Closing the loop in the synthesis of heteroscorpionate-based aluminium helicates. Catalytic studies for cyclic carbonate synthesis.
Lara, Agustin; Castro-Osma, José Antonio; North, Michael; Gaona, Miguel Ángel; de la Cruz-Martínez, Felipe; Rodríguez, Ana María; Caballero Espinosa, María del Prado; Francés-Poveda, Enrique; Rodríguez Diéguez, Antonio; Dalton Transactions  (2022) –; doi:10.1039/D2DT01645A

data_7710643
_publ_section_title
;
 Closing the loop in the synthesis of heteroscorpionate-based aluminium
 helicates. Catalytic studies for cyclic carbonate synthesis.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01645A
_journal_year                    2022
_chemical_formula_sum            'C36 H64 Al3 N5 O'
_chemical_formula_weight         663.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2022-06-28 deposited with the CCDC.	2022-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.022(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2041(8)
_cell_length_b                   10.0613(7)
_cell_length_c                   20.8767(11)
_cell_measurement_reflns_used    4308
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.58
_cell_measurement_theta_min      2.31
_cell_volume                     3845.5(4)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker ApexII'
_computing_data_reduction        'Bruker Apex II'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.582
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.582
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9512
_diffrn_reflns_point_group_measured_fraction_full 0.549
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         20.882
_diffrn_reflns_theta_min         2.225
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 1466 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.13(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         3824
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0538P)^2^+0.5649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.517
_reflns_Friedel_fraction_max     0.883
_reflns_number_gt                3425
_reflns_number_total             3824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01645a2.cif
_cod_data_source_block           17
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7710643
_shelxl_version_number           2014-3
_shelx_res_checksum              66148
_shelx_hkl_checksum              31015