# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Aldridge, S.' 'Mountford, Philip' 'Jones, Cameron' _publ_contact_author_name 'Aldridge, S.' _publ_contact_author_email simon.aldridge@chem.ox.ac.uk _publ_section_title ; Contrasting reactivity of anionic boron- and gallium-containing NHC analogues: E-C vs. E-M bond formation (E = B, Ga) ; # Attachment '- 015apdv10.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 784595' #TrackingRef '- 015apdv10.cif' _audit_creation_date 10-02-11 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 015apdv10 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 12.38040(10) _cell_length_b 16.7775(2) _cell_length_c 21.6398(2) _cell_angle_alpha 90 _cell_angle_beta 105.2587(5) _cell_angle_gamma 90 _cell_volume 4336.39(7) _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' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C45 H100 Ga1 N4 Ti1 # Dc = 1.25 Fooo = 1664.00 Mu = 8.41 M = 814.94 # Found Formula = C45 H65 Ga1 N4 Ti1 # Dc = 1.19 FOOO = 1664.00 Mu = 8.39 M = 779.66 _chemical_formula_sum 'C45 H65 Ga1 N4 Ti1' _chemical_formula_moiety 'C45 H65 Ga1 N4 Ti1' _chemical_compound_source . _chemical_formula_weight 779.66 _cell_measurement_reflns_used 10117 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour dark_brown _exptl_crystal_size_min 0.17 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.839 # Sheldrick geometric approximatio 0.84 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.87 # 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 67172 _reflns_number_total 9856 _diffrn_reflns_av_R_equivalents 0.085 # Number of reflections with Friedels Law is 9856 # Number of reflections without Friedels Law is 19444 # Theoretical number of reflections is about 9944 _diffrn_reflns_theta_min 5.101 _diffrn_reflns_theta_max 27.482 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.933 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -16 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _oxford_diffrn_Wilson_B_factor 1.90 _oxford_diffrn_Wilson_scale 49.02 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.86 _refine_diff_density_max 0.78 # 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 9855 _refine_ls_number_restraints 732 _refine_ls_number_parameters 579 _oxford_refine_ls_R_factor_ref 0.0825 _refine_ls_wR_factor_ref 0.1077 _refine_ls_goodness_of_fit_ref 0.9483 _refine_ls_shift/su_max 0.007665 # The values computed from all data _oxford_reflns_number_all 9856 _refine_ls_R_factor_all 0.0826 _refine_ls_wR_factor_all 0.1078 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6572 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_gt 0.0961 # 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^) + ( 0.05P)^2^ + 2.17P] ,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 0.94811(2) 0.693930(15) 0.691055(12) 0.0230 1.0000 Uani . . . . . . . Ti2 Ti 0.80545(3) 0.61358(2) 0.59665(2) 0.0226 1.0000 Uani . . . . . . . N3 N 0.69904(16) 0.68209(11) 0.58126(9) 0.0245 1.0000 Uani . . . . . . . C4 C 0.6090(2) 0.73975(15) 0.56292(12) 0.0307 1.0000 Uani . . . . . . . C5 C 0.6130(3) 0.79457(17) 0.61963(14) 0.0454 1.0000 Uani . . . . . . . C6 C 0.4979(2) 0.6962(2) 0.54414(19) 0.0611 1.0000 Uani . . . . . . . C7 C 0.6219(3) 0.7910(2) 0.50676(15) 0.0595 1.0000 Uani . . . . . . . N8 N 0.74659(17) 0.52897(12) 0.65702(9) 0.0283 1.0000 Uani . . . . . . . C9 C 0.8177(2) 0.49595(15) 0.70854(12) 0.0351 1.0000 Uani . . . . . . . C10 C 0.7860(3) 0.43915(17) 0.74597(13) 0.0451 1.0000 Uani . . . . . . . C11 C 0.6764(3) 0.41356(18) 0.72990(15) 0.0496 1.0000 Uani . . . . . . . C12 C 0.6018(3) 0.44747(18) 0.67794(14) 0.0472 1.0000 Uani . . . . . . . C13 C 0.6392(2) 0.50519(17) 0.64317(13) 0.0375 1.0000 Uani . . . . . . . N34 N 0.97036(16) 0.69772(11) 0.78199(9) 0.0246 1.0000 Uani . . . . . . . C35 C 1.0479(2) 0.75657(14) 0.80847(11) 0.0273 1.0000 Uani . . . . . . . C36 C 1.0917(2) 0.79894(14) 0.76859(11) 0.0272 1.0000 Uani . . . . . . . N37 N 1.05485(16) 0.77869(12) 0.70370(9) 0.0262 1.0000 Uani . . . . . . . C38 C 1.1172(2) 0.80532(14) 0.66074(11) 0.0272 1.0000 Uani . . . . . . . C39 C 1.2264(2) 0.77688(16) 0.66620(13) 0.0330 1.0000 Uani . . . . . . . C40 C 1.2803(2) 0.79800(17) 0.61954(14) 0.0418 1.0000 Uani . . . . . . . C41 C 1.2285(3) 0.84596(18) 0.56835(14) 0.0442 1.0000 Uani . . . . . . . C42 C 1.1230(3) 0.87571(17) 0.56445(14) 0.0415 1.0000 Uani . . . . . . . C43 C 1.0660(2) 0.85732(15) 0.61046(12) 0.0329 1.0000 Uani . . . . . . . C44 C 0.9546(2) 0.89594(17) 0.60909(13) 0.0393 1.0000 Uani . . . . . . . C45 C 0.9730(3) 0.9650(2) 0.65685(18) 0.0618 1.0000 Uani . . . . . . . C46 C 0.8894(3) 0.9245(2) 0.54304(16) 0.0632 1.0000 Uani . . . . . . . C47 C 1.2884(2) 0.72426(17) 0.72153(14) 0.0410 1.0000 Uani . . . . . . . C48 C 1.3750(3) 0.7739(2) 0.77068(16) 0.0530 1.0000 Uani . . . . . . . C49 C 1.3459(3) 0.6521(2) 0.70132(18) 0.0559 1.0000 Uani . . . . . . . C50 C 0.9549(2) 0.63644(14) 0.82499(11) 0.0249 1.0000 Uani . . . . . . . C51 C 0.8588(2) 0.63603(14) 0.84794(11) 0.0319 1.0000 Uani D . . . . . . C52 C 0.8475(2) 0.57649(16) 0.89087(13) 0.0384 1.0000 Uani . . . . . . . C53 C 0.9288(3) 0.51896(17) 0.91129(13) 0.0415 1.0000 Uani . . . . . . . C54 C 1.0229(2) 0.51938(16) 0.88792(13) 0.0375 1.0000 Uani . . . . . . . C55 C 1.0379(2) 0.57674(13) 0.84471(11) 0.0297 1.0000 Uani D . . . . . . C56 C 1.14226(16) 0.57583(11) 0.82053(9) 0.0359 1.0000 Uani D . . . . . . C57 C 1.1605(2) 0.49421(17) 0.79234(13) 0.0467 1.0000 Uani D . . . . . . C58 C 1.2465(2) 0.59836(17) 0.87306(14) 0.0510 1.0000 Uani D . . . . . . C70 C 0.7766(3) 0.5569(2) 0.4928(2) 0.0372 0.452(3) Uani D . P 1 1 . . C71 C 0.8290(3) 0.4966(2) 0.5356(3) 0.0367 0.452(3) Uani D . P 1 1 . . C72 C 0.9378(3) 0.5225(2) 0.5663(2) 0.0360 0.452(3) Uani D . P 1 1 . . C73 C 0.9533(3) 0.5980(2) 0.5420(2) 0.0363 0.452(3) Uani D . P 1 1 . . C74 C 0.8535(3) 0.6192(2) 0.4965(2) 0.0365 0.452(3) Uani D . P 1 1 . . C75 C 0.6610(4) 0.5515(3) 0.4458(3) 0.0467 0.452(3) Uani D . P 1 1 . . C76 C 0.7805(4) 0.4150(3) 0.5425(3) 0.0474 0.452(3) Uani D . P 1 1 . . C77 C 1.0261(4) 0.4746(3) 0.6141(3) 0.0454 0.452(3) Uani D . P 1 1 . . C78 C 1.0615(4) 0.6450(3) 0.5576(3) 0.0469 0.452(3) Uani D . P 1 1 . . C79 C 0.8362(4) 0.6929(3) 0.4540(3) 0.0461 0.452(3) Uani D . P 1 1 . . C80 C 0.9681(2) 0.57034(19) 0.56469(17) 0.0339 0.548(3) Uani D . P 1 2 . . C81 C 0.9012(3) 0.61983(19) 0.51737(18) 0.0345 0.548(3) Uani D . P 1 2 . . C82 C 0.7985(3) 0.5803(2) 0.49138(18) 0.0354 0.548(3) Uani D . P 1 2 . . C83 C 0.8012(3) 0.5079(2) 0.5239(2) 0.0328 0.548(3) Uani D . P 1 2 . . C84 C 0.9070(3) 0.50108(19) 0.5686(2) 0.0327 0.548(3) Uani D . P 1 2 . . C85 C 1.0902(3) 0.5848(2) 0.5995(2) 0.0424 0.548(3) Uani D . P 1 2 . . C86 C 0.9360(4) 0.6995(3) 0.4952(2) 0.0457 0.548(3) Uani D . P 1 2 . . C87 C 0.7072(4) 0.6070(3) 0.4334(2) 0.0464 0.548(3) Uani D . P 1 2 . . C88 C 0.7095(4) 0.4448(2) 0.5101(2) 0.0450 0.548(3) Uani D . P 1 2 . . C89 C 0.9504(3) 0.4285(2) 0.6096(2) 0.0440 0.548(3) Uani D . P 1 2 . . C90 C 0.7706(5) 0.6986(4) 0.8217(3) 0.0459 0.335(12) Uani D . P 2 1 . . C91 C 0.7634(11) 0.7595(7) 0.8719(5) 0.0582 0.335(12) Uani D . P 2 1 . . C92 C 0.6551(7) 0.6613(6) 0.7938(7) 0.0589 0.335(12) Uani D . P 2 1 . . C95 C 0.7664(3) 0.69773(18) 0.82740(16) 0.0388 0.665(12) Uani D . P 2 2 . . C96 C 0.7149(5) 0.7203(5) 0.8827(2) 0.0599 0.665(12) Uani D . P 2 2 . . C97 C 0.6750(4) 0.6696(4) 0.7708(3) 0.0507 0.665(12) Uani D . P 2 2 . . H51 H 0.5511 0.8319 0.6093 0.0719 1.0000 Uiso R . . . . . . H52 H 0.6821 0.8245 0.6303 0.0721 1.0000 Uiso R . . . . . . H53 H 0.6077 0.7630 0.6565 0.0716 1.0000 Uiso R . . . . . . H62 H 0.4361 0.7321 0.5317 0.0898 1.0000 Uiso R . . . . . . H63 H 0.4900 0.6651 0.5804 0.0899 1.0000 Uiso R . . . . . . H61 H 0.4976 0.6597 0.5101 0.0900 1.0000 Uiso R . . . . . . H71 H 0.5617 0.8299 0.4949 0.0959 1.0000 Uiso R . . . . . . H73 H 0.6927 0.8204 0.5190 0.0966 1.0000 Uiso R . . . . . . H72 H 0.6216 0.7584 0.4698 0.0968 1.0000 Uiso R . . . . . . H91 H 0.8939 0.5135 0.7193 0.0425 1.0000 Uiso R . . . . . . H101 H 0.8393 0.4185 0.7821 0.0545 1.0000 Uiso R . . . . . . H111 H 0.6528 0.3730 0.7543 0.0607 1.0000 Uiso R . . . . . . H121 H 0.5263 0.4322 0.6660 0.0595 1.0000 Uiso R . . . . . . H131 H 0.5885 0.5307 0.6079 0.0461 1.0000 Uiso R . . . . . . H351 H 1.0669 0.7660 0.8529 0.0343 1.0000 Uiso R . . . . . . H361 H 1.1448 0.8402 0.7828 0.0333 1.0000 Uiso R . . . . . . H401 H 1.3520 0.7792 0.6224 0.0539 1.0000 Uiso R . . . . . . H411 H 1.2667 0.8593 0.5368 0.0550 1.0000 Uiso R . . . . . . H421 H 1.0877 0.9091 0.5294 0.0524 1.0000 Uiso R . . . . . . H441 H 0.9089 0.8565 0.6232 0.0483 1.0000 Uiso R . . . . . . H451 H 0.9015 0.9842 0.6609 0.0935 1.0000 Uiso R . . . . . . H452 H 1.0107 1.0079 0.6399 0.0930 1.0000 Uiso R . . . . . . H453 H 1.0179 0.9454 0.6987 0.0934 1.0000 Uiso R . . . . . . H463 H 0.8152 0.9419 0.5448 0.0959 1.0000 Uiso R . . . . . . H461 H 0.9311 0.9665 0.5294 0.0962 1.0000 Uiso R . . . . . . H462 H 0.8815 0.8791 0.5140 0.0962 1.0000 Uiso R . . . . . . H471 H 1.2323 0.7043 0.7422 0.0503 1.0000 Uiso R . . . . . . H481 H 1.4097 0.7414 0.8077 0.0778 1.0000 Uiso R . . . . . . H483 H 1.3362 0.8197 0.7833 0.0778 1.0000 Uiso R . . . . . . H482 H 1.4321 0.7927 0.7500 0.0779 1.0000 Uiso R . . . . . . H492 H 1.3758 0.6172 0.7375 0.0855 1.0000 Uiso R . . . . . . H491 H 1.4051 0.6704 0.6834 0.0848 1.0000 Uiso R . . . . . . H493 H 1.2937 0.6237 0.6695 0.0850 1.0000 Uiso R . . . . . . H521 H 0.7830 0.5753 0.9066 0.0498 1.0000 Uiso R . . . . . . H531 H 0.9213 0.4793 0.9413 0.0489 1.0000 Uiso R . . . . . . H541 H 1.0801 0.4809 0.9008 0.0465 1.0000 Uiso R . . . . . . H561 H 1.1308 0.6152 0.7849 0.0430 1.0000 Uiso R . . . . . . H571 H 1.2222 0.4989 0.7741 0.0690 1.0000 Uiso R . . . . . . H573 H 1.1785 0.4544 0.8264 0.0689 1.0000 Uiso R . . . . . . H572 H 1.0940 0.4781 0.7598 0.0692 1.0000 Uiso R . . . . . . H582 H 1.3097 0.6010 0.8549 0.0758 1.0000 Uiso R . . . . . . H581 H 1.2375 0.6502 0.8910 0.0767 1.0000 Uiso R . . . . . . H583 H 1.2621 0.5577 0.9067 0.0754 1.0000 Uiso R . . . . . . H751 H 0.6320 0.6051 0.4364 0.0744 0.452(3) Uiso R . P 1 1 . . H752 H 0.6131 0.5208 0.4650 0.0738 0.452(3) Uiso R . P 1 1 . . H753 H 0.6667 0.5253 0.4073 0.0740 0.452(3) Uiso R . P 1 1 . . H762 H 0.8293 0.3896 0.5789 0.0829 0.452(3) Uiso R . P 1 1 . . H763 H 0.7074 0.4205 0.5499 0.0833 0.452(3) Uiso R . P 1 1 . . H761 H 0.7759 0.3828 0.5052 0.0831 0.452(3) Uiso R . P 1 1 . . H771 H 1.0744 0.5101 0.6434 0.0728 0.452(3) Uiso R . P 1 1 . . H773 H 0.9913 0.4380 0.6374 0.0735 0.452(3) Uiso R . P 1 1 . . H772 H 1.0712 0.4449 0.5924 0.0730 0.452(3) Uiso R . P 1 1 . . H782 H 1.0483 0.6955 0.5363 0.0838 0.452(3) Uiso R . P 1 1 . . H781 H 1.0857 0.6524 0.6028 0.0841 0.452(3) Uiso R . P 1 1 . . H783 H 1.1172 0.6160 0.5434 0.0841 0.452(3) Uiso R . P 1 1 . . H793 H 0.8569 0.7397 0.4798 0.0811 0.452(3) Uiso R . P 1 1 . . H791 H 0.7586 0.6947 0.4311 0.0810 0.452(3) Uiso R . P 1 1 . . H792 H 0.8814 0.6888 0.4242 0.0807 0.452(3) Uiso R . P 1 1 . . H851 H 1.1024 0.5688 0.6436 0.0690 0.548(3) Uiso R . P 1 2 . . H852 H 1.1089 0.6396 0.5973 0.0688 0.548(3) Uiso R . P 1 2 . . H853 H 1.1373 0.5530 0.5800 0.0688 0.548(3) Uiso R . P 1 2 . . H862 H 0.8712 0.7307 0.4779 0.0849 0.548(3) Uiso R . P 1 2 . . H863 H 0.9849 0.7261 0.5304 0.0850 0.548(3) Uiso R . P 1 2 . . H861 H 0.9740 0.6899 0.4623 0.0852 0.548(3) Uiso R . P 1 2 . . H871 H 0.6355 0.6070 0.4437 0.0745 0.548(3) Uiso R . P 1 2 . . H872 H 0.7246 0.6603 0.4214 0.0741 0.548(3) Uiso R . P 1 2 . . H873 H 0.7053 0.5707 0.3983 0.0742 0.548(3) Uiso R . P 1 2 . . H882 H 0.7158 0.4109 0.5470 0.0795 0.548(3) Uiso R . P 1 2 . . H883 H 0.6377 0.4724 0.4988 0.0790 0.548(3) Uiso R . P 1 2 . . H881 H 0.7148 0.4139 0.4737 0.0791 0.548(3) Uiso R . P 1 2 . . H891 H 0.8894 0.3964 0.6144 0.0739 0.548(3) Uiso R . P 1 2 . . H893 H 0.9932 0.4457 0.6516 0.0744 0.548(3) Uiso R . P 1 2 . . H892 H 0.9976 0.3966 0.5906 0.0743 0.548(3) Uiso R . P 1 2 . . H901 H 0.7903 0.7267 0.7859 0.0580 0.335(12) Uiso R . P 2 1 . . H911 H 0.7088 0.7995 0.8535 0.0849 0.335(12) Uiso R . P 2 1 . . H912 H 0.8349 0.7843 0.8880 0.0848 0.335(12) Uiso R . P 2 1 . . H913 H 0.7425 0.7330 0.9065 0.0853 0.335(12) Uiso R . P 2 1 . . H922 H 0.6003 0.7019 0.7763 0.0829 0.335(12) Uiso R . P 2 1 . . H923 H 0.6337 0.6334 0.8277 0.0830 0.335(12) Uiso R . P 2 1 . . H921 H 0.6589 0.6237 0.7608 0.0831 0.335(12) Uiso R . P 2 1 . . H951 H 0.7973 0.7471 0.8152 0.0505 0.665(12) Uiso R . P 2 2 . . H963 H 0.6567 0.7595 0.8668 0.0888 0.665(12) Uiso R . P 2 2 . . H961 H 0.7726 0.7413 0.9186 0.0891 0.665(12) Uiso R . P 2 2 . . H962 H 0.6817 0.6716 0.8950 0.0889 0.665(12) Uiso R . P 2 2 . . H971 H 0.6148 0.7086 0.7602 0.0778 0.665(12) Uiso R . P 2 2 . . H972 H 0.6472 0.6184 0.7820 0.0781 0.665(12) Uiso R . P 2 2 . . H973 H 0.7063 0.6628 0.7347 0.0779 0.665(12) Uiso R . P 2 2 . . 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 0.02389(14) 0.02171(14) 0.02110(14) -0.00048(11) 0.00207(10) -0.00106(11) Ti2 0.0232(2) 0.0219(2) 0.0211(2) -0.00123(17) 0.00324(17) -0.00173(17) N3 0.0248(10) 0.0269(11) 0.0212(10) -0.0041(8) 0.0051(8) -0.0022(8) C4 0.0288(13) 0.0313(14) 0.0304(13) -0.0011(11) 0.0049(11) 0.0056(11) C5 0.0531(18) 0.0392(17) 0.0434(17) -0.0096(13) 0.0117(14) 0.0140(14) C6 0.0303(15) 0.054(2) 0.092(3) -0.0207(19) 0.0032(16) 0.0066(15) C7 0.085(3) 0.054(2) 0.0436(18) 0.0175(16) 0.0237(17) 0.0317(18) N8 0.0313(11) 0.0260(11) 0.0263(11) -0.0003(9) 0.0054(9) -0.0030(9) C9 0.0408(15) 0.0288(14) 0.0325(14) -0.0014(12) 0.0038(12) -0.0049(12) C10 0.060(2) 0.0370(16) 0.0323(15) 0.0084(13) 0.0021(14) -0.0040(15) C11 0.070(2) 0.0391(17) 0.0430(17) 0.0068(14) 0.0205(16) -0.0124(16) C12 0.0458(17) 0.0489(18) 0.0460(18) 0.0038(15) 0.0102(14) -0.0198(15) C13 0.0371(15) 0.0398(16) 0.0340(15) 0.0026(12) 0.0066(12) -0.0076(13) N34 0.0296(10) 0.0188(10) 0.0221(10) 0.0003(8) 0.0012(8) -0.0009(9) C35 0.0312(13) 0.0250(12) 0.0228(12) -0.0020(10) 0.0020(10) 0.0027(11) C36 0.0300(13) 0.0233(12) 0.0257(13) -0.0071(10) 0.0027(10) -0.0048(10) N37 0.0280(11) 0.0274(11) 0.0226(10) 0.0010(9) 0.0054(8) -0.0025(9) C38 0.0295(13) 0.0244(12) 0.0268(13) -0.0061(10) 0.0060(10) -0.0090(11) C39 0.0329(14) 0.0310(14) 0.0356(15) -0.0055(12) 0.0100(11) -0.0063(12) C40 0.0358(15) 0.0440(17) 0.0495(18) -0.0084(14) 0.0182(13) -0.0083(13) C41 0.0481(18) 0.0475(18) 0.0421(17) -0.0054(14) 0.0210(14) -0.0169(15) C42 0.0509(18) 0.0393(16) 0.0346(15) 0.0031(13) 0.0116(13) -0.0104(14) C43 0.0364(14) 0.0313(14) 0.0299(14) -0.0009(11) 0.0068(11) -0.0084(12) C44 0.0402(16) 0.0362(16) 0.0399(16) 0.0136(13) 0.0079(13) -0.0024(13) C45 0.058(2) 0.057(2) 0.070(2) -0.0099(18) 0.0167(18) 0.0114(18) C46 0.065(2) 0.059(2) 0.057(2) 0.0232(18) 0.0008(17) 0.0077(18) C47 0.0304(14) 0.0412(16) 0.0498(18) 0.0031(14) 0.0077(13) 0.0026(13) C48 0.0384(17) 0.061(2) 0.0536(19) 0.0008(17) 0.0020(14) 0.0038(16) C49 0.0436(18) 0.0472(19) 0.072(2) -0.0023(17) 0.0067(16) 0.0053(15) C50 0.0304(13) 0.0222(12) 0.0187(12) -0.0006(9) 0.0007(10) -0.0011(10) C51 0.0362(14) 0.0258(13) 0.0308(13) -0.0008(11) 0.0038(11) -0.0008(11) C52 0.0459(17) 0.0351(15) 0.0370(15) 0.0004(12) 0.0157(13) -0.0072(13) C53 0.0580(19) 0.0326(15) 0.0314(15) 0.0083(12) 0.0076(13) -0.0074(14) C54 0.0438(16) 0.0301(14) 0.0335(15) 0.0084(12) 0.0012(12) 0.0031(12) C55 0.0357(14) 0.0237(12) 0.0246(13) -0.0005(10) -0.0012(10) 0.0021(11) C56 0.0343(13) 0.0338(14) 0.0360(14) 0.0038(11) 0.0030(11) 0.0087(11) C57 0.0523(17) 0.0461(17) 0.0383(16) -0.0051(14) 0.0061(13) 0.0105(14) C58 0.0367(16) 0.0535(19) 0.0571(19) -0.0112(15) 0.0024(14) 0.0040(14) C70 0.039(2) 0.045(2) 0.0282(19) -0.0101(17) 0.0094(17) 0.0039(17) C71 0.044(2) 0.0361(19) 0.033(2) -0.0076(17) 0.0156(17) -0.0015(17) C72 0.0397(19) 0.042(2) 0.0266(19) -0.0065(17) 0.0089(17) 0.0123(17) C73 0.0377(19) 0.043(2) 0.033(2) -0.0118(17) 0.0165(17) 0.0014(17) C74 0.045(2) 0.040(2) 0.0296(19) -0.0034(17) 0.0180(17) 0.0077(17) C75 0.041(3) 0.060(3) 0.035(3) -0.016(2) 0.002(2) 0.005(2) C76 0.058(3) 0.040(2) 0.048(3) -0.009(2) 0.019(2) -0.007(2) C77 0.049(3) 0.054(3) 0.030(2) -0.005(2) 0.005(2) 0.023(2) C78 0.043(2) 0.056(3) 0.047(3) -0.019(2) 0.021(2) -0.006(2) C79 0.060(3) 0.047(3) 0.038(3) 0.005(2) 0.024(2) 0.011(2) C80 0.0320(16) 0.0401(18) 0.0312(17) -0.0105(15) 0.0111(14) -0.0002(14) C81 0.0439(18) 0.0336(17) 0.0314(17) -0.0057(14) 0.0195(15) -0.0011(15) C82 0.0389(17) 0.0413(18) 0.0241(16) -0.0070(15) 0.0052(15) 0.0087(15) C83 0.0362(17) 0.0344(17) 0.0295(17) -0.0144(15) 0.0114(15) -0.0058(15) C84 0.0399(17) 0.0316(17) 0.0280(16) -0.0064(15) 0.0117(15) 0.0054(14) C85 0.031(2) 0.057(2) 0.039(2) -0.017(2) 0.0082(18) 0.001(2) C86 0.061(3) 0.038(2) 0.047(2) -0.0030(19) 0.029(2) -0.002(2) C87 0.050(2) 0.055(3) 0.028(2) -0.008(2) 0.0004(19) 0.020(2) C88 0.046(2) 0.047(2) 0.043(2) -0.024(2) 0.014(2) -0.0153(19) C89 0.057(2) 0.037(2) 0.037(2) -0.0029(18) 0.011(2) 0.014(2) C90 0.050(4) 0.036(4) 0.054(4) 0.007(4) 0.019(4) 0.008(4) C91 0.074(6) 0.039(5) 0.063(5) 0.000(4) 0.021(5) 0.012(5) C92 0.058(5) 0.054(5) 0.059(6) 0.017(5) 0.006(5) 0.009(5) C95 0.039(2) 0.036(3) 0.046(2) 0.005(2) 0.018(2) 0.004(2) C96 0.067(4) 0.060(4) 0.055(3) -0.011(3) 0.019(3) 0.016(3) C97 0.054(3) 0.059(3) 0.035(3) 0.005(2) 0.007(2) 0.019(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.14752(5) 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 . Ti2 . 2.6853(5) yes Ga1 . N34 . 1.9149(19) yes Ga1 . N37 . 1.911(2) yes Ti2 . N3 . 1.714(2) yes Ti2 . N8 . 2.180(2) yes Ti2 . C70 . 2.378(5) yes Ti2 . C71 . 2.426(6) yes Ti2 . C72 . 2.454(6) yes Ti2 . C73 . 2.441(5) yes Ti2 . C74 . 2.396(5) yes Ti2 . N3 . 1.714(2) yes Ti2 . N8 . 2.180(2) yes Ti2 . C80 . 2.407(4) yes Ti2 . C81 . 2.330(4) yes Ti2 . C82 . 2.325(4) yes Ti2 . C83 . 2.362(5) yes Ti2 . C84 . 2.431(4) yes N3 . C4 . 1.451(3) yes C4 . C5 . 1.524(4) yes C4 . C6 . 1.515(4) yes C4 . C7 . 1.531(4) yes C5 . H51 . 0.969 no C5 . H52 . 0.966 no C5 . H53 . 0.973 no C6 . H62 . 0.955 no C6 . H63 . 0.968 no C6 . H61 . 0.957 no C7 . H71 . 0.974 no C7 . H73 . 0.979 no C7 . H72 . 0.967 no N8 . C9 . 1.344(3) yes N8 . C13 . 1.344(3) yes C9 . C10 . 1.373(4) yes C9 . H91 . 0.957 no C10 . C11 . 1.377(4) yes C10 . H101 . 0.946 no C11 . C12 . 1.377(4) yes C11 . H111 . 0.953 no C12 . C13 . 1.379(4) yes C12 . H121 . 0.937 no C13 . H131 . 0.952 no N34 . C35 . 1.392(3) yes N34 . C50 . 1.433(3) yes C35 . C36 . 1.338(3) yes C35 . H351 . 0.941 no C36 . N37 . 1.399(3) yes C36 . H361 . 0.949 no N37 . C38 . 1.427(3) yes C38 . C39 . 1.409(4) yes C38 . C43 . 1.408(4) yes C39 . C40 . 1.394(4) yes C39 . C47 . 1.522(4) yes C40 . C41 . 1.382(4) yes C40 . H401 . 0.929 no C41 . C42 . 1.380(4) yes C41 . H411 . 0.954 no C42 . C43 . 1.398(4) yes C42 . H421 . 0.953 no C43 . C44 . 1.518(4) yes C44 . C45 . 1.529(4) yes C44 . C46 . 1.522(4) yes C44 . H441 . 0.971 no C45 . H451 . 0.968 no C45 . H452 . 0.980 no C45 . H453 . 0.986 no C46 . H463 . 0.975 no C46 . H461 . 0.964 no C46 . H462 . 0.977 no C47 . C48 . 1.541(4) yes C47 . C49 . 1.526(4) yes C47 . H471 . 0.979 no C48 . H481 . 0.970 no C48 . H483 . 0.982 no C48 . H482 . 0.983 no C49 . H492 . 0.969 no C49 . H491 . 0.966 no C49 . H493 . 0.941 no C50 . C51 . 1.404(3) yes C50 . C55 . 1.418(3) yes C51 . C52 . 1.396(4) yes C51 . C90 . 1.513(6) yes C51 . C52 . 1.396(4) yes C51 . C95 . 1.520(4) yes C52 . C53 . 1.381(4) yes C52 . H521 . 0.947 no C53 . C54 . 1.386(4) yes C53 . H531 . 0.951 no C54 . C55 . 1.388(3) yes C54 . H541 . 0.945 no C55 . C56 . 1.517(3) yes C56 . C57 . 1.540(3) yes C56 . C58 . 1.526(3) yes C56 . H561 . 0.997 no C57 . H571 . 0.951 no C57 . H573 . 0.976 no C57 . H572 . 0.970 no C58 . H582 . 0.965 no C58 . H581 . 0.971 no C58 . H583 . 0.980 no C70 . C71 . 1.408(4) yes C70 . C74 . 1.402(4) yes C70 . C75 . 1.525(4) yes C71 . C72 . 1.405(4) yes C71 . C76 . 1.520(5) yes C72 . C73 . 1.405(4) yes C72 . C77 . 1.520(4) yes C73 . C74 . 1.408(4) yes C73 . C78 . 1.514(5) yes C74 . C79 . 1.524(4) yes C75 . H751 . 0.968 no C75 . H752 . 0.958 no C75 . H753 . 0.962 no C76 . H762 . 0.957 no C76 . H763 . 0.964 no C76 . H761 . 0.961 no C77 . H771 . 0.956 no C77 . H773 . 0.965 no C77 . H772 . 0.958 no C78 . H782 . 0.958 no C78 . H781 . 0.954 no C78 . H783 . 0.958 no C79 . H793 . 0.958 no C79 . H791 . 0.959 no C79 . H792 . 0.960 no C80 . C81 . 1.407(3) yes C80 . C84 . 1.402(3) yes C80 . C85 . 1.520(4) yes C81 . C82 . 1.412(3) yes C81 . C86 . 1.521(4) yes C82 . C83 . 1.401(3) yes C82 . C87 . 1.518(4) yes C83 . C84 . 1.413(3) yes C83 . C88 . 1.523(4) yes C84 . C89 . 1.519(4) yes C85 . H851 . 0.965 no C85 . H852 . 0.952 no C85 . H853 . 0.965 no C86 . H862 . 0.947 no C86 . H863 . 0.951 no C86 . H861 . 0.965 no C87 . H871 . 0.971 no C87 . H872 . 0.970 no C87 . H873 . 0.969 no C88 . H882 . 0.966 no C88 . H883 . 0.974 no C88 . H881 . 0.961 no C89 . H891 . 0.955 no C89 . H893 . 0.968 no C89 . H892 . 0.962 no C90 . C91 . 1.513(6) yes C90 . C92 . 1.532(6) yes C90 . H901 . 0.990 no C91 . H911 . 0.962 no C91 . H912 . 0.957 no C91 . H913 . 0.961 no C92 . H922 . 0.965 no C92 . H923 . 0.963 no C92 . H921 . 0.964 no C95 . C96 . 1.544(5) yes C95 . C97 . 1.508(5) yes C95 . H951 . 0.976 no C96 . H963 . 0.969 no C96 . H961 . 0.973 no C96 . H962 . 0.981 no C97 . H971 . 0.973 no C97 . H972 . 0.980 no C97 . H973 . 0.964 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 Ti2 . Ga1 . N34 . 133.34(6) yes Ti2 . Ga1 . N37 . 140.71(6) yes N34 . Ga1 . N37 . 85.48(8) yes Ga1 . Ti2 . N3 . 97.43(6) yes Ga1 . Ti2 . N8 . 97.34(5) yes N3 . Ti2 . N8 . 101.07(9) yes Ga1 . Ti2 . C70 . 145.55(10) yes N3 . Ti2 . C70 . 99.67(11) yes N8 . Ti2 . C70 . 108.34(10) yes Ga1 . Ti2 . C71 . 132.15(8) yes N3 . Ti2 . C71 . 129.28(10) yes N8 . Ti2 . C71 . 84.66(12) yes C70 . Ti2 . C71 . 34.06(11) yes Ga1 . Ti2 . C72 . 99.45(9) yes N3 . Ti2 . C72 . 154.09(12) yes N8 . Ti2 . C72 . 96.12(11) yes C70 . Ti2 . C72 . 56.16(13) yes C71 . Ti2 . C72 . 33.46(11) yes Ga1 . Ti2 . C73 . 89.74(9) yes N3 . Ti2 . C73 . 127.88(11) yes N8 . Ti2 . C73 . 129.20(10) yes C70 . Ti2 . C73 . 56.28(12) yes C71 . Ti2 . C73 . 55.68(12) yes Ga1 . Ti2 . C74 . 113.48(9) yes N3 . Ti2 . C74 . 99.16(11) yes N8 . Ti2 . C74 . 140.29(11) yes C70 . Ti2 . C74 . 34.15(10) yes C71 . Ti2 . C74 . 56.25(12) yes C72 . Ti2 . C73 . 33.36(10) yes C72 . Ti2 . C74 . 55.95(12) yes C73 . Ti2 . C74 . 33.83(10) yes Ga1 . Ti2 . N3 . 97.43(6) yes Ga1 . Ti2 . N8 . 97.34(5) yes N3 . Ti2 . N8 . 101.07(9) yes Ga1 . Ti2 . C80 . 86.41(8) yes N3 . Ti2 . C80 . 143.60(10) yes N8 . Ti2 . C80 . 114.38(9) yes Ga1 . Ti2 . C81 . 100.22(8) yes N3 . Ti2 . C81 . 109.91(10) yes N8 . Ti2 . C81 . 141.76(10) yes C80 . Ti2 . C81 . 34.50(9) yes Ga1 . Ti2 . C82 . 135.51(8) yes N3 . Ti2 . C82 . 98.17(10) yes N8 . Ti2 . C82 . 119.92(9) yes C80 . Ti2 . C82 . 57.60(10) yes C81 . Ti2 . C82 . 35.33(10) yes Ga1 . Ti2 . C83 . 141.14(8) yes N3 . Ti2 . C83 . 119.51(10) yes N8 . Ti2 . C83 . 87.59(10) yes C80 . Ti2 . C83 . 57.06(11) yes C81 . Ti2 . C83 . 57.98(11) yes Ga1 . Ti2 . C84 . 107.45(7) yes N3 . Ti2 . C84 . 153.33(10) yes N8 . Ti2 . C84 . 85.43(10) yes C80 . Ti2 . C84 . 33.68(9) yes C81 . Ti2 . C84 . 56.96(11) yes C82 . Ti2 . C83 . 34.76(10) yes C82 . Ti2 . C84 . 57.14(11) yes C83 . Ti2 . C84 . 34.26(9) yes Ti2 . N3 . C4 . 175.46(17) yes N3 . C4 . C5 . 108.8(2) yes N3 . C4 . C6 . 109.2(2) yes C5 . C4 . C6 . 110.0(2) yes N3 . C4 . C7 . 111.0(2) yes C5 . C4 . C7 . 108.2(2) yes C6 . C4 . C7 . 109.6(3) yes C4 . C5 . H51 . 110.4 no C4 . C5 . H52 . 110.2 no H51 . C5 . H52 . 108.4 no C4 . C5 . H53 . 109.6 no H51 . C5 . H53 . 108.7 no H52 . C5 . H53 . 109.4 no C4 . C6 . H62 . 112.0 no C4 . C6 . H63 . 108.7 no H62 . C6 . H63 . 108.9 no C4 . C6 . H61 . 109.5 no H62 . C6 . H61 . 110.2 no H63 . C6 . H61 . 107.5 no C4 . C7 . H71 . 110.7 no C4 . C7 . H73 . 109.9 no H71 . C7 . H73 . 107.6 no C4 . C7 . H72 . 111.1 no H71 . C7 . H72 . 108.9 no H73 . C7 . H72 . 108.6 no Ti2 . N8 . C9 . 121.07(17) yes Ti2 . N8 . C13 . 121.78(17) yes C9 . N8 . C13 . 117.1(2) yes N8 . C9 . C10 . 123.3(3) yes N8 . C9 . H91 . 117.6 no C10 . C9 . H91 . 119.1 no C9 . C10 . C11 . 118.9(3) yes C9 . C10 . H101 . 119.7 no C11 . C10 . H101 . 121.4 no C10 . C11 . C12 . 118.8(3) yes C10 . C11 . H111 . 120.5 no C12 . C11 . H111 . 120.6 no C11 . C12 . C13 . 119.1(3) yes C11 . C12 . H121 . 121.2 no C13 . C12 . H121 . 119.7 no C12 . C13 . N8 . 122.8(3) yes C12 . C13 . H131 . 120.5 no N8 . C13 . H131 . 116.7 no Ga1 . N34 . C35 . 110.10(16) yes Ga1 . N34 . C50 . 129.48(15) yes C35 . N34 . C50 . 115.94(18) yes N34 . C35 . C36 . 117.7(2) yes N34 . C35 . H351 . 119.9 no C36 . C35 . H351 . 122.4 no C35 . C36 . N37 . 116.0(2) yes C35 . C36 . H361 . 122.9 no N37 . C36 . H361 . 121.2 no C36 . N37 . Ga1 . 110.79(15) yes C36 . N37 . C38 . 119.21(19) yes Ga1 . N37 . C38 . 127.72(15) yes N37 . C38 . C39 . 120.7(2) yes N37 . C38 . C43 . 119.1(2) yes C39 . C38 . C43 . 120.1(2) yes C38 . C39 . C40 . 119.0(2) yes C38 . C39 . C47 . 122.4(2) yes C40 . C39 . C47 . 118.6(2) yes C39 . C40 . C41 . 121.3(3) yes C39 . C40 . H401 . 119.8 no C41 . C40 . H401 . 118.9 no C40 . C41 . C42 . 119.4(3) yes C40 . C41 . H411 . 119.9 no C42 . C41 . H411 . 120.7 no C41 . C42 . C43 . 121.6(3) yes C41 . C42 . H421 . 119.4 no C43 . C42 . H421 . 119.0 no C38 . C43 . C42 . 118.6(3) yes C38 . C43 . C44 . 120.1(2) yes C42 . C43 . C44 . 121.2(2) yes C43 . C44 . C45 . 109.7(2) yes C43 . C44 . C46 . 114.0(3) yes C45 . C44 . C46 . 110.1(3) yes C43 . C44 . H441 . 107.8 no C45 . C44 . H441 . 107.5 no C46 . C44 . H441 . 107.5 no C44 . C45 . H451 . 109.6 no C44 . C45 . H452 . 107.7 no H451 . C45 . H452 . 109.1 no C44 . C45 . H453 . 108.4 no H451 . C45 . H453 . 109.6 no H452 . C45 . H453 . 112.4 no C44 . C46 . H463 . 109.2 no C44 . C46 . H461 . 108.9 no H463 . C46 . H461 . 112.3 no C44 . C46 . H462 . 107.3 no H463 . C46 . H462 . 108.9 no H461 . C46 . H462 . 110.2 no C39 . C47 . C48 . 110.1(2) yes C39 . C47 . C49 . 114.3(3) yes C48 . C47 . C49 . 109.5(2) yes C39 . C47 . H471 . 106.7 no C48 . C47 . H471 . 108.6 no C49 . C47 . H471 . 107.4 no C47 . C48 . H481 . 110.0 no C47 . C48 . H483 . 108.1 no H481 . C48 . H483 . 110.7 no C47 . C48 . H482 . 108.2 no H481 . C48 . H482 . 110.0 no H483 . C48 . H482 . 109.8 no C47 . C49 . H492 . 110.8 no C47 . C49 . H491 . 109.0 no H492 . C49 . H491 . 110.3 no C47 . C49 . H493 . 109.2 no H492 . C49 . H493 . 109.2 no H491 . C49 . H493 . 108.3 no N34 . C50 . C51 . 120.2(2) yes N34 . C50 . C55 . 119.5(2) yes C51 . C50 . C55 . 120.3(2) yes C50 . C51 . C52 . 118.8(2) yes C50 . C51 . C90 . 117.3(3) yes C52 . C51 . C90 . 123.9(3) yes C50 . C51 . C52 . 118.8(2) yes C50 . C51 . C95 . 122.4(2) yes C52 . C51 . C95 . 118.8(2) yes C51 . C52 . C53 . 121.4(3) yes C51 . C52 . H521 . 119.7 no C53 . C52 . H521 . 118.9 no C52 . C53 . C54 . 119.4(3) yes C52 . C53 . H531 . 120.9 no C54 . C53 . H531 . 119.7 no C53 . C54 . C55 . 121.6(2) yes C53 . C54 . H541 . 121.7 no C55 . C54 . H541 . 116.7 no C50 . C55 . C54 . 118.6(2) yes C50 . C55 . C56 . 121.25(19) yes C54 . C55 . C56 . 120.2(2) yes C55 . C56 . C57 . 111.90(7) yes C55 . C56 . C58 . 111.76(7) yes C57 . C56 . C58 . 109.39(7) yes C55 . C56 . H561 . 107.4 no C57 . C56 . H561 . 106.8 no C58 . C56 . H561 . 109.4 no C56 . C57 . H571 . 108.0 no C56 . C57 . H573 . 109.7 no H571 . C57 . H573 . 108.7 no C56 . C57 . H572 . 110.4 no H571 . C57 . H572 . 110.1 no H573 . C57 . H572 . 109.7 no C56 . C58 . H582 . 109.0 no C56 . C58 . H581 . 110.9 no H582 . C58 . H581 . 108.2 no C56 . C58 . H583 . 110.1 no H582 . C58 . H583 . 108.2 no H581 . C58 . H583 . 110.3 no Ti2 . C70 . C71 . 74.8(3) yes Ti2 . C70 . C74 . 73.6(2) yes C71 . C70 . C74 . 108.01(5) yes Ti2 . C70 . C75 . 122.3(3) yes C71 . C70 . C75 . 125.86(5) yes C74 . C70 . C75 . 125.84(5) yes Ti2 . C71 . C70 . 71.1(3) yes Ti2 . C71 . C72 . 74.3(3) yes C70 . C71 . C72 . 107.99(5) yes Ti2 . C71 . C76 . 124.6(4) yes C70 . C71 . C76 . 125.89(5) yes C72 . C71 . C76 . 125.89(5) yes Ti2 . C72 . C71 . 72.2(3) yes Ti2 . C72 . C73 . 72.8(3) yes C71 . C72 . C73 . 107.99(5) yes Ti2 . C72 . C77 . 124.0(4) yes C71 . C72 . C77 . 125.95(5) yes C73 . C72 . C77 . 125.93(5) yes Ti2 . C73 . C72 . 73.8(3) yes Ti2 . C73 . C74 . 71.3(2) yes C72 . C73 . C74 . 107.99(5) yes Ti2 . C73 . C78 . 124.6(3) yes C72 . C73 . C78 . 125.89(5) yes C74 . C73 . C78 . 125.91(5) yes Ti2 . C74 . C73 . 74.8(2) yes Ti2 . C74 . C70 . 72.2(2) yes C73 . C74 . C70 . 108.01(5) yes Ti2 . C74 . C79 . 123.3(3) yes C73 . C74 . C79 . 125.86(5) yes C70 . C74 . C79 . 125.88(5) yes C70 . C75 . H751 . 108.4 no C70 . C75 . H752 . 108.8 no H751 . C75 . H752 . 110.7 no C70 . C75 . H753 . 109.5 no H751 . C75 . H753 . 110.5 no H752 . C75 . H753 . 108.9 no C71 . C76 . H762 . 107.5 no C71 . C76 . H763 . 110.0 no H762 . C76 . H763 . 109.0 no C71 . C76 . H761 . 111.1 no H762 . C76 . H761 . 109.1 no H763 . C76 . H761 . 110.1 no C72 . C77 . H771 . 109.5 no C72 . C77 . H773 . 110.6 no H771 . C77 . H773 . 109.6 no C72 . C77 . H772 . 110.5 no H771 . C77 . H772 . 107.8 no H773 . C77 . H772 . 108.8 no C73 . C78 . H782 . 108.9 no C73 . C78 . H781 . 108.5 no H782 . C78 . H781 . 110.3 no C73 . C78 . H783 . 109.5 no H782 . C78 . H783 . 110.0 no H781 . C78 . H783 . 109.7 no C74 . C79 . H793 . 109.8 no C74 . C79 . H791 . 107.4 no H793 . C79 . H791 . 110.8 no C74 . C79 . H792 . 109.4 no H793 . C79 . H792 . 109.7 no H791 . C79 . H792 . 109.7 no Ti2 . C80 . C81 . 69.7(2) yes Ti2 . C80 . C84 . 74.1(2) yes C81 . C80 . C84 . 107.99(5) yes Ti2 . C80 . C85 . 127.4(3) yes C81 . C80 . C85 . 125.83(5) yes C84 . C80 . C85 . 125.79(5) yes Ti2 . C81 . C80 . 75.8(2) yes Ti2 . C81 . C82 . 72.1(2) yes C80 . C81 . C82 . 108.01(5) yes Ti2 . C81 . C86 . 120.9(3) yes C80 . C81 . C86 . 125.94(5) yes C82 . C81 . C86 . 125.95(5) yes Ti2 . C82 . C81 . 72.5(2) yes Ti2 . C82 . C83 . 74.1(2) yes C81 . C82 . C83 . 107.90(5) yes Ti2 . C82 . C87 . 124.5(3) yes C81 . C82 . C87 . 125.90(5) yes C83 . C82 . C87 . 125.84(5) yes Ti2 . C83 . C82 . 71.2(2) yes Ti2 . C83 . C84 . 75.5(2) yes C82 . C83 . C84 . 108.01(5) yes Ti2 . C83 . C88 . 122.5(3) yes C82 . C83 . C88 . 125.92(5) yes C84 . C83 . C88 . 125.93(5) yes Ti2 . C84 . C83 . 70.2(2) yes Ti2 . C84 . C80 . 72.22(19) yes C83 . C84 . C80 . 108.05(5) yes Ti2 . C84 . C89 . 127.1(3) yes C83 . C84 . C89 . 125.89(5) yes C80 . C84 . C89 . 125.87(5) yes C80 . C85 . H851 . 108.8 no C80 . C85 . H852 . 110.6 no H851 . C85 . H852 . 110.0 no C80 . C85 . H853 . 109.3 no H851 . C85 . H853 . 108.9 no H852 . C85 . H853 . 109.2 no C81 . C86 . H862 . 109.2 no C81 . C86 . H863 . 109.4 no H862 . C86 . H863 . 110.6 no C81 . C86 . H861 . 108.6 no H862 . C86 . H861 . 109.2 no H863 . C86 . H861 . 109.8 no C82 . C87 . H871 . 109.7 no C82 . C87 . H872 . 108.9 no H871 . C87 . H872 . 110.1 no C82 . C87 . H873 . 108.7 no H871 . C87 . H873 . 110.1 no H872 . C87 . H873 . 109.3 no C83 . C88 . H882 . 110.8 no C83 . C88 . H883 . 107.7 no H882 . C88 . H883 . 111.0 no C83 . C88 . H881 . 109.1 no H882 . C88 . H881 . 110.5 no H883 . C88 . H881 . 107.7 no C84 . C89 . H891 . 110.3 no C84 . C89 . H893 . 109.4 no H891 . C89 . H893 . 108.7 no C84 . C89 . H892 . 110.9 no H891 . C89 . H892 . 108.6 no H893 . C89 . H892 . 108.9 no C51 . C90 . C91 . 111.82(7) yes C51 . C90 . C92 . 111.83(7) yes C91 . C90 . C92 . 109.41(7) yes C51 . C90 . H901 . 108.9 no C91 . C90 . H901 . 108.2 no C92 . C90 . H901 . 106.5 no C90 . C91 . H911 . 110.0 no C90 . C91 . H912 . 109.3 no H911 . C91 . H912 . 109.2 no C90 . C91 . H913 . 109.0 no H911 . C91 . H913 . 110.0 no H912 . C91 . H913 . 109.4 no C90 . C92 . H922 . 110.7 no C90 . C92 . H923 . 108.3 no H922 . C92 . H923 . 109.7 no C90 . C92 . H921 . 109.6 no H922 . C92 . H921 . 109.7 no H923 . C92 . H921 . 108.9 no C51 . C95 . C96 . 111.90(7) yes C51 . C95 . C97 . 111.73(7) yes C96 . C95 . C97 . 109.39(7) yes C51 . C95 . H951 . 109.8 no C96 . C95 . H951 . 105.8 no C97 . C95 . H951 . 108.0 no C95 . C96 . H963 . 108.1 no C95 . C96 . H961 . 110.0 no H963 . C96 . H961 . 111.0 no C95 . C96 . H962 . 107.1 no H963 . C96 . H962 . 109.7 no H961 . C96 . H962 . 110.9 no C95 . C97 . H971 . 110.3 no C95 . C97 . H972 . 108.1 no H971 . C97 . H972 . 110.4 no C95 . C97 . H973 . 108.6 no H971 . C97 . H973 . 109.6 no H972 . C97 . H973 . 109.8 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C47 . H471 . C36 . 120 0.98 2.53 3.137(5) yes C77 . H772 . C74 2_766 162 0.96 2.58 3.506(5) yes C78 . H783 . C76 2_766 150 0.96 2.56 3.430(5) yes # Attachment '- 124apdv09_new.cif' data_124apdv09 _database_code_depnum_ccdc_archive 'CCDC 784596' #TrackingRef '- 124apdv09_new.cif' _audit_creation_date 10-07-08 _audit_creation_method CRYSTALS_ver_14.03 _oxford_structure_analysis_title 124apdv09 _chemical_name_systematic . _chemical_melting_point 'not measured' _refine_special_details ; The difference map indicated the presence of diffuse electron density believed to be disordered solvent. SQUEEZE was used leaving a void from which the electron density was removed. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 -0.081 0.250 400 32 ' ' 2 0.500 0.081 0.750 400 32 ' ' 3 0.000 0.419 0.250 400 32 ' ' 4 0.000 0.581 0.750 400 32 ' ' _platon_squeeze_details ; The discrete Fourier transform of the void region were treated as contributions to the A and B parts of the calculated structure factors. ; _cell_length_a 40.1529(3) _cell_length_b 10.87630(10) _cell_length_c 25.0464(2) _cell_angle_alpha 90 _cell_angle_beta 106.8532(4) _cell_angle_gamma 90 _cell_volume 10468.35(15) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -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' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C45 H60 B1 N4 Ti1 # Dc = 0.91 Fooo = 3456.00 Mu = 1.91 M = 715.71 # Found Formula = C50 H70 B1 N5 Ti1 # Dc = 1.01 FOOO = 3456.00 Mu = 1.97 M = 799.85 _chemical_formula_sum 'C50 H70 B1 N5 Ti1' _chemical_formula_moiety 'C50 H70 B1 N5 Ti1' _chemical_compound_source ? _chemical_formula_weight 799.85 _cell_measurement_reflns_used 12410 _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 0.160 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.015 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 0.197 # Sheldrick geometric approximatio 0.97 0.97 _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 0.97 # 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 '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 11929 _reflns_number_total 11929 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections without Friedels Law is 23651 # Number of reflections with Friedels Law is 11929 # Theoretical number of reflections is about 12108 _diffrn_reflns_theta_min 5.103 _diffrn_reflns_theta_max 27.569 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.018 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -52 _reflns_limit_h_max 49 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _oxford_diffrn_Wilson_B_factor 2.40 _oxford_diffrn_Wilson_scale 40.83 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.58 _refine_diff_density_max 0.55 # 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 11929 _refine_ls_number_restraints 162 _refine_ls_number_parameters 542 _oxford_refine_ls_R_factor_ref 0.0773 _refine_ls_wR_factor_ref 0.1627 _refine_ls_goodness_of_fit_ref 0.9480 _refine_ls_shift/su_max 0.0086733 _refine_ls_shift/su_mean 0.0011106 # The values computed from all data _oxford_reflns_number_all 11929 _refine_ls_R_factor_all 0.0773 _refine_ls_wR_factor_all 0.1627 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8768 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_gt 0.1505 # 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^) + ( 0.09P)^2^ +15.46P] ,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 (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 B1 B 0.59848(5) 0.6069(2) 0.67725(9) 0.0239 1.0000 Uani . . . . . . . Ti2 Ti 0.680518(9) 0.48130(3) 0.599220(14) 0.0239 1.0000 Uani . . . . . . . N3 N 0.64369(4) 0.48223(15) 0.64053(7) 0.0254 1.0000 Uani . . . . . . . C4 C 0.63545(5) 0.37165(19) 0.66042(8) 0.0289 1.0000 Uani . . . . . . . C5 C 0.60277(6) 0.3235(2) 0.64487(9) 0.0362 1.0000 Uani . . . . . . . C6 C 0.57749(6) 0.3814(2) 0.59896(10) 0.0406 1.0000 Uani . . . . . . . C7 C 0.58301(5) 0.4966(2) 0.58518(9) 0.0360 1.0000 Uani . . . . . . . C8 C 0.61278(5) 0.56515(19) 0.62634(8) 0.0265 1.0000 Uani . . . . . . . N9 N 0.60996(4) 0.59057(15) 0.73713(7) 0.0249 1.0000 Uani . . . . . . . C10 C 0.64291(5) 0.55910(19) 0.77647(8) 0.0259 1.0000 Uani . . . . . . . C11 C 0.64758(5) 0.4446(2) 0.80335(8) 0.0291 1.0000 Uani . . . . . . . C12 C 0.67909(6) 0.4230(2) 0.84417(9) 0.0355 1.0000 Uani . . . . . . . C13 C 0.70488(6) 0.5122(2) 0.85830(9) 0.0381 1.0000 Uani . . . . . . . C14 C 0.69959(5) 0.6252(2) 0.83220(9) 0.0349 1.0000 Uani . . . . . . . C15 C 0.66842(5) 0.6517(2) 0.79127(8) 0.0300 1.0000 Uani . . . . . . . C16 C 0.66271(5) 0.7786(2) 0.76493(9) 0.0350 1.0000 Uani . . . . . . . C17 C 0.66698(7) 0.8799(2) 0.80883(12) 0.0514 1.0000 Uani . . . . . . . C18 C 0.68709(8) 0.8004(3) 0.72883(12) 0.0551 1.0000 Uani . . . . . . . C19 C 0.61878(6) 0.3492(2) 0.79190(9) 0.0336 1.0000 Uani . . . . . . . C20 C 0.63173(7) 0.2180(2) 0.78811(10) 0.0437 1.0000 Uani . . . . . . . C21 C 0.59999(7) 0.3565(3) 0.83748(11) 0.0497 1.0000 Uani . . . . . . . C22 C 0.58533(5) 0.6461(2) 0.75960(8) 0.0299 1.0000 Uani . . . . . . . C23 C 0.55961(5) 0.6947(2) 0.71856(8) 0.0313 1.0000 Uani . . . . . . . N24 N 0.56638(4) 0.67501(16) 0.66765(7) 0.0270 1.0000 Uani . . . . . . . C25 C 0.54246(5) 0.7201(2) 0.61675(8) 0.0305 1.0000 Uani . . . . . . . C26 C 0.55137(6) 0.8259(2) 0.59140(9) 0.0340 1.0000 Uani . . . . . . . C27 C 0.58480(6) 0.8967(2) 0.61806(9) 0.0365 1.0000 Uani . . . . . . . C28 C 0.58298(8) 0.9668(2) 0.67005(11) 0.0499 1.0000 Uani . . . . . . . C29 C 0.59446(7) 0.9875(2) 0.57803(12) 0.0487 1.0000 Uani . . . . . . . C30 C 0.52790(7) 0.8657(2) 0.54167(10) 0.0464 1.0000 Uani . . . . . . . C31 C 0.49649(7) 0.8063(3) 0.51918(11) 0.0554 1.0000 Uani . . . . . . . C32 C 0.48788(6) 0.7055(3) 0.54541(11) 0.0505 1.0000 Uani . . . . . . . C33 C 0.51068(5) 0.6587(2) 0.59443(10) 0.0389 1.0000 Uani . . . . . . . C34 C 0.50065(6) 0.5454(3) 0.62181(11) 0.0491 1.0000 Uani . . . . . . . C35 C 0.48405(7) 0.4456(3) 0.57991(13) 0.0633 1.0000 Uani . . . . . . . C36 C 0.47593(8) 0.5793(4) 0.65619(15) 0.0747 1.0000 Uani . . . . . . . N37 N 0.65215(4) 0.38170(17) 0.52356(7) 0.0292 1.0000 Uani . . . . . . . C38 C 0.65644(6) 0.4121(2) 0.47369(8) 0.0345 1.0000 Uani . . . . . . . C39 C 0.64017(6) 0.3499(2) 0.42514(9) 0.0432 1.0000 Uani . . . . . . . C40 C 0.61819(7) 0.2542(3) 0.42693(10) 0.0497 1.0000 Uani . . . . . . . C41 C 0.61333(7) 0.2224(3) 0.47763(10) 0.0454 1.0000 Uani . . . . . . . C42 C 0.63073(6) 0.2876(2) 0.52465(9) 0.0348 1.0000 Uani . . . . . . . N43 N 0.67727(5) 0.62401(17) 0.56876(7) 0.0315 1.0000 Uani . . . . . . . C44 C 0.67503(6) 0.74229(16) 0.54112(8) 0.0480 1.0000 Uani D . . . . . . C45 C 0.72301(5) 0.3179(2) 0.59551(8) 0.0297 1.0000 Uani . . . . . . . C46 C 0.71393(5) 0.2945(2) 0.64550(8) 0.0298 1.0000 Uani . . . . . . . C47 C 0.72385(5) 0.3985(2) 0.68061(8) 0.0308 1.0000 Uani . . . . . . . C48 C 0.73925(5) 0.4859(2) 0.65245(9) 0.0328 1.0000 Uani . . . . . . . C49 C 0.73902(5) 0.4346(2) 0.60001(9) 0.0316 1.0000 Uani . . . . . . . C50 C 0.75619(6) 0.4876(3) 0.55912(11) 0.0466 1.0000 Uani . . . . . . . C51 C 0.75629(6) 0.6042(2) 0.67688(12) 0.0481 1.0000 Uani . . . . . . . C52 C 0.72099(6) 0.4139(3) 0.73877(9) 0.0408 1.0000 Uani . . . . . . . C53 C 0.70052(6) 0.1731(2) 0.65913(11) 0.0423 1.0000 Uani . . . . . . . C54 C 0.72003(6) 0.2264(2) 0.54914(9) 0.0402 1.0000 Uani . . . . . . . C55 C 0.68164(7) 0.8462(3) 0.58389(12) 0.0527 0.870(4) Uani D . P 2 1 . . C56 C 0.63737(8) 0.7534(3) 0.50157(11) 0.0590 0.870(4) Uani D . P 2 1 . . C57 C 0.70067(9) 0.7524(3) 0.50711(13) 0.0712 0.870(4) Uani D . P 2 1 . . C58 C 0.7093(3) 0.8014(14) 0.5770(6) 0.0538 0.130(4) Uani D . P 2 2 . . C59 C 0.6446(3) 0.8255(13) 0.5415(6) 0.0526 0.130(4) Uani D . P 2 2 . . C60 C 0.6766(4) 0.7278(15) 0.4809(3) 0.0530 0.130(4) Uani D . P 2 2 . . H41 H 0.6544 0.3268 0.6854 0.0330 1.0000 Uiso R . . . . . . H51 H 0.5970 0.2531 0.6630 0.0408 1.0000 Uiso R . . . . . . H61 H 0.5575 0.3387 0.5779 0.0455 1.0000 Uiso R . . . . . . H71 H 0.5696 0.5346 0.5522 0.0409 1.0000 Uiso R . . . . . . H81 H 0.6180 0.6400 0.6072 0.0282 1.0000 Uiso R . . . . . . H121 H 0.6829 0.3464 0.8622 0.0404 1.0000 Uiso R . . . . . . H131 H 0.7258 0.4967 0.8857 0.0446 1.0000 Uiso R . . . . . . H141 H 0.7170 0.6854 0.8414 0.0382 1.0000 Uiso R . . . . . . H161 H 0.6389 0.7851 0.7399 0.0413 1.0000 Uiso R . . . . . . H172 H 0.6636 0.9588 0.7900 0.0738 1.0000 Uiso R . . . . . . H171 H 0.6902 0.8750 0.8340 0.0746 1.0000 Uiso R . . . . . . H173 H 0.6495 0.8693 0.8280 0.0746 1.0000 Uiso R . . . . . . H181 H 0.6824 0.8806 0.7123 0.0819 1.0000 Uiso R . . . . . . H183 H 0.7107 0.7978 0.7518 0.0818 1.0000 Uiso R . . . . . . H182 H 0.6829 0.7384 0.6996 0.0820 1.0000 Uiso R . . . . . . H191 H 0.6012 0.3695 0.7556 0.0380 1.0000 Uiso R . . . . . . H201 H 0.6113 0.1655 0.7744 0.0615 1.0000 Uiso R . . . . . . H202 H 0.6448 0.1884 0.8251 0.0621 1.0000 Uiso R . . . . . . H203 H 0.6462 0.2145 0.7635 0.0624 1.0000 Uiso R . . . . . . H212 H 0.5795 0.3045 0.8287 0.0748 1.0000 Uiso R . . . . . . H213 H 0.6161 0.3265 0.8723 0.0748 1.0000 Uiso R . . . . . . H211 H 0.5932 0.4397 0.8419 0.0750 1.0000 Uiso R . . . . . . H221 H 0.5881 0.6473 0.7985 0.0327 1.0000 Uiso R . . . . . . H231 H 0.5399 0.7365 0.7231 0.0358 1.0000 Uiso R . . . . . . H271 H 0.6044 0.8371 0.6293 0.0406 1.0000 Uiso R . . . . . . H282 H 0.6039 1.0120 0.6861 0.0697 1.0000 Uiso R . . . . . . H283 H 0.5790 0.9115 0.6976 0.0698 1.0000 Uiso R . . . . . . H281 H 0.5642 1.0240 0.6597 0.0696 1.0000 Uiso R . . . . . . H291 H 0.6170 1.0199 0.5956 0.0717 1.0000 Uiso R . . . . . . H293 H 0.5946 0.9480 0.5435 0.0722 1.0000 Uiso R . . . . . . H292 H 0.5781 1.0551 0.5693 0.0715 1.0000 Uiso R . . . . . . H301 H 0.5338 0.9346 0.5235 0.0543 1.0000 Uiso R . . . . . . H311 H 0.4809 0.8363 0.4863 0.0656 1.0000 Uiso R . . . . . . H321 H 0.4658 0.6660 0.5289 0.0572 1.0000 Uiso R . . . . . . H341 H 0.5222 0.5118 0.6478 0.0543 1.0000 Uiso R . . . . . . H353 H 0.4820 0.3706 0.5994 0.0916 1.0000 Uiso R . . . . . . H351 H 0.4982 0.4299 0.5553 0.0915 1.0000 Uiso R . . . . . . H352 H 0.4607 0.4699 0.5588 0.0919 1.0000 Uiso R . . . . . . H361 H 0.4682 0.5058 0.6712 0.1032 1.0000 Uiso R . . . . . . H362 H 0.4875 0.6336 0.6863 0.1029 1.0000 Uiso R . . . . . . H363 H 0.4558 0.6198 0.6326 0.1027 1.0000 Uiso R . . . . . . H381 H 0.6714 0.4798 0.4731 0.0391 1.0000 Uiso R . . . . . . H391 H 0.6436 0.3707 0.3908 0.0484 1.0000 Uiso R . . . . . . H401 H 0.6069 0.2121 0.3942 0.0548 1.0000 Uiso R . . . . . . H411 H 0.5987 0.1573 0.4803 0.0530 1.0000 Uiso R . . . . . . H421 H 0.6275 0.2660 0.5590 0.0389 1.0000 Uiso R . . . . . . H501 H 0.7589 0.5735 0.5647 0.0673 1.0000 Uiso R . . . . . . H503 H 0.7791 0.4504 0.5648 0.0667 1.0000 Uiso R . . . . . . H502 H 0.7417 0.4745 0.5217 0.0672 1.0000 Uiso R . . . . . . H512 H 0.7527 0.6651 0.6476 0.0706 1.0000 Uiso R . . . . . . H511 H 0.7807 0.5895 0.6946 0.0705 1.0000 Uiso R . . . . . . H513 H 0.7452 0.6338 0.7039 0.0702 1.0000 Uiso R . . . . . . H523 H 0.7396 0.4660 0.7598 0.0592 1.0000 Uiso R . . . . . . H521 H 0.7235 0.3361 0.7571 0.0595 1.0000 Uiso R . . . . . . H522 H 0.6991 0.4500 0.7386 0.0589 1.0000 Uiso R . . . . . . H531 H 0.6968 0.1771 0.6958 0.0596 1.0000 Uiso R . . . . . . H532 H 0.7176 0.1096 0.6597 0.0602 1.0000 Uiso R . . . . . . H533 H 0.6789 0.1512 0.6320 0.0602 1.0000 Uiso R . . . . . . H543 H 0.7179 0.2682 0.5141 0.0570 1.0000 Uiso R . . . . . . H541 H 0.7398 0.1744 0.5579 0.0572 1.0000 Uiso R . . . . . . H542 H 0.6996 0.1774 0.5450 0.0576 1.0000 Uiso R . . . . . . H551 H 0.6767 0.9222 0.5633 0.0779 0.870(4) Uiso R . P 2 1 . . H552 H 0.7064 0.8427 0.6083 0.0782 0.870(4) Uiso R . P 2 1 . . H553 H 0.6644 0.8357 0.6041 0.0777 0.870(4) Uiso R . P 2 1 . . H562 H 0.6346 0.8291 0.4789 0.0872 0.870(4) Uiso R . P 2 1 . . H563 H 0.6210 0.7536 0.5235 0.0871 0.870(4) Uiso R . P 2 1 . . H561 H 0.6320 0.6825 0.4766 0.0870 0.870(4) Uiso R . P 2 1 . . H571 H 0.6978 0.8290 0.4865 0.0990 0.870(4) Uiso R . P 2 1 . . H572 H 0.7233 0.7467 0.5331 0.0989 0.870(4) Uiso R . P 2 1 . . H573 H 0.6963 0.6861 0.4813 0.0984 0.870(4) Uiso R . P 2 1 . . H582 H 0.7077 0.8867 0.5663 0.0710 0.130(4) Uiso R . P 2 2 . . H583 H 0.7304 0.7678 0.5724 0.0709 0.130(4) Uiso R . P 2 2 . . H581 H 0.7099 0.7947 0.6156 0.0710 0.130(4) Uiso R . P 2 2 . . H591 H 0.6362 0.8665 0.5062 0.0720 0.130(4) Uiso R . P 2 2 . . H593 H 0.6495 0.8851 0.5710 0.0719 0.130(4) Uiso R . P 2 2 . . H592 H 0.6273 0.7689 0.5463 0.0720 0.130(4) Uiso R . P 2 2 . . H602 H 0.6653 0.8290 0.4584 0.0660 0.130(4) Uiso R . P 2 2 . . H601 H 0.7090 0.7120 0.4888 0.0660 0.130(4) Uiso R . P 2 2 . . H603 H 0.6580 0.6359 0.4603 0.0660 0.130(4) Uiso R . P 2 2 . . 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 B1 0.0198(10) 0.0266(11) 0.0251(10) -0.0019(9) 0.0062(8) -0.0027(8) Ti2 0.02214(17) 0.02918(19) 0.02172(18) -0.00006(14) 0.00837(13) 0.00106(14) N3 0.0240(8) 0.0294(8) 0.0235(8) 0.0011(7) 0.0081(6) 0.0037(7) C4 0.0330(10) 0.0320(11) 0.0248(10) 0.0002(8) 0.0132(8) 0.0022(8) C5 0.0406(12) 0.0387(12) 0.0345(11) -0.0063(10) 0.0190(10) -0.0080(10) C6 0.0300(11) 0.0512(15) 0.0395(12) -0.0162(11) 0.0081(9) -0.0070(10) C7 0.0282(10) 0.0530(15) 0.0238(10) -0.0079(10) 0.0028(8) 0.0072(9) C8 0.0241(9) 0.0328(10) 0.0230(9) 0.0013(8) 0.0074(7) 0.0028(8) N9 0.0199(7) 0.0311(9) 0.0240(8) -0.0023(7) 0.0068(6) 0.0010(6) C10 0.0221(9) 0.0357(11) 0.0202(9) -0.0029(8) 0.0065(7) 0.0022(8) C11 0.0295(10) 0.0369(11) 0.0225(9) -0.0028(8) 0.0100(8) 0.0040(8) C12 0.0395(12) 0.0412(13) 0.0256(10) 0.0026(9) 0.0090(9) 0.0106(10) C13 0.0288(10) 0.0537(14) 0.0269(10) -0.0059(10) 0.0005(8) 0.0082(10) C14 0.0255(10) 0.0459(13) 0.0307(11) -0.0088(10) 0.0039(8) -0.0013(9) C15 0.0250(10) 0.0370(11) 0.0283(10) -0.0060(9) 0.0080(8) -0.0001(8) C16 0.0275(10) 0.0354(12) 0.0392(12) -0.0026(10) 0.0051(9) -0.0045(9) C17 0.0564(16) 0.0395(14) 0.0593(16) -0.0074(12) 0.0181(13) -0.0012(12) C18 0.0629(17) 0.0529(16) 0.0561(16) 0.0044(13) 0.0277(14) -0.0050(13) C19 0.0375(11) 0.0358(12) 0.0285(10) 0.0015(9) 0.0112(9) -0.0004(9) C20 0.0561(15) 0.0375(13) 0.0409(13) 0.0010(11) 0.0194(11) 0.0011(11) C21 0.0514(15) 0.0540(16) 0.0525(15) -0.0016(13) 0.0288(12) -0.0043(12) C22 0.0258(10) 0.0406(12) 0.0257(10) -0.0033(9) 0.0110(8) 0.0014(8) C23 0.0244(10) 0.0426(12) 0.0287(10) -0.0028(9) 0.0104(8) 0.0051(8) N24 0.0226(8) 0.0349(9) 0.0236(8) -0.0008(7) 0.0067(6) 0.0013(7) C25 0.0226(9) 0.0422(12) 0.0254(10) -0.0021(9) 0.0047(8) 0.0065(8) C26 0.0337(11) 0.0369(12) 0.0302(10) -0.0006(9) 0.0073(9) 0.0082(9) C27 0.0357(11) 0.0333(11) 0.0385(12) 0.0037(10) 0.0075(9) 0.0045(9) C28 0.0632(17) 0.0399(14) 0.0447(14) -0.0050(11) 0.0125(12) -0.0040(12) C29 0.0527(15) 0.0395(14) 0.0553(16) 0.0085(12) 0.0178(13) 0.0026(11) C30 0.0482(14) 0.0481(15) 0.0371(13) 0.0064(11) 0.0033(11) 0.0097(11) C31 0.0458(15) 0.0652(18) 0.0411(14) 0.0018(13) -0.0099(11) 0.0128(13) C32 0.0299(12) 0.0677(18) 0.0449(14) -0.0038(13) -0.0033(10) 0.0024(11) C33 0.0234(10) 0.0540(14) 0.0371(12) -0.0032(11) 0.0052(9) 0.0024(9) C34 0.0281(11) 0.0675(18) 0.0504(15) 0.0012(13) 0.0092(10) -0.0104(11) C35 0.0435(15) 0.071(2) 0.0701(19) -0.0055(16) 0.0079(14) -0.0182(14) C36 0.0479(17) 0.112(3) 0.073(2) -0.008(2) 0.0314(15) -0.0209(17) N37 0.0284(9) 0.0366(10) 0.0235(8) 0.0011(7) 0.0090(7) 0.0030(7) C38 0.0347(11) 0.0438(13) 0.0249(10) 0.0052(9) 0.0087(8) 0.0009(9) C39 0.0479(14) 0.0582(16) 0.0228(10) 0.0019(10) 0.0093(10) -0.0037(11) C40 0.0509(15) 0.0664(18) 0.0279(11) -0.0094(12) 0.0053(10) -0.0124(13) C41 0.0459(13) 0.0541(15) 0.0365(12) -0.0075(11) 0.0127(10) -0.0175(11) C42 0.0364(11) 0.0420(12) 0.0277(10) 0.0005(9) 0.0122(9) -0.0033(9) N43 0.0347(9) 0.0331(9) 0.0296(9) 0.0016(7) 0.0138(7) 0.0011(7) C44 0.0727(15) 0.0372(12) 0.0430(12) 0.0106(10) 0.0307(11) 0.0077(11) C45 0.0263(10) 0.0367(11) 0.0257(10) -0.0046(9) 0.0068(8) 0.0072(8) C46 0.0290(10) 0.0336(11) 0.0276(10) 0.0010(9) 0.0095(8) 0.0080(8) C47 0.0258(10) 0.0415(12) 0.0233(10) -0.0020(9) 0.0044(8) 0.0083(8) C48 0.0223(9) 0.0408(12) 0.0335(11) -0.0076(9) 0.0053(8) 0.0027(8) C49 0.0239(10) 0.0421(12) 0.0305(10) -0.0025(9) 0.0104(8) 0.0038(8) C50 0.0379(12) 0.0589(16) 0.0509(14) 0.0031(12) 0.0251(11) 0.0016(11) C51 0.0335(12) 0.0488(15) 0.0582(16) -0.0189(13) 0.0074(11) -0.0048(10) C52 0.0359(12) 0.0594(16) 0.0253(10) -0.0039(10) 0.0059(9) 0.0140(11) C53 0.0446(13) 0.0378(13) 0.0465(13) 0.0070(11) 0.0166(11) 0.0095(10) C54 0.0408(12) 0.0460(14) 0.0326(11) -0.0072(10) 0.0089(9) 0.0113(10) C55 0.069(2) 0.0341(15) 0.0584(18) 0.0034(13) 0.0247(15) -0.0014(13) C56 0.087(2) 0.0466(17) 0.0378(15) 0.0120(14) 0.0087(15) 0.0186(16) C57 0.100(3) 0.0532(19) 0.086(2) 0.0238(18) 0.067(2) 0.0085(18) C58 0.078(5) 0.044(5) 0.045(5) 0.009(5) 0.026(5) 0.011(5) C59 0.075(5) 0.043(5) 0.048(5) 0.010(5) 0.032(5) 0.008(4) C60 0.081(6) 0.043(5) 0.042(4) 0.012(5) 0.031(5) 0.005(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.15139(7) 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 B1 . C8 . 1.608(3) yes B1 . N9 . 1.446(3) yes B1 . N24 . 1.446(3) yes Ti2 . N3 . 2.0358(16) yes Ti2 . N37 . 2.1933(17) yes Ti2 . N43 . 1.7177(18) yes Ti2 . C45 . 2.484(2) yes Ti2 . C46 . 2.524(2) yes Ti2 . C47 . 2.437(2) yes Ti2 . C48 . 2.349(2) yes Ti2 . C49 . 2.398(2) yes N3 . C4 . 1.378(3) yes N3 . C8 . 1.491(2) yes C4 . C5 . 1.361(3) yes C4 . H41 . 0.965 no C5 . C6 . 1.440(3) yes C5 . H51 . 0.952 no C6 . C7 . 1.335(3) yes C6 . H61 . 0.946 no C7 . C8 . 1.527(3) yes C7 . H71 . 0.942 no C8 . H81 . 0.998 no N9 . C10 . 1.443(2) yes N9 . C22 . 1.408(2) yes C10 . C11 . 1.403(3) yes C10 . C15 . 1.407(3) yes C11 . C12 . 1.397(3) yes C11 . C19 . 1.518(3) yes C12 . C13 . 1.387(3) yes C12 . H121 . 0.939 no C13 . C14 . 1.379(3) yes C13 . H131 . 0.934 no C14 . C15 . 1.399(3) yes C14 . H141 . 0.937 no C15 . C16 . 1.519(3) yes C16 . C17 . 1.531(3) yes C16 . C18 . 1.531(3) yes C16 . H161 . 0.983 no C17 . H172 . 0.969 no C17 . H171 . 0.964 no C17 . H173 . 0.966 no C18 . H181 . 0.961 no C18 . H183 . 0.955 no C18 . H182 . 0.973 no C19 . C20 . 1.531(3) yes C19 . C21 . 1.542(3) yes C19 . H191 . 1.001 no C20 . H201 . 0.977 no C20 . H202 . 0.977 no C20 . H203 . 0.965 no C21 . H212 . 0.968 no C21 . H213 . 0.980 no C21 . H211 . 0.961 no C22 . C23 . 1.336(3) yes C22 . H221 . 0.947 no C23 . N24 . 1.395(3) yes C23 . H231 . 0.948 no N24 . C25 . 1.442(3) yes C25 . C26 . 1.409(3) yes C25 . C33 . 1.405(3) yes C26 . C27 . 1.523(3) yes C26 . C30 . 1.395(3) yes C27 . C28 . 1.529(3) yes C27 . C29 . 1.535(3) yes C27 . H271 . 0.994 no C28 . H282 . 0.954 no C28 . H283 . 0.962 no C28 . H281 . 0.953 no C29 . H291 . 0.952 no C29 . H293 . 0.967 no C29 . H292 . 0.967 no C30 . C31 . 1.383(4) yes C30 . H301 . 0.943 no C31 . C32 . 1.374(4) yes C31 . H311 . 0.937 no C32 . C33 . 1.398(3) yes C32 . H321 . 0.962 no C33 . C34 . 1.520(4) yes C34 . C35 . 1.522(4) yes C34 . C36 . 1.536(4) yes C34 . H341 . 0.989 no C35 . H353 . 0.966 no C35 . H351 . 0.966 no C35 . H352 . 0.969 no C36 . H361 . 0.972 no C36 . H362 . 0.965 no C36 . H363 . 0.959 no N37 . C38 . 1.351(3) yes N37 . C42 . 1.342(3) yes C38 . C39 . 1.380(3) yes C38 . H381 . 0.952 no C39 . C40 . 1.374(4) yes C39 . H391 . 0.937 no C40 . C41 . 1.383(3) yes C40 . H401 . 0.934 no C41 . C42 . 1.379(3) yes C41 . H411 . 0.934 no C42 . H421 . 0.935 no N43 . C44 . 1.451(2) yes C44 . C55 . 1.526(3) yes C44 . C56 . 1.554(3) yes C44 . C57 . 1.518(3) yes C44 . C58 . 1.548(6) yes C44 . C59 . 1.524(6) yes C44 . C60 . 1.536(6) yes C45 . C46 . 1.425(3) yes C45 . C49 . 1.413(3) yes C45 . C54 . 1.507(3) yes C46 . C47 . 1.417(3) yes C46 . C53 . 1.502(3) yes C47 . C48 . 1.427(3) yes C47 . C52 . 1.503(3) yes C48 . C49 . 1.424(3) yes C48 . C51 . 1.502(3) yes C49 . C50 . 1.505(3) yes C50 . H501 . 0.947 no C50 . H503 . 0.979 no C50 . H502 . 0.959 no C51 . H512 . 0.967 no C51 . H511 . 0.966 no C51 . H513 . 0.968 no C52 . H523 . 0.963 no C52 . H521 . 0.954 no C52 . H522 . 0.963 no C53 . H531 . 0.974 no C53 . H532 . 0.970 no C53 . H533 . 0.965 no C54 . H543 . 0.970 no C54 . H541 . 0.948 no C54 . H542 . 0.959 no C55 . H551 . 0.965 no C55 . H552 . 1.004 no C55 . H553 . 0.974 no C56 . H562 . 0.988 no C56 . H563 . 0.970 no C56 . H561 . 0.976 no C57 . H571 . 0.970 no C57 . H572 . 0.953 no C57 . H573 . 0.950 no C58 . H582 . 0.962 no C58 . H583 . 0.959 no C58 . H581 . 0.963 no C59 . H591 . 0.961 no C59 . H593 . 0.959 no C59 . H592 . 0.961 no C60 . H602 . 1.260 no C60 . H601 . 1.268 no C60 . H603 . 1.266 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 C8 . B1 . N9 . 135.07(17) yes C8 . B1 . N24 . 121.27(17) yes N9 . B1 . N24 . 103.64(16) yes N3 . Ti2 . N37 . 99.78(6) yes N3 . Ti2 . N43 . 104.39(7) yes N37 . Ti2 . N43 . 96.26(8) yes N3 . Ti2 . C45 . 129.09(7) yes N37 . Ti2 . C45 . 78.73(6) yes N43 . Ti2 . C45 . 126.47(8) yes N3 . Ti2 . C46 . 97.95(7) yes N37 . Ti2 . C46 . 94.18(7) yes N43 . Ti2 . C46 . 153.28(8) yes C45 . Ti2 . C46 . 33.04(6) yes N3 . Ti2 . C47 . 91.40(7) yes N37 . Ti2 . C47 . 127.31(7) yes N43 . Ti2 . C47 . 130.50(8) yes C45 . Ti2 . C47 . 55.61(7) yes C46 . Ti2 . C47 . 33.14(7) yes N3 . Ti2 . C48 . 117.98(7) yes N37 . Ti2 . C48 . 133.25(7) yes N43 . Ti2 . C48 . 99.64(8) yes C45 . Ti2 . C48 . 56.56(7) yes C46 . Ti2 . C48 . 56.21(7) yes N3 . Ti2 . C49 . 148.32(7) yes N37 . Ti2 . C49 . 99.48(7) yes N43 . Ti2 . C49 . 98.23(8) yes C45 . Ti2 . C49 . 33.58(7) yes C46 . Ti2 . C49 . 55.71(7) yes C47 . Ti2 . C48 . 34.63(8) yes C47 . Ti2 . C49 . 56.94(7) yes C48 . Ti2 . C49 . 34.90(7) yes Ti2 . N3 . C4 . 117.72(12) yes Ti2 . N3 . C8 . 123.97(12) yes C4 . N3 . C8 . 110.08(15) yes N3 . C4 . C5 . 123.0(2) yes N3 . C4 . H41 . 116.7 no C5 . C4 . H41 . 120.2 no C4 . C5 . C6 . 117.3(2) yes C4 . C5 . H51 . 121.4 no C6 . C5 . H51 . 121.3 no C5 . C6 . C7 . 119.1(2) yes C5 . C6 . H61 . 121.3 no C7 . C6 . H61 . 119.6 no C6 . C7 . C8 . 116.07(19) yes C6 . C7 . H71 . 122.9 no C8 . C7 . H71 . 121.0 no C7 . C8 . N3 . 107.46(16) yes C7 . C8 . B1 . 106.48(15) yes N3 . C8 . B1 . 116.45(16) yes C7 . C8 . H81 . 107.9 no N3 . C8 . H81 . 109.3 no B1 . C8 . H81 . 109.0 no B1 . N9 . C10 . 133.67(15) yes B1 . N9 . C22 . 108.21(16) yes C10 . N9 . C22 . 116.09(15) yes N9 . C10 . C11 . 120.47(17) yes N9 . C10 . C15 . 117.61(18) yes C11 . C10 . C15 . 121.54(18) yes C10 . C11 . C12 . 117.86(19) yes C10 . C11 . C19 . 121.85(18) yes C12 . C11 . C19 . 120.2(2) yes C11 . C12 . C13 . 121.3(2) yes C11 . C12 . H121 . 119.3 no C13 . C12 . H121 . 119.4 no C12 . C13 . C14 . 120.1(2) yes C12 . C13 . H131 . 120.5 no C14 . C13 . H131 . 119.4 no C13 . C14 . C15 . 120.9(2) yes C13 . C14 . H141 . 120.3 no C15 . C14 . H141 . 118.8 no C10 . C15 . C14 . 118.3(2) yes C10 . C15 . C16 . 121.97(18) yes C14 . C15 . C16 . 119.73(19) yes C15 . C16 . C17 . 111.79(19) yes C15 . C16 . C18 . 110.80(19) yes C17 . C16 . C18 . 110.8(2) yes C15 . C16 . H161 . 109.8 no C17 . C16 . H161 . 107.0 no C18 . C16 . H161 . 106.4 no C16 . C17 . H172 . 108.5 no C16 . C17 . H171 . 108.4 no H172 . C17 . H171 . 109.9 no C16 . C17 . H173 . 108.9 no H172 . C17 . H173 . 109.0 no H171 . C17 . H173 . 112.0 no C16 . C18 . H181 . 108.4 no C16 . C18 . H183 . 109.3 no H181 . C18 . H183 . 108.8 no C16 . C18 . H182 . 109.5 no H181 . C18 . H182 . 109.6 no H183 . C18 . H182 . 111.1 no C11 . C19 . C20 . 113.25(19) yes C11 . C19 . C21 . 109.53(18) yes C20 . C19 . C21 . 109.99(19) yes C11 . C19 . H191 . 108.6 no C20 . C19 . H191 . 108.2 no C21 . C19 . H191 . 107.1 no C19 . C20 . H201 . 107.5 no C19 . C20 . H202 . 110.4 no H201 . C20 . H202 . 107.9 no C19 . C20 . H203 . 110.8 no H201 . C20 . H203 . 110.7 no H202 . C20 . H203 . 109.4 no C19 . C21 . H212 . 111.5 no C19 . C21 . H213 . 107.7 no H212 . C21 . H213 . 107.8 no C19 . C21 . H211 . 110.6 no H212 . C21 . H211 . 108.9 no H213 . C21 . H211 . 110.4 no N9 . C22 . C23 . 109.72(17) yes N9 . C22 . H221 . 122.0 no C23 . C22 . H221 . 128.2 no C22 . C23 . N24 . 109.33(17) yes C22 . C23 . H231 . 125.7 no N24 . C23 . H231 . 125.0 no C23 . N24 . B1 . 109.10(16) yes C23 . N24 . C25 . 119.99(16) yes B1 . N24 . C25 . 130.91(16) yes N24 . C25 . C26 . 119.03(18) yes N24 . C25 . C33 . 119.0(2) yes C26 . C25 . C33 . 121.94(19) yes C25 . C26 . C27 . 121.43(18) yes C25 . C26 . C30 . 117.5(2) yes C27 . C26 . C30 . 121.1(2) yes C26 . C27 . C28 . 111.81(19) yes C26 . C27 . C29 . 113.35(19) yes C28 . C27 . C29 . 108.6(2) yes C26 . C27 . H271 . 108.6 no C28 . C27 . H271 . 108.3 no C29 . C27 . H271 . 106.0 no C27 . C28 . H282 . 111.2 no C27 . C28 . H283 . 110.9 no H282 . C28 . H283 . 109.3 no C27 . C28 . H281 . 108.9 no H282 . C28 . H281 . 107.8 no H283 . C28 . H281 . 108.6 no C27 . C29 . H291 . 108.9 no C27 . C29 . H293 . 111.5 no H291 . C29 . H293 . 109.0 no C27 . C29 . H292 . 110.8 no H291 . C29 . H292 . 108.3 no H293 . C29 . H292 . 108.3 no C26 . C30 . C31 . 121.3(3) yes C26 . C30 . H301 . 118.6 no C31 . C30 . H301 . 120.1 no C30 . C31 . C32 . 120.3(2) yes C30 . C31 . H311 . 119.6 no C32 . C31 . H311 . 120.1 no C31 . C32 . C33 . 121.3(2) yes C31 . C32 . H321 . 118.6 no C33 . C32 . H321 . 120.1 no C25 . C33 . C32 . 117.7(2) yes C25 . C33 . C34 . 122.3(2) yes C32 . C33 . C34 . 120.0(2) yes C33 . C34 . C35 . 112.8(2) yes C33 . C34 . C36 . 110.9(3) yes C35 . C34 . C36 . 109.4(2) yes C33 . C34 . H341 . 107.5 no C35 . C34 . H341 . 108.4 no C36 . C34 . H341 . 107.6 no C34 . C35 . H353 . 109.7 no C34 . C35 . H351 . 110.2 no H353 . C35 . H351 . 109.0 no C34 . C35 . H352 . 110.0 no H353 . C35 . H352 . 107.3 no H351 . C35 . H352 . 110.6 no C34 . C36 . H361 . 110.5 no C34 . C36 . H362 . 110.0 no H361 . C36 . H362 . 109.6 no C34 . C36 . H363 . 109.4 no H361 . C36 . H363 . 108.0 no H362 . C36 . H363 . 109.3 no Ti2 . N37 . C38 . 120.31(15) yes Ti2 . N37 . C42 . 122.29(13) yes C38 . N37 . C42 . 117.38(18) yes N37 . C38 . C39 . 122.7(2) yes N37 . C38 . H381 . 117.0 no C39 . C38 . H381 . 120.3 no C38 . C39 . C40 . 119.2(2) yes C38 . C39 . H391 . 122.2 no C40 . C39 . H391 . 118.7 no C39 . C40 . C41 . 118.8(2) yes C39 . C40 . H401 . 119.7 no C41 . C40 . H401 . 121.5 no C40 . C41 . C42 . 118.9(2) yes C40 . C41 . H411 . 121.0 no C42 . C41 . H411 . 120.1 no C41 . C42 . N37 . 123.0(2) yes C41 . C42 . H421 . 119.0 no N37 . C42 . H421 . 118.0 no Ti2 . N43 . C44 . 177.55(14) yes N43 . C44 . C55 . 110.31(17) yes N43 . C44 . C56 . 106.71(18) yes C55 . C44 . C56 . 109.21(6) yes N43 . C44 . C57 . 111.91(17) yes C55 . C44 . C57 . 109.39(6) yes C56 . C44 . C57 . 109.24(6) yes N43 . C44 . C58 . 99.7(6) yes N43 . C44 . C59 . 117.5(6) yes C58 . C44 . C59 . 109.25(6) yes N43 . C44 . C60 . 111.3(6) yes C58 . C44 . C60 . 109.23(6) yes C59 . C44 . C60 . 109.27(6) yes Ti2 . C45 . C46 . 75.02(11) yes Ti2 . C45 . C49 . 69.86(11) yes C46 . C45 . C49 . 108.47(18) yes Ti2 . C45 . C54 . 126.81(14) yes C46 . C45 . C54 . 125.1(2) yes C49 . C45 . C54 . 125.96(19) yes C45 . C46 . Ti2 . 71.94(11) yes C45 . C46 . C47 . 107.77(19) yes Ti2 . C46 . C47 . 70.05(11) yes C45 . C46 . C53 . 123.83(19) yes Ti2 . C46 . C53 . 129.36(14) yes C47 . C46 . C53 . 127.97(19) yes Ti2 . C47 . C46 . 76.81(11) yes Ti2 . C47 . C48 . 69.32(11) yes C46 . C47 . C48 . 107.99(18) yes Ti2 . C47 . C52 . 122.17(14) yes C46 . C47 . C52 . 127.1(2) yes C48 . C47 . C52 . 124.8(2) yes Ti2 . C48 . C47 . 76.05(11) yes Ti2 . C48 . C49 . 74.42(12) yes C47 . C48 . C49 . 107.89(19) yes Ti2 . C48 . C51 . 120.87(15) yes C47 . C48 . C51 . 125.5(2) yes C49 . C48 . C51 . 126.3(2) yes Ti2 . C49 . C48 . 70.68(11) yes Ti2 . C49 . C45 . 76.55(11) yes C48 . C49 . C45 . 107.85(18) yes Ti2 . C49 . C50 . 123.65(15) yes C48 . C49 . C50 . 126.6(2) yes C45 . C49 . C50 . 125.2(2) yes C49 . C50 . H501 . 109.4 no C49 . C50 . H503 . 110.0 no H501 . C50 . H503 . 108.8 no C49 . C50 . H502 . 110.0 no H501 . C50 . H502 . 107.6 no H503 . C50 . H502 . 110.9 no C48 . C51 . H512 . 109.2 no C48 . C51 . H511 . 109.1 no H512 . C51 . H511 . 111.7 no C48 . C51 . H513 . 108.8 no H512 . C51 . H513 . 107.8 no H511 . C51 . H513 . 110.2 no C47 . C52 . H523 . 109.3 no C47 . C52 . H521 . 109.9 no H523 . C52 . H521 . 107.6 no C47 . C52 . H522 . 111.6 no H523 . C52 . H522 . 109.0 no H521 . C52 . H522 . 109.4 no C46 . C53 . H531 . 109.8 no C46 . C53 . H532 . 109.3 no H531 . C53 . H532 . 108.7 no C46 . C53 . H533 . 111.4 no H531 . C53 . H533 . 108.7 no H532 . C53 . H533 . 108.9 no C45 . C54 . H543 . 110.7 no C45 . C54 . H541 . 110.0 no H543 . C54 . H541 . 109.8 no C45 . C54 . H542 . 108.9 no H543 . C54 . H542 . 108.3 no H541 . C54 . H542 . 109.1 no C44 . C55 . H551 . 107.0 no C44 . C55 . H552 . 109.9 no H551 . C55 . H552 . 111.8 no C44 . C55 . H553 . 105.8 no H551 . C55 . H553 . 108.1 no H552 . C55 . H553 . 113.9 no C44 . C56 . H562 . 111.0 no C44 . C56 . H563 . 109.5 no H562 . C56 . H563 . 109.9 no C44 . C56 . H561 . 109.8 no H562 . C56 . H561 . 108.9 no H563 . C56 . H561 . 107.7 no C44 . C57 . H571 . 111.4 no C44 . C57 . H572 . 106.1 no H571 . C57 . H572 . 111.2 no C44 . C57 . H573 . 107.8 no H571 . C57 . H573 . 108.6 no H572 . C57 . H573 . 111.6 no C44 . C58 . H582 . 105.2 no C44 . C58 . H583 . 116.1 no H582 . C58 . H583 . 108.9 no C44 . C58 . H581 . 108.1 no H582 . C58 . H581 . 109.3 no H583 . C58 . H581 . 109.0 no C44 . C59 . H591 . 109.7 no C44 . C59 . H593 . 114.7 no H591 . C59 . H593 . 109.5 no C44 . C59 . H592 . 103.4 no H591 . C59 . H592 . 109.8 no H593 . C59 . H592 . 109.6 no C44 . C60 . H602 . 103.8 no C44 . C60 . H601 . 101.2 no H602 . C60 . H601 . 114.1 no C44 . C60 . H603 . 107.1 no H602 . C60 . H603 . 114.3 no H601 . C60 . H603 . 114.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C28 . H283 . C23 . 147 0.96 2.59 3.432(4) yes C51 . H512 . C58 . 147 0.97 2.57 3.418(4) yes # start Validation Reply Form _vrf_PLAT412_124apdv09 ; PROBLEM: Short Intra XH3 .. XHn H381 .. H603 .. 1.78 Ang. RESPONSE: The contact is due to the disordered tBuN group found on the Ti center. ; # end Validation Reply Form