Formation of an Ag→Al dative bond is avoided in reactions of an alane/tris(phosphine) ligand with monovalent silver.
Lai, Qingheng; Bhuvanesh, Nattamai; Zhou, Jia; Ozerov, Oleg V.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 5776–5778; doi:10.1039/d1dt01068a

data_7707088
_publ_section_title
;
 Formation of an Ag\\rightarrow Al dative bond is avoided in reactions of
 an alane/tris(phosphine) ligand with monovalent silver.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5776
_journal_page_last               5778
_journal_paper_doi               10.1039/d1dt01068a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C30 H51 Ag Al N3 P3, C H B11 Cl11, 1.5(C7 H8)'
_chemical_formula_sum            'C41.5 H64 Ag Al B11 Cl11 N3 P3'
_chemical_formula_weight         1341.57
_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             2018-03-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2019-05-13 deposited with the CCDC.	2021-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                105.0880(10)
_cell_angle_beta                 102.9650(10)
_cell_angle_gamma                103.3940(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6286(10)
_cell_length_b                   15.2317(15)
_cell_length_c                   21.256(2)
_cell_measurement_reflns_used    9168
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.540
_cell_measurement_theta_min      2.305
_cell_volume                     3080.2(5)
_computing_cell_refinement       'SAINT V8.32B (2016)'
_computing_data_reduction        'SAINT V8.32B (2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            79626
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.602
_diffrn_reflns_theta_min         2.013
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0556 before and 0.0486 after correction. The Ratio of minimum to maximum transmission is 0.9213. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         14237
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0278P)^2^+1.4108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11545
_reflns_number_total             14237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01068a3.cif
_cod_data_source_block           qhl888_ovo
_cod_depositor_comments
'Adding full bibliography for 7707087--7707088.cif.'
_cod_original_formula_sum        'C41.50 H64 Ag Al B11 Cl11 N3 P3'
_cod_database_code               7707088
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.836
_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. Restrained distances
 C1A-C1B
 1.51 with sigma of 0.02
 C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F \\sim C1F-C1G \\sim C1G-C1B
 with sigma of 0.02
 C1B-C1F \\sim C1B-C1D \\sim C1G-C1E \\sim C1C-C1G \\sim C1D-C1F \\sim C1C-C1E
 with sigma of 0.04
 C1A-C1G \\sim C1A-C1C
 with sigma of 0.04
 P2-C26A \\sim P2-C26
 with sigma of 0.005
 C28A-C26A \\sim C28-C26 \\sim C27A-C26A \\sim C27-C26
 with sigma of 0.005
3. Restrained planarity
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F \\sim C1G: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
P2 \\sim C26 \\sim C27 \\sim C28 \\sim C26A \\sim C27A \\sim C28A: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C28A) = Uanis(C28)
5. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P2, C26, C27, C28, C26A, C27A, C28A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Others
 Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C28)=Sof(H28A)=
 Sof(H28B)=Sof(H28C)=FVAR(1)
 Fixed Sof: C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) C1C(0.5) H1C(0.5)
 C1D(0.5) H1D(0.5) C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5) C1G(0.5) H1G(0.5)
7.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C20(H20), C23(H23), C26(H26), C26A(H26A), C29(H29)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C11T(H11T), C12T(H12T), C13T(H13T), C14T(H14T), C15T(H15T), C1C(H1C), C1D(H1D),
  C1E(H1E), C1F(H1F), C1G(H1G)
7.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C27A(H27D,H27E,H27F),
 C28A(H28D,H28E,H28F), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C16T(H16D,H16E,
 H16F), C1A(H1AA,H1AB,H1AC)
7.d Boron cage BH refined with riding coordinates:
 C1(H1)
;
_shelx_res_checksum              10147
_shelx_hkl_checksum              71567
_olex2_submission_special_instructions 'No special instructions were received'