#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000396.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_4000396 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_formula_sum 'C28 H46 N6 O25 P4 Zn5' _chemical_formula_weight 1317.44 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.3635(8) _cell_length_b 12.0029(6) _cell_length_c 16.9974(9) _cell_angle_alpha 90.00 _cell_angle_beta 113.3810(10) _cell_angle_gamma 90.00 _cell_volume 2689.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brick _exptl_crystal_colour colorless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 2.396 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(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 Siemens Smart CCD _diffrn_measurement_method narrow frame method _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1.0% _diffrn_reflns_number 7916 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4678 _reflns_number_gt 3563 _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^)+(0.0772P)^2^+11.2678P] 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 SHELXL _refine_ls_extinction_coef 0.0001(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4678 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0811 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.002 _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 0.10632(5) 0.06245(6) 0.10909(4) 0.0223(2) Uani 1 1 d . . . Zn2 Zn 0.31876(5) -0.07586(6) 0.43504(4) 0.0231(2) Uani 1 1 d . A . Zn3 Zn 0.5000 0.01420(9) 0.2500 0.0262(3) Uani 1 2 d S . . P1 P 0.11709(12) -0.00649(14) 0.43073(10) 0.0248(4) Uani 1 1 d . . . P2 P 0.31400(12) 0.07122(14) 0.28793(10) 0.0222(4) Uani 1 1 d . A . N1 N 0.2792(4) 0.1087(4) 0.4320(3) 0.0207(11) Uani 1 1 d . . . N2 N 0.0630(5) 0.2216(5) 0.0674(4) 0.0405(15) Uani 1 1 d . . . N3 N 0.3839(4) -0.2321(5) 0.4576(4) 0.0325(13) Uani 1 1 d . . . C1 C 0.3904(5) 0.0666(5) 0.5835(4) 0.0277(14) Uani 1 1 d . . . C2 C 0.3256(5) 0.1612(5) 0.3778(4) 0.0258(14) Uani 1 1 d . . . H2A H 0.3967 0.1759 0.4120 0.031 Uiso 1 1 calc R . . H2B H 0.2924 0.2318 0.3563 0.031 Uiso 1 1 calc R . . C3 C 0.3218(5) 0.1508(5) 0.5206(4) 0.0281(14) Uani 1 1 d . . . H3A H 0.2667 0.1700 0.5375 0.034 Uiso 1 1 calc R . . H3B H 0.3601 0.2182 0.5230 0.034 Uiso 1 1 calc R . . C4 C 0.1655(5) 0.1117(5) 0.3928(4) 0.0253(14) Uani 1 1 d . . . H4A H 0.1413 0.1091 0.3308 0.030 Uiso 1 1 calc R . . H4B H 0.1417 0.1803 0.4086 0.030 Uiso 1 1 calc R . . C10 C 0.0843(19) 0.3042(17) 0.1277(15) 0.051(6) Uani 0.50 1 d P A 1 C11 C 0.060(3) 0.417(2) 0.1044(15) 0.071(9) Uani 0.50 1 d P A 1 C10' C 0.1291(17) 0.3056(19) 0.1056(17) 0.065(7) Uani 0.50 1 d P A 2 C11' C 0.107(2) 0.4149(18) 0.0788(17) 0.074(9) Uani 0.50 1 d P A 2 C12 C 0.0134(8) 0.4409(7) 0.0142(6) 0.073(3) Uani 1 1 d . . . C13 C -0.0334(7) 0.3530(6) -0.0365(5) 0.054(2) Uani 1 1 d . A . H13A H -0.0829 0.3653 -0.0911 0.064 Uiso 1 1 calc R . . C14 C -0.0083(7) 0.2474(6) -0.0076(5) 0.049(2) Uani 1 1 d . A . H14A H -0.0437 0.1893 -0.0431 0.059 Uiso 1 1 calc R . . C20 C 0.4003(9) -0.2875(7) 0.5296(6) 0.071(3) Uani 1 1 d . . . H20A H 0.3807 -0.2537 0.5699 0.086 Uiso 1 1 calc R . . C21 C 0.4441(9) -0.3913(7) 0.5486(6) 0.074(3) Uani 1 1 d . . . H21A H 0.4523 -0.4260 0.5998 0.089 Uiso 1 1 calc R . . C22 C 0.4759(5) -0.4439(6) 0.4915(4) 0.0325(16) Uani 1 1 d . . . C23 C 0.4642(7) -0.3839(6) 0.4190(5) 0.046(2) Uani 1 1 d . . . H23A H 0.4876 -0.4131 0.3795 0.056 Uiso 1 1 calc R . . C24 C 0.4183(6) -0.2813(6) 0.4050(5) 0.0416(18) Uani 1 1 d . . . H24A H 0.4108 -0.2438 0.3549 0.050 Uiso 1 1 calc R . . O1 O 0.4051(4) -0.0276(4) 0.5580(3) 0.0341(11) Uani 1 1 d . . . O2 O 0.4285(4) 0.0974(4) 0.6603(3) 0.0350(11) Uani 1 1 d . . . O11 O 0.0046(3) -0.0157(4) 0.3753(3) 0.0321(11) Uani 1 1 d . . . O12 O 0.1757(3) -0.1066(4) 0.4179(3) 0.0311(11) Uani 1 1 d . . . O13 O 0.1390(4) 0.0149(4) 0.5244(3) 0.0345(11) Uani 1 1 d . . . O21 O 0.2084(3) 0.0872(4) 0.2201(3) 0.0338(11) Uani 1 1 d . . . O22 O 0.3326(4) -0.0469(4) 0.3247(3) 0.0300(10) Uani 1 1 d . . . O23 O 0.3955(3) 0.1095(4) 0.2574(3) 0.0324(11) Uani 1 1 d . . . O1W O 0.4031(11) -0.3437(9) 0.7301(8) 0.167(5) Uani 1 1 d . . . O2W O -0.2176(16) 0.2141(12) -0.1982(8) 0.293(13) Uani 1 1 d . . . O3W O 0.5000 -0.318(2) 0.2500 0.214(9) Uiso 1 2 d S . . O4W O -0.0887(15) -0.1921(17) 0.2512(12) 0.114(6) Uiso 0.50 1 d P . . O5W O 0.320(2) -0.389(3) 0.1645(19) 0.191(11) Uiso 0.50 1 d P . . O6W O 0.275(2) 0.461(2) 0.2874(18) 0.170(10) Uiso 0.50 1 d P . . O7W O 0.235(2) 0.430(2) 0.4668(19) 0.180(11) Uiso 0.50 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 Zn1 0.0210(4) 0.0214(4) 0.0238(4) -0.0004(3) 0.0079(3) 0.0004(3) Zn2 0.0226(4) 0.0205(4) 0.0260(4) 0.0023(3) 0.0093(3) 0.0056(3) Zn3 0.0209(5) 0.0320(6) 0.0256(5) 0.000 0.0092(4) 0.000 P1 0.0223(8) 0.0273(9) 0.0283(9) 0.0013(7) 0.0138(7) 0.0013(7) P2 0.0187(8) 0.0261(9) 0.0231(8) 0.0024(7) 0.0096(7) 0.0016(7) N1 0.018(3) 0.027(3) 0.017(2) 0.000(2) 0.006(2) 0.001(2) N2 0.041(4) 0.019(3) 0.046(4) 0.004(3) 0.001(3) 0.007(3) N3 0.038(3) 0.023(3) 0.038(3) 0.002(3) 0.018(3) 0.008(3) C1 0.027(3) 0.030(4) 0.023(3) 0.002(3) 0.006(3) 0.004(3) C2 0.027(3) 0.024(3) 0.029(3) -0.002(3) 0.014(3) -0.005(3) C3 0.034(4) 0.025(3) 0.025(3) -0.003(3) 0.011(3) 0.000(3) C4 0.028(3) 0.027(3) 0.023(3) 0.006(3) 0.013(3) 0.005(3) C10 0.071(16) 0.018(9) 0.055(12) -0.010(7) 0.016(11) -0.004(10) C11 0.13(3) 0.034(11) 0.033(10) -0.004(8) 0.009(12) 0.020(15) C10' 0.048(14) 0.029(10) 0.077(17) 0.010(11) -0.019(11) -0.003(10) C11' 0.079(18) 0.020(9) 0.067(17) -0.017(11) -0.030(12) 0.001(11) C12 0.081(7) 0.026(5) 0.066(6) 0.007(4) -0.019(5) -0.003(5) C13 0.065(6) 0.022(4) 0.048(5) 0.001(3) -0.005(4) 0.003(4) C14 0.066(6) 0.022(4) 0.038(4) 0.000(3) -0.001(4) -0.003(4) C20 0.144(10) 0.036(5) 0.065(6) 0.021(4) 0.075(7) 0.041(6) C21 0.144(10) 0.038(5) 0.065(6) 0.030(4) 0.068(7) 0.053(6) C22 0.039(4) 0.025(4) 0.035(4) 0.002(3) 0.017(3) 0.009(3) C23 0.066(6) 0.035(4) 0.046(4) 0.011(4) 0.030(4) 0.023(4) C24 0.056(5) 0.032(4) 0.040(4) 0.013(3) 0.022(4) 0.018(4) O1 0.034(3) 0.029(3) 0.030(3) 0.001(2) 0.002(2) 0.009(2) O2 0.037(3) 0.038(3) 0.020(2) -0.003(2) 0.001(2) 0.001(2) O11 0.020(2) 0.038(3) 0.041(3) -0.002(2) 0.015(2) 0.000(2) O12 0.025(2) 0.025(2) 0.045(3) -0.003(2) 0.016(2) -0.001(2) O13 0.041(3) 0.037(3) 0.032(3) 0.004(2) 0.022(2) -0.004(2) O21 0.024(2) 0.047(3) 0.027(2) -0.005(2) 0.006(2) 0.002(2) O22 0.041(3) 0.024(2) 0.033(2) 0.0039(19) 0.022(2) 0.006(2) O23 0.026(2) 0.036(3) 0.043(3) 0.006(2) 0.022(2) 0.001(2) O1W 0.274(15) 0.107(8) 0.143(10) -0.018(7) 0.107(10) 0.040(9) O2W 0.42(3) 0.173(13) 0.107(9) 0.011(9) -0.085(12) -0.185(16)