# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_200328RaselPdBrSO4_2-93K
_database_code_depnum_ccdc_archive 'CCDC 1987451'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Iguchi'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-04-23 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 Br N4 O4 Pd 2+, S O4 2-, 3(O H2)'
_chemical_formula_sum            'C8 H30 Br N4 O11 Pd S'
_chemical_formula_weight         576.73

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.4228(3)
_cell_length_b                   10.2975(3)
_cell_length_c                   21.9679(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1905.36(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    5713
_cell_measurement_theta_min      2.5700
_cell_measurement_theta_max      29.5710

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_F_000             1164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    3.241
_shelx_estimated_absorpt_T_min   0.642
_shelx_estimated_absorpt_T_max   0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91231
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.896
_oxdiff_exptl_absorpt_empirical_full_max 1.138
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            12855
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.590
_diffrn_reflns_theta_max         29.666
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4590
_reflns_number_gt                4212
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.661
_reflns_Friedel_fraction_max     0.784
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_structure_solution    Sir2019
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0150P)²+2.7450P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1572 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(5)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         4590
_refine_ls_number_parameters     263
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0255
_refine_ls_wR_factor_ref         0.0519
_refine_ls_wR_factor_gt          0.0508
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
O1 O -0.0528(4) 0.5724(3) 0.54182(13) 0.0125(7) Uani 1 1 d . . . . .
H1B H -0.147808 0.548334 0.539219 0.019 Uiso 1 1 calc R U . . .
C1 C -0.0473(5) 0.7085(4) 0.55377(18) 0.0107(9) Uani 1 1 d . . . . .
H1C H -0.154743 0.745897 0.548529 0.013 Uiso 1 1 calc R U . . .
H1D H 0.024286 0.750877 0.524058 0.013 Uiso 1 1 calc R U . . .
C2 C 0.0115(5) 0.7363(4) 0.61830(14) 0.0071(7) Uani 1 1 d . . . . .
H2C H 0.023530 0.832400 0.622752 0.009 Uiso 1 1 calc R U . . .
C3 C 0.1702(5) 0.6736(4) 0.63381(17) 0.0070(8) Uani 1 1 d . . . . .
H3C H 0.159700 0.577427 0.629166 0.008 Uiso 1 1 calc R U . . .
C4 C 0.3020(5) 0.7210(5) 0.59162(18) 0.0137(9) Uani 1 1 d . . . . .
H4D H 0.278375 0.693098 0.549463 0.016 Uiso 1 1 calc R U . . .
H4C H 0.304797 0.817130 0.592203 0.016 Uiso 1 1 calc R U . . .
O2 O 0.4528(4) 0.6724(3) 0.60890(13) 0.0148(6) Uani 1 1 d . . . . .
H2B H 0.493927 0.722446 0.634677 0.022 Uiso 1 1 calc R U . . .
N1 N -0.1051(4) 0.6912(3) 0.66461(14) 0.0057(7) Uani 1 1 d . . . . .
H1 H -0.135434 0.608196 0.656412 0.007 Uiso 1 1 calc R U . . .
H1A H -0.192871 0.742684 0.663907 0.007 Uiso 1 1 calc R U . . .
N2 N 0.2080(4) 0.7033(3) 0.69881(14) 0.0062(7) Uani 1 1 d . . . . .
H2 H 0.254275 0.782979 0.701668 0.007 Uiso 1 1 calc R U . . .
H2A H 0.276984 0.643242 0.713753 0.007 Uiso 1 1 calc R U . . .
Pd1 Pd 0.00058(4) 0.70020(3) 0.74812(2) 0.00422(7) Uani 1 1 d . . . . .
Br1 Br -0.01483(4) 0.95095(4) 0.74373(2) 0.00695(8) Uani 1 1 d . . . . .
O3 O -0.3290(4) 0.8774(3) 0.89504(14) 0.0166(7) Uani 1 1 d . . . . .
H3B H -0.357216 0.899661 0.859878 0.025 Uiso 1 1 calc R U . . .
C5 C -0.3171(5) 0.7403(4) 0.89797(18) 0.0115(9) Uani 1 1 d . . . . .
H5 H -0.416049 0.701614 0.881738 0.014 Uiso 1 1 calc R U . . .
H5A H -0.307106 0.713684 0.941105 0.014 Uiso 1 1 calc R U . . .
C6 C -0.1763(5) 0.6867(4) 0.86237(17) 0.0078(8) Uani 1 1 d . . . . .
H6 H -0.164330 0.592647 0.872752 0.009 Uiso 1 1 calc R U . . .
C7 C -0.0201(5) 0.7552(4) 0.87718(15) 0.0085(8) Uani 1 1 d . . . . .
H7 H -0.037062 0.850947 0.873465 0.010 Uiso 1 1 calc R U . . .
C8 C 0.0367(5) 0.7260(4) 0.94155(17) 0.0124(9) Uani 1 1 d . . . . .
H8 H 0.142158 0.766099 0.948064 0.015 Uiso 1 1 calc R U . . .
H8A H -0.038219 0.764348 0.971279 0.015 Uiso 1 1 calc R U . . .
O4 O 0.0471(4) 0.5901(3) 0.95119(14) 0.0175(7) Uani 1 1 d . . . . .
H4B H 0.142905 0.568426 0.954276 0.026 Uiso 1 1 calc R U . . .
N3 N -0.2078(4) 0.6972(3) 0.79564(14) 0.0062(7) Uani 1 1 d . . . . .
H3 H -0.263412 0.771125 0.787928 0.007 Uiso 1 1 calc R U . . .
H3A H -0.267523 0.628428 0.783285 0.007 Uiso 1 1 calc R U . . .
N4 N 0.1019(4) 0.7154(3) 0.83175(14) 0.0063(7) Uani 1 1 d . . . . .
H4 H 0.144635 0.637684 0.842707 0.008 Uiso 1 1 calc R U . . .
H4A H 0.181243 0.775322 0.830690 0.008 Uiso 1 1 calc R U . . .
O5 O 0.4142(4) 0.4609(5) 0.72521(13) 0.0333(9) Uani 1 1 d . . . . .
S1 S 0.45426(11) 0.44745(11) 0.78991(4) 0.00790(19) Uani 1 1 d . . . . .
O6 O 0.3799(4) 0.5478(4) 0.82688(17) 0.0292(8) Uani 1 1 d . . . . .
O7 O 0.3965(4) 0.3184(4) 0.81006(18) 0.0297(9) Uani 1 1 d . . . . .
O8 O 0.6284(3) 0.4518(3) 0.79776(13) 0.0140(6) Uani 1 1 d . . . . .
O9 O 0.7035(3) 0.4404(3) 0.65552(13) 0.0124(6) Uani 1 1 d D . . . .
O10 O 0.6355(3) 0.5263(3) 0.53552(13) 0.0142(7) Uani 1 1 d D . . . .
O11 O 0.6600(5) 0.0063(6) 0.54876(17) 0.0513(15) Uani 1 1 d D . . . .
H9A H 0.665(5) 0.450(5) 0.6225(13) 0.019(13) Uiso 1 1 d D . . . .
H10A H 0.572(6) 0.577(5) 0.552(3) 0.05(2) Uiso 1 1 d D . . . .
H9B H 0.635(5) 0.450(6) 0.6824(17) 0.039(18) Uiso 1 1 d D . . . .
H11B H 0.592(6) -0.013(7) 0.524(2) 0.07(2) Uiso 1 1 d D . . . .
H10B H 0.582(7) 0.491(6) 0.509(2) 0.07(3) Uiso 1 1 d D . . . .
H11A H 0.622(8) 0.026(8) 0.5817(18) 0.08(3) Uiso 1 1 d D . . . .


_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
O1 C1 1.426(5) . ?
C1 C2 1.529(5) . ?
C2 N1 1.488(5) . ?
C2 C3 1.523(6) . ?
C3 N2 1.495(5) . ?
C3 C4 1.527(6) . ?
C4 O2 1.417(5) . ?
N1 Pd1 2.041(3) . ?
N2 Pd1 2.056(3) . ?
Pd1 N4 2.032(3) . ?
Pd1 N3 2.042(3) . ?
Pd1 Br1 2.5757(5) 4_546 ?
Pd1 Br1 2.5872(5) . ?
O3 C5 1.417(6) . ?
C5 C6 1.524(5) . ?
C6 N3 1.494(5) . ?
C6 C7 1.527(6) . ?
C7 N4 1.490(5) . ?
C7 C8 1.523(5) . ?
C8 O4 1.419(5) . ?
O5 S1 1.467(3) . ?
S1 O6 1.456(3) . ?
S1 O8 1.478(3) . ?
S1 O7 1.483(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 111.4(3) . . ?
N1 C2 C3 107.1(3) . . ?
N1 C2 C1 111.2(3) . . ?
C3 C2 C1 114.4(3) . . ?
N2 C3 C2 108.3(3) . . ?
N2 C3 C4 111.1(3) . . ?
C2 C3 C4 111.6(3) . . ?
O2 C4 C3 112.1(3) . . ?
C2 N1 Pd1 108.2(2) . . ?
C3 N2 Pd1 108.6(2) . . ?
N4 Pd1 N1 177.94(15) . . ?
N4 Pd1 N3 84.25(13) . . ?
N1 Pd1 N3 94.82(13) . . ?
N4 Pd1 N2 96.80(13) . . ?
N1 Pd1 N2 84.13(13) . . ?
N3 Pd1 N2 178.94(15) . . ?
N4 Pd1 Br1 89.68(10) . 4_546 ?
N1 Pd1 Br1 92.15(10) . 4_546 ?
N3 Pd1 Br1 89.39(10) . 4_546 ?
N2 Pd1 Br1 90.73(10) . 4_546 ?
N4 Pd1 Br1 88.74(10) . . ?
N1 Pd1 Br1 89.42(10) . . ?
N3 Pd1 Br1 89.49(10) . . ?
N2 Pd1 Br1 90.42(10) . . ?
Br1 Pd1 Br1 178.143(11) 4_546 . ?
Pd1 Br1 Pd1 171.731(15) 4_556 . ?
O3 C5 C6 113.1(3) . . ?
N3 C6 C5 109.8(3) . . ?
N3 C6 C7 109.2(3) . . ?
C5 C6 C7 113.2(3) . . ?
N4 C7 C8 110.6(3) . . ?
N4 C7 C6 108.9(3) . . ?
C8 C7 C6 112.2(3) . . ?
O4 C8 C7 110.6(3) . . ?
C6 N3 Pd1 110.5(3) . . ?
C7 N4 Pd1 109.7(2) . . ?
O6 S1 O5 112.0(2) . . ?
O6 S1 O8 109.9(2) . . ?
O5 S1 O8 109.77(18) . . ?
O6 S1 O7 109.2(2) . . ?
O5 S1 O7 107.4(2) . . ?
O8 S1 O7 108.5(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 -67.4(4) . . . . ?
O1 C1 C2 C3 54.1(5) . . . . ?
N1 C2 C3 N2 -53.4(4) . . . . ?
C1 C2 C3 N2 -177.1(3) . . . . ?
N1 C2 C3 C4 -175.9(3) . . . . ?
C1 C2 C3 C4 60.3(5) . . . . ?
N2 C3 C4 O2 53.8(5) . . . . ?
C2 C3 C4 O2 174.8(3) . . . . ?
C3 C2 N1 Pd1 43.7(3) . . . . ?
C1 C2 N1 Pd1 169.3(3) . . . . ?
C2 C3 N2 Pd1 36.7(4) . . . . ?
C4 C3 N2 Pd1 159.5(3) . . . . ?
O3 C5 C6 N3 -72.4(4) . . . . ?
O3 C5 C6 C7 49.9(5) . . . . ?
N3 C6 C7 N4 -45.9(4) . . . . ?
C5 C6 C7 N4 -168.6(3) . . . . ?
N3 C6 C7 C8 -168.6(3) . . . . ?
C5 C6 C7 C8 68.7(5) . . . . ?
N4 C7 C8 O4 -67.3(4) . . . . ?
C6 C7 C8 O4 54.5(5) . . . . ?
C5 C6 N3 Pd1 156.3(3) . . . . ?
C7 C6 N3 Pd1 31.6(4) . . . . ?
C8 C7 N4 Pd1 162.0(3) . . . . ?
C6 C7 N4 Pd1 38.3(4) . . . . ?

_refine_diff_density_max         1.356
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.095

####################################################################### 
# 
# 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_200328RaselPdBrSO4_2_250K
_database_code_depnum_ccdc_archive 'CCDC 1998642'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Iguchi'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-04-23 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 Br N4 O4 Pd 2+, S O4 2-, 3(H2 O)'
_chemical_formula_sum            'C8 H30 Br N4 O11 Pd S'
_chemical_formula_weight         576.73

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.4438(3)
_cell_length_b                   10.3354(3)
_cell_length_c                   22.0144(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1921.20(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    5359
_cell_measurement_theta_min      2.5650
_cell_measurement_theta_max      29.4960

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.994
_exptl_crystal_F_000             1164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    3.214
_shelx_estimated_absorpt_T_min   0.644
_shelx_estimated_absorpt_T_max   0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90796
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.896
_oxdiff_exptl_absorpt_empirical_full_max 1.138
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            12949
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.584
_diffrn_reflns_theta_max         29.628
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4623
_reflns_number_gt                4158
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.660
_reflns_Friedel_fraction_max     0.784
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_structure_solution    Sir2019
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0164P)²+2.0087P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1546 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(6)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         4623
_refine_ls_number_parameters     263
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0262
_refine_ls_wR_factor_ref         0.0547
_refine_ls_wR_factor_gt          0.0534
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 -0.00023(4) 0.70120(3) 0.74856(2) 0.00981(7) Uani 1 1 d . . . . .
Br1 Br -0.01309(4) 0.95193(4) 0.74415(2) 0.01621(8) Uani 1 1 d . . . . .
N1 N -0.1051(4) 0.6927(3) 0.66523(14) 0.0134(7) Uani 1 1 d . . . . .
H1 H -0.136148 0.611113 0.657276 0.016 Uiso 1 1 calc R U . . .
H1A H -0.190974 0.744186 0.664419 0.016 Uiso 1 1 calc R U . . .
N2 N 0.2060(4) 0.7044(3) 0.69950(14) 0.0131(7) Uani 1 1 d . . . . .
H2 H 0.251282 0.782975 0.702290 0.016 Uiso 1 1 calc R U . . .
H2A H 0.274117 0.645479 0.714447 0.016 Uiso 1 1 calc R U . . .
N3 N -0.2073(4) 0.6979(3) 0.79647(15) 0.0146(8) Uani 1 1 d . . . . .
H3 H -0.262034 0.771042 0.789204 0.017 Uiso 1 1 calc R U . . .
H3A H -0.266711 0.630558 0.784105 0.017 Uiso 1 1 calc R U . . .
N4 N 0.1012(4) 0.7148(3) 0.83224(15) 0.0143(7) Uani 1 1 d . . . . .
H4 H 0.143033 0.637935 0.842762 0.017 Uiso 1 1 calc R U . . .
H4A H 0.179745 0.773618 0.831354 0.017 Uiso 1 1 calc R U . . .
O1 O -0.0536(4) 0.5722(3) 0.54371(15) 0.0288(8) Uani 1 1 d . . . . .
H1B H -0.147474 0.548753 0.541625 0.043 Uiso 1 1 calc R U . . .
C1 C -0.0472(6) 0.7069(4) 0.55475(18) 0.0230(10) Uani 1 1 d . . . . .
H1C H -0.153067 0.744134 0.549466 0.028 Uiso 1 1 calc R U . . .
H1D H 0.023539 0.747599 0.525072 0.028 Uiso 1 1 calc R U . . .
C2 C 0.0120(5) 0.7362(4) 0.61877(15) 0.0154(8) Uani 1 1 d . . . . .
H2C H 0.023923 0.831135 0.622574 0.019 Uiso 1 1 calc R U . . .
C3 C 0.1699(5) 0.6744(4) 0.63477(17) 0.0153(9) Uani 1 1 d . . . . .
H3C H 0.159629 0.579454 0.630390 0.018 Uiso 1 1 calc R U . . .
C4 C 0.3011(5) 0.7208(5) 0.59282(19) 0.0277(12) Uani 1 1 d . . . . .
H4D H 0.277486 0.693309 0.551184 0.033 Uiso 1 1 calc R U . . .
H4C H 0.304543 0.815533 0.593396 0.033 Uiso 1 1 calc R U . . .
O2 O 0.4510(4) 0.6714(4) 0.61016(15) 0.0336(8) Uani 1 1 d . . . . .
H2B H 0.495125 0.723566 0.633307 0.050 Uiso 1 1 calc R U . . .
O3 O -0.3275(5) 0.8738(4) 0.89643(19) 0.0517(11) Uani 1 1 d . . . . .
H3B H -0.357954 0.895722 0.862093 0.078 Uiso 1 1 calc R U . . .
C5 C -0.3154(6) 0.7392(6) 0.8991(2) 0.0314(12) Uani 1 1 d . . . . .
H5 H -0.413383 0.701042 0.883332 0.038 Uiso 1 1 calc R U . . .
H5A H -0.304586 0.712815 0.941642 0.038 Uiso 1 1 calc R U . . .
C6 C -0.1757(5) 0.6862(4) 0.86310(18) 0.0187(10) Uani 1 1 d . . . . .
H6 H -0.163933 0.593300 0.873001 0.022 Uiso 1 1 calc R U . . .
C7 C -0.0197(5) 0.7540(4) 0.87764(15) 0.0167(8) Uani 1 1 d . . . . .
H7 H -0.036071 0.848549 0.874417 0.020 Uiso 1 1 calc R U . . .
C8 C 0.0387(6) 0.7232(5) 0.94167(19) 0.0297(11) Uani 1 1 d . . . . .
H8 H 0.143191 0.762338 0.947897 0.036 Uiso 1 1 calc R U . . .
H8A H -0.034299 0.760506 0.971513 0.036 Uiso 1 1 calc R U . . .
O4 O 0.0489(4) 0.5881(3) 0.95058(16) 0.0385(9) Uani 1 1 d . . . . .
H4B H 0.143334 0.566472 0.952904 0.058 Uiso 1 1 calc R U . . .
S1 S 0.45292(11) 0.44884(12) 0.78992(5) 0.0186(2) Uani 1 1 d . . . . .
O5 O 0.4094(4) 0.4483(6) 0.72609(16) 0.0658(14) Uani 1 1 d . . . . .
O6 O 0.3833(5) 0.5572(5) 0.8206(3) 0.0842(19) Uani 1 1 d . . . . .
O7 O 0.3939(5) 0.3306(5) 0.8168(2) 0.0738(17) Uani 1 1 d . . . . .
O8 O 0.6268(3) 0.4524(4) 0.79627(17) 0.0335(8) Uani 1 1 d . . . . .
O9 O 0.7020(4) 0.4399(4) 0.65644(16) 0.0316(8) Uani 1 1 d D . . . .
O10 O 0.6348(4) 0.5287(4) 0.53493(16) 0.0371(9) Uani 1 1 d D . . . .
O11 O 0.6607(6) 0.0013(7) 0.5481(2) 0.088(2) Uani 1 1 d D . . . .
H10B H 0.582(6) 0.492(5) 0.5081(19) 0.042(17) Uiso 1 1 d D . . . .
H9A H 0.662(5) 0.463(5) 0.6244(14) 0.034(15) Uiso 1 1 d D . . . .
H9B H 0.633(5) 0.446(6) 0.6837(17) 0.05(2) Uiso 1 1 d D . . . .
H10A H 0.571(7) 0.583(5) 0.549(3) 0.09(3) Uiso 1 1 d D . . . .
H11A H 0.640(7) -0.006(7) 0.5834(12) 0.07(2) Uiso 1 1 d D . . . .
H11B H 0.595(7) -0.022(9) 0.524(3) 0.11(3) Uiso 1 1 d D . . . .


_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 N4 2.036(3) . ?
Pd1 N1 2.039(3) . ?
Pd1 N3 2.043(3) . ?
Pd1 N2 2.049(3) . ?
Pd1 Br1 2.5838(5) 4_546 ?
Pd1 Br1 2.5954(5) . ?
N1 C2 1.492(5) . ?
N2 C3 1.490(5) . ?
N3 C6 1.496(5) . ?
N4 C7 1.485(5) . ?
O1 C1 1.415(5) . ?
C1 C2 1.526(5) . ?
C2 C3 1.519(6) . ?
C3 C4 1.519(6) . ?
C4 O2 1.417(6) . ?
O3 C5 1.395(7) . ?
C5 C6 1.523(6) . ?
C6 C7 1.526(6) . ?
C7 C8 1.527(5) . ?
C8 O4 1.412(6) . ?
S1 O6 1.434(4) . ?
S1 O7 1.447(4) . ?
S1 O5 1.452(4) . ?
S1 O8 1.475(3) . ?

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
N4 Pd1 N1 178.30(15) . . ?
N4 Pd1 N3 83.92(14) . . ?
N1 Pd1 N3 95.28(14) . . ?
N4 Pd1 N2 96.80(13) . . ?
N1 Pd1 N2 84.00(13) . . ?
N3 Pd1 N2 179.28(15) . . ?
N4 Pd1 Br1 89.68(10) . 4_546 ?
N1 Pd1 Br1 91.81(10) . 4_546 ?
N3 Pd1 Br1 89.35(10) . 4_546 ?
N2 Pd1 Br1 90.67(10) . 4_546 ?
N4 Pd1 Br1 89.00(10) . . ?
N1 Pd1 Br1 89.51(10) . . ?
N3 Pd1 Br1 90.01(10) . . ?
N2 Pd1 Br1 89.99(10) . . ?
Br1 Pd1 Br1 178.580(11) 4_546 . ?
Pd1 Br1 Pd1 172.479(15) 4_556 . ?
C2 N1 Pd1 108.4(2) . . ?
C3 N2 Pd1 109.1(3) . . ?
C6 N3 Pd1 110.8(3) . . ?
C7 N4 Pd1 109.8(2) . . ?
O1 C1 C2 111.5(4) . . ?
N1 C2 C3 107.2(3) . . ?
N1 C2 C1 110.9(3) . . ?
C3 C2 C1 114.7(3) . . ?
N2 C3 C2 108.3(3) . . ?
N2 C3 C4 111.5(3) . . ?
C2 C3 C4 111.5(3) . . ?
O2 C4 C3 112.0(4) . . ?
O3 C5 C6 113.2(4) . . ?
N3 C6 C5 110.0(4) . . ?
N3 C6 C7 108.8(3) . . ?
C5 C6 C7 113.2(4) . . ?
N4 C7 C6 109.1(3) . . ?
N4 C7 C8 110.1(4) . . ?
C6 C7 C8 112.2(4) . . ?
O4 C8 C7 110.7(4) . . ?
O6 S1 O7 109.0(3) . . ?
O6 S1 O5 110.8(3) . . ?
O7 S1 O5 107.8(3) . . ?
O6 S1 O8 110.1(2) . . ?
O7 S1 O8 109.0(2) . . ?
O5 S1 O8 110.1(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N1 C2 C3 42.8(4) . . . . ?
Pd1 N1 C2 C1 168.8(3) . . . . ?
O1 C1 C2 N1 -67.4(5) . . . . ?
O1 C1 C2 C3 54.3(5) . . . . ?
Pd1 N2 C3 C2 36.7(4) . . . . ?
Pd1 N2 C3 C4 159.7(3) . . . . ?
N1 C2 C3 N2 -52.6(4) . . . . ?
C1 C2 C3 N2 -176.2(3) . . . . ?
N1 C2 C3 C4 -175.7(3) . . . . ?
C1 C2 C3 C4 60.7(5) . . . . ?
N2 C3 C4 O2 54.4(5) . . . . ?
C2 C3 C4 O2 175.5(4) . . . . ?
Pd1 N3 C6 C5 156.3(3) . . . . ?
Pd1 N3 C6 C7 31.7(4) . . . . ?
O3 C5 C6 N3 -71.8(5) . . . . ?
O3 C5 C6 C7 50.3(5) . . . . ?
Pd1 N4 C7 C6 38.5(4) . . . . ?
Pd1 N4 C7 C8 162.0(3) . . . . ?
N3 C6 C7 N4 -46.0(4) . . . . ?
C5 C6 C7 N4 -168.7(4) . . . . ?
N3 C6 C7 C8 -168.2(4) . . . . ?
C5 C6 C7 C8 69.1(5) . . . . ?
N4 C7 C8 O4 -67.3(5) . . . . ?
C6 C7 C8 O4 54.3(5) . . . . ?

_refine_diff_density_max         0.778
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.084

####################################################################### 
# 
# 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_200328RaselPdBrSO4_200K
_database_code_depnum_ccdc_archive 'CCDC 1998641'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Iguchi'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-04-23 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 Br N4 O4 Pd 2+, S O4 2-, 3(H2 O)'
_chemical_formula_sum            'C8 H30 Br N4 O11 Pd S'
_chemical_formula_weight         576.73

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.4382(2)
_cell_length_b                   10.3226(3)
_cell_length_c                   21.9814(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1914.67(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    5429
_cell_measurement_theta_min      2.5600
_cell_measurement_theta_max      29.6590

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_F_000             1164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    3.225
_shelx_estimated_absorpt_T_min   0.643
_shelx_estimated_absorpt_T_max   0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.926
_oxdiff_exptl_absorpt_empirical_full_max 1.131
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            13284
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.586
_diffrn_reflns_theta_max         29.669
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4651
_reflns_number_gt                4176
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.674
_reflns_Friedel_fraction_max     0.798
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_structure_solution    Sir2019
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0165P)²+1.8401P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1561 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(6)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         4651
_refine_ls_number_parameters     263
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0548
_refine_ls_wR_factor_gt          0.0536
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000

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 -0.00013(4) 0.70062(3) 0.74839(2) 0.00774(7) Uani 1 1 d . . . . .
Br1 Br -0.01373(4) 0.95138(4) 0.74396(2) 0.01304(8) Uani 1 1 d . . . . .
N1 N -0.1050(4) 0.6916(3) 0.66488(15) 0.0112(8) Uani 1 1 d . . . . .
H1 H -0.136097 0.608943 0.656844 0.013 Uiso 1 1 calc R U . . .
H1A H -0.192028 0.743574 0.663980 0.013 Uiso 1 1 calc R U . . .
N2 N 0.2065(4) 0.7039(3) 0.69913(14) 0.0113(8) Uani 1 1 d . . . . .
H2 H 0.252039 0.783614 0.701823 0.014 Uiso 1 1 calc R U . . .
H2A H 0.275668 0.644588 0.714378 0.014 Uiso 1 1 calc R U . . .
N3 N -0.2077(4) 0.6975(3) 0.79618(14) 0.0109(8) Uani 1 1 d . . . . .
H3 H -0.263120 0.771447 0.788725 0.013 Uiso 1 1 calc R U . . .
H3A H -0.267675 0.629159 0.783757 0.013 Uiso 1 1 calc R U . . .
N4 N 0.1012(4) 0.7145(3) 0.83201(15) 0.0107(7) Uani 1 1 d . . . . .
H4 H 0.143514 0.636748 0.842749 0.013 Uiso 1 1 calc R U . . .
H4A H 0.180698 0.774057 0.831070 0.013 Uiso 1 1 calc R U . . .
O1 O -0.0522(4) 0.5720(3) 0.54265(14) 0.0231(8) Uani 1 1 d . . . . .
H1B H -0.143755 0.543827 0.549791 0.035 Uiso 1 1 calc R U . . .
C1 C -0.0472(6) 0.7073(4) 0.55447(18) 0.0185(10) Uani 1 1 d . . . . .
H1C H -0.154723 0.744290 0.549497 0.022 Uiso 1 1 calc R U . . .
H1D H 0.023511 0.749762 0.524571 0.022 Uiso 1 1 calc R U . . .
C2 C 0.0123(5) 0.7353(4) 0.61851(15) 0.0119(8) Uani 1 1 d . . . . .
H2C H 0.024331 0.831246 0.622645 0.014 Uiso 1 1 calc R U . . .
C3 C 0.1708(5) 0.6734(4) 0.63444(18) 0.0125(9) Uani 1 1 d . . . . .
H3C H 0.160516 0.577294 0.630142 0.015 Uiso 1 1 calc R U . . .
C4 C 0.3017(5) 0.7198(5) 0.5923(2) 0.0227(11) Uani 1 1 d . . . . .
H4D H 0.278080 0.691340 0.550212 0.027 Uiso 1 1 calc R U . . .
H4C H 0.304592 0.815708 0.592536 0.027 Uiso 1 1 calc R U . . .
O2 O 0.4517(4) 0.6713(3) 0.60986(14) 0.0273(8) Uani 1 1 d . . . . .
H2B H 0.492594 0.721428 0.635536 0.041 Uiso 1 1 calc R U . . .
O3 O -0.3285(5) 0.8750(4) 0.89572(17) 0.0378(10) Uani 1 1 d . . . . .
H3B H -0.351373 0.897239 0.860024 0.057 Uiso 1 1 calc R U . . .
C5 C -0.3166(6) 0.7397(5) 0.8988(2) 0.0235(11) Uani 1 1 d . . . . .
H5 H -0.415595 0.700886 0.882860 0.028 Uiso 1 1 calc R U . . .
H5A H -0.305855 0.713382 0.941914 0.028 Uiso 1 1 calc R U . . .
C6 C -0.1758(5) 0.6863(4) 0.86271(18) 0.0141(9) Uani 1 1 d . . . . .
H6 H -0.163858 0.592337 0.872836 0.017 Uiso 1 1 calc R U . . .
C7 C -0.0204(5) 0.7542(4) 0.87768(15) 0.0134(8) Uani 1 1 d . . . . .
H7 H -0.037165 0.849769 0.874188 0.016 Uiso 1 1 calc R U . . .
C8 C 0.0384(6) 0.7243(5) 0.94185(18) 0.0238(11) Uani 1 1 d . . . . .
H8 H 0.144177 0.763646 0.947946 0.029 Uiso 1 1 calc R U . . .
H8A H -0.035142 0.762527 0.972030 0.029 Uiso 1 1 calc R U . . .
O4 O 0.0479(4) 0.5887(3) 0.95089(15) 0.0310(9) Uani 1 1 d . . . . .
H4B H 0.140766 0.563477 0.943943 0.047 Uiso 1 1 calc R U . . .
S1 S 0.45335(12) 0.44822(12) 0.78980(5) 0.0145(2) Uani 1 1 d . . . . .
O5 O 0.4106(4) 0.4499(5) 0.72573(15) 0.0575(13) Uani 1 1 d . . . . .
O6 O 0.3826(4) 0.5549(5) 0.8218(3) 0.0682(16) Uani 1 1 d . . . . .
O7 O 0.3941(5) 0.3274(5) 0.8154(2) 0.0656(16) Uani 1 1 d . . . . .
O8 O 0.6274(3) 0.4517(4) 0.79668(16) 0.0273(8) Uani 1 1 d . . . . .
O9 O 0.7029(4) 0.4395(4) 0.65612(16) 0.0247(7) Uani 1 1 d D . . . .
O10 O 0.6355(4) 0.5284(4) 0.53482(15) 0.0284(8) Uani 1 1 d D . . . .
O11 O 0.6615(6) 0.0026(7) 0.5486(2) 0.0771(19) Uani 1 1 d D . . . .
H11B H 0.587(6) -0.012(8) 0.526(2) 0.09(3) Uiso 1 1 d D . . . .
H10B H 0.577(7) 0.490(6) 0.510(2) 0.08(2) Uiso 1 1 d D . . . .
H9B H 0.634(5) 0.450(6) 0.6831(18) 0.05(2) Uiso 1 1 d D . . . .
H10A H 0.571(6) 0.582(5) 0.550(3) 0.07(2) Uiso 1 1 d D . . . .
H9A H 0.664(5) 0.464(5) 0.6243(14) 0.031(15) Uiso 1 1 d D . . . .
H11A H 0.637(4) -0.005(7) 0.5843(12) 0.07(2) Uiso 1 1 d D . . . .


_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 N4 2.032(3) . ?
Pd1 N1 2.040(3) . ?
Pd1 N3 2.043(3) . ?
Pd1 N2 2.053(3) . ?
Pd1 Br1 2.5810(5) 4_546 ?
Pd1 Br1 2.5929(6) . ?
N1 C2 1.490(5) . ?
N2 C3 1.487(5) . ?
N3 C6 1.492(5) . ?
N4 C7 1.493(5) . ?
O1 C1 1.422(5) . ?
C1 C2 1.522(5) . ?
C2 C3 1.523(6) . ?
C3 C4 1.520(6) . ?
C4 O2 1.415(5) . ?
O3 C5 1.403(7) . ?
C5 C6 1.532(6) . ?
C6 C7 1.522(6) . ?
C7 C8 1.527(5) . ?
C8 O4 1.417(5) . ?
S1 O6 1.437(4) . ?
S1 O5 1.454(3) . ?
S1 O7 1.457(4) . ?
S1 O8 1.477(3) . ?

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
N4 Pd1 N1 178.37(15) . . ?
N4 Pd1 N3 84.07(13) . . ?
N1 Pd1 N3 95.18(14) . . ?
N4 Pd1 N2 96.82(13) . . ?
N1 Pd1 N2 83.93(14) . . ?
N3 Pd1 N2 179.10(15) . . ?
N4 Pd1 Br1 89.57(10) . 4_546 ?
N1 Pd1 Br1 91.88(10) . 4_546 ?
N3 Pd1 Br1 89.41(10) . 4_546 ?
N2 Pd1 Br1 90.71(10) . 4_546 ?
N4 Pd1 Br1 88.97(10) . . ?
N1 Pd1 Br1 89.58(10) . . ?
N3 Pd1 Br1 89.84(10) . . ?
N2 Pd1 Br1 90.07(10) . . ?
Br1 Pd1 Br1 178.418(12) 4_546 . ?
Pd1 Br1 Pd1 172.187(16) 4_556 . ?
C2 N1 Pd1 108.3(2) . . ?
C3 N2 Pd1 109.2(3) . . ?
C6 N3 Pd1 110.5(3) . . ?
C7 N4 Pd1 109.8(2) . . ?
O1 C1 C2 111.4(3) . . ?
N1 C2 C1 110.9(3) . . ?
N1 C2 C3 107.4(3) . . ?
C1 C2 C3 115.0(3) . . ?
N2 C3 C4 111.7(4) . . ?
N2 C3 C2 108.0(3) . . ?
C4 C3 C2 111.4(3) . . ?
O2 C4 C3 111.8(4) . . ?
O3 C5 C6 112.9(4) . . ?
N3 C6 C7 109.4(3) . . ?
N3 C6 C5 109.8(4) . . ?
C7 C6 C5 113.0(3) . . ?
N4 C7 C6 108.7(3) . . ?
N4 C7 C8 110.1(4) . . ?
C6 C7 C8 112.7(4) . . ?
O4 C8 C7 110.3(4) . . ?
O6 S1 O5 111.2(3) . . ?
O6 S1 O7 109.0(3) . . ?
O5 S1 O7 107.4(3) . . ?
O6 S1 O8 110.2(2) . . ?
O5 S1 O8 110.2(2) . . ?
O7 S1 O8 108.8(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N1 C2 C1 169.4(3) . . . . ?
Pd1 N1 C2 C3 43.0(4) . . . . ?
O1 C1 C2 N1 -68.3(5) . . . . ?
O1 C1 C2 C3 53.8(5) . . . . ?
Pd1 N2 C3 C4 159.7(3) . . . . ?
Pd1 N2 C3 C2 36.8(4) . . . . ?
N1 C2 C3 N2 -52.9(4) . . . . ?
C1 C2 C3 N2 -176.8(3) . . . . ?
N1 C2 C3 C4 -175.9(3) . . . . ?
C1 C2 C3 C4 60.2(5) . . . . ?
N2 C3 C4 O2 54.2(5) . . . . ?
C2 C3 C4 O2 175.1(3) . . . . ?
Pd1 N3 C6 C7 31.8(4) . . . . ?
Pd1 N3 C6 C5 156.4(3) . . . . ?
O3 C5 C6 N3 -71.9(5) . . . . ?
O3 C5 C6 C7 50.6(5) . . . . ?
Pd1 N4 C7 C6 38.4(4) . . . . ?
Pd1 N4 C7 C8 162.3(3) . . . . ?
N3 C6 C7 N4 -46.0(4) . . . . ?
C5 C6 C7 N4 -168.8(3) . . . . ?
N3 C6 C7 C8 -168.3(4) . . . . ?
C5 C6 C7 C8 68.9(5) . . . . ?
N4 C7 C8 O4 -67.7(5) . . . . ?
C6 C7 C8 O4 53.8(5) . . . . ?

_refine_diff_density_max         0.914
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.092

####################################################################### 
# 
# 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_200328RaselPdBrSO4_300K
_database_code_depnum_ccdc_archive 'CCDC 1998643'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Iguchi'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-04-23 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 Br N4 O4 Pd 2+, S O4 2-, 3(H2 O)'
_chemical_formula_sum            'C8 H30 Br N4 O11 Pd S'
_chemical_formula_weight         576.73

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.4409(3)
_cell_length_b                   10.3431(3)
_cell_length_c                   22.0437(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1924.53(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    4811
_cell_measurement_theta_min      3.0070
_cell_measurement_theta_max      29.4920

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.990
_exptl_crystal_F_000             1164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    3.209
_shelx_estimated_absorpt_T_min   0.645
_shelx_estimated_absorpt_T_max   0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83903
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.917
_oxdiff_exptl_absorpt_empirical_full_max 1.206
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            13166
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.584
_diffrn_reflns_theta_max         29.636
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4675
_reflns_number_gt                4052
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.673
_reflns_Friedel_fraction_max     0.801
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_structure_solution    Sir2019
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0159P)²+2.1892P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1473 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(7)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         4675
_refine_ls_number_parameters     263
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0578
_refine_ls_wR_factor_gt          0.0559
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.00030(5) 0.29795(3) 0.24873(2) 0.01128(7) Uani 1 1 d . . . . .
Br1 Br 1.01247(5) 0.04719(4) 0.24436(2) 0.01886(9) Uani 1 1 d . . . . .
N1 N 1.1058(5) 0.3062(4) 0.16565(16) 0.0146(9) Uani 1 1 d . . . . .
H1 H 1.137289 0.386686 0.157909 0.018 Uiso 1 1 calc R U . . .
H1A H 1.190424 0.254886 0.164913 0.018 Uiso 1 1 calc R U . . .
N2 N 0.7941(5) 0.2949(4) 0.19963(16) 0.0150(9) Uani 1 1 d . . . . .
H2 H 0.749285 0.217222 0.202336 0.018 Uiso 1 1 calc R U . . .
H2A H 0.726653 0.353048 0.214414 0.018 Uiso 1 1 calc R U . . .
N3 N 1.2076(5) 0.3012(4) 0.29687(16) 0.0164(9) Uani 1 1 d . . . . .
H3 H 1.261749 0.228961 0.289822 0.020 Uiso 1 1 calc R U . . .
H3A H 1.266438 0.367810 0.284773 0.020 Uiso 1 1 calc R U . . .
N4 N 0.8984(5) 0.2848(4) 0.33227(17) 0.0156(9) Uani 1 1 d . . . . .
H4 H 0.857127 0.360890 0.342550 0.019 Uiso 1 1 calc R U . . .
H4A H 0.820585 0.226831 0.331379 0.019 Uiso 1 1 calc R U . . .
O1 O 1.0534(5) 0.4282(3) 0.04436(16) 0.0335(9) Uani 1 1 d . . . . .
H1B H 1.139120 0.456681 0.055627 0.050 Uiso 1 1 calc R U . . .
C1 C 1.0477(7) 0.2930(5) 0.0552(2) 0.0265(12) Uani 1 1 d . . . . .
H1C H 1.152625 0.256561 0.049866 0.032 Uiso 1 1 calc R U . . .
H1D H 0.977587 0.252743 0.025921 0.032 Uiso 1 1 calc R U . . .
C2 C 0.9890(6) 0.2636(4) 0.11912(17) 0.0173(9) Uani 1 1 d . . . . .
H2C H 0.977298 0.169679 0.122692 0.021 Uiso 1 1 calc R U . . .
C3 C 0.8301(6) 0.3249(5) 0.1351(2) 0.0174(10) Uani 1 1 d . . . . .
H3C H 0.839938 0.418924 0.130877 0.021 Uiso 1 1 calc R U . . .
C4 C 0.6994(6) 0.2786(6) 0.0930(2) 0.0314(14) Uani 1 1 d . . . . .
H4D H 0.723023 0.305999 0.051883 0.038 Uiso 1 1 calc R U . . .
H4C H 0.696088 0.184879 0.093458 0.038 Uiso 1 1 calc R U . . .
O2 O 0.5493(4) 0.3278(4) 0.11024(17) 0.0413(10) Uani 1 1 d . . . . .
H2B H 0.508649 0.279090 0.135152 0.062 Uiso 1 1 calc R U . . .
O3 O 1.3275(7) 0.1272(6) 0.3967(2) 0.0681(15) Uani 1 1 d . . . . .
H3B H 1.351531 0.105540 0.362123 0.102 Uiso 1 1 calc R U . . .
C5 C 1.3147(7) 0.2611(6) 0.3995(2) 0.0375(14) Uani 1 1 d . . . . .
H5 H 1.411529 0.299529 0.384147 0.045 Uiso 1 1 calc R U . . .
H5A H 1.303116 0.287084 0.441588 0.045 Uiso 1 1 calc R U . . .
C6 C 1.1746(6) 0.3129(5) 0.3632(2) 0.0225(12) Uani 1 1 d . . . . .
H6 H 1.162662 0.404957 0.372807 0.027 Uiso 1 1 calc R U . . .
C7 C 1.0185(6) 0.2458(4) 0.37768(17) 0.0206(10) Uani 1 1 d . . . . .
H7 H 1.034554 0.152239 0.374524 0.025 Uiso 1 1 calc R U . . .
C8 C 0.9589(7) 0.2764(5) 0.4414(2) 0.0347(14) Uani 1 1 d . . . . .
H8 H 0.855007 0.238201 0.447120 0.042 Uiso 1 1 calc R U . . .
H8A H 1.030187 0.238808 0.471078 0.042 Uiso 1 1 calc R U . . .
O4 O 0.9497(5) 0.4117(4) 0.45057(18) 0.0442(11) Uani 1 1 d . . . . .
H4B H 0.861467 0.437429 0.440700 0.066 Uiso 1 1 calc R U . . .
S1 S 0.54736(13) 0.55035(14) 0.29007(5) 0.0222(3) Uani 1 1 d . . . . .
O5 O 0.5921(5) 0.5530(6) 0.22680(19) 0.0716(16) Uani 1 1 d . . . . .
O6 O 0.6161(6) 0.4408(6) 0.3194(3) 0.096(2) Uani 1 1 d . . . . .
O7 O 0.6069(5) 0.6665(6) 0.3181(3) 0.083(2) Uani 1 1 d . . . . .
O8 O 0.3740(4) 0.5473(4) 0.29593(19) 0.0384(10) Uani 1 1 d . . . . .
O9 O 0.3000(5) 0.5594(5) 0.15681(19) 0.0401(10) Uani 1 1 d D . . . .
O10 O 0.3659(5) 0.4707(5) 0.0343(2) 0.0462(11) Uani 1 1 d D . . . .
O11 O 0.3394(7) 1.0015(8) 0.0482(3) 0.095(2) Uani 1 1 d D . . . .
H10B H 0.421(8) 0.515(7) 0.011(3) 0.09(3) Uiso 1 1 d D . . . .
H9B H 0.377(5) 0.559(7) 0.182(2) 0.05(2) Uiso 1 1 d D . . . .
H10A H 0.428(8) 0.415(6) 0.049(3) 0.10(3) Uiso 1 1 d D . . . .
H11A H 0.386(3) 0.944(10) 0.069(6) 0.36(12) Uiso 1 1 d D . . . .
H9A H 0.336(6) 0.530(6) 0.1245(16) 0.05(2) Uiso 1 1 d D . . . .
H11B H 0.399(9) 1.024(10) 0.021(3) 0.13(4) Uiso 1 1 d D . . . .


_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 N4 2.037(4) . ?
Pd1 N1 2.038(4) . ?
Pd1 N3 2.047(4) . ?
Pd1 N2 2.050(4) . ?
Pd1 Br1 2.5847(6) 4_755 ?
Pd1 Br1 2.5974(6) . ?
N1 C2 1.489(5) . ?
N2 C3 1.487(6) . ?
N3 C6 1.494(6) . ?
N4 C7 1.480(5) . ?
O1 C1 1.419(6) . ?
C1 C2 1.524(6) . ?
C2 C3 1.525(6) . ?
C3 C4 1.520(6) . ?
C4 O2 1.418(6) . ?
O3 C5 1.391(9) . ?
C5 C6 1.525(7) . ?
C6 C7 1.523(7) . ?
C7 C8 1.525(6) . ?
C8 O4 1.416(6) . ?
S1 O6 1.428(5) . ?
S1 O7 1.441(5) . ?
S1 O5 1.445(4) . ?
S1 O8 1.469(3) . ?

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
N4 Pd1 N1 178.32(17) . . ?
N4 Pd1 N3 83.86(15) . . ?
N1 Pd1 N3 95.26(15) . . ?
N4 Pd1 N2 96.77(15) . . ?
N1 Pd1 N2 84.11(15) . . ?
N3 Pd1 N2 179.37(18) . . ?
N4 Pd1 Br1 89.75(11) . 4_755 ?
N1 Pd1 Br1 91.68(11) . 4_755 ?
N3 Pd1 Br1 89.34(11) . 4_755 ?
N2 Pd1 Br1 90.63(11) . 4_755 ?
N4 Pd1 Br1 89.06(11) . . ?
N1 Pd1 Br1 89.51(10) . . ?
N3 Pd1 Br1 90.11(11) . . ?
N2 Pd1 Br1 89.92(11) . . ?
Br1 Pd1 Br1 178.736(14) 4_755 . ?
Pd1 Br1 Pd1 172.790(18) 4_745 . ?
C2 N1 Pd1 108.5(3) . . ?
C3 N2 Pd1 109.2(3) . . ?
C6 N3 Pd1 110.5(3) . . ?
C7 N4 Pd1 109.9(3) . . ?
O1 C1 C2 111.3(4) . . ?
N1 C2 C1 111.3(4) . . ?
N1 C2 C3 107.5(3) . . ?
C1 C2 C3 114.6(4) . . ?
N2 C3 C4 111.7(4) . . ?
N2 C3 C2 108.3(4) . . ?
C4 C3 C2 111.5(4) . . ?
O2 C4 C3 111.8(4) . . ?
O3 C5 C6 112.8(5) . . ?
N3 C6 C7 109.2(4) . . ?
N3 C6 C5 109.9(4) . . ?
C7 C6 C5 113.7(4) . . ?
N4 C7 C6 109.1(3) . . ?
N4 C7 C8 109.9(4) . . ?
C6 C7 C8 112.5(4) . . ?
O4 C8 C7 110.7(4) . . ?
O6 S1 O7 109.0(4) . . ?
O6 S1 O5 110.2(4) . . ?
O7 S1 O5 107.8(4) . . ?
O6 S1 O8 110.4(3) . . ?
O7 S1 O8 109.1(3) . . ?
O5 S1 O8 110.2(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N1 C2 C1 168.5(3) . . . . ?
Pd1 N1 C2 C3 42.2(4) . . . . ?
O1 C1 C2 N1 -67.7(5) . . . . ?
O1 C1 C2 C3 54.5(6) . . . . ?
Pd1 N2 C3 C4 159.6(3) . . . . ?
Pd1 N2 C3 C2 36.5(4) . . . . ?
N1 C2 C3 N2 -52.2(5) . . . . ?
C1 C2 C3 N2 -176.4(4) . . . . ?
N1 C2 C3 C4 -175.5(4) . . . . ?
C1 C2 C3 C4 60.3(5) . . . . ?
N2 C3 C4 O2 54.4(6) . . . . ?
C2 C3 C4 O2 175.7(4) . . . . ?
Pd1 N3 C6 C7 31.5(4) . . . . ?
Pd1 N3 C6 C5 156.9(4) . . . . ?
O3 C5 C6 N3 -71.8(6) . . . . ?
O3 C5 C6 C7 50.9(7) . . . . ?
Pd1 N4 C7 C6 38.5(4) . . . . ?
Pd1 N4 C7 C8 162.3(3) . . . . ?
N3 C6 C7 N4 -46.0(5) . . . . ?
C5 C6 C7 N4 -169.1(4) . . . . ?
N3 C6 C7 C8 -168.3(4) . . . . ?
C5 C6 C7 C8 68.6(6) . . . . ?
N4 C7 C8 O4 -67.9(6) . . . . ?
C6 C7 C8 O4 53.9(6) . . . . ?

_refine_diff_density_max         0.712
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.089

####################################################################### 
# 
# 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_200328RaselPdBrSO4_150K
_database_code_depnum_ccdc_archive 'CCDC 1998640'
loop_
_audit_author_name
_audit_author_address
'Hiroaki Iguchi'
;Tohoku University
Japan
;
_audit_update_record             
;
2020-04-23 deposited with the CCDC.	2020-05-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H24 Br N4 O4 Pd 2+, S O4 2-, 3(H2 O)'
_chemical_formula_sum            'C8 H30 Br N4 O11 Pd S'
_chemical_formula_weight         576.73

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.4341(2)
_cell_length_b                   10.3131(3)
_cell_length_c                   21.9665(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1910.68(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5714
_cell_measurement_theta_min      2.5810
_cell_measurement_theta_max      29.3170

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.005
_exptl_crystal_F_000             1164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    3.232
_shelx_estimated_absorpt_T_min   0.643
_shelx_estimated_absorpt_T_max   0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88964
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.910
_oxdiff_exptl_absorpt_empirical_full_max 1.158
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            12940
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.182
_diffrn_reflns_theta_max         29.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4568
_reflns_number_gt                4178
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.678
_reflns_Friedel_fraction_max     0.799
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_structure_solution    Sir2019
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0161P)²+3.3342P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1591 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(5)
_chemical_absolute_configuration rmad
_refine_ls_number_reflns         4568
_refine_ls_number_parameters     263
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0558
_refine_ls_wR_factor_gt          0.0547
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001

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 0.00008(4) 0.79968(3) 0.75174(2) 0.00591(7) Uani 1 1 d . . . . .
Br1 Br -0.01430(4) 0.54892(4) 0.75617(2) 0.00998(9) Uani 1 1 d . . . . .
N1 N -0.1054(4) 0.8084(4) 0.83533(15) 0.0076(8) Uani 1 1 d . . . . .
H1 H -0.136681 0.891122 0.843377 0.009 Uiso 1 1 calc R U . . .
H1A H -0.192455 0.756354 0.836114 0.009 Uiso 1 1 calc R U . . .
N2 N 0.2072(4) 0.7964(4) 0.80079(15) 0.0086(8) Uani 1 1 d . . . . .
H2 H 0.252984 0.716740 0.797997 0.010 Uiso 1 1 calc R U . . .
H2A H 0.276168 0.856063 0.785610 0.010 Uiso 1 1 calc R U . . .
N3 N -0.2077(4) 0.8028(4) 0.70417(16) 0.0087(8) Uani 1 1 d . . . . .
H3 H -0.263154 0.728862 0.711756 0.010 Uiso 1 1 calc R U . . .
H3A H -0.267550 0.871275 0.716666 0.010 Uiso 1 1 calc R U . . .
N4 N 0.1010(4) 0.7851(4) 0.66799(16) 0.0087(8) Uani 1 1 d . . . . .
H4 H 0.143682 0.862752 0.657136 0.010 Uiso 1 1 calc R U . . .
H4A H 0.180278 0.725235 0.668923 0.010 Uiso 1 1 calc R U . . .
O1 O -0.0527(4) 0.9280(3) 0.95794(14) 0.0172(7) Uani 1 1 d . . . . .
H1B H -0.145751 0.955031 0.952836 0.026 Uiso 1 1 calc R U . . .
O2 O 0.4520(4) 0.8287(4) 0.89039(15) 0.0220(8) Uani 1 1 d . . . . .
H2B H 0.492279 0.779747 0.864043 0.033 Uiso 1 1 calc R U . . .
O3 O -0.3288(4) 0.6237(4) 0.60451(17) 0.0260(9) Uani 1 1 d . . . . .
H3B H -0.358009 0.601739 0.639584 0.039 Uiso 1 1 calc R U . . .
O4 O 0.0475(4) 0.9114(3) 0.54895(16) 0.0247(8) Uani 1 1 d . . . . .
H4B H 0.142674 0.934830 0.551272 0.037 Uiso 1 1 calc R U . . .
C1 C -0.0469(6) 0.7918(4) 0.94597(19) 0.0147(10) Uani 1 1 d . . . . .
H1C H -0.153984 0.754193 0.951299 0.018 Uiso 1 1 calc R U . . .
H1D H 0.025034 0.749649 0.975574 0.018 Uiso 1 1 calc R U . . .
C2 C 0.0112(5) 0.7648(4) 0.88172(16) 0.0097(8) Uani 1 1 d . . . . .
H2C H 0.023218 0.668806 0.877412 0.012 Uiso 1 1 calc R U . . .
C3 C 0.1707(5) 0.8267(5) 0.86576(19) 0.0098(9) Uani 1 1 d . . . . .
H3C H 0.160795 0.922846 0.870217 0.012 Uiso 1 1 calc R U . . .
C4 C 0.3016(5) 0.7795(5) 0.9079(2) 0.0178(11) Uani 1 1 d . . . . .
H4D H 0.277910 0.807331 0.950026 0.021 Uiso 1 1 calc R U . . .
H4C H 0.304670 0.683595 0.907211 0.021 Uiso 1 1 calc R U . . .
C5 C -0.3167(6) 0.7603(5) 0.6015(2) 0.0188(10) Uani 1 1 d . . . . .
H5 H -0.415772 0.799064 0.617407 0.023 Uiso 1 1 calc R U . . .
H5A H -0.305901 0.786618 0.558352 0.023 Uiso 1 1 calc R U . . .
C6 C -0.1766(5) 0.8139(5) 0.63742(19) 0.0119(10) Uani 1 1 d . . . . .
H6 H -0.164769 0.907886 0.627174 0.014 Uiso 1 1 calc R U . . .
C7 C -0.0209(5) 0.7457(4) 0.62261(16) 0.0115(9) Uani 1 1 d . . . . .
H7 H -0.037959 0.650102 0.626348 0.014 Uiso 1 1 calc R U . . .
C8 C 0.0372(6) 0.7744(5) 0.55810(19) 0.0181(10) Uani 1 1 d . . . . .
H8 H 0.142682 0.734539 0.551827 0.022 Uiso 1 1 calc R U . . .
H8A H -0.037151 0.736393 0.528142 0.022 Uiso 1 1 calc R U . . .
S1 S 0.45373(12) 1.05226(12) 0.71021(5) 0.0111(2) Uani 1 1 d . . . . .
O5 O 0.4123(4) 1.0459(6) 0.77444(16) 0.0480(13) Uani 1 1 d . . . . .
O6 O 0.3812(4) 0.9481(5) 0.6761(2) 0.0528(14) Uani 1 1 d . . . . .
O7 O 0.3952(5) 1.1765(5) 0.6870(2) 0.0505(14) Uani 1 1 d . . . . .
O8 O 0.6278(3) 1.0485(4) 0.70276(16) 0.0202(7) Uani 1 1 d . . . . .
O9 O 0.2961(4) 0.5598(4) 0.65578(15) 0.0185(7) Uani 1 1 d D . . . .
O11 O 0.3391(5) 0.9962(7) 0.5489(2) 0.0650(19) Uani 1 1 d D . . . .
O10 O 0.3646(4) 0.4728(4) 0.53527(16) 0.0212(8) Uani 1 1 d D . . . .
H10B H 0.421(7) 0.510(7) 0.509(3) 0.07(3) Uiso 1 1 d D . . . .
H9A H 0.332(6) 0.550(7) 0.6219(14) 0.036(17) Uiso 1 1 d D . . . .
H10A H 0.431(7) 0.423(6) 0.551(3) 0.06(2) Uiso 1 1 d D . . . .
H11B H 0.410(6) 1.009(8) 0.525(2) 0.07(3) Uiso 1 1 d D . . . .
H11A H 0.374(4) 0.972(9) 0.582(2) 0.11(4) Uiso 1 1 d D . . . .
H9B H 0.368(5) 0.552(7) 0.6815(19) 0.041(19) Uiso 1 1 d D . . . .


_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 N4 2.033(4) . ?
Pd1 N3 2.041(3) . ?
Pd1 N1 2.042(4) . ?
Pd1 N2 2.052(3) . ?
Pd1 Br1 2.5790(6) 4_556 ?
Pd1 Br1 2.5908(6) . ?
N1 C2 1.486(5) . ?
N2 C3 1.493(5) . ?
N3 C6 1.494(5) . ?
N4 C7 1.489(5) . ?
O1 C1 1.430(5) . ?
O2 C4 1.419(5) . ?
O3 C5 1.414(7) . ?
O4 C8 1.430(6) . ?
C1 C2 1.520(5) . ?
C2 C3 1.529(6) . ?
C3 C4 1.520(6) . ?
C5 C6 1.524(6) . ?
C6 C7 1.525(6) . ?
C7 C8 1.528(6) . ?
S1 O6 1.446(4) . ?
S1 O5 1.455(4) . ?
S1 O7 1.465(4) . ?
S1 O8 1.477(3) . ?

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
N4 Pd1 N3 84.11(14) . . ?
N4 Pd1 N1 178.01(16) . . ?
N3 Pd1 N1 94.91(14) . . ?
N4 Pd1 N2 96.74(14) . . ?
N3 Pd1 N2 179.14(16) . . ?
N1 Pd1 N2 84.23(14) . . ?
N4 Pd1 Br1 89.62(11) . 4_556 ?
N3 Pd1 Br1 89.40(10) . 4_556 ?
N1 Pd1 Br1 92.11(10) . 4_556 ?
N2 Pd1 Br1 90.70(10) . 4_556 ?
N4 Pd1 Br1 88.83(11) . . ?
N3 Pd1 Br1 89.71(10) . . ?
N1 Pd1 Br1 89.43(10) . . ?
N2 Pd1 Br1 90.22(10) . . ?
Br1 Pd1 Br1 178.286(12) 4_556 . ?
Pd1 Br1 Pd1 171.951(16) 4_546 . ?
C2 N1 Pd1 108.4(2) . . ?
C3 N2 Pd1 108.8(3) . . ?
C6 N3 Pd1 110.7(3) . . ?
C7 N4 Pd1 109.7(2) . . ?
O1 C1 C2 111.2(4) . . ?
N1 C2 C1 111.6(4) . . ?
N1 C2 C3 107.4(3) . . ?
C1 C2 C3 114.8(4) . . ?
N2 C3 C4 111.4(4) . . ?
N2 C3 C2 108.3(3) . . ?
C4 C3 C2 111.5(4) . . ?
O2 C4 C3 111.8(4) . . ?
O3 C5 C6 113.2(4) . . ?
N3 C6 C5 110.1(4) . . ?
N3 C6 C7 109.0(3) . . ?
C5 C6 C7 112.9(4) . . ?
N4 C7 C6 109.1(3) . . ?
N4 C7 C8 110.3(4) . . ?
C6 C7 C8 112.6(4) . . ?
O4 C8 C7 110.0(4) . . ?
O6 S1 O5 111.5(3) . . ?
O6 S1 O7 109.1(3) . . ?
O5 S1 O7 107.2(3) . . ?
O6 S1 O8 110.1(2) . . ?
O5 S1 O8 110.2(2) . . ?
O7 S1 O8 108.6(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N1 C2 C1 169.5(3) . . . . ?
Pd1 N1 C2 C3 42.8(4) . . . . ?
O1 C1 C2 N1 -67.8(5) . . . . ?
O1 C1 C2 C3 54.7(5) . . . . ?
Pd1 N2 C3 C4 159.4(3) . . . . ?
Pd1 N2 C3 C2 36.5(4) . . . . ?
N1 C2 C3 N2 -52.7(4) . . . . ?
C1 C2 C3 N2 -177.4(3) . . . . ?
N1 C2 C3 C4 -175.5(4) . . . . ?
C1 C2 C3 C4 59.7(5) . . . . ?
N2 C3 C4 O2 54.4(5) . . . . ?
C2 C3 C4 O2 175.5(4) . . . . ?
Pd1 N3 C6 C5 156.1(3) . . . . ?
Pd1 N3 C6 C7 31.7(4) . . . . ?
O3 C5 C6 N3 -71.8(5) . . . . ?
O3 C5 C6 C7 50.3(5) . . . . ?
Pd1 N4 C7 C6 38.3(4) . . . . ?
Pd1 N4 C7 C8 162.5(3) . . . . ?
N3 C6 C7 N4 -46.0(5) . . . . ?
C5 C6 C7 N4 -168.7(4) . . . . ?
N3 C6 C7 C8 -168.7(4) . . . . ?
C5 C6 C7 C8 68.5(5) . . . . ?
N4 C7 C8 O4 -67.6(5) . . . . ?
C6 C7 C8 O4 54.4(5) . . . . ?

_refine_diff_density_max         1.277
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.100

