# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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_shi_2057_rola
_database_code_depnum_ccdc_archive 'CCDC 1519078'
loop_
_audit_author_name
_audit_author_address
'Sergiu Shova'
;Institute of Macromolecular Chemistry of the Romanian Academy
Romania
;
_audit_update_record             
;
2018-08-29 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;
_audit_creation_date             2018-08-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C20 H22 N8 Pd'
_chemical_formula_sum            'C20 H22 N8 Pd'
_chemical_formula_weight         480.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H20 N8 Cl2 Pd1'
_chemical_oxdiff_usercomment     '_2'
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'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.4343(3)
_cell_length_b                   8.4913(3)
_cell_length_c                   10.9739(5)
_cell_angle_alpha                88.134(3)
_cell_angle_beta                 80.550(4)
_cell_angle_gamma                76.336(4)
_cell_volume                     485.36(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    483
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      26.9690
_cell_measurement_theta_min      3.0870
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.828
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_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    1.645
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3495
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         1.881
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector_area_resol_mean 16.1593
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -25.00   15.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789  -99.0000   30.0000 40

#__ type_ start__ end____ width___ exp.time_
  2 omega  -22.00    3.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7789  -99.0000  -90.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.1228541000
_diffrn_orient_matrix_UB_12      -0.0020071000
_diffrn_orient_matrix_UB_13      -0.0130365000
_diffrn_orient_matrix_UB_21      -0.0299717000
_diffrn_orient_matrix_UB_22      -0.0333461000
_diffrn_orient_matrix_UB_23      0.0591264000
_diffrn_orient_matrix_UB_31      -0.0504158000
_diffrn_orient_matrix_UB_32      0.0792348000
_diffrn_orient_matrix_UB_33      0.0250109000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1696
_reflns_number_total             1724
_reflns_odcompleteness_completeness 30.45
_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, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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         0.593
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1724
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0251
_refine_ls_restrained_S_all      1.109
_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)+(0.0208P)²+0.0035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0545
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.500000 0.000000 0.000000 0.02147(10) Uani 1 2 d S T P . .
N1 N 0.7284(4) 0.0734(2) 0.09955(19) 0.0243(5) Uani 1 1 d . . . . .
N2 N 0.8354(4) 0.0210(2) 0.20227(19) 0.0261(5) Uani 1 1 d . . . . .
N3 N 0.9586(4) 0.2482(2) 0.1298(2) 0.0265(5) Uani 1 1 d . . . . .
N4 N 0.5561(4) 0.2025(2) -0.09449(19) 0.0217(4) Uani 1 1 d . . . . .
C1 C 0.4523(5) 0.2604(3) -0.1948(2) 0.0279(6) Uani 1 1 d . . . . .
H1 H 0.345706 0.206024 -0.225788 0.034 Uiso 1 1 calc R . . . .
C2 C 0.5010(5) 0.3983(3) -0.2523(3) 0.0330(6) Uani 1 1 d . . . . .
H2 H 0.427556 0.436766 -0.321479 0.040 Uiso 1 1 calc R . . . .
C3 C 0.6583(5) 0.4797(3) -0.2075(3) 0.0328(6) Uani 1 1 d . . . . .
H3 H 0.691592 0.573520 -0.245674 0.039 Uiso 1 1 calc R . . . .
C4 C 0.7660(5) 0.4200(3) -0.1052(2) 0.0292(6) Uani 1 1 d . . . . .
H4 H 0.874208 0.472688 -0.073822 0.035 Uiso 1 1 calc R . . . .
C5 C 0.7116(5) 0.2816(3) -0.0499(2) 0.0236(6) Uani 1 1 d . . . . .
C6 C 0.8058(5) 0.2068(3) 0.0601(2) 0.0238(6) Uani 1 1 d . . . . .
C7 C 0.9715(5) 0.1296(3) 0.2165(2) 0.0251(6) Uani 1 1 d . . . . .
C8 C 1.1215(5) 0.1195(3) 0.3196(2) 0.0288(6) Uani 1 1 d . . . . .
H8A H 1.289910 0.136849 0.286798 0.035 Uiso 1 1 calc R . . . .
H8B H 1.145048 0.011156 0.353626 0.035 Uiso 1 1 calc R . . . .
C9 C 0.9960(5) 0.2415(3) 0.4231(3) 0.0353(6) Uani 1 1 d . . . . .
H9A H 0.949067 0.348429 0.387616 0.042 Uiso 1 1 calc R . . . .
H9B H 0.839722 0.214118 0.464357 0.042 Uiso 1 1 calc R . . . .
C10 C 1.1677(6) 0.2466(4) 0.5172(3) 0.0476(8) Uani 1 1 d . . . . .
H10A H 1.074428 0.318268 0.583647 0.071 Uiso 1 1 calc GR . . . .
H10B H 1.314276 0.284948 0.478785 0.071 Uiso 1 1 calc GR . . . .
H10C H 1.223670 0.139675 0.548950 0.071 Uiso 1 1 calc GR . . . .


_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 N1 1.994(2) 2_655 ?
Pd1 N1 1.994(2) . ?
Pd1 N4 2.0382(19) . ?
Pd1 N4 2.0382(19) 2_655 ?
N1 N2 1.366(3) . ?
N1 C6 1.334(3) . ?
N2 C7 1.338(3) . ?
N3 C6 1.327(3) . ?
N3 C7 1.360(3) . ?
N4 C1 1.346(3) . ?
N4 C5 1.352(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.372(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.374(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.378(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.377(3) . ?
C5 C6 1.457(3) . ?
C7 C8 1.488(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.522(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.509(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 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
N1 Pd1 N1 180.0 2_655 . ?
N1 Pd1 N4 79.36(8) . . ?
N1 Pd1 N4 100.64(8) 2_655 . ?
N1 Pd1 N4 100.64(8) . 2_655 ?
N1 Pd1 N4 79.36(8) 2_655 2_655 ?
N4 Pd1 N4 180.0 . 2_655 ?
N2 N1 Pd1 136.36(16) . . ?
C6 N1 Pd1 116.05(16) . . ?
C6 N1 N2 107.59(19) . . ?
C7 N2 N1 103.5(2) . . ?
C6 N3 C7 101.6(2) . . ?
C1 N4 Pd1 125.26(17) . . ?
C1 N4 C5 119.3(2) . . ?
C5 N4 Pd1 115.40(15) . . ?
N4 C1 H1 119.5 . . ?
N4 C1 C2 121.1(2) . . ?
C2 C1 H1 119.5 . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0(2) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 120.5 . . ?
C2 C3 C4 119.0(2) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.3(2) . . ?
C5 C4 H4 120.4 . . ?
N4 C5 C4 121.4(2) . . ?
N4 C5 C6 113.2(2) . . ?
C4 C5 C6 125.5(2) . . ?
N1 C6 C5 116.0(2) . . ?
N3 C6 N1 113.0(2) . . ?
N3 C6 C5 131.0(2) . . ?
N2 C7 N3 114.3(2) . . ?
N2 C7 C8 122.0(2) . . ?
N3 C7 C8 123.8(2) . . ?
C7 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
C7 C8 C9 113.8(2) . . ?
H8A C8 H8B 107.7 . . ?
C9 C8 H8A 108.8 . . ?
C9 C8 H8B 108.8 . . ?
C8 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 C8 113.0(2) . . ?
C10 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 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 N2 C7 179.27(17) . . . . ?
Pd1 N1 C6 N3 -179.50(16) . . . . ?
Pd1 N1 C6 C5 0.5(3) . . . . ?
Pd1 N4 C1 C2 179.87(18) . . . . ?
Pd1 N4 C5 C4 179.87(18) . . . . ?
Pd1 N4 C5 C6 -1.1(3) . . . . ?
N1 N2 C7 N3 0.1(3) . . . . ?
N1 N2 C7 C8 179.7(2) . . . . ?
N2 N1 C6 N3 -0.1(3) . . . . ?
N2 N1 C6 C5 179.89(19) . . . . ?
N2 C7 C8 C9 -104.1(3) . . . . ?
N3 C7 C8 C9 75.5(3) . . . . ?
N4 C1 C2 C3 0.1(4) . . . . ?
N4 C5 C6 N1 0.4(3) . . . . ?
N4 C5 C6 N3 -179.6(2) . . . . ?
C1 N4 C5 C4 -0.1(3) . . . . ?
C1 N4 C5 C6 178.9(2) . . . . ?
C1 C2 C3 C4 0.3(4) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C3 C4 C5 N4 0.5(4) . . . . ?
C3 C4 C5 C6 -178.4(2) . . . . ?
C4 C5 C6 N1 179.4(2) . . . . ?
C4 C5 C6 N3 -0.6(4) . . . . ?
C5 N4 C1 C2 -0.2(4) . . . . ?
C6 N1 N2 C7 0.0(3) . . . . ?
C6 N3 C7 N2 -0.1(3) . . . . ?
C6 N3 C7 C8 -179.7(2) . . . . ?
C7 N3 C6 N1 0.1(3) . . . . ?
C7 N3 C6 C5 -179.9(2) . . . . ?
C7 C8 C9 C10 -171.5(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shi_4129_rola
_database_code_depnum_ccdc_archive 'CCDC 1910554'
loop_
_audit_author_name
_audit_author_address
'Sergiu Shova'
;Institute of Macromolecular Chemistry of the Romanian Academy
Romania
;
_audit_update_record             
;
2019-04-16 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;
_audit_creation_date             2019-04-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H18 N8 Pd'
_chemical_formula_sum            'C18 H18 N8 Pd'
_chemical_formula_weight         452.80
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H15N8Pd1
_chemical_oxdiff_usercomment     s-Pd(LEt)2
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'
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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   4.5732(7)
_cell_length_b                   9.8193(12)
_cell_length_c                   10.5527(13)
_cell_angle_alpha                71.200(11)
_cell_angle_beta                 86.444(11)
_cell_angle_gamma                76.934(12)
_cell_volume                     436.95(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    648
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.7460
_cell_measurement_theta_min      2.0540
_shelx_estimated_absorpt_T_max   0.979
_shelx_estimated_absorpt_T_min   0.899
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.1046
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2905
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.039
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   3.00   1.00   30.00    --  -15.44 -38.00  30.00   86
  2  ω    -17.00  23.00   1.00   30.00    --  -15.44 -99.00-150.00   40
  3  ω     41.00  85.00   1.00   30.00    --   17.79  77.00-150.00   44
  4  ω      2.00  85.00   1.00   30.00    --   17.79  57.00 -30.00   83
  5  ω     24.00  76.00   1.00   30.00    --   17.79  57.00  30.00   52
  6  ω     35.00  90.00   1.00   30.00    --   17.79 178.00 -90.00   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1523687000
_diffrn_orient_matrix_UB_12      -0.0036513000
_diffrn_orient_matrix_UB_13      -0.0032704000
_diffrn_orient_matrix_UB_21      0.0336508000
_diffrn_orient_matrix_UB_22      -0.0741739000
_diffrn_orient_matrix_UB_23      0.0425990000
_diffrn_orient_matrix_UB_31      -0.0317197000
_diffrn_orient_matrix_UB_32      0.0244637000
_diffrn_orient_matrix_UB_33      0.0567166000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1409
_reflns_number_total             1543
_reflns_odcompleteness_completeness 99.33
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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         0.769
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1543
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0615
_refine_ls_restrained_S_all      1.081
_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)+(0.0185P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0865
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.000000 0.500000 0.500000 0.0263(2) Uani 1 2 d S T P . .
N1 N -0.1158(10) 0.6121(4) 0.3048(4) 0.0272(11) Uani 1 1 d . . . . .
N2 N 0.3271(10) 0.3948(5) 0.4093(4) 0.0303(12) Uani 1 1 d . . . . .
N3 N 0.5653(10) 0.2806(5) 0.4478(4) 0.0323(12) Uani 1 1 d . . . . .
N4 N 0.5401(10) 0.3688(5) 0.2208(4) 0.0291(12) Uani 1 1 d . . . . .
C1 C -0.3534(13) 0.7227(6) 0.2611(5) 0.0343(15) Uani 1 1 d . . . . .
H1 H -0.478512 0.755657 0.323053 0.041 Uiso 1 1 calc R . . . .
C2 C -0.4180(14) 0.7896(6) 0.1262(5) 0.0400(16) Uani 1 1 d . . . . .
H2 H -0.587739 0.864789 0.097646 0.048 Uiso 1 1 calc R . . . .
C3 C -0.2300(14) 0.7440(7) 0.0355(5) 0.0421(17) Uani 1 1 d . . . . .
H3 H -0.271349 0.788760 -0.055541 0.050 Uiso 1 1 calc R . . . .
C4 C 0.0195(14) 0.6329(6) 0.0773(5) 0.0357(15) Uani 1 1 d . . . . .
H4 H 0.150200 0.602778 0.015533 0.043 Uiso 1 1 calc R . . . .
C5 C 0.0724(12) 0.5669(6) 0.2125(5) 0.0272(14) Uani 1 1 d . . . . .
C6 C 0.3188(13) 0.4446(6) 0.2752(5) 0.0272(14) Uani 1 1 d . . . . .
C7 C 0.6896(12) 0.2685(6) 0.3322(5) 0.0297(14) Uani 1 1 d . . . . .
C8 C 0.9549(13) 0.1511(6) 0.3285(6) 0.0403(16) Uani 1 1 d . . . . .
H8A H 1.045556 0.106687 0.417201 0.048 Uiso 1 1 calc R . . . .
H8B H 1.101851 0.194849 0.268347 0.048 Uiso 1 1 calc R . . . .
C9 C 0.8779(15) 0.0323(6) 0.2830(6) 0.059(2) Uani 1 1 d . . . . .
H9A H 0.798020 0.074682 0.193411 0.089 Uiso 1 1 calc GR . . . .
H9B H 0.731099 -0.010825 0.341711 0.089 Uiso 1 1 calc GR . . . .
H9C H 1.055661 -0.042375 0.285080 0.089 Uiso 1 1 calc GR . . . .


_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 N1 2.036(4) 2_566 ?
Pd1 N1 2.037(4) . ?
Pd1 N2 1.995(4) . ?
Pd1 N2 1.995(4) 2_566 ?
N1 C1 1.333(6) . ?
N1 C5 1.374(6) . ?
N2 N3 1.348(5) . ?
N2 C6 1.340(6) . ?
N3 C7 1.342(6) . ?
N4 C6 1.330(6) . ?
N4 C7 1.367(6) . ?
C1 C2 1.381(7) . ?
C2 C3 1.362(7) . ?
C3 C4 1.370(7) . ?
C4 C5 1.375(7) . ?
C5 C6 1.455(7) . ?
C7 C8 1.481(7) . ?
C8 C9 1.511(8) . ?

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 Pd1 N1 180.0 2_566 . ?
N2 Pd1 N1 79.73(18) 2_566 2_566 ?
N2 Pd1 N1 79.73(18) . . ?
N2 Pd1 N1 100.27(18) 2_566 . ?
N2 Pd1 N1 100.27(18) . 2_566 ?
N2 Pd1 N2 180.0 . 2_566 ?
C1 N1 Pd1 125.8(3) . . ?
C1 N1 C5 118.8(5) . . ?
C5 N1 Pd1 115.4(4) . . ?
N3 N2 Pd1 136.4(3) . . ?
C6 N2 Pd1 115.7(4) . . ?
C6 N2 N3 107.9(4) . . ?
C7 N3 N2 104.1(4) . . ?
C6 N4 C7 101.4(4) . . ?
N1 C1 C2 121.6(5) . . ?
C3 C2 C1 119.2(6) . . ?
C2 C3 C4 120.6(5) . . ?
C3 C4 C5 118.5(5) . . ?
N1 C5 C4 121.4(5) . . ?
N1 C5 C6 112.4(5) . . ?
C4 C5 C6 126.2(5) . . ?
N2 C6 C5 116.8(5) . . ?
N4 C6 N2 112.8(5) . . ?
N4 C6 C5 130.4(5) . . ?
N3 C7 N4 113.8(5) . . ?
N3 C7 C8 122.0(5) . . ?
N4 C7 C8 124.0(5) . . ?
C7 C8 C9 112.8(5) . . ?

_olex2_date_sample_data_collection 2019-03-04
_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 1.179
_oxdiff_exptl_absorpt_empirical_full_min 0.862
####################################################################### 
# 
# 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_shi_3790_rola
_database_code_depnum_ccdc_archive 'CCDC 1864447'
loop_
_audit_author_name
_audit_author_address
'Sergiu Shova'
;Institute of Macromolecular Chemistry of the Romanian Academy
Romania
;
_audit_update_record             
;
2018-08-29 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;
_audit_creation_date             2018-08-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '3(C22 H26 N8 Pd), 2(C H Cl3), H4 O2'
_chemical_formula_sum            'C68 H84 Cl6 N24 O2 Pd3'
_chemical_formula_weight         1801.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H20N6O2Pd1
_chemical_oxdiff_usercomment     s-Pd(Lt-but)2(cryst)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   30.046(8)
_cell_length_b                   6.8662(12)
_cell_length_c                   23.785(6)
_cell_angle_alpha                90
_cell_angle_beta                 126.80(4)
_cell_angle_gamma                90
_cell_volume                     3929(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1627
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.9650
_cell_measurement_theta_min      1.7520
_shelx_estimated_absorpt_T_max   0.872
_shelx_estimated_absorpt_T_min   0.834
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.1462
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7696
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.693
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -41.00  23.00   1.00   30.00    --   26.04 -38.00  90.00   64
  2  ω     40.00  95.00   1.00   30.00    --   26.04  38.00 -90.00   55
  3  ω    -27.00  36.00   1.00   30.00    --   26.04 -57.00-180.00   63
  4  ω    -96.00 -39.00   1.00   30.00    --  -23.85-178.00 -30.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0028073000
_diffrn_orient_matrix_UB_12      -0.0734265000
_diffrn_orient_matrix_UB_13      0.0186359000
_diffrn_orient_matrix_UB_21      -0.0221944000
_diffrn_orient_matrix_UB_22      -0.0421456000
_diffrn_orient_matrix_UB_23      -0.0322859000
_diffrn_orient_matrix_UB_31      0.0192820000
_diffrn_orient_matrix_UB_32      -0.0591997000
_diffrn_orient_matrix_UB_33      -0.0002068000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2353
_reflns_number_total             3784
_reflns_odcompleteness_completeness 99.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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         1.231
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.105
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3784
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0601
_refine_ls_restrained_S_all      0.928
_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)+(0.0010P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.1030
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H9AA(0.5) H9AB(0.5) H9AC(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
 H10D(0.5) H10E(0.5) H10F(0.5) H1WA(0.5)
3.a Riding coordinates:
 C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C19A(H19A,H19B,H19C), C20A(H20A,
 H20B,H20C), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), O1W(H1WA,H1WB)
3.b Ternary CH refined with riding coordinates:
 C1(H1)
3.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C11A(H11A), C12A(H12A), C13A(H13A),
 C14A(H14A), C1B(H1B), C2B(H2B), C3B(H3B), C4B(H4B)
;
_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
Pd1A Pd 0.16706(3) 0.500000 0.35756(3) 0.0316(2) Uani 1 2 d S T P . .
N1A N 0.2476(3) 0.500000 0.3942(3) 0.0331(18) Uani 1 2 d S T P . .
N2A N 0.2757(3) 0.500000 0.3660(3) 0.0375(19) Uani 1 2 d S T P . .
N3A N 0.3366(3) 0.500000 0.4855(3) 0.0326(18) Uani 1 2 d S T P . .
N4A N 0.2056(3) 0.500000 0.4624(3) 0.0263(16) Uani 1 2 d S T P . .
N5A N 0.0871(3) 0.500000 0.3207(3) 0.0342(18) Uani 1 2 d S T P . .
N6A N 0.0586(3) 0.500000 0.3489(3) 0.0383(19) Uani 1 2 d S T P . .
N7A N -0.0028(3) 0.500000 0.2300(4) 0.0364(18) Uani 1 2 d S T P . .
N8A N 0.1288(3) 0.500000 0.2526(3) 0.0255(16) Uani 1 2 d S T P . .
C1A C 0.1804(3) 0.500000 0.4939(4) 0.034(2) Uani 1 2 d S T P . .
H1A H 0.141743 0.500000 0.465864 0.041 Uiso 1 2 calc RS T P . .
C2A C 0.2098(4) 0.500000 0.5668(4) 0.040(2) Uani 1 2 d S T P . .
H2A H 0.191104 0.500000 0.586841 0.048 Uiso 1 2 calc RS T P . .
C3A C 0.2672(4) 0.500000 0.6087(4) 0.035(2) Uani 1 2 d S T P . .
H3A H 0.287989 0.500000 0.657368 0.042 Uiso 1 2 calc RS T P . .
C4A C 0.2927(4) 0.500000 0.5760(4) 0.038(2) Uani 1 2 d S T P . .
H4A H 0.331288 0.500000 0.602513 0.045 Uiso 1 2 calc RS T P . .
C5A C 0.2606(4) 0.500000 0.5044(4) 0.030(2) Uani 1 2 d S T P . .
C6A C 0.2841(3) 0.500000 0.4641(4) 0.026(2) Uani 1 2 d S T P . .
C7A C 0.3292(4) 0.500000 0.4233(5) 0.033(2) Uani 1 2 d S T P . .
C8A C 0.3782(4) 0.500000 0.4202(5) 0.044(2) Uani 1 2 d S T P . .
C9A C 0.3583(4) 0.500000 0.3443(5) 0.082(4) Uani 1 2 d S T P . .
H9AA H 0.340639 0.378170 0.322473 0.123 Uiso 0.5 1 d R . . A -1
H9AB H 0.389869 0.517310 0.343913 0.123 Uiso 0.5 1 d R . . A -1
H9AC H 0.332479 0.604510 0.318923 0.123 Uiso 0.5 1 d R . . A -1
C10A C 0.4121(3) 0.3166(10) 0.4554(4) 0.101(3) Uani 1 1 d . . . . .
H10A H 0.426796 0.317344 0.504044 0.151 Uiso 1 1 d R . . . .
H10B H 0.442116 0.313294 0.451604 0.151 Uiso 1 1 d R . . . .
H10C H 0.389036 0.203804 0.432944 0.151 Uiso 1 1 d R . . . .
C11A C 0.1543(4) 0.500000 0.2218(4) 0.042(2) Uani 1 2 d S T P . .
H11A H 0.192949 0.500000 0.249960 0.051 Uiso 1 2 calc RS T P . .
C12A C 0.1253(4) 0.500000 0.1502(4) 0.046(3) Uani 1 2 d S T P . .
H12A H 0.144383 0.500000 0.130657 0.056 Uiso 1 2 calc RS T P . .
C13A C 0.0686(4) 0.500000 0.1076(4) 0.047(3) Uani 1 2 d S T P . .
H13A H 0.048450 0.500000 0.058967 0.057 Uiso 1 2 calc RS T P . .
C14A C 0.0426(4) 0.500000 0.1384(4) 0.047(3) Uani 1 2 d S T P . .
H14A H 0.003980 0.500000 0.110616 0.056 Uiso 1 2 calc RS T P . .
C15A C 0.0728(4) 0.500000 0.2110(4) 0.033(2) Uani 1 2 d S T P . .
C16A C 0.0494(3) 0.500000 0.2508(4) 0.031(2) Uani 1 2 d S T P . .
C17A C 0.0053(3) 0.500000 0.2925(4) 0.037(2) Uani 1 2 d S T P . .
C18A C -0.0422(4) 0.500000 0.2986(5) 0.044(2) Uani 1 2 d S T P . .
C19A C -0.0769(3) 0.6831(10) 0.2640(4) 0.092(3) Uani 1 1 d . . . . .
H19A H -0.054926 0.796364 0.288708 0.138 Uiso 1 1 d R . . . .
H19B H -0.108346 0.679154 0.265008 0.138 Uiso 1 1 d R . . . .
H19C H -0.089586 0.688714 0.216118 0.138 Uiso 1 1 d R . . . .
C20A C -0.0191(4) 0.500000 0.3762(5) 0.089(4) Uani 1 2 d S T P . .
H20A H 0.012341 0.414370 0.402185 0.133 Uiso 0.5 1 d R . . B -1
H20B H -0.047489 0.456020 0.380155 0.133 Uiso 0.5 1 d R . . B -1
H20C H -0.007969 0.629610 0.394705 0.133 Uiso 0.5 1 d R . . B -1
Pd1B Pd 0.000000 0.000000 0.000000 0.0386(3) Uani 1 4 d S T P . .
N1B N 0.0813(3) 0.000000 0.0771(3) 0.0380(19) Uani 1 2 d S T P . .
N2B N 0.1292(3) 0.000000 0.0814(4) 0.051(2) Uani 1 2 d S T P . .
N3B N 0.1515(3) 0.000000 0.1912(4) 0.047(2) Uani 1 2 d S T P . .
N4B N 0.0010(3) 0.000000 0.0861(3) 0.0368(18) Uani 1 2 d S T P . .
C1B C -0.0453(4) 0.000000 0.0850(5) 0.048(3) Uani 1 2 d S T P . .
H1B H -0.080429 0.000000 0.042127 0.058 Uiso 1 2 calc RS T P . .
C2B C -0.0406(4) 0.000000 0.1461(5) 0.058(3) Uani 1 2 d S T P . .
H2B H -0.072478 0.000000 0.144154 0.070 Uiso 1 2 calc RS T P . .
C3B C 0.0109(4) 0.000000 0.2103(5) 0.050(3) Uani 1 2 d S T P . .
H3B H 0.014305 0.000000 0.251820 0.061 Uiso 1 2 calc RS T P . .
C4B C 0.0586(4) 0.000000 0.2114(4) 0.044(2) Uani 1 2 d S T P . .
H4B H 0.094143 0.000000 0.253709 0.053 Uiso 1 2 calc RS T P . .
C5B C 0.0510(4) 0.000000 0.1495(4) 0.032(2) Uani 1 2 d S T P . .
C6B C 0.0957(4) 0.000000 0.1424(4) 0.037(2) Uani 1 2 d S T P . .
C7B C 0.1699(4) 0.000000 0.1508(4) 0.042(2) Uani 1 2 d S T P . .
C8B C 0.2315(4) 0.000000 0.1802(4) 0.049(3) Uani 1 2 d S T P . .
C9B C 0.2428(3) 0.1842(12) 0.1562(4) 0.133(4) Uani 1 1 d . . . . .
H9BA H 0.217736 0.192706 0.105933 0.200 Uiso 1 1 d R . . . .
H9BB H 0.280376 0.182086 0.171213 0.200 Uiso 1 1 d R . . . .
H9BC H 0.237566 0.294896 0.176363 0.200 Uiso 1 1 d R . . . .
C10B C 0.2683(4) 0.000000 0.2603(4) 0.082(4) Uani 1 2 d S T P . .
H10D H 0.305407 -0.036910 0.278152 0.123 Uiso 0.5 1 d R . . C -1
H10E H 0.253867 -0.091130 0.276312 0.123 Uiso 0.5 1 d R . . C -1
H10F H 0.268717 0.128050 0.276832 0.123 Uiso 0.5 1 d R . . C -1
Cl1 Cl -0.11776(14) 0.500000 0.00829(16) 0.1265(15) Uani 1 2 d S T P . .
Cl2 Cl -0.17304(11) 0.2921(4) 0.05413(14) 0.1313(11) Uani 1 1 d . . . . .
C1 C -0.1346(5) 0.500000 0.0654(5) 0.079(4) Uani 1 2 d S T P . .
H1 H -0.100148 0.500000 0.113394 0.095 Uiso 1 2 calc RS T P . .
O1W O 0.0669(3) 0.000000 0.3728(4) 0.150(4) Uani 1 2 d S T P . .
H1WA H 0.063810 -0.122690 0.366789 0.225 Uiso 0.5 1 d R . . . .
H1WB H 0.099490 0.000000 0.410899 0.225 Uiso 1 2 d RS T P . .


_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
Pd1A N1A 2.022(7) . ?
Pd1A N4A 2.026(6) . ?
Pd1A N5A 2.003(6) . ?
Pd1A N8A 2.029(6) . ?
N1A N2A 1.359(8) . ?
N1A C6A 1.335(9) . ?
N2A C7A 1.348(10) . ?
N3A C6A 1.336(10) . ?
N3A C7A 1.356(10) . ?
N4A C1A 1.346(9) . ?
N4A C5A 1.324(10) . ?
N5A N6A 1.371(9) . ?
N5A C16A 1.338(9) . ?
N6A C17A 1.337(10) . ?
N7A C16A 1.334(10) . ?
N7A C17A 1.356(10) . ?
N8A C11A 1.339(10) . ?
N8A C15A 1.348(10) . ?
C1A H1A 0.9300 . ?
C1A C2A 1.398(10) . ?
C2A H2A 0.9300 . ?
C2A C3A 1.380(11) . ?
C3A H3A 0.9300 . ?
C3A C4A 1.380(11) . ?
C4A H4A 0.9300 . ?
C4A C5A 1.366(10) . ?
C5A C6A 1.491(11) . ?
C7A C8A 1.517(11) . ?
C8A C9A 1.525(11) . ?
C8A C10A 1.517(7) . ?
C8A C10A 1.517(7) 6_565 ?
C9A H9AA 0.9600 . ?
C9A H9AB 0.9600 . ?
C9A H9AC 0.9599 . ?
C10A H10A 0.9600 . ?
C10A H10B 0.9596 . ?
C10A H10C 0.9600 . ?
C11A H11A 0.9300 . ?
C11A C12A 1.372(10) . ?
C12A H12A 0.9300 . ?
C12A C13A 1.365(11) . ?
C13A H13A 0.9300 . ?
C13A C14A 1.355(11) . ?
C14A H14A 0.9300 . ?
C14A C15A 1.388(10) . ?
C15A C16A 1.479(11) . ?
C17A C18A 1.518(11) . ?
C18A C19A 1.522(8) 6_565 ?
C18A C19A 1.522(8) . ?
C18A C20A 1.535(11) . ?
C19A H19A 0.9599 . ?
C19A H19B 0.9605 . ?
C19A H19C 0.9601 . ?
C20A H20A 0.9602 . ?
C20A H20B 0.9601 . ?
C20A H20C 0.9599 . ?
Pd1B N1B 1.990(7) 5 ?
Pd1B N1B 1.990(7) . ?
Pd1B N4B 2.031(7) . ?
Pd1B N4B 2.031(7) 5 ?
N1B N2B 1.381(9) . ?
N1B C6B 1.339(10) . ?
N2B C7B 1.343(10) . ?
N3B C6B 1.350(10) . ?
N3B C7B 1.365(11) . ?
N4B C1B 1.376(10) . ?
N4B C5B 1.349(10) . ?
C1B H1B 0.9300 . ?
C1B C2B 1.374(11) . ?
C2B H2B 0.9300 . ?
C2B C3B 1.376(11) . ?
C3B H3B 0.9300 . ?
C3B C4B 1.417(12) . ?
C4B H4B 0.9300 . ?
C4B C5B 1.348(11) . ?
C5B C6B 1.452(12) . ?
C7B C8B 1.539(11) . ?
C8B C9B 1.506(8) 6 ?
C8B C9B 1.506(8) . ?
C8B C10B 1.527(11) . ?
C9B H9BA 0.9599 . ?
C9B H9BB 0.9602 . ?
C9B H9BC 0.9600 . ?
C10B H10D 0.9599 . ?
C10B H10E 0.9603 . ?
C10B H10F 0.9602 . ?
Cl1 C1 1.709(10) . ?
Cl2 C1 1.753(7) . ?
C1 H1 0.9800 . ?
O1W H1WA 0.8502 . ?
O1W H1WA 0.8501 6 ?
O1W H1WB 0.8475 . ?

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
N1A Pd1A N4A 79.3(3) . . ?
N1A Pd1A N8A 100.4(3) . . ?
N4A Pd1A N8A 179.7(3) . . ?
N5A Pd1A N1A 179.7(3) . . ?
N5A Pd1A N4A 101.0(3) . . ?
N5A Pd1A N8A 79.3(3) . . ?
N2A N1A Pd1A 136.5(5) . . ?
C6A N1A Pd1A 114.6(6) . . ?
C6A N1A N2A 108.9(7) . . ?
C7A N2A N1A 102.5(7) . . ?
C6A N3A C7A 101.5(7) . . ?
C1A N4A Pd1A 125.9(5) . . ?
C5A N4A Pd1A 117.6(6) . . ?
C5A N4A C1A 116.5(7) . . ?
N6A N5A Pd1A 136.4(5) . . ?
C16A N5A Pd1A 116.4(6) . . ?
C16A N5A N6A 107.2(6) . . ?
C17A N6A N5A 103.4(7) . . ?
C16A N7A C17A 101.1(7) . . ?
C11A N8A Pd1A 125.7(6) . . ?
C11A N8A C15A 118.1(7) . . ?
C15A N8A Pd1A 116.2(5) . . ?
N4A C1A H1A 118.6 . . ?
N4A C1A C2A 122.7(8) . . ?
C2A C1A H1A 118.6 . . ?
C1A C2A H2A 120.5 . . ?
C3A C2A C1A 118.9(8) . . ?
C3A C2A H2A 120.5 . . ?
C2A C3A H3A 121.0 . . ?
C4A C3A C2A 118.0(8) . . ?
C4A C3A H3A 121.0 . . ?
C3A C4A H4A 120.4 . . ?
C5A C4A C3A 119.2(8) . . ?
C5A C4A H4A 120.4 . . ?
N4A C5A C4A 124.7(8) . . ?
N4A C5A C6A 111.9(7) . . ?
C4A C5A C6A 123.4(8) . . ?
N1A C6A N3A 112.1(7) . . ?
N1A C6A C5A 116.6(8) . . ?
N3A C6A C5A 131.3(8) . . ?
N2A C7A N3A 114.9(8) . . ?
N2A C7A C8A 123.6(8) . . ?
N3A C7A C8A 121.5(8) . . ?
C7A C8A C9A 110.8(8) . . ?
C10A C8A C7A 108.9(5) . . ?
C10A C8A C7A 108.9(5) 6_565 . ?
C10A C8A C9A 108.1(5) 6_565 . ?
C10A C8A C9A 108.1(5) . . ?
C10A C8A C10A 112.2(9) 6_565 . ?
C8A C9A H9AA 109.7 . . ?
C8A C9A H9AB 108.9 . . ?
C8A C9A H9AC 109.8 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C8A C10A H10A 109.4 . . ?
C8A C10A H10B 109.1 . . ?
C8A C10A H10C 109.9 . . ?
H10A C10A H10B 109.5 . . ?
H10A C10A H10C 109.4 . . ?
H10B C10A H10C 109.5 . . ?
N8A C11A H11A 118.9 . . ?
N8A C11A C12A 122.1(8) . . ?
C12A C11A H11A 118.9 . . ?
C11A C12A H12A 119.8 . . ?
C13A C12A C11A 120.3(9) . . ?
C13A C12A H12A 119.8 . . ?
C12A C13A H13A 121.1 . . ?
C14A C13A C12A 117.7(8) . . ?
C14A C13A H13A 121.1 . . ?
C13A C14A H14A 119.5 . . ?
C13A C14A C15A 121.0(8) . . ?
C15A C14A H14A 119.5 . . ?
N8A C15A C14A 120.8(8) . . ?
N8A C15A C16A 113.1(7) . . ?
C14A C15A C16A 126.1(8) . . ?
N5A C16A C15A 115.0(7) . . ?
N7A C16A N5A 113.2(7) . . ?
N7A C16A C15A 131.8(8) . . ?
N6A C17A N7A 115.0(8) . . ?
N6A C17A C18A 122.2(8) . . ?
N7A C17A C18A 122.8(8) . . ?
C17A C18A C19A 109.1(5) . . ?
C17A C18A C19A 109.1(5) . 6_565 ?
C17A C18A C20A 109.9(8) . . ?
C19A C18A C19A 111.4(9) 6_565 . ?
C19A C18A C20A 108.6(5) 6_565 . ?
C19A C18A C20A 108.6(5) . . ?
C18A C19A H19A 109.9 . . ?
C18A C19A H19B 109.2 . . ?
C18A C19A H19C 109.3 . . ?
H19A C19A H19B 109.4 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C18A C20A H20A 109.6 . . ?
C18A C20A H20B 109.3 . . ?
C18A C20A H20C 109.5 . . ?
H20A C20A H20B 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
N1B Pd1B N1B 180.0 . 5 ?
N1B Pd1B N4B 78.6(3) . . ?
N1B Pd1B N4B 101.4(3) 5 . ?
N1B Pd1B N4B 101.4(3) . 5 ?
N1B Pd1B N4B 78.6(3) 5 5 ?
N4B Pd1B N4B 180.0 . 5 ?
N2B N1B Pd1B 135.9(6) . . ?
C6B N1B Pd1B 115.8(6) . . ?
C6B N1B N2B 108.3(7) . . ?
C7B N2B N1B 103.4(7) . . ?
C6B N3B C7B 102.2(7) . . ?
C1B N4B Pd1B 125.2(6) . . ?
C5B N4B Pd1B 117.5(6) . . ?
C5B N4B C1B 117.3(8) . . ?
N4B C1B H1B 119.4 . . ?
C2B C1B N4B 121.2(9) . . ?
C2B C1B H1B 119.4 . . ?
C1B C2B H2B 119.7 . . ?
C1B C2B C3B 120.5(10) . . ?
C3B C2B H2B 119.7 . . ?
C2B C3B H3B 120.9 . . ?
C2B C3B C4B 118.3(9) . . ?
C4B C3B H3B 120.9 . . ?
C3B C4B H4B 120.9 . . ?
C5B C4B C3B 118.2(9) . . ?
C5B C4B H4B 120.9 . . ?
N4B C5B C4B 124.5(9) . . ?
N4B C5B C6B 111.0(8) . . ?
C4B C5B C6B 124.4(8) . . ?
N1B C6B N3B 111.8(8) . . ?
N1B C6B C5B 117.1(8) . . ?
N3B C6B C5B 131.1(8) . . ?
N2B C7B N3B 114.3(8) . . ?
N2B C7B C8B 121.3(9) . . ?
N3B C7B C8B 124.4(8) . . ?
C9B C8B C7B 108.1(5) 6 . ?
C9B C8B C7B 108.1(5) . . ?
C9B C8B C9B 114.2(10) . 6 ?
C9B C8B C10B 108.3(5) . . ?
C9B C8B C10B 108.3(5) 6 . ?
C10B C8B C7B 109.9(8) . . ?
C8B C9B H9BA 109.7 . . ?
C8B C9B H9BB 109.1 . . ?
C8B C9B H9BC 109.6 . . ?
H9BA C9B H9BB 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?
C8B C10B H10D 109.4 . . ?
C8B C10B H10E 109.5 . . ?
C8B C10B H10F 109.5 . . ?
H10D C10B H10E 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.4 . . ?
Cl1 C1 Cl2 111.1(4) . 6_565 ?
Cl1 C1 Cl2 111.1(4) . . ?
Cl1 C1 H1 108.5 . . ?
Cl2 C1 Cl2 109.0(7) . 6_565 ?
Cl2 C1 H1 108.5 . . ?
Cl2 C1 H1 108.5 6_565 . ?
H1WA O1W H1WA 164.5 . 6 ?
H1WA O1W H1WB 96.8 . . ?
H1WB O1W H1WA 96.8 . 6 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.102
_oxdiff_exptl_absorpt_empirical_full_min 0.922
####################################################################### 
# 
# 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_shi_4015_rola_twin1_hklf4
_database_code_depnum_ccdc_archive 'CCDC 1910553'
loop_
_audit_author_name
_audit_author_address
'Sergiu Shova'
;Institute of Macromolecular Chemistry of the Romanian Academy
Romania
;
_audit_update_record             
;
2019-04-16 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;
_audit_creation_date             2019-04-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H22 N8 Pd'
_chemical_formula_sum            'C20 H22 N8 Pd'
_chemical_formula_weight         480.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H20N6Pd1
_chemical_oxdiff_usercomment     s-Pd(Liso)2
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.4346(9)
_cell_length_b                   10.181(4)
_cell_length_c                   21.341(7)
_cell_angle_alpha                90
_cell_angle_beta                 92.15(2)
_cell_angle_gamma                90
_cell_volume                     962.9(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    289
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.8540
_cell_measurement_theta_min      4.5960
_shelx_estimated_absorpt_T_max   0.908
_shelx_estimated_absorpt_T_min   0.756
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.1108
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            2623
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.499
_diffrn_reflns_theta_min         2.217
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  21.00   1.00   30.00    --  -15.60 -99.00   0.00   40
  2  ω    -82.00 -25.00   1.00   30.00    --  -15.60 -77.00 120.00   57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0117488000
_diffrn_orient_matrix_UB_12      -0.0574365000
_diffrn_orient_matrix_UB_13      -0.0186862000
_diffrn_orient_matrix_UB_21      -0.1504546000
_diffrn_orient_matrix_UB_22      -0.0091610000
_diffrn_orient_matrix_UB_23      0.0093101000
_diffrn_orient_matrix_UB_31      -0.0533290000
_diffrn_orient_matrix_UB_32      0.0383499000
_diffrn_orient_matrix_UB_33      -0.0258907000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1804
_reflns_number_total             2623
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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    'SIR2008 (Burla et al.,  2007)'
_refine_diff_density_max         2.269
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2623
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0702
_refine_ls_restrained_S_all      1.011
_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)+(0.0838P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1615
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.655(2)
 0.345(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C8(H8)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.500000 1.000000 0.500000 0.0333(3) Uani 1 2 d S T P . .
N1 N 0.4650(16) 0.8277(6) 0.4533(3) 0.0338(16) Uani 1 1 d . . . . .
N2 N 0.7851(15) 0.8906(7) 0.5495(3) 0.0348(17) Uani 1 1 d . . . . .
N3 N 0.9645(16) 0.9062(7) 0.6019(3) 0.0362(15) Uani 1 1 d . . . . .
N4 N 1.0035(16) 0.6976(6) 0.5678(3) 0.0352(15) Uani 1 1 d . . . . .
C1 C 0.282(2) 0.8062(9) 0.4036(4) 0.039(2) Uani 1 1 d . . . . .
H1 H 0.163337 0.874698 0.387627 0.046 Uiso 1 1 calc R . . . .
C2 C 0.264(2) 0.6861(9) 0.3755(4) 0.048(2) Uani 1 1 d . . . . .
H2 H 0.132741 0.672817 0.341115 0.057 Uiso 1 1 calc R . . . .
C3 C 0.439(2) 0.5856(9) 0.3980(4) 0.050(2) Uani 1 1 d . . . . .
H3 H 0.431681 0.503881 0.378588 0.059 Uiso 1 1 calc R . . . .
C4 C 0.627(2) 0.6064(8) 0.4502(4) 0.042(2) Uani 1 1 d . . . . .
H4 H 0.746844 0.538848 0.466848 0.051 Uiso 1 1 calc R . . . .
C5 C 0.6344(19) 0.7296(8) 0.4771(4) 0.0318(18) Uani 1 1 d . . . . .
C6 C 0.816(2) 0.7656(9) 0.5314(4) 0.038(2) Uani 1 1 d . . . . .
C7 C 1.0877(19) 0.7899(8) 0.6106(4) 0.0356(19) Uani 1 1 d . . . . .
C8 C 1.298(2) 0.7610(9) 0.6650(4) 0.040(2) Uani 1 1 d . . . . .
H8 H 1.486366 0.726629 0.648857 0.048 Uiso 1 1 calc R . . . .
C9 C 1.372(2) 0.8813(9) 0.7030(4) 0.050(2) Uani 1 1 d . . . . .
H9A H 1.190249 0.915446 0.720096 0.075 Uiso 1 1 calc GR . . . .
H9B H 1.458804 0.946531 0.676731 0.075 Uiso 1 1 calc GR . . . .
H9C H 1.512517 0.859094 0.736575 0.075 Uiso 1 1 calc GR . . . .
C10 C 1.161(2) 0.6553(9) 0.7057(4) 0.052(3) Uani 1 1 d . . . . .
H10A H 1.108653 0.580185 0.680317 0.078 Uiso 1 1 calc GR . . . .
H10B H 0.982345 0.689062 0.724168 0.078 Uiso 1 1 calc GR . . . .
H10C H 1.304155 0.629921 0.738275 0.078 Uiso 1 1 calc GR . . . .


_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 N1 2.021(6) 3_676 ?
Pd1 N1 2.021(6) . ?
Pd1 N2 1.963(6) 3_676 ?
Pd1 N2 1.963(6) . ?
N1 C1 1.329(10) . ?
N1 C5 1.338(10) . ?
N2 N3 1.356(9) . ?
N2 C6 1.339(11) . ?
N3 C7 1.314(10) . ?
N4 C6 1.315(10) . ?
N4 C7 1.352(10) . ?
C1 C2 1.363(11) . ?
C2 C3 1.360(12) . ?
C3 C4 1.384(11) . ?
C4 C5 1.378(11) . ?
C5 C6 1.434(12) . ?
C7 C8 1.492(11) . ?
C8 C9 1.498(12) . ?
C8 C10 1.525(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 N1 180.0 3_676 . ?
N2 Pd1 N1 101.0(3) . 3_676 ?
N2 Pd1 N1 101.0(3) 3_676 . ?
N2 Pd1 N1 79.0(3) . . ?
N2 Pd1 N1 79.0(3) 3_676 3_676 ?
N2 Pd1 N2 180.0(3) 3_676 . ?
C1 N1 Pd1 124.7(6) . . ?
C1 N1 C5 119.8(7) . . ?
C5 N1 Pd1 115.4(5) . . ?
N3 N2 Pd1 136.3(6) . . ?
C6 N2 Pd1 117.0(6) . . ?
C6 N2 N3 106.6(7) . . ?
C7 N3 N2 103.8(6) . . ?
C6 N4 C7 100.7(7) . . ?
N1 C1 C2 121.5(8) . . ?
C3 C2 C1 119.8(9) . . ?
C2 C3 C4 119.2(8) . . ?
C5 C4 C3 118.5(8) . . ?
N1 C5 C4 121.2(8) . . ?
N1 C5 C6 113.9(7) . . ?
C4 C5 C6 124.8(8) . . ?
N2 C6 C5 114.6(8) . . ?
N4 C6 N2 113.5(8) . . ?
N4 C6 C5 131.9(8) . . ?
N3 C7 N4 115.3(7) . . ?
N3 C7 C8 122.1(7) . . ?
N4 C7 C8 122.5(8) . . ?
C7 C8 C9 112.2(7) . . ?
C7 C8 C10 109.3(7) . . ?
C9 C8 C10 110.7(7) . . ?

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
C1 H1 N3 0.93 2.31 3.126(10) 145.5 3_676 yes

_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 1.509
_oxdiff_exptl_absorpt_empirical_full_min 0.650
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.655(2) 79 1803 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.345(2) 84 1803 nmt 1.0007 -0.0009 -0.0001 0.0020 -1.0019 -0.0004 -0.3901
-0.0028 -0.9994

_twin_special_details            
;
Component 2 rotated by -179.9079° 
 around [0.98 0.00 -0.19] (reciprocal) or [1.00 0.00 -0.00] (direct)
;
