18   1   0.3937  0.3956  0.0385  11.00000  0.05    0.33
Q19   1   0.9202  0.5100  0.5000  10.50000  0.05    0.31
Q20   1   1.0000  0.0000  0.3306  10.25000  0.05    0.31

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0680 for 839 Fo > 4sig(Fo) and 0.0825 for all 4906 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.85, deepest hole -1.29
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0825
  REM R1_gt = 0.0680
  REM wR_ref = 0.2230
  REM GOOF = 1.125
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 4906
  REM Reflections_gt = 839
  REM Parameters = n/a
  REM Hole = -1.29
  REM Peak = 1.85
  REM Flack = n/a

  
;
_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 2.164
_oxdiff_exptl_absorpt_empirical_full_min 0.482
####################################################################### 
# 
# 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_1_95K
_database_code_depnum_ccdc_archive 'CCDC 2023230'
loop_
_audit_author_name
_audit_author_address
'Yue Li' 'Xiamen University'
_audit_update_record             
;
2020-08-13 deposited with the CCDC.	2020-12-22 downloaded from the CCDC.
;
_audit_creation_date             2020-07-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H10 Br2 Fe N6 Pt, 4(H2 O)'
_chemical_formula_sum            'C16 H18 Br2 Fe N6 O4 Pt'
_chemical_formula_weight         769.12
_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'
Br Br -0.2901 2.4595 '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      tetragonal
_space_group_IT_number           83
_space_group_name_H-M_alt        'P 4/m'
_space_group_name_Hall           '-P 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'

_cell_length_a                   7.3121(5)
_cell_length_b                   7.3121(5)
_cell_length_c                   13.3878(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     715.80(14)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1292
_cell_measurement_temperature    95(1)
_cell_measurement_theta_max      27.6370
_cell_measurement_theta_min      4.1340
_shelx_estimated_absorpt_T_max   0.684
_shelx_estimated_absorpt_T_min   0.494
_exptl_absorpt_coefficient_mu    8.205
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3800
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.295
_diffrn_reflns_theta_min         3.941
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      95(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     31.00  58.00   0.50   70.00    --    0.10  16.00 -64.00   54
  2  ω    -50.00  -8.00   0.50   70.00    --    0.10 -82.00-180.00   84
  3  ω    -56.00   7.00   0.50   70.00    --    0.10 -82.00-120.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0932420000
_diffrn_orient_matrix_UB_12      -0.0179849000
_diffrn_orient_matrix_UB_13      0.0104438000
_diffrn_orient_matrix_UB_21      -0.0174985000
_diffrn_orient_matrix_UB_22      -0.0100844000
_diffrn_orient_matrix_UB_23      -0.0518223000
_diffrn_orient_matrix_UB_31      0.0195182000
_diffrn_orient_matrix_UB_32      -0.0949512000
_diffrn_orient_matrix_UB_33      0.0033966000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                908
_reflns_number_total             949
_reflns_odcompleteness_completeness 99.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.681
_refine_diff_density_min         -2.197
_refine_diff_density_rms         0.287
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         949
_refine_ls_number_restraints     77
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0561
_refine_ls_restrained_S_all      1.113
_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)+(0.1221P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1554
_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,H) groups
2. Restrained distances
 N1-Fe1
 2 with sigma of 0.02
 N1-C1 = C2-C3 = C4-C5
 1.38 with sigma of 0.02
 C6-Br1
 1.9 with sigma of 0.02
 C3-C6
 1.5 with sigma of 0.02
 C2-C6
 2.55 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C4, C5, N1, Br1, C6
 with sigma of 0.1
4. Rigid bond restraints
 C1, C2, C3, C4, C5, N1, Br1, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(Br1) \\sim Ueq, Uanis(C6)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Fixed Sof: C1(0.25) H1(0.25) C2(0.25) H2(0.25) C3(0.25) C4(0.25) H4(0.25)
 C5(0.25) H5(0.25) N1(0.25) Br1(0.25) C6(0.25) H6(0.25) O1(0.25) H1a(0.25)
 H1b(0.25) O2(0.25) H2a(0.25) H2b(0.25)
7.a Riding coordinates:
 O1(H1a,H1b), O2(H2a,H2b)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6)
7.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,N1)
;
_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 1.0000 0.0000 0.5000 0.0237(3) Uani 1 8 d S T P A .
Fe1 Fe 0.5000 0.5000 0.5000 0.0218(6) Uani 1 8 d DS T P . .
N2 N 0.6963(14) 0.3032(13) 0.5000 0.032(2) Uani 1 2 d S T P A .
C7 C 0.8057(15) 0.1932(15) 0.5000 0.027(2) Uani 1 2 d S T P . .
C1 C 0.321(6) 0.501(9) 0.3088(19) 0.066(7) Uani 0.25 1 d D U . A -1
H1 H 0.2173 0.5062 0.3516 0.079 Uiso 0.25 1 calc R . . A -1
C2 C 0.297(4) 0.494(6) 0.206(2) 0.072(8) Uani 0.25 1 d DG U . A -1
H2 H 0.1770 0.4938 0.1784 0.086 Uiso 0.25 1 calc R . . A -1
C3 C 0.448(4) 0.487(5) 0.1431(9) 0.074(8) Uani 0.25 1 d DG U . A -1
C4 C 0.623(4) 0.487(7) 0.1834(18) 0.073(7) Uani 0.25 1 d DG U . A -1
H4 H 0.7268 0.4821 0.1405 0.088 Uiso 0.25 1 calc R . . A -1
C5 C 0.647(6) 0.494(9) 0.286(2) 0.068(7) Uani 0.25 1 d DG U . A -1
H5 H 0.7671 0.4945 0.3138 0.082 Uiso 0.25 1 calc R . . A -1
N1 N 0.496(7) 0.502(10) 0.3490(9) 0.043(3) Uani 0.25 1 d DG U . A -1
Br1 Br 0.190(2) 0.499(2) -0.0031(14) 0.218(6) Uani 0.25 1 d D U . A -1
C6 C 0.436(3) 0.457(7) 0.0329(17) 0.097(9) Uani 0.25 1 d D U . A -1
H6 H 0.5330 0.4241 -0.0106 0.116 Uiso 0.25 1 calc R . . A -1
O1 O 0.988(17) 0.488(19) 0.284(5) 0.12(3) Uani 0.25 1 d . . . B -1
H1A H 0.9734 0.3700 0.2818 0.173 Uiso 0.25 1 d R . . B -1
H1B H 0.9153 0.5296 0.2376 0.173 Uiso 0.25 1 d R . . B -1
O2 O 1.002(12) 0.133(15) 0.195(8) 0.21(5) Uani 0.25 1 d . . . C -1
H2A H 0.9992 0.0183 0.2113 0.319 Uiso 0.25 1 d R . . C -1
H2B H 1.0519 0.1343 0.1357 0.319 Uiso 0.25 1 d R . . C -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 0.0199(3) 0.0199(3) 0.0315(5) 0.000 0.000 0.000
Fe1 0.0143(7) 0.0143(7) 0.0368(14) 0.000 0.000 0.000
N2 0.025(4) 0.021(4) 0.051(6) 0.000 0.000 -0.005(3)
C7 0.021(4) 0.021(4) 0.038(5) 0.000 0.000 -0.005(4)
C1 0.064(9) 0.069(13) 0.066(9) 0.004(10) -0.007(8) -0.004(10)
C2 0.069(10) 0.079(13) 0.068(9) 0.001(10) -0.012(7) -0.002(10)
C3 0.072(10) 0.079(14) 0.071(8) 0.004(10) -0.006(6) 0.003(10)
C4 0.071(9) 0.080(13) 0.068(8) 0.003(10) 0.009(7) 0.001(10)
C5 0.066(9) 0.072(13) 0.067(9) 0.000(10) 0.003(7) 0.001(10)
N1 0.053(8) 0.030(8) 0.046(6) 0.003(10) -0.003(7) 0.001(10)
Br1 0.182(9) 0.360(16) 0.112(6) 0.005(12) -0.105(8) 0.003(10)
C6 0.109(10) 0.100(14) 0.080(9) -0.008(10) 0.002(8) -0.008(10)
O1 0.08(4) 0.13(5) 0.14(5) 0.06(6) 0.04(5) 0.00(3)
O2 0.06(3) 0.31(13) 0.27(10) 0.01(9) 0.00(6) 0.01(8)

_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 C7 2.004(11) 7_666 ?
Pt1 C7 2.004(11) 5_756 ?
Pt1 C7 2.004(11) 3_645 ?
Pt1 C7 2.004(11) . ?
Fe1 N2 2.032(11) 7_566 ?
Fe1 N2 2.032(11) . ?
Fe1 N2 2.032(11) 5_666 ?
Fe1 N2 2.032(11) 3_655 ?
Fe1 N1 2.022(12) . ?
N2 C7 1.134(18) . ?
C1 C2 1.3900 . ?
C1 N1 1.3900 . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C3 C6 1.494(17) . ?
C4 C5 1.3900 . ?
C5 N1 1.3900 . ?
Br1 C6 1.89(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Pt1 C7 180.0(4) 7_666 3_645 ?
C7 Pt1 C7 90.001(2) 7_666 . ?
C7 Pt1 C7 89.999(2) 3_645 . ?
C7 Pt1 C7 90.000(2) 3_645 5_756 ?
C7 Pt1 C7 90.000(2) 7_666 5_756 ?
C7 Pt1 C7 180.0 5_756 . ?
N2 Fe1 N2 90.0 . 7_566 ?
N2 Fe1 N2 90.000(1) 3_655 5_666 ?
N2 Fe1 N2 180.0 7_566 3_655 ?
N2 Fe1 N2 180.0 . 5_666 ?
N2 Fe1 N2 90.000(2) 7_566 5_666 ?
N2 Fe1 N2 90.000(1) . 3_655 ?
N1 Fe1 N2 89.2(18) . 5_666 ?
N1 Fe1 N2 89.6(17) . 7_566 ?
N1 Fe1 N2 90.8(18) . . ?
N1 Fe1 N2 90.4(17) . 3_655 ?
C7 N2 Fe1 179.9(10) . . ?
N2 C7 Pt1 179.7(11) . . ?
C2 C1 N1 120.0 . . ?
C1 C2 C3 120.0 . . ?
C2 C3 C6 123.7(16) . . ?
C4 C3 C2 120.0 . . ?
C4 C3 C6 116.0(16) . . ?
C3 C4 C5 120.0 . . ?
N1 C5 C4 120.0 . . ?
C1 N1 Fe1 114(3) . . ?
C5 N1 Fe1 126(3) . . ?
C5 N1 C1 120.0 . . ?
C3 C6 Br1 106.6(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2 Br1 0.95 2.43 2.91(3) 110.6 .
C5 H5 O1 0.95 1.66 2.49(13) 143.3 .
O1 H1A O2 0.87 2.10 2.86(17) 145.7 .

_iucr_refine_instructions_details 
;

    cbrpt-95k.res created by SHELXL-2014/7

TITL cbrpt-95k_a.res in P4/m
REM Old TITL cbrpt-95k_a.res in P4/m
REM SHELXT solution in P4/m
REM R1 0.094, Rweak 0.151, Alpha 0.126, Orientation as input
REM Formula found by SHELXT: Br C8 N2 O2 Pt
CELL 0.71073 7.3121 7.3121 13.3878 90 90 90
ZERR 1 0.0005 0.0005 0.0018 0 0 0
LATT 1
SYMM -X,-Y,+Z
SYMM -Y,+X,+Z
SYMM +Y,-X,+Z
SFAC C H Br Fe N O Pt
UNIT 16 18 2 1 6 4 1
DFIX 2 N1 Fe1
DFIX 1.38 N1 C1 C2 C3 C4 C5
DFIX 1.9 C6 Br1
DFIX 1.5 C3 C6
DFIX 2.55 C2 C6
FLAT C1 C2 C3 C4 C5 N1 Br1 C6
DELU C1 C2 C3 C4 C5 N1 Br1 C6
ISOR 0.01 0.02 C1 C2 C3 C4 C5 N1 Br1 C6
 
L.S. 14
PLAN  20
SIZE 0.05 0.1 0.1
TEMP -178.1(10)
HTAB C2 Br1
HTAB C5 O1
HTAB O1 O2
list 4
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\CBrPt-95K.hkl">
REM </olex2.extras>
 
WGHT    0.122100
FVAR       0.55255
PT1   7    1.000000    0.000000    0.500000    10.12500    0.01986    0.01986 =
         0.03146    0.00000    0.00000    0.00000
FE1   4    0.500000    0.500000    0.500000    10.12500    0.01435    0.01435 =
         0.03684    0.00000    0.00000    0.00000
N2    5    0.696271    0.303219    0.500000    10.50000    0.02499    0.02051 =
         0.05056    0.00000    0.00000   -0.00528
C7    1    0.805661    0.193214    0.500000    10.50000    0.02064    0.02076 =
         0.03818    0.00000    0.00000   -0.00496
PART -1
AFIX  66
C1    1    0.320734    0.501316    0.308781    10.25000    0.06419    0.06868 =
         0.06569    0.00391   -0.00738   -0.00407
AFIX  43
H1    2    0.217307    0.506220    0.351643    10.25000   -1.20000
AFIX  65
C2    1    0.296802    0.493934    0.205861    10.25000    0.06873    0.07941 =
         0.06769    0.00144   -0.01157   -0.00246
AFIX  43
H2    2    0.177018    0.493793    0.178381    10.25000   -1.20000
AFIX  65
C3    1    0.448131    0.486759    0.143148    10.25000    0.07160    0.07863 =
         0.07075    0.00423   -0.00574    0.00270
C4    1    0.623394    0.486966    0.183355    10.25000    0.07094    0.07966 =
         0.06831    0.00259    0.00880    0.00111
AFIX  43
H4    2    0.726820    0.482063    0.140493    10.25000   -1.20000
AFIX  65
C5    1    0.647328    0.494348    0.286275    10.25000    0.06595    0.07228 =
         0.06703    0.00018    0.00265    0.00087
AFIX  43
H5    2    0.767113    0.494489    0.313754    10.25000   -1.20000
AFIX  65
N1    5    0.496000    0.501523    0.348989    10.25000    0.05291    0.03030 =
         0.04583    0.00333   -0.00309    0.00051
AFIX   0
BR1   3    0.189553    0.499450   -0.003063    10.25000    0.18232    0.35957 =
         0.11240    0.00492   -0.10515    0.00271
C6    1    0.435919    0.457407    0.032930    10.25000    0.10944    0.10014 =
         0.08008   -0.00751    0.00157   -0.00789
AFIX  43
H6    2    0.533014    0.424113   -0.010571    10.25000   -1.20000
AFIX   0
O1    6    0.987504    0.488033    0.284025    10.25000    0.07576    0.13169 =
         0.13827    0.06461    0.04278    0.00420
AFIX   3
H1A   2    0.973404    0.369953    0.281815    10.25000   -1.50000
H1B   2    0.915344    0.529563    0.237605    10.25000   -1.50000
AFIX   0
 
O2    6    1.002392    0.133323    0.194753    10.25000    0.05843    0.31323 =
         0.26679    0.00621   -0.00303    0.01337
AFIX   3
H2A   2    0.999172    0.018293    0.211263    10.25000   -1.50000
H2B   2    1.051892    0.134313    0.135653    10.25000   -1.50000
AFIX   0
HKLF 4
 
REM  cbrpt-95k_a.res in P4/m
REM R1 =  0.0561 for     908 Fo > 4sig(Fo)  and  0.0595 for all     949 data
REM     95 parameters refined using     77 restraints
 
END  
     
WGHT      0.1223      0.0000 

REM Highest difference peak  1.681,  deepest hole -2.197,  1-sigma level  0.287
Q1    1   0.0036  0.3307  0.0000  10.50000  0.05    1.68
Q2    1   0.2454  0.2785  0.0000  10.50000  0.05    1.63
Q3    1   1.0000  0.0000  0.4426  10.25000  0.05    1.50
Q4    1   0.0000  0.5000  0.0000  10.25000  0.05    1.50
Q5    1   0.9192 -0.0032  0.5000  10.50000  0.05    1.09
Q6    1   0.8295  0.5038  0.2373  11.00000  0.05    1.00
Q7    1   0.9386  0.1380  0.5365  11.00000  0.05    0.81
Q8    1   0.4822  0.3590  0.0000  10.50000  0.05    0.76
Q9    1   1.2256  0.2247  0.0986  11.00000  0.05    0.76
Q10   1   0.7059  0.2242  0.5000  10.50000  0.05    0.52
Q11   1   0.3944  0.4053  0.0395  11.00000  0.05    0.51
Q12   1   0.7325  0.4425  0.5000  10.50000  0.05    0.48
Q13   1   0.3124  0.3527  0.0800  11.00000  0.05    0.48
Q14   1   0.7979  0.3367  0.0798  11.00000  0.05    0.45
Q15   1   0.8819  0.0758  0.5484  11.00000  0.05    0.44
Q16   1   0.8150  0.0867  0.5000  10.50000  0.05    0.44
Q17   1   0.4004  0.4988  0.5345  11.00000  0.05    0.43
Q18   1   0.8383  0.5181  0.3120  11.00000  0.05    0.42
Q19   1   0.8504  0.1969  0.5151  11.00000  0.05    0.42
Q20   1   0.9768  0.4831  0.1826  11.00000  0.05    0.41

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0561 for 908 Fo > 4sig(Fo) and 0.0595 for all 3800 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.68, deepest hole -2.20
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0595
  REM R1_gt = 0.0561
  REM wR_ref = 0.1554
  REM GOOF = 1.077
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3800
  REM Reflections_gt = 908
  REM Parameters = n/a
  REM Hole = -2.20
  REM Peak = 1.68
  REM Flack = n/a

  
;
_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 2.643
_oxdiff_exptl_absorpt_empirical_full_min 0.479
