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_7711286
_publ_section_title
;
 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         'C15 H31 Al Cl P2 Rh'
_chemical_formula_sum            'C15 H31 Al Cl P2 Rh'
_chemical_formula_weight         438.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-12
_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                90
_cell_angle_beta                 92.852(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.375(3)
_cell_length_b                   13.7736(18)
_cell_length_c                   11.9571(16)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.29
_cell_measurement_theta_min      2.39
_cell_volume                     3844.9(9)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            72957
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.618
_diffrn_reflns_theta_min         1.717
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0510 before and 0.0440 after correction.
The Ratio of minimum to maximum transmission is 0.9338.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         6425
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0263P)^2^+6.7091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5232
_reflns_number_total             6425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02519a2.cif
_cod_data_source_block           RhcodPPAlMeCl
_cod_database_code               7711286
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.639
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Al1-C7A \\sim Al1-C7
 with sigma of 0.02
 Cl1-Al1 \\sim Cl1A-Al1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) = Uanis(C7A)
Uanis(C7) = Uanis(Cl1A)
4. Others
 Sof(Cl1A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=1-FVAR(1)
 Sof(Cl1)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C12(H12), C15(H15)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C9(H9B,H9A), C10(H10A,H10B), C13(H13A,H13B),
 C14(H14A,H14B)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,
 H7B,H7C), C7A(H7AA,H7AB,H7AC)
;
_shelx_res_checksum              18310
_shelx_hkl_checksum              89556
_olex2_submission_special_instructions 'No special instructions were received'