Advances in Structural Studies on Alkylaluminum Species in the Solid State via Challenging27Al‒13C NMR Spectroscopy and X-ray Diffraction
Pourpoint, Frédérique; Morin, Yohann; Gauvin, Régis M.; Trébosc, Julien; Capet, Frédéric; Lafon, Olivier; Amoureux, Jean-Paul; The Journal of Physical Chemistry C 117 (2013) 18091–; doi:10.1021/jp4055044

data_1512252
_publ_section_title
;
 Advances in Structural Studies on Alkylaluminum Species in the Solid
 State via Challenging27Al--13C NMR Spectroscopy and X-ray Diffraction
;
_journal_issue                   35
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              18091
_journal_paper_doi               10.1021/jp4055044
_journal_volume                  117
_journal_year                    2013
_chemical_formula_moiety         'C4 H12 Al1 Li1'
_chemical_formula_sum            'C4 H12 Al Li'
_chemical_formula_weight         94.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.7480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.2978(2)
_cell_length_b                   11.6066(3)
_cell_length_c                   9.6537(3)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33
_cell_measurement_theta_min      4
_cell_volume                     702.10(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       'omega-scans and phi-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2640
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         34.41
_diffrn_reflns_theta_min         2.75
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'twinabs 2012/1 Bruker AXS'
_exptl_crystal_density_diffrn    0.890
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         2640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+0.0219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                2361
_reflns_number_total             2640
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp4055044_si_002.cif
_cod_data_source_block           twin5
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C4 H12 Al1 Li1'
_cod_database_code               1512252