# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_e54vb
_database_code_depnum_ccdc_archive 'CCDC 1855024'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-09-25 downloaded from the CCDC.
;
_audit_creation_date             2017-02-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H26 Cl2 N2 O4 Pd'
_chemical_formula_sum            'C12 H26 Cl2 N2 O4 Pd'
_chemical_formula_weight         439.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Pd Cl'
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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.2490(4)
_cell_length_b                   10.2640(3)
_cell_length_c                   9.9035(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.976(2)
_cell_angle_gamma                90
_cell_volume                     1639.48(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3472
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.7250
_cell_measurement_theta_min      3.9650
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6658
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.129
_diffrn_reflns_theta_min         3.032
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -54.00   85.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -       15.2374    0.0000  -90.0000 139

#__ type_ start__ end____ width___ exp.time_
  2 omega   -9.00   28.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -       15.2374   77.0000 -150.0000 37

#__ type_ start__ end____ width___ exp.time_
  3 omega  -11.00   70.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -       15.2374   77.0000  -90.0000 81

#__ type_ start__ end____ width___ exp.time_
  4 omega   -1.00   74.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -       15.2374   57.0000  120.0000 75

#__ type_ start__ end____ width___ exp.time_
  5 omega  -58.00  -18.00   1.0000    2.3600
omega____ theta____ kappa____ phi______ frames
    -      -16.1749  108.0000  -18.0000 40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0166924000
_diffrn_orient_matrix_UB_12      -0.0105769000
_diffrn_orient_matrix_UB_13      0.0619798000
_diffrn_orient_matrix_UB_21      0.0393367000
_diffrn_orient_matrix_UB_22      -0.0215628000
_diffrn_orient_matrix_UB_23      0.0307501000
_diffrn_orient_matrix_UB_31      0.0103915000
_diffrn_orient_matrix_UB_32      0.0648295000
_diffrn_orient_matrix_UB_33      0.0203854000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1764
_reflns_number_total             1964
_reflns_odcompleteness_completeness 99.83
_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 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         0.443
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1964
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0263
_refine_ls_restrained_S_all      1.062
_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)+(0.0170P)²+1.0740P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0532
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B), C3(H3A,H3B), C2(H2A,H2B), C5(H5A,H5B), C4(H4A,H4B)
;
_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 0.5000 0.27712(2) 0.2500 0.00810(8) Uani 1 2 d S T P . .
Cl2 Cl 0.5000 0.50501(7) 0.2500 0.01191(17) Uani 1 2 d S T P . .
Cl1 Cl 0.5000 0.05112(7) 0.2500 0.01602(18) Uani 1 2 d S T P . .
O1 O 0.67092(10) 0.30852(14) 0.38710(15) 0.0118(3) Uani 1 1 d . . . . .
O2 O 0.68014(10) 0.35059(14) 0.09908(16) 0.0137(4) Uani 1 1 d . . . . .
N1 N 0.49217(11) 0.28151(16) 0.45544(18) 0.0093(4) Uani 1 1 d . . . . .
H1 H 0.4807 0.3725 0.4767 0.011 Uiso 1 1 calc R . . . .
C1 C 0.57237(14) 0.2492(2) 0.5385(2) 0.0120(5) Uani 1 1 d . . . . .
H1A H 0.5883 0.1610 0.5179 0.014 Uiso 1 1 calc R . . . .
H1B H 0.5651 0.2527 0.6342 0.014 Uiso 1 1 calc R . . . .
C6 C 0.42375(15) 0.2045(2) 0.5032(2) 0.0138(5) Uani 1 1 d . . . . .
H6A H 0.4148 0.2340 0.5933 0.017 Uiso 1 1 calc R . . . .
H6B H 0.4399 0.1135 0.5100 0.017 Uiso 1 1 calc R . . . .
C3 C 0.71706(14) 0.4124(2) 0.3373(2) 0.0138(5) Uani 1 1 d . . . . .
H3A H 0.7644 0.4330 0.4034 0.017 Uiso 1 1 calc R . . . .
H3B H 0.6825 0.4895 0.3242 0.017 Uiso 1 1 calc R . . . .
C2 C 0.64080(14) 0.3417(2) 0.5115(2) 0.0128(5) Uani 1 1 d . . . . .
H2A H 0.6198 0.4303 0.5066 0.015 Uiso 1 1 calc R . . . .
H2B H 0.6857 0.3370 0.5855 0.015 Uiso 1 1 calc R . . . .
C5 C 0.65600(14) 0.2168(2) 0.0908(2) 0.0126(5) Uani 1 1 d . . . . .
H5A H 0.6483 0.1846 0.1805 0.015 Uiso 1 1 calc R . . . .
H5B H 0.6990 0.1653 0.0565 0.015 Uiso 1 1 calc R . . . .
C4 C 0.74640(14) 0.3742(2) 0.2050(2) 0.0150(5) Uani 1 1 d . . . . .
H4A H 0.7813 0.4431 0.1764 0.018 Uiso 1 1 calc R . . . .
H4B H 0.7800 0.2961 0.2190 0.018 Uiso 1 1 calc R . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.00972(14) 0.00759(13) 0.00706(13) 0.000 0.00125(9) 0.000
Cl2 0.0140(4) 0.0082(3) 0.0137(4) 0.000 0.0024(3) 0.000
Cl1 0.0264(5) 0.0083(4) 0.0137(4) 0.000 0.0036(3) 0.000
O1 0.0132(9) 0.0128(8) 0.0100(8) -0.0013(6) 0.0035(7) -0.0007(6)
O2 0.0134(9) 0.0144(8) 0.0128(9) 0.0021(6) -0.0002(7) -0.0003(6)
N1 0.0088(10) 0.0097(9) 0.0097(10) -0.0006(7) 0.0025(8) -0.0007(7)
C1 0.0140(13) 0.0136(11) 0.0084(11) 0.0001(8) 0.0013(9) 0.0028(9)
C6 0.0169(13) 0.0154(12) 0.0097(12) 0.0003(9) 0.0040(10) -0.0031(9)
C3 0.0108(12) 0.0147(12) 0.0158(12) 0.0002(9) 0.0009(9) -0.0027(9)
C2 0.0110(12) 0.0165(12) 0.0104(12) -0.0016(9) -0.0015(9) 0.0013(9)
C5 0.0140(13) 0.0107(11) 0.0133(12) 0.0002(9) 0.0027(10) 0.0043(9)
C4 0.0102(12) 0.0169(12) 0.0179(13) 0.0015(9) 0.0013(10) -0.0002(9)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Cl2 2.3391(7) . ?
Pd1 Cl1 2.3196(7) . ?
Pd1 N1 2.0544(18) . ?
Pd1 N1 2.0544(18) 2_655 ?
O1 C3 1.425(3) . ?
O1 C2 1.421(3) . ?
O2 C5 1.428(3) . ?
O2 C4 1.430(3) . ?
N1 H1 0.9800 . ?
N1 C1 1.491(3) . ?
N1 C6 1.488(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.511(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.507(3) 2_655 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.500(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 C6 1.507(3) 2_655 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
Cl1 Pd1 Cl2 180.0 . . ?
N1 Pd1 Cl2 88.74(5) 2_655 . ?
N1 Pd1 Cl2 88.74(5) . . ?
N1 Pd1 Cl1 91.26(5) . . ?
N1 Pd1 Cl1 91.26(5) 2_655 . ?
N1 Pd1 N1 177.49(9) 2_655 . ?
C2 O1 C3 111.79(16) . . ?
C5 O2 C4 112.48(16) . . ?
Pd1 N1 H1 105.6 . . ?
C1 N1 Pd1 112.72(14) . . ?
C1 N1 H1 105.6 . . ?
C6 N1 Pd1 116.23(13) . . ?
C6 N1 H1 105.6 . . ?
C6 N1 C1 110.07(17) . . ?
N1 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
N1 C1 C2 112.06(18) . . ?
H1A C1 H1B 107.9 . . ?
C2 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
N1 C6 H6A 109.2 . . ?
N1 C6 H6B 109.2 . . ?
N1 C6 C5 112.26(18) . 2_655 ?
H6A C6 H6B 107.9 . . ?
C5 C6 H6A 109.2 2_655 . ?
C5 C6 H6B 109.2 2_655 . ?
O1 C3 H3A 109.6 . . ?
O1 C3 H3B 109.6 . . ?
O1 C3 C4 110.06(18) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.6 . . ?
C4 C3 H3B 109.6 . . ?
O1 C2 C1 109.92(17) . . ?
O1 C2 H2A 109.7 . . ?
O1 C2 H2B 109.7 . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
O2 C5 C6 109.01(17) . 2_655 ?
O2 C5 H5A 109.9 . . ?
O2 C5 H5B 109.9 . . ?
C6 C5 H5A 109.9 2_655 . ?
C6 C5 H5B 109.9 2_655 . ?
H5A C5 H5B 108.3 . . ?
O2 C4 C3 113.24(19) . . ?
O2 C4 H4A 108.9 . . ?
O2 C4 H4B 108.9 . . ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4B 108.9 . . ?
H4A C4 H4B 107.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N1 C1 C2 58.9(2) . . . . ?
Pd1 N1 C6 C5 -41.1(2) . . . 2_655 ?
O1 C3 C4 O2 63.2(2) . . . . ?
N1 C1 C2 O1 -77.9(2) . . . . ?
C1 N1 C6 C5 -170.76(18) . . . 2_655 ?
C6 N1 C1 C2 -169.57(18) . . . . ?
C3 O1 C2 C1 162.89(18) . . . . ?
C2 O1 C3 C4 -179.04(17) . . . . ?
C5 O2 C4 C3 -92.5(2) . . . . ?
C4 O2 C5 C6 169.08(19) . . . 2_655 ?

_iucr_refine_instructions_details 
;

    e54vb.res created by SHELXL-2014/7

TITL e54vb_a.res in C2/c
REM Old TITL e54VB in Cc #9
REM SHELXT solution in C2/c
REM R1 0.056, Rweak 0.066, Alpha 0.044, Orientation as input
REM Formula found by SHELXT: C12 N4 O2 Cl2 Pd
CELL 0.71073 16.249022 10.263954 9.903529 90 96.9757 90
ZERR 4 0.000437 0.000267 0.000258 0 0.0024 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Cl N O Pd
UNIT 48 104 8 8 16 4
 
L.S. 8
PLAN  20
BOND $H
LIST 8
MORE -1
CONF
fmap 2
acta 52
REM <olex2.extras>
REM <HklSrc "%.\\e54VB.hkl">
REM </olex2.extras>
 
WGHT    0.017000    1.074000
FVAR       0.25787
PD1   6    0.500000    0.277117    0.250000    10.50000    0.00972    0.00759 =
         0.00706    0.00000    0.00125    0.00000
CL2   3    0.500000    0.505009    0.250000    10.50000    0.01403    0.00821 =
         0.01366    0.00000    0.00241    0.00000
CL1   3    0.500000    0.051123    0.250000    10.50000    0.02645    0.00825 =
         0.01365    0.00000    0.00355    0.00000
O1    5    0.670922    0.308522    0.387104    11.00000    0.01315    0.01276 =
         0.01000   -0.00133    0.00354   -0.00066
O2    5    0.680140    0.350587    0.099078    11.00000    0.01341    0.01440 =
         0.01275    0.00209   -0.00022   -0.00025
N1    4    0.492174    0.281508    0.455443    11.00000    0.00876    0.00971 =
         0.00970   -0.00061    0.00254   -0.00073
AFIX  13
H1    2    0.480723    0.372492    0.476668    11.00000   -1.20000
AFIX   0
C1    1    0.572367    0.249209    0.538470    11.00000    0.01397    0.01360 =
         0.00840    0.00012    0.00133    0.00277
AFIX  23
H1A   2    0.588279    0.161008    0.517858    11.00000   -1.20000
H1B   2    0.565112    0.252706    0.634186    11.00000   -1.20000
AFIX   0
C6    1    0.423755    0.204481    0.503220    11.00000    0.01693    0.01542 =
         0.00965    0.00033    0.00399   -0.00314
AFIX  23
H6A   2    0.414771    0.234042    0.593302    11.00000   -1.20000
H6B   2    0.439854    0.113490    0.510007    11.00000   -1.20000
AFIX   0
C3    1    0.717064    0.412415    0.337334    11.00000    0.01077    0.01469 =
         0.01582    0.00019    0.00085   -0.00274
AFIX  23
H3A   2    0.764355    0.432961    0.403398    11.00000   -1.20000
H3B   2    0.682490    0.489506    0.324188    11.00000   -1.20000
AFIX   0
C2    1    0.640804    0.341742    0.511520    11.00000    0.01095    0.01651 =
         0.01038   -0.00164   -0.00149    0.00132
AFIX  23
H2A   2    0.619846    0.430321    0.506572    11.00000   -1.20000
H2B   2    0.685656    0.337020    0.585523    11.00000   -1.20000
AFIX   0
C5    1    0.656004    0.216789    0.090814    11.00000    0.01403    0.01073 =
         0.01329    0.00025    0.00269    0.00427
AFIX  23
H5A   2    0.648266    0.184629    0.180505    11.00000   -1.20000
H5B   2    0.699004    0.165251    0.056532    11.00000   -1.20000
AFIX   0
C4    1    0.746400    0.374232    0.205036    11.00000    0.01019    0.01690 =
         0.01793    0.00148    0.00129   -0.00024
AFIX  23
H4A   2    0.781338    0.443066    0.176413    11.00000   -1.20000
H4B   2    0.779958    0.296121    0.218987    11.00000   -1.20000
AFIX   0
HKLF 4
 
REM  e54vb_a.res in C2/c
REM R1 =  0.0263 for    1764 Fo > 4sig(Fo)  and  0.0309 for all    1964 data
REM     97 parameters refined using      0 restraints
 
END  
     
WGHT      0.0165      1.0737 

REM Highest difference peak  0.443,  deepest hole -0.681,  1-sigma level  0.102
Q1    1   0.5291  0.2761  0.4821  11.00000  0.05    0.44
Q2    1   0.6863  0.3585  0.3545  11.00000  0.05    0.44
Q3    1   0.4848  0.5570  0.1474  11.00000  0.05    0.39
Q4    1   0.7100  0.2965  0.4167  11.00000  0.05    0.39
Q5    1   0.4955  0.0408  0.5867  11.00000  0.05    0.39
Q6    1   0.4987  0.2733  0.3878  11.00000  0.05    0.37
Q7    1   0.6795  0.3754  0.0426  11.00000  0.05    0.37
Q8    1   0.7075  0.3573  0.1439  11.00000  0.05    0.37
Q9    1   0.4363  0.1766  0.2468  11.00000  0.05    0.36
Q10   1   0.5260  0.0202  0.1706  11.00000  0.05    0.34
Q11   1   0.8789  0.3732  0.2636  11.00000  0.05    0.34
Q12   1   0.3998  0.3397  0.6010  11.00000  0.05    0.33
Q13   1   0.6787  0.4495  0.2983  11.00000  0.05    0.33
Q14   1   0.4541  0.3816  0.6245  11.00000  0.05    0.32
Q15   1   0.3904  0.2171  0.4551  11.00000  0.05    0.32
Q16   1   0.8100  0.1603  0.2108  11.00000  0.05    0.32
Q17   1   0.7841  0.2972  0.1664  11.00000  0.05    0.31
Q18   1   0.7201  0.2263  0.5130  11.00000  0.05    0.31
Q19   1   0.6459  0.5212  0.3504  11.00000  0.05    0.31
Q20   1   0.5997  0.2951  0.5012  11.00000  0.05    0.30

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0263 for 1764 Fo > 4sig(Fo) and 0.0309 for all 6816 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.44, deepest hole -0.68
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0309
  REM R1_gt = 0.0263
  REM wR_ref = 0.0532
  REM GOOF = 1.062
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 6816
  REM Reflections_gt = 1764
  REM Parameters = n/a
  REM Hole = -0.68
  REM Peak = 0.44
  REM Flack = n/a

  
;
_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_e97vb
_database_code_depnum_ccdc_archive 'CCDC 1855026'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-09-25 downloaded from the CCDC.
;
_audit_creation_date             2016-04-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H26 Cl2 N2 O4 Pb'
_chemical_formula_sum            'C12 H26 Cl2 N2 O4 Pb'
_chemical_formula_weight         540.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O S N Pd P Cl'
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'
Pb Pb -3.3944 10.1111 '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                   7.46450(19)
_cell_length_b                   7.6682(2)
_cell_length_c                   16.3035(5)
_cell_angle_alpha                90
_cell_angle_beta                 100.063(3)
_cell_angle_gamma                90
_cell_volume                     918.84(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2092
_cell_measurement_temperature    100.29(10)
_cell_measurement_theta_max      28.6920
_cell_measurement_theta_min      3.8750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0260
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4040
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.161
_diffrn_reflns_theta_min         2.771
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.29(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    3.00   87.00   1.0000   12.1000
omega____ theta____ kappa____ phi______ frames
    -       15.2374   19.0000  -90.0000 84

#__ type_ start__ end____ width___ exp.time_
  2 omega  -17.00   30.00   1.0000   12.1000
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -99.0000  -30.0000 47

#__ type_ start__ end____ width___ exp.time_
  3 omega  -64.00  -20.00   1.0000   12.1000
omega____ theta____ kappa____ phi______ frames
    -      -16.0187  -38.0000   60.0000 44

#__ type_ start__ end____ width___ exp.time_
  4 omega  -71.00  -31.00   1.0000   12.1000
omega____ theta____ kappa____ phi______ frames
    -      -16.0187  138.0000 -150.0000 40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0177970000
_diffrn_orient_matrix_UB_12      -0.0036653000
_diffrn_orient_matrix_UB_13      -0.0441394000
_diffrn_orient_matrix_UB_21      0.0399858000
_diffrn_orient_matrix_UB_22      -0.0841133000
_diffrn_orient_matrix_UB_23      0.0013880000
_diffrn_orient_matrix_UB_31      -0.0860260000
_diffrn_orient_matrix_UB_32      -0.0383363000
_diffrn_orient_matrix_UB_33      0.0011142000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1623
_reflns_number_total             2134
_reflns_odcompleteness_completeness 99.90
_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 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.158
_refine_diff_density_min         -1.100
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2134
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0262
_refine_ls_restrained_S_all      1.010
_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)+(0.0119P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0470
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B), C6(H6A,H6B), C5(H5A,H5B), C1(H1A,H1B)
;
_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
Pb1 Pb 1.0000 0.5000 0.5000 0.01249(7) Uani 1 2 d S T P . .
O2 O 1.1805(4) 0.4560(4) 0.66665(18) 0.0203(7) Uani 1 1 d . . . . .
O1 O 0.9510(3) 0.1979(4) 0.59271(16) 0.0173(7) Uani 1 1 d . . . . .
N1 N 0.7195(4) 0.2814(5) 0.4380(2) 0.0169(8) Uani 1 1 d . . . . .
H1 H 0.6107 0.3347 0.4534 0.020 Uiso 1 1 calc R . . . .
C4 C 1.1904(5) 0.2843(6) 0.6998(3) 0.0251(11) Uani 1 1 d . . . . .
H4A H 1.2320 0.2873 0.7596 0.030 Uiso 1 1 calc R . . . .
H4B H 1.2749 0.2144 0.6748 0.030 Uiso 1 1 calc R . . . .
C3 C 1.0028(5) 0.2081(7) 0.6801(2) 0.0240(11) Uani 1 1 d . . . . .
H3A H 1.0018 0.0928 0.7045 0.029 Uiso 1 1 calc R . . . .
H3B H 0.9179 0.2811 0.7033 0.029 Uiso 1 1 calc R . . . .
C2 C 0.7724(5) 0.1226(6) 0.5698(3) 0.0221(11) Uani 1 1 d . . . . .
H2A H 0.6824 0.1956 0.5893 0.026 Uiso 1 1 calc R . . . .
H2B H 0.7690 0.0078 0.5945 0.026 Uiso 1 1 calc R . . . .
C6 C 0.6822(5) 0.2702(6) 0.3475(2) 0.0223(11) Uani 1 1 d . . . . .
H6A H 0.5738 0.2006 0.3299 0.027 Uiso 1 1 calc R . . . .
H6B H 0.7831 0.2129 0.3282 0.027 Uiso 1 1 calc R . . . .
C5 C 1.3448(5) 0.5522(6) 0.6905(3) 0.0245(12) Uani 1 1 d . . . . .
H5A H 1.4446 0.4935 0.6711 0.029 Uiso 1 1 calc R . . . .
H5B H 1.3738 0.5614 0.7507 0.029 Uiso 1 1 calc R . . . .
Cl1 Cl 1.27292(14) 0.34990(18) 0.42491(8) 0.0324(3) Uani 1 1 d . . . . .
C1 C 0.7331(6) 0.1097(6) 0.4766(3) 0.0228(11) Uani 1 1 d . . . . .
H1A H 0.8293 0.0441 0.4578 0.027 Uiso 1 1 calc R . . . .
H1B H 0.6198 0.0471 0.4595 0.027 Uiso 1 1 calc R . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.01118(11) 0.01457(13) 0.01194(11) -0.00010(11) 0.00265(7) -0.00053(11)
O2 0.0169(15) 0.022(2) 0.0205(17) 0.0030(14) -0.0009(12) -0.0009(13)
O1 0.0195(15) 0.0193(19) 0.0133(15) -0.0002(14) 0.0040(11) -0.0019(13)
N1 0.0136(17) 0.018(2) 0.0192(19) -0.0003(17) 0.0031(14) 0.0006(16)
C4 0.029(3) 0.028(3) 0.016(2) 0.007(2) -0.0021(19) 0.007(2)
C3 0.035(3) 0.026(3) 0.012(2) 0.007(2) 0.0043(18) -0.004(2)
C2 0.017(2) 0.018(3) 0.030(3) 0.000(2) 0.0036(19) -0.007(2)
C6 0.018(2) 0.029(3) 0.020(2) -0.008(2) 0.0026(18) -0.002(2)
C5 0.019(2) 0.035(3) 0.017(2) -0.001(2) -0.0012(18) -0.002(2)
Cl1 0.0224(6) 0.0334(8) 0.0430(7) -0.0155(6) 0.0103(5) 0.0025(6)
C1 0.022(2) 0.019(3) 0.028(3) -0.001(2) 0.0041(19) -0.001(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N1 2.734(3) 3_766 ?
Pb1 N1 2.734(3) . ?
Pb1 Cl1 2.8010(10) . ?
Pb1 Cl1 2.8010(10) 3_766 ?
O2 C4 1.420(5) . ?
O2 C5 1.426(5) . ?
O1 C3 1.413(5) . ?
O1 C2 1.440(4) . ?
N1 H1 0.9800 . ?
N1 C6 1.456(5) . ?
N1 C1 1.456(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.499(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.499(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.495(6) 3_766 ?
C5 C6 1.495(6) 3_766 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?

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 Pb1 N1 180.0 3_766 . ?
N1 Pb1 Cl1 98.92(7) . . ?
N1 Pb1 Cl1 81.08(7) 3_766 . ?
N1 Pb1 Cl1 98.92(7) 3_766 3_766 ?
N1 Pb1 Cl1 81.08(7) . 3_766 ?
Cl1 Pb1 Cl1 180.0 3_766 . ?
C4 O2 C5 113.0(3) . . ?
C3 O1 C2 111.2(3) . . ?
Pb1 N1 H1 105.3 . . ?
C6 N1 Pb1 114.2(2) . . ?
C6 N1 H1 105.3 . . ?
C1 N1 Pb1 113.8(2) . . ?
C1 N1 H1 105.3 . . ?
C1 N1 C6 111.8(4) . . ?
O2 C4 H4A 110.3 . . ?
O2 C4 H4B 110.3 . . ?
O2 C4 C3 107.2(3) . . ?
H4A C4 H4B 108.5 . . ?
C3 C4 H4A 110.3 . . ?
C3 C4 H4B 110.3 . . ?
O1 C3 C4 108.6(3) . . ?
O1 C3 H3A 110.0 . . ?
O1 C3 H3B 110.0 . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
O1 C2 H2A 110.2 . . ?
O1 C2 H2B 110.2 . . ?
O1 C2 C1 107.3(3) . . ?
H2A C2 H2B 108.5 . . ?
C1 C2 H2A 110.2 . . ?
C1 C2 H2B 110.2 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 C5 110.7(4) . 3_766 ?
H6A C6 H6B 108.1 . . ?
C5 C6 H6A 109.5 3_766 . ?
C5 C6 H6B 109.5 3_766 . ?
O2 C5 C6 108.1(3) . 3_766 ?
O2 C5 H5A 110.1 . . ?
O2 C5 H5B 110.1 . . ?
C6 C5 H5A 110.1 3_766 . ?
C6 C5 H5B 110.1 3_766 . ?
H5A C5 H5B 108.4 . . ?
N1 C1 C2 111.4(4) . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pb1 N1 C6 C5 -53.2(4) . . . 3_766 ?
Pb1 N1 C1 C2 48.5(4) . . . . ?
O2 C4 C3 O1 62.9(5) . . . . ?
O1 C2 C1 N1 -65.6(5) . . . . ?
C4 O2 C5 C6 -179.7(3) . . . 3_766 ?
C3 O1 C2 C1 -177.5(4) . . . . ?
C2 O1 C3 C4 179.0(4) . . . . ?
C6 N1 C1 C2 179.7(3) . . . . ?
C5 O2 C4 C3 172.1(3) . . . . ?
C1 N1 C6 C5 175.8(3) . . . 3_766 ?

_shelx_SHELXL_version_number     2014/7
_iucr_refine_instructions_details 
;

    e97vb.res created by SHELXL-2014/7

TITL e97VB in P21/c #14
REM reset to P21/c #14
CELL 0.71073 7.4645 7.668198 16.303467 90 100.0632 90
ZERR 2 0.000194 0.000226 0.000455 0 0.0025 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N O Pb
UNIT 24 52 4 4 8 2
 
L.S. 4
PLAN  20
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\e97VB.hkl">
REM </olex2.extras>
 
WGHT    0.011900
FVAR       2.78308
PB1   6    1.000000    0.500000    0.500000    10.50000    0.01118    0.01457 =
         0.01194   -0.00010    0.00265   -0.00053
O2    5    1.180452    0.455966    0.666649    11.00000    0.01685    0.02203 =
         0.02051    0.00296   -0.00089   -0.00092
O1    5    0.950959    0.197872    0.592714    11.00000    0.01955    0.01933 =
         0.01329   -0.00025    0.00396   -0.00194
N1    4    0.719486    0.281431    0.437985    11.00000    0.01364    0.01796 =
         0.01918   -0.00033    0.00306    0.00058
AFIX  13
H1    2    0.610742    0.334733    0.453399    11.00000   -1.20000
AFIX   0
C4    1    1.190430    0.284307    0.699802    11.00000    0.02856    0.02849 =
         0.01611    0.00688   -0.00208    0.00660
AFIX  23
H4A   2    1.231985    0.287311    0.759579    11.00000   -1.20000
H4B   2    1.274940    0.214446    0.674802    11.00000   -1.20000
AFIX   0
C3    1    1.002825    0.208128    0.680149    11.00000    0.03458    0.02608 =
         0.01156    0.00704    0.00430   -0.00379
AFIX  23
H3A   2    1.001800    0.092781    0.704485    11.00000   -1.20000
H3B   2    0.917879    0.281127    0.703262    11.00000   -1.20000
AFIX   0
C2    1    0.772435    0.122604    0.569778    11.00000    0.01707    0.01844 =
         0.03046   -0.00040    0.00356   -0.00716
AFIX  23
H2A   2    0.682413    0.195626    0.589283    11.00000   -1.20000
H2B   2    0.769011    0.007838    0.594478    11.00000   -1.20000
AFIX   0
C6    1    0.682219    0.270158    0.347459    11.00000    0.01849    0.02864 =
         0.01955   -0.00805    0.00261   -0.00198
AFIX  23
H6A   2    0.573799    0.200550    0.329890    11.00000   -1.20000
H6B   2    0.783082    0.212944    0.328175    11.00000   -1.20000
AFIX   0
C5    1    1.344782    0.552229    0.690539    11.00000    0.01932    0.03526 =
         0.01726   -0.00072   -0.00116   -0.00175
AFIX  23
H5A   2    1.444572    0.493476    0.671090    11.00000   -1.20000
H5B   2    1.373815    0.561401    0.750740    11.00000   -1.20000
AFIX   0
CL1   3    1.272921    0.349902    0.424907    11.00000    0.02236    0.03343 =
         0.04305   -0.01546    0.01029    0.00252
C1    1    0.733128    0.109706    0.476648    11.00000    0.02199    0.01858 =
         0.02785   -0.00147    0.00412   -0.00108
AFIX  23
H1A   2    0.829347    0.044123    0.457759    11.00000   -1.20000
H1B   2    0.619836    0.047134    0.459502    11.00000   -1.20000
AFIX   0
HKLF 4
 
REM  e97VB in P21/c #14
REM R1 =  0.0262 for    1623 Fo > 4sig(Fo)  and  0.0405 for all    2134 data
REM     97 parameters refined using      0 restraints
 
END  
     
WGHT      0.0119      0.0000 

REM Highest difference peak  1.158,  deepest hole -1.100,  1-sigma level  0.157
Q1    1   1.0869  0.4979  0.4622  11.00000  0.05    1.16
Q2    1   0.9153  0.4966  0.4613  11.00000  0.05    0.96
Q3    1   0.5000  0.5000  0.5000  10.50000  0.05    0.66
Q4    1   1.0603  0.3460  0.4895  11.00000  0.05    0.65
Q5    1   0.9997  0.5943  0.4735  11.00000  0.05    0.65
Q6    1   0.8486  0.1921  0.6141  11.00000  0.05    0.58
Q7    1   1.5836  0.5240  0.6323  11.00000  0.05    0.58
Q8    1   1.1821  0.3766  0.4691  11.00000  0.05    0.57
Q9    1   1.3164  0.3188  0.4758  11.00000  0.05    0.57
Q10   1   1.2043  0.3297  0.5214  11.00000  0.05    0.54
Q11   1   0.9814  0.4105  0.4434  11.00000  0.05    0.53
Q12   1   0.7935  0.3210  0.4814  11.00000  0.05    0.52
Q13   1   1.2495  0.5019  0.7016  11.00000  0.05    0.52
Q14   1   1.1717  0.3354  0.4128  11.00000  0.05    0.50
Q15   1   1.0113 -0.0017  0.7320  11.00000  0.05    0.50
Q16   1   0.5388 -0.1317  0.3991  11.00000  0.05    0.50
Q17   1   0.7700  0.2884  0.2746  11.00000  0.05    0.50
Q18   1   0.6431  0.0051  0.4334  11.00000  0.05    0.48
Q19   1   0.8453  0.4241  0.4657  11.00000  0.05    0.48
Q20   1   1.1807  0.5156  0.4324  11.00000  0.05    0.48

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0262 for 1623 Fo > 4sig(Fo) and 0.0405 for all 4311 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.16, deepest hole -1.10
  REM Mean Shift 0, Max Shift 0.000.
  
  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0405
  REM R1_gt = 0.0262
  REM wR_ref = 0.0470
  REM GOOF = 1.010
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 4311
  REM Reflections_gt = 1623
  REM Parameters = n/a
  REM Hole = -1.10
  REM Peak = 1.16
  REM Flack = n/a
  
  
;
_olex2_date_sample_data_collection 2016-04-26
_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_e55vb
_database_code_depnum_ccdc_archive 'CCDC 1855025'
_audit_update_record             
;
2018-07-10 deposited with the CCDC.
2018-09-25 downloaded from the CCDC.
;
_audit_creation_date             2015-12-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H26 Cl2 N2 O4 Pd'
_chemical_formula_sum            'C12 H26 Cl2 N2 O4 Pd'
_chemical_formula_weight         439.65
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N S Rb'
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      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                   6.5577(3)
_cell_length_b                   7.8482(3)
_cell_length_c                   7.8785(3)
_cell_angle_alpha                83.909(3)
_cell_angle_beta                 81.020(3)
_cell_angle_gamma                87.767(3)
_cell_volume                     398.15(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5580
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.9800
_cell_measurement_theta_min      3.1330
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.517
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.23
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8570
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.147
_diffrn_reflns_theta_min         2.611
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -1.00   83.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374   57.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
  2 omega  -52.00   42.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -77.0000 -120.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega   -4.00   84.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374   38.0000 -180.0000 88

#__ type_ start__ end____ width___ exp.time_
  4 omega   -1.00   83.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374   57.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
  5 omega  -83.00    1.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -      -16.0187  -57.0000   30.0000 84

#__ type_ start__ end____ width___ exp.time_
  6 omega  -27.00   20.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -      -16.0187  -93.0000  135.0000 47

#__ type_ start__ end____ width___ exp.time_
  7 omega  -20.00   54.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -99.0000    0.0000 74

#__ type_ start__ end____ width___ exp.time_
  8 omega   34.00   88.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374 -178.0000 -120.0000 54

#__ type_ start__ end____ width___ exp.time_
  9 omega   -1.00   83.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374   57.0000  -90.0000 84

#__ type_ start__ end____ width___ exp.time_
 10 omega  -20.00   54.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -99.0000  150.0000 74

#__ type_ start__ end____ width___ exp.time_
 11 omega  -54.00   34.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -38.0000   30.0000 88

#__ type_ start__ end____ width___ exp.time_
 12 omega  -54.00   34.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -38.0000    0.0000 88

#__ type_ start__ end____ width___ exp.time_
 13 omega  -52.00  -12.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -      -16.0187   93.0000 -112.0000 40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0419045000
_diffrn_orient_matrix_UB_12      0.0820995000
_diffrn_orient_matrix_UB_13      0.0175739000
_diffrn_orient_matrix_UB_21      0.0891408000
_diffrn_orient_matrix_UB_22      0.0172042000
_diffrn_orient_matrix_UB_23      0.0354556000
_diffrn_orient_matrix_UB_31      0.0479106000
_diffrn_orient_matrix_UB_32      0.0350578000
_diffrn_orient_matrix_UB_33      -0.0826315000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1859
_reflns_number_total             1929
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1929
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0242
_refine_ls_restrained_S_all      1.080
_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)+(0.0167P)²+0.2810P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0508
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C1(H1A,H1B), C3(H3B,H3A), C2(H2A,H2B), C5(H5A,H5B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5000 1.0000 0.5000 0.00649(7) Uani 1 2 d S T P . .
Cl1 Cl 0.28005(8) 0.82692(6) 0.39309(6) 0.01083(11) Uani 1 1 d . . . . .
O2 O 0.6013(2) 0.73268(18) 0.79317(18) 0.0111(3) Uani 1 1 d . . . . .
O1 O 0.1649(2) 0.85543(18) 0.85795(18) 0.0115(3) Uani 1 1 d . . . . .
C4 C 0.4266(3) 0.6280(3) 0.8032(3) 0.0114(4) Uani 1 1 d . . . . .
H4A H 0.4604 0.5111 0.8446 0.014 Uiso 1 1 calc R . . . .
H4B H 0.3875 0.6277 0.6895 0.014 Uiso 1 1 calc R . . . .
C6 C 0.7676(3) 0.6817(3) 0.4956(3) 0.0108(4) Uani 1 1 d . . . . .
H6A H 0.8876 0.6222 0.4393 0.013 Uiso 1 1 calc R . . . .
H6B H 0.6465 0.6197 0.4830 0.013 Uiso 1 1 calc R . . . .
C1 C 0.2103(3) 1.1577(3) 0.7855(3) 0.0109(4) Uani 1 1 d . . . . .
H1A H 0.0648 1.1819 0.8219 0.013 Uiso 1 1 calc R . . . .
H1B H 0.2866 1.2542 0.8079 0.013 Uiso 1 1 calc R . . . .
C3 C 0.2492(3) 0.6971(3) 0.9251(3) 0.0121(4) Uani 1 1 d . . . . .
H3B H 0.1411 0.6131 0.9503 0.015 Uiso 1 1 calc R . . . .
H3A H 0.2967 0.7130 1.0328 0.015 Uiso 1 1 calc R . . . .
C2 C 0.2737(3) 1.0002(3) 0.8928(3) 0.0108(4) Uani 1 1 d . . . . .
H2A H 0.4214 0.9797 0.8651 0.013 Uiso 1 1 calc R . . . .
H2B H 0.2417 1.0168 1.0145 0.013 Uiso 1 1 calc R . . . .
C5 C 0.7821(3) 0.6760(3) 0.6871(3) 0.0119(4) Uani 1 1 d . . . . .
H5A H 0.8148 0.5591 0.7294 0.014 Uiso 1 1 calc R . . . .
H5B H 0.8961 0.7463 0.7000 0.014 Uiso 1 1 calc R . . . .
N1 N 0.2454(3) 1.1429(2) 0.5952(2) 0.0083(3) Uani 1 1 d . . . . .
H1 H 0.1255 1.0831 0.5726 0.010 Uiso 1 1 calc R . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.00510(12) 0.00734(11) 0.00679(12) -0.00152(8) 0.00010(8) 0.00078(8)
Cl1 0.0089(3) 0.0126(2) 0.0116(2) -0.00389(18) -0.00160(19) -0.00159(19)
O2 0.0099(8) 0.0118(7) 0.0111(7) -0.0028(6) 0.0007(6) -0.0001(6)
O1 0.0096(8) 0.0110(7) 0.0136(8) 0.0007(6) -0.0027(6) -0.0004(6)
C4 0.0120(11) 0.0102(10) 0.0122(10) -0.0008(8) -0.0025(8) -0.0013(8)
C6 0.0099(11) 0.0088(9) 0.0125(10) -0.0002(8) 0.0009(8) 0.0023(8)
C1 0.0095(11) 0.0132(10) 0.0096(10) -0.0048(8) 0.0015(8) 0.0009(8)
C3 0.0113(11) 0.0115(10) 0.0121(10) 0.0022(8) 0.0009(8) -0.0017(8)
C2 0.0086(11) 0.0145(10) 0.0090(10) -0.0024(8) 0.0003(8) -0.0007(8)
C5 0.0078(10) 0.0142(10) 0.0131(11) -0.0005(8) -0.0016(8) 0.0041(8)
N1 0.0073(9) 0.0087(8) 0.0084(8) -0.0013(6) 0.0007(7) 0.0011(7)

_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 Cl1 2.3259(5) . ?
Pd1 Cl1 2.3259(5) 2_676 ?
Pd1 N1 2.0618(17) 2_676 ?
Pd1 N1 2.0618(17) . ?
O2 C4 1.423(2) . ?
O2 C5 1.425(2) . ?
O1 C3 1.424(2) . ?
O1 C2 1.437(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.511(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.523(3) . ?
C6 N1 1.488(2) 2_676 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.505(3) . ?
C1 N1 1.496(3) . ?
C3 H3B 0.9700 . ?
C3 H3A 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
N1 C6 1.488(2) 2_676 ?
N1 H1 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pd1 Cl1 180.0 2_676 . ?
N1 Pd1 Cl1 91.44(5) 2_676 . ?
N1 Pd1 Cl1 91.44(5) . 2_676 ?
N1 Pd1 Cl1 88.56(5) . . ?
N1 Pd1 Cl1 88.56(5) 2_676 2_676 ?
N1 Pd1 N1 180.0 . 2_676 ?
C4 O2 C5 114.61(16) . . ?
C3 O1 C2 112.18(16) . . ?
O2 C4 H4A 109.8 . . ?
O2 C4 H4B 109.8 . . ?
O2 C4 C3 109.31(17) . . ?
H4A C4 H4B 108.3 . . ?
C3 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H6A C6 H6B 107.5 . . ?
C5 C6 H6A 108.6 . . ?
C5 C6 H6B 108.6 . . ?
N1 C6 H6A 108.6 2_676 . ?
N1 C6 H6B 108.6 2_676 . ?
N1 C6 C5 114.80(17) 2_676 . ?
H1A C1 H1B 107.6 . . ?
C2 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
N1 C1 H1A 108.7 . . ?
N1 C1 H1B 108.7 . . ?
N1 C1 C2 114.19(16) . . ?
O1 C3 C4 113.28(17) . . ?
O1 C3 H3B 108.9 . . ?
O1 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
C4 C3 H3A 108.9 . . ?
H3B C3 H3A 107.7 . . ?
O1 C2 C1 109.26(17) . . ?
O1 C2 H2A 109.8 . . ?
O1 C2 H2B 109.8 . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
O2 C5 C6 115.44(17) . . ?
O2 C5 H5A 108.4 . . ?
O2 C5 H5B 108.4 . . ?
C6 C5 H5A 108.4 . . ?
C6 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
Pd1 N1 H1 105.6 . . ?
C6 N1 Pd1 114.17(12) 2_676 . ?
C6 N1 C1 108.06(15) 2_676 . ?
C6 N1 H1 105.6 2_676 . ?
C1 N1 Pd1 116.80(13) . . ?
C1 N1 H1 105.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C4 C3 O1 70.4(2) . . . . ?
C4 O2 C5 C6 65.3(2) . . . . ?
C3 O1 C2 C1 167.15(16) . . . . ?
C2 O1 C3 C4 -86.2(2) . . . . ?
C2 C1 N1 Pd1 -34.2(2) . . . . ?
C2 C1 N1 C6 -164.49(17) . . . 2_676 ?
C5 O2 C4 C3 177.50(16) . . . . ?
N1 C6 C5 O2 68.4(2) 2_676 . . . ?
N1 C1 C2 O1 -57.2(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
_iucr_refine_instructions_details 
;

    e55vb.res created by SHELXL-2014/7

TITL CF solution in P-1
CELL 0.71073 6.557739 7.848212 7.878546 83.9093 81.0196 87.7671
ZERR 1 0.000261 0.000285 0.000267 0.0029 0.0031 0.0031
LATT 1
SFAC C H Cl N O Pd
UNIT 12 26 2 2 4 1
 
L.S. 4
PLAN  25
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\e55VB.hkl">
REM </olex2.extras>
 
WGHT    0.016700    0.281000
FVAR      10.69711
PD1   6    0.500000    1.000000    0.500000    10.50000    0.00510    0.00734 =
         0.00679   -0.00152    0.00010    0.00078
CL1   3    0.280047    0.826917    0.393089    11.00000    0.00893    0.01263 =
         0.01162   -0.00389   -0.00160   -0.00159
O2    5    0.601313    0.732676    0.793168    11.00000    0.00989    0.01183 =
         0.01112   -0.00276    0.00071   -0.00005
O1    5    0.164939    0.855434    0.857950    11.00000    0.00959    0.01102 =
         0.01364    0.00067   -0.00268   -0.00035
C4    1    0.426576    0.627977    0.803224    11.00000    0.01201    0.01024 =
         0.01222   -0.00077   -0.00247   -0.00131
AFIX  23
H4A   2    0.460376    0.511052    0.844646    11.00000   -1.20000
H4B   2    0.387526    0.627668    0.689473    11.00000   -1.20000
AFIX   0
C6    1    0.767551    0.681693    0.495576    11.00000    0.00991    0.00884 =
         0.01248   -0.00022    0.00089    0.00231
AFIX  23
H6A   2    0.887610    0.622205    0.439270    11.00000   -1.20000
H6B   2    0.646540    0.619737    0.482980    11.00000   -1.20000
AFIX   0
C1    1    0.210283    1.157659    0.785466    11.00000    0.00947    0.01322 =
         0.00964   -0.00483    0.00150    0.00086
AFIX  23
H1A   2    0.064775    1.181890    0.821863    11.00000   -1.20000
H1B   2    0.286636    1.254160    0.807857    11.00000   -1.20000
AFIX   0
C3    1    0.249175    0.697092    0.925104    11.00000    0.01128    0.01147 =
         0.01213    0.00220    0.00094   -0.00174
AFIX  23
H3B   2    0.141059    0.613141    0.950336    11.00000   -1.20000
H3A   2    0.296687    0.712972    1.032824    11.00000   -1.20000
AFIX   0
C2    1    0.273685    1.000179    0.892823    11.00000    0.00862    0.01445 =
         0.00904   -0.00236    0.00033   -0.00068
AFIX  23
H2A   2    0.421381    0.979716    0.865075    11.00000   -1.20000
H2B   2    0.241664    1.016772    1.014456    11.00000   -1.20000
AFIX   0
C5    1    0.782137    0.676033    0.687103    11.00000    0.00785    0.01417 =
         0.01313   -0.00051   -0.00159    0.00414
AFIX  23
H5A   2    0.814753    0.559098    0.729359    11.00000   -1.20000
H5B   2    0.896147    0.746266    0.700012    11.00000   -1.20000
AFIX   0
N1    4    0.245378    1.142925    0.595244    11.00000    0.00730    0.00866 =
         0.00841   -0.00134    0.00066    0.00113
AFIX  13
H1    2    0.125522    1.083115    0.572569    11.00000   -1.20000
AFIX   0
HKLF 4
 
REM  CF solution in P-1
REM R1 =  0.0242 for    1859 Fo > 4sig(Fo)  and  0.0264 for all    1929 data
REM     97 parameters refined using      0 restraints
 
END  
     
WGHT      0.0167      0.2810 

REM Highest difference peak  0.496,  deepest hole -0.954,  1-sigma level  0.132
Q1    1   0.2265  0.9257  0.8699  11.00000  0.05    0.50
Q2    1   0.1388  0.6546  0.9544  11.00000  0.05    0.41
Q3    1   0.3359  0.6513  0.8784  11.00000  0.05    0.41
Q4    1   0.3932  1.3327  0.8214  11.00000  0.05    0.41
Q5    1   0.2221  0.7797  0.8831  11.00000  0.05    0.41
Q6    1   0.2205  0.7011  1.0377  11.00000  0.05    0.40
Q7    1   0.5966  0.7308  0.8641  11.00000  0.05    0.38
Q8    1   0.0570  0.5120  0.9451  11.00000  0.05    0.37
Q9    1   0.0696  0.8564  0.8809  11.00000  0.05    0.37
Q10   1   0.1002  0.5217  1.0759  11.00000  0.05    0.37
Q11   1   0.2051  1.0781  0.8431  11.00000  0.05    0.37
Q12   1   0.7328  0.6052  0.9514  11.00000  0.05    0.37
Q13   1   0.8416  0.5011  0.7170  11.00000  0.05    0.36
Q14   1   0.0186  0.6391  0.9344  11.00000  0.05    0.36
Q15   1   0.2016  0.4827  0.9772  11.00000  0.05    0.36
Q16   1   0.2313  1.2934  0.8966  11.00000  0.05    0.35
Q17   1   0.1371  1.3622  0.9785  11.00000  0.05    0.35
Q18   1   0.7370  0.5208  0.8160  11.00000  0.05    0.35
Q19   1   0.4011  0.5818  1.0226  11.00000  0.05    0.35
Q20   1   0.3276  0.9134  0.4139  11.00000  0.05    0.34
Q21   1   0.4677  0.6635  1.1186  11.00000  0.05    0.34
Q22   1   0.8282  0.7772  0.8557  11.00000  0.05    0.34
Q23   1   0.2315  0.5624  0.7457  11.00000  0.05    0.34
Q24   1   0.3722  0.5438  0.7047  11.00000  0.05    0.34
Q25   1   0.2665  0.5147  0.8815  11.00000  0.05    0.34

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0242 for 1859 Fo > 4sig(Fo) and 0.0264 for all 8570 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 0.50, deepest hole -0.95
  REM Mean Shift 0, Max Shift 0.000.
  
  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0264
  REM R1_gt = 0.0242
  REM wR_ref = 0.0508
  REM GOOF = 1.080
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 8570
  REM Reflections_gt = 1859
  REM Parameters = n/a
  REM Hole = -0.95
  REM Peak = 0.50
  REM Flack = n/a
  
  
;
_olex2_date_sample_data_collection 2015-12-09
_olex2_submission_special_instructions 'No special instructions were received'
