On the alcoholysis of alkyl-aluminum(iii) alkoxy-NHC derivatives: reactivity of the Al-carbene Lewis pair versus Al-alkyl.
Dardun, Vincent; Escomel, Léon; Jeanneau, Erwann; Camp, Clément; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10429–10433; doi:10.1039/c8dt01498a

data_7046949
_publ_section_title
;
 On the alcoholysis of alkyl-aluminum(iii) alkoxy-NHC derivatives:
 reactivity of the Al-carbene Lewis pair versus Al-alkyl.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10429
_journal_page_last               10433
_journal_paper_doi               10.1039/c8dt01498a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '2(C50 H77 Al N2 O3), 3(C6 H6)'
_chemical_formula_sum            'C118 H172 Al2 N4 O6'
_chemical_formula_weight         1796.65
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2018-04-10 deposited with the CCDC.
2018-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.99(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.392(5)
_cell_length_b                   21.778(2)
_cell_length_c                   21.355(4)
_cell_measurement_reflns_used    3411
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.0690
_cell_measurement_theta_min      3.9720
_cell_volume                     10950(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.8703
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.068
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            111871
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         29.7061
_diffrn_reflns_theta_min         3.0635
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.954
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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            colorless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.544
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.80
_refine_ls_extinction_coef       271.441
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         27389
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.0005629
_refine_ls_shift/su_mean         0.0000338
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 423. 630. 315. 75.9 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1807
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1807
_reflns_limit_h_max              32
_reflns_limit_h_min              -35
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                17587
_reflns_number_total             27442
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.45
_oxford_diffrn_Wilson_scale      0.90
_oxford_refine_ls_r_factor_ref   0.1097
_oxford_refine_ls_scale          1.0598(19)
_oxford_reflns_number_all        27389
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c8dt01498a2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 7046949--7046951.cif.'
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7046949
_oxdiff_exptl_absorpt_empirical_full_min 0.741
_oxdiff_exptl_absorpt_empirical_full_max 1.432
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;