Synthesis, Characterisation and Reactivity studies of Chiral β-Diketiminate-like Supported Aluminium Lewis Acid Complexes Towards Difficult Diels Alder Cycloadditions
Dissanayake, Deepamali; Forsyth, Craig M.; Vidovic, Dragoslav; Dalton Transactions  (2023) –; doi:10.1039/D3DT00206C

data_7712494
_publ_section_title
;
 Synthesis, Characterisation and Reactivity studies of Chiral
 \b-Diketiminate-like Supported Aluminium Lewis Acid Complexes Towards
 Difficult Diels Alder Cycloadditions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00206C
_journal_year                    2023
_chemical_formula_moiety         'C45 H40 Al Cl2 N2 O'
_chemical_formula_sum            'C45 H40 Al Cl2 N2 O'
_chemical_formula_weight         722.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-18 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.056(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7756(2)
_cell_length_b                   9.9253(2)
_cell_length_c                   30.1239(5)
_cell_measurement_reflns_used    32612
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.6010
_cell_measurement_theta_min      3.5690
_cell_volume                     3782.07(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            49969
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.037
_diffrn_reflns_theta_min         3.221
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_description       prism
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.161
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 4366 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.031(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         11268
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0329
_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/[\s^2^(Fo^2^)+(0.0500P)^2^+0.5221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0845
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.812
_reflns_number_gt                10357
_reflns_number_total             11268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00206c2.cif
_cod_data_source_block           mx125_20
_cod_database_code               7712494
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C36(0.5) H36(0.5) C3'(0.5) H3'(0.5) C37(0.5) C4'(0.5) C38(0.5)
 H38(0.5) C5'(0.5) H5'(0.5) C14(0.5) C14'(0.5) C15(0.5) H15(0.5) C15'(0.5)
 H15'(0.5) C16(0.5) H16(0.5) C16'(0.5) H16'(0.5) C17(0.5) H17(0.5) C17'(0.5)
 H17'(0.5) C18(0.5) H18(0.5) C18'(0.5) H18'(0.5) C19(0.5) H19(0.5) C19'(0.5)
 H19'(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C20'(0.5) H20D(0.5) H20E(0.5)
 H20F(0.5)
3.a Ternary CH refined with riding coordinates:
 C21(H21), C42(H42), C43(H43)
3.b Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B)
3.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C3'(H3'), C38(H38), C5'(H5'), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C15'(H15'), C16(H16), C16'(H16'), C17(H17), C17'(H17'),
 C18(H18), C18'(H18'), C19(H19), C19'(H19'), C23(H23), C24(H24), C25(H25),
 C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C2(H2),
 C3(H3), C4(H4), C5(H5)
3.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C20'(H20D,H20E,H20F), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C)
;
_shelx_res_checksum              55337
_shelx_hkl_checksum              42668
_olex2_submission_special_instructions 'No special instructions were received'