Synthesis, structure, and photoluminesence of the chloridoaluminates [BMIm][Sn(AlCl<sub>4</sub>)<sub>3</sub>], [BMPyr][Sn(AlCl<sub>4</sub>)<sub>3</sub>], and [BMIm][Pb(AlCl<sub>4</sub>)<sub>3</sub>].
Wolf, Silke; Liebertseder, Mareike; Feldmann, Claus; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8549–8557; doi:10.1039/d0dt03766d

data_7707523
_publ_section_title
;
 Synthesis, structure, and photoluminesence of the chloridoaluminates
 [BMIm][Sn(AlCl<sub>4</sub>)<sub>3</sub>],
 [BMPyr][Sn(AlCl<sub>4</sub>)<sub>3</sub>], and
 [BMIm][Pb(AlCl<sub>4</sub>)<sub>3</sub>].
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8549
_journal_page_last               8557
_journal_paper_doi               10.1039/d0dt03766d
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'Al3 Cl12 Pb, 2(C5 H9 N)'
_chemical_formula_sum            'C10 H18 Al3 Cl12 N2 Pb'
_chemical_formula_weight         879.79
_chemical_properties_physical    Moisture-sensitive,Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-10-20
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-10-29 deposited with the CCDC.	2021-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.00(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.056(12)
_cell_length_b                   15.530(13)
_cell_length_c                   11.876(11)
_cell_measurement_reflns_used    362
_cell_measurement_temperature    213
_cell_measurement_theta_max      15.70
_cell_measurement_theta_min      1.83
_cell_volume                     2735(4)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      213
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_av_unetI/netI     0.0915
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9666
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.983
_diffrn_reflns_theta_min         1.899
_exptl_absorpt_coefficient_mu    7.443
_exptl_absorpt_correction_T_max  0.3204
_exptl_absorpt_correction_T_min  0.0669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.783
_refine_diff_density_min         -2.406
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2689
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0435P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1752
_reflns_number_total             2689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03766d2.cif
_cod_data_source_block           '[BMIm][Pb(AlCl4)3]'
_cod_depositor_comments
'Adding full bibliography for 7707523--7707525.cif.'
_cod_database_code               7707523
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C4 \\sim N2 \\sim C2 \\sim C1 \\sim C8 \\sim C3 \\sim N1 \\sim C5 \\sim C6
\\sim C7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 1.7A
3. Rigid body (RIGU) restrains
 C4, N2, C2, C1, C8, C3, N1, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N2(0.5) C3(0.5) H3(0.5) N1(0.5) C1(0.5) H1(0.5) C5(0.5) H5A(0.5)
 H5B(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C6(0.5) H6A(0.5) H6B(0.5) C7(0.5)
 H7A(0.5) H7B(0.5) H7C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C1(H1)
5.c Fitted pentagon refined as free rotating group:
 N2(C2,C3,N1,C1)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              86195
_shelx_hkl_checksum              60444
_olex2_submission_special_instructions 'No special instructions were received'