Synthesis and Calorimetric, Spectroscopic, and Structural Characterization of Isocyanide Complexes of Trialkylaluminum and Tri-tert-butylgallium
Nicholas B. Kingsley; Kristin Kirschbaum; Joseph A. Teprovich; Robert A. Flowers; Mark R. Mason; Inorganic Chemistry 51 (2012) 2494–2502; doi:10.1021/ic202427z

data_4328411
_publ_contact_author
;
     Professor Mark R. Mason
     Department of Chemistry
     MS 602
     University of Toledo
     Toledo
     OH 43606
     USA
;
_publ_contact_author_email       mmason5@utoledo.edu
_publ_contact_author_fax         '(419) 530-4033'
_publ_contact_author_phone       '(419) 530-1532'
_publ_section_title
;
 Synthesis and Calorimetric, Spectroscopic, and Structural
 Characterization of Isocyanide Complexes of Trialkylaluminum and
 Tri-tert-butylgallium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2494
_journal_page_last               2502
_journal_paper_doi               10.1021/ic202427z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C21 H36 Al N'
_chemical_formula_sum            'C21 H36 Al N'
_chemical_formula_weight         329.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-06-15 # Formatted by publCIF
;
_cell_angle_alpha                64.069(1)
_cell_angle_beta                 87.109(1)
_cell_angle_gamma                72.330(1)
_cell_formula_units_Z            2
_cell_length_a                   8.8875(2)
_cell_length_b                   11.8471(2)
_cell_length_c                   11.9501(2)
_cell_measurement_reflns_used    5900
_cell_measurement_temperature    140
_cell_measurement_theta_max      33.126
_cell_measurement_theta_min      2.412
_cell_volume                     1073.19(4)
_computing_cell_refinement       'Saintplus 5.45 '
_computing_data_collection       'Smart 5.630 '
_computing_data_reduction        'Saintplus 5.45'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Bruker platform with Smart6000 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19702
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         33.32
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS;Sheldrick1996;Blessing,ActaC.1995,A51,33
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.020
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             364
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .20
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         7553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.3523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                6228
_reflns_number_total             7553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202427z_si_001_3.cif
_cod_data_source_block           8
_cod_database_code               4328411