#------------------------------------------------------------------------------
#$Date: 2021-11-06 21:19:01 +0200 (Sat, 06 Nov 2021) $
#$Revision: 270408 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/90/7129089.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7129089
loop_
_publ_author_name
'Brown, Ryan K.'
'Hooper, Thomas N.'
'Rekhroukh, Feriel'
'White, Andrew J. P.'
'Costa, Paulo J.'
'Crimmin, Mark R.'
_publ_section_title
;
 Alumination of aryl methyl ethers: switching between sp² and
 sp³ C-O bond functionalisation with Pd-catalysis.
;
_journal_issue                   88
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11673
_journal_page_last               11676
_journal_paper_doi               10.1039/d1cc05408b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C36 H49 Al N2 O'
_chemical_formula_sum            'C36 H49 Al N2 O'
_chemical_formula_weight         552.75
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-19 deposited with the CCDC.	2021-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.380(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1329(4)
_cell_length_b                   36.3892(15)
_cell_length_c                   10.2426(4)
_cell_measurement_reflns_used    3114
_cell_measurement_temperature    173.05(10)
_cell_measurement_theta_max      27.0570
_cell_measurement_theta_min      3.0590
_cell_volume                     3382.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.797
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  50.00   1.00    4.96    --  -13.18  57.00-120.00   80
  2  ω    -78.00   4.00   1.00    4.96    --  -13.18 -37.00  60.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0517224000
_diffrn_orient_matrix_UB_12      -0.0120237000
_diffrn_orient_matrix_UB_13      0.0346343000
_diffrn_orient_matrix_UB_21      0.0161350000
_diffrn_orient_matrix_UB_22      0.0135801000
_diffrn_orient_matrix_UB_23      0.0491460000
_diffrn_orient_matrix_UB_31      -0.0563175000
_diffrn_orient_matrix_UB_32      -0.0071457000
_diffrn_orient_matrix_UB_33      0.0351951000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.797
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11733
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.364
_diffrn_reflns_theta_min         2.508
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: heptane'
_exptl_crystal_size_max          0.605
_exptl_crystal_size_mid          0.348
_exptl_crystal_size_min          0.256
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         6749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0633P)²+0.7177P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5004
_reflns_number_total             6749
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc05408b3.cif
_cod_data_source_block           9a
_cod_depositor_comments
'Adding full bibliography for 7129089--7129093.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7129089
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C36H49AlN2O
_chemical_oxdiff_usercomment     TH481
_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.
;
_reflns_odcompleteness_completeness 98.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_olex2_date_sample_data_collection 2019-09-04
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.056
_oxdiff_exptl_absorpt_empirical_full_min 0.935
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.54106(7) 0.37757(2) 0.43600(6) 0.02216(18) Uani 1 1 d . . . . .
O31 O 0.57113(17) 0.34719(4) 0.56598(14) 0.0306(4) Uani 1 1 d . . . . .
N1 N 0.50577(19) 0.35144(5) 0.27647(16) 0.0226(4) Uani 1 1 d . . . . .
N3 N 0.72255(19) 0.39909(5) 0.40245(17) 0.0230(4) Uani 1 1 d . . . . .
C1 C 0.6203(2) 0.33890(6) 0.2166(2) 0.0242(5) Uani 1 1 d . . . . .
C2 C 0.7635(2) 0.35175(6) 0.2487(2) 0.0263(5) Uani 1 1 d . . . . .
H2 H 0.836876 0.338689 0.212826 0.032 Uiso 1 1 calc R . . . .
C3 C 0.8114(2) 0.38171(6) 0.3277(2) 0.0249(5) Uani 1 1 d . . . . .
C4 C 0.5950(3) 0.31047(7) 0.1104(2) 0.0362(6) Uani 1 1 d . . . . .
H4A H 0.553386 0.288817 0.145111 0.054 Uiso 1 1 calc GR . . . .
H4B H 0.687083 0.304385 0.078795 0.054 Uiso 1 1 calc GR . . . .
H4C H 0.528350 0.320011 0.039426 0.054 Uiso 1 1 calc GR . . . .
C5 C 0.9680(3) 0.39371(7) 0.3249(3) 0.0367(6) Uani 1 1 d . . . . .
H5A H 0.981034 0.417771 0.362894 0.055 Uiso 1 1 calc GR . . . .
H5B H 0.990820 0.394358 0.235679 0.055 Uiso 1 1 calc GR . . . .
H5C H 1.032599 0.376695 0.374418 0.055 Uiso 1 1 calc GR . . . .
C6 C 0.3597(2) 0.34264(6) 0.2138(2) 0.0251(5) Uani 1 1 d . . . . .
C7 C 0.2995(3) 0.36479(7) 0.1089(2) 0.0333(6) Uani 1 1 d . . . . .
C8 C 0.1668(3) 0.35387(7) 0.0397(2) 0.0385(6) Uani 1 1 d . . . . .
H8 H 0.126960 0.367808 -0.031664 0.046 Uiso 1 1 calc R . . . .
C9 C 0.0933(3) 0.32315(7) 0.0739(2) 0.0372(6) Uani 1 1 d . . . . .
H9 H 0.006612 0.315913 0.024396 0.045 Uiso 1 1 calc R . . . .
C10 C 0.1487(3) 0.30304(7) 0.1823(2) 0.0340(6) Uani 1 1 d . . . . .
H10 H 0.096276 0.282812 0.207410 0.041 Uiso 1 1 calc R . . . .
C11 C 0.2821(2) 0.31235(6) 0.2553(2) 0.0268(5) Uani 1 1 d . . . . .
C12 C 0.3747(3) 0.39969(8) 0.0693(3) 0.0482(8) Uani 1 1 d . . . . .
H12 H 0.458211 0.404554 0.135774 0.058 Uiso 1 1 calc R . . . .
C13 C 0.4346(4) 0.39607(10) -0.0631(4) 0.0753(11) Uani 1 1 d . . . . .
H13A H 0.508009 0.377100 -0.058191 0.113 Uiso 1 1 calc GR . . . .
H13B H 0.477767 0.418970 -0.085281 0.113 Uiso 1 1 calc GR . . . .
H13C H 0.355611 0.389864 -0.129256 0.113 Uiso 1 1 calc GR . . . .
C14 C 0.2710(4) 0.43253(8) 0.0666(3) 0.0660(9) Uani 1 1 d . . . . .
H14A H 0.189676 0.428811 0.000069 0.099 Uiso 1 1 calc GR . . . .
H14B H 0.323165 0.454424 0.047253 0.099 Uiso 1 1 calc GR . . . .
H14C H 0.234866 0.435048 0.150598 0.099 Uiso 1 1 calc GR . . . .
C15 C 0.3333(3) 0.29100(6) 0.3786(2) 0.0335(6) Uani 1 1 d . . . . .
H15 H 0.438134 0.296234 0.402159 0.040 Uiso 1 1 calc R . . . .
C16 C 0.2501(3) 0.30411(9) 0.4909(3) 0.0523(8) Uani 1 1 d . . . . .
H16A H 0.266581 0.329946 0.504477 0.078 Uiso 1 1 calc GR . . . .
H16B H 0.284759 0.290988 0.569595 0.078 Uiso 1 1 calc GR . . . .
H16C H 0.146690 0.299639 0.469243 0.078 Uiso 1 1 calc GR . . . .
C17 C 0.3155(3) 0.24952(7) 0.3612(3) 0.0562(8) Uani 1 1 d . . . . .
H17A H 0.212893 0.243612 0.342414 0.084 Uiso 1 1 calc GR . . . .
H17B H 0.355140 0.237313 0.440390 0.084 Uiso 1 1 calc GR . . . .
H17C H 0.367382 0.241543 0.289675 0.084 Uiso 1 1 calc GR . . . .
C18 C 0.7701(2) 0.43306(6) 0.4687(2) 0.0271(5) Uani 1 1 d . . . . .
C19 C 0.8434(3) 0.43175(7) 0.5967(2) 0.0332(6) Uani 1 1 d . . . . .
C20 C 0.8816(3) 0.46508(8) 0.6589(3) 0.0453(7) Uani 1 1 d . . . . .
H20 H 0.929953 0.464906 0.743766 0.054 Uiso 1 1 calc R . . . .
C21 C 0.8493(3) 0.49797(8) 0.5979(3) 0.0506(8) Uani 1 1 d . . . . .
H21 H 0.875966 0.519854 0.641037 0.061 Uiso 1 1 calc R . . . .
C22 C 0.7779(3) 0.49866(7) 0.4734(3) 0.0458(7) Uani 1 1 d . . . . .
H22 H 0.757520 0.521232 0.432801 0.055 Uiso 1 1 calc R . . . .
C23 C 0.7349(3) 0.46679(6) 0.4059(3) 0.0344(6) Uani 1 1 d . . . . .
C24 C 0.8856(3) 0.39591(7) 0.6662(2) 0.0398(6) Uani 1 1 d . . . . .
H24 H 0.847968 0.375778 0.608387 0.048 Uiso 1 1 calc R . . . .
C25 C 1.0533(3) 0.39172(9) 0.6918(3) 0.0575(8) Uani 1 1 d . . . . .
H25A H 1.095755 0.394585 0.610765 0.086 Uiso 1 1 calc GR . . . .
H25B H 1.076924 0.367788 0.727572 0.086 Uiso 1 1 calc GR . . . .
H25C H 1.092307 0.410163 0.753089 0.086 Uiso 1 1 calc GR . . . .
C26 C 0.8172(4) 0.39220(9) 0.7945(3) 0.0596(9) Uani 1 1 d . . . . .
H26A H 0.858027 0.410500 0.855495 0.089 Uiso 1 1 calc GR . . . .
H26B H 0.837874 0.368194 0.830800 0.089 Uiso 1 1 calc GR . . . .
H26C H 0.712499 0.395560 0.778003 0.089 Uiso 1 1 calc GR . . . .
C27 C 0.6535(3) 0.46887(7) 0.2691(3) 0.0495(8) Uani 1 1 d . . . . .
H27 H 0.599655 0.445724 0.253047 0.059 Uiso 1 1 calc R . . . .
C28 C 0.5411(4) 0.49981(9) 0.2524(4) 0.0753(11) Uani 1 1 d . . . . .
H28A H 0.476851 0.498223 0.320219 0.113 Uiso 1 1 calc GR . . . .
H28B H 0.484251 0.497711 0.168050 0.113 Uiso 1 1 calc GR . . . .
H28C H 0.591280 0.523035 0.258255 0.113 Uiso 1 1 calc GR . . . .
C29 C 0.7593(5) 0.47221(12) 0.1653(3) 0.0920(13) Uani 1 1 d . . . . .
H29A H 0.812260 0.494966 0.176864 0.138 Uiso 1 1 calc GR . . . .
H29B H 0.704767 0.471685 0.079543 0.138 Uiso 1 1 calc GR . . . .
H29C H 0.827588 0.452075 0.173727 0.138 Uiso 1 1 calc GR . . . .
C30 C 0.3896(3) 0.41277(7) 0.4672(3) 0.0376(6) Uani 1 1 d . . . . .
H30A H 0.295200 0.403607 0.430883 0.056 Uiso 1 1 calc GR . . . .
H30B H 0.408931 0.435716 0.426169 0.056 Uiso 1 1 calc GR . . . .
H30C H 0.389625 0.416425 0.560033 0.056 Uiso 1 1 calc GR . . . .
C32 C 0.6520(2) 0.31891(6) 0.6190(2) 0.0264(5) Uani 1 1 d . . . . .
C33 C 0.7680(3) 0.30360(6) 0.5600(2) 0.0331(6) Uani 1 1 d . . . . .
H33 H 0.789244 0.312195 0.478741 0.040 Uiso 1 1 calc R . . . .
C34 C 0.8516(3) 0.27563(7) 0.6220(3) 0.0420(7) Uani 1 1 d . . . . .
H34 H 0.929606 0.265809 0.582348 0.050 Uiso 1 1 calc R . . . .
C35 C 0.8208(3) 0.26207(7) 0.7419(3) 0.0406(6) Uani 1 1 d . . . . .
H35 H 0.878365 0.243553 0.783835 0.049 Uiso 1 1 calc R . . . .
C36 C 0.7036(3) 0.27645(7) 0.7982(2) 0.0408(6) Uani 1 1 d . . . . .
H36 H 0.680276 0.267054 0.877816 0.049 Uiso 1 1 calc R . . . .
C37 C 0.6199(3) 0.30459(6) 0.7385(2) 0.0329(6) Uani 1 1 d . . . . .
H37 H 0.541469 0.314071 0.778434 0.039 Uiso 1 1 calc R . . . .
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -5 -3 0.1229
3 5 -3 0.1289
-3 -5 3 0.1289
1 5 1 0.1218
-3 5 3 0.0919
0 1 0 0.1814
3 -5 -3 0.2185
0 -1 0 0.2460
1 5 3 0.1246
2 5 2 0.1234
-1 -5 1 0.1761
4 0 5 0.1051
-5 -3 0 0.1883
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
O31 Al1 N1 109.99(8) . . ?
O31 Al1 N3 109.63(8) . . ?
O31 Al1 C30 110.54(10) . . ?
N1 Al1 N3 96.87(8) . . ?
N1 Al1 C30 114.80(10) . . ?
N3 Al1 C30 114.25(10) . . ?
C32 O31 Al1 146.42(15) . . ?
C1 N1 Al1 119.83(14) . . ?
C1 N1 C6 116.43(18) . . ?
C6 N1 Al1 123.70(14) . . ?
C3 N3 Al1 120.44(15) . . ?
C3 N3 C18 120.09(18) . . ?
C18 N3 Al1 119.23(13) . . ?
N1 C1 C2 122.25(19) . . ?
N1 C1 C4 119.85(19) . . ?
C2 C1 C4 117.9(2) . . ?
C1 C2 H2 115.7 . . ?
C1 C2 C3 128.6(2) . . ?
C3 C2 H2 115.7 . . ?
N3 C3 C2 122.0(2) . . ?
N3 C3 C5 121.0(2) . . ?
C2 C3 C5 117.02(19) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N1 118.31(19) . . ?
C11 C6 N1 120.70(19) . . ?
C11 C6 C7 121.0(2) . . ?
C6 C7 C12 122.2(2) . . ?
C8 C7 C6 118.0(2) . . ?
C8 C7 C12 119.8(2) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 C7 121.8(2) . . ?
C9 C8 H8 119.1 . . ?
C8 C9 H9 120.2 . . ?
C8 C9 C10 119.6(2) . . ?
C10 C9 H9 120.2 . . ?
C9 C10 H10 119.3 . . ?
C9 C10 C11 121.5(2) . . ?
C11 C10 H10 119.3 . . ?
C6 C11 C15 122.5(2) . . ?
C10 C11 C6 117.9(2) . . ?
C10 C11 C15 119.5(2) . . ?
C7 C12 H12 107.8 . . ?
C7 C12 C13 112.5(3) . . ?
C7 C12 C14 111.2(3) . . ?
C13 C12 H12 107.8 . . ?
C14 C12 H12 107.8 . . ?
C14 C12 C13 109.6(2) . . ?
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 . . ?
C11 C15 H15 108.0 . . ?
C11 C15 C16 109.6(2) . . ?
C11 C15 C17 113.0(2) . . ?
C16 C15 H15 108.0 . . ?
C16 C15 C17 110.0(2) . . ?
C17 C15 H15 108.0 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 N3 119.6(2) . . ?
C19 C18 C23 121.2(2) . . ?
C23 C18 N3 119.2(2) . . ?
C18 C19 C24 122.5(2) . . ?
C20 C19 C18 117.7(2) . . ?
C20 C19 C24 119.7(2) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.4(3) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.0(3) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 119.0 . . ?
C21 C22 C23 122.0(3) . . ?
C23 C22 H22 119.0 . . ?
C18 C23 C27 122.1(2) . . ?
C22 C23 C18 117.7(2) . . ?
C22 C23 C27 120.2(2) . . ?
C19 C24 H24 107.8 . . ?
C19 C24 C25 111.3(2) . . ?
C19 C24 C26 112.0(2) . . ?
C25 C24 H24 107.8 . . ?
C26 C24 H24 107.8 . . ?
C26 C24 C25 110.0(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C27 H27 107.3 . . ?
C23 C27 C28 113.4(3) . . ?
C23 C27 C29 111.6(3) . . ?
C28 C27 H27 107.3 . . ?
C29 C27 H27 107.3 . . ?
C29 C27 C28 109.6(3) . . ?
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 . . ?
Al1 C30 H30A 109.5 . . ?
Al1 C30 H30B 109.5 . . ?
Al1 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O31 C32 C33 122.7(2) . . ?
O31 C32 C37 118.8(2) . . ?
C37 C32 C33 118.5(2) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 C32 120.2(2) . . ?
C34 C33 H33 119.9 . . ?
C33 C34 H34 119.5 . . ?
C35 C34 C33 120.9(2) . . ?
C35 C34 H34 119.5 . . ?
C34 C35 H35 120.6 . . ?
C36 C35 C34 118.8(2) . . ?
C36 C35 H35 120.6 . . ?
C35 C36 H36 119.5 . . ?
C35 C36 C37 121.0(2) . . ?
C37 C36 H36 119.5 . . ?
C32 C37 H37 119.7 . . ?
C36 C37 C32 120.5(2) . . ?
C36 C37 H37 119.7 . . ?
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 O31 1.7288(16) . ?
Al1 N1 1.8871(18) . ?
Al1 N3 1.8988(18) . ?
Al1 C30 1.938(2) . ?
O31 C32 1.346(3) . ?
N1 C1 1.350(3) . ?
N1 C6 1.450(3) . ?
N3 C3 1.335(3) . ?
N3 C18 1.453(3) . ?
C1 C2 1.393(3) . ?
C1 C4 1.500(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.399(3) . ?
C3 C5 1.499(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.405(3) . ?
C6 C11 1.402(3) . ?
C7 C8 1.392(3) . ?
C7 C12 1.520(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.369(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.378(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.398(3) . ?
C11 C15 1.512(3) . ?
C12 H12 0.9800 . ?
C12 C13 1.523(4) . ?
C12 C14 1.523(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15 0.9800 . ?
C15 C16 1.523(4) . ?
C15 C17 1.527(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.405(3) . ?
C18 C23 1.406(3) . ?
C19 C20 1.397(3) . ?
C19 C24 1.515(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.367(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.366(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.385(3) . ?
C23 C27 1.513(4) . ?
C24 H24 0.9800 . ?
C24 C25 1.533(4) . ?
C24 C26 1.522(4) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27 0.9800 . ?
C27 C28 1.520(4) . ?
C27 C29 1.519(5) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C32 C33 1.393(3) . ?
C32 C37 1.391(3) . ?
C33 H33 0.9300 . ?
C33 C34 1.384(3) . ?
C34 H34 0.9300 . ?
C34 C35 1.381(3) . ?
C35 H35 0.9300 . ?
C35 C36 1.375(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.379(3) . ?
C37 H37 0.9300 . ?
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 O31 C32 C33 1.0(4) . . . . ?
Al1 O31 C32 C37 -179.76(19) . . . . ?
Al1 N1 C1 C2 -16.2(3) . . . . ?
Al1 N1 C1 C4 164.57(16) . . . . ?
Al1 N1 C6 C7 99.8(2) . . . . ?
Al1 N1 C6 C11 -81.4(2) . . . . ?
Al1 N3 C3 C2 14.2(3) . . . . ?
Al1 N3 C3 C5 -165.91(17) . . . . ?
Al1 N3 C18 C19 83.3(2) . . . . ?
Al1 N3 C18 C23 -93.3(2) . . . . ?
O31 Al1 N1 C1 -82.87(17) . . . . ?
O31 Al1 N1 C6 95.11(17) . . . . ?
O31 Al1 N3 C3 83.90(17) . . . . ?
O31 Al1 N3 C18 -90.48(16) . . . . ?
O31 C32 C33 C34 177.1(2) . . . . ?
O31 C32 C37 C36 -177.8(2) . . . . ?
N1 Al1 O31 C32 56.5(3) . . . . ?
N1 Al1 N3 C3 -30.22(17) . . . . ?
N1 Al1 N3 C18 155.40(16) . . . . ?
N1 C1 C2 C3 -10.2(4) . . . . ?
N1 C6 C7 C8 173.0(2) . . . . ?
N1 C6 C7 C12 -6.7(3) . . . . ?
N1 C6 C11 C10 -173.44(19) . . . . ?
N1 C6 C11 C15 9.8(3) . . . . ?
N3 Al1 O31 C32 -48.9(3) . . . . ?
N3 Al1 N1 C1 30.95(17) . . . . ?
N3 Al1 N1 C6 -151.06(16) . . . . ?
N3 C18 C19 C20 -177.3(2) . . . . ?
N3 C18 C19 C24 4.6(3) . . . . ?
N3 C18 C23 C22 178.0(2) . . . . ?
N3 C18 C23 C27 -2.3(3) . . . . ?
C1 N1 C6 C7 -82.2(3) . . . . ?
C1 N1 C6 C11 96.6(2) . . . . ?
C1 C2 C3 N3 11.3(4) . . . . ?
C1 C2 C3 C5 -168.6(2) . . . . ?
C3 N3 C18 C19 -91.1(3) . . . . ?
C3 N3 C18 C23 92.3(3) . . . . ?
C4 C1 C2 C3 169.1(2) . . . . ?
C6 N1 C1 C2 165.71(19) . . . . ?
C6 N1 C1 C4 -13.6(3) . . . . ?
C6 C7 C8 C9 2.0(4) . . . . ?
C6 C7 C12 C13 110.9(3) . . . . ?
C6 C7 C12 C14 -125.8(3) . . . . ?
C6 C11 C15 C16 98.2(3) . . . . ?
C6 C11 C15 C17 -138.6(2) . . . . ?
C7 C6 C11 C10 5.3(3) . . . . ?
C7 C6 C11 C15 -171.5(2) . . . . ?
C7 C8 C9 C10 2.3(4) . . . . ?
C8 C7 C12 C13 -68.8(3) . . . . ?
C8 C7 C12 C14 54.5(3) . . . . ?
C8 C9 C10 C11 -2.8(4) . . . . ?
C9 C10 C11 C6 -1.0(3) . . . . ?
C9 C10 C11 C15 175.9(2) . . . . ?
C10 C11 C15 C16 -78.5(3) . . . . ?
C10 C11 C15 C17 44.6(3) . . . . ?
C11 C6 C7 C8 -5.8(3) . . . . ?
C11 C6 C7 C12 174.5(2) . . . . ?
C12 C7 C8 C9 -178.3(3) . . . . ?
C18 N3 C3 C2 -171.4(2) . . . . ?
C18 N3 C3 C5 8.4(3) . . . . ?
C18 C19 C20 C21 -0.1(4) . . . . ?
C18 C19 C24 C25 114.9(3) . . . . ?
C18 C19 C24 C26 -121.5(3) . . . . ?
C18 C23 C27 C28 141.0(3) . . . . ?
C18 C23 C27 C29 -94.6(3) . . . . ?
C19 C18 C23 C22 1.5(3) . . . . ?
C19 C18 C23 C27 -178.8(2) . . . . ?
C19 C20 C21 C22 0.2(4) . . . . ?
C20 C19 C24 C25 -63.2(3) . . . . ?
C20 C19 C24 C26 60.4(3) . . . . ?
C20 C21 C22 C23 0.6(4) . . . . ?
C21 C22 C23 C18 -1.4(4) . . . . ?
C21 C22 C23 C27 178.9(3) . . . . ?
C22 C23 C27 C28 -39.3(4) . . . . ?
C22 C23 C27 C29 85.0(3) . . . . ?
C23 C18 C19 C20 -0.7(3) . . . . ?
C23 C18 C19 C24 -178.8(2) . . . . ?
C24 C19 C20 C21 178.0(2) . . . . ?
C30 Al1 O31 C32 -175.7(3) . . . . ?
C30 Al1 N1 C1 151.71(16) . . . . ?
C30 Al1 N1 C6 -30.3(2) . . . . ?
C30 Al1 N3 C3 -151.40(17) . . . . ?
C30 Al1 N3 C18 34.22(19) . . . . ?
C32 C33 C34 C35 0.9(4) . . . . ?
C33 C32 C37 C36 1.5(4) . . . . ?
C33 C34 C35 C36 1.1(4) . . . . ?
C34 C35 C36 C37 -1.7(4) . . . . ?
C35 C36 C37 C32 0.4(4) . . . . ?
C37 C32 C33 C34 -2.1(4) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0015 -4.9942 -2.9967 -0.0438 -0.2151 -0.0697
2.9989 4.9859 -3.0024 -0.0088 -0.0315 -0.3102
-2.9989 -4.9859 3.0024 0.0088 0.0315 0.3102
1.0007 4.9914 0.9970 0.0263 0.1329 -0.0569
-2.9979 5.0057 3.0024 -0.1113 0.1672 0.2387
0.0001 0.9992 0.0000 -0.0120 0.0136 -0.0071
2.9979 -5.0057 -3.0024 0.1113 -0.1672 -0.2387
-0.0001 -0.9992 -0.0000 0.0120 -0.0136 0.0071
1.0014 4.9903 2.9948 0.0955 0.2311 0.0133
2.0008 4.9870 1.9940 0.1126 0.1980 -0.0781
-0.9999 -4.9925 1.0008 0.0430 -0.0347 0.1272
4.0010 -0.0183 4.9869 0.3799 0.3094 -0.0497
-4.9994 -2.9782 0.0095 -0.2224 -0.1206 0.3032
