Insertion of benzonitrile into Al-N and ga-N bonds: formation of fused carbatriaza-gallanes/alanes and their subsequent synthesis from amidines and trimethyl-gallium/aluminum.
Maheswari, K.; Rao, A. Ramakrishna; Reddy, N. Dastagiri; Inorganic chemistry 54 (2015) 2000–2008; doi:10.1021/ic5029096

data_4342142
_publ_section_title
;
 Insertion of benzonitrile into Al-N and ga-N bonds: formation of fused
 carbatriaza-gallanes/alanes and their subsequent synthesis from amidines
 and trimethyl-gallium/aluminum.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2000
_journal_page_last               2008
_journal_paper_doi               10.1021/ic5029096
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C21 H21 Ga2 N3'
_chemical_formula_sum            'C21 H21 Ga2 N3'
_chemical_formula_weight         454.85
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   19.2352(4)
_cell_length_b                   19.2352(4)
_cell_length_c                   33.3633(9)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      3.67
_cell_volume                     10690.4(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.923
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            33439
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.10
_diffrn_reflns_theta_min         0.924
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.275
_exptl_absorpt_correction_T_max  0.664
_exptl_absorpt_correction_T_min  0.497
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4140
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         5892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                4062
_reflns_number_total             5892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5029096_si_002.cif
_cod_data_source_block           compound_5
_cod_depositor_comments
'Adding full bibliography for 4342142--4342150.cif.'
_cod_database_code               4342142
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C15(H15), C11(H11), C14(H14), C9(H9), C13(H13), C12(H12), C33(H33),
 C39(H39), C6(H6), C8(H8), C7(H7), C16(H16), C17(H17), C18(H18)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;