#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003546.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_2003546 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1075 _journal_page_last 1078 _publ_section_title ; A Chelate-Stabilized Molybdenum-Imido-Alkylidene Complex, [TpMo{CHC(Me)~2~Ph}(NAr)(OTf)] ; _chemical_formula_moiety 'C32 H39 B1 F3 Mo1 N7 O3 S1' _chemical_formula_sum 'C32 H39 B1 F3 Mo1 N7 O3 S1' _chemical_formula_weight 765.51 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '1/2-x,-y,1/2+z' '-x,1/2+y,1/2-z' '1/2+x,1/2-y,-z' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_length_a 10.434(2) _cell_length_b 13.699(2) _cell_length_c 25.148(4) _cell_angle_alpha 90. _cell_angle_beta 90. _cell_angle_gamma 90. _cell_volume 3595(1) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_meas ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 32 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_absorpt_coefficient_mu 0.48 _cell_measurement_temperature 293 _exptl_crystal_description 'needles' _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_colour 'orange-yellow' _chemical_compound_source ? _diffrn_measurement_device 'Siemens P3m/V' _diffrn_measurement_method '\w' _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.951 _exptl_absorpt_correction_T_max 0.960 _diffrn_reflns_number 3603 _reflns_number_total 3575 _reflns_number_observed 2489 _reflns_observed_criterion F>6\s(F) _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number 4 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0530 _refine_ls_wR_factor_obs 0.0546 _refine_ls_goodness_of_fit_obs 1.48 _refine_ls_number_reflns 2489 _refine_ls_number_parameters 437 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme 'w = 1/[\s^2^(F) + 0.0004F^2^]' _refine_ls_shift/esd_max 0.0001 _refine_diff_density_max 0.50 _refine_diff_density_min -0.54 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _atom_type_scat_source 'IntTabIV' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Mo .02932(9) .06468(6) .11559(3) .0288(2) S .2775(3) .1472(3) .1893(2) .0614(13) F1 .354(2) .2176(12) .2772(6) .236(10) F2 .245(2) .0858(10) .2851(4) .201(8) F3 .158(2) .2210(11) .2684(5) .187(9) O1 .1602(7) .0942(6) .1781(3) .043(3) O2 .2804(9) .2433(7) .1674(4) .075(4) O3 .3881(9) .0893(3) .1845(6) .131(6) N .0679(7) -.0592(6) .1083(3) .036(3) N1 -.0468(8) .2193(6) .1344(3) .039(3) N2 -.1711(9) .2343(7) .1456(3) .040(3) N3 -.1466(8) .0698(8) .0699(3) .039(3) N4 -.2606(8) .0980(6) .0918(4) .039(3) N5 -.1054(9) .0331(6) .1865(4) .041(3) N6 -.2238(9) .0731(8) .1893(3) .045(3) B -.2661(14) .1492(10) .1481(5) .050(5) C1 .1267(10) .1205(8) .0569(4) .028(3) C2 .2187(10) .0892(7) .0143(4) .036(4) C3 .3115(12) .1752(8) .0034(5) .052(4) C4 .2995(11) .0032(8) .0321(5) .049(4) C5 .1382(9) .0680(9) -.0352(3) .035(3) C6 .0661(11) .1406(10) -.0588(5) .054(5) C7 -.0121(12) .1213(11) -.1014(5) .070(6) C8 -.0198(15) .0282(12) -.1218(5) .084(6) C9 .0498(15) -.0435(12) -.0986(6) .089(7) C10 .1277(12) -.0246(9) -.0564(5) .062(5) C11 .0880(10) -.1598(7) .1101(5) .035(3) C12 -.0007(13) -.2232(8) .0866(5) .058(5) C13 .018(2) -.3224(8) .0922(5) .077(6) C14 .121(2) -.3596(9) .1181(6) .082(6) C15 .210(2) -.2976(10) .1389(5) .076(6) C16 .1967(12) -.1968(8) .1364(4) .049(4) C17 .3005(13) -.1323(10) .1613(5) .059(5) C18 .297(2) -.1426(12) .2217(5) .092(7) C19 .4320(11) -.1515(10) .1398(6) .074(6) C20 -.1187(13) -.1839(9) .0594(5) .057(5) C21 -.137(2) -.2303(11) .0048(6) .098(7) C22 -.237(2) -.1908(14) .0920(6) .115(9) C23 .0115(12) .3092(8) .1337(4) .047(4) C24 -.0788(13) .3777(9) .1461(5) .059(5) C25 -.1918(13) .3295(9) .1525(4) .051(5) C26 -.1773(12) .0456(8) .0202(5) .045(4) C27 -.3051(13) .0495(11) .0103(6) .062(5) C28 -.3564(11) .0861(9) .0579(6) .058(5) C29 -.0977(14) -.0306(9) .2248(4) .058(5) C30 -.2101(13) -.0339(11) .2537(5) .069(6) C31 -.2881(14) .0372(10) .2306(6) .070(6) C32 .260(3) .1658(13) .2602(8) .134(13) H -.37214 .18044 .15262 .08 H1 .096(8) .185(7) .055(3) .03(3) H3a .37168 .15671 -.02369 .08 H3b .3569 .19105 .03545 .08 H3c .26364 .23104 -.0083 .08 H4a .24428 -.05139 .03909 .08 H4b .34562 .01982 .06384 .08 H4c .3591 -.01378 .00451 .08 H6a .07151 .20603 -.04529 .08 H7a -.06228 .17285 -.11673 .08 H8a -.07188 .01535 -.1525 .08 H9a .04231 -.10921 -.1115 .08 H10a .17702 -.07652 -.04087 .08 H13a -.04483 -.36626 .078 .08 H14a .13266 -.42892 .12141 .08 H15a .28386 -.32533 .15564 .08 H17a .28129 -.06584 .15221 .08 H18a .36302 -.1023 .23699 .08 H18b .31193 -.20942 .2314 .08 H18c .21514 -.12212 .23486 .08 H19a .43003 -.14466 .10186 .08 H19b .45822 -.21657 .14891 .08 H19c .49162 -.10548 .15455 .08 H20a -.10343 -.11536 .05468 .08 H21a -.05927 -.22468 -.01538 .08 H21b -.20519 -.19765 -.01366 .08 H21c -.15834 -.29805 .00909 .08 H22a -.22254 -.16092 .12598 .08 H22b -.25924 -.25824 .09695 .08 H22c -.3061 -.15785 .07421 .08 H23a .09962 .32182 .125150 .08 H24a -.06499 .4465 .15038 .08 H25a -.27267 .3594 .16055 .08 H26a -.1155 .02687 -.00621 .08 H27a -.35048 .03089 -.02132 .08 H28a -.44484 .10094 .06469 .08 H29a -.02387 -.0704 .23175 .08 H30a -.23087 -.07599 .28301 .08 H31a -.37108 .05777 .24268 .08