# Electronic Supplementary Material (ESI) for Chemical Communications # 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_fb56 _database_code_depnum_ccdc_archive 'CCDC 927723' #TrackingRef '18245_web_deposit_cif_file_0_AlanL.Balch_1362431307.HgCo2(CO)8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(cobalt tetracarbonyl) mercury (II) ; _chemical_name_common ; bis(cobalt tetracarbonyl) mercury (II) ; _chemical_melting_point ? _chemical_formula_moiety 'C8 Co2 Hg O8' _chemical_formula_sum 'C8 Co2 Hg O8' _chemical_formula_weight 542.53 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' 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' 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' _symmetry_space_group_name_Hall '-P 2ybc' 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 6.5040(4) _cell_length_b 16.2802(10) _cell_length_c 12.2719(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.422(2) _cell_angle_gamma 90.00 _cell_volume 1277.99(14) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9905 _cell_measurement_theta_min 2.502 _cell_measurement_theta_max 32.844 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 14.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0601 _exptl_absorpt_correction_T_max 0.1030 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'Bruker Apex II' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 19814 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 30.50 _reflns_number_total 3884 _reflns_number_gt 3687 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, XP (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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. One residual electron peak was close to Hg and probably arises form absorption effects. ; _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^)+(0.0202P)^2^+1.9003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3884 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0218 _refine_ls_wR_factor_ref 0.0520 _refine_ls_wR_factor_gt 0.0514 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.002 _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 Hg1 Hg 0.615855(17) 0.328036(7) 0.622303(9) 0.01065(4) Uani 1 1 d . . . Co1 Co 0.41592(6) 0.19905(2) 0.56226(3) 0.00867(8) Uani 1 1 d . . . Co2 Co 0.82160(6) 0.45471(2) 0.68891(3) 0.00760(8) Uani 1 1 d . . . O1 O 0.1884(4) 0.04779(15) 0.4869(2) 0.0196(5) Uani 1 1 d . . . O2 O 0.4798(5) 0.16530(16) 0.8017(2) 0.0254(6) Uani 1 1 d . . . O3 O 0.0842(4) 0.31451(16) 0.4659(3) 0.0264(6) Uani 1 1 d . . . O4 O 0.7669(5) 0.16876(19) 0.4475(3) 0.0339(8) Uani 1 1 d . . . O5 O 1.1553(4) 0.33433(15) 0.7607(2) 0.0223(5) Uani 1 1 d . . . O6 O 0.4764(4) 0.47747(15) 0.8113(2) 0.0181(5) Uani 1 1 d . . . O7 O 0.7370(4) 0.50278(18) 0.4540(2) 0.0222(5) Uani 1 1 d . . . O8 O 1.0584(4) 0.60119(17) 0.7766(2) 0.0253(6) Uani 1 1 d . . . C1 C 0.2754(5) 0.1063(2) 0.5164(2) 0.0133(6) Uani 1 1 d . . . C2 C 0.4574(5) 0.18022(18) 0.7097(3) 0.0140(6) Uani 1 1 d . . . C3 C 0.2158(5) 0.2712(2) 0.5040(3) 0.0154(6) Uani 1 1 d . . . C4 C 0.6338(5) 0.1819(2) 0.4926(3) 0.0167(6) Uani 1 1 d . . . C5 C 1.0226(5) 0.3795(2) 0.7323(2) 0.0133(6) Uani 1 1 d . . . C6 C 0.6094(5) 0.46682(18) 0.7636(2) 0.0115(5) Uani 1 1 d . . . C7 C 0.7683(5) 0.4824(2) 0.5442(3) 0.0126(5) Uani 1 1 d . . . C8 C 0.9698(5) 0.5448(2) 0.7427(3) 0.0143(6) 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 Hg1 0.01440(6) 0.00699(6) 0.01000(6) -0.00258(4) 0.00065(4) -0.00340(4) Co1 0.01294(18) 0.00632(17) 0.00648(17) -0.00120(14) 0.00101(14) -0.00221(14) Co2 0.00984(17) 0.00659(17) 0.00595(16) -0.00026(14) 0.00032(13) -0.00152(13) O1 0.0265(13) 0.0149(11) 0.0174(12) -0.0024(9) 0.0038(10) -0.0109(10) O2 0.0449(17) 0.0187(13) 0.0123(12) 0.0004(10) 0.0042(11) -0.0040(11) O3 0.0248(13) 0.0168(12) 0.0337(16) 0.0035(11) -0.0049(11) 0.0030(10) O4 0.0291(15) 0.0342(17) 0.0436(19) -0.0228(13) 0.0208(14) -0.0128(12) O5 0.0236(13) 0.0192(13) 0.0214(13) -0.0021(10) -0.0030(10) 0.0084(10) O6 0.0209(11) 0.0166(12) 0.0188(12) -0.0031(9) 0.0085(9) -0.0023(9) O7 0.0202(12) 0.0339(15) 0.0121(11) 0.0100(10) 0.0017(9) -0.0032(10) O8 0.0228(13) 0.0189(13) 0.0316(15) -0.0047(11) -0.0016(11) -0.0078(10) C1 0.0179(14) 0.0136(14) 0.0084(13) 0.0018(11) 0.0024(11) -0.0008(11) C2 0.0211(15) 0.0084(13) 0.0121(14) -0.0015(11) 0.0022(12) -0.0025(11) C3 0.0183(15) 0.0109(14) 0.0161(14) -0.0006(11) 0.0008(11) -0.0046(11) C4 0.0197(15) 0.0128(15) 0.0172(15) -0.0071(12) 0.0028(12) -0.0058(11) C5 0.0167(14) 0.0138(14) 0.0088(13) -0.0039(11) 0.0002(11) -0.0018(11) C6 0.0162(14) 0.0075(13) 0.0098(13) -0.0017(10) -0.0006(10) -0.0033(10) C7 0.0109(13) 0.0137(14) 0.0131(13) 0.0018(11) 0.0020(10) -0.0025(10) C8 0.0144(14) 0.0138(14) 0.0139(14) 0.0019(11) 0.0000(11) 0.0012(11) _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 Hg1 Co1 2.5093(4) . ? Hg1 Co2 2.5132(4) . ? Co1 C1 1.802(3) . ? Co1 C3 1.803(3) . ? Co1 C4 1.804(4) . ? Co1 C2 1.807(3) . ? Co2 C6 1.800(3) . ? Co2 C5 1.800(3) . ? Co2 C7 1.803(3) . ? Co2 C8 1.812(3) . ? O1 C1 1.133(4) . ? O2 C2 1.137(4) . ? O3 C3 1.142(4) . ? O4 C4 1.129(5) . ? O5 C5 1.139(4) . ? O6 C6 1.142(4) . ? O7 C7 1.138(4) . ? O8 C8 1.124(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 Co1 Hg1 Co2 177.934(13) . . ? C1 Co1 C3 97.69(14) . . ? C1 Co1 C4 96.90(14) . . ? C3 Co1 C4 119.05(16) . . ? C1 Co1 C2 98.37(14) . . ? C3 Co1 C2 118.29(15) . . ? C4 Co1 C2 117.43(16) . . ? C1 Co1 Hg1 178.67(10) . . ? C3 Co1 Hg1 82.50(10) . . ? C4 Co1 Hg1 81.87(10) . . ? C2 Co1 Hg1 82.67(10) . . ? C6 Co2 C5 120.41(14) . . ? C6 Co2 C7 116.45(14) . . ? C5 Co2 C7 117.46(14) . . ? C6 Co2 C8 97.57(14) . . ? C5 Co2 C8 97.63(14) . . ? C7 Co2 C8 98.73(15) . . ? C6 Co2 Hg1 80.99(9) . . ? C5 Co2 Hg1 81.56(10) . . ? C7 Co2 Hg1 83.60(10) . . ? C8 Co2 Hg1 177.64(11) . . ? O1 C1 Co1 179.3(3) . . ? O2 C2 Co1 177.2(3) . . ? O3 C3 Co1 177.4(3) . . ? O4 C4 Co1 177.6(3) . . ? O5 C5 Co2 177.3(3) . . ? O6 C6 Co2 177.5(3) . . ? O7 C7 Co2 177.4(3) . . ? O8 C8 Co2 178.7(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.276 _refine_diff_density_min -1.766 _refine_diff_density_rms 0.200 _iucr_refine_instructions_details ; TITL fb56 in P2(1)/c CELL 0.71073 6.5040 16.2802 12.2719 90.000 100.422 90.000 ZERR 4.00 0.0004 0.0010 0.0008 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C O Co HG UNIT 32 32 8 4 TEMP -183.000 SIZE 0.286 0.330 0.441 L.S. 12 BOND ACTA WGHT 0.020200 1.900300 FVAR 0.07006 HG1 4 0.615855 0.328036 0.622303 11.00000 0.01440 0.00699 = 0.01000 -0.00258 0.00065 -0.00340 CO1 3 0.415917 0.199053 0.562257 11.00000 0.01294 0.00632 = 0.00648 -0.00120 0.00101 -0.00221 CO2 3 0.821601 0.454709 0.688907 11.00000 0.00984 0.00659 = 0.00595 -0.00026 0.00032 -0.00152 O1 2 0.188386 0.047794 0.486943 11.00000 0.02653 0.01494 = 0.01738 -0.00235 0.00384 -0.01093 O2 2 0.479839 0.165302 0.801681 11.00000 0.04493 0.01873 = 0.01232 0.00038 0.00421 -0.00395 O3 2 0.084176 0.314505 0.465882 11.00000 0.02482 0.01676 = 0.03372 0.00348 -0.00485 0.00304 O4 2 0.766935 0.168758 0.447541 11.00000 0.02913 0.03419 = 0.04357 -0.02279 0.02081 -0.01277 O5 2 1.155279 0.334327 0.760713 11.00000 0.02361 0.01919 = 0.02137 -0.00214 -0.00305 0.00838 O6 2 0.476386 0.477473 0.811343 11.00000 0.02086 0.01656 = 0.01883 -0.00306 0.00853 -0.00233 O7 2 0.737025 0.502780 0.454029 11.00000 0.02021 0.03394 = 0.01207 0.01001 0.00165 -0.00324 O8 2 1.058378 0.601188 0.776628 11.00000 0.02285 0.01893 = 0.03158 -0.00471 -0.00158 -0.00780 C1 1 0.275414 0.106274 0.516435 11.00000 0.01789 0.01356 = 0.00836 0.00175 0.00238 -0.00077 C2 1 0.457358 0.180216 0.709744 11.00000 0.02111 0.00838 = 0.01213 -0.00149 0.00223 -0.00248 C3 1 0.215816 0.271237 0.504022 11.00000 0.01835 0.01092 = 0.01610 -0.00057 0.00078 -0.00463 C4 1 0.633809 0.181944 0.492603 11.00000 0.01973 0.01282 = 0.01721 -0.00709 0.00277 -0.00582 C5 1 1.022591 0.379460 0.732328 11.00000 0.01666 0.01376 = 0.00881 -0.00391 0.00020 -0.00182 C6 1 0.609412 0.466824 0.763611 11.00000 0.01615 0.00751 = 0.00975 -0.00174 -0.00064 -0.00333 C7 1 0.768322 0.482366 0.544242 11.00000 0.01088 0.01372 = 0.01308 0.00175 0.00197 -0.00249 C8 1 0.969774 0.544755 0.742746 11.00000 0.01444 0.01378 = 0.01386 0.00189 0.00003 0.00123 HKLF 4 REM fb56 in P2(1)/c REM R1 = 0.0218 for 3687 Fo > 4sig(Fo) and 0.0237 for all 3884 data REM 172 parameters refined using 0 restraints END WGHT 0.0201 1.9442 REM Highest difference peak 1.276, deepest hole -1.766, 1-sigma level 0.200 Q1 1 0.4920 0.3277 0.6162 11.00000 0.05 1.28 Q2 1 0.7411 0.3285 0.6120 11.00000 0.05 0.93 Q3 1 0.6830 0.3339 0.7238 11.00000 0.05 0.76 Q4 1 0.5556 0.3215 0.5196 11.00000 0.05 0.72 Q5 1 0.7602 0.2956 0.6618 11.00000 0.05 0.72 Q6 1 0.9352 0.6746 0.8961 11.00000 0.05 0.62 Q7 1 0.4613 0.2929 0.5732 11.00000 0.05 0.61 Q8 1 0.7228 0.2891 0.5653 11.00000 0.05 0.57 Q9 1 0.5801 0.4127 0.6190 11.00000 0.05 0.56 Q10 1 0.4688 0.1708 0.6560 11.00000 0.05 0.54 ; data_fb06 _database_code_depnum_ccdc_archive 'CCDC 927724' #TrackingRef '18246_web_deposit_cif_file_1_AlanL.Balch_1362431307.HgCo2(CO)8_C60_toluene.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Hg[Co(CO)4)]2.C60.toluene _chemical_melting_point ? _chemical_formula_moiety 'C60, C8 Co2 Hg O8, C7 H8' _chemical_formula_sum 'C75 H8 Co2 Hg O8' _chemical_formula_weight 1355.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0034 0.0017 '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' O O 0.0115 0.0065 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3514 1.0236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.6413 9.6445 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 10.1012(4) _cell_length_b 13.6265(6) _cell_length_c 32.2524(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4439.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9931 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 33.71 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.01 _exptl_crystal_size_mid 0.009 _exptl_crystal_size_min 0.003 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 4.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9586 _exptl_absorpt_correction_T_max 0.9873 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker Apex II' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 45810 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 33.63 _reflns_number_total 6752 _reflns_number_gt 5807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SIR2004 (Burla et al., 2004)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, XP (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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 structure contains a molecule of toluene which has disorder with respect to the two fold axis. The toluene was refined with part -1 and simu commands. The largest peaks in the final difference map indicate minor disorder in the orientation of the C60, which was not modeled. ; _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^)+(0.0000P)^2^+26.9495P] 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 6752 _refine_ls_number_parameters 421 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.196 _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 Hg1 Hg 0.2500 0.2500 0.307545(7) 0.02305(7) Uani 1 2 d S . . Co1 Co 0.23847(5) 0.06637(3) 0.306831(16) 0.01655(10) Uani 1 1 d . . . O1 O 0.2305(3) -0.1452(2) 0.29080(11) 0.0274(7) Uani 1 1 d . . . O2 O 0.2310(4) 0.0736(3) 0.39826(10) 0.0354(8) Uani 1 1 d . . . O3 O -0.0170(3) 0.1088(2) 0.26707(11) 0.0300(7) Uani 1 1 d . . . O4 O 0.5034(4) 0.0919(3) 0.27151(12) 0.0356(8) Uani 1 1 d . . . C1 C 0.2335(4) -0.0640(3) 0.29763(13) 0.0198(7) Uani 1 1 d . . . C2 C 0.2336(4) 0.0722(3) 0.36310(13) 0.0211(7) Uani 1 1 d . . . C3 C 0.0823(4) 0.0944(3) 0.28229(13) 0.0205(8) Uani 1 1 d . . . C4 C 0.3987(5) 0.0844(3) 0.28456(14) 0.0242(8) Uani 1 1 d . . . C5 C 0.1471(7) 0.0079(4) 0.10958(18) 0.0426(14) Uani 1 1 d . . . C6 C 0.0352(6) 0.0639(5) 0.12308(19) 0.0479(16) Uani 1 1 d . . . C7 C 0.0470(5) 0.1255(4) 0.15903(17) 0.0368(12) Uani 1 1 d . . . C8 C 0.1712(5) 0.1274(3) 0.18075(13) 0.0285(9) Uani 1 1 d . . . C9 C 0.2753(5) 0.0715(4) 0.16633(15) 0.0337(11) Uani 1 1 d . . . C10 C 0.2620(7) 0.0113(3) 0.13031(16) 0.0409(13) Uani 1 1 d . . . C11 C 0.3938(6) 0.0174(4) 0.10713(19) 0.0399(13) Uani 1 1 d . . . C12 C 0.3930(6) 0.0174(4) 0.06556(18) 0.0401(12) Uani 1 1 d . . . C13 C 0.2640(7) 0.0117(4) 0.04310(17) 0.0417(13) Uani 1 1 d . . . C14 C 0.1474(8) 0.0079(4) 0.06380(18) 0.0452(15) Uani 1 1 d . . . C15 C 0.0333(6) 0.0651(5) 0.05064(18) 0.0467(16) Uani 1 1 d . . . C16 C -0.0358(5) 0.0997(4) 0.0867(2) 0.0420(13) Uani 1 1 d . . . C17 C 0.1902(6) 0.2292(4) 0.19477(15) 0.0392(12) Uani 1 1 d . . . C18 C 0.4061(5) 0.1151(4) 0.16664(15) 0.0356(11) Uani 1 1 d . . . C19 C 0.4774(5) 0.0810(4) 0.12999(15) 0.0305(10) Uani 1 1 d . . . C20 C 0.4786(5) 0.0816(4) 0.04390(17) 0.0334(11) Uani 1 1 d . . . C21 C 0.4061(5) 0.1152(4) 0.00735(17) 0.0397(13) Uani 1 1 d . . . C22 C 0.2752(6) 0.0718(4) 0.00745(17) 0.0390(12) Uani 1 1 d . . . C23 C 0.1709(5) 0.1281(3) -0.00642(14) 0.0295(9) Uani 1 1 d . . . C24 C 0.0471(5) 0.1268(4) 0.01456(17) 0.0361(11) Uani 1 1 d . . . C25 C 0.4239(6) 0.2115(5) 0.18060(15) 0.0387(12) Uani 1 1 d . . . C26 C 0.5627(4) 0.1462(4) 0.10983(15) 0.0288(9) Uani 1 1 d . . . C27 C 0.5638(4) 0.1460(4) 0.06480(15) 0.0282(9) Uani 1 1 d . . . C28 C 0.4232(6) 0.2107(5) -0.00677(15) 0.0399(13) Uani 1 1 d . . . C29 C 0.1903(7) 0.2290(4) -0.02084(15) 0.0431(14) Uani 1 1 d . . . C30 C 0.5101(5) 0.2771(4) 0.15935(19) 0.0415(13) Uani 1 1 d . . . C31 C 0.5784(4) 0.2446(4) 0.12491(18) 0.0369(11) Uani 1 1 d . . . C32 C 0.5904(5) 0.3099(5) 0.0861(2) 0.0492(16) Uani 1 1 d . . . C33 C 0.5788(4) 0.2436(4) 0.04929(16) 0.0326(10) Uani 1 1 d . . . C34 C 0.5102(5) 0.2756(4) 0.01448(16) 0.0392(13) Uani 1 1 d . . . C35 C 0.1551(11) -0.2423(6) 0.1175(3) 0.0230(16) Uani 0.50 1 d PU A -1 C36 C 0.191(2) -0.2499(14) 0.1588(4) 0.032(3) Uani 0.50 1 d PU A -1 H36 H 0.1229 -0.2468 0.1792 0.039 Uiso 0.50 1 calc PR A -1 C37 C 0.3176(19) -0.2615(15) 0.1714(4) 0.033(3) Uani 0.50 1 d PU A -1 H37 H 0.3381 -0.2668 0.2000 0.040 Uiso 0.50 1 calc PR A -1 C38 C 0.4159(11) -0.2655(8) 0.1423(4) 0.039(2) Uani 0.50 1 d PU A -1 H38 H 0.5050 -0.2743 0.1509 0.046 Uiso 0.50 1 calc PR A -1 C39 C 0.3884(12) -0.2571(8) 0.1011(4) 0.036(2) Uani 0.50 1 d PU A -1 H39 H 0.4577 -0.2600 0.0812 0.043 Uiso 0.50 1 calc PR A -1 C40 C 0.257(6) -0.244(5) 0.0883(3) 0.027(6) Uani 0.50 1 d PU A -1 H40 H 0.2374 -0.2365 0.0597 0.032 Uiso 0.50 1 calc PR A -1 C41 C 0.0146(11) -0.2310(9) 0.1041(4) 0.040(2) Uani 0.50 1 d PU A -1 H41A H -0.0384 -0.2062 0.1273 0.060 Uiso 0.50 1 calc PR A -1 H41B H -0.0202 -0.2948 0.0952 0.060 Uiso 0.50 1 calc PR A -1 H41C H 0.0099 -0.1846 0.0809 0.060 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 Hg1 0.03184(12) 0.01024(9) 0.02708(11) 0.000 0.000 -0.00134(8) Co1 0.0217(2) 0.0099(2) 0.0181(2) 0.00080(16) 0.0006(2) -0.00106(18) O1 0.0225(15) 0.0132(12) 0.0465(19) 0.0000(12) -0.0002(13) -0.0023(11) O2 0.049(2) 0.0353(18) 0.0215(15) -0.0002(13) -0.0036(14) -0.0126(16) O3 0.0313(17) 0.0237(15) 0.0351(18) -0.0045(13) -0.0089(14) 0.0057(13) O4 0.0340(18) 0.0260(17) 0.047(2) -0.0061(15) 0.0168(16) -0.0067(14) C1 0.0193(17) 0.0154(16) 0.0249(18) 0.0035(13) -0.0001(14) -0.0017(14) C2 0.0224(19) 0.0180(17) 0.0229(18) 0.0000(14) -0.0019(14) -0.0051(15) C3 0.0261(19) 0.0131(16) 0.0223(18) -0.0007(14) -0.0008(15) 0.0016(14) C4 0.030(2) 0.0133(16) 0.029(2) -0.0027(15) 0.0069(17) -0.0048(15) C5 0.073(4) 0.018(2) 0.037(3) 0.0021(19) 0.010(3) -0.015(2) C6 0.049(3) 0.051(3) 0.044(3) 0.026(3) -0.013(3) -0.037(3) C7 0.029(2) 0.036(3) 0.045(3) 0.019(2) 0.017(2) -0.003(2) C8 0.040(3) 0.027(2) 0.0177(18) 0.0088(16) 0.0074(17) -0.0042(19) C9 0.048(3) 0.030(2) 0.023(2) 0.0171(17) 0.0034(19) 0.006(2) C10 0.074(4) 0.0162(19) 0.033(2) 0.0077(17) 0.005(3) 0.005(2) C11 0.046(3) 0.021(2) 0.053(3) 0.001(2) -0.011(3) 0.017(2) C12 0.050(3) 0.025(2) 0.046(3) -0.002(2) 0.007(2) 0.016(2) C13 0.069(4) 0.019(2) 0.038(3) -0.0113(18) -0.005(3) 0.005(2) C14 0.083(5) 0.015(2) 0.038(3) -0.0018(19) -0.017(3) -0.015(2) C15 0.047(3) 0.053(3) 0.040(3) -0.025(3) 0.010(2) -0.036(3) C16 0.030(3) 0.041(3) 0.055(3) -0.005(3) -0.002(2) -0.015(2) C17 0.062(4) 0.035(3) 0.021(2) -0.0002(18) 0.009(2) -0.004(2) C18 0.031(2) 0.048(3) 0.028(2) 0.019(2) -0.0016(18) 0.012(2) C19 0.029(2) 0.032(2) 0.030(2) 0.0093(19) -0.0041(18) 0.0134(19) C20 0.030(2) 0.027(2) 0.043(3) -0.007(2) 0.010(2) 0.0129(19) C21 0.035(3) 0.048(3) 0.035(3) -0.025(2) 0.007(2) 0.011(2) C22 0.048(3) 0.029(2) 0.040(3) -0.022(2) -0.006(2) 0.010(2) C23 0.043(3) 0.026(2) 0.0195(19) -0.0098(16) -0.0030(18) 0.0004(19) C24 0.034(2) 0.037(3) 0.038(3) -0.018(2) -0.016(2) 0.003(2) C25 0.041(3) 0.055(3) 0.020(2) -0.004(2) -0.0158(19) 0.018(2) C26 0.0171(18) 0.035(2) 0.034(2) 0.0047(19) -0.0020(16) 0.0135(17) C27 0.0174(18) 0.030(2) 0.038(2) 0.0013(19) 0.0051(17) 0.0091(16) C28 0.046(3) 0.052(3) 0.022(2) -0.001(2) 0.014(2) 0.021(3) C29 0.075(4) 0.036(3) 0.018(2) -0.0029(18) -0.003(2) 0.001(3) C30 0.032(3) 0.044(3) 0.048(3) -0.014(2) -0.025(2) 0.007(2) C31 0.0166(19) 0.042(3) 0.052(3) -0.004(3) -0.0123(19) 0.005(2) C32 0.0114(19) 0.043(3) 0.094(5) -0.003(3) 0.004(2) -0.009(2) C33 0.0196(19) 0.039(3) 0.039(2) 0.003(2) 0.0135(17) 0.0050(19) C34 0.037(3) 0.048(3) 0.033(2) 0.016(2) 0.021(2) 0.013(2) C35 0.027(4) 0.013(4) 0.029(4) -0.005(3) 0.000(4) -0.004(3) C36 0.057(7) 0.024(5) 0.015(6) -0.002(6) 0.010(6) 0.009(5) C37 0.043(6) 0.032(7) 0.025(8) 0.001(6) -0.014(7) 0.004(5) C38 0.029(5) 0.038(6) 0.048(6) 0.008(5) -0.013(4) -0.001(4) C39 0.033(6) 0.028(5) 0.047(6) 0.007(5) 0.017(5) -0.001(4) C40 0.042(11) 0.015(13) 0.024(3) 0.003(7) 0.013(11) 0.002(9) C41 0.035(6) 0.045(6) 0.040(6) 0.002(5) -0.007(4) 0.006(5) _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 Hg1 Co1 2.5050(5) 2 ? Hg1 Co1 2.5050(5) . ? Co1 C4 1.788(4) . ? Co1 C1 1.802(4) . ? Co1 C3 1.806(4) . ? Co1 C2 1.817(4) . ? O1 C1 1.129(5) . ? O2 C2 1.135(5) . ? O3 C3 1.134(5) . ? O4 C4 1.143(5) . ? C5 C10 1.340(9) . ? C5 C6 1.432(10) . ? C5 C14 1.476(8) . ? C6 C7 1.436(9) . ? C6 C16 1.460(8) . ? C7 C8 1.437(8) . ? C7 C30 1.447(8) 2 ? C8 C9 1.380(7) . ? C8 C17 1.471(7) . ? C9 C10 1.429(7) . ? C9 C18 1.448(8) . ? C10 C11 1.529(9) . ? C11 C12 1.341(8) . ? C11 C19 1.417(8) . ? C12 C20 1.415(8) . ? C12 C13 1.493(9) . ? C13 C14 1.355(10) . ? C13 C22 1.416(8) . ? C14 C15 1.455(10) . ? C15 C16 1.435(8) . ? C15 C24 1.443(9) . ? C16 C32 1.350(9) 2 ? C17 C17 1.336(12) 2 ? C17 C25 1.480(8) 2 ? C18 C25 1.401(8) . ? C18 C19 1.460(7) . ? C19 C26 1.398(7) . ? C20 C27 1.401(7) . ? C20 C21 1.461(8) . ? C21 C28 1.390(9) . ? C21 C22 1.449(8) . ? C22 C23 1.378(7) . ? C23 C24 1.422(7) . ? C23 C29 1.465(7) . ? C24 C34 1.449(7) 2 ? C25 C30 1.424(9) . ? C25 C17 1.480(8) 2 ? C26 C31 1.435(7) . ? C26 C27 1.453(7) . ? C27 C33 1.429(7) . ? C28 C34 1.423(9) . ? C28 C29 1.481(8) 2 ? C29 C29 1.336(13) 2 ? C29 C28 1.481(8) 2 ? C30 C31 1.381(8) . ? C30 C7 1.447(8) 2 ? C31 C32 1.541(9) . ? C32 C16 1.350(9) 2 ? C32 C33 1.496(9) . ? C33 C34 1.389(7) . ? C34 C24 1.449(7) 2 ? C35 C36 1.383(18) . ? C35 C40 1.39(4) . ? C35 C41 1.492(15) . ? C36 C37 1.355(16) . ? C37 C38 1.37(2) . ? C38 C39 1.361(17) . ? C39 C40 1.40(6) . ? 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 Co1 Hg1 Co1 178.95(3) 2 . ? C4 Co1 C1 95.43(18) . . ? C4 Co1 C3 125.8(2) . . ? C1 Co1 C3 96.45(18) . . ? C4 Co1 C2 114.8(2) . . ? C1 Co1 C2 101.92(18) . . ? C3 Co1 C2 113.88(19) . . ? C4 Co1 Hg1 79.88(13) . . ? C1 Co1 Hg1 170.99(13) . . ? C3 Co1 Hg1 80.39(13) . . ? C2 Co1 Hg1 87.06(13) . . ? O1 C1 Co1 178.2(4) . . ? O2 C2 Co1 178.5(4) . . ? O3 C3 Co1 177.6(4) . . ? O4 C4 Co1 176.4(4) . . ? C10 C5 C6 120.9(5) . . ? C10 C5 C14 119.8(6) . . ? C6 C5 C14 107.8(6) . . ? C5 C6 C7 119.5(5) . . ? C5 C6 C16 108.7(6) . . ? C7 C6 C16 119.7(6) . . ? C6 C7 C8 118.5(5) . . ? C6 C7 C30 120.6(5) . 2 ? C8 C7 C30 109.1(5) . 2 ? C9 C8 C7 119.4(5) . . ? C9 C8 C17 121.6(5) . . ? C7 C8 C17 106.3(5) . . ? C8 C9 C10 121.3(5) . . ? C8 C9 C18 117.8(5) . . ? C10 C9 C18 109.1(5) . . ? C5 C10 C9 120.5(6) . . ? C5 C10 C11 120.8(5) . . ? C9 C10 C11 106.5(5) . . ? C12 C11 C19 121.6(6) . . ? C12 C11 C10 118.9(5) . . ? C19 C11 C10 107.3(5) . . ? C11 C12 C20 119.3(6) . . ? C11 C12 C13 119.4(6) . . ? C20 C12 C13 109.0(5) . . ? C14 C13 C22 119.5(6) . . ? C14 C13 C12 121.4(5) . . ? C22 C13 C12 107.1(5) . . ? C13 C14 C15 121.6(5) . . ? C13 C14 C5 119.6(6) . . ? C15 C14 C5 106.9(6) . . ? C16 C15 C24 120.6(6) . . ? C16 C15 C14 109.0(6) . . ? C24 C15 C14 118.1(5) . . ? C32 C16 C15 119.1(6) 2 . ? C32 C16 C6 121.1(6) 2 . ? C15 C16 C6 107.6(6) . . ? C17 C17 C8 121.3(7) 2 . ? C17 C17 C25 118.2(6) 2 2 ? C8 C17 C25 108.6(5) . 2 ? C25 C18 C9 120.2(5) . . ? C25 C18 C19 119.7(5) . . ? C9 C18 C19 108.3(5) . . ? C26 C19 C11 120.9(5) . . ? C26 C19 C18 118.6(5) . . ? C11 C19 C18 108.8(5) . . ? C27 C20 C12 121.6(5) . . ? C27 C20 C21 120.0(5) . . ? C12 C20 C21 106.6(5) . . ? C28 C21 C22 119.7(5) . . ? C28 C21 C20 119.7(5) . . ? C22 C21 C20 109.1(5) . . ? C23 C22 C13 121.6(6) . . ? C23 C22 C21 118.1(5) . . ? C13 C22 C21 108.1(5) . . ? C22 C23 C24 120.8(5) . . ? C22 C23 C29 121.5(5) . . ? C24 C23 C29 106.2(5) . . ? C23 C24 C15 118.4(5) . . ? C23 C24 C34 109.9(5) . 2 ? C15 C24 C34 119.8(5) . 2 ? C18 C25 C30 120.9(5) . . ? C18 C25 C17 120.8(5) . 2 ? C30 C25 C17 106.3(5) . 2 ? C19 C26 C31 120.3(5) . . ? C19 C26 C27 117.9(5) . . ? C31 C26 C27 109.9(4) . . ? C20 C27 C33 118.6(5) . . ? C20 C27 C26 118.6(5) . . ? C33 C27 C26 110.4(4) . . ? C21 C28 C34 120.1(5) . . ? C21 C28 C29 121.6(6) . 2 ? C34 C28 C29 106.3(5) . 2 ? C29 C29 C23 121.6(7) 2 . ? C29 C29 C28 117.4(6) 2 2 ? C23 C29 C28 108.7(5) . 2 ? C31 C30 C25 119.4(5) . . ? C31 C30 C7 119.2(6) . 2 ? C25 C30 C7 109.7(5) . 2 ? C30 C31 C26 121.1(5) . . ? C30 C31 C32 120.5(5) . . ? C26 C31 C32 105.8(5) . . ? C16 C32 C33 122.0(6) 2 . ? C16 C32 C31 118.9(6) 2 . ? C33 C32 C31 106.9(5) . . ? C34 C33 C27 121.5(5) . . ? C34 C33 C32 119.4(5) . . ? C27 C33 C32 107.0(5) . . ? C33 C34 C28 120.1(5) . . ? C33 C34 C24 119.1(5) . 2 ? C28 C34 C24 108.9(5) . 2 ? C36 C35 C40 117(2) . . ? C36 C35 C41 122.2(11) . . ? C40 C35 C41 120.6(19) . . ? C37 C36 C35 122.9(11) . . ? C36 C37 C38 119.1(11) . . ? C39 C38 C37 121.2(11) . . ? C38 C39 C40 119.4(13) . . ? C35 C40 C39 120.3(16) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 33.63 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.580 _refine_diff_density_min -1.486 _refine_diff_density_rms 0.131 _iucr_refine_instructions_details ; TITL fb06 in Pccn Hg[Co(CO)4)]2.C60.toluene CELL 0.7749 10.1012 13.6265 32.2524 90.000 90.000 90.000 ZERR 4 0.0004 0.0006 0.0013 0.000 0.000 0.000 LATT 1 SYMM 1/2-X,1/2-Y,Z SYMM 1/2+X,-Y,1/2-Z SYMM -X,1/2+Y,1/2-Z SFAC C H O CO HG DISP C 0.00337 0.00172 DISP O 0.01153 0.00645 DISP HG -2.64127 9.64453 DISP CO 0.35144 1.02359 UNIT 300 32 32 8 4 temp -173 SIMU c35 > c41 SIZE 0.009 0.010 0.003 !black plate ACTA L.S. 8 WGHT 0.000000 26.949501 FVAR 0.07574 HG1 5 0.250000 0.250000 0.307545 10.50000 0.03184 0.01024 = 0.02708 0.00000 0.00000 -0.00134 CO1 4 0.238469 0.066373 0.306831 11.00000 0.02166 0.00993 = 0.01806 0.00080 0.00060 -0.00106 O1 3 0.230455 -0.145235 0.290795 11.00000 0.02255 0.01321 = 0.04647 -0.00001 -0.00021 -0.00230 O2 3 0.230956 0.073573 0.398257 11.00000 0.04933 0.03531 = 0.02152 -0.00015 -0.00365 -0.01260 O3 3 -0.017001 0.108759 0.267068 11.00000 0.03128 0.02373 = 0.03508 -0.00449 -0.00889 0.00571 O4 3 0.503412 0.091910 0.271514 11.00000 0.03404 0.02598 = 0.04680 -0.00607 0.01679 -0.00668 C1 1 0.233495 -0.063997 0.297634 11.00000 0.01926 0.01535 = 0.02491 0.00353 -0.00009 -0.00173 C2 1 0.233594 0.072171 0.363095 11.00000 0.02241 0.01802 = 0.02294 0.00000 -0.00185 -0.00514 C3 1 0.082343 0.094449 0.282291 11.00000 0.02615 0.01310 = 0.02229 -0.00072 -0.00082 0.00158 C4 1 0.398698 0.084405 0.284558 11.00000 0.02996 0.01332 = 0.02944 -0.00275 0.00691 -0.00476 C5 1 0.147120 0.007851 0.109577 11.00000 0.07326 0.01775 = 0.03682 0.00206 0.01018 -0.01489 C6 1 0.035191 0.063905 0.123082 11.00000 0.04862 0.05080 = 0.04430 0.02639 -0.01325 -0.03702 C7 1 0.046957 0.125474 0.159031 11.00000 0.02941 0.03605 = 0.04502 0.01933 0.01666 -0.00253 C8 1 0.171157 0.127412 0.180746 11.00000 0.04042 0.02732 = 0.01769 0.00884 0.00740 -0.00422 C9 1 0.275301 0.071497 0.166335 11.00000 0.04809 0.02960 = 0.02347 0.01709 0.00342 0.00588 C10 1 0.261995 0.011258 0.130306 11.00000 0.07384 0.01621 = 0.03273 0.00772 0.00473 0.00478 C11 1 0.393838 0.017409 0.107132 11.00000 0.04562 0.02109 = 0.05306 0.00104 -0.01150 0.01708 C12 1 0.393016 0.017401 0.065563 11.00000 0.04957 0.02517 = 0.04561 -0.00194 0.00739 0.01550 C13 1 0.263999 0.011710 0.043097 11.00000 0.06860 0.01851 = 0.03786 -0.01126 -0.00511 0.00547 C14 1 0.147373 0.007904 0.063802 11.00000 0.08276 0.01525 = 0.03758 -0.00182 -0.01703 -0.01515 C15 1 0.033280 0.065138 0.050642 11.00000 0.04704 0.05260 = 0.04047 -0.02533 0.00955 -0.03571 C16 1 -0.035792 0.099685 0.086673 11.00000 0.03015 0.04123 = 0.05453 -0.00464 -0.00153 -0.01488 C17 1 0.190171 0.229153 0.194774 11.00000 0.06234 0.03455 = 0.02075 -0.00022 0.00892 -0.00363 C18 1 0.406087 0.115050 0.166643 11.00000 0.03063 0.04822 = 0.02800 0.01913 -0.00160 0.01233 C19 1 0.477379 0.081027 0.129988 11.00000 0.02892 0.03225 = 0.03033 0.00925 -0.00411 0.01342 C20 1 0.478610 0.081595 0.043897 11.00000 0.03013 0.02668 = 0.04330 -0.00706 0.00971 0.01289 C21 1 0.406138 0.115198 0.007351 11.00000 0.03512 0.04834 = 0.03549 -0.02506 0.00660 0.01098 C22 1 0.275212 0.071826 0.007452 11.00000 0.04777 0.02931 = 0.03997 -0.02208 -0.00600 0.01006 C23 1 0.170883 0.128052 -0.006419 11.00000 0.04304 0.02584 = 0.01950 -0.00983 -0.00304 0.00045 C24 1 0.047069 0.126847 0.014558 11.00000 0.03350 0.03716 = 0.03756 -0.01782 -0.01609 0.00273 C25 1 0.423881 0.211482 0.180597 11.00000 0.04118 0.05461 = 0.02036 -0.00381 -0.01578 0.01759 C26 1 0.562686 0.146204 0.109835 11.00000 0.01712 0.03543 = 0.03388 0.00468 -0.00196 0.01350 C27 1 0.563766 0.145957 0.064800 11.00000 0.01737 0.02968 = 0.03756 0.00133 0.00512 0.00906 C28 1 0.423176 0.210736 -0.006771 11.00000 0.04603 0.05153 = 0.02204 -0.00059 0.01415 0.02144 C29 1 0.190286 0.228954 -0.020838 11.00000 0.07511 0.03639 = 0.01783 -0.00294 -0.00298 0.00076 C30 1 0.510054 0.277136 0.159353 11.00000 0.03160 0.04435 = 0.04847 -0.01370 -0.02516 0.00690 C31 1 0.578391 0.244626 0.124908 11.00000 0.01657 0.04198 = 0.05217 -0.00409 -0.01226 0.00488 C32 1 0.590369 0.309857 0.086074 11.00000 0.01138 0.04268 = 0.09368 -0.00325 0.00417 -0.00896 C33 1 0.578763 0.243596 0.049288 11.00000 0.01963 0.03875 = 0.03933 0.00322 0.01350 0.00504 C34 1 0.510214 0.275649 0.014482 11.00000 0.03672 0.04819 = 0.03263 0.01563 0.02130 0.01330 PART -1 C35 1 0.155141 -0.242312 0.117472 10.50000 0.02739 0.01282 = 0.02872 -0.00509 0.00007 -0.00388 C36 1 0.190588 -0.249881 0.158772 10.50000 0.05707 0.02376 = 0.01545 -0.00249 0.00990 0.00925 AFIX 43 H36 2 0.122941 -0.246813 0.179194 10.50000 -1.20000 AFIX 0 C37 1 0.317589 -0.261480 0.171372 10.50000 0.04318 0.03167 = 0.02469 0.00140 -0.01356 0.00374 AFIX 43 H37 2 0.338060 -0.266763 0.200034 10.50000 -1.20000 AFIX 0 C38 1 0.415924 -0.265479 0.142264 10.50000 0.02923 0.03825 = 0.04819 0.00773 -0.01327 -0.00067 AFIX 43 H38 2 0.505020 -0.274266 0.150936 10.50000 -1.20000 AFIX 0 C39 1 0.388450 -0.257101 0.101108 10.50000 0.03298 0.02834 = 0.04727 0.00694 0.01688 -0.00086 AFIX 43 H39 2 0.457723 -0.260034 0.081225 10.50000 -1.20000 AFIX 0 C40 1 0.257138 -0.244119 0.088347 10.50000 0.04185 0.01458 = 0.02396 0.00287 0.01255 0.00187 AFIX 43 H40 2 0.237440 -0.236509 0.059725 10.50000 -1.20000 AFIX 0 C41 1 0.014571 -0.230989 0.104061 10.50000 0.03452 0.04490 = 0.03965 0.00204 -0.00723 0.00558 AFIX 137 H41A 2 -0.038351 -0.206169 0.127268 10.50000 -1.50000 H41B 2 -0.020163 -0.294789 0.095210 10.50000 -1.50000 H41C 2 0.009916 -0.184572 0.080897 10.50000 -1.50000 PART 0 HKLF 4 REM fb06 in Pccn Hg[Co(CO)4)]2.C60.toluene REM R1 = 0.0490 for 5807 Fo > 4sig(Fo) and 0.0565 for all 6752 data REM 421 parameters refined using 42 restraints END WGHT 0.0000 26.9208 REM Highest difference peak 1.580, deepest hole -1.486, 1-sigma level 0.131 Q1 1 0.5763 0.3336 0.1133 11.00000 0.05 1.58 Q2 1 0.2746 0.2001 -0.0179 11.00000 0.05 1.57 Q3 1 0.2971 -0.0092 0.0899 11.00000 0.05 1.45 Q4 1 0.2715 0.1972 0.1958 11.00000 0.05 1.45 Q5 1 0.5752 0.3317 0.0627 11.00000 0.05 1.17 Q6 1 0.4332 0.0294 0.0870 11.00000 0.05 1.01 Q7 1 -0.0112 0.1162 0.0480 11.00000 0.05 0.99 Q8 1 0.0666 0.0305 0.0712 11.00000 0.05 0.98 Q9 1 0.2571 0.0456 0.0274 11.00000 0.05 0.84 Q10 1 0.4017 0.0779 0.0260 11.00000 0.05 0.79 ;