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 'Christopher Ziegler' _publ_contact_author_address ; Department of Chemistry University of Akron KNCL 404 Akron OH 44325-3601 UNITED STATES OF AMERICA ; _publ_contact_author_email ZIEGLER@UAKRON.EDU _publ_section_title ; Coordinative flexibility in hydrotris(imazolyl)borate divalent metal compounds ; loop_ _publ_author_name 'Christopher Ziegler' 'Anil Cetin' # Attachment '285451.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 285450' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Barium bishydroxytris(methimazolyl)borate biswater' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18 B Ba0.50 N6 O S3' _chemical_formula_weight 437.98 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' 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' Ba Ba -0.3244 2.2819 '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' _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 7.5055(6) _cell_length_b 10.5872(8) _cell_length_c 12.5053(9) _cell_angle_alpha 81.1580(10) _cell_angle_beta 80.5120(10) _cell_angle_gamma 69.6220(10) _cell_volume 913.77(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6076 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 28.25 _exptl_crystal_description plate _exptl_crystal_colour clear _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 442 _exptl_absorpt_coefficient_mu 1.472 _exptl_absorpt_correction_type 'Empirical SADABS' _exptl_absorpt_correction_T_min 0.8074 _exptl_absorpt_correction_T_max 0.9711 _exptl_absorpt_process_details ? _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.831458 ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8131 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4225 _reflns_number_gt 3948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.6171P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4225 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.000 _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 Ba1 Ba 0.5000 0.0000 1.0000 0.01228(7) Uani 1 2 d S . . S2 S 0.72207(9) 0.21574(6) 0.98939(5) 0.01545(13) Uani 1 1 d . . . S1 S 0.16130(9) 0.38421(6) 0.72311(5) 0.01701(14) Uani 1 1 d . . . S3 S 0.64847(9) -0.12507(6) 0.77351(5) 0.01556(13) Uani 1 1 d . . . O1 O 0.1702(3) 0.1836(2) 0.9484(2) 0.0268(5) Uani 1 1 d . . . N1 N 0.5193(3) 0.2238(2) 0.64461(17) 0.0134(4) Uani 1 1 d . . . N2 N 0.3040(3) 0.2676(2) 0.53375(18) 0.0184(5) Uani 1 1 d . . . N3 N 0.6354(3) 0.3235(2) 0.78173(17) 0.0126(4) Uani 1 1 d . . . N4 N 0.6967(3) 0.4598(2) 0.87298(18) 0.0152(4) Uani 1 1 d . . . N5 N 0.8000(3) 0.0810(2) 0.74466(17) 0.0121(4) Uani 1 1 d . . . N6 N 1.0147(3) -0.1207(2) 0.74726(18) 0.0175(5) Uani 1 1 d . . . C5 C 0.6846(3) 0.3344(2) 0.8785(2) 0.0132(5) Uani 1 1 d . . . C7 C 0.6548(4) 0.5285(3) 0.7724(2) 0.0173(5) Uani 1 1 d . . . H7 H 0.6538 0.6182 0.7474 0.021 Uiso 1 1 calc R . . C6 C 0.6159(4) 0.4447(3) 0.7165(2) 0.0169(5) Uani 1 1 d . . . H6 H 0.5809 0.4650 0.6446 0.020 Uiso 1 1 calc R . . C1 C 0.3314(4) 0.2892(2) 0.6334(2) 0.0143(5) Uani 1 1 d . . . C3 C 0.4754(4) 0.1883(3) 0.4825(2) 0.0234(6) Uani 1 1 d . . . H3 H 0.4958 0.1585 0.4122 0.028 Uiso 1 1 calc R . . C2 C 0.6072(4) 0.1614(3) 0.5508(2) 0.0197(6) Uani 1 1 d . . . H2 H 0.7385 0.1086 0.5372 0.024 Uiso 1 1 calc R . . C9 C 0.8244(4) -0.0533(2) 0.7546(2) 0.0135(5) Uani 1 1 d . . . C11 C 1.1115(4) -0.0281(3) 0.7326(2) 0.0206(6) Uani 1 1 d . . . H11 H 1.2463 -0.0484 0.7251 0.025 Uiso 1 1 calc R . . C10 C 0.9789(4) 0.0954(3) 0.7311(2) 0.0177(5) Uani 1 1 d . . . H10 H 1.0036 0.1788 0.7223 0.021 Uiso 1 1 calc R . . C8 C 0.7580(4) 0.5105(3) 0.9577(2) 0.0204(6) Uani 1 1 d . . . H8A H 0.6881 0.4921 1.0284 0.031 Uiso 1 1 calc R . . H8B H 0.7315 0.6084 0.9413 0.031 Uiso 1 1 calc R . . H8C H 0.8957 0.4651 0.9604 0.031 Uiso 1 1 calc R . . C4 C 0.1216(4) 0.3153(3) 0.4889(2) 0.0259(6) Uani 1 1 d . . . H4A H 0.0164 0.3386 0.5481 0.039 Uiso 1 1 calc R . . H4B H 0.1110 0.2438 0.4516 0.039 Uiso 1 1 calc R . . H4C H 0.1150 0.3957 0.4369 0.039 Uiso 1 1 calc R . . C12 C 1.1042(4) -0.2681(3) 0.7566(2) 0.0242(6) Uani 1 1 d . . . H12A H 1.0108 -0.3105 0.7944 0.036 Uiso 1 1 calc R . . H12B H 1.2140 -0.2943 0.7979 0.036 Uiso 1 1 calc R . . H12C H 1.1476 -0.2983 0.6836 0.036 Uiso 1 1 calc R . . B1 B 0.6037(4) 0.1962(3) 0.7536(2) 0.0128(5) Uani 1 1 d . . . H1 H 0.500(4) 0.166(3) 0.821(2) 0.002(6) Uiso 1 1 d . . . H5 H 0.170(5) 0.222(4) 0.901(3) 0.019(10) Uiso 1 1 d . . . H9 H 0.061(7) 0.183(4) 0.965(3) 0.051(13) Uiso 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 Ba1 0.01286(11) 0.01108(11) 0.01270(11) -0.00048(7) -0.00157(8) -0.00401(8) S2 0.0159(3) 0.0162(3) 0.0159(3) -0.0002(2) -0.0030(2) -0.0075(2) S1 0.0135(3) 0.0141(3) 0.0206(3) -0.0020(2) -0.0022(2) -0.0009(2) S3 0.0179(3) 0.0125(3) 0.0183(3) -0.0037(2) -0.0015(2) -0.0069(2) O1 0.0148(11) 0.0368(13) 0.0234(12) 0.0102(10) -0.0038(9) -0.0066(9) N1 0.0136(10) 0.0125(10) 0.0139(10) -0.0019(8) -0.0018(8) -0.0038(8) N2 0.0161(11) 0.0210(12) 0.0164(11) -0.0020(9) -0.0055(9) -0.0024(9) N3 0.0110(10) 0.0097(10) 0.0162(10) -0.0011(8) -0.0009(8) -0.0028(8) N4 0.0113(10) 0.0125(10) 0.0222(11) -0.0050(9) -0.0006(9) -0.0037(8) N5 0.0095(10) 0.0115(10) 0.0160(10) -0.0039(8) -0.0009(8) -0.0034(8) N6 0.0154(11) 0.0138(11) 0.0226(12) -0.0069(9) -0.0045(9) -0.0006(9) C5 0.0081(11) 0.0121(11) 0.0193(12) -0.0041(9) 0.0016(9) -0.0035(9) C7 0.0135(12) 0.0116(12) 0.0248(14) 0.0002(10) -0.0014(10) -0.0026(10) C6 0.0143(12) 0.0126(12) 0.0220(13) 0.0024(10) -0.0023(10) -0.0039(10) C1 0.0164(13) 0.0105(11) 0.0164(12) 0.0021(9) -0.0046(10) -0.0052(10) C3 0.0282(16) 0.0250(15) 0.0133(13) -0.0056(11) -0.0015(11) -0.0032(12) C2 0.0188(13) 0.0205(13) 0.0161(13) -0.0050(10) 0.0011(10) -0.0019(11) C9 0.0143(12) 0.0111(11) 0.0134(12) -0.0032(9) -0.0020(9) -0.0010(9) C11 0.0126(13) 0.0237(14) 0.0265(15) -0.0084(11) -0.0019(11) -0.0052(11) C10 0.0142(13) 0.0177(13) 0.0236(14) -0.0035(10) -0.0018(10) -0.0079(10) C8 0.0173(13) 0.0187(13) 0.0285(15) -0.0098(11) -0.0020(11) -0.0074(11) C4 0.0221(15) 0.0289(16) 0.0258(15) -0.0021(12) -0.0126(12) -0.0034(12) C12 0.0231(15) 0.0135(13) 0.0314(16) -0.0066(11) -0.0089(12) 0.0040(11) B1 0.0121(13) 0.0104(13) 0.0155(13) -0.0009(10) -0.0026(11) -0.0031(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba1 O1 2.667(2) 2_657 ? Ba1 O1 2.667(2) . ? Ba1 S3 3.1784(7) 2_657 ? Ba1 S3 3.1784(7) . ? Ba1 S2 3.2401(6) 2_657 ? Ba1 S2 3.2401(6) . ? S2 C5 1.711(3) . ? S1 C1 1.698(3) . ? S3 C9 1.708(3) . ? N1 C1 1.357(3) . ? N1 C2 1.389(3) . ? N1 B1 1.543(3) . ? N2 C1 1.361(3) . ? N2 C3 1.382(4) . ? N2 C4 1.459(3) . ? N3 C5 1.354(3) . ? N3 C6 1.385(3) . ? N3 B1 1.548(3) . ? N4 C5 1.352(3) . ? N4 C7 1.379(3) . ? N4 C8 1.460(3) . ? N5 C9 1.358(3) . ? N5 C10 1.384(3) . ? N5 B1 1.551(3) . ? N6 C9 1.351(3) . ? N6 C11 1.385(3) . ? N6 C12 1.462(3) . ? C7 C6 1.341(4) . ? C3 C2 1.340(4) . ? C11 C10 1.339(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ba1 O1 180.0 2_657 . ? O1 Ba1 S3 98.73(5) 2_657 2_657 ? O1 Ba1 S3 81.27(5) . 2_657 ? O1 Ba1 S3 81.27(5) 2_657 . ? O1 Ba1 S3 98.73(5) . . ? S3 Ba1 S3 180.000(10) 2_657 . ? O1 Ba1 S2 95.52(6) 2_657 2_657 ? O1 Ba1 S2 84.48(6) . 2_657 ? S3 Ba1 S2 103.727(16) 2_657 2_657 ? S3 Ba1 S2 76.273(16) . 2_657 ? O1 Ba1 S2 84.48(6) 2_657 . ? O1 Ba1 S2 95.52(6) . . ? S3 Ba1 S2 76.273(16) 2_657 . ? S3 Ba1 S2 103.727(16) . . ? S2 Ba1 S2 180.00(2) 2_657 . ? C5 S2 Ba1 113.41(9) . . ? C9 S3 Ba1 88.72(8) . . ? C1 N1 C2 108.3(2) . . ? C1 N1 B1 124.0(2) . . ? C2 N1 B1 126.1(2) . . ? C1 N2 C3 109.4(2) . . ? C1 N2 C4 125.8(2) . . ? C3 N2 C4 124.8(2) . . ? C5 N3 C6 108.3(2) . . ? C5 N3 B1 124.2(2) . . ? C6 N3 B1 127.5(2) . . ? C5 N4 C7 109.5(2) . . ? C5 N4 C8 125.0(2) . . ? C7 N4 C8 125.3(2) . . ? C9 N5 C10 108.1(2) . . ? C9 N5 B1 125.1(2) . . ? C10 N5 B1 126.7(2) . . ? C9 N6 C11 109.1(2) . . ? C9 N6 C12 125.4(2) . . ? C11 N6 C12 125.4(2) . . ? N4 C5 N3 107.0(2) . . ? N4 C5 S2 125.2(2) . . ? N3 C5 S2 127.77(18) . . ? C6 C7 N4 106.9(2) . . ? C7 C6 N3 108.2(2) . . ? N1 C1 N2 106.9(2) . . ? N1 C1 S1 127.53(19) . . ? N2 C1 S1 125.6(2) . . ? C2 C3 N2 107.0(2) . . ? C3 C2 N1 108.4(2) . . ? N6 C9 N5 107.3(2) . . ? N6 C9 S3 125.94(19) . . ? N5 C9 S3 126.77(19) . . ? C10 C11 N6 107.0(2) . . ? C11 C10 N5 108.5(2) . . ? N1 B1 N3 111.3(2) . . ? N1 B1 N5 109.2(2) . . ? N3 B1 N5 108.2(2) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 1.049 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.105 data_1 _database_code_depnum_ccdc_archive 'CCDC 285451' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Calcium bishydrotris(methimazolyl)borate hexawater' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H26 B Ca0.50 N6 O5 S3' _chemical_formula_weight 461.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ca Ca 0.2262 0.3064 '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' O O 0.0106 0.0060 '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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8138(6) _cell_length_b 9.4094(7) _cell_length_c 13.1360(9) _cell_angle_alpha 91.5160(10) _cell_angle_beta 93.0220(10) _cell_angle_gamma 90.5400(10) _cell_volume 1087.44(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7971 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 28.27 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 486 _exptl_absorpt_coefficient_mu 0.493 _exptl_absorpt_correction_type 'Empirical SADABS' _exptl_absorpt_correction_T_min 0.4220 _exptl_absorpt_correction_T_max 0.9208 _exptl_absorpt_process_details ? _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.458279 ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8988 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4814 _reflns_number_gt 4418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.3192P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4814 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1261 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.000 _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 B1 B 0.3312(2) 0.7995(2) 0.20450(14) 0.0135(4) Uani 1 1 d . . . C1 C 0.15687(18) 0.81302(17) 0.04090(13) 0.0131(3) Uani 1 1 d . . . C2 C 0.3061(2) 1.00355(18) 0.07266(14) 0.0167(3) Uani 1 1 d . . . H2 H 0.3773 1.0681 0.1058 0.020 Uiso 1 1 calc R . . C3 C 0.23275(19) 1.02149(18) -0.01899(14) 0.0163(3) Uani 1 1 d . . . H3 H 0.2423 1.1005 -0.0618 0.020 Uiso 1 1 calc R . . C4 C 0.0472(2) 0.8779(2) -0.13243(14) 0.0181(4) Uani 1 1 d . . . H4A H 0.1125 0.8547 -0.1885 0.027 Uiso 1 1 calc R . . H4B H -0.0106 0.9638 -0.1483 0.027 Uiso 1 1 calc R . . H4C H -0.0232 0.7986 -0.1235 0.027 Uiso 1 1 calc R . . C5 C 0.34107(19) 0.99714(18) 0.34637(13) 0.0151(3) Uani 1 1 d . . . C6 C 0.56239(19) 0.9568(2) 0.27627(14) 0.0179(4) Uani 1 1 d . . . H6 H 0.6371 0.9166 0.2350 0.021 Uiso 1 1 calc R . . C7 C 0.5849(2) 1.0652(2) 0.34507(14) 0.0193(4) Uani 1 1 d . . . H7 H 0.6776 1.1152 0.3610 0.023 Uiso 1 1 calc R . . C8 C 0.4219(2) 1.1975(2) 0.46694(15) 0.0217(4) Uani 1 1 d . . . H8A H 0.3690 1.2783 0.4364 0.033 Uiso 1 1 calc R . . H8B H 0.5198 1.2298 0.4986 0.033 Uiso 1 1 calc R . . H8C H 0.3598 1.1568 0.5189 0.033 Uiso 1 1 calc R . . C9 C 0.52041(19) 0.58985(18) 0.21531(14) 0.0151(3) Uani 1 1 d . . . C10 C 0.52323(19) 0.70790(19) 0.07138(13) 0.0157(3) Uani 1 1 d . . . H10 H 0.4991 0.7750 0.0204 0.019 Uiso 1 1 calc R . . C11 C 0.6284(2) 0.60514(19) 0.06574(14) 0.0177(4) Uani 1 1 d . . . H11 H 0.6921 0.5868 0.0108 0.021 Uiso 1 1 calc R . . C12 C 0.7156(2) 0.4068(2) 0.17935(16) 0.0241(4) Uani 1 1 d . . . H12A H 0.7671 0.4207 0.2469 0.036 Uiso 1 1 calc R . . H12B H 0.7915 0.3926 0.1282 0.036 Uiso 1 1 calc R . . H12C H 0.6487 0.3230 0.1794 0.036 Uiso 1 1 calc R . . Ca1 Ca 0.0000 0.5000 0.5000 0.01384(13) Uani 1 2 d S . . H1 H 0.246(3) 0.737(2) 0.2432(18) 0.021(6) Uiso 1 1 d . . . H5 H 0.150(3) 0.463(3) 0.167(2) 0.040(8) Uiso 1 1 d . . . H9 H 0.268(4) 0.438(3) 0.226(2) 0.046(8) Uiso 1 1 d . . . H13 H 0.058(3) 0.247(3) 0.802(3) 0.041(8) Uiso 1 1 d . . . H14 H 0.031(3) 0.155(3) 0.736(2) 0.039(8) Uiso 1 1 d . . . H15 H 0.080(3) 0.349(3) 0.321(3) 0.036(8) Uiso 1 1 d . . . H16 H 0.059(4) 0.251(4) 0.381(3) 0.059(11) Uiso 1 1 d . . . H17 H 0.155(3) 0.323(3) 0.654(3) 0.045(8) Uiso 1 1 d . . . H18 H 0.267(4) 0.406(3) 0.616(2) 0.048(8) Uiso 1 1 d . . . H19 H 0.261(3) 0.634(3) 0.408(2) 0.034(7) Uiso 1 1 d . . . H20 H 0.175(3) 0.732(3) 0.433(2) 0.028(7) Uiso 1 1 d . . . N1 N 0.25948(16) 0.87461(15) 0.11014(11) 0.0130(3) Uani 1 1 d . . . N2 N 0.14130(16) 0.90290(15) -0.03833(11) 0.0139(3) Uani 1 1 d . . . N3 N 0.41043(16) 0.91438(15) 0.27645(11) 0.0137(3) Uani 1 1 d . . . N4 N 0.44746(17) 1.08953(16) 0.38786(12) 0.0177(3) Uani 1 1 d . . . N5 N 0.45605(16) 0.69878(15) 0.16466(11) 0.0143(3) Uani 1 1 d . . . N6 N 0.62553(16) 0.53214(16) 0.15487(12) 0.0164(3) Uani 1 1 d . . . O1 O 0.18734(16) 0.65465(16) 0.44344(11) 0.0207(3) Uani 1 1 d . . . O2 O 0.17131(15) 0.38324(15) 0.60705(11) 0.0204(3) Uani 1 1 d . . . O3 O 0.04344(17) 0.32788(16) 0.37115(12) 0.0226(3) Uani 1 1 d . . . O4 O 0.18529(19) 0.40176(17) 0.20079(12) 0.0267(3) Uani 1 1 d . . . O5 O 0.09734(16) 0.20729(16) 0.75692(12) 0.0214(3) Uani 1 1 d . . . S1 S 0.06309(5) 0.65454(4) 0.04811(3) 0.01573(13) Uani 1 1 d . . . S2 S 0.15623(5) 0.98931(5) 0.38052(3) 0.01786(13) Uani 1 1 d . . . S3 S 0.48170(5) 0.53005(5) 0.33317(3) 0.01686(13) 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 B1 0.0114(8) 0.0155(8) 0.0136(9) -0.0022(7) -0.0006(7) 0.0032(7) C1 0.0091(7) 0.0156(7) 0.0145(8) -0.0027(6) 0.0003(6) 0.0030(6) C2 0.0133(8) 0.0166(8) 0.0200(9) -0.0006(6) -0.0009(6) -0.0011(6) C3 0.0147(8) 0.0160(8) 0.0183(9) 0.0026(6) 0.0014(6) 0.0002(6) C4 0.0157(8) 0.0223(9) 0.0156(8) -0.0033(7) -0.0051(6) 0.0031(7) C5 0.0152(8) 0.0155(8) 0.0144(8) -0.0006(6) -0.0013(6) 0.0023(6) C6 0.0117(8) 0.0237(9) 0.0179(9) -0.0022(7) -0.0011(6) -0.0001(6) C7 0.0153(8) 0.0243(9) 0.0180(9) -0.0023(7) -0.0019(7) -0.0030(7) C8 0.0266(10) 0.0187(8) 0.0193(9) -0.0079(7) -0.0009(7) -0.0001(7) C9 0.0096(7) 0.0159(8) 0.0191(9) -0.0051(6) -0.0022(6) 0.0007(6) C10 0.0146(8) 0.0194(8) 0.0130(8) -0.0011(6) 0.0025(6) -0.0021(6) C11 0.0151(8) 0.0211(8) 0.0168(8) -0.0040(7) 0.0019(6) -0.0008(7) C12 0.0223(9) 0.0246(9) 0.0254(10) -0.0026(8) 0.0017(8) 0.0134(8) Ca1 0.0110(2) 0.0157(2) 0.0147(3) -0.00021(18) -0.00005(17) 0.00195(17) N1 0.0115(6) 0.0135(6) 0.0138(7) -0.0006(5) -0.0005(5) 0.0004(5) N2 0.0119(7) 0.0155(7) 0.0141(7) 0.0000(5) -0.0003(5) 0.0025(5) N3 0.0101(6) 0.0174(7) 0.0132(7) -0.0019(5) -0.0012(5) 0.0008(5) N4 0.0168(7) 0.0182(7) 0.0175(8) -0.0050(6) -0.0018(6) -0.0003(6) N5 0.0102(7) 0.0169(7) 0.0155(7) -0.0040(5) -0.0005(5) 0.0017(5) N6 0.0132(7) 0.0178(7) 0.0182(8) -0.0035(6) 0.0015(5) 0.0034(5) O1 0.0165(7) 0.0197(7) 0.0266(8) 0.0036(6) 0.0064(5) 0.0027(5) O2 0.0134(6) 0.0264(7) 0.0213(7) 0.0038(6) -0.0030(5) 0.0022(5) O3 0.0286(8) 0.0189(7) 0.0204(7) -0.0017(6) 0.0028(6) 0.0057(6) O4 0.0270(8) 0.0280(8) 0.0244(8) 0.0034(6) -0.0063(6) -0.0062(6) O5 0.0171(7) 0.0254(7) 0.0216(7) -0.0007(6) 0.0023(5) 0.0002(6) S1 0.0149(2) 0.0147(2) 0.0173(2) -0.00106(16) -0.00151(16) -0.00239(15) S2 0.0139(2) 0.0175(2) 0.0223(3) -0.00367(17) 0.00321(17) 0.00261(16) S3 0.0125(2) 0.0215(2) 0.0167(2) 0.00179(17) -0.00008(16) 0.00315(16) _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 B1 N1 1.552(2) . ? B1 N3 1.553(2) . ? B1 N5 1.561(2) . ? C1 N2 1.361(2) . ? C1 N1 1.363(2) . ? C1 S1 1.7054(17) . ? C2 C3 1.351(2) . ? C2 N1 1.388(2) . ? C3 N2 1.380(2) . ? C4 N2 1.464(2) . ? C5 N4 1.356(2) . ? C5 N3 1.362(2) . ? C5 S2 1.7139(18) . ? C6 C7 1.351(2) . ? C6 N3 1.394(2) . ? C7 N4 1.381(2) . ? C8 N4 1.461(2) . ? C9 N5 1.350(2) . ? C9 N6 1.359(2) . ? C9 S3 1.7112(19) . ? C10 C11 1.349(3) . ? C10 N5 1.393(2) . ? C11 N6 1.374(2) . ? C12 N6 1.461(2) . ? Ca1 O2 2.3138(13) . ? Ca1 O2 2.3138(13) 2_566 ? Ca1 O1 2.3531(14) . ? Ca1 O1 2.3531(14) 2_566 ? Ca1 O3 2.3600(14) 2_566 ? Ca1 O3 2.3600(14) . ? 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 N1 B1 N3 108.17(14) . . ? N1 B1 N5 106.70(13) . . ? N3 B1 N5 108.07(13) . . ? N2 C1 N1 106.78(14) . . ? N2 C1 S1 124.96(12) . . ? N1 C1 S1 128.26(14) . . ? C3 C2 N1 108.29(15) . . ? C2 C3 N2 106.79(15) . . ? N4 C5 N3 107.09(15) . . ? N4 C5 S2 124.56(13) . . ? N3 C5 S2 128.35(13) . . ? C7 C6 N3 108.07(16) . . ? C6 C7 N4 106.95(16) . . ? N5 C9 N6 107.28(16) . . ? N5 C9 S3 128.27(13) . . ? N6 C9 S3 124.46(14) . . ? C11 C10 N5 108.37(16) . . ? C10 C11 N6 106.63(15) . . ? O2 Ca1 O2 180.0 . 2_566 ? O2 Ca1 O1 93.09(5) . . ? O2 Ca1 O1 86.91(5) 2_566 . ? O2 Ca1 O1 86.91(5) . 2_566 ? O2 Ca1 O1 93.09(5) 2_566 2_566 ? O1 Ca1 O1 180.0 . 2_566 ? O2 Ca1 O3 91.28(5) . 2_566 ? O2 Ca1 O3 88.72(5) 2_566 2_566 ? O1 Ca1 O3 87.41(6) . 2_566 ? O1 Ca1 O3 92.59(6) 2_566 2_566 ? O2 Ca1 O3 88.72(5) . . ? O2 Ca1 O3 91.28(5) 2_566 . ? O1 Ca1 O3 92.59(6) . . ? O1 Ca1 O3 87.41(6) 2_566 . ? O3 Ca1 O3 180.0 2_566 . ? C1 N1 C2 108.38(14) . . ? C1 N1 B1 124.59(14) . . ? C2 N1 B1 126.21(14) . . ? C1 N2 C3 109.75(14) . . ? C1 N2 C4 126.14(15) . . ? C3 N2 C4 124.07(15) . . ? C5 N3 C6 108.17(14) . . ? C5 N3 B1 125.74(14) . . ? C6 N3 B1 125.98(14) . . ? C5 N4 C7 109.73(14) . . ? C5 N4 C8 125.41(16) . . ? C7 N4 C8 124.86(16) . . ? C9 N5 C10 108.00(14) . . ? C9 N5 B1 126.12(15) . . ? C10 N5 B1 125.87(15) . . ? C9 N6 C11 109.72(14) . . ? C9 N6 C12 124.76(16) . . ? C11 N6 C12 125.45(15) . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 0.632 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.086 # Attachment '285452.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 285452' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Tetramercury tetrahydoxytris(methimazolyl)borate tetrachloride' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H60 B4 Cl4 Hg4 N24 S12 O13' _chemical_formula_weight 2553.32 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' N N 0.0061 0.0033 '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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.923(3) _cell_length_b 18.019(4) _cell_length_c 20.599(5) _cell_angle_alpha 81.587(4) _cell_angle_beta 76.885(4) _cell_angle_gamma 70.578(4) _cell_volume 4392.5(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3874 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.06 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2440 _exptl_absorpt_coefficient_mu 7.440 _exptl_absorpt_correction_type 'Empirical SADABS' _exptl_absorpt_correction_T_min 0.1880 _exptl_absorpt_correction_T_max 0.8658 _exptl_absorpt_process_details ? _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.217138 ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33523 _diffrn_reflns_av_R_equivalents 0.1200 _diffrn_reflns_av_sigmaI/netI 0.3036 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 28.33 _reflns_number_total 19743 _reflns_number_gt 7522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.Hydrogen atoms were placed in ideal positions and were refined isotropically. The solvent disorder (thirteen water per unit cell) was refined as a diffuse contribution without specific atom positions using the SQUEEZE program, but the density, absorption coefficient and other parameters reflect the full formula. ; _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^)+(0.0465P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19743 _refine_ls_number_parameters 852 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1450 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1556 _refine_ls_wR_factor_gt 0.1438 _refine_ls_goodness_of_fit_ref 0.761 _refine_ls_restrained_S_all 0.762 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 1.1360(13) 0.5709(11) 0.2919(10) 0.040(5) Uani 1 1 d . . . B2 B 1.0689(14) 0.9542(11) 0.2980(9) 0.035(5) Uani 1 1 d . . . B3 B 0.6158(13) 0.7813(9) 0.4079(8) 0.023(4) Uani 1 1 d . . . B4 B 0.8238(12) 0.8426(10) 0.0900(8) 0.024(4) Uani 1 1 d U . . C1 C 1.2816(14) 0.6204(12) 0.2040(9) 0.054(5) Uani 1 1 d . . . C2 C 1.2837(15) 0.5000(12) 0.1955(12) 0.075(7) Uani 1 1 d . . . H2 H 1.2659 0.4520 0.2043 0.090 Uiso 1 1 calc R . . C3 C 1.3591(16) 0.5164(15) 0.1430(14) 0.105(9) Uani 1 1 d . . . H3 H 1.4044 0.4823 0.1093 0.126 Uiso 1 1 calc R . . C4 C 1.4107(16) 0.6366(13) 0.0982(11) 0.088(7) Uani 1 1 d U . . H4A H 1.4914 0.6093 0.0896 0.132 Uiso 1 1 calc R . . H4B H 1.3963 0.6891 0.1128 0.132 Uiso 1 1 calc R . . H4C H 1.3818 0.6419 0.0571 0.132 Uiso 1 1 calc R . . C6 C 1.2952(14) 0.5151(11) 0.3622(13) 0.069(7) Uani 1 1 d . . . H6 H 1.3530 0.4875 0.3286 0.083 Uiso 1 1 calc R . . C7 C 1.3019(16) 0.5237(11) 0.4255(13) 0.073(7) Uani 1 1 d . . . H7 H 1.3688 0.5063 0.4430 0.088 Uiso 1 1 calc R . . C8 C 1.1604(15) 0.5792(12) 0.5299(11) 0.069(7) Uani 1 1 d . . . H8A H 1.1348 0.6364 0.5331 0.103 Uiso 1 1 calc R . . H8B H 1.2237 0.5548 0.5528 0.103 Uiso 1 1 calc R . . H8C H 1.0992 0.5577 0.5511 0.103 Uiso 1 1 calc R . . C11 C 1.0154(14) 0.4062(11) 0.3133(10) 0.057(5) Uani 1 1 d . . . H11 H 1.0002 0.3586 0.3320 0.068 Uiso 1 1 calc R . . C12 C 0.9072(5) 0.4370(5) 0.2208(2) 0.088(8) Uani 1 1 d . . . H12A H 0.8344 0.4780 0.2278 0.132 Uiso 1 1 calc R . . H12B H 0.8973 0.3853 0.2365 0.132 Uiso 1 1 calc R . . H12C H 0.9405 0.4374 0.1730 0.132 Uiso 1 1 calc R . . Cl4 Cl 0.3903(3) 0.2620(2) 0.26094(18) 0.0845(18) Uani 1 1 d R . . Cl2 Cl 0.2642(3) 0.1138(2) 0.1180(2) 0.094(2) Uani 1 1 d R . . Cl3 Cl 0.6763(3) 0.3972(3) 0.1795(2) 0.183(5) Uani 1 1 d R . . C20 C 1.1573(8) 0.8648(3) 0.5313(5) 0.054(5) Uani 1 1 d RU . . H20A H 1.2339 0.8566 0.5365 0.080 Uiso 1 1 d R . . H20B H 1.1462 0.8135 0.5316 0.080 Uiso 1 1 d R . . H20C H 1.1047 0.8935 0.5683 0.080 Uiso 1 1 d R . . C13 C 1.1990(10) 0.9197(9) 0.1847(8) 0.034(4) Uani 1 1 d . . . C14 C 1.2870(11) 0.9328(9) 0.2587(8) 0.036(4) Uani 1 1 d U . . H14 H 1.2993 0.9448 0.2992 0.043 Uiso 1 1 calc R . . C15 C 1.3653(10) 0.9068(8) 0.2062(7) 0.024(3) Uani 1 1 d U . . H15 H 1.4435 0.8949 0.2031 0.028 Uiso 1 1 calc R . . C16 C 1.3621(16) 0.8790(13) 0.0895(10) 0.084(7) Uani 1 1 d . . . H16A H 1.4437 0.8637 0.0837 0.126 Uiso 1 1 calc R . . H16B H 1.3360 0.9242 0.0581 0.126 Uiso 1 1 calc R . . H16C H 1.3405 0.8346 0.0810 0.126 Uiso 1 1 calc R . . C17 C 1.1247(10) 0.8884(9) 0.4071(7) 0.025(3) Uani 1 1 d . . . C18 C 1.0883(11) 1.0199(9) 0.3950(7) 0.031(4) Uani 1 1 d . . . H18 H 1.0681 1.0732 0.3767 0.037 Uiso 1 1 calc R . . C19 C 1.1209(6) 0.9897(5) 0.4600(4) 0.032(4) Uani 1 1 d . . . H19 H 1.1273 1.0196 0.4925 0.038 Uiso 1 1 calc R . . C5 C 1.1210(6) 0.5815(5) 0.4182(4) 0.038(4) Uani 1 1 d R . . C9 C 1.0189(6) 0.5146(5) 0.2465(4) 0.044(4) Uani 1 1 d R . . C10 C 1.0759(6) 0.4434(5) 0.3356(4) 0.038(4) Uani 1 1 d RU . . H10 H 1.1092 0.4274 0.3741 0.045 Uiso 1 1 d R . . C21 C 0.8759(11) 1.0609(9) 0.2992(7) 0.027(4) Uani 1 1 d . . . C22 C 1.0058(14) 1.0950(12) 0.2291(8) 0.055(5) Uani 1 1 d . . . H22 H 1.0775 1.0950 0.2046 0.065 Uiso 1 1 calc R . . C23 C 0.9117(12) 1.1504(10) 0.2213(8) 0.042(4) Uani 1 1 d . . . H23 H 0.9015 1.1960 0.1907 0.051 Uiso 1 1 calc R . . C24 C 0.7095(11) 1.1699(10) 0.2768(7) 0.040(4) Uani 1 1 d . . . H24A H 0.6679 1.1327 0.2789 0.060 Uiso 1 1 calc R . . H24B H 0.6955 1.2090 0.2388 0.060 Uiso 1 1 calc R . . H24C H 0.6850 1.1967 0.3183 0.060 Uiso 1 1 calc R . . C25 C 0.7322(11) 0.7731(8) 0.4969(8) 0.029(4) Uani 1 1 d . . . C26 C 0.6374(12) 0.6915(10) 0.5202(8) 0.043(4) Uani 1 1 d . . . H26 H 0.5878 0.6636 0.5177 0.051 Uiso 1 1 calc R . . C28 C 0.8254(11) 0.7439(9) 0.5949(8) 0.036(4) Uani 1 1 d . . . H28A H 0.9013 0.7086 0.5810 0.054 Uiso 1 1 calc R . . H28B H 0.7976 0.7306 0.6420 0.054 Uiso 1 1 calc R . . H28C H 0.8264 0.7987 0.5890 0.054 Uiso 1 1 calc R . . C29 C 0.5118(10) 0.9242(9) 0.3770(7) 0.030(4) Uani 1 1 d . . . C30 C 0.4655(12) 0.8820(10) 0.4843(8) 0.039(4) Uani 1 1 d . . . H30 H 0.4611 0.8489 0.5245 0.047 Uiso 1 1 calc R . . C31 C 0.4113(13) 0.9589(14) 0.4750(8) 0.060(6) Uani 1 1 d . . . H31 H 0.3613 0.9913 0.5087 0.072 Uiso 1 1 calc R . . C32 C 0.4015(13) 1.0686(10) 0.3798(8) 0.053(5) Uani 1 1 d . . . H32A H 0.4577 1.0783 0.3417 0.079 Uiso 1 1 calc R . . H32B H 0.3908 1.1035 0.4147 0.079 Uiso 1 1 calc R . . H32C H 0.3306 1.0790 0.3652 0.079 Uiso 1 1 calc R . . C33 C 0.6201(10) 0.6540(9) 0.3652(7) 0.027(4) Uani 1 1 d . . . C34 C 0.4507(11) 0.7453(11) 0.3812(7) 0.041(5) Uani 1 1 d . . . H34 H 0.3933 0.7935 0.3912 0.049 Uiso 1 1 calc R . . C35 C 0.4448(12) 0.6806(12) 0.3567(9) 0.056(6) Uani 1 1 d . . . H35 H 0.3781 0.6748 0.3493 0.067 Uiso 1 1 calc R . . C36 C 0.5799(14) 0.5476(11) 0.3171(10) 0.066(6) Uani 1 1 d . . . H36A H 0.6614 0.5245 0.3067 0.099 Uiso 1 1 calc R . . H36B H 0.5497 0.5548 0.2762 0.099 Uiso 1 1 calc R . . H36C H 0.5480 0.5122 0.3501 0.099 Uiso 1 1 calc R . . C37 C 1.0286(12) 0.8114(10) 0.0284(7) 0.038(4) Uani 1 1 d . . . C38 C 0.9149(12) 0.9181(10) -0.0111(7) 0.038(4) Uani 1 1 d . . . H38 H 0.8494 0.9609 -0.0159 0.046 Uiso 1 1 calc R . . C39 C 1.0222(12) 0.9067(10) -0.0501(8) 0.041(4) Uani 1 1 d . . . H39 H 1.0443 0.9371 -0.0893 0.049 Uiso 1 1 calc R . . C40 C 1.2103(9) 0.8056(9) -0.0423(6) 0.048(5) Uani 1 1 d U . . H40A H 1.2510 0.8340 -0.0258 0.072 Uiso 1 1 calc R . . H40B H 1.2273 0.8093 -0.0913 0.072 Uiso 1 1 calc R . . H40C H 1.2333 0.7500 -0.0253 0.072 Uiso 1 1 calc R . . C27 C 0.6946(9) 0.6812(9) 0.5713(6) 0.043(4) Uani 1 1 d R . . H27 H 0.6941 0.6450 0.6097 0.052 Uiso 1 1 calc R . . C41 C 0.7014(10) 0.9814(10) 0.1233(8) 0.032(4) Uani 1 1 d . . . C42 C 0.6291(10) 0.9258(9) 0.0635(6) 0.024(4) Uani 1 1 d . . . H42 H 0.6201 0.8910 0.0364 0.029 Uiso 1 1 calc R . . C43 C 0.5523(13) 0.9964(11) 0.0839(8) 0.043(5) Uani 1 1 d . . . H43 H 0.4800 1.0187 0.0730 0.052 Uiso 1 1 calc R . . C44 C 0.5472(12) 1.1033(9) 0.1576(9) 0.044(5) Uani 1 1 d . . . H44A H 0.5067 1.0922 0.2024 0.065 Uiso 1 1 calc R . . H44B H 0.4950 1.1417 0.1318 0.065 Uiso 1 1 calc R . . H44C H 0.6055 1.1251 0.1615 0.065 Uiso 1 1 calc R . . C45 C 0.7341(11) 0.7333(10) 0.1155(7) 0.032(4) Uani 1 1 d . . . C46 C 0.8402(14) 0.7363(12) 0.0121(9) 0.053(5) Uani 1 1 d . . . H46 H 0.8807 0.7560 -0.0273 0.064 Uiso 1 1 calc R . . C47 C 0.8146(15) 0.6692(11) 0.0205(10) 0.056(5) Uani 1 1 d . . . H47 H 0.8377 0.6306 -0.0111 0.067 Uiso 1 1 calc R . . C48 C 0.7143(15) 0.5976(12) 0.1150(11) 0.080(7) Uani 1 1 d . . . H48A H 0.6784 0.5809 0.0852 0.120 Uiso 1 1 calc R . . H48B H 0.6613 0.6122 0.1568 0.120 Uiso 1 1 calc R . . H48C H 0.7799 0.5541 0.1246 0.120 Uiso 1 1 calc R . . Cl1 Cl 0.9093(3) 0.7924(2) 0.27713(18) 0.0301(9) Uani 1 1 d . . . Hg1 Hg 1.10017(5) 0.78355(4) 0.17428(3) 0.04027(19) Uani 1 1 d . . . Hg2 Hg 0.97249(4) 0.76967(4) 0.40481(3) 0.03110(17) Uani 1 1 d . . . Hg3 Hg 0.74844(4) 0.94187(4) 0.28204(3) 0.02929(17) Uani 1 1 d . . . Hg4 Hg 0.82255(5) 0.67974(4) 0.25221(3) 0.03988(19) Uani 1 1 d . . . N1 N 1.2377(10) 0.5619(8) 0.2333(8) 0.050(4) Uani 1 1 d . . . N2 N 1.3575(11) 0.5931(10) 0.1480(9) 0.064(5) Uani 1 1 d . . . N3 N 1.1831(10) 0.5565(7) 0.3577(7) 0.038(4) Uani 1 1 d . . . N4 N 1.1941(13) 0.5626(10) 0.4616(10) 0.071(5) Uani 1 1 d . . . N5 N 1.0809(9) 0.5076(7) 0.2910(7) 0.040(4) Uani 1 1 d . . . N6 N 0.9817(10) 0.4523(7) 0.2585(6) 0.036(3) Uani 1 1 d . . . N7 N 1.1862(8) 0.9396(8) 0.2451(6) 0.032(3) Uani 1 1 d . . . N8 N 1.3132(8) 0.8999(7) 0.1559(6) 0.029(3) Uani 1 1 d . . . N9 N 1.0933(9) 0.9547(7) 0.3666(6) 0.028(3) Uani 1 1 d . . . N10 N 1.1404(9) 0.9097(8) 0.4644(6) 0.036(3) Uani 1 1 d . . . N11 N 0.9863(9) 1.0362(8) 0.2782(6) 0.040(4) Uani 1 1 d . . . N12 N 0.8306(9) 1.1263(7) 0.2683(7) 0.035(3) Uani 1 1 d . . . N13 N 0.6627(10) 0.7476(8) 0.4742(7) 0.043(4) Uani 1 1 d . . . N14 N 0.7527(10) 0.7349(8) 0.5543(6) 0.035(3) Uani 1 1 d . . . N15 N 0.5312(9) 0.8608(7) 0.4204(6) 0.031(3) Uani 1 1 d . . . N16 N 0.4403(9) 0.9843(8) 0.4072(6) 0.033(3) Uani 1 1 d . . . N17 N 0.5666(9) 0.7220(8) 0.3881(6) 0.033(3) Uani 1 1 d . . . N18 N 0.5513(9) 0.6235(8) 0.3440(7) 0.042(4) Uani 1 1 d . . . N19 N 0.9237(9) 0.8562(8) 0.0346(6) 0.036(3) Uani 1 1 d . . . N20 N 1.0881(8) 0.8414(7) -0.0187(6) 0.026(3) Uani 1 1 d U . . N21 N 0.7224(9) 0.9161(7) 0.0909(6) 0.027(3) Uani 1 1 d . . . N22 N 0.5986(9) 1.0304(8) 0.1237(6) 0.034(3) Uani 1 1 d . . . N23 N 0.7959(9) 0.7718(7) 0.0722(6) 0.032(3) Uani 1 1 d . . . N24 N 0.7489(13) 0.6653(9) 0.0829(9) 0.059(5) Uani 1 1 d . . . S1 S 1.2505(3) 0.7096(3) 0.2361(2) 0.0420(12) Uani 1 1 d . . . S2 S 1.0760(3) 0.7235(3) 0.0803(2) 0.0362(10) Uani 1 1 d . . . S3 S 1.0986(3) 0.9231(3) 0.1418(2) 0.0370(11) Uani 1 1 d . . . S4 S 1.1540(3) 0.7919(2) 0.3901(2) 0.0361(10) Uani 1 1 d . . . S5 S 0.7847(3) 0.8499(2) 0.45608(19) 0.0282(9) Uani 1 1 d . . . S6 S 0.9817(3) 0.6284(3) 0.4353(2) 0.0440(11) Uani 1 1 d . . . S7 S 0.8078(3) 1.0057(2) 0.35970(19) 0.0303(9) Uani 1 1 d . . . S8 S 0.5655(3) 0.9218(2) 0.29227(19) 0.0320(10) Uani 1 1 d . . . S9 S 0.7995(3) 0.9965(2) 0.16384(18) 0.0280(9) Uani 1 1 d . . . S10 S 0.7636(3) 0.6074(2) 0.3603(2) 0.0371(10) Uani 1 1 d . . . S11 S 0.6660(3) 0.7549(3) 0.1940(2) 0.0488(13) Uani 1 1 d . . . S12 S 0.9892(4) 0.5907(3) 0.1831(2) 0.0469(12) 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 B1 0.020(9) 0.029(12) 0.056(14) 0.002(10) 0.001(9) 0.005(8) B2 0.031(10) 0.046(13) 0.033(11) -0.019(10) 0.006(8) -0.018(9) B3 0.035(9) 0.015(10) 0.023(10) -0.001(8) -0.011(7) -0.011(8) B4 0.016(6) 0.025(8) 0.025(7) -0.003(6) 0.009(5) -0.004(6) C1 0.038(10) 0.087(16) 0.042(12) -0.002(11) -0.013(9) -0.023(10) C2 0.049(12) 0.053(14) 0.12(2) -0.033(14) 0.017(13) -0.022(11) C3 0.042(13) 0.10(2) 0.15(3) -0.050(19) 0.029(14) -0.004(13) C4 0.063(9) 0.098(11) 0.078(10) -0.004(8) 0.026(7) -0.018(8) C6 0.028(10) 0.045(13) 0.13(2) -0.021(14) -0.003(12) -0.004(9) C7 0.038(12) 0.042(13) 0.13(2) -0.001(14) -0.036(14) 0.009(10) C8 0.061(13) 0.072(16) 0.098(19) 0.005(14) -0.051(13) -0.034(12) C11 0.067(12) 0.052(13) 0.070(15) -0.005(11) -0.018(11) -0.039(11) C12 0.110(18) 0.043(14) 0.14(2) 0.017(14) -0.062(17) -0.043(13) Cl4 0.077(4) 0.124(5) 0.056(4) -0.028(4) -0.001(3) -0.035(4) Cl2 0.067(4) 0.138(6) 0.078(4) -0.001(4) -0.017(3) -0.033(4) Cl3 0.119(6) 0.197(9) 0.267(12) -0.096(9) 0.043(7) -0.115(7) C20 0.077(8) 0.035(8) 0.079(9) 0.032(7) -0.069(7) -0.038(6) C13 0.012(7) 0.052(11) 0.039(10) 0.021(9) -0.017(7) -0.014(7) C14 0.031(6) 0.061(8) 0.031(7) -0.012(6) -0.016(6) -0.025(6) C15 0.008(5) 0.040(7) 0.020(6) -0.008(6) -0.006(5) 0.000(5) C16 0.074(14) 0.11(2) 0.077(16) -0.071(15) 0.021(12) -0.044(14) C17 0.024(7) 0.037(10) 0.025(9) -0.019(8) -0.002(6) -0.016(7) C18 0.031(8) 0.032(10) 0.037(10) -0.007(8) 0.002(7) -0.023(7) C19 0.011(7) 0.056(12) 0.026(9) -0.007(8) 0.002(6) -0.009(7) C5 0.029(9) 0.048(12) 0.041(11) -0.007(9) -0.015(8) -0.007(8) C9 0.031(9) 0.035(11) 0.057(12) -0.014(9) 0.003(8) -0.003(8) C10 0.050(7) 0.018(7) 0.049(8) -0.001(6) -0.022(6) -0.010(6) C21 0.019(7) 0.039(10) 0.028(9) 0.005(8) -0.012(6) -0.014(7) C22 0.037(10) 0.103(17) 0.034(11) -0.018(11) 0.014(8) -0.044(11) C23 0.029(9) 0.044(11) 0.052(12) 0.008(9) -0.007(8) -0.013(8) C24 0.041(9) 0.055(12) 0.020(9) -0.001(8) -0.007(7) -0.009(8) C25 0.030(8) 0.012(8) 0.042(10) -0.010(7) -0.009(7) 0.001(6) C26 0.040(9) 0.062(13) 0.026(10) 0.003(9) 0.005(8) -0.026(9) C28 0.035(9) 0.031(10) 0.049(11) -0.003(8) -0.029(8) -0.005(7) C29 0.012(7) 0.045(11) 0.026(9) -0.016(8) 0.016(6) -0.007(7) C30 0.028(9) 0.044(12) 0.040(11) -0.009(9) 0.005(8) -0.010(8) C31 0.024(9) 0.13(2) 0.029(11) -0.016(12) 0.009(8) -0.036(11) C32 0.048(10) 0.065(14) 0.027(10) 0.013(10) -0.015(8) 0.005(9) C33 0.011(7) 0.040(10) 0.027(9) -0.002(8) -0.001(6) -0.007(7) C34 0.014(7) 0.083(14) 0.029(9) -0.002(10) -0.001(7) -0.022(8) C35 0.019(9) 0.102(17) 0.053(12) 0.002(12) -0.021(8) -0.021(10) C36 0.054(11) 0.067(14) 0.090(17) -0.043(13) 0.015(11) -0.040(11) C37 0.031(9) 0.067(13) 0.020(9) -0.010(8) -0.015(7) -0.012(8) C38 0.030(8) 0.057(12) 0.022(9) 0.022(9) -0.018(7) -0.008(8) C39 0.038(9) 0.051(12) 0.033(10) 0.006(9) -0.016(8) -0.012(8) C40 0.031(7) 0.051(8) 0.046(8) -0.008(7) 0.020(6) -0.008(6) C27 0.053(10) 0.047(12) 0.027(10) 0.012(9) -0.009(8) -0.018(9) C41 0.003(6) 0.051(11) 0.042(10) 0.000(9) -0.001(6) -0.011(7) C42 0.019(7) 0.046(11) 0.008(7) 0.004(7) -0.011(6) -0.008(7) C43 0.040(10) 0.067(13) 0.043(11) 0.008(10) -0.033(9) -0.032(10) C44 0.032(9) 0.031(10) 0.064(13) 0.019(10) -0.021(9) -0.007(8) C45 0.021(8) 0.042(11) 0.034(10) 0.016(8) -0.021(7) -0.009(7) C46 0.057(11) 0.094(16) 0.032(11) -0.033(11) -0.009(9) -0.042(11) C47 0.055(12) 0.051(14) 0.058(14) -0.024(11) -0.037(11) 0.016(10) C48 0.068(14) 0.090(18) 0.106(19) 0.021(15) -0.042(13) -0.053(13) Cl1 0.0232(18) 0.042(2) 0.028(2) 0.0033(18) -0.0069(15) -0.0151(17) Hg1 0.0340(3) 0.0553(5) 0.0393(4) 0.0097(3) -0.0176(3) -0.0227(3) Hg2 0.0194(3) 0.0376(4) 0.0373(4) 0.0053(3) -0.0087(3) -0.0114(3) Hg3 0.0220(3) 0.0501(4) 0.0216(3) 0.0008(3) -0.0072(2) -0.0183(3) Hg4 0.0252(3) 0.0529(5) 0.0405(4) 0.0090(4) -0.0083(3) -0.0147(3) N1 0.024(7) 0.037(9) 0.085(13) -0.015(9) 0.006(7) -0.010(7) N2 0.032(8) 0.053(11) 0.096(14) -0.014(10) 0.005(9) -0.009(8) N3 0.028(7) 0.033(8) 0.061(10) 0.006(7) -0.027(7) -0.011(6) N4 0.058(11) 0.053(12) 0.104(16) -0.016(11) -0.012(11) -0.018(9) N5 0.023(7) 0.033(9) 0.058(10) -0.003(7) -0.015(7) 0.003(6) N6 0.050(8) 0.026(8) 0.043(9) 0.016(7) -0.023(7) -0.025(7) N7 0.007(5) 0.059(9) 0.034(8) -0.019(7) 0.002(5) -0.013(6) N8 0.012(6) 0.050(9) 0.030(8) -0.006(7) -0.002(5) -0.017(6) N9 0.022(6) 0.026(8) 0.041(8) 0.009(7) -0.012(6) -0.015(6) N10 0.033(7) 0.039(9) 0.040(9) 0.003(7) -0.008(6) -0.018(6) N11 0.025(7) 0.065(10) 0.040(9) 0.015(8) -0.015(6) -0.029(7) N12 0.025(7) 0.030(8) 0.052(9) 0.008(7) -0.019(6) -0.010(6) N13 0.035(7) 0.045(9) 0.058(10) 0.030(8) -0.025(7) -0.027(7) N14 0.056(8) 0.044(9) 0.023(7) -0.001(7) -0.019(6) -0.031(7) N15 0.027(7) 0.033(8) 0.033(8) 0.009(7) -0.005(6) -0.017(6) N16 0.023(7) 0.061(10) 0.019(7) -0.003(7) -0.002(6) -0.021(7) N17 0.015(6) 0.062(10) 0.023(7) -0.001(7) -0.002(5) -0.017(7) N18 0.023(7) 0.063(11) 0.042(9) -0.012(8) 0.001(6) -0.018(7) N19 0.014(6) 0.050(9) 0.042(9) 0.004(7) -0.012(6) -0.007(6) N20 0.009(5) 0.044(7) 0.021(6) 0.002(5) 0.004(4) -0.011(5) N21 0.029(7) 0.035(8) 0.024(7) -0.009(6) -0.009(5) -0.012(6) N22 0.012(6) 0.059(10) 0.027(8) -0.020(7) -0.005(5) 0.000(6) N23 0.019(6) 0.034(8) 0.042(9) -0.015(7) -0.011(6) 0.001(6) N24 0.067(10) 0.051(11) 0.086(14) 0.009(10) -0.061(10) -0.029(9) S1 0.040(2) 0.042(3) 0.054(3) 0.009(2) -0.030(2) -0.018(2) S2 0.032(2) 0.044(3) 0.028(2) -0.002(2) -0.0053(17) -0.0066(19) S3 0.030(2) 0.052(3) 0.038(3) 0.015(2) -0.0206(19) -0.025(2) S4 0.0208(19) 0.042(3) 0.047(3) -0.011(2) -0.0072(18) -0.0082(18) S5 0.0294(19) 0.022(2) 0.032(2) -0.0026(18) -0.0056(17) -0.0076(17) S6 0.039(2) 0.042(3) 0.051(3) 0.000(2) -0.006(2) -0.015(2) S7 0.0278(19) 0.044(3) 0.027(2) -0.0068(19) -0.0079(17) -0.0170(18) S8 0.0178(18) 0.056(3) 0.027(2) 0.000(2) -0.0102(16) -0.0154(18) S9 0.0194(18) 0.048(3) 0.022(2) 0.0001(19) -0.0040(15) -0.0176(18) S10 0.025(2) 0.037(3) 0.045(3) 0.005(2) -0.0070(18) -0.0077(18) S11 0.018(2) 0.073(4) 0.050(3) 0.017(3) -0.0089(19) -0.014(2) S12 0.058(3) 0.035(3) 0.042(3) -0.002(2) -0.008(2) -0.010(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 B1 N5 1.54(2) . ? B1 N1 1.55(2) . ? B1 N3 1.56(2) . ? B2 N9 1.52(2) . ? B2 N11 1.57(2) . ? B2 N7 1.620(19) . ? B3 N15 1.50(2) . ? B3 N17 1.553(19) . ? B3 N13 1.579(19) . ? B4 N21 1.520(19) . ? B4 N23 1.55(2) . ? B4 N19 1.578(18) . ? C1 N1 1.36(2) . ? C1 N2 1.37(2) . ? C1 S1 1.71(2) . ? C2 N1 1.34(2) . ? C2 C3 1.35(3) . ? C3 N2 1.39(3) . ? C4 N2 1.39(2) . ? C6 C7 1.36(3) . ? C6 N3 1.41(2) . ? C7 N4 1.42(2) . ? C8 N4 1.42(2) . ? C11 N6 1.37(2) . ? C11 C10 1.368(17) . ? C12 N6 1.479(12) . ? C20 N10 1.514(13) . ? C13 N7 1.303(18) . ? C13 N8 1.405(16) . ? C13 S3 1.709(13) . ? C14 C15 1.323(19) . ? C14 N7 1.357(15) . ? C15 N8 1.396(16) . ? C16 N8 1.42(2) . ? C17 N9 1.352(17) . ? C17 N10 1.368(17) . ? C17 S4 1.723(15) . ? C18 N9 1.365(18) . ? C18 C19 1.470(16) . ? C19 N10 1.372(14) . ? C5 N3 1.368(16) . ? C5 N4 1.374(19) . ? C5 S6 1.694(8) . ? C9 N5 1.317(14) . ? C9 N6 1.334(13) . ? C9 S12 1.755(9) . ? C10 N5 1.378(14) . ? C21 N12 1.277(16) . ? C21 N11 1.332(17) . ? C21 S7 1.743(13) . ? C22 C23 1.32(2) . ? C22 N11 1.40(2) . ? C23 N12 1.394(18) . ? C24 N12 1.481(17) . ? C25 N14 1.313(17) . ? C25 N13 1.327(17) . ? C25 S5 1.763(14) . ? C26 N13 1.351(17) . ? C26 C27 1.376(19) . ? C28 N14 1.451(16) . ? C29 N16 1.298(18) . ? C29 N15 1.334(17) . ? C29 S8 1.728(15) . ? C30 C31 1.34(2) . ? C30 N15 1.422(19) . ? C31 N16 1.411(19) . ? C32 N16 1.498(19) . ? C33 N17 1.288(18) . ? C33 N18 1.362(17) . ? C33 S10 1.749(13) . ? C34 C35 1.37(2) . ? C34 N17 1.448(16) . ? C35 N18 1.41(2) . ? C36 N18 1.45(2) . ? C37 N20 1.269(17) . ? C37 N19 1.315(17) . ? C37 S2 1.785(16) . ? C38 N19 1.340(17) . ? C38 C39 1.40(2) . ? C39 N20 1.374(18) . ? C40 N20 1.488(14) . ? C27 N14 1.374(17) . ? C41 N22 1.326(16) . ? C41 N21 1.355(19) . ? C41 S9 1.776(14) . ? C42 C43 1.38(2) . ? C42 N21 1.394(15) . ? C43 N22 1.421(18) . ? C44 N22 1.462(19) . ? C45 N23 1.334(17) . ? C45 N24 1.42(2) . ? C45 S11 1.688(16) . ? C46 C47 1.33(2) . ? C46 N23 1.393(19) . ? C47 N24 1.38(2) . ? C48 N24 1.46(2) . ? Cl1 Hg4 2.779(4) . ? Cl1 Hg3 2.801(4) . ? Cl1 Hg1 2.840(3) . ? Cl1 Hg2 2.861(3) . ? Hg1 S1 2.465(4) . ? Hg1 S2 2.475(4) . ? Hg1 S3 2.500(4) . ? Hg2 S4 2.454(3) . ? Hg2 S5 2.459(4) . ? Hg2 S6 2.502(4) . ? Hg3 S8 2.467(3) . ? Hg3 S7 2.480(4) . ? Hg3 S9 2.516(4) . ? Hg4 S11 2.483(4) . ? Hg4 S12 2.493(5) . ? Hg4 S10 2.505(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 B1 N1 109.5(15) . . ? N5 B1 N3 108.9(13) . . ? N1 B1 N3 106.5(12) . . ? N9 B2 N11 110.0(13) . . ? N9 B2 N7 107.4(12) . . ? N11 B2 N7 108.8(12) . . ? N15 B3 N17 113.2(11) . . ? N15 B3 N13 107.4(13) . . ? N17 B3 N13 109.4(11) . . ? N21 B4 N23 109.7(11) . . ? N21 B4 N19 109.5(11) . . ? N23 B4 N19 107.9(12) . . ? N1 C1 N2 107.8(17) . . ? N1 C1 S1 124.7(14) . . ? N2 C1 S1 127.4(15) . . ? N1 C2 C3 109.7(19) . . ? C2 C3 N2 107(2) . . ? C7 C6 N3 104.4(18) . . ? C6 C7 N4 110.0(18) . . ? N6 C11 C10 105.0(13) . . ? N7 C13 N8 108.2(11) . . ? N7 C13 S3 128.6(11) . . ? N8 C13 S3 123.0(12) . . ? C15 C14 N7 108.6(13) . . ? C14 C15 N8 108.2(11) . . ? N9 C17 N10 107.9(12) . . ? N9 C17 S4 128.2(11) . . ? N10 C17 S4 123.6(12) . . ? N9 C18 C19 104.9(12) . . ? N10 C19 C18 106.1(10) . . ? N3 C5 N4 106.6(10) . . ? N3 C5 S6 126.3(7) . . ? N4 C5 S6 127.0(10) . . ? N5 C9 N6 106.7(9) . . ? N5 C9 S12 127.5(8) . . ? N6 C9 S12 125.8(7) . . ? C11 C10 N5 107.0(11) . . ? N12 C21 N11 111.4(12) . . ? N12 C21 S7 126.8(11) . . ? N11 C21 S7 121.8(11) . . ? C23 C22 N11 111.2(13) . . ? C22 C23 N12 103.7(14) . . ? N14 C25 N13 110.5(12) . . ? N14 C25 S5 125.5(11) . . ? N13 C25 S5 124.0(12) . . ? N13 C26 C27 109.2(13) . . ? N16 C29 N15 109.9(13) . . ? N16 C29 S8 126.3(12) . . ? N15 C29 S8 123.6(12) . . ? C31 C30 N15 104.6(15) . . ? C30 C31 N16 109.0(17) . . ? N17 C33 N18 111.5(12) . . ? N17 C33 S10 124.4(11) . . ? N18 C33 S10 124.1(13) . . ? C35 C34 N17 102.6(14) . . ? C34 C35 N18 110.9(13) . . ? N20 C37 N19 109.2(14) . . ? N20 C37 S2 126.8(12) . . ? N19 C37 S2 123.9(12) . . ? N19 C38 C39 105.9(13) . . ? N20 C39 C38 104.1(13) . . ? N14 C27 C26 104.7(11) . . ? N22 C41 N21 112.7(12) . . ? N22 C41 S9 124.2(13) . . ? N21 C41 S9 123.1(10) . . ? C43 C42 N21 106.1(13) . . ? C42 C43 N22 109.0(12) . . ? N23 C45 N24 103.6(14) . . ? N23 C45 S11 128.1(13) . . ? N24 C45 S11 127.9(13) . . ? C47 C46 N23 106.5(16) . . ? C46 C47 N24 108.4(17) . . ? Hg4 Cl1 Hg3 111.11(11) . . ? Hg4 Cl1 Hg1 105.17(13) . . ? Hg3 Cl1 Hg1 114.00(12) . . ? Hg4 Cl1 Hg2 114.88(12) . . ? Hg3 Cl1 Hg2 102.35(12) . . ? Hg1 Cl1 Hg2 109.62(10) . . ? S1 Hg1 S2 118.97(15) . . ? S1 Hg1 S3 112.04(12) . . ? S2 Hg1 S3 111.06(13) . . ? S1 Hg1 Cl1 100.49(13) . . ? S2 Hg1 Cl1 107.22(11) . . ? S3 Hg1 Cl1 105.51(13) . . ? S4 Hg2 S5 130.27(13) . . ? S4 Hg2 S6 113.30(13) . . ? S5 Hg2 S6 106.74(13) . . ? S4 Hg2 Cl1 108.78(12) . . ? S5 Hg2 Cl1 91.37(11) . . ? S6 Hg2 Cl1 100.12(13) . . ? S8 Hg3 S7 127.91(13) . . ? S8 Hg3 S9 106.71(11) . . ? S7 Hg3 S9 109.85(12) . . ? S8 Hg3 Cl1 106.99(12) . . ? S7 Hg3 Cl1 102.17(12) . . ? S9 Hg3 Cl1 99.48(12) . . ? S11 Hg4 S12 115.92(16) . . ? S11 Hg4 S10 113.73(12) . . ? S12 Hg4 S10 110.24(14) . . ? S11 Hg4 Cl1 105.04(13) . . ? S12 Hg4 Cl1 101.44(13) . . ? S10 Hg4 Cl1 109.43(12) . . ? C2 N1 C1 108.3(16) . . ? C2 N1 B1 125.3(15) . . ? C1 N1 B1 125.4(16) . . ? C1 N2 C4 127.1(19) . . ? C1 N2 C3 107.6(17) . . ? C4 N2 C3 124(2) . . ? C5 N3 C6 111.4(14) . . ? C5 N3 B1 124.6(11) . . ? C6 N3 B1 124.1(16) . . ? C5 N4 C7 107.3(18) . . ? C5 N4 C8 123.2(14) . . ? C7 N4 C8 129.5(19) . . ? C9 N5 C10 109.7(10) . . ? C9 N5 B1 120.3(12) . . ? C10 N5 B1 129.6(12) . . ? C9 N6 C11 111.2(11) . . ? C9 N6 C12 125.0(9) . . ? C11 N6 C12 123.6(10) . . ? C13 N7 C14 109.9(11) . . ? C13 N7 B2 122.7(11) . . ? C14 N7 B2 126.6(13) . . ? C15 N8 C13 105.0(12) . . ? C15 N8 C16 128.6(12) . . ? C13 N8 C16 126.3(13) . . ? C17 N9 C18 111.4(12) . . ? C17 N9 B2 123.0(13) . . ? C18 N9 B2 125.6(13) . . ? C17 N10 C19 109.7(11) . . ? C17 N10 C20 132.3(11) . . ? C19 N10 C20 117.4(10) . . ? C21 N11 C22 103.6(13) . . ? C21 N11 B2 126.3(12) . . ? C22 N11 B2 129.6(13) . . ? C21 N12 C23 110.1(12) . . ? C21 N12 C24 126.5(12) . . ? C23 N12 C24 123.4(12) . . ? C25 N13 C26 106.7(13) . . ? C25 N13 B3 125.2(12) . . ? C26 N13 B3 128.0(12) . . ? C25 N14 C27 108.9(11) . . ? C25 N14 C28 128.0(12) . . ? C27 N14 C28 123.2(12) . . ? C29 N15 C30 108.8(13) . . ? C29 N15 B3 127.1(13) . . ? C30 N15 B3 123.8(13) . . ? C29 N16 C31 107.7(15) . . ? C29 N16 C32 128.4(13) . . ? C31 N16 C32 123.6(15) . . ? C33 N17 C34 110.2(12) . . ? C33 N17 B3 127.8(11) . . ? C34 N17 B3 121.0(14) . . ? C33 N18 C35 104.7(14) . . ? C33 N18 C36 127.7(13) . . ? C35 N18 C36 127.6(13) . . ? C37 N19 C38 109.8(12) . . ? C37 N19 B4 125.4(13) . . ? C38 N19 B4 124.7(12) . . ? C37 N20 C39 110.6(12) . . ? C37 N20 C40 124.8(12) . . ? C39 N20 C40 124.2(11) . . ? C41 N21 C42 107.1(12) . . ? C41 N21 B4 126.6(11) . . ? C42 N21 B4 126.1(13) . . ? C41 N22 C43 104.8(13) . . ? C41 N22 C44 126.5(12) . . ? C43 N22 C44 128.7(12) . . ? C45 N23 C46 112.1(13) . . ? C45 N23 B4 123.3(13) . . ? C46 N23 B4 124.4(13) . . ? C47 N24 C45 109.1(14) . . ? C47 N24 C48 125.9(19) . . ? C45 N24 C48 124.4(18) . . ? C1 S1 Hg1 97.0(6) . . ? C37 S2 Hg1 98.8(5) . . ? C13 S3 Hg1 95.9(5) . . ? C17 S4 Hg2 106.0(4) . . ? C25 S5 Hg2 98.8(5) . . ? C5 S6 Hg2 102.0(3) . . ? C21 S7 Hg3 97.2(5) . . ? C29 S8 Hg3 103.3(5) . . ? C41 S9 Hg3 103.0(5) . . ? C33 S10 Hg4 95.7(5) . . ? C45 S11 Hg4 97.4(4) . . ? C9 S12 Hg4 96.2(3) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 3.689 _refine_diff_density_min -2.588 _refine_diff_density_rms 0.252 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.031 0.500 0.000 787.9 343.1 #_platon_squeeze_details