#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003585.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_2003585 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 1232 _journal_page_last 1234 _publ_section_title ; (1R*,3S*,4R*)-4-tert-Butyldiphenylsilyloxy- 6,7-dimethoxy-1-methyl-3-phenyl-1,2,3,4-tetrahydroisoquinoline ; _chemical_formula_moiety 'C34 H39 N1 O3 Si1' _chemical_formula_sum 'C34 H39 N1 O3 Si1' _chemical_formula_weight 537.773 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' _symmetry_space_group_name_H-M 'P 21/n' _cell_length_a 13.747(9) _cell_length_b 21.08(4) _cell_length_c 10.30(1) _cell_angle_alpha 90. _cell_angle_beta 98.97(6) _cell_angle_gamma 90. _cell_volume 2949(7) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.21 _exptl_crystal_density_meas ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _exptl_absorpt_coefficient_mu 0.109 _cell_measurement_temperature 295 _exptl_crystal_description 'prismatic' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_colour 'colourless' _chemical_compound_source ? _diffrn_measurement_device 'Philips PW1100' _diffrn_measurement_method '\w/2\q' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 3904 _reflns_number_total 3759 _reflns_number_observed 3125 _reflns_observed_criterion I>3\s(I) _diffrn_reflns_av_R_equivalents '0.017' _diffrn_reflns_theta_max '25' _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% <1.0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.071 _refine_ls_wR_factor_obs 0.094 _refine_ls_goodness_of_fit_obs 1.115 _refine_ls_number_reflns 3125 _refine_ls_number_parameters 509 _refine_ls_hydrogen_treatment 'H atoms refined isotropically' _refine_ls_weighting_scheme 'w = 1/[\s^2^(F) + 0.014141F^2^]' _refine_ls_shift/esd_max 0.15 _refine_diff_density_max 0.28 _refine_diff_density_min -0.50 _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_B_iso_or_equiv Si1 .3785(1) .3159(1) .9110(1) 2.90(3) C3 .5957(2) .3795(2) 1.1067(3) 2.39(9) O1 .4249(2) .3749(1) 1.0019(2) 2.80(6) O6 .8831(2) .3769(1) 1.0347(3) 4.23(8) N10 .5363(2) .4502(2) 1.2998(3) 3.41(9) C5 .7235(3) .3365(2) .9985(3) 2.77(10) C18 .4344(3) .3213(2) .7600(4) 3.28(10) C20 .4662(3) .2790(2) .5526(4) 4.64(13) C17 .3006(3) .4961(2) 1.1595(4) 4.09(13) C2 .4880(2) .3805(2) 1.1228(3) 2.47(10) C23 .4945(3) .3724(2) .7384(4) 3.57(10) C12 .3634(2) .4487(2) 1.2157(3) 2.74(10) C4 .6278(2) .3366(2) 1.0198(3) 2.63(10) C9 .6338(3) .4649(2) 1.2754(4) 3.69(11) O5 .7599(2) .2973(1) .9135(3) 4.21(8) C8 .6625(3) .4204(2) 1.1791(3) 2.81(9) C6 .7902(2) .3789(2) 1.0660(3) 3.06(10) C91 .7031(3) .4653(3) 1.4020(4) 6.49(18) C30 .2414(3) .3275(2) .8699(4) 3.47(11) C13 .3327(3) .4105(2) 1.3079(4) 3.67(11) C19 .4207(3) .2752(2) .6609(4) 3.74(10) C51 .6947(3) .2509(2) .8509(5) 5.55(15) C7 .7599(3) .4188(2) 1.1540(4) 3.36(10) C11 .4657(2) .4437(2) 1.1834(3) 2.88(10) C22 .5412(3) .3763(2) .6319(4) 4.55(13) C21 .5260(3) .3301(2) .5382(4) 4.60(13) C61 .9544(3) .4162(3) 1.1079(5) 6.16(17) C24 .4099(3) .2385(2) .9966(3) 3.33(10) C14 .2412(3) .4186(2) 1.3445(4) 4.35(12) C15 .1790(3) .4657(2) 1.2867(4) 4.61(13) C25 .4536(3) .1890(2) .9392(4) 4.55(13) C26 .4745(4) .1317(2) 1.0070(5) 5.98(17) C27 .4481(4) .1220(2) 1.1255(5) 5.46(17) C28 .4040(4) .1708(2) 1.1822(5) 5.23(14) C16 .2093(3) .5040(3) 1.1967(5) 5.06(14) C29 .3854(3) .2275(2) 1.1189(5) 4.70(13) C31 .1921(4) .3248(4) .9937(6) 6.08(19) C32 .1948(4) .2752(3) .7800(7) 5.85(19) C33 .2207(4) .3919(3) .8071(6) 5.84(15) H19 .3826(27) .2423(19) .6614(39) 526(107) H613 .9346(28) .4627(20) 1.0819(37) 618(119) H23 .5111(27) .4065(17) .8266(37) 498(104) H14 .2295(19) .3943(13) 1.4021(26) 159(69) H321 .2220(30) .2681(19) .7010(43) 460(113) H22 .5793(31) .4132(20) .6330(39) 618(117) H25 .4748(26) .1990(18) .8578(35) 440(97) H17 .3204(26) .5248(16) 1.0992(32) 419(93) H13 .3739(33) .3831(20) 1.3724(45) 749(132) H511 .7386(23) .2237(15) .8119(31) 305(83) H29 .3515(24) .2607(16) 1.1673(34) 285(83) H21 .5573(35) .3338(23) .4692(44) 799(143) H20 .4523(28) .2508(17) .4762(38) 511(103) H322 .2191(34) .2344(23) .8097(43) 550(133) H512 .6688(41) .2153(27) .9188(55) 1027(176) H4 .5734(27) .3063(17) .9589(36) 447(98) H7 .7913(24) .4452(16) 1.1801(32) 400(92) H10 .5177(22) .4726(15) 1.3588(29) 294(80) H15 .1081(25) .4720(17) 1.3140(33) 419(93) H912 .6771(58) .4918(37) 1.4860(71) 1587(281) H28 .3898(34) .1673(22) 1.2631(47) 622(136) H323 .1262(46) .2745(25) .7931(50) 874(168) H913 .7185(29) .4236(19) 1.4430(38) 581(113) H27 .4681(43) .0879(26) 1.2153(51) 996(170) H611 1.0082(35) .4146(23) 1.0820(47) 821(148) H911 .7751(48) .4790(32) 1.3880(55) 1228(212) H16 .1827(66) .5454(42) 1.1837(80) 1821(363) H331 .2552(61) .4022(36) .7065(78) 1582(282) H2 .4762(20) .3442(13) 1.1928(27) 182(70) H11 .4736(26) .4826(16) 1.1066(32) 413(91) H9 .6344(25) .5017(16) 1.2383(32) 383(90) H311 .2207(33) .3520(22) 1.0445(45) 473(126) H312 .1304(47) .3354(27) .9814(52) 881(177) H26 .5121(32) .0995(21) .9685(41) 677(124) H313 .1866(39) .2640(31) 1.0079(55) 1005(178) H513 .6374(47) .2715(31) .8111(66) 1243(217) H612 .9554(56) .4254(37) 1.1997(71) 1458(244) H332 .2593(41) .4291(27) .8634(51) 860(158) H333 .1386(71) .3960(39) .8138(81) 1898(316)