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_1565063
_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         'C74 H97 Al2 N4 O6 Re, 1.5(C6 H6)'
_chemical_formula_sum            'C83 H106 Al2 N4 O6 Re'
_chemical_formula_weight         1495.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-26
_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                 95.819(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5551(2)
_cell_length_b                   15.5294(3)
_cell_length_c                   36.6963(10)
_cell_measurement_reflns_used    6631
_cell_measurement_temperature    173.1(2)
_cell_measurement_theta_max      72.7850
_cell_measurement_theta_min      4.3920
_cell_volume                     7684.9(3)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.953
_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 -18.00   1.00    9.35    --  -42.23 125.00-150.00   80
  2  \w    -67.00  35.00   1.00    9.35    --  -42.23  19.00  30.00  102
  3  \w     78.00 177.00   1.00   67.56    --  105.13  61.00 -60.00   99
  4  \w     67.00 138.00   1.00   67.56    --  105.13 -77.00-120.00   71
  5  \w     34.00 117.00   1.00   67.56    --  105.13 -45.00 150.00   83
  6  \w     79.00 168.00   1.00   67.56    --  105.13  45.00   0.00   89
;
_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      0.0834876000
_diffrn_orient_matrix_UB_12      0.0652073000
_diffrn_orient_matrix_UB_13      0.0108859000
_diffrn_orient_matrix_UB_21      -0.0011600000
_diffrn_orient_matrix_UB_22      0.0279252000
_diffrn_orient_matrix_UB_23      -0.0403340000
_diffrn_orient_matrix_UB_31      -0.0779284000
_diffrn_orient_matrix_UB_32      0.0693658000
_diffrn_orient_matrix_UB_33      0.0059919000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0763
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            24830
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.402
_diffrn_reflns_theta_min         3.377
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.731
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.594
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             3124
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.105
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         14739
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10643
_reflns_number_total             14739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04940b3.cif
_cod_data_source_block           4-Re
_cod_database_code               1565063
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C74 H63 N4 O6 Al2 Re'
_chemical_oxdiff_usercomment     RK234
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.421
_reflns_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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. Uiso/Uaniso restraints and constraints
C71 \\sim C70 \\sim C72 \\sim C172 \\sim C170 \\sim C171: within 1A with sigma
of 0.01 and sigma for terminal atoms of 0.01
C55 \\sim C56 \\sim C57 \\sim C156 \\sim C155 \\sim C157: within 1A with sigma
of 0.01 and sigma for terminal atoms of 0.01
C81 \\sim C83 \\sim C86 \\sim C89 \\sim C80 \\sim C84 \\sim C181 \\sim C183
\\sim C185 \\sim C189 \\sim C186 \\sim C180: within 1A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C92 \\sim C93 \\sim C90 \\sim C195 \\sim C190 \\sim C200: within 1A with sigma
of 0.01 and sigma for terminal atoms of 0.01
C92 \\sim C93 \\sim C90 \\sim C195 \\sim C190 \\sim C200 \\sim C100 \\sim C96
\\sim C97 \\sim C194 \\sim C192 \\sim C198: within 1.5A with sigma of 0.01 and
sigma for terminal atoms of 0.01
3. Others
 Sof(C172)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C170)=Sof(H170)=Sof(C171)=
 Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(1)
 Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C70)=Sof(H70)=Sof(C72)=Sof(H72A)=
 Sof(H72B)=Sof(H72C)=FVAR(1)
 Sof(C156)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C155)=Sof(H155)=Sof(C157)=
 Sof(H15G)=Sof(H15H)=Sof(H15I)=1-FVAR(2)
 Sof(C55)=Sof(H55)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C57)=Sof(H57A)=
 Sof(H57B)=Sof(H57C)=FVAR(2)
 Sof(C181)=Sof(H181)=Sof(C183)=Sof(H183)=Sof(C185)=Sof(H185)=Sof(C189)=
 Sof(H189)=Sof(C186)=Sof(H186)=Sof(C180)=Sof(H180)=1-FVAR(3)
 Sof(C81)=Sof(H81)=Sof(C83)=Sof(H83)=Sof(C86)=Sof(H86)=Sof(C89)=Sof(H89)=
 Sof(C80)=Sof(H80)=Sof(C84)=Sof(H84)=FVAR(3)
 Sof(C90)=Sof(H90)=Sof(C92)=Sof(H92)=Sof(C96)=Sof(H96)=Sof(C100)=Sof(H100)=
 Sof(C97)=Sof(H97)=Sof(C93)=Sof(H93)=0.5*(1-FVAR(5))
 Sof(C195)=Sof(H195)=Sof(C190)=Sof(H190)=Sof(C192)=Sof(H192)=Sof(C194)=
 Sof(H194)=Sof(C198)=Sof(H198)=Sof(C200)=Sof(H200)=0.5*FVAR(5)
4.a Ternary CH refined with riding coordinates:
 C42(H42), C58(H58), C67(H67), C39(H39), C55(H55), C27(H27), C30(H30),
 C70(H70), C170(H170), C155(H155)
4.b Me refined with riding coordinates:
 C15(H15A,H15B,H15C)
4.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C23(H23), C24(H24), C51(H51), C46(H46), C18(H18), C37(H37),
 C36(H36), C52(H52), C35(H35), C63(H63), C64(H64), C53(H53), C65(H65), C81(H81),
  C83(H83), C86(H86), C89(H89), C80(H80), C84(H84), C181(H181), C183(H183),
 C185(H185), C189(H189), C186(H186), C180(H180), C90(H90), C92(H92), C96(H96),
 C100(H100), C97(H97), C93(H93), C195(H195), C190(H190), C192(H192), C194(H194),
  C198(H198), C200(H200)
4.d Fitted hexagon refined as free rotating group:
 C81(C83,C86,C89,C80,C84), C181(C183,C185,C189,C186,C180), C90(C92,C96,C100,
 C97,C93), C195(C190,C192,C194,C198,C200)
4.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C13(H13A,H13B,H13C), C41(H41A,H41B,H41C), C20(H20A,H20B,
 H20C), C48(H48A,H48B,H48C), C59(H59A,H59B,H59C), C0AA(H0AA,H0AB,H0AC),
 C32(H32A,H32B,H32C), C12(H12A,H12B,H12C), C69(H69A,H69B,H69C), C68(H68A,H68B,
 H68C), C2AA(H2AA,H2AB,H2AC), C44(H44A,H44B,H44C), C31(H31A,H31B,H31C),
 C14(H14A,H14B,H14C), C71(H71A,H71B,H71C), C56(H56A,H56B,H56C), C60(H60A,H60B,
 H60C), C40(H40A,H40B,H40C), C28(H28A,H28B,H28C), C43(H43A,H43B,H43C), C72(H72A,
 H72B,H72C), C57(H57A,H57B,H57C), C29(H29A,H29B,H29C), C172(H17A,H17B,H17C),
 C171(H17D,H17E,H17F), C156(H15D,H15E,H15F), C157(H15G,H15H,H15I)
;
_shelx_res_checksum              47402
_shelx_hkl_checksum              27696
_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 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.883