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_4342150
_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         'C63 H86 Ga4 N6 O'
_chemical_formula_sum            'C63 H86 Ga4 N6 O'
_chemical_formula_weight         1222.26
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                94.308(2)
_cell_angle_beta                 96.002(2)
_cell_angle_gamma                100.953(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7317(3)
_cell_length_b                   14.9692(4)
_cell_length_c                   19.2449(5)
_cell_measurement_reflns_used    11707
_cell_measurement_temperature    149(2)
_cell_measurement_theta_max      29.1388
_cell_measurement_theta_min      3.6665
_cell_volume                     3004.32(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-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      149(2)
_diffrn_detector_area_resol_mean 15.9821
_diffrn_measured_fraction_theta_full 0.9904
_diffrn_measured_fraction_theta_max 0.9292
_diffrn_measurement_details
;
  1 omega  -86.00   11.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -77.0000   90.0000 97

  2 omega  -24.00   24.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -99.0000  -30.0000 48

  3 omega  -90.00    3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -37.0000  150.0000 93

  4 omega  -85.00    8.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  -37.0000 -120.0000 93

  5 omega  -83.00  -35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397 -178.0000  -90.0000 48

  6 omega  -94.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.3397  178.0000   30.0000 62

  7 omega  -25.00   10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0585  -99.0000    0.0000 35

  8 omega   32.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       19.0585 -178.0000  -30.0000 64
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0435410000
_diffrn_orient_matrix_UB_12      0.0425506000
_diffrn_orient_matrix_UB_13      0.0030017000
_diffrn_orient_matrix_UB_21      -0.0494017000
_diffrn_orient_matrix_UB_22      0.0229223000
_diffrn_orient_matrix_UB_23      0.0083235000
_diffrn_orient_matrix_UB_31      0.0162301000
_diffrn_orient_matrix_UB_32      -0.0039498000
_diffrn_orient_matrix_UB_33      0.0361697000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32174
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         3.67
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74868
_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    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         13854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0320P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0705
_reflns_number_gt                10888
_reflns_number_total             13854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5029096_si_002.cif
_cod_data_source_block           compound_18
_cod_depositor_comments
'Adding full bibliography for 4342142--4342150.cif.'
_cod_original_cell_volume        3004.34(14)
_cod_database_code               4342150
_chemical_oxdiff_formula         'C40 H40 N8 Ga4'
_chemical_oxdiff_usercomment     'AT 150 K, COLORLESS, RECTANGULAR BLOCK'
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H31 of C31, H18 of C18, H12 of C12, H56 of C56, H54 of C54, H47 of C47, H51
  of C51, H11 of C11, H23 of C23, H14 of C14, H25 of C25, H15 of C15, H40 of
  C40, {H8A,H8B,H8C} of C8, {H6A,H6B,H6C} of C6, {H9A,H9B,H9C} of C9, {H4A,H4B,
  H4C} of C4, H37 of C37, H29 of C29, H30 of C30, H38 of C38, H36 of C36, H33
  of C33, H32 of C32, H43 of C43, H58 of C58, H20 of C20, H19 of C19, H55 of
  C55, H13 of C13, H61 of C61, H48 of C48, H49 of C49, H50 of C50
 At 1.5 times of:
  {H22A,H22B,H22C} of C22, {H26A,H26B,H26C} of C26, {H62A,H62B,H62C} of C62,
  {H7A,H7B,H7C} of C7, {H42A,H42B,H42C} of C42, {H5A,H5B,H5C} of C5, {H60A,H60B,
  H60C} of C60, {H24A,H24B,H24C} of C24, {H45A,H45B,H45C} of C45, {H44A,H44B,
  H44C} of C44, {H41A,H41B,H41C} of C41, {H27A,H27B,H27C} of C27, {H59A,H59B,
  H59C} of C59, {H63A,H63B,H63C} of C63
2.a Ternary CH refined with riding coordinates:
 C40(H40), C43(H43), C58(H58), C25(H25), C23(H23), C61(H61)
2.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C29(H29), C30(H30), C38(H38), C36(H36), C33(H33), C32(H32),
 C20(H20), C15(H15), C14(H14), C11(H11), C51(H51), C47(H47), C54(H54), C56(H56),
  C12(H12), C18(H18), C31(H31), C19(H19), C55(H55), C13(H13), C48(H48),
 C49(H49), C50(H50)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C7(H7A,
 H7B,H7C), C42(H42A,H42B,H42C), C5(H5A,H5B,H5C), C60(H60A,H60B,H60C), C24(H24A,
 H24B,H24C), C45(H45A,H45B,H45C), C44(H44A,H44B,H44C), C62(H62A,H62B,H62C),
 C26(H26A,H26B,H26C), C22(H22A,H22B,H22C), C41(H41A,H41B,H41C), C27(H27A,H27B,
 H27C), C59(H59A,H59B,H59C), C63(H63A,H63B,H63C)
;