#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003517.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_2003517 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 1146 _journal_page_last 1148 _publ_section_title ; Two Isomers of 5,7,12,14-Tetramethyl-1,4,8,11-tetraazacyclotetradecane ; _chemical_formula_moiety 'C14 H32 N4,2H2 O1' _chemical_formula_sum 'C14 H36 N4 O2' _chemical_formula_weight 292.46 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 8.6917(7) _cell_length_b 11.576(1) _cell_length_c 15.006(3) _cell_angle_alpha 110.10(2) _cell_angle_beta 103.80(1) _cell_angle_gamma 91.465(9) _cell_volume 1367.3(3) _cell_formula_units_Z 3 _exptl_crystal_density_diffrn 1.066 _exptl_crystal_density_meas ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.42 _cell_measurement_theta_max 15.04 _exptl_absorpt_coefficient_mu 0.07 _cell_measurement_temperature 298(3) _exptl_crystal_description 'cuboid' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.42 _exptl_crystal_size_rad ? _exptl_crystal_colour 'transparent, colorless' _chemical_compound_source ? _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\q/2\q' _exptl_absorpt_correction_type 'empirical (North, Phillips & Matthews, 1968)' _exptl_absorpt_correction_T_min 0.8178 _exptl_absorpt_correction_T_max 0.9989 _diffrn_reflns_number 3860 _reflns_number_total 3572 _reflns_number_observed 2688 _reflns_observed_criterion I>=\s(I) _diffrn_reflns_av_R_equivalents 0.008 _diffrn_reflns_theta_max 22.5 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 14 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.051 _refine_ls_wR_factor_obs 0.068 _refine_ls_goodness_of_fit_obs 1.21 _refine_ls_number_reflns 2688 _refine_ls_number_parameters 488 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme 'w = 1/[\s(F~o~)^2^ + 0.002F~o~^2^]' _refine_ls_shift/esd_max 0.251 _refine_diff_density_max 0.28(4) _refine_diff_density_min -0.11(4) _refine_ls_extinction_method 'Zachariasen (1968)' _refine_ls_extinction_coef '1.2(2) (length in mm)' _atom_type_scat_source 'IntTabIV' loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv O(W1) 0.50 .4984(10) .4259(9) .2579(7) 7.6(5) O(W1') 0.50 .5805(9) .4121(9) .2732(7) 6.3(4) O(W2) 0.55 .8607(8) .4559(6) .2126(6) 6.7(3) O(W2') 0.30 .8470(14) .4617(10) .2746(9) 6.5(6) O(W2") 0.15 .942(3) .462(3) .254(4) 12.3(19) O(W3) 0.50 .3003(10) .5315(6) .2989(5) 8.7(4) O(W3') 0.50 .1933(7) .5335(6) .2900(5) 6.9(3) N(1) 1.00 .0222(3) .32458(20) .39019(16) 4.24(12) N(2) 1.00 -.3051(3) .24416(21) .37760(16) 4.34(12) N(3) 1.00 -.2010(3) .21660(21) .57267(16) 4.19(12) N(4) 1.00 .1296(3) .29992(21) .58722(16) 4.14(12) N(5) 1.00 .69413(25) .39217(19) .00204(16) 3.85(12) N(6) 1.00 .37921(24) .37867(19) .04593(16) 3.88(12) C(1) 1.00 .1244(5) .1981(5) .2512(3) 6.01(22) C(2) 1.00 .0159(3) .2005(3) .31749(20) 4.37(15) C(3) 1.00 -.1553(4) .1535(3) .25650(21) 4.56(16) C(4) 1.00 -.2752(4) .1274(3) .30843(20) 4.25(15) C(5) 1.00 -.4281(5) .0553(4) .2327(3) 6.29(21) C(6) 1.00 -.4112(4) .2322(4) .4369(3) 5.17(19) C(7) 1.00 -.3544(4) .1582(3) .50213(24) 5.09(18) C(8) 1.00 -.1245(4) .1403(3) .62663(22) 4.47(16) C(9) 1.00 -.2280(6) .1120(5) .6876(3) 6.67(25) C(10) 1.00 .0388(4) .2031(3) .69069(22) 4.84(18) C(11) 1.00 .1671(4) .2143(3) .63971(22) 4.54(15) C(12) 1.00 .3309(5) .2543(5) .7133(3) 6.86(24) C(13) 1.00 .2375(4) .3057(4) .52745(24) 4.85(18) C(14) 1.00 .1771(4) .3780(3) .46156(24) 4.98(17) C(15) 1.00 .8121(4) .1944(3) -.0294(3) 4.98(19) C(16) 1.00 .6606(3) .25633(23) -.03649(20) 3.62(13) C(18) 1.00 .3818(3) .24566(24) -.00300(21) 3.67(13) C(17) 1.00 .5537(3) .2153(3) .01620(22) 3.77(14) C(19) 1.00 .2791(4) .1679(4) .0291(3) 5.46(21) C(20) 1.00 .7785(3) .5795(3) -.0241(3) 4.60(17) C(21) 1.00 .7667(4) .4406(3) -.0583(3) 4.56(18) H(N1) 0.5 -.004 .382 .358 4.3(12) H(N1') 0.5 -.065 .336 .425 6.9(16) H(N2) 0.5 -.207 .299 .422 4.3(12) H(N2') 0.5 -.350 .306 .329 7.1(16) H(N3) 0.5 -.126 .227 .532 5.8(14) H(N3') 0.5 -.212 .298 .625 5.5(14) H(N4) 0.5 .008 .286 .557 4.9(12) H(N4') 0.5 .129 .384 .633 4.6(12) H(N5) 0.5 .750 .428 .075 8.2(19) H(N5') 0.5 .591 .428 .016 3.9(11) H(N6) 0.5 .457 .423 .032 3.6(11) H(N6') 0.5 .432 .407 .118 5.4(13) H(1) 1.0 .114(4) .118(3) .203(3) 6.5(9) H(2) 1.0 .090(5) .261(4) .212(3) 9.0(10) H(3) 1.0 .240(5) .230(4) .286(3) 8.6(11) H(4) 1.0 .053(3) .1430(25) .3540(19) 4.6(6) H(5) 1.0 -.201(3) .2139(24) .2227(19) 4.3(6) H(6) 1.0 -.154(4) .075(3) .2014(24) 6.3(8) H(7) 1.0 -.227(3) .0736(25) .3475(19) 4.6(6) H(8) 1.0 -.504(4) .032(3) .263(3) 7.3(10) H(9) 1.0 -.483(5) .116(4) .197(3) 9.6(11) H(10) 1.0 -.406(4) -.021(4) .186(3) 8.0(10) H(11) 1.0 -.524(4) .192(3) .3952(24) 6.8(8) H(12) 1.0 -.421(3) .319(3) .4781(21) 5.0(7) H(13) 1.0 -.445(3) .1547(24) .5379(20) 5.2(6) H(14) 1.0 -.336(4) .064(3) .4590(24) 6.6(8) H(15) 1.0 -.115(3) .063(3) .5763(22) 5.2(7) H(16) 1.0 -.163(4) .071(3) .730(3) 7.4(9) H(17) 1.0 -.244(4) .194(4) .735(3) 8.0(10) H(18) 1.0 -.340(7) .067(5) .640(4) 13.0(17) H(19) 1.0 .081(3) .163(3) .7341(22) 5.2(7) H(20) 1.0 .032(3) .285(3) .7350(22) 5.3(7) H(21) 1.0 .164(3) .131(3) .5879(21) 5.0(7) H(22) 1.0 .417(5) .267(4) .675(3) 10.0(12) H(23) 1.0 .345(5) .197(4) .741(3) 8.8(11) H(24) 1.0 .327(5) .340(4) .764(3) 9.6(12) H(25) 1.0 .251(3) .216(3) .4883(22) 5.8(7) H(26) 1.0 .348(4) .348(3) .5705(21) 5.3(7) H(27) 1.0 .257(3) .388(3) .4289(21) 5.3(7) H(28) 1.0 .162(3) .467(3) .5045(22) 5.3(7) H(29) 1.0 .882(4) .219(3) -.0616(21) 4.9(7) H(30) 1.0 .784(4) .104(4) -.0568(25) 7.2(9) H(31) 1.0 .872(4) .213(3) .046(3) 6.9(8) H(32) 1.0 .600(3) .2300(22) -.1070(20) 3.9(5) H(33) 1.0 .554(3) .123(3) -.0029(17) 3.8(5) H(34) 1.0 .607(3) .2506(22) .0868(21) 3.8(6) H(35) 1.0 .336(3) .2262(22) -.0771(19) 3.7(5) H(36) 1.0 .320(4) .198(3) .107(3) 7.6(9) H(37) 1.0 .170(5) .183(3) .019(3) 7.8(10) H(38) 1.0 .283(4) .076(4) -.0043(24) 6.9(8) H(39) 1.0 .832(3) .6196(24) .0520(21) 4.7(6) H(40) 1.0 .853(4) .610(3) -.0634(21) 5.6(7) H(41) 1.0 .870(4) .415(3) -.0571(20) 5.1(7) H(42) 1.0 .705(4) .401(3) -.1277(24) 5.3(7) _cod_database_code 2003517