Reversible Alkene Binding and Allylic C‒H Activation with an Aluminium(I) Complex
Bakewell, Clare; White, Andrew J. P.; Crimmin, Mark Richard; Chemical Science  (2019) –; doi:10.1039/C8SC04865G

data_1550406
_publ_section_title
;
 Reversible Alkene Binding and Allylic C--H Activation with an
 Aluminium(I) Complex
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04865G
_journal_year                    2019
_chemical_formula_moiety         'C31 H45 Al N2'
_chemical_formula_sum            'C31 H45 Al N2'
_chemical_formula_weight         472.67
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-09-27
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-27 deposited with the CCDC.
2019-01-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.507(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3658(5)
_cell_length_b                   17.1209(6)
_cell_length_c                   14.0230(5)
_cell_measurement_reflns_used    2817
_cell_measurement_temperature    172.95(10)
_cell_measurement_theta_max      27.9020
_cell_measurement_theta_min      2.8260
_cell_volume                     2874.20(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      172.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.820
_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    -35.00  53.00   1.00    2.65    --  -13.33  19.00 120.00   88
  2  \w    -40.00  42.00   1.00    2.65    --  -13.33  19.00-120.00   82
;
_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      -0.0518165000
_diffrn_orient_matrix_UB_12      -0.0009475000
_diffrn_orient_matrix_UB_13      -0.0359118000
_diffrn_orient_matrix_UB_21      -0.0159013000
_diffrn_orient_matrix_UB_22      -0.0334914000
_diffrn_orient_matrix_UB_23      0.0229956000
_diffrn_orient_matrix_UB_31      -0.0238839000
_diffrn_orient_matrix_UB_32      0.0243599000
_diffrn_orient_matrix_UB_33      0.0302116000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10315
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.163
_diffrn_reflns_theta_min         2.535
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.754
_exptl_crystal_size_mid          0.473
_exptl_crystal_size_min          0.235
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5791
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0564P)^2^+0.6637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4461
_reflns_number_total             5791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04865g2.cif
_cod_data_source_block           2b
_cod_original_cell_volume        2874.20(18)
_cod_database_code               1550406
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C31 H45 Al N2 '
_chemical_oxdiff_usercomment     CB551
_reflns_odcompleteness_completeness 99.11
_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.a Ternary CH refined with riding coordinates:
 C25(H25), C13(H13), C28(H28), C16(H16)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C20(H20), C22(H22), C9(H9), C8(H8), C21(H21)
2.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C29(H29A,H29B,H29C), C15(H15A,H15B,H15C),
 C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C14(H14A,H14B,
 H14C), C12(H12A,H12B,H12C), C27(H27A,H27B,H27C)
;
_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 1.043
_oxdiff_exptl_absorpt_empirical_full_min 0.952