# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_agriw _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H64 Ag2 Cl2 N4 P4' _chemical_formula_weight 1107.55 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 8.8284(2) _cell_length_b 9.9359(2) _cell_length_c 15.5614(3) _cell_angle_alpha 107.197(2) _cell_angle_beta 105.744(2) _cell_angle_gamma 90.499(2) _cell_volume 1249.18(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 53853 _cell_measurement_theta_min 2.1826 _cell_measurement_theta_max 30.8018 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85071 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81562 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0123 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7153 _reflns_number_gt 6718 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0206P)^2^+0.4896P] 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 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7153 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0194 _refine_ls_R_factor_gt 0.0171 _refine_ls_wR_factor_ref 0.0442 _refine_ls_wR_factor_gt 0.0428 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Ag Ag 0.173857(9) 0.079597(9) 0.501607(6) 0.01814(3) Uani 1 1 d . . . Cl Cl -0.12336(3) 0.11679(3) 0.429944(18) 0.01820(5) Uani 1 1 d . . . N1 N 0.66760(10) 0.34399(9) 0.66714(6) 0.01437(16) Uani 1 1 d . . . C2 C 0.54117(13) 0.29863(11) 0.58993(7) 0.01650(19) Uani 1 1 d . . . H2 H 0.5500 0.2799 0.5281 0.020 Uiso 1 1 calc R . . P3 P 0.36421(3) 0.27746(3) 0.61206(2) 0.01812(6) Uani 1 1 d . . . C3A C 0.46515(13) 0.32336(11) 0.73328(8) 0.01657(19) Uani 1 1 d . . . C4 C 0.40664(15) 0.33041(12) 0.80995(9) 0.0229(2) Uani 1 1 d . . . H4 H 0.2972 0.3079 0.8001 0.027 Uiso 1 1 calc R . . C5 C 0.50906(17) 0.37012(13) 0.89944(9) 0.0271(3) Uani 1 1 d . . . H5 H 0.4700 0.3736 0.9512 0.032 Uiso 1 1 calc R . . C6 C 0.67038(17) 0.40544(13) 0.91479(8) 0.0255(2) Uani 1 1 d . . . H6 H 0.7389 0.4334 0.9771 0.031 Uiso 1 1 calc R . . C7 C 0.73179(14) 0.40039(12) 0.84122(8) 0.0202(2) Uani 1 1 d . . . H7 H 0.8412 0.4247 0.8522 0.024 Uiso 1 1 calc R . . C7A C 0.62814(13) 0.35834(11) 0.74993(7) 0.01519(19) Uani 1 1 d . . . C8 C 0.82828(12) 0.36669(11) 0.66040(8) 0.01593(19) Uani 1 1 d . . . H8A H 0.8396 0.2944 0.6036 0.019 Uiso 1 1 calc R . . H8B H 0.9048 0.3512 0.7155 0.019 Uiso 1 1 calc R . . C9 C 0.87279(12) 0.51391(11) 0.65566(8) 0.01698(19) Uani 1 1 d . . . C10 C 1.03653(14) 0.50895(14) 0.63967(9) 0.0252(2) Uani 1 1 d . . . H10A H 1.0321 0.4338 0.5815 0.038 Uiso 1 1 calc R . . H10B H 1.1127 0.4898 0.6926 0.038 Uiso 1 1 calc R . . H10C H 1.0696 0.6001 0.6347 0.038 Uiso 1 1 calc R . . C11 C 0.87805(14) 0.62950(12) 0.74717(9) 0.0216(2) Uani 1 1 d . . . H11A H 0.9016 0.7224 0.7413 0.032 Uiso 1 1 calc R . . H11B H 0.9605 0.6142 0.7991 0.032 Uiso 1 1 calc R . . H11C H 0.7754 0.6258 0.7597 0.032 Uiso 1 1 calc R . . C12 C 0.75578(14) 0.54580(13) 0.57289(9) 0.0230(2) Uani 1 1 d . . . H12A H 0.6507 0.5506 0.5828 0.035 Uiso 1 1 calc R . . H12B H 0.7508 0.4705 0.5146 0.035 Uiso 1 1 calc R . . H12C H 0.7911 0.6366 0.5684 0.035 Uiso 1 1 calc R . . N1' N 0.40163(10) 0.00383(9) 0.23292(6) 0.01423(16) Uani 1 1 d . . . C2' C 0.42442(12) 0.03360(11) 0.32698(7) 0.01517(18) Uani 1 1 d . . . H2' H 0.5240 0.0692 0.3720 0.018 Uiso 1 1 calc R . . P3' P 0.25882(3) 0.00145(3) 0.35721(2) 0.01677(6) Uani 1 1 d . . . C3A' C 0.14920(12) -0.05527(11) 0.23745(8) 0.01626(19) Uani 1 1 d . . . C4' C -0.01039(13) -0.10964(13) 0.19488(9) 0.0225(2) Uani 1 1 d . . . H4' H -0.0780 -0.1138 0.2324 0.027 Uiso 1 1 calc R . . C5' C -0.06762(14) -0.15667(14) 0.09866(10) 0.0274(3) Uani 1 1 d . . . H5' H -0.1748 -0.1946 0.0698 0.033 Uiso 1 1 calc R . . C6' C 0.03094(15) -0.14912(13) 0.04261(9) 0.0264(3) Uani 1 1 d . . . H6' H -0.0109 -0.1818 -0.0238 0.032 Uiso 1 1 calc R . . C7' C 0.18781(14) -0.09498(12) 0.08226(8) 0.0210(2) Uani 1 1 d . . . H7' H 0.2536 -0.0896 0.0439 0.025 Uiso 1 1 calc R . . C7A' C 0.24736(12) -0.04825(11) 0.18049(7) 0.01538(19) Uani 1 1 d . . . C8' C 0.53228(12) 0.02485(11) 0.19501(7) 0.01527(19) Uani 1 1 d . . . H8'1 H 0.5133 -0.0458 0.1322 0.018 Uiso 1 1 calc R . . H8'2 H 0.6314 0.0059 0.2361 0.018 Uiso 1 1 calc R . . C9' C 0.55607(12) 0.17373(11) 0.18600(7) 0.01551(19) Uani 1 1 d . . . C10' C 0.71209(14) 0.17885(13) 0.16102(9) 0.0239(2) Uani 1 1 d . . . H10D H 0.7298 0.2692 0.1502 0.036 Uiso 1 1 calc R . . H10E H 0.7068 0.1008 0.1040 0.036 Uiso 1 1 calc R . . H10F H 0.7994 0.1698 0.2129 0.036 Uiso 1 1 calc R . . C11' C 0.42125(15) 0.19854(13) 0.10823(8) 0.0226(2) Uani 1 1 d . . . H11D H 0.3205 0.1878 0.1218 0.034 Uiso 1 1 calc R . . H11E H 0.4185 0.1293 0.0479 0.034 Uiso 1 1 calc R . . H11F H 0.4384 0.2944 0.1052 0.034 Uiso 1 1 calc R . . C12' C 0.56941(13) 0.28842(11) 0.27926(8) 0.0177(2) Uani 1 1 d . . . H12D H 0.6565 0.2725 0.3287 0.026 Uiso 1 1 calc R . . H12E H 0.4703 0.2844 0.2958 0.026 Uiso 1 1 calc R . . H12F H 0.5899 0.3817 0.2730 0.026 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 Ag 0.01500(4) 0.01948(5) 0.01990(4) 0.00535(3) 0.00587(3) -0.00212(3) Cl 0.01389(11) 0.02179(13) 0.02110(12) 0.01142(10) 0.00332(9) 0.00143(9) N1 0.0138(4) 0.0142(4) 0.0149(4) 0.0042(3) 0.0041(3) 0.0002(3) C2 0.0176(5) 0.0154(5) 0.0155(5) 0.0046(4) 0.0034(4) -0.0013(4) P3 0.01492(12) 0.01752(13) 0.02039(13) 0.00508(10) 0.00358(10) -0.00234(10) C3A 0.0205(5) 0.0107(4) 0.0196(5) 0.0041(4) 0.0083(4) 0.0014(4) C4 0.0297(6) 0.0149(5) 0.0283(6) 0.0050(4) 0.0172(5) 0.0008(4) C5 0.0462(8) 0.0174(5) 0.0224(6) 0.0041(4) 0.0201(5) 0.0025(5) C6 0.0403(7) 0.0187(6) 0.0160(5) 0.0042(4) 0.0071(5) 0.0044(5) C7 0.0237(5) 0.0174(5) 0.0177(5) 0.0052(4) 0.0033(4) 0.0034(4) C7A 0.0199(5) 0.0109(4) 0.0155(5) 0.0041(4) 0.0064(4) 0.0026(4) C8 0.0131(4) 0.0146(5) 0.0203(5) 0.0045(4) 0.0062(4) 0.0022(4) C9 0.0139(4) 0.0153(5) 0.0219(5) 0.0046(4) 0.0067(4) 0.0007(4) C10 0.0175(5) 0.0249(6) 0.0342(6) 0.0055(5) 0.0129(5) -0.0004(4) C11 0.0194(5) 0.0162(5) 0.0269(6) 0.0021(4) 0.0077(4) 0.0003(4) C12 0.0230(5) 0.0221(6) 0.0265(6) 0.0121(5) 0.0062(4) 0.0007(4) N1' 0.0138(4) 0.0149(4) 0.0145(4) 0.0055(3) 0.0041(3) 0.0006(3) C2' 0.0151(4) 0.0151(5) 0.0157(5) 0.0053(4) 0.0044(4) 0.0010(4) P3' 0.01599(12) 0.01857(13) 0.01701(12) 0.00564(10) 0.00670(10) 0.00018(10) C3A' 0.0155(5) 0.0138(5) 0.0198(5) 0.0066(4) 0.0039(4) 0.0019(4) C4' 0.0154(5) 0.0204(5) 0.0326(6) 0.0116(5) 0.0045(4) 0.0009(4) C5' 0.0177(5) 0.0246(6) 0.0341(7) 0.0114(5) -0.0045(5) -0.0024(4) C6' 0.0274(6) 0.0232(6) 0.0214(5) 0.0078(5) -0.0054(4) -0.0022(5) C7' 0.0249(5) 0.0192(5) 0.0173(5) 0.0070(4) 0.0019(4) -0.0010(4) C7A' 0.0159(5) 0.0125(5) 0.0171(5) 0.0058(4) 0.0023(4) 0.0007(4) C8' 0.0159(4) 0.0148(5) 0.0171(5) 0.0050(4) 0.0078(4) 0.0025(4) C9' 0.0165(5) 0.0146(5) 0.0166(5) 0.0054(4) 0.0062(4) 0.0009(4) C10' 0.0237(6) 0.0241(6) 0.0279(6) 0.0074(5) 0.0147(5) -0.0002(4) C11' 0.0257(6) 0.0215(6) 0.0205(5) 0.0102(4) 0.0022(4) 0.0000(4) C12' 0.0181(5) 0.0142(5) 0.0199(5) 0.0043(4) 0.0053(4) 0.0015(4) _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 Ag P3 2.4537(3) . ? Ag P3' 2.4714(3) . ? Ag Cl 2.5715(3) 2_556 ? Ag Cl 2.6340(3) . ? Cl Ag 2.5714(3) 2_556 ? N1 C2 1.3549(13) . ? N1 C7A 1.3919(13) . ? N1 C8 1.4709(13) . ? C2 P3 1.7125(11) . ? P3 C3A 1.7699(11) . ? C3A C4 1.4074(15) . ? C3A C7A 1.4121(15) . ? C4 C5 1.3777(19) . ? C5 C6 1.402(2) . ? C6 C7 1.3822(17) . ? C7 C7A 1.4025(15) . ? C8 C9 1.5392(15) . ? C9 C10 1.5308(15) . ? C9 C11 1.5314(16) . ? C9 C12 1.5335(16) . ? N1' C2' 1.3614(13) . ? N1' C7A' 1.3869(13) . ? N1' C8' 1.4696(13) . ? C2' P3' 1.7072(11) . ? P3' C3A' 1.7658(11) . ? C3A' C4' 1.4087(15) . ? C3A' C7A' 1.4121(15) . ? C4' C5' 1.3737(18) . ? C5' C6' 1.405(2) . ? C6' C7' 1.3838(17) . ? C7' C7A' 1.4030(15) . ? C8' C9' 1.5445(15) . ? C9' C11' 1.5303(15) . ? C9' C12' 1.5315(15) . ? C9' C10' 1.5336(15) . ? 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 P3 Ag P3' 106.815(10) . . ? P3 Ag Cl 114.571(10) . 2_556 ? P3' Ag Cl 115.576(10) . 2_556 ? P3 Ag Cl 121.406(10) . . ? P3' Ag Cl 100.201(9) . . ? Cl Ag Cl 97.793(8) 2_556 . ? Ag Cl Ag 82.206(8) 2_556 . ? C2 N1 C7A 112.59(9) . . ? C2 N1 C8 121.94(9) . . ? C7A N1 C8 125.39(9) . . ? N1 C2 P3 115.06(8) . . ? C2 P3 C3A 89.18(5) . . ? C2 P3 Ag 117.48(4) . . ? C3A P3 Ag 133.89(4) . . ? C4 C3A C7A 119.10(10) . . ? C4 C3A P3 129.95(9) . . ? C7A C3A P3 110.94(8) . . ? C5 C4 C3A 119.60(11) . . ? C4 C5 C6 120.56(11) . . ? C7 C6 C5 121.40(11) . . ? C6 C7 C7A 118.16(11) . . ? N1 C7A C7 126.70(10) . . ? N1 C7A C3A 112.13(9) . . ? C7 C7A C3A 121.17(10) . . ? N1 C8 C9 115.26(8) . . ? C10 C9 C11 110.17(9) . . ? C10 C9 C12 108.70(10) . . ? C11 C9 C12 109.63(9) . . ? C10 C9 C8 106.22(9) . . ? C11 C9 C8 111.06(9) . . ? C12 C9 C8 110.98(9) . . ? C2' N1' C7A' 112.95(9) . . ? C2' N1' C8' 121.24(9) . . ? C7A' N1' C8' 125.81(9) . . ? N1' C2' P3' 114.30(8) . . ? C2' P3' C3A' 89.90(5) . . ? C2' P3' Ag 135.41(4) . . ? C3A' P3' Ag 131.36(4) . . ? C4' C3A' C7A' 119.44(10) . . ? C4' C3A' P3' 129.93(9) . . ? C7A' C3A' P3' 110.54(8) . . ? C5' C4' C3A' 119.54(11) . . ? C4' C5' C6' 120.59(11) . . ? C7' C6' C5' 121.28(11) . . ? C6' C7' C7A' 118.38(11) . . ? N1' C7A' C7' 126.91(10) . . ? N1' C7A' C3A' 112.29(9) . . ? C7' C7A' C3A' 120.77(10) . . ? N1' C8' C9' 115.10(8) . . ? C11' C9' C12' 109.82(9) . . ? C11' C9' C10' 109.56(9) . . ? C12' C9' C10' 109.36(9) . . ? C11' C9' C8' 111.40(9) . . ? C12' C9' C8' 110.74(8) . . ? C10' C9' C8' 105.88(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P3 Ag Cl Ag -125.120(10) . . . 2_556 ? P3' Ag Cl Ag 117.864(9) . . . 2_556 ? Cl Ag Cl Ag 0.0 2_556 . . 2_556 ? C7A N1 C2 P3 2.72(12) . . . . ? C8 N1 C2 P3 179.61(8) . . . . ? N1 C2 P3 C3A -3.07(9) . . . . ? N1 C2 P3 Ag -143.79(7) . . . . ? P3' Ag P3 C2 -16.85(4) . . . . ? Cl Ag P3 C2 112.50(4) 2_556 . . . ? Cl Ag P3 C2 -130.51(4) . . . . ? P3' Ag P3 C3A -135.40(5) . . . . ? Cl Ag P3 C3A -6.05(5) 2_556 . . . ? Cl Ag P3 C3A 110.94(5) . . . . ? C2 P3 C3A C4 -178.20(11) . . . . ? Ag P3 C3A C4 -49.40(13) . . . . ? C2 P3 C3A C7A 2.60(8) . . . . ? Ag P3 C3A C7A 131.40(6) . . . . ? C7A C3A C4 C5 -0.47(16) . . . . ? P3 C3A C4 C5 -179.62(9) . . . . ? C3A C4 C5 C6 0.92(18) . . . . ? C4 C5 C6 C7 -0.60(19) . . . . ? C5 C6 C7 C7A -0.18(18) . . . . ? C2 N1 C7A C7 178.71(10) . . . . ? C8 N1 C7A C7 1.96(17) . . . . ? C2 N1 C7A C3A -0.59(13) . . . . ? C8 N1 C7A C3A -177.35(9) . . . . ? C6 C7 C7A N1 -178.63(10) . . . . ? C6 C7 C7A C3A 0.62(16) . . . . ? C4 C3A C7A N1 179.05(10) . . . . ? P3 C3A C7A N1 -1.66(11) . . . . ? C4 C3A C7A C7 -0.30(16) . . . . ? P3 C3A C7A C7 178.99(8) . . . . ? C2 N1 C8 C9 86.68(12) . . . . ? C7A N1 C8 C9 -96.85(12) . . . . ? N1 C8 C9 C10 -174.77(9) . . . . ? N1 C8 C9 C11 65.43(12) . . . . ? N1 C8 C9 C12 -56.78(12) . . . . ? C7A' N1' C2' P3' -0.57(12) . . . . ? C8' N1' C2' P3' -179.69(7) . . . . ? N1' C2' P3' C3A' -0.20(8) . . . . ? N1' C2' P3' Ag -160.17(6) . . . . ? P3 Ag P3' C2' 12.01(5) . . . . ? Cl Ag P3' C2' -116.76(5) 2_556 . . . ? Cl Ag P3' C2' 139.42(5) . . . . ? P3 Ag P3' C3A' -140.84(5) . . . . ? Cl Ag P3' C3A' 90.39(5) 2_556 . . . ? Cl Ag P3' C3A' -13.43(5) . . . . ? C2' P3' C3A' C4' 177.34(11) . . . . ? Ag P3' C3A' C4' -21.34(13) . . . . ? C2' P3' C3A' C7A' 0.89(8) . . . . ? Ag P3' C3A' C7A' 162.21(6) . . . . ? C7A' C3A' C4' C5' 0.82(17) . . . . ? P3' C3A' C4' C5' -175.37(9) . . . . ? C3A' C4' C5' C6' -0.89(18) . . . . ? C4' C5' C6' C7' 0.26(19) . . . . ? C5' C6' C7' C7A' 0.44(18) . . . . ? C2' N1' C7A' C7' -176.73(10) . . . . ? C8' N1' C7A' C7' 2.34(17) . . . . ? C2' N1' C7A' C3A' 1.26(13) . . . . ? C8' N1' C7A' C3A' -179.66(9) . . . . ? C6' C7' C7A' N1' 177.34(11) . . . . ? C6' C7' C7A' C3A' -0.50(16) . . . . ? C4' C3A' C7A' N1' -178.26(9) . . . . ? P3' C3A' C7A' N1' -1.38(11) . . . . ? C4' C3A' C7A' C7' -0.12(16) . . . . ? P3' C3A' C7A' C7' 176.76(8) . . . . ? C2' N1' C8' C9' -88.93(12) . . . . ? C7A' N1' C8' C9' 92.07(12) . . . . ? N1' C8' C9' C11' -69.96(12) . . . . ? N1' C8' C9' C12' 52.58(12) . . . . ? N1' C8' C9' C10' 171.02(9) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.435 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.052 _iucr_refine_instructions_details ; TITL agriw in P-1 CELL 0.71073 8.828414 9.935858 15.561381 107.1966 105.7441 90.4985 ZERR 1.00 0.0002 0.0002 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H N P Cl Ag UNIT 48 64 4 4 2 2 TEMP -173 SIZE 0.45 0.25 0.08 L.S. 4 OMIT 0 -1 1 OMIT 1 -1 6 OMIT -4 0 3 FMAP 2 PLAN 10 SHEL 999 0.71 ACTA CONF WGHT 0.020600 0.489600 FVAR 4.14826 AG 6 0.173857 0.079597 0.501607 11.00000 0.01500 0.01948 = 0.01990 0.00535 0.00587 -0.00212 CL 5 -0.123357 0.116791 0.429944 11.00000 0.01389 0.02179 = 0.02110 0.01142 0.00332 0.00143 N1 3 0.667597 0.343992 0.667141 11.00000 0.01384 0.01418 = 0.01486 0.00420 0.00409 0.00018 C2 1 0.541171 0.298628 0.589934 11.00000 0.01760 0.01537 = 0.01551 0.00457 0.00342 -0.00132 AFIX 43 H2 2 0.550039 0.279941 0.528082 11.00000 -1.20000 AFIX 0 P3 4 0.364212 0.277461 0.612064 11.00000 0.01492 0.01752 = 0.02039 0.00508 0.00358 -0.00234 C3A 1 0.465155 0.323355 0.733283 11.00000 0.02054 0.01073 = 0.01956 0.00406 0.00828 0.00136 C4 1 0.406640 0.330405 0.809949 11.00000 0.02970 0.01492 = 0.02832 0.00504 0.01721 0.00083 AFIX 43 H4 2 0.297187 0.307917 0.800052 11.00000 -1.20000 AFIX 0 C5 1 0.509061 0.370120 0.899440 11.00000 0.04623 0.01740 = 0.02242 0.00405 0.02008 0.00246 AFIX 43 H5 2 0.470045 0.373601 0.951185 11.00000 -1.20000 AFIX 0 C6 1 0.670381 0.405441 0.914789 11.00000 0.04029 0.01871 = 0.01605 0.00419 0.00710 0.00436 AFIX 43 H6 2 0.738938 0.433439 0.977078 11.00000 -1.20000 AFIX 0 C7 1 0.731790 0.400392 0.841222 11.00000 0.02369 0.01744 = 0.01773 0.00515 0.00326 0.00336 AFIX 43 H7 2 0.841189 0.424735 0.852191 11.00000 -1.20000 AFIX 0 C7A 1 0.628139 0.358339 0.749933 11.00000 0.01992 0.01090 = 0.01553 0.00405 0.00638 0.00265 C8 1 0.828283 0.366687 0.660400 11.00000 0.01308 0.01462 = 0.02034 0.00447 0.00623 0.00220 AFIX 23 H8A 2 0.839647 0.294400 0.603650 11.00000 -1.20000 H8B 2 0.904761 0.351250 0.715506 11.00000 -1.20000 AFIX 0 C9 1 0.872792 0.513908 0.655662 11.00000 0.01393 0.01529 = 0.02189 0.00460 0.00668 0.00068 C10 1 1.036534 0.508953 0.639670 11.00000 0.01748 0.02495 = 0.03422 0.00552 0.01295 -0.00038 AFIX 137 H10A 2 1.032147 0.433752 0.581468 11.00000 -1.50000 H10B 2 1.112715 0.489793 0.692558 11.00000 -1.50000 H10C 2 1.069567 0.600142 0.634747 11.00000 -1.50000 AFIX 0 C11 1 0.878049 0.629497 0.747171 11.00000 0.01940 0.01617 = 0.02685 0.00213 0.00772 0.00032 AFIX 137 H11A 2 0.901588 0.722392 0.741290 11.00000 -1.50000 H11B 2 0.960520 0.614221 0.799056 11.00000 -1.50000 H11C 2 0.775404 0.625850 0.759729 11.00000 -1.50000 AFIX 0 C12 1 0.755783 0.545798 0.572890 11.00000 0.02301 0.02213 = 0.02645 0.01210 0.00619 0.00072 AFIX 137 H12A 2 0.650708 0.550615 0.582780 11.00000 -1.50000 H12B 2 0.750792 0.470548 0.514603 11.00000 -1.50000 H12C 2 0.791072 0.636609 0.568390 11.00000 -1.50000 AFIX 0 N1' 3 0.401634 0.003825 0.232920 11.00000 0.01385 0.01491 = 0.01455 0.00551 0.00406 0.00058 C2' 1 0.424418 0.033595 0.326977 11.00000 0.01511 0.01507 = 0.01566 0.00526 0.00438 0.00099 AFIX 43 H2' 2 0.524009 0.069229 0.371967 11.00000 -1.20000 AFIX 0 P3' 4 0.258821 0.001455 0.357210 11.00000 0.01599 0.01857 = 0.01701 0.00564 0.00670 0.00018 C3A' 1 0.149199 -0.055267 0.237446 11.00000 0.01549 0.01377 = 0.01975 0.00659 0.00387 0.00192 C4' 1 -0.010391 -0.109644 0.194877 11.00000 0.01536 0.02037 = 0.03263 0.01162 0.00452 0.00092 AFIX 43 H4' 2 -0.077970 -0.113767 0.232449 11.00000 -1.20000 AFIX 0 C5' 1 -0.067622 -0.156666 0.098664 11.00000 0.01774 0.02459 = 0.03405 0.01140 -0.00450 -0.00242 AFIX 43 H5' 2 -0.174810 -0.194628 0.069779 11.00000 -1.20000 AFIX 0 C6' 1 0.030944 -0.149115 0.042607 11.00000 0.02740 0.02321 = 0.02138 0.00784 -0.00540 -0.00224 AFIX 43 H6' 2 -0.010900 -0.181805 -0.023815 11.00000 -1.20000 AFIX 0 C7' 1 0.187809 -0.094985 0.082258 11.00000 0.02490 0.01918 = 0.01728 0.00697 0.00194 -0.00095 AFIX 43 H7' 2 0.253569 -0.089599 0.043905 11.00000 -1.20000 AFIX 0 C7A' 1 0.247360 -0.048252 0.180485 11.00000 0.01586 0.01248 = 0.01715 0.00584 0.00230 0.00070 C8' 1 0.532277 0.024850 0.195013 11.00000 0.01594 0.01476 = 0.01710 0.00501 0.00784 0.00250 AFIX 23 H8'1 2 0.513306 -0.045794 0.132176 11.00000 -1.20000 H8'2 2 0.631422 0.005933 0.236074 11.00000 -1.20000 AFIX 0 C9' 1 0.556072 0.173734 0.186002 11.00000 0.01652 0.01463 = 0.01659 0.00536 0.00615 0.00087 C10' 1 0.712086 0.178848 0.161019 11.00000 0.02367 0.02412 = 0.02790 0.00744 0.01466 -0.00021 AFIX 137 H10D 2 0.729788 0.269205 0.150172 11.00000 -1.50000 H10E 2 0.706778 0.100803 0.104018 11.00000 -1.50000 H10F 2 0.799389 0.169804 0.212903 11.00000 -1.50000 AFIX 0 C11' 1 0.421251 0.198540 0.108231 11.00000 0.02574 0.02151 = 0.02046 0.01025 0.00221 0.00000 AFIX 137 H11D 2 0.320525 0.187799 0.121806 11.00000 -1.50000 H11E 2 0.418461 0.129314 0.047901 11.00000 -1.50000 H11F 2 0.438428 0.294393 0.105181 11.00000 -1.50000 AFIX 0 C12' 1 0.569413 0.288417 0.279264 11.00000 0.01807 0.01418 = 0.01994 0.00432 0.00526 0.00151 AFIX 137 H12D 2 0.656542 0.272546 0.328664 11.00000 -1.50000 H12E 2 0.470325 0.284426 0.295786 11.00000 -1.50000 H12F 2 0.589907 0.381663 0.273020 11.00000 -1.50000 HKLF 4 ; _database_code_depnum_ccdc_archive 'CCDC 926714' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_grehg _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H21 Cl2 Hg N P2' _chemical_formula_weight 680.87 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 9.3339(3) _cell_length_b 28.7742(9) _cell_length_c 9.6247(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.243(4) _cell_angle_gamma 90.00 _cell_volume 2577.87(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23313 _cell_measurement_theta_min 2.1835 _cell_measurement_theta_max 30.8396 _exptl_crystal_description tablet _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 6.316 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59323 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 96745 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7494 _reflns_number_gt 6659 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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. The NH hydrogen was refined freely. The methyl group was refined as an idealised rigid group allowed to rotate but not tip. Other hydrogens were included using a riding model. ; _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^)+(0.0113P)^2^+3.0617P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7494 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0442 _refine_ls_wR_factor_gt 0.0426 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.003 _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 Hg Hg 0.238764(10) 0.131387(3) 0.363217(10) 0.01631(3) Uani 1 1 d . . . Cl1 Cl 0.11638(6) 0.10420(2) 0.56217(6) 0.01804(12) Uani 1 1 d . . . Cl2 Cl 0.35580(7) 0.20702(2) 0.41938(7) 0.02122(13) Uani 1 1 d . . . P1 P 0.35836(6) 0.08127(2) 0.20176(6) 0.01252(12) Uani 1 1 d . . . N1 N 0.1582(2) 0.21539(7) 0.0564(2) 0.0165(4) Uani 1 1 d . . . H01 H 0.216(3) 0.2323(10) 0.020(3) 0.013(7) Uiso 1 1 d . . . C2 C 0.1721(3) 0.16891(8) 0.0598(3) 0.0150(5) Uani 1 1 d . . . P3 P 0.03639(7) 0.14196(2) 0.15056(7) 0.01580(13) Uani 1 1 d . . . C3A C -0.0285(3) 0.19812(8) 0.1940(3) 0.0164(5) Uani 1 1 d . . . C4 C -0.1384(3) 0.21147(9) 0.2777(3) 0.0195(5) Uani 1 1 d . . . H4 H -0.1924 0.1883 0.3211 0.023 Uiso 1 1 calc R . . C5 C -0.1692(3) 0.25796(9) 0.2978(3) 0.0212(5) Uani 1 1 d . . . C6 C -0.0906(3) 0.29193(9) 0.2296(3) 0.0234(6) Uani 1 1 d . . . H6 H -0.1129 0.3238 0.2417 0.028 Uiso 1 1 calc R . . C7 C 0.0178(3) 0.28013(9) 0.1456(3) 0.0210(5) Uani 1 1 d . . . H7 H 0.0693 0.3033 0.0998 0.025 Uiso 1 1 calc R . . C7A C 0.0490(3) 0.23317(8) 0.1303(3) 0.0168(5) Uani 1 1 d . . . C8 C -0.2846(3) 0.27213(10) 0.3915(3) 0.0290(7) Uani 1 1 d . . . H8A H -0.3793 0.2659 0.3444 0.044 Uiso 1 1 calc R . . H8B H -0.2758 0.3054 0.4124 0.044 Uiso 1 1 calc R . . H8C H -0.2735 0.2543 0.4784 0.044 Uiso 1 1 calc R . . C11 C 0.3746(3) 0.10984(8) 0.0353(2) 0.0143(5) Uani 1 1 d . . . C12 C 0.2880(3) 0.14733(8) -0.0157(3) 0.0145(5) Uani 1 1 d . . . C13 C 0.3150(3) 0.16650(9) -0.1454(3) 0.0201(5) Uani 1 1 d . . . H13 H 0.2586 0.1920 -0.1803 0.024 Uiso 1 1 calc R . . C14 C 0.4217(3) 0.14931(9) -0.2235(3) 0.0216(5) Uani 1 1 d . . . H14 H 0.4362 0.1625 -0.3119 0.026 Uiso 1 1 calc R . . C15 C 0.5074(3) 0.11288(9) -0.1726(3) 0.0204(5) Uani 1 1 d . . . H15 H 0.5814 0.1012 -0.2256 0.024 Uiso 1 1 calc R . . C16 C 0.4848(3) 0.09361(9) -0.0441(3) 0.0182(5) Uani 1 1 d . . . H16 H 0.5448 0.0690 -0.0091 0.022 Uiso 1 1 calc R . . C21 C 0.2554(2) 0.02870(8) 0.1679(2) 0.0139(5) Uani 1 1 d . . . C22 C 0.2064(3) 0.00504(9) 0.2815(3) 0.0222(6) Uani 1 1 d . . . H22 H 0.2223 0.0176 0.3726 0.027 Uiso 1 1 calc R . . C23 C 0.1342(3) -0.03690(10) 0.2618(3) 0.0260(6) Uani 1 1 d . . . H23 H 0.1020 -0.0532 0.3395 0.031 Uiso 1 1 calc R . . C24 C 0.1092(3) -0.05493(9) 0.1293(3) 0.0203(5) Uani 1 1 d . . . H24 H 0.0597 -0.0836 0.1160 0.024 Uiso 1 1 calc R . . C25 C 0.1561(3) -0.03143(9) 0.0159(3) 0.0214(5) Uani 1 1 d . . . H25 H 0.1385 -0.0439 -0.0752 0.026 Uiso 1 1 calc R . . C26 C 0.2287(3) 0.01034(9) 0.0352(3) 0.0178(5) Uani 1 1 d . . . H26 H 0.2605 0.0265 -0.0430 0.021 Uiso 1 1 calc R . . C31 C 0.5372(3) 0.06299(8) 0.2645(3) 0.0150(5) Uani 1 1 d . . . C32 C 0.6334(3) 0.09720(9) 0.3167(3) 0.0211(5) Uani 1 1 d . . . H32 H 0.6048 0.1289 0.3167 0.025 Uiso 1 1 calc R . . C33 C 0.7706(3) 0.08469(10) 0.3684(3) 0.0237(6) Uani 1 1 d . . . H33 H 0.8364 0.1079 0.4030 0.028 Uiso 1 1 calc R . . C34 C 0.8116(3) 0.03837(10) 0.3697(3) 0.0229(6) Uani 1 1 d . . . H34 H 0.9060 0.0300 0.4045 0.028 Uiso 1 1 calc R . . C35 C 0.7162(3) 0.00435(10) 0.3208(3) 0.0230(6) Uani 1 1 d . . . H35 H 0.7447 -0.0274 0.3231 0.028 Uiso 1 1 calc R . . C36 C 0.5788(3) 0.01652(9) 0.2683(3) 0.0182(5) Uani 1 1 d . . . H36 H 0.5132 -0.0069 0.2349 0.022 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 Hg 0.01934(5) 0.01345(5) 0.01601(5) -0.00207(4) 0.00045(3) 0.00178(4) Cl1 0.0183(3) 0.0143(3) 0.0216(3) 0.0012(2) 0.0024(2) -0.0010(2) Cl2 0.0217(3) 0.0140(3) 0.0285(3) -0.0038(2) 0.0052(2) -0.0028(2) P1 0.0133(3) 0.0096(3) 0.0145(3) -0.0003(2) 0.0001(2) 0.0004(2) N1 0.0163(11) 0.0119(10) 0.0209(11) 0.0042(8) -0.0011(8) -0.0012(8) C2 0.0169(12) 0.0132(12) 0.0140(12) 0.0002(9) -0.0042(9) -0.0004(9) P3 0.0150(3) 0.0110(3) 0.0209(3) 0.0011(2) -0.0018(2) -0.0012(2) C3A 0.0143(12) 0.0128(12) 0.0212(13) 0.0017(9) -0.0053(9) -0.0008(9) C4 0.0164(12) 0.0165(13) 0.0254(14) 0.0022(10) -0.0007(10) -0.0004(10) C5 0.0144(12) 0.0214(14) 0.0273(14) -0.0011(11) -0.0024(10) 0.0034(10) C6 0.0230(14) 0.0131(13) 0.0334(16) -0.0014(11) -0.0035(11) 0.0034(10) C7 0.0206(13) 0.0144(13) 0.0276(15) 0.0020(10) -0.0014(11) -0.0010(10) C7A 0.0137(12) 0.0138(12) 0.0221(13) 0.0007(9) -0.0035(9) 0.0006(9) C8 0.0227(15) 0.0249(15) 0.0395(18) -0.0021(12) 0.0023(12) 0.0061(11) C11 0.0164(12) 0.0127(12) 0.0136(11) 0.0000(9) -0.0007(9) -0.0040(9) C12 0.0160(12) 0.0106(11) 0.0163(12) -0.0018(9) -0.0022(9) -0.0040(9) C13 0.0211(13) 0.0193(13) 0.0192(13) 0.0018(10) -0.0035(10) -0.0025(10) C14 0.0269(14) 0.0217(13) 0.0160(13) 0.0031(10) -0.0005(10) -0.0062(11) C15 0.0225(13) 0.0202(13) 0.0187(13) -0.0032(10) 0.0036(10) -0.0041(10) C16 0.0178(12) 0.0156(12) 0.0211(13) -0.0001(9) 0.0017(10) -0.0004(9) C21 0.0131(11) 0.0127(11) 0.0160(12) -0.0015(8) 0.0022(9) 0.0004(9) C22 0.0320(15) 0.0204(14) 0.0149(13) -0.0024(10) 0.0050(11) -0.0091(11) C23 0.0328(16) 0.0230(15) 0.0230(14) 0.0007(11) 0.0070(12) -0.0120(12) C24 0.0203(13) 0.0156(13) 0.0249(14) -0.0016(10) 0.0007(10) -0.0056(10) C25 0.0252(14) 0.0207(14) 0.0182(13) -0.0055(10) 0.0007(10) -0.0055(10) C26 0.0188(13) 0.0172(13) 0.0177(13) -0.0001(9) 0.0034(10) -0.0017(9) C31 0.0153(12) 0.0157(12) 0.0142(12) 0.0028(9) 0.0016(9) 0.0007(9) C32 0.0194(13) 0.0180(13) 0.0254(14) 0.0033(10) -0.0015(10) 0.0004(10) C33 0.0161(13) 0.0278(15) 0.0267(15) 0.0041(11) -0.0023(11) -0.0031(10) C34 0.0143(13) 0.0356(16) 0.0187(13) 0.0046(11) 0.0005(10) 0.0088(11) C35 0.0295(15) 0.0228(14) 0.0166(13) 0.0035(10) 0.0012(11) 0.0127(11) C36 0.0230(13) 0.0162(12) 0.0153(12) 0.0004(9) 0.0006(10) 0.0028(10) _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 Hg Cl1 2.4305(6) . ? Hg P1 2.4489(6) . ? Hg Cl2 2.4766(6) . ? Hg P3 2.6978(7) . ? P1 C21 1.809(2) . ? P1 C31 1.811(2) . ? P1 C11 1.817(2) . ? N1 C2 1.344(3) . ? N1 C7A 1.383(3) . ? C2 C12 1.483(3) . ? C2 P3 1.770(3) . ? P3 C3A 1.786(3) . ? C3A C4 1.405(4) . ? C3A C7A 1.408(3) . ? C4 C5 1.385(4) . ? C5 C6 1.413(4) . ? C5 C8 1.511(4) . ? C6 C7 1.384(4) . ? C7 C7A 1.392(3) . ? C11 C16 1.405(3) . ? C11 C12 1.415(3) . ? C12 C13 1.404(3) . ? C13 C14 1.383(4) . ? C14 C15 1.386(4) . ? C15 C16 1.386(4) . ? C21 C26 1.388(3) . ? C21 C22 1.394(3) . ? C22 C23 1.388(4) . ? C23 C24 1.381(4) . ? C24 C25 1.382(4) . ? C25 C26 1.386(3) . ? C31 C36 1.392(3) . ? C31 C32 1.401(3) . ? C32 C33 1.386(4) . ? C33 C34 1.387(4) . ? C34 C35 1.383(4) . ? C35 C36 1.388(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 Cl1 Hg P1 124.98(2) . . ? Cl1 Hg Cl2 109.65(2) . . ? P1 Hg Cl2 116.20(2) . . ? Cl1 Hg P3 106.89(2) . . ? P1 Hg P3 84.92(2) . . ? Cl2 Hg P3 109.83(2) . . ? C21 P1 C31 106.35(11) . . ? C21 P1 C11 107.31(11) . . ? C31 P1 C11 106.86(11) . . ? C21 P1 Hg 110.22(8) . . ? C31 P1 Hg 114.32(8) . . ? C11 P1 Hg 111.40(8) . . ? C2 N1 C7A 115.4(2) . . ? N1 C2 C12 118.5(2) . . ? N1 C2 P3 112.14(18) . . ? C12 C2 P3 129.25(18) . . ? C2 P3 C3A 89.22(12) . . ? C2 P3 Hg 86.40(8) . . ? C3A P3 Hg 98.92(8) . . ? C4 C3A C7A 118.3(2) . . ? C4 C3A P3 131.0(2) . . ? C7A C3A P3 110.63(19) . . ? C5 C4 C3A 120.8(2) . . ? C4 C5 C6 118.9(2) . . ? C4 C5 C8 120.5(2) . . ? C6 C5 C8 120.5(2) . . ? C7 C6 C5 122.0(2) . . ? C6 C7 C7A 117.9(2) . . ? N1 C7A C7 125.5(2) . . ? N1 C7A C3A 112.4(2) . . ? C7 C7A C3A 122.1(2) . . ? C16 C11 C12 119.1(2) . . ? C16 C11 P1 116.20(18) . . ? C12 C11 P1 124.63(19) . . ? C13 C12 C11 118.2(2) . . ? C13 C12 C2 117.2(2) . . ? C11 C12 C2 124.6(2) . . ? C14 C13 C12 121.8(2) . . ? C13 C14 C15 119.9(2) . . ? C16 C15 C14 119.7(2) . . ? C15 C16 C11 121.2(2) . . ? C26 C21 C22 119.3(2) . . ? C26 C21 P1 122.73(19) . . ? C22 C21 P1 117.91(18) . . ? C23 C22 C21 120.1(2) . . ? C24 C23 C22 120.0(3) . . ? C23 C24 C25 120.3(2) . . ? C24 C25 C26 119.9(2) . . ? C25 C26 C21 120.4(2) . . ? C36 C31 C32 119.7(2) . . ? C36 C31 P1 122.43(19) . . ? C32 C31 P1 117.80(19) . . ? C33 C32 C31 119.8(2) . . ? C32 C33 C34 120.0(3) . . ? C35 C34 C33 120.4(2) . . ? C34 C35 C36 120.0(2) . . ? C35 C36 C31 120.0(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H01 Cl2 0.83(3) 2.42(3) 3.238(2) 169(3) 4_565 C7 H7 Cl1 0.95 2.73 3.560(3) 147.1 4_565 C23 H23 Cl1 0.95 2.74 3.560(3) 145.5 3_556 C35 H35 Cl1 0.95 2.75 3.634(3) 154.6 3_656 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.768 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.111 _iucr_refine_instructions_details ; TITL grehg in P2(1)/c CELL 0.71073 9.333921 28.774187 9.624676 90.0000 94.2430 90.0000 ZERR 4.00 0.0003 0.0009 0.0003 0.0000 0.004 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N P Cl Hg UNIT 104 84 4 8 8 4 TEMP -173 SIZE 0.2 0.15 0.05 L.S. 4 ACTA SHEL 999 0.71 EQIV $1 x,0.5-y,-0.5+z EQIV $2 -x,-y,1-z EQIV $3 1-x,-y,1-z HTAB N1 CL2_$1 HTAB C7 CL1_$1 HTAB C23 CL1_$2 HTAB C35 CL1_$3 FMAP 2 PLAN 10 WGHT 0.011300 3.061700 FVAR 1.20656 HG 6 0.238764 0.131387 0.363217 11.00000 0.01934 0.01345 = 0.01601 -0.00207 0.00045 0.00178 CL1 5 0.116381 0.104204 0.562175 11.00000 0.01833 0.01433 = 0.02160 0.00122 0.00235 -0.00105 CL2 5 0.355804 0.207015 0.419379 11.00000 0.02166 0.01400 = 0.02852 -0.00384 0.00524 -0.00282 P1 4 0.358362 0.081269 0.201764 11.00000 0.01333 0.00959 = 0.01451 -0.00028 0.00009 0.00042 N1 3 0.158170 0.215386 0.056352 11.00000 0.01635 0.01190 = 0.02090 0.00419 -0.00108 -0.00125 H01 2 0.216450 0.232260 0.019937 11.00000 0.01349 C2 1 0.172099 0.168914 0.059827 11.00000 0.01689 0.01317 = 0.01401 0.00025 -0.00421 -0.00037 P3 4 0.036389 0.141959 0.150557 11.00000 0.01500 0.01101 = 0.02094 0.00114 -0.00177 -0.00122 C3A 1 -0.028494 0.198116 0.193962 11.00000 0.01429 0.01283 = 0.02118 0.00171 -0.00534 -0.00084 C4 1 -0.138441 0.211468 0.277705 11.00000 0.01642 0.01647 = 0.02542 0.00215 -0.00070 -0.00037 AFIX 43 H4 2 -0.192392 0.188319 0.321065 11.00000 -1.20000 AFIX 0 C5 1 -0.169162 0.257959 0.297840 11.00000 0.01437 0.02143 = 0.02733 -0.00110 -0.00243 0.00335 C6 1 -0.090640 0.291927 0.229566 11.00000 0.02296 0.01310 = 0.03339 -0.00137 -0.00354 0.00343 AFIX 43 H6 2 -0.112950 0.323816 0.241687 11.00000 -1.20000 AFIX 0 C7 1 0.017796 0.280130 0.145568 11.00000 0.02060 0.01445 = 0.02756 0.00196 -0.00142 -0.00100 AFIX 43 H7 2 0.069324 0.303332 0.099789 11.00000 -1.20000 AFIX 0 C7A 1 0.048991 0.233173 0.130270 11.00000 0.01371 0.01383 = 0.02209 0.00068 -0.00350 0.00057 C8 1 -0.284603 0.272128 0.391524 11.00000 0.02265 0.02485 = 0.03951 -0.00207 0.00230 0.00606 AFIX 137 H8A 2 -0.379340 0.265873 0.344439 11.00000 -1.50000 H8B 2 -0.275805 0.305382 0.412439 11.00000 -1.50000 H8C 2 -0.273520 0.254316 0.478442 11.00000 -1.50000 AFIX 0 C11 1 0.374647 0.109835 0.035319 11.00000 0.01638 0.01266 = 0.01356 0.00004 -0.00073 -0.00403 C12 1 0.287954 0.147327 -0.015743 11.00000 0.01604 0.01061 = 0.01627 -0.00178 -0.00218 -0.00398 C13 1 0.315042 0.166505 -0.145362 11.00000 0.02105 0.01934 = 0.01923 0.00182 -0.00346 -0.00254 AFIX 43 H13 2 0.258553 0.191982 -0.180338 11.00000 -1.20000 AFIX 0 C14 1 0.421723 0.149312 -0.223500 11.00000 0.02689 0.02168 = 0.01598 0.00312 -0.00052 -0.00620 AFIX 43 H14 2 0.436240 0.162456 -0.311908 11.00000 -1.20000 AFIX 0 C15 1 0.507419 0.112877 -0.172628 11.00000 0.02254 0.02023 = 0.01869 -0.00321 0.00363 -0.00408 AFIX 43 H15 2 0.581377 0.101159 -0.225624 11.00000 -1.20000 AFIX 0 C16 1 0.484764 0.093607 -0.044110 11.00000 0.01784 0.01557 = 0.02109 -0.00009 0.00170 -0.00036 AFIX 43 H16 2 0.544795 0.068968 -0.009051 11.00000 -1.20000 AFIX 0 C21 1 0.255401 0.028696 0.167922 11.00000 0.01307 0.01273 = 0.01603 -0.00147 0.00222 0.00043 C22 1 0.206359 0.005040 0.281535 11.00000 0.03196 0.02036 = 0.01488 -0.00242 0.00497 -0.00906 AFIX 43 H22 2 0.222335 0.017640 0.372598 11.00000 -1.20000 AFIX 0 C23 1 0.134219 -0.036896 0.261850 11.00000 0.03281 0.02296 = 0.02296 0.00068 0.00698 -0.01203 AFIX 43 H23 2 0.102029 -0.053192 0.339540 11.00000 -1.20000 AFIX 0 C24 1 0.109248 -0.054926 0.129283 11.00000 0.02030 0.01564 = 0.02487 -0.00163 0.00068 -0.00558 AFIX 43 H24 2 0.059676 -0.083602 0.115994 11.00000 -1.20000 AFIX 0 C25 1 0.156062 -0.031434 0.015892 11.00000 0.02521 0.02072 = 0.01819 -0.00553 0.00071 -0.00548 AFIX 43 H25 2 0.138459 -0.043905 -0.075162 11.00000 -1.20000 AFIX 0 C26 1 0.228727 0.010345 0.035152 11.00000 0.01878 0.01717 = 0.01770 -0.00009 0.00340 -0.00169 AFIX 43 H26 2 0.260461 0.026515 -0.042967 11.00000 -1.20000 AFIX 0 C31 1 0.537207 0.062990 0.264470 11.00000 0.01534 0.01568 = 0.01415 0.00277 0.00158 0.00072 C32 1 0.633420 0.097203 0.316709 11.00000 0.01943 0.01804 = 0.02537 0.00331 -0.00151 0.00045 AFIX 43 H32 2 0.604788 0.128885 0.316711 11.00000 -1.20000 AFIX 0 C33 1 0.770557 0.084687 0.368410 11.00000 0.01607 0.02782 = 0.02669 0.00405 -0.00233 -0.00307 AFIX 43 H33 2 0.836418 0.107851 0.402964 11.00000 -1.20000 AFIX 0 C34 1 0.811637 0.038373 0.369709 11.00000 0.01432 0.03563 = 0.01872 0.00455 0.00050 0.00875 AFIX 43 H34 2 0.905991 0.029960 0.404459 11.00000 -1.20000 AFIX 0 C35 1 0.716205 0.004351 0.320771 11.00000 0.02948 0.02276 = 0.01665 0.00352 0.00122 0.01267 AFIX 43 H35 2 0.744662 -0.027355 0.323083 11.00000 -1.20000 AFIX 0 C36 1 0.578810 0.016524 0.268260 11.00000 0.02296 0.01620 = 0.01527 0.00041 0.00056 0.00280 AFIX 43 H36 2 0.513150 -0.006865 0.234897 11.00000 -1.20000 HKLF 4 ; #============================================================================= # end of cif data for "grehg" (compound 3) #============================================================================= #============================================================================= # end of combined cif file #============================================================================= _database_code_depnum_ccdc_archive 'CCDC 926715'