Reactivity of mono- and divalent aluminium compounds towards group 15 nanoparticles.
Hauser, Adrian; Münzfeld, Luca; Roesky, Peter W.; Chemical communications (Cambridge, England) 57 (2021) 5503–5506; doi:10.1039/d1cc01475g

data_7128309
_publ_section_title
;
 Reactivity of mono- and divalent aluminium compounds towards group 15
 nanoparticles.
;
_journal_issue                   45
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5503
_journal_page_last               5506
_journal_paper_doi               10.1039/d1cc01475g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C60 H90 Al7 As5, 2(C6 H6)'
_chemical_formula_sum            'C72 H102 Al7 As5'
_chemical_formula_weight         1530.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-18 deposited with the CCDC.	2021-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.0554(10)
_cell_length_b                   17.2141(4)
_cell_length_c                   13.6117(3)
_cell_measurement_reflns_used    30267
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.31
_cell_volume                     7276.7(3)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_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, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_details
;
 468 frames, detector distance = 80 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23729
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.474
_diffrn_reflns_theta_min         2.315
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.396
_exptl_absorpt_correction_T_max  0.8582
_exptl_absorpt_correction_T_min  0.6216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
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.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         9378
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0271P)^2^+7.6210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0722
_reflns_d_resolution_high        0.722
_reflns_d_resolution_low         8.871
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              18
_reflns_limit_h_min              -17
_reflns_limit_k_max              23
_reflns_limit_k_min              -21
_reflns_limit_l_max              42
_reflns_limit_l_min              -31
_reflns_number_gt                7207
_reflns_number_total             9378
_reflns_threshold_expression     I>2s/u(I)
_cod_data_source_file            d1cc01475g2.cif
_cod_data_source_block           ah105_rot3
_cod_depositor_comments
'Adding full bibliography for 7128306--7128309.cif.'
_cod_database_code               7128309
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.602
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
C42A \\sim C44A \\sim C39A \\sim C41A \\sim C43A \\sim C40A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C43B \\sim C39B \\sim C40B \\sim C42B \\sim C44B \\sim C41B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
2. Others
 Fixed Sof: H4A(0.5) H4B(0.5) H4C(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
 C43B(0.25) H43B(0.25) C42B(0.25) H42B(0.25) C41B(0.25) H41B(0.25) C40B(0.25)
 H40B(0.25) C39B(0.25) H39B(0.25) C44B(0.25) H44B(0.25) C42A(0.25) H42A(0.25)
 C41A(0.25) H41A(0.25) C40A(0.25) H40A(0.25) C39A(0.25) H39A(0.25) C44A(0.25)
 H44A(0.25) C43A(0.25) H43A(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C38(H38), C33(H33), C36(H36), C35(H35), C34(H34), C37(H37), C43B(H43B),
 C42B(H42B), C41B(H41B), C40B(H40B), C39B(H39B), C44B(H44B), C42A(H42A),
 C41A(H41A), C40A(H40A), C39A(H39A), C44A(H44A), C43A(H43A)
3.b Fitted hexagon refined as free rotating group:
 C43B(C42B,C41B,C40B,C39B,C44B), C42A(C41A,C40A,C39A,C44A,C43A)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C32(H32A,H32B,H32C), C12(H12A,H12B,H12C), C21(H21A,H21B,
 H21C), C6(H6A,H6B,H6C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C15(H15A,
 H15B,H15C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C5(H5A,H5B,H5C),
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C14(H14A,H14B,H14C), C13(H13A,H13B,
 H13C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              25250
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder oil'
_olex2_submission_special_instructions 'No special instructions were received'