#------------------------------------------------------------------------------ #$Date: 2008-02-24 20:27:26 +0000 (Sun, 24 Feb 2008) $ #$Revision: 175 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100870.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_1100870 _publ_section_title ; Step Wise Formation of s-Alkynyl, Vinylidene, and Vinylphosphonium Complexes of Manganese(I) ; loop_ _publ_author_name 'Ruiz, J.' 'Quesada, R.' 'Vivanco, M.' 'Castellano, E. E.' 'Piro, O. E.' _chemical_name_systematic ; fac-[tricarbonyl(2-methoxycarbonylvinyliden(diphenylphosphanylmethyl) diphenylphosphorane)maganese(I)] tetrafluoroborate ; _chemical_formula_sum 'C32 H26 B F4 Mn O5 P2' _chemical_formula_weight 694.22 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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~/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2407(2) _cell_length_b 16.6566(4) _cell_length_c 18.3683(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.650(1) _cell_angle_gamma 90.00 _cell_volume 3118.0(1) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22022 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 25.00 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.617 _exptl_absorpt_correction_T_max 0.849 _diffrn_ambient_temperature 100(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 KappaCCD _diffrn_measurement_method 'CCD with \f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 22022 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5480 _reflns_number_gt 4655 _reflns_threshold_expression >2\s(I) ##'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+2.0141P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0047(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5480 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn Mn 0.93171(3) 0.181639(19) 0.221905(17) 0.01814(12) Uani 1 d . . . P1 P 0.85675(5) 0.21032(3) 0.33392(3) 0.01820(15) Uani 1 d . . . P2 P 0.66605(5) 0.09088(3) 0.26595(3) 0.01868(15) Uani 1 d . . . B B 0.3918(3) 0.23558(19) 0.39605(16) 0.0302(6) Uani 1 d . . . F1 F 0.49390(16) 0.22549(12) 0.45046(8) 0.0519(5) Uani 1 d . . . F2 F 0.43176(17) 0.28708(12) 0.34391(11) 0.0606(5) Uani 1 d . . . F3 F 0.36634(19) 0.16121(12) 0.36386(12) 0.0662(6) Uani 1 d . . . F4 F 0.28007(15) 0.26384(12) 0.42347(10) 0.0544(5) Uani 1 d . . . O1 O 0.72166(17) 0.29027(11) 0.16291(10) 0.0325(4) Uani 1 d . . . O2 O 1.12908(18) 0.31370(11) 0.22474(11) 0.0368(4) Uani 1 d . . . O3 O 0.9473(2) 0.14554(13) 0.06452(10) 0.0446(5) Uani 1 d . . . O4 O 1.08137(14) 0.09876(9) 0.25177(8) 0.0208(3) Uani 1 d . . . O5 O 1.12072(14) -0.02942(9) 0.28548(8) 0.0228(3) Uani 1 d . . . C1 C 0.8043(2) 0.24757(14) 0.18727(12) 0.0230(5) Uani 1 d . . . C2 C 1.0531(2) 0.26297(14) 0.22409(12) 0.0244(5) Uani 1 d . . . C3 C 0.9470(2) 0.15711(14) 0.12572(13) 0.0262(5) Uani 1 d . . . C4 C 1.0416(2) 0.03060(13) 0.26513(11) 0.0198(5) Uani 1 d . . . C5 C 1.2601(2) -0.01051(15) 0.29511(14) 0.0284(5) Uani 1 d . . . H5A H 1.3095 -0.0581 0.3130 0.043 Uiso 1 calc R . . H5B H 1.2755 0.0332 0.3307 0.043 Uiso 1 calc R . . H5C H 1.2891 0.0062 0.2481 0.043 Uiso 1 calc R . . C6 C 0.9012(2) 0.01577(13) 0.26313(11) 0.0202(5) Uani 1 d . . . H6 H 0.8644 -0.0345 0.2747 0.024 Uiso 1 calc R . . C7 C 0.8297(2) 0.08106(13) 0.24312(11) 0.0191(5) Uani 1 d . . . C8 C 0.6810(2) 0.18078(13) 0.32201(12) 0.0201(5) Uani 1 d . . . H8A H 0.6491 0.1701 0.3702 0.024 Uiso 1 calc R . . H8B H 0.6276 0.2246 0.2979 0.024 Uiso 1 calc R . . C111 C 0.9247(2) 0.15961(14) 0.41680(12) 0.0229(5) Uani 1 d . . . C112 C 1.0557(2) 0.13675(16) 0.42124(13) 0.0295(5) Uani 1 d . . . H112 H 1.1044 0.1436 0.3802 0.035 Uiso 1 calc R . . C113 C 1.1154(3) 0.10396(19) 0.48530(15) 0.0430(7) Uani 1 d . . . H113 H 1.2054 0.0891 0.4884 0.052 Uiso 1 calc R . . C114 C 1.0446(3) 0.09278(19) 0.54475(15) 0.0480(8) Uani 1 d . . . H114 H 1.0853 0.0688 0.5882 0.058 Uiso 1 calc R . . C115 C 0.9152(3) 0.11625(18) 0.54122(14) 0.0426(7) Uani 1 d . . . H115 H 0.8674 0.1091 0.5825 0.051 Uiso 1 calc R . . C116 C 0.8539(3) 0.15029(15) 0.47768(13) 0.0305(6) Uani 1 d . . . H116 H 0.7649 0.1670 0.4756 0.037 Uiso 1 calc R . . C121 C 0.8541(2) 0.31486(13) 0.36354(12) 0.0209(5) Uani 1 d . . . C122 C 0.9758(2) 0.35225(14) 0.37964(12) 0.0236(5) Uani 1 d . . . H122 H 1.0545 0.3236 0.3743 0.028 Uiso 1 calc R . . C123 C 0.9811(2) 0.43139(15) 0.40344(12) 0.0269(5) Uani 1 d . . . H123 H 1.0638 0.4567 0.4146 0.032 Uiso 1 calc R . . C124 C 0.8667(2) 0.47390(15) 0.41099(13) 0.0297(6) Uani 1 d . . . H124 H 0.8710 0.5281 0.4270 0.036 Uiso 1 calc R . . C125 C 0.7465(3) 0.43693(15) 0.39507(14) 0.0315(6) Uani 1 d . . . H125 H 0.6682 0.4660 0.4003 0.038 Uiso 1 calc R . . C126 C 0.7392(2) 0.35751(14) 0.37143(13) 0.0277(5) Uani 1 d . . . H126 H 0.6562 0.3325 0.3607 0.033 Uiso 1 calc R . . C211 C 0.5556(2) 0.10817(13) 0.18566(12) 0.0213(5) Uani 1 d . . . C212 C 0.4302(2) 0.13814(14) 0.19287(13) 0.0252(5) Uani 1 d . . . H212 H 0.4038 0.1490 0.2400 0.030 Uiso 1 calc R . . C213 C 0.3449(2) 0.15195(15) 0.13128(15) 0.0328(6) Uani 1 d . . . H213 H 0.2594 0.1722 0.1361 0.039 Uiso 1 calc R . . C214 C 0.3832(3) 0.13639(17) 0.06245(15) 0.0377(6) Uani 1 d . . . H214 H 0.3244 0.1464 0.0202 0.045 Uiso 1 calc R . . C215 C 0.5073(3) 0.10622(18) 0.05518(14) 0.0395(7) Uani 1 d . . . H215 H 0.5330 0.0953 0.0079 0.047 Uiso 1 calc R . . C216 C 0.5938(2) 0.09187(16) 0.11638(13) 0.0309(6) Uani 1 d . . . H216 H 0.6788 0.0710 0.1113 0.037 Uiso 1 calc R . . C221 C 0.6121(2) 0.00610(14) 0.31530(12) 0.0208(5) Uani 1 d . . . C222 C 0.5938(2) 0.00841(15) 0.38952(13) 0.0265(5) Uani 1 d . . . H222 H 0.6013 0.0578 0.4155 0.032 Uiso 1 calc R . . C223 C 0.5645(2) -0.06166(15) 0.42519(13) 0.0285(5) Uani 1 d . . . H223 H 0.5513 -0.0600 0.4756 0.034 Uiso 1 calc R . . C224 C 0.5543(2) -0.13398(15) 0.38811(14) 0.0280(5) Uani 1 d . . . H224 H 0.5356 -0.1818 0.4132 0.034 Uiso 1 calc R . . C225 C 0.5715(2) -0.13657(15) 0.31415(14) 0.0270(5) Uani 1 d . . . H225 H 0.5641 -0.1862 0.2886 0.032 Uiso 1 calc R . . C226 C 0.5995(2) -0.06695(14) 0.27762(13) 0.0239(5) Uani 1 d . . . H226 H 0.6101 -0.0687 0.2269 0.029 Uiso 1 calc R . . 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 Mn 0.0198(2) 0.0142(2) 0.0209(2) 0.00117(13) 0.00428(14) 0.00124(13) P1 0.0197(3) 0.0143(3) 0.0209(3) -0.0007(2) 0.0038(2) -0.0011(2) P2 0.0181(3) 0.0155(3) 0.0227(3) -0.0008(2) 0.0032(2) 0.0000(2) B 0.0285(14) 0.0331(16) 0.0303(14) -0.0094(12) 0.0086(12) -0.0049(12) F1 0.0426(9) 0.0822(14) 0.0314(8) -0.0029(8) 0.0068(7) 0.0086(9) F2 0.0403(10) 0.0620(12) 0.0805(13) 0.0357(11) 0.0107(9) 0.0079(9) F3 0.0628(12) 0.0566(12) 0.0827(14) -0.0410(11) 0.0246(10) -0.0173(10) F4 0.0296(8) 0.0734(13) 0.0618(11) -0.0362(10) 0.0131(8) -0.0045(8) O1 0.0301(9) 0.0263(10) 0.0409(10) 0.0061(8) 0.0028(8) 0.0094(8) O2 0.0353(10) 0.0241(10) 0.0524(12) -0.0002(8) 0.0110(9) -0.0099(8) O3 0.0644(13) 0.0454(12) 0.0251(10) -0.0026(8) 0.0098(9) 0.0158(10) O4 0.0208(8) 0.0165(8) 0.0255(8) 0.0011(6) 0.0048(6) -0.0011(6) O5 0.0205(8) 0.0166(8) 0.0312(8) 0.0032(7) 0.0024(6) 0.0023(6) C1 0.0255(12) 0.0190(12) 0.0258(11) -0.0014(9) 0.0092(10) -0.0027(10) C2 0.0266(12) 0.0216(13) 0.0257(12) 0.0005(9) 0.0057(10) 0.0053(10) C3 0.0297(12) 0.0188(12) 0.0305(13) 0.0018(10) 0.0051(10) 0.0046(10) C4 0.0234(11) 0.0177(12) 0.0186(10) -0.0019(9) 0.0041(9) 0.0031(9) C5 0.0182(11) 0.0235(13) 0.0428(14) 0.0035(11) 0.0002(10) 0.0012(9) C6 0.0223(11) 0.0172(11) 0.0217(11) -0.0004(9) 0.0045(9) -0.0019(9) C7 0.0209(11) 0.0180(11) 0.0190(10) -0.0023(9) 0.0043(9) -0.0011(9) C8 0.0198(11) 0.0152(11) 0.0259(11) -0.0010(9) 0.0053(9) 0.0002(8) C111 0.0285(12) 0.0165(11) 0.0236(11) -0.0007(9) 0.0026(9) -0.0029(9) C112 0.0293(13) 0.0323(14) 0.0263(12) -0.0028(10) -0.0003(10) 0.0024(11) C113 0.0396(16) 0.0535(19) 0.0335(14) 0.0008(13) -0.0077(12) 0.0132(14) C114 0.068(2) 0.0485(19) 0.0254(14) 0.0072(13) -0.0053(14) 0.0143(16) C115 0.068(2) 0.0359(16) 0.0250(13) 0.0055(12) 0.0109(13) -0.0018(14) C116 0.0380(14) 0.0278(14) 0.0265(12) -0.0004(10) 0.0081(11) -0.0002(11) C121 0.0286(12) 0.0162(11) 0.0183(10) -0.0005(9) 0.0048(9) -0.0012(9) C122 0.0257(12) 0.0227(12) 0.0225(11) -0.0019(9) 0.0028(9) -0.0021(10) C123 0.0329(13) 0.0239(13) 0.0235(11) -0.0011(10) 0.0002(10) -0.0090(10) C124 0.0427(15) 0.0180(12) 0.0291(12) -0.0026(10) 0.0075(11) -0.0040(11) C125 0.0351(14) 0.0201(13) 0.0407(14) -0.0053(11) 0.0109(11) 0.0032(10) C126 0.0284(13) 0.0192(12) 0.0365(13) -0.0016(10) 0.0078(10) -0.0023(10) C211 0.0232(11) 0.0156(11) 0.0248(11) 0.0004(9) 0.0015(9) -0.0040(9) C212 0.0253(12) 0.0180(12) 0.0319(12) -0.0016(10) 0.0015(10) -0.0006(9) C213 0.0282(13) 0.0220(13) 0.0466(15) 0.0048(11) -0.0050(11) 0.0008(10) C214 0.0407(15) 0.0302(15) 0.0389(15) 0.0144(12) -0.0124(12) -0.0106(12) C215 0.0473(17) 0.0461(17) 0.0248(13) 0.0044(12) 0.0021(12) -0.0157(13) C216 0.0282(13) 0.0354(15) 0.0296(13) -0.0026(11) 0.0050(10) -0.0052(11) C221 0.0159(10) 0.0197(12) 0.0268(11) 0.0021(9) 0.0018(9) 0.0003(9) C222 0.0272(12) 0.0243(13) 0.0285(12) -0.0016(10) 0.0054(10) -0.0042(10) C223 0.0273(12) 0.0313(14) 0.0272(12) 0.0042(10) 0.0041(10) -0.0021(10) C224 0.0200(11) 0.0261(13) 0.0377(13) 0.0092(11) 0.0017(10) -0.0012(10) C225 0.0226(12) 0.0184(12) 0.0397(14) 0.0007(10) 0.0023(10) -0.0012(9) C226 0.0228(11) 0.0199(12) 0.0293(12) -0.0002(10) 0.0036(10) -0.0007(9)