Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Geoffrey Coates' 'Stephen Lee' 'Emil Lobkovsky' 'Zengquan Qin.' 'Nicholas J Robertson' _publ_contact_author_name 'Dr Geoffrey Coates' _publ_contact_author_address ; Department of Chemistry and Chemical Biology Cornell University Baker Laboratory Ithaca NY 14853-1301 UNITED STATES OF AMERICA ; _publ_contact_author_email GC39@CORNELL.EDU _publ_section_title ; Two-Dimensional Double Metal Cyanide Complexes: Highly Active Catalysts for the Copolymerization of Propylene Oxide and Carbon Dioxide ; # Attachment '06May30 PdCo.cif' data_PdCo _database_code_depnum_ccdc_archive 'CCDC 609905' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H6 Co0.50 N2 O3 Pd0.50' _chemical_formula_weight 188.75 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' Co Co 0.3494 0.9721 '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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 12.041(2) _cell_length_b 14.217(3) _cell_length_c 7.4030(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1267.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink-orange _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 2.745 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8311 _exptl_absorpt_correction_T_max 0.9810 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.93600 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Cornell High Energy Synchrotron Source' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ; ADSC (Area Detector Systems Corporation) Quantum 210 CCD ; _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 721 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 30.09 _reflns_number_total 721 _reflns_number_gt 651 _reflns_threshold_expression >2sigma(I) _computing_data_collection HKL2000 _computing_cell_refinement HKL2000 _computing_data_reduction HKL2000 _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^)+(0.1172P)^2^+3.2729P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 721 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1651 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.428 _refine_ls_shift/su_mean 0.060 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 0.43531(4) 0.7500 0.99069(6) 0.0111(2) Uani 1 2 d S . . Co1 Co 0.5000 0.5000 0.5000 0.0136(3) Uani 1 2 d S . . O1 O 0.6867(4) 0.7500 0.4263(7) 0.0301(14) Uani 1 2 d S . . O2 O 0.1810(2) 0.5691(2) 0.5585(5) 0.0232(9) Uani 1 1 d . . . O3 O 0.6601(3) 0.5605(2) 0.5591(5) 0.0203(9) Uani 1 1 d . . . O4 O 0.2479(4) 0.2500 -0.0499(7) 0.0269(14) Uani 1 2 d S . . N1 N 0.5285(3) 0.4032(3) 0.7113(5) 0.0185(11) Uani 1 1 d . . . N2 N 0.4334(3) 0.5945(3) 0.6926(6) 0.0176(12) Uani 1 1 d . . . C1 C 0.4292(3) 0.6517(3) 0.8010(7) 0.0109(13) Uani 1 1 d . . . C2 C 0.4556(4) 0.6522(3) 1.1787(7) 0.0147(14) Uani 1 1 d . . . 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 0.0071(4) 0.0158(4) 0.0105(4) 0.000 -0.00008(18) 0.000 Co1 0.0087(6) 0.0199(7) 0.0122(7) -0.0004(4) -0.0004(3) 0.0003(5) O1 0.020(3) 0.041(3) 0.030(3) 0.000 -0.004(3) 0.000 O2 0.0137(18) 0.030(2) 0.0265(19) -0.0014(18) 0.0000(18) 0.0020(16) O3 0.0140(16) 0.026(2) 0.0206(18) -0.0004(18) -0.0050(17) -0.0019(16) O4 0.027(3) 0.025(3) 0.029(3) 0.000 0.000(3) 0.000 N1 0.0164(19) 0.019(2) 0.020(3) -0.007(2) 0.0042(19) -0.0004(19) N2 0.014(2) 0.014(2) 0.025(3) 0.000(2) -0.0029(18) -0.0021(17) C1 0.011(2) 0.005(3) 0.017(3) -0.002(3) -0.003(2) -0.005(2) C2 0.014(2) 0.009(3) 0.020(3) -0.007(3) 0.003(2) 0.004(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 Pd1 C1 1.983(5) . ? Pd1 C1 1.983(5) 7_575 ? Pd1 C2 1.983(5) 7_575 ? Pd1 C2 1.983(5) . ? Co1 N2 2.117(4) . ? Co1 N2 2.117(4) 5_666 ? Co1 N1 2.111(4) 5_666 ? Co1 N1 2.111(4) . ? Co1 O3 2.156(3) 5_666 ? Co1 O3 2.156(3) . ? N1 C2 1.149(6) 5_667 ? N2 C1 1.143(6) . ? C2 N1 1.149(6) 5_667 ? 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 C1 89.6(3) . 7_575 ? C1 Pd1 C2 175.06(18) . 7_575 ? C1 Pd1 C2 90.4(2) 7_575 7_575 ? C1 Pd1 C2 90.4(2) . . ? C1 Pd1 C2 175.06(18) 7_575 . ? C2 Pd1 C2 89.1(3) 7_575 . ? N2 Co1 N2 180.0 . 5_666 ? N2 Co1 N1 91.36(16) . 5_666 ? N2 Co1 N1 88.64(16) 5_666 5_666 ? N2 Co1 N1 88.64(16) . . ? N2 Co1 N1 91.36(16) 5_666 . ? N1 Co1 N1 180.0 5_666 . ? N2 Co1 O3 92.94(13) . 5_666 ? N2 Co1 O3 87.06(13) 5_666 5_666 ? N1 Co1 O3 87.96(13) 5_666 5_666 ? N1 Co1 O3 92.05(13) . 5_666 ? N2 Co1 O3 87.06(13) . . ? N2 Co1 O3 92.94(13) 5_666 . ? N1 Co1 O3 92.05(13) 5_666 . ? N1 Co1 O3 87.95(13) . . ? O3 Co1 O3 180.0 5_666 . ? C2 N1 Co1 177.3(4) 5_667 . ? C1 N2 Co1 160.2(3) . . ? N2 C1 Pd1 175.3(4) . . ? N1 C2 Pd1 177.3(4) 5_667 . ? _diffrn_measured_fraction_theta_max 0.843 _diffrn_reflns_theta_full 30.09 _diffrn_measured_fraction_theta_full 0.843 _refine_diff_density_max 1.608 _refine_diff_density_min -1.543 _refine_diff_density_rms 0.210