# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Rob Gossage'
_publ_contact_author_email       ROB.GOSSAGE@ACADIAU.CA

_publ_section_title              
;
Pre-Catalyst Resting States: A Kinetic, Thermodynamic
and Quantum Mechanical Analyses of [PdCl2(2-oxazoline)2] Complexes
;
loop_
_publ_author_name
'Rob Gossage'
'Hilary A. Jenkins'
'Nathan Jones'
'Roderick C Jones'
'Brian Yates'

# Attachment 'Gossage_Cmpd_4.cif'

data_rg2m
_database_code_depnum_ccdc_archive 'CCDC 657356'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H14 Cl2 N2 O2 Pd'
_chemical_formula_weight         347.51

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'
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           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5416(8)
_cell_length_b                   8.4479(9)
_cell_length_c                   9.6688(10)
_cell_angle_alpha                84.997(2)
_cell_angle_beta                 81.775(2)
_cell_angle_gamma                85.269(2)
_cell_volume                     605.81(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          .1
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .4
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             344
_exptl_absorpt_coefficient_mu    1.955
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      223(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            3184
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         24.98
_reflns_number_total             2095
_reflns_number_gt                1862
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^ > 2sigma(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^)+(0.0604P)^2^+0.0649P] 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    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0047(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         2095
_refine_ls_number_parameters     140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0813
_refine_ls_wR_factor_gt          0.0798
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.007
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5000 0.0000 0.0000 0.02258(15) Uani 1 2 d S . .
Cl1 Cl 0.21591(10) 0.12481(9) 0.03350(9) 0.0380(2) Uani 1 1 d . . .
O1 O 0.3222(3) -0.4408(3) 0.1632(2) 0.0387(5) Uani 1 1 d . . .
N1 N 0.3925(3) -0.2107(3) 0.0493(2) 0.0256(5) Uani 1 1 d . . .
C1 C 0.2839(4) -0.2789(4) -0.0426(3) 0.0350(7) Uani 1 1 d . . .
H1A H 0.3546 -0.2994 -0.1332 0.042 Uiso 1 1 calc R . .
H1B H 0.1780 -0.2079 -0.0582 0.042 Uiso 1 1 calc R . .
C2 C 0.2300(4) -0.4341(4) 0.0397(4) 0.0366(7) Uani 1 1 d . . .
H2A H 0.0996 -0.4322 0.0664 0.044 Uiso 1 1 calc R . .
H2B H 0.2695 -0.5257 -0.0155 0.044 Uiso 1 1 calc R . .
C3 C 0.4043(4) -0.3049(4) 0.1567(3) 0.0294(7) Uani 1 1 d . . .
C4 C 0.4972(5) -0.2829(4) 0.2788(4) 0.0410(8) Uani 1 1 d . . .
H4A H 0.5517 -0.1816 0.2645 0.062 Uiso 1 1 calc R . .
H4B H 0.5896 -0.3686 0.2881 0.062 Uiso 1 1 calc R . .
H4C H 0.4108 -0.2841 0.3634 0.062 Uiso 1 1 calc R . .
Pd2 Pd 1.0000 -0.5000 0.5000 0.02485(15) Uani 1 2 d S . .
Cl2 Cl 1.15325(15) -0.40656(10) 0.66017(11) 0.0566(3) Uani 1 1 d . . .
O2 O 1.2500(3) -0.9589(2) 0.5519(2) 0.0350(5) Uani 1 1 d . . .
N2 N 1.0914(3) -0.7259(3) 0.5544(3) 0.0286(5) Uani 1 1 d . . .
C5 C 0.9981(5) -0.8239(4) 0.6716(4) 0.0412(8) Uani 1 1 d . . .
H5A H 0.8768 -0.8421 0.6542 0.049 Uiso 1 1 calc R . .
H5B H 0.9900 -0.7730 0.7597 0.049 Uiso 1 1 calc R . .
C6 C 1.1140(5) -0.9775(4) 0.6758(3) 0.0375(7) Uani 1 1 d . . .
H6A H 1.1701 -0.9926 0.7619 0.045 Uiso 1 1 calc R . .
H6B H 1.0435 -1.0686 0.6705 0.045 Uiso 1 1 calc R . .
C7 C 1.2245(4) -0.8097(3) 0.4959(3) 0.0289(7) Uani 1 1 d . . .
C8 C 1.3546(5) -0.7629(4) 0.3730(4) 0.0452(9) Uani 1 1 d . . .
H8A H 1.3243 -0.6537 0.3396 0.068 Uiso 1 1 calc R . .
H8B H 1.3503 -0.8327 0.2991 0.068 Uiso 1 1 calc R . .
H8C H 1.4746 -0.7715 0.3993 0.068 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 0.0237(2) 0.0202(2) 0.0242(2) 0.00122(13) -0.00341(13) -0.00648(13)
Cl1 0.0279(4) 0.0322(4) 0.0526(5) -0.0029(3) -0.0011(3) -0.0022(3)
O1 0.0432(13) 0.0290(12) 0.0445(13) 0.0117(10) -0.0098(11) -0.0142(10)
N1 0.0268(13) 0.0242(12) 0.0262(13) 0.0009(10) -0.0041(10) -0.0065(10)
C1 0.0400(18) 0.0338(17) 0.0347(18) -0.0019(13) -0.0103(14) -0.0140(14)
C2 0.0370(18) 0.0307(17) 0.044(2) -0.0050(14) -0.0044(14) -0.0123(14)
C3 0.0255(15) 0.0262(16) 0.0355(17) -0.0003(13) -0.0020(13) -0.0018(12)
C4 0.0424(19) 0.045(2) 0.038(2) 0.0085(16) -0.0177(15) -0.0053(15)
Pd2 0.0285(2) 0.0173(2) 0.0292(2) -0.00172(13) -0.00733(14) 0.00139(13)
Cl2 0.0782(7) 0.0303(5) 0.0734(7) -0.0144(4) -0.0511(6) 0.0074(4)
O2 0.0417(12) 0.0215(11) 0.0371(13) 0.0043(9) 0.0015(10) 0.0060(9)
N2 0.0332(14) 0.0224(12) 0.0305(13) -0.0002(10) -0.0067(11) -0.0013(10)
C5 0.045(2) 0.0340(18) 0.038(2) 0.0022(15) 0.0093(16) 0.0022(16)
C6 0.0470(19) 0.0268(16) 0.0359(18) 0.0050(13) 0.0009(15) -0.0052(14)
C7 0.0344(16) 0.0233(15) 0.0299(16) -0.0007(12) -0.0091(13) 0.0000(12)
C8 0.049(2) 0.042(2) 0.038(2) 0.0072(15) 0.0061(16) 0.0003(16)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 2.008(2) 2_655 ?
Pd1 N1 2.008(2) . ?
Pd1 Cl1 2.3011(8) . ?
Pd1 Cl1 2.3011(8) 2_655 ?
O1 C3 1.341(4) . ?
O1 C2 1.460(4) . ?
N1 C3 1.261(4) . ?
N1 C1 1.472(4) . ?
C1 C2 1.526(4) . ?
C3 C4 1.489(4) . ?
Pd2 N2 2.026(2) 2_746 ?
Pd2 N2 2.026(2) . ?
Pd2 Cl2 2.2876(8) 2_746 ?
Pd2 Cl2 2.2876(8) . ?
O2 C7 1.338(3) . ?
O2 C6 1.468(4) . ?
N2 C7 1.272(4) . ?
N2 C5 1.473(4) . ?
C5 C6 1.504(4) . ?
C7 C8 1.477(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
N1 Pd1 N1 180.00(6) 2_655 . ?
N1 Pd1 Cl1 90.85(7) 2_655 . ?
N1 Pd1 Cl1 89.15(7) . . ?
N1 Pd1 Cl1 89.15(7) 2_655 2_655 ?
N1 Pd1 Cl1 90.85(7) . 2_655 ?
Cl1 Pd1 Cl1 180.00(4) . 2_655 ?
C3 O1 C2 107.0(2) . . ?
C3 N1 C1 109.2(2) . . ?
C3 N1 Pd1 128.3(2) . . ?
C1 N1 Pd1 122.46(18) . . ?
N1 C1 C2 103.1(2) . . ?
O1 C2 C1 104.0(2) . . ?
N1 C3 O1 116.6(3) . . ?
N1 C3 C4 127.8(3) . . ?
O1 C3 C4 115.7(3) . . ?
N2 Pd2 N2 180.00(14) 2_746 . ?
N2 Pd2 Cl2 90.18(7) 2_746 2_746 ?
N2 Pd2 Cl2 89.82(7) . 2_746 ?
N2 Pd2 Cl2 89.82(7) 2_746 . ?
N2 Pd2 Cl2 90.18(7) . . ?
Cl2 Pd2 Cl2 180.00(3) 2_746 . ?
C7 O2 C6 106.8(2) . . ?
C7 N2 C5 108.6(3) . . ?
C7 N2 Pd2 129.2(2) . . ?
C5 N2 Pd2 122.2(2) . . ?
N2 C5 C6 103.8(3) . . ?
O2 C6 C5 104.1(2) . . ?
N2 C7 O2 116.3(3) . . ?
N2 C7 C8 128.0(3) . . ?
O2 C7 C8 115.7(3) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.102