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_7245832
_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 Cl2 N4), (Al Cl4)'
_chemical_formula_sum            'C24 H24 Al2 Cl6 N4'
_chemical_formula_weight         635.13
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-14 deposited with the CCDC.	2022-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   10.04888(13)
_cell_length_b                   10.04888(13)
_cell_length_c                   24.9760(5)
_cell_measurement_reflns_used    5417
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      73.9890
_cell_measurement_theta_min      5.2800
_cell_volume                     2184.18(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    SHELXT
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9216
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         74.162
_diffrn_reflns_theta_min         5.082
_diffrn_source_type              'microfocus SuperNova source'
_exptl_absorpt_coefficient_mu    6.146
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       'prism with broken vertices'
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.156
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         2922
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0499P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0742
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.696
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                2644
_reflns_number_total             2922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01063a2.cif
_cod_data_source_block           ayt73
_cod_original_cell_volume        2184.18(7)
_cod_database_code               7245832
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.447
_shelx_estimated_absorpt_t_max   0.642
_shelx_res_checksum              83377
_shelx_hkl_checksum              61956