#------------------------------------------------------------------------------ #$Date: 2008-02-25 18:36:12 +0200 (Mon, 25 Feb 2008) $ #$Revision: 177 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100749.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_1100749 _chemical_formula_sum 'C59.60 H78.40 Co4 F12 N12 O17.60 P2' _chemical_formula_weight 1770.20 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.867(4) _cell_length_b 14.534(6) _cell_length_c 12.289(5) _cell_angle_alpha 70.09(1) _cell_angle_beta 80.60(1) _cell_angle_gamma 69.86(1) _cell_volume 1868.3(1) _cell_formula_units_Z 1 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 11.6 _exptl_crystal_description 'parallelipiped' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 1.56 _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 907 _exptl_absorpt_coefficient_mu 1.018 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 298 _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 'Crystal Logic Dual Goniometer' _diffrn_measurement_method 'theta-2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 6364 _diffrn_reflns_av_R_equivalents 0.0172 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 24.25 _reflns_number_total 6046 _reflns_number_gt 4376 _reflns_threshold_expression >2sigma(I) ##'Program COLLECT (UCLA Cryst.package C.E.Strouse 1994)' ##'Program LEAST (UCLA Cryst.package C.E.Strouse 1994)' ##'Program REDUCE (UCLA Cryst.package C.E.Strouse 1994)' _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^)+(0.0673P)^2^+3.2720P] 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 6046 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1602 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.569 _refine_ls_shift/su_mean 0.023 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 Co1 Co -0.13924(6) 0.10415(5) 0.63492(6) 0.0393(2) Uani 1 1 d . . . Co2 Co 0.16158(6) 0.10824(5) 0.36788(6) 0.0377(2) Uani 1 1 d . . . O1 O 0.0217(3) 0.1228(3) 0.5710(3) 0.0513(9) Uani 1 1 d . . . N1 N 0.0918(4) 0.2369(3) 0.2480(3) 0.0431(10) Uani 1 1 d . . . N2 N 0.0303(4) 0.1676(3) 0.4592(3) 0.0411(9) Uani 1 1 d . . . N3 N -0.2054(4) 0.2619(3) 0.5616(4) 0.0457(10) Uani 1 1 d . . . O11 O 0.1742(3) -0.0915(2) 0.5121(3) 0.0441(8) Uani 1 1 d . . . N11 N 0.2655(4) 0.1515(3) 0.4331(4) 0.0446(10) Uani 1 1 d . . . N12 N 0.2170(3) -0.0142(3) 0.4915(3) 0.0396(9) Uani 1 1 d . . . O21 O -0.3004(3) 0.0947(3) 0.7102(3) 0.0510(9) Uani 1 1 d . . . O22 O -0.2946(3) -0.0674(3) 0.7371(3) 0.0460(8) Uani 1 1 d . . . OM1 O 0.0701(3) 0.0464(3) 0.3174(3) 0.0456(8) Uani 1 1 d . . . OE1 O -0.1016(4) 0.1254(4) 0.7806(4) 0.0744(13) Uani 1 1 d . . . C1 C 0.1292(6) 0.2632(5) 0.1368(5) 0.0560(15) Uani 1 1 d . . . C2 C 0.0598(7) 0.3421(5) 0.0544(6) 0.0682(19) Uani 1 1 d . . . C3 C -0.0540(6) 0.3941(5) 0.0860(5) 0.0657(17) Uani 1 1 d . . . C4 C -0.0940(6) 0.3693(4) 0.2006(5) 0.0538(14) Uani 1 1 d . . . C5 C -0.0188(5) 0.2921(4) 0.2813(4) 0.0442(12) Uani 1 1 d . . . C6 C -0.0476(5) 0.2548(4) 0.4072(4) 0.0424(11) Uani 1 1 d . . . C7 C -0.1495(5) 0.3143(4) 0.4672(4) 0.0473(12) Uani 1 1 d . . . C8 C -0.1861(6) 0.4209(5) 0.4295(6) 0.0617(16) Uani 1 1 d . . . C9 C -0.2866(7) 0.4753(5) 0.4842(6) 0.0720(19) Uani 1 1 d . . . C10 C -0.3427(7) 0.4212(6) 0.5774(7) 0.073(2) Uani 1 1 d . . . C11 C -0.2999(5) 0.3165(5) 0.6132(6) 0.0590(15) Uani 1 1 d . . . C21 C 0.2846(6) 0.2424(5) 0.3941(6) 0.0578(15) Uani 1 1 d . . . C22 C 0.3617(7) 0.2655(6) 0.4459(7) 0.0728(19) Uani 1 1 d . . . C23 C 0.4226(7) 0.1900(6) 0.5393(7) 0.080(2) Uani 1 1 d . . . H23 H 0.4760 0.2032 0.5750 0.10(3) Uiso 1 1 calc R . . C24 C 0.4044(7) 0.0963(6) 0.5789(6) 0.0700(18) Uani 1 1 d . . . C25 C 0.3229(5) 0.0777(4) 0.5263(5) 0.0493(13) Uani 1 1 d . . . C26 C 0.2928(4) -0.0188(4) 0.5612(4) 0.0438(12) Uani 1 1 d . . . C27 C 0.3367(5) -0.1083(5) 0.6632(5) 0.0609(16) Uani 1 1 d . . . C28 C 0.3499(7) -0.2110(5) 0.6651(7) 0.084(2) Uani 1 1 d . . . H28 H 0.3296 -0.2224 0.6019 0.16(2) Uiso 1 1 calc R . . C29 C 0.3934(8) -0.2931(7) 0.7629(8) 0.109(3) Uani 1 1 d . . . H29 H 0.4056 -0.3611 0.7678 0.16(2) Uiso 1 1 calc R . . C30 C 0.4180(10) -0.2654(9) 0.8552(8) 0.133(4) Uani 1 1 d . . . H30 H 0.4390 -0.3152 0.9262 0.16(2) Uiso 1 1 calc R . . C31 C 0.4113(14) -0.1731(9) 0.8408(10) 0.175(7) Uani 1 1 d . . . H31 H 0.4372 -0.1601 0.8999 0.16(2) Uiso 1 1 calc R . . N13 N 0.3702(9) -0.0932(6) 0.7482(6) 0.136(4) Uani 1 1 d . . . C41 C -0.3348(4) 0.0177(4) 0.7594(4) 0.0437(12) Uani 1 1 d . . . C42 C -0.4318(5) 0.0239(5) 0.8529(5) 0.0642(17) Uani 1 1 d . . . H42A H -0.4920 -0.0010 0.8399 0.132(19) Uiso 1 1 calc R . . H42B H -0.4675 0.0941 0.8525 0.132(19) Uiso 1 1 calc R . . H42C H -0.3983 -0.0175 0.9266 0.132(19) Uiso 1 1 calc R . . CM1 C -0.0254(14) 0.0960(11) 0.2438(18) 0.231(9) Uani 1 1 d . . . HM1A H -0.0710 0.0503 0.2532 0.278 Uiso 1 1 calc R . . HM1B H 0.0054 0.1151 0.1649 0.278 Uiso 1 1 calc R . . HM1C H -0.0763 0.1566 0.2626 0.278 Uiso 1 1 calc R . . CE1A C -0.118(2) 0.071(2) 0.878(2) 0.110(7) Uani 0.50 1 d P . . CE2A C -0.1159(18) -0.0190(17) 0.9040(14) 0.099(6) Uani 0.50 1 d P . . CE1B C -0.175(2) 0.130(2) 0.8920(19) 0.125(10) Uani 0.50 1 d P . . CE2B C -0.123(4) 0.123(3) 0.963(3) 0.198(15) Uani 0.50 1 d P . . P1 P 0.38668(16) 0.34844(14) 0.84663(15) 0.0678(5) Uani 1 1 d . . . F1 F 0.3994(5) 0.4558(4) 0.7625(5) 0.1149(17) Uani 1 1 d . . . F2 F 0.2493(4) 0.3899(4) 0.8170(4) 0.0998(14) Uani 1 1 d . . . F3 F 0.4214(5) 0.3051(4) 0.7408(4) 0.1080(16) Uani 1 1 d . . . F4 F 0.3510(6) 0.3930(5) 0.9507(5) 0.152(2) Uani 1 1 d . . . F5 F 0.5236(4) 0.3087(5) 0.8734(5) 0.134(2) Uani 1 1 d . . . F6 F 0.3699(5) 0.2445(4) 0.9292(5) 0.133(2) Uani 1 1 d . . . H1 H 0.196(5) 0.226(4) 0.128(5) 0.053(17) Uiso 1 1 d . . . H2 H 0.083(8) 0.351(6) -0.014(7) 0.11(3) Uiso 1 1 d . . . H3 H -0.105(5) 0.447(5) 0.036(5) 0.064(18) Uiso 1 1 d . . . H4 H -0.168(5) 0.401(4) 0.222(4) 0.045(15) Uiso 1 1 d . . . H8 H -0.145(6) 0.454(5) 0.365(6) 0.07(2) Uiso 1 1 d . . . H9 H -0.310(6) 0.550(5) 0.467(6) 0.08(2) Uiso 1 1 d . . . H10 H -0.400(6) 0.453(5) 0.607(5) 0.059(18) Uiso 1 1 d . . . H11 H -0.336(5) 0.269(4) 0.680(5) 0.054(16) Uiso 1 1 d . . . H21 H 0.242(5) 0.288(4) 0.330(5) 0.045(15) Uiso 1 1 d . . . H22 H 0.369(7) 0.348(6) 0.407(7) 0.11(3) Uiso 1 1 d . . . H24 H 0.446(6) 0.053(5) 0.636(6) 0.07(2) Uiso 1 1 d . . . OM2 O -0.0819(19) 0.8514(15) 0.1264(18) 0.172(7) Uiso 0.50 1 d P . . CM2 C -0.194(3) 0.846(3) 0.197(3) 0.166(11) Uiso 0.50 1 d P . . OM2A O -0.1582(19) 0.9110(17) 0.1817(19) 0.175(7) Uiso 0.50 1 d P . . CM2A C -0.216(4) 0.871(3) 0.121(4) 0.203(15) Uiso 0.50 1 d P . . OM3 O 0.294(2) 0.5322(17) 0.1449(18) 0.192(8) Uiso 0.50 1 d P . . CM3 C 0.263(2) 0.4587(19) 0.154(2) 0.128(7) Uiso 0.50 1 d P . . OM3A O 0.174(2) 0.4956(17) 0.209(2) 0.206(9) Uiso 0.50 1 d P . . CM3A C 0.086(4) 0.495(3) 0.319(4) 0.206(14) Uiso 0.50 1 d P . . OM4 O -0.067(3) 0.649(3) 0.378(3) 0.204(11) Uiso 0.40 1 d P . . CM4 C 0.028(3) 0.676(3) 0.298(3) 0.154(11) Uiso 0.40 1 d P . . OM4A O 0.009(4) 0.570(4) 0.363(4) 0.251(15) Uiso 0.40 1 d P . . CM4A C 0.003(4) 0.614(4) 0.256(4) 0.203(17) Uiso 0.40 1 d P . . 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 Co1 0.0371(4) 0.0407(4) 0.0361(4) -0.0117(3) 0.0025(3) -0.0092(3) Co2 0.0341(4) 0.0391(4) 0.0368(4) -0.0120(3) 0.0035(3) -0.0096(3) O1 0.047(2) 0.056(2) 0.0317(18) -0.0069(16) 0.0028(15) -0.0013(17) N1 0.046(2) 0.040(2) 0.039(2) -0.0090(18) 0.0052(18) -0.0139(19) N2 0.040(2) 0.039(2) 0.037(2) -0.0095(18) 0.0035(17) -0.0084(18) N3 0.039(2) 0.049(2) 0.046(2) -0.019(2) 0.0027(19) -0.0084(19) O11 0.051(2) 0.0408(19) 0.0391(18) -0.0049(15) -0.0120(15) -0.0161(16) N11 0.042(2) 0.052(3) 0.046(2) -0.021(2) 0.0052(19) -0.019(2) N12 0.035(2) 0.046(2) 0.038(2) -0.0151(18) 0.0019(17) -0.0110(18) O21 0.043(2) 0.047(2) 0.059(2) -0.0193(18) 0.0118(17) -0.0123(17) O22 0.0398(18) 0.048(2) 0.045(2) -0.0154(16) 0.0097(15) -0.0124(16) OM1 0.0407(19) 0.046(2) 0.047(2) -0.0099(16) -0.0089(16) -0.0108(16) OE1 0.076(3) 0.091(3) 0.054(3) -0.019(3) 0.002(2) -0.028(3) C1 0.052(4) 0.054(3) 0.046(3) -0.005(3) 0.011(3) -0.013(3) C2 0.076(4) 0.064(4) 0.044(3) -0.003(3) 0.015(3) -0.018(3) C3 0.074(4) 0.051(3) 0.051(4) 0.001(3) -0.007(3) -0.008(3) C4 0.051(3) 0.049(3) 0.049(3) -0.008(3) -0.002(3) -0.007(3) C5 0.048(3) 0.040(3) 0.040(3) -0.012(2) 0.002(2) -0.011(2) C6 0.045(3) 0.037(3) 0.039(3) -0.011(2) 0.004(2) -0.009(2) C7 0.049(3) 0.045(3) 0.044(3) -0.019(2) -0.001(2) -0.005(2) C8 0.068(4) 0.049(3) 0.058(4) -0.018(3) 0.004(3) -0.007(3) C9 0.087(5) 0.047(4) 0.068(4) -0.027(3) -0.004(4) 0.006(3) C10 0.065(4) 0.070(4) 0.075(5) -0.046(4) 0.012(4) 0.006(3) C11 0.046(3) 0.063(4) 0.067(4) -0.034(3) 0.011(3) -0.008(3) C21 0.057(4) 0.056(4) 0.066(4) -0.021(3) 0.002(3) -0.024(3) C22 0.076(5) 0.073(4) 0.085(5) -0.030(4) -0.001(4) -0.039(4) C23 0.081(5) 0.105(6) 0.080(5) -0.038(4) -0.001(4) -0.054(5) C24 0.069(4) 0.091(5) 0.061(4) -0.019(4) -0.007(3) -0.042(4) C25 0.040(3) 0.067(4) 0.045(3) -0.024(3) 0.006(2) -0.020(3) C26 0.041(3) 0.056(3) 0.034(3) -0.013(2) 0.000(2) -0.016(2) C27 0.056(3) 0.073(4) 0.050(3) -0.004(3) -0.014(3) -0.024(3) C28 0.078(5) 0.067(4) 0.089(5) 0.000(4) -0.032(4) -0.013(4) C29 0.098(6) 0.085(6) 0.121(7) 0.018(5) -0.048(6) -0.032(5) C30 0.166(10) 0.142(9) 0.089(7) 0.033(6) -0.070(7) -0.083(8) C31 0.325(19) 0.112(8) 0.118(8) 0.027(7) -0.142(11) -0.105(11) N13 0.246(11) 0.099(5) 0.087(5) 0.011(4) -0.096(6) -0.085(6) C41 0.032(2) 0.053(3) 0.039(3) -0.013(2) 0.001(2) -0.005(2) C42 0.053(3) 0.078(4) 0.065(4) -0.033(3) 0.020(3) -0.023(3) CM1 0.169(15) 0.149(13) 0.39(3) -0.079(15) -0.052(17) -0.055(11) CE1A 0.088(15) 0.13(2) 0.12(2) -0.049(17) -0.033(14) -0.023(14) CE2A 0.130(16) 0.135(16) 0.060(9) -0.039(10) 0.009(9) -0.075(14) CE1B 0.121(19) 0.17(2) 0.066(12) -0.066(15) 0.008(12) 0.002(16) CE2B 0.25(4) 0.23(4) 0.13(2) -0.10(3) 0.02(3) -0.07(3) P1 0.0582(10) 0.0700(11) 0.0575(10) -0.0198(8) 0.0022(8) -0.0005(8) F1 0.110(4) 0.090(3) 0.135(4) -0.018(3) 0.000(3) -0.039(3) F2 0.063(2) 0.099(3) 0.106(3) -0.012(3) -0.003(2) -0.008(2) F3 0.112(4) 0.125(4) 0.084(3) -0.059(3) 0.003(3) -0.011(3) F4 0.151(5) 0.204(7) 0.111(4) -0.105(5) 0.001(4) -0.014(5) F5 0.070(3) 0.201(6) 0.102(4) -0.040(4) -0.021(3) -0.006(3) F6 0.130(4) 0.089(3) 0.115(4) 0.012(3) 0.013(3) -0.008(3)