#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/5/5000324.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_5000324 ## 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C46 H80 B K N4 O4' _[local]_cod_chemical_formula_sum_orig 'C46 H80 B1 K1 N4 O4' _chemical_formula_moiety ? _chemical_formula_weight 803.075 _cell_length_a 19.4597(19) _cell_length_b 21.273(2) _cell_length_c 10.8452(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4489.6(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 176 _cell_measurement_theta_min 9.61 _cell_measurement_theta_max 12.27 _cell_measurement_temperature 107. _exptl_crystal_colour colorless _exptl_crystal_description 'partially redisolved' _exptl_crystal_size_max '.30 .30 .35' _exptl_crystal_size_mid .30 _exptl_crystal_size_min .30 _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.1644 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z 1/2-x,-y,1/2+z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature -166. _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_reflns_number 8532 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_theta_min 3.05734 _diffrn_reflns_theta_max 24.9894 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 4 _diffrn_standards_decay_% 1.4 _diffrn_standards_interval_count 400 _reflns_number_total 7876 _reflns_number_gt 5181 _reflns_threshold_expression F^2^>2.33\s(F^2^) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source K K 0.179 0.25 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' B B 0 0.001 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 5894 _refine_ls_number_parameters 506 _refine_ls_hydrogen_treatment 'fixed, idealized' _refine_ls_extinction_coef 0.00000060(7) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details ; absolute structure based on refinement using both possibilites ; _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.03F)^2^ _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.0484 _refine_ls_goodness_of_fit_ref 1.4135 _refine_ls_shift/su_max 0.0215 _refine_diff_density_max 0.39 _refine_diff_density_min -0.34 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_disorder_group _atom_site_disorder_assembly K1 K 0.99402(6) 0.57352(5) 0.01939(9) 0.0199(3) Uani 1 0 . B2 B 1.0680(3) 0.6405(3) 0.3081(5) 0.0183(18) Uani 1 0 . C3 C 1.1013(2) 0.6749(2) 0.4284(4) 0.0178(16) Uani 1 0 . C4 C 1.1768(3) 0.6562(2) 0.4438(4) 0.0221(18) Uani 1 0 . C5 C 1.2223(3) 0.6657(2) 0.3305(5) 0.0241(17) Uani 1 0 . C6 C 1.1885(3) 0.6422(2) 0.2114(5) 0.0236(17) Uani 1 0 . C7 C 1.1135(2) 0.6637(2) 0.1947(4) 0.0166(15) Uani 1 0 . C8 C 1.1059(2) 0.7352(2) 0.1796(5) 0.0207(16) Uani 1 0 . C9 C 1.1197(3) 0.7739(2) 0.2948(5) 0.0270(18) Uani 1 0 . C10 C 1.0918(3) 0.7469(2) 0.4126(4) 0.0227(18) Uani 1 0 . N11 N 1.06947(18) 0.56650(17) 0.3240(3) 0.0146(12) Uani 1 0 . C12 C 1.0708(2) 0.5330(2) 0.4294(4) 0.0193(16) Uani 1 0 . C13 C 1.0637(2) 0.4695(2) 0.3999(4) 0.0180(16) Uani 1 0 . C14 C 1.0599(2) 0.4122(2) 0.4811(4) 0.0218(16) Uani 1 0 . C15 C 1.0243(3) 0.3602(2) 0.4063(5) 0.0242(18) Uani 1 0 . C16 C 1.0553(3) 0.3531(2) 0.2772(5) 0.0231(17) Uani 1 0 . C17 C 1.0438(2) 0.4118(2) 0.1947(5) 0.0219(16) Uani 1 0 . C18 C 1.0578(2) 0.4697(2) 0.2744(4) 0.0172(15) Uani 1 0 . C19 C 1.1294(3) 0.3906(2) 0.5287(5) 0.0294(18) Uani 1 0 . C20 C 1.0837(3) 0.4106(2) 0.0751(4) 0.0233(17) Uani 1 0 . C21 C 0.0598(3) 0.3571(2) 0.9901(5) 0.0328(19) Uani 1 0 . C22 C 1.1609(3) 0.4079(3) 0.0952(5) 0.036(2) Uani 1 0 . N23 N 0.98903(19) 0.65863(16) 0.2947(3) 0.0144(12) Uani 1 0 . C24 C 0.9437(3) 0.6683(2) 0.3853(4) 0.0200(16) Uani 1 0 . C25 C 0.8818(2) 0.6884(2) 0.3378(4) 0.0159(15) Uani 1 0 . C26 C 0.8156(3) 0.7061(2) 0.3959(4) 0.0234(18) Uani 1 0 . C27 C 0.7600(3) 0.7058(3) 0.2970(5) 0.039(2) Uani 1 0 . C28 C 0.7792(3) 0.7384(3) 0.1808(5) 0.036(2) Uani 1 0 . C29 C 0.8447(3) 0.7150(2) 0.1156(5) 0.0220(17) Uani 1 0 . C30 C 0.8940(2) 0.6897(2) 0.2108(4) 0.0149(15) Uani 1 0 . N31 N 0.95853(18) 0.67170(16) 0.1838(3) 0.0136(12) Uani 1 0 . C32 C 0.7960(3) 0.6651(3) 0.5038(6) 0.045(2) Uani 1 0 . C33 C 0.8333(2) 0.6709(2) 0.0048(5) 0.0248(17) Uani 1 0 . C34 C 0.8001(3) 0.7061(3) 0.8956(5) 0.0312(19) Uani 1 0 . C35 C 0.7889(3) 0.6140(3) 0.0363(6) 0.052(3) Uani 1 0 . N36 N 1.0611(2) 0.52772(18) 0.2246(3) 0.0158(13) Uani 1 0 . O37 O 1.0237(2) 0.67160(19) -0.1662(4) 0.0543(17) Uani 1 0 . C38 C 0.0920(3) 0.7008(3) 0.8288(6) 0.051(3) Uani 1 0 . C39 C 0.9759(4) 0.7214(4) -0.1894(11) 0.113(5) Uani 1 0 . C40 C 0.0123(4) 0.7771(3) 0.7711(6) 0.064(3) Uani 1 0 . C41 C 0.0809(3) 0.7704(3) 0.8309(6) 0.046(2) Uani 1 0 . O42 O 0.9324(2) 0.51534(18) 0.8251(3) 0.0497(16) Uani 1 0 . C43 C 0.9129(3) 0.5553(3) -0.2775(6) 0.051(3) Uani 1 0 . C44 C 0.9013(3) 0.5138(3) 0.6163(5) 0.048(2) Uani 1 0 . C45 C 0.8880(3) 0.4507(3) -0.3270(6) 0.047(2) Uani 1 0 . C46 C 0.9315(4) 0.4523(3) 0.7845(5) 0.049(2) Uani 1 0 . O47 O 0.1125(2) 0.54878(18) 0.8936(3) 0.0393(15) Uani 1 0 . C48 C 1.1141(3) 0.5359(3) -0.2348(5) 0.050(2) Uani 1 0 . C49 C 0.1874(3) 0.5413(3) 0.7254(5) 0.046(2) Uani 1 0 . C50 C 1.2253(3) 0.5215(3) -0.1604(6) 0.045(2) Uani 1 0 . C51 C 0.1821(3) 0.5525(3) 0.9366(5) 0.041(2) Uani 1 0 . O52 O 0.89580(17) 0.49861(17) 0.1397(3) 0.0272(12) Uani 1 0 . C53 C 0.8462(3) 0.4530(3) 0.1018(5) 0.031(2) Uani 1 0 . C54 C 0.7978(3) 0.4457(3) 0.2075(6) 0.048(2) Uani 1 0 . C55 C 0.8242(4) 0.4819(5) 0.3062(7) 0.116(4) Uani 1 0 . C56 C 0.8878(3) 0.5107(3) 0.2680(4) 0.0285(18) Uani 1 0 . H1 H 1.0766 0.6616 0.5005 0.0315 Uiso 1 0 . H2 H 1.1955 0.6808 0.5085 0.0353 Uiso 1 0 . H3 H 1.1784 0.6131 0.4647 0.0353 Uiso 1 0 . H4 H 1.2314 0.7094 0.3227 0.0363 Uiso 1 0 . H5 H 1.2635 0.6435 0.3431 0.0363 Uiso 1 0 . H6 H 1.2142 0.6577 0.1432 0.0372 Uiso 1 0 . H7 H 1.189 0.5977 0.2108 0.0372 Uiso 1 0 . H8 H 1.0962 0.6443 0.1218 0.0293 Uiso 1 0 . H9 H 1.1374 0.7483 0.1167 0.0327 Uiso 1 0 . H10 H 1.0604 0.7435 0.1527 0.0327 Uiso 1 0 . H11 H 1.1683 0.7785 0.3028 0.0403 Uiso 1 0 . H12 H 1.0998 0.8144 0.2826 0.0403 Uiso 1 0 . H13 H 1.0443 0.756 0.4167 0.0352 Uiso 1 0 . H14 H 1.1149 0.767 0.4797 0.0352 Uiso 1 0 . H15 H 1.0761 0.5496 0.5099 0.0322 Uiso 1 0 . H16 H 1.032 0.4218 0.5507 0.0337 Uiso 1 0 . H17 H 1.0282 0.3219 0.4484 0.0376 Uiso 1 0 . H18 H 0.9769 0.3713 0.3973 0.0376 Uiso 1 0 . H19 H 1.103 0.346 0.2856 0.0345 Uiso 1 0 . H20 H 1.0342 0.318 0.2385 0.0345 Uiso 1 0 . H21 H 0.9964 0.413 0.1744 0.0342 Uiso 1 0 . H22 H 1.1241 0.3558 0.5816 0.0424 Uiso 1 0 . H23 H 1.1573 0.378 0.459 0.0424 Uiso 1 0 . H24 H 1.1518 0.4239 0.5698 0.0424 Uiso 1 0 . H25 H 1.074 0.4489 0.034 0.0358 Uiso 1 0 . H26 H 1.0116 0.3602 -0.0228 0.0436 Uiso 1 0 . H27 H 1.0829 0.3601 -0.0866 0.0436 Uiso 1 0 . H28 H 1.0701 0.3177 0.0273 0.0436 Uiso 1 0 . H29 H 1.1727 0.3676 0.1258 0.0477 Uiso 1 0 . H30 H 1.1829 0.4141 0.0172 0.0477 Uiso 1 0 . H31 H 1.1741 0.4394 0.1504 0.0477 Uiso 1 0 . H32 H 0.9529 0.6625 0.4701 0.033 Uiso 1 0 . H33 H 0.8197 0.7478 0.4239 0.0388 Uiso 1 0 . H34 H 0.7499 0.6629 0.2786 0.0513 Uiso 1 0 . H35 H 0.7206 0.7251 0.3314 0.0513 Uiso 1 0 . H36 H 0.7421 0.7344 0.1244 0.0482 Uiso 1 0 . H37 H 0.7857 0.7821 0.1992 0.0482 Uiso 1 0 . H38 H 0.8665 0.7514 0.0832 0.0356 Uiso 1 0 . H39 H 0.7542 0.6784 0.5387 0.0586 Uiso 1 0 . H40 H 0.7929 0.6223 0.4792 0.0586 Uiso 1 0 . H41 H 0.8316 0.6681 0.5661 0.0586 Uiso 1 0 . H42 H 0.8763 0.656 0.979 0.0369 Uiso 1 0 . H43 H 0.8302 0.7388 -0.1301 0.0424 Uiso 1 0 . H44 H 0.7941 0.6772 -0.171 0.0424 Uiso 1 0 . H45 H 0.7574 0.7228 -0.0809 0.0424 Uiso 1 0 . H46 H 0.7428 0.6268 0.0522 0.0619 Uiso 1 0 . H47 H 0.7895 0.5849 0.9704 0.0619 Uiso 1 0 . H48 H 0.8068 0.5942 0.1089 0.0619 Uiso 1 0 . H49 H 1.1187 0.688 -0.1008 0.0601 Uiso 1 0 . H50 H 1.116 0.6886 -0.2438 0.0601 Uiso 1 0 . H51 H 0.9415 0.7089 0.7538 0.112 Uiso 1 0 . H52 H 0.9515 0.7307 -0.1109 0.112 Uiso 1 0 . H53 H 1.0162 0.7785 -0.3178 0.0733 Uiso 1 0 . H54 H 0.9897 0.816 -0.2047 0.0733 Uiso 1 0 . H55 H 0.0802 0.7865 0.9132 0.0571 Uiso 1 0 . H56 H 0.1161 0.7922 0.786 0.0571 Uiso 1 0 . H57 H 0.8728 0.5788 0.7422 0.0614 Uiso 1 0 . H58 H 0.9494 0.5844 -0.2955 0.0614 Uiso 1 0 . H59 H 0.8621 0.5274 -0.4288 0.0618 Uiso 1 0 . H60 H 0.94 0.5123 -0.4351 0.0618 Uiso 1 0 . H61 H 0.8406 0.446 -0.306 0.0629 Uiso 1 0 . H62 H 0.9012 0.418 -0.381 0.0629 Uiso 1 0 . H63 H 0.9766 0.438 0.7664 0.061 Uiso 1 0 . H64 H 0.9123 0.4258 -0.1525 0.061 Uiso 1 0 . H65 H 1.0959 0.4961 -0.2523 0.0626 Uiso 1 0 . H66 H 1.0863 0.5674 -0.2773 0.0626 Uiso 1 0 . H67 H 1.197 0.5141 -0.3434 0.0582 Uiso 1 0 . H68 H 1.1994 0.5834 -0.2991 0.0582 Uiso 1 0 . H69 H 1.2265 0.4766 -0.15 0.0559 Uiso 1 0 . H70 H 1.272 0.5363 -0.1578 0.0559 Uiso 1 0 . H71 H 1.195 0.5954 -0.0517 0.0515 Uiso 1 0 . H72 H 1.1861 0.5314 0.0151 0.0515 Uiso 1 0 . H73 H 0.8211 0.4683 0.0332 0.0452 Uiso 1 0 . H74 H 0.8674 0.4146 0.083 0.0452 Uiso 1 0 . H75 H 0.7548 0.4625 0.19 0.0651 Uiso 1 0 . H76 H 0.7929 0.4011 0.2256 0.0651 Uiso 1 0 . H77 H 0.7964 0.5033 0.3446 0.1685 Uiso 1 0 . H78 H 0.8429 0.4453 0.3679 0.1685 Uiso 1 0 . H79 H 0.9274 0.4976 0.3118 0.0412 Uiso 1 0 . H80 H 0.8803 0.5543 0.2811 0.0412 Uiso 1 0 . _cod_database_code 5000324