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

data_7123384
_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         'C35 H49 Al N2'
_chemical_formula_sum            'C35 H49 Al N2'
_chemical_formula_weight         524.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-03-12
_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                 105.015(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.7484(13)
_cell_length_b                   9.4906(9)
_cell_length_c                   13.5651(15)
_cell_measurement_reflns_used    1471
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      27.3530
_cell_measurement_theta_min      2.9460
_cell_volume                     1585.2(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    'ShelXS (Sheldrick, 2008)'
_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 0.811
_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     -3.00  84.00   1.00    1.12    --   14.74  37.00  30.00   87
  2  \w    -53.00  32.00   1.00    1.12    --   14.74 -37.00-150.00   85
;
_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      0.0314308000
_diffrn_orient_matrix_UB_12      0.0621224000
_diffrn_orient_matrix_UB_13      0.0018043000
_diffrn_orient_matrix_UB_21      0.0415838000
_diffrn_orient_matrix_UB_22      -0.0297423000
_diffrn_orient_matrix_UB_23      0.0395971000
_diffrn_orient_matrix_UB_31      0.0244944000
_diffrn_orient_matrix_UB_32      -0.0291603000
_diffrn_orient_matrix_UB_33      -0.0367930000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.811
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5594
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.811
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.288
_diffrn_reflns_theta_min         2.710
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.919
_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    1.099
_exptl_crystal_description       plate
_exptl_crystal_F_000             572
_exptl_crystal_size_max          1.42
_exptl_crystal_size_mid          0.662
_exptl_crystal_size_min          0.212
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3191
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0663P)^2^+0.2408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2414
_reflns_number_total             3191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02818h2.cif
_cod_data_source_block           mrc18105
_cod_database_code               7123384
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C35 H49 N2 Al'
_chemical_oxdiff_usercomment     RK179
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.885
_reflns_odcompleteness_completeness 99.00
_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. Restrained distances
 C2-C3
 1.35 with sigma of 0.1
 C5-C6
 1.5 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C1 \\sim C6 \\sim C2 \\sim C4 \\sim C3 \\sim C5: within 3A with sigma of 0.01
and sigma for terminal atoms of 0.01
4. Others
 Sof(H16A)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=1-FVAR(1)
 Sof(H16)=Sof(C117)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C118)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=FVAR(1)
 Fixed Sof: C1(0.5) H1(0.5) C6(0.5) H6A(0.5) H6B(0.5) C2(0.5) H2(0.5) C4(0.5)
 H4(0.5) C3(0.5) H3(0.5) C5(0.5) H5A(0.5) H5B(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C19(H19), C16(H16), C16(H16A), C4(H4)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C5(H5A,H5B)
5.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C14(H14), C13(H13), C12(H12), C2(H2), C3(H3)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C7(H7A,H7B,H7C), C21(H21A,H21B,H21C), C117(H11A,H11B,
 H11C), C118(H11D,H11E,H11F), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              774
_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 1.287
_oxdiff_exptl_absorpt_empirical_full_min 0.786