Comparable syntheses of terminal aluminum selenide and telluride
Li, Bin; Wang, Yuanyuan; Suthar, Sonam; Zhang, Manbo; Mondal, Kartik Chandra; New Journal of Chemistry 49 (2025) 1133–1137; doi:10.1039/D4NJ04255G

data_7063586
_publ_section_title
;
 Comparable syntheses of terminal aluminum selenide and telluride
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1133
_journal_page_last               1137
_journal_paper_doi               10.1039/D4NJ04255G
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C40 H61 Al N4 Se, C7 H8'
_chemical_formula_sum            'C47 H69 Al N4 Se'
_chemical_formula_weight         796.00
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-25 deposited with the CCDC.	2024-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.056(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5944(2)
_cell_length_b                   22.4932(4)
_cell_length_c                   17.7244(4)
_cell_measurement_reflns_used    10184
_cell_measurement_temperature    122.97(10)
_cell_measurement_theta_max      73.5150
_cell_measurement_theta_min      3.9870
_cell_volume                     4369.13(16)
_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_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -112.00 -24.00   1.00    5.00    --  -44.65 -57.00  90.00   88
  2  \w     23.00 112.00   1.00    5.00    --   44.65  37.00  30.00   89
  3  \w     43.00 129.00   1.00   20.00    --  104.50 -45.00-180.00   86
  4  \w     80.00 174.00   1.00   20.00    --  104.50  30.00   0.00   94
  5  \w     47.00 118.00   1.00   20.00    --  104.50-125.00 150.00   71
  6  \w     34.00 114.00   1.00   20.00    --  104.50 -45.00 -30.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0551229000
_diffrn_orient_matrix_UB_12      0.0098804000
_diffrn_orient_matrix_UB_13      0.0907300000
_diffrn_orient_matrix_UB_21      0.1226611000
_diffrn_orient_matrix_UB_22      0.0176287000
_diffrn_orient_matrix_UB_23      -0.0100154000
_diffrn_orient_matrix_UB_31      -0.0411793000
_diffrn_orient_matrix_UB_32      0.0654342000
_diffrn_orient_matrix_UB_33      -0.0108144000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14877
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.609
_diffrn_reflns_theta_min         3.931
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_preparation       '?0.186, mid= 0.194, max= 0.224'
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.186
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         8407
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+2.7671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7674
_reflns_number_total             8407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj04255g2.cif
_cod_data_source_block           compound1
_cod_depositor_comments
'Adding full bibliography for 7063586--7063587.cif.'
_cod_original_cell_volume        4369.13(15)
_cod_database_code               7063586
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C188 H280 Al4 N16 Se4 '
_shelx_estimated_absorpt_t_max   0.753
_shelx_estimated_absorpt_t_min   0.713
_reflns_odcompleteness_completeness 98.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(C43B) \\sim Ueq, Uanis(C47B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Sof(C41B)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C44B)=Sof(H44B)=Sof(C45B)=
 Sof(H45B)=Sof(C46B)=Sof(H46B)=Sof(C47B)=Sof(H47B)=Sof(C42B)=Sof(C43B)=
 Sof(H43B)=1-FVAR(1)
 Sof(C43A)=Sof(H43A)=Sof(C42A)=Sof(C47A)=Sof(H47A)=Sof(C46A)=Sof(H46A)=
 Sof(C45A)=Sof(H45A)=Sof(C44A)=Sof(H44A)=Sof(C41A)=Sof(H41A)=Sof(H41B)=
 Sof(H41C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C38(H38), C26(H26), C9(H9), C35(H35), C23(H23), C6(H6)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C19(H19), C31(H31), C33(H33), C20(H20), C21(H21), C32(H32),
 C43A(H43A), C47A(H47A), C46A(H46A), C45A(H45A), C44A(H44A), C44B(H44B),
 C45B(H45B), C46B(H46B), C47B(H47B), C43B(H43B)
4.c Fitted hexagon refined as free rotating group:
 C43A(C42A,C47A,C46A,C45A,C44A), C44B(C45B,C46B,C47B,C42B,C43B)
4.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C37(H37A,H37B,H37C), C12(H12A,H12B,H12C), C10(H10A,H10B,
 H10C), C11(H11A,H11B,H11C), C39(H39A,H39B,H39C), C28(H28A,H28B,H28C), C27(H27A,
 H27B,H27C), C8(H8A,H8B,H8C), C24(H24A,H24B,H24C), C36(H36A,H36B,H36C), C7(H7A,
 H7B,H7C), C5(H5A,H5B,H5C), C40(H40A,H40B,H40C), C25(H25A,H25B,H25C), C2(H2A,
 H2B,H2C), C41A(H41A,H41B,H41C), C41B(H41D,H41E,H41F)
;
_shelx_res_checksum              47448
_olex2_date_sample_data_collection 2019-03-06
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.828
_oxdiff_exptl_absorpt_empirical_full_min 0.584