# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Partha Mukherjee'
_publ_contact_author_email       PSM@IPC.IISC.ERNET.IN

_publ_section_title              
;
Self-assembly of a PdII neutral molecular rectangle
via a new organometallic PdII2 molecular clip and oxygen donor linker
;
loop_
_publ_author_name
'Partha Mukherjee'
'Arun Kumar Bar'
'Bappaditya Gole'

# Attachment 'bs4-final_cif.cif'

data_bs4_m
_database_code_depnum_ccdc_archive 'CCDC 732627'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
'1,8-bis[{trans-bis(triethylphosphino)ethynylchloro}palladium(II)]anthracene'
;
_chemical_name_common            
;'1,8-bis((trans-
bis(triethylphosphino)ethynylchloro)palladium(ii))anthracene'
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H68 Cl2 P4 Pd2'
_chemical_formula_sum            'C42 H68 Cl2 P4 Pd2'
_chemical_formula_weight         980.54

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'
P P 0.1023 0.0942 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_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                   26.723(3)
_cell_length_b                   12.9521(16)
_cell_length_c                   14.0694(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.178(3)
_cell_angle_gamma                90.00
_cell_volume                     4793.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    792
_cell_measurement_theta_min      1.8
_cell_measurement_theta_max      26.4

_exptl_crystal_description       needles
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2024
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7099
_exptl_absorpt_correction_T_max  0.8618
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
'none'
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18892
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         26.37
_reflns_number_total             4916
_reflns_number_gt                2721
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows(Farrugia, 1997)'
_computing_publication_material  WinGX

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.9125P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4916
_refine_ls_number_parameters     233
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1507
_refine_ls_wR_factor_gt          0.1242
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.619968(16) 0.74493(3) 0.82734(3) 0.0591(2) Uani 1 1 d . . .
Cl1 Cl 0.64627(8) 0.91507(12) 0.86749(14) 0.0975(6) Uani 1 1 d . . .
P1 P 0.68298(7) 0.73175(13) 0.73408(14) 0.0751(5) Uani 1 1 d . . .
P2 P 0.56365(7) 0.74168(12) 0.93428(12) 0.0701(4) Uani 1 1 d D . .
C1 C 0.6032(2) 0.5993(5) 0.8061(4) 0.0623(15) Uani 1 1 d . . .
C2 C 0.5968(2) 0.5072(4) 0.8041(4) 0.0598(14) Uani 1 1 d . . .
C3 C 0.5934(2) 0.3970(4) 0.8059(4) 0.0615(15) Uani 1 1 d . . .
C4 C 0.6364(3) 0.3395(5) 0.8371(5) 0.087(2) Uani 1 1 d . . .
H4 H 0.6671 0.3734 0.8575 0.104 Uiso 1 1 calc R . .
C5 C 0.6355(3) 0.2304(6) 0.8391(6) 0.098(2) Uani 1 1 d . . .
H5 H 0.6654 0.1939 0.8598 0.118 Uiso 1 1 calc R . .
C6 C 0.5920(3) 0.1798(5) 0.8115(5) 0.089(2) Uani 1 1 d . . .
H6 H 0.5920 0.1080 0.8130 0.107 Uiso 1 1 calc R . .
C7 C 0.5453(3) 0.2332(4) 0.7795(5) 0.0684(17) Uani 1 1 d . . .
C8 C 0.5460(2) 0.3447(4) 0.7783(4) 0.0559(15) Uani 1 1 d . . .
C9 C 0.5000 0.1819(6) 0.7500 0.074(3) Uani 1 2 d S . .
H9 H 0.5000 0.1100 0.7500 0.089 Uiso 1 2 calc SR . .
C10 C 0.5000 0.3954(5) 0.7500 0.0525(19) Uani 1 2 d S . .
H10 H 0.5000 0.4672 0.7500 0.063 Uiso 1 2 calc SR . .
C11 C 0.6938(3) 0.8469(6) 0.6654(6) 0.115(3) Uani 1 1 d . . .
H11A H 0.7052 0.9025 0.7102 0.138 Uiso 1 1 calc R . .
H11B H 0.7208 0.8327 0.6293 0.138 Uiso 1 1 calc R . .
C12 C 0.6475(4) 0.8818(8) 0.5965(7) 0.164(4) Uani 1 1 d . . .
H12A H 0.6353 0.8265 0.5531 0.247 Uiso 1 1 calc R . .
H12B H 0.6560 0.9400 0.5603 0.247 Uiso 1 1 calc R . .
H12C H 0.6214 0.9012 0.6322 0.247 Uiso 1 1 calc R . .
C13 C 0.7433(3) 0.7174(7) 0.8152(6) 0.110(3) Uani 1 1 d . . .
H13A H 0.7703 0.7145 0.7772 0.132 Uiso 1 1 calc R . .
H13B H 0.7491 0.7780 0.8561 0.132 Uiso 1 1 calc R . .
C14 C 0.7466(3) 0.6240(8) 0.8776(7) 0.156(4) Uani 1 1 d . . .
H14A H 0.7228 0.6299 0.9210 0.235 Uiso 1 1 calc R . .
H14B H 0.7804 0.6180 0.9141 0.235 Uiso 1 1 calc R . .
H14C H 0.7388 0.5638 0.8379 0.235 Uiso 1 1 calc R . .
C15 C 0.6782(3) 0.6262(6) 0.6475(6) 0.098(2) Uani 1 1 d . . .
H15A H 0.6717 0.5634 0.6810 0.118 Uiso 1 1 calc R . .
H15B H 0.6485 0.6388 0.5984 0.118 Uiso 1 1 calc R . .
C16 C 0.7227(3) 0.6050(6) 0.5961(6) 0.125(3) Uani 1 1 d . . .
H16A H 0.7299 0.6658 0.5619 0.188 Uiso 1 1 calc R . .
H16B H 0.7141 0.5492 0.5512 0.188 Uiso 1 1 calc R . .
H16C H 0.7521 0.5866 0.6427 0.188 Uiso 1 1 calc R . .
C17 C 0.5404(5) 0.8647(7) 0.9685(8) 0.175(5) Uani 1 1 d . . .
H17A H 0.5192 0.8540 1.0170 0.211 Uiso 1 1 calc R . .
H17B H 0.5689 0.9077 0.9965 0.211 Uiso 1 1 calc R . .
C18 C 0.5103(6) 0.9184(9) 0.8836(11) 0.284(11) Uani 1 1 d . . .
H18A H 0.5088 0.9909 0.8971 0.427 Uiso 1 1 calc R . .
H18B H 0.4765 0.8906 0.8708 0.427 Uiso 1 1 calc R . .
H18C H 0.5262 0.9082 0.8282 0.427 Uiso 1 1 calc R . .
C19 C 0.5917(4) 0.6883(13) 1.0459(7) 0.232(7) Uani 1 1 d D . .
H19A H 0.5889 0.7416 1.0930 0.278 Uiso 1 1 calc R . .
H19B H 0.5687 0.6337 1.0578 0.278 Uiso 1 1 calc R . .
C20 C 0.6385(5) 0.6486(11) 1.0733(7) 0.213(6) Uani 1 1 d D . .
H20A H 0.6396 0.5801 1.0476 0.319 Uiso 1 1 calc R . .
H20B H 0.6465 0.6460 1.1425 0.319 Uiso 1 1 calc R . .
H20C H 0.6629 0.6914 1.0493 0.319 Uiso 1 1 calc R . .
C21 C 0.5069(3) 0.6642(6) 0.9013(6) 0.111(3) Uani 1 1 d . . .
H21A H 0.4877 0.6922 0.8419 0.133 Uiso 1 1 calc R . .
H21B H 0.5174 0.5951 0.8870 0.133 Uiso 1 1 calc R . .
C22 C 0.4714(3) 0.6553(7) 0.9732(6) 0.132(3) Uani 1 1 d . . .
H22A H 0.4897 0.6281 1.0329 0.198 Uiso 1 1 calc R . .
H22B H 0.4439 0.6099 0.9482 0.198 Uiso 1 1 calc R . .
H22C H 0.4582 0.7223 0.9843 0.198 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 0.0610(3) 0.0508(3) 0.0663(3) 0.0023(2) 0.0135(2) -0.0039(2)
Cl1 0.1161(15) 0.0555(9) 0.1222(15) -0.0080(9) 0.0249(12) -0.0122(10)
P1 0.0625(11) 0.0805(12) 0.0855(12) -0.0011(9) 0.0223(9) -0.0136(9)
P2 0.0754(11) 0.0727(11) 0.0647(10) -0.0002(8) 0.0190(8) 0.0030(9)
C1 0.059(4) 0.063(4) 0.068(4) -0.001(3) 0.020(3) 0.001(3)
C2 0.054(4) 0.057(4) 0.072(4) -0.002(3) 0.020(3) -0.001(3)
C3 0.058(4) 0.056(3) 0.076(4) 0.003(3) 0.026(3) 0.008(3)
C4 0.075(5) 0.084(5) 0.103(5) 0.008(4) 0.021(4) 0.008(4)
C5 0.093(6) 0.084(6) 0.123(7) 0.027(4) 0.036(5) 0.039(5)
C6 0.099(6) 0.047(4) 0.131(6) 0.017(4) 0.047(5) 0.024(4)
C7 0.088(5) 0.040(3) 0.085(4) 0.009(3) 0.037(4) 0.015(3)
C8 0.072(4) 0.038(3) 0.065(4) 0.007(2) 0.032(3) 0.006(3)
C9 0.089(7) 0.038(4) 0.105(7) 0.000 0.045(6) 0.000
C10 0.066(5) 0.030(3) 0.065(5) 0.000 0.021(4) 0.000
C11 0.130(7) 0.104(6) 0.125(7) 0.008(5) 0.061(6) -0.033(5)
C12 0.207(12) 0.162(9) 0.128(8) 0.054(7) 0.037(8) -0.008(9)
C13 0.074(5) 0.133(7) 0.123(7) -0.002(5) 0.016(5) -0.007(5)
C14 0.098(7) 0.186(10) 0.181(10) 0.044(8) 0.013(7) 0.035(7)
C15 0.086(5) 0.102(5) 0.117(6) -0.022(5) 0.049(5) -0.016(4)
C16 0.110(7) 0.147(8) 0.132(7) -0.026(6) 0.059(6) -0.008(6)
C17 0.250(13) 0.096(6) 0.230(12) -0.055(7) 0.177(11) -0.033(8)
C18 0.34(2) 0.153(11) 0.43(3) 0.145(14) 0.265(19) 0.144(13)
C19 0.116(9) 0.50(2) 0.086(7) 0.102(11) 0.034(6) 0.061(12)
C20 0.199(12) 0.327(18) 0.116(9) 0.078(9) 0.038(9) 0.105(13)
C21 0.100(6) 0.126(7) 0.119(6) -0.027(5) 0.050(5) -0.024(5)
C22 0.094(6) 0.178(9) 0.140(7) -0.003(6) 0.065(6) -0.015(6)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 1.949(6) . ?
Pd1 P2 2.3089(17) . ?
Pd1 P1 2.3167(18) . ?
Pd1 Cl1 2.3514(16) . ?
P1 C13 1.813(8) . ?
P1 C15 1.821(7) . ?
P1 C11 1.828(7) . ?
P2 C19 1.758(9) . ?
P2 C17 1.807(9) . ?
P2 C21 1.809(7) . ?
C1 C2 1.205(7) . ?
C2 C3 1.430(7) . ?
C3 C4 1.375(8) . ?
C3 C8 1.429(8) . ?
C4 C5 1.413(9) . ?
C5 C6 1.330(10) . ?
C6 C7 1.428(9) . ?
C7 C9 1.380(7) . ?
C7 C8 1.443(6) . ?
C8 C10 1.389(6) . ?
C9 C7 1.380(7) 2_656 ?
C10 C8 1.389(6) 2_656 ?
C11 C12 1.501(11) . ?
C13 C14 1.488(10) . ?
C15 C16 1.522(8) . ?
C17 C18 1.489(17) . ?
C19 C20 1.345(11) . ?
C21 C22 1.508(9) . ?

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
C1 Pd1 P2 85.60(15) . . ?
C1 Pd1 P1 90.72(16) . . ?
P2 Pd1 P1 172.08(6) . . ?
C1 Pd1 Cl1 173.96(18) . . ?
P2 Pd1 Cl1 93.56(6) . . ?
P1 Pd1 Cl1 89.36(6) . . ?
C13 P1 C15 107.1(4) . . ?
C13 P1 C11 102.1(4) . . ?
C15 P1 C11 105.0(4) . . ?
C13 P1 Pd1 107.8(3) . . ?
C15 P1 Pd1 117.5(2) . . ?
C11 P1 Pd1 116.0(3) . . ?
C19 P2 C17 102.8(6) . . ?
C19 P2 C21 102.5(5) . . ?
C17 P2 C21 104.2(4) . . ?
C19 P2 Pd1 111.4(3) . . ?
C17 P2 Pd1 116.9(3) . . ?
C21 P2 Pd1 117.1(2) . . ?
C2 C1 Pd1 171.7(6) . . ?
C1 C2 C3 175.3(7) . . ?
C4 C3 C8 118.7(5) . . ?
C4 C3 C2 119.6(6) . . ?
C8 C3 C2 121.7(5) . . ?
C3 C4 C5 122.1(7) . . ?
C6 C5 C4 120.3(7) . . ?
C5 C6 C7 121.5(6) . . ?
C9 C7 C6 122.2(5) . . ?
C9 C7 C8 119.4(6) . . ?
C6 C7 C8 118.4(6) . . ?
C10 C8 C3 123.4(5) . . ?
C10 C8 C7 117.7(6) . . ?
C3 C8 C7 119.0(5) . . ?
C7 C9 C7 122.3(7) . 2_656 ?
C8 C10 C8 123.5(6) 2_656 . ?
C12 C11 P1 113.4(6) . . ?
C14 C13 P1 114.1(6) . . ?
C16 C15 P1 119.0(5) . . ?
C18 C17 P2 111.1(8) . . ?
C20 C19 P2 129.4(8) . . ?
C22 C21 P2 117.9(6) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.083

#===END