# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 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_Ni(HDMG)2
_database_code_depnum_ccdc_archive 'CCDC 2149607'
_audit_update_record             
;
2022-02-03 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_audit_creation_date             2022-02-02
_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         'C8 H14 N4 Ni O4'
_chemical_formula_sum            'C8 H14 N4 Ni O4'
_chemical_formula_weight         288.94
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni C N O'
_chemical_oxdiff_usercomment     100
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'
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+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, z+1/2'

_cell_length_a                   16.210(2)
_cell_length_b                   10.5207(16)
_cell_length_c                   6.3360(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1080.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1044
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.9730
_cell_measurement_theta_min      3.8480
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.806
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2792
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.224
_diffrn_reflns_theta_min         2.308
_diffrn_ambient_temperature      123
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00 -18.00   0.50   15.00    --    5.00  45.00  30.00  130
  2  ω      8.00  34.00   0.50   15.00    --   -8.90  45.00  90.00   52
  3  ω    -98.00 -19.00   0.50   15.00    --   -8.90  45.00  90.00  158
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0271527000
_diffrn_orient_matrix_UB_12      0.0528357000
_diffrn_orient_matrix_UB_13      0.0003447000
_diffrn_orient_matrix_UB_21      -0.0343603000
_diffrn_orient_matrix_UB_22      0.0418331000
_diffrn_orient_matrix_UB_23      -0.0024058000
_diffrn_orient_matrix_UB_31      -0.0006494000
_diffrn_orient_matrix_UB_32      0.0009295000
_diffrn_orient_matrix_UB_33      0.1118503000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                637
_reflns_number_total             748
_reflns_odcompleteness_completeness 100.00
_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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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         1.014
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         748
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0480
_refine_ls_restrained_S_all      0.979
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1333
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H4A(0.5) H4B(0.5) H4C(0.5) H3B(0.5) H3C(0.5) H3A(0.5)
3.a Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C3(H3B,H3C,H3A)
;
_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
Ni1 Ni 0.5000 0.5000 0.5000 0.0141(3) Uani 1 4 d S T P . .
O1 O 0.66404(17) 0.4065(2) 0.5000 0.0201(6) Uani 1 2 d S T P . .
O2 O 0.44417(15) 0.7563(3) 0.5000 0.0194(6) Uani 1 2 d S T P . .
N1 N 0.6145(2) 0.5088(3) 0.5000 0.0176(7) Uani 1 2 d S T P . .
C2 C 0.5833(2) 0.7223(4) 0.5000 0.0183(7) Uani 1 2 d S T P . .
N2 N 0.50930(19) 0.6760(3) 0.5000 0.0179(7) Uani 1 2 d S T P . .
C4 C 0.6018(2) 0.8603(3) 0.5000 0.0230(8) Uani 1 2 d S T P . .
H4A H 0.5633 0.9036 0.5901 0.034 Uiso 0.5 1 calc GR . . A -1
H4B H 0.5971 0.8928 0.3589 0.034 Uiso 0.5 1 calc GR . . A -1
H4C H 0.6568 0.8739 0.5510 0.034 Uiso 0.5 1 calc GR . . A -1
C1 C 0.6470(2) 0.6218(4) 0.5000 0.0181(7) Uani 1 2 d S T P . .
C3 C 0.7368(2) 0.6438(4) 0.5000 0.0233(8) Uani 1 2 d S T P . .
H3B H 0.7630 0.5837 0.5921 0.035 Uiso 0.5 1 calc GR . . B -1
H3C H 0.7480 0.7285 0.5485 0.035 Uiso 0.5 1 calc GR . . B -1
H3A H 0.7579 0.6336 0.3594 0.035 Uiso 0.5 1 calc GR . . B -1
H1 H 0.626(7) 0.331(10) 0.5000 0.19(5) Uiso 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
Ni1 0.0149(4) 0.0151(4) 0.0123(4) 0.000 0.000 -0.0002(2)
O1 0.0166(12) 0.0202(14) 0.0236(13) 0.000 0.000 0.0049(11)
O2 0.0214(13) 0.0168(13) 0.0201(13) 0.000 0.000 0.0074(11)
N1 0.0163(16) 0.0197(16) 0.0169(15) 0.000 0.000 0.0013(11)
C2 0.0225(17) 0.0191(18) 0.0132(15) 0.000 0.000 -0.0003(16)
N2 0.0194(15) 0.0200(17) 0.0142(15) 0.000 0.000 0.0014(11)
C4 0.0252(18) 0.0191(18) 0.0246(18) 0.000 0.000 -0.0028(16)
C1 0.0206(17) 0.0215(17) 0.0123(15) 0.000 0.000 0.0005(16)
C3 0.0174(17) 0.029(2) 0.0240(19) 0.000 0.000 -0.0016(15)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.859(4) 9_666 ?
Ni1 N1 1.859(4) . ?
Ni1 N2 1.857(4) . ?
Ni1 N2 1.857(4) 9_666 ?
O1 N1 1.343(4) . ?
O2 N2 1.353(4) . ?
N1 C1 1.299(5) . ?
C2 N2 1.295(5) . ?
C2 C4 1.482(5) . ?
C2 C1 1.478(6) . ?
C1 C3 1.475(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 180.0 . 9_666 ?
N2 Ni1 N1 97.53(13) . 9_666 ?
N2 Ni1 N1 97.53(13) 9_666 . ?
N2 Ni1 N1 82.47(13) 9_666 9_666 ?
N2 Ni1 N1 82.47(13) . . ?
N2 Ni1 N2 180.0 9_666 . ?
O1 N1 Ni1 123.8(2) . . ?
C1 N1 Ni1 116.8(3) . . ?
C1 N1 O1 119.4(3) . . ?
N2 C2 C4 123.8(3) . . ?
N2 C2 C1 112.2(3) . . ?
C1 C2 C4 124.1(3) . . ?
O2 N2 Ni1 124.0(2) . . ?
C2 N2 Ni1 116.8(3) . . ?
C2 N2 O2 119.2(3) . . ?
N1 C1 C2 111.8(3) . . ?
N1 C1 C3 122.9(4) . . ?
C3 C1 C2 125.2(4) . . ?

_shelx_res_file                  
;
    200728_sugi_ni.res created by SHELXL-2014/7

TITL 200728_sugi_ni_a.res in Ibam
REM Old TITL 200728_sugi_Ni in Iba2
REM SHELXT solution in Ibam
REM R1 0.078, Rweak 0.004, Alpha 0.070, Orientation as input
REM Formula found by SHELXT: C12 O4 Ni
CELL 0.71073 16.2102 10.5207 6.336 90 90 90
ZERR 8 0.002 0.0016 0.0009 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N Ni O
UNIT 32 56 16 4 16

L.S. 5 0 0
PLAN  20
list 4
fmap 2 53
acta
OMIT 2 0 0
OMIT 17 7 2
REM <olex2.extras>
REM <HklSrc "%.\\200728_sugi_Ni.hkl">
REM </olex2.extras>

WGHT    0.100000
FVAR       0.23071
NI1   4    0.500000    0.500000    0.500000    10.25000    0.01494    0.01513 =
         0.01234    0.00000    0.00000   -0.00018
O1    5    0.664037    0.406521    0.500000    10.50000    0.01662    0.02019 =
         0.02363    0.00000    0.00000    0.00493
O2    5    0.444173    0.756309    0.500000    10.50000    0.02137    0.01681 =
         0.02014    0.00000    0.00000    0.00742
N1    3    0.614537    0.508847    0.500000    10.50000    0.01627    0.01971 =
         0.01690    0.00000    0.00000    0.00134
C2    1    0.583319    0.722333    0.500000    10.50000    0.02251    0.01909 =
         0.01315    0.00000    0.00000   -0.00027
N2    3    0.509302    0.675955    0.500000    10.50000    0.01942    0.02002 =
         0.01418    0.00000    0.00000    0.00137
C4    1    0.601767    0.860285    0.500000    10.50000    0.02517    0.01914 =
         0.02462    0.00000    0.00000   -0.00284
PART -1
AFIX 137
H4A   2    0.563299    0.903553    0.590051    10.50000   -1.50000
H4B   2    0.597122    0.892815    0.358940    10.50000   -1.50000
H4C   2    0.656832    0.873859    0.551010    10.50000   -1.50000
AFIX   0
PART 0
C1    1    0.646980    0.621751    0.500000    10.50000    0.02064    0.02151 =
         0.01227    0.00000    0.00000    0.00050
C3    1    0.736813    0.643804    0.500000    10.50000    0.01738    0.02860 =
         0.02397    0.00000    0.00000   -0.00162
PART -1
AFIX 137
H3B   2    0.763021    0.583666    0.592138    10.50000   -1.50000
H3C   2    0.748043    0.728509    0.548469    10.50000   -1.50000
H3A   2    0.757858    0.633595    0.359393    10.50000   -1.50000
AFIX   0
PART 0
H1    2    0.626310    0.331383    0.500000    10.50000    0.18748
HKLF 4

REM  200728_sugi_ni_a.res in Ibam
REM R1 =  0.0480 for     637 Fo > 4sig(Fo)  and  0.0566 for all     748 data
REM     58 parameters refined using      0 restraints

END

WGHT      0.0793      0.0664

REM Highest difference peak  1.014,  deepest hole -0.651,  1-sigma level  0.138
Q1    1   0.4806  0.4336  0.5000  10.50000  0.05    1.01
Q2    1   0.4833  0.5735  0.5000  10.50000  0.05    1.00
Q3    1   0.6160  0.6731  0.5000  10.50000  0.05    0.83
Q4    1   0.4800  0.5002  0.6191  11.00000  0.05    0.79
Q5    1   0.5001  0.6034  0.6457  11.00000  0.05    0.71
Q6    1   0.6351  0.4531  0.5000  10.50000  0.05    0.70
Q7    1   0.6382  0.5540  0.5000  10.50000  0.05    0.65
Q8    1   0.5680  0.5020  0.5000  10.50000  0.05    0.57
Q9    1   0.5857  0.7970  0.5000  10.50000  0.05    0.53
Q10   1   0.4180  0.7970  0.5000  10.50000  0.05    0.45
Q11   1   0.5865  0.6009  0.5000  10.50000  0.05    0.45
Q12   1   0.5875  0.3996  0.5000  10.50000  0.05    0.44
Q13   1   0.4630  0.7237  0.5000  10.50000  0.05    0.29
Q14   1   0.4547  0.8243  0.5000  10.50000  0.05    0.28
Q15   1   0.6569  0.4987  0.6391  11.00000  0.05    0.27
Q16   1   0.7471  0.6260  0.4091  11.00000  0.05    0.27
Q17   1   0.7392  0.7177  0.5000  10.50000  0.05    0.27
Q18   1   0.5976  0.5039  0.5902  11.00000  0.05    0.27
Q19   1   0.7604  0.6914  0.3355  11.00000  0.05    0.26
Q20   1   0.7612  0.5973  0.5000  10.50000  0.05    0.26
;
_shelx_res_checksum              77099
_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 2.913
_oxdiff_exptl_absorpt_empirical_full_min 0.444
####################################################################### 
# 
# 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_Pd(HDMG)2
_database_code_depnum_ccdc_archive 'CCDC 2149869'
_audit_update_record             
;
2022-02-03 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_audit_creation_date             2022-02-02
_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         'C8 H14 N4 O4 Pd'
_chemical_formula_sum            'C8 H14 N4 O4 Pd'
_chemical_formula_weight         336.63
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pd C N O'
_chemical_oxdiff_usercomment     100
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'
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+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, z+1/2'

_cell_length_a                   16.3415(10)
_cell_length_b                   10.6382(6)
_cell_length_c                   6.3897(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1110.81(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1956
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.3340
_cell_measurement_theta_min      3.7720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.681
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.013
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2671
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.411
_diffrn_reflns_theta_min         3.831
_diffrn_ambient_temperature      123
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'Rigaku IP'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.841
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -57.00 -31.00   0.50    0.71    --    5.00  45.00   0.00   52
  2  ω    -84.00  48.00   0.50    0.71    --    5.00  45.00  90.00  264
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IP'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0182941000
_diffrn_orient_matrix_UB_12      0.0601654000
_diffrn_orient_matrix_UB_13      0.0088173000
_diffrn_orient_matrix_UB_21      -0.0394069000
_diffrn_orient_matrix_UB_22      0.0281725000
_diffrn_orient_matrix_UB_23      0.0018974000
_diffrn_orient_matrix_UB_31      -0.0006509000
_diffrn_orient_matrix_UB_32      -0.0050248000
_diffrn_orient_matrix_UB_33      0.1106054000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                661
_reflns_number_total             704
_reflns_odcompleteness_completeness 98.52
_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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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         0.499
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         704
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0207
_refine_ls_restrained_S_all      1.093
_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)+(0.0428P)²+0.0387P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0600
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H4A(0.5) H4B(0.5) H4C(0.5) H3A(0.5) H3B(0.5) H3C(0.5)
3.a Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_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
Pd1 Pd 0.500000 0.500000 0.500000 0.01005(14) Uani 1 4 d S T P . .
O1 O 0.33367(10) 0.58927(14) 0.500000 0.0163(4) Uani 1 2 d S T P . .
O2 O 0.55212(11) 0.23642(14) 0.500000 0.0173(3) Uani 1 2 d S T P . .
N1 N 0.37980(18) 0.48748(16) 0.500000 0.0140(5) Uani 1 2 d S T P . .
N2 N 0.48633(13) 0.3170(2) 0.500000 0.0143(4) Uani 1 2 d S T P . .
C2 C 0.41283(15) 0.2736(2) 0.500000 0.0165(4) Uani 1 2 d S T P . .
C1 C 0.34976(15) 0.3742(2) 0.500000 0.0157(5) Uani 1 2 d S T P . .
C4 C 0.39404(13) 0.13723(17) 0.500000 0.0209(4) Uani 1 2 d S T P . .
H4A H 0.431421 0.094335 0.408731 0.031 Uiso 0.5 1 calc R U P A -1
H4B H 0.339026 0.124372 0.451821 0.031 Uiso 0.5 1 calc R U P A -1
H4C H 0.399499 0.104713 0.639448 0.031 Uiso 0.5 1 calc R U P A -1
C3 C 0.26016(12) 0.3525(2) 0.500000 0.0211(4) Uani 1 2 d S T P . .
H3A H 0.239338 0.362289 0.639540 0.032 Uiso 0.5 1 calc R U P B -1
H3B H 0.248909 0.268915 0.451318 0.032 Uiso 0.5 1 calc R U P B -1
H3C H 0.234210 0.412317 0.409141 0.032 Uiso 0.5 1 calc R U P B -1
H2 H 0.597(5) 0.300(7) 0.500000 0.22(3) Uiso 1 2 d S . 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 0.0128(2) 0.00949(19) 0.00788(18) 0.000 0.000 0.00058(5)
O1 0.0158(8) 0.0153(8) 0.0179(7) 0.000 0.000 0.0067(6)
O2 0.0208(8) 0.0123(7) 0.0190(7) 0.000 0.000 0.0065(7)
N1 0.0142(12) 0.0146(9) 0.0131(12) 0.000 0.000 0.0012(6)
N2 0.0202(8) 0.0096(10) 0.0131(9) 0.000 0.000 0.0021(8)
C2 0.0222(11) 0.0162(10) 0.0109(8) 0.000 0.000 -0.0001(9)
C1 0.0188(10) 0.0179(11) 0.0104(9) 0.000 0.000 -0.0016(9)
C4 0.0266(10) 0.0145(9) 0.0216(10) 0.000 0.000 -0.0022(8)
C3 0.0186(9) 0.0215(9) 0.0232(9) 0.000 0.000 -0.0036(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
Pd1 Pd1 3.1948(2) 7_546 ?
Pd1 Pd1 3.1948(2) 7_545 ?
Pd1 N1 1.969(3) 9_666 ?
Pd1 N1 1.969(3) . ?
Pd1 N2 1.960(3) . ?
Pd1 N2 1.960(3) 9_666 ?
O1 N1 1.319(3) . ?
O2 N2 1.375(3) . ?
O2 H2 1.00(7) . ?
N1 C1 1.301(3) . ?
N2 C2 1.287(3) . ?
C2 C1 1.486(4) . ?
C2 C4 1.483(3) . ?
C1 C3 1.482(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

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
Pd1 Pd1 Pd1 180.0 7_545 7_546 ?
N1 Pd1 Pd1 90.0 . 7_545 ?
N1 Pd1 Pd1 90.0 . 7_546 ?
N1 Pd1 Pd1 90.0 9_666 7_546 ?
N1 Pd1 Pd1 90.0 9_666 7_545 ?
N1 Pd1 N1 180.0 . 9_666 ?
N2 Pd1 Pd1 90.0 . 7_545 ?
N2 Pd1 Pd1 90.0 9_666 7_545 ?
N2 Pd1 Pd1 90.0 9_666 7_546 ?
N2 Pd1 Pd1 90.0 . 7_546 ?
N2 Pd1 N1 79.58(8) . . ?
N2 Pd1 N1 79.58(8) 9_666 9_666 ?
N2 Pd1 N1 100.42(8) 9_666 . ?
N2 Pd1 N1 100.42(8) . 9_666 ?
N2 Pd1 N2 180.0 . 9_666 ?
N2 O2 H2 99(5) . . ?
O1 N1 Pd1 120.97(15) . . ?
C1 N1 Pd1 116.04(18) . . ?
C1 N1 O1 123.0(3) . . ?
O2 N2 Pd1 122.02(16) . . ?
C2 N2 Pd1 117.56(18) . . ?
C2 N2 O2 120.4(2) . . ?
N2 C2 C1 112.9(2) . . ?
N2 C2 C4 123.0(2) . . ?
C4 C2 C1 124.1(2) . . ?
N1 C1 C2 113.9(2) . . ?
N1 C1 C3 121.1(2) . . ?
C3 C1 C2 125.0(2) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N1 C1 C2 0.0 . . . . ?
Pd1 N1 C1 C3 180.0 . . . . ?
Pd1 N2 C2 C1 0.0 . . . . ?
Pd1 N2 C2 C4 180.0 . . . . ?
O1 N1 C1 C2 180.0 . . . . ?
O1 N1 C1 C3 0.0 . . . . ?
O2 N2 C2 C1 180.0 . . . . ?
O2 N2 C2 C4 0.0 . . . . ?
N2 C2 C1 N1 0.0 . . . . ?
N2 C2 C1 C3 180.0 . . . . ?
C4 C2 C1 N1 180.0 . . . . ?
C4 C2 C1 C3 0.0 . . . . ?

_shelx_res_file                  
;
TITL 200728_sugi_pd_a.res in Ibam
    200728_sugi_pd.res
    created by SHELXL-2018/3 at 11:17:24 on 02-Feb-2022
REM Old TITL 200728_sugi_Pd in Iba2
REM SHELXT solution in Ibam
REM R1 0.047, Rweak 0.001, Alpha 0.026, Orientation as input
REM Formula found by SHELXT: C10 N4 O2 Pd
CELL 0.71073 16.3415 10.6382 6.3897 90 90 90
ZERR 4 0.001 0.0006 0.0004 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O Pd
UNIT 32 56 16 16 4

L.S. 5
PLAN  5
list 4
fmap 2 53
acta
MORE -1
CONF
BOND $H
REM <olex2.extras>
REM <HklSrc "%.\\200728_sugi_Pd.hkl">
REM </olex2.extras>

WGHT    0.042800    0.038700
FVAR       0.37584
PD1   5    0.500000    0.500000    0.500000    10.25000    0.01277    0.00949 =
         0.00788    0.00000    0.00000    0.00058
O1    4    0.333667    0.589271    0.500000    10.50000    0.01580    0.01535 =
         0.01787    0.00000    0.00000    0.00674
O2    4    0.552124    0.236423    0.500000    10.50000    0.02079    0.01229 =
         0.01896    0.00000    0.00000    0.00646
N1    3    0.379802    0.487482    0.500000    10.50000    0.01424    0.01465 =
         0.01311    0.00000    0.00000    0.00120
N2    3    0.486335    0.316992    0.500000    10.50000    0.02023    0.00962 =
         0.01306    0.00000    0.00000    0.00209
C2    1    0.412826    0.273615    0.500000    10.50000    0.02221    0.01625 =
         0.01092    0.00000    0.00000   -0.00006
C1    1    0.349759    0.374190    0.500000    10.50000    0.01878    0.01787 =
         0.01037    0.00000    0.00000   -0.00157
C4    1    0.394036    0.137235    0.500000    10.50000    0.02656    0.01447 =
         0.02164    0.00000    0.00000   -0.00220
PART -1
AFIX 137
H4A   2    0.431421    0.094335    0.408731    10.50000   -1.50000
H4B   2    0.339026    0.124372    0.451821    10.50000   -1.50000
H4C   2    0.399499    0.104713    0.639448    10.50000   -1.50000
AFIX   0
PART 0
C3    1    0.260163    0.352519    0.500000    10.50000    0.01861    0.02149 =
         0.02324    0.00000    0.00000   -0.00363
PART -1
AFIX 137
H3A   2    0.239338    0.362289    0.639540    10.50000   -1.50000
H3B   2    0.248909    0.268915    0.451318    10.50000   -1.50000
H3C   2    0.234210    0.412317    0.409141    10.50000   -1.50000
AFIX   0
PART 0
H2    2    0.597281    0.299609    0.500000    10.50000    0.22192
HKLF 4




REM  200728_sugi_pd_a.res in Ibam
REM wR2 = 0.0600, GooF = S = 1.093, Restrained GooF = 1.093 for all data
REM R1 = 0.0207 for 661 Fo > 4sig(Fo) and 0.0215 for all 704 data
REM 58 parameters refined using 0 restraints

END

WGHT      0.0390      0.2630

REM Highest difference peak  0.499,  deepest hole -0.814,  1-sigma level  0.101
Q1    1   0.4170  0.4998  0.5000  10.50000  0.05    0.50
Q2    1   0.3791  0.3183  0.5000  10.50000  0.05    0.48
Q3    1   0.4996  0.3950  0.3638  11.00000  0.05    0.37
Q4    1   0.4984  0.3611  0.5000  10.50000  0.05    0.31
Q5    1   0.5000  0.3056  0.3528  11.00000  0.05    0.29
;
_shelx_res_checksum              2220
_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 1.313
_oxdiff_exptl_absorpt_empirical_full_min 0.744
####################################################################### 
# 
# 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_Pt(HDMG)2
_database_code_depnum_ccdc_archive 'CCDC 2149870'
_audit_update_record             
;
2022-02-03 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_audit_creation_date             2022-02-03
_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         'C8 H14 N4 O4 Pt'
_chemical_formula_sum            'C8 H14 N4 O4 Pt'
_chemical_formula_weight         425.32
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pt C N O'
_chemical_oxdiff_usercomment     100
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'
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+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, z+1/2'

_cell_length_a                   16.2744(11)
_cell_length_b                   10.6919(7)
_cell_length_c                   6.3727(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1108.88(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1528
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.7350
_cell_measurement_theta_min      2.4530
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.665
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.548
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.874
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3042
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.803
_diffrn_reflns_theta_min         2.279
_diffrn_ambient_temperature      123
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00  -9.00   0.50    3.21    --    5.00  45.00 150.00  150
  2  ω     -1.00  42.00   0.50    3.21    --    5.00  45.00 150.00   86
  3  ω    -92.00 -30.00   0.50    3.21    --   -8.70  45.00  60.00  124
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0137117000
_diffrn_orient_matrix_UB_12      -0.0630403000
_diffrn_orient_matrix_UB_13      0.0008341000
_diffrn_orient_matrix_UB_21      0.0412755000
_diffrn_orient_matrix_UB_22      0.0208888000
_diffrn_orient_matrix_UB_23      -0.0063503000
_diffrn_orient_matrix_UB_31      0.0024125000
_diffrn_orient_matrix_UB_32      0.0014943000
_diffrn_orient_matrix_UB_33      0.1110328000
_diffrn_oxdiff_ac4_digest_frames 
;
01558bf129a7154c19822fa075033778eb003601e17
;
_diffrn_oxdiff_ac4_digest_hkl    
;
019b1de1032c46edae1731f2c8b82eeb43ecea
;
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                624
_reflns_number_total             761
_reflns_odcompleteness_completeness 100.00
_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 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_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         1.665
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         761
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0170
_refine_ls_restrained_S_all      1.111
_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)+(0.0263P)²+0.1950P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0456
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) H2A(0.5) H2B(0.5) H2C(0.5)
3.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
3.b 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 0.500000 0.500000 0.500000 0.00897(10) Uani 1 4 d S T P . .
O3 O 0.55162(17) 0.7627(3) 0.500000 0.0156(6) Uani 1 2 d S T P . .
H3 H 0.592883 0.725302 0.538894 0.023 Uiso 0.5 1 calc R U P . .
O4 O 0.33269(18) 0.4117(3) 0.500000 0.0162(6) Uani 1 2 d S T P . .
N2 N 0.3788(3) 0.5138(3) 0.500000 0.0127(8) Uani 1 2 d S T P . .
N1 N 0.4856(2) 0.6820(4) 0.500000 0.0133(8) Uani 1 2 d S T P . .
C3 C 0.2587(2) 0.6487(4) 0.500000 0.0207(9) Uani 1 2 d S T P . .
H3A H 0.237524 0.637120 0.639299 0.031 Uiso 0.5 1 calc R U P A -1
H3B H 0.232608 0.590585 0.406357 0.031 Uiso 0.5 1 calc R U P A -1
H3C H 0.247605 0.732567 0.454345 0.031 Uiso 0.5 1 calc R U P A -1
C1 C 0.3486(3) 0.6267(4) 0.500000 0.0137(8) Uani 1 2 d S T P . .
C2 C 0.3939(3) 0.8623(3) 0.500000 0.0181(9) Uani 1 2 d S T P . .
H2A H 0.404481 0.895980 0.362962 0.027 Uiso 0.5 1 calc R U P B -1
H2B H 0.428578 0.903172 0.600833 0.027 Uiso 0.5 1 calc R U P B -1
H2C H 0.337371 0.875951 0.536206 0.027 Uiso 0.5 1 calc R U P B -1
C0AA C 0.4115(2) 0.7258(4) 0.500000 0.0143(8) 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 0.00962(13) 0.00944(14) 0.00785(14) 0.000 0.000 -0.00019(7)
O3 0.0128(13) 0.0127(13) 0.0213(16) 0.000 0.000 -0.0055(12)
O4 0.0128(14) 0.0150(14) 0.0206(16) 0.000 0.000 -0.0069(12)
N2 0.0133(19) 0.0142(17) 0.0104(18) 0.000 0.000 0.0018(12)
N1 0.0164(17) 0.0105(18) 0.0130(19) 0.000 0.000 -0.0023(13)
C3 0.015(2) 0.021(2) 0.026(2) 0.000 0.000 0.0016(16)
C1 0.016(2) 0.0162(18) 0.0085(18) 0.000 0.000 0.0025(16)
C2 0.020(2) 0.0143(18) 0.020(2) 0.000 0.000 0.0047(15)
C0AA 0.015(2) 0.0173(19) 0.0106(19) 0.000 0.000 0.0011(16)

_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 Pt1 3.1864(2) 7_546 ?
Pt1 Pt1 3.1864(2) 7_545 ?
Pt1 N2 1.978(4) 9_666 ?
Pt1 N2 1.978(4) . ?
Pt1 N1 1.960(4) . ?
Pt1 N1 1.960(4) 9_666 ?
O3 H3 0.82(4) 10_556 ?
O3 H3 0.8200 . ?
O3 N1 1.378(4) . ?
O4 N2 1.324(4) . ?
N2 C1 1.303(5) . ?
N1 C0AA 1.293(5) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C1 1.483(5) . ?
C1 C0AA 1.473(6) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C2 C0AA 1.488(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Pt1 Pt1 Pt1 180.0 7_545 7_546 ?
N2 Pt1 Pt1 90.0 9_666 7_545 ?
N2 Pt1 Pt1 90.0 . 7_546 ?
N2 Pt1 Pt1 90.0 9_666 7_546 ?
N2 Pt1 Pt1 90.0 . 7_545 ?
N2 Pt1 N2 180.0 . 9_666 ?
N1 Pt1 Pt1 90.0 . 7_546 ?
N1 Pt1 Pt1 90.0 . 7_545 ?
N1 Pt1 Pt1 90.0 9_666 7_545 ?
N1 Pt1 Pt1 90.0 9_666 7_546 ?
N1 Pt1 N2 78.87(12) 9_666 9_666 ?
N1 Pt1 N2 78.87(12) . . ?
N1 Pt1 N2 101.13(12) 9_666 . ?
N1 Pt1 N2 101.13(12) . 9_666 ?
N1 Pt1 N1 180.0 . 9_666 ?
H3 O3 H3 35.2 . 10_556 ?
N1 O3 H3 109.5(10) . 10_556 ?
N1 O3 H3 109.5 . . ?
O4 N2 Pt1 120.2(2) . . ?
C1 N2 Pt1 116.4(3) . . ?
C1 N2 O4 123.4(4) . . ?
O3 N1 Pt1 121.9(3) . . ?
C0AA N1 Pt1 118.1(3) . . ?
C0AA N1 O3 120.1(4) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
N2 C1 C3 121.3(4) . . ?
N2 C1 C0AA 113.9(4) . . ?
C0AA C1 C3 124.9(3) . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C0AA C2 H2A 109.5 . . ?
C0AA C2 H2B 109.5 . . ?
C0AA C2 H2C 109.5 . . ?
N1 C0AA C1 112.8(3) . . ?
N1 C0AA C2 122.3(4) . . ?
C1 C0AA C2 124.9(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
Pt1 N2 C1 C3 180.0 . . . . ?
Pt1 N2 C1 C0AA 0.0 . . . . ?
Pt1 N1 C0AA C1 0.0 . . . . ?
Pt1 N1 C0AA C2 180.0 . . . . ?
O3 N1 C0AA C1 180.0 . . . . ?
O3 N1 C0AA C2 0.0 . . . . ?
O4 N2 C1 C3 0.0 . . . . ?
O4 N2 C1 C0AA 180.0 . . . . ?
N2 C1 C0AA N1 0.0 . . . . ?
N2 C1 C0AA C2 180.0 . . . . ?
C3 C1 C0AA N1 180.0 . . . . ?
C3 C1 C0AA C2 0.0 . . . . ?

_shelx_res_file                  
;
TITL 200728_sugi_pt2_a.res in Ibam
    200728_sugi_pt2.res
    created by SHELXL-2018/3 at 10:31:38 on 03-Feb-2022
REM Old TITL 200728_sugi_Pt2 in Iba2
REM SHELXT solution in Ibam
REM R1 0.027, Rweak 0.000, Alpha 0.013, Orientation as input
REM Formula found by SHELXT: C10 N2 O4 Pt
CELL 0.71073 16.2744 10.6919 6.3727 90 90 90
ZERR 4 0.0011 0.0007 0.0004 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O Pt
UNIT 32 56 16 16 4

L.S. 5 0 0
PLAN  5
CONF
list 4
fmap 2 53
acta
MORE -1
BOND $H
REM <olex2.extras>
REM <HklSrc "%.\\200728_sugi_Pt2.hkl">
REM </olex2.extras>

WGHT    0.026300    0.195000
FVAR       0.17273
PT1   5    0.500000    0.500000    0.500000    10.25000    0.00962    0.00944 =
         0.00785    0.00000    0.00000   -0.00019
O3    4    0.551618    0.762708    0.500000    10.50000    0.01282    0.01271 =
         0.02134    0.00000    0.00000   -0.00553
AFIX 147
H3    2    0.592883    0.725302    0.538894    10.50000   -1.50000
AFIX   0
O4    4    0.332693    0.411681    0.500000    10.50000    0.01282    0.01503 =
         0.02061    0.00000    0.00000   -0.00686
N2    3    0.378773    0.513771    0.500000    10.50000    0.01332    0.01425 =
         0.01044    0.00000    0.00000    0.00180
N1    3    0.485602    0.682045    0.500000    10.50000    0.01644    0.01052 =
         0.01295    0.00000    0.00000   -0.00229
C3    1    0.258659    0.648673    0.500000    10.50000    0.01546    0.02114 =
         0.02554    0.00000    0.00000    0.00158
PART -1
AFIX 137
H3A   2    0.237524    0.637120    0.639299    10.50000   -1.50000
H3B   2    0.232608    0.590585    0.406357    10.50000   -1.50000
H3C   2    0.247605    0.732567    0.454345    10.50000   -1.50000
AFIX   0
PART 0
C1    1    0.348620    0.626658    0.500000    10.50000    0.01637    0.01625 =
         0.00852    0.00000    0.00000    0.00253
C2    1    0.393927    0.862331    0.500000    10.50000    0.02010    0.01429 =
         0.02005    0.00000    0.00000    0.00466
PART -1
AFIX 137
H2A   2    0.404481    0.895980    0.362962    10.50000   -1.50000
H2B   2    0.428578    0.903172    0.600833    10.50000   -1.50000
H2C   2    0.337371    0.875951    0.536206    10.50000   -1.50000
AFIX   0
PART 0
C0AA  1    0.411519    0.725758    0.500000    10.50000    0.01510    0.01732 =
         0.01063    0.00000    0.00000    0.00114
HKLF 4




REM  200728_sugi_pt2_a.res in Ibam
REM wR2 = 0.0456, GooF = S = 1.111, Restrained GooF = 1.111 for all data
REM R1 = 0.0170 for 624 Fo > 4sig(Fo) and 0.0215 for all 761 data
REM 56 parameters refined using 0 restraints

END

WGHT      0.0263      0.1950

REM Highest difference peak  1.665,  deepest hole -1.304,  1-sigma level  0.158
Q1    1   0.4994  0.5192  0.6181  11.00000  0.05    1.66
Q2    1   0.5000  0.5618  0.2500  10.50000  0.05    0.79
Q3    1   0.4999  0.5965  0.5000  10.50000  0.05    0.69
Q4    1   0.4595  0.4962  0.5000  10.50000  0.05    0.60
Q5    1   0.5774  0.7241  0.5000  10.50000  0.05    0.54
;
_shelx_res_checksum              32367
_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 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.796
####################################################################### 
# 
# 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_Ni(x)Pt(1-x)(HDMG)2
_database_code_depnum_ccdc_archive 'CCDC 2149872'
loop_
_audit_author_name
_audit_author_address
'Akira Sugimoto'
;Kumamoto university
Japan
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_audit_creation_date             2022-04-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H14 N4 Ni0.551 O4 Pt0.449'
_chemical_formula_sum            'C8 H14 N4 Ni0.54 O4 Pt0.45'
_chemical_formula_weight         350.99
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'-x, -y, -z'
'x, y, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'

_cell_length_a                   10.5843(8)
_cell_length_b                   16.3239(11)
_cell_length_c                   6.3513(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1097.36(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1665
_cell_measurement_temperature    123
_cell_measurement_theta_max      31.0790
_cell_measurement_theta_min      2.2860
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.792
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.125
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             691
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2964
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.940
_diffrn_reflns_theta_min         2.495
_diffrn_ambient_temperature      123.00
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.855
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -75.00 -38.00   0.50    3.36    --    5.00  45.00 120.00   74
  2  ω    -99.00  38.00   0.50    3.36    --  -10.00  45.00  30.00  274
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                676
_reflns_number_total             809
_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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         809
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0229
_refine_ls_restrained_S_all      1.123
_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)+(0.0233P)²+0.4352P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0561
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{Pt, Ni3}
2. Uiso/Uaniso restraints and constraints
Uanis(Pt) = Uanis(Ni3)
3. Others
 Sof(Ni3)=0.25*(1-FVAR(2))
 Sof(Pt)=0.25*FVAR(2)
 Fixed Sof: H00A(0.5) H00B(0.5) H00C(0.5) H00D(0.5) H00E(0.5) H00F(0.5)
4.a Tetrahedral OH refined with riding coordinates:
 O003(H003)
4.b Idealised Me refined as rotating group:
 C006(H00A,H00B,H00C), C009(H00D,H00E,H00F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt Pt 0.500000 0.500000 0.500000 0.01213(12) Uani 0.449(5) 4 d S T P A 1
O002 O 0.5910(2) 0.66454(15) 0.500000 0.0224(7) Uani 1 2 d S T P A .
O003 O 0.2399(3) 0.44646(17) 0.500000 0.0246(7) Uani 1 2 d S T P A .
H003 H 0.281934 0.402821 0.499590 0.42(12) Uiso 1 2 calc R . P . .
N004 N 0.3205(3) 0.51213(17) 0.500000 0.0198(8) Uani 1 2 d S T P . .
N005 N 0.4883(3) 0.6174(2) 0.500000 0.0188(7) Uani 1 2 d S T P . .
C006 C 0.1375(3) 0.6031(3) 0.500000 0.0269(9) Uani 1 2 d S T P . .
H00A H 0.122126 0.658031 0.443361 0.018(14) Uiso 0.5 1 calc R . P A -1
H00B H 0.105165 0.599945 0.644363 0.05(2) Uiso 0.5 1 calc R . P A -1
H00C H 0.094215 0.562442 0.412276 0.005(12) Uiso 0.5 1 calc R . P A -1
C007 C 0.2766(4) 0.5860(2) 0.500000 0.0214(8) Uani 1 2 d S T P A .
C008 C 0.3761(4) 0.6480(2) 0.500000 0.0205(8) Uani 1 2 d S T P A .
C009 C 0.3547(4) 0.7378(2) 0.500000 0.0260(9) Uani 1 2 d S T P . .
H00D H 0.416578 0.764249 0.407511 0.022(15) Uiso 0.5 1 calc R . P A -1
H00E H 0.364194 0.759000 0.643489 0.09(3) Uiso 0.5 1 calc R . P A -1
H00F H 0.269193 0.749481 0.449000 0.017(15) Uiso 0.5 1 calc R . P A -1
Ni3 Ni 0.500000 0.500000 0.500000 0.01213(12) Uani 0.551(5) 4 d S T P A 2

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
Pt 0.01188(18) 0.01466(16) 0.00986(16) 0.000 0.000 0.00010(11)
O002 0.0212(14) 0.0194(13) 0.0265(15) 0.000 0.000 -0.0025(11)
O003 0.0209(14) 0.0294(14) 0.0234(14) 0.000 0.000 -0.0092(12)
N004 0.0180(17) 0.0254(17) 0.0159(15) 0.000 0.000 -0.0025(12)
N005 0.0200(17) 0.0232(16) 0.0131(14) 0.000 0.000 -0.0007(12)
C006 0.0185(19) 0.037(2) 0.025(2) 0.000 0.000 0.0030(17)
C007 0.021(2) 0.0297(19) 0.0129(17) 0.000 0.000 -0.0003(16)
C008 0.024(2) 0.0254(18) 0.0119(16) 0.000 0.000 -0.0007(16)
C009 0.029(2) 0.0278(19) 0.021(2) 0.000 0.000 -0.0014(17)
Ni3 0.01188(18) 0.01466(16) 0.00986(16) 0.000 0.000 0.00010(11)

_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
Pt Pt 3.1757(2) 3_565 ?
Pt Pt 3.1757(2) 3_566 ?
Pt N004 1.910(4) . ?
Pt N004 1.910(4) 9_666 ?
Pt N005 1.920(3) 9_666 ?
Pt N005 1.920(3) . ?
O002 N005 1.332(4) . ?
O003 H003 0.8400 . ?
O003 N004 1.370(4) . ?
N004 C007 1.293(5) . ?
N004 Ni3 1.910(4) . ?
N005 C008 1.289(5) . ?
N005 Ni3 1.920(3) . ?
C006 H00A 0.9800 . ?
C006 H00B 0.9800 . ?
C006 H00C 0.9800 . ?
C006 C007 1.499(5) . ?
C007 C008 1.461(5) . ?
C008 C009 1.483(5) . ?
C009 H00D 0.9800 . ?
C009 H00E 0.9800 . ?
C009 H00F 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
Pt Pt Pt 180.0 3_566 3_565 ?
N004 Pt Pt 90.0 . 3_566 ?
N004 Pt Pt 90.0 9_666 3_566 ?
N004 Pt Pt 90.0 . 3_565 ?
N004 Pt Pt 90.0 9_666 3_565 ?
N004 Pt N004 180.0 . 9_666 ?
N004 Pt N005 80.35(12) . . ?
N004 Pt N005 99.65(12) . 9_666 ?
N004 Pt N005 99.65(12) 9_666 . ?
N004 Pt N005 80.35(12) 9_666 9_666 ?
N005 Pt Pt 90.0 . 3_565 ?
N005 Pt Pt 90.0 9_666 3_565 ?
N005 Pt Pt 90.0 9_666 3_566 ?
N005 Pt Pt 90.0 . 3_566 ?
N005 Pt N005 180.0 . 9_666 ?
N004 O003 H003 109.5 . . ?
O003 N004 Pt 122.6(2) . . ?
O003 N004 Ni3 122.6(2) . . ?
C007 N004 Pt 117.0(3) . . ?
C007 N004 O003 120.4(3) . . ?
C007 N004 Ni3 117.0(3) . . ?
O002 N005 Pt 121.6(2) . . ?
O002 N005 Ni3 121.6(2) . . ?
C008 N005 Pt 116.5(3) . . ?
C008 N005 O002 121.9(3) . . ?
C008 N005 Ni3 116.5(3) . . ?
H00A C006 H00B 109.5 . . ?
H00A C006 H00C 109.5 . . ?
H00B C006 H00C 109.5 . . ?
C007 C006 H00A 109.5 . . ?
C007 C006 H00B 109.5 . . ?
C007 C006 H00C 109.5 . . ?
N004 C007 C006 121.8(4) . . ?
N004 C007 C008 112.8(3) . . ?
C008 C007 C006 125.4(3) . . ?
N005 C008 C007 113.3(3) . . ?
N005 C008 C009 121.6(4) . . ?
C007 C008 C009 125.1(4) . . ?
C008 C009 H00D 109.5 . . ?
C008 C009 H00E 109.5 . . ?
C008 C009 H00F 109.5 . . ?
H00D C009 H00E 109.5 . . ?
H00D C009 H00F 109.5 . . ?
H00E C009 H00F 109.5 . . ?
N004 Ni3 N004 180.0 . 9_666 ?
N004 Ni3 N005 80.35(12) . . ?
N004 Ni3 N005 99.65(12) 9_666 . ?
N004 Ni3 N005 99.65(12) . 9_666 ?
N004 Ni3 N005 80.35(12) 9_666 9_666 ?
N005 Ni3 N005 180.0 . 9_666 ?

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
_geom_hbond_publ_flag
O003 H003 O002 0.84 1.74 2.547(4) 161.3 2_665 yes

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
Pt N004 C007 C006 180.0 . . . . ?
Pt N004 C007 C008 0.0 . . . . ?
Pt N005 C008 C007 0.0 . . . . ?
Pt N005 C008 C009 180.0 . . . . ?
O002 N005 C008 C007 180.0 . . . . ?
O002 N005 C008 C009 0.0 . . . . ?
O003 N004 C007 C006 0.0 . . . . ?
O003 N004 C007 C008 180.0 . . . . ?
N004 C007 C008 N005 0.0 . . . . ?
N004 C007 C008 C009 180.0 . . . . ?
C006 C007 C008 N005 180.0 . . . . ?
C006 C007 C008 C009 0.0 . . . . ?
Ni3 N004 C007 C006 180.0 . . . . ?
Ni3 N004 C007 C008 0.0 . . . . ?
Ni3 N005 C008 C007 0.0 . . . . ?
Ni3 N005 C008 C009 180.0 . . . . ?

_shelx_res_file                  
;
TITL 220120_SUGIMOTO_NIPT OLEX2: imported from CIF
    220120_sugimoto_nipt.res
    created by SHELXL-2018/3 at 18:51:25 on 26-Apr-2022
CELL 0.71073 10.5843 16.3239 6.3513 90 90 90
ZERR 4 0.0008 0.0011 0.0004 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM +X,-Y,0.5-Z
SYMM -X,+Y,0.5-Z
SFAC C H N Ni O Pt
UNIT 32 56 16 2.18 16 1.82
EQIV $1 1-X,1-Y,+Z
EADP Pt Ni3
EXYZ Pt Ni3

L.S. 15 0 0
PLAN  5
TEMP -150.15
CONF
HTAB O003 O002_$1
fmap 2 53
MORE -1
BOND $H
ACTA
OMIT 1 1 0
REM <olex2.extras>
REM <HklSrc "%.\\220120_sugimoto_nipt.hkl">
REM </olex2.extras>

WGHT    0.023300    0.435200
FVAR       0.21183   0.44934
PART 1
PT    6    0.500000    0.500000    0.500000    20.25000    0.01188    0.01466 =
         0.00986    0.00000    0.00000    0.00010
PART 0
O002  5    0.591014    0.664535    0.500000    10.50000    0.02121    0.01942 =
         0.02653    0.00000    0.00000   -0.00255
O003  5    0.239886    0.446463    0.500000    10.50000    0.02091    0.02943 =
         0.02344    0.00000    0.00000   -0.00917
AFIX  83
H003  2    0.281934    0.402821    0.499590    10.50000    0.42158
AFIX   0
N004  3    0.320548    0.512130    0.500000    10.50000    0.01799    0.02545 =
         0.01592    0.00000    0.00000   -0.00246
N005  3    0.488307    0.617398    0.500000    10.50000    0.01996    0.02320 =
         0.01310    0.00000    0.00000   -0.00066
C006  1    0.137493    0.603084    0.500000    10.50000    0.01850    0.03698 =
         0.02509    0.00000    0.00000    0.00296
PART -1
AFIX 137
H00A  2    0.122126    0.658031    0.443361    10.50000    0.01781
H00B  2    0.105165    0.599945    0.644363    10.50000    0.04819
H00C  2    0.094215    0.562442    0.412276    10.50000    0.00492
AFIX   0
PART 0
C007  1    0.276606    0.586007    0.500000    10.50000    0.02146    0.02971 =
         0.01291    0.00000    0.00000   -0.00027
C008  1    0.376100    0.648025    0.500000    10.50000    0.02433    0.02543 =
         0.01187    0.00000    0.00000   -0.00070
C009  1    0.354702    0.737800    0.500000    10.50000    0.02860    0.02782 =
         0.02149    0.00000    0.00000   -0.00138
PART -1
AFIX 137
H00D  2    0.416578    0.764249    0.407511    10.50000    0.02202
H00E  2    0.364194    0.759000    0.643489    10.50000    0.08943
H00F  2    0.269193    0.749481    0.449000    10.50000    0.01729
AFIX   0
PART 2
NI3   4    0.500000    0.500000    0.500000   -20.25000    0.01188    0.01466 =
         0.00986    0.00000    0.00000    0.00010
HKLF 4




REM  220120_SUGIMOTO_NIPT OLEX2: imported from CIF
REM wR2 = 0.0561, GooF = S = 1.123, Restrained GooF = 1.123 for all data
REM R1 = 0.0229 for 676 Fo > 4sig(Fo) and 0.0303 for all 809 data
REM 63 parameters refined using 0 restraints

END

WGHT      0.0233      0.4352

REM Highest difference peak  1.024,  deepest hole -0.757,  1-sigma level  0.128
Q1    1   0.5006  0.5774  0.5000  10.50000  0.05    1.02
Q2    1   0.3988  0.4784  0.5000  10.50000  0.05    0.62
Q3    1   0.3883  0.5105  0.5000  10.50000  0.05    0.48
Q4    1   0.3047  0.5000  0.2500  10.50000  0.05    0.45
Q5    1   0.4155  0.4666  0.5566  11.00000  0.05    0.44
;
_shelx_res_checksum              40658
_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
;
####################################################################### 
# 
# 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_Ni(x)Pd(1-x)(HDMG)2
_database_code_depnum_ccdc_archive 'CCDC 2149871'
loop_
_audit_author_name
_audit_author_address
'Akira Sugimoto'
;Kumamoto university
Japan
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_audit_creation_date             2022-04-27
_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         'C8 H14 N4 Ni0.599 O4 Pd0.401'
_chemical_formula_sum            'C8 H14 N4 Ni0.60 O4 Pd0.40'
_chemical_formula_weight         308.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni Pd C N O H'
_chemical_oxdiff_usercomment     123K
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'
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+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, z+1/2'

_cell_length_a                   10.5483(7)
_cell_length_b                   16.3439(10)
_cell_length_c                   6.3648(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1097.29(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1924
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.5920
_cell_measurement_theta_min      2.4680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.748
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             629
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2907
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.677
_diffrn_reflns_theta_min         2.298
_diffrn_ambient_temperature      123
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -39.00 -13.00   0.50    4.12    --    5.00  45.00 120.00   52
  2  ω     38.00  79.00   0.50    4.12    --  -10.00  45.00  60.00   82
  3  ω    -99.00   4.00   0.50    4.12    --  -10.00  45.00  60.00  206
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0426334000
_diffrn_orient_matrix_UB_12      0.0116673000
_diffrn_orient_matrix_UB_13      0.0075415000
_diffrn_orient_matrix_UB_21      0.0072843000
_diffrn_orient_matrix_UB_22      0.0661696000
_diffrn_orient_matrix_UB_23      -0.0074809000
_diffrn_orient_matrix_UB_31      -0.0035816000
_diffrn_orient_matrix_UB_32      -0.0037807000
_diffrn_orient_matrix_UB_33      -0.1108431000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                712
_reflns_number_total             802
_reflns_odcompleteness_completeness 99.20
_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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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         0.351
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         802
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0219
_refine_ls_restrained_S_all      1.104
_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)+(0.0246P)²+0.6638P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0554
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Ni01, Pd01}
3. Restrained distances
 O003-H003
 0.84 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Ni01) = Uanis(Pd01)
5. Others
 Sof(Pd01)=0.25*(1-FVAR(2))
 Sof(Ni01)=0.25*FVAR(2)
 Fixed Sof: H00A(0.5) H00B(0.5) H00C(0.5) H00D(0.5) H00E(0.5) H00F(0.5)
6.a Idealised Me refined as rotating group:
 C008(H00A,H00B,H00C), C009(H00D,H00E,H00F)
;
_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
Ni01 Ni 0.500000 0.500000 0.500000 0.01309(12) Uani 0.599(7) 4 d S T P A 3
O002 O 0.59212(14) 0.66406(9) 0.500000 0.0221(4) Uani 1 2 d S T P A .
O003 O 0.23950(16) 0.44627(10) 0.500000 0.0249(4) Uani 1 2 d DS T P A .
N004 N 0.48963(15) 0.61664(12) 0.500000 0.0188(4) Uani 1 2 d S T P . .
N005 N 0.31988(19) 0.51132(11) 0.500000 0.0197(4) Uani 1 2 d S T P . .
C006 C 0.2757(2) 0.58486(14) 0.500000 0.0208(4) Uani 1 2 d S T P A .
C007 C 0.3764(2) 0.64759(13) 0.500000 0.0202(4) Uani 1 2 d S T P A .
C008 C 0.3546(2) 0.73740(14) 0.500000 0.0280(5) Uani 1 2 d S T P . .
H00A H 0.415668 0.763397 0.410337 0.042 Uiso 0.5 1 calc R U P A -1
H00B H 0.363263 0.758098 0.640418 0.042 Uiso 0.5 1 calc R U P A -1
H00C H 0.270684 0.748736 0.449245 0.042 Uiso 0.5 1 calc R U P A -1
C009 C 0.1376(2) 0.60306(15) 0.500000 0.0286(5) Uani 1 2 d S T P . .
H00D H 0.123942 0.657896 0.450874 0.043 Uiso 0.5 1 calc R U P A -1
H00E H 0.104923 0.597750 0.640133 0.043 Uiso 0.5 1 calc R U P A -1
H00F H 0.094656 0.565283 0.408993 0.043 Uiso 0.5 1 calc R U P A -1
H003 H 0.288(5) 0.403(2) 0.500000 0.16(2) Uiso 1 2 d DS . P . .
Pd01 Pd 0.500000 0.500000 0.500000 0.01309(12) Uani 0.401(7) 4 d S T P A 4

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
Ni01 0.01263(16) 0.01516(16) 0.01148(16) 0.000 0.000 -0.00012(9)
O002 0.0222(8) 0.0208(7) 0.0233(8) 0.000 0.000 -0.0059(6)
O003 0.0216(8) 0.0270(8) 0.0260(8) 0.000 0.000 -0.0083(7)
N004 0.0207(9) 0.0207(9) 0.0151(8) 0.000 0.000 -0.0021(6)
N005 0.0180(9) 0.0262(9) 0.0147(8) 0.000 0.000 -0.0043(7)
C006 0.0195(10) 0.0287(11) 0.0143(9) 0.000 0.000 0.0012(9)
C007 0.0226(10) 0.0232(10) 0.0146(9) 0.000 0.000 0.0015(8)
C008 0.0304(12) 0.0245(11) 0.0291(11) 0.000 0.000 0.0037(9)
C009 0.0214(11) 0.0360(12) 0.0284(11) 0.000 0.000 0.0039(10)
Pd01 0.01263(16) 0.01516(16) 0.01148(16) 0.000 0.000 -0.00012(9)

_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
Ni01 N004 1.909(2) 9_666 ?
Ni01 N004 1.909(2) . ?
Ni01 N005 1.909(2) . ?
Ni01 N005 1.909(2) 9_666 ?
O002 N004 1.330(2) . ?
O003 N005 1.360(2) . ?
O003 H003 0.87(2) . ?
N004 C007 1.297(3) . ?
N004 Pd01 1.909(2) . ?
N005 C006 1.289(3) . ?
N005 Pd01 1.909(2) . ?
C006 C007 1.476(3) . ?
C006 C009 1.488(3) . ?
C007 C008 1.486(3) . ?
C008 H00A 0.9600 . ?
C008 H00B 0.9600 . ?
C008 H00C 0.9600 . ?
C009 H00D 0.9600 . ?
C009 H00E 0.9600 . ?
C009 H00F 0.9600 . ?
Pd01 Pd01 3.1824(2) 7_546 ?
Pd01 Pd01 3.1824(2) 7_545 ?

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
N004 Ni01 N004 180.00(10) 9_666 . ?
N005 Ni01 N004 98.84(7) . 9_666 ?
N005 Ni01 N004 98.85(7) 9_666 . ?
N005 Ni01 N004 81.16(7) . . ?
N005 Ni01 N004 81.16(7) 9_666 9_666 ?
N005 Ni01 N005 180.0 . 9_666 ?
N005 O003 H003 106(4) . . ?
O002 N004 Ni01 122.35(13) . . ?
O002 N004 Pd01 122.35(13) . . ?
C007 N004 Ni01 116.23(15) . . ?
C007 N004 O002 121.4(2) . . ?
C007 N004 Pd01 116.23(15) . . ?
O003 N005 Ni01 123.01(14) . . ?
O003 N005 Pd01 123.01(14) . . ?
C006 N005 Ni01 116.73(15) . . ?
C006 N005 O003 120.25(19) . . ?
C006 N005 Pd01 116.73(15) . . ?
N005 C006 C007 112.84(19) . . ?
N005 C006 C009 122.7(2) . . ?
C007 C006 C009 124.5(2) . . ?
N004 C007 C006 113.04(19) . . ?
N004 C007 C008 121.9(2) . . ?
C006 C007 C008 125.1(2) . . ?
C007 C008 H00A 109.5 . . ?
C007 C008 H00B 109.5 . . ?
C007 C008 H00C 109.5 . . ?
H00A C008 H00B 109.5 . . ?
H00A C008 H00C 109.5 . . ?
H00B C008 H00C 109.5 . . ?
C006 C009 H00D 109.5 . . ?
C006 C009 H00E 109.5 . . ?
C006 C009 H00F 109.5 . . ?
H00D C009 H00E 109.5 . . ?
H00D C009 H00F 109.5 . . ?
H00E C009 H00F 109.5 . . ?
N004 Pd01 N004 180.00(10) 9_666 . ?
N004 Pd01 Pd01 90.0 . 7_546 ?
N004 Pd01 Pd01 90.0 9_666 7_545 ?
N004 Pd01 Pd01 90.0 9_666 7_546 ?
N004 Pd01 Pd01 90.0 . 7_545 ?
N005 Pd01 N004 81.16(7) 9_666 9_666 ?
N005 Pd01 N004 98.84(7) . 9_666 ?
N005 Pd01 N004 81.16(7) . . ?
N005 Pd01 N004 98.85(7) 9_666 . ?
N005 Pd01 N005 180.0 . 9_666 ?
N005 Pd01 Pd01 90.0 . 7_546 ?
N005 Pd01 Pd01 90.0 9_666 7_545 ?
N005 Pd01 Pd01 90.0 9_666 7_546 ?
N005 Pd01 Pd01 90.0 . 7_545 ?

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
Ni01 N004 C007 C006 0.0 . . . . ?
Ni01 N004 C007 C008 180.0 . . . . ?
Ni01 N005 C006 C007 0.0 . . . . ?
Ni01 N005 C006 C009 180.0 . . . . ?
O002 N004 C007 C006 180.0 . . . . ?
O002 N004 C007 C008 0.0 . . . . ?
O003 N005 C006 C007 180.0 . . . . ?
O003 N005 C006 C009 0.0 . . . . ?
N005 C006 C007 N004 0.0 . . . . ?
N005 C006 C007 C008 180.0 . . . . ?
C009 C006 C007 N004 180.0 . . . . ?
C009 C006 C007 C008 0.0 . . . . ?
Pd01 N004 C007 C006 0.0 . . . . ?
Pd01 N004 C007 C008 180.0 . . . . ?
Pd01 N005 C006 C007 0.0 . . . . ?
Pd01 N005 C006 C009 180.0 . . . . ?

_shelx_res_file                  
;
TITL 220120_sugimoto_nipd_a.res in Ibam
    220120_sugimoto_nipd.res
    created by SHELXL-2018/3 at 16:34:31 on 27-Apr-2022
REM Old TITL 220120_sugimoto_NiPd in Ibam #72
REM SHELXT solution in Ibam: R1 0.058, Rweak 0.001, Alpha 0.047
REM <I/s> 0.277 for 51 systematic absences, Orientation as input
REM Formula found by SHELXT: C12 O4 Ni
CELL 0.71073 10.5483 16.3439 6.3648 90 90 90
ZERR 4 0.0007 0.001 0.0004 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N Ni O Pd
UNIT 32 56 16 2.39 16 1.61
EADP Ni01 Pd01
DFIX 0.84 O003 H003
EXYZ Ni01 Pd01

L.S. 4 0 0
PLAN  5
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2 53
ACTA
OMIT 0 2 0
REM <olex2.extras>
REM <HklSrc "%.\\220120_sugimoto_NiPd.hkl">
REM </olex2.extras>

WGHT    0.024600    0.663800
FVAR       0.25285   0.59854
PART 3
NI01  4    0.500000    0.500000    0.500000    20.25000    0.01263    0.01516 =
         0.01148    0.00000    0.00000   -0.00012
PART 0
O002  5    0.592123    0.664058    0.500000    10.50000    0.02220    0.02076 =
         0.02334    0.00000    0.00000   -0.00593
O003  5    0.239500    0.446269    0.500000    10.50000    0.02164    0.02704 =
         0.02601    0.00000    0.00000   -0.00829
N004  3    0.489631    0.616639    0.500000    10.50000    0.02068    0.02071 =
         0.01514    0.00000    0.00000   -0.00211
N005  3    0.319884    0.511318    0.500000    10.50000    0.01800    0.02625 =
         0.01473    0.00000    0.00000   -0.00434
C006  1    0.275748    0.584860    0.500000    10.50000    0.01952    0.02865 =
         0.01426    0.00000    0.00000    0.00119
C007  1    0.376369    0.647594    0.500000    10.50000    0.02263    0.02318 =
         0.01464    0.00000    0.00000    0.00154
C008  1    0.354567    0.737401    0.500000    10.50000    0.03035    0.02454 =
         0.02910    0.00000    0.00000    0.00366
PART -1
AFIX 137
H00A  2    0.415668    0.763397    0.410337    10.50000   -1.50000
H00B  2    0.363263    0.758098    0.640418    10.50000   -1.50000
H00C  2    0.270684    0.748736    0.449245    10.50000   -1.50000
AFIX   0
PART 0
C009  1    0.137564    0.603061    0.500000    10.50000    0.02142    0.03597 =
         0.02840    0.00000    0.00000    0.00392
PART -1
AFIX 137
H00D  2    0.123942    0.657896    0.450874    10.50000   -1.50000
H00E  2    0.104923    0.597750    0.640133    10.50000   -1.50000
H00F  2    0.094656    0.565283    0.408993    10.50000   -1.50000
AFIX   0
PART 0
H003  2    0.287609    0.403086    0.500000    10.50000    0.15847
PART 4
PD01  6    0.500000    0.500000    0.500000   -20.25000    0.01263    0.01516 =
         0.01148    0.00000    0.00000   -0.00012
HKLF 4




REM  220120_sugimoto_nipd_a.res in Ibam
REM wR2 = 0.0554, GooF = S = 1.103, Restrained GooF = 1.104 for all data
REM R1 = 0.0219 for 712 Fo > 4sig(Fo) and 0.0251 for all 802 data
REM 59 parameters refined using 1 restraints

END

WGHT      0.0246      0.6639

REM Highest difference peak  0.351,  deepest hole -0.696,  1-sigma level  0.146
Q1    1   0.0392  0.6049  0.7784  11.00000  0.05    0.35
Q2    1   0.0196  0.5000  0.2500  10.50000  0.05    0.34
Q3    1   0.1161  0.5000  0.2500  10.50000  0.05    0.34
Q4    1   0.0607  0.5833  0.7148  11.00000  0.05    0.34
Q5    1   0.0343  0.6564  0.7550  11.00000  0.05    0.31
;
_shelx_res_checksum              10571
_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 1.114
_oxdiff_exptl_absorpt_empirical_full_min 0.933
####################################################################### 
# 
# 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_Pd(x)Pt(1-x)(HDMG)2
_database_code_depnum_ccdc_archive 'CCDC 2149873'
loop_
_audit_author_name
_audit_author_address
'Akira Sugimoto'
;Kumamoto university
Japan
;
_audit_update_record             
;
2022-04-28 deposited with the CCDC.	2022-05-23 downloaded from the CCDC.
;
_audit_creation_date             2022-04-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H14 N4 O4 Pd0.507 Pt0.493'
_chemical_formula_sum            'C8 H14 N4 O4 Pd0.50 Pt0.50'
_chemical_formula_weight         380.98
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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           72
_space_group_name_H-M_alt        'I b a m'
_space_group_name_Hall           '-I 2 2c'
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+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, z+1/2'

_cell_length_a                   16.3923(12)
_cell_length_b                   10.6456(7)
_cell_length_c                   6.3980(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1116.49(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1443
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.9210
_cell_measurement_theta_min      2.4560
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.266
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2493
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.857
_diffrn_reflns_theta_min         2.485
_diffrn_ambient_temperature      123.00
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.831
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -50.00 -15.00   0.50    1.77    --    5.00  45.00  90.00   70
  2  ω     50.00  79.00   0.50    1.77    --  -10.00  45.00  30.00   58
  3  ω    -99.00 -17.00   0.50    1.77    --  -10.00  45.00  30.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                649
_reflns_number_total             791
_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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.924
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         791
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0214
_refine_ls_restrained_S_all      1.089
_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)+(0.0382P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0605
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Pt01, Pd1}
3. Restrained distances
 O005-H005
 0.82 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Pt01) = Uanis(Pd1)
5. Others
 Sof(Pd1)=0.25*(1-FVAR(2))
 Sof(Pt01)=0.25*FVAR(2)
 Fixed Sof: H00A(0.5) H00B(0.5) H00C(0.5) H00D(0.5) H00E(0.5) H00F(0.5)
6.a Idealised Me refined as rotating group:
 C008(H00A,H00B,H00C), C009(H00D,H00E,H00F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt01 Pt 0.500000 0.500000 0.500000 0.01176(13) Uani 0.493(11) 4 d S T P A 1
O002 O 0.66603(18) 0.5891(3) 0.500000 0.0216(7) Uani 1 2 d S T P A .
N003 N 0.6202(3) 0.4872(3) 0.500000 0.0169(8) Uani 1 2 d S T P . .
N004 N 0.5137(2) 0.3171(4) 0.500000 0.0175(8) Uani 1 2 d S T P . .
O005 O 0.44808(18) 0.2370(3) 0.500000 0.0218(7) Uani 1 2 d DS T P A .
C006 C 0.6503(3) 0.3741(4) 0.500000 0.0185(9) Uani 1 2 d S T P A .
C007 C 0.5873(2) 0.2736(4) 0.500000 0.0201(9) Uani 1 2 d S T P A .
C008 C 0.7397(2) 0.3517(4) 0.500000 0.0255(9) Uani 1 2 d S T P . .
H00A H 0.750980 0.267278 0.446083 0.038 Uiso 0.5 1 calc R U P A -1
H00B H 0.760660 0.358783 0.642980 0.038 Uiso 0.5 1 calc R U P A -1
H00C H 0.766520 0.414178 0.410937 0.038 Uiso 0.5 1 calc R U P A -1
C009 C 0.6060(2) 0.1366(3) 0.500000 0.0241(9) Uani 1 2 d S T P . .
H00D H 0.565796 0.092252 0.585977 0.036 Uiso 0.5 1 calc R U P A -1
H00E H 0.660710 0.123002 0.557497 0.036 Uiso 0.5 1 calc R U P A -1
H00F H 0.603833 0.104575 0.356526 0.036 Uiso 0.5 1 calc R U P A -1
H005 H 0.405(6) 0.279(15) 0.500000 0.32(9) Uiso 1 2 d DS . P . .
Pd1 Pd 0.500000 0.500000 0.500000 0.01176(13) Uani 0.507(11) 4 d S T P A 2

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
Pt01 0.01432(18) 0.01283(17) 0.00812(16) 0.000 0.000 -0.00056(8)
O002 0.0225(15) 0.0199(15) 0.0224(15) 0.000 0.000 -0.0073(12)
N003 0.0175(18) 0.0209(17) 0.0123(16) 0.000 0.000 -0.0020(12)
N004 0.0241(17) 0.0158(18) 0.0127(16) 0.000 0.000 -0.0012(13)
O005 0.0244(15) 0.0191(14) 0.0218(15) 0.000 0.000 -0.0094(12)
C006 0.0236(19) 0.0219(18) 0.0101(16) 0.000 0.000 0.0041(17)
C007 0.027(2) 0.021(2) 0.0123(17) 0.000 0.000 -0.0017(17)
C008 0.0209(18) 0.027(2) 0.028(2) 0.000 0.000 0.0059(17)
C009 0.031(2) 0.0184(19) 0.0231(19) 0.000 0.000 0.0033(16)
Pd1 0.01432(18) 0.01283(17) 0.00812(16) 0.000 0.000 -0.00056(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
Pt01 Pt01 3.1990(2) 7_545 ?
Pt01 Pt01 3.1990(2) 7_546 ?
Pt01 N003 1.975(4) 9_666 ?
Pt01 N003 1.975(4) . ?
Pt01 N004 1.960(4) . ?
Pt01 N004 1.960(4) 9_666 ?
O002 N003 1.320(4) . ?
N003 C006 1.301(5) . ?
N003 Pd1 1.975(4) . ?
N004 O005 1.372(4) . ?
N004 C007 1.292(5) . ?
N004 Pd1 1.960(4) . ?
O005 H005 0.83(2) . ?
C006 C007 1.487(6) . ?
C006 C008 1.485(5) . ?
C007 C009 1.490(5) . ?
C008 H00A 0.9800 . ?
C008 H00B 0.9800 . ?
C008 H00C 0.9800 . ?
C009 H00D 0.9800 . ?
C009 H00E 0.9800 . ?
C009 H00F 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
Pt01 Pt01 Pt01 180.0 7_546 7_545 ?
N003 Pt01 Pt01 90.0 . 7_545 ?
N003 Pt01 Pt01 90.0 9_666 7_546 ?
N003 Pt01 Pt01 90.0 9_666 7_545 ?
N003 Pt01 Pt01 90.0 . 7_546 ?
N003 Pt01 N003 180.0 9_666 . ?
N004 Pt01 Pt01 90.0 . 7_546 ?
N004 Pt01 Pt01 90.0 . 7_545 ?
N004 Pt01 Pt01 90.0 9_666 7_546 ?
N004 Pt01 Pt01 90.0 9_666 7_545 ?
N004 Pt01 N003 79.47(13) . . ?
N004 Pt01 N003 100.53(13) 9_666 . ?
N004 Pt01 N003 100.53(13) . 9_666 ?
N004 Pt01 N003 79.47(13) 9_666 9_666 ?
N004 Pt01 N004 180.0 9_666 . ?
O002 N003 Pt01 120.7(3) . . ?
O002 N003 Pd1 120.7(3) . . ?
C006 N003 Pt01 116.2(3) . . ?
C006 N003 O002 123.0(4) . . ?
C006 N003 Pd1 116.2(3) . . ?
O005 N004 Pt01 121.9(3) . . ?
O005 N004 Pd1 121.9(3) . . ?
C007 N004 Pt01 117.5(3) . . ?
C007 N004 O005 120.6(4) . . ?
C007 N004 Pd1 117.5(3) . . ?
N004 O005 H005 109(10) . . ?
N003 C006 C007 113.7(4) . . ?
N003 C006 C008 121.5(4) . . ?
C008 C006 C007 124.7(4) . . ?
N004 C007 C006 113.0(4) . . ?
N004 C007 C009 122.9(4) . . ?
C006 C007 C009 124.1(4) . . ?
C006 C008 H00A 109.5 . . ?
C006 C008 H00B 109.5 . . ?
C006 C008 H00C 109.5 . . ?
H00A C008 H00B 109.5 . . ?
H00A C008 H00C 109.5 . . ?
H00B C008 H00C 109.5 . . ?
C007 C009 H00D 109.5 . . ?
C007 C009 H00E 109.5 . . ?
C007 C009 H00F 109.5 . . ?
H00D C009 H00E 109.5 . . ?
H00D C009 H00F 109.5 . . ?
H00E C009 H00F 109.5 . . ?
N003 Pd1 N003 180.0 9_666 . ?
N004 Pd1 N003 79.47(13) . . ?
N004 Pd1 N003 79.47(13) 9_666 9_666 ?
N004 Pd1 N003 100.53(13) 9_666 . ?
N004 Pd1 N003 100.53(13) . 9_666 ?
N004 Pd1 N004 180.0 9_666 . ?

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
Pt01 N003 C006 C007 0.0 . . . . ?
Pt01 N003 C006 C008 180.0 . . . . ?
Pt01 N004 C007 C006 0.0 . . . . ?
Pt01 N004 C007 C009 180.0 . . . . ?
O002 N003 C006 C007 180.0 . . . . ?
O002 N003 C006 C008 0.0 . . . . ?
N003 C006 C007 N004 0.0 . . . . ?
N003 C006 C007 C009 180.0 . . . . ?
O005 N004 C007 C006 180.0 . . . . ?
O005 N004 C007 C009 0.0 . . . . ?
C008 C006 C007 N004 180.0 . . . . ?
C008 C006 C007 C009 0.0 . . . . ?
Pd1 N003 C006 C007 0.0 . . . . ?
Pd1 N003 C006 C008 180.0 . . . . ?
Pd1 N004 C007 C006 0.0 . . . . ?
Pd1 N004 C007 C009 180.0 . . . . ?

_shelx_res_file                  
;
TITL 220120_sugimoto_pdpt_a.res in Ibam
    220120_sugimoto_pdpt.res
    created by SHELXL-2018/3 at 08:58:38 on 28-Apr-2022
REM Old TITL 220120_sugimoto_PdPt in Iba2
REM SHELXT solution in Ibam
REM R1 0.048, Rweak 0.000, Alpha 0.020, Orientation as input
REM Formula found by SHELXT: C6 N2 O8 Pt
CELL 0.71073 16.3923 10.6456 6.398 90 90 90
ZERR 4 0.0012 0.0007 0.0004 0 0 0
LATT 2
SYMM -X,-Y,+Z
SYMM 0.5-X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O Pd Pt
UNIT 32 56 16 16 2 2
DFIX 0.82 O005 H005
EADP Pt01 Pd1
EXYZ Pt01 Pd1

L.S. 20 0 0
PLAN  5
TEMP -150.15
CONF
BOND $H
list 4
MORE -1
fmap 2 53
acta
REM <olex2.extras>
REM <HklSrc "%.\\220120_sugimoto_PdPt.hkl">
REM </olex2.extras>

WGHT    0.038200
FVAR       0.19011   0.49327
PART 1
PT01  6    0.500000    0.500000    0.500000    20.25000    0.01432    0.01283 =
         0.00812    0.00000    0.00000   -0.00056
PART 0
O002  4    0.666030    0.589118    0.500000    10.50000    0.02254    0.01995 =
         0.02237    0.00000    0.00000   -0.00728
N003  3    0.620206    0.487185    0.500000    10.50000    0.01746    0.02089 =
         0.01231    0.00000    0.00000   -0.00197
N004  3    0.513675    0.317089    0.500000    10.50000    0.02406    0.01579 =
         0.01268    0.00000    0.00000   -0.00125
O005  4    0.448084    0.236973    0.500000    10.50000    0.02437    0.01908 =
         0.02183    0.00000    0.00000   -0.00937
C006  1    0.650296    0.374110    0.500000    10.50000    0.02361    0.02188 =
         0.01008    0.00000    0.00000    0.00407
C007  1    0.587292    0.273629    0.500000    10.50000    0.02722    0.02081 =
         0.01231    0.00000    0.00000   -0.00172
C008  1    0.739718    0.351680    0.500000    10.50000    0.02094    0.02725 =
         0.02827    0.00000    0.00000    0.00589
PART -1
AFIX 137
H00A  2    0.750980    0.267278    0.446083    10.50000   -1.50000
H00B  2    0.760660    0.358783    0.642980    10.50000   -1.50000
H00C  2    0.766520    0.414178    0.410937    10.50000   -1.50000
AFIX   0
PART 0
C009  1    0.606010    0.136638    0.500000    10.50000    0.03078    0.01839 =
         0.02313    0.00000    0.00000    0.00333
PART -1
AFIX 137
H00D  2    0.565796    0.092252    0.585977    10.50000   -1.50000
H00E  2    0.660710    0.123002    0.557497    10.50000   -1.50000
H00F  2    0.603833    0.104575    0.356526    10.50000   -1.50000
AFIX   0
PART 0
H005  2    0.405287    0.278915    0.500000    10.50000    0.32417
PART 2
PD1   5    0.500000    0.500000    0.500000   -20.25000    0.01432    0.01283 =
         0.00812    0.00000    0.00000   -0.00056
HKLF 4




REM  220120_sugimoto_pdpt_a.res in Ibam
REM wR2 = 0.0605, GooF = S = 1.089, Restrained GooF = 1.089 for all data
REM R1 = 0.0214 for 649 Fo > 4sig(Fo) and 0.0277 for all 791 data
REM 59 parameters refined using 1 restraints

END

WGHT      0.0382      0.0000

REM Highest difference peak  0.924,  deepest hole -1.348,  1-sigma level  0.161
Q1    1   0.4443  0.4983  0.5000  10.50000  0.05    0.92
Q2    1   0.5030  0.4167  0.5000  10.50000  0.05    0.84
Q3    1   0.7206  0.3817  0.7469  11.00000  0.05    0.51
Q4    1   0.4763  0.2888  0.5000  10.50000  0.05    0.49
Q5    1   0.6260  0.3154  0.5000  10.50000  0.05    0.48
;
_shelx_res_checksum              77768
_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
;
