#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003238.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_2003238 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 364 _journal_page_last 367 _publ_section_title ; [CpMoCl(PMe~3~)~3~][BF~4~] and [Cp*MoCl(PMe~3~)~3~][PF~6~] ; _chemical_formula_moiety 'C19 H42 Cl1 F6 Mo1 P4' _chemical_formula_sum 'C19 H42 Cl1 F6 Mo1 P4' _chemical_formula_weight 639.8 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' 'x,1/2-y,1/2+z' '-x,-y,-z' '-x,1/2+y,1/2-z' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_length_a 12.369(6) _cell_length_b 14.664(5) _cell_length_c 15.769(5) _cell_angle_alpha 90. _cell_angle_beta 90.96(3) _cell_angle_gamma 90. _cell_volume 2859.8(20) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_meas ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.70930 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20 _cell_measurement_theta_max 25 _exptl_absorpt_coefficient_mu 0.821 _cell_measurement_temperature 299 _exptl_crystal_description 'block' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.22 _exptl_crystal_size_rad ? _exptl_crystal_colour 'dark red' _chemical_compound_source ? _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\q/2\q' _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.9921 _exptl_absorpt_correction_T_max 1.0000 _diffrn_reflns_number 4749 _reflns_number_total 4349 _reflns_number_observed 3516 _reflns_observed_criterion F>4\s(F) _diffrn_reflns_av_R_equivalents 1.25 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% none _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0694 _refine_ls_wR_factor_obs 0.1193 _refine_ls_wR_factor_all 0.1255 _refine_ls_goodness_of_fit_obs 1.89 _refine_ls_number_reflns 3516 _refine_ls_number_parameters 281 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme 'w = 1/[\s^2^(F) + 0.003F^2^]' _refine_ls_shift/esd_max 0.079 _refine_diff_density_max 1.01 _refine_diff_density_min -0.75 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _atom_type_scat_source 'SHELXTL-Plus Sheldrick, 1987)' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Mo .7384(1) .1594(1) .8207(1) .028(1) Cl .7094(3) .2766(2) .7084(2) .068(1) P1 .7524(2) -.0091(2) .8386(2) .036(1) P2 .5514(3) .1270(2) .7557(2) .058(1) P3 .9024(3) .1439(2) .7258(2) .057(1) P4 .2437(2) .3464(2) .0145(2) .057(1) F1 .1767(7) .2784(6) .0637(6) .163(6) F2 .3101(8) .4157(8) -.0336(7) .232(10) F3 .3471(6) .2980(6) .0421(6) .148(6) F4 .2535(9) .4065(7) .0938(6) .176(7) F5 .1410(6) .3960(7) -.0119(8) .255(12) F6 .2340(10) .2864(8) -.0627(6) .247(12) C1 .6646(8) .1934(7) .9539(6) .041(3) C2 .6874(9) .2748(7) .9098(6) .045(3) C3 .8010(8) .2811(7) .9015(7) .044(3) C4 .8463(7) .2015(7) .9379(6) .042(3) C5 .7625(9) .1496(6) .9726(6) .041(3) C6 .5556(10) .1675(8) .9910(8) .064(4) C7 .6070(10) .3540(8) .8950(9) .063(4) C8 .8590(11) .3644(8) .8736(9) .070(5) C9 .9684(8) .1897(9) .9537(9) .068(5) C10 .7803(13) .0746(9) 1.0396(7) .082(6) C11 .7414(11) -.0763(8) .7408(8) .070(5) C12 .8769(9) -.0556(8) .8833(8) .057(4) C13 .6526(11) -.0679(8) .9023(9) .071(5) C21 .5590(11) .1009(11) .6446(9) .080(5) C22 .4599(10) .0381(10) .7910(12) .096(7) C23 .4600(10) .2241(10) .7534(9) .089(6) C31 1.0165(10) .0616(10) .7443(11) .089(6) C32 .8692(12) .1203(11) .6174(8) .086(6) C33 .9836(13) .2474(10) .7160(10) .097(6) H6a .5502 .1929 1.0469 .080 H6b .4973 .1899 .9559 .080 H6c .5517 .1022 .9943 .080 H7a .6023 .3902 .9455 .080 H7b .6335 .3910 .8496 .080 H7c .5366 .3310 .8798 .080 H8a .8753 .4014 .9224 .080 H8b .9249 .3488 .8458 .080 H8c .8129 .3978 .8351 .080 H9a .9884 .2151 1.0078 .080 H9b .9845 .1257 .9533 .080 H9c 1.0083 .2196 .9100 .080 H10a .7876 .1015 1.0949 .080 H10b .7194 .0341 1.0385 .080 H10c .8448 .0411 1.0270 .080 H11a .7479 -.1402 .7535 .080 H11b .6723 -.0648 .7144 .080 H11c .7978 -.0587 .7030 .080 H12a .8705 -.1208 .8861 .080 H12b .9370 -.0398 .8484 .080 H12c .8885 -.0316 .9393 .080 H13a .6686 -.1320 .9036 .080 H13b .6541 -.0444 .9591 .080 H13c .5821 -.0586 .8774 .080 H21a .4882 .0889 .6213 .080 H21b .5904 .1518 .6157 .080 H21c .6038 .0480 .6375 .080 H22a .3950 .0393 .7568 .080 H22b .4938 -.0205 .7862 .080 H22c .4423 .0491 .8492 .080 H23a .3921 .2062 .7283 .080 H23b .4487 .2455 .8101 .080 H23c .4913 .2720 .7204 .080 H31a 1.0689 .0677 .7004 .080 H31b 1.0501 .0745 .7983 .080 H31c .9886 .0005 .7443 .080 H32a .9345 .1153 .5857 .080 H32b .8297 .0640 .6135 .080 H32c .8257 .1689 .5946 .080 H33a 1.0434 .2364 .6794 .080 H33b .9398 .2959 .6932 .080 H33c 1.0103 .2643 .7714 .080