#------------------------------------------------------------------------------
#$Date: 2020-07-09 09:17:13 +0300 (Thu, 09 Jul 2020) $
#$Revision: 254136 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/85/1558547.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_1558547
loop_
_publ_author_name
'Hooper, Thomas'
'Brown, Ryan'
'Rekhroukh, Feriel'
'Garçon, Martí'
'White, Andrew J. P.'
'Costa, Paulo J.'
'Crimmin, Mark Richard'
_publ_section_title
;
 Catalyst Control of Selectivity in the C--O Bond Alumination of Biomass
 Derived Furans
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC01918F
_journal_year                    2020
_chemical_formula_moiety         'C34 H47 Al N2 O'
_chemical_formula_sum            'C34 H47 Al N2 O'
_chemical_formula_weight         526.71
_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             2018-08-01
_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.	2020-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 144.73(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.620(4)
_cell_length_b                   8.9532(3)
_cell_length_c                   32.557(7)
_cell_measurement_reflns_used    2685
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      72.8450
_cell_measurement_theta_min      4.0930
_cell_volume                     3134(4)
_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      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00  28.00   1.00   10.06    --  -41.98  38.00 120.00   91
  2  ω   -110.00 -22.00   1.00   10.06    --  -41.98 -38.00 -60.00   88
  3  ω     38.00 131.00   1.00   85.77    --  106.38 -61.00   0.00   93
  4  ω    109.00 178.00   1.00   85.77    --  106.38  45.00  30.00   69
  5  ω     89.00 174.00   1.00   85.77    --  106.38  77.00 120.00   85
  6  ω     33.00 121.00   1.00   85.77    --  106.38-125.00 -90.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1384201000
_diffrn_orient_matrix_UB_12      0.0344325000
_diffrn_orient_matrix_UB_13      0.0723063000
_diffrn_orient_matrix_UB_21      -0.0363056000
_diffrn_orient_matrix_UB_22      0.1469133000
_diffrn_orient_matrix_UB_23      0.0046049000
_diffrn_orient_matrix_UB_31      -0.0066121000
_diffrn_orient_matrix_UB_32      -0.0827757000
_diffrn_orient_matrix_UB_33      0.0383324000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9853
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.865
_diffrn_reflns_theta_min         4.111
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.918
_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_density_diffrn    1.116
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: heptane'
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0494
_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/[σ²(Fo²)+(0.0424P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3885
_reflns_number_total             6043
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc01918f3.cif
_cod_data_source_block           4b
_cod_original_cell_volume        3134(2)
_cod_database_code               1558547
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C34H47AlN2O
_chemical_oxdiff_usercomment     TH341
_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 98.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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. Uiso/Uaniso restraints and constraints
Uanis(O30) = Uanis(O30A)
Uanis(C31) = Uanis(C31A)
Uanis(C32) = Uanis(C32A)
Uanis(C33) = Uanis(C33A)
Uanis(C34) = Uanis(C34A)
Uanis(C35) = Uanis(C35A)
3. Others
 Sof(O30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=
 Sof(C34A)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(O30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C31(H31),
 C32(H32), C33(H33), C31A(H31A), C32A(H32A), C33A(H33A)
4.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), C35(H35A,H35B,H35C),
 C35A(H35D,H35E,H35F)
;
_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 1.111
_oxdiff_exptl_absorpt_empirical_full_min 0.898
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 0.33931(7) 0.43831(7) 0.28846(3) 0.03498(16) Uani 1 1 d . . . . .
N1 N 0.32170(16) 0.64223(18) 0.29378(9) 0.0264(3) Uani 1 1 d . . . . .
N3 N 0.23424(15) 0.44042(19) 0.19232(8) 0.0258(3) Uani 1 1 d . . . . .
C1 C 0.30455(19) 0.7433(2) 0.25597(11) 0.0278(4) Uani 1 1 d . . . . .
C2 C 0.2675(2) 0.7037(2) 0.19900(11) 0.0290(4) Uani 1 1 d . . . . .
H2 H 0.271849 0.780445 0.180933 0.035 Uiso 1 1 calc R . . . .
C3 C 0.22487(19) 0.5651(2) 0.16540(10) 0.0276(4) Uani 1 1 d . . . . .
C4 C 0.3255(2) 0.9063(2) 0.27430(12) 0.0361(5) Uani 1 1 d . . . . .
H4A H 0.283153 0.934038 0.280064 0.054 Uiso 1 1 calc GR . . . .
H4B H 0.292183 0.965808 0.236000 0.054 Uiso 1 1 calc GR . . . .
H4C H 0.414865 0.925388 0.318800 0.054 Uiso 1 1 calc GR . . . .
C5 C 0.1661(2) 0.5624(3) 0.09605(12) 0.0377(5) Uani 1 1 d . . . . .
H5A H 0.230825 0.548910 0.105378 0.057 Uiso 1 1 calc GR . . . .
H5B H 0.122558 0.656848 0.070841 0.057 Uiso 1 1 calc GR . . . .
H5C H 0.106744 0.479518 0.066746 0.057 Uiso 1 1 calc GR . . . .
C6 C 0.3288(2) 0.6965(2) 0.33916(11) 0.0275(4) Uani 1 1 d . . . . .
C7 C 0.2170(2) 0.7364(2) 0.30679(12) 0.0330(4) Uani 1 1 d . . . . .
C8 C 0.2249(2) 0.7968(3) 0.34975(14) 0.0448(6) Uani 1 1 d . . . . .
H8 H 0.150910 0.826150 0.328975 0.054 Uiso 1 1 calc R . . . .
C9 C 0.3381(3) 0.8149(3) 0.42198(14) 0.0499(6) Uani 1 1 d . . . . .
H9 H 0.341671 0.858055 0.450295 0.060 Uiso 1 1 calc R . . . .
C10 C 0.4456(2) 0.7704(3) 0.45288(12) 0.0441(6) Uani 1 1 d . . . . .
H10 H 0.522823 0.781159 0.502804 0.053 Uiso 1 1 calc R . . . .
C11 C 0.4442(2) 0.7098(2) 0.41266(11) 0.0330(4) Uani 1 1 d . . . . .
C12 C 0.0898(2) 0.7158(3) 0.22797(12) 0.0366(5) Uani 1 1 d . . . . .
H12 H 0.101912 0.664732 0.206580 0.044 Uiso 1 1 calc R . . . .
C13 C 0.0250(3) 0.8649(3) 0.18959(15) 0.0595(7) Uani 1 1 d . . . . .
H13A H 0.012280 0.917485 0.209704 0.089 Uiso 1 1 calc GR . . . .
H13B H -0.055600 0.846750 0.138826 0.089 Uiso 1 1 calc GR . . . .
H13C H 0.076878 0.926130 0.195647 0.089 Uiso 1 1 calc GR . . . .
C14 C 0.0068(3) 0.6166(4) 0.21556(16) 0.0565(7) Uani 1 1 d . . . . .
H14A H 0.048178 0.520649 0.239641 0.085 Uiso 1 1 calc GR . . . .
H14B H -0.072367 0.599715 0.164421 0.085 Uiso 1 1 calc GR . . . .
H14C H -0.008883 0.665758 0.234645 0.085 Uiso 1 1 calc GR . . . .
C15 C 0.5659(2) 0.6640(3) 0.44971(12) 0.0388(5) Uani 1 1 d . . . . .
H15 H 0.546089 0.618122 0.413244 0.047 Uiso 1 1 calc R . . . .
C16 C 0.6331(3) 0.5470(3) 0.50672(15) 0.0553(7) Uani 1 1 d . . . . .
H16A H 0.659675 0.591471 0.545205 0.083 Uiso 1 1 calc GR . . . .
H16B H 0.706050 0.510834 0.525751 0.083 Uiso 1 1 calc GR . . . .
H16C H 0.576769 0.463245 0.485924 0.083 Uiso 1 1 calc GR . . . .
C17 C 0.6504(3) 0.7979(3) 0.48152(16) 0.0554(7) Uani 1 1 d . . . . .
H17A H 0.606321 0.871804 0.444154 0.083 Uiso 1 1 calc GR . . . .
H17B H 0.725475 0.765016 0.502065 0.083 Uiso 1 1 calc GR . . . .
H17C H 0.673838 0.842996 0.518765 0.083 Uiso 1 1 calc GR . . . .
C18 C 0.17671(19) 0.3033(2) 0.15165(10) 0.0275(4) Uani 1 1 d . . . . .
C19 C 0.2350(2) 0.2137(2) 0.14887(11) 0.0302(4) Uani 1 1 d . . . . .
C20 C 0.1762(2) 0.0809(2) 0.11041(12) 0.0362(5) Uani 1 1 d . . . . .
H20 H 0.212976 0.019563 0.107110 0.043 Uiso 1 1 calc R . . . .
C21 C 0.0665(2) 0.0360(3) 0.07706(12) 0.0417(5) Uani 1 1 d . . . . .
H21 H 0.029263 -0.056028 0.051913 0.050 Uiso 1 1 calc R . . . .
C22 C 0.0103(2) 0.1256(3) 0.08031(12) 0.0379(5) Uani 1 1 d . . . . .
H22 H -0.065674 0.094280 0.056961 0.046 Uiso 1 1 calc R . . . .
C23 C 0.06336(19) 0.2602(2) 0.11712(10) 0.0297(4) Uani 1 1 d . . . . .
C24 C 0.3587(2) 0.2521(3) 0.18706(13) 0.0370(5) Uani 1 1 d . . . . .
H24 H 0.384894 0.352392 0.209721 0.044 Uiso 1 1 calc R . . . .
C25 C 0.4581(2) 0.1389(3) 0.24583(15) 0.0458(6) Uani 1 1 d . . . . .
H25A H 0.538335 0.168710 0.271578 0.069 Uiso 1 1 calc GR . . . .
H25B H 0.435182 0.039948 0.224727 0.069 Uiso 1 1 calc GR . . . .
H25C H 0.464638 0.135435 0.278880 0.069 Uiso 1 1 calc GR . . . .
C26 C 0.3501(3) 0.2609(3) 0.13604(17) 0.0552(7) Uani 1 1 d . . . . .
H26A H 0.330342 0.161915 0.115763 0.083 Uiso 1 1 calc GR . . . .
H26B H 0.429844 0.294842 0.162112 0.083 Uiso 1 1 calc GR . . . .
H26C H 0.284553 0.331565 0.097687 0.083 Uiso 1 1 calc GR . . . .
C27 C -0.0022(2) 0.3608(3) 0.11720(12) 0.0369(5) Uani 1 1 d . . . . .
H27 H 0.063348 0.414093 0.163926 0.044 Uiso 1 1 calc R . . . .
C28 C -0.0796(3) 0.4787(3) 0.05898(17) 0.0573(7) Uani 1 1 d . . . . .
H28A H -0.122564 0.540975 0.059234 0.086 Uiso 1 1 calc GR . . . .
H28B H -0.141053 0.429605 0.012641 0.086 Uiso 1 1 calc GR . . . .
H28C H -0.025015 0.541497 0.067659 0.086 Uiso 1 1 calc GR . . . .
C29 C -0.0835(3) 0.2758(3) 0.10968(15) 0.0503(6) Uani 1 1 d . . . . .
H29A H -0.151529 0.226562 0.063154 0.075 Uiso 1 1 calc GR . . . .
H29B H -0.118026 0.345773 0.113713 0.075 Uiso 1 1 calc GR . . . .
H29C H -0.033235 0.200479 0.147346 0.075 Uiso 1 1 calc GR . . . .
O30 O 0.4932(2) 0.4184(3) 0.33591(13) 0.0386(5) Uani 0.643(2) 1 d . . P A 1
C31 C 0.5781(5) 0.3169(5) 0.3884(2) 0.0411(9) Uani 0.643(2) 1 d . . P A 1
H31 H 0.656504 0.315446 0.411555 0.049 Uiso 0.643(2) 1 calc R . P A 1
C32 C 0.5598(5) 0.2209(4) 0.4094(2) 0.0478(9) Uani 0.643(2) 1 d . . P A 1
H32 H 0.625888 0.153395 0.445764 0.057 Uiso 0.643(2) 1 calc R . P A 1
C33 C 0.4506(5) 0.2061(6) 0.3836(3) 0.0376(12) Uani 0.643(2) 1 d . . P A 1
H33 H 0.452796 0.131425 0.405375 0.045 Uiso 0.643(2) 1 calc R . P A 1
C34 C 0.3439(4) 0.2887(4) 0.33099(19) 0.0373(7) Uani 0.643(2) 1 d . . P A 1
C35 C 0.2443(4) 0.2543(6) 0.3144(2) 0.0476(10) Uani 0.643(2) 1 d . . P A 1
H35A H 0.225473 0.343784 0.321825 0.071 Uiso 0.643(2) 1 calc GR . P A 1
H35B H 0.272096 0.174223 0.345785 0.071 Uiso 0.643(2) 1 calc GR . P A 1
H35C H 0.169446 0.222079 0.264782 0.071 Uiso 0.643(2) 1 calc GR . P A 1
O30A O 0.2443(4) 0.3419(5) 0.2872(2) 0.0386(5) Uani 0.357(2) 1 d . . P A 2
C31A C 0.2943(8) 0.2272(10) 0.3320(4) 0.0411(9) Uani 0.357(2) 1 d . . P A 2
H31A H 0.243403 0.185524 0.329172 0.049 Uiso 0.357(2) 1 calc R . P A 2
C32A C 0.3982(9) 0.1703(9) 0.3762(4) 0.0478(9) Uani 0.357(2) 1 d . . P A 2
H32A H 0.417681 0.089932 0.403194 0.057 Uiso 0.357(2) 1 calc R . P A 2
C33A C 0.4936(11) 0.2119(13) 0.3915(6) 0.0376(12) Uani 0.357(2) 1 d . . P A 2
H33A H 0.568366 0.155280 0.426369 0.045 Uiso 0.357(2) 1 calc R . P A 2
C34A C 0.4839(7) 0.3279(7) 0.3591(3) 0.0373(7) Uani 0.357(2) 1 d . . P A 2
C35A C 0.5955(10) 0.3556(11) 0.3850(6) 0.0476(10) Uani 0.357(2) 1 d . . P A 2
H35D H 0.568816 0.388282 0.345185 0.071 Uiso 0.357(2) 1 calc GR . P A 2
H35E H 0.643913 0.263348 0.405165 0.071 Uiso 0.357(2) 1 calc GR . P A 2
H35F H 0.646957 0.433490 0.421618 0.071 Uiso 0.357(2) 1 calc GR . P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 '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 0 -1 0.0220
-3 5 3 0.0684
0 0 1 0.0088
-1 0 2 0.0545
4 -5 -4 0.0489
5 0 -6 0.0719
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
N1 Al1 N3 96.83(8) . . ?
N1 Al1 O30A 102.05(14) . . ?
N3 Al1 O30A 105.93(16) . . ?
O30 Al1 N1 106.52(10) . . ?
O30 Al1 N3 100.74(12) . . ?
O30 Al1 C34 102.07(15) . . ?
C34 Al1 N1 121.94(12) . . ?
C34 Al1 N3 125.89(12) . . ?
C34A Al1 N1 126.1(2) . . ?
C34A Al1 N3 123.3(2) . . ?
C34A Al1 O30A 99.6(2) . . ?
C1 N1 Al1 119.85(13) . . ?
C1 N1 C6 117.60(16) . . ?
C6 N1 Al1 122.53(13) . . ?
C3 N3 Al1 119.60(14) . . ?
C3 N3 C18 120.31(16) . . ?
C18 N3 Al1 119.71(13) . . ?
N1 C1 C2 122.53(18) . . ?
N1 C1 C4 120.08(18) . . ?
C2 C1 C4 117.38(18) . . ?
C1 C2 H2 116.1 . . ?
C3 C2 C1 127.89(19) . . ?
C3 C2 H2 116.1 . . ?
N3 C3 C2 122.74(17) . . ?
N3 C3 C5 121.02(19) . . ?
C2 C3 C5 116.24(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 118.09(19) . . ?
C11 C6 N1 120.31(19) . . ?
C11 C6 C7 121.60(19) . . ?
C6 C7 C12 123.05(19) . . ?
C8 C7 C6 117.9(2) . . ?
C8 C7 C12 119.1(2) . . ?
C7 C8 H8 119.3 . . ?
C9 C8 C7 121.3(2) . . ?
C9 C8 H8 119.3 . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.9(2) . . ?
C10 C9 H9 120.1 . . ?
C9 C10 H10 119.2 . . ?
C9 C10 C11 121.6(2) . . ?
C11 C10 H10 119.2 . . ?
C6 C11 C15 123.21(19) . . ?
C10 C11 C6 117.6(2) . . ?
C10 C11 C15 119.1(2) . . ?
C7 C12 H12 107.8 . . ?
C7 C12 C13 112.1(2) . . ?
C7 C12 C14 111.3(2) . . ?
C13 C12 H12 107.8 . . ?
C14 C12 H12 107.8 . . ?
C14 C12 C13 109.8(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 107.7 . . ?
C11 C15 C16 111.3(2) . . ?
C11 C15 C17 111.8(2) . . ?
C16 C15 H15 107.7 . . ?
C16 C15 C17 110.4(2) . . ?
C17 C15 H15 107.7 . . ?
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 120.51(18) . . ?
C19 C18 C23 121.45(19) . . ?
C23 C18 N3 118.00(18) . . ?
C18 C19 C24 123.50(19) . . ?
C20 C19 C18 117.5(2) . . ?
C20 C19 C24 119.01(19) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 C19 122.0(2) . . ?
C21 C20 H20 119.0 . . ?
C20 C21 H21 120.1 . . ?
C20 C21 C22 119.7(2) . . ?
C22 C21 H21 120.1 . . ?
C21 C22 H22 119.4 . . ?
C21 C22 C23 121.2(2) . . ?
C23 C22 H22 119.4 . . ?
C18 C23 C27 121.19(19) . . ?
C22 C23 C18 118.1(2) . . ?
C22 C23 C27 120.6(2) . . ?
C19 C24 H24 108.0 . . ?
C19 C24 C25 110.7(2) . . ?
C19 C24 C26 112.2(2) . . ?
C25 C24 H24 108.0 . . ?
C25 C24 C26 109.8(2) . . ?
C26 C24 H24 108.0 . . ?
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 107.5 . . ?
C23 C27 C28 110.74(19) . . ?
C23 C27 C29 113.5(2) . . ?
C28 C27 H27 107.5 . . ?
C29 C27 H27 107.5 . . ?
C29 C27 C28 109.8(2) . . ?
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 . . ?
C31 O30 Al1 122.5(3) . . ?
O30 C31 H31 117.7 . . ?
C32 C31 O30 124.6(5) . . ?
C32 C31 H31 117.7 . . ?
C31 C32 H32 116.4 . . ?
C31 C32 C33 127.2(5) . . ?
C33 C32 H32 116.4 . . ?
C32 C33 H33 116.7 . . ?
C34 C33 C32 126.6(5) . . ?
C34 C33 H33 116.7 . . ?
C33 C34 Al1 117.0(3) . . ?
C33 C34 C35 116.8(4) . . ?
C35 C34 Al1 126.2(3) . . ?
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 . . ?
C31A O30A Al1 120.2(5) . . ?
O30A C31A H31A 116.1 . . ?
C32A C31A O30A 127.7(9) . . ?
C32A C31A H31A 116.1 . . ?
C31A C32A H32A 116.2 . . ?
C31A C32A C33A 127.6(9) . . ?
C33A C32A H32A 116.2 . . ?
C32A C33A H33A 117.6 . . ?
C34A C33A C32A 124.8(10) . . ?
C34A C33A H33A 117.6 . . ?
C33A C34A Al1 120.1(7) . . ?
C33A C34A C35A 116.0(8) . . ?
C35A C34A Al1 123.9(5) . . ?
C34A C35A H35D 109.5 . . ?
C34A C35A H35E 109.5 . . ?
C34A C35A H35F 109.5 . . ?
H35D C35A H35E 109.5 . . ?
H35D C35A H35F 109.5 . . ?
H35E C35A H35F 109.5 . . ?
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 1.8878(17) . ?
Al1 N3 1.904(2) . ?
Al1 O30 1.845(3) . ?
Al1 C34 1.878(4) . ?
Al1 O30A 1.938(5) . ?
Al1 C34A 1.845(8) . ?
N1 C1 1.339(3) . ?
N1 C6 1.455(2) . ?
N3 C3 1.340(3) . ?
N3 C18 1.446(3) . ?
C1 C2 1.397(3) . ?
C1 C4 1.503(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.396(3) . ?
C3 C5 1.504(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.411(3) . ?
C6 C11 1.401(4) . ?
C7 C8 1.391(3) . ?
C7 C12 1.518(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.380(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.376(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.397(3) . ?
C11 C15 1.515(3) . ?
C12 H12 1.0000 . ?
C12 C13 1.529(4) . ?
C12 C14 1.524(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.522(4) . ?
C15 C17 1.525(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.412(3) . ?
C18 C23 1.412(3) . ?
C19 C20 1.393(3) . ?
C19 C24 1.513(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.376(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.388(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.390(3) . ?
C23 C27 1.518(3) . ?
C24 H24 1.0000 . ?
C24 C25 1.527(4) . ?
C24 C26 1.535(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27 1.0000 . ?
C27 C28 1.525(4) . ?
C27 C29 1.525(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O30 C31 1.354(5) . ?
C31 H31 0.9500 . ?
C31 C32 1.305(6) . ?
C32 H32 0.9500 . ?
C32 C33 1.439(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.368(6) . ?
C34 C35 1.480(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
O30A C31A 1.353(10) . ?
C31A H31A 0.9500 . ?
C31A C32A 1.236(12) . ?
C32A H32A 0.9500 . ?
C32A C33A 1.448(13) . ?
C33A H33A 0.9500 . ?
C33A C34A 1.384(13) . ?
C34A C35A 1.492(11) . ?
C35A H35D 0.9800 . ?
C35A H35E 0.9800 . ?
C35A H35F 0.9800 . ?
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 C1 C2 16.8(3) . . . . ?
Al1 N1 C1 C4 -163.08(17) . . . . ?
Al1 N1 C6 C7 -104.3(2) . . . . ?
Al1 N1 C6 C11 76.4(2) . . . . ?
Al1 N3 C3 C2 -13.8(3) . . . . ?
Al1 N3 C3 C5 166.59(16) . . . . ?
Al1 N3 C18 C19 -92.8(2) . . . . ?
Al1 N3 C18 C23 85.2(2) . . . . ?
Al1 O30 C31 C32 2.1(5) . . . . ?
Al1 O30A C31A C32A -0.7(11) . . . . ?
N1 Al1 O30 C31 127.4(3) . . . . ?
N1 Al1 C34 C33 -117.6(3) . . . . ?
N1 Al1 C34 C35 60.4(4) . . . . ?
N1 Al1 C34A C33A 114.1(6) . . . . ?
N1 Al1 C34A C35A -65.7(7) . . . . ?
N1 C1 C2 C3 10.6(4) . . . . ?
N1 C6 C7 C8 -176.15(19) . . . . ?
N1 C6 C7 C12 4.1(3) . . . . ?
N1 C6 C11 C10 176.50(19) . . . . ?
N1 C6 C11 C15 -2.6(3) . . . . ?
N3 Al1 N1 C1 -31.94(17) . . . . ?
N3 Al1 N1 C6 149.51(16) . . . . ?
N3 Al1 O30 C31 -132.0(3) . . . . ?
N3 Al1 C34 C33 113.7(3) . . . . ?
N3 Al1 C34 C35 -68.2(4) . . . . ?
N3 Al1 C34A C33A -115.0(6) . . . . ?
N3 Al1 C34A C35A 65.3(7) . . . . ?
N3 C18 C19 C20 178.15(18) . . . . ?
N3 C18 C19 C24 0.1(3) . . . . ?
N3 C18 C23 C22 -177.52(18) . . . . ?
N3 C18 C23 C27 5.2(3) . . . . ?
C1 N1 C6 C7 77.1(2) . . . . ?
C1 N1 C6 C11 -102.2(2) . . . . ?
C1 C2 C3 N3 -12.1(3) . . . . ?
C1 C2 C3 C5 167.5(2) . . . . ?
C3 N3 C18 C19 80.0(3) . . . . ?
C3 N3 C18 C23 -102.0(2) . . . . ?
C4 C1 C2 C3 -169.6(2) . . . . ?
C6 N1 C1 C2 -164.63(19) . . . . ?
C6 N1 C1 C4 15.5(3) . . . . ?
C6 C7 C8 C9 -1.2(4) . . . . ?
C6 C7 C12 C13 -114.7(2) . . . . ?
C6 C7 C12 C14 121.9(2) . . . . ?
C6 C11 C15 C16 -122.0(2) . . . . ?
C6 C11 C15 C17 114.0(2) . . . . ?
C7 C6 C11 C10 -2.8(3) . . . . ?
C7 C6 C11 C15 178.1(2) . . . . ?
C7 C8 C9 C10 -1.1(4) . . . . ?
C8 C7 C12 C13 65.5(3) . . . . ?
C8 C7 C12 C14 -57.9(3) . . . . ?
C8 C9 C10 C11 1.5(4) . . . . ?
C9 C10 C11 C6 0.4(4) . . . . ?
C9 C10 C11 C15 179.5(2) . . . . ?
C10 C11 C15 C16 58.9(3) . . . . ?
C10 C11 C15 C17 -65.0(3) . . . . ?
C11 C6 C7 C8 3.2(3) . . . . ?
C11 C6 C7 C12 -176.6(2) . . . . ?
C12 C7 C8 C9 178.6(2) . . . . ?
C18 N3 C3 C2 173.35(18) . . . . ?
C18 N3 C3 C5 -6.3(3) . . . . ?
C18 C19 C20 C21 -1.0(3) . . . . ?
C18 C19 C24 C25 113.5(2) . . . . ?
C18 C19 C24 C26 -123.5(2) . . . . ?
C18 C23 C27 C28 82.7(3) . . . . ?
C18 C23 C27 C29 -153.3(2) . . . . ?
C19 C18 C23 C22 0.4(3) . . . . ?
C19 C18 C23 C27 -176.89(19) . . . . ?
C19 C20 C21 C22 1.1(3) . . . . ?
C20 C19 C24 C25 -64.5(3) . . . . ?
C20 C19 C24 C26 58.5(3) . . . . ?
C20 C21 C22 C23 -0.4(4) . . . . ?
C21 C22 C23 C18 -0.4(3) . . . . ?
C21 C22 C23 C27 177.0(2) . . . . ?
C22 C23 C27 C28 -94.5(3) . . . . ?
C22 C23 C27 C29 29.5(3) . . . . ?
C23 C18 C19 C20 0.3(3) . . . . ?
C23 C18 C19 C24 -177.76(19) . . . . ?
C24 C19 C20 C21 177.1(2) . . . . ?
O30 Al1 N1 C1 71.43(19) . . . . ?
O30 Al1 N1 C6 -107.11(19) . . . . ?
O30 Al1 C34 C33 0.8(3) . . . . ?
O30 Al1 C34 C35 178.9(3) . . . . ?
O30 C31 C32 C33 -2.0(7) . . . . ?
C31 C32 C33 C34 1.3(8) . . . . ?
C32 C33 C34 Al1 -0.8(6) . . . . ?
C32 C33 C34 C35 -179.0(4) . . . . ?
C34 Al1 N1 C1 -172.34(19) . . . . ?
C34 Al1 N1 C6 9.1(2) . . . . ?
C34 Al1 O30 C31 -1.4(3) . . . . ?
O30A Al1 N1 C1 -139.9(2) . . . . ?
O30A Al1 N1 C6 41.6(2) . . . . ?
O30A Al1 C34A C33A 1.4(7) . . . . ?
O30A Al1 C34A C35A -178.4(6) . . . . ?
O30A C31A C32A C33A 0.1(15) . . . . ?
C31A C32A C33A C34A 1.6(17) . . . . ?
C32A C33A C34A Al1 -2.3(13) . . . . ?
C32A C33A C34A C35A 177.5(9) . . . . ?
C34A Al1 N1 C1 108.6(3) . . . . ?
C34A Al1 N1 C6 -69.9(3) . . . . ?
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
0.0007 0.0004 -1.0004 -0.0722 -0.0046 -0.0384
-2.9940 4.9985 2.9904 -0.0261 0.8568 -0.2793
-0.0007 -0.0004 1.0004 0.0722 0.0046 0.0384
-1.0001 0.0000 1.9990 0.0061 0.0455 0.0832
3.9934 -4.9989 -3.9889 0.0922 -0.8978 0.2345
4.9975 -0.0015 -5.9933 0.2583 -0.2093 -0.2627
