Coordination chemistry and structural rearrangements of the Me2PCH2AlMe2 ambiphilic ligand
Paskaruk, Katarina; Emslie, David J. H.; Britten, James F.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02519A

data_7711291
_publ_section_title
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 Coordination chemistry and structural rearrangements of the Me2PCH2AlMe2
 ambiphilic ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02519A
_journal_year                    2022
_chemical_formula_moiety
'C12.921 H25.764 Al Cl1.079 P Rh, C12.36 H24.079 Al Cl1.64 P Rh'
_chemical_formula_sum            'C25.28 H49.84 Al2 Cl2.72 P2 Rh2'
_chemical_formula_weight         772.00
_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   mixed
_audit_creation_date             2022-07-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-07-05 deposited with the CCDC.	2022-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                71.297(2)
_cell_angle_beta                 66.453(2)
_cell_angle_gamma                75.357(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2567(4)
_cell_length_b                   12.8343(5)
_cell_length_c                   13.1652(5)
_cell_measurement_reflns_used    9403
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      33.36
_cell_measurement_theta_min      2.71
_cell_volume                     1634.43(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0194
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            99188
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.366
_diffrn_reflns_theta_min         1.693
_exptl_absorpt_coefficient_mu    1.398
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0383 before and 0.0293 after correction.
The Ratio of minimum to maximum transmission is 0.9281.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         12623
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0168
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+0.5609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11699
_reflns_number_total             12623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02519a2.cif
_cod_data_source_block           RhClcodPAl
_cod_original_cell_volume        1634.44(11)
_cod_database_code               7711291
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.713
_olex2_refinement_description
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1. Restrained distances
 Al2-C17 \\sim Al2-C26 \\sim Al1-C4 \\sim Al1-C5
 with sigma of 0.02
 Cl4-Al1 \\sim Cl3-Al2
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C26) = Uanis(Cl3)
Uanis(C4) = Uanis(Cl4)
3. Others
 Sof(C26)=Sof(HW)=Sof(HX)=Sof(HY)=1-FVAR(1)
 Sof(Cl3)=FVAR(1)
 Sof(Cl4)=1-FVAR(2)
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C6(H6), C7(H7), C11(H11), C18(HK), C19(HL), C23(HR)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,H13B), C16(HF,
 HG), C20(HM,HN), C21(HO,HP), C24(HS,HT), C25(HU,HV)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C14(H,HA,
 HB), C15(HC,HD,HE), C17(HH,HI,HJ), C26(HW,HX,HY)
;
_shelx_res_checksum              14053
_shelx_hkl_checksum              6504
_olex2_submission_special_instructions 'No special instructions were received'