#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/47/2004784.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2004784 loop_ _publ_author_name 'Champness, N. R.' 'Hopkins, A. M.' 'Reid, G.' _publ_section_title ; trans-[Mo(CO)~4~{P(OMe)~3~}~2~] ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 797 _journal_page_last 799 _journal_paper_doi 10.1107/S010827019501479X _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Mo (C3 H9 O3 P1)2 (C1 O1)4]' _chemical_formula_moiety 'C10 H18 Mo O10 P2' _chemical_formula_structural '[Mo(CO)~4~{P(OMe)~3~}~2~]' _chemical_formula_sum 'C10 H18 Mo O10 P2' _chemical_formula_weight 456.13 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 104.05(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.992(3) _cell_length_b 13.356(5) _cell_length_c 9.521(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 150.0 _cell_measurement_theta_max 25.0 _cell_measurement_theta_min 24.35 _cell_volume 862.5(6) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1992)' _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution 'direct methods SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 423.2 _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 1735 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.50 _diffrn_standards_decay_% 0.61 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.989 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.868 _exptl_absorpt_correction_type 'empirical via \y scans (TEXSAN; Molecular Structure Corporation, 1992)' _exptl_absorpt_process_details psi-scan _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.756 _exptl_crystal_description block _exptl_crystal_F_000 460 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.64 _refine_diff_density_min '-1.18 (within 1\%A of Mo)' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 2.870 _refine_ls_goodness_of_fit_obs 3.083 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 106 _refine_ls_number_reflns 1413 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_obs 0.0290 _refine_ls_shift/esd_max 0.006 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/\s^2^(F)' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0365 _refine_ls_wR_factor_obs 0.0363 _reflns_number_observed 1413 _reflns_number_total 1603 _reflns_observed_criterion I>=3\s(I) _[local]_cod_data_source_file mu1224.cif _[local]_cod_data_source_block mopome _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 1/\s^2^(F)' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/\s^2^(F)'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 862.5(5) _cod_database_code 2004784 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' 1/2-x,1/2+y,1/2-z ' -x, -y, -z' 1/2+x,1/2-y,1/2+z loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo 0.0157(2) 0.0149(2) 0.0131(2) -0.00030(10) 0.0016(2) -0.00010(10) P(1) 0.0161(4) 0.0163(4) 0.0153(4) -0.0011(3) 0.0017(3) 0.0003(3) O(1) 0.0380(10) 0.0290(10) 0.0300(10) -0.0070(10) 0.0130(10) 0.0050(10) O(2) 0.0250(10) 0.0320(10) 0.039(2) 0.0100(10) 0.0070(10) 0.0030(10) O(3) 0.0150(10) 0.0270(10) 0.0190(10) 0.0009(9) 0.0005(9) 0.0028(10) O(4) 0.0180(10) 0.0260(10) 0.0160(10) -0.0042(10) 0.0041(9) -0.0049(9) O(5) 0.0230(10) 0.0160(10) 0.0250(10) -0.0018(9) 0.0023(10) 0.0008(10) C(1) 0.020(2) 0.024(2) 0.013(2) -0.0010(10) 0.0040(10) -0.0030(10) C(2) 0.028(2) 0.018(2) 0.015(2) -0.0040(10) 0.0020(10) 0.0010(10) C(3) 0.015(2) 0.033(2) 0.026(2) -0.0010(10) 0.0020(10) -0.002(2) C(4) 0.029(2) 0.029(2) 0.019(2) -0.0030(10) 0.0070(10) -0.0070(10) C(5) 0.038(2) 0.018(2) 0.025(2) 0.004(2) 0.006(2) 0.0030(10) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Mo 0 0 0 .01490(10) Uij P(1) .12420(10) .08862(6) .22614(9) .0162(2) Uij O(1) .1450(4) .1682(2) -0.1878(3) .0317(7) Uij O(2) .4035(4) -0.1162(2) .0196(3) .0326(7) Uij O(3) .3162(3) .0490(2) .3418(2) .0211(6) Uij O(4) -.0307(3) .0856(2) .3246(2) .0200(6) Uij O(5) .1896(3) .2043(2) .2274(2) .0221(6) Uij C(1) .0936(5) .1080(2) -0.1198(3) .0191(8) Uij C(2) .2587(5) -.0742(2) .0148(3) .0209(9) Uij C(3) .5099(5) .0590(3) .3135(4) .0256(9) Uij C(4) .0116(5) .1333(3) .4665(4) .0254(9) Uij C(5) .0547(5) .2776(2) .1466(4) .0277(10) Uij H(1) .5392 .1274 .3013 .0308 Uiso H(2) .5152 .0231 .2274 .0308 Uiso H(3) .6087 .0320 .3922 .0308 Uiso H(4) .1260 .1044 .5280 .0325 Uiso H(5) -0.0972 .1246 .5097 .0325 Uiso H(6) .0333 .2034 .4574 .0325 Uiso H(7) -0.0633 .2785 .1812 .0343 Uiso H(8) .1126 .3419 .1583 .0343 Uiso H(9) .0204 .2601 .0467 .0343 Uiso loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 'International Tables' H 0.000 0.000 'International Tables' Mo -1.683 0.686 'International Tables' O 0.011 0.006 'International Tables' P 0.102 0.094 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -6 1 -3 -3 0 -1 -6 -1 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P(1) Mo P(1) . 3_555 180.0 no P(1) Mo C(1) . . 93.30(9) yes P(1) Mo C(1) . 3_555 86.70(9) no P(1) Mo C(2) . . 93.12(9) yes P(1) Mo C(2) . 3_555 86.88(9) no P(1) Mo C(1) 3_555 . 86.70(9) no P(1) Mo C(1) 3_555 3_555 93.30(9) no P(1) Mo C(2) 3_555 . 86.88(9) no P(1) Mo C(2) 3_555 3_555 93.12(9) no C(1) Mo C(1) . 3_555 180.0 no C(1) Mo C(2) . . 89.00(10) yes C(1) Mo C(2) . 3_555 91.00(10) no C(1) Mo C(2) 3_555 . 91.00(10) no C(1) Mo C(2) 3_555 3_555 89.00(10) no C(2) Mo C(2) . 3_555 180.0 no Mo P(1) O(3) . . 120.52(9) yes Mo P(1) O(4) . . 111.16(9) yes Mo P(1) O(5) . . 121.02(9) yes O(3) P(1) O(4) . . 99.30(10) yes O(3) P(1) O(5) . . 97.00(10) yes O(4) P(1) O(5) . . 104.60(10) yes P(1) O(3) C(3) . . 120.3(2) yes P(1) O(4) C(4) . . 121.3(2) yes P(1) O(5) C(5) . . 119.9(2) yes Mo C(1) O(1) . . 179.6(3) yes Mo C(2) O(2) . . 178.2(3) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo P(1) . 2.4256(8) yes Mo P(1) 3_555 2.4256(8) no Mo C(1) . 2.041(3) yes Mo C(1) 3_555 2.041(3) no Mo C(2) . 2.037(4) yes Mo C(2) 3_555 2.037(4) no P(1) O(3) . 1.606(2) yes P(1) O(4) . 1.595(2) yes P(1) O(5) . 1.611(2) yes O(1) C(1) . 1.145(4) yes O(2) C(2) . 1.149(4) yes O(3) C(3) . 1.451(4) yes O(4) C(4) . 1.458(4) yes O(5) C(5) . 1.445(4) yes