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_7712374
_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 Br Ga N2 O2'
_chemical_formula_sum            'C36 H46 Br Ga N2 O2'
_chemical_formula_weight         688.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-06-09 deposited with the CCDC.	2023-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                84.461(2)
_cell_angle_beta                 78.992(2)
_cell_angle_gamma                71.350(2)
_cell_formula_units_Z            2
_cell_length_a                   9.7269(4)
_cell_length_b                   12.7417(6)
_cell_length_c                   14.5254(7)
_cell_measurement_reflns_used    9049
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.35
_cell_volume                     1673.11(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            93581
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.919
_diffrn_reflns_theta_min         2.253
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.050
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0832 before and 0.0660 after correction.
The Ratio of minimum to maximum transmission is 0.9185.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0417P)^2^+1.0568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6089
_reflns_number_total             7986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00089c2.cif
_cod_data_source_block           megm_lamgabra_0m
_cod_database_code               7712374
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.646
_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:
 C3(H3), C5(H5), C7(H7), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
 C24(H24), C26(H26)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              60681
_shelx_hkl_checksum              72817
_olex2_submission_special_instructions 'No special instructions were received'