#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000035.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_4000035 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _chemical_formula_sum 'C12 H22 Cr Gd N8 O6' _chemical_formula_weight 583.63 _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 7.7102(2) _cell_length_b 9.4112(2) _cell_length_c 16.2819(4) _cell_angle_alpha 94.2590(10) _cell_angle_beta 99.9890(10) _cell_angle_gamma 100.990(2) _cell_volume 1135.14(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 572 _exptl_absorpt_coefficient_mu 3.415 _exptl_absorpt_correction_type 'SORTAV' _exptl_absorpt_correction_T_min 0.341 _exptl_absorpt_correction_T_max 0.436 _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 'NONIUS Kappa CCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 0.71 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22268 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 27.90 _reflns_number_total 5382 _reflns_number_gt 5046 _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^)+(0.0682P)^2^+0.8583P] 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 5382 _refine_ls_number_parameters 277 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.000 _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 Gd Gd 0.46415(2) 0.208306(18) 0.244467(10) 0.01960(8) Uani 1 1 d . . . Cr Cr 0.85207(8) 0.75346(6) 0.22961(4) 0.01948(13) Uani 1 1 d . . . C6 C 0.6431(6) 0.5823(4) 0.2339(3) 0.0278(8) Uani 1 1 d . . . O4 O 0.7841(4) 0.2922(4) 0.2985(3) 0.0435(9) Uani 1 1 d D . . O5 O 0.2680(5) 0.3189(4) 0.3182(2) 0.0348(7) Uani 1 1 d D . . C4 C 1.0779(6) 0.9145(5) 0.2296(3) 0.0297(9) Uani 1 1 d . . . C3 C 0.6875(6) 0.9032(5) 0.2338(3) 0.0282(8) Uani 1 1 d . . . O1 O 0.5176(5) 0.1677(4) 0.3858(2) 0.0448(9) Uani 1 1 d . . . O3 O 0.2294(5) 0.2608(4) 0.1380(2) 0.0419(8) Uani 1 1 d . . . O2 O 0.5826(5) 0.2133(4) 0.1226(2) 0.0416(8) Uani 1 1 d . . . C5 C 1.0022(6) 0.5915(5) 0.2247(3) 0.0292(9) Uani 1 1 d . . . C1 C 0.7907(6) 0.7308(5) 0.1002(3) 0.0317(9) Uani 1 1 d . . . C2 C 0.9147(7) 0.7809(6) 0.3597(3) 0.0374(10) Uani 1 1 d . . . C10 C 0.6284(7) 0.2869(6) 0.0679(3) 0.0382(10) Uani 1 1 d . . . H10A H 0.6054 0.3804 0.0684 0.046 Uiso 1 1 calc R . . N5 N 1.0672(7) 0.4933(5) 0.2219(4) 0.0526(12) Uani 1 1 d . . . N8 N 0.7073(6) 0.2425(5) 0.0089(3) 0.0410(9) Uani 1 1 d . . . N1 N 0.7616(7) 0.7192(7) 0.0287(3) 0.0546(13) Uani 1 1 d . . . C7 C 0.4971(8) 0.1735(7) 0.4593(3) 0.0452(12) Uani 1 1 d . . . H7A H 0.4115 0.0995 0.4726 0.054 Uiso 1 1 calc R . . N7 N 0.5829(7) 0.2724(7) 0.5198(3) 0.0587(14) Uani 1 1 d . . . N2 N 0.9493(9) 0.8010(7) 0.4310(3) 0.0687(16) Uani 1 1 d . . . C11 C 0.7462(11) 0.3320(9) -0.0580(4) 0.072(2) Uani 1 1 d . . . H11A H 0.7114 0.4235 -0.0482 0.107 Uiso 1 1 calc R . . H11B H 0.6800 0.2824 -0.1110 0.107 Uiso 1 1 calc R . . H11C H 0.8728 0.3489 -0.0585 0.107 Uiso 1 1 calc R . . C12 C 0.7509(12) 0.0987(8) 0.0047(5) 0.073(2) Uani 1 1 d . . . H12A H 0.7187 0.0508 0.0516 0.109 Uiso 1 1 calc R . . H12B H 0.8777 0.1083 0.0063 0.109 Uiso 1 1 calc R . . H12C H 0.6852 0.0422 -0.0466 0.109 Uiso 1 1 calc R . . C8 C 0.5605(14) 0.2627(14) 0.6065(4) 0.103(4) Uani 1 1 d . . . H8A H 0.4725 0.1769 0.6092 0.155 Uiso 1 1 calc R . . H8B H 0.5209 0.3472 0.6266 0.155 Uiso 1 1 calc R . . H8C H 0.6734 0.2577 0.6407 0.155 Uiso 1 1 calc R . . C9 C 0.7124(12) 0.3974(10) 0.5037(5) 0.085(3) Uani 1 1 d . . . H9A H 0.7149 0.3923 0.4448 0.128 Uiso 1 1 calc R . . H9B H 0.8299 0.3961 0.5347 0.128 Uiso 1 1 calc R . . H9C H 0.6774 0.4857 0.5211 0.128 Uiso 1 1 calc R . . O6 O 0.9817(5) 0.8458(5) 0.6044(2) 0.0421(8) Uani 1 1 d D . . N6 N 0.5472(5) 0.4767(4) 0.2392(3) 0.0363(9) Uani 1 1 d . . . N4 N 1.2031(5) 1.0011(4) 0.2328(3) 0.0354(9) Uani 1 1 d . . . N3 N 0.5975(6) 0.9871(4) 0.2369(3) 0.0356(8) Uani 1 1 d . . . H600 H 0.969(9) 0.834(7) 0.555(4) 0.051(19) Uiso 1 1 d D . . H401 H 0.843(9) 0.232(7) 0.318(4) 0.056(19) Uiso 1 1 d D . . H601 H 1.000(13) 0.927(9) 0.634(5) 0.10(3) Uiso 1 1 d D . . H400 H 0.862(9) 0.365(7) 0.283(4) 0.057(19) Uiso 1 1 d D . . H501 H 0.214(9) 0.376(7) 0.290(4) 0.050(18) Uiso 1 1 d D . . H500 H 0.198(6) 0.272(5) 0.337(3) 0.013(11) Uiso 1 1 d D . . 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 Gd 0.01897(11) 0.01757(12) 0.02304(12) 0.00154(7) 0.00830(7) 0.00208(8) Cr 0.0198(3) 0.0164(3) 0.0230(3) 0.0019(2) 0.0076(2) 0.0024(2) C6 0.029(2) 0.0196(19) 0.036(2) 0.0020(15) 0.0101(16) 0.0044(16) O4 0.0238(15) 0.042(2) 0.063(2) 0.0221(18) 0.0038(15) -0.0003(15) O5 0.0341(17) 0.0368(18) 0.0424(19) 0.0104(14) 0.0210(15) 0.0145(15) C4 0.029(2) 0.025(2) 0.035(2) 0.0027(16) 0.0100(17) 0.0016(17) C3 0.031(2) 0.023(2) 0.033(2) 0.0030(15) 0.0116(16) 0.0050(17) O1 0.058(2) 0.055(2) 0.0261(16) 0.0059(15) 0.0073(15) 0.0220(19) O3 0.0386(18) 0.059(2) 0.0294(16) 0.0102(15) 0.0059(14) 0.0117(17) O2 0.053(2) 0.045(2) 0.0358(18) 0.0099(15) 0.0275(16) 0.0154(17) C5 0.0272(19) 0.027(2) 0.038(2) 0.0101(17) 0.0127(17) 0.0073(17) C1 0.033(2) 0.035(2) 0.031(2) 0.0042(17) 0.0096(17) 0.0124(19) C2 0.044(3) 0.039(3) 0.031(2) 0.0039(18) 0.0097(19) 0.008(2) C10 0.043(3) 0.042(3) 0.034(2) 0.0042(19) 0.018(2) 0.010(2) N5 0.050(3) 0.043(3) 0.080(4) 0.022(2) 0.029(2) 0.025(2) N8 0.043(2) 0.051(3) 0.033(2) 0.0009(18) 0.0232(17) 0.009(2) N1 0.064(3) 0.077(4) 0.028(2) 0.005(2) 0.009(2) 0.025(3) C7 0.051(3) 0.058(3) 0.033(2) 0.013(2) 0.009(2) 0.023(3) N7 0.053(3) 0.095(4) 0.032(2) -0.009(2) 0.010(2) 0.031(3) N2 0.090(4) 0.084(4) 0.029(2) -0.001(2) 0.006(2) 0.017(3) C11 0.089(5) 0.079(5) 0.057(4) 0.021(3) 0.043(4) 0.011(4) C12 0.090(5) 0.051(4) 0.090(5) -0.008(3) 0.053(4) 0.020(4) C8 0.100(7) 0.177(11) 0.038(4) -0.008(5) 0.028(4) 0.038(7) C9 0.080(5) 0.084(6) 0.080(5) -0.028(4) 0.016(4) 0.003(5) O6 0.050(2) 0.049(2) 0.0283(18) 0.0040(15) 0.0109(15) 0.0076(18) N6 0.0316(19) 0.0267(19) 0.052(2) 0.0010(16) 0.0184(17) 0.0009(16) N4 0.0285(18) 0.0278(19) 0.048(2) 0.0048(16) 0.0094(16) -0.0002(16) N3 0.040(2) 0.029(2) 0.044(2) 0.0050(16) 0.0182(17) 0.0137(17)