# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Hassanatu B. Mansaray' ; ? # Address for author 1 ; ; ? # Footnote for author 1 ; 'Alexander D.R. Rowe' ; ? # Address 2 ; ; ? # Footnote 2 ; 'Nicholas Phillips' '' '' 'Jochen Niemeyer' '' '' 'Michael Kelly' '' '' 'David A. Addy' '' '' 'Joshua I. Bates' '' '' 'Simon Aldridge' '' '' _publ_contact_author_address ; Chemical Crystallography Laboratory, Department of Chemistry, University of Nowhere, Nowhere, NO1 4T, UK. ; _publ_contact_author_email simon.aldridge@chem.ox.ac.uk _publ_contact_author_fax '+44 1865 000000' _publ_contact_author_phone '+44 1865 000000' _publ_contact_author_name 'Simon Aldridge' #looking for refcif # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; Please consider this CIF submission for publication as a Short Format Paper in Acta Crystallographica E. ; _publ_requested_category EO # choose from: FI FM FO CI CM CO AD _publ_requested_coeditor_name 'Prof William Clegg' _publ_section_title # Title of paper - generally just the systematic or trivial name ; ? ; data_LNHCAlCl3 _database_code_depnum_ccdc_archive 'CCDC 839365' #TrackingRef 'LNHCAlCl3.cif' _audit_creation_date 11-05-23 _audit_creation_method CRYSTALS_ver_14.06 _oxford_structure_analysis_title '5120855 041armk11' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 9.3474(2) _cell_length_b 16.2628(4) _cell_length_c 15.8953(4) _cell_angle_alpha 90 _cell_angle_beta 106.3555(11) _cell_angle_gamma 90 _cell_volume 2318.54(10) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Al 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C22 H28 Al1 Cl3 N2 # Dc = 1.30 Fooo = 952.00 Mu = 4.44 M = 453.82 # Found Formula = C22 H28 Al1 Cl3 N2 # Dc = 1.30 FOOO = 952.00 Mu = 4.44 M = 453.82 _chemical_formula_sum 'C22 H28 Al1 Cl3 N2' _chemical_formula_moiety 'C22 H28 Al1 Cl3 N2' _chemical_compound_source ? _chemical_formula_weight 453.82 _cell_measurement_reflns_used 5314 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.080 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_max 0.160 _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.444 # Sheldrick geometric approximatio 0.95 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.97 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 10229 _reflns_number_total 5285 _diffrn_reflns_av_R_equivalents 0.141 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 5285 # Theoretical number of reflections is about 10661 _diffrn_reflns_theta_min 5.136 _diffrn_reflns_theta_max 27.507 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.957 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 2.73 _oxford_diffrn_Wilson_scale 32.86 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.53 _refine_diff_density_max 0.68 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 5285 _refine_ls_number_restraints 0 _refine_ls_number_parameters 253 _oxford_refine_ls_R_factor_ref 0.0816 _refine_ls_wR_factor_ref 0.1590 _refine_ls_goodness_of_fit_ref 1.0303 _refine_ls_shift/su_max 0.0005462 _refine_ls_shift/su_mean 0.0000336 # The values computed from all data _oxford_reflns_number_all 5285 _refine_ls_R_factor_all 0.0816 _refine_ls_wR_factor_all 0.1590 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3814 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_gt 0.1440 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.10P)^2^ + 0.00P] ,where P=p(6)*max(Fo^2^,0) + (1-p(6))Fc^2^ ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cl1 Cl 0.70133(8) 0.76555(4) 0.16358(4) 0.0368 1.0000 Uani . . . . . . . Al2 Al 0.72500(8) 0.71817(4) 0.29287(5) 0.0254 1.0000 Uani . . . . . . . Cl3 Cl 0.60141(12) 0.80246(4) 0.34638(7) 0.0654 1.0000 Uani . . . . . . . Cl4 Cl 0.95632(8) 0.72157(5) 0.36129(5) 0.0475 1.0000 Uani . . . . . . . C5 C 0.6589(3) 0.59718(14) 0.30099(14) 0.0234 1.0000 Uani . . . . . . . N6 N 0.6556(2) 0.54309(12) 0.23659(13) 0.0286 1.0000 Uani . . . . . . . C7 C 0.6103(4) 0.45616(16) 0.23687(19) 0.0467 1.0000 Uani . . . . . . . C8 C 0.5112(4) 0.44432(18) 0.29570(18) 0.0473 1.0000 Uani . . . . . . . C9 C 0.5863(4) 0.48205(16) 0.38383(17) 0.0396 1.0000 Uani . . . . . . . N10 N 0.6250(2) 0.56851(12) 0.37254(12) 0.0271 1.0000 Uani . . . . . . . C11 C 0.6294(3) 0.62067(14) 0.44775(15) 0.0253 1.0000 Uani . . . . . . . C12 C 0.4968(3) 0.65498(14) 0.45470(15) 0.0254 1.0000 Uani . . . . . . . C13 C 0.3501(3) 0.64015(19) 0.38478(18) 0.0407 1.0000 Uani . . . . . . . C14 C 0.5001(3) 0.70201(15) 0.52809(16) 0.0278 1.0000 Uani . . . . . . . C15 C 0.6325(3) 0.71450(14) 0.59398(15) 0.0268 1.0000 Uani . . . . . . . C16 C 0.6363(3) 0.76767(17) 0.67232(17) 0.0393 1.0000 Uani . . . . . . . C17 C 0.7597(3) 0.67653(15) 0.58661(16) 0.0288 1.0000 Uani . . . . . . . C18 C 0.7620(3) 0.62792(15) 0.51492(16) 0.0286 1.0000 Uani . . . . . . . C19 C 0.9017(3) 0.58214(19) 0.51417(19) 0.0413 1.0000 Uani . . . . . . . C20 C 0.6956(3) 0.56483(14) 0.15817(15) 0.0254 1.0000 Uani . . . . . . . C21 C 0.8426(3) 0.55279(15) 0.15558(16) 0.0302 1.0000 Uani . . . . . . . C22 C 0.9635(3) 0.52432(19) 0.2346(2) 0.0455 1.0000 Uani . . . . . . . C23 C 0.8741(3) 0.56835(16) 0.07676(18) 0.0363 1.0000 Uani . . . . . . . C24 C 0.7662(3) 0.59460(16) 0.00304(17) 0.0351 1.0000 Uani . . . . . . . C25 C 0.8034(4) 0.6100(2) -0.0822(2) 0.0529 1.0000 Uani . . . . . . . C26 C 0.6208(3) 0.60489(15) 0.00781(16) 0.0318 1.0000 Uani . . . . . . . C27 C 0.5832(3) 0.58927(14) 0.08474(15) 0.0262 1.0000 Uani . . . . . . . C28 C 0.4257(3) 0.60360(17) 0.08793(18) 0.0366 1.0000 Uani . . . . . . . H71 H 0.6991 0.4235 0.2591 0.0578 1.0000 Uiso R . . . . . . H72 H 0.5602 0.4398 0.1777 0.0574 1.0000 Uiso R . . . . . . H81 H 0.4122 0.4693 0.2691 0.0582 1.0000 Uiso R . . . . . . H82 H 0.5045 0.3864 0.3037 0.0589 1.0000 Uiso R . . . . . . H92 H 0.6788 0.4516 0.4120 0.0487 1.0000 Uiso R . . . . . . H91 H 0.5213 0.4803 0.4219 0.0483 1.0000 Uiso R . . . . . . H131 H 0.2696 0.6707 0.3964 0.0621 1.0000 Uiso R . . . . . . H132 H 0.3619 0.6560 0.3287 0.0620 1.0000 Uiso R . . . . . . H133 H 0.3240 0.5821 0.3833 0.0629 1.0000 Uiso R . . . . . . H141 H 0.4105 0.7267 0.5323 0.0324 1.0000 Uiso R . . . . . . H161 H 0.7001 0.7450 0.7260 0.0586 1.0000 Uiso R . . . . . . H163 H 0.6736 0.8214 0.6648 0.0588 1.0000 Uiso R . . . . . . H162 H 0.5357 0.7740 0.6788 0.0587 1.0000 Uiso R . . . . . . H171 H 0.8490 0.6826 0.6312 0.0341 1.0000 Uiso R . . . . . . H191 H 0.9939 0.6133 0.5428 0.0627 1.0000 Uiso R . . . . . . H193 H 0.8988 0.5690 0.4541 0.0623 1.0000 Uiso R . . . . . . H192 H 0.9015 0.5304 0.5464 0.0623 1.0000 Uiso R . . . . . . H221 H 1.0570 0.5267 0.2213 0.0688 1.0000 Uiso R . . . . . . H223 H 0.9737 0.5586 0.2858 0.0697 1.0000 Uiso R . . . . . . H222 H 0.9488 0.4686 0.2493 0.0686 1.0000 Uiso R . . . . . . H231 H 0.9750 0.5627 0.0733 0.0432 1.0000 Uiso R . . . . . . H251 H 0.7371 0.6508 -0.1181 0.0775 1.0000 Uiso R . . . . . . H253 H 0.9051 0.6293 -0.0673 0.0780 1.0000 Uiso R . . . . . . H252 H 0.7962 0.5592 -0.1143 0.0771 1.0000 Uiso R . . . . . . H261 H 0.5459 0.6225 -0.0431 0.0397 1.0000 Uiso R . . . . . . H282 H 0.3611 0.6154 0.0313 0.0570 1.0000 Uiso R . . . . . . H281 H 0.4270 0.6512 0.1249 0.0566 1.0000 Uiso R . . . . . . H283 H 0.3884 0.5580 0.1123 0.0569 1.0000 Uiso 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 Cl1 0.0519(4) 0.0264(3) 0.0335(4) 0.0025(2) 0.0142(3) -0.0064(3) Al2 0.0296(4) 0.0194(3) 0.0315(4) -0.0021(3) 0.0158(3) -0.0013(3) Cl3 0.1085(7) 0.0263(4) 0.0958(7) 0.0143(4) 0.0851(6) 0.0205(4) Cl4 0.0353(4) 0.0541(5) 0.0489(4) -0.0059(3) 0.0049(3) -0.0156(3) C5 0.0255(12) 0.0223(11) 0.0228(11) 0.0024(9) 0.0073(9) 0.0028(9) N6 0.0458(13) 0.0192(10) 0.0254(10) -0.0016(8) 0.0174(9) -0.0040(9) C7 0.091(2) 0.0231(13) 0.0349(15) -0.0048(11) 0.0320(16) -0.0108(14) C8 0.078(2) 0.0347(14) 0.0354(15) -0.0061(12) 0.0261(15) -0.0259(15) C9 0.067(2) 0.0266(13) 0.0281(14) 0.0000(10) 0.0191(13) -0.0100(12) N10 0.0396(12) 0.0214(10) 0.0225(10) 0.0006(8) 0.0125(9) -0.0012(8) C11 0.0388(13) 0.0198(11) 0.0202(11) 0.0012(9) 0.0133(10) 0.0002(9) C12 0.0286(12) 0.0262(12) 0.0228(12) 0.0060(9) 0.0097(9) -0.0006(10) C13 0.0334(15) 0.0514(17) 0.0348(15) 0.0027(13) 0.0054(12) -0.0011(13) C14 0.0295(13) 0.0286(12) 0.0303(13) 0.0077(10) 0.0162(10) 0.0030(10) C15 0.0386(14) 0.0218(11) 0.0255(12) 0.0011(9) 0.0180(10) -0.0007(10) C16 0.0541(17) 0.0361(15) 0.0340(15) -0.0090(12) 0.0225(13) -0.0036(12) C17 0.0299(13) 0.0290(12) 0.0251(12) 0.0007(10) 0.0037(10) 0.0008(10) C18 0.0310(13) 0.0275(12) 0.0278(12) 0.0030(10) 0.0093(10) 0.0066(10) C19 0.0385(15) 0.0470(16) 0.0370(15) -0.0022(13) 0.0083(12) 0.0171(13) C20 0.0372(14) 0.0182(11) 0.0249(12) 0.0003(9) 0.0154(10) -0.0003(9) C21 0.0355(14) 0.0243(11) 0.0318(13) -0.0061(10) 0.0113(11) 0.0014(10) C22 0.0452(17) 0.0413(16) 0.0469(17) -0.0086(13) 0.0082(13) 0.0114(13) C23 0.0349(14) 0.0343(14) 0.0456(16) -0.0129(12) 0.0214(12) -0.0051(11) C24 0.0499(16) 0.0324(13) 0.0295(13) -0.0088(11) 0.0218(12) -0.0133(12) C25 0.078(2) 0.0530(19) 0.0412(17) -0.0090(14) 0.0394(17) -0.0233(17) C26 0.0428(15) 0.0265(13) 0.0261(12) -0.0012(10) 0.0098(11) -0.0078(11) C27 0.0342(13) 0.0198(11) 0.0272(12) -0.0013(9) 0.0125(10) -0.0012(10) C28 0.0356(15) 0.0342(14) 0.0417(15) -0.0009(11) 0.0136(12) -0.0006(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2800(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 . Al2 . 2.1471(9) yes Al2 . Cl3 . 2.1191(10) yes Al2 . Cl4 . 2.1300(10) yes Al2 . C5 . 2.077(2) yes C5 . N6 . 1.343(3) yes C5 . N10 . 1.347(3) yes N6 . C7 . 1.476(3) yes N6 . C20 . 1.443(3) yes C7 . C8 . 1.502(4) yes C7 . H71 . 0.965 no C7 . H72 . 0.963 no C8 . C9 . 1.509(4) yes C8 . H81 . 0.990 no C8 . H82 . 0.955 no C9 . N10 . 1.476(3) yes C9 . H92 . 0.988 no C9 . H91 . 0.971 no N10 . C11 . 1.457(3) yes C11 . C12 . 1.392(3) yes C11 . C18 . 1.394(3) yes C12 . C13 . 1.521(3) yes C12 . C14 . 1.388(3) yes C13 . H131 . 0.962 no C13 . H132 . 0.963 no C13 . H133 . 0.974 no C14 . C15 . 1.392(3) yes C14 . H141 . 0.949 no C15 . C16 . 1.508(3) yes C15 . C17 . 1.374(4) yes C16 . H161 . 0.967 no C16 . H163 . 0.961 no C16 . H162 . 0.980 no C17 . C18 . 1.392(3) yes C17 . H171 . 0.936 no C18 . C19 . 1.506(4) yes C19 . H191 . 0.993 no C19 . H193 . 0.971 no C19 . H192 . 0.986 no C20 . C21 . 1.400(4) yes C20 . C27 . 1.391(3) yes C21 . C22 . 1.507(4) yes C21 . C23 . 1.388(4) yes C22 . H221 . 0.955 no C22 . H223 . 0.969 no C22 . H222 . 0.955 no C23 . C24 . 1.381(4) yes C23 . H231 . 0.965 no C24 . C25 . 1.512(3) yes C24 . C26 . 1.392(4) yes C25 . H251 . 0.975 no C25 . H253 . 0.965 no C25 . H252 . 0.963 no C26 . C27 . 1.387(3) yes C26 . H261 . 0.953 no C27 . C28 . 1.505(4) yes C28 . H282 . 0.952 no C28 . H281 . 0.970 no C28 . H283 . 0.947 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Al2 . Cl3 . 103.37(4) yes Cl1 . Al2 . Cl4 . 107.19(4) yes Cl3 . Al2 . Cl4 . 111.59(5) yes Cl1 . Al2 . C5 . 116.56(7) yes Cl3 . Al2 . C5 . 112.49(7) yes Cl4 . Al2 . C5 . 105.65(7) yes Al2 . C5 . N6 . 121.09(16) yes Al2 . C5 . N10 . 121.68(16) yes N6 . C5 . N10 . 117.1(2) yes C5 . N6 . C7 . 124.75(19) yes C5 . N6 . C20 . 122.81(19) yes C7 . N6 . C20 . 112.44(18) yes N6 . C7 . C8 . 110.6(2) yes N6 . C7 . H71 . 108.1 no C8 . C7 . H71 . 108.6 no N6 . C7 . H72 . 108.8 no C8 . C7 . H72 . 111.0 no H71 . C7 . H72 . 109.7 no C7 . C8 . C9 . 108.6(2) yes C7 . C8 . H81 . 110.3 no C9 . C8 . H81 . 111.4 no C7 . C8 . H82 . 106.5 no C9 . C8 . H82 . 108.0 no H81 . C8 . H82 . 111.9 no C8 . C9 . N10 . 109.9(2) yes C8 . C9 . H92 . 109.7 no N10 . C9 . H92 . 108.6 no C8 . C9 . H91 . 110.9 no N10 . C9 . H91 . 108.8 no H92 . C9 . H91 . 108.9 no C9 . N10 . C5 . 123.8(2) yes C9 . N10 . C11 . 113.97(18) yes C5 . N10 . C11 . 122.16(19) yes N10 . C11 . C12 . 118.6(2) yes N10 . C11 . C18 . 119.4(2) yes C12 . C11 . C18 . 121.6(2) yes C11 . C12 . C13 . 121.2(2) yes C11 . C12 . C14 . 118.5(2) yes C13 . C12 . C14 . 120.3(2) yes C12 . C13 . H131 . 111.7 no C12 . C13 . H132 . 108.6 no H131 . C13 . H132 . 109.8 no C12 . C13 . H133 . 109.8 no H131 . C13 . H133 . 107.6 no H132 . C13 . H133 . 109.3 no C12 . C14 . C15 . 121.2(2) yes C12 . C14 . H141 . 118.8 no C15 . C14 . H141 . 120.0 no C14 . C15 . C16 . 121.0(2) yes C14 . C15 . C17 . 118.5(2) yes C16 . C15 . C17 . 120.5(2) yes C15 . C16 . H161 . 112.1 no C15 . C16 . H163 . 110.1 no H161 . C16 . H163 . 107.6 no C15 . C16 . H162 . 110.3 no H161 . C16 . H162 . 108.5 no H163 . C16 . H162 . 108.1 no C15 . C17 . C18 . 122.6(2) yes C15 . C17 . H171 . 119.8 no C18 . C17 . H171 . 117.6 no C11 . C18 . C17 . 117.4(2) yes C11 . C18 . C19 . 122.5(2) yes C17 . C18 . C19 . 120.0(2) yes C18 . C19 . H191 . 112.7 no C18 . C19 . H193 . 109.4 no H191 . C19 . H193 . 110.1 no C18 . C19 . H192 . 106.8 no H191 . C19 . H192 . 109.0 no H193 . C19 . H192 . 108.7 no N6 . C20 . C21 . 119.1(2) yes N6 . C20 . C27 . 118.5(2) yes C21 . C20 . C27 . 122.1(2) yes C20 . C21 . C22 . 122.1(2) yes C20 . C21 . C23 . 117.4(2) yes C22 . C21 . C23 . 120.5(2) yes C21 . C22 . H221 . 108.8 no C21 . C22 . H223 . 113.3 no H221 . C22 . H223 . 106.4 no C21 . C22 . H222 . 111.7 no H221 . C22 . H222 . 107.3 no H223 . C22 . H222 . 109.1 no C21 . C23 . C24 . 122.2(2) yes C21 . C23 . H231 . 119.5 no C24 . C23 . H231 . 118.3 no C23 . C24 . C25 . 121.0(3) yes C23 . C24 . C26 . 118.8(2) yes C25 . C24 . C26 . 120.2(3) yes C24 . C25 . H251 . 111.6 no C24 . C25 . H253 . 107.1 no H251 . C25 . H253 . 110.0 no C24 . C25 . H252 . 109.5 no H251 . C25 . H252 . 109.6 no H253 . C25 . H252 . 109.0 no C24 . C26 . C27 . 121.3(2) yes C24 . C26 . H261 . 119.0 no C27 . C26 . H261 . 119.7 no C20 . C27 . C26 . 118.2(2) yes C20 . C27 . C28 . 122.1(2) yes C26 . C27 . C28 . 119.6(2) yes C27 . C28 . H282 . 111.4 no C27 . C28 . H281 . 107.4 no H282 . C28 . H281 . 108.0 no C27 . C28 . H283 . 111.6 no H282 . C28 . H283 . 109.6 no H281 . C28 . H283 . 108.6 no # Attachment 'LNHCBBr3.cif' data_LNHCBBr3 _database_code_depnum_ccdc_archive 'CCDC 839366' #TrackingRef 'LNHCBBr3.cif' _audit_creation_date 11-04-20 _audit_creation_method CRYSTALS_ver_14.06 _oxford_structure_analysis_title '4191413 008arnp11' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 8.27310(10) _cell_length_b 16.7816(2) _cell_length_c 16.7028(3) _cell_angle_alpha 90 _cell_angle_beta 92.0275(6) _cell_angle_gamma 90 _cell_volume 2317.50(6) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C22 H28 B1 Br3 N2 # Dc = 1.64 Fooo = 1136.00 Mu = 52.33 M = 571.00 # Found Formula = C22 H28 B1 Br3 N2 # Dc = 1.64 FOOO = 1136.00 Mu = 52.33 M = 571.00 _chemical_formula_sum 'C22 H28 B1 Br3 N2' _chemical_formula_moiety 'C22 H28 B1 Br3 N2' _chemical_compound_source ? _chemical_formula_weight 571.00 _cell_measurement_reflns_used 4683 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.200 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_max 0.300 _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 5.233 # Sheldrick geometric approximatio 0.28 0.35 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.29 _exptl_absorpt_correction_T_max 0.35 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 16415 _reflns_number_total 5207 _diffrn_reflns_av_R_equivalents 0.026 # Number of reflections without Friedels Law is 8989 # Number of reflections with Friedels Law is 5207 # Theoretical number of reflections is about 5310 _diffrn_reflns_theta_min 5.104 _diffrn_reflns_theta_max 27.473 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.275 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 2.20 _oxford_diffrn_Wilson_scale 19.99 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.89 _refine_diff_density_max 0.88 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 5207 _refine_ls_number_restraints 0 _refine_ls_number_parameters 254 _oxford_refine_ls_R_factor_ref 0.0498 _refine_ls_wR_factor_ref 0.0838 _refine_ls_goodness_of_fit_ref 0.8767 _refine_ls_shift/su_max 0.0011291 _refine_ls_shift/su_mean 0.0000211 # The values computed from all data _oxford_reflns_number_all 5207 _refine_ls_R_factor_all 0.0498 _refine_ls_wR_factor_all 0.0838 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4167 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_gt 0.0701 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 15.4 21.4 10.2 2.62 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Br1 Br 0.02603(4) 0.32327(2) 0.36002(2) 0.0279 1.0000 Uani . . . . . . . B2 B 0.0701(5) 0.2454(2) 0.4522(2) 0.0203 1.0000 Uani . . . . . . . Br3 Br -0.05331(4) 0.14479(2) 0.42506(2) 0.0288 1.0000 Uani . . . . . . . Br4 Br -0.03754(5) 0.28692(3) 0.55017(2) 0.0355 1.0000 Uani . . . . . . . C5 C 0.2717(4) 0.2415(2) 0.45596(19) 0.0184 1.0000 Uani . . . . . . . N6 N 0.3528(3) 0.18530(18) 0.41733(18) 0.0209 1.0000 Uani . . . . . . . C7 C 0.2891(4) 0.1117(2) 0.3833(2) 0.0214 1.0000 Uani . . . . . . . C8 C 0.2574(5) 0.1068(2) 0.3008(2) 0.0259 1.0000 Uani . . . . . . . C9 C 0.2793(6) 0.1765(3) 0.2458(2) 0.0370 1.0000 Uani . . . . . . . C10 C 0.2018(5) 0.0348(3) 0.2697(2) 0.0341 1.0000 Uani . . . . . . . C11 C 0.1829(5) -0.0319(2) 0.3178(3) 0.0325 1.0000 Uani . . . . . . . C12 C 0.2245(5) -0.0259(2) 0.3991(2) 0.0307 1.0000 Uani . . . . . . . C13 C 0.2771(4) 0.0452(2) 0.4334(2) 0.0258 1.0000 Uani . . . . . . . C14 C 0.3095(5) 0.0500(3) 0.5224(2) 0.0334 1.0000 Uani . . . . . . . C15 C 0.1204(7) -0.1092(3) 0.2826(3) 0.0517 1.0000 Uani . . . . . . . C16 C 0.5303(4) 0.1895(2) 0.4092(3) 0.0339 1.0000 Uani . . . . . . . C17 C 0.5807(4) 0.2752(2) 0.3987(3) 0.0311 1.0000 Uani . . . . . . . C18 C 0.5284(5) 0.3189(3) 0.4711(3) 0.0416 1.0000 Uani . . . . . . . N19 N 0.3574(3) 0.30315(19) 0.48773(19) 0.0245 1.0000 Uani . . . . . . . C20 C 0.3074(4) 0.3540(2) 0.5528(2) 0.0265 1.0000 Uani . . . . . . . C21 C 0.2710(4) 0.4344(2) 0.5389(2) 0.0274 1.0000 Uani . . . . . . . C22 C 0.2349(5) 0.4810(3) 0.6050(2) 0.0322 1.0000 Uani . . . . . . . C23 C 0.2401(5) 0.4510(3) 0.6826(3) 0.0362 1.0000 Uani . . . . . . . C24 C 0.2855(6) 0.3722(3) 0.6943(2) 0.0381 1.0000 Uani . . . . . . . C25 C 0.3202(5) 0.3225(3) 0.6305(2) 0.0334 1.0000 Uani . . . . . . . C26 C 0.3628(7) 0.2365(3) 0.6454(3) 0.0481 1.0000 Uani . . . . . . . C27 C 0.1985(7) 0.5021(3) 0.7537(3) 0.0497 1.0000 Uani . . . . . . . C28 C 0.2701(5) 0.4720(3) 0.4572(2) 0.0326 1.0000 Uani . . . . . . . H91 H 0.2322 0.1628 0.1937 0.0564 1.0000 Uiso R . . . . . . H93 H 0.3925 0.1861 0.2421 0.0567 1.0000 Uiso R . . . . . . H92 H 0.2300 0.2238 0.2671 0.0571 1.0000 Uiso R . . . . . . H101 H 0.1778 0.0313 0.2157 0.0421 1.0000 Uiso R . . . . . . H121 H 0.2160 -0.0721 0.4316 0.0383 1.0000 Uiso R . . . . . . H141 H 0.3210 -0.0038 0.5432 0.0529 1.0000 Uiso R . . . . . . H142 H 0.4071 0.0801 0.5337 0.0520 1.0000 Uiso R . . . . . . H143 H 0.2214 0.0750 0.5463 0.0524 1.0000 Uiso R . . . . . . H152 H 0.1245 -0.1504 0.3225 0.0763 1.0000 Uiso R . . . . . . H151 H 0.1870 -0.1249 0.2392 0.0759 1.0000 Uiso R . . . . . . H153 H 0.0110 -0.1029 0.2630 0.0766 1.0000 Uiso R . . . . . . H162 H 0.5839 0.1682 0.4573 0.0446 1.0000 Uiso R . . . . . . H161 H 0.5609 0.1578 0.3634 0.0443 1.0000 Uiso R . . . . . . H171 H 0.6973 0.2805 0.3952 0.0377 1.0000 Uiso R . . . . . . H172 H 0.5283 0.2980 0.3501 0.0359 1.0000 Uiso R . . . . . . H182 H 0.5960 0.3043 0.5184 0.0522 1.0000 Uiso R . . . . . . H181 H 0.5389 0.3753 0.4621 0.0518 1.0000 Uiso R . . . . . . H221 H 0.2060 0.5359 0.5964 0.0395 1.0000 Uiso R . . . . . . H241 H 0.2941 0.3505 0.7451 0.0489 1.0000 Uiso R . . . . . . H261 H 0.3696 0.2270 0.7027 0.0759 1.0000 Uiso R . . . . . . H262 H 0.4639 0.2231 0.6210 0.0761 1.0000 Uiso R . . . . . . H263 H 0.2793 0.2034 0.6222 0.0764 1.0000 Uiso R . . . . . . H272 H 0.2725 0.4879 0.7981 0.0711 1.0000 Uiso R . . . . . . H271 H 0.2077 0.5568 0.7392 0.0709 1.0000 Uiso R . . . . . . H273 H 0.0885 0.4899 0.7667 0.0712 1.0000 Uiso R . . . . . . H282 H 0.1924 0.5146 0.4541 0.0518 1.0000 Uiso R . . . . . . H281 H 0.3760 0.4929 0.4491 0.0525 1.0000 Uiso R . . . . . . H283 H 0.2497 0.4326 0.4172 0.0512 1.0000 Uiso 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 Br1 0.02165(17) 0.0329(2) 0.02867(19) 0.00974(15) -0.00480(13) -0.00058(15) B2 0.0190(17) 0.0226(19) 0.0193(17) -0.0007(14) 0.0003(13) 0.0031(15) Br3 0.01750(16) 0.02611(19) 0.0430(2) -0.00265(16) 0.00341(14) -0.00292(14) Br4 0.02423(19) 0.0570(3) 0.02575(19) -0.01316(18) 0.00741(14) -0.00119(17) C5 0.0162(14) 0.0221(17) 0.0168(15) 0.0016(12) 0.0005(11) -0.0001(13) N6 0.0146(13) 0.0197(15) 0.0283(15) -0.0004(12) 0.0020(11) 0.0012(11) C7 0.0191(15) 0.0169(16) 0.0284(17) 0.0004(14) 0.0054(13) 0.0007(13) C8 0.0307(18) 0.0254(19) 0.0223(17) -0.0019(14) 0.0086(14) -0.0020(15) C9 0.058(3) 0.030(2) 0.0237(18) 0.0040(16) 0.0113(18) 0.003(2) C10 0.045(2) 0.032(2) 0.0251(19) -0.0072(16) 0.0107(17) -0.0014(18) C11 0.039(2) 0.0238(19) 0.036(2) -0.0093(16) 0.0157(17) -0.0028(17) C12 0.039(2) 0.0210(19) 0.033(2) 0.0054(15) 0.0112(16) 0.0022(16) C13 0.0264(18) 0.0249(19) 0.0264(18) 0.0028(15) 0.0066(14) 0.0047(14) C14 0.042(2) 0.030(2) 0.0278(19) 0.0052(16) -0.0003(17) 0.0050(17) C15 0.072(3) 0.030(2) 0.055(3) -0.018(2) 0.019(3) -0.016(2) C16 0.0131(16) 0.031(2) 0.058(3) -0.0064(19) 0.0073(16) -0.0007(14) C17 0.0177(17) 0.031(2) 0.045(2) 0.0042(17) 0.0055(15) -0.0011(15) C18 0.0195(18) 0.039(2) 0.066(3) -0.020(2) 0.0004(18) -0.0097(17) N19 0.0147(13) 0.0281(16) 0.0306(16) -0.0055(13) -0.0009(11) -0.0004(11) C20 0.0231(17) 0.0284(19) 0.0275(18) -0.0071(15) -0.0060(14) 0.0002(15) C21 0.0236(17) 0.027(2) 0.0307(19) -0.0039(15) -0.0032(14) -0.0033(15) C22 0.033(2) 0.029(2) 0.034(2) -0.0038(16) 0.0001(16) 0.0016(16) C23 0.041(2) 0.037(2) 0.031(2) -0.0086(18) -0.0015(17) -0.0016(18) C24 0.048(3) 0.042(2) 0.0233(19) -0.0046(17) -0.0102(17) -0.002(2) C25 0.040(2) 0.032(2) 0.0279(19) -0.0028(16) -0.0124(16) 0.0017(18) C26 0.071(3) 0.038(3) 0.033(2) -0.0012(19) -0.024(2) 0.014(2) C27 0.063(3) 0.048(3) 0.038(2) -0.013(2) 0.004(2) 0.003(2) C28 0.039(2) 0.028(2) 0.031(2) -0.0017(16) 0.0018(16) -0.0039(17) _refine_ls_extinction_coef 71(5) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.22964(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 . B2 . 2.042(4) yes B2 . Br3 . 2.017(4) yes B2 . Br4 . 2.015(4) yes B2 . C5 . 1.668(5) yes C5 . N6 . 1.337(4) yes C5 . N19 . 1.352(5) yes N6 . C7 . 1.451(4) yes N6 . C16 . 1.481(4) yes C7 . C8 . 1.395(5) yes C7 . C13 . 1.400(5) yes C8 . C9 . 1.503(5) yes C8 . C10 . 1.387(6) yes C9 . H91 . 0.970 no C9 . H93 . 0.955 no C9 . H92 . 0.966 no C10 . C11 . 1.391(6) yes C10 . H101 . 0.918 no C11 . C12 . 1.393(6) yes C11 . C15 . 1.508(6) yes C12 . C13 . 1.388(6) yes C12 . H121 . 0.950 no C13 . C14 . 1.504(5) yes C14 . H141 . 0.970 no C14 . H142 . 0.964 no C14 . H143 . 0.941 no C15 . H152 . 0.960 no C15 . H151 . 0.962 no C15 . H153 . 0.957 no C16 . C17 . 1.510(6) yes C16 . H162 . 0.973 no C16 . H161 . 0.972 no C17 . C18 . 1.491(6) yes C17 . H171 . 0.973 no C17 . H172 . 0.984 no C18 . N19 . 1.476(5) yes C18 . H182 . 0.983 no C18 . H181 . 0.962 no N19 . C20 . 1.453(5) yes C20 . C21 . 1.399(6) yes C20 . C25 . 1.403(5) yes C21 . C22 . 1.395(5) yes C21 . C28 . 1.503(5) yes C22 . C23 . 1.389(6) yes C22 . H221 . 0.961 no C23 . C24 . 1.387(6) yes C23 . C27 . 1.515(6) yes C24 . C25 . 1.389(6) yes C24 . H241 . 0.925 no C25 . C26 . 1.506(6) yes C26 . H261 . 0.969 no C26 . H262 . 0.970 no C26 . H263 . 0.957 no C27 . H272 . 0.975 no C27 . H271 . 0.952 no C27 . H273 . 0.965 no C28 . H282 . 0.963 no C28 . H281 . 0.958 no C28 . H283 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 . B2 . Br3 . 106.91(17) yes Br1 . B2 . Br4 . 108.62(18) yes Br3 . B2 . Br4 . 103.70(17) yes Br1 . B2 . C5 . 101.9(2) yes Br3 . B2 . C5 . 118.2(2) yes Br4 . B2 . C5 . 116.9(2) yes B2 . C5 . N6 . 121.9(3) yes B2 . C5 . N19 . 119.6(3) yes N6 . C5 . N19 . 117.7(3) yes C5 . N6 . C7 . 127.4(3) yes C5 . N6 . C16 . 121.8(3) yes C7 . N6 . C16 . 110.6(3) yes N6 . C7 . C8 . 119.4(3) yes N6 . C7 . C13 . 118.4(3) yes C8 . C7 . C13 . 121.9(3) yes C7 . C8 . C9 . 122.3(3) yes C7 . C8 . C10 . 118.0(3) yes C9 . C8 . C10 . 119.6(4) yes C8 . C9 . H91 . 108.1 no C8 . C9 . H93 . 108.2 no H91 . C9 . H93 . 110.2 no C8 . C9 . H92 . 110.7 no H91 . C9 . H92 . 111.4 no H93 . C9 . H92 . 108.3 no C8 . C10 . C11 . 121.8(4) yes C8 . C10 . H101 . 118.8 no C11 . C10 . H101 . 119.4 no C10 . C11 . C12 . 118.5(4) yes C10 . C11 . C15 . 120.8(4) yes C12 . C11 . C15 . 120.8(4) yes C11 . C12 . C13 . 121.8(4) yes C11 . C12 . H121 . 118.5 no C13 . C12 . H121 . 119.6 no C7 . C13 . C12 . 117.8(3) yes C7 . C13 . C14 . 122.3(4) yes C12 . C13 . C14 . 119.7(3) yes C13 . C14 . H141 . 108.3 no C13 . C14 . H142 . 109.8 no H141 . C14 . H142 . 110.3 no C13 . C14 . H143 . 109.2 no H141 . C14 . H143 . 109.3 no H142 . C14 . H143 . 109.9 no C11 . C15 . H152 . 110.1 no C11 . C15 . H151 . 109.3 no H152 . C15 . H151 . 108.7 no C11 . C15 . H153 . 110.2 no H152 . C15 . H153 . 109.1 no H151 . C15 . H153 . 109.4 no N6 . C16 . C17 . 109.5(3) yes N6 . C16 . H162 . 109.3 no C17 . C16 . H162 . 109.1 no N6 . C16 . H161 . 109.4 no C17 . C16 . H161 . 110.5 no H162 . C16 . H161 . 109.0 no C16 . C17 . C18 . 106.6(4) yes C16 . C17 . H171 . 111.8 no C18 . C17 . H171 . 108.7 no C16 . C17 . H172 . 110.5 no C18 . C17 . H172 . 110.2 no H171 . C17 . H172 . 108.9 no C17 . C18 . N19 . 111.9(3) yes C17 . C18 . H182 . 110.8 no N19 . C18 . H182 . 109.0 no C17 . C18 . H181 . 109.1 no N19 . C18 . H181 . 107.4 no H182 . C18 . H181 . 108.6 no C18 . N19 . C5 . 123.8(3) yes C18 . N19 . C20 . 109.6(3) yes C5 . N19 . C20 . 125.7(3) yes N19 . C20 . C21 . 120.5(3) yes N19 . C20 . C25 . 117.2(3) yes C21 . C20 . C25 . 121.7(4) yes C20 . C21 . C22 . 117.4(4) yes C20 . C21 . C28 . 123.3(4) yes C22 . C21 . C28 . 119.3(4) yes C21 . C22 . C23 . 122.3(4) yes C21 . C22 . H221 . 118.6 no C23 . C22 . H221 . 119.1 no C22 . C23 . C24 . 118.4(4) yes C22 . C23 . C27 . 121.7(4) yes C24 . C23 . C27 . 119.8(4) yes C23 . C24 . C25 . 121.7(4) yes C23 . C24 . H241 . 121.1 no C25 . C24 . H241 . 117.2 no C20 . C25 . C24 . 118.2(4) yes C20 . C25 . C26 . 121.6(4) yes C24 . C25 . C26 . 120.2(4) yes C25 . C26 . H261 . 109.0 no C25 . C26 . H262 . 110.7 no H261 . C26 . H262 . 110.9 no C25 . C26 . H263 . 109.1 no H261 . C26 . H263 . 108.7 no H262 . C26 . H263 . 108.5 no C23 . C27 . H272 . 107.7 no C23 . C27 . H271 . 108.9 no H272 . C27 . H271 . 112.0 no C23 . C27 . H273 . 107.3 no H272 . C27 . H273 . 110.4 no H271 . C27 . H273 . 110.3 no C21 . C28 . H282 . 110.1 no C21 . C28 . H281 . 107.9 no H282 . C28 . H281 . 109.4 no C21 . C28 . H283 . 110.0 no H282 . C28 . H283 . 112.1 no H281 . C28 . H283 . 107.3 no # Attachment 'LNHCGaCl3.cif' data_LNHCGaCl3 _database_code_depnum_ccdc_archive 'CCDC 839367' #TrackingRef 'LNHCGaCl3.cif' _audit_creation_date 11-04-27 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title '4271304 003arir11' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; #--------------------------------------------------------------- # _oxford_ data items, April 2010: # There is some uncertainty about the correct way of forming local data # names, e.g. # _atom_site_special_shape_oxford # or # _oxford_atom_site_special_shape # see: # http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace # A reserved prefix, e.g. foo, must be used in the following way # " If the data file contains items defined in a DDL1 dictionary, the # local data names assigned under the reserved prefix must contain it as # their first component, e.g. _foo_atom_site_my_item. " # However, this seems to say the opposite: # http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html # According to advice from the IUCr, CRYSTALS is correct #--------------------------------------------------------------- # End of 'script/refcif.dat' #end of refcif _cell_length_a 9.37090(10) _cell_length_b 16.2052(2) _cell_length_c 15.8875(2) _cell_angle_alpha 90 _cell_angle_beta 106.2708(7) _cell_angle_gamma 90 _cell_volume 2316.00(5) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ga 0.2307 1.6083 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C22 H28 Cl3 Ga1 N2 # Dc = 1.42 Fooo = 1024.00 Mu = 15.45 M = 496.56 # Found Formula = C22 H28 Cl3 Ga1 N2 # Dc = 1.42 FOOO = 1024.00 Mu = 15.45 M = 496.56 _chemical_formula_sum 'C22 H28 Cl3 Ga1 N2' _chemical_formula_moiety 'C22 H28 Cl3 Ga1 N2' _chemical_compound_source ? _chemical_formula_weight 496.56 _cell_measurement_reflns_used 5410 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.080 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.100 _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.545 # Sheldrick geometric approximatio 0.86 0.88 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.88 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 30498 _reflns_number_total 5271 _diffrn_reflns_av_R_equivalents 0.044 # Number of reflections without Friedels Law is 10047 # Number of reflections with Friedels Law is 5271 # Theoretical number of reflections is about 5304 _diffrn_reflns_theta_min 5.130 _diffrn_reflns_theta_max 27.468 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.919 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 2.29 _oxford_diffrn_Wilson_scale 38.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.08 _refine_diff_density_max 1.16 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 5271 _refine_ls_number_restraints 0 _refine_ls_number_parameters 253 _oxford_refine_ls_R_factor_ref 0.0795 _refine_ls_wR_factor_ref 0.1220 _refine_ls_goodness_of_fit_ref 0.9731 _refine_ls_shift/su_max 0.0011111 _refine_ls_shift/su_mean 0.0000305 # The values computed from all data _oxford_reflns_number_all 5271 _refine_ls_R_factor_all 0.0795 _refine_ls_wR_factor_all 0.1220 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3469 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_gt 0.0846 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 6.99 9.65 4.77 1.37 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ga1 Ga 0.77588(5) 0.71586(2) 0.70774(3) 0.0242 1.0000 Uani . . . . . . Cl2 Cl 0.79947(13) 0.76717(6) 0.83852(7) 0.0360 1.0000 Uani . . . . . . Cl3 Cl 0.53949(12) 0.72260(8) 0.63991(8) 0.0451 1.0000 Uani . . . . . . Cl4 Cl 0.8953(2) 0.80523(7) 0.65195(11) 0.0664 1.0000 Uani . . . . . . C5 C 0.8408(4) 0.5951(2) 0.6993(2) 0.0213 1.0000 Uani . . . . . . N6 N 0.8739(4) 0.56793(19) 0.6275(2) 0.0258 1.0000 Uani . . . . . . C7 C 0.8702(4) 0.6200(2) 0.5531(2) 0.0222 1.0000 Uani . . . . . . C8 C 1.0032(4) 0.6548(2) 0.5467(3) 0.0247 1.0000 Uani . . . . . . C9 C 0.9991(4) 0.7025(2) 0.4731(2) 0.0256 1.0000 Uani . . . . . . C10 C 0.8681(4) 0.7151(2) 0.4072(2) 0.0261 1.0000 Uani . . . . . . C11 C 0.7399(5) 0.6766(3) 0.4138(3) 0.0298 1.0000 Uani . . . . . . C12 C 0.7386(4) 0.6281(2) 0.4863(3) 0.0268 1.0000 Uani . . . . . . C13 C 0.5997(5) 0.5821(3) 0.4867(3) 0.0402 1.0000 Uani . . . . . . C14 C 0.8651(5) 0.7687(3) 0.3292(3) 0.0362 1.0000 Uani . . . . . . C15 C 1.1474(5) 0.6408(3) 0.6165(3) 0.0398 1.0000 Uani . . . . . . C16 C 0.9117(6) 0.4804(2) 0.6160(3) 0.0352 1.0000 Uani . . . . . . C17 C 0.9854(6) 0.4425(3) 0.7039(3) 0.0433 1.0000 Uani . . . . . . C18 C 0.8888(6) 0.4544(3) 0.7635(3) 0.0404 1.0000 Uani . . . . . . N19 N 0.8440(4) 0.54234(18) 0.7640(2) 0.0263 1.0000 Uani . . . . . . C20 C 0.8039(4) 0.5642(2) 0.8424(2) 0.0240 1.0000 Uani . . . . . . C21 C 0.6575(5) 0.5522(2) 0.8448(3) 0.0281 1.0000 Uani . . . . . . C22 C 0.5366(5) 0.5238(3) 0.7659(3) 0.0396 1.0000 Uani . . . . . . C23 C 0.6258(5) 0.5682(3) 0.9241(3) 0.0332 1.0000 Uani . . . . . . C24 C 0.7338(5) 0.5941(3) 0.9977(3) 0.0333 1.0000 Uani . . . . . . C25 C 0.8785(5) 0.6049(2) 0.9923(3) 0.0304 1.0000 Uani . . . . . . C26 C 0.9165(4) 0.5893(2) 0.9155(3) 0.0251 1.0000 Uani . . . . . . C27 C 1.0731(5) 0.6037(3) 0.9118(3) 0.0347 1.0000 Uani . . . . . . C28 C 0.6974(7) 0.6101(3) 1.0831(3) 0.0480 1.0000 Uani . . . . . . H91 H 1.0871 0.7267 0.4682 0.0308 1.0000 Uiso R . . . . . H111 H 0.6510 0.6828 0.3685 0.0360 1.0000 Uiso R . . . . . H131 H 0.5139 0.6127 0.4557 0.0603 1.0000 Uiso R . . . . . H132 H 0.5942 0.5726 0.5453 0.0602 1.0000 Uiso R . . . . . H133 H 0.5976 0.5298 0.4583 0.0603 1.0000 Uiso R . . . . . H141 H 0.8009 0.7439 0.2771 0.0551 1.0000 Uiso R . . . . . H142 H 0.8272 0.8225 0.3370 0.0551 1.0000 Uiso R . . . . . H143 H 0.9638 0.7740 0.3227 0.0550 1.0000 Uiso R . . . . . H152 H 1.2240 0.6741 0.6047 0.0599 1.0000 Uiso R . . . . . H151 H 1.1363 0.6554 0.6726 0.0604 1.0000 Uiso R . . . . . H153 H 1.1760 0.5836 0.6178 0.0602 1.0000 Uiso R . . . . . H162 H 0.9799 0.4792 0.5795 0.0420 1.0000 Uiso R . . . . . H161 H 0.8216 0.4498 0.5869 0.0425 1.0000 Uiso R . . . . . H171 H 1.0807 0.4689 0.7287 0.0516 1.0000 Uiso R . . . . . H172 H 1.0002 0.3838 0.6961 0.0521 1.0000 Uiso R . . . . . H182 H 0.9428 0.4386 0.8227 0.0491 1.0000 Uiso R . . . . . H181 H 0.7995 0.4209 0.7431 0.0491 1.0000 Uiso R . . . . . H221 H 0.4405 0.5269 0.7761 0.0606 1.0000 Uiso R . . . . . H223 H 0.5341 0.5566 0.7153 0.0604 1.0000 Uiso R . . . . . H222 H 0.5533 0.4682 0.7524 0.0602 1.0000 Uiso R . . . . . H231 H 0.5289 0.5604 0.9274 0.0403 1.0000 Uiso R . . . . . H251 H 0.9522 0.6231 1.0415 0.0370 1.0000 Uiso R . . . . . H272 H 1.1370 0.6150 0.9693 0.0522 1.0000 Uiso R . . . . . H271 H 1.0761 0.6496 0.8737 0.0523 1.0000 Uiso R . . . . . H273 H 1.1084 0.5556 0.8887 0.0525 1.0000 Uiso R . . . . . H282 H 0.7646 0.6503 1.1176 0.0725 1.0000 Uiso R . . . . . H281 H 0.5974 0.6304 1.0708 0.0723 1.0000 Uiso R . . . . . H283 H 0.7044 0.5596 1.1150 0.0720 1.0000 Uiso 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 0.0286(2) 0.01742(18) 0.0305(2) 0.00160(18) 0.01500(16) 0.00091(17) Cl2 0.0509(6) 0.0260(5) 0.0317(5) -0.0035(4) 0.0128(4) 0.0061(4) Cl3 0.0340(6) 0.0507(7) 0.0471(6) 0.0061(5) 0.0055(5) 0.0136(5) Cl4 0.1115(12) 0.0248(5) 0.0986(11) -0.0146(6) 0.0883(11) -0.0217(6) C5 0.0233(18) 0.0181(16) 0.0231(18) 0.0015(14) 0.0076(14) 0.0000(13) N6 0.0403(19) 0.0174(14) 0.0225(16) 0.0005(12) 0.0134(14) 0.0028(13) C7 0.030(2) 0.0176(16) 0.0197(18) -0.0002(13) 0.0084(15) -0.0012(14) C8 0.0244(18) 0.0260(18) 0.0244(19) -0.0036(15) 0.0081(15) 0.0000(15) C9 0.0281(19) 0.0253(19) 0.0277(19) -0.0044(15) 0.0146(16) -0.0031(15) C10 0.038(2) 0.0199(16) 0.0233(17) -0.0002(15) 0.0131(15) 0.0003(16) C11 0.032(2) 0.030(2) 0.027(2) -0.0009(16) 0.0066(17) -0.0011(17) C12 0.029(2) 0.0279(19) 0.0240(19) -0.0035(15) 0.0075(16) -0.0058(16) C13 0.035(2) 0.046(3) 0.038(3) 0.002(2) 0.007(2) -0.018(2) C14 0.047(3) 0.034(2) 0.033(2) 0.0097(18) 0.020(2) 0.0037(19) C15 0.029(2) 0.057(3) 0.030(2) -0.001(2) 0.0024(18) 0.000(2) C16 0.060(3) 0.0226(19) 0.026(2) -0.0015(16) 0.018(2) 0.0122(19) C17 0.074(4) 0.029(2) 0.031(2) 0.0027(18) 0.021(2) 0.020(2) C18 0.073(3) 0.021(2) 0.032(2) 0.0035(17) 0.023(2) 0.011(2) N19 0.042(2) 0.0155(15) 0.0236(16) -0.0005(12) 0.0137(14) 0.0028(13) C20 0.034(2) 0.0171(16) 0.0247(19) 0.0003(14) 0.0146(16) -0.0004(15) C21 0.032(2) 0.0231(19) 0.029(2) 0.0051(16) 0.0095(17) -0.0006(16) C22 0.041(3) 0.035(2) 0.038(2) 0.0053(19) 0.002(2) -0.011(2) C23 0.034(2) 0.034(2) 0.037(2) 0.0114(18) 0.0188(19) 0.0036(18) C24 0.046(3) 0.032(2) 0.027(2) 0.0075(17) 0.0190(19) 0.0143(18) C25 0.042(2) 0.0261(19) 0.025(2) -0.0003(16) 0.0118(18) 0.0042(17) C26 0.033(2) 0.0198(17) 0.0249(19) 0.0003(14) 0.0115(16) 0.0000(15) C27 0.033(2) 0.032(2) 0.040(2) 0.0011(18) 0.0122(19) -0.0024(17) C28 0.072(4) 0.045(3) 0.038(3) 0.013(2) 0.034(3) 0.020(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.16023(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ga1 . Cl2 . 2.1909(11) yes Ga1 . Cl3 . 2.1777(12) yes Ga1 . Cl4 . 2.1657(12) yes Ga1 . C5 . 2.065(4) yes C5 . N6 . 1.338(5) yes C5 . N19 . 1.331(5) yes N6 . C7 . 1.445(5) yes N6 . C16 . 1.485(5) yes C7 . C8 . 1.397(5) yes C7 . C12 . 1.390(5) yes C8 . C9 . 1.393(5) yes C8 . C15 . 1.506(6) yes C9 . C10 . 1.387(6) yes C9 . H91 . 0.935 no C10 . C11 . 1.384(6) yes C10 . C14 . 1.506(5) yes C11 . C12 . 1.397(6) yes C11 . H111 . 0.942 no C12 . C13 . 1.502(5) yes C13 . H131 . 0.956 no C13 . H132 . 0.958 no C13 . H133 . 0.958 no C14 . H141 . 0.964 no C14 . H142 . 0.962 no C14 . H143 . 0.964 no C15 . H152 . 0.958 no C15 . H151 . 0.956 no C15 . H153 . 0.964 no C16 . C17 . 1.505(6) yes C16 . H162 . 0.976 no C16 . H161 . 0.976 no C17 . C18 . 1.493(6) yes C17 . H171 . 0.969 no C17 . H172 . 0.973 no C18 . N19 . 1.487(5) yes C18 . H182 . 0.970 no C18 . H181 . 0.973 no N19 . C20 . 1.443(5) yes C20 . C21 . 1.397(5) yes C20 . C26 . 1.393(6) yes C21 . C22 . 1.506(6) yes C21 . C23 . 1.398(6) yes C22 . H221 . 0.960 no C22 . H223 . 0.959 no C22 . H222 . 0.949 no C23 . C24 . 1.380(7) yes C23 . H231 . 0.932 no C24 . C25 . 1.393(6) yes C24 . C28 . 1.511(6) yes C25 . C26 . 1.387(5) yes C25 . H251 . 0.934 no C26 . C27 . 1.504(6) yes C27 . H272 . 0.959 no C27 . H271 . 0.964 no C27 . H273 . 0.960 no C28 . H282 . 0.964 no C28 . H281 . 0.960 no C28 . H283 . 0.954 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl2 . Ga1 . Cl3 . 105.58(5) yes Cl2 . Ga1 . Cl4 . 102.00(5) yes Cl3 . Ga1 . Cl4 . 109.54(7) yes Cl2 . Ga1 . C5 . 117.92(11) yes Cl3 . Ga1 . C5 . 107.01(11) yes Cl4 . Ga1 . C5 . 114.31(11) yes Ga1 . C5 . N6 . 120.7(3) yes Ga1 . C5 . N19 . 120.1(3) yes N6 . C5 . N19 . 119.1(3) yes C5 . N6 . C7 . 123.1(3) yes C5 . N6 . C16 . 122.6(3) yes C7 . N6 . C16 . 114.2(3) yes N6 . C7 . C8 . 118.5(3) yes N6 . C7 . C12 . 119.5(3) yes C8 . C7 . C12 . 121.7(3) yes C7 . C8 . C9 . 118.0(3) yes C7 . C8 . C15 . 121.4(4) yes C9 . C8 . C15 . 120.6(4) yes C8 . C9 . C10 . 121.7(3) yes C8 . C9 . H91 . 119.0 no C10 . C9 . H91 . 119.3 no C9 . C10 . C11 . 118.7(4) yes C9 . C10 . C14 . 121.0(4) yes C11 . C10 . C14 . 120.4(4) yes C10 . C11 . C12 . 121.7(4) yes C10 . C11 . H111 . 119.7 no C12 . C11 . H111 . 118.7 no C11 . C12 . C7 . 118.1(4) yes C11 . C12 . C13 . 119.5(4) yes C7 . C12 . C13 . 122.3(4) yes C12 . C13 . H131 . 110.1 no C12 . C13 . H132 . 111.5 no H131 . C13 . H132 . 108.6 no C12 . C13 . H133 . 109.8 no H131 . C13 . H133 . 108.3 no H132 . C13 . H133 . 108.4 no C10 . C14 . H141 . 109.3 no C10 . C14 . H142 . 109.8 no H141 . C14 . H142 . 108.9 no C10 . C14 . H143 . 110.1 no H141 . C14 . H143 . 109.3 no H142 . C14 . H143 . 109.4 no C8 . C15 . H152 . 109.7 no C8 . C15 . H151 . 109.9 no H152 . C15 . H151 . 109.0 no C8 . C15 . H153 . 110.3 no H152 . C15 . H153 . 109.1 no H151 . C15 . H153 . 108.8 no N6 . C16 . C17 . 109.8(3) yes N6 . C16 . H162 . 108.1 no C17 . C16 . H162 . 109.7 no N6 . C16 . H161 . 109.8 no C17 . C16 . H161 . 110.0 no H162 . C16 . H161 . 109.3 no C16 . C17 . C18 . 109.5(4) yes C16 . C17 . H171 . 109.1 no C18 . C17 . H171 . 109.8 no C16 . C17 . H172 . 109.0 no C18 . C17 . H172 . 109.9 no H171 . C17 . H172 . 109.5 no C17 . C18 . N19 . 110.5(4) yes C17 . C18 . H182 . 109.7 no N19 . C18 . H182 . 108.6 no C17 . C18 . H181 . 109.5 no N19 . C18 . H181 . 108.6 no H182 . C18 . H181 . 110.0 no C18 . N19 . C5 . 123.8(3) yes C18 . N19 . C20 . 112.5(3) yes C5 . N19 . C20 . 123.7(3) yes N19 . C20 . C21 . 119.0(4) yes N19 . C20 . C26 . 118.2(3) yes C21 . C20 . C26 . 122.5(4) yes C20 . C21 . C22 . 122.4(4) yes C20 . C21 . C23 . 117.2(4) yes C22 . C21 . C23 . 120.4(4) yes C21 . C22 . H221 . 111.5 no C21 . C22 . H223 . 111.3 no H221 . C22 . H223 . 107.9 no C21 . C22 . H222 . 110.2 no H221 . C22 . H222 . 108.1 no H223 . C22 . H222 . 107.7 no C21 . C23 . C24 . 122.0(4) yes C21 . C23 . H231 . 118.8 no C24 . C23 . H231 . 119.2 no C23 . C24 . C25 . 118.8(4) yes C23 . C24 . C28 . 121.1(4) yes C25 . C24 . C28 . 120.1(4) yes C24 . C25 . C26 . 121.7(4) yes C24 . C25 . H251 . 119.5 no C26 . C25 . H251 . 118.8 no C20 . C26 . C25 . 117.8(4) yes C20 . C26 . C27 . 122.1(4) yes C25 . C26 . C27 . 120.0(4) yes C26 . C27 . H272 . 110.3 no C26 . C27 . H271 . 110.2 no H272 . C27 . H271 . 109.4 no C26 . C27 . H273 . 109.4 no H272 . C27 . H273 . 109.2 no H271 . C27 . H273 . 108.3 no C24 . C28 . H282 . 110.4 no C24 . C28 . H281 . 109.2 no H282 . C28 . H281 . 109.2 no C24 . C28 . H283 . 109.3 no H282 . C28 . H283 . 110.0 no H281 . C28 . H283 . 108.7 no _iucr_refine_instruction_details_constraints ; # # Punched on 27/04/11 at 16:54:58 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 11,X'S) H ( 111,X'S) RIDE C ( 13,X'S) H ( 131,X'S) H ( 132,X'S) H ( 133,X'S) RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S) RIDE C ( 15,X'S) H ( 152,X'S) H ( 151,X'S) H ( 153,X'S) RIDE C ( 16,X'S) H ( 162,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) RIDE C ( 18,X'S) H ( 182,X'S) H ( 181,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 223,X'S) H ( 222,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 27,X'S) H ( 272,X'S) H ( 271,X'S) H ( 273,X'S) RIDE C ( 28,X'S) H ( 282,X'S) H ( 281,X'S) H ( 283,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 27/04/11 at 16:54:58 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; # Attachment 'LpyAlCl3.cif' data_LpyAlCl3 _database_code_depnum_ccdc_archive 'CCDC 839368' #TrackingRef 'LpyAlCl3.cif' _audit_creation_date 10-03-27 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title '3270019 010hmct10' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 9.30440(10) _cell_length_b 16.4546(2) _cell_length_c 15.8068(2) _cell_angle_alpha 90 _cell_angle_beta 106.6567(5) _cell_angle_gamma 90 _cell_volume 2318.48(5) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Al 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C30 H15 Al1 Cl3 N1 # Dc = 1.50 Fooo = 936.00 Mu = 4.55 M = 522.80 # Found Formula = C23 H25 Al1 Cl3 N1 # Dc = 1.29 FOOO = 936.00 Mu = 4.42 M = 448.80 _chemical_formula_sum 'C23 H25 Al1 Cl3 N1' _chemical_formula_moiety 'C23 H25 Al1 Cl3 N1' _chemical_compound_source ? _chemical_formula_weight 448.80 _cell_measurement_reflns_used 5283 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.22 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.42 _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 0.442 # Sheldrick geometric approximatio 0.89 0.91 # No experimental values of Tmin/max available _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.91 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 9919 _reflns_number_total 5275 _diffrn_reflns_av_R_equivalents 0.022 # Number of reflections with Friedels Law is 5275 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5314 _diffrn_reflns_theta_min 5.136 _diffrn_reflns_theta_max 27.477 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.652 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 2.90 _oxford_diffrn_Wilson_scale 3.53 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.76 _refine_diff_density_max 0.56 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 5275 _refine_ls_number_restraints 0 _refine_ls_number_parameters 254 _oxford_refine_ls_R_factor_ref 0.0663 _refine_ls_wR_factor_ref 0.1009 _refine_ls_goodness_of_fit_ref 0.9665 _refine_ls_shift/su_max 0.000564 # The values computed from all data _oxford_reflns_number_all 5275 _refine_ls_R_factor_all 0.0663 _refine_ls_wR_factor_all 0.1009 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3935 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_gt 0.0915 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 2.42P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cl1 Cl 1.02533(7) 0.75756(3) 0.83444(4) 0.0454 1.0000 Uani . . . . . . . Al2 Al 0.92385(6) 0.70997(3) 0.70626(4) 0.0284 1.0000 Uani . . . . . . . Cl3 Cl 0.74621(7) 0.79171(4) 0.65463(6) 0.0705 1.0000 Uani . . . . . . . Cl4 Cl 1.08448(7) 0.71039(4) 0.63547(5) 0.0561 1.0000 Uani . . . . . . . N5 N 0.85444(16) 0.59396(9) 0.70054(10) 0.0235 1.0000 Uani . . . . . . . C6 C 0.9211(2) 0.53947(11) 0.76582(12) 0.0272 1.0000 Uani . . . . . . . C7 C 1.0391(2) 0.56426(11) 0.84710(12) 0.0268 1.0000 Uani . . . . . . . C8 C 1.1906(2) 0.55244(12) 0.85207(14) 0.0322 1.0000 Uani . . . . . . . C9 C 1.2379(3) 0.52166(15) 0.77431(16) 0.0436 1.0000 Uani . . . . . . . C10 C 1.2978(2) 0.56915(13) 0.93195(15) 0.0390 1.0000 Uani . . . . . . . C11 C 1.2588(3) 0.59549(13) 1.00528(15) 0.0400 1.0000 Uani . . . . . . . C12 C 1.1079(3) 0.60550(12) 0.99886(14) 0.0370 1.0000 Uani . . . . . . . C13 C 0.9964(2) 0.58976(12) 0.92101(13) 0.0305 1.0000 Uani . . . . . . . C14 C 0.8341(2) 0.60310(14) 0.91716(16) 0.0405 1.0000 Uani . . . . . . . C15 C 1.3772(3) 0.61245(17) 1.09184(17) 0.0586 1.0000 Uani . . . . . . . C16 C 0.8811(2) 0.45812(12) 0.75909(14) 0.0370 1.0000 Uani . . . . . . . C17 C 0.7703(3) 0.42996(13) 0.68748(15) 0.0426 1.0000 Uani . . . . . . . C18 C 0.7023(3) 0.48449(13) 0.62230(14) 0.0384 1.0000 Uani . . . . . . . C19 C 0.7460(2) 0.56503(12) 0.62785(12) 0.0270 1.0000 Uani . . . . . . . C20 C 0.6732(2) 0.61893(11) 0.55164(12) 0.0261 1.0000 Uani . . . . . . . C21 C 0.5332(2) 0.65351(11) 0.54622(12) 0.0260 1.0000 Uani . . . . . . . C22 C 0.4644(2) 0.70136(11) 0.47340(13) 0.0282 1.0000 Uani . . . . . . . C23 C 0.5294(2) 0.71325(12) 0.40548(13) 0.0300 1.0000 Uani . . . . . . . C24 C 0.6630(2) 0.67419(13) 0.40975(13) 0.0337 1.0000 Uani . . . . . . . C25 C 0.7356(2) 0.62587(13) 0.48129(13) 0.0315 1.0000 Uani . . . . . . . C26 C 0.8734(3) 0.57842(16) 0.47885(16) 0.0478 1.0000 Uani . . . . . . . C27 C 0.4558(3) 0.76709(14) 0.32764(15) 0.0437 1.0000 Uani . . . . . . . C28 C 0.4581(2) 0.63949(15) 0.61736(14) 0.0402 1.0000 Uani . . . . . . . H91 H 1.3465 0.5239 0.7869 0.0687 1.0000 Uiso R . . . . . . H93 H 1.1948 0.5544 0.7211 0.0686 1.0000 Uiso R . . . . . . H92 H 1.2056 0.4663 0.7599 0.0691 1.0000 Uiso R . . . . . . H101 H 1.4029 0.5618 0.9361 0.0445 1.0000 Uiso R . . . . . . H121 H 1.0790 0.6243 1.0503 0.0437 1.0000 Uiso R . . . . . . H141 H 0.8212 0.6066 0.9758 0.0665 1.0000 Uiso R . . . . . . H142 H 0.7988 0.6530 0.8856 0.0663 1.0000 Uiso R . . . . . . H143 H 0.7741 0.5597 0.8844 0.0661 1.0000 Uiso R . . . . . . H151 H 1.3406 0.6541 1.1247 0.0825 1.0000 Uiso R . . . . . . H152 H 1.4666 0.6305 1.0784 0.0817 1.0000 Uiso R . . . . . . H153 H 1.3973 0.5632 1.1260 0.0821 1.0000 Uiso R . . . . . . H161 H 0.9311 0.4216 0.8056 0.0414 1.0000 Uiso R . . . . . . H171 H 0.7426 0.3744 0.6831 0.0475 1.0000 Uiso R . . . . . . H181 H 0.6232 0.4675 0.5717 0.0436 1.0000 Uiso R . . . . . . H221 H 0.3694 0.7255 0.4701 0.0327 1.0000 Uiso R . . . . . . H241 H 0.7077 0.6794 0.3608 0.0401 1.0000 Uiso R . . . . . . H262 H 0.9272 0.6064 0.4433 0.0749 1.0000 Uiso R . . . . . . H261 H 0.9389 0.5704 0.5384 0.0738 1.0000 Uiso R . . . . . . H263 H 0.8425 0.5255 0.4525 0.0745 1.0000 Uiso R . . . . . . H272 H 0.4629 0.7415 0.2728 0.0641 1.0000 Uiso R . . . . . . H271 H 0.5054 0.8194 0.3342 0.0635 1.0000 Uiso R . . . . . . H273 H 0.3513 0.7751 0.3258 0.0636 1.0000 Uiso R . . . . . . H282 H 0.3710 0.6747 0.6078 0.0628 1.0000 Uiso R . . . . . . H281 H 0.5261 0.6491 0.6753 0.0627 1.0000 Uiso R . . . . . . H283 H 0.4267 0.5831 0.6134 0.0635 1.0000 Uiso 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 Cl1 0.0571(4) 0.0301(3) 0.0415(3) -0.0006(2) 0.0020(3) -0.0100(2) Al2 0.0223(3) 0.0228(3) 0.0368(3) 0.0041(2) 0.0030(2) 0.0004(2) Cl3 0.0436(3) 0.0300(3) 0.1050(6) -0.0176(3) -0.0313(4) 0.0135(3) Cl4 0.0499(4) 0.0620(4) 0.0655(4) 0.0066(3) 0.0311(3) -0.0112(3) N5 0.0217(7) 0.0230(8) 0.0240(8) 0.0001(6) 0.0037(6) 0.0010(6) C6 0.0270(9) 0.0249(9) 0.0270(10) 0.0010(8) 0.0034(8) 0.0023(8) C7 0.0279(9) 0.0210(9) 0.0264(10) 0.0038(7) -0.0002(8) -0.0002(7) C8 0.0301(10) 0.0264(10) 0.0363(11) 0.0081(8) 0.0033(9) 0.0021(8) C9 0.0401(12) 0.0442(13) 0.0478(14) 0.0068(11) 0.0148(11) 0.0110(10) C10 0.0263(10) 0.0361(12) 0.0474(13) 0.0125(10) -0.0010(10) -0.0024(9) C11 0.0418(12) 0.0301(11) 0.0366(12) 0.0076(9) -0.0072(10) -0.0123(9) C12 0.0496(13) 0.0285(10) 0.0278(11) 0.0012(9) 0.0029(10) -0.0069(9) C13 0.0333(10) 0.0242(10) 0.0309(10) 0.0028(8) 0.0042(9) -0.0020(8) C14 0.0399(12) 0.0394(12) 0.0440(13) -0.0012(10) 0.0148(10) 0.0004(10) C15 0.0589(16) 0.0546(16) 0.0427(14) 0.0074(12) -0.0169(12) -0.0204(13) C16 0.0446(12) 0.0249(10) 0.0327(11) 0.0055(9) -0.003(1) 0.0015(9) C17 0.0513(14) 0.0225(10) 0.0428(13) -0.0004(9) -0.0044(11) -0.0045(9) C18 0.0416(12) 0.0289(11) 0.0328(11) -0.0035(9) -0.0081(10) -0.0014(9) C19 0.0261(9) 0.0266(10) 0.0248(10) -0.0014(8) 0.0014(8) 0.0032(8) C20 0.0267(9) 0.0240(9) 0.0239(9) -0.0025(8) 0.0015(8) 0.0027(7) C21 0.0245(9) 0.0280(10) 0.0235(9) -0.0060(8) 0.0034(8) -0.0011(7) C22 0.0214(9) 0.0274(10) 0.0308(10) -0.0046(8) -0.0006(8) 0.0024(7) C23 0.0303(10) 0.0259(9) 0.0276(10) 0.0007(8) -0.0019(8) 0.0003(8) C24 0.0366(11) 0.0379(11) 0.0277(10) 0.0029(9) 0.0110(9) 0.0024(9) C25 0.0302(10) 0.0327(10) 0.0314(11) -0.0011(9) 0.0086(9) 0.0068(8) C26 0.0440(13) 0.0573(15) 0.0455(14) 0.0022(12) 0.0181(11) 0.0215(11) C27 0.0475(13) 0.0397(12) 0.0361(12) 0.0106(10) -0.0003(10) 0.0015(10) C28 0.0365(12) 0.0518(14) 0.0347(12) -0.0007(10) 0.0140(10) 0.0042(10) _refine_ls_extinction_coef 140(20) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.5786(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 . Al2 . 2.1243(8) yes Al2 . Cl3 . 2.1056(8) yes Al2 . Cl4 . 2.1083(9) yes Al2 . N5 . 2.0089(16) yes N5 . C6 . 1.373(2) yes N5 . C19 . 1.378(2) yes C6 . C7 . 1.488(3) yes C6 . C16 . 1.385(3) yes C7 . C8 . 1.402(3) yes C7 . C13 . 1.402(3) yes C8 . C9 . 1.507(3) yes C8 . C10 . 1.394(3) yes C9 . H91 . 0.973 no C9 . H93 . 0.982 no C9 . H92 . 0.966 no C10 . C11 . 1.380(3) yes C10 . H101 . 0.969 no C11 . C12 . 1.388(3) yes C11 . C15 . 1.517(3) yes C12 . C13 . 1.388(3) yes C12 . H121 . 0.978 no C13 . C14 . 1.510(3) yes C14 . H141 . 0.969 no C14 . H142 . 0.967 no C14 . H143 . 0.962 no C15 . H151 . 0.979 no C15 . H152 . 0.962 no C15 . H153 . 0.962 no C16 . C17 . 1.375(3) yes C16 . H161 . 0.960 no C17 . C18 . 1.376(3) yes C17 . H171 . 0.948 no C18 . C19 . 1.381(3) yes C18 . H181 . 0.960 no C19 . C20 . 1.493(3) yes C20 . C21 . 1.401(3) yes C20 . C25 . 1.399(3) yes C21 . C22 . 1.390(3) yes C21 . C28 . 1.502(3) yes C22 . C23 . 1.389(3) yes C22 . H221 . 0.957 no C23 . C24 . 1.384(3) yes C23 . C27 . 1.512(3) yes C24 . C25 . 1.389(3) yes C24 . H241 . 0.982 no C25 . C26 . 1.511(3) yes C26 . H262 . 0.970 no C26 . H261 . 0.973 no C26 . H263 . 0.972 no C27 . H272 . 0.983 no C27 . H271 . 0.969 no C27 . H273 . 0.974 no C28 . H282 . 0.972 no C28 . H281 . 0.966 no C28 . H283 . 0.970 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Al2 . Cl3 . 102.66(4) yes Cl1 . Al2 . Cl4 . 108.43(4) yes Cl3 . Al2 . Cl4 . 112.91(4) yes Cl1 . Al2 . N5 . 116.26(5) yes Cl3 . Al2 . N5 . 112.52(5) yes Cl4 . Al2 . N5 . 104.29(5) yes Al2 . N5 . C6 . 121.09(12) yes Al2 . N5 . C19 . 120.98(12) yes C6 . N5 . C19 . 117.76(15) yes N5 . C6 . C7 . 122.16(16) yes N5 . C6 . C16 . 121.31(17) yes C7 . C6 . C16 . 116.53(17) yes C6 . C7 . C8 . 119.45(18) yes C6 . C7 . C13 . 119.09(17) yes C8 . C7 . C13 . 121.01(18) yes C7 . C8 . C9 . 121.64(19) yes C7 . C8 . C10 . 118.0(2) yes C9 . C8 . C10 . 120.31(19) yes C8 . C9 . H91 . 110.4 no C8 . C9 . H93 . 111.8 no H91 . C9 . H93 . 107.5 no C8 . C9 . H92 . 111.4 no H91 . C9 . H92 . 108.5 no H93 . C9 . H92 . 107.0 no C8 . C10 . C11 . 122.0(2) yes C8 . C10 . H101 . 118.9 no C11 . C10 . H101 . 119.0 no C10 . C11 . C12 . 118.68(19) yes C10 . C11 . C15 . 121.2(2) yes C12 . C11 . C15 . 120.2(2) yes C11 . C12 . C13 . 121.7(2) yes C11 . C12 . H121 . 119.4 no C13 . C12 . H121 . 118.9 no C7 . C13 . C12 . 118.46(19) yes C7 . C13 . C14 . 121.95(18) yes C12 . C13 . C14 . 119.6(2) yes C13 . C14 . H141 . 111.5 no C13 . C14 . H142 . 109.4 no H141 . C14 . H142 . 109.0 no C13 . C14 . H143 . 109.5 no H141 . C14 . H143 . 110.3 no H142 . C14 . H143 . 107.0 no C11 . C15 . H151 . 109.5 no C11 . C15 . H152 . 107.9 no H151 . C15 . H152 . 110.9 no C11 . C15 . H153 . 108.9 no H151 . C15 . H153 . 109.5 no H152 . C15 . H153 . 110.1 no C6 . C16 . C17 . 120.69(19) yes C6 . C16 . H161 . 119.1 no C17 . C16 . H161 . 120.2 no C16 . C17 . C18 . 118.16(19) yes C16 . C17 . H171 . 120.6 no C18 . C17 . H171 . 121.2 no C17 . C18 . C19 . 120.95(19) yes C17 . C18 . H181 . 120.8 no C19 . C18 . H181 . 118.3 no C18 . C19 . N5 . 121.06(17) yes C18 . C19 . C20 . 117.48(17) yes N5 . C19 . C20 . 121.45(16) yes C19 . C20 . C21 . 119.30(17) yes C19 . C20 . C25 . 119.61(17) yes C21 . C20 . C25 . 120.57(17) yes C20 . C21 . C22 . 118.67(17) yes C20 . C21 . C28 . 121.05(18) yes C22 . C21 . C28 . 120.28(17) yes C21 . C22 . C23 . 121.39(17) yes C21 . C22 . H221 . 118.7 no C23 . C22 . H221 . 120.0 no C22 . C23 . C24 . 118.75(18) yes C22 . C23 . C27 . 121.04(19) yes C24 . C23 . C27 . 120.21(19) yes C23 . C24 . C25 . 121.75(19) yes C23 . C24 . H241 . 119.9 no C25 . C24 . H241 . 118.3 no C20 . C25 . C24 . 118.54(18) yes C20 . C25 . C26 . 121.78(18) yes C24 . C25 . C26 . 119.57(19) yes C25 . C26 . H262 . 110.6 no C25 . C26 . H261 . 110.3 no H262 . C26 . H261 . 109.9 no C25 . C26 . H263 . 109.0 no H262 . C26 . H263 . 108.4 no H261 . C26 . H263 . 108.6 no C23 . C27 . H272 . 109.7 no C23 . C27 . H271 . 110.1 no H272 . C27 . H271 . 109.0 no C23 . C27 . H273 . 108.7 no H272 . C27 . H273 . 110.5 no H271 . C27 . H273 . 108.9 no C21 . C28 . H282 . 109.7 no C21 . C28 . H281 . 111.4 no H282 . C28 . H281 . 109.9 no C21 . C28 . H283 . 107.1 no H282 . C28 . H283 . 109.8 no H281 . C28 . H283 . 108.8 no # Attachment 'LpyGaCl3.cif' data_LpyGaCl3 _database_code_depnum_ccdc_archive 'CCDC 839369' #TrackingRef 'LpyGaCl3.cif' _audit_creation_date 10-02-01 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title '2010100 003HMCT10' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 9.3105(2) _cell_length_b 16.5276(3) _cell_length_c 15.7099(3) _cell_angle_alpha 90 _cell_angle_beta 106.6726(8) _cell_angle_gamma 90 _cell_volume 2315.81(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ga 0.2307 1.6083 15.2354 3.0669 6.7006 0.2412 4.3591 10.7805 2.9623 61.4135 1.7189 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C200 H30 Cl12 Ga4 N4 # Dc = 2.29 Fooo = 1008.00 Mu = 15.95 M = 798.19 # Found Formula = C92 H100 Cl12 Ga4 N4 # Dc = 1.41 FOOO = 1008.00 Mu = 15.43 M = 491.54 _chemical_formula_sum 'C92 H100 Cl12 Ga4 N4' _chemical_formula_moiety 'C92 H100 Cl12 Ga4 N4' _chemical_compound_source ? _chemical_formula_weight 1966.15 _cell_measurement_reflns_used 5022 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.36 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_max 0.51 _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 1.543 # Sheldrick geometric approximatio 0.51 0.57 # No experimental values of Tmin/max available _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.57 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 9727 _reflns_number_total 5262 _diffrn_reflns_av_R_equivalents 0.022 # Number of reflections with Friedels Law is 5262 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5306 _diffrn_reflns_theta_min 5.117 _diffrn_reflns_theta_max 27.474 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.101 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -12 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 2.51 _oxford_diffrn_Wilson_scale 7.75 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.74 _refine_diff_density_max 0.61 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 5262 _refine_ls_number_restraints 0 _refine_ls_number_parameters 253 _oxford_refine_ls_R_factor_ref 0.0550 _refine_ls_wR_factor_ref 0.0824 _refine_ls_goodness_of_fit_ref 0.9786 _refine_ls_shift/su_max 0.000607 # The values computed from all data _oxford_reflns_number_all 5262 _refine_ls_R_factor_all 0.0550 _refine_ls_wR_factor_all 0.0824 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4042 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_gt 0.0750 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 2.49P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ga1 Ga 0.42588(3) 0.291212(14) 0.706305(17) 0.0273 1.0000 Uani . . . . . . . Cl2 Cl 0.52700(8) 0.24245(4) 0.83768(5) 0.0462 1.0000 Uani . . . . . . . Cl3 Cl 0.24787(8) 0.20674(4) 0.65270(6) 0.0674 1.0000 Uani . . . . . . . Cl4 Cl 0.59051(8) 0.29078(5) 0.63442(5) 0.0546 1.0000 Uani . . . . . . . N5 N 0.35605(19) 0.40880(11) 0.70010(11) 0.0232 1.0000 Uani . . . . . . . C6 C 0.4239(2) 0.46272(13) 0.76542(14) 0.0262 1.0000 Uani . . . . . . . C7 C 0.5407(2) 0.43706(13) 0.84775(14) 0.0265 1.0000 Uani . . . . . . . C8 C 0.6923(3) 0.44840(14) 0.85302(16) 0.0302 1.0000 Uani . . . . . . . C9 C 0.7408(3) 0.47892(17) 0.77567(18) 0.0432 1.0000 Uani . . . . . . . C10 C 0.7987(3) 0.43093(16) 0.93386(17) 0.0378 1.0000 Uani . . . . . . . C11 C 0.7583(3) 0.40418(15) 1.00704(16) 0.0376 1.0000 Uani . . . . . . . C12 C 0.6074(3) 0.39444(15) 0.99976(16) 0.0354 1.0000 Uani . . . . . . . C13 C 0.4967(3) 0.41110(14) 0.92106(15) 0.0304 1.0000 Uani . . . . . . . C14 C 0.3343(3) 0.39784(17) 0.91643(18) 0.0394 1.0000 Uani . . . . . . . C15 C 0.8757(3) 0.3863(2) 1.09405(19) 0.0561 1.0000 Uani . . . . . . . C16 C 0.3851(3) 0.54374(14) 0.75836(16) 0.0368 1.0000 Uani . . . . . . . C17 C 0.2739(3) 0.57185(15) 0.68615(17) 0.0418 1.0000 Uani . . . . . . . C18 C 0.2050(3) 0.51714(15) 0.62124(17) 0.0379 1.0000 Uani . . . . . . . C19 C 0.2478(2) 0.43698(13) 0.62705(14) 0.0264 1.0000 Uani . . . . . . . C20 C 0.1746(2) 0.38249(13) 0.55141(14) 0.0248 1.0000 Uani . . . . . . . C21 C 0.2351(3) 0.37496(15) 0.48005(15) 0.0305 1.0000 Uani . . . . . . . C22 C 0.1615(3) 0.32589(16) 0.40916(16) 0.0342 1.0000 Uani . . . . . . . C23 C 0.0285(3) 0.28675(14) 0.40651(15) 0.0295 1.0000 Uani . . . . . . . C24 C -0.0339(2) 0.29939(13) 0.47542(15) 0.0279 1.0000 Uani . . . . . . . C25 C 0.0360(2) 0.34755(14) 0.54801(14) 0.0259 1.0000 Uani . . . . . . . C26 C -0.0366(3) 0.36186(18) 0.62050(17) 0.0411 1.0000 Uani . . . . . . . C27 C -0.0458(3) 0.23263(17) 0.32945(17) 0.0420 1.0000 Uani . . . . . . . C28 C 0.3722(3) 0.42168(19) 0.47618(19) 0.0461 1.0000 Uani . . . . . . . H91 H 0.8476 0.4750 0.7874 0.0663 1.0000 Uiso R . . . . . . H93 H 0.7117 0.5346 0.7652 0.0669 1.0000 Uiso R . . . . . . H92 H 0.6933 0.4495 0.7216 0.0662 1.0000 Uiso R . . . . . . H101 H 0.9035 0.4380 0.9377 0.0419 1.0000 Uiso R . . . . . . H121 H 0.5782 0.3757 1.0495 0.0416 1.0000 Uiso R . . . . . . H141 H 0.3230 0.3968 0.9746 0.0624 1.0000 Uiso R . . . . . . H142 H 0.2722 0.4413 0.8848 0.0616 1.0000 Uiso R . . . . . . H143 H 0.2982 0.3485 0.8871 0.0624 1.0000 Uiso R . . . . . . H151 H 0.8381 0.3461 1.1272 0.0771 1.0000 Uiso R . . . . . . H152 H 0.8991 0.4350 1.1291 0.0770 1.0000 Uiso R . . . . . . H153 H 0.9644 0.3664 1.0826 0.0767 1.0000 Uiso R . . . . . . H161 H 0.4356 0.5796 0.8045 0.0413 1.0000 Uiso R . . . . . . H171 H 0.2474 0.6273 0.6820 0.0455 1.0000 Uiso R . . . . . . H181 H 0.1267 0.5349 0.5717 0.0426 1.0000 Uiso R . . . . . . H221 H 0.2037 0.3188 0.3607 0.0413 1.0000 Uiso R . . . . . . H241 H -0.1265 0.2758 0.4745 0.0327 1.0000 Uiso R . . . . . . H262 H -0.1183 0.3251 0.6152 0.0652 1.0000 Uiso R . . . . . . H261 H -0.0725 0.4175 0.6176 0.0656 1.0000 Uiso R . . . . . . H263 H 0.0344 0.3531 0.6789 0.0655 1.0000 Uiso R . . . . . . H272 H -0.1470 0.2229 0.3282 0.0613 1.0000 Uiso R . . . . . . H271 H -0.0440 0.2583 0.2760 0.0620 1.0000 Uiso R . . . . . . H273 H 0.0065 0.1820 0.3351 0.0606 1.0000 Uiso R . . . . . . H282 H 0.4223 0.3950 0.4395 0.0720 1.0000 Uiso R . . . . . . H281 H 0.3407 0.4740 0.4514 0.0720 1.0000 Uiso R . . . . . . H283 H 0.4424 0.4282 0.5335 0.0724 1.0000 Uiso 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 0.02076(13) 0.02138(13) 0.03581(15) -0.00388(11) 0.00197(10) -0.00005(10) Cl2 0.0563(4) 0.0314(3) 0.0434(4) -0.0001(3) 0.0024(3) 0.0100(3) Cl3 0.0413(4) 0.0285(3) 0.1014(6) 0.0162(4) -0.0293(4) -0.0132(3) Cl4 0.0452(4) 0.0622(5) 0.0642(5) -0.0086(4) 0.0282(3) 0.0097(3) N5 0.0221(9) 0.0222(9) 0.0235(9) 0.0012(7) 0.0036(7) -0.0008(7) C6 0.0253(11) 0.0237(11) 0.0256(11) -0.0013(9) 0.0009(9) -0.0026(9) C7 0.0284(11) 0.0203(10) 0.0258(11) -0.0048(9) -0.0001(9) -0.0004(9) C8 0.0294(12) 0.0239(11) 0.0337(13) -0.0066(10) 0.0035(10) -0.0017(9) C9 0.0378(14) 0.0433(15) 0.0493(16) -0.0074(13) 0.0138(12) -0.0093(12) C10 0.0261(12) 0.0347(13) 0.0445(15) -0.0135(12) -0.0028(10) 0.0023(10) C11 0.0400(14) 0.0294(12) 0.0325(13) -0.0076(11) -0.0073(11) 0.0113(10) C12 0.0476(15) 0.0277(12) 0.0260(12) 0.0011(10) 0.0027(10) 0.0074(11) C13 0.0328(12) 0.0243(11) 0.0295(12) -0.0016(9) 0.0018(10) 0.0018(9) C14 0.0387(14) 0.0381(14) 0.0429(15) 0.0006(12) 0.0139(12) -0.0012(11) C15 0.0560(18) 0.0527(18) 0.0413(16) -0.0066(14) -0.0154(13) 0.0196(14) C16 0.0446(14) 0.0230(11) 0.0334(13) -0.0046(10) -0.0038(11) 0.0002(10) C17 0.0499(16) 0.0223(12) 0.0415(15) 0.0018(11) -0.0054(12) 0.0050(11) C18 0.0417(14) 0.0289(12) 0.0319(13) 0.0042(11) -0.0073(11) 0.0020(11) C19 0.0269(11) 0.0237(11) 0.0255(11) 0.0013(9) 0.0025(9) -0.0028(9) C20 0.0252(11) 0.0236(11) 0.0211(11) 0.0022(9) -0.0005(8) -0.0008(8) C21 0.0294(12) 0.0325(12) 0.0288(12) 0.0006(10) 0.0071(9) -0.0079(10) C22 0.0375(13) 0.0387(14) 0.0271(12) -0.0021(11) 0.0106(10) -0.0017(11) C23 0.0301(11) 0.0264(11) 0.0265(11) 0.0001(10) -0.0007(9) 0.0005(9) C24 0.0215(10) 0.0252(11) 0.0319(12) 0.0051(10) -0.0005(9) -0.0024(9) C25 0.0241(11) 0.0275(11) 0.0228(11) 0.0056(9) 0.0015(8) 0.0009(9) C26 0.0377(14) 0.0540(17) 0.0338(14) 0.0001(12) 0.0138(11) -0.0036(12) C27 0.0442(15) 0.0393(15) 0.0349(14) -0.0093(11) -0.0010(11) -0.0048(12) C28 0.0411(15) 0.0571(18) 0.0423(15) -0.0004(13) 0.0154(12) -0.0202(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3910(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ga1 . Cl2 . 2.1634(7) yes Ga1 . Cl3 . 2.1457(7) yes Ga1 . Cl4 . 2.1490(7) yes Ga1 . N5 . 2.0428(18) yes N5 . C6 . 1.369(3) yes N5 . C19 . 1.374(3) yes C6 . C7 . 1.493(3) yes C6 . C16 . 1.383(3) yes C7 . C8 . 1.403(3) yes C7 . C13 . 1.396(3) yes C8 . C9 . 1.500(4) yes C8 . C10 . 1.398(3) yes C9 . H91 . 0.961 no C9 . H93 . 0.960 no C9 . H92 . 0.968 no C10 . C11 . 1.381(4) yes C10 . H101 . 0.968 no C11 . C12 . 1.386(4) yes C11 . C15 . 1.514(3) yes C12 . C13 . 1.391(3) yes C12 . H121 . 0.949 no C13 . C14 . 1.509(3) yes C14 . H141 . 0.949 no C14 . H142 . 0.966 no C14 . H143 . 0.950 no C15 . H151 . 0.969 no C15 . H152 . 0.964 no C15 . H153 . 0.953 no C16 . C17 . 1.379(3) yes C16 . H161 . 0.950 no C17 . C18 . 1.376(3) yes C17 . H171 . 0.947 no C18 . C19 . 1.379(3) yes C18 . H181 . 0.947 no C19 . C20 . 1.491(3) yes C20 . C21 . 1.397(3) yes C20 . C25 . 1.400(3) yes C21 . C22 . 1.389(3) yes C21 . C28 . 1.508(3) yes C22 . C23 . 1.387(3) yes C22 . H221 . 0.959 no C23 . C24 . 1.383(3) yes C23 . C27 . 1.504(3) yes C24 . C25 . 1.390(3) yes C24 . H241 . 0.942 no C25 . C26 . 1.501(3) yes C26 . H262 . 0.959 no C26 . H261 . 0.976 no C26 . H263 . 0.975 no C27 . H272 . 0.951 no C27 . H271 . 0.945 no C27 . H273 . 0.960 no C28 . H282 . 0.948 no C28 . H281 . 0.959 no C28 . H283 . 0.956 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl2 . Ga1 . Cl3 . 101.99(3) yes Cl2 . Ga1 . Cl4 . 108.62(3) yes Cl3 . Ga1 . Cl4 . 112.25(4) yes Cl2 . Ga1 . N5 . 116.45(5) yes Cl3 . Ga1 . N5 . 113.63(5) yes Cl4 . Ga1 . N5 . 104.08(5) yes Ga1 . N5 . C6 . 120.75(14) yes Ga1 . N5 . C19 . 120.65(14) yes C6 . N5 . C19 . 118.42(18) yes N5 . C6 . C7 . 121.97(19) yes N5 . C6 . C16 . 121.1(2) yes C7 . C6 . C16 . 116.94(19) yes C6 . C7 . C8 . 118.9(2) yes C6 . C7 . C13 . 119.3(2) yes C8 . C7 . C13 . 121.4(2) yes C7 . C8 . C9 . 121.9(2) yes C7 . C8 . C10 . 117.7(2) yes C9 . C8 . C10 . 120.4(2) yes C8 . C9 . H91 . 111.0 no C8 . C9 . H93 . 109.0 no H91 . C9 . H93 . 108.8 no C8 . C9 . H92 . 111.9 no H91 . C9 . H92 . 108.8 no H93 . C9 . H92 . 107.2 no C8 . C10 . C11 . 122.1(2) yes C8 . C10 . H101 . 118.1 no C11 . C10 . H101 . 119.8 no C10 . C11 . C12 . 118.7(2) yes C10 . C11 . C15 . 121.0(3) yes C12 . C11 . C15 . 120.3(3) yes C11 . C12 . C13 . 121.7(2) yes C11 . C12 . H121 . 119.5 no C13 . C12 . H121 . 118.8 no C7 . C13 . C12 . 118.4(2) yes C7 . C13 . C14 . 122.1(2) yes C12 . C13 . C14 . 119.4(2) yes C13 . C14 . H141 . 110.0 no C13 . C14 . H142 . 111.1 no H141 . C14 . H142 . 107.1 no C13 . C14 . H143 . 111.0 no H141 . C14 . H143 . 109.3 no H142 . C14 . H143 . 108.3 no C11 . C15 . H151 . 109.9 no C11 . C15 . H152 . 109.8 no H151 . C15 . H152 . 108.9 no C11 . C15 . H153 . 109.7 no H151 . C15 . H153 . 109.3 no H152 . C15 . H153 . 109.2 no C6 . C16 . C17 . 120.6(2) yes C6 . C16 . H161 . 118.8 no C17 . C16 . H161 . 120.5 no C16 . C17 . C18 . 117.9(2) yes C16 . C17 . H171 . 120.1 no C18 . C17 . H171 . 121.9 no C17 . C18 . C19 . 121.2(2) yes C17 . C18 . H181 . 119.3 no C19 . C18 . H181 . 119.5 no C18 . C19 . N5 . 120.7(2) yes C18 . C19 . C20 . 118.06(19) yes N5 . C19 . C20 . 121.28(19) yes C19 . C20 . C21 . 119.7(2) yes C19 . C20 . C25 . 119.0(2) yes C21 . C20 . C25 . 120.8(2) yes C20 . C21 . C22 . 118.4(2) yes C20 . C21 . C28 . 121.8(2) yes C22 . C21 . C28 . 119.7(2) yes C21 . C22 . C23 . 121.8(2) yes C21 . C22 . H221 . 119.2 no C23 . C22 . H221 . 119.0 no C22 . C23 . C24 . 118.5(2) yes C22 . C23 . C27 . 120.1(2) yes C24 . C23 . C27 . 121.4(2) yes C23 . C24 . C25 . 121.7(2) yes C23 . C24 . H241 . 120.9 no C25 . C24 . H241 . 117.4 no C20 . C25 . C24 . 118.5(2) yes C20 . C25 . C26 . 121.1(2) yes C24 . C25 . C26 . 120.4(2) yes C25 . C26 . H262 . 110.7 no C25 . C26 . H261 . 109.6 no H262 . C26 . H261 . 110.0 no C25 . C26 . H263 . 111.0 no H262 . C26 . H263 . 107.1 no H261 . C26 . H263 . 108.4 no C23 . C27 . H272 . 109.9 no C23 . C27 . H271 . 109.1 no H272 . C27 . H271 . 109.1 no C23 . C27 . H273 . 109.9 no H272 . C27 . H273 . 109.1 no H271 . C27 . H273 . 109.6 no C21 . C28 . H282 . 110.9 no C21 . C28 . H281 . 108.3 no H282 . C28 . H281 . 108.6 no C21 . C28 . H283 . 112.2 no H282 . C28 . H283 . 107.7 no H281 . C28 . H283 . 109.1 no # Attachment '[LNHCBBr2][AlBr4].cif' data_[LNHCBBr2][AlBr4] _database_code_depnum_ccdc_archive 'CCDC 839370' #TrackingRef '[LNHCBBr2][AlBr4].cif' _audit_creation_date 11-06-25 _audit_creation_method CRYSTALS_ver_14.06 _oxford_structure_analysis_title '6241856 Compound X' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 14.9451(2) _cell_length_b 15.0835(2) _cell_length_c 15.2202(2) _cell_angle_alpha 100.9013(5) _cell_angle_beta 95.1777(5) _cell_angle_gamma 105.9880(5) _cell_volume 3201.74(7) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Al 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C44 H44 Al2 B2 Br12 F2 N4 # Dc = 1.76 Fooo = 1708.00 Mu = 75.70 M = 1701.29 # Found Formula = C50 H61 Al2 B2 Br12 F1 N4 # Dc = 1.84 FOOO = 1708.00 Mu = 75.72 M = 1771.49 _chemical_formula_sum 'C50 H61 Al2 B2 Br12 F1 N4' _chemical_formula_moiety 'C50 H61 Al2 B2 Br12 F1 N4' _chemical_compound_source ? _chemical_formula_weight 1771.49 _cell_measurement_reflns_used 13593 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.220 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_max 0.340 _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 7.572 # Sheldrick geometric approximatio 0.14 0.19 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.15 _exptl_absorpt_correction_T_max 0.19 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 80911 _reflns_number_total 14561 _diffrn_reflns_av_R_equivalents 0.036 # Number of reflections without Friedels Law is 25333 # Number of reflections with Friedels Law is 14561 # Theoretical number of reflections is about 14663 _diffrn_reflns_theta_min 1.378 _diffrn_reflns_theta_max 27.468 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.644 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min -19 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 2.97 _oxford_diffrn_Wilson_scale 28.80 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.86 _refine_diff_density_max 1.87 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 14545 _refine_ls_number_restraints 0 _refine_ls_number_parameters 641 _oxford_refine_ls_R_factor_ref 0.0753 _refine_ls_wR_factor_ref 0.0769 _refine_ls_goodness_of_fit_ref 0.9449 _refine_ls_shift/su_max 0.0010109 _refine_ls_shift/su_mean 0.0000280 # The values computed from all data _oxford_reflns_number_all 14545 _refine_ls_R_factor_all 0.0753 _refine_ls_wR_factor_all 0.0769 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10636 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_gt 0.0625 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 12.6 13.5 4.30 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Br1 Br -0.39927(4) 0.59495(4) 1.08886(4) 0.0306 1.0000 Uani . . . . . . . B2 B -0.3939(4) 0.6690(4) 1.0012(4) 0.0258 1.0000 Uani . . . . . . . Br3 Br -0.50574(4) 0.67549(4) 0.94011(4) 0.0358 1.0000 Uani . . . . . . . C4 C -0.2923(3) 0.7236(3) 0.9808(3) 0.0205 1.0000 Uani . . . . . . . N5 N -0.2476(3) 0.6770(3) 0.9279(3) 0.0236 1.0000 Uani . . . . . . . C6 C -0.2966(4) 0.5797(3) 0.8824(3) 0.0233 1.0000 Uani . . . . . . . C7 C -0.2801(4) 0.5067(4) 0.9191(4) 0.0315 1.0000 Uani . . . . . . . C8 C -0.2077(5) 0.5250(5) 1.0010(5) 0.0459 1.0000 Uani . . . . . . . C9 C -0.3335(5) 0.4147(4) 0.8761(5) 0.0406 1.0000 Uani . . . . . . . C10 C -0.3984(5) 0.3952(4) 0.7992(5) 0.0435 1.0000 Uani . . . . . . . C11 C -0.4578(5) 0.2956(5) 0.7569(6) 0.0659 1.0000 Uani . . . . . . . C12 C -0.4091(4) 0.4698(4) 0.7624(4) 0.0404 1.0000 Uani . . . . . . . C13 C -0.3580(4) 0.5628(4) 0.8015(4) 0.0283 1.0000 Uani . . . . . . . C14 C -0.3667(5) 0.6420(4) 0.7586(4) 0.0407 1.0000 Uani . . . . . . . C15 C -0.1527(4) 0.7227(4) 0.9098(4) 0.0313 1.0000 Uani . . . . . . . C16 C -0.1374(4) 0.8279(4) 0.9183(4) 0.0335 1.0000 Uani . . . . . . . C17 C -0.1607(4) 0.8700(4) 1.0081(4) 0.0315 1.0000 Uani . . . . . . . N18 N -0.2544(3) 0.8146(3) 1.0209(3) 0.0234 1.0000 Uani . . . . . . . C19 C -0.3088(3) 0.8606(3) 1.0776(3) 0.0207 1.0000 Uani . . . . . . . C20 C -0.3640(4) 0.9082(4) 1.0388(4) 0.0264 1.0000 Uani . . . . . . . C21 C -0.3663(5) 0.9149(4) 0.9413(4) 0.0388 1.0000 Uani . . . . . . . C22 C -0.4178(4) 0.9488(4) 1.0938(4) 0.0302 1.0000 Uani . . . . . . . C23 C -0.4193(4) 0.9421(4) 1.1835(4) 0.0282 1.0000 Uani . . . . . . . C24 C -0.3609(4) 0.8967(4) 1.2199(4) 0.0259 1.0000 Uani . . . . . . . C25 C -0.3031(4) 0.8562(3) 1.1685(3) 0.0228 1.0000 Uani . . . . . . . C26 C -0.2380(4) 0.8121(4) 1.2122(4) 0.0323 1.0000 Uani . . . . . . . C27 C -0.4836(4) 0.9819(5) 1.2388(4) 0.0401 1.0000 Uani . . . . . . . Br28 Br 0.04800(4) 0.39556(4) 0.55861(4) 0.0367 1.0000 Uani . . . . . . . B29 B -0.0815(4) 0.3334(4) 0.5247(4) 0.0260 1.0000 Uani . . . . . . . Br30 Br -0.14309(5) 0.34109(4) 0.41371(4) 0.0370 1.0000 Uani . . . . . . . C31 C -0.1380(3) 0.2752(3) 0.5905(3) 0.0199 1.0000 Uani . . . . . . . N32 N -0.1507(3) 0.1833(3) 0.5754(3) 0.0222 1.0000 Uani . . . . . . . C33 C -0.1133(4) 0.1408(3) 0.4987(3) 0.0216 1.0000 Uani . . . . . . . C34 C -0.0222(4) 0.1348(3) 0.5119(3) 0.0237 1.0000 Uani . . . . . . . C35 C 0.0126(4) 0.0967(4) 0.4365(4) 0.0267 1.0000 Uani . . . . . . . C36 C -0.0417(4) 0.0646(3) 0.3517(3) 0.0233 1.0000 Uani . . . . . . . C37 C -0.1333(4) 0.0681(3) 0.3423(3) 0.0225 1.0000 Uani . . . . . . . C38 C -0.1726(4) 0.1046(3) 0.4157(3) 0.0220 1.0000 Uani . . . . . . . C39 C -0.2727(4) 0.1053(4) 0.4038(4) 0.0339 1.0000 Uani . . . . . . . C40 C -0.0006(4) 0.0282(4) 0.2703(4) 0.0343 1.0000 Uani . . . . . . . C41 C 0.0395(4) 0.1687(4) 0.6030(4) 0.0373 1.0000 Uani . . . . . . . C42 C -0.2018(4) 0.1227(4) 0.6317(4) 0.0325 1.0000 Uani . . . . . . . C43 C -0.2645(5) 0.1698(4) 0.6813(4) 0.0377 1.0000 Uani . . . . . . . C44 C -0.2140(4) 0.2711(4) 0.7260(4) 0.0336 1.0000 Uani . . . . . . . N45 N -0.1669(3) 0.3211(3) 0.6601(3) 0.0249 1.0000 Uani . . . . . . . C46 C -0.1545(4) 0.4210(3) 0.6680(3) 0.0241 1.0000 Uani . . . . . . . C47 C -0.0764(4) 0.4858(4) 0.7251(4) 0.0280 1.0000 Uani . . . . . . . C48 C -0.0625(4) 0.5809(4) 0.7259(4) 0.0345 1.0000 Uani . . . . . . . C49 C -0.1234(5) 0.6118(4) 0.6743(4) 0.0365 1.0000 Uani . . . . . . . C50 C -0.2037(5) 0.5450(4) 0.6230(4) 0.0386 1.0000 Uani . . . . . . . C51 C -0.2216(4) 0.4486(4) 0.6190(4) 0.0296 1.0000 Uani . . . . . . . C52 C -0.3099(4) 0.3782(5) 0.5658(4) 0.0397 1.0000 Uani . . . . . . . C53 C -0.1039(6) 0.7145(4) 0.6723(5) 0.0544 1.0000 Uani . . . . . . . C54 C -0.0090(4) 0.4556(5) 0.7839(4) 0.0433 1.0000 Uani . . . . . . . Br55 Br -0.26700(5) -0.13115(5) 0.45833(4) 0.0431 1.0000 Uani . . . . . . . Al56 Al -0.37839(12) -0.18763(12) 0.54381(11) 0.0272 1.0000 Uani . . . . . . . Br57 Br -0.41989(5) -0.35036(4) 0.50726(5) 0.0442 1.0000 Uani . . . . . . . Br58 Br -0.31497(6) -0.12614(5) 0.69329(4) 0.0540 1.0000 Uani . . . . . . . Br59 Br -0.50473(5) -0.13585(5) 0.51204(6) 0.0599 1.0000 Uani . . . . . . . Br60 Br -0.06929(4) 0.34661(4) 0.99869(5) 0.0422 1.0000 Uani . . . . . . . Al61 Al -0.16035(12) 0.19587(11) 0.99387(11) 0.0271 1.0000 Uani . . . . . . . Br62 Br -0.31504(4) 0.18522(5) 0.95580(5) 0.0432 1.0000 Uani . . . . . . . Br63 Br -0.13798(5) 0.16002(6) 1.13175(5) 0.0535 1.0000 Uani . . . . . . . Br64 Br -0.11484(6) 0.09339(5) 0.88835(5) 0.0529 1.0000 Uani . . . . . . . F65 F 0.2119(5) 0.4461(6) 0.7702(4) 0.1150 1.0000 Uani . . . . . . . C66 C 0.2677(7) 0.5264(11) 0.7495(6) 0.0858 1.0000 Uani . . . . . . . C67 C 0.2650(6) 0.6123(10) 0.7925(5) 0.0818 1.0000 Uani . . . . . . . C68 C 0.3227(7) 0.6901(10) 0.7704(6) 0.1020 1.0000 Uani . . . . . . . C69 C 0.3806(7) 0.6763(13) 0.7042(9) 0.1208 1.0000 Uani . . . . . . . C70 C 0.3795(9) 0.5869(16) 0.6645(8) 0.1397 1.0000 Uani . . . . . . . C71 C 0.3223(8) 0.5093(12) 0.6863(6) 0.1187 1.0000 Uani . . . . . . . H81 H -0.2191 0.4713 1.0290 0.0771 1.0000 Uiso R . . . . . . H82 H -0.2081 0.5795 1.0445 0.0769 1.0000 Uiso R . . . . . . H83 H -0.1458 0.5366 0.9844 0.0775 1.0000 Uiso R . . . . . . H91 H -0.3250 0.3645 0.8993 0.0531 1.0000 Uiso R . . . . . . H111 H -0.5228 0.2929 0.7484 0.1019 1.0000 Uiso R . . . . . . H113 H -0.4493 0.2552 0.7961 0.1022 1.0000 Uiso R . . . . . . H112 H -0.4402 0.2741 0.6997 0.1019 1.0000 Uiso R . . . . . . H121 H -0.4503 0.4556 0.7078 0.0521 1.0000 Uiso R . . . . . . H141 H -0.4007 0.6172 0.6985 0.0641 1.0000 Uiso R . . . . . . H143 H -0.3990 0.6796 0.7933 0.0641 1.0000 Uiso R . . . . . . H142 H -0.3053 0.6812 0.7553 0.0642 1.0000 Uiso R . . . . . . H151 H -0.1073 0.7135 0.9537 0.0386 1.0000 Uiso R . . . . . . H152 H -0.1460 0.6934 0.8498 0.0391 1.0000 Uiso R . . . . . . H161 H -0.0720 0.8579 0.9156 0.0403 1.0000 Uiso R . . . . . . H162 H -0.1767 0.8361 0.8686 0.0398 1.0000 Uiso R . . . . . . H171 H -0.1604 0.9355 1.0093 0.0380 1.0000 Uiso R . . . . . . H172 H -0.1139 0.8703 1.0566 0.0380 1.0000 Uiso R . . . . . . H212 H -0.4045 0.9535 0.9280 0.0598 1.0000 Uiso R . . . . . . H211 H -0.3040 0.9444 0.9308 0.0604 1.0000 Uiso R . . . . . . H213 H -0.3901 0.8535 0.9009 0.0600 1.0000 Uiso R . . . . . . H221 H -0.4570 0.9796 1.0691 0.0343 1.0000 Uiso R . . . . . . H241 H -0.3584 0.8947 1.2801 0.0348 1.0000 Uiso R . . . . . . H261 H -0.2721 0.7669 1.2430 0.0536 1.0000 Uiso R . . . . . . H262 H -0.1908 0.8594 1.2555 0.0531 1.0000 Uiso R . . . . . . H263 H -0.2087 0.7803 1.1679 0.0532 1.0000 Uiso R . . . . . . H271 H -0.4799 0.9676 1.2978 0.0659 1.0000 Uiso R . . . . . . H272 H -0.4656 1.0479 1.2448 0.0659 1.0000 Uiso R . . . . . . H273 H -0.5469 0.9562 1.2091 0.0659 1.0000 Uiso R . . . . . . H351 H 0.0741 0.0913 0.4442 0.0310 1.0000 Uiso R . . . . . . H371 H -0.1700 0.0435 0.2859 0.0293 1.0000 Uiso R . . . . . . H391 H -0.2964 0.0950 0.3404 0.0512 1.0000 Uiso R . . . . . . H392 H -0.3091 0.0558 0.4277 0.0508 1.0000 Uiso R . . . . . . H393 H -0.2767 0.1660 0.4369 0.0510 1.0000 Uiso R . . . . . . H401 H -0.0075 0.0635 0.2247 0.0563 1.0000 Uiso R . . . . . . H402 H -0.0321 -0.0371 0.2458 0.0563 1.0000 Uiso R . . . . . . H403 H 0.0646 0.0361 0.2863 0.0561 1.0000 Uiso R . . . . . . H411 H 0.0650 0.1199 0.6154 0.0602 1.0000 Uiso R . . . . . . H412 H 0.0041 0.1839 0.6496 0.0602 1.0000 Uiso R . . . . . . H413 H 0.0907 0.2233 0.6033 0.0603 1.0000 Uiso R . . . . . . H422 H -0.1572 0.1106 0.6746 0.0426 1.0000 Uiso R . . . . . . H421 H -0.2381 0.0639 0.5919 0.0431 1.0000 Uiso R . . . . . . H431 H -0.2862 0.1354 0.7267 0.0466 1.0000 Uiso R . . . . . . H432 H -0.3179 0.1678 0.6372 0.0473 1.0000 Uiso R . . . . . . H441 H -0.2567 0.3039 0.7499 0.0449 1.0000 Uiso R . . . . . . H442 H -0.1664 0.2735 0.7754 0.0447 1.0000 Uiso R . . . . . . H481 H -0.0109 0.6252 0.7630 0.0461 1.0000 Uiso R . . . . . . H501 H -0.2478 0.5657 0.5911 0.0508 1.0000 Uiso R . . . . . . H522 H -0.3621 0.4031 0.5673 0.0651 1.0000 Uiso R . . . . . . H521 H -0.3241 0.3231 0.5904 0.0657 1.0000 Uiso R . . . . . . H523 H -0.3019 0.3590 0.5038 0.0647 1.0000 Uiso R . . . . . . H532 H -0.1571 0.7355 0.6864 0.0851 1.0000 Uiso R . . . . . . H531 H -0.0506 0.7510 0.7165 0.0855 1.0000 Uiso R . . . . . . H533 H -0.0908 0.7250 0.6140 0.0852 1.0000 Uiso R . . . . . . H541 H 0.0514 0.5036 0.7995 0.0701 1.0000 Uiso R . . . . . . H543 H -0.0342 0.4467 0.8380 0.0700 1.0000 Uiso R . . . . . . H542 H -0.0008 0.3983 0.7521 0.0699 1.0000 Uiso R . . . . . . H671 H 0.2262 0.6194 0.8360 0.0997 1.0000 Uiso R . . . . . . H681 H 0.3242 0.7511 0.7986 0.1241 1.0000 Uiso R . . . . . . H691 H 0.4191 0.7283 0.6869 0.1430 1.0000 Uiso R . . . . . . H701 H 0.4157 0.5789 0.6186 0.1650 1.0000 Uiso R . . . . . . H711 H 0.3199 0.4481 0.6596 0.1368 1.0000 Uiso 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 Br1 0.0350(3) 0.0286(3) 0.0296(3) 0.0110(2) 0.0096(2) 0.0076(2) B2 0.028(3) 0.024(3) 0.028(3) 0.004(2) 0.009(3) 0.010(3) Br3 0.0231(3) 0.0388(3) 0.0477(4) 0.0147(3) 0.0018(2) 0.0104(2) C4 0.020(2) 0.023(3) 0.021(2) 0.007(2) 0.0016(19) 0.010(2) N5 0.024(2) 0.021(2) 0.028(2) 0.0056(18) 0.0095(18) 0.0095(18) C6 0.029(3) 0.020(2) 0.025(3) 0.006(2) 0.012(2) 0.011(2) C7 0.039(3) 0.033(3) 0.035(3) 0.011(2) 0.022(3) 0.024(3) C8 0.057(4) 0.048(4) 0.051(4) 0.027(3) 0.013(3) 0.033(3) C9 0.058(4) 0.025(3) 0.054(4) 0.013(3) 0.042(4) 0.024(3) C10 0.047(4) 0.026(3) 0.055(4) -0.001(3) 0.035(3) 0.004(3) C11 0.058(5) 0.035(4) 0.094(6) -0.006(4) 0.049(5) -0.003(3) C12 0.037(3) 0.039(3) 0.036(3) -0.003(3) 0.016(3) 0.002(3) C13 0.031(3) 0.030(3) 0.026(3) 0.005(2) 0.011(2) 0.011(2) C14 0.045(4) 0.047(4) 0.031(3) 0.013(3) 0.000(3) 0.014(3) C15 0.026(3) 0.033(3) 0.040(3) 0.008(3) 0.017(2) 0.014(2) C16 0.032(3) 0.029(3) 0.041(3) 0.007(3) 0.013(3) 0.008(2) C17 0.023(3) 0.029(3) 0.040(3) 0.005(2) 0.011(2) 0.004(2) N18 0.021(2) 0.024(2) 0.026(2) 0.0033(18) 0.0059(18) 0.0081(18) C19 0.017(2) 0.014(2) 0.028(3) -0.0031(19) 0.005(2) 0.0031(19) C20 0.030(3) 0.024(3) 0.027(3) 0.007(2) 0.005(2) 0.008(2) C21 0.061(4) 0.036(3) 0.030(3) 0.013(3) 0.012(3) 0.027(3) C22 0.027(3) 0.025(3) 0.036(3) -0.002(2) 0.000(2) 0.011(2) C23 0.018(3) 0.027(3) 0.030(3) -0.007(2) 0.001(2) 0.002(2) C24 0.022(3) 0.027(3) 0.020(3) -0.003(2) -0.001(2) 0.001(2) C25 0.023(3) 0.017(2) 0.023(3) -0.002(2) -0.002(2) 0.003(2) C26 0.034(3) 0.034(3) 0.026(3) -0.001(2) -0.004(2) 0.013(3) C27 0.028(3) 0.051(4) 0.037(3) -0.010(3) 0.004(3) 0.017(3) Br28 0.0280(3) 0.0335(3) 0.0411(3) 0.0035(3) 0.0112(3) -0.0019(2) B29 0.031(3) 0.016(3) 0.030(3) 0.002(2) 0.008(3) 0.007(2) Br30 0.0462(4) 0.0382(3) 0.0282(3) 0.0127(3) 0.0066(3) 0.0112(3) C31 0.015(2) 0.021(2) 0.019(2) 0.0016(19) 0.0032(19) 0.0014(19) N32 0.028(2) 0.016(2) 0.021(2) 0.0017(17) 0.0106(18) 0.0034(17) C33 0.028(3) 0.016(2) 0.021(3) 0.0020(19) 0.007(2) 0.007(2) C34 0.029(3) 0.019(2) 0.022(3) 0.002(2) -0.001(2) 0.009(2) C35 0.027(3) 0.024(3) 0.033(3) 0.007(2) 0.006(2) 0.014(2) C36 0.031(3) 0.016(2) 0.023(3) 0.003(2) 0.009(2) 0.006(2) C37 0.029(3) 0.016(2) 0.020(2) 0.0016(19) 0.005(2) 0.005(2) C38 0.024(3) 0.014(2) 0.027(3) 0.002(2) 0.004(2) 0.004(2) C39 0.025(3) 0.030(3) 0.041(3) -0.003(3) 0.001(2) 0.007(2) C40 0.044(3) 0.036(3) 0.030(3) 0.007(3) 0.021(3) 0.018(3) C41 0.047(4) 0.041(3) 0.025(3) 0.006(3) -0.006(3) 0.020(3) C42 0.048(4) 0.019(3) 0.031(3) 0.009(2) 0.018(3) 0.006(2) C43 0.048(4) 0.030(3) 0.039(3) 0.013(3) 0.025(3) 0.007(3) C44 0.041(3) 0.031(3) 0.027(3) 0.003(2) 0.018(3) 0.007(3) N45 0.031(2) 0.019(2) 0.025(2) 0.0011(18) 0.0115(19) 0.0072(18) C46 0.028(3) 0.018(2) 0.024(3) 0.000(2) 0.013(2) 0.003(2) C47 0.031(3) 0.021(3) 0.025(3) -0.006(2) 0.011(2) 0.002(2) C48 0.040(3) 0.024(3) 0.033(3) -0.004(2) 0.020(3) 0.001(2) C49 0.054(4) 0.022(3) 0.035(3) 0.002(2) 0.029(3) 0.011(3) C50 0.049(4) 0.037(3) 0.038(3) 0.011(3) 0.020(3) 0.020(3) C51 0.030(3) 0.031(3) 0.028(3) 0.002(2) 0.012(2) 0.010(2) C52 0.027(3) 0.049(4) 0.039(3) 0.003(3) 0.007(3) 0.010(3) C53 0.084(6) 0.026(3) 0.056(4) 0.010(3) 0.041(4) 0.012(3) C54 0.038(4) 0.044(4) 0.039(4) -0.001(3) 0.000(3) 0.006(3) Br55 0.0355(3) 0.0596(4) 0.0367(3) 0.0176(3) 0.0153(3) 0.0103(3) Al56 0.0288(9) 0.0285(9) 0.0239(8) 0.0050(7) 0.0066(7) 0.0078(7) Br57 0.0570(4) 0.0286(3) 0.0424(4) 0.0040(3) 0.0039(3) 0.0093(3) Br58 0.0903(6) 0.0403(4) 0.0230(3) 0.0052(3) 0.0025(3) 0.0091(4) Br59 0.0338(4) 0.0535(4) 0.0873(6) -0.0073(4) 0.0011(4) 0.0230(3) Br60 0.0367(3) 0.0291(3) 0.0572(4) 0.0112(3) 0.0003(3) 0.0054(3) Al61 0.0298(9) 0.0265(8) 0.0276(9) 0.0059(7) 0.0028(7) 0.0130(7) Br62 0.0280(3) 0.0387(3) 0.0607(4) 0.0092(3) -0.0050(3) 0.0113(3) Br63 0.0589(5) 0.0740(5) 0.0401(4) 0.0314(4) 0.0064(3) 0.0278(4) Br64 0.0621(5) 0.0462(4) 0.0525(4) -0.0040(3) 0.0204(4) 0.0259(4) F65 0.094(5) 0.187(7) 0.077(4) 0.021(4) 0.004(4) 0.072(5) C66 0.047(5) 0.174(12) 0.046(5) 0.028(7) 0.007(4) 0.046(7) C67 0.047(5) 0.180(11) 0.033(4) 0.026(6) 0.010(4) 0.053(6) C68 0.054(6) 0.209(14) 0.055(6) 0.046(7) -0.002(5) 0.051(7) C69 0.047(6) 0.254(19) 0.082(9) 0.098(11) 0.004(6) 0.039(9) C70 0.070(8) 0.34(3) 0.045(6) 0.054(11) 0.023(6) 0.104(13) C71 0.077(7) 0.272(18) 0.040(5) 0.028(8) 0.010(5) 0.111(10) _refine_ls_extinction_coef 39.7(15) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.19397(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 . B2 . 1.888(6) yes B2 . Br3 . 1.874(6) yes B2 . C4 . 1.604(8) yes C4 . N5 . 1.316(6) yes C4 . N18 . 1.330(6) yes N5 . C6 . 1.450(6) yes N5 . C15 . 1.470(6) yes C6 . C7 . 1.394(7) yes C6 . C13 . 1.404(7) yes C7 . C8 . 1.504(8) yes C7 . C9 . 1.395(8) yes C8 . H81 . 0.966 no C8 . H82 . 0.955 no C8 . H83 . 0.959 no C9 . C10 . 1.380(10) yes C9 . H91 . 0.928 no C10 . C11 . 1.502(8) yes C10 . C12 . 1.388(9) yes C11 . H111 . 0.956 no C11 . H113 . 0.954 no C11 . H112 . 0.956 no C12 . C13 . 1.384(8) yes C12 . H121 . 0.940 no C13 . C14 . 1.495(8) yes C14 . H141 . 0.957 no C14 . H143 . 0.958 no C14 . H142 . 0.955 no C15 . C16 . 1.518(7) yes C15 . H151 . 0.966 no C15 . H152 . 0.963 no C16 . C17 . 1.508(8) yes C16 . H161 . 0.965 no C16 . H162 . 0.964 no C17 . N18 . 1.471(6) yes C17 . H171 . 0.983 no C17 . H172 . 0.969 no N18 . C19 . 1.449(6) yes C19 . C20 . 1.395(7) yes C19 . C25 . 1.395(7) yes C20 . C21 . 1.503(7) yes C20 . C22 . 1.386(7) yes C21 . H212 . 0.956 no C21 . H211 . 0.957 no C21 . H213 . 0.962 no C22 . C23 . 1.390(8) yes C22 . H221 . 0.936 no C23 . C24 . 1.387(7) yes C23 . C27 . 1.504(7) yes C24 . C25 . 1.400(7) yes C24 . H241 . 0.920 no C25 . C26 . 1.497(7) yes C26 . H261 . 0.957 no C26 . H262 . 0.949 no C26 . H263 . 0.961 no C27 . H271 . 0.964 no C27 . H272 . 0.940 no C27 . H273 . 0.951 no Br28 . B29 . 1.879(6) yes B29 . Br30 . 1.889(6) yes B29 . C31 . 1.600(7) yes C31 . N32 . 1.318(6) yes C31 . N45 . 1.326(6) yes N32 . C33 . 1.455(6) yes N32 . C42 . 1.479(6) yes C33 . C34 . 1.388(7) yes C33 . C38 . 1.396(7) yes C34 . C35 . 1.394(7) yes C34 . C41 . 1.508(7) yes C35 . C36 . 1.384(7) yes C35 . H351 . 0.944 no C36 . C37 . 1.380(7) yes C36 . C40 . 1.509(7) yes C37 . C38 . 1.400(7) yes C37 . H371 . 0.926 no C38 . C39 . 1.495(7) yes C39 . H391 . 0.966 no C39 . H392 . 0.948 no C39 . H393 . 0.978 no C40 . H401 . 0.966 no C40 . H402 . 0.951 no C40 . H403 . 0.953 no C41 . H411 . 0.957 no C41 . H412 . 0.953 no C41 . H413 . 0.955 no C42 . C43 . 1.498(8) yes C42 . H422 . 0.968 no C42 . H421 . 0.959 no C43 . C44 . 1.498(8) yes C43 . H431 . 0.968 no C43 . H432 . 0.985 no C44 . N45 . 1.481(6) yes C44 . H441 . 0.966 no C44 . H442 . 0.975 no N45 . C46 . 1.446(6) yes C46 . C47 . 1.392(7) yes C46 . C51 . 1.396(8) yes C47 . C48 . 1.389(7) yes C47 . C54 . 1.507(8) yes C48 . C49 . 1.380(9) yes C48 . H481 . 0.925 no C49 . C50 . 1.391(9) yes C49 . C53 . 1.503(8) yes C50 . C51 . 1.391(8) yes C50 . H501 . 0.938 no C51 . C52 . 1.496(8) yes C52 . H522 . 0.955 no C52 . H521 . 0.955 no C52 . H523 . 0.960 no C53 . H532 . 0.960 no C53 . H531 . 0.955 no C53 . H533 . 0.958 no C54 . H541 . 0.965 no C54 . H543 . 0.952 no C54 . H542 . 0.952 no Br55 . Al56 . 2.2844(17) yes Al56 . Br57 . 2.3026(18) yes Al56 . Br58 . 2.2942(17) yes Al56 . Br59 . 2.2802(18) yes Br60 . Al61 . 2.2894(18) yes Al61 . Br62 . 2.2857(17) yes Al61 . Br63 . 2.2826(18) yes Al61 . Br64 . 2.2953(17) yes F65 . C66 . 1.376(13) yes C66 . C67 . 1.349(15) yes C66 . C71 . 1.351(13) yes C67 . C68 . 1.370(15) yes C67 . H671 . 0.930 no C68 . C69 . 1.409(15) yes C68 . H681 . 0.932 no C69 . C70 . 1.36(2) yes C69 . H691 . 0.934 no C70 . C71 . 1.36(2) yes C70 . H701 . 0.932 no C71 . H711 . 0.925 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 . B2 . Br3 . 119.7(3) yes Br1 . B2 . C4 . 118.1(4) yes Br3 . B2 . C4 . 122.1(4) yes B2 . C4 . N5 . 119.6(4) yes B2 . C4 . N18 . 118.5(4) yes N5 . C4 . N18 . 121.9(5) yes C4 . N5 . C6 . 118.1(4) yes C4 . N5 . C15 . 121.9(4) yes C6 . N5 . C15 . 119.9(4) yes N5 . C6 . C7 . 119.3(5) yes N5 . C6 . C13 . 118.3(4) yes C7 . C6 . C13 . 122.4(5) yes C6 . C7 . C8 . 122.2(5) yes C6 . C7 . C9 . 117.0(6) yes C8 . C7 . C9 . 120.8(5) yes C7 . C8 . H81 . 111.2 no C7 . C8 . H82 . 110.7 no H81 . C8 . H82 . 109.0 no C7 . C8 . H83 . 110.4 no H81 . C8 . H83 . 107.9 no H82 . C8 . H83 . 107.5 no C7 . C9 . C10 . 122.3(6) yes C7 . C9 . H91 . 119.3 no C10 . C9 . H91 . 118.4 no C9 . C10 . C11 . 120.9(7) yes C9 . C10 . C12 . 118.7(6) yes C11 . C10 . C12 . 120.4(7) yes C10 . C11 . H111 . 109.9 no C10 . C11 . H113 . 109.3 no H111 . C11 . H113 . 108.8 no C10 . C11 . H112 . 110.5 no H111 . C11 . H112 . 109.3 no H113 . C11 . H112 . 109.2 no C10 . C12 . C13 . 122.0(6) yes C10 . C12 . H121 . 118.1 no C13 . C12 . H121 . 119.8 no C6 . C13 . C12 . 117.4(5) yes C6 . C13 . C14 . 121.2(5) yes C12 . C13 . C14 . 121.4(6) yes C13 . C14 . H141 . 110.0 no C13 . C14 . H143 . 110.5 no H141 . C14 . H143 . 109.1 no C13 . C14 . H142 . 109.5 no H141 . C14 . H142 . 108.6 no H143 . C14 . H142 . 109.0 no N5 . C15 . C16 . 110.3(4) yes N5 . C15 . H151 . 108.3 no C16 . C15 . H151 . 109.4 no N5 . C15 . H152 . 108.9 no C16 . C15 . H152 . 110.3 no H151 . C15 . H152 . 109.6 no C15 . C16 . C17 . 109.6(5) yes C15 . C16 . H161 . 108.8 no C17 . C16 . H161 . 108.8 no C15 . C16 . H162 . 108.4 no C17 . C16 . H162 . 111.3 no H161 . C16 . H162 . 110.0 no C16 . C17 . N18 . 110.0(4) yes C16 . C17 . H171 . 109.2 no N18 . C17 . H171 . 109.3 no C16 . C17 . H172 . 109.7 no N18 . C17 . H172 . 109.6 no H171 . C17 . H172 . 108.9 no C17 . N18 . C4 . 122.5(4) yes C17 . N18 . C19 . 119.2(4) yes C4 . N18 . C19 . 118.3(4) yes N18 . C19 . C20 . 118.4(5) yes N18 . C19 . C25 . 118.8(4) yes C20 . C19 . C25 . 122.8(5) yes C19 . C20 . C21 . 121.8(5) yes C19 . C20 . C22 . 117.1(5) yes C21 . C20 . C22 . 121.1(5) yes C20 . C21 . H212 . 110.0 no C20 . C21 . H211 . 109.5 no H212 . C21 . H211 . 107.6 no C20 . C21 . H213 . 111.7 no H212 . C21 . H213 . 109.3 no H211 . C21 . H213 . 108.6 no C20 . C22 . C23 . 122.7(5) yes C20 . C22 . H221 . 118.9 no C23 . C22 . H221 . 118.3 no C22 . C23 . C24 . 118.0(5) yes C22 . C23 . C27 . 120.7(5) yes C24 . C23 . C27 . 121.3(5) yes C23 . C24 . C25 . 122.1(5) yes C23 . C24 . H241 . 119.2 no C25 . C24 . H241 . 118.7 no C24 . C25 . C19 . 117.1(5) yes C24 . C25 . C26 . 119.9(5) yes C19 . C25 . C26 . 123.0(5) yes C25 . C26 . H261 . 110.1 no C25 . C26 . H262 . 109.8 no H261 . C26 . H262 . 108.1 no C25 . C26 . H263 . 110.9 no H261 . C26 . H263 . 108.5 no H262 . C26 . H263 . 109.4 no C23 . C27 . H271 . 110.7 no C23 . C27 . H272 . 108.7 no H271 . C27 . H272 . 109.7 no C23 . C27 . H273 . 110.2 no H271 . C27 . H273 . 108.9 no H272 . C27 . H273 . 108.5 no Br28 . B29 . Br30 . 119.4(3) yes Br28 . B29 . C31 . 119.5(4) yes Br30 . B29 . C31 . 121.1(4) yes B29 . C31 . N32 . 118.4(4) yes B29 . C31 . N45 . 119.3(4) yes N32 . C31 . N45 . 122.3(4) yes C31 . N32 . C33 . 117.6(4) yes C31 . N32 . C42 . 123.0(4) yes C33 . N32 . C42 . 119.4(4) yes N32 . C33 . C34 . 118.9(4) yes N32 . C33 . C38 . 118.0(4) yes C34 . C33 . C38 . 123.1(5) yes C33 . C34 . C35 . 117.4(5) yes C33 . C34 . C41 . 122.9(5) yes C35 . C34 . C41 . 119.7(5) yes C34 . C35 . C36 . 121.6(5) yes C34 . C35 . H351 . 118.6 no C36 . C35 . H351 . 119.7 no C35 . C36 . C37 . 119.1(5) yes C35 . C36 . C40 . 120.5(5) yes C37 . C36 . C40 . 120.5(5) yes C36 . C37 . C38 . 122.0(5) yes C36 . C37 . H371 . 118.3 no C38 . C37 . H371 . 119.6 no C37 . C38 . C33 . 116.6(5) yes C37 . C38 . C39 . 120.8(5) yes C33 . C38 . C39 . 122.6(5) yes C38 . C39 . H391 . 110.2 no C38 . C39 . H392 . 108.4 no H391 . C39 . H392 . 109.1 no C38 . C39 . H393 . 109.3 no H391 . C39 . H393 . 110.3 no H392 . C39 . H393 . 109.5 no C36 . C40 . H401 . 109.2 no C36 . C40 . H402 . 110.7 no H401 . C40 . H402 . 109.2 no C36 . C40 . H403 . 110.7 no H401 . C40 . H403 . 108.5 no H402 . C40 . H403 . 108.7 no C34 . C41 . H411 . 109.5 no C34 . C41 . H412 . 110.6 no H411 . C41 . H412 . 108.7 no C34 . C41 . H413 . 110.5 no H411 . C41 . H413 . 108.3 no H412 . C41 . H413 . 109.2 no N32 . C42 . C43 . 110.2(4) yes N32 . C42 . H422 . 109.7 no C43 . C42 . H422 . 109.8 no N32 . C42 . H421 . 107.3 no C43 . C42 . H421 . 110.7 no H422 . C42 . H421 . 109.1 no C42 . C43 . C44 . 111.8(5) yes C42 . C43 . H431 . 107.9 no C44 . C43 . H431 . 109.5 no C42 . C43 . H432 . 108.2 no C44 . C43 . H432 . 108.6 no H431 . C43 . H432 . 110.8 no C43 . C44 . N45 . 110.2(4) yes C43 . C44 . H441 . 111.6 no N45 . C44 . H441 . 108.0 no C43 . C44 . H442 . 109.2 no N45 . C44 . H442 . 108.8 no H441 . C44 . H442 . 109.0 no C44 . N45 . C31 . 121.1(4) yes C44 . N45 . C46 . 120.6(4) yes C31 . N45 . C46 . 118.2(4) yes N45 . C46 . C47 . 118.6(5) yes N45 . C46 . C51 . 118.9(5) yes C47 . C46 . C51 . 122.6(5) yes C46 . C47 . C48 . 117.2(5) yes C46 . C47 . C54 . 122.2(5) yes C48 . C47 . C54 . 120.6(5) yes C47 . C48 . C49 . 122.5(6) yes C47 . C48 . H481 . 118.7 no C49 . C48 . H481 . 118.8 no C48 . C49 . C50 . 118.2(5) yes C48 . C49 . C53 . 121.5(6) yes C50 . C49 . C53 . 120.3(6) yes C49 . C50 . C51 . 122.0(6) yes C49 . C50 . H501 . 118.9 no C51 . C50 . H501 . 119.1 no C46 . C51 . C50 . 117.2(5) yes C46 . C51 . C52 . 121.6(5) yes C50 . C51 . C52 . 121.2(6) yes C51 . C52 . H522 . 111.7 no C51 . C52 . H521 . 109.3 no H522 . C52 . H521 . 108.6 no C51 . C52 . H523 . 110.6 no H522 . C52 . H523 . 108.9 no H521 . C52 . H523 . 107.6 no C49 . C53 . H532 . 110.1 no C49 . C53 . H531 . 109.1 no H532 . C53 . H531 . 108.7 no C49 . C53 . H533 . 111.1 no H532 . C53 . H533 . 109.0 no H531 . C53 . H533 . 108.8 no C47 . C54 . H541 . 110.4 no C47 . C54 . H543 . 108.6 no H541 . C54 . H543 . 109.0 no C47 . C54 . H542 . 109.5 no H541 . C54 . H542 . 108.9 no H543 . C54 . H542 . 110.4 no Br55 . Al56 . Br57 . 108.08(7) yes Br55 . Al56 . Br58 . 107.88(7) yes Br57 . Al56 . Br58 . 112.27(7) yes Br55 . Al56 . Br59 . 108.38(7) yes Br57 . Al56 . Br59 . 111.03(7) yes Br58 . Al56 . Br59 . 109.07(7) yes Br60 . Al61 . Br62 . 109.05(7) yes Br60 . Al61 . Br63 . 109.94(7) yes Br62 . Al61 . Br63 . 109.85(7) yes Br60 . Al61 . Br64 . 108.28(7) yes Br62 . Al61 . Br64 . 110.83(7) yes Br63 . Al61 . Br64 . 108.87(7) yes F65 . C66 . C67 . 119.8(9) yes F65 . C66 . C71 . 114.1(13) yes C67 . C66 . C71 . 126.1(13) yes C66 . C67 . C68 . 117.6(10) yes C66 . C67 . H671 . 122.0 no C68 . C67 . H671 . 120.3 no C67 . C68 . C69 . 118.7(13) yes C67 . C68 . H681 . 121.1 no C69 . C68 . H681 . 120.3 no C68 . C69 . C70 . 120.0(14) yes C68 . C69 . H691 . 120.1 no C70 . C69 . H691 . 119.9 no C69 . C70 . C71 . 121.6(12) yes C69 . C70 . H701 . 118.9 no C71 . C70 . H701 . 119.4 no C70 . C71 . C66 . 116.1(14) yes C70 . C71 . H711 . 122.9 no C66 . C71 . H711 . 121.0 no # Attachment '[LpyBBr2][AlBr4].cif' data_[LpyBBr2][AlBr4] _database_code_depnum_ccdc_archive 'CCDC 839371' #TrackingRef '[LpyBBr2][AlBr4].cif' _audit_creation_date 10-09-30 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title '9301421 037hmct10' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 12.42260(10) _cell_length_b 13.30580(10) _cell_length_c 18.02260(10) _cell_angle_alpha 90 _cell_angle_beta 103.5928(3) _cell_angle_gamma 90 _cell_volume 2895.56(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Al 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C40 H20 Al1 B1 Br5 N1 # Dc = 2.18 Fooo = 1592.00 Mu = 70.08 M = 951.92 # Found Formula = C23 H25 Al1 B1 Br6 N1 # Dc = 1.91 FOOO = 1592.00 Mu = 83.62 M = 832.68 _chemical_formula_sum 'C23 H25 Al1 B1 Br6 N1' _chemical_formula_moiety 'C23 H25 Al1 B1 Br6 N1' _chemical_compound_source ? _chemical_formula_weight 832.68 _cell_measurement_reflns_used 6811 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.21 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 8.362 # Sheldrick geometric approximatio 0.16 0.17 # No experimental values of Tmin/max available _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.16 _exptl_absorpt_correction_T_max 0.17 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 13133 _reflns_number_total 6593 _diffrn_reflns_av_R_equivalents 0.021 # Number of reflections with Friedels Law is 6593 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 6642 _diffrn_reflns_theta_min 5.124 _diffrn_reflns_theta_max 27.485 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.485 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 2.84 _oxford_diffrn_Wilson_scale 11.44 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.51 _refine_diff_density_max 2.04 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 6593 _refine_ls_number_restraints 0 _refine_ls_number_parameters 290 _oxford_refine_ls_R_factor_ref 0.0400 _refine_ls_wR_factor_ref 0.0715 _refine_ls_goodness_of_fit_ref 1.0073 _refine_ls_shift/su_max 0.001358 # The values computed from all data _oxford_reflns_number_all 6593 _refine_ls_R_factor_all 0.0400 _refine_ls_wR_factor_all 0.0715 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5719 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_gt 0.0678 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 7.68P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Br1 Br 0.21386(3) 0.72187(3) 0.49689(2) 0.0421 1.0000 Uani . . . . . . . Al2 Al 0.37368(8) 0.66503(7) 0.57748(6) 0.0268 1.0000 Uani . . . . . . . Br3 Br 0.52223(3) 0.74056(2) 0.54439(2) 0.0338 1.0000 Uani . . . . . . . Br4 Br 0.36911(3) 0.70799(3) 0.70065(2) 0.0424 1.0000 Uani . . . . . . . Br5 Br 0.38523(3) 0.49461(3) 0.56894(3) 0.0469 1.0000 Uani . . . . . . . Br6 Br 0.17247(3) 0.57393(2) 0.14900(2) 0.0363 1.0000 Uani . . . . . . . B7 B 0.1361(3) 0.4377(3) 0.13442(19) 0.0242 1.0000 Uani . . . . . . . Br8 Br -0.00484(3) 0.39882(3) 0.077818(19) 0.0340 1.0000 Uani . . . . . . . N9 N 0.21965(18) 0.35553(17) 0.16726(13) 0.0178 1.0000 Uani . . . . . . . C10 C 0.2185(2) 0.3146(2) 0.23686(16) 0.0213 1.0000 Uani . . . . . . . C11 C 0.1409(2) 0.3603(2) 0.27881(15) 0.0211 1.0000 Uani . . . . . . . C12 C 0.1760(2) 0.4441(2) 0.32544(16) 0.0241 1.0000 Uani . . . . . . . C13 C 0.2922(3) 0.4849(3) 0.3389(2) 0.0325 1.0000 Uani . . . . . . . C14 C 0.1007(3) 0.4880(2) 0.36210(17) 0.0280 1.0000 Uani . . . . . . . C15 C -0.0051(3) 0.4505(2) 0.35451(17) 0.0289 1.0000 Uani . . . . . . . C16 C -0.0859(3) 0.5010(3) 0.3935(2) 0.0447 1.0000 Uani . . . . . . . C17 C -0.0363(3) 0.3645(2) 0.31027(17) 0.0280 1.0000 Uani . . . . . . . C18 C 0.0352(2) 0.3180(2) 0.27236(16) 0.0242 1.0000 Uani . . . . . . . C19 C -0.0018(3) 0.2238(3) 0.22624(19) 0.0319 1.0000 Uani . . . . . . . C20 C 0.2902(3) 0.2370(2) 0.26394(17) 0.0275 1.0000 Uani . . . . . . . C21 C 0.3619(3) 0.2013(2) 0.22142(18) 0.0289 1.0000 Uani . . . . . . . C22 C 0.3616(3) 0.2449(2) 0.15165(18) 0.0258 1.0000 Uani . . . . . . . C23 C 0.2906(2) 0.3226(2) 0.12491(16) 0.0196 1.0000 Uani . . . . . . . C24 C 0.2836(2) 0.3752(2) 0.05125(15) 0.0200 1.0000 Uani . . . . . . . C25 C 0.3512(2) 0.4592(2) 0.04963(17) 0.0235 1.0000 Uani . . . . . . . C26 C 0.3395(3) 0.5107(2) -0.01900(18) 0.0285 1.0000 Uani . . . . . . . C27 C 0.2639(3) 0.4794(3) -0.08478(17) 0.0286 1.0000 Uani . . . . . . . C28 C 0.2017(3) 0.3937(3) -0.08198(17) 0.0290 1.0000 Uani . . . . . . . C29 C 0.2112(2) 0.3389(2) -0.01519(17) 0.0254 1.0000 Uani . . . . . . . C30 C 0.1492(3) 0.2415(3) -0.0156(2) 0.0393 1.0000 Uani . . . . . . . C31 C 0.2506(3) 0.5382(3) -0.1579(2) 0.0442 1.0000 Uani . . . . . . . C32 C 0.4350(3) 0.4935(3) 0.11990(19) 0.0350 1.0000 Uani . . . . . . . H131 H 0.2928 0.5546 0.3515 0.0493 1.0000 Uiso R . . . . . . H133 H 0.3393 0.4492 0.3801 0.0492 1.0000 Uiso R . . . . . . H132 H 0.3194 0.4767 0.2933 0.0491 1.0000 Uiso R . . . . . . H141 H 0.1226 0.5442 0.3925 0.0330 1.0000 Uiso R . . . . . . H162 H -0.1534 0.5160 0.3562 0.0701 1.0000 Uiso R . . . . . . H161 H -0.1017 0.4565 0.4323 0.0700 1.0000 Uiso R . . . . . . H163 H -0.0537 0.5624 0.4173 0.0701 1.0000 Uiso R . . . . . . H171 H -0.1067 0.3377 0.3061 0.0331 1.0000 Uiso R . . . . . . H191 H -0.0795 0.2273 0.2035 0.0482 1.0000 Uiso R . . . . . . H192 H 0.0133 0.1655 0.2582 0.0483 1.0000 Uiso R . . . . . . H193 H 0.0369 0.2180 0.1860 0.0482 1.0000 Uiso R . . . . . . H201 H 0.2909 0.2088 0.3110 0.0318 1.0000 Uiso R . . . . . . H211 H 0.4093 0.1483 0.2399 0.0341 1.0000 Uiso R . . . . . . H221 H 0.4092 0.2216 0.1230 0.0299 1.0000 Uiso R . . . . . . H261 H 0.3837 0.5667 -0.0212 0.0359 1.0000 Uiso R . . . . . . H281 H 0.1518 0.3719 -0.1263 0.0349 1.0000 Uiso R . . . . . . H302 H 0.0835 0.2438 -0.0555 0.0593 1.0000 Uiso R . . . . . . H301 H 0.1943 0.1865 -0.0243 0.0591 1.0000 Uiso R . . . . . . H303 H 0.1295 0.2325 0.0326 0.0589 1.0000 Uiso R . . . . . . H312 H 0.1791 0.5252 -0.1901 0.0690 1.0000 Uiso R . . . . . . H311 H 0.2570 0.6088 -0.1471 0.0691 1.0000 Uiso R . . . . . . H313 H 0.3058 0.5190 -0.1847 0.0690 1.0000 Uiso R . . . . . . H322 H 0.4815 0.5452 0.1076 0.0521 1.0000 Uiso R . . . . . . H321 H 0.3974 0.5191 0.1562 0.0522 1.0000 Uiso R . . . . . . H323 H 0.4803 0.4380 0.1425 0.0522 1.0000 Uiso 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 Br1 0.03580(19) 0.03291(18) 0.0485(2) 0.00022(15) -0.00857(15) 0.00509(14) Al2 0.0254(4) 0.0203(4) 0.0342(5) 0.0044(4) 0.0062(4) 0.0010(3) Br3 0.03382(17) 0.02838(17) 0.04183(19) 0.00403(13) 0.01420(14) -0.00280(13) Br4 0.0395(2) 0.0559(2) 0.03243(18) 0.00194(16) 0.00940(15) -0.00446(16) Br5 0.0465(2) 0.02000(16) 0.0785(3) 0.00716(16) 0.0235(2) 0.00349(14) Br6 0.0482(2) 0.01914(15) 0.0438(2) 0.00089(13) 0.01505(15) 0.00147(13) B7 0.0265(16) 0.0251(16) 0.0226(16) 0.0013(13) 0.0089(13) 0.0000(13) Br8 0.02238(15) 0.0447(2) 0.03208(17) 0.00784(14) 0.00094(12) 0.00049(13) N9 0.0193(11) 0.0175(11) 0.0165(11) -0.0014(9) 0.0039(9) -0.0018(9) C10 0.0226(13) 0.0232(14) 0.0174(13) -0.0012(11) 0.0032(11) -0.0043(11) C11 0.0244(14) 0.0246(14) 0.0148(12) 0.0024(11) 0.0052(11) 0.0010(11) C12 0.0262(15) 0.0264(15) 0.0193(14) 0.0018(11) 0.0046(11) -0.0009(12) C13 0.0300(17) 0.0304(17) 0.0359(18) -0.0049(13) 0.0055(14) -0.0066(13) C14 0.0382(17) 0.0247(15) 0.0215(14) 0.0020(12) 0.0076(13) 0.0054(13) C15 0.0326(16) 0.0353(17) 0.0211(15) 0.0085(12) 0.0107(12) 0.0099(13) C16 0.046(2) 0.050(2) 0.044(2) 0.0068(17) 0.0236(18) 0.0168(18) C17 0.0228(14) 0.0374(17) 0.0245(15) 0.0098(13) 0.0072(12) 0.0023(12) C18 0.0259(14) 0.0295(15) 0.0165(13) 0.0043(11) 0.0038(11) -0.0021(12) C19 0.0327(17) 0.0340(17) 0.0281(16) 0.0011(13) 0.0055(13) -0.0101(14) C20 0.0309(16) 0.0279(16) 0.0232(15) 0.0071(12) 0.0053(12) 0.0017(12) C21 0.0299(16) 0.0231(15) 0.0327(16) 0.0068(12) 0.0051(13) 0.0076(12) C22 0.0274(15) 0.0234(14) 0.0286(15) -0.0024(12) 0.0104(12) 0.0034(12) C23 0.0199(13) 0.0194(13) 0.0195(13) -0.0032(10) 0.0047(10) -0.0039(10) C24 0.0224(13) 0.0218(14) 0.0173(13) -0.0023(11) 0.0082(10) 0.0018(11) C25 0.0262(14) 0.0249(14) 0.0220(14) -0.0014(11) 0.0107(12) 0.0011(11) C26 0.0319(16) 0.0273(16) 0.0310(16) 0.0037(13) 0.0166(13) 0.0025(12) C27 0.0278(15) 0.0372(17) 0.0238(15) 0.0069(13) 0.0123(12) 0.0112(13) C28 0.0273(15) 0.0422(18) 0.0171(14) -0.0038(13) 0.0041(11) 0.0061(13) C29 0.0273(15) 0.0291(16) 0.0203(14) -0.0069(12) 0.0069(11) 0.0000(12) C30 0.049(2) 0.0366(19) 0.0312(18) -0.0108(14) 0.0079(16) -0.0125(16) C31 0.046(2) 0.057(2) 0.0315(19) 0.0205(17) 0.0128(16) 0.0155(18) C32 0.0344(18) 0.0423(19) 0.0283(17) -0.0021(14) 0.0076(14) -0.0144(15) _refine_ls_extinction_coef 71(5) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.28022(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 . Al2 . 2.2952(10) yes Al2 . Br3 . 2.2996(10) yes Al2 . Br4 . 2.3058(10) yes Al2 . Br5 . 2.2795(10) yes Br6 . B7 . 1.872(3) yes B7 . Br8 . 1.880(3) yes B7 . N9 . 1.528(4) yes N9 . C10 . 1.370(4) yes N9 . C23 . 1.366(4) yes C10 . C11 . 1.487(4) yes C10 . C20 . 1.377(4) yes C11 . C12 . 1.402(4) yes C11 . C18 . 1.409(4) yes C12 . C13 . 1.508(4) yes C12 . C14 . 1.395(4) yes C13 . H131 . 0.955 no C13 . H133 . 0.957 no C13 . H132 . 0.965 no C14 . C15 . 1.382(5) yes C14 . H141 . 0.929 no C15 . C16 . 1.510(4) yes C15 . C17 . 1.397(5) yes C16 . H162 . 0.965 no C16 . H161 . 0.970 no C16 . H163 . 0.965 no C17 . C18 . 1.387(4) yes C17 . H171 . 0.931 no C18 . C19 . 1.514(4) yes C19 . H191 . 0.957 no C19 . H192 . 0.958 no C19 . H193 . 0.963 no C20 . C21 . 1.388(4) yes C20 . H201 . 0.925 no C21 . C22 . 1.384(4) yes C21 . H211 . 0.929 no C22 . C23 . 1.371(4) yes C22 . H221 . 0.926 no C23 . C24 . 1.485(4) yes C24 . C25 . 1.402(4) yes C24 . C29 . 1.404(4) yes C25 . C26 . 1.392(4) yes C25 . C32 . 1.509(4) yes C26 . C27 . 1.392(5) yes C26 . H261 . 0.932 no C27 . C28 . 1.385(5) yes C27 . C31 . 1.508(4) yes C28 . C29 . 1.389(4) yes C28 . H281 . 0.934 no C29 . C30 . 1.506(5) yes C30 . H302 . 0.954 no C30 . H301 . 0.957 no C30 . H303 . 0.964 no C31 . H312 . 0.956 no C31 . H311 . 0.959 no C31 . H313 . 0.962 no C32 . H322 . 0.957 no C32 . H321 . 0.953 no C32 . H323 . 0.960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 . Al2 . Br3 . 108.63(4) yes Br1 . Al2 . Br4 . 108.31(4) yes Br3 . Al2 . Br4 . 110.13(4) yes Br1 . Al2 . Br5 . 110.11(4) yes Br3 . Al2 . Br5 . 110.50(4) yes Br4 . Al2 . Br5 . 109.13(4) yes Br6 . B7 . Br8 . 120.39(18) yes Br6 . B7 . N9 . 121.3(2) yes Br8 . B7 . N9 . 118.3(2) yes B7 . N9 . C10 . 119.1(2) yes B7 . N9 . C23 . 118.8(2) yes C10 . N9 . C23 . 122.1(2) yes N9 . C10 . C11 . 116.8(2) yes N9 . C10 . C20 . 118.5(3) yes C11 . C10 . C20 . 124.7(3) yes C10 . C11 . C12 . 118.8(3) yes C10 . C11 . C18 . 119.8(3) yes C12 . C11 . C18 . 121.3(3) yes C11 . C12 . C13 . 122.3(3) yes C11 . C12 . C14 . 117.9(3) yes C13 . C12 . C14 . 119.8(3) yes C12 . C13 . H131 . 110.0 no C12 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.2 no C12 . C13 . H132 . 109.6 no H131 . C13 . H132 . 109.1 no H133 . C13 . H132 . 109.4 no C12 . C14 . C15 . 122.1(3) yes C12 . C14 . H141 . 118.7 no C15 . C14 . H141 . 119.2 no C14 . C15 . C16 . 121.0(3) yes C14 . C15 . C17 . 118.8(3) yes C16 . C15 . C17 . 120.3(3) yes C15 . C16 . H162 . 109.4 no C15 . C16 . H161 . 109.5 no H162 . C16 . H161 . 109.8 no C15 . C16 . H163 . 109.4 no H162 . C16 . H163 . 109.6 no H161 . C16 . H163 . 109.2 no C15 . C17 . C18 . 121.5(3) yes C15 . C17 . H171 . 119.3 no C18 . C17 . H171 . 119.1 no C11 . C18 . C17 . 118.3(3) yes C11 . C18 . C19 . 122.2(3) yes C17 . C18 . C19 . 119.5(3) yes C18 . C19 . H191 . 109.9 no C18 . C19 . H192 . 110.4 no H191 . C19 . H192 . 109.3 no C18 . C19 . H193 . 109.9 no H191 . C19 . H193 . 108.3 no H192 . C19 . H193 . 109.0 no C10 . C20 . C21 . 120.5(3) yes C10 . C20 . H201 . 119.7 no C21 . C20 . H201 . 119.9 no C20 . C21 . C22 . 119.5(3) yes C20 . C21 . H211 . 119.8 no C22 . C21 . H211 . 120.6 no C21 . C22 . C23 . 120.0(3) yes C21 . C22 . H221 . 120.1 no C23 . C22 . H221 . 119.9 no C22 . C23 . N9 . 119.4(3) yes C22 . C23 . C24 . 124.5(3) yes N9 . C23 . C24 . 116.0(2) yes C23 . C24 . C25 . 119.0(2) yes C23 . C24 . C29 . 119.4(3) yes C25 . C24 . C29 . 121.6(3) yes C24 . C25 . C26 . 118.2(3) yes C24 . C25 . C32 . 121.5(3) yes C26 . C25 . C32 . 120.3(3) yes C25 . C26 . C27 . 121.2(3) yes C25 . C26 . H261 . 119.5 no C27 . C26 . H261 . 119.3 no C26 . C27 . C28 . 119.1(3) yes C26 . C27 . C31 . 120.2(3) yes C28 . C27 . C31 . 120.8(3) yes C27 . C28 . C29 . 122.0(3) yes C27 . C28 . H281 . 119.2 no C29 . C28 . H281 . 118.9 no C24 . C29 . C28 . 117.8(3) yes C24 . C29 . C30 . 121.6(3) yes C28 . C29 . C30 . 120.6(3) yes C29 . C30 . H302 . 108.8 no C29 . C30 . H301 . 110.0 no H302 . C30 . H301 . 109.3 no C29 . C30 . H303 . 110.0 no H302 . C30 . H303 . 109.3 no H301 . C30 . H303 . 109.5 no C27 . C31 . H312 . 109.4 no C27 . C31 . H311 . 110.1 no H312 . C31 . H311 . 108.8 no C27 . C31 . H313 . 110.8 no H312 . C31 . H313 . 108.5 no H311 . C31 . H313 . 109.1 no C25 . C32 . H322 . 111.0 no C25 . C32 . H321 . 109.4 no H322 . C32 . H321 . 108.8 no C25 . C32 . H323 . 110.2 no H322 . C32 . H323 . 109.0 no H321 . C32 . H323 . 108.5 no # Attachment '[LpyBBr2][BBr4].cif' data_[LpyBBr2][BBr4] _database_code_depnum_ccdc_archive 'CCDC 839372' #TrackingRef '[LpyBBr2][BBr4].cif' _audit_creation_date 10-09-07 _audit_creation_method CRYSTALS_ver_14.06 _oxford_structure_analysis_title '9072332 029HMCT10' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 11.8539(2) _cell_length_b 13.1384(3) _cell_length_c 18.3488(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2857.67(10) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c n n ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,-y+1/2,z+1/2 -x+1/2,y+1/2,-z+1/2 -x+1/2,-y+1/2,z x+1/2,y+1/2,-z x,-y,-z+1/2 -x,y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C24 B1 Br6 # Dc = 1.81 Fooo = 1560.00 Mu = 84.38 M = 389.25 # Found Formula = C23 H25 B2 Br6 N1 # Dc = 1.90 FOOO = 1560.00 Mu = 84.42 M = 408.25 _chemical_formula_sum 'C23 H25 B2 Br6 N1' _chemical_formula_moiety 'C23 H25 B2 Br6 N1' _chemical_compound_source ? _chemical_formula_weight 816.50 _cell_measurement_reflns_used 3516 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour 'pale brown' _exptl_crystal_size_min 1.000 _exptl_crystal_size_mid 1.000 _exptl_crystal_size_max 1.000 _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 8.442 # Sheldrick geometric approximatio 0.00 0.00 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.00 _exptl_absorpt_correction_T_max 0.00 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 6088 _reflns_number_total 3257 _diffrn_reflns_av_R_equivalents 0.032 # Number of reflections without Friedels Law is 6458 # Number of reflections with Friedels Law is 3257 # Theoretical number of reflections is about 3273 _diffrn_reflns_theta_min 5.138 _diffrn_reflns_theta_max 27.473 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.923 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 2.83 _oxford_diffrn_Wilson_scale 48.52 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.99 _refine_diff_density_max 1.12 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 3257 _refine_ls_number_restraints 4 _refine_ls_number_parameters 150 _oxford_refine_ls_R_factor_ref 0.0578 _refine_ls_wR_factor_ref 0.0740 _refine_ls_goodness_of_fit_ref 0.9830 _refine_ls_shift/su_max 0.0011193 _refine_ls_shift/su_mean 0.0000372 # The values computed from all data _oxford_reflns_number_all 3257 _refine_ls_R_factor_all 0.0578 _refine_ls_wR_factor_all 0.0740 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2506 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_gt 0.0676 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 8.34P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Br1 Br 0.47410(3) 0.42634(3) 0.82205(2) 0.0351 1.0000 Uani . . . . . . . Br2 Br 0.85427(4) 0.16935(3) 0.66188(2) 0.0364 1.0000 Uani . . . . . . . Br3 Br 0.27826(4) 0.39862(4) 0.69752(3) 0.0563 1.0000 Uani . . . . . . . N4 N 0.7500 0.2500 0.5273(2) 0.0232 1.0000 Uani S T . . . . . C5 C 0.7094(3) 0.1662(3) 0.49083(18) 0.0244 1.0000 Uani . . . . . . . C6 C 0.7116(3) 0.1657(3) 0.41603(19) 0.0301 1.0000 Uani . . . . . . . C7 C 0.750000(7) 0.250000(7) 0.3778(3) 0.0308 1.0000 Uani S T . . . . . C8 C 0.6656(3) 0.0826(3) 0.53730(18) 0.0256 1.0000 Uani . . . . . . . C9 C 0.5595(3) 0.0933(3) 0.5700(2) 0.0301 1.0000 Uani . . . . . . . C10 C 0.4782(3) 0.1765(3) 0.5507(2) 0.0380 1.0000 Uani . . . . . . . C11 C 0.5273(3) 0.0190(3) 0.6207(2) 0.0364 1.0000 Uani . . . . . . . C12 C 0.5944(4) -0.0628(3) 0.6376(2) 0.0383 1.0000 Uani . . . . . . . C13 C 0.5595(5) -0.1393(4) 0.6947(3) 0.0594 1.0000 Uani . . . . . . . C14 C 0.6966(4) -0.0736(3) 0.6008(2) 0.0363 1.0000 Uani . . . . . . . C15 C 0.7337(3) -0.0033(3) 0.55021(19) 0.0289 1.0000 Uani . . . . . . . C16 C 0.8455(3) -0.0166(3) 0.5123(2) 0.0374 1.0000 Uani . . . . . . . B1 B 0.7500 0.2500 0.6107(3) 0.0276 1.0000 Uani S T . . . . . B2 B 0.3758(5) 0.5000 0.7500 0.0313 1.0000 Uani S T . . . . . H61 H 0.6871 0.1077 0.3907 0.0383 1.0000 Uiso R . . . . . . H71 H 0.7500 0.2500 0.3270 0.0390 1.0000 Uiso RS . . . . . . H101 H 0.4169 0.1817 0.5860 0.0607 1.0000 Uiso R . . . . . . H102 H 0.5159 0.2415 0.5466 0.0603 1.0000 Uiso R . . . . . . H103 H 0.4472 0.1602 0.5046 0.0607 1.0000 Uiso R . . . . . . H111 H 0.4578 0.0250 0.6442 0.0458 1.0000 Uiso R . . . . . . H131 H 0.6116 -0.1938 0.6943 0.0944 1.0000 Uiso R . . . . . . H133 H 0.5609 -0.1092 0.7416 0.0947 1.0000 Uiso R . . . . . . H132 H 0.4851 -0.1664 0.6859 0.0943 1.0000 Uiso R . . . . . . H141 H 0.7407 -0.1305 0.6107 0.0466 1.0000 Uiso R . . . . . . H162 H 0.8819 -0.0781 0.5280 0.0596 1.0000 Uiso R . . . . . . H161 H 0.8938 0.0420 0.5224 0.0595 1.0000 Uiso R . . . . . . H163 H 0.8339 -0.0223 0.4603 0.0594 1.0000 Uiso 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 Br1 0.0377(2) 0.0347(2) 0.0329(2) 0.00574(16) -0.00521(16) 0.00436(17) Br2 0.0455(2) 0.0331(2) 0.0306(2) 0.00045(16) -0.01098(17) 0.00380(18) Br3 0.0624(3) 0.0570(3) 0.0495(3) 0.0168(2) -0.0227(2) -0.0301(2) N4 0.025(2) 0.024(2) 0.021(2) 0.0000 0.0000 0.0003(17) C5 0.0244(17) 0.0233(18) 0.0255(17) -0.0021(14) -0.0009(14) 0.0009(15) C6 0.036(2) 0.029(2) 0.0256(18) -0.0050(15) -0.0030(15) -0.0002(17) C7 0.042(3) 0.029(3) 0.022(2) 0.0000 0.0000 0.001(2) C8 0.0310(19) 0.0227(18) 0.0230(17) -0.0007(14) -0.0056(15) -0.0050(15) C9 0.032(2) 0.032(2) 0.0269(18) -0.0029(15) -0.0043(15) -0.0104(16) C10 0.029(2) 0.042(2) 0.043(2) -0.0003(19) -0.0023(18) -0.0023(18) C11 0.040(2) 0.041(2) 0.0287(19) -0.0031(17) 0.0035(17) -0.0126(19) C12 0.055(3) 0.032(2) 0.0275(19) 0.0011(16) -0.0016(19) -0.018(2) C13 0.087(4) 0.047(3) 0.044(3) 0.014(2) 0.003(3) -0.027(3) C14 0.055(3) 0.023(2) 0.031(2) 0.0027(16) -0.0097(18) -0.0038(18) C15 0.036(2) 0.0258(19) 0.0249(17) -0.0040(14) -0.0044(16) -0.0038(16) C16 0.043(2) 0.035(2) 0.034(2) -0.0012(17) 0.0002(18) 0.0075(19) B1 0.035(3) 0.025(3) 0.023(3) 0.0000 0.0000 -0.002(3) B2 0.033(3) 0.035(4) 0.027(3) 0.006(3) 0.0000 0.0000 _refine_ls_extinction_coef 48(6) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.15466(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 . B2 . 2.010(4) yes Br2 . B1 . 1.880(3) yes Br3 . B2 . 2.010(4) yes N4 . C5 5_655 1.375(4) yes N4 . C5 . 1.375(4) yes N4 . B1 . 1.530(7) yes C5 . C6 . 1.373(5) yes C5 . C8 . 1.484(5) yes C6 . C7 . 1.388(5) yes C6 . H61 . 0.938 no C7 . H71 . 0.933 no C8 . C9 . 1.400(5) yes C8 . C15 . 1.408(5) yes C9 . C10 . 1.500(5) yes C9 . C11 . 1.402(5) yes C10 . H101 . 0.976 no C10 . H102 . 0.966 no C10 . H103 . 0.946 no C11 . C12 . 1.373(6) yes C11 . H111 . 0.933 no C12 . C13 . 1.510(5) yes C12 . C14 . 1.393(6) yes C13 . H131 . 0.945 no C13 . H133 . 0.947 no C13 . H132 . 0.966 no C14 . C15 . 1.382(5) yes C14 . H141 . 0.930 no C15 . C16 . 1.506(5) yes C16 . H162 . 0.960 no C16 . H161 . 0.977 no C16 . H163 . 0.967 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C5 5_655 N4 . C5 . 121.8(4) yes C5 5_655 N4 . B1 . 119.1(2) yes C5 . N4 . B1 . 119.1(2) yes N4 . C5 . C6 . 118.9(3) yes N4 . C5 . C8 . 115.8(3) yes C6 . C5 . C8 . 125.2(3) yes C5 . C6 . C7 . 120.5(4) yes C5 . C6 . H61 . 119.6 no C7 . C6 . H61 . 120.0 no C6 . C7 . C6 5_655 119.3(5) yes C6 . C7 . H71 . 120.3 no C6 5_655 C7 . H71 . 120.3 no C5 . C8 . C9 . 119.1(3) yes C5 . C8 . C15 . 119.3(3) yes C9 . C8 . C15 . 121.6(3) yes C8 . C9 . C10 . 123.3(3) yes C8 . C9 . C11 . 117.3(4) yes C10 . C9 . C11 . 119.3(3) yes C9 . C10 . H101 . 111.8 no C9 . C10 . H102 . 111.4 no H101 . C10 . H102 . 109.5 no C9 . C10 . H103 . 107.1 no H101 . C10 . H103 . 108.7 no H102 . C10 . H103 . 108.2 no C9 . C11 . C12 . 122.5(4) yes C9 . C11 . H111 . 119.2 no C12 . C11 . H111 . 118.3 no C11 . C12 . C13 . 121.3(4) yes C11 . C12 . C14 . 118.3(4) yes C13 . C12 . C14 . 120.4(4) yes C12 . C13 . H131 . 108.7 no C12 . C13 . H133 . 110.3 no H131 . C13 . H133 . 108.2 no C12 . C13 . H132 . 112.3 no H131 . C13 . H132 . 108.5 no H133 . C13 . H132 . 108.8 no C12 . C14 . C15 . 122.3(4) yes C12 . C14 . H141 . 118.5 no C15 . C14 . H141 . 119.2 no C8 . C15 . C14 . 117.8(3) yes C8 . C15 . C16 . 121.3(3) yes C14 . C15 . C16 . 120.9(4) yes C15 . C16 . H162 . 110.8 no C15 . C16 . H161 . 109.7 no H162 . C16 . H161 . 110.1 no C15 . C16 . H163 . 109.8 no H162 . C16 . H163 . 107.2 no H161 . C16 . H163 . 109.2 no Br2 . B1 . Br2 5_655 120.0(3) yes Br2 . B1 . N4 . 119.99(15) yes Br2 5_655 B1 . N4 . 119.99(15) yes Br1 . B2 . Br1 7_566 109.2(3) yes Br1 . B2 . Br3 . 109.237(18) yes Br1 7_566 B2 . Br3 . 109.723(18) yes Br1 . B2 . Br3 7_566 109.723(18) yes Br1 7_566 B2 . Br3 7_566 109.237(18) yes Br3 . B2 . Br3 7_566 109.7(3) yes # Attachment '[LpyBcat][AlCl4].cif' data_[LpyBcat][AlCl4] _database_code_depnum_ccdc_archive 'CCDC 839373' #TrackingRef '[LpyBcat][AlCl4].cif' _audit_creation_date 11-06-08 _audit_creation_method CRYSTALS_ver_14.06 _oxford_structure_analysis_title '6081134 054armk11' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 9.2145(3) _cell_length_b 12.0905(4) _cell_length_c 14.8659(5) _cell_angle_alpha 105.3386(12) _cell_angle_beta 107.5650(13) _cell_angle_gamma 93.3676(13) _cell_volume 1505.32(9) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Al 0.0645 0.0514 6.4202 3.0387 1.9002 0.7426 1.5936 31.5472 1.9646 85.0886 1.1151 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C1 Al1 B30 Cl4 O2 # Dc = 1.18 Fooo = 624.00 Mu = 4.27 M = 537.13 # Found Formula = C29 H29 Al1 B1 Cl4 N1 O2 # Dc = 1.33 FOOO = 624.00 Mu = 4.50 M = 603.16 _chemical_formula_sum 'C29 H29 Al1 B1 Cl4 N1 O2' _chemical_formula_moiety 'C29 H29 B N O2, Al Cl4' _chemical_compound_source . _chemical_formula_weight 603.16 _cell_measurement_reflns_used 5094 _cell_measurement_theta_min 5 _cell_measurement_theta_max 25 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.450 # Sheldrick geometric approximatio 0.94 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.96 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 25940 _reflns_number_total 5396 _diffrn_reflns_av_R_equivalents 0.000 # Number of reflections without Friedels Law is 9490 # Number of reflections with Friedels Law is 5396 # Theoretical number of reflections is about 5484 _diffrn_reflns_theta_min 5.124 _diffrn_reflns_theta_max 25.301 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.301 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -11 _reflns_limit_h_max 10 _reflns_limit_k_min -14 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 3.38 _oxford_diffrn_Wilson_scale 1.92 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.90 _refine_diff_density_max 1.09 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 5393 _refine_ls_number_restraints 0 _refine_ls_number_parameters 344 _oxford_refine_ls_R_factor_ref 0.0668 _refine_ls_wR_factor_ref 0.1777 _refine_ls_goodness_of_fit_ref 1.3142 _refine_ls_shift/su_max 0.0003140 _refine_ls_shift/su_mean 0.0000185 # The values computed from all data _oxford_reflns_number_all 5396 _refine_ls_R_factor_all 0.0669 _refine_ls_wR_factor_all 0.1781 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4415 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_gt 0.1672 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.10P)^2^ + 0.00P] ,where P=p(6)*max(Fo^2^,0) + (1-p(6))Fc^2^ ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cl1 Cl 0.87083(8) 0.51797(6) 0.31085(5) 0.0469 1.0000 Uani . . . . . . . Al2 Al 0.97732(9) 0.63365(6) 0.25386(6) 0.0370 1.0000 Uani . . . . . . . Cl3 Cl 0.92868(15) 0.55908(9) 0.09915(6) 0.0849 1.0000 Uani . . . . . . . Cl4 Cl 1.21907(10) 0.65868(11) 0.32182(8) 0.0798 1.0000 Uani . . . . . . . Cl5 Cl 0.89275(16) 0.79268(9) 0.27989(13) 0.1124 1.0000 Uani . . . . . . . O6 O 0.55819(19) 0.30962(14) 0.32677(12) 0.0334 1.0000 Uani . . . . . . . C7 C 0.6873(3) 0.2545(2) 0.35252(18) 0.0307 1.0000 Uani . . . . . . . C8 C 0.8240(3) 0.2964(2) 0.42799(19) 0.0390 1.0000 Uani . . . . . . . C9 C 0.9280(3) 0.2184(2) 0.4404(2) 0.0405 1.0000 Uani . . . . . . . C10 C 0.8967(3) 0.1056(2) 0.3774(2) 0.0395 1.0000 Uani . . . . . . . C11 C 0.7581(3) 0.0650(2) 0.3004(2) 0.0376 1.0000 Uani . . . . . . . C12 C 0.6548(3) 0.1413(2) 0.29046(17) 0.0302 1.0000 Uani . . . . . . . O13 O 0.50401(19) 0.12202(13) 0.22497(12) 0.0325 1.0000 Uani . . . . . . . B14 B 0.4520(3) 0.2251(2) 0.25235(19) 0.0314 1.0000 Uani . . . . . . . N15 N 0.2881(2) 0.24249(16) 0.20849(14) 0.0314 1.0000 Uani . . . . . . . C16 C 0.2409(3) 0.2631(2) 0.11880(18) 0.0344 1.0000 Uani . . . . . . . C17 C 0.3559(3) 0.2611(2) 0.06718(17) 0.0338 1.0000 Uani . . . . . . . C18 C 0.4550(3) 0.3635(2) 0.08578(18) 0.0358 1.0000 Uani . . . . . . . C19 C 0.4457(4) 0.4761(2) 0.1572(2) 0.0447 1.0000 Uani . . . . . . . C20 C 0.5606(3) 0.3593(2) 0.03614(19) 0.0387 1.0000 Uani . . . . . . . C21 C 0.5710(3) 0.2583(2) -0.03087(18) 0.0404 1.0000 Uani . . . . . . . C22 C 0.6849(4) 0.2568(3) -0.0858(2) 0.0496 1.0000 Uani . . . . . . . C23 C 0.4713(3) 0.1585(2) -0.04716(19) 0.0444 1.0000 Uani . . . . . . . C24 C 0.3636(3) 0.1579(2) -0.00029(19) 0.0403 1.0000 Uani . . . . . . . C25 C 0.2540(4) 0.0477(3) -0.0222(2) 0.0561 1.0000 Uani . . . . . . . C26 C 0.0924(3) 0.2850(3) 0.0833(2) 0.0449 1.0000 Uani . . . . . . . C27 C -0.0052(3) 0.2849(3) 0.1379(2) 0.0453 1.0000 Uani . . . . . . . C28 C 0.0445(3) 0.2624(2) 0.22785(19) 0.0375 1.0000 Uani . . . . . . . C29 C 0.1931(3) 0.2402(2) 0.26343(18) 0.0335 1.0000 Uani . . . . . . . C30 C 0.2574(3) 0.2127(2) 0.35767(17) 0.0306 1.0000 Uani . . . . . . . C31 C 0.2616(3) 0.0975(2) 0.35736(19) 0.0344 1.0000 Uani . . . . . . . C32 C 0.1979(3) -0.0015(2) 0.2628(2) 0.0441 1.0000 Uani . . . . . . . C33 C 0.3195(3) 0.0738(2) 0.4470(2) 0.0392 1.0000 Uani . . . . . . . C34 C 0.3748(3) 0.1623(3) 0.5361(2) 0.0413 1.0000 Uani . . . . . . . C35 C 0.3670(3) 0.2760(3) 0.53461(19) 0.0415 1.0000 Uani . . . . . . . C36 C 0.3092(3) 0.3038(2) 0.44688(19) 0.0363 1.0000 Uani . . . . . . . C37 C 0.2974(4) 0.4274(2) 0.4476(2) 0.0505 1.0000 Uani . . . . . . . C38 C 0.4394(4) 0.1358(3) 0.6323(2) 0.0567 1.0000 Uani . . . . . . . H81 H 0.8472 0.3736 0.4685 0.0463 1.0000 Uiso R . . . . . . H91 H 1.0216 0.2413 0.4922 0.0471 1.0000 Uiso R . . . . . . H101 H 0.9706 0.0557 0.3892 0.0472 1.0000 Uiso R . . . . . . H111 H 0.7364 -0.0118 0.2572 0.0452 1.0000 Uiso R . . . . . . H193 H 0.5081 0.5390 0.1513 0.0653 1.0000 Uiso R . . . . . . H192 H 0.4795 0.4707 0.2226 0.0660 1.0000 Uiso R . . . . . . H191 H 0.3401 0.4886 0.1408 0.0656 1.0000 Uiso R . . . . . . H201 H 0.6273 0.4266 0.0468 0.0451 1.0000 Uiso R . . . . . . H223 H 0.7402 0.1934 -0.0845 0.0719 1.0000 Uiso R . . . . . . H222 H 0.7574 0.3286 -0.0598 0.0731 1.0000 Uiso R . . . . . . H221 H 0.6282 0.2489 -0.1540 0.0727 1.0000 Uiso R . . . . . . H231 H 0.4768 0.0904 -0.0901 0.0532 1.0000 Uiso R . . . . . . H252 H 0.2822 -0.0169 -0.0647 0.0841 1.0000 Uiso R . . . . . . H251 H 0.2566 0.0319 0.0388 0.0833 1.0000 Uiso R . . . . . . H253 H 0.1517 0.0599 -0.0548 0.0844 1.0000 Uiso R . . . . . . H261 H 0.0603 0.2998 0.0237 0.0535 1.0000 Uiso R . . . . . . H271 H -0.1074 0.2997 0.1134 0.0549 1.0000 Uiso R . . . . . . H281 H -0.0205 0.2628 0.2674 0.0440 1.0000 Uiso R . . . . . . H323 H 0.1916 -0.0743 0.2773 0.0653 1.0000 Uiso R . . . . . . H322 H 0.2603 -0.0060 0.2213 0.0657 1.0000 Uiso R . . . . . . H321 H 0.0972 0.0044 0.2261 0.0649 1.0000 Uiso R . . . . . . H331 H 0.3184 -0.0040 0.4471 0.0475 1.0000 Uiso R . . . . . . H351 H 0.4026 0.3372 0.5951 0.0493 1.0000 Uiso R . . . . . . H372 H 0.3432 0.4764 0.5151 0.0748 1.0000 Uiso R . . . . . . H371 H 0.3512 0.4495 0.4054 0.0747 1.0000 Uiso R . . . . . . H373 H 0.1894 0.4350 0.4225 0.0743 1.0000 Uiso R . . . . . . H382 H 0.3870 0.1694 0.6760 0.0842 1.0000 Uiso R . . . . . . H381 H 0.5461 0.1683 0.6600 0.0842 1.0000 Uiso R . . . . . . H383 H 0.4291 0.0515 0.6211 0.0844 1.0000 Uiso 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 Cl1 0.0517(4) 0.0473(4) 0.0536(4) 0.0255(3) 0.0255(3) 0.0062(3) Al2 0.0372(4) 0.0353(4) 0.0462(5) 0.0184(3) 0.0182(4) 0.0100(3) Cl3 0.1225(9) 0.0819(7) 0.0452(5) 0.0221(4) 0.0259(5) -0.0293(6) Cl4 0.0396(5) 0.1253(9) 0.0884(7) 0.0618(7) 0.0159(4) 0.0059(5) Cl5 0.1249(10) 0.0649(6) 0.2208(16) 0.0794(8) 0.1209(11) 0.0604(7) O6 0.0291(9) 0.0338(9) 0.0368(9) 0.0108(7) 0.0088(7) 0.0104(7) C7 0.0283(12) 0.0344(12) 0.0346(12) 0.0140(10) 0.0132(10) 0.0112(10) C8 0.0304(13) 0.0464(14) 0.0378(14) 0.0082(11) 0.0114(11) 0.0069(11) C9 0.0264(12) 0.0582(16) 0.0404(14) 0.0205(12) 0.0103(11) 0.0108(11) C10 0.0318(13) 0.0473(14) 0.0493(15) 0.0232(12) 0.0175(12) 0.0173(11) C11 0.0346(13) 0.0390(13) 0.0460(15) 0.0185(11) 0.0164(12) 0.0139(11) C12 0.0256(12) 0.0357(12) 0.0327(12) 0.0151(10) 0.0095(10) 0.0091(9) O13 0.0303(9) 0.0291(8) 0.0356(9) 0.0078(7) 0.0082(7) 0.0086(7) B14 0.0291(14) 0.0392(14) 0.0283(13) 0.0131(11) 0.0095(11) 0.0086(11) N15 0.0308(11) 0.0335(10) 0.0304(10) 0.0110(8) 0.0081(9) 0.0112(8) C16 0.0350(13) 0.0338(12) 0.0350(13) 0.0127(10) 0.0094(11) 0.0092(10) C17 0.0335(13) 0.0405(13) 0.0278(12) 0.0140(10) 0.0060(10) 0.0114(10) C18 0.0361(13) 0.0436(14) 0.0296(12) 0.0145(11) 0.0090(10) 0.0137(11) C19 0.0541(17) 0.0403(14) 0.0453(15) 0.0131(12) 0.0223(13) 0.0154(12) C20 0.0395(14) 0.0392(13) 0.0376(14) 0.0123(11) 0.0116(11) 0.0093(11) C21 0.0346(13) 0.0574(16) 0.0276(13) 0.0128(11) 0.0063(10) 0.0137(12) C22 0.0492(17) 0.0646(18) 0.0364(15) 0.0112(13) 0.0178(13) 0.0184(14) C23 0.0457(16) 0.0512(16) 0.0329(13) 0.0082(12) 0.0102(12) 0.0148(13) C24 0.0383(14) 0.0438(14) 0.0339(14) 0.0114(11) 0.0045(11) 0.0092(11) C25 0.0603(19) 0.0433(16) 0.0582(19) 0.0074(14) 0.0180(16) 0.0020(14) C26 0.0377(14) 0.0627(17) 0.0419(15) 0.0290(13) 0.0106(12) 0.0172(13) C27 0.0319(14) 0.0621(17) 0.0474(16) 0.0262(13) 0.0100(12) 0.0184(12) C28 0.0307(13) 0.0441(13) 0.0413(14) 0.0171(11) 0.0118(11) 0.0132(11) C29 0.0301(13) 0.0383(13) 0.0351(13) 0.0139(10) 0.0112(10) 0.0112(10) C30 0.0235(11) 0.0388(13) 0.0321(12) 0.0131(10) 0.0096(10) 0.0097(10) C31 0.0266(12) 0.0396(13) 0.0418(14) 0.0167(11) 0.0134(10) 0.0092(10) C32 0.0432(15) 0.0416(14) 0.0466(16) 0.0133(12) 0.0126(13) 0.0090(12) C33 0.0311(13) 0.0493(15) 0.0477(15) 0.0260(12) 0.0164(11) 0.0133(11) C34 0.0258(12) 0.0667(18) 0.0411(15) 0.0271(13) 0.0141(11) 0.0126(12) C35 0.0297(13) 0.0584(17) 0.0332(13) 0.0079(12) 0.0103(11) 0.0086(12) C36 0.0283(12) 0.0454(14) 0.0366(13) 0.0121(11) 0.0115(10) 0.0119(11) C37 0.0473(16) 0.0393(14) 0.0542(18) 0.0047(13) 0.0084(14) 0.0122(12) C38 0.0487(17) 0.087(2) 0.0463(17) 0.0362(16) 0.0179(14) 0.0127(16) _refine_ls_extinction_coef 90(60) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.809(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 . Al2 . 2.1457(10) yes Al2 . Cl3 . 2.1300(12) yes Al2 . Cl4 . 2.1155(11) yes Al2 . Cl5 . 2.1021(12) yes O6 . C7 . 1.400(3) yes O6 . B14 . 1.363(3) yes C7 . C8 . 1.369(3) yes C7 . C12 . 1.389(3) yes C8 . C9 . 1.391(4) yes C8 . H81 . 0.938 no C9 . C10 . 1.391(4) yes C9 . H91 . 0.933 no C10 . C11 . 1.389(4) yes C10 . H101 . 0.943 no C11 . C12 . 1.368(3) yes C11 . H111 . 0.948 no C12 . O13 . 1.399(3) yes O13 . B14 . 1.366(3) yes B14 . N15 . 1.505(3) yes N15 . C16 . 1.367(3) yes N15 . C29 . 1.369(3) yes C16 . C17 . 1.482(4) yes C16 . C26 . 1.379(4) yes C17 . C18 . 1.406(4) yes C17 . C24 . 1.400(4) yes C18 . C19 . 1.514(3) yes C18 . C20 . 1.384(4) yes C19 . H193 . 0.965 no C19 . H192 . 0.948 no C19 . H191 . 0.961 no C20 . C21 . 1.386(4) yes C20 . H201 . 0.937 no C21 . C22 . 1.510(4) yes C21 . C23 . 1.393(4) yes C22 . H223 . 0.946 no C22 . H222 . 0.974 no C22 . H221 . 0.966 no C23 . C24 . 1.374(4) yes C23 . H231 . 0.914 no C24 . C25 . 1.522(4) yes C25 . H252 . 0.968 no C25 . H251 . 0.970 no C25 . H253 . 0.961 no C26 . C27 . 1.381(4) yes C26 . H261 . 0.914 no C27 . C28 . 1.382(4) yes C27 . H271 . 0.948 no C28 . C29 . 1.382(3) yes C28 . H281 . 0.957 no C29 . C30 . 1.481(3) yes C30 . C31 . 1.394(3) yes C30 . C36 . 1.408(3) yes C31 . C32 . 1.511(4) yes C31 . C33 . 1.391(4) yes C32 . H323 . 0.963 no C32 . H322 . 0.955 no C32 . H321 . 0.942 no C33 . C34 . 1.392(4) yes C33 . H331 . 0.940 no C34 . C35 . 1.386(4) yes C34 . C38 . 1.500(4) yes C35 . C36 . 1.390(4) yes C35 . H351 . 0.951 no C36 . C37 . 1.503(4) yes C37 . H372 . 0.968 no C37 . H371 . 0.986 no C37 . H373 . 0.971 no C38 . H382 . 0.946 no C38 . H381 . 0.956 no C38 . H383 . 0.982 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Al2 . Cl3 . 109.85(5) yes Cl1 . Al2 . Cl4 . 109.53(5) yes Cl3 . Al2 . Cl4 . 107.58(6) yes Cl1 . Al2 . Cl5 . 109.74(5) yes Cl3 . Al2 . Cl5 . 109.46(7) yes Cl4 . Al2 . Cl5 . 110.65(6) yes C7 . O6 . B14 . 103.78(18) yes O6 . C7 . C8 . 128.9(2) yes O6 . C7 . C12 . 108.83(19) yes C8 . C7 . C12 . 122.2(2) yes C7 . C8 . C9 . 116.1(2) yes C7 . C8 . H81 . 122.1 no C9 . C8 . H81 . 121.7 no C8 . C9 . C10 . 121.7(2) yes C8 . C9 . H91 . 119.9 no C10 . C9 . H91 . 118.4 no C9 . C10 . C11 . 121.3(2) yes C9 . C10 . H101 . 118.6 no C11 . C10 . H101 . 120.1 no C10 . C11 . C12 . 116.5(2) yes C10 . C11 . H111 . 121.6 no C12 . C11 . H111 . 121.9 no C7 . C12 . C11 . 122.0(2) yes C7 . C12 . O13 . 109.04(19) yes C11 . C12 . O13 . 128.9(2) yes C12 . O13 . B14 . 103.61(18) yes O13 . B14 . O6 . 114.7(2) yes O13 . B14 . N15 . 123.0(2) yes O6 . B14 . N15 . 122.2(2) yes B14 . N15 . C16 . 120.1(2) yes B14 . N15 . C29 . 117.2(2) yes C16 . N15 . C29 . 122.7(2) yes N15 . C16 . C17 . 116.6(2) yes N15 . C16 . C26 . 118.5(2) yes C17 . C16 . C26 . 124.9(2) yes C16 . C17 . C18 . 119.5(2) yes C16 . C17 . C24 . 119.8(2) yes C18 . C17 . C24 . 120.7(2) yes C17 . C18 . C19 . 121.2(2) yes C17 . C18 . C20 . 118.3(2) yes C19 . C18 . C20 . 120.5(2) yes C18 . C19 . H193 . 109.2 no C18 . C19 . H192 . 109.7 no H193 . C19 . H192 . 110.8 no C18 . C19 . H191 . 108.4 no H193 . C19 . H191 . 110.0 no H192 . C19 . H191 . 108.6 no C18 . C20 . C21 . 122.2(3) yes C18 . C20 . H201 . 119.9 no C21 . C20 . H201 . 117.9 no C20 . C21 . C22 . 121.1(3) yes C20 . C21 . C23 . 117.9(3) yes C22 . C21 . C23 . 121.0(3) yes C21 . C22 . H223 . 112.0 no C21 . C22 . H222 . 112.0 no H223 . C22 . H222 . 109.2 no C21 . C22 . H221 . 108.1 no H223 . C22 . H221 . 107.7 no H222 . C22 . H221 . 107.6 no C21 . C23 . C24 . 122.3(3) yes C21 . C23 . H231 . 119.7 no C24 . C23 . H231 . 118.0 no C17 . C24 . C23 . 118.6(2) yes C17 . C24 . C25 . 120.8(3) yes C23 . C24 . C25 . 120.6(2) yes C24 . C25 . H252 . 109.9 no C24 . C25 . H251 . 110.1 no H252 . C25 . H251 . 110.3 no C24 . C25 . H253 . 107.9 no H252 . C25 . H253 . 109.9 no H251 . C25 . H253 . 108.8 no C16 . C26 . C27 . 120.0(2) yes C16 . C26 . H261 . 119.1 no C27 . C26 . H261 . 121.0 no C26 . C27 . C28 . 120.5(2) yes C26 . C27 . H271 . 119.9 no C28 . C27 . H271 . 119.5 no C27 . C28 . C29 . 119.6(3) yes C27 . C28 . H281 . 122.1 no C29 . C28 . H281 . 118.3 no C28 . C29 . N15 . 118.7(2) yes C28 . C29 . C30 . 124.2(2) yes N15 . C29 . C30 . 117.2(2) yes C29 . C30 . C31 . 119.9(2) yes C29 . C30 . C36 . 119.1(2) yes C31 . C30 . C36 . 120.9(2) yes C30 . C31 . C32 . 121.5(2) yes C30 . C31 . C33 . 118.8(2) yes C32 . C31 . C33 . 119.6(2) yes C31 . C32 . H323 . 110.3 no C31 . C32 . H322 . 112.6 no H323 . C32 . H322 . 107.5 no C31 . C32 . H321 . 111.7 no H323 . C32 . H321 . 106.3 no H322 . C32 . H321 . 108.2 no C31 . C33 . C34 . 121.4(3) yes C31 . C33 . H331 . 118.9 no C34 . C33 . H331 . 119.7 no C33 . C34 . C35 . 118.6(2) yes C33 . C34 . C38 . 121.0(3) yes C35 . C34 . C38 . 120.3(3) yes C34 . C35 . C36 . 121.9(3) yes C34 . C35 . H351 . 119.5 no C36 . C35 . H351 . 118.6 no C30 . C36 . C35 . 118.2(2) yes C30 . C36 . C37 . 120.9(2) yes C35 . C36 . C37 . 120.8(2) yes C36 . C37 . H372 . 108.0 no C36 . C37 . H371 . 110.6 no H372 . C37 . H371 . 110.2 no C36 . C37 . H373 . 108.7 no H372 . C37 . H373 . 110.2 no H371 . C37 . H373 . 109.1 no C34 . C38 . H382 . 109.8 no C34 . C38 . H381 . 108.0 no H382 . C38 . H381 . 109.7 no C34 . C38 . H383 . 110.2 no H382 . C38 . H383 . 109.8 no H381 . C38 . H383 . 109.4 no