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_7128306
_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 Al6 As4, C7 H8'
_chemical_formula_sum            'C74 H106 Al6 As4'
_chemical_formula_weight         1457.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-03-04
_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                 117.164(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.9888(9)
_cell_length_b                   17.1848(6)
_cell_length_c                   10.7513(4)
_cell_measurement_reflns_used    24141
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.30
_cell_measurement_theta_min      1.58
_cell_volume                     3614.5(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
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.842
_diffrn_measurement_details
;
 565 frames, detector distance = 40 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  0.0324
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.842
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17651
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.842
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.620
_diffrn_reflns_theta_min         1.577
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.946
_exptl_absorpt_correction_T_max  0.8485
_exptl_absorpt_correction_T_min  0.3433
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         5274
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.9762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1063
_reflns_d_resolution_high        0.678
_reflns_d_resolution_low         12.911
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              29
_reflns_limit_h_min              -32
_reflns_limit_k_max              25
_reflns_limit_k_min              -24
_reflns_limit_l_max              14
_reflns_limit_l_min              -14
_reflns_number_gt                4228
_reflns_number_total             5274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01475g2.cif
_cod_data_source_block           ah064_3
_cod_depositor_comments
'Adding full bibliography for 7128306--7128309.cif.'
_cod_database_code               7128306
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.612
_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
C19 \\sim C18 \\sim C22 \\sim C23 \\sim C21 \\sim C20: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
3. Others
 Fixed Sof: H14A(0.5) H14B(0.5) H14C(0.5) C23(0.25) H23(0.25) C22(0.25)
 H22(0.25) C21(0.25) H21(0.25) C20(0.25) H20(0.25) C19(0.25) H19(0.25)
 C18(0.25) C17(0.25) H17A(0.25) H17B(0.25) H17C(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C22(H22), C21(H21), C20(H20), C19(H19)
4.b Fitted hexagon refined as free rotating group:
 C23(C22,C21,C20,C19,C18)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C8(H8A,H8B,
 H8C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C17(H17A,H17B,
 H17C), C9(H9A,H9B,H9C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              43855
_shelx_fab_checksum              27396
_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'