Coordination polymers and molecular complexes of group 13 metal halides with bis-pyridylethane: comparison with rigid N-containing ligands
Gugin, Nikita Y.; Virovets, Alexander V.; Peresypkina, Eugenia; Davydova, Elena I.; Timoshkin, Alexey Y.; CrystEngComm  (2022) –; doi:10.1039/D2CE01063A

data_7245835
_publ_section_title
;
 Coordination polymers and molecular complexes of group 13 metal halides
 with bis-pyridylethane: comparison with rigid N-containing ligands
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01063A
_journal_year                    2022
_chemical_formula_moiety         ' C24 H24 Al Br2 N4, Br'
_chemical_formula_sum            'C24 H24 Al Br3 N4'
_chemical_formula_weight         635.18
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-07-27 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.931(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7677(5)
_cell_length_b                   9.7423(7)
_cell_length_c                   11.5702(6)
_cell_measurement_reflns_used    3267
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      31.4630
_cell_measurement_theta_min      2.6820
_cell_volume                     1262.03(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_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, 2018)'
_computing_structure_solution    SHELXS-2018
_diffrn_ambient_temperature      80(2)
_diffrn_detector                 'pixel array detector'
_diffrn_detector_area_resol_mean 5.814
_diffrn_detector_type            'DECTIRS PILATUS 6M'
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.745
_diffrn_measurement_device_type  '1-cycle diffractometer'
_diffrn_measurement_method       \f-scans
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6888
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.745
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8335
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.745
_diffrn_reflns_theta_full        24.411
_diffrn_reflns_theta_max         31.556
_diffrn_reflns_theta_min         1.763
_diffrn_source                   'DESY PetraIII P11 beamline'
_exptl_absorpt_coefficient_mu    4.441
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.21a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       prism
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.548
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3459
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0903
_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^)+(0.1226P)^2^+5.2609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2379
_refine_ls_wR_factor_ref         0.2432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2948
_reflns_number_total             3459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01063a2.cif
_cod_data_source_block           ayt78
_cod_database_code               7245835
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.502
_olex2_refinement_description
;
1. Restrained distances
 Br1B-Al1 \\sim Br1A-Al1 \\sim Br1C-Al1
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: Br1A(0.83) Br1B(0.11) Br1C(0.06) C6A(0.6) H6AA(0.6) H6AB(0.6)
 C7A(0.6) H7AA(0.6) H7AB(0.6) C6B(0.4) H6BA(0.4) H6BB(0.4) C7B(0.4) H7BA(0.4)
 H7BB(0.4) Br2A(0.19) Br2B(0.31)
4.a Secondary CH2 refined with riding coordinates:
 C6A(H6AA,H6AB), C7A(H7AA,H7AB), C6B(H6BA,H6BB), C7B(H7BA,H7BB)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12)
;
_shelx_res_checksum              85320
_shelx_hkl_checksum              82580
_olex2_submission_special_instructions 'No special instructions were received'