# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;Preparation and characterization of the first pyrazole-based remote N-heterocyclic carbene complexes of palladium(II) ; _publ_contact_author_name 'Han Vinh Huynh' _publ_contact_author_email CHMHHV@NUS.EDU.SG loop_ _publ_author_name 'Han Vinh Huynh' 'Yuan Han' # Attachment 'Complex4a.cif' data_Complex4a _database_code_depnum_ccdc_archive 'CCDC 625238' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34.50 H35 I2 N2 P Pd' _chemical_formula_weight 868.82 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' P P 0.1023 0.0942 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3123(4) _cell_length_b 16.8404(7) _cell_length_c 21.6379(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.719(1) _cell_angle_gamma 90.00 _cell_volume 3376.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2380 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 20.49 _exptl_crystal_description 'Thin Plate' _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 2.451 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.7254 _exptl_absorpt_correction_T_max 0.9526 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 19717 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5935 _reflns_number_gt 4800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0497P)^2^+8.3387P] 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 5935 _refine_ls_number_parameters 388 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.1548 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.253 _refine_ls_restrained_S_all 1.250 _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 0.82605(8) 0.32191(4) 0.76713(3) 0.0304(2) Uani 1 1 d . . . I1 I 0.89237(10) 0.41825(5) 0.86372(4) 0.0631(3) Uani 1 1 d . . . I2 I 0.69675(8) 0.21989(4) 0.83710(3) 0.0521(2) Uani 1 1 d . . . P1 P 0.9445(3) 0.40043(15) 0.70396(12) 0.0341(6) Uani 1 1 d . . . N1 N 0.7603(9) 0.1433(5) 0.6326(4) 0.041(2) Uani 1 1 d . . . N2 N 0.6360(9) 0.1849(5) 0.6195(4) 0.044(2) Uani 1 1 d . . . C1 C 0.7683(10) 0.2477(6) 0.6961(4) 0.035(2) Uani 1 1 d . . . C2 C 0.8429(11) 0.1821(6) 0.6783(4) 0.040(2) Uani 1 1 d . . . C3 C 0.6406(11) 0.2488(6) 0.6585(5) 0.042(3) Uani 1 1 d . . . C4 C 0.9896(11) 0.1520(7) 0.7014(5) 0.057(3) Uani 1 1 d . . . H4A H 0.9856 0.0956 0.7074 0.085 Uiso 1 1 calc R . . H4B H 1.0213 0.1773 0.7402 0.085 Uiso 1 1 calc R . . H4C H 1.0561 0.1639 0.6715 0.085 Uiso 1 1 calc R . . C5 C 0.5153(14) 0.3042(8) 0.6573(7) 0.083(5) Uani 1 1 d . . . H5A H 0.4645 0.3046 0.6164 0.125 Uiso 1 1 calc R . . H5B H 0.5493 0.3567 0.6679 0.125 Uiso 1 1 calc R . . H5C H 0.4515 0.2868 0.6868 0.125 Uiso 1 1 calc R . . C6 C 0.7911(13) 0.0705(6) 0.5982(5) 0.051(3) Uani 1 1 d . . . H6A H 0.7007 0.0459 0.5823 0.061 Uiso 1 1 calc R . . H6B H 0.8431 0.0333 0.6264 0.061 Uiso 1 1 calc R . . C7 C 0.8778(15) 0.0873(8) 0.5454(6) 0.075(4) Uani 1 1 d . . . H7A H 0.8186 0.1138 0.5129 0.112 Uiso 1 1 calc R . . H7B H 0.9126 0.0382 0.5299 0.112 Uiso 1 1 calc R . . H7C H 0.9583 0.1205 0.5595 0.112 Uiso 1 1 calc R . . C8 C 0.5259(11) 0.1615(6) 0.5722(5) 0.043(3) Uani 1 1 d . . . C9 C 0.5259(15) 0.1934(8) 0.5139(6) 0.071(4) Uani 1 1 d . . . H9 H 0.5976 0.2288 0.5049 0.085 Uiso 1 1 calc R . . C10 C 0.4183(18) 0.1720(10) 0.4690(6) 0.088(5) Uani 1 1 d . . . H10 H 0.4185 0.1929 0.4292 0.105 Uiso 1 1 calc R . . C11 C 0.3131(18) 0.1220(9) 0.4810(7) 0.086(5) Uani 1 1 d . . . H11 H 0.2409 0.1087 0.4499 0.103 Uiso 1 1 calc R . . C12 C 0.3116(14) 0.0904(9) 0.5388(8) 0.082(5) Uani 1 1 d . . . H12 H 0.2396 0.0548 0.5472 0.098 Uiso 1 1 calc R . . C13 C 0.4199(13) 0.1119(8) 0.5857(6) 0.065(4) Uani 1 1 d . . . H13 H 0.4184 0.0922 0.6258 0.078 Uiso 1 1 calc R . . C1A C 0.8628(12) 0.4973(6) 0.6857(5) 0.043(3) Uani 1 1 d . . . C2A C 0.9134(14) 0.5462(7) 0.6397(6) 0.062(3) Uani 1 1 d . . . H2A H 0.9875 0.5288 0.6172 0.074 Uiso 1 1 calc R . . C3A C 0.8529(17) 0.6189(8) 0.6283(7) 0.082(5) Uani 1 1 d . . . H3A H 0.8885 0.6521 0.5991 0.098 Uiso 1 1 calc R . . C4A C 0.7393(16) 0.6436(8) 0.6597(7) 0.077(4) Uani 1 1 d . . . H4A1 H 0.6981 0.6932 0.6515 0.092 Uiso 1 1 calc R . . C5A C 0.6879(14) 0.5956(7) 0.7023(7) 0.069(4) Uani 1 1 d . . . H5A1 H 0.6104 0.6124 0.7230 0.082 Uiso 1 1 calc R . . C6A C 0.7486(11) 0.5215(7) 0.7158(5) 0.051(3) Uani 1 1 d . . . H6A1 H 0.7118 0.4888 0.7451 0.061 Uiso 1 1 calc R . . C1B C 1.1312(10) 0.4191(6) 0.7367(4) 0.032(2) Uani 1 1 d . . . C2B C 1.2015(13) 0.3587(7) 0.7717(5) 0.053(3) Uani 1 1 d . . . H2B H 1.1518 0.3122 0.7788 0.064 Uiso 1 1 calc R . . C3B C 1.3417(12) 0.3663(8) 0.7957(5) 0.058(3) Uani 1 1 d . . . H3B H 1.3900 0.3237 0.8157 0.070 Uiso 1 1 calc R . . C4B C 1.4113(12) 0.4377(8) 0.7902(6) 0.061(3) Uani 1 1 d . . . H4B1 H 1.5051 0.4446 0.8084 0.074 Uiso 1 1 calc R . . C5B C 1.3415(13) 0.4986(8) 0.7576(7) 0.069(4) Uani 1 1 d . . . H5B1 H 1.3894 0.5464 0.7531 0.082 Uiso 1 1 calc R . . C6B C 1.2029(11) 0.4901(7) 0.7317(5) 0.049(3) Uani 1 1 d . . . H6B1 H 1.1564 0.5323 0.7105 0.059 Uiso 1 1 calc R . . C1C C 0.9679(12) 0.3611(6) 0.6264(5) 0.044(3) Uani 1 1 d . . . C2C C 1.0894(13) 0.3196(7) 0.6142(5) 0.054(3) Uani 1 1 d . . . H2C H 1.1663 0.3153 0.6450 0.065 Uiso 1 1 calc R . . C3C C 1.0990(19) 0.2845(8) 0.5577(7) 0.084(5) Uani 1 1 d . . . H3C H 1.1819 0.2567 0.5505 0.101 Uiso 1 1 calc R . . C4C C 0.989(2) 0.2901(9) 0.5126(7) 0.086(5) Uani 1 1 d . . . H4C1 H 0.9963 0.2654 0.4746 0.103 Uiso 1 1 calc R . . C5C C 0.8664(18) 0.3318(9) 0.5219(6) 0.081(4) Uani 1 1 d . . . H5C1 H 0.7916 0.3369 0.4903 0.097 Uiso 1 1 calc R . . C6C C 0.8568(13) 0.3658(7) 0.5789(5) 0.058(3) Uani 1 1 d . . . H6C H 0.7730 0.3930 0.5859 0.070 Uiso 1 1 calc R . . C1S C 0.500(3) 0.4310(17) 0.4685(13) 0.097(12) Uani 0.50 1 d PGU A -1 H1SA H 0.5190 0.3940 0.4384 0.116 Uiso 0.50 1 calc PR A -1 C2S C 0.393(3) 0.4164(18) 0.5073(17) 0.138(17) Uani 0.50 1 d PGU A -1 H2SA H 0.3399 0.3697 0.5032 0.165 Uiso 0.50 1 calc PR A -1 C3S C 0.365(3) 0.472(3) 0.5523(15) 0.14(2) Uani 0.50 1 d PGU A -1 H3SA H 0.2936 0.4620 0.5783 0.163 Uiso 0.50 1 calc PR A -1 C4S C 0.445(4) 0.542(2) 0.5585(13) 0.143(17) Uani 0.50 1 d PGU A -1 H4SA H 0.4264 0.5786 0.5886 0.172 Uiso 0.50 1 calc PR A -1 C5S C 0.552(4) 0.5562(16) 0.5196(17) 0.121(16) Uani 0.50 1 d PGU A -1 H5SA H 0.6055 0.6030 0.5238 0.145 Uiso 0.50 1 calc PR A -1 C6S C 0.580(3) 0.501(2) 0.4746(15) 0.116(13) Uani 0.50 1 d PGU A -1 C7S C 0.696(5) 0.505(2) 0.436(2) 0.16(2) Uani 0.50 1 d PU A -1 H7SA H 0.7463 0.5545 0.4429 0.236 Uiso 0.50 1 calc PR A -1 H7SB H 0.6577 0.5016 0.3931 0.236 Uiso 0.50 1 calc PR A -1 H7SC H 0.7614 0.4618 0.4456 0.236 Uiso 0.50 1 calc PR A -1 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 0.0311(4) 0.0326(4) 0.0271(4) -0.0036(3) 0.0008(3) -0.0033(3) I1 0.0843(6) 0.0661(5) 0.0398(5) -0.0199(4) 0.0109(4) -0.0287(5) I2 0.0594(5) 0.0490(4) 0.0486(5) 0.0066(3) 0.0100(4) -0.0143(4) P1 0.0357(14) 0.0366(14) 0.0303(14) 0.0020(11) 0.0042(11) -0.0005(12) N1 0.041(5) 0.030(4) 0.051(6) -0.011(4) -0.002(4) 0.003(4) N2 0.049(5) 0.032(4) 0.049(6) -0.023(4) -0.009(4) 0.003(4) C1 0.034(6) 0.038(5) 0.031(5) -0.015(4) -0.002(4) -0.004(5) C2 0.052(6) 0.036(5) 0.032(6) -0.002(4) 0.008(5) -0.010(5) C3 0.040(6) 0.048(6) 0.038(6) -0.013(5) 0.003(5) 0.010(5) C4 0.040(6) 0.064(8) 0.063(8) -0.010(6) -0.010(6) 0.011(6) C5 0.060(8) 0.102(11) 0.083(10) -0.049(9) -0.016(7) 0.037(8) C6 0.059(7) 0.040(6) 0.056(7) -0.010(5) 0.016(6) -0.002(6) C7 0.090(10) 0.065(9) 0.074(10) -0.028(7) 0.030(8) -0.002(8) C8 0.045(6) 0.045(6) 0.036(6) -0.015(5) -0.006(5) -0.006(5) C9 0.079(9) 0.073(9) 0.055(8) 0.011(7) -0.017(7) -0.026(7) C10 0.121(13) 0.102(12) 0.035(8) -0.006(7) -0.020(8) -0.030(11) C11 0.114(13) 0.070(9) 0.064(10) -0.016(8) -0.037(9) 0.000(9) C12 0.055(8) 0.083(10) 0.104(13) -0.017(9) -0.014(8) -0.016(8) C13 0.050(8) 0.081(9) 0.061(8) 0.006(7) -0.013(6) -0.003(7) C1A 0.049(7) 0.042(6) 0.039(6) 0.005(5) 0.005(5) 0.000(5) C2A 0.069(8) 0.059(8) 0.059(8) 0.015(6) 0.010(6) 0.005(7) C3A 0.093(11) 0.070(9) 0.079(11) 0.038(8) -0.006(9) 0.006(9) C4A 0.068(9) 0.056(8) 0.103(12) 0.010(8) -0.006(9) 0.027(8) C5A 0.054(8) 0.056(8) 0.097(11) 0.015(7) 0.009(7) 0.009(7) C6A 0.036(6) 0.056(7) 0.061(8) 0.010(6) 0.002(5) -0.004(6) C1B 0.028(5) 0.045(6) 0.023(5) -0.005(4) 0.001(4) -0.004(5) C2B 0.059(8) 0.056(7) 0.044(7) 0.009(6) 0.001(6) -0.002(6) C3B 0.040(7) 0.073(9) 0.059(8) 0.009(6) -0.007(6) 0.013(6) C4B 0.032(6) 0.088(10) 0.061(8) -0.016(7) -0.006(6) -0.017(7) C5B 0.050(8) 0.058(8) 0.100(11) 0.008(8) 0.017(7) -0.012(7) C6B 0.035(6) 0.054(7) 0.058(7) 0.009(6) 0.006(5) 0.002(5) C1C 0.045(6) 0.052(7) 0.038(6) 0.000(5) 0.017(5) -0.004(5) C2C 0.054(7) 0.061(7) 0.048(7) 0.006(6) 0.007(6) -0.012(6) C3C 0.108(13) 0.077(10) 0.076(11) -0.025(8) 0.048(10) -0.014(9) C4C 0.128(15) 0.091(12) 0.043(9) -0.015(8) 0.030(9) -0.046(11) C5C 0.099(12) 0.102(12) 0.040(8) -0.008(8) -0.006(8) -0.029(10) C6C 0.054(7) 0.073(8) 0.048(7) -0.002(6) 0.002(6) 0.000(7) C1S 0.078(17) 0.10(2) 0.11(2) -0.008(15) 0.027(16) -0.023(15) C2S 0.14(2) 0.15(2) 0.12(2) -0.010(18) 0.026(17) -0.033(17) C3S 0.13(3) 0.13(3) 0.14(3) 0.019(18) 0.014(18) 0.012(18) C4S 0.16(2) 0.14(2) 0.13(2) -0.018(18) 0.009(18) 0.021(18) C5S 0.12(2) 0.11(2) 0.13(2) -0.008(17) -0.006(17) -0.008(17) C6S 0.13(2) 0.095(18) 0.12(2) 0.022(16) 0.001(16) 0.008(16) C7S 0.20(5) 0.06(2) 0.24(5) 0.04(3) 0.17(4) 0.03(3) _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 2.012(8) . ? Pd1 P1 2.266(3) . ? Pd1 I2 2.6564(10) . ? Pd1 I1 2.6691(10) . ? P1 C1A 1.826(10) . ? P1 C1C 1.837(10) . ? P1 C1B 1.838(9) . ? N1 C2 1.358(12) . ? N1 N2 1.358(11) . ? N1 C6 1.477(12) . ? N2 C3 1.366(12) . ? N2 C8 1.430(11) . ? C1 C3 1.373(13) . ? C1 C2 1.381(13) . ? C2 C4 1.495(14) . ? C3 C5 1.491(14) . ? C6 C7 1.489(16) . ? C8 C13 1.346(16) . ? C8 C9 1.372(16) . ? C9 C10 1.372(16) . ? C10 C11 1.34(2) . ? C11 C12 1.36(2) . ? C12 C13 1.406(16) . ? C1A C6A 1.364(15) . ? C1A C2A 1.409(15) . ? C2A C3A 1.360(17) . ? C3A C4A 1.38(2) . ? C4A C5A 1.349(19) . ? C5A C6A 1.389(15) . ? C1B C6B 1.378(14) . ? C1B C2B 1.392(14) . ? C2B C3B 1.363(15) . ? C3B C4B 1.376(16) . ? C4B C5B 1.372(17) . ? C5B C6B 1.362(15) . ? C1C C2C 1.377(15) . ? C1C C6C 1.386(15) . ? C2C C3C 1.369(17) . ? C3C C4C 1.35(2) . ? C4C C5C 1.37(2) . ? C5C C6C 1.371(17) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C3S C4S 1.3900 . ? C4S C5S 1.3900 . ? C5S C6S 1.3900 . ? C6S C7S 1.43(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 C1 Pd1 P1 90.6(3) . . ? C1 Pd1 I2 86.1(3) . . ? P1 Pd1 I2 175.39(8) . . ? C1 Pd1 I1 177.5(3) . . ? P1 Pd1 I1 91.67(7) . . ? I2 Pd1 I1 91.69(3) . . ? C1A P1 C1C 102.1(5) . . ? C1A P1 C1B 106.8(5) . . ? C1C P1 C1B 102.7(5) . . ? C1A P1 Pd1 115.7(4) . . ? C1C P1 Pd1 116.7(3) . . ? C1B P1 Pd1 111.5(3) . . ? C2 N1 N2 108.3(8) . . ? C2 N1 C6 129.9(9) . . ? N2 N1 C6 121.7(8) . . ? N1 N2 C3 107.7(7) . . ? N1 N2 C8 122.9(8) . . ? C3 N2 C8 129.4(9) . . ? C3 C1 C2 106.0(8) . . ? C3 C1 Pd1 126.5(7) . . ? C2 C1 Pd1 127.4(7) . . ? N1 C2 C1 108.9(9) . . ? N1 C2 C4 120.9(9) . . ? C1 C2 C4 130.2(9) . . ? N2 C3 C1 109.1(9) . . ? N2 C3 C5 120.4(9) . . ? C1 C3 C5 130.4(9) . . ? N1 C6 C7 112.1(9) . . ? C13 C8 C9 120.7(10) . . ? C13 C8 N2 120.2(10) . . ? C9 C8 N2 119.0(10) . . ? C8 C9 C10 118.8(13) . . ? C11 C10 C9 121.6(14) . . ? C10 C11 C12 120.1(13) . . ? C11 C12 C13 119.4(14) . . ? C8 C13 C12 119.4(13) . . ? C6A C1A C2A 119.6(10) . . ? C6A C1A P1 119.5(8) . . ? C2A C1A P1 120.9(9) . . ? C3A C2A C1A 119.5(13) . . ? C2A C3A C4A 120.4(14) . . ? C5A C4A C3A 119.9(12) . . ? C4A C5A C6A 121.1(13) . . ? C1A C6A C5A 119.3(12) . . ? C6B C1B C2B 118.1(9) . . ? C6B C1B P1 124.4(7) . . ? C2B C1B P1 117.4(8) . . ? C3B C2B C1B 121.3(11) . . ? C2B C3B C4B 119.3(11) . . ? C5B C4B C3B 119.7(10) . . ? C6B C5B C4B 120.9(11) . . ? C5B C6B C1B 120.4(10) . . ? C2C C1C C6C 117.0(10) . . ? C2C C1C P1 122.2(8) . . ? C6C C1C P1 120.6(9) . . ? C3C C2C C1C 121.2(12) . . ? C4C C3C C2C 120.4(15) . . ? C3C C4C C5C 120.9(14) . . ? C6C C5C C4C 118.4(13) . . ? C5C C6C C1C 122.2(13) . . ? C2S C1S C6S 120.0 . . ? C1S C2S C3S 120.0 . . ? C2S C3S C4S 120.0 . . ? C3S C4S C5S 120.0 . . ? C6S C5S C4S 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S C7S 126(3) . . ? C1S C6S C7S 114(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.052 _refine_diff_density_min -0.996 _refine_diff_density_rms 0.144 # Attachment 'Complex4b.cif' data_Complex4b _database_code_depnum_ccdc_archive 'CCDC 625239' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26.50 H30 Cl I2 N2 P Pd' _chemical_formula_weight 803.14 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3019(5) _cell_length_b 16.8771(9) _cell_length_c 18.9728(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.530(1) _cell_angle_gamma 90.00 _cell_volume 2969.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5492 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.86 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 2.865 _exptl_absorpt_correction_type 'Sadabs, (Sheldrick 2001)' _exptl_absorpt_correction_T_min 0.4252 _exptl_absorpt_correction_T_max 0.7626 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 20857 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6797 _reflns_number_gt 5735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0695P)^2^+7.1996P] 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 6797 _refine_ls_number_parameters 320 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.168 _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 0.70279(5) 0.20224(3) 0.27764(2) 0.03449(14) Uani 1 1 d . . . I1 I 0.68393(6) 0.08837(3) 0.37439(3) 0.05688(17) Uani 1 1 d . . . I2 I 0.86519(6) 0.29401(3) 0.36445(3) 0.06458(19) Uani 1 1 d . . . P1 P 0.55096(17) 0.13402(9) 0.19960(8) 0.0340(3) Uani 1 1 d . . . N1 N 0.8197(6) 0.3452(4) 0.1132(3) 0.0515(15) Uani 1 1 d . B . N2 N 0.6978(7) 0.3844(4) 0.1276(3) 0.0511(14) Uani 1 1 d . B . C1 C 0.7296(7) 0.2837(4) 0.2036(4) 0.0401(14) Uani 1 1 d . . . C2 C 0.8397(7) 0.2860(4) 0.1592(4) 0.0445(15) Uani 1 1 d . . . C3 C 0.6425(8) 0.3476(4) 0.1825(4) 0.0449(15) Uani 1 1 d . . . C4 C 0.9657(9) 0.2321(6) 0.1576(5) 0.075(3) Uani 1 1 d . . . H4A H 0.9661 0.2084 0.1116 0.113 Uiso 1 1 calc R . . H4B H 0.9593 0.1913 0.1925 0.113 Uiso 1 1 calc R . . H4C H 1.0530 0.2617 0.1677 0.113 Uiso 1 1 calc R . . C5 C 0.5070(9) 0.3753(4) 0.2112(5) 0.064(2) Uani 1 1 d . . . H5A H 0.4986 0.4317 0.2056 0.095 Uiso 1 1 calc R . . H5B H 0.5088 0.3621 0.2605 0.095 Uiso 1 1 calc R . . H5C H 0.4259 0.3499 0.1861 0.095 Uiso 1 1 calc R . . C6 C 0.9071(10) 0.3669(6) 0.0562(5) 0.074(3) Uani 1 1 d . . . H6A' H 0.8474 0.3931 0.0190 0.088 Uiso 0.85 1 calc PR A 1 H6B' H 0.9473 0.3195 0.0365 0.088 Uiso 0.85 1 calc PR A 1 H6A H 0.9876 0.3313 0.0557 0.110 Uiso 0.15 1 calc PR A 2 H6B H 0.9417 0.4201 0.0633 0.110 Uiso 0.15 1 calc PR A 2 H6C H 0.8500 0.3636 0.0119 0.110 Uiso 0.15 1 calc PR A 2 C7 C 1.0274(16) 0.4213(9) 0.0829(9) 0.113(5) Uani 0.85 1 d P B 1 H7A H 0.9874 0.4698 0.0994 0.170 Uiso 0.85 1 calc PR B 1 H7B H 1.0874 0.4328 0.0453 0.170 Uiso 0.85 1 calc PR B 1 H7C H 1.0840 0.3962 0.1211 0.170 Uiso 0.85 1 calc PR B 1 C7A C 0.707(7) 0.532(2) 0.073(4) 0.09(2) Uani 0.15 1 d PDU C 2 H7A1 H 0.6938 0.5655 0.1127 0.138 Uiso 0.15 1 calc PR C 2 H7A2 H 0.6618 0.5558 0.0308 0.138 Uiso 0.15 1 calc PR C 2 H7A3 H 0.8083 0.5256 0.0678 0.138 Uiso 0.15 1 calc PR C 2 C8 C 0.6395(12) 0.4513(6) 0.0843(6) 0.088(3) Uani 1 1 d D . . H8A1 H 0.5466 0.4628 0.1019 0.105 Uiso 0.15 1 calc PR C 2 H8B1 H 0.6189 0.4296 0.0373 0.105 Uiso 0.15 1 calc PR C 2 H8A H 0.5532 0.4705 0.1031 0.131 Uiso 0.85 1 calc PR C 1 H8B H 0.6177 0.4339 0.0365 0.131 Uiso 0.85 1 calc PR C 1 H8C H 0.7097 0.4931 0.0852 0.131 Uiso 0.85 1 calc PR C 1 C1A C 0.6195(7) 0.0406(4) 0.1673(3) 0.0410(14) Uani 1 1 d . . . C2A C 0.5487(10) 0.0026(5) 0.1100(4) 0.061(2) Uani 1 1 d . . . H2A H 0.4665 0.0251 0.0872 0.073 Uiso 1 1 calc R . . C3A C 0.6006(12) -0.0700(5) 0.0863(5) 0.078(3) Uani 1 1 d . . . H3A H 0.5530 -0.0958 0.0479 0.093 Uiso 1 1 calc R . . C4A C 0.7224(12) -0.1025(5) 0.1203(5) 0.077(3) Uani 1 1 d . . . H4A1 H 0.7561 -0.1511 0.1053 0.092 Uiso 1 1 calc R . . C5A C 0.7935(9) -0.0650(5) 0.1750(5) 0.063(2) Uani 1 1 d . . . H5A1 H 0.8774 -0.0870 0.1967 0.076 Uiso 1 1 calc R . . C6A C 0.7423(8) 0.0064(4) 0.1994(4) 0.0494(16) Uani 1 1 d . . . H6A1 H 0.7914 0.0315 0.2377 0.059 Uiso 1 1 calc R . . C1B C 0.3808(7) 0.1132(4) 0.2374(4) 0.0407(14) Uani 1 1 d . . . C2B C 0.2934(8) 0.0489(5) 0.2197(4) 0.0568(19) Uani 1 1 d . . . H2B H 0.3218 0.0115 0.1876 0.068 Uiso 1 1 calc R . . C3B C 0.1642(9) 0.0402(6) 0.2496(6) 0.074(3) Uani 1 1 d . . . H3B H 0.1081 -0.0045 0.2387 0.089 Uiso 1 1 calc R . . C4B C 0.1174(9) 0.0944(7) 0.2940(5) 0.074(3) Uani 1 1 d . . . H4B1 H 0.0277 0.0885 0.3118 0.089 Uiso 1 1 calc R . . C5B C 0.2015(9) 0.1585(6) 0.3131(5) 0.066(2) Uani 1 1 d . . . H5B1 H 0.1696 0.1958 0.3444 0.079 Uiso 1 1 calc R . . C6B C 0.3336(8) 0.1680(5) 0.2858(4) 0.0510(17) Uani 1 1 d . . . H6B1 H 0.3916 0.2110 0.2998 0.061 Uiso 1 1 calc R . . C1C C 0.4946(7) 0.1837(4) 0.1167(3) 0.0380(13) Uani 1 1 d . . . C2C C 0.3586(8) 0.2163(5) 0.1031(4) 0.0548(18) Uani 1 1 d . . . H2C H 0.2892 0.2098 0.1353 0.066 Uiso 1 1 calc R . . C3C C 0.3263(10) 0.2590(6) 0.0411(5) 0.073(2) Uani 1 1 d . . . H3C H 0.2340 0.2796 0.0319 0.088 Uiso 1 1 calc R . . C4C C 0.4237(11) 0.2711(6) -0.0055(5) 0.070(2) Uani 1 1 d . . . H4C1 H 0.3997 0.3011 -0.0458 0.085 Uiso 1 1 calc R . . C5C C 0.5577(10) 0.2398(5) 0.0057(4) 0.060(2) Uani 1 1 d . . . H5C1 H 0.6262 0.2484 -0.0267 0.072 Uiso 1 1 calc R . . C6C C 0.5919(8) 0.1945(4) 0.0663(4) 0.0492(16) Uani 1 1 d . . . H6C1 H 0.6824 0.1711 0.0729 0.059 Uiso 1 1 calc R . . C1S C 0.085(5) 0.9704(18) 0.0034(18) 0.174(18) Uani 0.50 1 d P . . H1S1 H 0.1101 0.9294 0.0380 0.208 Uiso 0.50 1 calc PR . . H1S2 H 0.1632 0.9749 -0.0272 0.208 Uiso 0.50 1 calc PR . . Cl1 Cl 0.0668(11) 1.0563(5) 0.0453(4) 0.262(4) 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 0.0317(2) 0.0350(2) 0.0375(3) -0.00469(18) 0.00788(18) -0.00561(18) I1 0.0665(3) 0.0582(3) 0.0458(3) 0.0030(2) 0.0038(2) -0.0120(2) I2 0.0640(3) 0.0712(4) 0.0597(3) -0.0208(3) 0.0119(3) -0.0339(3) P1 0.0310(8) 0.0345(8) 0.0372(8) -0.0039(6) 0.0065(6) -0.0023(6) N1 0.042(3) 0.056(4) 0.059(4) 0.012(3) 0.015(3) 0.000(3) N2 0.049(3) 0.045(3) 0.061(4) 0.007(3) 0.014(3) 0.007(3) C1 0.037(3) 0.039(3) 0.045(4) -0.004(3) 0.008(3) -0.006(2) C2 0.033(3) 0.048(4) 0.054(4) 0.008(3) 0.012(3) 0.008(3) C3 0.045(4) 0.035(3) 0.056(4) -0.003(3) 0.014(3) 0.001(3) C4 0.050(5) 0.094(7) 0.086(6) 0.035(5) 0.029(5) 0.031(5) C5 0.063(5) 0.042(4) 0.091(6) -0.004(4) 0.034(5) 0.012(3) C6 0.071(6) 0.082(6) 0.071(6) 0.022(5) 0.024(5) 0.012(5) C7 0.098(11) 0.105(11) 0.141(14) 0.016(10) 0.041(10) -0.028(9) C7A 0.11(3) 0.09(3) 0.08(3) 0.00(2) 0.02(2) 0.03(2) C8 0.097(8) 0.062(6) 0.107(8) 0.032(5) 0.032(6) 0.033(5) C1A 0.043(4) 0.038(3) 0.043(3) -0.008(3) 0.007(3) 0.001(3) C2A 0.073(5) 0.049(4) 0.059(5) -0.011(4) -0.005(4) 0.003(4) C3A 0.109(8) 0.057(5) 0.066(5) -0.031(4) -0.001(5) 0.000(5) C4A 0.097(7) 0.047(5) 0.086(7) -0.024(4) 0.004(6) 0.018(5) C5A 0.056(5) 0.058(5) 0.076(6) -0.008(4) 0.011(4) 0.018(4) C6A 0.042(4) 0.047(4) 0.059(4) -0.008(3) 0.005(3) 0.003(3) C1B 0.032(3) 0.047(4) 0.044(3) 0.009(3) 0.005(3) -0.005(3) C2B 0.047(4) 0.057(5) 0.065(5) 0.003(4) -0.005(4) -0.012(3) C3B 0.045(5) 0.085(6) 0.093(7) 0.013(5) -0.001(5) -0.026(4) C4B 0.037(4) 0.109(8) 0.078(6) 0.026(6) 0.019(4) 0.001(5) C5B 0.051(5) 0.082(6) 0.067(5) 0.007(4) 0.019(4) 0.011(4) C6B 0.043(4) 0.058(4) 0.053(4) -0.005(3) 0.015(3) -0.005(3) C1C 0.040(3) 0.042(3) 0.033(3) -0.002(2) 0.004(3) -0.004(3) C2C 0.044(4) 0.065(5) 0.057(4) 0.013(4) 0.010(3) 0.007(3) C3C 0.060(5) 0.086(6) 0.073(6) 0.018(5) 0.006(5) 0.020(5) C4C 0.084(7) 0.076(6) 0.050(5) 0.016(4) -0.002(5) 0.002(5) C5C 0.087(6) 0.060(5) 0.035(4) -0.010(3) 0.012(4) -0.018(4) C6C 0.049(4) 0.058(4) 0.042(4) -0.009(3) 0.009(3) -0.001(3) C1S 0.29(5) 0.10(2) 0.12(2) 0.056(19) -0.05(3) -0.01(3) Cl1 0.378(12) 0.234(8) 0.171(6) -0.069(5) -0.003(7) -0.063(8) _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 1.996(7) . ? Pd1 P1 2.2765(16) . ? Pd1 I2 2.6458(7) . ? Pd1 I1 2.6730(7) . ? P1 C1C 1.823(6) . ? P1 C1B 1.823(6) . ? P1 C1A 1.825(6) . ? N1 C2 1.330(9) . ? N1 N2 1.359(8) . ? N1 C6 1.450(10) . ? N2 C3 1.348(9) . ? N2 C8 1.475(10) . ? C1 C2 1.377(9) . ? C1 C3 1.388(9) . ? C2 C4 1.486(10) . ? C3 C5 1.488(10) . ? C6 C7 1.504(17) . ? C7A C8 1.52(2) . ? C1A C6A 1.378(10) . ? C1A C2A 1.383(10) . ? C2A C3A 1.403(11) . ? C3A C4A 1.373(14) . ? C4A C5A 1.345(13) . ? C5A C6A 1.388(10) . ? C1B C2B 1.381(10) . ? C1B C6B 1.398(10) . ? C2B C3B 1.376(12) . ? C3B C4B 1.340(14) . ? C4B C5B 1.366(13) . ? C5B C6B 1.380(11) . ? C1C C6C 1.379(9) . ? C1C C2C 1.385(10) . ? C2C C3C 1.392(11) . ? C3C C4C 1.329(13) . ? C4C C5C 1.355(13) . ? C5C C6C 1.397(11) . ? C1S Cl1 1.67(4) . ? C1S Cl1 1.69(4) 3_575 ? Cl1 C1S 1.69(4) 3_575 ? 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 P1 89.79(19) . . ? C1 Pd1 I2 86.44(18) . . ? P1 Pd1 I2 174.46(5) . . ? C1 Pd1 I1 176.01(19) . . ? P1 Pd1 I1 90.69(4) . . ? I2 Pd1 I1 93.35(2) . . ? C1C P1 C1B 103.2(3) . . ? C1C P1 C1A 101.1(3) . . ? C1B P1 C1A 107.6(3) . . ? C1C P1 Pd1 116.7(2) . . ? C1B P1 Pd1 110.8(2) . . ? C1A P1 Pd1 116.1(2) . . ? C2 N1 N2 107.9(6) . . ? C2 N1 C6 128.4(7) . . ? N2 N1 C6 123.6(7) . . ? C3 N2 N1 107.9(6) . . ? C3 N2 C8 129.5(7) . . ? N1 N2 C8 122.4(7) . . ? C2 C1 C3 104.3(6) . . ? C2 C1 Pd1 126.1(5) . . ? C3 C1 Pd1 129.5(5) . . ? N1 C2 C1 110.5(6) . . ? N1 C2 C4 121.1(6) . . ? C1 C2 C4 128.4(6) . . ? N2 C3 C1 109.3(6) . . ? N2 C3 C5 121.7(7) . . ? C1 C3 C5 129.0(7) . . ? N1 C6 C7 110.5(9) . . ? N2 C8 C7A 129(3) . . ? C6A C1A C2A 118.7(6) . . ? C6A C1A P1 120.8(5) . . ? C2A C1A P1 120.5(6) . . ? C1A C2A C3A 120.2(8) . . ? C4A C3A C2A 119.4(8) . . ? C5A C4A C3A 120.7(8) . . ? C4A C5A C6A 120.4(8) . . ? C1A C6A C5A 120.7(7) . . ? C2B C1B C6B 118.0(7) . . ? C2B C1B P1 124.7(6) . . ? C6B C1B P1 117.3(5) . . ? C3B C2B C1B 120.0(8) . . ? C4B C3B C2B 121.6(9) . . ? C3B C4B C5B 120.0(8) . . ? C4B C5B C6B 120.0(8) . . ? C5B C6B C1B 120.3(7) . . ? C6C C1C C2C 117.3(6) . . ? C6C C1C P1 119.9(5) . . ? C2C C1C P1 122.7(5) . . ? C1C C2C C3C 119.7(7) . . ? C4C C3C C2C 121.9(8) . . ? C3C C4C C5C 120.2(8) . . ? C4C C5C C6C 119.2(8) . . ? C1C C6C C5C 121.6(7) . . ? Cl1 C1S Cl1 113(2) . 3_575 ? C1S Cl1 C1S 67(2) . 3_575 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.832 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.168