Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof G. Bowmaker' _publ_contact_author_address ; Department of Chemistry University of Auckland Private Bag 92019 Auckland NEW ZEALAND ; _publ_contact_author_email G.BOWMAKER@AUCKLAND.AC.NZ _publ_section_title ; Structural and spectroscopic studies on mercury(II) tribenzylphosphine complexes ; loop_ _publ_author_name 'G. Bowmaker' 'Eric M. Ainscough' 'Behnam Assadollahzadeh' 'Andrew M. Brodie' ; G.Freeman ; 'Geoffrey B. Jameson' data_1_tetrafluoroborate _database_code_depnum_ccdc_archive 'CCDC 259223' #----------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 B2 F8 Hg P2' _chemical_formula_weight 982.91 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6436(2) _cell_length_b 10.0096(2) _cell_length_c 20.4090(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.5320(10) _cell_angle_gamma 90.00 _cell_volume 1936.86(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3956 _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 26.38 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 4.126 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2761 _exptl_absorpt_correction_T_max 0.5582 _exptl_absorpt_process_details 'blessing, Acta Cryst., (1995) A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Siemens SMART' _diffrn_measurement_method 'Area dectector /w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3956 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.38 _reflns_number_total 3956 _reflns_number_gt 3562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0198P)^2^+1.0548P] 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 SHELXL _refine_ls_extinction_coef 0.00079(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3956 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0189 _refine_ls_R_factor_gt 0.0157 _refine_ls_wR_factor_ref 0.0405 _refine_ls_wR_factor_gt 0.0394 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 Hg1 Hg 1.0000 1.0000 0.0000 0.01818(5) Uani 1 2 d S . . P1 P 0.89302(5) 0.85892(5) 0.07205(2) 0.01700(10) Uani 1 1 d . . . B1 B 0.6974(3) 0.6133(2) 0.18838(12) 0.0261(5) Uani 1 1 d . . . F11 F 0.61344(17) 0.53924(17) 0.22224(8) 0.0463(4) Uani 1 1 d . . . F12 F 0.82990(16) 0.5568(2) 0.19370(9) 0.0560(4) Uani 1 1 d . . . F13 F 0.63420(15) 0.61851(14) 0.12126(6) 0.0383(3) Uani 1 1 d . . . F14 F 0.71182(16) 0.74247(15) 0.21241(8) 0.0465(4) Uani 1 1 d . . . C11 C 0.70540(19) 0.8956(2) 0.05794(10) 0.0220(4) Uani 1 1 d . . . H11A H 0.6591 0.8568 0.0149 0.026 Uiso 1 1 calc R . . H11B H 0.6627 0.8547 0.0937 0.026 Uiso 1 1 calc R . . C12 C 0.68199(19) 1.0453(2) 0.05711(10) 0.0197(4) Uani 1 1 d . . . C13 C 0.6835(2) 1.1156(2) 0.11623(10) 0.0244(4) Uani 1 1 d . . . H13 H 0.6980 1.0693 0.1576 0.029 Uiso 1 1 calc R . . C14 C 0.6639(2) 1.2533(2) 0.11487(11) 0.0287(5) Uani 1 1 d . . . H14 H 0.6662 1.3010 0.1553 0.034 Uiso 1 1 calc R . . C15 C 0.6410(2) 1.3211(2) 0.05481(12) 0.0302(5) Uani 1 1 d . . . H15 H 0.6260 1.4150 0.0540 0.036 Uiso 1 1 calc R . . C16 C 0.6400(2) 1.2525(2) -0.00425(11) 0.0273(4) Uani 1 1 d . . . H16 H 0.6247 1.2992 -0.0455 0.033 Uiso 1 1 calc R . . C17 C 0.6613(2) 1.1149(2) -0.00297(10) 0.0231(4) Uani 1 1 d . . . H17 H 0.6618 1.0681 -0.0434 0.028 Uiso 1 1 calc R . . C21 C 0.9697(2) 0.8948(2) 0.15825(9) 0.0233(4) Uani 1 1 d . . . H21A H 0.9334 0.9814 0.1713 0.028 Uiso 1 1 calc R . . H21B H 0.9413 0.8246 0.1873 0.028 Uiso 1 1 calc R . . C22 C 1.1288(2) 0.9004(2) 0.16813(9) 0.0205(4) Uani 1 1 d . . . C23 C 1.1968(2) 1.0227(2) 0.16493(11) 0.0259(4) Uani 1 1 d . . . H23 H 1.1427 1.1019 0.1552 0.031 Uiso 1 1 calc R . . C24 C 1.3429(3) 1.0293(2) 0.17590(12) 0.0325(5) Uani 1 1 d . . . H24 H 1.3884 1.1131 0.1741 0.039 Uiso 1 1 calc R . . C25 C 1.4229(2) 0.9135(3) 0.18953(10) 0.0324(5) Uani 1 1 d . . . H25 H 1.5229 0.9181 0.1975 0.039 Uiso 1 1 calc R . . C26 C 1.3557(2) 0.7915(2) 0.19137(10) 0.0297(5) Uani 1 1 d . . . H26 H 1.4100 0.7121 0.1997 0.036 Uiso 1 1 calc R . . C27 C 1.2100(2) 0.7849(2) 0.18114(9) 0.0239(4) Uani 1 1 d . . . H27 H 1.1649 0.7009 0.1830 0.029 Uiso 1 1 calc R . . C31 C 0.9233(2) 0.6843(2) 0.05502(9) 0.0212(4) Uani 1 1 d . . . H31A H 1.0249 0.6639 0.0689 0.025 Uiso 1 1 calc R . . H31B H 0.8703 0.6276 0.0816 0.025 Uiso 1 1 calc R . . C32 C 0.87809(19) 0.65124(18) -0.01788(9) 0.0187(4) Uani 1 1 d . . . C33 C 0.7401(2) 0.6124(2) -0.04307(10) 0.0248(4) Uani 1 1 d . . . H33 H 0.6730 0.6083 -0.0143 0.030 Uiso 1 1 calc R . . C34 C 0.6999(2) 0.5796(2) -0.10983(11) 0.0288(5) Uani 1 1 d . . . H34 H 0.6057 0.5526 -0.1267 0.035 Uiso 1 1 calc R . . C35 C 0.7971(2) 0.5860(2) -0.15207(10) 0.0290(5) Uani 1 1 d . . . H35 H 0.7695 0.5633 -0.1978 0.035 Uiso 1 1 calc R . . C36 C 0.9346(2) 0.6255(2) -0.12771(10) 0.0275(4) Uani 1 1 d . . . H36 H 1.0013 0.6300 -0.1567 0.033 Uiso 1 1 calc R . . C37 C 0.9746(2) 0.6585(2) -0.06094(10) 0.0231(4) Uani 1 1 d . . . H37 H 1.0687 0.6862 -0.0444 0.028 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 Hg1 0.01956(6) 0.01802(6) 0.01717(6) 0.00028(4) 0.00392(4) -0.00093(4) P1 0.0180(2) 0.0180(2) 0.0150(2) -0.00054(18) 0.00297(17) 0.00087(18) B1 0.0277(12) 0.0263(12) 0.0254(11) 0.0051(9) 0.0082(9) 0.0028(9) F11 0.0525(9) 0.0518(9) 0.0380(8) 0.0165(7) 0.0177(7) -0.0087(7) F12 0.0410(9) 0.0667(11) 0.0627(11) 0.0207(9) 0.0158(8) 0.0275(8) F13 0.0519(8) 0.0376(8) 0.0243(6) 0.0049(5) 0.0041(6) -0.0040(6) F14 0.0499(9) 0.0370(8) 0.0517(9) -0.0145(7) 0.0071(7) -0.0064(6) C11 0.0177(9) 0.0220(10) 0.0261(10) 0.0011(8) 0.0036(7) 0.0007(7) C12 0.0134(8) 0.0199(9) 0.0255(10) 0.0014(8) 0.0029(7) 0.0000(7) C13 0.0252(10) 0.0263(11) 0.0233(10) 0.0021(8) 0.0085(8) 0.0013(8) C14 0.0289(11) 0.0285(12) 0.0304(11) -0.0071(9) 0.0098(9) 0.0014(8) C15 0.0266(11) 0.0208(10) 0.0441(13) 0.0008(9) 0.0088(9) 0.0022(8) C16 0.0251(10) 0.0258(11) 0.0300(11) 0.0086(9) 0.0024(8) 0.0018(8) C17 0.0205(9) 0.0269(11) 0.0210(9) -0.0003(8) 0.0011(7) 0.0005(8) C21 0.0226(9) 0.0311(11) 0.0164(9) -0.0048(8) 0.0038(7) 0.0012(8) C22 0.0241(10) 0.0246(10) 0.0122(8) -0.0025(7) 0.0015(7) -0.0001(8) C23 0.0339(12) 0.0233(11) 0.0198(10) -0.0009(8) 0.0029(9) 0.0014(8) C24 0.0364(13) 0.0354(13) 0.0255(11) -0.0017(9) 0.0049(9) -0.0140(10) C25 0.0225(10) 0.0511(14) 0.0234(11) -0.0046(10) 0.0038(8) -0.0018(10) C26 0.0297(11) 0.0357(12) 0.0225(10) -0.0033(9) 0.0014(8) 0.0103(9) C27 0.0299(10) 0.0215(10) 0.0186(9) -0.0015(8) 0.0001(8) 0.0015(8) C31 0.0254(10) 0.0187(9) 0.0191(9) 0.0010(7) 0.0032(7) 0.0030(7) C32 0.0235(9) 0.0140(9) 0.0179(9) 0.0007(7) 0.0024(7) 0.0032(7) C33 0.0265(10) 0.0217(10) 0.0275(10) -0.0010(8) 0.0084(8) -0.0027(8) C34 0.0291(11) 0.0265(11) 0.0279(11) -0.0038(9) -0.0028(8) -0.0022(8) C35 0.0434(13) 0.0230(10) 0.0181(10) -0.0022(8) -0.0009(9) 0.0062(9) C36 0.0360(11) 0.0254(11) 0.0234(10) 0.0010(8) 0.0117(8) 0.0071(9) C37 0.0225(10) 0.0229(10) 0.0244(10) 0.0000(8) 0.0057(8) 0.0037(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 Hg1 P1 2.4032(5) 3_775 ? Hg1 P1 2.4032(5) . ? P1 C21 1.8152(19) . ? P1 C31 1.816(2) . ? P1 C11 1.8169(19) . ? B1 F11 1.374(3) . ? B1 F14 1.380(3) . ? B1 F12 1.384(3) . ? B1 F13 1.395(3) . ? C11 C12 1.514(3) . ? C12 C17 1.393(3) . ? C12 C13 1.395(3) . ? C13 C14 1.391(3) . ? C14 C15 1.383(3) . ? C15 C16 1.386(3) . ? C16 C17 1.392(3) . ? C21 C22 1.511(3) . ? C22 C27 1.395(3) . ? C22 C23 1.396(3) . ? C23 C24 1.387(3) . ? C24 C25 1.392(4) . ? C25 C26 1.386(3) . ? C26 C27 1.384(3) . ? C31 C32 1.509(3) . ? C32 C33 1.392(3) . ? C32 C37 1.394(3) . ? C33 C34 1.386(3) . ? C34 C35 1.386(3) . ? C35 C36 1.386(3) . ? C36 C37 1.386(3) . ? 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 P1 Hg1 P1 180.0 3_775 . ? C21 P1 C31 108.92(9) . . ? C21 P1 C11 109.34(9) . . ? C31 P1 C11 110.79(9) . . ? C21 P1 Hg1 109.41(7) . . ? C31 P1 Hg1 110.26(7) . . ? C11 P1 Hg1 108.10(7) . . ? F11 B1 F14 110.92(19) . . ? F11 B1 F12 111.11(19) . . ? F14 B1 F12 108.9(2) . . ? F11 B1 F13 108.79(19) . . ? F14 B1 F13 108.16(18) . . ? F12 B1 F13 108.90(18) . . ? C12 C11 P1 110.12(13) . . ? C17 C12 C13 119.10(19) . . ? C17 C12 C11 120.12(18) . . ? C13 C12 C11 120.78(18) . . ? C14 C13 C12 120.21(19) . . ? C15 C14 C13 120.2(2) . . ? C14 C15 C16 120.1(2) . . ? C15 C16 C17 119.8(2) . . ? C16 C17 C12 120.56(19) . . ? C22 C21 P1 111.14(13) . . ? C27 C22 C23 118.91(19) . . ? C27 C22 C21 121.05(18) . . ? C23 C22 C21 120.04(18) . . ? C24 C23 C22 120.4(2) . . ? C23 C24 C25 120.1(2) . . ? C26 C25 C24 119.6(2) . . ? C27 C26 C25 120.3(2) . . ? C26 C27 C22 120.5(2) . . ? C32 C31 P1 111.85(13) . . ? C33 C32 C37 119.03(18) . . ? C33 C32 C31 120.69(17) . . ? C37 C32 C31 120.28(17) . . ? C34 C33 C32 120.39(19) . . ? C35 C34 C33 120.1(2) . . ? C34 C35 C36 120.10(19) . . ? C35 C36 C37 119.76(19) . . ? C36 C37 C32 120.64(19) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.646 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.061 #===END data_2_nitrate _database_code_depnum_ccdc_archive 'CCDC 259224' #----------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 Hg N2 O6 P2' _chemical_formula_weight 933.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 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 27.52790(10) _cell_length_b 14.5154(2) _cell_length_c 19.5340(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.2250(10) _cell_angle_gamma 90.00 _cell_volume 7743.39(16) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15298 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 26.20 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 4.108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3531 _exptl_absorpt_correction_T_max 0.6841 _exptl_absorpt_process_details 'blessing, Acta Cryst., (1995) A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Siemens SMART' _diffrn_measurement_method 'Area dectector /w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70267 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.20 _reflns_number_total 15298 _reflns_number_gt 12196 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0262P)^2^+6.4527P] 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 15298 _refine_ls_number_parameters 955 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 0.390890(6) 0.945792(11) 0.222387(9) 0.02256(5) Uani 1 1 d . . . P1 P 0.33204(4) 1.00901(8) 0.29247(6) 0.0224(2) Uani 1 1 d . . . P2 P 0.45928(4) 0.84857(7) 0.20392(6) 0.0216(2) Uani 1 1 d . . . N1 N 0.43774(17) 1.1335(3) 0.2768(3) 0.0445(12) Uani 1 1 d . . . O1 O 0.41276(17) 1.1199(3) 0.2186(2) 0.0589(11) Uani 1 1 d . . . O2 O 0.46406(14) 1.0702(3) 0.3041(2) 0.0547(11) Uani 1 1 d . . . O3 O 0.43504(16) 1.2080(3) 0.3068(3) 0.0712(15) Uani 1 1 d . . . N2 N 0.31600(17) 0.9891(3) 0.0900(2) 0.0392(11) Uani 1 1 d . . . O4 O 0.36209(13) 0.9960(3) 0.10287(19) 0.0421(9) Uani 1 1 d . . . O5 O 0.29319(14) 0.9490(3) 0.1315(2) 0.0528(11) Uani 1 1 d . . . O6 O 0.29539(17) 1.0214(3) 0.0349(2) 0.0688(14) Uani 1 1 d . . . C11 C 0.28478(16) 0.9254(3) 0.3051(3) 0.0289(11) Uani 1 1 d . . . H11A H 0.2670 0.9459 0.3434 0.035 Uiso 1 1 calc R . . H11B H 0.2610 0.9219 0.2627 0.035 Uiso 1 1 calc R . . C12 C 0.30618(15) 0.8315(3) 0.3213(2) 0.0254(10) Uani 1 1 d . . . C13 C 0.31963(16) 0.8024(3) 0.3889(3) 0.0289(11) Uani 1 1 d . . . H13A H 0.3134 0.8412 0.4260 0.035 Uiso 1 1 calc R . . C14 C 0.34195(17) 0.7181(3) 0.4029(3) 0.0321(11) Uani 1 1 d . . . H14A H 0.3514 0.6998 0.4493 0.038 Uiso 1 1 calc R . . C15 C 0.35064(16) 0.6603(3) 0.3497(3) 0.0312(11) Uani 1 1 d . . . H15A H 0.3661 0.6024 0.3593 0.037 Uiso 1 1 calc R . . C16 C 0.33658(17) 0.6875(3) 0.2822(3) 0.0319(11) Uani 1 1 d . . . H16A H 0.3421 0.6478 0.2453 0.038 Uiso 1 1 calc R . . C17 C 0.31442(16) 0.7727(3) 0.2682(2) 0.0258(10) Uani 1 1 d . . . H17A H 0.3048 0.7906 0.2217 0.031 Uiso 1 1 calc R . . C21 C 0.30367(16) 1.1169(3) 0.2580(3) 0.0267(10) Uani 1 1 d . . . H21A H 0.3195 1.1689 0.2851 0.032 Uiso 1 1 calc R . . H21B H 0.3106 1.1243 0.2098 0.032 Uiso 1 1 calc R . . C22 C 0.24900(17) 1.1236(3) 0.2590(3) 0.0279(11) Uani 1 1 d . . . C23 C 0.22857(18) 1.1374(3) 0.3197(3) 0.0365(12) Uani 1 1 d . . . H23A H 0.2492 1.1393 0.3625 0.044 Uiso 1 1 calc R . . C24 C 0.17805(19) 1.1488(3) 0.3184(3) 0.0427(14) Uani 1 1 d . . . H24A H 0.1643 1.1569 0.3602 0.051 Uiso 1 1 calc R . . C25 C 0.14832(19) 1.1481(3) 0.2563(3) 0.0451(15) Uani 1 1 d . . . H25A H 0.1140 1.1565 0.2552 0.054 Uiso 1 1 calc R . . C26 C 0.16804(19) 1.1352(3) 0.1960(3) 0.0439(14) Uani 1 1 d . . . H26A H 0.1474 1.1356 0.1532 0.053 Uiso 1 1 calc R . . C27 C 0.21805(17) 1.1216(3) 0.1974(3) 0.0332(12) Uani 1 1 d . . . H27A H 0.2312 1.1108 0.1554 0.040 Uiso 1 1 calc R . . C31 C 0.36574(17) 1.0313(3) 0.3783(2) 0.0291(11) Uani 1 1 d . . . H31C H 0.3723 0.9714 0.4019 0.035 Uiso 1 1 calc R . . H31D H 0.3978 1.0586 0.3720 0.035 Uiso 1 1 calc R . . C32 C 0.34122(16) 1.0935(3) 0.4252(2) 0.0272(10) Uani 1 1 d . . . C33 C 0.31041(18) 1.0588(3) 0.4702(3) 0.0312(11) Uani 1 1 d . . . H33A H 0.3038 0.9946 0.4703 0.037 Uiso 1 1 calc R . . C34 C 0.2892(2) 1.1154(3) 0.5148(3) 0.0409(13) Uani 1 1 d . . . H34A H 0.2678 1.0907 0.5447 0.049 Uiso 1 1 calc R . . C35 C 0.29953(19) 1.2089(3) 0.5154(3) 0.0383(13) Uani 1 1 d . . . H35A H 0.2860 1.2481 0.5470 0.046 Uiso 1 1 calc R . . C36 C 0.32931(18) 1.2456(3) 0.4706(3) 0.0349(12) Uani 1 1 d . . . H36A H 0.3355 1.3100 0.4706 0.042 Uiso 1 1 calc R . . C37 C 0.35022(17) 1.1881(3) 0.4255(2) 0.0294(11) Uani 1 1 d . . . H37A H 0.3707 1.2134 0.3946 0.035 Uiso 1 1 calc R . . C41 C 0.46645(16) 0.7623(3) 0.2730(2) 0.0240(10) Uani 1 1 d . . . H41A H 0.4344 0.7323 0.2756 0.029 Uiso 1 1 calc R . . H41B H 0.4896 0.7142 0.2612 0.029 Uiso 1 1 calc R . . C42 C 0.48498(16) 0.8019(3) 0.3426(2) 0.0232(10) Uani 1 1 d . . . C43 C 0.45269(17) 0.8371(3) 0.3847(2) 0.0292(11) Uani 1 1 d . . . H43A H 0.4186 0.8378 0.3687 0.035 Uiso 1 1 calc R . . C44 C 0.4692(2) 0.8715(4) 0.4498(3) 0.0421(13) Uani 1 1 d . . . H44A H 0.4465 0.8947 0.4783 0.051 Uiso 1 1 calc R . . C45 C 0.5186(2) 0.8719(4) 0.4728(3) 0.0488(15) Uani 1 1 d . . . H45A H 0.5301 0.8962 0.5170 0.059 Uiso 1 1 calc R . . C46 C 0.5512(2) 0.8371(4) 0.4316(3) 0.0471(15) Uani 1 1 d . . . H46A H 0.5852 0.8369 0.4476 0.057 Uiso 1 1 calc R . . C47 C 0.53461(18) 0.8025(3) 0.3670(3) 0.0358(12) Uani 1 1 d . . . H47A H 0.5574 0.7787 0.3389 0.043 Uiso 1 1 calc R . . C51 C 0.51741(15) 0.9108(3) 0.2110(2) 0.0257(10) Uani 1 1 d . . . H51A H 0.5169 0.9593 0.2466 0.031 Uiso 1 1 calc R . . H51B H 0.5440 0.8674 0.2276 0.031 Uiso 1 1 calc R . . C52 C 0.52978(16) 0.9555(3) 0.1454(2) 0.0243(10) Uani 1 1 d . . . C53 C 0.55961(16) 0.9095(3) 0.1041(3) 0.0319(11) Uani 1 1 d . . . H53A H 0.5698 0.8482 0.1155 0.038 Uiso 1 1 calc R . . C54 C 0.57459(18) 0.9515(3) 0.0470(3) 0.0357(12) Uani 1 1 d . . . H54A H 0.5952 0.9195 0.0196 0.043 Uiso 1 1 calc R . . C55 C 0.55955(19) 1.0398(3) 0.0300(3) 0.0380(13) Uani 1 1 d . . . H55A H 0.5704 1.0692 -0.0088 0.046 Uiso 1 1 calc R . . C56 C 0.52881(19) 1.0859(3) 0.0690(3) 0.0362(12) Uani 1 1 d . . . H56A H 0.5178 1.1463 0.0564 0.043 Uiso 1 1 calc R . . C57 C 0.51401(17) 1.0436(3) 0.1266(3) 0.0301(11) Uani 1 1 d . . . H57A H 0.4928 1.0753 0.1533 0.036 Uiso 1 1 calc R . . C61 C 0.45358(17) 0.7832(3) 0.1233(2) 0.0291(11) Uani 1 1 d . . . H61A H 0.4500 0.8267 0.0839 0.035 Uiso 1 1 calc R . . H61B H 0.4839 0.7471 0.1212 0.035 Uiso 1 1 calc R . . C62 C 0.41024(17) 0.7187(3) 0.1165(2) 0.0266(10) Uani 1 1 d . . . C63 C 0.36298(18) 0.7509(3) 0.0988(2) 0.0341(12) Uani 1 1 d . . . H63A H 0.3579 0.8147 0.0899 0.041 Uiso 1 1 calc R . . C64 C 0.3233(2) 0.6927(4) 0.0939(3) 0.0432(14) Uani 1 1 d . . . H64A H 0.2913 0.7165 0.0819 0.052 Uiso 1 1 calc R . . C65 C 0.3301(2) 0.5992(4) 0.1066(3) 0.0447(14) Uani 1 1 d . . . H65A H 0.3028 0.5587 0.1040 0.054 Uiso 1 1 calc R . . C66 C 0.3767(2) 0.5661(3) 0.1228(3) 0.0423(14) Uani 1 1 d . . . H66A H 0.3817 0.5020 0.1306 0.051 Uiso 1 1 calc R . . C67 C 0.41686(18) 0.6246(3) 0.1281(2) 0.0314(11) Uani 1 1 d . . . H67A H 0.4489 0.6004 0.1397 0.038 Uiso 1 1 calc R . . Hg1A Hg 0.125896(6) 0.524136(11) 0.283626(9) 0.02344(5) Uani 1 1 d . . . P1A P 0.19188(4) 0.49346(8) 0.37599(6) 0.0231(3) Uani 1 1 d . . . P2A P 0.05733(4) 0.61737(7) 0.23271(6) 0.0214(2) Uani 1 1 d . . . N1A N 0.06594(15) 0.3391(3) 0.3019(2) 0.0343(10) Uani 1 1 d . . . O1A O 0.10705(12) 0.3549(2) 0.28140(18) 0.0365(8) Uani 1 1 d . . . O2A O 0.04075(13) 0.4057(2) 0.31780(19) 0.0423(9) Uani 1 1 d . . . O3A O 0.05139(13) 0.2588(2) 0.3071(2) 0.0461(10) Uani 1 1 d . . . O6A O 0.20400(15) 0.5144(3) 0.1050(2) 0.0501(10) Uani 1 1 d . . . N2A N 0.18708(16) 0.5187(3) 0.1600(2) 0.0367(10) Uani 1 1 d . . . O4A O 0.14611(13) 0.4782(3) 0.16587(19) 0.0424(9) Uani 1 1 d . . . O5A O 0.20768(14) 0.5626(2) 0.2106(2) 0.0452(9) Uani 1 1 d . . . C11A C -0.00167(15) 0.5575(3) 0.2180(2) 0.0232(10) Uani 1 1 d . . . H11C H -0.0048 0.5172 0.2581 0.028 Uiso 1 1 calc R . . H11D H -0.0282 0.6038 0.2156 0.028 Uiso 1 1 calc R . . C12A C -0.00898(17) 0.4994(3) 0.1530(2) 0.0257(10) Uani 1 1 d . . . C13A C -0.04949(18) 0.5164(3) 0.1042(3) 0.0355(12) Uani 1 1 d . . . H13B H -0.0711 0.5658 0.1108 0.043 Uiso 1 1 calc R . . C14A C -0.0582(2) 0.4612(4) 0.0461(3) 0.0500(16) Uani 1 1 d . . . H14B H -0.0861 0.4727 0.0132 0.060 Uiso 1 1 calc R . . C15A C -0.0273(2) 0.3904(4) 0.0354(3) 0.0478(15) Uani 1 1 d . . . H15B H -0.0337 0.3526 -0.0044 0.057 Uiso 1 1 calc R . . C16A C 0.0133(2) 0.3742(3) 0.0829(3) 0.0413(13) Uani 1 1 d . . . H16B H 0.0350 0.3254 0.0753 0.050 Uiso 1 1 calc R . . C17A C 0.02294(18) 0.4282(3) 0.1414(3) 0.0313(11) Uani 1 1 d . . . H17B H 0.0512 0.4168 0.1736 0.038 Uiso 1 1 calc R . . C21A C 0.06295(18) 0.6709(3) 0.1491(2) 0.0295(11) Uani 1 1 d . . . H21C H 0.0734 0.6231 0.1179 0.035 Uiso 1 1 calc R . . H21D H 0.0302 0.6929 0.1290 0.035 Uiso 1 1 calc R . . C22A C 0.09827(16) 0.7503(3) 0.1512(2) 0.0245(10) Uani 1 1 d . . . C23A C 0.08301(18) 0.8393(3) 0.1652(2) 0.0286(11) Uani 1 1 d . . . H23B H 0.0505 0.8494 0.1749 0.034 Uiso 1 1 calc R . . C24A C 0.1151(2) 0.9132(3) 0.1650(3) 0.0356(12) Uani 1 1 d . . . H24B H 0.1044 0.9735 0.1746 0.043 Uiso 1 1 calc R . . C25A C 0.1625(2) 0.8996(4) 0.1507(3) 0.0401(13) Uani 1 1 d . . . H25B H 0.1844 0.9500 0.1505 0.048 Uiso 1 1 calc R . . C26A C 0.17740(18) 0.8120(4) 0.1370(3) 0.0378(12) Uani 1 1 d . . . H26B H 0.2100 0.8020 0.1274 0.045 Uiso 1 1 calc R . . C27A C 0.14574(17) 0.7378(3) 0.1371(2) 0.0318(11) Uani 1 1 d . . . H27B H 0.1568 0.6778 0.1272 0.038 Uiso 1 1 calc R . . C31A C 0.04869(17) 0.7108(3) 0.2927(2) 0.0235(10) Uani 1 1 d . . . H31A H 0.0781 0.7506 0.2980 0.028 Uiso 1 1 calc R . . H31B H 0.0204 0.7489 0.2734 0.028 Uiso 1 1 calc R . . C32A C 0.03994(16) 0.6753(3) 0.3623(2) 0.0236(10) Uani 1 1 d . . . C33A C 0.07712(17) 0.6753(3) 0.4168(2) 0.0270(10) Uani 1 1 d . . . H33B H 0.1088 0.6963 0.4098 0.032 Uiso 1 1 calc R . . C34A C 0.06891(18) 0.6451(3) 0.4814(3) 0.0325(11) Uani 1 1 d . . . H34B H 0.0947 0.6468 0.5186 0.039 Uiso 1 1 calc R . . C35A C 0.0234(2) 0.6125(3) 0.4919(3) 0.0389(13) Uani 1 1 d . . . H35B H 0.0178 0.5917 0.5363 0.047 Uiso 1 1 calc R . . C36A C -0.0140(2) 0.6102(4) 0.4376(3) 0.0409(13) Uani 1 1 d . . . H36B H -0.0451 0.5864 0.4445 0.049 Uiso 1 1 calc R . . C37A C -0.00614(17) 0.6425(3) 0.3736(3) 0.0310(11) Uani 1 1 d . . . H37B H -0.0323 0.6425 0.3368 0.037 Uiso 1 1 calc R . . C41A C 0.23670(16) 0.5865(3) 0.3799(3) 0.0285(10) Uani 1 1 d . . . H41C H 0.2628 0.5747 0.4187 0.034 Uiso 1 1 calc R . . H41D H 0.2521 0.5867 0.3368 0.034 Uiso 1 1 calc R . . C42A C 0.21463(15) 0.6805(3) 0.3896(2) 0.0247(10) Uani 1 1 d . . . C43A C 0.21574(17) 0.7181(3) 0.4549(3) 0.0317(11) Uani 1 1 d . . . H43B H 0.2290 0.6835 0.4941 0.038 Uiso 1 1 calc R . . C44A C 0.19747(19) 0.8065(4) 0.4635(3) 0.0388(13) Uani 1 1 d . . . H44B H 0.1982 0.8319 0.5084 0.047 Uiso 1 1 calc R . . C45A C 0.17832(18) 0.8569(3) 0.4066(3) 0.0402(13) Uani 1 1 d . . . H45B H 0.1660 0.9172 0.4123 0.048 Uiso 1 1 calc R . . C46A C 0.17707(17) 0.8200(3) 0.3413(3) 0.0368(12) Uani 1 1 d . . . H46B H 0.1637 0.8548 0.3023 0.044 Uiso 1 1 calc R . . C47A C 0.19528(16) 0.7325(3) 0.3324(3) 0.0301(11) Uani 1 1 d . . . H47B H 0.1946 0.7077 0.2873 0.036 Uiso 1 1 calc R . . C51A C 0.22627(17) 0.3870(3) 0.3693(2) 0.0290(11) Uani 1 1 d . . . H51C H 0.2479 0.3776 0.4132 0.035 Uiso 1 1 calc R . . H51D H 0.2028 0.3350 0.3639 0.035 Uiso 1 1 calc R . . C52A C 0.25726(16) 0.3837(3) 0.3106(2) 0.0241(10) Uani 1 1 d . . . C53A C 0.30586(17) 0.4107(3) 0.3204(3) 0.0308(11) Uani 1 1 d . . . H53B H 0.3197 0.4338 0.3640 0.037 Uiso 1 1 calc R . . C54A C 0.33440(18) 0.4043(4) 0.2674(3) 0.0369(12) Uani 1 1 d . . . H54B H 0.3677 0.4232 0.2745 0.044 Uiso 1 1 calc R . . C55A C 0.31458(19) 0.3703(3) 0.2037(3) 0.0357(12) Uani 1 1 d . . . H55B H 0.3341 0.3651 0.1671 0.043 Uiso 1 1 calc R . . C56A C 0.26590(18) 0.3440(3) 0.1942(3) 0.0330(11) Uani 1 1 d . . . H56B H 0.2520 0.3209 0.1506 0.040 Uiso 1 1 calc R . . C57A C 0.23725(17) 0.3506(3) 0.2470(2) 0.0287(11) Uani 1 1 d . . . H57B H 0.2038 0.3326 0.2397 0.034 Uiso 1 1 calc R . . C61A C 0.17278(18) 0.4871(3) 0.4622(2) 0.0309(11) Uani 1 1 d . . . H61C H 0.2010 0.5029 0.4967 0.037 Uiso 1 1 calc R . . H61D H 0.1468 0.5335 0.4658 0.037 Uiso 1 1 calc R . . C62A C 0.15368(17) 0.3929(3) 0.4790(2) 0.0285(11) Uani 1 1 d . . . C63A C 0.10629(18) 0.3668(4) 0.4574(3) 0.0383(12) Uani 1 1 d . . . H63B H 0.0841 0.4099 0.4340 0.046 Uiso 1 1 calc R . . C64A C 0.0905(2) 0.2786(4) 0.4692(3) 0.0510(16) Uani 1 1 d . . . H64B H 0.0577 0.2613 0.4531 0.061 Uiso 1 1 calc R . . C65A C 0.1219(2) 0.2151(4) 0.5043(3) 0.0498(15) Uani 1 1 d . . . H65B H 0.1109 0.1545 0.5126 0.060 Uiso 1 1 calc R . . C66A C 0.1690(2) 0.2411(4) 0.5269(3) 0.0477(15) Uani 1 1 d . . . H66B H 0.1909 0.1983 0.5513 0.057 Uiso 1 1 calc R . . C67A C 0.1850(2) 0.3293(4) 0.5145(3) 0.0430(14) Uani 1 1 d . . . H67B H 0.2178 0.3465 0.5304 0.052 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 Hg1 0.02256(10) 0.01967(9) 0.02579(10) -0.00007(7) 0.00442(7) 0.00005(6) P1 0.0210(6) 0.0210(6) 0.0261(7) 0.0030(5) 0.0060(5) 0.0012(4) P2 0.0251(6) 0.0175(6) 0.0226(7) 0.0017(4) 0.0051(5) -0.0006(4) N1 0.041(3) 0.039(3) 0.060(4) -0.015(2) 0.033(3) -0.020(2) O1 0.081(3) 0.043(2) 0.053(3) -0.001(2) 0.011(2) -0.013(2) O2 0.037(2) 0.058(3) 0.070(3) -0.014(2) 0.011(2) -0.008(2) O3 0.084(3) 0.040(2) 0.103(4) -0.039(2) 0.060(3) -0.030(2) N2 0.040(3) 0.034(2) 0.042(3) -0.004(2) -0.004(2) 0.006(2) O4 0.038(2) 0.050(2) 0.037(2) 0.0081(17) 0.0019(17) 0.0000(17) O5 0.047(2) 0.058(3) 0.055(3) -0.002(2) 0.012(2) -0.0099(19) O6 0.072(3) 0.076(3) 0.050(3) 0.021(2) -0.026(2) 0.009(2) C11 0.027(3) 0.028(3) 0.033(3) 0.008(2) 0.010(2) -0.0017(19) C12 0.019(2) 0.023(2) 0.035(3) 0.003(2) 0.005(2) -0.0031(17) C13 0.031(3) 0.023(2) 0.034(3) -0.001(2) 0.007(2) -0.0048(19) C14 0.037(3) 0.027(3) 0.032(3) 0.007(2) 0.002(2) -0.007(2) C15 0.028(3) 0.019(2) 0.046(3) 0.004(2) 0.001(2) -0.0048(18) C16 0.030(3) 0.027(3) 0.039(3) -0.006(2) 0.005(2) -0.0023(19) C17 0.027(3) 0.026(2) 0.025(3) 0.0016(19) 0.004(2) -0.0035(18) C21 0.027(3) 0.018(2) 0.036(3) 0.0087(19) 0.009(2) 0.0050(17) C22 0.032(3) 0.014(2) 0.039(3) 0.0039(19) 0.006(2) 0.0028(18) C23 0.039(3) 0.026(3) 0.045(3) 0.003(2) 0.008(2) 0.006(2) C24 0.040(3) 0.028(3) 0.064(4) -0.001(3) 0.021(3) 0.003(2) C25 0.027(3) 0.028(3) 0.080(5) -0.007(3) 0.005(3) 0.001(2) C26 0.033(3) 0.025(3) 0.070(4) -0.006(3) -0.007(3) -0.002(2) C27 0.034(3) 0.021(2) 0.043(3) -0.004(2) 0.001(2) -0.0002(19) C31 0.028(3) 0.026(3) 0.032(3) 0.008(2) 0.002(2) 0.0017(19) C32 0.028(3) 0.031(3) 0.023(3) 0.003(2) 0.000(2) 0.0033(19) C33 0.042(3) 0.023(2) 0.029(3) 0.005(2) 0.007(2) 0.005(2) C34 0.059(4) 0.032(3) 0.036(3) 0.008(2) 0.022(3) 0.009(2) C35 0.054(3) 0.028(3) 0.034(3) -0.002(2) 0.013(3) 0.015(2) C36 0.044(3) 0.023(3) 0.036(3) 0.004(2) 0.001(2) 0.003(2) C37 0.031(3) 0.029(3) 0.029(3) 0.002(2) 0.003(2) -0.0005(19) C41 0.026(2) 0.018(2) 0.029(3) 0.0037(18) 0.006(2) 0.0026(17) C42 0.025(2) 0.017(2) 0.028(3) 0.0064(18) 0.0047(19) 0.0019(17) C43 0.032(3) 0.027(3) 0.028(3) 0.005(2) 0.003(2) 0.0068(19) C44 0.058(4) 0.037(3) 0.031(3) 0.000(2) 0.004(3) 0.012(2) C45 0.066(4) 0.045(3) 0.031(3) -0.002(3) -0.013(3) 0.003(3) C46 0.046(4) 0.046(3) 0.044(4) 0.003(3) -0.014(3) 0.003(3) C47 0.030(3) 0.042(3) 0.035(3) 0.006(2) 0.003(2) 0.003(2) C51 0.018(2) 0.029(2) 0.030(3) 0.003(2) 0.0059(19) -0.0012(18) C52 0.023(2) 0.022(2) 0.028(3) 0.0012(18) -0.0004(19) -0.0046(17) C53 0.027(3) 0.033(3) 0.036(3) 0.009(2) 0.007(2) 0.005(2) C54 0.030(3) 0.045(3) 0.034(3) 0.008(2) 0.008(2) 0.004(2) C55 0.043(3) 0.041(3) 0.029(3) 0.013(2) -0.003(2) -0.015(2) C56 0.047(3) 0.021(2) 0.037(3) 0.006(2) -0.011(2) -0.006(2) C57 0.034(3) 0.022(2) 0.033(3) -0.003(2) -0.002(2) -0.0009(19) C61 0.041(3) 0.026(3) 0.022(3) -0.0028(19) 0.009(2) -0.002(2) C62 0.042(3) 0.021(2) 0.017(3) -0.0032(18) 0.006(2) -0.0022(19) C63 0.046(3) 0.031(3) 0.023(3) -0.004(2) -0.003(2) 0.005(2) C64 0.034(3) 0.061(4) 0.032(3) -0.016(3) -0.005(2) 0.003(3) C65 0.047(4) 0.049(4) 0.039(3) -0.021(3) 0.008(3) -0.017(3) C66 0.062(4) 0.025(3) 0.042(3) -0.009(2) 0.015(3) -0.009(2) C67 0.042(3) 0.024(3) 0.028(3) -0.002(2) 0.003(2) 0.002(2) Hg1A 0.02327(10) 0.02233(10) 0.02485(10) -0.00021(7) 0.00345(7) -0.00119(6) P1A 0.0233(6) 0.0236(6) 0.0228(7) 0.0000(5) 0.0043(5) -0.0013(4) P2A 0.0269(6) 0.0181(6) 0.0195(6) -0.0003(4) 0.0039(5) -0.0017(4) N1A 0.034(2) 0.030(2) 0.037(3) 0.0070(19) -0.0041(19) -0.0076(18) O1A 0.044(2) 0.0233(18) 0.044(2) 0.0031(15) 0.0099(17) -0.0026(15) O2A 0.041(2) 0.035(2) 0.051(3) 0.0086(17) 0.0061(18) 0.0144(16) O3A 0.048(2) 0.027(2) 0.062(3) 0.0068(17) 0.0006(19) -0.0181(16) O6A 0.064(3) 0.062(3) 0.030(2) 0.0048(18) 0.0262(19) 0.012(2) N2A 0.049(3) 0.029(2) 0.035(3) 0.010(2) 0.014(2) 0.014(2) O4A 0.035(2) 0.061(3) 0.035(2) 0.0044(18) 0.0206(17) 0.0047(17) O5A 0.060(3) 0.035(2) 0.040(2) 0.0014(17) 0.0044(19) 0.0044(18) C11A 0.022(2) 0.020(2) 0.028(3) -0.0032(18) 0.0041(19) 0.0021(17) C12A 0.033(3) 0.020(2) 0.024(3) -0.0017(18) 0.004(2) -0.0092(18) C13A 0.034(3) 0.033(3) 0.038(3) 0.002(2) -0.002(2) -0.003(2) C14A 0.060(4) 0.051(4) 0.034(3) 0.001(3) -0.011(3) -0.020(3) C15A 0.081(5) 0.036(3) 0.028(3) -0.011(2) 0.010(3) -0.023(3) C16A 0.066(4) 0.025(3) 0.036(3) -0.002(2) 0.020(3) -0.008(2) C17A 0.044(3) 0.022(3) 0.029(3) -0.002(2) 0.006(2) -0.003(2) C21A 0.042(3) 0.026(3) 0.021(3) 0.0034(19) 0.004(2) -0.001(2) C22A 0.031(3) 0.028(2) 0.014(2) 0.0023(18) 0.0017(19) 0.0006(19) C23A 0.035(3) 0.030(3) 0.022(3) 0.0020(19) 0.006(2) 0.003(2) C24A 0.056(4) 0.022(2) 0.029(3) -0.001(2) 0.009(2) -0.001(2) C25A 0.052(4) 0.036(3) 0.033(3) 0.003(2) 0.007(3) -0.015(2) C26A 0.031(3) 0.048(3) 0.035(3) 0.008(2) 0.007(2) -0.001(2) C27A 0.038(3) 0.030(3) 0.028(3) 0.006(2) 0.006(2) 0.009(2) C31A 0.036(3) 0.014(2) 0.021(3) -0.0040(17) 0.003(2) 0.0006(17) C32A 0.029(3) 0.020(2) 0.023(3) -0.0048(18) 0.007(2) 0.0020(18) C33A 0.030(3) 0.027(2) 0.024(3) -0.0051(19) 0.006(2) 0.0000(19) C34A 0.042(3) 0.032(3) 0.023(3) -0.005(2) 0.003(2) 0.005(2) C35A 0.056(4) 0.035(3) 0.028(3) 0.001(2) 0.016(3) -0.005(2) C36A 0.043(3) 0.041(3) 0.041(3) -0.008(2) 0.019(3) -0.014(2) C37A 0.031(3) 0.037(3) 0.026(3) -0.009(2) 0.006(2) -0.003(2) C41A 0.024(2) 0.032(3) 0.029(3) -0.003(2) 0.003(2) -0.0037(19) C42A 0.018(2) 0.024(2) 0.032(3) -0.0034(19) 0.0025(19) -0.0078(17) C43A 0.034(3) 0.034(3) 0.027(3) -0.002(2) 0.005(2) -0.007(2) C44A 0.044(3) 0.042(3) 0.032(3) -0.008(2) 0.011(2) -0.009(2) C45A 0.037(3) 0.025(3) 0.061(4) -0.004(3) 0.014(3) -0.003(2) C46A 0.029(3) 0.034(3) 0.046(4) 0.009(2) 0.003(2) -0.007(2) C47A 0.028(3) 0.032(3) 0.031(3) -0.003(2) 0.005(2) -0.012(2) C51A 0.032(3) 0.026(3) 0.029(3) 0.003(2) 0.005(2) 0.0047(19) C52A 0.029(3) 0.018(2) 0.026(3) 0.0057(18) 0.005(2) 0.0065(17) C53A 0.032(3) 0.030(3) 0.029(3) 0.000(2) 0.002(2) 0.004(2) C54A 0.023(3) 0.045(3) 0.043(3) 0.007(2) 0.005(2) 0.001(2) C55A 0.044(3) 0.031(3) 0.036(3) 0.005(2) 0.020(2) 0.002(2) C56A 0.049(3) 0.022(3) 0.028(3) -0.002(2) 0.007(2) -0.004(2) C57A 0.032(3) 0.023(2) 0.032(3) 0.001(2) 0.005(2) -0.0021(19) C61A 0.034(3) 0.035(3) 0.024(3) -0.001(2) 0.007(2) 0.005(2) C62A 0.030(3) 0.038(3) 0.019(3) 0.000(2) 0.008(2) 0.002(2) C63A 0.030(3) 0.054(3) 0.032(3) 0.003(2) 0.009(2) 0.000(2) C64A 0.043(3) 0.068(4) 0.045(4) -0.009(3) 0.016(3) -0.020(3) C65A 0.064(4) 0.042(3) 0.048(4) 0.001(3) 0.021(3) -0.013(3) C66A 0.059(4) 0.043(3) 0.043(4) 0.014(3) 0.013(3) -0.003(3) C67A 0.040(3) 0.050(3) 0.038(3) 0.008(3) -0.002(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 P2 2.4159(11) . ? Hg1 P1 2.4288(12) . ? Hg1 O4 2.479(4) . ? Hg1 O1 2.601(4) . ? Hg1 O2 3.010(4) . ? Hg1 O5 3.031(4) . ? P1 C11 1.818(4) . ? P1 C21 1.839(4) . ? P1 C31 1.840(5) . ? P2 C51 1.828(4) . ? P2 C61 1.829(5) . ? P2 C41 1.833(4) . ? N1 O3 1.237(5) . ? N1 O2 1.247(6) . ? N1 O1 1.267(6) . ? N2 O5 1.233(6) . ? N2 O6 1.243(6) . ? N2 O4 1.266(5) . ? C11 C12 1.502(6) . ? C12 C17 1.384(6) . ? C12 C13 1.391(6) . ? C13 C14 1.382(6) . ? C14 C15 1.380(7) . ? C15 C16 1.384(7) . ? C16 C17 1.391(6) . ? C21 C22 1.511(6) . ? C22 C27 1.386(7) . ? C22 C23 1.389(7) . ? C23 C24 1.397(7) . ? C24 C25 1.376(8) . ? C25 C26 1.370(8) . ? C26 C27 1.387(7) . ? C31 C32 1.505(6) . ? C32 C33 1.390(6) . ? C32 C37 1.396(6) . ? C33 C34 1.380(7) . ? C34 C35 1.386(7) . ? C35 C36 1.379(7) . ? C36 C37 1.390(7) . ? C41 C42 1.506(6) . ? C42 C43 1.382(6) . ? C42 C47 1.389(6) . ? C43 C44 1.389(7) . ? C44 C45 1.376(8) . ? C45 C46 1.375(8) . ? C46 C47 1.380(7) . ? C51 C52 1.512(6) . ? C52 C57 1.385(6) . ? C52 C53 1.392(6) . ? C53 C54 1.379(7) . ? C54 C55 1.375(7) . ? C55 C56 1.381(8) . ? C56 C57 1.387(7) . ? C61 C62 1.510(6) . ? C62 C63 1.385(7) . ? C62 C67 1.393(6) . ? C63 C64 1.373(7) . ? C64 C65 1.389(8) . ? C65 C66 1.369(8) . ? C66 C67 1.386(7) . ? Hg1A P2A 2.4313(11) . ? Hg1A P1A 2.4348(12) . ? Hg1A O1A 2.510(3) . ? Hg1A O4A 2.523(4) . ? Hg1A O5A 2.868(4) . ? Hg1A O2A 3.048(4) . ? P1A C41A 1.824(5) . ? P1A C51A 1.825(4) . ? P1A C61A 1.828(5) . ? P2A C31A 1.828(4) . ? P2A C21A 1.832(5) . ? P2A C11A 1.833(4) . ? N1A O3A 1.240(5) . ? N1A O2A 1.252(5) . ? N1A O1A 1.268(5) . ? O6A N2A 1.225(5) . ? N2A O5A 1.250(6) . ? N2A O4A 1.289(5) . ? C11A C12A 1.516(6) . ? C12A C17A 1.393(6) . ? C12A C13A 1.395(7) . ? C13A C14A 1.385(7) . ? C14A C15A 1.367(8) . ? C15A C16A 1.380(8) . ? C16A C17A 1.384(7) . ? C21A C22A 1.506(6) . ? C22A C27A 1.381(6) . ? C22A C23A 1.396(6) . ? C23A C24A 1.390(7) . ? C24A C25A 1.382(7) . ? C25A C26A 1.373(7) . ? C26A C27A 1.385(7) . ? C31A C32A 1.501(6) . ? C32A C33A 1.381(6) . ? C32A C37A 1.398(6) . ? C33A C34A 1.380(6) . ? C34A C35A 1.378(7) . ? C35A C36A 1.382(7) . ? C36A C37A 1.378(7) . ? C41A C42A 1.515(6) . ? C42A C43A 1.384(6) . ? C42A C47A 1.396(6) . ? C43A C44A 1.397(7) . ? C44A C45A 1.379(7) . ? C45A C46A 1.379(7) . ? C46A C47A 1.385(7) . ? C51A C52A 1.514(6) . ? C52A C57A 1.379(6) . ? C52A C53A 1.384(6) . ? C53A C54A 1.379(7) . ? C54A C55A 1.384(7) . ? C55A C56A 1.383(7) . ? C56A C57A 1.379(7) . ? C61A C62A 1.516(7) . ? C62A C63A 1.373(7) . ? C62A C67A 1.388(7) . ? C63A C64A 1.382(8) . ? C64A C65A 1.385(8) . ? C65A C66A 1.370(8) . ? C66A C67A 1.386(7) . ? 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 P2 Hg1 P1 153.18(4) . . ? P2 Hg1 O4 101.19(9) . . ? P1 Hg1 O4 105.23(9) . . ? P2 Hg1 O1 112.07(10) . . ? P1 Hg1 O1 79.76(10) . . ? O4 Hg1 O1 74.64(13) . . ? P2 Hg1 O2 87.00(8) . . ? P1 Hg1 O2 85.63(8) . . ? O4 Hg1 O2 115.86(12) . . ? O1 Hg1 O2 44.77(13) . . ? P2 Hg1 O5 124.91(8) . . ? P1 Hg1 O5 73.66(8) . . ? O4 Hg1 O5 44.66(11) . . ? O1 Hg1 O5 99.21(13) . . ? O2 Hg1 O5 141.88(12) . . ? C11 P1 C21 109.9(2) . . ? C11 P1 C31 106.3(2) . . ? C21 P1 C31 109.0(2) . . ? C11 P1 Hg1 111.30(16) . . ? C21 P1 Hg1 113.47(15) . . ? C31 P1 Hg1 106.52(16) . . ? C51 P2 C61 107.5(2) . . ? C51 P2 C41 105.7(2) . . ? C61 P2 C41 105.6(2) . . ? C51 P2 Hg1 113.03(15) . . ? C61 P2 Hg1 116.59(16) . . ? C41 P2 Hg1 107.65(15) . . ? O3 N1 O2 120.4(6) . . ? O3 N1 O1 120.2(6) . . ? O2 N1 O1 119.3(5) . . ? N1 O1 Hg1 103.1(3) . . ? N1 O2 Hg1 84.3(3) . . ? O5 N2 O6 122.2(5) . . ? O5 N2 O4 119.2(4) . . ? O6 N2 O4 118.6(5) . . ? N2 O4 Hg1 111.0(3) . . ? N2 O5 Hg1 84.5(3) . . ? C12 C11 P1 111.5(3) . . ? C17 C12 C13 118.3(4) . . ? C17 C12 C11 119.9(4) . . ? C13 C12 C11 121.8(4) . . ? C14 C13 C12 121.0(5) . . ? C15 C14 C13 120.3(5) . . ? C14 C15 C16 119.3(4) . . ? C15 C16 C17 120.2(5) . . ? C12 C17 C16 120.8(4) . . ? C22 C21 P1 115.3(3) . . ? C27 C22 C23 118.3(5) . . ? C27 C22 C21 119.5(4) . . ? C23 C22 C21 122.1(4) . . ? C22 C23 C24 120.7(5) . . ? C25 C24 C23 119.7(5) . . ? C26 C25 C24 120.2(5) . . ? C25 C26 C27 120.2(5) . . ? C22 C27 C26 120.9(5) . . ? C32 C31 P1 116.5(3) . . ? C33 C32 C37 118.4(4) . . ? C33 C32 C31 121.6(4) . . ? C37 C32 C31 120.0(4) . . ? C34 C33 C32 121.6(5) . . ? C33 C34 C35 119.0(5) . . ? C36 C35 C34 120.8(5) . . ? C35 C36 C37 119.8(5) . . ? C36 C37 C32 120.4(5) . . ? C42 C41 P2 113.4(3) . . ? C43 C42 C47 118.2(4) . . ? C43 C42 C41 120.5(4) . . ? C47 C42 C41 121.3(4) . . ? C42 C43 C44 121.1(5) . . ? C45 C44 C43 119.8(5) . . ? C46 C45 C44 119.9(5) . . ? C45 C46 C47 120.2(5) . . ? C46 C47 C42 120.9(5) . . ? C52 C51 P2 115.8(3) . . ? C57 C52 C53 118.5(4) . . ? C57 C52 C51 121.6(4) . . ? C53 C52 C51 119.8(4) . . ? C54 C53 C52 121.0(5) . . ? C55 C54 C53 119.7(5) . . ? C54 C55 C56 120.3(5) . . ? C55 C56 C57 119.8(5) . . ? C52 C57 C56 120.7(5) . . ? C62 C61 P2 112.3(3) . . ? C63 C62 C67 118.1(4) . . ? C63 C62 C61 121.3(4) . . ? C67 C62 C61 120.6(4) . . ? C64 C63 C62 121.6(5) . . ? C63 C64 C65 120.0(5) . . ? C66 C65 C64 119.0(5) . . ? C65 C66 C67 121.2(5) . . ? C66 C67 C62 120.1(5) . . ? P2A Hg1A P1A 150.85(4) . . ? P2A Hg1A O1A 112.93(8) . . ? P1A Hg1A O1A 88.12(8) . . ? P2A Hg1A O4A 91.32(9) . . ? P1A Hg1A O4A 113.43(9) . . ? O1A Hg1A O4A 78.14(12) . . ? P2A Hg1A O5A 107.80(8) . . ? P1A Hg1A O5A 81.10(8) . . ? O1A Hg1A O5A 110.82(11) . . ? O4A Hg1A O5A 47.22(11) . . ? P2A Hg1A O2A 79.91(7) . . ? P1A Hg1A O2A 104.90(7) . . ? O1A Hg1A O2A 44.66(10) . . ? O4A Hg1A O2A 108.33(11) . . ? O5A Hg1A O2A 153.16(10) . . ? C41A P1A C51A 106.0(2) . . ? C41A P1A C61A 105.6(2) . . ? C51A P1A C61A 103.6(2) . . ? C41A P1A Hg1A 109.48(16) . . ? C51A P1A Hg1A 116.56(16) . . ? C61A P1A Hg1A 114.68(16) . . ? C31A P2A C21A 106.8(2) . . ? C31A P2A C11A 105.6(2) . . ? C21A P2A C11A 103.5(2) . . ? C31A P2A Hg1A 107.90(15) . . ? C21A P2A Hg1A 116.90(16) . . ? C11A P2A Hg1A 115.29(14) . . ? O3A N1A O2A 120.7(4) . . ? O3A N1A O1A 120.4(4) . . ? O2A N1A O1A 118.9(4) . . ? N1A O1A Hg1A 111.3(3) . . ? N1A O2A Hg1A 85.2(3) . . ? O6A N2A O5A 122.3(5) . . ? O6A N2A O4A 119.3(5) . . ? O5A N2A O4A 118.5(4) . . ? N2A O4A Hg1A 104.9(3) . . ? N2A O5A Hg1A 89.3(3) . . ? C12A C11A P2A 114.7(3) . . ? C17A C12A C13A 119.1(4) . . ? C17A C12A C11A 121.9(4) . . ? C13A C12A C11A 119.0(4) . . ? C14A C13A C12A 120.0(5) . . ? C15A C14A C13A 120.8(5) . . ? C14A C15A C16A 119.5(5) . . ? C15A C16A C17A 120.9(5) . . ? C16A C17A C12A 119.6(5) . . ? C22A C21A P2A 115.3(3) . . ? C27A C22A C23A 118.4(4) . . ? C27A C22A C21A 121.2(4) . . ? C23A C22A C21A 120.3(4) . . ? C24A C23A C22A 120.5(4) . . ? C25A C24A C23A 120.4(5) . . ? C26A C25A C24A 119.0(5) . . ? C25A C26A C27A 121.1(5) . . ? C22A C27A C26A 120.6(5) . . ? C32A C31A P2A 112.0(3) . . ? C33A C32A C37A 118.5(4) . . ? C33A C32A C31A 120.7(4) . . ? C37A C32A C31A 120.8(4) . . ? C34A C33A C32A 120.9(4) . . ? C35A C34A C33A 120.1(5) . . ? C34A C35A C36A 119.8(5) . . ? C37A C36A C35A 120.1(5) . . ? C36A C37A C32A 120.5(5) . . ? C42A C41A P1A 113.1(3) . . ? C43A C42A C47A 119.1(4) . . ? C43A C42A C41A 120.4(4) . . ? C47A C42A C41A 120.4(4) . . ? C42A C43A C44A 120.4(5) . . ? C45A C44A C43A 119.9(5) . . ? C44A C45A C46A 120.1(5) . . ? C45A C46A C47A 120.3(5) . . ? C46A C47A C42A 120.2(5) . . ? C52A C51A P1A 115.3(3) . . ? C57A C52A C53A 119.5(4) . . ? C57A C52A C51A 119.6(4) . . ? C53A C52A C51A 120.9(4) . . ? C54A C53A C52A 120.6(5) . . ? C53A C54A C55A 120.1(5) . . ? C56A C55A C54A 119.0(5) . . ? C57A C56A C55A 121.0(5) . . ? C56A C57A C52A 119.8(4) . . ? C62A C61A P1A 113.1(3) . . ? C63A C62A C67A 118.5(5) . . ? C63A C62A C61A 121.6(4) . . ? C67A C62A C61A 119.8(4) . . ? C62A C63A C64A 120.8(5) . . ? C63A C64A C65A 120.6(5) . . ? C66A C65A C64A 118.9(5) . . ? C65A C66A C67A 120.5(5) . . ? C66A C67A C62A 120.7(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.20 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.915 _refine_diff_density_min -1.492 _refine_diff_density_rms 0.114 #===END data_3_chloride _database_code_depnum_ccdc_archive 'CCDC 259225' #----------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H24 Cl Hg N2 O3 P' _chemical_formula_weight 643.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2708(2) _cell_length_b 9.87260(10) _cell_length_c 20.6739(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.492(1) _cell_angle_gamma 90.00 _cell_volume 2289.87(5) _cell_formula_units_Z 4 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used 4680 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 26.41 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 6.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1679 _exptl_absorpt_correction_T_max 0.3376 _exptl_absorpt_process_details 'blessing, Acta Cryst., (1995) A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 'Siemens SMART' _diffrn_measurement_method 'Area dectector /w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13436 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.41 _reflns_number_total 4680 _reflns_number_gt 4423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0312P)^2^+2.1070P] 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 4680 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.102 _refine_ls_shift/su_mean 0.003 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 0.850998(9) 0.069005(10) 0.201245(5) 0.01070(6) Uani 1 1 d . . . Cl1 Cl 0.71837(7) 0.12924(8) 0.11201(4) 0.01684(16) Uani 1 1 d . . . P1 P 1.00599(7) -0.04061(8) 0.26713(4) 0.00938(15) Uani 1 1 d . . . O1 O 0.6713(2) 0.0059(2) 0.26897(11) 0.0174(5) Uani 1 1 d . . . O3 O 0.76300(19) 0.3051(2) 0.25472(11) 0.0162(5) Uani 1 1 d . . . O2 O 0.93546(19) 0.3259(2) 0.21675(12) 0.0174(5) Uani 1 1 d . . . N1 N 0.8426(2) 0.3786(3) 0.23456(13) 0.0126(5) Uani 1 1 d . . . C11 C 0.9659(3) -0.0795(3) 0.34870(16) 0.0129(6) Uani 1 1 d . . . H11A H 0.8837 -0.1099 0.3461 0.016 Uiso 1 1 calc R . . H11B H 1.0160 -0.1523 0.3672 0.016 Uiso 1 1 calc R . . C12 C 0.9809(3) 0.0437(3) 0.39230(15) 0.0122(6) Uani 1 1 d . . . C13 C 0.8998(3) 0.1518(3) 0.38411(15) 0.0146(6) Uani 1 1 d . . . H13 H 0.8333 0.1450 0.3539 0.018 Uiso 1 1 calc R . . C14 C 0.9187(3) 0.2694(3) 0.42117(16) 0.0176(6) Uani 1 1 d . . . H14 H 0.8657 0.3415 0.4150 0.021 Uiso 1 1 calc R . . C15 C 1.0168(3) 0.2788(3) 0.46737(16) 0.0181(6) Uani 1 1 d . . . H15 H 1.0295 0.3569 0.4922 0.022 Uiso 1 1 calc R . . C16 C 1.0962(3) 0.1699(3) 0.47611(16) 0.0182(7) Uani 1 1 d . . . H16 H 1.1611 0.1750 0.5074 0.022 Uiso 1 1 calc R . . C17 C 1.0783(3) 0.0542(3) 0.43829(16) 0.0147(6) Uani 1 1 d . . . H17 H 1.1323 -0.0170 0.4439 0.018 Uiso 1 1 calc R . . C21 C 1.0366(3) -0.2017(3) 0.22808(15) 0.0136(6) Uani 1 1 d . . . H21A H 1.1164 -0.2312 0.2436 0.016 Uiso 1 1 calc R . . H21B H 0.9811 -0.2694 0.2410 0.016 Uiso 1 1 calc R . . C22 C 1.0267(3) -0.1941(3) 0.15438(15) 0.0120(6) Uani 1 1 d . . . C23 C 1.1262(3) -0.1814(3) 0.12011(17) 0.0175(7) Uani 1 1 d . . . H23 H 1.2020 -0.1817 0.1423 0.021 Uiso 1 1 calc R . . C24 C 1.1137(3) -0.1682(3) 0.05296(17) 0.0203(7) Uani 1 1 d . . . H24 H 1.1811 -0.1588 0.0307 0.024 Uiso 1 1 calc R . . C25 C 1.0017(3) -0.1688(3) 0.01856(16) 0.0195(7) Uani 1 1 d . . . H25 H 0.9937 -0.1588 -0.0264 0.023 Uiso 1 1 calc R . . C26 C 0.9020(3) -0.1845(3) 0.05229(16) 0.0192(7) Uani 1 1 d . . . H26 H 0.8265 -0.1867 0.0297 0.023 Uiso 1 1 calc R . . C27 C 0.9139(3) -0.1970(3) 0.11958(16) 0.0168(6) Uani 1 1 d . . . H27 H 0.8464 -0.2074 0.1417 0.020 Uiso 1 1 calc R . . C31 C 1.1428(3) 0.0593(3) 0.28164(17) 0.0124(6) Uani 1 1 d . . . H31A H 1.1214 0.1501 0.2943 0.015 Uiso 1 1 calc R . . H31B H 1.1915 0.0198 0.3180 0.015 Uiso 1 1 calc R . . C32 C 1.2171(3) 0.0700(3) 0.22486(16) 0.0111(6) Uani 1 1 d . . . C33 C 1.3230(3) -0.0047(3) 0.22532(16) 0.0142(6) Uani 1 1 d . . . H33 H 1.3465 -0.0608 0.2603 0.017 Uiso 1 1 calc R . . C34 C 1.3930(3) 0.0047(3) 0.17387(16) 0.0170(7) Uani 1 1 d . . . H34 H 1.4630 -0.0454 0.1744 0.020 Uiso 1 1 calc R . . C35 C 1.3588(3) 0.0887(3) 0.12163(17) 0.0172(7) Uani 1 1 d . . . H35 H 1.4053 0.0938 0.0869 0.021 Uiso 1 1 calc R . . C36 C 1.2552(3) 0.1653(3) 0.12106(16) 0.0164(6) Uani 1 1 d . . . H36 H 1.2332 0.2226 0.0863 0.020 Uiso 1 1 calc R . . C37 C 1.1844(3) 0.1563(3) 0.17257(15) 0.0139(6) Uani 1 1 d . . . H37 H 1.1152 0.2078 0.1722 0.017 Uiso 1 1 calc R . . N41 N 1.1187(3) 0.4634(3) 0.09423(16) 0.0257(7) Uani 1 1 d . . . C41 C 0.8880(3) 0.4546(4) 0.07536(18) 0.0215(7) Uani 1 1 d . . . H41A H 0.8627 0.4853 0.0322 0.032 Uiso 1 1 calc R . . H41B H 0.8539 0.5118 0.1063 0.032 Uiso 1 1 calc R . . H41C H 0.8618 0.3631 0.0805 0.032 Uiso 1 1 calc R . . C42 C 1.0185(3) 0.4605(3) 0.08623(16) 0.0182(7) 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 0.01104(8) 0.00946(8) 0.01125(8) 0.00164(4) -0.00077(5) 0.00061(4) Cl1 0.0192(3) 0.0149(4) 0.0151(4) 0.0021(3) -0.0050(3) 0.0027(3) P1 0.0101(3) 0.0080(3) 0.0099(4) -0.0002(3) 0.0003(3) 0.0000(3) O1 0.0207(11) 0.0087(10) 0.0236(13) 0.0010(9) 0.0062(10) -0.0013(9) O3 0.0155(10) 0.0150(11) 0.0185(12) 0.0027(9) 0.0041(9) -0.0011(9) O2 0.0118(10) 0.0154(11) 0.0252(13) -0.0038(9) 0.0038(9) 0.0021(8) N1 0.0131(12) 0.0114(12) 0.0128(13) -0.0014(10) -0.0019(10) 0.0019(10) C11 0.0145(15) 0.0129(15) 0.0113(16) 0.0008(11) 0.0008(12) -0.0007(11) C12 0.0140(14) 0.0114(13) 0.0117(15) 0.0014(12) 0.0047(12) -0.0021(11) C13 0.0113(13) 0.0184(15) 0.0138(15) 0.0013(12) 0.0002(12) -0.0005(12) C14 0.0172(15) 0.0169(16) 0.0194(16) 0.0000(13) 0.0057(13) 0.0031(12) C15 0.0221(16) 0.0170(16) 0.0161(16) -0.0050(13) 0.0069(13) -0.0038(13) C16 0.0157(15) 0.0247(17) 0.0137(16) -0.0039(13) -0.0009(12) -0.0041(13) C17 0.0159(16) 0.0184(16) 0.0099(15) 0.0014(11) 0.0010(13) 0.0020(11) C21 0.0161(14) 0.0093(14) 0.0150(15) -0.0002(12) -0.0015(12) 0.0024(11) C22 0.0155(14) 0.0070(13) 0.0134(15) -0.0021(11) 0.0007(12) 0.0013(11) C23 0.0156(15) 0.0151(16) 0.0218(18) -0.0074(13) 0.0015(13) -0.0008(12) C24 0.0220(16) 0.0185(16) 0.0219(18) -0.0056(13) 0.0102(14) -0.0031(13) C25 0.0293(17) 0.0172(16) 0.0125(16) -0.0027(12) 0.0044(14) 0.0031(13) C26 0.0179(15) 0.0228(17) 0.0163(16) -0.0037(13) -0.0015(13) 0.0007(13) C27 0.0144(14) 0.0181(16) 0.0185(16) -0.0037(13) 0.0038(12) -0.0016(12) C31 0.0115(15) 0.0147(16) 0.0107(15) -0.0029(11) -0.0006(12) -0.0024(10) C32 0.0097(14) 0.0122(15) 0.0114(16) -0.0026(10) 0.0007(12) -0.0046(10) C33 0.0155(14) 0.0108(14) 0.0164(16) -0.0008(12) 0.0008(12) -0.0007(12) C34 0.0133(14) 0.0162(15) 0.0217(17) -0.0041(13) 0.0025(13) -0.0007(12) C35 0.0176(16) 0.0208(16) 0.0142(16) -0.0040(13) 0.0065(13) -0.0057(12) C36 0.0195(15) 0.0151(15) 0.0139(15) 0.0013(12) -0.0016(13) -0.0016(12) C37 0.0114(13) 0.0130(14) 0.0167(16) -0.0033(12) -0.0017(12) 0.0001(11) N41 0.0278(17) 0.0221(15) 0.0272(17) 0.0035(13) 0.0027(14) -0.0031(13) C41 0.0218(17) 0.0227(17) 0.0199(18) 0.0025(14) 0.0011(14) -0.0002(13) C42 0.0286(19) 0.0133(14) 0.0130(16) 0.0011(12) 0.0031(14) 0.0013(13) _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 Cl1 2.3375(7) . ? Hg1 P1 2.3713(8) . ? Hg1 O1 2.645(2) . ? Hg1 O2 2.717(2) . ? Hg1 O3 2.802(2) . ? Hg1 O3 3.081(2) 2_645 ? P1 C11 1.828(3) . ? P1 C31 1.831(3) . ? P1 C21 1.832(3) . ? O1 N1 1.268(4) 2_645 ? O3 N1 1.256(3) . ? O3 Hg1 3.081(2) 2_655 ? O2 N1 1.255(3) . ? N1 O1 1.268(4) 2_655 ? C11 C12 1.513(4) . ? C12 C17 1.386(5) . ? C12 C13 1.405(4) . ? C13 C14 1.396(4) . ? C14 C15 1.394(5) . ? C15 C16 1.399(5) . ? C16 C17 1.388(4) . ? C21 C22 1.519(4) . ? C22 C23 1.388(4) . ? C22 C27 1.400(4) . ? C23 C24 1.388(5) . ? C24 C25 1.388(5) . ? C25 C26 1.387(5) . ? C26 C27 1.390(5) . ? C31 C32 1.509(4) . ? C32 C37 1.398(4) . ? C32 C33 1.403(4) . ? C33 C34 1.387(5) . ? C34 C35 1.387(5) . ? C35 C36 1.391(5) . ? C36 C37 1.393(4) . ? N41 C42 1.126(5) . ? C41 C42 1.468(5) . ? 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 Hg1 P1 161.77(3) . . ? Cl1 Hg1 O1 90.77(5) . . ? P1 Hg1 O1 98.50(5) . . ? Cl1 Hg1 O2 92.64(5) . . ? P1 Hg1 O2 97.34(5) . . ? O1 Hg1 O2 115.78(7) . . ? Cl1 Hg1 O3 82.88(5) . . ? P1 Hg1 O3 114.97(5) . . ? O1 Hg1 O3 70.68(6) . . ? O2 Hg1 O3 46.38(6) . . ? Cl1 Hg1 O3 101.25(4) . 2_645 ? P1 Hg1 O3 75.49(4) . 2_645 ? O1 Hg1 O3 44.11(6) . 2_645 ? O2 Hg1 O3 154.93(6) . 2_645 ? O3 Hg1 O3 114.430(6) . 2_645 ? C11 P1 C31 103.93(15) . . ? C11 P1 C21 107.33(14) . . ? C31 P1 C21 110.43(14) . . ? C11 P1 Hg1 113.09(11) . . ? C31 P1 Hg1 114.24(11) . . ? C21 P1 Hg1 107.62(10) . . ? N1 O1 Hg1 107.46(16) 2_645 . ? N1 O3 Hg1 93.35(16) . . ? N1 O3 Hg1 86.62(16) . 2_655 ? Hg1 O3 Hg1 173.51(9) . 2_655 ? N1 O2 Hg1 97.40(17) . . ? O2 N1 O3 120.0(3) . . ? O2 N1 O1 119.7(2) . 2_655 ? O3 N1 O1 120.2(2) . 2_655 ? O2 N1 Hg1 59.23(15) . . ? O3 N1 Hg1 63.09(15) . . ? O1 N1 Hg1 163.65(18) 2_655 . ? C12 C11 P1 110.9(2) . . ? C17 C12 C13 119.3(3) . . ? C17 C12 C11 120.3(3) . . ? C13 C12 C11 120.3(3) . . ? C14 C13 C12 120.1(3) . . ? C15 C14 C13 120.0(3) . . ? C14 C15 C16 119.6(3) . . ? C17 C16 C15 120.2(3) . . ? C12 C17 C16 120.7(3) . . ? C22 C21 P1 113.6(2) . . ? C23 C22 C27 118.5(3) . . ? C23 C22 C21 122.1(3) . . ? C27 C22 C21 119.4(3) . . ? C24 C23 C22 120.6(3) . . ? C25 C24 C23 120.9(3) . . ? C26 C25 C24 118.9(3) . . ? C25 C26 C27 120.5(3) . . ? C26 C27 C22 120.6(3) . . ? C26 C27 Hg1 116.4(2) . . ? C22 C27 Hg1 87.06(18) . . ? C32 C31 P1 115.5(2) . . ? C37 C32 C33 119.1(3) . . ? C37 C32 C31 121.3(3) . . ? C33 C32 C31 119.6(3) . . ? C34 C33 C32 120.4(3) . . ? C35 C34 C33 120.1(3) . . ? C34 C35 C36 120.1(3) . . ? C35 C36 C37 120.1(3) . . ? C36 C37 C32 120.1(3) . . ? N41 C42 C41 179.1(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.693 _refine_diff_density_min -1.809 _refine_diff_density_rms 0.165 #===END data_4_bromide _database_code_depnum_ccdc_archive 'CCDC 259226' #------------------------------------------------------------------------ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H21 Br Hg N O3 P' _chemical_formula_weight 646.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.1973(3) _cell_length_b 10.6534(3) _cell_length_c 22.0565(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2161.15(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4392 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 26.40 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.988 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 9.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1301 _exptl_absorpt_correction_T_max 0.4642 _exptl_absorpt_process_details 'blessing, Acta Cryst., (1995) A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Siemens SMART' _diffrn_measurement_method 'Area dectector /w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13022 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.40 _reflns_number_total 4392 _reflns_number_gt 4134 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART (Siemens, 1995)' _computing_data_reduction 'Siemens SMART (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0445P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00048(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(9) _refine_ls_number_reflns 4392 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.073 _refine_ls_shift/su_mean 0.008 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 1.06455(3) 0.36491(2) 0.064218(10) 0.02932(9) Uani 1 1 d . . . Br1 Br 1.17676(10) 0.27882(8) 0.15562(3) 0.0510(2) Uani 1 1 d . . . P1 P 0.94607(19) 0.51795(13) 0.00364(6) 0.0252(3) Uani 1 1 d . . . N1 N 0.8625(5) 0.1459(5) 0.0102(2) 0.0239(10) Uani 1 1 d . . . O1 O 0.9920(6) 0.1504(5) 0.0287(3) 0.0496(14) Uani 1 1 d . . . O2 O 0.8117(6) 0.0404(5) -0.0036(3) 0.0495(13) Uani 1 1 d . . . O3 O 0.7887(5) 0.2412(5) 0.0059(3) 0.0436(12) Uani 1 1 d . . . C32 C 1.0940(7) 0.7199(5) 0.0585(3) 0.0308(13) Uani 1 1 d . . . C11 C 0.9059(7) 0.4776(6) -0.0753(3) 0.0333(15) Uani 1 1 d . . . H11A H 0.8490 0.3987 -0.0757 0.040 Uiso 1 1 calc R . . H11B H 0.8433 0.5443 -0.0925 0.040 Uiso 1 1 calc R . . C12 C 1.0336(7) 0.4612(7) -0.1159(3) 0.0330(15) Uani 1 1 d . . . C13 C 1.0861(9) 0.5623(8) -0.1496(3) 0.0464(19) Uani 1 1 d . . . H13 H 1.0440 0.6433 -0.1457 0.056 Uiso 1 1 calc R . . C14 C 1.2034(10) 0.5412(11) -0.1895(4) 0.066(3) Uani 1 1 d . . . H14 H 1.2404 0.6091 -0.2128 0.079 Uiso 1 1 calc R . . C15 C 1.2649(10) 0.4249(13) -0.1954(4) 0.074(3) Uani 1 1 d . . . H15 H 1.3433 0.4127 -0.2228 0.088 Uiso 1 1 calc R . . C16 C 1.2143(10) 0.3265(10) -0.1622(4) 0.067(3) Uani 1 1 d . . . H16 H 1.2582 0.2462 -0.1662 0.081 Uiso 1 1 calc R . . C17 C 1.0975(8) 0.3433(8) -0.1219(3) 0.0476(19) Uani 1 1 d . . . H17 H 1.0622 0.2744 -0.0988 0.057 Uiso 1 1 calc R . . C21 C 0.7666(7) 0.5587(7) 0.0331(3) 0.0318(14) Uani 1 1 d . . . H21A H 0.7477 0.6472 0.0217 0.038 Uiso 1 1 calc R . . H21B H 0.6948 0.5069 0.0109 0.038 Uiso 1 1 calc R . . C22 C 0.7327(7) 0.5463(6) 0.0997(3) 0.0303(14) Uani 1 1 d . . . C23 C 0.5945(8) 0.5064(8) 0.1161(4) 0.0443(18) Uani 1 1 d . . . H23 H 0.5283 0.4813 0.0854 0.053 Uiso 1 1 calc R . . C24 C 0.5507(9) 0.5024(9) 0.1762(4) 0.054(2) Uani 1 1 d . . . H24 H 0.4560 0.4739 0.1864 0.065 Uiso 1 1 calc R . . C25 C 0.6447(9) 0.5396(8) 0.2205(3) 0.0478(19) Uani 1 1 d . . . H25 H 0.6147 0.5390 0.2617 0.057 Uiso 1 1 calc R . . C26 C 0.7838(9) 0.5782(8) 0.2055(3) 0.0453(18) Uani 1 1 d . . . H26 H 0.8495 0.6028 0.2365 0.054 Uiso 1 1 calc R . . C27 C 0.8272(8) 0.5812(7) 0.1463(3) 0.0377(15) Uani 1 1 d . . . H27 H 0.9232 0.6075 0.1367 0.045 Uiso 1 1 calc R . . C31 C 1.0577(8) 0.6606(5) -0.0015(3) 0.0313(13) Uani 1 1 d . . . H31A H 1.1496 0.6396 -0.0226 0.038 Uiso 1 1 calc R . . H31B H 1.0056 0.7230 -0.0267 0.038 Uiso 1 1 calc R . . C33 C 1.2008(8) 0.6695(6) 0.0962(3) 0.0330(14) Uani 1 1 d . . . H33 H 1.2546 0.5983 0.0833 0.040 Uiso 1 1 calc R . . C34 C 1.2290(9) 0.7225(8) 0.1522(3) 0.0455(19) Uani 1 1 d . . . H34 H 1.3012 0.6865 0.1776 0.055 Uiso 1 1 calc R . . C35 C 1.1543(11) 0.8262(9) 0.1716(4) 0.057(2) Uani 1 1 d . . . H35 H 1.1720 0.8600 0.2108 0.068 Uiso 1 1 calc R . . C36 C 1.0534(10) 0.8812(7) 0.1339(4) 0.057(2) Uani 1 1 d . . . H36 H 1.0047 0.9555 0.1463 0.068 Uiso 1 1 calc R . . C37 C 1.0223(7) 0.8276(6) 0.0771(4) 0.0399(17) Uani 1 1 d . . . H37 H 0.9519 0.8654 0.0514 0.048 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 Hg1 0.03377(14) 0.02560(12) 0.02858(12) 0.00435(9) -0.00373(10) 0.00137(10) Br1 0.0677(6) 0.0519(4) 0.0333(4) 0.0072(3) -0.0150(4) 0.0121(4) P1 0.0279(8) 0.0256(7) 0.0221(6) 0.0030(5) -0.0031(7) 0.0002(7) N1 0.027(3) 0.024(2) 0.021(2) -0.002(2) -0.0005(18) -0.003(2) O1 0.034(3) 0.036(3) 0.078(4) -0.010(3) -0.013(3) 0.000(2) O2 0.052(3) 0.037(3) 0.059(3) -0.005(2) -0.010(3) -0.011(3) O3 0.036(3) 0.041(3) 0.054(3) 0.009(2) 0.000(2) 0.003(2) C32 0.036(4) 0.023(3) 0.033(3) 0.000(2) 0.007(3) -0.006(2) C11 0.038(4) 0.040(3) 0.022(3) 0.003(2) -0.004(2) -0.006(3) C12 0.036(4) 0.045(4) 0.018(3) -0.001(2) -0.004(2) -0.006(3) C13 0.058(5) 0.055(5) 0.026(3) 0.002(3) -0.003(3) -0.009(4) C14 0.053(5) 0.113(8) 0.032(4) 0.001(5) 0.000(4) -0.038(6) C15 0.048(5) 0.130(10) 0.042(5) -0.044(6) 0.011(4) -0.019(6) C16 0.052(6) 0.087(7) 0.063(6) -0.037(5) 0.006(5) -0.001(5) C17 0.051(5) 0.051(5) 0.041(4) -0.010(3) 0.000(3) -0.007(3) C21 0.027(3) 0.039(4) 0.030(3) 0.006(3) -0.003(3) 0.009(3) C22 0.031(3) 0.027(3) 0.033(3) 0.000(3) 0.001(3) 0.004(3) C23 0.029(4) 0.056(5) 0.047(4) 0.000(4) -0.003(3) -0.001(3) C24 0.034(4) 0.074(6) 0.053(5) 0.009(4) 0.010(4) -0.004(4) C25 0.056(5) 0.053(5) 0.035(4) 0.003(3) 0.016(4) 0.005(4) C26 0.052(5) 0.052(4) 0.031(4) -0.004(3) 0.004(3) -0.006(4) C27 0.041(4) 0.036(3) 0.035(4) 0.002(3) 0.001(3) -0.010(3) C31 0.036(3) 0.026(3) 0.032(3) 0.009(2) -0.004(3) -0.003(3) C33 0.039(4) 0.028(3) 0.032(3) -0.001(2) 0.001(3) -0.007(3) C34 0.056(5) 0.048(4) 0.032(4) -0.001(3) 0.000(3) -0.017(4) C35 0.073(6) 0.059(5) 0.039(4) -0.017(4) 0.016(4) -0.023(4) C36 0.058(5) 0.043(4) 0.070(5) -0.026(4) 0.036(5) -0.015(4) C37 0.031(4) 0.023(3) 0.066(5) -0.005(3) 0.013(3) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 P1 2.3729(15) . ? Hg1 Br1 2.4435(7) . ? Hg1 O1 2.506(5) . ? Hg1 O3 2.814(6) 4 ? Hg1 O2 2.824(6) 4 ? Hg1 O3 3.136(5) . ? P1 C21 1.827(7) . ? P1 C11 1.831(6) . ? P1 C31 1.838(6) . ? N1 O3 1.225(7) . ? N1 O2 1.255(7) . ? N1 O1 1.259(7) . ? N1 Hg1 3.197(5) 4_455 ? O2 Hg1 2.824(6) 4_455 ? O3 Hg1 2.814(6) 4_455 ? C32 C37 1.385(9) . ? C32 C33 1.394(9) . ? C32 C31 1.504(9) . ? C11 C12 1.486(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.393(11) . ? C12 C13 1.395(10) . ? C13 C14 1.411(12) . ? C13 H13 0.9500 . ? C14 C15 1.368(16) . ? C14 H14 0.9500 . ? C15 C16 1.360(16) . ? C15 H15 0.9500 . ? C16 C17 1.406(11) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C21 C22 1.508(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.389(10) . ? C22 C27 1.397(9) . ? C23 C24 1.385(11) . ? C23 H23 0.9500 . ? C24 C25 1.364(12) . ? C24 H24 0.9500 . ? C25 C26 1.384(11) . ? C25 H25 0.9500 . ? C26 C27 1.364(10) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C33 C34 1.384(9) . ? C33 H33 0.9500 . ? C34 C35 1.369(13) . ? C34 H34 0.9500 . ? C35 C36 1.377(14) . ? C35 H35 0.9500 . ? C36 C37 1.406(11) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? 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 P1 Hg1 Br1 156.41(4) . . ? P1 Hg1 O1 109.16(14) . . ? Br1 Hg1 O1 91.61(14) . . ? P1 Hg1 O3 107.65(11) . 4 ? Br1 Hg1 O3 89.60(11) . 4 ? O1 Hg1 O3 69.96(17) . 4 ? P1 Hg1 O2 81.81(12) . 4 ? Br1 Hg1 O2 100.65(12) . 4 ? O1 Hg1 O2 113.08(17) . 4 ? O3 Hg1 O2 45.04(14) 4 4 ? P1 Hg1 O3 71.71(10) . . ? Br1 Hg1 O3 121.51(10) . . ? O1 Hg1 O3 43.35(16) . . ? O3 Hg1 O3 101.45(2) 4 . ? O2 Hg1 O3 127.38(16) 4 . ? C21 P1 C11 102.2(3) . . ? C21 P1 C31 109.3(3) . . ? C11 P1 C31 104.4(3) . . ? C21 P1 Hg1 112.2(2) . . ? C11 P1 Hg1 117.8(2) . . ? C31 P1 Hg1 110.3(2) . . ? O3 N1 O2 121.1(5) . . ? O3 N1 O1 121.2(6) . . ? O2 N1 O1 117.7(6) . . ? O3 N1 Hg1 60.9(3) . 4_455 ? O2 N1 Hg1 61.6(3) . 4_455 ? O1 N1 Hg1 168.0(4) . 4_455 ? N1 O1 Hg1 112.8(4) . . ? N1 O2 Hg1 95.4(4) . 4_455 ? N1 O3 Hg1 96.7(4) . 4_455 ? N1 O3 Hg1 82.4(4) . . ? Hg1 O3 Hg1 170.8(2) 4_455 . ? C37 C32 C33 118.6(6) . . ? C37 C32 C31 120.2(6) . . ? C33 C32 C31 121.2(6) . . ? C12 C11 P1 116.1(4) . . ? C12 C11 H11A 108.2 . . ? P1 C11 H11A 108.3 . . ? C12 C11 H11B 108.3 . . ? P1 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? C17 C12 C13 119.9(7) . . ? C17 C12 C11 119.8(6) . . ? C13 C12 C11 120.2(7) . . ? C12 C13 C14 118.3(8) . . ? C12 C13 H13 120.8 . . ? C14 C13 H13 120.8 . . ? C15 C14 C13 121.3(9) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 120.4(9) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.2(10) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 119.8(8) . . ? C12 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C22 C21 P1 120.8(4) . . ? C22 C21 H21A 107.1 . . ? P1 C21 H21A 107.1 . . ? C22 C21 H21B 107.1 . . ? P1 C21 H21B 107.1 . . ? H21A C21 H21B 106.8 . . ? C23 C22 C27 117.4(6) . . ? C23 C22 C21 118.0(6) . . ? C27 C22 C21 124.4(6) . . ? C24 C23 C22 121.7(7) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C25 C24 C23 119.5(7) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 120.0(7) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 120.5(7) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C22 121.0(7) . . ? C26 C27 H27 119.5 . . ? C22 C27 H27 119.5 . . ? C32 C31 P1 114.7(4) . . ? C32 C31 H31A 108.6 . . ? P1 C31 H31A 108.6 . . ? C32 C31 H31B 108.6 . . ? P1 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? C34 C33 C32 120.5(7) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 120.9(8) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 119.6(7) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C37 120.1(7) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C32 C37 C36 120.2(8) . . ? C32 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.825 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.124 #===END data_5_iodide _database_code_depnum_ccdc_archive 'CCDC 259227' #----------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H21 Hg I N O3 P' _chemical_formula_weight 693.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.2803(2) _cell_length_b 10.58000(10) _cell_length_c 22.5316(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2212.28(7) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4194 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 25.71 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 8.446 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1123 _exptl_absorpt_correction_T_max 0.4855 _exptl_absorpt_process_details 'blessing, Acta Cryst., (1995) A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Siemens SMART' _diffrn_measurement_method 'Area dectector /w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12684 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.71 _reflns_number_total 4194 _reflns_number_gt 4095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0316P)^2^+0.0000P] 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 SHELXL _refine_ls_extinction_coef 0.00075(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(4) _refine_ls_number_reflns 4194 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0484 _refine_ls_wR_factor_gt 0.0481 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.002 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 1.042836(15) 0.636697(14) 0.062849(7) 0.02627(6) Uani 1 1 d . . . I1 I 1.15231(4) 0.72257(3) 0.161828(14) 0.04296(9) Uani 1 1 d . . . P1 P 0.92619(11) 0.47770(10) 0.00462(4) 0.0222(2) Uani 1 1 d . . . O1 O 0.9734(4) 0.8502(3) 0.02597(18) 0.0455(9) Uani 1 1 d . . . O2 O 0.7924(4) 0.9611(3) -0.00401(17) 0.0453(9) Uani 1 1 d . . . O3 O 0.7686(4) 0.7594(3) 0.00503(17) 0.0401(8) Uani 1 1 d . . . N1 N 0.8434(3) 0.8567(3) 0.00935(15) 0.0250(7) Uani 1 1 d . . . C11 C 0.8842(4) 0.5140(4) -0.07305(18) 0.0291(9) Uani 1 1 d . . . H11A H 0.8233 0.4451 -0.0891 0.035 Uiso 1 1 calc R . . H11B H 0.8264 0.5926 -0.0742 0.035 Uiso 1 1 calc R . . C12 C 1.0113(5) 0.5302(5) -0.11303(18) 0.0313(10) Uani 1 1 d . . . C13 C 1.0745(6) 0.6489(5) -0.1202(2) 0.0440(12) Uani 1 1 d . . . H13 H 1.0389 0.7187 -0.0981 0.053 Uiso 1 1 calc R . . C14 C 1.1889(6) 0.6662(6) -0.1591(3) 0.0570(16) Uani 1 1 d . . . H14 H 1.2308 0.7476 -0.1635 0.068 Uiso 1 1 calc R . . C15 C 1.2418(6) 0.5656(7) -0.1914(3) 0.0607(18) Uani 1 1 d . . . H15 H 1.3192 0.5780 -0.2184 0.073 Uiso 1 1 calc R . . C16 C 1.1823(6) 0.4471(7) -0.1846(2) 0.0545(16) Uani 1 1 d . . . H16 H 1.2193 0.3777 -0.2066 0.065 Uiso 1 1 calc R . . C17 C 1.0675(6) 0.4291(5) -0.1454(2) 0.0403(12) Uani 1 1 d . . . H17 H 1.0273 0.3471 -0.1406 0.048 Uiso 1 1 calc R . . C21 C 1.0386(5) 0.3354(4) 0.00114(19) 0.0293(9) Uani 1 1 d . . . H21A H 0.9875 0.2709 -0.0228 0.035 Uiso 1 1 calc R . . H21B H 1.1290 0.3565 -0.0199 0.035 Uiso 1 1 calc R . . C22 C 1.0766(4) 0.2781(4) 0.0605(2) 0.0273(8) Uani 1 1 d . . . C23 C 1.0054(5) 0.1708(4) 0.0807(2) 0.0382(12) Uani 1 1 d . . . H23 H 0.9340 0.1319 0.0567 0.046 Uiso 1 1 calc R . . C24 C 1.0387(6) 0.1204(5) 0.1362(3) 0.0528(15) Uani 1 1 d . . . H24 H 0.9918 0.0457 0.1493 0.063 Uiso 1 1 calc R . . C25 C 1.1396(6) 0.1785(6) 0.1724(3) 0.0528(15) Uani 1 1 d . . . H25 H 1.1580 0.1465 0.2110 0.063 Uiso 1 1 calc R . . C26 C 1.2131(6) 0.2830(5) 0.1519(2) 0.0436(12) Uani 1 1 d . . . H26 H 1.2844 0.3219 0.1761 0.052 Uiso 1 1 calc R . . C27 C 1.1827(5) 0.3313(4) 0.0961(2) 0.0298(9) Uani 1 1 d . . . H27 H 1.2355 0.4020 0.0818 0.036 Uiso 1 1 calc R . . C31 C 0.7490(5) 0.4371(5) 0.0346(2) 0.0343(10) Uani 1 1 d . . . H31A H 0.6768 0.4871 0.0124 0.041 Uiso 1 1 calc R . . H31B H 0.7311 0.3471 0.0250 0.041 Uiso 1 1 calc R . . C32 C 0.7171(5) 0.4542(4) 0.09972(19) 0.0266(9) Uani 1 1 d . . . C33 C 0.5795(5) 0.4925(5) 0.1158(2) 0.0386(11) Uani 1 1 d . . . H33 H 0.5111 0.5116 0.0858 0.046 Uiso 1 1 calc R . . C34 C 0.5401(6) 0.5034(6) 0.1750(3) 0.0504(13) Uani 1 1 d . . . H34 H 0.4457 0.5305 0.1851 0.060 Uiso 1 1 calc R . . C35 C 0.6380(6) 0.4749(5) 0.2189(2) 0.0467(13) Uani 1 1 d . . . H35 H 0.6103 0.4805 0.2594 0.056 Uiso 1 1 calc R . . C36 C 0.7774(6) 0.4381(5) 0.2041(2) 0.0396(11) Uani 1 1 d . . . H36 H 0.8458 0.4202 0.2343 0.048 Uiso 1 1 calc R . . C37 C 0.8157(5) 0.4277(4) 0.1445(2) 0.0316(10) Uani 1 1 d . . . H37 H 0.9106 0.4020 0.1343 0.038 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 Hg1 0.02786(8) 0.02287(8) 0.02808(9) -0.00377(6) -0.00404(7) -0.00055(6) I1 0.0541(2) 0.04384(18) 0.03099(17) -0.00591(14) -0.01373(14) -0.00538(15) P1 0.0242(5) 0.0220(5) 0.0205(5) -0.0013(4) -0.0013(4) 0.0007(4) O1 0.0307(16) 0.0307(17) 0.075(3) 0.0120(17) -0.0164(17) 0.0002(15) O2 0.043(2) 0.0363(19) 0.057(2) 0.0090(17) -0.0107(17) 0.0083(16) O3 0.0329(17) 0.0373(18) 0.050(2) -0.0088(15) -0.0013(15) -0.0015(15) N1 0.0234(16) 0.0257(17) 0.0260(17) 0.0029(15) -0.0028(13) 0.0053(16) C11 0.032(2) 0.036(2) 0.019(2) -0.0032(18) -0.0050(16) 0.0047(18) C12 0.034(2) 0.040(3) 0.019(2) 0.0032(18) -0.0061(16) 0.0041(18) C13 0.042(3) 0.044(3) 0.046(3) 0.007(2) -0.001(2) 0.003(2) C14 0.045(3) 0.066(4) 0.060(4) 0.028(3) 0.005(3) 0.001(3) C15 0.035(3) 0.104(5) 0.043(3) 0.032(3) 0.004(2) 0.018(3) C16 0.050(3) 0.088(5) 0.025(3) -0.004(3) 0.001(2) 0.033(3) C17 0.042(3) 0.052(3) 0.027(2) -0.006(2) -0.0033(19) 0.014(2) C21 0.033(2) 0.024(2) 0.031(2) -0.0067(16) -0.0030(19) 0.0026(18) C22 0.0286(19) 0.0207(18) 0.033(2) -0.0020(18) 0.0045(17) 0.0071(15) C23 0.032(2) 0.024(2) 0.059(3) 0.004(2) 0.009(2) 0.0036(16) C24 0.052(3) 0.035(3) 0.071(4) 0.026(3) 0.026(3) 0.011(3) C25 0.054(3) 0.059(3) 0.045(3) 0.021(3) 0.016(3) 0.024(3) C26 0.048(3) 0.046(3) 0.037(3) 0.002(2) -0.002(2) 0.015(2) C27 0.033(2) 0.023(2) 0.033(2) -0.0004(17) 0.0032(18) 0.0038(16) C31 0.026(2) 0.042(3) 0.035(2) -0.005(2) -0.0019(18) -0.0089(19) C32 0.028(2) 0.0226(19) 0.029(2) -0.0003(17) 0.0030(17) -0.0056(17) C33 0.025(2) 0.051(3) 0.040(3) 0.000(2) -0.0020(18) 0.001(2) C34 0.035(3) 0.064(3) 0.052(3) -0.005(3) 0.013(2) 0.005(3) C35 0.051(3) 0.056(3) 0.033(3) 0.000(2) 0.012(2) -0.001(3) C36 0.048(3) 0.042(3) 0.028(2) 0.007(2) 0.002(2) 0.004(2) C37 0.031(2) 0.033(2) 0.031(2) 0.0017(19) 0.0020(17) 0.0069(18) _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 P1 2.3923(10) . ? Hg1 O1 2.491(3) . ? Hg1 I1 2.6137(3) . ? Hg1 O3 2.817(4) 4_565 ? Hg1 O2 2.862(4) 4_565 ? Hg1 O3 3.140(4) . ? P1 C31 1.829(5) . ? P1 C21 1.833(4) . ? P1 C11 1.833(4) . ? O1 N1 1.266(5) . ? O2 N1 1.238(5) . ? O2 Hg1 2.862(4) 4_465 ? O3 N1 1.245(5) . ? O3 Hg1 2.817(4) 4_465 ? C11 C12 1.494(6) . ? C12 C13 1.395(7) . ? C12 C17 1.395(7) . ? C13 C14 1.389(8) . ? C14 C15 1.380(10) . ? C15 C16 1.379(10) . ? C16 C17 1.398(8) . ? C21 C22 1.511(6) . ? C22 C27 1.388(6) . ? C22 C23 1.390(6) . ? C23 C24 1.392(8) . ? C24 C25 1.386(9) . ? C25 C26 1.378(8) . ? C26 C27 1.388(7) . ? C31 C32 1.507(6) . ? C32 C33 1.388(6) . ? C32 C37 1.391(6) . ? C33 C34 1.387(7) . ? C34 C35 1.377(8) . ? C35 C36 1.392(7) . ? C36 C37 1.393(7) . ? 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 P1 Hg1 O1 109.73(8) . . ? P1 Hg1 I1 152.66(3) . . ? O1 Hg1 I1 94.01(9) . . ? P1 Hg1 O3 108.25(7) . 4_565 ? O1 Hg1 O3 69.98(11) . 4_565 ? I1 Hg1 O3 92.21(7) . 4_565 ? P1 Hg1 O2 81.84(8) . 4_565 ? O1 Hg1 O2 112.47(11) . 4_565 ? I1 Hg1 O2 101.90(8) . 4_565 ? O3 Hg1 O2 44.57(9) 4_565 4_565 ? P1 Hg1 O3 72.33(7) . . ? O1 Hg1 O3 43.71(10) . . ? I1 Hg1 O3 121.69(6) . . ? O3 Hg1 O3 102.488(12) 4_565 . ? O2 Hg1 O3 127.81(11) 4_565 . ? C31 P1 C21 109.5(2) . . ? C31 P1 C11 102.2(2) . . ? C21 P1 C11 104.60(19) . . ? C31 P1 Hg1 111.66(15) . . ? C21 P1 Hg1 110.09(14) . . ? C11 P1 Hg1 118.20(15) . . ? N1 O1 Hg1 113.2(2) . . ? N1 O2 Hg1 95.7(2) . 4_465 ? N1 O3 Hg1 97.7(2) . 4_465 ? N1 O3 Hg1 81.8(2) . . ? Hg1 O3 Hg1 171.62(14) 4_465 . ? O2 N1 O3 120.3(3) . . ? O2 N1 O1 119.0(4) . . ? O3 N1 O1 120.6(3) . . ? C12 C11 P1 115.6(3) . . ? C13 C12 C17 118.2(5) . . ? C13 C12 C11 120.3(4) . . ? C17 C12 C11 121.4(4) . . ? C14 C13 C12 120.8(5) . . ? C15 C14 C13 120.2(6) . . ? C16 C15 C14 120.0(5) . . ? C15 C16 C17 120.0(5) . . ? C12 C17 C16 120.7(5) . . ? C22 C21 P1 115.1(3) . . ? C27 C22 C23 118.7(4) . . ? C27 C22 C21 120.9(4) . . ? C23 C22 C21 120.4(4) . . ? C22 C23 C24 120.1(5) . . ? C25 C24 C23 120.5(5) . . ? C26 C25 C24 119.6(5) . . ? C25 C26 C27 119.8(5) . . ? C26 C27 C22 121.2(5) . . ? C32 C31 P1 120.5(3) . . ? C33 C32 C37 118.3(4) . . ? C33 C32 C31 118.0(4) . . ? C37 C32 C31 123.5(4) . . ? C34 C33 C32 121.2(5) . . ? C35 C34 C33 119.9(5) . . ? C34 C35 C36 120.1(5) . . ? C35 C36 C37 119.4(5) . . ? C32 C37 C36 121.0(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.342 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.092 #===END data_6_thiocyanate _database_code_depnum_ccdc_archive 'CCDC 259228' #-------------------------------------------------------------------- _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H21 Hg N2 O3 P S' _chemical_formula_weight 625.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4193(2) _cell_length_b 10.4422(2) _cell_length_c 11.55770(10) _cell_angle_alpha 109.463(1) _cell_angle_beta 105.806(1) _cell_angle_gamma 99.8370(10) _cell_volume 1092.34(3) _cell_formula_units_Z 2 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used 4777 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.11 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 7.240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2363 _exptl_absorpt_correction_T_max 0.3904 _exptl_absorpt_process_details 'blessing, Acta Cryst., (1995) A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 'Siemens SMART' _diffrn_measurement_method 'Area dectector /w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11269 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.11 _reflns_number_total 4777 _reflns_number_gt 4586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SMART (Siemens, 1995)' _computing_data_reduction 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0334P)^2^+1.1432P] 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 4777 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0604 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.003 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 0.263220(11) 0.544818(12) 0.584734(10) 0.01365(5) Uani 1 1 d . . . S1 S 0.23476(8) 0.31493(9) 0.41615(8) 0.01446(15) Uani 1 1 d . . . P1 P 0.27516(8) 0.67610(9) 0.80333(8) 0.01090(15) Uani 1 1 d . . . N1 N 0.0433(3) 0.6530(3) 0.4358(3) 0.0162(6) Uani 1 1 d . . . N2 N 0.4913(3) 0.6652(3) 0.5859(3) 0.0223(6) Uani 1 1 d . . . O1 O 0.1534(3) 0.6276(3) 0.4168(2) 0.0212(5) Uani 1 1 d . . . O2 O -0.0469(3) 0.6689(3) 0.3505(3) 0.0240(5) Uani 1 1 d . . . O3 O 0.0265(3) 0.6571(3) 0.5403(2) 0.0266(6) Uani 1 1 d . . . C1 C 0.3975(3) 0.3311(3) 0.4154(3) 0.0146(6) Uani 1 1 d . . . C11 C 0.3817(3) 0.8589(3) 0.8673(3) 0.0146(6) Uani 1 1 d . . . H11A H 0.3659 0.9126 0.9459 0.017 Uiso 1 1 calc R . . H11B H 0.4788 0.8602 0.8933 0.017 Uiso 1 1 calc R . . C12 C 0.3579(4) 0.9353(4) 0.7756(3) 0.0173(7) Uani 1 1 d . . . C13 C 0.2314(4) 0.9625(4) 0.7283(3) 0.0228(7) Uani 1 1 d . . . H13 H 0.1565 0.9302 0.7505 0.027 Uiso 1 1 calc R . . C14 C 0.2165(5) 1.0376(4) 0.6480(4) 0.0345(10) Uani 1 1 d . . . H14 H 0.1320 1.0553 0.6172 0.041 Uiso 1 1 calc R . . C15 C 0.3272(6) 1.0858(4) 0.6143(4) 0.0378(11) Uani 1 1 d . . . H15 H 0.3170 1.1357 0.5607 0.045 Uiso 1 1 calc R . . C16 C 0.4533(5) 1.0600(4) 0.6602(4) 0.0326(9) Uani 1 1 d . . . H16 H 0.5274 1.0918 0.6369 0.039 Uiso 1 1 calc R . . C17 C 0.4687(4) 0.9862(4) 0.7413(3) 0.0234(8) Uani 1 1 d . . . H17 H 0.5541 0.9705 0.7732 0.028 Uiso 1 1 calc R . . C21 C 0.1070(3) 0.6760(4) 0.8247(3) 0.0144(6) Uani 1 1 d . . . H21A H 0.0562 0.7155 0.7684 0.017 Uiso 1 1 calc R . . H21B H 0.0527 0.5789 0.7973 0.017 Uiso 1 1 calc R . . C22 C 0.1220(3) 0.7605(4) 0.9655(3) 0.0146(6) Uani 1 1 d . . . C23 C 0.1295(4) 0.9034(4) 1.0087(3) 0.0185(7) Uani 1 1 d . . . H23 H 0.1258 0.9485 0.9513 0.022 Uiso 1 1 calc R . . C24 C 0.1427(4) 0.9800(4) 1.1386(4) 0.0236(8) Uani 1 1 d . . . H24 H 0.1489 1.0761 1.1673 0.028 Uiso 1 1 calc R . . C25 C 0.1466(4) 0.9136(5) 1.2243(4) 0.0266(8) Uani 1 1 d . . . H25 H 0.1541 0.9645 1.3102 0.032 Uiso 1 1 calc R . . C26 C 0.1393(4) 0.7705(5) 1.1818(4) 0.0243(8) Uani 1 1 d . . . H26 H 0.1425 0.7256 1.2393 0.029 Uiso 1 1 calc R . . C27 C 0.1274(3) 0.6943(4) 1.0529(3) 0.0181(7) Uani 1 1 d . . . H27 H 0.1229 0.5986 1.0250 0.022 Uiso 1 1 calc R . . C31 C 0.3648(3) 0.6026(4) 0.9146(3) 0.0147(6) Uani 1 1 d . . . H31A H 0.3819 0.6642 1.0045 0.018 Uiso 1 1 calc R . . H31B H 0.3059 0.5103 0.8960 0.018 Uiso 1 1 calc R . . C32 C 0.5012(3) 0.5881(4) 0.8989(3) 0.0133(6) Uani 1 1 d . . . C33 C 0.6261(4) 0.6936(4) 0.9819(3) 0.0186(7) Uani 1 1 d . . . H33 H 0.6269 0.7708 1.0520 0.022 Uiso 1 1 calc R . . C34 C 0.7494(4) 0.6831(4) 0.9594(4) 0.0233(8) Uani 1 1 d . . . H34 H 0.8326 0.7531 1.0150 0.028 Uiso 1 1 calc R . . C35 C 0.7489(4) 0.5690(4) 0.8547(4) 0.0220(7) Uani 1 1 d . . . H35 H 0.8310 0.5641 0.8385 0.026 Uiso 1 1 calc R . . C36 C 0.6256(4) 0.4616(4) 0.7737(3) 0.0218(7) Uani 1 1 d . . . H36 H 0.6256 0.3835 0.7049 0.026 Uiso 1 1 calc R . . C37 C 0.5025(4) 0.4714(4) 0.7960(3) 0.0166(6) Uani 1 1 d . . . H37 H 0.4202 0.3995 0.7418 0.020 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 Hg1 0.01175(7) 0.01675(8) 0.01150(7) 0.00295(5) 0.00530(5) 0.00540(5) S1 0.0112(3) 0.0153(4) 0.0147(4) 0.0030(3) 0.0049(3) 0.0041(3) P1 0.0088(3) 0.0129(4) 0.0108(4) 0.0039(3) 0.0038(3) 0.0041(3) N1 0.0158(13) 0.0157(14) 0.0150(13) 0.0047(11) 0.0045(11) 0.0041(11) N2 0.0188(15) 0.0169(14) 0.0299(16) 0.0048(12) 0.0137(13) 0.0029(12) O1 0.0217(13) 0.0316(14) 0.0224(12) 0.0159(11) 0.0141(11) 0.0168(11) O2 0.0222(13) 0.0327(15) 0.0222(13) 0.0160(11) 0.0063(11) 0.0124(11) O3 0.0154(12) 0.0465(18) 0.0186(13) 0.0136(12) 0.0066(10) 0.0086(12) C1 0.0171(16) 0.0124(15) 0.0152(15) 0.0047(12) 0.0071(13) 0.0055(12) C11 0.0119(14) 0.0138(15) 0.0139(14) 0.0032(12) 0.0027(12) 0.0014(12) C12 0.0231(17) 0.0124(15) 0.0137(15) 0.0040(12) 0.0049(13) 0.0037(13) C13 0.0218(18) 0.0204(17) 0.0191(17) 0.0061(14) 0.0003(14) 0.0039(14) C14 0.041(2) 0.024(2) 0.027(2) 0.0104(16) -0.0050(18) 0.0077(18) C15 0.062(3) 0.0195(19) 0.0207(19) 0.0112(16) 0.001(2) 0.000(2) C16 0.046(3) 0.0206(19) 0.0253(19) 0.0082(15) 0.0122(18) -0.0036(18) C17 0.0291(19) 0.0190(17) 0.0185(17) 0.0050(14) 0.0090(15) 0.0023(15) C21 0.0095(14) 0.0180(16) 0.0130(14) 0.0033(12) 0.0039(12) 0.0039(12) C22 0.0067(13) 0.0211(16) 0.0146(15) 0.0051(13) 0.0034(12) 0.0050(12) C23 0.0189(16) 0.0212(17) 0.0154(16) 0.0057(13) 0.0059(13) 0.0091(14) C24 0.0208(17) 0.0218(18) 0.0201(17) -0.0018(14) 0.0059(14) 0.0096(15) C25 0.0199(18) 0.043(2) 0.0147(16) 0.0052(16) 0.0079(14) 0.0144(17) C26 0.0191(17) 0.043(2) 0.0199(18) 0.0171(17) 0.0104(15) 0.0147(16) C27 0.0148(15) 0.0238(18) 0.0206(16) 0.0102(14) 0.0097(13) 0.0089(13) C31 0.0131(14) 0.0192(16) 0.0157(15) 0.0098(13) 0.0059(12) 0.0070(12) C32 0.0127(15) 0.0170(16) 0.0146(14) 0.0097(12) 0.0050(12) 0.0079(12) C33 0.0174(16) 0.0164(16) 0.0188(16) 0.0051(13) 0.0033(13) 0.0061(14) C34 0.0120(16) 0.0247(19) 0.033(2) 0.0161(16) 0.0030(14) 0.0029(14) C35 0.0140(16) 0.032(2) 0.0316(19) 0.0202(16) 0.0121(15) 0.0134(15) C36 0.0260(19) 0.0265(19) 0.0179(16) 0.0103(14) 0.0091(14) 0.0151(15) C37 0.0156(16) 0.0162(16) 0.0156(15) 0.0050(13) 0.0024(13) 0.0066(13) _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 P1 2.3958(8) . ? Hg1 S1 2.4438(8) . ? Hg1 O1 2.464(3) . ? Hg1 N2 2.486(3) . ? Hg1 O3 2.902(3) . ? Hg1 O3 3.011(3) 2_566 ? S1 C1 1.677(3) . ? P1 C11 1.820(3) . ? P1 C31 1.834(3) . ? P1 C21 1.835(3) . ? N1 O2 1.242(4) . ? N1 O3 1.255(4) . ? N1 O1 1.279(4) . ? N2 C1 1.157(5) 2_666 ? O3 Hg1 3.011(3) 2_566 ? C1 N2 1.157(5) 2_666 ? C11 C12 1.520(5) . ? C12 C17 1.397(5) . ? C12 C13 1.398(5) . ? C13 C14 1.396(6) . ? C14 C15 1.383(7) . ? C15 C16 1.384(7) . ? C16 C17 1.393(6) . ? C21 C22 1.519(4) . ? C22 C23 1.387(5) . ? C22 C27 1.397(5) . ? C23 C24 1.401(5) . ? C24 C25 1.382(6) . ? C25 C26 1.390(6) . ? C26 C27 1.393(5) . ? C31 C32 1.507(4) . ? C32 C37 1.396(5) . ? C32 C33 1.397(5) . ? C33 C34 1.394(5) . ? C34 C35 1.384(6) . ? C35 C36 1.392(5) . ? C36 C37 1.388(5) . ? 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 P1 Hg1 S1 147.70(3) . . ? P1 Hg1 O1 116.13(6) . . ? S1 Hg1 O1 91.28(6) . . ? P1 Hg1 N2 101.92(7) . . ? S1 Hg1 N2 95.87(7) . . ? O1 Hg1 N2 87.14(10) . . ? P1 Hg1 O3 77.39(5) . . ? S1 Hg1 O3 115.34(6) . . ? O1 Hg1 O3 47.09(7) . . ? N2 Hg1 O3 121.69(9) . . ? P1 Hg1 O3 102.84(5) . 2_566 ? S1 Hg1 O3 64.36(6) . 2_566 ? O1 Hg1 O3 78.52(8) . 2_566 ? N2 Hg1 O3 154.93(9) . 2_566 ? O3 Hg1 O3 60.95(10) . 2_566 ? C1 S1 Hg1 101.45(12) . . ? C11 P1 C31 104.62(15) . . ? C11 P1 C21 108.71(15) . . ? C31 P1 C21 106.10(15) . . ? C11 P1 Hg1 111.38(11) . . ? C31 P1 Hg1 109.71(11) . . ? C21 P1 Hg1 115.63(11) . . ? O2 N1 O3 120.8(3) . . ? O2 N1 O1 120.4(3) . . ? O3 N1 O1 118.8(3) . . ? O2 N1 Hg1 164.8(2) . . ? O3 N1 Hg1 69.81(18) . . ? O1 N1 Hg1 49.89(16) . . ? C1 N2 Hg1 152.4(3) 2_666 . ? N1 O1 Hg1 106.72(19) . . ? N1 O3 Hg1 86.25(19) . . ? N1 O3 Hg1 96.78(19) . 2_566 ? Hg1 O3 Hg1 119.05(10) . 2_566 ? N2 C1 S1 176.3(3) 2_666 . ? C12 C11 P1 116.7(2) . . ? C17 C12 C13 118.4(3) . . ? C17 C12 C11 118.7(3) . . ? C13 C12 C11 122.8(3) . . ? C14 C13 C12 120.5(4) . . ? C15 C14 C13 120.1(4) . . ? C14 C15 C16 120.2(4) . . ? C15 C16 C17 119.8(4) . . ? C16 C17 C12 121.0(4) . . ? C22 C21 P1 112.9(2) . . ? C23 C22 C27 119.2(3) . . ? C23 C22 C21 120.8(3) . . ? C27 C22 C21 120.0(3) . . ? C22 C23 C24 120.3(3) . . ? C25 C24 C23 120.3(4) . . ? C24 C25 C26 119.7(3) . . ? C25 C26 C27 120.1(3) . . ? C26 C27 C22 120.4(3) . . ? C32 C31 P1 111.0(2) . . ? C37 C32 C33 119.3(3) . . ? C37 C32 C31 119.7(3) . . ? C33 C32 C31 121.0(3) . . ? C34 C33 C32 119.9(3) . . ? C35 C34 C33 120.4(3) . . ? C34 C35 C36 120.0(3) . . ? C37 C36 C35 119.8(3) . . ? C36 C37 C32 120.6(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.551 _refine_diff_density_min -2.030 _refine_diff_density_rms 0.146 #===END