#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100726.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100726 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M P2(1)/c loop_ _publ_author_name 'Tara J. Burchell and Richard J. Puddephatt' _publ_section_title ; Self-Assembly of Chiral Coordination Polymers and Macrocycles: A Metal Template Effect on the Polymer-Macrocycle Equilibrium ; _chemical_formula_sum 'C33 H24 Cl4 Hg N4 O2' _chemical_formula_weight 850.95 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' '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 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 17.124(3) _cell_length_b 11.727(2) _cell_length_c 16.249(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.84(3) _cell_angle_gamma 90.00 _cell_volume 3168.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7532 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.4 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 5.233 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3545 _exptl_absorpt_correction_T_max 0.7799 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _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 'Nonius Kappa CCD' _diffrn_measurement_method 'phi\omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36528 _diffrn_reflns_av_R_equivalents 0.113 _diffrn_reflns_av_sigmaI/netI 0.1045 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5589 _reflns_number_gt 3502 _reflns_threshold_expression I>2sigma(I) _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^)+(0.0468P)^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 0.00066(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5589 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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 0.340571(17) 0.70129(3) 0.025233(18) 0.03244(13) Uani 1 1 d . . . Cl1 Cl 0.26623(11) 0.60244(19) -0.09621(11) 0.0399(5) Uani 1 1 d . . . Cl2 Cl 0.36134(14) 0.7404(2) 0.16986(12) 0.0517(6) Uani 1 1 d . . . N1 N 0.3128(3) 0.8827(5) -0.0431(3) 0.0270(15) Uani 1 1 d . . . N2 N 0.2428(3) 1.2150(5) -0.2402(3) 0.0249(15) Uani 1 1 d . . . H2A H 0.2666 1.1590 -0.2608 0.030 Uiso 1 1 calc R . . N3 N 0.2439(3) 1.1232(5) -0.4569(3) 0.0250(15) Uani 1 1 d . . . H3A H 0.2400 1.1545 -0.5069 0.030 Uiso 1 1 calc R . . N4 N 0.5327(3) 1.1690(5) -0.4896(4) 0.0326(17) Uani 1 1 d . . . O1 O 0.2101(3) 1.2822(4) -0.1215(3) 0.0310(13) Uani 1 1 d . . . O2 O 0.3257(3) 1.0731(5) -0.3307(3) 0.0350(14) Uani 1 1 d . . . C1 C 0.3179(4) 0.9799(8) 0.0013(4) 0.032(2) Uani 1 1 d . . . H1A H 0.3406 0.9765 0.0606 0.038 Uiso 1 1 calc R . . C2 C 0.2925(4) 1.0844(6) -0.0337(4) 0.0232(17) Uani 1 1 d . . . H2B H 0.2958 1.1504 0.0009 0.028 Uiso 1 1 calc R . . C3 C 0.2620(4) 1.0911(7) -0.1200(4) 0.0239(18) Uani 1 1 d . . . C4 C 0.2557(4) 0.9926(7) -0.1663(4) 0.0281(19) Uani 1 1 d . . . H4A H 0.2334 0.9944 -0.2257 0.034 Uiso 1 1 calc R . . C5 C 0.2816(4) 0.8907(7) -0.1267(4) 0.034(2) Uani 1 1 d . . . H5A H 0.2772 0.8235 -0.1601 0.040 Uiso 1 1 calc R . . C6 C 0.2354(4) 1.2047(7) -0.1591(4) 0.0251(17) Uani 1 1 d . . . C7 C 0.2151(4) 1.3088(7) -0.2942(4) 0.0253(17) Uani 1 1 d . . . C8 C 0.2433(4) 1.4198(7) -0.2694(4) 0.0255(18) Uani 1 1 d . . . H8A H 0.2793 1.4324 -0.2158 0.031 Uiso 1 1 calc R . . C9 C 0.2182(4) 1.5082(7) -0.3234(5) 0.037(2) Uani 1 1 d . . . H9A H 0.2358 1.5832 -0.3063 0.044 Uiso 1 1 calc R . . C10 C 0.1659(4) 1.4908(7) -0.4051(5) 0.031(2) Uani 1 1 d . . . C11 C 0.1417(5) 1.5819(8) -0.4640(5) 0.045(2) Uani 1 1 d . . . H11A H 0.1584 1.6576 -0.4479 0.053 Uiso 1 1 calc R . . C12 C 0.0949(5) 1.5614(9) -0.5424(5) 0.048(3) Uani 1 1 d . . . H12A H 0.0797 1.6226 -0.5813 0.057 Uiso 1 1 calc R . . C13 C 0.0694(5) 1.4524(9) -0.5661(5) 0.044(2) Uani 1 1 d . . . H13A H 0.0365 1.4397 -0.6213 0.053 Uiso 1 1 calc R . . C14 C 0.0901(4) 1.3624(8) -0.5125(4) 0.037(2) Uani 1 1 d . . . H14A H 0.0713 1.2882 -0.5306 0.045 Uiso 1 1 calc R . . C15 C 0.1398(4) 1.3786(8) -0.4292(4) 0.0300(19) Uani 1 1 d . . . C16 C 0.1648(4) 1.2855(7) -0.3713(4) 0.0242(18) Uani 1 1 d . . . C17 C 0.1343(4) 1.1681(7) -0.3906(4) 0.0276(19) Uani 1 1 d . . . C18 C 0.0661(4) 1.1305(7) -0.3607(4) 0.029(2) Uani 1 1 d . . . C19 C 0.0241(4) 1.2035(8) -0.3178(5) 0.039(2) Uani 1 1 d . . . H19A H 0.0404 1.2808 -0.3085 0.047 Uiso 1 1 calc R . . C20 C -0.0396(5) 1.1642(9) -0.2894(5) 0.051(3) Uani 1 1 d . . . H20A H -0.0671 1.2145 -0.2602 0.062 Uiso 1 1 calc R . . C21 C -0.0655(5) 1.0505(9) -0.3026(5) 0.051(3) Uani 1 1 d . . . H21A H -0.1105 1.0248 -0.2830 0.061 Uiso 1 1 calc R . . C22 C -0.0263(4) 0.9773(9) -0.3435(5) 0.050(3) Uani 1 1 d . . . H22A H -0.0439 0.9004 -0.3516 0.059 Uiso 1 1 calc R . . C23 C 0.0409(4) 1.0138(8) -0.3744(4) 0.035(2) Uani 1 1 d . . . C24 C 0.0804(4) 0.9389(8) -0.4186(4) 0.041(2) Uani 1 1 d . . . H24A H 0.0622 0.8627 -0.4296 0.049 Uiso 1 1 calc R . . C25 C 0.1448(4) 0.9774(7) -0.4454(4) 0.035(2) Uani 1 1 d . . . H25A H 0.1722 0.9262 -0.4741 0.042 Uiso 1 1 calc R . . C26 C 0.1725(4) 1.0901(7) -0.4321(4) 0.0273(19) Uani 1 1 d . . . C27 C 0.3170(4) 1.1072(7) -0.4047(4) 0.0268(18) Uani 1 1 d . . . C28 C 0.3905(4) 1.1306(7) -0.4382(4) 0.0283(19) Uani 1 1 d . . . C29 C 0.4624(4) 1.1454(7) -0.3788(4) 0.034(2) Uani 1 1 d . . . H29A H 0.4641 1.1434 -0.3199 0.041 Uiso 1 1 calc R . . C30 C 0.5320(4) 1.1634(7) -0.4065(5) 0.041(2) Uani 1 1 d . . . H30A H 0.5814 1.1722 -0.3653 0.050 Uiso 1 1 calc R . . C31 C 0.4622(4) 1.1528(7) -0.5453(5) 0.033(2) Uani 1 1 d . . . H31A H 0.4612 1.1555 -0.6040 0.040 Uiso 1 1 calc R . . C32 C 0.3916(4) 1.1325(7) -0.5229(4) 0.0297(19) Uani 1 1 d . . . H32A H 0.3435 1.1197 -0.5653 0.036 Uiso 1 1 calc R . . C40 C 0.4682(5) 1.5466(8) -0.6866(5) 0.052(3) Uani 1 1 d . . . H40A H 0.4521 1.6141 -0.6581 0.062 Uiso 1 1 calc R . . H40B H 0.4263 1.5333 -0.7394 0.062 Uiso 1 1 calc R . . Cl3 Cl 0.55969(12) 1.5756(2) -0.71279(13) 0.0550(7) Uani 1 1 d . . . Cl4 Cl 0.47290(14) 1.4286(3) -0.62088(17) 0.0865(10) 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 0.03329(19) 0.0314(2) 0.03407(19) 0.00340(17) 0.01083(13) 0.00414(17) Cl1 0.0438(12) 0.0320(14) 0.0418(11) -0.0021(10) 0.0060(9) -0.0055(11) Cl2 0.0702(15) 0.0526(17) 0.0308(11) 0.0033(11) 0.0090(10) 0.0163(13) N1 0.033(3) 0.021(4) 0.026(3) 0.007(3) 0.005(3) 0.003(3) N2 0.034(3) 0.020(4) 0.025(3) 0.000(3) 0.014(3) 0.014(3) N3 0.022(3) 0.026(4) 0.029(3) 0.003(3) 0.011(3) 0.001(3) N4 0.022(3) 0.042(5) 0.035(4) -0.004(3) 0.009(3) 0.000(3) O1 0.045(3) 0.025(4) 0.024(3) -0.003(3) 0.010(2) 0.007(3) O2 0.035(3) 0.048(4) 0.024(3) 0.003(3) 0.011(2) 0.000(3) C1 0.030(4) 0.047(6) 0.023(4) -0.007(4) 0.012(3) -0.015(4) C2 0.033(4) 0.010(5) 0.029(4) -0.001(4) 0.011(3) -0.001(4) C3 0.016(4) 0.025(5) 0.032(4) -0.006(4) 0.008(3) -0.001(4) C4 0.029(4) 0.033(6) 0.022(4) 0.003(4) 0.006(3) -0.004(4) C5 0.043(5) 0.032(6) 0.026(4) 0.001(4) 0.007(4) 0.001(4) C6 0.024(4) 0.026(5) 0.024(4) -0.001(4) 0.003(3) -0.001(4) C7 0.032(4) 0.017(5) 0.029(4) 0.008(4) 0.011(3) 0.008(4) C8 0.031(4) 0.024(5) 0.025(4) 0.000(4) 0.014(3) 0.005(4) C9 0.045(5) 0.029(6) 0.044(5) -0.003(4) 0.025(4) -0.003(4) C10 0.029(4) 0.031(6) 0.040(5) 0.011(4) 0.023(4) 0.010(4) C11 0.043(5) 0.033(6) 0.066(6) 0.021(5) 0.030(5) 0.017(5) C12 0.042(5) 0.058(8) 0.044(5) 0.031(5) 0.013(4) 0.018(5) C13 0.033(5) 0.062(8) 0.035(5) 0.013(5) 0.003(4) 0.007(5) C14 0.029(4) 0.049(6) 0.034(5) 0.010(4) 0.010(4) 0.009(4) C15 0.031(4) 0.035(6) 0.030(4) 0.008(4) 0.018(3) 0.007(4) C16 0.021(4) 0.027(5) 0.026(4) 0.005(4) 0.011(3) 0.000(4) C17 0.022(4) 0.036(6) 0.026(4) 0.000(4) 0.007(3) -0.004(4) C18 0.022(4) 0.040(6) 0.023(4) 0.014(4) 0.003(3) 0.004(4) C19 0.029(4) 0.048(6) 0.041(5) 0.013(5) 0.011(4) 0.004(5) C20 0.041(5) 0.069(8) 0.052(6) 0.012(5) 0.025(4) 0.013(5) C21 0.028(5) 0.074(9) 0.053(6) 0.023(6) 0.018(4) -0.008(5) C22 0.028(5) 0.078(8) 0.041(5) 0.016(5) 0.005(4) -0.009(5) C23 0.023(4) 0.053(7) 0.027(4) 0.011(4) 0.004(3) -0.014(4) C24 0.036(5) 0.050(7) 0.040(5) 0.001(4) 0.016(4) -0.012(4) C25 0.039(5) 0.034(6) 0.031(4) -0.003(4) 0.006(4) -0.003(4) C26 0.021(4) 0.038(6) 0.023(4) -0.002(4) 0.007(3) 0.000(4) C27 0.025(4) 0.030(5) 0.027(4) -0.007(4) 0.012(3) 0.001(4) C28 0.033(4) 0.031(5) 0.026(4) -0.002(4) 0.017(3) -0.003(4) C29 0.041(5) 0.041(6) 0.024(4) -0.004(4) 0.016(4) -0.009(4) C30 0.028(4) 0.065(7) 0.032(5) -0.006(4) 0.009(3) 0.000(4) C31 0.035(5) 0.037(6) 0.033(4) 0.003(4) 0.020(4) 0.002(4) C32 0.030(4) 0.032(6) 0.027(4) -0.004(4) 0.007(3) 0.000(4) C40 0.044(5) 0.053(7) 0.061(6) 0.006(5) 0.016(4) -0.013(5) Cl3 0.0439(12) 0.069(2) 0.0516(13) 0.0126(13) 0.0111(10) -0.0015(13) Cl4 0.0490(15) 0.121(3) 0.0928(19) 0.0526(19) 0.0232(14) 0.0088(16)