#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000390.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_4000390 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_formula_sum 'C38 H72 Ce N4 O4' _chemical_formula_weight 789.12 _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 39.8617(24) _cell_length_b 10.5075(6) _cell_length_c 20.5428(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.758(1) _cell_angle_gamma 90.00 _cell_volume 8560.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5962 _cell_measurement_theta_min 1.03 _cell_measurement_theta_max 24.41 _exptl_crystal_description 'Multifaceted block' _exptl_crystal_colour Gold _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7029 _exptl_absorpt_correction_T_max 0.8096 _exptl_absorpt_process_details ? _publ_section_experimental ; All measurements were made with a Siemens SMART platform diffractometer equipped with a 1K CCD area detector. A hemisphere of data (1271 frames at 5 cm detector distance) was collected using a narrow-frame method with scan widths of 0.30\% in omega an an exposure time of 20 s/frame. The first 50 frames were re-measured at the end of data collection to monitor instrument and crystal stability, and the maximum correction on I was <1%. The data were integrated using the Siemens SAINT program, with the intensities corrected for Lorentz factor, polarization, air absorption, and absorption due to variation in the path length through the detector faceplate. A psi scan absorption correction was applied based on the entire data set. Redundant reflections were averaged. Final cell constants were refined using 5962 reflections having I>10\s(I), and these, along with other information pertinent to data collection and refinement, are listed in Table 1. The Laue symmetry was determined to be 2/m, and from the systematic absences noted the space group was shown to be either Cc or C2/c. One of the alkoxide ligands (O2) was found to be disordered over two different orientations, having approximately 55:45 occupancy. ; _publ_section_figure_captions ; Fig. 1 -- View of the molecule showing the atom numbering scheme for the core atoms. Thermal ellipsoids are 40% equiprobability envelopes, with hydrogens omitted. Only one orientation of the disordered alkoxide ligand is shown. Fig. 2 -- Packing of the molecules in the unit cell. ; _diffrn_ambient_temperature 223(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 CCD _diffrn_detector_area_resol_mean 1K _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 19720 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 24.41 _reflns_number_total 7238 _reflns_number_gt 4817 _reflns_threshold_expression >4sigma(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^)+(0.0150P)^2^+40.0000P] 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_number_reflns 6917 _refine_ls_number_parameters 419 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0823 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.550 _refine_ls_shift/su_mean 0.020 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 Ce Ce 0.119827(5) 0.74904(2) 0.379972(9) 0.02959(7) Uani 1 1 d . . . O1 O 0.16078(7) 0.6540(3) 0.43221(13) 0.0411(6) Uani 1 1 d . . . O2 O 0.0742(2) 0.6751(9) 0.4081(4) 0.041(3) Uiso 0.40 1 d PD . . O2' O 0.08041(14) 0.6447(6) 0.4154(3) 0.0400(17) Uiso 0.60 1 d PD . . O3 O 0.11980(7) 0.9060(3) 0.44510(14) 0.0455(7) Uiso 1 1 d . . . O4 O 0.11888(7) 0.6490(3) 0.28966(12) 0.0406(6) Uani 1 1 d . . . N1 N 0.16473(9) 0.8940(3) 0.32569(16) 0.0419(8) Uani 1 1 d . . . N2 N 0.22922(10) 1.1780(4) 0.2656(2) 0.0615(11) Uani 1 1 d . . . N3 N 0.07954(9) 0.9044(3) 0.30595(17) 0.0444(8) Uani 1 1 d . . . N4 N 0.02324(10) 1.1365(4) 0.16897(19) 0.0584(10) Uani 1 1 d . . . C1 C 0.18349(10) 0.5906(4) 0.47856(19) 0.0395(9) Uani 1 1 d . . . C2 C 0.20447(12) 0.6905(5) 0.5190(2) 0.0584(13) Uani 1 1 d . . . H2A H 0.2181 0.7378 0.4908 0.088 Uiso 1 1 calc R . . H2B H 0.2191 0.6484 0.5530 0.088 Uiso 1 1 calc R . . H2C H 0.1895 0.7485 0.5389 0.088 Uiso 1 1 calc R . . C3 C 0.16247(13) 0.5142(5) 0.5230(2) 0.0634(14) Uani 1 1 d . . . H3A H 0.1492 0.4514 0.4972 0.095 Uiso 1 1 calc R . . H3B H 0.1476 0.5712 0.5436 0.095 Uiso 1 1 calc R . . H3C H 0.1773 0.4716 0.5564 0.095 Uiso 1 1 calc R . . C4 C 0.20560(11) 0.5013(4) 0.4414(2) 0.0497(11) Uani 1 1 d . . . H4A H 0.1903 0.4391 0.4175 0.060 Uiso 1 1 calc R . . C5 C 0.23136(14) 0.4244(6) 0.4867(3) 0.0784(17) Uani 1 1 d . . . H5A H 0.2198 0.3795 0.5190 0.118 Uiso 1 1 calc R . . H5B H 0.2479 0.4819 0.5085 0.118 Uiso 1 1 calc R . . H5C H 0.2427 0.3636 0.4608 0.118 Uiso 1 1 calc R . . C6 C 0.22361(13) 0.5717(5) 0.3910(2) 0.0677(14) Uani 1 1 d . . . H6A H 0.2074 0.6211 0.3630 0.101 Uiso 1 1 calc R . . H6B H 0.2346 0.5109 0.3646 0.101 Uiso 1 1 calc R . . H6C H 0.2404 0.6282 0.4129 0.101 Uiso 1 1 calc R . . C7 C 0.0487(3) 0.6215(10) 0.4423(5) 0.077(4) Uiso 0.45 1 d PD . . C8 C 0.0223(5) 0.7233(16) 0.4485(8) 0.091(7) Uiso 0.45 1 d PD . . H8A H 0.0124 0.7477 0.4052 0.137 Uiso 0.45 1 calc PR . . H8B H 0.0327 0.7970 0.4706 0.137 Uiso 0.45 1 calc PR . . H8C H 0.0048 0.6903 0.4735 0.137 Uiso 0.45 1 calc PR . . C9 C 0.0591(3) 0.5793(13) 0.5130(5) 0.067(3) Uiso 0.45 1 d PD . . H9A H 0.0760 0.5128 0.5133 0.100 Uiso 0.45 1 calc PR . . H9B H 0.0395 0.5470 0.5322 0.100 Uiso 0.45 1 calc PR . . H9C H 0.0684 0.6513 0.5383 0.100 Uiso 0.45 1 calc PR . . C10 C 0.0367(3) 0.5039(11) 0.4047(5) 0.130(6) Uiso 0.45 1 d PGD . . H10 H 0.0179 0.4672 0.4238 0.156 Uiso 0.45 1 d PG . . C11 C 0.0257(4) 0.5561(14) 0.3369(7) 0.101(5) Uiso 0.45 1 d PG . . H11A H 0.0165 0.4885 0.3093 0.151 Uiso 0.45 1 d PG . . H11B H 0.0089 0.6206 0.3400 0.151 Uiso 0.45 1 d PG . . H11C H 0.0449 0.5923 0.3187 0.151 Uiso 0.45 1 d PG . . C12 C 0.0640(4) 0.4051(12) 0.3985(7) 0.058(4) Uiso 0.45 1 d PG . . H12A H 0.0548 0.3345 0.3730 0.087 Uiso 0.45 1 d PG . . H12B H 0.0820 0.4425 0.3773 0.087 Uiso 0.45 1 d PG . . H12C H 0.0726 0.3758 0.4413 0.087 Uiso 0.45 1 d PG . . C7' C 0.05884(18) 0.5493(8) 0.4380(4) 0.072(3) Uiso 0.55 1 d PD . . C8' C 0.0642(5) 0.4136(11) 0.4160(8) 0.112(7) Uiso 0.55 1 d PD . . H8'A H 0.0632 0.4109 0.3686 0.169 Uiso 0.55 1 calc PR . . H8'B H 0.0467 0.3593 0.4305 0.169 Uiso 0.55 1 calc PR . . H8'C H 0.0861 0.3837 0.4347 0.169 Uiso 0.55 1 calc PR . . C9' C 0.0644(3) 0.5103(11) 0.5099(4) 0.074(3) Uiso 0.55 1 d PD . . H9'A H 0.0626 0.5847 0.5374 0.112 Uiso 0.55 1 calc PR . . H9'B H 0.0867 0.4732 0.5189 0.112 Uiso 0.55 1 calc PR . . H9'C H 0.0475 0.4483 0.5192 0.112 Uiso 0.55 1 calc PR . . C10' C 0.0235(2) 0.5933(10) 0.4150(4) 0.083(3) Uiso 0.55 1 d PGD . . H10' H 0.0085 0.5292 0.4283 0.099 Uiso 0.55 1 d PG . . C11' C 0.0140(3) 0.6127(10) 0.3422(4) 0.072(3) Uiso 0.55 1 d PG . . H11D H 0.0192 0.5372 0.3189 0.108 Uiso 0.55 1 d PG . . H11E H -0.0097 0.6299 0.3344 0.108 Uiso 0.55 1 d PG . . H11F H 0.0264 0.6833 0.3272 0.108 Uiso 0.55 1 d PG . . C12' C 0.0149(5) 0.7142(14) 0.4503(6) 0.129(10) Uiso 0.55 1 d PG . . H12D H 0.0207 0.7039 0.4965 0.194 Uiso 0.55 1 d PG . . H12E H 0.0273 0.7843 0.4348 0.194 Uiso 0.55 1 d PG . . H12F H -0.0088 0.7309 0.4420 0.194 Uiso 0.55 1 d PG . . C13 C 0.11800(13) 0.9802(4) 0.5023(2) 0.0509(11) Uani 1 1 d . . . C14 C 0.11675(16) 0.8883(5) 0.5600(2) 0.0760(17) Uani 1 1 d . . . H14A H 0.0967 0.8359 0.5530 0.114 Uiso 1 1 calc R . . H14B H 0.1162 0.9366 0.6002 0.114 Uiso 1 1 calc R . . H14C H 0.1366 0.8344 0.5634 0.114 Uiso 1 1 calc R . . C15 C 0.08510(15) 1.0565(6) 0.4948(3) 0.0827(18) Uani 1 1 d . . . H15A H 0.0661 0.9985 0.4879 0.124 Uiso 1 1 calc R . . H15B H 0.0851 1.1133 0.4577 0.124 Uiso 1 1 calc R . . H15C H 0.0832 1.1058 0.5342 0.124 Uiso 1 1 calc R . . C16 C 0.15013(16) 1.0634(5) 0.5109(2) 0.0688(15) Uani 1 1 d . . . H16A H 0.1695 1.0046 0.5106 0.083 Uiso 1 1 calc R . . C17 C 0.15177(16) 1.1533(5) 0.4529(3) 0.0762(16) Uani 1 1 d . . . H17A H 0.1478 1.1056 0.4124 0.114 Uiso 1 1 calc R . . H17B H 0.1739 1.1926 0.4553 0.114 Uiso 1 1 calc R . . H17C H 0.1347 1.2187 0.4541 0.114 Uiso 1 1 calc R . . C18 C 0.1556(2) 1.1382(7) 0.5735(3) 0.136(3) Uani 1 1 d . . . H18A H 0.1764 1.1863 0.5741 0.204 Uiso 1 1 calc R . . H18B H 0.1570 1.0804 0.6105 0.204 Uiso 1 1 calc R . . H18C H 0.1369 1.1963 0.5763 0.204 Uiso 1 1 calc R . . C19 C 0.12506(11) 0.5780(4) 0.23355(19) 0.0439(10) Uani 1 1 d . . . C20 C 0.16166(12) 0.6013(5) 0.2198(2) 0.0636(14) Uani 1 1 d . . . H20A H 0.1649 0.6911 0.2116 0.095 Uiso 1 1 calc R . . H20B H 0.1665 0.5526 0.1816 0.095 Uiso 1 1 calc R . . H20C H 0.1768 0.5748 0.2573 0.095 Uiso 1 1 calc R . . C21 C 0.10123(14) 0.6258(5) 0.1754(2) 0.0666(14) Uani 1 1 d . . . H21A H 0.1057 0.7149 0.1676 0.100 Uiso 1 1 calc R . . H21B H 0.0780 0.6159 0.1850 0.100 Uiso 1 1 calc R . . H21C H 0.1048 0.5767 0.1367 0.100 Uiso 1 1 calc R . . C22 C 0.11798(12) 0.4360(4) 0.24650(19) 0.0469(11) Uani 1 1 d . . . H22A H 0.0943 0.4307 0.2567 0.056 Uiso 1 1 calc R . . C23 C 0.12095(14) 0.3494(5) 0.1870(2) 0.0636(14) Uani 1 1 d . . . H23A H 0.1074 0.3841 0.1492 0.095 Uiso 1 1 calc R . . H23B H 0.1129 0.2648 0.1962 0.095 Uiso 1 1 calc R . . H23C H 0.1443 0.3448 0.1780 0.095 Uiso 1 1 calc R . . C24 C 0.13960(13) 0.3832(5) 0.3057(2) 0.0617(13) Uani 1 1 d . . . H24A H 0.1342 0.2941 0.3113 0.093 Uiso 1 1 calc R . . H24B H 0.1351 0.4303 0.3445 0.093 Uiso 1 1 calc R . . H24C H 0.1632 0.3914 0.2989 0.093 Uiso 1 1 calc R . . C25 C 0.19292(11) 0.9297(4) 0.3617(2) 0.0474(11) Uani 1 1 d . . . H25A H 0.1980 0.8893 0.4023 0.057 Uiso 1 1 calc R . . C26 C 0.21495(11) 1.0204(4) 0.3442(2) 0.0483(11) Uani 1 1 d . . . H26A H 0.2344 1.0401 0.3722 0.058 Uiso 1 1 calc R . . C27 C 0.20837(11) 1.0840(4) 0.2840(2) 0.0433(10) Uani 1 1 d . . . C28 C 0.17944(11) 1.0445(4) 0.2453(2) 0.0511(11) Uani 1 1 d . . . H28A H 0.1739 1.0811 0.2039 0.061 Uiso 1 1 calc R . . C29 C 0.15915(11) 0.9522(4) 0.2678(2) 0.0485(11) Uani 1 1 d . . . H29A H 0.1399 0.9281 0.2405 0.058 Uiso 1 1 calc R . . C30 C 0.25675(14) 1.2230(6) 0.3104(3) 0.087(2) Uani 1 1 d G . . H30A H 0.2681 1.2836 0.2857 0.130 Uiso 1 1 d G . . H30B H 0.2721 1.1572 0.3259 0.130 Uiso 1 1 d G . . H30C H 0.2484 1.2646 0.3469 0.130 Uiso 1 1 d G . . C31 C 0.22098(15) 1.2481(6) 0.2055(3) 0.0813(18) Uani 1 1 d G . . H31A H 0.2415 1.2913 0.1991 0.122 Uiso 1 1 d G . . H31B H 0.2035 1.3092 0.2091 0.122 Uiso 1 1 d G . . H31C H 0.2148 1.1932 0.1691 0.122 Uiso 1 1 d G . . C32 C 0.05863(11) 0.8575(4) 0.2568(2) 0.0520(11) Uani 1 1 d . . . H32A H 0.0568 0.7685 0.2533 0.062 Uiso 1 1 calc R . . C33 C 0.03968(11) 0.9288(4) 0.2112(2) 0.0528(12) Uani 1 1 d . . . H33A H 0.0256 0.8888 0.1779 0.063 Uiso 1 1 calc R . . C34 C 0.04139(10) 1.0619(4) 0.2142(2) 0.0453(10) Uani 1 1 d . . . C35 C 0.06305(11) 1.1118(4) 0.2657(2) 0.0484(11) Uani 1 1 d . . . H35A H 0.0654 1.2004 0.2706 0.058 Uiso 1 1 calc R . . C36 C 0.08073(11) 1.0320(4) 0.3087(2) 0.0476(11) Uani 1 1 d . . . H36A H 0.0948 1.0692 0.3429 0.057 Uiso 1 1 calc R . . C37 C 0.00239(13) 1.0785(6) 0.1151(3) 0.0713(15) Uani 1 1 d G . . H37A H -0.0081 1.1483 0.0910 0.107 Uiso 1 1 d G . . H37B H -0.0146 1.0254 0.1307 0.107 Uiso 1 1 d G . . H37C H 0.0154 1.0300 0.0872 0.107 Uiso 1 1 d G . . C38 C 0.02689(17) 1.2724(5) 0.1706(3) 0.094(2) Uani 1 1 d G . . H38A H 0.0119 1.3129 0.1376 0.140 Uiso 1 1 d G . . H38B H 0.0496 1.2953 0.1648 0.140 Uiso 1 1 d G . . H38C H 0.0217 1.2994 0.2129 0.140 Uiso 1 1 d G . . 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 Ce 0.03403(12) 0.02888(11) 0.02577(11) 0.00292(10) 0.00248(8) -0.00349(10) O1 0.0458(16) 0.0390(15) 0.0368(15) 0.0038(13) -0.0049(12) 0.0020(13) O4 0.0496(16) 0.0435(16) 0.0287(14) -0.0027(13) 0.0040(12) -0.0027(13) N1 0.050(2) 0.0391(19) 0.0366(19) 0.0036(16) 0.0056(16) -0.0095(16) N2 0.057(3) 0.058(3) 0.072(3) 0.010(2) 0.019(2) -0.017(2) N3 0.045(2) 0.045(2) 0.042(2) 0.0072(17) -0.0017(16) -0.0024(17) N4 0.056(2) 0.055(3) 0.060(3) 0.014(2) -0.012(2) 0.003(2) C1 0.040(2) 0.041(2) 0.035(2) 0.0034(19) -0.0076(18) 0.0001(18) C2 0.061(3) 0.055(3) 0.055(3) -0.013(2) -0.015(2) 0.004(2) C3 0.071(3) 0.067(3) 0.052(3) 0.017(3) 0.007(2) 0.000(3) C4 0.054(3) 0.045(3) 0.047(3) -0.003(2) -0.008(2) 0.008(2) C5 0.078(4) 0.079(4) 0.075(4) 0.002(3) -0.012(3) 0.035(3) C6 0.061(3) 0.087(4) 0.056(3) -0.002(3) 0.012(3) 0.008(3) C13 0.081(3) 0.039(2) 0.033(2) -0.0036(19) 0.007(2) 0.011(2) C14 0.119(5) 0.065(3) 0.045(3) 0.011(3) 0.016(3) 0.005(3) C15 0.107(5) 0.077(4) 0.068(4) -0.002(3) 0.026(3) 0.031(4) C16 0.103(4) 0.053(3) 0.048(3) -0.006(2) -0.003(3) -0.012(3) C17 0.113(5) 0.052(3) 0.063(3) -0.004(3) 0.005(3) -0.016(3) C18 0.235(10) 0.107(6) 0.059(4) -0.019(4) -0.013(5) -0.049(6) C19 0.052(3) 0.052(3) 0.028(2) -0.0043(19) 0.0055(18) -0.005(2) C20 0.069(3) 0.068(3) 0.058(3) -0.012(3) 0.024(3) -0.014(3) C21 0.095(4) 0.068(3) 0.035(2) 0.001(2) -0.004(3) 0.003(3) C22 0.059(3) 0.050(3) 0.033(2) -0.008(2) 0.007(2) -0.007(2) C23 0.089(4) 0.059(3) 0.043(3) -0.019(2) 0.007(3) -0.005(3) C24 0.089(4) 0.055(3) 0.041(3) -0.005(2) 0.003(2) 0.004(3) C25 0.057(3) 0.046(3) 0.039(2) 0.009(2) 0.004(2) -0.005(2) C26 0.045(2) 0.052(3) 0.048(3) 0.000(2) 0.004(2) -0.008(2) C27 0.049(2) 0.038(2) 0.046(2) 0.003(2) 0.018(2) -0.002(2) C28 0.058(3) 0.060(3) 0.036(2) 0.010(2) 0.008(2) -0.010(2) C29 0.052(3) 0.057(3) 0.037(2) 0.001(2) 0.002(2) -0.014(2) C30 0.063(4) 0.075(4) 0.125(6) 0.004(4) 0.018(4) -0.028(3) C31 0.085(4) 0.071(4) 0.095(4) 0.033(4) 0.042(3) -0.005(3) C32 0.057(3) 0.038(2) 0.058(3) 0.006(2) -0.008(2) -0.006(2) C33 0.049(3) 0.051(3) 0.054(3) 0.001(2) -0.017(2) -0.009(2) C34 0.038(2) 0.052(3) 0.045(2) 0.008(2) 0.0014(19) 0.002(2) C35 0.053(3) 0.039(2) 0.051(3) 0.005(2) -0.002(2) 0.002(2) C36 0.055(3) 0.045(3) 0.040(2) 0.002(2) -0.007(2) 0.000(2) C37 0.066(3) 0.086(4) 0.057(3) 0.015(3) -0.018(3) 0.009(3) C38 0.102(5) 0.068(4) 0.103(5) 0.034(4) -0.029(4) 0.017(4)