#------------------------------------------------------------------------------ #$Date: 2016-03-21 04:06:01 +0000 (Mon, 21 Mar 2016) $ #$Revision: 178490 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/01/4060143.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_4060143 _journal_name_full Organometallics _journal_paper_doi 10.1021/om049263i _journal_year 2005 _chemical_formula_sum 'C35 H58 B Mg N3' _chemical_formula_weight 555.96 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 92.938(11) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.1020(10) _cell_length_b 35.987(6) _cell_length_c 10.833(2) _cell_measurement_reflns_used ? _cell_measurement_temperature 173(2) _cell_measurement_theta_max 25.1 _cell_measurement_theta_min 3.4 _cell_volume 3543.7(10) _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'Kappa CCD (Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 11926 _diffrn_reflns_theta_max 25.11 _diffrn_reflns_theta_min 3.45 _diffrn_standards_decay_% 'no decay' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_T_max 0.9910 _exptl_absorpt_correction_T_min 0.9851 _exptl_absorpt_correction_type none _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.042 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 1224 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 375 _refine_ls_number_reflns 6225 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.985 _refine_ls_R_factor_all 0.1052 _refine_ls_R_factor_gt 0.0652 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1556P)^2^+0.0304P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1931 _refine_ls_wR_factor_ref 0.2223 _reflns_number_gt 4154 _reflns_number_total 6225 _reflns_threshold_expression >2sigma(I) _cod_original_sg_symbol_H-M P21/c _cod_database_code 4060143 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' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.73517(10) 0.09598(3) 0.48611(8) 0.0274(3) Uani 1 1 d . . . N1 N 0.7479(2) 0.14673(6) 0.41135(18) 0.0237(5) Uani 1 1 d . . . N2 N 0.6759(2) 0.06907(6) 0.32102(19) 0.0276(5) Uani 1 1 d . . . N3 N 0.5119(2) 0.11342(6) 0.37538(19) 0.0257(5) Uani 1 1 d . . . C1 C 0.5452(3) 0.08209(8) 0.3005(2) 0.0264(6) Uani 1 1 d . . . C2 C 0.7801(3) 0.06512(8) 0.6546(3) 0.0338(7) Uani 1 1 d . . . C3 C 0.7533(3) 0.04034(8) 0.2501(3) 0.0344(7) Uani 1 1 d . . . H3A H 0.7273 0.0678 0.8392 0.085 Uiso 1 1 calc R . . H3B H 0.5943 0.0807 0.7466 0.085 Uiso 1 1 calc R . . H3C H 0.7309 0.1079 0.7753 0.085 Uiso 1 1 calc R . . C4 C 0.4325(3) 0.06722(8) 0.2052(2) 0.0342(7) Uani 1 1 d . . . H4A H 0.7918 0.0126 0.5789 0.069 Uiso 1 1 calc R . . H4B H 0.6291 0.0233 0.6158 0.069 Uiso 1 1 calc R . . H4C H 0.7509 0.0120 0.7208 0.069 Uiso 1 1 calc R . . C5 C 0.3698(3) 0.11400(8) 0.4427(2) 0.0294(7) Uani 1 1 d . . . H5A H 0.9641 0.0513 0.7667 0.077 Uiso 1 1 calc R . . H5B H 0.9797 0.0909 0.7014 0.077 Uiso 1 1 calc R . . H5C H 0.9988 0.0535 0.6236 0.077 Uiso 1 1 calc R . . C6 C 0.5306(3) 0.18721(8) 0.3138(2) 0.0265(6) Uani 1 1 d . . . C7 C 0.8614(3) 0.17363(7) 0.4019(2) 0.0231(6) Uani 1 1 d . . . C8 C 1.0503(3) 0.21204(8) 0.5033(3) 0.0313(7) Uani 1 1 d . . . H8 H 1.1004 0.2208 0.5767 0.038 Uiso 1 1 calc R . . C9 C 1.0921(3) 0.22488(8) 0.3905(3) 0.0358(7) Uani 1 1 d . . . H9 H 1.1688 0.2427 0.3863 0.043 Uiso 1 1 calc R . . C10 C 1.0210(3) 0.21148(8) 0.2833(3) 0.0314(7) Uani 1 1 d . . . H10 H 1.0509 0.2201 0.2056 0.038 Uiso 1 1 calc R . . C11 C 0.9075(3) 0.18585(8) 0.2866(2) 0.0266(6) Uani 1 1 d . . . C12 C 0.8936(3) 0.17235(8) 0.6381(2) 0.0276(6) Uani 1 1 d . . . H12 H 0.8658 0.1456 0.6274 0.033 Uiso 1 1 calc R . . C13 C 0.7599(3) 0.19226(9) 0.6846(3) 0.0393(8) Uani 1 1 d . . . H13A H 0.7822 0.2187 0.6953 0.059 Uiso 1 1 calc R . . H13B H 0.7348 0.1816 0.7641 0.059 Uiso 1 1 calc R . . H13C H 0.6766 0.1893 0.6245 0.059 Uiso 1 1 calc R . . C14 C 1.0193(3) 0.17386(9) 0.7380(2) 0.0395(8) Uani 1 1 d . . . H14A H 1.1077 0.1625 0.7062 0.059 Uiso 1 1 calc R . . H14B H 0.9906 0.1602 0.8112 0.059 Uiso 1 1 calc R . . H14C H 1.0398 0.1998 0.7603 0.059 Uiso 1 1 calc R . . C15 C 0.8448(3) 0.17020(8) 0.1638(2) 0.0297(7) Uani 1 1 d . . . H15 H 0.7602 0.1537 0.1820 0.036 Uiso 1 1 calc R . . C16 C 0.9597(4) 0.14641(10) 0.1025(3) 0.0421(8) Uani 1 1 d . . . H16A H 1.0434 0.1620 0.0823 0.063 Uiso 1 1 calc R . . H16B H 0.9158 0.1353 0.0267 0.063 Uiso 1 1 calc R . . H16C H 0.9936 0.1266 0.1594 0.063 Uiso 1 1 calc R . . C17 C 0.7870(4) 0.20073(9) 0.0748(3) 0.0419(8) Uani 1 1 d . . . H17A H 0.7165 0.2164 0.1164 0.063 Uiso 1 1 calc R . . H17B H 0.7382 0.1893 0.0016 0.063 Uiso 1 1 calc R . . H17C H 0.8694 0.2160 0.0498 0.063 Uiso 1 1 calc R . . C18 C 0.7010(4) 0.08191(11) 0.7638(3) 0.0568(10) Uani 1 1 d . . . C19 C 0.7505(4) 0.04812(10) 0.1109(3) 0.0460(8) Uani 1 1 d . . . H19A H 0.6527 0.0423 0.0738 0.069 Uiso 1 1 calc R . . H19B H 0.8242 0.0326 0.0728 0.069 Uiso 1 1 calc R . . H19C H 0.7729 0.0744 0.0971 0.069 Uiso 1 1 calc R . . C20 C 0.6937(4) 0.00162(9) 0.2777(3) 0.0443(8) Uani 1 1 d . . . H20A H 0.6883 -0.0015 0.3672 0.066 Uiso 1 1 calc R . . H20B H 0.7595 -0.0173 0.2457 0.066 Uiso 1 1 calc R . . H20C H 0.5953 -0.0012 0.2378 0.066 Uiso 1 1 calc R . . C21 C 0.9135(3) 0.04250(9) 0.3011(3) 0.0438(8) Uani 1 1 d . . . H21A H 0.9518 0.0676 0.2879 0.066 Uiso 1 1 calc R . . H21B H 0.9729 0.0244 0.2582 0.066 Uiso 1 1 calc R . . H21C H 0.9179 0.0369 0.3898 0.066 Uiso 1 1 calc R . . C22 C 0.9456(4) 0.06520(10) 0.6897(3) 0.0512(9) Uani 1 1 d . . . C23 C 0.3478(3) 0.07578(8) 0.5011(3) 0.0377(7) Uani 1 1 d . . . H23A H 0.3340 0.0571 0.4358 0.057 Uiso 1 1 calc R . . H23B H 0.2607 0.0764 0.5506 0.057 Uiso 1 1 calc R . . H23C H 0.4346 0.0694 0.5542 0.057 Uiso 1 1 calc R . . C24 C 0.2331(3) 0.12529(9) 0.3637(3) 0.0393(8) Uani 1 1 d . . . H24A H 0.2498 0.1495 0.3255 0.059 Uiso 1 1 calc R . . H24B H 0.1486 0.1269 0.4160 0.059 Uiso 1 1 calc R . . H24C H 0.2133 0.1067 0.2990 0.059 Uiso 1 1 calc R . . C25 C 0.3914(3) 0.14183(9) 0.5481(3) 0.0372(7) Uani 1 1 d . . . H25A H 0.4810 0.1356 0.5978 0.056 Uiso 1 1 calc R . . H25B H 0.3065 0.1409 0.6002 0.056 Uiso 1 1 calc R . . H25C H 0.4005 0.1669 0.5140 0.056 Uiso 1 1 calc R . . C26 C 0.9359(3) 0.18639(8) 0.5124(2) 0.0253(6) Uani 1 1 d . . . C27 C 0.4435(3) 0.18904(9) 0.2041(3) 0.0346(7) Uani 1 1 d . . . H27 H 0.4212 0.1667 0.1604 0.042 Uiso 1 1 calc R . . C28 C 0.3883(3) 0.22226(9) 0.1566(3) 0.0388(8) Uani 1 1 d . . . H28 H 0.3305 0.2224 0.0811 0.047 Uiso 1 1 calc R . . C29 C 0.4168(3) 0.25483(9) 0.2181(3) 0.0403(8) Uani 1 1 d . . . H29 H 0.3788 0.2776 0.1859 0.048 Uiso 1 1 calc R . . C30 C 0.5018(3) 0.25418(8) 0.3282(3) 0.0359(7) Uani 1 1 d . . . H30 H 0.5210 0.2766 0.3725 0.043 Uiso 1 1 calc R . . C31 C 0.5583(3) 0.22100(8) 0.3732(2) 0.0308(7) Uani 1 1 d . . . H31 H 0.6184 0.2212 0.4476 0.037 Uiso 1 1 calc R . . C32 C 0.7339(4) 0.02466(9) 0.6414(3) 0.0462(9) Uani 1 1 d . . . H32A H 0.3385 0.0633 0.2454 0.041 Uiso 1 1 calc R . . H32B H 0.4663 0.0427 0.1761 0.041 Uiso 1 1 calc R . . C33 C 0.4046(4) 0.09265(9) 0.0933(3) 0.0408(8) Uani 1 1 d . . . H33A H 0.3482 0.1146 0.1187 0.049 Uiso 1 1 calc R . . H33B H 0.5002 0.1015 0.0649 0.049 Uiso 1 1 calc R . . C34 C 0.3200(4) 0.07331(11) -0.0138(3) 0.0600(10) Uani 1 1 d . . . H34A H 0.2266 0.0632 0.0151 0.072 Uiso 1 1 calc R . . H34B H 0.3789 0.0523 -0.0434 0.072 Uiso 1 1 calc R . . C35 C 0.2874(5) 0.10041(13) -0.1192(3) 0.0793(14) Uani 1 1 d . . . H35A H 0.2232 0.1203 -0.0914 0.119 Uiso 1 1 calc R . . H35B H 0.2382 0.0872 -0.1890 0.119 Uiso 1 1 calc R . . H35C H 0.3796 0.1112 -0.1453 0.119 Uiso 1 1 calc R . . B1 B 0.6046(3) 0.14980(9) 0.3662(3) 0.0238(7) Uani 1 1 d . . . 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 Mg1 0.0299(5) 0.0242(5) 0.0278(5) 0.0044(4) -0.0013(4) -0.0001(4) N1 0.0241(12) 0.0237(13) 0.0231(11) 0.0002(9) -0.0002(9) -0.0018(10) N2 0.0285(13) 0.0236(13) 0.0305(13) -0.0006(10) 0.0006(10) 0.0028(10) N3 0.0220(12) 0.0238(13) 0.0315(12) -0.0001(9) 0.0018(9) -0.0009(10) C1 0.0301(16) 0.0216(15) 0.0277(15) 0.0024(11) 0.0031(11) -0.0036(12) C2 0.0356(17) 0.0320(17) 0.0333(16) 0.0091(13) -0.0025(12) 0.0020(13) C3 0.0386(18) 0.0265(16) 0.0386(17) -0.0058(12) 0.0061(13) 0.0024(13) C4 0.0324(17) 0.0283(17) 0.0411(17) -0.0040(13) -0.0067(13) -0.0032(13) C5 0.0240(15) 0.0269(16) 0.0377(16) 0.0013(12) 0.0048(12) -0.0031(12) C6 0.0226(14) 0.0281(16) 0.0289(15) 0.0049(12) 0.0040(11) 0.0005(12) C7 0.0209(14) 0.0189(14) 0.0296(15) 0.0004(11) 0.0009(11) 0.0047(11) C8 0.0308(16) 0.0276(16) 0.0349(16) -0.0016(12) -0.0018(12) 0.0002(13) C9 0.0293(16) 0.0264(17) 0.0517(19) 0.0035(13) 0.0025(14) -0.0046(13) C10 0.0308(16) 0.0306(17) 0.0330(16) 0.0067(12) 0.0043(12) 0.0002(13) C11 0.0267(15) 0.0256(15) 0.0275(15) 0.0036(11) 0.0022(11) 0.0040(12) C12 0.0308(16) 0.0260(15) 0.0259(14) 0.0000(11) -0.0007(11) 0.0014(12) C13 0.0371(18) 0.049(2) 0.0324(16) 0.0043(14) 0.0078(13) 0.0072(15) C14 0.0426(19) 0.045(2) 0.0302(16) 0.0003(14) -0.0044(13) 0.0045(15) C15 0.0279(15) 0.0343(17) 0.0269(15) 0.0076(12) 0.0017(11) 0.0013(13) C16 0.0461(19) 0.048(2) 0.0324(16) -0.0056(14) 0.0031(14) 0.0028(16) C17 0.046(2) 0.047(2) 0.0316(16) 0.0109(14) -0.0017(14) 0.0021(16) C18 0.076(3) 0.062(2) 0.0323(18) 0.0136(16) 0.0062(17) 0.016(2) C19 0.051(2) 0.048(2) 0.0402(18) -0.0045(15) 0.0111(15) 0.0042(17) C20 0.050(2) 0.0302(18) 0.0530(19) -0.0039(14) 0.0019(15) 0.0030(15) C21 0.0352(18) 0.042(2) 0.055(2) -0.0060(15) 0.0055(14) 0.0099(15) C22 0.048(2) 0.040(2) 0.063(2) 0.0159(17) -0.0185(17) 0.0006(16) C23 0.0291(16) 0.0351(18) 0.0497(19) 0.0088(14) 0.0091(13) -0.0032(14) C24 0.0266(16) 0.0368(18) 0.0543(19) 0.0055(15) 0.0012(13) 0.0004(14) C25 0.0357(17) 0.0365(18) 0.0405(17) 0.0004(14) 0.0129(13) 0.0010(14) C26 0.0241(15) 0.0231(15) 0.0286(15) -0.0005(11) 0.0010(11) 0.0050(11) C27 0.0361(18) 0.0313(17) 0.0359(17) 0.0027(13) -0.0037(13) -0.0005(13) C28 0.0328(17) 0.044(2) 0.0391(18) 0.0131(14) -0.0050(13) 0.0021(15) C29 0.0327(17) 0.0334(19) 0.055(2) 0.0187(15) 0.0064(15) 0.0028(14) C30 0.0349(17) 0.0232(16) 0.0497(18) 0.0018(13) 0.0047(14) -0.0012(13) C31 0.0290(16) 0.0293(17) 0.0340(16) 0.0032(12) 0.0001(12) 0.0009(13) C32 0.049(2) 0.0351(19) 0.053(2) 0.0191(15) -0.0061(16) -0.0050(16) C33 0.047(2) 0.0363(19) 0.0382(17) -0.0032(13) -0.0106(14) 0.0039(15) C34 0.072(3) 0.057(2) 0.048(2) -0.0103(17) -0.0258(18) 0.006(2) C35 0.085(3) 0.091(4) 0.058(2) -0.013(2) -0.026(2) 0.020(3) B1 0.0257(17) 0.0236(17) 0.0221(15) -0.0004(12) 0.0007(12) 0.0013(13)