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_4342149
_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         'C26 H42 Ga2 N4'
_chemical_formula_sum            'C26 H42 Ga2 N4'
_chemical_formula_weight         550.08
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-17
_audit_creation_method
;
  Olex2 1.2
  (compiled Oct 26 2012 17:06:22, GUI svn.r4371)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.884(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6745(7)
_cell_length_b                   9.7298(5)
_cell_length_c                   13.8119(7)
_cell_measurement_reflns_used    3422
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.6439
_cell_measurement_theta_min      3.8148
_cell_volume                     1432.70(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.9929
_diffrn_measured_fraction_theta_max 0.9325
_diffrn_measurement_details
;
  1 omega  -97.00   12.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.7238  -37.0000  -30.0000 109

  2 omega  -69.00  -42.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.7238  120.0000   22.0000 27

  3 omega  -10.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.1301   77.0000 -150.0000 107

  4 omega  -52.00   50.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.7238   57.0000  -30.0000 102

  5 omega  -49.00   22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       24.1301  -57.0000   90.0000 71
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0083015000
_diffrn_orient_matrix_UB_12      0.0228177000
_diffrn_orient_matrix_UB_13      -0.0480376000
_diffrn_orient_matrix_UB_21      0.0102866000
_diffrn_orient_matrix_UB_22      0.0678601000
_diffrn_orient_matrix_UB_23      0.0173631000
_diffrn_orient_matrix_UB_31      0.0652244000
_diffrn_orient_matrix_UB_32      -0.0135454000
_diffrn_orient_matrix_UB_33      0.0060063000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9475
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         3.82
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.899
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.283
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.337
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         3288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.337
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0320P)^2^+4.3795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1385
_reflns_number_gt                2725
_reflns_number_total             3288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5029096_si_002.cif
_cod_data_source_block           compound_17
_cod_depositor_comments
'Adding full bibliography for 4342142--4342150.cif.'
_cod_original_cell_volume        1432.69(13)
_cod_database_code               4342149
_chemical_oxdiff_formula         'C12 H14 N4 Ga2'
_chemical_oxdiff_usercomment     'AT 150 k, COLORLESS, BLOCK, .45 .45 .4'
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H12 of C12, H3 of N3, H9 of C9, H8 of C8, H10 of C10, H7 of C7
 At 1.5 times of:
  {H5A,H5B,H5C} of C5, {H1A,H1B,H1C} of C1, {H2A,H2B,H2C} of C2, {H6A,H6B,
  H6C} of C6, {H13A,H13B,H13C} of C13
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), N3(H3)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C13(H13A,
 H13B,H13C)
;