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_7128308
_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         'C30 H45 Al3 As Br3'
_chemical_formula_sum            'C30 H45 Al3 As Br3'
_chemical_formula_weight         801.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-01
_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                95.614(3)
_cell_angle_beta                 90.722(3)
_cell_angle_gamma                108.785(3)
_cell_formula_units_Z            4
_cell_length_a                   11.3402(4)
_cell_length_b                   16.7244(7)
_cell_length_c                   18.6143(8)
_cell_measurement_reflns_used    40134
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.30
_cell_measurement_theta_min      1.61
_cell_volume                     3322.6(2)
_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    'ShelXT (Sheldrick, 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 0.991
_diffrn_measured_fraction_theta_max 0.783
_diffrn_measurement_details
;
 505 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  0.0419
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.783
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32558
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.783
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.365
_diffrn_reflns_theta_min         1.606
_diffrn_source                   'Mo Genix 3D HF'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.729
_exptl_absorpt_correction_T_max  0.4261
_exptl_absorpt_correction_T_min  0.2490
_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    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.337
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.174
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         17117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0688P)^2^+2.2396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1291
_reflns_d_resolution_high        0.683
_reflns_d_resolution_low         12.683
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              14
_reflns_limit_h_min              -16
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              25
_reflns_limit_l_min              -24
_reflns_number_gt                12003
_reflns_number_total             17117
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            d1cc01475g2.cif
_cod_data_source_block           ah002_b
_cod_depositor_comments
'Adding full bibliography for 7128306--7128309.cif.'
_cod_database_code               7128308
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.493
_shelx_estimated_absorpt_t_min   0.299
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C29(H29A,H29B,H29C), C9(H9A,H9B,
 H9C), C39(H39A,H39B,H39C), C56(H56A,H56B,H56C), C49(H49A,H49B,H49C), C10(H10A,
 H10B,H10C), C57(H57A,H57B,H57C), C8(H8A,H8B,H8C), C60(H60A,H60B,H60C),
 C28(H28A,H28B,H28C), C50(H50A,H50B,H50C), C48(H48A,H48B,H48C), C30(H30A,H30B,
 H30C), C37(H37A,H37B,H37C), C27(H27A,H27B,H27C), C40(H40A,H40B,H40C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C26(H26A,
 H26B,H26C), C47(H47A,H47B,H47C), C46(H46A,H46B,H46C), C19(H19A,H19B,H19C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C17(H17A,H17B,H17C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              53276
_olex2_submission_special_instructions 'No special instructions were received'