# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 857128' #TrackingRef 'Final CrystallographicData.cif' #============================================================================== _audit_creation_date 11-12-05 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title '4030939 Compound X' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 9.9819(2) _cell_length_b 10.0605(2) _cell_length_c 12.3107(3) _cell_angle_alpha 83.6209(8) _cell_angle_beta 69.1742(8) _cell_angle_gamma 76.6715(10) _cell_volume 1123.80(4) _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' 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' Mn 0.3368 0.7283 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C23 Al1 Cl1 Mn1 N2 # Dc = 1.25 Fooo = 476.00 Mu = 7.53 M = 421.63 # Found Formula = C21 H27 Al1 Cl1 Mn1 N2 O2 # Dc = 1.35 FOOO = 476.00 Mu = 7.63 M = 456.82 _chemical_formula_sum 'C21 H27 Al1 Cl1 Mn1 N2 O2' _chemical_formula_moiety 'C21 H27 Al1 Cl1 Mn1 N2 O2' _chemical_compound_source . _chemical_formula_weight 456.82 _cell_measurement_reflns_used 4691 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.150 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_max 0.180 _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 476 _exptl_absorpt_coefficient_mu 0.763 # Sheldrick geometric approximatio 0.89 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.89 # 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 8684 _reflns_number_total 5039 _diffrn_reflns_av_R_equivalents 0.000 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 5039 # Theoretical number of reflections is about 10233 _diffrn_reflns_theta_min 5.108 _diffrn_reflns_theta_max 27.410 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.217 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -11 _reflns_limit_h_max 12 _reflns_limit_k_min -12 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 2.13 _oxford_diffrn_Wilson_scale 4.14 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.51 _refine_diff_density_max 0.46 # 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 5039 _refine_ls_number_restraints 0 _refine_ls_number_parameters 257 _oxford_refine_ls_R_factor_ref 0.0517 _refine_ls_wR_factor_ref 0.0711 _refine_ls_goodness_of_fit_ref 0.9218 _refine_ls_shift/su_max 0.0095554 _refine_ls_shift/su_mean 0.0001490 # The values computed from all data _oxford_reflns_number_all 5039 _refine_ls_R_factor_all 0.0517 _refine_ls_wR_factor_all 0.0711 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3942 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_gt 0.0571 # 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 mixed # 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: 6.66 7.63 2.26 ; # Insert your own references if required - in alphabetical order 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 Mn1 Mn 0.52835(4) 0.50457(3) 0.21398(3) 0.0220 1.0000 Uani . . . . . . Al2 Al 0.73540(7) 0.31223(6) 0.14854(6) 0.0235 1.0000 Uani . . . . . . Cl3 Cl 0.89646(8) 0.33782(7) -0.01978(6) 0.0431 1.0000 Uani . . . . . . N4 N 0.8326(2) 0.22074(18) 0.25418(17) 0.0256 1.0000 Uani . . . . . . C5 C 0.7861(2) 0.1084(2) 0.25002(19) 0.0224 1.0000 Uani . . . . . . N6 N 0.7109(2) 0.12768(18) 0.17731(17) 0.0261 1.0000 Uani . . . . . . C7 C 0.6535(3) 0.0218(2) 0.1461(2) 0.0269 1.0000 Uani . . . . . . C8 C 0.4968(3) 0.0780(3) 0.1515(2) 0.0340 1.0000 Uani . . . . . . C9 C 0.7500(3) -0.0284(3) 0.0257(2) 0.0388 1.0000 Uani . . . . . . C10 C 0.8069(2) -0.0206(2) 0.31971(19) 0.0229 1.0000 Uani . . . . . . C11 C 0.7100(3) -0.0319(3) 0.4321(2) 0.0327 1.0000 Uani . . . . . . C12 C 0.7234(3) -0.1549(3) 0.4954(2) 0.0412 1.0000 Uani . . . . . . C13 C 0.8322(3) -0.2649(3) 0.4469(2) 0.0398 1.0000 Uani . . . . . . C14 C 0.9286(3) -0.2542(2) 0.3352(2) 0.0365 1.0000 Uani . . . . . . C15 C 0.9160(3) -0.1322(2) 0.2710(2) 0.0296 1.0000 Uani . . . . . . C16 C 0.9202(2) 0.2315(2) 0.3251(2) 0.0266 1.0000 Uani . . . . . . C17 C 0.8931(3) 0.3797(2) 0.3557(3) 0.0392 1.0000 Uani . . . . . . C18 C 1.0816(3) 0.1767(3) 0.2620(3) 0.0439 1.0000 Uani . . . . . . C19 C 0.6201(3) 0.6389(2) 0.0731(2) 0.0335 1.0000 Uani . . . . . . C20 C 0.6958(3) 0.6210(2) 0.1540(2) 0.0321 1.0000 Uani . . . . . . C21 C 0.5922(3) 0.6700(2) 0.2621(2) 0.0290 1.0000 Uani . . . . . . C22 C 0.4532(3) 0.7165(2) 0.2498(2) 0.0282 1.0000 Uani . . . . . . C23 C 0.4721(3) 0.6964(2) 0.1315(2) 0.0322 1.0000 Uani . . . . . . C24 C 0.3151(3) 0.7832(3) 0.3403(2) 0.0424 1.0000 Uani . . . . . . C25 C 0.5312(2) 0.4109(2) 0.3436(2) 0.0264 1.0000 Uani . . . . . . O26 O 0.52389(19) 0.35470(18) 0.43307(15) 0.0367 1.0000 Uani . . . . . . C27 C 0.3524(3) 0.4686(2) 0.2429(2) 0.0332 1.0000 Uani . . . . . . O28 O 0.2369(2) 0.4470(2) 0.2645(2) 0.0539 1.0000 Uani . . . . . . H71 H 0.6546 -0.0549 0.2025 0.0324 1.0000 Uiso R . . . . . H81 H 0.4573 0.0095 0.1302 0.0502 1.0000 Uiso R . . . . . H82 H 0.4358 0.1048 0.2294 0.0510 1.0000 Uiso R . . . . . H83 H 0.4914 0.1582 0.0996 0.0505 1.0000 Uiso R . . . . . H91 H 0.7104 -0.0970 0.0050 0.0577 1.0000 Uiso R . . . . . H93 H 0.8489 -0.0679 0.0238 0.0577 1.0000 Uiso R . . . . . H92 H 0.7519 0.0473 -0.0307 0.0574 1.0000 Uiso R . . . . . H111 H 0.6359 0.0443 0.4653 0.0392 1.0000 Uiso R . . . . . H121 H 0.6572 -0.1633 0.5708 0.0498 1.0000 Uiso R . . . . . H131 H 0.8403 -0.3474 0.4901 0.0479 1.0000 Uiso R . . . . . H141 H 1.0018 -0.3289 0.3026 0.0448 1.0000 Uiso R . . . . . H151 H 0.9806 -0.1252 0.1945 0.0348 1.0000 Uiso R . . . . . H161 H 0.8901 0.1777 0.3961 0.0318 1.0000 Uiso R . . . . . H171 H 0.9498 0.3858 0.4040 0.0586 1.0000 Uiso R . . . . . H173 H 0.9233 0.4348 0.2855 0.0589 1.0000 Uiso R . . . . . H172 H 0.7907 0.4132 0.3984 0.0583 1.0000 Uiso R . . . . . H181 H 1.1379 0.1859 0.3105 0.0660 1.0000 Uiso R . . . . . H183 H 1.1116 0.2300 0.1899 0.0655 1.0000 Uiso R . . . . . H182 H 1.0982 0.0802 0.2456 0.0653 1.0000 Uiso R . . . . . H191 H 0.6641 0.6142 -0.0085 0.0408 1.0000 Uiso R . . . . . H201 H 0.8006 0.5886 0.1371 0.0392 1.0000 Uiso R . . . . . H211 H 0.6129 0.6726 0.3333 0.0350 1.0000 Uiso R . . . . . H231 H 0.3942 0.7158 0.0985 0.0395 1.0000 Uiso R . . . . . H241 H 0.2293 0.7646 0.3286 0.0641 1.0000 Uiso R . . . . . H243 H 0.3076 0.8823 0.3338 0.0638 1.0000 Uiso R . . . . . H242 H 0.3164 0.7486 0.4178 0.0639 1.0000 Uiso R . . . . . H21 H 0.581(3) 0.396(3) 0.119(2) 0.0333 1.0000 Uiso . . . . . . 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 Mn1 0.02267(17) 0.01840(16) 0.02561(18) 0.00125(12) -0.00890(13) -0.00515(12) Al2 0.0259(3) 0.0182(3) 0.0268(3) -0.0010(3) -0.0092(3) -0.0047(3) Cl3 0.0424(4) 0.0353(3) 0.0355(3) -0.0033(3) 0.0045(3) -0.0043(3) N4 0.0265(10) 0.0202(9) 0.0349(11) -0.0038(8) -0.0153(8) -0.0049(7) C5 0.0202(10) 0.0201(10) 0.0262(11) -0.0026(8) -0.0076(9) -0.0025(8) N6 0.0327(10) 0.0199(9) 0.0328(10) -0.0008(8) -0.0185(9) -0.0076(8) C7 0.0368(13) 0.0190(10) 0.0331(12) 0.0024(9) -0.0198(10) -0.0102(9) C8 0.0329(13) 0.0387(14) 0.0355(13) -0.0013(11) -0.0140(11) -0.0133(11) C9 0.0407(15) 0.0319(13) 0.0474(16) -0.0138(11) -0.0174(13) -0.0045(11) C10 0.0246(11) 0.0212(10) 0.0279(11) -0.0012(8) -0.0136(9) -0.0064(8) C11 0.0366(13) 0.0318(13) 0.0289(12) -0.0054(10) -0.0082(10) -0.0085(10) C12 0.0571(18) 0.0426(15) 0.0270(13) 0.0042(11) -0.0130(12) -0.0210(13) C13 0.0576(17) 0.0325(13) 0.0419(15) 0.0118(11) -0.0319(14) -0.0155(12) C14 0.0369(14) 0.0236(12) 0.0513(16) 0.0019(11) -0.0221(12) -0.0005(10) C15 0.0260(12) 0.0250(11) 0.0358(13) -0.0013(10) -0.0094(10) -0.0032(9) C16 0.0237(11) 0.0286(11) 0.0328(12) -0.0068(9) -0.0139(10) -0.0061(9) C17 0.0343(14) 0.0302(13) 0.0617(18) -0.0145(12) -0.0240(13) -0.0048(11) C18 0.0239(13) 0.0506(16) 0.0591(18) -0.0224(14) -0.0156(12) 0.0006(11) C19 0.0447(15) 0.0221(11) 0.0276(12) 0.0042(9) -0.0048(11) -0.0094(10) C20 0.0279(12) 0.0230(11) 0.0417(14) 0.0023(10) -0.0052(11) -0.0104(9) C21 0.0354(13) 0.0204(11) 0.0350(13) -0.0013(9) -0.0129(10) -0.0114(9) C22 0.0307(12) 0.0182(10) 0.0325(12) 0.0007(9) -0.0075(10) -0.0047(9) C23 0.0411(14) 0.0209(11) 0.0346(13) 0.0058(9) -0.0160(11) -0.0045(10) C24 0.0418(15) 0.0311(13) 0.0460(16) -0.0083(12) -0.0082(13) 0.0010(11) C25 0.0230(11) 0.0231(11) 0.0319(12) -0.0016(9) -0.0076(9) -0.0047(9) O26 0.0396(10) 0.0395(10) 0.0293(9) 0.0088(8) -0.0111(8) -0.0103(8) C27 0.0329(13) 0.0280(12) 0.0411(14) 0.0022(10) -0.0168(11) -0.0059(10) O28 0.0320(11) 0.0528(13) 0.0832(16) 0.0090(11) -0.0245(11) -0.0186(9) _refine_ls_extinction_coef 33(5) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.4893(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 Mn1 . Al2 . 2.4461(7) yes Mn1 . C19 . 2.143(2) yes Mn1 . C20 . 2.131(2) yes Mn1 . C21 . 2.122(2) yes Mn1 . C22 . 2.130(2) yes Mn1 . C23 . 2.131(2) yes Mn1 . C25 . 1.766(2) yes Mn1 . C27 . 1.778(2) yes Mn1 . H21 . 1.56(2) no Al2 . Cl3 . 2.1560(9) yes Al2 . N4 . 1.923(2) yes Al2 . C5 . 2.329(2) yes Al2 . N6 . 1.9062(19) yes Al2 . C25 . 2.650(2) yes Al2 . H21 . 1.71(2) no N4 . C5 . 1.329(3) yes N4 . C16 . 1.465(3) yes C5 . N6 . 1.331(3) yes C5 . C10 . 1.490(3) yes N6 . C7 . 1.463(3) yes C7 . C8 . 1.516(3) yes C7 . C9 . 1.519(3) yes C7 . H71 . 0.980 no C8 . H81 . 0.969 no C8 . H82 . 0.964 no C8 . H83 . 0.975 no C9 . H91 . 0.966 no C9 . H93 . 0.969 no C9 . H92 . 0.971 no C10 . C11 . 1.388(3) yes C10 . C15 . 1.388(3) yes C11 . C12 . 1.392(3) yes C11 . H111 . 0.947 no C12 . C13 . 1.375(4) yes C12 . H121 . 0.937 no C13 . C14 . 1.379(4) yes C13 . H131 . 0.938 no C14 . C15 . 1.390(3) yes C14 . H141 . 0.931 no C15 . H151 . 0.939 no C16 . C17 . 1.518(3) yes C16 . C18 . 1.517(3) yes C16 . H161 . 0.965 no C17 . H171 . 0.970 no C17 . H173 . 0.965 no C17 . H172 . 0.967 no C18 . H181 . 0.977 no C18 . H183 . 0.972 no C18 . H182 . 0.977 no C19 . C20 . 1.424(4) yes C19 . C23 . 1.406(3) yes C19 . H191 . 0.977 no C20 . C21 . 1.420(3) yes C20 . H201 . 0.973 no C21 . C22 . 1.416(3) yes C21 . H211 . 0.973 no C22 . C23 . 1.431(3) yes C22 . C24 . 1.496(3) yes C23 . H231 . 0.972 no C24 . H241 . 0.978 no C24 . H243 . 0.979 no C24 . H242 . 0.982 no C25 . O26 . 1.167(3) yes C27 . O28 . 1.154(3) yes 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 Al2 . Mn1 . C19 . 94.09(7) yes Al2 . Mn1 . C20 . 83.09(7) yes C19 . Mn1 . C20 . 38.92(10) yes Al2 . Mn1 . C21 . 111.40(7) yes C19 . Mn1 . C21 . 65.01(9) yes C20 . Mn1 . C21 . 39.00(9) yes Al2 . Mn1 . C22 . 148.18(7) yes C19 . Mn1 . C22 . 65.32(9) yes C20 . Mn1 . C22 . 65.58(9) yes C21 . Mn1 . C22 . 38.89(9) yes Al2 . Mn1 . C23 . 131.39(7) yes C19 . Mn1 . C23 . 38.41(9) yes C20 . Mn1 . C23 . 65.02(10) yes C21 . Mn1 . C23 . 65.00(9) yes C22 . Mn1 . C23 . 39.24(9) yes Al2 . Mn1 . C25 . 76.06(7) yes C19 . Mn1 . C25 . 150.09(10) yes C20 . Mn1 . C25 . 111.23(10) yes C21 . Mn1 . C25 . 91.99(10) yes C22 . Mn1 . C25 . 109.23(10) yes Al2 . Mn1 . C27 . 115.69(8) yes C19 . Mn1 . C27 . 121.95(11) yes C20 . Mn1 . C27 . 156.93(10) yes C21 . Mn1 . C27 . 131.18(11) yes C22 . Mn1 . C27 . 96.06(10) yes Al2 . Mn1 . H21 . 44.1(9) no C19 . Mn1 . H21 . 84.9(9) no C20 . Mn1 . H21 . 102.4(9) no C21 . Mn1 . H21 . 141.3(9) no C22 . Mn1 . H21 . 145.5(9) no C23 . Mn1 . C25 . 148.22(10) yes C23 . Mn1 . C27 . 91.96(11) yes C25 . Mn1 . C27 . 87.37(11) yes C23 . Mn1 . H21 . 106.3(9) no C25 . Mn1 . H21 . 105.3(9) no C27 . Mn1 . H21 . 84.8(9) no Mn1 . Al2 . Cl3 . 116.32(3) yes Mn1 . Al2 . N4 . 119.93(6) yes Cl3 . Al2 . N4 . 109.42(7) yes Mn1 . Al2 . C5 . 127.81(6) yes Cl3 . Al2 . C5 . 115.79(6) yes N4 . Al2 . C5 . 34.80(7) yes Mn1 . Al2 . N6 . 121.66(7) yes Cl3 . Al2 . N6 . 111.21(7) yes N4 . Al2 . N6 . 69.66(8) yes C5 . Al2 . N6 . 34.87(7) yes Mn1 . Al2 . C25 . 40.31(5) yes Cl3 . Al2 . C25 . 151.81(6) yes N4 . Al2 . C25 . 82.45(8) yes C5 . Al2 . C25 . 88.80(8) yes N6 . Al2 . C25 . 96.83(8) yes Mn1 . Al2 . H21 . 39.2(8) no Cl3 . Al2 . H21 . 98.7(8) no N4 . Al2 . H21 . 151.7(8) no C5 . Al2 . H21 . 132.1(8) no N6 . Al2 . H21 . 103.4(8) no C25 . Al2 . H21 . 70.9(8) no Al2 . N4 . C5 . 89.54(13) yes Al2 . N4 . C16 . 146.66(15) yes C5 . N4 . C16 . 123.79(19) yes Al2 . C5 . N4 . 55.66(11) yes Al2 . C5 . N6 . 54.94(11) yes N4 . C5 . N6 . 110.57(19) yes Al2 . C5 . C10 . 175.86(16) yes N4 . C5 . C10 . 126.06(19) yes N6 . C5 . C10 . 123.32(19) yes C5 . N6 . Al2 . 90.20(13) yes C5 . N6 . C7 . 124.68(18) yes Al2 . N6 . C7 . 145.04(15) yes N6 . C7 . C8 . 109.69(18) yes N6 . C7 . C9 . 109.80(19) yes C8 . C7 . C9 . 111.2(2) yes N6 . C7 . H71 . 108.6 no C8 . C7 . H71 . 108.7 no C9 . C7 . H71 . 108.8 no C7 . C8 . H81 . 110.8 no C7 . C8 . H82 . 110.2 no H81 . C8 . H82 . 107.8 no C7 . C8 . H83 . 110.5 no H81 . C8 . H83 . 109.3 no H82 . C8 . H83 . 108.1 no C7 . C9 . H91 . 109.4 no C7 . C9 . H93 . 110.8 no H91 . C9 . H93 . 109.0 no C7 . C9 . H92 . 109.6 no H91 . C9 . H92 . 108.7 no H93 . C9 . H92 . 109.3 no C5 . C10 . C11 . 119.4(2) yes C5 . C10 . C15 . 120.7(2) yes C11 . C10 . C15 . 119.8(2) yes C10 . C11 . C12 . 119.8(2) yes C10 . C11 . H111 . 119.7 no C12 . C11 . H111 . 120.6 no C11 . C12 . C13 . 120.2(2) yes C11 . C12 . H121 . 120.0 no C13 . C12 . H121 . 119.8 no C12 . C13 . C14 . 120.2(2) yes C12 . C13 . H131 . 119.7 no C14 . C13 . H131 . 120.1 no C13 . C14 . C15 . 120.1(2) yes C13 . C14 . H141 . 120.0 no C15 . C14 . H141 . 119.9 no C14 . C15 . C10 . 119.9(2) yes C14 . C15 . H151 . 120.2 no C10 . C15 . H151 . 119.9 no N4 . C16 . C17 . 109.19(19) yes N4 . C16 . C18 . 111.0(2) yes C17 . C16 . C18 . 111.0(2) yes N4 . C16 . H161 . 109.1 no C17 . C16 . H161 . 108.6 no C18 . C16 . H161 . 107.9 no C16 . C17 . H171 . 108.7 no C16 . C17 . H173 . 109.6 no H171 . C17 . H173 . 109.5 no C16 . C17 . H172 . 110.7 no H171 . C17 . H172 . 108.7 no H173 . C17 . H172 . 109.6 no C16 . C18 . H181 . 109.6 no C16 . C18 . H183 . 107.9 no H181 . C18 . H183 . 109.9 no C16 . C18 . H182 . 110.2 no H181 . C18 . H182 . 109.0 no H183 . C18 . H182 . 110.3 no Mn1 . C19 . C20 . 70.09(13) yes Mn1 . C19 . C23 . 70.33(13) yes C20 . C19 . C23 . 108.1(2) yes Mn1 . C19 . H191 . 124.8 no C20 . C19 . H191 . 125.4 no C23 . C19 . H191 . 126.5 no Mn1 . C20 . C19 . 70.99(13) yes Mn1 . C20 . C21 . 70.16(13) yes C19 . C20 . C21 . 107.4(2) yes Mn1 . C20 . H201 . 128.1 no C19 . C20 . H201 . 126.5 no C21 . C20 . H201 . 125.9 no Mn1 . C21 . C20 . 70.85(13) yes Mn1 . C21 . C22 . 70.87(13) yes C20 . C21 . C22 . 109.0(2) yes Mn1 . C21 . H211 . 125.0 no C20 . C21 . H211 . 125.9 no C22 . C21 . H211 . 125.1 no Mn1 . C22 . C21 . 70.25(12) yes Mn1 . C22 . C23 . 70.40(13) yes C21 . C22 . C23 . 106.8(2) yes Mn1 . C22 . C24 . 127.62(17) yes C21 . C22 . C24 . 126.7(2) yes C23 . C22 . C24 . 126.4(2) yes Mn1 . C23 . C22 . 70.36(13) yes Mn1 . C23 . C19 . 71.27(13) yes C22 . C23 . C19 . 108.8(2) yes Mn1 . C23 . H231 . 122.3 no C22 . C23 . H231 . 125.2 no C19 . C23 . H231 . 126.0 no C22 . C24 . H241 . 110.8 no C22 . C24 . H243 . 109.2 no H241 . C24 . H243 . 107.6 no C22 . C24 . H242 . 109.5 no H241 . C24 . H242 . 109.5 no H243 . C24 . H242 . 110.2 no Al2 . C25 . Mn1 . 63.63(7) yes Al2 . C25 . O26 . 120.98(17) yes Mn1 . C25 . O26 . 175.3(2) yes Mn1 . C27 . O28 . 178.2(3) yes Al2 . H21 . Mn1 . 96.7(13) no data_Fe _database_code_depnum_ccdc_archive 'CCDC 857132' #TrackingRef 'Final CrystallographicData.cif' #============================================================================== _audit_creation_date 10-06-02 _audit_creation_method CRYSTALS_ver_14.03 _oxford_structure_analysis_title 051irdv10 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 9.9088(2) _cell_length_b 12.3092(3) _cell_length_c 17.7168(4) _cell_angle_alpha 90 _cell_angle_beta 93.0773(10) _cell_angle_gamma 90 _cell_volume 2157.79(8) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' 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' 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' 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' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 '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' 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 = C20 H30 Al1 Cl1 Fe1 N2 O2 # Dc = 1.38 Fooo = 920.00 Mu = 8.81 M = 448.75 # Found Formula = C20 H24 Al1 Cl1 Fe1 N2 O2 # Dc = 1.36 FOOO = 920.00 Mu = 8.80 M = 442.70 _chemical_formula_sum 'C20 H24 Al1 Cl1 Fe1 N2 O2' _chemical_formula_moiety 'C20 H24 Al1 Cl1 Fe1 N2 O2' _chemical_compound_source . _chemical_formula_weight 442.70 _cell_measurement_reflns_used 4943 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.100 _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.880 # Sheldrick geometric approximatio 0.92 0.92 # 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 0.92 _exptl_absorpt_correction_T_max 0.92 # 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 9335 _reflns_number_total 4907 _diffrn_reflns_av_R_equivalents 0.033 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 4907 # Theoretical number of reflections is about 9902 _diffrn_reflns_theta_min 5.101 _diffrn_reflns_theta_max 27.487 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.388 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 2.34 _oxford_diffrn_Wilson_scale 16.53 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.78 _refine_diff_density_max 0.90 # 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 4907 _refine_ls_number_restraints 0 _refine_ls_number_parameters 244 _oxford_refine_ls_R_factor_ref 0.0675 _refine_ls_wR_factor_ref 0.1365 _refine_ls_goodness_of_fit_ref 0.9274 _refine_ls_shift/su_max 0.0010660 _refine_ls_shift/su_mean 4.7106056 # The values computed from all data _oxford_reflns_number_all 4907 _refine_ls_R_factor_all 0.0675 _refine_ls_wR_factor_all 0.1365 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3672 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_gt 0.1224 # 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^) + ( 0.10P)^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 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 Fe1 Fe 0.99485(3) 0.16823(3) 0.714115(18) 0.0254 1.0000 Uani . . . . . . . Al2 Al 0.82983(7) 0.10713(6) 0.62465(4) 0.0244 1.0000 Uani . . . . . . . Cl3 Cl 0.85460(7) -0.05454(5) 0.58051(4) 0.0388 1.0000 Uani . . . . . . . N4 N 0.7570(2) 0.20530(17) 0.54916(12) 0.0287 1.0000 Uani . . . . . . . C5 C 0.6379(2) 0.2034(2) 0.58123(14) 0.0279 1.0000 Uani . . . . . . . N6 N 0.6411(2) 0.13385(17) 0.63951(11) 0.0278 1.0000 Uani . . . . . . . C7 C 0.5287(2) 0.1138(2) 0.68709(13) 0.0297 1.0000 Uani . . . . . . . C8 C 0.5465(3) 0.1748(2) 0.76166(16) 0.0395 1.0000 Uani . . . . . . . C9 C 0.5181(3) -0.0081(2) 0.70020(18) 0.0446 1.0000 Uani . . . . . . . C10 C 0.5197(2) 0.2714(2) 0.55666(14) 0.0275 1.0000 Uani . . . . . . . C11 C 0.5017(3) 0.3720(2) 0.59046(16) 0.0366 1.0000 Uani . . . . . . . C12 C 0.3936(3) 0.4376(2) 0.56698(18) 0.0435 1.0000 Uani . . . . . . . C13 C 0.3037(3) 0.4034(2) 0.51009(18) 0.0412 1.0000 Uani . . . . . . . C14 C 0.3198(3) 0.3034(3) 0.47685(17) 0.0412 1.0000 Uani . . . . . . . C15 C 0.4278(3) 0.2367(2) 0.49954(16) 0.0382 1.0000 Uani . . . . . . . C16 C 0.7865(3) 0.2698(2) 0.48322(14) 0.0317 1.0000 Uani . . . . . . . C17 C 0.9191(3) 0.3302(2) 0.49688(19) 0.0454 1.0000 Uani . . . . . . . C18 C 0.7921(3) 0.1965(3) 0.41462(17) 0.0462 1.0000 Uani . . . . . . . C19 C 0.9075(2) 0.0830(2) 0.77332(14) 0.0315 1.0000 Uani . . . . . . . O20 O 0.8545(2) 0.02464(17) 0.81314(11) 0.0446 1.0000 Uani . . . . . . . C21 C 1.1359(3) 0.1454(2) 0.63051(14) 0.0321 1.0000 Uani . . . . . . . C22 C 1.1570(2) 0.0686(2) 0.68927(15) 0.0335 1.0000 Uani . . . . . . . C23 C 1.1881(2) 0.1256(2) 0.75893(16) 0.0370 1.0000 Uani . . . . . . . C24 C 1.1852(2) 0.2380(2) 0.74220(16) 0.0370 1.0000 Uani . . . . . . . C25 C 1.1514(2) 0.2503(2) 0.66373(16) 0.0346 1.0000 Uani . . . . . . . C26 C 0.8847(3) 0.2792(2) 0.71415(14) 0.0315 1.0000 Uani . . . . . . . O27 O 0.8137(2) 0.35388(16) 0.71230(12) 0.0430 1.0000 Uani . . . . . . . H71 H 0.4431 0.1401 0.6594 0.0334 1.0000 Uiso R . . . . . . H82 H 0.4742 0.1578 0.7931 0.0621 1.0000 Uiso R . . . . . . H81 H 0.6300 0.1542 0.7881 0.0613 1.0000 Uiso R . . . . . . H83 H 0.5481 0.2521 0.7526 0.0623 1.0000 Uiso R . . . . . . H92 H 0.4380 -0.0267 0.7271 0.0679 1.0000 Uiso R . . . . . . H91 H 0.5968 -0.0322 0.7289 0.0677 1.0000 Uiso R . . . . . . H93 H 0.5184 -0.0465 0.6513 0.0684 1.0000 Uiso R . . . . . . H111 H 0.5623 0.3955 0.6287 0.0445 1.0000 Uiso R . . . . . . H121 H 0.3839 0.5054 0.5895 0.0512 1.0000 Uiso R . . . . . . H131 H 0.2285 0.4477 0.4950 0.0487 1.0000 Uiso R . . . . . . H141 H 0.2570 0.2792 0.4377 0.0499 1.0000 Uiso R . . . . . . H151 H 0.4376 0.1685 0.4768 0.0467 1.0000 Uiso R . . . . . . H161 H 0.7135 0.3224 0.4774 0.0355 1.0000 Uiso R . . . . . . H172 H 0.9316 0.3780 0.4551 0.0706 1.0000 Uiso R . . . . . . H171 H 0.9090 0.3723 0.5424 0.0714 1.0000 Uiso R . . . . . . H173 H 0.9910 0.2781 0.5033 0.0705 1.0000 Uiso R . . . . . . H182 H 0.8108 0.2386 0.3697 0.0691 1.0000 Uiso R . . . . . . H181 H 0.8642 0.1444 0.4253 0.0691 1.0000 Uiso R . . . . . . H183 H 0.7070 0.1579 0.4083 0.0696 1.0000 Uiso R . . . . . . H211 H 1.1152 0.1280 0.5771 0.0365 1.0000 Uiso R . . . . . . H221 H 1.1521 -0.0114 0.6841 0.0399 1.0000 Uiso R . . . . . . H231 H 1.2143 0.0901 0.8080 0.0435 1.0000 Uiso R . . . . . . H241 H 1.1994 0.2967 0.7780 0.0445 1.0000 Uiso R . . . . . . H251 H 1.1338 0.3191 0.6385 0.0413 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 Fe1 0.0255(2) 0.0248(2) 0.0259(2) -0.00054(13) 0.00209(14) -0.00048(13) Al2 0.0253(4) 0.0234(4) 0.0247(3) -0.0005(3) 0.0021(3) 0.0020(3) Cl3 0.0441(4) 0.0273(3) 0.0445(4) -0.0091(3) -0.0012(3) 0.0032(3) N4 0.0292(10) 0.0290(10) 0.0279(10) 0.0047(9) 0.0036(8) 0.0037(8) C5 0.0272(12) 0.0249(12) 0.0312(13) -0.0028(10) -0.0019(9) 0.0022(10) N6 0.0268(10) 0.0294(10) 0.0270(10) 0.0053(9) 0.0006(8) -0.0002(9) C7 0.0235(11) 0.0383(14) 0.0277(12) 0.0034(11) 0.0058(10) -0.0007(10) C8 0.0327(14) 0.0449(16) 0.0416(15) -0.0034(12) 0.0088(12) 0.0007(12) C9 0.0404(16) 0.0387(16) 0.0555(18) 0.0090(14) 0.0104(13) -0.0044(12) C10 0.0268(11) 0.0285(12) 0.0275(12) 0.0029(10) 0.0044(9) 0.0015(10) C11 0.0360(14) 0.0312(13) 0.0423(15) -0.0030(12) -0.0012(11) 0.0042(11) C12 0.0443(16) 0.0324(14) 0.0542(18) -0.0015(13) 0.0073(13) 0.0095(12) C13 0.0313(13) 0.0343(14) 0.0582(18) 0.0131(13) 0.0050(12) 0.0054(11) C14 0.0351(14) 0.0478(16) 0.0398(16) 0.0078(13) -0.0069(11) 0.0017(12) C15 0.0394(14) 0.0326(14) 0.0418(15) -0.0020(12) -0.0043(11) 0.0025(11) C16 0.0334(13) 0.0303(13) 0.0314(13) 0.0069(11) 0.0021(10) 0.0080(10) C17 0.0451(17) 0.0443(17) 0.0460(16) 0.0185(14) -0.0043(13) -0.0095(13) C18 0.0563(18) 0.0506(17) 0.0321(14) -0.0023(13) 0.0051(13) 0.0039(15) C19 0.0295(12) 0.0351(13) 0.0297(12) -0.0022(11) 0.0005(10) 0.0028(11) O20 0.0453(11) 0.0457(11) 0.0438(11) 0.0140(10) 0.0118(9) -0.0037(9) C21 0.0328(13) 0.0427(15) 0.0216(11) 0.0014(11) 0.0079(10) 0.0006(11) C22 0.0263(12) 0.0350(14) 0.0397(14) -0.0012(12) 0.0047(10) 0.0045(10) C23 0.0259(13) 0.0444(16) 0.0400(15) 0.0033(13) -0.0047(10) 0.0024(11) C24 0.0306(13) 0.0410(15) 0.0392(15) -0.0087(12) 0.0001(11) -0.0065(11) C25 0.0281(12) 0.0319(13) 0.0445(16) 0.0016(12) 0.0082(11) -0.0025(11) C26 0.0348(13) 0.0331(14) 0.0269(12) -0.0047(11) 0.0033(10) -0.0064(11) O27 0.0454(11) 0.0319(10) 0.0513(12) -0.0101(9) -0.0001(9) 0.0104(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2371(3) 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 Fe1 . Al2 . 2.3396(8) yes Fe1 . C19 . 1.746(3) yes Fe1 . C21 . 2.109(2) yes Fe1 . C22 . 2.087(2) yes Fe1 . C23 . 2.100(3) yes Fe1 . C24 . 2.107(3) yes Fe1 . C25 . 2.091(2) yes Fe1 . C26 . 1.749(3) yes Al2 . Cl3 . 2.1569(9) yes Al2 . N4 . 1.915(2) yes Al2 . C5 . 2.335(2) yes Al2 . N6 . 1.931(2) yes N4 . C5 . 1.337(3) yes N4 . C16 . 1.455(3) yes C5 . N6 . 1.340(3) yes C5 . C10 . 1.486(3) yes N6 . C7 . 1.454(3) yes C7 . C8 . 1.522(4) yes C7 . C9 . 1.523(4) yes C7 . H71 . 1.010 no C8 . H82 . 0.954 no C8 . H81 . 0.962 no C8 . H83 . 0.965 no C9 . H92 . 0.974 no C9 . H91 . 0.955 no C9 . H93 . 0.986 no C10 . C11 . 1.392(4) yes C10 . C15 . 1.392(4) yes C11 . C12 . 1.387(4) yes C11 . H111 . 0.927 no C12 . C13 . 1.375(4) yes C12 . H121 . 0.932 no C13 . C14 . 1.377(4) yes C13 . H131 . 0.950 no C14 . C15 . 1.391(4) yes C14 . H141 . 0.954 no C15 . H151 . 0.939 no C16 . C17 . 1.518(4) yes C16 . C18 . 1.517(4) yes C16 . H161 . 0.973 no C17 . H172 . 0.959 no C17 . H171 . 0.969 no C17 . H173 . 0.961 no C18 . H182 . 0.976 no C18 . H181 . 0.971 no C18 . H183 . 0.969 no C19 . O20 . 1.153(3) yes C21 . C22 . 1.413(4) yes C21 . C25 . 1.424(4) yes C21 . H211 . 0.982 no C22 . C23 . 1.439(4) yes C22 . H221 . 0.990 no C23 . C24 . 1.415(4) yes C23 . H231 . 0.996 no C24 . C25 . 1.420(4) yes C24 . H241 . 0.967 no C25 . H251 . 0.969 no C26 . O27 . 1.156(3) yes 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 Al2 . Fe1 . C19 . 82.12(8) yes Al2 . Fe1 . C21 . 86.95(8) yes C19 . Fe1 . C21 . 135.26(11) yes Al2 . Fe1 . C22 . 100.72(8) yes C19 . Fe1 . C22 . 100.69(11) yes C21 . Fe1 . C22 . 39.36(10) yes Al2 . Fe1 . C23 . 139.99(8) yes C19 . Fe1 . C23 . 95.40(11) yes C21 . Fe1 . C23 . 66.85(10) yes C22 . Fe1 . C23 . 40.20(11) yes Al2 . Fe1 . C24 . 151.05(8) yes C19 . Fe1 . C24 . 124.71(11) yes C21 . Fe1 . C24 . 66.54(11) yes C22 . Fe1 . C24 . 66.44(11) yes C23 . Fe1 . C24 . 39.31(11) yes Al2 . Fe1 . C25 . 111.94(8) yes C19 . Fe1 . C25 . 161.78(11) yes C21 . Fe1 . C25 . 39.63(10) yes C22 . Fe1 . C25 . 66.21(11) yes C23 . Fe1 . C25 . 66.39(11) yes Al2 . Fe1 . C26 . 80.66(8) yes C19 . Fe1 . C26 . 98.03(12) yes C21 . Fe1 . C26 . 122.80(11) yes C22 . Fe1 . C26 . 161.25(11) yes C23 . Fe1 . C26 . 138.74(12) yes C24 . Fe1 . C25 . 39.54(10) yes C24 . Fe1 . C26 . 103.43(11) yes C25 . Fe1 . C26 . 95.77(11) yes Fe1 . Al2 . Cl3 . 116.95(3) yes Fe1 . Al2 . N4 . 119.58(7) yes Cl3 . Al2 . N4 . 112.03(7) yes Fe1 . Al2 . C5 . 125.96(7) yes Cl3 . Al2 . C5 . 117.07(7) yes N4 . Al2 . C5 . 34.94(9) yes Fe1 . Al2 . N6 . 119.98(7) yes Cl3 . Al2 . N6 . 109.66(7) yes N4 . Al2 . N6 . 69.90(9) yes C5 . Al2 . N6 . 35.01(9) yes Al2 . N4 . C5 . 89.99(15) yes Al2 . N4 . C16 . 145.19(16) yes C5 . N4 . C16 . 124.8(2) yes Al2 . C5 . N4 . 55.07(12) yes Al2 . C5 . N6 . 55.75(12) yes N4 . C5 . N6 . 110.7(2) yes Al2 . C5 . C10 . 175.93(18) yes N4 . C5 . C10 . 124.4(2) yes N6 . C5 . C10 . 124.8(2) yes C5 . N6 . Al2 . 89.24(15) yes C5 . N6 . C7 . 124.6(2) yes Al2 . N6 . C7 . 145.92(16) yes N6 . C7 . C8 . 111.3(2) yes N6 . C7 . C9 . 108.5(2) yes C8 . C7 . C9 . 111.1(2) yes N6 . C7 . H71 . 108.2 no C8 . C7 . H71 . 108.6 no C9 . C7 . H71 . 109.1 no C7 . C8 . H82 . 110.0 no C7 . C8 . H81 . 110.5 no H82 . C8 . H81 . 108.1 no C7 . C8 . H83 . 110.1 no H82 . C8 . H83 . 109.4 no H81 . C8 . H83 . 108.6 no C7 . C9 . H92 . 111.8 no C7 . C9 . H91 . 109.0 no H92 . C9 . H91 . 109.3 no C7 . C9 . H93 . 109.5 no H92 . C9 . H93 . 111.0 no H91 . C9 . H93 . 106.1 no C5 . C10 . C11 . 119.5(2) yes C5 . C10 . C15 . 121.0(2) yes C11 . C10 . C15 . 119.4(2) yes C10 . C11 . C12 . 120.3(3) yes C10 . C11 . H111 . 120.0 no C12 . C11 . H111 . 119.8 no C11 . C12 . C13 . 120.1(3) yes C11 . C12 . H121 . 119.2 no C13 . C12 . H121 . 120.7 no C12 . C13 . C14 . 120.1(3) yes C12 . C13 . H131 . 119.8 no C14 . C13 . H131 . 120.0 no C13 . C14 . C15 . 120.6(3) yes C13 . C14 . H141 . 120.2 no C15 . C14 . H141 . 119.2 no C10 . C15 . C14 . 119.5(3) yes C10 . C15 . H151 . 120.5 no C14 . C15 . H151 . 119.9 no N4 . C16 . C17 . 110.4(2) yes N4 . C16 . C18 . 109.7(2) yes C17 . C16 . C18 . 110.5(2) yes N4 . C16 . H161 . 105.6 no C17 . C16 . H161 . 108.8 no C18 . C16 . H161 . 111.7 no C16 . C17 . H172 . 108.9 no C16 . C17 . H171 . 105.5 no H172 . C17 . H171 . 109.7 no C16 . C17 . H173 . 108.8 no H172 . C17 . H173 . 112.1 no H171 . C17 . H173 . 111.6 no C16 . C18 . H182 . 110.7 no C16 . C18 . H181 . 107.1 no H182 . C18 . H181 . 109.8 no C16 . C18 . H183 . 108.4 no H182 . C18 . H183 . 111.6 no H181 . C18 . H183 . 109.0 no Fe1 . C19 . O20 . 177.4(2) yes Fe1 . C21 . C22 . 69.46(14) yes Fe1 . C21 . C25 . 69.49(14) yes C22 . C21 . C25 . 107.1(2) yes Fe1 . C21 . H211 . 126.5 no C22 . C21 . H211 . 125.4 no C25 . C21 . H211 . 127.5 no Fe1 . C22 . C21 . 71.18(14) yes Fe1 . C22 . C23 . 70.39(14) yes C21 . C22 . C23 . 108.8(2) yes Fe1 . C22 . H221 . 124.8 no C21 . C22 . H221 . 126.3 no C23 . C22 . H221 . 124.9 no Fe1 . C23 . C22 . 69.41(14) yes Fe1 . C23 . C24 . 70.63(14) yes C22 . C23 . C24 . 107.2(2) yes Fe1 . C23 . H231 . 129.0 no C22 . C23 . H231 . 124.7 no C24 . C23 . H231 . 127.9 no Fe1 . C24 . C23 . 70.06(14) yes Fe1 . C24 . C25 . 69.60(14) yes C23 . C24 . C25 . 108.1(2) yes Fe1 . C24 . H241 . 123.8 no C23 . C24 . H241 . 126.3 no C25 . C24 . H241 . 125.6 no Fe1 . C25 . C21 . 70.88(14) yes Fe1 . C25 . C24 . 70.85(14) yes C21 . C25 . C24 . 108.8(2) yes Fe1 . C25 . H251 . 119.9 no C21 . C25 . H251 . 126.1 no C24 . C25 . H251 . 124.8 no Fe1 . C26 . O27 . 177.9(2) yes 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 C22 . H221 . O27 3_746 126 0.99 2.48 3.171(4) yes data_1a _database_code_depnum_ccdc_archive 'CCDC 894957' #TrackingRef 'Combined Final VRFs.cif' #============================================================================== _audit_creation_date 10-02-26 _audit_creation_method CRYSTALS_ver_14.03 _oxford_structure_analysis_title 022irdv10 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 18.7208(8) _cell_length_b 10.1409(4) _cell_length_c 12.0592(6) _cell_angle_alpha 90 _cell_angle_beta 91.8321(19) _cell_angle_gamma 90 _cell_volume 2288.22(18) _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' 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 = C23 H30 Al1 Cl2 N3 # Dc = 1.30 Fooo = 872.00 Mu = 3.37 M = 223.20 # Found Formula = C19 H36 Al1 Cl2 N3 # Dc = 1.17 FOOO = 872.00 Mu = 3.29 M = 202.20 _chemical_formula_sum 'C19 H36 Al1 Cl2 N3' _chemical_formula_moiety 'C19 H36 Al1 Cl2 N3' _chemical_compound_source ? _chemical_formula_weight 404.40 _cell_measurement_reflns_used 2593 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_min 0.210 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_max 0.490 _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.329 # Sheldrick geometric approximatio 0.93 0.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.93 # 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 11690 _reflns_number_total 2587 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections without Friedels Law is 2587 # Number of reflections with Friedels Law is 4983 # Theoretical number of reflections is about 2613 _diffrn_reflns_theta_min 5.185 _diffrn_reflns_theta_max 27.442 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.796 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -24 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 2.87 _oxford_diffrn_Wilson_scale 2.70 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.30 _refine_diff_density_max 0.33 # 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 2587 _refine_ls_number_restraints 0 _refine_ls_number_parameters 115 _oxford_refine_ls_R_factor_ref 0.0507 _refine_ls_wR_factor_ref 0.1077 _refine_ls_goodness_of_fit_ref 0.9841 _refine_ls_shift/su_max 0.0004896 # The values computed from all data _oxford_reflns_number_all 2587 _refine_ls_R_factor_all 0.0507 _refine_ls_wR_factor_all 0.1077 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2175 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_gt 0.1023 # 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^) + ( 0.04P)^2^ + 4.00P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order 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 0.43084(3) -0.25622(5) 0.34349(5) 0.0477 1.0000 Uani . . . . . . . Al2 Al 0.5000 -0.13642(7) 0.2500 0.0282 1.0000 Uani S T . . . . . C3 C 0.5000 0.0904(2) 0.2500 0.0214 1.0000 Uani S T . . . . . N4 N 0.45885(7) 0.01180(13) 0.18232(11) 0.0241 1.0000 Uani . . . . . . . C5 C 0.38576(8) 0.04233(17) 0.14086(13) 0.0260 1.0000 Uani . . . . . . . C6 C 0.36121(10) -0.0685(2) 0.06342(16) 0.0358 1.0000 Uani . . . . . . . C7 C 0.28491(10) -0.0429(3) 0.01880(17) 0.0466 1.0000 Uani . . . . . . . C8 C 0.23309(11) -0.0220(3) 0.11271(19) 0.0514 1.0000 Uani . . . . . . . C9 C 0.25832(10) 0.0875(3) 0.18989(19) 0.0489 1.0000 Uani . . . . . . . C10 C 0.33423(9) 0.0600(2) 0.23496(15) 0.0362 1.0000 Uani . . . . . . . N11 N 0.5000 0.22414(18) 0.2500 0.0237 1.0000 Uani S T . . . . . C12 C 0.48442(9) 0.29270(17) 0.14256(14) 0.0283 1.0000 Uani . . . . . . . C13 C 0.54935(11) 0.36419(19) 0.09858(16) 0.0372 1.0000 Uani . . . . . . . C14 C 0.41936(11) 0.3836(2) 0.14263(17) 0.0392 1.0000 Uani . . . . . . . H51 H 0.3838 0.1257 0.1030 0.0301 1.0000 Uiso R . . . . . . H61 H 0.3944 -0.0777 0.0008 0.0405 1.0000 Uiso R . . . . . . H62 H 0.3606 -0.1500 0.1079 0.0402 1.0000 Uiso R . . . . . . H71 H 0.2833 0.0340 -0.0306 0.0524 1.0000 Uiso R . . . . . . H72 H 0.2667 -0.1221 -0.0147 0.0536 1.0000 Uiso R . . . . . . H81 H 0.2274 -0.1075 0.1524 0.0569 1.0000 Uiso R . . . . . . H82 H 0.1889 0.0058 0.0736 0.0554 1.0000 Uiso R . . . . . . H91 H 0.2601 0.1681 0.1452 0.0546 1.0000 Uiso R . . . . . . H92 H 0.2245 0.0939 0.2528 0.0550 1.0000 Uiso R . . . . . . H101 H 0.3500 0.1325 0.2848 0.0419 1.0000 Uiso R . . . . . . H102 H 0.3321 -0.0208 0.2818 0.0406 1.0000 Uiso R . . . . . . H121 H 0.4724 0.2221 0.0886 0.0285 1.0000 Uiso R . . . . . . H131 H 0.5417 0.3852 0.0182 0.0556 1.0000 Uiso R . . . . . . H132 H 0.5549 0.4416 0.1457 0.0535 1.0000 Uiso R . . . . . . H133 H 0.5897 0.3016 0.1108 0.0542 1.0000 Uiso R . . . . . . H141 H 0.4037 0.4009 0.0691 0.0545 1.0000 Uiso R . . . . . . H142 H 0.4323 0.4662 0.1754 0.0569 1.0000 Uiso R . . . . . . H143 H 0.3817 0.3394 0.1829 0.0567 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(3) 0.0363(3) 0.0543(3) 0.0150(2) -0.0072(2) -0.0150(2) Al2 0.0302(4) 0.0205(3) 0.0335(4) 0.0000 -0.0066(3) 0.0000 C3 0.0184(10) 0.0225(10) 0.0234(10) 0.0000 0.0009(8) 0.0000 N4 0.0213(6) 0.0233(7) 0.0274(7) 0.0004(5) -0.0045(5) -0.0008(5) C5 0.0198(7) 0.0293(8) 0.0286(8) 0.0034(7) -0.0042(6) -0.0021(6) C6 0.0316(9) 0.0423(10) 0.0328(9) -0.0037(8) -0.0072(7) -0.0074(8) C7 0.0303(10) 0.0680(15) 0.0406(11) 0.0009(10) -0.0116(8) -0.0128(10) C8 0.0253(9) 0.0793(17) 0.0492(12) 0.0107(11) -0.0070(9) -0.0137(10) C9 0.0219(9) 0.0773(16) 0.0474(12) 0.0013(11) 0.0013(8) 0.0041(10) C10 0.0252(9) 0.0519(12) 0.0314(9) -0.0025(8) -0.0019(7) 0.0002(8) N11 0.0232(9) 0.0214(9) 0.0265(10) 0.0000 -0.0008(8) 0.0000 C12 0.0296(8) 0.0243(8) 0.0309(8) 0.0048(7) -0.0011(7) -0.0009(7) C13 0.0410(10) 0.0310(9) 0.0397(10) 0.0057(8) 0.0034(8) -0.0086(8) C14 0.0396(11) 0.0355(10) 0.0424(11) 0.0098(8) -0.0011(8) 0.0098(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.6326(17) 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 . 2.1253(6) yes Al2 . N4 5_655 1.8651(15) yes Al2 . C3 . 2.300(2) yes Al2 . N4 . 1.8651(15) yes C3 . N4 5_655 1.3620(18) yes C3 . N4 . 1.3620(18) yes C3 . N11 . 1.356(3) yes N4 . C5 . 1.474(2) yes C5 . C6 . 1.523(2) yes C5 . C10 . 1.523(2) yes C5 . H51 . 0.961 no C6 . C7 . 1.532(3) yes C6 . H61 . 0.997 no C6 . H62 . 0.985 no C7 . C8 . 1.529(3) yes C7 . H71 . 0.981 no C7 . H72 . 0.956 no C8 . C9 . 1.515(3) yes C8 . H81 . 0.998 no C8 . H82 . 0.981 no C9 . C10 . 1.531(3) yes C9 . H91 . 0.981 no C9 . H92 . 1.006 no C10 . H101 . 0.988 no C10 . H102 . 0.997 no N11 . C12 5_655 1.4910(19) yes N11 . C12 . 1.4910(19) yes C12 . C13 . 1.525(2) yes C12 . C14 . 1.527(2) yes C12 . H121 . 0.988 no C13 . H131 . 0.998 no C13 . H132 . 0.972 no C13 . H133 . 0.994 no C14 . H141 . 0.941 no C14 . H142 . 0.954 no C14 . H143 . 0.978 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 N4 5_655 Al2 . Cl1 . 118.60(5) yes N4 5_655 Al2 . Cl1 5_655 116.27(5) yes Cl1 . Al2 . Cl1 5_655 110.27(4) yes N4 5_655 Al2 . C3 . 36.30(4) yes Cl1 . Al2 . C3 . 124.87(2) yes Cl1 5_655 Al2 . C3 . 124.87(2) yes N4 5_655 Al2 . N4 . 72.61(8) yes Cl1 . Al2 . N4 . 116.27(5) yes Cl1 5_655 Al2 . N4 . 118.60(5) yes C3 . Al2 . N4 . 36.30(4) yes Al2 . C3 . N4 5_655 54.17(9) yes Al2 . C3 . N4 . 54.17(9) yes N4 5_655 C3 . N4 . 108.35(19) yes Al2 . C3 . N11 . 179.992 yes N4 5_655 C3 . N11 . 125.83(9) yes N4 . C3 . N11 . 125.83(9) yes C3 . N4 . Al2 . 89.52(10) yes C3 . N4 . C5 . 125.54(13) yes Al2 . N4 . C5 . 133.11(11) yes N4 . C5 . C6 . 108.16(14) yes N4 . C5 . C10 . 112.03(13) yes C6 . C5 . C10 . 110.97(15) yes N4 . C5 . H51 . 111.5 no C6 . C5 . H51 . 110.6 no C10 . C5 . H51 . 103.6 no C5 . C6 . C7 . 110.50(17) yes C5 . C6 . H61 . 110.5 no C7 . C6 . H61 . 110.3 no C5 . C6 . H62 . 107.1 no C7 . C6 . H62 . 107.8 no H61 . C6 . H62 . 110.6 no C6 . C7 . C8 . 111.69(16) yes C6 . C7 . H71 . 110.9 no C8 . C7 . H71 . 109.4 no C6 . C7 . H72 . 108.8 no C8 . C7 . H72 . 101.7 no H71 . C7 . H72 . 114.1 no C7 . C8 . C9 . 111.34(17) yes C7 . C8 . H81 . 108.4 no C9 . C8 . H81 . 112.2 no C7 . C8 . H82 . 103.2 no C9 . C8 . H82 . 109.0 no H81 . C8 . H82 . 112.3 no C8 . C9 . C10 . 110.64(19) yes C8 . C9 . H91 . 106.8 no C10 . C9 . H91 . 107.4 no C8 . C9 . H92 . 108.6 no C10 . C9 . H92 . 110.1 no H91 . C9 . H92 . 113.2 no C9 . C10 . C5 . 111.09(15) yes C9 . C10 . H101 . 109.7 no C5 . C10 . H101 . 110.9 no C9 . C10 . H102 . 107.3 no C5 . C10 . H102 . 111.3 no H101 . C10 . H102 . 106.5 no C12 5_655 N11 . C3 . 117.80(9) yes C12 5_655 N11 . C12 . 124.40(19) yes C3 . N11 . C12 . 117.80(9) yes N11 . C12 . C13 . 112.82(14) yes N11 . C12 . C14 . 114.51(14) yes C13 . C12 . C14 . 110.97(15) yes N11 . C12 . H121 . 105.6 no C13 . C12 . H121 . 106.4 no C14 . C12 . H121 . 105.8 no C12 . C13 . H131 . 110.3 no C12 . C13 . H132 . 104.6 no H131 . C13 . H132 . 113.9 no C12 . C13 . H133 . 104.8 no H131 . C13 . H133 . 111.4 no H132 . C13 . H133 . 111.3 no C12 . C14 . H141 . 109.6 no C12 . C14 . H142 . 109.7 no H141 . C14 . H142 . 107.1 no C12 . C14 . H143 . 108.2 no H141 . C14 . H143 . 110.3 no H142 . C14 . H143 . 112.0 no data_1c _database_code_depnum_ccdc_archive 'CCDC 894958' #TrackingRef 'Combined Final VRFs.cif' #============================================================================== _audit_creation_date 11-12-05 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title '12051505 004juct10' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 13.4052(3) _cell_length_b 11.0555(2) _cell_length_c 11.9482(2) _cell_angle_alpha 90 _cell_angle_beta 113.5072(9) _cell_angle_gamma 90 _cell_volume 1623.78(6) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _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' 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 = C13 Cl3 N2 # Dc = 1.19 Fooo = 632.00 Mu = 5.48 M = 145.26 # Found Formula = C13 H19 Al1 Cl2 N2 # Dc = 1.23 FOOO = 632.00 Mu = 4.40 M = 150.60 _chemical_formula_sum 'C13 H19 Al1 Cl2 N2' _chemical_formula_moiety 'C13 H19 Al1 Cl2 N2' _chemical_compound_source . _chemical_formula_weight 301.19 _cell_measurement_reflns_used 1894 _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 0.360 _exptl_crystal_size_mid 0.380 _exptl_crystal_size_max 0.740 _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.440 # Sheldrick geometric approximatio 0.85 0.85 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.85 # 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 10036 _reflns_number_total 1845 _diffrn_reflns_av_R_equivalents 0.011 # Number of reflections without Friedels Law is 3515 # Number of reflections with Friedels Law is 1845 # Theoretical number of reflections is about 1864 _diffrn_reflns_theta_min 5.219 _diffrn_reflns_theta_max 27.492 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.942 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -17 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 2.74 _oxford_diffrn_Wilson_scale 0.62 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.32 _refine_diff_density_max 0.32 # 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 1845 _refine_ls_number_restraints 4 _refine_ls_number_parameters 86 _oxford_refine_ls_R_factor_ref 0.0349 _refine_ls_wR_factor_ref 0.0884 _refine_ls_goodness_of_fit_ref 0.8663 _refine_ls_shift/su_max 0.0002415 _refine_ls_shift/su_mean 0.0000273 # The values computed from all data _oxford_reflns_number_all 1845 _refine_ls_R_factor_all 0.0349 _refine_ls_wR_factor_all 0.0884 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1683 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_gt 0.0835 # 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: 93.6 153. 91.4 37.9 9.14 ; # Insert your own references if required - in alphabetical order 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 Cl1 Cl 0.40548(3) -0.23552(3) 0.59891(3) 0.0433 1.0000 Uani . . . . . . Al2 Al 0.5000 -0.12766(5) 0.7500 0.0278 1.0000 Uani S T . . . . N3 N 0.56697(9) 0.01083(10) 0.71910(10) 0.0279 1.0000 Uani . . . . . . C4 C 0.5000 0.07972(16) 0.7500 0.0238 1.0000 Uani S T . . . . C5 C 0.5000 0.21400(15) 0.7500 0.0226 1.0000 Uani S T . . . . C6 C 0.52213(11) 0.27650(12) 0.85813(12) 0.0284 1.0000 Uani . . . . . . C7 C 0.52273(11) 0.40234(13) 0.85737(13) 0.0337 1.0000 Uani . . . . . . C8 C 0.500000(7) 0.46457(17) 0.750000(7) 0.0341 1.0000 Uani S T . . . . C9 C 0.66461(10) 0.05491(13) 0.70449(12) 0.0291 1.0000 Uani . . . . . . C10 C 0.75929(12) 0.06722(17) 0.82784(14) 0.0427 1.0000 Uani . . . . . . C11 C 0.68984(13) -0.03107(16) 0.62031(15) 0.0421 1.0000 Uani . . . . . . H61 H 0.5402 0.2412 0.9340 0.0339 1.0000 Uiso R . . . . . H71 H 0.5361 0.4398 0.9278 0.0396 1.0000 Uiso R . . . . . H81 H 0.5000 0.5535 0.7500 0.0428 1.0000 Uiso RS . . . . . H91 H 0.6489 0.1341 0.6645 0.0379 1.0000 Uiso R . . . . . H103 H 0.8223 0.0988 0.8163 0.0637 1.0000 Uiso R . . . . . H102 H 0.7745 -0.0088 0.8625 0.0657 1.0000 Uiso R . . . . . H101 H 0.7454 0.1201 0.8873 0.0647 1.0000 Uiso R . . . . . H113 H 0.7466 0.0042 0.5994 0.0605 1.0000 Uiso R . . . . . H112 H 0.7083 -0.1106 0.6579 0.0610 1.0000 Uiso R . . . . . H111 H 0.6263 -0.0341 0.5458 0.0615 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 0.0569(3) 0.0335(2) 0.0308(2) -0.00298(13) 0.00822(16) -0.00800(15) Al2 0.0339(3) 0.0224(3) 0.0277(3) 0.0000 0.0128(2) 0.0000 N3 0.0289(5) 0.0256(5) 0.0335(6) -0.0020(4) 0.0170(4) 0.0005(4) C4 0.0244(7) 0.0249(8) 0.0224(7) 0.0000 0.0097(6) 0.0000 C5 0.0216(7) 0.0228(8) 0.0246(8) 0.0000 0.0105(6) 0.0000 C6 0.0311(6) 0.0311(6) 0.0235(6) -0.0014(5) 0.0115(5) 0.0008(5) C7 0.0334(7) 0.0318(7) 0.0360(7) -0.0107(5) 0.0141(5) -0.0010(5) C8 0.0285(9) 0.0233(8) 0.0509(11) 0.0000 0.0162(8) 0.0000 C9 0.0267(6) 0.0331(6) 0.0316(6) -0.0016(5) 0.0161(5) 0.0005(5) C10 0.0324(7) 0.0591(10) 0.0368(7) -0.0086(7) 0.0139(6) -0.0047(7) C11 0.0394(8) 0.0517(9) 0.0424(8) -0.0102(7) 0.0238(7) 0.0021(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.044(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 Cl1 . Al2 . 2.1122(5) yes Al2 . N3 6_656 1.8843(12) yes Al2 . N3 . 1.8843(12) yes Al2 . C4 . 2.2927(18) yes N3 . C4 . 1.3367(14) yes N3 . C9 . 1.4708(16) yes C4 . C5 . 1.485(2) yes C5 . C6 6_656 1.3888(15) yes C5 . C6 . 1.3888(15) yes C6 . C7 . 1.3913(19) yes C6 . H61 . 0.926 no C7 . C8 . 1.3784(18) yes C7 . H71 . 0.889 no C8 . H81 . 0.983 no C9 . C10 . 1.520(2) yes C9 . C11 . 1.5169(19) yes C9 . H91 . 0.979 no C10 . H103 . 0.974 no C10 . H102 . 0.923 no C10 . H101 . 0.994 no C11 . H113 . 0.973 no C11 . H112 . 0.973 no C11 . H111 . 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 N3 6_656 Al2 . Cl1 6_656 117.48(4) yes N3 6_656 Al2 . Cl1 . 117.12(4) yes Cl1 6_656 Al2 . Cl1 . 111.26(3) yes N3 6_656 Al2 . N3 . 71.32(7) yes Cl1 6_656 Al2 . N3 . 117.12(4) yes Cl1 . Al2 . N3 . 117.48(4) yes N3 6_656 Al2 . C4 . 35.66(3) yes Cl1 6_656 Al2 . C4 . 124.370(16) yes Cl1 . Al2 . C4 . 124.370(16) yes N3 . Al2 . C4 . 35.66(3) yes Al2 . N3 . C4 . 89.08(8) yes Al2 . N3 . C9 . 143.95(9) yes C4 . N3 . C9 . 124.85(11) yes Al2 . C4 . N3 . 55.26(8) yes Al2 . C4 . N3 6_656 55.26(8) yes N3 . C4 . N3 6_656 110.53(15) yes Al2 . C4 . C5 . 179.992 yes N3 . C4 . C5 . 124.74(8) yes N3 6_656 C4 . C5 . 124.74(8) yes C4 . C5 . C6 6_656 119.83(8) yes C4 . C5 . C6 . 119.83(8) yes C6 6_656 C5 . C6 . 120.33(16) yes C5 . C6 . C7 . 119.41(13) yes C5 . C6 . H61 . 125.2 no C7 . C6 . H61 . 115.3 no C6 . C7 . C8 . 120.36(13) yes C6 . C7 . H71 . 117.3 no C8 . C7 . H71 . 122.3 no C7 . C8 . C7 6_656 120.12(18) yes C7 . C8 . H81 . 119.9 no C7 6_656 C8 . H81 . 119.9 no N3 . C9 . C10 . 110.68(11) yes N3 . C9 . C11 . 108.38(11) yes C10 . C9 . C11 . 112.23(12) yes N3 . C9 . H91 . 109.0 no C10 . C9 . H91 . 109.1 no C11 . C9 . H91 . 107.3 no C9 . C10 . H103 . 109.3 no C9 . C10 . H102 . 107.7 no H103 . C10 . H102 . 110.0 no C9 . C10 . H101 . 115.1 no H103 . C10 . H101 . 108.1 no H102 . C10 . H101 . 106.6 no C9 . C11 . H113 . 108.9 no C9 . C11 . H112 . 110.1 no H113 . C11 . H112 . 113.6 no C9 . C11 . H111 . 106.8 no H113 . C11 . H111 . 105.8 no H112 . C11 . H111 . 111.5 no _iucr_refine_instruction_details_constraints ; # # Punched on 05/12/11 at 15:23:47 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 103,X'S) H ( 102,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 113,X'S) H ( 112,X'S) H ( 111,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 05/12/11 at 15:23:47 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; data_2a _database_code_depnum_ccdc_archive 'CCDC 894959' #TrackingRef 'Combined Final VRFs.cif' #============================================================================== _audit_creation_date 09-12-18 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title '12181918 131irdv09' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 9.8974(6) _cell_length_b 11.2803(6) _cell_length_c 12.8172(8) _cell_angle_alpha 81.952(3) _cell_angle_beta 83.391(3) _cell_angle_gamma 82.656(2) _cell_volume 1398.37(14) _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' 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' 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' 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' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 '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' _cell_formula_units_Z 2 # Given Formula = C26 H30 Al1 Cl1 Fe1 N2 O2 # Dc = 1.24 Fooo = 580.00 Mu = 6.89 M = 520.82 # Found Formula = C26 H41 Al1 Cl1 Fe1 N3 O2 # Dc = 1.30 FOOO = 580.00 Mu = 6.93 M = 545.91 _chemical_formula_sum 'C26 H41 Al1 Cl1 Fe1 N3 O2' _chemical_formula_moiety 'C26 H41 Al1 Cl1 Fe1 N3 O2' _chemical_compound_source . _chemical_formula_weight 545.91 _cell_measurement_reflns_used 5505 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.23 _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 0.693 # Sheldrick geometric approximatio 0.92 0.97 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.88 _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 '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 20032 _reflns_number_total 6368 _diffrn_reflns_av_R_equivalents 0.082 # Number of reflections with Friedels Law is 6368 # Number of reflections without Friedels Law is 10129 # Theoretical number of reflections is about 6476 _diffrn_reflns_theta_min 5.191 _diffrn_reflns_theta_max 27.579 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.751 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 1.99 _oxford_diffrn_Wilson_scale 11.34 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.88 _refine_diff_density_max 1.05 # 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 6368 _refine_ls_number_restraints 0 _refine_ls_number_parameters 307 _oxford_refine_ls_R_factor_ref 0.1082 _refine_ls_wR_factor_ref 0.1224 _refine_ls_goodness_of_fit_ref 0.9833 _refine_ls_shift/su_max 0.000179 # The values computed from all data _oxford_reflns_number_all 6368 _refine_ls_R_factor_all 0.1082 _refine_ls_wR_factor_all 0.1224 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4269 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_gt 0.1047 # 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 noref # 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^) + ( 0.01P)^2^ + 2.65P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order 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 Fe1 Fe 0.21687(5) 0.07292(4) 0.36483(4) 0.0267 1.0000 Uani . . . . . . . Al2 Al 0.29621(10) 0.21348(8) 0.22373(8) 0.0246 1.0000 Uani . . . . . . . Cl3 Cl 0.19040(10) 0.21601(8) 0.08559(7) 0.0385 1.0000 Uani . . . . . . . N4 N 0.3206(3) 0.3695(2) 0.2538(2) 0.0234 1.0000 Uani . . . . . . . C5 C 0.4554(3) 0.3497(3) 0.2243(2) 0.0247 1.0000 Uani . . . . . . . N6 N 0.4842(3) 0.2414(2) 0.1883(2) 0.0264 1.0000 Uani . . . . . . . C7 C 0.6219(3) 0.1767(3) 0.1786(3) 0.0272 1.0000 Uani . . . . . . . C8 C 0.6371(4) 0.0676(3) 0.2628(3) 0.0340 1.0000 Uani . . . . . . . C9 C 0.7804(4) -0.0010(3) 0.2518(3) 0.0396 1.0000 Uani . . . . . . . C10 C 0.8143(4) -0.0386(3) 0.1421(3) 0.0433 1.0000 Uani . . . . . . . C11 C 0.8006(4) 0.0684(4) 0.0572(3) 0.0467 1.0000 Uani . . . . . . . C12 C 0.6571(4) 0.1379(3) 0.0685(3) 0.0400 1.0000 Uani . . . . . . . N13 N 0.5510(3) 0.4274(2) 0.2309(2) 0.0252 1.0000 Uani . . . . . . . C14 C 0.6379(4) 0.4633(3) 0.1332(3) 0.0297 1.0000 Uani . . . . . . . C15 C 0.7887(4) 0.4612(4) 0.1471(3) 0.0396 1.0000 Uani . . . . . . . C16 C 0.5809(4) 0.5860(3) 0.0776(3) 0.0402 1.0000 Uani . . . . . . . C17 C 0.5515(3) 0.4725(3) 0.3339(3) 0.0281 1.0000 Uani . . . . . . . C18 C 0.5622(4) 0.6070(3) 0.3282(3) 0.0385 1.0000 Uani . . . . . . . C19 C 0.6625(4) 0.3975(4) 0.3970(3) 0.0414 1.0000 Uani . . . . . . . C20 C 0.2480(3) 0.4892(3) 0.2655(3) 0.0247 1.0000 Uani . . . . . . . C21 C 0.1696(4) 0.4907(3) 0.3749(3) 0.0313 1.0000 Uani . . . . . . . C22 C 0.0960(4) 0.6160(3) 0.3875(3) 0.0380 1.0000 Uani . . . . . . . C23 C -0.0001(4) 0.6577(3) 0.3026(4) 0.0446 1.0000 Uani . . . . . . . C24 C 0.0732(4) 0.6530(3) 0.1933(3) 0.0435 1.0000 Uani . . . . . . . C25 C 0.1508(4) 0.5287(3) 0.1802(3) 0.0348 1.0000 Uani . . . . . . . C26 C 0.2987(4) -0.0604(3) 0.2693(3) 0.0353 1.0000 Uani . . . . . . . C27 C 0.1535(4) -0.0500(3) 0.2784(3) 0.0330 1.0000 Uani . . . . . . . C28 C 0.1066(4) -0.0779(3) 0.3879(3) 0.0343 1.0000 Uani . . . . . . . C29 C 0.2211(4) -0.1034(3) 0.4450(3) 0.0350 1.0000 Uani . . . . . . . C30 C 0.3404(4) -0.0927(3) 0.3724(3) 0.0369 1.0000 Uani . . . . . . . C31 C 0.0752(4) 0.1805(3) 0.3601(3) 0.0307 1.0000 Uani . . . . . . . O32 O -0.0223(3) 0.2487(2) 0.3560(2) 0.0433 1.0000 Uani . . . . . . . C33 C 0.3076(4) 0.1462(3) 0.4403(3) 0.0353 1.0000 Uani . . . . . . . O34 O 0.3698(3) 0.1920(2) 0.4904(2) 0.0513 1.0000 Uani . . . . . . . H71 H 0.6883 0.2312 0.1890 0.0340 1.0000 Uiso . . . . . . . H82 H 0.6156 0.0940 0.3343 0.0404 1.0000 Uiso . . . . . . . H81 H 0.5691 0.0140 0.2547 0.0399 1.0000 Uiso . . . . . . . H91 H 0.8478 0.0505 0.2633 0.0490 1.0000 Uiso . . . . . . . H92 H 0.7862 -0.0741 0.3052 0.0491 1.0000 Uiso . . . . . . . H101 H 0.9074 -0.0812 0.1355 0.0529 1.0000 Uiso . . . . . . . H102 H 0.7507 -0.0964 0.1316 0.0531 1.0000 Uiso . . . . . . . H111 H 0.8698 0.1235 0.0638 0.0560 1.0000 Uiso . . . . . . . H112 H 0.8184 0.0420 -0.0136 0.0562 1.0000 Uiso . . . . . . . H121 H 0.6509 0.2108 0.0143 0.0472 1.0000 Uiso . . . . . . . H122 H 0.5893 0.0862 0.0550 0.0472 1.0000 Uiso . . . . . . . H141 H 0.6321 0.4036 0.0833 0.0358 1.0000 Uiso . . . . . . . H153 H 0.8405 0.4764 0.0787 0.0628 1.0000 Uiso . . . . . . . H152 H 0.7995 0.5219 0.1898 0.0629 1.0000 Uiso . . . . . . . H151 H 0.8245 0.3822 0.1815 0.0631 1.0000 Uiso . . . . . . . H162 H 0.6241 0.5996 0.0060 0.0631 1.0000 Uiso . . . . . . . H161 H 0.5997 0.6503 0.1153 0.0631 1.0000 Uiso . . . . . . . H163 H 0.4836 0.5899 0.0754 0.0628 1.0000 Uiso . . . . . . . H171 H 0.4623 0.4575 0.3750 0.0381 1.0000 Uiso . . . . . . . H182 H 0.5520 0.6290 0.4001 0.0633 1.0000 Uiso . . . . . . . H181 H 0.6514 0.6255 0.2947 0.0629 1.0000 Uiso . . . . . . . H183 H 0.4911 0.6535 0.2891 0.0630 1.0000 Uiso . . . . . . . H192 H 0.6522 0.4158 0.4687 0.0669 1.0000 Uiso . . . . . . . H193 H 0.7520 0.4153 0.3647 0.0669 1.0000 Uiso . . . . . . . H191 H 0.6559 0.3122 0.3978 0.0669 1.0000 Uiso . . . . . . . H201 H 0.3177 0.5470 0.2584 0.0310 1.0000 Uiso . . . . . . . H212 H 0.2319 0.4635 0.4309 0.0403 1.0000 Uiso . . . . . . . H211 H 0.1006 0.4339 0.3820 0.0400 1.0000 Uiso . . . . . . . H222 H 0.1645 0.6725 0.3823 0.0488 1.0000 Uiso . . . . . . . H221 H 0.0456 0.6167 0.4587 0.0492 1.0000 Uiso . . . . . . . H232 H -0.0424 0.7412 0.3097 0.0572 1.0000 Uiso . . . . . . . H231 H -0.0727 0.6054 0.3116 0.0569 1.0000 Uiso . . . . . . . H241 H 0.1406 0.7131 0.1812 0.0541 1.0000 Uiso . . . . . . . H242 H 0.0082 0.6741 0.1401 0.0539 1.0000 Uiso . . . . . . . H252 H 0.2044 0.5299 0.1100 0.0431 1.0000 Uiso . . . . . . . H251 H 0.0859 0.4703 0.1842 0.0430 1.0000 Uiso . . . . . . . H261 H 0.3599 -0.0450 0.2024 0.0482 1.0000 Uiso . . . . . . . H271 H 0.0940 -0.0281 0.2175 0.0420 1.0000 Uiso . . . . . . . H281 H 0.0100 -0.0782 0.4193 0.0442 1.0000 Uiso . . . . . . . H291 H 0.2204 -0.1241 0.5233 0.0430 1.0000 Uiso . . . . . . . H301 H 0.4364 -0.1044 0.3921 0.0470 1.0000 Uiso . . . . . . . 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 Fe1 0.0285(3) 0.0197(2) 0.0321(3) -0.00292(19) -0.0037(2) -0.00362(19) Al2 0.0249(6) 0.0193(5) 0.0297(5) -0.0048(4) -0.0021(4) -0.0020(4) Cl3 0.0442(6) 0.0401(5) 0.0347(5) -0.0025(4) -0.0110(4) -0.0135(4) N4 0.0204(15) 0.0193(13) 0.0297(15) -0.0037(11) 0.0006(12) -0.0009(11) C5 0.0292(19) 0.0213(15) 0.0227(16) 0.0004(12) -0.0038(14) -0.0018(13) N6 0.0261(16) 0.0187(13) 0.0338(15) -0.0082(11) 0.0006(13) 0.0013(11) C7 0.0245(18) 0.0240(16) 0.0336(18) -0.0089(14) -0.0017(15) -0.0005(13) C8 0.030(2) 0.0335(19) 0.036(2) -0.0058(15) -0.0025(16) 0.0044(15) C9 0.035(2) 0.036(2) 0.047(2) -0.0091(17) -0.0104(18) 0.0091(16) C10 0.034(2) 0.038(2) 0.057(3) -0.0187(19) -0.0050(19) 0.0112(17) C11 0.047(3) 0.046(2) 0.044(2) -0.0173(19) 0.006(2) 0.0105(19) C12 0.039(2) 0.041(2) 0.037(2) -0.0114(17) 0.0002(18) 0.0085(17) N13 0.0226(15) 0.0256(14) 0.0291(15) -0.0067(11) -0.0029(12) -0.0050(11) C14 0.028(2) 0.0321(18) 0.0287(18) -0.0033(14) -0.0002(15) -0.0051(15) C15 0.026(2) 0.055(2) 0.039(2) -0.0099(18) 0.0023(17) -0.0129(18) C16 0.052(3) 0.035(2) 0.034(2) 0.0028(16) -0.0048(19) -0.0132(18) C17 0.0250(19) 0.0303(17) 0.0303(18) -0.0090(14) -0.0039(15) -0.0018(14) C18 0.038(2) 0.0334(19) 0.048(2) -0.0180(17) -0.0035(18) -0.0029(16) C19 0.040(2) 0.049(2) 0.036(2) -0.0105(17) -0.0101(18) 0.0014(18) C20 0.0240(18) 0.0181(15) 0.0322(18) -0.0047(13) -0.0017(14) -0.0020(13) C21 0.037(2) 0.0217(16) 0.0347(19) -0.0082(14) 0.0054(16) -0.0030(14) C22 0.034(2) 0.0301(18) 0.051(2) -0.0177(17) 0.0042(18) -0.0031(16) C23 0.030(2) 0.0303(19) 0.077(3) -0.023(2) -0.007(2) 0.0042(16) C24 0.044(2) 0.0314(19) 0.057(3) -0.0099(18) -0.020(2) 0.0079(17) C25 0.035(2) 0.0288(18) 0.041(2) -0.0064(15) -0.0090(17) 0.0017(15) C26 0.036(2) 0.0231(17) 0.047(2) -0.0107(15) 0.0017(18) -0.0021(15) C27 0.036(2) 0.0227(17) 0.043(2) -0.0087(15) -0.0065(17) -0.0053(15) C28 0.036(2) 0.0182(16) 0.049(2) -0.0028(15) 0.0008(18) -0.0090(14) C29 0.041(2) 0.0224(17) 0.040(2) 0.0021(15) -0.0045(18) -0.0041(15) C30 0.038(2) 0.0206(17) 0.053(2) -0.0015(16) -0.0120(19) -0.0022(15) C31 0.029(2) 0.0251(17) 0.038(2) -0.0064(15) 0.0040(16) -0.0090(15) O32 0.0321(15) 0.0306(13) 0.0643(18) -0.0072(12) 0.0023(13) 0.0030(12) C33 0.043(2) 0.0302(18) 0.0315(19) 0.0025(15) -0.0115(18) -0.0002(16) O34 0.067(2) 0.0450(16) 0.0494(17) -0.0079(13) -0.0247(16) -0.0153(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3088(3) 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 Fe1 . Al2 . 2.3644(11) yes Fe1 . C26 . 2.096(3) yes Fe1 . C27 . 2.087(3) yes Fe1 . C28 . 2.105(3) yes Fe1 . C29 . 2.105(3) yes Fe1 . C30 . 2.095(3) yes Fe1 . C31 . 1.733(4) yes Fe1 . C33 . 1.743(4) yes Al2 . Cl3 . 2.1534(13) yes Al2 . N4 . 1.904(3) yes Al2 . N6 . 1.919(3) yes N4 . C5 . 1.343(4) yes N4 . C20 . 1.465(4) yes C5 . N6 . 1.351(4) yes C5 . N13 . 1.386(4) yes N6 . C7 . 1.463(4) yes C7 . C8 . 1.523(5) yes C7 . C12 . 1.524(5) yes C7 . H71 . 0.987 no C8 . C9 . 1.527(5) yes C8 . H82 . 0.995 no C8 . H81 . 0.983 no C9 . C10 . 1.514(5) yes C9 . H91 . 0.975 no C9 . H92 . 0.996 no C10 . C11 . 1.512(6) yes C10 . H101 . 0.983 no C10 . H102 . 0.994 no C11 . C12 . 1.534(5) yes C11 . H111 . 0.999 no C11 . H112 . 0.984 no C12 . H121 . 1.000 no C12 . H122 . 0.988 no N13 . C14 . 1.474(4) yes N13 . C17 . 1.480(4) yes C14 . C15 . 1.520(5) yes C14 . C16 . 1.536(5) yes C14 . H141 . 1.003 no C15 . H153 . 0.969 no C15 . H152 . 0.958 no C15 . H151 . 0.980 no C16 . H162 . 0.967 no C16 . H161 . 0.973 no C16 . H163 . 0.961 no C17 . C18 . 1.526(5) yes C17 . C19 . 1.535(5) yes C17 . H171 . 0.996 no C18 . H182 . 0.979 no C18 . H181 . 0.970 no C18 . H183 . 0.967 no C19 . H192 . 0.961 no C19 . H193 . 0.967 no C19 . H191 . 0.971 no C20 . C21 . 1.524(5) yes C20 . C25 . 1.521(5) yes C20 . H201 . 0.997 no C21 . C22 . 1.526(5) yes C21 . H212 . 0.991 no C21 . H211 . 0.983 no C22 . C23 . 1.514(6) yes C22 . H222 . 0.979 no C22 . H221 . 0.989 no C23 . C24 . 1.506(6) yes C23 . H232 . 0.993 no C23 . H231 . 0.974 no C24 . C25 . 1.531(5) yes C24 . H241 . 0.995 no C24 . H242 . 0.976 no C25 . H252 . 0.990 no C25 . H251 . 0.970 no C26 . C27 . 1.420(5) yes C26 . C30 . 1.415(5) yes C26 . H261 . 0.999 no C27 . C28 . 1.431(5) yes C27 . H271 . 1.016 no C28 . C29 . 1.397(5) yes C28 . H281 . 0.994 no C29 . C30 . 1.424(5) yes C29 . H291 . 0.998 no C30 . H301 . 0.999 no C31 . O32 . 1.156(4) yes C33 . O34 . 1.151(4) yes 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 Al2 . Fe1 . C26 . 86.44(11) yes Al2 . Fe1 . C27 . 99.55(11) yes C26 . Fe1 . C27 . 39.67(14) yes Al2 . Fe1 . C28 . 138.55(11) yes C26 . Fe1 . C28 . 66.53(14) yes C27 . Fe1 . C28 . 39.91(14) yes Al2 . Fe1 . C29 . 151.04(11) yes C26 . Fe1 . C29 . 66.37(14) yes C27 . Fe1 . C29 . 66.16(14) yes C28 . Fe1 . C29 . 38.76(14) yes Al2 . Fe1 . C30 . 112.17(12) yes C26 . Fe1 . C30 . 39.46(14) yes C27 . Fe1 . C30 . 66.30(14) yes C28 . Fe1 . C30 . 65.97(14) yes C29 . Fe1 . C30 . 39.63(15) yes Al2 . Fe1 . C31 . 79.65(12) yes C26 . Fe1 . C31 . 133.33(16) yes C27 . Fe1 . C31 . 99.18(15) yes C28 . Fe1 . C31 . 96.16(15) yes C29 . Fe1 . C31 . 126.04(16) yes Al2 . Fe1 . C33 . 83.92(12) yes C26 . Fe1 . C33 . 126.42(16) yes C27 . Fe1 . C33 . 164.55(15) yes C28 . Fe1 . C33 . 137.31(16) yes C29 . Fe1 . C33 . 103.81(15) yes C30 . Fe1 . C31 . 162.04(15) yes C30 . Fe1 . C33 . 98.39(15) yes C31 . Fe1 . C33 . 96.25(16) yes Fe1 . Al2 . Cl3 . 111.59(5) yes Fe1 . Al2 . N4 . 118.28(9) yes Cl3 . Al2 . N4 . 113.74(9) yes Fe1 . Al2 . N6 . 124.68(9) yes Cl3 . Al2 . N6 . 112.42(10) yes N4 . Al2 . N6 . 70.28(11) yes Al2 . N4 . C5 . 90.44(19) yes Al2 . N4 . C20 . 142.8(2) yes C5 . N4 . C20 . 123.6(3) yes N4 . C5 . N6 . 109.5(3) yes N4 . C5 . N13 . 125.5(3) yes N6 . C5 . N13 . 125.0(3) yes C5 . N6 . Al2 . 89.6(2) yes C5 . N6 . C7 . 123.5(3) yes Al2 . N6 . C7 . 141.2(2) yes N6 . C7 . C8 . 111.5(3) yes N6 . C7 . C12 . 110.7(3) yes C8 . C7 . C12 . 110.2(3) yes N6 . C7 . H71 . 108.7 no C8 . C7 . H71 . 107.5 no C12 . C7 . H71 . 108.2 no C7 . C8 . C9 . 111.6(3) yes C7 . C8 . H82 . 109.5 no C9 . C8 . H82 . 110.7 no C7 . C8 . H81 . 108.2 no C9 . C8 . H81 . 109.3 no H82 . C8 . H81 . 107.4 no C8 . C9 . C10 . 110.7(3) yes C8 . C9 . H91 . 109.6 no C10 . C9 . H91 . 108.4 no C8 . C9 . H92 . 110.1 no C10 . C9 . H92 . 109.1 no H91 . C9 . H92 . 108.8 no C9 . C10 . C11 . 111.5(3) yes C9 . C10 . H101 . 109.9 no C11 . C10 . H101 . 110.4 no C9 . C10 . H102 . 109.1 no C11 . C10 . H102 . 108.8 no H101 . C10 . H102 . 107.0 no C10 . C11 . C12 . 111.0(3) yes C10 . C11 . H111 . 109.0 no C12 . C11 . H111 . 109.0 no C10 . C11 . H112 . 110.4 no C12 . C11 . H112 . 109.2 no H111 . C11 . H112 . 108.1 no C11 . C12 . C7 . 111.4(3) yes C11 . C12 . H121 . 110.2 no C7 . C12 . H121 . 109.2 no C11 . C12 . H122 . 109.1 no C7 . C12 . H122 . 109.6 no H121 . C12 . H122 . 107.2 no C5 . N13 . C14 . 117.2(3) yes C5 . N13 . C17 . 117.1(3) yes C14 . N13 . C17 . 125.6(3) yes N13 . C14 . C15 . 114.9(3) yes N13 . C14 . C16 . 111.2(3) yes C15 . C14 . C16 . 110.9(3) yes N13 . C14 . H141 . 106.9 no C15 . C14 . H141 . 106.7 no C16 . C14 . H141 . 105.6 no C14 . C15 . H153 . 110.0 no C14 . C15 . H152 . 109.4 no H153 . C15 . H152 . 109.4 no C14 . C15 . H151 . 110.4 no H153 . C15 . H151 . 108.3 no H152 . C15 . H151 . 109.4 no C14 . C16 . H162 . 110.5 no C14 . C16 . H161 . 109.8 no H162 . C16 . H161 . 107.8 no C14 . C16 . H163 . 110.7 no H162 . C16 . H163 . 109.0 no H161 . C16 . H163 . 108.9 no N13 . C17 . C18 . 115.6(3) yes N13 . C17 . C19 . 110.2(3) yes C18 . C17 . C19 . 111.1(3) yes N13 . C17 . H171 . 106.6 no C18 . C17 . H171 . 106.6 no C19 . C17 . H171 . 106.2 no C17 . C18 . H182 . 109.1 no C17 . C18 . H181 . 110.1 no H182 . C18 . H181 . 108.3 no C17 . C18 . H183 . 110.5 no H182 . C18 . H183 . 109.0 no H181 . C18 . H183 . 109.9 no C17 . C19 . H192 . 110.6 no C17 . C19 . H193 . 109.8 no H192 . C19 . H193 . 108.6 no C17 . C19 . H191 . 109.9 no H192 . C19 . H191 . 108.9 no H193 . C19 . H191 . 109.1 no N4 . C20 . C21 . 110.8(3) yes N4 . C20 . C25 . 111.0(3) yes C21 . C20 . C25 . 110.2(3) yes N4 . C20 . H201 . 107.8 no C21 . C20 . H201 . 107.9 no C25 . C20 . H201 . 109.1 no C20 . C21 . C22 . 110.6(3) yes C20 . C21 . H212 . 110.6 no C22 . C21 . H212 . 111.0 no C20 . C21 . H211 . 108.0 no C22 . C21 . H211 . 108.4 no H212 . C21 . H211 . 108.0 no C21 . C22 . C23 . 111.2(3) yes C21 . C22 . H222 . 108.6 no C23 . C22 . H222 . 109.2 no C21 . C22 . H221 . 110.4 no C23 . C22 . H221 . 110.5 no H222 . C22 . H221 . 106.7 no C22 . C23 . C24 . 111.6(3) yes C22 . C23 . H232 . 109.7 no C24 . C23 . H232 . 109.6 no C22 . C23 . H231 . 109.2 no C24 . C23 . H231 . 108.4 no H232 . C23 . H231 . 108.3 no C23 . C24 . C25 . 112.1(3) yes C23 . C24 . H241 . 108.4 no C25 . C24 . H241 . 108.2 no C23 . C24 . H242 . 110.2 no C25 . C24 . H242 . 109.3 no H241 . C24 . H242 . 108.5 no C24 . C25 . C20 . 111.1(3) yes C24 . C25 . H252 . 110.6 no C20 . C25 . H252 . 108.7 no C24 . C25 . H251 . 109.5 no C20 . C25 . H251 . 109.4 no H252 . C25 . H251 . 107.5 no Fe1 . C26 . C27 . 69.83(19) yes Fe1 . C26 . C30 . 70.2(2) yes C27 . C26 . C30 . 107.6(3) yes Fe1 . C26 . H261 . 123.8 no C27 . C26 . H261 . 126.0 no C30 . C26 . H261 . 126.3 no Fe1 . C27 . C26 . 70.51(19) yes Fe1 . C27 . C28 . 70.72(19) yes C26 . C27 . C28 . 107.9(3) yes Fe1 . C27 . H271 . 125.2 no C26 . C27 . H271 . 125.7 no C28 . C27 . H271 . 126.4 no Fe1 . C28 . C27 . 69.36(19) yes Fe1 . C28 . C29 . 70.6(2) yes C27 . C28 . C29 . 108.0(3) yes Fe1 . C28 . H281 . 124.9 no C27 . C28 . H281 . 126.9 no C29 . C28 . H281 . 125.1 no Fe1 . C29 . C28 . 70.65(19) yes Fe1 . C29 . C30 . 69.81(19) yes C28 . C29 . C30 . 108.3(3) yes Fe1 . C29 . H291 . 124.4 no C28 . C29 . H291 . 126.3 no C30 . C29 . H291 . 125.3 no Fe1 . C30 . C29 . 70.6(2) yes Fe1 . C30 . C26 . 70.33(19) yes C29 . C30 . C26 . 108.2(3) yes Fe1 . C30 . H301 . 123.8 no C29 . C30 . H301 . 125.2 no C26 . C30 . H301 . 126.6 no Fe1 . C31 . O32 . 177.2(3) yes Fe1 . C33 . O34 . 178.3(3) yes 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 C30 . H301 . O34 2_656 155 1.00 2.59 3.516(5) yes data_2b _database_code_depnum_ccdc_archive 'CCDC 894960' #TrackingRef 'Combined Final VRFs.cif' #============================================================================== _audit_creation_date 12-03-26 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title '7110911 Compound X' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.72890(10) _cell_length_b 15.4840(2) _cell_length_c 17.7812(3) _cell_angle_alpha 92.0036(7) _cell_angle_beta 92.5025(7) _cell_angle_gamma 100.7188(6) _cell_volume 2356.82(6) _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' 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' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 '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 = C20 H33 Al1 Cl0.25 Fe1 N3 O2 # Dc = 1.24 Fooo = 984.00 Mu = 7.23 M = 878.39 # Found Formula = C20 H33 Al1 Cl1 Fe1 N3 O2 # Dc = 1.31 FOOO = 984.00 Mu = 8.10 M = 931.56 _chemical_formula_sum 'C20 H33 Al1 Cl1 Fe1 N3 O2' _chemical_formula_moiety 'C20 H33 Al1 Cl1 Fe1 N3 O2' _chemical_compound_source ? _chemical_formula_weight 465.78 _cell_measurement_reflns_used 9687 _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 0.180 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.220 _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.810 # Sheldrick geometric approximatio 0.85 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.86 # 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 34511 _reflns_number_total 10737 _diffrn_reflns_av_R_equivalents 0.053 # Number of reflections without Friedels Law is 18335 # Number of reflections with Friedels Law is 10737 # Theoretical number of reflections is about 11056 _diffrn_reflns_theta_min 5.108 _diffrn_reflns_theta_max 27.571 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.193 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min -20 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 2.06 _oxford_diffrn_Wilson_scale 11.02 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.65 _refine_diff_density_max 1.05 # 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 10737 _refine_ls_number_restraints 0 _refine_ls_number_parameters 506 _oxford_refine_ls_R_factor_ref 0.0924 _refine_ls_wR_factor_ref 0.2072 _refine_ls_goodness_of_fit_ref 0.9869 _refine_ls_shift/su_max 0.0004435 _refine_ls_shift/su_mean 0.0000175 # The values computed from all data _oxford_reflns_number_all 10737 _refine_ls_R_factor_all 0.0924 _refine_ls_wR_factor_all 0.2072 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8511 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_gt 0.1886 # 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: 35.0 54.9 31.7 12.4 2.72 ; # Insert your own references if required - in alphabetical order 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 Fe101 Fe -0.19173(9) 0.92484(5) 0.85720(4) 0.0246 1.0000 Uani . . . . . . Al102 Al 0.02747(18) 0.92722(10) 0.78451(9) 0.0213 1.0000 Uani . . . . . . Cl103 Cl 0.23589(16) 1.01192(10) 0.83490(8) 0.0317 1.0000 Uani . . . . . . N104 N 0.0317(5) 0.9343(3) 0.6776(3) 0.0244 1.0000 Uani . . . . . . C105 C 0.0798(6) 0.8580(3) 0.6723(3) 0.0184 1.0000 Uani . . . . . . N106 N 0.0881(5) 0.8249(3) 0.7407(2) 0.0218 1.0000 Uani . . . . . . C107 C -0.0208(7) 0.9804(4) 0.6132(3) 0.0274 1.0000 Uani . . . . . . C108 C -0.1979(8) 0.9704(5) 0.6090(4) 0.0390 1.0000 Uani . . . . . . C109 C 0.0536(8) 1.0784(4) 0.6206(4) 0.0362 1.0000 Uani . . . . . . N110 N 0.1119(5) 0.8198(3) 0.6023(2) 0.0234 1.0000 Uani . . . . . . C111 C 0.0258(7) 0.7292(4) 0.5838(3) 0.0264 1.0000 Uani . . . . . . C112 C -0.1472(8) 0.7252(5) 0.5947(4) 0.0398 1.0000 Uani . . . . . . C113 C 0.0472(8) 0.7014(4) 0.5026(4) 0.0377 1.0000 Uani . . . . . . C114 C 0.2749(7) 0.8428(4) 0.5777(3) 0.0279 1.0000 Uani . . . . . . C115 C 0.3461(7) 0.9389(4) 0.5975(4) 0.0359 1.0000 Uani . . . . . . C116 C 0.3856(8) 0.7844(5) 0.6073(4) 0.0374 1.0000 Uani . . . . . . C117 C 0.1557(7) 0.7491(4) 0.7623(3) 0.0244 1.0000 Uani . . . . . . C118 C 0.0305(8) 0.6791(4) 0.7929(3) 0.0332 1.0000 Uani . . . . . . C119 C 0.2906(8) 0.7793(4) 0.8209(4) 0.0359 1.0000 Uani . . . . . . C120 C -0.3310(9) 1.0114(5) 0.8182(4) 0.0395 1.0000 Uani . . . . . . C121 C -0.3763(8) 0.9857(5) 0.8914(4) 0.0370 1.0000 Uani . . . . . . C122 C -0.2470(8) 1.0116(4) 0.9418(4) 0.0371 1.0000 Uani . . . . . . C123 C -0.1185(8) 1.0543(4) 0.9015(4) 0.0381 1.0000 Uani . . . . . . C124 C -0.1712(9) 1.0550(4) 0.8245(4) 0.0392 1.0000 Uani . . . . . . C125 C -0.0952(8) 0.8620(4) 0.9154(3) 0.0346 1.0000 Uani . . . . . . O126 O -0.0326(7) 0.8196(4) 0.9544(3) 0.0526 1.0000 Uani . . . . . . C127 C -0.2778(7) 0.8331(4) 0.7995(3) 0.0315 1.0000 Uani . . . . . . O128 O -0.3352(5) 0.7725(3) 0.7626(3) 0.0444 1.0000 Uani . . . . . . Fe1 Fe 0.34190(9) 0.43544(5) 0.63714(4) 0.0237 1.0000 Uani . . . . . . Al2 Al 0.56309(18) 0.42256(10) 0.71233(9) 0.0209 1.0000 Uani . . . . . . Cl3 Cl 0.77970(17) 0.48840(10) 0.66828(8) 0.0345 1.0000 Uani . . . . . . N4 N 0.5829(6) 0.4330(3) 0.8204(2) 0.0261 1.0000 Uani . . . . . . C5 C 0.6058(6) 0.3504(4) 0.8219(3) 0.0240 1.0000 Uani . . . . . . N6 N 0.5950(6) 0.3144(3) 0.7529(2) 0.0245 1.0000 Uani . . . . . . C7 C 0.5671(8) 0.4881(4) 0.8864(3) 0.0332 1.0000 Uani . . . . . . C8 C 0.4072(11) 0.5135(6) 0.8842(4) 0.0533 1.0000 Uani . . . . . . C9 C 0.6967(11) 0.5699(5) 0.8914(4) 0.0523 1.0000 Uani . . . . . . N10 N 0.6336(6) 0.3100(3) 0.8902(3) 0.0309 1.0000 Uani . . . . . . C11 C 0.5144(9) 0.2308(5) 0.9048(4) 0.0399 1.0000 Uani . . . . . . C12 C 0.3509(9) 0.2527(5) 0.8926(4) 0.0449 1.0000 Uani . . . . . . C13 C 0.5312(11) 0.2007(5) 0.9849(4) 0.0537 1.0000 Uani . . . . . . C14 C 0.7990(8) 0.3082(5) 0.9128(3) 0.0380 1.0000 Uani . . . . . . C15 C 0.9126(9) 0.3477(7) 0.8553(5) 0.0619 1.0000 Uani . . . . . . C16 C 0.8452(9) 0.3574(6) 0.9884(4) 0.0474 1.0000 Uani . . . . . . C17 C 0.6286(7) 0.2281(4) 0.7302(3) 0.0283 1.0000 Uani . . . . . . C18 C 0.7433(8) 0.2385(5) 0.6679(4) 0.0407 1.0000 Uani . . . . . . C19 C 0.4781(9) 0.1655(4) 0.7034(4) 0.0371 1.0000 Uani . . . . . . C20 C 0.4357(8) 0.5561(4) 0.5928(4) 0.0332 1.0000 Uani . . . . . . C21 C 0.2871(8) 0.5228(4) 0.5560(3) 0.0326 1.0000 Uani . . . . . . C22 C 0.1751(8) 0.5142(4) 0.6104(4) 0.0379 1.0000 Uani . . . . . . C23 C 0.2523(9) 0.5409(5) 0.6818(4) 0.0408 1.0000 Uani . . . . . . C24 C 0.4129(9) 0.5674(4) 0.6716(4) 0.0362 1.0000 Uani . . . . . . C25 C 0.2362(7) 0.3532(4) 0.6889(4) 0.0326 1.0000 Uani . . . . . . O26 O 0.1634(6) 0.2984(3) 0.7223(3) 0.0469 1.0000 Uani . . . . . . C27 C 0.4133(7) 0.3594(4) 0.5804(3) 0.0292 1.0000 Uani . . . . . . O28 O 0.4590(6) 0.3087(3) 0.5429(2) 0.0419 1.0000 Uani . . . . . . H1071 H 0.0106 0.9545 0.5663 0.0331 1.0000 Uiso . . . . . . H1083 H -0.2270 1.0023 0.5670 0.0590 1.0000 Uiso . . . . . . H1082 H -0.2306 0.9939 0.6547 0.0589 1.0000 Uiso . . . . . . H1081 H -0.2454 0.9091 0.6019 0.0591 1.0000 Uiso . . . . . . H1091 H 0.0207 1.1072 0.5775 0.0540 1.0000 Uiso . . . . . . H1092 H 0.0175 1.1037 0.6650 0.0543 1.0000 Uiso . . . . . . H1093 H 0.1657 1.0856 0.6241 0.0538 1.0000 Uiso . . . . . . H1111 H 0.0616 0.6869 0.6177 0.0321 1.0000 Uiso . . . . . . H1121 H -0.2006 0.6645 0.5912 0.0599 1.0000 Uiso . . . . . . H1122 H -0.1613 0.7507 0.6434 0.0600 1.0000 Uiso . . . . . . H1123 H -0.1891 0.7579 0.5565 0.0599 1.0000 Uiso . . . . . . H1131 H -0.0282 0.6491 0.4876 0.0568 1.0000 Uiso . . . . . . H1132 H 0.0333 0.7470 0.4689 0.0568 1.0000 Uiso . . . . . . H1133 H 0.1490 0.6882 0.4974 0.0571 1.0000 Uiso . . . . . . H1141 H 0.2691 0.8353 0.5222 0.0341 1.0000 Uiso . . . . . . H1151 H 0.4467 0.9527 0.5768 0.0539 1.0000 Uiso . . . . . . H1152 H 0.3572 0.9493 0.6517 0.0539 1.0000 Uiso . . . . . . H1153 H 0.2807 0.9767 0.5770 0.0539 1.0000 Uiso . . . . . . H1161 H 0.4818 0.7960 0.5821 0.0560 1.0000 Uiso . . . . . . H1162 H 0.4076 0.7963 0.6611 0.0553 1.0000 Uiso . . . . . . H1163 H 0.3379 0.7235 0.5980 0.0559 1.0000 Uiso . . . . . . H1171 H 0.1971 0.7250 0.7173 0.0279 1.0000 Uiso . . . . . . H1181 H 0.0754 0.6317 0.8111 0.0499 1.0000 Uiso . . . . . . H1182 H -0.0203 0.7038 0.8325 0.0496 1.0000 Uiso . . . . . . H1183 H -0.0456 0.6568 0.7528 0.0499 1.0000 Uiso . . . . . . H1193 H 0.3417 0.7310 0.8333 0.0542 1.0000 Uiso . . . . . . H1192 H 0.2502 0.8005 0.8660 0.0540 1.0000 Uiso . . . . . . H1191 H 0.3653 0.8258 0.8021 0.0537 1.0000 Uiso . . . . . . H1201 H -0.3979 1.0031 0.7726 0.0470 1.0000 Uiso . . . . . . H1211 H -0.4800 0.9549 0.9045 0.0439 1.0000 Uiso . . . . . . H1221 H -0.2455 1.0027 0.9959 0.0449 1.0000 Uiso . . . . . . H1231 H -0.0139 1.0791 0.9225 0.0460 1.0000 Uiso . . . . . . H1241 H -0.1104 1.0801 0.7831 0.0470 1.0000 Uiso . . . . . . H71 H 0.5773 0.4537 0.9317 0.0399 1.0000 Uiso . . . . . . H83 H 0.3937 0.5475 0.9288 0.0800 1.0000 Uiso . . . . . . H82 H 0.3270 0.4614 0.8809 0.0797 1.0000 Uiso . . . . . . H81 H 0.3943 0.5481 0.8411 0.0799 1.0000 Uiso . . . . . . H91 H 0.6857 0.6041 0.9362 0.0781 1.0000 Uiso . . . . . . H92 H 0.7966 0.5523 0.8939 0.0782 1.0000 Uiso . . . . . . H93 H 0.6879 0.6044 0.8481 0.0780 1.0000 Uiso . . . . . . H111 H 0.5262 0.1820 0.8691 0.0478 1.0000 Uiso . . . . . . H121 H 0.2735 0.2012 0.9005 0.0672 1.0000 Uiso . . . . . . H122 H 0.3406 0.2989 0.9284 0.0670 1.0000 Uiso . . . . . . H123 H 0.3366 0.2720 0.8423 0.0669 1.0000 Uiso . . . . . . H131 H 0.4569 0.1472 0.9911 0.0799 1.0000 Uiso . . . . . . H132 H 0.5130 0.2459 1.0201 0.0799 1.0000 Uiso . . . . . . H133 H 0.6355 0.1905 0.9943 0.0799 1.0000 Uiso . . . . . . H141 H 0.8093 0.2468 0.9191 0.0459 1.0000 Uiso . . . . . . H151 H 1.0156 0.3394 0.8709 0.0929 1.0000 Uiso . . . . . . H152 H 0.9109 0.4095 0.8522 0.0930 1.0000 Uiso . . . . . . H153 H 0.8815 0.3180 0.8069 0.0929 1.0000 Uiso . . . . . . H161 H 0.9510 0.3528 1.0030 0.0709 1.0000 Uiso . . . . . . H162 H 0.7758 0.3324 1.0259 0.0709 1.0000 Uiso . . . . . . H163 H 0.8385 0.4183 0.9838 0.0710 1.0000 Uiso . . . . . . H171 H 0.6749 0.2047 0.7743 0.0336 1.0000 Uiso . . . . . . H181 H 0.7582 0.1806 0.6519 0.0614 1.0000 Uiso . . . . . . H182 H 0.8414 0.2739 0.6863 0.0609 1.0000 Uiso . . . . . . H183 H 0.7007 0.2657 0.6259 0.0609 1.0000 Uiso . . . . . . H193 H 0.5025 0.1111 0.6843 0.0562 1.0000 Uiso . . . . . . H192 H 0.4125 0.1539 0.7449 0.0559 1.0000 Uiso . . . . . . H191 H 0.4259 0.1918 0.6641 0.0555 1.0000 Uiso . . . . . . H201 H 0.5352 0.5698 0.5684 0.0397 1.0000 Uiso . . . . . . H211 H 0.2669 0.5077 0.5022 0.0387 1.0000 Uiso . . . . . . H221 H 0.0633 0.4906 0.6012 0.0450 1.0000 Uiso . . . . . . H231 H 0.2018 0.5420 0.7299 0.0490 1.0000 Uiso . . . . . . H241 H 0.4950 0.5918 0.7100 0.0434 1.0000 Uiso . . . . . . 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 Fe101 0.0250(4) 0.0268(4) 0.0232(4) -0.0003(3) 0.0019(3) 0.0084(3) Al102 0.0225(8) 0.0215(7) 0.0202(7) 0.0003(6) -0.0007(6) 0.0054(6) Cl103 0.0269(7) 0.0327(7) 0.0325(7) -0.0038(6) -0.0021(5) -0.0007(5) N104 0.029(2) 0.024(2) 0.023(2) 0.0028(17) 0.0000(18) 0.0097(18) C105 0.019(2) 0.020(2) 0.016(2) -0.0051(18) -0.0024(17) 0.0055(18) N106 0.024(2) 0.021(2) 0.022(2) 0.0018(16) -0.0013(17) 0.0088(17) C107 0.030(3) 0.031(3) 0.025(3) 0.002(2) -0.005(2) 0.015(2) C108 0.031(3) 0.046(4) 0.041(3) 0.006(3) -0.006(3) 0.013(3) C109 0.043(3) 0.027(3) 0.040(3) 0.007(2) 0.001(3) 0.009(3) N110 0.029(2) 0.026(2) 0.0151(19) -0.0017(17) 0.0045(17) 0.0048(18) C111 0.034(3) 0.024(3) 0.021(2) -0.003(2) -0.004(2) 0.004(2) C112 0.032(3) 0.038(3) 0.044(4) -0.009(3) -0.004(3) -0.005(3) C113 0.049(4) 0.032(3) 0.028(3) -0.008(2) 0.002(3) 0.000(3) C114 0.027(3) 0.033(3) 0.024(3) -0.003(2) 0.004(2) 0.004(2) C115 0.026(3) 0.034(3) 0.047(4) -0.001(3) 0.007(3) 0.003(2) C116 0.038(3) 0.040(3) 0.037(3) 0.003(3) 0.009(3) 0.014(3) C117 0.030(3) 0.028(3) 0.018(2) 0.0018(19) 0.000(2) 0.014(2) C118 0.044(3) 0.026(3) 0.030(3) 0.007(2) 0.007(3) 0.007(2) C119 0.036(3) 0.036(3) 0.037(3) 0.004(3) -0.008(3) 0.014(3) C120 0.050(4) 0.042(4) 0.034(3) 0.004(3) -0.001(3) 0.025(3) C121 0.032(3) 0.043(4) 0.040(3) 0.000(3) 0.008(3) 0.018(3) C122 0.042(3) 0.037(3) 0.036(3) -0.005(3) 0.008(3) 0.018(3) C123 0.043(4) 0.031(3) 0.042(4) -0.007(3) 0.007(3) 0.012(3) C124 0.054(4) 0.029(3) 0.039(3) 0.007(3) 0.016(3) 0.017(3) C125 0.041(3) 0.038(3) 0.028(3) -0.003(2) 0.000(2) 0.013(3) O126 0.080(4) 0.053(3) 0.033(2) 0.005(2) -0.008(2) 0.036(3) C127 0.023(3) 0.041(3) 0.031(3) 0.000(3) 0.002(2) 0.007(2) O128 0.032(2) 0.044(3) 0.054(3) -0.017(2) -0.004(2) 0.004(2) Fe1 0.0254(4) 0.0241(4) 0.0230(4) 0.0006(3) 0.0006(3) 0.0084(3) Al2 0.0219(7) 0.0211(7) 0.0195(7) 0.0008(6) 0.0023(6) 0.0034(6) Cl3 0.0281(7) 0.0391(8) 0.0337(7) 0.0070(6) 0.0061(5) -0.0021(6) N4 0.035(3) 0.026(2) 0.017(2) -0.0028(17) 0.0011(18) 0.0065(19) C5 0.023(2) 0.028(3) 0.021(2) 0.002(2) -0.0003(19) 0.005(2) N6 0.029(2) 0.026(2) 0.020(2) -0.0001(17) 0.0008(17) 0.0099(18) C7 0.050(4) 0.028(3) 0.019(3) -0.007(2) 0.005(2) 0.003(3) C8 0.071(5) 0.057(5) 0.040(4) -0.008(3) 0.012(4) 0.031(4) C9 0.074(5) 0.034(4) 0.040(4) -0.011(3) 0.007(4) -0.009(3) N10 0.038(3) 0.032(3) 0.024(2) 0.0034(19) -0.001(2) 0.009(2) C11 0.047(4) 0.040(3) 0.030(3) 0.013(3) 0.002(3) 0.001(3) C12 0.040(4) 0.048(4) 0.044(4) 0.010(3) 0.011(3) -0.002(3) C13 0.077(6) 0.050(4) 0.033(4) 0.018(3) 0.007(4) 0.008(4) C14 0.041(3) 0.048(4) 0.026(3) -0.002(3) -0.009(3) 0.014(3) C15 0.034(4) 0.114(8) 0.041(4) 0.007(4) 0.008(3) 0.019(4) C16 0.049(4) 0.062(5) 0.032(3) 0.000(3) -0.008(3) 0.015(4) C17 0.040(3) 0.026(3) 0.023(3) 0.003(2) 0.002(2) 0.016(2) C18 0.042(4) 0.051(4) 0.036(3) 0.000(3) 0.006(3) 0.026(3) C19 0.054(4) 0.020(3) 0.037(3) 0.002(2) 0.004(3) 0.004(3) C20 0.038(3) 0.030(3) 0.033(3) 0.006(2) -0.001(3) 0.012(2) C21 0.040(3) 0.031(3) 0.031(3) 0.005(2) -0.003(2) 0.018(3) C22 0.037(3) 0.036(3) 0.047(4) 0.002(3) 0.002(3) 0.022(3) C23 0.058(4) 0.039(3) 0.034(3) 0.000(3) 0.011(3) 0.028(3) C24 0.055(4) 0.024(3) 0.030(3) -0.001(2) -0.003(3) 0.010(3) C25 0.025(3) 0.034(3) 0.039(3) 0.000(3) 0.001(2) 0.007(2) O26 0.034(2) 0.044(3) 0.062(3) 0.016(2) 0.013(2) 0.002(2) C27 0.033(3) 0.028(3) 0.027(3) -0.001(2) -0.007(2) 0.009(2) O28 0.065(3) 0.041(3) 0.026(2) -0.0060(19) -0.001(2) 0.028(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3182(5) loop_ _oxford_twin_element_scale_factors 0.6278(16) 0.3722(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 Fe101 . Al102 . 2.3507(17) yes Fe101 . C120 . 2.086(6) yes Fe101 . C121 . 2.113(6) yes Fe101 . C122 . 2.113(6) yes Fe101 . C123 . 2.101(6) yes Fe101 . C124 . 2.096(6) yes Fe101 . C125 . 1.739(6) yes Fe101 . C127 . 1.752(6) yes Al102 . Cl103 . 2.173(2) yes Al102 . N104 . 1.909(5) yes Al102 . C105 . 2.335(5) yes Al102 . N106 . 1.912(5) yes N104 . C105 . 1.328(6) yes N104 . C107 . 1.471(7) yes C105 . N106 . 1.340(6) yes C105 . N110 . 1.421(6) yes N106 . C117 . 1.464(6) yes C107 . C108 . 1.524(8) yes C107 . C109 . 1.535(9) yes C107 . H1071 . 0.982 no C108 . H1083 . 0.961 no C108 . H1082 . 0.956 no C108 . H1081 . 0.963 no C109 . H1091 . 0.959 no C109 . H1092 . 0.961 no C109 . H1093 . 0.963 no N110 . C111 . 1.481(7) yes N110 . C114 . 1.489(7) yes C111 . C112 . 1.521(9) yes C111 . C113 . 1.522(8) yes C111 . H1111 . 0.989 no C112 . H1121 . 0.967 no C112 . H1122 . 0.962 no C112 . H1123 . 0.961 no C113 . H1131 . 0.966 no C113 . H1132 . 0.962 no C113 . H1133 . 0.956 no C114 . C115 . 1.524(8) yes C114 . C116 . 1.530(9) yes C114 . H1141 . 0.989 no C115 . H1151 . 0.958 no C115 . H1152 . 0.970 no C115 . H1153 . 0.961 no C116 . H1161 . 0.960 no C116 . H1162 . 0.972 no C116 . H1163 . 0.963 no C117 . C118 . 1.523(8) yes C117 . C119 . 1.532(8) yes C117 . H1171 . 0.983 no C118 . H1181 . 0.954 no C118 . H1182 . 0.955 no C118 . H1183 . 0.961 no C119 . H1193 . 0.965 no C119 . H1192 . 0.961 no C119 . H1191 . 0.958 no C120 . C121 . 1.424(9) yes C120 . C124 . 1.430(11) yes C120 . H1201 . 0.970 no C121 . C122 . 1.399(10) yes C121 . H1211 . 0.983 no C122 . C123 . 1.427(10) yes C122 . H1221 . 0.976 no C123 . C124 . 1.427(10) yes C123 . H1231 . 0.975 no C124 . H1241 . 0.975 no C125 . O126 . 1.160(8) yes C127 . O128 . 1.146(8) yes Fe1 . Al2 . 2.3435(17) yes Fe1 . C20 . 2.091(6) yes Fe1 . C21 . 2.111(6) yes Fe1 . C22 . 2.115(6) yes Fe1 . C23 . 2.085(6) yes Fe1 . C24 . 2.083(6) yes Fe1 . C25 . 1.743(6) yes Fe1 . C27 . 1.743(6) yes Al2 . Cl3 . 2.167(2) yes Al2 . N4 . 1.919(5) yes Al2 . C5 . 2.330(5) yes Al2 . N6 . 1.908(5) yes N4 . C5 . 1.331(7) yes N4 . C7 . 1.454(7) yes C5 . N6 . 1.323(7) yes C5 . N10 . 1.418(7) yes N6 . C17 . 1.467(7) yes C7 . C8 . 1.518(11) yes C7 . C9 . 1.530(9) yes C7 . H71 . 0.990 no C8 . H83 . 0.959 no C8 . H82 . 0.964 no C8 . H81 . 0.964 no C9 . H91 . 0.959 no C9 . H92 . 0.960 no C9 . H93 . 0.962 no N10 . C11 . 1.491(8) yes N10 . C14 . 1.487(8) yes C11 . C12 . 1.536(11) yes C11 . C13 . 1.524(9) yes C11 . H111 . 0.992 no C12 . H121 . 0.964 no C12 . H122 . 0.960 no C12 . H123 . 0.963 no C13 . H131 . 0.965 no C13 . H132 . 0.962 no C13 . H133 . 0.961 no C14 . C15 . 1.519(11) yes C14 . C16 . 1.522(9) yes C14 . H141 . 0.981 no C15 . H151 . 0.962 no C15 . H152 . 0.964 no C15 . H153 . 0.966 no C16 . H161 . 0.965 no C16 . H162 . 0.964 no C16 . H163 . 0.961 no C17 . C18 . 1.519(9) yes C17 . C19 . 1.527(9) yes C17 . H171 . 0.978 no C18 . H181 . 0.964 no C18 . H182 . 0.964 no C18 . H183 . 0.964 no C19 . H193 . 0.961 no C19 . H192 . 0.956 no C19 . H191 . 0.962 no C20 . C21 . 1.425(9) yes C20 . C24 . 1.432(9) yes C20 . H201 . 0.979 no C21 . C22 . 1.396(9) yes C21 . H211 . 0.978 no C22 . C23 . 1.422(10) yes C22 . H221 . 0.981 no C23 . C24 . 1.406(10) yes C23 . H231 . 0.981 no C24 . H241 . 0.980 no C25 . O26 . 1.159(8) yes C27 . O28 . 1.150(7) yes 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 Al102 . Fe101 . C120 . 111.5(2) yes Al102 . Fe101 . C121 . 149.0(2) yes C120 . Fe101 . C121 . 39.7(3) yes Al102 . Fe101 . C122 . 133.0(2) yes C120 . Fe101 . C122 . 65.9(3) yes C121 . Fe101 . C122 . 38.7(3) yes Al102 . Fe101 . C123 . 94.39(19) yes C120 . Fe101 . C123 . 66.7(3) yes C121 . Fe101 . C123 . 66.2(3) yes C122 . Fe101 . C123 . 39.6(3) yes Al102 . Fe101 . C124 . 82.98(19) yes C120 . Fe101 . C124 . 40.0(3) yes C121 . Fe101 . C124 . 66.6(3) yes C122 . Fe101 . C124 . 66.3(3) yes C123 . Fe101 . C124 . 39.7(3) yes Al102 . Fe101 . C125 . 83.0(2) yes C120 . Fe101 . C125 . 162.8(3) yes C121 . Fe101 . C125 . 123.9(3) yes C122 . Fe101 . C125 . 97.6(3) yes C123 . Fe101 . C125 . 104.2(3) yes Al102 . Fe101 . C127 . 85.5(2) yes C120 . Fe101 . C127 . 97.5(3) yes C121 . Fe101 . C127 . 106.2(3) yes C122 . Fe101 . C127 . 141.0(3) yes C123 . Fe101 . C127 . 163.1(3) yes C124 . Fe101 . C125 . 139.6(3) yes C124 . Fe101 . C127 . 123.8(3) yes C125 . Fe101 . C127 . 92.6(3) yes Fe101 . Al102 . Cl103 . 112.78(8) yes Fe101 . Al102 . N104 . 126.35(16) yes Cl103 . Al102 . N104 . 108.33(16) yes Fe101 . Al102 . C105 . 135.86(14) yes Cl103 . Al102 . C105 . 111.33(14) yes N104 . Al102 . C105 . 34.66(18) yes Fe101 . Al102 . N106 . 124.49(16) yes Cl103 . Al102 . N106 . 107.92(16) yes N104 . Al102 . N106 . 69.66(19) yes C105 . Al102 . N106 . 35.02(18) yes Al102 . N104 . C105 . 90.5(3) yes Al102 . N104 . C107 . 143.6(4) yes C105 . N104 . C107 . 124.6(4) yes Al102 . C105 . N104 . 54.8(3) yes Al102 . C105 . N106 . 55.0(2) yes N104 . C105 . N106 . 109.8(4) yes Al102 . C105 . N110 . 177.2(4) yes N104 . C105 . N110 . 122.4(5) yes N106 . C105 . N110 . 127.8(4) yes C105 . N106 . Al102 . 90.0(3) yes C105 . N106 . C117 . 127.9(4) yes Al102 . N106 . C117 . 140.6(4) yes N104 . C107 . C108 . 110.7(5) yes N104 . C107 . C109 . 110.0(5) yes C108 . C107 . C109 . 109.4(5) yes N104 . C107 . H1071 . 109.2 no C108 . C107 . H1071 . 108.2 no C109 . C107 . H1071 . 109.4 no C107 . C108 . H1083 . 108.0 no C107 . C108 . H1082 . 109.2 no H1083 . C108 . H1082 . 110.1 no C107 . C108 . H1081 . 109.9 no H1083 . C108 . H1081 . 109.9 no H1082 . C108 . H1081 . 109.7 no C107 . C109 . H1091 . 109.0 no C107 . C109 . H1092 . 108.7 no H1091 . C109 . H1092 . 108.7 no C107 . C109 . H1093 . 110.2 no H1091 . C109 . H1093 . 110.2 no H1092 . C109 . H1093 . 110.0 no C105 . N110 . C111 . 115.7(4) yes C105 . N110 . C114 . 116.9(4) yes C111 . N110 . C114 . 117.4(4) yes N110 . C111 . C112 . 109.5(5) yes N110 . C111 . C113 . 110.9(5) yes C112 . C111 . C113 . 108.9(5) yes N110 . C111 . H1111 . 110.9 no C112 . C111 . H1111 . 107.5 no C113 . C111 . H1111 . 109.1 no C111 . C112 . H1121 . 109.4 no C111 . C112 . H1122 . 109.8 no H1121 . C112 . H1122 . 109.3 no C111 . C112 . H1123 . 109.2 no H1121 . C112 . H1123 . 110.1 no H1122 . C112 . H1123 . 109.0 no C111 . C113 . H1131 . 110.0 no C111 . C113 . H1132 . 111.2 no H1131 . C113 . H1132 . 108.4 no C111 . C113 . H1133 . 110.5 no H1131 . C113 . H1133 . 107.9 no H1132 . C113 . H1133 . 108.8 no N110 . C114 . C115 . 111.6(5) yes N110 . C114 . C116 . 115.0(5) yes C115 . C114 . C116 . 109.2(5) yes N110 . C114 . H1141 . 106.6 no C115 . C114 . H1141 . 107.2 no C116 . C114 . H1141 . 106.8 no C114 . C115 . H1151 . 109.2 no C114 . C115 . H1152 . 110.4 no H1151 . C115 . H1152 . 109.3 no C114 . C115 . H1153 . 110.4 no H1151 . C115 . H1153 . 109.0 no H1152 . C115 . H1153 . 108.6 no C114 . C116 . H1161 . 110.1 no C114 . C116 . H1162 . 109.8 no H1161 . C116 . H1162 . 109.0 no C114 . C116 . H1163 . 109.5 no H1161 . C116 . H1163 . 108.9 no H1162 . C116 . H1163 . 109.5 no N106 . C117 . C118 . 109.9(5) yes N106 . C117 . C119 . 109.4(5) yes C118 . C117 . C119 . 111.2(5) yes N106 . C117 . H1171 . 108.2 no C118 . C117 . H1171 . 109.5 no C119 . C117 . H1171 . 108.7 no C117 . C118 . H1181 . 110.4 no C117 . C118 . H1182 . 110.3 no H1181 . C118 . H1182 . 109.7 no C117 . C118 . H1183 . 108.8 no H1181 . C118 . H1183 . 108.9 no H1182 . C118 . H1183 . 108.7 no C117 . C119 . H1193 . 110.6 no C117 . C119 . H1192 . 109.1 no H1193 . C119 . H1192 . 108.7 no C117 . C119 . H1191 . 110.2 no H1193 . C119 . H1191 . 109.3 no H1192 . C119 . H1191 . 108.9 no Fe101 . C120 . C121 . 71.2(4) yes Fe101 . C120 . C124 . 70.3(4) yes C121 . C120 . C124 . 108.0(6) yes Fe101 . C120 . H1201 . 126.0 no C121 . C120 . H1201 . 126.0 no C124 . C120 . H1201 . 125.9 no Fe101 . C121 . C120 . 69.2(4) yes Fe101 . C121 . C122 . 70.7(3) yes C120 . C121 . C122 . 108.1(6) yes Fe101 . C121 . H1211 . 125.6 no C120 . C121 . H1211 . 126.3 no C122 . C121 . H1211 . 125.6 no Fe101 . C122 . C121 . 70.7(4) yes Fe101 . C122 . C123 . 69.8(3) yes C121 . C122 . C123 . 108.9(6) yes Fe101 . C122 . H1221 . 126.3 no C121 . C122 . H1221 . 125.5 no C123 . C122 . H1221 . 125.6 no Fe101 . C123 . C122 . 70.7(4) yes Fe101 . C123 . C124 . 69.9(4) yes C122 . C123 . C124 . 107.5(6) yes Fe101 . C123 . H1231 . 125.3 no C122 . C123 . H1231 . 126.6 no C124 . C123 . H1231 . 125.9 no Fe101 . C124 . C120 . 69.7(4) yes Fe101 . C124 . C123 . 70.3(4) yes C120 . C124 . C123 . 107.5(6) yes Fe101 . C124 . H1241 . 125.1 no C120 . C124 . H1241 . 125.6 no C123 . C124 . H1241 . 126.9 no Fe101 . C125 . O126 . 179.2(7) yes Fe101 . C127 . O128 . 179.1(6) yes Al2 . Fe1 . C20 . 96.56(18) yes Al2 . Fe1 . C21 . 135.85(19) yes C20 . Fe1 . C21 . 39.6(2) yes Al2 . Fe1 . C22 . 146.2(2) yes C20 . Fe1 . C22 . 65.8(3) yes C21 . Fe1 . C22 . 38.6(3) yes Al2 . Fe1 . C23 . 107.7(2) yes C20 . Fe1 . C23 . 66.4(3) yes C21 . Fe1 . C23 . 65.9(3) yes C22 . Fe1 . C23 . 39.6(3) yes Al2 . Fe1 . C24 . 81.54(19) yes C20 . Fe1 . C24 . 40.1(2) yes C21 . Fe1 . C24 . 66.8(2) yes C22 . Fe1 . C24 . 66.3(3) yes C23 . Fe1 . C24 . 39.4(3) yes Al2 . Fe1 . C25 . 87.6(2) yes C20 . Fe1 . C25 . 164.1(3) yes C21 . Fe1 . C25 . 135.8(3) yes C22 . Fe1 . C25 . 102.6(3) yes C23 . Fe1 . C25 . 97.7(3) yes Al2 . Fe1 . C27 . 81.13(19) yes C20 . Fe1 . C27 . 103.3(3) yes C21 . Fe1 . C27 . 100.8(3) yes C22 . Fe1 . C27 . 129.6(3) yes C23 . Fe1 . C27 . 166.7(3) yes C24 . Fe1 . C25 . 126.3(3) yes C24 . Fe1 . C27 . 136.4(3) yes C25 . Fe1 . C27 . 92.5(3) yes Fe1 . Al2 . Cl3 . 113.27(8) yes Fe1 . Al2 . N4 . 126.14(17) yes Cl3 . Al2 . N4 . 108.48(17) yes Fe1 . Al2 . C5 . 134.74(15) yes Cl3 . Al2 . C5 . 111.94(15) yes N4 . Al2 . C5 . 34.86(19) yes Fe1 . Al2 . N6 . 123.27(16) yes Cl3 . Al2 . N6 . 108.77(17) yes N4 . Al2 . N6 . 69.4(2) yes C5 . Al2 . N6 . 34.60(19) yes Al2 . N4 . C5 . 89.7(3) yes Al2 . N4 . C7 . 144.9(4) yes C5 . N4 . C7 . 125.0(5) yes Al2 . C5 . N4 . 55.5(3) yes Al2 . C5 . N6 . 55.0(3) yes N4 . C5 . N6 . 110.4(5) yes Al2 . C5 . N10 . 177.6(4) yes N4 . C5 . N10 . 122.3(5) yes N6 . C5 . N10 . 127.3(5) yes C5 . N6 . Al2 . 90.4(3) yes C5 . N6 . C17 . 127.0(5) yes Al2 . N6 . C17 . 141.7(4) yes N4 . C7 . C8 . 110.4(5) yes N4 . C7 . C9 . 110.3(5) yes C8 . C7 . C9 . 111.0(6) yes N4 . C7 . H71 . 108.1 no C8 . C7 . H71 . 108.3 no C9 . C7 . H71 . 108.7 no C7 . C8 . H83 . 111.0 no C7 . C8 . H82 . 109.9 no H83 . C8 . H82 . 108.3 no C7 . C8 . H81 . 110.3 no H83 . C8 . H81 . 108.3 no H82 . C8 . H81 . 108.9 no C7 . C9 . H91 . 108.6 no C7 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no C7 . C9 . H93 . 109.7 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.9 no C5 . N10 . C11 . 114.4(5) yes C5 . N10 . C14 . 116.9(5) yes C11 . N10 . C14 . 117.4(5) yes N10 . C11 . C12 . 109.0(5) yes N10 . C11 . C13 . 112.2(6) yes C12 . C11 . C13 . 108.4(6) yes N10 . C11 . H111 . 109.0 no C12 . C11 . H111 . 109.5 no C13 . C11 . H111 . 108.6 no C11 . C12 . H121 . 109.2 no C11 . C12 . H122 . 108.3 no H121 . C12 . H122 . 109.6 no C11 . C12 . H123 . 110.5 no H121 . C12 . H123 . 109.7 no H122 . C12 . H123 . 109.4 no C11 . C13 . H131 . 109.7 no C11 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.9 no C11 . C13 . H133 . 109.1 no H131 . C13 . H133 . 109.8 no H132 . C13 . H133 . 108.9 no N10 . C14 . C15 . 113.0(5) yes N10 . C14 . C16 . 110.6(6) yes C15 . C14 . C16 . 108.6(7) yes N10 . C14 . H141 . 108.5 no C15 . C14 . H141 . 108.7 no C16 . C14 . H141 . 107.3 no C14 . C15 . H151 . 108.7 no C14 . C15 . H152 . 109.6 no H151 . C15 . H152 . 110.1 no C14 . C15 . H153 . 108.9 no H151 . C15 . H153 . 109.8 no H152 . C15 . H153 . 109.7 no C14 . C16 . H161 . 109.0 no C14 . C16 . H162 . 109.8 no H161 . C16 . H162 . 109.8 no C14 . C16 . H163 . 109.4 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.4 no N6 . C17 . C18 . 109.6(5) yes N6 . C17 . C19 . 110.3(5) yes C18 . C17 . C19 . 110.2(5) yes N6 . C17 . H171 . 107.7 no C18 . C17 . H171 . 109.7 no C19 . C17 . H171 . 109.4 no C17 . C18 . H181 . 107.9 no C17 . C18 . H182 . 110.0 no H181 . C18 . H182 . 110.1 no C17 . C18 . H183 . 109.5 no H181 . C18 . H183 . 109.3 no H182 . C18 . H183 . 110.0 no C17 . C19 . H193 . 109.6 no C17 . C19 . H192 . 109.1 no H193 . C19 . H192 . 109.2 no C17 . C19 . H191 . 109.4 no H193 . C19 . H191 . 109.4 no H192 . C19 . H191 . 110.3 no Fe1 . C20 . C21 . 70.9(4) yes Fe1 . C20 . C24 . 69.6(4) yes C21 . C20 . C24 . 107.7(6) yes Fe1 . C20 . H201 . 125.7 no C21 . C20 . H201 . 126.0 no C24 . C20 . H201 . 126.2 no Fe1 . C21 . C20 . 69.4(3) yes Fe1 . C21 . C22 . 70.9(4) yes C20 . C21 . C22 . 108.2(6) yes Fe1 . C21 . H211 . 124.6 no C20 . C21 . H211 . 126.0 no C22 . C21 . H211 . 125.8 no Fe1 . C22 . C21 . 70.5(3) yes Fe1 . C22 . C23 . 69.1(3) yes C21 . C22 . C23 . 108.2(6) yes Fe1 . C22 . H221 . 123.5 no C21 . C22 . H221 . 125.8 no C23 . C22 . H221 . 125.9 no Fe1 . C23 . C22 . 71.4(3) yes Fe1 . C23 . C24 . 70.2(3) yes C22 . C23 . C24 . 108.6(6) yes Fe1 . C23 . H231 . 125.4 no C22 . C23 . H231 . 125.7 no C24 . C23 . H231 . 125.7 no C20 . C24 . Fe1 . 70.2(4) yes C20 . C24 . C23 . 107.3(6) yes Fe1 . C24 . C23 . 70.4(4) yes C20 . C24 . H241 . 125.1 no Fe1 . C24 . H241 . 126.9 no C23 . C24 . H241 . 127.5 no Fe1 . C25 . O26 . 178.7(6) yes Fe1 . C27 . O28 . 179.3(6) yes _iucr_refine_instruction_details_constraints ; # # Punched on 26/03/12 at 15:59:38 # #LIST 12 BLOCK SCALE X'S, U'S SUMFIX ELEMENT SCALES END ; _iucr_refine_instruction_details_restraints ; # # Punched on 26/03/12 at 15:59:38 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; data_3 _database_code_depnum_ccdc_archive 'CCDC 894961' #TrackingRef 'Combined Final VRFs.cif' #============================================================================== _audit_creation_date 12-08-01 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '001dvdv10 At 15:43 on 1/ 8' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.12210(10) _cell_length_b 10.18430(10) _cell_length_c 18.3237(2) _cell_angle_alpha 94.1715(5) _cell_angle_beta 95.1909(5) _cell_angle_gamma 110.9440(6) _cell_volume 1400.72(3) _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' 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' 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' 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' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 '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 2 # Given Formula = C26 H30 Al1 Cl1 N3 O2 Ru1 # Dc = 1.38 Fooo = 616.00 Mu = 7.12 M = 580.05 # Found Formula = C26 H41 Al1 Cl1 N3 O2 Ru1 # Dc = 1.40 FOOO = 616.00 Mu = 7.13 M = 591.14 _chemical_formula_sum 'C26 H41 Al1 Cl1 N3 O2 Ru1' _chemical_formula_moiety 'C26 H41 Al1 Cl1 N3 O2 Ru1' _chemical_compound_source ? _chemical_formula_weight 591.14 _cell_measurement_reflns_used 5478 _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 0.140 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_max 0.300 _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.713 # Sheldrick geometric approximatio 0.89 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.90 # 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 21533 _reflns_number_total 6397 _diffrn_reflns_av_R_equivalents 0.020 # Number of reflections without Friedels Law is 11142 # Number of reflections with Friedels Law is 6397 # Theoretical number of reflections is about 6429 _diffrn_reflns_theta_min 5.168 _diffrn_reflns_theta_max 27.490 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.665 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 2.21 _oxford_diffrn_Wilson_scale 3.84 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.48 _refine_diff_density_max 0.80 # 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 6397 _refine_ls_number_restraints 216 _refine_ls_number_parameters 363 _oxford_refine_ls_R_factor_ref 0.0366 _refine_ls_wR_factor_ref 0.0720 _refine_ls_goodness_of_fit_ref 0.9078 _refine_ls_shift/su_max 0.0048870 _refine_ls_shift/su_mean 0.0003975 # The values computed with all filters except I/sigma _oxford_reflns_number_all 6397 _refine_ls_R_factor_all 0.0366 _refine_ls_wR_factor_all 0.0720 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5657 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_gt 0.0652 # 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 noref #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: 16.8 23.9 11.2 2.91 ; # Insert your own references if required - in alphabetical order 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 C400 C 0.7096(7) 1.2493(6) 0.0931(4) 0.0463 0.676(7) Uani D . P 2 1 . C401 C 0.6436(4) 1.1429(3) 0.14873(15) 0.0300 0.676(7) Uani D . P 2 1 . C402 C 0.4779(6) 1.0227(7) 0.1127(4) 0.0361 0.676(7) Uani D . P 2 1 . C403 C 0.7291(17) 1.2559(12) 0.0965(8) 0.0460 0.324(7) Uani D . P 2 2 . C404 C 0.6881(9) 1.1026(7) 0.1117(3) 0.0321 0.324(7) Uani D . P 2 2 . C405 C 0.4890(12) 1.0293(14) 0.1092(8) 0.0341 0.324(7) Uani D . P 2 2 . C300 C 1.1036(8) 1.1867(8) 0.1695(5) 0.0409 0.332(7) Uani D . P 1 1 . C301 C 0.9613(7) 1.1768(6) 0.2183(3) 0.0412 0.332(7) Uani D . P 1 1 . C302 C 0.9752(12) 1.3248(9) 0.2482(7) 0.0503 0.332(7) Uani D . P 1 1 . C303 C 1.0997(4) 1.1237(4) 0.2016(3) 0.0474 0.668(7) Uani D . P 1 2 . C304 C 0.9676(4) 1.1975(3) 0.19406(16) 0.0351 0.668(7) Uani D . P 1 2 . C305 C 0.9926(6) 1.2991(5) 0.2633(3) 0.0531 0.668(7) Uani D . P 1 2 . Ru1 Ru 0.70074(2) 0.629044(19) 0.352242(10) 0.0250 1.0000 Uani . . . . . . Al2 Al 0.59091(9) 0.75844(7) 0.26529(3) 0.0236 1.0000 Uani . . . . . . Cl3 Cl 0.31644(8) 0.65806(7) 0.21678(4) 0.0384 1.0000 Uani . . . . . . N4 N 0.6454(2) 0.95803(19) 0.27724(10) 0.0265 1.0000 Uani . . . . . . C5 C 0.7210(3) 0.9703(2) 0.21479(11) 0.0238 1.0000 Uani . . . . . . N6 N 0.7257(3) 0.8454(2) 0.18981(10) 0.0277 1.0000 Uani . . . . . . C7 C 0.7885(3) 0.8134(2) 0.12114(11) 0.0245 1.0000 Uani . . . . . . C8 C 0.6356(3) 0.7132(3) 0.06635(15) 0.0397 1.0000 Uani . . . . . . C9 C 0.7021(4) 0.6795(3) -0.00551(15) 0.0460 1.0000 Uani . . . . . . C10 C 0.8444(4) 0.6165(3) 0.00838(16) 0.0447 1.0000 Uani . . . . . . C11 C 0.9959(4) 0.7136(3) 0.06380(16) 0.0457 1.0000 Uani . . . . . . C12 C 0.9301(4) 0.7489(3) 0.13558(14) 0.0383 1.0000 Uani . . . . . . N13 N 0.7805(2) 1.09295(19) 0.17844(11) 0.0331 1.0000 Uani D . . . . . C20 C 0.6103(3) 1.0687(2) 0.32074(11) 0.0246 1.0000 Uani . . . . . . C21 C 0.7025(4) 1.0923(4) 0.39866(14) 0.0459 1.0000 Uani . . . . . . C22 C 0.6637(5) 1.2055(4) 0.44582(18) 0.0654 1.0000 Uani . . . . . . C23 C 0.4676(5) 1.1711(3) 0.44572(16) 0.0513 1.0000 Uani . . . . . . C24 C 0.3747(4) 1.1464(3) 0.36799(17) 0.0447 1.0000 Uani . . . . . . C25 C 0.4119(4) 1.0321(3) 0.32109(18) 0.0469 1.0000 Uani . . . . . . C26 C 0.4754(3) 0.5760(3) 0.38285(13) 0.0321 1.0000 Uani . . . . . . O27 O 0.3384(2) 0.5412(2) 0.40311(11) 0.0471 1.0000 Uani . . . . . . C28 C 0.6088(3) 0.4923(3) 0.27194(15) 0.0351 1.0000 Uani . . . . . . O29 O 0.5515(3) 0.4071(2) 0.22158(13) 0.0557 1.0000 Uani . . . . . . C30 C 0.9558(3) 0.8193(3) 0.37163(16) 0.0419 1.0000 Uani . . . . . . C31 C 0.9969(3) 0.6998(3) 0.35017(16) 0.0433 1.0000 Uani . . . . . . C32 C 0.9545(4) 0.6075(3) 0.40528(18) 0.0475 1.0000 Uani . . . . . . C33 C 0.8845(4) 0.6672(4) 0.45944(15) 0.0472 1.0000 Uani . . . . . . C34 C 0.8844(4) 0.7989(3) 0.43868(16) 0.0436 1.0000 Uani . . . . . . H4001 H 0.8035 1.3301 0.1170 0.0708 0.676(7) Uiso . . P 2 1 . H4002 H 0.6101 1.2747 0.0732 0.0712 0.676(7) Uiso . . P 2 1 . H4003 H 0.7507 1.2052 0.0529 0.0708 0.676(7) Uiso . . P 2 1 . H4011 H 0.6116 1.1925 0.1914 0.0381 0.676(7) Uiso . . P 2 1 . H4021 H 0.4287 0.9536 0.1486 0.0541 0.676(7) Uiso . . P 2 1 . H4023 H 0.3860 1.0581 0.0958 0.0541 0.676(7) Uiso . . P 2 1 . H4022 H 0.5069 0.9754 0.0727 0.0544 0.676(7) Uiso . . P 2 1 . H4031 H 0.8578 1.3024 0.0929 0.0569 0.324(7) Uiso . . P 2 2 . H4033 H 0.7009 1.3100 0.1354 0.0569 0.324(7) Uiso . . P 2 2 . H4032 H 0.6664 1.2603 0.0498 0.0571 0.324(7) Uiso . . P 2 2 . H4041 H 0.7306 1.0564 0.0715 0.0360 0.324(7) Uiso . . P 2 2 . H4052 H 0.4617 0.9361 0.1201 0.0439 0.324(7) Uiso . . P 2 2 . H4051 H 0.4451 1.0832 0.1408 0.0440 0.324(7) Uiso . . P 2 2 . H4053 H 0.4329 1.0270 0.0575 0.0440 0.324(7) Uiso . . P 2 2 . H3001 H 1.0930 1.0917 0.1496 0.0592 0.332(7) Uiso . . P 1 1 . H3003 H 1.2214 1.2317 0.1980 0.0590 0.332(7) Uiso . . P 1 1 . H3002 H 1.0950 1.2381 0.1298 0.0590 0.332(7) Uiso . . P 1 1 . H3011 H 0.9827 1.1309 0.2616 0.0500 0.332(7) Uiso . . P 1 1 . H3022 H 0.8825 1.3181 0.2830 0.0742 0.332(7) Uiso . . P 1 1 . H3021 H 1.0883 1.3773 0.2758 0.0741 0.332(7) Uiso . . P 1 1 . H3023 H 0.9509 1.3773 0.2092 0.0740 0.332(7) Uiso . . P 1 1 . H3032 H 1.0937 1.0640 0.1534 0.0733 0.668(7) Uiso . . P 1 2 . H3031 H 1.2198 1.1909 0.2137 0.0731 0.668(7) Uiso . . P 1 2 . H3033 H 1.0724 1.0594 0.2389 0.0730 0.668(7) Uiso . . P 1 2 . H3041 H 0.9918 1.2536 0.1513 0.0461 0.668(7) Uiso . . P 1 2 . H3051 H 0.8960 1.3387 0.2620 0.0815 0.668(7) Uiso . . P 1 2 . H3052 H 1.1066 1.3768 0.2661 0.0811 0.668(7) Uiso . . P 1 2 . H3053 H 0.9942 1.2491 0.3055 0.0802 0.668(7) Uiso . . P 1 2 . H71 H 0.8431 0.9023 0.0993 0.0285 1.0000 Uiso . . . . . . H82 H 0.5464 0.7569 0.0569 0.0494 1.0000 Uiso . . . . . . H81 H 0.5775 0.6238 0.0884 0.0496 1.0000 Uiso . . . . . . H91 H 0.7505 0.7682 -0.0293 0.0559 1.0000 Uiso . . . . . . H92 H 0.6003 0.6124 -0.0393 0.0564 1.0000 Uiso . . . . . . H101 H 0.8906 0.6007 -0.0381 0.0534 1.0000 Uiso . . . . . . H102 H 0.7910 0.5244 0.0277 0.0533 1.0000 Uiso . . . . . . H112 H 1.0582 0.8064 0.0430 0.0556 1.0000 Uiso . . . . . . H111 H 1.0843 0.6694 0.0743 0.0553 1.0000 Uiso . . . . . . H121 H 1.0301 0.8160 0.1706 0.0480 1.0000 Uiso . . . . . . H122 H 0.8787 0.6599 0.1592 0.0470 1.0000 Uiso . . . . . . H201 H 0.6588 1.1591 0.2991 0.0289 1.0000 Uiso . . . . . . H211 H 0.8302 1.1206 0.3970 0.0566 1.0000 Uiso . . . . . . H212 H 0.6597 1.0010 0.4208 0.0569 1.0000 Uiso . . . . . . H222 H 0.7189 1.2151 0.4965 0.0826 1.0000 Uiso . . . . . . H221 H 0.7178 1.2966 0.4254 0.0817 1.0000 Uiso . . . . . . H231 H 0.4461 1.2489 0.4736 0.0621 1.0000 Uiso . . . . . . H232 H 0.4168 1.0860 0.4710 0.0624 1.0000 Uiso . . . . . . H241 H 0.4179 1.2360 0.3450 0.0557 1.0000 Uiso . . . . . . H242 H 0.2458 1.1197 0.3685 0.0557 1.0000 Uiso . . . . . . H252 H 0.3512 1.0158 0.2702 0.0596 1.0000 Uiso . . . . . . H251 H 0.3676 0.9435 0.3436 0.0589 1.0000 Uiso . . . . . . H301 H 0.9763 0.9033 0.3451 0.0508 1.0000 Uiso . . . . . . H311 H 1.0514 0.6866 0.3063 0.0519 1.0000 Uiso . . . . . . H321 H 0.9690 0.5148 0.4045 0.0565 1.0000 Uiso . . . . . . H331 H 0.8428 0.6260 0.5043 0.0556 1.0000 Uiso . . . . . . H341 H 0.8506 0.8674 0.4686 0.0521 1.0000 Uiso . . . . . . 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 C400 0.059(3) 0.044(3) 0.041(3) 0.020(3) 0.011(3) 0.021(3) C401 0.0365(17) 0.0317(16) 0.0288(17) 0.0117(13) 0.0105(13) 0.0179(13) C402 0.031(3) 0.048(4) 0.033(3) 0.005(3) -0.001(2) 0.020(3) C403 0.055(6) 0.042(5) 0.040(6) 0.017(5) 0.012(5) 0.013(5) C404 0.039(3) 0.033(3) 0.028(3) 0.006(2) 0.012(2) 0.015(3) C405 0.039(5) 0.036(6) 0.031(6) 0.011(5) 0.011(5) 0.015(5) C300 0.032(4) 0.038(4) 0.054(4) 0.017(3) 0.016(3) 0.010(3) C301 0.030(3) 0.034(3) 0.052(4) 0.009(3) 0.009(3) 0.000(3) C302 0.042(5) 0.040(4) 0.050(5) -0.003(4) 0.002(4) -0.005(4) C303 0.0249(18) 0.041(2) 0.069(3) 0.002(2) 0.0036(18) 0.0047(16) C304 0.0269(17) 0.0265(17) 0.048(2) 0.0139(15) 0.0104(15) 0.0014(13) C305 0.039(3) 0.048(3) 0.053(3) -0.011(2) 0.012(2) -0.005(2) Ru1 0.02293(9) 0.02752(9) 0.02799(9) 0.00810(6) 0.00694(6) 0.01153(7) Al2 0.0241(3) 0.0243(3) 0.0239(3) 0.0034(2) 0.0036(2) 0.0104(2) Cl3 0.0260(3) 0.0428(3) 0.0424(3) 0.0074(3) -0.0024(2) 0.0089(2) N4 0.0290(9) 0.0241(9) 0.0291(9) 0.0031(7) 0.0090(7) 0.0117(7) C5 0.0215(9) 0.0266(10) 0.0234(10) 0.0020(8) -0.0003(8) 0.0098(8) N6 0.0365(10) 0.0258(9) 0.0239(9) 0.0034(7) 0.0081(8) 0.0139(8) C7 0.0284(10) 0.0258(10) 0.0220(10) 0.0031(8) 0.0073(8) 0.0121(8) C8 0.0339(13) 0.0460(15) 0.0363(13) -0.0117(11) 0.0004(10) 0.0152(11) C9 0.0559(17) 0.0517(16) 0.0325(13) -0.0108(12) 0.0011(12) 0.0263(14) C10 0.0648(18) 0.0399(14) 0.0399(14) 0.0045(11) 0.0213(13) 0.0283(14) C11 0.0489(16) 0.0602(18) 0.0449(15) 0.0071(13) 0.0157(12) 0.0376(14) C12 0.0444(14) 0.0497(15) 0.0316(12) 0.0058(11) 0.0068(10) 0.0297(12) N13 0.0252(9) 0.0270(9) 0.0458(11) 0.0106(8) 0.0034(8) 0.0072(8) C20 0.0294(11) 0.0225(10) 0.0222(10) 0.0016(8) 0.0071(8) 0.0090(8) C21 0.0472(15) 0.0689(19) 0.0263(12) -0.0038(12) 0.0022(11) 0.0294(14) C22 0.061(2) 0.093(3) 0.0382(16) -0.0301(17) -0.0036(14) 0.0329(19) C23 0.065(2) 0.0544(17) 0.0402(15) 0.0006(13) 0.0276(14) 0.0251(15) C24 0.0364(13) 0.0396(14) 0.0584(17) -0.0114(12) 0.0137(12) 0.0155(11) C25 0.0307(13) 0.0450(15) 0.0610(18) -0.0209(13) 0.0053(12) 0.0140(11) C26 0.0313(12) 0.0375(12) 0.0272(11) 0.0045(9) 0.0049(9) 0.0119(10) O27 0.0298(9) 0.0671(13) 0.0412(10) 0.0091(9) 0.0154(8) 0.0109(9) C28 0.0361(12) 0.0313(12) 0.0453(14) 0.0060(10) 0.0136(11) 0.0190(10) O29 0.0586(13) 0.0449(11) 0.0617(14) -0.0186(10) 0.0086(11) 0.0211(10) C30 0.0250(11) 0.0409(14) 0.0519(16) 0.0141(12) -0.0023(11) 0.0027(10) C31 0.0216(11) 0.0635(18) 0.0432(14) 0.0045(13) 0.0088(10) 0.0128(11) C32 0.0317(13) 0.0529(17) 0.0654(19) 0.0143(14) -0.0009(12) 0.0248(12) C33 0.0317(13) 0.075(2) 0.0336(13) 0.0215(13) 0.0003(10) 0.0155(13) C34 0.0305(13) 0.0519(16) 0.0436(15) -0.0105(12) -0.0037(11) 0.0143(12) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5252(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 C400 . C401 . 1.532(5) yes C400 . H4001 . 0.942 no C400 . H4002 . 0.981 no C400 . H4003 . 0.978 no C401 . C402 . 1.512(5) yes C401 . N13 . 1.458(3) yes C401 . H4011 . 1.003 no C402 . H4021 . 1.001 no C402 . H4023 . 0.975 no C402 . H4022 . 0.942 no C403 . C404 . 1.528(7) yes C403 . H4031 . 0.992 no C403 . H4033 . 0.963 no C403 . H4032 . 0.967 no C404 . C405 . 1.514(7) yes C404 . N13 . 1.404(5) yes C404 . H4041 . 0.998 no C405 . H4052 . 0.935 no C405 . H4051 . 0.946 no C405 . H4053 . 1.008 no C300 . C301 . 1.504(6) yes C300 . H3001 . 0.980 no C300 . H3003 . 0.980 no C300 . H3002 . 0.937 no C301 . C302 . 1.527(7) yes C301 . N13 . 1.496(5) yes C301 . H3011 . 0.983 no C302 . H3022 . 1.016 no C302 . H3021 . 0.955 no C302 . H3023 . 0.970 no C303 . C304 . 1.517(4) yes C303 . H3032 . 1.022 no C303 . H3031 . 0.965 no C303 . H3033 . 0.966 no C304 . C305 . 1.528(5) yes C304 . N13 . 1.499(3) yes C304 . H3041 . 0.995 no C305 . H3051 . 1.001 no C305 . H3052 . 0.973 no C305 . H3053 . 0.958 no Ru1 . Al2 . 2.4412(6) yes Ru1 . C26 . 1.865(2) yes Ru1 . C28 . 1.850(3) yes Ru1 . C30 . 2.252(2) yes Ru1 . C31 . 2.255(2) yes Ru1 . C32 . 2.288(3) yes Ru1 . C33 . 2.276(3) yes Ru1 . C34 . 2.248(3) yes Al2 . Cl3 . 2.1645(9) yes Al2 . N4 . 1.9105(19) yes Al2 . C5 . 2.338(2) yes Al2 . N6 . 1.912(2) yes N4 . C5 . 1.340(3) yes N4 . C20 . 1.458(3) yes C5 . N6 . 1.335(3) yes C5 . N13 . 1.409(3) yes N6 . C7 . 1.458(3) yes C7 . C8 . 1.520(3) yes C7 . C12 . 1.528(3) yes C7 . H71 . 0.987 no C8 . C9 . 1.529(4) yes C8 . H82 . 0.986 no C8 . H81 . 0.997 no C9 . C10 . 1.521(4) yes C9 . H91 . 0.997 no C9 . H92 . 0.988 no C10 . C11 . 1.510(4) yes C10 . H101 . 0.986 no C10 . H102 . 0.989 no C11 . C12 . 1.530(4) yes C11 . H112 . 1.020 no C11 . H111 . 0.987 no C12 . H121 . 0.992 no C12 . H122 . 1.002 no C20 . C21 . 1.512(3) yes C20 . C25 . 1.519(3) yes C20 . H201 . 0.992 no C21 . C22 . 1.530(4) yes C21 . H211 . 0.976 no C21 . H212 . 1.000 no C22 . C23 . 1.503(5) yes C22 . H222 . 0.975 no C22 . H221 . 0.992 no C23 . C24 . 1.510(4) yes C23 . H231 . 0.988 no C23 . H232 . 0.986 no C24 . C25 . 1.529(3) yes C24 . H241 . 0.993 no C24 . H242 . 0.984 no C25 . H252 . 0.988 no C25 . H251 . 0.981 no C26 . O27 . 1.146(3) yes C28 . O29 . 1.157(3) yes C30 . C31 . 1.411(4) yes C30 . C34 . 1.403(4) yes C30 . H301 . 0.984 no C31 . C32 . 1.411(4) yes C31 . H311 . 0.976 no C32 . C33 . 1.393(4) yes C32 . H321 . 0.992 no C33 . C34 . 1.420(4) yes C33 . H331 . 0.982 no C34 . H341 . 0.986 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 C401 . C400 . H4001 . 109.3 no C401 . C400 . H4002 . 108.3 no H4001 . C400 . H4002 . 110.6 no C401 . C400 . H4003 . 109.1 no H4001 . C400 . H4003 . 110.1 no H4002 . C400 . H4003 . 109.4 no C400 . C401 . C402 . 108.91(7) yes C400 . C401 . N13 . 112.28(7) yes C402 . C401 . N13 . 112.22(7) yes C400 . C401 . H4011 . 107.9 no C402 . C401 . H4011 . 108.5 no N13 . C401 . H4011 . 106.9 no C401 . C402 . H4021 . 110.6 no C401 . C402 . H4023 . 110.7 no H4021 . C402 . H4023 . 107.6 no C401 . C402 . H4022 . 109.0 no H4021 . C402 . H4022 . 108.7 no H4023 . C402 . H4022 . 110.1 no C404 . C403 . H4031 . 109.7 no C404 . C403 . H4033 . 111.9 no H4031 . C403 . H4033 . 107.2 no C404 . C403 . H4032 . 111.0 no H4031 . C403 . H4032 . 106.9 no H4033 . C403 . H4032 . 110.0 no C403 . C404 . C405 . 108.91(7) yes C403 . C404 . N13 . 112.25(7) yes C405 . C404 . N13 . 112.25(7) yes C403 . C404 . H4041 . 107.0 no C405 . C404 . H4041 . 109.3 no N13 . C404 . H4041 . 107.0 no C404 . C405 . H4052 . 110.1 no C404 . C405 . H4051 . 109.5 no H4052 . C405 . H4051 . 113.6 no C404 . C405 . H4053 . 108.0 no H4052 . C405 . H4053 . 108.4 no H4051 . C405 . H4053 . 107.0 no C301 . C300 . H3001 . 109.9 no C301 . C300 . H3003 . 110.2 no H3001 . C300 . H3003 . 107.4 no C301 . C300 . H3002 . 111.6 no H3001 . C300 . H3002 . 108.3 no H3003 . C300 . H3002 . 109.3 no C300 . C301 . C302 . 110.09(7) yes C300 . C301 . N13 . 111.30(7) yes C302 . C301 . N13 . 111.38(7) yes C300 . C301 . H3011 . 108.7 no C302 . C301 . H3011 . 105.9 no N13 . C301 . H3011 . 109.3 no C301 . C302 . H3022 . 110.1 no C301 . C302 . H3021 . 111.8 no H3022 . C302 . H3021 . 106.8 no C301 . C302 . H3023 . 111.8 no H3022 . C302 . H3023 . 105.9 no H3021 . C302 . H3023 . 110.1 no C304 . C303 . H3032 . 110.7 no C304 . C303 . H3031 . 111.4 no H3032 . C303 . H3031 . 107.8 no C304 . C303 . H3033 . 110.8 no H3032 . C303 . H3033 . 106.5 no H3031 . C303 . H3033 . 109.4 no C303 . C304 . C305 . 110.07(7) yes C303 . C304 . N13 . 111.33(7) yes C305 . C304 . N13 . 111.38(7) yes C303 . C304 . H3041 . 108.1 no C305 . C304 . H3041 . 108.4 no N13 . C304 . H3041 . 107.5 no C304 . C305 . H3051 . 110.8 no C304 . C305 . H3052 . 109.1 no H3051 . C305 . H3052 . 108.9 no C304 . C305 . H3053 . 108.4 no H3051 . C305 . H3053 . 111.2 no H3052 . C305 . H3053 . 108.4 no Al2 . Ru1 . C26 . 85.18(8) yes Al2 . Ru1 . C28 . 79.33(8) yes C26 . Ru1 . C28 . 89.47(11) yes Al2 . Ru1 . C30 . 86.88(7) yes C26 . Ru1 . C30 . 137.23(11) yes C28 . Ru1 . C30 . 130.00(11) yes Al2 . Ru1 . C31 . 106.98(8) yes C26 . Ru1 . C31 . 163.61(10) yes C28 . Ru1 . C31 . 103.35(11) yes C30 . Ru1 . C31 . 36.49(11) yes Al2 . Ru1 . C32 . 143.00(8) yes C26 . Ru1 . C32 . 130.15(11) yes C28 . Ru1 . C32 . 107.63(11) yes C30 . Ru1 . C32 . 60.38(10) yes C31 . Ru1 . C32 . 36.18(11) yes Al2 . Ru1 . C33 . 140.65(9) yes C26 . Ru1 . C33 . 103.43(10) yes C28 . Ru1 . C33 . 137.98(12) yes C30 . Ru1 . C33 . 60.56(10) yes C31 . Ru1 . C33 . 60.19(10) yes Al2 . Ru1 . C34 . 104.07(8) yes C26 . Ru1 . C34 . 106.31(10) yes C28 . Ru1 . C34 . 164.01(10) yes C30 . Ru1 . C34 . 36.34(11) yes C31 . Ru1 . C34 . 60.66(10) yes C32 . Ru1 . C33 . 35.55(11) yes C32 . Ru1 . C34 . 60.23(11) yes C33 . Ru1 . C34 . 36.58(11) yes Ru1 . Al2 . Cl3 . 116.47(3) yes Ru1 . Al2 . N4 . 124.93(7) yes Cl3 . Al2 . N4 . 107.60(7) yes Ru1 . Al2 . C5 . 134.24(6) yes Cl3 . Al2 . C5 . 109.20(6) yes N4 . Al2 . C5 . 34.97(7) yes Ru1 . Al2 . N6 . 121.55(7) yes Cl3 . Al2 . N6 . 107.55(7) yes N4 . Al2 . N6 . 69.65(8) yes C5 . Al2 . N6 . 34.82(7) yes Al2 . N4 . C5 . 90.21(13) yes Al2 . N4 . C20 . 142.35(15) yes C5 . N4 . C20 . 126.73(18) yes Al2 . C5 . N4 . 54.81(11) yes Al2 . C5 . N6 . 54.88(11) yes N4 . C5 . N6 . 109.40(19) yes Al2 . C5 . N13 . 173.13(15) yes N4 . C5 . N13 . 126.23(19) yes N6 . C5 . N13 . 124.32(19) yes C5 . N6 . Al2 . 90.31(13) yes C5 . N6 . C7 . 126.04(18) yes Al2 . N6 . C7 . 142.56(15) yes N6 . C7 . C8 . 110.93(19) yes N6 . C7 . C12 . 110.67(18) yes C8 . C7 . C12 . 109.9(2) yes N6 . C7 . H71 . 108.8 no C8 . C7 . H71 . 108.6 no C12 . C7 . H71 . 108.0 no C7 . C8 . C9 . 110.8(2) yes C7 . C8 . H82 . 108.9 no C9 . C8 . H82 . 110.6 no C7 . C8 . H81 . 109.2 no C9 . C8 . H81 . 109.5 no H82 . C8 . H81 . 107.7 no C8 . C9 . C10 . 111.3(2) yes C8 . C9 . H91 . 108.9 no C10 . C9 . H91 . 110.0 no C8 . C9 . H92 . 108.7 no C10 . C9 . H92 . 110.1 no H91 . C9 . H92 . 107.8 no C9 . C10 . C11 . 110.8(2) yes C9 . C10 . H101 . 110.1 no C11 . C10 . H101 . 109.2 no C9 . C10 . H102 . 108.8 no C11 . C10 . H102 . 109.2 no H101 . C10 . H102 . 108.7 no C10 . C11 . C12 . 111.5(2) yes C10 . C11 . H112 . 110.1 no C12 . C11 . H112 . 107.8 no C10 . C11 . H111 . 110.0 no C12 . C11 . H111 . 109.6 no H112 . C11 . H111 . 107.8 no C11 . C12 . C7 . 111.2(2) yes C11 . C12 . H121 . 110.6 no C7 . C12 . H121 . 109.1 no C11 . C12 . H122 . 108.9 no C7 . C12 . H122 . 109.3 no H121 . C12 . H122 . 107.7 no C301 . N13 . C401 . 128.9(3) yes C301 . N13 . C5 . 104.2(3) yes C401 . N13 . C5 . 115.98(19) yes C304 . N13 . C401 . 117.9(2) yes C304 . N13 . C5 . 121.91(18) yes C401 . N13 . C5 . 115.98(19) yes C301 . N13 . C5 . 104.2(3) yes C301 . N13 . C404 . 133.7(4) yes C5 . N13 . C404 . 120.9(3) yes C304 . N13 . C5 . 121.91(18) yes C304 . N13 . C404 . 114.5(3) yes C5 . N13 . C404 . 120.9(3) yes N4 . C20 . C21 . 110.46(19) yes N4 . C20 . C25 . 110.97(18) yes C21 . C20 . C25 . 110.4(2) yes N4 . C20 . H201 . 109.6 no C21 . C20 . H201 . 107.2 no C25 . C20 . H201 . 108.0 no C20 . C21 . C22 . 111.3(2) yes C20 . C21 . H211 . 108.8 no C22 . C21 . H211 . 110.1 no C20 . C21 . H212 . 108.6 no C22 . C21 . H212 . 109.5 no H211 . C21 . H212 . 108.5 no C21 . C22 . C23 . 112.0(3) yes C21 . C22 . H222 . 109.9 no C23 . C22 . H222 . 109.1 no C21 . C22 . H221 . 107.6 no C23 . C22 . H221 . 109.8 no H222 . C22 . H221 . 108.4 no C22 . C23 . C24 . 111.0(2) yes C22 . C23 . H231 . 110.3 no C24 . C23 . H231 . 109.3 no C22 . C23 . H232 . 109.4 no C24 . C23 . H232 . 109.8 no H231 . C23 . H232 . 107.0 no C23 . C24 . C25 . 111.5(3) yes C23 . C24 . H241 . 108.9 no C25 . C24 . H241 . 108.7 no C23 . C24 . H242 . 110.3 no C25 . C24 . H242 . 109.9 no H241 . C24 . H242 . 107.4 no C24 . C25 . C20 . 111.1(2) yes C24 . C25 . H252 . 111.6 no C20 . C25 . H252 . 110.6 no C24 . C25 . H251 . 108.4 no C20 . C25 . H251 . 106.5 no H252 . C25 . H251 . 108.4 no Ru1 . C26 . O27 . 178.0(2) yes Ru1 . C28 . O29 . 179.8(2) yes Ru1 . C30 . C31 . 71.89(15) yes Ru1 . C30 . C34 . 71.70(15) yes C31 . C30 . C34 . 107.8(2) yes Ru1 . C30 . H301 . 123.2 no C31 . C30 . H301 . 126.2 no C34 . C30 . H301 . 125.9 no Ru1 . C31 . C30 . 71.61(14) yes Ru1 . C31 . C32 . 73.15(15) yes C30 . C31 . C32 . 108.0(2) yes Ru1 . C31 . H311 . 123.6 no C30 . C31 . H311 . 125.6 no C32 . C31 . H311 . 126.4 no Ru1 . C32 . C31 . 70.67(15) yes Ru1 . C32 . C33 . 71.77(15) yes C31 . C32 . C33 . 108.3(3) yes Ru1 . C32 . H321 . 121.9 no C31 . C32 . H321 . 125.5 no C33 . C32 . H321 . 126.2 no Ru1 . C33 . C32 . 72.68(16) yes Ru1 . C33 . C34 . 70.65(15) yes C32 . C33 . C34 . 108.0(2) yes Ru1 . C33 . H331 . 122.5 no C32 . C33 . H331 . 126.2 no C34 . C33 . H331 . 125.8 no Ru1 . C34 . C33 . 72.76(16) yes Ru1 . C34 . C30 . 71.96(15) yes C33 . C34 . C30 . 107.9(2) yes Ru1 . C34 . H341 . 125.3 no C33 . C34 . H341 . 125.6 no C30 . C34 . H341 . 126.2 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 C401 . H4011 . O29 1_565 139.33(17) 1.003 2.441 3.268(6) yes C400 . H4033 . O29 1_565 156.3(3) 0.980 2.434 3.354(6) yes C403 . H4033 . O29 1_565 165.2(7) 0.963 2.434 3.374(6) yes C302 . H3023 . C403 . 121.7(4) 0.970 2.530 3.150(6) yes _iucr_refine_instruction_details_constraints ; # # Punched on 01/08/12 at 16:50:52 # #LIST 12 BLOCK SCALE X'S, U'S EQUIV PART(2001,OCC) PART(2002,OCC) WEIGHT -1 PART(2002,OCC) EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 01/08/12 at 16:50:52 # #LIST 16 SAME N(13) C(304) C(305) C(303) AND CONT N(13) C(304) C(303) C(305) AND CONT N(13) C(301) C(300) C(302) AND CONT N(13) C(301) C(302) C(300) SIMU 0.01 N(13) C(304) C(305) C(303) AND CONT N(13) C(304) C(303) C(305) AND CONT N(13) C(301) C(300) C(302) AND CONT N(13) C(301) C(302) C(300) DELU 0.01 N(13) C(304) C(305) C(303) AND CONT N(13) C(304) C(303) C(305) AND CONT N(13) C(301) C(300) C(302) AND CONT N(13) C(301) C(302) C(300) SAME N(13) C(404) C(405) C(403) AND CONT N(13) C(404) C(403) C(405) AND CONT N(13) C(401) C(400) C(402) AND CONT N(13) C(401) C(402) C(400) SIMU 0.01 N(13) C(404) C(405) C(403) AND CONT N(13) C(404) C(403) C(405) AND CONT N(13) C(401) C(400) C(402) AND CONT N(13) C(401) C(402) C(400) DELU 0.01 N(13) C(404) C(405) C(403) AND CONT N(13) C(404) C(403) C(405) AND CONT N(13) C(401) C(400) C(402) AND CONT N(13) C(401) C(402) C(400) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; data_4 _database_code_depnum_ccdc_archive 'CCDC 894962' #TrackingRef 'Combined Final VRFs.cif' #============================================================================== _audit_creation_date 12-08-01 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '020irnp11 At 16:51 on 29/ 6' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 10.5121(4) _cell_length_b 11.4183(4) _cell_length_c 14.4923(6) _cell_angle_alpha 89.0196(18) _cell_angle_beta 71.366(2) _cell_angle_gamma 80.7037(15) _cell_volume 1625.57(11) _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' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 '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' 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' 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' 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 2 # Given Formula = C31 H51 Al1 Cl1 Fe1 N3 O2 # Dc = 1.26 Fooo = 660.00 Mu = 6.04 M = 616.05 # Found Formula = C31 H51 Al1 Cl1 Fe1 N3 O2 # Dc = 1.26 FOOO = 660.00 Mu = 6.04 M = 616.05 _chemical_formula_sum 'C31 H51 Al1 Cl1 Fe1 N3 O2' _chemical_formula_moiety 'C31 H51 Al1 Cl1 Fe1 N3 O2' _chemical_compound_source ? _chemical_formula_weight 616.05 _cell_measurement_reflns_used 6381 _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 0.180 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 660.000 _exptl_absorpt_coefficient_mu 0.604 # Sheldrick geometric approximatio 0.89 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.90 # 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 21942 _reflns_number_total 7265 _diffrn_reflns_av_R_equivalents 0.020 # Number of reflections without Friedels Law is 12364 # Number of reflections with Friedels Law is 7265 # Theoretical number of reflections is about 7447 _diffrn_reflns_theta_min 5.159 _diffrn_reflns_theta_max 27.471 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.548 _diffrn_measured_fraction_theta_full 0.979 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -12 _reflns_limit_h_max 13 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 2.90 _oxford_diffrn_Wilson_scale 0.98 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.63 _refine_diff_density_max 0.85 # 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 7264 _refine_ls_number_restraints 42 _refine_ls_number_parameters 368 _oxford_refine_ls_R_factor_ref 0.0621 _refine_ls_wR_factor_ref 0.1242 _refine_ls_goodness_of_fit_ref 0.9257 _refine_ls_shift/su_max 0.0018998 _refine_ls_shift/su_mean 0.0000648 # The values computed with all filters except I/sigma _oxford_reflns_number_all 7265 _refine_ls_R_factor_all 0.0621 _refine_ls_wR_factor_all 0.1243 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5801 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_gt 0.1083 # 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 #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: 116. 188. 114. 47.3 10.9 ; # Insert your own references if required - in alphabetical order 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 Fe1 Fe 0.62179(3) 0.42595(3) 0.72456(2) 0.0329 1.0000 Uani . . . . . . Al2 Al 0.80514(7) 0.26660(6) 0.68905(5) 0.0344 1.0000 Uani . . . . . . Cl3 Cl 0.95100(7) 0.25993(6) 0.54409(5) 0.0481 1.0000 Uani . . . . . . N4 N 0.7753(2) 0.10655(16) 0.72023(15) 0.0349 1.0000 Uani . . . . . . C5 C 0.8595(2) 0.0974(2) 0.77255(16) 0.0343 1.0000 Uani . . . . . . N6 N 0.9018(2) 0.20164(18) 0.77561(16) 0.0398 1.0000 Uani . . . . . . C7 C 1.0064(2) 0.2207(2) 0.81676(18) 0.0381 1.0000 Uani . . . . . . C8 C 0.9499(3) 0.3162(2) 0.8985(2) 0.0468 1.0000 Uani . . . . . . C9 C 1.0577(4) 0.3390(3) 0.9422(3) 0.0694 1.0000 Uani . . . . . . C10 C 1.1770(4) 0.3761(3) 0.8656(4) 0.0790 1.0000 Uani . . . . . . C11 C 1.2358(3) 0.2832(4) 0.7837(4) 0.0788 1.0000 Uani . . . . . . C12 C 1.1286(3) 0.2574(3) 0.7392(2) 0.0556 1.0000 Uani . . . . . . N13 N 0.9054(2) -0.00437(17) 0.81658(14) 0.0388 1.0000 Uani D U . . . . C14 C 0.8169(3) -0.0278(2) 0.9148(2) 0.0497 0.736(7) Uani D U P 1 1 . C15 C 0.7280(5) -0.1196(4) 0.9178(3) 0.0557 0.736(7) Uani D U P 1 1 . C16 C 0.7602(5) 0.0753(4) 0.9803(3) 0.0654 0.736(7) Uani D U P 1 1 . C17 C 0.9898(3) -0.1033(3) 0.7498(2) 0.0576 1.0000 Uani . . . . . . C18 C 1.0884(3) -0.0598(3) 0.6613(2) 0.0568 1.0000 Uani . . . . . . C19 C 1.0661(4) -0.1939(4) 0.7979(3) 0.0815 1.0000 Uani . . . . . . C20 C 0.7059(2) 0.01279(19) 0.70187(17) 0.0349 1.0000 Uani . . . . . . C21 C 0.5524(3) 0.0449(2) 0.74945(18) 0.0394 1.0000 Uani . . . . . . C22 C 0.4784(3) -0.0498(3) 0.7274(2) 0.0518 1.0000 Uani . . . . . . C23 C 0.5142(4) -0.0693(3) 0.6180(2) 0.0589 1.0000 Uani . . . . . . C24 C 0.6667(3) -0.1036(3) 0.5702(2) 0.0531 1.0000 Uani . . . . . . C25 C 0.7421(3) -0.0098(2) 0.59208(18) 0.0424 1.0000 Uani . . . . . . C26 C 0.5333(3) 0.5889(2) 0.68388(18) 0.0388 1.0000 Uani . . . . . . C27 C 0.6762(3) 0.5646(2) 0.63036(17) 0.0378 1.0000 Uani . . . . . . C28 C 0.7500(3) 0.5573(2) 0.69833(18) 0.0386 1.0000 Uani . . . . . . C29 C 0.6511(3) 0.5745(2) 0.79368(17) 0.0391 1.0000 Uani . . . . . . C30 C 0.5184(3) 0.5955(2) 0.78423(18) 0.0401 1.0000 Uani . . . . . . C31 C 0.3875(3) 0.6279(2) 0.8664(2) 0.0495 1.0000 Uani . . . . . . C32 C 0.6800(3) 0.5816(3) 0.8882(2) 0.0511 1.0000 Uani . . . . . . C33 C 0.8997(3) 0.5530(2) 0.6729(2) 0.0486 1.0000 Uani . . . . . . C34 C 0.7391(3) 0.5586(2) 0.52156(18) 0.0457 1.0000 Uani . . . . . . C35 C 0.4200(3) 0.6074(3) 0.6409(2) 0.0505 1.0000 Uani . . . . . . C36 C 0.5664(3) 0.3436(2) 0.82732(18) 0.0398 1.0000 Uani . . . . . . O37 O 0.5267(2) 0.29265(16) 0.89891(13) 0.0519 1.0000 Uani . . . . . . C38 C 0.5832(3) 0.3410(2) 0.64211(17) 0.0371 1.0000 Uani . . . . . . O39 O 0.5564(2) 0.29000(17) 0.58425(14) 0.0498 1.0000 Uani . . . . . . C114 C 0.8406(9) -0.0490(6) 0.9135(5) 0.0497 0.264(7) Uani D U P 1 2 . C115 C 0.7075(15) -0.0867(16) 0.9272(9) 0.0557 0.264(7) Uani D U P 1 2 . C116 C 0.8582(14) 0.0127(10) 0.9955(5) 0.0567 0.264(7) Uani D U P 1 2 . H71 H 1.0383 0.1452 0.8431 0.0452 1.0000 Uiso R . . . . . H82 H 0.8741 0.2903 0.9498 0.0562 1.0000 Uiso R . . . . . H81 H 0.9174 0.3895 0.8715 0.0560 1.0000 Uiso R . . . . . H91 H 1.0193 0.4018 0.9931 0.0835 1.0000 Uiso R . . . . . H92 H 1.0889 0.2661 0.9692 0.0829 1.0000 Uiso R . . . . . H101 H 1.2470 0.3855 0.8946 0.0915 1.0000 Uiso R . . . . . H102 H 1.1475 0.4520 0.8401 0.0910 1.0000 Uiso R . . . . . H111 H 1.2705 0.2101 0.8105 0.0940 1.0000 Uiso R . . . . . H112 H 1.3091 0.3100 0.7329 0.0945 1.0000 Uiso R . . . . . H121 H 1.0960 0.3296 0.7099 0.0679 1.0000 Uiso R . . . . . H122 H 1.1671 0.1961 0.6881 0.0684 1.0000 Uiso R . . . . . H141 H 0.8852 -0.0675 0.9481 0.0632 0.736(7) Uiso R . P 1 1 . H152 H 0.6981 -0.1531 0.9814 0.0848 0.736(7) Uiso R . P 1 1 . H151 H 0.7769 -0.1847 0.8715 0.0852 0.736(7) Uiso R . P 1 1 . H153 H 0.6477 -0.0795 0.9013 0.0851 0.736(7) Uiso R . P 1 1 . H161 H 0.7095 0.0493 1.0438 0.1108 0.736(7) Uiso R . P 1 1 . H163 H 0.8328 0.1168 0.9854 0.1112 0.736(7) Uiso R . P 1 1 . H162 H 0.6984 0.1253 0.9513 0.1114 0.736(7) Uiso R . P 1 1 . H171 H 0.9271 -0.1473 0.7268 0.0728 1.0000 Uiso R . . . . . H182 H 1.1347 -0.1261 0.6178 0.0838 1.0000 Uiso R . . . . . H181 H 1.1532 -0.0228 0.6815 0.0846 1.0000 Uiso R . . . . . H183 H 1.0407 -0.0029 0.6290 0.0838 1.0000 Uiso R . . . . . H191 H 1.1270 -0.2519 0.7493 0.1228 1.0000 Uiso R . . . . . H193 H 1.1160 -0.1506 0.8279 0.1234 1.0000 Uiso R . . . . . H192 H 1.0014 -0.2310 0.8472 0.1231 1.0000 Uiso R . . . . . H201 H 0.7376 -0.0608 0.7289 0.0402 1.0000 Uiso R . . . . . H212 H 0.5313 0.0540 0.8191 0.0479 1.0000 Uiso R . . . . . H211 H 0.5219 0.1192 0.7236 0.0477 1.0000 Uiso R . . . . . H221 H 0.5057 -0.1254 0.7541 0.0623 1.0000 Uiso R . . . . . H222 H 0.3799 -0.0247 0.7581 0.0622 1.0000 Uiso R . . . . . H232 H 0.4691 -0.1314 0.6049 0.0719 1.0000 Uiso R . . . . . H231 H 0.4852 0.0060 0.5908 0.0719 1.0000 Uiso R . . . . . H241 H 0.6971 -0.1795 0.5955 0.0633 1.0000 Uiso R . . . . . H242 H 0.6881 -0.1131 0.4995 0.0632 1.0000 Uiso R . . . . . H251 H 0.8402 -0.0364 0.5642 0.0515 1.0000 Uiso R . . . . . H252 H 0.7154 0.0645 0.5644 0.0504 1.0000 Uiso R . . . . . H311 H 0.3962 0.5900 0.9241 0.0733 1.0000 Uiso R . . . . . H313 H 0.3681 0.7129 0.8777 0.0734 1.0000 Uiso R . . . . . H312 H 0.3141 0.6017 0.8503 0.0735 1.0000 Uiso R . . . . . H321 H 0.6395 0.5240 0.9308 0.0765 1.0000 Uiso R . . . . . H323 H 0.6420 0.6599 0.9179 0.0760 1.0000 Uiso R . . . . . H322 H 0.7755 0.5672 0.8773 0.0764 1.0000 Uiso R . . . . . H331 H 0.9314 0.5279 0.7269 0.0729 1.0000 Uiso R . . . . . H332 H 0.9224 0.6305 0.6541 0.0729 1.0000 Uiso R . . . . . H333 H 0.9464 0.4985 0.6188 0.0732 1.0000 Uiso R . . . . . H341 H 0.7996 0.4858 0.5011 0.0673 1.0000 Uiso R . . . . . H342 H 0.7888 0.6229 0.5013 0.0674 1.0000 Uiso R . . . . . H343 H 0.6689 0.5650 0.4930 0.0679 1.0000 Uiso R . . . . . H351 H 0.3445 0.5735 0.6801 0.0758 1.0000 Uiso R . . . . . H352 H 0.3915 0.6900 0.6344 0.0765 1.0000 Uiso R . . . . . H353 H 0.4503 0.5690 0.5772 0.0760 1.0000 Uiso R . . . . . H1141 H 0.8970 -0.1278 0.9114 0.0622 0.264(7) Uiso R . P 1 2 . H1152 H 0.6784 -0.1300 0.9919 0.0850 0.264(7) Uiso R . P 1 2 . H1151 H 0.6444 -0.0065 0.9294 0.0848 0.264(7) Uiso R . P 1 2 . H1153 H 0.7142 -0.1399 0.8685 0.0851 0.264(7) Uiso R . P 1 2 . H1162 H 0.7742 0.0258 1.0482 0.0689 0.264(7) Uiso R . P 1 2 . H1161 H 0.9262 -0.0349 1.0166 0.0689 0.264(7) Uiso R . P 1 2 . H1163 H 0.8867 0.0868 0.9747 0.0690 0.264(7) Uiso R . P 1 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 Fe1 0.03939(19) 0.02544(16) 0.02904(16) 0.00060(11) -0.00486(13) -0.00385(12) Al2 0.0365(4) 0.0277(3) 0.0360(3) -0.0002(3) -0.0079(3) -0.0042(3) Cl3 0.0481(4) 0.0410(3) 0.0420(3) -0.0019(2) 0.0024(3) -0.0041(3) N4 0.0380(10) 0.0263(9) 0.0389(10) -0.0021(7) -0.0111(8) -0.0036(8) C5 0.0326(11) 0.0313(11) 0.0330(11) -0.0021(9) -0.0037(9) -0.0018(9) N6 0.0399(11) 0.0337(10) 0.0487(12) 0.0025(9) -0.0173(9) -0.0077(8) C7 0.0340(12) 0.0354(12) 0.0435(13) 0.0005(10) -0.0110(10) -0.0044(9) C8 0.0533(15) 0.0378(13) 0.0454(14) -0.0018(11) -0.0123(12) -0.0037(11) C9 0.107(3) 0.0445(16) 0.075(2) -0.0008(15) -0.055(2) -0.0118(17) C10 0.084(3) 0.0567(19) 0.123(3) 0.009(2) -0.065(3) -0.0242(19) C11 0.0422(17) 0.072(2) 0.124(4) 0.005(2) -0.026(2) -0.0176(16) C12 0.0409(14) 0.0591(17) 0.0597(17) -0.0016(14) -0.0042(13) -0.0121(13) N13 0.0476(12) 0.0317(10) 0.0321(9) 0.0023(8) -0.0080(8) -0.0019(8) C14 0.062(2) 0.0498(18) 0.0330(13) 0.0043(12) -0.0069(13) -0.0132(16) C15 0.072(3) 0.039(3) 0.053(2) 0.0137(19) -0.0138(18) -0.017(3) C16 0.087(4) 0.050(2) 0.041(2) -0.0004(15) 0.006(2) -0.014(2) C17 0.0578(17) 0.0382(14) 0.0630(18) -0.0010(13) -0.0093(14) 0.0113(12) C18 0.0519(16) 0.0575(17) 0.0460(15) -0.0089(13) -0.0040(13) 0.0113(13) C19 0.078(2) 0.067(2) 0.079(2) 0.0145(19) -0.014(2) 0.0244(19) C20 0.0441(13) 0.0254(10) 0.0353(11) 0.0012(8) -0.0129(10) -0.0053(9) C21 0.0437(13) 0.0359(12) 0.0353(12) 0.0011(9) -0.0069(10) -0.0091(10) C22 0.0529(16) 0.0521(16) 0.0537(16) 0.0071(13) -0.0143(13) -0.0244(13) C23 0.068(2) 0.0619(18) 0.0578(18) -0.0023(14) -0.0280(15) -0.0269(16) C24 0.075(2) 0.0417(14) 0.0462(15) -0.0096(11) -0.0222(14) -0.0113(13) C25 0.0501(14) 0.0355(12) 0.0357(12) -0.0057(9) -0.0070(11) -0.0038(10) C26 0.0460(13) 0.0271(10) 0.0371(12) 0.0028(9) -0.0068(10) -0.0023(9) C27 0.0471(13) 0.0270(10) 0.0344(11) 0.0015(9) -0.0063(10) -0.0060(9) C28 0.0451(13) 0.0272(10) 0.0377(12) -0.0002(9) -0.0050(10) -0.0067(9) C29 0.0524(14) 0.0262(10) 0.0346(12) -0.0016(9) -0.0085(10) -0.0055(10) C30 0.0484(14) 0.0263(10) 0.0374(12) 0.0011(9) -0.0045(10) -0.0018(9) C31 0.0539(16) 0.0374(13) 0.0419(13) -0.0019(10) 0.0016(12) 0.0015(11) C32 0.0691(19) 0.0431(14) 0.0391(13) -0.0045(11) -0.0152(13) -0.0074(13) C33 0.0498(15) 0.0412(13) 0.0515(15) 0.0003(11) -0.0087(12) -0.0132(12) C34 0.0575(16) 0.0374(13) 0.0348(12) 0.0024(10) -0.0038(11) -0.0093(11) C35 0.0528(16) 0.0430(14) 0.0516(15) 0.0079(12) -0.0152(13) 0.0005(12) C36 0.0491(14) 0.0284(11) 0.0347(12) -0.0041(9) -0.0054(10) -0.0021(10) O37 0.0758(14) 0.0373(9) 0.0308(9) 0.0039(7) -0.0004(9) -0.0102(9) C38 0.0438(13) 0.0305(11) 0.0327(11) 0.0052(9) -0.0073(10) -0.0044(9) O39 0.0695(13) 0.0419(10) 0.0425(10) 0.0006(8) -0.0233(9) -0.0107(9) C114 0.062(2) 0.0498(18) 0.0330(13) 0.0043(12) -0.0069(13) -0.0132(16) C115 0.072(3) 0.039(3) 0.053(2) 0.0137(19) -0.0138(18) -0.017(3) C116 0.097(9) 0.044(6) 0.033(4) 0.013(4) -0.025(5) -0.015(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.019(3) 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 Fe1 . Al2 . 2.3570(8) yes Fe1 . C26 . 2.104(2) yes Fe1 . C27 . 2.101(2) yes Fe1 . C28 . 2.125(2) yes Fe1 . C29 . 2.098(2) yes Fe1 . C30 . 2.110(2) yes Fe1 . C36 . 1.737(2) yes Fe1 . C38 . 1.735(3) yes Al2 . Cl3 . 2.1631(9) yes Al2 . N4 . 1.926(2) yes Al2 . N6 . 1.922(2) yes N4 . C5 . 1.328(3) yes N4 . C20 . 1.462(3) yes C5 . N6 . 1.343(3) yes C5 . N13 . 1.407(3) yes N6 . C7 . 1.453(3) yes C7 . C8 . 1.527(4) yes C7 . C12 . 1.526(4) yes C7 . H71 . 0.989 no C8 . C9 . 1.520(4) yes C8 . H82 . 0.982 no C8 . H81 . 0.976 no C9 . C10 . 1.500(6) yes C9 . H91 . 0.977 no C9 . H92 . 0.968 no C10 . C11 . 1.510(6) yes C10 . H101 . 0.976 no C10 . H102 . 0.980 no C11 . C12 . 1.533(5) yes C11 . H111 . 0.981 no C11 . H112 . 0.968 no C12 . H121 . 0.983 no C12 . H122 . 0.968 no N13 . C14 . 1.479(3) yes N13 . C17 . 1.472(3) yes N13 . C17 . 1.472(3) yes N13 . C114 . 1.474(6) yes C14 . C15 . 1.504(4) yes C14 . C16 . 1.447(4) yes C14 . H141 . 1.030 no C15 . H152 . 0.968 no C15 . H151 . 0.970 no C15 . H153 . 0.990 no C16 . H161 . 0.973 no C16 . H163 . 0.983 no C16 . H162 . 0.985 no C17 . C18 . 1.504(4) yes C17 . C19 . 1.506(4) yes C17 . H171 . 1.025 no C18 . H182 . 0.953 no C18 . H181 . 0.975 no C18 . H183 . 0.963 no C19 . H191 . 0.968 no C19 . H193 . 0.972 no C19 . H192 . 0.961 no C20 . C21 . 1.523(3) yes C20 . C25 . 1.529(3) yes C20 . H201 . 0.976 no C21 . C22 . 1.524(4) yes C21 . H212 . 0.965 no C21 . H211 . 0.970 no C22 . C23 . 1.519(4) yes C22 . H221 . 0.978 no C22 . H222 . 0.983 no C23 . C24 . 1.517(5) yes C23 . H232 . 0.966 no C23 . H231 . 0.984 no C24 . C25 . 1.525(4) yes C24 . H241 . 0.980 no C24 . H242 . 0.980 no C25 . H251 . 0.977 no C25 . H252 . 0.971 no C26 . C27 . 1.436(3) yes C26 . C30 . 1.414(3) yes C26 . C35 . 1.497(4) yes C27 . C28 . 1.430(4) yes C27 . C34 . 1.500(3) yes C28 . C29 . 1.433(3) yes C28 . C33 . 1.490(4) yes C29 . C30 . 1.426(4) yes C29 . C32 . 1.502(4) yes C30 . C31 . 1.501(3) yes C31 . H311 . 0.959 no C31 . H313 . 0.964 no C31 . H312 . 0.964 no C32 . H321 . 0.950 no C32 . H323 . 0.965 no C32 . H322 . 0.952 no C33 . H331 . 0.966 no C33 . H332 . 0.965 no C33 . H333 . 0.957 no C34 . H341 . 0.949 no C34 . H342 . 0.957 no C34 . H343 . 0.948 no C35 . H351 . 0.953 no C35 . H352 . 0.955 no C35 . H353 . 0.963 no C36 . O37 . 1.170(3) yes C38 . O39 . 1.158(3) yes C114 . C115 . 1.482(7) yes C114 . C116 . 1.468(6) yes C114 . H1141 . 0.989 no C115 . H1152 . 1.032 no C115 . H1151 . 1.035 no C115 . H1153 . 1.031 no C116 . H1162 . 0.957 no C116 . H1161 . 0.953 no C116 . H1163 . 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 Al2 . Fe1 . C26 . 148.52(7) yes Al2 . Fe1 . C27 . 109.54(7) yes C26 . Fe1 . C27 . 39.94(10) yes Al2 . Fe1 . C28 . 93.68(7) yes C26 . Fe1 . C28 . 66.65(10) yes C27 . Fe1 . C28 . 39.54(10) yes Al2 . Fe1 . C29 . 114.51(8) yes C26 . Fe1 . C29 . 66.27(10) yes C27 . Fe1 . C29 . 66.39(9) yes C28 . Fe1 . C29 . 39.68(9) yes Al2 . Fe1 . C30 . 154.05(8) yes C26 . Fe1 . C30 . 39.21(9) yes C27 . Fe1 . C30 . 66.44(9) yes C28 . Fe1 . C30 . 66.59(10) yes C29 . Fe1 . C30 . 39.61(10) yes Al2 . Fe1 . C36 . 80.50(8) yes C26 . Fe1 . C36 . 130.96(10) yes C27 . Fe1 . C36 . 163.67(10) yes C28 . Fe1 . C36 . 129.58(11) yes C29 . Fe1 . C36 . 97.93(10) yes Al2 . Fe1 . C38 . 78.84(8) yes C26 . Fe1 . C38 . 94.65(10) yes C27 . Fe1 . C38 . 95.99(10) yes C28 . Fe1 . C38 . 129.53(10) yes C29 . Fe1 . C38 . 160.27(10) yes C30 . Fe1 . C36 . 98.78(10) yes C30 . Fe1 . C38 . 126.51(11) yes C36 . Fe1 . C38 . 98.66(11) yes Fe1 . Al2 . Cl3 . 115.82(4) yes Fe1 . Al2 . N4 . 121.09(7) yes Cl3 . Al2 . N4 . 107.36(7) yes Fe1 . Al2 . N6 . 126.67(7) yes Cl3 . Al2 . N6 . 107.63(8) yes N4 . Al2 . N6 . 69.15(9) yes Al2 . N4 . C5 . 90.65(14) yes Al2 . N4 . C20 . 143.27(16) yes C5 . N4 . C20 . 126.00(19) yes N4 . C5 . N6 . 109.7(2) yes N4 . C5 . N13 . 127.6(2) yes N6 . C5 . N13 . 122.7(2) yes C5 . N6 . Al2 . 90.35(15) yes C5 . N6 . C7 . 124.8(2) yes Al2 . N6 . C7 . 143.27(17) yes N6 . C7 . C8 . 110.7(2) yes N6 . C7 . C12 . 111.2(2) yes C8 . C7 . C12 . 109.2(2) yes N6 . C7 . H71 . 108.6 no C8 . C7 . H71 . 109.3 no C12 . C7 . H71 . 107.7 no C7 . C8 . C9 . 111.8(3) yes C7 . C8 . H82 . 108.8 no C9 . C8 . H82 . 109.1 no C7 . C8 . H81 . 108.2 no C9 . C8 . H81 . 108.9 no H82 . C8 . H81 . 110.0 no C8 . C9 . C10 . 110.9(3) yes C8 . C9 . H91 . 109.9 no C10 . C9 . H91 . 108.9 no C8 . C9 . H92 . 108.4 no C10 . C9 . H92 . 108.6 no H91 . C9 . H92 . 110.2 no C9 . C10 . C11 . 110.4(3) yes C9 . C10 . H101 . 109.3 no C11 . C10 . H101 . 109.0 no C9 . C10 . H102 . 109.3 no C11 . C10 . H102 . 109.7 no H101 . C10 . H102 . 109.2 no C10 . C11 . C12 . 111.9(3) yes C10 . C11 . H111 . 107.7 no C12 . C11 . H111 . 109.0 no C10 . C11 . H112 . 109.8 no C12 . C11 . H112 . 108.5 no H111 . C11 . H112 . 110.0 no C11 . C12 . C7 . 111.1(3) yes C11 . C12 . H121 . 109.4 no C7 . C12 . H121 . 107.8 no C11 . C12 . H122 . 111.0 no C7 . C12 . H122 . 109.8 no H121 . C12 . H122 . 107.6 no C5 . N13 . C14 . 116.33(18) yes C5 . N13 . C17 . 116.0(2) yes C14 . N13 . C17 . 120.43(18) yes C5 . N13 . C17 . 116.0(2) yes C5 . N13 . C114 . 128.5(4) yes C17 . N13 . C114 . 110.1(3) yes N13 . C14 . C15 . 115.16(7) yes N13 . C14 . C16 . 115.19(7) yes C15 . C14 . C16 . 117.99(7) yes N13 . C14 . H141 . 103.1 no C15 . C14 . H141 . 103.9 no C16 . C14 . H141 . 97.5 no C14 . C15 . H152 . 112.1 no C14 . C15 . H151 . 110.6 no H152 . C15 . H151 . 107.2 no C14 . C15 . H153 . 107.1 no H152 . C15 . H153 . 109.3 no H151 . C15 . H153 . 110.4 no C14 . C16 . H161 . 108.5 no C14 . C16 . H163 . 110.5 no H161 . C16 . H163 . 110.7 no C14 . C16 . H162 . 104.9 no H161 . C16 . H162 . 110.5 no H163 . C16 . H162 . 111.6 no N13 . C17 . C18 . 111.6(2) yes N13 . C17 . C19 . 112.9(3) yes C18 . C17 . C19 . 109.5(3) yes N13 . C17 . H171 . 108.5 no C18 . C17 . H171 . 108.0 no C19 . C17 . H171 . 106.1 no C17 . C18 . H182 . 108.4 no C17 . C18 . H181 . 109.0 no H182 . C18 . H181 . 110.4 no C17 . C18 . H183 . 110.3 no H182 . C18 . H183 . 109.1 no H181 . C18 . H183 . 109.6 no C17 . C19 . H191 . 109.3 no C17 . C19 . H193 . 106.4 no H191 . C19 . H193 . 111.4 no C17 . C19 . H192 . 108.7 no H191 . C19 . H192 . 111.0 no H193 . C19 . H192 . 109.9 no N4 . C20 . C21 . 111.03(19) yes N4 . C20 . C25 . 109.74(19) yes C21 . C20 . C25 . 110.8(2) yes N4 . C20 . H201 . 109.2 no C21 . C20 . H201 . 108.5 no C25 . C20 . H201 . 107.4 no C20 . C21 . C22 . 111.5(2) yes C20 . C21 . H212 . 109.5 no C22 . C21 . H212 . 109.2 no C20 . C21 . H211 . 108.2 no C22 . C21 . H211 . 108.5 no H212 . C21 . H211 . 109.9 no C21 . C22 . C23 . 110.3(2) yes C21 . C22 . H221 . 110.3 no C23 . C22 . H221 . 107.7 no C21 . C22 . H222 . 108.8 no C23 . C22 . H222 . 111.1 no H221 . C22 . H222 . 108.6 no C22 . C23 . C24 . 111.0(3) yes C22 . C23 . H232 . 109.6 no C24 . C23 . H232 . 109.4 no C22 . C23 . H231 . 108.2 no C24 . C23 . H231 . 107.6 no H232 . C23 . H231 . 111.0 no C23 . C24 . C25 . 111.1(2) yes C23 . C24 . H241 . 108.8 no C25 . C24 . H241 . 109.0 no C23 . C24 . H242 . 109.8 no C25 . C24 . H242 . 109.3 no H241 . C24 . H242 . 108.8 no C20 . C25 . C24 . 111.1(2) yes C20 . C25 . H251 . 109.1 no C24 . C25 . H251 . 109.4 no C20 . C25 . H252 . 107.6 no C24 . C25 . H252 . 109.2 no H251 . C25 . H252 . 110.4 no Fe1 . C26 . C27 . 69.91(13) yes Fe1 . C26 . C30 . 70.62(13) yes C27 . C26 . C30 . 108.1(2) yes Fe1 . C26 . C35 . 126.34(18) yes C27 . C26 . C35 . 126.0(2) yes C30 . C26 . C35 . 125.9(2) yes Fe1 . C27 . C26 . 70.14(13) yes Fe1 . C27 . C28 . 71.14(13) yes C26 . C27 . C28 . 108.3(2) yes Fe1 . C27 . C34 . 128.63(17) yes C26 . C27 . C34 . 126.3(2) yes C28 . C27 . C34 . 125.1(2) yes Fe1 . C28 . C27 . 69.32(14) yes Fe1 . C28 . C29 . 69.12(13) yes C27 . C28 . C29 . 106.8(2) yes Fe1 . C28 . C33 . 134.01(18) yes C27 . C28 . C33 . 125.6(2) yes C29 . C28 . C33 . 126.9(2) yes Fe1 . C29 . C28 . 71.20(13) yes Fe1 . C29 . C30 . 70.67(14) yes C28 . C29 . C30 . 108.8(2) yes Fe1 . C29 . C32 . 128.58(18) yes C28 . C29 . C32 . 126.3(3) yes C30 . C29 . C32 . 124.6(2) yes Fe1 . C30 . C29 . 69.71(13) yes Fe1 . C30 . C26 . 70.17(13) yes C29 . C30 . C26 . 107.9(2) yes Fe1 . C30 . C31 . 129.12(18) yes C29 . C30 . C31 . 125.5(2) yes C26 . C30 . C31 . 126.4(3) yes C30 . C31 . H311 . 109.2 no C30 . C31 . H313 . 109.3 no H311 . C31 . H313 . 109.6 no C30 . C31 . H312 . 110.0 no H311 . C31 . H312 . 109.0 no H313 . C31 . H312 . 109.7 no C29 . C32 . H321 . 109.8 no C29 . C32 . H323 . 108.9 no H321 . C32 . H323 . 109.4 no C29 . C32 . H322 . 110.4 no H321 . C32 . H322 . 108.8 no H323 . C32 . H322 . 109.5 no C28 . C33 . H331 . 111.6 no C28 . C33 . H332 . 109.7 no H331 . C33 . H332 . 109.3 no C28 . C33 . H333 . 109.7 no H331 . C33 . H333 . 108.5 no H332 . C33 . H333 . 108.0 no C27 . C34 . H341 . 110.1 no C27 . C34 . H342 . 109.8 no H341 . C34 . H342 . 108.9 no C27 . C34 . H343 . 108.8 no H341 . C34 . H343 . 110.1 no H342 . C34 . H343 . 109.1 no C26 . C35 . H351 . 110.7 no C26 . C35 . H352 . 110.8 no H351 . C35 . H352 . 109.6 no C26 . C35 . H353 . 109.8 no H351 . C35 . H353 . 107.6 no H352 . C35 . H353 . 108.3 no Fe1 . C36 . O37 . 177.1(2) yes Fe1 . C38 . O39 . 176.2(2) yes N13 . C114 . C115 . 115.23(7) yes N13 . C114 . C116 . 115.23(7) yes C115 . C114 . C116 . 118.05(7) yes N13 . C114 . H1141 . 102.4 no C115 . C114 . H1141 . 99.4 no C116 . C114 . H1141 . 102.5 no C114 . C115 . H1152 . 109.6 no C114 . C115 . H1151 . 102.3 no H1152 . C115 . H1151 . 112.0 no C114 . C115 . H1153 . 109.6 no H1152 . C115 . H1153 . 111.6 no H1151 . C115 . H1153 . 111.4 no C114 . C116 . H1162 . 109.8 no C114 . C116 . H1161 . 109.2 no H1162 . C116 . H1161 . 109.4 no C114 . C116 . H1163 . 109.2 no H1162 . C116 . H1163 . 110.0 no H1161 . C116 . H1163 . 109.1 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 C114 . H1141 . C19 . 124.7(2) 0.989 2.043 2.730(5) yes C116 . H1161 . C116 2_757 131.8(5) 0.953 2.272 2.993(5) yes _iucr_refine_instruction_details_constraints ; # # Punched on 01/08/12 at 15:04:27 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C(14,U'S) C(114,U'S) RIDE C(15,U'S) C(115,U'S) EQUIV PART(1001,OCC) PART(1002,OCC) WEIGHT -1 PART(1002,OCC) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 82,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) RIDE C ( 14,X'S) H ( 141,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 ( 161,X'S) H ( 163,X'S) H ( 162,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 182,X'S) H ( 181,X'S) H ( 183,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 193,X'S) H ( 192,X'S) RIDE C ( 20,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 212,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 222,X'S) RIDE C ( 23,X'S) H ( 232,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S) RIDE C ( 31,X'S) H ( 311,X'S) H ( 313,X'S) H ( 312,X'S) RIDE C ( 32,X'S) H ( 321,X'S) H ( 323,X'S) H ( 322,X'S) RIDE C ( 33,X'S) H ( 331,X'S) H ( 332,X'S) H ( 333,X'S) RIDE C ( 34,X'S) H ( 341,X'S) H ( 342,X'S) H ( 343,X'S) RIDE C ( 35,X'S) H ( 351,X'S) H ( 352,X'S) H ( 353,X'S) RIDE C ( 114,X'S) H (1141,X'S) RIDE C ( 115,X'S) H (1152,X'S) H (1151,X'S) H (1153,X'S) RIDE C ( 116,X'S) H (1162,X'S) H (1161,X'S) H (1163,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 01/08/12 at 15:04:27 # #LIST 16 SAME N(13) C(14) C(15) C(16) AND CONT N(13) C(14) C(16) C(15) AND CONT N(13) C(114) C(115) C(116) AND CONT N(13) C(114) C(116) C(115) REM DELU START (DO NOT REMOVE THIS LINE) VIBR .0, 0.00200 = C(14) TO C(16) VIBR .0, 0.00500 = C(16) TO N(13) VIBR .0, 0.00500 = C(16) TO C(15) VIBR .0, 0.00200 = C(114) TO C(116) VIBR .0, 0.00500 = C(116) TO N(13) VIBR .0, 0.00500 = C(116) TO C(115) REM DELU END (DO NOT REMOVE THIS LINE) REM THERMSIM START (DO NOT REMOVE THIS LINE) U(IJ) .0, 0.08000 = C(14) TO C(16) U(IJ) .0, 0.08000 = C(114) TO C(116) REM THERMSIM END (DO NOT REMOVE THIS LINE) END ; data_5 _database_code_depnum_ccdc_archive 'CCDC 894963' #TrackingRef 'Combined Final VRFs.cif' #============================================================================== _audit_creation_date 11-12-15 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 034irnp11 _chemical_name_systematic . _chemical_melting_point . _cell_length_a 18.75650(10) _cell_length_b 19.82660(10) _cell_length_c 20.35820(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7570.76(7) _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab' 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 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 x+1/2,-y+1/2,-z -x+1/2,y+1/2,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' 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' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 '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' I -0.4742 1.8119 20.1472 4.3470 18.9949 0.3814 7.5138 27.7660 2.2735 66.8776 4.0712 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C38 H41 Al1 Fe1 I1 N3 O2 # Dc = 1.37 Fooo = 3280.00 Mu = 12.72 M = 781.50 # Found Formula = C38 H53 Al1 Fe1 I1 N3 O2 # Dc = 1.39 FOOO = 3280.00 Mu = 12.73 M = 793.59 _chemical_formula_sum 'C38 H53 Al1 Fe1 I1 N3 O2' _chemical_formula_moiety 'C38 H53 Al1 Fe1 I1 N3 O2' _chemical_compound_source . _chemical_formula_weight 793.59 _cell_measurement_reflns_used 9362 _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 0.200 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_max 0.340 _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3280 _exptl_absorpt_coefficient_mu 1.273 # Sheldrick geometric approximatio 0.76 0.78 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.78 # 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 102060 _reflns_number_total 8617 _diffrn_reflns_av_R_equivalents 0.030 # Number of reflections without Friedels Law is 16512 # Number of reflections with Friedels Law is 8617 # Theoretical number of reflections is about 8681 _diffrn_reflns_theta_min 5.165 _diffrn_reflns_theta_max 27.482 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.932 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min 0 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 1.94 _oxford_diffrn_Wilson_scale 45.17 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.95 _refine_diff_density_max 0.79 # 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 8616 _refine_ls_number_restraints 0 _refine_ls_number_parameters 415 _oxford_refine_ls_R_factor_ref 0.0596 _refine_ls_wR_factor_ref 0.0902 _refine_ls_goodness_of_fit_ref 0.9418 _refine_ls_shift/su_max 0.0019101 _refine_ls_shift/su_mean 0.0000394 # The values computed from all data _oxford_reflns_number_all 8617 _refine_ls_R_factor_all 0.0596 _refine_ls_wR_factor_all 0.0903 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6192 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_gt 0.0693 # 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, 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: 7.23 10.3 5.05 1.34 ; # Insert your own references if required - in alphabetical order 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 I1 I 0.875018(12) 0.538746(10) 0.418380(10) 0.0308 1.0000 Uani . . . . . . Al2 Al 0.84224(4) 0.41258(4) 0.40629(4) 0.0197 1.0000 Uani . . . . . . Fe3 Fe 0.89519(2) 0.35554(2) 0.49648(2) 0.0253 1.0000 Uani . . . . . . C4 C 0.97333(19) 0.37910(19) 0.45603(17) 0.0351 1.0000 Uani . . . . . . O5 O 1.02584(14) 0.39329(17) 0.42958(14) 0.0524 1.0000 Uani . . . . . . C6 C 0.8925(2) 0.4299(2) 0.56922(16) 0.0396 1.0000 Uani . . . . . . C7 C 0.9202(2) 0.3697(2) 0.59634(17) 0.0431 1.0000 Uani . . . . . . C8 C 0.8675(2) 0.3193(2) 0.58993(17) 0.0422 1.0000 Uani . . . . . . C9 C 0.8065(2) 0.3488(2) 0.55961(17) 0.0386 1.0000 Uani . . . . . . C10 C 0.8221(2) 0.4169(2) 0.54673(17) 0.0381 1.0000 Uani . . . . . . C11 C 0.8964(2) 0.27496(18) 0.46232(17) 0.0344 1.0000 Uani . . . . . . O12 O 0.90085(18) 0.22004(14) 0.44462(15) 0.0524 1.0000 Uani . . . . . . N13 N 0.83587(12) 0.39087(12) 0.31414(11) 0.0187 1.0000 Uani . . . . . . C14 C 0.76331(15) 0.39286(14) 0.31629(14) 0.0198 1.0000 Uani . . . . . . N15 N 0.74481(12) 0.40670(12) 0.37995(11) 0.0183 1.0000 Uani . . . . . . C16 C 0.68139(14) 0.39094(14) 0.41652(14) 0.0193 1.0000 Uani . . . . . . C17 C 0.64553(15) 0.44414(15) 0.44872(14) 0.0211 1.0000 Uani . . . . . . C18 C 0.65972(16) 0.51780(15) 0.43373(15) 0.0241 1.0000 Uani . . . . . . C19 C 0.68027(19) 0.55772(16) 0.49522(17) 0.0327 1.0000 Uani . . . . . . C20 C 0.59344(19) 0.54984(17) 0.40228(18) 0.0338 1.0000 Uani . . . . . . C21 C 0.59234(16) 0.42833(17) 0.49401(15) 0.0275 1.0000 Uani . . . . . . C22 C 0.57360(17) 0.36256(18) 0.50794(16) 0.0312 1.0000 Uani . . . . . . C23 C 0.60654(17) 0.31112(16) 0.47398(16) 0.0284 1.0000 Uani . . . . . . C24 C 0.66016(16) 0.32340(15) 0.42758(15) 0.0242 1.0000 Uani . . . . . . C25 C 0.69153(17) 0.26306(15) 0.39244(18) 0.0306 1.0000 Uani . . . . . . C26 C 0.6334(2) 0.22719(18) 0.35224(19) 0.0376 1.0000 Uani . . . . . . C27 C 0.7249(2) 0.21241(18) 0.4400(2) 0.0457 1.0000 Uani . . . . . . N28 N 0.71587(13) 0.38491(14) 0.26617(12) 0.0235 1.0000 Uani . . . . . . C29 C 0.65029(15) 0.42737(17) 0.26910(15) 0.0268 1.0000 Uani . . . . . . C30 C 0.6654(2) 0.49932(19) 0.24603(19) 0.0373 1.0000 Uani . . . . . . C31 C 0.58638(17) 0.3980(2) 0.23336(18) 0.0387 1.0000 Uani . . . . . . C32 C 0.73653(17) 0.34692(18) 0.20539(15) 0.0305 1.0000 Uani . . . . . . C33 C 0.6932(2) 0.2824(2) 0.19458(19) 0.0421 1.0000 Uani . . . . . . C34 C 0.7387(2) 0.3885(2) 0.14288(17) 0.0428 1.0000 Uani . . . . . . C35 C 0.88017(16) 0.38640(15) 0.25641(14) 0.0214 1.0000 Uani . . . . . . C36 C 0.89391(16) 0.44271(16) 0.21590(15) 0.0248 1.0000 Uani . . . . . . C37 C 0.87453(18) 0.51492(16) 0.23388(15) 0.0285 1.0000 Uani . . . . . . C38 C 0.9430(2) 0.55265(18) 0.2535(2) 0.0390 1.0000 Uani . . . . . . C39 C 0.8375(2) 0.5548(2) 0.17903(19) 0.0443 1.0000 Uani . . . . . . C40 C 0.93295(16) 0.43202(18) 0.15833(15) 0.0299 1.0000 Uani . . . . . . C41 C 0.95924(18) 0.36900(19) 0.14143(16) 0.0340 1.0000 Uani . . . . . . C42 C 0.95015(16) 0.31599(17) 0.18462(16) 0.0292 1.0000 Uani . . . . . . C43 C 0.91230(16) 0.32343(16) 0.24279(15) 0.0240 1.0000 Uani . . . . . . C44 C 0.90716(17) 0.26413(16) 0.29033(16) 0.0284 1.0000 Uani . . . . . . C45 C 0.8614(3) 0.2067(2) 0.2648(2) 0.0594 1.0000 Uani . . . . . . C46 C 0.9805(2) 0.2380(2) 0.3093(2) 0.0550 1.0000 Uani . . . . . . H61 H 0.9173 0.4732 0.5657 0.0484 1.0000 Uiso R . . . . . H71 H 0.9680 0.3637 0.6155 0.0523 1.0000 Uiso R . . . . . H81 H 0.8719 0.2719 0.6035 0.0499 1.0000 Uiso R . . . . . H91 H 0.7620 0.3248 0.5491 0.0462 1.0000 Uiso R . . . . . H101 H 0.7899 0.4498 0.5254 0.0467 1.0000 Uiso R . . . . . H181 H 0.7000 0.5201 0.4028 0.0292 1.0000 Uiso R . . . . . H191 H 0.6844 0.6043 0.4837 0.0491 1.0000 Uiso R . . . . . H193 H 0.7256 0.5415 0.5116 0.0494 1.0000 Uiso R . . . . . H192 H 0.6442 0.5519 0.5287 0.0492 1.0000 Uiso R . . . . . H201 H 0.6039 0.5946 0.3874 0.0506 1.0000 Uiso R . . . . . H203 H 0.5559 0.5519 0.4345 0.0514 1.0000 Uiso R . . . . . H202 H 0.5779 0.5229 0.3646 0.0509 1.0000 Uiso R . . . . . H211 H 0.5687 0.4640 0.5153 0.0332 1.0000 Uiso R . . . . . H221 H 0.5389 0.3531 0.5403 0.0363 1.0000 Uiso R . . . . . H231 H 0.5925 0.2666 0.4820 0.0337 1.0000 Uiso R . . . . . H251 H 0.7294 0.2791 0.3625 0.0370 1.0000 Uiso R . . . . . H261 H 0.6550 0.1904 0.3280 0.0567 1.0000 Uiso R . . . . . H263 H 0.5978 0.2091 0.3820 0.0569 1.0000 Uiso R . . . . . H262 H 0.6113 0.2590 0.3221 0.0573 1.0000 Uiso R . . . . . H271 H 0.7475 0.1766 0.4152 0.0730 1.0000 Uiso R . . . . . H273 H 0.7598 0.2350 0.4666 0.0728 1.0000 Uiso R . . . . . H272 H 0.6873 0.1938 0.4674 0.0729 1.0000 Uiso R . . . . . H291 H 0.6373 0.4304 0.3166 0.0315 1.0000 Uiso R . . . . . H303 H 0.6236 0.5270 0.2528 0.0548 1.0000 Uiso R . . . . . H302 H 0.7047 0.5182 0.2708 0.0549 1.0000 Uiso R . . . . . H301 H 0.6768 0.4992 0.1997 0.0549 1.0000 Uiso R . . . . . H311 H 0.5453 0.4254 0.2427 0.0588 1.0000 Uiso R . . . . . H313 H 0.5948 0.3975 0.1863 0.0588 1.0000 Uiso R . . . . . H312 H 0.5778 0.3527 0.2484 0.0588 1.0000 Uiso R . . . . . H321 H 0.7856 0.3313 0.2128 0.0369 1.0000 Uiso R . . . . . H333 H 0.7178 0.2552 0.1619 0.0630 1.0000 Uiso R . . . . . H332 H 0.6899 0.2581 0.2352 0.0631 1.0000 Uiso R . . . . . H331 H 0.6463 0.2948 0.1792 0.0631 1.0000 Uiso R . . . . . H343 H 0.7605 0.3617 0.1089 0.0642 1.0000 Uiso R . . . . . H342 H 0.7659 0.4293 0.1499 0.0637 1.0000 Uiso R . . . . . H341 H 0.6906 0.4004 0.1300 0.0637 1.0000 Uiso R . . . . . H371 H 0.8426 0.5140 0.2727 0.0338 1.0000 Uiso R . . . . . H382 H 0.9299 0.5975 0.2693 0.0587 1.0000 Uiso R . . . . . H381 H 0.9746 0.5563 0.2159 0.0590 1.0000 Uiso R . . . . . H383 H 0.9661 0.5277 0.2893 0.0589 1.0000 Uiso R . . . . . H393 H 0.8261 0.5994 0.1946 0.0668 1.0000 Uiso R . . . . . H392 H 0.8690 0.5587 0.1419 0.0670 1.0000 Uiso R . . . . . H391 H 0.7943 0.5321 0.1655 0.0669 1.0000 Uiso R . . . . . H401 H 0.9415 0.4695 0.1308 0.0360 1.0000 Uiso R . . . . . H411 H 0.9837 0.3626 0.1013 0.0412 1.0000 Uiso R . . . . . H421 H 0.9702 0.2735 0.1745 0.0356 1.0000 Uiso R . . . . . H441 H 0.8836 0.2813 0.3305 0.0347 1.0000 Uiso R . . . . . H452 H 0.8551 0.1728 0.2985 0.0878 1.0000 Uiso R . . . . . H451 H 0.8840 0.1874 0.2263 0.0881 1.0000 Uiso R . . . . . H453 H 0.8158 0.2239 0.2527 0.0880 1.0000 Uiso R . . . . . H462 H 0.9752 0.2018 0.3403 0.0845 1.0000 Uiso R . . . . . H461 H 1.0086 0.2743 0.3277 0.0856 1.0000 Uiso R . . . . . H463 H 1.0025 0.2218 0.2698 0.0850 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 I1 0.03797(11) 0.02143(9) 0.03288(11) -0.00175(8) -0.00146(9) -0.00676(9) Al2 0.0184(4) 0.0199(4) 0.0208(4) -0.0001(3) -0.0004(3) -0.0002(3) Fe3 0.0257(2) 0.0276(2) 0.0225(2) 0.00220(18) -0.00385(17) 0.00085(17) C4 0.0306(17) 0.0405(19) 0.0341(18) -0.0025(15) -0.0055(14) 0.0008(15) O5 0.0326(14) 0.077(2) 0.0478(17) -0.0083(15) 0.0084(12) -0.0106(14) C6 0.053(2) 0.042(2) 0.0240(16) -0.0091(15) 0.0070(15) -0.0117(17) C7 0.043(2) 0.062(3) 0.0238(16) 0.0003(16) -0.0082(15) -0.0006(19) C8 0.057(2) 0.0417(19) 0.0273(17) 0.0110(15) 0.0015(17) -0.0012(18) C9 0.0386(19) 0.048(2) 0.0291(17) 0.0045(16) 0.0038(14) -0.0073(17) C10 0.042(2) 0.046(2) 0.0260(16) 0.0016(15) 0.0064(14) 0.0096(17) C11 0.0411(19) 0.0322(18) 0.0300(16) 0.0027(14) -0.0024(14) 0.0056(15) O12 0.076(2) 0.0282(14) 0.0531(17) 0.0011(12) 0.0032(16) 0.0007(14) N13 0.0171(11) 0.0202(11) 0.0188(11) -0.0011(9) 0.0018(9) 0.0011(9) C14 0.0190(13) 0.0182(13) 0.0221(13) 0.0018(11) -0.0005(10) 0.0000(11) N15 0.0172(11) 0.0206(11) 0.0171(10) -0.0010(9) 0.0007(9) -0.0019(9) C16 0.0162(12) 0.0238(13) 0.0180(12) 0.0024(11) -0.0004(11) -0.0021(10) C17 0.0203(13) 0.0229(14) 0.0203(13) -0.0012(11) -0.0003(11) 0.0010(11) C18 0.0230(14) 0.0216(14) 0.0276(15) -0.0037(11) 0.0064(12) 0.0021(11) C19 0.0380(18) 0.0258(16) 0.0342(17) -0.0051(14) 0.0025(15) -0.0008(13) C20 0.0355(17) 0.0277(16) 0.0381(18) 0.0040(14) 0.0009(14) 0.0073(14) C21 0.0252(15) 0.0328(16) 0.0244(14) -0.0013(13) 0.0073(12) -0.0027(13) C22 0.0275(15) 0.0399(18) 0.0264(15) 0.0045(14) 0.0048(13) -0.0068(14) C23 0.0260(15) 0.0232(14) 0.0361(17) 0.0095(13) 0.0008(13) -0.0060(12) C24 0.0236(14) 0.0226(14) 0.0263(15) 0.0037(12) -0.0032(12) -0.0010(11) C25 0.0278(15) 0.0183(14) 0.0456(19) 0.0015(13) 0.0000(14) -0.0003(12) C26 0.0407(19) 0.0293(16) 0.0428(19) -0.0002(15) -0.0034(16) -0.0014(15) C27 0.041(2) 0.0258(17) 0.070(3) -0.0010(17) -0.0211(19) 0.0025(15) N28 0.0177(11) 0.0344(14) 0.0183(12) -0.0024(11) -0.0011(9) 0.0020(10) C29 0.0182(13) 0.0404(18) 0.0216(14) 0.0059(13) -0.0004(11) 0.0064(13) C30 0.0319(18) 0.042(2) 0.0386(19) 0.0065(16) 0.0025(15) 0.0062(16) C31 0.0195(15) 0.061(2) 0.0354(18) 0.0017(17) -0.0027(13) 0.0017(16) C32 0.0223(15) 0.045(2) 0.0238(15) -0.0118(14) 0.0025(12) -0.0018(14) C33 0.0354(19) 0.055(2) 0.0360(19) -0.0212(18) 0.0037(15) -0.0097(17) C34 0.039(2) 0.067(3) 0.0233(16) -0.0015(17) 0.0028(14) -0.0084(19) C35 0.0179(13) 0.0256(13) 0.0205(13) -0.0027(11) 0.0011(11) -0.0011(12) C36 0.0204(13) 0.0296(15) 0.0244(14) -0.0026(12) -0.0002(11) -0.0011(11) C37 0.0309(16) 0.0269(14) 0.0276(15) 0.0043(12) 0.0075(14) 0.0014(14) C38 0.0384(19) 0.0328(19) 0.046(2) -0.0035(15) 0.0145(16) -0.0090(15) C39 0.052(2) 0.040(2) 0.040(2) 0.0152(17) 0.0047(18) 0.0078(17) C40 0.0244(15) 0.0406(18) 0.0247(15) 0.0023(14) 0.0047(12) -0.0036(14) C41 0.0280(16) 0.048(2) 0.0256(16) -0.0063(15) 0.0084(13) -0.0027(15) C42 0.0231(15) 0.0324(17) 0.0321(16) -0.0091(14) 0.0025(13) 0.0000(13) C43 0.0188(14) 0.0274(15) 0.0258(15) -0.0052(12) 0.0015(11) -0.0024(12) C44 0.0291(15) 0.0256(16) 0.0304(16) -0.0037(13) 0.0028(13) 0.0048(13) C45 0.084(4) 0.042(2) 0.052(3) 0.0127(19) -0.017(2) -0.029(2) C46 0.035(2) 0.056(3) 0.074(3) 0.027(2) 0.005(2) 0.0124(19) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.086618(15) 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 I1 . Al2 . 2.5876(9) yes Al2 . Fe3 . 2.3742(9) yes Al2 . N13 . 1.929(2) yes Al2 . N15 . 1.908(2) yes Fe3 . C4 . 1.745(4) yes Fe3 . C6 . 2.091(3) yes Fe3 . C7 . 2.105(3) yes Fe3 . C8 . 2.098(3) yes Fe3 . C9 . 2.106(4) yes Fe3 . C10 . 2.099(4) yes Fe3 . C11 . 1.742(4) yes C4 . O5 . 1.157(4) yes C6 . C7 . 1.415(6) yes C6 . C10 . 1.421(5) yes C6 . H61 . 0.978 no C7 . C8 . 1.410(6) yes C7 . H71 . 0.985 no C8 . C9 . 1.425(5) yes C8 . H81 . 0.983 no C9 . C10 . 1.406(5) yes C9 . H91 . 0.985 no C10 . H101 . 0.989 no C11 . O12 . 1.150(4) yes N13 . C14 . 1.362(4) yes N13 . C35 . 1.442(4) yes C14 . N15 . 1.369(4) yes C14 . N28 . 1.363(4) yes N15 . C16 . 1.438(3) yes C16 . C17 . 1.412(4) yes C16 . C24 . 1.415(4) yes C17 . C18 . 1.516(4) yes C17 . C21 . 1.394(4) yes C18 . C19 . 1.530(4) yes C18 . C20 . 1.536(5) yes C18 . H181 . 0.985 no C19 . H191 . 0.957 no C19 . H193 . 0.968 no C19 . H192 . 0.967 no C20 . H201 . 0.959 no C20 . H203 . 0.964 no C20 . H202 . 0.978 no C21 . C22 . 1.380(5) yes C21 . H211 . 0.940 no C22 . C23 . 1.378(5) yes C22 . H221 . 0.945 no C23 . C24 . 1.401(4) yes C23 . H231 . 0.936 no C24 . C25 . 1.513(4) yes C25 . C26 . 1.538(5) yes C25 . C27 . 1.530(5) yes C25 . H251 . 0.988 no C26 . H261 . 0.970 no C26 . H263 . 0.970 no C26 . H262 . 0.972 no C27 . H271 . 0.969 no C27 . H273 . 0.959 no C27 . H272 . 0.972 no N28 . C29 . 1.492(4) yes N28 . C32 . 1.499(4) yes C29 . C30 . 1.529(5) yes C29 . C31 . 1.518(4) yes C29 . H291 . 1.000 no C30 . H303 . 0.968 no C30 . H302 . 0.968 no C30 . H301 . 0.967 no C31 . H311 . 0.961 no C31 . H313 . 0.972 no C31 . H312 . 0.963 no C32 . C33 . 1.531(5) yes C32 . C34 . 1.517(5) yes C32 . H321 . 0.982 no C33 . H333 . 0.973 no C33 . H332 . 0.959 no C33 . H331 . 0.965 no C34 . H343 . 0.964 no C34 . H342 . 0.967 no C34 . H341 . 0.969 no C35 . C36 . 1.412(4) yes C35 . C43 . 1.414(4) yes C36 . C37 . 1.522(4) yes C36 . C40 . 1.398(4) yes C37 . C38 . 1.538(5) yes C37 . C39 . 1.535(5) yes C37 . H371 . 0.991 no C38 . H382 . 0.977 no C38 . H381 . 0.972 no C38 . H383 . 0.983 no C39 . H393 . 0.963 no C39 . H392 . 0.962 no C39 . H391 . 0.967 no C40 . C41 . 1.387(5) yes C40 . H401 . 0.944 no C41 . C42 . 1.381(5) yes C41 . H411 . 0.946 no C42 . C43 . 1.389(4) yes C42 . H421 . 0.947 no C43 . C44 . 1.526(4) yes C44 . C45 . 1.517(5) yes C44 . C46 . 1.520(5) yes C44 . H441 . 0.990 no C45 . H452 . 0.968 no C45 . H451 . 0.970 no C45 . H453 . 0.954 no C46 . H462 . 0.961 no C46 . H461 . 0.969 no C46 . H463 . 0.959 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 I1 . Al2 . Fe3 . 106.71(3) yes I1 . Al2 . N13 . 108.85(8) yes Fe3 . Al2 . N13 . 132.21(8) yes I1 . Al2 . N15 . 108.27(8) yes Fe3 . Al2 . N15 . 126.08(8) yes N13 . Al2 . N15 . 69.74(10) yes Al2 . Fe3 . C4 . 81.89(12) yes Al2 . Fe3 . C6 . 101.62(11) yes C4 . Fe3 . C6 . 99.54(16) yes Al2 . Fe3 . C7 . 140.95(12) yes C4 . Fe3 . C7 . 103.49(16) yes C6 . Fe3 . C7 . 39.42(16) yes Al2 . Fe3 . C8 . 139.52(12) yes C4 . Fe3 . C8 . 136.65(16) yes C6 . Fe3 . C8 . 66.00(15) yes C7 . Fe3 . C8 . 39.19(15) yes Al2 . Fe3 . C9 . 99.91(11) yes C4 . Fe3 . C9 . 165.55(16) yes C6 . Fe3 . C9 . 66.03(15) yes C7 . Fe3 . C9 . 66.10(15) yes C8 . Fe3 . C9 . 39.61(15) yes Al2 . Fe3 . C10 . 80.08(10) yes C4 . Fe3 . C10 . 128.59(17) yes C6 . Fe3 . C10 . 39.66(15) yes C7 . Fe3 . C10 . 66.26(15) yes C8 . Fe3 . C10 . 66.09(15) yes Al2 . Fe3 . C11 . 97.66(11) yes C4 . Fe3 . C11 . 92.67(17) yes C6 . Fe3 . C11 . 158.41(15) yes C7 . Fe3 . C11 . 120.31(17) yes C8 . Fe3 . C11 . 92.94(16) yes C9 . Fe3 . C10 . 39.08(15) yes C9 . Fe3 . C11 . 101.24(17) yes C10 . Fe3 . C11 . 137.21(17) yes Fe3 . C4 . O5 . 178.4(4) yes Fe3 . C6 . C7 . 70.8(2) yes Fe3 . C6 . C10 . 70.5(2) yes C7 . C6 . C10 . 108.2(3) yes Fe3 . C6 . H61 . 123.8 no C7 . C6 . H61 . 126.4 no C10 . C6 . H61 . 125.4 no Fe3 . C7 . C6 . 69.75(19) yes Fe3 . C7 . C8 . 70.2(2) yes C6 . C7 . C8 . 107.7(3) yes Fe3 . C7 . H71 . 124.7 no C6 . C7 . H71 . 126.1 no C8 . C7 . H71 . 126.1 no Fe3 . C8 . C7 . 70.7(2) yes Fe3 . C8 . C9 . 70.48(19) yes C7 . C8 . C9 . 108.2(3) yes Fe3 . C8 . H81 . 124.1 no C7 . C8 . H81 . 126.3 no C9 . C8 . H81 . 125.4 no Fe3 . C9 . C8 . 69.9(2) yes Fe3 . C9 . C10 . 70.2(2) yes C8 . C9 . C10 . 107.9(3) yes Fe3 . C9 . H91 . 124.6 no C8 . C9 . H91 . 125.3 no C10 . C9 . H91 . 126.8 no Fe3 . C10 . C6 . 69.9(2) yes Fe3 . C10 . C9 . 70.7(2) yes C6 . C10 . C9 . 108.0(3) yes Fe3 . C10 . H101 . 124.6 no C6 . C10 . H101 . 125.9 no C9 . C10 . H101 . 126.1 no Fe3 . C11 . O12 . 173.7(3) yes Al2 . N13 . C14 . 91.37(17) yes Al2 . N13 . C35 . 140.43(19) yes C14 . N13 . C35 . 127.1(2) yes N13 . C14 . N15 . 106.8(2) yes N13 . C14 . N28 . 128.7(3) yes N15 . C14 . N28 . 124.5(2) yes C14 . N15 . Al2 . 92.04(17) yes C14 . N15 . C16 . 131.0(2) yes Al2 . N15 . C16 . 131.31(18) yes N15 . C16 . C17 . 118.2(2) yes N15 . C16 . C24 . 121.4(3) yes C17 . C16 . C24 . 119.9(3) yes C16 . C17 . C18 . 122.9(3) yes C16 . C17 . C21 . 118.7(3) yes C18 . C17 . C21 . 118.4(3) yes C17 . C18 . C19 . 112.2(3) yes C17 . C18 . C20 . 109.9(3) yes C19 . C18 . C20 . 109.3(3) yes C17 . C18 . H181 . 108.0 no C19 . C18 . H181 . 107.8 no C20 . C18 . H181 . 109.6 no C18 . C19 . H191 . 108.6 no C18 . C19 . H193 . 109.4 no H191 . C19 . H193 . 109.5 no C18 . C19 . H192 . 109.8 no H191 . C19 . H192 . 110.2 no H193 . C19 . H192 . 109.4 no C18 . C20 . H201 . 110.4 no C18 . C20 . H203 . 109.0 no H201 . C20 . H203 . 109.0 no C18 . C20 . H202 . 110.0 no H201 . C20 . H202 . 108.5 no H203 . C20 . H202 . 109.9 no C17 . C21 . C22 . 122.1(3) yes C17 . C21 . H211 . 118.3 no C22 . C21 . H211 . 119.7 no C21 . C22 . C23 . 118.8(3) yes C21 . C22 . H221 . 120.4 no C23 . C22 . H221 . 120.8 no C22 . C23 . C24 . 122.1(3) yes C22 . C23 . H231 . 119.0 no C24 . C23 . H231 . 118.9 no C16 . C24 . C23 . 118.3(3) yes C16 . C24 . C25 . 124.3(3) yes C23 . C24 . C25 . 117.4(3) yes C24 . C25 . C26 . 110.0(3) yes C24 . C25 . C27 . 112.3(3) yes C26 . C25 . C27 . 108.9(3) yes C24 . C25 . H251 . 108.4 no C26 . C25 . H251 . 109.3 no C27 . C25 . H251 . 107.9 no C25 . C26 . H261 . 108.8 no C25 . C26 . H263 . 109.1 no H261 . C26 . H263 . 109.1 no C25 . C26 . H262 . 109.8 no H261 . C26 . H262 . 110.1 no H263 . C26 . H262 . 109.9 no C25 . C27 . H271 . 109.2 no C25 . C27 . H273 . 109.2 no H271 . C27 . H273 . 109.9 no C25 . C27 . H272 . 108.3 no H271 . C27 . H272 . 109.7 no H273 . C27 . H272 . 110.4 no C14 . N28 . C29 . 116.3(2) yes C14 . N28 . C32 . 120.5(2) yes C29 . N28 . C32 . 122.0(2) yes N28 . C29 . C30 . 111.2(3) yes N28 . C29 . C31 . 114.5(3) yes C30 . C29 . C31 . 110.9(3) yes N28 . C29 . H291 . 105.9 no C30 . C29 . H291 . 106.6 no C31 . C29 . H291 . 107.1 no C29 . C30 . H303 . 109.6 no C29 . C30 . H302 . 110.0 no H303 . C30 . H302 . 108.8 no C29 . C30 . H301 . 109.8 no H303 . C30 . H301 . 108.6 no H302 . C30 . H301 . 110.0 no C29 . C31 . H311 . 108.8 no C29 . C31 . H313 . 110.4 no H311 . C31 . H313 . 109.3 no C29 . C31 . H312 . 109.8 no H311 . C31 . H312 . 109.3 no H313 . C31 . H312 . 109.3 no N28 . C32 . C33 . 113.6(3) yes N28 . C32 . C34 . 115.2(3) yes C33 . C32 . C34 . 110.3(3) yes N28 . C32 . H321 . 105.9 no C33 . C32 . H321 . 104.9 no C34 . C32 . H321 . 106.0 no C32 . C33 . H333 . 108.1 no C32 . C33 . H332 . 109.3 no H333 . C33 . H332 . 110.0 no C32 . C33 . H331 . 108.6 no H333 . C33 . H331 . 110.5 no H332 . C33 . H331 . 110.4 no C32 . C34 . H343 . 108.4 no C32 . C34 . H342 . 110.1 no H343 . C34 . H342 . 110.0 no C32 . C34 . H341 . 109.6 no H343 . C34 . H341 . 109.6 no H342 . C34 . H341 . 109.2 no N13 . C35 . C36 . 122.2(3) yes N13 . C35 . C43 . 117.4(3) yes C36 . C35 . C43 . 120.4(3) yes C35 . C36 . C37 . 124.1(3) yes C35 . C36 . C40 . 117.7(3) yes C37 . C36 . C40 . 118.0(3) yes C36 . C37 . C38 . 108.7(3) yes C36 . C37 . C39 . 114.7(3) yes C38 . C37 . C39 . 108.4(3) yes C36 . C37 . H371 . 108.6 no C38 . C37 . H371 . 107.8 no C39 . C37 . H371 . 108.4 no C37 . C38 . H382 . 108.6 no C37 . C38 . H381 . 110.0 no H382 . C38 . H381 . 110.2 no C37 . C38 . H383 . 108.4 no H382 . C38 . H383 . 109.0 no H381 . C38 . H383 . 110.6 no C37 . C39 . H393 . 109.5 no C37 . C39 . H392 . 109.5 no H393 . C39 . H392 . 108.7 no C37 . C39 . H391 . 110.3 no H393 . C39 . H391 . 109.6 no H392 . C39 . H391 . 109.1 no C36 . C40 . C41 . 122.1(3) yes C36 . C40 . H401 . 117.8 no C41 . C40 . H401 . 120.1 no C40 . C41 . C42 . 118.9(3) yes C40 . C41 . H411 . 120.6 no C42 . C41 . H411 . 120.5 no C41 . C42 . C43 . 121.7(3) yes C41 . C42 . H421 . 119.3 no C43 . C42 . H421 . 119.0 no C35 . C43 . C42 . 118.6(3) yes C35 . C43 . C44 . 122.0(3) yes C42 . C43 . C44 . 119.4(3) yes C43 . C44 . C45 . 113.4(3) yes C43 . C44 . C46 . 111.5(3) yes C45 . C44 . C46 . 110.1(3) yes C43 . C44 . H441 . 106.6 no C45 . C44 . H441 . 106.8 no C46 . C44 . H441 . 108.2 no C44 . C45 . H452 . 110.4 no C44 . C45 . H451 . 109.0 no H452 . C45 . H451 . 110.5 no C44 . C45 . H453 . 109.2 no H452 . C45 . H453 . 108.8 no H451 . C45 . H453 . 109.0 no C44 . C46 . H462 . 109.2 no C44 . C46 . H461 . 109.7 no H462 . C46 . H461 . 110.9 no C44 . C46 . H463 . 106.9 no H462 . C46 . H463 . 110.2 no H461 . C46 . H463 . 109.9 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 C25 . H251 . C14 . 134.34 0.988 2.525 3.292(5) yes C29 . H291 . C16 . 137.50 1.000 2.331 3.142(5) yes C32 . H321 . C35 . 129.98 0.982 2.264 2.992(5) yes C32 . H321 . C43 . 164.50 0.982 2.459 3.415(5) yes _iucr_refine_instruction_details_constraints ; # # Punched on 15/12/11 at 13:32:18 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 193,X'S) H ( 192,X'S) RIDE C ( 20,X'S) H ( 201,X'S) H ( 203,X'S) H ( 202,X'S) RIDE C ( 21,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 231,X'S) RIDE C ( 25,X'S) H ( 251,X'S) RIDE C ( 26,X'S) H ( 261,X'S) H ( 263,X'S) H ( 262,X'S) RIDE C ( 27,X'S) H ( 271,X'S) H ( 273,X'S) H ( 272,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 303,X'S) H ( 302,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) H ( 313,X'S) H ( 312,X'S) RIDE C ( 32,X'S) H ( 321,X'S) RIDE C ( 33,X'S) H ( 333,X'S) H ( 332,X'S) H ( 331,X'S) RIDE C ( 34,X'S) H ( 343,X'S) H ( 342,X'S) H ( 341,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H ( 382,X'S) H ( 381,X'S) H ( 383,X'S) RIDE C ( 39,X'S) H ( 393,X'S) H ( 392,X'S) H ( 391,X'S) RIDE C ( 40,X'S) H ( 401,X'S) RIDE C ( 41,X'S) H ( 411,X'S) RIDE C ( 42,X'S) H ( 421,X'S) RIDE C ( 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 452,X'S) H ( 451,X'S) H ( 453,X'S) RIDE C ( 46,X'S) H ( 462,X'S) H ( 461,X'S) H ( 463,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 15/12/11 at 13:32:18 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; data_6 _database_code_depnum_ccdc_archive 'CCDC 894964' #TrackingRef 'Combined Final VRFs.cif' #============================================================================== _audit_creation_date 11-08-07 _audit_creation_method CRYSTALS_ver_14.06 _oxford_structure_analysis_title '8071311 062irmk11' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.24130(10) _cell_length_b 20.2466(2) _cell_length_c 17.08450(10) _cell_angle_alpha 90 _cell_angle_beta 90.4148(4) _cell_angle_gamma 90 _cell_volume 3888.30(6) _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' 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' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 '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' 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' 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 = C32 H56 Al1 Cl1 Fe1 N2 O2 # Dc = 1.06 Fooo = 1552.00 Mu = 5.05 M = 619.09 # Found Formula = C41 H56 Al1 Cl1 Fe1 N2 O2 # Dc = 1.24 FOOO = 1552.00 Mu = 5.15 M = 727.19 _chemical_formula_sum 'C41 H56 Al1 Cl1 Fe1 N2 O2' _chemical_formula_moiety 'C41 H56 Al1 Cl1 Fe1 N2 O2' _chemical_compound_source ? _chemical_formula_weight 727.19 _cell_measurement_reflns_used 9084 _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 0.150 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_max 0.180 _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.515 # Sheldrick geometric approximatio 0.91 0.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.93 # 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 101655 _reflns_number_total 8860 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections without Friedels Law is 15821 # Number of reflections with Friedels Law is 8860 # Theoretical number of reflections is about 8914 _diffrn_reflns_theta_min 5.175 _diffrn_reflns_theta_max 27.479 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.479 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _oxford_diffrn_Wilson_B_factor 1.99 _oxford_diffrn_Wilson_scale 12.74 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.68 _refine_diff_density_max 0.77 # 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 8860 _refine_ls_number_restraints 0 _refine_ls_number_parameters 434 _oxford_refine_ls_R_factor_ref 0.0615 _refine_ls_wR_factor_ref 0.1397 _refine_ls_goodness_of_fit_ref 1.0072 _refine_ls_shift/su_max 0.0014020 _refine_ls_shift/su_mean 0.0000659 # The values computed from all data _oxford_reflns_number_all 8860 _refine_ls_R_factor_all 0.0615 _refine_ls_wR_factor_all 0.1397 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6821 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_gt 0.1276 # 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 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 Fe1 Fe 0.54025(2) 0.746106(12) 0.413011(15) 0.0245 1.0000 Uani . . . . . . . Al2 Al 0.72254(5) 0.75751(2) 0.49451(3) 0.0199 1.0000 Uani . . . . . . . Cl3 Cl 0.67451(4) 0.76028(2) 0.61900(2) 0.0266 1.0000 Uani . . . . . . . N4 N 0.85573(13) 0.69503(7) 0.50212(8) 0.0234 1.0000 Uani . . . . . . . C5 C 0.83698(15) 0.62509(8) 0.49012(10) 0.0252 1.0000 Uani . . . . . . . C6 C 0.81755(16) 0.58252(9) 0.55450(11) 0.0299 1.0000 Uani . . . . . . . C7 C 0.79163(18) 0.51615(9) 0.53762(13) 0.0367 1.0000 Uani . . . . . . . C8 C 0.78906(18) 0.49288(9) 0.46159(13) 0.0386 1.0000 Uani . . . . . . . C9 C 0.81622(18) 0.53415(9) 0.40013(12) 0.0349 1.0000 Uani . . . . . . . C10 C 0.84092(16) 0.60099(9) 0.41277(11) 0.0297 1.0000 Uani . . . . . . . C11 C 0.87895(19) 0.64530(10) 0.34557(11) 0.0336 1.0000 Uani . . . . . . . C12 C 0.8384(2) 0.62002(11) 0.26504(12) 0.0456 1.0000 Uani . . . . . . . C13 C 1.0137(2) 0.65501(12) 0.34343(13) 0.0460 1.0000 Uani . . . . . . . C14 C 0.83137(17) 0.60283(10) 0.64002(11) 0.0329 1.0000 Uani . . . . . . . C15 C 0.9307(2) 0.56225(12) 0.68070(14) 0.0463 1.0000 Uani . . . . . . . C16 C 0.71766(19) 0.59561(10) 0.68719(11) 0.0372 1.0000 Uani . . . . . . . C17 C 0.96298(16) 0.71432(9) 0.52846(10) 0.0262 1.0000 Uani . . . . . . . C18 C 0.99483(16) 0.78002(9) 0.53955(11) 0.0279 1.0000 Uani . . . . . . . C19 C 0.93421(16) 0.83617(8) 0.51536(10) 0.0255 1.0000 Uani . . . . . . . N20 N 0.82388(12) 0.83520(7) 0.48536(8) 0.0215 1.0000 Uani . . . . . . . C21 C 0.78108(15) 0.89894(8) 0.45725(10) 0.0216 1.0000 Uani . . . . . . . C22 C 0.79114(16) 0.91405(9) 0.37705(10) 0.0257 1.0000 Uani . . . . . . . C23 C 0.75759(18) 0.97661(9) 0.35253(11) 0.0321 1.0000 Uani . . . . . . . C24 C 0.71255(19) 1.02298(9) 0.40399(12) 0.0348 1.0000 Uani . . . . . . . C25 C 0.70045(18) 1.00677(9) 0.48201(11) 0.0318 1.0000 Uani . . . . . . . C26 C 0.73540(16) 0.94503(8) 0.51047(10) 0.0263 1.0000 Uani . . . . . . . C27 C 0.72251(18) 0.93148(9) 0.59768(10) 0.0317 1.0000 Uani . . . . . . . C28 C 0.5908(2) 0.92641(11) 0.61939(13) 0.0438 1.0000 Uani . . . . . . . C29 C 0.7828(2) 0.98426(11) 0.64829(12) 0.0487 1.0000 Uani . . . . . . . C30 C 0.83997(17) 0.86402(9) 0.31927(10) 0.0303 1.0000 Uani . . . . . . . C31 C 0.7859(2) 0.87237(11) 0.23648(11) 0.0440 1.0000 Uani . . . . . . . C32 C 0.9745(2) 0.86649(13) 0.31418(14) 0.0481 1.0000 Uani . . . . . . . C33 C 1.00330(18) 0.89993(9) 0.52293(13) 0.0373 1.0000 Uani . . . . . . . C34 C 1.06048(18) 0.66518(10) 0.54585(13) 0.0356 1.0000 Uani . . . . . . . C35 C 0.62324(19) 0.74117(9) 0.32757(12) 0.0315 1.0000 Uani . . . . . . . O36 O 0.66356(16) 0.73704(8) 0.26566(9) 0.0471 1.0000 Uani . . . . . . . C37 C 0.35170(18) 0.74496(9) 0.41172(14) 0.0344 1.0000 Uani . . . . . . . C38 C 0.39535(16) 0.72951(10) 0.48906(11) 0.0306 1.0000 Uani . . . . . . . C39 C 0.46208(17) 0.67037(9) 0.48339(12) 0.0309 1.0000 Uani . . . . . . . C40 C 0.46399(17) 0.65004(9) 0.40428(12) 0.0346 1.0000 Uani . . . . . . . C41 C 0.39427(18) 0.69657(11) 0.35937(12) 0.0385 1.0000 Uani . . . . . . . C42 C 0.3663(2) 0.69104(15) 0.27337(13) 0.0601 1.0000 Uani . . . . . . . C43 C 0.5019(2) 0.62848(11) 0.55142(14) 0.0439 1.0000 Uani . . . . . . . C44 C 0.3640(2) 0.76616(12) 0.56221(14) 0.0424 1.0000 Uani . . . . . . . C45 C 0.2669(2) 0.79992(12) 0.39135(17) 0.0547 1.0000 Uani . . . . . . . C46 C 0.53459(16) 0.83188(10) 0.41792(11) 0.0312 1.0000 Uani . . . . . . . O47 O 0.51216(14) 0.88805(7) 0.41704(10) 0.0444 1.0000 Uani . . . . . . . C3 C 0.5144(2) 0.58657(11) 0.37467(16) 0.0516 1.0000 Uani . . . . . . . H71 H 0.7792 0.4871 0.5793 0.0432 1.0000 Uiso R . . . . . . H81 H 0.7697 0.4486 0.4522 0.0460 1.0000 Uiso R . . . . . . H91 H 0.8182 0.5169 0.3486 0.0430 1.0000 Uiso R . . . . . . H111 H 0.8439 0.6901 0.3540 0.0401 1.0000 Uiso R . . . . . . H122 H 0.8550 0.6539 0.2269 0.0705 1.0000 Uiso R . . . . . . H121 H 0.8824 0.5814 0.2499 0.0677 1.0000 Uiso R . . . . . . H123 H 0.7545 0.6103 0.2638 0.0687 1.0000 Uiso R . . . . . . H131 H 1.0329 0.6793 0.2973 0.0684 1.0000 Uiso R . . . . . . H133 H 1.0404 0.6777 0.3880 0.0679 1.0000 Uiso R . . . . . . H132 H 1.0502 0.6113 0.3417 0.0692 1.0000 Uiso R . . . . . . H141 H 0.8562 0.6500 0.6400 0.0377 1.0000 Uiso R . . . . . . H152 H 0.9499 0.5799 0.7306 0.0680 1.0000 Uiso R . . . . . . H151 H 0.9996 0.5626 0.6504 0.0674 1.0000 Uiso R . . . . . . H153 H 0.9048 0.5174 0.6874 0.0694 1.0000 Uiso R . . . . . . H161 H 0.7358 0.6022 0.7435 0.0546 1.0000 Uiso R . . . . . . H163 H 0.6600 0.6283 0.6712 0.0547 1.0000 Uiso R . . . . . . H162 H 0.6869 0.5525 0.6814 0.0554 1.0000 Uiso R . . . . . . H181 H 1.0670 0.7874 0.5637 0.0341 1.0000 Uiso R . . . . . . H231 H 0.7671 0.9878 0.3006 0.0388 1.0000 Uiso R . . . . . . H241 H 0.6876 1.0664 0.3854 0.0420 1.0000 Uiso R . . . . . . H251 H 0.6661 1.0383 0.5163 0.0376 1.0000 Uiso R . . . . . . H271 H 0.7599 0.8900 0.6111 0.0373 1.0000 Uiso R . . . . . . H282 H 0.5837 0.9153 0.6730 0.0646 1.0000 Uiso R . . . . . . H281 H 0.5516 0.9682 0.6099 0.0644 1.0000 Uiso R . . . . . . H283 H 0.5526 0.8907 0.5870 0.0635 1.0000 Uiso R . . . . . . H292 H 0.7799 0.9736 0.7042 0.0716 1.0000 Uiso R . . . . . . H291 H 0.7448 1.0282 0.6425 0.0720 1.0000 Uiso R . . . . . . H293 H 0.8667 0.9893 0.6339 0.0733 1.0000 Uiso R . . . . . . H301 H 0.8193 0.8209 0.3389 0.0355 1.0000 Uiso R . . . . . . H312 H 0.8117 0.8347 0.2055 0.0659 1.0000 Uiso R . . . . . . H311 H 0.8152 0.9140 0.2118 0.0649 1.0000 Uiso R . . . . . . H313 H 0.6977 0.8744 0.2377 0.0655 1.0000 Uiso R . . . . . . H322 H 1.0034 0.8335 0.2776 0.0722 1.0000 Uiso R . . . . . . H321 H 0.9999 0.9106 0.2975 0.0716 1.0000 Uiso R . . . . . . H323 H 1.0105 0.8571 0.3635 0.0709 1.0000 Uiso R . . . . . . H331 H 0.9886 0.9287 0.4813 0.0572 1.0000 Uiso R . . . . . . H333 H 0.9818 0.9222 0.5698 0.0591 1.0000 Uiso R . . . . . . H332 H 1.0859 0.8919 0.5250 0.0570 1.0000 Uiso R . . . . . . H341 H 1.1343 0.6771 0.5200 0.0531 1.0000 Uiso R . . . . . . H343 H 1.0751 0.6633 0.6012 0.0533 1.0000 Uiso R . . . . . . H342 H 1.0375 0.6196 0.5275 0.0534 1.0000 Uiso R . . . . . . H421 H 0.4329 0.6713 0.2448 0.0890 1.0000 Uiso R . . . . . . H422 H 0.3473 0.7338 0.2498 0.0896 1.0000 Uiso R . . . . . . H423 H 0.2958 0.6637 0.2687 0.0892 1.0000 Uiso R . . . . . . H431 H 0.5770 0.6083 0.5404 0.0651 1.0000 Uiso R . . . . . . H432 H 0.5108 0.6547 0.5994 0.0668 1.0000 Uiso R . . . . . . H433 H 0.4424 0.5936 0.5590 0.0667 1.0000 Uiso R . . . . . . H441 H 0.4280 0.7636 0.5985 0.0641 1.0000 Uiso R . . . . . . H442 H 0.3497 0.8106 0.5489 0.0657 1.0000 Uiso R . . . . . . H443 H 0.2914 0.7458 0.5832 0.0627 1.0000 Uiso R . . . . . . H452 H 0.2758 0.8121 0.3370 0.0823 1.0000 Uiso R . . . . . . H451 H 0.2810 0.8373 0.4238 0.0814 1.0000 Uiso R . . . . . . H453 H 0.1863 0.7859 0.4006 0.0819 1.0000 Uiso R . . . . . . H32 H 0.5410 0.5926 0.3213 0.0774 1.0000 Uiso R . . . . . . H31 H 0.5831 0.5723 0.4063 0.0773 1.0000 Uiso R . . . . . . H33 H 0.4514 0.5520 0.3743 0.0763 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 Fe1 0.02133(17) 0.02508(16) 0.02696(17) 0.00014(9) -0.00516(11) -0.00086(9) Al2 0.0184(3) 0.0206(2) 0.0207(3) -0.00076(18) -0.0018(2) 0.00037(18) Cl3 0.0273(2) 0.0301(2) 0.0224(2) -0.00067(15) 0.00161(18) 0.00012(16) N4 0.0222(7) 0.0231(7) 0.0249(7) 0.0004(6) 0.0009(6) 0.0011(6) C5 0.0216(9) 0.0202(8) 0.0339(9) -0.0005(7) 0.0015(7) 0.0043(6) C6 0.0235(9) 0.0264(8) 0.0398(10) 0.0058(8) 0.0038(8) 0.0057(7) C7 0.0314(10) 0.0230(9) 0.0557(12) 0.0074(9) 0.0044(9) 0.0049(8) C8 0.0325(11) 0.0192(8) 0.0639(13) -0.0055(9) 0.0004(10) 0.0008(7) C9 0.0327(10) 0.0276(9) 0.0446(11) -0.0093(8) 0.0011(9) 0.0031(8) C10 0.0241(9) 0.0302(9) 0.0348(10) -0.0045(8) 0.0026(8) 0.0039(7) C11 0.0401(11) 0.0318(9) 0.0291(9) -0.0061(7) 0.0071(8) 0.0000(8) C12 0.0555(15) 0.0452(12) 0.0362(11) -0.0123(9) 0.0070(10) -0.0020(10) C13 0.0441(13) 0.0525(13) 0.0415(12) -0.0066(10) 0.0126(10) -0.0072(10) C14 0.0324(10) 0.0313(9) 0.0349(10) 0.0089(8) 0.0004(8) 0.0062(8) C15 0.0382(12) 0.0515(13) 0.0491(12) 0.0129(11) -0.0020(10) 0.0094(10) C16 0.0398(11) 0.0364(10) 0.0354(10) 0.0116(8) 0.0024(9) 0.0073(9) C17 0.0218(9) 0.0268(9) 0.0298(9) 0.0014(7) 0.0004(7) 0.0027(7) C18 0.0216(9) 0.0270(9) 0.0349(10) 0.0003(7) -0.0077(7) 0.0009(7) C19 0.0225(9) 0.0246(8) 0.0295(9) -0.0027(7) 0.0008(7) -0.0058(7) N20 0.0209(7) 0.0212(7) 0.0225(7) -0.0016(5) -0.0004(6) 0.0008(5) C21 0.0203(8) 0.0153(7) 0.0291(8) -0.0016(6) 0.0003(7) -0.0007(6) C22 0.0229(9) 0.0267(8) 0.0276(9) -0.0013(7) 0.0025(7) -0.0016(7) C23 0.0353(11) 0.0317(9) 0.0293(9) 0.0053(8) 0.0023(8) 0.0027(8) C24 0.0389(11) 0.0250(9) 0.0404(10) 0.0035(8) 0.0013(9) 0.0031(8) C25 0.0327(10) 0.0240(9) 0.0388(10) -0.0032(7) 0.0016(8) 0.0067(7) C26 0.0262(9) 0.0217(8) 0.0309(9) -0.0018(7) 0.0007(7) -0.0017(7) C27 0.0431(12) 0.0248(9) 0.0272(9) -0.0046(7) 0.0027(8) 0.0029(8) C28 0.0475(13) 0.0407(11) 0.0434(12) 0.0056(9) 0.0178(10) 0.0123(10) C29 0.0783(18) 0.0373(11) 0.0304(10) -0.0097(9) -0.0069(11) -0.0052(11) C30 0.0353(10) 0.0284(9) 0.0275(9) 0.0018(7) 0.0067(8) 0.0002(8) C31 0.0634(15) 0.0415(11) 0.0271(10) -0.0011(8) -0.0012(10) 0.0090(11) C32 0.0357(12) 0.0609(14) 0.0480(12) -0.0064(11) 0.0121(10) 0.0090(11) C33 0.0293(10) 0.0254(9) 0.0570(13) -0.0024(9) -0.0098(9) -0.0068(8) C34 0.0247(9) 0.0333(10) 0.0489(11) 0.0044(9) -0.0058(8) 0.0097(8) C35 0.0334(11) 0.0296(9) 0.0313(10) -0.0043(7) -0.0068(9) -0.0040(8) O36 0.0517(10) 0.0548(10) 0.0347(9) -0.0071(7) 0.0025(8) -0.0049(8) C37 0.0185(9) 0.0347(10) 0.0497(12) 0.0086(8) -0.0062(9) -0.0034(7) C38 0.0206(9) 0.0333(9) 0.0378(10) 0.0006(8) -0.0001(8) -0.0032(7) C39 0.0226(9) 0.0293(9) 0.0407(10) 0.0045(8) -0.0061(8) -0.0056(7) C40 0.0243(9) 0.0303(9) 0.0491(11) -0.0045(8) -0.0054(8) -0.0084(7) C41 0.0285(10) 0.0444(11) 0.0423(11) 0.0016(9) -0.0108(9) -0.0095(9) C42 0.0579(16) 0.083(2) 0.0392(12) -0.0014(12) -0.0207(12) -0.0193(14) C43 0.0308(11) 0.0441(12) 0.0566(13) 0.0190(10) -0.0077(10) -0.0084(9) C44 0.0325(11) 0.0472(12) 0.0478(12) -0.0059(10) 0.0089(10) -0.0055(9) C45 0.0296(12) 0.0481(13) 0.0862(18) 0.0176(13) -0.0100(12) 0.0032(10) C46 0.0201(9) 0.0367(11) 0.0367(10) 0.0006(8) -0.0043(8) -0.0010(7) O47 0.0347(8) 0.0266(7) 0.0719(11) -0.0010(7) -0.0064(7) 0.0048(6) C3 0.0415(13) 0.0360(11) 0.0773(17) -0.0182(11) 0.0004(12) -0.0077(10) _refine_ls_extinction_coef 50(80) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.2498(2) 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 Fe1 . Al2 . 2.4799(5) yes Fe1 . C35 . 1.741(2) yes Fe1 . C37 . 2.120(2) yes Fe1 . C38 . 2.1178(19) yes Fe1 . C39 . 2.1411(19) yes Fe1 . C40 . 2.1303(19) yes Fe1 . C41 . 2.1254(19) yes Fe1 . C46 . 1.740(2) yes Al2 . Cl3 . 2.1988(7) yes Al2 . N4 . 1.9637(15) yes Al2 . N20 . 1.9491(15) yes N4 . C5 . 1.446(2) yes N4 . C17 . 1.342(2) yes C5 . C6 . 1.416(3) yes C5 . C10 . 1.410(3) yes C6 . C7 . 1.404(3) yes C6 . C14 . 1.525(3) yes C7 . C8 . 1.382(3) yes C7 . H71 . 0.935 no C8 . C9 . 1.378(3) yes C8 . H81 . 0.937 no C9 . C10 . 1.398(3) yes C9 . H91 . 0.947 no C10 . C11 . 1.521(3) yes C11 . C12 . 1.534(3) yes C11 . C13 . 1.529(3) yes C11 . H111 . 0.999 no C12 . H122 . 0.965 no C12 . H121 . 0.962 no C12 . H123 . 0.963 no C13 . H131 . 0.954 no C13 . H133 . 0.937 no C13 . H132 . 0.976 no C14 . C15 . 1.547(3) yes C14 . C16 . 1.523(3) yes C14 . H141 . 0.995 no C15 . H152 . 0.948 no C15 . H151 . 0.935 no C15 . H153 . 0.960 no C16 . H161 . 0.990 no C16 . H163 . 0.965 no C16 . H162 . 0.943 no C17 . C18 . 1.390(2) yes C17 . C34 . 1.508(2) yes C18 . C19 . 1.387(2) yes C18 . H181 . 0.920 no C19 . N20 . 1.339(2) yes C19 . C33 . 1.512(2) yes N20 . C21 . 1.457(2) yes C21 . C22 . 1.409(2) yes C21 . C26 . 1.403(2) yes C22 . C23 . 1.386(2) yes C22 . C30 . 1.520(2) yes C23 . C24 . 1.385(3) yes C23 . H231 . 0.922 no C24 . C25 . 1.381(3) yes C24 . H241 . 0.976 no C25 . C26 . 1.397(2) yes C25 . H251 . 0.950 no C26 . C27 . 1.523(2) yes C27 . C28 . 1.532(3) yes C27 . C29 . 1.530(3) yes C27 . H271 . 0.967 no C28 . H282 . 0.947 no C28 . H281 . 0.968 no C28 . H283 . 1.005 no C29 . H292 . 0.980 no C29 . H291 . 0.992 no C29 . H293 . 0.981 no C30 . C31 . 1.545(3) yes C30 . C32 . 1.517(3) yes C30 . H301 . 0.965 no C31 . H312 . 0.973 no C31 . H311 . 0.999 no C31 . H313 . 0.992 no C32 . H322 . 0.972 no C32 . H321 . 0.981 no C32 . H323 . 0.952 no C33 . H331 . 0.933 no C33 . H333 . 0.952 no C33 . H332 . 0.943 no C34 . H341 . 0.973 no C34 . H343 . 0.959 no C34 . H342 . 1.008 no C35 . O36 . 1.157(3) yes C37 . C38 . 1.440(3) yes C37 . C41 . 1.413(3) yes C37 . C45 . 1.504(3) yes C38 . C39 . 1.417(3) yes C38 . C44 . 1.498(3) yes C39 . C40 . 1.413(3) yes C39 . C43 . 1.504(3) yes C40 . C41 . 1.443(3) yes C40 . C3 . 1.494(3) yes C41 . C42 . 1.504(3) yes C42 . H421 . 0.981 no C42 . H422 . 0.978 no C42 . H423 . 0.970 no C43 . H431 . 0.956 no C43 . H432 . 0.982 no C43 . H433 . 0.982 no C44 . H441 . 0.948 no C44 . H442 . 0.941 no C44 . H443 . 0.985 no C45 . H452 . 0.966 no C45 . H451 . 0.950 no C45 . H453 . 0.963 no C46 . O47 . 1.165(2) yes C3 . H32 . 0.969 no C3 . H31 . 0.983 no C3 . H33 . 0.995 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 Al2 . Fe1 . C35 . 91.74(7) yes Al2 . Fe1 . C37 . 146.00(6) yes C35 . Fe1 . C37 . 122.18(9) yes Al2 . Fe1 . C38 . 107.85(5) yes C35 . Fe1 . C38 . 157.60(8) yes C37 . Fe1 . C38 . 39.75(8) yes Al2 . Fe1 . C39 . 95.29(5) yes C35 . Fe1 . C39 . 130.87(8) yes C37 . Fe1 . C39 . 65.39(7) yes C38 . Fe1 . C39 . 38.85(7) yes Al2 . Fe1 . C40 . 117.05(5) yes C35 . Fe1 . C40 . 96.13(8) yes C37 . Fe1 . C40 . 65.63(7) yes C38 . Fe1 . C40 . 65.62(8) yes C39 . Fe1 . C40 . 38.64(8) yes Al2 . Fe1 . C41 . 156.69(6) yes C35 . Fe1 . C41 . 91.61(9) yes C37 . Fe1 . C41 . 38.87(8) yes C38 . Fe1 . C41 . 66.09(8) yes C39 . Fe1 . C41 . 65.51(7) yes Al2 . Fe1 . C46 . 84.86(6) yes C35 . Fe1 . C46 . 96.76(9) yes C37 . Fe1 . C46 . 88.54(8) yes C38 . Fe1 . C46 . 95.76(9) yes C39 . Fe1 . C46 . 132.26(9) yes C40 . Fe1 . C41 . 39.64(8) yes C40 . Fe1 . C46 . 154.14(8) yes C41 . Fe1 . C46 . 117.61(8) yes Fe1 . Al2 . Cl3 . 109.74(3) yes Fe1 . Al2 . N4 . 127.14(5) yes Cl3 . Al2 . N4 . 98.32(5) yes Fe1 . Al2 . N20 . 120.74(5) yes Cl3 . Al2 . N20 . 101.81(5) yes N4 . Al2 . N20 . 94.55(6) yes Al2 . N4 . C5 . 120.74(11) yes Al2 . N4 . C17 . 121.16(12) yes C5 . N4 . C17 . 117.54(14) yes N4 . C5 . C6 . 120.62(15) yes N4 . C5 . C10 . 117.80(15) yes C6 . C5 . C10 . 121.57(16) yes C5 . C6 . C7 . 117.13(18) yes C5 . C6 . C14 . 124.40(16) yes C7 . C6 . C14 . 118.32(17) yes C6 . C7 . C8 . 121.48(19) yes C6 . C7 . H71 . 118.5 no C8 . C7 . H71 . 120.0 no C7 . C8 . C9 . 120.42(18) yes C7 . C8 . H81 . 119.4 no C9 . C8 . H81 . 120.2 no C8 . C9 . C10 . 120.94(19) yes C8 . C9 . H91 . 119.5 no C10 . C9 . H91 . 119.6 no C5 . C10 . C9 . 118.19(18) yes C5 . C10 . C11 . 120.95(16) yes C9 . C10 . C11 . 120.74(17) yes C10 . C11 . C12 . 113.36(17) yes C10 . C11 . C13 . 112.21(17) yes C12 . C11 . C13 . 108.06(17) yes C10 . C11 . H111 . 108.3 no C12 . C11 . H111 . 108.4 no C13 . C11 . H111 . 106.2 no C11 . C12 . H122 . 108.1 no C11 . C12 . H121 . 111.2 no H122 . C12 . H121 . 107.1 no C11 . C12 . H123 . 111.8 no H122 . C12 . H123 . 109.0 no H121 . C12 . H123 . 109.5 no C11 . C13 . H131 . 108.4 no C11 . C13 . H133 . 110.8 no H131 . C13 . H133 . 110.2 no C11 . C13 . H132 . 107.5 no H131 . C13 . H132 . 110.1 no H133 . C13 . H132 . 109.7 no C6 . C14 . C15 . 110.82(16) yes C6 . C14 . C16 . 113.64(16) yes C15 . C14 . C16 . 108.48(16) yes C6 . C14 . H141 . 106.6 no C15 . C14 . H141 . 108.0 no C16 . C14 . H141 . 109.2 no C14 . C15 . H152 . 111.3 no C14 . C15 . H151 . 110.2 no H152 . C15 . H151 . 108.1 no C14 . C15 . H153 . 109.7 no H152 . C15 . H153 . 108.5 no H151 . C15 . H153 . 109.0 no C14 . C16 . H161 . 109.5 no C14 . C16 . H163 . 110.4 no H161 . C16 . H163 . 108.4 no C14 . C16 . H162 . 110.0 no H161 . C16 . H162 . 107.4 no H163 . C16 . H162 . 111.1 no N4 . C17 . C18 . 123.66(16) yes N4 . C17 . C34 . 121.59(16) yes C18 . C17 . C34 . 114.73(16) yes C17 . C18 . C19 . 128.18(16) yes C17 . C18 . H181 . 116.3 no C19 . C18 . H181 . 115.4 no C18 . C19 . N20 . 123.64(15) yes C18 . C19 . C33 . 115.06(16) yes N20 . C19 . C33 . 121.28(16) yes C19 . N20 . Al2 . 121.43(11) yes C19 . N20 . C21 . 114.58(13) yes Al2 . N20 . C21 . 123.31(11) yes N20 . C21 . C22 . 118.95(14) yes N20 . C21 . C26 . 119.80(15) yes C22 . C21 . C26 . 121.20(15) yes C21 . C22 . C23 . 117.97(16) yes C21 . C22 . C30 . 121.25(15) yes C23 . C22 . C30 . 120.77(16) yes C22 . C23 . C24 . 121.86(17) yes C22 . C23 . H231 . 118.9 no C24 . C23 . H231 . 119.2 no C23 . C24 . C25 . 119.40(17) yes C23 . C24 . H241 . 120.7 no C25 . C24 . H241 . 119.9 no C24 . C25 . C26 . 121.30(17) yes C24 . C25 . H251 . 118.6 no C26 . C25 . H251 . 120.1 no C21 . C26 . C25 . 118.24(16) yes C21 . C26 . C27 . 123.51(15) yes C25 . C26 . C27 . 118.25(16) yes C26 . C27 . C28 . 110.36(16) yes C26 . C27 . C29 . 112.46(16) yes C28 . C27 . C29 . 109.57(17) yes C26 . C27 . H271 . 110.2 no C28 . C27 . H271 . 107.7 no C29 . C27 . H271 . 106.4 no C27 . C28 . H282 . 109.8 no C27 . C28 . H281 . 109.9 no H282 . C28 . H281 . 109.1 no C27 . C28 . H283 . 108.9 no H282 . C28 . H283 . 108.9 no H281 . C28 . H283 . 110.1 no C27 . C29 . H292 . 112.3 no C27 . C29 . H291 . 112.5 no H292 . C29 . H291 . 106.0 no C27 . C29 . H293 . 110.7 no H292 . C29 . H293 . 107.9 no H291 . C29 . H293 . 107.2 no C22 . C30 . C31 . 112.35(16) yes C22 . C30 . C32 . 112.36(16) yes C31 . C30 . C32 . 109.27(17) yes C22 . C30 . H301 . 106.7 no C31 . C30 . H301 . 108.9 no C32 . C30 . H301 . 107.0 no C30 . C31 . H312 . 107.1 no C30 . C31 . H311 . 110.5 no H312 . C31 . H311 . 109.3 no C30 . C31 . H313 . 111.8 no H312 . C31 . H313 . 110.2 no H311 . C31 . H313 . 107.8 no C30 . C32 . H322 . 110.6 no C30 . C32 . H321 . 109.8 no H322 . C32 . H321 . 109.9 no C30 . C32 . H323 . 111.1 no H322 . C32 . H323 . 106.8 no H321 . C32 . H323 . 108.5 no C19 . C33 . H331 . 112.3 no C19 . C33 . H333 . 110.1 no H331 . C33 . H333 . 107.5 no C19 . C33 . H332 . 111.2 no H331 . C33 . H332 . 107.8 no H333 . C33 . H332 . 107.8 no C17 . C34 . H341 . 111.6 no C17 . C34 . H343 . 109.8 no H341 . C34 . H343 . 108.4 no C17 . C34 . H342 . 111.0 no H341 . C34 . H342 . 107.6 no H343 . C34 . H342 . 108.3 no Fe1 . C35 . O36 . 170.65(18) yes Fe1 . C37 . C38 . 70.06(10) yes Fe1 . C37 . C41 . 70.78(12) yes C38 . C37 . C41 . 108.39(17) yes Fe1 . C37 . C45 . 128.78(15) yes C38 . C37 . C45 . 125.7(2) yes C41 . C37 . C45 . 125.7(2) yes Fe1 . C38 . C37 . 70.19(11) yes Fe1 . C38 . C39 . 71.46(11) yes C37 . C38 . C39 . 107.33(17) yes Fe1 . C38 . C44 . 128.31(14) yes C37 . C38 . C44 . 125.25(19) yes C39 . C38 . C44 . 127.14(19) yes Fe1 . C39 . C38 . 69.68(11) yes Fe1 . C39 . C40 . 70.27(11) yes C38 . C39 . C40 . 108.86(16) yes Fe1 . C39 . C43 . 135.77(13) yes C38 . C39 . C43 . 125.35(19) yes C40 . C39 . C43 . 124.62(19) yes Fe1 . C40 . C39 . 71.09(10) yes Fe1 . C40 . C41 . 70.00(11) yes C39 . C40 . C41 . 107.85(18) yes Fe1 . C40 . C3 . 130.96(15) yes C39 . C40 . C3 . 125.65(19) yes C41 . C40 . C3 . 126.0(2) yes Fe1 . C41 . C40 . 70.37(10) yes Fe1 . C41 . C37 . 70.34(11) yes C40 . C41 . C37 . 107.53(18) yes Fe1 . C41 . C42 . 127.69(16) yes C40 . C41 . C42 . 125.4(2) yes C37 . C41 . C42 . 126.9(2) yes C41 . C42 . H421 . 111.2 no C41 . C42 . H422 . 112.3 no H421 . C42 . H422 . 108.7 no C41 . C42 . H423 . 106.7 no H421 . C42 . H423 . 110.7 no H422 . C42 . H423 . 107.1 no C39 . C43 . H431 . 110.3 no C39 . C43 . H432 . 111.6 no H431 . C43 . H432 . 108.0 no C39 . C43 . H433 . 107.9 no H431 . C43 . H433 . 108.8 no H432 . C43 . H433 . 110.1 no C38 . C44 . H441 . 109.7 no C38 . C44 . H442 . 108.3 no H441 . C44 . H442 . 109.7 no C38 . C44 . H443 . 107.3 no H441 . C44 . H443 . 111.5 no H442 . C44 . H443 . 110.3 no C37 . C45 . H452 . 110.0 no C37 . C45 . H451 . 110.5 no H452 . C45 . H451 . 109.8 no C37 . C45 . H453 . 109.8 no H452 . C45 . H453 . 109.7 no H451 . C45 . H453 . 107.0 no Fe1 . C46 . O47 . 169.06(16) yes C40 . C3 . H32 . 109.3 no C40 . C3 . H31 . 111.5 no H32 . C3 . H31 . 107.9 no C40 . C3 . H33 . 109.6 no H32 . C3 . H33 . 107.8 no H31 . C3 . H33 . 110.7 no data_7 _database_code_depnum_ccdc_archive 'CCDC 894965' #TrackingRef 'Combined Final VRFs.cif' #============================================================================== _audit_creation_date 11-10-24 _audit_creation_method CRYSTALS_ver_14.11 _oxford_structure_analysis_title '10241000 Compound X' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 9.91410(10) _cell_length_b 11.3263(2) _cell_length_c 12.8550(2) _cell_angle_alpha 81.6863(7) _cell_angle_beta 83.7688(7) _cell_angle_gamma 82.6593(7) _cell_volume 1410.63(4) _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' 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' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C30 Al1 Fe1 N1 O1 # Dc = 1.11 Fooo = 564.00 Mu = 5.84 M = 473.17 # Found Formula = C27 H44 Al1 Fe1 N3 O2 # Dc = 1.24 FOOO = 564.00 Mu = 5.93 M = 525.49 _chemical_formula_sum 'C27 H44 Al1 Fe1 N3 O2' _chemical_formula_moiety 'C27 H44 Al1 Fe1 N3 O2' _chemical_compound_source ? _chemical_formula_weight 525.49 _cell_measurement_reflns_used 6160 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_min 0.090 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.110 _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 0.593 # Sheldrick geometric approximatio 0.94 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.95 # 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 25106 _reflns_number_total 6408 _diffrn_reflns_av_R_equivalents 0.057 # Number of reflections without Friedels Law is 11810 # Number of reflections with Friedels Law is 6408 # Theoretical number of reflections is about 6463 _diffrn_reflns_theta_min 5.187 _diffrn_reflns_theta_max 27.473 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.549 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 2.03 _oxford_diffrn_Wilson_scale 19.43 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.83 _refine_diff_density_max 0.91 # 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 6408 _refine_ls_number_restraints 0 _refine_ls_number_parameters 307 _oxford_refine_ls_R_factor_ref 0.0959 _refine_ls_wR_factor_ref 0.1478 _refine_ls_goodness_of_fit_ref 0.9102 _refine_ls_shift/su_max 0.0001105 _refine_ls_shift/su_mean 0.0000078 # The values computed from all data _oxford_reflns_number_all 6408 _refine_ls_R_factor_all 0.0959 _refine_ls_wR_factor_all 0.1478 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3965 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_gt 0.0937 # 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: 3.73 4.06 0.980 ; # Insert your own references if required - in alphabetical order 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 Fe1 Fe 0.28571(6) 0.42583(5) 0.13362(5) 0.0253 1.0000 Uani . . . . . . Al2 Al 0.21156(11) 0.28348(10) 0.28014(9) 0.0223 1.0000 Uani . . . . . . N3 N 0.0212(3) 0.2573(3) 0.3084(3) 0.0240 1.0000 Uani . . . . . . C4 C 0.0493(4) 0.1498(3) 0.2728(3) 0.0211 1.0000 Uani . . . . . . N5 N 0.1836(3) 0.1292(3) 0.2444(2) 0.0219 1.0000 Uani . . . . . . C6 C 0.2544(4) 0.0101(3) 0.2331(3) 0.0226 1.0000 Uani . . . . . . C7 C 0.3329(4) 0.0076(4) 0.1249(3) 0.0292 1.0000 Uani . . . . . . C8 C 0.4048(4) -0.1178(4) 0.1128(4) 0.0342 1.0000 Uani . . . . . . C9 C 0.5018(5) -0.1600(4) 0.1979(4) 0.0433 1.0000 Uani . . . . . . C10 C 0.4276(5) -0.1553(4) 0.3078(4) 0.0414 1.0000 Uani . . . . . . C11 C 0.3519(4) -0.0311(4) 0.3190(3) 0.0315 1.0000 Uani . . . . . . N12 N -0.0464(3) 0.0725(3) 0.2665(2) 0.0222 1.0000 Uani . . . . . . C13 C -0.1326(4) 0.0365(4) 0.3645(3) 0.0250 1.0000 Uani . . . . . . C14 C -0.2838(4) 0.0395(4) 0.3505(3) 0.0335 1.0000 Uani . . . . . . C15 C -0.0754(5) -0.0852(4) 0.4209(3) 0.0346 1.0000 Uani . . . . . . C16 C -0.0505(4) 0.0285(4) 0.1639(3) 0.0270 1.0000 Uani . . . . . . C17 C -0.1607(5) 0.1028(4) 0.1013(3) 0.0361 1.0000 Uani . . . . . . C18 C -0.0605(5) -0.1058(4) 0.1701(4) 0.0345 1.0000 Uani . . . . . . C19 C -0.1168(4) 0.3219(3) 0.3175(3) 0.0243 1.0000 Uani . . . . . . C20 C -0.1330(4) 0.4315(4) 0.2345(3) 0.0328 1.0000 Uani . . . . . . C21 C -0.2766(4) 0.4988(4) 0.2453(4) 0.0374 1.0000 Uani . . . . . . C22 C -0.3108(5) 0.5356(4) 0.3548(4) 0.0410 1.0000 Uani . . . . . . C23 C -0.2954(5) 0.4276(4) 0.4390(4) 0.0410 1.0000 Uani . . . . . . C24 C -0.1513(4) 0.3588(4) 0.4279(3) 0.0345 1.0000 Uani . . . . . . C25 C 0.3103(5) 0.2810(4) 0.4053(3) 0.0361 1.0000 Uani . . . . . . C26 C 0.4252(4) 0.3179(4) 0.1410(3) 0.0300 1.0000 Uani . . . . . . O27 O 0.5223(3) 0.2479(3) 0.1472(3) 0.0413 1.0000 Uani . . . . . . C28 C 0.3950(4) 0.5764(3) 0.1101(4) 0.0317 1.0000 Uani . . . . . . C29 C 0.3480(4) 0.5500(4) 0.2188(4) 0.0320 1.0000 Uani . . . . . . C30 C 0.2029(4) 0.5593(4) 0.2273(4) 0.0317 1.0000 Uani . . . . . . C31 C 0.1614(5) 0.5902(4) 0.1237(4) 0.0356 1.0000 Uani . . . . . . C32 C 0.2802(5) 0.6020(3) 0.0511(4) 0.0334 1.0000 Uani . . . . . . C33 C 0.1930(5) 0.3508(4) 0.0619(4) 0.0340 1.0000 Uani . . . . . . O34 O 0.1290(4) 0.3031(3) 0.0134(3) 0.0491 1.0000 Uani . . . . . . H61 H 0.1854 -0.0458 0.2428 0.0295 1.0000 Uiso R . . . . . H72 H 0.4019 0.0630 0.1198 0.0319 1.0000 Uiso R . . . . . H71 H 0.2671 0.0346 0.0728 0.0321 1.0000 Uiso R . . . . . H82 H 0.4533 -0.1145 0.0433 0.0430 1.0000 Uiso R . . . . . H81 H 0.3352 -0.1731 0.1172 0.0428 1.0000 Uiso R . . . . . H91 H 0.5710 -0.1073 0.1910 0.0504 1.0000 Uiso R . . . . . H92 H 0.5448 -0.2434 0.1920 0.0510 1.0000 Uiso R . . . . . H101 H 0.4925 -0.1760 0.3597 0.0495 1.0000 Uiso R . . . . . H102 H 0.3605 -0.2121 0.3178 0.0490 1.0000 Uiso R . . . . . H111 H 0.4179 0.0257 0.3119 0.0361 1.0000 Uiso R . . . . . H112 H 0.3030 -0.0294 0.3858 0.0364 1.0000 Uiso R . . . . . H131 H -0.1230 0.0940 0.4145 0.0299 1.0000 Uiso R . . . . . H142 H -0.3306 0.0249 0.4204 0.0506 1.0000 Uiso R . . . . . H143 H -0.3197 0.1176 0.3164 0.0502 1.0000 Uiso R . . . . . H141 H -0.2967 -0.0244 0.3113 0.0507 1.0000 Uiso R . . . . . H151 H -0.1115 -0.0938 0.4929 0.0529 1.0000 Uiso R . . . . . H153 H 0.0212 -0.0868 0.4166 0.0520 1.0000 Uiso R . . . . . H152 H -0.0978 -0.1506 0.3896 0.0514 1.0000 Uiso R . . . . . H161 H 0.0392 0.0434 0.1223 0.0301 1.0000 Uiso R . . . . . H171 H -0.1529 0.0804 0.0308 0.0539 1.0000 Uiso R . . . . . H172 H -0.2499 0.0931 0.1306 0.0538 1.0000 Uiso R . . . . . H173 H -0.1483 0.1871 0.0968 0.0540 1.0000 Uiso R . . . . . H182 H -0.0559 -0.1268 0.0999 0.0522 1.0000 Uiso R . . . . . H183 H -0.1483 -0.1249 0.2075 0.0512 1.0000 Uiso R . . . . . H181 H 0.0125 -0.1530 0.2046 0.0524 1.0000 Uiso R . . . . . H191 H -0.1832 0.2691 0.3067 0.0290 1.0000 Uiso R . . . . . H202 H -0.0697 0.4857 0.2465 0.0402 1.0000 Uiso R . . . . . H201 H -0.1090 0.4106 0.1634 0.0399 1.0000 Uiso R . . . . . H212 H -0.2837 0.5685 0.1907 0.0464 1.0000 Uiso R . . . . . H211 H -0.3451 0.4455 0.2353 0.0440 1.0000 Uiso R . . . . . H221 H -0.4041 0.5761 0.3622 0.0484 1.0000 Uiso R . . . . . H222 H -0.2491 0.5927 0.3660 0.0468 1.0000 Uiso R . . . . . H231 H -0.3091 0.4528 0.5079 0.0498 1.0000 Uiso R . . . . . H232 H -0.3657 0.3772 0.4290 0.0491 1.0000 Uiso R . . . . . H241 H -0.0847 0.4094 0.4392 0.0420 1.0000 Uiso R . . . . . H242 H -0.1453 0.2869 0.4817 0.0419 1.0000 Uiso R . . . . . H281 H 0.4896 0.5762 0.0811 0.0386 1.0000 Uiso R . . . . . H291 H 0.4041 0.5348 0.2770 0.0394 1.0000 Uiso R . . . . . H301 H 0.1443 0.5515 0.2918 0.0381 1.0000 Uiso R . . . . . H311 H 0.0658 0.6029 0.1076 0.0419 1.0000 Uiso R . . . . . H321 H 0.2846 0.6187 -0.0243 0.0421 1.0000 Uiso R . . . . . H29 H 0.2686 0.3411 0.4448 0.0551 1.0000 Uiso R . . . . . H251 H 0.4016 0.2971 0.3866 0.0550 1.0000 Uiso . . . . . . H252 H 0.3088 0.2067 0.4504 0.0557 1.0000 Uiso . . . . . . 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 Fe1 0.0265(3) 0.0203(3) 0.0296(3) -0.0023(2) -0.0041(2) -0.0042(2) Al2 0.0220(6) 0.0197(5) 0.0261(6) -0.0032(4) -0.0032(5) -0.0043(4) N3 0.0200(15) 0.0241(16) 0.0287(17) -0.0078(13) -0.0025(13) -0.0003(12) C4 0.0233(18) 0.0193(17) 0.0205(17) 0.0003(13) -0.0038(14) -0.0037(14) N5 0.0189(15) 0.0187(15) 0.0274(16) -0.0021(12) -0.0016(12) -0.0006(12) C6 0.0225(18) 0.0185(17) 0.0273(19) -0.0053(14) -0.0036(15) -0.0006(14) C7 0.029(2) 0.027(2) 0.032(2) -0.0083(16) 0.0026(17) -0.0057(16) C8 0.031(2) 0.029(2) 0.044(3) -0.0162(18) 0.0029(18) -0.0017(17) C9 0.028(2) 0.034(2) 0.071(3) -0.022(2) -0.009(2) 0.0039(18) C10 0.039(3) 0.032(2) 0.055(3) -0.010(2) -0.021(2) 0.0100(19) C11 0.032(2) 0.026(2) 0.037(2) -0.0081(17) -0.0088(18) 0.0017(16) N12 0.0234(16) 0.0228(15) 0.0216(15) -0.0022(12) -0.0039(12) -0.0065(12) C13 0.0216(18) 0.031(2) 0.0228(19) -0.0023(15) -0.0013(15) -0.0058(15) C14 0.025(2) 0.045(2) 0.031(2) -0.0061(18) 0.0010(17) -0.0086(18) C15 0.040(2) 0.035(2) 0.029(2) 0.0008(17) -0.0040(18) -0.0100(19) C16 0.0249(19) 0.030(2) 0.027(2) -0.0086(16) -0.0026(16) -0.0041(16) C17 0.036(2) 0.043(3) 0.030(2) -0.0087(19) -0.0127(18) 0.0037(19) C18 0.035(2) 0.030(2) 0.042(3) -0.0134(18) -0.0038(19) -0.0056(17) C19 0.0196(18) 0.0243(18) 0.030(2) -0.0081(15) -0.0025(15) 0.0001(14) C20 0.028(2) 0.036(2) 0.032(2) -0.0041(18) -0.0044(17) 0.0049(17) C21 0.030(2) 0.037(2) 0.044(3) -0.009(2) -0.0109(19) 0.0103(18) C22 0.037(2) 0.037(2) 0.050(3) -0.018(2) -0.008(2) 0.0128(19) C23 0.036(2) 0.043(3) 0.041(3) -0.016(2) 0.003(2) 0.009(2) C24 0.035(2) 0.034(2) 0.034(2) -0.0096(18) -0.0030(18) 0.0042(18) C25 0.043(3) 0.036(2) 0.034(2) -0.0031(18) -0.0132(19) -0.0139(19) C26 0.029(2) 0.027(2) 0.034(2) -0.0047(17) 0.0012(17) -0.0077(17) O27 0.0304(16) 0.0303(16) 0.060(2) -0.0033(15) 0.0015(15) 0.0009(13) C28 0.032(2) 0.0200(18) 0.044(2) -0.0032(17) -0.0030(18) -0.0079(16) C29 0.033(2) 0.0237(19) 0.042(2) -0.0086(17) -0.0053(18) -0.0051(16) C30 0.035(2) 0.0237(19) 0.037(2) -0.0090(17) 0.0008(18) -0.0025(16) C31 0.034(2) 0.0193(19) 0.053(3) -0.0011(18) -0.010(2) -0.0004(16) C32 0.040(2) 0.0207(19) 0.038(2) 0.0014(17) -0.0069(19) -0.0030(17) C33 0.037(2) 0.030(2) 0.035(2) 0.0007(18) -0.0059(19) -0.0041(18) O34 0.059(2) 0.046(2) 0.050(2) -0.0087(16) -0.0268(18) -0.0135(17) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.22771(17) 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 Fe1 . Al2 . 2.4107(13) yes Fe1 . C26 . 1.726(4) yes Fe1 . C28 . 2.104(4) yes Fe1 . C29 . 2.091(4) yes Fe1 . C30 . 2.098(4) yes Fe1 . C31 . 2.093(4) yes Fe1 . C32 . 2.117(4) yes Fe1 . C33 . 1.740(4) yes Al2 . N3 . 1.935(3) yes Al2 . N5 . 1.930(3) yes Al2 . C25 . 1.967(4) yes N3 . C4 . 1.348(5) yes N3 . C19 . 1.468(5) yes C4 . N5 . 1.341(5) yes C4 . N12 . 1.386(4) yes N5 . C6 . 1.459(4) yes C6 . C7 . 1.521(5) yes C6 . C11 . 1.528(5) yes C6 . H61 . 0.976 no C7 . C8 . 1.526(5) yes C7 . H72 . 0.977 no C7 . H71 . 0.976 no C8 . C9 . 1.520(6) yes C8 . H82 . 0.966 no C8 . H81 . 0.981 no C9 . C10 . 1.526(7) yes C9 . H91 . 0.954 no C9 . H92 . 0.995 no C10 . C11 . 1.526(6) yes C10 . H101 . 0.960 no C10 . H102 . 0.969 no C11 . H111 . 0.963 no C11 . H112 . 0.941 no N12 . C13 . 1.480(5) yes N12 . C16 . 1.483(5) yes C13 . C14 . 1.525(5) yes C13 . C15 . 1.533(6) yes C13 . H131 . 0.997 no C14 . H142 . 0.967 no C14 . H143 . 0.971 no C14 . H141 . 0.968 no C15 . H151 . 0.952 no C15 . H153 . 0.951 no C15 . H152 . 0.954 no C16 . C17 . 1.519(6) yes C16 . C18 . 1.527(5) yes C16 . H161 . 1.008 no C17 . H171 . 0.968 no C17 . H172 . 0.936 no C17 . H173 . 0.971 no C18 . H182 . 0.961 no C18 . H183 . 0.981 no C18 . H181 . 0.953 no C19 . C20 . 1.519(5) yes C19 . C24 . 1.528(5) yes C19 . H191 . 0.977 no C20 . C21 . 1.529(5) yes C20 . H202 . 0.970 no C20 . H201 . 0.974 no C21 . C22 . 1.517(6) yes C21 . H212 . 0.979 no C21 . H211 . 0.995 no C22 . C23 . 1.516(7) yes C22 . H221 . 0.979 no C22 . H222 . 0.980 no C23 . C24 . 1.540(6) yes C23 . H231 . 0.960 no C23 . H232 . 0.985 no C24 . H241 . 0.963 no C24 . H242 . 0.989 no C25 . H29 . 0.936 no C25 . H251 . 0.945 no C25 . H252 . 0.951 no C26 . O27 . 1.168(5) yes C28 . C29 . 1.426(6) yes C28 . C32 . 1.413(6) yes C28 . H281 . 0.970 no C29 . C30 . 1.422(6) yes C29 . H291 . 0.963 no C30 . C31 . 1.419(6) yes C30 . H301 . 0.959 no C31 . C32 . 1.429(6) yes C31 . H311 . 0.980 no C32 . H321 . 0.957 no C33 . O34 . 1.165(5) yes 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 Al2 . Fe1 . C26 . 77.75(14) yes Al2 . Fe1 . C28 . 137.15(13) yes C26 . Fe1 . C28 . 96.95(18) yes Al2 . Fe1 . C29 . 98.57(13) yes C26 . Fe1 . C29 . 99.79(18) yes C28 . Fe1 . C29 . 39.74(17) yes Al2 . Fe1 . C30 . 86.26(12) yes C26 . Fe1 . C30 . 133.52(19) yes C28 . Fe1 . C30 . 66.61(17) yes C29 . Fe1 . C30 . 39.69(16) yes Al2 . Fe1 . C31 . 112.88(13) yes C26 . Fe1 . C31 . 163.02(18) yes C28 . Fe1 . C31 . 66.18(17) yes C29 . Fe1 . C31 . 66.33(17) yes C30 . Fe1 . C31 . 39.58(17) yes Al2 . Fe1 . C32 . 151.55(13) yes C26 . Fe1 . C32 . 126.99(18) yes C28 . Fe1 . C32 . 39.11(16) yes C29 . Fe1 . C32 . 66.29(17) yes C30 . Fe1 . C32 . 66.59(17) yes Al2 . Fe1 . C33 . 83.88(15) yes C26 . Fe1 . C33 . 96.2(2) yes C28 . Fe1 . C33 . 138.77(19) yes C29 . Fe1 . C33 . 164.00(19) yes C30 . Fe1 . C33 . 125.40(19) yes C31 . Fe1 . C32 . 39.69(17) yes C31 . Fe1 . C33 . 98.07(19) yes C32 . Fe1 . C33 . 104.45(19) yes Fe1 . Al2 . N3 . 120.75(11) yes Fe1 . Al2 . N5 . 115.30(11) yes N3 . Al2 . N5 . 69.34(13) yes Fe1 . Al2 . C25 . 112.92(13) yes N3 . Al2 . C25 . 115.64(18) yes N5 . Al2 . C25 . 116.26(17) yes Al2 . N3 . C4 . 90.3(2) yes Al2 . N3 . C19 . 142.0(3) yes C4 . N3 . C19 . 123.2(3) yes N3 . C4 . N5 . 109.7(3) yes N3 . C4 . N12 . 125.0(3) yes N5 . C4 . N12 . 125.3(3) yes C4 . N5 . Al2 . 90.7(2) yes C4 . N5 . C6 . 123.5(3) yes Al2 . N5 . C6 . 142.0(2) yes N5 . C6 . C7 . 111.2(3) yes N5 . C6 . C11 . 111.1(3) yes C7 . C6 . C11 . 109.7(3) yes N5 . C6 . H61 . 107.4 no C7 . C6 . H61 . 110.0 no C11 . C6 . H61 . 107.4 no C6 . C7 . C8 . 111.0(3) yes C6 . C7 . H72 . 106.9 no C8 . C7 . H72 . 108.7 no C6 . C7 . H71 . 106.9 no C8 . C7 . H71 . 112.1 no H72 . C7 . H71 . 111.2 no C7 . C8 . C9 . 111.0(4) yes C7 . C8 . H82 . 107.7 no C9 . C8 . H82 . 111.0 no C7 . C8 . H81 . 108.6 no C9 . C8 . H81 . 110.3 no H82 . C8 . H81 . 108.2 no C8 . C9 . C10 . 111.1(4) yes C8 . C9 . H91 . 109.5 no C10 . C9 . H91 . 106.6 no C8 . C9 . H92 . 110.7 no C10 . C9 . H92 . 109.2 no H91 . C9 . H92 . 109.6 no C9 . C10 . C11 . 111.5(4) yes C9 . C10 . H101 . 109.4 no C11 . C10 . H101 . 109.7 no C9 . C10 . H102 . 107.7 no C11 . C10 . H102 . 107.8 no H101 . C10 . H102 . 110.7 no C6 . C11 . C10 . 111.8(3) yes C6 . C11 . H111 . 107.8 no C10 . C11 . H111 . 108.6 no C6 . C11 . H112 . 109.5 no C10 . C11 . H112 . 111.3 no H111 . C11 . H112 . 107.7 no C4 . N12 . C13 . 117.1(3) yes C4 . N12 . C16 . 117.7(3) yes C13 . N12 . C16 . 125.2(3) yes N12 . C13 . C14 . 114.7(3) yes N12 . C13 . C15 . 111.4(3) yes C14 . C13 . C15 . 111.3(3) yes N12 . C13 . H131 . 106.6 no C14 . C13 . H131 . 108.4 no C15 . C13 . H131 . 103.6 no C13 . C14 . H142 . 107.0 no C13 . C14 . H143 . 110.7 no H142 . C14 . H143 . 109.1 no C13 . C14 . H141 . 109.7 no H142 . C14 . H141 . 108.5 no H143 . C14 . H141 . 111.7 no C13 . C15 . H151 . 109.7 no C13 . C15 . H153 . 107.5 no H151 . C15 . H153 . 109.8 no C13 . C15 . H152 . 112.1 no H151 . C15 . H152 . 108.3 no H153 . C15 . H152 . 109.4 no N12 . C16 . C17 . 111.1(3) yes N12 . C16 . C18 . 115.3(3) yes C17 . C16 . C18 . 111.4(3) yes N12 . C16 . H161 . 105.9 no C17 . C16 . H161 . 106.2 no C18 . C16 . H161 . 106.2 no C16 . C17 . H171 . 109.7 no C16 . C17 . H172 . 114.2 no H171 . C17 . H172 . 107.0 no C16 . C17 . H173 . 108.7 no H171 . C17 . H173 . 109.2 no H172 . C17 . H173 . 108.0 no C16 . C18 . H182 . 109.3 no C16 . C18 . H183 . 109.7 no H182 . C18 . H183 . 108.4 no C16 . C18 . H181 . 111.8 no H182 . C18 . H181 . 107.8 no H183 . C18 . H181 . 109.8 no N3 . C19 . C20 . 112.0(3) yes N3 . C19 . C24 . 110.2(3) yes C20 . C19 . C24 . 110.1(3) yes N3 . C19 . H191 . 109.4 no C20 . C19 . H191 . 107.0 no C24 . C19 . H191 . 107.9 no C19 . C20 . C21 . 111.6(4) yes C19 . C20 . H202 . 107.4 no C21 . C20 . H202 . 107.2 no C19 . C20 . H201 . 111.7 no C21 . C20 . H201 . 111.3 no H202 . C20 . H201 . 107.4 no C20 . C21 . C22 . 110.9(4) yes C20 . C21 . H212 . 109.5 no C22 . C21 . H212 . 111.3 no C20 . C21 . H211 . 109.8 no C22 . C21 . H211 . 107.0 no H212 . C21 . H211 . 108.1 no C21 . C22 . C23 . 111.0(4) yes C21 . C22 . H221 . 110.7 no C23 . C22 . H221 . 109.6 no C21 . C22 . H222 . 109.6 no C23 . C22 . H222 . 108.6 no H221 . C22 . H222 . 107.3 no C22 . C23 . C24 . 111.3(4) yes C22 . C23 . H231 . 110.2 no C24 . C23 . H231 . 107.5 no C22 . C23 . H232 . 105.5 no C24 . C23 . H232 . 111.3 no H231 . C23 . H232 . 111.2 no C23 . C24 . C19 . 111.2(4) yes C23 . C24 . H241 . 109.6 no C19 . C24 . H241 . 108.0 no C23 . C24 . H242 . 109.6 no C19 . C24 . H242 . 110.1 no H241 . C24 . H242 . 108.3 no Al2 . C25 . H29 . 109.6 no Al2 . C25 . H251 . 111.8 no H29 . C25 . H251 . 106.6 no Al2 . C25 . H252 . 112.0 no H29 . C25 . H252 . 107.0 no H251 . C25 . H252 . 109.7 no Fe1 . C26 . O27 . 177.5(4) yes Fe1 . C28 . C29 . 69.7(2) yes Fe1 . C28 . C32 . 71.0(2) yes C29 . C28 . C32 . 108.3(4) yes Fe1 . C28 . H281 . 124.7 no C29 . C28 . H281 . 126.2 no C32 . C28 . H281 . 125.5 no Fe1 . C29 . C28 . 70.6(2) yes Fe1 . C29 . C30 . 70.4(2) yes C28 . C29 . C30 . 108.2(4) yes Fe1 . C29 . H291 . 128.3 no C28 . C29 . H291 . 125.9 no C30 . C29 . H291 . 125.7 no Fe1 . C30 . C29 . 69.9(2) yes Fe1 . C30 . C31 . 70.0(2) yes C29 . C30 . C31 . 107.4(4) yes Fe1 . C30 . H301 . 128.6 no C29 . C30 . H301 . 125.8 no C31 . C30 . H301 . 126.7 no Fe1 . C31 . C30 . 70.4(2) yes Fe1 . C31 . C32 . 71.1(2) yes C30 . C31 . C32 . 108.7(4) yes Fe1 . C31 . H311 . 125.7 no C30 . C31 . H311 . 123.8 no C32 . C31 . H311 . 127.5 no Fe1 . C32 . C31 . 69.2(2) yes Fe1 . C32 . C28 . 69.9(2) yes C31 . C32 . C28 . 107.4(4) yes Fe1 . C32 . H321 . 123.1 no C31 . C32 . H321 . 127.7 no C28 . C32 . H321 . 124.7 no Fe1 . C33 . O34 . 178.4(4) yes _iucr_refine_instruction_details_constraints ; # # Punched on 24/10/11 at 10:34:26 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 72,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 82,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) RIDE C ( 13,X'S) H ( 131,X'S) RIDE C ( 14,X'S) H ( 142,X'S) H ( 143,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) H ( 153,X'S) H ( 152,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,X'S) RIDE C ( 18,X'S) H ( 182,X'S) H ( 183,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 202,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 212,X'S) H ( 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 222,X'S) RIDE C ( 23,X'S) H ( 231,X'S) H ( 232,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) RIDE C ( 25,X'S) H ( 29,X'S) RIDE C ( 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H ( 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 32,X'S) H ( 321,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 24/10/11 at 10:34:26 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; data_8 _database_code_depnum_ccdc_archive 'CCDC 894966' #TrackingRef 'Combined Final VRFs.cif' #============================================================================== _audit_creation_date 12-03-21 _audit_creation_method CRYSTALS_ver_14.23 _oxford_structure_analysis_title 071IRMK11 _chemical_name_systematic . _chemical_melting_point . _cell_length_a 10.4973(2) _cell_length_b 11.4644(2) _cell_length_c 14.7576(3) _cell_angle_alpha 86.8923(17) _cell_angle_beta 70.6133(19) _cell_angle_gamma 79.5184(17) _cell_volume 1647.31(6) _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 0.0181 0.0091 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' N 0.0311 0.0180 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' O 0.0492 0.0322 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' Al 0.2130 0.2455 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' Fe -1.1336 3.1974 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 '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' _cell_formula_units_Z 2 # Given Formula = C34 H34 Al1 Fe1 N1 O1 # Dc = 1.12 Fooo = 644.00 Mu = 41.01 M = 555.48 # Found Formula = C32 H54 Al1 Fe1 N3 O2 # Dc = 1.20 FOOO = 644.00 Mu = 41.59 M = 595.63 _chemical_formula_sum 'C32 H54 Al1 Fe1 N3 O2' _chemical_formula_moiety 'C32 H54 Al1 Fe1 N3 O2' _chemical_compound_source . _chemical_formula_weight 595.63 _cell_measurement_reflns_used 22684 _cell_measurement_theta_min 3.1720 _cell_measurement_theta_max 76.3603 _cell_measurement_temperature 150 _exptl_crystal_description ? _exptl_crystal_colour colourless _exptl_crystal_size_min 0.040 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_max 0.120 _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 4.159 # Sheldrick geometric approximatio 0.78 0.85 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 0.85 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _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 33671 _reflns_number_total 6861 _diffrn_reflns_av_R_equivalents 0.0283 # Number of reflections without Friedels Law is 22684 # Number of reflections with Friedels Law is 6861 # Theoretical number of reflections is about 6928 _diffrn_reflns_theta_min 3.175 _diffrn_reflns_theta_max 76.551 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 74.255 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -12 _reflns_limit_h_max 13 _reflns_limit_k_min -14 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 2.27 _oxford_diffrn_Wilson_scale 0.02 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.40 _refine_diff_density_max 0.29 # 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 6861 _refine_ls_number_restraints 141 _refine_ls_number_parameters 406 _oxford_refine_ls_R_factor_ref 0.0319 _refine_ls_wR_factor_ref 0.0800 _refine_ls_goodness_of_fit_ref 0.9122 _refine_ls_shift/su_max 0.0060304 _refine_ls_shift/su_mean 0.0001909 # The values computed from all data _oxford_reflns_number_all 6861 _refine_ls_R_factor_all 0.0319 _refine_ls_wR_factor_all 0.0800 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6676 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_gt 0.0794 # 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^ + 0.82P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order 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 C121 C 0.7207(7) 0.5012(6) 0.0838(5) 0.0492 0.4807 Uani D . . 2 2 . C122 C 0.6599(8) 0.4882(4) 0.0053(3) 0.0852 0.4807 Uani D . . 2 2 . C123 C 0.7826(15) 0.6087(12) 0.0678(9) 0.1130 0.4807 Uani D . . 2 2 . C131 C 0.6816(5) 0.5343(4) 0.0858(4) 0.0322 0.5193 Uani D . . 2 1 . C132 C 0.7557(4) 0.4248(3) 0.0229(2) 0.0500 0.5193 Uani D . . 2 1 . C133 C 0.7887(8) 0.6138(5) 0.0809(5) 0.0454 0.5193 Uani D . . 2 1 . N100 N 0.60974(13) 0.49942(11) 0.18267(9) 0.0321 1.0000 Uani D . . . . . C101 C 0.5164(3) 0.5961(2) 0.2416(2) 0.0578 0.8066 Uani D . . 1 1 . C102 C 0.4513(5) 0.6935(3) 0.1979(3) 0.0894 0.8066 Uani D . . 1 1 . C103 C 0.4180(5) 0.5519(5) 0.3329(5) 0.0481 0.8066 Uani D . . 1 1 . C111 C 0.4698(7) 0.5663(7) 0.2164(5) 0.0269 0.1934 Uani D . . 1 2 . C112 C 0.4248(12) 0.6429(12) 0.1695(10) 0.0627 0.1934 Uani D . . 1 2 . C113 C 0.414(3) 0.565(2) 0.322(3) 0.0766 0.1934 Uani D . . 1 2 . Fe1 Fe 0.89292(2) 0.067219(17) 0.274256(14) 0.0253 1.0000 Uani . . . . . . Al2 Al 0.70022(4) 0.22714(3) 0.31935(3) 0.0271 1.0000 Uani . . . . . . N3 N 0.73592(12) 0.38617(10) 0.28066(8) 0.0269 1.0000 Uani D . . . . . C4 C 0.65051(14) 0.39674(12) 0.22986(10) 0.0265 1.0000 Uani . . . . . . N5 N 0.60506(13) 0.29493(11) 0.23144(10) 0.0347 1.0000 Uani D . . . . . C6 C 0.50657(14) 0.27597(13) 0.18687(11) 0.0300 1.0000 Uani D . . . . . C7 C 0.38050(17) 0.23830(18) 0.26025(15) 0.0509 1.0000 Uani D . . . . . C8 C 0.2808(2) 0.2118(2) 0.2113(2) 0.0809 1.0000 Uani D . . . . . C9 C 0.3480(3) 0.1201(2) 0.1327(2) 0.0802 1.0000 Uani D . . . . . C10 C 0.4717(3) 0.1584(2) 0.06046(18) 0.0712 1.0000 Uani D . . . . . C11 C 0.57162(19) 0.18205(15) 0.10844(12) 0.0428 1.0000 Uani D . . . . . C18 C 0.79933(15) 0.48115(11) 0.29893(10) 0.0284 1.0000 Uani D . . . . . C19 C 0.76272(16) 0.49861(13) 0.40712(11) 0.0353 1.0000 Uani D . . . . . C20 C 0.8301(2) 0.59572(15) 0.42887(14) 0.0476 1.0000 Uani D . . . . . C21 C 0.9839(2) 0.56985(19) 0.38106(15) 0.0536 1.0000 Uani D . . . . . C22 C 1.0212(2) 0.55367(18) 0.27297(14) 0.0511 1.0000 Uani D . . . . . C23 C 0.95449(16) 0.45584(14) 0.25112(11) 0.0355 1.0000 Uani D . . . . . C24 C 0.57161(17) 0.23090(14) 0.45171(12) 0.0402 1.0000 Uani . . . . . . C25 C 0.93967(18) 0.15494(13) 0.17306(11) 0.0367 1.0000 Uani . . . . . . O26 O 0.97415(17) 0.20945(11) 0.10310(8) 0.0576 1.0000 Uani . . . . . . C27 C 0.93097(15) 0.15140(12) 0.35254(11) 0.0313 1.0000 Uani . . . . . . O28 O 0.95837(13) 0.20183(10) 0.40806(9) 0.0434 1.0000 Uani . . . . . . C29 C 0.86907(16) -0.08057(12) 0.20648(10) 0.0318 1.0000 Uani D . . . . . C30 C 0.76881(15) -0.06628(12) 0.30032(10) 0.0305 1.0000 Uani D . . . . . C31 C 0.84092(16) -0.07441(12) 0.36772(10) 0.0306 1.0000 Uani D . . . . . C32 C 0.98611(16) -0.09621(12) 0.31522(11) 0.0315 1.0000 Uani D . . . . . C33 C 1.00302(16) -0.10022(12) 0.21599(10) 0.0326 1.0000 Uani D . . . . . C34 C 1.13549(18) -0.12800(14) 0.13521(12) 0.0428 1.0000 Uani D . . . . . C35 C 1.09855(18) -0.11443(15) 0.35824(13) 0.0430 1.0000 Uani D . . . . . C36 C 0.77774(18) -0.07201(14) 0.47495(11) 0.0377 1.0000 Uani D . . . . . C37 C 0.61828(17) -0.06399(15) 0.32436(12) 0.0403 1.0000 Uani D . . . . . C38 C 0.8434(2) -0.08676(15) 0.11286(12) 0.0431 1.0000 Uani D . . . . . H1211 H 0.8017 0.4359 0.0763 0.0649 0.4807 Uiso DR . . 2 2 . H1223 H 0.7292 0.4842 -0.0560 0.1257 0.4807 Uiso DR . . 2 2 . H1222 H 0.5878 0.5532 0.0067 0.1258 0.4807 Uiso DR . . 2 2 . H1221 H 0.6224 0.4153 0.0145 0.1253 0.4807 Uiso DR . . 2 2 . H1231 H 0.8264 0.6148 0.1161 0.1678 0.4807 Uiso DR . . 2 2 . H1232 H 0.8526 0.5999 0.0047 0.1678 0.4807 Uiso DR . . 2 2 . H1233 H 0.7134 0.6795 0.0701 0.1679 0.4807 Uiso DR . . 2 2 . H1311 H 0.6108 0.5775 0.0591 0.0395 0.5193 Uiso DR . . 2 1 . H1321 H 0.6931 0.3736 0.0188 0.0730 0.5193 Uiso DR . . 2 1 . H1322 H 0.8280 0.3819 0.0455 0.0740 0.5193 Uiso DR . . 2 1 . H1323 H 0.7978 0.4519 -0.0408 0.0733 0.5193 Uiso DR . . 2 1 . H1331 H 0.7524 0.6772 0.1287 0.0721 0.5193 Uiso DR . . 2 1 . H1332 H 0.8684 0.5642 0.0914 0.0716 0.5193 Uiso DR . . 2 1 . H1333 H 0.8162 0.6441 0.0171 0.0722 0.5193 Uiso DR . . 2 1 . H1011 H 0.5772 0.6404 0.2628 0.0683 0.8066 Uiso DR . . 1 1 . H1021 H 0.3905 0.7513 0.2446 0.1382 0.8066 Uiso DR . . 1 1 . H1022 H 0.5155 0.7276 0.1483 0.1384 0.8066 Uiso DR . . 1 1 . H1023 H 0.3961 0.6573 0.1702 0.1404 0.8066 Uiso DR . . 1 1 . H1033 H 0.3651 0.6216 0.3711 0.0701 0.8066 Uiso DR . . 1 1 . H1032 H 0.4714 0.5033 0.3678 0.0704 0.8066 Uiso DR . . 1 1 . H1031 H 0.3579 0.5066 0.3211 0.0706 0.8066 Uiso DR . . 1 1 . H1111 H 0.4224 0.5063 0.2041 0.0254 0.1934 Uiso DR . . 1 2 . H1123 H 0.3568 0.6994 0.2163 0.0861 0.1934 Uiso DR . . 1 2 . H1122 H 0.4947 0.6830 0.1273 0.0855 0.1934 Uiso DR . . 1 2 . H1121 H 0.3795 0.6084 0.1338 0.0859 0.1934 Uiso DR . . 1 2 . H1131 H 0.3044 0.5886 0.3392 0.1179 0.1934 Uiso DR . . 1 2 . H1132 H 0.4577 0.6326 0.3450 0.1177 0.1934 Uiso DR . . 1 2 . H1133 H 0.4443 0.4763 0.3476 0.1179 0.1934 Uiso DR . . 1 2 . H61 H 0.4769 0.3516 0.1587 0.0349 1.0000 Uiso DR . . . . . H71 H 0.3377 0.3012 0.3087 0.0598 1.0000 Uiso DR . . . . . H72 H 0.4099 0.1650 0.2910 0.0586 1.0000 Uiso DR . . . . . H81 H 0.2465 0.2860 0.1861 0.0958 1.0000 Uiso DR . . . . . H82 H 0.2082 0.1836 0.2606 0.0968 1.0000 Uiso DR . . . . . H91 H 0.3775 0.0421 0.1580 0.0949 1.0000 Uiso DR . . . . . H92 H 0.2843 0.1079 0.1010 0.0977 1.0000 Uiso DR . . . . . H101 H 0.4445 0.2341 0.0281 0.0849 1.0000 Uiso DR . . . . . H102 H 0.5172 0.0950 0.0128 0.0866 1.0000 Uiso DR . . . . . H111 H 0.6533 0.2047 0.0626 0.0516 1.0000 Uiso DR . . . . . H112 H 0.6019 0.1078 0.1362 0.0508 1.0000 Uiso DR . . . . . H181 H 0.7647 0.5560 0.2737 0.0347 1.0000 Uiso DR . . . . . H191 H 0.7944 0.4218 0.4348 0.0410 1.0000 Uiso DR . . . . . H192 H 0.6653 0.5182 0.4339 0.0424 1.0000 Uiso DR . . . . . H201 H 0.8063 0.6070 0.4972 0.0563 1.0000 Uiso DR . . . . . H202 H 0.7962 0.6699 0.4056 0.0554 1.0000 Uiso DR . . . . . H211 H 1.0255 0.6371 0.3920 0.0636 1.0000 Uiso DR . . . . . H212 H 1.0225 0.4997 0.4065 0.0627 1.0000 Uiso DR . . . . . H221 H 1.1197 0.5341 0.2433 0.0609 1.0000 Uiso DR . . . . . H222 H 0.9877 0.6295 0.2458 0.0602 1.0000 Uiso DR . . . . . H231 H 0.9909 0.3788 0.2740 0.0412 1.0000 Uiso DR . . . . . H232 H 0.9745 0.4439 0.1830 0.0417 1.0000 Uiso DR . . . . . H341 H 1.2119 -0.1110 0.1500 0.0657 1.0000 Uiso DR . . . . . H343 H 1.1300 -0.0848 0.0779 0.0649 1.0000 Uiso DR . . . . . H342 H 1.1531 -0.2111 0.1173 0.0631 1.0000 Uiso DR . . . . . H352 H 1.1771 -0.0826 0.3198 0.0633 1.0000 Uiso DR . . . . . H351 H 1.0670 -0.0743 0.4212 0.0646 1.0000 Uiso DR . . . . . H353 H 1.1262 -0.1951 0.3650 0.0634 1.0000 Uiso DR . . . . . H361 H 0.8370 -0.0461 0.5038 0.0579 1.0000 Uiso DR . . . . . H363 H 0.6949 -0.0195 0.4961 0.0575 1.0000 Uiso DR . . . . . H362 H 0.7611 -0.1486 0.4981 0.0572 1.0000 Uiso DR . . . . . H372 H 0.5665 -0.0183 0.3802 0.0577 1.0000 Uiso DR . . . . . H371 H 0.5982 -0.1419 0.3341 0.0584 1.0000 Uiso DR . . . . . H373 H 0.5832 -0.0322 0.2728 0.0604 1.0000 Uiso DR . . . . . H381 H 0.8813 -0.0273 0.0709 0.0669 1.0000 Uiso DR . . . . . H383 H 0.8855 -0.1638 0.0816 0.0638 1.0000 Uiso DR . . . . . H382 H 0.7451 -0.0758 0.1222 0.0657 1.0000 Uiso DR . . . . . H242 H 0.5084 0.3033 0.4675 0.0598 1.0000 Uiso R . . . . . H243 H 0.6191 0.2200 0.4961 0.0609 1.0000 Uiso R . . . . . H241 H 0.5174 0.1710 0.4629 0.0598 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 C121 0.049(4) 0.037(4) 0.036(2) 0.008(2) 0.012(2) 0.005(2) C122 0.180(7) 0.045(2) 0.033(2) 0.0103(18) -0.030(3) -0.038(3) C123 0.128(9) 0.161(10) 0.088(7) 0.061(6) -0.066(6) -0.080(8) C131 0.035(3) 0.025(2) 0.0293(17) -0.0002(17) -0.0052(19) 0.0021(17) C132 0.061(2) 0.0399(18) 0.0339(16) 0.0000(14) 0.0050(15) -0.0097(16) C133 0.062(3) 0.038(2) 0.038(2) 0.0171(18) -0.008(2) -0.032(2) N100 0.0375(7) 0.0258(6) 0.0281(6) 0.0042(5) -0.0069(5) -0.0014(5) C101 0.0547(15) 0.0323(12) 0.0665(17) 0.0040(11) -0.0060(14) 0.0150(11) C102 0.119(3) 0.057(2) 0.061(2) 0.0047(16) -0.020(2) 0.044(2) C103 0.040(2) 0.049(3) 0.0384(17) -0.009(2) -0.0007(14) 0.0163(16) C111 0.025(4) 0.027(4) 0.038(4) -0.016(3) -0.025(3) 0.005(3) C112 0.043(6) 0.072(9) 0.060(8) 0.001(6) -0.022(5) 0.031(6) C113 0.100(18) 0.022(7) 0.073(18) 0.009(8) -0.001(11) 0.022(8) Fe1 0.03047(12) 0.01627(10) 0.02231(11) 0.00114(7) -0.00128(8) -0.00132(8) Al2 0.0284(2) 0.01949(18) 0.0299(2) -0.00041(15) -0.00633(16) -0.00168(15) N3 0.0288(6) 0.0189(5) 0.0313(6) -0.0016(4) -0.0088(5) -0.0014(4) C4 0.0248(6) 0.0219(6) 0.0269(6) -0.0021(5) -0.0028(5) 0.0004(5) N5 0.0373(7) 0.0250(6) 0.0469(7) 0.0035(5) -0.0204(6) -0.0067(5) C6 0.0252(6) 0.0277(7) 0.0360(7) -0.0005(6) -0.0089(6) -0.0037(5) C7 0.0289(8) 0.0545(11) 0.0572(11) -0.0050(9) 0.0033(7) -0.0087(7) C8 0.0323(10) 0.0773(16) 0.137(3) 0.0073(16) -0.0285(13) -0.0184(10) C9 0.0839(17) 0.0524(13) 0.136(3) 0.0024(14) -0.0715(18) -0.0252(12) C10 0.119(2) 0.0446(11) 0.0708(15) -0.0063(10) -0.0540(15) -0.0195(12) C11 0.0482(9) 0.0335(8) 0.0404(9) -0.0040(7) -0.0059(7) -0.0067(7) C18 0.0352(7) 0.0171(6) 0.0326(7) -0.0005(5) -0.0117(6) -0.0028(5) C19 0.0385(8) 0.0299(7) 0.0334(7) -0.0078(6) -0.0073(6) -0.0021(6) C20 0.0679(12) 0.0335(8) 0.0466(10) -0.0098(7) -0.0240(9) -0.0084(8) C21 0.0636(12) 0.0529(11) 0.0583(11) 0.0012(9) -0.0305(10) -0.0257(9) C22 0.0534(11) 0.0529(11) 0.0536(11) 0.0082(8) -0.0166(9) -0.0299(9) C23 0.0367(8) 0.0344(8) 0.0335(7) 0.0018(6) -0.0061(6) -0.0122(6) C24 0.0381(8) 0.0324(8) 0.0377(8) -0.0009(6) 0.0021(7) -0.0019(6) C25 0.0505(9) 0.0200(6) 0.0288(7) -0.0027(5) -0.0004(6) -0.0019(6) O26 0.0956(11) 0.0317(6) 0.0269(6) 0.0065(5) 0.0034(6) -0.0111(6) C27 0.0341(7) 0.0213(6) 0.0322(7) 0.0065(5) -0.0052(6) -0.0013(5) O28 0.0606(8) 0.0336(6) 0.0424(6) 0.0011(5) -0.0250(6) -0.0091(5) C29 0.0444(8) 0.0183(6) 0.0272(7) -0.0021(5) -0.0054(6) -0.0030(5) C30 0.0376(8) 0.0192(6) 0.0300(7) 0.0010(5) -0.0043(6) -0.0062(5) C31 0.0403(8) 0.0180(6) 0.0271(7) 0.0026(5) -0.0029(6) -0.0048(5) C32 0.0389(8) 0.0180(6) 0.0315(7) 0.0038(5) -0.0066(6) -0.0003(5) C33 0.0402(8) 0.0168(6) 0.0302(7) -0.0013(5) -0.0012(6) 0.0024(5) C34 0.0443(9) 0.0314(8) 0.0368(8) -0.0018(6) 0.0020(7) 0.0047(7) C35 0.0444(9) 0.0334(8) 0.0474(9) 0.0071(7) -0.0152(7) 0.0007(7) C36 0.0498(9) 0.0300(7) 0.0262(7) 0.0035(6) -0.0030(6) -0.0083(7) C37 0.0413(9) 0.0340(8) 0.0434(9) 0.0029(7) -0.0077(7) -0.0134(7) C38 0.0604(11) 0.0341(8) 0.0318(8) -0.0049(6) -0.0125(7) -0.0044(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 7.58(12) 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 C121 . C122 . 1.522(10) yes C121 . C123 . 1.468(14) yes C121 . N100 . 1.537(7) yes C121 . H1211 . 1.005 no C122 . H1223 . 0.951 no C122 . H1222 . 0.956 no C122 . H1221 . 0.972 no C123 . H1231 . 0.980 no C123 . H1232 . 0.972 no C123 . H1233 . 0.979 no C131 . C132 . 1.529(6) yes C131 . C133 . 1.553(9) yes C131 . N100 . 1.450(6) yes C131 . H1311 . 0.996 no C132 . H1321 . 0.975 no C132 . H1322 . 0.971 no C132 . H1323 . 0.958 no C133 . H1331 . 0.974 no C133 . H1332 . 0.975 no C133 . H1333 . 0.954 no N100 . C101 . 1.446(3) yes N100 . C4 . 1.4070(18) yes N100 . C111 . 1.463(7) yes N100 . C4 . 1.4070(18) yes N100 . C101 . 1.446(3) yes N100 . C4 . 1.4070(18) yes N100 . C111 . 1.463(7) yes N100 . C4 . 1.4070(18) yes C101 . C102 . 1.437(4) yes C101 . C103 . 1.527(7) yes C101 . H1011 . 1.016 no C102 . H1021 . 0.962 no C102 . H1022 . 0.938 no C102 . H1023 . 0.969 no C103 . H1033 . 0.972 no C103 . H1032 . 0.968 no C103 . H1031 . 0.949 no C111 . C112 . 1.215(15) yes C111 . C113 . 1.47(4) yes C111 . H1111 . 0.975 no C112 . H1123 . 0.979 no C112 . H1122 . 0.962 no C112 . H1121 . 0.957 no C113 . H1131 . 1.081 no C113 . H1132 . 1.089 no C113 . H1133 . 1.094 no Fe1 . Al2 . 2.4053(4) yes Fe1 . C25 . 1.7357(15) yes Fe1 . C27 . 1.7301(16) yes Fe1 . C29 . 2.1067(14) yes Fe1 . C30 . 2.1253(14) yes Fe1 . C31 . 2.1016(13) yes Fe1 . C32 . 2.1061(14) yes Fe1 . C33 . 2.1147(13) yes Al2 . N3 . 1.9453(12) yes Al2 . C4 . 2.3678(14) yes Al2 . N5 . 1.9373(13) yes Al2 . C24 . 1.9690(16) yes Al2 . C27 . 2.6149(15) yes N3 . C4 . 1.3333(18) yes N3 . C18 . 1.4546(17) yes C4 . N5 . 1.3352(18) yes N5 . C6 . 1.4482(18) yes C6 . C7 . 1.522(2) yes C6 . C11 . 1.519(2) yes C6 . H61 . 0.985 no C7 . C8 . 1.533(3) yes C7 . H71 . 0.978 no C7 . H72 . 0.982 no C8 . C9 . 1.506(4) yes C8 . H81 . 0.967 no C8 . H82 . 0.954 no C9 . C10 . 1.501(4) yes C9 . H91 . 0.987 no C9 . H92 . 0.966 no C10 . C11 . 1.514(3) yes C10 . H101 . 1.010 no C10 . H102 . 0.978 no C11 . H111 . 0.968 no C11 . H112 . 0.972 no C18 . C19 . 1.529(2) yes C18 . C23 . 1.524(2) yes C18 . H181 . 0.974 no C19 . C20 . 1.523(2) yes C19 . H191 . 0.999 no C19 . H192 . 0.954 no C20 . C21 . 1.511(3) yes C20 . H201 . 0.965 no C20 . H202 . 0.953 no C21 . C22 . 1.524(3) yes C21 . H211 . 0.998 no C21 . H212 . 0.950 no C22 . C23 . 1.526(2) yes C22 . H221 . 0.967 no C22 . H222 . 0.992 no C23 . H231 . 0.985 no C23 . H232 . 0.968 no C24 . H242 . 0.949 no C24 . H243 . 0.937 no C24 . H241 . 0.944 no C25 . O26 . 1.1626(19) yes C27 . O28 . 1.1648(19) yes C29 . C30 . 1.431(2) yes C29 . C33 . 1.435(2) yes C29 . C38 . 1.500(2) yes C30 . C31 . 1.427(2) yes C30 . C37 . 1.496(2) yes C31 . C32 . 1.444(2) yes C31 . C36 . 1.4988(19) yes C32 . C33 . 1.418(2) yes C32 . C35 . 1.494(2) yes C33 . C34 . 1.495(2) yes C34 . H341 . 0.952 no C34 . H343 . 0.970 no C34 . H342 . 0.970 no C35 . H352 . 0.954 no C35 . H351 . 0.986 no C35 . H353 . 0.929 no C36 . H361 . 0.956 no C36 . H363 . 0.930 no C36 . H362 . 0.950 no C37 . H372 . 0.946 no C37 . H371 . 0.948 no C37 . H373 . 0.977 no C38 . H381 . 0.947 no C38 . H383 . 0.977 no C38 . H382 . 0.980 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 C122 . C121 . C123 . 109.9(7) yes C122 . C121 . N100 . 109.5(5) yes C123 . C121 . N100 . 113.2(7) yes C122 . C121 . H1211 . 108.8 no C123 . C121 . H1211 . 102.9 no N100 . C121 . H1211 . 112.3 no C121 . C122 . H1223 . 110.1 no C121 . C122 . H1222 . 111.0 no H1223 . C122 . H1222 . 109.5 no C121 . C122 . H1221 . 109.8 no H1223 . C122 . H1221 . 108.0 no H1222 . C122 . H1221 . 108.3 no C121 . C123 . H1231 . 110.0 no C121 . C123 . H1232 . 106.6 no H1231 . C123 . H1232 . 108.8 no C121 . C123 . H1233 . 110.7 no H1231 . C123 . H1233 . 110.1 no H1232 . C123 . H1233 . 110.6 no C132 . C131 . C133 . 108.0(4) yes C132 . C131 . N100 . 110.4(4) yes C133 . C131 . N100 . 113.6(4) yes C132 . C131 . H1311 . 107.8 no C133 . C131 . H1311 . 110.0 no N100 . C131 . H1311 . 107.0 no C131 . C132 . H1321 . 112.4 no C131 . C132 . H1322 . 110.1 no H1321 . C132 . H1322 . 111.7 no C131 . C132 . H1323 . 107.5 no H1321 . C132 . H1323 . 107.2 no H1322 . C132 . H1323 . 107.8 no C131 . C133 . H1331 . 112.2 no C131 . C133 . H1332 . 108.5 no H1331 . C133 . H1332 . 109.2 no C131 . C133 . H1333 . 106.6 no H1331 . C133 . H1333 . 111.9 no H1332 . C133 . H1333 . 108.4 no C131 . N100 . C101 . 113.7(2) yes C131 . N100 . C4 . 125.9(2) yes C101 . N100 . C4 . 117.52(15) yes C131 . N100 . C111 . 110.5(4) yes C131 . N100 . C4 . 125.9(2) yes C111 . N100 . C4 . 121.7(3) yes C121 . N100 . C101 . 130.1(3) yes C121 . N100 . C4 . 107.0(2) yes C101 . N100 . C4 . 117.52(15) yes C121 . N100 . C111 . 129.2(4) yes C121 . N100 . C4 . 107.0(2) yes C111 . N100 . C4 . 121.7(3) yes N100 . C101 . C102 . 119.9(3) yes N100 . C101 . C103 . 111.9(3) yes C102 . C101 . C103 . 113.1(3) yes N100 . C101 . H1011 . 104.7 no C102 . C101 . H1011 . 98.3 no C103 . C101 . H1011 . 106.6 no C101 . C102 . H1021 . 112.0 no C101 . C102 . H1022 . 111.8 no H1021 . C102 . H1022 . 112.3 no C101 . C102 . H1023 . 104.0 no H1021 . C102 . H1023 . 107.8 no H1022 . C102 . H1023 . 108.5 no C101 . C103 . H1033 . 106.9 no C101 . C103 . H1032 . 108.6 no H1033 . C103 . H1032 . 109.5 no C101 . C103 . H1031 . 113.6 no H1033 . C103 . H1031 . 109.7 no H1032 . C103 . H1031 . 108.6 no N100 . C111 . C112 . 123.3(8) yes N100 . C111 . C113 . 110.4(11) yes C112 . C111 . C113 . 121.9(13) yes N100 . C111 . H1111 . 98.4 no C112 . C111 . H1111 . 95.0 no C113 . C111 . H1111 . 97.6 no C111 . C112 . H1123 . 105.7 no C111 . C112 . H1122 . 112.5 no H1123 . C112 . H1122 . 109.7 no C111 . C112 . H1121 . 109.1 no H1123 . C112 . H1121 . 108.8 no H1122 . C112 . H1121 . 110.7 no C111 . C113 . H1131 . 105.2 no C111 . C113 . H1132 . 104.7 no H1131 . C113 . H1132 . 112.3 no C111 . C113 . H1133 . 109.3 no H1131 . C113 . H1133 . 111.8 no H1132 . C113 . H1133 . 113.0 no Al2 . Fe1 . C25 . 81.04(5) yes Al2 . Fe1 . C27 . 76.51(5) yes C25 . Fe1 . C27 . 98.13(7) yes Al2 . Fe1 . C29 . 116.61(5) yes C25 . Fe1 . C29 . 97.64(6) yes C27 . Fe1 . C29 . 160.94(6) yes Al2 . Fe1 . C30 . 93.91(4) yes C25 . Fe1 . C30 . 128.07(7) yes C27 . Fe1 . C30 . 131.10(6) yes C29 . Fe1 . C30 . 39.51(5) yes Al2 . Fe1 . C31 . 107.35(4) yes C25 . Fe1 . C31 . 163.83(6) yes C27 . Fe1 . C31 . 97.29(6) yes C29 . Fe1 . C31 . 66.31(6) yes C30 . Fe1 . C31 . 39.44(6) yes Al2 . Fe1 . C32 . 145.87(4) yes C25 . Fe1 . C32 . 133.09(7) yes C27 . Fe1 . C32 . 94.94(6) yes C29 . Fe1 . C32 . 66.35(6) yes C30 . Fe1 . C32 . 66.69(6) yes Al2 . Fe1 . C33 . 156.36(5) yes C25 . Fe1 . C33 . 100.10(6) yes C27 . Fe1 . C33 . 126.13(7) yes C29 . Fe1 . C33 . 39.75(6) yes C30 . Fe1 . C33 . 66.59(6) yes C31 . Fe1 . C32 . 40.13(6) yes C31 . Fe1 . C33 . 66.58(5) yes C32 . Fe1 . C33 . 39.25(6) yes Fe1 . Al2 . N3 . 117.13(4) yes Fe1 . Al2 . C4 . 128.72(4) yes N3 . Al2 . C4 . 34.27(5) yes Fe1 . Al2 . N5 . 122.63(4) yes N3 . Al2 . N5 . 68.51(5) yes C4 . Al2 . N5 . 34.32(5) yes Fe1 . Al2 . C24 . 118.08(5) yes N3 . Al2 . C24 . 109.79(6) yes C4 . Al2 . C24 . 112.93(6) yes N5 . Al2 . C24 . 110.53(7) yes Fe1 . Al2 . C27 . 40.04(3) yes N3 . Al2 . C27 . 96.02(5) yes C4 . Al2 . C27 . 126.62(5) yes N5 . Al2 . C27 . 149.24(6) yes C24 . Al2 . C27 . 99.59(6) yes Al2 . N3 . C4 . 90.50(8) yes Al2 . N3 . C18 . 143.55(9) yes C4 . N3 . C18 . 125.21(11) yes N100 . C4 . Al2 . 175.09(10) yes N100 . C4 . N3 . 126.21(13) yes Al2 . C4 . N3 . 55.24(7) yes N100 . C4 . N5 . 123.80(13) yes Al2 . C4 . N5 . 54.89(7) yes N3 . C4 . N5 . 109.98(12) yes C4 . N5 . Al2 . 90.78(9) yes C4 . N5 . C6 . 124.94(12) yes Al2 . N5 . C6 . 143.70(10) yes N5 . C6 . C7 . 111.37(14) yes N5 . C6 . C11 . 110.34(13) yes C7 . C6 . C11 . 109.42(13) yes N5 . C6 . H61 . 108.0 no C7 . C6 . H61 . 108.1 no C11 . C6 . H61 . 109.6 no C6 . C7 . C8 . 110.84(18) yes C6 . C7 . H71 . 108.4 no C8 . C7 . H71 . 111.8 no C6 . C7 . H72 . 108.5 no C8 . C7 . H72 . 107.8 no H71 . C7 . H72 . 109.5 no C7 . C8 . C9 . 112.21(18) yes C7 . C8 . H81 . 107.0 no C9 . C8 . H81 . 110.9 no C7 . C8 . H82 . 106.1 no C9 . C8 . H82 . 110.1 no H81 . C8 . H82 . 110.4 no C8 . C9 . C10 . 110.29(18) yes C8 . C9 . H91 . 111.9 no C10 . C9 . H91 . 108.2 no C8 . C9 . H92 . 110.5 no C10 . C9 . H92 . 109.5 no H91 . C9 . H92 . 106.3 no C9 . C10 . C11 . 110.83(19) yes C9 . C10 . H101 . 110.7 no C11 . C10 . H101 . 107.4 no C9 . C10 . H102 . 108.7 no C11 . C10 . H102 . 108.9 no H101 . C10 . H102 . 110.3 no C6 . C11 . C10 . 112.18(16) yes C6 . C11 . H111 . 109.7 no C10 . C11 . H111 . 111.9 no C6 . C11 . H112 . 109.5 no C10 . C11 . H112 . 107.2 no H111 . C11 . H112 . 106.1 no N3 . C18 . C19 . 109.88(12) yes N3 . C18 . C23 . 111.42(11) yes C19 . C18 . C23 . 110.36(12) yes N3 . C18 . H181 . 110.7 no C19 . C18 . H181 . 106.8 no C23 . C18 . H181 . 107.5 no C18 . C19 . C20 . 111.29(13) yes C18 . C19 . H191 . 108.1 no C20 . C19 . H191 . 110.0 no C18 . C19 . H192 . 107.8 no C20 . C19 . H192 . 110.7 no H191 . C19 . H192 . 108.9 no C19 . C20 . C21 . 111.20(14) yes C19 . C20 . H201 . 111.1 no C21 . C20 . H201 . 111.0 no C19 . C20 . H202 . 110.1 no C21 . C20 . H202 . 107.9 no H201 . C20 . H202 . 105.2 no C20 . C21 . C22 . 110.98(16) yes C20 . C21 . H211 . 110.1 no C22 . C21 . H211 . 107.9 no C20 . C21 . H212 . 110.5 no C22 . C21 . H212 . 108.6 no H211 . C21 . H212 . 108.7 no C21 . C22 . C23 . 110.65(14) yes C21 . C22 . H221 . 110.4 no C23 . C22 . H221 . 109.4 no C21 . C22 . H222 . 108.4 no C23 . C22 . H222 . 109.2 no H221 . C22 . H222 . 108.7 no C22 . C23 . C18 . 111.34(14) yes C22 . C23 . H231 . 110.4 no C18 . C23 . H231 . 108.6 no C22 . C23 . H232 . 113.1 no C18 . C23 . H232 . 108.5 no H231 . C23 . H232 . 104.6 no Al2 . C24 . H242 . 113.0 no Al2 . C24 . H243 . 110.7 no H242 . C24 . H243 . 107.7 no Al2 . C24 . H241 . 112.4 no H242 . C24 . H241 . 105.4 no H243 . C24 . H241 . 107.2 no Fe1 . C25 . O26 . 177.14(13) yes Al2 . C27 . Fe1 . 63.44(5) yes Al2 . C27 . O28 . 119.24(11) yes Fe1 . C27 . O28 . 175.91(12) yes Fe1 . C29 . C30 . 70.94(8) yes Fe1 . C29 . C33 . 70.42(8) yes C30 . C29 . C33 . 108.63(13) yes Fe1 . C29 . C38 . 129.04(10) yes C30 . C29 . C38 . 127.11(15) yes C33 . C29 . C38 . 124.01(14) yes Fe1 . C30 . C29 . 69.54(8) yes Fe1 . C30 . C31 . 69.38(8) yes C29 . C30 . C31 . 107.34(13) yes Fe1 . C30 . C37 . 133.91(10) yes C29 . C30 . C37 . 126.12(14) yes C31 . C30 . C37 . 125.80(13) yes Fe1 . C31 . C30 . 71.17(8) yes Fe1 . C31 . C32 . 70.10(8) yes C30 . C31 . C32 . 108.26(12) yes Fe1 . C31 . C36 . 128.61(10) yes C30 . C31 . C36 . 125.99(14) yes C32 . C31 . C36 . 125.53(14) yes Fe1 . C32 . C31 . 69.77(8) yes Fe1 . C32 . C33 . 70.70(8) yes C31 . C32 . C33 . 107.96(13) yes Fe1 . C32 . C35 . 126.27(11) yes C31 . C32 . C35 . 125.92(14) yes C33 . C32 . C35 . 126.11(14) yes Fe1 . C33 . C29 . 69.83(8) yes Fe1 . C33 . C32 . 70.05(8) yes C29 . C33 . C32 . 107.81(13) yes Fe1 . C33 . C34 . 128.67(11) yes C29 . C33 . C34 . 125.36(14) yes C32 . C33 . C34 . 126.71(15) yes C33 . C34 . H341 . 113.3 no C33 . C34 . H343 . 110.8 no H341 . C34 . H343 . 108.7 no C33 . C34 . H342 . 109.9 no H341 . C34 . H342 . 108.8 no H343 . C34 . H342 . 105.0 no C32 . C35 . H352 . 112.9 no C32 . C35 . H351 . 110.5 no H352 . C35 . H351 . 106.3 no C32 . C35 . H353 . 109.2 no H352 . C35 . H353 . 107.8 no H351 . C35 . H353 . 110.1 no C31 . C36 . H361 . 110.3 no C31 . C36 . H363 . 112.6 no H361 . C36 . H363 . 106.2 no C31 . C36 . H362 . 110.4 no H361 . C36 . H362 . 109.4 no H363 . C36 . H362 . 107.9 no C30 . C37 . H372 . 111.9 no C30 . C37 . H371 . 110.6 no H372 . C37 . H371 . 108.6 no C30 . C37 . H373 . 113.2 no H372 . C37 . H373 . 107.4 no H371 . C37 . H373 . 104.8 no C29 . C38 . H381 . 110.1 no C29 . C38 . H383 . 111.0 no H381 . C38 . H383 . 108.2 no C29 . C38 . H382 . 111.4 no H381 . C38 . H382 . 108.6 no H383 . C38 . H382 . 107.4 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 C132 . H1322 . O26 . 159.80(10) 0.971 2.562 3.490(6) yes C112 . H1121 . C122 2_665 160.2(3) 0.957 2.567 3.483(6) yes _iucr_refine_instruction_details_constraints ; # # Punched on 21/03/12 at 13:36:10 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 121,X'S) H (1211,X'S) RIDE C ( 122,X'S) H (1223,X'S) H (1222,X'S) H (1221,X'S) RIDE C ( 123,X'S) H (1231,X'S) H (1232,X'S) H (1233,X'S) RIDE C ( 131,X'S) H (1311,X'S) RIDE C ( 132,X'S) H (1321,X'S) H (1322,X'S) H (1323,X'S) RIDE C ( 133,X'S) H (1331,X'S) H (1332,X'S) H (1333,X'S) RIDE C ( 101,X'S) H (1011,X'S) RIDE C ( 102,X'S) H (1021,X'S) H (1022,X'S) H (1023,X'S) RIDE C ( 103,X'S) H (1033,X'S) H (1032,X'S) H (1031,X'S) RIDE C ( 111,X'S) H (1111,X'S) RIDE C ( 112,X'S) H (1123,X'S) H (1122,X'S) H (1121,X'S) RIDE C ( 113,X'S) H (1131,X'S) H (1132,X'S) H (1133,X'S) RIDE C ( 6,X'S) H ( 61,X'S) RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) RIDE C ( 10,X'S) H ( 101,X'S) H ( 102,X'S) RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S) RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) RIDE C ( 21,X'S) H ( 211,X'S) H ( 212,X'S) RIDE C ( 22,X'S) H ( 221,X'S) H ( 222,X'S) RIDE C ( 23,X'S) H ( 231,X'S) H ( 232,X'S) RIDE C ( 24,X'S) H ( 242,X'S) H ( 243,X'S) H ( 241,X'S) RIDE C ( 34,X'S) H ( 341,X'S) H ( 343,X'S) H ( 342,X'S) RIDE C ( 35,X'S) H ( 352,X'S) H ( 351,X'S) H ( 353,X'S) RIDE C ( 36,X'S) H ( 361,X'S) H ( 363,X'S) H ( 362,X'S) RIDE C ( 37,X'S) H ( 372,X'S) H ( 371,X'S) H ( 373,X'S) RIDE C ( 38,X'S) H ( 381,X'S) H ( 383,X'S) H ( 382,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 21/03/12 at 13:36:10 # #LIST 16 REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM 1 H ON SP 3 DIST 0.98, 0.02 = CONT C ( 121) TO H(1211) REST 0.069, 0.002 = H(1211,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1211) TO C ( 121) TO C(122) CONT H(1211) TO C ( 121) TO C(123) CONT H(1211) TO C ( 121) TO N(100) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 122) TO H(1223) CONT C ( 122) TO H(1222) CONT C ( 122) TO H(1221) REST 0.094, 0.002 = H(1223,U[ISO]) REST 0.094, 0.002 = H(1222,U[ISO]) REST 0.094, 0.002 = H(1221,U[ISO]) ANGLE 109.54, 2.0 = CONT C(121) TO C ( 122) TO H(1223) CONT C(121) TO C ( 122) TO H(1222) CONT C(121) TO C ( 122) TO H(1221) ANGLE 0.0, 2.0 = MEAN H(1223) TO C ( 122) TO H(1222) CONT H(1223) TO C ( 122) TO H(1221) CONT H(1222) TO C ( 122) TO H(1221) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 123) TO H(1231) CONT C ( 123) TO H(1232) CONT C ( 123) TO H(1233) REST 0.100, 0.002 = H(1231,U[ISO]) REST 0.100, 0.002 = H(1232,U[ISO]) REST 0.100, 0.002 = H(1233,U[ISO]) ANGLE 109.54, 2.0 = CONT C(121) TO C ( 123) TO H(1231) CONT C(121) TO C ( 123) TO H(1232) CONT C(121) TO C ( 123) TO H(1233) ANGLE 0.0, 2.0 = MEAN H(1231) TO C ( 123) TO H(1232) CONT H(1231) TO C ( 123) TO H(1233) CONT H(1232) TO C ( 123) TO H(1233) REM 1 H ON SP 3 DIST 0.98, 0.02 = CONT C ( 131) TO H(1311) REST 0.042, 0.002 = H(1311,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1311) TO C ( 131) TO C(132) CONT H(1311) TO C ( 131) TO C(133) CONT H(1311) TO C ( 131) TO N(100) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 132) TO H(1321) CONT C ( 132) TO H(1322) CONT C ( 132) TO H(1323) REST 0.074, 0.002 = H(1321,U[ISO]) REST 0.074, 0.002 = H(1322,U[ISO]) REST 0.074, 0.002 = H(1323,U[ISO]) ANGLE 109.54, 2.0 = CONT C(131) TO C ( 132) TO H(1321) CONT C(131) TO C ( 132) TO H(1322) CONT C(131) TO C ( 132) TO H(1323) ANGLE 0.0, 2.0 = MEAN H(1321) TO C ( 132) TO H(1322) CONT H(1321) TO C ( 132) TO H(1323) CONT H(1322) TO C ( 132) TO H(1323) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 133) TO H(1331) CONT C ( 133) TO H(1332) CONT C ( 133) TO H(1333) REST 0.073, 0.002 = H(1331,U[ISO]) REST 0.073, 0.002 = H(1332,U[ISO]) REST 0.073, 0.002 = H(1333,U[ISO]) ANGLE 109.54, 2.0 = CONT C(131) TO C ( 133) TO H(1331) CONT C(131) TO C ( 133) TO H(1332) CONT C(131) TO C ( 133) TO H(1333) ANGLE 0.0, 2.0 = MEAN H(1331) TO C ( 133) TO H(1332) CONT H(1331) TO C ( 133) TO H(1333) CONT H(1332) TO C ( 133) TO H(1333) REM 1 H ON SP 3 DIST 0.98, 0.02 = CONT C ( 101) TO H(1011) REST 0.069, 0.002 = H(1011,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1011) TO C ( 101) TO N(100) CONT H(1011) TO C ( 101) TO C(102) CONT H(1011) TO C ( 101) TO C(103) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 102) TO H(1021) CONT C ( 102) TO H(1022) CONT C ( 102) TO H(1023) REST 0.111, 0.002 = H(1021,U[ISO]) REST 0.111, 0.002 = H(1022,U[ISO]) REST 0.111, 0.002 = H(1023,U[ISO]) ANGLE 109.54, 2.0 = CONT C(101) TO C ( 102) TO H(1021) CONT C(101) TO C ( 102) TO H(1022) CONT C(101) TO C ( 102) TO H(1023) ANGLE 0.0, 2.0 = MEAN H(1021) TO C ( 102) TO H(1022) CONT H(1021) TO C ( 102) TO H(1023) CONT H(1022) TO C ( 102) TO H(1023) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 103) TO H(1031) CONT C ( 103) TO H(1032) CONT C ( 103) TO H(1033) REST 0.070, 0.002 = H(1031,U[ISO]) REST 0.070, 0.002 = H(1032,U[ISO]) REST 0.070, 0.002 = H(1033,U[ISO]) ANGLE 109.54, 2.0 = CONT C(101) TO C ( 103) TO H(1031) CONT C(101) TO C ( 103) TO H(1032) CONT C(101) TO C ( 103) TO H(1033) ANGLE 0.0, 2.0 = MEAN H(1031) TO C ( 103) TO H(1032) CONT H(1031) TO C ( 103) TO H(1033) CONT H(1032) TO C ( 103) TO H(1033) REM 1 H ON SP 3 DIST 0.98, 0.02 = CONT C ( 111) TO H(1111) REST 0.043, 0.002 = H(1111,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(1111) TO C ( 111) TO N(100) CONT H(1111) TO C ( 111) TO C(112) CONT H(1111) TO C ( 111) TO C(113) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 112) TO H(1121) CONT C ( 112) TO H(1122) CONT C ( 112) TO H(1123) REST 0.067, 0.002 = H(1121,U[ISO]) REST 0.067, 0.002 = H(1122,U[ISO]) REST 0.067, 0.002 = H(1123,U[ISO]) ANGLE 109.54, 2.0 = CONT C(111) TO C ( 112) TO H(1121) CONT C(111) TO C ( 112) TO H(1122) CONT C(111) TO C ( 112) TO H(1123) ANGLE 0.0, 2.0 = MEAN H(1121) TO C ( 112) TO H(1122) CONT H(1121) TO C ( 112) TO H(1123) CONT H(1122) TO C ( 112) TO H(1123) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 113) TO H(1133) CONT C ( 113) TO H(1132) CONT C ( 113) TO H(1131) REST 0.071, 0.002 = H(1133,U[ISO]) REST 0.071, 0.002 = H(1132,U[ISO]) REST 0.071, 0.002 = H(1131,U[ISO]) ANGLE 109.54, 2.0 = CONT C(111) TO C ( 113) TO H(1133) CONT C(111) TO C ( 113) TO H(1132) CONT C(111) TO C ( 113) TO H(1131) ANGLE 0.0, 2.0 = MEAN H(1133) TO C ( 113) TO H(1132) CONT H(1133) TO C ( 113) TO H(1131) CONT H(1132) TO C ( 113) TO H(1131) REM 1 H ON SP 3 DIST 0.98, 0.02 = CONT C ( 6) TO H(61) REST 0.034, 0.002 = H(61,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(61) TO C ( 6) TO N(5) CONT H(61) TO C ( 6) TO C(7) CONT H(61) TO C ( 6) TO C(11) REM 2 H ON SP 3 DIST 0.97, 0.02 = CONT C ( 7) TO H(71) CONT C ( 7) TO H(72) REST 0.060, 0.002 = H(71,U[ISO]) REST 0.060, 0.002 = H(72,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(71) TO C ( 7) TO C(6) CONT H(71) TO C ( 7) TO C(8) CONT H(72) TO C ( 7) TO C(6) CONT H(72) TO C ( 7) TO C(8) ANGLE 109.54, 2.0 = CONT H(71) TO C ( 7) TO H(72) REM 2 H ON SP 3 DIST 0.97, 0.02 = CONT C ( 8) TO H(81) CONT C ( 8) TO H(82) REST 0.098, 0.002 = H(81,U[ISO]) REST 0.098, 0.002 = H(82,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(81) TO C ( 8) TO C(7) CONT H(81) TO C ( 8) TO C(9) CONT H(82) TO C ( 8) TO C(7) CONT H(82) TO C ( 8) TO C(9) ANGLE 109.54, 2.0 = CONT H(81) TO C ( 8) TO H(82) REM 2 H ON SP 3 DIST 0.97, 0.02 = CONT C ( 9) TO H(91) CONT C ( 9) TO H(92) REST 0.093, 0.002 = H(91,U[ISO]) REST 0.093, 0.002 = H(92,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(91) TO C ( 9) TO C(8) CONT H(91) TO C ( 9) TO C(10) CONT H(92) TO C ( 9) TO C(8) CONT H(92) TO C ( 9) TO C(10) ANGLE 109.54, 2.0 = CONT H(91) TO C ( 9) TO H(92) REM 2 H ON SP 3 DIST 0.97, 0.02 = CONT C ( 10) TO H(101) CONT C ( 10) TO H(102) REST 0.084, 0.002 = H(101,U[ISO]) REST 0.084, 0.002 = H(102,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(101) TO C ( 10) TO C(9) CONT H(101) TO C ( 10) TO C(11) CONT H(102) TO C ( 10) TO C(9) CONT H(102) TO C ( 10) TO C(11) ANGLE 109.54, 2.0 = CONT H(101) TO C ( 10) TO H(102) REM 2 H ON SP 3 DIST 0.97, 0.02 = CONT C ( 11) TO H(111) CONT C ( 11) TO H(112) REST 0.050, 0.002 = H(111,U[ISO]) REST 0.050, 0.002 = H(112,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(111) TO C ( 11) TO C(6) CONT H(111) TO C ( 11) TO C(10) CONT H(112) TO C ( 11) TO C(6) CONT H(112) TO C ( 11) TO C(10) ANGLE 109.54, 2.0 = CONT H(111) TO C ( 11) TO H(112) REM 1 H ON SP 3 DIST 0.98, 0.02 = CONT C ( 18) TO H(181) REST 0.033, 0.002 = H(181,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(181) TO C ( 18) TO N(3) CONT H(181) TO C ( 18) TO C(19) CONT H(181) TO C ( 18) TO C(23) REM 2 H ON SP 3 DIST 0.97, 0.02 = CONT C ( 19) TO H(191) CONT C ( 19) TO H(192) REST 0.041, 0.002 = H(191,U[ISO]) REST 0.041, 0.002 = H(192,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(191) TO C ( 19) TO C(18) CONT H(191) TO C ( 19) TO C(20) CONT H(192) TO C ( 19) TO C(18) CONT H(192) TO C ( 19) TO C(20) ANGLE 109.54, 2.0 = CONT H(191) TO C ( 19) TO H(192) REM 2 H ON SP 3 DIST 0.97, 0.02 = CONT C ( 20) TO H(201) CONT C ( 20) TO H(202) REST 0.055, 0.002 = H(201,U[ISO]) REST 0.055, 0.002 = H(202,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(201) TO C ( 20) TO C(19) CONT H(201) TO C ( 20) TO C(21) CONT H(202) TO C ( 20) TO C(19) CONT H(202) TO C ( 20) TO C(21) ANGLE 109.54, 2.0 = CONT H(201) TO C ( 20) TO H(202) REM 2 H ON SP 3 DIST 0.97, 0.02 = CONT C ( 21) TO H(211) CONT C ( 21) TO H(212) REST 0.062, 0.002 = H(211,U[ISO]) REST 0.062, 0.002 = H(212,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(211) TO C ( 21) TO C(20) CONT H(211) TO C ( 21) TO C(22) CONT H(212) TO C ( 21) TO C(20) CONT H(212) TO C ( 21) TO C(22) ANGLE 109.54, 2.0 = CONT H(211) TO C ( 21) TO H(212) REM 2 H ON SP 3 DIST 0.97, 0.02 = CONT C ( 22) TO H(221) CONT C ( 22) TO H(222) REST 0.061, 0.002 = H(221,U[ISO]) REST 0.061, 0.002 = H(222,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(221) TO C ( 22) TO C(21) CONT H(221) TO C ( 22) TO C(23) CONT H(222) TO C ( 22) TO C(21) CONT H(222) TO C ( 22) TO C(23) ANGLE 109.54, 2.0 = CONT H(221) TO C ( 22) TO H(222) REM 2 H ON SP 3 DIST 0.97, 0.02 = CONT C ( 23) TO H(231) CONT C ( 23) TO H(232) REST 0.041, 0.002 = H(231,U[ISO]) REST 0.041, 0.002 = H(232,U[ISO]) ANGLE 0.0, 2.0 = MEAN CONT H(231) TO C ( 23) TO C(22) CONT H(231) TO C ( 23) TO C(18) CONT H(232) TO C ( 23) TO C(22) CONT H(232) TO C ( 23) TO C(18) ANGLE 109.54, 2.0 = CONT H(231) TO C ( 23) TO H(232) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 34) TO H(341) CONT C ( 34) TO H(342) CONT C ( 34) TO H(343) REST 0.065, 0.002 = H(341,U[ISO]) REST 0.065, 0.002 = H(342,U[ISO]) REST 0.065, 0.002 = H(343,U[ISO]) ANGLE 109.54, 2.0 = CONT C(33) TO C ( 34) TO H(341) CONT C(33) TO C ( 34) TO H(342) CONT C(33) TO C ( 34) TO H(343) ANGLE 0.0, 2.0 = MEAN H(341) TO C ( 34) TO H(342) CONT H(341) TO C ( 34) TO H(343) CONT H(342) TO C ( 34) TO H(343) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 35) TO H(353) CONT C ( 35) TO H(352) CONT C ( 35) TO H(351) REST 0.063, 0.002 = H(353,U[ISO]) REST 0.063, 0.002 = H(352,U[ISO]) REST 0.063, 0.002 = H(351,U[ISO]) ANGLE 109.54, 2.0 = CONT C(32) TO C ( 35) TO H(353) CONT C(32) TO C ( 35) TO H(352) CONT C(32) TO C ( 35) TO H(351) ANGLE 0.0, 2.0 = MEAN H(353) TO C ( 35) TO H(352) CONT H(353) TO C ( 35) TO H(351) CONT H(352) TO C ( 35) TO H(351) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 36) TO H(361) CONT C ( 36) TO H(362) CONT C ( 36) TO H(363) REST 0.056, 0.002 = H(361,U[ISO]) REST 0.056, 0.002 = H(362,U[ISO]) REST 0.056, 0.002 = H(363,U[ISO]) ANGLE 109.54, 2.0 = CONT C(31) TO C ( 36) TO H(361) CONT C(31) TO C ( 36) TO H(362) CONT C(31) TO C ( 36) TO H(363) ANGLE 0.0, 2.0 = MEAN H(361) TO C ( 36) TO H(362) CONT H(361) TO C ( 36) TO H(363) CONT H(362) TO C ( 36) TO H(363) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 37) TO H(371) CONT C ( 37) TO H(372) CONT C ( 37) TO H(373) REST 0.058, 0.002 = H(371,U[ISO]) REST 0.058, 0.002 = H(372,U[ISO]) REST 0.058, 0.002 = H(373,U[ISO]) ANGLE 109.54, 2.0 = CONT C(30) TO C ( 37) TO H(371) CONT C(30) TO C ( 37) TO H(372) CONT C(30) TO C ( 37) TO H(373) ANGLE 0.0, 2.0 = MEAN H(371) TO C ( 37) TO H(372) CONT H(371) TO C ( 37) TO H(373) CONT H(372) TO C ( 37) TO H(373) REM 3 H ON SP 3 DIST 0.96, 0.02 = CONT C ( 38) TO H(381) CONT C ( 38) TO H(382) CONT C ( 38) TO H(383) REST 0.063, 0.002 = H(381,U[ISO]) REST 0.063, 0.002 = H(382,U[ISO]) REST 0.063, 0.002 = H(383,U[ISO]) ANGLE 109.54, 2.0 = CONT C(29) TO C ( 38) TO H(381) CONT C(29) TO C ( 38) TO H(382) CONT C(29) TO C ( 38) TO H(383) ANGLE 0.0, 2.0 = MEAN H(381) TO C ( 38) TO H(382) CONT H(381) TO C ( 38) TO H(383) CONT H(382) TO C ( 38) TO H(383) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; data_PhC(CyN)2AlCl2 _database_code_depnum_ccdc_archive 'CCDC 894967' #TrackingRef 'Combined Final VRFs.cif' #============================================================================== _audit_creation_date 12-07-10 _audit_creation_method CRYSTALS_ver_14.40 _oxford_structure_analysis_title '047irmk11.cif_od At 17: 1 on 10/ 7' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 9.95850(10) _cell_length_b 9.27690(10) _cell_length_c 22.85560(10) _cell_angle_alpha 90 _cell_angle_beta 101.6000(7) _cell_angle_gamma 90 _cell_volume 2068.37(3) _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _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 0.0181 0.0091 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' N 0.0311 0.0180 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 0.2130 0.2455 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 0.3639 0.7018 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' 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' _cell_formula_units_Z 4 # Given Formula = C19 H34 Al1 Cl2 N2 # Dc = 1.25 Fooo = 808.00 Mu = 32.44 M = 388.38 # Found Formula = C19 H27 Al1 Cl2 N2 # Dc = 1.22 FOOO = 808.00 Mu = 32.43 M = 381.32 _chemical_formula_sum 'C19 H27 Al1 Cl2 N2' _chemical_formula_moiety 'C19 H27 Al1 Cl2 N2' _chemical_compound_source . _chemical_formula_weight 381.32 _cell_measurement_reflns_used 15605 _cell_measurement_theta_min 4 _cell_measurement_theta_max 76 _cell_measurement_temperature 150 _exptl_crystal_description . _exptl_crystal_colour yellow _exptl_crystal_size_min 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.100 _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 3.243 # Sheldrick geometric approximatio 0.72 0.72 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlis, (Oxford Diffraction, 2002)' _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.72 _diffrn_measurement_device_type 'Oxford Diffraction SuperNova' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SuperNova, (Oxford Diffraction, 2010)' _computing_cell_refinement 'CrysAlis, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis, (Oxford Diffraction, 2002)' _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 22073 _reflns_number_total 4338 _diffrn_reflns_av_R_equivalents 0.020 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 4338 # Theoretical number of reflections is about 8704 _diffrn_reflns_theta_min 4.566 _diffrn_reflns_theta_max 76.595 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 76.595 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 22 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 11 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _oxford_diffrn_Wilson_B_factor 3.16 _oxford_diffrn_Wilson_scale 0.03 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_diff_density_min -0.32 _refine_diff_density_max 0.39 # 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>0.0\s(I) _refine_ls_number_reflns 4324 _refine_ls_number_restraints 0 _refine_ls_number_parameters 217 _oxford_refine_ls_R_factor_ref 0.0339 _refine_ls_wR_factor_ref 0.0755 _refine_ls_goodness_of_fit_ref 0.8982 _refine_ls_shift/su_max 0.0011384 _refine_ls_shift/su_mean 0.0000511 # The values computed with all filters except I/sigma _oxford_reflns_number_all 4324 _refine_ls_R_factor_all 0.0339 _refine_ls_wR_factor_all 0.0755 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4229 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_gt 0.0754 # 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 #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: 0.169E+04 0.282E+04 0.173E+04 726. 173. ; # Insert your own references if required - in alphabetical order 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 Cl1 Cl 0.28737(4) 0.41959(4) 0.542274(15) 0.0471 1.0000 Uani . . . . . . Al2 Al 0.14751(4) 0.25148(5) 0.549632(17) 0.0335 1.0000 Uani . . . . . . Cl3 Cl 0.02538(4) 0.20013(5) 0.465534(16) 0.0541 1.0000 Uani . . . . . . N4 N 0.21481(12) 0.09788(13) 0.60125(5) 0.0351 1.0000 Uani . . . . . . C5 C 0.12972(13) 0.13650(15) 0.63666(6) 0.0305 1.0000 Uani . . . . . . N6 N 0.05982(12) 0.25470(13) 0.61548(5) 0.0373 1.0000 Uani . . . . . . C7 C -0.05527(14) 0.31422(16) 0.63841(6) 0.0358 1.0000 Uani . . . . . . C8 C -0.19046(16) 0.26526(18) 0.60040(9) 0.0500 1.0000 Uani . . . . . . C9 C -0.31208(17) 0.33041(19) 0.62264(10) 0.0540 1.0000 Uani . . . . . . C10 C -0.30361(15) 0.49370(17) 0.62389(7) 0.0405 1.0000 Uani . . . . . . C11 C -0.16913(16) 0.54478(19) 0.66079(8) 0.0486 1.0000 Uani . . . . . . C12 C -0.04716(15) 0.47803(17) 0.63947(8) 0.0464 1.0000 Uani . . . . . . C13 C 0.11465(13) 0.06129(14) 0.69246(6) 0.0293 1.0000 Uani . . . . . . C14 C 0.17591(14) 0.11904(16) 0.74731(6) 0.0363 1.0000 Uani . . . . . . C15 C 0.16234(14) 0.04998(16) 0.79975(6) 0.0358 1.0000 Uani . . . . . . C16 C 0.08627(15) -0.07505(16) 0.79726(6) 0.0365 1.0000 Uani . . . . . . C17 C 0.02373(18) -0.13118(17) 0.74277(7) 0.0450 1.0000 Uani . . . . . . C18 C 0.03813(17) -0.06393(17) 0.69003(6) 0.0408 1.0000 Uani . . . . . . C19 C 0.31304(14) -0.02050(15) 0.61130(6) 0.0337 1.0000 Uani . . . . . . C20 C 0.44375(15) 0.02229(17) 0.65480(7) 0.0404 1.0000 Uani . . . . . . C21 C 0.55604(18) -0.0919(2) 0.65917(8) 0.0500 1.0000 Uani . . . . . . C22 C 0.58503(16) -0.12691(17) 0.59773(8) 0.0458 1.0000 Uani . . . . . . C23 C 0.45505(17) -0.17625(18) 0.55610(8) 0.0489 1.0000 Uani . . . . . . C24 C 0.34353(16) -0.06204(18) 0.55055(7) 0.0428 1.0000 Uani . . . . . . H71 H -0.0495 0.2799 0.6805 0.0446 1.0000 Uiso R . . . . . H82 H -0.1965 0.1586 0.6017 0.0643 1.0000 Uiso R . . . . . H81 H -0.1902 0.2995 0.5576 0.0635 1.0000 Uiso R . . . . . H91 H -0.3061 0.2962 0.6656 0.0700 1.0000 Uiso R . . . . . H92 H -0.4026 0.3004 0.5962 0.0704 1.0000 Uiso R . . . . . H102 H -0.3803 0.5342 0.6408 0.0492 1.0000 Uiso R . . . . . H101 H -0.3106 0.5268 0.5817 0.0503 1.0000 Uiso R . . . . . H112 H -0.1655 0.5115 0.7032 0.0614 1.0000 Uiso R . . . . . H111 H -0.1655 0.6526 0.6592 0.0626 1.0000 Uiso R . . . . . H121 H 0.0402 0.5071 0.6674 0.0596 1.0000 Uiso R . . . . . H122 H -0.0466 0.5088 0.5972 0.0594 1.0000 Uiso R . . . . . H141 H 0.2290 0.2074 0.7484 0.0456 1.0000 Uiso R . . . . . H151 H 0.2059 0.0897 0.8385 0.0452 1.0000 Uiso R . . . . . H161 H 0.0770 -0.1230 0.8342 0.0440 1.0000 Uiso R . . . . . H171 H -0.0314 -0.2175 0.7412 0.0564 1.0000 Uiso R . . . . . H181 H -0.0071 -0.1033 0.6508 0.0506 1.0000 Uiso R . . . . . H191 H 0.2717 -0.1064 0.6288 0.0395 1.0000 Uiso R . . . . . H202 H 0.4204 0.0377 0.6950 0.0505 1.0000 Uiso R . . . . . H201 H 0.4770 0.1144 0.6393 0.0506 1.0000 Uiso R . . . . . H211 H 0.6422 -0.0584 0.6865 0.0634 1.0000 Uiso R . . . . . H212 H 0.5231 -0.1823 0.6753 0.0628 1.0000 Uiso R . . . . . H222 H 0.6582 -0.2028 0.6016 0.0562 1.0000 Uiso R . . . . . H221 H 0.6171 -0.0376 0.5789 0.0556 1.0000 Uiso R . . . . . H232 H 0.4217 -0.2654 0.5741 0.0609 1.0000 Uiso R . . . . . H231 H 0.4746 -0.1974 0.5162 0.0606 1.0000 Uiso R . . . . . H241 H 0.3797 0.0287 0.5341 0.0544 1.0000 Uiso R . . . . . H242 H 0.2566 -0.0933 0.5230 0.0546 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 0.0566(2) 0.0543(2) 0.03106(17) 0.00475(14) 0.01072(15) -0.02109(17) Al2 0.0362(2) 0.0401(2) 0.02611(19) 0.00504(16) 0.01075(16) -0.00178(16) Cl3 0.0611(2) 0.0675(3) 0.02995(18) 0.00316(16) 0.00014(16) -0.0207(2) N4 0.0376(6) 0.0408(6) 0.0305(6) 0.0054(5) 0.0153(5) 0.0035(5) C5 0.0300(6) 0.0357(7) 0.0273(6) 0.0028(5) 0.0091(5) -0.0017(5) N6 0.0385(6) 0.0436(7) 0.0335(6) 0.0114(5) 0.0159(5) 0.0080(5) C7 0.0376(7) 0.0409(7) 0.0321(7) 0.0090(6) 0.0144(5) 0.0070(6) C8 0.0398(8) 0.0384(8) 0.0759(12) -0.0146(8) 0.0212(8) -0.0070(6) C9 0.0387(8) 0.0447(9) 0.0835(13) -0.0087(9) 0.0242(8) -0.0051(7) C10 0.0369(7) 0.0420(8) 0.0447(8) 0.0025(6) 0.0133(6) 0.0047(6) C11 0.0457(8) 0.0439(8) 0.0543(9) -0.0120(7) 0.0053(7) 0.0039(7) C12 0.0340(7) 0.0433(8) 0.0602(10) -0.0078(7) 0.0050(7) -0.0041(6) C13 0.0293(6) 0.0330(6) 0.0279(6) 0.0045(5) 0.0109(5) 0.0029(5) C14 0.0388(7) 0.0390(7) 0.0324(7) 0.0020(6) 0.0101(6) -0.0063(6) C15 0.0381(7) 0.0432(7) 0.0269(6) 0.0016(5) 0.0084(5) 0.0008(6) C16 0.0428(7) 0.0386(7) 0.0314(7) 0.0086(5) 0.0154(6) 0.0043(6) C17 0.0587(9) 0.0404(8) 0.0379(8) 0.0040(6) 0.0144(7) -0.0146(7) C18 0.0520(8) 0.0409(8) 0.0303(7) 0.0001(6) 0.0100(6) -0.0102(7) C19 0.0373(7) 0.0319(6) 0.0355(7) 0.0009(5) 0.0162(5) -0.0009(5) C20 0.0417(8) 0.0417(8) 0.0388(7) -0.0045(6) 0.0101(6) 0.0042(6) C21 0.0471(9) 0.0542(10) 0.0493(9) 0.0037(8) 0.0115(7) 0.0126(7) C22 0.0434(8) 0.0402(8) 0.0588(10) 0.0017(7) 0.0223(7) 0.0079(6) C23 0.0534(9) 0.0421(8) 0.0587(10) -0.0133(7) 0.0289(8) -0.0025(7) C24 0.0407(8) 0.0523(9) 0.0387(8) -0.0110(7) 0.0158(6) -0.0029(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 6.21(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 Cl1 . Al2 . 2.1200(5) yes Al2 . Cl3 . 2.1120(5) yes Al2 . N4 . 1.8851(12) yes Al2 . C5 . 2.2951(13) yes Al2 . N6 . 1.8860(12) yes N4 . C5 . 1.3332(16) yes N4 . C19 . 1.4578(18) yes C5 . N6 . 1.3363(18) yes C5 . C13 . 1.4875(17) yes N6 . C7 . 1.4611(17) yes C7 . C8 . 1.518(2) yes C7 . C12 . 1.522(2) yes C7 . H71 . 1.004 no C8 . C9 . 1.529(2) yes C8 . H82 . 0.992 no C8 . H81 . 1.029 no C9 . C10 . 1.517(2) yes C9 . H91 . 1.022 no C9 . H92 . 1.019 no C10 . C11 . 1.508(2) yes C10 . H102 . 0.996 no C10 . H101 . 1.001 no C11 . C12 . 1.528(2) yes C11 . H112 . 1.010 no C11 . H111 . 1.002 no C12 . H121 . 1.007 no C12 . H122 . 1.009 no C13 . C14 . 1.3868(19) yes C13 . C18 . 1.3842(19) yes C14 . C15 . 1.3894(19) yes C14 . H141 . 0.973 no C15 . C16 . 1.380(2) yes C15 . H151 . 0.976 no C16 . C17 . 1.378(2) yes C16 . H161 . 0.975 no C17 . C18 . 1.390(2) yes C17 . H171 . 0.968 no C18 . H181 . 0.989 no C19 . C20 . 1.523(2) yes C19 . C24 . 1.5291(18) yes C19 . H191 . 1.015 no C20 . C21 . 1.529(2) yes C20 . H202 . 1.002 no C20 . H201 . 1.007 no C21 . C22 . 1.524(2) yes C21 . H211 . 1.004 no C21 . H212 . 0.998 no C22 . C23 . 1.515(2) yes C22 . H222 . 1.004 no C22 . H221 . 1.014 no C23 . C24 . 1.522(2) yes C23 . H232 . 1.009 no C23 . H231 . 0.990 no C24 . H241 . 1.016 no C24 . H242 . 1.006 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 . 111.16(2) yes Cl1 . Al2 . N4 . 116.69(4) yes Cl3 . Al2 . N4 . 117.79(4) yes Cl1 . Al2 . C5 . 125.25(4) yes Cl3 . Al2 . C5 . 123.59(4) yes N4 . Al2 . C5 . 35.51(5) yes Cl1 . Al2 . N6 . 117.94(5) yes Cl3 . Al2 . N6 . 117.10(4) yes N4 . Al2 . N6 . 71.09(5) yes C5 . Al2 . N6 . 35.60(5) yes Al2 . N4 . C5 . 89.28(8) yes Al2 . N4 . C19 . 144.19(9) yes C5 . N4 . C19 . 126.51(11) yes Al2 . C5 . N4 . 55.21(7) yes Al2 . C5 . N6 . 55.25(7) yes N4 . C5 . N6 . 110.42(11) yes Al2 . C5 . C13 . 178.62(10) yes N4 . C5 . C13 . 125.48(12) yes N6 . C5 . C13 . 124.09(12) yes C5 . N6 . Al2 . 89.15(8) yes C5 . N6 . C7 . 124.69(11) yes Al2 . N6 . C7 . 144.56(9) yes N6 . C7 . C8 . 110.56(12) yes N6 . C7 . C12 . 109.88(12) yes C8 . C7 . C12 . 110.25(12) yes N6 . C7 . H71 . 109.0 no C8 . C7 . H71 . 109.1 no C12 . C7 . H71 . 108.0 no C7 . C8 . C9 . 111.24(14) yes C7 . C8 . H82 . 109.5 no C9 . C8 . H82 . 109.1 no C7 . C8 . H81 . 106.3 no C9 . C8 . H81 . 110.3 no H82 . C8 . H81 . 110.3 no C8 . C9 . C10 . 110.86(13) yes C8 . C9 . H91 . 107.4 no C10 . C9 . H91 . 107.5 no C8 . C9 . H92 . 111.1 no C10 . C9 . H92 . 108.9 no H91 . C9 . H92 . 111.0 no C9 . C10 . C11 . 111.34(14) yes C9 . C10 . H102 . 109.9 no C11 . C10 . H102 . 109.2 no C9 . C10 . H101 . 107.2 no C11 . C10 . H101 . 108.9 no H102 . C10 . H101 . 110.4 no C10 . C11 . C12 . 111.57(13) yes C10 . C11 . H112 . 107.2 no C12 . C11 . H112 . 107.7 no C10 . C11 . H111 . 109.2 no C12 . C11 . H111 . 110.9 no H112 . C11 . H111 . 110.2 no C11 . C12 . C7 . 111.51(13) yes C11 . C12 . H121 . 109.3 no C7 . C12 . H121 . 108.3 no C11 . C12 . H122 . 110.4 no C7 . C12 . H122 . 106.1 no H121 . C12 . H122 . 111.2 no C5 . C13 . C14 . 119.47(12) yes C5 . C13 . C18 . 120.59(12) yes C14 . C13 . C18 . 119.93(12) yes C13 . C14 . C15 . 120.02(13) yes C13 . C14 . H141 . 119.2 no C15 . C14 . H141 . 120.8 no C14 . C15 . C16 . 119.98(13) yes C14 . C15 . H151 . 120.4 no C16 . C15 . H151 . 119.7 no C15 . C16 . C17 . 119.97(13) yes C15 . C16 . H161 . 119.6 no C17 . C16 . H161 . 120.4 no C16 . C17 . C18 . 120.50(14) yes C16 . C17 . H171 . 119.7 no C18 . C17 . H171 . 119.8 no C17 . C18 . C13 . 119.60(14) yes C17 . C18 . H181 . 120.9 no C13 . C18 . H181 . 119.5 no N4 . C19 . C20 . 111.40(11) yes N4 . C19 . C24 . 107.23(12) yes C20 . C19 . C24 . 111.02(11) yes N4 . C19 . H191 . 109.9 no C20 . C19 . H191 . 108.0 no C24 . C19 . H191 . 109.3 no C19 . C20 . C21 . 112.32(13) yes C19 . C20 . H202 . 108.1 no C21 . C20 . H202 . 109.9 no C19 . C20 . H201 . 106.8 no C21 . C20 . H201 . 108.9 no H202 . C20 . H201 . 110.8 no C20 . C21 . C22 . 111.03(13) yes C20 . C21 . H211 . 110.4 no C22 . C21 . H211 . 110.1 no C20 . C21 . H212 . 108.4 no C22 . C21 . H212 . 107.4 no H211 . C21 . H212 . 109.5 no C21 . C22 . C23 . 110.30(13) yes C21 . C22 . H222 . 109.7 no C23 . C22 . H222 . 110.9 no C21 . C22 . H221 . 110.5 no C23 . C22 . H221 . 106.4 no H222 . C22 . H221 . 109.0 no C22 . C23 . C24 . 111.04(13) yes C22 . C23 . H232 . 107.5 no C24 . C23 . H232 . 108.1 no C22 . C23 . H231 . 109.7 no C24 . C23 . H231 . 109.7 no H232 . C23 . H231 . 110.8 no C19 . C24 . C23 . 112.01(13) yes C19 . C24 . H241 . 106.1 no C23 . C24 . H241 . 107.5 no C19 . C24 . H242 . 109.8 no C23 . C24 . H242 . 111.9 no H241 . C24 . H242 . 109.3 no _iucr_refine_instruction_details_constraints ; # # Punched on 10/07/12 at 17:04:44 # #LIST 12 BLOCK SCALE X'S, U'S RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 82,X'S) H ( 81,X'S) RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) RIDE C ( 10,X'S) H ( 102,X'S) H ( 101,X'S) RIDE C ( 11,X'S) H ( 112,X'S) H ( 111,X'S) RIDE C ( 12,X'S) H ( 121,X'S) H ( 122,X'S) RIDE C ( 14,X'S) H ( 141,X'S) RIDE C ( 15,X'S) H ( 151,X'S) RIDE C ( 16,X'S) H ( 161,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 18,X'S) H ( 181,X'S) RIDE C ( 19,X'S) H ( 191,X'S) RIDE C ( 20,X'S) H ( 202,X'S) H ( 201,X'S) RIDE C ( 21,X'S) H ( 211,X'S) H ( 212,X'S) RIDE C ( 22,X'S) H ( 222,X'S) H ( 221,X'S) RIDE C ( 23,X'S) H ( 232,X'S) H ( 231,X'S) RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 10/07/12 at 17:04:44 # #LIST 16 NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #============================================================================== # start Validation Reply Form #============================================================================== _vrf_PLAT220_8 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.3 Ratio RESPONSE: This results from some terminal carbon atoms having more dynamic motion than others towards the centre of the molecule. ; _vrf_PLAT230_8 ; PROBLEM: Hirshfeld Test Diff for O28 -- C27 .. 11.3 su RESPONSE: This issue is not uncommon for metal bound carbonyl fragments and has been discussed at length by D. Braga and T. F. Koetzle, Acta. Cryst. (1988) B44 p 155-6. ; _vrf_PLAT410_8 ; PROBLEM: Short Intra H...H Contact H61 .. H1111 .. 1.85 Ang. RESPONSE: The issue arises from the close approach of the minor component of a disordered iso-propyl group to the hydrogen of a cyclohexyl residue. The approach is not significant and has no bearing on the structural parameters discussed. ; _vrf_PLAT232_6 ; PROBLEM: Hirshfeld Test Diff for O28 -- C27 .. 11.3 su RESPONSE: This issue is not uncommon for metal bound carbonyl fragments and has been discussed at length by D. Braga and T. F. Koetzle, Acta. Cryst. (1988) B44 p 155-6. ; _vrf_PLAT232_2c ; PROBLEM: Hirshfeld Test Diff for O28 -- C27 .. 11.3 su RESPONSE: This issue is not uncommon for metal bound carbonyl fragments and has been discussed at length by D. Braga and T. F. Koetzle, Acta. Cryst. (1988) B44 p 155-6. ; #============================================================================== # end Validation Reply Form #==============================================================================