Reactions of Aluminium(I) with Transition Metal Carbonyls: Scope, Mechanism and Selectivity of CO Homologation
Crimmin, Mark Richard; Kong, Richard Y.; Batuecas, Maria; Chemical Science  (2021) –; doi:10.1039/D1SC04940B

data_1565068
_publ_section_title
;
 &#x000D; Reactions of Aluminium(I) with Transition Metal Carbonyls:
 Scope, Mechanism and Selectivity of CO Homologation&#x000D;
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04940B
_journal_year                    2021
_chemical_formula_moiety
'C73 H97 Al2 N4 O5 Re, 0.25(C5 H12), 0.25(C7 H8)'
_chemical_formula_sum            'C76 H102 Al2 N4 O5 Re'
_chemical_formula_weight         1391.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-08 deposited with the CCDC.	2021-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3541(4)
_cell_length_b                   20.3340(5)
_cell_length_c                   45.6601(19)
_cell_measurement_reflns_used    9212
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      73.0890
_cell_measurement_theta_min      3.8470
_cell_volume                     16112.5(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -98.00  -2.00   1.00    8.71    --  -42.36 125.00 120.00   96
  2  \w     89.00 153.00   1.00   37.94    --  105.13  45.00 150.00   64
  3  \w     28.00 108.00   1.00   37.94    --  105.13 -95.00-120.00   80
  4  \w     81.00 175.00   1.00   37.94    --  105.13  77.00-120.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0871190000
_diffrn_orient_matrix_UB_12      0.0119592000
_diffrn_orient_matrix_UB_13      -0.0037671000
_diffrn_orient_matrix_UB_21      0.0000757000
_diffrn_orient_matrix_UB_22      -0.0439081000
_diffrn_orient_matrix_UB_23      -0.0274969000
_diffrn_orient_matrix_UB_31      -0.0170933000
_diffrn_orient_matrix_UB_32      0.0606058000
_diffrn_orient_matrix_UB_33      -0.0191601000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            33316
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.446
_diffrn_reflns_theta_min         3.485
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.513
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.533
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       plate
_exptl_crystal_F_000             5816
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.204
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         15643
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0901P)^2^+8.8892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11650
_reflns_number_total             15643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04940b3.cif
_cod_data_source_block           3-Re'
_cod_database_code               1565068
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C73 H97 Al2 N4 O5 Re'
_chemical_oxdiff_usercomment     RK551-extr1
_reflns_odcompleteness_completeness 98.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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
 C81-C82 = C82-C83 = C83-C84 = C84-C85
 1.5 with sigma of 0.02
 C81-C83 = C82-C84 = C83-C85
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C29 \\sim C28' \\sim C29' \\sim C28: within 1A with sigma of 0.01 and sigma for
terminal atoms of 0.01
C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85: within 5A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C69 \\sim C69' \\sim C70 \\sim C70': within 1.5A with sigma of 0.01 and sigma
for terminal atoms of 0.01
4. Others
 Sof(H27A)=Sof(C28')=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29')=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(H27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=FVAR(1)
 Sof(H68A)=Sof(C70')=Sof(H70D)=Sof(H70E)=Sof(H70F)=Sof(C69')=Sof(H69D)=
 Sof(H69E)=Sof(H69F)=1-FVAR(2)
 Sof(H68)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=Sof(C70)=Sof(H70A)=Sof(H70B)=
 Sof(H70C)=FVAR(2)
 Fixed Sof: C81(0.25) H81A(0.25) H81B(0.25) H81C(0.25) C85(0.25) H85A(0.25)
 H85B(0.25) H85C(0.25) C82(0.25) H82A(0.25) H82B(0.25) C83(0.25) H83A(0.25)
 H83B(0.25) C75(0.25) H75(0.25) C76(0.25) H76(0.25) C77(0.25) H77(0.25)
 C78(0.25) H78(0.25) C79(0.25) H79(0.25) C74(0.25) C80(0.25) H80A(0.25)
 H80B(0.25) H80C(0.25) C84(0.25) H84A(0.25) H84B(0.25)
5.a Ternary CH refined with riding coordinates:
 C39(H39), C30(H30), C56(H56), C68(H68), C68(H68A), C59(H59), C27(H27),
 C27(H27A), C71(H71), C42(H42)
5.b Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B)
5.c Me refined with riding coordinates:
 C81(H81A,H81B,H81C), C85(H85A,H85B,H85C), C80(H80A,H80B,H80C)
5.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C37(H37), C52(H52), C35(H35), C47(H47), C36(H36), C25(H25),
 C54(H54), C65(H65), C24(H24), C23(H23), C64(H64), C53(H53), C66(H66), C75(H75),
  C76(H76), C77(H77), C78(H78), C79(H79)
5.e Fitted hexagon refined as free rotating group:
 C75(C76,C77,C78,C79,C74)
5.f Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C20(H20A,H20B,
 H20C), C73(H73A,H73B,H73C), C49(H49A,H49B,H49C), C45(H45A,H45B,H45C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C40(H40A,H40B,H40C), C31(H31A,H31B,H31C),
 C41(H41A,H41B,H41C), C58(H58A,H58B,H58C), C61(H61A,H61B,H61C), C57(H57A,H57B,
 H57C), C28(H28A,H28B,H28C), C60(H60A,H60B,H60C), C29(H29A,H29B,H29C),
 C28'(H28D,H28E,H28F), C29'(H29D,H29E,H29F), C16(H16A,H16B,H16C), C32(H32A,H32B,
 H32C), C72(H72A,H72B,H72C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C69(H69A,
 H69B,H69C), C70(H70A,H70B,H70C), C70'(H70D,H70E,H70F), C69'(H69D,H69E,H69F)
;
_shelx_res_checksum              5462
_shelx_hkl_checksum              60243
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.146
_oxdiff_exptl_absorpt_empirical_full_min 0.829