# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_'complex1_AlMe2t-Bu'
_database_code_depnum_ccdc_archive 'CCDC 1551837'
_audit_update_record
;
2018-03-20 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety 'C54 H76 Al2 N2 O6'
_chemical_formula_sum 'C54 H76 Al2 N2 O6'
_chemical_formula_iupac ?
_chemical_formula_weight 903.12
_chemical_melting_point ?
_space_group_crystal_system monoclinic
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 21.288(10)
_cell_length_b 10.071(5)
_cell_length_c 26.440(13)
_cell_angle_alpha 90
_cell_angle_beta 112.811(18)
_cell_angle_gamma 90
_cell_volume 5225.(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9183
_cell_measurement_theta_min 2.3172
_cell_measurement_theta_max 36.9812
_cell_measurement_temperature 100
_exptl_crystal_description rectangle
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_size_max 0.365
_exptl_crystal_size_mid 0.212
_exptl_crystal_size_min 0.065
_exptl_crystal_density_diffrn 1.148
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1952
_exptl_absorpt_coefficient_mu 0.104
_exptl_absorpt_correction_type Multi-Scan
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min 0.94
_exptl_absorpt_correction_T_max 0.99
_exptl_special_details
;
;
_diffrn_ambient_temperature 100
_diffrn_source 'microfocus sealed x-ray tube'
_diffrn_source_type 'Incoatec I\mus'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator ?
_diffrn_measurement_device_type 'Bruker D8 venture'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number 311773
_diffrn_reflns_av_R_equivalents 0.1482
_diffrn_reflns_av_unetI/netI 0.0499
_diffrn_reflns_theta_min 2.19
_diffrn_reflns_theta_max 35.58
_diffrn_reflns_theta_full 35.58
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min -34
_diffrn_reflns_limit_h_max 34
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -43
_diffrn_reflns_limit_l_max 43
_refine_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_number_total 23962
_reflns_number_gt 17523
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0779
_refine_ls_R_factor_gt 0.0530
_refine_ls_wR_factor_gt 0.1354
_refine_ls_wR_factor_ref 0.1485
_refine_ls_goodness_of_fit_ref 1.041
_refine_ls_restrained_S_all 1.041
_refine_ls_number_reflns 23962
_refine_ls_number_parameters 593
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+0.9523P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.802
_refine_diff_density_min -0.609
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection 'APEX3 v2015.5-2 (Bruker AXS Inc., 2015)'
_computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution 'XT, VERSION 2014/4'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 717)'
_computing_publication_material 'Bruker SHELXL (Bruker AXS Inc., 2015)'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al Al1 0.62291(2) 0.25346(3) 0.32436(2) 0.01206(6) Uani d . . . 1 . .
O O1 0.64134(4) 0.40768(7) 0.35863(3) 0.01686(13) Uani d . . . 1 . .
N N1 0.71470(4) 0.23258(7) 0.31730(3) 0.01001(12) Uani d . . . 1 . .
C C1 0.69627(5) 0.48683(9) 0.37481(4) 0.01163(14) Uani d . . . 1 . .
Al Al2 0.86808(2) 0.61600(3) 0.67179(2) 0.01445(6) Uani d . . . 1 . .
O O2 0.85748(4) 0.08533(8) 0.34306(3) 0.01822(14) Uani d . . . 1 . .
N N2 0.77815(4) 0.63973(7) 0.68141(3) 0.01056(12) Uani d . . . 1 . .
C C2 0.70457(5) 0.59063(9) 0.41320(4) 0.01228(14) Uani d . . . 1 . .
O O3 0.71891(4) -0.08025(7) 0.30388(3) 0.01548(13) Uani d . . . 1 . .
C C3 0.76482(5) 0.66552(9) 0.42996(4) 0.01293(15) Uani d . . . 1 . .
H H3 0.7708 0.7345 0.4559 0.016 Uiso calc U . R 1 . .
C C4 0.81655(5) 0.64418(9) 0.41054(4) 0.01196(14) Uani d . . . 1 . .
O O4 0.84942(4) 0.45866(8) 0.64044(3) 0.01883(14) Uani d . . . 1 . .
C C5 0.80563(5) 0.54424(9) 0.37140(4) 0.01206(14) Uani d . . . 1 . .
H H5 0.8394 0.528 0.357 0.014 Uiso calc U . R 1 . .
O O5 0.63902(4) 0.79051(8) 0.66282(3) 0.01835(14) Uani d . . . 1 . .
C C6 0.74627(5) 0.46749(9) 0.35293(4) 0.01081(14) Uani d . . . 1 . .
O O6 0.77437(4) 0.95227(7) 0.69327(3) 0.01656(13) Uani d . . . 1 . .
C C7 0.64882(5) 0.62070(10) 0.43495(4) 0.01510(16) Uani d . . . 1 . .
C C8 0.58089(6) 0.65158(12) 0.38636(5) 0.0227(2) Uani d . . . 1 . .
H H8A 0.5868 0.7295 0.3665 0.034 Uiso calc U . R 1 . .
H H8B 0.5453 0.6696 0.4004 0.034 Uiso calc U . R 1 . .
H H8C 0.5675 0.5752 0.3615 0.034 Uiso calc U . R 1 . .
C C9 0.63974(6) 0.50156(11) 0.46792(5) 0.02080(19) Uani d . . . 1 . .
H H9A 0.6304 0.4215 0.4451 0.031 Uiso calc U . R 1 . .
H H9B 0.6016 0.5186 0.479 0.031 Uiso calc U . R 1 . .
H H9C 0.6815 0.4887 0.5007 0.031 Uiso calc U . R 1 . .
C C10 0.66601(6) 0.74262(11) 0.47300(5) 0.0227(2) Uani d . . . 1 . .
H H10A 0.6701 0.8211 0.4526 0.034 Uiso calc U . R 1 . .
H H10B 0.7092 0.7275 0.5042 0.034 Uiso calc U . R 1 . .
H H10C 0.6297 0.7569 0.4865 0.034 Uiso calc U . R 1 . .
C C11 0.88318(5) 0.72371(9) 0.43124(4) 0.01431(15) Uani d . . . 1 . .
C C13 0.94081(6) 0.63597(12) 0.47010(5) 0.0248(2) Uani d . . . 1 . .
H H13A 0.9451 0.556 0.4506 0.037 Uiso calc U . R 1 . .
H H13B 0.9303 0.6105 0.5017 0.037 Uiso calc U . R 1 . .
H H13C 0.9838 0.6855 0.4828 0.037 Uiso calc U . R 1 . .
C C12 0.87835(6) 0.85024(11) 0.46183(5) 0.0225(2) Uani d . . . 1 . .
H H12A 0.8406 0.9053 0.4378 0.034 Uiso calc U . R 1 . .
H H12B 0.9211 0.9001 0.4725 0.034 Uiso calc U . R 1 . .
H H12C 0.8703 0.8262 0.4947 0.034 Uiso calc U . R 1 . .
C C14 0.90162(6) 0.76539(11) 0.38276(5) 0.02051(19) Uani d . . . 1 . .
H H14A 0.9103 0.6861 0.365 0.031 Uiso calc U . R 1 . .
H H14B 0.9426 0.8211 0.3962 0.031 Uiso calc U . R 1 . .
H H14C 0.8637 0.8156 0.3562 0.031 Uiso calc U . R 1 . .
C C15 0.73417(5) 0.37031(9) 0.30649(4) 0.01135(14) Uani d . . . 1 . .
H H15A 0.6975 0.4055 0.2731 0.014 Uiso calc U . R 1 . .
H H15B 0.7761 0.3644 0.2989 0.014 Uiso calc U . R 1 . .
C C19 0.95157(6) 0.19699(13) 0.39459(5) 0.0237(2) Uani d . . . 1 . .
H H19 0.9976 0.2256 0.4109 0.028 Uiso calc U . R 1 . .
C C18 0.89506(5) 0.24826(11) 0.40518(4) 0.01967(19) Uani d . . . 1 . .
H H18 0.8963 0.318 0.4298 0.024 Uiso calc U . R 1 . .
C C17 0.83934(5) 0.17803(9) 0.37332(4) 0.01321(15) Uani d . . . 1 . .
C C16 0.76769(5) 0.17836(9) 0.36972(4) 0.01181(14) Uani d . . . 1 . .
H H16A 0.766 0.2311 0.4008 0.014 Uiso calc U . R 1 . .
H H16B 0.755 0.086 0.3745 0.014 Uiso calc U . R 1 . .
C C20 0.92628(6) 0.10006(12) 0.35691(5) 0.0225(2) Uani d . . . 1 . .
H H20 0.9525 0.049 0.342 0.027 Uiso calc U . R 1 . .
C C21 0.70851(5) 0.14745(9) 0.26869(4) 0.01155(14) Uani d . . . 1 . .
H H21A 0.68 0.1947 0.2347 0.014 Uiso calc U . R 1 . .
H H21B 0.7544 0.1357 0.2681 0.014 Uiso calc U . R 1 . .
C C22 0.67829(5) 0.01414(9) 0.26867(4) 0.01232(14) Uani d . . . 1 . .
C C23 0.61638(5) -0.03868(10) 0.23820(4) 0.01636(17) Uani d . . . 1 . .
H H23 0.5793 0.0054 0.2107 0.02 Uiso calc U . R 1 . .
C C24 0.61793(6) -0.17407(10) 0.25564(5) 0.01981(19) Uani d . . . 1 . .
H H24 0.5821 -0.2372 0.2421 0.024 Uiso calc U . R 1 . .
C C25 0.68055(6) -0.19395(10) 0.29521(4) 0.01875(18) Uani d . . . 1 . .
H H25 0.6958 -0.2752 0.3143 0.022 Uiso calc U . R 1 . .
C C26 0.55229(5) 0.28204(12) 0.25033(5) 0.02099(19) Uani d . . . 1 . .
H H26A 0.5737 0.2858 0.2236 0.031 Uiso calc U . R 1 . .
H H26B 0.5286 0.3659 0.2496 0.031 Uiso calc U . R 1 . .
H H26C 0.5195 0.2087 0.241 0.031 Uiso calc U . R 1 . .
C C27 0.61386(6) 0.11016(11) 0.37159(5) 0.0215(2) Uani d . . . 1 . .
H H27A 0.5718 0.1227 0.3778 0.032 Uiso calc U . R 1 . .
H H27B 0.653 0.112 0.4068 0.032 Uiso calc U . R 1 . .
H H27C 0.6123 0.0244 0.3537 0.032 Uiso calc U . R 1 . .
C C28 0.79281(5) 0.38414(9) 0.62376(4) 0.01204(14) Uani d . . . 1 . .
C C29 0.74438(5) 0.40514(9) 0.64707(4) 0.01089(14) Uani d . . . 1 . .
C C30 0.68423(5) 0.33145(9) 0.62953(4) 0.01208(14) Uani d . . . 1 . .
H H30 0.6517 0.3483 0.6452 0.014 Uiso calc U . R 1 . .
C C31 0.67078(5) 0.23320(9) 0.58926(4) 0.01310(15) Uani d . . . 1 . .
C C32 0.72039(5) 0.21186(9) 0.56763(4) 0.01350(15) Uani d . . . 1 . .
H H32 0.7122 0.145 0.5405 0.016 Uiso calc U . R 1 . .
C C33 0.78143(5) 0.28335(9) 0.58372(4) 0.01232(14) Uani d . . . 1 . .
C C34 0.83502(5) 0.25255(10) 0.55972(4) 0.01528(16) Uani d . . . 1 . .
C C35 0.90298(6) 0.21356(13) 0.60618(5) 0.0247(2) Uani d . . . 1 . .
H H35A 0.9366 0.1918 0.5905 0.037 Uiso calc U . R 1 . .
H H35B 0.8958 0.1361 0.6258 0.037 Uiso calc U . R 1 . .
H H35C 0.9197 0.288 0.6318 0.037 Uiso calc U . R 1 . .
C C36 0.84538(7) 0.37453(12) 0.52871(5) 0.0240(2) Uani d . . . 1 . .
H H36A 0.8822 0.3566 0.5161 0.036 Uiso calc U . R 1 . .
H H36B 0.8574 0.4515 0.5533 0.036 Uiso calc U . R 1 . .
H H36C 0.8031 0.3931 0.4971 0.036 Uiso calc U . R 1 . .
C C37 0.81351(6) 0.13561(11) 0.51922(5) 0.0226(2) Uani d . . . 1 . .
H H37A 0.77 0.1563 0.4893 0.034 Uiso calc U . R 1 . .
H H37B 0.8085 0.0555 0.5384 0.034 Uiso calc U . R 1 . .
H H37C 0.8484 0.1205 0.5042 0.034 Uiso calc U . R 1 . .
C C38 0.60306(5) 0.15713(10) 0.56863(4) 0.01640(17) Uani d . . . 1 . .
C C39 0.58332(6) 0.11799(12) 0.61668(5) 0.0247(2) Uani d . . . 1 . .
H H39A 0.5405 0.0681 0.6027 0.037 Uiso calc U . R 1 . .
H H39B 0.5776 0.1983 0.6354 0.037 Uiso calc U . R 1 . .
H H39C 0.6193 0.0626 0.6426 0.037 Uiso calc U . R 1 . .
C C40 0.54699(6) 0.24867(13) 0.52993(6) 0.0296(3) Uani d . . . 1 . .
H H40A 0.5572 0.2702 0.4978 0.044 Uiso calc U . R 1 . .
H H40B 0.5453 0.3306 0.5493 0.044 Uiso calc U . R 1 . .
H H40C 0.5029 0.2034 0.5181 0.044 Uiso calc U . R 1 . .
C C41 0.60657(7) 0.02937(14) 0.53857(7) 0.0364(3) Uani d . . . 1 . .
H H41A 0.5648 -0.0222 0.5307 0.055 Uiso calc U . R 1 . .
H H41B 0.646 -0.0232 0.5617 0.055 Uiso calc U . R 1 . .
H H41C 0.6112 0.0517 0.5041 0.055 Uiso calc U . R 1 . .
C C42 0.75923(5) 0.50284(8) 0.69382(4) 0.01091(14) Uani d . . . 1 . .
H H42A 0.7185 0.5098 0.7031 0.013 Uiso calc U . R 1 . .
H H42B 0.797 0.4677 0.7265 0.013 Uiso calc U . R 1 . .
C C43 0.72260(5) 0.69365(9) 0.63018(4) 0.01326(15) Uani d . . . 1 . .
H H43A 0.7351 0.7852 0.6241 0.016 Uiso calc U . R 1 . .
H H43B 0.7212 0.6393 0.5986 0.016 Uiso calc U . R 1 . .
C C44 0.65276(5) 0.69668(9) 0.63061(4) 0.01425(15) Uani d . . . 1 . .
C C45 0.59548(5) 0.62583(11) 0.60265(5) 0.02036(19) Uani d . . . 1 . .
H H45 0.5911 0.5556 0.5775 0.024 Uiso calc U . R 1 . .
C C46 0.54287(5) 0.67709(12) 0.61827(5) 0.0224(2) Uani d . . . 1 . .
H H46 0.4969 0.6476 0.6057 0.027 Uiso calc U . R 1 . .
C C47 0.57169(5) 0.77586(11) 0.65444(5) 0.0214(2) Uani d . . . 1 . .
H H47 0.5485 0.828 0.6717 0.026 Uiso calc U . R 1 . .
C C48 0.78854(5) 0.72638(9) 0.73052(4) 0.01164(14) Uani d . . . 1 . .
H H48A 0.7442 0.7383 0.734 0.014 Uiso calc U . R 1 . .
H H48B 0.8196 0.6803 0.764 0.014 Uiso calc U . R 1 . .
C C49 0.81736(5) 0.85948(9) 0.72760(4) 0.01249(15) Uani d . . . 1 . .
C C50 0.87999(5) 0.91352(11) 0.75479(4) 0.01792(17) Uani d . . . 1 . .
H H50 0.9187 0.8709 0.7811 0.022 Uiso calc U . R 1 . .
C C51 0.87589(6) 1.04848(11) 0.73569(5) 0.0222(2) Uani d . . . 1 . .
H H51 0.9115 1.1124 0.7469 0.027 Uiso calc U . R 1 . .
C C52 0.81173(6) 1.06631(10) 0.69884(5) 0.02051(19) Uani d . . . 1 . .
H H52 0.7948 1.1465 0.6795 0.025 Uiso calc U . R 1 . .
C C53 0.87369(8) 0.75497(14) 0.62146(6) 0.0317(3) Uani d . . . 1 . .
H H53A 0.8359 0.7446 0.5858 0.048 Uiso calc U . R 1 . .
H H53B 0.9171 0.7471 0.6169 0.048 Uiso calc U . R 1 . .
H H53C 0.8709 0.8425 0.6367 0.048 Uiso calc U . R 1 . .
C C54 0.94136(6) 0.59289(12) 0.74502(5) 0.0238(2) Uani d . . . 1 . .
H H54A 0.9728 0.5235 0.7433 0.036 Uiso calc U . R 1 . .
H H54B 0.9215 0.5671 0.7713 0.036 Uiso calc U . R 1 . .
H H54C 0.9662 0.6766 0.7567 0.036 Uiso calc U . R 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Al1 0.00940(12) 0.01334(12) 0.01256(12) -0.00061(9) 0.00328(10) -0.00112(9)
O1 0.0124(3) 0.0177(3) 0.0220(3) -0.0033(2) 0.0084(3) -0.0071(3)
N1 0.0103(3) 0.0103(3) 0.0080(3) 0.0002(2) 0.0020(2) -0.0003(2)
C1 0.0105(3) 0.0114(3) 0.0122(3) 0.0000(3) 0.0035(3) -0.0012(3)
Al2 0.01205(13) 0.01630(13) 0.01657(14) -0.00390(10) 0.00727(11) -0.00370(10)
O2 0.0135(3) 0.0180(3) 0.0229(4) 0.0027(2) 0.0068(3) -0.0028(3)
N2 0.0114(3) 0.0103(3) 0.0093(3) -0.0014(2) 0.0033(2) -0.0010(2)
C2 0.0134(4) 0.0118(3) 0.0116(3) 0.0018(3) 0.0049(3) -0.0002(3)
O3 0.0165(3) 0.0123(3) 0.0143(3) 0.0005(2) 0.0024(2) 0.0006(2)
C3 0.0152(4) 0.0119(3) 0.0108(3) 0.0002(3) 0.0039(3) -0.0012(3)
C4 0.0124(3) 0.0109(3) 0.0109(3) -0.0008(3) 0.0026(3) -0.0001(3)
O4 0.0134(3) 0.0212(3) 0.0250(4) -0.0064(3) 0.0108(3) -0.0103(3)
C5 0.0117(3) 0.0117(3) 0.0123(3) -0.0005(3) 0.0041(3) -0.0004(3)
O5 0.0133(3) 0.0169(3) 0.0234(4) 0.0003(2) 0.0054(3) -0.0040(3)
C6 0.0110(3) 0.0103(3) 0.0107(3) 0.0003(3) 0.0038(3) -0.0008(3)
O6 0.0182(3) 0.0138(3) 0.0153(3) 0.0000(2) 0.0039(3) 0.0005(2)
C7 0.0161(4) 0.0153(4) 0.0156(4) 0.0018(3) 0.0080(3) -0.0020(3)
C8 0.0172(4) 0.0264(5) 0.0239(5) 0.0079(4) 0.0074(4) -0.0005(4)
C9 0.0237(5) 0.0211(5) 0.0218(5) -0.0003(4) 0.0135(4) 0.0010(4)
C10 0.0278(5) 0.0203(5) 0.0252(5) -0.0007(4) 0.0160(4) -0.0076(4)
C11 0.0131(4) 0.0134(4) 0.0135(4) -0.0021(3) 0.0019(3) -0.0016(3)
C13 0.0164(4) 0.0213(5) 0.0251(5) -0.0016(4) -0.0048(4) 0.0028(4)
C12 0.0240(5) 0.0179(4) 0.0254(5) -0.0070(4) 0.0093(4) -0.0091(4)
C14 0.0192(4) 0.0227(5) 0.0194(4) -0.0084(4) 0.0073(4) -0.0029(4)
C15 0.0126(3) 0.0108(3) 0.0106(3) -0.0007(3) 0.0045(3) -0.0001(3)
C19 0.0110(4) 0.0336(6) 0.0239(5) -0.0002(4) 0.0039(4) 0.0021(4)
C18 0.0117(4) 0.0267(5) 0.0167(4) -0.0019(3) 0.0013(3) -0.0029(4)
C17 0.0104(3) 0.0152(4) 0.0123(4) 0.0015(3) 0.0026(3) 0.0010(3)
C16 0.0107(3) 0.0142(4) 0.0094(3) 0.0009(3) 0.0025(3) 0.0013(3)
C20 0.0133(4) 0.0279(5) 0.0275(5) 0.0047(4) 0.0092(4) 0.0031(4)
C21 0.0136(4) 0.0113(3) 0.0092(3) -0.0002(3) 0.0039(3) -0.0007(3)
C22 0.0135(4) 0.0115(3) 0.0114(3) 0.0004(3) 0.0041(3) -0.0008(3)
C23 0.0134(4) 0.0169(4) 0.0165(4) -0.0010(3) 0.0032(3) -0.0021(3)
C24 0.0206(5) 0.0167(4) 0.0229(5) -0.0058(3) 0.0093(4) -0.0043(3)
C25 0.0256(5) 0.0117(4) 0.0197(4) -0.0018(3) 0.0096(4) 0.0000(3)
C26 0.0143(4) 0.0247(5) 0.0186(4) 0.0041(4) 0.0005(3) -0.0014(4)
C27 0.0205(5) 0.0222(5) 0.0248(5) -0.0005(4) 0.0120(4) 0.0040(4)
C28 0.0111(3) 0.0129(4) 0.0120(3) -0.0012(3) 0.0043(3) -0.0023(3)
C29 0.0110(3) 0.0103(3) 0.0109(3) -0.0012(3) 0.0037(3) -0.0017(3)
C30 0.0112(3) 0.0119(3) 0.0124(3) -0.0016(3) 0.0038(3) -0.0014(3)
C31 0.0124(4) 0.0118(3) 0.0124(4) -0.0017(3) 0.0020(3) -0.0018(3)
C32 0.0148(4) 0.0125(4) 0.0112(3) -0.0004(3) 0.0029(3) -0.0023(3)
C33 0.0130(4) 0.0129(3) 0.0109(3) 0.0008(3) 0.0044(3) -0.0011(3)
C34 0.0171(4) 0.0169(4) 0.0134(4) 0.0022(3) 0.0078(3) -0.0020(3)
C35 0.0174(5) 0.0347(6) 0.0217(5) 0.0081(4) 0.0072(4) -0.0023(4)
C36 0.0319(6) 0.0226(5) 0.0248(5) -0.0004(4) 0.0189(5) 0.0004(4)
C37 0.0295(5) 0.0223(5) 0.0199(5) 0.0008(4) 0.0139(4) -0.0067(4)
C38 0.0136(4) 0.0150(4) 0.0170(4) -0.0035(3) 0.0020(3) -0.0028(3)
C39 0.0229(5) 0.0238(5) 0.0249(5) -0.0104(4) 0.0066(4) 0.0008(4)
C40 0.0173(5) 0.0302(6) 0.0289(6) -0.0060(4) -0.0045(4) 0.0087(5)
C41 0.0290(6) 0.0302(6) 0.0517(9) -0.0152(5) 0.0176(6) -0.0265(6)
C42 0.0126(3) 0.0101(3) 0.0105(3) -0.0016(3) 0.0050(3) -0.0011(3)
C43 0.0146(4) 0.0138(4) 0.0095(3) -0.0001(3) 0.0026(3) 0.0012(3)
C44 0.0129(4) 0.0129(4) 0.0135(4) 0.0008(3) 0.0014(3) 0.0006(3)
C45 0.0146(4) 0.0204(4) 0.0192(4) -0.0014(3) -0.0010(3) -0.0023(3)
C46 0.0119(4) 0.0237(5) 0.0253(5) -0.0003(3) 0.0002(4) 0.0036(4)
C47 0.0126(4) 0.0224(5) 0.0278(5) 0.0029(3) 0.0064(4) 0.0026(4)
C48 0.0132(4) 0.0112(3) 0.0102(3) -0.0014(3) 0.0042(3) -0.0018(3)
C49 0.0134(4) 0.0111(3) 0.0129(4) -0.0011(3) 0.0050(3) -0.0015(3)
C50 0.0131(4) 0.0201(4) 0.0189(4) -0.0028(3) 0.0043(3) -0.0042(3)
C51 0.0245(5) 0.0195(4) 0.0260(5) -0.0097(4) 0.0135(4) -0.0063(4)
C52 0.0308(5) 0.0121(4) 0.0206(5) -0.0038(4) 0.0121(4) 0.0000(3)
C53 0.0353(7) 0.0327(6) 0.0372(7) -0.0050(5) 0.0253(6) 0.0043(5)
C54 0.0134(4) 0.0288(5) 0.0251(5) 0.0029(4) 0.0031(4) -0.0075(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Al1 O1 . 1.7640(10) ?
Al1 C27 . 1.9661(13) ?
Al1 C26 . 1.9729(14) ?
Al1 N1 . 2.0446(12) ?
O1 C1 . 1.3410(12) ?
N1 C15 . 1.5066(13) ?
N1 C21 . 1.5076(13) ?
N1 C16 . 1.5098(13) ?
C1 C6 . 1.4082(13) ?
C1 C2 . 1.4197(13) ?
Al2 O4 . 1.7609(10) ?
Al2 C53 . 1.9666(15) ?
Al2 C54 . 1.9734(15) ?
Al2 N2 . 2.0405(12) ?
O2 C20 . 1.3731(15) ?
O2 C17 . 1.3785(12) ?
N2 C42 . 1.5077(13) ?
N2 C48 . 1.5078(13) ?
N2 C43 . 1.5121(13) ?
C2 C3 . 1.4035(14) ?
C2 C7 . 1.5362(14) ?
O3 C25 . 1.3731(13) ?
O3 C22 . 1.3762(12) ?
C3 C4 . 1.4004(14) ?
C3 H3 . 0.95 ?
C4 C5 . 1.3969(13) ?
C4 C11 . 1.5334(14) ?
O4 C28 . 1.3409(12) ?
C5 C6 . 1.3979(13) ?
C5 H5 . 0.95 ?
O5 C47 . 1.3709(14) ?
O5 C44 . 1.3774(13) ?
C6 C15 . 1.5122(13) ?
O6 C52 . 1.3721(13) ?
O6 C49 . 1.3751(12) ?
C7 C9 . 1.5386(15) ?
C7 C10 . 1.5389(15) ?
C7 C8 . 1.5485(16) ?
C8 H8A . 0.98 ?
C8 H8B . 0.98 ?
C8 H8C . 0.98 ?
C9 H9A . 0.98 ?
C9 H9B . 0.98 ?
C9 H9C . 0.98 ?
C10 H10A . 0.98 ?
C10 H10B . 0.98 ?
C10 H10C . 0.98 ?
C11 C12 . 1.5339(15) ?
C11 C14 . 1.5373(16) ?
C11 C13 . 1.5377(15) ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C14 H14A . 0.98 ?
C14 H14B . 0.98 ?
C14 H14C . 0.98 ?
C15 H15A . 0.99 ?
C15 H15B . 0.99 ?
C19 C20 . 1.3488(18) ?
C19 C18 . 1.4332(17) ?
C19 H19 . 0.95 ?
C18 C17 . 1.3573(14) ?
C18 H18 . 0.95 ?
C17 C16 . 1.4909(15) ?
C16 H16A . 0.99 ?
C16 H16B . 0.99 ?
C20 H20 . 0.95 ?
C21 C22 . 1.4887(14) ?
C21 H21A . 0.99 ?
C21 H21B . 0.99 ?
C22 C23 . 1.3586(14) ?
C23 C24 . 1.4356(16) ?
C23 H23 . 0.95 ?
C24 C25 . 1.3529(17) ?
C24 H24 . 0.95 ?
C25 H25 . 0.95 ?
C26 H26A . 0.98 ?
C26 H26B . 0.98 ?
C26 H26C . 0.98 ?
C27 H27A . 0.98 ?
C27 H27B . 0.98 ?
C27 H27C . 0.98 ?
C28 C29 . 1.4072(13) ?
C28 C33 . 1.4181(13) ?
C29 C30 . 1.3946(13) ?
C29 C42 . 1.5144(13) ?
C30 C31 . 1.3993(13) ?
C30 H30 . 0.95 ?
C31 C32 . 1.3989(14) ?
C31 C38 . 1.5339(15) ?
C32 C33 . 1.3997(14) ?
C32 H32 . 0.95 ?
C33 C34 . 1.5367(15) ?
C34 C37 . 1.5374(15) ?
C34 C36 . 1.5396(16) ?
C34 C35 . 1.5422(16) ?
C35 H35A . 0.98 ?
C35 H35B . 0.98 ?
C35 H35C . 0.98 ?
C36 H36A . 0.98 ?
C36 H36B . 0.98 ?
C36 H36C . 0.98 ?
C37 H37A . 0.98 ?
C37 H37B . 0.98 ?
C37 H37C . 0.98 ?
C38 C41 . 1.5293(17) ?
C38 C39 . 1.5362(17) ?
C38 C40 . 1.5410(17) ?
C39 H39A . 0.98 ?
C39 H39B . 0.98 ?
C39 H39C . 0.98 ?
C40 H40A . 0.98 ?
C40 H40B . 0.98 ?
C40 H40C . 0.98 ?
C41 H41A . 0.98 ?
C41 H41B . 0.98 ?
C41 H41C . 0.98 ?
C42 H42A . 0.99 ?
C42 H42B . 0.99 ?
C43 C44 . 1.4914(15) ?
C43 H43A . 0.99 ?
C43 H43B . 0.99 ?
C44 C45 . 1.3578(14) ?
C45 C46 . 1.4318(17) ?
C45 H45 . 0.95 ?
C46 C47 . 1.3512(17) ?
C46 H46 . 0.95 ?
C47 H47 . 0.95 ?
C48 C49 . 1.4885(14) ?
C48 H48A . 0.99 ?
C48 H48B . 0.99 ?
C49 C50 . 1.3592(14) ?
C50 C51 . 1.4408(17) ?
C50 H50 . 0.95 ?
C51 C52 . 1.3472(18) ?
C51 H51 . 0.95 ?
C52 H52 . 0.95 ?
C53 H53A . 0.98 ?
C53 H53B . 0.98 ?
C53 H53C . 0.98 ?
C54 H54A . 0.98 ?
C54 H54B . 0.98 ?
C54 H54C . 0.98 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Al1 C27 . . 112.16(6) ?
O1 Al1 C26 . . 108.26(5) ?
C27 Al1 C26 . . 120.84(6) ?
O1 Al1 N1 . . 96.16(4) ?
C27 Al1 N1 . . 108.35(4) ?
C26 Al1 N1 . . 108.18(5) ?
C1 O1 Al1 . . 132.85(6) ?
C15 N1 C21 . . 107.54(7) ?
C15 N1 C16 . . 110.16(7) ?
C21 N1 C16 . . 111.36(7) ?
C15 N1 Al1 . . 105.40(6) ?
C21 N1 Al1 . . 111.45(6) ?
C16 N1 Al1 . . 110.72(6) ?
O1 C1 C6 . . 119.43(8) ?
O1 C1 C2 . . 121.14(8) ?
C6 C1 C2 . . 119.43(8) ?
O4 Al2 C53 . . 112.56(6) ?
O4 Al2 C54 . . 107.70(5) ?
C53 Al2 C54 . . 121.03(7) ?
O4 Al2 N2 . . 96.47(4) ?
C53 Al2 N2 . . 107.88(5) ?
C54 Al2 N2 . . 108.33(5) ?
C20 O2 C17 . . 106.38(9) ?
C42 N2 C48 . . 107.71(7) ?
C42 N2 C43 . . 109.95(7) ?
C48 N2 C43 . . 111.48(8) ?
C42 N2 Al2 . . 105.24(6) ?
C48 N2 Al2 . . 110.10(6) ?
C43 N2 Al2 . . 112.10(6) ?
C3 C2 C1 . . 117.81(8) ?
C3 C2 C7 . . 121.33(9) ?
C1 C2 C7 . . 120.85(8) ?
C25 O3 C22 . . 106.63(8) ?
C4 C3 C2 . . 123.65(9) ?
C4 C3 H3 . . 118.2 ?
C2 C3 H3 . . 118.2 ?
C5 C4 C3 . . 116.97(8) ?
C5 C4 C11 . . 120.40(8) ?
C3 C4 C11 . . 122.62(9) ?
C28 O4 Al2 . . 131.95(7) ?
C4 C5 C6 . . 121.71(9) ?
C4 C5 H5 . . 119.1 ?
C6 C5 H5 . . 119.1 ?
C47 O5 C44 . . 106.60(8) ?
C5 C6 C1 . . 120.31(8) ?
C5 C6 C15 . . 119.21(8) ?
C1 C6 C15 . . 120.34(8) ?
C52 O6 C49 . . 106.75(9) ?
C2 C7 C9 . . 110.07(8) ?
C2 C7 C10 . . 112.31(9) ?
C9 C7 C10 . . 107.59(9) ?
C2 C7 C8 . . 109.73(9) ?
C9 C7 C8 . . 110.16(9) ?
C10 C7 C8 . . 106.92(9) ?
C7 C8 H8A . . 109.5 ?
C7 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C7 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
C7 C9 H9A . . 109.5 ?
C7 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C7 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C7 C10 H10A . . 109.5 ?
C7 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C7 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C4 C11 C12 . . 112.35(9) ?
C4 C11 C14 . . 110.18(8) ?
C12 C11 C14 . . 107.68(9) ?
C4 C11 C13 . . 109.05(9) ?
C12 C11 C13 . . 108.92(9) ?
C14 C11 C13 . . 108.58(10) ?
C11 C13 H13A . . 109.5 ?
C11 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C11 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C11 C12 H12A . . 109.5 ?
C11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C11 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C11 C14 H14A . . 109.5 ?
C11 C14 H14B . . 109.5 ?
H14A C14 H14B . . 109.5 ?
C11 C14 H14C . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
N1 C15 C6 . . 114.49(8) ?
N1 C15 H15A . . 108.6 ?
C6 C15 H15A . . 108.6 ?
N1 C15 H15B . . 108.6 ?
C6 C15 H15B . . 108.6 ?
H15A C15 H15B . . 107.6 ?
C20 C19 C18 . . 106.27(10) ?
C20 C19 H19 . . 126.9 ?
C18 C19 H19 . . 126.9 ?
C17 C18 C19 . . 106.78(10) ?
C17 C18 H18 . . 126.6 ?
C19 C18 H18 . . 126.6 ?
C18 C17 O2 . . 109.82(9) ?
C18 C17 C16 . . 131.65(9) ?
O2 C17 C16 . . 118.32(8) ?
C17 C16 N1 . . 116.18(8) ?
C17 C16 H16A . . 108.2 ?
N1 C16 H16A . . 108.2 ?
C17 C16 H16B . . 108.2 ?
N1 C16 H16B . . 108.2 ?
H16A C16 H16B . . 107.4 ?
C19 C20 O2 . . 110.75(10) ?
C19 C20 H20 . . 124.6 ?
O2 C20 H20 . . 124.6 ?
C22 C21 N1 . . 114.08(8) ?
C22 C21 H21A . . 108.7 ?
N1 C21 H21A . . 108.7 ?
C22 C21 H21B . . 108.7 ?
N1 C21 H21B . . 108.7 ?
H21A C21 H21B . . 107.6 ?
C23 C22 O3 . . 109.96(9) ?
C23 C22 C21 . . 132.31(9) ?
O3 C22 C21 . . 117.69(8) ?
C22 C23 C24 . . 106.57(9) ?
C22 C23 H23 . . 126.7 ?
C24 C23 H23 . . 126.7 ?
C25 C24 C23 . . 106.38(9) ?
C25 C24 H24 . . 126.8 ?
C23 C24 H24 . . 126.8 ?
C24 C25 O3 . . 110.46(9) ?
C24 C25 H25 . . 124.8 ?
O3 C25 H25 . . 124.8 ?
Al1 C26 H26A . . 109.5 ?
Al1 C26 H26B . . 109.5 ?
H26A C26 H26B . . 109.5 ?
Al1 C26 H26C . . 109.5 ?
H26A C26 H26C . . 109.5 ?
H26B C26 H26C . . 109.5 ?
Al1 C27 H27A . . 109.5 ?
Al1 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
Al1 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 109.5 ?
O4 C28 C29 . . 119.31(8) ?
O4 C28 C33 . . 121.18(8) ?
C29 C28 C33 . . 119.50(8) ?
C30 C29 C28 . . 120.56(8) ?
C30 C29 C42 . . 119.44(8) ?
C28 C29 C42 . . 119.91(8) ?
C29 C30 C31 . . 121.33(9) ?
C29 C30 H30 . . 119.3 ?
C31 C30 H30 . . 119.3 ?
C32 C31 C30 . . 117.10(9) ?
C32 C31 C38 . . 122.16(9) ?
C30 C31 C38 . . 120.70(9) ?
C31 C32 C33 . . 123.76(9) ?
C31 C32 H32 . . 118.1 ?
C33 C32 H32 . . 118.1 ?
C32 C33 C28 . . 117.70(8) ?
C32 C33 C34 . . 121.40(9) ?
C28 C33 C34 . . 120.89(8) ?
C33 C34 C37 . . 111.96(9) ?
C33 C34 C36 . . 109.96(8) ?
C37 C34 C36 . . 107.80(9) ?
C33 C34 C35 . . 109.88(9) ?
C37 C34 C35 . . 107.09(9) ?
C36 C34 C35 . . 110.09(10) ?
C34 C35 H35A . . 109.5 ?
C34 C35 H35B . . 109.5 ?
H35A C35 H35B . . 109.5 ?
C34 C35 H35C . . 109.5 ?
H35A C35 H35C . . 109.5 ?
H35B C35 H35C . . 109.5 ?
C34 C36 H36A . . 109.5 ?
C34 C36 H36B . . 109.5 ?
H36A C36 H36B . . 109.5 ?
C34 C36 H36C . . 109.5 ?
H36A C36 H36C . . 109.5 ?
H36B C36 H36C . . 109.5 ?
C34 C37 H37A . . 109.5 ?
C34 C37 H37B . . 109.5 ?
H37A C37 H37B . . 109.5 ?
C34 C37 H37C . . 109.5 ?
H37A C37 H37C . . 109.5 ?
H37B C37 H37C . . 109.5 ?
C41 C38 C31 . . 112.12(9) ?
C41 C38 C39 . . 107.33(10) ?
C31 C38 C39 . . 110.78(9) ?
C41 C38 C40 . . 109.85(11) ?
C31 C38 C40 . . 108.45(9) ?
C39 C38 C40 . . 108.23(10) ?
C38 C39 H39A . . 109.5 ?
C38 C39 H39B . . 109.5 ?
H39A C39 H39B . . 109.5 ?
C38 C39 H39C . . 109.5 ?
H39A C39 H39C . . 109.5 ?
H39B C39 H39C . . 109.5 ?
C38 C40 H40A . . 109.5 ?
C38 C40 H40B . . 109.5 ?
H40A C40 H40B . . 109.5 ?
C38 C40 H40C . . 109.5 ?
H40A C40 H40C . . 109.5 ?
H40B C40 H40C . . 109.5 ?
C38 C41 H41A . . 109.5 ?
C38 C41 H41B . . 109.5 ?
H41A C41 H41B . . 109.5 ?
C38 C41 H41C . . 109.5 ?
H41A C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
N2 C42 C29 . . 113.91(8) ?
N2 C42 H42A . . 108.8 ?
C29 C42 H42A . . 108.8 ?
N2 C42 H42B . . 108.8 ?
C29 C42 H42B . . 108.8 ?
H42A C42 H42B . . 107.7 ?
C44 C43 N2 . . 115.87(8) ?
C44 C43 H43A . . 108.3 ?
N2 C43 H43A . . 108.3 ?
C44 C43 H43B . . 108.3 ?
N2 C43 H43B . . 108.3 ?
H43A C43 H43B . . 107.4 ?
C45 C44 O5 . . 109.63(9) ?
C45 C44 C43 . . 132.26(10) ?
O5 C44 C43 . . 118.04(8) ?
C44 C45 C46 . . 106.93(10) ?
C44 C45 H45 . . 126.5 ?
C46 C45 H45 . . 126.5 ?
C47 C46 C45 . . 106.16(10) ?
C47 C46 H46 . . 126.9 ?
C45 C46 H46 . . 126.9 ?
C46 C47 O5 . . 110.67(10) ?
C46 C47 H47 . . 124.7 ?
O5 C47 H47 . . 124.7 ?
C49 C48 N2 . . 113.73(8) ?
C49 C48 H48A . . 108.8 ?
N2 C48 H48A . . 108.8 ?
C49 C48 H48B . . 108.8 ?
N2 C48 H48B . . 108.8 ?
H48A C48 H48B . . 107.7 ?
C50 C49 O6 . . 110.02(9) ?
C50 C49 C48 . . 132.27(9) ?
O6 C49 C48 . . 117.65(8) ?
C49 C50 C51 . . 106.18(10) ?
C49 C50 H50 . . 126.9 ?
C51 C50 H50 . . 126.9 ?
C52 C51 C50 . . 106.61(9) ?
C52 C51 H51 . . 126.7 ?
C50 C51 H51 . . 126.7 ?
C51 C52 O6 . . 110.43(10) ?
C51 C52 H52 . . 124.8 ?
O6 C52 H52 . . 124.8 ?
Al2 C53 H53A . . 109.5 ?
Al2 C53 H53B . . 109.5 ?
H53A C53 H53B . . 109.5 ?
Al2 C53 H53C . . 109.5 ?
H53A C53 H53C . . 109.5 ?
H53B C53 H53C . . 109.5 ?
Al2 C54 H54A . . 109.5 ?
Al2 C54 H54B . . 109.5 ?
H54A C54 H54B . . 109.5 ?
Al2 C54 H54C . . 109.5 ?
H54A C54 H54C . . 109.5 ?
H54B C54 H54C . . 109.5 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C27 Al1 O1 C1 . . . . 113.01(10) ?
C26 Al1 O1 C1 . . . . -111.17(10) ?
N1 Al1 O1 C1 . . . . 0.30(10) ?
Al1 O1 C1 C6 . . . . 15.95(14) ?
Al1 O1 C1 C2 . . . . -164.67(7) ?
O1 C1 C2 C3 . . . . 177.25(8) ?
C6 C1 C2 C3 . . . . -3.38(13) ?
O1 C1 C2 C7 . . . . -3.55(13) ?
C6 C1 C2 C7 . . . . 175.82(8) ?
C1 C2 C3 C4 . . . . 0.61(14) ?
C7 C2 C3 C4 . . . . -178.58(9) ?
C2 C3 C4 C5 . . . . 1.52(14) ?
C2 C3 C4 C11 . . . . -177.46(9) ?
C53 Al2 O4 C28 . . . . -107.10(10) ?
C54 Al2 O4 C28 . . . . 116.97(10) ?
N2 Al2 O4 C28 . . . . 5.35(10) ?
C3 C4 C5 C6 . . . . -0.90(13) ?
C11 C4 C5 C6 . . . . 178.11(8) ?
C4 C5 C6 C1 . . . . -1.86(14) ?
C4 C5 C6 C15 . . . . 173.92(8) ?
O1 C1 C6 C5 . . . . -176.58(8) ?
C2 C1 C6 C5 . . . . 4.03(13) ?
O1 C1 C6 C15 . . . . 7.69(13) ?
C2 C1 C6 C15 . . . . -171.70(8) ?
C3 C2 C7 C9 . . . . -116.81(10) ?
C1 C2 C7 C9 . . . . 64.01(12) ?
C3 C2 C7 C10 . . . . 3.03(13) ?
C1 C2 C7 C10 . . . . -176.14(9) ?
C3 C2 C7 C8 . . . . 121.80(10) ?
C1 C2 C7 C8 . . . . -57.38(12) ?
C5 C4 C11 C12 . . . . 165.07(9) ?
C3 C4 C11 C12 . . . . -15.98(13) ?
C5 C4 C11 C14 . . . . 45.00(12) ?
C3 C4 C11 C14 . . . . -136.05(10) ?
C5 C4 C11 C13 . . . . -74.07(12) ?
C3 C4 C11 C13 . . . . 104.87(11) ?
C21 N1 C15 C6 . . . . -176.87(7) ?
C16 N1 C15 C6 . . . . -55.35(10) ?
Al1 N1 C15 C6 . . . . 64.13(8) ?
C5 C6 C15 N1 . . . . 130.75(9) ?
C1 C6 C15 N1 . . . . -53.48(11) ?
C20 C19 C18 C17 . . . . 0.36(13) ?
C19 C18 C17 O2 . . . . -0.13(12) ?
C19 C18 C17 C16 . . . . 174.45(10) ?
C20 O2 C17 C18 . . . . -0.16(12) ?
C20 O2 C17 C16 . . . . -175.55(9) ?
C18 C17 C16 N1 . . . . 111.92(12) ?
O2 C17 C16 N1 . . . . -73.88(11) ?
C15 N1 C16 C17 . . . . -54.62(10) ?
C21 N1 C16 C17 . . . . 64.60(10) ?
Al1 N1 C16 C17 . . . . -170.82(6) ?
C18 C19 C20 O2 . . . . -0.47(14) ?
C17 O2 C20 C19 . . . . 0.40(13) ?
C15 N1 C21 C22 . . . . -170.28(7) ?
C16 N1 C21 C22 . . . . 68.95(10) ?
Al1 N1 C21 C22 . . . . -55.23(9) ?
C25 O3 C22 C23 . . . . -0.68(11) ?
C25 O3 C22 C21 . . . . -178.44(8) ?
N1 C21 C22 C23 . . . . 107.00(12) ?
N1 C21 C22 O3 . . . . -75.84(11) ?
O3 C22 C23 C24 . . . . 0.53(11) ?
C21 C22 C23 C24 . . . . 177.86(10) ?
C22 C23 C24 C25 . . . . -0.18(12) ?
C23 C24 C25 O3 . . . . -0.24(12) ?
C22 O3 C25 C24 . . . . 0.56(12) ?
Al2 O4 C28 C29 . . . . -22.60(14) ?
Al2 O4 C28 C33 . . . . 158.39(8) ?
O4 C28 C29 C30 . . . . 178.36(9) ?
C33 C28 C29 C30 . . . . -2.60(13) ?
O4 C28 C29 C42 . . . . -5.14(13) ?
C33 C28 C29 C42 . . . . 173.89(8) ?
C28 C29 C30 C31 . . . . 1.27(14) ?
C42 C29 C30 C31 . . . . -175.24(8) ?
C29 C30 C31 C32 . . . . 0.28(14) ?
C29 C30 C31 C38 . . . . -177.35(9) ?
C30 C31 C32 C33 . . . . -0.49(14) ?
C38 C31 C32 C33 . . . . 177.11(9) ?
C31 C32 C33 C28 . . . . -0.82(14) ?
C31 C32 C33 C34 . . . . 178.13(9) ?
O4 C28 C33 C32 . . . . -178.64(9) ?
C29 C28 C33 C32 . . . . 2.34(13) ?
O4 C28 C33 C34 . . . . 2.40(14) ?
C29 C28 C33 C34 . . . . -176.61(8) ?
C32 C33 C34 C37 . . . . -1.66(13) ?
C28 C33 C34 C37 . . . . 177.26(9) ?
C32 C33 C34 C36 . . . . 118.16(11) ?
C28 C33 C34 C36 . . . . -62.92(12) ?
C32 C33 C34 C35 . . . . -120.52(11) ?
C28 C33 C34 C35 . . . . 58.40(12) ?
C32 C31 C38 C41 . . . . 19.61(14) ?
C30 C31 C38 C41 . . . . -162.88(11) ?
C32 C31 C38 C39 . . . . 139.49(10) ?
C30 C31 C38 C39 . . . . -43.00(13) ?
C32 C31 C38 C40 . . . . -101.87(12) ?
C30 C31 C38 C40 . . . . 75.65(13) ?
C48 N2 C42 C29 . . . . 177.74(7) ?
C43 N2 C42 C29 . . . . 56.09(10) ?
Al2 N2 C42 C29 . . . . -64.82(8) ?
C30 C29 C42 N2 . . . . -129.22(9) ?
C28 C29 C42 N2 . . . . 54.25(11) ?
C42 N2 C43 C44 . . . . 55.17(10) ?
C48 N2 C43 C44 . . . . -64.21(10) ?
Al2 N2 C43 C44 . . . . 171.85(6) ?
C47 O5 C44 C45 . . . . 0.32(12) ?
C47 O5 C44 C43 . . . . 177.75(9) ?
N2 C43 C44 C45 . . . . -110.30(13) ?
N2 C43 C44 O5 . . . . 72.96(11) ?
O5 C44 C45 C46 . . . . -0.35(12) ?
C43 C44 C45 C46 . . . . -177.29(10) ?
C44 C45 C46 C47 . . . . 0.25(13) ?
C45 C46 C47 O5 . . . . -0.06(13) ?
C44 O5 C47 C46 . . . . -0.15(12) ?
C42 N2 C48 C49 . . . . 171.53(7) ?
C43 N2 C48 C49 . . . . -67.77(10) ?
Al2 N2 C48 C49 . . . . 57.28(9) ?
C52 O6 C49 C50 . . . . 0.82(11) ?
C52 O6 C49 C48 . . . . 178.33(8) ?
N2 C48 C49 C50 . . . . -107.42(12) ?
N2 C48 C49 O6 . . . . 75.74(11) ?
O6 C49 C50 C51 . . . . -0.62(11) ?
C48 C49 C50 C51 . . . . -177.64(10) ?
C49 C50 C51 C52 . . . . 0.17(12) ?
C50 C51 C52 O6 . . . . 0.33(13) ?
C49 O6 C52 C51 . . . . -0.71(12) ?
_shelx_res_file
;
P21n.res created by SHELXL-2014/7
TITL P21n_a.res in P2(1)/n
REM Old TITL P21n in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.132, Rweak 0.005, Alpha 0.032, Orientation as input
REM Formula found by SHELXT: C54 N2 O6 Al2
CELL 0.71073 21.2880 10.0714 26.4396 90.000 112.811 90.000
ZERR 4.000 0.0096 0.0045 0.0134 0.000 0.018 0.000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC C H N O AL
UNIT 216 304 8 24 8
TEMP -173.160
SIZE 0.065 0.212 0.365
L.S. 10
BOND $H
LIST 4
ACTA
CONF
FMAP 2
PLAN 20
WGHT 0.078200 0.952300
FVAR 0.20746
AL1 5 0.622907 0.253459 0.324362 11.00000 0.00940 0.01334 =
0.01256 -0.00112 0.00328 -0.00061
O1 4 0.641336 0.407678 0.358632 11.00000 0.01240 0.01772 =
0.02203 -0.00712 0.00840 -0.00329
N1 3 0.714698 0.232575 0.317301 11.00000 0.01032 0.01033 =
0.00798 -0.00026 0.00204 0.00016
C1 1 0.696273 0.486831 0.374807 11.00000 0.01050 0.01137 =
0.01219 -0.00120 0.00348 0.00004
AL2 5 0.868077 0.616005 0.671788 11.00000 0.01205 0.01630 =
0.01657 -0.00370 0.00727 -0.00390
O2 4 0.857481 0.085332 0.343061 11.00000 0.01352 0.01805 =
0.02286 -0.00284 0.00679 0.00269
N2 3 0.778155 0.639726 0.681410 11.00000 0.01138 0.01029 =
0.00933 -0.00101 0.00326 -0.00143
C2 1 0.704565 0.590630 0.413201 11.00000 0.01343 0.01182 =
0.01163 -0.00025 0.00488 0.00183
O3 4 0.718908 -0.080254 0.303880 11.00000 0.01654 0.01228 =
0.01432 0.00062 0.00236 0.00053
C3 1 0.764817 0.665523 0.429958 11.00000 0.01515 0.01187 =
0.01075 -0.00122 0.00391 0.00016
AFIX 43
H3 2 0.770843 0.734537 0.455921 11.00000 -1.20000
AFIX 0
C4 1 0.816548 0.644182 0.410538 11.00000 0.01236 0.01086 =
0.01091 -0.00013 0.00259 -0.00078
O4 4 0.849418 0.458659 0.640436 11.00000 0.01341 0.02121 =
0.02496 -0.01027 0.01081 -0.00641
C5 1 0.805626 0.544243 0.371404 11.00000 0.01171 0.01171 =
0.01230 -0.00036 0.00415 -0.00047
AFIX 43
H5 2 0.839412 0.528014 0.356970 11.00000 -1.20000
AFIX 0
O5 4 0.639021 0.790509 0.662825 11.00000 0.01326 0.01692 =
0.02336 -0.00404 0.00545 0.00031
C6 1 0.746274 0.467491 0.352929 11.00000 0.01103 0.01029 =
0.01069 -0.00081 0.00375 0.00031
O6 4 0.774367 0.952266 0.693269 11.00000 0.01816 0.01383 =
0.01529 0.00052 0.00385 -0.00001
C7 1 0.648817 0.620699 0.434949 11.00000 0.01614 0.01525 =
0.01556 -0.00202 0.00797 0.00185
C8 1 0.580888 0.651581 0.386362 11.00000 0.01717 0.02640 =
0.02394 -0.00049 0.00745 0.00795
AFIX 137
H8A 2 0.586797 0.729545 0.366466 11.00000 -1.50000
H8B 2 0.545331 0.669583 0.400371 11.00000 -1.50000
H8C 2 0.567545 0.575161 0.361499 11.00000 -1.50000
AFIX 0
C9 1 0.639744 0.501560 0.467916 11.00000 0.02372 0.02114 =
0.02182 0.00102 0.01354 -0.00030
AFIX 137
H9A 2 0.630362 0.421503 0.445103 11.00000 -1.50000
H9B 2 0.601561 0.518617 0.478987 11.00000 -1.50000
H9C 2 0.681531 0.488677 0.500656 11.00000 -1.50000
AFIX 0
C10 1 0.666007 0.742619 0.473001 11.00000 0.02778 0.02032 =
0.02524 -0.00755 0.01601 -0.00067
AFIX 137
H10A 2 0.670094 0.821140 0.452596 11.00000 -1.50000
H10B 2 0.709220 0.727501 0.504156 11.00000 -1.50000
H10C 2 0.629653 0.756855 0.486481 11.00000 -1.50000
AFIX 0
C11 1 0.883182 0.723710 0.431238 11.00000 0.01312 0.01335 =
0.01346 -0.00164 0.00188 -0.00211
C13 1 0.940814 0.635965 0.470103 11.00000 0.01635 0.02134 =
0.02508 0.00278 -0.00476 -0.00157
AFIX 137
H13A 2 0.945092 0.555979 0.450571 11.00000 -1.50000
H13B 2 0.930286 0.610515 0.501728 11.00000 -1.50000
H13C 2 0.983794 0.685481 0.482779 11.00000 -1.50000
AFIX 0
C12 1 0.878355 0.850236 0.461829 11.00000 0.02405 0.01794 =
0.02541 -0.00907 0.00934 -0.00704
AFIX 137
H12A 2 0.840619 0.905251 0.437789 11.00000 -1.50000
H12B 2 0.921094 0.900093 0.472526 11.00000 -1.50000
H12C 2 0.870267 0.826197 0.494716 11.00000 -1.50000
AFIX 0
C14 1 0.901622 0.765391 0.382760 11.00000 0.01922 0.02268 =
0.01942 -0.00285 0.00725 -0.00839
AFIX 137
H14A 2 0.910344 0.686052 0.365023 11.00000 -1.50000
H14B 2 0.942551 0.821124 0.396171 11.00000 -1.50000
H14C 2 0.863726 0.815567 0.356183 11.00000 -1.50000
AFIX 0
C15 1 0.734169 0.370311 0.306485 11.00000 0.01265 0.01079 =
0.01063 -0.00011 0.00453 -0.00073
AFIX 23
H15A 2 0.697520 0.405537 0.273088 11.00000 -1.20000
H15B 2 0.776137 0.364442 0.298925 11.00000 -1.20000
AFIX 0
C19 1 0.951573 0.196987 0.394586 11.00000 0.01105 0.03363 =
0.02389 0.00214 0.00395 -0.00021
AFIX 43
H19 2 0.997642 0.225555 0.410850 11.00000 -1.20000
AFIX 0
C18 1 0.895057 0.248259 0.405181 11.00000 0.01173 0.02675 =
0.01670 -0.00285 0.00131 -0.00190
AFIX 43
H18 2 0.896345 0.317970 0.429770 11.00000 -1.20000
AFIX 0
C17 1 0.839336 0.178027 0.373316 11.00000 0.01045 0.01524 =
0.01226 0.00097 0.00256 0.00152
C16 1 0.767694 0.178364 0.369724 11.00000 0.01067 0.01416 =
0.00936 0.00131 0.00252 0.00086
AFIX 23
H16A 2 0.766029 0.231109 0.400777 11.00000 -1.20000
H16B 2 0.754992 0.086047 0.374509 11.00000 -1.20000
AFIX 0
C20 1 0.926279 0.100063 0.356907 11.00000 0.01330 0.02789 =
0.02749 0.00306 0.00920 0.00472
AFIX 43
H20 2 0.952488 0.048964 0.341985 11.00000 -1.20000
AFIX 0
C21 1 0.708513 0.147448 0.268691 11.00000 0.01365 0.01133 =
0.00923 -0.00067 0.00394 -0.00022
AFIX 23
H21A 2 0.680042 0.194729 0.234681 11.00000 -1.20000
H21B 2 0.754385 0.135709 0.268079 11.00000 -1.20000
AFIX 0
C22 1 0.678291 0.014137 0.268670 11.00000 0.01346 0.01149 =
0.01140 -0.00084 0.00414 0.00040
C23 1 0.616375 -0.038679 0.238203 11.00000 0.01337 0.01694 =
0.01645 -0.00212 0.00325 -0.00099
AFIX 43
H23 2 0.579306 0.005365 0.210737 11.00000 -1.20000
AFIX 0
C24 1 0.617928 -0.174068 0.255636 11.00000 0.02057 0.01675 =
0.02289 -0.00427 0.00926 -0.00584
AFIX 43
H24 2 0.582093 -0.237183 0.242072 11.00000 -1.20000
AFIX 0
C25 1 0.680546 -0.193948 0.295212 11.00000 0.02561 0.01169 =
0.01969 -0.00004 0.00960 -0.00181
AFIX 43
H25 2 0.695827 -0.275153 0.314320 11.00000 -1.20000
AFIX 0
C26 1 0.552291 0.282040 0.250331 11.00000 0.01432 0.02466 =
0.01858 -0.00138 0.00045 0.00407
AFIX 137
H26A 2 0.573702 0.285768 0.223559 11.00000 -1.50000
H26B 2 0.528588 0.365869 0.249620 11.00000 -1.50000
H26C 2 0.519506 0.208680 0.241042 11.00000 -1.50000
AFIX 0
C27 1 0.613862 0.110157 0.371588 11.00000 0.02054 0.02221 =
0.02477 0.00397 0.01195 -0.00051
AFIX 137
H27A 2 0.571770 0.122678 0.377818 11.00000 -1.50000
H27B 2 0.652991 0.112011 0.406824 11.00000 -1.50000
H27C 2 0.612318 0.024354 0.353662 11.00000 -1.50000
AFIX 0
C28 1 0.792805 0.384139 0.623756 11.00000 0.01108 0.01293 =
0.01200 -0.00228 0.00435 -0.00115
C29 1 0.744376 0.405137 0.647068 11.00000 0.01100 0.01032 =
0.01087 -0.00172 0.00370 -0.00117
C30 1 0.684229 0.331446 0.629527 11.00000 0.01121 0.01193 =
0.01242 -0.00137 0.00385 -0.00158
AFIX 43
H30 2 0.651731 0.348290 0.645230 11.00000 -1.20000
AFIX 0
C31 1 0.670783 0.233198 0.589265 11.00000 0.01244 0.01184 =
0.01244 -0.00182 0.00199 -0.00172
C32 1 0.720392 0.211855 0.567633 11.00000 0.01485 0.01249 =
0.01120 -0.00228 0.00289 -0.00039
AFIX 43
H32 2 0.712185 0.144998 0.540468 11.00000 -1.20000
AFIX 0
C33 1 0.781427 0.283352 0.583717 11.00000 0.01304 0.01285 =
0.01086 -0.00112 0.00440 0.00084
C34 1 0.835016 0.252554 0.559723 11.00000 0.01714 0.01694 =
0.01344 -0.00200 0.00776 0.00222
C35 1 0.902983 0.213560 0.606182 11.00000 0.01736 0.03472 =
0.02167 -0.00231 0.00718 0.00809
AFIX 137
H35A 2 0.936574 0.191803 0.590521 11.00000 -1.50000
H35B 2 0.895828 0.136114 0.625751 11.00000 -1.50000
H35C 2 0.919736 0.287986 0.631796 11.00000 -1.50000
AFIX 0
C36 1 0.845380 0.374525 0.528711 11.00000 0.03189 0.02263 =
0.02479 0.00037 0.01891 -0.00041
AFIX 137
H36A 2 0.882154 0.356614 0.516057 11.00000 -1.50000
H36B 2 0.857443 0.451547 0.553283 11.00000 -1.50000
H36C 2 0.803141 0.393053 0.497052 11.00000 -1.50000
AFIX 0
C37 1 0.813512 0.135611 0.519218 11.00000 0.02951 0.02231 =
0.01989 -0.00666 0.01392 0.00082
AFIX 137
H37A 2 0.769971 0.156254 0.489263 11.00000 -1.50000
H37B 2 0.808469 0.055530 0.538363 11.00000 -1.50000
H37C 2 0.848389 0.120503 0.504206 11.00000 -1.50000
AFIX 0
C38 1 0.603065 0.157129 0.568633 11.00000 0.01361 0.01496 =
0.01700 -0.00285 0.00195 -0.00349
C39 1 0.583324 0.117993 0.616681 11.00000 0.02292 0.02380 =
0.02489 0.00083 0.00658 -0.01036
AFIX 137
H39A 2 0.540451 0.068112 0.602715 11.00000 -1.50000
H39B 2 0.577602 0.198283 0.635399 11.00000 -1.50000
H39C 2 0.619325 0.062618 0.642581 11.00000 -1.50000
AFIX 0
C40 1 0.546994 0.248669 0.529929 11.00000 0.01734 0.03020 =
0.02893 0.00874 -0.00450 -0.00599
AFIX 137
H40A 2 0.557198 0.270197 0.497769 11.00000 -1.50000
H40B 2 0.545256 0.330648 0.549312 11.00000 -1.50000
H40C 2 0.502870 0.203375 0.518092 11.00000 -1.50000
AFIX 0
C41 1 0.606567 0.029367 0.538575 11.00000 0.02899 0.03019 =
0.05168 -0.02650 0.01758 -0.01518
AFIX 137
H41A 2 0.564794 -0.022208 0.530699 11.00000 -1.50000
H41B 2 0.645993 -0.023214 0.561674 11.00000 -1.50000
H41C 2 0.611160 0.051653 0.504089 11.00000 -1.50000
AFIX 0
C42 1 0.759232 0.502838 0.693823 11.00000 0.01264 0.01012 =
0.01048 -0.00112 0.00503 -0.00156
AFIX 23
H42A 2 0.718507 0.509849 0.703050 11.00000 -1.20000
H42B 2 0.797020 0.467672 0.726501 11.00000 -1.20000
AFIX 0
C43 1 0.722596 0.693655 0.630179 11.00000 0.01462 0.01379 =
0.00949 0.00123 0.00261 -0.00006
AFIX 23
H43A 2 0.735104 0.785179 0.624064 11.00000 -1.20000
H43B 2 0.721216 0.639260 0.598576 11.00000 -1.20000
AFIX 0
C44 1 0.652763 0.696677 0.630611 11.00000 0.01292 0.01295 =
0.01349 0.00058 0.00140 0.00082
C45 1 0.595479 0.625829 0.602648 11.00000 0.01464 0.02036 =
0.01921 -0.00229 -0.00097 -0.00142
AFIX 43
H45 2 0.591136 0.555628 0.577510 11.00000 -1.20000
AFIX 0
C46 1 0.542868 0.677088 0.618268 11.00000 0.01187 0.02372 =
0.02526 0.00363 0.00020 -0.00031
AFIX 43
H46 2 0.496947 0.647594 0.605723 11.00000 -1.20000
AFIX 0
C47 1 0.571685 0.775858 0.654443 11.00000 0.01264 0.02242 =
0.02784 0.00261 0.00642 0.00288
AFIX 43
H47 2 0.548476 0.827979 0.671696 11.00000 -1.20000
AFIX 0
C48 1 0.788544 0.726379 0.730515 11.00000 0.01321 0.01118 =
0.01021 -0.00178 0.00419 -0.00145
AFIX 23
H48A 2 0.744211 0.738273 0.733964 11.00000 -1.20000
H48B 2 0.819555 0.680346 0.763962 11.00000 -1.20000
AFIX 0
C49 1 0.817359 0.859476 0.727601 11.00000 0.01344 0.01111 =
0.01286 -0.00147 0.00503 -0.00107
C50 1 0.879990 0.913518 0.754788 11.00000 0.01313 0.02007 =
0.01885 -0.00416 0.00434 -0.00278
AFIX 43
H50 2 0.918686 0.870881 0.781095 11.00000 -1.20000
AFIX 0
C51 1 0.875889 1.048476 0.735686 11.00000 0.02451 0.01947 =
0.02600 -0.00629 0.01346 -0.00968
AFIX 43
H51 2 0.911483 1.112412 0.746885 11.00000 -1.20000
AFIX 0
C52 1 0.811731 1.066306 0.698845 11.00000 0.03078 0.01212 =
0.02056 0.00001 0.01207 -0.00380
AFIX 43
H52 2 0.794752 1.146529 0.679458 11.00000 -1.20000
AFIX 0
C53 1 0.873690 0.754974 0.621457 11.00000 0.03534 0.03272 =
0.03720 0.00430 0.02528 -0.00499
AFIX 137
H53A 2 0.835890 0.744610 0.585757 11.00000 -1.50000
H53B 2 0.917062 0.747078 0.616869 11.00000 -1.50000
H53C 2 0.870914 0.842488 0.636663 11.00000 -1.50000
AFIX 0
C54 1 0.941359 0.592895 0.745017 11.00000 0.01344 0.02884 =
0.02507 -0.00752 0.00306 0.00291
AFIX 137
H54A 2 0.972771 0.523520 0.743334 11.00000 -1.50000
H54B 2 0.921465 0.567054 0.771348 11.00000 -1.50000
H54C 2 0.966232 0.676633 0.756732 11.00000 -1.50000
AFIX 0
HKLF 4
REM P21n_a.res in P2(1)/n
REM R1 = 0.0530 for 17523 Fo > 4sig(Fo) and 0.0779 for all 23962 data
REM 593 parameters refined using 0 restraints
END
WGHT 0.0782 0.9522
REM Highest difference peak 0.802, deepest hole -0.609, 1-sigma level 0.077
Q1 1 0.7196 0.4800 0.3623 11.00000 0.05 0.80
Q2 1 0.7683 0.3957 0.6357 11.00000 0.05 0.76
Q3 1 0.7912 0.6574 0.4198 11.00000 0.05 0.72
Q4 1 0.6977 0.2178 0.5798 11.00000 0.05 0.62
Q5 1 0.8897 0.9904 0.7496 11.00000 0.05 0.59
Q6 1 0.8096 0.2650 0.5714 11.00000 0.05 0.58
Q7 1 0.8117 0.5990 0.3887 11.00000 0.05 0.58
Q8 1 0.6783 0.6026 0.4263 11.00000 0.05 0.58
Q9 1 0.7890 0.3381 0.6027 11.00000 0.05 0.57
Q10 1 0.8864 0.6186 0.6555 11.00000 0.05 0.54
Q11 1 0.6013 0.2504 0.3396 11.00000 0.05 0.53
Q12 1 0.6716 0.2931 0.6051 11.00000 0.05 0.52
Q13 1 0.6981 0.5461 0.3913 11.00000 0.05 0.52
Q14 1 0.6921 0.0828 0.2695 11.00000 0.05 0.50
Q15 1 0.5932 0.1382 0.5894 11.00000 0.05 0.50
Q16 1 0.6469 0.2556 0.3113 11.00000 0.05 0.48
Q17 1 0.8025 0.7920 0.7296 11.00000 0.05 0.46
Q18 1 0.7526 0.4505 0.6705 11.00000 0.05 0.45
Q19 1 0.9004 0.7434 0.4125 11.00000 0.05 0.45
Q20 1 0.7399 0.4195 0.3293 11.00000 0.05 0.45
;
_shelx_res_checksum 88339
_chemical_properties_physical Air-sensitive,Moisture-sensitive
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_tBufuranlargecryatal
_database_code_depnum_ccdc_archive 'CCDC 1551838'
_audit_update_record
;
2018-03-20 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety 'C25 H33 N O3'
_chemical_formula_sum 'C25 H33 N O3'
_chemical_formula_iupac ?
_chemical_formula_weight 395.52
_chemical_melting_point ?
_space_group_crystal_system monoclinic
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 18.3409(19)
_cell_length_b 6.4457(6)
_cell_length_c 38.253(3)
_cell_angle_alpha 90
_cell_angle_beta 95.468(7)
_cell_angle_gamma 90
_cell_volume 4501.7(7)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9990
_cell_measurement_theta_min 2.5645
_cell_measurement_theta_max 24.739
_cell_measurement_temperature 100
_exptl_crystal_description rectangular
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_size_max 0.500
_exptl_crystal_size_mid 0.300
_exptl_crystal_size_min 0.200
_exptl_crystal_density_diffrn 1.167
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1712
_exptl_absorpt_coefficient_mu 0.076
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min 0.973
_exptl_absorpt_correction_T_max 0.985
_exptl_special_details
;
;
_diffrn_ambient_temperature 100
_diffrn_source 'microfocus sealed x-ray tube'
_diffrn_source_type 'Incoatec I\mus'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator ?
_diffrn_measurement_device_type 'Bruker d8 venture'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 30413
_diffrn_reflns_av_R_equivalents 0.0937
_diffrn_reflns_av_unetI/netI 0.0394
_diffrn_reflns_theta_min 2.38
_diffrn_reflns_theta_max 24.76
_diffrn_reflns_theta_full 24.76
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -7
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -44
_diffrn_reflns_limit_l_max 44
_refine_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_number_total 3850
_reflns_number_gt 3527
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0847
_refine_ls_R_factor_gt 0.0785
_refine_ls_wR_factor_gt 0.1605
_refine_ls_wR_factor_ref 0.1634
_refine_ls_goodness_of_fit_ref 1.090
_refine_ls_restrained_S_all 1.090
_refine_ls_number_reflns 3850
_refine_ls_number_parameters 272
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+27.3858P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.376
_refine_diff_density_min -0.263
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection 'APEX3 v2015.5-2 (Bruker AXS Inc., 2015)'
_computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution 'XS, VERSION 2013/1'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 717)'
_computing_publication_material 'Bruker SHELXL (Bruker AXS Inc., 2015)'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.54105(12) 0.8555(4) 0.29099(6) 0.0274(6) Uani d . . . 1 . .
H H1 0.766(2) 0.483(6) 0.3513(10) 0.035(11) Uiso d . . . 1 . .
C C1 0.65890(16) 0.7979(5) 0.32387(8) 0.0183(6) Uani d . . . 1 . .
H H1A 0.6733 0.7935 0.2996 0.022 Uiso calc U . R 1 . .
H H1B 0.6916 0.8978 0.3373 0.022 Uiso calc U . R 1 . .
N N1 0.67045(13) 0.5895(4) 0.33982(6) 0.0169(5) Uani d . . . 1 . .
O O2 0.70296(12) 0.2504(4) 0.28614(6) 0.0275(5) Uani d . . . 1 . .
C C2 0.58201(16) 0.8757(4) 0.32282(7) 0.0176(6) Uani d . . . 1 . .
C C3 0.54059(17) 0.9548(5) 0.34665(8) 0.0215(7) Uani d . . . 1 . .
H H3 0.5559 0.9838 0.3706 0.026 Uiso calc U . R 1 . .
O O3 0.79689(11) 0.4065(3) 0.36490(5) 0.0194(5) Uani d . . . 1 . .
C C5 0.47236(19) 0.9265(6) 0.29613(10) 0.0339(8) Uani d . . . 1 . .
H H5 0.4324 0.9316 0.2784 0.041 Uiso calc U . R 1 . .
C C4 0.46917(18) 0.9872(5) 0.32919(9) 0.0279(8) Uani d . . . 1 . .
H H4 0.4277 1.0412 0.3392 0.033 Uiso calc U . R 1 . .
C C7 0.64225(16) 0.3731(5) 0.28686(8) 0.0186(6) Uani d . . . 1 . .
C C6 0.62181(16) 0.4304(5) 0.32224(7) 0.0172(6) Uani d . . . 1 . .
H H6A 0.5709 0.4831 0.32 0.021 Uiso calc U . R 1 . .
H H6B 0.6233 0.3045 0.3371 0.021 Uiso calc U . R 1 . .
C C25 0.68857(19) 0.0248(6) 0.50501(8) 0.0327(8) Uani d . . . 1 . .
H H25A 0.7323 -0.0555 0.5009 0.049 Uiso calc U . R 1 . .
H H25B 0.6627 -0.0439 0.5231 0.049 Uiso calc U . R 1 . .
H H25C 0.7031 0.1647 0.5129 0.049 Uiso calc U . R 1 . .
C C24 0.6124(2) -0.1805(6) 0.46053(9) 0.0339(9) Uani d . . . 1 . .
H H24A 0.5783 -0.1754 0.4392 0.051 Uiso calc U . R 1 . .
H H24B 0.5879 -0.2418 0.4797 0.051 Uiso calc U . R 1 . .
H H24C 0.655 -0.2652 0.4562 0.051 Uiso calc U . R 1 . .
C C23 0.5724(2) 0.1698(7) 0.47915(10) 0.0443(11) Uani d . . . 1 . .
H H23A 0.5355 0.1715 0.4588 0.066 Uiso calc U . R 1 . .
H H23B 0.5887 0.3119 0.4847 0.066 Uiso calc U . R 1 . .
H H23C 0.551 0.11 0.4994 0.066 Uiso calc U . R 1 . .
C C22 0.63759(16) 0.0393(5) 0.47064(8) 0.0198(7) Uani d . . . 1 . .
C C21 0.86094(17) -0.0171(5) 0.36163(8) 0.0213(7) Uani d . . . 1 . .
H H21A 0.8469 0.103 0.3468 0.032 Uiso calc U . R 1 . .
H H21B 0.8258 -0.1299 0.3563 0.032 Uiso calc U . R 1 . .
H H21C 0.91 -0.0635 0.3571 0.032 Uiso calc U . R 1 . .
C C20 0.87990(17) -0.1518(5) 0.42246(8) 0.0251(7) Uani d . . . 1 . .
H H20A 0.8412 -0.2554 0.4175 0.038 Uiso calc U . R 1 . .
H H20B 0.8839 -0.1164 0.4475 0.038 Uiso calc U . R 1 . .
H H20C 0.9266 -0.2086 0.4164 0.038 Uiso calc U . R 1 . .
C C19 0.92112(16) 0.2067(5) 0.41025(8) 0.0244(7) Uani d . . . 1 . .
H H19A 0.9686 0.1522 0.4047 0.037 Uiso calc U . R 1 . .
H H19B 0.9231 0.2375 0.4354 0.037 Uiso calc U . R 1 . .
H H19C 0.9099 0.334 0.3968 0.037 Uiso calc U . R 1 . .
C C18 0.86108(15) 0.0441(5) 0.40054(8) 0.0186(7) Uani d . . . 1 . .
C C17 0.75788(15) 0.3128(5) 0.38934(7) 0.0152(6) Uani d . . . 1 . .
C C16 0.78634(15) 0.1356(5) 0.40763(7) 0.0154(6) Uani d . . . 1 . .
C C15 0.74489(15) 0.0530(5) 0.43304(7) 0.0160(6) Uani d . . . 1 . .
H H15 0.7632 -0.0665 0.4455 0.019 Uiso calc U . R 1 . .
C C14 0.67818(16) 0.1351(5) 0.44126(7) 0.0171(6) Uani d . . . 1 . .
C C13 0.65154(15) 0.3053(5) 0.42193(7) 0.0170(6) Uani d . . . 1 . .
H H13 0.6054 0.3616 0.4263 0.02 Uiso calc U . R 1 . .
C C8 0.61249(18) 0.4100(6) 0.25403(8) 0.0289(8) Uani d . . . 1 . .
H H8 0.5704 0.4916 0.2473 0.035 Uiso calc U . R 1 . .
C C9 0.6570(2) 0.3015(6) 0.23112(8) 0.0348(9) Uani d . . . 1 . .
H H9 0.6501 0.2966 0.2062 0.042 Uiso calc U . R 1 . .
C C12 0.69029(16) 0.3964(5) 0.39635(7) 0.0174(6) Uani d . . . 1 . .
C C11 0.66219(16) 0.5926(5) 0.37788(7) 0.0176(6) Uani d . . . 1 . .
H H11A 0.6098 0.6105 0.3814 0.021 Uiso calc U . R 1 . .
H H11B 0.6892 0.7131 0.3887 0.021 Uiso calc U . R 1 . .
C C10 0.7093(2) 0.2100(6) 0.25145(9) 0.0342(9) Uani d . . . 1 . .
H H10 0.7467 0.1266 0.2431 0.041 Uiso calc U . R 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0266(12) 0.0329(14) 0.0219(12) 0.0116(10) -0.0019(9) -0.0031(10)
C1 0.0182(15) 0.0160(15) 0.0211(15) -0.0008(12) 0.0037(12) 0.0019(12)
N1 0.0198(13) 0.0149(13) 0.0162(12) -0.0008(11) 0.0019(10) 0.0018(10)
O2 0.0328(13) 0.0243(13) 0.0266(12) 0.0092(10) 0.0084(10) 0.0036(10)
C2 0.0254(16) 0.0095(14) 0.0174(15) -0.0017(12) -0.0004(12) 0.0024(12)
C3 0.0283(17) 0.0171(16) 0.0193(15) 0.0016(14) 0.0038(13) 0.0014(13)
O3 0.0174(11) 0.0221(12) 0.0187(11) 0.0012(9) 0.0024(9) 0.0058(9)
C5 0.0261(18) 0.037(2) 0.037(2) 0.0116(16) -0.0025(15) -0.0028(17)
C4 0.0245(17) 0.0242(18) 0.0361(19) 0.0095(14) 0.0091(14) 0.0044(15)
C7 0.0204(15) 0.0126(15) 0.0230(16) -0.0022(12) 0.0029(12) 0.0008(12)
C6 0.0173(15) 0.0157(15) 0.0188(15) -0.0033(12) 0.0033(12) 0.0001(12)
C25 0.036(2) 0.043(2) 0.0191(16) -0.0106(17) 0.0030(14) 0.0031(15)
C24 0.038(2) 0.040(2) 0.0244(17) -0.0185(17) 0.0069(15) -0.0031(16)
C23 0.044(2) 0.052(3) 0.042(2) 0.015(2) 0.0287(18) 0.0185(19)
C22 0.0185(15) 0.0212(16) 0.0201(15) -0.0040(13) 0.0042(12) 0.0012(13)
C21 0.0191(15) 0.0234(17) 0.0213(16) 0.0021(13) 0.0020(12) -0.0012(13)
C20 0.0199(16) 0.0287(18) 0.0266(17) 0.0064(14) 0.0014(13) 0.0053(14)
C19 0.0185(16) 0.0320(19) 0.0225(16) -0.0005(14) 0.0014(13) -0.0017(14)
C18 0.0146(14) 0.0211(16) 0.0196(15) 0.0006(13) -0.0005(12) -0.0004(13)
C17 0.0159(14) 0.0177(15) 0.0121(14) -0.0058(12) 0.0013(11) -0.0024(12)
C16 0.0140(14) 0.0183(15) 0.0133(14) -0.0028(12) -0.0020(11) -0.0036(12)
C15 0.0184(14) 0.0164(15) 0.0125(14) -0.0033(12) -0.0025(11) 0.0002(12)
C14 0.0173(15) 0.0186(16) 0.0147(14) -0.0027(12) -0.0016(12) -0.0029(12)
C13 0.0129(14) 0.0213(16) 0.0166(14) 0.0006(12) 0.0006(11) -0.0045(12)
C8 0.0203(16) 0.040(2) 0.0256(17) -0.0029(15) -0.0034(13) 0.0040(15)
C9 0.048(2) 0.043(2) 0.0139(16) -0.0168(19) 0.0039(15) -0.0057(15)
C12 0.0195(15) 0.0161(15) 0.0160(14) -0.0005(12) -0.0014(12) -0.0006(12)
C11 0.0214(15) 0.0152(15) 0.0167(14) 0.0019(13) 0.0042(12) -0.0018(12)
C10 0.052(2) 0.0228(18) 0.0312(19) -0.0023(17) 0.0223(18) -0.0043(15)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C5 . 1.372(4) ?
O1 C2 . 1.375(4) ?
C1 N1 . 1.482(4) ?
C1 C2 . 1.494(4) ?
C1 H1A . 0.99 ?
C1 H1B . 0.99 ?
N1 C6 . 1.478(4) ?
N1 C11 . 1.478(4) ?
O2 C7 . 1.368(4) ?
O2 C10 . 1.368(4) ?
C2 C3 . 1.342(4) ?
C3 C4 . 1.428(5) ?
C3 H3 . 0.95 ?
O3 C17 . 1.370(3) ?
O3 H1 . 0.89(4) ?
C5 C4 . 1.331(5) ?
C5 H5 . 0.95 ?
C4 H4 . 0.95 ?
C7 C8 . 1.342(4) ?
C7 C6 . 1.485(4) ?
C6 H6A . 0.99 ?
C6 H6B . 0.99 ?
C25 C22 . 1.542(4) ?
C25 H25A . 0.98 ?
C25 H25B . 0.98 ?
C25 H25C . 0.98 ?
C24 C22 . 1.528(5) ?
C24 H24A . 0.98 ?
C24 H24B . 0.98 ?
C24 H24C . 0.98 ?
C23 C22 . 1.523(5) ?
C23 H23A . 0.98 ?
C23 H23B . 0.98 ?
C23 H23C . 0.98 ?
C22 C14 . 1.536(4) ?
C21 C18 . 1.540(4) ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
C20 C18 . 1.537(4) ?
C20 H20A . 0.98 ?
C20 H20B . 0.98 ?
C20 H20C . 0.98 ?
C19 C18 . 1.540(4) ?
C19 H19A . 0.98 ?
C19 H19B . 0.98 ?
C19 H19C . 0.98 ?
C18 C16 . 1.540(4) ?
C17 C12 . 1.401(4) ?
C17 C16 . 1.413(4) ?
C16 C15 . 1.395(4) ?
C15 C14 . 1.396(4) ?
C15 H15 . 0.95 ?
C14 C13 . 1.386(4) ?
C13 C12 . 1.393(4) ?
C13 H13 . 0.95 ?
C8 C9 . 1.436(5) ?
C8 H8 . 0.95 ?
C9 C10 . 1.315(5) ?
C9 H9 . 0.95 ?
C12 C11 . 1.514(4) ?
C11 H11A . 0.99 ?
C11 H11B . 0.99 ?
C10 H10 . 0.95 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C5 O1 C2 . . 105.9(2) ?
N1 C1 C2 . . 114.4(2) ?
N1 C1 H1A . . 108.7 ?
C2 C1 H1A . . 108.7 ?
N1 C1 H1B . . 108.7 ?
C2 C1 H1B . . 108.7 ?
H1A C1 H1B . . 107.6 ?
C6 N1 C11 . . 110.1(2) ?
C6 N1 C1 . . 112.6(2) ?
C11 N1 C1 . . 111.7(2) ?
C7 O2 C10 . . 105.9(3) ?
C3 C2 O1 . . 109.9(3) ?
C3 C2 C1 . . 134.7(3) ?
O1 C2 C1 . . 115.3(2) ?
C2 C3 C4 . . 106.9(3) ?
C2 C3 H3 . . 126.5 ?
C4 C3 H3 . . 126.5 ?
C17 O3 H1 . . 107.(2) ?
C4 C5 O1 . . 111.0(3) ?
C4 C5 H5 . . 124.5 ?
O1 C5 H5 . . 124.5 ?
C5 C4 C3 . . 106.3(3) ?
C5 C4 H4 . . 126.9 ?
C3 C4 H4 . . 126.9 ?
C8 C7 O2 . . 110.1(3) ?
C8 C7 C6 . . 133.9(3) ?
O2 C7 C6 . . 116.0(3) ?
N1 C6 C7 . . 113.2(2) ?
N1 C6 H6A . . 108.9 ?
C7 C6 H6A . . 108.9 ?
N1 C6 H6B . . 108.9 ?
C7 C6 H6B . . 108.9 ?
H6A C6 H6B . . 107.8 ?
C22 C25 H25A . . 109.5 ?
C22 C25 H25B . . 109.5 ?
H25A C25 H25B . . 109.5 ?
C22 C25 H25C . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
C22 C24 H24A . . 109.5 ?
C22 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C22 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
C22 C23 H23A . . 109.5 ?
C22 C23 H23B . . 109.5 ?
H23A C23 H23B . . 109.5 ?
C22 C23 H23C . . 109.5 ?
H23A C23 H23C . . 109.5 ?
H23B C23 H23C . . 109.5 ?
C23 C22 C24 . . 110.0(3) ?
C23 C22 C14 . . 112.3(3) ?
C24 C22 C14 . . 110.1(3) ?
C23 C22 C25 . . 106.0(3) ?
C24 C22 C25 . . 107.7(3) ?
C14 C22 C25 . . 110.6(2) ?
C18 C21 H21A . . 109.5 ?
C18 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C18 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C18 C20 H20A . . 109.5 ?
C18 C20 H20B . . 109.5 ?
H20A C20 H20B . . 109.5 ?
C18 C20 H20C . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
C18 C19 H19A . . 109.5 ?
C18 C19 H19B . . 109.5 ?
H19A C19 H19B . . 109.5 ?
C18 C19 H19C . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
C20 C18 C21 . . 107.2(3) ?
C20 C18 C19 . . 108.0(2) ?
C21 C18 C19 . . 110.1(2) ?
C20 C18 C16 . . 112.1(2) ?
C21 C18 C16 . . 110.4(2) ?
C19 C18 C16 . . 109.0(2) ?
O3 C17 C12 . . 119.4(3) ?
O3 C17 C16 . . 120.1(3) ?
C12 C17 C16 . . 120.5(3) ?
C15 C16 C17 . . 117.0(3) ?
C15 C16 C18 . . 122.0(3) ?
C17 C16 C18 . . 121.0(3) ?
C16 C15 C14 . . 124.0(3) ?
C16 C15 H15 . . 118.0 ?
C14 C15 H15 . . 118.0 ?
C13 C14 C15 . . 116.9(3) ?
C13 C14 C22 . . 122.6(3) ?
C15 C14 C22 . . 120.6(3) ?
C14 C13 C12 . . 122.1(3) ?
C14 C13 H13 . . 119.0 ?
C12 C13 H13 . . 119.0 ?
C7 C8 C9 . . 106.3(3) ?
C7 C8 H8 . . 126.9 ?
C9 C8 H8 . . 126.9 ?
C10 C9 C8 . . 106.4(3) ?
C10 C9 H9 . . 126.8 ?
C8 C9 H9 . . 126.8 ?
C13 C12 C17 . . 119.5(3) ?
C13 C12 C11 . . 120.4(3) ?
C17 C12 C11 . . 120.0(3) ?
N1 C11 C12 . . 112.7(2) ?
N1 C11 H11A . . 109.1 ?
C12 C11 H11A . . 109.1 ?
N1 C11 H11B . . 109.1 ?
C12 C11 H11B . . 109.1 ?
H11A C11 H11B . . 107.8 ?
C9 C10 O2 . . 111.3(3) ?
C9 C10 H10 . . 124.4 ?
O2 C10 H10 . . 124.4 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 C1 N1 C6 . . . . 56.4(3) ?
C2 C1 N1 C11 . . . . -68.1(3) ?
C5 O1 C2 C3 . . . . 0.2(3) ?
C5 O1 C2 C1 . . . . 177.3(3) ?
N1 C1 C2 C3 . . . . 75.9(4) ?
N1 C1 C2 O1 . . . . -100.3(3) ?
O1 C2 C3 C4 . . . . 0.0(4) ?
C1 C2 C3 C4 . . . . -176.3(3) ?
C2 O1 C5 C4 . . . . -0.4(4) ?
O1 C5 C4 C3 . . . . 0.4(4) ?
C2 C3 C4 C5 . . . . -0.3(4) ?
C10 O2 C7 C8 . . . . -0.7(3) ?
C10 O2 C7 C6 . . . . 177.3(3) ?
C11 N1 C6 C7 . . . . -162.7(2) ?
C1 N1 C6 C7 . . . . 72.0(3) ?
C8 C7 C6 N1 . . . . -108.0(4) ?
O2 C7 C6 N1 . . . . 74.6(3) ?
O3 C17 C16 C15 . . . . 177.7(2) ?
C12 C17 C16 C15 . . . . -1.3(4) ?
O3 C17 C16 C18 . . . . -0.1(4) ?
C12 C17 C16 C18 . . . . -179.1(3) ?
C20 C18 C16 C15 . . . . 4.1(4) ?
C21 C18 C16 C15 . . . . 123.6(3) ?
C19 C18 C16 C15 . . . . -115.4(3) ?
C20 C18 C16 C17 . . . . -178.1(3) ?
C21 C18 C16 C17 . . . . -58.7(4) ?
C19 C18 C16 C17 . . . . 62.3(3) ?
C17 C16 C15 C14 . . . . -0.2(4) ?
C18 C16 C15 C14 . . . . 177.6(3) ?
C16 C15 C14 C13 . . . . 2.0(4) ?
C16 C15 C14 C22 . . . . -177.6(3) ?
C23 C22 C14 C13 . . . . -8.2(4) ?
C24 C22 C14 C13 . . . . 114.7(3) ?
C25 C22 C14 C13 . . . . -126.4(3) ?
C23 C22 C14 C15 . . . . 171.4(3) ?
C24 C22 C14 C15 . . . . -65.7(4) ?
C25 C22 C14 C15 . . . . 53.2(4) ?
C15 C14 C13 C12 . . . . -2.4(4) ?
C22 C14 C13 C12 . . . . 177.2(3) ?
O2 C7 C8 C9 . . . . 0.6(4) ?
C6 C7 C8 C9 . . . . -176.9(3) ?
C7 C8 C9 C10 . . . . -0.2(4) ?
C14 C13 C12 C17 . . . . 1.0(4) ?
C14 C13 C12 C11 . . . . -175.0(3) ?
O3 C17 C12 C13 . . . . -178.1(3) ?
C16 C17 C12 C13 . . . . 0.9(4) ?
O3 C17 C12 C11 . . . . -2.0(4) ?
C16 C17 C12 C11 . . . . 176.9(3) ?
C6 N1 C11 C12 . . . . 67.2(3) ?
C1 N1 C11 C12 . . . . -166.9(2) ?
C13 C12 C11 N1 . . . . -138.7(3) ?
C17 C12 C11 N1 . . . . 45.3(4) ?
C8 C9 C10 O2 . . . . -0.2(4) ?
C7 O2 C10 C9 . . . . 0.6(4) ?
_shelx_res_file
;
C2-c.res created by SHELXL-2014/7
TITL C2-c_a.res in C2/c
REM Old TITL C2-c in C2/c
REM SHELXT solution in C2/c
REM R1 0.149, Rweak 0.017, Alpha 0.048, Orientation as input
REM Formula found by SHELXT: C25 N O3
CELL 0.71073 18.3409 6.4457 38.2526 90.000 95.468 90.000
ZERR 8.000 0.0019 0.0006 0.0033 0.000 0.007 0.000
LATT 7
SYMM -X, Y, 1/2-Z
SFAC C H N O
UNIT 200 264 8 24
TEMP -173.140
L.S. 4
BOND $H
OMIT 0 2 2
OMIT 0 2 0
OMIT -16 0 4
LIST 4
ACTA
CONF
FMAP 2
PLAN 20
WGHT 0.021700 27.385777
FVAR 0.30089
O1 4 0.541054 0.855484 0.290991 11.00000 0.02661 0.03287 =
0.02190 -0.00307 -0.00195 0.01156
H1 2 0.765579 0.482503 0.351299 11.00000 0.03543
C1 1 0.658900 0.797876 0.323867 11.00000 0.01816 0.01604 =
0.02113 0.00189 0.00366 -0.00083
AFIX 23
H1A 2 0.673296 0.793500 0.299584 11.00000 -1.20000
H1B 2 0.691642 0.897767 0.337291 11.00000 -1.20000
AFIX 0
N1 3 0.670448 0.589516 0.339816 11.00000 0.01975 0.01489 =
0.01620 0.00176 0.00193 -0.00076
O2 4 0.702960 0.250431 0.286137 11.00000 0.03278 0.02425 =
0.02662 0.00363 0.00842 0.00919
C2 1 0.582008 0.875665 0.322823 11.00000 0.02537 0.00954 =
0.01738 0.00240 -0.00035 -0.00175
C3 1 0.540590 0.954813 0.346646 11.00000 0.02834 0.01706 =
0.01933 0.00140 0.00380 0.00163
AFIX 43
H3 2 0.555872 0.983818 0.370576 11.00000 -1.20000
AFIX 0
O3 4 0.796887 0.406481 0.364895 11.00000 0.01744 0.02212 =
0.01870 0.00579 0.00237 0.00125
C5 1 0.472362 0.926454 0.296126 11.00000 0.02607 0.03746 =
0.03704 -0.00275 -0.00253 0.01164
AFIX 43
H5 2 0.432387 0.931574 0.278425 11.00000 -1.20000
AFIX 0
C4 1 0.469169 0.987159 0.329190 11.00000 0.02452 0.02416 =
0.03607 0.00443 0.00909 0.00947
AFIX 43
H4 2 0.427666 1.041216 0.339185 11.00000 -1.20000
AFIX 0
C7 1 0.642254 0.373113 0.286855 11.00000 0.02038 0.01257 =
0.02297 0.00075 0.00291 -0.00223
C6 1 0.621810 0.430415 0.322240 11.00000 0.01733 0.01568 =
0.01882 0.00011 0.00330 -0.00326
AFIX 23
H6A 2 0.570880 0.483132 0.320004 11.00000 -1.20000
H6B 2 0.623294 0.304539 0.337120 11.00000 -1.20000
AFIX 0
C25 1 0.688573 0.024836 0.505012 11.00000 0.03628 0.04279 =
0.01906 0.00306 0.00299 -0.01055
AFIX 137
H25A 2 0.732304 -0.055462 0.500877 11.00000 -1.50000
H25B 2 0.662720 -0.043904 0.523064 11.00000 -1.50000
H25C 2 0.703097 0.164708 0.512942 11.00000 -1.50000
AFIX 0
C24 1 0.612415 -0.180512 0.460526 11.00000 0.03808 0.03987 =
0.02442 -0.00310 0.00688 -0.01847
AFIX 137
H24A 2 0.578263 -0.175429 0.439220 11.00000 -1.50000
H24B 2 0.587859 -0.241787 0.479711 11.00000 -1.50000
H24C 2 0.654977 -0.265248 0.456162 11.00000 -1.50000
AFIX 0
C23 1 0.572384 0.169802 0.479153 11.00000 0.04369 0.05235 =
0.04161 0.01854 0.02873 0.01505
AFIX 137
H23A 2 0.535527 0.171542 0.458847 11.00000 -1.50000
H23B 2 0.588653 0.311874 0.484686 11.00000 -1.50000
H23C 2 0.551003 0.110005 0.499406 11.00000 -1.50000
AFIX 0
C22 1 0.637595 0.039260 0.470641 11.00000 0.01845 0.02116 =
0.02011 0.00116 0.00423 -0.00397
C21 1 0.860939 -0.017132 0.361630 11.00000 0.01908 0.02337 =
0.02132 -0.00117 0.00199 0.00205
AFIX 137
H21A 2 0.846898 0.103025 0.346794 11.00000 -1.50000
H21B 2 0.825801 -0.129873 0.356259 11.00000 -1.50000
H21C 2 0.910028 -0.063534 0.357071 11.00000 -1.50000
AFIX 0
C20 1 0.879898 -0.151850 0.422459 11.00000 0.01991 0.02873 =
0.02659 0.00532 0.00141 0.00638
AFIX 137
H20A 2 0.841185 -0.255443 0.417494 11.00000 -1.50000
H20B 2 0.883887 -0.116421 0.447483 11.00000 -1.50000
H20C 2 0.926621 -0.208628 0.416377 11.00000 -1.50000
AFIX 0
C19 1 0.921117 0.206731 0.410248 11.00000 0.01848 0.03201 =
0.02247 -0.00165 0.00140 -0.00045
AFIX 137
H19A 2 0.968570 0.152214 0.404735 11.00000 -1.50000
H19B 2 0.923097 0.237495 0.435409 11.00000 -1.50000
H19C 2 0.909893 0.333979 0.396777 11.00000 -1.50000
AFIX 0
C18 1 0.861082 0.044117 0.400539 11.00000 0.01458 0.02110 =
0.01959 -0.00041 -0.00051 0.00061
C17 1 0.757879 0.312819 0.389336 11.00000 0.01586 0.01768 =
0.01208 -0.00238 0.00128 -0.00582
C16 1 0.786336 0.135577 0.407634 11.00000 0.01403 0.01830 =
0.01326 -0.00357 -0.00202 -0.00276
C15 1 0.744887 0.052951 0.433041 11.00000 0.01835 0.01643 =
0.01249 0.00018 -0.00246 -0.00326
AFIX 43
H15 2 0.763178 -0.066506 0.445512 11.00000 -1.20000
AFIX 0
C14 1 0.678176 0.135085 0.441259 11.00000 0.01733 0.01859 =
0.01473 -0.00292 -0.00158 -0.00273
C13 1 0.651537 0.305290 0.421931 11.00000 0.01289 0.02126 =
0.01664 -0.00450 0.00055 0.00057
AFIX 43
H13 2 0.605386 0.361615 0.426264 11.00000 -1.20000
AFIX 0
C8 1 0.612493 0.409968 0.254034 11.00000 0.02025 0.03987 =
0.02561 0.00401 -0.00342 -0.00290
AFIX 43
H8 2 0.570355 0.491584 0.247299 11.00000 -1.20000
AFIX 0
C9 1 0.657035 0.301456 0.231123 11.00000 0.04751 0.04334 =
0.01386 -0.00572 0.00390 -0.01680
AFIX 43
H9 2 0.650100 0.296644 0.206206 11.00000 -1.20000
AFIX 0
C12 1 0.690292 0.396420 0.396345 11.00000 0.01947 0.01614 =
0.01605 -0.00061 -0.00138 -0.00051
C11 1 0.662190 0.592567 0.377883 11.00000 0.02137 0.01517 =
0.01666 -0.00184 0.00422 0.00194
AFIX 23
H11A 2 0.609770 0.610523 0.381376 11.00000 -1.20000
H11B 2 0.689202 0.713102 0.388661 11.00000 -1.20000
AFIX 0
C10 1 0.709344 0.210016 0.251448 11.00000 0.05198 0.02284 =
0.03118 -0.00425 0.02227 -0.00229
AFIX 43
H10 2 0.746741 0.126647 0.243115 11.00000 -1.20000
REM #####
REM #####
AFIX 0
HKLF 4
REM C2-c_a.res in C2/c
REM R1 = 0.0785 for 3527 Fo > 4sig(Fo) and 0.0847 for all 3850 data
REM 272 parameters refined using 0 restraints
END
WGHT 0.0216 20.1596
REM Highest difference peak 0.376, deepest hole -0.263, 1-sigma level 0.064
Q1 1 0.5675 -0.0612 0.4456 11.00000 0.05 0.38
Q2 1 0.7617 0.1670 0.3901 11.00000 0.05 0.29
Q3 1 0.8615 0.0260 0.3819 11.00000 0.05 0.27
Q4 1 0.8152 0.6131 0.3619 11.00000 0.05 0.27
Q5 1 0.8393 -0.3018 0.4116 11.00000 0.05 0.25
Q6 1 0.6475 -0.0783 0.4811 11.00000 0.05 0.24
Q7 1 0.7644 0.1103 0.2604 11.00000 0.05 0.22
Q8 1 0.8862 0.1290 0.4006 11.00000 0.05 0.22
Q9 1 0.8035 0.5961 0.3872 11.00000 0.05 0.21
Q10 1 0.5402 0.1032 0.4575 11.00000 0.05 0.21
Q11 1 0.9608 0.1359 0.4165 11.00000 0.05 0.20
Q12 1 0.8818 0.0027 0.4185 11.00000 0.05 0.20
Q13 1 0.6425 0.7274 0.2510 11.00000 0.05 0.19
Q14 1 0.7865 0.1971 0.2901 11.00000 0.05 0.19
Q15 1 0.6562 0.1472 0.4234 11.00000 0.05 0.19
Q16 1 0.9194 0.3845 0.4199 11.00000 0.05 0.19
Q17 1 0.5585 0.8477 0.3398 11.00000 0.05 0.19
Q18 1 0.7936 0.1927 0.2560 11.00000 0.05 0.18
Q19 1 0.8253 0.0887 0.4029 11.00000 0.05 0.18
Q20 1 0.5212 -0.0041 0.5287 11.00000 0.05 0.18
;
_shelx_res_checksum 1344
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_'complex2_LAlMeCl'
_database_code_depnum_ccdc_archive 'CCDC 1563972'
_audit_update_record
;
2018-03-20 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C26 H35 Al Cl N O3'
_chemical_formula_iupac ?
_chemical_formula_weight 471.98
_chemical_melting_point ?
_space_group_crystal_system monoclinic
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 21.164(3)
_cell_length_b 10.0463(13)
_cell_length_c 26.332(3)
_cell_angle_alpha 90
_cell_angle_beta 112.398(4)
_cell_angle_gamma 90
_cell_volume 5176.3(11)
_cell_formula_units_Z 8
_cell_measurement_reflns_used 9689
_cell_measurement_theta_min 2.2874
_cell_measurement_theta_max 27.5367
_cell_measurement_temperature 133
_exptl_crystal_description rectangle
_exptl_crystal_colour 'clear light colourless'
_exptl_crystal_size_max 0.423
_exptl_crystal_size_mid 0.263
_exptl_crystal_size_min 0.098
_exptl_crystal_density_diffrn 1.211
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2016
_exptl_absorpt_coefficient_mu 0.208
_exptl_absorpt_correction_type Multi-Scan
_exptl_absorpt_process_details
;
SADABS-2014/5 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min 0.65
_exptl_absorpt_correction_T_max 0.74
_exptl_special_details
;
;
_diffrn_ambient_temperature 133
_diffrn_source 'microfocus sealed x-ray tube'
_diffrn_source_type 'Incoatec I\mus'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_monochromator ?
_diffrn_measurement_device_type 'Bruker D8 venture'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number 173047
_diffrn_reflns_av_R_equivalents 0.0812
_diffrn_reflns_av_unetI/netI 0.0374
_diffrn_reflns_theta_min 2.19
_diffrn_reflns_theta_max 27.10
_diffrn_reflns_theta_full 27.10
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -27
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_limit_l_max 32
_refine_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_number_total 11382
_reflns_number_gt 8703
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_R_factor_all 0.0758
_refine_ls_R_factor_gt 0.0524
_refine_ls_wR_factor_gt 0.1235
_refine_ls_wR_factor_ref 0.1362
_refine_ls_goodness_of_fit_ref 1.054
_refine_ls_restrained_S_all 1.070
_refine_ls_number_reflns 11382
_refine_ls_number_parameters 595
_refine_ls_number_restraints 72
_refine_ls_number_constraints ?
_refine_ls_hydrogen_treatment constr
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+6.3558P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.478
_refine_diff_density_min -0.677
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection 'APEX3 v2015.5-2 (Bruker AXS Inc., 2015)'
_computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 717)'
_computing_publication_material 'Bruker SHELXL (Bruker AXS Inc., 2015)'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl1A 0.44326(4) 0.58087(9) 0.74799(3) 0.02863(19) Uani d U P D 0.858(2) A 1
Al Al1 0.36550(3) 0.61097(7) 0.66827(3) 0.01985(15) Uani d U . D 1.0 . .
O O1 0.34687(8) 0.45724(16) 0.63635(6) 0.0253(4) Uani d . . . 1.0 . .
O O2 0.14092(8) 0.78903(15) 0.66585(6) 0.0238(3) Uani d . . . 1.0 . .
O O3 0.27691(7) 0.95047(14) 0.69489(6) 0.0203(3) Uani d . . . 1.0 . .
N N1A 0.27891(8) 0.63680(16) 0.68120(7) 0.0145(3) Uani d . . . 1.0 . .
C C26A 0.38270(18) 0.7560(3) 0.62537(15) 0.02863(19) Uani d U P D 0.858(2) A 1
H H26A 0.420462 0.811162 0.649379 0.043 Uiso calc . P GR 0.858(2) A 1
H H26B 0.341477 0.810718 0.609421 0.043 Uiso calc . P GR 0.858(2) A 1
H H26C 0.394751 0.71862 0.595875 0.043 Uiso calc . P GR 0.858(2) A 1
C C1 0.29048(10) 0.3804(2) 0.62179(8) 0.0172(4) Uani d . . . 1.0 . .
C C2 0.24335(10) 0.4020(2) 0.64676(8) 0.0152(4) Uani d . . . 1.0 . .
C C3 0.18331(10) 0.3286(2) 0.63067(8) 0.0163(4) Uani d . . . 1.0 . .
H H3 0.151356 0.346126 0.647213 0.02 Uiso calc . . R 1.0 . .
C C4 0.16898(10) 0.2296(2) 0.59068(8) 0.0177(4) Uani d . . . 1.0 . .
C C5 0.21775(11) 0.2072(2) 0.56786(8) 0.0186(4) Uani d . . . 1.0 . .
H H5 0.208947 0.139596 0.540813 0.022 Uiso calc . . R 1.0 . .
C C6 0.27865(10) 0.2786(2) 0.58254(8) 0.0176(4) Uani d . . . 1.0 . .
C C7 0.25929(10) 0.49990(19) 0.69366(8) 0.0148(4) Uani d . . . 1.0 . .
H H7A 0.218729 0.507918 0.70351 0.018 Uiso calc . . R 1.0 . .
H H7B 0.297178 0.463871 0.726045 0.018 Uiso calc . . R 1.0 . .
C C8 0.10069(11) 0.1546(2) 0.57082(9) 0.0226(5) Uani d . . . 1.0 . .
C C9 0.04584(12) 0.2450(3) 0.53113(11) 0.0367(6) Uani d . . . 1.0 . .
H H9A 0.044499 0.329274 0.549445 0.055 Uiso calc . . GR 1.0 . .
H H9B 0.001219 0.201138 0.519778 0.055 Uiso calc . . GR 1.0 . .
H H9C 0.056668 0.262573 0.498727 0.055 Uiso calc . . GR 1.0 . .
C C10 0.08016(13) 0.1208(3) 0.61917(10) 0.0344(6) Uani d . . . 1.0 . .
H H10A 0.115894 0.066211 0.645823 0.052 Uiso calc . . GR 1.0 . .
H H10B 0.037005 0.071248 0.605746 0.052 Uiso calc . . GR 1.0 . .
H H10C 0.074437 0.203174 0.636869 0.052 Uiso calc . . GR 1.0 . .
C C11 0.10463(14) 0.0239(3) 0.54259(13) 0.0437(7) Uani d . . . 1.0 . .
H H11A 0.11088 0.042899 0.508292 0.065 Uiso calc . . GR 1.0 . .
H H11B 0.062193 -0.026268 0.53447 0.065 Uiso calc . . GR 1.0 . .
H H11C 0.143335 -0.028683 0.566875 0.065 Uiso calc . . GR 1.0 . .
C C12 0.33164(11) 0.2465(2) 0.55737(9) 0.0224(5) Uani d . . . 1.0 . .
C C13 0.34151(14) 0.3673(3) 0.52528(10) 0.0322(6) Uani d . . . 1.0 . .
H H13A 0.298663 0.386001 0.494251 0.048 Uiso calc . . GR 1.0 . .
H H13B 0.377529 0.347853 0.511536 0.048 Uiso calc . . GR 1.0 . .
H H13C 0.354612 0.444968 0.549582 0.048 Uiso calc . . GR 1.0 . .
C C14 0.40010(12) 0.2081(3) 0.60309(10) 0.0340(6) Uani d . . . 1.0 . .
H H14A 0.417385 0.283294 0.62829 0.051 Uiso calc . . GR 1.0 . .
H H14B 0.433248 0.185186 0.58674 0.051 Uiso calc . . GR 1.0 . .
H H14C 0.393268 0.131217 0.623354 0.051 Uiso calc . . GR 1.0 . .
C C15 0.30933(14) 0.1283(3) 0.51761(10) 0.0318(6) Uani d . . . 1.0 . .
H H15A 0.30465 0.048831 0.537504 0.048 Uiso calc . . GR 1.0 . .
H H15B 0.343748 0.111967 0.501841 0.048 Uiso calc . . GR 1.0 . .
H H15C 0.265344 0.148444 0.488101 0.048 Uiso calc . . GR 1.0 . .
C C16 0.22280(10) 0.6931(2) 0.63075(8) 0.0179(4) Uani d . . . 1.0 . .
H H16A 0.23559 0.784966 0.62498 0.022 Uiso calc . . R 1.0 . .
H H16B 0.220677 0.639709 0.598535 0.022 Uiso calc . . R 1.0 . .
C C17 0.15335(11) 0.6965(2) 0.63235(8) 0.0193(4) Uani d . . . 1.0 . .
C C18 0.09564(11) 0.6278(2) 0.60465(9) 0.0260(5) Uani d . . . 1.0 . .
H H18 0.090388 0.558363 0.578869 0.031 Uiso calc . . R 1.0 . .
C C19 0.04396(11) 0.6798(2) 0.62160(10) 0.0294(5) Uani d . . . 1.0 . .
H H19 -0.002344 0.651798 0.609252 0.035 Uiso calc . . R 1.0 . .
C C20 0.07348(11) 0.7757(2) 0.65825(10) 0.0281(5) Uani d . . . 1.0 . .
H H20 0.05086 0.827331 0.676453 0.034 Uiso calc . . R 1.0 . .
C C21 0.29074(10) 0.7233(2) 0.73106(8) 0.0161(4) Uani d . . . 1.0 . .
H H21A 0.246659 0.736414 0.735322 0.019 Uiso calc . . R 1.0 . .
H H21B 0.321879 0.676139 0.764146 0.019 Uiso calc . . R 1.0 . .
C C22 0.32047(10) 0.8560(2) 0.72796(8) 0.0173(4) Uani d . . . 1.0 . .
C C23 0.38389(11) 0.9072(2) 0.75259(9) 0.0231(5) Uani d . . . 1.0 . .
H H23 0.423107 0.862567 0.777329 0.028 Uiso calc . . R 1.0 . .
C C24 0.38041(13) 1.0418(2) 0.73412(10) 0.0279(5) Uani d . . . 1.0 . .
H H24 0.416846 1.104186 0.744239 0.034 Uiso calc . . R 1.0 . .
C C25 0.31541(12) 1.0627(2) 0.69961(9) 0.0260(5) Uani d . . . 1.0 . .
H H25 0.298554 1.144144 0.681064 0.031 Uiso calc . . R 1.0 . .
Cl Cl2A 0.55083(4) 0.21113(9) 0.74626(3) 0.02660(18) Uani d U P D 0.855(2) B 1
Al Al2 0.62492(3) 0.24612(6) 0.82711(3) 0.01782(14) Uani d U . D 1.0 . .
O O4 0.64271(7) 0.09420(15) 0.86097(6) 0.0231(3) Uani d . . . 1.0 . .
O O5 0.71872(7) 0.58319(14) 0.80238(6) 0.0201(3) Uani d . . . 1.0 . .
O O6 0.85501(8) 0.41876(16) 0.83933(6) 0.0248(3) Uani d . . . 1.0 . .
N N1B 0.71377(8) 0.26949(16) 0.81717(7) 0.0144(3) Uani d . . . 1.0 . .
C C52A 0.61556(18) 0.3904(4) 0.87724(15) 0.02660(18) Uani d U P D 0.855(2) B 1
H H52A 0.609238 0.476584 0.858502 0.04 Uiso calc . P GR 0.855(2) B 1
H H52B 0.656958 0.393149 0.910837 0.04 Uiso calc . P GR 0.855(2) B 1
H H52C 0.575936 0.371502 0.886695 0.04 Uiso calc . P GR 0.855(2) B 1
C C27 0.69784(10) 0.0138(2) 0.87596(8) 0.0163(4) Uani d . . . 1.0 . .
C C28 0.74722(10) 0.0342(2) 0.85297(8) 0.0163(4) Uani d . . . 1.0 . .
C C29 0.80660(10) -0.0413(2) 0.87076(8) 0.0164(4) Uani d . . . 1.0 . .
H H29 0.840235 -0.024245 0.855876 0.02 Uiso calc . . R 1.0 . .
C C30 0.81824(10) -0.1417(2) 0.90995(8) 0.0176(4) Uani d . . . 1.0 . .
C C31 0.76691(11) -0.1636(2) 0.93020(8) 0.0183(4) Uani d . . . 1.0 . .
H H31 0.773364 -0.232896 0.956252 0.022 Uiso calc . . R 1.0 . .
C C32 0.70665(10) -0.0893(2) 0.91428(8) 0.0179(4) Uani d . . . 1.0 . .
C C33 0.73424(10) 0.1313(2) 0.80631(8) 0.0161(4) Uani d . . . 1.0 . .
H H33A 0.697622 0.095163 0.773126 0.019 Uiso calc . . R 1.0 . .
H H33B 0.776181 0.138363 0.7983 0.019 Uiso calc . . R 1.0 . .
C C34 0.88507(11) -0.2207(2) 0.93008(9) 0.0217(5) Uani d . . . 1.0 . .
C C35 0.94195(13) -0.1335(3) 0.96964(11) 0.0389(6) Uani d . . . 1.0 . .
H H35A 0.946638 -0.05258 0.950608 0.058 Uiso calc . . GR 1.0 . .
H H35B 0.985151 -0.182898 0.982466 0.058 Uiso calc . . GR 1.0 . .
H H35C 0.930472 -0.109363 1.001155 0.058 Uiso calc . . GR 1.0 . .
C C36 0.90465(13) -0.2600(3) 0.88172(10) 0.0317(5) Uani d . . . 1.0 . .
H H36A 0.866908 -0.309378 0.854564 0.048 Uiso calc . . GR 1.0 . .
H H36B 0.945601 -0.316097 0.895021 0.048 Uiso calc . . GR 1.0 . .
H H36C 0.913946 -0.179551 0.864678 0.048 Uiso calc . . GR 1.0 . .
C C37 0.88020(14) -0.3497(2) 0.95961(11) 0.0342(6) Uani d . . . 1.0 . .
H H37A 0.872053 -0.327913 0.992889 0.051 Uiso calc . . GR 1.0 . .
H H37B 0.923068 -0.399469 0.969638 0.051 Uiso calc . . GR 1.0 . .
H H37C 0.842374 -0.40402 0.935177 0.051 Uiso calc . . GR 1.0 . .
C C38 0.65098(11) -0.1209(2) 0.93665(9) 0.0224(5) Uani d . . . 1.0 . .
C C39 0.64148(13) -0.0023(2) 0.97012(10) 0.0290(5) Uani d . . . 1.0 . .
H H39A 0.683773 0.012283 1.002211 0.044 Uiso calc . . GR 1.0 . .
H H39B 0.60407 -0.021438 0.982304 0.044 Uiso calc . . GR 1.0 . .
H H39C 0.630537 0.077802 0.947128 0.044 Uiso calc . . GR 1.0 . .
C C40 0.58322(12) -0.1525(3) 0.88861(10) 0.0313(5) Uani d . . . 1.0 . .
H H40A 0.569864 -0.076528 0.863396 0.047 Uiso calc . . GR 1.0 . .
H H40B 0.54752 -0.169822 0.902932 0.047 Uiso calc . . GR 1.0 . .
H H40C 0.589178 -0.231315 0.868946 0.047 Uiso calc . . GR 1.0 . .
C C41 0.66935(13) -0.2429(2) 0.97479(10) 0.0319(6) Uani d . . . 1.0 . .
H H41A 0.673392 -0.321424 0.954151 0.048 Uiso calc . . GR 1.0 . .
H H41B 0.633426 -0.257917 0.989076 0.048 Uiso calc . . GR 1.0 . .
H H41C 0.712946 -0.227115 1.005445 0.048 Uiso calc . . GR 1.0 . .
C C42 0.76745(10) 0.3252(2) 0.86897(8) 0.0161(4) Uani d . . . 1.0 . .
H H42A 0.75431 0.417492 0.873852 0.019 Uiso calc . . R 1.0 . .
H H42B 0.76677 0.272431 0.900505 0.019 Uiso calc . . R 1.0 . .
C C43 0.83858(11) 0.3273(2) 0.87124(8) 0.0196(4) Uani d . . . 1.0 . .
C C44 0.89505(11) 0.2592(3) 0.90257(10) 0.0285(5) Uani d . . . 1.0 . .
H H44 0.897533 0.190085 0.927872 0.034 Uiso calc . . R 1.0 . .
C C45 0.95037(12) 0.3117(3) 0.89017(11) 0.0350(6) Uani d . . . 1.0 . .
H H45 0.996893 0.285012 0.905984 0.042 Uiso calc . . R 1.0 . .
C C46 0.92375(11) 0.4059(3) 0.85193(11) 0.0309(5) Uani d . . . 1.0 . .
H H46 0.949068 0.456658 0.835761 0.037 Uiso calc . . R 1.0 . .
C C47 0.70600(10) 0.3543(2) 0.76774(8) 0.0166(4) Uani d . . . 1.0 . .
H H47A 0.751445 0.36606 0.765763 0.02 Uiso calc . . R 1.0 . .
H H47B 0.676511 0.306823 0.734108 0.02 Uiso calc . . R 1.0 . .
C C48 0.67612(10) 0.4873(2) 0.76884(8) 0.0169(4) Uani d . . . 1.0 . .
C C49 0.61356(11) 0.5400(2) 0.74185(9) 0.0225(5) Uani d . . . 1.0 . .
H H49 0.57502 0.495524 0.716117 0.027 Uiso calc . . R 1.0 . .
C C50 0.61629(12) 0.6753(2) 0.75931(10) 0.0262(5) Uani d . . . 1.0 . .
H H50 0.580039 0.73823 0.747499 0.031 Uiso calc . . R 1.0 . .
C C51 0.68018(12) 0.6961(2) 0.79571(9) 0.0238(5) Uani d . . . 1.0 . .
H H51 0.696393 0.777794 0.814266 0.029 Uiso calc . . R 1.0 . .
C C52B 0.5449(10) 0.240(3) 0.7562(7) 0.02660(18) Uani d U P D 0.145(2) B 2
H H52D 0.510158 0.180376 0.759605 0.04 Uiso calc . P GR 0.145(2) B 2
H H52E 0.559409 0.207462 0.727282 0.04 Uiso calc . P GR 0.145(2) B 2
H H52F 0.52572 0.329801 0.746769 0.04 Uiso calc . P GR 0.145(2) B 2
Cl Cl2B 0.6017(2) 0.3939(5) 0.86468(17) 0.02660(18) Uani d U P D 0.145(2) B 2
C C26B 0.4484(10) 0.608(3) 0.7366(8) 0.02863(19) Uani d U P D 0.142(2) A 2
H H26D 0.460712 0.699082 0.749955 0.043 Uiso calc . P GR 0.142(2) A 2
H H26E 0.486201 0.567505 0.729215 0.043 Uiso calc . P GR 0.142(2) A 2
H H26F 0.439489 0.55556 0.764588 0.043 Uiso calc . P GR 0.142(2) A 2
Cl Cl1B 0.3657(2) 0.7534(5) 0.61096(18) 0.02863(19) Uani d U P D 0.142(2) A 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_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl1A 0.0190(3) 0.0359(4) 0.0282(4) 0.0020(3) 0.0059(3) -0.0025(3)
Al1 0.0185(3) 0.0229(3) 0.0224(3) -0.0041(3) 0.0126(3) -0.0035(3)
O1 0.0217(8) 0.0286(9) 0.0316(9) -0.0062(6) 0.0168(7) -0.0113(7)
O2 0.0216(8) 0.0225(8) 0.0278(8) 0.0008(6) 0.0101(7) -0.0039(7)
O3 0.0265(8) 0.0156(7) 0.0190(7) -0.0018(6) 0.0088(6) -0.0002(6)
N1A 0.0176(8) 0.0136(8) 0.0127(8) -0.0021(6) 0.0061(7) -0.0015(6)
C26A 0.0190(3) 0.0359(4) 0.0282(4) 0.0020(3) 0.0059(3) -0.0025(3)
C1 0.0182(10) 0.0182(10) 0.0161(10) 0.0000(8) 0.0077(8) 0.0004(8)
C2 0.0189(10) 0.0151(10) 0.0128(9) 0.0023(8) 0.0073(8) 0.0003(8)
C3 0.0189(10) 0.0151(10) 0.0164(10) 0.0005(8) 0.0082(8) -0.0008(8)
C4 0.0197(10) 0.0148(10) 0.0162(10) -0.0005(8) 0.0042(8) -0.0006(8)
C5 0.0266(11) 0.0154(10) 0.0137(10) 0.0022(8) 0.0075(8) -0.0017(8)
C6 0.0224(10) 0.0165(10) 0.0154(10) 0.0034(8) 0.0089(8) 0.0011(8)
C7 0.0172(9) 0.0140(10) 0.0158(9) -0.0017(8) 0.0092(8) -0.0001(8)
C8 0.0224(11) 0.0189(11) 0.0237(11) -0.0046(9) 0.0055(9) -0.0057(9)
C9 0.0249(12) 0.0385(15) 0.0359(14) -0.0063(11) -0.0003(10) 0.0036(12)
C10 0.0340(13) 0.0345(14) 0.0336(13) -0.0157(11) 0.0118(11) -0.0032(11)
C11 0.0363(14) 0.0344(15) 0.0591(18) -0.0133(12) 0.0170(13) -0.0256(14)
C12 0.0283(11) 0.0241(11) 0.0203(11) 0.0046(9) 0.0155(9) -0.0011(9)
C13 0.0452(15) 0.0319(14) 0.0316(13) 0.0012(11) 0.0280(12) 0.0008(11)
C14 0.0295(13) 0.0456(16) 0.0305(13) 0.0129(11) 0.0156(11) 0.0009(11)
C15 0.0449(15) 0.0300(13) 0.0293(13) 0.0036(11) 0.0239(11) -0.0064(10)
C16 0.0217(10) 0.0190(10) 0.0126(9) -0.0009(8) 0.0061(8) 0.0001(8)
C17 0.0210(10) 0.0174(10) 0.0177(10) 0.0018(8) 0.0056(8) 0.0016(8)
C18 0.0217(11) 0.0249(12) 0.0257(12) -0.0012(9) 0.0026(9) -0.0027(9)
C19 0.0170(10) 0.0310(13) 0.0365(13) 0.0000(9) 0.0060(10) 0.0060(11)
C20 0.0197(11) 0.0312(13) 0.0350(13) 0.0043(9) 0.0122(10) 0.0028(10)
C21 0.0199(10) 0.0159(10) 0.0141(9) -0.0010(8) 0.0081(8) -0.0012(8)
C22 0.0227(10) 0.0169(10) 0.0148(10) 0.0001(8) 0.0100(8) -0.0023(8)
C23 0.0222(11) 0.0235(12) 0.0234(11) -0.0045(9) 0.0086(9) -0.0037(9)
C24 0.0348(13) 0.0248(12) 0.0291(12) -0.0136(10) 0.0175(10) -0.0069(10)
C25 0.0402(13) 0.0174(11) 0.0242(11) -0.0066(10) 0.0163(10) -0.0001(9)
Cl2A 0.0200(3) 0.0334(4) 0.0221(4) -0.0059(3) 0.0033(2) -0.0007(3)
Al2 0.0161(3) 0.0195(3) 0.0194(3) 0.0003(2) 0.0085(2) 0.0019(2)
O4 0.0193(7) 0.0246(8) 0.0296(8) 0.0036(6) 0.0140(6) 0.0088(7)
O5 0.0230(7) 0.0175(7) 0.0187(7) -0.0019(6) 0.0069(6) -0.0015(6)
O6 0.0210(8) 0.0260(8) 0.0302(9) -0.0030(6) 0.0130(7) 0.0033(7)
N1B 0.0166(8) 0.0150(8) 0.0116(8) -0.0002(6) 0.0055(6) -0.0003(6)
C52A 0.0200(3) 0.0334(4) 0.0221(4) -0.0059(3) 0.0033(2) -0.0007(3)
C27 0.0169(9) 0.0158(10) 0.0168(10) -0.0012(8) 0.0068(8) -0.0015(8)
C28 0.0219(10) 0.0144(10) 0.0144(9) -0.0025(8) 0.0088(8) -0.0010(8)
C29 0.0182(10) 0.0174(10) 0.0146(9) -0.0015(8) 0.0072(8) -0.0017(8)
C30 0.0216(10) 0.0162(10) 0.0135(9) -0.0014(8) 0.0052(8) -0.0024(8)
C31 0.0257(11) 0.0148(10) 0.0143(10) -0.0026(8) 0.0074(8) 0.0008(8)
C32 0.0229(10) 0.0176(10) 0.0159(10) -0.0034(8) 0.0106(8) -0.0026(8)
C33 0.0200(10) 0.0154(10) 0.0145(9) 0.0003(8) 0.0082(8) -0.0011(8)
C34 0.0226(11) 0.0210(11) 0.0186(10) 0.0028(9) 0.0046(9) 0.0020(8)
C35 0.0270(13) 0.0334(14) 0.0398(15) 0.0021(11) -0.0059(11) -0.0040(12)
C36 0.0315(13) 0.0352(14) 0.0291(13) 0.0145(11) 0.0121(10) 0.0064(11)
C37 0.0390(14) 0.0262(13) 0.0393(14) 0.0092(11) 0.0169(12) 0.0124(11)
C38 0.0278(11) 0.0216(11) 0.0224(11) -0.0035(9) 0.0148(9) 0.0014(9)
C39 0.0352(13) 0.0296(13) 0.0303(12) -0.0007(10) 0.0215(11) -0.0005(10)
C40 0.0282(12) 0.0366(14) 0.0331(13) -0.0102(10) 0.0161(11) -0.0005(11)
C41 0.0417(14) 0.0293(13) 0.0352(13) -0.0006(11) 0.0264(12) 0.0088(11)
C42 0.0167(9) 0.0196(10) 0.0123(9) -0.0017(8) 0.0059(8) -0.0020(8)
C43 0.0215(10) 0.0209(11) 0.0168(10) -0.0031(8) 0.0078(8) -0.0027(8)
C44 0.0216(11) 0.0371(14) 0.0240(12) 0.0000(10) 0.0057(9) 0.0015(10)
C45 0.0177(11) 0.0483(16) 0.0384(14) -0.0008(11) 0.0102(10) -0.0059(12)
C46 0.0201(11) 0.0386(14) 0.0394(14) -0.0084(10) 0.0174(10) -0.0068(11)
C47 0.0200(10) 0.0181(10) 0.0130(9) -0.0008(8) 0.0079(8) 0.0011(8)
C48 0.0227(10) 0.0162(10) 0.0130(9) -0.0039(8) 0.0083(8) -0.0013(8)
C49 0.0230(11) 0.0222(11) 0.0215(11) 0.0006(9) 0.0078(9) 0.0025(9)
C50 0.0298(12) 0.0221(12) 0.0295(12) 0.0062(9) 0.0144(10) 0.0051(9)
C51 0.0352(12) 0.0159(11) 0.0245(11) 0.0024(9) 0.0161(10) 0.0002(9)
C52B 0.0200(3) 0.0334(4) 0.0221(4) -0.0059(3) 0.0033(2) -0.0007(3)
Cl2B 0.0200(3) 0.0334(4) 0.0221(4) -0.0059(3) 0.0033(2) -0.0007(3)
C26B 0.0190(3) 0.0359(4) 0.0282(4) 0.0020(3) 0.0059(3) -0.0025(3)
Cl1B 0.0190(3) 0.0359(4) 0.0282(4) 0.0020(3) 0.0059(3) -0.0025(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cl1A Al1 . 2.1386(10) ?
Al1 O1 . 1.7304(17) ?
Al1 N1A . 2.0042(18) ?
Al1 C26A . 1.961(4) ?
Al1 C26B . 1.978(15) ?
Al1 Cl1B . 2.081(5) ?
O1 C1 . 1.348(2) ?
O2 C17 . 1.375(3) ?
O2 C20 . 1.370(3) ?
O3 C22 . 1.377(3) ?
O3 C25 . 1.369(3) ?
N1A C7 . 1.509(2) ?
N1A C16 . 1.514(2) ?
N1A C21 . 1.514(2) ?
C26A H26A . 0.98 ?
C26A H26B . 0.98 ?
C26A H26C . 0.98 ?
C1 C2 . 1.405(3) ?
C1 C6 . 1.407(3) ?
C2 C3 . 1.388(3) ?
C2 C7 . 1.513(3) ?
C3 H3 . 0.95 ?
C3 C4 . 1.395(3) ?
C4 C5 . 1.396(3) ?
C4 C8 . 1.534(3) ?
C5 H5 . 0.95 ?
C5 C6 . 1.395(3) ?
C6 C12 . 1.539(3) ?
C7 H7A . 0.99 ?
C7 H7B . 0.99 ?
C8 C9 . 1.530(3) ?
C8 C10 . 1.532(3) ?
C8 C11 . 1.526(3) ?
C9 H9A . 0.98 ?
C9 H9B . 0.98 ?
C9 H9C . 0.98 ?
C10 H10A . 0.98 ?
C10 H10B . 0.98 ?
C10 H10C . 0.98 ?
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 C13 . 1.538(3) ?
C12 C14 . 1.539(3) ?
C12 C15 . 1.534(3) ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
C14 H14A . 0.98 ?
C14 H14B . 0.98 ?
C14 H14C . 0.98 ?
C15 H15A . 0.98 ?
C15 H15B . 0.98 ?
C15 H15C . 0.98 ?
C16 H16A . 0.99 ?
C16 H16B . 0.99 ?
C16 C17 . 1.487(3) ?
C17 C18 . 1.349(3) ?
C18 H18 . 0.95 ?
C18 C19 . 1.428(3) ?
C19 H19 . 0.95 ?
C19 C20 . 1.338(4) ?
C20 H20 . 0.95 ?
C21 H21A . 0.99 ?
C21 H21B . 0.99 ?
C21 C22 . 1.490(3) ?
C22 C23 . 1.350(3) ?
C23 H23 . 0.95 ?
C23 C24 . 1.429(3) ?
C24 H24 . 0.95 ?
C24 C25 . 1.345(3) ?
C25 H25 . 0.95 ?
Cl2A Al2 . 2.1379(10) ?
Al2 O4 . 1.7351(16) ?
Al2 N1B . 2.0086(18) ?
Al2 C52A . 2.021(4) ?
Al2 C52B . 1.987(14) ?
Al2 Cl2B . 1.948(5) ?
O4 C27 . 1.348(2) ?
O5 C48 . 1.383(2) ?
O5 C51 . 1.369(3) ?
O6 C43 . 1.376(3) ?
O6 C46 . 1.370(3) ?
N1B C33 . 1.513(3) ?
N1B C42 . 1.511(2) ?
N1B C47 . 1.511(2) ?
C52A H52A . 0.98 ?
C52A H52B . 0.98 ?
C52A H52C . 0.98 ?
C27 C28 . 1.408(3) ?
C27 C32 . 1.408(3) ?
C28 C29 . 1.388(3) ?
C28 C33 . 1.510(3) ?
C29 H29 . 0.95 ?
C29 C30 . 1.396(3) ?
C30 C31 . 1.398(3) ?
C30 C34 . 1.530(3) ?
C31 H31 . 0.95 ?
C31 C32 . 1.397(3) ?
C32 C38 . 1.538(3) ?
C33 H33A . 0.99 ?
C33 H33B . 0.99 ?
C34 C35 . 1.532(3) ?
C34 C36 . 1.533(3) ?
C34 C37 . 1.535(3) ?
C35 H35A . 0.98 ?
C35 H35B . 0.98 ?
C35 H35C . 0.98 ?
C36 H36A . 0.98 ?
C36 H36B . 0.98 ?
C36 H36C . 0.98 ?
C37 H37A . 0.98 ?
C37 H37B . 0.98 ?
C37 H37C . 0.98 ?
C38 C39 . 1.540(3) ?
C38 C40 . 1.541(3) ?
C38 C41 . 1.538(3) ?
C39 H39A . 0.98 ?
C39 H39B . 0.98 ?
C39 H39C . 0.98 ?
C40 H40A . 0.98 ?
C40 H40B . 0.98 ?
C40 H40C . 0.98 ?
C41 H41A . 0.98 ?
C41 H41B . 0.98 ?
C41 H41C . 0.98 ?
C42 H42A . 0.99 ?
C42 H42B . 0.99 ?
C42 C43 . 1.484(3) ?
C43 C44 . 1.351(3) ?
C44 H44 . 0.95 ?
C44 C45 . 1.431(3) ?
C45 H45 . 0.95 ?
C45 C46 . 1.339(4) ?
C46 H46 . 0.95 ?
C47 H47A . 0.99 ?
C47 H47B . 0.99 ?
C47 C48 . 1.484(3) ?
C48 C49 . 1.349(3) ?
C49 H49 . 0.95 ?
C49 C50 . 1.430(3) ?
C50 H50 . 0.95 ?
C50 C51 . 1.343(3) ?
C51 H51 . 0.95 ?
C52B H52D . 0.98 ?
C52B H52E . 0.98 ?
C52B H52F . 0.98 ?
C26B H26D . 0.98 ?
C26B H26E . 0.98 ?
C26B H26F . 0.98 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Al1 Cl1A . . 107.36(7) ?
O1 Al1 N1A . . 98.29(7) ?
O1 Al1 C26A . . 116.19(12) ?
O1 Al1 C26B . . 112.8(9) ?
O1 Al1 Cl1B . . 108.94(14) ?
N1A Al1 Cl1A . . 105.25(6) ?
N1A Al1 Cl1B . . 106.77(13) ?
C26A Al1 Cl1A . . 115.35(11) ?
C26A Al1 N1A . . 112.59(11) ?
C26B Al1 N1A . . 113.5(8) ?
C26B Al1 Cl1B . . 115.1(8) ?
C1 O1 Al1 . . 131.46(13) ?
C20 O2 C17 . . 106.49(17) ?
C25 O3 C22 . . 106.17(17) ?
C7 N1A Al1 . . 105.32(12) ?
C7 N1A C16 . . 110.02(15) ?
C7 N1A C21 . . 107.64(14) ?
C16 N1A Al1 . . 111.20(12) ?
C21 N1A Al1 . . 111.22(12) ?
C21 N1A C16 . . 111.21(15) ?
Al1 C26A H26A . . 109.5 ?
Al1 C26A H26B . . 109.5 ?
Al1 C26A H26C . . 109.5 ?
H26A C26A H26B . . 109.5 ?
H26A C26A H26C . . 109.5 ?
H26B C26A H26C . . 109.5 ?
O1 C1 C2 . . 119.21(18) ?
O1 C1 C6 . . 121.03(18) ?
C2 C1 C6 . . 119.75(18) ?
C1 C2 C7 . . 120.32(18) ?
C3 C2 C1 . . 120.39(18) ?
C3 C2 C7 . . 119.20(17) ?
C2 C3 H3 . . 119.4 ?
C2 C3 C4 . . 121.29(19) ?
C4 C3 H3 . . 119.4 ?
C3 C4 C5 . . 117.12(19) ?
C3 C4 C8 . . 120.86(19) ?
C5 C4 C8 . . 121.93(18) ?
C4 C5 H5 . . 118.2 ?
C6 C5 C4 . . 123.69(19) ?
C6 C5 H5 . . 118.2 ?
C1 C6 C12 . . 120.91(19) ?
C5 C6 C1 . . 117.66(18) ?
C5 C6 C12 . . 121.43(18) ?
N1A C7 C2 . . 114.18(15) ?
N1A C7 H7A . . 108.7 ?
N1A C7 H7B . . 108.7 ?
C2 C7 H7A . . 108.7 ?
C2 C7 H7B . . 108.7 ?
H7A C7 H7B . . 107.6 ?
C9 C8 C4 . . 108.19(18) ?
C9 C8 C10 . . 108.5(2) ?
C10 C8 C4 . . 110.75(18) ?
C11 C8 C4 . . 111.67(19) ?
C11 C8 C9 . . 110.2(2) ?
C11 C8 C10 . . 107.4(2) ?
C8 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
C8 C9 H9C . . 109.5 ?
H9A C9 H9B . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C8 C10 H10A . . 109.5 ?
C8 C10 H10B . . 109.5 ?
C8 C10 H10C . . 109.5 ?
H10A C10 H10B . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C8 C11 H11A . . 109.5 ?
C8 C11 H11B . . 109.5 ?
C8 C11 H11C . . 109.5 ?
H11A C11 H11B . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C6 C12 C14 . . 109.83(17) ?
C13 C12 C6 . . 110.20(18) ?
C13 C12 C14 . . 110.1(2) ?
C15 C12 C6 . . 111.76(19) ?
C15 C12 C13 . . 107.87(18) ?
C15 C12 C14 . . 107.02(19) ?
C12 C13 H13A . . 109.5 ?
C12 C13 H13B . . 109.5 ?
C12 C13 H13C . . 109.5 ?
H13A C13 H13B . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
C12 C14 H14A . . 109.5 ?
C12 C14 H14B . . 109.5 ?
C12 C14 H14C . . 109.5 ?
H14A C14 H14B . . 109.5 ?
H14A C14 H14C . . 109.5 ?
H14B C14 H14C . . 109.5 ?
C12 C15 H15A . . 109.5 ?
C12 C15 H15B . . 109.5 ?
C12 C15 H15C . . 109.5 ?
H15A C15 H15B . . 109.5 ?
H15A C15 H15C . . 109.5 ?
H15B C15 H15C . . 109.5 ?
N1A C16 H16A . . 108.3 ?
N1A C16 H16B . . 108.3 ?
H16A C16 H16B . . 107.4 ?
C17 C16 N1A . . 115.93(16) ?
C17 C16 H16A . . 108.3 ?
C17 C16 H16B . . 108.3 ?
O2 C17 C16 . . 117.82(18) ?
C18 C17 O2 . . 109.72(19) ?
C18 C17 C16 . . 132.4(2) ?
C17 C18 H18 . . 126.6 ?
C17 C18 C19 . . 106.7(2) ?
C19 C18 H18 . . 126.6 ?
C18 C19 H19 . . 126.7 ?
C20 C19 C18 . . 106.6(2) ?
C20 C19 H19 . . 126.7 ?
O2 C20 H20 . . 124.8 ?
C19 C20 O2 . . 110.5(2) ?
C19 C20 H20 . . 124.8 ?
N1A C21 H21A . . 108.9 ?
N1A C21 H21B . . 108.9 ?
H21A C21 H21B . . 107.7 ?
C22 C21 N1A . . 113.57(16) ?
C22 C21 H21A . . 108.9 ?
C22 C21 H21B . . 108.9 ?
O3 C22 C21 . . 117.16(17) ?
C23 C22 O3 . . 110.14(19) ?
C23 C22 C21 . . 132.7(2) ?
C22 C23 H23 . . 126.7 ?
C22 C23 C24 . . 106.5(2) ?
C24 C23 H23 . . 126.7 ?
C23 C24 H24 . . 126.7 ?
C25 C24 C23 . . 106.5(2) ?
C25 C24 H24 . . 126.7 ?
O3 C25 H25 . . 124.7 ?
C24 C25 O3 . . 110.6(2) ?
C24 C25 H25 . . 124.7 ?
O4 Al2 Cl2A . . 107.48(7) ?
O4 Al2 N1B . . 98.01(7) ?
O4 Al2 C52A . . 110.57(12) ?
O4 Al2 C52B . . 113.4(8) ?
O4 Al2 Cl2B . . 117.16(15) ?
N1B Al2 Cl2A . . 104.91(6) ?
N1B Al2 C52A . . 109.33(11) ?
C52A Al2 Cl2A . . 123.45(11) ?
C52B Al2 N1B . . 112.7(7) ?
Cl2B Al2 N1B . . 114.01(15) ?
Cl2B Al2 C52B . . 102.2(8) ?
C27 O4 Al2 . . 132.16(13) ?
C51 O5 C48 . . 106.46(16) ?
C46 O6 C43 . . 106.33(18) ?
C33 N1B Al2 . . 105.48(12) ?
C42 N1B Al2 . . 110.16(12) ?
C42 N1B C33 . . 109.85(15) ?
C42 N1B C47 . . 111.48(15) ?
C47 N1B Al2 . . 112.21(12) ?
C47 N1B C33 . . 107.43(14) ?
Al2 C52A H52A . . 109.5 ?
Al2 C52A H52B . . 109.5 ?
Al2 C52A H52C . . 109.5 ?
H52A C52A H52B . . 109.5 ?
H52A C52A H52C . . 109.5 ?
H52B C52A H52C . . 109.5 ?
O4 C27 C28 . . 119.24(18) ?
O4 C27 C32 . . 120.93(18) ?
C32 C27 C28 . . 119.83(18) ?
C27 C28 C33 . . 120.58(18) ?
C29 C28 C27 . . 120.04(18) ?
C29 C28 C33 . . 119.26(18) ?
C28 C29 H29 . . 119.1 ?
C28 C29 C30 . . 121.78(19) ?
C30 C29 H29 . . 119.1 ?
C29 C30 C31 . . 116.85(19) ?
C29 C30 C34 . . 120.70(18) ?
C31 C30 C34 . . 122.44(18) ?
C30 C31 H31 . . 118.2 ?
C32 C31 C30 . . 123.69(19) ?
C32 C31 H31 . . 118.2 ?
C27 C32 C38 . . 120.98(18) ?
C31 C32 C27 . . 117.69(18) ?
C31 C32 C38 . . 121.32(19) ?
N1B C33 H33A . . 108.6 ?
N1B C33 H33B . . 108.6 ?
C28 C33 N1B . . 114.55(16) ?
C28 C33 H33A . . 108.6 ?
C28 C33 H33B . . 108.6 ?
H33A C33 H33B . . 107.6 ?
C30 C34 C35 . . 108.80(19) ?
C30 C34 C36 . . 110.63(17) ?
C30 C34 C37 . . 112.46(19) ?
C35 C34 C36 . . 108.7(2) ?
C35 C34 C37 . . 109.0(2) ?
C36 C34 C37 . . 107.2(2) ?
C34 C35 H35A . . 109.5 ?
C34 C35 H35B . . 109.5 ?
C34 C35 H35C . . 109.5 ?
H35A C35 H35B . . 109.5 ?
H35A C35 H35C . . 109.5 ?
H35B C35 H35C . . 109.5 ?
C34 C36 H36A . . 109.5 ?
C34 C36 H36B . . 109.5 ?
C34 C36 H36C . . 109.5 ?
H36A C36 H36B . . 109.5 ?
H36A C36 H36C . . 109.5 ?
H36B C36 H36C . . 109.5 ?
C34 C37 H37A . . 109.5 ?
C34 C37 H37B . . 109.5 ?
C34 C37 H37C . . 109.5 ?
H37A C37 H37B . . 109.5 ?
H37A C37 H37C . . 109.5 ?
H37B C37 H37C . . 109.5 ?
C32 C38 C39 . . 110.22(18) ?
C32 C38 C40 . . 109.71(18) ?
C39 C38 C40 . . 110.2(2) ?
C41 C38 C32 . . 112.01(18) ?
C41 C38 C39 . . 107.38(18) ?
C41 C38 C40 . . 107.23(19) ?
C38 C39 H39A . . 109.5 ?
C38 C39 H39B . . 109.5 ?
C38 C39 H39C . . 109.5 ?
H39A C39 H39B . . 109.5 ?
H39A C39 H39C . . 109.5 ?
H39B C39 H39C . . 109.5 ?
C38 C40 H40A . . 109.5 ?
C38 C40 H40B . . 109.5 ?
C38 C40 H40C . . 109.5 ?
H40A C40 H40B . . 109.5 ?
H40A C40 H40C . . 109.5 ?
H40B C40 H40C . . 109.5 ?
C38 C41 H41A . . 109.5 ?
C38 C41 H41B . . 109.5 ?
C38 C41 H41C . . 109.5 ?
H41A C41 H41B . . 109.5 ?
H41A C41 H41C . . 109.5 ?
H41B C41 H41C . . 109.5 ?
N1B C42 H42A . . 108.2 ?
N1B C42 H42B . . 108.2 ?
H42A C42 H42B . . 107.4 ?
C43 C42 N1B . . 116.34(16) ?
C43 C42 H42A . . 108.2 ?
C43 C42 H42B . . 108.2 ?
O6 C43 C42 . . 118.25(18) ?
C44 C43 O6 . . 109.89(19) ?
C44 C43 C42 . . 131.7(2) ?
C43 C44 H44 . . 126.7 ?
C43 C44 C45 . . 106.5(2) ?
C45 C44 H44 . . 126.7 ?
C44 C45 H45 . . 126.7 ?
C46 C45 C44 . . 106.6(2) ?
C46 C45 H45 . . 126.7 ?
O6 C46 H46 . . 124.7 ?
C45 C46 O6 . . 110.6(2) ?
C45 C46 H46 . . 124.7 ?
N1B C47 H47A . . 108.9 ?
N1B C47 H47B . . 108.9 ?
H47A C47 H47B . . 107.7 ?
C48 C47 N1B . . 113.48(16) ?
C48 C47 H47A . . 108.9 ?
C48 C47 H47B . . 108.9 ?
O5 C48 C47 . . 117.43(17) ?
C49 C48 O5 . . 109.49(18) ?
C49 C48 C47 . . 133.06(19) ?
C48 C49 H49 . . 126.5 ?
C48 C49 C50 . . 107.0(2) ?
C50 C49 H49 . . 126.5 ?
C49 C50 H50 . . 126.8 ?
C51 C50 C49 . . 106.5(2) ?
C51 C50 H50 . . 126.8 ?
O5 C51 H51 . . 124.7 ?
C50 C51 O5 . . 110.6(2) ?
C50 C51 H51 . . 124.7 ?
Al2 C52B H52D . . 109.5 ?
Al2 C52B H52E . . 109.5 ?
Al2 C52B H52F . . 109.5 ?
H52D C52B H52E . . 109.5 ?
H52D C52B H52F . . 109.5 ?
H52E C52B H52F . . 109.5 ?
Al1 C26B H26D . . 109.5 ?
Al1 C26B H26E . . 109.5 ?
Al1 C26B H26F . . 109.5 ?
H26D C26B H26E . . 109.5 ?
H26D C26B H26F . . 109.5 ?
H26E C26B H26F . . 109.5 ?
_shelx_res_file
;
TITL mo_kpjk6001301_AlMeCltBu_0m_a.res in P2(1)/n
mo_kpjk6001301_almecltbu_0m_a.res
created by SHELXL-2016/6 at 17:40:48 on 22-Jul-2017
REM Old TITL mo_kpjk6001301_AlMeCltBu_0m in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.140, Rweak 0.007, Alpha 0.031, Orientation as input
REM Formula found by SHELXT: C51 Al2 Cl2 N3 O6
CELL 0.71073 21.164 10.0463 26.3318 90 112.398 90
ZERR 8 0.0026 0.0013 0.0032 0 0.004 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Al Cl N O
UNIT 208 280 8 8 8 24
SADI Al2 C52A Al2 C52B
SADI Cl2A Al2 Cl2B Al2
SADI Al2 C52A Al1 C26B Al1 C26A
SADI Cl2A Al2 Cl1A Al1 Cl1B Al1
SIMU Cl2A Al2 C52A
SIMU Al2 C52B Cl2B
SIMU Cl1A Al1 C26A
SIMU Al1 C26B Cl1B
RIGU 0.001 0.001 Cl2A Al2 C52A
RIGU 0.001 0.001 Al2 C52B Cl2B
RIGU 0.001 0.001 Cl1A Al1 C26A
RIGU 0.001 0.001 Al1 C26B Cl1B
EADP C26B Cl1A C26A Cl1B
EADP Cl2B C52A C52B Cl2A
L.S. 8
PLAN 10
TEMP -140.15
BOND $H
LIST 4
fmap 2
acta
REM
REM
REM
WGHT 0.049500 6.355801
FVAR 0.33047 0.85546 0.85808
PART 1
CL1A 4 0.443260 0.580869 0.747994 31.00000 0.01904 0.03586 =
0.02822 -0.00246 0.00590 0.00201
PART 0
AL1 3 0.365499 0.610965 0.668274 11.00000 0.01847 0.02291 =
0.02243 -0.00349 0.01257 -0.00410
O1 6 0.346867 0.457244 0.636352 11.00000 0.02165 0.02864 =
0.03161 -0.01128 0.01677 -0.00625
O2 6 0.140918 0.789030 0.665851 11.00000 0.02160 0.02250 =
0.02777 -0.00394 0.01009 0.00085
O3 6 0.276911 0.950471 0.694890 11.00000 0.02645 0.01556 =
0.01900 -0.00017 0.00876 -0.00181
N1A 5 0.278912 0.636796 0.681203 11.00000 0.01755 0.01362 =
0.01268 -0.00155 0.00609 -0.00208
PART 1
C26A 1 0.382698 0.756005 0.625372 31.00000 0.01904 0.03586 =
0.02822 -0.00246 0.00590 0.00201
AFIX 137
H26A 2 0.420462 0.811162 0.649379 31.00000 -1.50000
H26B 2 0.341477 0.810718 0.609421 31.00000 -1.50000
H26C 2 0.394751 0.718620 0.595875 31.00000 -1.50000
AFIX 0
PART 0
C1 1 0.290482 0.380435 0.621789 11.00000 0.01824 0.01819 =
0.01607 0.00040 0.00771 0.00004
C2 1 0.243345 0.401965 0.646763 11.00000 0.01894 0.01510 =
0.01279 0.00032 0.00727 0.00226
C3 1 0.183308 0.328592 0.630672 11.00000 0.01889 0.01506 =
0.01638 -0.00079 0.00817 0.00047
AFIX 43
H3 2 0.151356 0.346126 0.647213 11.00000 -1.20000
AFIX 0
C4 1 0.168980 0.229610 0.590683 11.00000 0.01974 0.01477 =
0.01621 -0.00059 0.00416 -0.00053
C5 1 0.217749 0.207230 0.567860 11.00000 0.02656 0.01537 =
0.01369 -0.00167 0.00746 0.00216
AFIX 43
H5 2 0.208947 0.139596 0.540813 11.00000 -1.20000
AFIX 0
C6 1 0.278651 0.278580 0.582537 11.00000 0.02236 0.01654 =
0.01535 0.00109 0.00891 0.00344
C7 1 0.259285 0.499896 0.693662 11.00000 0.01719 0.01404 =
0.01579 -0.00015 0.00918 -0.00166
AFIX 23
H7A 2 0.218729 0.507918 0.703510 11.00000 -1.20000
H7B 2 0.297178 0.463871 0.726045 11.00000 -1.20000
AFIX 0
C8 1 0.100690 0.154595 0.570819 11.00000 0.02237 0.01891 =
0.02373 -0.00569 0.00554 -0.00459
C9 1 0.045840 0.245021 0.531125 11.00000 0.02490 0.03854 =
0.03593 0.00360 -0.00033 -0.00630
AFIX 137
H9A 2 0.044499 0.329274 0.549445 11.00000 -1.50000
H9B 2 0.001219 0.201138 0.519778 11.00000 -1.50000
H9C 2 0.056668 0.262573 0.498727 11.00000 -1.50000
AFIX 0
C10 1 0.080157 0.120759 0.619169 11.00000 0.03397 0.03454 =
0.03365 -0.00316 0.01180 -0.01572
AFIX 137
H10A 2 0.115894 0.066211 0.645823 11.00000 -1.50000
H10B 2 0.037005 0.071248 0.605746 11.00000 -1.50000
H10C 2 0.074437 0.203174 0.636869 11.00000 -1.50000
AFIX 0
C11 1 0.104627 0.023945 0.542588 11.00000 0.03632 0.03445 =
0.05911 -0.02563 0.01695 -0.01326
AFIX 137
H11A 2 0.110880 0.042899 0.508292 11.00000 -1.50000
H11B 2 0.062193 -0.026268 0.534470 11.00000 -1.50000
H11C 2 0.143335 -0.028683 0.566875 11.00000 -1.50000
AFIX 0
C12 1 0.331645 0.246504 0.557373 11.00000 0.02829 0.02412 =
0.02029 -0.00110 0.01546 0.00464
C13 1 0.341506 0.367283 0.525275 11.00000 0.04519 0.03188 =
0.03156 0.00085 0.02800 0.00116
AFIX 137
H13A 2 0.298663 0.386001 0.494251 11.00000 -1.50000
H13B 2 0.377529 0.347853 0.511536 11.00000 -1.50000
H13C 2 0.354612 0.444968 0.549582 11.00000 -1.50000
AFIX 0
C14 1 0.400102 0.208060 0.603090 11.00000 0.02950 0.04562 =
0.03051 0.00088 0.01563 0.01294
AFIX 137
H14A 2 0.417385 0.283294 0.628290 11.00000 -1.50000
H14B 2 0.433248 0.185186 0.586740 11.00000 -1.50000
H14C 2 0.393268 0.131217 0.623354 11.00000 -1.50000
AFIX 0
C15 1 0.309332 0.128260 0.517615 11.00000 0.04491 0.02996 =
0.02934 -0.00640 0.02393 0.00364
AFIX 137
H15A 2 0.304650 0.048831 0.537504 11.00000 -1.50000
H15B 2 0.343748 0.111967 0.501841 11.00000 -1.50000
H15C 2 0.265344 0.148444 0.488101 11.00000 -1.50000
AFIX 0
C16 1 0.222801 0.693068 0.630754 11.00000 0.02172 0.01903 =
0.01260 0.00006 0.00608 -0.00085
AFIX 23
H16A 2 0.235590 0.784966 0.624980 11.00000 -1.20000
H16B 2 0.220677 0.639709 0.598535 11.00000 -1.20000
AFIX 0
C17 1 0.153353 0.696464 0.632345 11.00000 0.02104 0.01741 =
0.01773 0.00161 0.00560 0.00181
C18 1 0.095637 0.627819 0.604647 11.00000 0.02174 0.02490 =
0.02572 -0.00267 0.00257 -0.00117
AFIX 43
H18 2 0.090388 0.558363 0.578869 11.00000 -1.20000
AFIX 0
C19 1 0.043958 0.679827 0.621597 11.00000 0.01702 0.03099 =
0.03649 0.00600 0.00602 0.00005
AFIX 43
H19 2 -0.002344 0.651798 0.609252 11.00000 -1.20000
AFIX 0
C20 1 0.073481 0.775725 0.658254 11.00000 0.01968 0.03121 =
0.03495 0.00275 0.01223 0.00426
AFIX 43
H20 2 0.050860 0.827331 0.676453 11.00000 -1.20000
AFIX 0
C21 1 0.290742 0.723298 0.731063 11.00000 0.01985 0.01587 =
0.01411 -0.00122 0.00807 -0.00102
AFIX 23
H21A 2 0.246659 0.736414 0.735322 11.00000 -1.20000
H21B 2 0.321879 0.676139 0.764146 11.00000 -1.20000
AFIX 0
C22 1 0.320470 0.855983 0.727958 11.00000 0.02273 0.01691 =
0.01477 -0.00231 0.01002 0.00005
C23 1 0.383886 0.907211 0.752587 11.00000 0.02216 0.02353 =
0.02341 -0.00375 0.00862 -0.00447
AFIX 43
H23 2 0.423107 0.862567 0.777329 11.00000 -1.20000
AFIX 0
C24 1 0.380407 1.041758 0.734124 11.00000 0.03476 0.02475 =
0.02909 -0.00690 0.01750 -0.01360
AFIX 43
H24 2 0.416846 1.104186 0.744239 11.00000 -1.20000
AFIX 0
C25 1 0.315408 1.062694 0.699607 11.00000 0.04016 0.01739 =
0.02421 -0.00010 0.01633 -0.00657
AFIX 43
H25 2 0.298554 1.144144 0.681064 11.00000 -1.20000
AFIX 0
PART 1
CL2A 4 0.550832 0.211129 0.746259 21.00000 0.02000 0.03344 =
0.02212 -0.00072 0.00327 -0.00586
PART 0
AL2 3 0.624925 0.246122 0.827105 11.00000 0.01610 0.01953 =
0.01936 0.00191 0.00846 0.00027
O4 6 0.642707 0.094197 0.860972 11.00000 0.01927 0.02455 =
0.02955 0.00876 0.01395 0.00360
O5 6 0.718722 0.583185 0.802379 11.00000 0.02302 0.01754 =
0.01872 -0.00145 0.00690 -0.00187
O6 6 0.855015 0.418765 0.839329 11.00000 0.02099 0.02598 =
0.03019 0.00328 0.01298 -0.00299
N1B 5 0.713772 0.269492 0.817165 11.00000 0.01665 0.01503 =
0.01161 -0.00027 0.00550 -0.00020
PART 1
C52A 1 0.615558 0.390417 0.877240 21.00000 0.02000 0.03344 =
0.02212 -0.00072 0.00327 -0.00586
AFIX 137
H52A 2 0.609238 0.476584 0.858502 21.00000 -1.50000
H52B 2 0.656958 0.393149 0.910837 21.00000 -1.50000
H52C 2 0.575936 0.371502 0.886695 21.00000 -1.50000
AFIX 0
PART 0
C27 1 0.697836 0.013831 0.875962 11.00000 0.01686 0.01578 =
0.01676 -0.00148 0.00685 -0.00125
C28 1 0.747225 0.034185 0.852972 11.00000 0.02187 0.01438 =
0.01438 -0.00099 0.00880 -0.00247
C29 1 0.806600 -0.041324 0.870764 11.00000 0.01820 0.01739 =
0.01461 -0.00173 0.00721 -0.00147
AFIX 43
H29 2 0.840235 -0.024245 0.855876 11.00000 -1.20000
AFIX 0
C30 1 0.818242 -0.141704 0.909949 11.00000 0.02162 0.01625 =
0.01351 -0.00239 0.00521 -0.00139
C31 1 0.766911 -0.163595 0.930202 11.00000 0.02568 0.01483 =
0.01428 0.00084 0.00738 -0.00265
AFIX 43
H31 2 0.773364 -0.232896 0.956252 11.00000 -1.20000
AFIX 0
C32 1 0.706655 -0.089281 0.914284 11.00000 0.02286 0.01764 =
0.01593 -0.00263 0.01060 -0.00344
C33 1 0.734237 0.131346 0.806309 11.00000 0.01996 0.01538 =
0.01452 -0.00112 0.00824 0.00029
AFIX 23
H33A 2 0.697622 0.095163 0.773126 11.00000 -1.20000
H33B 2 0.776181 0.138363 0.798300 11.00000 -1.20000
AFIX 0
C34 1 0.885071 -0.220728 0.930084 11.00000 0.02257 0.02102 =
0.01860 0.00200 0.00457 0.00283
C35 1 0.941955 -0.133542 0.969639 11.00000 0.02703 0.03340 =
0.03978 -0.00400 -0.00589 0.00212
AFIX 137
H35A 2 0.946638 -0.052580 0.950608 11.00000 -1.50000
H35B 2 0.985151 -0.182898 0.982466 11.00000 -1.50000
H35C 2 0.930472 -0.109363 1.001155 11.00000 -1.50000
AFIX 0
C36 1 0.904647 -0.259979 0.881724 11.00000 0.03149 0.03520 =
0.02908 0.00641 0.01214 0.01447
AFIX 137
H36A 2 0.866908 -0.309378 0.854564 11.00000 -1.50000
H36B 2 0.945601 -0.316097 0.895021 11.00000 -1.50000
H36C 2 0.913946 -0.179551 0.864678 11.00000 -1.50000
AFIX 0
C37 1 0.880202 -0.349682 0.959615 11.00000 0.03903 0.02615 =
0.03927 0.01239 0.01695 0.00923
AFIX 137
H37A 2 0.872053 -0.327913 0.992889 11.00000 -1.50000
H37B 2 0.923068 -0.399469 0.969638 11.00000 -1.50000
H37C 2 0.842374 -0.404020 0.935177 11.00000 -1.50000
AFIX 0
C38 1 0.650983 -0.120880 0.936653 11.00000 0.02784 0.02161 =
0.02236 0.00139 0.01480 -0.00355
C39 1 0.641476 -0.002275 0.970116 11.00000 0.03523 0.02956 =
0.03032 -0.00053 0.02147 -0.00072
AFIX 137
H39A 2 0.683773 0.012283 1.002211 11.00000 -1.50000
H39B 2 0.604070 -0.021438 0.982304 11.00000 -1.50000
H39C 2 0.630537 0.077802 0.947128 11.00000 -1.50000
AFIX 0
C40 1 0.583216 -0.152517 0.888607 11.00000 0.02824 0.03659 =
0.03307 -0.00048 0.01608 -0.01022
AFIX 137
H40A 2 0.569864 -0.076528 0.863396 11.00000 -1.50000
H40B 2 0.547520 -0.169822 0.902932 11.00000 -1.50000
H40C 2 0.589178 -0.231315 0.868946 11.00000 -1.50000
AFIX 0
C41 1 0.669352 -0.242898 0.974790 11.00000 0.04172 0.02927 =
0.03521 0.00877 0.02645 -0.00065
AFIX 137
H41A 2 0.673392 -0.321424 0.954151 11.00000 -1.50000
H41B 2 0.633426 -0.257917 0.989076 11.00000 -1.50000
H41C 2 0.712946 -0.227115 1.005445 11.00000 -1.50000
AFIX 0
C42 1 0.767446 0.325234 0.868972 11.00000 0.01672 0.01960 =
0.01235 -0.00201 0.00591 -0.00168
AFIX 23
H42A 2 0.754310 0.417492 0.873852 11.00000 -1.20000
H42B 2 0.766770 0.272431 0.900505 11.00000 -1.20000
AFIX 0
C43 1 0.838579 0.327307 0.871242 11.00000 0.02145 0.02091 =
0.01676 -0.00269 0.00779 -0.00307
C44 1 0.895048 0.259236 0.902572 11.00000 0.02160 0.03711 =
0.02404 0.00149 0.00569 0.00000
AFIX 43
H44 2 0.897533 0.190085 0.927872 11.00000 -1.20000
AFIX 0
C45 1 0.950367 0.311718 0.890174 11.00000 0.01771 0.04834 =
0.03840 -0.00594 0.01022 -0.00085
AFIX 43
H45 2 0.996893 0.285012 0.905984 11.00000 -1.20000
AFIX 0
C46 1 0.923754 0.405851 0.851925 11.00000 0.02008 0.03859 =
0.03937 -0.00680 0.01736 -0.00842
AFIX 43
H46 2 0.949068 0.456658 0.835761 11.00000 -1.20000
AFIX 0
C47 1 0.705996 0.354301 0.767742 11.00000 0.02001 0.01812 =
0.01304 0.00106 0.00790 -0.00081
AFIX 23
H47A 2 0.751445 0.366060 0.765763 11.00000 -1.20000
H47B 2 0.676511 0.306823 0.734108 11.00000 -1.20000
AFIX 0
C48 1 0.676118 0.487332 0.768843 11.00000 0.02272 0.01624 =
0.01300 -0.00135 0.00828 -0.00387
C49 1 0.613559 0.539970 0.741845 11.00000 0.02300 0.02224 =
0.02154 0.00251 0.00779 0.00059
AFIX 43
H49 2 0.575020 0.495524 0.716117 11.00000 -1.20000
AFIX 0
C50 1 0.616287 0.675349 0.759315 11.00000 0.02976 0.02210 =
0.02950 0.00507 0.01438 0.00615
AFIX 43
H50 2 0.580039 0.738230 0.747499 11.00000 -1.20000
AFIX 0
C51 1 0.680182 0.696085 0.795712 11.00000 0.03516 0.01590 =
0.02450 0.00020 0.01614 0.00238
AFIX 43
H51 2 0.696393 0.777794 0.814266 11.00000 -1.20000
AFIX 0
PART 2
C52B 1 0.544918 0.240189 0.756210 -21.00000 0.02000 0.03344 =
0.02212 -0.00072 0.00327 -0.00586
AFIX 137
H52D 2 0.510158 0.180376 0.759605 -21.00000 -1.50000
H52E 2 0.559409 0.207462 0.727282 -21.00000 -1.50000
H52F 2 0.525720 0.329801 0.746769 -21.00000 -1.50000
AFIX 0
CL2B 4 0.601721 0.393863 0.864681 -21.00000 0.02000 0.03344 =
0.02212 -0.00072 0.00327 -0.00586
C26B 1 0.448439 0.607890 0.736633 -31.00000 0.01904 0.03586 =
0.02822 -0.00246 0.00590 0.00201
AFIX 137
H26D 2 0.460712 0.699082 0.749955 -31.00000 -1.50000
H26E 2 0.486201 0.567505 0.729215 -31.00000 -1.50000
H26F 2 0.439489 0.555560 0.764588 -31.00000 -1.50000
AFIX 0
CL1B 4 0.365674 0.753429 0.610960 -31.00000 0.01904 0.03586 =
0.02822 -0.00246 0.00590 0.00201
HKLF 4
REM mo_kpjk6001301_AlMeCltBu_0m_a.res in P2(1)/n
REM R1 = 0.0524 for 8703 Fo > 4sig(Fo) and 0.0758 for all 11382 data
REM 595 parameters refined using 72 restraints
END
WGHT 0.0495 6.3557
REM Highest difference peak 0.478, deepest hole -0.677, 1-sigma level 0.061
Q1 1 0.3818 0.8688 0.6709 11.00000 0.05 0.43
Q2 1 0.4574 0.8457 0.7554 11.00000 0.05 0.42
Q3 1 0.5578 0.9547 0.7566 11.00000 0.05 0.39
Q4 1 0.4026 0.7116 0.6262 11.00000 0.05 0.37
Q5 1 0.3370 0.7440 0.5802 11.00000 0.05 0.37
Q6 1 0.7430 0.0825 0.8323 11.00000 0.05 0.35
Q7 1 0.6396 -0.0130 0.8355 11.00000 0.05 0.35
Q8 1 0.3626 0.7048 0.6464 11.00000 0.05 0.34
Q9 1 0.5621 0.4183 0.8384 11.00000 0.05 0.33
Q10 1 0.7223 0.0212 0.8595 11.00000 0.05 0.30
;
_shelx_res_checksum 67022
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
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data_complex3_AlOt-BuMe
_database_code_depnum_ccdc_archive 'CCDC 1553618'
_audit_update_record
;
2018-03-20 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_audit_creation_date 2018-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C30 H44 Al N O4'
_chemical_formula_sum 'C30 H44 Al N O4'
_chemical_formula_weight 509.64
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.098(5)
_cell_length_b 10.771(4)
_cell_length_c 14.599(8)
_cell_angle_alpha 105.627(16)
_cell_angle_beta 97.16(2)
_cell_angle_gamma 96.551(13)
_cell_volume 1499.1(12)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9890
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 33.74
_cell_measurement_theta_min 2.33
_shelx_estimated_absorpt_T_max 0.7457
_shelx_estimated_absorpt_T_min 0.7113
_exptl_absorpt_coefficient_mu 0.100
_exptl_absorpt_correction_T_max 0.7457
_exptl_absorpt_correction_T_min 0.7113
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.129
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description rectangular
_exptl_crystal_F_000 552
_exptl_crystal_size_max 0.70
_exptl_crystal_size_mid 0.40
_exptl_crystal_size_min 0.10
_exptl_transmission_factor_max 0.7457
_exptl_transmission_factor_min 0.7113
_diffrn_reflns_av_R_equivalents 0.0361
_diffrn_reflns_av_unetI/netI 0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 74896
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.328
_diffrn_reflns_theta_min 2.715
_diffrn_ambient_temperature 150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'Bruker D8 venture'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed x-ray tube'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6532
_reflns_number_total 7430
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection 'APEX3 v2015.5-2 (Bruker AXS Inc., 2015)'
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'XT, VERSION 2014/4'
_refine_diff_density_max 0.750
_refine_diff_density_min -0.476
_refine_diff_density_rms 0.048
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 398
_refine_ls_number_reflns 7430
_refine_ls_number_restraints 156
_refine_ls_R_factor_all 0.0587
_refine_ls_R_factor_gt 0.0514
_refine_ls_restrained_S_all 1.055
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+0.9082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1293
_refine_ls_wR_factor_ref 0.1343
_refine_special_details ?
_olex2_refinement_description
;
1. Shared sites
{H14G, H14F}
2. Others
Fixed Uiso: H1A(0.053) H1B(0.053) H1C(0.053) H4(0.028) H6(0.026) H8A(0.025)
H8B(0.025) H10A(0.056) H10B(0.056) H10C(0.056) H11A(0.06) H11B(0.06)
H11C(0.06) H12A(0.058) H12B(0.058) H12C(0.058) H14A(0.054) H14B(0.054)
H14C(0.054) H15A(0.054) H15B(0.054) H15C(0.054) H16A(0.054) H16B(0.054)
H16C(0.054) H17A(0.027) H17B(0.027) H19(0.045) H20(0.053) H21(0.054)
H22A(0.027) H22B(0.027) H24(0.037) H25(0.043) H26(0.043) H28A(0.061)
H28B(0.061) H28C(0.061) H29A(0.071) H29B(0.071) H29C(0.071) H30A(0.068)
H30B(0.068) H30C(0.068) H14D(0.055) H14E(0.055) H14F(0.055) H15D(0.054)
H15E(0.054) H15F(0.054) H16D(0.053) H16E(0.053) H16F(0.053) H14G(0.053)
H14H(0.053) H14I(0.053) H16G(0.053) H16H(0.053) H16I(0.053) H15G(0.054)
H15H(0.054) H15I(0.054)
Fixed X: H1A(0.8631) H1B(0.8404) H1C(0.9619) H4(0.2088) H6(0.4247)
H8A(0.6009) H8B(0.6172) H10A(0.5536) H10B(0.455) H10C(0.4712) H11A(0.262)
H11B(0.3253) H11C(0.422) H12A(0.2235) H12B(0.2086) H12C(0.1422) H14A(0.224)
H14B(0.3549) H14C(0.3278) H15A(0.0914) H15B(0.1011) H15C(0.2286) H16A(0.12)
H16B(0.0415) H16C(0.0204) H17A(0.7236) H17B(0.8777) H19(0.5956) H20(0.6575)
H21(0.8599) H22A(0.8306) H22B(0.8545) H24(1.0453) H25(1.28) H26(1.2737)
H28A(0.8873) H28B(0.8103) H28C(0.915) H29A(0.7393) H29B(0.6311) H29C(0.598)
H30A(0.5503) H30B(0.5882) H30C(0.6639) H14D(0.192) H14E(0.3419) H14F(0.2713)
H15D(0.1044) H15E(0.1439) H15F(0.2579) H16D(0.0645) H16E(0.0284) H16F(-0.0087)
H14G(0.2744) H14H(0.1548) H14I(0.1212) H16G(0.0328) H16H(0.0566) H16I(-0.0123)
H15G(0.1543) H15H(0.2503) H15I(0.311)
Fixed Y: H1A(0.8136) H1B(0.6611) H1C(0.7217) H4(0.429) H6(0.2645) H8A(0.5263)
H8B(0.3778) H10A(0.7219) H10B(0.7792) H10C(0.6282) H11A(0.7683) H11B(0.8634)
H11C(0.8122) H12A(0.5666) H12B(0.7179) H12C(0.6212) H14A(0.0023) H14B(0.0748)
H14C(0.1106) H15A(0.0703) H15B(0.22) H15C(0.146) H16A(0.2071) H16B(0.2761)
H16C(0.1203) H17A(0.4276) H17B(0.4426) H19(0.178) H20(-0.0258) H21(0.0453)
H22A(0.5676) H22B(0.4231) H24(0.7622) H25(0.737) H26(0.5063) H28A(0.8797)
H28B(1.0035) H28C(0.9932) H29A(1.0208) H29B(1.0308) H29C(0.9248) H30A(0.7511)
H30B(0.8541) H30C(0.7295) H14D(0.0256) H14E(0.0871) H14F(0.1479) H15D(0.0548)
H15E(0.1938) H15F(0.1052) H16D(0.253) H16E(0.2937) H16F(0.1451) H14G(0.1401)
H14H(0.2245) H14I(0.075) H16G(0.2984) H16H(0.264) H16I(0.1527) H15G(0.0187)
H15H(0.1214) H15I(0.0564)
Fixed Z: H1A(0.2133) H1B(0.1574) H1C(0.2457) H4(0.0743) H6(0.2479)
H8A(0.4009) H8B(0.3538) H10A(0.1109) H10B(0.0435) H10C(0.0106) H11A(0.2318)
H11B(0.1757) H11C(0.2483) H12A(-0.0105) H12B(0.0217) H12C(0.0754) H14A(0.0351)
H14B(0.113) H14C(0.0135) H15A(0.1705) H15B(0.2308) H15C(0.24) H16A(-0.0196)
H16B(0.0641) H16C(0.0241) H17A(0.1744) H17B(0.2223) H19(0.1253) H20(0.1724)
H21(0.2933) H22A(0.4661) H22B(0.414) H24(0.4684) H25(0.4233) H26(0.3384)
H28A(0.6068) H28B(0.6312) H28C(0.5568) H29A(0.432) H29B(0.5039) H29C(0.4003)
H30A(0.4799) H30B(0.5847) H30C(0.5585) H14D(0.0087) H14E(0.0639) H14F(-0.0146)
H15D(0.1658) H15E(0.2453) H15F(0.2173) H16D(0.0137) H16E(0.1204) H16F(0.0553)
H14G(-0.0151) H14H(-0.0215) H14I(-0.0232) H16G(0.1018) H16H(0.202)
H16I(0.1056) H15G(0.1325) H15H(0.2231) H15I(0.1285)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Al1 Al 0.74998(4) 0.69168(4) 0.30959(3) 0.02067(11) Uani 1 1 d . . . . .
N1 N 0.75510(11) 0.50826(11) 0.32094(8) 0.0193(2) Uani 1 1 d . . . . .
O1 O 0.78877(11) 0.78683(11) 0.42686(8) 0.0324(3) Uani 1 1 d . . . . .
O2 O 0.57757(10) 0.67094(10) 0.26279(8) 0.0272(2) Uani 1 1 d . . . . .
O3 O 0.85532(12) 0.23170(12) 0.28242(10) 0.0396(3) Uani 1 1 d . . . . .
O4 O 1.07489(10) 0.47459(11) 0.35758(8) 0.0311(2) Uani 1 1 d . . . . .
C1 C 0.86865(18) 0.72635(17) 0.22039(13) 0.0352(4) Uani 1 1 d . . . . .
H1A H 0.8631 0.8136 0.2133 0.053 Uiso 1 1 calc GR . . . .
H1B H 0.8404 0.6611 0.1574 0.053 Uiso 1 1 calc GR . . . .
H1C H 0.9619 0.7217 0.2457 0.053 Uiso 1 1 calc GR . . . .
C2 C 0.48635(13) 0.56065(13) 0.22650(10) 0.0205(3) Uani 1 1 d . . . . .
C3 C 0.37364(13) 0.55302(13) 0.15570(10) 0.0215(3) Uani 1 1 d . . . . .
C4 C 0.28437(14) 0.43503(14) 0.12193(10) 0.0236(3) Uani 1 1 d . . . . .
H4 H 0.2088 0.4290 0.0743 0.028 Uiso 1 1 calc R . . . .
C5 C 0.29948(14) 0.32551(14) 0.15399(10) 0.0233(3) Uani 1 1 d D . . . .
C6 C 0.41107(13) 0.33696(13) 0.22434(10) 0.0218(3) Uani 1 1 d . . . . .
H6 H 0.4247 0.2645 0.2479 0.026 Uiso 1 1 calc R . . . .
C7 C 0.50301(13) 0.45254(13) 0.26090(9) 0.0198(3) Uani 1 1 d . . . . .
C8 C 0.61734(13) 0.46380(13) 0.34153(10) 0.0205(3) Uani 1 1 d . . . . .
H8A H 0.6009 0.5263 0.4009 0.025 Uiso 1 1 calc R . . . .
H8B H 0.6172 0.3778 0.3538 0.025 Uiso 1 1 calc R . . . .
C9 C 0.35060(15) 0.67016(14) 0.11745(11) 0.0269(3) Uani 1 1 d . . . . .
C10 C 0.46827(18) 0.70281(18) 0.06593(13) 0.0376(4) Uani 1 1 d . . . . .
H10A H 0.5536 0.7219 0.1109 0.056 Uiso 1 1 calc GR . . . .
H10B H 0.4550 0.7792 0.0435 0.056 Uiso 1 1 calc GR . . . .
H10C H 0.4712 0.6282 0.0106 0.056 Uiso 1 1 calc GR . . . .
C11 C 0.3389(2) 0.78934(17) 0.20091(14) 0.0399(4) Uani 1 1 d . . . . .
H11A H 0.2620 0.7683 0.2318 0.060 Uiso 1 1 calc GR . . . .
H11B H 0.3253 0.8634 0.1757 0.060 Uiso 1 1 calc GR . . . .
H11C H 0.4220 0.8122 0.2483 0.060 Uiso 1 1 calc GR . . . .
C12 C 0.21933(17) 0.64135(18) 0.04438(13) 0.0384(4) Uani 1 1 d . . . . .
H12A H 0.2235 0.5666 -0.0105 0.058 Uiso 1 1 calc GR . . . .
H12B H 0.2086 0.7179 0.0217 0.058 Uiso 1 1 calc GR . . . .
H12C H 0.1422 0.6212 0.0754 0.058 Uiso 1 1 calc GR . . . .
C13 C 0.20010(17) 0.19697(16) 0.11285(12) 0.0352(3) Uani 1 1 d D U . . .
C14A C 0.2851(5) 0.0851(4) 0.0638(3) 0.0359(5) Uani 0.424(3) 1 d D U P A 1
H14A H 0.2240 0.0023 0.0351 0.054 Uiso 0.424(3) 1 calc GR . P A 1
H14B H 0.3549 0.0748 0.1130 0.054 Uiso 0.424(3) 1 calc GR . P A 1
H14C H 0.3278 0.1106 0.0135 0.054 Uiso 0.424(3) 1 calc GR . P A 1
C15A C 0.1509(6) 0.1545(5) 0.1960(4) 0.0359(5) Uani 0.424(3) 1 d D U P A 1
H15A H 0.0914 0.0703 0.1705 0.054 Uiso 0.424(3) 1 calc GR . P A 1
H15B H 0.1011 0.2200 0.2308 0.054 Uiso 0.424(3) 1 calc GR . P A 1
H15C H 0.2286 0.1460 0.2400 0.054 Uiso 0.424(3) 1 calc GR . P A 1
C16A C 0.0857(5) 0.2004(4) 0.0390(4) 0.0363(5) Uani 0.424(3) 1 d D U P A 1
H16A H 0.1200 0.2071 -0.0196 0.054 Uiso 0.424(3) 1 calc GR . P A 1
H16B H 0.0415 0.2761 0.0641 0.054 Uiso 0.424(3) 1 calc GR . P A 1
H16C H 0.0204 0.1203 0.0241 0.054 Uiso 0.424(3) 1 calc GR . P A 1
C17 C 0.78331(14) 0.41646(13) 0.22978(10) 0.0222(3) Uani 1 1 d . . . . .
H17A H 0.7236 0.4276 0.1744 0.027 Uiso 1 1 calc R . . . .
H17B H 0.8777 0.4426 0.2223 0.027 Uiso 1 1 calc R . . . .
C18 C 0.76425(14) 0.27513(14) 0.22491(10) 0.0249(3) Uani 1 1 d . . . . .
C19 C 0.66972(18) 0.17476(17) 0.17104(13) 0.0372(4) Uani 1 1 d . . . . .
H19 H 0.5956 0.1780 0.1253 0.045 Uiso 1 1 calc R . . . .
C20 C 0.7047(2) 0.06081(17) 0.19750(15) 0.0439(4) Uani 1 1 d . . . . .
H20 H 0.6575 -0.0258 0.1724 0.053 Uiso 1 1 calc R . . . .
C21 C 0.8149(2) 0.10048(18) 0.26331(16) 0.0448(4) Uani 1 1 d . . . . .
H21 H 0.8599 0.0453 0.2933 0.054 Uiso 1 1 calc R . . . .
C22 C 0.85723(13) 0.51240(14) 0.40738(10) 0.0227(3) Uani 1 1 d . . . . .
H22A H 0.8306 0.5676 0.4661 0.027 Uiso 1 1 calc R . . . .
H22B H 0.8545 0.4231 0.4140 0.027 Uiso 1 1 calc R . . . .
C23 C 0.99849(14) 0.56383(14) 0.40172(10) 0.0233(3) Uani 1 1 d . . . . .
C24 C 1.07383(15) 0.68386(16) 0.43493(12) 0.0307(3) Uani 1 1 d . . . . .
H24 H 1.0453 0.7622 0.4684 0.037 Uiso 1 1 calc R . . . .
C25 C 1.20456(16) 0.66982(18) 0.40984(13) 0.0358(4) Uani 1 1 d . . . . .
H25 H 1.2800 0.7370 0.4233 0.043 Uiso 1 1 calc R . . . .
C26 C 1.20012(16) 0.54324(18) 0.36359(12) 0.0355(4) Uani 1 1 d . . . . .
H26 H 1.2737 0.5063 0.3384 0.043 Uiso 1 1 calc R . . . .
C27 C 0.73176(15) 0.87269(15) 0.49746(11) 0.0293(3) Uani 1 1 d . . . . .
C28 C 0.84641(19) 0.94367(19) 0.58056(12) 0.0410(4) Uani 1 1 d . . . . .
H28A H 0.8873 0.8797 0.6068 0.061 Uiso 1 1 calc GR . . . .
H28B H 0.8103 1.0035 0.6312 0.061 Uiso 1 1 calc GR . . . .
H28C H 0.9150 0.9932 0.5568 0.061 Uiso 1 1 calc GR . . . .
C29 C 0.6695(2) 0.97105(19) 0.45460(15) 0.0473(5) Uani 1 1 d . . . . .
H29A H 0.7393 1.0208 0.4320 0.071 Uiso 1 1 calc GR . . . .
H29B H 0.6311 1.0308 0.5039 0.071 Uiso 1 1 calc GR . . . .
H29C H 0.5980 0.9248 0.4003 0.071 Uiso 1 1 calc GR . . . .
C30 C 0.62388(19) 0.79486(19) 0.53334(15) 0.0452(4) Uani 1 1 d . . . . .
H30A H 0.5503 0.7511 0.4799 0.068 Uiso 1 1 calc GR . . . .
H30B H 0.5882 0.8541 0.5847 0.068 Uiso 1 1 calc GR . . . .
H30C H 0.6639 0.7295 0.5585 0.068 Uiso 1 1 calc GR . . . .
C14B C 0.2561(4) 0.1067(4) 0.0362(3) 0.0364(4) Uani 0.452(3) 1 d D U P A 2
H14D H 0.1920 0.0256 0.0087 0.055 Uiso 0.452(3) 1 calc GR . P A 2
H14E H 0.3419 0.0871 0.0639 0.055 Uiso 0.452(3) 1 calc GR . P A 2
H14F H 0.2713 0.1479 -0.0146 0.055 Uiso 0.452(3) 1 calc GR . P A 2
C15B C 0.1742(5) 0.1317(5) 0.1926(4) 0.0361(5) Uani 0.452(3) 1 d D U P A 2
H15D H 0.1044 0.0548 0.1658 0.054 Uiso 0.452(3) 1 calc GR . P A 2
H15E H 0.1439 0.1938 0.2453 0.054 Uiso 0.452(3) 1 calc GR . P A 2
H15F H 0.2579 0.1052 0.2173 0.054 Uiso 0.452(3) 1 calc GR . P A 2
C16B C 0.0575(4) 0.2249(4) 0.0716(3) 0.0355(5) Uani 0.452(3) 1 d D U P A 2
H16D H 0.0645 0.2530 0.0137 0.053 Uiso 0.452(3) 1 calc GR . P A 2
H16E H 0.0284 0.2937 0.1204 0.053 Uiso 0.452(3) 1 calc GR . P A 2
H16F H -0.0087 0.1451 0.0553 0.053 Uiso 0.452(3) 1 calc GR . P A 2
C14C C 0.1864(13) 0.1554(12) 0.0036(7) 0.0353(5) Uani 0.1248(18) 1 d D U P A 3
H14G H 0.2744 0.1401 -0.0151 0.053 Uiso 0.1248(18) 1 calc GR . P A 3
H14H H 0.1548 0.2245 -0.0215 0.053 Uiso 0.1248(18) 1 calc GR . P A 3
H14I H 0.1212 0.0750 -0.0232 0.053 Uiso 0.1248(18) 1 calc GR . P A 3
C16C C 0.0555(11) 0.2313(12) 0.1324(10) 0.0352(6) Uani 0.1248(18) 1 d D U P A 3
H16G H 0.0328 0.2984 0.1018 0.053 Uiso 0.1248(18) 1 calc GR . P A 3
H16H H 0.0566 0.2640 0.2020 0.053 Uiso 0.1248(18) 1 calc GR . P A 3
H16I H -0.0123 0.1527 0.1056 0.053 Uiso 0.1248(18) 1 calc GR . P A 3
C15C C 0.2316(14) 0.0893(11) 0.1526(10) 0.0357(5) Uani 0.1248(18) 1 d D U P A 3
H15G H 0.1543 0.0187 0.1325 0.054 Uiso 0.1248(18) 1 calc GR . P A 3
H15H H 0.2503 0.1214 0.2231 0.054 Uiso 0.1248(18) 1 calc GR . P A 3
H15I H 0.3110 0.0564 0.1285 0.054 Uiso 0.1248(18) 1 calc GR . P A 3
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Al1 0.0194(2) 0.0188(2) 0.0217(2) 0.00456(15) 0.00062(15) 0.00024(14)
N1 0.0162(5) 0.0228(5) 0.0185(5) 0.0066(4) 0.0010(4) 0.0019(4)
O1 0.0256(5) 0.0350(6) 0.0276(5) -0.0051(4) -0.0008(4) 0.0080(4)
O2 0.0231(5) 0.0188(5) 0.0357(6) 0.0085(4) -0.0075(4) -0.0019(4)
O3 0.0346(6) 0.0308(6) 0.0540(8) 0.0183(5) -0.0030(5) 0.0046(5)
O4 0.0205(5) 0.0343(6) 0.0347(6) 0.0034(5) 0.0055(4) 0.0031(4)
C1 0.0398(9) 0.0317(8) 0.0398(9) 0.0169(7) 0.0137(7) 0.0044(7)
C2 0.0181(6) 0.0197(6) 0.0221(6) 0.0048(5) 0.0014(5) 0.0011(5)
C3 0.0200(6) 0.0230(6) 0.0217(6) 0.0079(5) 0.0015(5) 0.0028(5)
C4 0.0197(6) 0.0278(7) 0.0214(6) 0.0074(5) -0.0010(5) 0.0000(5)
C5 0.0203(6) 0.0245(7) 0.0230(6) 0.0061(5) 0.0021(5) -0.0027(5)
C6 0.0208(6) 0.0213(6) 0.0240(6) 0.0087(5) 0.0038(5) 0.0009(5)
C7 0.0172(6) 0.0225(6) 0.0193(6) 0.0062(5) 0.0019(5) 0.0021(5)
C8 0.0168(6) 0.0238(6) 0.0214(6) 0.0088(5) 0.0018(5) 0.0012(5)
C9 0.0259(7) 0.0257(7) 0.0299(7) 0.0127(6) -0.0018(6) 0.0030(5)
C10 0.0350(8) 0.0401(9) 0.0438(9) 0.0257(8) 0.0037(7) 0.0007(7)
C11 0.0467(10) 0.0299(8) 0.0432(9) 0.0111(7) -0.0021(8) 0.0150(7)
C12 0.0328(8) 0.0427(9) 0.0410(9) 0.0230(8) -0.0097(7) 0.0016(7)
C13 0.0322(6) 0.0297(6) 0.0373(6) 0.0075(5) -0.0002(5) -0.0094(4)
C14A 0.0336(9) 0.0308(8) 0.0375(8) 0.0080(6) 0.0002(6) -0.0083(8)
C15A 0.0332(9) 0.0308(11) 0.0381(7) 0.0083(7) 0.0005(6) -0.0085(7)
C16A 0.0333(7) 0.0309(11) 0.0382(7) 0.0079(6) -0.0007(5) -0.0090(7)
C17 0.0237(6) 0.0231(6) 0.0205(6) 0.0067(5) 0.0040(5) 0.0043(5)
C18 0.0240(7) 0.0250(7) 0.0260(7) 0.0067(5) 0.0054(5) 0.0056(5)
C19 0.0362(9) 0.0336(8) 0.0336(8) 0.0013(7) -0.0001(7) -0.0015(7)
C20 0.0539(11) 0.0232(8) 0.0504(11) 0.0036(7) 0.0152(9) -0.0022(7)
C21 0.0513(11) 0.0289(8) 0.0592(12) 0.0198(8) 0.0088(9) 0.0090(8)
C22 0.0177(6) 0.0300(7) 0.0209(6) 0.0101(5) 0.0000(5) 0.0027(5)
C23 0.0193(6) 0.0294(7) 0.0216(6) 0.0087(5) 0.0007(5) 0.0047(5)
C24 0.0230(7) 0.0308(8) 0.0364(8) 0.0093(6) 0.0004(6) 0.0027(6)
C25 0.0233(7) 0.0416(9) 0.0418(9) 0.0148(7) 0.0038(6) -0.0031(6)
C26 0.0199(7) 0.0490(10) 0.0354(8) 0.0087(7) 0.0075(6) 0.0016(6)
C27 0.0273(7) 0.0288(7) 0.0266(7) 0.0000(6) 0.0042(6) 0.0030(6)
C28 0.0388(9) 0.0460(10) 0.0269(8) -0.0033(7) 0.0036(7) -0.0041(7)
C29 0.0544(11) 0.0388(10) 0.0481(11) 0.0067(8) 0.0088(9) 0.0187(8)
C30 0.0366(9) 0.0430(10) 0.0515(11) 0.0052(8) 0.0155(8) -0.0004(8)
C14B 0.0333(9) 0.0314(8) 0.0380(7) 0.0073(6) 0.0003(6) -0.0085(7)
C15B 0.0338(9) 0.0310(10) 0.0384(7) 0.0086(7) 0.0011(6) -0.0077(7)
C16B 0.0323(7) 0.0303(11) 0.0381(8) 0.0082(7) 0.0001(5) -0.0093(6)
C14C 0.0329(11) 0.0293(12) 0.0374(6) 0.0075(5) -0.0001(5) -0.0096(9)
C16C 0.0322(7) 0.0294(14) 0.0374(9) 0.0073(9) -0.0002(7) -0.0096(8)
C15C 0.0332(12) 0.0304(8) 0.0379(9) 0.0081(8) 0.0005(8) -0.0087(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al1 N1 2.0323(14) . ?
Al1 O1 1.7120(14) . ?
Al1 O2 1.7552(13) . ?
Al1 C1 1.9545(18) . ?
N1 C8 1.5116(17) . ?
N1 C17 1.5099(18) . ?
N1 C22 1.5143(17) . ?
O1 C27 1.4159(19) . ?
O2 C2 1.3528(16) . ?
O3 C18 1.3737(19) . ?
O3 C21 1.367(2) . ?
O4 C23 1.3762(18) . ?
O4 C26 1.3703(19) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.4179(19) . ?
C2 C7 1.4054(19) . ?
C3 C4 1.4004(19) . ?
C3 C9 1.540(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.398(2) . ?
C5 C6 1.397(2) . ?
C5 C13 1.539(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.3970(19) . ?
C7 C8 1.5119(19) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.540(2) . ?
C9 C11 1.541(2) . ?
C9 C12 1.538(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14A 1.620(5) . ?
C13 C15A 1.525(6) . ?
C13 C16A 1.489(5) . ?
C13 C14B 1.488(5) . ?
C13 C15B 1.547(5) . ?
C13 C16B 1.583(4) . ?
C13 C14C 1.520(10) . ?
C13 C16C 1.588(10) . ?
C13 C15C 1.478(10) . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C14A H14C 0.9800 . ?
C15A H15A 0.9800 . ?
C15A H15B 0.9800 . ?
C15A H15C 0.9800 . ?
C16A H16A 0.9800 . ?
C16A H16B 0.9800 . ?
C16A H16C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.494(2) . ?
C18 C19 1.348(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.449(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.322(3) . ?
C21 H21 0.9500 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.491(2) . ?
C23 C24 1.353(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.427(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.341(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.531(2) . ?
C27 C29 1.523(3) . ?
C27 C30 1.528(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C15B H15D 0.9800 . ?
C15B H15E 0.9800 . ?
C15B H15F 0.9800 . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?
C14C H14G 0.9800 . ?
C14C H14H 0.9800 . ?
C14C H14I 0.9800 . ?
C16C H16G 0.9800 . ?
C16C H16H 0.9800 . ?
C16C H16I 0.9800 . ?
C15C H15G 0.9800 . ?
C15C H15H 0.9800 . ?
C15C H15I 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Al1 N1 103.16(6) . . ?
O1 Al1 O2 112.93(6) . . ?
O1 Al1 C1 117.38(8) . . ?
O2 Al1 N1 97.52(5) . . ?
O2 Al1 C1 113.46(8) . . ?
C1 Al1 N1 109.86(6) . . ?
C8 N1 Al1 105.51(8) . . ?
C8 N1 C22 107.12(10) . . ?
C17 N1 Al1 112.14(8) . . ?
C17 N1 C8 110.44(10) . . ?
C17 N1 C22 111.46(11) . . ?
C22 N1 Al1 109.89(8) . . ?
C27 O1 Al1 140.65(10) . . ?
C2 O2 Al1 130.05(9) . . ?
C21 O3 C18 106.62(14) . . ?
C26 O4 C23 106.20(13) . . ?
Al1 C1 H1A 109.5 . . ?
Al1 C1 H1B 109.5 . . ?
Al1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 C2 C3 121.23(12) . . ?
O2 C2 C7 119.15(12) . . ?
C7 C2 C3 119.62(12) . . ?
C2 C3 C9 121.16(12) . . ?
C4 C3 C2 117.47(12) . . ?
C4 C3 C9 121.38(12) . . ?
C3 C4 H4 118.0 . . ?
C5 C4 C3 124.09(13) . . ?
C5 C4 H4 118.0 . . ?
C4 C5 C13 122.04(13) . . ?
C6 C5 C4 116.86(12) . . ?
C6 C5 C13 121.09(13) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 C5 121.47(13) . . ?
C7 C6 H6 119.3 . . ?
C2 C7 C8 119.65(12) . . ?
C6 C7 C2 120.49(12) . . ?
C6 C7 C8 119.78(12) . . ?
N1 C8 C7 113.88(11) . . ?
N1 C8 H8A 108.8 . . ?
N1 C8 H8B 108.8 . . ?
C7 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C3 C9 C11 110.31(13) . . ?
C10 C9 C3 109.58(12) . . ?
C10 C9 C11 110.25(14) . . ?
C12 C9 C3 112.01(12) . . ?
C12 C9 C10 107.57(14) . . ?
C12 C9 C11 107.07(14) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 C13 C14A 107.43(19) . . ?
C5 C13 C15B 111.2(2) . . ?
C5 C13 C16B 110.13(19) . . ?
C5 C13 C16C 106.3(5) . . ?
C15A C13 C5 109.0(2) . . ?
C15A C13 C14A 105.0(3) . . ?
C16A C13 C5 114.8(2) . . ?
C16A C13 C14A 108.3(3) . . ?
C16A C13 C15A 111.9(3) . . ?
C14B C13 C5 109.28(19) . . ?
C14B C13 C15B 109.7(3) . . ?
C14B C13 C16B 110.8(3) . . ?
C15B C13 C16B 105.6(3) . . ?
C14C C13 C5 109.1(5) . . ?
C14C C13 C16C 103.9(6) . . ?
C15C C13 C5 115.5(5) . . ?
C15C C13 C14C 111.1(7) . . ?
C15C C13 C16C 110.2(8) . . ?
C13 C14A H14A 109.5 . . ?
C13 C14A H14B 109.5 . . ?
C13 C14A H14C 109.5 . . ?
H14A C14A H14B 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
C13 C15A H15A 109.5 . . ?
C13 C15A H15B 109.5 . . ?
C13 C15A H15C 109.5 . . ?
H15A C15A H15B 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
C13 C16A H16A 109.5 . . ?
C13 C16A H16B 109.5 . . ?
C13 C16A H16C 109.5 . . ?
H16A C16A H16B 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
N1 C17 H17A 108.3 . . ?
N1 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C18 C17 N1 115.72(11) . . ?
C18 C17 H17A 108.3 . . ?
C18 C17 H17B 108.3 . . ?
O3 C18 C17 118.80(13) . . ?
C19 C18 O3 110.03(14) . . ?
C19 C18 C17 131.16(15) . . ?
C18 C19 H19 127.2 . . ?
C18 C19 C20 105.70(16) . . ?
C20 C19 H19 127.2 . . ?
C19 C20 H20 126.6 . . ?
C21 C20 C19 106.86(16) . . ?
C21 C20 H20 126.6 . . ?
O3 C21 H21 124.6 . . ?
C20 C21 O3 110.78(16) . . ?
C20 C21 H21 124.6 . . ?
N1 C22 H22A 108.8 . . ?
N1 C22 H22B 108.8 . . ?
H22A C22 H22B 107.6 . . ?
C23 C22 N1 113.99(11) . . ?
C23 C22 H22A 108.8 . . ?
C23 C22 H22B 108.8 . . ?
O4 C23 C22 116.84(13) . . ?
C24 C23 O4 109.90(13) . . ?
C24 C23 C22 133.20(14) . . ?
C23 C24 H24 126.7 . . ?
C23 C24 C25 106.61(15) . . ?
C25 C24 H24 126.7 . . ?
C24 C25 H25 126.7 . . ?
C26 C25 C24 106.57(14) . . ?
C26 C25 H25 126.7 . . ?
O4 C26 H26 124.6 . . ?
C25 C26 O4 110.71(14) . . ?
C25 C26 H26 124.6 . . ?
O1 C27 C28 107.24(13) . . ?
O1 C27 C29 109.80(14) . . ?
O1 C27 C30 109.76(14) . . ?
C29 C27 C28 109.91(15) . . ?
C29 C27 C30 109.93(16) . . ?
C30 C27 C28 110.15(15) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C13 C14B H14D 109.5 . . ?
C13 C14B H14E 109.5 . . ?
C13 C14B H14F 109.5 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C13 C15B H15D 109.5 . . ?
C13 C15B H15E 109.5 . . ?
C13 C15B H15F 109.5 . . ?
H15D C15B H15E 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C13 C16B H16D 109.5 . . ?
C13 C16B H16E 109.5 . . ?
C13 C16B H16F 109.5 . . ?
H16D C16B H16E 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
C13 C14C H14G 109.5 . . ?
C13 C14C H14H 109.5 . . ?
C13 C14C H14I 109.5 . . ?
H14G C14C H14H 109.5 . . ?
H14G C14C H14I 109.5 . . ?
H14H C14C H14I 109.5 . . ?
C13 C16C H16G 109.5 . . ?
C13 C16C H16H 109.5 . . ?
C13 C16C H16I 109.5 . . ?
H16G C16C H16H 109.5 . . ?
H16G C16C H16I 109.5 . . ?
H16H C16C H16I 109.5 . . ?
C13 C15C H15G 109.5 . . ?
C13 C15C H15H 109.5 . . ?
C13 C15C H15I 109.5 . . ?
H15G C15C H15H 109.5 . . ?
H15G C15C H15I 109.5 . . ?
H15H C15C H15I 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Al1 N1 C8 C7 63.76(12) . . . . ?
Al1 N1 C17 C18 -169.32(9) . . . . ?
Al1 N1 C22 C23 -61.73(13) . . . . ?
Al1 O1 C27 C28 -167.46(14) . . . . ?
Al1 O1 C27 C29 -48.1(2) . . . . ?
Al1 O1 C27 C30 72.9(2) . . . . ?
Al1 O2 C2 C3 -151.55(11) . . . . ?
Al1 O2 C2 C7 29.39(19) . . . . ?
N1 Al1 O1 C27 -116.83(17) . . . . ?
N1 Al1 O2 C2 -12.68(13) . . . . ?
N1 C17 C18 O3 -71.15(17) . . . . ?
N1 C17 C18 C19 109.56(19) . . . . ?
N1 C22 C23 O4 -88.72(15) . . . . ?
N1 C22 C23 C24 94.23(19) . . . . ?
O1 Al1 O2 C2 -120.45(13) . . . . ?
O2 Al1 O1 C27 -12.66(19) . . . . ?
O2 C2 C3 C4 179.85(13) . . . . ?
O2 C2 C3 C9 -0.1(2) . . . . ?
O2 C2 C7 C6 -179.53(12) . . . . ?
O2 C2 C7 C8 3.53(19) . . . . ?
O3 C18 C19 C20 0.22(19) . . . . ?
O4 C23 C24 C25 0.41(17) . . . . ?
C1 Al1 O1 C27 122.24(17) . . . . ?
C1 Al1 O2 C2 102.84(13) . . . . ?
C2 C3 C4 C5 0.3(2) . . . . ?
C2 C3 C9 C10 63.04(18) . . . . ?
C2 C3 C9 C11 -58.52(18) . . . . ?
C2 C3 C9 C12 -177.67(14) . . . . ?
C2 C7 C8 N1 -55.17(17) . . . . ?
C3 C2 C7 C6 1.4(2) . . . . ?
C3 C2 C7 C8 -175.54(12) . . . . ?
C3 C4 C5 C6 0.2(2) . . . . ?
C3 C4 C5 C13 -178.61(14) . . . . ?
C4 C3 C9 C10 -116.90(16) . . . . ?
C4 C3 C9 C11 121.54(16) . . . . ?
C4 C3 C9 C12 2.4(2) . . . . ?
C4 C5 C6 C7 0.1(2) . . . . ?
C4 C5 C13 C14A 118.7(2) . . . . ?
C4 C5 C13 C15A -128.1(2) . . . . ?
C4 C5 C13 C16A -1.7(3) . . . . ?
C4 C5 C13 C14B 96.7(3) . . . . ?
C4 C5 C13 C15B -142.1(2) . . . . ?
C4 C5 C13 C16B -25.3(3) . . . . ?
C4 C5 C13 C14C 52.7(6) . . . . ?
C4 C5 C13 C16C -58.8(6) . . . . ?
C4 C5 C13 C15C 178.7(7) . . . . ?
C5 C6 C7 C2 -0.9(2) . . . . ?
C5 C6 C7 C8 176.06(12) . . . . ?
C6 C5 C13 C14A -60.1(3) . . . . ?
C6 C5 C13 C15A 53.2(3) . . . . ?
C6 C5 C13 C16A 179.5(3) . . . . ?
C6 C5 C13 C14B -82.1(3) . . . . ?
C6 C5 C13 C15B 39.2(3) . . . . ?
C6 C5 C13 C16B 155.9(2) . . . . ?
C6 C5 C13 C14C -126.1(5) . . . . ?
C6 C5 C13 C16C 122.4(6) . . . . ?
C6 C5 C13 C15C -0.1(7) . . . . ?
C6 C7 C8 N1 127.87(13) . . . . ?
C7 C2 C3 C4 -1.1(2) . . . . ?
C7 C2 C3 C9 178.97(13) . . . . ?
C8 N1 C17 C18 -51.95(15) . . . . ?
C8 N1 C22 C23 -175.87(11) . . . . ?
C9 C3 C4 C5 -179.77(14) . . . . ?
C13 C5 C6 C7 178.91(14) . . . . ?
C17 N1 C8 C7 -57.62(14) . . . . ?
C17 N1 C22 C23 63.22(15) . . . . ?
C17 C18 C19 C20 179.56(15) . . . . ?
C18 O3 C21 C20 0.1(2) . . . . ?
C18 C19 C20 C21 -0.2(2) . . . . ?
C19 C20 C21 O3 0.0(2) . . . . ?
C21 O3 C18 C17 -179.63(14) . . . . ?
C21 O3 C18 C19 -0.20(19) . . . . ?
C22 N1 C8 C7 -179.18(11) . . . . ?
C22 N1 C17 C18 67.00(15) . . . . ?
C22 C23 C24 C25 177.61(15) . . . . ?
C23 O4 C26 C25 0.48(19) . . . . ?
C23 C24 C25 C26 -0.11(19) . . . . ?
C24 C25 C26 O4 -0.2(2) . . . . ?
C26 O4 C23 C22 -178.26(13) . . . . ?
C26 O4 C23 C24 -0.55(17) . . . . ?
_shelx_SHELXL_version_number 2014/7
_iucr_refine_instructions_details
;
mo_kpjk60010701_alotbume_tbufuran_0m_a.res created by SHELXL-2014/7
TITL mo_KPJK60010701_AlOtBuMe_tBufuran_0m_a.res in P-1
REM Old TITL mo_KPJK60010701_AlOtBuMe_tBufu in P-1
REM SHELXT solution in P-1
REM R1 0.141, Rweak 0.010, Alpha 0.056, Orientation as input
REM Formula found by SHELXT: C31 Al O4
REM #####
CELL 0.71073 10.0983 10.771 14.5991 105.627 97.157 96.551
ZERR 2 0.0045 0.004 0.0075 0.016 0.023 0.013
LATT 1
SFAC C H Al O N
UNIT 60 88 2 8 2
SADI 0.04 C14B C15B C14C C16C
SADI C13 C15C C13 C16A C13 C14B C13 C15A C13 C5 C13 C15B C13 C16B C13 C14C =
C13 C14A C13 C16C
SADI C16C C14C C14C C15C
SIMU C13 C14A C15A C16A
SIMU C13 C14B C15B C16B
SIMU C13 C14C C15C C16C
RIGU 0.0001 0.0001 C13 C14A C15A C16A C14B C15B C16B C14C C15C C16C
SUMP 1 0.0001 1 2 1 3 1 4
L.S. 20
PLAN 20
TEMP -123.15
BOND $H
LIST 4
MORE -1
CONF
fmap 2
acta
OMIT -1 0 1
OMIT -1 1 0
REM
REM
REM
WGHT 0.064300 0.908200
FVAR 1.25684 0.42353 0.45164 0.12480
AL1 3 0.749975 0.691676 0.309587 11.00000 0.01937 0.01883 =
0.02165 0.00456 0.00062 0.00024
N1 5 0.755104 0.508263 0.320936 11.00000 0.01616 0.02280 =
0.01846 0.00662 0.00104 0.00194
O1 4 0.788769 0.786834 0.426858 11.00000 0.02562 0.03499 =
0.02759 -0.00510 -0.00079 0.00796
O2 4 0.577566 0.670942 0.262787 11.00000 0.02310 0.01876 =
0.03571 0.00847 -0.00745 -0.00187
O3 4 0.855323 0.231696 0.282415 11.00000 0.03462 0.03080 =
0.05404 0.01831 -0.00305 0.00465
O4 4 1.074887 0.474592 0.357579 11.00000 0.02050 0.03428 =
0.03468 0.00339 0.00550 0.00312
C1 1 0.868648 0.726349 0.220392 11.00000 0.03976 0.03175 =
0.03978 0.01690 0.01374 0.00439
AFIX 137
H1A 2 0.863081 0.813623 0.213318 11.00000 -1.50000
H1B 2 0.840446 0.661146 0.157439 11.00000 -1.50000
H1C 2 0.961923 0.721663 0.245695 11.00000 -1.50000
AFIX 0
C2 1 0.486350 0.560652 0.226503 11.00000 0.01813 0.01965 =
0.02207 0.00482 0.00145 0.00110
C3 1 0.373641 0.553024 0.155700 11.00000 0.01997 0.02302 =
0.02167 0.00794 0.00146 0.00277
C4 1 0.284374 0.435032 0.121927 11.00000 0.01971 0.02784 =
0.02143 0.00743 -0.00096 -0.00004
AFIX 43
H4 2 0.208845 0.429034 0.074258 11.00000 -1.20000
AFIX 0
C5 1 0.299476 0.325513 0.153989 11.00000 0.02030 0.02445 =
0.02296 0.00612 0.00211 -0.00272
C6 1 0.411072 0.336955 0.224345 11.00000 0.02076 0.02130 =
0.02401 0.00867 0.00380 0.00089
AFIX 43
H6 2 0.424737 0.264521 0.247850 11.00000 -1.20000
AFIX 0
C7 1 0.503015 0.452542 0.260901 11.00000 0.01724 0.02251 =
0.01933 0.00616 0.00188 0.00211
C8 1 0.617342 0.463798 0.341532 11.00000 0.01680 0.02383 =
0.02137 0.00881 0.00180 0.00124
AFIX 23
H8A 2 0.600851 0.526287 0.400943 11.00000 -1.20000
H8B 2 0.617214 0.377777 0.353831 11.00000 -1.20000
AFIX 0
C9 1 0.350599 0.670164 0.117445 11.00000 0.02591 0.02570 =
0.02986 0.01275 -0.00182 0.00296
C10 1 0.468270 0.702815 0.065934 11.00000 0.03503 0.04009 =
0.04382 0.02573 0.00373 0.00066
AFIX 137
H10A 2 0.553554 0.721873 0.110860 11.00000 -1.50000
H10B 2 0.454976 0.779161 0.043528 11.00000 -1.50000
H10C 2 0.471169 0.628191 0.010631 11.00000 -1.50000
AFIX 0
C11 1 0.338930 0.789340 0.200907 11.00000 0.04672 0.02990 =
0.04320 0.01113 -0.00211 0.01500
AFIX 137
H11A 2 0.261996 0.768267 0.231781 11.00000 -1.50000
H11B 2 0.325326 0.863370 0.175712 11.00000 -1.50000
H11C 2 0.422046 0.812185 0.248314 11.00000 -1.50000
AFIX 0
C12 1 0.219326 0.641351 0.044377 11.00000 0.03281 0.04267 =
0.04097 0.02302 -0.00967 0.00160
AFIX 137
H12A 2 0.223543 0.566602 -0.010482 11.00000 -1.50000
H12B 2 0.208571 0.717912 0.021673 11.00000 -1.50000
H12C 2 0.142245 0.621187 0.075397 11.00000 -1.50000
AFIX 0
C13 1 0.200099 0.196966 0.112855 11.00000 0.03216 0.02972 =
0.03728 0.00752 -0.00019 -0.00943
PART 1
C14A 1 0.285062 0.085135 0.063763 21.00000 0.03361 0.03082 =
0.03749 0.00795 0.00019 -0.00831
AFIX 137
H14A 2 0.223971 0.002317 0.035109 21.00000 -1.50000
H14B 2 0.354853 0.074802 0.112992 21.00000 -1.50000
H14C 2 0.327757 0.110639 0.013493 21.00000 -1.50000
AFIX 0
C15A 1 0.150898 0.154516 0.195990 21.00000 0.03322 0.03079 =
0.03809 0.00828 0.00054 -0.00848
AFIX 137
H15A 2 0.091357 0.070319 0.170536 21.00000 -1.50000
H15B 2 0.101095 0.219986 0.230835 21.00000 -1.50000
H15C 2 0.228630 0.145968 0.240015 21.00000 -1.50000
AFIX 0
C16A 1 0.085736 0.200391 0.039048 21.00000 0.03331 0.03092 =
0.03819 0.00791 -0.00072 -0.00897
AFIX 137
H16A 2 0.120029 0.207072 -0.019630 21.00000 -1.50000
H16B 2 0.041537 0.276065 0.064097 21.00000 -1.50000
H16C 2 0.020372 0.120290 0.024102 21.00000 -1.50000
AFIX 0
PART 0
C17 1 0.783310 0.416459 0.229779 11.00000 0.02366 0.02311 =
0.02048 0.00672 0.00401 0.00427
AFIX 23
H17A 2 0.723586 0.427607 0.174357 11.00000 -1.20000
H17B 2 0.877661 0.442562 0.222301 11.00000 -1.20000
AFIX 0
C18 1 0.764252 0.275132 0.224907 11.00000 0.02399 0.02502 =
0.02602 0.00671 0.00544 0.00561
C19 1 0.669724 0.174759 0.171039 11.00000 0.03624 0.03356 =
0.03364 0.00127 -0.00008 -0.00146
AFIX 43
H19 2 0.595591 0.178041 0.125257 11.00000 -1.20000
AFIX 0
C20 1 0.704715 0.060815 0.197498 11.00000 0.05385 0.02320 =
0.05036 0.00360 0.01521 -0.00217
AFIX 43
H20 2 0.657513 -0.025787 0.172362 11.00000 -1.20000
AFIX 0
C21 1 0.814899 0.100480 0.263309 11.00000 0.05128 0.02889 =
0.05917 0.01984 0.00877 0.00902
AFIX 43
H21 2 0.859876 0.045317 0.293255 11.00000 -1.20000
AFIX 0
C22 1 0.857227 0.512401 0.407381 11.00000 0.01771 0.02999 =
0.02092 0.01013 0.00003 0.00267
AFIX 23
H22A 2 0.830600 0.567628 0.466095 11.00000 -1.20000
H22B 2 0.854546 0.423090 0.413988 11.00000 -1.20000
AFIX 0
C23 1 0.998486 0.563834 0.401716 11.00000 0.01930 0.02936 =
0.02160 0.00872 0.00069 0.00470
C24 1 1.073834 0.683859 0.434931 11.00000 0.02304 0.03082 =
0.03645 0.00928 0.00043 0.00268
AFIX 43
H24 2 1.045267 0.762187 0.468421 11.00000 -1.20000
AFIX 0
C25 1 1.204560 0.669816 0.409838 11.00000 0.02328 0.04162 =
0.04184 0.01480 0.00377 -0.00309
AFIX 43
H25 2 1.279984 0.736975 0.423262 11.00000 -1.20000
AFIX 0
C26 1 1.200122 0.543240 0.363587 11.00000 0.01992 0.04905 =
0.03542 0.00866 0.00748 0.00158
AFIX 43
H26 2 1.273714 0.506253 0.338441 11.00000 -1.20000
AFIX 0
C27 1 0.731759 0.872693 0.497460 11.00000 0.02731 0.02879 =
0.02661 0.00000 0.00420 0.00298
C28 1 0.846415 0.943671 0.580555 11.00000 0.03877 0.04600 =
0.02686 -0.00332 0.00356 -0.00413
AFIX 137
H28A 2 0.887329 0.879700 0.606825 11.00000 -1.50000
H28B 2 0.810287 1.003531 0.631249 11.00000 -1.50000
H28C 2 0.915002 0.993205 0.556768 11.00000 -1.50000
AFIX 0
C29 1 0.669458 0.971050 0.454602 11.00000 0.05439 0.03880 =
0.04805 0.00670 0.00883 0.01867
AFIX 137
H29A 2 0.739277 1.020813 0.431994 11.00000 -1.50000
H29B 2 0.631053 1.030821 0.503937 11.00000 -1.50000
H29C 2 0.597964 0.924789 0.400304 11.00000 -1.50000
AFIX 0
C30 1 0.623877 0.794863 0.533339 11.00000 0.03662 0.04298 =
0.05150 0.00523 0.01552 -0.00045
AFIX 137
H30A 2 0.550333 0.751058 0.479886 11.00000 -1.50000
H30B 2 0.588230 0.854105 0.584673 11.00000 -1.50000
H30C 2 0.663870 0.729505 0.558470 11.00000 -1.50000
AFIX 0
PART 2
C14B 1 0.256110 0.106687 0.036171 31.00000 0.03334 0.03139 =
0.03800 0.00735 0.00034 -0.00855
AFIX 137
H14D 2 0.192000 0.025598 0.008694 31.00000 -1.50000
H14E 2 0.341945 0.087101 0.063939 31.00000 -1.50000
H14F 2 0.271263 0.147923 -0.014608 31.00000 -1.50000
AFIX 0
C15B 1 0.174192 0.131698 0.192597 31.00000 0.03377 0.03103 =
0.03844 0.00862 0.00114 -0.00769
AFIX 137
H15D 2 0.104362 0.054756 0.165781 31.00000 -1.50000
H15E 2 0.143914 0.193818 0.245261 31.00000 -1.50000
H15F 2 0.257887 0.105170 0.217269 31.00000 -1.50000
AFIX 0
C16B 1 0.057483 0.224869 0.071635 31.00000 0.03228 0.03029 =
0.03811 0.00819 0.00012 -0.00930
AFIX 137
H16D 2 0.064459 0.253024 0.013702 31.00000 -1.50000
H16E 2 0.028432 0.293732 0.120409 31.00000 -1.50000
H16F 2 -0.008716 0.145124 0.055280 31.00000 -1.50000
AFIX 0
PART 0
PART 3
C14C 1 0.186429 0.155426 0.003561 41.00000 0.03289 0.02927 =
0.03738 0.00746 -0.00005 -0.00964
AFIX 137
H14G 2 0.274412 0.140085 -0.015092 41.00000 -1.50000
H14H 2 0.154828 0.224457 -0.021516 41.00000 -1.50000
H14I 2 0.121238 0.074960 -0.023156 41.00000 -1.50000
AFIX 0
C16C 1 0.055462 0.231316 0.132431 41.00000 0.03224 0.02941 =
0.03740 0.00730 -0.00023 -0.00961
AFIX 137
H16G 2 0.032832 0.298369 0.101779 41.00000 -1.50000
H16H 2 0.056577 0.264045 0.202042 41.00000 -1.50000
H16I 2 -0.012274 0.152729 0.105553 41.00000 -1.50000
AFIX 0
C15C 1 0.231604 0.089291 0.152608 41.00000 0.03316 0.03039 =
0.03787 0.00812 0.00046 -0.00870
AFIX 137
H15G 2 0.154335 0.018702 0.132501 41.00000 -1.50000
H15H 2 0.250331 0.121369 0.223143 41.00000 -1.50000
H15I 2 0.311037 0.056397 0.128542 41.00000 -1.50000
AFIX 0
HKLF 4
REM mo_KPJK60010701_AlOtBuMe_tBufuran_0m_a.res in P-1
REM R1 = 0.0514 for 6532 Fo > 4sig(Fo) and 0.0587 for all 7430 data
REM 398 parameters refined using 156 restraints
END
WGHT 0.0643 0.9082
REM Highest difference peak 0.750, deepest hole -0.476, 1-sigma level 0.048
Q1 1 0.1298 0.1775 0.0017 11.00000 0.05 0.75
Q2 1 0.6443 0.0969 0.1741 11.00000 0.05 0.44
Q3 1 0.2355 0.1457 0.0092 11.00000 0.05 0.42
Q4 1 0.4271 0.5586 0.1948 11.00000 0.05 0.39
Q5 1 0.0882 0.2025 0.1704 11.00000 0.05 0.36
Q6 1 0.5609 0.4593 0.2971 11.00000 0.05 0.35
Q7 1 0.4989 0.5011 0.2400 11.00000 0.05 0.33
Q8 1 0.7641 0.3474 0.2291 11.00000 0.05 0.32
Q9 1 0.3671 0.6108 0.1365 11.00000 0.05 0.32
Q10 1 0.7593 0.5972 0.3210 11.00000 0.05 0.30
Q11 1 0.3493 0.3386 0.1944 11.00000 0.05 0.29
Q12 1 0.6319 0.2170 0.1461 11.00000 0.05 0.29
Q13 1 0.2411 0.2596 0.1351 11.00000 0.05 0.29
Q14 1 0.8210 0.7134 0.2651 11.00000 0.05 0.29
Q15 1 0.3001 0.3775 0.1357 11.00000 0.05 0.28
Q16 1 0.1866 0.1702 0.2348 11.00000 0.05 0.28
Q17 1 0.3233 0.5001 0.1499 11.00000 0.05 0.28
Q18 1 0.2763 0.0821 0.1147 11.00000 0.05 0.28
Q19 1 0.9277 0.5451 0.3997 11.00000 0.05 0.27
Q20 1 0.3464 0.0770 0.0885 11.00000 0.05 0.27
REM The information below was added by Olex2.
REM
REM R1 = 0.0514 for 6532 Fo > 4sig(Fo) and 0.0587 for all 74898 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.75, deepest hole -0.48
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0587
REM R1_gt = 0.0514
REM wR_ref = 0.1343
REM GOOF = 1.028
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 74898
REM Reflections_gt = 6532
REM Parameters = n/a
REM Hole = -0.48
REM Peak = 0.75
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'