#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060150.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_4060150 _journal_name_full 'Organometallics' _journal_year 2005 _chemical_formula_sum 'C26 H20 Mo O5 P2' _chemical_formula_weight 570.30 _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 10.3259(5) _cell_length_b 18.5007(8) _cell_length_c 13.7720(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.500(3) _cell_angle_gamma 90.00 _cell_volume 2547.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2301 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.14 _exptl_crystal_description Prism _exptl_crystal_colour clear _exptl_crystal_size_max 0.265 _exptl_crystal_size_mid 0.229 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8416 _exptl_absorpt_correction_T_max 0.9543 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 180(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56946 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 33.17 _reflns_number_total 9720 _reflns_number_gt 7320 _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^)+(0.0315P)^2^+0.8883P] 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 9720 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Mo1 Mo 0.308367(13) 0.132174(7) 0.813870(10) 0.02625(4) Uani 1 1 d . . . P1 P 0.21538(4) 0.01639(2) 0.74616(3) 0.02801(8) Uani 1 1 d . . . P2 P 0.50926(4) 0.07031(2) 0.78155(3) 0.02706(8) Uani 1 1 d . . . O1 O 0.09760(12) 0.00669(6) 0.64359(9) 0.0373(3) Uani 1 1 d . . . O2 O 0.47682(17) 0.27109(9) 0.88919(19) 0.0852(7) Uani 1 1 d . . . O3 O 0.37255(19) 0.07419(10) 1.03653(11) 0.0658(5) Uani 1 1 d . . . O4 O 0.06243(16) 0.20366(11) 0.87080(13) 0.0679(5) Uani 1 1 d . . . O5 O 0.1799(2) 0.20022(11) 0.60079(12) 0.0740(5) Uani 1 1 d . . . C1 C 0.2694(2) -0.08643(11) 0.89901(15) 0.0455(4) Uani 1 1 d . . . H1 H 0.3607 -0.0773 0.9015 0.055 Uiso 1 1 calc R . . C2 C 0.2374(3) -0.13561(12) 0.96513(17) 0.0571(6) Uani 1 1 d . . . H2 H 0.3066 -0.1597 1.0127 0.069 Uiso 1 1 calc R . . C3 C 0.1082(3) -0.14939(16) 0.9620(2) 0.0781(8) Uani 1 1 d . . . H3 H 0.0863 -0.1821 1.0086 0.094 Uiso 1 1 calc R . . C4 C 0.0077(3) -0.1159(2) 0.8910(3) 0.0966(11) Uani 1 1 d . . . H4 H -0.0831 -0.1270 0.8879 0.116 Uiso 1 1 calc R . . C5 C 0.0380(2) -0.06607(15) 0.8239(2) 0.0659(7) Uani 1 1 d . . . H5 H -0.0314 -0.0433 0.7751 0.079 Uiso 1 1 calc R . . C6 C 0.17107(17) -0.05037(9) 0.82957(13) 0.0350(3) Uani 1 1 d . . . C7 C 0.1123(2) -0.06066(10) 0.59147(16) 0.0467(5) Uani 1 1 d . . . H7A H 0.0934 -0.0515 0.5184 0.056 Uiso 1 1 calc R . . H7B H 0.0468 -0.0966 0.6031 0.056 Uiso 1 1 calc R . . C8 C 0.25498(19) -0.09105(9) 0.62933(14) 0.0400(4) Uani 1 1 d . . . H8A H 0.2538 -0.1364 0.6672 0.048 Uiso 1 1 calc R . . H8B H 0.2946 -0.1011 0.5723 0.048 Uiso 1 1 calc R . . C9 C 0.33424(16) -0.03373(8) 0.69645(12) 0.0297(3) Uani 1 1 d . . . C10 C 0.46179(16) -0.01417(8) 0.70967(11) 0.0282(3) Uani 1 1 d . . . C11 C 0.56017(16) -0.05845(8) 0.67307(12) 0.0298(3) Uani 1 1 d . . . C12 C 0.5887(2) -0.12781(9) 0.71161(14) 0.0402(4) Uani 1 1 d . . . H12 H 0.5472 -0.1452 0.7614 0.048 Uiso 1 1 calc R . . C13 C 0.6772(2) -0.17180(11) 0.67788(16) 0.0482(5) Uani 1 1 d . . . H13 H 0.6967 -0.2189 0.7051 0.058 Uiso 1 1 calc R . . C14 C 0.7367(2) -0.14745(11) 0.60505(16) 0.0471(5) Uani 1 1 d . . . H14 H 0.7966 -0.1778 0.5816 0.056 Uiso 1 1 calc R . . C15 C 0.7091(2) -0.07892(11) 0.56630(15) 0.0433(4) Uani 1 1 d . . . H15 H 0.7501 -0.0622 0.5160 0.052 Uiso 1 1 calc R . . C16 C 0.62191(17) -0.03414(9) 0.60012(13) 0.0349(3) Uani 1 1 d . . . H16 H 0.6043 0.0132 0.5735 0.042 Uiso 1 1 calc R . . C17 C 0.62192(16) 0.11551(8) 0.71832(12) 0.0303(3) Uani 1 1 d . . . C18 C 0.5715(2) 0.16410(10) 0.64220(14) 0.0412(4) Uani 1 1 d . . . H18 H 0.4793 0.1764 0.6259 0.049 Uiso 1 1 calc R . . C19 C 0.6560(3) 0.19512(12) 0.58927(17) 0.0531(5) Uani 1 1 d . . . H19 H 0.6210 0.2284 0.5368 0.064 Uiso 1 1 calc R . . C20 C 0.7898(2) 0.17783(12) 0.61249(17) 0.0521(5) Uani 1 1 d . . . H20 H 0.8468 0.1990 0.5759 0.063 Uiso 1 1 calc R . . C21 C 0.8408(2) 0.12995(12) 0.68847(17) 0.0508(5) Uani 1 1 d . . . H21 H 0.9331 0.1179 0.7042 0.061 Uiso 1 1 calc R . . C22 C 0.75788(18) 0.09905(11) 0.74247(15) 0.0413(4) Uani 1 1 d . . . H22 H 0.7940 0.0667 0.7959 0.050 Uiso 1 1 calc R . . C23 C 0.41618(18) 0.22034(10) 0.86167(17) 0.0451(4) Uani 1 1 d . . . C24 C 0.3532(2) 0.09329(10) 0.95562(14) 0.0403(4) Uani 1 1 d . . . C25 C 0.15010(18) 0.17627(10) 0.84835(13) 0.0393(4) Uani 1 1 d . . . C26 C 0.2338(2) 0.17513(10) 0.67512(14) 0.0413(4) Uani 1 1 d . . . H1P H 0.598(2) 0.0485(11) 0.8583(14) 0.038(5) 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 Mo1 0.02642(6) 0.02340(6) 0.02899(6) -0.00237(5) 0.00705(4) 0.00041(5) P1 0.02536(18) 0.02547(17) 0.03263(19) -0.00159(14) 0.00622(15) -0.00012(14) P2 0.02629(18) 0.02495(17) 0.02898(18) -0.00001(14) 0.00512(14) 0.00111(14) O1 0.0333(6) 0.0325(6) 0.0402(6) -0.0046(5) -0.0020(5) 0.0025(5) O2 0.0471(9) 0.0396(8) 0.154(2) -0.0224(10) -0.0019(11) -0.0097(7) O3 0.0813(12) 0.0765(11) 0.0353(7) 0.0107(7) 0.0066(8) -0.0027(9) O4 0.0451(8) 0.0930(13) 0.0680(10) -0.0313(9) 0.0187(8) 0.0145(8) O5 0.0811(13) 0.0903(13) 0.0481(9) 0.0280(9) 0.0112(9) 0.0278(11) C1 0.0419(10) 0.0455(10) 0.0465(10) 0.0076(8) 0.0064(8) -0.0056(8) C2 0.0726(16) 0.0462(11) 0.0471(11) 0.0093(9) 0.0048(10) -0.0118(11) C3 0.087(2) 0.0748(17) 0.0766(18) 0.0261(14) 0.0286(16) -0.0238(16) C4 0.0622(18) 0.114(3) 0.124(3) 0.039(2) 0.0434(19) -0.0226(18) C5 0.0385(11) 0.0745(16) 0.0869(18) 0.0231(14) 0.0200(11) -0.0051(11) C6 0.0332(8) 0.0302(7) 0.0428(9) 0.0001(6) 0.0121(7) -0.0040(6) C7 0.0438(10) 0.0357(9) 0.0515(11) -0.0122(8) -0.0052(8) 0.0020(8) C8 0.0395(9) 0.0322(8) 0.0467(10) -0.0134(7) 0.0079(8) -0.0020(7) C9 0.0320(7) 0.0240(6) 0.0333(7) -0.0024(5) 0.0086(6) 0.0006(5) C10 0.0309(7) 0.0236(6) 0.0307(7) 0.0002(5) 0.0088(6) 0.0018(5) C11 0.0290(7) 0.0271(7) 0.0329(7) -0.0026(6) 0.0069(6) 0.0035(5) C12 0.0485(10) 0.0310(8) 0.0444(9) 0.0043(7) 0.0180(8) 0.0087(7) C13 0.0516(12) 0.0356(9) 0.0572(11) 0.0038(8) 0.0131(9) 0.0165(8) C14 0.0390(10) 0.0487(11) 0.0544(11) -0.0094(8) 0.0132(8) 0.0145(8) C15 0.0414(10) 0.0496(10) 0.0440(10) -0.0033(8) 0.0199(8) 0.0031(8) C16 0.0361(8) 0.0330(8) 0.0368(8) 0.0001(6) 0.0116(7) 0.0026(6) C17 0.0286(7) 0.0273(7) 0.0351(8) -0.0047(5) 0.0085(6) -0.0020(5) C18 0.0429(10) 0.0388(9) 0.0454(10) 0.0059(7) 0.0178(8) 0.0051(8) C19 0.0678(14) 0.0465(11) 0.0530(12) 0.0087(9) 0.0305(11) 0.0021(10) C20 0.0587(13) 0.0517(11) 0.0562(12) -0.0160(10) 0.0334(11) -0.0183(10) C21 0.0324(9) 0.0648(13) 0.0581(12) -0.0215(10) 0.0165(8) -0.0128(9) C22 0.0282(8) 0.0487(10) 0.0450(10) -0.0054(8) 0.0053(7) -0.0013(7) C23 0.0314(8) 0.0327(8) 0.0675(13) -0.0067(8) 0.0054(8) 0.0026(7) C24 0.0425(10) 0.0410(9) 0.0359(9) -0.0018(7) 0.0069(7) -0.0016(7) C25 0.0337(8) 0.0459(9) 0.0374(8) -0.0127(7) 0.0071(7) 0.0009(7) C26 0.0435(10) 0.0424(9) 0.0404(9) 0.0044(7) 0.0146(8) 0.0082(8)