data_camps10 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H26 Cd N2 Te2' _chemical_formula_weight 638.01 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' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.0754(8) _cell_length_b 11.4619(7) _cell_length_c 15.1442(10) _cell_angle_alpha 90 _cell_angle_beta 112.3765(8) _cell_angle_gamma 90 _cell_volume 2098.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 9655 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 32.98 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.019 _exptl_crystal_F_000 1200 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 3.767 _shelx_estimated_absorpt_T_min 0.265 _shelx_estimated_absorpt_T_max 0.753 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5030 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36660 _diffrn_reflns_av_unetI/netI 0.0209 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.684 _diffrn_reflns_theta_max 33.004 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.959 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.959 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.959 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 7586 _reflns_number_gt 7079 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+1.0935P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7586 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0206 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0432 _refine_ls_wR_factor_gt 0.0424 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.67761(2) 0.46008(2) 0.15080(2) 0.01687(3) Uani 1 1 d . . . . . Te1 Te 0.82624(2) 0.31093(2) 0.12296(2) 0.02138(3) Uani 1 1 d . . . . . Te2 Te 0.54136(2) 0.64145(2) 0.05930(2) 0.01652(3) Uani 1 1 d . . . . . N1 N 0.78550(12) 0.52954(13) 0.31151(11) 0.0243(3) Uani 1 1 d . . . . . N2 N 0.60290(12) 0.35134(12) 0.24674(10) 0.0204(2) Uani 1 1 d . . . . . C1 C 0.73797(19) 0.63437(17) 0.33708(15) 0.0358(4) Uani 1 1 d . . . . . H1A H 0.7759 0.6500 0.4055 0.054 Uiso 1 1 calc R U . . . H1B H 0.6590 0.6218 0.3223 0.054 Uiso 1 1 calc R U . . . H1C H 0.7473 0.7012 0.3005 0.054 Uiso 1 1 calc R U . . . C2 C 0.90263(17) 0.55308(19) 0.32810(16) 0.0361(4) Uani 1 1 d . . . . . H2A H 0.9446 0.5655 0.3964 0.054 Uiso 1 1 calc R U . . . H2B H 0.9074 0.6230 0.2926 0.054 Uiso 1 1 calc R U . . . H2C H 0.9335 0.4863 0.3062 0.054 Uiso 1 1 calc R U . . . C3 C 0.77995(16) 0.42622(17) 0.36817(13) 0.0288(4) Uani 1 1 d . . . . . H3A H 0.8169 0.4447 0.4369 0.035 Uiso 1 1 calc R U . . . H3B H 0.8208 0.3610 0.3537 0.035 Uiso 1 1 calc R U . . . C4 C 0.66232(17) 0.38781(18) 0.34783(13) 0.0292(4) Uani 1 1 d . . . . . H4A H 0.6635 0.3218 0.3904 0.035 Uiso 1 1 calc R U . . . H4B H 0.6215 0.4529 0.3625 0.035 Uiso 1 1 calc R U . . . C5 C 0.62141(18) 0.22575(15) 0.23592(15) 0.0310(4) Uani 1 1 d . . . . . H5A H 0.5903 0.1799 0.2744 0.047 Uiso 1 1 calc R U . . . H5B H 0.7010 0.2106 0.2576 0.047 Uiso 1 1 calc R U . . . H5C H 0.5852 0.2035 0.1686 0.047 Uiso 1 1 calc R U . . . C6 C 0.48295(15) 0.37217(16) 0.21813(13) 0.0265(3) Uani 1 1 d . . . . . H6A H 0.4561 0.3295 0.2611 0.040 Uiso 1 1 calc R U . . . H6B H 0.4437 0.3450 0.1525 0.040 Uiso 1 1 calc R U . . . H6C H 0.4696 0.4558 0.2218 0.040 Uiso 1 1 calc R U . . . C7 C 0.84608(13) 0.38508(13) 0.00215(11) 0.0187(3) Uani 1 1 d . . . . . C8 C 0.93383(15) 0.34489(15) -0.02052(14) 0.0263(3) Uani 1 1 d . . . . . H8A H 0.9807 0.2850 0.0167 0.032 Uiso 1 1 calc R U . . . C9 C 0.95305(17) 0.39230(18) -0.09767(15) 0.0318(4) Uani 1 1 d . . . . . H9A H 1.0131 0.3646 -0.1126 0.038 Uiso 1 1 calc R U . . . C10 C 0.88558(17) 0.47907(19) -0.15234(13) 0.0321(4) Uani 1 1 d . . . . . H10A H 0.8996 0.5119 -0.2042 0.039 Uiso 1 1 calc R U . . . C11 C 0.79706(16) 0.51828(18) -0.13134(13) 0.0301(4) Uani 1 1 d . . . . . H11A H 0.7498 0.5773 -0.1695 0.036 Uiso 1 1 calc R U . . . C12 C 0.77699(14) 0.47154(15) -0.05452(12) 0.0227(3) Uani 1 1 d . . . . . H12A H 0.7160 0.4987 -0.0407 0.027 Uiso 1 1 calc R U . . . C13 C 0.65791(13) 0.77761(13) 0.08015(11) 0.0174(3) Uani 1 1 d . . . . . C14 C 0.77043(14) 0.75642(14) 0.10405(13) 0.0241(3) Uani 1 1 d . . . . . H14A H 0.7970 0.6784 0.1116 0.029 Uiso 1 1 calc R U . . . C15 C 0.84429(15) 0.84867(15) 0.11687(14) 0.0276(3) Uani 1 1 d . . . . . H15A H 0.9208 0.8332 0.1339 0.033 Uiso 1 1 calc R U . . . C16 C 0.80641(15) 0.96318(14) 0.10480(13) 0.0245(3) Uani 1 1 d . . . . . H16A H 0.8568 1.0259 0.1136 0.029 Uiso 1 1 calc R U . . . C17 C 0.69465(15) 0.98532(14) 0.07980(13) 0.0241(3) Uani 1 1 d . . . . . H17A H 0.6684 1.0634 0.0707 0.029 Uiso 1 1 calc R U . . . C18 C 0.62054(14) 0.89345(14) 0.06785(12) 0.0216(3) Uani 1 1 d . . . . . H18A H 0.5442 0.9095 0.0513 0.026 Uiso 1 1 calc R U . . . 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 Cd 0.01792(5) 0.01383(5) 0.02074(5) 0.00228(3) 0.00947(4) 0.00162(3) Te1 0.02237(5) 0.01652(5) 0.02836(6) 0.00393(4) 0.01315(4) 0.00532(3) Te2 0.01444(4) 0.01417(4) 0.01960(5) 0.00048(3) 0.00497(3) -0.00019(3) N1 0.0234(7) 0.0215(6) 0.0241(7) -0.0018(5) 0.0046(5) 0.0030(5) N2 0.0236(7) 0.0179(6) 0.0223(6) 0.0041(5) 0.0117(5) 0.0020(5) C1 0.0456(12) 0.0259(9) 0.0311(9) -0.0053(7) 0.0093(8) 0.0103(8) C2 0.0252(9) 0.0375(10) 0.0378(10) -0.0062(8) 0.0032(8) -0.0066(8) C3 0.0290(9) 0.0290(9) 0.0227(8) 0.0029(6) 0.0033(7) 0.0054(7) C4 0.0341(9) 0.0348(9) 0.0202(7) 0.0052(7) 0.0121(7) 0.0024(7) C5 0.0423(11) 0.0181(7) 0.0418(10) 0.0071(7) 0.0261(9) 0.0027(7) C6 0.0239(8) 0.0293(8) 0.0310(8) 0.0054(7) 0.0158(7) 0.0010(6) C7 0.0178(7) 0.0172(6) 0.0222(7) -0.0044(5) 0.0087(6) -0.0029(5) C8 0.0242(8) 0.0227(8) 0.0356(9) -0.0057(7) 0.0154(7) 0.0011(6) C9 0.0311(9) 0.0368(10) 0.0367(10) -0.0092(8) 0.0231(8) -0.0037(8) C10 0.0326(10) 0.0430(11) 0.0242(8) -0.0032(7) 0.0146(7) -0.0103(8) C11 0.0261(9) 0.0358(10) 0.0269(8) 0.0052(7) 0.0085(7) -0.0029(7) C12 0.0192(7) 0.0241(7) 0.0250(7) 0.0015(6) 0.0087(6) 0.0006(6) C13 0.0190(7) 0.0141(6) 0.0191(6) 0.0005(5) 0.0074(5) -0.0003(5) C14 0.0187(7) 0.0162(7) 0.0355(9) 0.0011(6) 0.0082(6) 0.0006(5) C15 0.0191(7) 0.0224(8) 0.0398(10) 0.0006(7) 0.0095(7) -0.0029(6) C16 0.0267(8) 0.0182(7) 0.0273(8) -0.0007(6) 0.0091(7) -0.0061(6) C17 0.0314(9) 0.0140(6) 0.0279(8) 0.0011(6) 0.0125(7) 0.0000(6) C18 0.0222(7) 0.0163(6) 0.0263(7) 0.0020(5) 0.0095(6) 0.0024(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd N2 2.3874(13) . ? Cd N1 2.4358(15) . ? Cd Te1 2.73873(19) . ? Cd Te2 2.74511(18) . ? Te1 C7 2.1209(16) . ? Te2 C13 2.1193(15) . ? N1 C1 1.471(2) . ? N1 C2 1.479(3) . ? N1 C3 1.480(2) . ? N2 C6 1.479(2) . ? N2 C5 1.479(2) . ? N2 C4 1.489(2) . ? C3 C4 1.515(3) . ? C7 C12 1.394(2) . ? C7 C8 1.395(2) . ? C8 C9 1.395(3) . ? C9 C10 1.377(3) . ? C10 C11 1.387(3) . ? C11 C12 1.393(2) . ? C13 C14 1.396(2) . ? C13 C18 1.403(2) . ? C14 C15 1.395(2) . ? C15 C16 1.390(2) . ? C16 C17 1.386(3) . ? C17 C18 1.395(2) . ? 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 N2 Cd N1 77.18(5) . . ? N2 Cd Te1 104.27(3) . . ? N1 Cd Te1 100.53(4) . . ? N2 Cd Te2 111.42(3) . . ? N1 Cd Te2 105.93(3) . . ? Te1 Cd Te2 139.217(6) . . ? C7 Te1 Cd 102.10(4) . . ? C13 Te2 Cd 101.00(4) . . ? C1 N1 C2 108.67(16) . . ? C1 N1 C3 112.46(16) . . ? C2 N1 C3 108.87(15) . . ? C1 N1 Cd 112.84(11) . . ? C2 N1 Cd 113.43(12) . . ? C3 N1 Cd 100.38(10) . . ? C6 N2 C5 108.94(14) . . ? C6 N2 C4 109.63(14) . . ? C5 N2 C4 110.11(14) . . ? C6 N2 Cd 111.80(10) . . ? C5 N2 Cd 108.57(10) . . ? C4 N2 Cd 107.76(10) . . ? N1 C3 C4 112.63(15) . . ? N2 C4 C3 112.50(15) . . ? C12 C7 C8 118.94(16) . . ? C12 C7 Te1 123.53(12) . . ? C8 C7 Te1 117.52(13) . . ? C7 C8 C9 120.30(17) . . ? C10 C9 C8 120.42(17) . . ? C9 C10 C11 119.71(17) . . ? C10 C11 C12 120.38(18) . . ? C11 C12 C7 120.23(16) . . ? C14 C13 C18 118.59(14) . . ? C14 C13 Te2 122.52(11) . . ? C18 C13 Te2 118.88(11) . . ? C15 C14 C13 120.64(15) . . ? C16 C15 C14 120.28(16) . . ? C17 C16 C15 119.64(15) . . ? C16 C17 C18 120.34(15) . . ? C17 C18 C13 120.50(15) . . ? _refine_diff_density_max 1.012 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.091 _shelxl_version_number 2013-4 _shelx_res_file ; TITL camps10 in P2(1)/c CELL 0.71073 13.07540 11.46190 15.14420 90.0000 112.3765 90.0000 ZERR 4.00 0.00080 0.00070 0.00100 0.0000 0.0008 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N CD TE UNIT 72 104 8 4 8 TEMP -143.150 SIZE .48 .20 .08 L.S. 16 BOND FMAP 2 PLAN 20 ACTA WPDB -1 REM EXTI 0.000020 WGHT 0.015400 1.093500 FVAR 0.08703 CD 4 0.677612 0.460079 0.150796 11.00000 0.01792 0.01383 = 0.02074 0.00228 0.00947 0.00162 TE1 5 0.826240 0.310930 0.122962 11.00000 0.02237 0.01652 = 0.02836 0.00393 0.01315 0.00532 TE2 5 0.541364 0.641446 0.059302 11.00000 0.01444 0.01417 = 0.01960 0.00048 0.00497 -0.00019 N1 3 0.785500 0.529540 0.311505 11.00000 0.02338 0.02148 = 0.02407 -0.00183 0.00460 0.00300 N2 3 0.602896 0.351338 0.246740 11.00000 0.02359 0.01789 = 0.02229 0.00410 0.01165 0.00199 C1 1 0.737973 0.634371 0.337078 11.00000 0.04561 0.02588 = 0.03111 -0.00526 0.00933 0.01033 AFIX 137 H1A 2 0.775881 0.649990 0.405501 11.00000 -1.50000 H1B 2 0.659031 0.621778 0.322287 11.00000 -1.50000 H1C 2 0.747339 0.701195 0.300486 11.00000 -1.50000 AFIX 0 C2 1 0.902627 0.553077 0.328101 11.00000 0.02522 0.03751 = 0.03782 -0.00616 0.00316 -0.00661 AFIX 137 H2A 2 0.944603 0.565525 0.396448 11.00000 -1.50000 H2B 2 0.907353 0.623001 0.292607 11.00000 -1.50000 H2C 2 0.933518 0.486296 0.306244 11.00000 -1.50000 AFIX 0 C3 1 0.779950 0.426218 0.368168 11.00000 0.02898 0.02900 = 0.02268 0.00290 0.00326 0.00540 AFIX 23 H3A 2 0.816854 0.444721 0.436948 11.00000 -1.20000 H3B 2 0.820768 0.360998 0.353747 11.00000 -1.20000 AFIX 0 C4 1 0.662317 0.387806 0.347835 11.00000 0.03415 0.03478 = 0.02023 0.00520 0.01208 0.00243 AFIX 23 H4A 2 0.663466 0.321797 0.390364 11.00000 -1.20000 H4B 2 0.621543 0.452902 0.362475 11.00000 -1.20000 AFIX 0 C5 1 0.621406 0.225745 0.235922 11.00000 0.04227 0.01806 = 0.04180 0.00709 0.02610 0.00268 AFIX 137 H5A 2 0.590346 0.179929 0.274397 11.00000 -1.50000 H5B 2 0.700973 0.210566 0.257578 11.00000 -1.50000 H5C 2 0.585165 0.203530 0.168623 11.00000 -1.50000 AFIX 0 C6 1 0.482945 0.372168 0.218130 11.00000 0.02390 0.02927 = 0.03099 0.00539 0.01585 0.00102 AFIX 137 H6A 2 0.456066 0.329506 0.261107 11.00000 -1.50000 H6B 2 0.443690 0.344982 0.152483 11.00000 -1.50000 H6C 2 0.469595 0.455819 0.221842 11.00000 -1.50000 AFIX 0 C7 1 0.846084 0.385078 0.002155 11.00000 0.01779 0.01717 = 0.02217 -0.00441 0.00867 -0.00289 C8 1 0.933831 0.344885 -0.020516 11.00000 0.02424 0.02274 = 0.03555 -0.00570 0.01541 0.00112 AFIX 43 H8A 2 0.980710 0.284961 0.016740 11.00000 -1.20000 AFIX 0 C9 1 0.953051 0.392303 -0.097667 11.00000 0.03110 0.03678 = 0.03665 -0.00915 0.02315 -0.00367 AFIX 43 H9A 2 1.013055 0.364558 -0.112572 11.00000 -1.20000 AFIX 0 C10 1 0.885580 0.479072 -0.152339 11.00000 0.03257 0.04303 = 0.02420 -0.00321 0.01462 -0.01029 AFIX 43 H10A 2 0.899623 0.511925 -0.204214 11.00000 -1.20000 AFIX 0 C11 1 0.797057 0.518276 -0.131339 11.00000 0.02613 0.03577 = 0.02685 0.00516 0.00848 -0.00295 AFIX 43 H11A 2 0.749820 0.577341 -0.169546 11.00000 -1.20000 AFIX 0 C12 1 0.776995 0.471536 -0.054524 11.00000 0.01920 0.02406 = 0.02500 0.00155 0.00872 0.00059 AFIX 43 H12A 2 0.716039 0.498661 -0.040718 11.00000 -1.20000 AFIX 0 C13 1 0.657908 0.777612 0.080155 11.00000 0.01902 0.01409 = 0.01913 0.00052 0.00740 -0.00026 C14 1 0.770434 0.756423 0.104049 11.00000 0.01874 0.01616 = 0.03546 0.00105 0.00818 0.00063 AFIX 43 H14A 2 0.796952 0.678416 0.111648 11.00000 -1.20000 AFIX 0 C15 1 0.844295 0.848668 0.116873 11.00000 0.01909 0.02243 = 0.03978 0.00055 0.00950 -0.00289 AFIX 43 H15A 2 0.920813 0.833177 0.133926 11.00000 -1.20000 AFIX 0 C16 1 0.806409 0.963180 0.104804 11.00000 0.02674 0.01818 = 0.02735 -0.00071 0.00905 -0.00610 AFIX 43 H16A 2 0.856830 1.025920 0.113647 11.00000 -1.20000 AFIX 0 C17 1 0.694649 0.985319 0.079795 11.00000 0.03138 0.01398 = 0.02790 0.00107 0.01249 0.00003 AFIX 43 H17A 2 0.668387 1.063433 0.070744 11.00000 -1.20000 AFIX 0 C18 1 0.620537 0.893450 0.067849 11.00000 0.02220 0.01634 = 0.02631 0.00197 0.00945 0.00238 AFIX 43 H18A 2 0.544189 0.909489 0.051256 11.00000 -1.20000 AFIX 0 HKLF 4 REM camps10 in P2(1)/c REM R1 = 0.0184 for 7079 Fo > 4sig(Fo) and 0.0206 for all 7586 data REM 212 parameters refined using 0 restraints END WGHT 0.0154 1.0929 REM Highest difference peak 1.012, deepest hole -0.705, 1-sigma level 0.091 Q1 1 0.4792 0.6419 0.0306 11.00000 0.05 1.01 Q2 1 0.8902 0.3143 0.1542 11.00000 0.05 0.94 Q3 1 0.6030 0.6418 0.0884 11.00000 0.05 0.87 Q4 1 0.7605 0.3113 0.0938 11.00000 0.05 0.81 Q5 1 0.7395 0.4609 0.1783 11.00000 0.05 0.81 Q6 1 0.8284 0.2868 0.1689 11.00000 0.05 0.75 Q7 1 0.6125 0.4593 0.1136 11.00000 0.05 0.73 Q8 1 0.5276 0.6406 0.0025 11.00000 0.05 0.67 Q9 1 0.6853 0.4712 0.2030 11.00000 0.05 0.67 Q10 1 0.5457 0.6531 0.1143 11.00000 0.05 0.63 Q11 1 0.8355 0.3598 0.1497 11.00000 0.05 0.58 Q12 1 0.8233 0.3322 0.0675 11.00000 0.05 0.54 Q13 1 0.7125 0.7654 0.0856 11.00000 0.05 0.53 Q14 1 0.6762 0.4816 0.1035 11.00000 0.05 0.52 Q15 1 0.7880 0.4908 -0.0906 11.00000 0.05 0.49 Q16 1 0.8208 0.9064 0.1070 11.00000 0.05 0.47 Q17 1 0.7173 0.4041 0.3533 11.00000 0.05 0.47 Q18 1 0.7519 0.9729 0.0887 11.00000 0.05 0.45 Q19 1 0.6227 0.3937 0.2182 11.00000 0.05 0.43 Q20 1 0.6344 0.8363 0.0690 11.00000 0.05 0.42 ; _shelx_res_checksum 9775 _shelx_hkl_file ; -1 0 0 184.94 5.94 1 0 0 184.22 6.03 1 0 0 183.48 6.01 -2 0 0 214.43 6.66 2 0 0 208.24 6.74 -2 0 0 204.35 6.64 2 0 0 205.38 6.81 3 0 0 240.91 7.55 -3 0 0 232.94 7.38 3 0 0 231.50 7.52 -3 0 0 217.10 7.40 -4 0 0 9.66 0.39 4 0 0 7.58 0.38 -5 0 0 0.41 0.10 5 0 0 0.19 0.06 -5 0 0 0.13 0.08 5 0 0 0.11 0.08 -6 0 0 458.80 14.70 6 0 0 477.42 14.94 6 0 0 450.86 14.97 -6 0 0 455.48 14.74 -7 0 0 1.03 0.17 7 0 0 1.67 0.23 7 0 0 1.74 0.18 -7 0 0 1.00 0.20 -8 0 0 400.81 13.53 8 0 0 422.77 13.77 -8 0 0 432.19 13.49 8 0 0 426.30 13.70 9 0 0 35.04 1.45 -9 0 0 36.67 1.34 9 0 0 35.00 1.34 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11 -6 0 39.75 1.69 11 6 0 36.35 1.56 -11 6 0 33.78 1.54 11 6 0 37.70 1.60 12 -6 0 0.11 0.17 -12 -6 0 0.03 0.16 12 6 0 0.13 0.15 -12 6 0 0.37 0.19 12 6 0 0.33 0.20 -13 -6 0 12.96 0.88 13 -6 0 13.05 0.90 13 6 0 13.42 0.88 -13 6 0 12.73 0.80 13 6 0 12.07 0.78 -14 -6 0 23.69 1.33 14 -6 0 24.39 1.36 14 6 0 26.98 1.34 -14 6 0 25.09 1.26 14 6 0 25.95 1.25 15 -6 0 0.52 0.28 -15 -6 0 0.44 0.26 -15 6 0 0.12 0.22 15 6 0 -0.12 0.21 -16 -6 0 0.41 0.29 16 -6 0 0.33 0.28 16 6 0 0.66 0.30 -16 6 0 0.41 0.22 0 -7 0 -0.04 0.05 0 -7 0 0.30 0.11 0 -7 0 0.20 0.09 0 7 0 0.15 0.08 1 -7 0 267.25 8.35 -1 -7 0 263.33 8.38 1 -7 0 258.32 8.62 -1 -7 0 264.26 8.57 1 -7 0 260.20 8.59 -1 -7 0 267.44 8.65 -1 7 0 251.48 8.46 1 7 0 258.52 8.42 -2 -7 0 5.35 0.29 -2 -7 0 4.52 0.35 2 -7 0 5.30 0.33 2 -7 0 5.11 0.25 2 -7 0 4.66 0.33 2 7 0 4.87 0.30 2 7 0 5.31 0.28 -2 7 0 4.88 0.34 -3 -7 0 3.63 0.26 3 -7 0 4.38 0.32 3 -7 0 4.27 0.29 -3 -7 0 3.50 0.31 3 7 0 4.15 0.22 3 7 0 3.91 0.27 -3 7 0 4.30 0.32 -3 7 0 3.90 0.21 4 -7 0 0.76 0.14 4 -7 0 0.33 0.12 -4 -7 0 0.16 0.10 -4 -7 0 0.48 0.12 -4 7 0 0.23 0.06 -4 7 0 0.16 0.10 4 7 0 0.17 0.08 -5 -7 0 101.30 3.41 5 -7 0 104.50 3.43 5 -7 0 94.29 3.48 -5 -7 0 101.29 3.52 -5 7 0 101.18 3.28 5 7 0 94.40 3.41 -5 7 0 102.91 3.48 -6 -7 0 5.78 0.42 6 -7 0 6.92 0.39 -6 -7 0 5.35 0.42 6 -7 0 5.18 0.43 -6 7 0 5.72 0.32 6 7 0 6.91 0.41 -6 7 0 6.83 0.46 7 -7 0 141.76 5.24 -7 -7 0 152.74 5.27 7 -7 0 163.82 5.17 -7 -7 0 157.47 5.20 -7 7 0 156.16 5.02 -7 7 0 148.62 5.20 7 7 0 151.68 5.18 -8 -7 0 0.11 0.12 -8 -7 0 0.13 0.12 8 -7 0 0.29 0.15 -8 7 0 0.25 0.14 -9 -7 0 19.24 1.00 -9 -7 0 18.60 0.95 9 -7 0 19.33 1.00 9 7 0 19.29 0.93 -9 7 0 19.43 0.96 10 -7 0 -0.02 0.15 -10 -7 0 0.57 0.20 -10 7 0 0.29 0.17 -11 -7 0 15.00 0.93 11 -7 0 16.86 0.98 11 7 0 16.17 0.89 -11 7 0 14.92 0.88 11 7 0 16.78 0.89 12 -7 0 4.26 0.54 -12 -7 0 4.13 0.52 12 7 0 4.98 0.52 12 7 0 4.31 0.48 -12 7 0 4.78 0.50 -13 -7 0 63.00 2.65 13 -7 0 65.24 2.71 13 7 0 66.05 2.58 -13 7 0 64.61 2.57 13 7 0 66.78 2.64 -14 -7 0 3.22 0.52 14 -7 0 4.00 0.58 -14 7 0 4.02 0.49 14 7 0 2.91 0.49 14 7 0 3.37 0.46 15 -7 0 22.83 1.40 -15 -7 0 24.03 1.38 15 7 0 25.28 1.29 15 7 0 26.80 1.38 -15 7 0 26.79 1.32 -16 -7 0 0.00 0.21 16 -7 0 0.01 0.24 -16 7 0 0.19 0.19 0 -8 0 7.59 0.46 0 -8 0 8.05 0.45 0 -8 0 7.73 0.37 0 8 0 7.99 0.43 1 -8 0 104.96 3.55 1 -8 0 104.55 3.58 1 -8 0 104.63 3.38 -1 -8 0 103.05 3.54 -1 -8 0 106.85 3.42 -1 -8 0 102.11 3.59 1 8 0 100.62 3.44 -1 8 0 99.14 3.49 2 -8 0 162.73 5.15 2 -8 0 164.33 5.39 -2 -8 0 162.02 5.21 2 -8 0 166.22 5.38 -2 -8 0 152.81 5.41 2 8 0 160.44 5.21 -2 8 0 154.97 5.30 2 8 0 153.57 5.30 -3 -8 0 2.00 0.26 3 -8 0 1.92 0.24 -3 -8 0 2.28 0.21 3 -8 0 1.98 0.23 3 8 0 1.64 0.20 -3 8 0 1.75 0.24 3 8 0 2.12 0.17 -3 8 0 2.25 0.15 -4 -8 0 51.41 1.87 -4 -8 0 49.81 1.98 4 -8 0 52.45 1.97 4 -8 0 54.76 1.94 -4 8 0 53.43 1.76 4 8 0 51.63 1.89 -4 8 0 53.02 1.97 -5 -8 0 23.18 1.10 -5 -8 0 26.04 1.05 5 -8 0 24.46 1.09 5 -8 0 26.12 1.05 5 8 0 24.17 1.02 -5 8 0 25.33 1.11 -5 8 0 25.80 0.92 6 -8 0 89.31 3.35 6 -8 0 97.92 3.29 -6 -8 0 96.48 3.29 -6 -8 0 95.19 3.39 6 8 0 94.42 3.28 -6 8 0 91.84 3.34 -7 -8 0 0.00 0.10 7 -8 0 0.43 0.16 -7 -8 0 0.23 0.15 -7 8 0 0.52 0.19 7 8 0 0.06 0.09 8 -8 0 34.51 1.48 -8 -8 0 33.79 1.44 -8 -8 0 34.23 1.46 8 8 0 31.97 1.38 -8 8 0 34.43 1.46 9 -8 0 34.57 1.56 -9 -8 0 37.87 1.56 -9 -8 0 33.18 1.53 9 8 0 37.18 1.50 -9 8 0 34.42 1.52 -10 -8 0 15.12 0.93 10 -8 0 15.62 0.94 -10 -8 0 18.29 0.95 10 8 0 16.19 0.87 -10 8 0 15.80 0.91 10 8 0 17.73 0.92 11 -8 0 0.17 0.19 -11 -8 0 0.55 0.24 11 8 0 0.18 0.17 -11 8 0 0.39 0.20 11 8 0 0.13 0.19 -12 -8 0 77.45 3.16 12 -8 0 83.43 3.23 12 8 0 84.46 3.14 -12 8 0 82.64 3.11 12 8 0 79.70 3.10 13 -8 0 10.72 0.87 -13 -8 0 10.17 0.84 13 8 0 12.92 0.82 13 8 0 12.83 0.85 -13 8 0 12.90 0.84 -14 -8 0 4.19 0.58 14 -8 0 3.38 0.56 -14 8 0 4.73 0.53 14 8 0 4.51 0.55 14 8 0 5.36 0.54 15 -8 0 11.81 0.97 -15 -8 0 12.85 0.96 -15 8 0 13.98 0.91 15 8 0 11.96 0.86 -16 8 0 4.92 0.58 0 -9 0 0.30 0.11 0 -9 0 -0.01 0.06 0 -9 0 0.15 0.11 0 9 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9 0 20.44 1.05 9 9 0 19.73 0.98 -10 -9 0 126.00 4.63 10 -9 0 128.01 4.70 -10 -9 0 137.47 4.70 10 9 0 130.86 4.59 -10 9 0 126.07 4.61 -11 -9 0 0.04 0.20 11 -9 0 -0.04 0.18 11 9 0 0.24 0.18 11 9 0 0.22 0.19 -11 9 0 0.21 0.19 12 -9 0 20.23 1.21 -12 -9 0 19.73 1.20 12 9 0 21.35 1.14 -12 9 0 19.97 1.12 12 9 0 22.37 1.15 -13 -9 0 0.11 0.23 13 -9 0 0.07 0.20 13 9 0 -0.02 0.15 13 9 0 -0.16 0.16 -13 9 0 0.27 0.23 -14 -9 0 9.59 0.86 14 -9 0 12.00 0.94 14 9 0 11.08 0.80 -14 9 0 12.02 0.85 -15 -9 0 3.65 0.59 15 -9 0 4.04 0.62 15 9 0 3.91 0.52 -15 9 0 3.62 0.52 0 -10 0 64.58 2.43 0 -10 0 64.53 2.38 0 -10 0 66.25 2.23 0 10 0 64.42 2.32 1 -10 0 133.70 4.34 -1 -10 0 130.62 4.54 -1 -10 0 137.25 4.38 1 -10 0 134.72 4.61 1 -10 0 128.94 4.55 -1 -10 0 129.42 4.62 1 10 0 133.77 4.44 -1 10 0 128.63 4.49 1 10 0 135.96 4.51 -2 -10 0 35.15 1.29 2 -10 0 35.80 1.44 2 -10 0 34.36 1.40 -2 -10 0 32.36 1.44 -2 10 0 34.02 1.39 2 10 0 32.85 1.33 2 10 0 34.77 1.30 3 -10 0 27.39 1.16 -3 -10 0 27.00 1.05 3 -10 0 24.28 1.12 -3 -10 0 24.82 1.18 3 10 0 26.13 1.08 -3 10 0 25.73 1.15 4 -10 0 15.65 0.79 -4 -10 0 15.50 0.73 4 -10 0 15.15 0.80 -4 -10 0 15.05 0.84 -4 10 0 15.43 0.82 4 10 0 15.29 0.74 5 -10 0 74.54 2.89 -5 -10 0 81.74 2.97 5 -10 0 83.39 2.89 -5 -10 0 76.17 2.78 5 10 0 78.17 2.82 -5 10 0 81.00 2.92 6 -10 0 2.03 0.32 -6 -10 0 2.15 0.31 -6 -10 0 2.06 0.29 6 10 0 1.50 0.24 -6 10 0 2.51 0.32 -7 -10 0 0.00 0.12 7 -10 0 0.08 0.13 -7 -10 0 0.09 0.13 7 10 0 0.17 0.12 -7 10 0 0.57 0.21 -8 -10 0 7.83 0.60 8 -10 0 7.16 0.58 -8 -10 0 6.92 0.54 -8 10 0 6.19 0.56 8 10 0 6.55 0.50 -9 -10 0 108.29 3.93 -9 -10 0 110.28 4.00 9 -10 0 107.08 4.00 -9 10 0 110.82 3.96 9 10 0 105.96 3.87 -10 -10 0 10.86 0.78 -10 -10 0 10.84 0.78 10 -10 0 11.80 0.83 10 10 0 11.27 0.73 -10 10 0 11.29 0.79 11 -10 0 5.25 0.60 -11 -10 0 5.54 0.58 11 10 0 5.83 0.55 -11 10 0 4.98 0.55 11 10 0 5.31 0.56 12 -10 0 13.29 0.96 -12 -10 0 11.69 0.90 12 10 0 13.25 0.87 -12 10 0 14.47 0.92 12 10 0 13.23 0.88 13 -10 0 31.77 1.67 -13 -10 0 28.53 1.58 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0.26 -8 11 0 0.57 0.25 8 11 0 0.80 0.22 9 -11 0 0.32 0.22 -9 -11 0 0.46 0.25 -9 -11 0 0.05 0.17 9 11 0 -0.08 0.13 -9 11 0 -0.11 0.19 10 -11 0 0.72 0.26 -10 -11 0 0.18 0.19 -10 -11 0 0.68 0.25 10 11 0 0.80 0.24 -10 11 0 0.09 0.20 -11 -11 0 2.13 0.42 11 -11 0 2.64 0.47 11 11 0 2.40 0.42 -11 11 0 2.59 0.41 11 11 0 2.26 0.40 -12 -11 0 -0.16 0.19 12 -11 0 0.31 0.26 12 11 0 -0.18 0.19 -12 11 0 0.24 0.23 13 -11 0 7.55 0.78 -13 -11 0 7.67 0.77 13 11 0 9.11 0.76 -13 11 0 7.41 0.72 0 -12 0 101.00 3.57 0 -12 0 97.96 3.65 0 12 0 99.44 3.47 1 -12 0 21.70 1.10 -1 -12 0 22.31 1.12 1 -12 0 21.09 1.04 -1 12 0 21.10 1.01 1 12 0 23.20 1.01 2 -12 0 5.76 0.47 2 -12 0 6.08 0.51 -2 -12 0 5.36 0.50 -2 12 0 5.56 0.46 2 12 0 6.25 0.45 3 -12 0 10.29 0.66 -3 -12 0 10.32 0.56 3 -12 0 10.97 0.69 -3 -12 0 9.46 0.68 -3 12 0 9.19 0.63 3 12 0 9.90 0.59 -4 -12 0 0.26 0.19 -4 -12 0 0.08 0.11 4 -12 0 0.04 0.15 4 -12 0 0.25 0.17 -4 12 0 0.11 0.16 4 12 0 0.26 0.13 -5 -12 0 12.46 0.82 -5 -12 0 13.49 0.71 5 -12 0 12.34 0.77 5 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