#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100959.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_1100959 _chemical_formula_sum 'C24 H40 Fe P2' _chemical_formula_weight 446.35 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4702(5) _cell_length_b 13.8619(8) _cell_length_c 18.8839(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.9160(10) _cell_angle_gamma 90.00 _cell_volume 2455.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.751 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8060 _exptl_absorpt_correction_T_max 0.9634 _diffrn_ambient_temperature 173(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 'Bruker 1K CCD area detector' _diffrn_measurement_method '0.3 deg. omega scans' _diffrn_standards_decay_% ? _diffrn_reflns_number 17030 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.33 _reflns_number_total 6040 _reflns_number_gt 3779 _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^)+(0.0677P)^2^+0.8638P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6040 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1362 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.317 _refine_ls_shift/su_mean 0.027 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 Fe1 Fe 0.01005(5) 0.48443(3) 0.26512(2) 0.01923(13) Uani 1 1 d . . . P1 P 0.15789(9) 0.44315(6) 0.18616(4) 0.0245(2) Uani 1 1 d . . . P2 P -0.13198(9) 0.53077(6) 0.34492(4) 0.0243(2) Uani 1 1 d . . . C1 C 0.1815(5) 0.3142(3) 0.1740(2) 0.0382(9) Uani 1 1 d . . . C2 C 0.3434(4) 0.4813(4) 0.2087(3) 0.0464(11) Uani 1 1 d . . . C3 C 0.1172(5) 0.4848(3) 0.0940(2) 0.0402(10) Uani 1 1 d . . . C4 C -0.2908(4) 0.6020(4) 0.3136(2) 0.0568(12) Uani 1 1 d . . . H4A H -0.3420 0.6166 0.3540 0.085 Uiso 1 1 calc R . . H4B H -0.3531 0.5652 0.2776 0.085 Uiso 1 1 calc R . . H4C H -0.2625 0.6623 0.2925 0.085 Uiso 1 1 calc R . . C5 C -0.0492(5) 0.6093(4) 0.4157(3) 0.0689(15) Uani 1 1 d . . . H5A H -0.1188 0.6256 0.4477 0.103 Uiso 1 1 calc R . . H5B H -0.0163 0.6685 0.3948 0.103 Uiso 1 1 calc R . . H5C H 0.0323 0.5761 0.4429 0.103 Uiso 1 1 calc R . . C6 C -0.2080(6) 0.4385(3) 0.3953(3) 0.0691(15) Uani 1 1 d . . . H6A H -0.2670 0.4686 0.4279 0.104 Uiso 1 1 calc R . . H6B H -0.1314 0.4014 0.4230 0.104 Uiso 1 1 calc R . . H6C H -0.2671 0.3953 0.3624 0.104 Uiso 1 1 calc R . . C7 C 0.1387(3) 0.4137(2) 0.34330(16) 0.0223(7) Uani 1 1 d . . . C8 C 0.1125(3) 0.3156(2) 0.35719(16) 0.0228(7) Uani 1 1 d . . . C9 C 0.1969(4) 0.2645(3) 0.41012(17) 0.0274(7) Uani 1 1 d . . . C10 C 0.3123(4) 0.3061(3) 0.45223(17) 0.0292(8) Uani 1 1 d . . . C11 C 0.3392(4) 0.4018(3) 0.43982(17) 0.0287(8) Uani 1 1 d . . . C12 C 0.2568(3) 0.4558(2) 0.38730(17) 0.0258(7) Uani 1 1 d . . . C13 C -0.0101(4) 0.2644(2) 0.31346(18) 0.0309(8) Uani 1 1 d . . . H13A H 0.0158(6) 0.2448(5) 0.2741(9) 0.046 Uiso 1 1 calc R . . H13B H -0.0807(16) 0.3034(8) 0.3044(3) 0.046 Uiso 1 1 calc R . . H13C H -0.0352(7) 0.2158(11) 0.3370(5) 0.046 Uiso 1 1 calc R . . C14 C 0.4027(4) 0.2495(3) 0.51021(18) 0.0445(11) Uani 1 1 d . . . H14A H 0.3473(14) 0.2182(8) 0.5358(6) 0.067 Uiso 1 1 calc R . . H14B H 0.4573(14) 0.2892(10) 0.5378(7) 0.067 Uiso 1 1 calc R . . H14C H 0.4559(14) 0.2084(10) 0.4906(5) 0.067 Uiso 1 1 calc R . . C15 C 0.2937(5) 0.5608(3) 0.3774(2) 0.0355(9) Uani 1 1 d . . . C16 C -0.1213(3) 0.5470(2) 0.18501(16) 0.0227(7) Uani 1 1 d . . . C17 C -0.0962(3) 0.6422(2) 0.16418(17) 0.0260(7) Uani 1 1 d . . . C18 C -0.1765(4) 0.6834(3) 0.10454(18) 0.0301(8) Uani 1 1 d . . . C19 C -0.2865(4) 0.6346(3) 0.06437(17) 0.0305(8) Uani 1 1 d . . . C20 C -0.3142(4) 0.5415(3) 0.08521(18) 0.0301(8) Uani 1 1 d . . . C21 C -0.2344(3) 0.4974(2) 0.14390(17) 0.0253(7) Uani 1 1 d . . . C22 C 0.0220(4) 0.7000(3) 0.20644(19) 0.0354(9) Uani 1 1 d . . . H22A H 0.0611(10) 0.7354(8) 0.1784(6) 0.053 Uiso 1 1 calc R . . H22B H 0.0832(14) 0.6620(8) 0.2280(5) 0.053 Uiso 1 1 calc R . . H22C H -0.0123(8) 0.7349(8) 0.2366(7) 0.053 Uiso 1 1 calc R . . C23 C -0.3754(5) 0.6825(4) 0.0018(2) 0.0418(10) Uani 1 1 d . . . C24 C -0.2674(4) 0.3951(3) 0.1631(2) 0.0355(9) Uani 1 1 d . . . H20 H -0.381(3) 0.506(2) 0.0600(17) 0.022(9) Uiso 1 1 d . . . H9 H 0.178(3) 0.199(2) 0.4182(16) 0.019(8) Uiso 1 1 d . . . H3C H 0.026(5) 0.466(3) 0.074(2) 0.056(14) Uiso 1 1 d . . . H11 H 0.414(4) 0.432(2) 0.4658(18) 0.030(9) Uiso 1 1 d . . . H24B H -0.189(4) 0.352(2) 0.1617(17) 0.030(9) Uiso 1 1 d . . . H18 H -0.150(3) 0.744(2) 0.0930(16) 0.023(9) Uiso 1 1 d . . . H15C H 0.289(5) 0.596(3) 0.417(3) 0.069(15) Uiso 1 1 d . . . H24A H -0.340(4) 0.365(3) 0.136(2) 0.055(13) Uiso 1 1 d . . . H15B H 0.224(5) 0.596(3) 0.341(2) 0.064(13) Uiso 1 1 d . . . H2A H 0.091(4) 0.289(3) 0.156(2) 0.049(12) Uiso 1 1 d . . . H1A H 0.215(4) 0.282(3) 0.221(2) 0.039(10) Uiso 1 1 d . . . H15A H 0.383(5) 0.567(4) 0.362(3) 0.082(17) Uiso 1 1 d . . . H3B H 0.187(4) 0.461(3) 0.068(2) 0.044(11) Uiso 1 1 d . . . H2C H 0.398(4) 0.455(3) 0.174(2) 0.044(11) Uiso 1 1 d . . . H2B H 0.342(4) 0.544(3) 0.212(2) 0.039(12) Uiso 1 1 d . . . H3A H 0.117(4) 0.562(3) 0.092(2) 0.053(12) Uiso 1 1 d . . . H2A H 0.387(5) 0.455(3) 0.257(2) 0.060(14) Uiso 1 1 d . . . H23C H -0.409(4) 0.638(3) -0.035(2) 0.054(13) Uiso 1 1 d . . . H23B H -0.314(5) 0.725(4) -0.019(2) 0.076(16) Uiso 1 1 d . . . H24C H -0.302(4) 0.389(3) 0.209(2) 0.049(12) Uiso 1 1 d . . . H23A H -0.456(5) 0.706(4) 0.019(3) 0.078(16) Uiso 1 1 d . . . H1C H 0.250(5) 0.303(3) 0.141(2) 0.065(14) Uiso 1 1 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 Fe1 0.0196(2) 0.0184(2) 0.0190(2) 0.00011(18) 0.00033(16) 0.00045(18) P1 0.0259(4) 0.0241(5) 0.0238(4) 0.0005(3) 0.0045(3) 0.0037(4) P2 0.0244(4) 0.0266(5) 0.0219(4) -0.0017(3) 0.0033(3) 0.0005(4) C1 0.053(3) 0.031(2) 0.032(2) -0.0005(17) 0.0113(19) 0.0119(19) C2 0.028(2) 0.063(3) 0.050(3) -0.009(2) 0.0130(19) -0.007(2) C3 0.049(3) 0.049(3) 0.0252(19) 0.0076(18) 0.0134(18) 0.019(2) C4 0.046(3) 0.077(3) 0.049(3) -0.002(2) 0.012(2) 0.023(2) C5 0.054(3) 0.086(4) 0.069(3) -0.048(3) 0.017(2) -0.015(3) C6 0.092(4) 0.049(3) 0.076(3) 0.017(3) 0.048(3) 0.006(3) C7 0.0224(16) 0.0249(17) 0.0195(15) 0.0012(13) 0.0030(12) 0.0015(13) C8 0.0229(16) 0.0249(17) 0.0213(15) 0.0001(13) 0.0061(13) -0.0003(13) C9 0.0334(19) 0.0235(18) 0.0275(17) 0.0044(14) 0.0122(15) 0.0052(15) C10 0.0293(18) 0.038(2) 0.0210(16) 0.0035(14) 0.0061(14) 0.0129(15) C11 0.0235(18) 0.039(2) 0.0226(17) -0.0066(15) -0.0007(14) 0.0005(15) C12 0.0255(17) 0.0257(18) 0.0257(16) -0.0054(13) 0.0016(14) 0.0000(13) C13 0.0314(19) 0.0260(18) 0.0357(19) 0.0028(15) 0.0064(15) -0.0035(15) C14 0.052(3) 0.050(3) 0.0293(19) 0.0044(18) -0.0010(18) 0.018(2) C15 0.035(2) 0.030(2) 0.039(2) -0.0043(18) 0.0002(18) -0.0072(17) C16 0.0217(16) 0.0262(17) 0.0207(15) 0.0006(13) 0.0051(13) 0.0056(13) C17 0.0263(17) 0.0262(18) 0.0262(17) -0.0001(14) 0.0059(14) 0.0044(14) C18 0.036(2) 0.0257(19) 0.0310(19) 0.0063(15) 0.0135(16) 0.0099(16) C19 0.0305(18) 0.040(2) 0.0207(16) 0.0029(15) 0.0031(14) 0.0141(16) C20 0.0245(18) 0.040(2) 0.0248(17) -0.0059(15) -0.0022(14) 0.0029(15) C21 0.0247(17) 0.0285(19) 0.0229(16) -0.0002(13) 0.0040(13) 0.0017(13) C22 0.040(2) 0.029(2) 0.037(2) 0.0031(16) 0.0062(16) -0.0022(16) C23 0.044(3) 0.051(3) 0.029(2) 0.0103(19) 0.0020(19) 0.016(2) C24 0.032(2) 0.032(2) 0.041(2) -0.0025(17) -0.0036(18) -0.0044(17)