#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100769.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_1100769 _chemical_formula_sum 'C18 H20 B Cl N6 S2 Zn' _chemical_formula_weight 496.15 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.688(4) _cell_length_b 8.5506(17) _cell_length_c 25.364(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.111(4) _cell_angle_gamma 90.00 _cell_volume 4417.2(15) _cell_formula_units_Z 8 _cell_measurement_temperature 245(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description isometric _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.439 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 245(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 11586 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 30.03 _reflns_number_total 5801 _reflns_number_gt 3669 _reflns_threshold_expression >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^)+(0.0356P)^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 5801 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _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 Zn1 Zn -0.312081(11) 0.82127(3) 0.605150(10) 0.03669(8) Uani 1 1 d . . . S1 S -0.41926(3) 0.85446(7) 0.56216(2) 0.04478(15) Uani 1 1 d . . . S2 S -0.23248(3) 0.93409(7) 0.56894(3) 0.04773(16) Uani 1 1 d . . . N1 N -0.45327(8) 0.66344(19) 0.64285(7) 0.0387(4) Uani 1 1 d . . . N2 N -0.53312(8) 0.7313(2) 0.57848(8) 0.0408(4) Uani 1 1 d . . . N3 N -0.35284(9) 0.7692(2) 0.70787(7) 0.0434(4) Uani 1 1 d . . . N4 N -0.31599(9) 0.8669(2) 0.68287(7) 0.0422(4) Uani 1 1 d . . . N5 N -0.34168(8) 0.5263(2) 0.65271(7) 0.0410(4) Uani 1 1 d . . . N6 N -0.30641(8) 0.5883(2) 0.61752(7) 0.0411(4) Uani 1 1 d . . . Cl1 Cl 0.02182(3) 0.57644(9) 0.67846(3) 0.0730(2) Uani 1 1 d . . . B1 B -0.38759(13) 0.6230(3) 0.68154(11) 0.0432(6) Uani 1 1 d . . . HB1 H -0.4020(9) 0.545(2) 0.7115(7) 0.033(5) Uiso 1 1 d . . . C1 C -0.63845(11) 0.8274(3) 0.52846(13) 0.0692(8) Uani 1 1 d . . . H1A H -0.6394 0.9068 0.5556 0.104 Uiso 1 1 calc R . . H1B H -0.6611 0.7345 0.5376 0.104 Uiso 1 1 calc R . . H1C H -0.6601 0.8668 0.4940 0.104 Uiso 1 1 calc R . . C2 C -0.56231(14) 0.6653(3) 0.48335(11) 0.0693(8) Uani 1 1 d . . . H2A H -0.5163 0.6441 0.4829 0.104 Uiso 1 1 calc R . . H2B H -0.5831 0.7040 0.4485 0.104 Uiso 1 1 calc R . . H2C H -0.5839 0.5697 0.4914 0.104 Uiso 1 1 calc R . . C3 C -0.56793(11) 0.7868(3) 0.52564(10) 0.0482(6) Uani 1 1 d . . . H3A H -0.5459 0.8832 0.5164 0.058 Uiso 1 1 calc R . . C4 C -0.55999(12) 0.6414(3) 0.61370(11) 0.0531(6) Uani 1 1 d . . . H4A H -0.6045 0.6138 0.6108 0.064 Uiso 1 1 calc R . . C5 C -0.51131(12) 0.6000(3) 0.65292(10) 0.0514(6) Uani 1 1 d . . . H5A H -0.5158 0.5377 0.6826 0.062 Uiso 1 1 calc R . . C6 C -0.46792(10) 0.7446(2) 0.59636(9) 0.0352(5) Uani 1 1 d . . . C7 C -0.35341(12) 0.8245(3) 0.75772(9) 0.0563(7) Uani 1 1 d . . . H7A H -0.3754 0.7786 0.7832 0.068 Uiso 1 1 calc R . . C8 C -0.31664(13) 0.9585(3) 0.76485(10) 0.0603(7) Uani 1 1 d . . . H8A H -0.3084 1.0220 0.7955 0.072 Uiso 1 1 calc R . . C9 C -0.29454(11) 0.9798(3) 0.71770(10) 0.0505(6) Uani 1 1 d . . . H9A H -0.2677 1.0633 0.7108 0.061 Uiso 1 1 calc R . . C10 C -0.33272(12) 0.3699(3) 0.65387(10) 0.0534(6) Uani 1 1 d . . . H10A H -0.3519 0.2990 0.6749 0.064 Uiso 1 1 calc R . . C11 C -0.29131(13) 0.3314(3) 0.61952(11) 0.0580(7) Uani 1 1 d . . . H11A H -0.2761 0.2312 0.6125 0.070 Uiso 1 1 calc R . . C12 C -0.27671(11) 0.4707(3) 0.59741(10) 0.0495(6) Uani 1 1 d . . . H12A H -0.2495 0.4813 0.5716 0.059 Uiso 1 1 calc R . . C13 C -0.16298(10) 0.8272(2) 0.60128(9) 0.0386(5) Uani 1 1 d . . . C14 C -0.12153(11) 0.7594(3) 0.57040(10) 0.0484(6) Uani 1 1 d . . . H14A H -0.1322 0.7649 0.5329 0.058 Uiso 1 1 calc R . . C15 C -0.06459(12) 0.6834(3) 0.59401(10) 0.0538(6) Uani 1 1 d . . . H15A H -0.0364 0.6394 0.5727 0.065 Uiso 1 1 calc R . . C16 C -0.04973(11) 0.6731(3) 0.64848(10) 0.0464(6) Uani 1 1 d . . . C17 C -0.08980(11) 0.7388(3) 0.68031(10) 0.0481(6) Uani 1 1 d . . . H17A H -0.0790 0.7313 0.7178 0.058 Uiso 1 1 calc R . . C18 C -0.14619(10) 0.8162(3) 0.65648(9) 0.0452(5) Uani 1 1 d . . . H18A H -0.1735 0.8620 0.6781 0.054 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 Zn1 0.03079(14) 0.03922(14) 0.03981(15) 0.00173(11) 0.00550(11) 0.00045(11) S1 0.0292(3) 0.0619(4) 0.0430(3) 0.0169(3) 0.0056(3) -0.0002(3) S2 0.0371(3) 0.0486(3) 0.0580(4) 0.0157(3) 0.0098(3) 0.0007(3) N1 0.0343(10) 0.0410(10) 0.0414(11) 0.0068(8) 0.0085(9) -0.0013(8) N2 0.0305(9) 0.0403(10) 0.0499(12) 0.0059(9) 0.0024(9) -0.0034(8) N3 0.0406(11) 0.0554(11) 0.0335(10) 0.0002(9) 0.0039(9) 0.0076(9) N4 0.0434(11) 0.0425(10) 0.0392(11) -0.0034(9) 0.0033(9) 0.0004(8) N5 0.0398(10) 0.0380(10) 0.0430(11) 0.0058(8) 0.0015(9) 0.0036(8) N6 0.0375(10) 0.0417(10) 0.0440(11) 0.0017(8) 0.0069(9) 0.0068(8) Cl1 0.0514(4) 0.0855(5) 0.0771(5) -0.0089(4) -0.0026(4) 0.0269(4) B1 0.0413(15) 0.0487(15) 0.0387(15) 0.0116(12) 0.0042(13) 0.0019(12) C1 0.0337(13) 0.0652(17) 0.104(2) 0.0187(16) -0.0018(15) 0.0043(12) C2 0.0612(18) 0.0773(19) 0.0603(18) -0.0026(15) -0.0146(15) 0.0015(15) C3 0.0321(12) 0.0467(13) 0.0610(16) 0.0145(12) -0.0047(11) -0.0010(10) C4 0.0366(13) 0.0519(14) 0.0709(18) 0.0116(13) 0.0101(13) -0.0114(11) C5 0.0441(14) 0.0530(14) 0.0591(16) 0.0168(12) 0.0142(13) -0.0068(11) C6 0.0306(11) 0.0350(11) 0.0393(12) 0.0014(9) 0.0046(10) 0.0001(9) C7 0.0534(15) 0.0819(19) 0.0327(13) -0.0004(13) 0.0053(12) 0.0174(14) C8 0.0608(17) 0.0714(18) 0.0429(15) -0.0178(13) -0.0067(13) 0.0197(14) C9 0.0445(14) 0.0488(13) 0.0520(16) -0.0097(12) -0.0087(12) 0.0090(11) C10 0.0540(15) 0.0380(13) 0.0616(17) 0.0103(11) -0.0079(14) 0.0003(11) C11 0.0603(16) 0.0408(14) 0.0658(17) -0.0068(12) -0.0081(14) 0.0141(12) C12 0.0420(13) 0.0535(14) 0.0509(15) -0.0108(12) 0.0022(12) 0.0109(11) C13 0.0312(11) 0.0378(11) 0.0472(13) 0.0029(10) 0.0079(10) -0.0070(9) C14 0.0475(14) 0.0549(14) 0.0415(14) -0.0056(11) 0.0047(12) 0.0030(12) C15 0.0470(14) 0.0597(15) 0.0565(16) -0.0112(13) 0.0135(13) 0.0087(12) C16 0.0351(12) 0.0456(13) 0.0572(16) -0.0040(11) 0.0047(12) 0.0040(10) C17 0.0417(13) 0.0581(14) 0.0446(14) 0.0060(11) 0.0082(12) 0.0020(11) C18 0.0363(12) 0.0539(13) 0.0497(14) 0.0035(12) 0.0194(11) 0.0038(11)