Group 13 Salphen compounds (In, Ga and Al): A comparison of their structural features and activities as catalysts for cyclic carbonate synthesis
Jaraba Cabrera, Diego; Lewis, Ryan; Díez-Poza, Carlos; Alvarez-Miguel, Lucia; Mosquera, Marta Elena Gonzalez; Hamilton, Alex; Whiteoak, Christopher J.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00089C

data_7712375
_publ_section_title
;
 Group 13 Salphen compounds (In, Ga and Al): A comparison of their
 structural features and activities as catalysts for cyclic carbonate
 synthesis
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00089C
_journal_year                    2023
_chemical_formula_moiety         'C36 H46 Ga I N2 O2'
_chemical_formula_sum            'C36 H46 Ga I N2 O2'
_chemical_formula_weight         735.37
_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             2022-06-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-06-08 deposited with the CCDC.	2023-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.779(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6466(3)
_cell_length_b                   18.2837(7)
_cell_length_c                   25.0241(11)
_cell_measurement_reflns_used    9507
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      2.70
_cell_volume                     3474.1(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'Apex3 v2019.11-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL 2013/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'multilayer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0784
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            142440
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.564
_diffrn_reflns_theta_min         2.374
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'INCOATEC I\ms 3.0'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.713
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0915 before and 0.0638 after correction.
The Ratio of minimum to maximum transmission is 0.9086.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         11584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+2.6355P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8570
_reflns_number_total             11584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00089c2.cif
_cod_data_source_block           megm_lamgail_a_0m
_cod_database_code               7712375
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.637
_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.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
 C24(H24), C30(H30)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C)
;
_shelx_res_checksum              74943
_shelx_hkl_checksum              24033
_olex2_submission_special_instructions 'No special instructions were received'