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_1565070
_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         'C67 H82 Al2 Mo N4 O9, C7 H8'
_chemical_formula_sum            'C74 H90 Al2 Mo N4 O9'
_chemical_formula_weight         1329.39
_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             2021-03-29
_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                 96.194(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5122(5)
_cell_length_b                   12.6927(3)
_cell_length_c                   36.0314(9)
_cell_measurement_reflns_used    8734
_cell_measurement_temperature    173.05(10)
_cell_measurement_theta_max      73.1680
_cell_measurement_theta_min      4.2580
_cell_volume                     7052.9(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)'
_computing_structure_solution
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.948
_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    -71.00  12.00   1.00    5.00    --  -42.36  57.00  30.00   83
  2  \w   -107.00 -18.00   1.00    5.00    --  -42.36 -38.00  30.00   89
  3  \w     34.00 131.00   1.00   20.00    --  105.13 -61.00-150.00   97
  4  \w     77.00 172.00   1.00   20.00    --  105.13  61.00   0.00   95
  5  \w     24.00  95.00   1.00   20.00    --  105.13 -95.00 120.00   71
  6  \w     23.00 101.00   1.00   20.00    --  105.13 -95.00-180.00   78
;
_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      0.0343907000
_diffrn_orient_matrix_UB_12      0.0046140000
_diffrn_orient_matrix_UB_13      0.0417398000
_diffrn_orient_matrix_UB_21      -0.0854688000
_diffrn_orient_matrix_UB_22      -0.0494992000
_diffrn_orient_matrix_UB_23      0.0099542000
_diffrn_orient_matrix_UB_31      0.0391111000
_diffrn_orient_matrix_UB_32      -0.1105173000
_diffrn_orient_matrix_UB_33      -0.0028326000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            22491
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.565
_diffrn_reflns_theta_min         3.240
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.222
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.872
_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            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       block
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         13474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0612P)^2^+1.5471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10739
_reflns_number_total             13474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04940b3.cif
_cod_data_source_block           4-Mo
_cod_database_code               1565070
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C67 H82 Al2 N4 O9 Mo1'
_reflns_odcompleteness_completeness 98.28
_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.a Ternary CH refined with riding coordinates:
 C24(H24), C50(H50), C33(H33), C65(H65), C62(H62), C21(H21), C36(H36), C53(H53)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C41(H41), C19(H19), C17(H17), C29(H29), C60(H60), C18(H18),
 C31(H31), C30(H30), C46(H46), C58(H58), C47(H47), C59(H59), C48(H48), C72(H72),
  C73(H73), C69(H69), C70(H70), C71(H71)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C43(H43A,H43B,H43C), C14(H14A,H14B,H14C), C34(H34A,H34B,
 H34C), C52(H52A,H52B,H52C), C51(H51A,H51B,H51C), C64(H64A,H64B,H64C), C63(H63A,
 H63B,H63C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C), C39(H39A,H39B,H39C),
 C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C67(H67A,H67B,H67C), C22(H22A,H22B,
 H22C), C37(H37A,H37B,H37C), C66(H66A,H66B,H66C), C38(H38A,H38B,H38C), C74(H74A,
 H74B,H74C), C55(H55A,H55B,H55C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              35090
_shelx_hkl_checksum              44020
_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 1.345
_oxdiff_exptl_absorpt_empirical_full_min 0.772