# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_NbO-Pd-1
_database_code_depnum_ccdc_archive 'CCDC 1482371'
_audit_update_record             
;
2016-05-28 deposited with the CCDC.
2016-08-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        NbO-Pd-1
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H6 Cl2 Cu2 N2 O10 Pd'
_chemical_formula_weight         642.57

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
N N 0.0061 0.0033 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_H-M_alt        'R -3 m :H'
_space_group_name_Hall           '-R 3 2"'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'

_cell_length_a                   18.899(6)
_cell_length_b                   18.899(6)
_cell_length_c                   31.690(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9802(7)
_cell_formula_units_Z            9
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    8699
_cell_measurement_theta_min      1.4
_cell_measurement_theta_max      26.6

_exptl_crystal_description       Cube
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.980
_exptl_crystal_F_000             2790
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.523
_shelx_estimated_absorpt_T_min   0.750
_shelx_estimated_absorpt_T_max   0.750
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.6889
_diffrn_radiation_type           ?
_diffrn_source                   Synchrotron
_diffrn_measurement_device       
;
CrystalLogic Kappa (3 circle)
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            32466
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.492
_diffrn_reflns_theta_max         26.573
_diffrn_reflns_theta_full        24.415
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             2722
_reflns_number_gt                2618
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2722
_refine_ls_number_parameters     83
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0877
_refine_ls_wR_factor_ref         0.2946
_refine_ls_wR_factor_gt          0.2933
_refine_ls_goodness_of_fit_ref   2.415
_refine_ls_restrained_S_all      2.415
_refine_ls_shift/su_max          0.000
_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
Cu1 Cu 0.47815(2) 0.52185(2) 0.03591(2) 0.0396(4) Uani 1 2 d S T P . .
Pd2 Pd 0.6667 0.8333 -0.1667 0.0701(5) Uani 1 4 d S T P . .
O1 O 0.5175(3) 0.6269(2) 0.00691(11) 0.0536(9) Uani 1 1 d . . . . .
O2 O 0.4452(3) 0.4097(2) 0.05272(12) 0.0586(10) Uani 1 1 d . . . . .
O3 O 0.4471(3) 0.5529(3) 0.0942(3) 0.120(3) Uani 1 2 d S T P . .
N1 N 0.6189(5) 0.8095(3) -0.1079(2) 0.069(2) Uani 1 2 d S T P . .
C1 C 0.6013(5) 0.7393(4) -0.0888(2) 0.0255(13) Uani 0.5 1 d . . P . .
H1 H 0.6121 0.7024 -0.1027 0.031 Uiso 1 1 calc R U . . .
C2 C 0.5457(3) 0.6404(3) -0.02920(18) 0.0499(11) Uani 1 1 d . . . . .
C3 C 0.5674(3) 0.7209(3) -0.04899(16) 0.0501(11) Uani 1 1 d . . . . .
C4 C 0.5507(5) 0.7753(2) -0.0289(2) 0.0506(15) Uani 1 2 d S T P . .
H4 H 0.5283 0.7642 -0.0019 0.061 Uiso 1 2 calc R U P . .
Cl1 Cl 0.5590(3) 0.8460(4) -0.19104(13) 0.1120(17) Uani 0.5 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.961(4) 22_665 ?
Cu1 O2 1.961(4) . ?
Cu1 O1 1.966(3) 22_665 ?
Cu1 O1 1.966(3) . ?
Cu1 O3 2.109(7) . ?
Cu1 Cu1 2.6883(17) 19_665 ?
Pd2 N1 2.019(7) . ?
Pd2 N1 2.019(7) 31_664 ?
Pd2 Cl1 2.298(5) 18_654 ?
Pd2 Cl1 2.298(5) . ?
Pd2 Cl1 2.298(5) 31_664 ?
Pd2 Cl1 2.298(5) 24_565 ?
O1 C2 1.234(6) . ?
O2 C2 1.281(6) 19_665 ?
N1 C1 1.339(6) . ?
N1 C1 1.339(6) 24_565 ?
C1 C3 1.379(8) . ?
C2 O2 1.282(6) 19_665 ?
C2 C3 1.501(6) . ?
C3 C4 1.376(6) . ?
C4 C3 1.376(6) 24_565 ?

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
O2 Cu1 O2 88.7(3) 22_665 . ?
O2 Cu1 O1 166.98(16) 22_665 22_665 ?
O2 Cu1 O1 90.22(19) . 22_665 ?
O2 Cu1 O1 90.22(19) 22_665 . ?
O2 Cu1 O1 166.98(16) . . ?
O1 Cu1 O1 87.9(2) 22_665 . ?
O2 Cu1 O3 94.7(3) 22_665 . ?
O2 Cu1 O3 94.7(3) . . ?
O1 Cu1 O3 98.4(3) 22_665 . ?
O1 Cu1 O3 98.4(3) . . ?
O2 Cu1 Cu1 82.99(11) 22_665 19_665 ?
O2 Cu1 Cu1 82.99(11) . 19_665 ?
O1 Cu1 Cu1 84.00(11) 22_665 19_665 ?
O1 Cu1 Cu1 84.00(11) . 19_665 ?
O3 Cu1 Cu1 176.7(3) . 19_665 ?
N1 Pd2 N1 180.0 . 31_664 ?
N1 Pd2 Cl1 89.3(2) . 18_654 ?
N1 Pd2 Cl1 90.7(2) 31_664 18_654 ?
N1 Pd2 Cl1 90.7(2) . . ?
N1 Pd2 Cl1 89.3(2) 31_664 . ?
Cl1 Pd2 Cl1 113.7(3) 18_654 . ?
N1 Pd2 Cl1 89.3(2) . 31_664 ?
N1 Pd2 Cl1 90.7(2) 31_664 31_664 ?
Cl1 Pd2 Cl1 66.3(3) 18_654 31_664 ?
Cl1 Pd2 Cl1 180.0 . 31_664 ?
N1 Pd2 Cl1 90.7(2) . 24_565 ?
N1 Pd2 Cl1 89.3(2) 31_664 24_565 ?
Cl1 Pd2 Cl1 180.0 18_654 24_565 ?
Cl1 Pd2 Cl1 66.3(3) . 24_565 ?
Cl1 Pd2 Cl1 113.7(3) 31_664 24_565 ?
C2 O1 Cu1 123.2(3) . . ?
C2 O2 Cu1 123.6(3) 19_665 . ?
C1 N1 C1 119.9(7) . 24_565 ?
C1 N1 Pd2 120.0(4) . . ?
C1 N1 Pd2 120.0(4) 24_565 . ?
N1 C1 C3 121.2(5) . . ?
O1 C2 O2 126.2(5) . 19_665 ?
O1 C2 C3 117.9(4) . . ?
O2 C2 C3 115.8(5) 19_665 . ?
C4 C3 C1 119.1(5) . . ?
C4 C3 C2 121.1(5) . . ?
C1 C3 C2 119.7(5) . . ?
C3 C4 C3 119.4(6) . 24_565 ?

_refine_diff_density_max         1.650
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.193

_shelxl_version_number           2013-4



