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#$Date: 2022-02-10 01:00:40 +0100 (jue 10 de feb de 2022) $
#$Revision: 272894 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/94/7709450.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_7709450
loop_
_publ_author_name
'Petrus, Rafał'
'Utko, Józef'
'Petrus, Joanna Katarzyna'
'Awashra, Mohammad'
'Lis, Tadeusz'
_publ_section_title
;
 Use of group 13 aryloxides for the synthesis of green chemicals and oxide
 materials
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03777C
_journal_year                    2022
_chemical_formula_moiety         'C27 H27 Al O9'
_chemical_formula_sum            'C27 H27 Al O9'
_chemical_formula_weight         522.46
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-12-14 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.171(3)
_cell_length_b                   13.171(3)
_cell_length_c                   8.265(2)
_cell_measurement_reflns_used    1064
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3.5
_cell_volume                     1241.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'DIAMOND  (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2905
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.940
_diffrn_reflns_theta_min         3.572
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            colorless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.500
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         1766
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0366
_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)+(0.0371P)²+0.3847P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1525
_reflns_number_total             1766
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt03777c2.cif
_cod_data_source_block           1A
_cod_original_cell_volume        1241.7(6)
_cod_database_code               7709450
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.935
_oxdiff_exptl_absorpt_empirical_full_min 0.971
_oxdiff_exptl_absorpt_empirical_full_max 1.044
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
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 0.6667 0.3333 0.35369(9) 0.01226(19) Uani 1 3 d S T P . .
O1 O 0.75558(9) 0.28847(9) 0.23811(12) 0.0149(2) Uani 1 1 d . . . . .
O2 O 0.62400(8) 0.20568(8) 0.50502(12) 0.0140(2) Uani 1 1 d . . . . .
O3 O 0.61513(9) 0.04974(9) 0.62239(12) 0.0171(3) Uani 1 1 d . . . . .
C1 C 0.78069(12) 0.20548(12) 0.26369(17) 0.0136(3) Uani 1 1 d . . . . .
C2 C 0.85879(13) 0.19465(13) 0.15738(18) 0.0173(3) Uani 1 1 d . . . . .
H2 H 0.8923 0.2482 0.0700 0.021 Uiso 1 1 calc R U . . .
C3 C 0.88728(13) 0.10845(14) 0.17760(19) 0.0205(4) Uani 1 1 d . . . . .
H3 H 0.9403 0.1037 0.1042 0.025 Uiso 1 1 calc R U . . .
C4 C 0.83977(14) 0.02730(14) 0.3043(2) 0.0227(4) Uani 1 1 d . . . . .
H4 H 0.8594 -0.0326 0.3163 0.027 Uiso 1 1 calc R U . . .
C5 C 0.76467(14) 0.03578(13) 0.4103(2) 0.0192(3) Uani 1 1 d . . . . .
H5 H 0.7325 -0.0185 0.4972 0.023 Uiso 1 1 calc R U . . .
C6 C 0.73410(12) 0.12355(12) 0.39308(17) 0.0146(3) Uani 1 1 d . . . . .
C7 C 0.65516(12) 0.13109(12) 0.50819(17) 0.0139(3) Uani 1 1 d . . . . .
C8 C 0.54681(13) 0.06087(13) 0.75331(18) 0.0181(3) Uani 1 1 d . . . . .
H8A H 0.4959 -0.0168 0.8031 0.022 Uiso 1 1 calc R U . . .
H8B H 0.4960 0.0899 0.7095 0.022 Uiso 1 1 calc R U . . .
C9 C 0.62789(15) 0.14483(15) 0.87910(19) 0.0242(4) Uani 1 1 d . . . . .
H9A H 0.6780 0.1158 0.9222 0.036 Uiso 1 1 calc R U . . .
H9B H 0.5816 0.1513 0.9671 0.036 Uiso 1 1 calc R U . . .
H9C H 0.6769 0.2221 0.8299 0.036 Uiso 1 1 calc R U . . .
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'
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_
_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 O1 95.07(5) . 3_665 ?
O1 Al1 O1 95.07(5) . 2_655 ?
O1 Al1 O1 95.07(5) 3_665 2_655 ?
O1 Al1 O2 90.66(4) . . ?
O1 Al1 O2 90.75(4) 3_665 . ?
O1 Al1 O2 171.44(5) 2_655 . ?
O1 Al1 O2 90.74(4) . 2_655 ?
O1 Al1 O2 171.44(5) 3_665 2_655 ?
O1 Al1 O2 90.66(4) 2_655 2_655 ?
O2 Al1 O2 82.89(5) . 2_655 ?
O1 Al1 O2 171.44(5) . 3_665 ?
O1 Al1 O2 90.66(4) 3_665 3_665 ?
O1 Al1 O2 90.75(4) 2_655 3_665 ?
O2 Al1 O2 82.90(5) . 3_665 ?
O2 Al1 O2 82.90(5) 2_655 3_665 ?
C1 O1 Al1 131.14(9) . . ?
C7 O2 Al1 129.29(10) . . ?
C7 O3 C8 117.58(12) . . ?
O1 C1 C2 119.01(13) . . ?
O1 C1 C6 124.21(13) . . ?
C2 C1 C6 116.78(13) . . ?
C3 C2 C1 121.45(14) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 121.31(15) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 118.84(15) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 121.16(15) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 120.46(14) . . ?
C5 C6 C7 119.94(14) . . ?
C1 C6 C7 119.60(13) . . ?
O2 C7 O3 120.05(13) . . ?
O2 C7 C6 125.00(13) . . ?
O3 C7 C6 114.96(12) . . ?
O3 C8 C9 109.83(12) . . ?
O3 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
O3 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 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 O1 1.8235(11) . ?
Al1 O1 1.8235(11) 3_665 ?
Al1 O1 1.8235(11) 2_655 ?
Al1 O2 1.9397(11) . ?
Al1 O2 1.9397(11) 2_655 ?
Al1 O2 1.9397(11) 3_665 ?
O1 C1 1.3078(17) . ?
O2 C7 1.2399(17) . ?
O3 C7 1.3236(17) . ?
O3 C8 1.4608(18) . ?
C1 C2 1.413(2) . ?
C1 C6 1.422(2) . ?
C2 C3 1.373(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.400(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.368(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.409(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.449(2) . ?
C8 C9 1.504(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 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
O1 Al1 O1 C1 -94.34(14) 3_665 . . . ?
O1 Al1 O1 C1 170.10(12) 2_655 . . . ?
O2 Al1 O1 C1 -3.53(12) . . . . ?
O2 Al1 O1 C1 79.37(12) 2_655 . . . ?
Al1 O1 C1 C2 -176.21(10) . . . . ?
Al1 O1 C1 C6 3.9(2) . . . . ?
O1 C1 C2 C3 -179.34(13) . . . . ?
C6 C1 C2 C3 0.6(2) . . . . ?
C1 C2 C3 C4 0.2(2) . . . . ?
C2 C3 C4 C5 -0.8(2) . . . . ?
C3 C4 C5 C6 0.5(2) . . . . ?
C4 C5 C6 C1 0.3(2) . . . . ?
C4 C5 C6 C7 -179.42(14) . . . . ?
O1 C1 C6 C5 179.11(13) . . . . ?
C2 C1 C6 C5 -0.8(2) . . . . ?
O1 C1 C6 C7 -1.2(2) . . . . ?
C2 C1 C6 C7 178.89(12) . . . . ?
Al1 O2 C7 O3 -179.58(9) . . . . ?
Al1 O2 C7 C6 -0.1(2) . . . . ?
C8 O3 C7 O2 -7.74(19) . . . . ?
C8 O3 C7 C6 172.69(12) . . . . ?
C5 C6 C7 O2 179.06(14) . . . . ?
C1 C6 C7 O2 -0.6(2) . . . . ?
C5 C6 C7 O3 -1.40(19) . . . . ?
C1 C6 C7 O3 178.92(12) . . . . ?
C7 O3 C8 C9 -82.53(15) . . . . ?
