Electronic Supplementary MAterial for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Alan Cowley' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Texas at Austin 1 University Station A5300 AUSTIN Texas 78712 UNITED STATES OF AMERICA ; _publ_contact_author_email COWLEY@MAIL.UTEXAS.EDU _publ_section_title ; Group 13 decamethylmetallocenium cations ; loop_ _publ_author_name 'A. Cowley' 'Silvia Filipponi' 'John D. Gorden' 'Charles Macdonald' 'Andreas Voigt' data_1 _database_code_depnum_ccdc_archive 'CCDC 199049' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; decamethylaluminocenium tetrachloroaluminate ; _chemical_melting_point 123-124C _chemical_formula_moiety '[c20 h30 al][alcl4]' _chemical_formula_sum 'C20 H30 Al2 Cl4' _chemical_formula_weight 466.20 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.75480(10) _cell_length_b 17.3747(3) _cell_length_c 18.0806(4) _cell_angle_alpha 85.7100(7) _cell_angle_beta 83.6011(8) _cell_angle_gamma 84.7879(7) _cell_volume 2405.79(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 32448 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 25.06 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; crystals were covered in perfluoro(poly)ether and rapidly placed in the stream of cold N2 ; _diffrn_ambient_temperature 153(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32448 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.06 _reflns_number_total 8499 _reflns_number_gt 6324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'collect software, nonius b.v. 1998' _computing_cell_refinement denzo-smn _computing_data_reduction denzo-smn _computing_structure_solution 'sir92(altomare et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'shelxtl-plus, xp, siemens, 1994' _computing_publication_material 'shelxtl-plus, xcif, siemens, 1994' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+2.7586P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8499 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.771 _refine_ls_shift/su_mean 0.014 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 C10 C 0.7615(3) -0.43763(15) 0.75932(15) 0.0247(6) Uani 1 1 d . . . C11 C 0.4138(4) -0.55663(15) 0.67296(15) 0.0254(6) Uani 1 1 d . . . C12 C 0.4164(4) -0.47576(15) 0.65175(15) 0.0253(6) Uani 1 1 d . . . C13 C 0.3218(4) -0.43397(15) 0.71078(15) 0.0246(6) Uani 1 1 d . . . C14 C 0.2615(3) -0.48886(16) 0.76900(15) 0.0252(6) Uani 1 1 d . . . C15 C 0.3192(4) -0.56485(15) 0.74536(15) 0.0259(6) Uani 1 1 d . . . C16 C 0.6672(3) -0.44778(16) 0.83211(15) 0.0246(6) Uani 1 1 d . . . C17 C 0.6686(4) -0.52945(16) 0.85170(15) 0.0255(6) Uani 1 1 d . . . C18 C 0.7630(4) -0.56940(16) 0.79145(15) 0.0258(6) Uani 1 1 d . . . C19 C 0.8202(3) -0.51296(16) 0.73432(15) 0.0256(6) Uani 1 1 d . . . C20 C 0.6384(3) 0.08591(15) 0.68961(16) 0.0256(6) Uani 1 1 d . . . C21 C 0.3035(3) -0.08157(15) 0.73194(16) 0.0251(6) Uani 1 1 d . . . C22 C 0.2290(3) -0.00359(15) 0.72041(16) 0.0243(6) Uani 1 1 d . . . C23 C 0.2267(3) 0.03354(15) 0.78907(16) 0.0244(6) Uani 1 1 d . . . C24 C 0.2973(4) -0.02155(16) 0.84288(16) 0.0274(6) Uani 1 1 d . . . C25 C 0.3452(3) -0.09294(15) 0.80783(16) 0.0266(6) Uani 1 1 d . . . C26 C 0.6776(3) 0.07744(15) 0.76569(16) 0.0257(6) Uani 1 1 d . . . C27 C 0.7505(3) -0.00017(15) 0.78023(15) 0.0237(6) Uani 1 1 d . . . C28 C 0.7560(3) -0.03999(15) 0.71307(15) 0.0225(6) Uani 1 1 d . . . C29 C 0.6872(3) 0.01290(15) 0.65727(15) 0.0244(6) Uani 1 1 d . . . C101 C 0.7964(4) -0.36139(16) 0.71827(16) 0.0314(7) Uani 1 1 d . . . H10A H 0.8891 -0.3398 0.7387 0.047 Uiso 1 1 calc R . . H10B H 0.6932 -0.3265 0.7235 0.047 Uiso 1 1 calc R . . H10C H 0.8293 -0.3691 0.6664 0.047 Uiso 1 1 calc R . . C111 C 0.4927(4) -0.62229(17) 0.62706(17) 0.0386(8) Uani 1 1 d . . . H11A H 0.4093 -0.6360 0.5959 0.058 Uiso 1 1 calc R . . H11B H 0.5249 -0.6662 0.6596 0.058 Uiso 1 1 calc R . . H11C H 0.5943 -0.6065 0.5964 0.058 Uiso 1 1 calc R . . C121 C 0.4987(4) -0.43969(17) 0.57999(16) 0.0359(7) Uani 1 1 d . . . H12A H 0.5868 -0.4759 0.5578 0.054 Uiso 1 1 calc R . . H12B H 0.5504 -0.3939 0.5898 0.054 Uiso 1 1 calc R . . H12C H 0.4114 -0.4263 0.5465 0.054 Uiso 1 1 calc R . . C131 C 0.2917(4) -0.34704(16) 0.70954(18) 0.0333(7) Uani 1 1 d . . . H13A H 0.3984 -0.3244 0.6919 0.050 Uiso 1 1 calc R . . H13B H 0.2530 -0.3318 0.7590 0.050 Uiso 1 1 calc R . . H13C H 0.2046 -0.3295 0.6769 0.050 Uiso 1 1 calc R . . C141 C 0.1550(4) -0.47028(17) 0.84110(16) 0.0313(7) Uani 1 1 d . . . H14A H 0.1534 -0.4159 0.8477 0.047 Uiso 1 1 calc R . . H14B H 0.2055 -0.4992 0.8818 0.047 Uiso 1 1 calc R . . H14C H 0.0382 -0.4838 0.8399 0.047 Uiso 1 1 calc R . . C151 C 0.2806(4) -0.64022(16) 0.78806(17) 0.0350(7) Uani 1 1 d . . . H15A H 0.1995 -0.6653 0.7636 0.053 Uiso 1 1 calc R . . H15B H 0.2312 -0.6302 0.8378 0.053 Uiso 1 1 calc R . . H15C H 0.3864 -0.6732 0.7900 0.053 Uiso 1 1 calc R . . C161 C 0.5866(4) -0.38423(17) 0.88019(17) 0.0347(7) Uani 1 1 d . . . H16A H 0.4702 -0.3950 0.8992 0.052 Uiso 1 1 calc R . . H16B H 0.5838 -0.3357 0.8510 0.052 Uiso 1 1 calc R . . H16C H 0.6546 -0.3814 0.9210 0.052 Uiso 1 1 calc R . . C171 C 0.5881(4) -0.56664(18) 0.92314(16) 0.0366(7) Uani 1 1 d . . . H17A H 0.5708 -0.6195 0.9161 0.055 Uiso 1 1 calc R . . H17B H 0.4780 -0.5391 0.9377 0.055 Uiso 1 1 calc R . . H17C H 0.6639 -0.5651 0.9614 0.055 Uiso 1 1 calc R . . C181 C 0.7946(4) -0.65594(17) 0.79040(18) 0.0380(8) Uani 1 1 d . . . H18A H 0.8840 -0.6740 0.8217 0.057 Uiso 1 1 calc R . . H18B H 0.8307 -0.6698 0.7403 0.057 Uiso 1 1 calc R . . H18C H 0.6891 -0.6793 0.8086 0.057 Uiso 1 1 calc R . . C191 C 0.9254(4) -0.52885(17) 0.66122(16) 0.0322(7) Uani 1 1 d . . . H19A H 1.0449 -0.5202 0.6643 0.048 Uiso 1 1 calc R . . H19B H 0.8807 -0.4948 0.6222 0.048 Uiso 1 1 calc R . . H19C H 0.9178 -0.5816 0.6505 0.048 Uiso 1 1 calc R . . C201 C 0.5663(4) 0.15906(17) 0.65062(19) 0.0384(8) Uani 1 1 d . . . H20A H 0.4772 0.1846 0.6835 0.058 Uiso 1 1 calc R . . H20B H 0.5178 0.1468 0.6068 0.058 Uiso 1 1 calc R . . H20C H 0.6580 0.1926 0.6366 0.058 Uiso 1 1 calc R . . C211 C 0.3314(4) -0.14191(16) 0.67552(18) 0.0354(7) Uani 1 1 d . . . H21A H 0.2432 -0.1777 0.6859 0.053 Uiso 1 1 calc R . . H21B H 0.4441 -0.1692 0.6781 0.053 Uiso 1 1 calc R . . H21C H 0.3246 -0.1173 0.6265 0.053 Uiso 1 1 calc R . . C221 C 0.1635(4) 0.03307(17) 0.64988(17) 0.0331(7) Uani 1 1 d . . . H22A H 0.1795 -0.0039 0.6123 0.050 Uiso 1 1 calc R . . H22B H 0.2271 0.0771 0.6329 0.050 Uiso 1 1 calc R . . H22C H 0.0419 0.0495 0.6593 0.050 Uiso 1 1 calc R . . C231 C 0.1554(4) 0.11523(17) 0.80266(18) 0.0360(7) Uani 1 1 d . . . H23A H 0.0341 0.1158 0.8206 0.054 Uiso 1 1 calc R . . H23B H 0.1691 0.1469 0.7569 0.054 Uiso 1 1 calc R . . H23C H 0.2175 0.1352 0.8391 0.054 Uiso 1 1 calc R . . C241 C 0.3111(4) -0.0086(2) 0.92289(17) 0.0413(8) Uani 1 1 d . . . H24A H 0.3298 0.0446 0.9274 0.062 Uiso 1 1 calc R . . H24B H 0.4072 -0.0413 0.9401 0.062 Uiso 1 1 calc R . . H24C H 0.2054 -0.0209 0.9525 0.062 Uiso 1 1 calc R . . C251 C 0.4219(4) -0.16708(17) 0.84337(18) 0.0369(8) Uani 1 1 d . . . H25A H 0.4837 -0.1558 0.8839 0.055 Uiso 1 1 calc R . . H25B H 0.5007 -0.1936 0.8071 0.055 Uiso 1 1 calc R . . H25C H 0.3303 -0.1993 0.8619 0.055 Uiso 1 1 calc R . . C261 C 0.6482(4) 0.14000(17) 0.81989(19) 0.0395(8) Uani 1 1 d . . . H26A H 0.6347 0.1169 0.8699 0.059 Uiso 1 1 calc R . . H26B H 0.5449 0.1724 0.8105 0.059 Uiso 1 1 calc R . . H26C H 0.7463 0.1707 0.8139 0.059 Uiso 1 1 calc R . . C271 C 0.8141(4) -0.03439(17) 0.85241(16) 0.0335(7) Uani 1 1 d . . . H27A H 0.9370 -0.0487 0.8445 0.050 Uiso 1 1 calc R . . H27B H 0.7540 -0.0794 0.8693 0.050 Uiso 1 1 calc R . . H27C H 0.7919 0.0032 0.8893 0.050 Uiso 1 1 calc R . . C281 C 0.8274(4) -0.12222(16) 0.70241(17) 0.0318(7) Uani 1 1 d . . . H28A H 0.7618 -0.1446 0.6687 0.048 Uiso 1 1 calc R . . H28B H 0.8188 -0.1516 0.7496 0.048 Uiso 1 1 calc R . . H28C H 0.9473 -0.1230 0.6821 0.048 Uiso 1 1 calc R . . C291 C 0.6741(4) -0.00395(18) 0.57797(16) 0.0366(7) Uani 1 1 d . . . H29A H 0.7800 0.0073 0.5479 0.055 Uiso 1 1 calc R . . H29B H 0.5781 0.0277 0.5595 0.055 Uiso 1 1 calc R . . H29C H 0.6558 -0.0576 0.5758 0.055 Uiso 1 1 calc R . . Al1 Al 0.54096(10) -0.50171(4) 0.75195(4) 0.02082(19) Uani 1 1 d . . . Al2 Al 0.49088(10) -0.00254(4) 0.74980(4) 0.02023(19) Uani 1 1 d . . . Al3 Al 0.06756(11) -0.74058(5) 1.01743(5) 0.0299(2) Uani 1 1 d . . . Al4 Al 0.93087(12) -0.25179(5) 0.48388(5) 0.0310(2) Uani 1 1 d . . . Cl31 Cl -0.11625(14) -0.80199(8) 0.97229(6) 0.0739(4) Uani 1 1 d . . . Cl32 Cl 0.32631(11) -0.78349(6) 0.97951(5) 0.0523(2) Uani 1 1 d . . . Cl33 Cl 0.03166(13) -0.62027(5) 0.98484(5) 0.0566(3) Uani 1 1 d . . . Cl34 Cl 0.02734(11) -0.75290(4) 1.13657(4) 0.0377(2) Uani 1 1 d . . . Cl41 Cl 1.04756(15) -0.36049(6) 0.52220(5) 0.0703(3) Uani 1 1 d . . . Cl42 Cl 0.93230(13) -0.25049(5) 0.36568(4) 0.0460(2) Uani 1 1 d . . . Cl43 Cl 1.07132(14) -0.15902(7) 0.50967(6) 0.0739(4) Uani 1 1 d . . . Cl44 Cl 0.66894(10) -0.23429(5) 0.53359(5) 0.0447(2) 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 C10 0.0232(14) 0.0262(15) 0.0259(16) -0.0031(12) -0.0042(12) -0.0046(11) C11 0.0318(16) 0.0246(15) 0.0219(15) -0.0048(11) -0.0060(12) -0.0069(12) C12 0.0289(15) 0.0253(15) 0.0231(15) -0.0008(12) -0.0068(12) -0.0047(12) C13 0.0254(15) 0.0236(14) 0.0257(16) -0.0009(12) -0.0077(12) -0.0016(11) C14 0.0204(14) 0.0282(15) 0.0272(16) -0.0037(12) -0.0023(12) -0.0029(11) C15 0.0279(15) 0.0247(15) 0.0260(16) -0.0008(12) -0.0036(12) -0.0069(12) C16 0.0246(15) 0.0294(15) 0.0212(15) -0.0025(12) -0.0055(12) -0.0044(12) C17 0.0280(15) 0.0283(15) 0.0204(15) -0.0003(12) -0.0059(12) -0.0006(12) C18 0.0244(15) 0.0279(15) 0.0247(16) -0.0020(12) -0.0032(12) 0.0018(12) C19 0.0221(14) 0.0299(15) 0.0253(16) -0.0045(12) -0.0027(12) -0.0031(12) C20 0.0199(14) 0.0204(14) 0.0361(17) 0.0019(12) -0.0011(12) -0.0041(11) C21 0.0190(14) 0.0231(14) 0.0339(17) -0.0016(12) -0.0022(12) -0.0064(11) C22 0.0188(14) 0.0236(14) 0.0309(16) -0.0016(12) -0.0037(12) -0.0030(11) C23 0.0156(13) 0.0260(14) 0.0306(16) -0.0033(12) 0.0020(11) -0.0014(11) C24 0.0223(15) 0.0322(16) 0.0268(16) -0.0002(12) 0.0017(12) -0.0051(12) C25 0.0204(14) 0.0245(15) 0.0346(17) 0.0032(12) -0.0011(12) -0.0058(11) C26 0.0195(14) 0.0229(14) 0.0355(17) -0.0041(12) -0.0010(12) -0.0064(11) C27 0.0166(13) 0.0255(14) 0.0293(16) 0.0002(12) -0.0037(11) -0.0042(11) C28 0.0157(13) 0.0239(14) 0.0270(16) -0.0011(12) -0.0007(11) 0.0003(11) C29 0.0196(14) 0.0274(15) 0.0254(16) -0.0004(12) 0.0018(11) -0.0042(11) C101 0.0341(17) 0.0292(16) 0.0318(17) -0.0010(13) -0.0012(13) -0.0107(13) C111 0.056(2) 0.0280(16) 0.0321(18) -0.0088(13) 0.0008(15) -0.0075(15) C121 0.052(2) 0.0315(17) 0.0247(17) 0.0004(13) -0.0055(14) -0.0079(14) C131 0.0369(17) 0.0235(15) 0.0398(19) -0.0019(13) -0.0068(14) -0.0001(13) C141 0.0261(15) 0.0344(16) 0.0321(17) -0.0050(13) 0.0028(13) 0.0001(13) C151 0.0388(18) 0.0278(16) 0.0385(19) 0.0024(13) -0.0010(14) -0.0104(13) C161 0.0447(19) 0.0323(17) 0.0284(17) -0.0113(13) -0.0010(14) -0.0065(14) C171 0.0456(19) 0.0374(17) 0.0246(17) 0.0030(13) 0.0003(14) -0.0014(14) C181 0.0382(18) 0.0300(17) 0.043(2) 0.0015(14) -0.0006(15) 0.0050(14) C191 0.0303(16) 0.0377(17) 0.0270(17) -0.0052(13) 0.0033(13) 0.0003(13) C201 0.0358(18) 0.0259(16) 0.051(2) 0.0076(14) 0.0008(15) -0.0028(13) C211 0.0336(17) 0.0256(16) 0.049(2) -0.0091(14) -0.0078(15) -0.0018(13) C221 0.0301(16) 0.0344(17) 0.0355(18) 0.0007(13) -0.0100(13) -0.0012(13) C231 0.0290(16) 0.0330(17) 0.044(2) -0.0107(14) 0.0039(14) 0.0048(13) C241 0.0435(19) 0.054(2) 0.0259(18) -0.0012(15) -0.0004(14) -0.0063(16) C251 0.0343(17) 0.0303(16) 0.045(2) 0.0107(14) -0.0056(15) -0.0063(13) C261 0.0363(18) 0.0297(17) 0.055(2) -0.0168(15) -0.0061(16) -0.0040(14) C271 0.0324(17) 0.0370(17) 0.0323(17) -0.0041(13) -0.0077(13) -0.0031(13) C281 0.0302(16) 0.0270(15) 0.0364(18) -0.0037(13) -0.0005(13) 0.0046(12) C291 0.0376(18) 0.0419(18) 0.0289(18) 0.0015(14) -0.0012(14) -0.0021(14) Al1 0.0240(4) 0.0191(4) 0.0193(4) -0.0025(3) -0.0009(3) -0.0022(3) Al2 0.0191(4) 0.0187(4) 0.0230(4) -0.0017(3) -0.0016(3) -0.0023(3) Al3 0.0304(5) 0.0374(5) 0.0225(5) -0.0045(4) -0.0033(4) -0.0029(4) Al4 0.0322(5) 0.0370(5) 0.0232(5) -0.0036(4) 0.0002(4) -0.0029(4) Cl31 0.0636(7) 0.1235(10) 0.0447(6) -0.0301(6) -0.0011(5) -0.0480(7) Cl32 0.0393(5) 0.0634(6) 0.0520(6) -0.0172(4) 0.0001(4) 0.0119(4) Cl33 0.0689(6) 0.0490(5) 0.0424(5) 0.0167(4) 0.0067(4) 0.0146(4) Cl34 0.0553(5) 0.0343(4) 0.0232(4) -0.0009(3) -0.0063(3) 0.0001(3) Cl41 0.0763(7) 0.0772(7) 0.0419(6) 0.0213(5) 0.0091(5) 0.0381(6) Cl42 0.0747(6) 0.0365(4) 0.0249(4) -0.0050(3) -0.0074(4) 0.0114(4) Cl43 0.0640(7) 0.1071(9) 0.0585(7) -0.0384(6) 0.0157(5) -0.0495(6) Cl44 0.0335(4) 0.0455(5) 0.0536(5) -0.0104(4) 0.0061(4) -0.0029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C10 C19 1.435(4) . ? C10 C16 1.439(4) . ? C10 C101 1.501(4) . ? C10 Al1 2.145(3) . ? C11 C12 1.430(4) . ? C11 C15 1.431(4) . ? C11 C111 1.505(4) . ? C11 Al1 2.147(3) . ? C12 C13 1.431(4) . ? C12 C121 1.500(4) . ? C12 Al1 2.146(3) . ? C13 C14 1.434(4) . ? C13 C131 1.506(4) . ? C13 Al1 2.148(3) . ? C14 C15 1.435(4) . ? C14 C141 1.503(4) . ? C14 Al1 2.148(3) . ? C15 C151 1.506(4) . ? C15 Al1 2.141(3) . ? C16 C17 1.436(4) . ? C16 C161 1.504(4) . ? C16 Al1 2.150(3) . ? C17 C18 1.431(4) . ? C17 C171 1.498(4) . ? C17 Al1 2.155(3) . ? C18 C19 1.432(4) . ? C18 C181 1.503(4) . ? C18 Al1 2.154(3) . ? C19 C191 1.504(4) . ? C19 Al1 2.147(3) . ? C20 C26 1.436(4) . ? C20 C29 1.438(4) . ? C20 C201 1.500(4) . ? C20 Al2 2.156(3) . ? C21 C22 1.434(4) . ? C21 C25 1.440(4) . ? C21 C211 1.502(4) . ? C21 Al2 2.153(3) . ? C22 C23 1.439(4) . ? C22 C221 1.501(4) . ? C22 Al2 2.158(3) . ? C23 C24 1.431(4) . ? C23 C231 1.503(4) . ? C23 Al2 2.145(3) . ? C24 C25 1.435(4) . ? C24 C241 1.497(4) . ? C24 Al2 2.154(3) . ? C25 C251 1.499(4) . ? C25 Al2 2.158(3) . ? C26 C27 1.431(4) . ? C26 C261 1.503(4) . ? C26 Al2 2.151(3) . ? C27 C28 1.437(4) . ? C27 C271 1.508(4) . ? C27 Al2 2.150(3) . ? C28 C29 1.428(4) . ? C28 C281 1.503(4) . ? C28 Al2 2.146(3) . ? C29 C291 1.501(4) . ? C29 Al2 2.151(3) . ? Al3 Cl31 2.1218(13) . ? Al3 Cl33 2.1309(12) . ? Al3 Cl32 2.1331(12) . ? Al3 Cl34 2.1394(11) . ? Al4 Cl41 2.1213(13) . ? Al4 Cl43 2.1321(13) . ? Al4 Cl44 2.1326(12) . ? Al4 Cl42 2.1344(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C19 C10 C16 108.0(2) . . ? C19 C10 C101 126.3(2) . . ? C16 C10 C101 125.7(2) . . ? C19 C10 Al1 70.54(15) . . ? C16 C10 Al1 70.62(15) . . ? C101 C10 Al1 125.9(2) . . ? C12 C11 C15 108.1(2) . . ? C12 C11 C111 126.4(2) . . ? C15 C11 C111 125.5(2) . . ? C12 C11 Al1 70.51(15) . . ? C15 C11 Al1 70.25(15) . . ? C111 C11 Al1 125.9(2) . . ? C11 C12 C13 107.9(2) . . ? C11 C12 C121 126.9(3) . . ? C13 C12 C121 125.1(2) . . ? C11 C12 Al1 70.58(16) . . ? C13 C12 Al1 70.60(16) . . ? C121 C12 Al1 125.5(2) . . ? C12 C13 C14 108.3(2) . . ? C12 C13 C131 124.5(2) . . ? C14 C13 C131 127.2(2) . . ? C12 C13 Al1 70.46(16) . . ? C14 C13 Al1 70.49(15) . . ? C131 C13 Al1 125.3(2) . . ? C13 C14 C15 107.5(2) . . ? C13 C14 C141 126.3(2) . . ? C15 C14 C141 126.2(2) . . ? C13 C14 Al1 70.50(15) . . ? C15 C14 Al1 70.17(15) . . ? C141 C14 Al1 125.4(2) . . ? C11 C15 C14 108.2(2) . . ? C11 C15 C151 125.9(3) . . ? C14 C15 C151 125.8(3) . . ? C11 C15 Al1 70.74(15) . . ? C14 C15 Al1 70.72(15) . . ? C151 C15 Al1 126.1(2) . . ? C17 C16 C10 107.8(2) . . ? C17 C16 C161 126.0(2) . . ? C10 C16 C161 126.2(2) . . ? C17 C16 Al1 70.71(15) . . ? C10 C16 Al1 70.22(15) . . ? C161 C16 Al1 126.0(2) . . ? C18 C17 C16 108.0(2) . . ? C18 C17 C171 125.8(3) . . ? C16 C17 C171 126.2(2) . . ? C18 C17 Al1 70.54(16) . . ? C16 C17 Al1 70.32(15) . . ? C171 C17 Al1 125.5(2) . . ? C17 C18 C19 108.3(2) . . ? C17 C18 C181 124.6(2) . . ? C19 C18 C181 127.1(2) . . ? C17 C18 Al1 70.67(15) . . ? C19 C18 Al1 70.29(16) . . ? C181 C18 Al1 124.9(2) . . ? C18 C19 C10 107.9(2) . . ? C18 C19 C191 126.6(2) . . ? C10 C19 C191 125.5(2) . . ? C18 C19 Al1 70.81(16) . . ? C10 C19 Al1 70.39(15) . . ? C191 C19 Al1 125.0(2) . . ? C26 C20 C29 107.7(2) . . ? C26 C20 C201 125.6(3) . . ? C29 C20 C201 126.6(3) . . ? C26 C20 Al2 70.37(15) . . ? C29 C20 Al2 70.33(14) . . ? C201 C20 Al2 126.62(19) . . ? C22 C21 C25 108.2(2) . . ? C22 C21 C211 126.4(3) . . ? C25 C21 C211 125.4(2) . . ? C22 C21 Al2 70.75(15) . . ? C25 C21 Al2 70.66(15) . . ? C211 C21 Al2 124.98(19) . . ? C21 C22 C23 107.7(2) . . ? C21 C22 C221 126.5(3) . . ? C23 C22 C221 125.8(2) . . ? C21 C22 Al2 70.39(15) . . ? C23 C22 Al2 70.00(15) . . ? C221 C22 Al2 125.40(19) . . ? C24 C23 C22 108.3(2) . . ? C24 C23 C231 126.0(3) . . ? C22 C23 C231 125.7(3) . . ? C24 C23 Al2 70.88(15) . . ? C22 C23 Al2 70.93(15) . . ? C231 C23 Al2 125.84(19) . . ? C23 C24 C25 108.1(2) . . ? C23 C24 C241 126.2(3) . . ? C25 C24 C241 125.7(3) . . ? C23 C24 Al2 70.25(15) . . ? C25 C24 Al2 70.70(15) . . ? C241 C24 Al2 126.9(2) . . ? C24 C25 C21 107.8(2) . . ? C24 C25 C251 126.7(3) . . ? C21 C25 C251 125.5(3) . . ? C24 C25 Al2 70.41(15) . . ? C21 C25 Al2 70.31(15) . . ? C251 C25 Al2 125.65(19) . . ? C27 C26 C20 108.2(2) . . ? C27 C26 C261 126.4(3) . . ? C20 C26 C261 125.4(3) . . ? C27 C26 Al2 70.51(15) . . ? C20 C26 Al2 70.69(15) . . ? C261 C26 Al2 124.95(19) . . ? C26 C27 C28 107.9(2) . . ? C26 C27 C271 126.6(3) . . ? C28 C27 C271 125.6(2) . . ? C26 C27 Al2 70.62(15) . . ? C28 C27 Al2 70.34(15) . . ? C271 C27 Al2 125.50(19) . . ? C29 C28 C27 108.2(2) . . ? C29 C28 C281 125.8(3) . . ? C27 C28 C281 126.0(2) . . ? C29 C28 Al2 70.77(15) . . ? C27 C28 Al2 70.60(15) . . ? C281 C28 Al2 125.91(19) . . ? C28 C29 C20 108.1(2) . . ? C28 C29 C291 125.9(3) . . ? C20 C29 C291 126.0(3) . . ? C28 C29 Al2 70.42(15) . . ? C20 C29 Al2 70.66(15) . . ? C291 C29 Al2 126.2(2) . . ? C15 Al1 C10 179.39(11) . . ? C15 Al1 C12 65.40(11) . . ? C10 Al1 C12 114.71(11) . . ? C15 Al1 C19 141.50(11) . . ? C10 Al1 C19 39.07(10) . . ? C12 Al1 C19 114.13(11) . . ? C15 Al1 C11 39.00(10) . . ? C10 Al1 C11 141.45(11) . . ? C12 Al1 C11 38.91(10) . . ? C19 Al1 C11 114.75(11) . . ? C15 Al1 C13 65.31(11) . . ? C10 Al1 C13 114.37(11) . . ? C12 Al1 C13 38.94(10) . . ? C19 Al1 C13 140.29(11) . . ? C11 Al1 C13 65.18(11) . . ? C15 Al1 C14 39.11(10) . . ? C10 Al1 C14 140.32(11) . . ? C12 Al1 C14 65.51(11) . . ? C19 Al1 C14 179.23(11) . . ? C11 Al1 C14 65.46(11) . . ? C13 Al1 C14 39.01(10) . . ? C15 Al1 C16 140.39(11) . . ? C10 Al1 C16 39.16(10) . . ? C12 Al1 C16 141.72(11) . . ? C19 Al1 C16 65.51(10) . . ? C11 Al1 C16 179.28(11) . . ? C13 Al1 C16 115.11(11) . . ? C14 Al1 C16 114.30(11) . . ? C15 Al1 C18 115.04(11) . . ? C10 Al1 C18 65.29(11) . . ? C12 Al1 C18 140.26(11) . . ? C19 Al1 C18 38.90(10) . . ? C11 Al1 C18 114.49(11) . . ? C13 Al1 C18 179.06(11) . . ? C14 Al1 C18 141.80(11) . . ? C16 Al1 C18 65.24(11) . . ? C15 Al1 C17 114.50(11) . . ? C10 Al1 C17 65.40(11) . . ? C12 Al1 C17 179.01(11) . . ? C19 Al1 C17 65.28(11) . . ? C11 Al1 C17 140.41(11) . . ? C13 Al1 C17 142.01(11) . . ? C14 Al1 C17 115.09(11) . . ? C16 Al1 C17 38.97(10) . . ? C18 Al1 C17 38.79(10) . . ? C23 Al2 C28 178.64(11) . . ? C23 Al2 C27 140.10(11) . . ? C28 Al2 C27 39.07(10) . . ? C23 Al2 C29 142.54(11) . . ? C28 Al2 C29 38.81(10) . . ? C27 Al2 C29 65.29(11) . . ? C23 Al2 C26 114.74(11) . . ? C28 Al2 C26 65.28(10) . . ? C27 Al2 C26 38.87(10) . . ? C29 Al2 C26 65.29(11) . . ? C23 Al2 C21 65.30(10) . . ? C28 Al2 C21 114.72(11) . . ? C27 Al2 C21 141.75(11) . . ? C29 Al2 C21 114.00(11) . . ? C26 Al2 C21 178.97(11) . . ? C23 Al2 C24 38.88(11) . . ? C28 Al2 C24 139.78(11) . . ? C27 Al2 C24 114.20(11) . . ? C29 Al2 C24 178.29(11) . . ? C26 Al2 C24 115.44(11) . . ? C21 Al2 C24 65.28(11) . . ? C23 Al2 C20 115.69(10) . . ? C28 Al2 C20 65.25(10) . . ? C27 Al2 C20 65.27(10) . . ? C29 Al2 C20 39.02(10) . . ? C26 Al2 C20 38.94(11) . . ? C21 Al2 C20 140.04(12) . . ? C24 Al2 C20 142.51(11) . . ? C23 Al2 C25 65.23(10) . . ? C28 Al2 C25 113.85(11) . . ? C27 Al2 C25 114.83(11) . . ? C29 Al2 C25 139.60(11) . . ? C26 Al2 C25 141.99(12) . . ? C21 Al2 C25 39.03(11) . . ? C24 Al2 C25 38.88(11) . . ? C20 Al2 C25 178.58(11) . . ? C23 Al2 C22 39.07(11) . . ? C28 Al2 C22 141.76(11) . . ? C27 Al2 C22 179.14(11) . . ? C29 Al2 C22 115.24(11) . . ? C26 Al2 C22 140.54(11) . . ? C21 Al2 C22 38.85(10) . . ? C24 Al2 C22 65.30(11) . . ? C20 Al2 C22 114.65(11) . . ? C25 Al2 C22 65.28(11) . . ? Cl31 Al3 Cl33 110.16(6) . . ? Cl31 Al3 Cl32 110.38(6) . . ? Cl33 Al3 Cl32 109.25(5) . . ? Cl31 Al3 Cl34 109.29(5) . . ? Cl33 Al3 Cl34 107.67(5) . . ? Cl32 Al3 Cl34 110.05(5) . . ? Cl41 Al4 Cl43 111.28(7) . . ? Cl41 Al4 Cl44 110.63(5) . . ? Cl43 Al4 Cl44 108.57(5) . . ? Cl41 Al4 Cl42 108.35(5) . . ? Cl43 Al4 Cl42 108.71(5) . . ? Cl44 Al4 Cl42 109.28(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.970 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.061 # Attachment '(MCp2B)(AlCl4).cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 665221' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'decamethylborocenium tetrachloroaluminate' _chemical_melting_point ? _chemical_formula_moiety '[C20H30B] [AlCl4]' _chemical_formula_sum 'C20 H30 Al B Cl4' _chemical_formula_weight 450.03 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.133(3) _cell_length_b 13.611(3) _cell_length_c 20.493(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.30(3) _cell_angle_gamma 90.00 _cell_volume 4778.8(16) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 19718 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.535 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19718 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10898 _reflns_number_gt 7129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus, XP, Siemens, 1994' _computing_publication_material 'SHELXTL-Plus, XCIF, Siemens, 1994' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+8.0030P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10898 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.2117 _refine_ls_wR_factor_gt 0.1889 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 C1 C 1.05417(19) 0.8344(3) 0.37240(16) 0.0314(7) Uani 1 1 d . . . C2 C 1.0984(2) 0.8461(3) 0.43605(19) 0.0384(8) Uani 1 1 d . . . C3 C 1.0475(2) 0.8573(3) 0.48510(18) 0.0429(9) Uani 1 1 d . . . C4 C 0.9677(2) 0.8617(3) 0.45841(19) 0.0411(9) Uani 1 1 d . . . C5 C 0.9702(2) 0.8526(3) 0.39328(18) 0.0354(8) Uani 1 1 d . . . C6 C 1.0827(2) 0.9019(3) 0.31749(19) 0.0417(9) Uani 1 1 d . . . H6A H 1.0514 0.8903 0.2781 0.063 Uiso 1 1 calc R . . H6B H 1.1377 0.8879 0.3084 0.063 Uiso 1 1 calc R . . H6C H 1.0772 0.9707 0.3310 0.063 Uiso 1 1 calc R . . C7 C 1.1861(2) 0.8498(4) 0.4397(2) 0.0520(11) Uani 1 1 d . . . H7A H 1.2079 0.8390 0.3962 0.078 Uiso 1 1 calc R . . H7B H 1.2050 0.7985 0.4694 0.078 Uiso 1 1 calc R . . H7C H 1.2026 0.9143 0.4560 0.078 Uiso 1 1 calc R . . C8 C 1.0644(3) 0.8667(4) 0.5570(2) 0.0606(12) Uani 1 1 d . . . H8A H 1.0153 0.8741 0.5807 0.091 Uiso 1 1 calc R . . H8B H 1.0973 0.9245 0.5646 0.091 Uiso 1 1 calc R . . H8C H 1.0917 0.8077 0.5723 0.091 Uiso 1 1 calc R . . C9 C 0.8962(3) 0.8760(4) 0.4991(2) 0.0575(12) Uani 1 1 d . . . H9A H 0.9113 0.8803 0.5452 0.086 Uiso 1 1 calc R . . H9B H 0.8608 0.8203 0.4928 0.086 Uiso 1 1 calc R . . H9C H 0.8699 0.9368 0.4860 0.086 Uiso 1 1 calc R . . C10 C 0.9035(2) 0.8621(3) 0.3466(2) 0.0466(10) Uani 1 1 d . . . H10A H 0.9222 0.8520 0.3020 0.070 Uiso 1 1 calc R . . H10B H 0.8806 0.9278 0.3503 0.070 Uiso 1 1 calc R . . H10C H 0.8638 0.8126 0.3568 0.070 Uiso 1 1 calc R . . C11 C 1.0065(2) 0.6347(3) 0.30546(19) 0.0383(8) Uani 1 1 d . . . C12 C 1.0854(2) 0.6486(3) 0.28524(18) 0.0381(8) Uani 1 1 d . . . C13 C 1.1346(2) 0.6336(3) 0.34051(18) 0.0358(8) Uani 1 1 d . . . C14 C 1.0866(2) 0.6147(3) 0.39549(18) 0.0378(8) Uani 1 1 d . . . C15 C 1.0071(2) 0.6151(3) 0.3737(2) 0.0401(9) Uani 1 1 d . . . C16 C 0.9356(2) 0.6447(3) 0.2626(2) 0.0528(11) Uani 1 1 d . . . H16A H 0.9519 0.6580 0.2176 0.079 Uiso 1 1 calc R . . H16B H 0.9033 0.6990 0.2783 0.079 Uiso 1 1 calc R . . H16C H 0.9055 0.5835 0.2638 0.079 Uiso 1 1 calc R . . C17 C 1.1114(3) 0.6804(4) 0.21890(19) 0.0535(11) Uani 1 1 d . . . H17A H 1.1686 0.6840 0.2181 0.080 Uiso 1 1 calc R . . H17B H 1.0895 0.7452 0.2090 0.080 Uiso 1 1 calc R . . H17C H 1.0934 0.6328 0.1863 0.080 Uiso 1 1 calc R . . C18 C 1.2222(2) 0.6436(3) 0.3406(2) 0.0447(9) Uani 1 1 d . . . H18A H 1.2402 0.6566 0.2962 0.067 Uiso 1 1 calc R . . H18B H 1.2458 0.5826 0.3567 0.067 Uiso 1 1 calc R . . H18C H 1.2375 0.6982 0.3692 0.067 Uiso 1 1 calc R . . C19 C 1.1134(3) 0.6015(3) 0.4649(2) 0.0501(10) Uani 1 1 d . . . H19A H 1.0681 0.5894 0.4928 0.075 Uiso 1 1 calc R . . H19B H 1.1404 0.6611 0.4796 0.075 Uiso 1 1 calc R . . H19C H 1.1491 0.5454 0.4676 0.075 Uiso 1 1 calc R . . C20 C 0.9369(2) 0.6042(4) 0.4160(2) 0.0569(12) Uani 1 1 d . . . H20A H 0.9535 0.5912 0.4610 0.085 Uiso 1 1 calc R . . H20B H 0.9049 0.5494 0.4001 0.085 Uiso 1 1 calc R . . H20C H 0.9062 0.6649 0.4146 0.085 Uiso 1 1 calc R . . C21 C 1.0454(2) 0.6612(3) -0.12586(17) 0.0337(8) Uani 1 1 d . . . C22 C 1.1164(2) 0.6147(3) -0.0933(2) 0.0406(9) Uani 1 1 d . . . C23 C 1.1026(3) 0.6057(3) -0.0288(2) 0.0476(10) Uani 1 1 d . . . C24 C 1.0219(3) 0.6342(3) -0.01477(19) 0.0442(9) Uani 1 1 d . . . C25 C 0.9868(2) 0.6618(3) -0.07031(19) 0.0377(8) Uani 1 1 d . . . C26 C 1.0173(3) 0.6105(3) -0.1877(2) 0.0502(10) Uani 1 1 d . . . H26A H 0.9718 0.6454 -0.2052 0.075 Uiso 1 1 calc R . . H26B H 1.0029 0.5425 -0.1777 0.075 Uiso 1 1 calc R . . H26C H 1.0592 0.6109 -0.2201 0.075 Uiso 1 1 calc R . . C27 C 1.1861(2) 0.5826(3) -0.1309(3) 0.0607(13) Uani 1 1 d . . . H27A H 1.1788 0.5994 -0.1771 0.091 Uiso 1 1 calc R . . H27B H 1.1926 0.5114 -0.1265 0.091 Uiso 1 1 calc R . . H27C H 1.2326 0.6159 -0.1140 0.091 Uiso 1 1 calc R . . C28 C 1.1582(3) 0.5692(5) 0.0232(3) 0.0818(18) Uani 1 1 d . . . H28A H 1.1322 0.5707 0.0657 0.123 Uiso 1 1 calc R . . H28B H 1.2044 0.6116 0.0246 0.123 Uiso 1 1 calc R . . H28C H 1.1740 0.5018 0.0132 0.123 Uiso 1 1 calc R . . C29 C 0.9875(4) 0.6311(4) 0.0520(2) 0.0728(16) Uani 1 1 d . . . H29A H 1.0268 0.6078 0.0832 0.109 Uiso 1 1 calc R . . H29B H 0.9426 0.5864 0.0521 0.109 Uiso 1 1 calc R . . H29C H 0.9703 0.6972 0.0645 0.109 Uiso 1 1 calc R . . C30 C 0.9027(2) 0.6893(3) -0.0802(3) 0.0577(12) Uani 1 1 d . . . H30A H 0.8938 0.7065 -0.1261 0.087 Uiso 1 1 calc R . . H30B H 0.8900 0.7458 -0.0526 0.087 Uiso 1 1 calc R . . H30C H 0.8694 0.6336 -0.0684 0.087 Uiso 1 1 calc R . . C31 C 1.1403(2) 0.8397(3) -0.17983(18) 0.0373(8) Uani 1 1 d . . . C32 C 1.1460(2) 0.8486(3) -0.11100(18) 0.0348(8) Uani 1 1 d . . . C33 C 1.0711(2) 0.8769(3) -0.08689(18) 0.0343(8) Uani 1 1 d . . . C34 C 1.0199(2) 0.8881(3) -0.14144(19) 0.0368(8) Uani 1 1 d . . . C35 C 1.0623(2) 0.8626(3) -0.19866(19) 0.0402(9) Uani 1 1 d . . . C36 C 1.2028(3) 0.8071(4) -0.2256(2) 0.0547(11) Uani 1 1 d . . . H36A H 1.1826 0.8080 -0.2704 0.082 Uiso 1 1 calc R . . H36B H 1.2193 0.7403 -0.2143 0.082 Uiso 1 1 calc R . . H36C H 1.2476 0.8517 -0.2221 0.082 Uiso 1 1 calc R . . C37 C 1.2152(2) 0.8244(3) -0.0692(2) 0.0450(9) Uani 1 1 d . . . H37A H 1.2028 0.8376 -0.0234 0.067 Uiso 1 1 calc R . . H37B H 1.2596 0.8650 -0.0824 0.067 Uiso 1 1 calc R . . H37C H 1.2284 0.7548 -0.0745 0.067 Uiso 1 1 calc R . . C38 C 1.0502(2) 0.8825(3) -0.01551(18) 0.0417(9) Uani 1 1 d . . . H38A H 1.0972 0.8720 0.0111 0.063 Uiso 1 1 calc R . . H38B H 1.0115 0.8318 -0.0054 0.063 Uiso 1 1 calc R . . H38C H 1.0284 0.9475 -0.0059 0.063 Uiso 1 1 calc R . . C39 C 0.9352(2) 0.9176(3) -0.1405(2) 0.0537(11) Uani 1 1 d . . . H39A H 0.9194 0.9315 -0.0956 0.081 Uiso 1 1 calc R . . H39B H 0.9033 0.8639 -0.1581 0.081 Uiso 1 1 calc R . . H39C H 0.9278 0.9765 -0.1673 0.081 Uiso 1 1 calc R . . C40 C 1.0308(3) 0.8562(4) -0.2668(2) 0.0605(12) Uani 1 1 d . . . H40A H 0.9757 0.8756 -0.2671 0.091 Uiso 1 1 calc R . . H40B H 1.0356 0.7885 -0.2826 0.091 Uiso 1 1 calc R . . H40C H 1.0605 0.9002 -0.2952 0.091 Uiso 1 1 calc R . . B1 B 1.0594(2) 0.7217(3) 0.3534(2) 0.0319(8) Uani 1 1 d . . . B2 B 1.0680(2) 0.7729(3) -0.13722(19) 0.0314(8) Uani 1 1 d . . . Al1 Al 0.81620(7) 0.85430(9) 0.11879(5) 0.0407(3) Uani 1 1 d . . . Al2 Al 0.67387(8) 1.17229(10) -0.16388(6) 0.0472(3) Uani 1 1 d . . . Cl1 Cl 0.81477(6) 0.90846(8) 0.02152(5) 0.0464(3) Uani 1 1 d . . . Cl2 Cl 0.78707(7) 0.70235(8) 0.11937(5) 0.0529(3) Uani 1 1 d . . . Cl3 Cl 0.93269(8) 0.87324(9) 0.15608(7) 0.0702(4) Uani 1 1 d . . . Cl4 Cl 0.73674(10) 0.93641(10) 0.17671(7) 0.0869(5) Uani 1 1 d . . . Cl5 Cl 0.69193(7) 1.10309(11) -0.25585(5) 0.0626(3) Uani 1 1 d . . . Cl6 Cl 0.76419(11) 1.12351(13) -0.10073(7) 0.0925(5) Uani 1 1 d . . . Cl7 Cl 0.67761(7) 1.32788(9) -0.17518(7) 0.0659(4) Uani 1 1 d . . . Cl8 Cl 0.56173(8) 1.13299(9) -0.12651(7) 0.0716(4) 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 C1 0.0293(17) 0.0316(18) 0.0334(17) -0.0001(14) -0.0006(14) -0.0019(14) C2 0.0373(19) 0.036(2) 0.041(2) -0.0035(16) -0.0045(15) -0.0013(16) C3 0.059(2) 0.036(2) 0.0334(19) -0.0024(16) -0.0020(17) -0.0007(18) C4 0.046(2) 0.032(2) 0.045(2) -0.0020(16) 0.0106(17) -0.0020(17) C5 0.0316(17) 0.0292(19) 0.045(2) -0.0049(16) -0.0007(15) 0.0000(15) C6 0.042(2) 0.036(2) 0.047(2) 0.0037(17) 0.0027(17) -0.0009(17) C7 0.039(2) 0.062(3) 0.055(3) -0.010(2) -0.0130(18) -0.002(2) C8 0.084(3) 0.060(3) 0.038(2) -0.005(2) -0.005(2) -0.004(3) C9 0.057(3) 0.058(3) 0.057(3) -0.003(2) 0.025(2) 0.002(2) C10 0.0326(19) 0.046(2) 0.061(3) -0.008(2) -0.0034(17) 0.0064(17) C11 0.0376(19) 0.0287(19) 0.048(2) -0.0028(16) -0.0084(16) 0.0014(15) C12 0.0369(19) 0.039(2) 0.0384(19) -0.0051(16) -0.0032(15) 0.0079(16) C13 0.0309(17) 0.0337(19) 0.043(2) 0.0002(16) 0.0002(15) 0.0070(15) C14 0.0381(19) 0.034(2) 0.042(2) 0.0060(16) -0.0020(15) 0.0027(16) C15 0.0367(19) 0.0307(19) 0.053(2) 0.0061(17) 0.0008(16) -0.0025(16) C16 0.042(2) 0.049(3) 0.067(3) -0.015(2) -0.018(2) 0.0025(19) C17 0.060(3) 0.066(3) 0.035(2) -0.005(2) 0.0002(18) 0.015(2) C18 0.0301(18) 0.052(3) 0.052(2) -0.0015(19) 0.0006(16) 0.0059(17) C19 0.053(2) 0.054(3) 0.043(2) 0.018(2) 0.0000(18) 0.004(2) C20 0.043(2) 0.053(3) 0.075(3) 0.017(2) 0.012(2) -0.007(2) C21 0.0325(17) 0.0314(19) 0.0373(18) -0.0048(15) -0.0009(14) -0.0004(15) C22 0.0335(18) 0.0290(19) 0.059(2) 0.0034(17) -0.0034(17) -0.0015(15) C23 0.054(2) 0.038(2) 0.050(2) 0.0090(18) -0.0153(19) -0.0117(19) C24 0.059(2) 0.036(2) 0.038(2) -0.0027(17) 0.0026(18) -0.0128(19) C25 0.0383(19) 0.0299(19) 0.045(2) -0.0049(16) 0.0083(16) -0.0051(15) C26 0.067(3) 0.039(2) 0.045(2) -0.0115(18) -0.006(2) -0.005(2) C27 0.041(2) 0.042(3) 0.099(4) 0.008(2) 0.011(2) 0.0099(19) C28 0.082(4) 0.081(4) 0.082(4) 0.039(3) -0.038(3) -0.015(3) C29 0.111(4) 0.063(3) 0.044(3) -0.003(2) 0.016(3) -0.031(3) C30 0.035(2) 0.046(3) 0.093(4) 0.003(2) 0.012(2) 0.0008(19) C31 0.0413(19) 0.0326(19) 0.0380(19) -0.0004(15) 0.0098(16) -0.0034(16) C32 0.0325(18) 0.0299(19) 0.042(2) -0.0045(15) 0.0034(15) -0.0009(15) C33 0.0341(18) 0.0276(18) 0.0411(19) -0.0053(15) 0.0061(15) -0.0008(15) C34 0.0338(18) 0.0327(19) 0.044(2) 0.0047(16) 0.0010(15) 0.0028(15) C35 0.048(2) 0.035(2) 0.038(2) 0.0061(16) -0.0008(16) 0.0015(17) C36 0.060(3) 0.051(3) 0.053(2) -0.005(2) 0.027(2) -0.002(2) C37 0.036(2) 0.044(2) 0.055(2) -0.0057(19) -0.0054(17) -0.0013(17) C38 0.046(2) 0.040(2) 0.039(2) -0.0134(17) 0.0075(16) -0.0064(17) C39 0.037(2) 0.045(3) 0.080(3) 0.012(2) 0.002(2) 0.0092(18) C40 0.080(3) 0.063(3) 0.038(2) 0.014(2) -0.011(2) 0.001(3) B1 0.0245(17) 0.035(2) 0.036(2) 0.0038(17) -0.0021(15) 0.0004(16) B2 0.0300(19) 0.033(2) 0.0311(19) -0.0002(16) 0.0010(15) 0.0020(16) Al1 0.0536(7) 0.0363(6) 0.0321(6) 0.0012(5) 0.0038(5) -0.0026(5) Al2 0.0559(7) 0.0497(8) 0.0361(6) 0.0066(5) -0.0003(5) 0.0099(6) Cl1 0.0477(5) 0.0568(6) 0.0346(5) 0.0068(4) -0.0025(4) -0.0098(5) Cl2 0.0649(7) 0.0400(6) 0.0540(6) -0.0014(5) 0.0116(5) -0.0117(5) Cl3 0.0857(9) 0.0525(7) 0.0720(8) 0.0140(6) -0.0405(7) -0.0177(6) Cl4 0.1247(12) 0.0530(7) 0.0836(9) 0.0003(7) 0.0601(9) 0.0087(8) Cl5 0.0574(6) 0.0907(9) 0.0397(5) -0.0075(6) -0.0045(5) 0.0136(6) Cl6 0.1215(13) 0.0914(11) 0.0639(8) -0.0047(7) -0.0510(8) 0.0306(10) Cl7 0.0641(7) 0.0515(7) 0.0823(8) 0.0164(6) 0.0239(6) 0.0086(6) Cl8 0.0832(9) 0.0506(7) 0.0814(9) 0.0069(6) 0.0349(7) -0.0011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.514(5) . ? C1 C5 1.524(5) . ? C1 C6 1.534(5) . ? C1 B1 1.585(5) . ? C2 C3 1.344(5) . ? C2 C7 1.504(5) . ? C3 C4 1.471(6) . ? C3 C8 1.505(6) . ? C4 C5 1.341(5) . ? C4 C9 1.498(5) . ? C5 C10 1.492(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C15 1.425(6) . ? C11 C12 1.427(5) . ? C11 C16 1.502(5) . ? C11 B1 1.783(5) . ? C12 C13 1.424(5) . ? C12 C17 1.497(5) . ? C12 B1 1.775(5) . ? C13 C14 1.423(5) . ? C13 C18 1.506(5) . ? C13 B1 1.781(5) . ? C14 C15 1.431(5) . ? C14 C19 1.504(5) . ? C14 B1 1.755(5) . ? C15 C20 1.493(6) . ? C15 B1 1.757(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.520(5) . ? C21 C22 1.521(5) . ? C21 C25 1.521(5) . ? C21 B2 1.587(5) . ? C22 C23 1.349(6) . ? C22 C27 1.490(6) . ? C23 C24 1.467(6) . ? C23 C28 1.510(6) . ? C24 C25 1.338(6) . ? C24 C29 1.493(6) . ? C25 C30 1.502(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.419(5) . ? C31 C35 1.422(5) . ? C31 C36 1.495(5) . ? C31 B2 1.770(5) . ? C32 C33 1.430(5) . ? C32 C37 1.495(5) . ? C32 B2 1.769(5) . ? C33 C34 1.426(5) . ? C33 C38 1.510(5) . ? C33 B2 1.752(5) . ? C34 C35 1.426(5) . ? C34 C39 1.506(5) . ? C34 B2 1.774(5) . ? C35 C40 1.497(6) . ? C35 B2 1.756(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? Al1 Cl1 2.1254(15) . ? Al1 Cl2 2.1275(16) . ? Al1 Cl4 2.1279(18) . ? Al1 Cl3 2.1489(18) . ? Al2 Cl6 2.1187(19) . ? Al2 Cl5 2.1311(17) . ? Al2 Cl7 2.1312(19) . ? Al2 Cl8 2.1400(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 102.2(3) . . ? C2 C1 C6 114.2(3) . . ? C5 C1 C6 114.4(3) . . ? C2 C1 B1 106.5(3) . . ? C5 C1 B1 106.3(3) . . ? C6 C1 B1 112.4(3) . . ? C3 C2 C7 127.7(4) . . ? C3 C2 C1 109.4(3) . . ? C7 C2 C1 122.9(3) . . ? C2 C3 C4 109.4(3) . . ? C2 C3 C8 128.3(4) . . ? C4 C3 C8 122.3(4) . . ? C5 C4 C3 109.4(3) . . ? C5 C4 C9 126.6(4) . . ? C3 C4 C9 124.0(4) . . ? C4 C5 C10 127.0(4) . . ? C4 C5 C1 109.2(3) . . ? C10 C5 C1 123.7(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C11 C12 108.0(3) . . ? C15 C11 C16 126.4(4) . . ? C12 C11 C16 125.6(4) . . ? C15 C11 B1 65.3(2) . . ? C12 C11 B1 66.0(2) . . ? C16 C11 B1 132.1(3) . . ? C13 C12 C11 107.9(3) . . ? C13 C12 C17 125.8(3) . . ? C11 C12 C17 126.1(3) . . ? C13 C12 B1 66.6(2) . . ? C11 C12 B1 66.7(2) . . ? C17 C12 B1 129.0(3) . . ? C14 C13 C12 108.2(3) . . ? C14 C13 C18 126.5(3) . . ? C12 C13 C18 125.1(3) . . ? C14 C13 B1 65.3(2) . . ? C12 C13 B1 66.2(2) . . ? C18 C13 B1 131.3(3) . . ? C13 C14 C15 107.8(3) . . ? C13 C14 C19 126.6(3) . . ? C15 C14 C19 125.5(4) . . ? C13 C14 B1 67.3(2) . . ? C15 C14 B1 66.1(2) . . ? C19 C14 B1 130.0(3) . . ? C11 C15 C14 107.9(3) . . ? C11 C15 C20 126.0(4) . . ? C14 C15 C20 126.0(4) . . ? C11 C15 B1 67.2(3) . . ? C14 C15 B1 65.9(2) . . ? C20 C15 B1 129.3(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 115.2(3) . . ? C26 C21 C25 114.8(3) . . ? C22 C21 C25 101.7(3) . . ? C26 C21 B2 112.9(3) . . ? C22 C21 B2 105.6(3) . . ? C25 C21 B2 105.5(3) . . ? C23 C22 C27 128.6(4) . . ? C23 C22 C21 108.9(3) . . ? C27 C22 C21 122.4(4) . . ? C22 C23 C24 109.8(3) . . ? C22 C23 C28 127.5(5) . . ? C24 C23 C28 122.7(4) . . ? C25 C24 C23 109.1(3) . . ? C25 C24 C29 127.6(4) . . ? C23 C24 C29 123.4(4) . . ? C24 C25 C30 127.7(4) . . ? C24 C25 C21 109.9(3) . . ? C30 C25 C21 122.5(4) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C35 108.1(3) . . ? C32 C31 C36 127.1(4) . . ? C35 C31 C36 124.7(4) . . ? C32 C31 B2 66.3(2) . . ? C35 C31 B2 65.7(2) . . ? C36 C31 B2 131.5(3) . . ? C31 C32 C33 108.0(3) . . ? C31 C32 C37 126.9(3) . . ? C33 C32 C37 124.9(3) . . ? C31 C32 B2 66.4(2) . . ? C33 C32 B2 65.4(2) . . ? C37 C32 B2 129.9(3) . . ? C34 C33 C32 107.9(3) . . ? C34 C33 C38 127.3(3) . . ? C32 C33 C38 124.5(3) . . ? C34 C33 B2 66.9(2) . . ? C32 C33 B2 66.6(2) . . ? C38 C33 B2 127.2(3) . . ? C35 C34 C33 107.7(3) . . ? C35 C34 C39 124.8(4) . . ? C33 C34 C39 127.4(4) . . ? C35 C34 B2 65.5(2) . . ? C33 C34 B2 65.4(2) . . ? C39 C34 B2 133.0(3) . . ? C31 C35 C34 108.2(3) . . ? C31 C35 C40 125.0(4) . . ? C34 C35 C40 126.7(4) . . ? C31 C35 B2 66.7(2) . . ? C34 C35 B2 66.8(2) . . ? C40 C35 B2 130.2(4) . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C1 B1 C14 134.3(3) . . ? C1 B1 C15 135.4(3) . . ? C14 B1 C15 48.1(2) . . ? C1 B1 C12 138.7(3) . . ? C14 B1 C12 81.6(3) . . ? C15 B1 C12 81.6(3) . . ? C1 B1 C13 136.9(3) . . ? C14 B1 C13 47.4(2) . . ? C15 B1 C13 81.3(2) . . ? C12 B1 C13 47.2(2) . . ? C1 B1 C11 138.4(3) . . ? C14 B1 C11 81.5(3) . . ? C15 B1 C11 47.4(2) . . ? C12 B1 C11 47.3(2) . . ? C13 B1 C11 80.6(2) . . ? C21 B2 C33 134.0(3) . . ? C21 B2 C35 139.4(3) . . ? C33 B2 C35 82.0(3) . . ? C21 B2 C32 134.3(3) . . ? C33 B2 C32 47.93(19) . . ? C35 B2 C32 81.5(3) . . ? C21 B2 C31 137.4(3) . . ? C33 B2 C31 81.7(2) . . ? C35 B2 C31 47.6(2) . . ? C32 B2 C31 47.3(2) . . ? C21 B2 C34 137.8(3) . . ? C33 B2 C34 47.7(2) . . ? C35 B2 C34 47.6(2) . . ? C32 B2 C34 81.4(2) . . ? C31 B2 C34 81.3(2) . . ? Cl1 Al1 Cl2 109.93(7) . . ? Cl1 Al1 Cl4 109.68(8) . . ? Cl2 Al1 Cl4 110.90(7) . . ? Cl1 Al1 Cl3 107.34(7) . . ? Cl2 Al1 Cl3 109.40(7) . . ? Cl4 Al1 Cl3 109.53(9) . . ? Cl6 Al2 Cl5 107.02(8) . . ? Cl6 Al2 Cl7 110.82(9) . . ? Cl5 Al2 Cl7 109.79(8) . . ? Cl6 Al2 Cl8 110.93(9) . . ? Cl5 Al2 Cl8 109.93(8) . . ? Cl7 Al2 Cl8 108.35(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 6.1(4) . . . . ? C6 C1 C2 C3 130.2(4) . . . . ? B1 C1 C2 C3 -105.2(4) . . . . ? C5 C1 C2 C7 -170.6(4) . . . . ? C6 C1 C2 C7 -46.6(5) . . . . ? B1 C1 C2 C7 78.0(4) . . . . ? C7 C2 C3 C4 172.3(4) . . . . ? C1 C2 C3 C4 -4.3(5) . . . . ? C7 C2 C3 C8 -6.4(7) . . . . ? C1 C2 C3 C8 177.0(4) . . . . ? C2 C3 C4 C5 0.3(5) . . . . ? C8 C3 C4 C5 179.1(4) . . . . ? C2 C3 C4 C9 -178.6(4) . . . . ? C8 C3 C4 C9 0.2(6) . . . . ? C3 C4 C5 C10 -174.1(4) . . . . ? C9 C4 C5 C10 4.8(7) . . . . ? C3 C4 C5 C1 3.8(4) . . . . ? C9 C4 C5 C1 -177.3(4) . . . . ? C2 C1 C5 C4 -5.9(4) . . . . ? C6 C1 C5 C4 -129.8(4) . . . . ? B1 C1 C5 C4 105.5(3) . . . . ? C2 C1 C5 C10 172.0(3) . . . . ? C6 C1 C5 C10 48.1(5) . . . . ? B1 C1 C5 C10 -76.6(4) . . . . ? C15 C11 C12 C13 2.3(4) . . . . ? C16 C11 C12 C13 179.3(4) . . . . ? B1 C11 C12 C13 53.6(3) . . . . ? C15 C11 C12 C17 -173.6(4) . . . . ? C16 C11 C12 C17 3.4(6) . . . . ? B1 C11 C12 C17 -122.3(4) . . . . ? C15 C11 C12 B1 -51.3(3) . . . . ? C16 C11 C12 B1 125.7(4) . . . . ? C11 C12 C13 C14 -2.4(4) . . . . ? C17 C12 C13 C14 173.5(4) . . . . ? B1 C12 C13 C14 51.2(3) . . . . ? C11 C12 C13 C18 -178.4(4) . . . . ? C17 C12 C13 C18 -2.5(6) . . . . ? B1 C12 C13 C18 -124.8(4) . . . . ? C11 C12 C13 B1 -53.6(3) . . . . ? C17 C12 C13 B1 122.3(4) . . . . ? C12 C13 C14 C15 1.6(4) . . . . ? C18 C13 C14 C15 177.6(4) . . . . ? B1 C13 C14 C15 53.3(3) . . . . ? C12 C13 C14 C19 -175.5(4) . . . . ? C18 C13 C14 C19 0.4(7) . . . . ? B1 C13 C14 C19 -123.8(4) . . . . ? C12 C13 C14 B1 -51.7(3) . . . . ? C18 C13 C14 B1 124.3(4) . . . . ? C12 C11 C15 C14 -1.2(4) . . . . ? C16 C11 C15 C14 -178.2(4) . . . . ? B1 C11 C15 C14 -53.0(3) . . . . ? C12 C11 C15 C20 174.7(4) . . . . ? C16 C11 C15 C20 -2.3(7) . . . . ? B1 C11 C15 C20 122.9(4) . . . . ? C12 C11 C15 B1 51.7(3) . . . . ? C16 C11 C15 B1 -125.3(4) . . . . ? C13 C14 C15 C11 -0.2(4) . . . . ? C19 C14 C15 C11 177.0(4) . . . . ? B1 C14 C15 C11 53.8(3) . . . . ? C13 C14 C15 C20 -176.2(4) . . . . ? C19 C14 C15 C20 1.0(7) . . . . ? B1 C14 C15 C20 -122.1(4) . . . . ? C13 C14 C15 B1 -54.0(3) . . . . ? C19 C14 C15 B1 123.2(4) . . . . ? C26 C21 C22 C23 -132.8(4) . . . . ? C25 C21 C22 C23 -8.0(4) . . . . ? B2 C21 C22 C23 101.9(4) . . . . ? C26 C21 C22 C27 44.9(5) . . . . ? C25 C21 C22 C27 169.7(4) . . . . ? B2 C21 C22 C27 -80.4(4) . . . . ? C27 C22 C23 C24 -171.7(4) . . . . ? C21 C22 C23 C24 5.8(4) . . . . ? C27 C22 C23 C28 6.5(7) . . . . ? C21 C22 C23 C28 -176.0(4) . . . . ? C22 C23 C24 C25 -0.8(5) . . . . ? C28 C23 C24 C25 -179.1(4) . . . . ? C22 C23 C24 C29 179.0(4) . . . . ? C28 C23 C24 C29 0.7(7) . . . . ? C23 C24 C25 C30 174.8(4) . . . . ? C29 C24 C25 C30 -5.0(7) . . . . ? C23 C24 C25 C21 -4.6(4) . . . . ? C29 C24 C25 C21 175.6(4) . . . . ? C26 C21 C25 C24 132.6(4) . . . . ? C22 C21 C25 C24 7.6(4) . . . . ? B2 C21 C25 C24 -102.4(4) . . . . ? C26 C21 C25 C30 -46.8(5) . . . . ? C22 C21 C25 C30 -171.9(4) . . . . ? B2 C21 C25 C30 78.2(4) . . . . ? C35 C31 C32 C33 0.2(4) . . . . ? C36 C31 C32 C33 -176.9(4) . . . . ? B2 C31 C32 C33 -51.8(3) . . . . ? C35 C31 C32 C37 175.1(4) . . . . ? C36 C31 C32 C37 -2.0(6) . . . . ? B2 C31 C32 C37 123.1(4) . . . . ? C35 C31 C32 B2 52.0(3) . . . . ? C36 C31 C32 B2 -125.1(4) . . . . ? C31 C32 C33 C34 -1.6(4) . . . . ? C37 C32 C33 C34 -176.7(4) . . . . ? B2 C32 C33 C34 -54.0(3) . . . . ? C31 C32 C33 C38 172.5(3) . . . . ? C37 C32 C33 C38 -2.6(6) . . . . ? B2 C32 C33 C38 120.1(4) . . . . ? C31 C32 C33 B2 52.3(3) . . . . ? C37 C32 C33 B2 -122.7(4) . . . . ? C32 C33 C34 C35 2.4(4) . . . . ? C38 C33 C34 C35 -171.5(4) . . . . ? B2 C33 C34 C35 -51.4(3) . . . . ? C32 C33 C34 C39 -179.7(4) . . . . ? C38 C33 C34 C39 6.4(6) . . . . ? B2 C33 C34 C39 126.5(4) . . . . ? C32 C33 C34 B2 53.8(3) . . . . ? C38 C33 C34 B2 -120.1(4) . . . . ? C32 C31 C35 C34 1.3(4) . . . . ? C36 C31 C35 C34 178.5(4) . . . . ? B2 C31 C35 C34 53.6(3) . . . . ? C32 C31 C35 C40 -176.2(4) . . . . ? C36 C31 C35 C40 1.0(6) . . . . ? B2 C31 C35 C40 -123.9(4) . . . . ? C32 C31 C35 B2 -52.3(3) . . . . ? C36 C31 C35 B2 124.8(4) . . . . ? C33 C34 C35 C31 -2.3(4) . . . . ? C39 C34 C35 C31 179.8(4) . . . . ? B2 C34 C35 C31 -53.6(3) . . . . ? C33 C34 C35 C40 175.1(4) . . . . ? C39 C34 C35 C40 -2.8(7) . . . . ? B2 C34 C35 C40 123.9(5) . . . . ? C33 C34 C35 B2 51.3(3) . . . . ? C39 C34 C35 B2 -126.7(4) . . . . ? C2 C1 B1 C14 14.3(5) . . . . ? C5 C1 B1 C14 -94.1(4) . . . . ? C6 C1 B1 C14 140.0(4) . . . . ? C2 C1 B1 C15 84.4(5) . . . . ? C5 C1 B1 C15 -24.0(5) . . . . ? C6 C1 B1 C15 -149.9(4) . . . . ? C2 C1 B1 C12 -128.9(4) . . . . ? C5 C1 B1 C12 122.7(4) . . . . ? C6 C1 B1 C12 -3.2(6) . . . . ? C2 C1 B1 C13 -55.8(5) . . . . ? C5 C1 B1 C13 -164.2(4) . . . . ? C6 C1 B1 C13 69.9(5) . . . . ? C2 C1 B1 C11 156.5(4) . . . . ? C5 C1 B1 C11 48.0(5) . . . . ? C6 C1 B1 C11 -77.9(5) . . . . ? C13 C14 B1 C1 -119.3(4) . . . . ? C15 C14 B1 C1 117.4(4) . . . . ? C19 C14 B1 C1 0.2(6) . . . . ? C13 C14 B1 C15 123.3(3) . . . . ? C19 C14 B1 C15 -117.2(5) . . . . ? C13 C14 B1 C12 37.2(2) . . . . ? C15 C14 B1 C12 -86.2(3) . . . . ? C19 C14 B1 C12 156.6(4) . . . . ? C15 C14 B1 C13 -123.3(3) . . . . ? C19 C14 B1 C13 119.5(5) . . . . ? C13 C14 B1 C11 85.0(3) . . . . ? C15 C14 B1 C11 -38.3(3) . . . . ? C19 C14 B1 C11 -155.5(4) . . . . ? C11 C15 B1 C1 121.1(4) . . . . ? C14 C15 B1 C1 -115.3(5) . . . . ? C20 C15 B1 C1 2.4(7) . . . . ? C11 C15 B1 C14 -123.6(3) . . . . ? C20 C15 B1 C14 117.7(5) . . . . ? C11 C15 B1 C12 -37.4(2) . . . . ? C14 C15 B1 C12 86.2(3) . . . . ? C20 C15 B1 C12 -156.0(4) . . . . ? C11 C15 B1 C13 -85.2(3) . . . . ? C14 C15 B1 C13 38.5(2) . . . . ? C20 C15 B1 C13 156.2(4) . . . . ? C14 C15 B1 C11 123.6(3) . . . . ? C20 C15 B1 C11 -118.7(5) . . . . ? C13 C12 B1 C1 117.0(5) . . . . ? C11 C12 B1 C1 -119.5(5) . . . . ? C17 C12 B1 C1 -1.1(7) . . . . ? C13 C12 B1 C14 -37.3(2) . . . . ? C11 C12 B1 C14 86.1(3) . . . . ? C17 C12 B1 C14 -155.4(4) . . . . ? C13 C12 B1 C15 -86.0(3) . . . . ? C11 C12 B1 C15 37.5(2) . . . . ? C17 C12 B1 C15 155.9(4) . . . . ? C11 C12 B1 C13 123.5(3) . . . . ? C17 C12 B1 C13 -118.1(5) . . . . ? C13 C12 B1 C11 -123.5(3) . . . . ? C17 C12 B1 C11 118.4(4) . . . . ? C14 C13 B1 C1 114.0(5) . . . . ? C12 C13 B1 C1 -120.6(5) . . . . ? C18 C13 B1 C1 -3.9(7) . . . . ? C12 C13 B1 C14 125.4(3) . . . . ? C18 C13 B1 C14 -117.9(5) . . . . ? C14 C13 B1 C15 -39.0(3) . . . . ? C12 C13 B1 C15 86.5(3) . . . . ? C18 C13 B1 C15 -156.9(4) . . . . ? C14 C13 B1 C12 -125.4(3) . . . . ? C18 C13 B1 C12 116.6(5) . . . . ? C14 C13 B1 C11 -87.0(3) . . . . ? C12 C13 B1 C11 38.4(2) . . . . ? C18 C13 B1 C11 155.0(4) . . . . ? C15 C11 B1 C1 -114.9(5) . . . . ? C12 C11 B1 C1 120.0(5) . . . . ? C16 C11 B1 C1 2.8(7) . . . . ? C15 C11 B1 C14 38.8(2) . . . . ? C12 C11 B1 C14 -86.4(3) . . . . ? C16 C11 B1 C14 156.5(4) . . . . ? C12 C11 B1 C15 -125.2(3) . . . . ? C16 C11 B1 C15 117.7(5) . . . . ? C15 C11 B1 C12 125.2(3) . . . . ? C16 C11 B1 C12 -117.1(5) . . . . ? C15 C11 B1 C13 86.8(3) . . . . ? C12 C11 B1 C13 -38.3(2) . . . . ? C16 C11 B1 C13 -155.5(4) . . . . ? C26 C21 B2 C33 154.1(4) . . . . ? C22 C21 B2 C33 -79.2(5) . . . . ? C25 C21 B2 C33 28.0(5) . . . . ? C26 C21 B2 C35 8.1(6) . . . . ? C22 C21 B2 C35 134.7(4) . . . . ? C25 C21 B2 C35 -118.1(4) . . . . ? C26 C21 B2 C32 -136.9(4) . . . . ? C22 C21 B2 C32 -10.3(5) . . . . ? C25 C21 B2 C32 96.9(4) . . . . ? C26 C21 B2 C31 -66.7(5) . . . . ? C22 C21 B2 C31 59.9(5) . . . . ? C25 C21 B2 C31 167.1(4) . . . . ? C26 C21 B2 C34 83.3(5) . . . . ? C22 C21 B2 C34 -150.1(4) . . . . ? C25 C21 B2 C34 -42.9(5) . . . . ? C34 C33 B2 C21 -120.9(4) . . . . ? C32 C33 B2 C21 115.9(4) . . . . ? C38 C33 B2 C21 -0.6(6) . . . . ? C34 C33 B2 C35 37.6(2) . . . . ? C32 C33 B2 C35 -85.7(3) . . . . ? C38 C33 B2 C35 157.8(4) . . . . ? C34 C33 B2 C32 123.2(3) . . . . ? C38 C33 B2 C32 -116.5(4) . . . . ? C34 C33 B2 C31 85.7(3) . . . . ? C32 C33 B2 C31 -37.6(2) . . . . ? C38 C33 B2 C31 -154.1(4) . . . . ? C32 C33 B2 C34 -123.2(3) . . . . ? C38 C33 B2 C34 120.2(4) . . . . ? C31 C35 B2 C21 -117.9(5) . . . . ? C34 C35 B2 C21 118.5(5) . . . . ? C40 C35 B2 C21 -0.9(7) . . . . ? C31 C35 B2 C33 86.1(3) . . . . ? C34 C35 B2 C33 -37.6(2) . . . . ? C40 C35 B2 C33 -157.0(4) . . . . ? C31 C35 B2 C32 37.6(2) . . . . ? C34 C35 B2 C32 -86.1(3) . . . . ? C40 C35 B2 C32 154.6(4) . . . . ? C34 C35 B2 C31 -123.7(3) . . . . ? C40 C35 B2 C31 117.0(5) . . . . ? C31 C35 B2 C34 123.7(3) . . . . ? C40 C35 B2 C34 -119.3(5) . . . . ? C31 C32 B2 C21 120.0(4) . . . . ? C33 C32 B2 C21 -115.3(4) . . . . ? C37 C32 B2 C21 0.7(6) . . . . ? C31 C32 B2 C33 -124.8(3) . . . . ? C37 C32 B2 C33 115.9(4) . . . . ? C31 C32 B2 C35 -37.8(2) . . . . ? C33 C32 B2 C35 86.9(3) . . . . ? C37 C32 B2 C35 -157.1(4) . . . . ? C33 C32 B2 C31 124.8(3) . . . . ? C37 C32 B2 C31 -119.3(4) . . . . ? C31 C32 B2 C34 -86.0(3) . . . . ? C33 C32 B2 C34 38.7(2) . . . . ? C37 C32 B2 C34 154.7(4) . . . . ? C32 C31 B2 C21 -113.6(5) . . . . ? C35 C31 B2 C21 121.7(5) . . . . ? C36 C31 B2 C21 5.9(7) . . . . ? C32 C31 B2 C33 38.0(2) . . . . ? C35 C31 B2 C33 -86.7(3) . . . . ? C36 C31 B2 C33 157.5(4) . . . . ? C32 C31 B2 C35 124.8(3) . . . . ? C36 C31 B2 C35 -115.8(5) . . . . ? C35 C31 B2 C32 -124.8(3) . . . . ? C36 C31 B2 C32 119.4(5) . . . . ? C32 C31 B2 C34 86.3(3) . . . . ? C35 C31 B2 C34 -38.5(2) . . . . ? C36 C31 B2 C34 -154.3(4) . . . . ? C35 C34 B2 C21 -121.6(5) . . . . ? C33 C34 B2 C21 113.3(5) . . . . ? C39 C34 B2 C21 -5.9(7) . . . . ? C35 C34 B2 C33 125.2(3) . . . . ? C39 C34 B2 C33 -119.1(5) . . . . ? C33 C34 B2 C35 -125.2(3) . . . . ? C39 C34 B2 C35 115.7(5) . . . . ? C35 C34 B2 C32 86.3(3) . . . . ? C33 C34 B2 C32 -38.9(2) . . . . ? C39 C34 B2 C32 -158.0(4) . . . . ? C35 C34 B2 C31 38.4(2) . . . . ? C33 C34 B2 C31 -86.7(3) . . . . ? C39 C34 B2 C31 154.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.825 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.074 # Attachment '(MCp2Ga)(AlCl4).cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 664840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H30 Al Cl4 Ga' _chemical_formula_weight 508.94 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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 13.3800(7) _cell_length_b 11.5016(7) _cell_length_c 15.8623(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.449(3) _cell_angle_gamma 90.00 _cell_volume 2408.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'bright yellow' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 1.626 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22788 _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5470 _reflns_number_gt 3515 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution SHELX-93 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+1.0386P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5470 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.000 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 C11 C 0.7808(2) -0.0372(3) 0.36479(19) 0.0268(7) Uani 1 1 d . . . C12 C 0.6965(2) 0.0361(3) 0.38874(19) 0.0298(7) Uani 1 1 d . . . C13 C 0.7352(2) 0.1388(3) 0.41852(19) 0.0319(8) Uani 1 1 d . . . C14 C 0.8449(2) 0.1413(3) 0.41612(19) 0.0305(8) Uani 1 1 d . . . C15 C 0.8724(2) 0.0394(3) 0.38431(19) 0.0275(7) Uani 1 1 d . . . C21 C 0.7114(3) -0.0347(3) 0.10404(19) 0.0318(8) Uani 1 1 d . . . C22 C 0.8065(2) 0.0270(3) 0.1241(2) 0.0344(8) Uani 1 1 d . . . C23 C 0.7887(2) 0.1324(3) 0.1671(2) 0.0304(8) Uani 1 1 d . . . C24 C 0.6846(2) 0.1363(3) 0.17448(19) 0.0272(7) Uani 1 1 d . . . C25 C 0.6359(2) 0.0346(3) 0.13713(19) 0.0290(7) Uani 1 1 d . . . C111 C 0.7932(2) -0.1559(3) 0.4077(2) 0.0335(8) Uani 1 1 d . . . H11A H 0.7325 -0.2005 0.3914 0.050 Uiso 1 1 calc R . . H11B H 0.8057 -0.1462 0.4686 0.050 Uiso 1 1 calc R . . H11C H 0.8493 -0.1959 0.3901 0.050 Uiso 1 1 calc R . . C121 C 0.5904(2) -0.0093(3) 0.3837(2) 0.0440(9) Uani 1 1 d . . . H12A H 0.5885 -0.0652 0.4283 0.066 Uiso 1 1 calc R . . H12B H 0.5694 -0.0456 0.3292 0.066 Uiso 1 1 calc R . . H12C H 0.5456 0.0540 0.3904 0.066 Uiso 1 1 calc R . . C131 C 0.6799(3) 0.2371(3) 0.4528(2) 0.0454(10) Uani 1 1 d . . . H13A H 0.6865 0.3061 0.4201 0.068 Uiso 1 1 calc R . . H13B H 0.7083 0.2507 0.5115 0.068 Uiso 1 1 calc R . . H13C H 0.6095 0.2175 0.4486 0.068 Uiso 1 1 calc R . . C141 C 0.9116(3) 0.2419(3) 0.4462(2) 0.0470(10) Uani 1 1 d . . . H14A H 0.9105 0.2552 0.5058 0.070 Uiso 1 1 calc R . . H14B H 0.8875 0.3100 0.4141 0.070 Uiso 1 1 calc R . . H14C H 0.9796 0.2252 0.4379 0.070 Uiso 1 1 calc R . . C151 C 0.9768(2) -0.0001(3) 0.3726(2) 0.0387(8) Uani 1 1 d . . . H15A H 0.9762 -0.0206 0.3138 0.058 Uiso 1 1 calc R . . H15B H 0.9961 -0.0666 0.4081 0.058 Uiso 1 1 calc R . . H15C H 1.0244 0.0617 0.3884 0.058 Uiso 1 1 calc R . . C211 C 0.6916(3) -0.1378(3) 0.0458(2) 0.0447(10) Uani 1 1 d . . . H21A H 0.7466 -0.1920 0.0583 0.067 Uiso 1 1 calc R . . H21B H 0.6859 -0.1126 -0.0125 0.067 Uiso 1 1 calc R . . H21C H 0.6297 -0.1748 0.0542 0.067 Uiso 1 1 calc R . . C221 C 0.9038(3) -0.0090(3) 0.0945(2) 0.0512(11) Uani 1 1 d . . . H22A H 0.9035 0.0184 0.0373 0.077 Uiso 1 1 calc R . . H22B H 0.9091 -0.0922 0.0956 0.077 Uiso 1 1 calc R . . H22C H 0.9604 0.0239 0.1319 0.077 Uiso 1 1 calc R . . C231 C 0.8653(3) 0.2238(3) 0.1973(2) 0.0440(9) Uani 1 1 d . . . H23A H 0.9316 0.1960 0.1920 0.066 Uiso 1 1 calc R . . H23B H 0.8630 0.2416 0.2561 0.066 Uiso 1 1 calc R . . H23C H 0.8505 0.2927 0.1633 0.066 Uiso 1 1 calc R . . C241 C 0.6341(3) 0.2341(3) 0.2137(2) 0.0385(9) Uani 1 1 d . . . H24A H 0.5964 0.2807 0.1693 0.058 Uiso 1 1 calc R . . H24B H 0.6846 0.2811 0.2477 0.058 Uiso 1 1 calc R . . H24C H 0.5889 0.2029 0.2491 0.058 Uiso 1 1 calc R . . C251 C 0.5244(2) 0.0082(3) 0.1260(2) 0.0434(9) Uani 1 1 d . . . H25A H 0.5144 -0.0744 0.1236 0.065 Uiso 1 1 calc R . . H25B H 0.4908 0.0428 0.0739 0.065 Uiso 1 1 calc R . . H25C H 0.4969 0.0395 0.1734 0.065 Uiso 1 1 calc R . . Al Al 0.74559(7) -0.38055(8) 0.22406(6) 0.0310(2) Uani 1 1 d . . . Cl1 Cl 0.72008(8) -0.48374(8) 0.11278(6) 0.0484(3) Uani 1 1 d . . . Cl2 Cl 0.61814(6) -0.26910(8) 0.23012(6) 0.0416(2) Uani 1 1 d . . . Cl3 Cl 0.86894(6) -0.26091(7) 0.21830(5) 0.0358(2) Uani 1 1 d . . . Cl4 Cl 0.77890(8) -0.48251(8) 0.33642(6) 0.0526(3) Uani 1 1 d . . . Ga1 Ga 0.75246(3) -0.04220(3) 0.23732(2) 0.03040(12) 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 C11 0.0335(17) 0.0288(18) 0.0185(16) 0.0012(14) 0.0050(13) -0.0003(15) C12 0.0348(18) 0.035(2) 0.0193(16) 0.0042(15) 0.0041(13) 0.0055(16) C13 0.049(2) 0.0278(19) 0.0195(17) 0.0030(14) 0.0074(15) 0.0064(16) C14 0.045(2) 0.0243(18) 0.0196(17) 0.0047(14) -0.0006(14) -0.0042(15) C15 0.0327(17) 0.0254(18) 0.0238(17) 0.0055(14) 0.0030(13) -0.0006(15) C21 0.049(2) 0.0280(19) 0.0188(16) 0.0019(14) 0.0069(14) 0.0101(17) C22 0.0407(19) 0.037(2) 0.0283(18) 0.0143(16) 0.0147(15) 0.0110(17) C23 0.0330(18) 0.0316(19) 0.0272(18) 0.0110(15) 0.0069(14) 0.0017(15) C24 0.0326(17) 0.0240(17) 0.0260(17) 0.0089(14) 0.0076(14) 0.0077(15) C25 0.0329(17) 0.0302(19) 0.0232(17) 0.0053(15) 0.0024(13) 0.0071(15) C111 0.047(2) 0.0257(19) 0.0271(18) 0.0048(15) 0.0050(15) -0.0032(16) C121 0.041(2) 0.052(2) 0.041(2) -0.0002(18) 0.0160(17) 0.0028(19) C131 0.063(3) 0.038(2) 0.036(2) -0.0054(17) 0.0115(18) 0.0142(19) C141 0.065(3) 0.032(2) 0.042(2) -0.0019(17) 0.0033(19) -0.0098(19) C151 0.0366(19) 0.036(2) 0.043(2) 0.0021(17) 0.0066(16) -0.0030(17) C211 0.071(3) 0.037(2) 0.026(2) -0.0023(16) 0.0078(18) 0.0106(19) C221 0.052(2) 0.051(2) 0.058(3) 0.022(2) 0.032(2) 0.021(2) C231 0.041(2) 0.043(2) 0.049(2) 0.0119(19) 0.0098(17) -0.0041(18) C241 0.044(2) 0.032(2) 0.041(2) 0.0008(17) 0.0113(17) 0.0063(16) C251 0.0359(19) 0.046(2) 0.045(2) 0.0001(18) -0.0048(16) 0.0063(18) Al 0.0404(6) 0.0249(5) 0.0287(6) 0.0000(4) 0.0088(5) -0.0004(5) Cl1 0.0746(7) 0.0389(5) 0.0319(5) -0.0079(4) 0.0098(5) -0.0057(5) Cl2 0.0346(5) 0.0441(6) 0.0485(6) -0.0021(4) 0.0134(4) -0.0004(4) Cl3 0.0324(4) 0.0336(5) 0.0423(5) 0.0010(4) 0.0088(4) 0.0010(4) Cl4 0.0888(7) 0.0358(5) 0.0333(5) 0.0075(4) 0.0105(5) 0.0025(5) Ga1 0.0351(2) 0.0341(2) 0.0222(2) 0.00345(16) 0.00524(15) 0.00197(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 C15 1.500(4) . ? C11 C12 1.505(4) . ? C11 C111 1.523(4) . ? C11 Ga1 1.996(3) . ? C12 C13 1.344(4) . ? C12 C121 1.502(4) . ? C13 C14 1.475(4) . ? C13 C131 1.501(4) . ? C14 C15 1.351(4) . ? C14 C141 1.491(4) . ? C15 C151 1.508(4) . ? C21 C22 1.447(5) . ? C21 C25 1.451(4) . ? C21 C211 1.500(4) . ? C21 Ga1 2.097(3) . ? C22 C23 1.430(4) . ? C22 C221 1.511(4) . ? C22 Ga1 2.192(3) . ? C23 C24 1.417(4) . ? C23 C231 1.492(5) . ? C23 Ga1 2.385(3) . ? C24 C25 1.420(4) . ? C24 C241 1.499(4) . ? C24 Ga1 2.395(3) . ? C25 C251 1.504(4) . ? C25 Ga1 2.219(3) . ? C111 H11A 0.9600 . ? C111 H11B 0.9600 . ? C111 H11C 0.9600 . ? C121 H12A 0.9600 . ? C121 H12B 0.9600 . ? C121 H12C 0.9600 . ? C131 H13A 0.9600 . ? C131 H13B 0.9600 . ? C131 H13C 0.9600 . ? C141 H14A 0.9600 . ? C141 H14B 0.9600 . ? C141 H14C 0.9600 . ? C151 H15A 0.9600 . ? C151 H15B 0.9600 . ? C151 H15C 0.9600 . ? C211 H21A 0.9600 . ? C211 H21B 0.9600 . ? C211 H21C 0.9600 . ? C221 H22A 0.9600 . ? C221 H22B 0.9600 . ? C221 H22C 0.9600 . ? C231 H23A 0.9600 . ? C231 H23B 0.9600 . ? C231 H23C 0.9600 . ? C241 H24A 0.9600 . ? C241 H24B 0.9600 . ? C241 H24C 0.9600 . ? C251 H25A 0.9600 . ? C251 H25B 0.9600 . ? C251 H25C 0.9600 . ? Al Cl1 2.1078(13) . ? Al Cl4 2.1190(13) . ? Al Cl2 2.1481(13) . ? Al Cl3 2.1623(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 C11 C12 103.9(3) . . ? C15 C11 C111 114.1(3) . . ? C12 C11 C111 114.9(2) . . ? C15 C11 Ga1 103.82(18) . . ? C12 C11 Ga1 104.3(2) . . ? C111 C11 Ga1 114.5(2) . . ? C13 C12 C121 129.0(3) . . ? C13 C12 C11 108.6(3) . . ? C121 C12 C11 122.2(3) . . ? C12 C13 C14 109.6(3) . . ? C12 C13 C131 127.3(3) . . ? C14 C13 C131 123.1(3) . . ? C15 C14 C13 109.1(3) . . ? C15 C14 C141 127.3(3) . . ? C13 C14 C141 123.6(3) . . ? C14 C15 C11 108.8(3) . . ? C14 C15 C151 128.5(3) . . ? C11 C15 C151 122.7(3) . . ? C22 C21 C25 106.9(3) . . ? C22 C21 C211 125.7(3) . . ? C25 C21 C211 126.5(3) . . ? C22 C21 Ga1 73.88(18) . . ? C25 C21 Ga1 74.97(17) . . ? C211 C21 Ga1 125.4(2) . . ? C23 C22 C21 108.1(3) . . ? C23 C22 C221 126.9(3) . . ? C21 C22 C221 124.6(3) . . ? C23 C22 Ga1 79.31(17) . . ? C21 C22 Ga1 66.77(16) . . ? C221 C22 Ga1 124.9(2) . . ? C24 C23 C22 108.0(3) . . ? C24 C23 C231 125.7(3) . . ? C22 C23 C231 126.2(3) . . ? C24 C23 Ga1 73.13(17) . . ? C22 C23 Ga1 64.59(16) . . ? C231 C23 Ga1 128.7(2) . . ? C23 C24 C25 109.2(3) . . ? C23 C24 C241 125.0(3) . . ? C25 C24 C241 125.7(3) . . ? C23 C24 Ga1 72.38(17) . . ? C25 C24 Ga1 65.44(16) . . ? C241 C24 Ga1 129.5(2) . . ? C24 C25 C21 107.7(3) . . ? C24 C25 C251 126.4(3) . . ? C21 C25 C251 125.6(3) . . ? C24 C25 Ga1 78.96(18) . . ? C21 C25 Ga1 65.88(17) . . ? C251 C25 Ga1 124.8(2) . . ? C11 C111 H11A 109.5 . . ? C11 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C11 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C13 C131 H13A 109.5 . . ? C13 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C13 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C15 C151 H15A 109.5 . . ? C15 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C15 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? C21 C211 H21A 109.5 . . ? C21 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C21 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C23 C231 H23A 109.5 . . ? C23 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C23 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C24 C241 H24A 109.5 . . ? C24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? C24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C25 C251 H25A 109.5 . . ? C25 C251 H25B 109.5 . . ? H25A C251 H25B 109.5 . . ? C25 C251 H25C 109.5 . . ? H25A C251 H25C 109.5 . . ? H25B C251 H25C 109.5 . . ? Cl1 Al Cl4 112.06(6) . . ? Cl1 Al Cl2 110.66(6) . . ? Cl4 Al Cl2 110.58(5) . . ? Cl1 Al Cl3 110.04(5) . . ? Cl4 Al Cl3 109.34(6) . . ? Cl2 Al Cl3 103.84(5) . . ? C11 Ga1 C21 174.19(12) . . ? C11 Ga1 C22 141.79(13) . . ? C21 Ga1 C22 39.35(12) . . ? C11 Ga1 C25 135.09(11) . . ? C21 Ga1 C25 39.16(11) . . ? C22 Ga1 C25 63.69(11) . . ? C11 Ga1 C23 115.44(12) . . ? C21 Ga1 C23 62.24(12) . . ? C22 Ga1 C23 36.10(11) . . ? C25 Ga1 C23 60.20(11) . . ? C11 Ga1 C24 113.13(11) . . ? C21 Ga1 C24 61.74(11) . . ? C22 Ga1 C24 60.10(11) . . ? C25 Ga1 C24 35.60(11) . . ? C23 Ga1 C24 34.49(10) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.345 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.083 # Attachment '(MCp2Ga)(BF4).cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 664841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H30 B1 F4 Ga1' _chemical_formula_sum 'C20 H30 B F4 Ga' _chemical_formula_weight 426.97 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' B B 0.0013 0.0007 '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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 11.9721(4) _cell_length_b 16.4808(4) _cell_length_c 20.4486(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4034.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 1.400 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7671 _exptl_absorpt_correction_T_max 0.9333 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24914 _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4539 _reflns_number_gt 2958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution SHELX-93 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+4.6725P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4539 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 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 C151 C 0.3413(3) 0.28348(18) 0.26687(18) 0.0334(8) Uani 1 1 d . . . H15A H 0.2666 0.2890 0.2478 0.050 Uiso 1 1 calc R . . H15B H 0.3976 0.2882 0.2323 0.050 Uiso 1 1 calc R . . H15C H 0.3530 0.3263 0.2994 0.050 Uiso 1 1 calc R . . C121 C 0.3498(3) -0.02781(19) 0.2957(2) 0.0551(13) Uani 1 1 d . . . H12A H 0.4073 -0.0414 0.2635 0.083 Uiso 1 1 calc R . . H12B H 0.2759 -0.0399 0.2776 0.083 Uiso 1 1 calc R . . H12C H 0.3615 -0.0600 0.3354 0.083 Uiso 1 1 calc R . . C131 C 0.4492(3) 0.0554(3) 0.4265(2) 0.0618(13) Uani 1 1 d . . . H13A H 0.4126 0.0766 0.4658 0.093 Uiso 1 1 calc R . . H13B H 0.5299 0.0648 0.4294 0.093 Uiso 1 1 calc R . . H13C H 0.4348 -0.0029 0.4228 0.093 Uiso 1 1 calc R . . Ga1 Ga 0.18849(3) 0.131613(18) 0.329815(15) 0.02072(11) Uani 1 1 d . . . F22 F 0.04297(17) 0.31221(10) 0.20031(9) 0.0346(5) Uani 1 1 d . . . F12 F 0.04574(17) -0.05081(10) 0.20121(8) 0.0335(5) Uani 1 1 d . . . C11 C 0.3183(2) 0.12580(16) 0.26827(14) 0.0209(6) Uani 1 1 d . . . F11 F 0.08375(16) 0.04547(11) 0.27659(9) 0.0394(5) Uani 1 1 d . . . C23 C 0.1963(2) 0.08520(17) 0.50896(14) 0.0230(7) Uani 1 1 d . . . C24 C 0.2012(2) 0.17434(17) 0.50912(14) 0.0224(7) Uani 1 1 d . . . B2 B 0.0000 0.2674(3) 0.2500 0.0188(10) Uani 1 2 d S . . C22 C 0.1449(2) 0.05959(17) 0.45394(14) 0.0196(6) Uani 1 1 d . . . F21 F 0.08530(15) 0.21575(11) 0.27455(9) 0.0359(5) Uani 1 1 d . . . C25 C 0.1518(2) 0.20310(17) 0.45460(14) 0.0201(7) Uani 1 1 d . . . C21 C 0.1099(2) 0.13271(17) 0.41454(13) 0.0172(6) Uani 1 1 d . . . C211 C -0.0169(2) 0.13504(18) 0.40264(14) 0.0216(6) Uani 1 1 d . . . H22A H -0.0397 0.0862 0.3788 0.032 Uiso 1 1 calc R . . H22B H -0.0358 0.1832 0.3768 0.032 Uiso 1 1 calc R . . H22C H -0.0560 0.1372 0.4447 0.032 Uiso 1 1 calc R . . B1 B 0.0000 -0.0059(3) 0.2500 0.0194(10) Uani 1 2 d S . . C241 C 0.2534(3) 0.2215(2) 0.56400(16) 0.0337(8) Uani 1 1 d . . . H24A H 0.3326 0.2070 0.5676 0.051 Uiso 1 1 calc R . . H24B H 0.2153 0.2084 0.6051 0.051 Uiso 1 1 calc R . . H24C H 0.2465 0.2797 0.5552 0.051 Uiso 1 1 calc R . . C231 C 0.2406(3) 0.0346(2) 0.56422(16) 0.0327(8) Uani 1 1 d . . . H23A H 0.1931 0.0418 0.6028 0.049 Uiso 1 1 calc R . . H23B H 0.3170 0.0515 0.5746 0.049 Uiso 1 1 calc R . . H23C H 0.2406 -0.0227 0.5514 0.049 Uiso 1 1 calc R . . C221 C 0.1187(3) -0.02564(17) 0.43406(15) 0.0267(7) Uani 1 1 d . . . H22D H 0.1436 -0.0346 0.3890 0.040 Uiso 1 1 calc R . . H22E H 0.0380 -0.0347 0.4369 0.040 Uiso 1 1 calc R . . H22F H 0.1574 -0.0635 0.4633 0.040 Uiso 1 1 calc R . . C14 C 0.4003(2) 0.18373(19) 0.35907(15) 0.0256(7) Uani 1 1 d . . . C13 C 0.4034(3) 0.0983(2) 0.36676(16) 0.0313(8) Uani 1 1 d . . . C251 C 0.1356(3) 0.29009(17) 0.43436(16) 0.0282(7) Uani 1 1 d . . . H25A H 0.0565 0.2997 0.4247 0.042 Uiso 1 1 calc R . . H25B H 0.1803 0.3013 0.3953 0.042 Uiso 1 1 calc R . . H25C H 0.1594 0.3260 0.4699 0.042 Uiso 1 1 calc R . . C15 C 0.3515(2) 0.20178(17) 0.29934(14) 0.0203(7) Uani 1 1 d . . . C111 C 0.2979(3) 0.1158(2) 0.19640(15) 0.0366(9) Uani 1 1 d . . . H11A H 0.2605 0.0638 0.1884 0.055 Uiso 1 1 calc R . . H11B H 0.3694 0.1169 0.1730 0.055 Uiso 1 1 calc R . . H11C H 0.2504 0.1602 0.1807 0.055 Uiso 1 1 calc R . . C12 C 0.3570(3) 0.06136(18) 0.31226(17) 0.0281(8) Uani 1 1 d . . . C141 C 0.4422(3) 0.2444(3) 0.40778(17) 0.0479(10) Uani 1 1 d . . . H14A H 0.5157 0.2275 0.4238 0.072 Uiso 1 1 calc R . . H14B H 0.3899 0.2476 0.4446 0.072 Uiso 1 1 calc R . . H14C H 0.4482 0.2977 0.3869 0.072 Uiso 1 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 C151 0.0242(18) 0.0267(17) 0.049(2) 0.0111(16) 0.0030(16) -0.0029(14) C121 0.040(2) 0.0213(18) 0.104(4) 0.001(2) 0.030(2) 0.0070(16) C131 0.024(2) 0.106(4) 0.056(3) 0.045(3) 0.0026(19) 0.019(2) Ga1 0.02248(18) 0.01964(16) 0.02003(17) 0.00124(14) 0.00655(14) 0.00128(15) F22 0.0464(12) 0.0276(9) 0.0298(10) 0.0092(8) -0.0001(9) -0.0028(9) F12 0.0435(12) 0.0291(10) 0.0279(10) -0.0064(8) 0.0015(9) 0.0100(9) C11 0.0171(14) 0.0224(14) 0.0232(15) -0.0018(12) 0.0022(12) -0.0031(14) F11 0.0343(12) 0.0479(12) 0.0359(11) -0.0121(9) 0.0040(9) -0.0230(10) C23 0.0133(15) 0.0339(17) 0.0219(16) 0.0050(13) 0.0024(13) 0.0014(14) C24 0.0172(16) 0.0320(16) 0.0181(15) -0.0028(13) 0.0029(13) -0.0025(14) B2 0.018(3) 0.019(2) 0.020(2) 0.000 -0.007(2) 0.000 C22 0.0160(15) 0.0249(15) 0.0180(16) 0.0043(12) 0.0055(13) -0.0007(13) F21 0.0224(10) 0.0460(11) 0.0394(11) 0.0197(9) 0.0018(9) 0.0119(9) C25 0.0176(15) 0.0218(15) 0.0210(16) -0.0059(12) 0.0026(13) -0.0002(12) C21 0.0158(14) 0.0201(14) 0.0159(14) 0.0000(12) 0.0021(11) -0.0010(13) C211 0.0165(14) 0.0271(15) 0.0214(15) 0.0008(14) 0.0029(12) -0.0001(14) B1 0.023(3) 0.015(2) 0.020(3) 0.000 -0.003(2) 0.000 C241 0.032(2) 0.0461(19) 0.0230(19) -0.0085(15) -0.0045(14) -0.0066(16) C231 0.0237(19) 0.0464(19) 0.028(2) 0.0105(16) -0.0028(14) 0.0009(16) C221 0.0317(19) 0.0222(16) 0.0262(18) 0.0045(13) 0.0028(15) -0.0003(14) C14 0.0123(15) 0.0400(19) 0.0246(17) -0.0036(15) 0.0014(13) -0.0018(14) C13 0.0129(15) 0.050(2) 0.0306(19) 0.0168(16) 0.0039(13) 0.0065(15) C251 0.0317(19) 0.0227(16) 0.0301(18) -0.0034(14) 0.0016(15) -0.0029(14) C15 0.0130(15) 0.0226(15) 0.0253(17) 0.0006(13) 0.0042(12) -0.0027(13) C111 0.0305(19) 0.054(2) 0.0255(17) -0.0110(16) 0.0107(14) -0.0131(17) C12 0.0154(16) 0.0213(15) 0.048(2) 0.0066(14) 0.0162(15) 0.0056(13) C141 0.030(2) 0.079(3) 0.035(2) -0.019(2) -0.0031(17) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C151 C15 1.506(4) . ? C121 C12 1.510(4) . ? C131 C13 1.513(5) . ? Ga1 C21 1.972(3) . ? Ga1 C11 2.002(3) . ? Ga1 F21 2.1740(17) . ? Ga1 F11 2.1847(18) . ? Ga1 C15 2.353(3) . ? Ga1 C12 2.354(3) . ? F22 B2 1.357(3) . ? F12 B1 1.358(3) . ? C11 C15 1.459(4) . ? C11 C12 1.467(4) . ? C11 C111 1.499(4) . ? F11 B1 1.420(3) . ? C23 C22 1.350(4) . ? C23 C24 1.470(4) . ? C23 C231 1.502(4) . ? C24 C25 1.348(4) . ? C24 C241 1.501(4) . ? B2 F22 1.357(3) 4 ? B2 F21 1.421(3) 4 ? B2 F21 1.421(3) . ? C22 C221 1.495(4) . ? C22 C21 1.509(4) . ? C25 C251 1.505(4) . ? C25 C21 1.506(4) . ? C21 C211 1.538(4) . ? B1 F12 1.358(3) 4 ? B1 F11 1.420(3) 4 ? C14 C15 1.386(4) . ? C14 C13 1.417(5) . ? C14 C141 1.498(4) . ? C13 C12 1.386(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Ga1 C11 157.40(12) . . ? C21 Ga1 F21 100.36(9) . . ? C11 Ga1 F21 98.33(10) . . ? C21 Ga1 F11 99.78(9) . . ? C11 Ga1 F11 95.81(9) . . ? F21 Ga1 F11 80.17(8) . . ? C21 Ga1 C15 128.62(11) . . ? C11 Ga1 C15 38.10(10) . . ? F21 Ga1 C15 91.16(9) . . ? F11 Ga1 C15 131.58(9) . . ? C21 Ga1 C12 123.20(11) . . ? C11 Ga1 C12 38.29(11) . . ? F21 Ga1 C12 136.18(9) . . ? F11 Ga1 C12 95.53(10) . . ? C15 Ga1 C12 59.36(10) . . ? C15 C11 C12 105.6(2) . . ? C15 C11 C111 124.5(3) . . ? C12 C11 C111 125.0(3) . . ? C15 C11 Ga1 84.06(17) . . ? C12 C11 Ga1 83.93(17) . . ? C111 C11 Ga1 119.7(2) . . ? B1 F11 Ga1 169.47(14) . . ? C22 C23 C24 109.4(3) . . ? C22 C23 C231 127.9(3) . . ? C24 C23 C231 122.7(3) . . ? C25 C24 C23 109.4(3) . . ? C25 C24 C241 128.3(3) . . ? C23 C24 C241 122.4(3) . . ? F22 B2 F22 114.1(4) 4 . ? F22 B2 F21 108.54(11) 4 4 ? F22 B2 F21 109.50(11) . 4 ? F22 B2 F21 109.50(11) 4 . ? F22 B2 F21 108.54(11) . . ? F21 B2 F21 106.4(3) 4 . ? C23 C22 C221 128.0(3) . . ? C23 C22 C21 108.8(2) . . ? C221 C22 C21 123.1(3) . . ? B2 F21 Ga1 166.93(13) . . ? C24 C25 C251 128.2(3) . . ? C24 C25 C21 109.0(2) . . ? C251 C25 C21 122.8(3) . . ? C25 C21 C22 103.4(2) . . ? C25 C21 C211 113.3(2) . . ? C22 C21 C211 112.2(2) . . ? C25 C21 Ga1 109.04(18) . . ? C22 C21 Ga1 109.23(18) . . ? C211 C21 Ga1 109.40(18) . . ? F12 B1 F12 113.9(4) . 4 ? F12 B1 F11 109.17(11) . 4 ? F12 B1 F11 108.76(12) 4 4 ? F12 B1 F11 108.76(12) . . ? F12 B1 F11 109.17(11) 4 . ? F11 B1 F11 106.9(3) 4 . ? C15 C14 C13 108.8(3) . . ? C15 C14 C141 125.7(3) . . ? C13 C14 C141 125.5(3) . . ? C12 C13 C14 109.7(3) . . ? C12 C13 C131 126.0(3) . . ? C14 C13 C131 124.3(4) . . ? C14 C15 C11 108.3(3) . . ? C14 C15 C151 127.9(3) . . ? C11 C15 C151 123.6(3) . . ? C14 C15 Ga1 90.60(19) . . ? C11 C15 Ga1 57.84(14) . . ? C151 C15 Ga1 119.3(2) . . ? C13 C12 C11 107.5(3) . . ? C13 C12 C121 129.1(3) . . ? C11 C12 C121 123.3(3) . . ? C13 C12 Ga1 90.28(19) . . ? C11 C12 Ga1 57.77(15) . . ? C121 C12 Ga1 117.6(2) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.733 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.077 # Attachment 'MCp2AlMe.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 665220' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common bis(pentamethylcyclopentadienyl)methylalane _chemical_melting_point ? _chemical_formula_moiety 'C21 H33 Al' _chemical_formula_sum 'C21 H33 Al' _chemical_formula_weight 312.45 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 0.0000 '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' Al Al 0.0645 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 10.443(2) _cell_length_b 11.874(2) _cell_length_c 15.806(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1959.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 1983 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 25.02 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6572 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1983 _reflns_number_gt 1712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution SHELX-93 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1633P)^2^+4.1477P] 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 none _refine_ls_extinction_coef 0.019(7) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -10(10) _refine_ls_number_reflns 1983 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0936 _refine_ls_wR_factor_ref 0.2834 _refine_ls_wR_factor_gt 0.2749 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Al1 Al 1.0000 0.0000 0.66484(16) 0.0274(7) Uani 1 2 d S . . C1 C 1.0000 0.0000 0.5412(6) 0.053(3) Uani 1 2 d S . . H1A H 1.0311 -0.0729 0.5205 0.080 Uiso 0.50 1 calc PR . . H1B H 1.0562 0.0601 0.5205 0.080 Uiso 0.50 1 calc PR . . H1C H 0.9127 0.0128 0.5205 0.080 Uiso 0.50 1 calc PR . . C11 C 0.9405(7) 0.1406(6) 0.7393(4) 0.0337(16) Uani 1 1 d . . . C12 C 0.8212(8) 0.0823(7) 0.7195(5) 0.0409(18) Uani 1 1 d . . . C13 C 0.7772(7) 0.1255(7) 0.6431(5) 0.0402(19) Uani 1 1 d . . . C14 C 0.8618(7) 0.2090(6) 0.6146(4) 0.0345(17) Uani 1 1 d . . . C15 C 0.9602(8) 0.2201(6) 0.6729(5) 0.0371(18) Uani 1 1 d . . . C111 C 0.9929(10) 0.1570(7) 0.8284(4) 0.0444(18) Uani 1 1 d . . . H11A H 0.9679 0.0929 0.8638 0.067 Uiso 1 1 calc R . . H11B H 0.9580 0.2265 0.8524 0.067 Uiso 1 1 calc R . . H11C H 1.0865 0.1620 0.8261 0.067 Uiso 1 1 calc R . . C121 C 0.7452(9) 0.0115(9) 0.7807(6) 0.060(2) Uani 1 1 d . . . H12A H 0.7987 -0.0072 0.8297 0.090 Uiso 1 1 calc R . . H12B H 0.7178 -0.0581 0.7527 0.090 Uiso 1 1 calc R . . H12C H 0.6697 0.0536 0.7996 0.090 Uiso 1 1 calc R . . C131 C 0.6638(8) 0.0828(10) 0.5941(6) 0.064(3) Uani 1 1 d . . . H13A H 0.6200 0.0244 0.6270 0.095 Uiso 1 1 calc R . . H13B H 0.6928 0.0510 0.5402 0.095 Uiso 1 1 calc R . . H13C H 0.6045 0.1451 0.5832 0.095 Uiso 1 1 calc R . . C141 C 0.8509(10) 0.2722(8) 0.5323(5) 0.054(2) Uani 1 1 d . . . H14A H 0.7724 0.2492 0.5030 0.080 Uiso 1 1 calc R . . H14B H 0.9252 0.2552 0.4967 0.080 Uiso 1 1 calc R . . H14C H 0.8479 0.3533 0.5437 0.080 Uiso 1 1 calc R . . C151 C 1.0726(10) 0.2969(9) 0.6670(6) 0.062(3) Uani 1 1 d . . . H15A H 1.1277 0.2863 0.7165 0.094 Uiso 1 1 calc R . . H15B H 1.0429 0.3752 0.6649 0.094 Uiso 1 1 calc R . . H15C H 1.1212 0.2798 0.6155 0.094 Uiso 1 1 calc R . . Al2 Al 1.5000 0.5000 0.83533(16) 0.0286(7) Uani 1 2 d S . . C2 C 1.5000 0.5000 0.9595(6) 0.067(5) Uani 1 2 d S . . H2A H 1.5846 0.5227 0.9802 0.100 Uiso 0.50 1 calc PR . . H2B H 1.4800 0.4242 0.9802 0.100 Uiso 0.50 1 calc PR . . H2C H 1.4353 0.5531 0.9802 0.100 Uiso 0.50 1 calc PR . . C21 C 1.3379(7) 0.4558(6) 0.7610(4) 0.0345(17) Uani 1 1 d . . . C22 C 1.3940(7) 0.3482(7) 0.7812(5) 0.0384(18) Uani 1 1 d . . . C23 C 1.3417(8) 0.3132(6) 0.8576(4) 0.0355(17) Uani 1 1 d . . . C24 C 1.2546(7) 0.3943(7) 0.8865(5) 0.0357(17) Uani 1 1 d . . . C25 C 1.2510(7) 0.4825(6) 0.8283(4) 0.0351(17) Uani 1 1 d . . . C211 C 1.3216(8) 0.5042(9) 0.6719(4) 0.0466(19) Uani 1 1 d . . . H21A H 1.3908 0.4767 0.6355 0.070 Uiso 1 1 calc R . . H21B H 1.3247 0.5866 0.6745 0.070 Uiso 1 1 calc R . . H21C H 1.2389 0.4804 0.6488 0.070 Uiso 1 1 calc R . . C221 C 1.4669(9) 0.2760(8) 0.7188(6) 0.052(2) Uani 1 1 d . . . H22A H 1.4937 0.3222 0.6706 0.079 Uiso 1 1 calc R . . H22B H 1.4116 0.2148 0.6988 0.079 Uiso 1 1 calc R . . H22C H 1.5426 0.2441 0.7465 0.079 Uiso 1 1 calc R . . C231 C 1.3821(10) 0.2100(7) 0.9074(6) 0.054(2) Uani 1 1 d . . . H23A H 1.3300 0.2040 0.9588 0.082 Uiso 1 1 calc R . . H23B H 1.4726 0.2167 0.9230 0.082 Uiso 1 1 calc R . . H23C H 1.3699 0.1425 0.8726 0.082 Uiso 1 1 calc R . . C241 C 1.1813(9) 0.3898(9) 0.9686(5) 0.056(2) Uani 1 1 d . . . H24A H 1.2004 0.3190 0.9978 0.083 Uiso 1 1 calc R . . H24B H 1.0893 0.3942 0.9569 0.083 Uiso 1 1 calc R . . H24C H 1.2067 0.4534 1.0044 0.083 Uiso 1 1 calc R . . C251 C 1.1700(10) 0.5885(8) 0.8353(6) 0.056(2) Uani 1 1 d . . . H25A H 1.1849 0.6363 0.7857 0.084 Uiso 1 1 calc R . . H25B H 1.1937 0.6297 0.8867 0.084 Uiso 1 1 calc R . . H25C H 1.0792 0.5678 0.8380 0.084 Uiso 1 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 Al1 0.0342(15) 0.0281(14) 0.0197(13) 0.000 0.000 -0.0006(13) C1 0.066(8) 0.060(8) 0.034(6) 0.000 0.000 0.026(8) C11 0.041(4) 0.034(4) 0.026(3) 0.001(3) -0.001(3) 0.006(3) C12 0.041(4) 0.041(4) 0.042(4) 0.000(4) 0.007(4) -0.005(4) C13 0.030(4) 0.047(4) 0.044(4) -0.016(4) -0.003(3) -0.001(4) C14 0.047(4) 0.031(4) 0.025(3) 0.002(3) 0.000(3) 0.008(3) C15 0.049(5) 0.036(4) 0.026(3) -0.002(3) 0.005(3) -0.004(3) C111 0.062(5) 0.042(4) 0.029(3) -0.002(3) -0.003(5) 0.010(4) C121 0.057(5) 0.058(6) 0.065(5) 0.003(6) 0.029(5) -0.005(5) C131 0.030(4) 0.097(8) 0.064(6) -0.023(6) -0.002(4) -0.004(5) C141 0.079(7) 0.050(5) 0.031(4) 0.006(4) -0.003(4) 0.007(5) C151 0.074(7) 0.070(6) 0.043(5) -0.002(5) 0.013(5) -0.036(6) Al2 0.0302(14) 0.0347(15) 0.0208(13) 0.000 0.000 -0.0038(14) C2 0.086(10) 0.096(11) 0.019(5) 0.000 0.000 -0.059(10) C21 0.036(4) 0.036(4) 0.031(4) 0.001(3) -0.001(3) -0.012(3) C22 0.026(3) 0.048(4) 0.041(4) -0.004(4) -0.006(3) -0.007(4) C23 0.042(4) 0.034(4) 0.031(4) -0.003(3) -0.016(3) -0.002(3) C24 0.030(4) 0.042(4) 0.035(4) -0.002(3) -0.003(3) -0.007(3) C25 0.029(3) 0.041(4) 0.035(3) -0.003(4) -0.002(3) 0.002(3) C211 0.050(4) 0.061(5) 0.028(3) 0.002(5) -0.003(3) -0.013(4) C221 0.052(5) 0.046(5) 0.059(5) -0.019(4) 0.012(4) -0.008(4) C231 0.072(6) 0.042(5) 0.049(5) 0.005(4) -0.017(5) -0.011(5) C241 0.053(5) 0.082(7) 0.032(4) 0.004(4) 0.012(4) -0.007(5) C251 0.067(6) 0.052(5) 0.050(5) 0.001(5) -0.004(5) 0.014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 C1 1.955(11) . ? Al1 C11 2.135(8) 2_755 ? Al1 C11 2.135(8) . ? Al1 C12 2.277(8) 2_755 ? Al1 C12 2.277(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C11 C15 1.427(10) . ? C11 C12 1.459(11) . ? C11 C111 1.523(9) . ? C12 C13 1.390(11) . ? C12 C121 1.508(11) . ? C13 C14 1.402(11) . ? C13 C131 1.503(11) . ? C14 C15 1.386(11) . ? C14 C141 1.506(10) . ? C15 C151 1.490(11) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C151 H15A 0.9800 . ? C151 H15B 0.9800 . ? C151 H15C 0.9800 . ? Al2 C2 1.963(10) . ? Al2 C21 2.126(8) . ? Al2 C21 2.126(8) 2_865 ? Al2 C22 2.282(8) . ? Al2 C22 2.282(8) 2_865 ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C21 C25 1.434(10) . ? C21 C22 1.442(11) . ? C21 C211 1.530(10) . ? C22 C23 1.389(11) . ? C22 C221 1.512(11) . ? C23 C24 1.402(11) . ? C23 C231 1.517(11) . ? C24 C25 1.396(11) . ? C24 C241 1.507(10) . ? C25 C251 1.520(11) . ? C211 H21A 0.9800 . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C231 H23A 0.9800 . ? C231 H23B 0.9800 . ? C231 H23C 0.9800 . ? C241 H24A 0.9800 . ? C241 H24B 0.9800 . ? C241 H24C 0.9800 . ? C251 H25A 0.9800 . ? C251 H25B 0.9800 . ? C251 H25C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Al1 C11 123.5(2) . 2_755 ? C1 Al1 C11 123.5(2) . . ? C11 Al1 C11 113.1(4) 2_755 . ? C1 Al1 C12 112.3(2) . 2_755 ? C11 Al1 C12 38.4(3) 2_755 2_755 ? C11 Al1 C12 111.4(3) . 2_755 ? C1 Al1 C12 112.3(2) . . ? C11 Al1 C12 111.4(3) 2_755 . ? C11 Al1 C12 38.4(3) . . ? C12 Al1 C12 135.4(4) 2_755 . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C15 C11 C12 106.2(6) . . ? C15 C11 C111 122.9(7) . . ? C12 C11 C111 124.5(7) . . ? C15 C11 Al1 94.0(5) . . ? C12 C11 Al1 76.1(4) . . ? C111 C11 Al1 120.3(5) . . ? C13 C12 C11 107.0(7) . . ? C13 C12 C121 126.1(8) . . ? C11 C12 C121 125.2(8) . . ? C13 C12 Al1 95.7(5) . . ? C11 C12 Al1 65.5(4) . . ? C121 C12 Al1 115.8(6) . . ? C12 C13 C14 109.4(7) . . ? C12 C13 C131 125.7(8) . . ? C14 C13 C131 124.8(8) . . ? C15 C14 C13 108.7(6) . . ? C15 C14 C141 125.6(8) . . ? C13 C14 C141 125.6(8) . . ? C14 C15 C11 108.6(7) . . ? C14 C15 C151 126.9(8) . . ? C11 C15 C151 124.4(8) . . ? C11 C111 H11A 109.5 . . ? C11 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C11 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C13 C131 H13A 109.5 . . ? C13 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C13 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C15 C151 H15A 109.5 . . ? C15 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C15 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? C2 Al2 C21 123.5(2) . . ? C2 Al2 C21 123.5(2) . 2_865 ? C21 Al2 C21 112.9(4) . 2_865 ? C2 Al2 C22 112.0(2) . . ? C21 Al2 C22 38.0(3) . . ? C21 Al2 C22 112.0(3) 2_865 . ? C2 Al2 C22 112.0(2) . 2_865 ? C21 Al2 C22 112.0(3) . 2_865 ? C21 Al2 C22 38.0(3) 2_865 2_865 ? C22 Al2 C22 136.0(4) . 2_865 ? Al2 C2 H2A 109.5 . . ? Al2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Al2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C25 C21 C22 106.8(6) . . ? C25 C21 C211 121.9(7) . . ? C22 C21 C211 125.6(7) . . ? C25 C21 Al2 92.3(4) . . ? C22 C21 Al2 76.9(4) . . ? C211 C21 Al2 120.3(5) . . ? C23 C22 C21 107.3(7) . . ? C23 C22 C221 126.6(8) . . ? C21 C22 C221 124.2(7) . . ? C23 C22 Al2 95.8(5) . . ? C21 C22 Al2 65.2(4) . . ? C221 C22 Al2 116.6(5) . . ? C22 C23 C24 109.5(7) . . ? C22 C23 C231 125.7(8) . . ? C24 C23 C231 124.5(7) . . ? C25 C24 C23 108.5(6) . . ? C25 C24 C241 125.5(8) . . ? C23 C24 C241 125.9(8) . . ? C24 C25 C21 107.8(6) . . ? C24 C25 C251 126.0(7) . . ? C21 C25 C251 126.1(7) . . ? C21 C211 H21A 109.5 . . ? C21 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C21 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C23 C231 H23A 109.5 . . ? C23 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C23 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C24 C241 H24A 109.5 . . ? C24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? C24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C25 C251 H25A 109.5 . . ? C25 C251 H25B 109.5 . . ? H25A C251 H25B 109.5 . . ? C25 C251 H25C 109.5 . . ? H25A C251 H25C 109.5 . . ? H25B C251 H25C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Al1 C11 C15 -21.5(6) . . . . ? C11 Al1 C11 C15 158.5(6) 2_755 . . . ? C12 Al1 C11 C15 116.8(5) 2_755 . . . ? C12 Al1 C11 C15 -105.7(6) . . . . ? C1 Al1 C11 C12 84.2(5) . . . . ? C11 Al1 C11 C12 -95.8(4) 2_755 . . . ? C12 Al1 C11 C12 -137.4(5) 2_755 . . . ? C1 Al1 C11 C111 -153.8(5) . . . . ? C11 Al1 C11 C111 26.2(5) 2_755 . . . ? C12 Al1 C11 C111 -15.4(7) 2_755 . . . ? C12 Al1 C11 C111 122.0(8) . . . . ? C15 C11 C12 C13 1.6(8) . . . . ? C111 C11 C12 C13 154.0(7) . . . . ? Al1 C11 C12 C13 -88.6(6) . . . . ? C15 C11 C12 C121 -164.5(8) . . . . ? C111 C11 C12 C121 -12.1(13) . . . . ? Al1 C11 C12 C121 105.3(8) . . . . ? C15 C11 C12 Al1 90.2(5) . . . . ? C111 C11 C12 Al1 -117.4(7) . . . . ? C1 Al1 C12 C13 -10.1(6) . . . . ? C11 Al1 C12 C13 -153.3(5) 2_755 . . . ? C11 Al1 C12 C13 106.1(7) . . . . ? C12 Al1 C12 C13 169.9(6) 2_755 . . . ? C1 Al1 C12 C11 -116.2(4) . . . . ? C11 Al1 C12 C11 100.6(6) 2_755 . . . ? C12 Al1 C12 C11 63.8(4) 2_755 . . . ? C1 Al1 C12 C121 124.9(6) . . . . ? C11 Al1 C12 C121 -18.3(7) 2_755 . . . ? C11 Al1 C12 C121 -118.9(8) . . . . ? C12 Al1 C12 C121 -55.1(6) 2_755 . . . ? C11 C12 C13 C14 -0.9(9) . . . . ? C121 C12 C13 C14 165.1(8) . . . . ? Al1 C12 C13 C14 -66.9(6) . . . . ? C11 C12 C13 C131 173.9(8) . . . . ? C121 C12 C13 C131 -20.1(13) . . . . ? Al1 C12 C13 C131 107.9(8) . . . . ? C12 C13 C14 C15 -0.3(9) . . . . ? C131 C13 C14 C15 -175.1(8) . . . . ? C12 C13 C14 C141 177.0(8) . . . . ? C131 C13 C14 C141 2.2(13) . . . . ? C13 C14 C15 C11 1.3(9) . . . . ? C141 C14 C15 C11 -176.0(7) . . . . ? C13 C14 C15 C151 178.4(8) . . . . ? C141 C14 C15 C151 1.1(13) . . . . ? C12 C11 C15 C14 -1.8(8) . . . . ? C111 C11 C15 C14 -154.7(7) . . . . ? Al1 C11 C15 C14 74.9(6) . . . . ? C12 C11 C15 C151 -178.9(8) . . . . ? C111 C11 C15 C151 28.1(12) . . . . ? Al1 C11 C15 C151 -102.3(8) . . . . ? C2 Al2 C21 C25 23.6(5) . . . . ? C21 Al2 C21 C25 -156.4(5) 2_865 . . . ? C22 Al2 C21 C25 106.8(6) . . . . ? C22 Al2 C21 C25 -115.2(5) 2_865 . . . ? C2 Al2 C21 C22 -83.2(5) . . . . ? C21 Al2 C21 C22 96.8(5) 2_865 . . . ? C22 Al2 C21 C22 138.0(5) 2_865 . . . ? C2 Al2 C21 C211 153.0(5) . . . . ? C21 Al2 C21 C211 -27.0(5) 2_865 . . . ? C22 Al2 C21 C211 -123.8(8) . . . . ? C22 Al2 C21 C211 14.2(7) 2_865 . . . ? C25 C21 C22 C23 0.0(8) . . . . ? C211 C21 C22 C23 -153.5(7) . . . . ? Al2 C21 C22 C23 88.4(5) . . . . ? C25 C21 C22 C221 165.2(7) . . . . ? C211 C21 C22 C221 11.6(12) . . . . ? Al2 C21 C22 C221 -106.4(7) . . . . ? C25 C21 C22 Al2 -88.4(5) . . . . ? C211 C21 C22 Al2 118.0(8) . . . . ? C2 Al2 C22 C23 10.4(5) . . . . ? C21 Al2 C22 C23 -106.4(7) . . . . ? C21 Al2 C22 C23 154.1(5) 2_865 . . . ? C22 Al2 C22 C23 -169.6(5) 2_865 . . . ? C2 Al2 C22 C21 116.8(4) . . . . ? C21 Al2 C22 C21 -99.5(6) 2_865 . . . ? C22 Al2 C22 C21 -63.2(4) 2_865 . . . ? C2 Al2 C22 C221 -125.8(6) . . . . ? C21 Al2 C22 C221 117.5(8) . . . . ? C21 Al2 C22 C221 17.9(7) 2_865 . . . ? C22 Al2 C22 C221 54.2(6) 2_865 . . . ? C21 C22 C23 C24 0.0(8) . . . . ? C221 C22 C23 C24 -164.7(8) . . . . ? Al2 C22 C23 C24 65.8(6) . . . . ? C21 C22 C23 C231 -173.8(7) . . . . ? C221 C22 C23 C231 21.6(12) . . . . ? Al2 C22 C23 C231 -108.0(7) . . . . ? C22 C23 C24 C25 -0.1(8) . . . . ? C231 C23 C24 C25 173.8(7) . . . . ? C22 C23 C24 C241 -177.6(8) . . . . ? C231 C23 C24 C241 -3.8(12) . . . . ? C23 C24 C25 C21 0.1(8) . . . . ? C241 C24 C25 C21 177.7(7) . . . . ? C23 C24 C25 C251 -179.5(7) . . . . ? C241 C24 C25 C251 -1.9(13) . . . . ? C22 C21 C25 C24 -0.1(8) . . . . ? C211 C21 C25 C24 154.7(7) . . . . ? Al2 C21 C25 C24 -77.1(6) . . . . ? C22 C21 C25 C251 179.5(7) . . . . ? C211 C21 C25 C251 -25.7(12) . . . . ? Al2 C21 C25 C251 102.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.717 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.089 # Attachment 'MCp2BBr.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 664842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common bispentamethylcyclopentadienylbromoborane _chemical_melting_point ? _chemical_formula_moiety 'C20 H30 B Br' _chemical_formula_sum 'C20 H30 B Br' _chemical_formula_weight 361.16 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7070(15) _cell_length_b 15.777(3) _cell_length_c 16.096(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00(3) _cell_angle_gamma 90.00 _cell_volume 1957.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 13037 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 2.096 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6793 _exptl_absorpt_correction_T_max 0.6793 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13037 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4426 _reflns_number_gt 2800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4426 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1679 _refine_ls_R_factor_gt 0.1255 _refine_ls_wR_factor_ref 0.3874 _refine_ls_wR_factor_gt 0.3423 _refine_ls_goodness_of_fit_ref 1.427 _refine_ls_restrained_S_all 1.427 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 C11 C -0.0354(11) 0.3345(4) 0.1448(5) 0.0401(18) Uani 1 1 d . . . C12 C -0.1115(9) 0.3280(4) 0.0574(5) 0.0376(17) Uani 1 1 d . . . C13 C -0.0070(10) 0.3646(5) -0.0007(6) 0.0399(18) Uani 1 1 d . . . C14 C 0.1484(10) 0.3965(4) 0.0426(6) 0.0413(19) Uani 1 1 d . . . C15 C 0.1374(11) 0.3801(4) 0.1250(6) 0.044(2) Uani 1 1 d . . . C16 C 0.0823(10) 0.1637(4) 0.1375(6) 0.0407(19) Uani 1 1 d . . . C17 C -0.0919(12) 0.1160(5) 0.1364(7) 0.051(2) Uani 1 1 d . . . C18 C -0.1331(10) 0.1010(4) 0.0569(6) 0.050(2) Uani 1 1 d . . . C19 C -0.0015(10) 0.1332(5) -0.0001(6) 0.0417(19) Uani 1 1 d . . . C10 C 0.1235(9) 0.1704(4) 0.0455(5) 0.0363(17) Uani 1 1 d . . . C111 C -0.1521(14) 0.3869(5) 0.2040(7) 0.057(3) Uani 1 1 d . . . H11A H -0.0991 0.3889 0.2593 0.086 Uiso 1 1 calc R . . H11B H -0.2668 0.3603 0.2077 0.086 Uiso 1 1 calc R . . H11C H -0.1644 0.4446 0.1823 0.086 Uiso 1 1 calc R . . C121 C -0.2902(10) 0.2944(5) 0.0434(6) 0.052(2) Uani 1 1 d . . . H12A H -0.3367 0.2724 0.0958 0.078 Uiso 1 1 calc R . . H12B H -0.2862 0.2488 0.0022 0.078 Uiso 1 1 calc R . . H12C H -0.3651 0.3401 0.0230 0.078 Uiso 1 1 calc R . . C131 C -0.0339(14) 0.3735(6) -0.0944(7) 0.054(2) Uani 1 1 d . . . H13A H 0.0661 0.4026 -0.1189 0.082 Uiso 1 1 calc R . . H13B H -0.1393 0.4065 -0.1050 0.082 Uiso 1 1 calc R . . H13C H -0.0458 0.3172 -0.1193 0.082 Uiso 1 1 calc R . . C141 C 0.2897(11) 0.4401(5) -0.0059(7) 0.062(3) Uani 1 1 d . . . H14A H 0.2588 0.4409 -0.0649 0.094 Uiso 1 1 calc R . . H14B H 0.3991 0.4093 0.0015 0.094 Uiso 1 1 calc R . . H14C H 0.3032 0.4983 0.0143 0.094 Uiso 1 1 calc R . . C151 C 0.2633(16) 0.4061(6) 0.1922(9) 0.072(3) Uani 1 1 d . . . H15A H 0.2200 0.3869 0.2462 0.108 Uiso 1 1 calc R . . H15B H 0.2749 0.4680 0.1925 0.108 Uiso 1 1 calc R . . H15C H 0.3768 0.3804 0.1814 0.108 Uiso 1 1 calc R . . C161 C 0.2269(16) 0.1146(5) 0.1838(8) 0.066(3) Uani 1 1 d . . . H16A H 0.1979 0.1108 0.2429 0.100 Uiso 1 1 calc R . . H16B H 0.3375 0.1445 0.1772 0.100 Uiso 1 1 calc R . . H16C H 0.2369 0.0574 0.1605 0.100 Uiso 1 1 calc R . . C171 C -0.181(2) 0.0854(7) 0.2165(8) 0.094(5) Uani 1 1 d . . . H17A H -0.1213 0.1094 0.2648 0.142 Uiso 1 1 calc R . . H17B H -0.1761 0.0233 0.2191 0.142 Uiso 1 1 calc R . . H17C H -0.3024 0.1038 0.2165 0.142 Uiso 1 1 calc R . . C181 C -0.2905(12) 0.0548(5) 0.0241(9) 0.087(4) Uani 1 1 d . . . H18A H -0.2844 0.0517 -0.0366 0.130 Uiso 1 1 calc R . . H18B H -0.3958 0.0853 0.0406 0.130 Uiso 1 1 calc R . . H18C H -0.2934 -0.0027 0.0472 0.130 Uiso 1 1 calc R . . C191 C -0.0058(17) 0.1275(6) -0.0949(8) 0.068(3) Uani 1 1 d . . . H19A H -0.1126 0.0990 -0.1125 0.103 Uiso 1 1 calc R . . H19B H 0.0949 0.0952 -0.1144 0.103 Uiso 1 1 calc R . . H19C H -0.0024 0.1847 -0.1186 0.103 Uiso 1 1 calc R . . C101 C 0.2925(11) 0.2067(5) 0.0122(7) 0.058(3) Uani 1 1 d . . . H10A H 0.3625 0.2282 0.0584 0.087 Uiso 1 1 calc R . . H10B H 0.2670 0.2531 -0.0264 0.087 Uiso 1 1 calc R . . H10C H 0.3570 0.1622 -0.0170 0.087 Uiso 1 1 calc R . . B B 0.0271(14) 0.2487(4) 0.1829(6) 0.037(2) Uani 1 1 d . . . Br Br 0.0445(2) 0.24827(5) 0.30699(8) 0.0645(5) 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 C11 0.046(4) 0.022(3) 0.053(5) -0.003(3) 0.001(4) 0.002(3) C12 0.033(4) 0.021(3) 0.058(5) 0.006(3) -0.001(4) -0.003(3) C13 0.035(4) 0.027(3) 0.058(5) 0.005(3) 0.002(3) 0.005(3) C14 0.028(4) 0.020(3) 0.076(6) 0.001(3) -0.005(4) 0.000(3) C15 0.039(4) 0.020(3) 0.073(6) -0.005(3) -0.011(4) -0.004(3) C16 0.033(4) 0.021(3) 0.068(5) 0.004(3) -0.004(4) 0.002(3) C17 0.053(5) 0.018(3) 0.083(7) 0.001(4) 0.021(5) -0.007(3) C18 0.029(4) 0.019(3) 0.100(7) -0.008(4) 0.003(4) -0.005(3) C19 0.036(4) 0.030(4) 0.060(5) -0.004(4) -0.002(4) 0.006(3) C10 0.027(4) 0.019(3) 0.063(5) -0.002(3) 0.002(3) 0.006(3) C111 0.072(6) 0.035(4) 0.065(6) 0.000(4) 0.013(5) 0.015(4) C121 0.025(4) 0.039(4) 0.093(7) 0.013(4) -0.004(4) -0.004(3) C131 0.060(6) 0.036(4) 0.067(6) 0.012(4) -0.001(5) -0.006(4) C141 0.042(5) 0.031(4) 0.114(8) 0.015(5) 0.001(5) -0.006(3) C151 0.079(7) 0.045(5) 0.093(8) -0.007(5) -0.034(7) -0.015(5) C161 0.082(7) 0.028(4) 0.089(8) -0.008(5) -0.022(6) 0.023(4) C171 0.142(13) 0.049(6) 0.093(8) -0.007(5) 0.047(8) -0.047(7) C181 0.036(5) 0.041(5) 0.183(12) -0.040(6) -0.012(6) -0.006(4) C191 0.089(8) 0.042(5) 0.074(7) -0.018(5) -0.010(6) 0.012(5) C101 0.034(4) 0.036(4) 0.105(8) -0.002(4) 0.023(5) -0.003(3) B 0.046(5) 0.032(4) 0.033(5) 0.001(3) -0.005(4) -0.008(3) Br 0.1015(10) 0.0462(6) 0.0457(6) -0.0011(3) -0.0087(7) 0.0141(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 C12 1.528(11) . ? C11 C15 1.547(11) . ? C11 C111 1.549(12) . ? C11 B 1.562(11) . ? C12 C13 1.362(11) . ? C12 C121 1.493(10) . ? C13 C14 1.475(11) . ? C13 C131 1.528(14) . ? C14 C15 1.354(12) . ? C14 C141 1.506(12) . ? C15 C151 1.509(13) . ? C16 C10 1.518(12) . ? C16 C17 1.539(11) . ? C16 C161 1.548(12) . ? C16 B 1.585(11) . ? C17 C18 1.340(13) . ? C17 C171 1.538(14) . ? C18 C19 1.459(12) . ? C18 C181 1.511(11) . ? C19 C10 1.346(11) . ? C19 C191 1.529(16) . ? C10 C101 1.521(11) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C151 H15A 0.9800 . ? C151 H15B 0.9800 . ? C151 H15C 0.9800 . ? C161 H16A 0.9800 . ? C161 H16B 0.9800 . ? C161 H16C 0.9800 . ? C171 H17A 0.9800 . ? C171 H17B 0.9800 . ? C171 H17C 0.9800 . ? C181 H18A 0.9800 . ? C181 H18B 0.9800 . ? C181 H18C 0.9800 . ? C191 H19A 0.9800 . ? C191 H19B 0.9800 . ? C191 H19C 0.9800 . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? B Br 2.003(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 C11 C15 99.9(6) . . ? C12 C11 C111 112.3(7) . . ? C15 C11 C111 112.2(7) . . ? C12 C11 B 114.9(6) . . ? C15 C11 B 102.6(7) . . ? C111 C11 B 113.6(7) . . ? C13 C12 C121 126.3(8) . . ? C13 C12 C11 112.1(7) . . ? C121 C12 C11 121.1(7) . . ? C12 C13 C14 107.5(8) . . ? C12 C13 C131 129.5(8) . . ? C14 C13 C131 123.0(8) . . ? C15 C14 C13 110.3(7) . . ? C15 C14 C141 129.8(8) . . ? C13 C14 C141 119.9(8) . . ? C14 C15 C151 127.5(9) . . ? C14 C15 C11 110.1(7) . . ? C151 C15 C11 122.2(9) . . ? C10 C16 C17 101.8(7) . . ? C10 C16 C161 110.7(8) . . ? C17 C16 C161 112.9(7) . . ? C10 C16 B 116.5(6) . . ? C17 C16 B 100.7(7) . . ? C161 C16 B 113.3(8) . . ? C18 C17 C171 129.7(9) . . ? C18 C17 C16 107.7(8) . . ? C171 C17 C16 122.3(10) . . ? C17 C18 C19 112.0(7) . . ? C17 C18 C181 127.5(9) . . ? C19 C18 C181 120.4(10) . . ? C10 C19 C18 107.8(8) . . ? C10 C19 C191 125.9(9) . . ? C18 C19 C191 126.3(8) . . ? C19 C10 C16 110.6(7) . . ? C19 C10 C101 125.8(8) . . ? C16 C10 C101 123.4(7) . . ? C11 C111 H11A 109.5 . . ? C11 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C11 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C13 C131 H13A 109.5 . . ? C13 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C13 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C15 C151 H15A 109.5 . . ? C15 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C15 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? C16 C161 H16A 109.5 . . ? C16 C161 H16B 109.5 . . ? H16A C161 H16B 109.5 . . ? C16 C161 H16C 109.5 . . ? H16A C161 H16C 109.5 . . ? H16B C161 H16C 109.5 . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C18 C181 H18A 109.5 . . ? C18 C181 H18B 109.5 . . ? H18A C181 H18B 109.5 . . ? C18 C181 H18C 109.5 . . ? H18A C181 H18C 109.5 . . ? H18B C181 H18C 109.5 . . ? C19 C191 H19A 109.5 . . ? C19 C191 H19B 109.5 . . ? H19A C191 H19B 109.5 . . ? C19 C191 H19C 109.5 . . ? H19A C191 H19C 109.5 . . ? H19B C191 H19C 109.5 . . ? C10 C101 H10A 109.5 . . ? C10 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C10 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C11 B C16 129.5(8) . . ? C11 B Br 114.5(6) . . ? C16 B Br 116.0(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 C11 C12 C13 -1.6(7) . . . . ? C111 C11 C12 C13 117.5(8) . . . . ? B C11 C12 C13 -110.6(8) . . . . ? C15 C11 C12 C121 -174.5(6) . . . . ? C111 C11 C12 C121 -55.4(9) . . . . ? B C11 C12 C121 76.5(9) . . . . ? C121 C12 C13 C14 173.8(7) . . . . ? C11 C12 C13 C14 1.3(8) . . . . ? C121 C12 C13 C131 -6.5(13) . . . . ? C11 C12 C13 C131 -179.0(8) . . . . ? C12 C13 C14 C15 -0.4(9) . . . . ? C131 C13 C14 C15 179.9(7) . . . . ? C12 C13 C14 C141 179.5(6) . . . . ? C131 C13 C14 C141 -0.2(11) . . . . ? C13 C14 C15 C151 -176.4(8) . . . . ? C141 C14 C15 C151 3.7(14) . . . . ? C13 C14 C15 C11 -0.6(8) . . . . ? C141 C14 C15 C11 179.4(7) . . . . ? C12 C11 C15 C14 1.3(7) . . . . ? C111 C11 C15 C14 -117.9(8) . . . . ? B C11 C15 C14 119.8(7) . . . . ? C12 C11 C15 C151 177.3(8) . . . . ? C111 C11 C15 C151 58.1(10) . . . . ? B C11 C15 C151 -64.2(9) . . . . ? C10 C16 C17 C18 -0.2(8) . . . . ? C161 C16 C17 C18 -118.9(9) . . . . ? B C16 C17 C18 120.1(7) . . . . ? C10 C16 C17 C171 173.8(8) . . . . ? C161 C16 C17 C171 55.1(12) . . . . ? B C16 C17 C171 -66.0(10) . . . . ? C171 C17 C18 C19 -172.7(10) . . . . ? C16 C17 C18 C19 0.7(9) . . . . ? C171 C17 C18 C181 5.5(15) . . . . ? C16 C17 C18 C181 178.9(7) . . . . ? C17 C18 C19 C10 -1.0(9) . . . . ? C181 C18 C19 C10 -179.3(7) . . . . ? C17 C18 C19 C191 -179.9(8) . . . . ? C181 C18 C19 C191 1.7(12) . . . . ? C18 C19 C10 C16 0.8(8) . . . . ? C191 C19 C10 C16 179.8(8) . . . . ? C18 C19 C10 C101 175.1(7) . . . . ? C191 C19 C10 C101 -5.9(12) . . . . ? C17 C16 C10 C19 -0.4(7) . . . . ? C161 C16 C10 C19 119.8(7) . . . . ? B C16 C10 C19 -108.8(8) . . . . ? C17 C16 C10 C101 -174.9(6) . . . . ? C161 C16 C10 C101 -54.6(9) . . . . ? B C16 C10 C101 76.7(9) . . . . ? C12 C11 B C16 22.7(13) . . . . ? C15 C11 B C16 -84.6(11) . . . . ? C111 C11 B C16 154.0(10) . . . . ? C12 C11 B Br -158.8(6) . . . . ? C15 C11 B Br 93.8(7) . . . . ? C111 C11 B Br -27.6(10) . . . . ? C10 C16 B C11 16.7(13) . . . . ? C17 C16 B C11 -92.4(11) . . . . ? C161 C16 B C11 146.8(10) . . . . ? C10 C16 B Br -161.7(6) . . . . ? C17 C16 B Br 89.1(8) . . . . ? C161 C16 B Br -31.7(10) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.031 _refine_diff_density_min -1.547 _refine_diff_density_rms 0.150 # Attachment 'MCp2BCl.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 664843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common bispentamethylcyclopentadienylchloroborane _chemical_melting_point 89-90 _chemical_formula_moiety 'C20 H30 B Cl' _chemical_formula_sum 'C20 H30 B Cl' _chemical_formula_weight 316.70 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.6333(14) _cell_length_b 16.202(2) _cell_length_c 15.542(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.212(13) _cell_angle_gamma 90.00 _cell_volume 1920.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 4.84 _cell_measurement_theta_max 12.49 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.194 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The crystal was coated in perfluoropoly ether ; _diffrn_ambient_temperature 153(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 18.98 _diffrn_reflns_number 5686 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4351 _reflns_number_gt 2579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1346P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4351 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.2161 _refine_ls_wR_factor_gt 0.1809 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cl Cl 0.07627(13) 0.25183(4) 0.70593(4) 0.0585(3) Uani 1 1 d . . . B B 0.0459(4) 0.25188(16) 0.81953(16) 0.0318(6) Uani 1 1 d . . . C10 C -0.1117(3) 0.17364(14) 0.94210(14) 0.0315(5) Uani 1 1 d . . . C11 C 0.0971(3) 0.33582(14) 0.86684(14) 0.0320(5) Uani 1 1 d . . . C12 C -0.0725(4) 0.38544(14) 0.85684(16) 0.0384(6) Uani 1 1 d . . . C13 C -0.1295(3) 0.40209(14) 0.93612(17) 0.0373(6) Uani 1 1 d . . . C14 C -0.0097(3) 0.36808(14) 1.00131(15) 0.0331(5) Uani 1 1 d . . . C15 C 0.1226(3) 0.32992(13) 0.96382(14) 0.0297(5) Uani 1 1 d . . . C16 C -0.0287(3) 0.16753(14) 0.85567(14) 0.0331(6) Uani 1 1 d . . . C17 C 0.1398(4) 0.11992(14) 0.87828(15) 0.0364(6) Uani 1 1 d . . . C18 C 0.1453(3) 0.10358(14) 0.96349(16) 0.0351(6) Uani 1 1 d . . . C19 C -0.0108(3) 0.13592(14) 1.00202(14) 0.0328(5) Uani 1 1 d . . . C101 C -0.2908(3) 0.20980(16) 0.95211(19) 0.0431(6) Uani 1 1 d . . . H10A H -0.2989 0.2320 1.0091 0.065 Uiso 1 1 calc R . . H10B H -0.3777 0.1675 0.9431 0.065 Uiso 1 1 calc R . . H10C H -0.3103 0.2530 0.9106 0.065 Uiso 1 1 calc R . . C111 C 0.2548(4) 0.38115(18) 0.82856(18) 0.0526(8) Uani 1 1 d . . . H11A H 0.2745 0.4323 0.8585 0.079 Uiso 1 1 calc R . . H11B H 0.2300 0.3920 0.7686 0.079 Uiso 1 1 calc R . . H11C H 0.3575 0.3472 0.8348 0.079 Uiso 1 1 calc R . . C121 C -0.1475(6) 0.4152(2) 0.77231(19) 0.0742(11) Uani 1 1 d . . . H12A H -0.2332 0.4573 0.7819 0.111 Uiso 1 1 calc R . . H12B H -0.2020 0.3700 0.7417 0.111 Uiso 1 1 calc R . . H12C H -0.0554 0.4376 0.7390 0.111 Uiso 1 1 calc R . . C131 C -0.2906(4) 0.45126(19) 0.9564(2) 0.0634(9) Uani 1 1 d . . . H13A H -0.3539 0.4651 0.9038 0.095 Uiso 1 1 calc R . . H13B H -0.2561 0.5009 0.9862 0.095 Uiso 1 1 calc R . . H13C H -0.3642 0.4190 0.9922 0.095 Uiso 1 1 calc R . . C141 C -0.0362(5) 0.3767(2) 1.09630(16) 0.0556(8) Uani 1 1 d . . . H14A H 0.0556 0.3480 1.1278 0.083 Uiso 1 1 calc R . . H14B H -0.1475 0.3536 1.1099 0.083 Uiso 1 1 calc R . . H14C H -0.0335 0.4341 1.1118 0.083 Uiso 1 1 calc R . . C151 C 0.2815(4) 0.29339(17) 1.00645(18) 0.0468(7) Uani 1 1 d . . . H15A H 0.2534 0.2730 1.0622 0.070 Uiso 1 1 calc R . . H15B H 0.3711 0.3348 1.0126 0.070 Uiso 1 1 calc R . . H15C H 0.3230 0.2488 0.9721 0.070 Uiso 1 1 calc R . . C161 C -0.1486(5) 0.12001(19) 0.79162(17) 0.0554(8) Uani 1 1 d . . . H16A H -0.1851 0.0693 0.8175 0.083 Uiso 1 1 calc R . . H16B H -0.0861 0.1080 0.7407 0.083 Uiso 1 1 calc R . . H16C H -0.2498 0.1529 0.7766 0.083 Uiso 1 1 calc R . . C171 C 0.2688(5) 0.09176(19) 0.81371(19) 0.0605(9) Uani 1 1 d . . . H17A H 0.3426 0.0495 0.8389 0.091 Uiso 1 1 calc R . . H17B H 0.3396 0.1377 0.7972 0.091 Uiso 1 1 calc R . . H17C H 0.2066 0.0701 0.7638 0.091 Uiso 1 1 calc R . . C181 C 0.2851(4) 0.05735(18) 1.01320(19) 0.0528(8) Uani 1 1 d . . . H18A H 0.3740 0.0401 0.9750 0.079 Uiso 1 1 calc R . . H18B H 0.2348 0.0097 1.0395 0.079 Uiso 1 1 calc R . . H18C H 0.3364 0.0925 1.0571 0.079 Uiso 1 1 calc R . . C191 C -0.0465(4) 0.12641(19) 1.09611(15) 0.0488(7) Uani 1 1 d . . . H19A H -0.1559 0.1525 1.1080 0.073 Uiso 1 1 calc R . . H19B H 0.0462 0.1519 1.1301 0.073 Uiso 1 1 calc R . . H19C H -0.0526 0.0688 1.1102 0.073 Uiso 1 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 Cl 0.1059(7) 0.0478(4) 0.0229(3) -0.0033(3) 0.0165(3) -0.0165(4) B 0.0408(15) 0.0309(13) 0.0241(11) 0.0005(10) 0.0070(11) 0.0003(12) C10 0.0381(13) 0.0243(11) 0.0330(11) -0.0006(9) 0.0103(10) -0.0037(10) C11 0.0454(14) 0.0249(11) 0.0264(11) 0.0006(9) 0.0099(10) -0.0036(10) C12 0.0494(16) 0.0221(11) 0.0426(13) 0.0027(10) -0.0107(12) -0.0008(11) C13 0.0319(13) 0.0243(11) 0.0556(15) -0.0055(10) 0.0012(11) -0.0020(10) C14 0.0417(14) 0.0241(11) 0.0342(12) -0.0032(9) 0.0123(10) -0.0069(10) C15 0.0359(13) 0.0247(11) 0.0289(11) 0.0004(9) 0.0046(9) -0.0036(10) C16 0.0456(15) 0.0281(11) 0.0258(11) -0.0002(9) 0.0033(10) -0.0045(11) C17 0.0483(15) 0.0237(11) 0.0381(12) -0.0040(10) 0.0131(11) 0.0007(11) C18 0.0411(14) 0.0239(11) 0.0409(13) 0.0014(10) 0.0089(11) 0.0027(10) C19 0.0444(15) 0.0245(11) 0.0300(11) 0.0035(9) 0.0103(10) 0.0002(10) C101 0.0354(14) 0.0363(14) 0.0581(16) 0.0049(12) 0.0092(12) -0.0017(12) C111 0.070(2) 0.0425(15) 0.0470(15) -0.0053(13) 0.0226(15) -0.0202(15) C121 0.113(3) 0.0491(18) 0.0574(19) 0.0078(15) -0.034(2) 0.013(2) C131 0.0428(17) 0.0413(16) 0.106(3) -0.0199(17) 0.0079(17) 0.0049(14) C141 0.079(2) 0.0513(16) 0.0377(15) -0.0128(13) 0.0229(15) -0.0140(16) C151 0.0462(17) 0.0398(15) 0.0536(17) 0.0011(12) -0.0073(13) 0.0011(13) C161 0.083(2) 0.0431(15) 0.0402(14) -0.0062(12) -0.0016(15) -0.0220(16) C171 0.081(2) 0.0471(17) 0.0561(18) -0.0063(14) 0.0343(17) 0.0128(17) C181 0.0545(18) 0.0436(16) 0.0604(18) 0.0126(14) 0.0053(15) 0.0120(14) C191 0.0642(19) 0.0509(16) 0.0321(13) 0.0067(12) 0.0130(13) 0.0028(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl B 1.790(3) . ? B C11 1.588(3) . ? B C16 1.591(3) . ? C10 C19 1.334(3) . ? C10 C101 1.501(4) . ? C10 C16 1.510(3) . ? C11 C15 1.515(3) . ? C11 C12 1.527(4) . ? C11 C111 1.548(3) . ? C12 C13 1.350(4) . ? C12 C121 1.493(4) . ? C13 C14 1.447(4) . ? C13 C131 1.508(4) . ? C14 C15 1.337(3) . ? C14 C141 1.504(3) . ? C15 C151 1.483(4) . ? C16 C17 1.529(4) . ? C16 C161 1.533(4) . ? C17 C18 1.350(3) . ? C17 C171 1.504(3) . ? C18 C19 1.452(3) . ? C18 C181 1.494(4) . ? C19 C191 1.506(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 B C16 131.1(2) . . ? C11 B Cl 114.73(17) . . ? C16 B Cl 114.18(17) . . ? C19 C10 C101 127.6(2) . . ? C19 C10 C16 109.9(2) . . ? C101 C10 C16 122.2(2) . . ? C15 C11 C12 102.14(19) . . ? C15 C11 C111 109.9(2) . . ? C12 C11 C111 112.3(2) . . ? C15 C11 B 115.24(18) . . ? C12 C11 B 102.2(2) . . ? C111 C11 B 114.17(19) . . ? C13 C12 C121 127.8(3) . . ? C13 C12 C11 108.3(2) . . ? C121 C12 C11 123.7(3) . . ? C12 C13 C14 110.2(2) . . ? C12 C13 C131 126.2(3) . . ? C14 C13 C131 123.5(2) . . ? C15 C14 C13 109.8(2) . . ? C15 C14 C141 127.1(2) . . ? C13 C14 C141 123.1(2) . . ? C14 C15 C151 127.5(2) . . ? C14 C15 C11 109.5(2) . . ? C151 C15 C11 122.7(2) . . ? C10 C16 C17 101.92(18) . . ? C10 C16 C161 110.5(2) . . ? C17 C16 C161 111.8(2) . . ? C10 C16 B 115.19(19) . . ? C17 C16 B 101.8(2) . . ? C161 C16 B 114.5(2) . . ? C18 C17 C171 126.8(3) . . ? C18 C17 C16 108.6(2) . . ? C171 C17 C16 124.5(2) . . ? C17 C18 C19 109.8(2) . . ? C17 C18 C181 126.9(2) . . ? C19 C18 C181 123.3(2) . . ? C10 C19 C18 109.8(2) . . ? C10 C19 C191 127.1(2) . . ? C18 C19 C191 123.1(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.351 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.071 # Attachment 'MCp2BMe.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 664851' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; ? ; _chemical_melting_point 56-57C _chemical_formula_moiety 'c21 h33 b' _chemical_formula_sum 'C21 H33 B' _chemical_formula_weight 296.28 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 0.0000 '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' B B 0.0013 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M p2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.5688(15) _cell_length_b 17.863(4) _cell_length_c 27.857(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3766.4(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7702 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.045 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.057 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7702 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_sigmaI/netI 0.0943 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4672 _reflns_number_gt 2804 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement DENZO-SMN _computing_data_reduction ScalePack _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus, XP, Siemens, 1994' _computing_publication_material 'SHELXTL-Plus, XCIF, Siemens, 1994' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+0.6240P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -10(10) _refine_ls_number_reflns 4672 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1297 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1691 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.403 _refine_ls_shift/su_mean 0.009 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 C1 C 0.8536(5) 0.66076(18) 0.15801(12) 0.0257(8) Uani 1 1 d . . . H1A H 0.9477 0.6534 0.1354 0.039 Uiso 1 1 calc R . . H1B H 0.8078 0.6130 0.1678 0.039 Uiso 1 1 calc R . . H1C H 0.8977 0.6871 0.1855 0.039 Uiso 1 1 calc R . . C2 C 1.3566(5) 0.27611(18) 0.15176(12) 0.0259(8) Uani 1 1 d . . . H2A H 1.4522 0.2821 0.1294 0.039 Uiso 1 1 calc R . . H2B H 1.3979 0.2499 0.1797 0.039 Uiso 1 1 calc R . . H2C H 1.3130 0.3245 0.1610 0.039 Uiso 1 1 calc R . . C10 C 0.5751(6) 0.5953(2) 0.09388(12) 0.0284(9) Uani 1 1 d . . . C11 C 0.7431(6) 0.7952(2) 0.12325(14) 0.0328(10) Uani 1 1 d . . . C12 C 0.6476(6) 0.83041(19) 0.16591(12) 0.0292(9) Uani 1 1 d . . . C13 C 0.5086(6) 0.87037(19) 0.14921(12) 0.0294(10) Uani 1 1 d . . . C14 C 0.5099(6) 0.87054(19) 0.09697(13) 0.0309(10) Uani 1 1 d . . . C15 C 0.6449(7) 0.8276(2) 0.08155(12) 0.0335(10) Uani 1 1 d . . . C16 C 0.5205(5) 0.66366(19) 0.12230(13) 0.0282(9) Uani 1 1 d . . . C17 C 0.4547(6) 0.6290(2) 0.16854(12) 0.0287(9) Uani 1 1 d . . . C18 C 0.4723(6) 0.5536(2) 0.16595(13) 0.0300(9) Uani 1 1 d . . . C19 C 0.5459(5) 0.53302(18) 0.11934(13) 0.0271(8) Uani 1 1 d . . . C20 C 0.9569(6) 0.3101(2) 0.15989(13) 0.0289(9) Uani 1 1 d . . . C21 C 1.2406(6) 0.1411(2) 0.11761(14) 0.0328(10) Uani 1 1 d . . . C22 C 1.1444(6) 0.1089(2) 0.07545(13) 0.0311(10) Uani 1 1 d . . . C23 C 1.0093(6) 0.06582(19) 0.09109(13) 0.0297(9) Uani 1 1 d . . . C24 C 1.0059(6) 0.0657(2) 0.14332(13) 0.0315(10) Uani 1 1 d . . . C25 C 1.1442(6) 0.10681(19) 0.16001(13) 0.0332(10) Uani 1 1 d . . . C26 C 1.0240(6) 0.27466(19) 0.11388(12) 0.0282(9) Uani 1 1 d . . . C27 C 1.0819(6) 0.3429(2) 0.08510(12) 0.0304(9) Uani 1 1 d . . . C28 C 1.0521(6) 0.4056(2) 0.11113(14) 0.0333(10) Uani 1 1 d . . . C29 C 0.9764(6) 0.3850(2) 0.15746(13) 0.0321(10) Uani 1 1 d . . . C101 C 0.6520(7) 0.6010(2) 0.04418(12) 0.0377(11) Uani 1 1 d . . . H10A H 0.7656 0.6248 0.0458 0.057 Uiso 1 1 calc R . . H10B H 0.5746 0.6301 0.0242 0.057 Uiso 1 1 calc R . . H10C H 0.6647 0.5518 0.0308 0.057 Uiso 1 1 calc R . . C111 C 0.9411(6) 0.8137(2) 0.12187(18) 0.0501(12) Uani 1 1 d . . . H11A H 0.9946 0.7995 0.1517 0.075 Uiso 1 1 calc R . . H11B H 0.9565 0.8665 0.1169 0.075 Uiso 1 1 calc R . . H11C H 0.9960 0.7868 0.0961 0.075 Uiso 1 1 calc R . . C121 C 0.7112(7) 0.8242(2) 0.21717(13) 0.0460(13) Uani 1 1 d . . . H12A H 0.8275 0.8453 0.2197 0.069 Uiso 1 1 calc R . . H12B H 0.7144 0.7725 0.2265 0.069 Uiso 1 1 calc R . . H12C H 0.6320 0.8510 0.2379 0.069 Uiso 1 1 calc R . . C131 C 0.3751(7) 0.9111(2) 0.17901(14) 0.0446(12) Uani 1 1 d . . . H13A H 0.2586 0.9003 0.1673 0.067 Uiso 1 1 calc R . . H13B H 0.3965 0.9640 0.1770 0.067 Uiso 1 1 calc R . . H13C H 0.3845 0.8952 0.2118 0.067 Uiso 1 1 calc R . . C141 C 0.3744(7) 0.9088(2) 0.06675(14) 0.0443(12) Uani 1 1 d . . . H14A H 0.3228 0.9493 0.0845 0.066 Uiso 1 1 calc R . . H14B H 0.2840 0.8736 0.0580 0.066 Uiso 1 1 calc R . . H14C H 0.4293 0.9280 0.0382 0.066 Uiso 1 1 calc R . . C151 C 0.6961(7) 0.8138(2) 0.02968(13) 0.0485(13) Uani 1 1 d . . . H15A H 0.7988 0.7823 0.0286 0.073 Uiso 1 1 calc R . . H15B H 0.7218 0.8607 0.0143 0.073 Uiso 1 1 calc R . . H15C H 0.6002 0.7896 0.0133 0.073 Uiso 1 1 calc R . . C161 C 0.3643(6) 0.7026(2) 0.09697(13) 0.0333(10) Uani 1 1 d . . . H16A H 0.4012 0.7198 0.0659 0.050 Uiso 1 1 calc R . . H16B H 0.3259 0.7445 0.1159 0.050 Uiso 1 1 calc R . . H16C H 0.2686 0.6678 0.0934 0.050 Uiso 1 1 calc R . . C171 C 0.3737(6) 0.6737(2) 0.20822(13) 0.0375(10) Uani 1 1 d . . . H17A H 0.2996 0.7120 0.1948 0.056 Uiso 1 1 calc R . . H17B H 0.4654 0.6964 0.2271 0.056 Uiso 1 1 calc R . . H17C H 0.3040 0.6414 0.2282 0.056 Uiso 1 1 calc R . . C181 C 0.4217(6) 0.4973(2) 0.20381(14) 0.0411(11) Uani 1 1 d . . . H18A H 0.5262 0.4733 0.2159 0.062 Uiso 1 1 calc R . . H18B H 0.3448 0.4603 0.1900 0.062 Uiso 1 1 calc R . . H18C H 0.3620 0.5223 0.2296 0.062 Uiso 1 1 calc R . . C191 C 0.5720(6) 0.4525(2) 0.10380(14) 0.0372(10) Uani 1 1 d . . . H19A H 0.4591 0.4301 0.0975 0.056 Uiso 1 1 calc R . . H19B H 0.6306 0.4253 0.1289 0.056 Uiso 1 1 calc R . . H19C H 0.6427 0.4512 0.0752 0.056 Uiso 1 1 calc R . . C201 C 0.8730(7) 0.2654(2) 0.19972(13) 0.0408(11) Uani 1 1 d . . . H20A H 0.8901 0.2130 0.1938 0.061 Uiso 1 1 calc R . . H20B H 0.7488 0.2762 0.2010 0.061 Uiso 1 1 calc R . . H20C H 0.9266 0.2786 0.2298 0.061 Uiso 1 1 calc R . . C211 C 1.4397(6) 0.1222(2) 0.11660(17) 0.0449(11) Uani 1 1 d . . . H21A H 1.4956 0.1423 0.1447 0.067 Uiso 1 1 calc R . . H21B H 1.4924 0.1436 0.0884 0.067 Uiso 1 1 calc R . . H21C H 1.4547 0.0688 0.1160 0.067 Uiso 1 1 calc R . . C221 C 1.2005(7) 0.1235(2) 0.02489(13) 0.0452(12) Uani 1 1 d . . . H22A H 1.3032 0.0942 0.0176 0.068 Uiso 1 1 calc R . . H22B H 1.2278 0.1757 0.0212 0.068 Uiso 1 1 calc R . . H22C H 1.1064 0.1102 0.0034 0.068 Uiso 1 1 calc R . . C231 C 0.8760(7) 0.0259(2) 0.06030(15) 0.0440(12) Uani 1 1 d . . . H23A H 0.7610 0.0469 0.0657 0.066 Uiso 1 1 calc R . . H23B H 0.8746 -0.0263 0.0685 0.066 Uiso 1 1 calc R . . H23C H 0.9074 0.0316 0.0271 0.066 Uiso 1 1 calc R . . C241 C 0.8733(7) 0.0246(2) 0.17242(15) 0.0462(12) Uani 1 1 d . . . H24A H 0.8500 -0.0231 0.1579 0.069 Uiso 1 1 calc R . . H24B H 0.7659 0.0531 0.1739 0.069 Uiso 1 1 calc R . . H24C H 0.9182 0.0173 0.2043 0.069 Uiso 1 1 calc R . . C251 C 1.2015(7) 0.1139(2) 0.21124(13) 0.0450(12) Uani 1 1 d . . . H25A H 1.2058 0.1658 0.2200 0.067 Uiso 1 1 calc R . . H25B H 1.3167 0.0921 0.2150 0.067 Uiso 1 1 calc R . . H25C H 1.1189 0.0883 0.2316 0.067 Uiso 1 1 calc R . . C261 C 0.8668(6) 0.2355(2) 0.08812(13) 0.0366(10) Uani 1 1 d . . . H26A H 0.8260 0.1944 0.1073 0.055 Uiso 1 1 calc R . . H26B H 0.9051 0.2173 0.0574 0.055 Uiso 1 1 calc R . . H26C H 0.7724 0.2707 0.0837 0.055 Uiso 1 1 calc R . . C271 C 1.1599(7) 0.3362(2) 0.03586(13) 0.0427(11) Uani 1 1 d . . . H27A H 1.0905 0.3021 0.0171 0.064 Uiso 1 1 calc R . . H27B H 1.2788 0.3179 0.0382 0.064 Uiso 1 1 calc R . . H27C H 1.1604 0.3845 0.0207 0.064 Uiso 1 1 calc R . . C281 C 1.0798(7) 0.4853(2) 0.09546(16) 0.0438(12) Uani 1 1 d . . . H28A H 1.1613 0.5094 0.1169 0.066 Uiso 1 1 calc R . . H28B H 0.9689 0.5114 0.0961 0.066 Uiso 1 1 calc R . . H28C H 1.1267 0.4860 0.0634 0.066 Uiso 1 1 calc R . . C291 C 0.9270(7) 0.4416(2) 0.19565(15) 0.0453(12) Uani 1 1 d . . . H29A H 0.8326 0.4726 0.1841 0.068 Uiso 1 1 calc R . . H29B H 1.0278 0.4721 0.2030 0.068 Uiso 1 1 calc R . . H29C H 0.8894 0.4158 0.2241 0.068 Uiso 1 1 calc R . . B1 B 0.7008(6) 0.7082(2) 0.13367(14) 0.0283(11) Uani 1 1 d . . . B2 B 1.2012(7) 0.2293(2) 0.12704(14) 0.0304(11) 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 C1 0.022(2) 0.0198(16) 0.0352(19) -0.0022(15) -0.0011(19) -0.0020(18) C2 0.023(2) 0.0210(17) 0.0338(19) 0.0002(15) 0.0005(18) 0.0000(18) C10 0.024(2) 0.034(2) 0.0267(19) -0.0079(16) 0.0001(17) -0.0039(19) C11 0.026(2) 0.031(2) 0.041(2) -0.0027(18) -0.001(2) 0.0010(19) C12 0.035(3) 0.0230(18) 0.0300(19) 0.0000(15) -0.0080(19) -0.003(2) C13 0.035(3) 0.0235(18) 0.0302(19) -0.0029(15) 0.0003(19) -0.001(2) C14 0.033(3) 0.0256(19) 0.034(2) 0.0020(16) -0.0060(19) -0.002(2) C15 0.042(3) 0.029(2) 0.029(2) 0.0008(16) 0.004(2) -0.008(2) C16 0.029(2) 0.0264(18) 0.0296(18) -0.0005(16) 0.0023(19) 0.0022(19) C17 0.025(2) 0.033(2) 0.0281(19) -0.0018(15) 0.0048(18) -0.0016(19) C18 0.024(2) 0.035(2) 0.031(2) 0.0019(16) 0.0001(18) -0.001(2) C19 0.024(2) 0.0239(17) 0.0339(19) -0.0024(15) 0.0024(18) -0.0021(17) C20 0.024(2) 0.033(2) 0.0293(19) 0.0027(16) 0.0010(18) 0.0025(19) C21 0.032(3) 0.0268(19) 0.040(2) -0.0008(17) -0.002(2) -0.0022(19) C22 0.031(3) 0.0276(19) 0.035(2) -0.0060(16) 0.001(2) 0.002(2) C23 0.030(3) 0.0217(17) 0.038(2) -0.0014(15) -0.0013(19) 0.0000(19) C24 0.034(3) 0.0230(18) 0.037(2) 0.0050(16) 0.000(2) 0.001(2) C25 0.040(3) 0.0232(18) 0.036(2) -0.0001(16) -0.001(2) 0.003(2) C26 0.030(2) 0.0258(18) 0.0293(19) 0.0011(15) 0.0002(18) 0.0000(18) C27 0.028(2) 0.036(2) 0.0275(19) 0.0023(16) 0.0013(18) -0.003(2) C28 0.026(2) 0.0301(19) 0.044(2) 0.0015(17) -0.004(2) 0.004(2) C29 0.027(3) 0.033(2) 0.036(2) -0.0049(16) -0.0028(19) 0.005(2) C101 0.047(3) 0.036(2) 0.030(2) -0.0024(17) 0.010(2) 0.002(2) C111 0.036(3) 0.037(2) 0.078(3) 0.010(2) -0.002(3) -0.006(2) C121 0.062(4) 0.036(2) 0.040(2) -0.0008(18) -0.015(2) 0.001(2) C131 0.044(3) 0.044(2) 0.045(2) -0.0093(19) 0.002(2) 0.003(3) C141 0.052(3) 0.037(2) 0.044(2) 0.0005(19) -0.013(2) 0.005(3) C151 0.065(4) 0.042(2) 0.039(2) 0.0012(19) 0.017(3) -0.006(3) C161 0.026(2) 0.035(2) 0.039(2) 0.0000(16) -0.005(2) -0.001(2) C171 0.041(3) 0.038(2) 0.034(2) -0.0035(17) 0.006(2) 0.001(2) C181 0.038(3) 0.041(2) 0.044(2) 0.0080(19) 0.002(2) -0.005(2) C191 0.038(3) 0.034(2) 0.039(2) -0.0081(17) 0.001(2) -0.002(2) C201 0.039(3) 0.044(2) 0.040(2) 0.0032(18) 0.010(2) -0.001(2) C211 0.039(3) 0.027(2) 0.068(3) -0.006(2) -0.003(3) 0.003(2) C221 0.056(3) 0.043(2) 0.037(2) -0.0043(18) 0.010(2) 0.001(2) C231 0.042(3) 0.038(2) 0.052(3) -0.0018(19) -0.014(2) -0.003(2) C241 0.051(3) 0.036(2) 0.051(3) 0.0060(19) 0.002(2) -0.004(3) C251 0.062(4) 0.036(2) 0.037(2) 0.0007(17) -0.011(2) 0.000(2) C261 0.033(3) 0.035(2) 0.042(2) -0.0003(17) -0.008(2) 0.007(2) C271 0.051(3) 0.040(2) 0.036(2) 0.0041(18) 0.006(2) -0.003(2) C281 0.044(3) 0.029(2) 0.058(3) 0.006(2) -0.004(2) 0.001(2) C291 0.042(3) 0.042(2) 0.052(3) -0.011(2) 0.001(2) 0.004(2) B1 0.028(3) 0.030(2) 0.026(2) -0.0036(17) 0.003(2) 0.003(2) B2 0.033(3) 0.030(2) 0.028(2) 0.0032(19) 0.007(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 B1 1.586(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 B2 1.599(6) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C10 C19 1.338(5) . ? C10 C101 1.505(5) . ? C10 C16 1.513(5) . ? C11 C15 1.495(6) . ? C11 C12 1.526(5) . ? C11 C111 1.535(6) . ? C11 B1 1.614(6) . ? C12 C13 1.354(5) . ? C12 C121 1.511(5) . ? C13 C14 1.455(5) . ? C13 C131 1.497(6) . ? C14 C15 1.347(6) . ? C14 C141 1.492(6) . ? C15 C151 1.516(5) . ? C16 C17 1.513(5) . ? C16 C161 1.542(6) . ? C16 B1 1.611(6) . ? C17 C18 1.355(5) . ? C17 C171 1.495(5) . ? C18 C19 1.460(5) . ? C18 C181 1.507(5) . ? C19 C191 1.514(5) . ? C20 C29 1.348(5) . ? C20 C201 1.507(5) . ? C20 C26 1.517(5) . ? C21 C22 1.497(5) . ? C21 C25 1.517(5) . ? C21 C211 1.545(6) . ? C21 B2 1.626(6) . ? C22 C23 1.351(6) . ? C22 C221 1.494(5) . ? C23 C24 1.455(5) . ? C23 C231 1.504(6) . ? C24 C25 1.360(6) . ? C24 C241 1.484(6) . ? C25 C251 1.497(5) . ? C26 C27 1.523(5) . ? C26 C261 1.556(6) . ? C26 B2 1.609(6) . ? C27 C28 1.353(5) . ? C27 C271 1.498(5) . ? C28 C29 1.459(5) . ? C28 C281 1.504(5) . ? C29 C291 1.514(5) . ? C101 H10A 0.9600 . ? C101 H10B 0.9600 . ? C101 H10C 0.9600 . ? C111 H11A 0.9600 . ? C111 H11B 0.9600 . ? C111 H11C 0.9600 . ? C121 H12A 0.9600 . ? C121 H12B 0.9600 . ? C121 H12C 0.9600 . ? C131 H13A 0.9600 . ? C131 H13B 0.9600 . ? C131 H13C 0.9600 . ? C141 H14A 0.9600 . ? C141 H14B 0.9600 . ? C141 H14C 0.9600 . ? C151 H15A 0.9600 . ? C151 H15B 0.9600 . ? C151 H15C 0.9600 . ? C161 H16A 0.9600 . ? C161 H16B 0.9600 . ? C161 H16C 0.9600 . ? C171 H17A 0.9600 . ? C171 H17B 0.9600 . ? C171 H17C 0.9600 . ? C181 H18A 0.9600 . ? C181 H18B 0.9600 . ? C181 H18C 0.9600 . ? C191 H19A 0.9600 . ? C191 H19B 0.9600 . ? C191 H19C 0.9600 . ? C201 H20A 0.9600 . ? C201 H20B 0.9600 . ? C201 H20C 0.9600 . ? C211 H21A 0.9600 . ? C211 H21B 0.9600 . ? C211 H21C 0.9600 . ? C221 H22A 0.9600 . ? C221 H22B 0.9600 . ? C221 H22C 0.9600 . ? C231 H23A 0.9600 . ? C231 H23B 0.9600 . ? C231 H23C 0.9600 . ? C241 H24A 0.9600 . ? C241 H24B 0.9600 . ? C241 H24C 0.9600 . ? C251 H25A 0.9600 . ? C251 H25B 0.9600 . ? C251 H25C 0.9600 . ? C261 H26A 0.9600 . ? C261 H26B 0.9600 . ? C261 H26C 0.9600 . ? C271 H27A 0.9600 . ? C271 H27B 0.9600 . ? C271 H27C 0.9600 . ? C281 H28A 0.9600 . ? C281 H28B 0.9600 . ? C281 H28C 0.9600 . ? C291 H29A 0.9600 . ? C291 H29B 0.9600 . ? C291 H29C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B1 C1 H1A 109.5 . . ? B1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? B1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? B2 C2 H2A 109.5 . . ? B2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? B2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C19 C10 C101 127.4(3) . . ? C19 C10 C16 110.4(3) . . ? C101 C10 C16 122.2(3) . . ? C15 C11 C12 102.1(3) . . ? C15 C11 C111 112.5(4) . . ? C12 C11 C111 113.2(4) . . ? C15 C11 B1 114.5(3) . . ? C12 C11 B1 99.3(3) . . ? C111 C11 B1 113.9(4) . . ? C13 C12 C121 127.7(4) . . ? C13 C12 C11 108.5(3) . . ? C121 C12 C11 123.7(4) . . ? C12 C13 C14 109.8(4) . . ? C12 C13 C131 126.2(4) . . ? C14 C13 C131 123.9(4) . . ? C15 C14 C13 108.8(4) . . ? C15 C14 C141 127.0(4) . . ? C13 C14 C141 124.1(4) . . ? C14 C15 C11 110.4(3) . . ? C14 C15 C151 126.2(4) . . ? C11 C15 C151 123.4(4) . . ? C10 C16 C17 101.8(3) . . ? C10 C16 C161 109.5(3) . . ? C17 C16 C161 108.8(3) . . ? C10 C16 B1 105.7(3) . . ? C17 C16 B1 108.3(3) . . ? C161 C16 B1 121.1(3) . . ? C18 C17 C171 127.6(3) . . ? C18 C17 C16 109.2(3) . . ? C171 C17 C16 123.1(3) . . ? C17 C18 C19 109.6(3) . . ? C17 C18 C181 127.0(4) . . ? C19 C18 C181 123.5(3) . . ? C10 C19 C18 109.0(3) . . ? C10 C19 C191 128.1(3) . . ? C18 C19 C191 122.9(3) . . ? C29 C20 C201 127.5(4) . . ? C29 C20 C26 109.6(3) . . ? C201 C20 C26 122.8(3) . . ? C22 C21 C25 102.8(3) . . ? C22 C21 C211 112.1(4) . . ? C25 C21 C211 113.3(4) . . ? C22 C21 B2 114.2(3) . . ? C25 C21 B2 100.2(3) . . ? C211 C21 B2 113.2(3) . . ? C23 C22 C221 128.2(4) . . ? C23 C22 C21 109.5(3) . . ? C221 C22 C21 122.3(4) . . ? C22 C23 C24 109.7(4) . . ? C22 C23 C231 126.4(4) . . ? C24 C23 C231 123.9(4) . . ? C25 C24 C23 109.1(4) . . ? C25 C24 C241 126.9(4) . . ? C23 C24 C241 124.0(4) . . ? C24 C25 C251 126.5(4) . . ? C24 C25 C21 108.8(3) . . ? C251 C25 C21 124.6(4) . . ? C20 C26 C27 101.9(3) . . ? C20 C26 C261 108.7(3) . . ? C27 C26 C261 109.7(3) . . ? C20 C26 B2 107.3(3) . . ? C27 C26 B2 106.4(3) . . ? C261 C26 B2 121.1(3) . . ? C28 C27 C271 128.5(3) . . ? C28 C27 C26 109.4(3) . . ? C271 C27 C26 122.1(3) . . ? C27 C28 C29 109.3(3) . . ? C27 C28 C281 127.2(4) . . ? C29 C28 C281 123.4(3) . . ? C20 C29 C28 109.7(3) . . ? C20 C29 C291 126.9(4) . . ? C28 C29 C291 123.4(3) . . ? C10 C101 H10A 109.5 . . ? C10 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C10 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C11 C111 H11A 109.5 . . ? C11 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C11 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C13 C131 H13A 109.5 . . ? C13 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C13 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C15 C151 H15A 109.5 . . ? C15 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C15 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? C16 C161 H16A 109.5 . . ? C16 C161 H16B 109.5 . . ? H16A C161 H16B 109.5 . . ? C16 C161 H16C 109.5 . . ? H16A C161 H16C 109.5 . . ? H16B C161 H16C 109.5 . . ? C17 C171 H17A 109.5 . . ? C17 C171 H17B 109.5 . . ? H17A C171 H17B 109.5 . . ? C17 C171 H17C 109.5 . . ? H17A C171 H17C 109.5 . . ? H17B C171 H17C 109.5 . . ? C18 C181 H18A 109.5 . . ? C18 C181 H18B 109.5 . . ? H18A C181 H18B 109.5 . . ? C18 C181 H18C 109.5 . . ? H18A C181 H18C 109.5 . . ? H18B C181 H18C 109.5 . . ? C19 C191 H19A 109.5 . . ? C19 C191 H19B 109.5 . . ? H19A C191 H19B 109.5 . . ? C19 C191 H19C 109.5 . . ? H19A C191 H19C 109.5 . . ? H19B C191 H19C 109.5 . . ? C20 C201 H20A 109.5 . . ? C20 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C20 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C21 C211 H21A 109.5 . . ? C21 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C21 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C23 C231 H23A 109.5 . . ? C23 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C23 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C24 C241 H24A 109.5 . . ? C24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? C24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C25 C251 H25A 109.5 . . ? C25 C251 H25B 109.5 . . ? H25A C251 H25B 109.5 . . ? C25 C251 H25C 109.5 . . ? H25A C251 H25C 109.5 . . ? H25B C251 H25C 109.5 . . ? C26 C261 H26A 109.5 . . ? C26 C261 H26B 109.5 . . ? H26A C261 H26B 109.5 . . ? C26 C261 H26C 109.5 . . ? H26A C261 H26C 109.5 . . ? H26B C261 H26C 109.5 . . ? C27 C271 H27A 109.5 . . ? C27 C271 H27B 109.5 . . ? H27A C271 H27B 109.5 . . ? C27 C271 H27C 109.5 . . ? H27A C271 H27C 109.5 . . ? H27B C271 H27C 109.5 . . ? C28 C281 H28A 109.5 . . ? C28 C281 H28B 109.5 . . ? H28A C281 H28B 109.5 . . ? C28 C281 H28C 109.5 . . ? H28A C281 H28C 109.5 . . ? H28B C281 H28C 109.5 . . ? C29 C291 H29A 109.5 . . ? C29 C291 H29B 109.5 . . ? H29A C291 H29B 109.5 . . ? C29 C291 H29C 109.5 . . ? H29A C291 H29C 109.5 . . ? H29B C291 H29C 109.5 . . ? C1 B1 C16 115.9(3) . . ? C1 B1 C11 116.6(4) . . ? C16 B1 C11 127.5(4) . . ? C2 B2 C26 116.7(3) . . ? C2 B2 C21 116.2(4) . . ? C26 B2 C21 127.1(4) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.176 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.049 # Attachment 'MCp2Ga(mu-Cl)2GaMCpArF.cif' data_9 _database_code_depnum_ccdc_archive 'CCDC 664844' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H45 Cl2 F5 Ga2' _chemical_formula_weight 783.06 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.844(3) _cell_length_b 13.772(3) _cell_length_c 17.627(4) _cell_angle_alpha 90.00 _cell_angle_beta 118.04(3) _cell_angle_gamma 90.00 _cell_volume 3609.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 18562 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 27.53 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 1.691 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18562 _diffrn_reflns_av_R_equivalents 0.1238 _diffrn_reflns_av_sigmaI/netI 0.1319 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.53 _reflns_number_total 8235 _reflns_number_gt 5002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+2.8391P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8235 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 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 C11 C 0.1991(3) 0.3970(3) 0.4917(3) 0.0419(11) Uani 1 1 d . . . C12 C 0.2650(3) 0.3244(3) 0.4952(3) 0.0463(11) Uani 1 1 d . . . C13 C 0.2814(3) 0.2606(3) 0.5596(3) 0.0496(12) Uani 1 1 d . . . C14 C 0.2223(3) 0.2838(3) 0.5960(3) 0.0499(12) Uani 1 1 d . . . C15 C 0.1718(3) 0.3629(3) 0.5557(3) 0.0499(12) Uani 1 1 d . . . C21 C 0.4075(3) 0.4977(3) 0.6760(2) 0.0317(9) Uani 1 1 d . . . C22 C 0.4783(3) 0.4411(3) 0.6655(3) 0.0390(10) Uani 1 1 d . . . C23 C 0.5024(3) 0.3629(3) 0.7179(2) 0.0386(10) Uani 1 1 d . . . C24 C 0.4489(3) 0.3617(3) 0.7639(2) 0.0358(9) Uani 1 1 d . . . C25 C 0.3950(3) 0.4396(3) 0.7415(2) 0.0336(9) Uani 1 1 d . . . C31 C 0.1307(3) 0.7702(3) 0.3783(2) 0.0324(9) Uani 1 1 d . . . C32 C 0.1114(3) 0.8520(3) 0.4219(2) 0.0359(9) Uani 1 1 d . . . C33 C 0.1502(3) 0.9334(3) 0.4108(3) 0.0518(13) Uani 1 1 d . . . C34 C 0.1913(3) 0.9103(4) 0.3573(3) 0.0564(14) Uani 1 1 d . . . C35 C 0.1784(3) 0.8149(4) 0.3344(3) 0.0461(12) Uani 1 1 d . . . C41 C 0.3432(3) 0.8200(3) 0.5483(2) 0.0297(8) Uani 1 1 d . . . C42 C 0.3485(3) 0.8735(3) 0.6167(2) 0.0353(9) Uani 1 1 d . . . C43 C 0.4163(3) 0.9392(3) 0.6619(2) 0.0402(10) Uani 1 1 d . . . C44 C 0.4829(3) 0.9523(3) 0.6389(3) 0.0452(11) Uani 1 1 d . . . C45 C 0.4809(3) 0.9005(3) 0.5713(3) 0.0434(11) Uani 1 1 d . . . C46 C 0.4121(3) 0.8371(3) 0.5279(2) 0.0350(9) Uani 1 1 d . . . C111 C 0.1278(4) 0.4363(4) 0.4055(3) 0.0658(16) Uani 1 1 d . . . H11A H 0.0930 0.4871 0.4154 0.099 Uiso 1 1 calc R . . H11B H 0.0875 0.3835 0.3721 0.099 Uiso 1 1 calc R . . H11C H 0.1571 0.4636 0.3737 0.099 Uiso 1 1 calc R . . C121 C 0.3079(4) 0.3232(4) 0.4367(3) 0.0768(18) Uani 1 1 d . . . H12A H 0.2986 0.3862 0.4079 0.115 Uiso 1 1 calc R . . H12B H 0.2804 0.2719 0.3936 0.115 Uiso 1 1 calc R . . H12C H 0.3725 0.3108 0.4708 0.115 Uiso 1 1 calc R . . C131 C 0.3487(4) 0.1799(3) 0.5901(3) 0.0693(16) Uani 1 1 d . . . H13A H 0.3182 0.1184 0.5875 0.104 Uiso 1 1 calc R . . H13B H 0.3943 0.1926 0.6495 0.104 Uiso 1 1 calc R . . H13C H 0.3776 0.1759 0.5533 0.104 Uiso 1 1 calc R . . C141 C 0.2200(4) 0.2271(4) 0.6681(4) 0.0809(18) Uani 1 1 d . . . H14A H 0.2776 0.2343 0.7204 0.121 Uiso 1 1 calc R . . H14B H 0.2094 0.1583 0.6522 0.121 Uiso 1 1 calc R . . H14C H 0.1715 0.2518 0.6786 0.121 Uiso 1 1 calc R . . C151 C 0.0968(4) 0.4068(4) 0.5668(4) 0.0724(16) Uani 1 1 d . . . H15A H 0.0391 0.3889 0.5180 0.109 Uiso 1 1 calc R . . H15B H 0.1030 0.4777 0.5696 0.109 Uiso 1 1 calc R . . H15C H 0.0992 0.3827 0.6202 0.109 Uiso 1 1 calc R . . C211 C 0.4344(3) 0.6035(3) 0.7020(3) 0.0416(10) Uani 1 1 d . . . H21A H 0.4425 0.6366 0.6569 0.062 Uiso 1 1 calc R . . H21B H 0.4909 0.6055 0.7560 0.062 Uiso 1 1 calc R . . H21C H 0.3871 0.6362 0.7098 0.062 Uiso 1 1 calc R . . C221 C 0.5199(4) 0.4755(5) 0.6119(3) 0.0737(17) Uani 1 1 d . . . H22A H 0.5364 0.5441 0.6242 0.111 Uiso 1 1 calc R . . H22B H 0.4768 0.4679 0.5509 0.111 Uiso 1 1 calc R . . H22C H 0.5740 0.4371 0.6254 0.111 Uiso 1 1 calc R . . C231 C 0.5728(3) 0.2883(4) 0.7308(3) 0.0590(13) Uani 1 1 d . . . H23A H 0.5448 0.2239 0.7159 0.088 Uiso 1 1 calc R . . H23B H 0.6193 0.2886 0.7911 0.088 Uiso 1 1 calc R . . H23C H 0.6000 0.3037 0.6939 0.088 Uiso 1 1 calc R . . C241 C 0.4591(4) 0.2841(3) 0.8286(3) 0.0579(13) Uani 1 1 d . . . H24A H 0.5186 0.2895 0.8789 0.087 Uiso 1 1 calc R . . H24B H 0.4529 0.2198 0.8025 0.087 Uiso 1 1 calc R . . H24C H 0.4125 0.2925 0.8465 0.087 Uiso 1 1 calc R . . C251 C 0.3322(3) 0.4711(3) 0.7758(3) 0.0493(12) Uani 1 1 d . . . H25A H 0.2710 0.4769 0.7282 0.074 Uiso 1 1 calc R . . H25B H 0.3517 0.5340 0.8046 0.074 Uiso 1 1 calc R . . H25C H 0.3330 0.4227 0.8170 0.074 Uiso 1 1 calc R . . C311 C 0.0631(3) 0.6899(3) 0.3361(3) 0.0473(11) Uani 1 1 d . . . H31A H 0.0462 0.6622 0.3777 0.071 Uiso 1 1 calc R . . H31B H 0.0898 0.6391 0.3163 0.071 Uiso 1 1 calc R . . H31C H 0.0096 0.7161 0.2870 0.071 Uiso 1 1 calc R . . C321 C 0.0542(3) 0.8436(4) 0.4650(3) 0.0573(13) Uani 1 1 d . . . H32A H 0.0652 0.7809 0.4946 0.086 Uiso 1 1 calc R . . H32B H -0.0093 0.8481 0.4220 0.086 Uiso 1 1 calc R . . H32C H 0.0688 0.8962 0.5070 0.086 Uiso 1 1 calc R . . C331 C 0.1490(5) 1.0318(4) 0.4470(4) 0.095(2) Uani 1 1 d . . . H33A H 0.1816 1.0781 0.4297 0.142 Uiso 1 1 calc R . . H33B H 0.1780 1.0279 0.5099 0.142 Uiso 1 1 calc R . . H33C H 0.0866 1.0534 0.4252 0.142 Uiso 1 1 calc R . . C341 C 0.2412(4) 0.9842(5) 0.3321(5) 0.110(3) Uani 1 1 d . . . H34A H 0.2899 1.0129 0.3841 0.165 Uiso 1 1 calc R . . H34B H 0.1995 1.0354 0.2974 0.165 Uiso 1 1 calc R . . H34C H 0.2666 0.9523 0.2987 0.165 Uiso 1 1 calc R . . C351 C 0.2011(4) 0.7604(5) 0.2737(3) 0.084(2) Uani 1 1 d . . . H35A H 0.1469 0.7531 0.2182 0.126 Uiso 1 1 calc R . . H35B H 0.2244 0.6960 0.2975 0.126 Uiso 1 1 calc R . . H35C H 0.2468 0.7962 0.2657 0.126 Uiso 1 1 calc R . . F42 F 0.28442(17) 0.86236(18) 0.64135(15) 0.0486(6) Uani 1 1 d . . . F43 F 0.4188(2) 0.98861(17) 0.72871(15) 0.0575(7) Uani 1 1 d . . . F44 F 0.54989(19) 1.0154(2) 0.68250(18) 0.0679(8) Uani 1 1 d . . . F45 F 0.54625(18) 0.9135(2) 0.54890(18) 0.0644(8) Uani 1 1 d . . . F46 F 0.41188(18) 0.78863(19) 0.46058(16) 0.0515(7) Uani 1 1 d . . . Cl1 Cl 0.20778(6) 0.63840(7) 0.57432(6) 0.0337(2) Uani 1 1 d . . . Cl2 Cl 0.31157(7) 0.59175(7) 0.46054(6) 0.0353(2) Uani 1 1 d . . . Ga1 Ga 0.29227(3) 0.49203(3) 0.56673(3) 0.03090(12) Uani 1 1 d . . . Ga2 Ga 0.24345(3) 0.72925(3) 0.48266(3) 0.02983(12) 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 C11 0.042(3) 0.029(2) 0.045(2) -0.0009(19) 0.012(2) -0.010(2) C12 0.051(3) 0.040(2) 0.044(2) -0.012(2) 0.018(2) -0.006(2) C13 0.047(3) 0.031(2) 0.052(3) -0.008(2) 0.008(2) -0.003(2) C14 0.048(3) 0.039(2) 0.055(3) 0.006(2) 0.017(2) -0.012(2) C15 0.041(3) 0.038(2) 0.067(3) -0.002(2) 0.022(2) -0.012(2) C21 0.029(2) 0.036(2) 0.0290(18) 0.0020(17) 0.0126(16) 0.0027(19) C22 0.027(2) 0.058(3) 0.035(2) -0.002(2) 0.0165(18) 0.006(2) C23 0.034(2) 0.047(2) 0.032(2) -0.0059(19) 0.0127(18) 0.007(2) C24 0.041(2) 0.036(2) 0.031(2) -0.0009(17) 0.0175(18) 0.002(2) C25 0.031(2) 0.043(2) 0.0311(19) -0.0024(18) 0.0177(17) 0.001(2) C31 0.028(2) 0.037(2) 0.0284(19) 0.0042(17) 0.0095(16) 0.0026(19) C32 0.028(2) 0.042(2) 0.030(2) -0.0019(18) 0.0072(17) 0.000(2) C33 0.034(3) 0.042(3) 0.048(3) 0.004(2) -0.007(2) -0.005(2) C34 0.024(2) 0.069(3) 0.054(3) 0.032(3) 0.000(2) -0.008(3) C35 0.029(2) 0.073(3) 0.031(2) 0.018(2) 0.0101(18) 0.006(2) C41 0.027(2) 0.0273(19) 0.033(2) 0.0042(17) 0.0126(17) -0.0001(18) C42 0.034(2) 0.037(2) 0.037(2) 0.0038(19) 0.0181(18) 0.003(2) C43 0.046(3) 0.033(2) 0.032(2) -0.0013(18) 0.011(2) 0.001(2) C44 0.036(3) 0.035(2) 0.047(3) 0.003(2) 0.005(2) -0.011(2) C45 0.034(2) 0.047(3) 0.049(3) 0.008(2) 0.019(2) -0.007(2) C46 0.032(2) 0.038(2) 0.034(2) 0.0000(18) 0.0146(18) -0.003(2) C111 0.055(3) 0.046(3) 0.059(3) 0.003(2) -0.004(2) -0.016(3) C121 0.099(5) 0.075(4) 0.057(3) -0.026(3) 0.037(3) 0.001(4) C131 0.059(3) 0.043(3) 0.077(4) -0.009(3) 0.007(3) 0.007(3) C141 0.080(4) 0.068(3) 0.092(4) 0.023(3) 0.039(4) -0.023(4) C151 0.049(3) 0.063(3) 0.117(5) 0.003(3) 0.049(3) -0.005(3) C211 0.034(2) 0.040(2) 0.041(2) 0.0015(19) 0.0093(19) -0.004(2) C221 0.053(3) 0.125(5) 0.061(3) 0.028(3) 0.042(3) 0.025(4) C231 0.050(3) 0.063(3) 0.059(3) -0.005(2) 0.022(2) 0.019(3) C241 0.071(4) 0.045(3) 0.057(3) 0.012(2) 0.029(3) 0.013(3) C251 0.059(3) 0.053(3) 0.051(3) 0.006(2) 0.039(2) 0.013(3) C311 0.035(2) 0.041(2) 0.045(2) 0.000(2) 0.002(2) 0.000(2) C321 0.048(3) 0.077(3) 0.046(3) 0.005(2) 0.020(2) 0.029(3) C331 0.088(5) 0.038(3) 0.082(4) -0.005(3) -0.023(3) 0.002(3) C341 0.050(4) 0.124(6) 0.124(5) 0.078(5) 0.016(4) -0.022(4) C351 0.075(4) 0.145(6) 0.046(3) 0.030(3) 0.040(3) 0.045(4) F42 0.0500(15) 0.0533(14) 0.0522(14) -0.0095(12) 0.0319(13) -0.0028(14) F43 0.074(2) 0.0450(14) 0.0435(14) -0.0117(12) 0.0191(14) -0.0055(15) F44 0.0522(18) 0.0573(17) 0.0716(18) -0.0107(14) 0.0104(15) -0.0300(16) F45 0.0420(16) 0.0742(19) 0.086(2) -0.0028(16) 0.0370(15) -0.0206(15) F46 0.0513(16) 0.0632(16) 0.0548(15) -0.0108(13) 0.0372(13) -0.0138(14) Cl1 0.0325(5) 0.0369(5) 0.0380(5) 0.0039(4) 0.0217(4) 0.0015(5) Cl2 0.0386(6) 0.0388(5) 0.0352(5) 0.0014(4) 0.0229(4) 0.0024(5) Ga1 0.0281(2) 0.0347(2) 0.0294(2) 0.00004(18) 0.01313(18) -0.0008(2) Ga2 0.0248(2) 0.0343(2) 0.0289(2) 0.00084(18) 0.01135(17) -0.0029(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 C12 1.473(6) . ? C11 C15 1.480(6) . ? C11 C111 1.527(6) . ? C11 Ga1 1.993(4) . ? C12 C13 1.357(6) . ? C12 C121 1.512(7) . ? C13 C14 1.451(7) . ? C13 C131 1.495(6) . ? C14 C15 1.359(6) . ? C14 C141 1.508(7) . ? C15 C151 1.495(7) . ? C21 C25 1.498(5) . ? C21 C22 1.507(5) . ? C21 C211 1.532(5) . ? C21 Ga1 1.992(4) . ? C22 C23 1.350(6) . ? C22 C221 1.495(6) . ? C23 C24 1.469(6) . ? C23 C231 1.503(6) . ? C24 C25 1.339(5) . ? C24 C241 1.514(6) . ? C25 C251 1.509(6) . ? C31 C32 1.483(6) . ? C31 C35 1.487(6) . ? C31 C311 1.508(6) . ? C31 Ga2 2.006(4) . ? C32 C33 1.359(6) . ? C32 C321 1.486(6) . ? C33 C34 1.443(7) . ? C33 C331 1.502(7) . ? C34 C35 1.362(7) . ? C34 C341 1.514(7) . ? C35 C351 1.496(7) . ? C41 C42 1.379(5) . ? C41 C46 1.389(5) . ? C41 Ga2 1.974(4) . ? C42 F42 1.349(5) . ? C42 C43 1.379(6) . ? C43 F43 1.344(5) . ? C43 C44 1.372(6) . ? C44 F44 1.343(5) . ? C44 C45 1.375(6) . ? C45 F45 1.345(5) . ? C45 C46 1.363(6) . ? C46 F46 1.359(4) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C151 H15A 0.9800 . ? C151 H15B 0.9800 . ? C151 H15C 0.9800 . ? C211 H21A 0.9800 . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C231 H23A 0.9800 . ? C231 H23B 0.9800 . ? C231 H23C 0.9800 . ? C241 H24A 0.9800 . ? C241 H24B 0.9800 . ? C241 H24C 0.9800 . ? C251 H25A 0.9800 . ? C251 H25B 0.9800 . ? C251 H25C 0.9800 . ? C311 H31A 0.9800 . ? C311 H31B 0.9800 . ? C311 H31C 0.9800 . ? C321 H32A 0.9800 . ? C321 H32B 0.9800 . ? C321 H32C 0.9800 . ? C331 H33A 0.9800 . ? C331 H33B 0.9800 . ? C331 H33C 0.9800 . ? C341 H34A 0.9800 . ? C341 H34B 0.9800 . ? C341 H34C 0.9800 . ? C351 H35A 0.9800 . ? C351 H35B 0.9800 . ? C351 H35C 0.9800 . ? Cl1 Ga2 2.3345(10) . ? Cl1 Ga1 2.5071(11) . ? Cl2 Ga2 2.3399(11) . ? Cl2 Ga1 2.4632(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 C11 C15 104.5(3) . . ? C12 C11 C111 120.5(4) . . ? C15 C11 C111 119.3(4) . . ? C12 C11 Ga1 94.3(3) . . ? C15 C11 Ga1 97.6(3) . . ? C111 C11 Ga1 115.6(3) . . ? C13 C12 C11 109.1(4) . . ? C13 C12 C121 126.0(5) . . ? C11 C12 C121 124.8(4) . . ? C12 C13 C14 108.4(4) . . ? C12 C13 C131 127.2(5) . . ? C14 C13 C131 124.5(5) . . ? C15 C14 C13 109.6(4) . . ? C15 C14 C141 126.8(5) . . ? C13 C14 C141 123.6(5) . . ? C14 C15 C11 108.1(4) . . ? C14 C15 C151 128.0(5) . . ? C11 C15 C151 123.8(4) . . ? C25 C21 C22 103.0(3) . . ? C25 C21 C211 113.9(3) . . ? C22 C21 C211 112.9(3) . . ? C25 C21 Ga1 107.4(3) . . ? C22 C21 Ga1 109.2(2) . . ? C211 C21 Ga1 110.1(3) . . ? C23 C22 C221 127.3(4) . . ? C23 C22 C21 109.2(3) . . ? C221 C22 C21 123.2(4) . . ? C22 C23 C24 108.7(4) . . ? C22 C23 C231 127.7(4) . . ? C24 C23 C231 123.6(4) . . ? C25 C24 C23 109.6(3) . . ? C25 C24 C241 127.5(4) . . ? C23 C24 C241 122.8(4) . . ? C24 C25 C21 109.4(3) . . ? C24 C25 C251 128.2(4) . . ? C21 C25 C251 122.4(3) . . ? C32 C31 C35 105.0(4) . . ? C32 C31 C311 121.0(4) . . ? C35 C31 C311 120.9(4) . . ? C32 C31 Ga2 94.7(2) . . ? C35 C31 Ga2 94.7(2) . . ? C311 C31 Ga2 114.6(3) . . ? C33 C32 C31 108.3(4) . . ? C33 C32 C321 127.6(4) . . ? C31 C32 C321 123.9(4) . . ? C32 C33 C34 108.9(4) . . ? C32 C33 C331 125.4(5) . . ? C34 C33 C331 125.7(5) . . ? C35 C34 C33 110.3(4) . . ? C35 C34 C341 126.6(6) . . ? C33 C34 C341 123.1(6) . . ? C34 C35 C31 107.2(4) . . ? C34 C35 C351 129.5(5) . . ? C31 C35 C351 123.2(5) . . ? C42 C41 C46 114.7(4) . . ? C42 C41 Ga2 122.6(3) . . ? C46 C41 Ga2 122.7(3) . . ? F42 C42 C43 117.3(4) . . ? F42 C42 C41 119.2(4) . . ? C43 C42 C41 123.5(4) . . ? F43 C43 C44 119.9(4) . . ? F43 C43 C42 121.0(4) . . ? C44 C43 C42 119.1(4) . . ? F44 C44 C43 120.0(4) . . ? F44 C44 C45 120.2(4) . . ? C43 C44 C45 119.8(4) . . ? F45 C45 C46 121.1(4) . . ? F45 C45 C44 119.7(4) . . ? C46 C45 C44 119.2(4) . . ? F46 C46 C45 117.3(4) . . ? F46 C46 C41 118.9(3) . . ? C45 C46 C41 123.8(4) . . ? C11 C111 H11A 109.5 . . ? C11 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C11 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C13 C131 H13A 109.5 . . ? C13 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C13 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C15 C151 H15A 109.5 . . ? C15 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C15 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? C21 C211 H21A 109.5 . . ? C21 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C21 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C23 C231 H23A 109.5 . . ? C23 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C23 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C24 C241 H24A 109.5 . . ? C24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? C24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C25 C251 H25A 109.5 . . ? C25 C251 H25B 109.5 . . ? H25A C251 H25B 109.5 . . ? C25 C251 H25C 109.5 . . ? H25A C251 H25C 109.5 . . ? H25B C251 H25C 109.5 . . ? C31 C311 H31A 109.5 . . ? C31 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? C31 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? C32 C321 H32A 109.5 . . ? C32 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? C32 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? C33 C331 H33A 109.5 . . ? C33 C331 H33B 109.5 . . ? H33A C331 H33B 109.5 . . ? C33 C331 H33C 109.5 . . ? H33A C331 H33C 109.5 . . ? H33B C331 H33C 109.5 . . ? C34 C341 H34A 109.5 . . ? C34 C341 H34B 109.5 . . ? H34A C341 H34B 109.5 . . ? C34 C341 H34C 109.5 . . ? H34A C341 H34C 109.5 . . ? H34B C341 H34C 109.5 . . ? C35 C351 H35A 109.5 . . ? C35 C351 H35B 109.5 . . ? H35A C351 H35B 109.5 . . ? C35 C351 H35C 109.5 . . ? H35A C351 H35C 109.5 . . ? H35B C351 H35C 109.5 . . ? Ga2 Cl1 Ga1 93.25(4) . . ? Ga2 Cl2 Ga1 94.26(4) . . ? C21 Ga1 C11 140.55(16) . . ? C21 Ga1 Cl2 107.23(11) . . ? C11 Ga1 Cl2 101.90(13) . . ? C21 Ga1 Cl1 103.69(11) . . ? C11 Ga1 Cl1 105.90(13) . . ? Cl2 Ga1 Cl1 82.72(4) . . ? C41 Ga2 C31 122.54(15) . . ? C41 Ga2 Cl1 111.01(11) . . ? C31 Ga2 Cl1 110.12(12) . . ? C41 Ga2 Cl2 105.15(11) . . ? C31 Ga2 Cl2 113.70(12) . . ? Cl1 Ga2 Cl2 89.28(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 C11 C12 C13 -5.5(5) . . . . ? C111 C11 C12 C13 -143.2(4) . . . . ? Ga1 C11 C12 C13 93.6(3) . . . . ? C15 C11 C12 C121 175.4(4) . . . . ? C111 C11 C12 C121 37.7(6) . . . . ? Ga1 C11 C12 C121 -85.5(4) . . . . ? C11 C12 C13 C14 4.5(5) . . . . ? C121 C12 C13 C14 -176.4(4) . . . . ? C11 C12 C13 C131 -175.0(4) . . . . ? C121 C12 C13 C131 4.1(7) . . . . ? C12 C13 C14 C15 -1.6(5) . . . . ? C131 C13 C14 C15 177.9(4) . . . . ? C12 C13 C14 C141 178.8(5) . . . . ? C131 C13 C14 C141 -1.7(7) . . . . ? C13 C14 C15 C11 -1.9(5) . . . . ? C141 C14 C15 C11 177.7(5) . . . . ? C13 C14 C15 C151 174.1(5) . . . . ? C141 C14 C15 C151 -6.3(8) . . . . ? C12 C11 C15 C14 4.4(5) . . . . ? C111 C11 C15 C14 142.7(4) . . . . ? Ga1 C11 C15 C14 -92.1(3) . . . . ? C12 C11 C15 C151 -171.8(4) . . . . ? C111 C11 C15 C151 -33.5(6) . . . . ? Ga1 C11 C15 C151 91.6(5) . . . . ? C25 C21 C22 C23 -0.3(4) . . . . ? C211 C21 C22 C23 123.0(4) . . . . ? Ga1 C21 C22 C23 -114.2(3) . . . . ? C25 C21 C22 C221 -174.2(4) . . . . ? C211 C21 C22 C221 -50.9(5) . . . . ? Ga1 C21 C22 C221 71.9(5) . . . . ? C221 C22 C23 C24 174.8(5) . . . . ? C21 C22 C23 C24 1.2(5) . . . . ? C221 C22 C23 C231 -4.2(8) . . . . ? C21 C22 C23 C231 -177.8(4) . . . . ? C22 C23 C24 C25 -1.8(5) . . . . ? C231 C23 C24 C25 177.2(4) . . . . ? C22 C23 C24 C241 -179.6(4) . . . . ? C231 C23 C24 C241 -0.5(6) . . . . ? C23 C24 C25 C21 1.6(4) . . . . ? C241 C24 C25 C21 179.2(4) . . . . ? C23 C24 C25 C251 -176.5(4) . . . . ? C241 C24 C25 C251 1.1(7) . . . . ? C22 C21 C25 C24 -0.8(4) . . . . ? C211 C21 C25 C24 -123.5(4) . . . . ? Ga1 C21 C25 C24 114.4(3) . . . . ? C22 C21 C25 C251 177.4(4) . . . . ? C211 C21 C25 C251 54.7(5) . . . . ? Ga1 C21 C25 C251 -67.4(4) . . . . ? C35 C31 C32 C33 -4.6(4) . . . . ? C311 C31 C32 C33 -146.0(4) . . . . ? Ga2 C31 C32 C33 91.6(3) . . . . ? C35 C31 C32 C321 172.0(4) . . . . ? C311 C31 C32 C321 30.6(6) . . . . ? Ga2 C31 C32 C321 -91.8(4) . . . . ? C31 C32 C33 C34 2.9(5) . . . . ? C321 C32 C33 C34 -173.6(4) . . . . ? C31 C32 C33 C331 -178.1(4) . . . . ? C321 C32 C33 C331 5.4(7) . . . . ? C32 C33 C34 C35 0.2(5) . . . . ? C331 C33 C34 C35 -178.8(4) . . . . ? C32 C33 C34 C341 -179.6(4) . . . . ? C331 C33 C34 C341 1.4(7) . . . . ? C33 C34 C35 C31 -3.1(5) . . . . ? C341 C34 C35 C31 176.7(4) . . . . ? C33 C34 C35 C351 173.8(4) . . . . ? C341 C34 C35 C351 -6.3(8) . . . . ? C32 C31 C35 C34 4.7(4) . . . . ? C311 C31 C35 C34 146.1(4) . . . . ? Ga2 C31 C35 C34 -91.5(3) . . . . ? C32 C31 C35 C351 -172.5(4) . . . . ? C311 C31 C35 C351 -31.1(6) . . . . ? Ga2 C31 C35 C351 91.3(4) . . . . ? C46 C41 C42 F42 179.8(3) . . . . ? Ga2 C41 C42 F42 1.5(5) . . . . ? C46 C41 C42 C43 0.1(6) . . . . ? Ga2 C41 C42 C43 -178.2(3) . . . . ? F42 C42 C43 F43 1.1(5) . . . . ? C41 C42 C43 F43 -179.2(4) . . . . ? F42 C42 C43 C44 179.7(4) . . . . ? C41 C42 C43 C44 -0.6(6) . . . . ? F43 C43 C44 F44 -0.9(6) . . . . ? C42 C43 C44 F44 -179.6(4) . . . . ? F43 C43 C44 C45 179.0(4) . . . . ? C42 C43 C44 C45 0.4(6) . . . . ? F44 C44 C45 F45 -0.1(6) . . . . ? C43 C44 C45 F45 180.0(4) . . . . ? F44 C44 C45 C46 -179.8(4) . . . . ? C43 C44 C45 C46 0.3(6) . . . . ? F45 C45 C46 F46 -0.8(6) . . . . ? C44 C45 C46 F46 178.9(4) . . . . ? F45 C45 C46 C41 179.5(4) . . . . ? C44 C45 C46 C41 -0.8(6) . . . . ? C42 C41 C46 F46 -179.1(3) . . . . ? Ga2 C41 C46 F46 -0.8(5) . . . . ? C42 C41 C46 C45 0.6(6) . . . . ? Ga2 C41 C46 C45 178.9(3) . . . . ? C25 C21 Ga1 C11 -46.0(4) . . . . ? C22 C21 Ga1 C11 65.0(4) . . . . ? C211 C21 Ga1 C11 -170.5(3) . . . . ? C25 C21 Ga1 Cl2 178.2(2) . . . . ? C22 C21 Ga1 Cl2 -70.8(3) . . . . ? C211 C21 Ga1 Cl2 53.7(3) . . . . ? C25 C21 Ga1 Cl1 91.7(2) . . . . ? C22 C21 Ga1 Cl1 -157.3(2) . . . . ? C211 C21 Ga1 Cl1 -32.8(3) . . . . ? C12 C11 Ga1 C21 -45.4(4) . . . . ? C15 C11 Ga1 C21 59.9(4) . . . . ? C111 C11 Ga1 C21 -172.3(3) . . . . ? C12 C11 Ga1 Cl2 91.7(2) . . . . ? C15 C11 Ga1 Cl2 -163.0(2) . . . . ? C111 C11 Ga1 Cl2 -35.3(4) . . . . ? C12 C11 Ga1 Cl1 177.4(2) . . . . ? C15 C11 Ga1 Cl1 -77.3(3) . . . . ? C111 C11 Ga1 Cl1 50.5(4) . . . . ? Ga2 Cl2 Ga1 C21 -97.04(12) . . . . ? Ga2 Cl2 Ga1 C11 109.89(14) . . . . ? Ga2 Cl2 Ga1 Cl1 5.10(4) . . . . ? Ga2 Cl1 Ga1 C21 100.94(12) . . . . ? Ga2 Cl1 Ga1 C11 -105.45(13) . . . . ? Ga2 Cl1 Ga1 Cl2 -5.10(4) . . . . ? C42 C41 Ga2 C31 90.5(3) . . . . ? C46 C41 Ga2 C31 -87.7(4) . . . . ? C42 C41 Ga2 Cl1 -42.6(3) . . . . ? C46 C41 Ga2 Cl1 139.3(3) . . . . ? C42 C41 Ga2 Cl2 -137.7(3) . . . . ? C46 C41 Ga2 Cl2 44.1(3) . . . . ? C32 C31 Ga2 C41 -53.8(3) . . . . ? C35 C31 Ga2 C41 51.7(3) . . . . ? C311 C31 Ga2 C41 178.9(3) . . . . ? C32 C31 Ga2 Cl1 79.5(2) . . . . ? C35 C31 Ga2 Cl1 -174.9(2) . . . . ? C311 C31 Ga2 Cl1 -47.7(3) . . . . ? C32 C31 Ga2 Cl2 177.9(2) . . . . ? C35 C31 Ga2 Cl2 -76.5(3) . . . . ? C311 C31 Ga2 Cl2 50.7(3) . . . . ? Ga1 Cl1 Ga2 C41 -100.65(12) . . . . ? Ga1 Cl1 Ga2 C31 120.38(12) . . . . ? Ga1 Cl1 Ga2 Cl2 5.33(4) . . . . ? Ga1 Cl2 Ga2 C41 106.16(11) . . . . ? Ga1 Cl2 Ga2 C31 -117.16(13) . . . . ? Ga1 Cl2 Ga2 Cl1 -5.43(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.589 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.101 # Attachment 'MCp2GaBr.cif' data_10 _database_code_depnum_ccdc_archive 'CCDC 664845' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'bis(pentamethylcyclopentadienyl)gallium bromide' _chemical_formula_moiety 'C20 H30 Br Ga' _chemical_formula_structural 'C20 H30 Br Ga' _chemical_formula_analytical 'C20 H30 Br Ga' _chemical_formula_sum 'C20 H30 Br Ga' _chemical_formula_weight 420.07 _chemical_melting_point ? _chemical_compound_source selfmade 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.735(2) _cell_length_b 14.378(3) _cell_length_c 23.430(5) _cell_angle_alpha 80.09(3) _cell_angle_beta 85.88(3) _cell_angle_gamma 85.08(3) _cell_volume 2883.1(10) _cell_formula_units_Z 6 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 33809 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.20 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method ? _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 3.506 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33809 _diffrn_reflns_av_R_equivalents 0.1129 _diffrn_reflns_av_sigmaI/netI 0.1068 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.20 _reflns_number_total 12635 _reflns_number_observed 8717 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-Plus, XP, Siemens, 1994' _computing_publication_material 'SHELXTL-Plus, XCIF, Siemens, 1994' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1392P)^2^+411.4887P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12635 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2372 _refine_ls_R_factor_obs 0.2045 _refine_ls_wR_factor_all 0.5245 _refine_ls_wR_factor_obs 0.5061 _refine_ls_goodness_of_fit_all 1.066 _refine_ls_goodness_of_fit_obs 1.235 _refine_ls_restrained_S_all 1.066 _refine_ls_restrained_S_obs 1.235 _refine_ls_shift/esd_max 0.039 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ga3 Ga 0.3881(3) 0.6157(2) 0.01352(11) 0.0259(6) Uani 1 d . . Br3 Br 0.6687(3) 0.5470(2) 0.01390(11) 0.0319(6) Uani 1 d . . C41 C 0.3152(27) 0.6227(20) 0.0965(12) 0.036(6) Uani 1 d . . C35 C 0.1942(29) 0.7402(18) -0.0659(12) 0.034(5) Uani 1 d . . C31 C 0.3670(27) 0.7094(20) -0.0617(11) 0.034(6) Uani 1 d . . C351 C 0.0807(37) 0.6757(22) -0.0707(13) 0.046(7) Uani 1 d . . H35A H -0.0202(38) 0.7075(51) -0.0682(99) 0.068 Uiso 1 calc R . H35B H 0.0891(176) 0.6226(81) -0.0397(59) 0.068 Uiso 1 calc R . H35C H 0.0974(163) 0.6540(126) -0.1073(44) 0.068 Uiso 1 calc R . C34 C 0.1779(25) 0.8364(19) -0.0657(12) 0.032(5) Uani 1 d . . C321 C 0.6074(34) 0.8006(23) -0.0540(12) 0.045(7) Uani 1 d . . H32A H 0.6344(43) 0.8643(30) -0.0555(98) 0.067 Uiso 1 calc R . H32B H 0.6579(35) 0.7753(149) -0.0864(55) 0.067 Uiso 1 calc R . H32C H 0.6392(48) 0.7624(130) -0.0185(47) 0.067 Uiso 1 calc R . C42 C 0.1467(28) 0.6137(20) 0.0946(12) 0.034(6) Uani 1 d . . C32 C 0.4348(26) 0.8003(15) -0.0567(9) 0.023(4) Uani 1 d . . C341 C 0.0323(39) 0.8952(29) -0.0738(16) 0.062(9) Uani 1 d . . H34A H -0.0495(67) 0.8556(35) -0.0758(120) 0.093 Uiso 1 calc R . H34B H 0.0411(112) 0.9399(132) -0.1092(63) 0.093 Uiso 1 calc R . H34C H 0.0103(165) 0.9286(152) -0.0417(62) 0.093 Uiso 1 calc R . C33 C 0.3245(32) 0.8711(20) -0.0596(12) 0.038(6) Uani 1 d . . C311 C 0.4331(34) 0.6675(20) -0.1121(11) 0.038(6) Uani 1 d . . H31A H 0.4434(219) 0.7165(27) -0.1453(24) 0.056 Uiso 1 calc R . H31B H 0.3663(120) 0.6223(106) -0.1203(55) 0.056 Uiso 1 calc R . H31C H 0.5324(105) 0.6363(123) -0.1036(34) 0.056 Uiso 1 calc R . Br2 Br 0.4543(3) 0.1389(2) 0.33160(11) 0.0309(6) Uani 1 d . . Br1 Br 0.1128(3) 0.0327(2) 0.32816(12) 0.0311(6) Uani 1 d . . Ga1 Ga 0.1694(3) 0.2025(2) 0.33852(12) 0.0297(6) Uani 1 d . . Ga2 Ga 0.3968(3) -0.0311(2) 0.32164(12) 0.0302(6) Uani 1 d . . C11 C 0.1352(28) 0.2926(17) 0.2648(10) 0.028(5) Uani 1 d . . C111 C 0.2209(35) 0.2513(27) 0.2118(13) 0.056(9) Uani 1 d . . H11A H 0.1901(228) 0.2896(109) 0.1761(14) 0.083 Uiso 1 calc R . H11B H 0.1944(232) 0.1876(68) 0.2129(64) 0.083 Uiso 1 calc R . H11C H 0.3301(36) 0.2518(170) 0.2141(62) 0.083 Uiso 1 calc R . C12 C -0.0331(28) 0.3091(29) 0.2551(13) 0.053(9) Uani 1 d . . C14 C 0.0602(35) 0.4547(21) 0.2641(12) 0.043(7) Uani 1 d . . C23 C -0.0649(27) 0.3502(19) 0.4134(12) 0.034(6) Uani 1 d . . C141 C 0.0544(35) 0.5541(19) 0.2643(13) 0.043(7) Uani 1 d . . H14A H 0.1572(35) 0.5742(33) 0.2609(96) 0.064 Uiso 1 calc R . H14B H 0.0037(224) 0.5679(27) 0.2999(42) 0.064 Uiso 1 calc R . H14C H -0.0015(218) 0.5872(21) 0.2322(56) 0.064 Uiso 1 calc R . C13 C -0.0704(30) 0.4053(23) 0.2534(11) 0.038(6) Uani 1 d . . C15 C 0.1803(29) 0.3840(18) 0.2721(12) 0.035(6) Uani 1 d . . C21 C 0.1037(29) 0.2154(21) 0.4229(11) 0.036(6) Uani 1 d . . C25 C 0.1883(31) 0.2966(21) 0.4309(12) 0.038(6) Uani 1 d . . C24 C 0.0881(36) 0.3781(20) 0.4230(12) 0.041(6) Uani 1 d . . C251 C 0.3560(34) 0.2908(28) 0.4458(15) 0.056(9) Uani 1 d . . H25A H 0.3801(87) 0.3507(59) 0.4542(109) 0.084 Uiso 1 calc R . H25B H 0.4211(36) 0.2752(181) 0.4135(44) 0.084 Uiso 1 calc R . H25C H 0.3725(76) 0.2427(126) 0.4792(69) 0.084 Uiso 1 calc R . C121 C -0.1335(38) 0.2361(23) 0.2442(16) 0.053(8) Uani 1 d . . H12A H -0.2381(58) 0.2528(93) 0.2563(99) 0.080 Uiso 1 calc R . H12B H -0.1001(181) 0.1756(39) 0.2657(86) 0.080 Uiso 1 calc R . H12C H -0.1271(222) 0.2327(125) 0.2035(22) 0.080 Uiso 1 calc R . C211 C 0.1271(35) 0.1234(24) 0.4687(13) 0.048(7) Uani 1 d . . H21A H 0.0755(227) 0.1330(60) 0.5050(30) 0.072 Uiso 1 calc R . H21B H 0.2351(38) 0.1086(94) 0.4738(75) 0.072 Uiso 1 calc R . H21C H 0.0851(241) 0.0719(44) 0.4553(48) 0.072 Uiso 1 calc R . C22 C -0.0557(30) 0.2529(19) 0.4143(11) 0.034(5) Uani 1 d . . C131 C -0.2296(44) 0.4565(27) 0.2413(17) 0.064(10) Uani 1 d . . H13A H -0.3076(50) 0.4127(54) 0.2528(112) 0.096 Uiso 1 calc R . H13B H -0.2337(117) 0.4810(172) 0.2007(25) 0.096 Uiso 1 calc R . H13C H -0.2469(138) 0.5077(124) 0.2630(95) 0.096 Uiso 1 calc R . C52 C 0.4207(26) -0.1512(19) 0.2474(11) 0.031(5) Uani 1 d . . C44 C 0.1947(27) 0.7757(18) 0.0875(11) 0.030(5) Uani 1 d . . C43 C 0.0780(24) 0.7066(19) 0.0890(11) 0.030(5) Uani 1 d . . C53 C 0.5537(28) -0.2047(20) 0.2509(12) 0.034(6) Uani 1 d . . C45 C 0.3341(31) 0.7269(20) 0.0938(11) 0.036(6) Uani 1 d . . C411 C 0.3990(33) 0.5540(20) 0.1440(10) 0.037(6) Uani 1 d . . H41A H 0.3690(180) 0.5715(88) 0.1812(14) 0.055 Uiso 1 calc R . H41B H 0.5082(34) 0.5569(106) 0.1367(49) 0.055 Uiso 1 calc R . H41C H 0.3721(182) 0.4907(27) 0.1438(59) 0.055 Uiso 1 calc R . C521 C 0.2621(36) -0.1913(23) 0.2507(14) 0.048(7) Uani 1 d . . H52A H 0.2754(36) -0.2579(40) 0.2495(103) 0.072 Uiso 1 calc R . H52B H 0.2053(110) -0.1598(118) 0.2184(57) 0.072 Uiso 1 calc R . H52C H 0.2067(111) -0.1812(149) 0.2863(49) 0.072 Uiso 1 calc R . C451 C 0.4865(36) 0.7665(25) 0.0973(14) 0.050(8) Uani 1 d . . H45A H 0.4924(115) 0.8248(88) 0.0705(74) 0.075 Uiso 1 calc R . H45B H 0.5685(37) 0.7219(74) 0.0878(101) 0.075 Uiso 1 calc R . H45C H 0.4959(122) 0.7781(159) 0.1360(29) 0.075 Uiso 1 calc R . C51 C 0.4387(31) -0.0506(20) 0.2378(10) 0.035(6) Uani 1 d . . C511 C 0.3459(36) 0.0130(22) 0.1925(11) 0.043(7) Uani 1 d . . H51A H 0.3633(198) -0.0095(92) 0.1561(26) 0.065 Uiso 1 calc R . H51B H 0.3769(177) 0.0764(38) 0.1881(68) 0.065 Uiso 1 calc R . H51C H 0.2385(40) 0.0124(122) 0.2044(46) 0.065 Uiso 1 calc R . C441 C 0.1581(35) 0.8780(18) 0.0816(14) 0.042(7) Uani 1 d . . H44A H 0.2518(36) 0.9097(20) 0.0759(94) 0.064 Uiso 1 calc R . H44B H 0.1019(217) 0.8925(23) 0.1160(40) 0.064 Uiso 1 calc R . H44C H 0.0968(211) 0.8990(30) 0.0487(57) 0.064 Uiso 1 calc R . C221 C -0.1821(31) 0.1970(21) 0.4107(16) 0.047(8) Uani 1 d . . H22A H -0.2557(132) 0.2333(61) 0.3856(80) 0.071 Uiso 1 calc R . H22B H -0.2303(167) 0.1793(138) 0.4487(21) 0.071 Uiso 1 calc R . H22C H -0.1447(49) 0.1410(84) 0.3953(96) 0.071 Uiso 1 calc R . C65 C 0.6280(26) -0.1426(20) 0.3909(12) 0.036(6) Uani 1 d . . C621 C 0.2153(36) -0.2215(23) 0.4161(16) 0.052(8) Uani 1 d . . H62A H 0.1807(77) -0.2499(162) 0.3856(58) 0.078 Uiso 1 calc R . H62B H 0.1576(47) -0.1619(31) 0.4174(108) 0.078 Uiso 1 calc R . H62C H 0.2001(51) -0.2627(142) 0.4525(53) 0.078 Uiso 1 calc R . C551 C 0.6927(43) 0.0426(24) 0.2159(14) 0.055(9) Uani 1 d . . H55A H 0.7772(180) 0.0397(77) 0.2403(76) 0.082 Uiso 1 calc R . H55B H 0.6219(85) 0.0956(28) 0.2215(105) 0.082 Uiso 1 calc R . H55C H 0.7309(259) 0.0500(95) 0.1760(34) 0.082 Uiso 1 calc R . C62 C 0.3911(30) -0.2050(21) 0.4042(12) 0.038(6) Uani 1 d . . C54 C 0.6691(29) -0.1386(25) 0.2426(12) 0.045(7) Uani 1 d . . C55 C 0.6123(30) -0.0464(20) 0.2311(12) 0.036(6) Uani 1 d . . C61 C 0.4580(25) -0.1112(18) 0.3970(12) 0.032(5) Uani 1 d . . C611 C 0.4157(33) -0.0619(25) 0.4460(12) 0.048(8) Uani 1 d . . H61A H 0.4153(263) -0.1069(32) 0.4814(15) 0.072 Uiso 1 calc R . H61B H 0.3149(116) -0.0302(139) 0.4415(53) 0.072 Uiso 1 calc R . H61C H 0.4889(155) -0.0163(117) 0.4473(61) 0.072 Uiso 1 calc R . C64 C 0.6473(27) -0.2315(19) 0.3986(11) 0.034(6) Uani 1 d . . C151 C 0.3490(34) 0.4045(25) 0.2824(13) 0.048(7) Uani 1 d . . H15A H 0.3637(87) 0.4702(42) 0.2686(91) 0.072 Uiso 1 calc R . H15B H 0.4208(34) 0.3661(119) 0.2618(81) 0.072 Uiso 1 calc R . H15C H 0.3656(91) 0.3899(156) 0.3231(17) 0.072 Uiso 1 calc R . C63 C 0.4991(30) -0.2768(20) 0.4077(13) 0.040(6) Uani 1 d . . C331 C 0.3376(34) 0.9782(21) -0.0612(13) 0.044(7) Uani 1 d . . H33A H 0.4427(56) 0.9894(29) -0.0570(98) 0.066 Uiso 1 calc R . H33B H 0.2738(202) 0.9988(40) -0.0299(60) 0.066 Uiso 1 calc R . H33C H 0.3044(244) 1.0128(25) -0.0975(41) 0.066 Uiso 1 calc R . C651 C 0.7424(34) -0.0691(21) 0.3836(13) 0.043(7) Uani 1 d . . H65A H 0.8401(72) -0.0981(34) 0.3962(89) 0.065 Uiso 1 calc R . H65B H 0.7072(125) -0.0212(83) 0.4064(75) 0.065 Uiso 1 calc R . H65C H 0.7534(191) -0.0408(111) 0.3434(19) 0.065 Uiso 1 calc R . C641 C 0.7997(33) -0.2940(21) 0.4014(15) 0.047(7) Uani 1 d . . H64A H 0.8817(55) -0.2572(47) 0.4077(99) 0.070 Uiso 1 calc R . H64B H 0.8212(136) -0.3176(132) 0.3656(39) 0.070 Uiso 1 calc R . H64C H 0.7912(94) -0.3462(91) 0.4328(63) 0.070 Uiso 1 calc R . C541 C 0.8476(32) -0.1672(26) 0.2432(17) 0.056(9) Uani 1 d . . H54A H 0.9032(33) -0.1116(36) 0.2313(107) 0.084 Uiso 1 calc R . H54B H 0.8751(59) -0.2112(141) 0.2170(84) 0.084 Uiso 1 calc R . H54C H 0.8732(56) -0.1961(164) 0.2817(29) 0.084 Uiso 1 calc R . C631 C 0.4768(47) -0.3802(22) 0.4214(18) 0.065(10) Uani 1 d . . H63A H 0.3857(185) -0.3902(27) 0.4465(101) 0.097 Uiso 1 calc R . H63B H 0.5643(154) -0.4129(33) 0.4405(111) 0.097 Uiso 1 calc R . H63C H 0.4660(329) -0.4039(47) 0.3862(22) 0.097 Uiso 1 calc R . C421 C 0.0716(38) 0.5242(22) 0.1046(15) 0.050(8) Uani 1 d . . H42A H -0.0354(69) 0.5360(33) 0.1156(102) 0.075 Uiso 1 calc R . H42B H 0.1200(182) 0.4809(63) 0.1351(72) 0.075 Uiso 1 calc R . H42C H 0.0811(245) 0.4972(89) 0.0697(33) 0.075 Uiso 1 calc R . C531 C 0.5803(44) -0.3109(23) 0.2622(16) 0.057(9) Uani 1 d . . H53A H 0.4908(120) -0.3379(24) 0.2824(99) 0.085 Uiso 1 calc R . H53B H 0.6675(185) -0.3290(24) 0.2855(96) 0.085 Uiso 1 calc R . H53C H 0.5996(298) -0.3336(27) 0.2260(17) 0.085 Uiso 1 calc R . C231 C -0.2134(34) 0.4167(31) 0.4072(15) 0.064(11) Uani 1 d . . H23A H -0.2904(108) 0.3864(82) 0.3914(113) 0.096 Uiso 1 calc R . H23B H -0.1918(78) 0.4744(83) 0.3817(96) 0.096 Uiso 1 calc R . H23C H -0.2502(180) 0.4307(162) 0.4446(23) 0.096 Uiso 1 calc R . C241 C 0.1194(41) 0.4765(23) 0.4249(17) 0.057(9) Uani 1 d . . H24A H 0.2267(70) 0.4845(53) 0.4153(112) 0.086 Uiso 1 calc R . H24B H 0.0929(286) 0.4903(62) 0.4632(34) 0.086 Uiso 1 calc R . H24C H 0.0589(228) 0.5187(25) 0.3974(82) 0.086 Uiso 1 calc R . C431 C -0.0912(36) 0.7297(35) 0.0807(21) 0.081(14) Uani 1 d . . H43A H -0.1443(66) 0.6728(51) 0.0903(140) 0.121 Uiso 1 calc R . H43B H -0.1057(45) 0.7572(219) 0.0409(40) 0.121 Uiso 1 calc R . H43C H -0.1315(91) 0.7738(187) 0.1054(110) 0.121 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 Ga3 0.0266(13) 0.0282(13) 0.0222(12) -0.0026(10) -0.0028(9) -0.0008(10) Br3 0.0255(12) 0.0343(13) 0.0371(13) -0.0078(10) -0.0074(9) -0.0009(10) C41 0.016(11) 0.046(16) 0.043(14) -0.008(12) 0.006(10) 0.015(10) C35 0.028(13) 0.030(13) 0.041(14) 0.002(10) 0.005(10) -0.005(10) C31 0.019(11) 0.054(16) 0.030(12) -0.005(11) -0.004(9) -0.014(11) C351 0.051(18) 0.050(17) 0.037(15) -0.007(13) -0.020(13) 0.003(14) C34 0.010(10) 0.038(14) 0.049(15) -0.009(11) -0.009(9) 0.008(9) C321 0.045(17) 0.059(19) 0.034(14) -0.013(13) -0.001(12) -0.017(14) C42 0.020(11) 0.045(15) 0.040(14) -0.012(11) 0.009(10) -0.012(11) C32 0.029(11) 0.015(10) 0.025(11) 0.004(8) -0.012(9) -0.008(8) C341 0.044(19) 0.085(27) 0.058(21) -0.026(19) 0.008(15) 0.006(18) C33 0.035(14) 0.039(15) 0.036(14) 0.014(11) -0.003(11) -0.014(12) C311 0.044(16) 0.039(15) 0.031(13) -0.009(11) 0.007(11) -0.007(12) Br2 0.0163(10) 0.0300(12) 0.0469(14) -0.0080(10) -0.0048(9) 0.0010(9) Br1 0.0163(10) 0.0290(12) 0.0481(14) -0.0077(10) 0.0007(9) -0.0006(9) Ga1 0.0194(12) 0.0306(14) 0.0391(15) -0.0066(11) -0.0012(10) -0.0007(10) Ga2 0.0211(13) 0.0290(14) 0.0394(15) -0.0039(11) -0.0020(11) 0.0016(10) C11 0.026(12) 0.030(12) 0.029(12) -0.006(9) -0.008(9) -0.003(9) C111 0.033(15) 0.083(25) 0.043(17) 0.013(16) -0.012(13) 0.004(15) C12 0.009(11) 0.108(29) 0.037(15) 0.003(16) 0.000(10) -0.009(14) C14 0.045(16) 0.046(16) 0.032(14) -0.005(12) 0.022(12) 0.008(13) C23 0.018(11) 0.038(14) 0.050(15) -0.017(12) 0.004(10) -0.014(10) C141 0.042(16) 0.033(14) 0.053(17) -0.013(12) -0.007(13) 0.018(12) C13 0.027(13) 0.063(19) 0.026(12) -0.009(12) 0.000(10) -0.006(12) C15 0.028(13) 0.029(13) 0.047(15) 0.002(11) 0.010(11) -0.016(10) C21 0.026(12) 0.054(17) 0.032(13) -0.022(12) -0.006(10) 0.011(11) C25 0.028(13) 0.049(16) 0.044(15) -0.025(13) -0.003(11) -0.002(12) C24 0.052(17) 0.035(15) 0.036(14) -0.011(11) 0.011(12) -0.006(12) C251 0.030(15) 0.086(26) 0.058(20) -0.028(18) -0.015(14) 0.000(15) C121 0.046(18) 0.044(17) 0.072(22) 0.000(15) -0.021(16) -0.018(14) C211 0.038(16) 0.065(21) 0.041(16) -0.012(14) -0.004(12) -0.001(14) C22 0.033(13) 0.033(13) 0.035(13) -0.005(10) 0.000(10) 0.003(10) C131 0.064(23) 0.058(22) 0.070(24) -0.020(18) 0.000(18) 0.015(18) C52 0.014(10) 0.044(15) 0.037(13) -0.009(11) -0.001(9) -0.001(10) C44 0.023(11) 0.039(14) 0.033(12) -0.010(10) -0.017(9) -0.002(10) C43 0.008(9) 0.042(14) 0.046(14) -0.020(11) -0.004(9) 0.002(9) C53 0.020(11) 0.045(15) 0.040(14) -0.021(12) 0.002(10) 0.001(10) C45 0.034(14) 0.047(16) 0.026(12) -0.013(11) -0.003(10) 0.011(12) C411 0.046(16) 0.040(15) 0.022(12) -0.006(10) -0.005(11) 0.007(12) C521 0.048(18) 0.051(18) 0.049(17) -0.010(14) -0.017(14) -0.013(14) C451 0.048(18) 0.064(21) 0.046(17) -0.034(15) -0.002(13) -0.004(15) C51 0.035(14) 0.050(16) 0.023(12) -0.018(11) 0.003(10) -0.013(12) C511 0.050(17) 0.051(17) 0.027(13) -0.008(12) -0.001(12) 0.003(14) C441 0.045(16) 0.025(13) 0.058(18) -0.017(12) -0.014(13) 0.017(12) C221 0.025(13) 0.036(15) 0.083(22) -0.025(15) 0.008(14) 0.008(11) C65 0.012(10) 0.045(16) 0.045(15) 0.009(12) -0.008(10) -0.008(10) C621 0.043(17) 0.043(17) 0.075(22) -0.020(16) -0.013(15) -0.008(14) C551 0.068(22) 0.051(19) 0.050(18) -0.012(15) 0.006(16) -0.030(17) C62 0.024(12) 0.050(16) 0.037(14) 0.003(12) -0.006(10) -0.008(11) C54 0.017(12) 0.081(23) 0.043(15) -0.018(15) -0.006(10) -0.022(13) C55 0.027(13) 0.042(15) 0.042(15) -0.016(12) 0.009(11) -0.002(11) C61 0.010(10) 0.032(13) 0.050(15) -0.003(11) 0.001(9) 0.006(9) C611 0.030(14) 0.078(23) 0.034(14) -0.004(14) -0.009(11) 0.006(14) C64 0.017(11) 0.040(15) 0.041(14) -0.005(11) -0.004(10) 0.008(10) C151 0.037(16) 0.066(21) 0.041(16) -0.006(14) -0.001(12) -0.015(14) C63 0.023(12) 0.039(15) 0.059(18) -0.005(13) 0.003(12) -0.015(11) C331 0.040(15) 0.049(17) 0.050(16) -0.022(13) 0.012(12) -0.024(13) C651 0.041(16) 0.048(17) 0.045(16) -0.013(13) 0.000(12) -0.024(13) C641 0.033(15) 0.040(16) 0.064(20) -0.004(14) -0.012(13) 0.013(12) C541 0.022(14) 0.066(22) 0.084(25) -0.031(19) 0.005(14) -0.001(14) C631 0.077(26) 0.027(15) 0.089(27) -0.014(16) 0.003(21) 0.003(16) C421 0.052(19) 0.045(17) 0.060(19) -0.026(15) 0.015(15) -0.023(15) C531 0.067(23) 0.047(18) 0.064(21) -0.027(16) -0.027(17) 0.009(16) C231 0.025(15) 0.113(32) 0.058(20) -0.035(20) -0.016(14) 0.022(17) C241 0.055(20) 0.047(19) 0.077(24) -0.021(17) 0.003(17) -0.023(16) C431 0.023(16) 0.120(37) 0.116(35) -0.065(30) -0.008(18) -0.005(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga3 C41 2.02(3) . ? Ga3 C31 2.03(3) . ? Ga3 Br3 2.562(4) . ? Ga3 Br3 2.625(4) 2_665 ? Br3 Ga3 2.625(4) 2_665 ? C41 C42 1.49(3) . ? C41 C45 1.51(4) . ? C41 C411 1.54(4) . ? C35 C34 1.38(4) . ? C35 C351 1.44(4) . ? C35 C31 1.54(4) . ? C31 C311 1.48(4) . ? C31 C32 1.51(3) . ? C34 C33 1.44(3) . ? C34 C341 1.47(4) . ? C321 C32 1.51(4) . ? C42 C43 1.40(4) . ? C42 C421 1.47(4) . ? C32 C33 1.34(4) . ? C33 C331 1.55(4) . ? Br2 Ga1 2.580(4) . ? Br2 Ga2 2.590(4) . ? Br1 Ga2 2.573(4) . ? Br1 Ga1 2.588(4) . ? Ga1 C11 2.00(2) . ? Ga1 C21 2.05(2) . ? Ga2 C61 2.02(3) . ? Ga2 C51 2.04(2) . ? C11 C15 1.45(3) . ? C11 C12 1.50(3) . ? C11 C111 1.58(4) . ? C12 C13 1.39(5) . ? C12 C121 1.49(4) . ? C14 C15 1.40(4) . ? C14 C141 1.43(4) . ? C14 C13 1.45(4) . ? C23 C22 1.39(4) . ? C23 C24 1.47(4) . ? C23 C231 1.54(4) . ? C13 C131 1.54(4) . ? C15 C151 1.57(4) . ? C21 C22 1.46(4) . ? C21 C25 1.48(4) . ? C21 C211 1.56(4) . ? C25 C24 1.39(4) . ? C25 C251 1.52(4) . ? C24 C241 1.47(4) . ? C22 C221 1.44(4) . ? C52 C53 1.34(3) . ? C52 C51 1.45(4) . ? C52 C521 1.54(4) . ? C44 C45 1.36(3) . ? C44 C441 1.46(3) . ? C44 C43 1.48(3) . ? C43 C431 1.51(4) . ? C53 C54 1.42(4) . ? C53 C531 1.50(4) . ? C45 C451 1.51(4) . ? C51 C511 1.51(4) . ? C51 C55 1.52(4) . ? C65 C64 1.26(4) . ? C65 C651 1.50(3) . ? C65 C61 1.52(3) . ? C621 C62 1.57(4) . ? C551 C55 1.49(4) . ? C62 C63 1.33(4) . ? C62 C61 1.49(4) . ? C54 C55 1.36(4) . ? C54 C541 1.58(4) . ? C61 C611 1.46(4) . ? C64 C63 1.49(3) . ? C64 C641 1.54(3) . ? C63 C631 1.49(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C41 Ga3 C31 132.5(11) . . ? C41 Ga3 Br3 107.5(7) . . ? C31 Ga3 Br3 106.8(7) . . ? C41 Ga3 Br3 110.8(9) . 2_665 ? C31 Ga3 Br3 104.2(8) . 2_665 ? Br3 Ga3 Br3 84.60(11) . 2_665 ? Ga3 Br3 Ga3 95.41(11) . 2_665 ? C42 C41 C45 106.2(21) . . ? C42 C41 C411 116.4(24) . . ? C45 C41 C411 116.7(24) . . ? C42 C41 Ga3 101.2(18) . . ? C45 C41 Ga3 96.9(17) . . ? C411 C41 Ga3 116.8(16) . . ? C34 C35 C351 130.0(25) . . ? C34 C35 C31 107.0(21) . . ? C351 C35 C31 122.9(24) . . ? C311 C31 C32 113.1(21) . . ? C311 C31 C35 112.7(22) . . ? C32 C31 C35 102.5(22) . . ? C311 C31 Ga3 111.3(20) . . ? C32 C31 Ga3 110.0(15) . . ? C35 C31 Ga3 106.7(16) . . ? C35 C34 C33 110.3(22) . . ? C35 C34 C341 124.5(26) . . ? C33 C34 C341 125.2(27) . . ? C43 C42 C421 128.5(24) . . ? C43 C42 C41 105.6(21) . . ? C421 C42 C41 125.5(27) . . ? C33 C32 C31 110.1(21) . . ? C33 C32 C321 130.7(22) . . ? C31 C32 C321 119.0(22) . . ? C32 C33 C34 110.1(23) . . ? C32 C33 C331 129.7(24) . . ? C34 C33 C331 120.1(25) . . ? Ga1 Br2 Ga2 95.24(12) . . ? Ga2 Br1 Ga1 95.47(12) . . ? C11 Ga1 C21 130.4(11) . . ? C11 Ga1 Br2 106.0(7) . . ? C21 Ga1 Br2 109.7(7) . . ? C11 Ga1 Br1 110.9(7) . . ? C21 Ga1 Br1 105.7(9) . . ? Br2 Ga1 Br1 84.60(11) . . ? C61 Ga2 C51 131.6(11) . . ? C61 Ga2 Br1 111.3(6) . . ? C51 Ga2 Br1 104.8(8) . . ? C61 Ga2 Br2 104.5(8) . . ? C51 Ga2 Br2 109.9(8) . . ? Br1 Ga2 Br2 84.69(11) . . ? C15 C11 C12 104.3(25) . . ? C15 C11 C111 114.8(23) . . ? C12 C11 C111 109.2(22) . . ? C15 C11 Ga1 108.0(17) . . ? C12 C11 Ga1 110.3(18) . . ? C111 C11 Ga1 110.1(17) . . ? C13 C12 C121 128.1(26) . . ? C13 C12 C11 106.5(26) . . ? C121 C12 C11 125.2(33) . . ? C15 C14 C141 131.8(30) . . ? C15 C14 C13 104.3(25) . . ? C141 C14 C13 123.9(28) . . ? C22 C23 C24 108.7(24) . . ? C22 C23 C231 125.5(25) . . ? C24 C23 C231 125.7(26) . . ? C12 C13 C14 112.2(25) . . ? C12 C13 C131 125.4(27) . . ? C14 C13 C131 122.5(29) . . ? C14 C15 C11 112.6(24) . . ? C14 C15 C151 123.0(26) . . ? C11 C15 C151 124.1(25) . . ? C22 C21 C25 105.9(23) . . ? C22 C21 C211 116.2(24) . . ? C25 C21 C211 116.3(23) . . ? C22 C21 Ga1 98.5(16) . . ? C25 C21 Ga1 101.7(19) . . ? C211 C21 Ga1 115.8(18) . . ? C24 C25 C21 108.4(23) . . ? C24 C25 C251 126.4(28) . . ? C21 C25 C251 125.2(27) . . ? C25 C24 C241 128.9(29) . . ? C25 C24 C23 108.1(24) . . ? C241 C24 C23 123.0(28) . . ? C23 C22 C221 126.1(24) . . ? C23 C22 C21 108.7(24) . . ? C221 C22 C21 125.1(25) . . ? C53 C52 C51 113.9(23) . . ? C53 C52 C521 123.9(26) . . ? C51 C52 C521 122.2(23) . . ? C45 C44 C441 128.3(25) . . ? C45 C44 C43 108.0(23) . . ? C441 C44 C43 123.7(22) . . ? C42 C43 C44 111.0(20) . . ? C42 C43 C431 122.6(26) . . ? C44 C43 C431 126.1(27) . . ? C52 C53 C54 104.6(25) . . ? C52 C53 C531 129.0(27) . . ? C54 C53 C531 126.4(27) . . ? C44 C45 C451 127.3(27) . . ? C44 C45 C41 109.1(24) . . ? C451 C45 C41 123.5(23) . . ? C52 C51 C511 118.6(22) . . ? C52 C51 C55 102.7(23) . . ? C511 C51 C55 116.8(23) . . ? C52 C51 Ga2 97.2(17) . . ? C511 C51 Ga2 117.3(19) . . ? C55 C51 Ga2 100.9(16) . . ? C64 C65 C651 130.6(25) . . ? C64 C65 C61 110.4(22) . . ? C651 C65 C61 118.6(25) . . ? C63 C62 C61 112.4(22) . . ? C63 C62 C621 121.8(25) . . ? C61 C62 C621 125.2(25) . . ? C55 C54 C53 113.9(24) . . ? C55 C54 C541 121.8(26) . . ? C53 C54 C541 124.2(30) . . ? C54 C55 C551 130.9(27) . . ? C54 C55 C51 104.6(23) . . ? C551 C55 C51 124.5(27) . . ? C611 C61 C62 112.6(24) . . ? C611 C61 C65 114.2(23) . . ? C62 C61 C65 99.9(20) . . ? C611 C61 Ga2 111.2(18) . . ? C62 C61 Ga2 109.8(18) . . ? C65 C61 Ga2 108.4(17) . . ? C65 C64 C63 112.2(22) . . ? C65 C64 C641 128.4(25) . . ? C63 C64 C641 119.4(24) . . ? C62 C63 C64 104.9(23) . . ? C62 C63 C631 127.8(26) . . ? C64 C63 C631 127.3(27) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.20 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 4.769 _refine_diff_density_min -4.241 _refine_diff_density_rms 0.372 # Attachment 'MCp2GaC6F5.cif' data_11 _database_code_depnum_ccdc_archive 'CCDC 664846' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H30 F5 Ga' _chemical_formula_weight 507.22 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7661(2) _cell_length_b 16.3514(4) _cell_length_c 15.2095(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.3840(10) _cell_angle_gamma 90.00 _cell_volume 2418.08(10) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 33064 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method ? _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7972 _exptl_absorpt_correction_T_max 0.8905 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33064 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5518 _reflns_number_gt 4219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus, XP, Siemens, 1994' _computing_publication_material 'SHELXTL-Plus, XCIF, Siemens, 1994' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+2.2683P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5518 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0858 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.000 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 Ga Ga 0.74741(2) 0.292378(15) 0.560730(16) 0.02678(8) Uani 1 1 d . . . F2 F 1.01568(13) 0.18678(9) 0.56774(10) 0.0422(4) Uani 1 1 d . A . F3 F 1.09108(19) 0.06526(10) 0.46351(13) 0.0694(6) Uani 1 1 d . . . F4 F 0.9129(3) 0.00956(11) 0.32830(13) 0.0889(7) Uani 1 1 d . A . F5 F 0.6604(2) 0.07872(12) 0.29675(11) 0.0797(6) Uani 1 1 d . . . F6 F 0.58776(15) 0.20405(10) 0.39702(10) 0.0506(4) Uani 1 1 d . A . C11 C 0.5767(4) 0.2726(3) 0.6408(3) 0.0273(7) Uiso 0.677(4) 1 d P A 1 C12 C 0.7092(7) 0.2641(3) 0.6966(4) 0.0270(12) Uani 0.677(4) 1 d P A 1 C13 C 0.7420(6) 0.1793(4) 0.6954(4) 0.0311(12) Uani 0.677(4) 1 d P A 1 C14 C 0.6347(9) 0.1340(5) 0.6419(6) 0.0392(18) Uani 0.677(4) 1 d P A 1 C15 C 0.5296(11) 0.1926(4) 0.6091(7) 0.0279(13) Uani 0.677(4) 1 d P A 1 C111 C 0.4801(5) 0.3456(3) 0.6487(4) 0.0444(12) Uani 0.677(4) 1 d P A 1 H11A H 0.4215 0.3355 0.6965 0.067 Uiso 0.677(4) 1 calc PR A 1 H11B H 0.4223 0.3527 0.5930 0.067 Uiso 0.677(4) 1 calc PR A 1 H11C H 0.5346 0.3952 0.6617 0.067 Uiso 0.677(4) 1 calc PR A 1 C121 C 0.7708(5) 0.3256(3) 0.7639(3) 0.0485(12) Uani 0.677(4) 1 d P A 1 H12A H 0.7374 0.3144 0.8215 0.073 Uiso 0.677(4) 1 calc PR A 1 H12B H 0.7435 0.3810 0.7449 0.073 Uiso 0.677(4) 1 calc PR A 1 H12C H 0.8713 0.3212 0.7688 0.073 Uiso 0.677(4) 1 calc PR A 1 C131 C 0.8677(5) 0.1421(4) 0.7433(3) 0.0622(16) Uani 0.677(4) 1 d P A 1 H13A H 0.9384 0.1843 0.7548 0.093 Uiso 0.677(4) 1 calc PR A 1 H13B H 0.9026 0.0987 0.7070 0.093 Uiso 0.677(4) 1 calc PR A 1 H13C H 0.8443 0.1190 0.7994 0.093 Uiso 0.677(4) 1 calc PR A 1 C141 C 0.6372(6) 0.0480(3) 0.6222(4) 0.0618(15) Uani 0.677(4) 1 d P A 1 H14A H 0.5478 0.0237 0.6311 0.093 Uiso 0.677(4) 1 calc PR A 1 H14B H 0.7091 0.0213 0.6615 0.093 Uiso 0.677(4) 1 calc PR A 1 H14C H 0.6566 0.0403 0.5607 0.093 Uiso 0.677(4) 1 calc PR A 1 C151 C 0.4036(7) 0.1758(4) 0.5546(4) 0.0585(18) Uani 0.677(4) 1 d P A 1 H15A H 0.4126 0.1239 0.5233 0.088 Uiso 0.677(4) 1 calc PR A 1 H15B H 0.3855 0.2200 0.5116 0.088 Uiso 0.677(4) 1 calc PR A 1 H15C H 0.3273 0.1719 0.5919 0.088 Uiso 0.677(4) 1 calc PR A 1 C41 C 0.6030(10) 0.2778(6) 0.6531(6) 0.0273(7) Uiso 0.323(4) 1 d P A 2 C42 C 0.7247(17) 0.2346(9) 0.6959(11) 0.0270(12) Uani 0.323(4) 1 d P A 2 C43 C 0.7169(16) 0.1546(10) 0.6740(8) 0.0311(12) Uani 0.323(4) 1 d P A 2 C44 C 0.602(3) 0.1481(14) 0.6266(16) 0.0392(18) Uani 0.323(4) 1 d P A 2 C45 C 0.541(3) 0.2150(11) 0.6107(18) 0.0279(13) Uani 0.323(4) 1 d P A 2 C411 C 0.5333(11) 0.3504(8) 0.6802(8) 0.0444(12) Uani 0.323(4) 1 d P A 2 H41A H 0.4687 0.3354 0.7230 0.067 Uiso 0.323(4) 1 calc PR A 2 H41B H 0.4829 0.3758 0.6285 0.067 Uiso 0.323(4) 1 calc PR A 2 H41C H 0.6011 0.3892 0.7074 0.067 Uiso 0.323(4) 1 calc PR A 2 C421 C 0.8235(11) 0.2788(7) 0.7626(6) 0.0485(12) Uani 0.323(4) 1 d P A 2 H42A H 0.7965 0.2693 0.8222 0.073 Uiso 0.323(4) 1 calc PR A 2 H42B H 0.8209 0.3376 0.7500 0.073 Uiso 0.323(4) 1 calc PR A 2 H42C H 0.9170 0.2582 0.7588 0.073 Uiso 0.323(4) 1 calc PR A 2 C431 C 0.8290(11) 0.0927(8) 0.7060(7) 0.0622(16) Uani 0.323(4) 1 d P A 2 H43A H 0.9165 0.1214 0.7195 0.093 Uiso 0.323(4) 1 calc PR A 2 H43B H 0.8387 0.0520 0.6597 0.093 Uiso 0.323(4) 1 calc PR A 2 H43C H 0.8031 0.0652 0.7593 0.093 Uiso 0.323(4) 1 calc PR A 2 C441 C 0.5617(14) 0.0533(7) 0.5832(9) 0.0618(15) Uani 0.323(4) 1 d P A 2 H44A H 0.5749 0.0121 0.6300 0.093 Uiso 0.323(4) 1 calc PR A 2 H44B H 0.6218 0.0409 0.5369 0.093 Uiso 0.323(4) 1 calc PR A 2 H44C H 0.4656 0.0528 0.5580 0.093 Uiso 0.323(4) 1 calc PR A 2 C451 C 0.3908(16) 0.2187(8) 0.5538(11) 0.0585(18) Uani 0.323(4) 1 d P A 2 H45A H 0.3810 0.1718 0.5135 0.088 Uiso 0.323(4) 1 calc PR A 2 H45B H 0.3830 0.2695 0.5197 0.088 Uiso 0.323(4) 1 calc PR A 2 H45C H 0.3183 0.2168 0.5941 0.088 Uiso 0.323(4) 1 calc PR A 2 C21 C 0.8158(2) 0.40559(14) 0.52861(15) 0.0327(5) Uani 1 1 d . A . C22 C 0.9570(2) 0.37879(15) 0.51726(16) 0.0348(5) Uani 1 1 d . . . C23 C 0.9607(2) 0.35420(14) 0.43134(16) 0.0336(5) Uani 1 1 d . A . C24 C 0.8292(3) 0.36787(14) 0.38361(15) 0.0351(5) Uani 1 1 d . . . C25 C 0.7419(3) 0.40050(14) 0.44006(16) 0.0357(5) Uani 1 1 d . A . C211 C 0.7897(3) 0.47581(16) 0.59050(19) 0.0487(7) Uani 1 1 d . . . H21A H 0.8419 0.4667 0.6479 0.073 Uiso 1 1 calc R A . H21B H 0.6914 0.4786 0.5983 0.073 Uiso 1 1 calc R . . H21C H 0.8191 0.5273 0.5652 0.073 Uiso 1 1 calc R . . C221 C 1.0724(3) 0.38186(19) 0.58929(19) 0.0508(7) Uani 1 1 d . A . H22A H 1.0408 0.3601 0.6439 0.076 Uiso 1 1 calc R . . H22B H 1.1025 0.4386 0.5987 0.076 Uiso 1 1 calc R . . H22C H 1.1495 0.3488 0.5724 0.076 Uiso 1 1 calc R . . C231 C 1.0778(3) 0.31432(16) 0.39029(19) 0.0455(7) Uani 1 1 d . . . H23A H 1.1016 0.3471 0.3399 0.068 Uiso 1 1 calc R A . H23B H 1.0504 0.2593 0.3700 0.068 Uiso 1 1 calc R . . H23C H 1.1577 0.3106 0.4341 0.068 Uiso 1 1 calc R . . C241 C 0.7951(3) 0.34682(18) 0.28812(17) 0.0518(7) Uani 1 1 d . A . H24A H 0.7964 0.2873 0.2809 0.078 Uiso 1 1 calc R . . H24B H 0.8632 0.3716 0.2529 0.078 Uiso 1 1 calc R . . H24C H 0.7034 0.3678 0.2682 0.078 Uiso 1 1 calc R . . C251 C 0.5973(3) 0.4302(2) 0.4180(2) 0.0585(8) Uani 1 1 d . . . H25A H 0.5872 0.4847 0.4435 0.088 Uiso 1 1 calc R A . H25B H 0.5330 0.3923 0.4424 0.088 Uiso 1 1 calc R . . H25C H 0.5774 0.4331 0.3537 0.088 Uiso 1 1 calc R . . C31 C 0.7980(2) 0.19909(13) 0.48675(14) 0.0270(5) Uani 1 1 d . A . C32 C 0.9248(2) 0.16143(14) 0.50073(15) 0.0325(5) Uani 1 1 d . . . C33 C 0.9650(3) 0.09888(15) 0.44830(19) 0.0453(7) Uani 1 1 d . A . C34 C 0.8755(4) 0.07116(16) 0.37984(19) 0.0538(8) Uani 1 1 d . . . C35 C 0.7484(3) 0.10622(17) 0.36377(17) 0.0496(7) Uani 1 1 d . A . C36 C 0.7126(3) 0.16940(15) 0.41702(15) 0.0362(5) 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 Ga 0.02647(13) 0.02739(14) 0.02753(13) -0.00059(11) 0.00802(9) 0.00248(10) F2 0.0289(7) 0.0521(9) 0.0456(9) 0.0081(7) 0.0028(6) 0.0094(6) F3 0.0726(12) 0.0504(10) 0.0916(14) 0.0178(9) 0.0420(10) 0.0366(9) F4 0.161(2) 0.0413(10) 0.0722(13) -0.0190(9) 0.0538(14) 0.0135(12) F5 0.1285(18) 0.0728(13) 0.0359(10) -0.0201(9) -0.0022(10) -0.0281(12) F6 0.0425(9) 0.0689(11) 0.0377(8) 0.0010(8) -0.0106(7) -0.0017(8) C12 0.029(2) 0.034(3) 0.0186(12) 0.001(3) 0.0069(13) -0.005(3) C13 0.027(3) 0.046(5) 0.021(3) 0.008(2) 0.005(2) 0.005(2) C14 0.051(6) 0.021(4) 0.051(4) 0.018(2) 0.032(4) 0.016(2) C15 0.024(2) 0.027(5) 0.0339(14) -0.008(3) 0.0078(14) -0.018(3) C111 0.036(3) 0.048(2) 0.053(4) 0.007(3) 0.022(2) 0.010(3) C121 0.056(3) 0.062(3) 0.0278(16) -0.002(2) 0.0039(19) -0.027(2) C131 0.047(3) 0.090(4) 0.052(3) 0.036(3) 0.018(2) 0.029(3) C141 0.086(5) 0.038(2) 0.067(4) 0.004(3) 0.038(3) -0.003(3) C151 0.037(2) 0.090(5) 0.049(2) -0.017(4) 0.0058(16) -0.026(4) C42 0.029(2) 0.034(3) 0.0186(12) 0.001(3) 0.0069(13) -0.005(3) C43 0.027(3) 0.046(5) 0.021(3) 0.008(2) 0.005(2) 0.005(2) C44 0.051(6) 0.021(4) 0.051(4) 0.018(2) 0.032(4) 0.016(2) C45 0.024(2) 0.027(5) 0.0339(14) -0.008(3) 0.0078(14) -0.018(3) C411 0.036(3) 0.048(2) 0.053(4) 0.007(3) 0.022(2) 0.010(3) C421 0.056(3) 0.062(3) 0.0278(16) -0.002(2) 0.0039(19) -0.027(2) C431 0.047(3) 0.090(4) 0.052(3) 0.036(3) 0.018(2) 0.029(3) C441 0.086(5) 0.038(2) 0.067(4) 0.004(3) 0.038(3) -0.003(3) C451 0.037(2) 0.090(5) 0.049(2) -0.017(4) 0.0058(16) -0.026(4) C21 0.0406(13) 0.0281(12) 0.0318(12) -0.0017(10) 0.0165(10) -0.0005(10) C22 0.0373(13) 0.0320(13) 0.0370(13) -0.0011(10) 0.0141(11) -0.0077(10) C23 0.0408(14) 0.0267(12) 0.0365(13) 0.0009(10) 0.0203(11) -0.0025(10) C24 0.0516(15) 0.0287(12) 0.0267(12) 0.0051(10) 0.0122(11) 0.0050(11) C25 0.0480(14) 0.0276(12) 0.0331(12) 0.0054(10) 0.0114(11) 0.0098(11) C211 0.0685(19) 0.0329(14) 0.0492(16) -0.0104(12) 0.0290(14) -0.0085(13) C221 0.0435(15) 0.0629(19) 0.0467(16) -0.0089(14) 0.0079(13) -0.0160(14) C231 0.0478(16) 0.0405(15) 0.0525(17) -0.0047(12) 0.0279(13) -0.0024(12) C241 0.076(2) 0.0511(17) 0.0294(14) 0.0042(12) 0.0132(13) 0.0117(15) C251 0.064(2) 0.063(2) 0.0491(17) 0.0070(15) 0.0068(15) 0.0345(16) C31 0.0315(11) 0.0262(11) 0.0243(11) 0.0039(9) 0.0071(9) 0.0023(9) C32 0.0379(13) 0.0293(12) 0.0315(12) 0.0068(10) 0.0093(10) 0.0046(10) C33 0.0560(17) 0.0308(13) 0.0536(17) 0.0115(12) 0.0286(14) 0.0183(12) C34 0.096(2) 0.0271(14) 0.0431(16) -0.0051(12) 0.0316(17) 0.0040(15) C35 0.083(2) 0.0391(15) 0.0276(13) -0.0046(11) 0.0070(13) -0.0122(15) C36 0.0469(15) 0.0354(13) 0.0263(12) 0.0029(10) 0.0032(10) -0.0010(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga C31 1.985(2) . ? Ga C21 2.043(2) . ? Ga C41 2.095(10) . ? Ga C11 2.179(5) . ? Ga C12 2.184(6) . ? Ga C42 2.293(16) . ? F2 C32 1.352(3) . ? F3 C33 1.348(3) . ? F4 C34 1.348(3) . ? F5 C35 1.347(3) . ? F6 C36 1.353(3) . ? C11 C15 1.454(7) . ? C11 C12 1.486(8) . ? C11 C111 1.534(7) . ? C12 C13 1.424(7) . ? C12 C121 1.518(7) . ? C13 C14 1.466(13) . ? C13 C131 1.496(7) . ? C14 C141 1.439(11) . ? C14 C15 1.457(12) . ? C15 C151 1.444(12) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C151 H15A 0.9800 . ? C151 H15B 0.9800 . ? C151 H15C 0.9800 . ? C41 C45 1.33(2) . ? C41 C411 1.448(16) . ? C41 C42 1.480(18) . ? C42 C43 1.350(18) . ? C42 C421 1.517(19) . ? C43 C44 1.28(3) . ? C43 C431 1.536(19) . ? C44 C45 1.26(3) . ? C44 C441 1.71(3) . ? C45 C451 1.63(3) . ? C411 H41A 0.9800 . ? C411 H41B 0.9800 . ? C411 H41C 0.9800 . ? C421 H42A 0.9800 . ? C421 H42B 0.9800 . ? C421 H42C 0.9800 . ? C431 H43A 0.9800 . ? C431 H43B 0.9800 . ? C431 H43C 0.9800 . ? C441 H44A 0.9800 . ? C441 H44B 0.9800 . ? C441 H44C 0.9800 . ? C451 H45A 0.9800 . ? C451 H45B 0.9800 . ? C451 H45C 0.9800 . ? C21 C25 1.470(3) . ? C21 C22 1.472(3) . ? C21 C211 1.521(3) . ? C22 C23 1.371(3) . ? C22 C221 1.497(4) . ? C23 C24 1.432(4) . ? C23 C231 1.502(3) . ? C24 C25 1.374(3) . ? C24 C241 1.499(3) . ? C25 C251 1.501(4) . ? C211 H21A 0.9800 . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C231 H23A 0.9800 . ? C231 H23B 0.9800 . ? C231 H23C 0.9800 . ? C241 H24A 0.9800 . ? C241 H24B 0.9800 . ? C241 H24C 0.9800 . ? C251 H25A 0.9800 . ? C251 H25B 0.9800 . ? C251 H25C 0.9800 . ? C31 C36 1.375(3) . ? C31 C32 1.381(3) . ? C32 C33 1.377(3) . ? C33 C34 1.372(4) . ? C34 C35 1.368(4) . ? C35 C36 1.378(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31 Ga C21 117.14(9) . . ? C31 Ga C41 120.8(3) . . ? C21 Ga C41 121.3(3) . . ? C31 Ga C11 116.55(14) . . ? C21 Ga C11 123.56(14) . . ? C41 Ga C11 8.1(3) . . ? C31 Ga C12 116.59(13) . . ? C21 Ga C12 120.46(15) . . ? C41 Ga C12 32.4(3) . . ? C11 Ga C12 39.8(2) . . ? C31 Ga C42 104.0(4) . . ? C21 Ga C42 130.5(4) . . ? C41 Ga C42 39.1(5) . . ? C11 Ga C42 45.1(4) . . ? C12 Ga C42 12.7(4) . . ? C15 C11 C12 109.7(6) . . ? C15 C11 C111 123.3(6) . . ? C12 C11 C111 122.5(4) . . ? C15 C11 Ga 100.6(5) . . ? C12 C11 Ga 70.3(3) . . ? C111 C11 Ga 115.9(3) . . ? C13 C12 C11 105.6(5) . . ? C13 C12 C121 125.3(5) . . ? C11 C12 C121 126.3(4) . . ? C13 C12 Ga 97.8(4) . . ? C11 C12 Ga 69.9(3) . . ? C121 C12 Ga 113.9(3) . . ? C12 C13 C14 110.5(5) . . ? C12 C13 C131 124.4(5) . . ? C14 C13 C131 125.2(5) . . ? C141 C14 C15 126.6(9) . . ? C141 C14 C13 125.7(5) . . ? C15 C14 C13 107.6(7) . . ? C151 C15 C11 126.0(8) . . ? C151 C15 C14 127.3(7) . . ? C11 C15 C14 106.7(8) . . ? C45 C41 C411 124.5(15) . . ? C45 C41 C42 98.9(15) . . ? C411 C41 C42 130.2(10) . . ? C45 C41 Ga 93.9(12) . . ? C411 C41 Ga 117.5(8) . . ? C42 C41 Ga 77.7(7) . . ? C43 C42 C41 109.2(13) . . ? C43 C42 C421 130.2(13) . . ? C41 C42 C421 120.1(11) . . ? C43 C42 Ga 100.7(10) . . ? C41 C42 Ga 63.2(7) . . ? C421 C42 Ga 107.1(9) . . ? C44 C43 C42 104.2(15) . . ? C44 C43 C431 133.2(14) . . ? C42 C43 C431 122.5(13) . . ? C45 C44 C43 114(2) . . ? C45 C44 C441 129(2) . . ? C43 C44 C441 116.5(14) . . ? C44 C45 C41 113(2) . . ? C44 C45 C451 121.1(19) . . ? C41 C45 C451 125.1(18) . . ? C41 C411 H41A 109.5 . . ? C41 C411 H41B 109.5 . . ? H41A C411 H41B 109.5 . . ? C41 C411 H41C 109.5 . . ? H41A C411 H41C 109.5 . . ? H41B C411 H41C 109.5 . . ? C42 C421 H42A 109.5 . . ? C42 C421 H42B 109.5 . . ? H42A C421 H42B 109.5 . . ? C42 C421 H42C 109.5 . . ? H42A C421 H42C 109.5 . . ? H42B C421 H42C 109.5 . . ? C43 C431 H43A 109.5 . . ? C43 C431 H43B 109.5 . . ? H43A C431 H43B 109.5 . . ? C43 C431 H43C 109.5 . . ? H43A C431 H43C 109.5 . . ? H43B C431 H43C 109.5 . . ? C44 C441 H44A 109.5 . . ? C44 C441 H44B 109.5 . . ? H44A C441 H44B 109.5 . . ? C44 C441 H44C 109.5 . . ? H44A C441 H44C 109.5 . . ? H44B C441 H44C 109.5 . . ? C45 C451 H45A 109.5 . . ? C45 C451 H45B 109.5 . . ? H45A C451 H45B 109.5 . . ? C45 C451 H45C 109.5 . . ? H45A C451 H45C 109.5 . . ? H45B C451 H45C 109.5 . . ? C25 C21 C22 105.13(19) . . ? C25 C21 C211 120.9(2) . . ? C22 C21 C211 120.7(2) . . ? C25 C21 Ga 91.38(15) . . ? C22 C21 Ga 95.12(15) . . ? C211 C21 Ga 117.28(16) . . ? C23 C22 C21 107.9(2) . . ? C23 C22 C221 128.5(2) . . ? C21 C22 C221 123.6(2) . . ? C22 C23 C24 109.6(2) . . ? C22 C23 C231 127.8(2) . . ? C24 C23 C231 122.6(2) . . ? C25 C24 C23 108.9(2) . . ? C25 C24 C241 126.9(2) . . ? C23 C24 C241 124.2(2) . . ? C24 C25 C21 108.3(2) . . ? C24 C25 C251 127.7(2) . . ? C21 C25 C251 123.9(2) . . ? C21 C211 H21A 109.5 . . ? C21 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C21 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C23 C231 H23A 109.5 . . ? C23 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C23 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C24 C241 H24A 109.5 . . ? C24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? C24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C25 C251 H25A 109.5 . . ? C25 C251 H25B 109.5 . . ? H25A C251 H25B 109.5 . . ? C25 C251 H25C 109.5 . . ? H25A C251 H25C 109.5 . . ? H25B C251 H25C 109.5 . . ? C36 C31 C32 115.6(2) . . ? C36 C31 Ga 122.90(17) . . ? C32 C31 Ga 121.51(17) . . ? F2 C32 C33 117.5(2) . . ? F2 C32 C31 119.7(2) . . ? C33 C32 C31 122.9(2) . . ? F3 C33 C34 120.1(2) . . ? F3 C33 C32 120.6(3) . . ? C34 C33 C32 119.3(2) . . ? F4 C34 C35 120.0(3) . . ? F4 C34 C33 120.0(3) . . ? C35 C34 C33 120.0(2) . . ? F5 C35 C34 119.9(3) . . ? F5 C35 C36 121.1(3) . . ? C34 C35 C36 119.0(3) . . ? F6 C36 C31 119.6(2) . . ? F6 C36 C35 117.0(2) . . ? C31 C36 C35 123.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C31 Ga C11 C15 -6.8(5) . . . . ? C21 Ga C11 C15 153.8(5) . . . . ? C41 Ga C11 C15 -130(3) . . . . ? C12 Ga C11 C15 -107.3(6) . . . . ? C42 Ga C11 C15 -90.1(7) . . . . ? C31 Ga C11 C12 100.5(3) . . . . ? C21 Ga C11 C12 -98.9(3) . . . . ? C41 Ga C11 C12 -23(3) . . . . ? C42 Ga C11 C12 17.2(6) . . . . ? C31 Ga C11 C111 -142.1(3) . . . . ? C21 Ga C11 C111 18.5(4) . . . . ? C41 Ga C11 C111 95(3) . . . . ? C12 Ga C11 C111 117.4(4) . . . . ? C42 Ga C11 C111 134.6(6) . . . . ? C15 C11 C12 C13 1.8(7) . . . . ? C111 C11 C12 C13 158.5(5) . . . . ? Ga C11 C12 C13 -92.7(4) . . . . ? C15 C11 C12 C121 -160.0(6) . . . . ? C111 C11 C12 C121 -3.3(8) . . . . ? Ga C11 C12 C121 105.5(5) . . . . ? C15 C11 C12 Ga 94.5(5) . . . . ? C111 C11 C12 Ga -108.8(4) . . . . ? C31 Ga C12 C13 3.4(4) . . . . ? C21 Ga C12 C13 -149.0(3) . . . . ? C41 Ga C12 C13 109.6(7) . . . . ? C11 Ga C12 C13 103.8(5) . . . . ? C42 Ga C12 C13 -4(2) . . . . ? C31 Ga C12 C11 -100.4(3) . . . . ? C21 Ga C12 C11 107.2(3) . . . . ? C41 Ga C12 C11 5.8(7) . . . . ? C42 Ga C12 C11 -108(3) . . . . ? C31 Ga C12 C121 137.8(3) . . . . ? C21 Ga C12 C121 -14.6(4) . . . . ? C41 Ga C12 C121 -116.0(7) . . . . ? C11 Ga C12 C121 -121.9(4) . . . . ? C42 Ga C12 C121 130(3) . . . . ? C11 C12 C13 C14 -0.6(7) . . . . ? C121 C12 C13 C14 161.4(6) . . . . ? Ga C12 C13 C14 -71.9(6) . . . . ? C11 C12 C13 C131 -179.9(5) . . . . ? C121 C12 C13 C131 -17.9(9) . . . . ? Ga C12 C13 C131 108.9(5) . . . . ? C12 C13 C14 C141 176.5(7) . . . . ? C131 C13 C14 C141 -4.3(11) . . . . ? C12 C13 C14 C15 -0.7(9) . . . . ? C131 C13 C14 C15 178.5(6) . . . . ? C12 C11 C15 C151 178.6(8) . . . . ? C111 C11 C15 C151 22.1(12) . . . . ? Ga C11 C15 C151 -108.7(8) . . . . ? C12 C11 C15 C14 -2.2(9) . . . . ? C111 C11 C15 C14 -158.7(6) . . . . ? Ga C11 C15 C14 70.5(7) . . . . ? C141 C14 C15 C151 3.8(15) . . . . ? C13 C14 C15 C151 -179.1(8) . . . . ? C141 C14 C15 C11 -175.4(7) . . . . ? C13 C14 C15 C11 1.8(9) . . . . ? C31 Ga C41 C45 -24.9(14) . . . . ? C21 Ga C41 C45 144.5(13) . . . . ? C11 Ga C41 C45 36(3) . . . . ? C12 Ga C41 C45 -116.9(14) . . . . ? C42 Ga C41 C45 -98.3(15) . . . . ? C31 Ga C41 C411 -157.5(6) . . . . ? C21 Ga C41 C411 12.0(9) . . . . ? C11 Ga C41 C411 -97(3) . . . . ? C12 Ga C41 C411 110.6(10) . . . . ? C42 Ga C41 C411 129.2(11) . . . . ? C31 Ga C41 C42 73.4(7) . . . . ? C21 Ga C41 C42 -117.2(7) . . . . ? C11 Ga C41 C42 134(3) . . . . ? C12 Ga C41 C42 -18.6(7) . . . . ? C45 C41 C42 C43 -0.5(17) . . . . ? C411 C41 C42 C43 151.7(13) . . . . ? Ga C41 C42 C43 -92.5(12) . . . . ? C45 C41 C42 C421 -172.8(15) . . . . ? C411 C41 C42 C421 -21(2) . . . . ? Ga C41 C42 C421 95.1(12) . . . . ? C45 C41 C42 Ga 92.1(12) . . . . ? C411 C41 C42 Ga -115.7(12) . . . . ? C31 Ga C42 C43 -15.7(11) . . . . ? C21 Ga C42 C43 -161.9(8) . . . . ? C41 Ga C42 C43 106.2(13) . . . . ? C11 Ga C42 C43 98.0(12) . . . . ? C12 Ga C42 C43 157(3) . . . . ? C31 Ga C42 C41 -122.0(6) . . . . ? C21 Ga C42 C41 91.8(7) . . . . ? C11 Ga C42 C41 -8.3(6) . . . . ? C12 Ga C42 C41 51(2) . . . . ? C31 Ga C42 C421 122.5(8) . . . . ? C21 Ga C42 C421 -23.7(11) . . . . ? C41 Ga C42 C421 -115.6(11) . . . . ? C11 Ga C42 C421 -123.8(10) . . . . ? C12 Ga C42 C421 -64(2) . . . . ? C41 C42 C43 C44 -2.5(19) . . . . ? C421 C42 C43 C44 168.8(16) . . . . ? Ga C42 C43 C44 -67.7(15) . . . . ? C41 C42 C43 C431 178.7(11) . . . . ? C421 C42 C43 C431 -10(2) . . . . ? Ga C42 C43 C431 113.5(12) . . . . ? C42 C43 C44 C45 5(3) . . . . ? C431 C43 C44 C45 -176.4(18) . . . . ? C42 C43 C44 C441 177.5(14) . . . . ? C431 C43 C44 C441 -4(3) . . . . ? C43 C44 C45 C41 -6(3) . . . . ? C441 C44 C45 C41 -177.1(17) . . . . ? C43 C44 C45 C451 -178.2(18) . . . . ? C441 C44 C45 C451 10(4) . . . . ? C411 C41 C45 C44 -150.9(18) . . . . ? C42 C41 C45 C44 4(2) . . . . ? Ga C41 C45 C44 82(2) . . . . ? C411 C41 C45 C451 21(3) . . . . ? C42 C41 C45 C451 175.6(19) . . . . ? Ga C41 C45 C451 -106.3(19) . . . . ? C31 Ga C21 C25 59.86(16) . . . . ? C41 Ga C21 C25 -109.9(3) . . . . ? C11 Ga C21 C25 -100.68(18) . . . . ? C12 Ga C21 C25 -147.9(2) . . . . ? C42 Ga C21 C25 -157.5(5) . . . . ? C31 Ga C21 C22 -45.46(18) . . . . ? C41 Ga C21 C22 144.7(3) . . . . ? C11 Ga C21 C22 154.00(17) . . . . ? C12 Ga C21 C22 106.8(2) . . . . ? C42 Ga C21 C22 97.2(5) . . . . ? C31 Ga C21 C211 -173.98(19) . . . . ? C41 Ga C21 C211 16.2(4) . . . . ? C11 Ga C21 C211 25.5(3) . . . . ? C12 Ga C21 C211 -21.7(3) . . . . ? C42 Ga C21 C211 -31.3(6) . . . . ? C25 C21 C22 C23 -4.5(3) . . . . ? C211 C21 C22 C23 -145.6(2) . . . . ? Ga C21 C22 C23 88.37(18) . . . . ? C25 C21 C22 C221 173.9(2) . . . . ? C211 C21 C22 C221 32.8(4) . . . . ? Ga C21 C22 C221 -93.2(2) . . . . ? C21 C22 C23 C24 3.2(3) . . . . ? C221 C22 C23 C24 -175.1(2) . . . . ? C21 C22 C23 C231 -173.5(2) . . . . ? C221 C22 C23 C231 8.2(4) . . . . ? C22 C23 C24 C25 -0.6(3) . . . . ? C231 C23 C24 C25 176.3(2) . . . . ? C22 C23 C24 C241 -178.9(2) . . . . ? C231 C23 C24 C241 -2.0(4) . . . . ? C23 C24 C25 C21 -2.3(3) . . . . ? C241 C24 C25 C21 176.0(2) . . . . ? C23 C24 C25 C251 175.2(3) . . . . ? C241 C24 C25 C251 -6.5(4) . . . . ? C22 C21 C25 C24 4.1(3) . . . . ? C211 C21 C25 C24 145.1(2) . . . . ? Ga C21 C25 C24 -91.59(18) . . . . ? C22 C21 C25 C251 -173.5(2) . . . . ? C211 C21 C25 C251 -32.5(4) . . . . ? Ga C21 C25 C251 90.8(3) . . . . ? C21 Ga C31 C36 -95.9(2) . . . . ? C41 Ga C31 C36 74.0(4) . . . . ? C11 Ga C31 C36 66.1(2) . . . . ? C12 Ga C31 C36 110.8(3) . . . . ? C42 Ga C31 C36 112.5(5) . . . . ? C21 Ga C31 C32 82.0(2) . . . . ? C41 Ga C31 C32 -108.2(4) . . . . ? C11 Ga C31 C32 -116.1(2) . . . . ? C12 Ga C31 C32 -71.4(3) . . . . ? C42 Ga C31 C32 -69.6(5) . . . . ? C36 C31 C32 F2 179.8(2) . . . . ? Ga C31 C32 F2 1.9(3) . . . . ? C36 C31 C32 C33 0.7(3) . . . . ? Ga C31 C32 C33 -177.24(18) . . . . ? F2 C32 C33 F3 -0.6(3) . . . . ? C31 C32 C33 F3 178.5(2) . . . . ? F2 C32 C33 C34 179.7(2) . . . . ? C31 C32 C33 C34 -1.2(4) . . . . ? F3 C33 C34 F4 0.8(4) . . . . ? C32 C33 C34 F4 -179.5(2) . . . . ? F3 C33 C34 C35 -179.0(2) . . . . ? C32 C33 C34 C35 0.7(4) . . . . ? F4 C34 C35 F5 0.5(4) . . . . ? C33 C34 C35 F5 -179.7(2) . . . . ? F4 C34 C35 C36 -179.6(2) . . . . ? C33 C34 C35 C36 0.2(4) . . . . ? C32 C31 C36 F6 -178.3(2) . . . . ? Ga C31 C36 F6 -0.4(3) . . . . ? C32 C31 C36 C35 0.2(3) . . . . ? Ga C31 C36 C35 178.1(2) . . . . ? F5 C35 C36 F6 -2.2(4) . . . . ? C34 C35 C36 F6 177.9(2) . . . . ? F5 C35 C36 C31 179.3(2) . . . . ? C34 C35 C36 C31 -0.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.441 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.064 # Attachment 'MCp2GaCl.cif' data_12 _database_code_depnum_ccdc_archive 'CCDC 664847' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'bis(pentamethylcyclopentadienyl)gallium chloride' _chemical_formula_moiety 'C20 H30 Cl Ga' _chemical_formula_structural 'C20 H30 Cl Ga' _chemical_formula_analytical ? _chemical_formula_sum 'C20 H30 Cl Ga' _chemical_formula_weight 375.61 _chemical_melting_point ? _chemical_compound_source selfmade 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.672(2) _cell_length_b 14.309(3) _cell_length_c 23.345(5) _cell_angle_alpha 80.23(3) _cell_angle_beta 85.84(3) _cell_angle_gamma 84.53(3) _cell_volume 2837.4(10) _cell_formula_units_Z 6 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 45374 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 27.56 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method ? _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 1.592 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45374 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.56 _reflns_number_total 12490 _reflns_number_observed 8695 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution SHELX-93 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+5.8287P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12486 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_obs 0.0555 _refine_ls_wR_factor_all 0.1452 _refine_ls_wR_factor_obs 0.1273 _refine_ls_goodness_of_fit_all 1.059 _refine_ls_goodness_of_fit_obs 1.124 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.124 _refine_ls_shift/esd_max 0.474 _refine_ls_shift/esd_mean 0.004 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group C11 C 0.9552(5) -0.1091(3) 0.3932(2) 0.0289(9) Uani 1 d . . C12 C 1.1265(5) -0.1357(3) 0.3882(2) 0.0279(9) Uani 1 d . . C13 C 1.1526(5) -0.2317(3) 0.3963(2) 0.0294(9) Uani 1 d . . C14 C 1.0041(5) -0.2735(3) 0.4056(2) 0.0296(9) Uani 1 d . . C15 C 0.8879(5) -0.2032(3) 0.4026(2) 0.0288(9) Uani 1 d . . C21 C 0.9312(5) -0.0486(3) 0.2366(2) 0.0300(9) Uani 1 d . . C22 C 1.1011(5) -0.0407(3) 0.2294(2) 0.0326(9) Uani 1 d . . C23 C 1.1750(5) -0.1292(3) 0.2384(2) 0.0353(10) Uani 1 d . . C24 C 1.0602(5) -0.1989(3) 0.2494(2) 0.0316(9) Uani 1 d . . C25 C 0.9164(5) -0.1534(3) 0.2469(2) 0.0290(9) Uani 1 d . . C31 C 0.6039(5) 0.2099(3) 0.4233(2) 0.0306(9) Uani 1 d . . C32 C 0.4417(5) 0.2533(3) 0.4142(2) 0.0322(9) Uani 1 d . . C33 C 0.4389(5) 0.3482(3) 0.4139(2) 0.0331(9) Uani 1 d . . C34 C 0.5926(5) 0.3722(3) 0.4246(2) 0.0360(10) Uani 1 d . . C35 C 0.6907(5) 0.2915(3) 0.4314(2) 0.0332(9) Uani 1 d . . C41 C 0.6366(5) 0.2883(3) 0.2668(2) 0.0276(9) Uani 1 d . . C42 C 0.4668(5) 0.3091(3) 0.2559(2) 0.0307(9) Uani 1 d . . C43 C 0.4269(5) 0.4025(3) 0.2546(2) 0.0329(9) Uani 1 d . . C44 C 0.5634(5) 0.4495(3) 0.2663(2) 0.0331(9) Uani 1 d . . C45 C 0.6856(5) 0.3839(3) 0.2744(2) 0.0292(9) Uani 1 d . . C51 C 1.1323(5) 0.2940(3) 0.0587(2) 0.0281(9) Uani 1 d . . C52 C 1.3017(5) 0.2618(3) 0.0642(2) 0.0277(9) Uani 1 d . . C53 C 1.3236(5) 0.1674(3) 0.0644(2) 0.0316(9) Uani 1 d . . C54 C 1.1736(5) 0.1307(3) 0.0583(2) 0.0297(9) Uani 1 d . . C55 C 1.0609(5) 0.2038(3) 0.0544(2) 0.0276(9) Uani 1 d . . C61 C 1.1769(5) 0.3791(3) -0.0971(2) 0.0264(8) Uani 1 d . . C62 C 1.3462(5) 0.3888(3) -0.0957(2) 0.0316(9) Uani 1 d . . C63 C 1.4228(5) 0.3011(3) -0.0887(2) 0.0323(9) Uani 1 d . . C64 C 1.3122(5) 0.2305(3) -0.0882(2) 0.0308(9) Uani 1 d . . C65 C 1.1686(5) 0.2743(3) -0.0940(2) 0.0280(9) Uani 1 d . . C111 C 0.9112(5) -0.0580(3) 0.4457(2) 0.0352(10) Uani 1 d . . H11A H 0.9586(28) 0.0011(10) 0.4399(6) 0.053 Uiso 1 calc R . H11B H 0.9471(30) -0.0975(9) 0.4805(3) 0.053 Uiso 1 calc R . H11C H 0.8005(6) -0.0457(19) 0.4496(8) 0.053 Uiso 1 calc R . C121 C 1.2445(5) -0.0634(3) 0.3796(2) 0.0382(10) Uani 1 d . . H12A H 1.2232(21) -0.0219(13) 0.4080(8) 0.057 Uiso 1 calc R . H12B H 1.2393(24) -0.0268(14) 0.3413(5) 0.057 Uiso 1 calc R . H12C H 1.3464(6) -0.0954(3) 0.3842(13) 0.057 Uiso 1 calc R . C131 C 1.3058(5) -0.2902(3) 0.3997(2) 0.0373(10) Uani 1 d . . H13A H 1.3121(15) -0.3338(15) 0.3725(9) 0.056 Uiso 1 calc R . H13B H 1.3149(15) -0.3252(16) 0.4384(4) 0.056 Uiso 1 calc R . H13C H 1.3884(5) -0.2490(3) 0.3906(13) 0.056 Uiso 1 calc R . C141 C 0.9889(5) -0.3793(3) 0.4184(2) 0.0424(11) Uani 1 d . . H14A H 1.0379(33) -0.4059(5) 0.4538(8) 0.064 Uiso 1 calc R . H14B H 1.0381(33) -0.4085(4) 0.3869(7) 0.064 Uiso 1 calc R . H14C H 0.8811(5) -0.3907(3) 0.4227(14) 0.064 Uiso 1 calc R . C151 C 0.7174(5) -0.2147(3) 0.4132(2) 0.0391(10) Uani 1 d . . H15A H 0.6598(5) -0.1627(12) 0.3903(10) 0.059 Uiso 1 calc R . H15B H 0.6883(8) -0.2154(22) 0.4537(3) 0.059 Uiso 1 calc R . H15C H 0.6951(7) -0.2736(11) 0.4023(12) 0.059 Uiso 1 calc R . C211 C 0.8306(6) 0.0106(3) 0.1907(2) 0.0407(11) Uani 1 d . . H21A H 0.7231(6) 0.0064(18) 0.2032(6) 0.061 Uiso 1 calc R . H21B H 0.8507(27) -0.0132(14) 0.1546(4) 0.061 Uiso 1 calc R . H21C H 0.8543(26) 0.0757(5) 0.1854(10) 0.061 Uiso 1 calc R . C221 C 1.1731(6) 0.0525(3) 0.2136(2) 0.0453(12) Uani 1 d . . H22A H 1.1409(31) 0.0919(10) 0.2424(8) 0.068 Uiso 1 calc R . H22B H 1.1403(31) 0.0841(11) 0.1763(7) 0.068 Uiso 1 calc R . H22C H 1.2841(6) 0.0409(4) 0.2119(14) 0.068 Uiso 1 calc R . C231 C 1.3472(5) -0.1555(4) 0.2391(2) 0.0528(13) Uani 1 d . . H23A H 1.3763(8) -0.2007(19) 0.2134(12) 0.079 Uiso 1 calc R . H23B H 1.3737(8) -0.1831(23) 0.2779(4) 0.079 Uiso 1 calc R . H23C H 1.4014(5) -0.0995(6) 0.2264(15) 0.079 Uiso 1 calc R . C241 C 1.1018(6) -0.3044(3) 0.2592(2) 0.0473(12) Uani 1 d . . H24A H 1.1659(33) -0.3214(5) 0.2919(9) 0.071 Uiso 1 calc R . H24B H 1.1574(34) -0.3223(5) 0.2251(6) 0.071 Uiso 1 calc R . H24C H 1.0089(7) -0.3370(3) 0.2670(15) 0.071 Uiso 1 calc R . C251 C 0.7631(5) -0.1970(3) 0.2515(2) 0.0414(11) Uani 1 d . . H25A H 0.7350(18) -0.2032(21) 0.2134(2) 0.062 Uiso 1 calc R . H25B H 0.6845(9) -0.1568(11) 0.2688(12) 0.062 Uiso 1 calc R . H25C H 0.7723(11) -0.2587(10) 0.2754(11) 0.062 Uiso 1 calc R . C311 C 0.6192(6) 0.1209(3) 0.4694(2) 0.0431(11) Uani 1 d . . H31A H 0.5704(33) 0.0708(8) 0.4571(7) 0.065 Uiso 1 calc R . H31B H 0.5698(33) 0.1345(7) 0.5056(4) 0.065 Uiso 1 calc R . H31C H 0.7270(6) 0.1015(13) 0.4745(10) 0.065 Uiso 1 calc R . C321 C 0.3080(5) 0.1968(3) 0.4081(2) 0.0434(11) Uani 1 d . . H32A H 0.2644(24) 0.1723(19) 0.4460(2) 0.065 Uiso 1 calc R . H32B H 0.3441(9) 0.1449(14) 0.3880(12) 0.065 Uiso 1 calc R . H32C H 0.2303(17) 0.2371(6) 0.3864(12) 0.065 Uiso 1 calc R . C331 C 0.2975(6) 0.4190(4) 0.4056(2) 0.0499(13) Uani 1 d . . H33A H 0.3205(14) 0.4703(13) 0.3749(10) 0.075 Uiso 1 calc R . H33B H 0.2700(25) 0.4437(19) 0.4411(5) 0.075 Uiso 1 calc R . H33C H 0.2123(12) 0.3878(7) 0.3956(15) 0.075 Uiso 1 calc R . C341 C 0.6324(6) 0.4708(3) 0.4263(2) 0.0493(12) Uani 1 d . . H34A H 0.5531(20) 0.5020(9) 0.4489(12) 0.074 Uiso 1 calc R . H34B H 0.6396(39) 0.5056(8) 0.3874(3) 0.074 Uiso 1 calc R . H34C H 0.7301(20) 0.4682(3) 0.4436(14) 0.074 Uiso 1 calc R . C351 C 0.8570(5) 0.2806(4) 0.4465(2) 0.0443(11) Uani 1 d . . H35A H 0.9175(8) 0.2440(20) 0.4207(9) 0.066 Uiso 1 calc R . H35B H 0.8651(7) 0.2486(20) 0.4860(5) 0.066 Uiso 1 calc R . H35C H 0.8952(12) 0.3423(4) 0.4426(13) 0.066 Uiso 1 calc R . C411 C 0.7235(5) 0.2513(3) 0.2145(2) 0.0384(10) Uani 1 d . . H41A H 0.8323(7) 0.2407(21) 0.2210(6) 0.058 Uiso 1 calc R . H41B H 0.7080(30) 0.2974(10) 0.1800(3) 0.058 Uiso 1 calc R . H41C H 0.6847(24) 0.1926(12) 0.2097(8) 0.058 Uiso 1 calc R . C421 C 0.3687(5) 0.2355(3) 0.2426(2) 0.0411(11) Uani 1 d . . H42A H 0.3860(28) 0.1779(8) 0.2700(9) 0.062 Uiso 1 calc R . H42B H 0.3960(25) 0.2229(16) 0.2039(5) 0.062 Uiso 1 calc R . H42C H 0.2612(6) 0.2586(10) 0.2455(13) 0.062 Uiso 1 calc R . C431 C 0.2719(5) 0.4554(3) 0.2408(2) 0.0439(11) Uani 1 d . . H43A H 0.2858(7) 0.5070(14) 0.2093(9) 0.066 Uiso 1 calc R . H43B H 0.2267(17) 0.4801(20) 0.2745(5) 0.066 Uiso 1 calc R . H43C H 0.2045(13) 0.4128(6) 0.2298(14) 0.066 Uiso 1 calc R . C441 C 0.5589(6) 0.5540(3) 0.2663(2) 0.0417(11) Uani 1 d . . H44A H 0.4794(25) 0.5721(5) 0.2941(10) 0.063 Uiso 1 calc R . H44B H 0.5369(37) 0.5877(3) 0.2282(4) 0.063 Uiso 1 calc R . H44C H 0.6575(13) 0.5694(4) 0.2766(13) 0.063 Uiso 1 calc R . C451 C 0.8488(5) 0.3981(3) 0.2853(2) 0.0386(10) Uani 1 d . . H45A H 0.9177(6) 0.3772(20) 0.2551(7) 0.058 Uiso 1 calc R . H45B H 0.8755(12) 0.3618(17) 0.3223(6) 0.058 Uiso 1 calc R . H45C H 0.8579(9) 0.4643(4) 0.2856(13) 0.058 Uiso 1 calc R . C511 C 1.0638(5) 0.3367(3) 0.1120(2) 0.0326(9) Uani 1 d . . H51A H 0.9562(9) 0.3572(18) 0.1071(6) 0.049 Uiso 1 calc R . H51B H 1.1189(22) 0.3901(13) 0.1160(7) 0.049 Uiso 1 calc R . H51C H 1.0733(30) 0.2894(7) 0.1464(2) 0.049 Uiso 1 calc R . C521 C 1.4208(5) 0.3278(3) 0.0717(2) 0.0349(10) Uani 1 d . . H52A H 1.3883(16) 0.3600(15) 0.1040(8) 0.052 Uiso 1 calc R . H52B H 1.4316(24) 0.3738(13) 0.0369(5) 0.052 Uiso 1 calc R . H52C H 1.5186(9) 0.2918(4) 0.0789(12) 0.052 Uiso 1 calc R . C531 C 1.4705(5) 0.1042(3) 0.0741(2) 0.0415(11) Uani 1 d . . H53A H 1.4965(20) 0.0728(17) 0.0410(6) 0.062 Uiso 1 calc R . H53B H 1.4563(12) 0.0575(14) 0.1083(8) 0.062 Uiso 1 calc R . H53C H 1.5530(10) 0.1419(4) 0.0790(14) 0.062 Uiso 1 calc R . C541 C 1.1552(6) 0.0272(3) 0.0583(2) 0.0402(11) Uani 1 d . . H54A H 1.1762(35) -0.0086(4) 0.0960(4) 0.060 Uiso 1 calc R . H54B H 1.2267(25) 0.0043(6) 0.0294(9) 0.060 Uiso 1 calc R . H54C H 1.0510(11) 0.0199(4) 0.0495(13) 0.060 Uiso 1 calc R . C551 C 0.8901(5) 0.1988(3) 0.0528(2) 0.0349(10) Uani 1 d . . H55A H 0.8499(7) 0.2476(13) 0.0228(8) 0.052 Uiso 1 calc R . H55B H 0.8403(6) 0.2080(20) 0.0897(4) 0.052 Uiso 1 calc R . H55C H 0.8702(5) 0.1376(8) 0.0447(12) 0.052 Uiso 1 calc R . C611 C 1.0897(5) 0.4419(3) -0.1457(2) 0.0394(11) Uani 1 d . . H61A H 0.9806(7) 0.4348(17) -0.1390(7) 0.059 Uiso 1 calc R . H61B H 1.1252(26) 0.4233(15) -0.1824(2) 0.059 Uiso 1 calc R . H61C H 1.1082(29) 0.5072(4) -0.1464(9) 0.059 Uiso 1 calc R . C621 C 1.4156(6) 0.4830(3) -0.1043(2) 0.0449(12) Uani 1 d . . H62A H 1.3585(24) 0.5235(9) -0.0799(11) 0.067 Uiso 1 calc R . H62B H 1.4106(35) 0.5126(11) -0.1443(4) 0.067 Uiso 1 calc R . H62C H 1.5219(12) 0.4731(4) -0.0941(13) 0.067 Uiso 1 calc R . C631 C 1.5939(5) 0.2759(4) -0.0815(2) 0.0534(13) Uani 1 d . . H63A H 1.6367(10) 0.2423(23) -0.1120(9) 0.080 Uiso 1 calc R . H63B H 1.6088(6) 0.2362(21) -0.0445(7) 0.080 Uiso 1 calc R . H63C H 1.6451(8) 0.3330(4) -0.0834(16) 0.080 Uiso 1 calc R . C641 C 1.3583(6) 0.1257(3) -0.0827(2) 0.0435(12) Uani 1 d . . H64A H 1.4248(31) 0.1064(5) -0.0509(9) 0.065 Uiso 1 calc R . H64B H 1.4126(33) 0.1124(4) -0.1182(6) 0.065 Uiso 1 calc R . H64C H 1.2672(6) 0.0914(3) -0.0756(14) 0.065 Uiso 1 calc R . C651 C 1.0197(5) 0.2295(3) -0.0986(2) 0.0382(10) Uani 1 d . . H65A H 1.0105(18) 0.2214(20) -0.1382(3) 0.057 Uiso 1 calc R . H65B H 0.9329(5) 0.2700(11) -0.0867(12) 0.057 Uiso 1 calc R . H65C H 1.0213(16) 0.1685(10) -0.0739(10) 0.057 Uiso 1 calc R . Cl1 Cl 0.61961(11) 0.03583(7) 0.32843(4) 0.0306(2) Uani 1 d . . Cl2 Cl 0.93896(11) 0.13368(7) 0.33194(4) 0.0290(2) Uani 1 d . . Cl3 Cl 0.84121(11) 0.45791(7) -0.01258(4) 0.0281(2) Uani 1 d . . Ga1 Ga 0.88940(5) -0.02656(3) 0.31932(2) 0.02653(12) Uani 1 d . . Ga2 Ga 0.67000(5) 0.19616(3) 0.34069(2) 0.02674(12) Uani 1 d . . Ga3 Ga 1.10581(5) 0.38910(3) -0.01426(2) 0.02510(12) Uani 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 C11 0.026(2) 0.030(2) 0.031(2) -0.004(2) -0.009(2) 0.004(2) C12 0.026(2) 0.034(2) 0.025(2) -0.004(2) -0.007(2) -0.005(2) C13 0.023(2) 0.035(2) 0.031(2) -0.009(2) -0.007(2) 0.001(2) C14 0.027(2) 0.027(2) 0.034(2) -0.004(2) -0.006(2) -0.002(2) C15 0.021(2) 0.032(2) 0.033(2) -0.004(2) -0.001(2) -0.004(2) C21 0.033(2) 0.031(2) 0.027(2) -0.008(2) -0.006(2) -0.001(2) C22 0.034(2) 0.042(2) 0.024(2) -0.009(2) -0.003(2) -0.010(2) C23 0.025(2) 0.052(3) 0.031(2) -0.012(2) -0.003(2) -0.002(2) C24 0.033(2) 0.033(2) 0.031(2) -0.010(2) -0.011(2) 0.001(2) C25 0.027(2) 0.030(2) 0.032(2) -0.007(2) -0.007(2) -0.004(2) C31 0.029(2) 0.031(2) 0.032(2) -0.005(2) -0.002(2) -0.005(2) C32 0.026(2) 0.034(2) 0.038(2) -0.008(2) -0.001(2) -0.005(2) C33 0.029(2) 0.033(2) 0.036(2) -0.004(2) -0.005(2) 0.001(2) C34 0.038(3) 0.036(2) 0.036(2) -0.008(2) -0.005(2) -0.005(2) C35 0.027(2) 0.040(2) 0.033(2) -0.007(2) -0.002(2) -0.003(2) C41 0.028(2) 0.024(2) 0.030(2) -0.002(2) -0.006(2) -0.001(2) C42 0.029(2) 0.031(2) 0.033(2) -0.005(2) -0.005(2) -0.003(2) C43 0.028(2) 0.036(2) 0.034(2) -0.005(2) -0.006(2) 0.000(2) C44 0.034(2) 0.031(2) 0.035(2) -0.007(2) -0.004(2) -0.003(2) C45 0.024(2) 0.032(2) 0.030(2) -0.003(2) -0.002(2) -0.004(2) C51 0.029(2) 0.024(2) 0.031(2) -0.003(2) -0.005(2) -0.001(2) C52 0.025(2) 0.026(2) 0.032(2) -0.005(2) -0.005(2) -0.003(2) C53 0.028(2) 0.035(2) 0.032(2) -0.007(2) -0.005(2) -0.001(2) C54 0.034(2) 0.027(2) 0.029(2) -0.004(2) -0.003(2) -0.005(2) C55 0.027(2) 0.030(2) 0.027(2) -0.003(2) -0.006(2) -0.008(2) C61 0.025(2) 0.026(2) 0.029(2) -0.007(2) -0.003(2) -0.001(2) C62 0.033(2) 0.035(2) 0.030(2) -0.012(2) 0.000(2) -0.008(2) C63 0.024(2) 0.042(2) 0.033(2) -0.012(2) -0.004(2) -0.003(2) C64 0.035(2) 0.028(2) 0.030(2) -0.007(2) -0.007(2) 0.001(2) C65 0.026(2) 0.030(2) 0.029(2) -0.008(2) -0.004(2) -0.003(2) C111 0.040(3) 0.031(2) 0.035(2) -0.008(2) -0.006(2) 0.005(2) C121 0.032(2) 0.041(3) 0.043(3) -0.002(2) -0.012(2) -0.010(2) C131 0.029(2) 0.036(2) 0.048(3) -0.008(2) -0.009(2) 0.002(2) C141 0.035(3) 0.027(2) 0.066(3) -0.006(2) -0.008(2) -0.007(2) C151 0.024(2) 0.042(3) 0.049(3) 0.000(2) -0.004(2) -0.004(2) C211 0.054(3) 0.034(2) 0.035(2) -0.008(2) -0.015(2) 0.007(2) C221 0.050(3) 0.049(3) 0.041(3) -0.013(2) 0.006(2) -0.023(2) C231 0.030(3) 0.074(4) 0.056(3) -0.020(3) -0.005(2) 0.005(2) C241 0.058(3) 0.036(3) 0.051(3) -0.015(2) -0.021(2) 0.012(2) C251 0.035(3) 0.045(3) 0.048(3) -0.012(2) -0.010(2) -0.013(2) C311 0.049(3) 0.040(3) 0.035(2) -0.002(2) 0.002(2) 0.010(2) C321 0.031(3) 0.042(3) 0.059(3) -0.013(2) 0.002(2) -0.012(2) C331 0.035(3) 0.048(3) 0.065(3) -0.007(2) -0.003(2) 0.005(2) C341 0.047(3) 0.038(3) 0.067(3) -0.014(2) -0.007(2) -0.007(2) C351 0.036(3) 0.058(3) 0.041(3) -0.014(2) -0.012(2) 0.002(2) C411 0.040(3) 0.037(2) 0.035(2) -0.003(2) -0.003(2) 0.009(2) C421 0.038(3) 0.037(2) 0.051(3) -0.004(2) -0.018(2) -0.011(2) C431 0.030(2) 0.043(3) 0.058(3) -0.008(2) -0.010(2) 0.006(2) C441 0.041(3) 0.033(2) 0.053(3) -0.010(2) -0.002(2) -0.002(2) C451 0.029(2) 0.042(3) 0.044(3) 0.002(2) -0.007(2) -0.010(2) C511 0.035(2) 0.032(2) 0.030(2) -0.004(2) -0.005(2) 0.002(2) C521 0.028(2) 0.036(2) 0.043(2) -0.005(2) -0.014(2) -0.006(2) C531 0.038(3) 0.029(2) 0.056(3) -0.006(2) -0.007(2) 0.007(2) C541 0.044(3) 0.030(2) 0.049(3) -0.010(2) -0.004(2) -0.006(2) C551 0.030(2) 0.037(2) 0.039(2) -0.004(2) -0.007(2) -0.009(2) C611 0.044(3) 0.040(3) 0.033(2) -0.010(2) -0.006(2) 0.012(2) C621 0.045(3) 0.045(3) 0.050(3) -0.017(2) 0.006(2) -0.018(2) C631 0.028(3) 0.071(4) 0.065(3) -0.026(3) -0.010(2) 0.003(2) C641 0.052(3) 0.031(2) 0.048(3) -0.012(2) -0.011(2) 0.011(2) C651 0.031(2) 0.045(3) 0.044(3) -0.017(2) -0.005(2) -0.010(2) Cl1 0.0217(5) 0.0285(5) 0.0426(6) -0.0074(4) -0.0053(4) -0.0024(4) Cl2 0.0220(5) 0.0272(5) 0.0391(5) -0.0079(4) -0.0054(4) -0.0017(4) Cl3 0.0228(5) 0.0275(5) 0.0358(5) -0.0088(4) -0.0075(4) -0.0002(4) Ga1 0.0228(2) 0.0262(2) 0.0314(2) -0.0058(2) -0.0064(2) -0.0006(2) Ga2 0.0221(2) 0.0266(2) 0.0314(2) -0.0041(2) -0.0040(2) -0.0008(2) Ga3 0.0232(2) 0.0247(2) 0.0280(2) -0.0054(2) -0.0056(2) 0.0002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 C15 1.493(6) . ? C11 C12 1.500(6) . ? C11 C111 1.538(6) . ? C11 Ga1 2.005(4) . ? C12 C13 1.354(6) . ? C12 C121 1.503(6) . ? C13 C14 1.458(6) . ? C13 C131 1.501(6) . ? C14 C15 1.352(6) . ? C14 C141 1.508(6) . ? C15 C151 1.501(6) . ? C21 C22 1.484(6) . ? C21 C25 1.494(6) . ? C21 C211 1.521(6) . ? C21 Ga1 2.010(4) . ? C22 C23 1.354(6) . ? C22 C221 1.504(6) . ? C23 C24 1.456(6) . ? C23 C231 1.506(6) . ? C24 C25 1.351(6) . ? C24 C241 1.500(6) . ? C25 C251 1.511(6) . ? C31 C35 1.492(6) . ? C31 C32 1.498(6) . ? C31 C311 1.523(6) . ? C31 Ga2 2.009(4) . ? C32 C33 1.354(6) . ? C32 C321 1.503(6) . ? C33 C34 1.457(6) . ? C33 C331 1.517(6) . ? C34 C35 1.361(6) . ? C34 C341 1.491(6) . ? C35 C351 1.497(6) . ? C41 C42 1.506(6) . ? C41 C45 1.513(6) . ? C41 C411 1.533(6) . ? C41 Ga2 2.006(4) . ? C42 C43 1.345(6) . ? C42 C421 1.499(6) . ? C43 C44 1.479(6) . ? C43 C431 1.506(6) . ? C44 C45 1.348(6) . ? C44 C441 1.493(6) . ? C45 C451 1.494(6) . ? C51 C52 1.505(6) . ? C51 C55 1.505(5) . ? C51 C511 1.534(5) . ? C51 Ga3 2.005(4) . ? C52 C53 1.346(6) . ? C52 C521 1.503(5) . ? C53 C54 1.473(6) . ? C53 C531 1.498(6) . ? C54 C55 1.357(6) . ? C54 C541 1.505(6) . ? C55 C551 1.494(6) . ? C61 C62 1.491(6) . ? C61 C65 1.498(5) . ? C61 C611 1.521(5) . ? C61 Ga3 2.011(4) . ? C62 C63 1.352(6) . ? C62 C621 1.506(6) . ? C63 C64 1.456(6) . ? C63 C631 1.508(6) . ? C64 C65 1.344(6) . ? C64 C641 1.501(6) . ? C65 C651 1.514(6) . ? Cl1 Ga1 2.4313(12) . ? Cl1 Ga2 2.4429(12) . ? Cl2 Ga2 2.4243(12) . ? Cl2 Ga1 2.4422(11) . ? Cl3 Ga3 2.4097(12) . ? Cl3 Ga3 2.4687(11) 2_765 ? Ga3 Cl3 2.4688(11) 2_765 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 C11 C12 103.1(3) . . ? C15 C11 C111 110.3(3) . . ? C12 C11 C111 111.1(3) . . ? C15 C11 Ga1 112.1(3) . . ? C12 C11 Ga1 109.4(3) . . ? C111 C11 Ga1 110.6(3) . . ? C13 C12 C11 109.2(3) . . ? C13 C12 C121 127.9(4) . . ? C11 C12 C121 122.8(4) . . ? C12 C13 C14 109.0(3) . . ? C12 C13 C131 127.8(4) . . ? C14 C13 C131 123.0(4) . . ? C15 C14 C13 109.2(3) . . ? C15 C14 C141 127.2(4) . . ? C13 C14 C141 123.6(4) . . ? C14 C15 C11 109.4(3) . . ? C14 C15 C151 126.7(4) . . ? C11 C15 C151 123.6(4) . . ? C22 C21 C25 104.0(3) . . ? C22 C21 C211 117.7(4) . . ? C25 C21 C211 116.0(3) . . ? C22 C21 Ga1 100.5(3) . . ? C25 C21 Ga1 98.0(3) . . ? C211 C21 Ga1 117.6(3) . . ? C23 C22 C21 108.9(4) . . ? C23 C22 C221 127.5(4) . . ? C21 C22 C221 123.6(4) . . ? C22 C23 C24 109.1(4) . . ? C22 C23 C231 127.5(4) . . ? C24 C23 C231 123.4(4) . . ? C25 C24 C23 109.4(4) . . ? C25 C24 C241 127.3(4) . . ? C23 C24 C241 123.3(4) . . ? C24 C25 C21 108.5(4) . . ? C24 C25 C251 127.8(4) . . ? C21 C25 C251 123.7(4) . . ? C35 C31 C32 104.0(3) . . ? C35 C31 C311 116.9(4) . . ? C32 C31 C311 115.4(4) . . ? C35 C31 Ga2 101.5(3) . . ? C32 C31 Ga2 98.9(3) . . ? C311 C31 Ga2 117.5(3) . . ? C33 C32 C31 108.6(4) . . ? C33 C32 C321 127.8(4) . . ? C31 C32 C321 123.6(4) . . ? C32 C33 C34 109.6(4) . . ? C32 C33 C331 125.8(4) . . ? C34 C33 C331 124.6(4) . . ? C35 C34 C33 109.1(4) . . ? C35 C34 C341 126.8(4) . . ? C33 C34 C341 124.1(4) . . ? C34 C35 C351 128.0(4) . . ? C34 C35 C31 108.7(4) . . ? C351 C35 C31 123.2(4) . . ? C42 C41 C45 103.2(3) . . ? C42 C41 C411 109.8(3) . . ? C45 C41 C411 112.0(3) . . ? C42 C41 Ga2 111.6(3) . . ? C45 C41 Ga2 108.7(3) . . ? C411 C41 Ga2 111.2(3) . . ? C43 C42 C421 127.7(4) . . ? C43 C42 C41 109.3(4) . . ? C421 C42 C41 122.7(4) . . ? C42 C43 C44 109.3(4) . . ? C42 C43 C431 127.2(4) . . ? C44 C43 C431 123.4(4) . . ? C45 C44 C43 109.2(4) . . ? C45 C44 C441 128.1(4) . . ? C43 C44 C441 122.7(4) . . ? C44 C45 C451 128.6(4) . . ? C44 C45 C41 109.0(4) . . ? C451 C45 C41 122.3(4) . . ? C52 C51 C55 103.2(3) . . ? C52 C51 C511 111.3(3) . . ? C55 C51 C511 111.4(3) . . ? C52 C51 Ga3 109.4(3) . . ? C55 C51 Ga3 110.7(3) . . ? C511 C51 Ga3 110.6(3) . . ? C53 C52 C51 109.6(3) . . ? C53 C52 C521 127.5(4) . . ? C51 C52 C521 122.9(3) . . ? C52 C53 C54 109.1(4) . . ? C52 C53 C531 127.8(4) . . ? C54 C53 C531 122.9(4) . . ? C55 C54 C53 109.2(3) . . ? C55 C54 C541 127.6(4) . . ? C53 C54 C541 123.2(4) . . ? C54 C55 C551 127.8(4) . . ? C54 C55 C51 109.0(3) . . ? C551 C55 C51 122.9(4) . . ? C62 C61 C65 103.4(3) . . ? C62 C61 C611 117.6(4) . . ? C65 C61 C611 115.2(3) . . ? C62 C61 Ga3 100.8(2) . . ? C65 C61 Ga3 98.5(2) . . ? C611 C61 Ga3 118.3(3) . . ? C63 C62 C61 109.0(4) . . ? C63 C62 C621 127.3(4) . . ? C61 C62 C621 123.6(4) . . ? C62 C63 C64 109.0(4) . . ? C62 C63 C631 127.7(4) . . ? C64 C63 C631 123.3(4) . . ? C65 C64 C63 109.6(4) . . ? C65 C64 C641 127.2(4) . . ? C63 C64 C641 123.2(4) . . ? C64 C65 C61 108.8(3) . . ? C64 C65 C651 127.8(4) . . ? C61 C65 C651 123.4(4) . . ? Ga1 Cl1 Ga2 96.73(4) . . ? Ga2 Cl2 Ga1 96.94(4) . . ? Ga3 Cl3 Ga3 96.82(4) . 2_765 ? C11 Ga1 C21 129.2(2) . . ? C11 Ga1 Cl1 111.36(12) . . ? C21 Ga1 Cl1 106.76(12) . . ? C11 Ga1 Cl2 104.19(12) . . ? C21 Ga1 Cl2 112.63(12) . . ? Cl1 Ga1 Cl2 83.10(4) . . ? C41 Ga2 C31 129.7(2) . . ? C41 Ga2 Cl2 104.97(12) . . ? C31 Ga2 Cl2 111.42(12) . . ? C41 Ga2 Cl1 110.64(12) . . ? C31 Ga2 Cl1 107.14(12) . . ? Cl2 Ga2 Cl1 83.23(4) . . ? C51 Ga3 C61 130.1(2) . . ? C51 Ga3 Cl3 107.94(12) . . ? C61 Ga3 Cl3 108.56(12) . . ? C51 Ga3 Cl3 104.76(12) . 2_765 ? C61 Ga3 Cl3 112.35(12) . 2_765 ? Cl3 Ga3 Cl3 83.18(4) . 2_765 ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 1.145 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.090 # Attachment 'MCp2GaMe.cif' data_13 _database_code_depnum_ccdc_archive 'CCDC 664848' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common bis(pentamethylcyclopentadienyl)methylgallane _chemical_melting_point ? _chemical_formula_moiety 'C21 H33 Ga1' _chemical_formula_sum 'C21 H33 Ga' _chemical_formula_weight 355.19 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.8112(4) _cell_length_b 11.2335(4) _cell_length_c 11.1606(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.797(3) _cell_angle_gamma 90.00 _cell_volume 977.16(8) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 11100 _cell_measurement_theta_min 3.29 _cell_measurement_theta_max 24.98 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method ? _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 1.404 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius KAPPA-CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11100 _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 24.98 _reflns_number_total 3352 _reflns_number_gt 3123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution SHELX-93 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.12(5) _refine_ls_number_reflns 3352 _refine_ls_number_parameters 201 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1170 _refine_ls_R_factor_gt 0.1135 _refine_ls_wR_factor_ref 0.3038 _refine_ls_wR_factor_gt 0.2995 _refine_ls_goodness_of_fit_ref 1.408 _refine_ls_restrained_S_all 1.408 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 Ga01 Ga 0.31711(10) 0.44402(12) 0.74115(7) 0.0211(4) Uani 1 1 d . . . C1 C 0.0702(12) 0.4292(13) 0.7434(10) 0.027(3) Uani 1 1 d . . . H1A H 0.0413 0.3498 0.7723 0.041 Uiso 1 1 calc R . . H1B H 0.0176 0.4407 0.6620 0.041 Uiso 1 1 calc R . . H1C H 0.0267 0.4897 0.7969 0.041 Uiso 1 1 calc R . . C24 C 0.2185(13) 0.6019(10) 0.9754(10) 0.030(2) Uani 1 1 d . . . C22 C 0.3541(14) 0.6669(10) 0.8110(10) 0.029(2) Uani 1 1 d . . . C23 C 0.2201(13) 0.6864(9) 0.8843(10) 0.028(2) Uani 1 1 d . . . C231 C 0.0860(19) 0.7847(13) 0.8641(14) 0.052(4) Uani 1 1 d . . . H23A H 0.1153 0.8344 0.7963 0.078 Uiso 1 1 calc R . . H23B H 0.0841 0.8339 0.9366 0.078 Uiso 1 1 calc R . . H23C H -0.0273 0.7488 0.8466 0.078 Uiso 1 1 calc R . . C15 C 0.3068(15) 0.2145(10) 0.6483(11) 0.033(2) Uani 1 1 d . . . C13 C 0.3051(15) 0.3595(10) 0.5070(9) 0.031(2) Uani 1 1 d . . . C11 C 0.4556(13) 0.2882(10) 0.6737(11) 0.031(2) Uani 1 1 d . . . C221 C 0.406(2) 0.7374(13) 0.7049(11) 0.048(3) Uani 1 1 d . . . H22A H 0.3573 0.7006 0.6307 0.072 Uiso 1 1 calc R . . H22B H 0.5316 0.7383 0.7044 0.072 Uiso 1 1 calc R . . H22C H 0.3637 0.8191 0.7104 0.072 Uiso 1 1 calc R . . C121 C 0.6049(16) 0.4546(15) 0.5552(11) 0.044(3) Uani 1 1 d . . . H12A H 0.6622 0.4131 0.4917 0.065 Uiso 1 1 calc R . . H12B H 0.6852 0.4639 0.6258 0.065 Uiso 1 1 calc R . . H12C H 0.5668 0.5332 0.5263 0.065 Uiso 1 1 calc R . . C25 C 0.3576(14) 0.5249(10) 0.9658(9) 0.031(2) Uani 1 1 d . . . C131 C 0.243(2) 0.4404(19) 0.4012(11) 0.062(4) Uani 1 1 d . . . H13A H 0.3200 0.5090 0.3974 0.092 Uiso 1 1 calc R . . H13B H 0.1264 0.4682 0.4130 0.092 Uiso 1 1 calc R . . H13C H 0.2431 0.3954 0.3260 0.092 Uiso 1 1 calc R . . C241 C 0.0875(18) 0.5927(12) 1.0670(12) 0.044(3) Uani 1 1 d . . . H24A H 0.1327 0.5434 1.1342 0.066 Uiso 1 1 calc R . . H24B H -0.0174 0.5564 1.0303 0.066 Uiso 1 1 calc R . . H24C H 0.0612 0.6725 1.0964 0.066 Uiso 1 1 calc R . . C12 C 0.4517(13) 0.3829(9) 0.5887(10) 0.026(2) Uani 1 1 d . . . C151 C 0.258(2) 0.1111(12) 0.7215(14) 0.047(3) Uani 1 1 d . . . H15A H 0.2603 0.1345 0.8062 0.070 Uiso 1 1 calc R . . H15B H 0.3402 0.0461 0.7122 0.070 Uiso 1 1 calc R . . H15C H 0.1428 0.0844 0.6945 0.070 Uiso 1 1 calc R . . C14 C 0.2202(15) 0.2613(10) 0.5453(11) 0.038(3) Uani 1 1 d . . . C111 C 0.6146(16) 0.2523(12) 0.7531(11) 0.042(3) Uani 1 1 d . . . H11A H 0.6957 0.3190 0.7589 0.062 Uiso 1 1 calc R . . H11B H 0.6692 0.1834 0.7177 0.062 Uiso 1 1 calc R . . H11C H 0.5806 0.2317 0.8334 0.062 Uiso 1 1 calc R . . C21 C 0.4469(14) 0.5605(10) 0.8580(11) 0.035(3) Uani 1 1 d . . . C211 C 0.6429(14) 0.5621(13) 0.8660(16) 0.056(4) Uani 1 1 d . . . H21A H 0.6864 0.4869 0.9005 0.084 Uiso 1 1 calc R . . H21B H 0.6843 0.6283 0.9172 0.084 Uiso 1 1 calc R . . H21C H 0.6837 0.5720 0.7854 0.084 Uiso 1 1 calc R . . C251 C 0.413(2) 0.4212(13) 1.0394(13) 0.052(4) Uiso 1 1 d . . . H25A H 0.5323 0.4323 1.0705 0.077 Uiso 1 1 calc R . . H25B H 0.4044 0.3490 0.9899 0.077 Uiso 1 1 calc R . . H25C H 0.3393 0.4132 1.1066 0.077 Uiso 1 1 calc R . . C141 C 0.0500(17) 0.2122(12) 0.4895(13) 0.045(3) Uiso 1 1 d . . . H14A H -0.0421 0.2693 0.5015 0.067 Uiso 1 1 calc R . . H14B H 0.0240 0.1365 0.5280 0.067 Uiso 1 1 calc R . . H14C H 0.0593 0.1993 0.4033 0.067 Uiso 1 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 Ga01 0.0165(6) 0.0263(6) 0.0205(6) -0.0047(6) 0.0013(3) 0.0004(5) C1 0.017(4) 0.027(7) 0.036(5) -0.013(5) -0.004(3) -0.009(5) C24 0.021(5) 0.033(5) 0.036(6) -0.013(5) -0.007(4) -0.003(4) C22 0.027(5) 0.029(5) 0.032(6) -0.010(4) -0.003(4) -0.008(4) C23 0.023(5) 0.022(5) 0.038(6) -0.011(4) -0.002(4) 0.004(4) C231 0.042(8) 0.051(8) 0.062(9) -0.008(7) -0.005(6) 0.025(6) C15 0.036(6) 0.029(6) 0.037(6) -0.005(5) 0.019(5) 0.009(5) C13 0.042(6) 0.031(5) 0.020(5) -0.010(4) 0.002(4) 0.002(5) C11 0.016(5) 0.034(6) 0.043(6) -0.015(5) 0.000(4) 0.007(4) C221 0.070(10) 0.045(7) 0.029(6) 0.007(5) 0.002(6) -0.013(7) C121 0.043(6) 0.037(6) 0.053(6) -0.006(7) 0.021(5) -0.009(6) C25 0.033(6) 0.036(6) 0.021(5) 0.006(4) -0.011(4) -0.007(5) C131 0.085(11) 0.058(8) 0.042(6) -0.004(9) 0.003(6) 0.044(10) C241 0.048(8) 0.046(7) 0.038(7) -0.008(6) 0.009(5) -0.018(6) C12 0.016(5) 0.031(5) 0.031(5) -0.025(5) 0.007(4) 0.000(4) C151 0.051(8) 0.032(7) 0.060(8) -0.008(6) 0.023(6) -0.005(6) C14 0.028(6) 0.032(6) 0.053(7) -0.022(5) 0.009(5) 0.009(4) C111 0.029(6) 0.056(8) 0.038(6) -0.003(6) -0.012(5) 0.027(6) C21 0.023(5) 0.035(6) 0.046(7) -0.025(5) -0.007(5) 0.009(4) C211 0.008(5) 0.064(9) 0.095(11) -0.047(8) -0.006(6) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga01 C1 1.938(10) . ? Ga01 C21 2.065(11) . ? Ga01 C12 2.170(9) . ? Ga01 C11 2.215(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C24 C23 1.391(16) . ? C24 C25 1.399(17) . ? C24 C241 1.497(17) . ? C22 C23 1.388(16) . ? C22 C21 1.475(17) . ? C22 C221 1.503(16) . ? C23 C231 1.528(15) . ? C231 H23A 0.9800 . ? C231 H23B 0.9800 . ? C231 H23C 0.9800 . ? C15 C14 1.397(18) . ? C15 C11 1.441(17) . ? C15 C151 1.483(17) . ? C13 C14 1.370(17) . ? C13 C12 1.439(15) . ? C13 C131 1.542(19) . ? C11 C12 1.425(17) . ? C11 C111 1.530(14) . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C121 C12 1.510(16) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C25 C251 1.474(18) . ? C25 C21 1.486(18) . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? C241 H24A 0.9800 . ? C241 H24B 0.9800 . ? C241 H24C 0.9800 . ? C151 H15A 0.9800 . ? C151 H15B 0.9800 . ? C151 H15C 0.9800 . ? C14 C141 1.533(19) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C21 C211 1.528(15) . ? C211 H21A 0.9800 . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? C251 H25A 0.9800 . ? C251 H25B 0.9800 . ? C251 H25C 0.9800 . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ga01 C21 119.6(5) . . ? C1 Ga01 C12 121.1(4) . . ? C21 Ga01 C12 116.9(4) . . ? C1 Ga01 C11 116.5(5) . . ? C21 Ga01 C11 119.0(4) . . ? C12 Ga01 C11 37.9(4) . . ? Ga01 C1 H1A 109.5 . . ? Ga01 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Ga01 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C23 C24 C25 108.8(10) . . ? C23 C24 C241 125.8(10) . . ? C25 C24 C241 125.4(11) . . ? C23 C22 C21 106.9(10) . . ? C23 C22 C221 129.4(11) . . ? C21 C22 C221 123.6(11) . . ? C22 C23 C24 111.5(9) . . ? C22 C23 C231 124.3(11) . . ? C24 C23 C231 124.2(11) . . ? C23 C231 H23A 109.5 . . ? C23 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C23 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C14 C15 C11 106.6(10) . . ? C14 C15 C151 128.4(12) . . ? C11 C15 C151 125.0(12) . . ? C14 C13 C12 109.3(10) . . ? C14 C13 C131 125.4(13) . . ? C12 C13 C131 125.0(13) . . ? C12 C11 C15 108.4(9) . . ? C12 C11 C111 124.3(10) . . ? C15 C11 C111 125.2(11) . . ? C12 C11 Ga01 69.3(5) . . ? C15 C11 Ga01 96.6(6) . . ? C111 C11 Ga01 114.0(8) . . ? C22 C221 H22A 109.5 . . ? C22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C12 C121 H12A 109.5 . . ? C12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C24 C25 C251 130.4(11) . . ? C24 C25 C21 107.7(10) . . ? C251 C25 C21 121.9(11) . . ? C13 C131 H13A 109.5 . . ? C13 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C13 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? C24 C241 H24A 109.5 . . ? C24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? C24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C11 C12 C13 105.5(9) . . ? C11 C12 C121 125.5(10) . . ? C13 C12 C121 123.4(10) . . ? C11 C12 Ga01 72.8(6) . . ? C13 C12 Ga01 98.5(6) . . ? C121 C12 Ga01 117.3(7) . . ? C15 C151 H15A 109.5 . . ? C15 C151 H15B 109.5 . . ? H15A C151 H15B 109.5 . . ? C15 C151 H15C 109.5 . . ? H15A C151 H15C 109.5 . . ? H15B C151 H15C 109.5 . . ? C13 C14 C15 110.0(11) . . ? C13 C14 C141 126.0(11) . . ? C15 C14 C141 123.9(11) . . ? C11 C111 H11A 109.5 . . ? C11 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C11 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C22 C21 C25 105.1(9) . . ? C22 C21 C211 118.6(12) . . ? C25 C21 C211 118.5(11) . . ? C22 C21 Ga01 94.6(7) . . ? C25 C21 Ga01 95.9(7) . . ? C211 C21 Ga01 119.5(8) . . ? C21 C211 H21A 109.5 . . ? C21 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C21 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C25 C251 H25A 109.5 . . ? C25 C251 H25B 109.5 . . ? H25A C251 H25B 109.5 . . ? C25 C251 H25C 109.5 . . ? H25A C251 H25C 109.5 . . ? H25B C251 H25C 109.5 . . ? C14 C141 H14A 109.5 . . ? C14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 C22 C23 C24 0.3(11) . . . . ? C221 C22 C23 C24 -178.3(10) . . . . ? C21 C22 C23 C231 -177.0(11) . . . . ? C221 C22 C23 C231 4.4(17) . . . . ? C25 C24 C23 C22 1.7(12) . . . . ? C241 C24 C23 C22 -177.1(10) . . . . ? C25 C24 C23 C231 178.9(11) . . . . ? C241 C24 C23 C231 0.2(16) . . . . ? C14 C15 C11 C12 3.0(11) . . . . ? C151 C15 C11 C12 -175.9(10) . . . . ? C14 C15 C11 C111 -160.9(11) . . . . ? C151 C15 C11 C111 20.2(18) . . . . ? C14 C15 C11 Ga01 73.4(8) . . . . ? C151 C15 C11 Ga01 -105.5(10) . . . . ? C1 Ga01 C11 C12 107.5(7) . . . . ? C21 Ga01 C11 C12 -97.5(7) . . . . ? C1 Ga01 C11 C15 0.3(9) . . . . ? C21 Ga01 C11 C15 155.2(8) . . . . ? C12 Ga01 C11 C15 -107.2(10) . . . . ? C1 Ga01 C11 C111 -133.1(9) . . . . ? C21 Ga01 C11 C111 21.9(11) . . . . ? C12 Ga01 C11 C111 119.4(11) . . . . ? C23 C24 C25 C251 -179.9(11) . . . . ? C241 C24 C25 C251 -1.1(18) . . . . ? C23 C24 C25 C21 -2.9(12) . . . . ? C241 C24 C25 C21 175.9(10) . . . . ? C15 C11 C12 C13 -4.1(11) . . . . ? C111 C11 C12 C13 160.0(10) . . . . ? Ga01 C11 C12 C13 -94.3(7) . . . . ? C15 C11 C12 C121 -158.2(10) . . . . ? C111 C11 C12 C121 6.0(16) . . . . ? Ga01 C11 C12 C121 111.6(10) . . . . ? C15 C11 C12 Ga01 90.2(7) . . . . ? C111 C11 C12 Ga01 -105.7(10) . . . . ? C14 C13 C12 C11 3.7(11) . . . . ? C131 C13 C12 C11 177.5(10) . . . . ? C14 C13 C12 C121 158.5(11) . . . . ? C131 C13 C12 C121 -27.7(16) . . . . ? C14 C13 C12 Ga01 -70.7(9) . . . . ? C131 C13 C12 Ga01 103.2(11) . . . . ? C1 Ga01 C12 C11 -94.1(7) . . . . ? C21 Ga01 C12 C11 103.5(6) . . . . ? C1 Ga01 C12 C13 9.6(10) . . . . ? C21 Ga01 C12 C13 -152.9(7) . . . . ? C11 Ga01 C12 C13 103.7(9) . . . . ? C1 Ga01 C12 C121 144.3(9) . . . . ? C21 Ga01 C12 C121 -18.1(11) . . . . ? C11 Ga01 C12 C121 -121.6(11) . . . . ? C12 C13 C14 C15 -1.9(12) . . . . ? C131 C13 C14 C15 -175.7(10) . . . . ? C12 C13 C14 C141 174.9(11) . . . . ? C131 C13 C14 C141 1.1(18) . . . . ? C11 C15 C14 C13 -0.7(12) . . . . ? C151 C15 C14 C13 178.2(10) . . . . ? C11 C15 C14 C141 -177.6(11) . . . . ? C151 C15 C14 C141 1.3(17) . . . . ? C23 C22 C21 C25 -1.9(11) . . . . ? C221 C22 C21 C25 176.8(9) . . . . ? C23 C22 C21 C211 -137.2(11) . . . . ? C221 C22 C21 C211 41.5(15) . . . . ? C23 C22 C21 Ga01 95.5(8) . . . . ? C221 C22 C21 Ga01 -85.8(10) . . . . ? C24 C25 C21 C22 2.9(11) . . . . ? C251 C25 C21 C22 -179.7(10) . . . . ? C24 C25 C21 C211 138.2(10) . . . . ? C251 C25 C21 C211 -44.5(16) . . . . ? C24 C25 C21 Ga01 -93.5(8) . . . . ? C251 C25 C21 Ga01 83.9(11) . . . . ? C1 Ga01 C21 C22 -60.1(9) . . . . ? C12 Ga01 C21 C22 102.6(8) . . . . ? C11 Ga01 C21 C22 145.7(7) . . . . ? C1 Ga01 C21 C25 45.6(9) . . . . ? C12 Ga01 C21 C25 -151.7(7) . . . . ? C11 Ga01 C21 C25 -108.6(7) . . . . ? C1 Ga01 C21 C211 173.2(11) . . . . ? C12 Ga01 C21 C211 -24.1(13) . . . . ? C11 Ga01 C21 C211 19.0(13) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.347 _refine_diff_density_min -1.385 _refine_diff_density_rms 0.272 # Attachment 'MCpArFAlCl.cif' data_14 _database_code_depnum_ccdc_archive 'CCDC 664849' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 Al2 Cl2 F10' _chemical_formula_sum 'C32 H30 Al2 Cl2 F10' _chemical_formula_weight 729.42 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _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 11.3045(8) _cell_length_b 29.205(3) _cell_length_c 15.4522(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.299(4) _cell_angle_gamma 90.00 _cell_volume 4843.6(7) _cell_formula_units_Z 6 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 73 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 12.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 0.336 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.07 _diffrn_reflns_number 6350 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5253 _reflns_number_gt 3690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5253 _refine_ls_number_parameters 637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 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 C37 C 0.2501(6) 0.5738(3) 0.9629(4) 0.081(2) Uani 1 1 d . . . C41 C 0.4020(10) 0.5940(4) 0.8693(5) 0.217(7) Uani 1 1 d . . . H41A H 0.4886 0.5838 0.8838 0.325 Uiso 1 1 calc R . . H41B H 0.3947 0.6255 0.8463 0.325 Uiso 1 1 calc R . . H41C H 0.3479 0.5739 0.8228 0.325 Uiso 1 1 calc R . . C42 C 0.1472(7) 0.5497(3) 0.8889(5) 0.196(6) Uani 1 1 d . . . H42A H 0.1128 0.5248 0.9161 0.294 Uiso 1 1 calc R . . H42B H 0.1815 0.5371 0.8430 0.294 Uiso 1 1 calc R . . H42C H 0.0810 0.5716 0.8599 0.294 Uiso 1 1 calc R . . C1 C -0.0419(4) 0.83162(19) 0.4828(3) 0.0407(13) Uani 1 1 d . . . C2 C -0.0236(4) 0.8309(2) 0.3971(3) 0.0434(14) Uani 1 1 d . . . C3 C 0.0866(4) 0.80711(18) 0.4046(2) 0.0358(13) Uani 1 1 d . . . C4 C 0.1385(3) 0.79159(17) 0.4969(2) 0.0280(11) Uani 1 1 d . . . C5 C 0.0567(4) 0.80767(17) 0.5448(2) 0.0284(11) Uani 1 1 d . . . C6 C -0.1492(5) 0.8540(2) 0.5041(4) 0.0722(19) Uani 1 1 d . . . H6A H -0.1400 0.8873 0.5033 0.108 Uiso 1 1 calc R . . H6B H -0.1502 0.8442 0.5645 0.108 Uiso 1 1 calc R . . H6C H -0.2275 0.8450 0.4582 0.108 Uiso 1 1 calc R . . C7 C -0.1088(6) 0.8529(2) 0.3114(4) 0.089(3) Uani 1 1 d . . . H7A H -0.1956 0.8492 0.3098 0.134 Uiso 1 1 calc R . . H7B H -0.0969 0.8381 0.2579 0.134 Uiso 1 1 calc R . . H7C H -0.0891 0.8855 0.3111 0.134 Uiso 1 1 calc R . . C8 C 0.1475(5) 0.8015(2) 0.3313(3) 0.074(2) Uani 1 1 d . . . H8A H 0.2015 0.8279 0.3322 0.110 Uiso 1 1 calc R . . H8B H 0.0831 0.7996 0.2717 0.110 Uiso 1 1 calc R . . H8C H 0.1974 0.7734 0.3424 0.110 Uiso 1 1 calc R . . C9 C 0.2621(4) 0.7687(2) 0.5369(3) 0.0502(15) Uani 1 1 d . . . H9A H 0.2749 0.7464 0.4932 0.075 Uiso 1 1 calc R . . H9B H 0.2638 0.7529 0.5932 0.075 Uiso 1 1 calc R . . H9C H 0.3284 0.7917 0.5504 0.075 Uiso 1 1 calc R . . C10 C 0.0750(5) 0.8012(2) 0.6450(3) 0.0519(16) Uani 1 1 d . . . H10A H 0.1001 0.8303 0.6770 0.078 Uiso 1 1 calc R . . H10B H 0.1401 0.7782 0.6700 0.078 Uiso 1 1 calc R . . H10C H -0.0032 0.7908 0.6532 0.078 Uiso 1 1 calc R . . C11 C -0.2124(3) 0.75068(16) 0.3908(2) 0.0250(11) Uani 1 1 d . . . C12 C -0.2898(4) 0.74982(17) 0.4440(2) 0.0303(12) Uani 1 1 d . . . C13 C -0.4181(4) 0.74841(19) 0.4093(3) 0.0384(13) Uani 1 1 d . . . C14 C -0.4733(4) 0.74796(19) 0.3166(3) 0.0422(14) Uani 1 1 d . . . C15 C -0.4002(4) 0.74843(18) 0.2604(3) 0.0382(13) Uani 1 1 d . . . C16 C -0.2735(3) 0.75004(17) 0.2980(2) 0.0290(11) Uani 1 1 d . . . C17 C -0.0384(4) 0.58581(18) 0.3650(3) 0.0360(13) Uani 1 1 d . . . C18 C -0.1120(4) 0.60307(18) 0.4173(3) 0.0337(12) Uani 1 1 d . . . C19 C -0.0563(4) 0.58778(19) 0.5091(3) 0.0361(13) Uani 1 1 d . . . C20 C 0.0504(4) 0.56249(19) 0.5134(3) 0.0381(13) Uani 1 1 d . . . C21 C 0.0616(4) 0.56067(18) 0.4241(3) 0.0352(13) Uani 1 1 d . . . C22 C -0.0676(5) 0.5907(2) 0.2629(3) 0.0586(17) Uani 1 1 d . . . H22A H 0.0103 0.5923 0.2478 0.088 Uiso 1 1 calc R . . H22B H -0.1156 0.6188 0.2424 0.088 Uiso 1 1 calc R . . H22C H -0.1164 0.5643 0.2323 0.088 Uiso 1 1 calc R . . C23 C -0.2338(4) 0.6289(2) 0.3822(3) 0.0553(16) Uani 1 1 d . . . H23A H -0.3034 0.6073 0.3713 0.083 Uiso 1 1 calc R . . H23B H -0.2379 0.6444 0.3251 0.083 Uiso 1 1 calc R . . H23C H -0.2389 0.6516 0.4275 0.083 Uiso 1 1 calc R . . C24 C -0.1108(5) 0.5957(2) 0.5855(3) 0.0635(18) Uani 1 1 d . . . H24A H -0.1768 0.5732 0.5812 0.095 Uiso 1 1 calc R . . H24B H -0.1457 0.6266 0.5806 0.095 Uiso 1 1 calc R . . H24C H -0.0453 0.5923 0.6443 0.095 Uiso 1 1 calc R . . C25 C 0.1381(5) 0.5398(2) 0.5965(3) 0.0609(17) Uani 1 1 d . . . H25A H 0.1206 0.5508 0.6511 0.091 Uiso 1 1 calc R . . H25B H 0.2243 0.5474 0.6008 0.091 Uiso 1 1 calc R . . H25C H 0.1266 0.5066 0.5915 0.091 Uiso 1 1 calc R . . C26 C 0.1621(5) 0.5361(2) 0.3987(4) 0.0592(16) Uani 1 1 d . . . H26A H 0.1561 0.5031 0.4087 0.089 Uiso 1 1 calc R . . H26B H 0.2437 0.5473 0.4364 0.089 Uiso 1 1 calc R . . H26C H 0.1523 0.5417 0.3343 0.089 Uiso 1 1 calc R . . C27 C 0.2432(3) 0.64127(16) 0.5119(2) 0.0262(11) Uani 1 1 d . . . C28 C 0.3126(4) 0.64424(17) 0.6026(2) 0.0290(11) Uani 1 1 d . . . C29 C 0.4403(4) 0.64723(18) 0.6337(3) 0.0369(13) Uani 1 1 d . . . C30 C 0.5046(4) 0.6476(2) 0.5719(3) 0.0445(14) Uani 1 1 d . . . C31 C 0.4414(4) 0.64480(19) 0.4811(3) 0.0393(13) Uani 1 1 d . . . C32 C 0.3130(4) 0.64171(17) 0.4528(3) 0.0313(12) Uani 1 1 d . . . Al1 Al 0.05836(10) 0.63901(5) 0.46619(7) 0.0258(3) Uani 1 1 d . . . Al2 Al -0.02814(10) 0.75412(5) 0.44287(7) 0.0241(3) Uani 1 1 d . . . Cl1 Cl 0.00894(8) 0.69628(4) 0.55489(6) 0.0274(3) Uani 1 1 d . . . Cl2 Cl 0.02559(8) 0.69705(4) 0.35579(6) 0.0283(3) Uani 1 1 d . . . F1 F 0.2533(2) 0.64389(10) 0.66654(14) 0.0426(8) Uani 1 1 d . . . F2 F 0.5029(2) 0.65001(12) 0.72343(16) 0.0601(10) Uani 1 1 d . . . F3 F 0.6298(2) 0.65164(13) 0.6005(2) 0.0720(11) Uani 1 1 d . . . F4 F 0.5038(2) 0.64471(12) 0.41957(18) 0.0628(10) Uani 1 1 d . . . F5 F 0.2560(2) 0.63829(10) 0.36170(14) 0.0442(8) Uani 1 1 d . . . F6 F -0.2404(2) 0.75078(10) 0.53609(14) 0.0437(8) Uani 1 1 d . . . F7 F -0.4891(2) 0.74741(11) 0.46485(17) 0.0559(9) Uani 1 1 d . . . F8 F -0.5986(2) 0.74632(12) 0.28139(19) 0.0687(10) Uani 1 1 d . . . F9 F -0.4551(2) 0.74833(11) 0.16937(15) 0.0572(9) Uani 1 1 d . . . F10 F -0.2064(2) 0.75129(10) 0.23926(14) 0.0429(7) Uani 1 1 d . . . C33 C 0.2475(4) 0.5836(2) 1.0508(3) 0.0485(15) Uani 1 1 d . . . C34 C 0.3545(5) 0.6079(2) 1.0953(3) 0.0427(14) Uani 1 1 d . . . C35 C 0.4267(5) 0.6129(2) 1.0378(4) 0.0602(18) Uani 1 1 d . . . C36 C 0.3631(8) 0.5922(3) 0.9546(4) 0.085(3) Uani 1 1 d . . . C38 C 0.1460(5) 0.5697(3) 1.0902(5) 0.105(3) Uani 1 1 d . . . H38A H 0.1836 0.5608 1.1542 0.158 Uiso 1 1 calc R . . H38B H 0.0993 0.5438 1.0556 0.158 Uiso 1 1 calc R . . H38C H 0.0895 0.5956 1.0865 0.158 Uiso 1 1 calc R . . C39 C 0.3880(6) 0.6253(2) 1.1919(3) 0.082(2) Uani 1 1 d . . . H39A H 0.3402 0.6532 1.1933 0.123 Uiso 1 1 calc R . . H39B H 0.4773 0.6323 1.2145 0.123 Uiso 1 1 calc R . . H39C H 0.3683 0.6019 1.2306 0.123 Uiso 1 1 calc R . . C40 C 0.5485(7) 0.6391(3) 1.0587(6) 0.141(4) Uani 1 1 d . . . H40A H 0.5966 0.6352 1.1231 0.211 Uiso 1 1 calc R . . H40B H 0.5308 0.6717 1.0459 0.211 Uiso 1 1 calc R . . H40C H 0.5966 0.6274 1.0206 0.211 Uiso 1 1 calc R . . C43 C 0.4339(4) 0.50970(17) 1.1681(3) 0.0310(12) Uani 1 1 d . . . C44 C 0.3473(4) 0.48069(19) 1.1829(3) 0.0398(13) Uani 1 1 d . . . C45 C 0.3511(5) 0.4650(2) 1.2686(3) 0.0541(16) Uani 1 1 d . . . C46 C 0.4447(6) 0.4792(2) 1.3431(3) 0.0556(17) Uani 1 1 d . . . C47 C 0.5332(4) 0.5084(2) 1.3325(3) 0.0430(14) Uani 1 1 d . . . C48 C 0.5262(4) 0.52254(18) 1.2458(3) 0.0362(13) Uani 1 1 d . . . Al3 Al 0.41840(12) 0.53756(5) 1.04764(8) 0.0320(4) Uani 1 1 d . . . Cl3 Cl 0.37606(9) 0.47224(5) 0.95552(7) 0.0377(3) Uani 1 1 d . . . F11 F 0.2496(2) 0.46611(12) 1.11190(17) 0.0574(9) Uani 1 1 d . . . F12 F 0.2630(4) 0.43678(14) 1.2790(2) 0.0952(14) Uani 1 1 d . . . F13 F 0.4508(4) 0.46435(13) 1.42654(17) 0.0860(13) Uani 1 1 d . . . F14 F 0.6252(3) 0.52365(12) 1.40635(16) 0.0654(10) Uani 1 1 d . . . F15 F 0.6166(2) 0.55160(11) 1.23933(15) 0.0486(8) 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 C37 0.085(5) 0.062(6) 0.063(4) -0.020(3) -0.023(4) 0.049(4) C41 0.413(16) 0.198(13) 0.118(6) 0.128(7) 0.196(9) 0.243(12) C42 0.143(8) 0.169(13) 0.168(8) -0.096(7) -0.106(6) 0.113(8) C1 0.035(3) 0.028(5) 0.059(3) -0.007(2) 0.015(2) -0.003(2) C2 0.050(3) 0.032(5) 0.037(3) 0.011(2) -0.004(2) -0.008(3) C3 0.047(3) 0.036(4) 0.027(2) -0.003(2) 0.017(2) -0.015(2) C4 0.023(2) 0.028(4) 0.032(2) -0.0026(19) 0.0083(18) -0.006(2) C5 0.035(2) 0.025(4) 0.027(2) -0.0030(19) 0.0119(19) -0.007(2) C6 0.047(3) 0.043(6) 0.128(5) -0.020(4) 0.029(3) 0.008(3) C7 0.098(5) 0.050(6) 0.079(4) 0.041(3) -0.031(3) -0.022(4) C8 0.114(5) 0.071(6) 0.062(3) -0.024(3) 0.065(3) -0.053(4) C9 0.027(3) 0.044(5) 0.074(3) -0.011(3) 0.009(2) -0.008(2) C10 0.081(4) 0.047(5) 0.032(3) -0.014(2) 0.024(2) -0.023(3) C11 0.024(2) 0.020(4) 0.030(2) 0.0044(18) 0.0078(18) 0.0031(19) C12 0.031(2) 0.029(4) 0.030(2) -0.0040(19) 0.0081(19) 0.004(2) C13 0.029(2) 0.037(4) 0.054(3) -0.006(2) 0.020(2) -0.002(2) C14 0.020(2) 0.047(5) 0.053(3) -0.008(2) 0.002(2) -0.001(2) C15 0.034(3) 0.037(4) 0.035(3) -0.004(2) -0.002(2) 0.005(2) C16 0.026(2) 0.029(4) 0.031(2) -0.0019(19) 0.0070(19) 0.002(2) C17 0.042(3) 0.036(4) 0.033(2) -0.006(2) 0.015(2) -0.013(2) C18 0.027(2) 0.031(4) 0.046(3) -0.005(2) 0.016(2) -0.007(2) C19 0.048(3) 0.023(4) 0.046(3) -0.006(2) 0.028(2) -0.012(2) C20 0.043(3) 0.030(4) 0.040(3) 0.002(2) 0.011(2) -0.009(2) C21 0.033(3) 0.024(4) 0.052(3) -0.007(2) 0.019(2) -0.003(2) C22 0.079(4) 0.061(5) 0.033(3) -0.014(2) 0.014(2) -0.018(3) C23 0.032(3) 0.045(5) 0.083(4) -0.008(3) 0.009(3) -0.006(3) C24 0.100(4) 0.044(5) 0.073(4) -0.008(3) 0.065(3) -0.023(3) C25 0.074(4) 0.041(5) 0.062(3) 0.013(3) 0.012(3) -0.004(3) C26 0.065(4) 0.034(5) 0.092(4) -0.011(3) 0.044(3) 0.003(3) C27 0.028(2) 0.020(4) 0.034(2) 0.0036(18) 0.0149(19) 0.0004(19) C28 0.033(2) 0.027(4) 0.028(2) 0.0024(19) 0.012(2) 0.000(2) C29 0.029(2) 0.035(4) 0.038(3) 0.001(2) -0.002(2) -0.001(2) C30 0.026(3) 0.039(5) 0.066(3) 0.005(2) 0.011(2) 0.000(2) C31 0.035(3) 0.037(4) 0.055(3) 0.003(2) 0.027(2) 0.000(2) C32 0.031(2) 0.029(4) 0.034(2) 0.0016(19) 0.010(2) 0.003(2) Al1 0.0255(7) 0.0287(11) 0.0245(6) -0.0004(5) 0.0099(5) -0.0035(6) Al2 0.0213(6) 0.0289(10) 0.0217(6) 0.0013(5) 0.0063(5) -0.0025(6) Cl1 0.0322(6) 0.0303(9) 0.0219(5) 0.0003(4) 0.0117(4) -0.0011(5) Cl2 0.0318(6) 0.0336(9) 0.0216(5) 0.0010(4) 0.0114(4) 0.0000(5) F1 0.0403(14) 0.059(3) 0.0296(13) 0.0065(12) 0.0120(11) -0.0004(13) F2 0.0435(16) 0.077(3) 0.0431(16) 0.0053(14) -0.0103(13) -0.0052(16) F3 0.0225(15) 0.094(4) 0.094(2) 0.0029(18) 0.0097(14) -0.0024(15) F4 0.0419(16) 0.086(3) 0.0767(19) 0.0017(17) 0.0413(15) 0.0027(16) F5 0.0419(15) 0.062(3) 0.0334(14) -0.0022(12) 0.0190(11) 0.0055(14) F6 0.0413(14) 0.061(3) 0.0327(13) -0.0025(12) 0.0175(11) 0.0051(14) F7 0.0380(15) 0.071(3) 0.0720(18) -0.0111(15) 0.0359(14) -0.0035(14) F8 0.0199(14) 0.096(3) 0.081(2) -0.0214(18) 0.0025(13) -0.0011(15) F9 0.0388(15) 0.081(3) 0.0362(14) -0.0071(14) -0.0105(12) 0.0059(15) F10 0.0380(14) 0.064(2) 0.0264(12) 0.0065(12) 0.0099(11) 0.0068(14) C33 0.039(3) 0.032(5) 0.076(4) 0.010(3) 0.020(3) 0.018(3) C34 0.056(3) 0.031(5) 0.048(3) 0.002(2) 0.026(3) 0.013(3) C35 0.076(4) 0.021(5) 0.108(5) 0.023(3) 0.065(4) 0.022(3) C36 0.146(7) 0.076(7) 0.049(4) 0.036(3) 0.053(4) 0.080(5) C38 0.068(4) 0.057(8) 0.217(8) 0.012(5) 0.083(5) 0.014(4) C39 0.113(5) 0.067(7) 0.062(4) -0.016(3) 0.023(4) 0.035(4) C40 0.123(7) 0.029(9) 0.326(12) 0.030(6) 0.150(8) 0.004(5) C43 0.042(3) 0.026(4) 0.032(2) -0.0028(19) 0.020(2) 0.001(2) C44 0.056(3) 0.029(4) 0.038(3) -0.009(2) 0.021(2) -0.007(3) C45 0.090(4) 0.036(5) 0.055(3) -0.009(3) 0.050(3) -0.022(3) C46 0.105(4) 0.043(5) 0.030(3) 0.002(2) 0.037(3) 0.002(3) C47 0.059(3) 0.039(5) 0.031(3) 0.001(2) 0.013(2) 0.010(3) C48 0.041(3) 0.035(4) 0.036(3) 0.000(2) 0.018(2) 0.000(2) Al3 0.0395(8) 0.0293(11) 0.0290(7) 0.0031(6) 0.0135(6) 0.0069(6) Cl3 0.0387(6) 0.0401(10) 0.0366(6) -0.0062(5) 0.0149(5) -0.0006(5) F11 0.0610(18) 0.063(3) 0.0568(17) -0.0210(15) 0.0311(15) -0.0254(16) F12 0.154(3) 0.081(4) 0.081(2) -0.0212(19) 0.081(2) -0.068(3) F13 0.166(3) 0.063(4) 0.0428(17) 0.0071(15) 0.053(2) -0.017(2) F14 0.081(2) 0.076(3) 0.0325(15) -0.0049(14) 0.0081(15) 0.0061(19) F15 0.0483(16) 0.057(3) 0.0413(14) -0.0077(12) 0.0149(12) -0.0142(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C37 C33 1.398(7) . ? C37 C36 1.428(10) . ? C37 C42 1.524(9) . ? C37 Al3 2.212(6) . ? C41 C36 1.516(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C1 C2 1.404(6) . ? C1 C5 1.408(6) . ? C1 C6 1.502(6) . ? C1 Al2 2.364(6) . ? C2 C3 1.399(7) . ? C2 C7 1.513(6) . ? C2 Al2 2.358(6) . ? C3 C4 1.434(5) . ? C3 C8 1.508(6) . ? C3 Al2 2.215(5) . ? C4 C5 1.433(5) . ? C4 C9 1.496(6) . ? C4 Al2 2.111(4) . ? C5 C10 1.508(5) . ? C5 Al2 2.214(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.375(5) . ? C11 C16 1.383(5) . ? C11 Al2 1.986(4) . ? C12 F6 1.356(4) . ? C12 C13 1.380(6) . ? C13 F7 1.347(4) . ? C13 C14 1.371(6) . ? C14 F8 1.349(4) . ? C14 C15 1.374(6) . ? C15 F9 1.347(4) . ? C15 C16 1.367(5) . ? C16 F10 1.354(4) . ? C17 C21 1.415(6) . ? C17 C18 1.422(6) . ? C17 C22 1.514(5) . ? C17 Al1 2.232(5) . ? C18 C19 1.432(6) . ? C18 C23 1.512(6) . ? C18 Al1 2.114(4) . ? C19 C20 1.399(6) . ? C19 C24 1.511(6) . ? C19 Al1 2.214(5) . ? C20 C21 1.425(5) . ? C20 C25 1.507(6) . ? C20 Al1 2.361(5) . ? C21 C26 1.498(6) . ? C21 Al1 2.382(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.377(5) . ? C27 C32 1.382(5) . ? C27 Al1 1.985(4) . ? C28 F1 1.357(4) . ? C28 C29 1.373(5) . ? C29 F2 1.347(4) . ? C29 C30 1.370(6) . ? C30 F3 1.349(5) . ? C30 C31 1.362(6) . ? C31 F4 1.351(4) . ? C31 C32 1.381(6) . ? C32 F5 1.356(4) . ? Al1 Cl1 2.3385(16) . ? Al1 Cl2 2.3501(17) . ? Al2 Cl2 2.3390(16) . ? Al2 Cl1 2.3601(16) . ? C33 C34 1.385(7) . ? C33 C38 1.513(7) . ? C33 Al3 2.366(5) . ? C34 C35 1.390(6) . ? C34 C39 1.508(6) . ? C34 Al3 2.371(5) . ? C35 C36 1.398(9) . ? C35 C40 1.519(9) . ? C35 Al3 2.210(6) . ? C36 Al3 2.107(6) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C43 C44 1.367(6) . ? C43 C48 1.373(6) . ? C43 Al3 1.989(4) . ? C44 F11 1.357(5) . ? C44 C45 1.390(6) . ? C45 F12 1.339(6) . ? C45 C46 1.362(7) . ? C46 F13 1.341(5) . ? C46 C47 1.363(7) . ? C47 F14 1.355(5) . ? C47 C48 1.379(6) . ? C48 F15 1.356(5) . ? Al3 Cl3 2.3380(18) . ? Al3 Cl3 2.3567(16) 3_667 ? Cl3 Al3 2.3567(16) 3_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C33 C37 C36 107.6(5) . . ? C33 C37 C42 125.4(8) . . ? C36 C37 C42 127.0(8) . . ? C33 C37 Al3 78.4(3) . . ? C36 C37 Al3 66.8(3) . . ? C42 C37 Al3 122.3(5) . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C2 C1 C5 108.4(4) . . ? C2 C1 C6 125.5(5) . . ? C5 C1 C6 126.1(4) . . ? C2 C1 Al2 72.5(3) . . ? C5 C1 Al2 66.3(3) . . ? C6 C1 Al2 126.7(4) . . ? C3 C2 C1 108.6(4) . . ? C3 C2 C7 126.1(5) . . ? C1 C2 C7 125.3(5) . . ? C3 C2 Al2 66.7(3) . . ? C1 C2 Al2 72.9(3) . . ? C7 C2 Al2 126.7(4) . . ? C2 C3 C4 108.4(4) . . ? C2 C3 C8 126.5(4) . . ? C4 C3 C8 124.9(5) . . ? C2 C3 Al2 77.8(3) . . ? C4 C3 Al2 66.8(2) . . ? C8 C3 Al2 124.6(4) . . ? C5 C4 C3 106.3(4) . . ? C5 C4 C9 127.1(4) . . ? C3 C4 C9 126.2(4) . . ? C5 C4 Al2 74.6(2) . . ? C3 C4 Al2 74.6(2) . . ? C9 C4 Al2 122.2(4) . . ? C1 C5 C4 108.2(3) . . ? C1 C5 C10 125.8(4) . . ? C4 C5 C10 125.9(4) . . ? C1 C5 Al2 78.0(3) . . ? C4 C5 Al2 66.8(2) . . ? C10 C5 Al2 122.1(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 114.5(3) . . ? C12 C11 Al2 122.8(3) . . ? C16 C11 Al2 122.6(3) . . ? F6 C12 C11 119.8(3) . . ? F6 C12 C13 116.4(3) . . ? C11 C12 C13 123.8(4) . . ? F7 C13 C14 119.9(4) . . ? F7 C13 C12 121.1(4) . . ? C14 C13 C12 119.0(4) . . ? F8 C14 C13 119.8(4) . . ? F8 C14 C15 120.6(4) . . ? C13 C14 C15 119.6(4) . . ? F9 C15 C16 121.4(4) . . ? F9 C15 C14 119.3(4) . . ? C16 C15 C14 119.3(4) . . ? F10 C16 C15 116.6(3) . . ? F10 C16 C11 119.5(3) . . ? C15 C16 C11 123.9(4) . . ? C21 C17 C18 108.0(4) . . ? C21 C17 C22 126.2(4) . . ? C18 C17 C22 125.7(4) . . ? C21 C17 Al1 78.0(3) . . ? C18 C17 Al1 66.5(2) . . ? C22 C17 Al1 124.2(3) . . ? C17 C18 C19 107.4(4) . . ? C17 C18 C23 127.1(4) . . ? C19 C18 C23 125.3(4) . . ? C17 C18 Al1 75.5(2) . . ? C19 C18 Al1 74.5(2) . . ? C23 C18 Al1 120.3(4) . . ? C20 C19 C18 108.4(4) . . ? C20 C19 C24 127.0(4) . . ? C18 C19 C24 124.5(4) . . ? C20 C19 Al1 78.1(3) . . ? C18 C19 Al1 67.0(2) . . ? C24 C19 Al1 123.5(4) . . ? C19 C20 C21 108.2(4) . . ? C19 C20 C25 126.8(4) . . ? C21 C20 C25 125.0(5) . . ? C19 C20 Al1 66.5(3) . . ? C21 C20 Al1 73.3(3) . . ? C25 C20 Al1 126.9(4) . . ? C17 C21 C20 108.1(4) . . ? C17 C21 C26 126.7(4) . . ? C20 C21 C26 125.2(4) . . ? C17 C21 Al1 66.4(3) . . ? C20 C21 Al1 71.7(3) . . ? C26 C21 Al1 127.6(3) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 114.2(4) . . ? C28 C27 Al1 124.3(3) . . ? C32 C27 Al1 121.4(3) . . ? F1 C28 C29 116.8(3) . . ? F1 C28 C27 119.1(3) . . ? C29 C28 C27 124.1(4) . . ? F2 C29 C30 119.6(4) . . ? F2 C29 C28 121.3(4) . . ? C30 C29 C28 119.1(4) . . ? F3 C30 C31 120.0(4) . . ? F3 C30 C29 120.3(4) . . ? C31 C30 C29 119.7(4) . . ? F4 C31 C30 120.3(4) . . ? F4 C31 C32 120.4(4) . . ? C30 C31 C32 119.3(4) . . ? F5 C32 C31 116.3(3) . . ? F5 C32 C27 120.1(3) . . ? C31 C32 C27 123.6(4) . . ? C27 Al1 C18 152.0(2) . . ? C27 Al1 C19 124.45(19) . . ? C18 Al1 C19 38.55(16) . . ? C27 Al1 C17 120.12(18) . . ? C18 Al1 C17 38.08(16) . . ? C19 Al1 C17 62.30(16) . . ? C27 Al1 Cl1 100.73(14) . . ? C18 Al1 Cl1 101.90(13) . . ? C19 Al1 Cl1 92.16(13) . . ? C17 Al1 Cl1 138.92(13) . . ? C27 Al1 Cl2 98.21(13) . . ? C18 Al1 Cl2 100.38(13) . . ? C19 Al1 Cl2 137.00(13) . . ? C17 Al1 Cl2 93.59(13) . . ? Cl1 Al1 Cl2 84.11(6) . . ? C27 Al1 C20 93.40(18) . . ? C18 Al1 C20 61.44(17) . . ? C19 Al1 C20 35.42(16) . . ? C17 Al1 C20 59.98(16) . . ? Cl1 Al1 C20 117.18(12) . . ? Cl2 Al1 C20 153.40(12) . . ? C27 Al1 C21 91.40(17) . . ? C18 Al1 C21 61.04(17) . . ? C19 Al1 C21 59.54(16) . . ? C17 Al1 C21 35.53(16) . . ? Cl1 Al1 C21 150.92(12) . . ? Cl2 Al1 C21 120.46(11) . . ? C20 Al1 C21 34.96(14) . . ? C11 Al2 C4 151.5(2) . . ? C11 Al2 C5 119.28(17) . . ? C4 Al2 C5 38.62(15) . . ? C11 Al2 C3 123.71(18) . . ? C4 Al2 C3 38.62(15) . . ? C5 Al2 C3 62.42(15) . . ? C11 Al2 Cl2 99.20(13) . . ? C4 Al2 Cl2 103.66(13) . . ? C5 Al2 Cl2 141.27(12) . . ? C3 Al2 Cl2 93.73(13) . . ? C11 Al2 C2 92.62(18) . . ? C4 Al2 C2 61.62(17) . . ? C5 Al2 C2 59.74(16) . . ? C3 Al2 C2 35.46(17) . . ? Cl2 Al2 C2 118.13(13) . . ? C11 Al2 Cl1 100.53(13) . . ? C4 Al2 Cl1 98.63(12) . . ? C5 Al2 Cl1 92.64(12) . . ? C3 Al2 Cl1 135.36(13) . . ? Cl2 Al2 Cl1 83.88(6) . . ? C2 Al2 Cl1 152.32(12) . . ? C11 Al2 C1 90.42(17) . . ? C4 Al2 C1 61.60(17) . . ? C5 Al2 C1 35.63(15) . . ? C3 Al2 C1 59.52(17) . . ? Cl2 Al2 C1 151.98(12) . . ? C2 Al2 C1 34.58(16) . . ? Cl1 Al2 C1 120.33(12) . . ? Al1 Cl1 Al2 95.86(5) . . ? Al2 Cl2 Al1 96.12(5) . . ? C34 C33 C37 107.8(5) . . ? C34 C33 C38 126.3(5) . . ? C37 C33 C38 125.9(6) . . ? C34 C33 Al3 73.2(3) . . ? C37 C33 Al3 66.3(3) . . ? C38 C33 Al3 125.7(4) . . ? C33 C34 C35 109.4(5) . . ? C33 C34 C39 125.0(5) . . ? C35 C34 C39 125.6(6) . . ? C33 C34 Al3 72.8(3) . . ? C35 C34 Al3 66.1(3) . . ? C39 C34 Al3 126.4(4) . . ? C34 C35 C36 107.9(6) . . ? C34 C35 C40 126.3(7) . . ? C36 C35 C40 125.7(6) . . ? C34 C35 Al3 78.8(3) . . ? C36 C35 Al3 67.2(4) . . ? C40 C35 Al3 122.9(4) . . ? C35 C36 C37 107.3(5) . . ? C35 C36 C41 125.4(9) . . ? C37 C36 C41 127.0(8) . . ? C35 C36 Al3 75.1(3) . . ? C37 C36 Al3 74.7(4) . . ? C41 C36 Al3 121.0(4) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C44 C43 C48 114.3(4) . . ? C44 C43 Al3 123.5(3) . . ? C48 C43 Al3 121.8(4) . . ? F11 C44 C43 120.2(4) . . ? F11 C44 C45 116.1(4) . . ? C43 C44 C45 123.6(4) . . ? F12 C45 C46 119.7(4) . . ? F12 C45 C44 121.0(5) . . ? C46 C45 C44 119.2(5) . . ? F13 C46 C45 120.4(5) . . ? F13 C46 C47 120.0(5) . . ? C45 C46 C47 119.6(4) . . ? F14 C47 C46 120.1(4) . . ? F14 C47 C48 120.9(5) . . ? C46 C47 C48 118.9(4) . . ? F15 C48 C43 119.3(4) . . ? F15 C48 C47 116.4(4) . . ? C43 C48 C47 124.3(5) . . ? C43 Al3 C36 150.3(2) . . ? C43 Al3 C35 118.6(2) . . ? C36 Al3 C35 37.7(3) . . ? C43 Al3 C37 123.9(3) . . ? C36 Al3 C37 38.5(3) . . ? C35 Al3 C37 61.9(3) . . ? C43 Al3 Cl3 100.21(15) . . ? C36 Al3 Cl3 104.1(2) . . ? C35 Al3 Cl3 140.87(18) . . ? C37 Al3 Cl3 93.24(17) . . ? C43 Al3 Cl3 99.91(13) . 3_667 ? C36 Al3 Cl3 99.3(2) . 3_667 ? C35 Al3 Cl3 93.21(15) . 3_667 ? C37 Al3 Cl3 135.7(2) . 3_667 ? Cl3 Al3 Cl3 84.44(6) . 3_667 ? C43 Al3 C33 92.61(18) . . ? C36 Al3 C33 61.0(2) . . ? C35 Al3 C33 59.2(2) . . ? C37 Al3 C33 35.36(19) . . ? Cl3 Al3 C33 117.63(15) . . ? Cl3 Al3 C33 152.36(16) 3_667 . ? C43 Al3 C34 90.55(18) . . ? C36 Al3 C34 60.1(2) . . ? C35 Al3 C34 35.10(17) . . ? C37 Al3 C34 58.65(19) . . ? Cl3 Al3 C34 150.72(14) . . ? Cl3 Al3 C34 120.67(14) 3_667 . ? C33 Al3 C34 34.00(17) . . ? Al3 Cl3 Al3 95.56(6) . 3_667 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -0.6(6) . . . . ? C6 C1 C2 C3 179.7(5) . . . . ? Al2 C1 C2 C3 -57.3(4) . . . . ? C5 C1 C2 C7 -180.0(5) . . . . ? C6 C1 C2 C7 0.3(9) . . . . ? Al2 C1 C2 C7 123.3(5) . . . . ? C5 C1 C2 Al2 56.7(4) . . . . ? C6 C1 C2 Al2 -123.0(5) . . . . ? C1 C2 C3 C4 1.0(5) . . . . ? C7 C2 C3 C4 -179.6(5) . . . . ? Al2 C2 C3 C4 -60.2(3) . . . . ? C1 C2 C3 C8 -174.5(5) . . . . ? C7 C2 C3 C8 4.9(9) . . . . ? Al2 C2 C3 C8 124.3(5) . . . . ? C1 C2 C3 Al2 61.2(4) . . . . ? C7 C2 C3 Al2 -119.4(5) . . . . ? C2 C3 C4 C5 -1.0(5) . . . . ? C8 C3 C4 C5 174.6(5) . . . . ? Al2 C3 C4 C5 -68.4(3) . . . . ? C2 C3 C4 C9 -173.7(5) . . . . ? C8 C3 C4 C9 1.9(8) . . . . ? Al2 C3 C4 C9 118.9(5) . . . . ? C2 C3 C4 Al2 67.4(4) . . . . ? C8 C3 C4 Al2 -117.0(5) . . . . ? C2 C1 C5 C4 -0.1(6) . . . . ? C6 C1 C5 C4 179.6(5) . . . . ? Al2 C1 C5 C4 60.4(3) . . . . ? C2 C1 C5 C10 178.4(4) . . . . ? C6 C1 C5 C10 -1.9(8) . . . . ? Al2 C1 C5 C10 -121.1(5) . . . . ? C2 C1 C5 Al2 -60.5(4) . . . . ? C6 C1 C5 Al2 119.2(5) . . . . ? C3 C4 C5 C1 0.7(5) . . . . ? C9 C4 C5 C1 173.3(5) . . . . ? Al2 C4 C5 C1 -67.8(4) . . . . ? C3 C4 C5 C10 -177.8(4) . . . . ? C9 C4 C5 C10 -5.2(8) . . . . ? Al2 C4 C5 C10 113.8(4) . . . . ? C3 C4 C5 Al2 68.4(3) . . . . ? C9 C4 C5 Al2 -119.0(5) . . . . ? C16 C11 C12 F6 -179.4(4) . . . . ? Al2 C11 C12 F6 -0.8(6) . . . . ? C16 C11 C12 C13 0.0(7) . . . . ? Al2 C11 C12 C13 178.6(4) . . . . ? F6 C12 C13 F7 -0.9(7) . . . . ? C11 C12 C13 F7 179.7(5) . . . . ? F6 C12 C13 C14 179.2(4) . . . . ? C11 C12 C13 C14 -0.2(8) . . . . ? F7 C13 C14 F8 -0.2(7) . . . . ? C12 C13 C14 F8 179.6(5) . . . . ? F7 C13 C14 C15 -179.2(5) . . . . ? C12 C13 C14 C15 0.6(8) . . . . ? F8 C14 C15 F9 1.5(8) . . . . ? C13 C14 C15 F9 -179.5(4) . . . . ? F8 C14 C15 C16 -179.9(5) . . . . ? C13 C14 C15 C16 -0.9(8) . . . . ? F9 C15 C16 F10 -0.3(7) . . . . ? C14 C15 C16 F10 -178.8(5) . . . . ? F9 C15 C16 C11 179.3(4) . . . . ? C14 C15 C16 C11 0.8(8) . . . . ? C12 C11 C16 F10 179.3(4) . . . . ? Al2 C11 C16 F10 0.7(6) . . . . ? C12 C11 C16 C15 -0.3(7) . . . . ? Al2 C11 C16 C15 -178.9(4) . . . . ? C21 C17 C18 C19 -0.5(5) . . . . ? C22 C17 C18 C19 175.5(4) . . . . ? Al1 C17 C18 C19 -68.2(3) . . . . ? C21 C17 C18 C23 -175.0(5) . . . . ? C22 C17 C18 C23 1.0(8) . . . . ? Al1 C17 C18 C23 117.3(5) . . . . ? C21 C17 C18 Al1 67.7(4) . . . . ? C22 C17 C18 Al1 -116.3(5) . . . . ? C17 C18 C19 C20 1.1(5) . . . . ? C23 C18 C19 C20 175.8(5) . . . . ? Al1 C18 C19 C20 -67.8(3) . . . . ? C17 C18 C19 C24 -175.3(5) . . . . ? C23 C18 C19 C24 -0.7(8) . . . . ? Al1 C18 C19 C24 115.8(5) . . . . ? C17 C18 C19 Al1 68.9(3) . . . . ? C23 C18 C19 Al1 -116.5(5) . . . . ? C18 C19 C20 C21 -1.3(5) . . . . ? C24 C19 C20 C21 175.0(5) . . . . ? Al1 C19 C20 C21 -61.9(3) . . . . ? C18 C19 C20 C25 -180.0(5) . . . . ? C24 C19 C20 C25 -3.6(9) . . . . ? Al1 C19 C20 C25 119.5(5) . . . . ? C18 C19 C20 Al1 60.5(3) . . . . ? C24 C19 C20 Al1 -123.2(5) . . . . ? C18 C17 C21 C20 -0.3(6) . . . . ? C22 C17 C21 C20 -176.3(4) . . . . ? Al1 C17 C21 C20 59.9(3) . . . . ? C18 C17 C21 C26 179.5(5) . . . . ? C22 C17 C21 C26 3.5(8) . . . . ? Al1 C17 C21 C26 -120.4(5) . . . . ? C18 C17 C21 Al1 -60.1(3) . . . . ? C22 C17 C21 Al1 123.9(5) . . . . ? C19 C20 C21 C17 1.0(6) . . . . ? C25 C20 C21 C17 179.7(5) . . . . ? Al1 C20 C21 C17 -56.6(4) . . . . ? C19 C20 C21 C26 -178.8(5) . . . . ? C25 C20 C21 C26 -0.1(8) . . . . ? Al1 C20 C21 C26 123.6(5) . . . . ? C19 C20 C21 Al1 57.6(3) . . . . ? C25 C20 C21 Al1 -123.7(5) . . . . ? C32 C27 C28 F1 -179.7(4) . . . . ? Al1 C27 C28 F1 2.7(6) . . . . ? C32 C27 C28 C29 -0.2(7) . . . . ? Al1 C27 C28 C29 -177.9(4) . . . . ? F1 C28 C29 F2 -0.5(7) . . . . ? C27 C28 C29 F2 -179.9(4) . . . . ? F1 C28 C29 C30 179.8(4) . . . . ? C27 C28 C29 C30 0.3(8) . . . . ? F2 C29 C30 F3 -1.4(8) . . . . ? C28 C29 C30 F3 178.3(5) . . . . ? F2 C29 C30 C31 -179.9(4) . . . . ? C28 C29 C30 C31 -0.2(8) . . . . ? F3 C30 C31 F4 2.0(7) . . . . ? C29 C30 C31 F4 -179.5(5) . . . . ? F3 C30 C31 C32 -178.5(5) . . . . ? C29 C30 C31 C32 0.0(8) . . . . ? F4 C31 C32 F5 0.5(7) . . . . ? C30 C31 C32 F5 -178.9(4) . . . . ? F4 C31 C32 C27 179.5(5) . . . . ? C30 C31 C32 C27 0.1(8) . . . . ? C28 C27 C32 F5 179.0(4) . . . . ? Al1 C27 C32 F5 -3.3(6) . . . . ? C28 C27 C32 C31 0.1(7) . . . . ? Al1 C27 C32 C31 177.8(4) . . . . ? C28 C27 Al1 C18 -99.1(5) . . . . ? C32 C27 Al1 C18 83.4(5) . . . . ? C28 C27 Al1 C19 -56.0(5) . . . . ? C32 C27 Al1 C19 126.6(4) . . . . ? C28 C27 Al1 C17 -131.3(4) . . . . ? C32 C27 Al1 C17 51.3(5) . . . . ? C28 C27 Al1 Cl1 44.2(4) . . . . ? C32 C27 Al1 Cl1 -133.3(4) . . . . ? C28 C27 Al1 Cl2 129.7(4) . . . . ? C32 C27 Al1 Cl2 -47.8(4) . . . . ? C28 C27 Al1 C20 -74.3(4) . . . . ? C32 C27 Al1 C20 108.2(4) . . . . ? C28 C27 Al1 C21 -109.2(4) . . . . ? C32 C27 Al1 C21 73.3(4) . . . . ? C17 C18 Al1 C27 -48.3(5) . . . . ? C19 C18 Al1 C27 64.8(4) . . . . ? C23 C18 Al1 C27 -173.0(3) . . . . ? C17 C18 Al1 C19 -113.1(4) . . . . ? C23 C18 Al1 C19 122.2(5) . . . . ? C19 C18 Al1 C17 113.1(4) . . . . ? C23 C18 Al1 C17 -124.7(5) . . . . ? C17 C18 Al1 Cl1 168.6(3) . . . . ? C19 C18 Al1 Cl1 -78.3(3) . . . . ? C23 C18 Al1 Cl1 43.9(4) . . . . ? C17 C18 Al1 Cl2 82.5(3) . . . . ? C19 C18 Al1 Cl2 -164.4(3) . . . . ? C23 C18 Al1 Cl2 -42.2(4) . . . . ? C17 C18 Al1 C20 -76.8(3) . . . . ? C19 C18 Al1 C20 36.3(3) . . . . ? C23 C18 Al1 C20 158.5(4) . . . . ? C17 C18 Al1 C21 -36.7(3) . . . . ? C19 C18 Al1 C21 76.4(3) . . . . ? C23 C18 Al1 C21 -161.4(4) . . . . ? C20 C19 Al1 C27 -32.8(3) . . . . ? C18 C19 Al1 C27 -148.9(3) . . . . ? C24 C19 Al1 C27 93.9(5) . . . . ? C20 C19 Al1 C18 116.1(4) . . . . ? C24 C19 Al1 C18 -117.2(5) . . . . ? C20 C19 Al1 C17 76.3(3) . . . . ? C18 C19 Al1 C17 -39.8(3) . . . . ? C24 C19 Al1 C17 -157.0(5) . . . . ? C20 C19 Al1 Cl1 -137.4(2) . . . . ? C18 C19 Al1 Cl1 106.5(3) . . . . ? C24 C19 Al1 Cl1 -10.7(4) . . . . ? C20 C19 Al1 Cl2 139.0(2) . . . . ? C18 C19 Al1 Cl2 22.8(4) . . . . ? C24 C19 Al1 Cl2 -94.4(4) . . . . ? C18 C19 Al1 C20 -116.1(4) . . . . ? C24 C19 Al1 C20 126.7(5) . . . . ? C20 C19 Al1 C21 35.6(2) . . . . ? C18 C19 Al1 C21 -80.6(3) . . . . ? C24 C19 Al1 C21 162.2(5) . . . . ? C21 C17 Al1 C27 40.2(3) . . . . ? C18 C17 Al1 C27 156.1(3) . . . . ? C22 C17 Al1 C27 -85.7(4) . . . . ? C21 C17 Al1 C18 -115.9(4) . . . . ? C22 C17 Al1 C18 118.2(5) . . . . ? C21 C17 Al1 C19 -75.5(3) . . . . ? C18 C17 Al1 C19 40.3(3) . . . . ? C22 C17 Al1 C19 158.6(4) . . . . ? C21 C17 Al1 Cl1 -133.0(2) . . . . ? C18 C17 Al1 Cl1 -17.1(4) . . . . ? C22 C17 Al1 Cl1 101.1(4) . . . . ? C21 C17 Al1 Cl2 141.8(2) . . . . ? C18 C17 Al1 Cl2 -102.3(3) . . . . ? C22 C17 Al1 Cl2 16.0(4) . . . . ? C21 C17 Al1 C20 -35.0(2) . . . . ? C18 C17 Al1 C20 80.9(3) . . . . ? C22 C17 Al1 C20 -160.8(4) . . . . ? C18 C17 Al1 C21 115.9(4) . . . . ? C22 C17 Al1 C21 -125.9(5) . . . . ? C19 C20 Al1 C27 153.4(3) . . . . ? C21 C20 Al1 C27 -87.6(3) . . . . ? C25 C20 Al1 C27 34.0(4) . . . . ? C19 C20 Al1 C18 -39.6(2) . . . . ? C21 C20 Al1 C18 79.4(3) . . . . ? C25 C20 Al1 C18 -158.9(5) . . . . ? C21 C20 Al1 C19 119.0(4) . . . . ? C25 C20 Al1 C19 -119.4(5) . . . . ? C19 C20 Al1 C17 -83.5(3) . . . . ? C21 C20 Al1 C17 35.5(2) . . . . ? C25 C20 Al1 C17 157.2(5) . . . . ? C19 C20 Al1 Cl1 49.5(3) . . . . ? C21 C20 Al1 Cl1 168.5(2) . . . . ? C25 C20 Al1 Cl1 -69.8(4) . . . . ? C19 C20 Al1 Cl2 -90.6(4) . . . . ? C21 C20 Al1 Cl2 28.4(4) . . . . ? C25 C20 Al1 Cl2 150.0(3) . . . . ? C19 C20 Al1 C21 -119.0(4) . . . . ? C25 C20 Al1 C21 121.6(5) . . . . ? C17 C21 Al1 C27 -146.0(3) . . . . ? C20 C21 Al1 C27 93.9(3) . . . . ? C26 C21 Al1 C27 -26.9(4) . . . . ? C17 C21 Al1 C18 39.4(2) . . . . ? C20 C21 Al1 C18 -80.7(3) . . . . ? C26 C21 Al1 C18 158.5(5) . . . . ? C17 C21 Al1 C19 84.0(3) . . . . ? C20 C21 Al1 C19 -36.0(2) . . . . ? C26 C21 Al1 C19 -156.9(5) . . . . ? C20 C21 Al1 C17 -120.0(4) . . . . ? C26 C21 Al1 C17 119.1(5) . . . . ? C17 C21 Al1 Cl1 98.7(3) . . . . ? C20 C21 Al1 Cl1 -21.3(4) . . . . ? C26 C21 Al1 Cl1 -142.2(3) . . . . ? C17 C21 Al1 Cl2 -45.7(3) . . . . ? C20 C21 Al1 Cl2 -165.7(2) . . . . ? C26 C21 Al1 Cl2 73.5(4) . . . . ? C17 C21 Al1 C20 120.0(4) . . . . ? C26 C21 Al1 C20 -120.8(5) . . . . ? C12 C11 Al2 C4 -83.3(5) . . . . ? C16 C11 Al2 C4 95.2(5) . . . . ? C12 C11 Al2 C5 -50.9(5) . . . . ? C16 C11 Al2 C5 127.6(4) . . . . ? C12 C11 Al2 C3 -125.6(4) . . . . ? C16 C11 Al2 C3 52.9(4) . . . . ? C12 C11 Al2 Cl2 133.6(4) . . . . ? C16 C11 Al2 Cl2 -47.9(4) . . . . ? C12 C11 Al2 C2 -107.3(4) . . . . ? C16 C11 Al2 C2 71.1(4) . . . . ? C12 C11 Al2 Cl1 48.2(4) . . . . ? C16 C11 Al2 Cl1 -133.3(4) . . . . ? C12 C11 Al2 C1 -72.8(4) . . . . ? C16 C11 Al2 C1 105.7(4) . . . . ? C5 C4 Al2 C11 48.5(4) . . . . ? C3 C4 Al2 C11 -63.8(4) . . . . ? C9 C4 Al2 C11 172.9(3) . . . . ? C3 C4 Al2 C5 -112.2(4) . . . . ? C9 C4 Al2 C5 124.4(4) . . . . ? C5 C4 Al2 C3 112.2(4) . . . . ? C9 C4 Al2 C3 -123.4(4) . . . . ? C5 C4 Al2 Cl2 -169.1(2) . . . . ? C3 C4 Al2 Cl2 78.6(3) . . . . ? C9 C4 Al2 Cl2 -44.7(3) . . . . ? C5 C4 Al2 C2 76.0(3) . . . . ? C3 C4 Al2 C2 -36.2(3) . . . . ? C9 C4 Al2 C2 -159.6(4) . . . . ? C5 C4 Al2 Cl1 -83.4(2) . . . . ? C3 C4 Al2 Cl1 164.4(3) . . . . ? C9 C4 Al2 Cl1 41.0(3) . . . . ? C5 C4 Al2 C1 36.5(2) . . . . ? C3 C4 Al2 C1 -75.7(3) . . . . ? C9 C4 Al2 C1 160.9(4) . . . . ? C1 C5 Al2 C11 -39.8(3) . . . . ? C4 C5 Al2 C11 -155.8(3) . . . . ? C10 C5 Al2 C11 85.1(4) . . . . ? C1 C5 Al2 C4 116.0(4) . . . . ? C10 C5 Al2 C4 -119.0(5) . . . . ? C1 C5 Al2 C3 75.3(3) . . . . ? C4 C5 Al2 C3 -40.7(3) . . . . ? C10 C5 Al2 C3 -159.7(4) . . . . ? C1 C5 Al2 Cl2 133.0(2) . . . . ? C4 C5 Al2 Cl2 17.0(3) . . . . ? C10 C5 Al2 Cl2 -102.0(4) . . . . ? C1 C5 Al2 C2 34.7(3) . . . . ? C4 C5 Al2 C2 -81.3(3) . . . . ? C10 C5 Al2 C2 159.7(4) . . . . ? C1 C5 Al2 Cl1 -143.5(2) . . . . ? C4 C5 Al2 Cl1 100.5(2) . . . . ? C10 C5 Al2 Cl1 -18.5(4) . . . . ? C4 C5 Al2 C1 -116.0(4) . . . . ? C10 C5 Al2 C1 125.0(5) . . . . ? C2 C3 Al2 C11 32.6(3) . . . . ? C4 C3 Al2 C11 149.0(3) . . . . ? C8 C3 Al2 C11 -93.6(5) . . . . ? C2 C3 Al2 C4 -116.4(4) . . . . ? C8 C3 Al2 C4 117.3(5) . . . . ? C2 C3 Al2 C5 -75.7(3) . . . . ? C4 C3 Al2 C5 40.7(3) . . . . ? C8 C3 Al2 C5 158.0(5) . . . . ? C2 C3 Al2 Cl2 136.3(2) . . . . ? C4 C3 Al2 Cl2 -107.3(2) . . . . ? C8 C3 Al2 Cl2 10.0(4) . . . . ? C4 C3 Al2 C2 116.4(4) . . . . ? C8 C3 Al2 C2 -126.3(5) . . . . ? C2 C3 Al2 Cl1 -138.6(2) . . . . ? C4 C3 Al2 Cl1 -22.2(3) . . . . ? C8 C3 Al2 Cl1 95.1(4) . . . . ? C2 C3 Al2 C1 -34.9(2) . . . . ? C4 C3 Al2 C1 81.5(3) . . . . ? C8 C3 Al2 C1 -161.1(5) . . . . ? C3 C2 Al2 C11 -153.3(3) . . . . ? C1 C2 Al2 C11 86.9(3) . . . . ? C7 C2 Al2 C11 -34.7(5) . . . . ? C3 C2 Al2 C4 39.5(2) . . . . ? C1 C2 Al2 C4 -80.3(3) . . . . ? C7 C2 Al2 C4 158.1(6) . . . . ? C3 C2 Al2 C5 84.0(3) . . . . ? C1 C2 Al2 C5 -35.8(2) . . . . ? C7 C2 Al2 C5 -157.4(6) . . . . ? C1 C2 Al2 C3 -119.7(4) . . . . ? C7 C2 Al2 C3 118.6(6) . . . . ? C3 C2 Al2 Cl2 -51.4(3) . . . . ? C1 C2 Al2 Cl2 -171.2(2) . . . . ? C7 C2 Al2 Cl2 67.2(5) . . . . ? C3 C2 Al2 Cl1 87.9(4) . . . . ? C1 C2 Al2 Cl1 -31.8(4) . . . . ? C7 C2 Al2 Cl1 -153.5(4) . . . . ? C3 C2 Al2 C1 119.7(4) . . . . ? C7 C2 Al2 C1 -121.6(6) . . . . ? C2 C1 Al2 C11 -94.0(3) . . . . ? C5 C1 Al2 C11 146.0(3) . . . . ? C6 C1 Al2 C11 27.7(4) . . . . ? C2 C1 Al2 C4 80.3(3) . . . . ? C5 C1 Al2 C4 -39.6(2) . . . . ? C6 C1 Al2 C4 -158.0(5) . . . . ? C2 C1 Al2 C5 120.0(4) . . . . ? C6 C1 Al2 C5 -118.4(5) . . . . ? C2 C1 Al2 C3 35.8(2) . . . . ? C5 C1 Al2 C3 -84.2(3) . . . . ? C6 C1 Al2 C3 157.4(5) . . . . ? C2 C1 Al2 Cl2 16.7(4) . . . . ? C5 C1 Al2 Cl2 -103.2(3) . . . . ? C6 C1 Al2 Cl2 138.4(4) . . . . ? C5 C1 Al2 C2 -120.0(4) . . . . ? C6 C1 Al2 C2 121.7(5) . . . . ? C2 C1 Al2 Cl1 163.5(2) . . . . ? C5 C1 Al2 Cl1 43.6(3) . . . . ? C6 C1 Al2 Cl1 -74.8(4) . . . . ? C27 Al1 Cl1 Al2 98.41(13) . . . . ? C18 Al1 Cl1 Al2 -98.27(14) . . . . ? C19 Al1 Cl1 Al2 -135.91(12) . . . . ? C17 Al1 Cl1 Al2 -87.6(2) . . . . ? Cl2 Al1 Cl1 Al2 1.14(5) . . . . ? C20 Al1 Cl1 Al2 -162.09(13) . . . . ? C21 Al1 Cl1 Al2 -148.5(2) . . . . ? C11 Al2 Cl1 Al1 97.11(13) . . . . ? C4 Al2 Cl1 Al1 -104.08(13) . . . . ? C5 Al2 Cl1 Al1 -142.45(11) . . . . ? C3 Al2 Cl1 Al1 -90.26(19) . . . . ? Cl2 Al2 Cl1 Al1 -1.14(5) . . . . ? C2 Al2 Cl1 Al1 -145.9(3) . . . . ? C1 Al2 Cl1 Al1 -166.14(13) . . . . ? C11 Al2 Cl2 Al1 -98.58(13) . . . . ? C4 Al2 Cl2 Al1 98.56(13) . . . . ? C5 Al2 Cl2 Al1 87.7(2) . . . . ? C3 Al2 Cl2 Al1 136.39(12) . . . . ? C2 Al2 Cl2 Al1 163.42(13) . . . . ? Cl1 Al2 Cl2 Al1 1.14(5) . . . . ? C1 Al2 Cl2 Al1 152.7(2) . . . . ? C27 Al1 Cl2 Al2 -101.18(13) . . . . ? C18 Al1 Cl2 Al2 99.91(14) . . . . ? C19 Al1 Cl2 Al2 85.7(2) . . . . ? C17 Al1 Cl2 Al2 137.69(12) . . . . ? Cl1 Al1 Cl2 Al2 -1.15(5) . . . . ? C20 Al1 Cl2 Al2 143.9(3) . . . . ? C21 Al1 Cl2 Al2 162.31(12) . . . . ? C36 C37 C33 C34 1.0(7) . . . . ? C42 C37 C33 C34 -176.7(7) . . . . ? Al3 C37 C33 C34 61.8(4) . . . . ? C36 C37 C33 C38 -178.8(6) . . . . ? C42 C37 C33 C38 3.6(10) . . . . ? Al3 C37 C33 C38 -118.0(6) . . . . ? C36 C37 C33 Al3 -60.8(4) . . . . ? C42 C37 C33 Al3 121.6(8) . . . . ? C37 C33 C34 C35 -1.4(7) . . . . ? C38 C33 C34 C35 178.3(5) . . . . ? Al3 C33 C34 C35 56.0(4) . . . . ? C37 C33 C34 C39 179.8(6) . . . . ? C38 C33 C34 C39 -0.5(10) . . . . ? Al3 C33 C34 C39 -122.8(6) . . . . ? C37 C33 C34 Al3 -57.4(4) . . . . ? C38 C33 C34 Al3 122.3(6) . . . . ? C33 C34 C35 C36 1.3(7) . . . . ? C39 C34 C35 C36 -179.9(6) . . . . ? Al3 C34 C35 C36 61.4(4) . . . . ? C33 C34 C35 C40 177.2(6) . . . . ? C39 C34 C35 C40 -4.0(10) . . . . ? Al3 C34 C35 C40 -122.8(7) . . . . ? C33 C34 C35 Al3 -60.0(4) . . . . ? C39 C34 C35 Al3 118.8(6) . . . . ? C34 C35 C36 C37 -0.7(7) . . . . ? C40 C35 C36 C37 -176.6(6) . . . . ? Al3 C35 C36 C37 68.4(5) . . . . ? C34 C35 C36 C41 173.3(5) . . . . ? C40 C35 C36 C41 -2.6(10) . . . . ? Al3 C35 C36 C41 -117.7(6) . . . . ? C34 C35 C36 Al3 -69.1(4) . . . . ? C40 C35 C36 Al3 115.0(6) . . . . ? C33 C37 C36 C35 -0.2(7) . . . . ? C42 C37 C36 C35 177.4(7) . . . . ? Al3 C37 C36 C35 -68.7(4) . . . . ? C33 C37 C36 C41 -174.0(6) . . . . ? C42 C37 C36 C41 3.6(11) . . . . ? Al3 C37 C36 C41 117.5(7) . . . . ? C33 C37 C36 Al3 68.5(4) . . . . ? C42 C37 C36 Al3 -113.9(7) . . . . ? C48 C43 C44 F11 178.7(4) . . . . ? Al3 C43 C44 F11 6.0(7) . . . . ? C48 C43 C44 C45 -0.3(8) . . . . ? Al3 C43 C44 C45 -173.0(4) . . . . ? F11 C44 C45 F12 0.5(8) . . . . ? C43 C44 C45 F12 179.5(5) . . . . ? F11 C44 C45 C46 -178.3(5) . . . . ? C43 C44 C45 C46 0.8(9) . . . . ? F12 C45 C46 F13 1.6(9) . . . . ? C44 C45 C46 F13 -179.6(5) . . . . ? F12 C45 C46 C47 -179.1(6) . . . . ? C44 C45 C46 C47 -0.3(9) . . . . ? F13 C46 C47 F14 -2.2(8) . . . . ? C45 C46 C47 F14 178.5(5) . . . . ? F13 C46 C47 C48 178.8(5) . . . . ? C45 C46 C47 C48 -0.5(9) . . . . ? C44 C43 C48 F15 -179.4(4) . . . . ? Al3 C43 C48 F15 -6.6(6) . . . . ? C44 C43 C48 C47 -0.6(7) . . . . ? Al3 C43 C48 C47 172.2(4) . . . . ? F14 C47 C48 F15 0.9(7) . . . . ? C46 C47 C48 F15 179.9(5) . . . . ? F14 C47 C48 C43 -177.9(5) . . . . ? C46 C47 C48 C43 1.0(8) . . . . ? C44 C43 Al3 C36 94.0(7) . . . . ? C48 C43 Al3 C36 -78.2(7) . . . . ? C44 C43 Al3 C35 124.3(4) . . . . ? C48 C43 Al3 C35 -47.9(4) . . . . ? C44 C43 Al3 C37 50.5(5) . . . . ? C48 C43 Al3 C37 -121.6(4) . . . . ? C44 C43 Al3 Cl3 -50.4(4) . . . . ? C48 C43 Al3 Cl3 137.4(4) . . . . ? C44 C43 Al3 Cl3 -136.5(4) . . . 3_667 ? C48 C43 Al3 Cl3 51.3(4) . . . 3_667 ? C44 C43 Al3 C33 68.3(4) . . . . ? C48 C43 Al3 C33 -103.9(4) . . . . ? C44 C43 Al3 C34 102.2(4) . . . . ? C48 C43 Al3 C34 -70.0(4) . . . . ? C35 C36 Al3 C43 46.4(8) . . . . ? C37 C36 Al3 C43 -66.6(8) . . . . ? C41 C36 Al3 C43 169.1(7) . . . . ? C37 C36 Al3 C35 -113.0(5) . . . . ? C41 C36 Al3 C35 122.6(10) . . . . ? C35 C36 Al3 C37 113.0(5) . . . . ? C41 C36 Al3 C37 -124.3(10) . . . . ? C35 C36 Al3 Cl3 -169.7(3) . . . . ? C37 C36 Al3 Cl3 77.2(4) . . . . ? C41 C36 Al3 Cl3 -47.1(9) . . . . ? C35 C36 Al3 Cl3 -83.2(3) . . . 3_667 ? C37 C36 Al3 Cl3 163.8(3) . . . 3_667 ? C41 C36 Al3 Cl3 39.4(8) . . . 3_667 ? C35 C36 Al3 C33 76.2(3) . . . . ? C37 C36 Al3 C33 -36.8(3) . . . . ? C41 C36 Al3 C33 -161.2(9) . . . . ? C35 C36 Al3 C34 37.0(3) . . . . ? C37 C36 Al3 C34 -76.1(3) . . . . ? C41 C36 Al3 C34 159.6(9) . . . . ? C34 C35 Al3 C43 -40.9(4) . . . . ? C36 C35 Al3 C43 -155.9(4) . . . . ? C40 C35 Al3 C43 85.3(6) . . . . ? C34 C35 Al3 C36 115.0(5) . . . . ? C40 C35 Al3 C36 -118.8(7) . . . . ? C34 C35 Al3 C37 74.5(4) . . . . ? C36 C35 Al3 C37 -40.5(4) . . . . ? C40 C35 Al3 C37 -159.3(7) . . . . ? C34 C35 Al3 Cl3 130.9(3) . . . . ? C36 C35 Al3 Cl3 15.9(5) . . . . ? C40 C35 Al3 Cl3 -102.9(6) . . . . ? C34 C35 Al3 Cl3 -144.0(3) . . . 3_667 ? C36 C35 Al3 Cl3 101.0(4) . . . 3_667 ? C40 C35 Al3 Cl3 -17.8(6) . . . 3_667 ? C34 C35 Al3 C33 33.8(3) . . . . ? C36 C35 Al3 C33 -81.2(4) . . . . ? C40 C35 Al3 C33 160.0(7) . . . . ? C36 C35 Al3 C34 -115.0(5) . . . . ? C40 C35 Al3 C34 126.2(8) . . . . ? C33 C37 Al3 C43 31.7(5) . . . . ? C36 C37 Al3 C43 146.8(4) . . . . ? C42 C37 Al3 C43 -93.0(8) . . . . ? C33 C37 Al3 C36 -115.1(6) . . . . ? C42 C37 Al3 C36 120.2(10) . . . . ? C33 C37 Al3 C35 -75.5(4) . . . . ? C36 C37 Al3 C35 39.6(4) . . . . ? C42 C37 Al3 C35 159.8(9) . . . . ? C33 C37 Al3 Cl3 136.3(4) . . . . ? C36 C37 Al3 Cl3 -108.6(4) . . . . ? C42 C37 Al3 Cl3 11.5(8) . . . . ? C33 C37 Al3 Cl3 -138.4(3) . . . 3_667 ? C36 C37 Al3 Cl3 -23.3(5) . . . 3_667 ? C42 C37 Al3 Cl3 96.9(8) . . . 3_667 ? C36 C37 Al3 C33 115.1(6) . . . . ? C42 C37 Al3 C33 -124.7(10) . . . . ? C33 C37 Al3 C34 -35.0(3) . . . . ? C36 C37 Al3 C34 80.1(4) . . . . ? C42 C37 Al3 C34 -159.8(9) . . . . ? C34 C33 Al3 C43 87.1(3) . . . . ? C37 C33 Al3 C43 -154.1(5) . . . . ? C38 C33 Al3 C43 -35.8(5) . . . . ? C34 C33 Al3 C36 -78.6(4) . . . . ? C37 C33 Al3 C36 40.2(4) . . . . ? C38 C33 Al3 C36 158.4(7) . . . . ? C34 C33 Al3 C35 -34.9(3) . . . . ? C37 C33 Al3 C35 83.9(4) . . . . ? C38 C33 Al3 C35 -157.9(6) . . . . ? C34 C33 Al3 C37 -118.8(5) . . . . ? C38 C33 Al3 C37 118.3(8) . . . . ? C34 C33 Al3 Cl3 -169.9(3) . . . . ? C37 C33 Al3 Cl3 -51.2(5) . . . . ? C38 C33 Al3 Cl3 67.1(5) . . . . ? C34 C33 Al3 Cl3 -30.2(5) . . . 3_667 ? C37 C33 Al3 Cl3 88.6(5) . . . 3_667 ? C38 C33 Al3 Cl3 -153.1(4) . . . 3_667 ? C37 C33 Al3 C34 118.8(5) . . . . ? C38 C33 Al3 C34 -122.9(6) . . . . ? C33 C34 Al3 C43 -93.8(3) . . . . ? C35 C34 Al3 C43 144.9(4) . . . . ? C39 C34 Al3 C43 27.3(5) . . . . ? C33 C34 Al3 C36 81.5(4) . . . . ? C35 C34 Al3 C36 -39.7(4) . . . . ? C39 C34 Al3 C36 -157.4(6) . . . . ? C33 C34 Al3 C35 121.2(5) . . . . ? C39 C34 Al3 C35 -117.6(7) . . . . ? C33 C34 Al3 C37 36.4(4) . . . . ? C35 C34 Al3 C37 -84.8(4) . . . . ? C39 C34 Al3 C37 157.6(6) . . . . ? C33 C34 Al3 Cl3 18.5(5) . . . . ? C35 C34 Al3 Cl3 -102.8(4) . . . . ? C39 C34 Al3 Cl3 139.6(4) . . . . ? C33 C34 Al3 Cl3 164.3(3) . . . 3_667 ? C35 C34 Al3 Cl3 43.1(4) . . . 3_667 ? C39 C34 Al3 Cl3 -74.6(5) . . . 3_667 ? C35 C34 Al3 C33 -121.2(5) . . . . ? C39 C34 Al3 C33 121.1(6) . . . . ? C43 Al3 Cl3 Al3 -99.10(13) . . . 3_667 ? C36 Al3 Cl3 Al3 98.2(2) . . . 3_667 ? C35 Al3 Cl3 Al3 88.2(2) . . . 3_667 ? C37 Al3 Cl3 Al3 135.6(2) . . . 3_667 ? Cl3 Al3 Cl3 Al3 0.0 3_667 . . 3_667 ? C33 Al3 Cl3 Al3 162.48(16) . . . 3_667 ? C34 Al3 Cl3 Al3 151.0(3) . . . 3_667 ? _diffrn_measured_fraction_theta_max 0.830 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.830 _refine_diff_density_max 0.278 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.076 # Attachment 'MCpArFGaCl.cif' data_15 _database_code_depnum_ccdc_archive 'CCDC 664850' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H15 Cl F5 Ga' _chemical_formula_weight 407.45 _chemical_melting_point ? _chemical_compound_source ? 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8805(7) _cell_length_b 11.0468(8) _cell_length_c 14.4924(13) _cell_angle_alpha 81.353(6) _cell_angle_beta 82.605(6) _cell_angle_gamma 77.414(5) _cell_volume 1672.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 68 _cell_measurement_theta_min 4.74 _cell_measurement_theta_max 12.74 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method ? _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.849 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 26.52 _diffrn_reflns_number 7954 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0800 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7112 _reflns_number_observed 4330 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1312P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7112 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_obs 0.0755 _refine_ls_wR_factor_all 0.2075 _refine_ls_wR_factor_obs 0.1853 _refine_ls_goodness_of_fit_all 0.961 _refine_ls_goodness_of_fit_obs 1.113 _refine_ls_restrained_S_all 0.961 _refine_ls_restrained_S_obs 1.113 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ga1 Ga 0.14402(6) 0.90102(6) 0.50711(5) 0.0302(2) Uani 1 d . . Ga2 Ga 0.40174(7) 0.14455(7) -0.00791(5) 0.0315(2) Uani 1 d . . Cl1 Cl 0.0399(2) 1.0463(2) 0.38949(12) 0.0387(4) Uani 1 d . . Cl2 Cl 0.4497(2) -0.0263(2) 0.11052(12) 0.0415(4) Uani 1 d . . F22 F 0.2021(4) 0.7932(4) 0.3150(3) 0.0479(11) Uani 1 d . . F23 F 0.2136(5) 0.5620(5) 0.2737(4) 0.069(2) Uani 1 d . . F24 F 0.1790(5) 0.3755(4) 0.4114(5) 0.078(2) Uani 1 d . . F25 F 0.1301(5) 0.4185(4) 0.5931(4) 0.074(2) Uani 1 d . . F26 F 0.1079(5) 0.6534(4) 0.6354(3) 0.0536(11) Uani 1 d . . F42 F 0.2947(4) 0.1891(5) -0.2029(3) 0.0519(11) Uani 1 d . . F43 F 0.0567(5) 0.2119(6) -0.2472(3) 0.0666(15) Uani 1 d . . F44 F -0.1332(4) 0.1863(6) -0.1118(4) 0.075(2) Uani 1 d . . F45 F -0.0870(4) 0.1398(5) 0.0705(3) 0.0655(14) Uani 1 d . . F46 F 0.1485(4) 0.1181(5) 0.1167(3) 0.0544(12) Uani 1 d . . C11 C 0.2895(6) 0.9643(6) 0.5435(5) 0.0328(14) Uani 1 d . . C12 C 0.3701(6) 0.9210(6) 0.4596(5) 0.0330(14) Uani 1 d . . C13 C 0.4268(6) 0.7994(6) 0.4846(5) 0.0353(15) Uani 1 d . . C14 C 0.3916(6) 0.7627(6) 0.5832(5) 0.037(2) Uani 1 d . . C15 C 0.3098(6) 0.8631(6) 0.6184(5) 0.0344(14) Uani 1 d . . C21 C 0.1522(6) 0.7316(6) 0.4762(6) 0.040(2) Uani 1 d . . C22 C 0.1784(6) 0.7046(7) 0.3870(5) 0.039(2) Uani 1 d . . C23 C 0.1889(7) 0.5847(7) 0.3625(6) 0.047(2) Uani 1 d . . C24 C 0.1709(7) 0.4906(7) 0.4330(7) 0.051(2) Uani 1 d . . C25 C 0.1450(7) 0.5124(7) 0.5243(6) 0.048(2) Uani 1 d . . C26 C 0.1335(6) 0.6344(7) 0.5440(6) 0.040(2) Uani 1 d . . C31 C 0.4676(6) 0.2905(6) 0.0175(5) 0.0342(15) Uani 1 d . . C32 C 0.3606(6) 0.3242(6) 0.0871(5) 0.0344(14) Uani 1 d . . C33 C 0.2650(6) 0.4022(6) 0.0421(5) 0.037(2) Uani 1 d . . C34 C 0.3053(7) 0.4268(6) -0.0547(5) 0.0365(15) Uani 1 d . . C35 C 0.4303(7) 0.3622(6) -0.0709(5) 0.037(2) Uani 1 d . . C41 C 0.2306(6) 0.1506(6) -0.0422(4) 0.0321(14) Uani 1 d . . C42 C 0.2031(7) 0.1729(7) -0.1313(5) 0.038(2) Uani 1 d . . C43 C 0.0814(7) 0.1856(8) -0.1575(5) 0.045(2) Uani 1 d . . C44 C -0.0156(7) 0.1722(8) -0.0877(6) 0.047(2) Uani 1 d . . C45 C 0.0077(7) 0.1506(7) 0.0022(6) 0.044(2) Uani 1 d . . C46 C 0.1299(7) 0.1382(7) 0.0264(5) 0.041(2) Uani 1 d . . C111 C 0.2570(8) 1.0998(7) 0.5606(7) 0.054(2) Uani 1 d . . H11A H 0.2461(60) 1.1524(7) 0.5020(9) 0.081 Uiso 1 calc R . H11B H 0.3243(29) 1.1186(17) 0.5892(41) 0.081 Uiso 1 calc R . H11C H 0.1800(34) 1.1143(16) 0.6015(37) 0.081 Uiso 1 calc R . C121 C 0.3884(8) 1.0021(8) 0.3686(5) 0.054(2) Uani 1 d . . H12A H 0.3079(10) 1.0360(45) 0.3449(21) 0.081 Uiso 1 calc R . H12B H 0.4425(46) 0.9533(15) 0.3242(14) 0.081 Uiso 1 calc R . H12C H 0.4265(53) 1.0692(33) 0.3784(10) 0.081 Uiso 1 calc R . C131 C 0.5069(7) 0.7122(8) 0.4199(7) 0.063(3) Uani 1 d . . H13A H 0.5789(37) 0.6644(48) 0.4500(20) 0.095 Uiso 1 calc R . H13B H 0.5352(56) 0.7599(9) 0.3632(21) 0.095 Uiso 1 calc R . H13C H 0.4578(22) 0.6566(46) 0.4050(41) 0.095 Uiso 1 calc R . C141 C 0.4327(8) 0.6337(7) 0.6367(7) 0.065(3) Uani 1 d . . H14A H 0.5221(13) 0.6178(26) 0.6416(40) 0.097 Uiso 1 calc R . H14B H 0.4137(58) 0.5717(9) 0.6040(26) 0.097 Uiso 1 calc R . H14C H 0.3882(46) 0.6302(21) 0.6984(18) 0.097 Uiso 1 calc R . C151 C 0.2584(8) 0.8711(9) 0.7203(5) 0.053(2) Uani 1 d . . H15A H 0.1744(24) 0.9214(48) 0.7233(5) 0.079 Uiso 1 calc R . H15B H 0.3122(33) 0.9081(53) 0.7501(12) 0.079 Uiso 1 calc R . H15C H 0.2560(55) 0.7886(10) 0.7518(12) 0.079 Uiso 1 calc R . C311 C 0.6038(7) 0.2604(7) 0.0423(6) 0.049(2) Uani 1 d . . H22D H 0.6155(16) 0.1884(32) 0.0889(29) 0.074 Uiso 1 calc R . H22E H 0.6213(17) 0.3305(21) 0.0665(38) 0.074 Uiso 1 calc R . H22F H 0.6603(7) 0.2435(52) -0.0129(10) 0.074 Uiso 1 calc R . C321 C 0.3617(8) 0.2819(8) 0.1885(5) 0.055(2) Uani 1 d . . H22A H 0.4285(37) 0.2100(36) 0.1987(6) 0.082 Uiso 1 calc R . H22B H 0.2820(22) 0.2602(54) 0.2132(10) 0.082 Uiso 1 calc R . H22C H 0.3753(58) 0.3478(22) 0.2198(8) 0.082 Uiso 1 calc R . C331 C 0.1356(7) 0.4531(8) 0.0841(6) 0.053(2) Uani 1 d . . H23A H 0.0742(7) 0.4329(48) 0.0501(26) 0.079 Uiso 1 calc R . H23B H 0.1236(21) 0.5423(10) 0.0811(38) 0.079 Uiso 1 calc R . H23C H 0.1252(20) 0.4169(42) 0.1485(13) 0.079 Uiso 1 calc R . C341 C 0.2250(8) 0.5018(8) -0.1269(6) 0.055(2) Uani 1 d . . H24A H 0.1961(46) 0.5856(16) -0.1115(23) 0.082 Uiso 1 calc R . H24B H 0.1535(30) 0.4648(31) -0.1287(29) 0.082 Uiso 1 calc R . H24C H 0.2736(18) 0.5036(46) -0.1871(9) 0.082 Uiso 1 calc R . C351 C 0.5173(8) 0.3683(8) -0.1573(6) 0.059(2) Uani 1 d . . H25A H 0.5760(40) 0.2898(23) -0.1593(23) 0.088 Uiso 1 calc R . H25B H 0.5630(47) 0.4337(42) -0.1580(23) 0.088 Uiso 1 calc R . H25C H 0.4698(10) 0.3853(62) -0.2108(6) 0.088 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 Ga1 0.0264(4) 0.0302(4) 0.0351(4) -0.0038(3) -0.0050(3) -0.0072(3) Ga2 0.0300(4) 0.0307(4) 0.0349(4) -0.0061(3) -0.0024(3) -0.0075(3) Cl1 0.0317(8) 0.0452(9) 0.0330(9) 0.0038(7) -0.0020(7) -0.0011(7) Cl2 0.0505(10) 0.0343(8) 0.0328(9) -0.0026(7) 0.0060(8) -0.0005(7) F22 0.056(3) 0.045(2) 0.047(3) -0.010(2) -0.001(2) -0.020(2) F23 0.076(4) 0.064(3) 0.078(4) -0.042(3) 0.010(3) -0.022(3) F24 0.077(4) 0.038(2) 0.125(5) -0.029(3) 0.003(3) -0.018(2) F25 0.074(4) 0.040(2) 0.105(5) 0.009(3) -0.002(3) -0.023(2) F26 0.058(3) 0.055(3) 0.049(3) 0.003(2) -0.004(2) -0.021(2) F42 0.037(2) 0.078(3) 0.041(3) -0.007(2) 0.001(2) -0.017(2) F43 0.048(3) 0.108(4) 0.047(3) -0.013(3) -0.014(2) -0.015(3) F44 0.030(2) 0.125(5) 0.079(4) -0.026(4) -0.007(2) -0.022(3) F45 0.040(3) 0.098(4) 0.059(3) -0.010(3) 0.015(2) -0.025(3) F46 0.049(3) 0.077(3) 0.039(3) -0.009(2) 0.005(2) -0.020(2) C11 0.034(3) 0.032(3) 0.035(4) -0.009(3) -0.005(3) -0.010(3) C12 0.029(3) 0.039(3) 0.037(4) -0.006(3) -0.004(3) -0.017(3) C13 0.027(3) 0.035(3) 0.049(4) -0.009(3) -0.008(3) -0.011(3) C14 0.029(3) 0.032(3) 0.051(4) 0.000(3) -0.014(3) -0.010(3) C15 0.031(3) 0.039(3) 0.038(4) -0.004(3) -0.009(3) -0.015(3) C21 0.019(3) 0.036(3) 0.072(5) -0.019(4) -0.007(3) -0.007(3) C22 0.027(3) 0.041(4) 0.052(4) -0.010(3) -0.002(3) -0.014(3) C23 0.036(4) 0.046(4) 0.065(5) -0.022(4) -0.002(4) -0.013(3) C24 0.038(4) 0.035(4) 0.083(6) -0.017(4) 0.001(4) -0.014(3) C25 0.034(4) 0.036(4) 0.075(6) -0.001(4) -0.005(4) -0.013(3) C26 0.027(3) 0.044(4) 0.053(5) -0.006(4) -0.006(3) -0.012(3) C31 0.028(3) 0.036(3) 0.044(4) -0.014(3) -0.009(3) -0.008(3) C32 0.038(3) 0.030(3) 0.037(4) -0.005(3) -0.010(3) -0.008(3) C33 0.036(3) 0.028(3) 0.049(4) -0.009(3) -0.010(3) -0.006(3) C34 0.037(3) 0.027(3) 0.048(4) -0.002(3) -0.012(3) -0.011(3) C35 0.037(3) 0.029(3) 0.049(4) -0.001(3) -0.006(3) -0.014(3) C41 0.040(4) 0.028(3) 0.028(3) 0.000(3) -0.003(3) -0.011(3) C42 0.035(4) 0.044(4) 0.039(4) -0.012(3) 0.000(3) -0.011(3) C43 0.033(4) 0.064(5) 0.046(5) -0.018(4) -0.008(3) -0.013(3) C44 0.027(3) 0.062(5) 0.056(5) -0.015(4) -0.007(3) -0.013(3) C45 0.034(4) 0.049(4) 0.050(5) -0.009(4) 0.006(3) -0.013(3) C46 0.040(4) 0.042(4) 0.042(4) -0.016(3) 0.002(3) -0.011(3) C111 0.047(4) 0.037(4) 0.086(7) -0.025(4) -0.008(4) -0.014(3) C121 0.054(5) 0.068(5) 0.041(4) 0.007(4) -0.002(4) -0.027(4) C131 0.036(4) 0.066(5) 0.097(7) -0.050(5) 0.005(4) -0.012(4) C141 0.059(5) 0.035(4) 0.105(8) 0.012(5) -0.040(5) -0.015(4) C151 0.051(5) 0.077(6) 0.035(4) -0.006(4) -0.004(4) -0.022(4) C311 0.037(4) 0.049(4) 0.062(5) 0.004(4) -0.022(4) -0.010(3) C321 0.060(5) 0.054(5) 0.053(5) -0.020(4) -0.018(4) 0.001(4) C331 0.043(4) 0.058(5) 0.054(5) -0.017(4) -0.002(4) 0.004(4) C341 0.049(5) 0.053(5) 0.061(6) 0.009(4) -0.020(4) -0.010(4) C351 0.046(5) 0.056(5) 0.071(6) -0.003(5) 0.010(4) -0.018(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 C21 1.971(6) . ? Ga1 C11 2.019(6) . ? Ga1 Cl1 2.361(2) 2_576 ? Ga1 Cl1 2.376(2) . ? Ga1 C15 2.499(7) . ? Ga1 C12 2.516(6) . ? Ga2 C41 1.973(7) . ? Ga2 C31 1.999(6) . ? Ga2 Cl2 2.361(2) 2_655 ? Ga2 Cl2 2.368(2) . ? Ga2 C35 2.511(6) . ? Ga2 C32 2.512(6) . ? Cl1 Ga1 2.360(2) 2_576 ? Cl2 Ga2 2.361(2) 2_655 ? F22 C22 1.359(8) . ? F23 C23 1.331(9) . ? F24 C24 1.338(8) . ? F25 C25 1.348(9) . ? F26 C26 1.357(8) . ? F42 C42 1.363(8) . ? F43 C43 1.337(9) . ? F44 C44 1.341(8) . ? F45 C45 1.346(8) . ? F46 C46 1.328(8) . ? C11 C15 1.437(10) . ? C11 C12 1.481(9) . ? C11 C111 1.512(9) . ? C12 C13 1.366(10) . ? C12 C121 1.495(10) . ? C13 C14 1.451(10) . ? C13 C131 1.505(9) . ? C14 C15 1.382(9) . ? C14 C141 1.520(10) . ? C15 C151 1.517(9) . ? C21 C22 1.351(10) . ? C21 C26 1.373(11) . ? C22 C23 1.399(10) . ? C23 C24 1.372(12) . ? C24 C25 1.363(12) . ? C25 C26 1.396(10) . ? C31 C35 1.457(10) . ? C31 C32 1.460(9) . ? C31 C311 1.523(9) . ? C32 C33 1.366(10) . ? C32 C321 1.475(10) . ? C33 C34 1.419(10) . ? C33 C331 1.485(10) . ? C34 C35 1.400(10) . ? C34 C341 1.484(11) . ? C35 C351 1.472(10) . ? C41 C42 1.338(10) . ? C41 C46 1.397(9) . ? C42 C43 1.396(10) . ? C43 C44 1.381(10) . ? C44 C45 1.335(11) . ? C45 C46 1.392(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Ga1 C11 125.6(3) . . ? C21 Ga1 Cl1 108.0(2) . 2_576 ? C11 Ga1 Cl1 110.9(2) . 2_576 ? C21 Ga1 Cl1 107.8(2) . . ? C11 Ga1 Cl1 110.3(2) . . ? Cl1 Ga1 Cl1 87.59(6) 2_576 . ? C21 Ga1 C15 102.1(3) . . ? C11 Ga1 C15 35.1(2) . . ? Cl1 Ga1 C15 100.2(2) 2_576 . ? Cl1 Ga1 C15 145.0(2) . . ? C21 Ga1 C12 99.9(2) . . ? C11 Ga1 C12 36.1(2) . . ? Cl1 Ga1 C12 146.8(2) 2_576 . ? Cl1 Ga1 C12 100.7(2) . . ? C15 Ga1 C12 55.7(2) . . ? C41 Ga2 C31 125.7(3) . . ? C41 Ga2 Cl2 108.4(2) . 2_655 ? C31 Ga2 Cl2 110.1(2) . 2_655 ? C41 Ga2 Cl2 108.2(2) . . ? C31 Ga2 Cl2 110.4(2) . . ? Cl2 Ga2 Cl2 87.08(6) 2_655 . ? C41 Ga2 C35 100.8(2) . . ? C31 Ga2 C35 35.5(3) . . ? Cl2 Ga2 C35 101.0(2) 2_655 . ? Cl2 Ga2 C35 145.7(2) . . ? C41 Ga2 C32 101.2(2) . . ? C31 Ga2 C32 35.5(2) . . ? Cl2 Ga2 C32 145.3(2) 2_655 . ? Cl2 Ga2 C32 100.6(2) . . ? C35 Ga2 C32 55.1(2) . . ? Ga1 Cl1 Ga1 92.41(6) 2_576 . ? Ga2 Cl2 Ga2 92.92(6) 2_655 . ? C15 C11 C12 106.8(6) . . ? C15 C11 C111 122.3(6) . . ? C12 C11 C111 122.8(6) . . ? C15 C11 Ga1 91.0(4) . . ? C12 C11 Ga1 90.6(4) . . ? C111 C11 Ga1 114.2(5) . . ? C13 C12 C11 106.8(6) . . ? C13 C12 C121 128.7(7) . . ? C11 C12 C121 124.3(6) . . ? C13 C12 Ga1 98.3(4) . . ? C11 C12 Ga1 53.4(3) . . ? C121 C12 Ga1 113.7(5) . . ? C12 C13 C14 109.7(6) . . ? C12 C13 C131 126.1(7) . . ? C14 C13 C131 124.1(7) . . ? C15 C14 C13 108.2(6) . . ? C15 C14 C141 126.1(7) . . ? C13 C14 C141 125.7(7) . . ? C14 C15 C11 108.4(6) . . ? C14 C15 C151 126.4(7) . . ? C11 C15 C151 125.0(6) . . ? C14 C15 Ga1 99.3(4) . . ? C11 C15 Ga1 53.9(3) . . ? C151 C15 Ga1 114.6(5) . . ? C22 C21 C26 116.5(6) . . ? C22 C21 Ga1 121.6(6) . . ? C26 C21 Ga1 121.9(6) . . ? C21 C22 F22 121.1(6) . . ? C21 C22 C23 123.3(7) . . ? F22 C22 C23 115.5(6) . . ? F23 C23 C24 120.5(7) . . ? F23 C23 C22 121.6(8) . . ? C24 C23 C22 117.9(7) . . ? F24 C24 C25 119.6(8) . . ? F24 C24 C23 119.1(8) . . ? C25 C24 C23 121.3(7) . . ? F25 C25 C24 120.7(7) . . ? F25 C25 C26 121.3(8) . . ? C24 C25 C26 118.1(7) . . ? F26 C26 C21 120.2(6) . . ? F26 C26 C25 116.8(7) . . ? C21 C26 C25 122.9(7) . . ? C35 C31 C32 105.6(6) . . ? C35 C31 C311 122.6(6) . . ? C32 C31 C311 121.9(6) . . ? C35 C31 Ga2 91.8(4) . . ? C32 C31 Ga2 91.8(4) . . ? C311 C31 Ga2 115.3(5) . . ? C33 C32 C31 108.4(6) . . ? C33 C32 C321 127.5(7) . . ? C31 C32 C321 124.1(6) . . ? C33 C32 Ga2 99.8(4) . . ? C31 C32 Ga2 52.7(3) . . ? C321 C32 Ga2 112.2(4) . . ? C32 C33 C34 109.8(6) . . ? C32 C33 C331 127.0(7) . . ? C34 C33 C331 123.2(7) . . ? C35 C34 C33 108.4(6) . . ? C35 C34 C341 126.2(7) . . ? C33 C34 C341 125.3(7) . . ? C34 C35 C31 107.8(6) . . ? C34 C35 C351 128.8(8) . . ? C31 C35 C351 123.3(7) . . ? C34 C35 Ga2 99.3(4) . . ? C31 C35 Ga2 52.7(3) . . ? C351 C35 Ga2 113.5(5) . . ? C42 C41 C46 116.5(7) . . ? C42 C41 Ga2 122.2(5) . . ? C46 C41 Ga2 121.2(5) . . ? C41 C42 F42 120.6(6) . . ? C41 C42 C43 123.6(7) . . ? F42 C42 C43 115.7(7) . . ? F43 C43 C44 119.8(7) . . ? F43 C43 C42 122.0(7) . . ? C44 C43 C42 118.2(7) . . ? C45 C44 F44 121.1(7) . . ? C45 C44 C43 120.1(7) . . ? F44 C44 C43 118.8(7) . . ? C44 C45 F45 120.2(7) . . ? C44 C45 C46 120.6(7) . . ? F45 C45 C46 119.2(7) . . ? F46 C46 C45 118.6(6) . . ? F46 C46 C41 120.3(7) . . ? C45 C46 C41 121.0(7) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.458 _refine_diff_density_min -2.659 _refine_diff_density_rms 0.221