Reversible Insertion of CO into an Aluminium‒Carbon Bond
Kong, Richard Y.; Crimmin, Mark Richard; Chemical Communications  (2019) –; doi:10.1039/C9CC02818H

data_7123385
_publ_section_title
;
 Reversible Insertion of CO into an Aluminium--Carbon Bond
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02818H
_journal_year                    2019
_chemical_formula_moiety         'C37 H51 Al N2 O, 0.5(C14 H16)'
_chemical_formula_sum            'C44 H59 Al N2 O'
_chemical_formula_weight         658.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-25 deposited with the CCDC.    2019-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.3410(10)
_cell_length_b                   14.7167(6)
_cell_length_c                   10.9529(5)
_cell_measurement_reflns_used    2036
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.1410
_cell_measurement_theta_min      3.4360
_cell_volume                     3923.5(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.816
_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    -25.00  52.00   1.00    5.10    --  -13.33  57.00 150.00   77
  2  \w    -74.00 -41.00   1.00    5.10    --  -13.33-178.00 -30.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0082340000
_diffrn_orient_matrix_UB_12      -0.0256662000
_diffrn_orient_matrix_UB_13      0.0516195000
_diffrn_orient_matrix_UB_21      -0.0179914000
_diffrn_orient_matrix_UB_22      0.0355712000
_diffrn_orient_matrix_UB_23      0.0177190000
_diffrn_orient_matrix_UB_31      -0.0213968000
_diffrn_orient_matrix_UB_32      -0.0200044000
_diffrn_orient_matrix_UB_33      -0.0348159000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8658
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.201
_diffrn_reflns_theta_min         2.502
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.923
_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    1.115
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.787
_exptl_crystal_size_mid          0.637
_exptl_crystal_size_min          0.315
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+2.0502P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2954
_reflns_number_total             4102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02818h2.cif
_cod_data_source_block           mrc18111
_cod_database_code               7123385
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C36 H51 Al N2 O'
_reflns_odcompleteness_completeness 98.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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. Others
 Fixed Sof: H30A(0.5) H30B(0.5) H30C(0.5) C2(0.5) H2(0.5) C4(0.5) H4(0.5)
 C8(0.5) H8A(0.5) H8B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C7(0.5) H7(0.5) C3(0.5)
 H3(0.5) C6(0.5) H6A(0.5) H6B(0.5) C1(0.5)
3.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C2(H2), C4(H4), C7(H7), C3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C5(H5A,H5B), C6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C16(H16), C15(H15), C26(H26), C27(H27), C25(H25),
 C28(H28), C29(H29)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C20(H20A,H20B,
 H20C), C19(H19A,H19B,H19C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              60890
_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 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.817