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_7710644
_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_moiety         'C27 H45 Al2 N5 O'
_chemical_formula_sum            'C27 H45 Al2 N5 O'
_chemical_formula_weight         509.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-06-28 deposited with the CCDC.	2022-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.2330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7654(13)
_cell_length_b                   19.445(2)
_cell_length_c                   13.2565(15)
_cell_measurement_reflns_used    3736
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      21.313
_cell_measurement_theta_min      2.421
_cell_volume                     3008.7(6)
_computing_cell_refinement       'Bruker SAINT V8.37 (Bruker AXS Inc. 2016)'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT V8.37 (Bruker AXS Inc. 2016)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'WINGX v2014.1 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013/4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013/4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector, APEX'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15843
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_min         2.727
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.156
_refine_diff_density_min         -0.173
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0496P)^2^+1.0634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2955
_reflns_number_total             3933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01645a2.cif
_cod_data_source_block           22
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710644
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.950
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              12415
_shelx_hkl_checksum              5236