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_4328413
_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 Ga N'
_chemical_formula_sum            'C21 H36 Ga N'
_chemical_formula_weight         372.23
_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                64.192(1)
_cell_angle_beta                 87.174(1)
_cell_angle_gamma                72.371(1)
_cell_formula_units_Z            2
_cell_length_a                   8.9135(2)
_cell_length_b                   11.8766(2)
_cell_length_c                   11.9732(3)
_cell_measurement_reflns_used    6687
_cell_measurement_temperature    140
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.90
_cell_volume                     1082.45(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 1.000
_diffrn_measurement_device_type  'Bruker platform with 6k CCD'
_diffrn_measurement_method       'omega 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  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15412
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.858
_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    1.142
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             400
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .25
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+0.3121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                5143
_reflns_number_total             5367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202427z_si_001_5.cif
_cod_data_source_block           10
_cod_database_code               4328413